data_(FCA3)2PbBr4_150K # was data_FB_0m _publ_contact_author_name 'Zeller, Matthias' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Dr. West Lafayette IN 47907-2084 USA ; _publ_contact_author_email 'zeller4@purdue.edu' _publ_contact_author_fax '1(765)4940239' _publ_contact_author_phone '1(765)4944572' loop_ _publ_author_name _publ_author_address 'Zeller, Matthias' ; Department of Chemistry Purdue University 560 Oval Dr. West Lafayette IN 47907-2084 USA ; 'Shao, Wenhao' ; Department of Chemistry Purdue University 560 Oval Dr. West Lafayette IN 47907-2084 USA ; 'Dou, Letian' ; Department of Chemistry Purdue University 560 Oval Dr. West Lafayette IN 47907-2084 USA ; _publ_section_references ; Bruker (2022). Apex4 2022.1-1, SAINT V8.40B, Bruker AXS Inc.: Madison (WI), USA, 2022. H\"ubschle, C. B., Sheldrick, G. M. and Dittrich, B. (2011). J. Appl. Cryst. 44, 1281--1284. Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D. (2015). J. Appl. Cryst. 48, 3--10. Sheldrick, G.M. (2008). Acta Cryst. A64, 112--122. Sheldrick, G. M. (2019). SHELXL2019. University of G\"ottingen, Germany. Sheldrick, G. M. (2015a). Crystal structure refinement with SHELXL, Acta Cryst. C71, 3--8. Sheldrick, G. M. (2015b). SHELXT--Integrated space-group and crystal-structure determination, Acta Cryst. A71 3--8. ; _publ_section_acknowledgements ; This material is based upon work supported by the National Science Foundation through the Major Research Instrumentation Program under Grant No. CHE 1625543. (Funding for the single crystal X-ray diffractometer). ; # start Validation Reply Form _vrf_PLAT971_FB_0m ; PROBLEM: Check Calcd Resid. Dens. 0.84Ang From Br7 3.47 eA-3 RESPONSE: The crystal exhibits pseudo-lattice translation along of the a-axis. The largest Q peaks are located at the positions of Pb and Br atoms translated by [0.5 0 0]. Crystals were rod/needle shaped and were face indexed for absorption correction. Crystals splinter upon attempts to cut crystals to a smaller size, preventing use of a smaller less assymmetric crystal for data collection. ; # end Validation Reply Form _audit_creation_method 'SHELXL-2019/3' _shelx_SHELXL_version_number '2019/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Br8 Pb2, 4(C9 H11 F N O3), H2 O' _chemical_formula_sum 'C36 H46 Br8 F4 N4 O13 Pb2' _chemical_formula_weight 1872.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.897(8) _cell_length_b 7.7711(19) _cell_length_c 41.271(17) _cell_angle_alpha 90 _cell_angle_beta 98.49(3) _cell_angle_gamma 90 _cell_volume 5360(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9182 _cell_measurement_theta_min 2.4158 _cell_measurement_theta_max 30.5026 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.320 _exptl_crystal_F_000 3496 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.710 _exptl_crystal_size_mid 0.176 _exptl_crystal_size_min 0.166 _exptl_absorpt_coefficient_mu 12.310 _shelx_estimated_absorpt_T_min 0.042 _shelx_estimated_absorpt_T_max 0.234 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.041 _exptl_absorpt_correction_T_max 0.228 _exptl_absorpt_process_details ; SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'fine focus sealed tube X-ray source' _diffrn_source_current '30 mA' _diffrn_source_voltage '50 kV' _diffrn_radiation_monochromator 'Triumph curved graphite crystal' _diffrn_measurement_device 'three circle diffractometer' _diffrn_measurement_device_type 'Bruker AXS D8 Quest' _diffrn_detector_type 'PhotonII charge-integrating pixel array (CPAD)' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean 7.4074 _diffrn_reflns_number 143170 _diffrn_reflns_av_unetI/netI 0.0247 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -55 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 2.437 _diffrn_reflns_theta_max 28.281 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 13319 _reflns_number_gt 11994 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Apex4 v2022.10-1 (Bruker, 2022)' _computing_cell_refinement 'SAINT V8.40B (Bruker, 2020)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2020)' _computing_structure_solution 'SHELXT (Sheldrick, 2015b)' _computing_structure_refinement ; SHELXL-2019/2 (Sheldrick, 2015a, 2019), SHELXLE Rev1573 (H\"ubschle et al., 2011) ; _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The crystal exhibits pseudo-lattice translation along of the a-axis. Exact translational symmetry is broken by the presence or absence of a water molecule, by different torsion angles for the ethyl ammonium groups of two cations (residues 1 and 3) and by a slight modulation of the Pb and Br atoms. Water H atom positions were refined and O-H and H...H distances were restrained to 0.84(2) and 1.36(2) Angstrom, respectively. Carboxylic acid H atoms were placed in calculated positions and allowed to refine, but were constrained to coplanar with the COO fragments they are part of. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+52.5124P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 13319 _refine_ls_number_parameters 618 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.12934(2) 0.08788(3) 0.24543(2) 0.02204(5) Uani 1 1 d . . . . . Pb2 Pb 0.37124(2) 0.59205(3) 0.24394(2) 0.02267(5) Uani 1 1 d . . . . . Br1 Br -0.01080(3) -0.11395(7) 0.26063(2) 0.02827(12) Uani 1 1 d . . . . . Br2 Br 0.28106(4) 0.26184(8) 0.23170(2) 0.03487(13) Uani 1 1 d . . . . . Br3 Br 0.07801(4) 0.02383(8) 0.17622(2) 0.03134(12) Uani 1 1 d . . . . . Br4 Br 0.16762(4) 0.15635(8) 0.31936(2) 0.03129(12) Uani 1 1 d . . . . . Br5 Br 0.22048(5) 0.76747(10) 0.25458(2) 0.0556(2) Uani 1 1 d . . . . . Br6 Br 0.47650(3) 0.89861(7) 0.25921(2) 0.02616(11) Uani 1 1 d . . . . . Br7 Br 0.35915(4) 0.67232(8) 0.17353(2) 0.03549(14) Uani 1 1 d . . . . . Br8 Br 0.39498(4) 0.53642(8) 0.31786(2) 0.03158(12) Uani 1 1 d . . . . . F1_1 F 0.0102(2) 0.6031(6) 0.05715(9) 0.0454(10) Uani 1 1 d . . . . . O1_1 O 0.1067(2) 0.5866(6) 0.11319(10) 0.0316(9) Uani 1 1 d . . . . . O2_1 O 0.3635(2) 0.8741(6) 0.08887(10) 0.0362(10) Uani 1 1 d . . . . . H2O_1 H 0.407585 0.918127 0.086412 0.054 Uiso 1 1 calc R U . . . O3_1 O 0.3368(3) 0.9353(7) 0.03563(11) 0.0399(11) Uani 1 1 d . . . . . O4_1 O -0.0559(3) 0.4585(10) 0.11541(14) 0.0629(17) Uani 1 1 d D . . . . H4A_1 H -0.032(5) 0.484(14) 0.0995(14) 0.094 Uiso 1 1 d D U . . . H4B_1 H -0.102(3) 0.424(14) 0.108(2) 0.094 Uiso 1 1 d D U . . . N1_1 N 0.0334(3) 0.6000(7) 0.17017(14) 0.0381(12) Uani 1 1 d . . . . . H1A_1 H -0.001787 0.567025 0.152414 0.057 Uiso 1 1 calc R U . . . H1B_1 H 0.040191 0.716098 0.169771 0.057 Uiso 1 1 calc R U . . . H1C_1 H 0.014050 0.569711 0.188798 0.057 Uiso 1 1 calc R U . . . C1_1 C 0.1101(4) 0.5152(8) 0.16941(15) 0.0334(13) Uani 1 1 d . . . . . H1D_1 H 0.100870 0.391741 0.164294 0.040 Uiso 1 1 calc R U . . . H1E_1 H 0.142864 0.523519 0.191324 0.040 Uiso 1 1 calc R U . . . C2_1 C 0.1557(3) 0.5947(9) 0.14420(14) 0.0320(12) Uani 1 1 d . . . . . H2A_1 H 0.169093 0.715916 0.150009 0.038 Uiso 1 1 calc R U . . . H2B_1 H 0.206176 0.531003 0.143523 0.038 Uiso 1 1 calc R U . . . C3_1 C 0.1370(3) 0.6576(8) 0.08768(14) 0.0272(11) Uani 1 1 d . . . . . C4_1 C 0.0854(3) 0.6668(9) 0.05810(15) 0.0319(13) Uani 1 1 d . . . . . C5_1 C 0.1070(4) 0.7373(9) 0.02998(16) 0.0369(14) Uani 1 1 d . . . . . H5_1 H 0.070198 0.740343 0.010214 0.044 Uiso 1 1 calc R U . . . C6_1 C 0.1839(3) 0.8040(8) 0.03125(14) 0.0303(12) Uani 1 1 d . . . . . H6_1 H 0.200109 0.853849 0.012273 0.036 Uiso 1 1 calc R U . . . C7_1 C 0.2367(3) 0.7972(8) 0.06040(14) 0.0261(11) Uani 1 1 d . . . . . C8_1 C 0.2139(3) 0.7233(8) 0.08864(13) 0.0256(11) Uani 1 1 d . . . . . H8_1 H 0.250788 0.718233 0.108351 0.031 Uiso 1 1 calc R U . . . C9_1 C 0.3173(3) 0.8734(8) 0.06151(13) 0.0268(11) Uani 1 1 d . . . . . F1_2 F 0.3272(2) 0.3954(6) 0.05299(10) 0.0465(10) Uani 1 1 d . . . . . O1_2 O 0.3087(3) 0.2710(6) 0.11017(11) 0.0428(12) Uani 1 1 d . . . . . O2_2 O 0.0233(3) 0.0280(7) 0.09142(11) 0.0431(11) Uani 1 1 d . . . . . H2O_2 H -0.022514 -0.015802 0.089754 0.065 Uiso 1 1 calc R U . . . O3_2 O -0.0221(3) 0.1080(8) 0.04048(12) 0.0565(16) Uani 1 1 d . . . . . N1_2 N 0.4086(3) 0.0808(7) 0.18605(13) 0.0347(11) Uani 1 1 d . . . . . H1A_2 H 0.379489 0.125057 0.200966 0.052 Uiso 1 1 calc R U . . . H1B_2 H 0.461494 0.083165 0.194451 0.052 Uiso 1 1 calc R U . . . H1C_2 H 0.393198 -0.029747 0.181399 0.052 Uiso 1 1 calc R U . . . C1_2 C 0.3948(4) 0.1855(8) 0.15552(15) 0.0331(13) Uani 1 1 d . . . . . H1D_2 H 0.430618 0.144836 0.140179 0.040 Uiso 1 1 calc R U . . . H1E_2 H 0.407965 0.307399 0.160856 0.040 Uiso 1 1 calc R U . . . C2_2 C 0.3083(4) 0.1723(8) 0.13919(15) 0.0334(13) Uani 1 1 d . . . . . H2A_2 H 0.293062 0.051334 0.134002 0.040 Uiso 1 1 calc R U . . . H2B_2 H 0.271353 0.221900 0.153193 0.040 Uiso 1 1 calc R U . . . C3_2 C 0.2437(4) 0.2583(8) 0.08636(15) 0.0321(13) Uani 1 1 d . . . . . C4_2 C 0.2552(4) 0.3264(8) 0.05588(16) 0.0335(13) Uani 1 1 d . . . . . C5_2 C 0.1969(4) 0.3240(9) 0.02924(15) 0.0365(14) Uani 1 1 d . . . . . H5_2 H 0.206432 0.370907 0.008908 0.044 Uiso 1 1 calc R U . . . C6_2 C 0.1228(4) 0.2510(9) 0.03253(15) 0.0352(14) Uani 1 1 d . . . . . H6_2 H 0.081155 0.247780 0.014335 0.042 Uiso 1 1 calc R U . . . C7_2 C 0.1104(4) 0.1839(8) 0.06222(15) 0.0304(12) Uani 1 1 d . . . . . C8_2 C 0.1704(4) 0.1863(8) 0.08951(14) 0.0301(12) Uani 1 1 d . . . . . H8_2 H 0.160917 0.139261 0.109836 0.036 Uiso 1 1 calc R U . . . C9_2 C 0.0318(4) 0.1029(9) 0.06458(15) 0.0343(13) Uani 1 1 d . . . . . F1_3 F 0.5234(2) 0.6049(6) 0.06241(9) 0.0461(10) Uani 1 1 d . . . . . O1_3 O 0.6361(3) 0.5732(6) 0.11979(10) 0.0335(9) Uani 1 1 d . . . . . O2_3 O 0.8775(3) 0.8890(7) 0.09188(11) 0.0412(11) Uani 1 1 d . . . . . O3_3 O 0.8438(3) 0.9501(7) 0.03877(11) 0.0470(13) Uani 1 1 d . . . . . H3O_3 H 0.890703 0.988647 0.041262 0.071 Uiso 1 1 calc R U . . . N1_3 N 0.6348(3) 0.6136(7) 0.18845(12) 0.0343(11) Uani 1 1 d . . . . . H1A_3 H 0.636150 0.566045 0.208671 0.051 Uiso 1 1 calc R U . . . H1B_3 H 0.626218 0.728911 0.189636 0.051 Uiso 1 1 calc R U . . . H1C_3 H 0.682343 0.594623 0.181170 0.051 Uiso 1 1 calc R U . . . C1_3 C 0.5694(4) 0.5345(9) 0.16548(15) 0.0359(14) Uani 1 1 d . . . . . H1D_3 H 0.518074 0.551313 0.173954 0.043 Uiso 1 1 calc R U . . . H1E_3 H 0.578997 0.409152 0.164233 0.043 Uiso 1 1 calc R U . . . C2_3 C 0.5631(4) 0.6106(9) 0.13177(16) 0.0376(14) Uani 1 1 d . . . . . H2A_3 H 0.517264 0.559582 0.117215 0.045 Uiso 1 1 calc R U . . . H2B_3 H 0.554924 0.736588 0.132661 0.045 Uiso 1 1 calc R U . . . C3_3 C 0.6517(4) 0.6594(8) 0.09252(14) 0.0284(12) Uani 1 1 d . . . . . C4_3 C 0.5977(4) 0.6739(9) 0.06357(15) 0.0336(13) Uani 1 1 d . . . . . C5_3 C 0.6168(4) 0.7534(10) 0.03609(16) 0.0391(15) Uani 1 1 d . . . . . H5_3 H 0.578267 0.761502 0.016895 0.047 Uiso 1 1 calc R U . . . C6_3 C 0.6926(4) 0.8218(9) 0.03657(14) 0.0336(13) Uani 1 1 d . . . . . H6_3 H 0.706626 0.876960 0.017673 0.040 Uiso 1 1 calc R U . . . C7_3 C 0.7482(4) 0.8092(8) 0.06496(14) 0.0282(12) Uani 1 1 d . . . . . C8_3 C 0.7274(4) 0.7272(8) 0.09264(13) 0.0286(12) Uani 1 1 d . . . . . H8_3 H 0.765855 0.717958 0.111828 0.034 Uiso 1 1 calc R U . . . C9_3 C 0.8289(4) 0.8860(8) 0.06599(14) 0.0309(12) Uani 1 1 d . . . . . F1_4 F 0.8172(2) 0.3898(5) 0.05594(9) 0.0389(9) Uani 1 1 d . . . . . O1_4 O 0.7927(2) 0.2650(6) 0.11243(10) 0.0320(9) Uani 1 1 d . . . . . O2_4 O 0.5035(3) 0.0310(6) 0.08913(10) 0.0356(10) Uani 1 1 d . . . . . O3_4 O 0.4705(3) 0.0946(7) 0.03618(11) 0.0438(12) Uani 1 1 d . . . . . H3O_4 H 0.429715 0.037028 0.038670 0.066 Uiso 1 1 calc R U . . . N1_4 N 0.8779(3) 0.0715(7) 0.19084(13) 0.0350(12) Uani 1 1 d . . . . . H1A_4 H 0.848071 0.120201 0.205040 0.053 Uiso 1 1 calc R U . . . H1B_4 H 0.929953 0.065846 0.200378 0.053 Uiso 1 1 calc R U . . . H1C_4 H 0.859465 -0.036551 0.185629 0.053 Uiso 1 1 calc R U . . . C1_4 C 0.8717(4) 0.1777(8) 0.16051(15) 0.0315(13) Uani 1 1 d . . . . . H1D_4 H 0.909866 0.134280 0.146393 0.038 Uiso 1 1 calc R U . . . H1E_4 H 0.886042 0.298412 0.166403 0.038 Uiso 1 1 calc R U . . . C2_4 C 0.7869(3) 0.1710(8) 0.14178(14) 0.0303(12) Uani 1 1 d . . . . . H2A_4 H 0.770014 0.050712 0.136775 0.036 Uiso 1 1 calc R U . . . H2B_4 H 0.748415 0.225983 0.154449 0.036 Uiso 1 1 calc R U . . . C3_4 C 0.7299(3) 0.2536(7) 0.08777(14) 0.0262(11) Uani 1 1 d . . . . . C4_4 C 0.6554(3) 0.1827(7) 0.08960(14) 0.0253(11) Uani 1 1 d . . . . . H4_4 H 0.643741 0.135469 0.109603 0.030 Uiso 1 1 calc R U . . . C5_4 C 0.5978(3) 0.1816(8) 0.06165(14) 0.0270(11) Uani 1 1 d . . . . . C6_4 C 0.6126(4) 0.2506(8) 0.03234(15) 0.0315(13) Uani 1 1 d . . . . . H6_4 H 0.572180 0.249023 0.013719 0.038 Uiso 1 1 calc R U . . . C7_4 C 0.6877(4) 0.3232(9) 0.03016(14) 0.0323(13) Uani 1 1 d . . . . . H7_4 H 0.699240 0.371176 0.010204 0.039 Uiso 1 1 calc R U . . . C8_4 C 0.7437(3) 0.3225(8) 0.05763(15) 0.0294(12) Uani 1 1 d . . . . . C9_4 C 0.5190(3) 0.0972(8) 0.06312(14) 0.0282(12) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01803(9) 0.02139(9) 0.02636(10) 0.00132(8) 0.00218(7) -0.00017(7) Pb2 0.01845(9) 0.02029(9) 0.02891(10) -0.00020(8) 0.00230(7) 0.00016(7) Br1 0.0311(3) 0.0264(3) 0.0280(3) -0.0005(2) 0.0068(2) -0.0092(2) Br2 0.0300(3) 0.0312(3) 0.0443(3) -0.0019(3) 0.0082(2) -0.0108(2) Br3 0.0432(3) 0.0275(3) 0.0231(3) -0.0007(2) 0.0043(2) 0.0020(2) Br4 0.0328(3) 0.0354(3) 0.0245(3) -0.0008(2) 0.0004(2) -0.0040(2) Br5 0.0463(4) 0.0433(4) 0.0844(6) 0.0254(4) 0.0331(4) 0.0270(3) Br6 0.0280(3) 0.0250(3) 0.0257(2) -0.0015(2) 0.0048(2) -0.0076(2) Br7 0.0429(3) 0.0331(3) 0.0272(3) 0.0011(2) -0.0055(2) -0.0005(3) Br8 0.0392(3) 0.0295(3) 0.0275(3) 0.0003(2) 0.0098(2) -0.0011(2) F1_1 0.0254(18) 0.073(3) 0.037(2) 0.007(2) 0.0002(15) -0.0144(19) O1_1 0.030(2) 0.040(2) 0.025(2) 0.0001(18) 0.0066(16) -0.0115(18) O2_1 0.027(2) 0.055(3) 0.027(2) 0.000(2) 0.0031(16) -0.010(2) O3_1 0.036(2) 0.055(3) 0.029(2) 0.005(2) 0.0075(18) -0.015(2) O4_1 0.048(3) 0.090(5) 0.050(3) 0.009(3) 0.003(3) -0.029(3) N1_1 0.040(3) 0.036(3) 0.040(3) 0.009(2) 0.012(2) -0.004(2) C1_1 0.035(3) 0.032(3) 0.034(3) 0.010(3) 0.010(3) 0.001(3) C2_1 0.027(3) 0.037(3) 0.032(3) 0.001(3) 0.005(2) 0.001(2) C3_1 0.025(3) 0.030(3) 0.028(3) 0.002(2) 0.009(2) -0.003(2) C4_1 0.022(3) 0.043(4) 0.031(3) 0.001(3) 0.004(2) -0.005(2) C5_1 0.025(3) 0.053(4) 0.031(3) 0.004(3) -0.001(2) -0.004(3) C6_1 0.029(3) 0.039(3) 0.023(3) 0.005(2) 0.005(2) -0.001(2) C7_1 0.024(3) 0.030(3) 0.024(3) 0.002(2) 0.004(2) -0.003(2) C8_1 0.025(3) 0.032(3) 0.020(2) -0.001(2) 0.003(2) 0.000(2) C9_1 0.027(3) 0.032(3) 0.022(3) -0.003(2) 0.006(2) 0.001(2) F1_2 0.034(2) 0.057(3) 0.048(2) 0.009(2) 0.0048(17) -0.0072(19) O1_2 0.042(3) 0.043(3) 0.038(3) 0.012(2) -0.011(2) -0.011(2) O2_2 0.042(3) 0.060(3) 0.028(2) 0.010(2) 0.0055(19) -0.004(2) O3_2 0.036(3) 0.091(4) 0.039(3) 0.026(3) -0.006(2) -0.013(3) N1_2 0.037(3) 0.031(3) 0.033(3) 0.002(2) -0.002(2) 0.001(2) C1_2 0.037(3) 0.030(3) 0.030(3) 0.005(2) -0.002(2) -0.003(3) C2_2 0.036(3) 0.033(3) 0.029(3) 0.000(2) -0.002(2) 0.001(3) C3_2 0.034(3) 0.028(3) 0.032(3) 0.001(2) -0.001(2) 0.001(2) C4_2 0.032(3) 0.033(3) 0.036(3) -0.001(3) 0.006(3) -0.001(3) C5_2 0.038(3) 0.045(4) 0.027(3) 0.006(3) 0.007(2) 0.002(3) C6_2 0.035(3) 0.045(4) 0.025(3) 0.006(3) 0.004(2) 0.003(3) C7_2 0.030(3) 0.034(3) 0.028(3) 0.000(2) 0.006(2) 0.001(2) C8_2 0.035(3) 0.029(3) 0.025(3) 0.001(2) 0.000(2) 0.003(2) C9_2 0.030(3) 0.046(4) 0.027(3) 0.002(3) 0.005(2) 0.004(3) F1_3 0.037(2) 0.066(3) 0.034(2) 0.0025(19) -0.0006(16) -0.015(2) O1_3 0.040(2) 0.034(2) 0.028(2) 0.0029(18) 0.0122(18) 0.0002(19) O2_3 0.039(2) 0.058(3) 0.026(2) 0.005(2) 0.0033(18) -0.003(2) O3_3 0.040(3) 0.071(4) 0.031(2) 0.015(2) 0.006(2) -0.013(3) N1_3 0.036(3) 0.039(3) 0.029(3) 0.004(2) 0.008(2) 0.003(2) C1_3 0.042(3) 0.037(3) 0.031(3) 0.003(3) 0.013(3) -0.008(3) C2_3 0.034(3) 0.044(4) 0.035(3) 0.002(3) 0.006(3) -0.002(3) C3_3 0.036(3) 0.028(3) 0.021(3) -0.001(2) 0.007(2) 0.001(2) C4_3 0.030(3) 0.040(3) 0.031(3) -0.002(3) 0.004(2) -0.004(3) C5_3 0.036(3) 0.052(4) 0.028(3) 0.006(3) 0.000(3) 0.002(3) C6_3 0.039(3) 0.040(3) 0.022(3) 0.007(2) 0.007(2) 0.004(3) C7_3 0.034(3) 0.026(3) 0.025(3) 0.002(2) 0.005(2) 0.002(2) C8_3 0.034(3) 0.033(3) 0.019(3) -0.001(2) 0.005(2) 0.003(2) C9_3 0.035(3) 0.034(3) 0.025(3) 0.002(2) 0.007(2) 0.004(3) F1_4 0.0288(18) 0.049(2) 0.040(2) 0.0057(17) 0.0065(15) -0.0111(16) O1_4 0.025(2) 0.039(2) 0.031(2) 0.0067(18) -0.0010(16) -0.0088(18) O2_4 0.031(2) 0.050(3) 0.025(2) 0.0059(19) 0.0039(17) -0.008(2) O3_4 0.030(2) 0.070(4) 0.029(2) 0.008(2) -0.0025(18) -0.017(2) N1_4 0.040(3) 0.032(3) 0.032(3) 0.004(2) -0.002(2) 0.003(2) C1_4 0.030(3) 0.027(3) 0.035(3) 0.002(2) -0.001(2) 0.000(2) C2_4 0.029(3) 0.037(3) 0.024(3) 0.002(2) 0.003(2) 0.000(2) C3_4 0.026(3) 0.025(3) 0.027(3) 0.000(2) 0.001(2) 0.000(2) C4_4 0.025(3) 0.027(3) 0.024(3) -0.001(2) 0.004(2) -0.001(2) C5_4 0.024(3) 0.032(3) 0.025(3) -0.002(2) 0.005(2) -0.003(2) C6_4 0.029(3) 0.039(3) 0.026(3) 0.001(2) 0.002(2) -0.004(3) C7_4 0.034(3) 0.041(3) 0.023(3) 0.003(2) 0.008(2) -0.005(3) C8_4 0.025(3) 0.032(3) 0.032(3) -0.001(2) 0.009(2) -0.007(2) C9_4 0.026(3) 0.034(3) 0.025(3) 0.001(2) 0.004(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 Br3 2.9030(13) . ? Pb1 Br5 2.9226(9) 1_545 ? Pb1 Br1 2.9831(11) . ? Pb1 Br2 3.0249(12) . ? Pb1 Br1 3.0489(9) 2 ? Pb1 Br4 3.0704(14) . ? Pb2 Br7 2.9495(14) . ? Pb2 Br5 2.9784(12) . ? Pb2 Br6 2.9841(9) . ? Pb2 Br2 2.9891(9) . ? Pb2 Br6 2.9990(12) 2_645 ? Pb2 Br8 3.0485(14) . ? F1_1 C4_1 1.360(7) . ? O1_1 C3_1 1.354(7) . ? O1_1 C2_1 1.419(7) . ? O2_1 C9_1 1.274(7) . ? O2_1 H2O_1 0.8400 . ? O3_1 C9_1 1.260(7) . ? O4_1 H4A_1 0.84(2) . ? O4_1 H4B_1 0.85(2) . ? N1_1 C1_1 1.458(8) . ? N1_1 H1A_1 0.9100 . ? N1_1 H1B_1 0.9100 . ? N1_1 H1C_1 0.9100 . ? C1_1 C2_1 1.514(8) . ? C1_1 H1D_1 0.9900 . ? C1_1 H1E_1 0.9900 . ? C2_1 H2A_1 0.9900 . ? C2_1 H2B_1 0.9900 . ? C3_1 C8_1 1.390(8) . ? C3_1 C4_1 1.393(8) . ? C4_1 C5_1 1.380(9) . ? C5_1 C6_1 1.392(8) . ? C5_1 H5_1 0.9500 . ? C6_1 C7_1 1.389(8) . ? C6_1 H6_1 0.9500 . ? C7_1 C8_1 1.404(8) . ? C7_1 C9_1 1.479(8) . ? C8_1 H8_1 0.9500 . ? F1_2 C4_2 1.351(7) . ? O1_2 C3_2 1.365(7) . ? O1_2 C2_2 1.423(7) . ? O2_2 C9_2 1.278(7) . ? O2_2 H2O_2 0.8400 . ? O3_2 C9_2 1.246(7) . ? N1_2 C1_2 1.489(7) . ? N1_2 H1A_2 0.9100 . ? N1_2 H1B_2 0.9100 . ? N1_2 H1C_2 0.9100 . ? C1_2 C2_2 1.520(8) . ? C1_2 H1D_2 0.9900 . ? C1_2 H1E_2 0.9900 . ? C2_2 H2A_2 0.9900 . ? C2_2 H2B_2 0.9900 . ? C3_2 C8_2 1.383(9) . ? C3_2 C4_2 1.404(9) . ? C4_2 C5_2 1.363(9) . ? C5_2 C6_2 1.401(9) . ? C5_2 H5_2 0.9500 . ? C6_2 C7_2 1.375(8) . ? C6_2 H6_2 0.9500 . ? C7_2 C8_2 1.400(8) . ? C7_2 C9_2 1.487(9) . ? C8_2 H8_2 0.9500 . ? F1_3 C4_3 1.359(7) . ? O1_3 C3_3 1.369(7) . ? O1_3 C2_3 1.425(7) . ? O2_3 C9_3 1.248(7) . ? O3_3 C9_3 1.287(7) . ? O3_3 H3O_3 0.8400 . ? N1_3 C1_3 1.480(8) . ? N1_3 H1A_3 0.9100 . ? N1_3 H1B_3 0.9100 . ? N1_3 H1C_3 0.9100 . ? C1_3 C2_3 1.501(9) . ? C1_3 H1D_3 0.9900 . ? C1_3 H1E_3 0.9900 . ? C2_3 H2A_3 0.9900 . ? C2_3 H2B_3 0.9900 . ? C3_3 C8_3 1.383(8) . ? C3_3 C4_3 1.397(8) . ? C4_3 C5_3 1.371(9) . ? C5_3 C6_3 1.385(9) . ? C5_3 H5_3 0.9500 . ? C6_3 C7_3 1.393(8) . ? C6_3 H6_3 0.9500 . ? C7_3 C8_3 1.397(8) . ? C7_3 C9_3 1.484(8) . ? C8_3 H8_3 0.9500 . ? F1_4 C8_4 1.360(6) . ? O1_4 C3_4 1.361(7) . ? O1_4 C2_4 1.430(7) . ? O2_4 C9_4 1.252(7) . ? O3_4 C9_4 1.280(7) . ? O3_4 H3O_4 0.8400 . ? N1_4 C1_4 1.490(8) . ? N1_4 H1A_4 0.9100 . ? N1_4 H1B_4 0.9100 . ? N1_4 H1C_4 0.9100 . ? C1_4 C2_4 1.525(8) . ? C1_4 H1D_4 0.9900 . ? C1_4 H1E_4 0.9900 . ? C2_4 H2A_4 0.9900 . ? C2_4 H2B_4 0.9900 . ? C3_4 C4_4 1.387(8) . ? C3_4 C8_4 1.405(8) . ? C4_4 C5_4 1.395(8) . ? C4_4 H4_4 0.9500 . ? C5_4 C6_4 1.380(8) . ? C5_4 C9_4 1.493(8) . ? C6_4 C7_4 1.404(8) . ? C6_4 H6_4 0.9500 . ? C7_4 C8_4 1.365(8) . ? C7_4 H7_4 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br3 Pb1 Br5 93.22(3) . 1_545 ? Br3 Pb1 Br1 89.17(3) . . ? Br5 Pb1 Br1 86.81(3) 1_545 . ? Br3 Pb1 Br2 91.75(3) . . ? Br5 Pb1 Br2 87.71(3) 1_545 . ? Br1 Pb1 Br2 174.485(19) . . ? Br3 Pb1 Br1 87.27(3) . 2 ? Br5 Pb1 Br1 170.16(2) 1_545 2 ? Br1 Pb1 Br1 83.37(3) . 2 ? Br2 Pb1 Br1 102.10(3) . 2 ? Br3 Pb1 Br4 174.838(18) . . ? Br5 Pb1 Br4 89.41(3) 1_545 . ? Br1 Pb1 Br4 86.53(3) . . ? Br2 Pb1 Br4 92.79(3) . . ? Br1 Pb1 Br4 89.39(3) 2 . ? Br7 Pb2 Br5 96.43(3) . . ? Br7 Pb2 Br6 89.52(3) . . ? Br5 Pb2 Br6 95.72(3) . . ? Br7 Pb2 Br2 93.19(2) . . ? Br5 Pb2 Br2 89.54(3) . . ? Br6 Pb2 Br2 173.784(18) . . ? Br7 Pb2 Br6 89.91(3) . 2_645 ? Br5 Pb2 Br6 173.55(2) . 2_645 ? Br6 Pb2 Br6 85.47(3) . 2_645 ? Br2 Pb2 Br6 88.94(3) . 2_645 ? Br7 Pb2 Br8 174.657(19) . . ? Br5 Pb2 Br8 84.63(3) . . ? Br6 Pb2 Br8 85.16(2) . . ? Br2 Pb2 Br8 92.06(2) . . ? Br6 Pb2 Br8 89.16(3) 2_645 . ? Pb1 Br1 Pb1 156.15(2) . 2_545 ? Pb2 Br2 Pb1 140.99(3) . . ? Pb1 Br5 Pb2 144.76(3) 1_565 . ? Pb2 Br6 Pb2 151.56(2) . 2_655 ? C3_1 O1_1 C2_1 116.5(4) . . ? C9_1 O2_1 H2O_1 109.5 . . ? H4A_1 O4_1 H4B_1 108(3) . . ? C1_1 N1_1 H1A_1 109.5 . . ? C1_1 N1_1 H1B_1 109.5 . . ? H1A_1 N1_1 H1B_1 109.5 . . ? C1_1 N1_1 H1C_1 109.5 . . ? H1A_1 N1_1 H1C_1 109.5 . . ? H1B_1 N1_1 H1C_1 109.5 . . ? N1_1 C1_1 C2_1 112.0(5) . . ? N1_1 C1_1 H1D_1 109.2 . . ? C2_1 C1_1 H1D_1 109.2 . . ? N1_1 C1_1 H1E_1 109.2 . . ? C2_1 C1_1 H1E_1 109.2 . . ? H1D_1 C1_1 H1E_1 107.9 . . ? O1_1 C2_1 C1_1 108.3(5) . . ? O1_1 C2_1 H2A_1 110.0 . . ? C1_1 C2_1 H2A_1 110.0 . . ? O1_1 C2_1 H2B_1 110.0 . . ? C1_1 C2_1 H2B_1 110.0 . . ? H2A_1 C2_1 H2B_1 108.4 . . ? O1_1 C3_1 C8_1 125.9(5) . . ? O1_1 C3_1 C4_1 116.3(5) . . ? C8_1 C3_1 C4_1 117.9(5) . . ? F1_1 C4_1 C5_1 118.8(5) . . ? F1_1 C4_1 C3_1 117.9(5) . . ? C5_1 C4_1 C3_1 123.3(5) . . ? C4_1 C5_1 C6_1 118.5(6) . . ? C4_1 C5_1 H5_1 120.8 . . ? C6_1 C5_1 H5_1 120.8 . . ? C7_1 C6_1 C5_1 119.7(5) . . ? C7_1 C6_1 H6_1 120.2 . . ? C5_1 C6_1 H6_1 120.2 . . ? C6_1 C7_1 C8_1 121.0(5) . . ? C6_1 C7_1 C9_1 118.9(5) . . ? C8_1 C7_1 C9_1 120.2(5) . . ? C3_1 C8_1 C7_1 119.8(5) . . ? C3_1 C8_1 H8_1 120.1 . . ? C7_1 C8_1 H8_1 120.1 . . ? O3_1 C9_1 O2_1 123.1(5) . . ? O3_1 C9_1 C7_1 118.8(5) . . ? O2_1 C9_1 C7_1 118.0(5) . . ? C3_2 O1_2 C2_2 117.7(5) . . ? C9_2 O2_2 H2O_2 109.5 . . ? C1_2 N1_2 H1A_2 109.5 . . ? C1_2 N1_2 H1B_2 109.5 . . ? H1A_2 N1_2 H1B_2 109.5 . . ? C1_2 N1_2 H1C_2 109.5 . . ? H1A_2 N1_2 H1C_2 109.5 . . ? H1B_2 N1_2 H1C_2 109.5 . . ? N1_2 C1_2 C2_2 111.0(5) . . ? N1_2 C1_2 H1D_2 109.4 . . ? C2_2 C1_2 H1D_2 109.4 . . ? N1_2 C1_2 H1E_2 109.4 . . ? C2_2 C1_2 H1E_2 109.4 . . ? H1D_2 C1_2 H1E_2 108.0 . . ? O1_2 C2_2 C1_2 102.3(5) . . ? O1_2 C2_2 H2A_2 111.3 . . ? C1_2 C2_2 H2A_2 111.3 . . ? O1_2 C2_2 H2B_2 111.3 . . ? C1_2 C2_2 H2B_2 111.3 . . ? H2A_2 C2_2 H2B_2 109.2 . . ? O1_2 C3_2 C8_2 126.7(6) . . ? O1_2 C3_2 C4_2 114.5(6) . . ? C8_2 C3_2 C4_2 118.7(6) . . ? F1_2 C4_2 C5_2 119.1(6) . . ? F1_2 C4_2 C3_2 118.3(6) . . ? C5_2 C4_2 C3_2 122.6(6) . . ? C4_2 C5_2 C6_2 118.5(6) . . ? C4_2 C5_2 H5_2 120.7 . . ? C6_2 C5_2 H5_2 120.7 . . ? C7_2 C6_2 C5_2 119.7(6) . . ? C7_2 C6_2 H6_2 120.2 . . ? C5_2 C6_2 H6_2 120.2 . . ? C6_2 C7_2 C8_2 121.7(6) . . ? C6_2 C7_2 C9_2 118.2(6) . . ? C8_2 C7_2 C9_2 120.0(5) . . ? C3_2 C8_2 C7_2 118.8(6) . . ? C3_2 C8_2 H8_2 120.6 . . ? C7_2 C8_2 H8_2 120.6 . . ? O3_2 C9_2 O2_2 123.0(6) . . ? O3_2 C9_2 C7_2 119.3(6) . . ? O2_2 C9_2 C7_2 117.7(5) . . ? C3_3 O1_3 C2_3 117.9(5) . . ? C9_3 O3_3 H3O_3 109.5 . . ? C1_3 N1_3 H1A_3 109.5 . . ? C1_3 N1_3 H1B_3 109.5 . . ? H1A_3 N1_3 H1B_3 109.5 . . ? C1_3 N1_3 H1C_3 109.5 . . ? H1A_3 N1_3 H1C_3 109.5 . . ? H1B_3 N1_3 H1C_3 109.5 . . ? N1_3 C1_3 C2_3 112.0(5) . . ? N1_3 C1_3 H1D_3 109.2 . . ? C2_3 C1_3 H1D_3 109.2 . . ? N1_3 C1_3 H1E_3 109.2 . . ? C2_3 C1_3 H1E_3 109.2 . . ? H1D_3 C1_3 H1E_3 107.9 . . ? O1_3 C2_3 C1_3 107.1(5) . . ? O1_3 C2_3 H2A_3 110.3 . . ? C1_3 C2_3 H2A_3 110.3 . . ? O1_3 C2_3 H2B_3 110.3 . . ? C1_3 C2_3 H2B_3 110.3 . . ? H2A_3 C2_3 H2B_3 108.5 . . ? O1_3 C3_3 C8_3 118.3(5) . . ? O1_3 C3_3 C4_3 124.2(6) . . ? C8_3 C3_3 C4_3 117.3(5) . . ? F1_3 C4_3 C5_3 118.5(6) . . ? F1_3 C4_3 C3_3 118.8(5) . . ? C5_3 C4_3 C3_3 122.7(6) . . ? C4_3 C5_3 C6_3 119.4(6) . . ? C4_3 C5_3 H5_3 120.3 . . ? C6_3 C5_3 H5_3 120.3 . . ? C5_3 C6_3 C7_3 119.5(6) . . ? C5_3 C6_3 H6_3 120.3 . . ? C7_3 C6_3 H6_3 120.3 . . ? C6_3 C7_3 C8_3 120.0(6) . . ? C6_3 C7_3 C9_3 119.9(5) . . ? C8_3 C7_3 C9_3 120.1(5) . . ? C3_3 C8_3 C7_3 121.0(5) . . ? C3_3 C8_3 H8_3 119.5 . . ? C7_3 C8_3 H8_3 119.5 . . ? O2_3 C9_3 O3_3 123.5(6) . . ? O2_3 C9_3 C7_3 121.2(5) . . ? O3_3 C9_3 C7_3 115.3(5) . . ? C3_4 O1_4 C2_4 117.2(4) . . ? C9_4 O3_4 H3O_4 109.5 . . ? C1_4 N1_4 H1A_4 109.5 . . ? C1_4 N1_4 H1B_4 109.5 . . ? H1A_4 N1_4 H1B_4 109.5 . . ? C1_4 N1_4 H1C_4 109.5 . . ? H1A_4 N1_4 H1C_4 109.5 . . ? H1B_4 N1_4 H1C_4 109.5 . . ? N1_4 C1_4 C2_4 110.5(5) . . ? N1_4 C1_4 H1D_4 109.5 . . ? C2_4 C1_4 H1D_4 109.5 . . ? N1_4 C1_4 H1E_4 109.5 . . ? C2_4 C1_4 H1E_4 109.5 . . ? H1D_4 C1_4 H1E_4 108.1 . . ? O1_4 C2_4 C1_4 103.6(5) . . ? O1_4 C2_4 H2A_4 111.0 . . ? C1_4 C2_4 H2A_4 111.0 . . ? O1_4 C2_4 H2B_4 111.0 . . ? C1_4 C2_4 H2B_4 111.0 . . ? H2A_4 C2_4 H2B_4 109.0 . . ? O1_4 C3_4 C4_4 126.8(5) . . ? O1_4 C3_4 C8_4 115.1(5) . . ? C4_4 C3_4 C8_4 118.1(5) . . ? C3_4 C4_4 C5_4 119.1(5) . . ? C3_4 C4_4 H4_4 120.5 . . ? C5_4 C4_4 H4_4 120.5 . . ? C6_4 C5_4 C4_4 121.8(5) . . ? C6_4 C5_4 C9_4 119.0(5) . . ? C4_4 C5_4 C9_4 119.1(5) . . ? C5_4 C6_4 C7_4 119.7(5) . . ? C5_4 C6_4 H6_4 120.1 . . ? C7_4 C6_4 H6_4 120.1 . . ? C8_4 C7_4 C6_4 117.8(5) . . ? C8_4 C7_4 H7_4 121.1 . . ? C6_4 C7_4 H7_4 121.1 . . ? F1_4 C8_4 C7_4 118.8(5) . . ? F1_4 C8_4 C3_4 117.7(5) . . ? C7_4 C8_4 C3_4 123.5(5) . . ? O2_4 C9_4 O3_4 123.4(5) . . ? O2_4 C9_4 C5_4 121.0(5) . . ? O3_4 C9_4 C5_4 115.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3_1 O1_1 C2_1 C1_1 177.9(5) . . . . ? N1_1 C1_1 C2_1 O1_1 -57.0(7) . . . . ? C2_1 O1_1 C3_1 C8_1 6.0(9) . . . . ? C2_1 O1_1 C3_1 C4_1 -173.0(6) . . . . ? O1_1 C3_1 C4_1 F1_1 -0.6(9) . . . . ? C8_1 C3_1 C4_1 F1_1 -179.8(6) . . . . ? O1_1 C3_1 C4_1 C5_1 179.2(6) . . . . ? C8_1 C3_1 C4_1 C5_1 0.1(10) . . . . ? F1_1 C4_1 C5_1 C6_1 179.3(6) . . . . ? C3_1 C4_1 C5_1 C6_1 -0.5(11) . . . . ? C4_1 C5_1 C6_1 C7_1 0.3(10) . . . . ? C5_1 C6_1 C7_1 C8_1 0.3(10) . . . . ? C5_1 C6_1 C7_1 C9_1 -178.2(6) . . . . ? O1_1 C3_1 C8_1 C7_1 -178.5(6) . . . . ? C4_1 C3_1 C8_1 C7_1 0.6(9) . . . . ? C6_1 C7_1 C8_1 C3_1 -0.8(9) . . . . ? C9_1 C7_1 C8_1 C3_1 177.7(5) . . . . ? C6_1 C7_1 C9_1 O3_1 -3.1(9) . . . . ? C8_1 C7_1 C9_1 O3_1 178.4(6) . . . . ? C6_1 C7_1 C9_1 O2_1 176.4(6) . . . . ? C8_1 C7_1 C9_1 O2_1 -2.1(9) . . . . ? C3_2 O1_2 C2_2 C1_2 167.2(5) . . . . ? N1_2 C1_2 C2_2 O1_2 -176.8(5) . . . . ? C2_2 O1_2 C3_2 C8_2 13.5(10) . . . . ? C2_2 O1_2 C3_2 C4_2 -166.2(6) . . . . ? O1_2 C3_2 C4_2 F1_2 0.2(9) . . . . ? C8_2 C3_2 C4_2 F1_2 -179.5(6) . . . . ? O1_2 C3_2 C4_2 C5_2 179.6(6) . . . . ? C8_2 C3_2 C4_2 C5_2 -0.1(10) . . . . ? F1_2 C4_2 C5_2 C6_2 179.5(6) . . . . ? C3_2 C4_2 C5_2 C6_2 0.1(10) . . . . ? C4_2 C5_2 C6_2 C7_2 0.0(10) . . . . ? C5_2 C6_2 C7_2 C8_2 -0.1(10) . . . . ? C5_2 C6_2 C7_2 C9_2 -178.3(6) . . . . ? O1_2 C3_2 C8_2 C7_2 -179.7(6) . . . . ? C4_2 C3_2 C8_2 C7_2 0.0(9) . . . . ? C6_2 C7_2 C8_2 C3_2 0.1(9) . . . . ? C9_2 C7_2 C8_2 C3_2 178.2(6) . . . . ? C6_2 C7_2 C9_2 O3_2 -4.7(10) . . . . ? C8_2 C7_2 C9_2 O3_2 177.1(7) . . . . ? C6_2 C7_2 C9_2 O2_2 174.1(6) . . . . ? C8_2 C7_2 C9_2 O2_2 -4.1(9) . . . . ? C3_3 O1_3 C2_3 C1_3 -166.5(5) . . . . ? N1_3 C1_3 C2_3 O1_3 62.7(7) . . . . ? C2_3 O1_3 C3_3 C8_3 134.6(6) . . . . ? C2_3 O1_3 C3_3 C4_3 -49.8(8) . . . . ? O1_3 C3_3 C4_3 F1_3 2.9(10) . . . . ? C8_3 C3_3 C4_3 F1_3 178.5(6) . . . . ? O1_3 C3_3 C4_3 C5_3 -176.5(6) . . . . ? C8_3 C3_3 C4_3 C5_3 -0.9(10) . . . . ? F1_3 C4_3 C5_3 C6_3 -178.9(6) . . . . ? C3_3 C4_3 C5_3 C6_3 0.5(11) . . . . ? C4_3 C5_3 C6_3 C7_3 -0.2(10) . . . . ? C5_3 C6_3 C7_3 C8_3 0.3(10) . . . . ? C5_3 C6_3 C7_3 C9_3 -178.4(6) . . . . ? O1_3 C3_3 C8_3 C7_3 176.8(5) . . . . ? C4_3 C3_3 C8_3 C7_3 1.0(9) . . . . ? C6_3 C7_3 C8_3 C3_3 -0.7(9) . . . . ? C9_3 C7_3 C8_3 C3_3 178.0(6) . . . . ? C6_3 C7_3 C9_3 O2_3 174.0(6) . . . . ? C8_3 C7_3 C9_3 O2_3 -4.7(9) . . . . ? C6_3 C7_3 C9_3 O3_3 -4.9(9) . . . . ? C8_3 C7_3 C9_3 O3_3 176.3(6) . . . . ? C3_4 O1_4 C2_4 C1_4 167.7(5) . . . . ? N1_4 C1_4 C2_4 O1_4 -175.1(5) . . . . ? C2_4 O1_4 C3_4 C4_4 10.8(9) . . . . ? C2_4 O1_4 C3_4 C8_4 -169.4(5) . . . . ? O1_4 C3_4 C4_4 C5_4 -179.8(6) . . . . ? C8_4 C3_4 C4_4 C5_4 0.4(8) . . . . ? C3_4 C4_4 C5_4 C6_4 -0.6(9) . . . . ? C3_4 C4_4 C5_4 C9_4 176.9(5) . . . . ? C4_4 C5_4 C6_4 C7_4 0.5(10) . . . . ? C9_4 C5_4 C6_4 C7_4 -177.0(6) . . . . ? C5_4 C6_4 C7_4 C8_4 -0.1(10) . . . . ? C6_4 C7_4 C8_4 F1_4 179.0(6) . . . . ? C6_4 C7_4 C8_4 C3_4 -0.1(10) . . . . ? O1_4 C3_4 C8_4 F1_4 1.0(8) . . . . ? C4_4 C3_4 C8_4 F1_4 -179.2(5) . . . . ? O1_4 C3_4 C8_4 C7_4 -179.8(6) . . . . ? C4_4 C3_4 C8_4 C7_4 0.0(9) . . . . ? C6_4 C5_4 C9_4 O2_4 179.0(6) . . . . ? C4_4 C5_4 C9_4 O2_4 1.5(9) . . . . ? C6_4 C5_4 C9_4 O3_4 0.5(9) . . . . ? C4_4 C5_4 C9_4 O3_4 -177.1(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2_1 H2O_1 O2_4 0.84 1.83 2.661(6) 168.8 1_565 yes O4_1 H4A_1 F1_1 0.84(2) 2.19(3) 3.013(7) 167(11) . yes O4_1 H4A_1 O1_1 0.84(2) 2.47(8) 2.936(7) 116(7) . yes O4_1 H4B_1 F1_4 0.85(2) 2.37(6) 3.058(7) 138(7) 1_455 yes O4_1 H4B_1 O1_4 0.85(2) 2.19(5) 2.955(7) 150(9) 1_455 yes N1_1 H1A_1 O4_1 0.91 1.86 2.754(8) 166.3 . yes N1_1 H1B_1 Br3 0.91 2.48 3.380(6) 170.2 1_565 yes N1_1 H1C_1 Br1 0.91 2.54 3.375(5) 153.5 2 yes C5_1 H5_1 O3_2 0.95 2.43 3.275(8) 147.5 3_565 yes O2_2 H2O_2 O2_3 0.84 1.86 2.694(7) 172.6 1_445 yes N1_2 H1A_2 Br2 0.91 2.48 3.372(6) 168.4 . yes N1_2 H1B_2 Br8 0.91 2.58 3.365(6) 145.3 2_645 yes N1_2 H1C_2 Br7 0.91 2.40 3.304(6) 175.1 1_545 yes O3_3 H3O_3 O3_2 0.84 1.75 2.569(7) 166.4 1_665 yes N1_3 H1A_3 Br6 0.91 2.80 3.492(5) 134.2 2_645 yes N1_3 H1B_3 Br8 0.91 2.43 3.328(6) 169.5 2_655 yes N1_3 H1C_3 Br4 0.91 2.58 3.417(5) 152.6 2_655 yes C2_3 H2A_3 F1_3 0.99 2.31 2.843(7) 112.9 . yes C5_3 H5_3 O3_4 0.95 2.49 3.342(8) 149.4 3_665 yes O3_4 H3O_4 O3_1 0.84 1.74 2.572(6) 167.7 1_545 yes N1_4 H1A_4 Br5 0.91 2.45 3.356(6) 174.4 2_645 yes N1_4 H1B_4 Br1 0.91 2.90 3.508(5) 125.7 1_655 yes N1_4 H1B_4 Br3 0.91 2.85 3.541(6) 134.2 1_655 yes N1_4 H1C_4 Br4 0.91 2.43 3.329(6) 168.0 2_645 yes _refine_diff_density_max 3.581 _refine_diff_density_min -2.306 _refine_diff_density_rms 0.156 _shelx_res_file ; TITL FB_0m_a.res in P2(1)/c FB_0m.res created by SHELXL-2019/3 at 13:51:18 on 23-Jan-2024 REM Old TITL FB_0m in P2(1)/c REM SHELXT solution in P2(1)/c: R1 0.111, Rweak 0.003, Alpha 0.038 REM 0.778 for 552 systematic absences, Orientation as input REM Formula found by SHELXT: C46 N7 O9 F7 Br8 Pb2 CELL 0.71073 16.8970 7.7711 41.2710 90.000 98.489 90.000 ZERR 4.000 0.0077 0.0019 0.0172 0.000 0.027 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H N O F BR PB UNIT 144 184 16 52 16 32 8 OMIT -1 0 4 OMIT 0 6 3 OMIT 0 0 4 TEMP -123.150 SIZE 0.166 0.176 0.710 L.S. 10 BOND $H ACTA CONF HTAB EQIV $1 x, y+1, z HTAB_4 O2_1 O2_$1 HTAB O4_1 F1_1 HTAB O4_1 O1_1 EQIV $7 x-1, y, z HTAB_4 O4_1 F1_$7 HTAB_4 O4_1 O1_$7 HTAB N1_1 O4_1 HTAB N1_1 Br3_$1 EQIV $4 -x, y+1/2, -z+1/2 HTAB N1_1 Br1_$4 EQIV $8 -x, -y+1, -z HTAB_2 C5_1 O3_$8 EQIV $9 x-1, y-1, z HTAB_3 O2_2 O2_$9 HTAB N1_2 Br2 EQIV $6 -x+1, y-1/2, -z+1/2 HTAB N1_2 Br8_$6 EQIV $5 x, y-1, z HTAB N1_2 Br7_$5 EQIV $10 x+1, y+1, z HTAB_2 O3_3 O3_$10 EQIV $3 -x+1, y+1/2, -z+1/2 HTAB N1_3 Br6_$6 HTAB N1_3 Br8_$3 HTAB N1_3 Br4_$3 HTAB C2_3 F1_3 EQIV $11 -x+1, -y+1, -z HTAB_4 C5_3 O3_$11 HTAB_1 O3_4 O3_$5 HTAB N1_4 Br5_$6 EQIV $12 x+1, y, z HTAB N1_4 Br1_$12 HTAB N1_4 Br3_$12 HTAB N1_4 Br4_$6 LIST 4 FMAP 2 PLAN 20 DFIX_1 0.84 O4 H4A O4 H4B DFIX_1 1.36 H4A H4B FLAT_* C9 O2 O3 H2O FLAT_* C9 O2 O3 H3O SHEL 99 0.75 WGHT 0.012200 52.512398 FVAR 0.07979 PB1 7 0.129343 0.087877 0.245432 11.00000 0.01803 0.02139 = 0.02636 0.00132 0.00218 -0.00017 PB2 7 0.371242 0.592054 0.243939 11.00000 0.01845 0.02029 = 0.02891 -0.00020 0.00230 0.00016 BR1 6 -0.010798 -0.113949 0.260628 11.00000 0.03112 0.02641 = 0.02801 -0.00050 0.00676 -0.00919 BR2 6 0.281061 0.261842 0.231697 11.00000 0.02996 0.03120 = 0.04426 -0.00194 0.00819 -0.01080 BR3 6 0.078012 0.023830 0.176221 11.00000 0.04321 0.02753 = 0.02309 -0.00073 0.00426 0.00199 BR4 6 0.167624 0.156354 0.319358 11.00000 0.03284 0.03538 = 0.02449 -0.00085 0.00043 -0.00400 BR5 6 0.220475 0.767469 0.254576 11.00000 0.04630 0.04327 = 0.08442 0.02537 0.03305 0.02703 BR6 6 0.476501 0.898611 0.259209 11.00000 0.02802 0.02497 = 0.02575 -0.00154 0.00482 -0.00760 BR7 6 0.359150 0.672324 0.173529 11.00000 0.04290 0.03314 = 0.02720 0.00107 -0.00554 -0.00049 BR8 6 0.394977 0.536425 0.317857 11.00000 0.03917 0.02953 = 0.02750 0.00030 0.00980 -0.00110 RESI 1 F1 5 0.010158 0.603100 0.057149 11.00000 0.02536 0.07297 = 0.03669 0.00726 0.00018 -0.01444 O1 4 0.106727 0.586612 0.113186 11.00000 0.02986 0.04034 = 0.02535 0.00010 0.00662 -0.01148 O2 4 0.363462 0.874082 0.088868 11.00000 0.02657 0.05528 = 0.02651 -0.00029 0.00310 -0.01045 AFIX 147 H2O 2 0.407585 0.918127 0.086412 11.00000 -1.50000 AFIX 0 O3 4 0.336846 0.935295 0.035628 11.00000 0.03628 0.05528 = 0.02888 0.00538 0.00749 -0.01506 O4 4 -0.055860 0.458514 0.115412 11.00000 0.04754 0.08960 = 0.05033 0.00923 0.00338 -0.02876 H4A 2 -0.032365 0.484122 0.099485 11.00000 -1.50000 H4B 2 -0.102459 0.424133 0.107820 11.00000 -1.50000 N1 3 0.033440 0.599980 0.170170 11.00000 0.03954 0.03608 = 0.04042 0.00924 0.01155 -0.00404 AFIX 137 H1A 2 -0.001787 0.567025 0.152414 11.00000 -1.50000 H1B 2 0.040191 0.716098 0.169771 11.00000 -1.50000 H1C 2 0.014050 0.569711 0.188798 11.00000 -1.50000 AFIX 0 C1 1 0.110144 0.515216 0.169411 11.00000 0.03544 0.03199 = 0.03414 0.00968 0.00960 0.00109 AFIX 23 H1D 2 0.100870 0.391741 0.164294 11.00000 -1.20000 H1E 2 0.142864 0.523519 0.191324 11.00000 -1.20000 AFIX 0 C2 1 0.155702 0.594698 0.144195 11.00000 0.02691 0.03703 = 0.03210 0.00147 0.00456 0.00058 AFIX 23 H2A 2 0.169093 0.715916 0.150009 11.00000 -1.20000 H2B 2 0.206176 0.531003 0.143523 11.00000 -1.20000 AFIX 0 C3 1 0.137012 0.657610 0.087677 11.00000 0.02536 0.03029 = 0.02751 0.00232 0.00899 -0.00267 C4 1 0.085429 0.666797 0.058099 11.00000 0.02184 0.04319 = 0.03072 0.00063 0.00375 -0.00535 C5 1 0.106974 0.737334 0.029980 11.00000 0.02485 0.05324 = 0.03096 0.00396 -0.00111 -0.00356 AFIX 43 H5 2 0.070198 0.740343 0.010214 11.00000 -1.20000 AFIX 0 C6 1 0.183854 0.803987 0.031250 11.00000 0.02900 0.03925 = 0.02292 0.00539 0.00453 -0.00127 AFIX 43 H6 2 0.200109 0.853849 0.012273 11.00000 -1.20000 AFIX 0 C7 1 0.236677 0.797226 0.060400 11.00000 0.02448 0.02994 = 0.02403 0.00190 0.00409 -0.00270 C8 1 0.213861 0.723329 0.088645 11.00000 0.02467 0.03159 = 0.02028 -0.00086 0.00274 0.00013 AFIX 43 H8 2 0.250788 0.718233 0.108351 11.00000 -1.20000 AFIX 0 C9 1 0.317263 0.873371 0.061509 11.00000 0.02698 0.03184 = 0.02225 -0.00255 0.00613 0.00105 RESI 2 F1 5 0.327226 0.395381 0.052995 11.00000 0.03414 0.05660 = 0.04834 0.00936 0.00479 -0.00724 O1 4 0.308703 0.270964 0.110174 11.00000 0.04189 0.04297 = 0.03850 0.01196 -0.01102 -0.01099 O2 4 0.023349 0.028042 0.091425 11.00000 0.04192 0.05977 = 0.02783 0.00971 0.00547 -0.00352 AFIX 147 H2O 2 -0.022514 -0.015802 0.089754 11.00000 -1.50000 AFIX 0 O3 4 -0.022093 0.107984 0.040479 11.00000 0.03629 0.09093 = 0.03887 0.02589 -0.00597 -0.01323 N1 3 0.408589 0.080824 0.186053 11.00000 0.03739 0.03140 = 0.03320 0.00217 -0.00169 0.00085 AFIX 137 H1A 2 0.379489 0.125057 0.200966 11.00000 -1.50000 H1B 2 0.461494 0.083165 0.194451 11.00000 -1.50000 H1C 2 0.393198 -0.029747 0.181399 11.00000 -1.50000 AFIX 0 C1 1 0.394820 0.185540 0.155525 11.00000 0.03741 0.03024 = 0.02953 0.00492 -0.00217 -0.00312 AFIX 23 H1D 2 0.430618 0.144836 0.140179 11.00000 -1.20000 H1E 2 0.407965 0.307399 0.160856 11.00000 -1.20000 AFIX 0 C2 1 0.308349 0.172316 0.139187 11.00000 0.03645 0.03300 = 0.02868 0.00016 -0.00240 0.00066 AFIX 23 H2A 2 0.293062 0.051334 0.134002 11.00000 -1.20000 H2B 2 0.271353 0.221900 0.153193 11.00000 -1.20000 AFIX 0 C3 1 0.243722 0.258298 0.086360 11.00000 0.03438 0.02803 = 0.03195 0.00136 -0.00150 0.00145 C4 1 0.255201 0.326413 0.055883 11.00000 0.03234 0.03254 = 0.03596 -0.00079 0.00612 -0.00147 C5 1 0.196931 0.324049 0.029243 11.00000 0.03765 0.04528 = 0.02737 0.00617 0.00696 0.00162 AFIX 43 H5 2 0.206432 0.370907 0.008908 11.00000 -1.20000 AFIX 0 C6 1 0.122754 0.250995 0.032525 11.00000 0.03522 0.04476 = 0.02539 0.00640 0.00362 0.00347 AFIX 43 H6 2 0.081155 0.247780 0.014335 11.00000 -1.20000 AFIX 0 C7 1 0.110441 0.183933 0.062218 11.00000 0.02982 0.03371 = 0.02812 -0.00021 0.00625 0.00143 C8 1 0.170409 0.186285 0.089512 11.00000 0.03513 0.02916 = 0.02479 0.00062 0.00045 0.00334 AFIX 43 H8 2 0.160917 0.139261 0.109836 11.00000 -1.20000 AFIX 0 C9 1 0.031804 0.102892 0.064582 11.00000 0.03039 0.04590 = 0.02675 0.00154 0.00455 0.00363 RESI 3 F1 5 0.523417 0.604919 0.062409 11.00000 0.03713 0.06555 = 0.03384 0.00247 -0.00062 -0.01461 O1 4 0.636072 0.573191 0.119791 11.00000 0.04040 0.03416 = 0.02812 0.00290 0.01216 0.00018 O2 4 0.877498 0.888976 0.091882 11.00000 0.03924 0.05806 = 0.02593 0.00464 0.00330 -0.00254 O3 4 0.843757 0.950070 0.038766 11.00000 0.03971 0.07054 = 0.03100 0.01502 0.00585 -0.01268 AFIX 147 H3O 2 0.890703 0.988647 0.041262 11.00000 -1.50000 AFIX 0 N1 3 0.634823 0.613637 0.188451 11.00000 0.03598 0.03921 = 0.02871 0.00423 0.00799 0.00277 AFIX 137 H1A 2 0.636150 0.566045 0.208671 11.00000 -1.50000 H1B 2 0.626218 0.728911 0.189636 11.00000 -1.50000 H1C 2 0.682343 0.594623 0.181170 11.00000 -1.50000 AFIX 0 C1 1 0.569370 0.534477 0.165482 11.00000 0.04169 0.03732 = 0.03093 0.00338 0.01287 -0.00803 AFIX 23 H1D 2 0.518074 0.551313 0.173954 11.00000 -1.20000 H1E 2 0.578997 0.409152 0.164233 11.00000 -1.20000 AFIX 0 C2 1 0.563069 0.610615 0.131775 11.00000 0.03411 0.04433 = 0.03450 0.00177 0.00575 -0.00176 AFIX 23 H2A 2 0.517264 0.559582 0.117215 11.00000 -1.20000 H2B 2 0.554924 0.736588 0.132661 11.00000 -1.20000 AFIX 0 C3 1 0.651699 0.659364 0.092516 11.00000 0.03641 0.02840 = 0.02117 -0.00122 0.00714 0.00056 C4 1 0.597714 0.673863 0.063567 11.00000 0.03026 0.03982 = 0.03051 -0.00157 0.00358 -0.00360 C5 1 0.616754 0.753390 0.036092 11.00000 0.03617 0.05206 = 0.02791 0.00589 0.00043 0.00190 AFIX 43 H5 2 0.578267 0.761502 0.016895 11.00000 -1.20000 AFIX 0 C6 1 0.692609 0.821819 0.036570 11.00000 0.03915 0.04040 = 0.02189 0.00665 0.00707 0.00368 AFIX 43 H6 2 0.706626 0.876960 0.017673 11.00000 -1.20000 AFIX 0 C7 1 0.748174 0.809169 0.064965 11.00000 0.03381 0.02602 = 0.02495 0.00174 0.00528 0.00200 C8 1 0.727405 0.727214 0.092640 11.00000 0.03449 0.03252 = 0.01915 -0.00079 0.00531 0.00292 AFIX 43 H8 2 0.765855 0.717958 0.111828 11.00000 -1.20000 AFIX 0 C9 1 0.828905 0.885982 0.065995 11.00000 0.03498 0.03409 = 0.02453 0.00237 0.00732 0.00422 RESI 4 F1 5 0.817214 0.389820 0.055944 11.00000 0.02881 0.04857 = 0.03967 0.00571 0.00650 -0.01108 O1 4 0.792706 0.264958 0.112431 11.00000 0.02530 0.03857 = 0.03059 0.00675 -0.00095 -0.00885 O2 4 0.503546 0.030984 0.089127 11.00000 0.03135 0.04979 = 0.02544 0.00585 0.00389 -0.00807 O3 4 0.470458 0.094608 0.036180 11.00000 0.03000 0.06997 = 0.02920 0.00843 -0.00253 -0.01736 AFIX 147 H3O 2 0.429715 0.037028 0.038670 11.00000 -1.50000 AFIX 0 N1 3 0.877903 0.071460 0.190843 11.00000 0.03965 0.03167 = 0.03165 0.00400 -0.00152 0.00319 AFIX 137 H1A 2 0.848071 0.120201 0.205040 11.00000 -1.50000 H1B 2 0.929953 0.065846 0.200378 11.00000 -1.50000 H1C 2 0.859465 -0.036551 0.185629 11.00000 -1.50000 AFIX 0 C1 1 0.871712 0.177713 0.160514 11.00000 0.03047 0.02701 = 0.03537 0.00192 -0.00056 -0.00003 AFIX 23 H1D 2 0.909866 0.134280 0.146393 11.00000 -1.20000 H1E 2 0.886042 0.298412 0.166403 11.00000 -1.20000 AFIX 0 C2 1 0.786930 0.170954 0.141783 11.00000 0.02870 0.03736 = 0.02443 0.00160 0.00275 -0.00044 AFIX 23 H2A 2 0.770014 0.050712 0.136775 11.00000 -1.20000 H2B 2 0.748415 0.225983 0.154449 11.00000 -1.20000 AFIX 0 C3 1 0.729887 0.253629 0.087766 11.00000 0.02589 0.02492 = 0.02693 -0.00008 0.00097 -0.00026 C4 1 0.655384 0.182668 0.089603 11.00000 0.02469 0.02736 = 0.02387 -0.00066 0.00361 -0.00097 AFIX 43 H4 2 0.643741 0.135469 0.109603 11.00000 -1.20000 AFIX 0 C5 1 0.597758 0.181581 0.061655 11.00000 0.02397 0.03228 = 0.02518 -0.00224 0.00531 -0.00275 C6 1 0.612608 0.250600 0.032342 11.00000 0.02880 0.03930 = 0.02598 0.00138 0.00224 -0.00396 AFIX 43 H6 2 0.572180 0.249023 0.013719 11.00000 -1.20000 AFIX 0 C7 1 0.687725 0.323166 0.030158 11.00000 0.03448 0.04086 = 0.02269 0.00257 0.00825 -0.00457 AFIX 43 H7 2 0.699240 0.371176 0.010204 11.00000 -1.20000 AFIX 0 C8 1 0.743666 0.322504 0.057627 11.00000 0.02500 0.03210 = 0.03237 -0.00112 0.00862 -0.00713 C9 1 0.518967 0.097200 0.063118 11.00000 0.02618 0.03383 = 0.02471 0.00063 0.00405 -0.00091 RESI 0 HKLF 4 REM FB_0m_a.res in P2(1)/c REM wR2 = 0.0822, GooF = S = 1.100, Restrained GooF = 1.100 for all data REM R1 = 0.0361 for 11994 Fo > 4sig(Fo) and 0.0412 for all 13319 data REM 618 parameters refined using 7 restraints END WGHT 0.0122 52.5106 REM Instructions for potential hydrogen bonds HTAB_4 O2_1 O2_$1 HTAB O4_1 F1_1 HTAB O4_1 O1_1 HTAB_4 O4_1 F1_$7 HTAB_4 O4_1 O1_$7 HTAB N1_1 O4_1 HTAB N1_1 Br3_$1 HTAB N1_1 Br1_$4 HTAB C1_1 Br3 HTAB C2_1 Br3_$1 HTAB C2_1 Br7 HTAB_2 C5_1 O3_$8 HTAB C8_1 Br7 HTAB_3 O2_2 O2_$9 HTAB N1_2 Br2 HTAB N1_2 Br8_$6 HTAB N1_2 Br7_$5 HTAB C1_2 Br7 HTAB_2 O3_3 O3_$10 HTAB N1_3 Br2_$3 HTAB N1_3 Br6_$6 HTAB N1_3 Br8_$3 HTAB N1_3 Br4_$3 HTAB C1_3 Br6_$6 HTAB C1_3 Br7 HTAB C1_3 Br8_$6 HTAB C2_3 F1_3 HTAB C2_3 Br8_$3 HTAB_4 C5_3 O3_$11 HTAB C8_3 Br4_$3 HTAB_1 O3_4 O3_$5 HTAB N1_4 Br5_$6 HTAB N1_4 Br1_$12 HTAB N1_4 Br3_$12 HTAB N1_4 Br4_$6 HTAB C1_4 Br3_$12 HTAB C1_4 Br4_$3 REM Highest difference peak 3.581, deepest hole -2.306, 1-sigma level 0.156 Q1 1 0.1216 0.1103 0.2618 11.00000 0.05 3.58 Q2 1 0.3159 0.6619 0.1800 11.00000 0.05 3.44 Q3 1 0.3575 0.6015 0.2604 11.00000 0.05 3.25 Q4 1 0.1246 0.1788 0.3258 11.00000 0.05 2.74 Q5 1 0.1255 0.0355 0.1786 11.00000 0.05 1.71 Q6 1 0.2768 0.2766 0.2525 11.00000 0.05 1.56 Q7 1 0.1033 0.0796 0.1964 11.00000 0.05 1.39 Q8 1 0.3874 0.5935 0.2822 11.00000 0.05 1.28 Q9 1 0.2106 0.7832 0.2717 11.00000 0.05 1.27 Q10 1 -0.1231 -0.0538 0.2526 11.00000 0.05 1.20 Q11 1 -0.0481 -0.0672 0.2577 11.00000 0.05 1.14 Q12 1 0.1299 0.6132 0.1876 11.00000 0.05 1.08 Q13 1 0.4416 0.5333 0.3205 11.00000 0.05 1.07 Q14 1 0.1451 0.0970 0.2869 11.00000 0.05 1.02 Q15 1 0.3737 0.9512 0.2476 11.00000 0.05 0.98 Q16 1 0.2075 0.7401 0.2480 11.00000 0.05 0.92 Q17 1 0.0520 0.6060 0.1287 11.00000 0.05 0.89 Q18 1 0.6210 0.5386 0.1690 11.00000 0.05 0.85 Q19 1 0.1265 0.6574 0.2489 11.00000 0.05 0.75 Q20 1 0.3827 0.1553 0.2473 11.00000 0.05 0.75 ; _shelx_res_checksum 50522 _shelx_hkl_file ; -2 0 0 68.7123 4.42925 3 2 0 0 72.6239 4.40521 2 -2 0 0 62.4988 4.57217 1 -2 0 0 104.564 4.56813 2 -2 0 0 63.6965 4.37867 3 -3 0 0 29.7701 1.98722 3 -3 0 0 25.6721 1.89496 2 4 0 0 2388.40 134.531 3 4 0 0 2418.79 134.486 2 4 0 0 1330.88 134.391 2 -4 0 0 2455.38 134.570 3 4 0 0 2616.73 134.960 1 4 0 0 2387.49 134.488 3 -4 0 0 2350.32 134.510 2 -4 0 0 2418.58 134.483 3 -4 0 0 2398.80 134.499 2 -4 0 0 2455.25 134.927 1 5 0 0 102.518 5.99122 3 5 0 0 77.9717 5.94248 2 5 0 0 96.3217 6.57144 1 5 0 0 100.017 5.97010 2 -5 0 0 100.249 6.01907 2 -5 0 0 96.3098 5.92515 3 -5 0 0 101.363 6.08517 3 -5 0 0 95.4510 6.57964 1 -6 0 0 476.125 27.6836 3 6 0 0 461.049 27.6293 3 6 0 0 395.277 27.5611 2 -6 0 0 492.739 28.2686 1 6 0 0 484.424 27.5915 3 -6 0 0 464.760 27.6170 2 -6 0 0 482.281 27.6086 2 6 0 0 488.184 28.2463 1 -6 0 0 479.587 27.5688 3 6 0 0 479.547 27.5769 2 7 0 0 32.6486 3.90394 1 7 0 0 35.6991 2.97328 2 -7 0 0 37.7720 2.87229 3 7 0 0 38.0276 2.99636 3 7 0 0 40.4784 2.97221 3 -7 0 0 34.1267 2.98680 2 7 0 0 38.2245 2.98361 2 -7 0 0 36.2663 3.06838 3 -7 0 0 38.1911 3.07657 2 -7 0 0 39.1538 4.06018 1 8 0 0 2983.09 172.030 3 -8 0 0 3055.54 172.846 1 8 0 0 3040.59 172.837 1 -8 0 0 2930.11 171.977 3 -8 0 0 2879.07 172.084 3 8 0 0 2946.30 172.068 2 -8 0 0 2904.51 172.006 2 8 0 0 3041.23 171.972 2 -8 0 0 2944.12 172.053 2 8 0 0 2937.59 172.061 3 9 0 0 46.0615 3.73087 3 -9 0 0 49.0920 3.88194 3 9 0 0 48.2474 5.02002 1 9 0 0 46.6161 3.75588 2 -9 0 0 47.4185 3.91538 2 -9 0 0 44.4658 3.81903 2 9 0 0 48.1853 3.72955 3 10 0 0 10.6623 2.78449 1 10 0 0 17.5942 2.23649 3 -10 0 0 17.9452 2.21269 3 10 0 0 15.8541 2.22861 2 10 0 0 18.4665 2.14167 3 10 0 0 14.9020 2.67211 1 -10 0 0 14.6552 2.05440 2 -10 0 0 15.2638 2.10327 2 -11 0 0 104.959 7.35791 2 11 0 0 116.184 8.74147 1 11 0 0 109.608 7.31733 3 11 0 0 108.399 8.57850 1 -11 0 0 109.264 7.41743 2 11 0 0 112.498 7.33211 3 11 0 0 105.459 7.32360 2 -11 0 0 108.883 7.45497 3 -12 0 0 602.434 37.2708 2 -12 0 0 632.118 37.4385 3 12 0 0 648.036 38.3823 1 12 0 0 614.622 37.2970 3 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2 3 411.256 24.4697 2 0 2 3 420.244 24.7359 1 0 2 -3 427.543 24.5509 1 0 2 3 424.444 24.4637 2 0 2 -3 420.164 24.3695 2 -1 -2 -3 1.71932 0.51905 2 -1 -2 -3 0.99203 0.51825 3 -1 -2 -3 1.14991 0.54694 2 -1 -2 -3 0.44784 0.17811 3 -1 -2 -3 1.03264 0.81944 1 1 2 3 1.23012 0.88658 1 1 2 3 1.76075 0.53791 3 1 2 3 1.02930 0.51143 2 -1 2 -3 0.98931 0.31345 1 -1 2 -3 1.31883 0.37141 1 1 2 3 0.31576 0.53792 2 1 2 3 0.27358 0.49057 3 -2 -2 -3 1943.99 113.386 2 -2 -2 -3 1993.67 113.393 3 -2 -2 -3 1974.17 113.796 1 -2 -2 -3 1811.34 113.546 3 2 2 3 1998.52 113.416 3 2 2 3 1927.85 113.375 3 2 2 3 2038.96 113.817 1 2 2 3 1968.09 113.408 2 2 2 3 1954.15 113.399 2 -3 -2 -3 31.6967 2.35427 2 -3 -2 -3 32.7506 2.40188 3 -3 -2 -3 31.4929 2.42062 3 -3 -2 -3 29.1270 3.00724 1 3 -2 3 30.5357 2.14089 1 3 -2 3 34.9106 2.32244 1 -3 2 -3 30.1719 1.96776 2 -3 2 -3 32.9480 2.01391 2 3 2 3 33.1867 2.34020 3 3 2 3 34.9015 2.47172 3 3 2 3 34.8633 2.44858 2 3 2 3 33.4199 3.07606 1 3 2 3 32.3756 2.42375 2 -4 -2 -3 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4 431.625 25.8273 2 -4 2 4 424.631 26.1675 1 4 2 -4 424.425 25.9501 2 4 2 -4 432.244 25.9344 3 -4 2 4 463.723 25.7062 3 -4 2 4 476.429 25.6903 3 3 -2 -4 12.7779 1.19042 3 -3 -2 4 11.4553 1.29755 2 -3 -2 4 11.0709 1.36380 3 3 -2 -4 10.9502 1.09984 2 3 -2 -4 11.3812 1.11365 2 3 -2 -4 12.2112 1.14605 3 3 -2 -4 6.93191 1.36901 1 3 2 -4 12.0012 1.36207 3 -3 2 4 11.4131 0.94080 3 3 2 -4 12.4287 1.24403 3 3 2 -4 7.91118 1.16203 2 -3 2 4 10.8925 0.89052 3 3 2 -4 11.7932 1.45232 2 -3 2 4 12.9518 1.23463 2 -3 2 4 7.36731 1.29650 1 3 2 -4 7.08276 1.61853 1 -3 2 4 10.9270 1.25656 2 2 -2 -4 1360.50 75.9695 2 -2 -2 4 1178.10 76.3800 1 2 -2 -4 1368.72 75.9626 2 2 -2 -4 1364.25 75.9728 3 -2 -2 4 1303.55 76.0201 3 -2 -2 4 1353.60 76.0511 2 2 -2 -4 1346.54 76.3561 1 -2 -2 4 781.343 75.9568 3 -2 -2 4 1299.19 76.0171 2 2 -2 -4 1358.75 75.9862 3 2 2 -4 1311.64 76.0001 3 -2 2 4 1408.11 76.0209 2 -2 2 4 1340.38 75.9169 3 -2 2 4 1366.56 76.3293 1 2 2 -4 1337.51 76.0878 2 -2 2 4 1363.60 76.0130 2 -2 2 4 1409.62 75.9140 3 2 2 -4 1267.54 75.9772 3 2 2 -4 1391.83 76.5229 1 -1 -2 4 10.3102 0.88651 2 -1 -2 4 9.39783 0.90963 3 1 -2 -4 10.4391 0.96600 2 1 -2 -4 10.7342 1.02134 3 1 -2 -4 9.59399 0.96383 3 1 -2 -4 8.59202 0.97609 2 -1 -2 4 10.3977 0.94023 2 -1 -2 4 8.31545 0.95299 3 -1 -2 4 6.30246 1.19109 1 1 -2 -4 7.01765 1.14927 1 -1 2 4 9.07323 0.89311 3 1 2 -4 6.24546 1.23569 1 1 2 -4 9.49666 0.74221 3 -1 2 4 8.52046 1.29736 1 -1 2 4 10.2837 1.09199 2 1 2 -4 10.4974 0.75828 3 -1 2 4 10.0236 0.87699 3 1 2 -4 10.6662 1.11850 2 1 2 -4 8.99142 0.98521 2 -1 2 4 9.33395 1.03132 2 0 -2 4 12.4657 0.86000 3 0 -2 -4 13.7367 1.25220 3 0 -2 -4 10.0926 1.05964 3 0 -2 4 12.6743 1.35518 1 0 -2 -4 13.9993 1.21892 2 0 -2 4 12.7692 0.88057 3 0 -2 -4 12.4760 1.20829 2 0 -2 -4 12.3366 1.67060 1 0 2 4 12.4080 1.20875 2 0 2 4 12.5186 1.23390 2 0 2 -4 13.2016 1.01355 2 0 2 4 13.2968 1.10397 3 0 2 4 13.6683 1.14291 3 0 2 -4 12.4005 0.98158 2 0 2 -4 14.3946 1.46406 1 0 2 4 12.7903 1.66125 1 -1 -2 -4 51.1766 3.23829 2 -1 -2 -4 46.4151 3.67375 1 -1 -2 -4 49.8877 3.23801 3 -1 2 -4 52.0472 3.08464 1 1 2 4 47.7948 3.67658 1 1 2 4 50.5170 3.26274 2 1 2 4 49.8506 3.24986 3 1 2 4 53.9850 3.24569 3 1 2 4 51.1540 3.27950 2 -2 -2 -4 2014.84 117.770 2 -2 -2 -4 2007.93 117.793 3 -2 -2 -4 2092.44 118.213 1 -2 -2 -4 2005.15 117.779 3 2 2 4 2104.50 118.209 1 2 2 4 2048.61 117.796 3 2 2 4 1956.62 117.750 3 2 2 4 2042.90 117.789 2 2 2 4 2019.32 117.781 2 3 -2 4 0.18306 0.47675 1 -3 -2 -4 1.22074 1.20147 1 3 -2 4 1.12083 0.65942 1 -3 -2 -4 0.68392 0.70174 3 -3 -2 -4 0.53946 0.72235 3 -3 -2 -4 0.43093 0.59047 2 3 2 4 2.32610 1.15794 1 3 2 4 -0.6290 0.69289 2 3 2 4 -0.0149 0.61447 3 -3 2 -4 0.89351 0.33812 2 3 2 4 -0.1894 0.68870 2 3 2 4 0.76605 0.72955 3 -3 2 -4 0.32226 0.37509 2 4 -2 4 501.393 28.6389 3 4 -2 4 475.275 28.6786 3 4 -2 4 506.750 28.9673 1 -4 -2 -4 475.693 28.9022 2 -4 -2 -4 496.005 28.9141 3 -4 -2 -4 494.212 29.5027 1 -4 -2 -4 496.961 28.9638 2 4 -2 4 508.840 28.8710 1 -4 -2 -4 492.433 28.9409 3 4 2 4 501.105 28.9367 2 4 2 4 499.192 28.9469 2 4 2 4 504.678 29.5221 1 -4 2 -4 489.423 28.7168 2 4 2 4 477.041 28.8946 3 -4 2 -4 490.768 28.6759 2 4 2 4 488.548 28.9395 3 -5 -2 -4 7.12172 1.13064 2 -5 -2 -4 6.63315 1.24455 2 -5 -2 -4 5.32679 1.75504 1 5 -2 4 8.03242 0.92549 2 5 -2 4 6.55545 1.38102 1 5 -2 4 5.53245 1.13176 1 -5 -2 -4 5.50229 1.15140 3 5 -2 4 8.45365 0.74928 2 5 -2 4 6.70565 0.93107 3 5 -2 4 6.03324 0.76937 3 -5 -2 -4 5.25237 1.12961 3 5 2 4 8.97743 1.59715 2 -5 2 -4 5.72392 0.85320 2 5 2 4 4.16788 1.09759 2 5 2 4 7.07024 1.11559 3 -5 2 -4 6.68010 0.93946 2 5 2 4 7.12886 1.77494 1 5 2 4 6.76784 1.19453 3 6 -2 4 120.345 7.33367 3 6 -2 4 120.251 7.83947 1 6 -2 4 127.805 7.71245 1 -6 -2 -4 114.877 7.52078 3 6 -2 4 117.248 7.19291 3 -6 -2 -4 119.021 7.58990 2 -6 -2 -4 122.067 7.54130 3 -6 -2 -4 113.176 7.45981 2 6 -2 4 116.668 7.30001 2 6 -2 4 121.134 7.10784 2 6 2 4 120.846 7.53497 2 6 2 4 118.984 8.37599 1 -6 2 -4 120.592 7.30233 2 -6 2 -4 120.444 7.26250 2 6 2 4 117.195 7.56421 3 6 2 4 115.112 7.46483 3 6 2 4 122.610 7.56436 2 -7 -2 -4 47.7185 3.80866 2 7 -2 4 48.7209 3.38285 3 7 -2 4 44.6201 3.23916 3 7 -2 4 43.4241 3.88382 1 -7 -2 -4 51.5265 3.74132 3 7 -2 4 49.4319 3.46492 2 -7 -2 -4 46.5142 3.65207 3 -7 -2 -4 47.8145 3.61224 2 7 -2 4 47.2577 4.17004 1 7 2 4 43.6462 3.53575 3 7 2 4 46.9716 4.71325 1 -7 2 -4 45.0627 2.92900 3 7 2 4 49.6187 4.91587 1 -7 2 -4 47.1494 3.34864 2 -7 2 -4 42.8542 3.08001 3 7 2 4 49.2210 3.74901 2 7 2 4 60.6486 4.25754 2 7 2 4 48.0825 3.70528 3 -8 -2 -4 21.7518 2.58072 3 -8 -2 -4 14.8688 1.95955 2 8 -2 4 23.5808 2.27108 3 8 -2 4 22.0967 2.84489 1 8 -2 4 20.7589 2.13181 3 -8 -2 -4 22.3947 2.58515 3 -8 -2 -4 21.9558 2.51323 2 8 -2 4 20.3280 2.54366 1 8 -2 4 18.4860 2.30120 2 8 2 4 17.8287 3.05296 1 8 2 4 19.3562 2.17758 2 -8 2 -4 25.8535 2.25504 3 8 2 4 19.3383 2.38012 3 8 2 4 23.7382 3.41088 1 8 2 4 21.5851 2.64846 2 -8 2 -4 21.8104 2.31499 2 8 2 4 26.0443 2.71461 3 -8 2 -4 18.2116 2.26309 2 9 -2 4 2.21659 1.17096 3 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4.71699 3 11 -2 4 54.7708 6.02166 1 -11 2 -4 57.2688 4.77888 3 -11 2 -4 60.1116 4.82619 2 11 2 4 64.0160 5.03532 2 11 2 4 69.3481 5.09949 3 11 2 4 63.6052 6.69416 1 -11 2 -4 62.5541 4.72960 2 11 2 4 60.9610 6.48665 1 12 -2 4 73.5638 6.87374 1 -12 -2 -4 75.6501 5.77968 2 12 -2 4 40.9346 4.66829 3 12 -2 4 72.5099 5.21089 3 -12 -2 -4 74.9393 5.50876 3 12 -2 4 66.8130 5.18718 2 12 -2 4 78.4597 6.31871 1 12 2 4 75.8290 7.36919 1 12 2 4 79.0052 5.58475 2 12 2 4 71.8250 5.52647 3 -12 2 -4 69.7572 5.24648 2 12 2 4 76.9577 7.17535 1 -12 2 -4 67.8599 5.39054 3 -12 2 -4 69.2940 5.38591 2 -13 -2 -4 -1.2965 2.01547 2 13 -2 4 0.02731 1.58682 3 13 -2 4 0.86344 1.51284 2 -13 -2 -4 2.16358 1.84465 3 13 -2 4 1.33794 2.75878 1 13 -2 4 -0.3918 2.20018 1 13 2 4 2.59659 1.84616 2 13 2 4 0.20709 1.84782 3 13 2 4 -0.8494 2.61997 1 13 2 4 -0.2736 2.73724 1 -13 2 -4 1.64338 1.88600 2 -13 2 -4 -0.8098 1.52572 3 -13 2 -4 0.71810 1.53392 2 -14 -2 -4 10.5154 2.50457 2 14 -2 4 6.57514 3.16245 1 14 -2 4 9.41925 2.02848 2 14 -2 4 9.69812 2.90680 1 -14 -2 -4 8.51530 2.31320 3 14 -2 4 8.49607 2.06147 3 -14 2 -4 7.54815 1.92775 3 14 2 4 9.69529 2.30493 3 14 2 4 9.88299 3.69753 1 14 2 4 10.2191 2.40277 2 14 2 4 6.15866 3.16524 1 -14 2 -4 8.34742 2.28704 2 -14 2 -4 7.11864 1.93167 2 15 -2 4 3.00909 1.74894 3 15 -2 4 4.92403 3.28567 1 -15 -2 -4 5.61004 2.22959 3 15 -2 4 5.71859 1.83887 2 15 -2 4 1.66977 2.59203 1 -15 -2 -4 6.19595 2.46193 2 15 -2 4 3.60920 1.96324 3 -15 2 -4 3.19590 1.88257 3 15 2 4 6.72861 2.36817 3 -15 2 -4 3.49252 1.82339 2 -15 2 -4 4.88019 2.21162 2 15 2 4 4.21869 2.14648 2 15 2 4 10.3029 3.89281 1 15 2 4 7.03759 3.48268 1 -16 -2 -4 73.2656 6.33301 3 16 -2 4 80.0577 7.53566 1 16 -2 4 77.6617 6.13316 3 16 -2 4 86.7669 8.37088 1 16 -2 4 78.0065 6.06104 2 -16 -2 -4 77.3937 6.70633 2 16 -2 4 79.3505 5.93886 3 -16 2 -4 77.3692 5.99878 2 16 2 4 70.8972 6.27312 3 -16 2 -4 77.6305 6.42023 2 16 2 4 82.7366 6.40208 2 16 2 4 87.1720 8.63458 1 16 2 4 72.8408 8.60229 1 -17 -2 -4 27.0149 3.42682 3 17 -2 4 29.8538 3.22403 3 -17 -2 -4 23.9747 3.56429 2 17 -2 4 31.2285 3.66133 3 17 -2 4 26.1037 6.96332 1 17 -2 4 21.6056 4.13762 1 17 -2 4 24.5076 3.11355 2 17 2 4 26.7603 5.38936 1 17 2 4 20.2002 4.90793 1 17 2 4 27.6546 3.34559 3 17 2 4 33.8482 4.11187 2 -17 2 -4 24.2234 3.02313 2 -17 2 -4 22.9749 3.28071 2 -18 -2 -4 63.3558 5.98988 3 18 -2 4 69.7597 5.78438 3 18 -2 4 78.8937 7.73328 1 18 -2 4 67.5082 5.52486 3 -18 -2 -4 64.3317 6.43610 2 -18 2 -4 62.3007 5.73096 2 18 2 4 72.4049 8.70752 1 18 2 4 64.6291 5.93914 2 18 2 4 67.7969 6.03053 3 -18 2 -4 63.6747 6.18443 2 18 2 4 65.3684 8.54152 1 19 -2 4 8.29396 2.64117 3 -19 -2 -4 9.81676 2.75405 3 19 -2 4 11.1734 4.06803 1 -19 -2 -4 11.2118 3.03472 2 19 2 4 7.29635 4.31732 1 19 2 4 8.72288 2.73926 3 -19 2 -4 14.9743 3.20782 2 19 2 4 11.9076 2.68612 2 19 2 4 7.12504 4.75562 1 20 -2 4 5.80574 6.61905 1 -20 -2 -4 1.47203 2.96284 2 20 -2 4 6.60026 2.59620 3 -20 -2 -4 9.79621 2.72895 3 -20 2 -4 8.34474 2.98031 2 20 2 4 8.12427 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2.13752 2.70078 2 -20 3 4 0.83893 2.60033 2 19 -3 -4 4.91098 2.49529 3 19 -3 -4 10.1248 3.91026 1 -19 -3 4 5.12513 2.66684 3 -19 -3 4 5.23898 2.90253 2 19 3 -4 5.29745 2.53659 3 -19 3 4 5.54357 2.62335 2 19 3 -4 3.83226 2.68517 2 19 3 -4 10.9143 4.87429 1 19 3 -4 0.90175 4.68228 1 -18 -3 4 221.375 14.0064 3 18 -3 -4 220.594 13.5638 3 18 -3 -4 213.419 13.5127 3 18 -3 -4 217.958 15.0233 1 -18 -3 4 209.588 13.9211 2 18 3 -4 215.118 13.7872 3 18 3 -4 198.317 16.1577 1 -18 3 4 215.820 13.7332 2 18 3 -4 219.933 13.9751 2 18 3 -4 196.029 15.9506 1 -18 3 4 193.764 13.3603 2 17 -3 -4 4.66226 2.30027 3 -17 -3 4 2.76650 2.44635 2 17 -3 -4 3.20286 1.96008 3 -17 -3 4 0.35339 2.34732 3 17 -3 -4 -0.2118 3.01993 1 17 3 -4 5.88090 2.67982 2 17 3 -4 3.53747 3.96401 1 -17 3 4 2.87292 1.97708 2 -17 3 4 1.70516 2.39356 2 17 3 -4 0.65398 4.01552 1 17 3 -4 1.81633 2.28778 3 16 -3 -4 135.116 9.52705 2 16 -3 -4 140.425 9.33190 3 -16 -3 4 134.430 9.74580 2 -16 -3 4 144.136 9.81833 3 16 -3 -4 135.135 11.1982 1 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236.819 14.2457 1 -1 1 -12 242.171 13.7454 2 1 1 12 240.516 14.4509 1 1 1 12 245.492 13.8661 2 -1 1 -12 251.118 13.8830 2 1 1 12 236.341 13.8522 2 -1 1 -12 234.081 13.9220 3 -1 1 -12 235.502 13.6560 3 1 1 12 230.172 13.8599 3 1 1 12 251.551 13.8490 3 -2 -1 -12 1868.43 110.410 3 2 -1 12 1975.18 110.421 3 -2 -1 -12 2582.38 110.756 2 2 -1 12 1568.06 110.694 1 2 -1 12 2019.81 110.298 2 2 -1 12 919.883 110.156 3 -2 -1 -12 1937.84 110.416 3 -2 -1 -12 1914.20 110.408 2 -2 -1 -12 1847.30 110.953 1 2 -1 12 1984.29 110.429 2 -2 1 -12 1926.89 110.315 2 2 1 12 1978.73 110.435 2 -2 1 -12 1991.75 110.399 2 -2 1 -12 1932.76 110.527 3 2 1 12 1994.13 110.480 3 -2 1 -12 1942.05 110.259 3 2 1 12 1921.39 110.419 2 2 1 12 1912.03 110.411 3 -2 1 -12 1955.29 110.758 1 -3 -1 -12 18.1110 1.93173 2 3 -1 12 13.9939 1.47485 2 3 -1 12 16.4185 1.71238 3 -3 -1 -12 15.5481 1.78040 3 3 -1 12 8.86098 1.22729 3 3 -1 12 14.0399 1.62335 2 -3 -1 -12 16.5091 1.79768 3 -3 -1 -12 8.56853 1.91523 1 -3 -1 -12 15.0749 1.67700 2 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36.4638 4.22971 3 -10 -2 21 40.0058 5.50352 1 10 -2 -21 39.9228 5.35979 1 -10 -2 21 40.5047 4.58668 3 10 -2 -21 43.6982 4.64556 2 10 -2 -21 46.6607 4.19011 3 -10 -2 21 44.7221 4.12397 2 -10 -2 21 36.4163 3.87869 3 10 2 -21 41.0737 5.54760 1 10 2 -21 43.8635 4.62470 2 -10 2 21 42.5550 4.25457 2 10 2 -21 37.5123 3.99705 2 -10 2 21 28.4444 4.63806 1 -10 2 21 36.3054 3.90997 2 -10 2 21 38.0611 4.34960 3 10 2 -21 40.0274 3.93041 3 -9 -2 21 50.4344 4.10680 3 9 -2 -21 36.3348 5.14147 1 9 -2 -21 43.1196 4.77422 2 -9 -2 21 44.3276 4.25398 2 9 -2 -21 46.7185 4.44205 3 -9 -2 21 47.2997 6.48787 1 9 -2 -21 43.0969 4.18272 3 -9 -2 21 58.9012 4.96425 3 -9 2 21 43.3722 5.89137 1 9 2 -21 43.9627 4.17926 2 9 2 -21 38.7311 5.28716 1 9 2 -21 45.1019 4.03708 3 -9 2 21 41.4782 4.26695 2 -9 2 21 44.5780 4.32606 2 9 2 -21 45.9536 4.78519 2 -9 2 21 43.1664 4.89896 3 8 -2 -21 744.187 45.2978 1 8 -2 -21 740.980 44.1837 3 -8 -2 21 741.157 43.9136 2 -8 -2 21 746.967 43.9411 3 -8 -2 21 736.455 44.1985 3 8 -2 -21 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223.437 13.9827 2 0 -4 -21 242.221 15.4346 1 0 4 21 222.997 13.9440 3 0 4 -21 228.860 13.6831 2 0 4 21 222.518 13.8698 2 0 4 21 217.644 15.1353 1 0 4 -21 224.901 13.7165 2 0 4 -21 225.045 14.3324 1 0 4 21 231.738 14.0271 2 -1 -4 -21 203.339 12.5241 3 1 -4 21 191.525 13.2883 1 1 -4 21 199.414 12.3109 3 1 -4 21 206.316 12.2302 3 -1 -4 -21 197.139 12.6259 3 -1 -4 -21 206.823 12.6912 2 -1 -4 -21 209.203 14.0296 1 1 4 21 207.211 12.6240 3 1 4 21 203.676 12.6958 2 -1 4 -21 195.289 12.8813 1 -1 4 -21 202.020 12.3171 2 1 4 21 203.303 12.5638 2 1 4 21 204.718 13.8647 1 -1 4 -21 193.524 12.3050 2 2 -4 21 237.438 14.5340 3 2 -4 21 238.897 14.6445 3 -2 -4 -21 237.045 14.8900 3 -2 -4 -21 251.230 16.3549 1 -2 -4 -21 245.114 15.0234 2 -2 -4 -21 243.353 15.0271 3 2 -4 21 249.224 15.6487 1 2 4 21 250.401 15.0615 2 2 4 21 248.886 14.9975 3 -2 4 -21 244.940 14.6422 2 -2 4 -21 248.054 15.1050 1 -2 4 -21 236.532 14.7171 2 2 4 21 230.530 14.8840 2 2 4 21 240.959 16.2871 1 -3 -4 -21 15.6514 3.53077 1 3 -4 21 30.6037 3.92668 1 -3 -4 -21 21.8101 2.86829 2 -3 -4 -21 23.0091 2.79772 3 3 -4 21 28.8085 2.45327 3 3 -4 21 27.5061 2.82033 3 -3 -4 -21 26.3115 3.08674 3 3 4 21 20.7087 2.82014 2 3 4 21 26.8263 3.26910 3 -3 4 -21 21.0521 2.74375 1 3 4 21 24.8924 3.10848 2 -3 4 -21 24.4036 2.69741 2 -3 4 -21 27.5643 2.89492 2 3 4 21 18.8473 3.59874 1 -4 -4 -21 279.367 16.6643 3 -4 -4 -21 264.125 16.6129 2 4 -4 21 278.504 16.2422 3 -4 -4 -21 284.778 18.1005 1 4 -4 21 283.067 17.0680 1 4 -4 21 260.289 16.0345 3 -4 -4 -21 253.338 16.4662 3 4 4 21 276.875 17.9086 1 4 4 21 268.465 16.5050 2 4 4 21 275.164 16.6087 3 -4 4 -21 280.467 16.5974 1 4 4 21 270.146 16.6436 2 -4 4 -21 269.831 16.1711 2 -4 4 -21 244.826 16.1915 2 -5 -4 -21 118.876 8.45448 3 -5 -4 -21 122.833 8.75838 2 5 -4 21 128.541 7.92796 3 5 -4 21 130.561 8.13083 3 -5 -4 -21 132.677 8.73771 3 5 -4 21 127.149 9.24517 1 -5 -4 -21 124.264 10.2123 1 -5 4 -21 125.944 8.07317 2 -5 4 -21 131.844 8.21853 2 5 4 21 130.677 8.66722 2 5 4 21 131.268 8.47901 2 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110.949 11.4291 1 14 -5 -21 109.109 8.02584 3 -14 5 21 110.846 8.01467 2 14 5 -21 110.110 7.83630 3 14 5 -21 106.807 8.68071 2 14 5 -21 102.863 10.7629 1 -14 5 21 115.617 8.48207 2 -13 -5 21 32.8228 5.96550 1 -13 -5 21 35.8733 4.03150 2 13 -5 -21 27.7552 3.58130 3 13 -5 -21 30.7892 3.63608 3 -13 -5 21 30.7594 4.04757 3 13 5 -21 31.9307 3.73133 3 13 5 -21 31.2651 3.92945 2 -13 5 21 30.8401 3.93699 2 -13 5 21 33.6167 3.83118 2 13 5 -21 35.1340 4.51108 2 13 5 -21 30.9043 5.36827 1 -12 -5 21 39.5579 4.26831 3 -12 -5 21 38.4474 5.76706 1 12 -5 -21 36.6384 6.00264 1 12 -5 -21 34.6863 5.03965 2 -12 -5 21 31.3801 3.58167 3 12 -5 -21 34.8645 4.31542 3 12 5 -21 33.7538 5.35195 1 12 5 -21 31.7614 4.08228 2 -12 5 21 36.3059 4.46837 2 -12 5 21 38.1310 5.50001 1 12 5 -21 32.3871 3.78719 3 12 5 -21 35.4953 3.92698 2 -12 5 21 29.3120 3.95565 2 11 -5 -21 179.880 12.7288 2 -11 -5 21 164.916 14.7435 1 11 -5 -21 200.537 12.5800 3 -11 -5 21 189.008 12.5760 3 -11 -5 21 208.556 13.0306 3 -11 -5 21 203.815 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2.04169 3 -8 -5 21 6.36268 2.01677 3 -8 -5 21 9.03695 3.75073 1 -8 -5 21 6.15605 2.43385 3 8 -5 -21 5.57358 3.85263 1 -8 -5 21 6.03697 1.75520 2 -8 5 21 4.16603 2.15750 2 8 5 -21 5.52505 1.54295 3 -8 5 21 4.03356 2.91559 1 8 5 -21 6.50990 2.10637 2 8 5 -21 6.05400 2.35388 2 -8 5 21 6.84790 1.69405 3 8 5 -21 3.54417 3.00085 1 -8 5 21 5.00448 2.02570 2 7 -5 -21 182.829 13.6722 3 -7 -5 21 209.577 12.8254 2 7 -5 -21 223.249 13.1922 3 7 -5 -21 198.011 13.0639 2 -7 -5 21 225.216 13.4381 3 7 -5 -21 202.246 15.0070 1 -7 -5 21 223.815 15.3277 1 -7 -5 21 208.277 13.1011 3 -7 5 21 193.377 12.7899 3 -7 5 21 216.435 13.2558 2 7 5 -21 205.477 12.6708 3 -7 5 21 200.586 13.1728 2 -7 5 21 207.031 14.4630 1 7 5 -21 209.623 13.2857 2 7 5 -21 210.992 14.5020 1 7 5 -21 218.214 13.4328 2 6 -5 -21 876.010 54.5048 3 6 -5 -21 928.955 54.4367 2 -6 -5 21 950.546 54.2153 2 6 -5 -21 951.769 55.9346 1 -6 -5 21 909.096 54.4979 3 -6 -5 21 952.509 56.1688 1 6 -5 -21 927.906 54.4703 3 -6 5 21 955.647 55.6190 1 -6 5 21 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2.41047 2.12796 3 11 -2 -28 4.12202 2.68156 2 -11 -2 28 5.76688 3.94323 1 -11 2 28 6.48303 2.25875 2 -11 2 28 7.81138 2.86058 3 11 2 -28 4.18844 2.02148 3 -11 2 28 2.75570 1.94629 2 11 2 -28 2.44171 3.59279 1 11 2 -28 4.16687 2.51722 2 -11 2 28 5.34353 3.67103 1 -10 -2 28 2.62269 1.86473 2 -10 -2 28 0.64406 3.59675 1 10 -2 -28 5.74866 2.48890 3 10 -2 -28 4.15687 2.72461 2 -10 -2 28 5.60282 2.49910 3 10 -2 -28 7.53981 3.66405 1 10 -2 -28 1.42742 2.14415 3 -10 2 28 3.15987 2.21943 2 -10 2 28 6.54439 2.22917 2 10 2 -28 2.59740 1.86382 3 10 2 -28 3.13726 3.66438 1 -10 2 28 4.78730 2.49295 3 10 2 -28 2.13602 1.99028 2 10 2 -28 3.08602 2.46333 2 -10 2 28 3.58294 3.51082 1 -9 -2 28 144.371 10.0194 3 9 -2 -28 135.768 10.4234 3 -9 -2 28 170.981 10.7928 3 9 -2 -28 156.182 12.3855 1 9 -2 -28 159.082 10.9048 2 9 -2 -28 168.035 10.2899 3 -9 -2 28 154.394 12.5524 1 -9 -2 28 149.110 10.0809 2 9 2 -28 147.700 9.97314 3 -9 2 28 143.635 10.3404 2 -9 2 28 156.134 10.2954 2 -9 2 28 161.990 11.0085 3 9 2 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16.5525 1 8 -6 28 199.248 12.8350 3 -8 -6 -28 210.226 13.7354 3 8 -6 28 200.888 12.7455 3 -8 -6 -28 217.452 13.8361 2 8 6 28 212.628 13.7274 2 8 6 28 196.281 15.7181 1 8 6 28 206.626 13.6238 3 -8 6 -28 210.185 12.7901 2 -8 6 -28 204.386 12.9177 2 9 -6 28 168.589 10.3842 3 -9 -6 -28 139.517 13.6835 1 -9 -6 -28 161.176 11.3524 2 9 -6 28 166.574 10.2116 3 -9 -6 -28 168.308 11.2907 3 -9 6 -28 162.277 10.2885 2 -9 6 -28 157.461 10.3903 2 9 6 28 155.590 14.2354 1 9 6 28 169.621 11.3465 2 9 6 28 163.451 11.1418 3 -10 -6 -28 9.01158 3.10062 2 10 -6 28 8.32293 2.16265 3 -10 -6 -28 6.84097 2.96625 3 10 -6 28 9.61361 1.90432 3 -10 6 -28 8.99641 2.14115 2 10 6 28 8.27879 2.90746 2 10 6 28 5.93253 2.63741 3 -10 6 -28 7.99972 2.08168 2 11 -6 28 1.54685 1.63993 3 11 -6 28 1.50727 2.03261 3 -11 -6 -28 -0.7456 2.54913 3 -11 -6 -28 0.62111 2.78595 2 11 6 28 1.39499 2.89308 3 11 6 28 3.14730 2.56455 2 -11 6 -28 0.34922 1.77148 2 -11 6 -28 1.15085 1.96687 2 12 -6 28 37.4477 3.69302 3 -12 -6 -28 35.3578 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4 -2 -29 334.285 20.1831 2 -4 2 29 350.719 19.9451 2 4 2 -29 339.080 21.0676 1 -4 2 29 338.827 19.9454 2 -4 2 29 349.104 21.4266 1 4 2 -29 331.337 19.9486 2 4 2 -29 333.178 19.6014 3 -4 2 29 348.264 20.2663 3 4 2 -29 328.852 19.8144 2 3 -2 -29 383.082 23.3096 3 -3 -2 29 381.496 23.3865 3 -3 -2 29 371.387 23.1679 3 3 -2 -29 376.743 23.5340 2 -3 -2 29 402.032 24.7231 1 3 -2 -29 383.775 24.9365 1 3 2 -29 392.267 23.0504 3 -3 2 29 393.950 24.8208 1 -3 2 29 379.813 23.3917 2 3 2 -29 376.770 23.3350 2 -3 2 29 394.765 23.3365 2 3 2 -29 407.114 24.5628 1 -3 2 29 388.007 23.5991 3 3 2 -29 374.068 23.1992 2 -2 -2 29 27.1083 2.91352 2 2 -2 -29 24.9418 4.47130 1 2 -2 -29 19.7550 3.04102 2 -2 -2 29 23.8954 2.91015 3 -2 -2 29 24.5830 2.98763 3 -2 -2 29 23.0204 4.11409 1 2 -2 -29 26.7706 3.44458 3 -2 2 29 27.8110 4.44749 1 2 2 -29 24.5387 3.07664 2 -2 2 29 21.4608 2.75763 2 -2 2 29 19.4376 3.06206 2 -2 2 29 27.9144 3.26999 3 2 2 -29 24.6084 4.07119 1 2 2 -29 22.4795 2.70462 3 2 2 -29 22.5888 2.66025 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166.294 10.6422 3 -4 2 -29 178.864 12.2665 1 -4 2 -29 172.228 10.9991 2 4 2 29 176.028 11.2695 2 4 2 29 182.631 12.8518 1 4 2 29 167.235 11.3974 3 -4 2 -29 165.506 11.1706 2 5 -2 29 141.441 9.19233 2 -5 -2 -29 157.743 11.6392 1 5 -2 29 148.984 9.57631 3 -5 -2 -29 147.991 9.97523 2 5 -2 29 138.660 10.6576 1 -5 -2 -29 140.170 9.71155 3 -5 2 -29 139.428 9.36618 2 5 2 29 138.776 9.69502 2 -5 2 -29 146.565 9.04845 3 -5 2 -29 144.045 9.60042 2 5 2 29 153.909 9.90469 3 5 2 29 148.083 11.3741 1 -5 2 -29 148.328 10.8055 1 6 -2 29 26.6629 3.13315 3 6 -2 29 31.0554 4.22244 1 -6 -2 -29 31.4352 5.11622 1 -6 -2 -29 30.1279 3.24550 3 -6 -2 -29 26.3309 3.43229 2 6 -2 29 30.4841 2.95761 2 6 2 29 29.9551 3.79652 2 -6 2 -29 26.5810 3.20419 2 6 2 29 29.4805 3.44600 3 6 2 29 31.4647 4.58862 1 -6 2 -29 27.4518 2.83334 3 -6 2 -29 27.3442 3.22926 2 -6 2 -29 28.1687 3.98642 1 -7 -2 -29 18.7586 2.80249 3 -7 -2 -29 12.6667 4.14655 1 -7 -2 -29 19.4861 3.06275 2 7 -2 29 22.6813 3.89277 1 7 -2 29 16.7439 2.17856 2 7 -2 29 18.1868 2.63948 3 -7 2 -29 18.4242 2.69950 2 7 2 29 21.6303 3.00876 3 -7 2 -29 21.2147 2.54835 2 7 2 29 13.2636 3.93758 1 -7 2 -29 14.1388 3.45555 1 7 2 29 19.3653 2.76450 2 -8 -2 -29 7.44402 2.78302 2 -8 -2 -29 0.38734 1.98911 3 8 -2 29 1.69734 1.52088 2 8 -2 29 2.73942 2.73877 1 -8 -2 -29 1.27269 3.41543 1 8 -2 29 2.93374 2.08818 3 8 2 29 8.37613 3.44785 1 -8 2 -29 6.59866 2.95852 1 8 2 29 2.38243 2.14510 3 -8 2 -29 3.54562 2.17670 2 -8 2 -29 4.42959 1.80694 2 8 2 29 3.72698 2.07493 2 -9 -2 -29 212.503 13.3690 3 -9 -2 -29 200.527 15.2784 1 9 -2 29 193.336 14.3824 1 9 -2 29 218.770 13.0856 2 9 -2 29 217.281 13.2841 3 -9 -2 -29 215.700 13.7326 2 9 -2 29 189.697 13.4212 3 9 2 29 205.387 13.3705 2 9 2 29 209.292 13.5094 3 -9 2 -29 214.546 13.3699 2 -9 2 -29 210.928 13.1294 2 -9 2 -29 211.690 14.4571 1 9 2 29 225.359 15.2288 1 10 -2 29 101.520 8.75410 1 10 -2 29 100.109 7.09333 3 -10 -2 -29 105.447 9.64592 1 10 -2 29 105.687 7.51836 3 10 -2 29 101.849 7.08226 2 -10 -2 -29 106.680 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5.60418 2 7 5 -29 57.6428 6.85476 1 -7 5 29 58.0996 7.28124 1 7 5 -29 59.8112 5.12389 2 -7 5 29 51.3365 5.47280 3 7 5 -29 57.8808 5.65285 2 -7 5 29 55.8540 5.25488 2 -7 5 29 56.6873 5.49771 2 -6 -5 29 65.5819 4.82684 2 -6 -5 29 69.8508 5.76175 3 -6 -5 29 60.8248 8.38147 1 6 -5 -29 59.5459 5.42594 3 -6 -5 29 57.7623 5.03884 3 6 -5 -29 60.5281 5.85938 2 6 -5 -29 59.3267 5.61925 3 6 -5 -29 78.5314 8.20834 1 6 5 -29 53.3188 5.23535 2 6 5 -29 57.8048 6.78724 1 -6 5 29 69.5504 5.89939 2 -6 5 29 67.7155 5.52163 2 6 5 -29 62.1894 5.78300 2 -6 5 29 64.1237 6.93749 1 -6 5 29 57.4434 5.67559 3 5 -5 -29 74.8348 6.27362 3 -5 -5 29 71.3739 5.27179 2 5 -5 -29 64.1220 6.37993 2 -5 -5 29 83.9534 6.15683 3 -5 -5 29 75.2364 8.71179 1 5 -5 -29 74.7040 8.79913 1 5 -5 -29 68.6045 6.03641 3 -5 5 29 65.0514 5.94866 2 5 5 -29 74.3520 6.14994 2 -5 5 29 74.6168 6.25056 2 -5 5 29 70.2498 6.20308 3 -5 5 29 75.0705 7.90805 1 5 5 -29 78.8538 7.23653 1 5 5 -29 76.9010 5.80676 2 -4 -5 29 63.8669 5.05863 3 4 -5 -29 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5 29 45.4533 5.07700 2 1 5 29 45.9138 5.88086 1 1 5 29 51.2471 4.90255 3 -1 5 -29 47.7923 4.97080 1 -2 -5 -29 190.858 12.1025 2 -2 -5 -29 186.219 11.9387 3 2 -5 29 174.435 11.2738 3 2 -5 29 213.198 13.6404 1 2 -5 29 174.977 11.4523 3 -2 -5 -29 185.136 14.1209 1 -2 5 -29 179.849 11.4610 2 2 5 29 179.803 12.0215 2 2 5 29 178.325 11.9179 3 2 5 29 170.491 11.7086 2 -2 5 -29 175.900 11.9491 1 -2 5 -29 176.223 11.5109 2 2 5 29 184.472 13.7291 1 3 -5 29 109.459 8.99913 1 3 -5 29 107.015 7.05653 3 -3 -5 -29 98.9152 9.92816 1 -3 -5 -29 95.4187 7.57135 3 -3 -5 -29 103.562 7.72287 2 3 -5 29 100.715 6.76366 3 -3 5 -29 97.6866 6.99024 2 -3 5 -29 96.0691 6.96700 2 3 5 29 98.7470 9.38820 1 -3 5 -29 94.5722 7.56680 1 3 5 29 99.6818 7.66777 2 3 5 29 105.644 7.57399 3 4 -5 29 11.3096 1.87083 3 4 -5 29 13.1259 3.71784 1 4 -5 29 12.8091 2.16163 3 -4 -5 -29 13.2157 2.96105 3 -4 -5 -29 13.3713 2.86959 2 -4 -5 -29 1.51591 3.87429 1 -4 5 -29 12.9202 2.12308 2 -4 5 -29 12.8070 2.66529 1 4 5 29 13.7123 2.65579 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3.48887 3.78726 2 -9 0 57 2.54170 3.41390 3 8 0 -57 3.58230 3.82816 2 -8 0 57 4.95784 3.32778 3 7 0 -57 1.32047 3.65489 2 -7 0 57 0.24784 3.07618 3 -6 0 57 -0.3107 2.90531 3 6 0 -57 -1.5219 3.34525 2 5 0 -57 3.63030 3.77414 2 -5 0 57 3.13538 2.90246 3 -4 0 57 0.07829 3.09395 3 4 0 -57 -1.5957 3.45888 2 -3 0 57 4.04203 3.08635 3 3 0 -57 5.59047 3.86679 2 2 0 -57 -0.7672 3.48625 2 -2 0 57 3.08300 3.15241 3 -1 0 57 -2.1970 2.96896 3 1 0 -57 0.62748 3.59669 2 0 0 -57 1.10740 3.52801 2 0 0 57 -0.3969 2.90529 3 1 0 57 8.72076 3.49494 3 -1 0 -57 6.41853 3.90833 2 -2 0 -57 -1.6012 3.42662 2 2 0 57 -5.5756 2.78875 3 -9 -1 57 26.7338 4.63633 3 9 -1 -57 35.1966 5.46272 2 -9 1 57 24.0527 4.31337 3 9 1 -57 33.8596 5.13806 2 -8 -1 57 -0.2242 3.23704 3 8 -1 -57 -4.1241 3.42598 2 -8 1 57 1.29415 3.39522 3 8 1 -57 -3.2744 3.28734 2 -7 -1 57 19.7758 4.19098 3 7 -1 -57 21.9247 4.74752 2 7 1 -57 32.7778 5.00399 2 -7 1 57 25.8756 4.73421 3 6 -1 -57 22.2863 4.89727 2 -6 -1 57 25.7093 4.28697 3 -6 1 57 33.8628 4.66272 3 6 1 -57 18.4609 4.60391 2 5 -1 -57 60.1015 7.96865 2 -5 -1 57 80.1950 7.12886 3 -5 1 57 72.6685 7.36285 3 5 1 -57 81.4039 8.10955 2 -4 -1 57 0.27542 2.95251 3 4 -1 -57 4.25759 4.06124 2 -4 1 57 3.71319 3.41457 3 4 1 -57 3.54147 3.64805 2 3 -1 -57 34.4110 5.38457 2 -3 -1 57 45.4160 5.67222 3 -3 1 57 34.6284 4.85642 3 3 1 -57 37.1257 5.29314 2 -2 -1 57 8.35682 3.25994 3 2 -1 -57 10.2828 4.03102 2 2 1 -57 4.14017 3.85620 2 -2 1 57 3.19260 3.32104 3 1 -1 -57 91.5261 8.60085 2 -1 -1 57 90.3421 7.85086 3 1 1 -57 78.5526 8.52338 2 -1 1 57 83.4540 8.44606 3 0 -1 -57 14.2504 4.05998 2 0 -1 57 7.98403 3.19510 3 0 1 -57 9.74712 4.06015 2 0 1 57 12.8139 3.81104 3 -1 -1 -57 35.4998 5.29986 2 1 -1 57 34.1849 4.76336 3 1 1 57 41.6036 5.16666 3 -1 1 -57 41.2100 5.15624 2 2 -1 57 11.0637 3.33800 3 -2 -1 -57 10.4887 4.13162 2 -2 1 -57 4.97944 3.63417 2 2 1 57 9.91814 3.56219 3 7 -2 -57 35.0414 5.24841 2 -7 -2 57 29.5442 4.47963 3 7 2 -57 29.4461 5.06189 2 -7 2 57 28.5207 4.76724 2 -6 -2 57 3.88159 3.25247 3 6 -2 -57 11.0268 4.57875 2 -6 2 57 5.60348 3.36304 3 -6 2 57 10.9237 3.86861 2 6 2 -57 11.7895 4.17928 2 5 -2 -57 33.4364 5.54376 2 -5 -2 57 42.2971 4.98453 3 5 2 -57 36.1821 5.15046 2 -5 2 57 28.1755 4.50545 3 -4 -2 57 49.0152 5.89754 3 4 -2 -57 41.3371 5.45144 2 4 2 -57 46.6089 5.70959 2 -4 2 57 53.7256 5.69606 3 3 -2 -57 80.7648 8.53312 2 -3 -2 57 87.1211 8.06211 3 3 2 -57 91.4714 8.60298 2 -3 2 57 88.7799 8.50089 3 -2 -2 57 4.15984 2.99527 3 2 -2 -57 -1.9696 3.91100 2 2 2 -57 1.20501 3.47860 2 -2 2 57 4.98939 3.40092 3 -1 -2 57 15.6432 3.38750 3 1 -2 -57 17.9792 4.56556 2 -1 2 57 14.8879 3.94052 3 1 2 -57 16.8302 4.22092 2 0 -2 57 2.84291 2.86882 3 0 -2 -57 4.70983 3.97138 2 0 2 -57 -2.7938 3.55648 2 0 2 57 5.25757 3.55337 3 1 -2 57 73.0804 6.95290 3 1 2 57 70.0936 7.45896 3 -7 0 58 97.0451 8.87472 3 7 0 -58 98.0563 9.46231 2 6 0 -58 6.49301 3.82941 2 -6 0 58 4.80836 3.25938 3 -5 0 58 21.0997 4.30062 3 5 0 -58 24.2656 4.79001 2 -4 0 58 4.18518 3.16180 3 4 0 -58 2.35122 3.72238 2 -3 0 58 117.622 9.35867 3 3 0 -58 110.292 9.88692 2 2 0 -58 13.4544 3.99092 2 -2 0 58 3.60538 3.11476 3 1 0 -58 17.0124 4.01460 2 -1 0 58 23.1573 4.27986 3 0 0 -58 23.3169 4.61629 2 0 0 58 28.3431 4.32159 3 -7 -1 58 16.8491 4.16291 3 7 -1 -58 14.5344 4.39104 2 -7 1 58 16.6394 3.88529 3 7 1 -58 18.6541 4.53898 2 6 -1 -58 5.39635 4.00545 2 -6 -1 58 1.01934 2.79178 3 6 1 -58 0.76867 3.97208 2 -6 1 58 5.55939 3.36706 3 5 -1 -58 29.8668 5.14667 2 -5 -1 58 37.2337 4.67897 3 5 1 -58 32.3117 5.03687 2 -5 1 58 35.1417 4.74871 3 -4 -1 58 -1.6300 3.06547 3 4 -1 -58 -0.9296 3.45726 2 -4 1 58 1.45261 3.11261 3 4 1 -58 0.33996 3.67376 2 -3 -1 58 10.0822 3.61117 3 3 -1 -58 14.6013 4.51762 2 3 1 -58 13.1329 4.34337 2 -3 1 58 15.8242 3.94808 3 2 -1 -58 11.0712 4.22010 2 -2 -1 58 17.0026 3.97818 3 2 1 -58 16.5557 4.25399 2 -2 1 58 17.9901 3.90943 3 1 -1 -58 27.0763 4.81560 2 -1 -1 58 29.8245 4.54751 3 1 1 -58 37.0798 5.35872 2 -1 1 58 39.3022 4.87893 3 0 -1 -58 -1.8021 3.58135 2 0 -1 58 4.32282 3.44226 3 0 1 58 1.16570 3.37356 3 0 1 -58 1.08468 3.41685 2 -4 -2 58 3.48731 3.42684 3 -4 2 58 4.33610 3.31169 3 -3 -2 58 17.5162 3.97703 3 -3 2 58 13.1957 4.03991 3 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_max 0.0228 _exptl_absorpt_correction_T_min 0.0041 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71095 16.902 7.771 41.275 89.972 98.440 90.023 ) ; _shelx_hkl_checksum 42954