data_(FCA3)2PbBr4_294K # was data_FB_RT_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. Cooper, R. I, Gould, R. O., Parsons, S. and Watkin, D. J. (2002). The derivation of non-merohedral twin laws during refinement by analysis of poorly fitting intensity data and the refinement of non-merohedrally twinned crystal structures in the program CRYSTALS, J. Appl. Cryst. 35, 168-174. Farrugia, L. J (2012). J Appl. Cryst. 45, 849-854. 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. (2008). CELL_NOW. Version 2008/4. University of G\"ottingen, Germany. 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. Sheldrick, G. M. (2012). TWINABS. Ver. 2012/1. ; _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). ; _audit_creation_method 'SHELXL-2019/3' _shelx_SHELXL_version_number '2019/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Br4 Pb, 2(C9 H11 F N O3), 0.145(H2 O)' _chemical_formula_sum 'C18 H22.29 Br4 F2 N2 O6.15 Pb' _chemical_formula_weight 929.79 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/n' _space_group_name_Hall '-P 2yn' _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+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.373(2) _cell_length_b 7.8455(15) _cell_length_c 41.44(2) _cell_angle_alpha 90 _cell_angle_beta 93.03(2) _cell_angle_gamma 90 _cell_volume 2718.4(16) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 9182 _cell_measurement_theta_min 2.4158 _cell_measurement_theta_max 30.5026 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 2.272 _exptl_crystal_F_000 1733.8 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.312 _exptl_crystal_size_mid 0.149 _exptl_crystal_size_min 0.085 _exptl_absorpt_coefficient_mu 12.134 _shelx_estimated_absorpt_T_min 0.116 _shelx_estimated_absorpt_T_max 0.425 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.141 _exptl_absorpt_correction_T_max 0.695 _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 294(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 67803 _diffrn_reflns_av_unetI/netI 0.0664 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _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 2.436 _diffrn_reflns_theta_max 28.282 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6854 _reflns_number_gt 5300 _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. Completness statistics refer to single and composite reflections containing twin component 1 only. ; _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 ; At lower temperature (150 K), the compound exhibits a well defined superstructure with one water molecule for every four ammonium cations with pseudo-translation along the a-axis broken by presence or absence of the water molecule (and modulation of the associated ethyl ammonium group and of Pb and Br atoms). See structure FB_0m_150_complete.cif for details. Upon warming to room temperature the unit cell doubling along the a-axis disappears, together with development of worse peak shapes and onset of twinning. This is independent of whether crystals were cooled previously or were taken fresh from mother liquor without ever having been cooled. Several crystals were investigated. Best data were obtained from a piece of the crystal of the 150 K structure determination after rewarming to RT. The crystal under investigation was found to be non-merohedrally twinned. The orientation matrices for the two components were identified using the program Cell_Now, with the two components being related by a 180 degree rotation around the real a-axis [1 0 0]. Attempts were made to integrate the two components using Saint. Integration proved problematic due to excessive multiple overlap of reflections, resulting in excessive numbers of rejected reflections. Attempts were made to adjust integration parameters to avoid excessive rejections (through adjustments to integration queue size, integration box slicing and twin overlap parameters, and omission of box size optimization), which led to less but still substantial numbers of rejected reflections, or to complete but severely deteriorated data (no box size optimization). With no acceptable quality complete data set obtainable through simultaneous integration of both twin domains, the data were instead handled as if not twinned, and twinning was handled using a TWIN transformation matrix in ShelXl. The transformation matrix was obtained using Rotax (as embedded in WinGX) and was TWIN 1.000 0.000 0.000 0.000 -1.000 0.000 -0.522 0.000 -1.000. The minor twin ratio refined to only 0.0350(6) (likley an underestimation due to use of a TWIN command rather than separate domains), but led to substantial improvement of model and refinement (R1 fell from 7.86 to 6.06 %; the largest hole rose from -4.54 to -3.00; ADPs of atoms, especially disordered C and N atoms, improved substantially). One of the ammonium ethyl fragments (associated with the at 150 K ordered and modulated two ammonium ethyl fragments) was refined, initially as 1:1 disordered. Difference densities indicated a lower occupancy of the moiety associated with the water molecule, and occupancies were independently refined. The minor ammonium ethyl fragment and the water occupancy refined to similar values and a common value was thus used. 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. Some water H atom positions were further restrained based on hydrogen bonding considerations. The two disordered ammonium ethyl moieties were restrained to have similar geometries as the other not disordered moiety. Uij components of ADPs for disordered atoms closer to each other than 2.0 Angstrom were restrained to be similar. Subject to these conditions the occupancy ratio refined to 0.855(13) to 0.145(13), indicating that some water might have been lost from the structure after warming up from 150 K to RT, or that the remaining water is distributed within the structure in an ill-defined and not resolved manner. ; _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^)+42.5536P] 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 6854 _refine_ls_number_parameters 355 _refine_ls_number_restraints 139 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1575 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.000 _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 0.49597(5) 0.84777(6) 0.25089(2) 0.04259(13) Uani 1 1 d . . . . . Br1 Br 0.18629(19) 0.6652(2) 0.23749(4) 0.0769(4) Uani 1 1 d . . . . . Br2 Br 0.80738(16) 1.03645(19) 0.25907(3) 0.0647(4) Uani 1 1 d . . . . . Br3 Br 0.49538(19) 0.91153(19) 0.18010(3) 0.0652(4) Uani 1 1 d . . . . . Br4 Br 0.4921(2) 0.7828(2) 0.32185(3) 0.0750(4) Uani 1 1 d . . . . . F1_1 F 0.5312(11) 0.3919(16) 0.0623(2) 0.098(3) Uani 1 1 d D . . . . O2_1 O -0.1457(12) 0.0906(15) 0.0901(2) 0.075(3) Uani 1 1 d . . . . . O3_1 O -0.1399(13) 0.0495(19) 0.0374(2) 0.083(3) Uani 1 1 d . . . . . H3O_1 H -0.237360 0.045684 0.038446 0.125 Uiso 1 1 calc R U . . . N1A_1 N 0.4321(15) 0.3304(18) 0.1857(3) 0.061(3) Uani 0.855(13) 1 d D U P A 1 H1AA_1 H 0.464401 0.352211 0.206138 0.092 Uiso 0.855(13) 1 calc R U P A 1 H1AB_1 H 0.429188 0.218195 0.182615 0.092 Uiso 0.855(13) 1 calc R U P A 1 H1AC_1 H 0.334946 0.373851 0.181713 0.092 Uiso 0.855(13) 1 calc R U P A 1 C1A_1 C 0.541(2) 0.406(2) 0.1646(3) 0.065(3) Uani 0.855(13) 1 d D U P A 1 H1AD_1 H 0.649439 0.381059 0.172589 0.078 Uiso 0.855(13) 1 calc R U P A 1 H1AE_1 H 0.527110 0.528392 0.164817 0.078 Uiso 0.855(13) 1 calc R U P A 1 C2A_1 C 0.5198(19) 0.345(2) 0.1307(3) 0.067(3) Uani 0.855(13) 1 d D U P A 1 H2AA_1 H 0.601175 0.393319 0.117695 0.080 Uiso 0.855(13) 1 calc R U P A 1 H2AB_1 H 0.528758 0.221366 0.129987 0.080 Uiso 0.855(13) 1 calc R U P A 1 O1A_1 O 0.369(3) 0.395(3) 0.1191(3) 0.065(3) Uani 0.855(13) 1 d D U P A 1 N1B_1 N 0.585(7) 0.336(12) 0.173(2) 0.066(6) Uani 0.145(13) 1 d D U P A 2 H1BA_1 H 0.632975 0.349127 0.154463 0.098 Uiso 0.145(13) 1 d R U P A 2 H1BB_1 H 0.565582 0.226006 0.176144 0.098 Uiso 0.145(13) 1 d R U P A 2 H1BC_1 H 0.647252 0.376369 0.189186 0.098 Uiso 0.145(13) 1 d R U P A 2 C1B_1 C 0.438(9) 0.427(10) 0.1712(14) 0.065(4) Uani 0.145(13) 1 d D U P A 2 H1BD_1 H 0.459024 0.546240 0.166865 0.079 Uiso 0.145(13) 1 calc R U P A 2 H1BE_1 H 0.389594 0.420165 0.191936 0.079 Uiso 0.145(13) 1 calc R U P A 2 C2B_1 C 0.323(8) 0.359(11) 0.1455(18) 0.065(3) Uani 0.145(13) 1 d D U P A 2 H2BA_1 H 0.319739 0.235424 0.146319 0.078 Uiso 0.145(13) 1 calc R U P A 2 H2BB_1 H 0.216182 0.402385 0.148346 0.078 Uiso 0.145(13) 1 calc R U P A 2 O1B_1 O 0.377(16) 0.413(15) 0.1162(13) 0.065(4) Uani 0.145(13) 1 d D U P A 2 O4B_1 O 0.730(10) 0.506(16) 0.1215(13) 0.15(4) Uani 0.145(13) 1 d D U P A 2 H4A_1 H 0.664(16) 0.45(2) 0.1106(13) 0.221 Uiso 0.145(13) 1 d D U P A 2 H4B_1 H 0.776(13) 0.57(3) 0.1087(11) 0.221 Uiso 0.145(13) 1 d D U P A 2 C3_1 C 0.3051(16) 0.3256(18) 0.0916(3) 0.059(3) Uani 1 1 d D . . . . C4_1 C 0.3838(18) 0.324(2) 0.0628(3) 0.069(4) Uani 1 1 d . . . . . C5_1 C 0.3154(19) 0.254(2) 0.0351(3) 0.075(4) Uani 1 1 d . . . . . H5_1 H 0.370323 0.254731 0.016190 0.090 Uiso 1 1 calc R U . . . C6_1 C 0.1670(18) 0.184(2) 0.0354(3) 0.066(4) Uani 1 1 d . . . . . H6_1 H 0.121275 0.135304 0.016601 0.079 Uiso 1 1 calc R U . . . C7_1 C 0.0825(16) 0.1832(17) 0.0636(3) 0.053(3) Uani 1 1 d . . . . . C8_1 C 0.1536(16) 0.2557(17) 0.0917(3) 0.057(3) Uani 1 1 d . . . . . H8_1 H 0.098504 0.256932 0.110586 0.068 Uiso 1 1 calc R U . . . C9_1 C -0.0774(16) 0.1060(18) 0.0639(3) 0.058(3) Uani 1 1 d . . . . . F1_2 F -0.0950(11) 0.5932(16) 0.0550(3) 0.107(4) Uani 1 1 d . . . . . O1_2 O 0.0172(13) 0.7002(16) 0.1110(3) 0.085(3) Uani 1 1 d D . . . . O2_2 O 0.5717(13) 0.9367(19) 0.0893(2) 0.083(3) Uani 1 1 d . . . . . H2O_2 H 0.667124 0.957272 0.087961 0.125 Uiso 1 1 calc R U . . . O3_2 O 0.5869(13) 0.8909(17) 0.0370(2) 0.086(4) Uani 1 1 d . . . . . N1_2 N -0.0903(17) 0.863(2) 0.1867(3) 0.096(5) Uani 1 1 d D . . . . H1A_2 H -0.022141 0.811624 0.200777 0.144 Uiso 1 1 calc R U . . . H1B_2 H -0.186847 0.866308 0.194722 0.144 Uiso 1 1 calc R U . . . H1C_2 H -0.056920 0.968622 0.183163 0.144 Uiso 1 1 calc R U . . . C1_2 C -0.0983(19) 0.772(2) 0.1576(4) 0.077(4) Uani 1 1 d D . . . . H1D_2 H -0.185840 0.816282 0.143798 0.093 Uiso 1 1 calc R U . . . H1E_2 H -0.121272 0.653328 0.162065 0.093 Uiso 1 1 calc R U . . . C2_2 C 0.0539(17) 0.782(2) 0.1399(4) 0.076(4) Uani 1 1 d D . . . . H2A_2 H 0.083716 0.899843 0.136271 0.091 Uiso 1 1 calc R U . . . H2B_2 H 0.140929 0.725182 0.151883 0.091 Uiso 1 1 calc R U . . . C3_2 C 0.1158(17) 0.717(2) 0.0867(3) 0.065(4) Uani 1 1 d D . . . . C4_2 C 0.0558(19) 0.657(2) 0.0569(4) 0.079(4) Uani 1 1 d . . . . . C5_2 C 0.140(2) 0.669(2) 0.0298(4) 0.083(5) Uani 1 1 d . . . . . H5_2 H 0.096233 0.629991 0.010011 0.100 Uiso 1 1 calc R U . . . C6_2 C 0.288(2) 0.740(2) 0.0320(4) 0.076(4) Uani 1 1 d . . . . . H6_2 H 0.346919 0.748508 0.013601 0.091 Uiso 1 1 calc R U . . . C7_2 C 0.3546(16) 0.8006(18) 0.0613(3) 0.060(3) Uani 1 1 d . . . . . C8_2 C 0.2681(16) 0.7883(18) 0.0889(3) 0.059(3) Uani 1 1 d . . . . . H8_2 H 0.311523 0.827611 0.108618 0.071 Uiso 1 1 calc R U . . . C9_2 C 0.5150(17) 0.879(2) 0.0626(3) 0.063(3) 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 0.0385(2) 0.0376(2) 0.0521(2) -0.00102(16) 0.00611(16) -0.00058(15) Br1 0.0661(9) 0.0628(9) 0.1012(11) 0.0098(8) -0.0024(8) -0.0304(7) Br2 0.0596(7) 0.0603(8) 0.0733(9) 0.0097(7) -0.0056(6) -0.0237(6) Br3 0.0798(9) 0.0628(8) 0.0529(7) 0.0021(6) 0.0038(6) 0.0031(7) Br4 0.0916(11) 0.0830(11) 0.0510(7) 0.0056(7) 0.0098(7) -0.0041(9) F1_1 0.065(5) 0.156(10) 0.074(6) -0.003(6) 0.014(4) -0.029(6) O2_1 0.072(6) 0.105(9) 0.048(5) -0.007(5) 0.007(5) -0.016(6) O3_1 0.072(7) 0.121(10) 0.056(6) -0.010(6) 0.000(5) -0.023(7) N1A_1 0.065(7) 0.063(7) 0.055(6) 0.001(6) -0.004(5) -0.020(6) C1A_1 0.065(6) 0.068(7) 0.061(6) 0.000(6) -0.001(5) -0.010(6) C2A_1 0.066(6) 0.074(6) 0.060(6) 0.000(5) -0.001(5) -0.007(5) O1A_1 0.066(5) 0.071(6) 0.058(5) -0.003(5) -0.004(5) -0.004(5) N1B_1 0.065(11) 0.070(12) 0.061(11) 0.003(11) -0.003(11) -0.010(11) C1B_1 0.065(7) 0.071(8) 0.060(7) 0.000(7) -0.003(7) -0.009(7) C2B_1 0.065(6) 0.071(7) 0.060(6) -0.001(6) -0.002(6) -0.008(6) O1B_1 0.065(7) 0.071(8) 0.059(7) -0.001(7) -0.002(7) -0.006(7) O4B_1 0.07(5) 0.23(9) 0.14(7) 0.00(6) -0.04(5) -0.08(6) C3_1 0.059(7) 0.068(8) 0.050(7) -0.003(6) 0.004(6) 0.001(6) C4_1 0.062(8) 0.087(11) 0.058(8) 0.005(7) 0.007(6) -0.010(8) C5_1 0.070(9) 0.102(13) 0.054(8) -0.006(8) 0.015(7) -0.007(9) C6_1 0.073(9) 0.079(10) 0.047(7) -0.005(7) 0.008(6) 0.008(8) C7_1 0.060(7) 0.056(7) 0.044(6) -0.002(5) 0.000(5) -0.001(6) C8_1 0.066(8) 0.060(8) 0.045(6) 0.003(6) 0.001(6) -0.003(6) C9_1 0.058(7) 0.064(8) 0.051(7) -0.003(6) 0.000(6) 0.002(6) F1_2 0.062(6) 0.131(10) 0.128(9) -0.013(7) -0.009(6) -0.024(6) O1_2 0.078(7) 0.091(8) 0.086(8) -0.007(6) 0.021(6) -0.018(6) O2_2 0.067(6) 0.131(10) 0.053(5) -0.010(6) 0.005(5) -0.020(7) O3_2 0.074(7) 0.134(11) 0.050(5) -0.017(6) 0.013(5) -0.015(7) N1_2 0.081(10) 0.113(13) 0.096(11) 0.012(10) 0.015(8) -0.023(9) C1_2 0.082(11) 0.067(10) 0.084(11) -0.001(8) 0.024(9) -0.001(8) C2_2 0.063(9) 0.077(10) 0.089(11) 0.001(9) 0.021(8) -0.003(8) C3_2 0.057(8) 0.068(9) 0.071(9) 0.007(7) 0.006(7) 0.003(7) C4_2 0.063(9) 0.077(10) 0.094(12) -0.007(9) -0.011(8) -0.015(8) C5_2 0.086(11) 0.096(13) 0.066(10) -0.012(9) -0.007(8) -0.008(10) C6_2 0.078(10) 0.094(12) 0.056(8) -0.007(8) -0.005(7) -0.011(9) C7_2 0.058(8) 0.063(8) 0.059(8) -0.004(6) 0.009(6) 0.003(6) C8_2 0.056(7) 0.059(8) 0.061(8) -0.002(6) 0.003(6) -0.001(6) C9_2 0.061(8) 0.075(10) 0.054(8) -0.010(7) 0.003(6) -0.001(7) _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 Br1 2.9733(15) 2 ? Pb1 Br3 2.976(2) . ? Pb1 Br4 2.986(2) . ? Pb1 Br2 2.9864(14) 2_645 ? Pb1 Br1 2.9885(16) . ? Pb1 Br2 3.0019(14) . ? F1_1 C4_1 1.344(16) . ? O2_1 C9_1 1.260(15) . ? O3_1 C9_1 1.269(15) . ? O3_1 H3O_1 0.8200 . ? N1A_1 C1A_1 1.427(16) . ? N1A_1 H1AA_1 0.8900 . ? N1A_1 H1AB_1 0.8900 . ? N1A_1 H1AC_1 0.8900 . ? C1A_1 C2A_1 1.483(18) . ? C1A_1 H1AD_1 0.9700 . ? C1A_1 H1AE_1 0.9700 . ? C2A_1 O1A_1 1.39(2) . ? C2A_1 H2AA_1 0.9700 . ? C2A_1 H2AB_1 0.9700 . ? O1A_1 C3_1 1.349(14) . ? N1B_1 C1B_1 1.42(2) . ? N1B_1 H1BA_1 0.8900 . ? N1B_1 H1BB_1 0.8900 . ? N1B_1 H1BC_1 0.8900 . ? C1B_1 C2B_1 1.50(2) . ? C1B_1 H1BD_1 0.9700 . ? C1B_1 H1BE_1 0.9700 . ? C2B_1 O1B_1 1.38(3) . ? C2B_1 H2BA_1 0.9700 . ? C2B_1 H2BB_1 0.9700 . ? O1B_1 C3_1 1.35(2) . ? O4B_1 H4A_1 0.84(2) . ? O4B_1 H4B_1 0.84(2) . ? C3_1 C8_1 1.382(18) . ? C3_1 C4_1 1.393(18) . ? C4_1 C5_1 1.37(2) . ? C5_1 C6_1 1.36(2) . ? C5_1 H5_1 0.9300 . ? C6_1 C7_1 1.400(17) . ? C6_1 H6_1 0.9300 . ? C7_1 C8_1 1.398(17) . ? C7_1 C9_1 1.470(18) . ? C8_1 H8_1 0.9300 . ? F1_2 C4_2 1.356(17) . ? O1_2 C3_2 1.340(14) . ? O1_2 C2_2 1.379(17) . ? O2_2 C9_2 1.265(16) . ? O2_2 H2O_2 0.8200 . ? O3_2 C9_2 1.248(16) . ? N1_2 C1_2 1.401(16) . ? N1_2 H1A_2 0.8900 . ? N1_2 H1B_2 0.8900 . ? N1_2 H1C_2 0.8900 . ? C1_2 C2_2 1.506(16) . ? C1_2 H1D_2 0.9700 . ? C1_2 H1E_2 0.9700 . ? C2_2 H2A_2 0.9700 . ? C2_2 H2B_2 0.9700 . ? C3_2 C4_2 1.39(2) . ? C3_2 C8_2 1.392(19) . ? C4_2 C5_2 1.36(2) . ? C5_2 C6_2 1.36(2) . ? C5_2 H5_2 0.9300 . ? C6_2 C7_2 1.392(19) . ? C6_2 H6_2 0.9300 . ? C7_2 C8_2 1.387(18) . ? C7_2 C9_2 1.476(19) . ? C8_2 H8_2 0.9300 . ? 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 Br1 Pb1 Br3 92.57(5) 2 . ? Br1 Pb1 Br4 87.19(5) 2 . ? Br3 Pb1 Br4 179.27(5) . . ? Br1 Pb1 Br2 177.24(5) 2 2_645 ? Br3 Pb1 Br2 88.48(5) . 2_645 ? Br4 Pb1 Br2 91.79(5) . 2_645 ? Br1 Pb1 Br1 89.08(3) 2 . ? Br3 Pb1 Br1 86.63(5) . . ? Br4 Pb1 Br1 92.68(5) . . ? Br2 Pb1 Br1 93.53(5) 2_645 . ? Br1 Pb1 Br2 91.08(5) 2 . ? Br3 Pb1 Br2 89.12(5) . . ? Br4 Pb1 Br2 91.57(5) . . ? Br2 Pb1 Br2 86.39(2) 2_645 . ? Br1 Pb1 Br2 175.75(5) . . ? Pb1 Br1 Pb1 144.99(7) 2_545 . ? Pb1 Br2 Pb1 150.41(6) 2_655 . ? C9_1 O3_1 H3O_1 109.5 . . ? C1A_1 N1A_1 H1AA_1 109.5 . . ? C1A_1 N1A_1 H1AB_1 109.5 . . ? H1AA_1 N1A_1 H1AB_1 109.5 . . ? C1A_1 N1A_1 H1AC_1 109.5 . . ? H1AA_1 N1A_1 H1AC_1 109.5 . . ? H1AB_1 N1A_1 H1AC_1 109.5 . . ? N1A_1 C1A_1 C2A_1 113.6(13) . . ? N1A_1 C1A_1 H1AD_1 108.9 . . ? C2A_1 C1A_1 H1AD_1 108.9 . . ? N1A_1 C1A_1 H1AE_1 108.9 . . ? C2A_1 C1A_1 H1AE_1 108.9 . . ? H1AD_1 C1A_1 H1AE_1 107.7 . . ? O1A_1 C2A_1 C1A_1 107.3(13) . . ? O1A_1 C2A_1 H2AA_1 110.3 . . ? C1A_1 C2A_1 H2AA_1 110.3 . . ? O1A_1 C2A_1 H2AB_1 110.3 . . ? C1A_1 C2A_1 H2AB_1 110.3 . . ? H2AA_1 C2A_1 H2AB_1 108.5 . . ? C3_1 O1A_1 C2A_1 119.3(19) . . ? C1B_1 N1B_1 H1BA_1 109.4 . . ? C1B_1 N1B_1 H1BB_1 109.6 . . ? H1BA_1 N1B_1 H1BB_1 109.5 . . ? C1B_1 N1B_1 H1BC_1 109.5 . . ? H1BA_1 N1B_1 H1BC_1 109.5 . . ? H1BB_1 N1B_1 H1BC_1 109.5 . . ? N1B_1 C1B_1 C2B_1 112(3) . . ? N1B_1 C1B_1 H1BD_1 109.2 . . ? C2B_1 C1B_1 H1BD_1 109.2 . . ? N1B_1 C1B_1 H1BE_1 109.2 . . ? C2B_1 C1B_1 H1BE_1 109.2 . . ? H1BD_1 C1B_1 H1BE_1 107.9 . . ? O1B_1 C2B_1 C1B_1 107(3) . . ? O1B_1 C2B_1 H2BA_1 110.4 . . ? C1B_1 C2B_1 H2BA_1 110.4 . . ? O1B_1 C2B_1 H2BB_1 110.4 . . ? C1B_1 C2B_1 H2BB_1 110.4 . . ? H2BA_1 C2B_1 H2BB_1 108.6 . . ? C3_1 O1B_1 C2B_1 111(6) . . ? H4A_1 O4B_1 H4B_1 108(4) . . ? O1B_1 C3_1 C8_1 125(5) . . ? O1A_1 C3_1 C8_1 118.7(13) . . ? O1B_1 C3_1 C4_1 116(5) . . ? O1A_1 C3_1 C4_1 122.9(15) . . ? C8_1 C3_1 C4_1 118.4(12) . . ? F1_1 C4_1 C5_1 119.3(13) . . ? F1_1 C4_1 C3_1 119.1(13) . . ? C5_1 C4_1 C3_1 121.6(14) . . ? C6_1 C5_1 C4_1 119.9(13) . . ? C6_1 C5_1 H5_1 120.0 . . ? C4_1 C5_1 H5_1 120.0 . . ? C5_1 C6_1 C7_1 120.6(14) . . ? C5_1 C6_1 H6_1 119.7 . . ? C7_1 C6_1 H6_1 119.7 . . ? C8_1 C7_1 C6_1 118.8(13) . . ? C8_1 C7_1 C9_1 120.7(11) . . ? C6_1 C7_1 C9_1 120.5(12) . . ? C3_1 C8_1 C7_1 120.6(12) . . ? C3_1 C8_1 H8_1 119.7 . . ? C7_1 C8_1 H8_1 119.7 . . ? O2_1 C9_1 O3_1 121.8(13) . . ? O2_1 C9_1 C7_1 120.0(12) . . ? O3_1 C9_1 C7_1 118.2(12) . . ? C3_2 O1_2 C2_2 119.2(12) . . ? 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_2 113.0(13) . . ? N1_2 C1_2 H1D_2 109.0 . . ? C2_2 C1_2 H1D_2 109.0 . . ? N1_2 C1_2 H1E_2 109.0 . . ? C2_2 C1_2 H1E_2 109.0 . . ? H1D_2 C1_2 H1E_2 107.8 . . ? O1_2 C2_2 C1_2 104.1(12) . . ? O1_2 C2_2 H2A_2 110.9 . . ? C1_2 C2_2 H2A_2 110.9 . . ? O1_2 C2_2 H2B_2 110.9 . . ? C1_2 C2_2 H2B_2 110.9 . . ? H2A_2 C2_2 H2B_2 109.0 . . ? O1_2 C3_2 C4_2 115.2(14) . . ? O1_2 C3_2 C8_2 126.1(14) . . ? C4_2 C3_2 C8_2 118.7(13) . . ? F1_2 C4_2 C5_2 119.8(16) . . ? F1_2 C4_2 C3_2 117.9(15) . . ? C5_2 C4_2 C3_2 122.2(15) . . ? C4_2 C5_2 C6_2 118.8(15) . . ? C4_2 C5_2 H5_2 120.6 . . ? C6_2 C5_2 H5_2 120.6 . . ? C5_2 C6_2 C7_2 121.2(15) . . ? C5_2 C6_2 H6_2 119.4 . . ? C7_2 C6_2 H6_2 119.4 . . ? C8_2 C7_2 C6_2 119.6(14) . . ? C8_2 C7_2 C9_2 121.0(13) . . ? C6_2 C7_2 C9_2 119.4(13) . . ? C7_2 C8_2 C3_2 119.5(13) . . ? C7_2 C8_2 H8_2 120.3 . . ? C3_2 C8_2 H8_2 120.3 . . ? O3_2 C9_2 O2_2 122.7(14) . . ? O3_2 C9_2 C7_2 118.7(13) . . ? O2_2 C9_2 C7_2 118.5(12) . . ? 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 N1A_1 C1A_1 C2A_1 O1A_1 64(2) . . . . ? C1A_1 C2A_1 O1A_1 C3_1 -165.6(15) . . . . ? N1B_1 C1B_1 C2B_1 O1B_1 -75(12) . . . . ? C1B_1 C2B_1 O1B_1 C3_1 165(9) . . . . ? C2B_1 O1B_1 C3_1 C8_1 29(15) . . . . ? C2B_1 O1B_1 C3_1 C4_1 -159(8) . . . . ? C2A_1 O1A_1 C3_1 C8_1 127.8(17) . . . . ? C2A_1 O1A_1 C3_1 C4_1 -54(2) . . . . ? O1B_1 C3_1 C4_1 F1_1 7(8) . . . . ? O1A_1 C3_1 C4_1 F1_1 2(3) . . . . ? C8_1 C3_1 C4_1 F1_1 180.0(14) . . . . ? O1B_1 C3_1 C4_1 C5_1 -174(7) . . . . ? O1A_1 C3_1 C4_1 C5_1 -179.2(19) . . . . ? C8_1 C3_1 C4_1 C5_1 -1(2) . . . . ? F1_1 C4_1 C5_1 C6_1 179.3(16) . . . . ? C3_1 C4_1 C5_1 C6_1 0(3) . . . . ? C4_1 C5_1 C6_1 C7_1 1(3) . . . . ? C5_1 C6_1 C7_1 C8_1 0(2) . . . . ? C5_1 C6_1 C7_1 C9_1 -179.7(15) . . . . ? O1B_1 C3_1 C8_1 C7_1 173(8) . . . . ? O1A_1 C3_1 C8_1 C7_1 179.5(16) . . . . ? C4_1 C3_1 C8_1 C7_1 1(2) . . . . ? C6_1 C7_1 C8_1 C3_1 0(2) . . . . ? C9_1 C7_1 C8_1 C3_1 178.9(13) . . . . ? C8_1 C7_1 C9_1 O2_1 -7(2) . . . . ? C6_1 C7_1 C9_1 O2_1 172.8(14) . . . . ? C8_1 C7_1 C9_1 O3_1 176.6(14) . . . . ? C6_1 C7_1 C9_1 O3_1 -4(2) . . . . ? C3_2 O1_2 C2_2 C1_2 166.4(14) . . . . ? N1_2 C1_2 C2_2 O1_2 -174.4(15) . . . . ? C2_2 O1_2 C3_2 C4_2 -168.7(15) . . . . ? C2_2 O1_2 C3_2 C8_2 11(2) . . . . ? O1_2 C3_2 C4_2 F1_2 2(2) . . . . ? C8_2 C3_2 C4_2 F1_2 -177.6(15) . . . . ? O1_2 C3_2 C4_2 C5_2 177.9(17) . . . . ? C8_2 C3_2 C4_2 C5_2 -1(3) . . . . ? F1_2 C4_2 C5_2 C6_2 177.2(17) . . . . ? C3_2 C4_2 C5_2 C6_2 1(3) . . . . ? C4_2 C5_2 C6_2 C7_2 0(3) . . . . ? C5_2 C6_2 C7_2 C8_2 0(3) . . . . ? C5_2 C6_2 C7_2 C9_2 -179.0(16) . . . . ? C6_2 C7_2 C8_2 C3_2 0(2) . . . . ? C9_2 C7_2 C8_2 C3_2 178.7(14) . . . . ? O1_2 C3_2 C8_2 C7_2 -178.2(14) . . . . ? C4_2 C3_2 C8_2 C7_2 1(2) . . . . ? C8_2 C7_2 C9_2 O3_2 -178.4(14) . . . . ? C6_2 C7_2 C9_2 O3_2 1(2) . . . . ? C8_2 C7_2 C9_2 O2_2 -1(2) . . . . ? C6_2 C7_2 C9_2 O2_2 178.4(16) . . . . ? _refine_diff_density_max 4.297 _refine_diff_density_min -3.006 _refine_diff_density_rms 0.257 _shelx_res_file ; TITL FB_RT_0m_a.res in P2(1)/n FB_RT_0m.res created by SHELXL-2019/3 at 10:36:45 on 24-Jan-2024 REM Old TITL FB_RT_0m in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.196, Rweak 0.027, Alpha 0.051 REM 2.137 for 422 systematic absences, Orientation as input REM Formula found by SHELXT: C18 N4 O7 Br4 Pb CELL 0.71073 8.3729 7.8455 41.4402 90.000 93.029 90.000 ZERR 2.000 0.0022 0.0015 0.0198 0.000 0.021 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O F BR PB UNIT 72 89.6363 8 24.8182 8 16 4 OMIT 0 0 4 TEMP 20.850 SIZE 0.085 0.149 0.312 L.S. 20 BOND $H ACTA CONF HTAB LIST 4 FMAP -2 PLAN 20 SADI C3_1 O1A_1 C3_1 O1B_1 C3_2 O1_2 DFIX_1 0.84 O4B H4A O4B H4B DFIX_1 1.36 H4A H4B SIMU_1 0.01 N1A > O1B REM DAMP 200 DFIX_1 2.28 H4A F1 DFIX_1 2.44 H4A O1B DFIX_2 2.53 H4B_1 F1_$1 DFIX_2 2.26 H4B_1 O1_$1 EQIV $1 1+x, +y, +z ISOR_1 0.05 O4B TWIN 1.000 0.000 0.000 0.000 -1.000 0.000 -0.522 0.000 -1.000 SHEL 99 0.75 WGHT 0.000000 42.553596 BASF 0.03452 FVAR 0.15179 0.85480 PB1 7 0.495969 0.847769 0.250886 11.00000 0.03847 0.03764 = 0.05206 -0.00102 0.00611 -0.00058 BR1 6 0.186290 0.665192 0.237489 11.00000 0.06610 0.06278 = 0.10115 0.00976 -0.00239 -0.03037 BR2 6 0.807384 1.036449 0.259074 11.00000 0.05959 0.06031 = 0.07325 0.00975 -0.00558 -0.02374 BR3 6 0.495382 0.911532 0.180098 11.00000 0.07983 0.06280 = 0.05293 0.00212 0.00378 0.00314 BR4 6 0.492099 0.782820 0.321846 11.00000 0.09165 0.08300 = 0.05101 0.00560 0.00979 -0.00414 RESI 1 F1 5 0.531239 0.391912 0.062260 11.00000 0.06477 0.15600 = 0.07391 -0.00291 0.01400 -0.02867 O2 4 -0.145672 0.090554 0.090097 11.00000 0.07217 0.10539 = 0.04841 -0.00733 0.00697 -0.01612 O3 4 -0.139895 0.049498 0.037410 11.00000 0.07178 0.12126 = 0.05578 -0.00996 -0.00013 -0.02268 AFIX 147 H3O 2 -0.237360 0.045684 0.038446 11.00000 -1.50000 AFIX 0 PART 1 21 SAME_2 N1 C1 C2 O1 N1A 3 0.432145 0.330403 0.185747 21.00000 0.06465 0.06288 = 0.05537 0.00101 -0.00367 -0.01960 AFIX 137 H1AA 2 0.464401 0.352211 0.206138 21.00000 -1.50000 H1AB 2 0.429188 0.218195 0.182615 21.00000 -1.50000 H1AC 2 0.334946 0.373851 0.181713 21.00000 -1.50000 AFIX 0 C1A 1 0.540979 0.405660 0.164552 21.00000 0.06529 0.06840 = 0.06136 -0.00019 -0.00119 -0.01039 AFIX 23 H1AD 2 0.649439 0.381059 0.172589 21.00000 -1.20000 H1AE 2 0.527110 0.528392 0.164817 21.00000 -1.20000 AFIX 0 C2A 1 0.519812 0.344556 0.130725 21.00000 0.06585 0.07443 = 0.06047 0.00003 -0.00070 -0.00718 AFIX 23 H2AA 2 0.601175 0.393319 0.117695 21.00000 -1.20000 H2AB 2 0.528758 0.221366 0.129987 21.00000 -1.20000 AFIX 0 O1A 4 0.368826 0.395484 0.119069 21.00000 0.06561 0.07107 = 0.05834 -0.00286 -0.00424 -0.00413 PART 2 -21 SAME_2 N1 C1 C2 O1 N1B 3 0.584580 0.336145 0.172916 -21.00000 0.06508 0.06983 = 0.06099 0.00279 -0.00265 -0.00988 AFIX 3 H1BA 2 0.632975 0.349127 0.154463 -21.00000 -1.50000 H1BB 2 0.565582 0.226006 0.176144 -21.00000 -1.50000 H1BC 2 0.647252 0.376369 0.189186 -21.00000 -1.50000 AFIX 0 C1B 1 0.437926 0.427088 0.171213 -21.00000 0.06461 0.07101 = 0.06004 0.00021 -0.00257 -0.00944 AFIX 23 H1BD 2 0.459024 0.546240 0.166865 -21.00000 -1.20000 H1BE 2 0.389594 0.420165 0.191936 -21.00000 -1.20000 AFIX 0 C2B 1 0.322943 0.358925 0.145461 -21.00000 0.06514 0.07050 = 0.05957 -0.00051 -0.00201 -0.00775 AFIX 23 H2BA 2 0.319739 0.235424 0.146319 -21.00000 -1.20000 H2BB 2 0.216182 0.402385 0.148346 -21.00000 -1.20000 AFIX 0 O1B 4 0.377242 0.412774 0.116248 -21.00000 0.06520 0.07146 = 0.05921 -0.00107 -0.00239 -0.00587 O4B 4 0.729670 0.506268 0.121475 -21.00000 0.06996 0.22908 = 0.13830 -0.00434 -0.04017 -0.08154 REM AFIX 3 H4A 2 0.664274 0.445275 0.110631 -21.00000 -1.50000 H4B 2 0.776026 0.570170 0.108671 -21.00000 -1.50000 REM AFIX 0 PART 0 C3 1 0.305124 0.325589 0.091554 11.00000 0.05933 0.06784 = 0.04994 -0.00330 0.00362 0.00066 C4 1 0.383828 0.324345 0.062755 11.00000 0.06154 0.08674 = 0.05839 0.00506 0.00671 -0.00950 C5 1 0.315440 0.254200 0.035124 11.00000 0.06967 0.10176 = 0.05404 -0.00616 0.01484 -0.00740 AFIX 43 H5 2 0.370323 0.254731 0.016190 11.00000 -1.20000 AFIX 0 C6 1 0.167019 0.183660 0.035382 11.00000 0.07268 0.07933 = 0.04683 -0.00470 0.00773 0.00813 AFIX 43 H6 2 0.121275 0.135304 0.016601 11.00000 -1.20000 AFIX 0 C7 1 0.082539 0.183184 0.063646 11.00000 0.06002 0.05586 = 0.04372 -0.00184 -0.00031 -0.00082 C8 1 0.153633 0.255707 0.091684 11.00000 0.06564 0.06023 = 0.04511 0.00272 0.00140 -0.00340 AFIX 43 H8 2 0.098504 0.256932 0.110586 11.00000 -1.20000 AFIX 0 C9 1 -0.077416 0.105972 0.063869 11.00000 0.05812 0.06446 = 0.05100 -0.00301 0.00009 0.00231 RESI 2 F1 5 -0.094975 0.593198 0.055003 11.00000 0.06200 0.13120 = 0.12775 -0.01339 -0.00895 -0.02443 O1 4 0.017207 0.700237 0.110975 11.00000 0.07845 0.09132 = 0.08605 -0.00690 0.02060 -0.01817 O2 4 0.571685 0.936660 0.089291 11.00000 0.06650 0.13074 = 0.05299 -0.01009 0.00496 -0.01976 AFIX 147 H2O 2 0.667124 0.957272 0.087961 11.00000 -1.50000 AFIX 0 O3 4 0.586913 0.890865 0.037038 11.00000 0.07437 0.13438 = 0.04976 -0.01656 0.01328 -0.01495 N1 3 -0.090328 0.862914 0.186719 11.00000 0.08063 0.11337 = 0.09581 0.01208 0.01496 -0.02331 AFIX 137 H1A 2 -0.022141 0.811624 0.200777 11.00000 -1.50000 H1B 2 -0.186847 0.866308 0.194722 11.00000 -1.50000 H1C 2 -0.056920 0.968622 0.183163 11.00000 -1.50000 AFIX 0 C1 1 -0.098316 0.771940 0.157600 11.00000 0.08236 0.06705 = 0.08415 -0.00062 0.02402 -0.00108 AFIX 23 H1D 2 -0.185840 0.816282 0.143798 11.00000 -1.20000 H1E 2 -0.121272 0.653328 0.162065 11.00000 -1.20000 AFIX 0 C2 1 0.053855 0.782178 0.139871 11.00000 0.06341 0.07653 = 0.08945 0.00113 0.02056 -0.00320 AFIX 23 H2A 2 0.083716 0.899843 0.136271 11.00000 -1.20000 H2B 2 0.140929 0.725182 0.151883 11.00000 -1.20000 AFIX 0 C3 1 0.115829 0.716611 0.086743 11.00000 0.05668 0.06821 = 0.07149 0.00660 0.00647 0.00257 C4 1 0.055840 0.656742 0.056944 11.00000 0.06338 0.07680 = 0.09436 -0.00736 -0.01079 -0.01472 C5 1 0.139689 0.669206 0.029753 11.00000 0.08591 0.09649 = 0.06607 -0.01190 -0.00686 -0.00762 AFIX 43 H5 2 0.096233 0.629991 0.010011 11.00000 -1.20000 AFIX 0 C6 1 0.288496 0.740228 0.032010 11.00000 0.07778 0.09402 = 0.05579 -0.00709 -0.00475 -0.01100 AFIX 43 H6 2 0.346919 0.748508 0.013601 11.00000 -1.20000 AFIX 0 C7 1 0.354583 0.800551 0.061340 11.00000 0.05823 0.06318 = 0.05903 -0.00422 0.00934 0.00315 C8 1 0.268119 0.788279 0.088880 11.00000 0.05599 0.05890 = 0.06144 -0.00164 0.00323 -0.00147 AFIX 43 H8 2 0.311523 0.827611 0.108618 11.00000 -1.20000 AFIX 0 C9 1 0.514999 0.879102 0.062559 11.00000 0.06058 0.07467 = 0.05363 -0.00968 0.00257 -0.00086 RESI 0 HKLF 4 REM FB_RT_0m_a.res in P2(1)/n REM wR2 = 0.1575, GooF = S = 1.076, Restrained GooF = 1.066 for all data REM R1 = 0.0581 for 5300 Fo > 4sig(Fo) and 0.0696 for all 6854 data REM 355 parameters refined using 139 restraints END WGHT 0.0000 42.5536 REM Instructions for potential hydrogen bonds EQIV $6 x-1, y-1, z HTAB_2 O3_1 O3_$6 EQIV $2 -x+1/2, y-1/2, -z+1/2 HTAB N1A_1 Br1_$2 EQIV $5 -x+3/2, y-1/2, -z+1/2 HTAB N1A_1 Br2_$5 EQIV $7 x, y-1, z HTAB N1A_1 Br3_$7 HTAB N1A_1 Br4_$2 HTAB C1A_1 Br4_$5 HTAB C1A_1 Br3 HTAB C2A_1 F1_1 HTAB N1B_1 O4B_1 HTAB N1B_1 Br3_$7 HTAB N1B_1 Br2_$5 HTAB C1B_1 Br3 HTAB C2B_1 Br4_$2 HTAB O4B_1 F1_1 HTAB O4B_1 O1B_1 HTAB_2 O4B_1 F1_$1 HTAB_2 O4B_1 O1_$1 EQIV $8 -x+1, -y+1, -z HTAB_2 C5_1 O3_$8 HTAB C8_1 Br4_$2 EQIV $9 x+1, y+1, z HTAB_1 O2_2 O2_$9 HTAB N1_2 Br1 EQIV $10 x-1, y, z HTAB N1_2 Br2_$10 HTAB N1_2 Br3_$10 EQIV $4 -x+1/2, y+1/2, -z+1/2 HTAB N1_2 Br4_$4 HTAB_1 C1_2 O4B_$10 REM Highest difference peak 4.297, deepest hole -3.006, 1-sigma level 0.257 Q1 1 0.5019 0.3785 0.2499 11.00000 0.05 4.30 Q2 1 0.0010 0.7423 0.2499 11.00000 0.05 3.67 Q3 1 0.9955 0.9622 0.2522 11.00000 0.05 -3.01 Q4 1 0.9990 1.0473 0.2502 11.00000 0.05 2.60 Q5 1 0.4934 0.9208 0.2507 11.00000 0.05 2.25 Q6 1 0.5936 0.7788 0.3235 11.00000 0.05 2.06 Q7 1 0.7471 0.9934 0.2498 11.00000 0.05 -2.04 Q8 1 0.4986 0.6402 0.2505 11.00000 0.05 1.99 Q9 1 0.4966 0.7264 0.2513 11.00000 0.05 1.90 Q10 1 0.2448 0.5039 0.2504 11.00000 0.05 -1.89 Q11 1 0.3232 0.5563 0.2625 11.00000 0.05 1.82 Q12 1 0.2820 0.7765 0.2562 11.00000 0.05 -1.79 Q13 1 0.2430 0.8958 0.2492 11.00000 0.05 -1.56 Q14 1 0.6693 0.9239 0.2392 11.00000 0.05 1.49 Q15 1 0.3323 0.9160 0.2610 11.00000 0.05 1.45 Q16 1 0.8253 0.9960 0.2390 11.00000 0.05 1.37 Q17 1 0.4834 0.9077 0.3221 11.00000 0.05 1.34 Q18 1 0.4874 0.8543 0.2287 11.00000 0.05 1.34 Q19 1 -0.0146 0.8108 0.1768 11.00000 0.05 1.32 Q20 1 0.8334 1.0752 0.2621 11.00000 0.05 1.29 ; _shelx_res_checksum 49125 _shelx_hkl_file ; 1 0 0 5.96165 2.45780 1 1 0 0 8.21196 1.16224 2 1 0 0 -0.1559 1.01759 3 -1 0 0 13.9591 1.13294 4 -1 0 0 1.65892 1.98600 1 -1 0 0 16.6371 1.17590 3 2 0 0 4534.48 765.288 1 -2 0 0 4806.76 765.478 1 -2 0 0 4594.35 763.488 3 -3 0 0 3.13987 0.99648 4 -3 0 0 2.43277 1.26699 2 -3 0 0 5.08028 1.14173 3 3 0 0 1.66152 0.99049 3 -3 0 0 -0.8807 5.48232 1 3 0 0 4.36387 1.22714 2 3 0 0 4.05602 1.08882 4 3 0 0 2.54133 5.25790 1 -4 0 0 1662.66 284.510 4 4 0 0 1650.95 284.522 4 4 0 0 1664.93 284.626 2 4 0 0 1781.87 288.369 1 -4 0 0 1846.45 288.538 1 -4 0 0 1738.09 284.522 3 4 0 0 1713.29 284.502 3 4 0 0 1810.17 284.780 2 -5 0 0 2.54236 1.19775 4 5 0 0 2.53198 2.04441 2 5 0 0 1.34207 1.61240 2 5 0 0 4.55087 1.31548 3 -5 0 0 -0.5758 8.97812 1 -5 0 0 4.64247 1.50400 3 5 0 0 2.38456 1.42192 4 5 0 0 -0.3096 8.58815 1 -6 0 0 1304.51 253.942 1 6 0 0 1251.02 253.367 1 6 0 0 1714.04 248.293 4 6 0 0 1506.71 248.460 2 6 0 0 1367.05 248.713 2 -6 0 0 1539.44 248.267 3 6 0 0 1618.87 248.245 3 -6 0 0 1693.38 248.279 4 7 0 0 0.35133 1.63268 3 7 0 0 -0.9727 2.27254 2 7 0 0 2.89280 3.13769 2 7 0 0 -1.3957 1.77979 4 7 0 0 6.11508 14.5866 1 -7 0 0 -9.2323 15.1126 1 -8 0 0 75.7140 32.2826 1 8 0 0 111.910 21.4578 2 8 0 0 137.759 20.6112 3 8 0 0 140.033 20.8206 4 8 0 0 89.5334 31.4243 1 -9 0 0 -2.7298 24.6918 1 9 0 0 0.99691 4.17700 2 9 0 0 -1.3611 2.52271 4 9 0 0 -10.530 21.8012 1 9 0 0 0.08736 2.05461 3 10 0 0 165.610 24.0840 4 10 0 0 151.233 23.9243 3 10 0 0 127.693 25.3444 2 10 0 0 95.6582 41.1569 1 -10 0 0 84.8374 43.6965 1 -11 0 0 -9.3263 51.9509 1 11 0 0 2.28713 5.10491 2 11 0 0 2.97751 2.95641 4 11 0 0 -1.2925 2.36224 3 0 -1 0 5.00844 0.34941 3 0 -1 0 2.26915 1.12481 1 0 -1 0 3.72381 0.62684 2 0 1 0 -0.0525 0.16419 3 0 1 0 0.13714 0.19767 4 0 1 0 0.32562 0.26192 2 0 1 0 0.24255 0.89879 1 1 -1 0 1054.86 188.535 2 1 -1 0 988.875 188.490 4 -1 -1 0 1053.69 188.500 4 -1 -1 0 1299.57 188.521 2 -1 -1 0 1337.22 189.728 1 1 -1 0 1135.26 188.484 3 1 -1 0 1263.33 189.262 1 -1 -1 0 996.684 188.481 3 -1 1 0 1286.86 189.323 1 -1 1 0 1105.25 188.482 3 1 1 0 1090.31 188.507 4 1 1 0 1340.00 189.718 1 1 1 0 1065.69 188.485 3 -1 1 0 1073.67 188.535 2 -2 -1 0 219.593 41.6060 4 2 -1 0 245.453 41.6685 2 2 -1 0 202.839 41.5889 4 -2 -1 0 235.314 41.5829 3 -2 -1 0 358.576 44.6763 1 2 -1 0 245.032 41.5867 3 2 -1 0 352.966 43.9467 1 2 1 0 314.246 41.6478 2 -2 1 0 203.308 41.5867 4 2 1 0 233.293 41.5809 3 2 1 0 359.800 44.5733 1 -2 1 0 251.323 41.6758 2 -2 1 0 251.409 41.5875 3 2 1 0 215.987 41.6201 4 -3 -1 0 2143.40 354.560 3 -3 -1 0 2085.77 354.579 4 -3 -1 0 2418.26 357.958 1 3 -1 0 2135.53 354.557 3 3 -1 0 2237.93 357.102 1 3 -1 0 2028.52 354.572 4 3 -1 0 2047.33 354.678 2 -3 1 0 1990.21 354.565 4 -3 1 0 2236.72 354.566 3 3 1 0 2458.91 357.868 1 3 1 0 2230.02 354.726 2 -3 1 0 2117.69 354.703 2 -3 1 0 2168.41 357.757 1 3 1 0 2040.18 354.619 2 3 1 0 2064.52 354.598 4 3 1 0 2170.09 354.556 3 -4 -1 0 197.084 41.7399 1 -4 -1 0 227.518 36.5303 4 4 -1 0 210.547 36.6332 2 -4 -1 0 230.509 36.5258 3 4 -1 0 237.936 36.5210 3 4 -1 0 222.936 36.5293 4 4 -1 0 200.260 40.6079 1 -4 1 0 226.941 36.6835 2 4 1 0 210.315 36.5386 2 4 1 0 232.936 36.5990 4 4 1 0 217.236 41.7094 1 4 1 0 230.894 36.5041 3 -4 1 0 199.754 41.0009 1 4 1 0 221.533 36.6449 2 -4 1 0 217.945 36.5153 4 -4 1 0 220.997 36.5266 3 5 -1 0 341.736 57.3995 4 5 -1 0 339.722 57.5383 2 5 -1 0 363.117 57.6492 2 -5 -1 0 336.959 57.3864 3 -5 -1 0 341.452 57.3941 4 5 -1 0 371.631 63.0833 1 -5 -1 0 375.547 63.8349 1 5 -1 0 350.168 57.3786 3 5 1 0 358.992 63.4537 1 5 1 0 344.210 57.4687 4 5 1 0 332.989 57.4345 2 -5 1 0 338.365 57.3883 4 -5 1 0 337.039 57.3988 3 -5 1 0 354.401 57.5807 2 5 1 0 347.756 57.3722 3 -5 1 0 367.646 63.4232 1 5 1 0 363.289 57.5984 2 6 -1 0 6.70856 2.94632 2 6 -1 0 6.72413 1.88680 3 -6 -1 0 -3.1081 11.6575 1 6 -1 0 6.29863 1.89662 4 6 -1 0 6.73497 2.48209 2 6 -1 0 -18.111 9.74061 1 -6 -1 0 6.09162 1.75716 4 6 1 0 8.19898 2.87852 2 6 1 0 6.39978 2.19288 2 -6 1 0 7.77561 12.4885 1 -6 1 0 6.39269 1.93895 3 6 1 0 4.16457 1.77922 3 6 1 0 3.39289 11.9374 1 6 1 0 2.85927 2.21970 4 7 -1 0 207.716 36.3893 3 7 -1 0 238.903 36.9425 2 -7 -1 0 262.528 49.8044 1 7 -1 0 215.491 36.4644 4 7 -1 0 239.888 46.7274 1 7 1 0 200.762 36.5309 4 7 1 0 213.950 36.3952 3 7 1 0 226.726 36.8713 2 7 1 0 214.804 36.5809 2 -7 1 0 235.599 48.1722 1 7 1 0 236.309 48.3539 1 8 -1 0 16.1709 3.51137 4 8 -1 0 16.3217 18.7792 1 -8 -1 0 6.35261 20.7715 1 8 -1 0 16.2852 3.33379 3 8 -1 0 15.3315 5.00237 2 8 1 0 14.5007 3.89401 2 -8 1 0 32.5503 22.2498 1 8 1 0 17.4756 3.32198 3 8 1 0 17.6649 3.79948 4 8 1 0 0.59847 17.9512 1 8 1 0 14.6959 4.81812 2 9 -1 0 79.8651 13.5798 4 -9 -1 0 61.8107 32.4828 1 9 -1 0 69.0901 14.8840 2 9 -1 0 58.8037 27.9230 1 9 -1 0 79.8873 13.4305 3 9 1 0 48.1689 28.5086 1 9 1 0 86.0814 13.7695 4 9 1 0 77.1616 15.0266 2 9 1 0 93.0369 13.4369 3 -9 1 0 52.5097 31.2299 1 10 -1 0 15.8563 28.9353 1 10 -1 0 13.9647 3.63307 4 -10 -1 0 18.3331 33.9852 1 10 -1 0 15.3742 3.24504 3 10 -1 0 8.41903 5.69031 2 10 1 0 12.3070 3.82902 4 10 1 0 7.72028 31.3304 1 -10 1 0 17.1881 33.7261 1 10 1 0 14.2381 3.16426 3 10 1 0 10.5967 5.75467 2 11 -1 0 14.0127 3.54196 3 11 -1 0 14.9629 6.60415 2 11 -1 0 14.6823 4.12200 4 -11 -1 0 37.4076 45.6986 1 11 1 0 17.7255 4.36999 4 11 1 0 -18.711 37.9144 1 11 1 0 13.1900 6.25933 2 11 1 0 14.5953 3.55166 3 0 -2 0 1514.88 230.716 3 0 -2 0 1485.03 230.730 4 0 -2 0 1278.02 231.204 1 0 -2 0 1299.17 230.758 2 0 2 0 1529.52 230.718 3 0 2 0 1492.58 230.731 4 0 2 0 1222.54 230.752 2 1 -2 0 27.2394 5.58828 1 1 -2 0 18.1122 3.62727 2 -1 -2 0 27.8889 6.30816 1 -1 2 0 20.2302 3.42423 4 1 2 0 18.7950 3.43114 2 1 2 0 24.1039 6.20091 1 -1 2 0 16.9498 3.63442 2 -1 2 0 35.4162 6.19895 1 2 -2 0 714.597 112.025 4 2 -2 0 734.831 112.032 4 -2 -2 0 708.681 112.040 2 -2 -2 0 811.746 112.064 4 2 -2 0 619.544 112.112 2 2 -2 0 744.952 112.005 3 -2 -2 0 719.616 112.006 3 2 -2 0 531.050 113.278 1 -2 2 0 632.080 112.117 2 2 2 0 786.779 112.067 4 2 2 0 524.182 113.910 1 -2 2 0 707.098 112.003 3 2 2 0 656.635 112.006 2 2 2 0 719.751 112.013 3 -2 2 0 551.887 113.457 1 3 -2 0 2.38438 5.24254 1 -3 -2 0 3.36752 1.23696 4 -3 -2 0 3.84714 0.96803 3 3 -2 0 1.75280 1.51965 2 -3 -2 0 7.13912 6.90985 1 3 -2 0 3.39670 0.99904 3 3 -2 0 3.28897 1.07181 4 3 2 0 -2.3566 6.07587 1 -3 2 0 4.35860 1.66252 2 -3 2 0 2.58305 0.99855 3 3 2 0 2.66084 1.41816 4 -3 2 0 2.19255 0.93953 4 -3 2 0 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68.8764 12.8299 3 3 -4 10 69.3821 12.7639 3 -3 -4 -10 91.7516 14.0500 2 3 4 10 86.3164 13.3082 2 3 4 10 69.1995 13.0766 4 3 4 10 73.0293 12.8435 3 3 4 10 127.836 24.5213 1 -3 4 -10 121.700 18.5242 1 -4 -4 -10 336.310 53.4570 2 4 -4 10 301.061 53.1158 4 4 -4 10 323.713 53.0379 3 -4 -4 -10 346.380 60.8337 1 4 -4 10 298.842 53.0168 3 4 -4 10 344.025 53.5539 2 4 -4 10 360.454 57.7979 1 4 4 10 310.458 53.0634 3 -4 4 -10 342.294 57.7295 1 4 4 10 309.076 53.2232 4 4 4 10 324.953 53.3570 2 4 4 10 296.145 60.8084 1 5 -4 10 182.695 29.6696 4 5 -4 10 182.011 29.5640 3 5 -4 10 172.788 36.6882 1 -5 -4 -10 180.355 29.9208 2 5 -4 10 184.777 30.2679 2 -5 -4 -10 187.347 40.6793 1 5 4 10 187.450 29.5606 3 5 4 10 172.164 29.8001 4 5 4 10 138.045 40.0139 1 -5 4 -10 170.061 29.5101 3 5 4 10 178.105 29.9771 2 -5 4 -10 184.139 37.4370 1 6 -4 10 111.012 19.5151 4 6 -4 10 110.467 19.4123 3 6 -4 10 135.404 31.6006 1 -6 -4 -10 126.077 19.7931 2 6 -4 10 128.379 20.4527 2 -6 -4 -10 101.215 30.5477 1 6 4 10 115.867 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6.23045 6.36693 2 -2 3 54 7.75683 2.54676 4 1 -3 -54 16.0530 3.73856 3 -1 -3 54 11.9611 6.82347 2 -1 3 54 11.4235 7.09492 2 -1 3 54 21.5550 3.75386 4 0 -3 -54 -6.9732 60.9455 1 0 -3 -54 8.45334 2.36914 3 0 3 54 0.43281 6.32581 2 0 3 54 6.14293 2.50835 4 1 -3 54 7.69154 6.95809 2 -1 -3 -54 9.61985 2.75420 3 -1 -3 -54 -1.5708 64.5259 1 1 3 54 15.7344 3.14042 4 1 3 54 5.22153 7.19676 2 -2 -3 -54 1.56005 1.93885 3 2 -3 54 4.87203 6.33909 2 2 3 54 2.16863 2.51147 4 2 3 54 -1.9998 6.62884 2 3 -3 54 15.9063 3.19683 4 3 -3 54 11.9440 7.59351 2 3 3 54 14.4953 3.54660 4 3 3 54 15.0384 8.44876 2 3 -4 -54 -1.4997 2.42041 3 -3 -4 54 0.44097 5.41470 2 -3 4 54 0.71138 6.58887 2 -3 4 54 -3.8068 1.98950 4 2 -4 -54 4.67624 2.41891 3 -2 -4 54 4.33134 6.03418 2 -2 4 54 2.67033 6.70032 2 -2 4 54 -1.2899 2.26033 4 -1 -4 54 7.79755 7.02873 2 1 -4 -54 3.43068 2.29750 3 -1 4 54 0.17717 2.28909 4 -1 4 54 -0.7185 6.50465 2 0 -4 54 6.45939 6.85277 2 0 -4 -54 7.11592 2.62922 3 0 4 54 6.51346 7.03510 2 0 4 54 5.31419 2.75283 4 -1 -4 -54 0.57255 2.18541 3 1 -4 54 6.27876 6.64117 2 1 4 54 -0.6989 2.24558 4 1 4 54 1.71701 6.95735 2 -2 -4 -54 3.02425 2.18444 3 2 4 54 2.17457 2.46669 4 -5 0 55 3.69123 5.94078 2 5 0 -55 6.15372 2.34626 3 -4 0 55 -3.3419 5.48780 2 4 0 -55 2.49781 2.03766 3 -3 0 55 3.51591 5.82233 2 3 0 -55 7.60848 2.22074 3 -2 0 55 4.11940 5.60707 2 -2 0 55 -0.0889 0.97903 4 2 0 -55 2.75779 1.72392 3 -1 0 55 5.40298 6.14991 2 -1 0 55 8.53287 2.07499 4 1 0 -55 10.0119 2.02410 3 0 0 55 -0.6694 1.68888 4 0 0 55 1.67570 6.32205 2 1 0 55 0.79961 6.48234 2 1 0 55 0.72656 1.87852 4 2 0 55 2.01684 6.75828 2 2 0 55 -0.4412 1.99234 4 3 0 55 5.69629 2.30584 4 3 0 55 3.30810 7.32406 2 4 0 55 0.76118 2.33448 4 -4 -1 55 2.68306 5.59289 2 4 -1 -55 7.18573 2.29381 3 -4 1 55 2.64378 6.04766 2 4 1 -55 1.05107 2.01154 3 3 -1 -55 25.5238 4.39162 3 3 -1 -55 26.4173 4.29694 4 -3 -1 55 17.2922 7.68373 2 3 1 -55 19.7210 4.16224 3 -3 1 55 16.1068 7.71982 2 2 -1 -55 0.47478 1.96540 3 -2 -1 55 5.25387 6.04207 2 2 1 -55 1.20231 1.33855 3 -2 1 55 3.58896 6.38946 2 -2 1 55 1.60737 1.59463 4 1 -1 -55 27.9024 4.76351 3 -1 -1 55 15.9694 8.26017 2 1 -1 -55 30.1350 67.7854 1 -1 1 55 29.5541 5.06634 4 -1 1 55 22.3754 7.67493 2 0 -1 55 -1.7349 6.04622 2 0 -1 -55 3.11940 1.56178 3 0 -1 55 4.94213 1.62275 4 0 1 55 3.77004 2.11035 4 0 1 55 1.51396 6.60194 2 1 -1 55 22.6592 4.30307 4 1 -1 55 21.9223 7.73973 2 1 1 55 18.1803 9.16938 2 1 1 55 24.3237 4.53570 4 2 -1 55 0.49921 7.06664 2 2 -1 55 4.75875 2.08138 4 2 1 55 3.69407 2.31606 4 2 1 55 -0.3258 6.30903 2 3 -1 55 18.1948 3.70984 4 3 1 55 15.9385 3.93501 4 4 -2 -55 21.3701 4.00785 3 4 -2 -55 19.4201 3.57686 4 -4 -2 55 15.0434 6.60301 2 4 2 -55 17.2675 3.50105 3 -4 2 55 14.8989 7.56772 2 3 -2 -55 -0.2727 2.13330 3 -3 -2 55 -0.7550 5.56630 2 3 2 -55 0.70752 1.37853 3 -3 2 55 1.08749 1.41407 4 -3 2 55 -1.2167 6.15110 2 -3 2 55 15.6564 57.4653 1 2 -2 -55 26.7760 47.1367 1 2 -2 -55 17.2073 3.68933 3 -2 -2 55 12.4067 7.06265 2 -2 2 55 15.2126 6.97456 2 -2 2 55 20.1229 3.68259 4 -1 -2 55 3.60530 6.06141 2 1 -2 -55 18.4628 45.0162 1 1 -2 -55 42.6566 64.0043 1 1 -2 -55 4.41101 2.07806 3 -1 2 55 0.76868 6.11964 2 -1 2 55 3.30023 2.05310 4 0 -2 55 17.4600 7.05229 2 0 -2 -55 20.3126 45.9098 1 0 -2 -55 -4.3649 58.4236 1 0 2 55 21.8594 7.80571 2 0 2 55 22.5268 4.25170 4 1 -2 55 -0.7883 5.81028 2 1 2 55 3.33293 6.74428 2 1 2 55 1.33996 2.17199 4 2 -2 55 13.0228 6.67578 2 2 -2 55 11.6835 2.75834 4 2 2 55 11.5968 3.08175 4 2 2 55 11.7394 7.29654 2 3 -2 55 1.04915 1.93397 4 3 -2 55 -1.2368 6.57789 2 3 2 55 3.45053 7.47763 2 3 2 55 -1.0535 2.38962 4 3 -3 -55 2.97860 2.36973 3 -3 -3 55 3.91379 5.77115 2 -3 3 55 -2.3383 6.37761 2 -3 3 55 0.78834 1.85541 4 2 -3 -55 -2.0269 2.09822 3 -2 -3 55 4.59150 6.04175 2 -2 3 55 3.57096 2.12660 4 -2 3 55 0.74535 6.17767 2 -1 -3 55 0.79471 6.43763 2 1 -3 -55 0.49696 2.20930 3 -1 3 55 0.39701 2.15156 4 -1 3 55 3.98996 6.43952 2 0 -3 55 -0.7993 5.78468 2 0 -3 -55 -1.5813 2.08171 3 0 3 55 -0.7525 2.09740 4 0 3 55 -3.9128 5.60784 2 1 -3 55 0.64221 5.91291 2 1 3 55 1.09925 6.39742 2 1 3 55 2.14461 2.46025 4 2 -3 55 1.54703 6.26688 2 2 3 55 -3.5397 2.14837 4 2 3 55 -2.1770 7.24839 2 2 -4 -55 6.14044 2.64269 3 -2 4 55 3.80715 2.38461 4 -2 4 55 2.34717 6.68203 2 1 -4 -55 -0.1993 2.50074 3 -1 -4 55 2.26441 5.84333 2 -1 4 55 -0.8539 6.00566 2 -1 4 55 0.82509 2.23258 4 0 -4 -55 0.88234 2.23888 3 0 -4 55 -5.7474 6.02690 2 0 4 55 -2.4668 6.39094 2 0 4 55 3.17028 2.27229 4 1 4 55 2.86632 2.43883 4 4 0 -56 19.7127 4.02352 3 -4 0 56 20.0570 7.21635 2 -3 0 56 -1.8636 5.63057 2 3 0 -56 -2.7440 1.78673 3 2 0 -56 39.8928 6.83615 3 -2 0 56 34.2064 10.0190 2 -1 0 56 0.79377 6.02244 2 -1 0 56 0.45844 1.45270 4 0 0 56 37.5722 6.57373 4 0 0 56 32.2873 9.42907 2 1 0 56 -4.3152 6.75037 2 1 0 56 -1.1910 1.80280 4 2 0 56 32.0597 5.98162 4 3 0 56 1.62235 2.04827 4 3 0 56 -2.6286 7.11583 2 4 -1 -56 2.49213 2.03401 3 -4 -1 56 2.06797 5.39932 2 -4 1 56 4.47495 5.86775 2 4 1 -56 -0.3167 1.82122 3 3 -1 -56 6.21599 1.81885 4 -3 -1 56 6.46426 5.81074 2 3 -1 -56 5.74369 2.39290 3 3 1 -56 6.32770 1.99141 3 -3 1 56 7.76411 6.23884 2 -2 -1 56 -0.1679 5.91449 2 2 -1 -56 3.62743 1.93841 3 -2 1 56 3.89398 1.66983 4 -2 1 56 0.97443 6.23832 2 -1 -1 56 11.1329 7.13602 2 1 -1 -56 10.2438 2.88108 3 -1 1 56 18.0137 3.09442 4 -1 1 56 10.3752 7.56271 2 0 -1 56 -1.6525 5.92144 2 0 1 56 2.23465 1.91728 4 0 1 56 -0.2449 6.53734 2 1 -1 56 14.2234 3.07418 4 1 1 56 12.2116 7.90341 2 1 1 56 14.6372 3.34892 4 2 -1 56 -4.0120 5.89831 2 2 -1 56 1.70007 1.80342 4 2 1 56 2.37293 6.77420 2 2 1 56 1.09553 2.15223 4 3 -1 56 8.15240 2.34547 4 3 -1 56 8.09372 6.57607 2 3 1 56 2.64996 2.31615 4 4 -2 -56 1.38901 1.67417 4 3 -2 -56 6.63218 2.40468 3 -3 -2 56 2.81621 5.72201 2 -3 2 56 1.54106 6.23784 2 -3 2 56 4.40639 1.55730 4 2 -2 -56 1.49617 2.10381 3 -2 -2 56 3.25903 5.48869 2 -2 2 56 -4.9457 5.74988 2 -2 2 56 1.20798 1.87383 4 1 -2 -56 -58.260 58.2024 1 1 -2 -56 5.41285 2.19040 3 -1 -2 56 2.97481 5.57866 2 -1 2 56 4.88131 2.19852 4 -1 2 56 -1.5447 6.15937 2 0 -2 -56 7.43032 2.24135 3 0 -2 56 4.07865 7.29410 2 0 2 56 6.85407 6.35466 2 0 2 56 7.42752 2.44827 4 1 2 56 2.34406 6.50165 2 1 2 56 0.93480 2.26743 4 2 -2 56 1.22103 1.70312 4 2 -2 56 0.17506 7.33468 2 2 2 56 0.44621 6.38665 2 2 2 56 -0.6988 2.12128 4 -3 3 56 15.3665 3.24869 4 2 -3 -56 5.49387 2.43874 3 -2 -3 56 -1.2821 5.10490 2 -2 3 56 -3.7897 6.14989 2 -2 3 56 -0.7829 2.10625 4 1 -3 -56 9.02378 3.43493 3 -1 -3 56 17.9290 6.74285 2 -1 3 56 14.0513 7.43942 2 -1 3 56 19.2396 3.63420 4 0 -3 -56 1.52843 2.17755 3 0 -3 56 -1.0261 5.72951 2 0 3 56 2.34502 2.16320 4 0 3 56 1.98310 6.37932 2 1 -3 56 4.38003 6.26606 2 1 3 56 11.3758 2.80909 4 1 3 56 6.40180 6.59840 2 3 0 -57 5.96607 2.09131 3 -3 0 57 2.11758 5.91969 2 -2 0 57 2.14373 6.29408 2 2 0 -57 -0.8589 1.64684 3 -1 0 57 4.75592 6.86269 2 0 0 57 -0.2102 5.48032 2 0 0 57 2.35658 1.77232 4 1 0 57 2.89061 2.00894 4 1 0 57 2.09515 6.23732 2 2 0 57 1.14376 2.02533 4 2 0 57 -0.7802 7.68882 2 -3 -1 57 12.7137 6.61243 2 3 -1 -57 11.1367 2.71529 3 -3 1 57 12.1525 6.93332 2 3 1 -57 7.47284 2.36577 3 2 -1 -57 -1.3150 1.75024 3 -2 -1 57 -1.9376 6.07212 2 -2 1 57 -0.7170 6.33534 2 -2 1 57 1.02749 1.56043 4 -1 -1 57 11.8647 7.46344 2 1 -1 -57 14.1756 3.19340 3 -1 1 57 18.3773 7.52210 2 -1 1 57 17.5434 3.35319 4 0 -1 57 -1.6671 5.65227 2 0 1 57 0.05416 1.94348 4 0 1 57 1.39825 6.37384 2 1 -1 57 15.6917 7.53642 2 1 -1 57 23.8125 4.02683 4 1 1 57 10.6135 7.68806 2 1 1 57 22.9365 4.28687 4 2 -1 57 2.64861 1.86037 4 2 1 57 1.02101 6.96578 2 2 1 57 0.74249 2.08227 4 3 -2 -57 1.68560 2.08576 3 -3 -2 57 1.26839 5.30152 2 -3 2 57 -1.3512 5.96682 2 -3 2 57 3.50034 1.44082 4 -2 -2 57 9.97515 6.02042 2 2 -2 -57 13.7531 2.89700 3 -2 2 57 8.79228 2.58725 4 -2 2 57 3.04071 6.50329 2 -1 -2 57 -4.4697 5.84262 2 1 -2 -57 -0.2610 1.99022 3 -1 2 57 2.44874 2.04056 4 -1 2 57 4.65531 6.47199 2 0 2 57 14.3793 7.95648 2 0 2 57 25.6574 4.54380 4 1 -2 57 1.00040 5.79122 2 1 2 57 5.58890 7.52433 2 1 2 57 2.34118 2.23795 4 2 2 57 19.2118 4.18752 4 -1 -3 57 0.21362 6.44511 2 1 -3 -57 -1.0687 2.17909 3 -1 3 57 2.62538 6.36419 2 -1 3 57 -1.0275 2.08764 4 0 -3 57 -3.5503 6.58107 2 0 3 57 1.50004 6.57198 2 0 3 57 2.74446 2.35316 4 -3 0 58 0.84949 5.19327 2 3 0 -58 -2.4768 1.90508 3 -2 0 58 24.8219 8.48111 2 -1 0 58 2.97493 6.69361 2 0 0 58 9.11206 6.86380 2 0 0 58 16.3782 3.15138 4 1 0 58 1.35631 1.82511 4 1 0 58 2.13133 6.46685 2 2 0 58 28.5142 5.37119 4 3 -1 -58 2.17651 1.96894 3 -2 -1 58 -3.0366 5.16285 2 2 -1 -58 2.37770 1.82926 3 -2 1 58 2.17137 6.17985 2 -1 -1 58 1.16321 6.05717 2 -1 1 58 8.67386 2.21792 4 -1 1 58 8.83224 7.08755 2 0 -1 58 -1.4603 6.45933 2 0 1 58 3.75623 2.01087 4 0 1 58 0.09623 7.12850 2 1 -1 58 9.77229 6.66272 2 1 1 58 13.8129 3.03451 4 1 1 58 7.21245 6.70401 2 -2 -2 58 -2.1323 5.41090 2 2 -2 -58 1.38276 2.12368 3 -2 2 58 2.02170 1.89960 4 -2 2 58 0.30351 6.00709 2 -1 -2 58 -2.1978 6.80277 2 1 -2 -58 2.53788 2.06600 3 -1 2 58 0.17742 1.94640 4 -1 2 58 2.76255 6.85201 2 0 -2 58 2.53749 6.73336 2 0 2 58 1.45111 2.19910 4 0 2 58 2.63858 6.59174 2 1 2 58 1.97302 2.22053 4 -1 0 59 1.73297 5.70847 2 0 0 59 -0.0254 7.08685 2 1 0 59 2.46930 1.95504 4 -1 -1 59 11.0678 6.74203 2 -1 1 59 1.28839 6.35410 2 -1 1 59 4.48274 1.98748 4 0 1 59 -1.0430 1.94537 4 0 1 59 4.66434 6.45999 2 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 0.0695 _exptl_absorpt_correction_T_min 0.0141 _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 0.71079 8.341 7.832 41.597 90.002 92.920 90.052 ) ; _shelx_hkl_checksum 76558