data_nims_pzdi_1 _audit_creation_date 2023-09-28 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'I4 Pb, 3(C2 H6 O S), C4 H12 N2' _chemical_formula_sum 'C10 H30 I4 N2 O3 Pb S3' _chemical_formula_weight 1037.33 _chemical_absolute_configuration ? _chemical_melting_point ? _chemical_oxdiff_formula PbI2C8N4H24 _chemical_oxdiff_usercomment 'PdI2 + PZDI 1:2 (sample #1)' 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' 'I' 'I' -0.4742 1.8119 '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' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system 'orthorhombic' _space_group_IT_number 33 _space_group_name_H-M_alt 'P n a 21' _space_group_name_Hall 'P 2c -2n' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 20.3941(3) _cell_length_b 13.7425(2) _cell_length_c 19.2851(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5404.96(14) _cell_formula_units_Z 8 _cell_measurement_reflns_used 27916 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 31.1950 _cell_measurement_theta_min 2.6940 _shelx_estimated_absorpt_T_max 0.436 _shelx_estimated_absorpt_T_min 0.113 _exptl_absorpt_coefficient_mu 11.055 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.123 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.550 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description ? _exptl_crystal_F_000 3760 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 1 0 0.0880 0 -1 0 0.0838 24 -4 10 0.1449 -25 -13 0 0.1279 11 -12 -16 0.0276 -7 -15 -15 0.0732 -1 16 -16 0.1210 3 -27 1 0.0800 -2 -16 16 0.1023 9 9 17 0.1068 -2 -26 6 0.0850 6 24 -9 0.1012 -21 10 -11 0.1884 -17 2 15 0.0596 -14 13 14 0.0703 -13 5 17 0.0553 1 11 18 0.0673 -5 10 18 0.0444 -3 26 -4 0.1087 -8 19 13 0.0689 21 -19 -1 0.1154 9 21 11 0.1242 16 -22 -4 0.0886 8 17 -14 0.0944 23 16 3 0.1763 _exptl_crystal_size_max 0.354 _exptl_crystal_size_mid 0.192 _exptl_crystal_size_min 0.089 loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z -0.0001 0.9994 0.0001 0.0195 0.0036 0.0309 0.0001 -0.9994 -0.0001 -0.0195 -0.0036 -0.0309 24.2577 -4.1460 9.9727 0.2094 0.8841 -0.4178 -25.2991 -12.9088 -0.2767 -0.1208 -0.9171 -0.3799 11.0801 -11.5890 -15.8595 -0.9696 0.2317 0.0785 -6.5479 -15.3282 -15.3848 -0.9225 -0.3837 -0.0422 -0.5043 15.8636 -15.7310 -0.3620 -0.0648 0.9299 2.9909 -27.0116 0.8804 -0.5070 0.0099 -0.8619 -1.6696 -16.1174 15.5624 0.3622 -0.0119 -0.9320 9.3038 8.7592 17.2397 0.8581 0.4667 -0.2141 -2.0050 -25.5790 6.4221 -0.2130 -0.1192 -0.9698 5.6135 23.5963 -8.8470 0.0498 0.2195 0.9743 -20.6499 9.9518 -11.4657 -0.1805 -0.7491 0.6374 -17.2497 1.5816 15.4610 0.7919 -0.4826 -0.3742 -13.8546 13.2351 14.1190 0.9428 -0.3325 0.0223 -12.9805 4.7960 16.9489 0.8944 -0.3144 -0.3182 0.6681 11.1865 17.6562 0.9723 0.1820 -0.1466 -5.2355 10.4651 17.5336 0.9864 -0.0240 -0.1627 -3.4951 26.3972 -3.9929 0.3643 -0.0503 0.9299 -8.2142 18.5714 13.0262 0.9683 -0.1268 0.2153 20.7611 -18.7115 -1.3652 -0.5418 0.6349 -0.5507 8.7473 21.1025 10.7026 0.8220 0.4489 0.3504 15.5969 -22.0505 -4.2454 -0.7014 0.4263 -0.5713 8.3843 16.7790 -14.1585 -0.3270 0.2541 0.9102 22.9552 15.8309 2.9664 0.3066 0.8654 0.3964 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_unetI/netI 0.0321 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.909 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 134993 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.858 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.909 _diffrn_reflns_theta_min 1.997 _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.909 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -21.00 57.00 0.25 0.50 -- -5.40 34.00-122.24 312 2 \w -21.00 68.00 0.25 0.50 -- -5.40 34.00 2.62 356 3 \w -21.00 61.00 0.25 0.50 -- -5.40 34.00 57.47 328 4 \w -20.00 69.00 0.25 0.50 -- -5.40 32.00 120.01 356 5 \w -21.00 67.00 0.25 0.50 -- -5.40 31.00 169.73 352 6 \w -21.00 66.00 0.25 0.50 -- -5.40 30.00 -63.37 348 7 \w -17.00 25.00 0.25 0.50 -- -5.40 -99.00 30.00 168 8 \w -12.00 28.00 0.25 0.50 -- -5.40 -99.00 90.00 160 9 \w -14.00 22.00 0.25 0.50 -- -5.40 -99.00 150.00 144 10 \w -16.00 24.00 0.25 0.50 -- -5.40 -99.00 -30.00 160 11 \w -15.00 28.00 0.25 0.50 -- -5.40 -99.00 -90.00 172 12 \w -13.00 27.00 0.25 0.50 -- -5.40 -99.00-150.00 160 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0056638000 _diffrn_orient_matrix_UB_12 0.0195415000 _diffrn_orient_matrix_UB_13 0.0429020000 _diffrn_orient_matrix_UB_21 0.0343142000 _diffrn_orient_matrix_UB_22 0.0036510000 _diffrn_orient_matrix_UB_23 0.0066990000 _diffrn_orient_matrix_UB_31 -0.0004692000 _diffrn_orient_matrix_UB_32 0.0309467000 _diffrn_orient_matrix_UB_33 -0.0278906000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Mo) X-ray Source' _reflns_Friedel_coverage 0.840 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.806 _reflns_number_gt 13163 _reflns_number_total 14685 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.42.90a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 1.676 _refine_diff_density_min -1.370 _refine_diff_density_rms 0.154 _refine_ls_abs_structure_details ; Flack x determined using 5184 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.089(2) _refine_ls_extinction_coef 0.000248(15) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 475 _refine_ls_number_reflns 14685 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0434 _refine_ls_restrained_S_all 1.151 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+24.8727P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0939 _refine_ls_wR_factor_ref 0.0961 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H,H) groups 2. Restrained distances S00G-O00L \\sim S00H-O00L with sigma of 0.02 S00E-C6 \\sim S1-C6 with sigma of 0.02 S00B-C1 \\sim S00B-C1A with sigma of 0.02 S00G-C3 \\sim S00H-C3 with sigma of 0.02 S00E-C4 \\sim S1-C4 with sigma of 0.02 S00G-C016 \\sim S00H-C016 with sigma of 0.02 S00B-O00O \\sim S00B-O00P with sigma of 0.02 S00B-C2 \\sim S00B-C2A with sigma of 0.02 S00E-O00I \\sim S1-O00I with sigma of 0.02 3. Uiso/Uaniso restraints and constraints S1 \\sim O00I \\sim C6 \\sim C4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A S00B \\sim C1A \\sim C2A \\sim O00P: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04 within 2A 4. Rigid body (RIGU) restrains S00B, C1A, C2A, O00P with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 5. Others Sof(H01D)=Sof(H01E)=Sof(H01F)=Sof(H3BD)=Sof(H3BE)=Sof(H3BF)=Sof(S00H)=1-FVAR(1) Sof(S00G)=Sof(H01A)=Sof(H01B)=Sof(H01C)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1) Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)= Sof(O00P)=1-FVAR(2) Sof(O00O)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2)=Sof(H2A)=Sof(H2B)= Sof(H2C)=FVAR(2) Sof(H6BD)=Sof(H6BE)=Sof(H6BF)=Sof(H4BD)=Sof(H4BE)=Sof(H4BF)=Sof(S1)=1-FVAR(3) Sof(S00E)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(H4AA)=Sof(H4AB)=Sof(H4AC)=FVAR(3) 6.a Secondary CH2 refined with riding coordinates: N00H(H00A,H00B), N00J(H00M,H00N), C00M(H00O,H00P), N00N(H00Q,H00R), N00P(H00C, H00D), C00R(H00E,H00F), C00S(H00S,H00T), C00T(H00U,H00V), C00U(H00W,H00X), C00X(H00G,H00H), C00Y(H00I,H00J), C00Z(H00K,H00L) 6.b Me refined with riding coordinates: C3(H3AA,H3AB,H3AC), C3(H3BD,H3BE,H3BF), C6(H6AA,H6AB,H6AC), C6(H6BD,H6BE, H6BF), C4(H4AA,H4AB,H4AC), C4(H4BD,H4BE,H4BF) 6.c Idealised Me refined as rotating group: C00W(H00Y,H,HA), C010(H01G,H01H,H01I), C013(H01M,H01N,H01O), C014(H01J,H01K, H01L), C015(H01P,H01Q,H01R), C016(H01A,H01B,H01C), C016(H01D,H01E,H01F), C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C1A(H1AA,H1AB,H1AC), C2A(H2AA,H2AB,H2AC) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 Pb01 Pb 0.37401(2) -0.22121(4) 0.46363(2) 0.03938(11) Uani 1 1 d . . . . . Pb02 Pb 0.37620(2) 0.27311(4) 0.46592(2) 0.03925(11) Uani 1 1 d . . . . . I003 I 0.26965(5) 0.24150(7) 0.57216(6) 0.0487(2) Uani 1 1 d . . . . . I004 I 0.25852(5) -0.22502(7) 0.35818(5) 0.0502(2) Uani 1 1 d . . . . . I005 I 0.25658(4) 0.28016(8) 0.34950(5) 0.0505(2) Uani 1 1 d . . . . . I006 I 0.37021(5) 0.49508(7) 0.47648(7) 0.0549(3) Uani 1 1 d . . . . . I007 I 0.49392(4) -0.21460(8) 0.58188(5) 0.0542(3) Uani 1 1 d . . . . . I008 I 0.49451(5) 0.26633(8) 0.56859(6) 0.0526(3) Uani 1 1 d . . . . . I009 I 0.38202(5) -0.00130(7) 0.45541(8) 0.0586(3) Uani 1 1 d . . . . . I00A I 0.48212(5) -0.25271(7) 0.35958(6) 0.0466(2) Uani 1 1 d . . . . . S00B S 0.5662(2) 0.5509(3) 0.2425(2) 0.0648(11) Uani 1 1 d D U . . . S00C S 0.48885(19) 0.2859(3) 0.3037(2) 0.0579(9) Uani 1 1 d . . . . . S00D S 0.24269(18) 0.3007(3) 0.1257(2) 0.0545(8) Uani 1 1 d . . . . . S00E S 0.5757(7) -0.0615(7) 0.2429(6) 0.073(4) Uani 0.53(3) 1 d D . P A 1 S00F S 0.3151(3) -0.0606(3) 0.1875(2) 0.0673(11) Uani 1 1 d . . . . . S00G S 0.3248(3) 0.5547(4) 0.1892(3) 0.0542(18) Uani 0.685(13) 1 d D . P B 1 N00H N 0.6884(5) 0.0457(8) 0.4870(6) 0.044(2) Uani 1 1 d . . . . . H00A H 0.722602 0.082440 0.475327 0.053 Uiso 1 1 calc R U . . . H00B H 0.690947 0.033565 0.532214 0.053 Uiso 1 1 calc R U . . . O00I O 0.5814(7) -0.0010(9) 0.3115(7) 0.078(3) Uani 1 1 d D U . . . N00J N 0.6774(5) 0.5467(7) 0.4962(6) 0.043(2) Uani 1 1 d . . . . . H00M H 0.711210 0.587678 0.494541 0.051 Uiso 1 1 calc R U . . . H00N H 0.674349 0.524246 0.539367 0.051 Uiso 1 1 calc R U . . . O00K O 0.3187(7) 0.0042(9) 0.1241(6) 0.075(4) Uani 1 1 d . . . . . O00L O 0.3505(7) 0.4962(9) 0.1303(6) 0.073(3) Uani 1 1 d D . . . . C00M C 0.6895(6) 0.4654(9) 0.4489(7) 0.044(3) Uani 1 1 d . . . . . H00O H 0.728749 0.430844 0.462947 0.053 Uiso 1 1 calc R U . . . H00P H 0.696169 0.489848 0.402217 0.053 Uiso 1 1 calc R U . . . N00N N 0.5702(5) 0.4482(7) 0.4315(6) 0.043(2) Uani 1 1 d . . . . . H00Q H 0.536418 0.407315 0.433236 0.051 Uiso 1 1 calc R U . . . H00R H 0.573436 0.470550 0.388286 0.051 Uiso 1 1 calc R U . . . O00O O 0.6033(19) 0.490(3) 0.293(2) 0.079(11) Uani 0.59(3) 1 d D . P C 1 N00P N 0.5701(5) -0.0526(7) 0.4453(6) 0.043(2) Uani 1 1 d . . . . . H00C H 0.535148 -0.089338 0.454175 0.051 Uiso 1 1 calc R U . . . H00D H 0.569338 -0.036916 0.400491 0.051 Uiso 1 1 calc R U . . . O00Q O 0.2431(6) 0.3019(11) 0.0459(6) 0.087(4) Uani 1 1 d . . . . . C00R C 0.6913(6) -0.0450(9) 0.4492(8) 0.051(3) Uani 1 1 d . . . . . H00E H 0.729682 -0.081147 0.463951 0.061 Uiso 1 1 calc R U . . . H00F H 0.695929 -0.031235 0.400126 0.061 Uiso 1 1 calc R U . . . C00S C 0.6164(6) 0.5998(8) 0.4782(8) 0.043(3) Uani 1 1 d . . . . . H00S H 0.620353 0.627242 0.432028 0.052 Uiso 1 1 calc R U . . . H00T H 0.609685 0.652809 0.510613 0.052 Uiso 1 1 calc R U . . . C00T C 0.5586(6) 0.5320(9) 0.4806(9) 0.051(3) Uani 1 1 d . . . . . H00U H 0.519083 0.566567 0.467361 0.061 Uiso 1 1 calc R U . . . H00V H 0.552808 0.507550 0.527399 0.061 Uiso 1 1 calc R U . . . C00U C 0.6307(6) 0.3963(8) 0.4500(7) 0.044(3) Uani 1 1 d . . . . . H00W H 0.637982 0.343530 0.417502 0.053 Uiso 1 1 calc R U . . . H00X H 0.626093 0.368364 0.495982 0.053 Uiso 1 1 calc R U . . . C00W C 0.3206(6) 0.2578(10) 0.1508(9) 0.048(3) Uani 1 1 d . . . . . H00Y H 0.325819 0.191627 0.135825 0.073 Uiso 1 1 calc R U . . . H H 0.324566 0.261003 0.200340 0.073 Uiso 1 1 calc R U . . . HA H 0.353956 0.297454 0.129862 0.073 Uiso 1 1 calc R U . . . C00X C 0.6269(6) 0.1001(9) 0.4724(9) 0.051(3) Uani 1 1 d . . . . . H00G H 0.625800 0.118239 0.423851 0.061 Uiso 1 1 calc R U . . . H00H H 0.626279 0.159370 0.499760 0.061 Uiso 1 1 calc R U . . . C00Y C 0.5674(6) 0.0402(9) 0.4893(8) 0.046(3) Uani 1 1 d . . . . . H00I H 0.527823 0.076630 0.478925 0.056 Uiso 1 1 calc R U . . . H00J H 0.567041 0.023698 0.538244 0.056 Uiso 1 1 calc R U . . . C00Z C 0.6300(6) -0.1076(9) 0.4606(8) 0.047(3) Uani 1 1 d . . . . . H00K H 0.632017 -0.164508 0.430893 0.057 Uiso 1 1 calc R U . . . H00L H 0.628754 -0.129766 0.508353 0.057 Uiso 1 1 calc R U . . . C010 C 0.5666(8) 0.2477(10) 0.2796(10) 0.057(4) Uani 1 1 d . . . . . H01G H 0.597274 0.299735 0.286710 0.086 Uiso 1 1 calc R U . . . H01H H 0.566347 0.229675 0.231520 0.086 Uiso 1 1 calc R U . . . H01I H 0.579103 0.192698 0.307228 0.086 Uiso 1 1 calc R U . . . O011 O 0.4883(7) 0.2987(10) 0.3802(6) 0.087(4) Uani 1 1 d . . . . . C013 C 0.1938(8) 0.1961(12) 0.1485(8) 0.068(4) Uani 1 1 d . . . . . H01M H 0.148457 0.209510 0.139059 0.101 Uiso 1 1 calc R U . . . H01N H 0.199174 0.182137 0.196947 0.101 Uiso 1 1 calc R U . . . H01O H 0.207685 0.141017 0.121659 0.101 Uiso 1 1 calc R U . . . C014 C 0.4501(8) 0.1741(13) 0.2869(8) 0.075(5) Uani 1 1 d . . . . . H01J H 0.449925 0.162195 0.237838 0.112 Uiso 1 1 calc R U . . . H01K H 0.405825 0.176343 0.303651 0.112 Uiso 1 1 calc R U . . . H01L H 0.473455 0.122851 0.309968 0.112 Uiso 1 1 calc R U . . . C015 C 0.2970(10) 0.0195(13) 0.2565(7) 0.079(5) Uani 1 1 d . . . . . H01P H 0.324084 0.076475 0.252936 0.118 Uiso 1 1 calc R U . . . H01Q H 0.305435 -0.012437 0.299892 0.118 Uiso 1 1 calc R U . . . H01R H 0.251694 0.038151 0.254300 0.118 Uiso 1 1 calc R U . . . C016 C 0.3702(8) 0.6602(12) 0.1945(9) 0.066(4) Uani 1 1 d D . . . . H01A H 0.416001 0.644401 0.195522 0.099 Uiso 0.685(13) 1 calc R U P B 1 H01B H 0.358637 0.694686 0.236069 0.099 Uiso 0.685(13) 1 calc R U P B 1 H01C H 0.361106 0.700353 0.154922 0.099 Uiso 0.685(13) 1 calc R U P B 1 H01D H 0.354092 0.686915 0.151776 0.099 Uiso 0.315(13) 1 calc R U P B 2 H01E H 0.408610 0.695197 0.208779 0.099 Uiso 0.315(13) 1 calc R U P B 2 H01F H 0.336976 0.665893 0.229596 0.099 Uiso 0.315(13) 1 calc R U P B 2 C5 C 0.3984(14) -0.086(2) 0.2077(14) 0.149(13) Uani 1 1 d . . . . . H5A H 0.413655 -0.138903 0.179214 0.224 Uiso 1 1 calc R U . . . H5B H 0.401985 -0.104072 0.255632 0.224 Uiso 1 1 calc R U . . . H5C H 0.424641 -0.029465 0.198997 0.224 Uiso 1 1 calc R U . . . C3 C 0.3559(13) 0.5006(18) 0.2688(11) 0.133(11) Uani 1 1 d D . . . . H3AA H 0.340061 0.536879 0.307925 0.200 Uiso 0.685(13) 1 calc R U P B 1 H3AB H 0.340984 0.434447 0.272161 0.200 Uiso 0.685(13) 1 calc R U P B 1 H3AC H 0.402923 0.501795 0.268382 0.200 Uiso 0.685(13) 1 calc R U P B 1 H3BD H 0.381068 0.529507 0.305454 0.200 Uiso 0.315(13) 1 calc R U P B 2 H3BE H 0.310923 0.520591 0.272816 0.200 Uiso 0.315(13) 1 calc R U P B 2 H3BF H 0.358477 0.430969 0.272188 0.200 Uiso 0.315(13) 1 calc R U P B 2 S00H S 0.3893(9) 0.5408(12) 0.1829(8) 0.096(7) Uani 0.315(13) 1 d D . P B 2 C1 C 0.5371(19) 0.481(2) 0.1715(16) 0.073(9) Uani 0.59(3) 1 d D . P C 1 H1A H 0.557330 0.418357 0.172117 0.109 Uiso 0.59(3) 1 calc R U P C 1 H1B H 0.547800 0.513984 0.128956 0.109 Uiso 0.59(3) 1 calc R U P C 1 H1C H 0.490396 0.474301 0.175034 0.109 Uiso 0.59(3) 1 calc R U P C 1 C2 C 0.6369(12) 0.590(3) 0.1984(17) 0.079(11) Uani 0.59(3) 1 d D . P C 1 H2A H 0.670249 0.606742 0.231407 0.119 Uiso 0.59(3) 1 calc R U P C 1 H2B H 0.626474 0.646057 0.170744 0.119 Uiso 0.59(3) 1 calc R U P C 1 H2C H 0.652457 0.538727 0.168918 0.119 Uiso 0.59(3) 1 calc R U P C 1 C1A C 0.582(4) 0.491(3) 0.1632(16) 0.084(14) Uani 0.41(3) 1 d D U P C 2 H1AA H 0.621566 0.452442 0.167632 0.126 Uiso 0.41(3) 1 calc R U P C 2 H1AB H 0.587924 0.537711 0.127010 0.126 Uiso 0.41(3) 1 calc R U P C 2 H1AC H 0.546172 0.448596 0.152027 0.126 Uiso 0.41(3) 1 calc R U P C 2 C2A C 0.6135(14) 0.653(2) 0.2323(16) 0.040(8) Uani 0.41(3) 1 d D U P C 2 H2AA H 0.625157 0.678685 0.277028 0.060 Uiso 0.41(3) 1 calc R U P C 2 H2AB H 0.589235 0.701490 0.207022 0.060 Uiso 0.41(3) 1 calc R U P C 2 H2AC H 0.652649 0.637017 0.207164 0.060 Uiso 0.41(3) 1 calc R U P C 2 O00P O 0.583(3) 0.480(4) 0.298(2) 0.068(12) Uani 0.41(3) 1 d D U P C 2 C6 C 0.6160(16) -0.161(3) 0.229(2) 0.211(16) Uani 1 1 d D U . . . H6AA H 0.605045 -0.185236 0.183534 0.317 Uiso 0.53(3) 1 calc R U P A 1 H6AB H 0.662219 -0.147324 0.230676 0.317 Uiso 0.53(3) 1 calc R U P A 1 H6AC H 0.604841 -0.207994 0.263189 0.317 Uiso 0.53(3) 1 calc R U P A 1 H6BD H 0.651418 -0.171879 0.196798 0.317 Uiso 0.47(3) 1 calc R U P A 2 H6BE H 0.617761 -0.207776 0.265259 0.317 Uiso 0.47(3) 1 calc R U P A 2 H6BF H 0.574999 -0.166143 0.204573 0.317 Uiso 0.47(3) 1 calc R U P A 2 C4 C 0.6180(16) 0.010(2) 0.1812(12) 0.193(16) Uani 1 1 d D U . . . H4AA H 0.616935 -0.021907 0.136930 0.289 Uiso 0.53(3) 1 calc R U P A 1 H4AB H 0.597278 0.072568 0.177469 0.289 Uiso 0.53(3) 1 calc R U P A 1 H4AC H 0.662672 0.018304 0.195646 0.289 Uiso 0.53(3) 1 calc R U P A 1 H4BD H 0.643098 -0.022248 0.145932 0.289 Uiso 0.47(3) 1 calc R U P A 2 H4BE H 0.573087 0.014866 0.166596 0.289 Uiso 0.47(3) 1 calc R U P A 2 H4BF H 0.635373 0.074093 0.188688 0.289 Uiso 0.47(3) 1 calc R U P A 2 S1 S 0.6224(13) -0.0576(13) 0.2595(7) 0.125(7) Uani 0.47(3) 1 d D U P A 2 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 Pb01 0.0311(2) 0.0500(2) 0.0370(2) 0.0075(3) 0.00154(18) 0.00209(17) Pb02 0.0291(2) 0.0537(2) 0.0350(2) -0.0058(3) 0.00307(17) -0.00236(18) I003 0.0483(6) 0.0595(5) 0.0384(5) 0.0032(4) 0.0123(5) -0.0007(4) I004 0.0441(5) 0.0582(5) 0.0484(6) 0.0086(5) -0.0107(4) -0.0084(4) I005 0.0436(5) 0.0719(6) 0.0358(5) -0.0011(4) -0.0022(3) -0.0075(4) I006 0.0421(4) 0.0501(4) 0.0724(8) 0.0051(5) -0.0107(4) -0.0052(3) I007 0.0420(5) 0.0831(7) 0.0374(5) 0.0121(5) -0.0013(4) -0.0005(4) I008 0.0431(5) 0.0616(5) 0.0531(6) -0.0112(5) -0.0118(4) 0.0135(4) I009 0.0454(5) 0.0454(4) 0.0851(9) -0.0052(5) -0.0110(5) 0.0051(3) I00A 0.0413(5) 0.0563(5) 0.0421(6) -0.0075(4) 0.0056(4) 0.0012(4) S00B 0.085(3) 0.060(2) 0.050(2) -0.0068(17) 0.000(2) 0.007(2) S00C 0.057(2) 0.068(2) 0.049(2) -0.0134(17) 0.0079(15) -0.0039(17) S00D 0.057(2) 0.056(2) 0.0503(19) 0.0065(16) -0.0021(15) -0.0014(16) S00E 0.089(9) 0.075(6) 0.056(6) -0.009(4) 0.016(5) 0.003(5) S00F 0.101(3) 0.049(2) 0.052(2) 0.0026(17) -0.009(2) -0.010(2) S00G 0.058(4) 0.063(3) 0.042(3) -0.008(2) 0.010(2) -0.011(2) N00H 0.032(5) 0.051(6) 0.050(6) 0.001(5) -0.002(4) -0.013(4) O00I 0.112(9) 0.068(7) 0.054(6) -0.007(5) 0.014(6) -0.002(7) N00J 0.035(5) 0.044(5) 0.049(6) 0.004(5) -0.020(4) -0.009(4) O00K 0.132(11) 0.054(6) 0.040(5) 0.001(5) 0.003(6) 0.001(7) O00L 0.115(10) 0.062(6) 0.041(5) -0.008(5) 0.000(6) -0.002(6) C00M 0.032(5) 0.055(8) 0.046(7) 0.004(6) 0.002(5) 0.007(5) N00N 0.045(6) 0.045(5) 0.037(5) -0.003(4) -0.009(4) -0.016(4) O00O 0.083(18) 0.068(18) 0.09(2) 0.020(14) -0.004(16) -0.014(15) N00P 0.036(5) 0.042(5) 0.049(6) -0.021(4) 0.007(4) -0.006(4) O00Q 0.075(8) 0.135(12) 0.050(6) 0.031(7) -0.014(5) -0.053(8) C00R 0.034(6) 0.053(7) 0.066(9) -0.009(6) 0.002(6) -0.001(5) C00S 0.037(6) 0.029(5) 0.063(9) 0.000(5) -0.008(6) 0.005(4) C00T 0.033(6) 0.045(7) 0.075(10) -0.006(6) 0.007(6) 0.001(5) C00U 0.066(8) 0.025(5) 0.043(7) -0.003(4) 0.009(6) -0.005(5) C00W 0.036(7) 0.067(9) 0.042(8) 0.003(6) 0.005(6) -0.009(5) C00X 0.053(7) 0.033(5) 0.065(10) 0.000(6) 0.006(7) -0.002(5) C00Y 0.042(6) 0.044(7) 0.053(8) -0.023(6) -0.005(6) 0.005(5) C00Z 0.042(6) 0.048(6) 0.052(8) -0.010(6) 0.002(6) -0.012(5) C010 0.064(10) 0.058(9) 0.049(10) -0.002(6) 0.007(8) -0.011(7) O011 0.100(9) 0.114(10) 0.047(6) -0.047(7) 0.022(6) -0.056(8) C013 0.058(8) 0.090(11) 0.055(9) 0.020(8) 0.013(7) -0.020(8) C014 0.069(10) 0.098(13) 0.056(9) -0.037(9) 0.017(8) -0.015(9) C015 0.128(15) 0.071(11) 0.037(7) 0.015(7) -0.024(9) -0.022(10) C016 0.081(11) 0.062(9) 0.055(9) -0.003(7) -0.003(8) -0.002(8) C5 0.17(2) 0.18(3) 0.099(19) 0.032(19) -0.024(18) 0.11(2) C3 0.24(3) 0.107(17) 0.048(11) 0.026(11) 0.014(15) -0.06(2) S00H 0.117(15) 0.111(14) 0.059(9) 0.025(9) 0.007(9) -0.033(11) C1 0.09(2) 0.050(15) 0.08(2) -0.002(14) -0.031(17) -0.016(16) C2 0.061(16) 0.09(2) 0.08(2) 0.034(19) -0.012(15) -0.017(16) C1A 0.17(4) 0.06(2) 0.023(12) -0.015(13) -0.01(2) 0.03(2) C2A 0.036(13) 0.048(14) 0.036(14) 0.013(11) -0.009(11) 0.002(12) O00P 0.12(3) 0.058(17) 0.024(12) 0.010(12) -0.005(17) -0.032(19) C6 0.26(4) 0.19(3) 0.18(3) -0.01(3) 0.07(3) 0.02(3) C4 0.34(4) 0.17(3) 0.066(15) 0.024(16) 0.10(2) 0.06(3) S1 0.157(19) 0.147(13) 0.069(8) -0.039(8) -0.014(8) 0.039(11) _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 Pb01 I004 3.1122(10) . ? Pb01 I007 3.3450(10) . ? Pb01 I009 3.0306(12) . ? Pb01 I00A 3.0125(12) . ? Pb02 I003 3.0180(11) . ? Pb02 I005 3.3168(10) . ? Pb02 I006 3.0596(12) . ? Pb02 I008 3.1228(11) . ? S00B O00O 1.50(2) . ? S00B C1 1.77(2) . ? S00B C2 1.76(2) . ? S00B C1A 1.77(2) . ? S00B C2A 1.72(2) . ? S00B O00P 1.49(2) . ? S00C C010 1.733(17) . ? S00C O011 1.485(12) . ? S00C C014 1.757(16) . ? S00D O00Q 1.539(13) . ? S00D C00W 1.763(14) . ? S00D C013 1.804(14) . ? S00E O00I 1.566(15) . ? S00E C6 1.61(4) . ? S00E C4 1.77(3) . ? S00F O00K 1.515(12) . ? S00F C015 1.767(18) . ? S00F C5 1.78(2) . ? S00G O00L 1.487(13) . ? S00G C016 1.723(17) . ? S00G C3 1.82(2) . ? N00H C00R 1.445(18) . ? N00H C00X 1.486(16) . ? O00I S1 1.519(18) . ? N00J C00M 1.463(17) . ? N00J C00S 1.485(14) . ? O00L S00H 1.424(19) . ? C00M C00U 1.531(17) . ? N00N C00T 1.510(17) . ? N00N C00U 1.468(16) . ? N00P C00Y 1.534(15) . ? N00P C00Z 1.466(16) . ? C00R C00Z 1.535(16) . ? C00S C00T 1.503(16) . ? C00X C00Y 1.503(18) . ? C016 S00H 1.70(2) . ? C3 S00H 1.88(2) . ? C6 S1 1.54(4) . ? C4 S1 1.78(3) . ? 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 I004 Pb01 I007 177.73(3) . . ? I009 Pb01 I004 91.34(3) . . ? I009 Pb01 I007 88.23(4) . . ? I00A Pb01 I004 96.67(3) . . ? I00A Pb01 I007 85.58(3) . . ? I00A Pb01 I009 93.95(3) . . ? I003 Pb02 I005 86.23(3) . . ? I003 Pb02 I006 93.99(3) . . ? I003 Pb02 I008 96.98(4) . . ? I006 Pb02 I005 89.23(3) . . ? I006 Pb02 I008 91.05(3) . . ? I008 Pb02 I005 176.75(3) . . ? O00O S00B C1 112(2) . . ? O00O S00B C2 94.4(19) . . ? C2 S00B C1 93.8(17) . . ? C2A S00B C1A 100(2) . . ? O00P S00B C1A 106(3) . . ? O00P S00B C2A 119(2) . . ? C010 S00C C014 95.6(7) . . ? O011 S00C C010 108.0(9) . . ? O011 S00C C014 106.5(8) . . ? O00Q S00D C00W 105.8(8) . . ? O00Q S00D C013 104.8(8) . . ? C00W S00D C013 99.5(7) . . ? O00I S00E C6 123.6(17) . . ? O00I S00E C4 103.7(12) . . ? C6 S00E C4 96.1(17) . . ? O00K S00F C015 104.6(7) . . ? O00K S00F C5 104.3(11) . . ? C015 S00F C5 99.1(12) . . ? O00L S00G C016 108.1(8) . . ? O00L S00G C3 107.5(10) . . ? C016 S00G C3 96.2(10) . . ? C00R N00H C00X 111.9(10) . . ? C00M N00J C00S 111.7(9) . . ? N00J C00M C00U 109.5(10) . . ? C00U N00N C00T 110.4(9) . . ? C00Z N00P C00Y 110.3(9) . . ? N00H C00R C00Z 112.2(11) . . ? N00J C00S C00T 110.2(10) . . ? C00S C00T N00N 109.3(11) . . ? N00N C00U C00M 110.6(9) . . ? N00H C00X C00Y 111.4(10) . . ? C00X C00Y N00P 107.8(11) . . ? N00P C00Z C00R 111.1(10) . . ? O00L S00H C016 112.4(13) . . ? O00L S00H C3 107.4(12) . . ? C016 S00H C3 94.8(12) . . ? O00I S1 C6 133(2) . . ? O00I S1 C4 105.4(13) . . ? C6 S1 C4 98.5(19) . . ? _shelx_res_file ; TITL nims_pzdi_1_a.res in Pna2(1) nims_pzdi_1.res created by SHELXL-2018/3 at 14:57:18 on 28-Sep-2023 REM Old TITL NIMS_PZDI_1 in Pnma REM SHELXT solution in Pna2(1): R1 0.133, Rweak 0.012, Alpha 0.019 REM 3.656 for 418 systematic absences, Orientation a'=-a, b'=c, c'=b REM Flack x = 0.164 ( 0.003 ) from 5054 Parsons' quotients REM Formula found by SHELXT: C19 N13 I8 Pb2 CELL 0.71073 20.3941 13.7425 19.2851 90 90 90 ZERR 8 0.0003 0.0002 0.0003 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,+Z SYMM 0.5-X,0.5+Y,0.5+Z SFAC C H I N O Pb S UNIT 80 240 32 16 24 8 24 SADI S00G O00L S00H O00L SIMU S1 O00I C6 C4 SADI S00E C6 S1 C6 SADI S00B C1 S00B C1A SADI S00G C3 S00H C3 SIMU 0.02 0.04 2 S00B C1A C2A O00P SADI S00E C4 S1 C4 RIGU S00B C1A C2A O00P SADI S00G C016 S00H C016 SADI S00B O00O S00B O00P SADI S00B C2 S00B C2A SADI S00E O00I S1 O00I L.S. 10 0 0 PLAN 20 SIZE 0.09 0.19 0.35 list 4 fmap 2 53 ACTA REM REM REM WGHT 0.028600 24.872700 EXTI 0.000248 FVAR 0.06221 0.68515 0.59264 0.52561 PB01 6 0.374011 -0.221207 0.463631 11.00000 0.03114 0.05004 = 0.03696 0.00748 0.00154 0.00209 PB02 6 0.376200 0.273108 0.465918 11.00000 0.02906 0.05366 = 0.03502 -0.00576 0.00307 -0.00236 I003 3 0.269651 0.241499 0.572156 11.00000 0.04829 0.05948 = 0.03842 0.00321 0.01227 -0.00068 I004 3 0.258521 -0.225018 0.358180 11.00000 0.04412 0.05818 = 0.04841 0.00860 -0.01069 -0.00836 I005 3 0.256581 0.280155 0.349498 11.00000 0.04360 0.07193 = 0.03584 -0.00112 -0.00217 -0.00748 I006 3 0.370214 0.495077 0.476475 11.00000 0.04214 0.05011 = 0.07241 0.00509 -0.01071 -0.00517 I007 3 0.493925 -0.214598 0.581878 11.00000 0.04196 0.08315 = 0.03743 0.01205 -0.00126 -0.00047 I008 3 0.494514 0.266330 0.568592 11.00000 0.04313 0.06160 = 0.05307 -0.01119 -0.01185 0.01348 I009 3 0.382023 -0.001299 0.455406 11.00000 0.04542 0.04541 = 0.08508 -0.00524 -0.01095 0.00514 I00A 3 0.482120 -0.252706 0.359582 11.00000 0.04133 0.05633 = 0.04206 -0.00747 0.00559 0.00118 S00B 7 0.566242 0.550919 0.242505 11.00000 0.08454 0.05971 = 0.05011 -0.00678 -0.00009 0.00679 S00C 7 0.488851 0.285899 0.303708 11.00000 0.05691 0.06813 = 0.04864 -0.01343 0.00793 -0.00390 S00D 7 0.242692 0.300661 0.125694 11.00000 0.05670 0.05633 = 0.05033 0.00651 -0.00210 -0.00143 PART 1 S00E 7 0.575695 -0.061470 0.242885 41.00000 0.08858 0.07471 = 0.05627 -0.00906 0.01639 0.00268 PART 0 S00F 7 0.315124 -0.060617 0.187504 11.00000 0.10117 0.04868 = 0.05216 0.00262 -0.00926 -0.00968 PART 1 S00G 7 0.324805 0.554662 0.189236 21.00000 0.05790 0.06303 = 0.04161 -0.00810 0.00959 -0.01075 PART 0 N00H 4 0.688369 0.045748 0.486970 11.00000 0.03191 0.05080 = 0.05019 0.00093 -0.00196 -0.01344 AFIX 23 H00A 2 0.722602 0.082440 0.475327 11.00000 -1.20000 H00B 2 0.690947 0.033565 0.532214 11.00000 -1.20000 AFIX 0 O00I 5 0.581425 -0.001014 0.311479 11.00000 0.11186 0.06781 = 0.05401 -0.00749 0.01378 -0.00233 N00J 4 0.677438 0.546727 0.496210 11.00000 0.03496 0.04433 = 0.04928 0.00440 -0.01985 -0.00887 AFIX 23 H00M 2 0.711210 0.587678 0.494541 11.00000 -1.20000 H00N 2 0.674349 0.524246 0.539367 11.00000 -1.20000 AFIX 0 O00K 5 0.318717 0.004188 0.124055 11.00000 0.13163 0.05405 = 0.03984 0.00143 0.00312 0.00135 O00L 5 0.350470 0.496171 0.130349 11.00000 0.11548 0.06196 = 0.04086 -0.00790 0.00018 -0.00206 C00M 1 0.689484 0.465444 0.448881 11.00000 0.03155 0.05509 = 0.04646 0.00373 0.00178 0.00698 AFIX 23 H00O 2 0.728749 0.430844 0.462947 11.00000 -1.20000 H00P 2 0.696169 0.489848 0.402217 11.00000 -1.20000 AFIX 0 N00N 4 0.570244 0.448156 0.431457 11.00000 0.04545 0.04507 = 0.03748 -0.00284 -0.00942 -0.01586 AFIX 23 H00Q 2 0.536418 0.407315 0.433236 11.00000 -1.20000 H00R 2 0.573436 0.470550 0.388286 11.00000 -1.20000 AFIX 0 PART 1 O00O 5 0.603297 0.489670 0.293450 31.00000 0.08265 0.06767 = 0.08775 0.02026 -0.00420 -0.01361 PART 0 N00P 4 0.570093 -0.052619 0.445257 11.00000 0.03622 0.04235 = 0.04929 -0.02069 0.00699 -0.00592 AFIX 23 H00C 2 0.535148 -0.089338 0.454175 11.00000 -1.20000 H00D 2 0.569338 -0.036916 0.400491 11.00000 -1.20000 AFIX 0 O00Q 5 0.243128 0.301912 0.045875 11.00000 0.07497 0.13531 = 0.04992 0.03081 -0.01354 -0.05320 C00R 1 0.691297 -0.044955 0.449220 11.00000 0.03355 0.05265 = 0.06591 -0.00882 0.00212 -0.00059 AFIX 23 H00E 2 0.729682 -0.081147 0.463951 11.00000 -1.20000 H00F 2 0.695929 -0.031235 0.400126 11.00000 -1.20000 AFIX 0 C00S 1 0.616364 0.599786 0.478173 11.00000 0.03697 0.02943 = 0.06291 0.00025 -0.00844 0.00538 AFIX 23 H00S 2 0.620353 0.627242 0.432028 11.00000 -1.20000 H00T 2 0.609685 0.652809 0.510613 11.00000 -1.20000 AFIX 0 C00T 1 0.558602 0.531970 0.480607 11.00000 0.03343 0.04521 = 0.07495 -0.00564 0.00667 0.00145 AFIX 23 H00U 2 0.519083 0.566567 0.467361 11.00000 -1.20000 H00V 2 0.552808 0.507550 0.527399 11.00000 -1.20000 AFIX 0 C00U 1 0.630669 0.396259 0.450033 11.00000 0.06561 0.02502 = 0.04281 -0.00279 0.00880 -0.00548 AFIX 23 H00W 2 0.637982 0.343530 0.417502 11.00000 -1.20000 H00X 2 0.626093 0.368364 0.495982 11.00000 -1.20000 AFIX 0 C00W 1 0.320632 0.257807 0.150787 11.00000 0.03579 0.06722 = 0.04245 0.00267 0.00537 -0.00930 AFIX 137 H00Y 2 0.325819 0.191627 0.135825 11.00000 -1.50000 H 2 0.324566 0.261003 0.200340 11.00000 -1.50000 HA 2 0.353956 0.297454 0.129862 11.00000 -1.50000 AFIX 0 C00X 1 0.626918 0.100107 0.472447 11.00000 0.05269 0.03335 = 0.06549 0.00043 0.00562 -0.00192 AFIX 23 H00G 2 0.625800 0.118239 0.423851 11.00000 -1.20000 H00H 2 0.626279 0.159370 0.499760 11.00000 -1.20000 AFIX 0 C00Y 1 0.567360 0.040219 0.489344 11.00000 0.04247 0.04367 = 0.05324 -0.02251 -0.00526 0.00496 AFIX 23 H00I 2 0.527823 0.076630 0.478925 11.00000 -1.20000 H00J 2 0.567041 0.023698 0.538244 11.00000 -1.20000 AFIX 0 C00Z 1 0.629953 -0.107640 0.460607 11.00000 0.04234 0.04766 = 0.05242 -0.01038 0.00219 -0.01231 AFIX 23 H00K 2 0.632017 -0.164508 0.430893 11.00000 -1.20000 H00L 2 0.628754 -0.129766 0.508353 11.00000 -1.20000 AFIX 0 C010 1 0.566557 0.247748 0.279604 11.00000 0.06390 0.05785 = 0.04928 -0.00189 0.00709 -0.01099 AFIX 137 H01G 2 0.597274 0.299735 0.286710 11.00000 -1.50000 H01H 2 0.566347 0.229675 0.231520 11.00000 -1.50000 H01I 2 0.579103 0.192698 0.307228 11.00000 -1.50000 AFIX 0 O011 5 0.488345 0.298676 0.380177 11.00000 0.09967 0.11361 = 0.04726 -0.04704 0.02242 -0.05578 C013 1 0.193783 0.196105 0.148507 11.00000 0.05761 0.08999 = 0.05521 0.01993 0.01340 -0.02010 AFIX 137 H01M 2 0.148457 0.209510 0.139059 11.00000 -1.50000 H01N 2 0.199174 0.182137 0.196947 11.00000 -1.50000 H01O 2 0.207685 0.141017 0.121659 11.00000 -1.50000 AFIX 0 C014 1 0.450121 0.174147 0.286883 11.00000 0.06924 0.09848 = 0.05626 -0.03674 0.01714 -0.01487 AFIX 137 H01J 2 0.449925 0.162195 0.237838 11.00000 -1.50000 H01K 2 0.405825 0.176343 0.303651 11.00000 -1.50000 H01L 2 0.473455 0.122851 0.309968 11.00000 -1.50000 AFIX 0 C015 1 0.297017 0.019546 0.256541 11.00000 0.12835 0.07123 = 0.03699 0.01490 -0.02364 -0.02206 AFIX 137 H01P 2 0.324084 0.076475 0.252936 11.00000 -1.50000 H01Q 2 0.305435 -0.012437 0.299892 11.00000 -1.50000 H01R 2 0.251694 0.038151 0.254300 11.00000 -1.50000 AFIX 0 C016 1 0.370160 0.660214 0.194523 11.00000 0.08063 0.06170 = 0.05529 -0.00252 -0.00311 -0.00167 PART 1 AFIX 137 H01A 2 0.416001 0.644401 0.195522 21.00000 -1.50000 H01B 2 0.358637 0.694686 0.236069 21.00000 -1.50000 H01C 2 0.361106 0.700353 0.154922 21.00000 -1.50000 AFIX 137 PART 2 H01D 2 0.354092 0.686915 0.151776 -21.00000 -1.50000 H01E 2 0.408610 0.695197 0.208779 -21.00000 -1.50000 H01F 2 0.336976 0.665893 0.229596 -21.00000 -1.50000 AFIX 0 PART 0 C5 1 0.398433 -0.086208 0.207654 11.00000 0.16928 0.17901 = 0.09918 0.03221 -0.02385 0.10629 AFIX 137 H5A 2 0.413655 -0.138903 0.179214 11.00000 -1.50000 H5B 2 0.401985 -0.104072 0.255632 11.00000 -1.50000 H5C 2 0.424641 -0.029465 0.198997 11.00000 -1.50000 AFIX 0 C3 1 0.355860 0.500557 0.268824 11.00000 0.24431 0.10714 = 0.04840 0.02556 0.01409 -0.05611 PART 1 AFIX 33 H3AA 2 0.340061 0.536879 0.307925 21.00000 -1.50000 H3AB 2 0.340984 0.434447 0.272161 21.00000 -1.50000 H3AC 2 0.402923 0.501795 0.268382 21.00000 -1.50000 AFIX 33 PART 2 H3BD 2 0.381068 0.529507 0.305454 -21.00000 -1.50000 H3BE 2 0.310923 0.520591 0.272816 -21.00000 -1.50000 H3BF 2 0.358477 0.430969 0.272188 -21.00000 -1.50000 AFIX 0 S00H 7 0.389305 0.540825 0.182855 -21.00000 0.11684 0.11097 = 0.05904 0.02457 0.00727 -0.03306 PART 1 C1 1 0.537105 0.481431 0.171523 31.00000 0.09025 0.05026 = 0.07813 -0.00177 -0.03145 -0.01616 AFIX 137 H1A 2 0.557330 0.418357 0.172117 31.00000 -1.50000 H1B 2 0.547800 0.513984 0.128956 31.00000 -1.50000 H1C 2 0.490396 0.474301 0.175034 31.00000 -1.50000 AFIX 0 C2 1 0.636865 0.590049 0.198390 31.00000 0.06051 0.09230 = 0.08421 0.03422 -0.01205 -0.01706 AFIX 137 H2A 2 0.670249 0.606742 0.231407 31.00000 -1.50000 H2B 2 0.626474 0.646057 0.170744 31.00000 -1.50000 H2C 2 0.652457 0.538727 0.168918 31.00000 -1.50000 AFIX 0 PART 2 C1A 1 0.582316 0.490503 0.163219 -31.00000 0.17432 0.05509 = 0.02337 -0.01453 -0.01353 0.03450 AFIX 137 H1AA 2 0.621566 0.452442 0.167632 -31.00000 -1.50000 H1AB 2 0.587924 0.537711 0.127010 -31.00000 -1.50000 H1AC 2 0.546172 0.448596 0.152027 -31.00000 -1.50000 AFIX 0 C2A 1 0.613535 0.653316 0.232305 -31.00000 0.03645 0.04832 = 0.03599 0.01330 -0.00933 0.00218 AFIX 137 H2AA 2 0.625157 0.678685 0.277028 -31.00000 -1.50000 H2AB 2 0.589235 0.701490 0.207022 -31.00000 -1.50000 H2AC 2 0.652649 0.637017 0.207164 -31.00000 -1.50000 AFIX 0 O00P 5 0.583395 0.480326 0.298165 -31.00000 0.12161 0.05808 = 0.02444 0.00970 -0.00514 -0.03167 PART 0 C6 1 0.616039 -0.160547 0.228626 11.00000 0.26013 0.19124 = 0.18302 -0.00558 0.07259 0.01771 PART 1 AFIX 33 H6AA 2 0.605045 -0.185236 0.183534 41.00000 -1.50000 H6AB 2 0.662219 -0.147324 0.230676 41.00000 -1.50000 H6AC 2 0.604841 -0.207994 0.263189 41.00000 -1.50000 AFIX 33 PART 2 H6BD 2 0.651418 -0.171879 0.196798 -41.00000 -1.50000 H6BE 2 0.617761 -0.207776 0.265259 -41.00000 -1.50000 H6BF 2 0.574999 -0.166143 0.204573 -41.00000 -1.50000 AFIX 0 PART 0 C4 1 0.617975 0.010043 0.181184 11.00000 0.34257 0.17024 = 0.06607 0.02384 0.10467 0.05933 PART 1 AFIX 33 H4AA 2 0.616935 -0.021907 0.136930 41.00000 -1.50000 H4AB 2 0.597278 0.072568 0.177469 41.00000 -1.50000 H4AC 2 0.662672 0.018304 0.195646 41.00000 -1.50000 AFIX 33 PART 2 H4BD 2 0.643098 -0.022248 0.145932 -41.00000 -1.50000 H4BE 2 0.573087 0.014866 0.166596 -41.00000 -1.50000 H4BF 2 0.635373 0.074093 0.188688 -41.00000 -1.50000 AFIX 0 S1 7 0.622355 -0.057630 0.259501 -41.00000 0.15736 0.14687 = 0.06946 -0.03891 -0.01444 0.03895 HKLF 4 REM nims_pzdi_1_a.res in Pna2(1) REM wR2 = 0.0961, GooF = S = 1.149, Restrained GooF = 1.151 for all data REM R1 = 0.0434 for 13163 Fo > 4sig(Fo) and 0.0517 for all 14685 data REM 475 parameters refined using 61 restraints END WGHT 0.0286 24.8859 REM Highest difference peak 1.676, deepest hole -1.370, 1-sigma level 0.154 Q1 1 0.5086 0.2229 0.3415 11.00000 0.05 1.68 Q2 1 0.2592 0.2367 0.0816 11.00000 0.05 1.41 Q3 1 0.2621 -0.2756 0.3470 11.00000 0.05 1.38 Q4 1 0.3744 0.3240 0.4607 11.00000 0.05 1.34 Q5 1 0.3619 0.0007 0.1928 11.00000 0.05 1.29 Q6 1 0.3773 -0.1665 0.4637 11.00000 0.05 1.24 Q7 1 0.4949 0.2180 0.5808 11.00000 0.05 1.05 Q8 1 0.6174 0.0067 0.2404 11.00000 0.05 1.05 Q9 1 0.6183 0.5162 0.2273 11.00000 0.05 0.90 Q10 1 0.2546 0.2195 0.3519 11.00000 0.05 0.90 Q11 1 0.2835 0.3009 0.5835 11.00000 0.05 0.89 Q12 1 0.3999 0.5152 0.4413 11.00000 0.05 0.89 Q13 1 0.4919 0.3209 0.5868 11.00000 0.05 0.88 Q14 1 0.3412 -0.0022 0.4742 11.00000 0.05 0.87 Q15 1 0.5210 0.2799 0.5774 11.00000 0.05 0.86 Q16 1 0.4975 -0.2815 0.5879 11.00000 0.05 0.85 Q17 1 0.4643 -0.2015 0.3485 11.00000 0.05 0.85 Q18 1 0.5586 -0.0737 0.1853 11.00000 0.05 0.78 Q19 1 0.4017 -0.2374 0.4620 11.00000 0.05 0.77 Q20 1 0.3384 0.2789 0.4677 11.00000 0.05 0.77 ; _shelx_res_checksum 54519 _shelx_hkl_file ; 0 2 0 2014.40 136.74 0 -2 0 1871.64 136.78 0 3 0 0.26 0.17 0 -3 0 0.61 0.20 0 -3 0 0.25 0.27 0 3 0 0.41 0.31 0 4 0 5916.05 433.58 0 -4 0 6330.38 433.56 0 -4 0 8757.71 433.62 0 4 0 8155.41 433.74 0 -4 0 4883.57 433.63 0 5 0 0.75 0.57 0 -5 0 0.54 0.49 0 -5 0 0.64 0.30 0 5 0 0.34 0.32 0 -5 0 0.05 0.33 0 5 0 0.21 0.36 0 -5 0 0.75 0.36 0 6 0 900.51 55.50 0 -6 0 813.71 55.40 0 6 0 756.67 55.32 0 -6 0 820.86 55.30 0 -6 0 878.18 55.33 0 6 0 879.06 55.34 0 -6 0 828.58 55.34 0 7 0 0.84 0.78 0 -7 0 0.80 0.60 0 7 0 -0.04 0.47 0 -7 0 0.64 0.40 0 -7 0 0.30 0.46 0 7 0 0.83 0.50 0 -7 0 0.54 0.48 0 8 0 1029.25 60.46 0 -8 0 863.99 60.30 0 8 0 917.10 60.34 0 -8 0 906.75 60.20 0 8 0 826.09 60.25 0 -8 0 945.18 60.24 0 8 0 940.67 60.25 0 -8 0 884.85 60.26 0 9 0 1.24 1.13 0 9 0 0.52 0.90 0 -9 0 1.25 0.85 0 9 0 0.50 0.77 0 -9 0 0.90 0.59 0 -9 0 -0.10 0.67 0 9 0 0.87 0.77 0 -9 0 0.68 0.72 0 10 0 12.75 1.70 0 -10 0 10.17 1.30 0 10 0 12.32 1.48 0 10 0 12.07 1.31 0 -10 0 10.58 1.19 0 10 0 10.99 1.26 0 -10 0 9.07 1.27 0 11 0 1.32 1.32 0 -11 0 1.11 0.94 0 11 0 -0.11 1.10 0 11 0 1.03 0.96 0 11 0 0.49 0.43 0 -11 0 0.25 0.81 0 11 0 0.96 0.94 0 -11 0 0.88 0.90 0 12 0 9.99 1.74 0 12 0 7.19 1.29 0 -12 0 8.14 1.31 0 12 0 7.19 1.59 0 -12 0 7.41 1.16 0 12 0 10.14 1.31 0 -12 0 8.02 1.31 0 -13 0 0.41 1.20 0 13 0 3.13 1.21 0 13 0 0.41 1.58 0 -13 0 0.49 1.20 0 -13 0 0.71 1.06 0 13 0 1.09 1.23 0 13 0 0.13 1.64 0 -14 0 113.35 8.05 0 14 0 119.49 7.91 0 -14 0 113.89 8.00 0 14 0 111.16 8.08 0 14 0 115.48 7.97 0 -14 0 108.98 7.86 0 -15 0 1.08 1.21 0 15 0 1.08 1.63 0 15 0 0.74 1.14 0 -15 0 -0.11 1.35 0 -15 0 1.39 1.21 0 -15 0 5.02 1.53 0 15 0 -0.50 1.43 0 -16 0 2.75 1.27 0 16 0 3.20 1.19 0 16 0 1.74 1.77 0 -16 0 1.62 1.49 0 -16 0 2.41 1.30 0 16 0 3.66 1.60 0 -16 0 4.04 1.59 0 -17 0 2.16 1.40 0 17 0 0.92 2.06 0 17 0 2.25 1.80 0 -17 0 2.06 1.71 0 -17 0 1.57 1.68 0 -18 0 41.57 3.74 0 18 0 41.14 3.99 0 18 0 47.19 3.82 0 -19 0 0.91 1.81 0 -2 -1 0.35 0.19 0 2 1 0.09 0.21 0 2 -1 0.30 0.23 0 2 -1 0.81 0.17 0 2 -1 0.12 0.12 0 2 1 0.30 0.19 0 -2 -1 0.48 0.14 0 -2 1 0.20 0.12 0 2 -1 0.34 0.13 0 -3 1 17.95 1.32 0 3 1 18.13 1.38 0 3 -1 20.87 1.32 0 3 -1 21.18 1.35 0 -3 1 17.78 1.35 0 3 -1 21.60 1.36 0 3 -1 21.13 1.46 0 -3 -1 19.83 1.42 0 3 1 17.19 1.42 0 4 -1 -0.05 0.60 0 -4 -1 0.62 0.44 0 4 1 0.15 0.50 0 -4 1 0.47 0.40 0 4 -1 0.30 0.26 0 4 1 0.15 0.36 0 -4 -1 -0.05 0.33 0 -4 1 0.09 0.22 0 -4 1 0.48 0.29 0 4 1 0.29 0.33 0 -4 1 0.98 0.32 0 5 1 393.50 25.21 0 5 -1 361.01 25.20 0 -5 -1 319.16 25.15 0 -5 1 384.03 25.13 0 5 1 346.62 25.11 0 5 -1 353.48 25.06 0 -5 -1 390.09 25.10 0 -5 1 382.88 25.04 0 -5 1 438.75 25.09 0 5 1 387.62 25.09 0 -5 1 379.51 25.09 0 -6 -1 0.64 0.56 0 6 -1 0.52 0.71 0 6 1 1.16 0.74 0 -6 1 0.69 0.51 0 -6 1 0.16 0.30 0 -6 -1 0.13 0.40 0 6 1 0.30 0.47 0 6 -1 0.48 0.37 0 -6 1 0.09 0.39 0 6 1 0.03 0.43 0 6 -1 0.60 0.44 0 -6 1 0.15 0.42 0 -7 -1 125.84 9.67 0 7 -1 151.67 9.77 0 7 1 164.21 9.78 0 -7 1 152.32 9.65 0 -7 -1 136.00 9.67 0 7 -1 135.99 9.64 0 7 1 136.64 9.61 0 7 -1 132.27 9.56 0 -7 -1 142.85 9.57 0 -7 1 146.09 9.52 0 -7 1 143.89 9.57 0 7 1 156.30 9.59 0 7 -1 146.12 9.60 0 -7 1 146.48 9.60 0 -7 -1 129.13 9.59 0 8 1 1.94 1.14 0 -8 -1 1.06 0.87 0 8 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722.27 48.06 0 -2 2 741.50 48.07 0 2 -2 748.43 48.07 0 2 -2 738.66 48.07 0 -2 -2 620.72 48.08 0 2 -2 736.88 48.12 0 -3 -2 0.58 0.27 0 3 -2 -0.12 0.34 0 3 -2 0.40 0.21 0 -3 2 0.22 0.17 0 3 2 -0.03 0.31 0 3 2 0.31 0.21 0 -3 -2 0.14 0.18 0 3 2 0.40 0.17 0 3 -2 0.20 0.18 0 3 -2 0.17 0.20 0 -3 2 0.13 0.22 0 4 -2 1934.96 133.66 0 -4 -2 1665.38 133.61 0 -4 2 2088.18 133.57 0 4 2 1762.90 133.61 0 4 -2 1887.76 133.52 0 4 2 2214.44 133.57 0 4 -2 2141.58 133.56 0 -4 2 2188.53 133.58 0 4 -2 2205.57 133.57 0 -4 2 2097.82 133.57 0 5 -2 0.96 0.58 0 -5 -2 -0.32 0.45 0 5 2 0.47 0.59 0 -5 2 0.23 0.34 0 5 -2 0.19 0.23 0 -5 -2 0.39 0.41 0 5 2 0.36 0.43 0 5 2 0.08 0.33 0 5 2 0.36 0.21 0 5 -2 0.30 0.31 0 -5 2 0.27 0.33 0 -5 2 0.06 0.35 0 5 -2 0.76 0.35 0 -6 -2 83.72 5.56 0 6 2 77.97 5.59 0 6 -2 88.91 5.64 0 6 -2 84.01 5.49 0 -6 2 82.38 5.49 0 6 2 73.44 5.50 0 -6 -2 91.09 5.50 0 6 -2 83.42 5.40 0 6 2 76.81 5.45 0 6 2 76.07 5.37 0 -6 2 80.07 5.46 0 -6 2 78.44 5.44 0 7 -2 1.13 0.84 0 7 2 0.65 0.81 0 -7 -2 0.07 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1766.58 122.24 0 2 8 1879.60 122.23 0 2 8 1902.61 122.27 0 2 -8 1796.60 122.24 0 2 -8 2038.01 122.37 0 -2 -8 1866.64 122.21 0 2 -8 1834.94 122.22 0 2 -8 1717.16 122.18 0 -2 8 1948.77 122.30 0 2 -8 1871.22 122.20 0 2 8 2007.91 122.50 0 -2 8 1778.70 122.18 0 2 -8 1720.69 122.19 0 3 8 0.46 0.36 0 3 -8 0.15 0.27 0 3 -8 0.30 0.42 0 -3 -8 0.46 0.41 0 3 -8 0.32 0.26 0 3 8 -0.11 0.77 0 -3 -8 0.71 0.49 0 3 -8 0.46 0.44 0 3 8 0.67 0.51 0 3 -8 0.60 0.43 0 3 -8 0.36 0.20 0 -3 -8 -0.43 0.82 0 3 -8 0.10 0.55 0 3 -8 0.28 0.30 0 4 -8 2250.24 167.68 0 -4 -8 2311.70 167.66 0 -4 -8 2649.39 167.67 0 4 -8 2492.99 167.56 0 4 8 2491.92 167.70 0 4 8 2449.95 167.91 0 4 -8 2573.26 167.66 0 4 -8 2516.40 167.57 0 4 -8 2560.55 167.57 0 4 -8 2558.99 167.57 0 4 8 2562.80 167.66 0 4 -8 2555.51 167.65 0 4 -8 2531.04 167.67 0 5 -8 0.64 0.56 0 5 -8 1.09 0.62 0 -5 8 0.08 0.31 0 5 -8 0.43 0.27 0 5 8 -0.22 0.97 0 5 -8 0.47 0.45 0 5 -8 0.10 0.35 0 5 -8 0.96 0.36 0 -5 -8 0.26 0.59 0 5 -8 -0.12 0.64 0 5 8 -0.05 0.61 0 5 -8 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14.96 0.96 2 3 -3 13.56 0.95 2 3 3 11.66 1.17 2 3 3 12.86 1.24 -2 -3 -3 15.27 1.22 -2 3 -3 13.95 1.04 2 3 3 14.28 1.07 -2 -3 3 12.61 1.05 -2 3 -3 12.60 1.01 2 3 -3 12.32 1.06 -2 3 3 13.62 1.01 -2 3 -3 12.86 0.97 2 -3 3 15.31 0.95 2 3 -3 13.32 0.97 -2 -3 -3 13.52 1.11 -2 3 -3 13.67 0.98 -2 -3 -3 10.67 1.07 2 -3 3 14.45 1.00 2 -3 -3 12.65 0.99 2 3 -3 13.56 1.02 2 -4 -3 1982.45 127.65 -2 4 -3 2018.24 127.75 -2 -4 3 1760.87 127.77 -2 4 -3 2043.32 127.73 -2 -4 -3 1818.61 127.76 2 4 -3 1926.49 127.78 2 4 3 1665.86 127.88 -2 4 3 1788.74 127.72 -2 4 -3 1907.85 127.70 2 4 -3 1944.04 127.70 -2 -4 3 1963.73 127.70 -2 -4 -3 1797.57 127.81 2 -4 3 2099.69 127.70 2 4 3 1634.78 127.92 -2 -4 3 1995.94 127.68 2 -4 3 1746.17 127.73 -2 4 -3 1876.58 127.72 -2 -4 -3 1702.28 127.81 2 -4 -3 1760.98 127.72 2 4 -3 1865.99 127.78 2 4 -3 2001.25 127.69 -2 4 -3 1962.77 127.71 2 4 -3 2052.95 127.71 2 -4 3 1993.72 127.72 -2 5 -3 63.65 4.17 -2 5 3 63.75 4.08 -2 5 -3 59.64 4.14 -2 -5 -3 56.50 4.18 -2 -5 -3 74.32 4.36 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5.42 2.04 2 -16 6 9.07 1.82 -2 -16 -6 9.50 1.77 2 -16 -6 7.61 1.87 -2 -16 -6 5.95 1.36 2 -16 -6 6.85 1.59 2 16 -6 6.26 2.01 -2 16 -6 9.59 1.88 2 -17 6 4.44 1.87 2 17 6 0.95 2.11 -2 17 6 2.70 2.00 2 17 6 1.20 1.52 2 17 -6 0.29 2.07 -2 17 -6 0.25 1.83 -2 -17 -6 2.86 1.83 2 -17 6 0.38 1.35 -2 -17 6 3.63 1.56 2 -17 -6 2.19 1.76 -2 -18 6 5.81 1.82 -2 0 -7 1937.22 131.31 2 0 -7 1950.55 131.38 2 0 -7 1800.74 131.33 -2 0 -7 2055.04 131.35 2 0 -7 1907.33 131.34 -2 0 7 2064.47 131.36 2 0 7 2016.97 131.30 -2 0 -7 1964.95 131.48 -2 0 7 1864.50 131.43 2 0 -7 2100.30 131.37 2 0 7 2036.55 131.42 -2 0 -7 2005.59 131.35 -2 0 7 2002.84 131.45 2 0 7 1976.83 131.34 2 0 -7 2059.52 131.34 2 -1 7 30.64 2.13 2 1 7 29.98 2.24 -2 1 -7 33.26 2.27 2 1 7 29.30 2.12 2 1 -7 31.59 2.16 2 -1 -7 28.53 2.16 -2 1 -7 31.25 2.13 -2 1 7 29.09 2.16 2 1 -7 32.81 2.21 -2 1 7 30.98 2.17 2 1 -7 32.06 2.17 -2 1 -7 28.46 2.13 -2 1 7 31.39 2.08 2 -1 7 31.04 2.09 2 1 7 31.87 2.10 -2 -1 -7 29.24 2.13 -2 1 7 31.29 2.35 -2 -1 -7 30.01 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19.91 -8 6 -4 307.87 20.01 8 6 -4 303.55 19.92 -8 -6 4 321.04 20.06 -8 -6 4 310.69 20.03 8 -6 4 299.80 19.94 -8 -6 4 327.56 20.07 8 6 4 231.32 20.15 -8 -6 -4 312.34 20.15 -8 -6 -4 305.24 20.08 8 -6 4 308.41 20.04 8 6 -4 312.07 20.09 8 6 4 360.21 20.02 -8 -6 4 299.04 20.23 -8 6 4 317.50 20.00 -8 6 -4 297.97 20.02 -8 6 4 292.22 20.04 8 -6 4 317.85 20.03 8 -6 -4 298.00 20.01 -8 -6 -4 310.67 20.19 8 6 -4 301.50 20.02 -8 6 -4 317.25 19.94 8 -6 -4 292.51 20.01 -8 6 4 305.94 20.01 -8 6 4 298.06 20.03 8 -7 4 32.04 2.33 8 7 -4 30.06 2.37 8 7 4 34.02 2.43 -8 7 -4 31.44 2.32 -8 -7 4 30.84 2.30 8 -7 -4 30.31 2.30 8 7 -4 31.19 2.17 8 -7 4 32.07 2.19 -8 -7 4 31.72 2.31 -8 -7 4 33.49 2.37 -8 -7 -4 31.16 2.52 8 7 4 26.11 2.54 -8 -7 4 33.47 2.20 8 -7 4 28.12 2.29 -8 -7 -4 29.46 2.44 -8 -7 4 31.88 2.58 8 7 -4 35.48 2.46 -8 -7 -4 30.13 2.45 -8 7 4 28.38 2.32 -8 7 -4 30.06 2.32 8 -7 4 33.03 2.33 8 -7 -4 30.23 2.31 8 7 -4 33.74 2.34 -8 -7 -4 33.29 2.60 8 7 -4 30.60 2.24 8 -7 -4 31.49 2.35 8 -7 -4 29.79 2.31 -8 7 -4 32.93 2.18 -8 -8 4 110.06 7.32 8 -8 -4 108.45 7.32 -8 8 -4 111.06 7.32 8 -8 4 109.72 7.19 -8 -8 4 107.84 7.31 -8 -8 -4 114.05 7.48 8 8 -4 95.13 7.27 8 8 4 77.48 7.51 8 -8 4 109.26 7.26 8 8 -4 109.16 7.18 -8 -8 -4 104.19 7.40 -8 -8 4 105.59 7.54 8 8 -4 117.71 7.46 -8 -8 -4 97.82 7.41 -8 -8 4 102.84 7.25 -8 8 4 105.22 7.32 8 -8 4 110.23 7.32 -8 8 -4 108.51 7.32 8 8 -4 111.40 7.33 -8 -8 4 105.71 7.36 8 -8 -4 111.33 7.32 -8 -8 -4 102.11 7.52 8 8 -4 109.14 7.39 8 -8 -4 106.96 7.35 8 -8 4 108.23 7.34 8 8 4 107.82 7.39 8 -8 -4 112.79 7.31 8 -9 -4 14.18 1.33 -8 -9 4 15.53 1.68 8 9 -4 19.09 1.70 -8 -9 -4 15.33 1.49 -8 -9 4 15.40 1.28 -8 -9 -4 12.21 1.52 -8 9 4 14.07 1.38 -8 9 -4 13.38 1.38 8 9 -4 14.44 1.43 8 -9 4 13.70 1.36 -8 -9 4 15.79 1.45 8 9 4 11.54 1.64 8 9 -4 12.15 1.32 -8 -9 4 14.09 1.34 8 -9 4 14.45 1.11 8 9 -4 15.68 1.55 8 9 4 16.42 1.55 8 -9 4 13.91 1.42 8 -9 -4 14.49 1.43 -8 -9 4 15.25 1.37 8 -9 -4 14.59 1.41 -8 9 -4 12.91 1.35 8 -9 4 15.77 1.56 8 -10 -4 163.07 11.02 8 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42.21 3.01 8 -3 5 44.99 3.04 -8 3 -5 41.10 3.01 8 -3 5 44.65 2.94 8 3 -5 41.15 3.03 8 3 5 44.84 3.07 -8 -3 -5 40.69 3.09 -8 3 -5 45.50 3.04 8 3 5 41.10 3.09 -8 -3 5 44.95 2.94 -8 3 5 44.29 3.04 -8 -3 5 44.42 3.04 8 -4 5 9.34 0.81 8 4 5 9.78 1.00 -8 4 -5 10.11 0.87 8 4 5 9.40 0.87 8 -4 5 10.26 0.96 -8 -4 5 9.13 0.76 8 -4 -5 9.05 0.75 -8 4 -5 9.53 0.86 -8 -4 -5 7.53 0.76 8 4 -5 8.55 0.84 8 -4 5 8.11 0.69 -8 -4 5 8.73 0.73 -8 -4 -5 9.61 0.94 8 -4 5 10.73 1.07 8 4 -5 10.27 0.92 -8 -4 5 9.30 0.87 -8 4 -5 8.46 0.71 -8 4 5 7.56 0.76 8 -4 -5 9.83 0.86 -8 4 5 8.06 0.85 8 -4 5 8.44 0.86 -8 4 -5 9.55 0.84 8 4 5 8.47 0.95 -8 -4 -5 9.21 0.99 8 4 -5 8.10 0.85 -8 4 5 8.06 0.87 -8 -4 5 8.92 0.85 -8 4 -5 9.19 0.75 -8 4 5 9.65 0.87 8 -5 5 1.98 0.55 8 5 -5 3.97 0.41 -8 5 -5 3.60 0.63 8 -5 -5 4.22 0.63 8 5 5 3.28 0.83 8 5 5 2.49 0.65 -8 -5 -5 4.41 0.48 8 -5 5 2.70 0.71 8 -5 -5 3.77 0.50 -8 5 -5 2.90 0.61 -8 -5 5 1.92 0.49 8 -5 5 1.57 0.36 -8 -5 5 2.40 0.62 8 5 -5 4.33 0.58 -8 -5 5 2.16 0.60 -8 -5 -5 4.67 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59.24 4.05 -10 10 -3 54.46 4.00 10 -10 -3 54.72 4.02 -10 -10 3 57.65 4.03 10 -10 3 58.18 3.86 10 10 3 47.14 4.23 10 -10 -3 52.38 3.76 10 -10 3 59.17 4.19 -10 -10 3 56.92 4.21 10 10 3 73.78 4.17 -10 -10 -3 49.28 4.08 10 10 -3 73.60 4.32 -10 10 -3 54.66 3.94 -10 -10 -3 54.01 4.11 -10 -10 3 57.25 3.96 -10 10 3 53.42 3.99 -10 10 -3 55.07 4.04 10 -10 3 58.27 4.02 10 -10 -3 54.11 4.01 -10 -10 3 59.43 4.14 10 10 -3 56.33 4.06 10 10 -3 44.18 3.97 10 -10 -3 59.74 3.98 10 -11 3 2.31 1.07 10 11 -3 2.56 1.21 -10 -11 3 2.99 1.06 10 -11 -3 2.13 1.05 10 -11 3 4.03 0.70 -10 -11 3 2.15 1.13 -10 -11 3 3.33 1.03 10 -11 3 1.67 1.33 10 11 -3 3.74 1.43 -10 -11 3 3.62 1.28 10 11 3 3.07 1.18 -10 -11 -3 2.47 1.11 -10 11 3 3.26 1.01 -10 -11 3 3.70 0.87 -10 11 -3 2.98 0.89 -10 -11 -3 3.65 1.13 -10 11 -3 2.64 1.09 10 11 -3 4.15 1.15 10 -11 3 3.59 1.06 10 -11 -3 3.30 0.92 10 11 -3 2.48 0.92 10 11 3 0.87 1.24 -10 -12 3 1.27 1.17 10 -12 -3 0.36 1.17 10 -12 3 2.38 0.67 -10 -12 3 1.47 1.25 -10 -12 3 1.95 1.10 10 12 3 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1.12 -10 15 -3 3.51 1.11 -10 15 3 1.91 1.33 10 -15 3 1.78 1.31 -10 -15 -3 1.57 1.80 10 -15 3 1.28 1.52 10 15 3 0.69 1.61 10 15 -3 1.48 1.23 -10 -15 3 4.68 1.43 -10 -15 3 1.94 1.68 10 -16 3 4.63 1.79 -10 16 3 4.12 1.61 10 16 3 3.44 1.76 -10 -16 -3 3.06 1.90 10 -16 3 5.30 1.45 -10 -16 3 4.00 1.90 -10 -16 3 2.36 1.45 -10 16 -3 5.88 1.54 10 16 3 8.16 1.68 -10 16 3 3.06 1.32 10 16 -3 7.57 1.90 -10 17 3 0.56 1.67 10 -17 -3 1.20 1.77 -10 -17 3 2.67 1.61 -10 -17 -3 0.76 1.83 10 17 3 2.73 1.85 -10 17 -3 1.70 1.62 10 17 3 1.50 1.61 -10 17 3 1.94 1.37 10 17 -3 -1.52 1.89 -10 -18 -3 14.55 2.35 10 -18 -3 16.07 2.32 10 18 3 14.66 2.11 -10 0 4 33.70 2.50 -10 0 4 37.26 2.48 10 0 -4 36.37 2.49 10 0 4 36.24 2.46 -10 0 4 34.96 2.52 10 0 -4 33.37 2.49 -10 0 -4 39.34 2.52 -10 0 -4 34.40 2.47 -10 0 4 32.70 2.44 10 0 4 32.37 2.52 10 0 4 35.89 2.47 -10 -1 4 89.41 6.07 10 -1 4 89.97 5.98 -10 1 4 89.31 6.06 -10 1 -4 89.85 6.07 10 -1 -4 89.02 6.01 10 -1 -4 92.73 6.07 10 1 -4 86.84 6.06 10 -1 4 90.76 6.03 10 1 4 91.48 6.06 -10 1 4 91.56 6.09 10 1 -4 87.83 6.07 -10 -1 4 87.79 6.09 -10 1 -4 89.31 6.07 10 1 -4 83.80 6.07 -10 -1 -4 92.38 6.07 -10 -1 -4 89.67 6.10 -10 1 -4 91.86 6.04 -10 1 -4 86.09 6.06 10 -1 4 90.75 6.10 10 1 4 90.29 6.11 -10 -1 4 85.27 6.02 10 -1 4 92.52 6.07 10 1 4 89.97 6.03 -10 -2 -4 64.84 4.40 -10 -2 4 64.75 4.53 10 2 -4 70.39 4.54 -10 2 -4 61.33 4.49 10 -2 -4 58.56 4.43 -10 -2 4 63.57 4.46 10 2 4 80.94 4.62 -10 2 -4 61.32 4.50 -10 2 4 61.54 4.48 10 -2 -4 60.08 4.49 -10 -2 -4 68.78 4.56 10 2 4 81.01 4.57 10 -2 4 68.97 4.46 10 2 -4 78.42 4.56 -10 2 -4 61.07 4.45 -10 2 -4 64.45 4.49 10 2 -4 83.76 4.56 -10 -2 4 77.94 4.58 -10 -2 -4 74.00 4.59 10 -2 4 63.13 4.53 -10 -2 4 62.95 4.39 10 2 4 61.61 4.47 -10 2 4 60.82 4.52 10 -3 4 111.44 7.39 -10 -3 4 110.92 7.27 10 3 -4 109.79 7.36 -10 3 -4 106.69 7.33 10 -3 4 99.74 7.53 -10 -3 4 109.22 7.35 10 3 -4 107.15 7.36 -10 3 4 108.31 7.36 10 -3 -4 110.85 7.36 -10 3 -4 98.57 7.34 -10 -3 -4 104.96 7.40 10 3 4 112.11 7.38 10 3 -4 108.05 7.36 10 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2.58 10 -5 -4 32.72 2.56 10 -5 4 35.72 2.60 10 5 -4 35.37 2.57 -10 -5 -4 35.45 2.68 -10 5 4 36.58 2.60 -10 5 4 36.28 2.57 10 -5 -4 33.45 2.56 -10 5 -4 34.21 2.50 10 6 -4 8.86 0.88 10 -6 4 9.15 0.99 10 6 4 8.34 1.24 10 -6 -4 9.03 1.02 10 6 4 8.25 1.06 -10 6 -4 9.00 0.95 -10 -6 4 8.50 0.92 10 -6 -4 10.46 0.89 10 -6 4 9.33 0.81 -10 -6 4 9.60 1.11 10 -6 4 9.52 0.84 -10 -6 -4 9.16 1.23 -10 -6 4 7.42 1.08 -10 -6 -4 9.75 1.12 10 -6 4 9.18 1.12 10 -6 4 8.79 1.10 -10 -6 4 10.39 1.40 10 6 -4 9.89 1.12 10 6 4 9.89 0.91 -10 6 4 9.17 0.85 -10 6 -4 9.95 0.75 10 -6 4 9.23 1.03 -10 6 4 9.29 1.03 10 -6 -4 10.14 1.03 -10 6 -4 10.52 0.99 10 6 -4 8.71 1.02 -10 -6 -4 9.88 1.27 -10 6 4 9.59 1.04 -10 6 -4 8.59 0.84 10 -6 -4 8.17 0.99 -10 -6 4 9.15 1.05 -10 6 4 9.97 1.00 10 -7 -4 35.14 2.87 10 -7 4 43.69 2.88 10 7 4 35.54 3.05 10 7 -4 35.91 2.77 10 7 4 43.11 2.93 10 7 -4 38.08 2.90 -10 7 -4 38.61 2.83 -10 -7 4 40.78 2.82 10 7 -4 35.88 2.67 10 -7 -4 36.12 2.79 10 -7 4 41.09 2.96 -10 -7 4 44.92 2.89 -10 -7 4 41.32 2.93 10 -7 4 41.62 2.74 10 -7 4 43.16 2.75 -10 -7 4 46.39 2.93 -10 -7 -4 39.92 3.06 -10 -7 -4 38.58 2.93 10 -7 4 41.67 2.90 10 7 4 47.45 2.87 10 7 -4 36.03 2.96 -10 -7 4 41.13 3.12 -10 7 4 40.91 2.79 10 -7 4 42.71 2.89 -10 7 -4 35.49 2.85 -10 7 4 38.72 2.88 10 -7 -4 37.31 2.85 -10 -7 -4 37.92 3.06 10 7 -4 37.97 2.87 -10 7 4 40.39 2.89 10 -7 -4 35.16 2.83 -10 7 4 38.76 2.82 -10 7 -4 37.83 2.73 10 8 4 1.34 0.99 10 8 -4 3.06 0.65 10 8 4 2.27 0.99 10 -8 4 1.41 0.79 10 -8 -4 2.64 0.90 10 8 -4 3.98 0.93 10 -8 -4 2.23 0.76 -10 -8 4 2.34 0.77 -10 8 -4 2.72 0.78 -10 -8 4 2.35 0.79 10 -8 4 1.96 0.54 -10 -8 4 1.67 0.88 -10 -8 -4 3.38 1.15 -10 -8 -4 3.77 1.05 -10 -8 4 2.06 0.60 10 -8 4 1.61 0.76 10 8 -4 2.04 0.39 10 8 4 2.73 0.88 -10 -8 -4 1.35 1.03 10 8 -4 2.06 1.04 -10 -8 4 2.60 1.13 -10 8 4 2.33 0.70 -10 8 -4 3.70 0.87 -10 8 4 3.36 0.88 -10 -8 -4 2.25 1.10 10 -8 4 2.52 0.85 10 -8 -4 1.98 0.82 10 8 -4 2.58 0.86 -10 8 -4 2.79 0.52 10 -8 -4 2.88 0.78 -10 8 4 2.02 0.86 10 9 -4 23.20 2.11 10 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1.09 0.90 -25 -2 -4 0.67 1.40 25 2 -4 0.96 1.56 25 -2 -4 1.89 1.52 -25 2 -4 0.24 0.94 -25 3 -4 3.63 1.45 -25 3 4 3.42 1.49 25 3 -4 3.14 1.04 -25 -3 -4 4.31 1.64 25 -3 -4 3.76 1.55 25 3 -4 4.22 1.70 -25 3 -4 4.66 1.05 -25 -4 -4 3.45 1.63 -25 4 -4 2.04 1.03 -25 4 -4 0.40 1.39 -25 4 4 2.13 1.45 25 4 -4 2.19 1.67 -25 -5 -4 2.06 1.65 25 5 -4 0.27 1.58 -25 5 4 1.60 1.44 -25 5 -4 2.81 1.41 -25 6 -4 6.27 1.50 -25 7 -4 3.21 1.37 25 0 -5 1.13 1.55 -25 0 5 2.85 1.51 -25 0 -5 1.44 1.56 -25 -1 -5 1.99 1.48 -25 1 -5 1.23 1.05 25 1 -5 2.42 1.57 25 -1 -5 2.31 1.47 -25 1 5 0.22 1.47 -25 -1 -5 3.01 1.59 -25 1 -5 4.66 1.63 -25 -2 -5 1.85 1.55 -25 2 5 -0.43 1.43 -25 2 -5 1.20 1.51 25 2 -5 0.92 0.95 -25 -2 -5 2.24 1.50 25 2 -5 0.23 1.50 25 -2 -5 0.65 1.50 -25 2 -5 1.11 1.05 -25 3 -5 7.70 1.57 25 3 -5 4.55 1.13 -25 -3 -5 4.67 1.65 -25 3 -5 4.59 1.18 25 -3 -5 5.10 1.57 25 3 -5 5.59 1.67 -25 -4 -5 0.77 1.68 -25 4 -5 1.83 1.14 -25 4 -5 1.49 1.42 25 4 -5 1.38 1.58 -25 -5 -5 3.91 1.68 -25 5 -5 0.93 1.32 -25 5 -5 2.15 1.18 25 5 -5 3.01 1.66 25 -6 5 -0.44 1.51 -25 6 -5 2.04 1.41 -25 7 -5 5.19 1.42 25 0 -6 0.33 1.48 -25 0 -6 1.45 1.51 -25 -1 -6 1.88 1.36 -25 1 -6 1.27 1.13 25 1 -6 1.58 1.54 25 -1 -6 2.47 1.49 -25 -1 -6 1.66 1.55 -25 1 -6 1.04 1.52 -25 -2 -6 4.34 1.72 -25 2 -6 2.08 1.56 25 2 -6 1.89 1.04 -25 -2 -6 4.27 1.52 25 2 -6 5.40 1.64 25 -2 -6 2.68 1.51 -25 2 -6 2.18 1.16 -25 3 -6 1.99 1.41 25 3 -6 1.37 1.12 -25 -3 -6 3.01 1.51 25 3 -6 2.48 1.62 25 -3 -6 4.05 1.58 -25 3 -6 2.45 1.13 -25 4 -6 4.38 1.47 25 4 -6 2.36 1.16 -25 -4 -6 5.20 1.72 -25 4 -6 4.07 1.25 25 4 -6 3.31 1.63 -25 -5 -6 1.14 1.67 -25 5 -6 2.54 1.40 -25 5 -6 1.50 1.22 25 5 -6 3.44 1.65 -25 6 -6 11.74 1.59 -25 6 -6 11.23 1.70 25 -6 6 11.84 1.91 -25 0 -7 -0.74 1.55 25 0 -7 0.32 1.46 -25 -1 -7 3.32 1.49 25 1 -7 3.20 1.57 25 -1 -7 1.80 1.43 -25 -1 -7 2.35 1.65 -25 1 -7 0.12 1.48 -25 2 -7 4.74 1.52 25 2 -7 3.58 1.16 -25 -2 -7 4.94 1.59 25 -2 -7 4.62 1.62 25 2 -7 4.40 1.64 -25 2 -7 4.58 1.28 -25 3 -7 2.53 1.45 25 3 -7 2.58 1.15 -25 -3 -7 3.15 1.62 25 3 -7 2.87 1.55 25 -3 -7 3.56 1.51 -25 3 -7 2.85 1.22 -25 4 -7 7.39 1.71 25 4 -7 10.03 1.50 -25 -4 -7 9.36 1.91 25 4 -7 11.13 1.90 -25 4 -7 9.96 1.51 -25 5 -7 2.65 1.44 -25 5 -7 1.21 1.28 25 5 -7 0.12 1.60 -25 6 -7 15.20 1.85 -25 6 -7 16.61 1.89 25 -6 7 16.43 2.11 -25 0 -8 0.50 1.57 25 0 -8 1.67 1.50 -25 -1 -8 4.65 1.50 25 1 -8 1.50 1.49 25 -1 -8 1.24 1.54 -25 -1 -8 0.53 1.65 -25 1 -8 4.02 1.60 -25 2 -8 6.39 1.66 25 2 -8 5.30 1.29 -25 -2 -8 6.96 1.68 25 -2 -8 9.05 1.61 25 2 -8 7.16 1.70 -25 2 -8 5.14 1.40 -25 3 -8 2.55 1.50 25 3 -8 0.14 1.19 -25 -3 -8 1.22 1.54 25 3 -8 -0.22 1.52 25 -3 -8 0.93 1.48 -25 3 -8 2.06 1.30 -25 4 -8 15.73 2.03 25 4 -8 18.73 1.85 -25 -4 -8 17.14 2.19 25 4 -8 13.34 2.11 -25 4 -8 15.19 1.89 25 5 -8 -0.42 1.29 -25 5 -8 1.63 1.36 -25 5 -8 2.75 1.44 25 5 -8 1.81 1.63 -25 6 -8 32.27 2.68 25 -6 8 26.57 2.80 25 -7 8 1.49 1.56 -25 0 9 0.83 1.47 -25 0 -9 1.15 1.62 25 0 -9 0.82 1.55 -25 -1 9 0.20 1.52 -25 1 -9 1.08 1.58 -25 -1 -9 1.75 1.41 25 -1 -9 3.45 1.53 25 1 -9 -0.52 1.51 25 -2 -9 8.16 1.69 25 2 -9 10.42 1.81 -25 2 -9 8.28 1.80 25 2 -9 7.47 1.38 -25 -2 -9 4.72 1.72 -25 -2 9 10.30 1.75 -25 3 -9 2.35 1.54 25 3 -9 2.47 1.29 -25 -3 -9 2.46 1.65 25 3 -9 4.40 1.60 25 -3 -9 3.94 1.57 -25 3 -9 4.90 1.42 -25 4 -9 19.85 2.30 25 4 -9 16.35 2.10 -25 4 -9 20.12 2.16 25 4 -9 22.90 2.39 25 5 -9 -1.05 1.60 25 5 -9 -0.09 1.35 -25 5 -9 0.57 1.42 25 -5 9 1.38 1.57 -25 5 -9 1.26 1.46 -25 6 -9 35.07 3.01 25 6 -9 36.41 3.20 25 -6 9 37.22 3.13 25 6 -9 32.79 3.03 25 -7 9 4.31 1.59 -25 7 -9 2.82 1.55 25 0 -10 0.10 1.52 -25 1 -10 0.24 1.64 -25 -1 -10 0.71 1.47 25 -1 -10 3.07 1.54 25 1 -10 2.22 1.56 -25 -1 10 1.76 1.53 -25 2 -10 4.93 1.67 -25 -2 10 3.75 1.55 -25 -2 -10 4.61 1.67 25 -2 -10 3.75 1.55 25 2 -10 4.14 1.64 25 3 -10 1.39 1.62 25 -3 -10 1.39 1.56 -25 3 -10 3.54 1.58 -25 -3 -10 0.12 1.64 25 3 -10 2.42 1.38 -25 3 -10 -0.27 1.53 -25 -3 10 0.20 1.49 25 4 -10 9.31 1.94 -25 4 -10 11.23 1.87 -25 -4 -10 12.49 2.11 25 4 -10 9.17 1.69 -25 -4 10 10.89 1.82 -25 4 -10 13.54 1.83 -25 5 -10 1.00 1.52 25 5 -10 1.38 1.44 -25 -5 10 -1.06 1.49 25 5 -10 2.36 1.67 25 -5 10 0.10 1.54 -25 6 -10 22.42 2.29 25 6 -10 20.12 2.28 -25 -6 10 19.02 2.19 25 6 -10 19.27 2.39 25 -6 10 17.78 2.26 25 -7 10 2.06 1.60 -25 7 -10 2.16 1.62 25 7 -10 2.33 1.66 25 0 -11 1.36 1.50 -25 1 -11 1.37 1.63 25 -1 -11 2.41 1.51 25 1 -11 1.18 1.49 -25 2 -11 1.97 1.60 -25 -2 11 2.27 1.57 -25 -2 -11 3.37 1.60 25 -2 -11 1.16 1.56 25 2 -11 2.49 1.56 25 -3 -11 0.97 1.50 25 3 -11 2.99 1.67 -25 3 -11 2.73 1.61 -25 -3 -11 3.64 1.66 25 3 -11 1.23 1.48 -25 -3 11 -0.10 1.59 -25 3 -11 4.19 1.68 -25 4 -11 8.94 1.84 -25 -4 -11 11.89 2.06 25 4 -11 11.05 1.74 -25 -4 11 6.44 1.80 25 4 -11 9.77 1.82 25 5 -11 2.01 1.51 -25 -5 11 0.68 1.52 -25 5 -11 1.07 1.59 25 -5 11 1.83 1.53 -25 6 -11 12.91 1.98 25 6 -11 10.47 1.92 25 -6 11 13.61 1.91 25 0 -12 2.35 1.49 25 1 -12 1.91 1.49 25 -1 -12 -0.19 1.46 -25 2 -12 2.24 1.64 25 -2 -12 3.59 1.60 -25 3 -12 0.21 1.55 -25 3 -12 1.32 1.55 -25 -3 12 -0.82 1.55 25 4 -12 4.59 1.62 -25 -4 12 3.89 1.58 25 -4 12 3.64 1.63 -25 4 -12 4.69 1.74 -25 5 -12 2.93 1.72 -25 -5 12 -0.78 1.49 25 5 -12 1.50 1.54 -25 3 -13 0.68 1.73 -25 -4 13 -0.10 1.57 25 5 -13 2.22 1.65 -26 2 0 0.11 1.55 -26 3 0 2.57 1.58 -26 4 0 3.10 1.61 -26 5 0 0.60 1.44 -26 1 -1 8.56 1.78 -26 2 -1 88.27 6.44 -26 3 -1 9.09 1.73 -26 -3 -1 10.35 1.91 -26 4 -1 103.02 7.35 -26 5 -1 7.13 1.60 -26 6 -1 14.62 1.91 -26 7 -1 6.28 1.54 -26 1 -2 1.53 1.60 -26 2 -2 27.61 2.68 -26 -2 -2 27.71 2.70 -26 3 -2 2.48 1.52 -26 -3 -2 2.24 1.71 -26 4 -2 14.80 1.98 -26 5 -2 1.98 1.45 -26 6 -2 6.78 1.56 -26 7 -2 0.36 1.41 -26 1 -3 3.31 1.63 -26 2 -3 6.12 1.63 -26 -2 -3 9.15 1.72 -26 3 -3 1.09 1.50 -26 -3 -3 1.25 1.53 -26 4 -3 24.83 2.49 -26 5 -3 2.07 1.46 -26 6 -3 4.13 1.49 -26 7 -3 2.08 1.43 -26 1 -4 1.55 1.63 -26 2 -4 8.19 1.76 -26 -2 -4 13.03 1.91 -26 3 -4 3.27 1.57 -26 -3 -4 2.37 1.66 -26 4 -4 4.04 1.52 -26 5 -4 1.57 1.45 -26 6 -4 4.77 1.52 -26 7 -4 0.44 1.40 -26 1 -5 5.03 1.68 26 1 -5 1.09 1.64 -26 2 -5 2.75 1.63 -26 -2 -5 3.51 1.60 -26 3 -5 3.50 1.59 -26 -3 -5 2.89 1.71 -26 4 -5 11.17 1.84 -26 5 -5 0.39 1.47 -26 6 -5 -0.28 1.39 26 1 -6 2.03 1.57 -26 -1 -6 0.54 1.50 -26 1 -6 3.61 1.57 -26 -2 -6 2.81 1.58 -26 2 -6 2.19 1.57 -26 -3 -6 0.38 1.58 -26 3 -6 0.66 1.51 -26 4 -6 10.98 1.86 -26 5 -6 1.47 1.48 -26 6 -6 1.57 1.44 -26 -1 -7 0.22 1.52 26 1 -7 0.12 1.59 -26 1 -7 0.35 1.28 26 2 -7 32.33 2.92 -26 2 -7 31.00 2.84 -26 -2 -7 25.06 2.79 -26 3 -7 0.33 1.53 -26 -3 -7 -0.51 1.60 -26 4 -7 34.98 3.12 -26 5 -7 0.99 1.47 26 1 -8 2.13 1.60 -26 -1 -8 1.08 1.46 -26 -2 -8 4.45 1.66 -26 2 -8 5.16 1.45 -26 3 -8 2.45 1.61 -26 -3 -8 1.66 1.66 -26 4 -8 12.17 1.97 -26 5 -8 0.89 1.53 -26 -1 -9 7.94 1.76 -26 -2 -9 56.95 4.54 -26 2 -9 58.20 4.36 -26 3 -9 5.26 1.74 -26 -3 -9 7.84 1.84 -26 3 -9 8.55 1.65 -26 4 -9 61.08 4.71 26 -5 9 5.02 1.75 -26 2 -10 8.78 1.77 -26 3 -10 2.55 1.53 -26 -3 -10 1.04 1.65 -26 -5 10 -0.50 1.58 26 -5 10 -0.44 1.65 -26 3 -11 7.39 1.78 -26 3 -12 0.21 1.72 0 0 0 0.00 0.00 TITL NIMS_PZDI_1 in Pnma REM Pnma (#62, found as Pcmn in -cba setting) CELL 0.71073 20.394136 19.285071 13.742544 90.0000 90.0000 90.0000 ZERR 21.00 0.000335 0.000282 0.000233 0.0000 0.0000 0.0000 LATT 1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z SYMM x+1/2,-y+1/2,-z+1/2 SFAC C H N I Pb UNIT 168.00 504.00 84.00 42.00 21.00 SIZE 0.09 0.19 0.35 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 84696 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling - B-factor correction ; _oxdiff_exptl_absorpt_empirical_full_max 1.836 _oxdiff_exptl_absorpt_empirical_full_min 0.753