#------------------------------------------------------------------------------ #$Date: 2021-04-23 04:44:12 +0300 (Fri, 23 Apr 2021) $ #$Revision: 264436 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707174.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7707174 loop_ _publ_author_name 'Lin, Lin' 'Jiang, Xingxing' 'Wu, Chao' 'Lin, Zheshuai' 'Huang, Zhipeng' 'Humphrey, Mark G.' 'Zhang, Chi' _publ_section_title ; First chiral fluorinated lead vanadate selenite Pb2(V2O4F)(VO2)(SeO3)3 with five asymmetric motifs and large optical properties ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00536G _journal_year 2021 _chemical_formula_sum 'F O15 Pb2 Se3 V3' _chemical_formula_weight 1063.08 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2021-02-17 deposited with the CCDC. 2021-04-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.2548(2) _cell_length_b 12.0864(5) _cell_length_c 21.0937(10) _cell_measurement_reflns_used 3724 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.0301 _cell_measurement_theta_min 3.3522 _cell_volume 1339.69(10) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type bruker-CCD _diffrn_measurement_method 'w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0511 _diffrn_reflns_av_unetI/netI 0.0712 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 8102 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.098 _diffrn_reflns_theta_min 3.352 _exptl_absorpt_coefficient_mu 35.312 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_correction_T_min 0.2541 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 5.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rodlike _exptl_crystal_F_000 1856 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _refine_diff_density_max 1.497 _refine_diff_density_min -1.810 _refine_diff_density_rms 0.370 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.021(14) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 2927 _refine_ls_number_restraints 48 _refine_ls_restrained_S_all 0.987 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0347 _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^)+(0.0180P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0654 _refine_ls_wR_factor_ref 0.0687 _reflns_Friedel_coverage 0.699 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 2504 _reflns_number_total 2927 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00536g2.cif _cod_data_source_block 1 _cod_database_code 7707174 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P2(1)2(1)2(1) New: P212121 CELL 0.71073 5.2548 12.0864 21.0937 90.000 90.000 90.000 ZERR 4 0.0002 0.0005 0.0010 0.000 0.000 0.000 LATT -1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC F O Pb Se V UNIT 4 60 8 12 12 L.S. 20 ACTA BOND $H FMAP 2 PLAN -20 CONF TWIN ISOR 0.001 O1 O3 O6 O7 O10 O12 O13 O14 WGHT 0.018000 SWAT 0.076786 0.2340 BASF 0.02125 FVAR 0.04913 PB1 3 0.489015 0.281084 0.575514 11.00000 0.01254 0.01624 = 0.01220 0.00213 0.00001 0.00226 PB2 3 0.502983 0.470220 0.778883 11.00000 0.01608 0.01415 = 0.01430 0.00081 0.00109 -0.00045 SE1 4 0.514009 -0.009175 0.490944 11.00000 0.01271 0.00769 = 0.00479 -0.00028 -0.00119 -0.00204 SE2 4 0.137976 0.225969 0.713720 11.00000 0.00692 0.00472 = 0.00481 -0.00006 0.00016 0.00018 SE3 4 -0.049735 0.318471 0.885045 11.00000 0.00537 0.00499 = 0.00676 -0.00024 0.00049 -0.00106 V1 5 0.517935 0.022846 0.339986 11.00000 0.00691 0.00696 = 0.01050 0.00214 -0.00010 -0.00152 V2 5 0.465531 0.172244 0.853750 11.00000 0.00683 0.00535 = 0.00726 0.00130 -0.00142 -0.00188 V3 5 0.946587 0.086057 0.588788 11.00000 0.01209 0.00425 = 0.00422 -0.00052 -0.00156 0.00119 F1 1 1.015441 0.509362 0.748620 11.00000 0.02680 0.01883 = 0.00947 -0.00687 -0.00113 0.00720 O1 2 0.372919 -0.097469 0.361319 11.00000 0.00626 0.00608 = 0.00569 -0.00018 0.00041 -0.00073 O2 2 0.630895 0.063178 0.425633 11.00000 0.01572 0.01692 = 0.00390 0.00425 -0.00436 -0.01287 O3 2 0.263611 0.352361 0.691482 11.00000 0.00529 0.00513 = 0.00548 0.00055 0.00060 -0.00015 O4 2 0.778822 0.390708 0.662485 11.00000 0.00695 0.01061 = 0.02056 0.00625 -0.00161 -0.00501 O5 2 0.373513 0.553977 0.665896 11.00000 0.00443 0.00796 = 0.01280 0.00021 -0.00142 -0.00123 O6 2 0.385865 0.172895 0.753374 11.00000 0.00743 0.00750 = 0.00743 0.00041 0.00014 0.00053 O7 2 0.734910 0.275744 0.828085 11.00000 0.00430 0.00463 = 0.00444 0.00027 0.00041 -0.00026 O8 2 0.511352 0.185652 0.928880 11.00000 0.02593 0.02025 = 0.01059 -0.00336 -0.00303 -0.00723 O9 2 0.224047 0.317966 0.842403 11.00000 0.00831 0.00426 = 0.01111 -0.00108 0.00221 -0.00051 O10 2 0.714666 0.100834 0.639462 11.00000 0.00916 0.00928 = 0.00888 -0.00050 0.00038 0.00020 O11 2 0.898045 0.193752 0.538701 11.00000 0.01501 0.01133 = 0.00961 -0.00062 -0.00073 0.00638 O12 2 0.196120 0.161297 0.642349 11.00000 0.00839 0.00891 = 0.00832 -0.00069 0.00025 -0.00041 O13 2 0.787095 -0.022683 0.534434 11.00000 0.01415 0.01334 = 0.01352 -0.00018 -0.00133 0.00008 O14 2 0.862422 0.452854 0.881760 11.00000 0.01262 0.01256 = 0.01300 -0.00024 -0.00064 -0.00051 O15 2 0.347110 0.093058 0.524531 11.00000 0.01202 0.01223 = 0.01655 -0.00497 0.00258 0.00217 HKLF 4 REM 1 in P2(1)2(1)2(1) New: P212121 REM R1 = 0.0347 for 2504 Fo > 4sig(Fo) and 0.0465 for all 2927 data REM 220 parameters refined using 48 restraints END WGHT 0.0208 0.0000 REM Highest difference peak 1.497, deepest hole -1.810, 1-sigma level 0.370 Q1 1 0.6675 0.4666 0.7812 11.00000 0.05 1.50 Q2 1 0.1998 -0.0028 0.3836 11.00000 0.05 1.36 Q3 1 0.0243 0.1576 0.9111 11.00000 0.05 1.29 Q4 1 0.4991 0.4573 0.8185 11.00000 0.05 1.26 Q5 1 0.1397 -0.0159 0.5140 11.00000 0.05 1.26 Q6 1 0.8684 -0.0241 0.5098 11.00000 0.05 1.25 Q7 1 0.5071 0.1165 0.4277 11.00000 0.05 1.23 Q8 1 0.5005 0.1692 0.8051 11.00000 0.05 1.23 Q9 1 0.9771 0.5242 0.8043 11.00000 0.05 1.22 Q10 1 0.4978 0.5192 0.7450 11.00000 0.05 1.20 Q11 1 0.1343 0.4942 0.8000 11.00000 0.05 1.18 Q12 1 0.6618 0.2649 0.6238 11.00000 0.05 1.13 Q13 1 0.9786 0.2945 0.5873 11.00000 0.05 1.13 Q14 1 0.9667 -0.0155 0.5306 11.00000 0.05 1.12 Q15 1 0.7698 0.2133 0.5125 11.00000 0.05 1.11 Q16 1 0.2337 0.1966 0.5119 11.00000 0.05 1.11 Q17 1 0.2217 -0.0979 0.3632 11.00000 0.05 1.11 Q18 1 0.3580 0.4813 0.7303 11.00000 0.05 1.10 Q19 1 0.2623 0.5451 0.8334 11.00000 0.05 1.09 Q20 1 0.2568 0.2377 0.6607 11.00000 0.05 1.07 ; _shelx_res_checksum 51424 _shelx_hkl_file ; 1 0 0 -0.25 0.24 2 0 0 1000.00 56.56 3 0 0 -0.27 0.58 4 0 0 521.91 29.97 5 0 0 -0.97 1.57 5 0 0 -2.22 1.66 6 0 0 217.20 13.55 6 0 0 213.59 13.40 -1 -1 0 1.11 0.32 1 -1 0 1.56 0.29 1 1 0 1.06 0.30 2 1 0 2.86 0.56 2 -1 0 2.97 0.55 2 -1 0 2.85 0.51 -2 -1 0 3.31 0.63 3 1 0 0.18 0.59 3 -1 0 0.19 0.61 3 -1 0 -0.01 0.56 4 1 0 95.06 6.82 4 -1 0 100.01 6.48 4 -1 0 112.72 6.49 5 -1 0 9.22 1.85 5 -1 0 7.58 1.59 5 1 0 6.94 1.62 6 -1 0 68.36 6.44 6 -1 0 68.53 5.39 6 1 0 62.78 5.54 6 1 0 65.37 5.74 0 2 0 3.25 0.47 0 -2 0 2.91 0.47 -1 -2 0 19.54 1.40 -1 2 0 18.93 1.32 1 -2 0 19.84 1.43 1 2 0 17.47 1.38 2 -2 0 39.14 2.52 2 2 0 38.62 2.58 -2 -2 0 37.34 2.57 3 -2 0 27.63 2.22 3 2 0 28.34 2.29 3 -2 0 30.08 2.16 4 -2 0 36.15 2.80 4 -2 0 35.75 2.90 4 2 0 33.98 2.93 5 -2 0 11.65 1.94 5 -2 0 14.14 1.97 5 2 0 12.23 2.07 6 -2 0 9.82 2.27 6 2 0 14.40 2.86 6 -2 0 7.50 2.36 6 2 0 6.96 2.47 0 3 0 -0.11 0.38 0 -3 0 -0.15 0.39 -1 3 0 29.87 2.26 1 3 0 33.59 2.18 1 -3 0 32.35 2.30 -1 -3 0 34.14 2.17 2 3 0 3.83 0.74 -2 3 0 4.90 0.72 2 -3 0 3.04 0.72 -2 -3 0 3.42 0.71 3 3 0 42.22 3.09 3 -3 0 45.33 3.06 -3 -3 0 43.31 3.17 4 -3 0 9.74 1.46 4 3 0 11.07 1.66 4 -3 0 11.13 1.62 5 -3 0 8.29 1.64 5 3 0 7.99 1.94 5 -3 0 10.43 1.87 6 -3 0 12.88 2.74 6 -3 0 14.39 3.07 0 -4 0 533.60 29.52 0 4 0 506.41 29.55 1 4 0 38.17 2.51 1 -4 0 38.42 2.61 -1 4 0 33.48 2.88 -1 -4 0 40.09 2.55 2 -4 0 395.50 24.88 2 4 0 450.92 24.91 -2 -4 0 446.57 24.91 -2 4 0 445.89 24.76 -3 -4 0 98.26 6.23 3 -4 0 97.33 6.19 3 4 0 100.30 6.23 4 4 0 174.81 10.58 4 -4 0 173.05 10.28 4 -4 0 170.06 10.49 5 4 0 -0.56 1.46 5 -4 0 0.64 1.56 5 -4 0 0.61 1.20 6 -4 0 145.80 9.47 6 -4 0 145.66 9.98 0 5 0 0.88 0.60 0 -5 0 0.03 0.48 1 -5 0 4.55 0.83 -1 -5 0 5.26 0.83 -1 5 0 4.75 1.34 1 5 0 4.47 0.84 2 5 0 30.03 2.32 2 -5 0 30.09 2.48 -2 5 0 31.77 2.22 -2 -5 0 28.03 2.31 3 -5 0 11.52 1.69 -3 -5 0 13.41 1.88 3 5 0 15.74 1.88 4 5 0 2.23 1.29 4 -5 0 1.13 1.38 -4 -5 0 0.64 1.59 5 -5 0 0.09 1.24 5 -5 0 1.39 1.76 5 5 0 0.78 1.66 6 -5 0 3.29 2.65 6 -5 0 -0.24 2.09 0 6 0 89.05 5.53 0 -6 0 87.29 5.39 -1 -6 0 281.05 15.92 -1 6 0 251.45 16.44 1 -6 0 285.49 15.88 1 6 0 279.51 15.96 -2 6 0 112.86 6.93 -2 -6 0 109.99 6.93 2 6 0 115.30 6.99 2 -6 0 111.42 6.93 -3 6 0 149.00 8.72 -3 -6 0 148.37 9.06 3 6 0 146.54 9.05 3 -6 0 142.96 9.06 4 6 0 89.46 6.10 -4 -6 0 90.67 6.04 4 -6 0 81.86 6.11 5 6 0 101.00 7.39 5 -6 0 98.34 7.35 5 -6 0 105.66 6.65 6 -6 0 4.28 3.09 0 -7 0 0.49 0.67 0 7 0 0.97 0.80 1 -7 0 6.37 0.98 -1 -7 0 6.18 1.06 -1 7 0 4.97 1.78 1 7 0 6.66 1.14 -2 -7 0 16.82 1.89 -2 7 0 16.49 2.27 2 7 0 17.44 2.41 2 -7 0 17.71 1.97 -3 7 0 2.10 0.84 3 -7 0 1.85 1.28 -3 -7 0 2.52 1.20 3 7 0 0.74 1.23 4 -7 0 6.20 1.82 -4 -7 0 8.61 1.91 5 -7 0 10.93 1.79 5 -7 0 11.64 2.61 6 -7 0 1.50 3.30 0 -8 0 4.94 1.04 0 8 0 4.09 1.23 1 8 0 69.02 4.64 -1 -8 0 65.18 4.48 1 -8 0 67.56 4.39 -1 8 0 65.42 5.58 -2 8 0 -1.77 1.43 -2 -8 0 0.62 1.02 2 8 0 1.58 1.23 2 -8 0 1.50 0.95 3 -8 0 -0.09 1.14 -3 -8 0 -0.40 1.14 3 8 0 2.46 1.49 -3 8 0 0.13 0.89 -4 -8 0 6.97 1.87 4 -8 0 5.57 1.81 5 -8 0 1.99 2.24 5 -8 0 0.95 2.22 0 -9 0 0.68 0.88 0 9 0 2.02 1.27 -1 9 0 0.28 1.95 -1 -9 0 1.68 1.06 1 -9 0 3.56 1.04 2 9 0 19.90 2.42 2 -9 0 16.56 2.11 -2 -9 0 19.78 2.43 -2 9 0 16.02 2.77 3 9 0 19.23 3.11 -3 9 0 19.30 2.29 -3 -9 0 21.90 2.88 3 -9 0 20.99 2.46 -4 -9 0 16.96 2.75 4 -9 0 22.09 3.01 5 -9 0 67.56 5.89 0 10 0 58.08 4.72 0 -10 0 49.36 3.83 1 -10 0 469.26 26.40 1 10 0 445.86 26.71 -1 10 0 453.10 27.52 -1 -10 0 463.94 26.55 -2 10 0 25.32 3.68 2 10 0 32.85 3.46 2 -10 0 32.17 2.74 -2 -10 0 30.33 3.28 3 -10 0 152.43 9.39 -3 -10 0 161.62 9.92 -3 10 0 146.93 9.47 -4 -10 0 14.86 2.70 4 -10 0 18.44 2.88 5 -10 0 68.76 7.72 0 11 0 1.80 1.95 0 -11 0 -0.58 1.12 -1 -11 0 2.05 1.40 1 11 0 3.04 1.85 -1 11 0 1.15 2.79 1 -11 0 2.82 1.22 2 -11 0 -0.16 1.10 2 11 0 1.78 2.21 -2 -11 0 0.34 1.60 -2 11 0 -0.98 2.82 -3 -11 0 3.36 1.86 3 11 0 2.79 2.29 3 -11 0 2.35 1.29 -3 11 0 -1.06 1.55 -4 -11 0 0.65 2.11 4 -11 0 1.02 1.54 0 12 0 9.17 2.60 0 -12 0 7.82 1.76 1 -12 0 17.28 2.45 1 12 0 14.80 4.17 -1 12 0 18.81 3.98 -1 -12 0 12.60 2.13 -2 -12 0 6.71 2.25 -2 12 0 3.88 3.40 2 -12 0 7.85 1.55 3 -12 0 2.01 1.45 -3 -12 0 0.89 2.12 -3 12 0 0.34 1.84 4 -12 0 8.23 2.76 -4 -12 0 8.79 2.91 0 13 0 1.32 2.83 0 -13 0 0.45 1.63 1 -13 0 0.47 1.50 -1 13 0 10.63 3.95 -1 -13 0 3.43 1.90 -2 13 0 6.87 3.86 2 13 0 8.11 3.25 -2 -13 0 10.38 2.45 2 -13 0 8.59 1.78 3 -13 0 7.99 1.77 -3 -13 0 4.85 2.57 0 -14 0 4.81 1.97 1 14 0 81.11 7.81 -1 -14 0 86.75 6.35 1 -14 0 75.14 5.95 2 -14 0 2.23 1.76 -2 -14 0 5.31 2.58 -2 14 0 6.21 4.03 0 15 0 -5.98 4.08 0 -15 0 2.32 2.11 -1 -15 0 6.90 2.65 1 -15 0 9.31 2.34 -1 0 1 78.28 4.57 1 0 -1 79.54 4.57 2 0 1 -0.26 0.38 2 0 -1 0.46 0.37 3 0 1 248.21 14.63 3 0 -1 255.95 14.60 4 0 1 0.08 1.05 4 0 -1 1.28 0.92 4 0 1 2.22 1.13 5 0 -1 101.80 6.91 5 0 -1 107.35 7.06 5 0 1 108.32 7.00 6 0 1 -1.89 2.15 6 0 -1 0.10 1.89 6 0 1 -4.00 1.94 6 0 -1 0.37 2.19 -1 -1 -1 27.26 1.91 1 1 -1 29.74 1.92 1 -1 1 30.20 1.93 -1 -1 1 29.85 1.92 -1 1 -1 32.22 1.92 1 1 1 31.77 1.93 2 -1 1 33.04 2.32 2 1 -1 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6 86.96 5.43 3 -3 6 72.68 5.08 3 3 -6 69.97 4.79 -3 3 -6 75.59 4.96 3 -3 -6 75.05 4.41 -3 -3 6 68.17 4.83 3 -3 -6 75.14 4.37 4 -3 6 87.85 6.74 4 3 -6 88.86 6.44 4 -3 -6 103.93 6.47 4 3 6 108.74 6.68 -4 -3 6 103.89 6.64 4 -3 -6 107.87 6.19 5 3 -6 35.84 3.67 5 -3 6 32.33 3.62 5 -3 6 35.30 4.25 5 -3 -6 37.51 3.07 5 -3 -6 45.83 3.35 -5 -3 6 36.68 3.86 5 3 6 32.80 3.90 5 3 6 44.34 4.10 6 -3 6 9.79 5.65 6 3 -6 7.62 3.02 6 -3 6 10.32 3.08 6 3 6 11.38 3.07 6 -3 -6 12.77 2.18 6 -3 -6 13.24 2.38 0 -4 6 56.76 4.15 0 4 6 58.88 3.44 0 4 -6 54.37 4.14 1 -4 6 2.20 1.26 1 4 -6 -1.12 0.71 -1 4 -6 0.22 1.22 1 4 6 0.80 0.52 -1 -4 6 0.68 0.85 2 4 -6 20.45 1.92 2 -4 6 19.79 2.49 -2 4 -6 13.76 2.22 2 4 6 14.73 1.60 -2 -4 6 17.84 1.86 3 -4 6 11.10 1.98 3 -4 -6 14.83 1.11 3 -4 -6 12.83 1.82 -3 4 -6 14.57 2.15 -3 -4 6 15.25 2.05 3 4 6 15.20 1.83 4 4 -6 18.93 2.46 4 -4 6 19.81 3.04 -4 -4 6 18.66 2.54 4 -4 -6 14.40 1.49 4 -4 -6 16.82 1.80 5 -4 6 5.54 2.40 5 4 -6 7.92 1.97 5 4 6 6.00 2.17 5 -4 -6 5.17 1.40 5 -4 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19.88 2.09 2 0 11 21.19 2.28 3 0 11 21.47 2.58 3 0 -11 21.49 2.28 -3 0 11 24.15 2.25 4 0 11 3.06 1.82 -4 0 11 1.62 1.20 4 0 -11 5.36 1.32 5 0 -11 2.65 1.54 5 0 11 4.85 2.21 5 0 11 4.23 2.19 6 0 -11 2.26 2.53 6 0 11 0.09 3.14 0 -1 -11 47.24 3.31 0 1 -11 45.47 3.62 0 1 11 47.01 3.71 0 -1 11 53.29 4.24 -1 -1 -11 66.31 4.19 1 1 -11 63.16 4.34 -1 1 11 57.01 4.90 1 -1 11 60.06 4.56 -1 -1 11 64.21 5.13 1 1 11 61.12 4.27 -1 1 -11 59.94 4.33 1 -1 -11 61.22 4.09 -2 1 11 94.80 5.97 2 -1 11 89.76 6.30 2 1 -11 93.88 6.16 -2 1 -11 96.99 6.35 2 -1 -11 97.48 5.98 2 1 11 100.31 6.23 -2 -1 11 97.41 6.37 3 1 -11 54.31 4.27 -3 1 11 54.54 3.98 3 -1 11 54.01 4.56 3 1 11 66.71 4.58 3 -1 -11 67.10 4.18 -3 -1 11 69.32 4.41 -4 1 11 54.07 3.99 4 -1 11 50.53 4.58 4 -1 -11 60.57 4.08 4 1 11 59.81 4.72 -4 -1 11 60.09 4.38 5 -1 11 49.38 5.49 5 1 -11 62.75 4.84 5 -1 -11 58.94 4.99 -5 -1 11 58.79 5.22 5 1 11 64.47 5.24 5 1 11 66.50 5.54 6 -1 11 2.98 3.07 6 1 -11 1.52 2.35 6 1 11 4.46 3.12 0 2 -11 2.76 1.24 0 2 11 3.40 1.08 0 -2 -11 2.63 0.72 0 -2 11 2.18 1.59 1 2 -11 367.12 21.89 1 -2 11 347.86 22.06 -1 -2 -11 384.65 21.65 1 -2 -11 390.52 21.52 -1 2 -11 381.11 22.06 1 2 11 384.44 21.71 -1 -2 11 371.01 22.37 2 2 -11 23.19 2.39 -2 2 11 23.06 1.76 2 -2 11 24.38 2.67 -2 2 -11 17.37 2.49 2 -2 -11 19.07 1.78 -2 -2 11 17.51 2.65 2 2 11 16.89 2.00 -3 2 11 118.29 6.97 3 -2 11 124.20 7.90 3 2 -11 122.41 7.49 3 -2 -11 111.80 7.07 3 2 11 114.89 7.46 -3 2 -11 113.31 7.68 -3 -2 11 114.03 7.54 4 2 -11 0.37 1.32 4 -2 11 2.67 2.01 -4 -2 11 1.41 1.51 4 2 11 -0.38 1.50 4 -2 -11 -0.03 0.96 5 -2 11 42.19 5.13 5 2 -11 39.36 4.17 -5 -2 11 50.60 4.50 5 -2 -11 45.06 3.69 5 2 11 43.33 4.78 6 2 -11 7.03 2.83 6 -2 11 7.85 3.60 6 2 11 7.59 3.14 6 -2 -11 8.10 2.24 0 3 11 43.14 3.26 0 -3 11 46.52 4.28 0 3 -11 46.93 3.96 0 -3 -11 48.03 3.04 -1 3 11 19.08 2.97 1 -3 11 20.82 3.08 1 3 -11 25.34 2.66 -1 3 -11 22.00 2.82 1 -3 -11 23.78 1.70 1 3 11 25.04 2.12 -1 -3 11 23.82 3.49 -2 3 11 16.79 1.36 2 3 -11 16.59 2.40 2 -3 11 16.80 2.68 -2 -3 11 18.62 2.76 2 3 11 16.69 1.94 2 -3 -11 19.21 1.42 3 -3 11 1.03 1.70 3 3 -11 1.62 1.39 3 -3 -11 2.91 0.78 -3 -3 11 3.54 1.45 3 3 11 3.21 1.48 3 3 11 1.81 1.26 -3 3 -11 2.88 1.60 4 3 -11 6.16 1.68 4 -3 11 6.56 2.38 4 -3 -11 7.38 1.18 -4 -3 11 8.57 2.06 4 3 11 6.96 1.86 5 -3 11 17.19 3.35 5 3 -11 18.61 2.61 -5 -3 11 17.78 2.88 5 -3 -11 15.99 2.30 5 3 11 14.95 2.88 5 -3 -11 18.29 2.34 6 -3 11 5.06 3.52 0 4 11 14.60 1.63 0 4 -11 14.78 2.30 0 -4 11 17.48 2.82 -1 4 11 16.37 2.70 1 4 -11 20.94 2.60 1 -4 11 21.77 3.13 -1 4 -11 24.78 3.16 -1 -4 11 29.42 3.63 1 4 11 25.00 2.08 2 -4 11 2.48 1.76 2 4 -11 3.35 1.64 2 4 11 1.07 1.14 2 4 11 1.24 1.06 -2 4 -11 0.52 1.71 -2 -4 11 2.03 1.68 3 4 -11 6.63 1.66 3 -4 11 8.25 2.40 3 4 11 4.80 1.52 -3 -4 11 5.63 1.83 3 4 11 3.98 1.52 -3 4 -11 4.50 2.11 4 -4 11 5.73 2.60 -4 -4 11 11.81 2.42 4 4 11 11.06 2.26 4 -4 -11 11.10 1.29 4 -4 -11 10.20 1.30 5 -4 11 5.17 3.03 5 4 -11 6.41 2.21 5 4 11 5.79 2.42 -5 -4 11 5.03 2.65 5 -4 -11 5.64 1.19 5 -4 -11 4.39 1.18 0 5 -11 47.24 4.33 0 -5 11 47.17 4.71 0 5 11 47.13 3.03 0 5 11 43.88 3.21 1 -5 11 14.53 2.67 -1 5 11 14.35 2.11 2 5 -11 67.34 5.63 2 -5 11 68.39 6.14 2 5 11 82.07 5.21 2 5 11 76.68 5.94 -2 -5 11 90.31 6.18 -2 5 -11 93.56 6.69 3 5 -11 35.56 3.38 -3 5 -11 24.69 3.75 3 5 11 26.17 3.05 -3 -5 11 25.56 3.62 4 5 -11 36.97 4.11 4 -5 11 35.15 5.17 4 5 11 48.76 4.22 -4 -5 11 45.94 4.66 5 5 -11 16.92 3.11 5 -5 11 18.29 3.87 5 5 11 12.84 3.02 -5 -5 11 16.62 3.41 0 6 11 32.67 2.33 0 6 -11 33.69 3.83 0 6 11 32.24 2.42 0 -6 11 32.01 4.16 1 -6 11 3.39 2.17 -1 6 11 1.38 0.97 -1 6 11 2.07 0.43 1 6 -11 1.04 1.52 -1 -6 11 5.21 2.15 -1 6 -11 3.42 2.40 1 6 11 4.28 0.99 1 6 11 4.28 0.97 2 -6 11 17.03 3.11 2 6 -11 15.46 2.43 2 6 11 13.68 2.12 -2 -6 11 16.66 2.83 -2 6 -11 19.91 3.43 2 6 11 10.42 1.62 3 -6 11 0.97 2.37 3 6 -11 -0.61 1.48 3 6 11 0.36 1.34 3 6 11 -0.46 1.36 -3 -6 11 0.20 1.80 -3 6 -11 -0.81 2.57 4 -6 11 6.65 2.90 4 6 -11 9.23 2.21 4 6 11 6.54 2.20 -4 -6 11 7.04 2.54 4 6 11 5.12 2.13 5 -6 11 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4 -9 13 32.43 5.47 4 9 13 27.27 3.85 -4 -9 13 32.34 5.32 0 10 13 5.04 1.23 0 -10 13 2.52 2.73 0 10 -13 -1.52 2.49 0 10 13 4.57 1.33 1 10 -13 1.53 3.99 1 -10 13 4.07 3.01 -1 -10 13 -0.28 2.76 1 10 13 6.17 1.58 -1 10 -13 -1.80 3.22 1 10 13 5.85 1.71 2 -10 13 36.25 5.97 -2 -10 13 39.22 6.09 2 10 13 41.99 4.04 -2 10 -13 50.90 8.18 2 10 13 46.01 4.41 3 -10 13 2.66 3.84 -3 -10 13 3.00 3.44 3 10 13 1.81 2.18 3 10 13 3.09 2.81 0 11 -13 -2.54 3.44 0 11 13 2.38 1.20 0 11 13 0.59 1.48 0 -11 13 0.95 2.96 1 -11 13 25.94 4.18 1 11 13 32.27 3.73 -1 -11 13 36.60 5.18 1 11 13 24.98 3.21 -1 11 -13 47.37 7.23 2 -11 13 -0.82 3.26 2 11 13 -2.52 1.77 -2 -11 13 0.08 3.39 3 -11 13 10.40 4.27 3 11 13 17.38 3.00 -3 -11 13 11.73 4.88 0 12 13 24.80 3.50 0 12 13 24.09 2.91 0 -12 13 30.28 4.62 1 -12 13 3.31 3.34 1 12 13 -0.30 1.69 -1 -12 13 1.50 3.18 1 12 13 4.99 2.30 2 -12 13 7.87 3.80 2 12 13 2.91 2.35 -2 -12 13 4.03 5.25 2 12 13 2.78 2.58 0 -13 13 30.59 4.85 0 13 13 31.18 3.25 1 -13 13 65.22 6.69 1 13 13 37.75 5.38 1 13 13 50.58 5.25 -1 -13 13 44.69 5.76 0 0 14 488.64 28.31 0 0 -14 475.93 27.88 1 0 -14 0.64 1.09 -1 0 -14 1.72 1.20 1 0 14 2.74 1.47 -1 0 14 0.11 2.14 2 0 -14 279.38 16.44 -2 0 -14 271.70 16.60 -2 0 14 272.86 16.85 2 0 14 289.65 16.78 3 0 14 -0.34 1.65 -3 0 14 0.11 1.25 3 0 -14 0.31 1.23 -4 0 14 128.28 8.21 4 0 -14 127.36 8.30 4 0 14 127.89 8.87 5 0 -14 3.38 2.04 -5 0 14 5.68 2.02 5 0 14 1.36 2.69 0 1 -14 1.12 1.22 0 -1 -14 1.11 0.93 0 1 14 3.13 1.63 0 -1 14 0.62 1.85 1 1 -14 5.21 1.47 1 -1 14 3.49 1.61 -1 -1 -14 4.91 1.33 -1 1 14 3.98 2.33 1 -1 -14 5.35 1.18 1 1 14 4.41 1.45 -1 1 -14 2.16 1.44 -1 -1 14 2.89 2.34 -2 1 14 19.87 3.08 2 -1 14 24.97 3.43 2 1 -14 25.89 2.98 -2 -1 -14 26.48 2.95 -2 -1 14 35.61 3.97 2 -1 -14 31.79 2.68 -2 1 -14 34.40 3.29 2 1 14 32.31 3.06 -3 1 14 1.33 1.10 3 -1 14 -0.40 1.82 3 1 -14 -0.42 1.36 3 1 14 0.16 1.53 3 -1 -14 1.52 1.17 -3 -1 14 0.73 1.48 4 -1 14 5.88 2.32 -4 1 14 5.83 1.43 4 1 -14 4.83 1.79 4 1 14 2.87 2.05 4 -1 -14 1.94 1.44 -4 -1 14 4.41 1.78 5 -1 14 0.41 2.67 5 1 -14 1.22 2.14 5 1 14 1.68 2.69 5 -1 -14 2.43 1.86 -5 -1 14 0.75 2.25 0 2 -14 2.91 1.50 0 2 14 4.14 1.54 0 -2 -14 3.77 0.99 0 -2 14 5.44 2.29 -1 -2 -14 60.91 4.35 1 2 -14 60.76 4.77 1 -2 14 61.25 5.06 -1 2 14 52.77 5.52 1 2 14 64.86 4.58 1 -2 -14 66.27 4.16 -1 2 -14 57.66 5.72 -1 -2 14 70.37 6.16 -2 2 14 6.34 1.38 2 2 -14 3.58 1.55 2 -2 14 4.10 2.01 2 2 14 5.83 1.56 2 -2 -14 3.10 0.98 -2 2 -14 4.55 1.79 -2 -2 14 5.98 2.34 -3 2 14 12.94 1.72 3 -2 14 9.52 2.37 3 2 -14 10.52 2.04 -3 -2 14 18.34 2.61 3 2 14 17.28 2.40 4 2 -14 6.82 2.12 -4 2 14 8.22 1.37 4 -2 14 8.85 2.62 -4 -2 14 8.47 2.26 4 2 14 10.90 2.46 4 -2 -14 9.61 1.62 5 2 -14 2.48 3.78 5 -2 14 4.70 3.15 5 -2 -14 4.31 2.95 5 2 14 9.49 2.76 -5 -2 14 10.43 2.80 0 3 14 10.64 1.80 0 -3 -14 12.12 1.59 0 -3 14 10.75 2.79 1 -3 14 65.04 5.67 1 3 -14 63.51 5.23 -1 3 14 63.04 5.57 -1 -3 14 78.71 6.53 -1 3 -14 75.70 5.50 1 3 14 63.62 4.74 1 -3 -14 68.55 4.30 2 3 -14 23.82 3.39 2 -3 14 23.80 3.41 -2 3 14 25.84 2.14 -2 -3 14 19.36 3.41 2 3 14 16.27 2.60 -2 3 -14 23.24 3.48 2 -3 -14 22.68 1.83 3 -3 14 17.15 3.18 -3 3 14 20.70 1.82 3 3 -14 21.38 3.22 3 -3 -14 27.32 2.01 -3 -3 14 21.52 3.16 3 3 14 23.20 3.10 4 -3 14 8.03 2.69 4 3 -14 6.46 2.21 -4 -3 14 7.73 2.61 4 3 14 4.53 2.14 4 -3 -14 4.21 1.14 4 3 14 5.19 2.11 5 3 -14 15.51 3.07 5 -3 14 18.07 3.69 -5 -3 14 13.80 3.27 5 3 14 21.15 3.46 5 -3 -14 19.32 3.33 5 -3 -14 17.37 2.28 0 -4 14 214.83 13.81 0 4 14 212.21 12.76 0 4 -14 212.88 13.35 1 4 -14 7.67 2.08 -1 4 14 8.17 2.11 1 -4 14 8.77 2.48 1 4 14 5.88 1.38 -1 4 -14 6.72 2.21 -1 -4 14 3.83 2.77 2 4 -14 156.12 10.36 2 -4 14 141.16 11.17 -2 4 14 148.98 9.35 2 4 14 178.12 10.11 -2 4 -14 182.30 11.05 -2 -4 14 171.77 11.26 3 -4 14 3.63 2.37 3 4 -14 8.63 2.16 -3 -4 14 3.29 2.90 -3 4 -14 5.82 2.92 3 4 14 4.99 1.88 3 4 14 5.83 1.85 4 -4 14 41.75 5.94 4 4 -14 45.60 5.04 -4 -4 14 66.55 6.01 -4 4 -14 43.43 7.42 4 4 14 66.02 5.46 4 4 14 68.49 5.29 5 -4 14 9.68 3.55 -5 -4 14 9.69 3.63 5 4 14 19.57 3.46 0 5 -14 71.71 5.60 0 -5 14 70.28 6.45 0 5 14 64.69 4.66 1 5 -14 8.41 2.17 -1 5 14 12.65 2.10 1 -5 14 12.18 2.95 1 5 14 7.98 1.50 1 5 14 8.64 1.51 -1 -5 14 11.66 3.23 -1 5 -14 8.31 2.38 2 -5 14 65.27 5.88 2 5 -14 60.68 5.18 -2 5 -14 64.98 6.13 2 5 14 61.01 4.62 -2 -5 14 54.05 6.26 2 5 14 58.97 4.56 3 -5 14 1.70 2.62 3 5 -14 3.52 2.00 -3 -5 14 2.67 2.77 3 5 14 6.01 1.91 3 5 14 5.11 1.73 4 5 -14 8.36 2.41 4 -5 14 11.22 3.46 -4 -5 14 5.90 3.11 -4 5 -14 10.31 3.70 4 5 14 11.92 2.60 5 -5 14 21.24 4.24 5 5 14 12.62 3.15 -5 -5 14 17.35 4.13 0 6 14 3.55 0.93 0 6 -14 1.56 2.09 0 6 14 3.26 1.14 0 -6 14 1.32 2.42 -1 6 14 246.41 14.16 1 6 -14 242.40 15.30 -1 6 14 258.59 14.71 -1 -6 14 203.27 18.65 1 6 14 249.03 14.65 1 6 14 244.63 14.66 -1 6 -14 277.14 16.60 2 -6 14 4.23 2.48 2 6 -14 2.47 1.93 -2 6 -14 3.63 2.77 2 6 14 3.40 1.51 2 6 14 3.53 1.51 -2 -6 14 3.50 2.85 3 6 -14 87.15 7.07 3 -6 14 94.62 8.00 -3 -6 14 101.93 8.21 3 6 14 98.58 6.73 4 6 -14 12.85 3.21 4 -6 14 14.22 3.84 -4 6 -14 10.00 4.23 -4 -6 14 24.88 4.43 4 6 14 20.17 2.99 5 -6 14 53.88 7.69 5 6 14 56.47 6.37 -5 -6 14 68.15 7.98 0 7 14 0.20 0.97 0 7 14 0.42 0.79 0 -7 14 2.07 2.46 -1 7 14 50.39 3.66 1 7 -14 43.21 4.78 1 -7 14 45.79 5.70 -1 7 14 46.46 2.92 1 7 14 48.56 3.65 -1 -7 14 54.17 5.84 1 7 14 42.90 3.65 2 7 -14 0.29 1.98 2 -7 14 1.03 2.84 2 7 14 0.10 1.36 2 7 14 2.89 1.47 -2 -7 14 -0.40 2.76 3 7 -14 20.61 3.34 3 -7 14 21.47 3.89 -3 -7 14 27.40 4.29 3 7 14 25.82 3.47 4 -7 14 0.92 3.58 -4 -7 14 8.00 3.99 4 7 14 7.56 2.72 0 8 14 21.60 2.31 0 8 14 21.24 2.13 0 -8 14 20.69 3.68 1 -8 14 10.52 3.17 1 8 14 5.80 1.42 -1 -8 14 6.91 2.96 1 8 14 4.46 2.25 2 8 -14 12.86 2.70 2 -8 14 10.58 3.64 2 8 14 8.70 2.01 -2 -8 14 5.78 3.23 -2 8 -14 8.59 4.13 3 -8 14 7.12 3.66 3 8 -14 5.78 2.91 3 8 14 7.10 2.14 -3 -8 14 10.05 3.61 -3 8 -14 9.33 5.05 4 -8 14 -0.87 3.73 4 8 14 -0.49 2.59 -4 -8 14 3.97 4.22 0 9 14 8.41 1.37 0 9 14 6.56 1.39 0 -9 14 10.74 3.33 1 -9 14 5.00 3.21 -1 9 -14 4.39 3.20 -1 -9 14 6.89 3.04 1 9 14 5.16 1.44 1 9 14 4.99 1.60 2 -9 14 9.10 3.53 2 9 -14 4.45 2.69 2 9 14 11.00 2.18 2 9 14 9.72 2.00 -2 -9 14 10.71 3.58 -2 9 -14 10.04 3.87 3 -9 14 10.35 3.65 3 9 14 4.20 2.17 3 9 14 6.64 2.54 -3 -9 14 3.87 3.84 4 -9 14 18.08 4.71 -4 -9 14 13.23 4.72 4 9 14 14.82 3.14 0 10 14 1.22 1.26 0 -10 14 -1.62 2.60 0 10 -14 0.24 3.05 0 10 14 0.25 1.13 1 -10 14 162.57 11.39 -1 -10 14 166.28 11.62 1 10 14 161.73 9.94 -1 10 -14 152.71 11.99 1 10 14 158.88 10.04 2 -10 14 6.12 3.61 2 10 14 1.35 2.30 -2 10 -14 -2.52 4.57 2 10 14 3.01 1.86 -2 -10 14 -2.66 3.40 3 -10 14 72.53 7.87 3 10 14 57.93 7.51 -3 -10 14 51.10 7.58 3 10 14 49.78 5.32 0 11 14 1.00 1.33 0 11 14 3.07 1.55 0 -11 14 2.00 2.94 1 -11 14 4.82 3.64 1 11 14 10.24 2.28 1 11 14 6.74 1.91 -1 -11 14 8.53 3.40 2 -11 14 -0.50 3.63 2 11 14 1.14 2.10 -2 -11 14 3.87 3.70 3 -11 14 2.99 4.20 3 11 14 3.69 2.66 -3 -11 14 7.48 4.51 0 12 14 23.47 3.07 0 12 14 24.88 3.47 0 -12 14 26.20 4.66 1 -12 14 3.43 3.11 1 12 14 -1.05 2.10 1 12 14 3.06 2.26 -1 -12 14 0.11 3.43 2 -12 14 24.66 4.76 -2 -12 14 26.52 4.95 2 12 14 19.88 3.32 2 12 14 19.20 3.10 0 -13 14 1.59 3.80 -1 -13 14 24.35 4.95 1 13 14 25.71 3.91 0 0 15 4.06 1.99 0 0 -15 3.05 1.26 1 0 15 157.82 10.09 1 0 -15 167.75 9.76 -1 0 -15 135.78 10.82 -1 0 15 162.93 10.99 -2 0 -15 7.12 1.85 2 0 15 8.54 2.03 2 0 -15 6.20 1.55 -2 0 15 4.09 2.11 3 0 15 227.14 13.94 -3 0 15 224.71 13.63 3 0 -15 223.33 13.59 4 0 15 2.49 2.28 -4 0 15 1.80 1.58 5 0 15 65.18 6.37 -5 0 15 60.16 5.38 5 0 -15 67.43 5.58 0 1 15 65.10 5.09 0 1 -15 62.67 4.69 0 -1 15 68.76 5.61 0 -1 -15 54.19 4.27 -1 -1 -15 37.04 3.16 1 -1 15 38.32 3.72 1 1 -15 35.73 3.41 -1 1 15 42.97 4.93 1 -1 -15 33.28 2.89 -1 1 -15 29.47 3.33 1 1 15 26.57 3.31 -2 1 15 21.73 3.05 2 1 15 10.52 2.06 -2 -1 15 10.08 2.74 2 -1 -15 15.20 2.14 -2 1 -15 14.90 2.28 -3 1 15 42.17 3.39 3 1 -15 38.80 3.77 3 -1 15 39.88 4.32 3 1 15 38.07 3.84 3 -1 -15 38.39 3.36 -3 -1 15 35.39 3.96 4 -1 15 34.68 4.54 -4 1 15 36.34 3.23 4 1 -15 38.92 3.92 4 1 15 37.00 4.39 -4 -1 15 29.87 3.82 4 -1 -15 28.72 3.44 5 1 -15 9.47 2.64 5 -1 15 13.77 3.17 5 -1 -15 9.09 2.47 -5 -1 15 12.88 3.14 5 1 15 8.95 3.01 0 2 -15 6.73 2.15 0 -2 -15 6.39 1.20 0 2 15 6.32 1.82 0 -2 15 9.91 2.58 1 2 -15 19.90 2.90 -1 -2 -15 16.20 2.26 1 -2 15 24.09 3.60 -1 2 15 21.08 3.17 1 -2 -15 17.03 1.96 -1 -2 15 18.29 3.50 -1 2 -15 20.04 3.04 1 2 15 18.38 2.66 2 2 -15 0.90 1.79 2 -2 15 0.80 1.88 -2 2 15 1.43 1.40 -2 2 -15 3.89 1.93 2 -2 -15 4.69 1.08 -2 -2 15 2.59 2.59 2 2 15 2.76 1.49 3 -2 15 51.12 4.91 3 2 -15 50.76 4.56 -3 2 15 53.25 3.75 3 -2 -15 53.17 3.84 -3 -2 15 54.54 5.05 3 2 15 54.83 4.74 4 -2 15 8.10 2.68 4 2 -15 10.09 2.32 -4 2 15 7.74 1.45 4 -2 -15 13.17 1.81 4 2 15 7.78 2.60 -4 -2 15 14.60 2.81 5 -2 15 12.74 3.38 5 2 -15 2.94 2.50 5 2 15 5.83 3.04 -5 -2 15 12.54 2.88 5 -2 -15 4.52 2.80 0 -3 15 45.12 4.93 0 3 15 33.93 3.58 0 -3 -15 38.68 2.96 0 3 -15 39.33 3.82 1 -3 15 17.99 2.98 -1 3 15 21.04 3.06 1 3 -15 18.19 2.63 -1 3 -15 23.73 3.14 1 3 15 18.71 2.62 1 -3 -15 19.16 1.96 -1 -3 15 18.30 3.50 2 3 -15 19.11 3.07 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5 15 31.95 3.03 1 5 -15 58.59 5.12 -1 5 15 57.13 4.76 -1 5 -15 58.90 5.50 -1 -5 15 50.46 5.97 1 5 15 54.91 4.26 2 -5 15 19.17 3.42 2 5 -15 15.79 2.68 2 5 15 20.86 2.80 2 5 15 17.88 2.80 -2 -5 15 20.55 5.08 3 5 -15 23.50 3.24 3 -5 15 19.96 3.59 3 5 15 23.06 3.38 -3 -5 15 24.64 4.33 4 5 -15 15.57 3.09 4 -5 15 13.98 3.49 -4 -5 15 8.10 3.83 4 5 15 10.60 2.80 5 -5 15 23.31 4.91 -5 -5 15 31.40 5.28 5 5 15 30.48 4.35 0 6 15 66.23 4.37 0 6 15 63.25 4.67 0 -6 15 67.28 6.56 0 6 -15 71.46 6.00 1 6 -15 28.15 4.38 -1 6 15 33.90 2.19 1 -6 15 30.81 4.63 -1 6 15 35.84 3.48 1 6 15 32.03 2.99 1 6 15 28.72 3.04 -1 -6 15 29.44 4.44 2 -6 15 100.25 7.83 2 6 -15 94.67 7.37 -2 -6 15 96.93 8.56 2 6 15 100.78 6.71 2 6 15 97.56 6.74 3 -6 15 2.33 2.90 3 6 -15 1.46 2.14 -3 6 -15 2.78 2.96 3 6 15 0.92 1.92 -3 -6 15 -3.47 3.28 4 -6 15 97.43 8.74 4 6 -15 99.77 7.95 4 6 15 95.15 7.26 -4 -6 15 87.19 9.01 0 7 15 1.65 1.18 0 -7 15 2.17 2.62 0 7 15 -0.31 0.81 -1 7 15 18.18 2.68 1 7 -15 18.05 3.02 -1 7 15 19.90 1.55 1 -7 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21 37.82 5.89 -2 3 21 28.68 3.71 2 3 -21 39.55 4.94 -2 -3 21 31.52 6.34 2 3 21 34.24 5.11 -2 3 -21 38.79 5.46 2 -3 -21 37.89 4.02 3 -3 21 38.10 6.02 3 3 -21 30.79 5.06 -3 3 21 30.56 3.19 3 -3 -21 33.57 3.09 3 3 21 29.46 4.43 -3 -3 21 22.29 5.94 4 3 -21 10.97 5.38 -4 -3 21 11.08 5.22 4 3 21 3.46 3.47 0 -4 21 2.42 3.50 0 4 21 0.14 2.26 0 4 -21 -0.02 2.39 1 -4 21 135.97 10.33 -1 4 21 134.09 9.48 1 4 -21 121.22 9.34 -1 4 -21 122.26 9.49 1 4 21 123.69 9.23 -1 -4 21 147.54 11.51 2 -4 21 1.75 3.38 -2 4 21 0.02 1.77 2 4 -21 8.75 2.96 -2 -4 21 2.04 5.06 2 4 21 3.53 2.69 -3 4 21 61.02 4.14 3 -4 21 74.72 7.30 3 4 -21 68.13 7.22 -3 -4 21 52.09 8.18 3 4 21 78.77 7.01 0 -5 21 14.03 3.98 0 5 21 14.40 2.80 0 5 -21 11.93 3.45 1 5 -21 43.34 5.46 -1 5 21 33.85 4.80 1 -5 21 44.84 6.53 1 5 21 36.01 5.02 -1 5 -21 32.42 5.13 -1 -5 21 44.53 6.38 2 5 -21 -2.46 3.16 2 -5 21 -1.71 3.47 -2 5 21 0.58 1.10 -2 -5 21 5.79 5.52 2 5 21 -0.98 2.60 3 -5 21 1.17 3.64 3 5 21 0.93 3.07 -3 -5 21 1.08 5.95 0 6 21 54.53 5.44 0 -6 21 64.89 7.61 0 6 21 56.07 4.71 -1 6 21 39.59 4.43 1 6 -21 33.61 6.82 1 -6 21 27.54 4.87 -1 6 21 29.63 2.85 1 6 21 32.69 4.79 -1 -6 21 36.16 6.15 1 6 21 34.66 4.28 2 -6 21 47.95 6.04 -2 -6 21 42.19 7.55 2 6 21 34.39 4.48 3 -6 21 20.74 4.98 3 6 21 16.88 3.80 -3 -6 21 12.49 6.81 0 -7 21 44.79 7.20 0 7 21 42.50 4.91 1 -7 21 60.25 7.23 -1 7 21 45.46 3.61 -1 7 21 42.08 4.28 1 7 21 50.95 5.89 -1 -7 21 66.58 8.43 1 7 21 45.79 5.56 2 -7 21 11.28 4.37 -2 -7 21 8.29 5.92 2 7 21 7.89 3.22 2 7 21 8.21 3.03 0 8 21 12.59 2.76 0 -8 21 8.50 4.27 0 8 21 9.51 1.99 1 -8 21 19.20 4.76 1 8 21 14.03 2.77 1 8 21 22.33 3.36 -1 -8 21 11.01 5.28 2 -8 21 7.81 4.49 2 8 21 7.60 3.02 2 8 21 5.44 3.28 -2 -8 21 3.51 5.64 0 -9 21 3.92 4.49 0 9 21 1.47 2.41 1 -9 21 41.43 6.19 1 9 21 36.15 5.49 1 9 21 36.90 4.49 -1 -9 21 33.53 6.46 0 0 -22 9.36 2.39 0 0 22 12.66 3.69 -1 0 -22 9.43 2.37 1 0 -22 9.59 2.27 1 0 22 10.33 3.31 -2 0 22 -8.83 3.70 2 0 -22 1.21 2.04 -2 0 -22 2.10 2.65 2 0 22 -0.94 2.80 -3 0 22 2.38 3.60 3 0 22 12.93 4.00 3 0 -22 12.66 2.61 0 -1 -22 73.58 5.89 0 1 -22 78.73 6.23 0 1 22 81.36 7.48 0 -1 22 84.90 7.77 -1 1 22 15.84 4.13 -1 -1 -22 18.02 2.86 1 1 -22 15.73 3.24 1 -1 22 13.45 3.48 1 1 22 14.58 3.34 -1 -1 22 26.80 4.91 -1 1 -22 16.87 2.74 1 -1 -22 21.61 3.17 -2 -1 -22 42.09 5.09 2 1 -22 49.59 5.53 2 -1 22 48.37 6.26 -2 1 22 32.35 5.34 -2 -1 22 38.11 6.45 -2 1 -22 46.46 5.51 2 -1 -22 47.64 4.27 2 1 22 45.19 6.08 3 -1 22 58.40 6.62 3 1 -22 46.48 5.21 -3 1 22 41.50 5.58 -3 -1 22 37.40 5.85 3 1 22 50.73 6.50 3 -1 -22 47.95 4.61 0 2 22 100.16 9.03 0 2 -22 98.41 7.26 0 -2 22 100.50 8.71 0 -2 -22 82.15 6.56 -1 2 22 38.73 5.91 1 -2 22 36.89 5.86 -1 -2 -22 34.39 4.25 1 2 -22 30.18 4.41 1 2 22 33.83 5.22 -1 -2 22 36.19 5.60 1 -2 -22 30.92 3.54 -1 2 -22 33.82 4.58 2 2 -22 65.25 5.73 2 -2 22 65.93 7.00 -2 2 22 49.56 6.32 -2 -2 22 45.42 7.02 2 2 22 51.77 6.29 -3 2 22 5.97 2.38 3 -2 22 13.52 4.01 3 2 -22 7.78 3.05 -3 -2 22 0.90 4.80 3 2 22 4.23 3.34 3 -2 -22 12.04 2.32 0 -3 -22 41.66 4.25 0 -3 22 49.16 6.10 0 3 -22 47.98 5.12 0 3 22 41.68 5.56 1 3 -22 58.39 5.50 -1 3 22 50.03 6.13 1 -3 22 41.49 6.05 -1 3 -22 50.92 5.88 1 -3 -22 50.09 4.31 -1 -3 22 55.73 8.01 1 3 22 47.16 5.72 -2 3 22 43.14 5.43 2 -3 22 60.12 6.78 2 3 -22 59.45 5.73 2 -3 -22 55.75 4.17 2 3 22 51.17 6.21 -2 -3 22 46.22 7.51 3 3 -22 58.35 6.69 -3 3 22 60.60 4.57 3 -3 22 66.49 7.59 -3 -3 22 38.05 7.67 0 -4 22 3.13 3.67 0 4 -22 10.01 2.98 0 4 22 2.17 2.63 1 -4 22 41.54 6.46 1 4 -22 35.36 5.00 -1 4 22 43.78 5.32 1 4 22 31.49 5.16 -1 -4 22 31.49 5.84 -1 4 -22 28.16 4.58 2 4 -22 8.01 3.31 2 -4 22 4.20 3.46 -2 4 22 2.09 2.02 -2 -4 22 2.87 5.40 2 4 22 -1.85 2.79 3 -4 22 16.86 4.53 3 4 -22 9.32 4.32 3 4 22 14.10 3.82 -3 -4 22 -2.48 6.35 0 5 -22 18.27 4.55 0 5 22 19.37 3.27 0 -5 22 19.11 4.65 1 5 -22 24.44 4.22 -1 5 22 28.72 4.55 1 -5 22 18.62 4.57 -1 -5 22 20.90 5.41 1 5 22 22.35 3.65 2 -5 22 4.00 3.72 -2 5 22 3.83 1.42 2 5 22 6.76 3.21 -2 -5 22 2.97 6.03 3 -5 22 1.47 4.06 -3 -5 22 -1.72 6.39 3 5 22 -2.14 3.22 0 6 22 -0.38 1.80 0 6 22 2.02 2.42 0 -6 22 -0.20 3.74 -1 6 22 14.82 2.28 1 -6 22 18.30 4.43 -1 6 22 11.88 2.86 1 6 22 10.35 3.19 1 6 22 8.65 3.87 -1 -6 22 16.15 5.62 2 -6 22 3.27 4.03 2 6 22 8.57 3.28 2 6 22 5.67 3.27 -2 -6 22 6.39 6.22 0 7 22 39.19 4.92 0 7 22 30.65 4.63 0 -7 22 38.91 5.72 1 -7 22 2.77 4.35 -1 7 22 9.67 2.31 -1 -7 22 7.77 4.77 1 7 22 9.07 2.72 1 7 22 18.64 3.42 2 -7 22 63.58 8.42 2 7 22 64.20 6.83 2 7 22 58.25 7.03 -2 -7 22 70.12 10.99 0 8 22 4.17 2.64 0 -8 22 2.22 4.63 1 -8 22 56.91 8.24 1 8 22 60.67 5.71 1 8 22 71.59 6.52 -1 -8 22 60.19 9.29 0 0 23 4.83 3.33 0 0 -23 1.27 1.99 1 0 23 2.45 3.27 -1 0 23 1.70 3.75 -1 0 -23 1.95 2.18 1 0 -23 1.35 3.23 2 0 -23 2.51 2.14 -2 0 23 -5.35 4.36 2 0 23 -2.53 3.27 3 0 23 4.82 3.99 3 0 -23 12.88 2.83 -3 0 23 5.94 3.94 0 1 23 22.69 4.18 0 -1 -23 14.70 2.62 0 1 -23 16.34 2.85 0 -1 23 18.28 4.18 1 -1 23 26.58 4.46 1 1 -23 21.21 3.09 -1 -1 -23 22.80 3.29 -1 -1 23 27.84 5.13 1 1 23 29.38 4.38 1 -1 -23 29.95 3.71 -1 1 -23 27.75 4.35 -2 -1 -23 -0.60 3.26 2 1 -23 5.02 2.64 -2 1 23 -2.25 3.59 2 -1 23 2.63 3.55 2 -1 -23 2.53 1.90 -2 -1 23 0.28 4.69 2 1 23 7.64 3.40 3 1 -23 29.87 4.77 -3 1 23 16.10 3.76 3 -1 23 21.10 4.50 -3 -1 23 17.29 4.99 3 1 23 23.24 4.75 0 -2 23 32.40 5.06 0 -2 -23 30.41 4.11 0 2 -23 32.65 3.96 0 2 23 29.71 4.38 1 2 -23 26.32 3.61 -1 2 23 29.80 4.65 1 -2 23 25.76 4.49 -1 -2 -23 24.24 3.43 1 2 23 22.87 4.13 1 -2 -23 28.01 3.46 -1 -2 23 35.04 5.48 -1 2 -23 25.28 3.81 2 2 -23 11.52 2.95 -2 2 23 6.80 3.62 2 -2 23 15.29 3.86 2 2 23 14.09 3.90 2 -2 -23 18.09 2.30 -2 -2 23 13.41 5.71 3 2 -23 48.33 6.53 3 -2 23 45.39 6.94 -3 2 23 27.83 4.59 -3 -2 23 24.23 6.28 3 2 23 38.85 5.38 0 3 -23 33.79 4.81 0 -3 -23 19.73 2.88 0 -3 23 29.12 5.11 -1 3 23 4.83 3.30 1 3 -23 5.02 2.83 1 -3 23 6.28 3.99 -1 -3 23 10.61 4.65 1 -3 -23 8.28 1.92 1 3 23 7.31 3.24 2 -3 23 9.94 3.85 2 3 -23 10.90 3.28 -2 3 23 2.39 2.78 -2 -3 23 8.96 5.59 2 3 23 9.51 3.56 3 3 -23 7.61 3.70 3 -3 23 3.35 4.25 3 3 23 0.55 3.75 -3 -3 23 -2.69 6.08 0 4 23 34.99 5.63 0 4 -23 57.22 6.95 0 -4 23 46.55 7.31 1 4 -23 22.85 3.91 1 -4 23 9.45 4.00 -1 4 23 10.54 3.43 1 4 23 11.55 3.34 -1 -4 23 13.60 5.15 2 -4 23 57.95 7.62 2 4 -23 56.59 6.82 -2 4 23 39.29 5.42 -2 -4 23 76.17 10.55 2 4 23 56.86 6.69 3 4 23 22.61 4.35 -3 -4 23 9.81 7.34 0 5 23 26.98 3.94 0 -5 23 31.64 5.44 -1 5 23 34.72 5.27 1 -5 23 46.94 7.08 -1 -5 23 41.67 6.81 1 5 23 35.44 4.67 2 -5 23 34.99 5.57 2 5 23 42.44 5.25 -2 -5 23 36.83 7.68 0 6 23 17.27 3.48 0 -6 23 26.49 5.36 0 6 23 18.43 2.69 -1 6 23 26.17 3.60 1 -6 23 20.41 4.89 1 6 23 18.43 3.76 -1 -6 23 23.53 5.75 2 -6 23 21.39 4.95 -2 -6 23 28.40 7.62 2 6 23 35.44 5.34 2 6 23 27.68 4.64 0 7 23 16.03 3.28 0 -7 23 26.24 5.19 0 7 23 13.23 2.72 1 -7 23 13.67 4.95 1 7 23 17.50 3.78 -1 -7 23 20.48 5.93 0 8 23 18.85 3.96 0 -8 23 24.87 6.09 0 0 24 14.26 4.07 0 0 -24 14.96 2.70 -1 0 -24 -0.75 2.67 1 0 24 0.98 3.55 1 0 -24 -1.31 2.04 -1 0 24 1.88 4.06 2 0 -24 2.93 2.29 2 0 24 3.49 3.84 -2 0 24 -7.93 4.16 -3 0 24 2.26 4.01 3 0 24 10.13 4.14 0 -1 -24 26.31 4.08 0 1 24 32.23 4.86 0 1 -24 26.71 3.57 0 -1 24 36.52 5.37 1 -1 24 83.83 8.88 1 1 -24 88.67 7.35 -1 -1 -24 91.32 7.46 -1 1 24 124.42 9.51 1 1 24 100.92 8.64 -1 1 -24 95.69 7.84 1 -1 -24 97.83 7.09 -1 -1 24 105.50 9.88 2 1 -24 21.83 3.40 2 -1 24 29.85 4.97 2 -1 -24 17.98 2.78 2 1 24 23.70 4.52 -2 -1 24 12.62 5.58 3 1 -24 24.31 4.32 -3 1 24 21.77 4.27 3 -1 24 17.08 4.88 3 1 24 22.25 4.77 -3 -1 24 24.78 5.71 0 2 -24 14.90 3.30 0 -2 24 11.38 4.13 0 -2 -24 11.42 2.54 0 2 24 6.72 3.55 1 -2 24 4.59 4.04 1 2 -24 5.83 2.71 -1 -2 -24 7.35 2.70 1 -2 -24 4.51 2.05 -1 -2 24 10.86 4.63 1 2 24 9.83 3.51 2 2 -24 4.65 2.91 -2 2 24 1.68 3.56 2 -2 24 -2.37 3.32 -2 -2 24 2.83 5.62 2 2 24 2.24 3.65 2 -2 -24 4.42 2.10 0 3 -24 0.80 4.99 0 3 24 1.49 3.12 0 -3 24 1.82 3.95 0 -3 -24 -0.66 2.12 1 3 -24 9.21 3.39 -1 3 24 18.84 4.00 1 -3 24 10.15 4.23 1 -3 -24 13.15 2.80 1 3 24 10.49 3.57 -1 -3 24 17.66 5.31 -2 3 24 5.95 3.04 2 -3 24 10.00 4.22 2 3 -24 8.47 3.49 2 3 24 5.54 3.88 -2 -3 24 10.71 6.32 0 4 24 13.06 3.73 0 -4 24 22.18 5.24 1 -4 24 26.88 4.99 -1 4 24 37.05 5.69 1 4 24 21.05 4.27 -1 -4 24 21.87 5.70 2 -4 24 0.10 3.91 -2 4 24 0.32 2.19 -2 -4 24 12.80 6.35 2 4 24 1.34 3.55 0 -5 24 19.77 5.20 -1 5 24 39.98 5.44 1 -5 24 43.98 6.18 1 5 24 33.16 6.73 -1 -5 24 31.79 6.49 2 -5 24 5.03 4.77 -2 -5 24 20.15 6.76 2 5 24 13.36 4.33 0 6 24 9.68 2.48 0 6 24 9.23 3.42 0 -6 24 6.61 4.78 1 -6 24 -1.62 4.02 -1 6 24 -3.34 3.04 1 6 24 2.73 3.45 1 6 24 -2.71 3.00 -1 -6 24 -0.29 5.45 0 7 24 46.96 6.33 0 -7 24 63.00 8.57 0 0 -25 -1.41 2.47 0 0 25 -1.76 3.74 1 0 -25 95.51 7.30 -1 0 25 108.13 9.85 1 0 25 79.19 12.44 2 0 -25 -2.02 2.43 -2 0 25 -1.23 4.80 2 0 25 -4.66 3.78 0 1 25 15.28 4.22 0 -1 25 14.15 4.23 0 -1 -25 6.72 2.62 0 1 -25 11.07 3.74 1 1 -25 38.29 4.92 1 -1 25 35.46 5.42 -1 -1 -25 36.38 5.78 -1 1 25 42.00 5.71 1 -1 -25 36.59 4.29 -1 -1 25 25.83 5.60 1 1 25 32.38 5.01 -2 1 25 29.28 5.59 2 1 -25 31.16 4.70 2 -1 25 29.27 5.42 2 1 25 33.89 5.30 -2 -1 25 28.62 6.53 2 -1 -25 32.26 5.19 0 2 25 27.14 4.64 0 -2 25 25.55 5.91 0 -2 -25 23.93 3.30 1 -2 25 -1.20 3.99 -1 -2 -25 -4.93 2.92 -1 2 25 -4.55 3.61 1 2 -25 7.62 4.34 1 -2 -25 2.97 2.93 -1 -2 25 0.75 4.58 1 2 25 3.32 3.46 2 -2 25 14.61 4.42 -2 2 25 10.93 4.07 2 2 -25 9.80 3.60 2 2 25 12.59 4.28 -2 -2 25 17.13 6.19 0 3 25 2.36 3.55 0 -3 25 7.12 4.23 1 -3 25 5.02 4.27 1 -3 -25 0.77 2.24 1 3 25 7.39 3.72 -1 -3 25 14.78 5.21 -2 3 25 -1.26 3.02 2 -3 25 -4.66 4.05 2 3 25 4.19 3.84 -2 -3 25 2.11 6.14 0 -4 25 1.03 4.50 0 4 25 1.48 3.38 -1 4 25 39.46 6.34 1 -4 25 42.67 6.15 -1 -4 25 50.27 7.16 1 4 25 36.67 5.33 0 -5 25 39.13 6.36 0 5 25 39.23 6.21 1 -5 25 22.84 5.69 -1 5 25 32.41 5.29 1 5 25 41.66 6.60 -1 -5 25 33.19 6.63 0 0 -26 45.29 5.46 0 0 26 45.47 6.04 1 0 -26 2.45 2.64 -1 0 26 0.00 4.40 1 0 26 5.01 4.18 0 1 26 52.43 7.79 0 -1 -26 47.25 7.41 0 -1 26 71.52 8.19 1 1 -26 5.03 2.92 1 -1 26 2.26 4.07 -1 1 26 -0.03 4.10 1 1 26 -0.10 3.75 -1 -1 26 -1.47 4.63 1 -1 -26 5.98 2.46 0 -2 -26 11.47 3.06 0 -2 26 16.84 4.81 0 2 26 19.14 4.60 1 -2 26 2.69 4.16 -1 2 26 4.18 4.08 1 -2 -26 2.81 2.69 -1 -2 26 3.45 4.91 1 2 26 8.84 4.20 0 3 26 99.99 9.03 0 -3 26 90.51 9.76 1 -3 26 2.23 4.28 -1 3 26 2.34 3.90 1 3 26 2.03 3.82 -1 -3 26 4.21 5.28 0 -4 26 8.80 4.72 0 4 26 7.10 3.94 0 0 27 -1.41 4.20 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 47492 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' 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 0.48901(13) 0.28108(5) 0.57551(3) 0.0137(3) Uani 1 1 d . . . . . Pb2 Pb 0.50298(15) 0.47022(4) 0.77888(3) 0.0148(3) Uani 1 1 d . . . . . Se1 Se 0.5140(4) -0.00917(11) 0.49094(6) 0.0084(4) Uani 1 1 d . . . . . Se2 Se 0.1380(3) 0.22597(12) 0.71372(7) 0.0055(4) Uani 1 1 d . . . . . Se3 Se -0.0497(2) 0.31847(11) 0.88505(7) 0.0057(4) Uani 1 1 d . . . . . V1 V 0.5179(5) 0.02285(19) 0.33999(11) 0.0081(6) Uani 1 1 d . . . . . V2 V 0.4655(5) 0.17224(19) 0.85375(12) 0.0065(6) Uani 1 1 d . . . . . V3 V 0.9466(5) 0.08606(19) 0.58879(12) 0.0069(7) Uani 1 1 d . . . . . F1 F 1.015(2) 0.5094(7) 0.7486(4) 0.018(2) Uani 1 1 d . . . . . O1 O 0.3729(19) -0.0975(8) 0.3613(5) 0.006(2) Uani 1 1 d . U . . . O2 O 0.631(2) 0.0632(9) 0.4256(5) 0.012(3) Uani 1 1 d . . . . . O3 O 0.2636(18) 0.3524(8) 0.6915(5) 0.005(2) Uani 1 1 d . U . . . O4 O 0.779(2) 0.3907(9) 0.6625(6) 0.013(3) Uani 1 1 d . . . . . O5 O 0.3735(19) 0.5540(8) 0.6659(5) 0.008(2) Uani 1 1 d . . . . . O6 O 0.3859(19) 0.1729(8) 0.7534(5) 0.007(2) Uani 1 1 d . U . . . O7 O 0.7349(17) 0.2757(9) 0.8281(5) 0.004(2) Uani 1 1 d . U . . . O8 O 0.511(3) 0.1857(8) 0.9289(4) 0.019(2) Uani 1 1 d . . . . . O9 O 0.2240(19) 0.3180(9) 0.8424(5) 0.008(2) Uani 1 1 d . . . . . O10 O 0.7147(19) 0.1008(9) 0.6395(5) 0.009(2) Uani 1 1 d . U . . . O11 O 0.898(2) 0.1938(9) 0.5387(5) 0.012(2) Uani 1 1 d . . . . . O12 O 0.1961(19) 0.1613(8) 0.6423(5) 0.009(2) Uani 1 1 d . U . . . O13 O 0.787(2) -0.0227(9) 0.5344(6) 0.014(3) Uani 1 1 d . U . . . O14 O 0.862(2) 0.4529(9) 0.8818(5) 0.013(2) Uani 1 1 d . U . . . O15 O 0.347(2) 0.0931(9) 0.5245(5) 0.014(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 0.0125(4) 0.0162(4) 0.0122(4) 0.0021(2) 0.0000(4) 0.0023(3) Pb2 0.0161(4) 0.0142(4) 0.0143(4) 0.0008(2) 0.0011(4) -0.0004(3) Se1 0.0127(7) 0.0077(7) 0.0048(7) -0.0003(5) -0.0012(8) -0.0020(8) Se2 0.0069(7) 0.0047(7) 0.0048(8) -0.0001(7) 0.0002(6) 0.0002(6) Se3 0.0054(8) 0.0050(7) 0.0068(8) -0.0002(6) 0.0005(6) -0.0011(6) V1 0.0069(12) 0.0070(11) 0.0105(13) 0.0021(10) -0.0001(13) -0.0015(14) V2 0.0068(13) 0.0053(11) 0.0073(12) 0.0013(9) -0.0014(11) -0.0019(12) V3 0.0121(15) 0.0043(11) 0.0042(13) -0.0005(10) -0.0016(11) 0.0012(10) F1 0.027(5) 0.019(5) 0.009(4) -0.007(4) -0.001(5) 0.007(6) O1 0.006(2) 0.006(2) 0.006(2) -0.0002(13) 0.0004(13) -0.0007(13) O2 0.016(6) 0.017(6) 0.004(6) 0.004(5) -0.004(5) -0.013(5) O3 0.005(3) 0.005(3) 0.005(3) 0.0005(13) 0.0006(13) -0.0001(13) O4 0.007(5) 0.011(6) 0.021(7) 0.006(5) -0.002(5) -0.005(5) O5 0.004(5) 0.008(5) 0.013(6) 0.000(5) -0.001(5) -0.001(4) O6 0.007(3) 0.008(3) 0.007(3) 0.0004(13) 0.0001(13) 0.0005(13) O7 0.004(2) 0.005(2) 0.004(2) 0.0003(13) 0.0004(13) -0.0003(13) O8 0.026(6) 0.020(5) 0.011(5) -0.003(4) -0.003(7) -0.007(7) O9 0.008(5) 0.004(5) 0.011(6) -0.001(5) 0.002(4) -0.001(5) O10 0.009(3) 0.009(3) 0.009(3) -0.0005(13) 0.0004(13) 0.0002(13) O11 0.015(5) 0.011(5) 0.010(6) -0.001(5) -0.001(5) 0.006(5) O12 0.008(3) 0.009(3) 0.008(3) -0.0007(13) 0.0002(13) -0.0004(13) O13 0.014(3) 0.013(3) 0.014(3) -0.0002(13) -0.0013(13) 0.0001(13) O14 0.013(3) 0.013(3) 0.013(3) -0.0002(13) -0.0006(13) -0.0005(13) O15 0.012(6) 0.012(6) 0.017(6) -0.005(5) 0.003(5) 0.002(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source F F 0.0171 0.0103 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O11 Pb1 O11 85.2(3) 3_456 . ? O11 Pb1 O12 119.6(3) 3_456 . ? O11 Pb1 O12 116.7(3) . . ? O11 Pb1 O15 69.7(4) 3_456 . ? O11 Pb1 O15 75.7(3) . . ? O12 Pb1 O15 64.0(3) . . ? O11 Pb1 O2 76.6(3) 3_456 3_456 ? O11 Pb1 O2 153.8(3) . 3_456 ? O12 Pb1 O2 88.8(3) . 3_456 ? O15 Pb1 O2 114.1(3) . 3_456 ? O11 Pb1 O4 134.7(3) 3_456 . ? O11 Pb1 O4 86.2(3) . . ? O12 Pb1 O4 104.0(3) . . ? O15 Pb1 O4 148.8(3) . . ? O2 Pb1 O4 93.3(3) 3_456 . ? O11 Pb1 V3 107.7(3) 3_456 . ? O11 Pb1 V3 29.0(3) . . ? O12 Pb1 V3 89.3(2) . . ? O15 Pb1 V3 68.4(2) . . ? O2 Pb1 V3 175.7(2) 3_456 . ? O4 Pb1 V3 83.4(2) . . ? O10 Pb2 O6 72.6(3) 4_656 4_656 ? O10 Pb2 O3 125.4(3) 4_656 . ? O6 Pb2 O3 115.5(3) 4_656 . ? O10 Pb2 O5 104.4(3) 4_656 . ? O6 Pb2 O5 58.0(3) 4_656 . ? O3 Pb2 O5 57.5(3) . . ? O10 Pb2 F1 68.3(3) 4_656 1_455 ? O6 Pb2 F1 89.2(3) 4_656 1_455 ? O3 Pb2 F1 58.4(3) . 1_455 ? O5 Pb2 F1 58.6(3) . 1_455 ? O10 Pb2 O9 81.2(3) 4_656 . ? O6 Pb2 O9 152.7(3) 4_656 . ? O3 Pb2 O9 73.8(3) . . ? O5 Pb2 O9 124.1(3) . . ? F1 Pb2 O9 73.8(3) 1_455 . ? O15 Se1 O13 106.4(5) . . ? O15 Se1 O2 98.6(5) . . ? O13 Se1 O2 100.1(5) . . ? O6 Se2 O12 97.2(5) . . ? O6 Se2 O3 100.2(5) . . ? O12 Se2 O3 95.5(5) . . ? O14 Se3 O9 102.3(5) 1_455 . ? O14 Se3 O7 94.6(5) 1_455 1_455 ? O9 Se3 O7 100.7(5) . 1_455 ? O4 V1 O1 102.1(5) 3_456 . ? O4 V1 F1 95.4(6) 3_456 3_456 ? O1 V1 F1 94.7(5) . 3_456 ? O4 V1 O2 95.9(6) 3_456 . ? O1 V1 O2 96.0(5) . . ? F1 V1 O2 162.5(5) 3_456 . ? O4 V1 O3 90.2(5) 3_456 3_556 ? O1 V1 O3 167.3(5) . 3_556 ? F1 V1 O3 80.8(4) 3_456 3_556 ? O2 V1 O3 85.8(4) . 3_556 ? O4 V1 O5 165.7(5) 3_456 3_556 ? O1 V1 O5 92.1(4) . 3_556 ? F1 V1 O5 81.8(5) 3_456 3_556 ? O2 V1 O5 84.0(5) . 3_556 ? O3 V1 O5 75.5(4) 3_556 3_556 ? O8 V2 O5 104.4(6) . 4_646 ? O8 V2 O7 95.7(6) . . ? O5 V2 O7 96.3(5) 4_646 . ? O8 V2 O1 95.7(6) . 2 ? O5 V2 O1 94.7(5) 4_646 2 ? O7 V2 O1 161.7(4) . 2 ? O8 V2 O6 173.5(5) . . ? O5 V2 O6 82.0(5) 4_646 . ? O7 V2 O6 82.4(4) . . ? O1 V2 O6 84.7(4) 2 . ? O8 V2 O9 96.5(5) . . ? O5 V2 O9 159.1(5) 4_646 . ? O7 V2 O9 82.8(4) . . ? O1 V2 O9 81.8(4) 2 . ? O6 V2 O9 77.1(4) . . ? O10 V3 O11 102.2(5) . . ? O10 V3 O13 98.0(5) . . ? O11 V3 O13 95.0(5) . . ? O10 V3 O12 94.1(5) . 1_655 ? O11 V3 O12 96.0(5) . 1_655 ? O13 V3 O12 161.6(5) . 1_655 ? O10 V3 O14 105.1(5) . 4_746 ? O11 V3 O14 152.7(5) . 4_746 ? O13 V3 O14 81.6(5) . 4_746 ? O12 V3 O14 81.8(4) 1_655 4_746 ? O10 V3 Pb1 56.4(4) . . ? O11 V3 Pb1 46.0(4) . . ? O13 V3 Pb1 96.7(3) . . ? O12 V3 Pb1 101.6(3) 1_655 . ? O14 V3 Pb1 161.1(3) 4_746 . ? V1 F1 Pb2 101.0(5) 3_556 1_655 ? V1 O1 V2 139.7(6) . 2_554 ? Se1 O2 V1 119.7(5) . . ? Se1 O2 Pb1 127.7(5) . 3_556 ? V1 O2 Pb1 112.4(4) . 3_556 ? Se2 O3 V1 119.2(5) . 3_456 ? Se2 O3 Pb2 117.9(5) . . ? V1 O3 Pb2 97.2(4) 3_456 . ? V1 O4 Pb1 135.9(6) 3_556 . ? V2 O5 V1 143.0(6) 4_656 3_456 ? V2 O5 Pb2 113.9(5) 4_656 . ? V1 O5 Pb2 96.4(4) 3_456 . ? Se2 O6 V2 129.9(6) . . ? Se2 O6 Pb2 113.8(5) . 4_646 ? V2 O6 Pb2 102.1(4) . 4_646 ? Se3 O7 V2 118.0(6) 1_655 . ? Se3 O9 V2 115.9(5) . . ? Se3 O9 Pb2 136.0(5) . . ? V2 O9 Pb2 106.7(4) . . ? V3 O10 Pb2 134.1(6) . 4_646 ? V3 O11 Pb1 132.2(5) . 3_556 ? V3 O11 Pb1 105.0(5) . . ? Pb1 O11 Pb1 114.4(4) 3_556 . ? Se2 O12 V3 126.6(6) . 1_455 ? Se2 O12 Pb1 109.5(5) . . ? V3 O12 Pb1 110.5(5) 1_455 . ? Se1 O13 V3 128.0(6) . . ? Se3 O14 V3 128.7(6) 1_655 4_756 ? Se1 O15 Pb1 131.7(6) . . ? 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 O11 2.475(11) 3_456 ? Pb1 O11 2.517(10) . ? Pb1 O12 2.540(10) . ? Pb1 O15 2.622(11) . ? Pb1 O2 2.662(10) 3_456 ? Pb1 O4 2.728(11) . ? Pb1 V3 3.379(2) . ? Pb2 O10 2.601(10) 4_656 ? Pb2 O6 2.609(10) 4_656 ? Pb2 O3 2.648(10) . ? Pb2 O5 2.677(10) . ? Pb2 F1 2.682(13) 1_455 ? Pb2 O9 2.707(10) . ? Se1 O15 1.673(11) . ? Se1 O13 1.711(11) . ? Se1 O2 1.744(10) . ? Se2 O6 1.676(10) . ? Se2 O12 1.724(11) . ? Se2 O3 1.729(10) . ? Se3 O14 1.690(11) 1_455 ? Se3 O9 1.697(10) . ? Se3 O7 1.729(10) 1_455 ? V1 O4 1.635(11) 3_456 ? V1 O1 1.702(10) . ? V1 F1 1.909(9) 3_456 ? V1 O2 1.963(11) . ? V1 O3 2.093(10) 3_556 ? V1 O5 2.090(10) 3_556 ? V2 O8 1.611(10) . ? V2 O5 1.712(10) 4_646 ? V2 O7 1.965(10) . ? V2 O1 2.001(10) 2 ? V2 O6 2.158(10) . ? V2 O9 2.184(11) . ? V3 O10 1.631(11) . ? V3 O11 1.696(11) . ? V3 O13 1.935(11) . ? V3 O12 1.955(10) 1_655 ? V3 O14 1.996(11) 4_746 ? F1 V1 1.909(9) 3_556 ? F1 Pb2 2.682(13) 1_655 ? O1 V2 2.001(10) 2_554 ? O2 Pb1 2.662(10) 3_556 ? O3 V1 2.093(10) 3_456 ? O4 V1 1.635(11) 3_556 ? O5 V2 1.712(10) 4_656 ? O5 V1 2.090(10) 3_456 ? O6 Pb2 2.609(10) 4_646 ? O7 Se3 1.729(10) 1_655 ? O10 Pb2 2.601(10) 4_646 ? O11 Pb1 2.475(11) 3_556 ? O12 V3 1.955(10) 1_455 ? O14 Se3 1.690(11) 1_655 ? O14 V3 1.996(11) 4_756 ? 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 O4 V1 O1 V2 28.2(10) 3_456 . . 2_554 ? F1 V1 O1 V2 -68.3(10) 3_456 . . 2_554 ? O2 V1 O1 V2 125.6(9) . . . 2_554 ? O3 V1 O1 V2 -137.0(18) 3_556 . . 2_554 ? O5 V1 O1 V2 -150.2(9) 3_556 . . 2_554 ? O15 Se1 O2 V1 -113.4(7) . . . . ? O13 Se1 O2 V1 138.1(7) . . . . ? O15 Se1 O2 Pb1 72.2(7) . . . 3_556 ? O13 Se1 O2 Pb1 -36.3(8) . . . 3_556 ? O6 Se2 O3 V1 -164.3(6) . . . 3_456 ? O12 Se2 O3 V1 97.4(6) . . . 3_456 ? O6 Se2 O3 Pb2 -47.0(6) . . . . ? O12 Se2 O3 Pb2 -145.3(5) . . . . ? O12 Se2 O6 V2 -166.8(7) . . . . ? O3 Se2 O6 V2 96.2(7) . . . . ? O12 Se2 O6 Pb2 -35.0(6) . . . 4_646 ? O3 Se2 O6 Pb2 -132.0(5) . . . 4_646 ? O14 Se3 O9 V2 164.1(6) 1_455 . . . ? O7 Se3 O9 V2 -98.7(6) 1_455 . . . ? O14 Se3 O9 Pb2 -0.4(9) 1_455 . . . ? O7 Se3 O9 Pb2 96.7(8) 1_455 . . . ? O11 V3 O10 Pb2 161.3(7) . . . 4_646 ? O13 V3 O10 Pb2 64.4(8) . . . 4_646 ? O12 V3 O10 Pb2 -101.7(8) 1_655 . . 4_646 ? O14 V3 O10 Pb2 -19.0(9) 4_746 . . 4_646 ? Pb1 V3 O10 Pb2 157.2(9) . . . 4_646 ? O10 V3 O11 Pb1 -149.9(7) . . . 3_556 ? O13 V3 O11 Pb1 -50.6(8) . . . 3_556 ? O12 V3 O11 Pb1 114.5(7) 1_655 . . 3_556 ? O14 V3 O11 Pb1 30.8(15) 4_746 . . 3_556 ? Pb1 V3 O11 Pb1 -145.1(10) . . . 3_556 ? O10 V3 O11 Pb1 -4.8(6) . . . . ? O13 V3 O11 Pb1 94.5(5) . . . . ? O12 V3 O11 Pb1 -100.3(5) 1_655 . . . ? O14 V3 O11 Pb1 175.9(8) 4_746 . . . ? O6 Se2 O12 V3 134.4(7) . . . 1_455 ? O3 Se2 O12 V3 -124.5(7) . . . 1_455 ? O6 Se2 O12 Pb1 -88.9(5) . . . . ? O3 Se2 O12 Pb1 12.1(5) . . . . ? O15 Se1 O13 V3 -22.1(9) . . . . ? O2 Se1 O13 V3 80.1(8) . . . . ? O13 Se1 O15 Pb1 38.1(9) . . . . ? O2 Se1 O15 Pb1 -65.2(8) . . . . ?