#------------------------------------------------------------------------------ #$Date: 2022-08-14 01:46:42 +0300 (Sun, 14 Aug 2022) $ #$Revision: 277242 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/09/7710968.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_7710968 loop_ _publ_author_name 'Radius, Udo' 'Philipp, Michael S. M.' 'Bertermann, R\"udiger' _publ_section_title ; N-Heterocyclic Carbene and Cyclic (Alkyl)(amino)carbene Adducts of Plumbanes and Plumbylenes ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D2DT02462D _journal_year 2022 _chemical_formula_moiety 'C39 H46 Cl2 N2 Pb, 1.5(C6 H6)' _chemical_formula_sum 'C48 H55 Cl2 N2 Pb' _chemical_formula_weight 938.03 _space_group_crystal_system monoclinic _space_group_IT_number 11 _space_group_name_Hall '-P 2yb' _space_group_name_H-M_alt 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-07-28 deposited with the CCDC. 2022-08-12 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 114.541(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.3251(4) _cell_length_b 37.2721(10) _cell_length_c 12.1542(4) _cell_measurement_reflns_used 15747 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 31.1330 _cell_measurement_theta_min 2.1120 _cell_volume 4254.9(3) _computing_cell_refinement 'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)' _computing_data_collection 'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)' _computing_data_reduction 'CrysAlisPro 1.171.41.63a (Rigaku OD, 2020)' _computing_molecular_graphics 'ShelXLe (Huebschle et all, 2011)' _computing_publication_material 'SHELXL-2014/6 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_Laue_measured_fraction_full 0.975 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 27625 _diffrn_reflns_point_group_measured_fraction_full 0.975 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 1.921 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 4.125 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.729 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.63a (Rigaku Oxford Diffraction, 2020) 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_crystal_colour colourless _exptl_crystal_density_diffrn 1.464 _exptl_crystal_description block _exptl_crystal_F_000 1892 _exptl_crystal_size_max 0.143 _exptl_crystal_size_mid 0.078 _exptl_crystal_size_min 0.056 _refine_diff_density_max 1.156 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.094 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.201 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 489 _refine_ls_number_reflns 8594 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.201 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+9.1700P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0548 _refine_ls_wR_factor_ref 0.0559 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7890 _reflns_number_total 8594 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt02462d2.cif _cod_data_source_block compound_7 _cod_original_sg_symbol_H-M 'P 21/m' _cod_database_code 7710968 _shelx_shelxl_version_number 2018/3 _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_estimated_absorpt_t_min 0.596 _shelx_estimated_absorpt_t_max 0.790 _shelx_res_file ; TITL MiPh047_test_a.res in P2(1)/m MiPh047_test_a.res created by SHELXL-2018/3 at 09:42:31 on 26-Mar-2021 REM Old TITL MiPh047_test in P2/m REM SHELXT solution in P2(1)/m REM R1 0.064, Rweak 0.010, Alpha 0.114, Orientation as input REM Formula found by SHELXT: C40 N10 Cl2 Pb CELL 0.71073 10.3251 37.2721 12.1542 90.000 114.541 90.000 ZERR 4.000 0.0004 0.0010 0.0004 0.000 0.004 0.000 LATT 1 SYMM -X, 1/2+Y, -Z SFAC C H N CL PB UNIT 192 220 8 8 4 TEMP -173 SIZE 0.06 0.08 0.14 L.S. 10 BOND $H LIST 4 Acta 52 Shel 1000000 0.8 FMAP 2 PLAN 20 WGHT 0.000000 9.170000 FVAR 0.22321 PB01 5 0.206986 0.569757 0.683976 11.00000 0.01090 0.01210 = 0.01011 0.00004 0.00375 -0.00069 C1 1 0.391763 0.673123 0.619173 11.00000 0.01881 0.01382 = 0.01751 0.00163 0.00768 -0.00467 AFIX 43 H1 2 0.399169 0.691217 0.567033 11.00000 -1.20000 AFIX 0 CL02 4 0.000475 0.614758 0.680327 11.00000 0.01271 0.01659 = 0.01419 0.00078 0.00494 0.00337 C2 1 0.151577 0.655153 0.969395 11.00000 0.01818 0.02169 = 0.02207 -0.00503 0.01134 -0.00315 AFIX 137 H2A 2 0.063730 0.668681 0.925287 11.00000 -1.50000 H2B 2 0.188681 0.660966 1.055709 11.00000 -1.50000 H2C 2 0.131482 0.629390 0.958022 11.00000 -1.50000 AFIX 0 CL03 4 0.431135 0.534334 0.691624 11.00000 0.01255 0.01854 = 0.01573 0.00127 0.00651 0.00337 C3 1 0.653229 0.603925 1.076584 11.00000 0.01294 0.01691 = 0.01348 0.00055 -0.00110 -0.00069 AFIX 43 H3 2 0.740506 0.591177 1.113053 11.00000 -1.20000 AFIX 0 N004 3 0.413039 0.642060 0.779394 11.00000 0.01094 0.01390 = 0.01093 -0.00009 0.00471 -0.00054 C4 1 0.243321 0.553756 0.869063 11.00000 0.01681 0.01042 = 0.01459 -0.00067 0.00836 -0.00259 C5 1 0.130129 0.535451 0.428895 11.00000 0.01546 0.01878 = 0.01871 -0.00121 0.00671 -0.00252 AFIX 43 H5 2 0.230621 0.533239 0.458627 11.00000 -1.20000 AFIX 0 C6 1 0.485037 0.598795 0.489639 11.00000 0.01753 0.02413 = 0.01733 0.00278 0.00851 0.00270 AFIX 13 H6 2 0.497082 0.596390 0.575304 11.00000 -1.20000 AFIX 0 C7 1 0.331159 0.609438 0.413101 11.00000 0.01311 0.01504 = 0.01430 0.00159 0.00678 -0.00423 C00E 1 0.397976 0.530042 1.063429 11.00000 0.01945 0.01547 = 0.01248 -0.00038 0.00022 0.00071 AFIX 43 H00E 2 0.490005 0.522885 1.119777 11.00000 -1.20000 AFIX 0 N9 3 0.317809 0.641182 0.584728 11.00000 0.00878 0.01367 = 0.01196 -0.00068 0.00409 0.00099 C8 1 0.249498 0.629486 0.458751 11.00000 0.01343 0.01385 = 0.01049 -0.00097 0.00540 -0.00385 C00F 1 0.261871 0.665154 0.921388 11.00000 0.01507 0.01609 = 0.01411 -0.00126 0.00535 -0.00128 AFIX 13 H00F 2 0.217874 0.661420 0.831822 11.00000 -1.20000 AFIX 0 C00H 1 0.469253 0.631324 0.906313 11.00000 0.01222 0.01398 = 0.00882 -0.00139 0.00284 -0.00662 C00I 1 0.283419 0.528172 1.095300 11.00000 0.03052 0.01484 = 0.01413 0.00003 0.01020 0.00073 AFIX 43 H00I 2 0.296820 0.519274 1.172538 11.00000 -1.20000 AFIX 0 C00J 1 -0.129464 0.654879 0.393509 11.00000 0.01502 0.02466 = 0.01997 0.00343 0.00543 0.00149 AFIX 137 H00A 2 -0.176954 0.660294 0.306905 11.00000 -1.50000 H00B 2 -0.173916 0.668775 0.437031 11.00000 -1.50000 H00C 2 -0.138528 0.629210 0.406303 11.00000 -1.50000 AFIX 0 C00K 1 -0.164162 0.540984 0.344175 11.00000 0.01700 0.01761 = 0.02149 0.00021 0.00057 -0.00229 AFIX 43 H00K 2 -0.264724 0.542333 0.315984 11.00000 -1.20000 AFIX 0 C00L 1 0.149010 0.539372 1.013742 11.00000 0.02300 0.01694 = 0.02021 0.00203 0.01352 0.00178 AFIX 43 H00L 2 0.070683 0.537940 1.035362 11.00000 -1.20000 AFIX 0 C00M 1 0.679480 0.602505 0.877659 11.00000 0.01006 0.02289 = 0.01629 -0.00308 0.00372 0.00108 AFIX 13 H00M 2 0.608245 0.599959 0.791877 11.00000 -1.20000 AFIX 0 C00N 1 -0.077277 0.553295 0.459571 11.00000 0.01739 0.01621 = 0.01713 -0.00046 0.00529 -0.00110 AFIX 43 H00N 2 -0.117753 0.563467 0.509773 11.00000 -1.20000 AFIX 0 C00O 1 0.378648 0.542325 0.949557 11.00000 0.00987 0.01402 = 0.01672 -0.00017 0.00773 -0.00124 AFIX 43 H00O 2 0.456233 0.542938 0.926821 11.00000 -1.20000 AFIX 0 C00P 1 0.109405 0.641169 0.389984 11.00000 0.01554 0.01430 = 0.01453 0.00337 0.00671 -0.00494 C00Q 1 0.759178 0.566965 0.916111 11.00000 0.01537 0.02552 = 0.02924 -0.00388 0.00695 0.00054 AFIX 137 H00D 2 0.694793 0.548598 0.922607 11.00000 -1.50000 H00G 2 0.840164 0.569942 0.994698 11.00000 -1.50000 H00H 2 0.793736 0.559541 0.855711 11.00000 -1.50000 AFIX 0 C00R 1 0.049352 0.630712 0.268271 11.00000 0.01599 0.01967 = 0.01305 0.00255 0.00133 -0.00343 AFIX 43 H00R 2 -0.045625 0.637569 0.218016 11.00000 -1.20000 AFIX 0 C00S 1 0.264188 0.600225 0.290423 11.00000 0.02037 0.01785 = 0.01890 -0.00102 0.01287 -0.00047 AFIX 43 H00S 2 0.314765 0.586607 0.254999 11.00000 -1.20000 AFIX 0 C00T 1 0.451581 0.673632 0.741556 11.00000 0.01714 0.01349 = 0.01737 -0.00338 0.00522 -0.00586 AFIX 43 H00T 2 0.509116 0.692174 0.791847 11.00000 -1.20000 AFIX 0 C00U 1 0.128817 0.552669 0.900588 11.00000 0.01380 0.01272 = 0.01624 0.00268 0.00655 0.00280 AFIX 43 H00U 2 0.037701 0.560889 0.845720 11.00000 -1.20000 AFIX 0 C00V 1 -0.105133 0.526800 0.270255 11.00000 0.02778 0.01461 = 0.01189 0.00229 -0.00059 -0.00311 AFIX 43 H00V 2 -0.165001 0.519267 0.190519 11.00000 -1.20000 AFIX 0 C00W 1 0.027834 0.664781 0.440680 11.00000 0.01755 0.01847 = 0.01263 0.00172 0.00536 0.00043 AFIX 13 H00W 2 0.071202 0.661788 0.530560 11.00000 -1.20000 AFIX 0 C00X 1 0.069016 0.550498 0.500112 11.00000 0.01551 0.01184 = 0.00979 0.00102 0.00125 -0.00343 C00Y 1 0.042023 0.523563 0.312713 11.00000 0.03115 0.01932 = 0.01567 -0.00487 0.01039 -0.00236 AFIX 43 H00Y 2 0.082496 0.513273 0.262686 11.00000 -1.20000 AFIX 0 C00Z 1 0.526708 0.562918 0.451628 11.00000 0.02323 0.02868 = 0.03015 0.00458 0.01625 0.00758 AFIX 137 H00J 2 0.456540 0.544577 0.446808 11.00000 -1.50000 H00P 2 0.620923 0.555665 0.511438 11.00000 -1.50000 H00Q 2 0.529289 0.565586 0.372350 11.00000 -1.50000 AFIX 0 C010 1 0.586475 0.628436 0.485541 11.00000 0.01447 0.03304 = 0.02973 -0.00260 0.01035 -0.00338 AFIX 137 H01A 2 0.576104 0.631482 0.402196 11.00000 -1.50000 H01B 2 0.684868 0.621700 0.537385 11.00000 -1.50000 H01C 2 0.563118 0.651021 0.514430 11.00000 -1.50000 AFIX 0 C10 1 0.329538 0.621830 0.682927 11.00000 0.00600 0.01372 = 0.01297 0.00165 0.00404 0.00073 C011 1 0.455606 0.632862 1.096954 11.00000 0.02175 0.01821 = 0.01340 -0.00137 0.00889 -0.00363 AFIX 43 H011 2 0.408873 0.639504 1.146723 11.00000 -1.20000 AFIX 0 C012 1 0.396231 0.642448 0.974800 11.00000 0.01347 0.01064 = 0.01373 -0.00083 0.00518 -0.00317 C013 1 0.599366 0.612368 0.953619 11.00000 0.01486 0.01469 = 0.01977 -0.00103 0.00539 -0.00332 C014 1 0.581888 0.613777 1.146151 11.00000 0.02168 0.01782 = 0.01244 0.00268 0.00364 -0.00284 AFIX 43 H014 2 0.620215 0.607334 1.229257 11.00000 -1.20000 AFIX 0 C015 1 0.783136 0.632406 0.882065 11.00000 0.01987 0.02646 = 0.02886 -0.00153 0.01472 -0.00126 AFIX 137 H01D 2 0.830047 0.626173 0.829178 11.00000 -1.50000 H01E 2 0.854999 0.635237 0.965231 11.00000 -1.50000 H01F 2 0.730731 0.654954 0.854607 11.00000 -1.50000 AFIX 0 C016 1 0.042258 0.704343 0.412930 11.00000 0.02397 0.02166 = 0.02939 -0.00110 0.01218 0.00065 AFIX 137 H01G 2 0.000924 0.707954 0.325145 11.00000 -1.50000 H01H 2 0.143179 0.711004 0.447204 11.00000 -1.50000 H01I 2 -0.008113 0.719351 0.448710 11.00000 -1.50000 AFIX 0 C017 1 0.125373 0.610660 0.219951 11.00000 0.02542 0.01919 = 0.01188 -0.00273 0.00657 -0.00860 AFIX 43 H017 2 0.081914 0.603906 0.137145 11.00000 -1.20000 AFIX 0 C018 1 0.673057 0.731475 1.135125 11.00000 0.03205 0.04376 = 0.03144 0.00201 -0.00002 -0.00837 AFIX 43 H018 2 0.632229 0.718665 1.180474 11.00000 -1.20000 AFIX 0 C019 1 0.299777 0.705092 0.945710 11.00000 0.01885 0.02018 = 0.03117 0.00026 0.01002 0.00006 AFIX 137 H01J 2 0.364318 0.711988 0.908762 11.00000 -1.50000 H01K 2 0.346496 0.709253 1.033152 11.00000 -1.50000 H01L 2 0.212697 0.719510 0.910731 11.00000 -1.50000 AFIX 0 C01A 1 0.732526 0.713201 1.069067 11.00000 0.04398 0.02793 = 0.02721 0.00205 -0.00053 0.00028 AFIX 43 H01M 2 0.730201 0.687720 1.067543 11.00000 -1.20000 AFIX 0 C01B 1 0.719383 0.750000 0.681781 10.50000 0.05263 0.10532 = 0.03248 0.00000 0.01801 0.00000 AFIX 43 H01N 2 0.627936 0.750000 0.682912 10.50000 -1.20000 AFIX 0 C01C 1 0.794984 0.731180 1.005517 11.00000 0.06256 0.04226 = 0.02990 -0.00470 0.01552 0.00624 AFIX 43 H01O 2 0.837860 0.718301 0.961894 11.00000 -1.20000 AFIX 0 C01D 1 0.476441 0.730381 0.361341 11.00000 0.06081 0.07440 = 0.03429 0.01581 0.01090 0.01548 AFIX 43 H01P 2 0.561124 0.717148 0.404648 11.00000 -1.20000 AFIX 0 C01E 1 0.982760 0.750000 0.678513 10.50000 0.02372 0.11039 = 0.02052 0.00000 0.00473 0.00000 AFIX 43 H01Q 2 1.074244 0.750000 0.677454 10.50000 -1.20000 AFIX 0 C01F 1 0.912390 0.782409 0.679326 11.00000 0.08506 0.02942 = 0.01955 0.00059 0.00571 -0.02669 AFIX 43 H01R 2 0.955540 0.804875 0.678708 11.00000 -1.20000 AFIX 0 C01G 1 0.782461 0.780853 0.681000 11.00000 0.07320 0.05848 = 0.02498 -0.00231 0.00869 0.02940 AFIX 43 H01S 2 0.734851 0.802611 0.681637 11.00000 -1.20000 AFIX 0 C01H 1 0.229415 0.731803 0.231202 11.00000 0.06457 0.06262 = 0.04578 0.00408 0.03817 -0.00029 AFIX 43 H01T 2 0.144282 0.719091 0.184988 11.00000 -1.20000 AFIX 0 C01I 1 0.350452 0.713546 0.296907 11.00000 0.06935 0.03493 = 0.02991 -0.00155 0.02448 -0.00033 AFIX 43 H01U 2 0.347331 0.688081 0.298079 11.00000 -1.20000 AFIX 0 HKLF 4 REM MiPh047_test_a.res in P2(1)/m REM wR2 = 0.055946, GooF = S = 1.20142, Restrained GooF = 1.20142 for all data REM R1 = 0.031914 for 7890 Fo > 4sig(Fo) and 0.037477 for all 8594 data REM 489 parameters refined using 0 restraints END WGHT 0.0000 9.3330 REM Highest difference peak 1.156, deepest hole -0.926, 1-sigma level 0.094 Q1 1 0.6244 0.7095 1.0530 11.00000 0.05 1.16 Q2 1 0.5632 0.7500 0.3552 10.50000 0.05 0.97 Q3 1 0.2870 0.7500 0.2803 10.50000 0.05 0.71 Q4 1 0.1595 0.5548 0.7175 11.00000 0.05 0.65 Q5 1 0.4147 0.7500 1.0571 10.50000 0.05 0.58 Q6 1 0.5070 0.7145 0.3223 11.00000 0.05 0.56 Q7 1 0.2557 0.5875 0.6611 11.00000 0.05 0.55 Q8 1 0.2414 0.5551 0.6434 11.00000 0.05 0.51 Q9 1 0.5154 0.6121 0.9243 11.00000 0.05 0.50 Q10 1 0.1598 0.5854 0.7248 11.00000 0.05 0.49 Q11 1 0.3249 0.6545 0.9426 11.00000 0.05 0.46 Q12 1 0.2789 0.5781 0.7647 11.00000 0.05 0.43 Q13 1 0.0355 0.5722 0.4270 11.00000 0.05 0.42 Q14 1 0.3978 0.6097 0.6221 11.00000 0.05 0.42 Q15 1 0.2032 0.5310 0.7798 11.00000 0.05 0.42 Q16 1 0.2791 0.6851 0.9344 11.00000 0.05 0.42 Q17 1 0.3792 0.5334 0.5995 11.00000 0.05 0.41 Q18 1 0.1844 0.5469 0.6258 11.00000 0.05 0.40 Q19 1 1.0184 0.7770 0.6966 11.00000 0.05 0.39 Q20 1 0.3219 0.5542 0.9131 11.00000 0.05 0.39 ; _shelx_res_checksum 33259 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' 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 0.20699(2) 0.56976(2) 0.68398(2) 0.01124(4) Uani 1 1 d . . . . . C1 C 0.3918(4) 0.67312(9) 0.6192(3) 0.0167(7) Uani 1 1 d . . . . . H1 H 0.399169 0.691217 0.567033 0.020 Uiso 1 1 calc R U . . . Cl02 Cl 0.00047(9) 0.61476(2) 0.68033(7) 0.01471(17) Uani 1 1 d . . . . . C2 C 0.1516(4) 0.65515(10) 0.9694(3) 0.0196(8) Uani 1 1 d . . . . . H2A H 0.063730 0.668681 0.925287 0.029 Uiso 1 1 calc R U . . . H2B H 0.188681 0.660966 1.055709 0.029 Uiso 1 1 calc R U . . . H2C H 0.131482 0.629390 0.958022 0.029 Uiso 1 1 calc R U . . . Cl03 Cl 0.43114(9) 0.53433(2) 0.69162(7) 0.01539(17) Uani 1 1 d . . . . . C3 C 0.6532(4) 0.60393(10) 1.0766(3) 0.0166(7) Uani 1 1 d . . . . . H3 H 0.740506 0.591177 1.113053 0.020 Uiso 1 1 calc R U . . . N004 N 0.4130(3) 0.64206(7) 0.7794(2) 0.0119(6) Uani 1 1 d . . . . . C4 C 0.2433(4) 0.55376(9) 0.8691(3) 0.0133(7) Uani 1 1 d . . . . . C5 C 0.1301(4) 0.53545(10) 0.4289(3) 0.0178(8) Uani 1 1 d . . . . . H5 H 0.230621 0.533239 0.458627 0.021 Uiso 1 1 calc R U . . . C6 C 0.4850(4) 0.59880(10) 0.4896(3) 0.0192(8) Uani 1 1 d . . . . . H6 H 0.497082 0.596390 0.575304 0.023 Uiso 1 1 calc R U . . . C7 C 0.3312(4) 0.60944(9) 0.4131(3) 0.0138(7) Uani 1 1 d . . . . . C00E C 0.3980(4) 0.53004(9) 1.0634(3) 0.0179(8) Uani 1 1 d . . . . . H00E H 0.490005 0.522885 1.119777 0.022 Uiso 1 1 calc R U . . . N9 N 0.3178(3) 0.64118(7) 0.5847(2) 0.0115(6) Uani 1 1 d . . . . . C8 C 0.2495(4) 0.62949(9) 0.4588(3) 0.0124(7) Uani 1 1 d . . . . . C00F C 0.2619(4) 0.66515(9) 0.9214(3) 0.0153(7) Uani 1 1 d . . . . . H00F H 0.217874 0.661420 0.831822 0.018 Uiso 1 1 calc R U . . . C00H C 0.4693(4) 0.63132(9) 0.9063(3) 0.0122(7) Uani 1 1 d . . . . . C00I C 0.2834(4) 0.52817(10) 1.0953(3) 0.0195(8) Uani 1 1 d . . . . . H00I H 0.296820 0.519274 1.172538 0.023 Uiso 1 1 calc R U . . . C00J C -0.1295(4) 0.65488(10) 0.3935(3) 0.0205(8) Uani 1 1 d . . . . . H00A H -0.176954 0.660294 0.306905 0.031 Uiso 1 1 calc R U . . . H00B H -0.173916 0.668775 0.437031 0.031 Uiso 1 1 calc R U . . . H00C H -0.138528 0.629210 0.406303 0.031 Uiso 1 1 calc R U . . . C00K C -0.1642(4) 0.54098(10) 0.3442(3) 0.0212(8) Uani 1 1 d . . . . . H00K H -0.264724 0.542333 0.315984 0.025 Uiso 1 1 calc R U . . . C00L C 0.1490(4) 0.53937(9) 1.0137(3) 0.0185(8) Uani 1 1 d . . . . . H00L H 0.070683 0.537940 1.035362 0.022 Uiso 1 1 calc R U . . . C00M C 0.6795(4) 0.60250(10) 0.8777(3) 0.0170(7) Uani 1 1 d . . . . . H00M H 0.608245 0.599959 0.791877 0.020 Uiso 1 1 calc R U . . . C00N C -0.0773(4) 0.55330(10) 0.4596(3) 0.0175(7) Uani 1 1 d . . . . . H00N H -0.117753 0.563467 0.509773 0.021 Uiso 1 1 calc R U . . . C00O C 0.3786(4) 0.54233(9) 0.9496(3) 0.0128(7) Uani 1 1 d . . . . . H00O H 0.456233 0.542938 0.926821 0.015 Uiso 1 1 calc R U . . . C00P C 0.1094(4) 0.64117(9) 0.3900(3) 0.0146(7) Uani 1 1 d . . . . . C00Q C 0.7592(4) 0.56696(11) 0.9161(3) 0.0242(8) Uani 1 1 d . . . . . H00D H 0.694793 0.548598 0.922607 0.036 Uiso 1 1 calc R U . . . H00G H 0.840164 0.569942 0.994698 0.036 Uiso 1 1 calc R U . . . H00H H 0.793736 0.559541 0.855711 0.036 Uiso 1 1 calc R U . . . C00R C 0.0494(4) 0.63071(10) 0.2683(3) 0.0178(8) Uani 1 1 d . . . . . H00R H -0.045625 0.637569 0.218016 0.021 Uiso 1 1 calc R U . . . C00S C 0.2642(4) 0.60023(10) 0.2904(3) 0.0175(8) Uani 1 1 d . . . . . H00S H 0.314765 0.586607 0.254999 0.021 Uiso 1 1 calc R U . . . C00T C 0.4516(4) 0.67363(9) 0.7416(3) 0.0167(7) Uani 1 1 d . . . . . H00T H 0.509116 0.692174 0.791847 0.020 Uiso 1 1 calc R U . . . C00U C 0.1288(4) 0.55267(9) 0.9006(3) 0.0141(7) Uani 1 1 d . . . . . H00U H 0.037701 0.560889 0.845720 0.017 Uiso 1 1 calc R U . . . C00V C -0.1051(4) 0.52680(10) 0.2703(3) 0.0210(8) Uani 1 1 d . . . . . H00V H -0.165001 0.519267 0.190519 0.025 Uiso 1 1 calc R U . . . C00W C 0.0278(4) 0.66478(9) 0.4407(3) 0.0165(7) Uani 1 1 d . . . . . H00W H 0.071202 0.661788 0.530560 0.020 Uiso 1 1 calc R U . . . C00X C 0.0690(4) 0.55050(9) 0.5001(3) 0.0137(7) Uani 1 1 d . . . . . C00Y C 0.0420(4) 0.52356(10) 0.3127(3) 0.0218(8) Uani 1 1 d . . . . . H00Y H 0.082496 0.513273 0.262686 0.026 Uiso 1 1 calc R U . . . C00Z C 0.5267(4) 0.56292(11) 0.4516(3) 0.0256(9) Uani 1 1 d . . . . . H00J H 0.456540 0.544577 0.446808 0.038 Uiso 1 1 calc R U . . . H00P H 0.620923 0.555665 0.511438 0.038 Uiso 1 1 calc R U . . . H00Q H 0.529289 0.565586 0.372350 0.038 Uiso 1 1 calc R U . . . C010 C 0.5865(4) 0.62844(11) 0.4855(3) 0.0254(9) Uani 1 1 d . . . . . H01A H 0.576104 0.631482 0.402196 0.038 Uiso 1 1 calc R U . . . H01B H 0.684868 0.621700 0.537385 0.038 Uiso 1 1 calc R U . . . H01C H 0.563118 0.651021 0.514430 0.038 Uiso 1 1 calc R U . . . C10 C 0.3295(3) 0.62183(9) 0.6829(3) 0.0109(7) Uani 1 1 d . . . . . C011 C 0.4556(4) 0.63286(9) 1.0970(3) 0.0173(8) Uani 1 1 d . . . . . H011 H 0.408873 0.639504 1.146723 0.021 Uiso 1 1 calc R U . . . C012 C 0.3962(4) 0.64245(9) 0.9748(3) 0.0128(7) Uani 1 1 d . . . . . C013 C 0.5994(4) 0.61237(9) 0.9536(3) 0.0170(8) Uani 1 1 d . . . . . C014 C 0.5819(4) 0.61378(10) 1.1462(3) 0.0185(8) Uani 1 1 d . . . . . H014 H 0.620215 0.607334 1.229257 0.022 Uiso 1 1 calc R U . . . C015 C 0.7831(4) 0.63241(11) 0.8821(3) 0.0235(8) Uani 1 1 d . . . . . H01D H 0.830047 0.626173 0.829178 0.035 Uiso 1 1 calc R U . . . H01E H 0.854999 0.635237 0.965231 0.035 Uiso 1 1 calc R U . . . H01F H 0.730731 0.654954 0.854607 0.035 Uiso 1 1 calc R U . . . C016 C 0.0423(4) 0.70434(10) 0.4129(3) 0.0246(9) Uani 1 1 d . . . . . H01G H 0.000924 0.707954 0.325145 0.037 Uiso 1 1 calc R U . . . H01H H 0.143179 0.711004 0.447204 0.037 Uiso 1 1 calc R U . . . H01I H -0.008113 0.719351 0.448710 0.037 Uiso 1 1 calc R U . . . C017 C 0.1254(4) 0.61066(9) 0.2200(3) 0.0192(8) Uani 1 1 d . . . . . H017 H 0.081914 0.603906 0.137145 0.023 Uiso 1 1 calc R U . . . C018 C 0.6731(5) 0.73148(13) 1.1351(4) 0.0402(11) Uani 1 1 d . . . . . H018 H 0.632229 0.718665 1.180474 0.048 Uiso 1 1 calc R U . . . C019 C 0.2998(4) 0.70509(10) 0.9457(3) 0.0235(8) Uani 1 1 d . . . . . H01J H 0.364318 0.711988 0.908762 0.035 Uiso 1 1 calc R U . . . H01K H 0.346496 0.709253 1.033152 0.035 Uiso 1 1 calc R U . . . H01L H 0.212697 0.719510 0.910731 0.035 Uiso 1 1 calc R U . . . C01A C 0.7325(5) 0.71320(12) 1.0691(4) 0.0382(11) Uani 1 1 d . . . . . H01M H 0.730201 0.687720 1.067543 0.046 Uiso 1 1 calc R U . . . C01B C 0.7194(10) 0.750000 0.6818(7) 0.063(2) Uani 1 2 d S T P . . H01N H 0.627936 0.750000 0.682912 0.076 Uiso 1 2 calc R U P . . C01C C 0.7950(6) 0.73118(13) 1.0055(4) 0.0461(13) Uani 1 1 d . . . . . H01O H 0.837860 0.718301 0.961894 0.055 Uiso 1 1 calc R U . . . C01D C 0.4764(7) 0.73038(16) 0.3613(4) 0.0595(16) Uani 1 1 d . . . . . H01P H 0.561124 0.717148 0.404648 0.071 Uiso 1 1 calc R U . . . C01E C 0.9828(8) 0.750000 0.6785(5) 0.053(2) Uani 1 2 d S T P . . H01Q H 1.074244 0.750000 0.677454 0.064 Uiso 1 2 calc R U P . . C01F C 0.9124(7) 0.78241(13) 0.6793(4) 0.0500(16) Uani 1 1 d . . . . . H01R H 0.955540 0.804875 0.678708 0.060 Uiso 1 1 calc R U . . . C01G C 0.7825(7) 0.78085(16) 0.6810(4) 0.0561(17) Uani 1 1 d . . . . . H01S H 0.734851 0.802611 0.681637 0.067 Uiso 1 1 calc R U . . . C01H C 0.2294(7) 0.73180(15) 0.2312(5) 0.0526(14) Uani 1 1 d . . . . . H01T H 0.144282 0.719091 0.184988 0.063 Uiso 1 1 calc R U . . . C01I C 0.3505(6) 0.71355(13) 0.2969(4) 0.0434(13) Uani 1 1 d . . . . . H01U H 0.347331 0.688081 0.298079 0.052 Uiso 1 1 calc R U . . . 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 0.01090(6) 0.01210(6) 0.01011(6) 0.00004(5) 0.00375(4) -0.00069(6) C1 0.0188(19) 0.0138(18) 0.0175(17) 0.0016(14) 0.0077(15) -0.0047(14) Cl02 0.0127(4) 0.0166(4) 0.0142(4) 0.0008(3) 0.0049(3) 0.0034(3) C2 0.0182(19) 0.022(2) 0.0221(18) -0.0050(15) 0.0113(15) -0.0031(15) Cl03 0.0126(4) 0.0185(4) 0.0157(4) 0.0013(3) 0.0065(3) 0.0034(3) C3 0.0129(18) 0.0169(18) 0.0135(17) 0.0006(14) -0.0011(14) -0.0007(14) N004 0.0109(15) 0.0139(15) 0.0109(13) -0.0001(11) 0.0047(11) -0.0005(11) C4 0.0168(18) 0.0104(16) 0.0146(16) -0.0007(13) 0.0084(14) -0.0026(14) C5 0.0155(19) 0.0188(19) 0.0187(18) -0.0012(14) 0.0067(15) -0.0025(15) C6 0.0175(19) 0.024(2) 0.0173(17) 0.0028(15) 0.0085(15) 0.0027(16) C7 0.0131(18) 0.0150(18) 0.0143(17) 0.0016(13) 0.0068(14) -0.0042(13) C00E 0.019(2) 0.0155(18) 0.0125(17) -0.0004(14) 0.0002(14) 0.0007(15) N9 0.0088(14) 0.0137(15) 0.0120(13) -0.0007(11) 0.0041(11) 0.0010(11) C8 0.0134(18) 0.0138(17) 0.0105(15) -0.0010(13) 0.0054(13) -0.0039(14) C00F 0.0151(18) 0.0161(18) 0.0141(16) -0.0013(14) 0.0053(14) -0.0013(14) C00H 0.0122(17) 0.0140(17) 0.0088(15) -0.0014(13) 0.0028(13) -0.0066(14) C00I 0.031(2) 0.0148(18) 0.0141(17) 0.0000(14) 0.0102(16) 0.0007(16) C00J 0.0150(19) 0.025(2) 0.0200(18) 0.0034(15) 0.0054(15) 0.0015(15) C00K 0.0170(19) 0.0176(19) 0.0215(19) 0.0002(15) 0.0006(15) -0.0023(15) C00L 0.023(2) 0.0169(19) 0.0202(18) 0.0020(14) 0.0135(16) 0.0018(15) C00M 0.0101(17) 0.0229(19) 0.0163(17) -0.0031(14) 0.0037(14) 0.0011(15) C00N 0.0174(19) 0.0162(18) 0.0171(17) -0.0005(14) 0.0053(15) -0.0011(15) C00O 0.0099(17) 0.0140(17) 0.0167(16) -0.0002(13) 0.0077(13) -0.0012(14) C00P 0.0155(18) 0.0143(18) 0.0145(16) 0.0034(13) 0.0067(14) -0.0049(14) C00Q 0.0154(18) 0.026(2) 0.029(2) -0.0039(17) 0.0070(15) 0.0005(17) C00R 0.0160(19) 0.0197(19) 0.0130(17) 0.0026(14) 0.0013(14) -0.0034(15) C00S 0.020(2) 0.0178(18) 0.0189(18) -0.0010(14) 0.0129(15) -0.0005(15) C00T 0.0171(19) 0.0135(18) 0.0174(17) -0.0034(14) 0.0052(14) -0.0059(14) C00U 0.0138(18) 0.0127(17) 0.0162(17) 0.0027(13) 0.0066(14) 0.0028(14) C00V 0.028(2) 0.0146(18) 0.0119(17) 0.0023(14) -0.0006(15) -0.0031(16) C00W 0.0176(19) 0.0185(19) 0.0126(16) 0.0017(14) 0.0054(14) 0.0004(15) C00X 0.0155(18) 0.0118(17) 0.0098(15) 0.0010(13) 0.0013(13) -0.0034(14) C00Y 0.031(2) 0.0193(19) 0.0157(17) -0.0049(15) 0.0104(16) -0.0024(17) C00Z 0.023(2) 0.029(2) 0.030(2) 0.0046(17) 0.0162(17) 0.0076(17) C010 0.014(2) 0.033(2) 0.030(2) -0.0026(17) 0.0103(16) -0.0034(17) C10 0.0060(16) 0.0137(17) 0.0130(16) 0.0017(13) 0.0040(13) 0.0007(13) C011 0.022(2) 0.0182(18) 0.0134(16) -0.0014(14) 0.0089(14) -0.0036(15) C012 0.0135(18) 0.0106(17) 0.0137(16) -0.0008(13) 0.0052(13) -0.0032(13) C013 0.0149(19) 0.0147(19) 0.0198(18) -0.0010(14) 0.0054(15) -0.0033(14) C014 0.022(2) 0.0178(19) 0.0124(17) 0.0027(13) 0.0036(15) -0.0028(15) C015 0.020(2) 0.026(2) 0.029(2) -0.0015(16) 0.0147(17) -0.0013(17) C016 0.024(2) 0.022(2) 0.029(2) -0.0011(16) 0.0122(17) 0.0007(17) C017 0.025(2) 0.019(2) 0.0119(17) -0.0027(14) 0.0066(15) -0.0086(15) C018 0.032(3) 0.044(3) 0.031(2) 0.002(2) 0.0000(19) -0.008(2) C019 0.019(2) 0.020(2) 0.031(2) 0.0003(16) 0.0100(16) 0.0001(16) C01A 0.044(3) 0.028(2) 0.027(2) 0.0021(19) -0.001(2) 0.000(2) C01B 0.053(5) 0.105(8) 0.032(4) 0.000 0.018(4) 0.000 C01C 0.063(4) 0.042(3) 0.030(2) -0.005(2) 0.016(2) 0.006(3) C01D 0.061(4) 0.074(4) 0.034(3) 0.016(3) 0.011(3) 0.015(3) C01E 0.024(4) 0.110(8) 0.021(3) 0.000 0.005(3) 0.000 C01F 0.085(5) 0.029(3) 0.020(2) 0.0006(18) 0.006(2) -0.027(3) C01G 0.073(4) 0.058(4) 0.025(2) -0.002(2) 0.009(3) 0.029(3) C01H 0.065(4) 0.063(3) 0.046(3) 0.004(2) 0.038(3) 0.000(3) C01I 0.069(4) 0.035(3) 0.030(2) -0.002(2) 0.024(2) 0.000(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 C4 Pb01 C00X 135.12(13) . . ? C4 Pb01 C10 111.72(12) . . ? C00X Pb01 C10 112.94(12) . . ? C4 Pb01 Cl03 93.08(10) . . ? C00X Pb01 Cl03 93.48(10) . . ? C10 Pb01 Cl03 86.92(8) . . ? C4 Pb01 Cl02 89.04(9) . . ? C00X Pb01 Cl02 90.70(10) . . ? C10 Pb01 Cl02 84.78(8) . . ? Cl03 Pb01 Cl02 171.63(3) . . ? C00T C1 N9 106.7(3) . . ? C00T C1 H1 126.6 . . ? N9 C1 H1 126.6 . . ? C00F C2 H2A 109.5 . . ? C00F C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C00F C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C014 C3 C013 121.2(3) . . ? C014 C3 H3 119.4 . . ? C013 C3 H3 119.4 . . ? C10 N004 C00T 110.7(3) . . ? C10 N004 C00H 126.2(3) . . ? C00T N004 C00H 122.8(3) . . ? C00U C4 C00O 121.1(3) . . ? C00U C4 Pb01 119.1(2) . . ? C00O C4 Pb01 119.6(2) . . ? C00X C5 C00Y 119.1(4) . . ? C00X C5 H5 120.5 . . ? C00Y C5 H5 120.5 . . ? C7 C6 C00Z 113.3(3) . . ? C7 C6 C010 110.2(3) . . ? C00Z C6 C010 109.7(3) . . ? C7 C6 H6 107.8 . . ? C00Z C6 H6 107.8 . . ? C010 C6 H6 107.8 . . ? C00S C7 C8 116.1(3) . . ? C00S C7 C6 121.0(3) . . ? C8 C7 C6 122.9(3) . . ? C00I C00E C00O 120.4(3) . . ? C00I C00E H00E 119.8 . . ? C00O C00E H00E 119.8 . . ? C10 N9 C1 110.8(3) . . ? C10 N9 C8 126.3(3) . . ? C1 N9 C8 122.7(3) . . ? C7 C8 C00P 124.7(3) . . ? C7 C8 N9 117.8(3) . . ? C00P C8 N9 117.4(3) . . ? C012 C00F C2 113.2(3) . . ? C012 C00F C019 110.0(3) . . ? C2 C00F C019 109.5(3) . . ? C012 C00F H00F 108.0 . . ? C2 C00F H00F 108.0 . . ? C019 C00F H00F 108.0 . . ? C012 C00H C013 124.3(3) . . ? C012 C00H N004 118.1(3) . . ? C013 C00H N004 117.4(3) . . ? C00E C00I C00L 119.9(3) . . ? C00E C00I H00I 120.1 . . ? C00L C00I H00I 120.1 . . ? C00W C00J H00A 109.5 . . ? C00W C00J H00B 109.5 . . ? H00A C00J H00B 109.5 . . ? C00W C00J H00C 109.5 . . ? H00A C00J H00C 109.5 . . ? H00B C00J H00C 109.5 . . ? C00V C00K C00N 120.5(4) . . ? C00V C00K H00K 119.8 . . ? C00N C00K H00K 119.8 . . ? C00I C00L C00U 120.4(3) . . ? C00I C00L H00L 119.8 . . ? C00U C00L H00L 119.8 . . ? C013 C00M C00Q 112.6(3) . . ? C013 C00M C015 110.6(3) . . ? C00Q C00M C015 109.9(3) . . ? C013 C00M H00M 107.8 . . ? C00Q C00M H00M 107.8 . . ? C015 C00M H00M 107.8 . . ? C00X C00N C00K 119.0(4) . . ? C00X C00N H00N 120.5 . . ? C00K C00N H00N 120.5 . . ? C00E C00O C4 119.0(3) . . ? C00E C00O H00O 120.5 . . ? C4 C00O H00O 120.5 . . ? C00R C00P C8 115.9(3) . . ? C00R C00P C00W 120.9(3) . . ? C8 C00P C00W 123.1(3) . . ? C00M C00Q H00D 109.5 . . ? C00M C00Q H00G 109.5 . . ? H00D C00Q H00G 109.5 . . ? C00M C00Q H00H 109.5 . . ? H00D C00Q H00H 109.5 . . ? H00G C00Q H00H 109.5 . . ? C017 C00R C00P 121.3(3) . . ? C017 C00R H00R 119.3 . . ? C00P C00R H00R 119.3 . . ? C017 C00S C7 121.0(3) . . ? C017 C00S H00S 119.5 . . ? C7 C00S H00S 119.5 . . ? C1 C00T N004 106.9(3) . . ? C1 C00T H00T 126.5 . . ? N004 C00T H00T 126.5 . . ? C4 C00U C00L 119.2(3) . . ? C4 C00U H00U 120.4 . . ? C00L C00U H00U 120.4 . . ? C00K C00V C00Y 120.0(3) . . ? C00K C00V H00V 120.0 . . ? C00Y C00V H00V 120.0 . . ? C00P C00W C00J 113.0(3) . . ? C00P C00W C016 110.4(3) . . ? C00J C00W C016 109.6(3) . . ? C00P C00W H00W 107.9 . . ? C00J C00W H00W 107.9 . . ? C016 C00W H00W 107.9 . . ? C5 C00X C00N 121.4(3) . . ? C5 C00X Pb01 119.6(3) . . ? C00N C00X Pb01 119.0(3) . . ? C00V C00Y C5 120.0(4) . . ? C00V C00Y H00Y 120.0 . . ? C5 C00Y H00Y 120.0 . . ? C6 C00Z H00J 109.5 . . ? C6 C00Z H00P 109.5 . . ? H00J C00Z H00P 109.5 . . ? C6 C00Z H00Q 109.5 . . ? H00J C00Z H00Q 109.5 . . ? H00P C00Z H00Q 109.5 . . ? C6 C010 H01A 109.5 . . ? C6 C010 H01B 109.5 . . ? H01A C010 H01B 109.5 . . ? C6 C010 H01C 109.5 . . ? H01A C010 H01C 109.5 . . ? H01B C010 H01C 109.5 . . ? N9 C10 N004 104.9(3) . . ? N9 C10 Pb01 126.9(2) . . ? N004 C10 Pb01 127.7(2) . . ? C014 C011 C012 120.6(3) . . ? C014 C011 H011 119.7 . . ? C012 C011 H011 119.7 . . ? C011 C012 C00H 116.7(3) . . ? C011 C012 C00F 121.0(3) . . ? C00H C012 C00F 122.2(3) . . ? C3 C013 C00H 115.9(3) . . ? C3 C013 C00M 121.4(3) . . ? C00H C013 C00M 122.7(3) . . ? C3 C014 C011 121.2(3) . . ? C3 C014 H014 119.4 . . ? C011 C014 H014 119.4 . . ? C00M C015 H01D 109.5 . . ? C00M C015 H01E 109.5 . . ? H01D C015 H01E 109.5 . . ? C00M C015 H01F 109.5 . . ? H01D C015 H01F 109.5 . . ? H01E C015 H01F 109.5 . . ? C00W C016 H01G 109.5 . . ? C00W C016 H01H 109.5 . . ? H01G C016 H01H 109.5 . . ? C00W C016 H01I 109.5 . . ? H01G C016 H01I 109.5 . . ? H01H C016 H01I 109.5 . . ? C00R C017 C00S 121.0(3) . . ? C00R C017 H017 119.5 . . ? C00S C017 H017 119.5 . . ? C01A C018 C018 119.7(3) . 4_575 ? C01A C018 H018 120.2 . . ? C018 C018 H018 120.2 4_575 . ? C00F C019 H01J 109.5 . . ? C00F C019 H01K 109.5 . . ? H01J C019 H01K 109.5 . . ? C00F C019 H01L 109.5 . . ? H01J C019 H01L 109.5 . . ? H01K C019 H01L 109.5 . . ? C01C C01A C018 121.0(4) . . ? C01C C01A H01M 119.5 . . ? C018 C01A H01M 119.5 . . ? C01G C01B C01G 120.6(9) . 4_575 ? C01G C01B H01N 119.7 . . ? C01G C01B H01N 119.7 4_575 . ? C01A C01C C01C 119.3(3) . 4_575 ? C01A C01C H01O 120.4 . . ? C01C C01C H01O 120.4 4_575 . ? C01I C01D C01D 117.4(3) . 4_575 ? C01I C01D H01P 121.3 . . ? C01D C01D H01P 121.3 4_575 . ? C01F C01E C01F 117.7(7) . 4_575 ? C01F C01E H01Q 121.2 . . ? C01F C01E H01Q 121.2 4_575 . ? C01G C01F C01E 118.7(5) . . ? C01G C01F H01R 120.6 . . ? C01E C01F H01R 120.6 . . ? C01B C01G C01F 122.1(6) . . ? C01B C01G H01S 118.9 . . ? C01F C01G H01S 118.9 . . ? C01I C01H C01H 120.2(3) . 4_575 ? C01I C01H H01T 119.9 . . ? C01H C01H H01T 119.9 4_575 . ? C01H C01I C01D 122.3(5) . . ? C01H C01I H01U 118.8 . . ? C01D C01I H01U 118.8 . . ? 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 C4 2.204(3) . ? Pb01 C00X 2.212(3) . ? Pb01 C10 2.320(3) . ? Pb01 Cl03 2.6324(9) . ? Pb01 Cl02 2.6987(8) . ? C1 C00T 1.353(5) . ? C1 N9 1.382(4) . ? C1 H1 0.9500 . ? C2 C00F 1.526(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C014 1.382(5) . ? C3 C013 1.397(5) . ? C3 H3 0.9500 . ? N004 C10 1.359(4) . ? N004 C00T 1.381(4) . ? N004 C00H 1.460(4) . ? C4 C00U 1.387(5) . ? C4 C00O 1.398(5) . ? C5 C00X 1.384(5) . ? C5 C00Y 1.397(5) . ? C5 H5 0.9500 . ? C6 C7 1.523(5) . ? C6 C00Z 1.534(5) . ? C6 C010 1.537(5) . ? C6 H6 1.0000 . ? C7 C00S 1.401(5) . ? C7 C8 1.402(5) . ? C00E C00I 1.391(6) . ? C00E C00O 1.391(5) . ? C00E H00E 0.9500 . ? N9 C10 1.356(4) . ? N9 C8 1.461(4) . ? C8 C00P 1.406(5) . ? C00F C012 1.521(5) . ? C00F C019 1.536(5) . ? C00F H00F 1.0000 . ? C00H C012 1.398(5) . ? C00H C013 1.412(5) . ? C00I C00L 1.393(5) . ? C00I H00I 0.9500 . ? C00J C00W 1.526(5) . ? C00J H00A 0.9800 . ? C00J H00B 0.9800 . ? C00J H00C 0.9800 . ? C00K C00V 1.383(6) . ? C00K C00N 1.392(5) . ? C00K H00K 0.9500 . ? C00L C00U 1.394(5) . ? C00L H00L 0.9500 . ? C00M C013 1.519(5) . ? C00M C00Q 1.527(5) . ? C00M C015 1.531(5) . ? C00M H00M 1.0000 . ? C00N C00X 1.385(5) . ? C00N H00N 0.9500 . ? C00O H00O 0.9500 . ? C00P C00R 1.401(5) . ? C00P C00W 1.515(5) . ? C00Q H00D 0.9800 . ? C00Q H00G 0.9800 . ? C00Q H00H 0.9800 . ? C00R C017 1.379(5) . ? C00R H00R 0.9500 . ? C00S C017 1.385(5) . ? C00S H00S 0.9500 . ? C00T H00T 0.9500 . ? C00U H00U 0.9500 . ? C00V C00Y 1.392(6) . ? C00V H00V 0.9500 . ? C00W C016 1.534(5) . ? C00W H00W 1.0000 . ? C00Y H00Y 0.9500 . ? C00Z H00J 0.9800 . ? C00Z H00P 0.9800 . ? C00Z H00Q 0.9800 . ? C010 H01A 0.9800 . ? C010 H01B 0.9800 . ? C010 H01C 0.9800 . ? C011 C014 1.384(5) . ? C011 C012 1.397(5) . ? C011 H011 0.9500 . ? C014 H014 0.9500 . ? C015 H01D 0.9800 . ? C015 H01E 0.9800 . ? C015 H01F 0.9800 . ? C016 H01G 0.9800 . ? C016 H01H 0.9800 . ? C016 H01I 0.9800 . ? C017 H017 0.9500 . ? C018 C01A 1.377(7) . ? C018 C018 1.381(10) 4_575 ? C018 H018 0.9500 . ? C019 H01J 0.9800 . ? C019 H01K 0.9800 . ? C019 H01L 0.9800 . ? C01A C01C 1.369(7) . ? C01A H01M 0.9500 . ? C01B C01G 1.324(8) . ? C01B C01G 1.324(8) 4_575 ? C01B H01N 0.9500 . ? C01C C01C 1.403(10) 4_575 ? C01C H01O 0.9500 . ? C01D C01I 1.361(8) . ? C01D C01D 1.463(12) 4_575 ? C01D H01P 0.9500 . ? C01E C01F 1.412(7) . ? C01E C01F 1.412(7) 4_575 ? C01E H01Q 0.9500 . ? C01F C01G 1.351(9) . ? C01F H01R 0.9500 . ? C01G H01S 0.9500 . ? C01H C01I 1.354(7) . ? C01H C01H 1.356(11) 4_575 ? C01H H01T 0.9500 . ? C01I H01U 0.9500 . ?