# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_absolute_configuration rm _chemical_melting_point ? _chemical_formula_moiety 'C39 H59 N5 O Pb2 S4, 4(F6 P), 2(C2 H3 N)' _chemical_formula_sum 'C43 H65 F24 N7 O P4 Pb2 S4' _chemical_formula_weight 1818.52 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 37.896(6) _cell_length_b 12.929(2) _cell_length_c 12.973(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.194(10) _cell_angle_gamma 90.00 _cell_volume 6330.3(18) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7242 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.0 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3536 _exptl_absorpt_coefficient_mu 5.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1325 _exptl_absorpt_correction_T_max 0.3230 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication to Rigaku Company, Tokyo, Japan.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method /w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26276 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11005 _reflns_number_gt 10436 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1020P)^2^+368.5409P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00134(13) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881, with 5122 Friedel pairs' _refine_ls_abs_structure_Flack 0.384(13) _refine_ls_number_reflns 11005 _refine_ls_number_parameters 506 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0962 _refine_ls_wR_factor_ref 0.2359 _refine_ls_wR_factor_gt 0.2331 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.5000 0.09590(7) 2.0000 0.0346(3) Uani 1 2 d S . . Pb2 Pb 0.501981(19) 0.33984(6) 1.79814(7) 0.0383(3) Uani 1 1 d . . . Pb3 Pb 0.47956(4) 0.47817(12) 1.55230(11) 0.0328(4) Uani 0.50 1 d P . . S1 S 0.54578(13) 0.2517(4) 2.0453(4) 0.0316(10) Uani 1 1 d . . . S2 S 0.51237(15) 0.1298(4) 1.7763(5) 0.0441(14) Uani 1 1 d . . . S3 S 0.53567(14) 0.3412(5) 1.6102(4) 0.0412(11) Uani 1 1 d . . . S4 S 0.44614(13) 0.3200(5) 1.6611(4) 0.0406(13) Uani 1 1 d . . . P1 P 0.75619(15) 0.7765(5) 1.0016(4) 0.0375(12) Uani 1 1 d . . . P2 P 0.40286(19) 0.8216(6) 1.0285(5) 0.0563(17) Uani 1 1 d . . . P3 P 0.40084(17) 0.7589(5) 1.5420(5) 0.0477(15) Uani 1 1 d . . . P4 P 0.24446(13) 0.8187(4) 0.5034(4) 0.0330(12) Uani 1 1 d . . . F1 F 0.7140(6) 0.7754(17) 0.9807(17) 0.0952(13) Uani 1 1 d . . . F2 F 0.7594(6) 0.7844(17) 0.8777(17) 0.0952(13) Uani 1 1 d . . . F3 F 0.7978(6) 0.7771(17) 1.0275(17) 0.0952(13) Uani 1 1 d . . . F4 F 0.7528(6) 0.7693(17) 1.1254(16) 0.0952(13) Uani 1 1 d . . . F5 F 0.7570(6) 0.6561(18) 0.9917(17) 0.0952(13) Uani 1 1 d . . . F6 F 0.7577(7) 0.8994(18) 1.0170(18) 0.0952(13) Uani 1 1 d . . . F7 F 0.4389(6) 0.7697(17) 1.0176(16) 0.0952(13) Uani 1 1 d . . . F8 F 0.4116(6) 0.8056(17) 1.1501(16) 0.0952(13) Uani 1 1 d . . . F9 F 0.3683(6) 0.8768(17) 1.0550(17) 0.0952(13) Uani 1 1 d . . . F10 F 0.3952(6) 0.8196(18) 0.9077(16) 0.0952(13) Uani 1 1 d . . . F11 F 0.4228(6) 0.9308(18) 1.0341(17) 0.0952(13) Uani 1 1 d . . . F12 F 0.3838(6) 0.7092(18) 1.0322(16) 0.0952(13) Uani 1 1 d . . . F13 F 0.3612(6) 0.7468(19) 1.5744(16) 0.0952(13) Uani 1 1 d . . . F14 F 0.3982(7) 0.8774(18) 1.5535(17) 0.0952(13) Uani 1 1 d . . . F15 F 0.3890(6) 0.7553(18) 1.4218(16) 0.0952(13) Uani 1 1 d . . . F16 F 0.4398(6) 0.7842(17) 1.5161(17) 0.0952(13) Uani 1 1 d . . . F17 F 0.4112(6) 0.7516(18) 1.6605(16) 0.0952(13) Uani 1 1 d . . . F18 F 0.4009(6) 0.6365(17) 1.5268(17) 0.0952(13) Uani 1 1 d . . . F19 F 0.2862(6) 0.8141(18) 0.5023(16) 0.0952(13) Uani 1 1 d . . . F20 F 0.2413(6) 0.8132(17) 0.3815(16) 0.0952(13) Uani 1 1 d . . . F21 F 0.2428(6) 0.7000(18) 0.5107(17) 0.0952(13) Uani 1 1 d . . . F22 F 0.2024(6) 0.825(2) 0.5052(15) 0.0952(13) Uani 1 1 d . . . F23 F 0.2486(6) 0.8222(18) 0.6278(15) 0.0952(13) Uani 1 1 d . . . F24 F 0.2476(6) 0.9416(18) 0.4989(17) 0.0952(13) Uani 1 1 d . . . O1 O 0.4971(7) 0.5672(14) 1.790(2) 0.089(5) Uani 1 1 d . . . N1 N 0.6754(4) 0.0253(13) 2.2413(12) 0.029(3) Uani 1 1 d . . . N2 N 0.6691(5) 0.0529(15) 1.7348(15) 0.049(5) Uani 1 1 d D . . N3 N 0.6727(5) 0.5712(15) 1.7232(14) 0.041(4) Uani 1 1 d . . . N4 N 0.3200(4) 0.5654(13) 1.7818(14) 0.035(4) Uani 1 1 d D . . N5 N 0.1263(12) 0.957(3) 0.960(4) 0.136(18) Uani 1 1 d . . . N6 N 0.6215(6) 0.1228(18) 1.4796(15) 0.053(6) Uani 1 1 d . . . N7 N 0.4959(8) 0.7477(18) 1.765(3) 0.089(5) Uani 1 1 d . . . C1 C 0.5834(5) 0.1830(16) 2.0993(15) 0.029(2) Uani 1 1 d . . . C2 C 0.5798(5) 0.1052(16) 2.1687(14) 0.029(2) Uani 1 1 d . . . H2 H 0.5566 0.0891 2.1862 0.035 Uiso 1 1 calc R . . C3 C 0.6081(5) 0.0477(16) 2.2155(15) 0.029(2) Uani 1 1 d . . . H3 H 0.6042 -0.0083 2.2605 0.035 Uiso 1 1 calc R . . C4 C 0.6434(5) 0.0757(16) 2.1937(15) 0.032(4) Uani 1 1 d . . . C5 C 0.6466(5) 0.1602(16) 2.1269(15) 0.029(2) Uani 1 1 d . . . H5 H 0.6696 0.1829 2.1138 0.035 Uiso 1 1 calc R . . C6 C 0.6178(5) 0.2110(16) 2.0801(15) 0.029(2) Uani 1 1 d . . . H6 H 0.6212 0.2662 2.0338 0.035 Uiso 1 1 calc R . . C7 C 0.6661(7) -0.061(2) 2.311(2) 0.0560(19) Uani 1 1 d . . . H7A H 0.6515 -0.0348 2.3633 0.084 Uiso 1 1 calc R . . H7B H 0.6878 -0.0920 2.3443 0.084 Uiso 1 1 calc R . . H7C H 0.6528 -0.1144 2.2693 0.084 Uiso 1 1 calc R . . C8 C 0.6952(7) -0.019(2) 2.156(2) 0.0560(19) Uani 1 1 d . . . H8A H 0.6791 -0.0611 2.1104 0.084 Uiso 1 1 calc R . . H8B H 0.7149 -0.0613 2.1860 0.084 Uiso 1 1 calc R . . H8C H 0.7045 0.0380 2.1162 0.084 Uiso 1 1 calc R . . C9 C 0.6986(7) 0.101(3) 2.311(2) 0.0560(19) Uani 1 1 d . . . H9A H 0.7056 0.1592 2.2687 0.084 Uiso 1 1 calc R . . H9B H 0.7199 0.0647 2.3404 0.084 Uiso 1 1 calc R . . H9C H 0.6851 0.1263 2.3662 0.084 Uiso 1 1 calc R . . C10 C 0.5575(5) 0.1123(16) 1.7687(14) 0.029(2) Uani 1 1 d . . . C11 C 0.5682(5) 0.0223(16) 1.7220(18) 0.035(2) Uani 1 1 d . . . H11 H 0.5509 -0.0277 1.6989 0.042 Uiso 1 1 calc R . . C12 C 0.6034(5) 0.0037(16) 1.7082(18) 0.035(2) Uani 1 1 d . . . H12 H 0.6096 -0.0563 1.6717 0.042 Uiso 1 1 calc R . . C13 C 0.6298(5) 0.0711(16) 1.7469(16) 0.031(4) Uani 1 1 d . . . C14 C 0.6201(5) 0.1595(16) 1.7982(18) 0.035(2) Uani 1 1 d . . . H14 H 0.6379 0.2048 1.8278 0.042 Uiso 1 1 calc R . . C15 C 0.5855(5) 0.1822(16) 1.8069(18) 0.035(2) Uani 1 1 d . . . H15 H 0.5796 0.2453 1.8386 0.042 Uiso 1 1 calc R . . C16 C 0.6734(7) -0.0373(19) 1.6645(19) 0.0560(19) Uani 1 1 d D . . H16A H 0.6608 -0.0973 1.6893 0.084 Uiso 1 1 calc R . . H16B H 0.6986 -0.0538 1.6639 0.084 Uiso 1 1 calc R . . H16C H 0.6635 -0.0198 1.5942 0.084 Uiso 1 1 calc R . . C17 C 0.6881(7) 0.144(2) 1.697(2) 0.0560(19) Uani 1 1 d . . . H17A H 0.7095 0.1211 1.6662 0.084 Uiso 1 1 calc R . . H17B H 0.6947 0.1912 1.7545 0.084 Uiso 1 1 calc R . . H17C H 0.6726 0.1806 1.6439 0.084 Uiso 1 1 calc R . . C18 C 0.6878(7) 0.020(2) 1.842(2) 0.0560(19) Uani 1 1 d . . . H18A H 0.6959 -0.0520 1.8385 0.084 Uiso 1 1 calc R . . H18B H 0.6710 0.0255 1.8951 0.084 Uiso 1 1 calc R . . H18C H 0.7081 0.0650 1.8604 0.084 Uiso 1 1 calc R . . C19 C 0.5747(5) 0.4120(16) 1.6429(15) 0.029(2) Uani 1 1 d . . . C20 C 0.5752(5) 0.5071(18) 1.6979(16) 0.036(5) Uani 1 1 d . . . H20 H 0.5537 0.5358 1.7179 0.043 Uiso 1 1 calc R . . C21 C 0.6063(5) 0.5567(18) 1.7216(17) 0.037(5) Uani 1 1 d . . . H21 H 0.6064 0.6202 1.7584 0.045 Uiso 1 1 calc R . . C22 C 0.6385(5) 0.5163(16) 1.6929(15) 0.030(4) Uani 1 1 d . . . C23 C 0.6386(6) 0.4262(17) 1.6370(18) 0.041(5) Uani 1 1 d . . . H23 H 0.6601 0.3991 1.6160 0.049 Uiso 1 1 calc R . . C24 C 0.6074(6) 0.3760(19) 1.612(2) 0.051(6) Uani 1 1 d . . . H24 H 0.6076 0.3143 1.5724 0.061 Uiso 1 1 calc R . . C25 C 0.6672(7) 0.671(2) 1.780(2) 0.0560(19) Uani 1 1 d . . . H25A H 0.6540 0.6563 1.8402 0.084 Uiso 1 1 calc R . . H25B H 0.6538 0.7192 1.7339 0.084 Uiso 1 1 calc R . . H25C H 0.6902 0.7008 1.8038 0.084 Uiso 1 1 calc R . . C26 C 0.6902(7) 0.597(3) 1.620(2) 0.0560(19) Uani 1 1 d . . . H26A H 0.7138 0.6268 1.6371 0.084 Uiso 1 1 calc R . . H26B H 0.6753 0.6464 1.5788 0.084 Uiso 1 1 calc R . . H26C H 0.6924 0.5332 1.5800 0.084 Uiso 1 1 calc R . . C27 C 0.6955(7) 0.499(2) 1.793(2) 0.0560(19) Uani 1 1 d . . . H27A H 0.6804 0.4503 1.8260 0.084 Uiso 1 1 calc R . . H27B H 0.7094 0.5397 1.8461 0.084 Uiso 1 1 calc R . . H27C H 0.7116 0.4611 1.7516 0.084 Uiso 1 1 calc R . . C28 C 0.4098(5) 0.3894(16) 1.7028(15) 0.029(2) Uani 1 1 d . . . C29 C 0.4145(5) 0.4857(17) 1.7593(19) 0.041(5) Uani 1 1 d . . . H29 H 0.4376 0.5099 1.7818 0.049 Uiso 1 1 calc R . . C30 C 0.3859(8) 0.540(2) 1.780(2) 0.058(7) Uani 1 1 d . . . H30 H 0.3891 0.6057 1.8122 0.070 Uiso 1 1 calc R . . C31 C 0.3520(5) 0.5046(16) 1.7545(15) 0.031(4) Uani 1 1 d . . . C32 C 0.3481(6) 0.4148(19) 1.701(2) 0.047(6) Uani 1 1 d . . . H32 H 0.3249 0.3907 1.6791 0.056 Uiso 1 1 calc R . . C33 C 0.3773(5) 0.3568(18) 1.6778(16) 0.038(5) Uani 1 1 d . . . H33 H 0.3737 0.2925 1.6431 0.045 Uiso 1 1 calc R . . C34 C 0.3307(7) 0.6669(17) 1.832(2) 0.0560(19) Uani 1 1 d D . . H34A H 0.3452 0.7058 1.7867 0.084 Uiso 1 1 calc R . . H34B H 0.3443 0.6541 1.8985 0.084 Uiso 1 1 calc R . . H34C H 0.3094 0.7069 1.8433 0.084 Uiso 1 1 calc R . . C35 C 0.3006(7) 0.600(3) 1.678(2) 0.0560(19) Uani 1 1 d . . . H35A H 0.2864 0.5422 1.6478 0.084 Uiso 1 1 calc R . . H35B H 0.3179 0.6208 1.6306 0.084 Uiso 1 1 calc R . . H35C H 0.2850 0.6583 1.6900 0.084 Uiso 1 1 calc R . . C36 C 0.2991(7) 0.508(2) 1.842(2) 0.0560(19) Uani 1 1 d . . . H36A H 0.3141 0.4733 1.8976 0.084 Uiso 1 1 calc R . . H36B H 0.2860 0.4555 1.7995 0.084 Uiso 1 1 calc R . . H36C H 0.2822 0.5534 1.8732 0.084 Uiso 1 1 calc R . . C37 C 0.1009(8) 0.979(2) 0.964(2) 0.061(7) Uani 1 1 d D . . C38 C 0.0650(8) 1.023(2) 0.972(3) 0.088(13) Uani 1 1 d D . . H38A H 0.0571 1.0060 1.0398 0.133 Uiso 1 1 calc R . . H38B H 0.0485 0.9928 0.9175 0.133 Uiso 1 1 calc R . . H38C H 0.0658 1.0978 0.9634 0.133 Uiso 1 1 calc R . . C39 C 0.5914(8) 0.104(2) 1.4668(17) 0.049(6) Uani 1 1 d . . . C40 C 0.5538(7) 0.086(2) 1.471(2) 0.070(9) Uani 1 1 d . . . H40A H 0.5496 0.0115 1.4780 0.105 Uiso 1 1 calc R . . H40B H 0.5408 0.1110 1.4068 0.105 Uiso 1 1 calc R . . H40C H 0.5455 0.1226 1.5301 0.105 Uiso 1 1 calc R . . C41 C 0.5184(10) 0.753(2) 1.673(3) 0.089(5) Uani 1 1 d . . . H41A H 0.5427 0.7725 1.6976 0.133 Uiso 1 1 calc R . . H41B H 0.5085 0.8056 1.6237 0.133 Uiso 1 1 calc R . . H41C H 0.5184 0.6859 1.6387 0.133 Uiso 1 1 calc R . . C42 C 0.4866(10) 0.853(2) 1.812(3) 0.089(5) Uani 1 1 d . . . H42A H 0.4839 0.8445 1.8855 0.133 Uiso 1 1 calc R . . H42B H 0.4644 0.8789 1.7763 0.133 Uiso 1 1 calc R . . H42C H 0.5057 0.9026 1.8025 0.133 Uiso 1 1 calc R . . C43 C 0.4889(10) 0.672(2) 1.795(3) 0.089(5) Uani 1 1 d . . . H43 H 0.4709 0.6815 1.8408 0.107 Uiso 1 1 calc R . . 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 0.0305(6) 0.0228(5) 0.0488(7) 0.000 -0.0050(5) 0.000 Pb2 0.0272(4) 0.0296(4) 0.0589(5) -0.0089(4) 0.0084(3) -0.0024(3) Pb3 0.0326(8) 0.0315(8) 0.0339(7) -0.0021(6) -0.0002(6) -0.0008(6) S1 0.023(2) 0.034(3) 0.038(3) 0.001(2) -0.001(2) -0.0003(19) S2 0.029(3) 0.038(3) 0.070(4) 0.019(3) 0.029(3) 0.010(2) S3 0.047(3) 0.034(2) 0.041(3) 0.003(2) -0.008(2) -0.009(3) S4 0.030(2) 0.049(4) 0.044(3) -0.005(2) 0.010(2) 0.002(2) P1 0.036(3) 0.037(3) 0.042(3) 0.000(2) 0.015(2) -0.002(2) P2 0.054(4) 0.057(5) 0.056(4) 0.003(3) -0.004(3) 0.004(3) P3 0.037(3) 0.048(4) 0.058(4) 0.001(3) 0.005(3) -0.002(3) P4 0.029(3) 0.034(3) 0.035(3) -0.004(2) 0.000(2) 0.001(2) F1 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F2 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F3 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F4 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F5 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F6 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F7 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F8 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F9 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F10 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F11 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F12 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F13 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F14 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F15 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F16 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F17 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F18 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F19 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F20 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F21 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F22 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F23 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) F24 0.106(3) 0.094(3) 0.086(3) -0.005(2) 0.014(2) -0.008(3) O1 0.096(10) 0.025(6) 0.153(13) -0.008(6) 0.054(9) 0.000(6) N1 0.011(7) 0.040(9) 0.035(9) -0.005(7) 0.001(6) 0.004(6) N2 0.032(10) 0.057(12) 0.062(13) 0.033(10) 0.027(9) 0.016(9) N3 0.034(10) 0.040(11) 0.046(10) 0.006(8) -0.007(8) -0.009(8) N4 0.010(7) 0.044(10) 0.052(10) -0.007(8) 0.004(7) -0.007(7) N5 0.14(4) 0.09(3) 0.19(4) 0.07(3) 0.11(3) 0.02(3) N6 0.045(13) 0.070(16) 0.044(11) 0.014(10) 0.000(9) 0.035(11) N7 0.096(10) 0.025(6) 0.153(13) -0.008(6) 0.054(9) 0.000(6) C1 0.024(5) 0.037(5) 0.028(4) 0.003(4) 0.008(4) 0.003(4) C2 0.014(4) 0.040(5) 0.032(5) 0.006(4) 0.000(4) -0.001(4) C3 0.014(4) 0.040(5) 0.032(5) 0.006(4) 0.000(4) -0.001(4) C4 0.025(9) 0.040(12) 0.033(10) -0.002(8) 0.005(8) -0.007(8) C5 0.014(4) 0.040(5) 0.032(5) 0.006(4) 0.000(4) -0.001(4) C6 0.014(4) 0.040(5) 0.032(5) 0.006(4) 0.000(4) -0.001(4) C7 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C8 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C9 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C10 0.024(5) 0.037(5) 0.028(4) 0.003(4) 0.008(4) 0.003(4) C11 0.016(5) 0.032(5) 0.058(7) -0.010(5) 0.005(4) -0.001(4) C12 0.016(5) 0.032(5) 0.058(7) -0.010(5) 0.005(4) -0.001(4) C13 0.015(9) 0.038(12) 0.039(11) 0.006(8) -0.002(7) 0.010(8) C14 0.016(5) 0.032(5) 0.058(7) -0.010(5) 0.005(4) -0.001(4) C15 0.016(5) 0.032(5) 0.058(7) -0.010(5) 0.005(4) -0.001(4) C16 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C17 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C18 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C19 0.024(5) 0.037(5) 0.028(4) 0.003(4) 0.008(4) 0.003(4) C20 0.017(9) 0.049(13) 0.041(11) 0.001(9) -0.006(8) -0.002(8) C21 0.020(10) 0.045(12) 0.048(12) -0.008(10) 0.009(9) 0.002(8) C22 0.012(9) 0.046(12) 0.030(10) -0.007(8) -0.005(7) -0.006(8) C23 0.029(11) 0.041(12) 0.055(13) -0.015(10) 0.022(10) 0.000(9) C24 0.027(11) 0.037(12) 0.089(19) 0.001(12) 0.004(12) 0.010(9) C25 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C26 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C27 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C28 0.024(5) 0.037(5) 0.028(4) 0.003(4) 0.008(4) 0.003(4) C29 0.026(10) 0.034(11) 0.062(14) -0.022(10) -0.004(9) 0.000(9) C30 0.074(19) 0.038(13) 0.069(17) -0.021(12) 0.040(15) -0.012(13) C31 0.031(10) 0.036(11) 0.026(9) 0.006(8) -0.006(8) 0.003(8) C32 0.023(11) 0.047(13) 0.067(15) -0.008(11) -0.019(10) 0.008(9) C33 0.023(9) 0.049(14) 0.039(11) -0.018(10) -0.004(8) 0.012(9) C34 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C35 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C36 0.044(4) 0.067(5) 0.057(4) 0.005(4) 0.006(3) 0.002(4) C37 0.07(2) 0.051(16) 0.063(16) -0.007(13) 0.034(15) -0.006(15) C38 0.14(3) 0.061(19) 0.062(18) 0.024(15) -0.01(2) -0.06(2) C39 0.069(18) 0.045(14) 0.035(11) 0.008(10) 0.010(11) 0.028(13) C40 0.047(14) 0.065(18) 0.09(2) 0.046(17) -0.041(14) 0.001(14) C41 0.096(10) 0.025(6) 0.153(13) -0.008(6) 0.054(9) 0.000(6) C42 0.096(10) 0.025(6) 0.153(13) -0.008(6) 0.054(9) 0.000(6) C43 0.096(10) 0.025(6) 0.153(13) -0.008(6) 0.054(9) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 S1 2.688(5) . yes Pb1 S1 2.688(5) 2_659 yes Pb1 S2 3.013(6) 2_659 yes Pb1 S2 3.013(6) . yes Pb2 S4 2.650(6) . yes Pb2 S2 2.763(6) . yes Pb2 S3 2.852(6) . yes Pb2 S1 3.061(5) 2_659 yes Pb2 Pb3 3.6881(18) . yes Pb3 S3 2.774(6) 2_658 yes Pb3 S3 2.816(6) . yes Pb3 S4 2.846(6) . yes S1 C1 1.77(2) . yes S1 Pb2 3.061(5) 2_659 yes S2 C10 1.738(19) . yes S3 C19 1.76(2) . yes S3 Pb3 2.774(6) 2_658 yes S4 C28 1.77(2) . yes P1 F5 1.56(2) . no P1 F3 1.58(2) . no P1 F1 1.60(2) . no P1 F6 1.60(2) . no P1 F4 1.62(2) . no P1 F2 1.63(2) . no P2 F7 1.54(2) . no P2 F9 1.56(2) . no P2 F10 1.57(2) . no P2 F8 1.60(2) . no P2 F11 1.60(2) . no P2 F12 1.62(2) . no P3 F14 1.54(2) . no P3 F17 1.55(2) . no P3 F16 1.58(2) . no P3 F15 1.58(2) . no P3 F18 1.59(2) . no P3 F13 1.60(2) . no P4 F21 1.54(2) . no P4 F20 1.58(2) . no P4 F19 1.58(2) . no P4 F24 1.59(2) . no P4 F22 1.60(2) . no P4 F23 1.61(2) . no O1 C43 1.40(3) . no N1 C4 1.47(3) . no N1 C7 1.50(3) . no N1 C8 1.50(3) . no N1 C9 1.54(3) . no N2 C17 1.49(3) . no N2 C16 1.498(18) . no N2 C13 1.53(2) . no N2 C18 1.56(3) . no N3 C22 1.50(2) . no N3 C25 1.51(3) . no N3 C27 1.51(3) . no N3 C26 1.58(3) . no N4 C36 1.39(3) . no N4 C34 1.503(18) . no N4 C31 1.51(3) . no N4 C35 1.54(3) . no N5 C37 1.01(4) . no N6 C39 1.16(3) . no N7 C43 1.09(4) . no N7 C41 1.53(5) . no N7 C42 1.55(4) . no C1 C2 1.37(3) . no C1 C6 1.40(3) . no C2 C3 1.40(3) . no C2 H2 0.9500 . no C3 C4 1.44(3) . no C3 H3 0.9500 . no C4 C5 1.41(3) . no C5 C6 1.37(3) . no C5 H5 0.9500 . no C6 H6 0.9500 . no C7 H7A 0.9800 . no C7 H7B 0.9800 . no C7 H7C 0.9800 . no C8 H8A 0.9800 . no C8 H8B 0.9800 . no C8 H8C 0.9800 . no C9 H9A 0.9800 . no C9 H9B 0.9800 . no C9 H9C 0.9800 . no C10 C11 1.39(3) . no C10 C15 1.45(3) . no C11 C12 1.38(3) . no C11 H11 0.9500 . no C12 C13 1.39(3) . no C12 H12 0.9500 . no C13 C14 1.39(3) . no C14 C15 1.36(3) . no C14 H14 0.9500 . no C15 H15 0.9500 . no C16 H16A 0.9800 . no C16 H16B 0.9800 . no C16 H16C 0.9800 . no C17 H17A 0.9800 . no C17 H17B 0.9800 . no C17 H17C 0.9800 . no C18 H18A 0.9800 . no C18 H18B 0.9800 . no C18 H18C 0.9800 . no C19 C24 1.41(3) . no C19 C20 1.42(3) . no C20 C21 1.35(3) . no C20 H20 0.9500 . no C21 C22 1.41(3) . no C21 H21 0.9500 . no C22 C23 1.37(3) . no C23 C24 1.36(3) . no C23 H23 0.9500 . no C24 H24 0.9500 . no C25 H25A 0.9800 . no C25 H25B 0.9800 . no C25 H25C 0.9800 . no C26 H26A 0.9800 . no C26 H26B 0.9800 . no C26 H26C 0.9800 . no C27 H27A 0.9800 . no C27 H27B 0.9800 . no C27 H27C 0.9800 . no C28 C33 1.31(3) . no C28 C29 1.45(3) . no C29 C30 1.34(3) . no C29 H29 0.9500 . no C30 C31 1.37(4) . no C30 H30 0.9500 . no C31 C32 1.35(3) . no C32 C33 1.39(3) . no C32 H32 0.9500 . no C33 H33 0.9500 . no C34 H34A 0.9800 . no C34 H34B 0.9800 . no C34 H34C 0.9800 . no C35 H35A 0.9800 . no C35 H35B 0.9800 . no C35 H35C 0.9800 . no C36 H36A 0.9800 . no C36 H36B 0.9800 . no C36 H36C 0.9800 . no C38 H38A 0.9800 . no C38 H38B 0.9800 . no C38 H38C 0.9800 . no C39 C40 1.45(4) . no C40 H40A 0.9800 . no C40 H40B 0.9800 . no C40 H40C 0.9800 . no C41 H41A 0.9800 . no C41 H41B 0.9800 . no C41 H41C 0.9800 . no C42 H42A 0.9800 . no C42 H42B 0.9800 . no C42 H42C 0.9800 . no C43 H43 0.9500 . no 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 S1 Pb1 S1 83.0(2) . 2_659 yes S1 Pb1 S2 80.46(15) . 2_659 yes S1 Pb1 S2 87.02(16) 2_659 2_659 yes S1 Pb1 S2 87.02(16) . . yes S1 Pb1 S2 80.46(15) 2_659 . yes S2 Pb1 S2 163.3(2) 2_659 . yes S4 Pb2 S2 87.05(19) . . yes S4 Pb2 S3 79.57(15) . . yes S2 Pb2 S3 80.76(17) . . yes S4 Pb2 S1 85.70(15) . 2_659 yes S2 Pb2 S1 78.47(14) . 2_659 yes S3 Pb2 S1 155.06(16) . 2_659 yes S4 Pb2 Pb3 50.16(13) . . yes S2 Pb2 Pb3 114.32(14) . . yes S3 Pb2 Pb3 48.99(12) . . yes S1 Pb2 Pb3 130.61(10) 2_659 . yes S3 Pb3 S3 84.3(2) 2_658 . yes S3 Pb3 S4 81.19(17) 2_658 . yes S3 Pb3 S4 76.99(16) . . yes S3 Pb3 Pb2 111.32(13) 2_658 . yes S3 Pb3 Pb2 49.84(11) . . yes S4 Pb3 Pb2 45.64(11) . . yes C1 S1 Pb1 101.0(7) . . yes C1 S1 Pb2 115.3(6) . 2_659 yes Pb1 S1 Pb2 90.89(14) . 2_659 yes C10 S2 Pb2 106.5(7) . . yes C10 S2 Pb1 106.0(7) . . yes Pb2 S2 Pb1 90.46(18) . . yes C19 S3 Pb3 87.9(7) . 2_658 yes C19 S3 Pb3 109.6(7) . . yes Pb3 S3 Pb3 45.22(11) 2_658 . yes C19 S3 Pb2 103.2(7) . . yes Pb3 S3 Pb2 125.1(2) 2_658 . yes Pb3 S3 Pb2 81.17(16) . . yes C28 S4 Pb2 110.0(7) . . yes C28 S4 Pb3 100.4(7) . . yes Pb2 S4 Pb3 84.20(16) . . yes F5 P1 F3 89.8(13) . . no F5 P1 F1 90.2(13) . . no F3 P1 F1 177.5(12) . . no F5 P1 F6 176.2(14) . . no F3 P1 F6 86.9(13) . . no F1 P1 F6 93.0(13) . . no F5 P1 F4 91.6(12) . . no F3 P1 F4 87.5(12) . . no F1 P1 F4 90.1(12) . . no F6 P1 F4 86.5(12) . . no F5 P1 F2 88.7(12) . . no F3 P1 F2 92.8(12) . . no F1 P1 F2 89.7(12) . . no F6 P1 F2 93.2(12) . . no F4 P1 F2 179.6(15) . . no F7 P2 F9 172.3(13) . . no F7 P2 F10 89.2(12) . . no F9 P2 F10 98.4(12) . . no F7 P2 F8 85.9(12) . . no F9 P2 F8 86.8(12) . . no F10 P2 F8 171.5(13) . . no F7 P2 F11 88.2(13) . . no F9 P2 F11 89.4(13) . . no F10 P2 F11 95.9(12) . . no F8 P2 F11 90.9(12) . . no F7 P2 F12 90.7(12) . . no F9 P2 F12 91.1(13) . . no F10 P2 F12 88.4(12) . . no F8 P2 F12 84.7(11) . . no F11 P2 F12 175.5(12) . . no F14 P3 F17 88.7(13) . . no F14 P3 F16 83.4(13) . . no F17 P3 F16 93.8(12) . . no F14 P3 F15 96.3(13) . . no F17 P3 F15 174.5(13) . . no F16 P3 F15 89.0(12) . . no F14 P3 F18 176.1(14) . . no F17 P3 F18 93.4(12) . . no F16 P3 F18 99.7(12) . . no F15 P3 F18 81.5(12) . . no F14 P3 F13 90.0(13) . . no F17 P3 F13 83.8(12) . . no F16 P3 F13 173.1(13) . . no F15 P3 F13 93.9(12) . . no F18 P3 F13 87.0(13) . . no F21 P4 F20 91.0(12) . . no F21 P4 F19 90.6(13) . . no F20 P4 F19 88.6(12) . . no F21 P4 F24 177.8(13) . . no F20 P4 F24 90.4(12) . . no F19 P4 F24 87.7(12) . . no F21 P4 F22 90.2(13) . . no F20 P4 F22 91.8(11) . . no F19 P4 F22 179.2(13) . . no F24 P4 F22 91.6(13) . . no F21 P4 F23 88.1(12) . . no F20 P4 F23 178.4(13) . . no F19 P4 F23 90.2(11) . . no F24 P4 F23 90.5(12) . . no F22 P4 F23 89.5(11) . . no C4 N1 C7 110.6(16) . . no C4 N1 C8 107.9(16) . . no C7 N1 C8 108.6(19) . . no C4 N1 C9 111.8(17) . . no C7 N1 C9 106.1(18) . . no C8 N1 C9 111.8(18) . . no C17 N2 C16 109.4(19) . . no C17 N2 C13 114.6(17) . . no C16 N2 C13 110.0(19) . . no C17 N2 C18 109(2) . . no C16 N2 C18 105.4(19) . . no C13 N2 C18 108.4(16) . . no C22 N3 C25 112.2(18) . . no C22 N3 C27 107.4(18) . . no C25 N3 C27 109.2(19) . . no C22 N3 C26 107.2(17) . . no C25 N3 C26 109.0(19) . . no C27 N3 C26 112.0(19) . . no C36 N4 C34 112(2) . . no C36 N4 C31 111.4(18) . . no C34 N4 C31 111.4(16) . . no C36 N4 C35 113.5(18) . . no C34 N4 C35 102.4(19) . . no C31 N4 C35 106.0(16) . . no C43 N7 C41 120(3) . . no C43 N7 C42 125(3) . . no C41 N7 C42 115(2) . . no C2 C1 C6 117.4(18) . . no C2 C1 S1 120.3(14) . . no C6 C1 S1 122.1(15) . . no C1 C2 C3 123.9(17) . . no C1 C2 H2 118.0 . . no C3 C2 H2 118.0 . . no C2 C3 C4 118.1(18) . . no C2 C3 H3 120.9 . . no C4 C3 H3 120.9 . . no C5 C4 C3 116.9(18) . . no C5 C4 N1 119.3(16) . . no C3 C4 N1 123.7(17) . . no C6 C5 C4 122.4(18) . . no C6 C5 H5 118.8 . . no C4 C5 H5 118.8 . . no C5 C6 C1 121.1(18) . . no C5 C6 H6 119.5 . . no C1 C6 H6 119.5 . . no N1 C7 H7A 109.5 . . no N1 C7 H7B 109.5 . . no H7A C7 H7B 109.5 . . no N1 C7 H7C 109.5 . . no H7A C7 H7C 109.5 . . no H7B C7 H7C 109.5 . . no N1 C8 H8A 109.5 . . no N1 C8 H8B 109.5 . . no H8A C8 H8B 109.5 . . no N1 C8 H8C 109.5 . . no H8A C8 H8C 109.5 . . no H8B C8 H8C 109.5 . . no N1 C9 H9A 109.5 . . no N1 C9 H9B 109.5 . . no H9A C9 H9B 109.5 . . no N1 C9 H9C 109.5 . . no H9A C9 H9C 109.5 . . no H9B C9 H9C 109.5 . . no C11 C10 C15 116.0(17) . . no C11 C10 S2 117.4(15) . . no C15 C10 S2 126.5(15) . . no C12 C11 C10 121.7(19) . . no C12 C11 H11 119.2 . . no C10 C11 H11 119.2 . . no C11 C12 C13 121.1(19) . . no C11 C12 H12 119.4 . . no C13 C12 H12 119.4 . . no C12 C13 C14 118.5(17) . . no C12 C13 N2 122.9(18) . . no C14 C13 N2 118.6(18) . . no C15 C14 C13 121.2(19) . . no C15 C14 H14 119.4 . . no C13 C14 H14 119.4 . . no C14 C15 C10 121.3(19) . . no C14 C15 H15 119.3 . . no C10 C15 H15 119.3 . . no N2 C16 H16A 109.5 . . no N2 C16 H16B 109.5 . . no H16A C16 H16B 109.5 . . no N2 C16 H16C 109.5 . . no H16A C16 H16C 109.5 . . no H16B C16 H16C 109.5 . . no N2 C17 H17A 109.5 . . no N2 C17 H17B 109.5 . . no H17A C17 H17B 109.5 . . no N2 C17 H17C 109.5 . . no H17A C17 H17C 109.5 . . no H17B C17 H17C 109.5 . . no N2 C18 H18A 109.5 . . no N2 C18 H18B 109.5 . . no H18A C18 H18B 109.5 . . no N2 C18 H18C 109.5 . . no H18A C18 H18C 109.5 . . no H18B C18 H18C 109.5 . . no C24 C19 C20 117(2) . . no C24 C19 S3 119.9(17) . . no C20 C19 S3 122.9(15) . . no C21 C20 C19 120(2) . . no C21 C20 H20 120.2 . . no C19 C20 H20 120.2 . . no C20 C21 C22 122(2) . . no C20 C21 H21 119.2 . . no C22 C21 H21 119.2 . . no C23 C22 C21 119.8(18) . . no C23 C22 N3 119.9(18) . . no C21 C22 N3 120.3(18) . . no C24 C23 C22 119(2) . . no C24 C23 H23 120.4 . . no C22 C23 H23 120.4 . . no C23 C24 C19 123(2) . . no C23 C24 H24 118.7 . . no C19 C24 H24 118.7 . . no N3 C25 H25A 109.5 . . no N3 C25 H25B 109.5 . . no H25A C25 H25B 109.5 . . no N3 C25 H25C 109.5 . . no H25A C25 H25C 109.5 . . no H25B C25 H25C 109.5 . . no N3 C26 H26A 109.5 . . no N3 C26 H26B 109.5 . . no H26A C26 H26B 109.5 . . no N3 C26 H26C 109.5 . . no H26A C26 H26C 109.5 . . no H26B C26 H26C 109.5 . . no N3 C27 H27A 109.5 . . no N3 C27 H27B 109.5 . . no H27A C27 H27B 109.5 . . no N3 C27 H27C 109.5 . . no H27A C27 H27C 109.5 . . no H27B C27 H27C 109.5 . . no C33 C28 C29 118.0(18) . . no C33 C28 S4 120.0(16) . . no C29 C28 S4 121.9(15) . . no C30 C29 C28 119(2) . . no C30 C29 H29 120.4 . . no C28 C29 H29 120.4 . . no C29 C30 C31 122(2) . . no C29 C30 H30 118.9 . . no C31 C30 H30 118.9 . . no C32 C31 C30 118(2) . . no C32 C31 N4 120.8(18) . . no C30 C31 N4 121.4(19) . . no C31 C32 C33 121(2) . . no C31 C32 H32 119.3 . . no C33 C32 H32 119.3 . . no C28 C33 C32 121(2) . . no C28 C33 H33 119.4 . . no C32 C33 H33 119.4 . . no N4 C34 H34A 109.5 . . no N4 C34 H34B 109.5 . . no H34A C34 H34B 109.5 . . no N4 C34 H34C 109.5 . . no H34A C34 H34C 109.5 . . no H34B C34 H34C 109.5 . . no N4 C35 H35A 109.5 . . no N4 C35 H35B 109.5 . . no H35A C35 H35B 109.5 . . no N4 C35 H35C 109.5 . . no H35A C35 H35C 109.5 . . no H35B C35 H35C 109.5 . . no N4 C36 H36A 109.5 . . no N4 C36 H36B 109.5 . . no H36A C36 H36B 109.5 . . no N4 C36 H36C 109.5 . . no H36A C36 H36C 109.5 . . no H36B C36 H36C 109.5 . . no N5 C37 C38 174(4) . . no C37 C38 H38A 109.5 . . no C37 C38 H38B 109.5 . . no H38A C38 H38B 109.5 . . no C37 C38 H38C 109.5 . . no H38A C38 H38C 109.5 . . no H38B C38 H38C 109.5 . . no N6 C39 C40 170(3) . . no C39 C40 H40A 109.5 . . no C39 C40 H40B 109.5 . . no H40A C40 H40B 109.5 . . no C39 C40 H40C 109.5 . . no H40A C40 H40C 109.5 . . no H40B C40 H40C 109.5 . . no N7 C41 H41A 109.5 . . no N7 C41 H41B 109.5 . . no H41A C41 H41B 109.5 . . no N7 C41 H41C 109.5 . . no H41A C41 H41C 109.5 . . no H41B C41 H41C 109.5 . . no N7 C42 H42A 109.5 . . no N7 C42 H42B 109.5 . . no H42A C42 H42B 109.5 . . no N7 C42 H42C 109.5 . . no H42A C42 H42C 109.5 . . no H42B C42 H42C 109.5 . . no N7 C43 O1 142(4) . . no O1 C43 H43 109.1 . . no _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.782 _refine_diff_density_min -1.030 _refine_diff_density_rms 0.293 _database_code_depnum_ccdc_archive 'CCDC 948421' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H34 N4 Pb S2, 2(F6 P), 2(C2 H3 N)' _chemical_formula_sum 'C32 H40 F12 N6 P2 Pb S2' _chemical_formula_weight 1069.95 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_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' '-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 41.814(8) _cell_length_b 8.9420(16) _cell_length_c 22.936(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.692(4) _cell_angle_gamma 90.00 _cell_volume 8256(3) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 17463 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 25.3 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.722 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4208 _exptl_absorpt_coefficient_mu 4.352 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1708 _exptl_absorpt_correction_T_max 0.3370 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 43828 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0372 _diffrn_reflns_limit_h_min -54 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9366 _reflns_number_gt 8847 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Shelxl-97 (Sheldrick, 1997)' _computing_publication_material 'Shelxl-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+63.4080P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9366 _refine_ls_number_parameters 623 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.174 _refine_ls_restrained_S_all 11.349 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.25178(4) 0.20783(19) 0.26485(7) 0.0242(6) Uani 1 1 d . . . P2 P 0.5145(5) 0.336(2) 0.6092(9) 0.061(5) Uani 1 1 d . . . S1 S 0.2959(3) -0.0036(13) 0.2518(5) 0.029(2) Uani 1 1 d . . . S2 S 0.2025(3) 0.0121(14) 0.2061(5) 0.029(2) Uani 1 1 d . . . P1 P 0.8709(5) 0.415(2) 0.5922(9) 0.055(4) Uani 1 1 d . . . F1 F 0.851(3) 0.424(18) 0.528(5) 0.11(4) Uani 0.61(11) 1 d PU A 1 F2 F 0.899(3) 0.34(2) 0.572(7) 0.09(4) Uani 0.61(11) 1 d PU A 1 F3 F 0.844(3) 0.292(17) 0.567(9) 0.13(4) Uani 0.61(11) 1 d PU A 1 F4 F 0.895(2) 0.412(18) 0.662(4) 0.10(4) Uani 0.61(11) 1 d PU A 1 F5 F 0.842(3) 0.467(16) 0.625(5) 0.08(3) Uani 0.61(11) 1 d PU A 1 F6 F 0.897(3) 0.546(15) 0.603(7) 0.13(5) Uani 0.61(11) 1 d PU A 1 F1A F 0.852(5) 0.52(2) 0.534(10) 0.11(5) Uani 0.39(11) 1 d PU A 2 F2A F 0.892(7) 0.36(3) 0.544(10) 0.10(7) Uani 0.39(11) 1 d PU A 2 F3A F 0.861(5) 0.256(16) 0.612(10) 0.09(5) Uani 0.39(11) 1 d PU A 2 F4A F 0.886(5) 0.30(2) 0.637(11) 0.12(6) Uani 0.39(11) 1 d PU A 2 F5A F 0.852(6) 0.52(2) 0.617(12) 0.11(6) Uani 0.39(11) 1 d PU A 2 F6A F 0.877(7) 0.582(19) 0.586(11) 0.11(5) Uani 0.39(11) 1 d PU A 2 F7 F 0.480(3) 0.413(15) 0.582(6) 0.12(5) Uani 0.68(13) 1 d PU B 1 F8 F 0.504(2) 0.303(17) 0.669(5) 0.12(5) Uani 0.68(13) 1 d PU B 1 F9 F 0.532(5) 0.476(16) 0.643(6) 0.15(7) Uani 0.68(13) 1 d PU B 1 F10 F 0.548(2) 0.243(18) 0.641(5) 0.10(5) Uani 0.68(13) 1 d PU B 1 F11 F 0.530(5) 0.37(2) 0.557(6) 0.17(7) Uani 0.68(13) 1 d PU B 1 F12 F 0.501(2) 0.187(11) 0.574(7) 0.11(5) Uani 0.68(13) 1 d PU B 1 F7A F 0.480(6) 0.28(3) 0.613(12) 0.13(9) Uani 0.32(13) 1 d PU B 2 F8A F 0.529(8) 0.20(2) 0.649(8) 0.10(8) Uani 0.32(13) 1 d PU B 2 F9A F 0.516(8) 0.43(4) 0.668(12) 0.13(12) Uani 0.32(13) 1 d PU B 2 F10A F 0.546(6) 0.39(5) 0.61(2) 0.16(13) Uani 0.32(13) 1 d PU B 2 F11A F 0.499(8) 0.47(3) 0.568(14) 0.13(9) Uani 0.32(13) 1 d PU B 2 F12A F 0.510(8) 0.26(4) 0.550(8) 0.12(11) Uani 0.32(13) 1 d PU B 2 N1 N 0.2529(10) 0.271(5) 0.1597(17) 0.029(8) Uani 1 1 d . . . N2 N 0.2598(17) 0.687(7) -0.100(2) 0.058(15) Uani 1 1 d . . . N3 N 0.4249(12) 0.154(5) 0.436(2) 0.047(12) Uani 1 1 d D . . N4 N 0.0863(11) 0.073(5) 0.315(2) 0.036(10) Uani 1 1 d . . . C29 C 0.873(2) 0.213(8) 0.406(4) 0.07(2) Uani 1 1 d . . . H29A H 0.8543 0.2118 0.3689 0.108 Uiso 1 1 calc R . . H29B H 0.8939 0.2064 0.3942 0.108 Uiso 1 1 calc R . . H29C H 0.8726 0.3066 0.4277 0.108 Uiso 1 1 calc R . . C1 C 0.2819(13) 0.302(7) 0.148(2) 0.037(12) Uani 1 1 d . . . H1 H 0.3018 0.2732 0.1774 0.044 Uiso 1 1 calc R . . C2 C 0.2842(14) 0.374(7) 0.097(2) 0.041(13) Uani 1 1 d . . . H2 H 0.3053 0.3928 0.0906 0.049 Uiso 1 1 calc R . . C3 C 0.2557(14) 0.420(6) 0.054(2) 0.032(11) Uani 1 1 d . . . C4 C 0.2259(15) 0.385(8) 0.065(2) 0.045(14) Uani 1 1 d . . . H4 H 0.2056 0.4121 0.0368 0.054 Uiso 1 1 calc R . . C5 C 0.2256(13) 0.311(7) 0.118(2) 0.039(13) Uani 1 1 d . . . H5 H 0.2047 0.2876 0.1249 0.047 Uiso 1 1 calc R . . C6 C 0.2572(15) 0.507(6) -0.001(2) 0.036(11) Uani 1 1 d . . . C7 C 0.286(2) 0.532(10) -0.017(3) 0.07(2) Uani 1 1 d . . . H7 H 0.3061 0.4875 0.0061 0.084 Uiso 1 1 calc R . . C8 C 0.286(2) 0.620(10) -0.066(3) 0.07(2) Uani 1 1 d . . . H8 H 0.3062 0.6320 -0.0760 0.088 Uiso 1 1 calc R . . C9 C 0.232(2) 0.656(12) -0.087(4) 0.09(3) Uani 1 1 d . . . H9 H 0.2125 0.6971 -0.1124 0.106 Uiso 1 1 calc R . . C10 C 0.229(2) 0.567(11) -0.039(3) 0.08(3) Uani 1 1 d . . . H10 H 0.2079 0.5485 -0.0325 0.096 Uiso 1 1 calc R . . C11 C 0.3329(11) 0.042(5) 0.307(2) 0.026(9) Uani 1 1 d . . . C12 C 0.3632(12) 0.028(6) 0.293(2) 0.033(11) Uani 1 1 d . C . H12 H 0.3635 -0.0067 0.2538 0.040 Uiso 1 1 calc R . . C13 C 0.3926(13) 0.066(6) 0.334(3) 0.038(12) Uani 1 1 d . . . H13 H 0.4129 0.0583 0.3236 0.046 Uiso 1 1 calc R C . C14 C 0.3925(13) 0.113(6) 0.391(2) 0.035(11) Uani 1 1 d . C . C15 C 0.3631(14) 0.130(6) 0.407(2) 0.039(12) Uani 1 1 d . . . H15 H 0.3631 0.1662 0.4456 0.047 Uiso 1 1 calc R C . C16 C 0.3335(13) 0.093(6) 0.364(2) 0.032(10) Uani 1 1 d . C . H16 H 0.3131 0.1035 0.3751 0.039 Uiso 1 1 calc R . . C17 C 0.449(2) 0.028(9) 0.445(5) 0.07(3) Uani 0.77(8) 1 d PD C 1 H17A H 0.4531 0.0051 0.4057 0.099 Uiso 0.77(8) 1 calc PR C 1 H17B H 0.4392 -0.0597 0.4591 0.099 Uiso 0.77(8) 1 calc PR C 1 H17C H 0.4695 0.0560 0.4741 0.099 Uiso 0.77(8) 1 calc PR C 1 C17A C 0.458(4) 0.16(4) 0.421(14) 0.07(3) Uani 0.23(8) 1 d PD C 2 H17D H 0.4738 0.0933 0.4465 0.099 Uiso 0.23(8) 1 calc PR C 2 H17E H 0.4669 0.2655 0.4284 0.099 Uiso 0.23(8) 1 calc PR C 2 H17F H 0.4549 0.1381 0.3783 0.099 Uiso 0.23(8) 1 calc PR C 2 C18 C 0.437(2) 0.297(9) 0.418(4) 0.05(2) Uani 0.77(8) 1 d PD C 1 H18A H 0.4565 0.3317 0.4496 0.082 Uiso 0.77(8) 1 calc PR C 1 H18B H 0.4196 0.3725 0.4107 0.082 Uiso 0.77(8) 1 calc PR C 1 H18C H 0.4438 0.2813 0.3802 0.082 Uiso 0.77(8) 1 calc PR C 1 C18A C 0.429(7) 0.313(16) 0.459(14) 0.05(2) Uani 0.23(8) 1 d PD C 2 H18D H 0.4520 0.3331 0.4786 0.082 Uiso 0.23(8) 1 calc PR C 2 H18E H 0.4153 0.3279 0.4873 0.082 Uiso 0.23(8) 1 calc PR C 2 H18F H 0.4209 0.3808 0.4241 0.082 Uiso 0.23(8) 1 calc PR C 2 C19 C 0.420(2) 0.181(13) 0.499(3) 0.06(3) Uani 0.77(8) 1 d PD C 1 H19A H 0.4091 0.0933 0.5108 0.093 Uiso 0.77(8) 1 calc PR C 1 H19B H 0.4052 0.2687 0.4968 0.093 Uiso 0.77(8) 1 calc PR C 1 H19C H 0.4410 0.1996 0.5280 0.093 Uiso 0.77(8) 1 calc PR C 1 C19A C 0.437(7) 0.03(3) 0.482(11) 0.06(3) Uani 0.23(8) 1 d PD C 2 H19D H 0.4469 -0.0473 0.4637 0.093 Uiso 0.23(8) 1 calc PR C 2 H19E H 0.4182 -0.0071 0.4952 0.093 Uiso 0.23(8) 1 calc PR C 2 H19F H 0.4536 0.0735 0.5171 0.093 Uiso 0.23(8) 1 calc PR C 2 C20 C 0.1698(12) 0.032(5) 0.240(2) 0.027(9) Uani 1 1 d . . . C21 C 0.1669(13) 0.149(6) 0.279(2) 0.035(11) Uani 1 1 d . . . H21 H 0.1839 0.2226 0.2889 0.042 Uiso 1 1 calc R . . C22 C 0.1400(13) 0.161(6) 0.302(2) 0.036(11) Uani 1 1 d . . . H22 H 0.1386 0.2420 0.3282 0.043 Uiso 1 1 calc R . . C23 C 0.1153(12) 0.054(6) 0.289(2) 0.031(10) Uani 1 1 d . . . C24 C 0.1172(14) -0.063(6) 0.251(3) 0.040(13) Uani 1 1 d . . . H24 H 0.1001 -0.1358 0.2410 0.049 Uiso 1 1 calc R . . C25 C 0.1442(13) -0.073(6) 0.227(3) 0.037(12) Uani 1 1 d . . . H25 H 0.1452 -0.1538 0.2005 0.044 Uiso 1 1 calc R . . C26 C 0.0987(17) 0.069(8) 0.384(3) 0.050(15) Uani 1 1 d . . . H26A H 0.1114 -0.0224 0.3964 0.076 Uiso 1 1 calc R . . H26B H 0.0797 0.0722 0.4009 0.076 Uiso 1 1 calc R . . H26C H 0.1129 0.1564 0.3977 0.076 Uiso 1 1 calc R . . C27 C 0.0693(16) 0.220(7) 0.294(3) 0.053(16) Uani 1 1 d . . . H27A H 0.0847 0.3026 0.3101 0.080 Uiso 1 1 calc R . . H27B H 0.0496 0.2297 0.3094 0.080 Uiso 1 1 calc R . . H27C H 0.0627 0.2235 0.2500 0.080 Uiso 1 1 calc R . . C28 C 0.0612(15) -0.050(8) 0.295(3) 0.053(16) Uani 1 1 d . . . H28A H 0.0521 -0.0461 0.2512 0.079 Uiso 1 1 calc R . . H28B H 0.0432 -0.0368 0.3147 0.079 Uiso 1 1 calc R . . H28C H 0.0719 -0.1470 0.3069 0.079 Uiso 1 1 calc R . . N5 N 0.868(2) -0.011(8) 0.473(3) 0.08(2) Uani 1 1 d . . . C30 C 0.8703(18) 0.087(8) 0.444(3) 0.055(17) Uani 1 1 d . . . N6 N 1.039(5) 0.39(3) 0.734(11) 0.09(4) Uiso 0.42(14) 1 d PD D 1 C31 C 0.976(6) 0.44(4) 0.671(16) 0.12(6) Uiso 0.42(14) 1 d PD D 1 H31A H 0.9622 0.3895 0.6931 0.184 Uiso 0.42(14) 1 calc PR D 1 H31B H 0.9704 0.4047 0.6292 0.184 Uiso 0.42(14) 1 calc PR D 1 H31C H 0.9730 0.5479 0.6720 0.184 Uiso 0.42(14) 1 calc PR D 1 C32 C 1.011(6) 0.40(4) 0.700(15) 0.11(6) Uiso 0.42(14) 1 d PD D 1 N6A N 1.033(4) 0.335(19) 0.702(8) 0.09(4) Uiso 0.58(14) 1 d PD D 2 C31A C 0.971(5) 0.39(3) 0.636(12) 0.12(6) Uiso 0.58(14) 1 d PD D 2 H31D H 0.9563 0.3877 0.6620 0.184 Uiso 0.58(14) 1 calc PR D 2 H31E H 0.9627 0.3280 0.6003 0.184 Uiso 0.58(14) 1 calc PR D 2 H31F H 0.9732 0.4948 0.6229 0.184 Uiso 0.58(14) 1 calc PR D 2 C32A C 1.003(5) 0.34(3) 0.669(11) 0.11(6) Uiso 0.58(14) 1 d PD D 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 Pb1 0.0257(9) 0.0262(10) 0.0217(9) 0.0021(7) 0.0083(6) 0.0014(7) P2 0.051(10) 0.068(12) 0.058(11) -0.002(9) 0.006(8) -0.014(9) S1 0.024(5) 0.026(6) 0.034(6) -0.004(5) 0.005(5) 0.003(5) S2 0.027(6) 0.031(6) 0.032(6) -0.004(5) 0.012(5) -0.002(5) P1 0.053(10) 0.045(9) 0.068(11) -0.003(8) 0.017(8) 0.004(8) F1 0.11(7) 0.12(9) 0.09(6) -0.02(6) -0.01(5) 0.02(8) F2 0.05(6) 0.11(8) 0.11(10) -0.01(9) 0.04(7) 0.01(5) F3 0.10(8) 0.13(9) 0.18(11) -0.03(8) 0.05(8) -0.05(7) F4 0.08(6) 0.15(11) 0.07(5) 0.01(6) 0.01(4) 0.00(6) F5 0.07(6) 0.11(10) 0.08(5) 0.01(6) 0.04(4) 0.01(6) F6 0.09(8) 0.08(8) 0.18(12) -0.06(8) -0.01(8) -0.04(7) F1A 0.09(9) 0.11(11) 0.11(9) 0.05(9) 0.03(7) 0.01(9) F2A 0.10(14) 0.10(12) 0.11(14) -0.03(12) 0.06(11) -0.01(10) F3A 0.08(9) 0.07(7) 0.15(13) 0.01(8) 0.04(9) -0.02(7) F4A 0.10(11) 0.09(11) 0.15(15) 0.06(11) 0.01(11) 0.02(9) F5A 0.12(13) 0.09(12) 0.15(12) -0.05(10) 0.08(10) 0.00(9) F6A 0.15(13) 0.05(7) 0.14(12) 0.00(8) 0.07(10) -0.01(9) F7 0.11(9) 0.10(9) 0.13(9) -0.02(7) -0.02(7) 0.05(7) F8 0.07(6) 0.17(12) 0.12(8) 0.05(8) 0.06(6) 0.00(7) F9 0.22(16) 0.12(10) 0.10(8) -0.03(7) 0.03(8) -0.11(10) F10 0.05(5) 0.16(12) 0.09(7) -0.04(7) -0.01(5) 0.02(6) F11 0.25(18) 0.20(14) 0.09(8) 0.00(9) 0.07(10) -0.09(14) F12 0.06(5) 0.07(6) 0.17(12) -0.04(6) -0.04(6) 0.00(4) F7A 0.09(12) 0.18(17) 0.14(15) 0.00(12) 0.07(11) -0.03(11) F8A 0.1(2) 0.06(10) 0.06(10) 0.02(7) -0.02(13) 0.01(13) F9A 0.1(2) 0.11(19) 0.10(17) -0.05(15) -0.03(15) 0.05(17) F10A 0.08(14) 0.2(3) 0.2(3) 0.0(3) 0.01(16) -0.07(17) F11A 0.12(15) 0.10(13) 0.15(15) 0.06(12) 0.00(12) 0.03(12) F12A 0.1(2) 0.2(3) 0.05(9) -0.03(14) 0.01(10) 0.1(2) N1 0.03(2) 0.03(2) 0.022(18) 0.004(16) 0.007(16) 0.001(18) N2 0.09(5) 0.06(3) 0.03(3) 0.01(2) 0.03(3) 0.01(3) N3 0.04(3) 0.04(3) 0.05(3) 0.00(2) -0.01(2) 0.00(2) N4 0.03(2) 0.04(2) 0.04(2) -0.008(19) 0.013(18) -0.004(19) C29 0.07(5) 0.05(4) 0.09(6) 0.00(4) 0.00(4) 0.00(4) C1 0.03(2) 0.05(3) 0.03(2) 0.01(2) 0.01(2) 0.00(2) C2 0.03(3) 0.06(4) 0.04(3) 0.01(3) 0.01(2) 0.00(3) C3 0.05(3) 0.03(3) 0.02(2) 0.002(19) 0.01(2) 0.00(2) C4 0.04(3) 0.06(4) 0.03(3) 0.02(3) 0.01(2) 0.01(3) C5 0.03(3) 0.06(4) 0.03(2) 0.02(2) 0.01(2) 0.00(2) C6 0.05(3) 0.03(3) 0.03(2) 0.00(2) 0.02(2) 0.00(2) C7 0.07(5) 0.09(6) 0.06(4) 0.04(4) 0.04(4) 0.01(4) C8 0.09(6) 0.09(6) 0.06(4) 0.03(4) 0.04(4) 0.00(5) C9 0.08(6) 0.12(8) 0.05(4) 0.05(5) 0.00(4) -0.01(6) C10 0.06(4) 0.13(8) 0.05(4) 0.04(5) 0.00(3) -0.01(5) C11 0.02(2) 0.02(2) 0.03(2) 0.000(18) 0.003(17) 0.001(18) C12 0.03(2) 0.04(3) 0.04(3) 0.00(2) 0.01(2) 0.00(2) C13 0.03(3) 0.04(3) 0.05(3) 0.00(2) 0.01(2) 0.00(2) C14 0.03(3) 0.03(2) 0.04(3) 0.00(2) 0.00(2) 0.00(2) C15 0.05(3) 0.04(3) 0.03(2) 0.00(2) 0.00(2) 0.00(3) C16 0.03(2) 0.03(3) 0.03(2) 0.00(2) 0.01(2) 0.00(2) C17 0.03(4) 0.05(5) 0.09(7) 0.00(5) -0.02(4) 0.00(4) C17A 0.03(4) 0.05(5) 0.09(7) 0.00(5) -0.02(4) 0.00(4) C18 0.04(4) 0.05(5) 0.06(5) 0.00(4) 0.01(4) -0.02(4) C18A 0.04(4) 0.05(5) 0.06(5) 0.00(4) 0.01(4) -0.02(4) C19 0.04(4) 0.10(8) 0.04(4) -0.01(4) 0.00(3) -0.01(4) C19A 0.04(4) 0.10(8) 0.04(4) -0.01(4) 0.00(3) -0.01(4) C20 0.03(2) 0.03(2) 0.03(2) 0.001(18) 0.008(18) -0.001(19) C21 0.04(3) 0.03(3) 0.04(3) -0.01(2) 0.02(2) -0.01(2) C22 0.04(3) 0.03(3) 0.04(3) -0.01(2) 0.02(2) -0.01(2) C23 0.03(2) 0.04(3) 0.03(2) -0.01(2) 0.011(19) 0.00(2) C24 0.03(3) 0.04(3) 0.05(3) -0.02(3) 0.02(2) -0.01(2) C25 0.03(3) 0.03(3) 0.05(3) -0.01(2) 0.02(2) 0.00(2) C26 0.06(4) 0.06(4) 0.04(3) -0.01(3) 0.02(3) -0.01(3) C27 0.04(3) 0.05(4) 0.07(4) 0.00(3) 0.02(3) 0.01(3) C28 0.04(3) 0.06(4) 0.07(4) -0.01(3) 0.03(3) -0.02(3) N5 0.10(6) 0.06(4) 0.08(5) 0.00(4) 0.02(4) 0.00(4) C30 0.06(4) 0.05(4) 0.05(4) -0.01(3) 0.00(3) 0.01(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N1 2.49(4) . yes Pb1 S1 2.715(12) . yes Pb1 S2 2.762(12) . yes P2 F10A 1.4(2) . no P2 F12A 1.5(2) . no P2 F8A 1.53(16) . no P2 F7A 1.53(19) . no P2 F9 1.55(11) . no P2 F11A 1.6(2) . no P2 F11 1.56(12) . no P2 F7 1.57(10) . no P2 F8 1.57(9) . no P2 F9A 1.6(2) . no P2 F12 1.58(9) . no P2 F10 1.63(10) . no S1 C11 1.76(5) . no S2 C20 1.76(5) . no P1 F5A 1.47(19) . no P1 F4A 1.48(14) . no P1 F1 1.49(11) . no P1 F6A 1.53(17) . no P1 F2 1.55(15) . no P1 F3 1.56(11) . no P1 F6 1.58(11) . no P1 F3A 1.58(14) . no P1 F4 1.64(9) . no P1 F5 1.65(11) . no P1 F2A 1.7(2) . no P1 F1A 1.67(16) . no F1 F3 1.6(2) . no F1A F6A 1.4(3) . no F3A F4A 1.1(3) . no F5A F6A 1.5(3) . no N1 C5 1.32(6) . no N1 C1 1.33(7) . no N2 C9 1.30(11) . no N2 C8 1.30(10) . no N3 C17 1.48(7) . no N3 C18 1.48(7) . no N3 C18A 1.50(9) . no N3 C19A 1.50(9) . no N3 C14 1.51(7) . no N3 C19 1.52(7) . no N3 C17A 1.53(9) . no N4 C28 1.50(7) . no N4 C23 1.51(6) . no N4 C26 1.51(7) . no N4 C27 1.51(8) . no C29 C30 1.45(11) . no C29 H29A 0.9800 . no C29 H29B 0.9800 . no C29 H29C 0.9800 . no C1 C2 1.37(7) . no C1 H1 0.9500 . no C2 C3 1.39(7) . no C2 H2 0.9500 . no C3 C4 1.37(8) . no C3 C6 1.50(6) . no C4 C5 1.39(7) . no C4 H4 0.9500 . no C5 H5 0.9500 . no C6 C7 1.37(9) . no C6 C10 1.37(9) . no C7 C8 1.38(9) . no C7 H7 0.9500 . no C8 H8 0.9500 . no C9 C10 1.40(10) . no C9 H9 0.9500 . no C10 H10 0.9500 . no C11 C16 1.39(7) . no C11 C12 1.40(7) . no C12 C13 1.38(7) . no C12 H12 0.9500 . no C13 C14 1.38(8) . no C13 H13 0.9500 . no C14 C15 1.37(8) . no C15 C16 1.39(7) . no C15 H15 0.9500 . no C16 H16 0.9500 . no C17 H17A 0.9800 . no C17 H17B 0.9800 . no C17 H17C 0.9800 . no C17A H17F 0.9800 . no C18 H18A 0.9800 . no C18 H18B 0.9800 . no C18 H18C 0.9800 . no C18A H18E 0.9800 . no C18A H18F 0.9800 . no C19 H19A 0.9800 . no C19 H19B 0.9800 . no C19A H19E 0.9800 . no C19A H19F 0.9800 . no C20 C25 1.39(7) . no C20 C21 1.40(7) . no C21 C22 1.38(7) . no C21 H21 0.9500 . no C22 C23 1.38(7) . no C22 H22 0.9500 . no C23 C24 1.38(7) . no C24 C25 1.38(7) . no C24 H24 0.9500 . no C25 H25 0.9500 . no C26 H26A 0.9800 . no C26 H26B 0.9800 . no C26 H26C 0.9800 . no C27 H27A 0.9800 . no C27 H27B 0.9800 . no C27 H27C 0.9800 . no C28 H28A 0.9800 . no C28 H28B 0.9800 . no C28 H28C 0.9800 . no N5 C30 1.13(10) . no N6 C32 1.25(13) . no C31 C32 1.4(2) . no N6A C32A 1.25(12) . no C31A C32A 1.43(19) . no C31A H31D 0.9800 . no C31A H31E 0.9800 . no 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 N1 Pb1 S1 81.9(10) . . yes N1 Pb1 S2 83.0(10) . . yes S1 Pb1 S2 86.8(4) . . yes F10A P2 F12A 94(10) . . no F12A P2 F8A 97(10) . . no F10A P2 F7A 175(10) . . no F12A P2 F7A 91(10) . . no F8A P2 F7A 87(10) . . no F10A P2 F9 52(10) . . no F12A P2 F9 139(10) . . no F8A P2 F9 106(10) . . no F7A P2 F9 123(10) . . no F10A P2 F11A 90(10) . . no F12A P2 F11A 83(10) . . no F8A P2 F11A 179(10) . . no F7A P2 F11A 92(10) . . no F9 P2 F11A 75(10) . . no F10A P2 F11 50(10) . . no F12A P2 F11 51(10) . . no F8A P2 F11 116(10) . . no F7A P2 F11 135(10) . . no F9 P2 F11 88(8) . . no F11A P2 F11 64(10) . . no F10A P2 F7 129(10) . . no F12A P2 F7 88(10) . . no F8A P2 F7 140(10) . . no F7A P2 F7 52(10) . . no F9 P2 F7 96(9) . . no F11 P2 F7 98(10) . . no F10A P2 F8 121(10) . . no F12A P2 F8 136(10) . . no F8A P2 F8 60(10) . . no F7A P2 F8 54(10) . . no F9 P2 F8 86(7) . . no F11A P2 F8 120(10) . . no F11 P2 F8 171(8) . . no F7 P2 F8 89(7) . . no F10A P2 F9A 89(10) . . no F12A P2 F9A 173(10) . . no F8A P2 F9A 90(10) . . no F7A P2 F9A 86(10) . . no F11A P2 F9A 91(10) . . no F11 P2 F9A 129(10) . . no F7 P2 F9A 85(9) . . no F8 P2 F9A 46(10) . . no F10A P2 F12 120(10) . . no F8A P2 F12 71(9) . . no F7A P2 F12 64(10) . . no F9 P2 F12 172(10) . . no F11A P2 F12 108(10) . . no F11 P2 F12 87(8) . . no F7 P2 F12 91(6) . . no F8 P2 F12 98(9) . . no F9A P2 F12 144(10) . . no F10A P2 F10 57(10) . . no F12A P2 F10 93(10) . . no F7A P2 F10 122(10) . . no F9 P2 F10 87(9) . . no F11A P2 F10 147(10) . . no F11 P2 F10 88(9) . . no F7 P2 F10 174(9) . . no F8 P2 F10 86(6) . . no F9A P2 F10 94(9) . . no F12 P2 F10 87(6) . . no C11 S1 Pb1 104.6(16) . . no C20 S2 Pb1 106.8(16) . . no F5A P1 F4A 111(10) . . no F5A P1 F1 97(10) . . no F4A P1 F1 138(10) . . no F5A P1 F6A 61(10) . . no F4A P1 F6A 135(10) . . no F1 P1 F6A 85(10) . . no F5A P1 F2 162(10) . . no F4A P1 F2 71(10) . . no F1 P1 F2 91(7) . . no F6A P1 F2 104(10) . . no F5A P1 F3 102(10) . . no F4A P1 F3 83(10) . . no F1 P1 F3 61(10) . . no F6A P1 F3 141(10) . . no F2 P1 F3 96(9) . . no F5A P1 F6 83(10) . . no F4A P1 F6 106(10) . . no F1 P1 F6 107(10) . . no F2 P1 F6 80(9) . . no F3 P1 F6 168(9) . . no F5A P1 F3A 106(10) . . no F1 P1 F3A 102(10) . . no F6A P1 F3A 166(10) . . no F2 P1 F3A 88(9) . . no F6 P1 F3A 148(10) . . no F5A P1 F4 83(10) . . no F1 P1 F4 176(8) . . no F6A P1 F4 92(10) . . no F2 P1 F4 88(6) . . no F3 P1 F4 122(9) . . no F6 P1 F4 69(8) . . no F3A P1 F4 81(10) . . no F4A P1 F5 95(10) . . no F1 P1 F5 99(7) . . no F6A P1 F5 86(10) . . no F2 P1 F5 167(8) . . no F3 P1 F5 81(7) . . no F6 P1 F5 106(8) . . no F3A P1 F5 81(8) . . no F4 P1 F5 83(5) . . no F5A P1 F2A 155(10) . . no F4A P1 F2A 92(10) . . no F1 P1 F2A 68(10) . . no F6A P1 F2A 97(10) . . no F3 P1 F2A 89(10) . . no F6 P1 F2A 83(10) . . no F3A P1 F2A 98(10) . . no F4 P1 F2A 111(10) . . no F5 P1 F2A 166(10) . . no F5A P1 F1A 74(10) . . no F4A P1 F1A 171(10) . . no F6A P1 F1A 53(10) . . no F2 P1 F1A 106(9) . . no F3 P1 F1A 89(10) . . no F6 P1 F1A 81(10) . . no F3A P1 F1A 131(10) . . no F4 P1 F1A 145(10) . . no F5 P1 F1A 87(8) . . no F2A P1 F1A 83(10) . . no P1 F1 F3 62(8) . . no F1 F3 P1 57(6) . . no F6A F1A P1 58(10) . . no F4A F3A P1 64(10) . . no F3A F4A P1 74(10) . . no P1 F5A F6A 61(10) . . no F1A F6A F5A 80(10) . . no F1A F6A P1 68(10) . . no F5A F6A P1 58(10) . . no C5 N1 C1 117(4) . . no C5 N1 Pb1 121(3) . . no C1 N1 Pb1 119(3) . . no C9 N2 C8 114(6) . . no C17 N3 C18 115(7) . . no C17 N3 C18A 132(10) . . no C18 N3 C19A 139(10) . . no C18A N3 C19A 118(10) . . no C17 N3 C14 110(5) . . no C18 N3 C14 109(5) . . no C18A N3 C14 117(10) . . no C19A N3 C14 112(10) . . no C17 N3 C19 106(7) . . no C18 N3 C19 107(6) . . no C18A N3 C19 64(10) . . no C19A N3 C19 64(10) . . no C14 N3 C19 110(5) . . no C17 N3 C17A 56(10) . . no C18 N3 C17A 58(10) . . no C18A N3 C17A 91(10) . . no C19A N3 C17A 93(10) . . no C14 N3 C17A 124(10) . . no C19 N3 C17A 126(10) . . no C28 N4 C23 112(4) . . no C28 N4 C26 108(5) . . no C23 N4 C26 109(4) . . no C28 N4 C27 108(5) . . no C23 N4 C27 109(4) . . no C26 N4 C27 110(5) . . no C30 C29 H29A 109.5 . . no C30 C29 H29B 109.5 . . no H29A C29 H29B 109.5 . . no C30 C29 H29C 109.5 . . no H29A C29 H29C 109.5 . . no H29B C29 H29C 109.5 . . no N1 C1 C2 123(5) . . no N1 C1 H1 118.6 . . no C2 C1 H1 118.6 . . no C1 C2 C3 120(5) . . no C1 C2 H2 119.9 . . no C3 C2 H2 119.9 . . no C4 C3 C2 117(4) . . no C4 C3 C6 121(5) . . no C2 C3 C6 122(5) . . no C3 C4 C5 120(5) . . no C3 C4 H4 120.2 . . no C5 C4 H4 120.2 . . no N1 C5 C4 123(5) . . no N1 C5 H5 118.3 . . no C4 C5 H5 118.3 . . no C7 C6 C10 116(6) . . no C7 C6 C3 123(5) . . no C10 C6 C3 121(6) . . no C6 C7 C8 120(7) . . no C6 C7 H7 120.0 . . no C8 C7 H7 120.0 . . no N2 C8 C7 126(7) . . no N2 C8 H8 117.2 . . no C7 C8 H8 117.2 . . no N2 C9 C10 126(8) . . no N2 C9 H9 116.9 . . no C6 C10 C9 118(8) . . no C6 C10 H10 120.8 . . no C9 C10 H10 120.8 . . no C16 C11 C12 118(4) . . no C16 C11 S1 123(4) . . no C12 C11 S1 119(4) . . no C13 C12 C11 121(5) . . no C13 C12 H12 119.5 . . no C11 C12 H12 119.5 . . no C14 C13 C12 120(5) . . no C15 C14 C13 120(5) . . no C15 C14 N3 120(5) . . no C13 C14 N3 120(5) . . no C14 C15 C16 119(5) . . no C14 C15 H15 120.4 . . no C16 C15 H15 120.4 . . no C11 C16 C15 122(5) . . no C11 C16 H16 119.2 . . no N3 C17 H17B 109.5 . . no N3 C17 H17C 109.5 . . no N3 C17A H17F 109.5 . . no N3 C18 H18A 109.5 . . no N3 C18 H18C 109.5 . . no N3 C18A H18D 109.5 . . no N3 C18A H18E 109.5 . . no H18D C18A H18F 109.5 . . no H18E C18A H18F 109.5 . . no N3 C19 H19A 109.5 . . no N3 C19 H19B 109.5 . . no N3 C19 H19C 109.5 . . no N3 C19A H19D 109.5 . . no N3 C19A H19E 109.5 . . no H19D C19A H19F 109.5 . . no H19E C19A H19F 109.5 . . no C25 C20 C21 117(4) . . no C25 C20 S2 119(4) . . no C21 C20 S2 125(4) . . no C22 C21 C20 122(5) . . no C22 C21 H21 119.2 . . no C20 C21 H21 119.1 . . no C21 C22 C23 120(5) . . no C21 C22 H22 120.0 . . no C23 C22 H22 120.0 . . no C24 C23 C22 120(5) . . no C24 C23 N4 122(4) . . no C22 C23 N4 118(4) . . no C23 C24 C25 120(5) . . no C23 C24 H24 120.2 . . no C25 C24 H24 120.2 . . no C24 C25 C20 122(5) . . no C24 C25 H25 119.0 . . no C20 C25 H25 119.0 . . no N4 C26 H26A 109.5 . . no N4 C26 H26B 109.5 . . no H26A C26 H26B 109.5 . . no N4 C26 H26C 109.5 . . no H26A C26 H26C 109.5 . . no H26B C26 H26C 109.5 . . no N4 C27 H27A 109.5 . . no N4 C27 H27B 109.5 . . no H27A C27 H27B 109.5 . . no N4 C27 H27C 109.5 . . no H27A C27 H27C 109.5 . . no H27B C27 H27C 109.5 . . no N4 C28 H28A 109.5 . . no N4 C28 H28B 109.5 . . no H28A C28 H28B 109.5 . . no N4 C28 H28C 109.5 . . no H28A C28 H28C 109.5 . . no H28B C28 H28C 109.5 . . no N5 C30 C29 179(9) . . no N6 C32 C31 165(10) . . no C32A C31A H31D 109.8 . . no C32A C31A H31E 109.3 . . no H31D C31A H31F 109.5 . . no H31E C31A H31F 109.5 . . no _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.196 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.117 #===END _database_code_depnum_ccdc_archive 'CCDC 948422'