# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Lars Wesemann' _publ_contact_author_email LARS.WESEMANN@UNI-TUEBINGEN.DE _publ_section_title ; Chalcogen chemistry of Group(IV)-closo-dodecaborates, Synthesis, Theory and Coordination Chemistry ; loop_ _publ_author_name 'L Wesemann' 'Jorg-Alexander Dimmer' 'Martin Hornung' 'Florian Weigend' # Attachment '765675_compound_6.cif' data_hornung116 _database_code_depnum_ccdc_archive 'CCDC 765675' #TrackingRef '765675_compound_6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B22 P2 Pt S2 Sn2, 2(C8 H20 N), 3(C2 H3 N) ' _chemical_formula_sum 'C49 H97 B22 N5 P2 Pt S2 Sn2' _chemical_formula_weight 1552.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' B B 0.0010 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pt Pt -1.7030 8.3910 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1250 0.1230 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6540 1.4250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.2397(6) _cell_length_b 22.4086(12) _cell_length_c 26.6785(14) _cell_angle_alpha 90.00 _cell_angle_beta 105.233(4) _cell_angle_gamma 90.00 _cell_volume 7060.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40236 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 54.42 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2993 _exptl_crystal_size_mid 0.2466 _exptl_crystal_size_min 0.0723 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3104 _exptl_absorpt_coefficient_mu 2.820 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3383 _exptl_absorpt_correction_T_max 0.7972 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 75007 _diffrn_reflns_av_R_equivalents 0.1118 _diffrn_reflns_av_sigmaI/netI 0.0633 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 5.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12739 _reflns_number_gt 9983 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep3 for windows' _computing_publication_material ? _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. Due to moderate crystal quality even after several attempts of crystallization the R(int) has a value >0.1 ; _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^)+(0.0278P)^2^+13.0116P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12739 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0753 _refine_ls_R_factor_gt 0.0506 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0836 _refine_ls_goodness_of_fit_ref 1.108 _refine_ls_restrained_S_all 1.108 _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 Pt1 Pt 0.780106(19) 0.220367(10) 0.256809(9) 0.02075(7) Uani 1 1 d . . . Sn1 Sn 0.65013(4) 0.337410(18) 0.305350(17) 0.02764(11) Uani 1 1 d . . . Sn2 Sn 0.84194(4) 0.351744(19) 0.205491(17) 0.02803(11) Uani 1 1 d . . . S1 S 0.61421(12) 0.28030(7) 0.22830(6) 0.0284(3) Uani 1 1 d . . . S2 S 0.88334(13) 0.30874(7) 0.28823(6) 0.0262(3) Uani 1 1 d . . . P1 P 0.67006(13) 0.14026(7) 0.22706(6) 0.0247(3) Uani 1 1 d . . . P2 P 0.94010(13) 0.16776(7) 0.29161(6) 0.0248(3) Uani 1 1 d . . . C111 C 0.7425(5) 0.0700(2) 0.2207(3) 0.0293(14) Uani 1 1 d . . . H11A H 0.6875 0.0379 0.2152 0.035 Uiso 1 1 calc R . . H11B H 0.7708 0.0724 0.1901 0.035 Uiso 1 1 calc R . . C112 C 0.8406(5) 0.0541(3) 0.2670(2) 0.0282(14) Uani 1 1 d . . . H11C H 0.8588 0.0122 0.2651 0.034 Uiso 1 1 calc R . . H11D H 0.8176 0.0602 0.2988 0.034 Uiso 1 1 calc R . . C121 C 0.5762(5) 0.1211(3) 0.2675(2) 0.0266(14) Uani 1 1 d . . . C122 C 0.5753(6) 0.1538(3) 0.3110(3) 0.0369(16) Uani 1 1 d . . . H122 H 0.6226 0.1868 0.3197 0.044 Uiso 1 1 calc R . . C123 C 0.5045(6) 0.1382(3) 0.3421(3) 0.0428(18) Uani 1 1 d . . . H123 H 0.5040 0.1609 0.3713 0.051 Uiso 1 1 calc R . . C124 C 0.4356(6) 0.0891(3) 0.3293(3) 0.0469(19) Uani 1 1 d . . . H124 H 0.3891 0.0781 0.3503 0.056 Uiso 1 1 calc R . . C125 C 0.4346(6) 0.0559(3) 0.2856(3) 0.0442(18) Uani 1 1 d . . . H125 H 0.3865 0.0232 0.2769 0.053 Uiso 1 1 calc R . . C126 C 0.5046(6) 0.0712(3) 0.2548(3) 0.0381(17) Uani 1 1 d . . . H126 H 0.5046 0.0485 0.2256 0.046 Uiso 1 1 calc R . . C131 C 0.5853(5) 0.1507(3) 0.1610(3) 0.0317(15) Uani 1 1 d . . . C132 C 0.6411(7) 0.1562(4) 0.1225(3) 0.059(2) Uani 1 1 d . . . H132 H 0.7198 0.1568 0.1315 0.070 Uiso 1 1 calc R . . C133 C 0.5829(9) 0.1609(5) 0.0710(4) 0.072(3) Uani 1 1 d . . . H133 H 0.6222 0.1643 0.0457 0.087 Uiso 1 1 calc R . . C134 C 0.4695(9) 0.1606(4) 0.0574(3) 0.061(2) Uani 1 1 d . . . H134 H 0.4305 0.1626 0.0224 0.073 Uiso 1 1 calc R . . C135 C 0.4105(7) 0.1574(4) 0.0942(4) 0.068(3) Uani 1 1 d . . . H135 H 0.3318 0.1590 0.0843 0.081 Uiso 1 1 calc R . . C136 C 0.4677(6) 0.1518(3) 0.1464(3) 0.050(2) Uani 1 1 d . . . H136 H 0.4274 0.1488 0.1714 0.060 Uiso 1 1 calc R . . C211 C 0.9461(5) 0.0914(3) 0.2691(3) 0.0278(14) Uani 1 1 d . . . H21A H 0.9583 0.0925 0.2346 0.033 Uiso 1 1 calc R . . H21B H 1.0110 0.0716 0.2918 0.033 Uiso 1 1 calc R . . C221 C 0.9591(5) 0.1598(3) 0.3608(2) 0.0272(13) Uani 1 1 d . . . C222 C 1.0393(6) 0.1205(3) 0.3901(3) 0.0371(16) Uani 1 1 d . . . H222 H 1.0869 0.0994 0.3745 0.045 Uiso 1 1 calc R . . C223 C 1.0480(6) 0.1128(4) 0.4427(3) 0.048(2) Uani 1 1 d . . . H223 H 1.1025 0.0871 0.4622 0.057 Uiso 1 1 calc R . . C224 C 0.9765(7) 0.1431(4) 0.4663(3) 0.052(2) Uani 1 1 d . . . H224 H 0.9821 0.1371 0.5014 0.062 Uiso 1 1 calc R . . C225 C 0.8973(7) 0.1819(3) 0.4379(3) 0.0448(18) Uani 1 1 d . . . H225 H 0.8496 0.2026 0.4538 0.054 Uiso 1 1 calc R . . C226 C 0.8887(6) 0.1904(3) 0.3853(3) 0.0320(15) Uani 1 1 d . . . H226 H 0.8350 0.2168 0.3662 0.038 Uiso 1 1 calc R . . C231 C 1.0681(5) 0.1996(3) 0.2807(3) 0.0286(14) Uani 1 1 d . . . C232 C 1.1669(5) 0.2102(3) 0.3198(3) 0.0342(15) Uani 1 1 d . . . H232 H 1.1692 0.2020 0.3542 0.041 Uiso 1 1 calc R . . C233 C 1.2618(6) 0.2331(3) 0.3074(3) 0.0422(18) Uani 1 1 d . . . H233 H 1.3274 0.2403 0.3336 0.051 Uiso 1 1 calc R . . C234 C 1.2596(6) 0.2454(3) 0.2567(3) 0.047(2) Uani 1 1 d . . . H234 H 1.3240 0.2601 0.2487 0.057 Uiso 1 1 calc R . . C235 C 1.1622(6) 0.2358(3) 0.2177(3) 0.0435(18) Uani 1 1 d . . . H235 H 1.1608 0.2444 0.1835 0.052 Uiso 1 1 calc R . . C236 C 1.0675(6) 0.2137(3) 0.2294(3) 0.0366(16) Uani 1 1 d . . . H236 H 1.0018 0.2080 0.2029 0.044 Uiso 1 1 calc R . . B101 B 0.7326(7) 0.4190(3) 0.3543(3) 0.0375(19) Uani 1 1 d . . . H101 H 0.8030 0.4379 0.3409 0.045 Uiso 1 1 calc R . . B102 B 0.5767(7) 0.4287(3) 0.3176(3) 0.0355(18) Uani 1 1 d . . . H102 H 0.5490 0.4534 0.2808 0.043 Uiso 1 1 calc R . . B103 B 0.4941(7) 0.3643(4) 0.3342(3) 0.0335(18) Uani 1 1 d . . . H103 H 0.4141 0.3485 0.3081 0.040 Uiso 1 1 calc R . . B104 B 0.5969(7) 0.3127(3) 0.3795(3) 0.0345(18) Uani 1 1 d . . . H104 H 0.5822 0.2645 0.3818 0.041 Uiso 1 1 calc R . . B105 B 0.7423(6) 0.3461(3) 0.3920(3) 0.0327(17) Uani 1 1 d . . . H105 H 0.8196 0.3188 0.4024 0.039 Uiso 1 1 calc R . . B106 B 0.6408(6) 0.4644(3) 0.3779(3) 0.0352(18) Uani 1 1 d . . . H106 H 0.6548 0.5129 0.3786 0.042 Uiso 1 1 calc R . . B107 B 0.5016(7) 0.4338(3) 0.3659(3) 0.0335(18) Uani 1 1 d . . . H107 H 0.4257 0.4621 0.3587 0.040 Uiso 1 1 calc R . . B108 B 0.5139(7) 0.3660(4) 0.4021(3) 0.0351(18) Uani 1 1 d . . . H108 H 0.4457 0.3502 0.4186 0.042 Uiso 1 1 calc R . . B109 B 0.6571(7) 0.3552(4) 0.4350(3) 0.0370(18) Uani 1 1 d . . . H109 H 0.6816 0.3325 0.4728 0.044 Uiso 1 1 calc R . . B110 B 0.7365(7) 0.4170(4) 0.4204(4) 0.041(2) Uani 1 1 d . . . H110 H 0.8123 0.4342 0.4487 0.049 Uiso 1 1 calc R . . B111 B 0.5973(7) 0.4285(4) 0.4278(3) 0.0391(19) Uani 1 1 d . . . H111 H 0.5828 0.4536 0.4609 0.047 Uiso 1 1 calc R . . B201 B 0.8962(6) 0.3284(3) 0.1319(3) 0.0307(17) Uani 1 1 d . . . H201 H 0.9261 0.2820 0.1323 0.037 Uiso 1 1 calc R . . B202 B 0.7383(6) 0.3487(4) 0.1195(3) 0.0318(17) Uani 1 1 d . . . H202 H 0.6690 0.3159 0.1120 0.038 Uiso 1 1 calc R . . B203 B 0.7325(7) 0.4232(3) 0.1539(3) 0.0326(17) Uani 1 1 d . . . H203 H 0.6597 0.4368 0.1682 0.039 Uiso 1 1 calc R . . B204 B 0.8852(6) 0.4482(3) 0.1867(3) 0.0335(18) Uani 1 1 d . . . H204 H 0.9076 0.4770 0.2213 0.040 Uiso 1 1 calc R . . B205 B 0.9841(6) 0.3898(4) 0.1727(3) 0.0323(17) Uani 1 1 d . . . H205 H 1.0687 0.3821 0.1988 0.039 Uiso 1 1 calc R . . B206 B 0.8188(6) 0.3622(3) 0.0745(3) 0.0301(16) Uani 1 1 d . . . H206 H 0.7995 0.3358 0.0385 0.036 Uiso 1 1 calc R . . B207 B 0.7241(7) 0.4174(4) 0.0867(3) 0.0349(18) Uani 1 1 d . . . H207 H 0.6428 0.4272 0.0585 0.042 Uiso 1 1 calc R . . B208 B 0.8066(6) 0.4749(3) 0.1249(3) 0.0331(18) Uani 1 1 d . . . H208 H 0.7785 0.5217 0.1215 0.040 Uiso 1 1 calc R . . B209 B 0.9521(6) 0.4558(4) 0.1356(3) 0.0337(18) Uani 1 1 d . . . H209 H 1.0178 0.4901 0.1387 0.040 Uiso 1 1 calc R . . B210 B 0.9589(6) 0.3862(4) 0.1051(3) 0.0332(17) Uani 1 1 d . . . H210 H 1.0304 0.3755 0.0889 0.040 Uiso 1 1 calc R . . B211 B 0.8542(6) 0.4389(3) 0.0751(3) 0.0337(18) Uani 1 1 d . . . H211 H 0.8568 0.4623 0.0392 0.040 Uiso 1 1 calc R . . N1 N 0.1597(4) 0.4122(2) 0.4246(2) 0.0318(12) Uani 1 1 d . . . C101 C 0.1020(6) 0.4186(3) 0.3669(3) 0.0426(18) Uani 1 1 d . . . H10A H 0.0307 0.3972 0.3595 0.051 Uiso 1 1 calc R . . H10B H 0.0846 0.4604 0.3596 0.051 Uiso 1 1 calc R . . C102 C 0.1680(7) 0.3966(4) 0.3303(3) 0.057(2) Uani 1 1 d . . . H10C H 0.1243 0.4027 0.2951 0.086 Uiso 1 1 calc R . . H10D H 0.1838 0.3549 0.3361 0.086 Uiso 1 1 calc R . . H10E H 0.2379 0.4183 0.3363 0.086 Uiso 1 1 calc R . . C103 C 0.2712(6) 0.4463(3) 0.4401(3) 0.0388(17) Uani 1 1 d . . . H10F H 0.3043 0.4405 0.4770 0.047 Uiso 1 1 calc R . . H10G H 0.3225 0.4288 0.4220 0.047 Uiso 1 1 calc R . . C104 C 0.2650(7) 0.5119(3) 0.4295(3) 0.050(2) Uani 1 1 d . . . H10H H 0.3395 0.5288 0.4408 0.074 Uiso 1 1 calc R . . H10I H 0.2165 0.5303 0.4481 0.074 Uiso 1 1 calc R . . H10J H 0.2350 0.5186 0.3929 0.074 Uiso 1 1 calc R . . C105 C 0.1887(5) 0.3469(3) 0.4382(3) 0.0351(16) Uani 1 1 d . . . H10K H 0.2427 0.3339 0.4195 0.042 Uiso 1 1 calc R . . H10L H 0.2260 0.3443 0.4750 0.042 Uiso 1 1 calc R . . C106 C 0.0905(6) 0.3040(3) 0.4263(3) 0.0447(18) Uani 1 1 d . . . H10M H 0.1175 0.2644 0.4362 0.067 Uiso 1 1 calc R . . H10N H 0.0541 0.3048 0.3897 0.067 Uiso 1 1 calc R . . H10O H 0.0372 0.3155 0.4453 0.067 Uiso 1 1 calc R . . C107 C 0.0773(6) 0.4357(3) 0.4532(3) 0.0464(19) Uani 1 1 d . . . H10P H 0.0071 0.4135 0.4416 0.056 Uiso 1 1 calc R . . H10Q H 0.0608 0.4771 0.4432 0.056 Uiso 1 1 calc R . . C108 C 0.1160(8) 0.4325(4) 0.5119(3) 0.059(2) Uani 1 1 d . . . H10R H 0.0580 0.4485 0.5263 0.088 Uiso 1 1 calc R . . H10S H 0.1841 0.4554 0.5241 0.088 Uiso 1 1 calc R . . H10T H 0.1302 0.3917 0.5225 0.088 Uiso 1 1 calc R . . N2 N 0.3286(4) 0.4236(2) 0.0995(2) 0.0363(13) Uani 1 1 d . . . C201 C 0.2823(6) 0.3614(3) 0.0841(4) 0.052(2) Uani 1 1 d . . . H20A H 0.2225 0.3536 0.1010 0.062 Uiso 1 1 calc R . . H20B H 0.2483 0.3609 0.0469 0.062 Uiso 1 1 calc R . . C202 C 0.3677(8) 0.3107(4) 0.0974(4) 0.074(3) Uani 1 1 d . . . H20C H 0.3303 0.2735 0.0861 0.112 Uiso 1 1 calc R . . H20D H 0.4003 0.3096 0.1343 0.112 Uiso 1 1 calc R . . H20E H 0.4264 0.3171 0.0802 0.112 Uiso 1 1 calc R . . C203 C 0.3855(6) 0.4253(4) 0.1575(3) 0.049(2) Uani 1 1 d . . . H20F H 0.4485 0.3975 0.1647 0.059 Uiso 1 1 calc R . . H20G H 0.4167 0.4649 0.1662 0.059 Uiso 1 1 calc R . . C204 C 0.3113(7) 0.4106(5) 0.1926(3) 0.067(3) Uani 1 1 d . . . H20H H 0.3549 0.4129 0.2281 0.101 Uiso 1 1 calc R . . H20I H 0.2816 0.3710 0.1852 0.101 Uiso 1 1 calc R . . H20J H 0.2499 0.4386 0.1868 0.101 Uiso 1 1 calc R . . C205 C 0.4187(6) 0.4398(4) 0.0724(3) 0.048(2) Uani 1 1 d . . . H20K H 0.4791 0.4105 0.0816 0.058 Uiso 1 1 calc R . . H20L H 0.4506 0.4782 0.0853 0.058 Uiso 1 1 calc R . . C206 C 0.3769(7) 0.4429(4) 0.0137(3) 0.059(2) Uani 1 1 d . . . H20M H 0.4386 0.4535 -0.0006 0.088 Uiso 1 1 calc R . . H20N H 0.3183 0.4725 0.0041 0.088 Uiso 1 1 calc R . . H20O H 0.3473 0.4047 0.0004 0.088 Uiso 1 1 calc R . . C207 C 0.2286(6) 0.4660(3) 0.0852(3) 0.0463(19) Uani 1 1 d . . . H20P H 0.1922 0.4617 0.0484 0.056 Uiso 1 1 calc R . . H20Q H 0.1742 0.4543 0.1040 0.056 Uiso 1 1 calc R . . C208 C 0.2580(8) 0.5310(4) 0.0965(4) 0.063(2) Uani 1 1 d . . . H20R H 0.1904 0.5547 0.0864 0.094 Uiso 1 1 calc R . . H20S H 0.3101 0.5436 0.0772 0.094 Uiso 1 1 calc R . . H20T H 0.2922 0.5361 0.1329 0.094 Uiso 1 1 calc R . . N3 N 0.1220(7) 0.2212(5) 0.0723(4) 0.094(3) Uani 1 1 d . . . C31 C 0.0295(8) 0.2106(4) 0.0596(3) 0.056(2) Uani 1 1 d . . . C32 C -0.0899(7) 0.1951(4) 0.0429(3) 0.057(2) Uani 1 1 d . . . H32A H -0.1098 0.1849 0.0067 0.085 Uiso 1 1 calc R . . H32B H -0.1346 0.2285 0.0483 0.085 Uiso 1 1 calc R . . H32C H -0.1042 0.1616 0.0627 0.085 Uiso 1 1 calc R . . N5 N 0.3393(7) 0.2121(4) 0.4506(4) 0.086(3) Uani 1 1 d . . . C51 C 0.4330(8) 0.2084(4) 0.4657(3) 0.056(2) Uani 1 1 d . . . C52 C 0.5546(7) 0.2030(4) 0.4866(3) 0.059(2) Uani 1 1 d . . . H52A H 0.5745 0.2122 0.5231 0.089 Uiso 1 1 calc R . . H52B H 0.5921 0.2303 0.4690 0.089 Uiso 1 1 calc R . . H52C H 0.5775 0.1629 0.4817 0.089 Uiso 1 1 calc R . . N4 N -0.0123(9) 0.0790(4) 0.1339(4) 0.085(3) Uani 1 1 d . . . C41 C 0.0784(9) 0.0798(5) 0.1555(4) 0.068(3) Uani 1 1 d . . . C42 C 0.1937(9) 0.0788(6) 0.1862(7) 0.137(7) Uani 1 1 d . . . H42A H 0.1976 0.0936 0.2204 0.206 Uiso 1 1 calc R . . H42B H 0.2390 0.1036 0.1702 0.206 Uiso 1 1 calc R . . H42C H 0.2218 0.0386 0.1886 0.206 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 Pt1 0.02219(12) 0.01887(11) 0.02018(12) -0.00019(10) 0.00377(8) 0.00051(10) Sn1 0.0346(2) 0.0224(2) 0.0263(2) -0.00006(18) 0.00886(19) 0.00291(18) Sn2 0.0344(2) 0.0265(2) 0.0238(2) -0.00150(18) 0.00871(18) -0.00266(18) S1 0.0269(8) 0.0270(7) 0.0281(8) -0.0017(7) 0.0017(6) 0.0042(7) S2 0.0273(8) 0.0250(7) 0.0242(8) -0.0011(6) 0.0031(7) -0.0016(6) P1 0.0269(8) 0.0223(7) 0.0233(8) -0.0027(7) 0.0038(7) -0.0014(6) P2 0.0257(8) 0.0232(8) 0.0252(9) 0.0002(7) 0.0061(7) 0.0033(6) C111 0.034(4) 0.015(3) 0.033(4) -0.008(3) -0.001(3) -0.002(3) C112 0.032(3) 0.024(3) 0.027(4) 0.005(3) 0.006(3) 0.007(3) C121 0.027(3) 0.022(3) 0.032(4) 0.000(3) 0.009(3) -0.003(2) C122 0.050(4) 0.020(3) 0.045(4) -0.006(3) 0.019(3) -0.002(3) C123 0.052(5) 0.034(4) 0.050(5) -0.002(3) 0.028(4) -0.001(3) C124 0.044(4) 0.045(4) 0.060(5) 0.014(4) 0.028(4) 0.002(3) C125 0.048(4) 0.030(4) 0.059(5) 0.001(4) 0.020(4) -0.011(3) C126 0.046(4) 0.027(3) 0.044(4) -0.003(3) 0.018(3) -0.006(3) C131 0.039(4) 0.020(3) 0.031(4) -0.005(3) -0.001(3) 0.002(3) C132 0.049(5) 0.090(7) 0.036(5) 0.020(5) 0.011(4) 0.020(5) C133 0.086(7) 0.095(8) 0.038(5) 0.012(5) 0.022(5) 0.022(6) C134 0.092(7) 0.044(5) 0.031(5) 0.005(4) -0.010(5) -0.011(5) C135 0.048(5) 0.060(6) 0.076(7) 0.014(5) -0.019(5) -0.024(4) C136 0.042(4) 0.050(5) 0.051(5) 0.011(4) -0.001(4) -0.011(4) C211 0.031(3) 0.021(3) 0.032(4) 0.002(3) 0.009(3) 0.008(3) C221 0.027(3) 0.029(3) 0.025(3) -0.001(3) 0.005(3) -0.003(3) C222 0.037(4) 0.041(4) 0.029(4) 0.005(3) 0.003(3) 0.009(3) C223 0.048(5) 0.049(5) 0.036(4) 0.012(4) -0.007(4) 0.007(4) C224 0.068(5) 0.059(5) 0.026(4) 0.009(4) 0.006(4) -0.015(4) C225 0.064(5) 0.045(4) 0.026(4) -0.006(3) 0.014(4) -0.005(4) C226 0.042(4) 0.026(3) 0.024(3) -0.001(3) 0.001(3) -0.002(3) C231 0.029(3) 0.022(3) 0.036(4) 0.002(3) 0.010(3) 0.009(2) C232 0.031(3) 0.033(4) 0.035(4) 0.003(3) 0.003(3) 0.001(3) C233 0.028(4) 0.042(4) 0.051(5) -0.004(4) 0.001(3) -0.002(3) C234 0.029(4) 0.044(4) 0.073(6) 0.005(4) 0.023(4) -0.001(3) C235 0.044(4) 0.047(4) 0.042(4) 0.006(3) 0.017(4) -0.004(3) C236 0.034(4) 0.043(4) 0.032(4) 0.004(3) 0.008(3) 0.001(3) B101 0.037(4) 0.029(4) 0.051(5) -0.007(4) 0.020(4) -0.010(3) B102 0.045(5) 0.019(3) 0.043(5) 0.006(3) 0.013(4) 0.011(3) B103 0.031(4) 0.041(4) 0.029(4) -0.003(3) 0.008(3) 0.005(3) B104 0.042(5) 0.028(4) 0.034(4) 0.008(3) 0.011(4) 0.001(3) B105 0.036(4) 0.030(4) 0.035(4) -0.002(3) 0.013(3) 0.010(3) B106 0.034(4) 0.026(4) 0.048(5) -0.010(4) 0.017(4) -0.003(3) B107 0.038(4) 0.025(4) 0.038(5) 0.001(3) 0.011(4) 0.010(3) B108 0.032(4) 0.042(4) 0.033(4) 0.003(4) 0.011(3) 0.002(3) B109 0.046(5) 0.040(4) 0.026(4) 0.005(4) 0.012(4) 0.006(4) B110 0.027(4) 0.048(5) 0.046(5) -0.021(4) 0.007(4) -0.002(4) B111 0.042(5) 0.041(5) 0.038(5) -0.011(4) 0.018(4) 0.007(4) B201 0.036(4) 0.033(4) 0.023(4) 0.006(3) 0.007(3) 0.005(3) B202 0.030(4) 0.042(4) 0.022(4) 0.002(3) 0.005(3) -0.005(3) B203 0.034(4) 0.032(4) 0.033(4) 0.003(3) 0.011(3) 0.000(3) B204 0.036(4) 0.030(4) 0.040(5) -0.006(3) 0.019(4) -0.011(3) B205 0.024(4) 0.044(4) 0.026(4) -0.004(3) 0.002(3) 0.001(3) B206 0.034(4) 0.033(4) 0.023(4) 0.000(3) 0.008(3) -0.003(3) B207 0.031(4) 0.040(4) 0.032(4) 0.010(4) 0.007(3) 0.001(3) B208 0.036(4) 0.027(4) 0.039(5) 0.008(3) 0.016(4) -0.004(3) B209 0.028(4) 0.039(4) 0.036(5) -0.004(4) 0.013(3) -0.007(3) B210 0.022(4) 0.045(5) 0.035(4) -0.004(4) 0.011(3) 0.001(3) B211 0.035(4) 0.035(4) 0.030(4) 0.005(3) 0.006(3) 0.004(3) N1 0.022(3) 0.036(3) 0.036(3) -0.003(3) 0.006(2) 0.001(2) C101 0.035(4) 0.047(4) 0.036(4) 0.001(3) -0.007(3) 0.002(3) C102 0.051(5) 0.084(6) 0.038(5) -0.010(5) 0.013(4) -0.010(4) C103 0.033(4) 0.041(4) 0.040(4) 0.001(3) 0.005(3) -0.005(3) C104 0.056(5) 0.042(4) 0.045(5) -0.001(4) 0.005(4) -0.006(4) C105 0.030(4) 0.036(4) 0.036(4) 0.003(3) 0.003(3) 0.006(3) C106 0.037(4) 0.047(4) 0.047(5) 0.001(4) 0.007(3) -0.002(3) C107 0.042(4) 0.045(4) 0.059(5) -0.001(4) 0.025(4) 0.011(3) C108 0.076(6) 0.056(5) 0.051(5) -0.007(4) 0.028(5) 0.004(4) N2 0.025(3) 0.038(3) 0.043(4) 0.000(3) 0.003(3) -0.001(2) C201 0.037(4) 0.048(5) 0.064(6) -0.007(4) 0.003(4) -0.005(3) C202 0.073(6) 0.048(5) 0.096(8) 0.004(5) 0.011(6) 0.013(5) C203 0.037(4) 0.066(5) 0.041(5) -0.002(4) 0.004(4) -0.003(4) C204 0.045(5) 0.106(8) 0.050(6) 0.004(5) 0.011(4) 0.004(5) C205 0.030(4) 0.060(5) 0.055(5) 0.002(4) 0.012(4) -0.004(3) C206 0.048(5) 0.079(6) 0.052(5) 0.008(5) 0.017(4) 0.012(4) C207 0.042(4) 0.048(4) 0.047(5) -0.003(4) 0.008(4) 0.002(3) C208 0.074(6) 0.043(5) 0.073(7) -0.005(4) 0.022(5) 0.003(4) N3 0.053(5) 0.117(8) 0.109(8) -0.032(6) 0.017(5) 0.002(5) C31 0.064(6) 0.053(5) 0.053(5) -0.012(4) 0.018(5) 0.008(4) C32 0.057(5) 0.057(5) 0.051(5) -0.003(4) 0.006(4) 0.003(4) N5 0.060(5) 0.100(7) 0.087(7) 0.006(6) 0.000(5) 0.015(5) C51 0.062(6) 0.048(5) 0.050(5) 0.008(4) 0.004(4) 0.008(4) C52 0.056(5) 0.067(6) 0.049(5) 0.009(4) 0.007(4) -0.006(4) N4 0.091(7) 0.083(6) 0.066(6) 0.001(5) -0.003(5) -0.023(5) C41 0.071(7) 0.078(7) 0.064(7) -0.025(5) 0.031(6) -0.024(6) C42 0.046(6) 0.120(10) 0.244(19) -0.106(12) 0.036(9) 0.003(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 Pt1 P1 2.2593(15) . ? Pt1 P2 2.2652(15) . ? Pt1 S2 2.3799(15) . ? Pt1 S1 2.3860(15) . ? Sn1 B102 2.292(7) . ? Sn1 B105 2.298(8) . ? Sn1 B104 2.308(8) . ? Sn1 B101 2.317(8) . ? Sn1 B103 2.319(8) . ? Sn1 S1 2.3626(16) . ? Sn2 B201 2.293(8) . ? Sn2 B203 2.299(8) . ? Sn2 B205 2.306(8) . ? Sn2 B204 2.312(7) . ? Sn2 B202 2.313(7) . ? Sn2 S2 2.3388(16) . ? P1 C131 1.809(7) . ? P1 C121 1.822(6) . ? P1 C111 1.837(6) . ? P2 C221 1.808(6) . ? P2 C231 1.814(6) . ? P2 C211 1.823(6) . ? C111 C112 1.520(8) . ? C111 H11A 0.9700 . ? C111 H11B 0.9700 . ? C112 C211 1.527(8) . ? C112 H11C 0.9700 . ? C112 H11D 0.9700 . ? C121 C122 1.374(9) . ? C121 C126 1.407(9) . ? C122 C123 1.393(10) . ? C122 H122 0.9300 . ? C123 C124 1.376(10) . ? C123 H123 0.9300 . ? C124 C125 1.380(11) . ? C124 H124 0.9300 . ? C125 C126 1.378(10) . ? C125 H125 0.9300 . ? C126 H126 0.9300 . ? C131 C132 1.381(10) . ? C131 C136 1.390(9) . ? C132 C133 1.375(12) . ? C132 H132 0.9300 . ? C133 C134 1.339(13) . ? C133 H133 0.9300 . ? C134 C135 1.365(14) . ? C134 H134 0.9300 . ? C135 C136 1.392(12) . ? C135 H135 0.9300 . ? C136 H136 0.9300 . ? C211 H21A 0.9700 . ? C211 H21B 0.9700 . ? C221 C226 1.391(9) . ? C221 C222 1.396(9) . ? C222 C223 1.388(10) . ? C222 H222 0.9300 . ? C223 C224 1.384(11) . ? C223 H223 0.9300 . ? C224 C225 1.374(11) . ? C224 H224 0.9300 . ? C225 C226 1.393(9) . ? C225 H225 0.9300 . ? C226 H226 0.9300 . ? C231 C232 1.395(9) . ? C231 C236 1.402(9) . ? C232 C233 1.386(9) . ? C232 H232 0.9300 . ? C233 C234 1.374(11) . ? C233 H233 0.9300 . ? C234 C235 1.377(10) . ? C234 H234 0.9300 . ? C235 C236 1.369(9) . ? C235 H235 0.9300 . ? C236 H236 0.9300 . ? B101 B106 1.752(11) . ? B101 B110 1.752(13) . ? B101 B105 1.904(11) . ? B101 B102 1.915(12) . ? B101 H101 1.1000 . ? B102 B107 1.773(11) . ? B102 B106 1.785(12) . ? B102 B103 1.882(11) . ? B102 H102 1.1000 . ? B103 B108 1.763(11) . ? B103 B107 1.764(11) . ? B103 B104 1.893(11) . ? B103 H103 1.1000 . ? B104 B109 1.750(11) . ? B104 B108 1.772(11) . ? B104 B105 1.879(11) . ? B104 H104 1.1000 . ? B105 B109 1.753(11) . ? B105 B110 1.768(11) . ? B105 H105 1.1000 . ? B106 B111 1.753(12) . ? B106 B110 1.757(12) . ? B106 B107 1.786(11) . ? B106 H106 1.1000 . ? B107 B111 1.759(12) . ? B107 B108 1.784(11) . ? B107 H107 1.1000 . ? B108 B109 1.758(11) . ? B108 B111 1.764(12) . ? B108 H108 1.1000 . ? B109 B111 1.788(11) . ? B109 B110 1.792(12) . ? B109 H109 1.1000 . ? B110 B111 1.785(11) . ? B110 H110 1.1000 . ? B111 H111 1.1000 . ? B201 B206 1.748(10) . ? B201 B210 1.751(11) . ? B201 B205 1.903(11) . ? B201 B202 1.928(11) . ? B201 H201 1.1000 . ? B202 B207 1.756(11) . ? B202 B206 1.768(10) . ? B202 B203 1.917(11) . ? B202 H202 1.1000 . ? B203 B208 1.770(10) . ? B203 B207 1.774(11) . ? B203 B204 1.926(11) . ? B203 H203 1.1000 . ? B204 B209 1.775(11) . ? B204 B208 1.781(11) . ? B204 B205 1.886(11) . ? B204 H204 1.1000 . ? B205 B210 1.750(11) . ? B205 B209 1.765(11) . ? B205 H205 1.1000 . ? B206 B211 1.771(11) . ? B206 B210 1.778(10) . ? B206 B207 1.783(11) . ? B206 H206 1.1000 . ? B207 B211 1.768(11) . ? B207 B208 1.782(11) . ? B207 H207 1.1000 . ? B208 B211 1.777(11) . ? B208 B209 1.780(11) . ? B208 H208 1.1000 . ? B209 B210 1.770(11) . ? B209 B211 1.779(11) . ? B209 H209 1.1000 . ? B210 B211 1.771(11) . ? B210 H210 1.1000 . ? B211 H211 1.1000 . ? N1 C107 1.510(9) . ? N1 C101 1.523(9) . ? N1 C103 1.524(8) . ? N1 C105 1.527(8) . ? C101 C102 1.504(11) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C102 H10C 0.9600 . ? C102 H10D 0.9600 . ? C102 H10E 0.9600 . ? C103 C104 1.494(10) . ? C103 H10F 0.9700 . ? C103 H10G 0.9700 . ? C104 H10H 0.9600 . ? C104 H10I 0.9600 . ? C104 H10J 0.9600 . ? C105 C106 1.506(9) . ? C105 H10K 0.9700 . ? C105 H10L 0.9700 . ? C106 H10M 0.9600 . ? C106 H10N 0.9600 . ? C106 H10O 0.9600 . ? C107 C108 1.514(11) . ? C107 H10P 0.9700 . ? C107 H10Q 0.9700 . ? C108 H10R 0.9600 . ? C108 H10S 0.9600 . ? C108 H10T 0.9600 . ? N2 C205 1.513(9) . ? N2 C207 1.518(9) . ? N2 C201 1.520(9) . ? N2 C203 1.522(9) . ? C201 C202 1.520(11) . ? C201 H20A 0.9700 . ? C201 H20B 0.9700 . ? C202 H20C 0.9600 . ? C202 H20D 0.9600 . ? C202 H20E 0.9600 . ? C203 C204 1.502(11) . ? C203 H20F 0.9700 . ? C203 H20G 0.9700 . ? C204 H20H 0.9600 . ? C204 H20I 0.9600 . ? C204 H20J 0.9600 . ? C205 C206 1.516(11) . ? C205 H20K 0.9700 . ? C205 H20L 0.9700 . ? C206 H20M 0.9600 . ? C206 H20N 0.9600 . ? C206 H20O 0.9600 . ? C207 C208 1.512(11) . ? C207 H20P 0.9700 . ? C207 H20Q 0.9700 . ? C208 H20R 0.9600 . ? C208 H20S 0.9600 . ? C208 H20T 0.9600 . ? N3 C31 1.118(10) . ? C31 C32 1.454(12) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N5 C51 1.114(10) . ? C51 C52 1.451(12) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? N4 C41 1.109(11) . ? C41 C42 1.434(15) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 P1 Pt1 P2 95.85(6) . . ? P1 Pt1 S2 175.68(6) . . ? P2 Pt1 S2 88.10(5) . . ? P1 Pt1 S1 87.50(6) . . ? P2 Pt1 S1 174.38(6) . . ? S2 Pt1 S1 88.43(5) . . ? B102 Sn1 B105 83.6(3) . . ? B102 Sn1 B104 83.3(3) . . ? B105 Sn1 B104 48.1(3) . . ? B102 Sn1 B101 49.1(3) . . ? B105 Sn1 B101 48.7(3) . . ? B104 Sn1 B101 83.4(3) . . ? B102 Sn1 B103 48.2(3) . . ? B105 Sn1 B103 82.8(3) . . ? B104 Sn1 B103 48.3(3) . . ? B101 Sn1 B103 83.3(3) . . ? B102 Sn1 S1 128.1(2) . . ? B105 Sn1 S1 148.32(18) . . ? B104 Sn1 S1 125.9(2) . . ? B101 Sn1 S1 150.6(2) . . ? B103 Sn1 S1 116.6(2) . . ? B201 Sn2 B203 84.3(3) . . ? B201 Sn2 B205 48.9(3) . . ? B203 Sn2 B205 83.9(3) . . ? B201 Sn2 B204 83.9(3) . . ? B203 Sn2 B204 49.4(3) . . ? B205 Sn2 B204 48.2(3) . . ? B201 Sn2 B202 49.5(3) . . ? B203 Sn2 B202 49.1(3) . . ? B205 Sn2 B202 84.6(3) . . ? B204 Sn2 B202 84.8(3) . . ? B201 Sn2 S2 132.42(19) . . ? B203 Sn2 S2 143.1(2) . . ? B205 Sn2 S2 120.82(19) . . ? B204 Sn2 S2 125.8(2) . . ? B202 Sn2 S2 148.3(2) . . ? Sn1 S1 Pt1 94.55(5) . . ? Sn2 S2 Pt1 92.70(5) . . ? C131 P1 C121 108.5(3) . . ? C131 P1 C111 100.9(3) . . ? C121 P1 C111 104.3(3) . . ? C131 P1 Pt1 112.1(2) . . ? C121 P1 Pt1 112.9(2) . . ? C111 P1 Pt1 117.1(2) . . ? C221 P2 C231 108.6(3) . . ? C221 P2 C211 103.8(3) . . ? C231 P2 C211 101.8(3) . . ? C221 P2 Pt1 109.6(2) . . ? C231 P2 Pt1 114.8(2) . . ? C211 P2 Pt1 117.3(2) . . ? C112 C111 P1 115.1(4) . . ? C112 C111 H11A 108.5 . . ? P1 C111 H11A 108.5 . . ? C112 C111 H11B 108.5 . . ? P1 C111 H11B 108.5 . . ? H11A C111 H11B 107.5 . . ? C111 C112 C211 112.4(5) . . ? C111 C112 H11C 109.1 . . ? C211 C112 H11C 109.1 . . ? C111 C112 H11D 109.1 . . ? C211 C112 H11D 109.1 . . ? H11C C112 H11D 107.9 . . ? C122 C121 C126 119.0(6) . . ? C122 C121 P1 121.4(5) . . ? C126 C121 P1 119.6(5) . . ? C121 C122 C123 121.0(6) . . ? C121 C122 H122 119.5 . . ? C123 C122 H122 119.5 . . ? C124 C123 C122 119.3(7) . . ? C124 C123 H123 120.4 . . ? C122 C123 H123 120.4 . . ? C123 C124 C125 120.6(7) . . ? C123 C124 H124 119.7 . . ? C125 C124 H124 119.7 . . ? C126 C125 C124 120.1(7) . . ? C126 C125 H125 119.9 . . ? C124 C125 H125 119.9 . . ? C125 C126 C121 120.0(7) . . ? C125 C126 H126 120.0 . . ? C121 C126 H126 120.0 . . ? C132 C131 C136 117.9(7) . . ? C132 C131 P1 117.9(5) . . ? C136 C131 P1 124.2(6) . . ? C133 C132 C131 121.5(8) . . ? C133 C132 H132 119.2 . . ? C131 C132 H132 119.2 . . ? C134 C133 C132 119.9(9) . . ? C134 C133 H133 120.0 . . ? C132 C133 H133 120.0 . . ? C133 C134 C135 120.7(8) . . ? C133 C134 H134 119.6 . . ? C135 C134 H134 119.6 . . ? C134 C135 C136 120.2(8) . . ? C134 C135 H135 119.9 . . ? C136 C135 H135 119.9 . . ? C135 C136 C131 119.6(8) . . ? C135 C136 H136 120.2 . . ? C131 C136 H136 120.2 . . ? C112 C211 P2 114.7(4) . . ? C112 C211 H21A 108.6 . . ? P2 C211 H21A 108.6 . . ? C112 C211 H21B 108.6 . . ? P2 C211 H21B 108.6 . . ? H21A C211 H21B 107.6 . . ? C226 C221 C222 118.6(6) . . ? C226 C221 P2 120.1(5) . . ? C222 C221 P2 121.2(5) . . ? C223 C222 C221 120.0(7) . . ? C223 C222 H222 120.0 . . ? C221 C222 H222 120.0 . . ? C224 C223 C222 120.6(7) . . ? C224 C223 H223 119.7 . . ? C222 C223 H223 119.7 . . ? C225 C224 C223 119.9(7) . . ? C225 C224 H224 120.0 . . ? C223 C224 H224 120.0 . . ? C224 C225 C226 119.9(7) . . ? C224 C225 H225 120.1 . . ? C226 C225 H225 120.1 . . ? C221 C226 C225 120.9(6) . . ? C221 C226 H226 119.6 . . ? C225 C226 H226 119.6 . . ? C232 C231 C236 118.2(6) . . ? C232 C231 P2 124.2(5) . . ? C236 C231 P2 117.6(5) . . ? C233 C232 C231 120.0(7) . . ? C233 C232 H232 120.0 . . ? C231 C232 H232 120.0 . . ? C234 C233 C232 120.5(7) . . ? C234 C233 H233 119.7 . . ? C232 C233 H233 119.7 . . ? C233 C234 C235 120.1(7) . . ? C233 C234 H234 120.0 . . ? C235 C234 H234 120.0 . . ? C236 C235 C234 120.1(7) . . ? C236 C235 H235 120.0 . . ? C234 C235 H235 120.0 . . ? C235 C236 C231 121.0(6) . . ? C235 C236 H236 119.5 . . ? C231 C236 H236 119.5 . . ? B106 B101 B110 60.2(5) . . ? B106 B101 B105 105.4(5) . . ? B110 B101 B105 57.7(4) . . ? B106 B101 B102 58.0(4) . . ? B110 B101 B102 106.1(5) . . ? B105 B101 B102 106.5(5) . . ? B106 B101 Sn1 115.8(5) . . ? B110 B101 Sn1 116.1(5) . . ? B105 B101 Sn1 65.1(3) . . ? B102 B101 Sn1 64.8(3) . . ? B106 B101 H101 121.6 . . ? B110 B101 H101 121.3 . . ? B105 B101 H101 123.8 . . ? B102 B101 H101 123.4 . . ? Sn1 B101 H101 112.6 . . ? B107 B102 B106 60.3(5) . . ? B107 B102 B103 57.6(4) . . ? B106 B102 B103 105.5(6) . . ? B107 B102 B101 105.8(6) . . ? B106 B102 B101 56.4(4) . . ? B103 B102 B101 108.5(5) . . ? B107 B102 Sn1 117.3(4) . . ? B106 B102 Sn1 115.6(5) . . ? B103 B102 Sn1 66.6(3) . . ? B101 B102 Sn1 66.1(3) . . ? B107 B102 H102 121.3 . . ? B106 B102 H102 122.6 . . ? B103 B102 H102 122.5 . . ? B101 B102 H102 123.1 . . ? Sn1 B102 H102 111.3 . . ? B108 B103 B107 60.8(4) . . ? B108 B103 B102 106.7(6) . . ? B107 B103 B102 58.1(4) . . ? B108 B103 B104 57.8(4) . . ? B107 B103 B104 106.8(5) . . ? B102 B103 B104 108.1(5) . . ? B108 B103 Sn1 116.3(5) . . ? B107 B103 Sn1 116.4(5) . . ? B102 B103 Sn1 65.2(3) . . ? B104 B103 Sn1 65.6(3) . . ? B108 B103 H103 121.2 . . ? B107 B103 H103 121.0 . . ? B102 B103 H103 122.8 . . ? B104 B103 H103 122.7 . . ? Sn1 B103 H103 112.3 . . ? B109 B104 B108 59.9(5) . . ? B109 B104 B105 57.6(4) . . ? B108 B104 B105 105.8(5) . . ? B109 B104 B103 105.6(5) . . ? B108 B104 B103 57.4(4) . . ? B105 B104 B103 108.0(5) . . ? B109 B104 Sn1 116.3(5) . . ? B108 B104 Sn1 116.4(4) . . ? B105 B104 Sn1 65.7(3) . . ? B103 B104 Sn1 66.1(3) . . ? B109 B104 H104 121.8 . . ? B108 B104 H104 121.8 . . ? B105 B104 H104 122.9 . . ? B103 B104 H104 122.9 . . ? Sn1 B104 H104 111.7 . . ? B109 B105 B110 61.2(5) . . ? B109 B105 B104 57.5(4) . . ? B110 B105 B104 106.9(5) . . ? B109 B105 B101 106.3(5) . . ? B110 B105 B101 56.8(5) . . ? B104 B105 B101 108.9(5) . . ? B109 B105 Sn1 116.6(5) . . ? B110 B105 Sn1 116.3(5) . . ? B104 B105 Sn1 66.2(3) . . ? B101 B105 Sn1 66.2(3) . . ? B109 B105 H105 121.3 . . ? B110 B105 H105 121.4 . . ? B104 B105 H105 122.3 . . ? B101 B105 H105 122.8 . . ? Sn1 B105 H105 111.6 . . ? B101 B106 B111 111.0(6) . . ? B101 B106 B110 59.9(5) . . ? B111 B106 B110 61.1(5) . . ? B101 B106 B102 65.5(5) . . ? B111 B106 B102 109.3(5) . . ? B110 B106 B102 111.8(5) . . ? B101 B106 B107 112.5(5) . . ? B111 B106 B107 59.6(4) . . ? B110 B106 B107 109.0(6) . . ? B102 B106 B107 59.5(4) . . ? B101 B106 H106 117.9 . . ? B111 B106 H106 121.2 . . ? B110 B106 H106 120.9 . . ? B102 B106 H106 119.1 . . ? B107 B106 H106 121.3 . . ? B111 B107 B103 109.3(5) . . ? B111 B107 B102 109.5(6) . . ? B103 B107 B102 64.3(4) . . ? B111 B107 B108 59.7(5) . . ? B103 B107 B108 59.6(4) . . ? B102 B107 B108 110.7(5) . . ? B111 B107 B106 59.3(5) . . ? B103 B107 B106 110.7(5) . . ? B102 B107 B106 60.2(5) . . ? B108 B107 B106 106.8(5) . . ? B111 B107 H107 121.8 . . ? B103 B107 H107 119.3 . . ? B102 B107 H107 119.0 . . ? B108 B107 H107 122.2 . . ? B106 B107 H107 122.1 . . ? B109 B108 B111 61.0(5) . . ? B109 B108 B103 111.1(6) . . ? B111 B108 B103 109.1(6) . . ? B109 B108 B104 59.4(4) . . ? B111 B108 B104 110.1(6) . . ? B103 B108 B104 64.8(5) . . ? B109 B108 B107 108.5(6) . . ? B111 B108 B107 59.4(5) . . ? B103 B108 B107 59.6(4) . . ? B104 B108 B107 111.4(6) . . ? B109 B108 H108 121.2 . . ? B111 B108 H108 121.4 . . ? B103 B108 H108 119.4 . . ? B104 B108 H108 118.9 . . ? B107 B108 H108 121.6 . . ? B104 B109 B105 64.9(5) . . ? B104 B109 B108 60.7(5) . . ? B105 B109 B108 112.1(6) . . ? B104 B109 B111 109.9(6) . . ? B105 B109 B111 109.5(6) . . ? B108 B109 B111 59.6(4) . . ? B104 B109 B110 111.7(6) . . ? B105 B109 B110 59.8(4) . . ? B108 B109 B110 108.2(6) . . ? B111 B109 B110 59.8(5) . . ? B104 B109 H109 118.5 . . ? B105 B109 H109 118.8 . . ? B108 B109 H109 121.1 . . ? B111 B109 H109 121.9 . . ? B110 B109 H109 121.6 . . ? B101 B110 B106 59.9(5) . . ? B101 B110 B105 65.5(5) . . ? B106 B110 B105 111.2(6) . . ? B101 B110 B111 109.5(6) . . ? B106 B110 B111 59.3(5) . . ? B105 B110 B111 109.0(6) . . ? B101 B110 B109 111.4(6) . . ? B106 B110 B109 107.4(5) . . ? B105 B110 B109 59.0(4) . . ? B111 B110 B109 60.0(5) . . ? B101 B110 H110 118.5 . . ? B106 B110 H110 121.9 . . ? B105 B110 H110 119.2 . . ? B111 B110 H110 122.0 . . ? B109 B110 H110 122.0 . . ? B106 B111 B107 61.1(5) . . ? B106 B111 B108 109.2(6) . . ? B107 B111 B108 60.9(5) . . ? B106 B111 B110 59.5(5) . . ? B107 B111 B110 108.9(6) . . ? B108 B111 B110 108.2(5) . . ? B106 B111 B109 107.8(5) . . ? B107 B111 B109 108.3(6) . . ? B108 B111 B109 59.3(5) . . ? B110 B111 B109 60.2(5) . . ? B106 B111 H111 121.3 . . ? B107 B111 H111 120.7 . . ? B108 B111 H111 121.3 . . ? B110 B111 H111 121.6 . . ? B109 B111 H111 122.2 . . ? B206 B201 B210 61.1(4) . . ? B206 B201 B205 106.4(5) . . ? B210 B201 B205 57.1(4) . . ? B206 B201 B202 57.2(4) . . ? B210 B201 B202 106.4(5) . . ? B205 B201 B202 108.5(5) . . ? B206 B201 Sn2 116.0(4) . . ? B210 B201 Sn2 115.9(5) . . ? B205 B201 Sn2 65.9(3) . . ? B202 B201 Sn2 65.8(3) . . ? B206 B201 H201 121.4 . . ? B210 B201 H201 121.5 . . ? B205 B201 H201 122.7 . . ? B202 B201 H201 122.7 . . ? Sn2 B201 H201 112.1 . . ? B207 B202 B206 60.8(4) . . ? B207 B202 B203 57.6(4) . . ? B206 B202 B203 105.9(5) . . ? B207 B202 B201 104.8(5) . . ? B206 B202 B201 56.2(4) . . ? B203 B202 B201 106.6(5) . . ? B207 B202 Sn2 115.1(5) . . ? B206 B202 Sn2 114.2(4) . . ? B203 B202 Sn2 65.1(3) . . ? B201 B202 Sn2 64.7(3) . . ? B207 B202 H202 121.6 . . ? B206 B202 H202 122.1 . . ? B203 B202 H202 123.1 . . ? B201 B202 H202 124.3 . . ? Sn2 B202 H202 113.3 . . ? B208 B203 B207 60.4(4) . . ? B208 B203 B202 105.8(5) . . ? B207 B203 B202 56.7(4) . . ? B208 B203 B204 57.4(4) . . ? B207 B203 B204 105.8(5) . . ? B202 B203 B204 108.5(5) . . ? B208 B203 Sn2 115.7(5) . . ? B207 B203 Sn2 115.1(5) . . ? B202 B203 Sn2 65.8(3) . . ? B204 B203 Sn2 65.6(3) . . ? B208 B203 H203 121.7 . . ? B207 B203 H203 122.3 . . ? B202 B203 H203 122.9 . . ? B204 B203 H203 122.6 . . ? Sn2 B203 H203 112.5 . . ? B209 B204 B208 60.1(4) . . ? B209 B204 B205 57.6(4) . . ? B208 B204 B205 105.5(5) . . ? B209 B204 B203 105.5(5) . . ? B208 B204 B203 56.9(4) . . ? B205 B204 B203 107.7(5) . . ? B209 B204 Sn2 115.7(5) . . ? B208 B204 Sn2 114.6(4) . . ? B205 B204 Sn2 65.7(3) . . ? B203 B204 Sn2 65.0(3) . . ? B209 B204 H204 121.7 . . ? B208 B204 H204 122.4 . . ? B205 B204 H204 122.8 . . ? B203 B204 H204 123.4 . . ? Sn2 B204 H204 112.8 . . ? B210 B205 B209 60.5(4) . . ? B210 B205 B204 106.8(5) . . ? B209 B205 B204 58.1(4) . . ? B210 B205 B201 57.1(4) . . ? B209 B205 B201 106.0(5) . . ? B204 B205 B201 108.7(5) . . ? B210 B205 Sn2 115.3(4) . . ? B209 B205 Sn2 116.4(4) . . ? B204 B205 Sn2 66.0(3) . . ? B201 B205 Sn2 65.2(3) . . ? B210 B205 H205 121.8 . . ? B209 B205 H205 121.3 . . ? B204 B205 H205 122.0 . . ? B201 B205 H205 123.1 . . ? Sn2 B205 H205 112.4 . . ? B201 B206 B202 66.5(4) . . ? B201 B206 B211 109.7(5) . . ? B202 B206 B211 109.8(6) . . ? B201 B206 B210 59.5(4) . . ? B202 B206 B210 112.5(5) . . ? B211 B206 B210 59.9(4) . . ? B201 B206 B207 111.7(5) . . ? B202 B206 B207 59.3(4) . . ? B211 B206 B207 59.6(4) . . ? B210 B206 B207 107.5(5) . . ? B201 B206 H206 118.3 . . ? B202 B206 H206 118.1 . . ? B211 B206 H206 121.8 . . ? B210 B206 H206 121.6 . . ? B207 B206 H206 122.2 . . ? B202 B207 B211 110.5(5) . . ? B202 B207 B203 65.8(4) . . ? B211 B207 B203 109.9(6) . . ? B202 B207 B208 112.5(6) . . ? B211 B207 B208 60.1(4) . . ? B203 B207 B208 59.7(4) . . ? B202 B207 B206 59.9(4) . . ? B211 B207 B206 59.8(4) . . ? B203 B207 B206 111.6(5) . . ? B208 B207 B206 107.9(5) . . ? B202 B207 H207 117.9 . . ? B211 B207 H207 121.4 . . ? B203 B207 H207 118.6 . . ? B208 B207 H207 121.4 . . ? B206 B207 H207 121.8 . . ? B203 B208 B211 109.7(5) . . ? B203 B208 B209 112.2(5) . . ? B211 B208 B209 60.0(4) . . ? B203 B208 B207 59.9(4) . . ? B211 B208 B207 59.6(4) . . ? B209 B208 B207 108.1(5) . . ? B203 B208 B204 65.7(4) . . ? B211 B208 B204 109.7(5) . . ? B209 B208 B204 59.8(4) . . ? B207 B208 B204 111.9(5) . . ? B203 B208 H208 118.3 . . ? B211 B208 H208 121.9 . . ? B209 B208 H208 121.4 . . ? B207 B208 H208 121.6 . . ? B204 B208 H208 118.5 . . ? B205 B209 B210 59.4(4) . . ? B205 B209 B204 64.4(5) . . ? B210 B209 B204 110.9(5) . . ? B205 B209 B211 109.1(5) . . ? B210 B209 B211 59.9(4) . . ? B204 B209 B211 109.9(5) . . ? B205 B209 B208 110.9(5) . . ? B210 B209 B208 107.7(5) . . ? B204 B209 B208 60.1(4) . . ? B211 B209 B208 59.9(4) . . ? B205 B209 H209 119.5 . . ? B210 B209 H209 122.0 . . ? B204 B209 H209 118.9 . . ? B211 B209 H209 121.5 . . ? B208 B209 H209 121.6 . . ? B201 B210 B205 65.8(5) . . ? B201 B210 B211 109.6(5) . . ? B205 B210 B211 110.2(5) . . ? B201 B210 B209 112.7(5) . . ? B205 B210 B209 60.2(5) . . ? B211 B210 B209 60.3(4) . . ? B201 B210 B206 59.4(4) . . ? B205 B210 B206 112.0(5) . . ? B211 B210 B206 59.9(4) . . ? B209 B210 B206 108.7(5) . . ? B201 B210 H210 118.5 . . ? B205 B210 H210 118.2 . . ? B211 B210 H210 121.6 . . ? B209 B210 H210 120.8 . . ? B206 B210 H210 121.6 . . ? B207 B211 B210 108.5(5) . . ? B207 B211 B206 60.5(4) . . ? B210 B211 B206 60.3(4) . . ? B207 B211 B208 60.4(4) . . ? B210 B211 B208 107.8(6) . . ? B206 B211 B208 108.7(5) . . ? B207 B211 B209 108.8(6) . . ? B210 B211 B209 59.8(4) . . ? B206 B211 B209 108.7(5) . . ? B208 B211 B209 60.1(4) . . ? B207 B211 H211 121.1 . . ? B210 B211 H211 121.8 . . ? B206 B211 H211 121.1 . . ? B208 B211 H211 121.6 . . ? B209 B211 H211 121.4 . . ? C107 N1 C101 106.5(5) . . ? C107 N1 C103 110.9(5) . . ? C101 N1 C103 111.8(5) . . ? C107 N1 C105 111.1(5) . . ? C101 N1 C105 110.3(5) . . ? C103 N1 C105 106.4(5) . . ? C102 C101 N1 116.1(6) . . ? C102 C101 H10A 108.3 . . ? N1 C101 H10A 108.3 . . ? C102 C101 H10B 108.3 . . ? N1 C101 H10B 108.3 . . ? H10A C101 H10B 107.4 . . ? C101 C102 H10C 109.5 . . ? C101 C102 H10D 109.5 . . ? H10C C102 H10D 109.5 . . ? C101 C102 H10E 109.5 . . ? H10C C102 H10E 109.5 . . ? H10D C102 H10E 109.5 . . ? C104 C103 N1 116.4(6) . . ? C104 C103 H10F 108.2 . . ? N1 C103 H10F 108.2 . . ? C104 C103 H10G 108.2 . . ? N1 C103 H10G 108.2 . . ? H10F C103 H10G 107.3 . . ? C103 C104 H10H 109.5 . . ? C103 C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? C103 C104 H10J 109.5 . . ? H10H C104 H10J 109.5 . . ? H10I C104 H10J 109.5 . . ? C106 C105 N1 116.0(5) . . ? C106 C105 H10K 108.3 . . ? N1 C105 H10K 108.3 . . ? C106 C105 H10L 108.3 . . ? N1 C105 H10L 108.3 . . ? H10K C105 H10L 107.4 . . ? C105 C106 H10M 109.5 . . ? C105 C106 H10N 109.5 . . ? H10M C106 H10N 109.5 . . ? C105 C106 H10O 109.5 . . ? H10M C106 H10O 109.5 . . ? H10N C106 H10O 109.5 . . ? N1 C107 C108 115.9(6) . . ? N1 C107 H10P 108.3 . . ? C108 C107 H10P 108.3 . . ? N1 C107 H10Q 108.3 . . ? C108 C107 H10Q 108.3 . . ? H10P C107 H10Q 107.4 . . ? C107 C108 H10R 109.5 . . ? C107 C108 H10S 109.5 . . ? H10R C108 H10S 109.5 . . ? C107 C108 H10T 109.5 . . ? H10R C108 H10T 109.5 . . ? H10S C108 H10T 109.5 . . ? C205 N2 C207 111.8(6) . . ? C205 N2 C201 111.1(6) . . ? C207 N2 C201 106.7(5) . . ? C205 N2 C203 106.5(5) . . ? C207 N2 C203 111.3(6) . . ? C201 N2 C203 109.6(6) . . ? C202 C201 N2 115.9(6) . . ? C202 C201 H20A 108.3 . . ? N2 C201 H20A 108.3 . . ? C202 C201 H20B 108.3 . . ? N2 C201 H20B 108.3 . . ? H20A C201 H20B 107.4 . . ? C201 C202 H20C 109.5 . . ? C201 C202 H20D 109.5 . . ? H20C C202 H20D 109.5 . . ? C201 C202 H20E 109.5 . . ? H20C C202 H20E 109.5 . . ? H20D C202 H20E 109.5 . . ? C204 C203 N2 116.0(6) . . ? C204 C203 H20F 108.3 . . ? N2 C203 H20F 108.3 . . ? C204 C203 H20G 108.3 . . ? N2 C203 H20G 108.3 . . ? H20F C203 H20G 107.4 . . ? C203 C204 H20H 109.5 . . ? C203 C204 H20I 109.5 . . ? H20H C204 H20I 109.5 . . ? C203 C204 H20J 109.5 . . ? H20H C204 H20J 109.5 . . ? H20I C204 H20J 109.5 . . ? N2 C205 C206 114.4(6) . . ? N2 C205 H20K 108.7 . . ? C206 C205 H20K 108.7 . . ? N2 C205 H20L 108.7 . . ? C206 C205 H20L 108.7 . . ? H20K C205 H20L 107.6 . . ? C205 C206 H20M 109.5 . . ? C205 C206 H20N 109.5 . . ? H20M C206 H20N 109.5 . . ? C205 C206 H20O 109.5 . . ? H20M C206 H20O 109.5 . . ? H20N C206 H20O 109.5 . . ? C208 C207 N2 114.8(6) . . ? C208 C207 H20P 108.6 . . ? N2 C207 H20P 108.6 . . ? C208 C207 H20Q 108.6 . . ? N2 C207 H20Q 108.6 . . ? H20P C207 H20Q 107.5 . . ? C207 C208 H20R 109.5 . . ? C207 C208 H20S 109.5 . . ? H20R C208 H20S 109.5 . . ? C207 C208 H20T 109.5 . . ? H20R C208 H20T 109.5 . . ? H20S C208 H20T 109.5 . . ? N3 C31 C32 178.3(10) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N5 C51 C52 178.6(11) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N4 C41 C42 176.2(13) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.453 _refine_diff_density_min -0.927 _refine_diff_density_rms 0.119 # Attachment '765676_compound_7.cif' data_hornung117 _database_code_depnum_ccdc_archive 'CCDC 765676' #TrackingRef '765676_compound_7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B22 P2 Pd S2 Sn2, 2(C8 H20 N), 3(C2 H3 N)' _chemical_formula_sum 'C49 H97 B22 N5 P2 Pd S2 Sn2' _chemical_formula_weight 1464.04 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.2389(6) _cell_length_b 22.4120(15) _cell_length_c 26.2350(12) _cell_angle_alpha 90.00 _cell_angle_beta 101.540(4) _cell_angle_gamma 90.00 _cell_volume 7050.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 31424 _cell_measurement_theta_min 3.32 _cell_measurement_theta_max 54.38 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.1770 _exptl_crystal_size_mid 0.1660 _exptl_crystal_size_min 0.1203 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.097 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7889 _exptl_absorpt_correction_T_max 0.9301 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70966 _diffrn_reflns_av_R_equivalents 0.1427 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 5.67 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12717 _reflns_number_gt 9399 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXL-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep3 for windows' _computing_publication_material ? _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. Due to moderate crystal quality even after several attempts of crystallization the R(int) has a value >0.1 ; _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^)+(0.0332P)^2^+10.9588P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12717 _refine_ls_number_parameters 751 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0950 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1023 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _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 C221 C 0.0964(5) 0.8403(3) 0.1393(2) 0.0267(13) Uani 1 1 d . . . C231 C 0.2882(5) 0.8007(3) 0.2197(3) 0.0296(14) Uani 1 1 d . . . C121 C -0.1906(5) 0.8790(3) 0.2327(2) 0.0281(13) Uani 1 1 d . . . C111 C 0.0222(6) 0.9310(3) 0.2795(3) 0.0326(15) Uani 1 1 d . . . H11A H -0.0276 0.9631 0.2847 0.039 Uiso 1 1 calc R . . H11B H 0.0812 0.9289 0.3102 0.039 Uiso 1 1 calc R . . C122 C -0.2347(5) 0.8459(3) 0.1889(3) 0.0370(15) Uani 1 1 d . . . H122 H -0.1964 0.8126 0.1804 0.044 Uiso 1 1 calc R . . B201 B 0.1179(6) 0.6505(3) 0.3799(3) 0.0318(16) Uani 1 1 d . . . H201 H 0.0556 0.6833 0.3869 0.038 Uiso 1 1 calc R . . C226 C 0.1463(6) 0.8793(3) 0.1097(3) 0.0406(17) Uani 1 1 d . . . H226 H 0.2100 0.9004 0.1249 0.049 Uiso 1 1 calc R . . C223 C -0.0433(6) 0.8164(3) 0.0637(3) 0.0415(17) Uani 1 1 d . . . H223 H -0.1070 0.7954 0.0483 0.050 Uiso 1 1 calc R . . B202 B 0.0775(6) 0.5753(3) 0.3455(3) 0.0325(16) Uani 1 1 d . . . H202 H -0.0095 0.5614 0.3313 0.039 Uiso 1 1 calc R . . C131 C -0.0761(5) 0.8495(3) 0.3395(2) 0.0323(14) Uani 1 1 d . . . C211 C 0.1774(5) 0.9088(2) 0.2317(2) 0.0264(13) Uani 1 1 d . . . H21A H 0.2234 0.9077 0.2665 0.032 Uiso 1 1 calc R . . H21B H 0.2202 0.9285 0.2092 0.032 Uiso 1 1 calc R . . C123 C -0.3350(6) 0.8617(3) 0.1577(3) 0.0435(17) Uani 1 1 d . . . H123 H -0.3637 0.8395 0.1282 0.052 Uiso 1 1 calc R . . C222 C 0.0021(5) 0.8089(3) 0.1158(2) 0.0336(14) Uani 1 1 d . . . H222 H -0.0310 0.7825 0.1354 0.040 Uiso 1 1 calc R . . N1 N 0.2352(4) 0.5880(2) 0.0758(2) 0.0311(12) Uani 1 1 d . . . N2 N 0.7288(4) 0.5769(2) 0.4002(2) 0.0347(13) Uani 1 1 d . . . C234 C 0.5041(6) 0.7551(3) 0.2428(3) 0.0459(18) Uani 1 1 d . . . H234 H 0.5770 0.7410 0.2507 0.055 Uiso 1 1 calc R . . C232 C 0.3386(6) 0.7870(3) 0.2706(3) 0.0383(15) Uani 1 1 d . . . H232 H 0.3001 0.7933 0.2973 0.046 Uiso 1 1 calc R . . C102 C 0.1641(6) 0.6957(3) 0.0746(3) 0.0453(18) Uani 1 1 d . . . H10A H 0.1804 0.7354 0.0646 0.068 Uiso 1 1 calc R . . H10B H 0.1653 0.6947 0.1113 0.068 Uiso 1 1 calc R . . H10C H 0.0916 0.6841 0.0559 0.068 Uiso 1 1 calc R . . C101 C 0.2504(5) 0.6532(3) 0.0621(3) 0.0371(15) Uani 1 1 d . . . H10D H 0.3233 0.6663 0.0805 0.044 Uiso 1 1 calc R . . H10E H 0.2499 0.6558 0.0251 0.044 Uiso 1 1 calc R . . C112 C 0.0735(5) 0.9462(2) 0.2332(2) 0.0283(13) Uani 1 1 d . . . H11C H 0.0933 0.9881 0.2346 0.034 Uiso 1 1 calc R . . H11D H 0.0188 0.9395 0.2014 0.034 Uiso 1 1 calc R . . C233 C 0.4460(6) 0.7642(3) 0.2820(3) 0.0435(17) Uani 1 1 d . . . H233 H 0.4789 0.7549 0.3162 0.052 Uiso 1 1 calc R . . C103 C 0.2349(6) 0.5808(3) 0.1331(3) 0.0377(16) Uani 1 1 d . . . H10F H 0.2259 0.5388 0.1401 0.045 Uiso 1 1 calc R . . H10G H 0.1703 0.6016 0.1406 0.045 Uiso 1 1 calc R . . C224 C 0.0070(7) 0.8555(4) 0.0342(3) 0.052(2) Uani 1 1 d . . . H224 H -0.0224 0.8606 -0.0010 0.063 Uiso 1 1 calc R . . C201 C 0.7272(6) 0.5749(4) 0.3424(3) 0.051(2) Uani 1 1 d . . . H20A H 0.7836 0.6021 0.3350 0.061 Uiso 1 1 calc R . . H20B H 0.7480 0.5350 0.3336 0.061 Uiso 1 1 calc R . . C105 C 0.3302(6) 0.5536(3) 0.0601(3) 0.0398(16) Uani 1 1 d . . . H10H H 0.3267 0.5599 0.0233 0.048 Uiso 1 1 calc R . . H10I H 0.4000 0.5705 0.0786 0.048 Uiso 1 1 calc R . . C124 C -0.3931(6) 0.9107(3) 0.1703(3) 0.0466(18) Uani 1 1 d . . . H124 H -0.4608 0.9215 0.1494 0.056 Uiso 1 1 calc R . . C132 C 0.0183(7) 0.8448(4) 0.3778(3) 0.064(2) Uani 1 1 d . . . H132 H 0.0881 0.8450 0.3688 0.076 Uiso 1 1 calc R . . C205 C 0.8461(6) 0.5610(4) 0.4273(3) 0.051(2) Uani 1 1 d . . . H20C H 0.8970 0.5904 0.4180 0.062 Uiso 1 1 calc R . . H20D H 0.8653 0.5226 0.4145 0.062 Uiso 1 1 calc R . . C203 C 0.6437(6) 0.5341(3) 0.4148(3) 0.0465(18) Uani 1 1 d . . . H20E H 0.5703 0.5454 0.3957 0.056 Uiso 1 1 calc R . . H20F H 0.6438 0.5388 0.4516 0.056 Uiso 1 1 calc R . . C236 C 0.3474(5) 0.7903(3) 0.1801(3) 0.0369(15) Uani 1 1 d . . . H236 H 0.3149 0.7992 0.1457 0.044 Uiso 1 1 calc R . . C106 C 0.3323(7) 0.4876(3) 0.0702(3) 0.052(2) Uani 1 1 d . . . H10J H 0.3949 0.4702 0.0588 0.078 Uiso 1 1 calc R . . H10K H 0.2646 0.4700 0.0515 0.078 Uiso 1 1 calc R . . H10L H 0.3387 0.4806 0.1068 0.078 Uiso 1 1 calc R . . C125 C -0.3505(6) 0.9430(3) 0.2135(3) 0.0455(18) Uani 1 1 d . . . H125 H -0.3907 0.9755 0.2220 0.055 Uiso 1 1 calc R . . C107 C 0.1232(6) 0.5647(3) 0.0471(3) 0.0466(18) Uani 1 1 d . . . H10M H 0.1161 0.5234 0.0571 0.056 Uiso 1 1 calc R . . H10N H 0.0648 0.5871 0.0586 0.056 Uiso 1 1 calc R . . C235 C 0.4544(6) 0.7668(3) 0.1920(3) 0.0467(18) Uani 1 1 d . . . H235 H 0.4928 0.7590 0.1655 0.056 Uiso 1 1 calc R . . B205 B 0.2643(6) 0.6712(3) 0.3683(3) 0.0307(16) Uani 1 1 d . . . H205 H 0.2944 0.7174 0.3681 0.037 Uiso 1 1 calc R . . C104 C 0.3380(7) 0.6036(4) 0.1702(3) 0.055(2) Uani 1 1 d . . . H10O H 0.3298 0.5971 0.2054 0.083 Uiso 1 1 calc R . . H10P H 0.3468 0.6455 0.1645 0.083 Uiso 1 1 calc R . . H10Q H 0.4024 0.5825 0.1641 0.083 Uiso 1 1 calc R . . C126 C -0.2501(6) 0.9292(3) 0.2452(3) 0.0394(16) Uani 1 1 d . . . H126 H -0.2218 0.9525 0.2742 0.047 Uiso 1 1 calc R . . C108 C 0.1039(7) 0.5679(3) -0.0114(3) 0.057(2) Uani 1 1 d . . . H10R H 0.0314 0.5522 -0.0260 0.085 Uiso 1 1 calc R . . H10S H 0.1597 0.5448 -0.0234 0.085 Uiso 1 1 calc R . . H10T H 0.1084 0.6087 -0.0219 0.085 Uiso 1 1 calc R . . C207 C 0.6970(7) 0.6382(3) 0.4162(4) 0.056(2) Uani 1 1 d . . . H20G H 0.6994 0.6382 0.4533 0.068 Uiso 1 1 calc R . . H20H H 0.6206 0.6464 0.3989 0.068 Uiso 1 1 calc R . . B203 B 0.1978(6) 0.5511(3) 0.3128(3) 0.0320(16) Uani 1 1 d . . . H203 H 0.1857 0.5224 0.2781 0.038 Uiso 1 1 calc R . . C206 C 0.8637(7) 0.5580(4) 0.4864(3) 0.062(2) Uani 1 1 d . . . H20I H 0.9398 0.5475 0.5006 0.093 Uiso 1 1 calc R . . H20J H 0.8150 0.5284 0.4962 0.093 Uiso 1 1 calc R . . H20K H 0.8474 0.5962 0.4997 0.093 Uiso 1 1 calc R . . B204 B 0.3110(6) 0.6102(3) 0.3273(3) 0.0307(16) Uani 1 1 d . . . H204 H 0.3696 0.6183 0.3012 0.037 Uiso 1 1 calc R . . B210 B 0.2421(6) 0.6376(3) 0.4258(3) 0.0293(16) Uani 1 1 d . . . H210 H 0.2571 0.6641 0.4618 0.035 Uiso 1 1 calc R . . B209 B 0.3536(6) 0.6133(3) 0.3952(3) 0.0320(16) Uani 1 1 d . . . H209 H 0.4412 0.6240 0.4119 0.038 Uiso 1 1 calc R . . B104 B -0.3406(6) 0.6360(3) 0.1660(3) 0.0339(17) Uani 1 1 d . . . H104 H -0.3941 0.6521 0.1921 0.041 Uiso 1 1 calc R . . B208 B 0.3159(6) 0.5439(3) 0.3637(3) 0.0319(16) Uani 1 1 d . . . H208 H 0.3787 0.5098 0.3601 0.038 Uiso 1 1 calc R . . B107 B -0.2375(7) 0.5347(3) 0.1229(3) 0.0377(18) Uani 1 1 d . . . H107 H -0.2242 0.4861 0.1229 0.045 Uiso 1 1 calc R . . B211 B 0.2783(6) 0.5603(3) 0.4242(3) 0.0327(16) Uani 1 1 d . . . H211 H 0.3170 0.5366 0.4600 0.039 Uiso 1 1 calc R . . B101 B -0.1488(6) 0.6528(4) 0.1085(3) 0.0354(17) Uani 1 1 d . . . H101 H -0.0814 0.6799 0.0983 0.042 Uiso 1 1 calc R . . B102 B -0.1211(7) 0.5809(4) 0.1463(4) 0.043(2) Uani 1 1 d . . . H102 H -0.0371 0.5623 0.1597 0.051 Uiso 1 1 calc R . . C225 C 0.1003(7) 0.8865(4) 0.0576(3) 0.051(2) Uani 1 1 d . . . H225 H 0.1333 0.9130 0.0379 0.062 Uiso 1 1 calc R . . B207 B 0.1817(6) 0.5237(3) 0.3743(3) 0.0381(18) Uani 1 1 d . . . H207 H 0.1578 0.4768 0.3776 0.046 Uiso 1 1 calc R . . B206 B 0.1368(6) 0.5819(4) 0.4131(3) 0.0370(18) Uani 1 1 d . . . H206 H 0.0841 0.5722 0.4414 0.044 Uiso 1 1 calc R . . B103 B -0.2414(7) 0.5712(3) 0.1826(3) 0.0386(18) Uani 1 1 d . . . H103 H -0.2326 0.5466 0.2195 0.046 Uiso 1 1 calc R . . B106 B -0.1842(6) 0.5821(4) 0.0796(3) 0.0391(19) Uani 1 1 d . . . H106 H -0.1373 0.5646 0.0512 0.047 Uiso 1 1 calc R . . C136 C -0.1788(7) 0.8475(3) 0.3527(3) 0.056(2) Uani 1 1 d . . . H136 H -0.2434 0.8494 0.3271 0.067 Uiso 1 1 calc R . . B110 B -0.2775(6) 0.6439(4) 0.0648(3) 0.0364(17) Uani 1 1 d . . . H110 H -0.2897 0.6665 0.0269 0.044 Uiso 1 1 calc R . . C134 C -0.0877(10) 0.8396(4) 0.4430(3) 0.066(3) Uani 1 1 d . . . H134 H -0.0916 0.8374 0.4780 0.079 Uiso 1 1 calc R . . B108 B -0.3649(6) 0.5660(3) 0.1343(3) 0.0358(17) Uani 1 1 d . . . H108 H -0.4338 0.5379 0.1416 0.043 Uiso 1 1 calc R . . B109 B -0.3889(6) 0.6336(3) 0.0977(3) 0.0347(17) Uani 1 1 d . . . H109 H -0.4735 0.6494 0.0809 0.042 Uiso 1 1 calc R . . B105 B -0.2841(6) 0.6866(3) 0.1206(3) 0.0337(17) Uani 1 1 d . . . H105 H -0.3021 0.7347 0.1182 0.040 Uiso 1 1 calc R . . C202 C 0.6176(7) 0.5906(5) 0.3077(3) 0.067(3) Uani 1 1 d . . . H20L H 0.6248 0.5880 0.2719 0.101 Uiso 1 1 calc R . . H20M H 0.5970 0.6305 0.3151 0.101 Uiso 1 1 calc R . . H20N H 0.5612 0.5632 0.3138 0.101 Uiso 1 1 calc R . . C135 C -0.1850(10) 0.8425(4) 0.4060(4) 0.081(3) Uani 1 1 d . . . H135 H -0.2538 0.8412 0.4159 0.098 Uiso 1 1 calc R . . C133 C 0.0110(9) 0.8399(5) 0.4297(3) 0.078(3) Uani 1 1 d . . . H133 H 0.0755 0.8369 0.4552 0.094 Uiso 1 1 calc R . . C204 C 0.6628(8) 0.4685(4) 0.4042(4) 0.068(3) Uani 1 1 d . . . H20O H 0.6058 0.4449 0.4148 0.102 Uiso 1 1 calc R . . H20P H 0.7346 0.4565 0.4234 0.102 Uiso 1 1 calc R . . H20Q H 0.6600 0.4629 0.3677 0.102 Uiso 1 1 calc R . . B111 B -0.3320(6) 0.5706(4) 0.0719(3) 0.0388(18) Uani 1 1 d . . . H111 H -0.3800 0.5455 0.0388 0.047 Uiso 1 1 calc R . . C208 C 0.7711(9) 0.6887(4) 0.4035(5) 0.079(3) Uani 1 1 d . . . H20R H 0.7461 0.7259 0.4152 0.118 Uiso 1 1 calc R . . H20S H 0.7670 0.6903 0.3666 0.118 Uiso 1 1 calc R . . H20T H 0.8468 0.6815 0.4208 0.118 Uiso 1 1 calc R . . N4 N 0.1439(9) 0.4211(4) 0.1344(3) 0.088(3) Uani 1 1 d . . . N5 N 0.5492(7) 0.7787(4) 0.4285(4) 0.095(3) Uani 1 1 d . . . C52 C 0.3672(7) 0.8043(4) 0.4567(4) 0.062(2) Uani 1 1 d . . . H52A H 0.3836 0.8198 0.4914 0.093 Uiso 1 1 calc R . . H52B H 0.3210 0.7695 0.4555 0.093 Uiso 1 1 calc R . . H52C H 0.3288 0.8341 0.4335 0.093 Uiso 1 1 calc R . . N3 N 0.3889(8) 0.7877(4) 0.0498(4) 0.085(3) Uani 1 1 d . . . C41 C 0.0759(8) 0.4217(4) 0.1560(4) 0.068(3) Uani 1 1 d . . . C32 C 0.5671(7) 0.7958(4) 0.0130(3) 0.063(2) Uani 1 1 d . . . H32A H 0.5499 0.7855 -0.0233 0.095 Uiso 1 1 calc R . . H32B H 0.6227 0.7689 0.0311 0.095 Uiso 1 1 calc R . . H32C H 0.5949 0.8359 0.0169 0.095 Uiso 1 1 calc R . . C31 C 0.4670(8) 0.7912(4) 0.0345(3) 0.059(2) Uani 1 1 d . . . C51 C 0.4696(8) 0.7885(4) 0.4409(4) 0.060(2) Uani 1 1 d . . . C42 C -0.0066(10) 0.4219(6) 0.1884(8) 0.147(7) Uani 1 1 d . . . H42A H -0.0619 0.3920 0.1764 0.221 Uiso 1 1 calc R . . H42B H -0.0416 0.4604 0.1867 0.221 Uiso 1 1 calc R . . H42C H 0.0289 0.4135 0.2237 0.221 Uiso 1 1 calc R . . Pd1 Pd 0.02327(4) 0.778594(19) 0.243686(16) 0.02062(11) Uani 1 1 d . . . Sn1 Sn -0.15577(4) 0.662476(18) 0.194865(16) 0.02801(11) Uani 1 1 d . . . Sn2 Sn 0.13588(4) 0.647729(18) 0.294142(16) 0.02794(11) Uani 1 1 d . . . S1 S -0.11578(13) 0.71975(7) 0.27164(6) 0.0289(3) Uani 1 1 d . . . P1 P -0.05675(13) 0.85987(7) 0.27324(6) 0.0252(3) Uani 1 1 d . . . S2 S 0.09568(12) 0.69118(6) 0.21155(6) 0.0258(3) Uani 1 1 d . . . P2 P 0.14923(13) 0.83213(7) 0.20906(6) 0.0249(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C221 0.034(3) 0.025(3) 0.024(3) 0.000(2) 0.012(3) 0.001(3) C231 0.029(3) 0.022(3) 0.039(4) -0.001(3) 0.008(3) -0.006(3) C121 0.030(3) 0.024(3) 0.031(3) -0.002(3) 0.008(3) -0.001(3) C111 0.043(4) 0.018(3) 0.038(4) -0.013(3) 0.011(3) -0.005(3) C122 0.033(3) 0.031(3) 0.045(4) -0.002(3) 0.003(3) 0.004(3) B201 0.031(4) 0.038(4) 0.028(4) -0.002(3) 0.007(3) 0.000(3) C226 0.048(4) 0.046(4) 0.031(4) 0.012(3) 0.017(3) -0.005(3) C223 0.047(4) 0.045(4) 0.030(4) -0.003(3) 0.000(3) 0.006(3) B202 0.023(4) 0.037(4) 0.036(4) -0.004(3) 0.003(3) -0.005(3) C131 0.047(4) 0.020(3) 0.034(3) -0.004(3) 0.018(3) 0.004(3) C211 0.033(3) 0.023(3) 0.025(3) 0.004(2) 0.008(3) -0.005(3) C123 0.041(4) 0.039(4) 0.045(4) -0.003(3) -0.006(3) 0.001(3) C222 0.039(4) 0.032(3) 0.030(3) 0.002(3) 0.007(3) 0.002(3) N1 0.029(3) 0.032(3) 0.034(3) 0.000(2) 0.010(2) -0.004(2) N2 0.026(3) 0.041(3) 0.041(3) -0.002(3) 0.017(2) 0.000(2) C234 0.030(4) 0.042(4) 0.067(5) -0.003(4) 0.012(4) 0.006(3) C232 0.037(4) 0.039(4) 0.040(4) 0.005(3) 0.010(3) 0.004(3) C102 0.047(4) 0.044(4) 0.048(4) 0.009(3) 0.018(4) 0.009(3) C101 0.033(3) 0.037(4) 0.043(4) -0.004(3) 0.013(3) -0.009(3) C112 0.037(4) 0.020(3) 0.029(3) 0.003(2) 0.010(3) -0.006(3) C233 0.040(4) 0.045(4) 0.043(4) 0.003(3) 0.003(3) 0.008(3) C103 0.040(4) 0.042(4) 0.035(4) 0.003(3) 0.017(3) 0.005(3) C224 0.067(5) 0.064(5) 0.028(4) 0.011(4) 0.013(4) 0.020(4) C201 0.046(4) 0.068(5) 0.045(4) -0.001(4) 0.024(4) 0.006(4) C105 0.039(4) 0.045(4) 0.039(4) 0.001(3) 0.016(3) 0.006(3) C124 0.027(4) 0.047(4) 0.061(5) 0.008(4) -0.004(3) 0.003(3) C132 0.056(5) 0.103(7) 0.031(4) 0.011(4) 0.006(4) -0.018(5) C205 0.031(4) 0.067(5) 0.055(5) 0.009(4) 0.007(4) 0.003(4) C203 0.040(4) 0.052(4) 0.053(5) 0.002(4) 0.023(4) -0.003(3) C236 0.034(4) 0.044(4) 0.036(4) -0.002(3) 0.014(3) -0.004(3) C106 0.071(6) 0.041(4) 0.049(5) -0.005(3) 0.020(4) 0.008(4) C125 0.042(4) 0.032(4) 0.064(5) 0.003(3) 0.013(4) 0.009(3) C107 0.032(4) 0.046(4) 0.060(5) 0.000(4) 0.006(4) -0.015(3) C235 0.040(4) 0.046(4) 0.061(5) 0.001(4) 0.026(4) 0.000(3) B205 0.034(4) 0.034(4) 0.027(4) -0.001(3) 0.010(3) -0.006(3) C104 0.054(5) 0.071(5) 0.037(4) -0.005(4) 0.002(4) 0.008(4) C126 0.044(4) 0.030(3) 0.044(4) -0.001(3) 0.007(3) 0.007(3) C108 0.062(5) 0.043(4) 0.055(5) -0.004(4) -0.011(4) 0.002(4) C207 0.055(5) 0.053(5) 0.068(6) -0.002(4) 0.029(4) -0.001(4) B203 0.029(4) 0.026(4) 0.036(4) -0.001(3) -0.005(3) 0.007(3) C206 0.056(5) 0.081(6) 0.049(5) 0.015(4) 0.009(4) -0.005(5) B204 0.024(4) 0.044(4) 0.025(4) -0.005(3) 0.007(3) 0.000(3) B210 0.031(4) 0.037(4) 0.024(3) -0.005(3) 0.013(3) 0.004(3) B209 0.025(4) 0.047(4) 0.025(4) -0.007(3) 0.008(3) -0.002(3) B104 0.030(4) 0.042(4) 0.033(4) -0.007(3) 0.012(3) 0.003(3) B208 0.029(4) 0.040(4) 0.026(4) -0.007(3) 0.005(3) 0.005(3) B107 0.040(4) 0.023(4) 0.050(5) -0.011(3) 0.010(4) -0.002(3) B211 0.032(4) 0.037(4) 0.030(4) 0.005(3) 0.007(3) 0.004(3) B101 0.025(4) 0.046(5) 0.035(4) -0.006(4) 0.007(3) -0.005(3) B102 0.033(4) 0.035(4) 0.056(5) -0.013(4) 0.002(4) 0.005(3) C225 0.072(6) 0.051(5) 0.035(4) 0.012(4) 0.020(4) 0.001(4) B207 0.027(4) 0.028(4) 0.058(5) 0.011(4) 0.003(4) 0.000(3) B206 0.027(4) 0.051(5) 0.034(4) 0.008(4) 0.010(3) 0.001(4) B103 0.050(5) 0.030(4) 0.033(4) 0.005(3) 0.002(4) -0.007(4) B106 0.030(4) 0.045(5) 0.045(5) -0.017(4) 0.015(4) -0.005(4) C136 0.062(5) 0.056(5) 0.060(5) 0.013(4) 0.035(4) 0.022(4) B110 0.029(4) 0.047(4) 0.033(4) 0.002(4) 0.004(3) -0.007(3) C134 0.118(8) 0.058(5) 0.031(4) 0.004(4) 0.034(5) 0.010(6) B108 0.034(4) 0.035(4) 0.040(4) -0.001(3) 0.010(3) -0.006(3) B109 0.024(4) 0.045(4) 0.036(4) -0.003(3) 0.007(3) 0.009(3) B105 0.037(4) 0.024(4) 0.042(4) 0.008(3) 0.012(3) 0.001(3) C202 0.047(5) 0.109(8) 0.045(5) 0.011(5) 0.008(4) -0.005(5) C135 0.111(8) 0.074(6) 0.083(7) 0.019(6) 0.077(7) 0.028(6) C133 0.088(7) 0.106(8) 0.035(4) 0.005(5) 0.000(5) -0.032(6) C204 0.072(6) 0.047(5) 0.087(7) -0.005(5) 0.020(5) -0.003(4) B111 0.028(4) 0.047(5) 0.039(4) -0.010(4) 0.000(3) -0.005(4) C208 0.092(7) 0.051(5) 0.105(8) -0.008(5) 0.046(6) -0.017(5) N4 0.121(8) 0.092(7) 0.056(5) -0.004(5) 0.028(5) -0.024(6) N5 0.068(6) 0.108(7) 0.116(8) -0.039(6) 0.035(6) -0.010(5) C52 0.066(6) 0.065(5) 0.060(5) -0.014(4) 0.023(5) -0.010(5) N3 0.082(6) 0.098(7) 0.085(6) 0.012(5) 0.043(5) -0.004(5) C41 0.063(6) 0.066(6) 0.070(7) 0.028(5) 0.004(5) 0.000(5) C32 0.066(6) 0.080(6) 0.048(5) 0.020(5) 0.020(4) 0.015(5) C31 0.069(6) 0.063(5) 0.046(5) 0.006(4) 0.014(4) 0.003(5) C51 0.056(5) 0.065(6) 0.061(5) -0.012(4) 0.017(4) -0.015(5) C42 0.077(8) 0.123(11) 0.26(2) 0.108(12) 0.086(11) 0.047(8) Pd1 0.0234(2) 0.0199(2) 0.0198(2) -0.00009(17) 0.00721(18) -0.00056(18) Sn1 0.0346(2) 0.0225(2) 0.0260(2) 0.00015(17) 0.00388(18) -0.00309(18) Sn2 0.0337(2) 0.0260(2) 0.0230(2) -0.00080(17) 0.00290(17) 0.00155(18) S1 0.0335(8) 0.0293(8) 0.0270(8) -0.0024(6) 0.0137(7) -0.0062(7) P1 0.0301(8) 0.0223(7) 0.0247(8) -0.0021(6) 0.0092(6) 0.0013(6) S2 0.0310(8) 0.0246(7) 0.0234(7) -0.0014(6) 0.0095(6) 0.0016(6) P2 0.0291(8) 0.0243(7) 0.0224(7) 0.0020(6) 0.0077(6) -0.0029(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 C221 C222 1.387(9) . ? C221 C226 1.389(8) . ? C221 P2 1.824(6) . ? C231 C232 1.389(9) . ? C231 C236 1.402(9) . ? C231 P2 1.810(6) . ? C121 C122 1.384(9) . ? C121 C126 1.414(8) . ? C121 P1 1.817(6) . ? C111 C112 1.513(8) . ? C111 P1 1.854(6) . ? C122 C123 1.379(9) . ? B201 B206 1.759(11) . ? B201 B210 1.764(10) . ? B201 B202 1.928(10) . ? B201 B205 1.933(10) . ? B201 Sn2 2.304(7) . ? C226 C225 1.379(10) . ? C223 C222 1.380(9) . ? C223 C224 1.391(10) . ? B202 B207 1.775(10) . ? B202 B206 1.782(11) . ? B202 B203 1.925(11) . ? B202 Sn2 2.311(8) . ? C131 C136 1.370(10) . ? C131 C132 1.376(10) . ? C131 P1 1.815(6) . ? C211 C112 1.530(8) . ? C211 P2 1.829(6) . ? C123 C124 1.384(10) . ? N1 C103 1.511(8) . ? N1 C107 1.518(8) . ? N1 C105 1.519(8) . ? N1 C101 1.526(8) . ? N2 C207 1.510(9) . ? N2 C205 1.512(9) . ? N2 C201 1.513(9) . ? N2 C203 1.520(8) . ? C234 C235 1.376(11) . ? C234 C233 1.378(10) . ? C232 C233 1.386(9) . ? C102 C101 1.507(9) . ? C103 C104 1.519(10) . ? C224 C225 1.372(11) . ? C201 C202 1.504(11) . ? C105 C106 1.502(9) . ? C124 C125 1.357(11) . ? C132 C133 1.387(11) . ? C205 C206 1.523(11) . ? C203 C204 1.523(11) . ? C236 C235 1.389(10) . ? C125 C126 1.374(10) . ? C107 C108 1.506(11) . ? B205 B209 1.751(11) . ? B205 B210 1.755(9) . ? B205 B204 1.898(10) . ? B205 Sn2 2.303(7) . ? C207 C208 1.526(11) . ? B203 B208 1.768(10) . ? B203 B207 1.774(11) . ? B203 B204 1.898(10) . ? B203 Sn2 2.315(7) . ? B204 B209 1.755(10) . ? B204 B208 1.761(11) . ? B204 Sn2 2.304(7) . ? B210 B206 1.777(11) . ? B210 B211 1.791(10) . ? B210 B209 1.800(9) . ? B209 B211 1.767(10) . ? B209 B208 1.779(10) . ? B104 B109 1.771(11) . ? B104 B108 1.771(11) . ? B104 B105 1.874(10) . ? B104 B103 1.885(11) . ? B104 Sn1 2.315(8) . ? B208 B211 1.778(10) . ? B208 B207 1.779(10) . ? B107 B102 1.769(11) . ? B107 B106 1.774(12) . ? B107 B103 1.777(11) . ? B107 B111 1.777(12) . ? B107 B108 1.788(11) . ? B211 B206 1.765(10) . ? B211 B207 1.778(11) . ? B101 B110 1.763(10) . ? B101 B106 1.772(11) . ? B101 B102 1.888(12) . ? B101 B105 1.904(10) . ? B101 Sn1 2.296(8) . ? B102 B106 1.765(12) . ? B102 B103 1.920(12) . ? B102 Sn1 2.317(8) . ? B207 B206 1.805(12) . ? B103 B108 1.772(11) . ? B103 Sn1 2.291(7) . ? B106 B110 1.788(12) . ? B106 B111 1.798(11) . ? C136 C135 1.422(12) . ? B110 B105 1.764(11) . ? B110 B109 1.768(10) . ? B110 B111 1.796(11) . ? C134 C133 1.322(13) . ? C134 C135 1.378(15) . ? B108 B111 1.765(11) . ? B108 B109 1.785(11) . ? B109 B105 1.762(11) . ? B109 B111 1.768(11) . ? B105 Sn1 2.309(8) . ? N4 C41 1.096(12) . ? N5 C51 1.109(10) . ? C52 C51 1.439(12) . ? N3 C31 1.112(10) . ? C41 C42 1.446(16) . ? C32 C31 1.451(12) . ? Pd1 P1 2.2765(15) . ? Pd1 P2 2.2807(15) . ? Pd1 S2 2.3734(15) . ? Pd1 S1 2.3818(15) . ? Sn1 S1 2.3559(15) . ? Sn2 S2 2.3365(15) . ? 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 C222 C221 C226 119.4(6) . . ? C222 C221 P2 119.5(4) . . ? C226 C221 P2 121.1(5) . . ? C232 C231 C236 118.7(6) . . ? C232 C231 P2 117.3(5) . . ? C236 C231 P2 124.0(5) . . ? C122 C121 C126 119.1(6) . . ? C122 C121 P1 121.0(5) . . ? C126 C121 P1 119.9(5) . . ? C112 C111 P1 114.5(4) . . ? C123 C122 C121 120.5(6) . . ? B206 B201 B210 60.6(4) . . ? B206 B201 B202 57.6(4) . . ? B210 B201 B202 106.3(5) . . ? B206 B201 B205 104.6(5) . . ? B210 B201 B205 56.4(4) . . ? B202 B201 B205 107.1(5) . . ? B206 B201 Sn2 115.5(4) . . ? B210 B201 Sn2 115.1(4) . . ? B202 B201 Sn2 65.5(3) . . ? B205 B201 Sn2 65.2(3) . . ? C225 C226 C221 119.3(7) . . ? C222 C223 C224 119.4(7) . . ? B207 B202 B206 61.0(5) . . ? B207 B202 B203 57.1(4) . . ? B206 B202 B203 105.7(5) . . ? B207 B202 B201 105.9(5) . . ? B206 B202 B201 56.4(4) . . ? B203 B202 B201 107.9(5) . . ? B207 B202 Sn2 115.2(4) . . ? B206 B202 Sn2 114.2(4) . . ? B203 B202 Sn2 65.5(3) . . ? B201 B202 Sn2 65.1(3) . . ? C136 C131 C132 119.5(7) . . ? C136 C131 P1 123.2(6) . . ? C132 C131 P1 117.3(5) . . ? C112 C211 P2 114.7(4) . . ? C122 C123 C124 120.1(7) . . ? C223 C222 C221 120.9(6) . . ? C103 N1 C107 106.0(5) . . ? C103 N1 C105 111.7(5) . . ? C107 N1 C105 110.8(5) . . ? C103 N1 C101 111.1(5) . . ? C107 N1 C101 110.7(5) . . ? C105 N1 C101 106.5(5) . . ? C207 N2 C205 110.9(6) . . ? C207 N2 C201 110.7(6) . . ? C205 N2 C201 106.6(5) . . ? C207 N2 C203 106.1(5) . . ? C205 N2 C203 111.5(5) . . ? C201 N2 C203 111.1(6) . . ? C235 C234 C233 120.1(7) . . ? C233 C232 C231 120.6(6) . . ? C102 C101 N1 115.5(5) . . ? C111 C112 C211 112.2(5) . . ? C234 C233 C232 120.1(7) . . ? N1 C103 C104 115.8(6) . . ? C225 C224 C223 119.5(7) . . ? C202 C201 N2 115.6(6) . . ? C106 C105 N1 116.0(6) . . ? C125 C124 C123 119.5(7) . . ? C131 C132 C133 120.9(8) . . ? N2 C205 C206 114.7(6) . . ? N2 C203 C204 115.2(6) . . ? C235 C236 C231 120.0(7) . . ? C124 C125 C126 122.2(7) . . ? C108 C107 N1 115.6(6) . . ? C234 C235 C236 120.3(7) . . ? B209 B205 B210 61.8(4) . . ? B209 B205 B204 57.3(4) . . ? B210 B205 B204 107.1(5) . . ? B209 B205 B201 106.4(5) . . ? B210 B205 B201 56.9(4) . . ? B204 B205 B201 108.1(5) . . ? B209 B205 Sn2 115.9(4) . . ? B210 B205 Sn2 115.5(4) . . ? B204 B205 Sn2 65.7(3) . . ? B201 B205 Sn2 65.2(3) . . ? C125 C126 C121 118.6(7) . . ? N2 C207 C208 114.6(6) . . ? B208 B203 B207 60.3(4) . . ? B208 B203 B204 57.3(4) . . ? B207 B203 B204 105.6(5) . . ? B208 B203 B202 105.8(5) . . ? B207 B203 B202 57.2(4) . . ? B204 B203 B202 107.9(5) . . ? B208 B203 Sn2 115.4(4) . . ? B207 B203 Sn2 115.1(4) . . ? B204 B203 Sn2 65.5(3) . . ? B202 B203 Sn2 65.3(3) . . ? B209 B204 B208 60.8(4) . . ? B209 B204 B205 57.1(4) . . ? B208 B204 B205 106.4(5) . . ? B209 B204 B203 106.7(5) . . ? B208 B204 B203 57.6(4) . . ? B205 B204 B203 109.0(5) . . ? B209 B204 Sn2 115.7(4) . . ? B208 B204 Sn2 116.2(4) . . ? B205 B204 Sn2 65.6(3) . . ? B203 B204 Sn2 66.0(3) . . ? B205 B210 B201 66.6(4) . . ? B205 B210 B206 111.8(5) . . ? B201 B210 B206 59.6(4) . . ? B205 B210 B211 108.3(5) . . ? B201 B210 B211 109.0(5) . . ? B206 B210 B211 59.3(4) . . ? B205 B210 B209 59.0(4) . . ? B201 B210 B209 111.8(5) . . ? B206 B210 B209 106.9(5) . . ? B211 B210 B209 59.0(4) . . ? B205 B209 B204 65.5(4) . . ? B205 B209 B211 109.6(5) . . ? B204 B209 B211 109.6(5) . . ? B205 B209 B208 112.2(5) . . ? B204 B209 B208 59.8(4) . . ? B211 B209 B208 60.2(4) . . ? B205 B209 B210 59.2(4) . . ? B204 B209 B210 111.5(5) . . ? B211 B209 B210 60.3(4) . . ? B208 B209 B210 108.8(5) . . ? B109 B104 B108 60.5(4) . . ? B109 B104 B105 57.7(4) . . ? B108 B104 B105 106.6(5) . . ? B109 B104 B103 106.3(5) . . ? B108 B104 B103 57.9(4) . . ? B105 B104 B103 108.1(5) . . ? B109 B104 Sn1 116.4(4) . . ? B108 B104 Sn1 116.3(4) . . ? B105 B104 Sn1 65.9(3) . . ? B103 B104 Sn1 65.2(3) . . ? B204 B208 B203 65.1(4) . . ? B204 B208 B211 108.8(5) . . ? B203 B208 B211 109.7(5) . . ? B204 B208 B209 59.4(4) . . ? B203 B208 B209 111.5(5) . . ? B211 B208 B209 59.6(4) . . ? B204 B208 B207 111.5(5) . . ? B203 B208 B207 60.0(4) . . ? B211 B208 B207 60.0(4) . . ? B209 B208 B207 108.1(5) . . ? B102 B107 B106 59.7(5) . . ? B102 B107 B103 65.6(5) . . ? B106 B107 B103 111.5(5) . . ? B102 B107 B111 110.7(6) . . ? B106 B107 B111 60.8(5) . . ? B103 B107 B111 109.0(5) . . ? B102 B107 B108 112.4(5) . . ? B106 B107 B108 108.4(5) . . ? B103 B107 B108 59.6(4) . . ? B111 B107 B108 59.3(4) . . ? B206 B211 B209 108.8(5) . . ? B206 B211 B208 109.3(5) . . ? B209 B211 B208 60.2(4) . . ? B206 B211 B207 61.2(4) . . ? B209 B211 B207 108.7(5) . . ? B208 B211 B207 60.0(4) . . ? B206 B211 B210 60.0(4) . . ? B209 B211 B210 60.8(4) . . ? B208 B211 B210 109.3(5) . . ? B207 B211 B210 109.4(5) . . ? B110 B101 B106 60.7(4) . . ? B110 B101 B102 106.7(5) . . ? B106 B101 B102 57.5(4) . . ? B110 B101 B105 57.3(4) . . ? B106 B101 B105 106.3(5) . . ? B102 B101 B105 108.8(5) . . ? B110 B101 Sn1 116.6(4) . . ? B106 B101 Sn1 116.9(5) . . ? B102 B101 Sn1 66.4(4) . . ? B105 B101 Sn1 65.9(3) . . ? B106 B102 B107 60.3(5) . . ? B106 B102 B101 57.9(4) . . ? B107 B102 B101 105.7(6) . . ? B106 B102 B103 105.5(5) . . ? B107 B102 B103 57.4(4) . . ? B101 B102 B103 106.4(5) . . ? B106 B102 Sn1 116.1(5) . . ? B107 B102 Sn1 115.4(5) . . ? B101 B102 Sn1 65.2(3) . . ? B103 B102 Sn1 64.7(3) . . ? C224 C225 C226 121.4(7) . . ? B203 B207 B202 65.7(4) . . ? B203 B207 B211 109.4(5) . . ? B202 B207 B211 109.2(5) . . ? B203 B207 B208 59.7(4) . . ? B202 B207 B208 112.0(5) . . ? B211 B207 B208 60.0(4) . . ? B203 B207 B206 111.4(5) . . ? B202 B207 B206 59.7(4) . . ? B211 B207 B206 59.0(4) . . ? B208 B207 B206 107.4(5) . . ? B201 B206 B211 110.5(5) . . ? B201 B206 B210 59.9(4) . . ? B211 B206 B210 60.7(4) . . ? B201 B206 B202 66.0(4) . . ? B211 B206 B202 109.5(5) . . ? B210 B206 B202 112.4(5) . . ? B201 B206 B207 112.2(5) . . ? B211 B206 B207 59.7(4) . . ? B210 B206 B207 108.8(5) . . ? B202 B206 B207 59.3(4) . . ? B108 B103 B107 60.5(4) . . ? B108 B103 B104 57.8(4) . . ? B107 B103 B104 106.3(5) . . ? B108 B103 B102 106.3(5) . . ? B107 B103 B102 57.0(4) . . ? B104 B103 B102 108.7(5) . . ? B108 B103 Sn1 117.4(5) . . ? B107 B103 Sn1 116.3(5) . . ? B104 B103 Sn1 66.5(3) . . ? B102 B103 Sn1 66.1(3) . . ? B102 B106 B101 64.6(5) . . ? B102 B106 B107 60.0(5) . . ? B101 B106 B107 110.7(5) . . ? B102 B106 B110 111.2(5) . . ? B101 B106 B110 59.4(4) . . ? B107 B106 B110 107.6(5) . . ? B102 B106 B111 109.9(6) . . ? B101 B106 B111 109.3(5) . . ? B107 B106 B111 59.7(4) . . ? B110 B106 B111 60.1(4) . . ? C131 C136 C135 118.9(9) . . ? B101 B110 B105 65.4(4) . . ? B101 B110 B109 111.9(5) . . ? B105 B110 B109 59.8(4) . . ? B101 B110 B106 59.9(4) . . ? B105 B110 B106 111.9(5) . . ? B109 B110 B106 108.3(5) . . ? B101 B110 B111 109.8(6) . . ? B105 B110 B111 109.3(5) . . ? B109 B110 B111 59.5(4) . . ? B106 B110 B111 60.2(4) . . ? C133 C134 C135 121.4(8) . . ? B111 B108 B104 109.6(5) . . ? B111 B108 B103 109.9(5) . . ? B104 B108 B103 64.3(4) . . ? B111 B108 B109 59.7(4) . . ? B104 B108 B109 59.7(4) . . ? B103 B108 B109 110.7(5) . . ? B111 B108 B107 60.0(4) . . ? B104 B108 B107 110.8(5) . . ? B103 B108 B107 59.9(4) . . ? B109 B108 B107 107.4(5) . . ? B105 B109 B110 60.0(4) . . ? B105 B109 B111 110.7(5) . . ? B110 B109 B111 61.1(4) . . ? B105 B109 B104 64.1(4) . . ? B110 B109 B104 110.9(5) . . ? B111 B109 B104 109.5(5) . . ? B105 B109 B108 111.0(5) . . ? B110 B109 B108 108.2(5) . . ? B111 B109 B108 59.5(4) . . ? B104 B109 B108 59.8(4) . . ? B109 B105 B110 60.2(4) . . ? B109 B105 B104 58.2(4) . . ? B110 B105 B104 106.4(5) . . ? B109 B105 B101 105.8(5) . . ? B110 B105 B101 57.3(4) . . ? B104 B105 B101 108.0(5) . . ? B109 B105 Sn1 117.1(4) . . ? B110 B105 Sn1 115.9(4) . . ? B104 B105 Sn1 66.2(3) . . ? B101 B105 Sn1 65.2(3) . . ? C134 C135 C136 119.2(8) . . ? C134 C133 C132 120.1(9) . . ? B108 B111 B109 60.7(4) . . ? B108 B111 B107 60.7(5) . . ? B109 B111 B107 108.7(6) . . ? B108 B111 B110 107.9(5) . . ? B109 B111 B110 59.5(4) . . ? B107 B111 B110 107.1(5) . . ? B108 B111 B106 108.4(6) . . ? B109 B111 B106 107.8(5) . . ? B107 B111 B106 59.5(5) . . ? B110 B111 B106 59.6(4) . . ? N4 C41 C42 175.1(13) . . ? N3 C31 C32 178.4(10) . . ? N5 C51 C52 177.2(11) . . ? P1 Pd1 P2 94.92(6) . . ? P1 Pd1 S2 176.49(6) . . ? P2 Pd1 S2 87.86(5) . . ? P1 Pd1 S1 87.45(6) . . ? P2 Pd1 S1 174.56(6) . . ? S2 Pd1 S1 89.60(5) . . ? B103 Sn1 B101 83.3(3) . . ? B103 Sn1 B105 82.8(3) . . ? B101 Sn1 B105 48.9(3) . . ? B103 Sn1 B104 48.3(3) . . ? B101 Sn1 B104 83.1(3) . . ? B105 Sn1 B104 47.8(3) . . ? B103 Sn1 B102 49.2(3) . . ? B101 Sn1 B102 48.3(3) . . ? B105 Sn1 B102 83.6(3) . . ? B104 Sn1 B102 83.8(3) . . ? B103 Sn1 S1 128.1(2) . . ? B101 Sn1 S1 148.6(2) . . ? B105 Sn1 S1 125.72(19) . . ? B104 Sn1 S1 116.24(18) . . ? B102 Sn1 S1 150.6(2) . . ? B205 Sn2 B201 49.6(2) . . ? B205 Sn2 B204 48.6(3) . . ? B201 Sn2 B204 84.6(3) . . ? B205 Sn2 B202 84.6(3) . . ? B201 Sn2 B202 49.4(3) . . ? B204 Sn2 B202 84.1(3) . . ? B205 Sn2 B203 84.0(3) . . ? B201 Sn2 B203 84.8(3) . . ? B204 Sn2 B203 48.5(3) . . ? B202 Sn2 B203 49.2(3) . . ? B205 Sn2 S2 132.01(18) . . ? B201 Sn2 S2 148.25(19) . . ? B204 Sn2 S2 120.62(18) . . ? B202 Sn2 S2 143.19(19) . . ? B203 Sn2 S2 125.9(2) . . ? Sn1 S1 Pd1 94.44(5) . . ? C131 P1 C121 108.4(3) . . ? C131 P1 C111 101.0(3) . . ? C121 P1 C111 104.0(3) . . ? C131 P1 Pd1 111.80(19) . . ? C121 P1 Pd1 112.9(2) . . ? C111 P1 Pd1 117.8(2) . . ? Sn2 S2 Pd1 92.23(5) . . ? C231 P2 C221 109.1(3) . . ? C231 P2 C211 101.8(3) . . ? C221 P2 C211 103.8(3) . . ? C231 P2 Pd1 115.0(2) . . ? C221 P2 Pd1 108.7(2) . . ? C211 P2 Pd1 117.62(19) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.438 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.106 # Attachment '765677_compound_8.cif' data_hornung126 _database_code_depnum_ccdc_archive 'CCDC 765677' #TrackingRef '765677_compound_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H63 B11 P4 Pd2 S2 Sn, 3(C H2 Cl2)' _chemical_formula_sum 'C57 H69 B11 Cl6 P4 Pd2 S2 Sn' _chemical_formula_weight 1605.27 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 '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' Sn Sn -0.6537 1.4246 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7694(7) _cell_length_b 20.8261(11) _cell_length_c 21.8590(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.542(3) _cell_angle_gamma 90.00 _cell_volume 6806.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 43011 _cell_measurement_theta_min 4.45 _cell_measurement_theta_max 59.31 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2371 _exptl_crystal_size_mid 0.1795 _exptl_crystal_size_min 0.1292 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7722 _exptl_absorpt_correction_T_max 0.8746 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84890 _diffrn_reflns_av_R_equivalents 0.0959 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.71 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12293 _reflns_number_gt 10423 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep3 for windows' _computing_publication_material ? _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^)+(0.0229P)^2^+22.4054P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12293 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.0973 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.002 _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 Pd1 Pd 0.63703(2) 0.163271(17) 0.923838(17) 0.02593(9) Uani 1 1 d . . . Pd2 Pd 0.81212(2) 0.242389(16) 0.970885(16) 0.02323(9) Uani 1 1 d . . . Sn1 Sn 0.75202(2) 0.143503(15) 1.071283(15) 0.02693(9) Uani 1 1 d . . . S2 S 0.68428(8) 0.24322(6) 1.00475(6) 0.0274(2) Uani 1 1 d . . . P2 P 0.49420(9) 0.20145(7) 0.89304(6) 0.0336(3) Uani 1 1 d . . . P4 P 0.94480(8) 0.23292(6) 0.95131(6) 0.0287(3) Uani 1 1 d . . . P1 P 0.60597(9) 0.08352(6) 0.84843(6) 0.0311(3) Uani 1 1 d . . . P3 P 0.82447(9) 0.35128(6) 0.97451(6) 0.0282(3) Uani 1 1 d . . . S1 S 0.78862(8) 0.13068(5) 0.96706(6) 0.0268(2) Uani 1 1 d . . . C311 C 0.8907(4) 0.3775(2) 1.0539(2) 0.0338(11) Uani 1 1 d . . . C221 C 0.4658(3) 0.2330(3) 0.9608(3) 0.0394(13) Uani 1 1 d . . . C321 C 0.7191(4) 0.3936(2) 0.9566(3) 0.0370(12) Uani 1 1 d . . . C316 C 0.9465(4) 0.4312(3) 1.0647(3) 0.0442(13) Uani 1 1 d . . . H316 H 0.9499 0.4553 1.0298 0.053 Uiso 1 1 calc R . . C111 C 0.6270(3) 0.1077(2) 0.7751(2) 0.0319(11) Uani 1 1 d . . . C121 C 0.6712(4) 0.0119(2) 0.8773(3) 0.0410(13) Uani 1 1 d . . . C431 C 0.9677(4) 0.2929(3) 0.8982(3) 0.0373(12) Uani 1 1 d . . . H43A H 1.0257 0.2839 0.8935 0.045 Uiso 1 1 calc R . . H43B H 0.9232 0.2891 0.8560 0.045 Uiso 1 1 calc R . . C332 C 0.9675(4) 0.3616(2) 0.9217(3) 0.0367(12) Uani 1 1 d . . . H33A H 0.9924 0.3894 0.8961 0.044 Uiso 1 1 calc R . . H33B H 1.0061 0.3642 0.9661 0.044 Uiso 1 1 calc R . . C331 C 0.8739(4) 0.3867(2) 0.9178(2) 0.0344(11) Uani 1 1 d . . . H33C H 0.8338 0.3794 0.8745 0.041 Uiso 1 1 calc R . . H33D H 0.8779 0.4328 0.9248 0.041 Uiso 1 1 calc R . . C216 C 0.5309(4) 0.2745(3) 0.7986(3) 0.0418(13) Uani 1 1 d . . . H216 H 0.5868 0.2550 0.8124 0.050 Uiso 1 1 calc R . . B1 B 0.6922(4) 0.1524(3) 1.1563(3) 0.0323(13) Uani 1 1 d . . . H1 H 0.6391 0.1888 1.1468 0.039 Uiso 1 1 calc R . . B6 B 0.7664(4) 0.1404(3) 1.2345(3) 0.0337(13) Uani 1 1 d . . . H6 H 0.7596 0.1706 1.2740 0.040 Uiso 1 1 calc R . . C421 C 0.9603(3) 0.1569(2) 0.9167(3) 0.0347(12) Uani 1 1 d . . . C411 C 1.0352(3) 0.2393(2) 1.0274(3) 0.0341(11) Uani 1 1 d . . . C422 C 0.9184(4) 0.1453(3) 0.8521(3) 0.0456(14) Uani 1 1 d . . . H422 H 0.8862 0.1779 0.8257 0.055 Uiso 1 1 calc R . . C212 C 0.3871(4) 0.2920(3) 0.8096(3) 0.0495(15) Uani 1 1 d . . . H212 H 0.3446 0.2832 0.8298 0.059 Uiso 1 1 calc R . . C231 C 0.4069(4) 0.1420(3) 0.8592(3) 0.0447(14) Uani 1 1 d . . . H23A H 0.4060 0.1117 0.8926 0.054 Uiso 1 1 calc R . . H23B H 0.3493 0.1635 0.8450 0.054 Uiso 1 1 calc R . . C211 C 0.4694(3) 0.2616(3) 0.8302(2) 0.0360(12) Uani 1 1 d . . . C426 C 1.0079(4) 0.1065(3) 0.9555(3) 0.0436(13) Uani 1 1 d . . . H426 H 1.0361 0.1133 0.9994 0.052 Uiso 1 1 calc R . . C116 C 0.6851(4) 0.1579(3) 0.7769(3) 0.0392(12) Uani 1 1 d . . . H116 H 0.7152 0.1773 0.8162 0.047 Uiso 1 1 calc R . . B5 B 0.8151(4) 0.1735(3) 1.1790(3) 0.0315(12) Uani 1 1 d . . . H5 H 0.8394 0.2234 1.1833 0.038 Uiso 1 1 calc R . . C312 C 0.8882(4) 0.3421(3) 1.1071(3) 0.0470(14) Uani 1 1 d . . . H312 H 0.8533 0.3052 1.1011 0.056 Uiso 1 1 calc R . . C115 C 0.6994(4) 0.1798(3) 0.7211(3) 0.0451(14) Uani 1 1 d . . . H115 H 0.7388 0.2136 0.7232 0.054 Uiso 1 1 calc R . . C214 C 0.4291(4) 0.3468(3) 0.7270(3) 0.0525(16) Uani 1 1 d . . . H214 H 0.4156 0.3751 0.6923 0.063 Uiso 1 1 calc R . . C412 C 1.1182(4) 0.2638(3) 1.0313(3) 0.0474(14) Uani 1 1 d . . . H412 H 1.1294 0.2778 0.9942 0.057 Uiso 1 1 calc R . . B2 B 0.6766(5) 0.0701(3) 1.1143(3) 0.0396(14) Uani 1 1 d . . . H2 H 0.6137 0.0549 1.0781 0.048 Uiso 1 1 calc R . . C215 C 0.5101(5) 0.3161(3) 0.7466(3) 0.0518(15) Uani 1 1 d . . . H215 H 0.5512 0.3233 0.7250 0.062 Uiso 1 1 calc R . . C131 C 0.4913(4) 0.0538(3) 0.8227(3) 0.0456(14) Uani 1 1 d . . . H13A H 0.4838 0.0244 0.7869 0.055 Uiso 1 1 calc R . . H13B H 0.4820 0.0295 0.8579 0.055 Uiso 1 1 calc R . . C226 C 0.4670(4) 0.1903(3) 1.0099(3) 0.0506(15) Uani 1 1 d . . . H226 H 0.4812 0.1474 1.0063 0.061 Uiso 1 1 calc R . . C213 C 0.3675(4) 0.3357(3) 0.7588(3) 0.0533(16) Uani 1 1 d . . . H213 H 0.3131 0.3573 0.7463 0.064 Uiso 1 1 calc R . . C222 C 0.4470(5) 0.2962(3) 0.9673(3) 0.0577(17) Uani 1 1 d . . . H222 H 0.4468 0.3254 0.9351 0.069 Uiso 1 1 calc R . . C114 C 0.6561(5) 0.1521(3) 0.6631(3) 0.0541(16) Uani 1 1 d . . . H114 H 0.6655 0.1669 0.6257 0.065 Uiso 1 1 calc R . . C416 C 1.0207(4) 0.2194(3) 1.0834(3) 0.0473(14) Uani 1 1 d . . . H416 H 0.9650 0.2031 1.0813 0.057 Uiso 1 1 calc R . . C112 C 0.5827(5) 0.0802(3) 0.7159(3) 0.0522(16) Uani 1 1 d . . . H112 H 0.5424 0.0468 0.7130 0.063 Uiso 1 1 calc R . . C415 C 1.0872(5) 0.2231(4) 1.1426(3) 0.0607(18) Uani 1 1 d . . . H415 H 1.0763 0.2096 1.1800 0.073 Uiso 1 1 calc R . . B10 B 0.8735(5) 0.1134(3) 1.2334(3) 0.0386(14) Uani 1 1 d . . . H10 H 0.9355 0.1264 1.2717 0.046 Uiso 1 1 calc R . . C425 C 1.0129(4) 0.0476(3) 0.9289(4) 0.0538(17) Uani 1 1 d . . . H425 H 1.0448 0.0146 0.9548 0.065 Uiso 1 1 calc R . . B7 B 0.6862(5) 0.0808(3) 1.1970(3) 0.0388(14) Uani 1 1 d . . . H7 H 0.6269 0.0723 1.2120 0.047 Uiso 1 1 calc R . . B4 B 0.8756(4) 0.1044(3) 1.1530(3) 0.0331(13) Uani 1 1 d . . . H4 H 0.9377 0.1107 1.1409 0.040 Uiso 1 1 calc R . . B9 B 0.8587(5) 0.0361(3) 1.1961(3) 0.0404(15) Uani 1 1 d . . . H9 H 0.9110 -0.0009 1.2109 0.049 Uiso 1 1 calc R . . C423 C 0.9241(5) 0.0846(3) 0.8263(3) 0.0560(18) Uani 1 1 d . . . H423 H 0.8956 0.0769 0.7826 0.067 Uiso 1 1 calc R . . B3 B 0.7905(5) 0.0409(3) 1.1141(3) 0.0369(14) Uani 1 1 d . . . H3 H 0.7994 0.0072 1.0779 0.044 Uiso 1 1 calc R . . B11 B 0.7940(5) 0.0584(3) 1.2460(3) 0.0411(15) Uani 1 1 d . . . H11 H 0.8046 0.0354 1.2931 0.049 Uiso 1 1 calc R . . C132 C 0.4200(4) 0.1052(3) 0.8022(3) 0.0465(15) Uani 1 1 d . . . H13C H 0.3638 0.0854 0.7777 0.056 Uiso 1 1 calc R . . H13D H 0.4362 0.1353 0.7739 0.056 Uiso 1 1 calc R . . C126 C 0.7314(4) -0.0118(3) 0.8495(3) 0.0499(15) Uani 1 1 d . . . H126 H 0.7396 0.0086 0.8139 0.060 Uiso 1 1 calc R . . C315 C 0.9968(4) 0.4492(3) 1.1264(3) 0.0525(16) Uani 1 1 d . . . H315 H 1.0345 0.4846 1.1331 0.063 Uiso 1 1 calc R . . C326 C 0.6931(5) 0.4237(3) 1.0036(3) 0.0541(16) Uani 1 1 d . . . H326 H 0.7312 0.4244 1.0460 0.065 Uiso 1 1 calc R . . C313 C 0.9364(5) 0.3608(3) 1.1684(3) 0.0611(19) Uani 1 1 d . . . H313 H 0.9325 0.3373 1.2036 0.073 Uiso 1 1 calc R . . C122 C 0.6584(6) -0.0194(3) 0.9297(3) 0.0622(19) Uani 1 1 d . . . H122 H 0.6175 -0.0034 0.9486 0.075 Uiso 1 1 calc R . . B8 B 0.7429(5) 0.0168(3) 1.1729(3) 0.0446(17) Uani 1 1 d . . . H8 H 0.7203 -0.0332 1.1723 0.054 Uiso 1 1 calc R . . C322 C 0.6602(4) 0.3936(3) 0.8936(3) 0.0559(17) Uani 1 1 d . . . H322 H 0.6764 0.3732 0.8611 0.067 Uiso 1 1 calc R . . C225 C 0.4474(4) 0.2105(4) 1.0641(3) 0.0599(18) Uani 1 1 d . . . H225 H 0.4473 0.1812 1.0962 0.072 Uiso 1 1 calc R . . C113 C 0.5988(6) 0.1027(4) 0.6606(3) 0.066(2) Uani 1 1 d . . . H113 H 0.5697 0.0835 0.6210 0.079 Uiso 1 1 calc R . . C424 C 0.9711(5) 0.0370(3) 0.8646(4) 0.0568(18) Uani 1 1 d . . . H424 H 0.9749 -0.0032 0.8470 0.068 Uiso 1 1 calc R . . C224 C 0.4284(5) 0.2725(5) 1.0702(3) 0.068(2) Uani 1 1 d . . . H224 H 0.4154 0.2860 1.1069 0.082 Uiso 1 1 calc R . . C124 C 0.7665(6) -0.0976(3) 0.9258(4) 0.069(2) Uani 1 1 d . . . H124 H 0.7982 -0.1348 0.9419 0.083 Uiso 1 1 calc R . . C314 C 0.9902(5) 0.4137(3) 1.1780(3) 0.0618(19) Uani 1 1 d . . . H314 H 1.0228 0.4260 1.2198 0.074 Uiso 1 1 calc R . . C223 C 0.4278(6) 0.3169(4) 1.0227(4) 0.078(2) Uani 1 1 d . . . H223 H 0.4150 0.3598 1.0274 0.094 Uiso 1 1 calc R . . C123 C 0.7060(7) -0.0740(3) 0.9536(4) 0.076(2) Uani 1 1 d . . . H123 H 0.6974 -0.0952 0.9886 0.091 Uiso 1 1 calc R . . C325 C 0.6091(6) 0.4535(4) 0.9879(4) 0.075(2) Uani 1 1 d . . . H325 H 0.5914 0.4735 1.0199 0.091 Uiso 1 1 calc R . . C414 C 1.1689(5) 0.2466(3) 1.1453(4) 0.066(2) Uani 1 1 d . . . H414 H 1.2143 0.2484 1.1848 0.079 Uiso 1 1 calc R . . C323 C 0.5781(5) 0.4234(4) 0.8792(4) 0.071(2) Uani 1 1 d . . . H323 H 0.5394 0.4230 0.8370 0.085 Uiso 1 1 calc R . . C324 C 0.5533(5) 0.4532(4) 0.9255(4) 0.069(2) Uani 1 1 d . . . H324 H 0.4980 0.4735 0.9150 0.083 Uiso 1 1 calc R . . C125 C 0.7803(5) -0.0669(3) 0.8751(4) 0.067(2) Uani 1 1 d . . . H125 H 0.8225 -0.0826 0.8573 0.080 Uiso 1 1 calc R . . C413 C 1.1852(4) 0.2676(3) 1.0911(4) 0.0614(19) Uani 1 1 d . . . H413 H 1.2409 0.2844 1.0939 0.074 Uiso 1 1 calc R . . Cl2 Cl 0.22129(14) 0.19869(9) 0.92160(9) 0.0696(5) Uani 1 1 d . . . Cl1 Cl 0.15551(18) 0.17626(13) 0.78497(11) 0.1032(8) Uani 1 1 d . . . C1 C 0.1639(5) 0.1454(3) 0.8603(4) 0.0629(19) Uani 1 1 d . . . H1A H 0.1953 0.1047 0.8663 0.076 Uiso 1 1 calc R . . H1B H 0.1044 0.1377 0.8629 0.076 Uiso 1 1 calc R . . Cl4 Cl 0.34493(16) 0.08934(12) 0.63533(10) 0.0851(6) Uani 1 1 d . . . Cl3 Cl 0.18040(18) 0.06275(11) 0.53547(15) 0.1114(9) Uani 1 1 d . . . Cl6 Cl 0.7788(2) 0.98103(14) 0.68333(17) 0.1228(10) Uani 1 1 d . . . Cl5 Cl 0.8343(3) 0.85509(16) 0.6585(3) 0.177(2) Uani 1 1 d . . . C2 C 0.2355(7) 0.0636(4) 0.6142(5) 0.097(3) Uani 1 1 d . . . H2A H 0.2349 0.0206 0.6309 0.116 Uiso 1 1 calc R . . H2B H 0.2035 0.0912 0.6351 0.116 Uiso 1 1 calc R . . C3 C 0.8680(8) 0.9285(5) 0.6841(8) 0.142(5) Uani 1 1 d . . . H3A H 0.9002 0.9464 0.6570 0.170 Uiso 1 1 calc R . . H3B H 0.9092 0.9259 0.7277 0.170 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 Pd1 0.02684(19) 0.02880(19) 0.02291(18) -0.00128(14) 0.00896(15) -0.00373(15) Pd2 0.02482(18) 0.02335(18) 0.02160(17) -0.00104(14) 0.00748(14) -0.00063(14) Sn1 0.03157(18) 0.02853(17) 0.02213(16) 0.00158(13) 0.01059(14) -0.00099(14) S2 0.0291(6) 0.0289(6) 0.0249(6) -0.0020(5) 0.0096(5) 0.0012(5) P2 0.0254(7) 0.0471(8) 0.0291(7) 0.0019(6) 0.0101(6) -0.0020(6) P4 0.0286(6) 0.0289(6) 0.0305(6) 0.0004(5) 0.0122(5) -0.0005(5) P1 0.0385(7) 0.0296(7) 0.0263(6) -0.0039(5) 0.0116(6) -0.0099(6) P3 0.0323(7) 0.0248(6) 0.0268(6) -0.0002(5) 0.0085(5) -0.0012(5) S1 0.0296(6) 0.0252(6) 0.0272(6) -0.0011(5) 0.0113(5) 0.0000(5) C311 0.040(3) 0.030(3) 0.029(3) -0.004(2) 0.008(2) -0.004(2) C221 0.026(3) 0.061(4) 0.033(3) 0.001(3) 0.011(2) -0.003(3) C321 0.039(3) 0.025(3) 0.049(3) 0.004(2) 0.017(3) 0.004(2) C316 0.052(4) 0.035(3) 0.043(3) 0.000(2) 0.011(3) -0.007(3) C111 0.036(3) 0.030(3) 0.029(3) 0.000(2) 0.011(2) -0.001(2) C121 0.058(4) 0.027(3) 0.032(3) -0.003(2) 0.007(3) -0.009(3) C431 0.041(3) 0.040(3) 0.035(3) 0.003(2) 0.019(2) -0.003(2) C332 0.043(3) 0.034(3) 0.036(3) 0.004(2) 0.017(2) -0.007(2) C331 0.041(3) 0.028(3) 0.033(3) 0.002(2) 0.011(2) -0.001(2) C216 0.040(3) 0.050(3) 0.040(3) 0.004(3) 0.019(3) 0.005(3) B1 0.041(3) 0.035(3) 0.026(3) 0.000(2) 0.019(3) 0.003(3) B6 0.045(3) 0.033(3) 0.028(3) 0.001(2) 0.018(3) 0.003(3) C421 0.031(3) 0.033(3) 0.046(3) -0.006(2) 0.020(2) 0.000(2) C411 0.029(3) 0.028(3) 0.042(3) 0.001(2) 0.007(2) 0.005(2) C422 0.043(3) 0.050(3) 0.048(3) -0.013(3) 0.020(3) -0.001(3) C212 0.034(3) 0.074(4) 0.041(3) 0.007(3) 0.011(3) 0.000(3) C231 0.032(3) 0.061(4) 0.042(3) -0.001(3) 0.014(3) -0.012(3) C211 0.029(3) 0.049(3) 0.029(3) 0.000(2) 0.008(2) 0.002(2) C426 0.040(3) 0.037(3) 0.056(4) -0.001(3) 0.018(3) 0.003(2) C116 0.047(3) 0.041(3) 0.031(3) -0.004(2) 0.015(2) -0.010(3) B5 0.044(3) 0.030(3) 0.022(3) -0.001(2) 0.013(3) -0.006(3) C312 0.067(4) 0.036(3) 0.033(3) -0.004(2) 0.008(3) -0.014(3) C115 0.056(4) 0.041(3) 0.045(3) 0.004(3) 0.027(3) -0.007(3) C214 0.059(4) 0.060(4) 0.036(3) 0.010(3) 0.012(3) 0.010(3) C412 0.034(3) 0.043(3) 0.063(4) 0.002(3) 0.011(3) 0.004(3) B2 0.052(4) 0.034(3) 0.037(3) 0.000(3) 0.021(3) -0.014(3) C215 0.059(4) 0.063(4) 0.039(3) 0.012(3) 0.024(3) 0.003(3) C131 0.049(3) 0.051(3) 0.040(3) -0.012(3) 0.020(3) -0.028(3) C226 0.044(3) 0.073(4) 0.037(3) 0.005(3) 0.016(3) -0.001(3) C213 0.040(3) 0.068(4) 0.043(3) 0.012(3) 0.000(3) 0.010(3) C222 0.068(4) 0.065(4) 0.050(4) 0.000(3) 0.031(3) 0.003(4) C114 0.074(5) 0.057(4) 0.039(3) 0.007(3) 0.027(3) 0.001(3) C416 0.033(3) 0.065(4) 0.040(3) 0.003(3) 0.006(3) -0.001(3) C112 0.072(4) 0.052(4) 0.033(3) -0.004(3) 0.018(3) -0.021(3) C415 0.059(4) 0.078(5) 0.034(3) -0.001(3) 0.000(3) 0.007(4) B10 0.044(4) 0.044(4) 0.027(3) 0.003(3) 0.010(3) 0.005(3) C425 0.055(4) 0.037(3) 0.083(5) 0.004(3) 0.040(4) 0.004(3) B7 0.047(4) 0.038(3) 0.040(3) 0.003(3) 0.026(3) -0.004(3) B4 0.032(3) 0.037(3) 0.032(3) 0.006(2) 0.013(3) 0.009(3) B9 0.057(4) 0.033(3) 0.037(3) 0.010(3) 0.022(3) 0.012(3) C423 0.061(4) 0.056(4) 0.061(4) -0.029(3) 0.035(4) -0.017(3) B3 0.056(4) 0.026(3) 0.036(3) 0.000(2) 0.023(3) 0.002(3) B11 0.062(4) 0.034(3) 0.034(3) 0.007(3) 0.026(3) 0.004(3) C132 0.032(3) 0.068(4) 0.037(3) -0.007(3) 0.008(2) -0.020(3) C126 0.047(3) 0.040(3) 0.058(4) 0.000(3) 0.009(3) 0.001(3) C315 0.053(4) 0.041(3) 0.059(4) -0.018(3) 0.011(3) -0.017(3) C326 0.065(4) 0.052(4) 0.052(4) 0.014(3) 0.027(3) 0.022(3) C313 0.098(6) 0.048(4) 0.028(3) -0.004(3) 0.005(3) -0.012(4) C122 0.108(6) 0.038(3) 0.043(4) 0.007(3) 0.027(4) 0.001(4) B8 0.074(5) 0.027(3) 0.045(4) -0.001(3) 0.037(4) -0.006(3) C322 0.041(3) 0.061(4) 0.055(4) -0.017(3) 0.000(3) 0.008(3) C225 0.051(4) 0.099(6) 0.034(3) 0.006(3) 0.019(3) -0.003(4) C113 0.093(6) 0.074(5) 0.029(3) -0.008(3) 0.017(3) -0.028(4) C424 0.067(4) 0.037(3) 0.084(5) -0.015(3) 0.050(4) -0.005(3) C224 0.057(4) 0.117(7) 0.037(4) -0.010(4) 0.023(3) -0.008(4) C124 0.078(5) 0.035(3) 0.067(5) 0.004(3) -0.015(4) -0.002(3) C314 0.084(5) 0.050(4) 0.033(3) -0.015(3) -0.007(3) -0.007(4) C223 0.096(6) 0.082(5) 0.066(5) -0.021(4) 0.039(5) 0.011(5) C123 0.129(8) 0.036(4) 0.052(4) 0.007(3) 0.012(5) -0.003(4) C325 0.083(6) 0.080(5) 0.082(6) 0.019(4) 0.053(5) 0.037(5) C414 0.051(4) 0.059(4) 0.065(5) -0.007(4) -0.014(4) 0.012(3) C323 0.052(4) 0.065(5) 0.079(5) -0.010(4) -0.004(4) 0.016(4) C324 0.054(4) 0.058(4) 0.098(6) 0.016(4) 0.028(4) 0.030(4) C125 0.058(4) 0.047(4) 0.084(5) -0.006(4) 0.007(4) 0.007(3) C413 0.031(3) 0.050(4) 0.088(5) -0.008(4) -0.002(3) -0.003(3) Cl2 0.0817(13) 0.0681(11) 0.0622(11) 0.0064(9) 0.0276(10) 0.0101(10) Cl1 0.0996(17) 0.1113(18) 0.0689(13) 0.0228(13) -0.0153(12) -0.0247(15) C1 0.051(4) 0.058(4) 0.088(5) 0.014(4) 0.034(4) -0.002(3) Cl4 0.0814(14) 0.0977(16) 0.0662(12) -0.0007(11) 0.0094(11) -0.0122(12) Cl3 0.0951(17) 0.0699(14) 0.129(2) -0.0196(14) -0.0205(15) 0.0129(13) Cl6 0.142(3) 0.1024(19) 0.145(3) -0.0400(18) 0.075(2) -0.0009(18) Cl5 0.136(3) 0.096(2) 0.348(6) -0.075(3) 0.148(4) -0.037(2) C2 0.120(8) 0.065(5) 0.110(7) 0.009(5) 0.043(6) -0.033(5) C3 0.097(8) 0.098(8) 0.257(17) -0.057(9) 0.092(10) -0.018(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 Pd1 P2 2.2792(14) . ? Pd1 P1 2.2809(13) . ? Pd1 S2 2.3702(12) . ? Pd1 S1 2.3730(13) . ? Pd1 Pd2 3.0968(5) . ? Pd1 Sn1 3.1825(5) . ? Pd2 P4 2.2735(13) . ? Pd2 P3 2.2753(13) . ? Pd2 S1 2.3532(12) . ? Pd2 S2 2.3583(12) . ? Sn1 B2 2.312(6) . ? Sn1 B4 2.331(6) . ? Sn1 B5 2.332(6) . ? Sn1 B3 2.333(6) . ? Sn1 B1 2.343(5) . ? Sn1 S1 2.5359(12) . ? Sn1 S2 2.5653(12) . ? P2 C221 1.803(5) . ? P2 C211 1.807(5) . ? P2 C231 1.824(6) . ? P4 C421 1.806(5) . ? P4 C431 1.818(5) . ? P4 C411 1.819(5) . ? P1 C111 1.808(5) . ? P1 C121 1.808(6) . ? P1 C131 1.823(6) . ? P3 C311 1.801(5) . ? P3 C321 1.810(5) . ? P3 C331 1.817(5) . ? C311 C312 1.389(7) . ? C311 C316 1.397(7) . ? C221 C222 1.367(9) . ? C221 C226 1.390(8) . ? C321 C326 1.373(8) . ? C321 C322 1.395(8) . ? C316 C315 1.381(8) . ? C111 C116 1.383(7) . ? C111 C112 1.385(8) . ? C121 C126 1.372(9) . ? C121 C122 1.388(8) . ? C431 C332 1.520(7) . ? C332 C331 1.542(7) . ? C216 C215 1.382(8) . ? C216 C211 1.385(7) . ? B1 B7 1.754(8) . ? B1 B6 1.756(8) . ? B1 B5 1.893(9) . ? B1 B2 1.922(8) . ? B6 B11 1.759(8) . ? B6 B5 1.769(8) . ? B6 B7 1.775(9) . ? B6 B10 1.786(9) . ? C421 C422 1.376(8) . ? C421 C426 1.406(8) . ? C411 C416 1.379(8) . ? C411 C412 1.382(8) . ? C422 C423 1.399(8) . ? C212 C211 1.385(8) . ? C212 C213 1.391(8) . ? C231 C132 1.532(8) . ? C426 C425 1.372(8) . ? C116 C115 1.387(7) . ? B5 B10 1.769(8) . ? B5 B4 1.910(8) . ? C312 C313 1.369(8) . ? C115 C114 1.361(9) . ? C214 C215 1.369(9) . ? C214 C213 1.383(9) . ? C412 C413 1.398(9) . ? B2 B8 1.764(10) . ? B2 B7 1.781(9) . ? B2 B3 1.898(9) . ? C131 C132 1.514(9) . ? C226 C225 1.380(9) . ? C222 C223 1.406(9) . ? C114 C113 1.359(9) . ? C416 C415 1.385(8) . ? C112 C113 1.394(8) . ? C415 C414 1.362(10) . ? B10 B4 1.780(8) . ? B10 B11 1.782(9) . ? B10 B9 1.787(9) . ? C425 C424 1.368(10) . ? B7 B11 1.759(10) . ? B7 B8 1.775(9) . ? B4 B9 1.773(8) . ? B4 B3 1.884(9) . ? B9 B11 1.776(9) . ? B9 B3 1.776(9) . ? B9 B8 1.779(10) . ? C423 C424 1.357(10) . ? B3 B8 1.756(8) . ? B11 B8 1.771(10) . ? C126 C125 1.397(9) . ? C315 C314 1.378(9) . ? C326 C325 1.402(10) . ? C313 C314 1.366(9) . ? C122 C123 1.372(10) . ? C322 C323 1.380(9) . ? C225 C224 1.344(11) . ? C224 C223 1.389(11) . ? C124 C125 1.355(11) . ? C124 C123 1.373(12) . ? C325 C324 1.369(11) . ? C414 C413 1.361(11) . ? C323 C324 1.346(11) . ? Cl2 C1 1.754(8) . ? Cl1 C1 1.733(7) . ? Cl4 C2 1.723(10) . ? Cl3 C2 1.663(10) . ? Cl6 C3 1.778(11) . ? Cl5 C3 1.656(11) . ? 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 P2 Pd1 P1 94.34(5) . . ? P2 Pd1 S2 91.26(5) . . ? P1 Pd1 S2 174.37(5) . . ? P2 Pd1 S1 173.31(5) . . ? P1 Pd1 S1 92.12(5) . . ? S2 Pd1 S1 82.30(4) . . ? P2 Pd1 Pd2 127.26(4) . . ? P1 Pd1 Pd2 126.25(4) . . ? S2 Pd1 Pd2 48.92(3) . . ? S1 Pd1 Pd2 48.79(3) . . ? P2 Pd1 Sn1 122.38(4) . . ? P1 Pd1 Sn1 124.05(4) . . ? S2 Pd1 Sn1 52.59(3) . . ? S1 Pd1 Sn1 51.86(3) . . ? Pd2 Pd1 Sn1 64.648(11) . . ? P4 Pd2 P3 91.11(5) . . ? P4 Pd2 S1 92.96(4) . . ? P3 Pd2 S1 175.86(5) . . ? P4 Pd2 S2 171.66(5) . . ? P3 Pd2 S2 93.09(4) . . ? S1 Pd2 S2 82.97(4) . . ? P4 Pd2 Pd1 131.91(4) . . ? P3 Pd2 Pd1 126.82(4) . . ? S1 Pd2 Pd1 49.34(3) . . ? S2 Pd2 Pd1 49.25(3) . . ? B2 Sn1 B4 82.6(2) . . ? B2 Sn1 B5 82.9(2) . . ? B4 Sn1 B5 48.3(2) . . ? B2 Sn1 B3 48.2(2) . . ? B4 Sn1 B3 47.6(2) . . ? B5 Sn1 B3 82.4(2) . . ? B2 Sn1 B1 48.8(2) . . ? B4 Sn1 B1 82.5(2) . . ? B5 Sn1 B1 47.8(2) . . ? B3 Sn1 B1 82.7(2) . . ? B2 Sn1 S1 126.09(16) . . ? B4 Sn1 S1 106.13(14) . . ? B5 Sn1 S1 142.15(15) . . ? B3 Sn1 S1 99.15(15) . . ? B1 Sn1 S1 169.96(16) . . ? B2 Sn1 S2 126.17(18) . . ? B4 Sn1 S2 144.36(16) . . ? B5 Sn1 S2 108.83(15) . . ? B3 Sn1 S2 167.59(17) . . ? B1 Sn1 S2 100.71(15) . . ? S1 Sn1 S2 75.44(4) . . ? B2 Sn1 Pd1 107.22(17) . . ? B4 Sn1 Pd1 152.77(14) . . ? B5 Sn1 Pd1 155.64(15) . . ? B3 Sn1 Pd1 121.07(16) . . ? B1 Sn1 Pd1 123.34(15) . . ? S1 Sn1 Pd1 47.39(3) . . ? S2 Sn1 Pd1 47.21(3) . . ? Pd2 S2 Pd1 81.83(4) . . ? Pd2 S2 Sn1 85.91(4) . . ? Pd1 S2 Sn1 80.20(4) . . ? C221 P2 C211 108.8(3) . . ? C221 P2 C231 103.2(3) . . ? C211 P2 C231 102.1(3) . . ? C221 P2 Pd1 111.39(18) . . ? C211 P2 Pd1 114.89(17) . . ? C231 P2 Pd1 115.5(2) . . ? C421 P4 C431 104.8(2) . . ? C421 P4 C411 106.0(2) . . ? C431 P4 C411 106.0(3) . . ? C421 P4 Pd2 114.25(17) . . ? C431 P4 Pd2 116.24(19) . . ? C411 P4 Pd2 108.81(17) . . ? C111 P1 C121 107.2(3) . . ? C111 P1 C131 105.3(3) . . ? C121 P1 C131 103.0(3) . . ? C111 P1 Pd1 112.31(17) . . ? C121 P1 Pd1 112.40(18) . . ? C131 P1 Pd1 115.8(2) . . ? C311 P3 C321 105.8(3) . . ? C311 P3 C331 106.9(2) . . ? C321 P3 C331 102.6(2) . . ? C311 P3 Pd2 110.63(17) . . ? C321 P3 Pd2 114.56(18) . . ? C331 P3 Pd2 115.58(17) . . ? Pd2 S1 Pd1 81.87(4) . . ? Pd2 S1 Sn1 86.69(4) . . ? Pd1 S1 Sn1 80.76(4) . . ? C312 C311 C316 117.8(5) . . ? C312 C311 P3 119.0(4) . . ? C316 C311 P3 123.2(4) . . ? C222 C221 C226 119.2(5) . . ? C222 C221 P2 123.7(4) . . ? C226 C221 P2 117.1(5) . . ? C326 C321 C322 118.4(5) . . ? C326 C321 P3 122.2(5) . . ? C322 C321 P3 119.3(4) . . ? C315 C316 C311 121.2(5) . . ? C116 C111 C112 118.1(5) . . ? C116 C111 P1 119.5(4) . . ? C112 C111 P1 122.2(4) . . ? C126 C121 C122 120.0(6) . . ? C126 C121 P1 122.7(4) . . ? C122 C121 P1 117.4(5) . . ? C332 C431 P4 114.2(4) . . ? C431 C332 C331 113.9(4) . . ? C332 C331 P3 115.8(4) . . ? C215 C216 C211 120.8(6) . . ? B7 B1 B6 60.8(4) . . ? B7 B1 B5 106.3(4) . . ? B6 B1 B5 57.9(3) . . ? B7 B1 B2 57.7(3) . . ? B6 B1 B2 106.4(4) . . ? B5 B1 B2 107.3(4) . . ? B7 B1 Sn1 115.8(3) . . ? B6 B1 Sn1 116.7(3) . . ? B5 B1 Sn1 65.8(2) . . ? B2 B1 Sn1 64.8(2) . . ? B1 B6 B11 109.6(4) . . ? B1 B6 B5 65.0(3) . . ? B11 B6 B5 109.5(4) . . ? B1 B6 B7 59.6(3) . . ? B11 B6 B7 59.7(4) . . ? B5 B6 B7 110.9(4) . . ? B1 B6 B10 111.8(4) . . ? B11 B6 B10 60.3(4) . . ? B5 B6 B10 59.7(3) . . ? B7 B6 B10 108.2(4) . . ? C422 C421 C426 118.7(5) . . ? C422 C421 P4 119.9(4) . . ? C426 C421 P4 121.2(4) . . ? C416 C411 C412 118.5(5) . . ? C416 C411 P4 119.1(4) . . ? C412 C411 P4 122.4(4) . . ? C421 C422 C423 120.0(6) . . ? C211 C212 C213 120.4(6) . . ? C132 C231 P2 113.0(4) . . ? C216 C211 C212 118.7(5) . . ? C216 C211 P2 119.9(4) . . ? C212 C211 P2 121.2(4) . . ? C425 C426 C421 120.2(6) . . ? C111 C116 C115 121.1(5) . . ? B10 B5 B6 60.6(3) . . ? B10 B5 B1 106.4(4) . . ? B6 B5 B1 57.2(3) . . ? B10 B5 B4 57.7(3) . . ? B6 B5 B4 106.1(4) . . ? B1 B5 B4 108.3(4) . . ? B10 B5 Sn1 117.0(3) . . ? B6 B5 Sn1 116.7(4) . . ? B1 B5 Sn1 66.4(2) . . ? B4 B5 Sn1 65.8(2) . . ? C313 C312 C311 121.0(6) . . ? C114 C115 C116 120.3(6) . . ? C215 C214 C213 119.9(6) . . ? C411 C412 C413 119.8(6) . . ? B8 B2 B7 60.1(4) . . ? B8 B2 B3 57.2(3) . . ? B7 B2 B3 105.5(5) . . ? B8 B2 B1 104.9(4) . . ? B7 B2 B1 56.4(3) . . ? B3 B2 B1 108.0(4) . . ? B8 B2 Sn1 116.6(4) . . ? B7 B2 Sn1 116.2(4) . . ? B3 B2 Sn1 66.5(3) . . ? B1 B2 Sn1 66.5(2) . . ? C214 C215 C216 120.3(6) . . ? C132 C131 P1 114.9(4) . . ? C225 C226 C221 121.0(7) . . ? C214 C213 C212 119.8(6) . . ? C221 C222 C223 119.8(7) . . ? C113 C114 C115 119.4(6) . . ? C411 C416 C415 121.5(6) . . ? C111 C112 C113 119.7(6) . . ? C414 C415 C416 119.0(7) . . ? B5 B10 B4 65.1(3) . . ? B5 B10 B11 108.5(5) . . ? B4 B10 B11 108.7(5) . . ? B5 B10 B6 59.7(3) . . ? B4 B10 B6 111.2(4) . . ? B11 B10 B6 59.1(4) . . ? B5 B10 B9 111.4(4) . . ? B4 B10 B9 59.6(3) . . ? B11 B10 B9 59.7(4) . . ? B6 B10 B9 107.6(5) . . ? C424 C425 C426 120.4(6) . . ? B1 B7 B11 109.6(4) . . ? B1 B7 B6 59.7(3) . . ? B11 B7 B6 59.7(4) . . ? B1 B7 B8 111.9(4) . . ? B11 B7 B8 60.1(4) . . ? B6 B7 B8 108.0(5) . . ? B1 B7 B2 65.9(3) . . ? B11 B7 B2 109.8(4) . . ? B6 B7 B2 112.0(4) . . ? B8 B7 B2 59.5(4) . . ? B9 B4 B10 60.4(3) . . ? B9 B4 B3 58.0(3) . . ? B10 B4 B3 106.6(4) . . ? B9 B4 B5 105.8(4) . . ? B10 B4 B5 57.2(3) . . ? B3 B4 B5 108.2(4) . . ? B9 B4 Sn1 117.2(4) . . ? B10 B4 Sn1 116.5(3) . . ? B3 B4 Sn1 66.2(3) . . ? B5 B4 Sn1 65.8(2) . . ? B4 B9 B11 109.2(4) . . ? B4 B9 B3 64.1(3) . . ? B11 B9 B3 108.9(5) . . ? B4 B9 B8 110.1(4) . . ? B11 B9 B8 59.8(4) . . ? B3 B9 B8 59.2(4) . . ? B4 B9 B10 60.0(3) . . ? B11 B9 B10 60.0(4) . . ? B3 B9 B10 111.1(4) . . ? B8 B9 B10 107.9(4) . . ? C424 C423 C422 120.3(6) . . ? B8 B3 B9 60.5(4) . . ? B8 B3 B4 106.2(4) . . ? B9 B3 B4 57.9(3) . . ? B8 B3 B2 57.6(4) . . ? B9 B3 B2 106.5(4) . . ? B4 B3 B2 108.2(4) . . ? B8 B3 Sn1 115.9(4) . . ? B9 B3 Sn1 116.9(4) . . ? B4 B3 Sn1 66.1(2) . . ? B2 B3 Sn1 65.3(3) . . ? B6 B11 B7 60.6(4) . . ? B6 B11 B8 108.9(5) . . ? B7 B11 B8 60.4(4) . . ? B6 B11 B9 109.3(4) . . ? B7 B11 B9 109.1(4) . . ? B8 B11 B9 60.2(4) . . ? B6 B11 B10 60.6(3) . . ? B7 B11 B10 109.1(4) . . ? B8 B11 B10 108.4(4) . . ? B9 B11 B10 60.3(4) . . ? C131 C132 C231 113.1(5) . . ? C121 C126 C125 119.4(7) . . ? C314 C315 C316 119.0(6) . . ? C321 C326 C325 120.2(7) . . ? C314 C313 C312 120.3(6) . . ? C123 C122 C121 119.8(7) . . ? B3 B8 B2 65.3(4) . . ? B3 B8 B11 110.1(5) . . ? B2 B8 B11 110.0(4) . . ? B3 B8 B7 112.1(4) . . ? B2 B8 B7 60.4(4) . . ? B11 B8 B7 59.5(4) . . ? B3 B8 B9 60.3(4) . . ? B2 B8 B9 112.5(4) . . ? B11 B8 B9 60.0(4) . . ? B7 B8 B9 108.3(5) . . ? C323 C322 C321 120.4(6) . . ? C224 C225 C226 119.8(7) . . ? C114 C113 C112 121.4(6) . . ? C423 C424 C425 120.5(6) . . ? C225 C224 C223 120.9(6) . . ? C125 C124 C123 120.6(7) . . ? C313 C314 C315 120.7(6) . . ? C224 C223 C222 119.3(8) . . ? C122 C123 C124 120.0(7) . . ? C324 C325 C326 119.9(7) . . ? C413 C414 C415 121.0(6) . . ? C324 C323 C322 120.8(7) . . ? C323 C324 C325 120.2(7) . . ? C124 C125 C126 120.1(7) . . ? C414 C413 C412 120.0(6) . . ? Cl1 C1 Cl2 110.9(4) . . ? Cl3 C2 Cl4 115.5(5) . . ? Cl5 C3 Cl6 113.4(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.994 _refine_diff_density_min -0.965 _refine_diff_density_rms 0.090 # Attachment '765678_compound_9.cif' data_hornung128 _database_code_depnum_ccdc_archive 'CCDC 765678' #TrackingRef '765678_compound_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H63 B11 P4 Pt2 S2 Sn, 3(C H2 Cl2)' _chemical_formula_sum 'C57 H69 B11 Cl6 P4 Pt2 S2 Sn' _chemical_formula_weight 1782.63 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' B B 0.0013 0.0007 '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' Pt Pt -1.7033 8.3905 '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' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.7902(7) _cell_length_b 20.8158(10) _cell_length_c 21.8516(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.343(3) _cell_angle_gamma 90.00 _cell_volume 6817.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 44129 _cell_measurement_theta_min 3.69 _cell_measurement_theta_max 59.18 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1950 _exptl_crystal_size_mid 0.1870 _exptl_crystal_size_min 0.1413 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3464 _exptl_absorpt_coefficient_mu 4.885 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4424 _exptl_absorpt_correction_T_max 0.5580 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS II 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78142 _diffrn_reflns_av_R_equivalents 0.1132 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.67 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12309 _reflns_number_gt 9898 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep3 for windows' _computing_publication_material ? _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. Due to moderate crystal quality even after several attempts of crystallization the R(int) has a valu > 0.1 ; _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^)+(0.0000P)^2^+45.9858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12309 _refine_ls_number_parameters 748 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0587 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _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 C421 C 0.0410(5) 0.6565(4) 0.5822(4) 0.0282(18) Uani 1 1 d . . . C411 C -0.0354(5) 0.7403(4) 0.4731(4) 0.0300(19) Uani 1 1 d . . . C331 C 0.1268(6) 0.8858(4) 0.5814(4) 0.0298(19) Uani 1 1 d . . . H33A H 0.1676 0.8785 0.6244 0.036 Uiso 1 1 calc R . . H33B H 0.1229 0.9318 0.5744 0.036 Uiso 1 1 calc R . . C431 C 0.0350(6) 0.7927(4) 0.6025(4) 0.0302(19) Uani 1 1 d . . . H43A H -0.0224 0.7838 0.6080 0.036 Uiso 1 1 calc R . . H43B H 0.0801 0.7884 0.6443 0.036 Uiso 1 1 calc R . . C332 C 0.0352(6) 0.8616(4) 0.5796(4) 0.035(2) Uani 1 1 d . . . H33C H 0.0122 0.8893 0.6065 0.042 Uiso 1 1 calc R . . H33D H -0.0049 0.8649 0.5358 0.042 Uiso 1 1 calc R . . C321 C 0.2812(6) 0.8918(4) 0.5409(5) 0.034(2) Uani 1 1 d . . . C121 C 0.3276(7) 0.5111(4) 0.6238(4) 0.037(2) Uani 1 1 d . . . C111 C 0.3729(6) 0.6071(4) 0.7256(4) 0.0275(19) Uani 1 1 d . . . C311 C 0.1083(6) 0.8772(4) 0.4447(4) 0.031(2) Uani 1 1 d . . . C312 C 0.0534(6) 0.9305(4) 0.4347(5) 0.040(2) Uani 1 1 d . . . H312 H 0.0501 0.9544 0.4698 0.047 Uiso 1 1 calc R . . C231 C 0.5927(6) 0.6394(5) 0.6418(5) 0.041(2) Uani 1 1 d . . . H23A H 0.5934 0.6091 0.6082 0.049 Uiso 1 1 calc R . . H23B H 0.6504 0.6605 0.6560 0.049 Uiso 1 1 calc R . . C221 C 0.5358(5) 0.7310(5) 0.5403(4) 0.033(2) Uani 1 1 d . . . C132 C 0.5794(6) 0.6028(5) 0.6981(4) 0.045(3) Uani 1 1 d . . . H13A H 0.6352 0.5825 0.7222 0.054 Uiso 1 1 calc R . . H13B H 0.5635 0.6329 0.7266 0.054 Uiso 1 1 calc R . . C212 C 0.6145(6) 0.7902(5) 0.6906(4) 0.044(2) Uani 1 1 d . . . H212 H 0.6570 0.7805 0.6707 0.053 Uiso 1 1 calc R . . C211 C 0.5317(5) 0.7601(5) 0.6706(4) 0.036(2) Uani 1 1 d . . . C426 C 0.0827(7) 0.6443(5) 0.6465(5) 0.042(2) Uani 1 1 d . . . H426 H 0.1144 0.6769 0.6731 0.050 Uiso 1 1 calc R . . C216 C 0.4714(6) 0.7729(5) 0.7031(4) 0.040(2) Uani 1 1 d . . . H216 H 0.4166 0.7520 0.6909 0.048 Uiso 1 1 calc R . . B3 B 0.3067(7) 0.6517(5) 0.3431(4) 0.029(2) Uani 1 1 d . . . H3 H 0.3605 0.6876 0.3530 0.035 Uiso 1 1 calc R . . C131 C 0.5078(6) 0.5520(5) 0.6772(5) 0.042(3) Uani 1 1 d . . . H13C H 0.5149 0.5222 0.7126 0.051 Uiso 1 1 calc R . . H13D H 0.5165 0.5281 0.6415 0.051 Uiso 1 1 calc R . . C222 C 0.5531(7) 0.7947(5) 0.5331(5) 0.048(3) Uani 1 1 d . . . H222 H 0.5522 0.8243 0.5648 0.058 Uiso 1 1 calc R . . C116 C 0.3160(6) 0.6576(4) 0.7248(4) 0.036(2) Uani 1 1 d . . . H116 H 0.2867 0.6778 0.6859 0.044 Uiso 1 1 calc R . . C412 C -0.1178(6) 0.7644(5) 0.4717(5) 0.045(2) Uani 1 1 d . . . H412 H -0.1278 0.7775 0.5095 0.054 Uiso 1 1 calc R . . C422 C -0.0073(7) 0.6076(4) 0.5437(5) 0.041(2) Uani 1 1 d . . . H422 H -0.0353 0.6152 0.5000 0.049 Uiso 1 1 calc R . . C316 C 0.1131(7) 0.8420(5) 0.3913(4) 0.045(2) Uani 1 1 d . . . H316 H 0.1491 0.8058 0.3969 0.053 Uiso 1 1 calc R . . C322 C 0.3053(7) 0.9255(5) 0.4942(5) 0.050(3) Uani 1 1 d . . . H322 H 0.2667 0.9272 0.4521 0.059 Uiso 1 1 calc R . . C122 C 0.2698(6) 0.4869(4) 0.6528(5) 0.042(2) Uani 1 1 d . . . H122 H 0.2636 0.5065 0.6894 0.050 Uiso 1 1 calc R . . C115 C 0.3016(7) 0.6788(5) 0.7803(5) 0.041(2) Uani 1 1 d . . . H115 H 0.2622 0.7126 0.7782 0.050 Uiso 1 1 calc R . . C214 C 0.5737(7) 0.8468(5) 0.7730(5) 0.048(3) Uani 1 1 d . . . H214 H 0.5881 0.8750 0.8078 0.057 Uiso 1 1 calc R . . B4 B 0.1857(7) 0.6742(5) 0.3221(5) 0.033(2) Uani 1 1 d . . . H4 H 0.1631 0.7244 0.3191 0.040 Uiso 1 1 calc R . . C112 C 0.4160(7) 0.5785(5) 0.7852(5) 0.049(3) Uani 1 1 d . . . H112 H 0.4545 0.5441 0.7877 0.058 Uiso 1 1 calc R . . C215 C 0.4913(7) 0.8164(5) 0.7536(5) 0.048(3) Uani 1 1 d . . . H215 H 0.4496 0.8252 0.7744 0.058 Uiso 1 1 calc R . . C423 C -0.0144(7) 0.5477(5) 0.5689(6) 0.052(3) Uani 1 1 d . . . H423 H -0.0476 0.5154 0.5428 0.062 Uiso 1 1 calc R . . C415 C -0.0901(8) 0.7259(5) 0.3578(5) 0.054(3) Uani 1 1 d . . . H415 H -0.0810 0.7130 0.3197 0.064 Uiso 1 1 calc R . . C226 C 0.5339(6) 0.6882(5) 0.4915(4) 0.044(2) Uani 1 1 d . . . H226 H 0.5203 0.6453 0.4955 0.053 Uiso 1 1 calc R . . C416 C -0.0221(6) 0.7217(5) 0.4161(5) 0.044(2) Uani 1 1 d . . . H416 H 0.0334 0.7060 0.4169 0.053 Uiso 1 1 calc R . . B2 B 0.3202(8) 0.5685(5) 0.3830(5) 0.040(3) Uani 1 1 d . . . H2 H 0.3826 0.5518 0.4183 0.048 Uiso 1 1 calc R . . C114 C 0.3440(7) 0.6510(5) 0.8382(5) 0.052(3) Uani 1 1 d . . . H114 H 0.3342 0.6654 0.8757 0.062 Uiso 1 1 calc R . . B5 B 0.1239(7) 0.6056(5) 0.3477(5) 0.030(2) Uani 1 1 d . . . H5 H 0.0624 0.6126 0.3603 0.036 Uiso 1 1 calc R . . C313 C 0.0038(7) 0.9484(5) 0.3734(5) 0.050(3) Uani 1 1 d . . . H313 H -0.0340 0.9838 0.3673 0.060 Uiso 1 1 calc R . . C213 C 0.6337(7) 0.8351(6) 0.7406(5) 0.049(3) Uani 1 1 d . . . H213 H 0.6876 0.8572 0.7521 0.059 Uiso 1 1 calc R . . B10 B 0.1255(7) 0.6152(5) 0.2670(5) 0.033(2) Uani 1 1 d . . . H10 H 0.0635 0.6292 0.2293 0.040 Uiso 1 1 calc R . . C425 C 0.0782(7) 0.5838(5) 0.6722(5) 0.051(3) Uani 1 1 d . . . H425 H 0.1088 0.5754 0.7153 0.061 Uiso 1 1 calc R . . C126 C 0.3404(9) 0.4811(5) 0.5706(5) 0.058(3) Uani 1 1 d . . . H126 H 0.3809 0.4973 0.5516 0.070 Uiso 1 1 calc R . . B9 B 0.2313(7) 0.6410(5) 0.2644(5) 0.033(2) Uani 1 1 d . . . H9 H 0.2378 0.6712 0.2248 0.040 Uiso 1 1 calc R . . C424 C 0.0287(7) 0.5368(5) 0.6339(6) 0.053(3) Uani 1 1 d . . . H424 H 0.0238 0.4968 0.6515 0.064 Uiso 1 1 calc R . . B8 B 0.3102(8) 0.5808(5) 0.3004(5) 0.034(2) Uani 1 1 d . . . H8 H 0.3688 0.5723 0.2845 0.041 Uiso 1 1 calc R . . C113 C 0.4016(9) 0.6011(6) 0.8400(5) 0.062(3) Uani 1 1 d . . . H113 H 0.4316 0.5821 0.8794 0.075 Uiso 1 1 calc R . . B6 B 0.1392(8) 0.5371(5) 0.3036(5) 0.040(3) Uani 1 1 d . . . H6 H 0.0866 0.5003 0.2894 0.049 Uiso 1 1 calc R . . C326 C 0.3421(7) 0.8890(5) 0.6020(6) 0.054(3) Uani 1 1 d . . . H326 H 0.3279 0.8658 0.6338 0.065 Uiso 1 1 calc R . . C315 C 0.0639(9) 0.8619(5) 0.3306(5) 0.062(3) Uani 1 1 d . . . H315 H 0.0677 0.8389 0.2951 0.074 Uiso 1 1 calc R . . B7 B 0.2535(8) 0.5172(5) 0.3240(5) 0.036(3) Uani 1 1 d . . . H7 H 0.2752 0.4671 0.3229 0.044 Uiso 1 1 calc R . . C323 C 0.3860(9) 0.9562(6) 0.5101(7) 0.071(4) Uani 1 1 d . . . H323 H 0.4001 0.9801 0.4787 0.085 Uiso 1 1 calc R . . Cl1 Cl 0.7780(2) 0.69722(16) 0.57911(15) 0.0688(8) Uani 1 1 d . . . B11 B 0.2020(8) 0.5600(5) 0.2530(5) 0.037(3) Uani 1 1 d . . . H11 H 0.1894 0.5376 0.2054 0.045 Uiso 1 1 calc R . . C224 C 0.5713(7) 0.7712(7) 0.4298(5) 0.062(3) Uani 1 1 d . . . H224 H 0.5840 0.7850 0.3932 0.074 Uiso 1 1 calc R . . C413 C -0.1855(7) 0.7687(5) 0.4128(7) 0.060(3) Uani 1 1 d . . . H413 H -0.2410 0.7849 0.4114 0.072 Uiso 1 1 calc R . . C225 C 0.5525(7) 0.7090(6) 0.4361(5) 0.053(3) Uani 1 1 d . . . H225 H 0.5518 0.6798 0.4037 0.063 Uiso 1 1 calc R . . C124 C 0.2324(9) 0.4020(5) 0.5740(6) 0.065(4) Uani 1 1 d . . . H124 H 0.2005 0.3649 0.5574 0.078 Uiso 1 1 calc R . . C324 C 0.4473(9) 0.9528(6) 0.5713(7) 0.067(4) Uani 1 1 d . . . H324 H 0.5029 0.9723 0.5810 0.080 Uiso 1 1 calc R . . C414 C -0.1716(8) 0.7497(6) 0.3578(6) 0.067(4) Uani 1 1 d . . . H414 H -0.2179 0.7527 0.3190 0.080 Uiso 1 1 calc R . . C123 C 0.2198(8) 0.4323(6) 0.6267(7) 0.065(3) Uani 1 1 d . . . H123 H 0.1780 0.4165 0.6448 0.078 Uiso 1 1 calc R . . C314 C 0.0097(8) 0.9143(5) 0.3210(5) 0.056(3) Uani 1 1 d . . . H314 H -0.0230 0.9269 0.2794 0.067 Uiso 1 1 calc R . . C223 C 0.5720(9) 0.8150(6) 0.4779(6) 0.071(4) Uani 1 1 d . . . H223 H 0.5851 0.8579 0.4733 0.085 Uiso 1 1 calc R . . C325 C 0.4228(8) 0.9194(5) 0.6170(7) 0.068(4) Uani 1 1 d . . . H325 H 0.4616 0.9175 0.6590 0.082 Uiso 1 1 calc R . . C125 C 0.2917(10) 0.4267(6) 0.5468(6) 0.074(4) Uani 1 1 d . . . H125 H 0.2996 0.4063 0.5111 0.089 Uiso 1 1 calc R . . C1 C 0.8379(8) 0.6454(6) 0.6405(6) 0.063(3) Uani 1 1 d . . . H1A H 0.8086 0.6038 0.6350 0.075 Uiso 1 1 calc R . . H1B H 0.8975 0.6393 0.6378 0.075 Uiso 1 1 calc R . . Cl2 Cl 0.8446(3) 0.6766(2) 0.71602(18) 0.1060(15) Uani 1 1 d . . . Cl5 Cl 0.6538(2) 0.58894(18) 0.86614(16) 0.0798(10) Uani 1 1 d . . . Cl6 Cl 0.8212(3) 0.56203(17) 0.9631(2) 0.1019(14) Uani 1 1 d . . . Cl3 Cl 0.2196(4) 0.4804(2) 0.8170(3) 0.1179(16) Uani 1 1 d . . . Cl4 Cl 0.1665(4) 0.3550(2) 0.8437(4) 0.181(3) Uani 1 1 d . . . C3 C 0.7616(10) 0.5626(7) 0.8838(7) 0.092(5) Uani 1 1 d . . . H3A H 0.7607 0.5194 0.8670 0.110 Uiso 1 1 calc R . . H3B H 0.7921 0.5897 0.8613 0.110 Uiso 1 1 calc R . . C2 C 0.1339(12) 0.4279(8) 0.8195(13) 0.152(10) Uani 1 1 d . . . H2A H 0.1038 0.4458 0.8480 0.183 Uiso 1 1 calc R . . H2B H 0.0906 0.4255 0.7767 0.183 Uiso 1 1 calc R . . Pt2 Pt 0.18760(2) 0.742135(14) 0.528482(14) 0.02032(8) Uani 1 1 d . . . Pt1 Pt 0.36543(2) 0.661632(15) 0.577885(15) 0.02296(8) Uani 1 1 d . . . Sn1 Sn 0.24858(4) 0.64231(3) 0.42860(3) 0.02491(13) Uani 1 1 d . . . S2 S 0.31759(13) 0.74142(10) 0.49645(9) 0.0258(4) Uani 1 1 d . . . S1 S 0.21354(13) 0.63033(9) 0.53402(9) 0.0242(4) Uani 1 1 d . . . P3 P 0.17586(14) 0.85041(10) 0.52380(10) 0.0257(5) Uani 1 1 d . . . P4 P 0.05606(14) 0.73302(10) 0.54832(10) 0.0258(5) Uani 1 1 d . . . P1 P 0.39441(15) 0.58260(10) 0.65251(10) 0.0278(5) Uani 1 1 d . . . P2 P 0.50685(15) 0.69940(12) 0.60817(11) 0.0303(5) Uani 1 1 d . . . B1 B 0.2076(8) 0.5407(5) 0.3848(5) 0.036(2) Uani 1 1 d . . . H1 H 0.1988 0.5067 0.4208 0.043 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 C421 0.025(4) 0.030(5) 0.035(5) 0.003(4) 0.016(4) 0.002(4) C411 0.023(4) 0.024(4) 0.037(5) 0.000(4) 0.000(4) -0.005(4) C331 0.041(5) 0.025(4) 0.024(4) -0.002(3) 0.011(4) -0.002(4) C431 0.029(5) 0.034(5) 0.032(5) -0.009(4) 0.016(4) -0.002(4) C332 0.048(6) 0.030(5) 0.031(5) -0.012(4) 0.017(4) 0.003(4) C321 0.036(5) 0.018(4) 0.045(6) -0.002(4) 0.009(4) 0.004(4) C121 0.058(6) 0.021(4) 0.033(5) 0.004(4) 0.013(5) 0.010(4) C111 0.036(5) 0.025(4) 0.024(4) 0.001(3) 0.013(4) -0.006(4) C311 0.034(5) 0.029(5) 0.027(5) 0.004(4) 0.006(4) 0.003(4) C312 0.045(6) 0.034(5) 0.040(5) 0.005(4) 0.012(5) 0.012(4) C231 0.031(5) 0.054(6) 0.038(5) 0.003(5) 0.013(4) 0.009(5) C221 0.020(4) 0.052(6) 0.028(5) -0.004(4) 0.007(4) 0.004(4) C132 0.030(5) 0.073(7) 0.029(5) 0.007(5) 0.006(4) 0.029(5) C212 0.034(5) 0.071(7) 0.027(5) -0.005(5) 0.008(4) -0.007(5) C211 0.019(4) 0.056(6) 0.030(5) 0.000(4) 0.002(4) 0.004(4) C426 0.049(6) 0.042(6) 0.041(6) 0.006(4) 0.024(5) -0.007(5) C216 0.029(5) 0.056(6) 0.032(5) -0.004(4) 0.005(4) -0.007(4) B3 0.041(6) 0.027(5) 0.026(5) -0.007(4) 0.019(5) -0.006(4) C131 0.043(6) 0.052(6) 0.035(5) 0.016(5) 0.017(5) 0.031(5) C222 0.055(7) 0.054(7) 0.039(6) -0.004(5) 0.019(5) 0.005(5) C116 0.047(6) 0.032(5) 0.031(5) 0.000(4) 0.012(4) 0.006(4) C412 0.030(5) 0.040(5) 0.059(6) -0.004(5) 0.006(5) 0.004(4) C422 0.043(6) 0.032(5) 0.054(6) 0.005(4) 0.024(5) 0.000(4) C316 0.060(7) 0.033(5) 0.037(5) 0.002(4) 0.010(5) 0.009(5) C322 0.058(7) 0.055(7) 0.042(6) -0.008(5) 0.024(5) -0.025(5) C122 0.036(5) 0.034(5) 0.049(6) 0.002(4) 0.004(5) 0.000(4) C115 0.052(6) 0.039(6) 0.042(6) -0.002(4) 0.027(5) 0.009(5) C214 0.047(6) 0.059(7) 0.032(5) -0.009(5) 0.006(5) -0.009(5) B4 0.042(6) 0.025(5) 0.032(5) -0.003(4) 0.010(5) -0.008(5) C112 0.068(7) 0.047(6) 0.036(6) 0.010(5) 0.024(5) 0.021(5) C215 0.048(6) 0.067(7) 0.035(5) -0.010(5) 0.020(5) 0.003(5) C423 0.055(7) 0.030(5) 0.080(9) -0.005(5) 0.035(6) -0.011(5) C415 0.065(8) 0.057(7) 0.032(5) 0.000(5) 0.005(5) -0.012(6) C226 0.042(6) 0.057(6) 0.034(5) -0.003(5) 0.011(5) 0.003(5) C416 0.030(5) 0.058(7) 0.038(6) -0.005(5) 0.003(4) 0.004(5) B2 0.052(7) 0.047(7) 0.024(5) 0.003(5) 0.016(5) 0.025(6) C114 0.064(7) 0.064(7) 0.035(6) -0.011(5) 0.028(5) 0.005(6) B5 0.032(6) 0.028(5) 0.035(6) -0.003(4) 0.018(5) -0.003(4) C313 0.040(6) 0.041(6) 0.062(7) 0.019(5) 0.007(5) 0.014(5) C213 0.035(5) 0.071(7) 0.038(5) -0.013(5) 0.007(4) -0.016(5) B10 0.039(6) 0.034(6) 0.027(5) 0.000(4) 0.011(5) 0.002(5) C425 0.058(7) 0.051(7) 0.054(7) 0.026(5) 0.032(6) 0.016(6) C126 0.098(10) 0.031(5) 0.044(6) -0.004(5) 0.020(6) -0.006(6) B9 0.043(6) 0.033(6) 0.023(5) -0.002(4) 0.011(5) -0.005(5) C424 0.055(7) 0.040(6) 0.084(9) 0.017(6) 0.051(7) 0.005(5) B8 0.048(7) 0.028(5) 0.037(6) -0.002(4) 0.028(5) 0.008(5) C113 0.090(9) 0.071(8) 0.022(5) 0.015(5) 0.013(6) 0.032(7) B6 0.062(8) 0.024(5) 0.043(6) -0.014(5) 0.029(6) -0.017(5) C326 0.037(6) 0.046(6) 0.066(7) 0.015(5) -0.004(5) -0.011(5) C315 0.103(10) 0.046(6) 0.028(5) 0.010(5) 0.008(6) 0.010(6) B7 0.063(8) 0.018(5) 0.037(6) -0.005(4) 0.029(6) 0.008(5) C323 0.075(9) 0.078(9) 0.083(10) -0.019(7) 0.058(8) -0.036(7) Cl1 0.082(2) 0.069(2) 0.0583(18) -0.0062(15) 0.0267(17) -0.0124(17) B11 0.063(8) 0.029(6) 0.022(5) -0.007(4) 0.016(5) 0.003(5) C224 0.051(7) 0.096(10) 0.040(6) 0.018(6) 0.018(5) 0.001(7) C413 0.035(6) 0.041(6) 0.091(9) -0.004(6) 0.001(6) -0.006(5) C225 0.050(7) 0.084(9) 0.027(5) -0.007(5) 0.018(5) 0.000(6) C124 0.073(9) 0.036(6) 0.055(7) -0.003(6) -0.023(7) -0.002(6) C324 0.056(8) 0.056(7) 0.090(10) -0.020(7) 0.026(7) -0.031(6) C414 0.045(7) 0.059(8) 0.070(8) 0.020(7) -0.019(6) -0.013(6) C123 0.043(7) 0.049(7) 0.090(10) 0.011(7) 0.002(6) 0.000(6) C314 0.074(8) 0.043(6) 0.035(6) 0.016(5) -0.008(5) 0.005(6) C223 0.098(10) 0.064(8) 0.059(8) 0.012(6) 0.036(8) -0.012(7) C325 0.058(8) 0.048(7) 0.081(9) 0.000(6) -0.003(7) -0.019(6) C125 0.113(12) 0.037(7) 0.056(8) -0.001(6) 0.005(8) 0.006(7) C1 0.048(7) 0.054(7) 0.094(9) -0.001(7) 0.035(7) 0.007(6) Cl2 0.102(3) 0.113(3) 0.069(2) -0.025(2) -0.021(2) 0.028(2) Cl5 0.077(2) 0.093(3) 0.059(2) -0.0014(18) 0.0068(17) 0.0107(19) Cl6 0.082(3) 0.064(2) 0.126(3) 0.015(2) -0.016(2) -0.007(2) Cl3 0.138(4) 0.101(3) 0.138(4) 0.035(3) 0.077(3) -0.004(3) Cl4 0.142(5) 0.090(3) 0.367(10) 0.081(5) 0.160(6) 0.039(3) C3 0.091(11) 0.075(10) 0.103(12) -0.009(9) 0.022(9) 0.035(8) C2 0.097(13) 0.081(12) 0.32(3) 0.063(15) 0.117(17) 0.020(10) Pt2 0.02135(15) 0.01977(16) 0.01871(14) 0.00081(12) 0.00471(11) 0.00023(13) Pt1 0.02321(16) 0.02525(16) 0.02084(15) 0.00104(13) 0.00755(12) 0.00396(14) Sn1 0.0286(3) 0.0259(3) 0.0212(3) -0.0015(2) 0.0093(2) 0.0004(2) S2 0.0259(10) 0.0273(11) 0.0248(10) 0.0025(9) 0.0088(8) -0.0028(9) S1 0.0244(11) 0.0235(10) 0.0243(10) 0.0026(8) 0.0072(9) 0.0007(8) P3 0.0273(12) 0.0221(11) 0.0250(11) -0.0014(9) 0.0042(9) 0.0001(9) P4 0.0239(11) 0.0263(11) 0.0280(11) -0.0019(9) 0.0094(9) -0.0006(9) P1 0.0338(13) 0.0246(11) 0.0257(11) 0.0041(9) 0.0105(10) 0.0075(9) P2 0.0211(11) 0.0441(14) 0.0256(11) -0.0017(10) 0.0072(9) 0.0053(10) B1 0.050(7) 0.035(6) 0.028(5) -0.003(4) 0.020(5) -0.006(5) _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 C421 C426 1.375(12) . ? C421 C422 1.387(12) . ? C421 P4 1.803(9) . ? C411 C416 1.381(12) . ? C411 C412 1.386(12) . ? C411 P4 1.821(8) . ? C331 C332 1.521(12) . ? C331 P3 1.827(8) . ? C431 C332 1.518(12) . ? C431 P4 1.817(8) . ? C321 C326 1.380(13) . ? C321 C322 1.386(13) . ? C321 P3 1.805(9) . ? C121 C122 1.361(13) . ? C121 C126 1.387(14) . ? C121 P1 1.818(10) . ? C111 C116 1.381(12) . ? C111 C112 1.399(12) . ? C111 P1 1.808(8) . ? C311 C312 1.382(12) . ? C311 C316 1.399(12) . ? C311 P3 1.810(9) . ? C312 C313 1.374(13) . ? C231 C132 1.516(13) . ? C231 P2 1.820(9) . ? C221 C222 1.374(14) . ? C221 C226 1.382(13) . ? C221 P2 1.807(9) . ? C132 C131 1.510(14) . ? C212 C211 1.391(12) . ? C212 C213 1.398(13) . ? C211 C216 1.382(12) . ? C211 P2 1.810(9) . ? C426 C425 1.390(13) . ? C216 C215 1.384(13) . ? B3 B8 1.758(13) . ? B3 B9 1.771(14) . ? B3 B4 1.878(15) . ? B3 B2 1.920(15) . ? B3 Sn1 2.333(9) . ? C131 P1 1.815(9) . ? C222 C223 1.396(15) . ? C116 C115 1.374(12) . ? C412 C413 1.393(14) . ? C422 C423 1.381(13) . ? C316 C315 1.373(13) . ? C322 C323 1.369(15) . ? C122 C123 1.399(14) . ? C115 C114 1.361(13) . ? C214 C213 1.370(14) . ? C214 C215 1.387(14) . ? B4 B10 1.772(14) . ? B4 B9 1.778(14) . ? B4 B5 1.909(14) . ? B4 Sn1 2.321(10) . ? C112 C113 1.370(14) . ? C423 C424 1.386(15) . ? C415 C414 1.378(16) . ? C415 C416 1.387(13) . ? C226 C225 1.401(14) . ? B2 B7 1.749(16) . ? B2 B8 1.780(14) . ? B2 B1 1.881(16) . ? B2 Sn1 2.311(10) . ? C114 C113 1.373(15) . ? B5 B6 1.779(14) . ? B5 B10 1.782(14) . ? B5 B1 1.886(15) . ? B5 Sn1 2.323(10) . ? C313 C314 1.375(15) . ? B10 B11 1.762(15) . ? B10 B9 1.774(15) . ? B10 B6 1.795(15) . ? C425 C424 1.363(15) . ? C126 C125 1.375(16) . ? B9 B11 1.746(14) . ? B9 B8 1.769(15) . ? B8 B11 1.752(16) . ? B8 B7 1.765(15) . ? B6 B1 1.763(15) . ? B6 B7 1.766(17) . ? B6 B11 1.768(15) . ? C326 C325 1.367(14) . ? C315 C314 1.362(15) . ? B7 B11 1.753(15) . ? B7 B1 1.770(14) . ? C323 C324 1.386(17) . ? Cl1 C1 1.749(12) . ? C224 C225 1.347(16) . ? C224 C223 1.388(17) . ? C413 C414 1.347(17) . ? C124 C125 1.360(18) . ? C124 C123 1.381(17) . ? C324 C325 1.368(17) . ? C1 Cl2 1.745(13) . ? Cl5 C3 1.712(14) . ? Cl6 C3 1.693(15) . ? Cl3 C2 1.754(16) . ? Cl4 C2 1.636(16) . ? Pt2 P4 2.259(2) . ? Pt2 P3 2.261(2) . ? Pt2 S1 2.360(2) . ? Pt2 S2 2.368(2) . ? Pt2 Pt1 3.1544(4) . ? Pt1 P1 2.259(2) . ? Pt1 P2 2.261(2) . ? Pt1 S1 2.377(2) . ? Pt1 S2 2.377(2) . ? Pt1 Sn1 3.2280(6) . ? Sn1 B1 2.328(10) . ? Sn1 S1 2.545(2) . ? Sn1 S2 2.574(2) . ? 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 C426 C421 C422 118.7(8) . . ? C426 C421 P4 120.0(7) . . ? C422 C421 P4 121.2(7) . . ? C416 C411 C412 119.3(8) . . ? C416 C411 P4 119.2(7) . . ? C412 C411 P4 121.5(7) . . ? C332 C331 P3 117.1(6) . . ? C332 C431 P4 114.3(6) . . ? C431 C332 C331 113.8(7) . . ? C326 C321 C322 117.7(9) . . ? C326 C321 P3 119.8(8) . . ? C322 C321 P3 122.6(8) . . ? C122 C121 C126 121.2(10) . . ? C122 C121 P1 122.9(7) . . ? C126 C121 P1 115.9(8) . . ? C116 C111 C112 117.4(8) . . ? C116 C111 P1 120.4(6) . . ? C112 C111 P1 122.1(7) . . ? C312 C311 C316 118.9(8) . . ? C312 C311 P3 123.4(7) . . ? C316 C311 P3 117.7(7) . . ? C313 C312 C311 120.7(9) . . ? C132 C231 P2 113.3(6) . . ? C222 C221 C226 119.3(9) . . ? C222 C221 P2 123.8(7) . . ? C226 C221 P2 116.7(8) . . ? C131 C132 C231 112.9(8) . . ? C211 C212 C213 119.8(9) . . ? C216 C211 C212 119.0(9) . . ? C216 C211 P2 120.1(7) . . ? C212 C211 P2 120.7(7) . . ? C421 C426 C425 120.7(10) . . ? C211 C216 C215 121.0(9) . . ? B8 B3 B9 60.1(6) . . ? B8 B3 B4 106.2(7) . . ? B9 B3 B4 58.2(6) . . ? B8 B3 B2 57.7(5) . . ? B9 B3 B2 105.8(7) . . ? B4 B3 B2 107.1(7) . . ? B8 B3 Sn1 116.2(6) . . ? B9 B3 Sn1 117.0(6) . . ? B4 B3 Sn1 65.8(4) . . ? B2 B3 Sn1 65.0(4) . . ? C132 C131 P1 114.8(7) . . ? C221 C222 C223 119.8(10) . . ? C115 C116 C111 121.4(9) . . ? C411 C412 C413 119.0(10) . . ? C423 C422 C421 121.2(10) . . ? C315 C316 C311 119.0(9) . . ? C323 C322 C321 119.9(11) . . ? C121 C122 C123 119.1(11) . . ? C114 C115 C116 121.0(9) . . ? C213 C214 C215 119.7(9) . . ? B10 B4 B9 60.0(6) . . ? B10 B4 B3 106.3(7) . . ? B9 B4 B3 57.9(5) . . ? B10 B4 B5 57.8(5) . . ? B9 B4 B5 106.0(7) . . ? B3 B4 B5 108.5(7) . . ? B10 B4 Sn1 116.9(6) . . ? B9 B4 Sn1 117.3(6) . . ? B3 B4 Sn1 66.6(4) . . ? B5 B4 Sn1 65.8(4) . . ? C113 C112 C111 120.1(9) . . ? C216 C215 C214 119.9(9) . . ? C422 C423 C424 118.8(10) . . ? C414 C415 C416 118.5(11) . . ? C221 C226 C225 120.6(10) . . ? C411 C416 C415 121.1(10) . . ? B7 B2 B8 60.0(6) . . ? B7 B2 B1 58.2(6) . . ? B8 B2 B1 106.4(8) . . ? B7 B2 B3 105.2(7) . . ? B8 B2 B3 56.6(5) . . ? B1 B2 B3 108.4(7) . . ? B7 B2 Sn1 117.5(7) . . ? B8 B2 Sn1 116.3(6) . . ? B1 B2 Sn1 66.6(4) . . ? B3 B2 Sn1 66.2(4) . . ? C115 C114 C113 118.4(9) . . ? B6 B5 B10 60.5(6) . . ? B6 B5 B1 57.4(6) . . ? B10 B5 B1 106.2(7) . . ? B6 B5 B4 105.8(7) . . ? B10 B5 B4 57.3(5) . . ? B1 B5 B4 107.9(7) . . ? B6 B5 Sn1 116.6(7) . . ? B10 B5 Sn1 116.3(6) . . ? B1 B5 Sn1 66.2(4) . . ? B4 B5 Sn1 65.7(4) . . ? C312 C313 C314 120.3(9) . . ? C214 C213 C212 120.5(9) . . ? B11 B10 B4 108.6(8) . . ? B11 B10 B9 59.2(6) . . ? B4 B10 B9 60.2(6) . . ? B11 B10 B5 108.8(7) . . ? B4 B10 B5 65.0(6) . . ? B9 B10 B5 111.9(7) . . ? B11 B10 B6 59.6(6) . . ? B4 B10 B6 111.1(7) . . ? B9 B10 B6 107.8(8) . . ? B5 B10 B6 59.6(5) . . ? C424 C425 C426 119.7(10) . . ? C125 C126 C121 118.5(12) . . ? B11 B9 B8 59.8(6) . . ? B11 B9 B3 109.1(7) . . ? B8 B9 B3 59.6(6) . . ? B11 B9 B10 60.1(6) . . ? B8 B9 B10 108.1(7) . . ? B3 B9 B10 111.0(7) . . ? B11 B9 B4 109.1(7) . . ? B8 B9 B4 110.2(7) . . ? B3 B9 B4 63.9(6) . . ? B10 B9 B4 59.9(6) . . ? C425 C424 C423 120.8(10) . . ? B11 B8 B3 109.4(7) . . ? B11 B8 B7 59.8(6) . . ? B3 B8 B7 111.8(7) . . ? B11 B8 B9 59.5(6) . . ? B3 B8 B9 60.3(5) . . ? B7 B8 B9 108.1(8) . . ? B11 B8 B2 108.8(8) . . ? B3 B8 B2 65.7(6) . . ? B7 B8 B2 59.1(6) . . ? B9 B8 B2 112.2(7) . . ? C112 C113 C114 121.7(9) . . ? B1 B6 B7 60.2(6) . . ? B1 B6 B11 109.4(8) . . ? B7 B6 B11 59.5(6) . . ? B1 B6 B5 64.3(6) . . ? B7 B6 B5 110.8(8) . . ? B11 B6 B5 108.7(7) . . ? B1 B6 B10 111.1(7) . . ? B7 B6 B10 107.2(8) . . ? B11 B6 B10 59.3(6) . . ? B5 B6 B10 59.8(6) . . ? C325 C326 C321 121.8(11) . . ? C314 C315 C316 121.9(11) . . ? B2 B7 B11 110.2(7) . . ? B2 B7 B8 60.9(6) . . ? B11 B7 B8 59.7(6) . . ? B2 B7 B6 111.9(7) . . ? B11 B7 B6 60.3(6) . . ? B8 B7 B6 108.8(7) . . ? B2 B7 B1 64.6(6) . . ? B11 B7 B1 109.7(7) . . ? B8 B7 B1 112.1(7) . . ? B6 B7 B1 59.8(6) . . ? C322 C323 C324 122.2(11) . . ? B9 B11 B8 60.8(6) . . ? B9 B11 B7 109.7(7) . . ? B8 B11 B7 60.5(6) . . ? B9 B11 B10 60.7(6) . . ? B8 B11 B10 109.4(7) . . ? B7 B11 B10 109.3(7) . . ? B9 B11 B6 110.3(7) . . ? B8 B11 B6 109.4(7) . . ? B7 B11 B6 60.2(6) . . ? B10 B11 B6 61.1(6) . . ? C225 C224 C223 120.3(11) . . ? C414 C413 C412 120.9(11) . . ? C224 C225 C226 119.8(11) . . ? C125 C124 C123 119.5(11) . . ? C325 C324 C323 117.3(11) . . ? C413 C414 C415 121.2(10) . . ? C124 C123 C122 120.0(12) . . ? C315 C314 C313 119.3(9) . . ? C224 C223 C222 120.1(11) . . ? C326 C325 C324 121.1(12) . . ? C124 C125 C126 121.6(13) . . ? Cl2 C1 Cl1 110.7(6) . . ? Cl6 C3 Cl5 115.2(9) . . ? Cl4 C2 Cl3 114.9(10) . . ? P4 Pt2 P3 91.44(8) . . ? P4 Pt2 S1 93.59(7) . . ? P3 Pt2 S1 174.81(8) . . ? P4 Pt2 S2 172.26(8) . . ? P3 Pt2 S2 93.39(8) . . ? S1 Pt2 S2 81.74(7) . . ? P4 Pt2 Pt1 131.52(6) . . ? P3 Pt2 Pt1 126.62(6) . . ? S1 Pt2 Pt1 48.47(5) . . ? S2 Pt2 Pt1 48.45(5) . . ? P1 Pt1 P2 94.87(9) . . ? P1 Pt1 S1 92.34(8) . . ? P2 Pt1 S1 172.61(8) . . ? P1 Pt1 S2 173.48(8) . . ? P2 Pt1 S2 91.61(8) . . ? S1 Pt1 S2 81.20(7) . . ? P1 Pt1 Pt2 126.16(6) . . ? P2 Pt1 Pt2 127.32(6) . . ? S1 Pt1 Pt2 48.01(5) . . ? S2 Pt1 Pt2 48.21(5) . . ? P1 Pt1 Sn1 124.07(6) . . ? P2 Pt1 Sn1 122.47(6) . . ? S1 Pt1 Sn1 51.32(5) . . ? S2 Pt1 Sn1 52.02(5) . . ? Pt2 Pt1 Sn1 63.653(13) . . ? B2 Sn1 B4 82.6(4) . . ? B2 Sn1 B5 82.3(4) . . ? B4 Sn1 B5 48.5(3) . . ? B2 Sn1 B1 47.8(4) . . ? B4 Sn1 B1 82.6(4) . . ? B5 Sn1 B1 47.8(4) . . ? B2 Sn1 B3 48.8(4) . . ? B4 Sn1 B3 47.6(4) . . ? B5 Sn1 B3 82.6(4) . . ? B1 Sn1 B3 82.8(3) . . ? B2 Sn1 S1 126.9(3) . . ? B4 Sn1 S1 142.1(3) . . ? B5 Sn1 S1 106.5(2) . . ? B1 Sn1 S1 99.9(3) . . ? B3 Sn1 S1 170.0(3) . . ? B2 Sn1 S2 127.3(3) . . ? B4 Sn1 S2 108.6(2) . . ? B5 Sn1 S2 143.7(2) . . ? B1 Sn1 S2 167.9(3) . . ? B3 Sn1 S2 101.1(2) . . ? S1 Sn1 S2 74.36(6) . . ? B2 Sn1 Pt1 108.5(3) . . ? B4 Sn1 Pt1 154.9(2) . . ? B5 Sn1 Pt1 152.7(2) . . ? B1 Sn1 Pt1 121.7(3) . . ? B3 Sn1 Pt1 123.7(3) . . ? S1 Sn1 Pt1 46.79(5) . . ? S2 Sn1 Pt1 46.70(5) . . ? Pt2 S2 Pt1 83.33(6) . . ? Pt2 S2 Sn1 85.76(6) . . ? Pt1 S2 Sn1 81.28(7) . . ? Pt2 S1 Pt1 83.52(6) . . ? Pt2 S1 Sn1 86.59(6) . . ? Pt1 S1 Sn1 81.89(6) . . ? C321 P3 C311 106.1(4) . . ? C321 P3 C331 103.2(4) . . ? C311 P3 C331 106.5(4) . . ? C321 P3 Pt2 114.2(3) . . ? C311 P3 Pt2 111.4(3) . . ? C331 P3 Pt2 114.6(3) . . ? C421 P4 C431 105.2(4) . . ? C421 P4 C411 105.9(4) . . ? C431 P4 C411 106.0(4) . . ? C421 P4 Pt2 113.6(3) . . ? C431 P4 Pt2 115.8(3) . . ? C411 P4 Pt2 109.6(3) . . ? C111 P1 C131 106.2(4) . . ? C111 P1 C121 106.7(4) . . ? C131 P1 C121 103.1(5) . . ? C111 P1 Pt1 112.4(3) . . ? C131 P1 Pt1 115.3(3) . . ? C121 P1 Pt1 112.5(3) . . ? C221 P2 C211 108.3(4) . . ? C221 P2 C231 103.4(4) . . ? C211 P2 C231 102.6(4) . . ? C221 P2 Pt1 111.6(3) . . ? C211 P2 Pt1 115.0(3) . . ? C231 P2 Pt1 114.9(3) . . ? B6 B1 B7 60.0(6) . . ? B6 B1 B2 106.0(7) . . ? B7 B1 B2 57.1(6) . . ? B6 B1 B5 58.2(6) . . ? B7 B1 B5 105.8(7) . . ? B2 B1 B5 108.0(7) . . ? B6 B1 Sn1 117.1(6) . . ? B7 B1 Sn1 115.7(6) . . ? B2 B1 Sn1 65.6(4) . . ? B5 B1 Sn1 66.0(4) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.345 _refine_diff_density_min -1.326 _refine_diff_density_rms 0.152 # Attachment '765679_jd29.cif' data_jd29 _database_code_depnum_ccdc_archive 'CCDC 765679' #TrackingRef '765679_jd29.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C7 H18 N), B11 Ge H11 S, C2 H3 N ' _chemical_formula_sum 'C16 H50 B11 Ge N3 S' _chemical_formula_weight 508.15 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' 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 'p 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.9413(10) _cell_length_b 13.6807(8) _cell_length_c 15.6580(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.098(6) _cell_angle_gamma 90.00 _cell_volume 2985.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28396 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 59.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.130 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 1.106 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7732 _exptl_absorpt_correction_T_max 0.9186 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36751 _diffrn_reflns_av_R_equivalents 0.0872 _diffrn_reflns_av_sigmaI/netI 0.0375 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 5.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5400 _reflns_number_gt 4528 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep3 for windows' _computing_publication_material ? _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. In order to attempt more appropriate values for the thermal ellipsoids and the geometry of the serve disordered cations, the restraints DELU, SIMU ISOR and DFIX were used. The acetonitrile was treated with EADP constraint. ; _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^)+(0.0349P)^2^+6.9014P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5400 _refine_ls_number_parameters 390 _refine_ls_number_restraints 85 _refine_ls_R_factor_all 0.0747 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1299 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.133 _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 N2 N 0.0038(2) 0.4770(2) 0.21945(19) 0.0323(7) Uani 1 1 d D . . C31 C 0.1650(5) 0.6586(6) 0.4612(4) 0.0947(12) Uani 1 1 d . . . H31A H 0.1721 0.5892 0.4675 0.142 Uiso 1 1 calc R . . H31B H 0.1757 0.6766 0.4029 0.142 Uiso 1 1 calc R . . H31C H 0.1014 0.6775 0.4768 0.142 Uiso 1 1 calc R . . C30 C 0.2316(5) 0.7059(6) 0.5142(4) 0.0947(12) Uani 1 1 d . . . N3 N 0.2854(4) 0.7401(5) 0.5599(3) 0.0947(12) Uani 1 1 d . . . C212 C 0.0819(7) 0.4021(9) 0.2106(8) 0.043(2) Uani 0.499(9) 1 d P A 1 H21A H 0.0754 0.3541 0.2557 0.051 Uiso 0.499(9) 1 calc PR A 1 H21B H 0.1433 0.4343 0.2192 0.051 Uiso 0.499(9) 1 calc PR A 1 C222 C -0.0926(6) 0.4416(7) 0.2151(5) 0.034(2) Uani 0.499(9) 1 d P A 1 H22A H -0.1023 0.4070 0.1616 0.041 Uiso 0.499(9) 1 calc PR A 1 H22B H -0.1360 0.4971 0.2149 0.041 Uiso 0.499(9) 1 calc PR A 1 C232 C 0.0189(7) 0.5534(7) 0.1458(5) 0.041(2) Uani 0.499(9) 1 d P A 1 H23A H 0.0867 0.5686 0.1435 0.049 Uiso 0.499(9) 1 calc PR A 1 H23B H 0.0008 0.5227 0.0920 0.049 Uiso 0.499(9) 1 calc PR A 1 C214 C 0.0829(10) 0.3492(11) 0.1259(9) 0.056(3) Uani 0.499(9) 1 d P A 1 H21C H 0.1353 0.3038 0.1256 0.084 Uiso 0.499(9) 1 calc PR A 1 H21D H 0.0904 0.3958 0.0806 0.084 Uiso 0.499(9) 1 calc PR A 1 H21E H 0.0236 0.3146 0.1175 0.084 Uiso 0.499(9) 1 calc PR A 1 C233 C -0.035(3) 0.647(2) 0.153(2) 0.080(10) Uani 0.499(9) 1 d P A 1 H23C H -0.0217 0.6876 0.1048 0.120 Uiso 0.499(9) 1 calc PR A 1 H23D H -0.0159 0.6797 0.2047 0.120 Uiso 0.499(9) 1 calc PR A 1 H23E H -0.1027 0.6332 0.1542 0.120 Uiso 0.499(9) 1 calc PR A 1 C224 C -0.118(4) 0.375(3) 0.287(2) 0.063(10) Uani 0.499(9) 1 d P A 1 H22C H -0.1834 0.3548 0.2800 0.095 Uiso 0.499(9) 1 calc PR A 1 H22D H -0.1099 0.4094 0.3400 0.095 Uiso 0.499(9) 1 calc PR A 1 H22E H -0.0766 0.3192 0.2865 0.095 Uiso 0.499(9) 1 calc PR A 1 C211 C 0.0923(8) 0.4449(10) 0.1774(7) 0.047(3) Uani 0.501(9) 1 d P A 2 H21F H 0.1272 0.4023 0.2166 0.057 Uiso 0.501(9) 1 calc PR A 2 H21G H 0.1320 0.5020 0.1683 0.057 Uiso 0.501(9) 1 calc PR A 2 C221 C -0.0542(8) 0.3813(7) 0.2413(6) 0.048(3) Uani 0.501(9) 1 d PD A 2 H22F H -0.0807 0.3550 0.1884 0.058 Uiso 0.501(9) 1 calc PR A 2 H22G H -0.0093 0.3334 0.2641 0.058 Uiso 0.501(9) 1 calc PR A 2 C231 C -0.0632(7) 0.5372(7) 0.1656(6) 0.048(3) Uani 0.501(9) 1 d PU A 2 H23F H -0.1206 0.5511 0.1975 0.058 Uiso 0.501(9) 1 calc PR A 2 H23G H -0.0821 0.5003 0.1151 0.058 Uiso 0.501(9) 1 calc PR A 2 C213 C 0.0807(12) 0.3911(14) 0.0915(8) 0.073(5) Uani 0.501(9) 1 d P A 2 H21H H 0.1428 0.3743 0.0705 0.109 Uiso 0.501(9) 1 calc PR A 2 H21I H 0.0481 0.4327 0.0510 0.109 Uiso 0.501(9) 1 calc PR A 2 H21J H 0.0438 0.3326 0.0995 0.109 Uiso 0.501(9) 1 calc PR A 2 C234 C -0.018(3) 0.632(2) 0.139(2) 0.086(10) Uani 0.501(9) 1 d PU A 2 H23H H -0.0630 0.6685 0.1047 0.130 Uiso 0.501(9) 1 calc PR A 2 H23I H 0.0380 0.6181 0.1062 0.130 Uiso 0.501(9) 1 calc PR A 2 H23J H 0.0000 0.6687 0.1887 0.130 Uiso 0.501(9) 1 calc PR A 2 C223 C -0.135(4) 0.392(3) 0.303(3) 0.051(6) Uani 0.501(9) 1 d P A 2 H22H H -0.1639 0.3291 0.3120 0.076 Uiso 0.501(9) 1 calc PR A 2 H22I H -0.1815 0.4365 0.2806 0.076 Uiso 0.501(9) 1 calc PR A 2 H22J H -0.1096 0.4160 0.3567 0.076 Uiso 0.501(9) 1 calc PR A 2 C241 C 0.0273(3) 0.5281(3) 0.3020(3) 0.0416(10) Uani 1 1 d . A . H24A H -0.0282 0.5630 0.3209 0.062 Uiso 1 1 calc R . . H24B H 0.0789 0.5732 0.2937 0.062 Uiso 1 1 calc R . . H24C H 0.0460 0.4807 0.3444 0.062 Uiso 1 1 calc R . . N1 N 0.5019(3) 0.4823(3) 0.2462(2) 0.0438(9) Uani 1 1 d DU . . C141 C 0.5861(4) 0.4370(6) 0.2948(4) 0.088(2) Uani 1 1 d U B . H14A H 0.5628 0.3998 0.3421 0.133 Uiso 1 1 calc R . . H14B H 0.6279 0.4878 0.3156 0.133 Uiso 1 1 calc R . . H14C H 0.6207 0.3947 0.2574 0.133 Uiso 1 1 calc R . . C111 C 0.5437(5) 0.5093(6) 0.1568(5) 0.047(2) Uani 0.618(9) 1 d P B 1 H11A H 0.5581 0.4490 0.1271 0.056 Uiso 0.618(9) 1 calc PR B 1 H11B H 0.4940 0.5426 0.1238 0.056 Uiso 0.618(9) 1 calc PR B 1 C121 C 0.4710(6) 0.5722(5) 0.2888(5) 0.047(2) Uani 0.618(9) 1 d P B 1 H12A H 0.4208 0.6024 0.2542 0.057 Uiso 0.618(9) 1 calc PR B 1 H12B H 0.5248 0.6172 0.2913 0.057 Uiso 0.618(9) 1 calc PR B 1 C112 C 0.6324(9) 0.5723(15) 0.1571(13) 0.075(4) Uani 0.618(9) 1 d P B 1 H11C H 0.6514 0.5841 0.0994 0.113 Uiso 0.618(9) 1 calc PR B 1 H11D H 0.6834 0.5395 0.1877 0.113 Uiso 0.618(9) 1 calc PR B 1 H11E H 0.6190 0.6335 0.1845 0.113 Uiso 0.618(9) 1 calc PR B 1 C131 C 0.4321(6) 0.4032(5) 0.2333(6) 0.045(2) Uani 0.618(9) 1 d P B 1 H13A H 0.4651 0.3474 0.2096 0.054 Uiso 0.618(9) 1 calc PR B 1 H13B H 0.4084 0.3838 0.2887 0.054 Uiso 0.618(9) 1 calc PR B 1 C132 C 0.3516(10) 0.4260(11) 0.1788(8) 0.064(3) Uani 0.618(9) 1 d P B 1 H13C H 0.3102 0.3701 0.1743 0.096 Uiso 0.618(9) 1 calc PR B 1 H13D H 0.3737 0.4433 0.1231 0.096 Uiso 0.618(9) 1 calc PR B 1 H13E H 0.3168 0.4799 0.2024 0.096 Uiso 0.618(9) 1 calc PR B 1 C124 C 0.4351(19) 0.559(2) 0.3763(18) 0.053(5) Uani 0.618(9) 1 d P B 1 H12C H 0.4169 0.6210 0.3992 0.079 Uiso 0.618(9) 1 calc PR B 1 H12D H 0.4847 0.5305 0.4118 0.079 Uiso 0.618(9) 1 calc PR B 1 H12E H 0.3804 0.5161 0.3746 0.079 Uiso 0.618(9) 1 calc PR B 1 C113 C 0.5127(12) 0.5808(12) 0.2102(10) 0.072(5) Uani 0.382(9) 1 d P B 2 H11F H 0.5336 0.6256 0.2548 0.086 Uiso 0.382(9) 1 calc PR B 2 H11G H 0.4512 0.6034 0.1878 0.086 Uiso 0.382(9) 1 calc PR B 2 C114 C 0.585(2) 0.580(3) 0.139(2) 0.113(11) Uani 0.382(9) 1 d P B 2 H11H H 0.5907 0.6451 0.1162 0.170 Uiso 0.382(9) 1 calc PR B 2 H11I H 0.5642 0.5363 0.0951 0.170 Uiso 0.382(9) 1 calc PR B 2 H11J H 0.6463 0.5597 0.1618 0.170 Uiso 0.382(9) 1 calc PR B 2 C123 C 0.4191(9) 0.4939(10) 0.3120(8) 0.056(4) Uani 0.382(9) 1 d PDU B 2 H12F H 0.3657 0.5265 0.2834 0.067 Uiso 0.382(9) 1 calc PR B 2 H12G H 0.3975 0.4292 0.3279 0.067 Uiso 0.382(9) 1 calc PR B 2 C134 C 0.370(2) 0.421(3) 0.1352(17) 0.119(13) Uani 0.382(9) 1 d PD B 2 H13F H 0.3584 0.3650 0.0996 0.179 Uiso 0.382(9) 1 calc PR B 2 H13G H 0.3699 0.4789 0.1005 0.179 Uiso 0.382(9) 1 calc PR B 2 H13H H 0.3202 0.4259 0.1766 0.179 Uiso 0.382(9) 1 calc PR B 2 C133 C 0.4633(17) 0.4109(19) 0.1793(17) 0.131(10) Uani 0.382(9) 1 d PD B 2 H13I H 0.5109 0.4080 0.1350 0.157 Uiso 0.382(9) 1 calc PR B 2 H13J H 0.4631 0.3471 0.2063 0.157 Uiso 0.382(9) 1 calc PR B 2 C122 C 0.443(4) 0.551(4) 0.394(4) 0.080(13) Uani 0.382(9) 1 d PU B 2 H12H H 0.3881 0.5526 0.4295 0.120 Uiso 0.382(9) 1 calc PR B 2 H12I H 0.4624 0.6159 0.3798 0.120 Uiso 0.382(9) 1 calc PR B 2 H12J H 0.4951 0.5184 0.4242 0.120 Uiso 0.382(9) 1 calc PR B 2 Ge1 Ge 0.26004(3) 0.73212(3) 0.11030(2) 0.02974(14) Uani 1 1 d . . . S1 S 0.24168(10) 0.68443(9) 0.23652(7) 0.0492(3) Uani 1 1 d . . . B108 B 0.2809(4) 0.7028(4) -0.0949(3) 0.0408(11) Uani 1 1 d . . . H108 H 0.2808 0.6487 -0.1468 0.049 Uiso 1 1 calc R . . B107 B 0.3880(3) 0.7622(4) -0.0602(3) 0.0443(12) Uani 1 1 d . . . H107 H 0.4573 0.7469 -0.0899 0.053 Uiso 1 1 calc R . . B109 B 0.1844(3) 0.7857(3) -0.0823(3) 0.0355(10) Uani 1 1 d . . . H109 H 0.1218 0.7855 -0.1261 0.043 Uiso 1 1 calc R . . B105 B 0.1691(3) 0.8136(3) 0.0271(3) 0.0329(9) Uani 1 1 d . . . H105 H 0.0982 0.8315 0.0524 0.040 Uiso 1 1 calc R . . B110 B 0.2319(4) 0.8965(4) -0.0380(3) 0.0400(11) Uani 1 1 d . . . H110 H 0.2001 0.9682 -0.0529 0.048 Uiso 1 1 calc R . . B106 B 0.3579(4) 0.8814(4) -0.0245(3) 0.0404(11) Uani 1 1 d . . . H106 H 0.4079 0.9431 -0.0309 0.048 Uiso 1 1 calc R . . B101 B 0.2820(3) 0.8755(3) 0.0646(3) 0.0323(9) Uani 1 1 d . . . H101 H 0.2828 0.9327 0.1139 0.039 Uiso 1 1 calc R . . B104 B 0.2015(3) 0.6875(3) -0.0097(3) 0.0323(9) Uani 1 1 d . . . H104 H 0.1513 0.6255 -0.0074 0.039 Uiso 1 1 calc R . . B111 B 0.2970(4) 0.8296(4) -0.1146(3) 0.0435(12) Uani 1 1 d . . . H111 H 0.3072 0.8580 -0.1795 0.052 Uiso 1 1 calc R . . B103 B 0.3340(3) 0.6723(4) 0.0049(3) 0.0377(11) Uani 1 1 d . . . H103 H 0.3678 0.6007 0.0165 0.045 Uiso 1 1 calc R . . B102 B 0.3838(3) 0.7883(4) 0.0508(3) 0.0372(11) Uani 1 1 d . . . H102 H 0.4491 0.7900 0.0914 0.045 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 N2 0.0348(17) 0.0394(19) 0.0225(15) -0.0022(13) -0.0034(13) 0.0061(14) C31 0.089(3) 0.131(3) 0.064(2) -0.010(2) 0.0032(18) -0.043(2) C30 0.089(3) 0.131(3) 0.064(2) -0.010(2) 0.0032(18) -0.043(2) N3 0.089(3) 0.131(3) 0.064(2) -0.010(2) 0.0032(18) -0.043(2) C212 0.032(5) 0.050(7) 0.047(6) 0.004(5) 0.007(4) 0.010(5) C222 0.030(4) 0.040(5) 0.032(4) 0.003(4) -0.003(3) -0.004(4) C232 0.051(6) 0.043(5) 0.028(4) 0.010(4) 0.001(4) -0.002(4) C214 0.053(7) 0.066(9) 0.050(8) -0.022(6) -0.001(7) 0.012(6) C233 0.11(3) 0.044(8) 0.080(12) 0.004(8) -0.015(15) 0.006(11) C224 0.07(2) 0.09(2) 0.032(14) 0.004(12) -0.006(12) -0.030(14) C211 0.041(6) 0.063(8) 0.038(6) -0.009(5) 0.004(5) 0.008(5) C221 0.057(6) 0.048(6) 0.038(5) -0.002(4) -0.003(5) -0.010(5) C231 0.043(6) 0.067(6) 0.036(5) 0.010(4) 0.003(4) 0.015(4) C213 0.072(9) 0.113(15) 0.033(7) -0.025(7) 0.005(6) 0.019(9) C234 0.055(9) 0.099(19) 0.10(2) 0.074(17) -0.002(11) 0.006(12) C223 0.055(12) 0.063(11) 0.034(14) 0.003(9) 0.002(9) -0.020(8) C241 0.043(2) 0.051(3) 0.031(2) -0.0068(19) -0.0008(18) -0.002(2) N1 0.047(2) 0.045(2) 0.039(2) -0.0045(16) -0.0022(16) -0.0030(17) C141 0.060(4) 0.124(6) 0.081(4) -0.014(4) -0.004(3) 0.028(4) C111 0.045(4) 0.056(5) 0.040(4) 0.004(4) 0.011(3) -0.012(4) C121 0.046(4) 0.041(4) 0.056(5) -0.005(3) 0.012(4) -0.006(3) C112 0.052(7) 0.090(9) 0.084(8) -0.014(6) 0.016(7) -0.026(8) C131 0.052(5) 0.038(4) 0.044(4) 0.004(3) 0.004(4) -0.009(3) C132 0.063(6) 0.053(6) 0.075(8) 0.005(6) -0.028(6) -0.020(4) C124 0.058(7) 0.051(7) 0.050(14) -0.003(8) 0.011(7) -0.013(6) C113 0.073(10) 0.067(10) 0.077(11) -0.009(8) 0.022(8) -0.026(8) C114 0.11(2) 0.111(19) 0.12(3) 0.005(18) 0.06(2) -0.03(2) C123 0.064(9) 0.049(8) 0.056(8) 0.005(6) 0.011(6) 0.013(6) C134 0.14(3) 0.115(19) 0.10(2) 0.000(18) -0.08(2) -0.026(18) C133 0.15(2) 0.14(2) 0.100(17) -0.054(16) 0.033(17) -0.073(18) C122 0.11(3) 0.09(2) 0.038(14) -0.003(13) 0.030(14) -0.005(16) Ge1 0.0341(2) 0.0303(2) 0.0248(2) -0.00103(17) 0.00023(14) -0.00080(18) S1 0.0669(8) 0.0514(7) 0.0294(5) 0.0062(5) 0.0017(5) -0.0081(6) B108 0.040(3) 0.051(3) 0.031(2) -0.009(2) 0.000(2) -0.004(2) B107 0.033(2) 0.064(3) 0.036(2) -0.013(2) 0.0074(19) -0.007(2) B109 0.038(2) 0.035(3) 0.033(2) 0.0030(18) -0.0098(19) -0.0057(19) B105 0.026(2) 0.032(2) 0.040(2) -0.0001(19) -0.0036(18) 0.0006(18) B110 0.044(3) 0.037(3) 0.039(3) 0.005(2) -0.006(2) -0.006(2) B106 0.041(3) 0.050(3) 0.031(2) -0.004(2) 0.006(2) -0.017(2) B101 0.033(2) 0.032(2) 0.032(2) -0.0058(18) 0.0032(18) -0.0064(18) B104 0.035(2) 0.030(2) 0.032(2) -0.0040(18) -0.0029(19) -0.0022(19) B111 0.050(3) 0.054(3) 0.026(2) 0.000(2) 0.000(2) -0.016(2) B103 0.034(2) 0.042(3) 0.037(2) -0.011(2) -0.003(2) 0.010(2) B102 0.030(2) 0.049(3) 0.033(2) -0.009(2) 0.0006(18) -0.004(2) _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 N2 C222 1.429(8) . ? N2 C211 1.477(11) . ? N2 C231 1.494(9) . ? N2 C241 1.500(5) . ? N2 C212 1.503(10) . ? N2 C232 1.573(9) . ? N2 C221 1.581(9) . ? C31 C30 1.392(8) . ? C30 N3 1.128(8) . ? C212 C214 1.511(17) . ? C222 C224 1.49(4) . ? C232 C233 1.49(4) . ? C211 C213 1.539(18) . ? C221 C223 1.50(4) . ? C231 C234 1.50(3) . ? N1 C131 1.466(8) . ? N1 C121 1.468(8) . ? N1 C113 1.470(16) . ? N1 C141 1.519(7) . ? N1 C133 1.52(2) . ? N1 C123 1.570(10) . ? N1 C111 1.571(8) . ? C111 C112 1.507(16) . ? C121 C124 1.48(3) . ? C131 C132 1.432(14) . ? C113 C114 1.51(3) . ? C123 C122 1.53(5) . ? C134 C133 1.469(19) . ? Ge1 S1 2.1015(11) . ? Ge1 B101 2.113(5) . ? Ge1 B105 2.118(4) . ? Ge1 B102 2.120(5) . ? Ge1 B104 2.124(4) . ? Ge1 B103 2.126(5) . ? B108 B104 1.762(7) . ? B108 B103 1.766(7) . ? B108 B109 1.773(7) . ? B108 B107 1.776(7) . ? B108 B111 1.777(7) . ? B107 B111 1.773(8) . ? B107 B103 1.775(7) . ? B107 B106 1.777(8) . ? B107 B102 1.778(6) . ? B109 B111 1.764(7) . ? B109 B105 1.772(6) . ? B109 B104 1.773(6) . ? B109 B110 1.789(6) . ? B105 B110 1.767(7) . ? B105 B101 1.872(6) . ? B105 B104 1.876(6) . ? B110 B101 1.763(6) . ? B110 B111 1.772(7) . ? B110 B106 1.777(7) . ? B106 B101 1.769(6) . ? B106 B102 1.769(7) . ? B106 B111 1.780(7) . ? B101 B102 1.869(7) . ? B104 B103 1.869(6) . ? B103 B102 1.871(7) . ? 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 C222 N2 C211 132.2(6) . . ? C222 N2 C231 65.3(5) . . ? C211 N2 C231 115.6(6) . . ? C222 N2 C241 112.8(4) . . ? C211 N2 C241 110.7(5) . . ? C231 N2 C241 110.7(5) . . ? C222 N2 C212 116.5(6) . . ? C211 N2 C212 31.0(5) . . ? C231 N2 C212 140.3(6) . . ? C241 N2 C212 104.5(5) . . ? C222 N2 C232 109.2(5) . . ? C211 N2 C232 75.3(7) . . ? C231 N2 C232 46.5(5) . . ? C241 N2 C232 107.0(4) . . ? C212 N2 C232 106.1(6) . . ? C222 N2 C221 40.9(5) . . ? C211 N2 C221 106.6(7) . . ? C231 N2 C221 105.2(6) . . ? C241 N2 C221 107.6(4) . . ? C212 N2 C221 80.2(6) . . ? C232 N2 C221 141.7(5) . . ? N3 C30 C31 176.4(9) . . ? N2 C212 C214 115.2(9) . . ? N2 C222 C224 114(2) . . ? C233 C232 N2 116.1(16) . . ? N2 C211 C213 117.2(10) . . ? C223 C221 N2 116.9(18) . . ? N2 C231 C234 111.7(16) . . ? C131 N1 C121 118.8(5) . . ? C131 N1 C113 134.1(8) . . ? C121 N1 C113 55.9(7) . . ? C131 N1 C141 105.8(5) . . ? C121 N1 C141 110.1(5) . . ? C113 N1 C141 118.9(8) . . ? C131 N1 C133 37.6(10) . . ? C121 N1 C133 138.4(11) . . ? C113 N1 C133 111.2(13) . . ? C141 N1 C133 110.1(11) . . ? C131 N1 C123 70.8(7) . . ? C121 N1 C123 52.5(6) . . ? C113 N1 C123 103.9(8) . . ? C141 N1 C123 106.4(6) . . ? C133 N1 C123 105.2(11) . . ? C131 N1 C111 108.0(5) . . ? C121 N1 C111 108.9(5) . . ? C113 N1 C111 53.1(7) . . ? C141 N1 C111 104.2(5) . . ? C133 N1 C111 70.7(11) . . ? C123 N1 C111 148.3(6) . . ? C112 C111 N1 116.8(9) . . ? N1 C121 C124 115.1(12) . . ? C132 C131 N1 115.6(7) . . ? N1 C113 C114 110.6(18) . . ? C122 C123 N1 117(2) . . ? C134 C133 N1 124(2) . . ? S1 Ge1 B101 128.91(13) . . ? S1 Ge1 B105 131.30(14) . . ? B101 Ge1 B105 52.52(17) . . ? S1 Ge1 B102 129.81(13) . . ? B101 Ge1 B102 52.40(18) . . ? B105 Ge1 B102 91.21(18) . . ? S1 Ge1 B104 133.71(13) . . ? B101 Ge1 B104 91.31(17) . . ? B105 Ge1 B104 52.51(18) . . ? B102 Ge1 B104 91.04(17) . . ? S1 Ge1 B103 132.85(14) . . ? B101 Ge1 B103 91.08(19) . . ? B105 Ge1 B103 91.05(18) . . ? B102 Ge1 B103 52.28(18) . . ? B104 Ge1 B103 52.17(17) . . ? B104 B108 B103 63.9(3) . . ? B104 B108 B109 60.2(3) . . ? B103 B108 B109 111.0(3) . . ? B104 B108 B107 111.1(3) . . ? B103 B108 B107 60.1(3) . . ? B109 B108 B107 108.0(4) . . ? B104 B108 B111 109.3(3) . . ? B103 B108 B111 109.4(3) . . ? B109 B108 B111 59.6(3) . . ? B107 B108 B111 59.9(3) . . ? B111 B107 B103 109.2(3) . . ? B111 B107 B108 60.1(3) . . ? B103 B107 B108 59.7(3) . . ? B111 B107 B106 60.2(3) . . ? B103 B107 B106 110.5(3) . . ? B108 B107 B106 108.3(4) . . ? B111 B107 B102 109.2(4) . . ? B103 B107 B102 63.6(3) . . ? B108 B107 B102 110.3(3) . . ? B106 B107 B102 59.7(3) . . ? B111 B109 B105 109.1(3) . . ? B111 B109 B108 60.3(3) . . ? B105 B109 B108 110.5(3) . . ? B111 B109 B104 109.4(3) . . ? B105 B109 B104 63.9(3) . . ? B108 B109 B104 59.6(3) . . ? B111 B109 B110 59.8(3) . . ? B105 B109 B110 59.5(3) . . ? B108 B109 B110 108.0(3) . . ? B104 B109 B110 110.4(3) . . ? B110 B105 B109 60.7(3) . . ? B110 B105 B101 57.9(2) . . ? B109 B105 B101 106.6(3) . . ? B110 B105 B104 106.8(3) . . ? B109 B105 B104 58.1(2) . . ? B101 B105 B104 107.9(3) . . ? B110 B105 Ge1 113.3(3) . . ? B109 B105 Ge1 113.6(3) . . ? B101 B105 Ge1 63.61(19) . . ? B104 B105 Ge1 63.91(19) . . ? B101 B110 B105 64.0(3) . . ? B101 B110 B111 109.5(4) . . ? B105 B110 B111 108.9(3) . . ? B101 B110 B106 59.9(3) . . ? B105 B110 B106 110.9(3) . . ? B111 B110 B106 60.2(3) . . ? B101 B110 B109 110.7(3) . . ? B105 B110 B109 59.8(3) . . ? B111 B110 B109 59.4(3) . . ? B106 B110 B109 107.8(4) . . ? B101 B106 B102 63.8(3) . . ? B101 B106 B107 110.8(3) . . ? B102 B106 B107 60.2(3) . . ? B101 B106 B110 59.6(3) . . ? B102 B106 B110 110.6(3) . . ? B107 B106 B110 107.9(3) . . ? B101 B106 B111 108.9(3) . . ? B102 B106 B111 109.3(4) . . ? B107 B106 B111 59.8(3) . . ? B110 B106 B111 59.8(3) . . ? B110 B101 B106 60.4(3) . . ? B110 B101 B102 106.7(3) . . ? B106 B101 B102 58.1(3) . . ? B110 B101 B105 58.1(3) . . ? B106 B101 B105 106.6(3) . . ? B102 B101 B105 108.1(3) . . ? B110 B101 Ge1 113.7(3) . . ? B106 B101 Ge1 113.7(3) . . ? B102 B101 Ge1 64.0(2) . . ? B105 B101 Ge1 63.87(19) . . ? B108 B104 B109 60.2(3) . . ? B108 B104 B103 58.1(3) . . ? B109 B104 B103 106.4(3) . . ? B108 B104 B105 106.3(3) . . ? B109 B104 B105 58.0(2) . . ? B103 B104 B105 107.9(3) . . ? B108 B104 Ge1 113.5(3) . . ? B109 B104 Ge1 113.2(3) . . ? B103 B104 Ge1 63.98(19) . . ? B105 B104 Ge1 63.57(19) . . ? B109 B111 B110 60.8(3) . . ? B109 B111 B107 108.5(3) . . ? B110 B111 B107 108.3(3) . . ? B109 B111 B108 60.1(3) . . ? B110 B111 B108 108.5(3) . . ? B107 B111 B108 60.0(3) . . ? B109 B111 B106 108.8(3) . . ? B110 B111 B106 60.1(3) . . ? B107 B111 B106 60.0(3) . . ? B108 B111 B106 108.1(4) . . ? B108 B103 B107 60.2(3) . . ? B108 B103 B104 57.9(3) . . ? B107 B103 B104 106.4(3) . . ? B108 B103 B102 106.6(3) . . ? B107 B103 B102 58.3(3) . . ? B104 B103 B102 108.1(3) . . ? B108 B103 Ge1 113.2(3) . . ? B107 B103 Ge1 113.4(3) . . ? B104 B103 Ge1 63.85(19) . . ? B102 B103 Ge1 63.7(2) . . ? B106 B102 B107 60.1(3) . . ? B106 B102 B101 58.1(3) . . ? B107 B102 B101 106.3(3) . . ? B106 B102 B103 106.6(3) . . ? B107 B102 B103 58.2(3) . . ? B101 B102 B103 108.0(3) . . ? B106 B102 Ge1 113.4(3) . . ? B107 B102 Ge1 113.5(3) . . ? B101 B102 Ge1 63.60(19) . . ? B103 B102 Ge1 64.0(2) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.375 _refine_diff_density_min -1.532 _refine_diff_density_rms 0.066 # Attachment '765680_jd34.cif' data_jd34 _database_code_depnum_ccdc_archive 'CCDC 765680' #TrackingRef '765680_jd34.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B22 Ge2 P2 Pt S2, 2(C7 H18 N), 2(C2 H3 N)' _chemical_formula_sum 'C45 H90 B22 Ge2 N4 P2 Pt S2' _chemical_formula_weight 1391.36 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' Pt Pt -1.7033 8.3905 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1599(9) _cell_length_b 12.6755(8) _cell_length_c 24.7185(16) _cell_angle_alpha 76.675(5) _cell_angle_beta 82.331(6) _cell_angle_gamma 63.982(5) _cell_volume 3329.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 36216 _cell_measurement_theta_min 3.15 _cell_measurement_theta_max 54.44 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.388 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1404 _exptl_absorpt_coefficient_mu 3.138 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5684 _exptl_absorpt_correction_T_max 0.7019 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37886 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0423 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 5.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11883 _reflns_number_gt 10898 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep for windows' _computing_publication_material ? _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. In order to attempt more appropriate values for the thermal ellipsoids and the geometry of the serve disordered cations, the restraints DELU, SIMU ISOR and DFIX were used. The phenylring C201-C206 was treated with EADP constraint. ; _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^)+(0.0009P)^2^+9.8592P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11883 _refine_ls_number_parameters 813 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0715 _refine_ls_wR_factor_gt 0.0690 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.136 _refine_ls_shift/su_max 0.005 _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 Pt1 Pt 0.611179(14) 0.931079(14) 0.742393(6) 0.02073(5) Uani 1 1 d . . . Ge2 Ge 0.33816(4) 1.19596(4) 0.701347(17) 0.02415(10) Uani 1 1 d . . . Ge1 Ge 0.63830(5) 1.15594(4) 0.793639(18) 0.03203(11) Uani 1 1 d . . . S1 S 0.65142(10) 1.10297(9) 0.71592(4) 0.0264(2) Uani 1 1 d . . . S2 S 0.40608(9) 1.04791(9) 0.76981(4) 0.0288(2) Uani 1 1 d . . . P2 P 0.56258(10) 0.77319(9) 0.76760(4) 0.0260(2) Uani 1 1 d . . . P1 P 0.79978(10) 0.82275(10) 0.70805(4) 0.0261(2) Uani 1 1 d . . . B205 B 0.3338(5) 1.3685(5) 0.6768(2) 0.0317(11) Uani 1 1 d . . . H205 H 0.3923 1.3876 0.6998 0.038 Uiso 1 1 calc R . . B201 B 0.1861(5) 1.3606(4) 0.7071(2) 0.0292(10) Uani 1 1 d . . . H201 H 0.1513 1.3747 0.7495 0.035 Uiso 1 1 calc R . . C201 C 0.7890(5) 0.8365(5) 0.6338(2) 0.0515(6) Uani 1 1 d . . . C3 C 0.6892(4) 0.6270(4) 0.78646(19) 0.0342(10) Uani 1 1 d . . . H3A H 0.7231 0.6243 0.8204 0.041 Uiso 1 1 calc R . . H3B H 0.6578 0.5665 0.7942 0.041 Uiso 1 1 calc R . . C302 C 0.4549(4) 0.8401(4) 0.66529(19) 0.0348(10) Uani 1 1 d . . . H302 H 0.4720 0.9065 0.6600 0.042 Uiso 1 1 calc R . . C301 C 0.4852(4) 0.7561(4) 0.71456(18) 0.0286(9) Uani 1 1 d . . . C1 C 0.8716(4) 0.6628(4) 0.73775(18) 0.0326(10) Uani 1 1 d . . . H1A H 0.9450 0.6256 0.7155 0.039 Uiso 1 1 calc R . . H1B H 0.8968 0.6531 0.7749 0.039 Uiso 1 1 calc R . . C2 C 0.7924(4) 0.5959(4) 0.74148(19) 0.0342(10) Uani 1 1 d . . . H2A H 0.8437 0.5106 0.7495 0.041 Uiso 1 1 calc R . . H2B H 0.7567 0.6148 0.7057 0.041 Uiso 1 1 calc R . . C202 C 0.6986(5) 0.9382(5) 0.6051(2) 0.0515(6) Uani 1 1 d . . . H202 H 0.6462 0.9984 0.6240 0.062 Uiso 1 1 calc R . . C306 C 0.4593(5) 0.6558(4) 0.7215(2) 0.0391(11) Uani 1 1 d . . . H306 H 0.4799 0.5982 0.7540 0.047 Uiso 1 1 calc R . . B206 B 0.0868(4) 1.4125(5) 0.6515(2) 0.0310(11) Uani 1 1 d . . . H206 H -0.0124 1.4599 0.6593 0.037 Uiso 1 1 calc R . . B202 B 0.1589(5) 1.2560(5) 0.6732(2) 0.0315(11) Uani 1 1 d . . . H20A H 0.1072 1.2043 0.6942 0.038 Uiso 1 1 calc R . . C303 C 0.3995(5) 0.8253(5) 0.6241(2) 0.0467(12) Uani 1 1 d . . . H303 H 0.3797 0.8818 0.5912 0.056 Uiso 1 1 calc R . . B210 B 0.1885(5) 1.4789(4) 0.6537(2) 0.0313(11) Uani 1 1 d . . . H210 H 0.1551 1.5691 0.6628 0.038 Uiso 1 1 calc R . . C203 C 0.6845(5) 0.9522(5) 0.5489(2) 0.0515(6) Uani 1 1 d . . . H203 H 0.6237 1.0216 0.5303 0.062 Uiso 1 1 calc R . . B211 B 0.1611(5) 1.4553(5) 0.5892(2) 0.0349(12) Uani 1 1 d . . . H211 H 0.1099 1.5308 0.5566 0.042 Uiso 1 1 calc R . . C401 C 0.4658(4) 0.7854(4) 0.83044(17) 0.0280(9) Uani 1 1 d . . . C101 C 0.9197(4) 0.8670(4) 0.7152(2) 0.0380(11) Uani 1 1 d . . . C406 C 0.5082(5) 0.8002(5) 0.8761(2) 0.0433(12) Uani 1 1 d . . . H406 H 0.5845 0.8016 0.8740 0.052 Uiso 1 1 calc R . . B203 B 0.2894(5) 1.1981(5) 0.6219(2) 0.0346(12) Uani 1 1 d . . . H20B H 0.3195 1.1101 0.6108 0.042 Uiso 1 1 calc R . . B207 B 0.1473(5) 1.3182(5) 0.6011(2) 0.0354(12) Uani 1 1 d . . . H207 H 0.0875 1.3048 0.5762 0.043 Uiso 1 1 calc R . . C404 C 0.3252(5) 0.8118(6) 0.9291(2) 0.0535(15) Uani 1 1 d . . . H404 H 0.2781 0.8211 0.9620 0.064 Uiso 1 1 calc R . . C402 C 0.3514(5) 0.7841(5) 0.8345(2) 0.0432(12) Uani 1 1 d . . . H402 H 0.3214 0.7747 0.8041 0.052 Uiso 1 1 calc R . . B204 B 0.3972(5) 1.2672(5) 0.6235(2) 0.0352(12) Uani 1 1 d . . . H204 H 0.4955 1.2224 0.6129 0.042 Uiso 1 1 calc R . . B208 B 0.2867(5) 1.3254(5) 0.5723(2) 0.0376(12) Uani 1 1 d . . . H208 H 0.3170 1.3168 0.5290 0.045 Uiso 1 1 calc R . . C304 C 0.3731(5) 0.7265(5) 0.6316(3) 0.0528(14) Uani 1 1 d . . . H304 H 0.3352 0.7171 0.6039 0.063 Uiso 1 1 calc R . . C305 C 0.4033(5) 0.6432(5) 0.6800(3) 0.0522(14) Uani 1 1 d . . . H305 H 0.3858 0.5771 0.6849 0.063 Uiso 1 1 calc R . . C405 C 0.4374(5) 0.8130(6) 0.9252(2) 0.0525(14) Uani 1 1 d . . . H405 H 0.4669 0.8224 0.9557 0.063 Uiso 1 1 calc R . . B209 B 0.3121(5) 1.4249(5) 0.6050(2) 0.0376(12) Uani 1 1 d . . . H209 H 0.3589 1.4805 0.5827 0.045 Uiso 1 1 calc R . . C403 C 0.2815(5) 0.7967(6) 0.8840(2) 0.0544(15) Uani 1 1 d . . . H403 H 0.2053 0.7950 0.8867 0.065 Uiso 1 1 calc R . . B101 B 0.6331(5) 1.3216(5) 0.7992(2) 0.0373(12) Uani 1 1 d . . . H101 H 0.6317 1.3831 0.7595 0.045 Uiso 1 1 calc R . . B105 B 0.4959(6) 1.2928(5) 0.8289(2) 0.0443(14) Uani 1 1 d . . . H105 H 0.4083 1.3364 0.8079 0.053 Uiso 1 1 calc R . . B110 B 0.5503(7) 1.3739(5) 0.8592(3) 0.0513(16) Uani 1 1 d . . . H110 H 0.4955 1.4706 0.8569 0.062 Uiso 1 1 calc R . . B103 B 0.7274(8) 1.0700(5) 0.8694(2) 0.0577(19) Uani 1 1 d . . . H103 H 0.7858 0.9735 0.8737 0.069 Uiso 1 1 calc R . . B102 B 0.7745(7) 1.1843(5) 0.8240(3) 0.0481(15) Uani 1 1 d . . . H102 H 0.8620 1.1597 0.7998 0.058 Uiso 1 1 calc R . . B109 B 0.5035(9) 1.2647(7) 0.9027(3) 0.064(2) Uani 1 1 d . . . H109 H 0.4183 1.2909 0.9284 0.077 Uiso 1 1 calc R . . B106 B 0.7133(7) 1.3100(6) 0.8566(3) 0.0567(18) Uani 1 1 d . . . H106 H 0.7643 1.3649 0.8528 0.068 Uiso 1 1 calc R . . B104 B 0.5531(8) 1.1346(6) 0.8736(3) 0.060(2) Uani 1 1 d . . . H104 H 0.5019 1.0792 0.8808 0.072 Uiso 1 1 calc R . . B107 B 0.7661(9) 1.1636(6) 0.8976(3) 0.071(3) Uani 1 1 d . . . H107 H 0.8510 1.1243 0.9206 0.086 Uiso 1 1 calc R . . B108 B 0.6378(10) 1.1355(6) 0.9254(3) 0.073(3) Uani 1 1 d . . . H108 H 0.6399 1.0774 0.9663 0.087 Uiso 1 1 calc R . . B111 B 0.6310(8) 1.2803(6) 0.9189(3) 0.064(2) Uani 1 1 d . . . H111 H 0.6277 1.3171 0.9556 0.077 Uiso 1 1 calc R . . C41 C 0.1982(7) 0.5860(7) 0.8003(5) 0.091(3) Uani 1 1 d . . . H41A H 0.1854 0.6616 0.7766 0.136 Uiso 1 1 calc R . . H41B H 0.1676 0.5441 0.7831 0.136 Uiso 1 1 calc R . . H41C H 0.2841 0.5393 0.8061 0.136 Uiso 1 1 calc R . . C40 C 0.1349(10) 0.6055(9) 0.8524(7) 0.124(5) Uani 1 1 d . . . N4 N 0.0892(14) 0.6202(12) 0.8944(7) 0.220(8) Uani 1 1 d . . . N5 N 0.8164(15) 0.5306(14) 0.9199(8) 0.196(8) Uani 1 1 d . . . C50 C 0.732(2) 0.5138(13) 0.9599(11) 0.171(10) Uani 1 1 d . . . C51 C 0.651(3) 0.5090(16) 1.0018(9) 0.258(14) Uani 1 1 d . . . H51A H 0.6146 0.5834 1.0146 0.387 Uiso 1 1 calc R . . H51B H 0.6922 0.4451 1.0318 0.387 Uiso 1 1 calc R . . H51C H 0.5887 0.4948 0.9889 0.387 Uiso 1 1 calc R . . N2 N 0.1986(12) 0.6942(12) 0.4149(5) 0.059(3) Uani 0.591(9) 1 d P A 1 C222 C 0.0753(17) 0.8819(13) 0.4578(8) 0.107(5) Uani 0.591(9) 1 d P A 1 H22A H 0.0155 0.9109 0.4867 0.160 Uiso 0.591(9) 1 calc PR A 1 H22B H 0.0434 0.9284 0.4223 0.160 Uiso 0.591(9) 1 calc PR A 1 H22C H 0.1485 0.8886 0.4632 0.160 Uiso 0.591(9) 1 calc PR A 1 C221 C 0.1049(13) 0.7507(13) 0.4598(6) 0.066(4) Uani 0.591(9) 1 d P A 1 H22D H 0.0296 0.7447 0.4559 0.079 Uiso 0.591(9) 1 calc PR A 1 H22E H 0.1360 0.7049 0.4961 0.079 Uiso 0.591(9) 1 calc PR A 1 C211 C 0.3140(9) 0.7099(12) 0.4168(4) 0.068(4) Uani 0.591(9) 1 d P A 1 H21A H 0.3733 0.6706 0.3893 0.081 Uiso 0.591(9) 1 calc PR A 1 H21B H 0.2953 0.7945 0.4070 0.081 Uiso 0.591(9) 1 calc PR A 1 C212 C 0.3698(10) 0.6599(17) 0.4729(5) 0.099(6) Uani 0.591(9) 1 d P A 1 H21C H 0.4431 0.6714 0.4717 0.149 Uiso 0.591(9) 1 calc PR A 1 H21D H 0.3894 0.5760 0.4827 0.149 Uiso 0.591(9) 1 calc PR A 1 H21E H 0.3126 0.7004 0.5001 0.149 Uiso 0.591(9) 1 calc PR A 1 C231 C 0.2194(19) 0.5642(16) 0.4271(8) 0.065(5) Uani 0.591(9) 1 d P A 1 H23A H 0.2414 0.5316 0.4656 0.078 Uiso 0.591(9) 1 calc PR A 1 H23B H 0.1419 0.5621 0.4235 0.078 Uiso 0.591(9) 1 calc PR A 1 C232 C 0.3119(16) 0.4840(16) 0.3930(7) 0.105(6) Uani 0.591(9) 1 d P A 1 H23C H 0.3145 0.4053 0.4045 0.158 Uiso 0.591(9) 1 calc PR A 1 H23D H 0.3907 0.4806 0.3975 0.158 Uiso 0.591(9) 1 calc PR A 1 H23E H 0.2913 0.5135 0.3546 0.158 Uiso 0.591(9) 1 calc PR A 1 C241 C 0.1466(13) 0.7549(14) 0.3560(6) 0.069(4) Uani 0.591(9) 1 d P A 1 H24A H 0.0724 0.7469 0.3538 0.104 Uiso 0.591(9) 1 calc PR A 1 H24B H 0.2056 0.7171 0.3286 0.104 Uiso 0.591(9) 1 calc PR A 1 H24C H 0.1295 0.8382 0.3491 0.104 Uiso 0.591(9) 1 calc PR A 1 N3 N 0.2629(12) 0.6143(16) 0.4208(5) 0.042(3) Uani 0.409(9) 1 d P A 2 C311 C 0.2752(13) 0.6656(15) 0.3597(5) 0.057(4) Uani 0.409(9) 1 d P A 2 H31A H 0.3069 0.7249 0.3566 0.069 Uiso 0.409(9) 1 calc PR A 2 H31B H 0.3349 0.6019 0.3417 0.069 Uiso 0.409(9) 1 calc PR A 2 C341 C 0.3887(13) 0.5609(16) 0.4447(6) 0.060(5) Uani 0.409(9) 1 d P A 2 H34A H 0.3846 0.5260 0.4833 0.089 Uiso 0.409(9) 1 calc PR A 2 H34B H 0.4164 0.6225 0.4410 0.089 Uiso 0.409(9) 1 calc PR A 2 H34C H 0.4450 0.5003 0.4248 0.089 Uiso 0.409(9) 1 calc PR A 2 C332 C 0.198(2) 0.820(2) 0.4467(11) 0.105(8) Uani 0.409(9) 1 d P A 2 H33A H 0.1336 0.8737 0.4673 0.158 Uiso 0.409(9) 1 calc PR A 2 H33B H 0.1965 0.8582 0.4083 0.158 Uiso 0.409(9) 1 calc PR A 2 H33C H 0.2753 0.7982 0.4614 0.158 Uiso 0.409(9) 1 calc PR A 2 C331 C 0.177(2) 0.7080(18) 0.4513(11) 0.062(5) Uani 0.409(9) 1 d P A 2 H33D H 0.1782 0.6715 0.4904 0.075 Uiso 0.409(9) 1 calc PR A 2 H33E H 0.0955 0.7331 0.4390 0.075 Uiso 0.409(9) 1 calc PR A 2 C321 C 0.2159(19) 0.5178(17) 0.4296(10) 0.039(5) Uani 0.409(9) 1 d P A 2 H32A H 0.1366 0.5518 0.4132 0.047 Uiso 0.409(9) 1 calc PR A 2 H32B H 0.2051 0.4912 0.4692 0.047 Uiso 0.409(9) 1 calc PR A 2 C322 C 0.3031(18) 0.4097(17) 0.4040(7) 0.062(4) Uani 0.409(9) 1 d P A 2 H32C H 0.2688 0.3525 0.4097 0.093 Uiso 0.409(9) 1 calc PR A 2 H32D H 0.3807 0.3735 0.4213 0.093 Uiso 0.409(9) 1 calc PR A 2 H32E H 0.3144 0.4355 0.3648 0.093 Uiso 0.409(9) 1 calc PR A 2 C312 C 0.1586(15) 0.7223(18) 0.3290(7) 0.053(4) Uani 0.409(9) 1 d P A 2 H31C H 0.1739 0.7540 0.2910 0.079 Uiso 0.409(9) 1 calc PR A 2 H31D H 0.0987 0.7858 0.3462 0.079 Uiso 0.409(9) 1 calc PR A 2 H31E H 0.1284 0.6633 0.3300 0.079 Uiso 0.409(9) 1 calc PR A 2 N1 N 1.1459(5) 0.2131(5) 0.9310(2) 0.0635(13) Uani 1 1 d DU . . C141 C 1.145(2) 0.3223(19) 0.8925(9) 0.135(9) Uani 0.525(9) 1 d P B 1 H14A H 1.2237 0.3037 0.8735 0.203 Uiso 0.525(9) 1 calc PR B 1 H14B H 1.1285 0.3833 0.9133 0.203 Uiso 0.525(9) 1 calc PR B 1 H14C H 1.0831 0.3504 0.8658 0.203 Uiso 0.525(9) 1 calc PR B 1 C113 C 1.2430(13) 0.1675(14) 0.9705(6) 0.075(4) Uani 0.525(9) 1 d PU B 1 H11A H 1.3183 0.1660 0.9511 0.090 Uiso 0.525(9) 1 calc PR B 1 H11B H 1.2577 0.0866 0.9894 0.090 Uiso 0.525(9) 1 calc PR B 1 C123 C 1.0324(15) 0.2408(11) 0.9599(5) 0.092(6) Uani 0.525(9) 1 d PD B 1 H12A H 0.9713 0.2596 0.9335 0.110 Uiso 0.525(9) 1 calc PR B 1 H12B H 1.0116 0.3128 0.9741 0.110 Uiso 0.525(9) 1 calc PR B 1 C133 C 1.1808(14) 0.128(2) 0.8914(8) 0.110(7) Uani 0.525(9) 1 d P B 1 H13A H 1.2594 0.1217 0.8742 0.132 Uiso 0.525(9) 1 calc PR B 1 H13B H 1.1947 0.0502 0.9140 0.132 Uiso 0.525(9) 1 calc PR B 1 C134 C 1.104(3) 0.147(5) 0.8475(19) 0.16(2) Uani 0.525(9) 1 d P B 1 H13C H 1.1421 0.0823 0.8278 0.242 Uiso 0.525(9) 1 calc PR B 1 H13D H 1.0939 0.2210 0.8223 0.242 Uiso 0.525(9) 1 calc PR B 1 H13E H 1.0260 0.1521 0.8629 0.242 Uiso 0.525(9) 1 calc PR B 1 C114 C 1.201(4) 0.253(3) 1.0139(15) 0.135(13) Uani 0.525(9) 1 d PU B 1 H11C H 1.2635 0.2249 1.0402 0.202 Uiso 0.525(9) 1 calc PR B 1 H11D H 1.1267 0.2528 1.0331 0.202 Uiso 0.525(9) 1 calc PR B 1 H11E H 1.1860 0.3325 0.9948 0.202 Uiso 0.525(9) 1 calc PR B 1 C122 C 1.022(2) 0.146(3) 1.0081(13) 0.170(17) Uani 0.525(9) 1 d PD B 1 H12C H 0.9397 0.1740 1.0233 0.255 Uiso 0.525(9) 1 calc PR B 1 H12D H 1.0771 0.1311 1.0364 0.255 Uiso 0.525(9) 1 calc PR B 1 H12E H 1.0432 0.0737 0.9951 0.255 Uiso 0.525(9) 1 calc PR B 1 C142 C 1.2770(17) 0.1399(17) 0.9136(7) 0.096(6) Uani 0.475(9) 1 d P B 2 H14D H 1.3242 0.0962 0.9462 0.144 Uiso 0.475(9) 1 calc PR B 2 H14E H 1.3109 0.1923 0.8916 0.144 Uiso 0.475(9) 1 calc PR B 2 H14F H 1.2789 0.0849 0.8922 0.144 Uiso 0.475(9) 1 calc PR B 2 C131 C 1.0718(19) 0.2756(18) 0.8823(8) 0.098(6) Uani 0.475(9) 1 d PD B 2 H13F H 1.1052 0.3284 0.8591 0.118 Uiso 0.475(9) 1 calc PR B 2 H13G H 0.9897 0.3253 0.8945 0.118 Uiso 0.475(9) 1 calc PR B 2 C111 C 1.1483(17) 0.2991(13) 0.9665(7) 0.090(6) Uani 0.475(9) 1 d PD B 2 H11F H 1.1717 0.3584 0.9421 0.108 Uiso 0.475(9) 1 calc PR B 2 H11G H 1.0659 0.3412 0.9810 0.108 Uiso 0.475(9) 1 calc PR B 2 C121 C 1.1035(15) 0.1287(14) 0.9720(7) 0.076(5) Uani 0.475(9) 1 d PD B 2 H12F H 1.1107 0.0668 0.9530 0.091 Uiso 0.475(9) 1 calc PR B 2 H12G H 1.1616 0.0899 1.0016 0.091 Uiso 0.475(9) 1 calc PR B 2 C132 C 1.063(3) 0.197(4) 0.8471(12) 0.109(13) Uani 0.475(9) 1 d PD B 2 H13H H 1.0133 0.2464 0.8158 0.163 Uiso 0.475(9) 1 calc PR B 2 H13I H 1.0264 0.1468 0.8689 0.163 Uiso 0.475(9) 1 calc PR B 2 H13J H 1.1434 0.1483 0.8340 0.163 Uiso 0.475(9) 1 calc PR B 2 C112 C 1.235(3) 0.239(4) 1.0155(10) 0.093(10) Uani 0.475(9) 1 d PD B 2 H11H H 1.2291 0.2990 1.0350 0.140 Uiso 0.475(9) 1 calc PR B 2 H11I H 1.3177 0.2005 1.0017 0.140 Uiso 0.475(9) 1 calc PR B 2 H11J H 1.2124 0.1812 1.0404 0.140 Uiso 0.475(9) 1 calc PR B 2 C124 C 0.9808(17) 0.173(2) 0.9986(6) 0.079(7) Uani 0.475(9) 1 d PD B 2 H12H H 0.9689 0.1066 1.0224 0.119 Uiso 0.475(9) 1 calc PR B 2 H12I H 0.9206 0.2102 0.9706 0.119 Uiso 0.475(9) 1 calc PR B 2 H12J H 0.9726 0.2295 1.0203 0.119 Uiso 0.475(9) 1 calc PR B 2 C106 C 0.9347(5) 0.8824(5) 0.7671(3) 0.0528(14) Uani 1 1 d . . . H10A H 0.8842 0.8699 0.7972 0.063 Uiso 1 1 calc R . . C102 C 0.9956(5) 0.8861(5) 0.6705(3) 0.0626(17) Uani 1 1 d . . . H10B H 0.9876 0.8758 0.6354 0.075 Uiso 1 1 calc R . . C105 C 1.0254(7) 0.9165(6) 0.7740(4) 0.079(2) Uani 1 1 d . . . H10C H 1.0365 0.9245 0.8091 0.095 Uiso 1 1 calc R . . C104 C 1.0983(6) 0.9383(6) 0.7301(5) 0.086(3) Uani 1 1 d . . . H10D H 1.1563 0.9644 0.7349 0.103 Uiso 1 1 calc R . . C103 C 1.0857(6) 0.9220(7) 0.6799(5) 0.090(3) Uani 1 1 d . . . H10E H 1.1376 0.9344 0.6505 0.108 Uiso 1 1 calc R . . C206 C 0.8656(6) 0.7482(5) 0.6049(2) 0.0515(6) Uani 1 1 d . . . H20C H 0.9275 0.6795 0.6232 0.062 Uiso 1 1 calc R . . C204 C 0.7611(5) 0.8630(5) 0.5204(2) 0.0515(6) Uani 1 1 d . . . H20D H 0.7519 0.8717 0.4826 0.062 Uiso 1 1 calc R . . C205 C 0.8510(5) 0.7612(5) 0.5483(2) 0.0515(6) Uani 1 1 d . . . H20E H 0.9023 0.7006 0.5294 0.062 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 Pt1 0.02204(8) 0.01919(8) 0.01909(8) -0.00562(5) 0.00144(5) -0.00672(6) Ge2 0.0238(2) 0.0202(2) 0.0262(2) -0.00592(16) 0.00110(17) -0.00709(18) Ge1 0.0473(3) 0.0253(2) 0.0255(2) -0.00689(18) -0.0028(2) -0.0159(2) S1 0.0308(5) 0.0243(5) 0.0248(5) -0.0063(4) 0.0011(4) -0.0122(4) S2 0.0258(5) 0.0232(5) 0.0286(5) -0.0034(4) 0.0059(4) -0.0051(4) P2 0.0290(6) 0.0205(5) 0.0251(5) -0.0039(4) 0.0029(4) -0.0087(5) P1 0.0242(5) 0.0243(5) 0.0258(5) -0.0076(4) 0.0023(4) -0.0063(5) B205 0.032(3) 0.029(3) 0.040(3) -0.004(2) -0.001(2) -0.019(2) B201 0.030(3) 0.021(2) 0.032(2) -0.0090(19) 0.004(2) -0.006(2) C201 0.0663(15) 0.0387(12) 0.0305(10) -0.0105(9) 0.0013(10) -0.0041(11) C3 0.036(2) 0.023(2) 0.034(2) 0.0019(18) 0.0028(19) -0.0083(19) C302 0.042(3) 0.030(2) 0.034(2) -0.0082(19) -0.002(2) -0.015(2) C301 0.031(2) 0.026(2) 0.031(2) -0.0121(17) 0.0052(18) -0.0122(19) C1 0.029(2) 0.027(2) 0.028(2) -0.0064(18) 0.0014(18) -0.0004(19) C2 0.037(2) 0.024(2) 0.035(2) -0.0057(18) 0.0050(19) -0.009(2) C202 0.0663(15) 0.0387(12) 0.0305(10) -0.0105(9) 0.0013(10) -0.0041(11) C306 0.045(3) 0.031(2) 0.047(3) -0.011(2) 0.006(2) -0.021(2) B206 0.022(2) 0.030(3) 0.036(3) -0.008(2) 0.002(2) -0.007(2) B202 0.026(2) 0.029(3) 0.038(3) -0.007(2) -0.004(2) -0.010(2) C303 0.051(3) 0.049(3) 0.042(3) -0.010(2) -0.010(2) -0.020(3) B210 0.034(3) 0.022(2) 0.035(3) -0.006(2) 0.002(2) -0.011(2) C203 0.0663(15) 0.0387(12) 0.0305(10) -0.0105(9) 0.0013(10) -0.0041(11) B211 0.031(3) 0.027(3) 0.032(3) -0.003(2) 0.003(2) -0.002(2) C401 0.029(2) 0.023(2) 0.026(2) 0.0009(16) 0.0031(17) -0.0092(18) C101 0.022(2) 0.031(2) 0.058(3) -0.013(2) 0.001(2) -0.007(2) C406 0.036(3) 0.062(3) 0.032(2) -0.012(2) 0.004(2) -0.021(3) B203 0.036(3) 0.030(3) 0.031(3) -0.011(2) -0.005(2) -0.005(2) B207 0.034(3) 0.032(3) 0.035(3) -0.009(2) -0.007(2) -0.006(2) C404 0.046(3) 0.073(4) 0.028(3) -0.006(2) 0.012(2) -0.019(3) C402 0.040(3) 0.056(3) 0.036(3) -0.011(2) 0.005(2) -0.022(3) B204 0.027(3) 0.038(3) 0.028(3) -0.003(2) 0.004(2) -0.006(2) B208 0.034(3) 0.037(3) 0.029(3) -0.006(2) 0.002(2) -0.004(2) C304 0.056(3) 0.052(3) 0.063(4) -0.030(3) -0.009(3) -0.023(3) C305 0.060(3) 0.042(3) 0.071(4) -0.026(3) 0.002(3) -0.031(3) C405 0.047(3) 0.076(4) 0.029(3) -0.012(3) 0.002(2) -0.021(3) B209 0.034(3) 0.035(3) 0.037(3) 0.005(2) 0.004(2) -0.016(2) C403 0.041(3) 0.076(4) 0.046(3) -0.009(3) 0.013(2) -0.030(3) B101 0.051(3) 0.024(3) 0.037(3) -0.005(2) -0.009(2) -0.015(2) B105 0.050(3) 0.041(3) 0.042(3) -0.022(3) 0.007(3) -0.016(3) B110 0.083(5) 0.029(3) 0.041(3) -0.015(2) -0.007(3) -0.017(3) B103 0.106(6) 0.027(3) 0.032(3) 0.000(2) -0.019(3) -0.018(3) B102 0.062(4) 0.032(3) 0.053(4) -0.010(3) -0.021(3) -0.015(3) B109 0.110(6) 0.060(4) 0.038(3) -0.025(3) 0.020(4) -0.048(5) B106 0.085(5) 0.037(3) 0.058(4) -0.013(3) -0.025(4) -0.027(3) B104 0.111(6) 0.053(4) 0.032(3) -0.021(3) 0.022(3) -0.050(4) B107 0.109(6) 0.040(4) 0.058(4) -0.009(3) -0.051(4) -0.012(4) B108 0.155(8) 0.041(4) 0.026(3) -0.005(3) -0.004(4) -0.045(5) B111 0.119(7) 0.038(3) 0.037(3) -0.010(3) -0.021(4) -0.027(4) C41 0.066(5) 0.052(4) 0.151(9) -0.013(5) -0.024(5) -0.020(4) C40 0.077(6) 0.072(6) 0.195(14) 0.027(8) -0.003(8) -0.032(5) N4 0.193(13) 0.141(11) 0.244(16) 0.033(10) 0.088(12) -0.056(9) N5 0.174(13) 0.142(11) 0.249(19) -0.107(12) -0.115(12) 0.018(10) C50 0.197(19) 0.076(8) 0.21(2) -0.082(12) -0.107(15) 0.020(11) C51 0.42(4) 0.147(15) 0.24(2) -0.132(15) 0.13(2) -0.149(19) N2 0.054(7) 0.065(8) 0.056(6) 0.007(6) 0.000(5) -0.035(6) C222 0.110(13) 0.075(10) 0.146(15) -0.027(10) 0.003(11) -0.048(9) C221 0.053(7) 0.073(9) 0.088(9) -0.020(7) 0.015(7) -0.044(7) C211 0.041(5) 0.101(9) 0.054(6) 0.019(6) -0.003(4) -0.039(6) C212 0.047(6) 0.174(16) 0.049(7) 0.035(8) -0.009(5) -0.047(8) C231 0.075(10) 0.059(12) 0.058(8) -0.002(9) 0.016(7) -0.036(10) C232 0.106(12) 0.075(11) 0.104(12) -0.032(9) 0.033(9) -0.012(10) C241 0.063(8) 0.083(10) 0.065(9) 0.010(7) -0.012(7) -0.043(7) N3 0.036(7) 0.047(8) 0.039(6) 0.007(6) -0.009(5) -0.021(7) C311 0.052(8) 0.080(11) 0.037(7) 0.025(7) -0.015(6) -0.039(8) C341 0.051(8) 0.086(12) 0.045(8) 0.009(8) -0.022(6) -0.036(8) C332 0.117(19) 0.100(17) 0.14(2) -0.042(15) 0.036(16) -0.087(16) C331 0.062(13) 0.061(12) 0.075(14) -0.005(11) 0.007(12) -0.042(11) C321 0.030(7) 0.052(13) 0.037(7) 0.017(9) 0.000(5) -0.031(10) C322 0.084(12) 0.051(10) 0.054(9) -0.018(8) 0.007(8) -0.029(9) C312 0.048(8) 0.080(12) 0.041(9) -0.004(8) 0.009(7) -0.043(8) N1 0.064(3) 0.055(3) 0.064(3) 0.001(3) -0.005(3) -0.023(3) C141 0.18(2) 0.128(17) 0.114(15) 0.055(13) -0.042(15) -0.112(17) C113 0.069(8) 0.096(10) 0.070(8) -0.017(7) 0.001(6) -0.045(8) C123 0.111(12) 0.042(7) 0.055(7) -0.010(6) 0.032(8) 0.019(7) C133 0.060(9) 0.169(19) 0.126(15) -0.105(14) 0.022(9) -0.042(11) C134 0.10(3) 0.28(5) 0.15(3) -0.14(3) 0.054(19) -0.09(3) C114 0.19(3) 0.19(3) 0.128(18) -0.094(18) 0.051(16) -0.16(2) C122 0.090(17) 0.16(2) 0.24(4) 0.11(2) -0.10(2) -0.075(16) C142 0.089(12) 0.100(14) 0.075(11) -0.027(10) 0.039(9) -0.026(11) C131 0.092(13) 0.092(14) 0.086(13) 0.009(11) -0.002(10) -0.030(11) C111 0.094(13) 0.047(9) 0.117(16) 0.003(9) -0.018(11) -0.024(9) C121 0.079(11) 0.068(10) 0.079(10) -0.006(8) 0.019(8) -0.040(9) C132 0.08(2) 0.23(4) 0.055(12) -0.046(17) 0.031(11) -0.10(3) C112 0.112(17) 0.18(3) 0.037(9) -0.008(11) 0.001(9) -0.110(18) C124 0.074(14) 0.14(2) 0.035(7) -0.017(10) 0.005(8) -0.060(14) C106 0.035(3) 0.044(3) 0.078(4) -0.024(3) -0.019(3) -0.005(2) C102 0.043(3) 0.053(4) 0.091(5) -0.014(3) 0.015(3) -0.024(3) C105 0.057(4) 0.043(4) 0.141(7) -0.033(4) -0.047(5) -0.004(3) C104 0.041(4) 0.053(4) 0.176(9) -0.021(5) -0.041(5) -0.021(3) C103 0.036(3) 0.067(5) 0.165(9) -0.012(5) 0.009(4) -0.029(3) C206 0.0663(15) 0.0387(12) 0.0305(10) -0.0105(9) 0.0013(10) -0.0041(11) C204 0.0663(15) 0.0387(12) 0.0305(10) -0.0105(9) 0.0013(10) -0.0041(11) C205 0.0663(15) 0.0387(12) 0.0305(10) -0.0105(9) 0.0013(10) -0.0041(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pt1 P2 2.2599(11) . ? Pt1 P1 2.2629(11) . ? Pt1 S1 2.3680(11) . ? Pt1 S2 2.3757(10) . ? Ge2 B204 2.106(5) . ? Ge2 B205 2.110(5) . ? Ge2 B201 2.116(5) . ? Ge2 B203 2.117(5) . ? Ge2 B202 2.126(5) . ? Ge2 S2 2.1488(11) . ? Ge1 B102 2.101(6) . ? Ge1 B105 2.104(6) . ? Ge1 B103 2.105(6) . ? Ge1 B101 2.109(5) . ? Ge1 B104 2.123(6) . ? Ge1 S1 2.1413(11) . ? P2 C401 1.812(4) . ? P2 C301 1.813(4) . ? P2 C3 1.820(4) . ? P1 C101 1.818(5) . ? P1 C201 1.821(5) . ? P1 C1 1.829(4) . ? B205 B209 1.762(7) . ? B205 B210 1.772(7) . ? B205 B201 1.888(7) . ? B205 B204 1.902(8) . ? B201 B206 1.763(7) . ? B201 B210 1.763(7) . ? B201 B202 1.882(7) . ? C201 C206 1.381(7) . ? C201 C202 1.385(7) . ? C3 C2 1.537(6) . ? C302 C303 1.380(7) . ? C302 C301 1.390(6) . ? C301 C306 1.408(6) . ? C1 C2 1.520(7) . ? C202 C203 1.384(7) . ? C306 C305 1.378(7) . ? B206 B202 1.762(7) . ? B206 B211 1.776(7) . ? B206 B207 1.787(7) . ? B206 B210 1.787(7) . ? B202 B207 1.773(7) . ? B202 B203 1.880(7) . ? C303 C304 1.392(8) . ? B210 B209 1.781(7) . ? B210 B211 1.785(8) . ? C203 C204 1.383(7) . ? B211 B207 1.773(8) . ? B211 B208 1.777(7) . ? B211 B209 1.781(8) . ? C401 C406 1.384(7) . ? C401 C402 1.389(7) . ? C101 C106 1.388(8) . ? C101 C102 1.389(8) . ? C406 C405 1.388(7) . ? B203 B207 1.771(7) . ? B203 B208 1.777(8) . ? B203 B204 1.878(8) . ? B207 B208 1.780(8) . ? C404 C405 1.361(8) . ? C404 C403 1.379(8) . ? C402 C403 1.393(7) . ? B204 B208 1.762(8) . ? B204 B209 1.780(8) . ? B208 B209 1.794(9) . ? C304 C305 1.370(8) . ? B101 B110 1.768(8) . ? B101 B106 1.770(8) . ? B101 B102 1.877(8) . ? B101 B105 1.882(9) . ? B105 B110 1.772(9) . ? B105 B109 1.782(9) . ? B105 B104 1.919(9) . ? B110 B111 1.762(9) . ? B110 B106 1.781(11) . ? B110 B109 1.798(10) . ? B103 B107 1.753(10) . ? B103 B108 1.769(10) . ? B103 B102 1.869(10) . ? B103 B104 1.905(12) . ? B102 B106 1.770(9) . ? B102 B107 1.773(10) . ? B109 B111 1.752(12) . ? B109 B108 1.772(12) . ? B109 B104 1.777(9) . ? B106 B107 1.773(10) . ? B106 B111 1.780(11) . ? B104 B108 1.753(11) . ? B107 B108 1.767(14) . ? B107 B111 1.778(12) . ? B108 B111 1.771(9) . ? C41 C40 1.423(17) . ? C40 N4 1.124(18) . ? N5 C50 1.38(3) . ? C50 C51 1.34(3) . ? N2 C211 1.509(14) . ? N2 C231 1.515(18) . ? N2 C221 1.535(17) . ? N2 C241 1.555(17) . ? C222 C221 1.529(19) . ? C211 C212 1.501(14) . ? C231 C232 1.47(2) . ? N3 C331 1.48(3) . ? N3 C341 1.515(17) . ? N3 C311 1.516(17) . ? N3 C321 1.525(18) . ? C311 C312 1.50(2) . ? C332 C331 1.52(2) . ? C321 C322 1.53(3) . ? N1 C123 1.402(15) . ? N1 C131 1.454(19) . ? N1 C113 1.459(14) . ? N1 C141 1.486(16) . ? N1 C133 1.507(16) . ? N1 C121 1.511(15) . ? N1 C142 1.513(16) . ? N1 C111 1.559(14) . ? C113 C114 1.58(4) . ? C123 C122 1.518(18) . ? C133 C134 1.43(4) . ? C131 C132 1.509(19) . ? C111 C112 1.541(18) . ? C121 C124 1.465(16) . ? C106 C105 1.390(9) . ? C102 C103 1.419(10) . ? C105 C104 1.364(12) . ? C104 C103 1.342(12) . ? C206 C205 1.396(7) . ? C204 C205 1.374(7) . ? 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 P2 Pt1 P1 93.83(4) . . ? P2 Pt1 S1 177.11(4) . . ? P1 Pt1 S1 88.85(4) . . ? P2 Pt1 S2 85.97(4) . . ? P1 Pt1 S2 174.47(4) . . ? S1 Pt1 S2 91.26(4) . . ? B204 Ge2 B205 53.7(2) . . ? B204 Ge2 B201 92.6(2) . . ? B205 Ge2 B201 53.1(2) . . ? B204 Ge2 B203 52.8(2) . . ? B205 Ge2 B203 92.8(2) . . ? B201 Ge2 B203 92.0(2) . . ? B204 Ge2 B202 92.0(2) . . ? B205 Ge2 B202 92.4(2) . . ? B201 Ge2 B202 52.7(2) . . ? B203 Ge2 B202 52.6(2) . . ? B204 Ge2 S2 140.43(15) . . ? B205 Ge2 S2 136.77(15) . . ? B201 Ge2 S2 124.50(14) . . ? B203 Ge2 S2 128.90(15) . . ? B202 Ge2 S2 120.32(15) . . ? B102 Ge1 B105 92.7(3) . . ? B102 Ge1 B103 52.8(3) . . ? B105 Ge1 B103 93.3(3) . . ? B102 Ge1 B101 53.0(2) . . ? B105 Ge1 B101 53.1(2) . . ? B103 Ge1 B101 92.5(2) . . ? B102 Ge1 B104 93.1(3) . . ? B105 Ge1 B104 54.0(3) . . ? B103 Ge1 B104 53.6(3) . . ? B101 Ge1 B104 93.4(2) . . ? B102 Ge1 S1 124.8(2) . . ? B105 Ge1 S1 130.50(18) . . ? B103 Ge1 S1 134.03(18) . . ? B101 Ge1 S1 122.85(16) . . ? B104 Ge1 S1 137.9(2) . . ? Ge1 S1 Pt1 102.79(4) . . ? Ge2 S2 Pt1 104.83(4) . . ? C401 P2 C301 108.2(2) . . ? C401 P2 C3 102.51(19) . . ? C301 P2 C3 104.6(2) . . ? C401 P2 Pt1 110.46(15) . . ? C301 P2 Pt1 113.79(15) . . ? C3 P2 Pt1 116.39(16) . . ? C101 P1 C201 106.3(3) . . ? C101 P1 C1 101.1(2) . . ? C201 P1 C1 107.0(2) . . ? C101 P1 Pt1 116.47(15) . . ? C201 P1 Pt1 108.01(19) . . ? C1 P1 Pt1 117.14(15) . . ? B209 B205 B210 60.5(3) . . ? B209 B205 B201 106.0(4) . . ? B210 B205 B201 57.5(3) . . ? B209 B205 B204 58.0(3) . . ? B210 B205 B204 106.2(4) . . ? B201 B205 B204 107.2(3) . . ? B209 B205 Ge2 112.5(3) . . ? B210 B205 Ge2 112.6(3) . . ? B201 B205 Ge2 63.6(2) . . ? B204 B205 Ge2 63.1(2) . . ? B206 B201 B210 60.9(3) . . ? B206 B201 B202 57.7(3) . . ? B210 B201 B202 106.8(3) . . ? B206 B201 B205 106.8(3) . . ? B210 B201 B205 57.9(3) . . ? B202 B201 B205 108.3(3) . . ? B206 B201 Ge2 112.9(3) . . ? B210 B201 Ge2 112.7(3) . . ? B202 B201 Ge2 64.0(2) . . ? B205 B201 Ge2 63.3(2) . . ? C206 C201 C202 118.3(5) . . ? C206 C201 P1 122.7(4) . . ? C202 C201 P1 118.9(4) . . ? C2 C3 P2 114.1(3) . . ? C303 C302 C301 120.2(5) . . ? C302 C301 C306 118.9(4) . . ? C302 C301 P2 120.1(3) . . ? C306 C301 P2 120.9(4) . . ? C2 C1 P1 115.7(3) . . ? C1 C2 C3 112.9(4) . . ? C203 C202 C201 121.4(5) . . ? C305 C306 C301 119.8(5) . . ? B202 B206 B201 64.5(3) . . ? B202 B206 B211 109.3(4) . . ? B201 B206 B211 109.2(4) . . ? B202 B206 B207 59.9(3) . . ? B201 B206 B207 111.2(3) . . ? B211 B206 B207 59.7(3) . . ? B202 B206 B210 111.2(4) . . ? B201 B206 B210 59.6(3) . . ? B211 B206 B210 60.1(3) . . ? B207 B206 B210 108.2(4) . . ? B206 B202 B207 60.7(3) . . ? B206 B202 B203 106.8(4) . . ? B207 B202 B203 57.9(3) . . ? B206 B202 B201 57.8(3) . . ? B207 B202 B201 106.5(4) . . ? B203 B202 B201 108.1(3) . . ? B206 B202 Ge2 112.4(3) . . ? B207 B202 Ge2 112.4(3) . . ? B203 B202 Ge2 63.5(2) . . ? B201 B202 Ge2 63.4(2) . . ? C302 C303 C304 120.5(5) . . ? B201 B210 B205 64.6(3) . . ? B201 B210 B209 110.7(4) . . ? B205 B210 B209 59.5(3) . . ? B201 B210 B211 108.8(4) . . ? B205 B210 B211 109.1(4) . . ? B209 B210 B211 59.9(3) . . ? B201 B210 B206 59.6(3) . . ? B205 B210 B206 111.0(4) . . ? B209 B210 B206 107.8(4) . . ? B211 B210 B206 59.6(3) . . ? C204 C203 C202 119.9(5) . . ? B207 B211 B206 60.5(3) . . ? B207 B211 B208 60.2(3) . . ? B206 B211 B208 108.6(4) . . ? B207 B211 B209 108.8(4) . . ? B206 B211 B209 108.3(4) . . ? B208 B211 B209 60.5(3) . . ? B207 B211 B210 108.9(4) . . ? B206 B211 B210 60.2(3) . . ? B208 B211 B210 108.7(4) . . ? B209 B211 B210 59.9(3) . . ? C406 C401 C402 118.9(4) . . ? C406 C401 P2 117.3(3) . . ? C402 C401 P2 123.7(4) . . ? C106 C101 C102 119.5(5) . . ? C106 C101 P1 118.4(4) . . ? C102 C101 P1 122.2(5) . . ? C401 C406 C405 120.3(5) . . ? B207 B203 B208 60.2(3) . . ? B207 B203 B204 106.2(4) . . ? B208 B203 B204 57.6(3) . . ? B207 B203 B202 58.0(3) . . ? B208 B203 B202 106.2(4) . . ? B204 B203 B202 108.2(3) . . ? B207 B203 Ge2 112.9(3) . . ? B208 B203 Ge2 112.1(3) . . ? B204 B203 Ge2 63.3(2) . . ? B202 B203 Ge2 64.0(2) . . ? B203 B207 B211 109.5(4) . . ? B203 B207 B202 64.1(3) . . ? B211 B207 B202 108.9(4) . . ? B203 B207 B208 60.1(3) . . ? B211 B207 B208 60.0(3) . . ? B202 B207 B208 110.9(4) . . ? B203 B207 B206 110.6(4) . . ? B211 B207 B206 59.9(3) . . ? B202 B207 B206 59.3(3) . . ? B208 B207 B206 108.0(4) . . ? C405 C404 C403 119.8(5) . . ? C401 C402 C403 120.1(5) . . ? B208 B204 B209 60.9(3) . . ? B208 B204 B203 58.4(3) . . ? B209 B204 B203 106.9(4) . . ? B208 B204 B205 106.4(4) . . ? B209 B204 B205 57.1(3) . . ? B203 B204 B205 108.2(3) . . ? B208 B204 Ge2 113.3(3) . . ? B209 B204 Ge2 112.0(3) . . ? B203 B204 Ge2 63.9(2) . . ? B205 B204 Ge2 63.3(2) . . ? B204 B208 B211 109.6(4) . . ? B204 B208 B203 64.1(3) . . ? B211 B208 B203 109.0(4) . . ? B204 B208 B207 111.0(4) . . ? B211 B208 B207 59.8(3) . . ? B203 B208 B207 59.7(3) . . ? B204 B208 B209 60.1(3) . . ? B211 B208 B209 59.8(3) . . ? B203 B208 B209 110.7(4) . . ? B207 B208 B209 107.9(4) . . ? C305 C304 C303 119.5(5) . . ? C304 C305 C306 121.1(5) . . ? C404 C405 C406 120.7(5) . . ? B205 B209 B204 65.0(3) . . ? B205 B209 B211 109.7(4) . . ? B204 B209 B211 108.6(4) . . ? B205 B209 B210 60.0(3) . . ? B204 B209 B210 111.3(4) . . ? B211 B209 B210 60.1(3) . . ? B205 B209 B208 111.2(4) . . ? B204 B209 B208 59.1(3) . . ? B211 B209 B208 59.6(3) . . ? B210 B209 B208 108.1(4) . . ? C404 C403 C402 120.2(5) . . ? B110 B101 B106 60.4(4) . . ? B110 B101 B102 106.6(4) . . ? B106 B101 B102 58.0(3) . . ? B110 B101 B105 58.0(3) . . ? B106 B101 B105 106.4(4) . . ? B102 B101 B105 108.1(4) . . ? B110 B101 Ge1 112.4(4) . . ? B106 B101 Ge1 112.3(3) . . ? B102 B101 Ge1 63.3(2) . . ? B105 B101 Ge1 63.3(2) . . ? B110 B105 B109 60.8(4) . . ? B110 B105 B101 57.8(3) . . ? B109 B105 B101 106.5(5) . . ? B110 B105 B104 106.4(4) . . ? B109 B105 B104 57.2(3) . . ? B101 B105 B104 108.2(4) . . ? B110 B105 Ge1 112.5(4) . . ? B109 B105 Ge1 111.9(4) . . ? B101 B105 Ge1 63.6(2) . . ? B104 B105 Ge1 63.5(3) . . ? B111 B110 B101 109.5(5) . . ? B111 B110 B105 108.8(5) . . ? B101 B110 B105 64.2(3) . . ? B111 B110 B106 60.3(4) . . ? B101 B110 B106 59.8(4) . . ? B105 B110 B106 110.9(4) . . ? B111 B110 B109 59.0(4) . . ? B101 B110 B109 110.8(4) . . ? B105 B110 B109 59.9(4) . . ? B106 B110 B109 107.6(5) . . ? B107 B103 B108 60.2(5) . . ? B107 B103 B102 58.5(4) . . ? B108 B103 B102 106.6(4) . . ? B107 B103 B104 106.0(5) . . ? B108 B103 B104 56.8(4) . . ? B102 B103 B104 108.7(4) . . ? B107 B103 Ge1 112.6(4) . . ? B108 B103 Ge1 111.5(5) . . ? B102 B103 Ge1 63.5(3) . . ? B104 B103 Ge1 63.7(3) . . ? B106 B102 B107 60.1(4) . . ? B106 B102 B103 106.4(5) . . ? B107 B102 B103 57.5(4) . . ? B106 B102 B101 58.0(3) . . ? B107 B102 B101 106.0(5) . . ? B103 B102 B101 108.7(5) . . ? B106 B102 Ge1 112.6(4) . . ? B107 B102 Ge1 111.9(5) . . ? B103 B102 Ge1 63.7(3) . . ? B101 B102 Ge1 63.7(3) . . ? B111 B109 B108 60.3(5) . . ? B111 B109 B104 109.7(6) . . ? B108 B109 B104 59.2(4) . . ? B111 B109 B105 108.7(5) . . ? B108 B109 B105 110.5(5) . . ? B104 B109 B105 65.3(4) . . ? B111 B109 B110 59.5(4) . . ? B108 B109 B110 107.7(6) . . ? B104 B109 B110 111.6(5) . . ? B105 B109 B110 59.3(4) . . ? B102 B106 B101 64.1(3) . . ? B102 B106 B107 60.1(4) . . ? B101 B106 B107 110.8(4) . . ? B102 B106 B111 109.4(5) . . ? B101 B106 B111 108.6(5) . . ? B107 B106 B111 60.1(5) . . ? B102 B106 B110 110.9(5) . . ? B101 B106 B110 59.7(4) . . ? B107 B106 B110 107.9(6) . . ? B111 B106 B110 59.3(4) . . ? B108 B104 B109 60.3(4) . . ? B108 B104 B103 57.7(4) . . ? B109 B104 B103 105.7(5) . . ? B108 B104 B105 105.3(4) . . ? B109 B104 B105 57.5(3) . . ? B103 B104 B105 106.3(4) . . ? B108 B104 Ge1 111.3(5) . . ? B109 B104 Ge1 111.3(4) . . ? B103 B104 Ge1 62.7(3) . . ? B105 B104 Ge1 62.5(2) . . ? B103 B107 B108 60.3(4) . . ? B103 B107 B102 64.0(4) . . ? B108 B107 B102 111.0(5) . . ? B103 B107 B106 111.5(4) . . ? B108 B107 B106 108.5(6) . . ? B102 B107 B106 59.9(4) . . ? B103 B107 B111 109.9(6) . . ? B108 B107 B111 59.9(5) . . ? B102 B107 B111 109.3(5) . . ? B106 B107 B111 60.1(4) . . ? B104 B108 B107 112.3(5) . . ? B104 B108 B103 65.5(4) . . ? B107 B108 B103 59.5(4) . . ? B104 B108 B111 110.0(5) . . ? B107 B108 B111 60.4(5) . . ? B103 B108 B111 109.5(5) . . ? B104 B108 B109 60.6(4) . . ? B107 B108 B109 108.3(5) . . ? B103 B108 B109 112.1(5) . . ? B111 B108 B109 59.3(4) . . ? B109 B111 B110 61.6(4) . . ? B109 B111 B108 60.4(5) . . ? B110 B111 B108 109.3(5) . . ? B109 B111 B107 108.7(5) . . ? B110 B111 B107 108.5(5) . . ? B108 B111 B107 59.7(5) . . ? B109 B111 B106 109.7(5) . . ? B110 B111 B106 60.4(4) . . ? B108 B111 B106 108.1(5) . . ? B107 B111 B106 59.8(4) . . ? N4 C40 C41 177.2(16) . . ? C51 C50 N5 172.4(16) . . ? C211 N2 C231 113.1(14) . . ? C211 N2 C221 110.3(11) . . ? C231 N2 C221 105.3(11) . . ? C211 N2 C241 107.9(9) . . ? C231 N2 C241 109.6(12) . . ? C221 N2 C241 110.7(11) . . ? C222 C221 N2 114.5(12) . . ? C212 C211 N2 112.9(9) . . ? C232 C231 N2 118.1(16) . . ? C331 N3 C341 109.1(13) . . ? C331 N3 C311 111.4(17) . . ? C341 N3 C311 107.3(11) . . ? C331 N3 C321 107.4(14) . . ? C341 N3 C321 109.5(16) . . ? C311 N3 C321 112.2(14) . . ? C312 C311 N3 114.8(12) . . ? N3 C331 C332 119(2) . . ? N3 C321 C322 112.5(17) . . ? C123 N1 C131 84.0(10) . . ? C123 N1 C113 109.6(10) . . ? C131 N1 C113 162.8(11) . . ? C123 N1 C141 109.5(12) . . ? C131 N1 C141 54.4(11) . . ? C113 N1 C141 109.8(12) . . ? C123 N1 C133 117.7(11) . . ? C131 N1 C133 71.7(12) . . ? C113 N1 C133 108.8(10) . . ? C141 N1 C133 101.0(14) . . ? C123 N1 C121 52.2(8) . . ? C131 N1 C121 114.7(12) . . ? C113 N1 C121 82.4(10) . . ? C141 N1 C121 161.5(12) . . ? C133 N1 C121 87.5(11) . . ? C123 N1 C142 159.1(10) . . ? C131 N1 C142 110.2(12) . . ? C113 N1 C142 60.0(9) . . ? C141 N1 C142 91.3(13) . . ? C133 N1 C142 56.6(10) . . ? C121 N1 C142 107.0(10) . . ? C123 N1 C111 79.3(11) . . ? C131 N1 C111 113.1(11) . . ? C113 N1 C111 61.5(8) . . ? C141 N1 C111 71.8(12) . . ? C133 N1 C111 162.9(11) . . ? C121 N1 C111 104.1(10) . . ? C142 N1 C111 107.3(12) . . ? N1 C113 C114 107.9(17) . . ? N1 C123 C122 117.3(15) . . ? C134 C133 N1 123(2) . . ? N1 C131 C132 116(2) . . ? C112 C111 N1 115.7(17) . . ? C124 C121 N1 120.9(14) . . ? C101 C106 C105 119.9(7) . . ? C101 C102 C103 118.1(7) . . ? C104 C105 C106 121.0(7) . . ? C103 C104 C105 119.5(6) . . ? C104 C103 C102 122.0(8) . . ? C201 C206 C205 120.6(5) . . ? C205 C204 C203 119.5(5) . . ? C204 C205 C206 120.4(5) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.327 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.088 # Attachment '765681_jd40.cif' data_jd40 _database_code_depnum_ccdc_archive 'CCDC 765681' #TrackingRef '765681_jd40.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C7 H18 N), B11 Ge H11 Te, C2 H3 N' _chemical_formula_sum 'C16 H50 B11 Ge N3 Te' _chemical_formula_weight 603.72 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4400(11) _cell_length_b 14.1849(8) _cell_length_c 16.2170(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.300(6) _cell_angle_gamma 90.00 _cell_volume 3090.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29073 _cell_measurement_theta_min 3.50 _cell_measurement_theta_max 59.19 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 1.927 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6978 _exptl_absorpt_correction_T_max 0.7715 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28402 _diffrn_reflns_av_R_equivalents 0.0852 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 5.68 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5453 _reflns_number_gt 4243 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep3 for windows' _computing_publication_material ? _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. The distance C234-C235 in the dissordered ethyl chain of a cation was corrected by using DFIX 1.5 ; _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^)+(0.0114P)^2^+5.3662P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5453 _refine_ls_number_parameters 310 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0710 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.0726 _refine_ls_wR_factor_gt 0.0677 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.181 _refine_ls_shift/su_max 0.002 _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 N1 N 0.4962(3) 0.4756(2) 0.28668(19) 0.0281(7) Uani 1 1 d . . . C111 C 0.4728(4) 0.5249(3) 0.2065(2) 0.0376(11) Uani 1 1 d . . . H11A H 0.5329 0.5331 0.1764 0.056 Uiso 1 1 calc R . . H11B H 0.4440 0.5854 0.2174 0.056 Uiso 1 1 calc R . . H11C H 0.4266 0.4877 0.1744 0.056 Uiso 1 1 calc R . . C131 C 0.3993(4) 0.4646(4) 0.3309(3) 0.0447(12) Uani 1 1 d . . . H13A H 0.3712 0.5268 0.3390 0.054 Uiso 1 1 calc R . . H13B H 0.3534 0.4300 0.2952 0.054 Uiso 1 1 calc R . . B109 B 0.2813(4) 0.2182(4) 0.9090(3) 0.0371(12) Uani 1 1 d . . . H109 H 0.2825 0.1615 0.8627 0.045 Uiso 1 1 calc R . . B110 B 0.1787(4) 0.2974(3) 0.9157(3) 0.0323(11) Uani 1 1 d . . . H110 H 0.1135 0.2921 0.8738 0.039 Uiso 1 1 calc R . . C121 C 0.5389(4) 0.3789(3) 0.2696(3) 0.0489(13) Uani 1 1 d . . . H12A H 0.5586 0.3504 0.3219 0.059 Uiso 1 1 calc R . . H12B H 0.4866 0.3400 0.2453 0.059 Uiso 1 1 calc R . . B106 B 0.2258(4) 0.4087(4) 0.9500(3) 0.0328(11) Uani 1 1 d . . . H106 H 0.1913 0.4756 0.9302 0.039 Uiso 1 1 calc R . . B108 B 0.3912(4) 0.2804(4) 0.9389(3) 0.0411(13) Uani 1 1 d . . . H108 H 0.4635 0.2642 0.9117 0.049 Uiso 1 1 calc R . . B107 B 0.3570(4) 0.3977(4) 0.9647(3) 0.0353(12) Uani 1 1 d . . . H107 H 0.4074 0.4575 0.9545 0.042 Uiso 1 1 calc R . . C132 C 0.4050(5) 0.4156(5) 0.4130(3) 0.0686(17) Uani 1 1 d . . . H13C H 0.3398 0.4124 0.4357 0.103 Uiso 1 1 calc R . . H13D H 0.4485 0.4500 0.4498 0.103 Uiso 1 1 calc R . . H13E H 0.4304 0.3529 0.4059 0.103 Uiso 1 1 calc R . . B111 B 0.2958(4) 0.3386(4) 0.8814(3) 0.0391(13) Uani 1 1 d . . . H111 H 0.3063 0.3600 0.8170 0.047 Uiso 1 1 calc R . . N2 N 0.4890(3) 0.0029(3) 0.2365(2) 0.0464(11) Uani 1 1 d . . . C222 C 0.4444(4) 0.0531(4) 0.3807(3) 0.0598(15) Uani 1 1 d . . . H22A H 0.3910 0.0499 0.4190 0.090 Uiso 1 1 calc R A . H22B H 0.4591 0.1179 0.3691 0.090 Uiso 1 1 calc R . . H22C H 0.5024 0.0231 0.4043 0.090 Uiso 1 1 calc R . . C221 C 0.4148(4) 0.0049(4) 0.3041(3) 0.0532(14) Uani 1 1 d . A . H22D H 0.3546 0.0347 0.2826 0.064 Uiso 1 1 calc R . . H22E H 0.3981 -0.0597 0.3176 0.064 Uiso 1 1 calc R . . C300 C 0.1933(5) 0.2519(6) 0.5272(4) 0.076(2) Uani 1 1 d . . . C122 C 0.6258(4) 0.3771(4) 0.2144(3) 0.0612(16) Uani 1 1 d . . . H12C H 0.6474 0.3132 0.2072 0.092 Uiso 1 1 calc R . . H12D H 0.6791 0.4136 0.2385 0.092 Uiso 1 1 calc R . . H12E H 0.6069 0.4034 0.1618 0.092 Uiso 1 1 calc R . . C301 C 0.1765(5) 0.1663(5) 0.4824(4) 0.0717(18) Uani 1 1 d . . . H30A H 0.1075 0.1492 0.4849 0.108 Uiso 1 1 calc R . . H30B H 0.2166 0.1169 0.5062 0.108 Uiso 1 1 calc R . . H30C H 0.1940 0.1752 0.4258 0.108 Uiso 1 1 calc R . . C211 C 0.5858(4) -0.0346(4) 0.2628(3) 0.0625(15) Uani 1 1 d . A . H21A H 0.6142 0.0058 0.3056 0.075 Uiso 1 1 calc R . . H21B H 0.6302 -0.0336 0.2165 0.075 Uiso 1 1 calc R . . C241 C 0.5109(5) 0.1075(4) 0.2083(4) 0.0730(18) Uani 1 1 d . A . H24A H 0.5404 0.1420 0.2535 0.110 Uiso 1 1 calc R . . H24B H 0.4497 0.1373 0.1912 0.110 Uiso 1 1 calc R . . H24C H 0.5557 0.1067 0.1631 0.110 Uiso 1 1 calc R . . N3 N 0.2066(6) 0.3210(6) 0.5627(5) 0.118(2) Uani 1 1 d . . . C212 C 0.5791(6) -0.1340(4) 0.2954(5) 0.107(3) Uani 1 1 d . . . H21C H 0.6442 -0.1554 0.3121 0.161 Uiso 1 1 calc R A . H21D H 0.5526 -0.1745 0.2529 0.161 Uiso 1 1 calc R . . H21E H 0.5361 -0.1352 0.3418 0.161 Uiso 1 1 calc R . . C141 C 0.5716(3) 0.5320(3) 0.3371(3) 0.0390(11) Uani 1 1 d . . . H14A H 0.5900 0.4961 0.3861 0.047 Uiso 1 1 calc R . . H14B H 0.6311 0.5397 0.3050 0.047 Uiso 1 1 calc R . . C142 C 0.5365(4) 0.6271(4) 0.3632(3) 0.0586(15) Uani 1 1 d . . . H14C H 0.5883 0.6580 0.3947 0.088 Uiso 1 1 calc R . . H14D H 0.4787 0.6203 0.3963 0.088 Uiso 1 1 calc R . . H14E H 0.5200 0.6641 0.3152 0.088 Uiso 1 1 calc R . . C232 C 0.4777(11) -0.0426(8) 0.0905(7) 0.082(5) Uani 0.562(14) 1 d P A 1 H23A H 0.4331 -0.0624 0.0468 0.122 Uiso 0.562(14) 1 calc PR A 1 H23B H 0.5275 -0.0901 0.1000 0.122 Uiso 0.562(14) 1 calc PR A 1 H23C H 0.5091 0.0155 0.0754 0.122 Uiso 0.562(14) 1 calc PR A 1 C236 C 0.4199(10) -0.0279(9) 0.1681(7) 0.053(3) Uani 0.562(14) 1 d P A 1 H23D H 0.3691 0.0196 0.1586 0.064 Uiso 0.562(14) 1 calc PR A 1 H23E H 0.3874 -0.0862 0.1833 0.064 Uiso 0.562(14) 1 calc PR A 1 C235 C 0.3749(11) -0.0500(11) 0.1168(8) 0.069(5) Uani 0.438(14) 1 d PD A 2 H23F H 0.3675 -0.0945 0.0724 0.104 Uiso 0.438(14) 1 calc PR A 2 H23G H 0.3748 0.0128 0.0948 0.104 Uiso 0.438(14) 1 calc PR A 2 H23H H 0.3206 -0.0570 0.1537 0.104 Uiso 0.438(14) 1 calc PR A 2 C234 C 0.4688(11) -0.0674(12) 0.1615(7) 0.045(4) Uani 0.438(14) 1 d PD A 2 H23I H 0.5230 -0.0621 0.1232 0.054 Uiso 0.438(14) 1 calc PR A 2 H23J H 0.4687 -0.1315 0.1824 0.054 Uiso 0.438(14) 1 calc PR A 2 Te1 Te 0.23698(2) 0.22877(2) 1.250798(17) 0.03806(10) Uani 1 1 d . . . Ge1 Ge 0.25839(3) 0.26462(3) 1.10472(2) 0.02876(12) Uani 1 1 d . . . B102 B 0.2782(4) 0.3990(3) 1.0505(3) 0.0274(10) Uani 1 1 d . . . H102 H 0.2777 0.4586 1.0939 0.033 Uiso 1 1 calc R . . B103 B 0.3856(4) 0.3156(4) 1.0437(3) 0.0328(11) Uani 1 1 d . . . H103 H 0.4532 0.3221 1.0828 0.039 Uiso 1 1 calc R . . B105 B 0.1988(4) 0.2101(3) 0.9918(3) 0.0327(11) Uani 1 1 d . . . H105 H 0.1482 0.1497 0.9979 0.039 Uiso 1 1 calc R . . B104 B 0.3371(4) 0.1995(4) 1.0077(3) 0.0379(12) Uani 1 1 d . . . H104 H 0.3740 0.1326 1.0241 0.045 Uiso 1 1 calc R . . B101 B 0.1622(4) 0.3337(3) 1.0187(3) 0.0287(10) Uani 1 1 d . . . H101 H 0.0883 0.3517 1.0418 0.034 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 N1 0.029(2) 0.0312(19) 0.0246(16) 0.0018(14) -0.0007(14) 0.0001(16) C111 0.042(3) 0.045(3) 0.026(2) 0.0049(19) -0.0045(19) 0.006(2) C131 0.038(3) 0.051(3) 0.046(3) 0.001(2) 0.006(2) -0.010(2) B109 0.036(3) 0.043(3) 0.032(2) -0.014(2) 0.001(2) 0.003(3) B110 0.033(3) 0.033(3) 0.031(2) -0.0050(19) -0.0056(19) -0.002(2) C121 0.062(4) 0.036(3) 0.049(3) 0.001(2) -0.006(2) 0.016(2) B106 0.042(3) 0.028(3) 0.028(2) 0.0012(19) -0.006(2) 0.001(2) B108 0.030(3) 0.058(4) 0.036(2) -0.013(3) 0.006(2) -0.003(3) B107 0.033(3) 0.043(3) 0.030(2) -0.002(2) 0.005(2) -0.011(2) C132 0.072(4) 0.087(5) 0.048(3) 0.011(3) 0.012(3) -0.024(3) B111 0.046(4) 0.047(3) 0.025(2) -0.004(2) 0.003(2) -0.011(3) N2 0.041(3) 0.064(3) 0.033(2) 0.0015(18) -0.0098(17) -0.018(2) C222 0.052(4) 0.061(4) 0.068(4) 0.004(3) 0.017(3) -0.007(3) C221 0.048(4) 0.049(3) 0.063(3) 0.021(3) 0.004(3) -0.007(3) C300 0.071(5) 0.077(6) 0.080(5) 0.026(4) 0.007(3) -0.008(4) C122 0.056(4) 0.075(4) 0.052(3) -0.015(3) -0.007(3) 0.030(3) C301 0.081(5) 0.078(5) 0.057(3) 0.022(3) 0.023(3) 0.026(4) C211 0.061(4) 0.071(4) 0.056(3) -0.004(3) 0.013(3) 0.008(3) C241 0.067(4) 0.072(4) 0.080(4) 0.028(3) -0.011(3) -0.010(3) N3 0.121(6) 0.098(6) 0.136(6) 0.022(5) 0.001(5) -0.031(5) C212 0.150(7) 0.040(4) 0.137(6) 0.013(4) 0.105(6) 0.015(4) C141 0.033(3) 0.048(3) 0.036(2) -0.001(2) -0.0017(19) -0.005(2) C142 0.072(4) 0.046(3) 0.057(3) -0.008(3) -0.009(3) -0.012(3) C232 0.128(14) 0.056(7) 0.059(8) -0.011(6) -0.021(7) 0.041(7) C236 0.054(9) 0.038(7) 0.067(8) 0.007(5) -0.011(6) 0.000(5) C235 0.076(12) 0.082(11) 0.049(8) 0.017(7) -0.017(7) -0.033(9) C234 0.059(11) 0.052(10) 0.025(6) -0.005(6) 0.000(6) -0.022(7) Te1 0.0497(2) 0.03688(16) 0.02762(13) 0.00573(13) 0.00144(12) -0.00560(16) Ge1 0.0317(3) 0.0294(2) 0.0252(2) 0.00008(19) 0.00092(18) 0.0011(2) B102 0.028(3) 0.028(3) 0.027(2) -0.0033(19) 0.0022(18) -0.002(2) B103 0.024(3) 0.044(3) 0.030(2) -0.008(2) 0.0013(19) 0.002(2) B105 0.031(3) 0.030(3) 0.036(2) -0.007(2) -0.001(2) -0.002(2) B104 0.034(3) 0.039(3) 0.041(3) -0.009(2) 0.001(2) 0.007(2) B101 0.024(3) 0.033(3) 0.029(2) -0.0049(19) -0.0034(19) 0.001(2) _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 N1 C111 1.504(5) . ? N1 C131 1.509(5) . ? N1 C121 1.514(6) . ? N1 C141 1.516(5) . ? C131 C132 1.503(7) . ? B109 B105 1.764(7) . ? B109 B104 1.772(7) . ? B109 B111 1.777(8) . ? B109 B108 1.779(7) . ? B109 B110 1.783(7) . ? B110 B105 1.764(7) . ? B110 B101 1.766(6) . ? B110 B111 1.780(7) . ? B110 B106 1.786(7) . ? C121 C122 1.488(7) . ? B106 B102 1.766(6) . ? B106 B101 1.774(7) . ? B106 B111 1.778(7) . ? B106 B107 1.780(7) . ? B108 B104 1.769(8) . ? B108 B111 1.772(8) . ? B108 B103 1.775(6) . ? B108 B107 1.779(8) . ? B107 B103 1.768(7) . ? B107 B102 1.768(6) . ? B107 B111 1.776(7) . ? N2 C211 1.460(7) . ? N2 C236 1.495(12) . ? N2 C221 1.499(6) . ? N2 C241 1.582(7) . ? N2 C234 1.592(13) . ? C222 C221 1.465(7) . ? C300 N3 1.150(9) . ? C300 C301 1.430(10) . ? C211 C212 1.509(8) . ? C141 C142 1.494(7) . ? C232 C236 1.508(18) . ? C235 C234 1.463(16) . ? Te1 Ge1 2.4462(5) . ? Ge1 B102 2.119(5) . ? Ge1 B101 2.121(5) . ? Ge1 B103 2.122(5) . ? Ge1 B104 2.128(5) . ? Ge1 B105 2.128(5) . ? B102 B103 1.872(7) . ? B102 B101 1.876(7) . ? B103 B104 1.860(7) . ? B105 B101 1.875(7) . ? B105 B104 1.876(7) . ? 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 C111 N1 C131 107.0(3) . . ? C111 N1 C121 109.6(3) . . ? C131 N1 C121 109.1(4) . . ? C111 N1 C141 110.2(3) . . ? C131 N1 C141 111.8(3) . . ? C121 N1 C141 108.9(3) . . ? C132 C131 N1 116.2(4) . . ? B105 B109 B104 64.1(3) . . ? B105 B109 B111 109.2(3) . . ? B104 B109 B111 109.0(4) . . ? B105 B109 B108 110.9(3) . . ? B104 B109 B108 59.8(3) . . ? B111 B109 B108 59.8(3) . . ? B105 B109 B110 59.7(3) . . ? B104 B109 B110 110.6(3) . . ? B111 B109 B110 60.0(3) . . ? B108 B109 B110 108.0(4) . . ? B105 B110 B101 64.2(3) . . ? B105 B110 B111 109.1(4) . . ? B101 B110 B111 109.3(3) . . ? B105 B110 B109 59.6(3) . . ? B101 B110 B109 110.8(3) . . ? B111 B110 B109 59.8(3) . . ? B105 B110 B106 110.8(3) . . ? B101 B110 B106 59.9(3) . . ? B111 B110 B106 59.8(3) . . ? B109 B110 B106 107.9(4) . . ? C122 C121 N1 115.5(4) . . ? B102 B106 B101 64.0(3) . . ? B102 B106 B111 109.2(4) . . ? B101 B106 B111 109.1(4) . . ? B102 B106 B107 59.8(3) . . ? B101 B106 B107 110.7(3) . . ? B111 B106 B107 59.9(3) . . ? B102 B106 B110 110.5(3) . . ? B101 B106 B110 59.5(3) . . ? B111 B106 B110 59.9(3) . . ? B107 B106 B110 107.9(4) . . ? B104 B108 B111 109.3(4) . . ? B104 B108 B103 63.3(3) . . ? B111 B108 B103 109.1(4) . . ? B104 B108 B107 110.3(3) . . ? B111 B108 B107 60.0(3) . . ? B103 B108 B107 59.7(3) . . ? B104 B108 B109 59.9(3) . . ? B111 B108 B109 60.0(3) . . ? B103 B108 B109 110.3(3) . . ? B107 B108 B109 108.1(4) . . ? B103 B107 B102 63.9(3) . . ? B103 B107 B111 109.2(4) . . ? B102 B107 B111 109.2(4) . . ? B103 B107 B108 60.0(3) . . ? B102 B107 B108 111.0(4) . . ? B111 B107 B108 59.8(3) . . ? B103 B107 B106 110.7(3) . . ? B102 B107 B106 59.7(3) . . ? B111 B107 B106 60.0(3) . . ? B108 B107 B106 108.1(4) . . ? B108 B111 B107 60.2(3) . . ? B108 B111 B109 60.2(3) . . ? B107 B111 B109 108.3(4) . . ? B108 B111 B106 108.6(3) . . ? B107 B111 B106 60.1(3) . . ? B109 B111 B106 108.5(3) . . ? B108 B111 B110 108.5(4) . . ? B107 B111 B110 108.3(3) . . ? B109 B111 B110 60.2(3) . . ? B106 B111 B110 60.3(3) . . ? C211 N2 C236 130.1(7) . . ? C211 N2 C221 113.3(4) . . ? C236 N2 C221 97.8(6) . . ? C211 N2 C241 104.8(4) . . ? C236 N2 C241 100.2(6) . . ? C221 N2 C241 109.0(4) . . ? C211 N2 C234 97.5(7) . . ? C236 N2 C234 32.6(5) . . ? C221 N2 C234 117.8(6) . . ? C241 N2 C234 113.4(6) . . ? C222 C221 N2 117.2(4) . . ? N3 C300 C301 179.5(8) . . ? N2 C211 C212 112.5(6) . . ? C142 C141 N1 114.7(4) . . ? N2 C236 C232 109.7(10) . . ? C235 C234 N2 113.8(13) . . ? B102 Ge1 B101 52.53(18) . . ? B102 Ge1 B103 52.40(19) . . ? B101 Ge1 B103 91.22(19) . . ? B102 Ge1 B104 90.84(19) . . ? B101 Ge1 B104 91.13(19) . . ? B103 Ge1 B104 51.92(19) . . ? B102 Ge1 B105 91.06(18) . . ? B101 Ge1 B105 52.39(18) . . ? B103 Ge1 B105 90.78(19) . . ? B104 Ge1 B105 52.33(19) . . ? B102 Ge1 Te1 127.41(12) . . ? B101 Ge1 Te1 130.54(13) . . ? B103 Ge1 Te1 129.52(13) . . ? B104 Ge1 Te1 134.23(15) . . ? B105 Ge1 Te1 135.05(14) . . ? B106 B102 B107 60.5(3) . . ? B106 B102 B103 106.6(3) . . ? B107 B102 B103 58.0(3) . . ? B106 B102 B101 58.2(3) . . ? B107 B102 B101 106.7(3) . . ? B103 B102 B101 108.0(3) . . ? B106 B102 Ge1 113.7(3) . . ? B107 B102 Ge1 113.6(3) . . ? B103 B102 Ge1 63.9(2) . . ? B101 B102 Ge1 63.8(2) . . ? B107 B103 B108 60.3(3) . . ? B107 B103 B104 106.7(3) . . ? B108 B103 B104 58.2(3) . . ? B107 B103 B102 58.0(3) . . ? B108 B103 B102 106.5(3) . . ? B104 B103 B102 108.3(3) . . ? B107 B103 Ge1 113.5(3) . . ? B108 B103 Ge1 113.8(3) . . ? B104 B103 Ge1 64.2(2) . . ? B102 B103 Ge1 63.7(2) . . ? B109 B105 B110 60.7(3) . . ? B109 B105 B101 106.8(3) . . ? B110 B105 B101 58.0(2) . . ? B109 B105 B104 58.2(3) . . ? B110 B105 B104 106.7(4) . . ? B101 B105 B104 107.9(3) . . ? B109 B105 Ge1 113.6(3) . . ? B110 B105 Ge1 113.3(3) . . ? B101 B105 Ge1 63.61(19) . . ? B104 B105 Ge1 63.8(2) . . ? B108 B104 B109 60.3(3) . . ? B108 B104 B103 58.5(3) . . ? B109 B104 B103 106.8(4) . . ? B108 B104 B105 106.4(4) . . ? B109 B104 B105 57.7(3) . . ? B103 B104 B105 108.1(3) . . ? B108 B104 Ge1 113.8(3) . . ? B109 B104 Ge1 113.3(3) . . ? B103 B104 Ge1 63.9(2) . . ? B105 B104 Ge1 63.8(2) . . ? B110 B101 B106 60.6(3) . . ? B110 B101 B105 57.9(3) . . ? B106 B101 B105 106.4(3) . . ? B110 B101 B102 106.4(3) . . ? B106 B101 B102 57.8(2) . . ? B105 B101 B102 107.8(3) . . ? B110 B101 Ge1 113.5(3) . . ? B106 B101 Ge1 113.2(3) . . ? B105 B101 Ge1 64.0(2) . . ? B102 B101 Ge1 63.7(2) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.775 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.077 # Attachment '765682_substituted_jd90.cif' data_jd90 _database_code_depnum_ccdc_archive 'CCDC 765682' #TrackingRef '765682_substituted_jd90.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C8 H20 N), B11 Ge H11 Se, C2 H3 N' _chemical_formula_sum 'C18 H54 B11 Ge1 N3 Se1' _chemical_formula_weight 583.14 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.1594(5) _cell_length_b 14.6085(9) _cell_length_c 21.6075(13) _cell_angle_alpha 90.00 _cell_angle_beta 97.115(4) _cell_angle_gamma 90.00 _cell_volume 3182.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29811 _cell_measurement_theta_min 4.31 _cell_measurement_theta_max 59.27 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216 _exptl_absorpt_coefficient_mu 2.120 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5759 _exptl_absorpt_correction_T_max 0.7981 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40249 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 5.67 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5768 _reflns_number_gt 5303 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep for windows' _computing_publication_material ? _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. Due to moderate crystal quality the R(int) has a value >0.1 ; _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^)+(0.0279P)^2^+1.9131P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5768 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.0421 _refine_ls_wR_factor_ref 0.0906 _refine_ls_wR_factor_gt 0.0884 _refine_ls_goodness_of_fit_ref 1.188 _refine_ls_restrained_S_all 1.188 _refine_ls_shift/su_max 0.002 _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 Se1 Se 0.94311(3) 0.70572(2) 0.490996(13) 0.03150(10) Uani 1 1 d . . . Ge1 Ge 0.81476(3) 0.759362(19) 0.559346(12) 0.02380(9) Uani 1 1 d . . . N1 N 0.7927(2) 0.94295(14) 0.34839(9) 0.0219(4) Uani 1 1 d . . . N2 N 0.7602(2) 0.46631(15) 0.37799(11) 0.0272(5) Uani 1 1 d . . . C121 C 0.8958(3) 0.9964(2) 0.39025(13) 0.0320(6) Uani 1 1 d . . . H12A H 0.9495 0.9534 0.4167 0.038 Uiso 1 1 calc R . . H12B H 0.9537 1.0269 0.3643 0.038 Uiso 1 1 calc R . . B107 B 0.7614(3) 0.8044(2) 0.70167(14) 0.0278(7) Uani 1 1 d . . . H107 H 0.8020 0.7979 0.7511 0.033 Uiso 1 1 calc R . . C221 C 0.9068(3) 0.4893(2) 0.39066(14) 0.0342(6) Uani 1 1 d . . . H22A H 0.9207 0.5268 0.4279 0.041 Uiso 1 1 calc R . . H22B H 0.9556 0.4328 0.3995 0.041 Uiso 1 1 calc R . . C131 C 0.7222(3) 0.8793(2) 0.38918(13) 0.0324(6) Uani 1 1 d . . . H13A H 0.7887 0.8431 0.4144 0.039 Uiso 1 1 calc R . . H13B H 0.6776 0.9164 0.4174 0.039 Uiso 1 1 calc R . . C141 C 0.6909(3) 1.0052(2) 0.31296(14) 0.0321(6) Uani 1 1 d . . . H14A H 0.6275 0.9676 0.2870 0.039 Uiso 1 1 calc R . . H14B H 0.6429 1.0366 0.3428 0.039 Uiso 1 1 calc R . . C111 C 0.8622(3) 0.8900(2) 0.30168(13) 0.0310(6) Uani 1 1 d . . . H11A H 0.7965 0.8538 0.2760 0.037 Uiso 1 1 calc R . . H11B H 0.8989 0.9335 0.2745 0.037 Uiso 1 1 calc R . . B102 B 0.7832(3) 0.7140(2) 0.64959(14) 0.0262(6) Uani 1 1 d . . . H102 H 0.8357 0.6507 0.6655 0.031 Uiso 1 1 calc R . . B101 B 0.6342(3) 0.7143(2) 0.58909(15) 0.0289(7) Uani 1 1 d . . . H101 H 0.5924 0.6515 0.5665 0.035 Uiso 1 1 calc R . . B106 B 0.6227(3) 0.7379(2) 0.66851(15) 0.0292(7) Uani 1 1 d . . . H106 H 0.5732 0.6884 0.6962 0.035 Uiso 1 1 calc R . . B105 B 0.6279(3) 0.8275(2) 0.54814(15) 0.0318(7) Uani 1 1 d . . . H105 H 0.5821 0.8363 0.4997 0.038 Uiso 1 1 calc R . . C231 C 0.6816(3) 0.5548(2) 0.37057(17) 0.0410(7) Uani 1 1 d . . . H23A H 0.7113 0.5944 0.4056 0.049 Uiso 1 1 calc R . . H23B H 0.7017 0.5853 0.3330 0.049 Uiso 1 1 calc R . . C122 C 0.8420(3) 1.0669(2) 0.43125(14) 0.0408(7) Uani 1 1 d . . . H12C H 0.9143 1.0972 0.4558 0.061 Uiso 1 1 calc R . . H12D H 0.7869 1.0375 0.4583 0.061 Uiso 1 1 calc R . . H12E H 0.7905 1.1110 0.4057 0.061 Uiso 1 1 calc R . . B103 B 0.8695(3) 0.8263(2) 0.64557(14) 0.0250(6) Uani 1 1 d . . . H103 H 0.9770 0.8341 0.6588 0.030 Uiso 1 1 calc R . . B111 B 0.6075(3) 0.8584(2) 0.67872(15) 0.0336(7) Uani 1 1 d . . . H111 H 0.5481 0.8869 0.7134 0.040 Uiso 1 1 calc R . . C142 C 0.7460(3) 1.0760(2) 0.27212(16) 0.0433(8) Uani 1 1 d . . . H14C H 0.6746 1.1122 0.2516 0.065 Uiso 1 1 calc R . . H14D H 0.7913 1.0458 0.2414 0.065 Uiso 1 1 calc R . . H14E H 0.8070 1.1149 0.2974 0.065 Uiso 1 1 calc R . . C132 C 0.6221(4) 0.8150(2) 0.35533(17) 0.0498(9) Uani 1 1 d . . . H13C H 0.5833 0.7782 0.3851 0.075 Uiso 1 1 calc R . . H13D H 0.6653 0.7762 0.3282 0.075 Uiso 1 1 calc R . . H13E H 0.5540 0.8498 0.3311 0.075 Uiso 1 1 calc R . . C222 C 0.9645(3) 0.5381(2) 0.33946(16) 0.0453(8) Uani 1 1 d . . . H22C H 1.0571 0.5491 0.3519 0.068 Uiso 1 1 calc R . . H22D H 0.9196 0.5955 0.3312 0.068 Uiso 1 1 calc R . . H22E H 0.9537 0.5012 0.3024 0.068 Uiso 1 1 calc R . . C211 C 0.7242(3) 0.4101(2) 0.43265(16) 0.0440(8) Uani 1 1 d . . . H21A H 0.6346 0.3872 0.4222 0.053 Uiso 1 1 calc R . . H21B H 0.7830 0.3576 0.4380 0.053 Uiso 1 1 calc R . . B104 B 0.7741(3) 0.8966(2) 0.58305(14) 0.0281(7) Uani 1 1 d . . . H104 H 0.8210 0.9491 0.5566 0.034 Uiso 1 1 calc R . . B108 B 0.7561(3) 0.9118(2) 0.66279(15) 0.0313(7) Uani 1 1 d . . . H108 H 0.7931 0.9749 0.6868 0.038 Uiso 1 1 calc R . . C241 C 0.7296(3) 0.4111(2) 0.31860(16) 0.0429(8) Uani 1 1 d . . . H24A H 0.6363 0.3949 0.3138 0.051 Uiso 1 1 calc R . . H24B H 0.7444 0.4496 0.2835 0.051 Uiso 1 1 calc R . . C112 C 0.9715(3) 0.8274(2) 0.32907(16) 0.0427(8) Uani 1 1 d . . . H11C H 1.0093 0.7969 0.2961 0.064 Uiso 1 1 calc R . . H11D H 0.9362 0.7827 0.3551 0.064 Uiso 1 1 calc R . . H11E H 1.0389 0.8625 0.3535 0.064 Uiso 1 1 calc R . . B109 B 0.6136(3) 0.9125(2) 0.60539(15) 0.0330(7) Uani 1 1 d . . . H109 H 0.5584 0.9758 0.5924 0.040 Uiso 1 1 calc R . . B110 B 0.5323(3) 0.8051(2) 0.60911(16) 0.0333(7) Uani 1 1 d . . . H110 H 0.4239 0.7991 0.5985 0.040 Uiso 1 1 calc R . . C232 C 0.5337(3) 0.5436(3) 0.3669(2) 0.0583(10) Uani 1 1 d . . . H23C H 0.4920 0.6026 0.3625 0.087 Uiso 1 1 calc R . . H23D H 0.5121 0.5149 0.4043 0.087 Uiso 1 1 calc R . . H23E H 0.5024 0.5063 0.3316 0.087 Uiso 1 1 calc R . . C212 C 0.7318(4) 0.4600(3) 0.49374(17) 0.0619(11) Uani 1 1 d . . . H21C H 0.7073 0.4193 0.5253 0.093 Uiso 1 1 calc R . . H21D H 0.6721 0.5113 0.4896 0.093 Uiso 1 1 calc R . . H21E H 0.8207 0.4815 0.5054 0.093 Uiso 1 1 calc R . . C242 C 0.8096(4) 0.3248(3) 0.3157(2) 0.0603(10) Uani 1 1 d . . . H24C H 0.7836 0.2943 0.2768 0.090 Uiso 1 1 calc R . . H24D H 0.7941 0.2851 0.3495 0.090 Uiso 1 1 calc R . . H24E H 0.9022 0.3399 0.3191 0.090 Uiso 1 1 calc R . . C30 C 0.2817(4) 0.7606(3) 0.39557(18) 0.0507(9) Uani 1 1 d . . . C31 C 0.2763(4) 0.8224(3) 0.44679(18) 0.0571(10) Uani 1 1 d . . . H31A H 0.2848 0.8842 0.4327 0.086 Uiso 1 1 calc R . . H31B H 0.3475 0.8090 0.4790 0.086 Uiso 1 1 calc R . . H31C H 0.1930 0.8154 0.4629 0.086 Uiso 1 1 calc R . . N3 N 0.2835(4) 0.7123(3) 0.3552(2) 0.0939(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.03367(17) 0.03528(17) 0.02660(16) 0.00009(11) 0.00792(11) 0.00596(12) Ge1 0.02425(16) 0.02577(16) 0.02160(15) 0.00157(11) 0.00379(11) -0.00007(11) N1 0.0252(11) 0.0224(10) 0.0184(10) 0.0003(8) 0.0038(9) 0.0003(9) N2 0.0257(12) 0.0258(11) 0.0301(12) 0.0028(9) 0.0035(9) 0.0013(9) C121 0.0339(15) 0.0323(15) 0.0287(14) -0.0016(12) 0.0003(12) -0.0046(12) B107 0.0339(17) 0.0279(16) 0.0210(15) 0.0028(12) 0.0014(12) -0.0010(13) C221 0.0279(15) 0.0354(15) 0.0387(16) 0.0017(13) 0.0019(12) -0.0003(12) C131 0.0389(16) 0.0308(15) 0.0295(15) 0.0068(12) 0.0123(12) -0.0021(12) C141 0.0304(15) 0.0346(15) 0.0309(15) 0.0041(12) 0.0021(12) 0.0038(12) C111 0.0373(16) 0.0325(15) 0.0250(14) -0.0030(12) 0.0110(12) 0.0001(12) B102 0.0292(16) 0.0233(14) 0.0261(15) 0.0019(12) 0.0031(12) -0.0017(12) B101 0.0275(16) 0.0340(17) 0.0253(15) 0.0017(13) 0.0041(12) -0.0079(13) B106 0.0294(16) 0.0331(16) 0.0256(16) 0.0043(13) 0.0058(13) -0.0030(13) B105 0.0274(16) 0.0408(18) 0.0269(16) 0.0051(14) 0.0021(13) 0.0025(14) C231 0.0419(18) 0.0304(15) 0.0504(19) 0.0059(14) 0.0047(15) 0.0093(13) C122 0.055(2) 0.0341(16) 0.0342(16) -0.0090(13) 0.0075(14) -0.0062(14) B103 0.0252(15) 0.0234(14) 0.0259(15) 0.0017(12) 0.0011(12) -0.0015(12) B111 0.0341(18) 0.0420(19) 0.0260(16) 0.0041(14) 0.0087(13) 0.0076(15) C142 0.0407(18) 0.0423(18) 0.0463(19) 0.0178(15) 0.0027(15) 0.0025(14) C132 0.059(2) 0.049(2) 0.0447(19) -0.0026(16) 0.0166(17) -0.0219(17) C222 0.0375(17) 0.0485(19) 0.052(2) 0.0062(16) 0.0142(15) -0.0038(15) C211 0.0427(18) 0.0414(18) 0.0501(19) 0.0159(15) 0.0143(15) 0.0032(15) B104 0.0304(16) 0.0281(15) 0.0263(15) 0.0061(12) 0.0053(13) -0.0003(13) B108 0.0415(19) 0.0258(15) 0.0269(16) 0.0017(13) 0.0054(14) 0.0021(14) C241 0.0427(18) 0.0418(18) 0.0435(18) -0.0084(15) 0.0030(15) -0.0068(14) C112 0.0403(18) 0.0445(18) 0.0447(18) -0.0031(15) 0.0104(14) 0.0135(15) B109 0.0329(17) 0.0358(18) 0.0313(17) 0.0094(14) 0.0076(14) 0.0094(14) B110 0.0259(16) 0.0448(19) 0.0294(16) 0.0049(14) 0.0038(13) 0.0013(14) C232 0.0348(18) 0.053(2) 0.088(3) 0.012(2) 0.0082(19) 0.0139(16) C212 0.072(3) 0.078(3) 0.040(2) 0.0088(19) 0.0223(19) 0.000(2) C242 0.070(3) 0.042(2) 0.072(3) -0.0170(19) 0.022(2) -0.0018(18) C30 0.0381(19) 0.062(2) 0.051(2) -0.0153(18) -0.0007(16) 0.0149(17) C31 0.049(2) 0.072(3) 0.049(2) -0.0219(19) 0.0004(17) -0.0034(19) N3 0.080(3) 0.109(3) 0.087(3) -0.055(3) -0.011(2) 0.044(2) _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 Se1 Ge1 2.2299(4) . ? Ge1 B103 2.116(3) . ? Ge1 B102 2.121(3) . ? Ge1 B101 2.122(3) . ? Ge1 B104 2.123(3) . ? Ge1 B105 2.131(3) . ? N1 C141 1.512(3) . ? N1 C121 1.513(3) . ? N1 C111 1.514(3) . ? N1 C131 1.520(3) . ? N2 C241 1.515(4) . ? N2 C231 1.517(4) . ? N2 C221 1.518(3) . ? N2 C211 1.520(4) . ? C121 C122 1.505(4) . ? B107 B103 1.763(4) . ? B107 B102 1.767(4) . ? B107 B111 1.767(5) . ? B107 B108 1.778(4) . ? B107 B106 1.787(5) . ? C221 C222 1.496(4) . ? C131 C132 1.505(4) . ? C141 C142 1.511(4) . ? C111 C112 1.503(4) . ? B102 B106 1.764(5) . ? B102 B103 1.867(4) . ? B102 B101 1.874(4) . ? B101 B106 1.768(4) . ? B101 B110 1.769(5) . ? B101 B105 1.873(5) . ? B106 B110 1.779(5) . ? B106 B111 1.783(5) . ? B105 B110 1.762(5) . ? B105 B109 1.771(5) . ? B105 B104 1.875(5) . ? C231 C232 1.504(5) . ? B103 B108 1.771(4) . ? B103 B104 1.870(4) . ? B111 B108 1.771(5) . ? B111 B109 1.779(4) . ? B111 B110 1.780(5) . ? C211 C212 1.502(5) . ? B104 B108 1.769(4) . ? B104 B109 1.772(5) . ? B108 B109 1.786(5) . ? C241 C242 1.506(5) . ? B109 B110 1.780(5) . ? C30 N3 1.124(5) . ? C30 C31 1.435(5) . ? 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 B103 Ge1 B102 52.29(11) . . ? B103 Ge1 B101 91.11(12) . . ? B102 Ge1 B101 52.41(12) . . ? B103 Ge1 B104 52.35(12) . . ? B102 Ge1 B104 91.00(12) . . ? B101 Ge1 B104 91.06(13) . . ? B103 Ge1 B105 91.00(12) . . ? B102 Ge1 B105 90.95(12) . . ? B101 Ge1 B105 52.26(13) . . ? B104 Ge1 B105 52.31(13) . . ? B103 Ge1 Se1 129.33(9) . . ? B102 Ge1 Se1 131.78(9) . . ? B101 Ge1 Se1 133.63(9) . . ? B104 Ge1 Se1 129.71(9) . . ? B105 Ge1 Se1 132.44(9) . . ? C141 N1 C121 111.9(2) . . ? C141 N1 C111 108.4(2) . . ? C121 N1 C111 108.4(2) . . ? C141 N1 C131 108.7(2) . . ? C121 N1 C131 108.0(2) . . ? C111 N1 C131 111.5(2) . . ? C241 N2 C231 108.3(2) . . ? C241 N2 C221 111.4(2) . . ? C231 N2 C221 108.8(2) . . ? C241 N2 C211 109.1(2) . . ? C231 N2 C211 111.6(2) . . ? C221 N2 C211 107.7(2) . . ? C122 C121 N1 115.5(2) . . ? B103 B107 B102 63.88(18) . . ? B103 B107 B111 109.3(2) . . ? B102 B107 B111 109.4(2) . . ? B103 B107 B108 60.01(18) . . ? B102 B107 B108 111.0(2) . . ? B111 B107 B108 59.93(19) . . ? B103 B107 B106 110.5(2) . . ? B102 B107 B106 59.54(18) . . ? B111 B107 B106 60.24(19) . . ? B108 B107 B106 108.3(2) . . ? C222 C221 N2 115.9(2) . . ? C132 C131 N1 116.0(2) . . ? C142 C141 N1 115.3(2) . . ? C112 C111 N1 115.6(2) . . ? B106 B102 B107 60.79(18) . . ? B106 B102 B103 106.8(2) . . ? B107 B102 B103 57.95(16) . . ? B106 B102 B101 58.06(17) . . ? B107 B102 B101 106.7(2) . . ? B103 B102 B101 108.0(2) . . ? B106 B102 Ge1 113.59(19) . . ? B107 B102 Ge1 113.38(18) . . ? B103 B102 Ge1 63.72(13) . . ? B101 B102 Ge1 63.83(13) . . ? B106 B101 B110 60.38(19) . . ? B106 B101 B105 106.5(2) . . ? B110 B101 B105 57.77(18) . . ? B106 B101 B102 57.86(17) . . ? B110 B101 B102 106.2(2) . . ? B105 B101 B102 108.0(2) . . ? B106 B101 Ge1 113.37(19) . . ? B110 B101 Ge1 113.3(2) . . ? B105 B101 Ge1 64.10(14) . . ? B102 B101 Ge1 63.77(13) . . ? B102 B106 B101 64.07(18) . . ? B102 B106 B110 110.6(2) . . ? B101 B106 B110 59.82(19) . . ? B102 B106 B111 108.7(2) . . ? B101 B106 B111 109.2(2) . . ? B110 B106 B111 59.95(19) . . ? B102 B106 B107 59.67(18) . . ? B101 B106 B107 110.6(2) . . ? B110 B106 B107 107.5(2) . . ? B111 B106 B107 59.34(18) . . ? B110 B105 B109 60.50(19) . . ? B110 B105 B101 58.14(18) . . ? B109 B105 B101 106.9(2) . . ? B110 B105 B104 106.4(2) . . ? B109 B105 B104 58.08(18) . . ? B101 B105 B104 107.8(2) . . ? B110 B105 Ge1 113.2(2) . . ? B109 B105 Ge1 113.4(2) . . ? B101 B105 Ge1 63.64(14) . . ? B104 B105 Ge1 63.62(14) . . ? C232 C231 N2 115.0(3) . . ? B107 B103 B108 60.42(18) . . ? B107 B103 B102 58.16(17) . . ? B108 B103 B102 106.8(2) . . ? B107 B103 B104 106.6(2) . . ? B108 B103 B104 58.07(17) . . ? B102 B103 B104 108.2(2) . . ? B107 B103 Ge1 113.78(18) . . ? B108 B103 Ge1 113.83(19) . . ? B102 B103 Ge1 63.99(13) . . ? B104 B103 Ge1 63.99(14) . . ? B107 B111 B108 60.35(18) . . ? B107 B111 B109 108.7(2) . . ? B108 B111 B109 60.41(19) . . ? B107 B111 B110 108.3(2) . . ? B108 B111 B110 108.4(2) . . ? B109 B111 B110 60.02(19) . . ? B107 B111 B106 60.43(18) . . ? B108 B111 B106 108.8(2) . . ? B109 B111 B106 108.4(2) . . ? B110 B111 B106 59.89(19) . . ? C212 C211 N2 115.5(3) . . ? B108 B104 B109 60.56(19) . . ? B108 B104 B103 58.15(17) . . ? B109 B104 B103 106.7(2) . . ? B108 B104 B105 106.7(2) . . ? B109 B104 B105 58.03(18) . . ? B103 B104 B105 108.0(2) . . ? B108 B104 Ge1 113.60(19) . . ? B109 B104 Ge1 113.7(2) . . ? B103 B104 Ge1 63.66(13) . . ? B105 B104 Ge1 64.06(15) . . ? B104 B108 B103 63.77(18) . . ? B104 B108 B111 109.1(2) . . ? B103 B108 B111 108.8(2) . . ? B104 B108 B107 110.4(2) . . ? B103 B108 B107 59.57(17) . . ? B111 B108 B107 59.72(18) . . ? B104 B108 B109 59.81(18) . . ? B103 B108 B109 110.5(2) . . ? B111 B108 B109 60.02(19) . . ? B107 B108 B109 107.9(2) . . ? C242 C241 N2 115.2(3) . . ? B105 B109 B104 63.89(19) . . ? B105 B109 B111 109.0(2) . . ? B104 B109 B111 108.6(2) . . ? B105 B109 B110 59.48(19) . . ? B104 B109 B110 110.1(2) . . ? B111 B109 B110 60.01(19) . . ? B105 B109 B108 110.6(2) . . ? B104 B109 B108 59.63(18) . . ? B111 B109 B108 59.57(19) . . ? B110 B109 B108 107.7(2) . . ? B105 B110 B101 64.09(19) . . ? B105 B110 B106 111.0(2) . . ? B101 B110 B106 59.80(18) . . ? B105 B110 B111 109.4(2) . . ? B101 B110 B111 109.4(2) . . ? B106 B110 B111 60.15(19) . . ? B105 B110 B109 60.02(19) . . ? B101 B110 B109 111.2(2) . . ? B106 B110 B109 108.6(2) . . ? B111 B110 B109 59.96(19) . . ? N3 C30 C31 178.7(4) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.316 _refine_diff_density_min -0.675 _refine_diff_density_rms 0.069 # Attachment '765683_jd45.cif' data_jd45 _database_code_depnum_ccdc_archive 'CCDC 765683' #TrackingRef '765683_jd45.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H48 B22 Ge2 P2 Pd S2, 2(C7 H18 N), 2(C2 H3 N)' _chemical_formula_sum 'C45 H90 B22 Ge2 N4 P2 Pd S2' _chemical_formula_weight 1302.67 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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' Pd Pd -0.9988 1.0072 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1903(11) _cell_length_b 12.6501(10) _cell_length_c 24.7573(19) _cell_angle_alpha 76.972(6) _cell_angle_beta 82.111(7) _cell_angle_gamma 63.939(6) _cell_volume 3338.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28925 _cell_measurement_theta_min 3.41 _cell_measurement_theta_max 59.18 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 1.306 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7644 _exptl_absorpt_correction_T_max 0.8622 _exptl_absorpt_process_details 'x-red, x-shape' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS 2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35498 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 5.67 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12061 _reflns_number_gt 9611 _reflns_threshold_expression >2sigma(I) _computing_data_collection x-Area _computing_cell_refinement x-Area _computing_data_reduction x-Area _computing_structure_solution 'ShelXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ortep for windows' _computing_publication_material ? _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. In order to attempt more appropriate values for the thermal ellipsoids and the geometry of the serve disordered cations, the restraint DFIX was used. The pheny rings C301-C306 and C401-C406 was treated with EADP constraint. Because of the very serve disorder of the cation N2, C211, C212, c221, C222, C231,C232, c241 we were not able to attempt anisotropic refinement. So in this extreme case this cation was refined isotropically. ; _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^)+(0.0572P)^2^+17.5793P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens calculated _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12061 _refine_ls_number_parameters 669 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0682 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1527 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.086 _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 Pd1 Pd 0.10780(4) 0.43350(4) 0.742374(18) 0.02196(13) Uani 1 1 d . . . Ge1 Ge -0.16571(5) 0.69630(5) 0.70025(3) 0.02452(16) Uani 1 1 d . . . Ge2 Ge 0.13439(6) 0.65842(6) 0.79297(3) 0.03189(17) Uani 1 1 d . . . P2 P 0.06042(14) 0.27344(13) 0.76744(7) 0.0268(3) Uani 1 1 d . . . P1 P 0.29901(14) 0.32271(14) 0.70897(7) 0.0271(3) Uani 1 1 d . . . S2 S 0.14984(13) 0.60419(13) 0.71547(6) 0.0268(3) Uani 1 1 d . . . S1 S -0.09964(13) 0.54783(13) 0.76776(6) 0.0284(3) Uani 1 1 d . . . C401 C 0.2880(8) 0.3373(7) 0.6347(3) 0.0509(8) Uani 1 1 d . . . C1 C 0.3698(6) 0.1631(6) 0.7378(3) 0.0341(14) Uani 1 1 d . . . H1A H 0.4434 0.1261 0.7155 0.041 Uiso 1 1 calc R . . H1B H 0.3945 0.1533 0.7748 0.041 Uiso 1 1 calc R . . C406 C 0.1972(8) 0.4382(7) 0.6065(3) 0.0509(8) Uani 1 1 d . . . H406 H 0.1443 0.4981 0.6256 0.061 Uiso 1 1 calc R . . B105 B -0.3443(6) 0.7578(6) 0.6712(3) 0.0305(15) Uani 1 1 d . . . H105 H -0.3971 0.7069 0.6915 0.037 Uiso 1 1 calc R . . B110 B -0.4151(6) 0.9147(6) 0.6498(3) 0.0320(16) Uani 1 1 d . . . H110 H -0.5143 0.9630 0.6572 0.038 Uiso 1 1 calc R . . B106 B -0.3130(7) 0.9800(6) 0.6530(3) 0.0345(16) Uani 1 1 d . . . H106 H -0.3463 1.0704 0.6622 0.041 Uiso 1 1 calc R . . C3 C 0.1877(6) 0.1264(5) 0.7859(3) 0.0369(15) Uani 1 1 d . . . H3A H 0.2208 0.1238 0.8199 0.044 Uiso 1 1 calc R . . H3B H 0.1565 0.0657 0.7934 0.044 Uiso 1 1 calc R . . B102 B -0.1690(6) 0.8676(6) 0.6762(3) 0.0313(15) Uani 1 1 d . . . H102 H -0.1110 0.8859 0.6998 0.038 Uiso 1 1 calc R . . C2 C 0.2915(6) 0.0951(6) 0.7412(3) 0.0339(14) Uani 1 1 d . . . H2A H 0.3431 0.0098 0.7492 0.041 Uiso 1 1 calc R . . H2B H 0.2567 0.1133 0.7055 0.041 Uiso 1 1 calc R . . C405 C 0.1832(8) 0.4519(7) 0.5509(3) 0.0509(8) Uani 1 1 d . . . H405 H 0.1214 0.5206 0.5328 0.061 Uiso 1 1 calc R . . B104 B -0.2124(7) 0.6990(7) 0.6207(3) 0.0369(17) Uani 1 1 d . . . H104 H -0.1820 0.6107 0.6095 0.044 Uiso 1 1 calc R . . C101 C -0.0174(6) 0.2561(5) 0.7147(3) 0.0326(14) Uani 1 1 d . . . C201 C -0.0348(6) 0.2852(5) 0.8307(3) 0.0287(13) Uani 1 1 d . . . C102 C -0.0476(6) 0.3402(6) 0.6657(3) 0.0346(14) Uani 1 1 d . . . H10A H -0.0303 0.4065 0.6603 0.042 Uiso 1 1 calc R . . B111 B -0.3381(7) 0.9559(7) 0.5885(3) 0.0356(17) Uani 1 1 d . . . H111 H -0.3876 1.0316 0.5559 0.043 Uiso 1 1 calc R . . C206 C 0.0081(6) 0.2998(7) 0.8763(3) 0.0439(17) Uani 1 1 d . . . H206 H 0.0842 0.3015 0.8735 0.053 Uiso 1 1 calc R . . C202 C -0.1496(6) 0.2843(7) 0.8355(3) 0.0413(16) Uani 1 1 d . . . H202 H -0.1803 0.2742 0.8056 0.050 Uiso 1 1 calc R . . C204 C -0.1732(7) 0.3113(7) 0.9301(3) 0.0505(19) Uani 1 1 d . . . H204 H -0.2195 0.3195 0.9633 0.061 Uiso 1 1 calc R . . B103 B -0.1036(6) 0.7678(7) 0.6230(3) 0.0337(16) Uani 1 1 d . . . H103 H -0.0051 0.7235 0.6126 0.040 Uiso 1 1 calc R . . C301 C 0.4192(7) 0.3668(8) 0.7164(5) 0.0616(10) Uani 1 1 d . . . B101 B -0.3171(6) 0.8615(6) 0.7062(3) 0.0319(15) Uani 1 1 d . . . H101 H -0.3526 0.8756 0.7486 0.038 Uiso 1 1 calc R . . C106 C -0.0437(7) 0.1568(7) 0.7214(3) 0.0458(17) Uani 1 1 d . . . H10B H -0.0237 0.0998 0.7539 0.055 Uiso 1 1 calc R . . C203 C -0.2176(7) 0.2986(8) 0.8849(3) 0.054(2) Uani 1 1 d . . . H203 H -0.2949 0.2997 0.8877 0.065 Uiso 1 1 calc R . . B109 B -0.3533(7) 0.8197(7) 0.5996(3) 0.0351(16) Uani 1 1 d . . . H109 H -0.4123 0.8064 0.5744 0.042 Uiso 1 1 calc R . . B203 B 0.2693(9) 0.6861(8) 0.8255(4) 0.050(2) Uani 1 1 d . . . H20A H 0.3581 0.6609 0.8024 0.060 Uiso 1 1 calc R . . C402 C 0.3670(8) 0.2501(7) 0.6050(3) 0.0509(8) Uani 1 1 d . . . H402 H 0.4307 0.1826 0.6226 0.061 Uiso 1 1 calc R . . C205 C -0.0596(7) 0.3116(8) 0.9255(3) 0.052(2) Uani 1 1 d . . . H205 H -0.0286 0.3200 0.9558 0.063 Uiso 1 1 calc R . . B204 B 0.1291(7) 0.8229(7) 0.8001(4) 0.0388(18) Uani 1 1 d . . . H20B H 0.1291 0.8841 0.7607 0.047 Uiso 1 1 calc R . . B108 B -0.2137(7) 0.8262(7) 0.5715(3) 0.0380(18) Uani 1 1 d . . . H108 H -0.1829 0.8177 0.5281 0.046 Uiso 1 1 calc R . . C104 C -0.1282(8) 0.2271(8) 0.6319(4) 0.056(2) Uani 1 1 d . . . H10C H -0.1649 0.2175 0.6040 0.067 Uiso 1 1 calc R . . C105 C -0.0990(8) 0.1423(7) 0.6804(4) 0.053(2) Uani 1 1 d . . . H10D H -0.1166 0.0762 0.6852 0.064 Uiso 1 1 calc R . . C302 C 0.4321(7) 0.3815(7) 0.7685(5) 0.0616(10) Uani 1 1 d . . . H302 H 0.3816 0.3674 0.7983 0.074 Uiso 1 1 calc R . . C103 C -0.1035(7) 0.3247(7) 0.6250(3) 0.0518(19) Uani 1 1 d . . . H10E H -0.1246 0.3816 0.5925 0.062 Uiso 1 1 calc R . . B205 B -0.0089(8) 0.7946(8) 0.8285(4) 0.048(2) Uani 1 1 d . . . H20C H -0.0958 0.8376 0.8074 0.057 Uiso 1 1 calc R . . B209 B 0.0449(10) 0.8765(8) 0.8596(4) 0.053(2) Uani 1 1 d . . . H209 H -0.0094 0.9733 0.8575 0.063 Uiso 1 1 calc R . . C303 C 0.5216(7) 0.4178(7) 0.7765(5) 0.0616(10) Uani 1 1 d . . . H303 H 0.5314 0.4272 0.8115 0.074 Uiso 1 1 calc R . . C306 C 0.4948(7) 0.3871(7) 0.6727(5) 0.0616(10) Uani 1 1 d . . . H306 H 0.4878 0.3768 0.6375 0.074 Uiso 1 1 calc R . . C404 C 0.2609(7) 0.3639(7) 0.5220(3) 0.0509(8) Uani 1 1 d . . . H404 H 0.2520 0.3728 0.4843 0.061 Uiso 1 1 calc R . . C403 C 0.3510(8) 0.2636(7) 0.5491(3) 0.0509(8) Uani 1 1 d . . . H403 H 0.4025 0.2034 0.5298 0.061 Uiso 1 1 calc R . . B211 B 0.1231(11) 0.7831(9) 0.9189(4) 0.060(3) Uani 1 1 d . . . H211 H 0.1190 0.8197 0.9559 0.071 Uiso 1 1 calc R . . C304 C 0.5944(7) 0.4391(7) 0.7318(4) 0.0616(10) Uani 1 1 d . . . H304 H 0.6526 0.4648 0.7365 0.074 Uiso 1 1 calc R . . B210 B -0.0034(11) 0.7686(9) 0.9015(4) 0.057(2) Uani 1 1 d . . . H210 H -0.0895 0.7960 0.9267 0.068 Uiso 1 1 calc R . . B207 B 0.2587(11) 0.6657(9) 0.8979(4) 0.064(3) Uani 1 1 d . . . H207 H 0.3426 0.6260 0.9212 0.076 Uiso 1 1 calc R . . B208 B 0.2062(9) 0.8123(8) 0.8575(4) 0.053(2) Uani 1 1 d . . . H208 H 0.2565 0.8677 0.8541 0.063 Uiso 1 1 calc R . . B202 B 0.2205(11) 0.5728(8) 0.8681(4) 0.059(3) Uani 1 1 d . . . H20D H 0.2786 0.4763 0.8717 0.071 Uiso 1 1 calc R . . B201 B 0.0475(12) 0.6383(10) 0.8718(4) 0.062(3) Uani 1 1 d . . . H201 H -0.0035 0.5828 0.8783 0.074 Uiso 1 1 calc R . . B206 B 0.1287(13) 0.6385(9) 0.9248(4) 0.068(3) Uani 1 1 d . . . H20E H 0.1285 0.5807 0.9653 0.082 Uiso 1 1 calc R . . B107 B -0.1882(7) 0.9238(7) 0.6053(4) 0.0389(18) Uani 1 1 d . . . H107 H -0.1403 0.9786 0.5838 0.047 Uiso 1 1 calc R . . C305 C 0.5826(7) 0.4237(7) 0.6824(5) 0.0616(10) Uani 1 1 d . . . H305 H 0.6340 0.4375 0.6531 0.074 Uiso 1 1 calc R . . C31 C 0.6923(11) 0.0881(10) 0.8019(8) 0.101(5) Uani 1 1 d . . . H31A H 0.6756 0.1642 0.7780 0.152 Uiso 1 1 calc R . . H31B H 0.6577 0.0459 0.7873 0.152 Uiso 1 1 calc R . . H31C H 0.7791 0.0419 0.8040 0.152 Uiso 1 1 calc R . . N3 N 0.5977(16) 0.1244(17) 0.9007(10) 0.183(9) Uani 1 1 d . . . C30 C 0.6391(14) 0.1067(13) 0.8567(11) 0.120(7) Uani 1 1 d . . . N4 N 0.3234(19) 0.038(2) 0.9144(12) 0.196(14) Uani 1 1 d . . . C40 C 0.243(3) 0.0241(19) 0.9505(17) 0.183(18) Uani 1 1 d . . . C41 C 0.163(3) 0.0070(19) 0.9948(13) 0.195(13) Uani 1 1 d . . . H41A H 0.1854 -0.0771 1.0073 0.292 Uiso 1 1 calc R . . H41B H 0.0807 0.0454 0.9824 0.292 Uiso 1 1 calc R . . H41C H 0.1675 0.0412 1.0249 0.292 Uiso 1 1 calc R . . N1 N 0.6433(6) 0.7129(6) 0.9292(3) 0.0541(17) Uani 1 1 d . . . C134 C 0.706(7) 0.749(7) 1.0183(19) 0.15(3) Uani 0.384(12) 1 d PD A 1 H13A H 0.6968 0.8148 1.0342 0.232 Uiso 0.384(12) 1 calc PR A 1 H13B H 0.7910 0.6991 1.0125 0.232 Uiso 0.384(12) 1 calc PR A 1 H13C H 0.6683 0.7025 1.0431 0.232 Uiso 0.384(12) 1 calc PR A 1 C124 C 0.470(2) 0.682(3) 0.9955(12) 0.066(9) Uani 0.384(12) 1 d PD A 1 H12A H 0.4521 0.6196 1.0195 0.099 Uiso 0.384(12) 1 calc PR A 1 H12B H 0.4112 0.7223 0.9673 0.099 Uiso 0.384(12) 1 calc PR A 1 H12C H 0.4670 0.7377 1.0168 0.099 Uiso 0.384(12) 1 calc PR A 1 C123 C 0.595(2) 0.6275(19) 0.9690(11) 0.061(7) Uani 0.384(12) 1 d PD A 1 H12D H 0.5961 0.5701 0.9485 0.073 Uiso 0.384(12) 1 calc PR A 1 H12E H 0.6520 0.5831 0.9984 0.073 Uiso 0.384(12) 1 calc PR A 1 C133 C 0.645(2) 0.795(2) 0.9641(14) 0.073(8) Uani 0.384(12) 1 d PD A 1 H13D H 0.6824 0.8446 0.9411 0.088 Uiso 0.384(12) 1 calc PR A 1 H13E H 0.5606 0.8483 0.9714 0.088 Uiso 0.384(12) 1 calc PR A 1 C114 C 0.561(7) 0.695(6) 0.8446(16) 0.12(3) Uani 0.384(12) 1 d PD A 1 H11A H 0.5108 0.7437 0.8137 0.175 Uiso 0.384(12) 1 calc PR A 1 H11B H 0.5246 0.6448 0.8668 0.175 Uiso 0.384(12) 1 calc PR A 1 H11C H 0.6410 0.6460 0.8312 0.175 Uiso 0.384(12) 1 calc PR A 1 C113 C 0.570(2) 0.774(3) 0.8792(13) 0.082(9) Uani 0.384(12) 1 d PD A 1 H11D H 0.6044 0.8257 0.8558 0.098 Uiso 0.384(12) 1 calc PR A 1 H11E H 0.4877 0.8255 0.8909 0.098 Uiso 0.384(12) 1 calc PR A 1 C142 C 0.768(2) 0.637(3) 0.9122(11) 0.073(8) Uani 0.384(12) 1 d P A 1 H14A H 0.8155 0.5945 0.9444 0.110 Uiso 0.384(12) 1 calc PR A 1 H14B H 0.8039 0.6854 0.8884 0.110 Uiso 0.384(12) 1 calc PR A 1 H14C H 0.7662 0.5802 0.8925 0.110 Uiso 0.384(12) 1 calc PR A 1 C112 C 0.588(4) 0.659(6) 0.8465(18) 0.15(2) Uani 0.616(12) 1 d P A 2 H11F H 0.6180 0.5956 0.8258 0.230 Uiso 0.616(12) 1 calc PR A 2 H11G H 0.5830 0.7319 0.8222 0.230 Uiso 0.616(12) 1 calc PR A 2 H11H H 0.5081 0.6704 0.8625 0.230 Uiso 0.616(12) 1 calc PR A 2 C121 C 0.5234(16) 0.7409(13) 0.9590(7) 0.071(5) Uani 0.616(12) 1 d PD A 2 H12F H 0.4625 0.7626 0.9322 0.085 Uiso 0.616(12) 1 calc PR A 2 H12G H 0.5025 0.8104 0.9755 0.085 Uiso 0.616(12) 1 calc PR A 2 C111 C 0.6719(14) 0.628(2) 0.8911(8) 0.089(7) Uani 0.616(12) 1 d P A 2 H11I H 0.7520 0.6151 0.8738 0.106 Uiso 0.616(12) 1 calc PR A 2 H11J H 0.6786 0.5524 0.9136 0.106 Uiso 0.616(12) 1 calc PR A 2 C131 C 0.7442(16) 0.6621(16) 0.9691(8) 0.076(5) Uani 0.616(12) 1 d P A 2 H13F H 0.7531 0.5821 0.9864 0.091 Uiso 0.616(12) 1 calc PR A 2 H13G H 0.8192 0.6532 0.9473 0.091 Uiso 0.616(12) 1 calc PR A 2 C141 C 0.645(2) 0.825(2) 0.8926(10) 0.114(9) Uani 0.616(12) 1 d P A 2 H14D H 0.7229 0.8068 0.8735 0.172 Uiso 0.616(12) 1 calc PR A 2 H14E H 0.6296 0.8834 0.9151 0.172 Uiso 0.616(12) 1 calc PR A 2 H14F H 0.5821 0.8572 0.8661 0.172 Uiso 0.616(12) 1 calc PR A 2 C122 C 0.516(3) 0.641(3) 1.0042(14) 0.141(16) Uani 0.616(12) 1 d PD A 2 H12H H 0.4346 0.6668 1.0208 0.212 Uiso 0.616(12) 1 calc PR A 2 H12I H 0.5731 0.6209 1.0319 0.212 Uiso 0.616(12) 1 calc PR A 2 H12J H 0.5348 0.5719 0.9884 0.212 Uiso 0.616(12) 1 calc PR A 2 C132 C 0.738(4) 0.723(4) 1.0129(9) 0.097(12) Uani 0.616(12) 1 d P A 2 H13H H 0.8095 0.6783 1.0341 0.146 Uiso 0.616(12) 1 calc PR A 2 H13I H 0.6665 0.7294 1.0366 0.146 Uiso 0.616(12) 1 calc PR A 2 H13J H 0.7323 0.8015 0.9971 0.146 Uiso 0.616(12) 1 calc PR A 2 C211 C 0.7183(11) 0.0458(10) 0.4286(5) 0.089(3) Uiso 1 1 d D . . H21A H 0.7354 0.0178 0.4677 0.107 Uiso 1 1 calc R . . H21B H 0.6361 0.0550 0.4252 0.107 Uiso 1 1 calc R . . N2 N 0.7142(12) 0.1736(11) 0.4132(6) 0.125(4) Uiso 1 1 d D . . C221 C 0.6283(15) 0.2365(15) 0.4545(7) 0.122(5) Uiso 1 1 d . . . H22A H 0.6579 0.1920 0.4910 0.147 Uiso 1 1 calc R . . H22B H 0.5507 0.2345 0.4516 0.147 Uiso 1 1 calc R . . C231 C 0.8139(18) 0.2136(18) 0.4164(9) 0.149(6) Uiso 1 1 d . . . H23A H 0.7789 0.3001 0.4123 0.179 Uiso 1 1 calc R . . H23B H 0.8752 0.1902 0.3867 0.179 Uiso 1 1 calc R . . C212 C 0.806(2) -0.057(2) 0.3984(10) 0.179(8) Uiso 1 1 d . . . H21C H 0.7905 -0.1269 0.4128 0.269 Uiso 1 1 calc R . . H21D H 0.8887 -0.0753 0.4042 0.269 Uiso 1 1 calc R . . H21E H 0.7915 -0.0332 0.3594 0.269 Uiso 1 1 calc R . . C232 C 0.8728(18) 0.1550(18) 0.4727(9) 0.157(7) Uiso 1 1 d . . . H23C H 0.9374 0.1778 0.4746 0.235 Uiso 1 1 calc R . . H23D H 0.9057 0.0695 0.4768 0.235 Uiso 1 1 calc R . . H23E H 0.8124 0.1809 0.5019 0.235 Uiso 1 1 calc R . . C222 C 0.604(3) 0.367(3) 0.4517(14) 0.255(14) Uiso 1 1 d . . . H22C H 0.5425 0.4000 0.4792 0.383 Uiso 1 1 calc R . . H22D H 0.5776 0.4121 0.4155 0.383 Uiso 1 1 calc R . . H22E H 0.6785 0.3701 0.4585 0.383 Uiso 1 1 calc R . . C241 C 0.6594(16) 0.2359(16) 0.3541(6) 0.140(6) Uiso 1 1 d D . . H24A H 0.7162 0.1967 0.3263 0.210 Uiso 1 1 calc R . . H24B H 0.6448 0.3187 0.3471 0.210 Uiso 1 1 calc R . . H24C H 0.5838 0.2301 0.3531 0.210 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 Pd1 0.0195(2) 0.0208(2) 0.0228(2) -0.00501(16) 0.00113(16) -0.00623(17) Ge1 0.0218(3) 0.0213(3) 0.0278(3) -0.0052(2) 0.0008(2) -0.0069(2) Ge2 0.0392(4) 0.0285(3) 0.0301(4) -0.0069(3) -0.0028(3) -0.0152(3) P2 0.0263(8) 0.0223(7) 0.0285(8) -0.0042(6) 0.0036(6) -0.0088(6) P1 0.0224(7) 0.0250(8) 0.0282(8) -0.0055(6) 0.0015(6) -0.0054(6) S2 0.0288(7) 0.0263(7) 0.0276(8) -0.0061(6) 0.0009(6) -0.0138(6) S1 0.0230(7) 0.0242(7) 0.0287(8) -0.0014(6) 0.0048(6) -0.0051(6) C401 0.062(2) 0.0399(16) 0.0311(15) -0.0086(12) 0.0007(14) -0.0040(14) C1 0.026(3) 0.031(3) 0.033(3) -0.006(3) 0.000(3) -0.001(3) C406 0.062(2) 0.0399(16) 0.0311(15) -0.0086(12) 0.0007(14) -0.0040(14) B105 0.025(3) 0.027(3) 0.039(4) -0.004(3) -0.004(3) -0.011(3) B110 0.021(3) 0.028(4) 0.036(4) -0.006(3) 0.001(3) -0.001(3) B106 0.033(4) 0.025(3) 0.044(4) -0.006(3) 0.001(3) -0.011(3) C3 0.038(4) 0.020(3) 0.040(4) -0.001(3) 0.004(3) -0.005(3) B102 0.028(4) 0.029(4) 0.039(4) 0.000(3) -0.006(3) -0.016(3) C2 0.028(3) 0.025(3) 0.041(4) -0.008(3) 0.002(3) -0.005(3) C405 0.062(2) 0.0399(16) 0.0311(15) -0.0086(12) 0.0007(14) -0.0040(14) B104 0.036(4) 0.032(4) 0.036(4) -0.012(3) -0.006(3) -0.004(3) C101 0.034(3) 0.026(3) 0.041(4) -0.013(3) 0.003(3) -0.014(3) C201 0.032(3) 0.025(3) 0.026(3) -0.001(2) 0.007(2) -0.013(3) C102 0.038(4) 0.026(3) 0.043(4) -0.007(3) -0.006(3) -0.015(3) B111 0.030(4) 0.034(4) 0.029(4) -0.004(3) 0.005(3) -0.003(3) C206 0.032(4) 0.065(5) 0.038(4) -0.016(3) 0.006(3) -0.023(3) C202 0.038(4) 0.055(4) 0.038(4) -0.005(3) 0.000(3) -0.028(3) C204 0.041(4) 0.063(5) 0.035(4) -0.004(4) 0.010(3) -0.016(4) B103 0.023(3) 0.036(4) 0.033(4) -0.002(3) 0.004(3) -0.008(3) C301 0.0365(17) 0.0477(18) 0.100(3) -0.015(2) -0.0123(18) -0.0139(14) B101 0.027(4) 0.026(3) 0.036(4) -0.005(3) 0.004(3) -0.007(3) C106 0.053(4) 0.036(4) 0.050(5) -0.008(3) 0.004(4) -0.023(3) C203 0.032(4) 0.072(5) 0.049(5) -0.007(4) 0.009(3) -0.019(4) B109 0.028(4) 0.036(4) 0.039(4) -0.011(3) -0.007(3) -0.007(3) B203 0.054(5) 0.039(5) 0.057(6) -0.006(4) -0.025(4) -0.016(4) C402 0.062(2) 0.0399(16) 0.0311(15) -0.0086(12) 0.0007(14) -0.0040(14) C205 0.037(4) 0.079(6) 0.036(4) -0.019(4) 0.007(3) -0.018(4) B204 0.042(4) 0.028(4) 0.047(5) -0.008(3) -0.009(4) -0.012(3) B108 0.031(4) 0.040(4) 0.027(4) -0.008(3) 0.002(3) -0.002(3) C104 0.057(5) 0.057(5) 0.061(5) -0.029(4) -0.014(4) -0.019(4) C105 0.058(5) 0.039(4) 0.076(6) -0.027(4) 0.001(4) -0.025(4) C302 0.0365(17) 0.0477(18) 0.100(3) -0.015(2) -0.0123(18) -0.0139(14) C103 0.055(5) 0.051(5) 0.047(5) -0.014(4) -0.011(4) -0.015(4) B205 0.046(5) 0.049(5) 0.046(5) -0.022(4) 0.000(4) -0.012(4) B209 0.072(6) 0.041(5) 0.046(5) -0.017(4) -0.013(5) -0.018(4) C303 0.0365(17) 0.0477(18) 0.100(3) -0.015(2) -0.0123(18) -0.0139(14) C306 0.0365(17) 0.0477(18) 0.100(3) -0.015(2) -0.0123(18) -0.0139(14) C404 0.062(2) 0.0399(16) 0.0311(15) -0.0086(12) 0.0007(14) -0.0040(14) C403 0.062(2) 0.0399(16) 0.0311(15) -0.0086(12) 0.0007(14) -0.0040(14) B211 0.095(8) 0.050(5) 0.044(5) -0.013(4) -0.025(5) -0.032(5) C304 0.0365(17) 0.0477(18) 0.100(3) -0.015(2) -0.0123(18) -0.0139(14) B210 0.082(7) 0.061(6) 0.036(5) -0.021(4) 0.015(5) -0.038(5) B207 0.082(7) 0.051(6) 0.057(6) -0.009(5) -0.037(6) -0.019(5) B208 0.066(6) 0.040(5) 0.057(6) -0.015(4) -0.014(5) -0.021(4) B202 0.101(8) 0.034(4) 0.038(5) -0.003(4) -0.016(5) -0.022(5) B201 0.106(9) 0.065(6) 0.033(5) -0.019(4) 0.019(5) -0.054(6) B206 0.129(10) 0.045(5) 0.034(5) -0.001(4) -0.010(6) -0.041(6) B107 0.025(4) 0.036(4) 0.046(5) 0.006(3) 0.002(3) -0.011(3) C305 0.0365(17) 0.0477(18) 0.100(3) -0.015(2) -0.0123(18) -0.0139(14) C31 0.062(7) 0.056(6) 0.178(16) -0.014(8) -0.030(9) -0.016(5) N3 0.125(13) 0.141(14) 0.25(2) 0.010(14) 0.053(14) -0.066(11) C30 0.061(8) 0.078(9) 0.20(2) 0.016(12) -0.005(10) -0.034(7) N4 0.133(15) 0.154(15) 0.27(3) -0.133(18) -0.120(17) 0.043(13) C40 0.17(2) 0.081(12) 0.26(4) -0.10(2) -0.16(3) 0.058(17) C41 0.24(3) 0.106(14) 0.27(3) -0.110(19) 0.04(2) -0.078(17) N1 0.052(4) 0.046(4) 0.056(4) -0.004(3) -0.001(3) -0.017(3) C134 0.16(5) 0.23(7) 0.16(6) -0.16(5) 0.09(4) -0.13(5) C124 0.07(2) 0.11(3) 0.039(13) -0.018(15) 0.008(13) -0.05(2) C123 0.057(14) 0.044(13) 0.065(16) 0.006(10) 0.001(12) -0.016(11) C133 0.044(13) 0.071(17) 0.10(2) -0.004(15) 0.002(13) -0.027(12) C114 0.12(5) 0.23(6) 0.020(16) -0.02(2) 0.013(18) -0.10(4) C113 0.048(14) 0.09(2) 0.08(2) 0.011(16) -0.003(13) -0.015(13) C142 0.050(14) 0.09(2) 0.062(16) -0.021(14) 0.024(12) -0.025(13) C112 0.074(18) 0.31(5) 0.15(3) -0.14(4) 0.041(18) -0.12(3) C121 0.077(11) 0.056(9) 0.066(10) -0.014(8) 0.015(8) -0.019(8) C111 0.049(9) 0.148(18) 0.091(13) -0.081(13) 0.029(9) -0.042(10) C131 0.078(11) 0.086(12) 0.079(12) 0.001(9) -0.012(9) -0.054(10) C141 0.116(18) 0.100(16) 0.117(19) 0.039(13) -0.017(14) -0.061(14) C122 0.060(16) 0.14(2) 0.19(3) 0.08(2) -0.028(17) -0.057(16) C132 0.15(3) 0.17(3) 0.027(8) -0.016(14) 0.011(13) -0.13(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 Pd1 P2 2.2762(16) . ? Pd1 P1 2.2812(16) . ? Pd1 S2 2.3662(15) . ? Pd1 S1 2.3752(15) . ? Ge1 B102 2.098(7) . ? Ge1 B104 2.113(8) . ? Ge1 B101 2.114(7) . ? Ge1 B103 2.114(7) . ? Ge1 B105 2.134(7) . ? Ge1 S1 2.1436(16) . ? Ge2 B202 2.089(9) . ? Ge2 B205 2.100(8) . ? Ge2 B204 2.100(7) . ? Ge2 B201 2.108(9) . ? Ge2 B203 2.114(9) . ? Ge2 S2 2.1373(16) . ? P2 C201 1.810(6) . ? P2 C101 1.817(7) . ? P2 C3 1.831(6) . ? P1 C1 1.821(6) . ? P1 C401 1.824(8) . ? P1 C301 1.826(8) . ? C401 C406 1.382(10) . ? C401 C402 1.386(10) . ? C1 C2 1.525(9) . ? C406 C405 1.372(10) . ? B105 B110 1.763(10) . ? B105 B109 1.765(11) . ? B105 B104 1.875(11) . ? B105 B101 1.886(10) . ? B110 B111 1.772(10) . ? B110 B101 1.777(11) . ? B110 B109 1.783(10) . ? B110 B106 1.787(11) . ? B106 B101 1.774(10) . ? B106 B107 1.775(11) . ? B106 B102 1.775(10) . ? B106 B111 1.779(11) . ? C3 C2 1.535(9) . ? B102 B107 1.746(11) . ? B102 B103 1.882(11) . ? B102 B101 1.884(10) . ? C405 C404 1.376(10) . ? B104 B109 1.771(10) . ? B104 B108 1.782(12) . ? B104 B103 1.892(11) . ? C101 C102 1.392(10) . ? C101 C106 1.398(9) . ? C201 C206 1.386(9) . ? C201 C202 1.394(9) . ? C102 C103 1.383(10) . ? B111 B108 1.766(10) . ? B111 B109 1.771(11) . ? B111 B107 1.776(11) . ? C206 C205 1.374(10) . ? C202 C203 1.381(10) . ? C204 C205 1.376(11) . ? C204 C203 1.376(12) . ? B103 B107 1.760(10) . ? B103 B108 1.775(11) . ? C301 C306 1.376(14) . ? C301 C302 1.382(14) . ? C106 C105 1.378(11) . ? B109 B108 1.778(11) . ? B203 B207 1.747(14) . ? B203 B208 1.758(13) . ? B203 B202 1.847(14) . ? B203 B204 1.875(12) . ? C402 C403 1.386(10) . ? B204 B208 1.757(12) . ? B204 B209 1.763(13) . ? B204 B205 1.882(13) . ? B108 B107 1.788(12) . ? C104 C103 1.364(12) . ? C104 C105 1.385(12) . ? C302 C303 1.408(11) . ? B205 B210 1.767(13) . ? B205 B209 1.786(12) . ? B205 B201 1.893(14) . ? B209 B211 1.753(13) . ? B209 B208 1.766(14) . ? B209 B210 1.784(14) . ? C303 C304 1.375(13) . ? C306 C305 1.406(11) . ? C404 C403 1.364(10) . ? B211 B210 1.750(15) . ? B211 B208 1.770(16) . ? B211 B206 1.775(13) . ? B211 B207 1.780(16) . ? C304 C305 1.317(13) . ? B210 B206 1.770(16) . ? B210 B201 1.779(13) . ? B207 B202 1.762(14) . ? B207 B208 1.774(14) . ? B207 B206 1.779(18) . ? B202 B206 1.786(15) . ? B202 B201 1.894(17) . ? B201 B206 1.748(15) . ? C31 C30 1.44(3) . ? N3 C30 1.16(3) . ? N4 C40 1.27(5) . ? C40 C41 1.42(4) . ? N1 C142 1.46(2) . ? N1 C121 1.474(17) . ? N1 C111 1.479(17) . ? N1 C113 1.48(3) . ? N1 C131 1.502(18) . ? N1 C133 1.50(3) . ? N1 C141 1.51(2) . ? N1 C123 1.55(2) . ? C134 C133 1.49(2) . ? C124 C123 1.489(18) . ? C114 C113 1.50(2) . ? C112 C111 1.48(4) . ? C121 C122 1.515(18) . ? C131 C132 1.44(4) . ? C211 C212 1.55(2) . ? C211 N2 1.555(13) . ? N2 C221 1.455(19) . ? N2 C231 1.52(2) . ? N2 C241 1.579(10) . ? C221 C222 1.53(3) . ? C231 C232 1.53(2) . ? 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 P2 Pd1 P1 93.25(6) . . ? P2 Pd1 S2 177.98(6) . . ? P1 Pd1 S2 88.39(6) . . ? P2 Pd1 S1 85.17(5) . . ? P1 Pd1 S1 173.45(6) . . ? S2 Pd1 S1 93.07(5) . . ? B102 Ge1 B104 92.4(3) . . ? B102 Ge1 B101 53.1(3) . . ? B104 Ge1 B101 92.0(3) . . ? B102 Ge1 B103 53.1(3) . . ? B104 Ge1 B103 53.2(3) . . ? B101 Ge1 B103 92.6(3) . . ? B102 Ge1 B105 92.1(3) . . ? B104 Ge1 B105 52.4(3) . . ? B101 Ge1 B105 52.7(3) . . ? B103 Ge1 B105 92.0(3) . . ? B102 Ge1 S1 137.3(2) . . ? B104 Ge1 S1 128.7(2) . . ? B101 Ge1 S1 124.7(2) . . ? B103 Ge1 S1 140.1(2) . . ? B105 Ge1 S1 120.6(2) . . ? B202 Ge2 B205 93.2(4) . . ? B202 Ge2 B204 92.1(3) . . ? B205 Ge2 B204 53.3(4) . . ? B202 Ge2 B201 53.7(5) . . ? B205 Ge2 B201 53.5(4) . . ? B204 Ge2 B201 92.8(4) . . ? B202 Ge2 B203 52.1(4) . . ? B205 Ge2 B203 92.5(4) . . ? B204 Ge2 B203 52.8(3) . . ? B201 Ge2 B203 92.2(4) . . ? B202 Ge2 S2 133.7(3) . . ? B205 Ge2 S2 130.7(3) . . ? B204 Ge2 S2 123.7(2) . . ? B201 Ge2 S2 137.8(3) . . ? B203 Ge2 S2 125.6(3) . . ? C201 P2 C101 108.5(3) . . ? C201 P2 C3 102.0(3) . . ? C101 P2 C3 104.8(3) . . ? C201 P2 Pd1 110.1(2) . . ? C101 P2 Pd1 113.8(2) . . ? C3 P2 Pd1 116.7(2) . . ? C1 P1 C401 107.1(3) . . ? C1 P1 C301 101.2(4) . . ? C401 P1 C301 106.5(5) . . ? C1 P1 Pd1 117.7(2) . . ? C401 P1 Pd1 106.7(3) . . ? C301 P1 Pd1 116.8(3) . . ? Ge2 S2 Pd1 102.16(6) . . ? Ge1 S1 Pd1 105.22(6) . . ? C406 C401 C402 118.1(7) . . ? C406 C401 P1 119.4(5) . . ? C402 C401 P1 122.5(6) . . ? C2 C1 P1 116.4(4) . . ? C405 C406 C401 121.6(7) . . ? B110 B105 B109 60.7(4) . . ? B110 B105 B104 106.8(5) . . ? B109 B105 B104 58.1(4) . . ? B110 B105 B101 58.2(4) . . ? B109 B105 B101 106.8(5) . . ? B104 B105 B101 107.9(5) . . ? B110 B105 Ge1 112.5(4) . . ? B109 B105 Ge1 112.5(4) . . ? B104 B105 Ge1 63.2(3) . . ? B101 B105 Ge1 63.1(3) . . ? B105 B110 B111 109.1(5) . . ? B105 B110 B101 64.4(4) . . ? B111 B110 B101 109.1(5) . . ? B105 B110 B109 59.7(4) . . ? B111 B110 B109 59.8(4) . . ? B101 B110 B109 110.9(5) . . ? B105 B110 B106 111.1(5) . . ? B111 B110 B106 60.0(4) . . ? B101 B110 B106 59.7(4) . . ? B109 B110 B106 108.2(5) . . ? B101 B106 B107 110.1(5) . . ? B101 B106 B102 64.1(4) . . ? B107 B106 B102 58.9(4) . . ? B101 B106 B111 108.9(5) . . ? B107 B106 B111 60.0(4) . . ? B102 B106 B111 108.5(5) . . ? B101 B106 B110 59.9(4) . . ? B107 B106 B110 107.6(5) . . ? B102 B106 B110 110.6(5) . . ? B111 B106 B110 59.6(4) . . ? C2 C3 P2 114.3(5) . . ? B107 B102 B106 60.5(4) . . ? B107 B102 B103 57.9(4) . . ? B106 B102 B103 106.8(5) . . ? B107 B102 B101 106.4(5) . . ? B106 B102 B101 57.9(4) . . ? B103 B102 B101 108.5(5) . . ? B107 B102 Ge1 113.0(5) . . ? B106 B102 Ge1 113.3(4) . . ? B103 B102 Ge1 63.9(3) . . ? B101 B102 Ge1 63.9(3) . . ? C1 C2 C3 112.8(5) . . ? C406 C405 C404 119.8(7) . . ? B109 B104 B108 60.0(4) . . ? B109 B104 B105 57.8(4) . . ? B108 B104 B105 106.1(5) . . ? B109 B104 B103 106.3(5) . . ? B108 B104 B103 57.7(4) . . ? B105 B104 B103 108.5(5) . . ? B109 B104 Ge1 113.2(4) . . ? B108 B104 Ge1 112.4(5) . . ? B105 B104 Ge1 64.4(3) . . ? B103 B104 Ge1 63.5(3) . . ? C102 C101 C106 118.7(6) . . ? C102 C101 P2 120.0(5) . . ? C106 C101 P2 121.2(6) . . ? C206 C201 C202 118.5(6) . . ? C206 C201 P2 117.6(5) . . ? C202 C201 P2 123.8(5) . . ? C103 C102 C101 119.8(6) . . ? B108 B111 B109 60.3(4) . . ? B108 B111 B110 109.0(5) . . ? B109 B111 B110 60.4(4) . . ? B108 B111 B107 60.6(5) . . ? B109 B111 B107 108.6(5) . . ? B110 B111 B107 108.2(5) . . ? B108 B111 B106 109.2(5) . . ? B109 B111 B106 109.1(5) . . ? B110 B111 B106 60.4(4) . . ? B107 B111 B106 59.9(5) . . ? C205 C206 C201 121.3(7) . . ? C203 C202 C201 119.6(7) . . ? C205 C204 C203 119.2(7) . . ? B107 B103 B108 60.8(5) . . ? B107 B103 B102 57.2(4) . . ? B108 B103 B102 106.1(5) . . ? B107 B103 B104 106.3(5) . . ? B108 B103 B104 58.1(4) . . ? B102 B103 B104 107.3(5) . . ? B107 B103 Ge1 111.7(4) . . ? B108 B103 Ge1 112.7(4) . . ? B102 B103 Ge1 63.0(3) . . ? B104 B103 Ge1 63.4(3) . . ? C306 C301 C302 119.7(8) . . ? C306 C301 P1 122.8(8) . . ? C302 C301 P1 117.4(7) . . ? B106 B101 B110 60.5(4) . . ? B106 B101 B102 58.0(4) . . ? B110 B101 B102 106.2(5) . . ? B106 B101 B105 106.2(5) . . ? B110 B101 B105 57.5(4) . . ? B102 B101 B105 107.8(5) . . ? B106 B101 Ge1 112.6(4) . . ? B110 B101 Ge1 112.8(4) . . ? B102 B101 Ge1 63.0(3) . . ? B105 B101 Ge1 64.2(3) . . ? C105 C106 C101 120.9(7) . . ? C204 C203 C202 121.3(7) . . ? B105 B109 B111 109.0(5) . . ? B105 B109 B104 64.0(4) . . ? B111 B109 B104 109.3(5) . . ? B105 B109 B108 111.2(5) . . ? B111 B109 B108 59.7(4) . . ? B104 B109 B108 60.3(4) . . ? B105 B109 B110 59.6(4) . . ? B111 B109 B110 59.8(4) . . ? B104 B109 B110 110.6(5) . . ? B108 B109 B110 108.0(5) . . ? B207 B203 B208 60.8(6) . . ? B207 B203 B202 58.6(6) . . ? B208 B203 B202 107.6(7) . . ? B207 B203 B204 106.5(7) . . ? B208 B203 B204 57.7(5) . . ? B202 B203 B204 108.3(7) . . ? B207 B203 Ge2 112.6(7) . . ? B208 B203 Ge2 112.4(6) . . ? B202 B203 Ge2 63.2(4) . . ? B204 B203 Ge2 63.2(4) . . ? C403 C402 C401 120.0(7) . . ? C206 C205 C204 120.1(7) . . ? B208 B204 B209 60.2(5) . . ? B208 B204 B203 57.8(5) . . ? B209 B204 B203 106.4(6) . . ? B208 B204 B205 106.8(6) . . ? B209 B204 B205 58.6(5) . . ? B203 B204 B205 108.3(6) . . ? B208 B204 Ge2 113.1(5) . . ? B209 B204 Ge2 113.2(5) . . ? B203 B204 Ge2 64.0(3) . . ? B205 B204 Ge2 63.4(3) . . ? B111 B108 B103 109.3(5) . . ? B111 B108 B109 59.9(4) . . ? B103 B108 B109 111.2(5) . . ? B111 B108 B104 108.9(5) . . ? B103 B108 B104 64.3(4) . . ? B109 B108 B104 59.7(4) . . ? B111 B108 B107 60.0(4) . . ? B103 B108 B107 59.2(4) . . ? B109 B108 B107 107.8(5) . . ? B104 B108 B107 109.9(5) . . ? C103 C104 C105 120.4(7) . . ? C106 C105 C104 119.4(7) . . ? C301 C302 C303 119.9(10) . . ? C104 C103 C102 120.8(8) . . ? B210 B205 B209 60.3(5) . . ? B210 B205 B204 105.7(6) . . ? B209 B205 B204 57.4(5) . . ? B210 B205 B201 58.0(5) . . ? B209 B205 B201 106.4(7) . . ? B204 B205 B201 107.6(6) . . ? B210 B205 Ge2 112.5(6) . . ? B209 B205 Ge2 112.2(6) . . ? B204 B205 Ge2 63.4(4) . . ? B201 B205 Ge2 63.5(4) . . ? B211 B209 B204 109.3(7) . . ? B211 B209 B208 60.4(6) . . ? B204 B209 B208 59.7(5) . . ? B211 B209 B210 59.3(6) . . ? B204 B209 B210 110.2(6) . . ? B208 B209 B210 107.8(7) . . ? B211 B209 B205 108.6(7) . . ? B204 B209 B205 64.1(5) . . ? B208 B209 B205 110.8(6) . . ? B210 B209 B205 59.3(5) . . ? C304 C303 C302 119.0(10) . . ? C301 C306 C305 118.5(10) . . ? C403 C404 C405 119.5(7) . . ? C404 C403 C402 121.0(7) . . ? B210 B211 B209 61.2(6) . . ? B210 B211 B208 109.1(6) . . ? B209 B211 B208 60.2(6) . . ? B210 B211 B206 60.3(6) . . ? B209 B211 B206 109.2(6) . . ? B208 B211 B206 108.3(7) . . ? B210 B211 B207 108.7(7) . . ? B209 B211 B207 108.6(7) . . ? B208 B211 B207 59.9(6) . . ? B206 B211 B207 60.1(7) . . ? C305 C304 C303 120.8(9) . . ? B211 B210 B205 109.5(7) . . ? B211 B210 B206 60.5(6) . . ? B205 B210 B206 110.6(7) . . ? B211 B210 B201 109.5(8) . . ? B205 B210 B201 64.5(5) . . ? B206 B210 B201 59.0(6) . . ? B211 B210 B209 59.5(6) . . ? B205 B210 B209 60.4(5) . . ? B206 B210 B209 108.1(8) . . ? B201 B210 B209 111.5(7) . . ? B203 B207 B202 63.5(5) . . ? B203 B207 B208 59.9(5) . . ? B202 B207 B208 110.7(7) . . ? B203 B207 B206 110.8(7) . . ? B202 B207 B206 60.6(6) . . ? B208 B207 B206 107.9(8) . . ? B203 B207 B211 109.2(7) . . ? B202 B207 B211 109.8(8) . . ? B208 B207 B211 59.7(6) . . ? B206 B207 B211 59.8(6) . . ? B204 B208 B203 64.5(5) . . ? B204 B208 B209 60.0(5) . . ? B203 B208 B209 111.5(6) . . ? B204 B208 B211 108.7(7) . . ? B203 B208 B211 109.1(7) . . ? B209 B208 B211 59.4(6) . . ? B204 B208 B207 110.6(6) . . ? B203 B208 B207 59.3(5) . . ? B209 B208 B207 108.3(8) . . ? B211 B208 B207 60.3(6) . . ? B207 B202 B206 60.2(6) . . ? B207 B202 B203 57.8(6) . . ? B206 B202 B203 106.1(6) . . ? B207 B202 B201 105.8(7) . . ? B206 B202 B201 56.6(6) . . ? B203 B202 B201 108.8(6) . . ? B207 B202 Ge2 113.1(6) . . ? B206 B202 Ge2 111.6(7) . . ? B203 B202 Ge2 64.6(4) . . ? B201 B202 Ge2 63.7(4) . . ? B206 B201 B210 60.2(6) . . ? B206 B201 B205 105.9(7) . . ? B210 B201 B205 57.4(5) . . ? B206 B201 B202 58.6(6) . . ? B210 B201 B202 106.2(7) . . ? B205 B201 B202 107.0(6) . . ? B206 B201 Ge2 112.3(7) . . ? B210 B201 Ge2 111.7(6) . . ? B205 B201 Ge2 63.0(4) . . ? B202 B201 Ge2 62.7(4) . . ? B201 B206 B210 60.7(6) . . ? B201 B206 B211 109.8(7) . . ? B210 B206 B211 59.2(6) . . ? B201 B206 B207 111.6(7) . . ? B210 B206 B207 107.9(7) . . ? B211 B206 B207 60.1(6) . . ? B201 B206 B202 64.8(6) . . ? B210 B206 B202 111.4(7) . . ? B211 B206 B202 108.9(8) . . ? B207 B206 B202 59.3(6) . . ? B102 B107 B103 64.9(4) . . ? B102 B107 B106 60.6(4) . . ? B103 B107 B106 112.4(5) . . ? B102 B107 B111 110.0(5) . . ? B103 B107 B111 109.5(6) . . ? B106 B107 B111 60.1(4) . . ? B102 B107 B108 111.7(5) . . ? B103 B107 B108 60.0(4) . . ? B106 B107 B108 108.4(5) . . ? B111 B107 B108 59.4(4) . . ? C304 C305 C306 122.0(10) . . ? N3 C30 C31 177.8(19) . . ? N4 C40 C41 174(2) . . ? C142 N1 C121 156.4(14) . . ? C142 N1 C111 56.8(13) . . ? C121 N1 C111 113.5(10) . . ? C142 N1 C113 108.9(17) . . ? C121 N1 C113 84.2(13) . . ? C111 N1 C113 69.9(16) . . ? C142 N1 C131 59.9(13) . . ? C121 N1 C131 111.0(11) . . ? C111 N1 C131 108.5(11) . . ? C113 N1 C131 163.1(14) . . ? C142 N1 C133 110.2(16) . . ? C121 N1 C133 80.1(12) . . ? C111 N1 C133 166.3(13) . . ? C113 N1 C133 114.7(18) . . ? C131 N1 C133 63.0(13) . . ? C142 N1 C141 93.9(16) . . ? C121 N1 C141 109.7(12) . . ? C111 N1 C141 105.2(16) . . ? C113 N1 C141 57.3(15) . . ? C131 N1 C141 108.7(13) . . ? C133 N1 C141 69.8(16) . . ? C142 N1 C123 105.8(14) . . ? C121 N1 C123 50.6(10) . . ? C111 N1 C123 83.8(13) . . ? C113 N1 C123 111.8(16) . . ? C131 N1 C123 84.4(12) . . ? C133 N1 C123 105.1(16) . . ? C141 N1 C123 160.1(13) . . ? C124 C123 N1 118(2) . . ? C134 C133 N1 122(4) . . ? N1 C113 C114 116(3) . . ? N1 C121 C122 115.3(16) . . ? C112 C111 N1 119(3) . . ? C132 C131 N1 121(2) . . ? C212 C211 N2 122.7(13) . . ? C221 N2 C231 97.9(13) . . ? C221 N2 C211 103.7(11) . . ? C231 N2 C211 129.2(13) . . ? C221 N2 C241 108.5(13) . . ? C231 N2 C241 106.0(13) . . ? C211 N2 C241 109.4(11) . . ? N2 C221 C222 117.3(18) . . ? N2 C231 C232 109.0(16) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.904 _refine_diff_density_min -1.049 _refine_diff_density_rms 0.115