# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1824 data_manuscript loop_ _publ_author_name _publ_author_address 'Andreas Eichhofer' ; Institut f\"ur Nanotechnologie, Forschungszentrum Karlsruhe Postfach 3640 D-76021 Karlsruhe Deutschland ; 'Dieter Fenske' ; Institut f\"ur Anorganische Chemie der Universit\"at Engesserstrasse, Geb\"aude 30.45 D-76128 Karlsruhe Deutschland ; _publ_contact_author ; Institut fur Nanotechnologie, Forschungszentrum Karlsruhe Postfach 3640 D-76021 Karlsruhe Deutschland ; _publ_contact_author_email 'eichhoefer@int.fzk.de' _publ_contact_author_fax 'Int 7427 82 636368' _publ_contact_author_phone 'Int 7247 82 637185' _publ_requested_journal 'Journal of the Chemical Society Dalton Transactions' _publ_section_title ; Syntheses and Structures of new copper(I)-indium(III)-selenide clusters ; data_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural [Cu6In8Se13Cl4(PPh3)6(C4H8O)]*0.5C4H8O _chemical_formula_analytical ? _chemical_formula_sum 'C114 H90 Cl4 Cu6 In8 O1.50 P6 Se13' _chemical_formula_weight 4137.76 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 22.228(4) _cell_length_b 22.989(5) _cell_length_c 28.829(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 14731.6(51) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.866 _exptl_crystal_density_method ? _exptl_crystal_F_000 7808 _exptl_absorpt_coefficient_mu 5.461 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 95174 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0608 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 25505 _reflns_number_observed 21812 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 599 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.026(10) _refine_ls_number_reflns 24906 _refine_ls_number_parameters 1346 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_obs 0.0605 _refine_ls_wR_factor_all 0.1686 _refine_ls_wR_factor_obs 0.1555 _refine_ls_goodness_of_fit_all 1.178 _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_restrained_S_obs 1.190 _refine_ls_shift/esd_max -0.030 _refine_ls_shift/esd_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.90660(4) 1.08112(4) 0.44224(3) 0.0279(2) Uani 1 d . . In2 In 0.99860(4) 0.98937(4) 0.34026(3) 0.0266(2) Uani 1 d . . In3 In 0.99400(4) 1.18802(4) 0.32193(3) 0.0285(2) Uani 1 d . . In4 In 1.09702(4) 1.08902(4) 0.43784(3) 0.0274(2) Uani 1 d . . In5 In 1.00671(4) 0.94856(4) 0.46996(3) 0.0314(2) Uani 1 d . . In6 In 0.85422(4) 1.07514(4) 0.31686(3) 0.0279(2) Uani 1 d . . In7 In 0.99620(4) 1.22153(4) 0.45998(3) 0.0296(2) Uani 1 d . . In8 In 1.13577(4) 1.08111(4) 0.30737(3) 0.0294(2) Uani 1 d . . Se1 Se 0.99925(5) 1.08910(5) 0.38506(4) 0.0242(2) Uani 1 d . . Se2 Se 0.96013(6) 0.90941(6) 0.39428(4) 0.0326(3) Uani 1 d . . Se3 Se 0.92794(6) 1.00935(6) 0.27234(4) 0.0309(3) Uani 1 d . . Se4 Se 1.10679(6) 0.97255(6) 0.31474(4) 0.0318(3) Uani 1 d . . Se5 Se 1.11530(6) 0.98467(6) 0.46365(4) 0.0329(3) Uani 1 d . . Se6 Se 1.17938(6) 1.12441(6) 0.38272(5) 0.0335(3) Uani 1 d . . Se7 Se 1.07052(6) 1.15730(6) 0.50514(4) 0.0328(3) Uani 1 d . . Se8 Se 0.88623(6) 1.18725(6) 0.46396(4) 0.0322(3) Uani 1 d . . Se9 Se 1.04149(6) 1.25500(6) 0.38197(4) 0.0315(3) Uani 1 d . . Se10 Se 0.82019(6) 1.03519(6) 0.39571(4) 0.0324(3) Uani 1 d . . Se11 Se 0.87990(5) 1.18417(6) 0.31423(4) 0.0301(3) Uani 1 d . . Se12 Se 0.93739(6) 1.02160(6) 0.51261(4) 0.0333(3) Uani 1 d . . Se13 Se 1.06148(6) 1.14236(6) 0.25996(4) 0.0302(3) Uani 1 d . . Cu1 Cu 0.98452(7) 1.08004(7) 0.23001(5) 0.0331(3) Uani 1 d . . Cu2 Cu 1.01323(7) 1.08463(7) 0.54541(5) 0.0347(3) Uani 1 d . . Cu3 Cu 1.14378(8) 0.94677(8) 0.38951(6) 0.0380(4) Uani 1 d . . Cu4 Cu 0.85392(7) 1.21959(7) 0.39033(6) 0.0339(4) Uani 1 d . . Cu5 Cu 0.85657(7) 0.93810(7) 0.40504(6) 0.0347(4) Uani 1 d . . Cu6 Cu 1.14441(7) 1.22276(7) 0.38284(6) 0.0348(4) Uani 1 d . . P1 P 0.9713(2) 1.0797(2) 0.15291(11) 0.0334(7) Uani 1 d . . P2 P 1.02789(15) 1.0637(2) 0.62094(11) 0.0354(8) Uani 1 d . . P3 P 0.7753(2) 1.2802(2) 0.38545(12) 0.0363(8) Uani 1 d . . P4 P 1.2104(2) 1.2964(2) 0.38038(14) 0.0362(8) Uani 1 d . . P5 P 0.8030(2) 0.8621(2) 0.43228(14) 0.0390(8) Uani 1 d . . P6 P 1.2197(2) 0.8825(2) 0.39529(13) 0.0442(9) Uani 1 d . . Cl1 Cl 0.9900(2) 1.31362(15) 0.49875(12) 0.0438(8) Uani 1 d . . Cl2 Cl 1.0210(2) 0.8657(2) 0.51871(13) 0.0500(9) Uani 1 d . . Cl3 Cl 0.76393(14) 1.0727(2) 0.27092(12) 0.0442(8) Uani 1 d . . Cl4 Cl 1.2199(2) 1.0777(2) 0.25544(14) 0.0569(11) Uani 1 d . . C1 C 1.0204(7) 1.0255(8) 0.1295(6) 0.056(4) Uani 1 d . . C2 C 1.0022(10) 0.9736(8) 0.1107(6) 0.068(5) Uani 1 d . . H2 H 0.9607(10) 0.9664(8) 0.1087(6) 0.081 Uiso 1 calc R . C3 C 1.0410(16) 0.9314(11) 0.0947(9) 0.114(11) Uani 1 d . . H3 H 1.0263(16) 0.8950(11) 0.0850(9) 0.137 Uiso 1 calc R . C4 C 1.1047(13) 0.9441(13) 0.0930(8) 0.096(9) Uani 1 d . . H4 H 1.1315(13) 0.9198(13) 0.0768(8) 0.115 Uiso 1 calc R . C5 C 1.1254(11) 0.9944(17) 0.1164(11) 0.122(12) Uani 1 d . . H5 H 1.1668(11) 0.9993(17) 0.1215(11) 0.146 Uiso 1 calc R . C6 C 1.0850(10) 1.0375(11) 0.1324(7) 0.083(7) Uani 1 d . . H6 H 1.0992(10) 1.0729(11) 0.1446(7) 0.100 Uiso 1 calc R . C7 C 0.9874(7) 1.1460(7) 0.1194(6) 0.050(4) Uani 1 d . . C8 C 0.9659(8) 1.1978(7) 0.1403(7) 0.059(5) Uani 1 d . . H8 H 0.9497(8) 1.1984(7) 0.1704(7) 0.071 Uiso 1 calc R . C9 C 0.9709(10) 1.2509(9) 0.1115(9) 0.081(7) Uani 1 d . . H9 H 0.9574(10) 1.2868(9) 0.1232(9) 0.098 Uiso 1 calc R . C10 C 0.9941(11) 1.2481(10) 0.0695(9) 0.092(8) Uani 1 d . . H10 H 0.9952(11) 1.2817(10) 0.0509(9) 0.110 Uiso 1 calc R . C11 C 1.0165(11) 1.1977(11) 0.0527(6) 0.081(7) Uani 1 d . . H11 H 1.0350(11) 1.1979(11) 0.0234(6) 0.098 Uiso 1 calc R . C12 C 1.0134(7) 1.1458(8) 0.0769(5) 0.053(4) Uani 1 d . . H12 H 1.0290(7) 1.1113(8) 0.0642(5) 0.063 Uiso 1 calc R . C13 C 0.8977(6) 1.0630(6) 0.1309(4) 0.033(3) Uani 1 d . . C14 C 0.8494(7) 1.0585(7) 0.1617(5) 0.046(4) Uani 1 d . . H14 H 0.8565(7) 1.0606(7) 0.1938(5) 0.055 Uiso 1 calc R . C15 C 0.7915(7) 1.0510(8) 0.1455(6) 0.051(4) Uani 1 d . . H15 H 0.7593(7) 1.0495(8) 0.1667(6) 0.061 Uiso 1 calc R . C16 C 0.7804(8) 1.0457(7) 0.0992(6) 0.053(4) Uani 1 d . . H16 H 0.7410(8) 1.0391(7) 0.0885(6) 0.064 Uiso 1 calc R . C17 C 0.8259(8) 1.0501(8) 0.0693(6) 0.061(5) Uani 1 d . . H17 H 0.8179(8) 1.0466(8) 0.0373(6) 0.073 Uiso 1 calc R . C18 C 0.8838(8) 1.0595(9) 0.0836(6) 0.062(5) Uani 1 d . . H18 H 0.9146(8) 1.0637(9) 0.0614(6) 0.075 Uiso 1 calc R . C19 C 0.9667(6) 1.0235(7) 0.6463(4) 0.043(4) Uani 1 d . . C20 C 0.9084(6) 1.0412(9) 0.6392(6) 0.056(4) Uani 1 d . . H20 H 0.9023(6) 1.0737(9) 0.6200(6) 0.067 Uiso 1 calc R . C21 C 0.8580(8) 1.0149(10) 0.6581(8) 0.072(6) Uani 1 d . . H21 H 0.8192(8) 1.0292(10) 0.6521(8) 0.087 Uiso 1 calc R . C22 C 0.8672(9) 0.9670(14) 0.6860(8) 0.095(8) Uani 1 d . . H22 H 0.8340(9) 0.9498(14) 0.7008(8) 0.114 Uiso 1 calc R . C23 C 0.9261(10) 0.9425(12) 0.6932(9) 0.110(10) Uani 1 d . . H23 H 0.9307(10) 0.9077(12) 0.7100(9) 0.132 Uiso 1 calc R . C24 C 0.9781(9) 0.9718(11) 0.6744(8) 0.084(7) Uani 1 d . . H24 H 1.0174(9) 0.9583(11) 0.6799(8) 0.100 Uiso 1 calc R . C25 C 1.0374(6) 1.1255(7) 0.6597(5) 0.038(3) Uani 1 d . . C26 C 1.0227(9) 1.1229(9) 0.7063(5) 0.061(5) Uani 1 d . . H26 H 1.0080(9) 1.0880(9) 0.7190(5) 0.074 Uiso 1 calc R . C27 C 1.0295(11) 1.1713(10) 0.7343(6) 0.075(6) Uani 1 d . . H27 H 1.0202(11) 1.1686(10) 0.7660(6) 0.090 Uiso 1 calc R . C28 C 1.0493(9) 1.2220(10) 0.7169(7) 0.073(6) Uani 1 d . . H28 H 1.0534(9) 1.2545(10) 0.7365(7) 0.087 Uiso 1 calc R . C29 C 1.0638(7) 1.2268(8) 0.6706(6) 0.053(4) Uani 1 d . . H29 H 1.0778(7) 1.2621(8) 0.6582(6) 0.064 Uiso 1 calc R . C30 C 1.0570(6) 1.1772(7) 0.6422(5) 0.040(3) Uani 1 d . . H30 H 1.0662(6) 1.1799(7) 0.6104(5) 0.048 Uiso 1 calc R . C31 C 1.0917(6) 1.0170(7) 0.6308(4) 0.040(3) Uani 1 d . . C32 C 1.1360(7) 1.0295(7) 0.6632(5) 0.045(4) Uani 1 d . . H32 H 1.1334(7) 1.0629(7) 0.6818(5) 0.054 Uiso 1 calc R . C33 C 1.1853(8) 0.9909(9) 0.6677(8) 0.076(6) Uani 1 d . . H33 H 1.2145(8) 0.9978(9) 0.6906(8) 0.091 Uiso 1 calc R . C34 C 1.1907(8) 0.9453(8) 0.6399(7) 0.060(5) Uani 1 d . . H34 H 1.2239(8) 0.9201(8) 0.6428(7) 0.072 Uiso 1 calc R . C35 C 1.1491(9) 0.9353(9) 0.6081(7) 0.067(5) Uani 1 d . . H35 H 1.1539(9) 0.9022(9) 0.5893(7) 0.080 Uiso 1 calc R . C36 C 1.0991(8) 0.9697(9) 0.6001(5) 0.057(4) Uani 1 d . . H36 H 1.0718(8) 0.9621(9) 0.5759(5) 0.068 Uiso 1 calc R . C37 C 0.7140(6) 1.2326(7) 0.3883(5) 0.043(3) Uani 1 d . . C38 C 0.7100(8) 1.1854(8) 0.3580(7) 0.060(5) Uani 1 d . . H38 H 0.7378(8) 1.1827(8) 0.3336(7) 0.071 Uiso 1 calc R . C39 C 0.6660(9) 1.1415(10) 0.3624(8) 0.074(6) Uani 1 d . . H39 H 0.6654(9) 1.1099(10) 0.3417(8) 0.089 Uiso 1 calc R . C40 C 0.6269(10) 1.1451(10) 0.3949(8) 0.080(6) Uani 1 d . . H40 H 0.5980(10) 1.1155(10) 0.3978(8) 0.096 Uiso 1 calc R . C41 C 0.6260(9) 1.1929(11) 0.4269(8) 0.082(7) Uani 1 d . . H41 H 0.5959(9) 1.1957(11) 0.4497(8) 0.099 Uiso 1 calc R . C42 C 0.6688(7) 1.2331(8) 0.4234(6) 0.056(4) Uani 1 d . . H42 H 0.6693(7) 1.2634(8) 0.4453(6) 0.067 Uiso 1 calc R . C43 C 0.7655(6) 1.3220(7) 0.3322(5) 0.044(4) Uani 1 d . . C44 C 0.7184(7) 1.3182(8) 0.3022(5) 0.052(4) Uani 1 d . . H44 H 0.6889(7) 1.2895(8) 0.3070(5) 0.062 Uiso 1 calc R . C45 C 0.7131(10) 1.3551(10) 0.2652(6) 0.074(6) Uani 1 d . . H45 H 0.6803(10) 1.3512(10) 0.2448(6) 0.089 Uiso 1 calc R . C46 C 0.7527(11) 1.3954(9) 0.2581(7) 0.076(7) Uani 1 d . . H46 H 0.7474(11) 1.4218(9) 0.2336(7) 0.092 Uiso 1 calc R . C47 C 0.8027(9) 1.3996(9) 0.2863(7) 0.063(5) Uani 1 d . . H47 H 0.8315(9) 1.4285(9) 0.2800(7) 0.076 Uiso 1 calc R . C48 C 0.8116(10) 1.3621(9) 0.3239(6) 0.067(5) Uani 1 d . . H48 H 0.8464(10) 1.3637(9) 0.3424(6) 0.081 Uiso 1 calc R . C49 C 0.7621(6) 1.3353(7) 0.4292(5) 0.041(3) Uani 1 d . . C50 C 0.7927(7) 1.3345(7) 0.4700(5) 0.048(4) Uani 1 d . . H50 H 0.8180(7) 1.3028(7) 0.4767(5) 0.058 Uiso 1 calc R . C51 C 0.7874(8) 1.3802(7) 0.5026(5) 0.054(4) Uani 1 d . . H51 H 0.8108(8) 1.3801(7) 0.5297(5) 0.064 Uiso 1 calc R . C52 C 0.7474(7) 1.4250(7) 0.4941(5) 0.046(4) Uani 1 d . . H52 H 0.7420(7) 1.4549(7) 0.5159(5) 0.055 Uiso 1 calc R . C53 C 0.7157(7) 1.4250(7) 0.4532(5) 0.049(4) Uani 1 d . . H53 H 0.6892(7) 1.4558(7) 0.4468(5) 0.059 Uiso 1 calc R . C54 C 0.7220(7) 1.3811(8) 0.4217(5) 0.054(4) Uani 1 d . . H54 H 0.6988(7) 1.3817(8) 0.3944(5) 0.065 Uiso 1 calc R . C55 C 1.2037(6) 1.3358(6) 0.3265(5) 0.037(3) Uani 1 d . . C56 C 1.1989(8) 1.3032(8) 0.2857(6) 0.057(4) Uani 1 d . . H56 H 1.1971(8) 1.2624(8) 0.2863(6) 0.069 Uiso 1 calc R . C57 C 1.1968(9) 1.3344(11) 0.2431(6) 0.075(6) Uani 1 d . . H57 H 1.1973(9) 1.3129(11) 0.2154(6) 0.090 Uiso 1 calc R . C58 C 1.1943(8) 1.3933(8) 0.2400(6) 0.054(4) Uani 1 d . . H58 H 1.1914(8) 1.4122(8) 0.2112(6) 0.064 Uiso 1 calc R . C59 C 1.1962(8) 1.4248(8) 0.2819(6) 0.057(4) Uani 1 d . . H59 H 1.1941(8) 1.4657(8) 0.2812(6) 0.068 Uiso 1 calc R . C60 C 1.2012(7) 1.3965(8) 0.3240(6) 0.048(4) Uani 1 d . . H60 H 1.2030(7) 1.4185(8) 0.3515(6) 0.058 Uiso 1 calc R . C61 C 1.2020(7) 1.3495(7) 0.4272(5) 0.047(4) Uani 1 d . . C62 C 1.2496(11) 1.3730(11) 0.4505(8) 0.098(9) Uani 1 d . . H62 H 1.2886(11) 1.3618(11) 0.4416(8) 0.118 Uiso 1 calc R . C63 C 1.2438(12) 1.4123(13) 0.4863(8) 0.104(10) Uani 1 d . . H63 H 1.2777(12) 1.4279(13) 0.5012(8) 0.124 Uiso 1 calc R . C64 C 1.1895(13) 1.4270(11) 0.4989(7) 0.090(7) Uani 1 d . . H64 H 1.1853(13) 1.4523(11) 0.5243(7) 0.108 Uiso 1 calc R . C65 C 1.1362(11) 1.4071(10) 0.4764(9) 0.096(8) Uani 1 d . . H65 H 1.0976(11) 1.4198(10) 0.4850(9) 0.115 Uiso 1 calc R . C66 C 1.1456(9) 1.3670(9) 0.4404(7) 0.072(6) Uani 1 d . . H66 H 1.1121(9) 1.3516(9) 0.4247(7) 0.086 Uiso 1 calc R . C67 C 1.2900(7) 1.2793(7) 0.3827(6) 0.049(4) Uani 1 d . . C68 C 1.3317(7) 1.3070(8) 0.3560(7) 0.062(5) Uani 1 d . . H68 H 1.3193(7) 1.3335(8) 0.3330(7) 0.074 Uiso 1 calc R . C69 C 1.3921(8) 1.2961(9) 0.3626(7) 0.068(5) Uani 1 d . . H69 H 1.4209(8) 1.3158(9) 0.3446(7) 0.082 Uiso 1 calc R . C70 C 1.4106(7) 1.2559(8) 0.3961(7) 0.061(5) Uani 1 d . . H70 H 1.4518(7) 1.2489(8) 0.4010(7) 0.073 Uiso 1 calc R . C71 C 1.3693(7) 1.2273(8) 0.4211(6) 0.052(4) Uani 1 d . . H71 H 1.3813(7) 1.1997(8) 0.4432(6) 0.063 Uiso 1 calc R . C72 C 1.3084(6) 1.2390(7) 0.4140(6) 0.047(4) Uani 1 d . . H72 H 1.2795(6) 1.2185(7) 0.4313(6) 0.056 Uiso 1 calc R . C73 C 0.8355(6) 0.8379(6) 0.4871(5) 0.040(3) Uani 1 d . . C74 C 0.8468(7) 0.7789(7) 0.4966(5) 0.049(4) Uani 1 d . . H74 H 0.8404(7) 0.7499(7) 0.4741(5) 0.059 Uiso 1 calc R . C75 C 0.8681(8) 0.7651(10) 0.5416(6) 0.065(5) Uani 1 d . . H75 H 0.8765(8) 0.7260(10) 0.5488(6) 0.078 Uiso 1 calc R . C76 C 0.8769(10) 0.8067(12) 0.5753(7) 0.084(7) Uani 1 d . . H76 H 0.8886(10) 0.7967(12) 0.6056(7) 0.100 Uiso 1 calc R . C77 C 0.8673(9) 0.8667(11) 0.5617(7) 0.079(7) Uani 1 d . . H77 H 0.8763(9) 0.8966(11) 0.5828(7) 0.094 Uiso 1 calc R . C78 C 0.8458(8) 0.8809(7) 0.5192(6) 0.053(4) Uani 1 d . . H78 H 0.8379(8) 0.9199(7) 0.5117(6) 0.063 Uiso 1 calc R . C79 C 0.7253(7) 0.8699(7) 0.4492(6) 0.045(4) Uani 1 d . . C80 C 0.6974(8) 0.8321(9) 0.4789(7) 0.065(5) Uani 1 d . . H80 H 0.7205(8) 0.8024(9) 0.4925(7) 0.078 Uiso 1 calc R . C81 C 0.6366(7) 0.8355(11) 0.4901(7) 0.074(6) Uani 1 d . . H81 H 0.6180(7) 0.8082(11) 0.5096(7) 0.089 Uiso 1 calc R . C82 C 0.6048(8) 0.8821(12) 0.4705(8) 0.085(7) Uani 1 d . . H82 H 0.5639(8) 0.8863(12) 0.4781(8) 0.102 Uiso 1 calc R . C83 C 0.6309(7) 0.9235(10) 0.4399(8) 0.077(6) Uani 1 d . . H83 H 0.6081(7) 0.9536(10) 0.4265(8) 0.092 Uiso 1 calc R . C84 C 0.6934(7) 0.9167(9) 0.4306(7) 0.065(5) Uani 1 d . . H84 H 0.7133(7) 0.9440(9) 0.4118(7) 0.078 Uiso 1 calc R . C85 C 0.8031(6) 0.8010(6) 0.3932(5) 0.036(3) Uani 1 d . . C86 C 0.7508(7) 0.7761(8) 0.3745(6) 0.053(4) Uani 1 d . . H86 H 0.7130(7) 0.7916(8) 0.3823(6) 0.063 Uiso 1 calc R . C87 C 0.7541(8) 0.7289(8) 0.3446(6) 0.059(5) Uani 1 d . . H87 H 0.7188(8) 0.7131(8) 0.3318(6) 0.070 Uiso 1 calc R . C88 C 0.8083(9) 0.7058(7) 0.3338(5) 0.053(4) Uani 1 d . . H88 H 0.8102(9) 0.6736(7) 0.3137(5) 0.064 Uiso 1 calc R . C89 C 0.8586(8) 0.7275(7) 0.3508(5) 0.051(4) Uani 1 d . . H89 H 0.8958(8) 0.7110(7) 0.3424(5) 0.061 Uiso 1 calc R . C90 C 0.8570(7) 0.7744(7) 0.3810(5) 0.044(3) Uani 1 d . . H90 H 0.8932(7) 0.7886(7) 0.3935(5) 0.052 Uiso 1 calc R . C91 C 1.2412(8) 0.8686(7) 0.4547(6) 0.050(4) Uani 1 d . . C92 C 1.2933(12) 0.8896(10) 0.4734(6) 0.083(7) Uani 1 d . . H92 H 1.3208(12) 0.9100(10) 0.4547(6) 0.100 Uiso 1 calc R . C93 C 1.3055(11) 0.8806(11) 0.5199(8) 0.087(7) Uani 1 d . . H93 H 1.3406(11) 0.8969(11) 0.5327(8) 0.105 Uiso 1 calc R . C94 C 1.2681(16) 0.8486(11) 0.5479(7) 0.101(10) Uani 1 d . . H94 H 1.2794(16) 0.8408(11) 0.5787(7) 0.121 Uiso 1 calc R . C95 C 1.2139(13) 0.8279(9) 0.5313(7) 0.077(6) Uani 1 d . . H95 H 1.1872(13) 0.8071(9) 0.5504(7) 0.093 Uiso 1 calc R . C96 C 1.2006(9) 0.8392(8) 0.4846(6) 0.058(4) Uani 1 d . . H96 H 1.1634(9) 0.8268(8) 0.4726(6) 0.069 Uiso 1 calc R . C97 C 1.2876(7) 0.9091(8) 0.3676(6) 0.053(4) Uani 1 d . . C98 C 1.2870(8) 0.9668(9) 0.3538(8) 0.071(6) Uani 1 d . . H98 H 1.2539(8) 0.9912(9) 0.3593(8) 0.086 Uiso 1 calc R . C99 C 1.3386(15) 0.9863(16) 0.3313(14) 0.151(17) Uani 1 d . . H99 H 1.3427(15) 1.0253(16) 0.3220(14) 0.182 Uiso 1 calc R . C100 C 1.3867(12) 0.9434(23) 0.3228(11) 0.146(17) Uani 1 d . . H100 H 1.4192(12) 0.9544(23) 0.3038(11) 0.176 Uiso 1 calc R . C101 C 1.3866(13) 0.8949(13) 0.3388(9) 0.093(8) Uani 1 d . . H101 H 1.4217(13) 0.8721(13) 0.3374(9) 0.112 Uiso 1 calc R . C102 C 1.3357(9) 0.8727(9) 0.3593(6) 0.063(5) Uani 1 d . . H102 H 1.3337(9) 0.8332(9) 0.3674(6) 0.075 Uiso 1 calc R . C103 C 1.2081(7) 0.8123(7) 0.3695(5) 0.046(4) Uani 1 d . . C104 C 1.2317(12) 0.7597(9) 0.3875(7) 0.094(9) Uani 1 d . . H104 H 1.2522(12) 0.7599(9) 0.4160(7) 0.113 Uiso 1 calc R . C105 C 1.2250(13) 0.7083(10) 0.3634(9) 0.102(9) Uani 1 d . . H105 H 1.2392(13) 0.6736(10) 0.3767(9) 0.122 Uiso 1 calc R . C106 C 1.1980(10) 0.7064(8) 0.3202(7) 0.074(6) Uani 1 d . . H106 H 1.1960(10) 0.6710(8) 0.3039(7) 0.089 Uiso 1 calc R . C107 C 1.1735(9) 0.7574(8) 0.3005(7) 0.067(5) Uani 1 d . . H107 H 1.1543(9) 0.7572(8) 0.2715(7) 0.080 Uiso 1 calc R . C108 C 1.1795(8) 0.8099(7) 0.3276(5) 0.054(4) Uani 1 d . . H108 H 1.1629(8) 0.8444(7) 0.3157(5) 0.064 Uiso 1 calc R . O1 O 0.9870(4) 1.2727(4) 0.2727(3) 0.042(2) Uiso 1 d . . C109 C 1.0320(11) 1.2931(11) 0.2449(9) 0.089(7) Uiso 1 d . . C110 C 1.0193(12) 1.3548(12) 0.2308(9) 0.096(7) Uiso 1 d . . C111 C 0.9858(12) 1.3731(12) 0.2774(9) 0.096(7) Uiso 1 d . . C112 C 0.9511(8) 1.3227(8) 0.2884(6) 0.060(4) Uiso 1 d . . O2 O 0.0205(11) 0.2297(12) 0.8546(9) 0.067(7) Uiso 0.50 d P . C113 C -0.0094(22) 0.2064(22) 0.8951(16) 0.087(13) Uiso 0.50 d P . C114 C -0.0646(18) 0.2484(19) 0.8913(14) 0.067(10) Uiso 0.50 d P . C115 C -0.0563(23) 0.2893(25) 0.8693(19) 0.095(14) Uiso 0.50 d P . C116 C -0.0039(17) 0.2769(16) 0.8378(13) 0.063(9) Uiso 0.50 d P . 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 In1 0.0294(4) 0.0273(5) 0.0271(4) -0.0021(3) 0.0015(3) -0.0012(3) In2 0.0282(4) 0.0246(4) 0.0269(4) -0.0005(3) 0.0002(4) 0.0002(4) In3 0.0278(4) 0.0268(4) 0.0308(4) -0.0019(3) 0.0009(3) -0.0003(4) In4 0.0297(4) 0.0236(5) 0.0288(4) -0.0009(3) -0.0016(3) 0.0001(3) In5 0.0394(5) 0.0257(5) 0.0291(4) 0.0026(3) -0.0036(4) -0.0031(4) In6 0.0278(4) 0.0268(5) 0.0290(4) -0.0014(3) -0.0018(3) -0.0004(3) In7 0.0318(4) 0.0249(5) 0.0322(4) -0.0034(3) 0.0005(4) -0.0007(4) In8 0.0285(4) 0.0289(5) 0.0308(4) 0.0010(4) 0.0042(3) 0.0027(3) Se1 0.0254(5) 0.0217(6) 0.0254(5) -0.0007(4) -0.0001(5) -0.0001(5) Se2 0.0397(7) 0.0255(7) 0.0326(7) 0.0003(5) -0.0012(5) -0.0042(5) Se3 0.0342(6) 0.0310(7) 0.0275(6) -0.0040(5) -0.0031(5) 0.0037(5) Se4 0.0329(6) 0.0293(7) 0.0331(6) -0.0018(5) 0.0015(5) 0.0049(5) Se5 0.0346(7) 0.0293(7) 0.0349(7) 0.0026(5) -0.0044(5) 0.0019(5) Se6 0.0291(6) 0.0320(8) 0.0394(7) -0.0013(5) 0.0000(5) -0.0023(5) Se7 0.0395(7) 0.0282(7) 0.0305(6) -0.0038(5) -0.0051(5) 0.0016(5) Se8 0.0317(6) 0.0298(7) 0.0351(7) -0.0054(5) 0.0018(5) 0.0030(5) Se9 0.0338(6) 0.0269(7) 0.0340(7) -0.0023(5) 0.0010(5) -0.0037(5) Se10 0.0319(6) 0.0328(8) 0.0324(6) 0.0002(5) 0.0005(5) -0.0046(5) Se11 0.0285(6) 0.0276(7) 0.0343(6) 0.0014(5) -0.0016(5) 0.0018(5) Se12 0.0393(7) 0.0329(7) 0.0277(6) 0.0003(5) -0.0012(5) -0.0008(5) Se13 0.0317(6) 0.0305(7) 0.0282(6) 0.0014(5) 0.0034(5) 0.0031(5) Cu1 0.0348(8) 0.0364(9) 0.0282(7) -0.0016(6) -0.0029(6) 0.0011(6) Cu2 0.0391(8) 0.0369(9) 0.0282(7) 0.0019(6) -0.0039(6) -0.0010(7) Cu3 0.0436(9) 0.0325(10) 0.0379(8) -0.0003(7) -0.0053(7) 0.0081(7) Cu4 0.0318(8) 0.0330(10) 0.0370(8) -0.0040(7) 0.0000(7) 0.0059(7) Cu5 0.0391(8) 0.0289(9) 0.0361(8) 0.0001(6) 0.0010(7) -0.0069(7) Cu6 0.0338(8) 0.0281(9) 0.0424(9) -0.0007(7) 0.0004(7) -0.0039(7) P1 0.041(2) 0.032(2) 0.028(2) 0.0002(14) -0.0002(13) -0.0021(14) P2 0.032(2) 0.046(2) 0.027(2) 0.0018(14) -0.0032(13) -0.0020(15) P3 0.040(2) 0.039(2) 0.030(2) -0.0011(15) 0.0031(14) 0.015(2) P4 0.031(2) 0.026(2) 0.052(2) 0.0015(15) -0.002(2) -0.0059(13) P5 0.037(2) 0.033(2) 0.047(2) -0.001(2) 0.006(2) -0.0076(15) P6 0.055(2) 0.038(2) 0.040(2) -0.003(2) -0.011(2) 0.021(2) Cl1 0.046(2) 0.030(2) 0.055(2) -0.0159(14) 0.006(2) 0.0012(14) Cl2 0.072(3) 0.029(2) 0.049(2) 0.0143(15) -0.007(2) -0.002(2) Cl3 0.031(2) 0.059(2) 0.042(2) -0.012(2) -0.0117(14) 0.0049(15) Cl4 0.044(2) 0.071(3) 0.056(2) 0.011(2) 0.028(2) 0.014(2) C1 0.049(9) 0.069(12) 0.049(9) 0.004(8) -0.003(7) 0.021(8) C2 0.092(14) 0.052(11) 0.059(10) 0.001(8) -0.011(11) 0.025(10) C3 0.185(32) 0.064(17) 0.094(18) -0.015(13) -0.019(18) 0.067(18) C4 0.104(20) 0.119(23) 0.065(13) -0.001(14) -0.014(13) 0.060(17) C5 0.058(14) 0.193(36) 0.115(22) 0.020(23) 0.025(14) 0.041(18) C6 0.077(14) 0.099(18) 0.075(13) -0.012(12) -0.001(11) 0.023(12) C7 0.048(9) 0.035(9) 0.065(10) 0.013(7) -0.013(7) -0.012(7) C8 0.063(10) 0.030(10) 0.085(13) 0.023(8) 0.011(9) 0.017(7) C9 0.081(14) 0.052(13) 0.111(18) 0.046(12) -0.006(13) -0.004(10) C10 0.108(17) 0.071(16) 0.097(17) 0.045(13) -0.048(15) -0.059(14) C11 0.115(18) 0.085(17) 0.044(10) 0.019(10) -0.009(10) -0.062(14) C12 0.060(10) 0.056(10) 0.043(8) 0.004(7) 0.002(7) -0.015(8) C13 0.041(7) 0.035(8) 0.022(6) 0.004(5) 0.000(5) -0.012(6) C14 0.057(9) 0.051(10) 0.029(7) 0.011(6) 0.001(6) -0.007(7) C15 0.045(8) 0.060(11) 0.047(9) -0.008(7) -0.003(7) -0.010(7) C16 0.067(11) 0.046(10) 0.047(9) -0.001(7) -0.017(8) 0.001(8) C17 0.070(11) 0.063(12) 0.049(9) 0.000(8) -0.017(9) -0.017(9) C18 0.047(9) 0.096(15) 0.043(9) -0.003(9) -0.001(7) -0.021(9) C19 0.037(7) 0.069(11) 0.023(6) 0.019(6) -0.001(5) 0.009(7) C20 0.030(7) 0.075(13) 0.062(10) 0.012(9) -0.007(7) -0.011(7) C21 0.038(9) 0.077(15) 0.102(16) -0.020(12) -0.003(10) -0.008(9) C22 0.043(11) 0.159(26) 0.082(15) 0.004(16) 0.000(10) -0.037(13) C23 0.082(15) 0.133(23) 0.115(19) 0.092(18) 0.000(13) -0.040(15) C24 0.055(11) 0.104(18) 0.091(15) 0.050(13) 0.004(10) 0.002(11) C25 0.027(6) 0.058(10) 0.029(6) -0.014(6) -0.006(5) 0.008(6) C26 0.080(12) 0.069(12) 0.035(8) -0.003(8) 0.005(8) -0.016(9) C27 0.112(17) 0.077(16) 0.038(9) -0.019(9) 0.004(10) 0.025(12) C28 0.071(12) 0.082(16) 0.065(12) -0.050(12) -0.020(9) 0.014(11) C29 0.041(8) 0.062(11) 0.057(10) -0.009(8) -0.003(7) -0.008(7) C30 0.032(7) 0.049(10) 0.037(7) 0.001(6) 0.002(6) -0.010(6) C31 0.046(8) 0.055(10) 0.021(6) -0.010(6) 0.005(5) -0.008(7) C32 0.048(8) 0.042(9) 0.046(8) -0.004(6) -0.015(7) -0.015(7) C33 0.045(9) 0.076(14) 0.106(16) -0.013(12) -0.056(10) 0.015(9) C34 0.044(9) 0.048(11) 0.088(13) -0.007(9) -0.013(9) 0.011(7) C35 0.080(13) 0.059(12) 0.061(11) -0.003(9) 0.026(10) 0.022(10) C36 0.058(10) 0.084(14) 0.028(7) -0.002(7) 0.002(7) 0.003(9) C37 0.044(8) 0.046(9) 0.037(7) -0.001(6) 0.008(6) 0.016(7) C38 0.049(9) 0.055(12) 0.074(12) -0.020(9) 0.005(8) 0.014(8) C39 0.062(12) 0.064(14) 0.097(16) 0.001(11) 0.014(11) -0.013(9) C40 0.089(15) 0.058(14) 0.092(15) 0.016(11) 0.014(12) -0.022(11) C41 0.064(12) 0.084(17) 0.099(16) 0.035(13) 0.035(11) 0.004(11) C42 0.054(10) 0.052(11) 0.062(11) 0.016(8) 0.011(8) 0.006(8) C43 0.035(7) 0.060(11) 0.037(8) -0.011(7) 0.007(6) 0.014(7) C44 0.043(8) 0.065(11) 0.046(9) 0.012(8) 0.002(7) 0.002(7) C45 0.097(15) 0.098(17) 0.028(8) 0.018(9) -0.002(9) 0.021(13) C46 0.119(18) 0.053(12) 0.057(12) 0.013(9) 0.048(13) 0.023(12) C47 0.068(12) 0.059(13) 0.063(11) 0.017(9) 0.003(9) -0.011(9) C48 0.085(13) 0.079(14) 0.037(8) 0.009(9) 0.012(9) -0.012(11) C49 0.046(8) 0.049(9) 0.029(7) 0.001(6) 0.012(6) 0.012(6) C50 0.055(9) 0.049(10) 0.040(8) -0.007(7) -0.008(7) 0.016(7) C51 0.082(12) 0.046(10) 0.034(8) -0.016(7) -0.012(8) 0.020(8) C52 0.051(8) 0.033(9) 0.054(9) -0.007(7) 0.003(7) 0.003(7) C53 0.059(9) 0.048(10) 0.041(8) -0.018(7) 0.003(7) 0.020(8) C54 0.057(9) 0.068(12) 0.038(8) 0.000(7) -0.005(7) 0.040(9) C55 0.037(7) 0.038(9) 0.037(7) -0.006(6) 0.010(6) -0.011(6) C56 0.070(11) 0.057(11) 0.045(9) -0.021(8) 0.004(8) -0.002(8) C57 0.068(12) 0.112(20) 0.044(10) -0.015(11) -0.004(9) 0.006(11) C58 0.070(11) 0.051(11) 0.040(8) 0.002(7) -0.005(8) 0.015(8) C59 0.066(10) 0.042(10) 0.063(11) 0.006(8) -0.015(8) 0.008(8) C60 0.046(8) 0.054(11) 0.044(8) 0.002(7) -0.001(7) -0.008(7) C61 0.060(10) 0.033(9) 0.047(8) -0.002(6) -0.022(7) -0.003(7) C62 0.093(15) 0.103(19) 0.100(17) -0.031(14) -0.073(14) 0.047(14) C63 0.094(17) 0.132(23) 0.085(15) -0.060(16) -0.061(14) 0.034(16) C64 0.135(22) 0.077(16) 0.057(12) -0.030(11) -0.010(13) 0.000(15) C65 0.102(17) 0.073(16) 0.113(18) -0.038(13) 0.057(15) -0.035(13) C66 0.071(12) 0.070(14) 0.075(12) -0.026(10) 0.022(10) -0.022(10) C67 0.041(8) 0.038(9) 0.069(11) 0.004(8) -0.010(7) -0.010(6) C68 0.034(8) 0.057(12) 0.094(14) 0.030(10) -0.006(8) -0.012(7) C69 0.050(10) 0.062(13) 0.092(14) 0.019(10) 0.021(9) -0.007(8) C70 0.032(8) 0.060(12) 0.090(13) 0.009(10) 0.010(8) -0.002(7) C71 0.052(9) 0.048(10) 0.056(9) 0.011(8) -0.013(8) -0.002(7) C72 0.030(7) 0.055(10) 0.056(9) 0.015(8) -0.002(6) -0.013(7) C73 0.049(8) 0.035(9) 0.035(7) -0.014(6) 0.016(6) -0.007(6) C74 0.052(9) 0.048(10) 0.047(9) -0.003(7) -0.004(7) -0.009(7) C75 0.073(12) 0.078(14) 0.045(9) 0.024(9) 0.003(8) -0.012(10) C76 0.084(14) 0.117(21) 0.049(11) 0.026(12) -0.006(10) -0.023(14) C77 0.061(12) 0.118(20) 0.056(11) -0.035(12) -0.005(9) -0.023(12) C78 0.067(11) 0.031(9) 0.060(10) 0.005(7) -0.003(8) -0.014(7) C79 0.049(8) 0.032(9) 0.055(9) -0.012(7) 0.003(7) -0.003(6) C80 0.055(10) 0.069(13) 0.070(12) 0.006(9) 0.018(9) -0.011(9) C81 0.029(8) 0.114(18) 0.078(13) 0.019(12) 0.009(8) -0.005(10) C82 0.036(9) 0.135(21) 0.083(14) -0.032(14) 0.020(9) -0.028(11) C83 0.038(9) 0.083(15) 0.108(16) 0.009(13) 0.003(10) 0.033(9) C84 0.045(9) 0.077(14) 0.073(12) -0.015(10) 0.020(8) 0.003(9) C85 0.032(7) 0.034(8) 0.041(7) -0.002(6) 0.009(6) -0.008(5) C86 0.044(8) 0.048(10) 0.066(10) -0.008(8) 0.005(8) 0.000(7) C87 0.058(10) 0.060(12) 0.058(10) -0.012(9) -0.015(8) -0.021(9) C88 0.085(13) 0.036(10) 0.039(8) -0.008(7) 0.011(8) -0.009(8) C89 0.064(10) 0.045(10) 0.045(8) -0.005(7) 0.017(8) 0.027(8) C90 0.048(8) 0.043(9) 0.040(8) 0.002(6) 0.008(6) -0.002(7) C91 0.074(11) 0.031(9) 0.045(8) 0.003(7) -0.007(8) 0.027(7) C92 0.133(20) 0.080(15) 0.036(9) -0.005(9) -0.022(11) 0.040(14) C93 0.091(16) 0.093(18) 0.077(15) -0.013(13) -0.041(13) 0.003(13) C94 0.186(30) 0.074(17) 0.043(11) 0.014(11) -0.003(15) 0.055(18) C95 0.129(20) 0.049(13) 0.054(11) 0.009(9) 0.008(12) 0.021(12) C96 0.070(11) 0.047(11) 0.055(10) 0.010(8) -0.001(8) 0.014(8) C97 0.044(8) 0.052(11) 0.063(10) -0.017(8) -0.008(7) 0.011(7) C98 0.045(10) 0.071(14) 0.099(15) 0.020(11) -0.019(10) -0.009(9) C99 0.113(24) 0.134(29) 0.207(37) 0.076(27) -0.074(25) -0.080(22) C100 0.050(14) 0.285(57) 0.104(23) 0.018(30) 0.001(14) -0.019(24) C101 0.095(19) 0.104(22) 0.081(17) 0.019(15) -0.013(14) -0.007(15) C102 0.073(12) 0.064(13) 0.051(10) -0.011(8) -0.015(9) 0.012(9) C103 0.061(9) 0.033(9) 0.043(8) -0.005(6) -0.004(7) 0.013(7) C104 0.154(22) 0.061(14) 0.067(12) -0.022(10) -0.066(14) 0.055(14) C105 0.155(24) 0.045(14) 0.105(19) -0.005(12) -0.052(17) 0.015(14) C106 0.107(16) 0.035(11) 0.081(13) -0.037(9) -0.039(12) 0.016(9) C107 0.092(14) 0.037(11) 0.073(12) -0.013(8) 0.002(10) 0.004(9) C108 0.081(12) 0.037(9) 0.043(8) 0.006(7) -0.018(8) 0.004(8) _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 In1 Se12 2.541(2) . ? In1 Se8 2.559(2) . ? In1 Se10 2.570(2) . ? In1 Se1 2.6442(14) . ? In2 Se4 2.544(2) . ? In2 Se3 2.5518(15) . ? In2 Se2 2.557(2) . ? In2 Se1 2.6314(14) . ? In3 O1 2.415(10) . ? In3 Se9 2.546(2) . ? In3 Se11 2.5475(15) . ? In3 Se13 2.5579(14) . ? In3 Se1 2.9150(15) . ? In4 Se5 2.544(2) . ? In4 Se6 2.557(2) . ? In4 Se7 2.564(2) . ? In4 Se1 2.6529(14) . ? In5 Cl2 2.388(3) . ? In5 Se5 2.559(2) . ? In5 Se2 2.577(2) . ? In5 Se12 2.589(2) . ? In6 Cl3 2.405(3) . ? In6 Se10 2.566(2) . ? In6 Se11 2.572(2) . ? In6 Se3 2.5729(15) . ? In7 Cl1 2.398(3) . ? In7 Se7 2.570(2) . ? In7 Se8 2.571(2) . ? In7 Se9 2.582(2) . ? In8 Cl4 2.398(3) . ? In8 Se13 2.565(2) . ? In8 Se6 2.579(2) . ? In8 Se4 2.586(2) . ? Se2 Cu5 2.415(2) . ? Se3 Cu1 2.390(2) . ? Se4 Cu3 2.382(2) . ? Se5 Cu3 2.394(2) . ? Se6 Cu6 2.391(2) . ? Se7 Cu2 2.400(2) . ? Se8 Cu4 2.361(2) . ? Se9 Cu6 2.405(2) . ? Se10 Cu5 2.389(2) . ? Se11 Cu4 2.410(2) . ? Se12 Cu2 2.416(2) . ? Se13 Cu1 2.392(2) . ? Cu1 P1 2.242(4) . ? Cu2 P2 2.254(4) . ? Cu3 P6 2.249(4) . ? Cu4 P3 2.239(4) . ? Cu5 P5 2.255(4) . ? Cu6 P4 2.241(4) . ? P1 C1 1.79(2) . ? P1 C13 1.797(13) . ? P1 C7 1.84(2) . ? P2 C19 1.801(15) . ? P2 C31 1.80(2) . ? P2 C25 1.820(14) . ? P3 C37 1.75(2) . ? P3 C49 1.812(15) . ? P3 C43 1.82(2) . ? P4 C55 1.803(15) . ? P4 C67 1.81(2) . ? P4 C61 1.83(2) . ? P5 C85 1.802(14) . ? P5 C79 1.80(2) . ? P5 C73 1.83(2) . ? P6 C103 1.80(2) . ? P6 C91 1.81(2) . ? P6 C97 1.81(2) . ? C1 C2 1.37(3) . ? C1 C6 1.46(3) . ? C2 C3 1.38(3) . ? C3 C4 1.45(4) . ? C4 C5 1.42(4) . ? C5 C6 1.41(4) . ? C7 C12 1.35(2) . ? C7 C8 1.42(2) . ? C8 C9 1.48(2) . ? C9 C10 1.32(4) . ? C10 C11 1.35(3) . ? C11 C12 1.39(3) . ? C13 C14 1.40(2) . ? C13 C18 1.40(2) . ? C14 C15 1.38(2) . ? C15 C16 1.36(2) . ? C16 C17 1.33(2) . ? C17 C18 1.37(2) . ? C19 C20 1.37(2) . ? C19 C24 1.46(2) . ? C20 C21 1.38(2) . ? C21 C22 1.38(3) . ? C22 C23 1.44(3) . ? C23 C24 1.44(3) . ? C25 C30 1.36(2) . ? C25 C26 1.38(2) . ? C26 C27 1.38(3) . ? C27 C28 1.34(3) . ? C28 C29 1.38(3) . ? C29 C30 1.41(2) . ? C31 C32 1.39(2) . ? C31 C36 1.41(2) . ? C32 C33 1.41(2) . ? C33 C34 1.33(3) . ? C34 C35 1.32(3) . ? C35 C36 1.38(3) . ? C37 C38 1.40(2) . ? C37 C42 1.43(2) . ? C38 C39 1.41(3) . ? C39 C40 1.28(3) . ? C40 C41 1.44(3) . ? C41 C42 1.33(3) . ? C43 C44 1.36(2) . ? C43 C48 1.40(2) . ? C44 C45 1.37(2) . ? C45 C46 1.29(3) . ? C46 C47 1.38(3) . ? C47 C48 1.40(3) . ? C49 C50 1.36(2) . ? C49 C54 1.40(2) . ? C50 C51 1.41(2) . ? C51 C52 1.38(2) . ? C52 C53 1.37(2) . ? C53 C54 1.36(2) . ? C55 C60 1.40(2) . ? C55 C56 1.40(2) . ? C56 C57 1.42(3) . ? C57 C58 1.36(3) . ? C58 C59 1.41(2) . ? C59 C60 1.38(2) . ? C61 C62 1.37(3) . ? C61 C66 1.37(3) . ? C62 C63 1.38(3) . ? C63 C64 1.30(3) . ? C64 C65 1.43(3) . ? C65 C66 1.40(3) . ? C67 C72 1.36(2) . ? C67 C68 1.36(2) . ? C68 C69 1.38(2) . ? C69 C70 1.40(3) . ? C70 C71 1.34(2) . ? C71 C72 1.40(2) . ? C73 C78 1.37(2) . ? C73 C74 1.41(2) . ? C74 C75 1.42(2) . ? C75 C76 1.38(3) . ? C76 C77 1.45(3) . ? C77 C78 1.35(3) . ? C79 C80 1.37(2) . ? C79 C84 1.40(3) . ? C80 C81 1.39(2) . ? C81 C82 1.40(3) . ? C82 C83 1.42(3) . ? C83 C84 1.42(2) . ? C85 C90 1.39(2) . ? C85 C86 1.40(2) . ? C86 C87 1.39(2) . ? C87 C88 1.35(3) . ? C88 C89 1.32(2) . ? C89 C90 1.39(2) . ? C91 C92 1.37(3) . ? C91 C96 1.42(3) . ? C92 C93 1.38(3) . ? C93 C94 1.37(4) . ? C94 C95 1.38(4) . ? C95 C96 1.40(3) . ? C97 C102 1.38(2) . ? C97 C98 1.38(3) . ? C98 C99 1.39(4) . ? C99 C100 1.48(5) . ? C100 C101 1.21(5) . ? C101 C102 1.37(3) . ? C103 C108 1.36(2) . ? C103 C104 1.42(2) . ? C104 C105 1.38(3) . ? C105 C106 1.38(3) . ? C106 C107 1.41(3) . ? C107 C108 1.44(2) . ? O1 C109 1.36(3) . ? O1 C112 1.47(2) . ? C109 C110 1.50(4) . ? C110 C111 1.59(4) . ? C111 C112 1.43(3) . ? O2 C116 1.31(4) . ? O2 C113 1.45(5) . ? C113 C114 1.56(6) . ? C114 C115 1.15(6) . ? C115 C116 1.51(6) . ? 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 Se12 In1 Se8 111.45(5) . . ? Se12 In1 Se10 113.38(5) . . ? Se8 In1 Se10 112.78(5) . . ? Se12 In1 Se1 108.98(5) . . ? Se8 In1 Se1 102.96(5) . . ? Se10 In1 Se1 106.57(5) . . ? Se4 In2 Se3 112.79(5) . . ? Se4 In2 Se2 112.52(5) . . ? Se3 In2 Se2 113.01(5) . . ? Se4 In2 Se1 105.61(5) . . ? Se3 In2 Se1 102.90(5) . . ? Se2 In2 Se1 109.22(5) . . ? O1 In3 Se9 86.5(2) . . ? O1 In3 Se11 85.0(2) . . ? Se9 In3 Se11 119.54(5) . . ? O1 In3 Se13 87.6(2) . . ? Se9 In3 Se13 118.68(5) . . ? Se11 In3 Se13 120.57(5) . . ? O1 In3 Se1 177.1(2) . . ? Se9 In3 Se1 91.77(5) . . ? Se11 In3 Se1 93.85(4) . . ? Se13 In3 Se1 95.30(5) . . ? Se5 In4 Se6 111.56(5) . . ? Se5 In4 Se7 113.11(5) . . ? Se6 In4 Se7 116.10(6) . . ? Se5 In4 Se1 107.41(5) . . ? Se6 In4 Se1 103.29(5) . . ? Se7 In4 Se1 104.20(5) . . ? Cl2 In5 Se5 100.07(11) . . ? Cl2 In5 Se2 105.86(11) . . ? Se5 In5 Se2 115.60(5) . . ? Cl2 In5 Se12 108.47(11) . . ? Se5 In5 Se12 112.62(5) . . ? Se2 In5 Se12 112.92(5) . . ? Cl3 In6 Se10 103.50(10) . . ? Cl3 In6 Se11 101.05(11) . . ? Se10 In6 Se11 116.13(5) . . ? Cl3 In6 Se3 104.07(9) . . ? Se10 In6 Se3 114.79(5) . . ? Se11 In6 Se3 114.64(5) . . ? Cl1 In7 Se7 107.94(10) . . ? Cl1 In7 Se8 101.26(9) . . ? Se7 In7 Se8 114.36(5) . . ? Cl1 In7 Se9 99.51(10) . . ? Se7 In7 Se9 111.22(5) . . ? Se8 In7 Se9 120.07(5) . . ? Cl4 In8 Se13 100.80(11) . . ? Cl4 In8 Se6 104.19(12) . . ? Se13 In8 Se6 118.62(5) . . ? Cl4 In8 Se4 102.39(12) . . ? Se13 In8 Se4 114.41(5) . . ? Se6 In8 Se4 113.39(5) . . ? In2 Se1 In1 103.96(5) . . ? In2 Se1 In4 106.58(5) . . ? In1 Se1 In4 106.29(5) . . ? In2 Se1 In3 111.90(5) . . ? In1 Se1 In3 114.34(5) . . ? In4 Se1 In3 113.04(5) . . ? Cu5 Se2 In2 101.58(6) . . ? Cu5 Se2 In5 100.30(6) . . ? In2 Se2 In5 97.48(5) . . ? Cu1 Se3 In2 100.97(6) . . ? Cu1 Se3 In6 100.96(6) . . ? In2 Se3 In6 96.61(5) . . ? Cu3 Se4 In2 95.88(6) . . ? Cu3 Se4 In8 103.21(7) . . ? In2 Se4 In8 96.46(5) . . ? Cu3 Se5 In4 97.14(6) . . ? Cu3 Se5 In5 101.23(7) . . ? In4 Se5 In5 100.14(5) . . ? Cu6 Se6 In4 93.86(6) . . ? Cu6 Se6 In8 104.13(7) . . ? In4 Se6 In8 97.55(5) . . ? Cu2 Se7 In4 93.54(6) . . ? Cu2 Se7 In7 107.69(7) . . ? In4 Se7 In7 96.66(5) . . ? Cu4 Se8 In1 97.71(6) . . ? Cu4 Se8 In7 98.78(6) . . ? In1 Se8 In7 96.50(5) . . ? Cu6 Se9 In3 102.42(6) . . ? Cu6 Se9 In7 105.67(7) . . ? In3 Se9 In7 104.49(5) . . ? Cu5 Se10 In6 109.54(7) . . ? Cu5 Se10 In1 94.14(6) . . ? In6 Se10 In1 95.45(5) . . ? Cu4 Se11 In3 98.48(6) . . ? Cu4 Se11 In6 104.44(6) . . ? In3 Se11 In6 104.61(5) . . ? Cu2 Se12 In1 100.22(6) . . ? Cu2 Se12 In5 99.18(7) . . ? In1 Se12 In5 97.49(5) . . ? Cu1 Se13 In3 94.51(6) . . ? Cu1 Se13 In8 108.90(7) . . ? In3 Se13 In8 103.33(5) . . ? P1 Cu1 Se3 115.77(12) . . ? P1 Cu1 Se13 116.98(12) . . ? Se3 Cu1 Se13 126.81(8) . . ? P2 Cu2 Se7 122.64(12) . . ? P2 Cu2 Se12 110.54(12) . . ? Se7 Cu2 Se12 126.76(8) . . ? P6 Cu3 Se4 119.31(13) . . ? P6 Cu3 Se5 111.80(12) . . ? Se4 Cu3 Se5 128.77(8) . . ? P3 Cu4 Se8 119.33(12) . . ? P3 Cu4 Se11 109.88(12) . . ? Se8 Cu4 Se11 129.72(8) . . ? P5 Cu5 Se10 125.74(13) . . ? P5 Cu5 Se2 109.66(12) . . ? Se10 Cu5 Se2 124.29(8) . . ? P4 Cu6 Se6 120.11(12) . . ? P4 Cu6 Se9 112.91(12) . . ? Se6 Cu6 Se9 126.92(8) . . ? C1 P1 C13 105.9(8) . . ? C1 P1 C7 105.1(8) . . ? C13 P1 C7 99.7(6) . . ? C1 P1 Cu1 107.3(5) . . ? C13 P1 Cu1 118.1(4) . . ? C7 P1 Cu1 119.5(5) . . ? C19 P2 C31 103.0(7) . . ? C19 P2 C25 103.8(7) . . ? C31 P2 C25 106.1(6) . . ? C19 P2 Cu2 113.2(4) . . ? C31 P2 Cu2 113.2(4) . . ? C25 P2 Cu2 116.3(5) . . ? C37 P3 C49 106.2(7) . . ? C37 P3 C43 106.0(7) . . ? C49 P3 C43 101.5(7) . . ? C37 P3 Cu4 102.4(5) . . ? C49 P3 Cu4 121.2(5) . . ? C43 P3 Cu4 118.3(4) . . ? C55 P4 C67 102.8(7) . . ? C55 P4 C61 107.0(7) . . ? C67 P4 C61 102.5(8) . . ? C55 P4 Cu6 110.6(5) . . ? C67 P4 Cu6 118.3(5) . . ? C61 P4 Cu6 114.4(6) . . ? C85 P5 C79 104.3(6) . . ? C85 P5 C73 107.7(7) . . ? C79 P5 C73 100.1(7) . . ? C85 P5 Cu5 112.7(4) . . ? C79 P5 Cu5 121.6(5) . . ? C73 P5 Cu5 109.2(5) . . ? C103 P6 C91 105.8(7) . . ? C103 P6 C97 103.9(8) . . ? C91 P6 C97 104.9(8) . . ? C103 P6 Cu3 116.9(5) . . ? C91 P6 Cu3 112.6(5) . . ? C97 P6 Cu3 111.7(6) . . ? C2 C1 C6 118.4(17) . . ? C2 C1 P1 125.1(14) . . ? C6 C1 P1 116.5(15) . . ? C1 C2 C3 124.1(24) . . ? C2 C3 C4 118.7(26) . . ? C5 C4 C3 117.9(22) . . ? C6 C5 C4 121.4(25) . . ? C5 C6 C1 118.1(25) . . ? C12 C7 C8 122.0(15) . . ? C12 C7 P1 123.7(13) . . ? C8 C7 P1 114.1(12) . . ? C7 C8 C9 115.5(18) . . ? C10 C9 C8 120.2(22) . . ? C9 C10 C11 121.1(18) . . ? C10 C11 C12 122.7(19) . . ? C7 C12 C11 118.3(18) . . ? C14 C13 C18 116.5(13) . . ? C14 C13 P1 119.4(10) . . ? C18 C13 P1 123.8(10) . . ? C15 C14 C13 120.8(13) . . ? C16 C15 C14 120.7(15) . . ? C17 C16 C15 119.4(16) . . ? C16 C17 C18 122.0(16) . . ? C17 C18 C13 120.6(15) . . ? C20 C19 C24 119.3(15) . . ? C20 C19 P2 120.0(12) . . ? C24 C19 P2 120.7(12) . . ? C19 C20 C21 125.1(18) . . ? C22 C21 C20 117.2(18) . . ? C21 C22 C23 122.1(18) . . ? C22 C23 C24 119.3(20) . . ? C23 C24 C19 116.7(18) . . ? C30 C25 C26 118.3(14) . . ? C30 C25 P2 119.3(10) . . ? C26 C25 P2 122.3(13) . . ? C27 C26 C25 120.4(18) . . ? C28 C27 C26 121.1(17) . . ? C27 C28 C29 120.5(16) . . ? C28 C29 C30 118.2(17) . . ? C25 C30 C29 121.5(14) . . ? C32 C31 C36 119.9(15) . . ? C32 C31 P2 122.8(12) . . ? C36 C31 P2 116.9(11) . . ? C31 C32 C33 118.8(15) . . ? C34 C33 C32 120.8(15) . . ? C35 C34 C33 119.4(16) . . ? C34 C35 C36 125.3(18) . . ? C35 C36 C31 115.5(16) . . ? C38 C37 C42 113.9(16) . . ? C38 C37 P3 120.5(12) . . ? C42 C37 P3 125.2(13) . . ? C37 C38 C39 122.9(17) . . ? C40 C39 C38 119.4(21) . . ? C39 C40 C41 121.9(19) . . ? C42 C41 C40 118.3(19) . . ? C41 C42 C37 123.4(20) . . ? C44 C43 C48 119.8(16) . . ? C44 C43 P3 126.4(13) . . ? C48 C43 P3 113.8(12) . . ? C43 C44 C45 121.5(18) . . ? C46 C45 C44 120.6(21) . . ? C45 C46 C47 120.3(19) . . ? C46 C47 C48 121.8(18) . . ? C43 C48 C47 115.7(18) . . ? C50 C49 C54 117.7(14) . . ? C50 C49 P3 120.8(11) . . ? C54 C49 P3 121.5(11) . . ? C49 C50 C51 121.5(14) . . ? C52 C51 C50 119.3(14) . . ? C53 C52 C51 118.8(14) . . ? C54 C53 C52 121.2(14) . . ? C53 C54 C49 121.3(15) . . ? C60 C55 C56 119.1(15) . . ? C60 C55 P4 123.3(11) . . ? C56 C55 P4 117.5(13) . . ? C55 C56 C57 117.3(18) . . ? C58 C57 C56 124.1(17) . . ? C57 C58 C59 117.1(16) . . ? C60 C59 C58 120.8(17) . . ? C59 C60 C55 121.3(16) . . ? C62 C61 C66 117.2(18) . . ? C62 C61 P4 123.2(15) . . ? C66 C61 P4 119.6(12) . . ? C61 C62 C63 123.7(23) . . ? C64 C63 C62 117.7(21) . . ? C63 C64 C65 124.0(20) . . ? C66 C65 C64 115.0(21) . . ? C61 C66 C65 122.2(20) . . ? C72 C67 C68 119.3(14) . . ? C72 C67 P4 117.8(12) . . ? C68 C67 P4 122.8(13) . . ? C67 C68 C69 119.9(16) . . ? C68 C69 C70 120.2(16) . . ? C71 C70 C69 119.6(15) . . ? C70 C71 C72 119.5(16) . . ? C67 C72 C71 121.4(14) . . ? C78 C73 C74 122.3(15) . . ? C78 C73 P5 115.5(12) . . ? C74 C73 P5 122.1(11) . . ? C73 C74 C75 116.9(16) . . ? C76 C75 C74 122.5(19) . . ? C75 C76 C77 116.7(17) . . ? C78 C77 C76 121.7(18) . . ? C77 C78 C73 119.7(17) . . ? C80 C79 C84 119.8(16) . . ? C80 C79 P5 122.8(14) . . ? C84 C79 P5 117.4(13) . . ? C79 C80 C81 123.4(20) . . ? C80 C81 C82 116.0(18) . . ? C81 C82 C83 123.8(16) . . ? C82 C83 C84 116.1(18) . . ? C79 C84 C83 120.7(18) . . ? C90 C85 C86 116.0(14) . . ? C90 C85 P5 120.2(11) . . ? C86 C85 P5 123.8(11) . . ? C87 C86 C85 120.9(15) . . ? C88 C87 C86 119.8(15) . . ? C89 C88 C87 121.4(15) . . ? C88 C89 C90 120.4(15) . . ? C89 C90 C85 121.5(15) . . ? C92 C91 C96 118.0(16) . . ? C92 C91 P6 122.3(15) . . ? C96 C91 P6 119.4(14) . . ? C91 C92 C93 119.7(24) . . ? C94 C93 C92 122.1(24) . . ? C93 C94 C95 120.6(20) . . ? C94 C95 C96 116.9(22) . . ? C95 C96 C91 122.4(20) . . ? C102 C97 C98 122.6(18) . . ? C102 C97 P6 121.2(15) . . ? C98 C97 P6 116.2(13) . . ? C97 C98 C99 115.8(24) . . ? C98 C99 C100 117.4(28) . . ? C101 C100 C99 123.5(31) . . ? C100 C101 C102 120.5(31) . . ? C101 C102 C97 119.2(22) . . ? C108 C103 C104 117.5(15) . . ? C108 C103 P6 118.0(12) . . ? C104 C103 P6 124.2(13) . . ? C105 C104 C103 120.4(17) . . ? C104 C105 C106 121.9(20) . . ? C105 C106 C107 120.1(17) . . ? C106 C107 C108 116.2(17) . . ? C103 C108 C107 123.7(16) . . ? C109 O1 C112 108.1(14) . . ? C109 O1 In3 125.1(12) . . ? C112 O1 In3 118.9(9) . . ? O1 C109 C110 110.3(20) . . ? C109 C110 C111 96.3(20) . . ? C112 C111 C110 103.0(20) . . ? C111 C112 O1 105.9(16) . . ? C116 O2 C113 114.6(31) . . ? O2 C113 C114 94.4(33) . . ? C115 C114 C113 114.7(44) . . ? C114 C115 C116 107.6(48) . . ? O2 C116 C115 104.7(35) . . ? _refine_diff_density_max 2.560 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.229 #===END data_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Cu6In8Cl4Se13(PnPr2Ph)12]' _chemical_formula_analytical ? _chemical_formula_sum 'C144 H228 Cl4 Cu6 In8 P12 Se13' _chemical_formula_weight 4798.98 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 19.609(4) _cell_length_b 31.841(6) _cell_length_c 34.232(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.72(3) _cell_angle_gamma 90.00 _cell_volume 21363.8(74) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour yellow _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.492 _exptl_crystal_density_method ? _exptl_crystal_F_000 9392 _exptl_absorpt_coefficient_mu 3.819 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30564 _diffrn_reflns_av_R_equivalents 0.0923 _diffrn_reflns_av_sigmaI/netI 0.1147 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.14 _reflns_number_total 26186 _reflns_number_observed 14452 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 26181 _refine_ls_number_parameters 964 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1351 _refine_ls_R_factor_obs 0.0854 _refine_ls_wR_factor_all 0.2341 _refine_ls_wR_factor_obs 0.2148 _refine_ls_goodness_of_fit_all 1.186 _refine_ls_goodness_of_fit_obs 1.482 _refine_ls_restrained_S_all 1.190 _refine_ls_restrained_S_obs 1.482 _refine_ls_shift/esd_max 0.122 _refine_ls_shift/esd_mean 0.005 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.24906(7) 0.61149(3) 0.36501(3) 0.0355(3) Uani 1 d . . In2 In 0.29861(7) 0.51870(3) 0.30036(4) 0.0379(3) Uani 1 d . . In3 In 0.18983(7) 0.70795(3) 0.28114(3) 0.0362(3) Uani 1 d . . In4 In 0.14476(7) 0.57752(3) 0.25436(3) 0.0354(3) Uani 1 d . . In5 In 0.35421(7) 0.62242(4) 0.25519(4) 0.0359(3) Uani 1 d . . In6 In 0.06364(7) 0.64027(4) 0.33768(4) 0.0372(3) Uani 1 d . . In7 In 0.21359(7) 0.65629(4) 0.18021(4) 0.0377(3) Uani 1 d . . In8 In 0.36143(8) 0.70535(4) 0.33765(4) 0.0397(3) Uani 1 d . . Se1 Se 0.36783(10) 0.64025(5) 0.38228(5) 0.0384(5) Uani 1 d . . Se2 Se 0.09977(10) 0.61999(5) 0.19581(5) 0.0371(4) Uani 1 d . . Se3 Se 0.23439(10) 0.62939(5) 0.28914(5) 0.0343(4) Uani 1 d . . Se4 Se 0.40879(10) 0.56124(5) 0.29302(5) 0.0386(4) Uani 1 d . . Se5 Se 0.23774(11) 0.53152(5) 0.36492(5) 0.0376(4) Uani 1 d . . Se6 Se 0.06154(10) 0.69891(5) 0.28592(5) 0.0379(4) Uani 1 d . . Se7 Se 0.23112(11) 0.72808(5) 0.21358(5) 0.0375(4) Uani 1 d . . Se8 Se 0.31859(11) 0.60768(5) 0.18384(5) 0.0383(4) Uani 1 d . . Se9 Se 0.15042(10) 0.65144(5) 0.39463(5) 0.0365(4) Uani 1 d . . Se10 Se 0.21991(11) 0.51462(5) 0.23879(5) 0.0382(4) Uani 1 d . . Se11 Se 0.40899(11) 0.69390(5) 0.26911(5) 0.0385(4) Uani 1 d . . Se12 Se 0.24786(11) 0.74566(5) 0.33884(5) 0.0386(5) Uani 1 d . . Se13 Se 0.06018(10) 0.56530(5) 0.30859(5) 0.0366(4) Uani 1 d . . Cu1 Cu 0.28208(14) 0.53241(6) 0.17804(7) 0.0439(6) Uani 1 d . . Cu2 Cu 0.18661(15) 0.72690(7) 0.39881(6) 0.0474(7) Uani 1 d . . Cu3 Cu 0.45418(14) 0.59056(7) 0.35666(7) 0.0446(6) Uani 1 d . . Cu4 Cu 0.11520(13) 0.51339(6) 0.35399(6) 0.0410(6) Uani 1 d . . Cu5 Cu 0.01569(14) 0.67112(7) 0.22252(7) 0.0447(6) Uani 1 d . . Cu6 Cu 0.35484(14) 0.74226(7) 0.21951(7) 0.0473(6) Uani 1 d . . Cl1 Cl 0.3390(3) 0.44727(14) 0.3084(2) 0.0594(15) Uani 1 d . . Cl2 Cl -0.0458(3) 0.6499(2) 0.36762(15) 0.0526(13) Uani 1 d . . Cl3 Cl 0.2012(3) 0.6756(2) 0.11174(13) 0.0544(14) Uani 1 d . . Cl4 Cl 0.4398(3) 0.7551(2) 0.3684(2) 0.061(2) Uani 1 d . . P1 P 0.3761(3) 0.4907(2) 0.1713(2) 0.0536(15) Uani 1 d . . P2 P -0.0862(3) 0.6377(2) 0.2294(2) 0.0565(15) Uani 1 d . . P3 P 0.0611(3) 0.5164(2) 0.41183(15) 0.0479(13) Uani 1 d . . P4 P 0.2136(3) 0.5212(2) 0.12383(15) 0.0500(14) Uani 1 d . . P5 P 0.4730(3) 0.5367(2) 0.4002(2) 0.0532(15) Uani 1 d . . P6 P 0.3693(4) 0.8105(2) 0.2397(2) 0.058(2) Uani 1 d . . P7 P 0.2526(4) 0.7368(2) 0.45487(15) 0.056(2) Uani 1 d . . P8 P 0.1009(3) 0.44593(15) 0.3318(2) 0.0511(15) Uani 1 d . . P9 P 0.0941(4) 0.7705(2) 0.4032(2) 0.056(2) Uani 1 d . . P10 P 0.4091(4) 0.7361(2) 0.1614(2) 0.060(2) Uani 1 d . . P11 P 0.5581(3) 0.6217(2) 0.3488(2) 0.0537(14) Uani 1 d . . P12 P -0.0021(3) 0.7273(2) 0.1812(2) 0.0529(15) Uani 1 d . . C1 C 0.4363(14) 0.5103(7) 0.1367(7) 0.065(6) Uiso 1 d . . C2 C 0.4550(22) 0.4881(11) 0.1068(10) 0.113(11) Uiso 1 d . . H2 H 0.4338(22) 0.4615(11) 0.1033(10) 0.136 Uiso 1 calc R . C3 C 0.5081(34) 0.5006(18) 0.0762(17) 0.190(22) Uiso 1 d . . H3 H 0.5229(34) 0.4834(18) 0.0555(17) 0.227 Uiso 1 calc R . C4 C 0.5334(30) 0.5465(16) 0.0853(15) 0.165(18) Uiso 1 d . . H4 H 0.5625(30) 0.5604(16) 0.0678(15) 0.198 Uiso 1 calc R . C5 C 0.5124(24) 0.5677(12) 0.1206(12) 0.123(12) Uiso 1 d . . H5 H 0.5308(24) 0.5942(12) 0.1283(12) 0.148 Uiso 1 calc R . C6 C 0.4671(19) 0.5486(9) 0.1412(9) 0.094(9) Uiso 1 d . . H6 H 0.4528(19) 0.5640(9) 0.1632(9) 0.113 Uiso 1 calc R . C7 C 0.3563(14) 0.4386(6) 0.1547(7) 0.061(6) Uiso 1 d . . H7A H 0.3321(14) 0.4407(6) 0.1289(7) 0.073 Uiso 1 calc R . H7B H 0.3996(14) 0.4235(6) 0.1507(7) 0.073 Uiso 1 calc R . C8 C 0.3121(16) 0.4120(8) 0.1821(8) 0.081(7) Uiso 1 d . . H8A H 0.3364(16) 0.4092(8) 0.2077(8) 0.097 Uiso 1 calc R . H8B H 0.2688(16) 0.4270(8) 0.1864(8) 0.097 Uiso 1 calc R . C9 C 0.2961(17) 0.3692(8) 0.1668(8) 0.090(8) Uiso 1 d . . H9A H 0.2682(17) 0.3541(8) 0.1855(8) 0.136 Uiso 1 calc R . H9B H 0.3387(17) 0.3537(8) 0.1631(8) 0.136 Uiso 1 calc R . H9C H 0.2709(17) 0.3715(8) 0.1417(8) 0.136 Uiso 1 calc R . C10 C 0.4291(13) 0.4819(7) 0.2162(7) 0.063(6) Uiso 1 d . . H10A H 0.4408(13) 0.5096(7) 0.2277(7) 0.075 Uiso 1 calc R . H10B H 0.4012(13) 0.4667(7) 0.2352(7) 0.075 Uiso 1 calc R . C11 C 0.4958(15) 0.4572(8) 0.2112(7) 0.073(7) Uiso 1 d . . H11A H 0.4854(15) 0.4277(8) 0.2043(7) 0.087 Uiso 1 calc R . H11B H 0.5224(15) 0.4698(8) 0.1900(7) 0.087 Uiso 1 calc R . C12 C 0.5356(15) 0.4589(8) 0.2485(7) 0.077(7) Uiso 1 d . . H12A H 0.5784(15) 0.4434(8) 0.2459(7) 0.116 Uiso 1 calc R . H12B H 0.5091(15) 0.4462(8) 0.2693(7) 0.116 Uiso 1 calc R . H12C H 0.5458(15) 0.4882(8) 0.2551(7) 0.116 Uiso 1 calc R . C13 C -0.1506(14) 0.6781(7) 0.2302(7) 0.065(6) Uiso 1 d . . C14 C -0.1615(15) 0.7020(8) 0.2647(8) 0.071(7) Uiso 1 d . . H14 H -0.1405(15) 0.6943(8) 0.2890(8) 0.086 Uiso 1 calc R . C15 C -0.1995(25) 0.7333(13) 0.2620(13) 0.132(13) Uiso 1 d . . H15 H -0.1983(25) 0.7523(13) 0.2835(13) 0.158 Uiso 1 calc R . C16 C -0.2404(22) 0.7425(12) 0.2329(11) 0.119(12) Uiso 1 d . . H16 H -0.2717(22) 0.7651(12) 0.2352(11) 0.143 Uiso 1 calc R . C17 C -0.2393(24) 0.7219(12) 0.2016(12) 0.126(13) Uiso 1 d . . H17 H -0.2688(24) 0.7286(12) 0.1799(12) 0.151 Uiso 1 calc R . C18 C -0.1921(22) 0.6883(11) 0.2000(11) 0.118(12) Uiso 1 d . . H18 H -0.1898(22) 0.6725(11) 0.1766(11) 0.142 Uiso 1 calc R . C19 C -0.1122(15) 0.6027(7) 0.1892(7) 0.073(7) Uiso 1 d . . H19A H -0.1615(15) 0.5964(7) 0.1907(7) 0.088 Uiso 1 calc R . H19B H -0.1045(15) 0.6168(7) 0.1640(7) 0.088 Uiso 1 calc R . C20 C -0.0687(23) 0.5592(11) 0.1915(11) 0.125(12) Uiso 1 d . . H20A H -0.0192(23) 0.5652(11) 0.1908(11) 0.150 Uiso 1 calc R . H20B H -0.0778(23) 0.5441(11) 0.2161(11) 0.150 Uiso 1 calc R . C21 C -0.0917(34) 0.5320(17) 0.1555(16) 0.201(23) Uiso 1 d . . H21A H -0.0665(34) 0.5054(17) 0.1559(16) 0.301 Uiso 1 calc R . H21B H -0.0824(34) 0.5473(17) 0.1314(16) 0.301 Uiso 1 calc R . H21C H -0.1407(34) 0.5263(17) 0.1566(16) 0.301 Uiso 1 calc R . C22 C -0.1017(14) 0.6043(7) 0.2725(7) 0.068(6) Uiso 1 d . . H22A H -0.0710(14) 0.5797(7) 0.2719(7) 0.081 Uiso 1 calc R . H22B H -0.0899(14) 0.6205(7) 0.2965(7) 0.081 Uiso 1 calc R . C23 C -0.1780(16) 0.5884(8) 0.2749(8) 0.083(8) Uiso 1 d . . H23A H -0.2091(16) 0.6128(8) 0.2762(8) 0.100 Uiso 1 calc R . H23B H -0.1904(16) 0.5721(8) 0.2511(8) 0.100 Uiso 1 calc R . C24 C -0.1853(19) 0.5615(9) 0.3102(9) 0.101(9) Uiso 1 d . . H24A H -0.2326(19) 0.5517(9) 0.3114(9) 0.151 Uiso 1 calc R . H24B H -0.1735(19) 0.5778(9) 0.3337(9) 0.151 Uiso 1 calc R . H24C H -0.1548(19) 0.5372(9) 0.3086(9) 0.151 Uiso 1 calc R . C25 C -0.0185(12) 0.4876(6) 0.4091(6) 0.051(5) Uiso 1 d . . C26 C -0.0745(14) 0.5024(7) 0.3885(7) 0.065(6) Uiso 1 d . . H26 H -0.0729(14) 0.5297(7) 0.3774(7) 0.078 Uiso 1 calc R . C27 C -0.1363(16) 0.4776(8) 0.3830(8) 0.081(7) Uiso 1 d . . H27 H -0.1719(16) 0.4865(8) 0.3656(8) 0.097 Uiso 1 calc R . C28 C -0.1417(17) 0.4428(9) 0.4026(8) 0.084(8) Uiso 1 d . . H28 H -0.1842(17) 0.4283(9) 0.4017(8) 0.101 Uiso 1 calc R . C29 C -0.0914(14) 0.4269(8) 0.4234(7) 0.069(6) Uiso 1 d . . H29 H -0.0968(14) 0.4006(8) 0.4360(7) 0.083 Uiso 1 calc R . C30 C -0.0282(12) 0.4488(6) 0.4272(6) 0.052(5) Uiso 1 d . . H30 H 0.0081(12) 0.4368(6) 0.4425(6) 0.062 Uiso 1 calc R . C31 C 0.1043(12) 0.4932(6) 0.4550(6) 0.053(5) Uiso 1 d . . H31A H 0.0732(12) 0.4934(6) 0.4772(6) 0.063 Uiso 1 calc R . H31B H 0.1165(12) 0.4637(6) 0.4494(6) 0.063 Uiso 1 calc R . C32 C 0.1693(15) 0.5182(8) 0.4658(8) 0.075(7) Uiso 1 d . . H32A H 0.1574(15) 0.5473(8) 0.4732(8) 0.090 Uiso 1 calc R . H32B H 0.1998(15) 0.5193(8) 0.4433(8) 0.090 Uiso 1 calc R . C33 C 0.2056(21) 0.4949(11) 0.5015(10) 0.115(11) Uiso 1 d . . H33A H 0.2473(21) 0.5100(11) 0.5093(10) 0.173 Uiso 1 calc R . H33B H 0.2172(21) 0.4661(11) 0.4937(10) 0.173 Uiso 1 calc R . H33C H 0.1748(21) 0.4940(11) 0.5235(10) 0.173 Uiso 1 calc R . C34 C 0.0311(12) 0.5673(6) 0.4305(6) 0.051(5) Uiso 1 d . . H34A H 0.0714(12) 0.5855(6) 0.4353(6) 0.062 Uiso 1 calc R . H34B H 0.0025(12) 0.5807(6) 0.4097(6) 0.062 Uiso 1 calc R . C35 C -0.0067(14) 0.5662(7) 0.4649(7) 0.066(6) Uiso 1 d . . H35A H 0.0219(14) 0.5541(7) 0.4864(7) 0.079 Uiso 1 calc R . H35B H -0.0469(14) 0.5478(7) 0.4607(7) 0.079 Uiso 1 calc R . C36 C -0.0317(21) 0.6117(10) 0.4774(10) 0.116(11) Uiso 1 d . . H36A H -0.0577(21) 0.6095(10) 0.5013(10) 0.174 Uiso 1 calc R . H36B H -0.0608(21) 0.6236(10) 0.4564(10) 0.174 Uiso 1 calc R . H36C H 0.0080(21) 0.6299(10) 0.4821(10) 0.174 Uiso 1 calc R . C37 C 0.2666(13) 0.5149(6) 0.0816(6) 0.057(5) Uiso 1 d . . C38 C 0.3064(16) 0.5480(8) 0.0723(8) 0.076(7) Uiso 1 d . . H38 H 0.3046(16) 0.5725(8) 0.0880(8) 0.091 Uiso 1 calc R . C39 C 0.3511(19) 0.5478(10) 0.0401(9) 0.099(9) Uiso 1 d . . H39 H 0.3807(19) 0.5708(10) 0.0357(9) 0.119 Uiso 1 calc R . C40 C 0.3501(20) 0.5143(10) 0.0161(10) 0.101(10) Uiso 1 d . . H40 H 0.3742(20) 0.5152(10) -0.0075(10) 0.121 Uiso 1 calc R . C41 C 0.3127(23) 0.4773(12) 0.0260(11) 0.121(12) Uiso 1 d . . H41 H 0.3166(23) 0.4518(12) 0.0118(11) 0.146 Uiso 1 calc R . C42 C 0.2678(19) 0.4814(10) 0.0598(9) 0.098(9) Uiso 1 d . . H42 H 0.2387(19) 0.4586(10) 0.0658(9) 0.118 Uiso 1 calc R . C43 C 0.1663(15) 0.4716(7) 0.1249(7) 0.071(7) Uiso 1 d . . H43A H 0.1461(15) 0.4657(7) 0.0986(7) 0.085 Uiso 1 calc R . H43B H 0.1978(15) 0.4484(7) 0.1320(7) 0.085 Uiso 1 calc R . C44 C 0.1075(19) 0.4743(9) 0.1558(9) 0.098(9) Uiso 1 d . . H44A H 0.1269(19) 0.4835(9) 0.1814(9) 0.118 Uiso 1 calc R . H44B H 0.0728(19) 0.4952(9) 0.1470(9) 0.118 Uiso 1 calc R . C45 C 0.0727(23) 0.4295(11) 0.1601(11) 0.128(13) Uiso 1 d . . H45A H 0.0365(23) 0.4311(11) 0.1792(11) 0.192 Uiso 1 calc R . H45B H 0.1071(23) 0.4090(11) 0.1691(11) 0.192 Uiso 1 calc R . H45C H 0.0532(23) 0.4206(11) 0.1348(11) 0.192 Uiso 1 calc R . C46 C 0.1590(13) 0.5610(7) 0.1046(7) 0.063(6) Uiso 1 d . . H46A H 0.1279(13) 0.5691(7) 0.1255(7) 0.075 Uiso 1 calc R . H46B H 0.1878(13) 0.5858(7) 0.0994(7) 0.075 Uiso 1 calc R . C47 C 0.1150(13) 0.5532(7) 0.0678(7) 0.062(6) Uiso 1 d . . H47A H 0.1445(13) 0.5519(7) 0.0448(7) 0.074 Uiso 1 calc R . H47B H 0.0917(13) 0.5257(7) 0.0700(7) 0.074 Uiso 1 calc R . C48 C 0.0630(19) 0.5870(10) 0.0618(10) 0.103(10) Uiso 1 d . . H48A H 0.0355(19) 0.5812(10) 0.0381(10) 0.155 Uiso 1 calc R . H48B H 0.0860(19) 0.6141(10) 0.0591(10) 0.155 Uiso 1 calc R . H48C H 0.0333(19) 0.5880(10) 0.0843(10) 0.155 Uiso 1 calc R . C49 C 0.5505(12) 0.5075(6) 0.3895(6) 0.052(5) Uiso 1 d . . C50 C 0.5523(14) 0.4886(7) 0.3545(7) 0.063(6) Uiso 1 d . . H50 H 0.5137(14) 0.4904(7) 0.3372(7) 0.076 Uiso 1 calc R . C51 C 0.6131(17) 0.4649(9) 0.3424(9) 0.089(8) Uiso 1 d . . H51 H 0.6134(17) 0.4513(9) 0.3177(9) 0.107 Uiso 1 calc R . C52 C 0.6686(17) 0.4631(8) 0.3673(8) 0.081(7) Uiso 1 d . . H52 H 0.7102(17) 0.4505(8) 0.3598(8) 0.097 Uiso 1 calc R . C53 C 0.6608(16) 0.4817(8) 0.4065(8) 0.077(7) Uiso 1 d . . H53 H 0.6962(16) 0.4780(8) 0.4258(8) 0.093 Uiso 1 calc R . C54 C 0.6049(14) 0.5036(7) 0.4154(7) 0.067(6) Uiso 1 d . . H54 H 0.6030(14) 0.5168(7) 0.4402(7) 0.080 Uiso 1 calc R . C55 C 0.4118(15) 0.4933(7) 0.4003(7) 0.073(7) Uiso 1 d . . H55A H 0.3671(15) 0.5040(7) 0.4086(7) 0.087 Uiso 1 calc R . H55B H 0.4057(15) 0.4823(7) 0.3734(7) 0.087 Uiso 1 calc R . C56 C 0.4349(18) 0.4573(9) 0.4277(9) 0.095(9) Uiso 1 d . . H56A H 0.4544(18) 0.4678(9) 0.4528(9) 0.114 Uiso 1 calc R . H56B H 0.4680(18) 0.4384(9) 0.4153(9) 0.114 Uiso 1 calc R . C57 C 0.3588(34) 0.4341(17) 0.4330(17) 0.208(24) Uiso 1 d . . H57A H 0.3643(34) 0.4096(17) 0.4501(17) 0.312 Uiso 1 calc R . H57B H 0.3406(34) 0.4251(17) 0.4074(17) 0.312 Uiso 1 calc R . H57C H 0.3272(34) 0.4540(17) 0.4446(17) 0.312 Uiso 1 calc R . C58 C 0.4851(14) 0.5494(7) 0.4509(7) 0.066(6) Uiso 1 d . . H58A H 0.4963(14) 0.5236(7) 0.4658(7) 0.079 Uiso 1 calc R . H58B H 0.5239(14) 0.5691(7) 0.4542(7) 0.079 Uiso 1 calc R . C59 C 0.4145(22) 0.5715(11) 0.4686(11) 0.121(12) Uiso 1 d . . H59A H 0.4015(22) 0.5961(11) 0.4524(11) 0.146 Uiso 1 calc R . H59B H 0.3765(22) 0.5510(11) 0.4669(11) 0.146 Uiso 1 calc R . C60 C 0.4242(31) 0.5850(15) 0.5095(14) 0.175(19) Uiso 1 d . . H60A H 0.3818(31) 0.5975(15) 0.5186(14) 0.263 Uiso 1 calc R . H60B H 0.4609(31) 0.6059(15) 0.5113(14) 0.263 Uiso 1 calc R . H60C H 0.4364(31) 0.5607(15) 0.5258(14) 0.263 Uiso 1 calc R . C61 C 0.4578(13) 0.8267(6) 0.2362(6) 0.056(5) Uiso 1 d . . C62 C 0.4766(16) 0.8558(8) 0.2078(8) 0.075(7) Uiso 1 d . . H62 H 0.4424(16) 0.8695(8) 0.1921(8) 0.090 Uiso 1 calc R . C63 C 0.5474(18) 0.8651(9) 0.2022(9) 0.096(9) Uiso 1 d . . H63 H 0.5607(18) 0.8822(9) 0.1810(9) 0.115 Uiso 1 calc R . C64 C 0.5961(20) 0.8486(10) 0.2285(9) 0.104(10) Uiso 1 d . . H64 H 0.6419(20) 0.8581(10) 0.2271(9) 0.125 Uiso 1 calc R . C65 C 0.5815(21) 0.8206(11) 0.2552(11) 0.113(11) Uiso 1 d . . H65 H 0.6167(21) 0.8082(11) 0.2710(11) 0.135 Uiso 1 calc R . C66 C 0.5078(17) 0.8086(9) 0.2601(8) 0.086(8) Uiso 1 d . . H66 H 0.4959(17) 0.7887(9) 0.2795(8) 0.103 Uiso 1 calc R . C67 C 0.3256(13) 0.8512(7) 0.2125(7) 0.066(6) Uiso 1 d . . H67A H 0.3410(13) 0.8789(7) 0.2224(7) 0.079 Uiso 1 calc R . H67B H 0.3376(13) 0.8492(7) 0.1847(7) 0.079 Uiso 1 calc R . C68 C 0.2445(15) 0.8479(8) 0.2158(7) 0.073(7) Uiso 1 d . . H68A H 0.2298(15) 0.8188(8) 0.2097(7) 0.088 Uiso 1 calc R . H68B H 0.2318(15) 0.8542(8) 0.2430(7) 0.088 Uiso 1 calc R . C69 C 0.2067(22) 0.8785(11) 0.1876(10) 0.118(12) Uiso 1 d . . H69A H 0.1574(22) 0.8756(11) 0.1905(10) 0.178 Uiso 1 calc R . H69B H 0.2183(22) 0.8720(11) 0.1607(10) 0.178 Uiso 1 calc R . H69C H 0.2206(22) 0.9074(11) 0.1938(10) 0.178 Uiso 1 calc R . C70 C 0.3578(15) 0.8240(7) 0.2891(7) 0.068(6) Uiso 1 d . . H70A H 0.3102(15) 0.8169(7) 0.2953(7) 0.082 Uiso 1 calc R . H70B H 0.3877(15) 0.8054(7) 0.3052(7) 0.082 Uiso 1 calc R . C71 C 0.3708(17) 0.8695(8) 0.3034(8) 0.083(8) Uiso 1 d . . H71A H 0.4166(17) 0.8788(8) 0.2955(8) 0.100 Uiso 1 calc R . H71B H 0.3365(17) 0.8885(8) 0.2910(8) 0.100 Uiso 1 calc R . C72 C 0.3665(23) 0.8717(12) 0.3461(10) 0.127(12) Uiso 1 d . . H72A H 0.3746(23) 0.9006(12) 0.3548(10) 0.190 Uiso 1 calc R . H72B H 0.4010(23) 0.8532(12) 0.3582(10) 0.190 Uiso 1 calc R . H72C H 0.3210(23) 0.8627(12) 0.3538(10) 0.190 Uiso 1 calc R . C73 C 0.2601(11) 0.7912(5) 0.4669(5) 0.042(4) Uiso 1 d . . C74 C 0.2831(14) 0.8180(7) 0.4404(7) 0.061(6) Uiso 1 d . . H74 H 0.2982(14) 0.8070(7) 0.4163(7) 0.074 Uiso 1 calc R . C75 C 0.2862(15) 0.8615(8) 0.4461(8) 0.074(7) Uiso 1 d . . H75 H 0.3036(15) 0.8792(8) 0.4263(8) 0.089 Uiso 1 calc R . C76 C 0.2644(16) 0.8784(9) 0.4800(8) 0.081(7) Uiso 1 d . . H76 H 0.2666(16) 0.9078(9) 0.4846(8) 0.097 Uiso 1 calc R . C77 C 0.2400(14) 0.8524(7) 0.5060(7) 0.065(6) Uiso 1 d . . H77 H 0.2259(14) 0.8636(7) 0.5302(7) 0.078 Uiso 1 calc R . C78 C 0.2339(15) 0.8091(7) 0.4998(7) 0.067(6) Uiso 1 d . . H78 H 0.2115(15) 0.7921(7) 0.5182(7) 0.080 Uiso 1 calc R . C79 C 0.3433(14) 0.7231(7) 0.4575(7) 0.063(6) Uiso 1 d . . H79A H 0.3479(14) 0.6926(7) 0.4526(7) 0.076 Uiso 1 calc R . H79B H 0.3666(14) 0.7381(7) 0.4364(7) 0.076 Uiso 1 calc R . C80 C 0.3796(16) 0.7335(8) 0.4964(8) 0.080(7) Uiso 1 d . . H80A H 0.3582(16) 0.7178(8) 0.5178(8) 0.096 Uiso 1 calc R . H80B H 0.3753(16) 0.7639(8) 0.5020(8) 0.096 Uiso 1 calc R . C81 C 0.4552(18) 0.7215(9) 0.4944(9) 0.097(9) Uiso 1 d . . H81A H 0.4785(18) 0.7281(9) 0.5193(9) 0.145 Uiso 1 calc R . H81B H 0.4762(18) 0.7374(9) 0.4734(9) 0.145 Uiso 1 calc R . H81C H 0.4591(18) 0.6914(9) 0.4892(9) 0.145 Uiso 1 calc R . C82 C 0.2181(14) 0.7113(7) 0.4986(6) 0.062(6) Uiso 1 d . . H82A H 0.2385(14) 0.7235(7) 0.5228(6) 0.074 Uiso 1 calc R . H82B H 0.1679(14) 0.7144(7) 0.4990(6) 0.074 Uiso 1 calc R . C83 C 0.2425(22) 0.6564(11) 0.4933(11) 0.115(11) Uiso 1 d . . H83A H 0.2388(22) 0.6478(11) 0.4655(11) 0.137 Uiso 1 calc R . H83B H 0.2901(22) 0.6520(11) 0.5029(11) 0.137 Uiso 1 calc R . C84 C 0.2016(31) 0.6354(16) 0.5135(14) 0.172(19) Uiso 1 d . . H84A H 0.2127(31) 0.6055(16) 0.5117(14) 0.257 Uiso 1 calc R . H84B H 0.1548(31) 0.6401(16) 0.5037(14) 0.257 Uiso 1 calc R . H84C H 0.2058(31) 0.6444(16) 0.5409(14) 0.257 Uiso 1 calc R . C85 C 0.1190(12) 0.4089(6) 0.3707(6) 0.048(5) Uiso 1 d . . C86 C 0.1778(14) 0.4117(7) 0.3911(7) 0.069(6) Uiso 1 d . . H86 H 0.2099(14) 0.4326(7) 0.3842(7) 0.082 Uiso 1 calc R . C87 C 0.1940(19) 0.3840(9) 0.4230(9) 0.094(9) Uiso 1 d . . H87 H 0.2371(19) 0.3855(9) 0.4363(9) 0.113 Uiso 1 calc R . C88 C 0.1451(15) 0.3546(8) 0.4344(8) 0.073(7) Uiso 1 d . . H88 H 0.1544(15) 0.3370(8) 0.4563(8) 0.087 Uiso 1 calc R . C89 C 0.0866(14) 0.3513(7) 0.4150(7) 0.070(6) Uiso 1 d . . H89 H 0.0557(14) 0.3297(7) 0.4219(7) 0.083 Uiso 1 calc R . C90 C 0.0684(13) 0.3782(6) 0.3846(6) 0.056(5) Uiso 1 d . . H90 H 0.0239(13) 0.3770(6) 0.3728(6) 0.067 Uiso 1 calc R . C91 C 0.0144(11) 0.4323(6) 0.3125(6) 0.045(4) Uiso 1 d . . H91A H 0.0125(11) 0.4019(6) 0.3068(6) 0.054 Uiso 1 calc R . H91B H -0.0193(11) 0.4384(6) 0.3328(6) 0.054 Uiso 1 calc R . C92 C -0.0045(18) 0.4563(9) 0.2763(8) 0.089(8) Uiso 1 d . . H92A H -0.0004(18) 0.4866(9) 0.2822(8) 0.107 Uiso 1 calc R . H92B H 0.0294(18) 0.4497(9) 0.2563(8) 0.107 Uiso 1 calc R . C93 C -0.0731(19) 0.4485(10) 0.2591(9) 0.101(9) Uiso 1 d . . H93A H -0.0798(19) 0.4658(10) 0.2355(9) 0.151 Uiso 1 calc R . H93B H -0.1075(19) 0.4559(10) 0.2781(9) 0.151 Uiso 1 calc R . H93C H -0.0776(19) 0.4188(10) 0.2521(9) 0.151 Uiso 1 calc R . C94 C 0.1525(13) 0.4229(6) 0.2943(6) 0.056(5) Uiso 1 d . . H94A H 0.1443(13) 0.4393(6) 0.2700(6) 0.067 Uiso 1 calc R . H94B H 0.2009(13) 0.4271(6) 0.3023(6) 0.067 Uiso 1 calc R . C95 C 0.1435(19) 0.3768(9) 0.2839(9) 0.094(9) Uiso 1 d . . H95A H 0.0962(19) 0.3719(9) 0.2739(9) 0.113 Uiso 1 calc R . H95B H 0.1510(19) 0.3594(9) 0.3077(9) 0.113 Uiso 1 calc R . C96 C 0.1939(22) 0.3639(11) 0.2529(11) 0.120(12) Uiso 1 d . . H96A H 0.1876(22) 0.3341(11) 0.2466(11) 0.180 Uiso 1 calc R . H96B H 0.2406(22) 0.3685(11) 0.2630(11) 0.180 Uiso 1 calc R . H96C H 0.1859(22) 0.3809(11) 0.2293(11) 0.180 Uiso 1 calc R . C97 C 0.0577(13) 0.7666(6) 0.4518(6) 0.055(5) Uiso 1 d . . C98 C 0.0305(16) 0.7296(8) 0.4618(8) 0.079(7) Uiso 1 d . . H98 H 0.0291(16) 0.7070(8) 0.4436(8) 0.095 Uiso 1 calc R . C99 C 0.0037(18) 0.7242(9) 0.4999(9) 0.091(8) Uiso 1 d . . H99 H -0.0167(18) 0.6985(9) 0.5075(9) 0.109 Uiso 1 calc R . C100 C 0.0090(18) 0.7599(9) 0.5266(9) 0.091(8) Uiso 1 d . . H100 H -0.0112(18) 0.7579(9) 0.5513(9) 0.109 Uiso 1 calc R . C101 C 0.0397(17) 0.7936(9) 0.5179(9) 0.087(8) Uiso 1 d . . H101 H 0.0474(17) 0.8148(9) 0.5370(9) 0.105 Uiso 1 calc R . C102 C 0.0618(15) 0.7991(8) 0.4804(7) 0.075(7) Uiso 1 d . . H102 H 0.0804(15) 0.8254(8) 0.4733(7) 0.089 Uiso 1 calc R . C103 C 0.1104(15) 0.8268(7) 0.3963(7) 0.073(7) Uiso 1 d . . H10C H 0.0692(15) 0.8430(7) 0.4028(7) 0.088 Uiso 1 calc R . H10D H 0.1481(15) 0.8358(7) 0.4144(7) 0.088 Uiso 1 calc R . C104 C 0.1300(19) 0.8366(9) 0.3528(9) 0.096(9) Uiso 1 d . . H10E H 0.0928(19) 0.8277(9) 0.3345(9) 0.115 Uiso 1 calc R . H10F H 0.1721(19) 0.8212(9) 0.3463(9) 0.115 Uiso 1 calc R . C105 C 0.1421(24) 0.8860(11) 0.3495(11) 0.130(13) Uiso 1 d . . H10G H 0.1543(24) 0.8931(11) 0.3228(11) 0.194 Uiso 1 calc R . H10H H 0.1791(24) 0.8945(11) 0.3677(11) 0.194 Uiso 1 calc R . H10I H 0.1002(24) 0.9009(11) 0.3561(11) 0.194 Uiso 1 calc R . C106 C 0.0200(15) 0.7629(8) 0.3708(7) 0.072(7) Uiso 1 d . . H10J H 0.0343(15) 0.7665(8) 0.3435(7) 0.086 Uiso 1 calc R . H10K H 0.0039(15) 0.7337(8) 0.3736(7) 0.086 Uiso 1 calc R . C107 C -0.0413(15) 0.7933(8) 0.3779(7) 0.072(7) Uiso 1 d . . H10L H -0.0565(15) 0.7898(8) 0.4051(7) 0.087 Uiso 1 calc R . H10M H -0.0262(15) 0.8227(8) 0.3747(7) 0.087 Uiso 1 calc R . C108 C -0.1009(20) 0.7843(10) 0.3494(10) 0.111(11) Uiso 1 d . . H10N H -0.1384(20) 0.8037(10) 0.3545(10) 0.166 Uiso 1 calc R . H10O H -0.1164(20) 0.7553(10) 0.3529(10) 0.166 Uiso 1 calc R . H10P H -0.0861(20) 0.7882(10) 0.3226(10) 0.166 Uiso 1 calc R . C109 C 0.3889(13) 0.7826(7) 0.1314(6) 0.059(6) Uiso 1 d . . C110 C 0.4329(18) 0.8132(8) 0.1215(8) 0.085(8) Uiso 1 d . . H110 H 0.4794(18) 0.8106(8) 0.1299(8) 0.102 Uiso 1 calc R . C111 C 0.4131(15) 0.8492(8) 0.0991(7) 0.073(7) Uiso 1 d . . H111 H 0.4465(15) 0.8690(8) 0.0915(7) 0.087 Uiso 1 calc R . C112 C 0.3499(15) 0.8549(8) 0.0892(7) 0.072(7) Uiso 1 d . . H112 H 0.3365(15) 0.8799(8) 0.0759(7) 0.087 Uiso 1 calc R . C113 C 0.3011(17) 0.8248(8) 0.0978(8) 0.079(7) Uiso 1 d . . H113 H 0.2550(17) 0.8278(8) 0.0889(8) 0.095 Uiso 1 calc R . C114 C 0.3223(14) 0.7895(7) 0.1201(7) 0.069(6) Uiso 1 d . . H114 H 0.2889(14) 0.7697(7) 0.1276(7) 0.082 Uiso 1 calc R . C115 C 0.3925(15) 0.6956(7) 0.1256(7) 0.069(6) Uiso 1 d . . H11C H 0.4016(15) 0.6682(7) 0.1383(7) 0.082 Uiso 1 calc R . H11D H 0.3432(15) 0.6964(7) 0.1184(7) 0.082 Uiso 1 calc R . C116 C 0.4316(15) 0.6968(7) 0.0883(7) 0.069(6) Uiso 1 d . . H11E H 0.4242(15) 0.7243(7) 0.0753(7) 0.083 Uiso 1 calc R . H11F H 0.4810(15) 0.6940(7) 0.0946(7) 0.083 Uiso 1 calc R . C117 C 0.4101(19) 0.6632(9) 0.0618(9) 0.100(9) Uiso 1 d . . H11G H 0.4363(19) 0.6648(9) 0.0379(9) 0.149 Uiso 1 calc R . H11H H 0.3614(19) 0.6663(9) 0.0552(9) 0.149 Uiso 1 calc R . H11I H 0.4181(19) 0.6360(9) 0.0745(9) 0.149 Uiso 1 calc R . C118 C 0.4978(15) 0.7368(7) 0.1673(8) 0.071(7) Uiso 1 d . . H11J H 0.5194(15) 0.7412(7) 0.1419(8) 0.085 Uiso 1 calc R . H11K H 0.5123(15) 0.7598(7) 0.1852(8) 0.085 Uiso 1 calc R . C119 C 0.5204(25) 0.6907(11) 0.1860(12) 0.128(13) Uiso 1 d . . H11L H 0.4938(25) 0.6853(11) 0.2096(12) 0.153 Uiso 1 calc R . H11M H 0.5094(25) 0.6684(11) 0.1667(12) 0.153 Uiso 1 calc R . C120 C 0.5892(35) 0.6890(17) 0.1959(17) 0.200(23) Uiso 1 d . . H12D H 0.6003(35) 0.6612(17) 0.2067(17) 0.299 Uiso 1 calc R . H12E H 0.6002(35) 0.7106(17) 0.2155(17) 0.299 Uiso 1 calc R . H12F H 0.6158(35) 0.6939(17) 0.1726(17) 0.299 Uiso 1 calc R . C121 C 0.6069(15) 0.6234(8) 0.3953(7) 0.069(6) Uiso 1 d . . C122 C 0.6639(17) 0.5987(9) 0.4042(9) 0.090(8) Uiso 1 d . . H122 H 0.6785(17) 0.5791(9) 0.3853(9) 0.108 Uiso 1 calc R . C123 C 0.6990(19) 0.6014(10) 0.4382(9) 0.098(9) Uiso 1 d . . H123 H 0.7404(19) 0.5865(10) 0.4427(9) 0.117 Uiso 1 calc R . C124 C 0.6722(23) 0.6265(11) 0.4658(12) 0.117(11) Uiso 1 d . . H124 H 0.6988(23) 0.6301(11) 0.4892(12) 0.141 Uiso 1 calc R . C125 C 0.6128(24) 0.6466(12) 0.4636(12) 0.129(13) Uiso 1 d . . H125 H 0.5939(24) 0.6613(12) 0.4849(12) 0.155 Uiso 1 calc R . C126 C 0.5792(17) 0.6436(8) 0.4241(8) 0.081(7) Uiso 1 d . . H126 H 0.5362(17) 0.6568(8) 0.4197(8) 0.098 Uiso 1 calc R . C127 C 0.6132(15) 0.5974(8) 0.3134(7) 0.071(6) Uiso 1 d . . H12G H 0.6588(15) 0.6106(8) 0.3159(7) 0.085 Uiso 1 calc R . H12H H 0.6185(15) 0.5673(8) 0.3202(7) 0.085 Uiso 1 calc R . C128 C 0.5875(21) 0.6007(11) 0.2700(9) 0.108(10) Uiso 1 d . . H12I H 0.5392(21) 0.5917(11) 0.2676(9) 0.130 Uiso 1 calc R . H12J H 0.5903(21) 0.6302(11) 0.2611(9) 0.130 Uiso 1 calc R . C129 C 0.6276(25) 0.5752(13) 0.2465(12) 0.142(15) Uiso 1 d . . H12K H 0.6115(25) 0.5775(13) 0.2192(12) 0.213 Uiso 1 calc R . H12L H 0.6241(25) 0.5460(13) 0.2551(12) 0.213 Uiso 1 calc R . H12M H 0.6753(25) 0.5844(13) 0.2488(12) 0.213 Uiso 1 calc R . C130 C 0.5655(16) 0.6778(8) 0.3369(8) 0.075(7) Uiso 1 d . . H13A H 0.5408(16) 0.6826(8) 0.3116(8) 0.091 Uiso 1 calc R . H13B H 0.5411(16) 0.6938(8) 0.3570(8) 0.091 Uiso 1 calc R . C131 C 0.6329(17) 0.6960(8) 0.3340(9) 0.083(8) Uiso 1 d . . H13C H 0.6546(17) 0.6848(8) 0.3104(9) 0.099 Uiso 1 calc R . H13D H 0.6612(17) 0.6874(8) 0.3570(9) 0.099 Uiso 1 calc R . C132 C 0.6315(24) 0.7427(11) 0.3318(11) 0.129(13) Uiso 1 d . . H13E H 0.6782(24) 0.7534(11) 0.3298(11) 0.193 Uiso 1 calc R . H13F H 0.6111(24) 0.7541(11) 0.3553(11) 0.193 Uiso 1 calc R . H13G H 0.6043(24) 0.7514(11) 0.3087(11) 0.193 Uiso 1 calc R . C133 C -0.0593(14) 0.7155(7) 0.1395(7) 0.066(6) Uiso 1 d . . C134 C -0.0443(16) 0.6775(8) 0.1201(8) 0.076(7) Uiso 1 d . . H134 H -0.0081(16) 0.6601(8) 0.1296(8) 0.091 Uiso 1 calc R . C135 C -0.0844(20) 0.6650(10) 0.0854(10) 0.104(10) Uiso 1 d . . H135 H -0.0725(20) 0.6410(10) 0.0705(10) 0.125 Uiso 1 calc R . C136 C -0.1425(28) 0.6902(14) 0.0745(13) 0.147(15) Uiso 1 d . . H136 H -0.1730(28) 0.6811(14) 0.0541(13) 0.177 Uiso 1 calc R . C137 C -0.1544(18) 0.7277(9) 0.0935(9) 0.090(8) Uiso 1 d . . H137 H -0.1907(18) 0.7458(9) 0.0853(9) 0.108 Uiso 1 calc R . C138 C -0.1118(17) 0.7379(9) 0.1247(8) 0.086(8) Uiso 1 d . . H138 H -0.1205(17) 0.7639(9) 0.1372(8) 0.103 Uiso 1 calc R . C139 C 0.0713(14) 0.7468(7) 0.1557(7) 0.065(6) Uiso 1 d . . H13H H 0.1081(14) 0.7531(7) 0.1752(7) 0.079 Uiso 1 calc R . H13I H 0.0880(14) 0.7243(7) 0.1385(7) 0.079 Uiso 1 calc R . C140 C 0.0575(17) 0.7878(8) 0.1298(8) 0.084(8) Uiso 1 d . . H14A H 0.0199(17) 0.7827(8) 0.1103(8) 0.100 Uiso 1 calc R . H14B H 0.0447(17) 0.8117(8) 0.1465(8) 0.100 Uiso 1 calc R . C141 C 0.1257(24) 0.7975(12) 0.1086(12) 0.133(13) Uiso 1 d . . H14C H 0.1197(24) 0.8226(12) 0.0922(12) 0.199 Uiso 1 calc R . H14D H 0.1377(24) 0.7735(12) 0.0922(12) 0.199 Uiso 1 calc R . H14E H 0.1623(24) 0.8024(12) 0.1282(12) 0.199 Uiso 1 calc R . C142 C -0.0499(17) 0.7707(8) 0.2030(8) 0.085(8) Uiso 1 d . . H14F H -0.0509(17) 0.7940(8) 0.1838(8) 0.102 Uiso 1 calc R . H14G H -0.0976(17) 0.7610(8) 0.2053(8) 0.102 Uiso 1 calc R . C143 C -0.0285(18) 0.7889(9) 0.2413(9) 0.097(9) Uiso 1 d . . H14H H -0.0300(18) 0.7672(9) 0.2619(9) 0.116 Uiso 1 calc R . H14I H -0.0597(18) 0.8120(9) 0.2483(9) 0.116 Uiso 1 calc R . C144 C 0.0504(19) 0.8071(10) 0.2377(10) 0.107(10) Uiso 1 d . . H14J H 0.0656(19) 0.8194(10) 0.2628(10) 0.160 Uiso 1 calc R . H14K H 0.0514(19) 0.8286(10) 0.2173(10) 0.160 Uiso 1 calc R . H14L H 0.0810(19) 0.7840(10) 0.2310(10) 0.160 Uiso 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 In1 0.0406(8) 0.0322(6) 0.0338(6) 0.0024(5) 0.0030(6) 0.0005(5) In2 0.0426(9) 0.0292(6) 0.0419(7) 0.0016(5) 0.0041(6) 0.0028(5) In3 0.0464(9) 0.0294(6) 0.0328(6) 0.0019(5) 0.0042(6) 0.0005(5) In4 0.0411(8) 0.0313(6) 0.0340(6) 0.0010(5) 0.0030(6) -0.0015(5) In5 0.0395(8) 0.0317(6) 0.0366(7) 0.0001(5) 0.0040(6) -0.0004(5) In6 0.0427(9) 0.0350(6) 0.0343(7) 0.0034(5) 0.0068(6) 0.0022(5) In7 0.0484(9) 0.0323(6) 0.0325(6) 0.0011(5) 0.0040(6) -0.0003(5) In8 0.0478(9) 0.0349(6) 0.0365(7) -0.0014(5) 0.0025(6) -0.0051(6) Se1 0.0437(12) 0.0357(9) 0.0357(9) -0.0003(7) -0.0005(9) -0.0010(8) Se2 0.0431(12) 0.0348(9) 0.0336(9) 0.0020(7) 0.0009(9) -0.0005(8) Se3 0.0424(12) 0.0277(8) 0.0329(9) 0.0005(6) 0.0012(8) 0.0003(7) Se4 0.0401(12) 0.0353(9) 0.0405(10) -0.0001(7) 0.0047(9) 0.0022(8) Se5 0.0456(12) 0.0285(8) 0.0387(10) 0.0060(7) 0.0035(9) 0.0004(7) Se6 0.0440(12) 0.0339(9) 0.0360(9) 0.0045(7) 0.0046(9) 0.0054(8) Se7 0.0514(13) 0.0279(8) 0.0334(9) 0.0040(7) 0.0050(9) -0.0025(8) Se8 0.0469(13) 0.0332(9) 0.0352(9) -0.0026(7) 0.0063(9) 0.0012(8) Se9 0.0433(12) 0.0352(9) 0.0313(9) 0.0002(7) 0.0078(8) 0.0004(8) Se10 0.0463(12) 0.0293(8) 0.0391(10) -0.0025(7) 0.0040(9) -0.0004(7) Se11 0.0435(12) 0.0359(9) 0.0363(9) 0.0004(7) 0.0053(9) -0.0063(8) Se12 0.0517(13) 0.0284(8) 0.0360(9) -0.0022(7) 0.0049(9) -0.0020(8) Se13 0.0411(12) 0.0303(8) 0.0387(10) 0.0052(7) 0.0048(9) -0.0017(7) Cu1 0.053(2) 0.0371(11) 0.0416(13) -0.0045(9) 0.0026(12) 0.0029(10) Cu2 0.069(2) 0.0365(12) 0.0369(12) -0.0023(9) 0.0025(13) 0.0037(11) Cu3 0.044(2) 0.0466(13) 0.0437(13) 0.0047(10) 0.0019(12) 0.0025(10) Cu4 0.049(2) 0.0323(11) 0.0419(12) 0.0065(9) 0.0042(12) -0.0043(9) Cu5 0.045(2) 0.0459(13) 0.0431(13) 0.0030(10) 0.0012(12) 0.0033(10) Cu6 0.056(2) 0.0417(12) 0.0442(13) 0.0093(10) 0.0086(13) -0.0074(11) Cl1 0.065(4) 0.033(2) 0.080(4) 0.001(2) 0.009(3) 0.012(2) Cl2 0.049(3) 0.055(3) 0.055(3) 0.004(2) 0.014(3) 0.005(2) Cl3 0.074(4) 0.054(3) 0.036(2) 0.007(2) 0.005(3) -0.002(2) Cl4 0.067(4) 0.057(3) 0.058(3) -0.016(2) -0.002(3) -0.025(3) P1 0.060(4) 0.050(3) 0.051(3) -0.007(2) 0.009(3) 0.014(3) P2 0.048(4) 0.066(3) 0.056(3) -0.006(3) 0.000(3) -0.003(3) P3 0.053(4) 0.052(3) 0.039(3) 0.010(2) 0.005(3) -0.006(2) P4 0.063(4) 0.048(3) 0.039(3) -0.006(2) 0.001(3) -0.003(2) P5 0.056(4) 0.052(3) 0.052(3) 0.014(2) 0.005(3) 0.011(3) P6 0.076(5) 0.043(3) 0.055(3) 0.007(2) 0.005(3) -0.017(3) P7 0.086(5) 0.044(3) 0.037(3) -0.004(2) -0.001(3) -0.001(3) P8 0.064(4) 0.033(2) 0.057(3) 0.003(2) 0.003(3) -0.010(2) P9 0.075(5) 0.040(3) 0.052(3) -0.003(2) 0.012(3) 0.008(3) P10 0.063(4) 0.072(4) 0.044(3) 0.010(3) 0.009(3) -0.003(3) P11 0.049(4) 0.061(3) 0.051(3) 0.004(2) 0.003(3) -0.005(3) P12 0.062(4) 0.053(3) 0.044(3) 0.007(2) 0.006(3) 0.015(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 In1 Se9 2.551(2) . ? In1 Se1 2.555(2) . ? In1 Se5 2.556(2) . ? In1 Se3 2.666(2) . ? In2 Cl1 2.421(5) . ? In2 Se4 2.569(2) . ? In2 Se5 2.576(3) . ? In2 Se10 2.578(2) . ? In3 Se6 2.542(3) . ? In3 Se12 2.550(2) . ? In3 Se7 2.555(2) . ? In3 Se3 2.661(2) . ? In4 Se10 2.552(2) . ? In4 Se2 2.553(2) . ? In4 Se13 2.556(3) . ? In4 Se3 2.666(2) . ? In5 Se11 2.556(2) . ? In5 Se4 2.556(2) . ? In5 Se8 2.564(2) . ? In5 Se3 2.662(3) . ? In6 Cl2 2.424(6) . ? In6 Se6 2.574(2) . ? In6 Se9 2.574(2) . ? In6 Se13 2.587(2) . ? In7 Cl3 2.428(5) . ? In7 Se7 2.574(2) . ? In7 Se8 2.576(2) . ? In7 Se2 2.583(3) . ? In8 Cl4 2.426(5) . ? In8 Se12 2.572(3) . ? In8 Se1 2.576(2) . ? In8 Se11 2.576(2) . ? Se1 Cu3 2.496(3) . ? Se2 Cu5 2.509(3) . ? Se4 Cu3 2.509(3) . ? Se5 Cu4 2.489(3) . ? Se6 Cu5 2.487(3) . ? Se7 Cu6 2.470(3) . ? Se8 Cu1 2.508(3) . ? Se9 Cu2 2.508(3) . ? Se10 Cu1 2.507(3) . ? Se11 Cu6 2.504(3) . ? Se12 Cu2 2.482(3) . ? Se13 Cu4 2.492(3) . ? Cu1 P4 2.285(5) . ? Cu1 P1 2.290(6) . ? Cu2 P9 2.294(7) . ? Cu2 P7 2.304(6) . ? Cu3 P11 2.290(7) . ? Cu3 P5 2.295(5) . ? Cu4 P3 2.277(6) . ? Cu4 P8 2.292(5) . ? Cu5 P2 2.283(7) . ? Cu5 P12 2.300(5) . ? Cu6 P10 2.293(7) . ? Cu6 P6 2.297(6) . ? P1 C7 1.79(2) . ? P1 C1 1.81(3) . ? P1 C10 1.85(2) . ? P2 C13 1.80(3) . ? P2 C19 1.83(2) . ? P2 C22 1.85(2) . ? P3 C25 1.81(2) . ? P3 C31 1.84(2) . ? P3 C34 1.84(2) . ? P4 C46 1.77(2) . ? P4 C37 1.81(3) . ? P4 C43 1.83(2) . ? P5 C58 1.79(2) . ? P5 C49 1.83(2) . ? P5 C55 1.83(3) . ? P6 C70 1.77(2) . ? P6 C67 1.80(2) . ? P6 C61 1.82(3) . ? P7 C73 1.78(2) . ? P7 C79 1.83(3) . ? P7 C82 1.85(2) . ? P8 C85 1.81(2) . ? P8 C94 1.81(2) . ? P8 C91 1.85(2) . ? P9 C106 1.82(3) . ? P9 C103 1.84(2) . ? P9 C97 1.84(2) . ? P10 C118 1.75(3) . ? P10 C115 1.80(2) . ? P10 C109 1.84(2) . ? P11 C127 1.82(3) . ? P11 C121 1.83(2) . ? P11 C130 1.84(2) . ? P12 C139 1.81(3) . ? P12 C133 1.83(2) . ? P12 C142 1.84(3) . ? C1 C2 1.31(4) . ? C1 C6 1.37(4) . ? C2 C3 1.55(7) . ? C3 C4 1.57(6) . ? C4 C5 1.45(6) . ? C5 C6 1.30(5) . ? C7 C8 1.55(4) . ? C8 C9 1.49(3) . ? C10 C11 1.54(4) . ? C11 C12 1.48(3) . ? C13 C18 1.34(4) . ? C13 C14 1.43(3) . ? C14 C15 1.25(5) . ? C15 C16 1.29(5) . ? C16 C17 1.26(5) . ? C17 C18 1.42(5) . ? C19 C20 1.63(4) . ? C20 C21 1.56(5) . ? C22 C23 1.58(4) . ? C23 C24 1.49(4) . ? C25 C26 1.37(3) . ? C25 C30 1.40(3) . ? C26 C27 1.45(4) . ? C27 C28 1.30(3) . ? C28 C29 1.30(3) . ? C29 C30 1.43(3) . ? C31 C32 1.54(3) . ? C32 C33 1.58(4) . ? C34 C35 1.41(3) . ? C35 C36 1.59(4) . ? C37 C42 1.30(3) . ? C37 C38 1.36(4) . ? C38 C39 1.43(4) . ? C39 C40 1.35(4) . ? C40 C41 1.43(5) . ? C41 C42 1.48(5) . ? C43 C44 1.59(4) . ? C44 C45 1.59(4) . ? C46 C47 1.53(3) . ? C47 C48 1.49(4) . ? C49 C50 1.34(3) . ? C49 C54 1.37(3) . ? C50 C51 1.48(4) . ? C51 C52 1.36(4) . ? C52 C53 1.48(4) . ? C53 C54 1.34(4) . ? C55 C56 1.54(4) . ? C56 C57 1.68(7) . ? C58 C59 1.68(5) . ? C59 C60 1.47(5) . ? C61 C66 1.38(3) . ? C61 C62 1.40(3) . ? C62 C63 1.44(4) . ? C63 C64 1.40(4) . ? C64 C65 1.31(4) . ? C65 C66 1.51(5) . ? C67 C68 1.60(4) . ? C68 C69 1.54(4) . ? C70 C71 1.55(3) . ? C71 C72 1.47(4) . ? C73 C74 1.33(3) . ? C73 C78 1.37(3) . ? C74 C75 1.40(3) . ? C75 C76 1.36(4) . ? C76 C77 1.32(4) . ? C77 C78 1.40(3) . ? C79 C80 1.53(3) . ? C80 C81 1.53(4) . ? C82 C83 1.82(4) . ? C83 C84 1.27(6) . ? C85 C86 1.33(3) . ? C85 C90 1.48(3) . ? C86 C87 1.43(4) . ? C87 C88 1.40(4) . ? C88 C89 1.31(3) . ? C89 C90 1.39(3) . ? C91 C92 1.49(3) . ? C92 C93 1.47(4) . ? C94 C95 1.52(3) . ? C95 C96 1.53(5) . ? C97 C98 1.34(3) . ? C97 C102 1.42(3) . ? C98 C99 1.43(4) . ? C99 C100 1.46(4) . ? C100 C101 1.27(4) . ? C101 C102 1.38(4) . ? C103 C104 1.58(4) . ? C104 C105 1.60(4) . ? C106 C107 1.57(4) . ? C107 C108 1.53(4) . ? C109 C110 1.35(4) . ? C109 C114 1.37(3) . ? C110 C111 1.43(3) . ? C111 C112 1.29(4) . ? C112 C113 1.39(4) . ? C113 C114 1.42(3) . ? C115 C116 1.51(4) . ? C116 C117 1.46(3) . ? C118 C119 1.66(4) . ? C119 C120 1.38(7) . ? C121 C126 1.31(4) . ? C121 C122 1.39(4) . ? C122 C123 1.34(4) . ? C123 C124 1.35(5) . ? C124 C125 1.33(5) . ? C125 C126 1.49(4) . ? C127 C128 1.56(4) . ? C128 C129 1.40(5) . ? C130 C131 1.45(4) . ? C131 C132 1.49(4) . ? C133 C138 1.34(4) . ? C133 C134 1.42(3) . ? C134 C135 1.46(4) . ? C135 C136 1.43(6) . ? C136 C137 1.38(5) . ? C137 C138 1.37(4) . ? C139 C140 1.60(3) . ? C140 C141 1.57(5) . ? C142 C143 1.48(4) . ? C143 C144 1.66(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 Se9 In1 Se1 115.23(7) . . ? Se9 In1 Se5 115.49(8) . . ? Se1 In1 Se5 115.83(7) . . ? Se9 In1 Se3 102.70(7) . . ? Se1 In1 Se3 102.69(8) . . ? Se5 In1 Se3 101.83(6) . . ? Cl1 In2 Se4 103.5(2) . . ? Cl1 In2 Se5 102.1(2) . . ? Se4 In2 Se5 114.40(8) . . ? Cl1 In2 Se10 103.39(14) . . ? Se4 In2 Se10 115.54(8) . . ? Se5 In2 Se10 115.35(8) . . ? Se6 In3 Se12 115.01(8) . . ? Se6 In3 Se7 115.33(8) . . ? Se12 In3 Se7 115.91(8) . . ? Se6 In3 Se3 102.09(7) . . ? Se12 In3 Se3 103.03(7) . . ? Se7 In3 Se3 102.53(7) . . ? Se10 In4 Se2 116.09(8) . . ? Se10 In4 Se13 115.06(7) . . ? Se2 In4 Se13 115.75(8) . . ? Se10 In4 Se3 101.67(7) . . ? Se2 In4 Se3 103.30(7) . . ? Se13 In4 Se3 101.73(7) . . ? Se11 In5 Se4 114.65(7) . . ? Se11 In5 Se8 116.21(7) . . ? Se4 In5 Se8 116.18(7) . . ? Se11 In5 Se3 102.47(7) . . ? Se4 In5 Se3 101.77(7) . . ? Se8 In5 Se3 102.27(8) . . ? Cl2 In6 Se6 101.75(13) . . ? Cl2 In6 Se9 103.63(14) . . ? Se6 In6 Se9 114.70(7) . . ? Cl2 In6 Se13 105.40(14) . . ? Se6 In6 Se13 113.87(7) . . ? Se9 In6 Se13 115.36(7) . . ? Cl3 In7 Se7 102.20(13) . . ? Cl3 In7 Se8 104.8(2) . . ? Se7 In7 Se8 114.61(8) . . ? Cl3 In7 Se2 104.5(2) . . ? Se7 In7 Se2 114.22(8) . . ? Se8 In7 Se2 114.55(7) . . ? Cl4 In8 Se12 101.8(2) . . ? Cl4 In8 Se1 104.44(15) . . ? Se12 In8 Se1 114.77(9) . . ? Cl4 In8 Se11 104.2(2) . . ? Se12 In8 Se11 114.98(8) . . ? Se1 In8 Se11 114.44(7) . . ? Cu3 Se1 In1 108.36(9) . . ? Cu3 Se1 In8 108.86(10) . . ? In1 Se1 In8 97.08(7) . . ? Cu5 Se2 In4 105.84(9) . . ? Cu5 Se2 In7 111.48(9) . . ? In4 Se2 In7 96.83(8) . . ? In3 Se3 In5 108.96(7) . . ? In3 Se3 In1 109.07(7) . . ? In5 Se3 In1 109.68(8) . . ? In3 Se3 In4 109.04(7) . . ? In5 Se3 In4 109.39(7) . . ? In1 Se3 In4 110.67(8) . . ? Cu3 Se4 In5 106.77(8) . . ? Cu3 Se4 In2 112.88(10) . . ? In5 Se4 In2 96.36(8) . . ? Cu4 Se5 In1 108.35(9) . . ? Cu4 Se5 In2 107.72(9) . . ? In1 Se5 In2 96.69(7) . . ? Cu5 Se6 In3 108.46(10) . . ? Cu5 Se6 In6 109.92(9) . . ? In3 Se6 In6 97.53(7) . . ? Cu6 Se7 In3 107.98(9) . . ? Cu6 Se7 In7 108.45(10) . . ? In3 Se7 In7 97.89(7) . . ? Cu1 Se8 In5 108.62(8) . . ? Cu1 Se8 In7 110.16(10) . . ? In5 Se8 In7 97.49(8) . . ? Cu2 Se9 In1 106.48(11) . . ? Cu2 Se9 In6 110.79(8) . . ? In1 Se9 In6 97.01(7) . . ? Cu1 Se10 In4 107.11(8) . . ? Cu1 Se10 In2 111.89(10) . . ? In4 Se10 In2 97.18(7) . . ? Cu6 Se11 In5 104.71(9) . . ? Cu6 Se11 In8 111.88(10) . . ? In5 Se11 In8 97.71(8) . . ? Cu2 Se12 In3 108.15(9) . . ? Cu2 Se12 In8 109.50(9) . . ? In3 Se12 In8 96.84(7) . . ? Cu4 Se13 In4 106.01(10) . . ? Cu4 Se13 In6 111.48(8) . . ? In4 Se13 In6 97.42(7) . . ? P4 Cu1 P1 106.4(2) . . ? P4 Cu1 Se10 110.5(2) . . ? P1 Cu1 Se10 111.5(2) . . ? P4 Cu1 Se8 111.9(2) . . ? P1 Cu1 Se8 109.5(2) . . ? Se10 Cu1 Se8 107.16(10) . . ? P9 Cu2 P7 106.7(2) . . ? P9 Cu2 Se12 108.2(2) . . ? P7 Cu2 Se12 112.5(2) . . ? P9 Cu2 Se9 111.2(2) . . ? P7 Cu2 Se9 109.3(2) . . ? Se12 Cu2 Se9 109.06(10) . . ? P11 Cu3 P5 105.9(2) . . ? P11 Cu3 Se1 112.5(2) . . ? P5 Cu3 Se1 110.1(2) . . ? P11 Cu3 Se4 110.7(2) . . ? P5 Cu3 Se4 109.4(2) . . ? Se1 Cu3 Se4 108.32(11) . . ? P3 Cu4 P8 105.8(2) . . ? P3 Cu4 Se5 109.4(2) . . ? P8 Cu4 Se5 112.0(2) . . ? P3 Cu4 Se13 108.0(2) . . ? P8 Cu4 Se13 111.6(2) . . ? Se5 Cu4 Se13 109.75(10) . . ? P2 Cu5 P12 108.0(2) . . ? P2 Cu5 Se6 111.7(2) . . ? P12 Cu5 Se6 107.7(2) . . ? P2 Cu5 Se2 108.8(2) . . ? P12 Cu5 Se2 111.7(2) . . ? Se6 Cu5 Se2 108.94(11) . . ? P10 Cu6 P6 106.6(2) . . ? P10 Cu6 Se7 113.1(2) . . ? P6 Cu6 Se7 108.0(2) . . ? P10 Cu6 Se11 109.7(2) . . ? P6 Cu6 Se11 109.4(2) . . ? Se7 Cu6 Se11 109.79(11) . . ? C7 P1 C1 104.6(11) . . ? C7 P1 C10 103.5(10) . . ? C1 P1 C10 103.6(12) . . ? C7 P1 Cu1 113.6(9) . . ? C1 P1 Cu1 114.2(8) . . ? C10 P1 Cu1 116.0(8) . . ? C13 P2 C19 105.4(12) . . ? C13 P2 C22 105.5(13) . . ? C19 P2 C22 101.6(11) . . ? C13 P2 Cu5 106.5(9) . . ? C19 P2 Cu5 115.5(10) . . ? C22 P2 Cu5 121.0(8) . . ? C25 P3 C31 102.3(10) . . ? C25 P3 C34 100.4(11) . . ? C31 P3 C34 102.7(9) . . ? C25 P3 Cu4 110.9(7) . . ? C31 P3 Cu4 117.8(8) . . ? C34 P3 Cu4 120.1(7) . . ? C46 P4 C37 97.9(11) . . ? C46 P4 C43 108.8(12) . . ? C37 P4 C43 102.8(11) . . ? C46 P4 Cu1 121.6(7) . . ? C37 P4 Cu1 109.1(8) . . ? C43 P4 Cu1 113.9(8) . . ? C58 P5 C49 102.9(11) . . ? C58 P5 C55 103.7(12) . . ? C49 P5 C55 99.5(12) . . ? C58 P5 Cu3 118.3(8) . . ? C49 P5 Cu3 111.6(7) . . ? C55 P5 Cu3 118.2(8) . . ? C70 P6 C67 104.4(12) . . ? C70 P6 C61 98.3(12) . . ? C67 P6 C61 101.7(11) . . ? C70 P6 Cu6 120.0(8) . . ? C67 P6 Cu6 118.2(8) . . ? C61 P6 Cu6 110.9(7) . . ? C73 P7 C79 98.4(10) . . ? C73 P7 C82 105.6(10) . . ? C79 P7 C82 103.5(11) . . ? C73 P7 Cu2 111.5(6) . . ? C79 P7 Cu2 122.0(8) . . ? C82 P7 Cu2 113.8(8) . . ? C85 P8 C94 99.0(10) . . ? C85 P8 C91 105.5(9) . . ? C94 P8 C91 100.2(10) . . ? C85 P8 Cu4 110.4(6) . . ? C94 P8 Cu4 123.3(8) . . ? C91 P8 Cu4 116.0(7) . . ? C106 P9 C103 101.0(11) . . ? C106 P9 C97 102.7(12) . . ? C103 P9 C97 104.9(11) . . ? C106 P9 Cu2 119.9(8) . . ? C103 P9 Cu2 116.2(10) . . ? C97 P9 Cu2 110.4(7) . . ? C118 P10 C115 104.3(13) . . ? C118 P10 C109 104.6(12) . . ? C115 P10 C109 99.6(11) . . ? C118 P10 Cu6 112.6(9) . . ? C115 P10 Cu6 124.9(9) . . ? C109 P10 Cu6 108.5(9) . . ? C127 P11 C121 106.6(12) . . ? C127 P11 C130 102.3(13) . . ? C121 P11 C130 96.9(11) . . ? C127 P11 Cu3 116.2(9) . . ? C121 P11 Cu3 110.7(10) . . ? C130 P11 Cu3 121.6(10) . . ? C139 P12 C133 99.9(11) . . ? C139 P12 C142 111.0(13) . . ? C133 P12 C142 99.3(12) . . ? C139 P12 Cu5 117.1(8) . . ? C133 P12 Cu5 113.5(8) . . ? C142 P12 Cu5 113.8(9) . . ? C2 C1 C6 116.0(33) . . ? C2 C1 P1 122.1(25) . . ? C6 C1 P1 121.9(23) . . ? C1 C2 C3 126.9(39) . . ? C2 C3 C4 108.7(47) . . ? C5 C4 C3 120.1(51) . . ? C6 C5 C4 116.5(42) . . ? C5 C6 C1 131.5(37) . . ? C8 C7 P1 115.8(17) . . ? C9 C8 C7 113.8(23) . . ? C11 C10 P1 116.3(17) . . ? C12 C11 C10 108.4(22) . . ? C18 C13 C14 114.0(26) . . ? C18 C13 P2 125.0(23) . . ? C14 C13 P2 121.0(18) . . ? C15 C14 C13 118.1(30) . . ? C14 C15 C16 126.3(42) . . ? C17 C16 C15 120.8(44) . . ? C16 C17 C18 117.0(42) . . ? C13 C18 C17 122.5(36) . . ? C20 C19 P2 110.4(20) . . ? C21 C20 C19 107.1(34) . . ? C23 C22 P2 113.7(17) . . ? C24 C23 C22 109.8(23) . . ? C26 C25 C30 114.4(20) . . ? C26 C25 P3 121.8(17) . . ? C30 C25 P3 123.7(15) . . ? C25 C26 C27 122.1(23) . . ? C28 C27 C26 118.6(25) . . ? C27 C28 C29 122.7(30) . . ? C28 C29 C30 120.2(25) . . ? C25 C30 C29 121.5(19) . . ? C32 C31 P3 110.1(16) . . ? C31 C32 C33 107.0(24) . . ? C35 C34 P3 116.7(15) . . ? C34 C35 C36 112.1(22) . . ? C42 C37 C38 118.7(28) . . ? C42 C37 P4 124.7(22) . . ? C38 C37 P4 116.7(19) . . ? C37 C38 C39 123.3(27) . . ? C40 C39 C38 118.4(32) . . ? C39 C40 C41 120.4(38) . . ? C40 C41 C42 115.6(35) . . ? C37 C42 C41 122.9(32) . . ? C44 C43 P4 110.1(17) . . ? C45 C44 C43 109.5(27) . . ? C47 C46 P4 120.7(16) . . ? C48 C47 C46 111.3(21) . . ? C50 C49 C54 119.7(23) . . ? C50 C49 P5 116.9(17) . . ? C54 C49 P5 123.4(17) . . ? C49 C50 C51 121.5(24) . . ? C52 C51 C50 118.8(27) . . ? C51 C52 C53 116.6(29) . . ? C54 C53 C52 121.5(26) . . ? C53 C54 C49 121.6(24) . . ? C56 C55 P5 112.5(20) . . ? C55 C56 C57 98.5(30) . . ? C59 C58 P5 111.0(18) . . ? C60 C59 C58 112.4(36) . . ? C66 C61 C62 119.3(26) . . ? C66 C61 P6 120.3(20) . . ? C62 C61 P6 120.3(18) . . ? C61 C62 C63 120.2(25) . . ? C64 C63 C62 118.8(32) . . ? C65 C64 C63 123.0(38) . . ? C64 C65 C66 118.6(34) . . ? C61 C66 C65 119.4(28) . . ? C68 C67 P6 112.1(16) . . ? C69 C68 C67 111.9(25) . . ? C71 C70 P6 120.3(18) . . ? C72 C71 C70 110.1(25) . . ? C74 C73 C78 115.8(19) . . ? C74 C73 P7 119.3(16) . . ? C78 C73 P7 124.1(17) . . ? C73 C74 C75 123.5(23) . . ? C76 C75 C74 119.8(26) . . ? C77 C76 C75 117.4(26) . . ? C76 C77 C78 123.1(26) . . ? C73 C78 C77 120.0(23) . . ? C80 C79 P7 114.8(19) . . ? C79 C80 C81 109.4(25) . . ? C83 C82 P7 103.7(18) . . ? C84 C83 C82 106.2(42) . . ? C86 C85 C90 117.0(19) . . ? C86 C85 P8 119.3(17) . . ? C90 C85 P8 123.2(16) . . ? C85 C86 C87 121.7(26) . . ? C88 C87 C86 119.0(30) . . ? C89 C88 C87 120.4(26) . . ? C88 C89 C90 122.2(26) . . ? C89 C90 C85 119.2(22) . . ? C92 C91 P8 112.2(18) . . ? C93 C92 C91 116.6(26) . . ? C95 C94 P8 119.5(19) . . ? C94 C95 C96 110.3(27) . . ? C98 C97 C102 118.6(24) . . ? C98 C97 P9 117.3(19) . . ? C102 C97 P9 123.9(18) . . ? C97 C98 C99 119.7(26) . . ? C98 C99 C100 117.1(28) . . ? C101 C100 C99 122.5(33) . . ? C100 C101 C102 119.3(30) . . ? C101 C102 C97 122.3(25) . . ? C104 C103 P9 111.2(18) . . ? C103 C104 C105 107.6(24) . . ? C107 C106 P9 115.1(17) . . ? C108 C107 C106 111.1(22) . . ? C110 C109 C114 115.2(23) . . ? C110 C109 P10 126.3(22) . . ? C114 C109 P10 118.3(19) . . ? C109 C110 C111 123.2(30) . . ? C112 C111 C110 120.0(28) . . ? C111 C112 C113 120.5(26) . . ? C112 C113 C114 117.9(29) . . ? C109 C114 C113 122.8(26) . . ? C116 C115 P10 118.1(18) . . ? C117 C116 C115 111.2(23) . . ? C119 C118 P10 106.7(21) . . ? C120 C119 C118 112.2(36) . . ? C126 C121 C122 117.4(25) . . ? C126 C121 P11 116.9(22) . . ? C122 C121 P11 124.6(22) . . ? C123 C122 C121 122.9(31) . . ? C122 C123 C124 116.4(35) . . ? C125 C124 C123 127.0(40) . . ? C124 C125 C126 112.5(40) . . ? C121 C126 C125 122.3(32) . . ? C128 C127 P11 115.2(22) . . ? C129 C128 C127 109.7(30) . . ? C131 C130 P11 118.8(21) . . ? C130 C131 C132 112.8(26) . . ? C138 C133 C134 116.5(23) . . ? C138 C133 P12 129.3(21) . . ? C134 C133 P12 114.2(18) . . ? C133 C134 C135 120.0(26) . . ? C136 C135 C134 117.5(35) . . ? C137 C136 C135 120.5(39) . . ? C138 C137 C136 117.4(32) . . ? C133 C138 C137 127.7(29) . . ? C140 C139 P12 115.1(19) . . ? C141 C140 C139 106.5(25) . . ? C143 C142 P12 121.2(23) . . ? C142 C143 C144 108.2(28) . . ? _refine_diff_density_max 1.842 _refine_diff_density_min -2.260 _refine_diff_density_rms 0.240 #===END data_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical '[Cu11In15Se16(SePh)24(PPh3)4]' _chemical_formula_sum 'C216 H180 Cu11 In15 P4 Se40' _chemical_formula_weight 8456.29 _chemical_melting_point ? _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 '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' 'In' 'In' -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M I-43m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' _cell_length_a 25.431(3) _cell_length_b 25.431(3) _cell_length_c 25.431(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 16446.6(32) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'cubic blocks' _exptl_crystal_colour red _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method ? _exptl_crystal_F_000 7540 _exptl_absorpt_coefficient_mu 6.201 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoKa _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47580 _diffrn_reflns_av_R_equivalents 0.0709 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2670 _reflns_number_observed 2539 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 27 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[s^2^(Fo^2^)+( 0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(2) _refine_ls_number_reflns 2643 _refine_ls_number_parameters 75 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0461 _refine_ls_R_factor_obs 0.0439 _refine_ls_wR_factor_all 0.1449 _refine_ls_wR_factor_obs 0.1429 _refine_ls_goodness_of_fit_all 1.281 _refine_ls_goodness_of_fit_obs 1.297 _refine_ls_restrained_S_all 1.282 _refine_ls_restrained_S_obs 1.297 _refine_ls_shift/esd_max 0.011 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group In1 In 0.0000 0.10758(5) 0.0000 0.0307(3) Uiso 0.50 d SP . Cu1 Cu 0.0000 0.10758(5) 0.0000 0.0307(3) Uiso 0.50 d SP . In2 In 0.14859(2) 0.14859(2) 0.03656(3) 0.0297(2) Uani 1 d S . Se1 Se -0.05918(4) 0.05918(4) 0.05918(4) 0.0323(4) Uani 1 d S . Se2 Se 0.05264(3) 0.17576(4) 0.05264(3) 0.0289(3) Uani 1 d S . Se3 Se 0.17096(3) 0.17096(3) -0.06030(4) 0.0335(3) Uani 1 d S . Se4 Se 0.20711(3) 0.20711(3) 0.09559(5) 0.0610(5) Uani 1 d S . Cu2 Cu 0.18798(5) 0.18798(5) 0.18798(5) 0.0358(5) Uani 1 d S . Cu3 Cu 0.11463(5) 0.11463(5) -0.11463(5) 0.0332(5) Uani 1 d S . P1 P 0.24009(10) 0.24009(10) 0.24009(10) 0.0388(11) Uani 1 d S . C1 C 0.1347(4) 0.2405(4) -0.0579(5) 0.039(3) Uiso 0.50 d PG 1 C2 C 0.0803(4) 0.2445(4) -0.0615(4) 0.037(4) Uiso 0.50 d PG 1 C3 C 0.0563(4) 0.2936(5) -0.0577(6) 0.077(5) Uiso 1 d SG 1 C4 C 0.0869(6) 0.3388(3) -0.0566(6) 0.081(7) Uiso 0.50 d PG 1 C5 C 0.1413(6) 0.3348(4) -0.0531(6) 0.093(8) Uiso 0.50 d PG 1 C6 C 0.1652(3) 0.2857(5) -0.0538(6) 0.070(6) Uiso 0.50 d PG 1 C7 C 0.2192(5) 0.2452(4) 0.3077(4) 0.045(4) Uiso 0.50 d PG 2 C8 C 0.1994(6) 0.1990(4) 0.3312(5) 0.064(4) Uiso 1 d SG 2 C9 C 0.1790(6) 0.2023(4) 0.3819(5) 0.069(6) Uiso 0.50 d PG 2 C10 C 0.1785(6) 0.2498(5) 0.4090(4) 0.082(7) Uiso 0.50 d PG 2 C11 C 0.1983(6) 0.2949(4) 0.3855(5) 0.074(6) Uiso 0.50 d PG 2 C12 C 0.2187(5) 0.2927(4) 0.3348(5) 0.055(5) Uiso 0.50 d PG 2 C13 C 0.2754(5) 0.1667(5) 0.0746(6) 0.052(4) Uiso 0.50 d PG 3 C14 C 0.2910(5) 0.1204(5) 0.0992(5) 0.080(7) Uiso 0.50 d PG 3 C15 C 0.3377(6) 0.0960(5) 0.0845(6) 0.072(5) Uiso 0.50 d PG 3 C16 C 0.3687(5) 0.1178(7) 0.0452(7) 0.095(8) Uiso 0.50 d PG 3 C17 C 0.3531(7) 0.1641(7) 0.0206(7) 0.106(9) Uiso 0.50 d PG 3 C18 C 0.3065(7) 0.1885(5) 0.0353(6) 0.087(8) Uiso 0.50 d PG 3 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 In2 0.0308(3) 0.0308(3) 0.0276(4) -0.0010(2) -0.0010(2) -0.0076(3) Se1 0.0323(4) 0.0323(4) 0.0323(4) -0.0045(4) 0.0045(4) 0.0045(4) Se2 0.0294(3) 0.0280(5) 0.0294(3) -0.0015(3) -0.0021(4) -0.0015(3) Se3 0.0352(4) 0.0352(4) 0.0299(5) 0.0019(3) 0.0019(3) -0.0097(4) Se4 0.0744(7) 0.0744(7) 0.0343(6) -0.0043(3) -0.0043(3) -0.0476(8) Cu2 0.0358(5) 0.0358(5) 0.0358(5) -0.0075(5) -0.0075(5) -0.0075(5) Cu3 0.0332(5) 0.0332(5) 0.0332(5) 0.0010(5) 0.0010(5) -0.0010(5) P1 0.0388(11) 0.0388(11) 0.0388(11) -0.0084(11) -0.0084(11) -0.0084(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 In1 Se1 2.4587(10) . ? In1 Se1 2.4587(10) 3 ? In1 Se2 2.5672(13) 3 ? In1 Se2 2.5672(13) . ? Cu1 Se1 2.4587(10) . ? Cu1 Se1 2.4587(10) 3 ? Cu1 Se2 2.5672(13) 3 ? Cu1 Se2 2.5672(13) . ? In2 Se2 2.5686(8) 9 ? In2 Se2 2.5686(8) . ? In2 Se4 2.5854(14) . ? In2 Se3 2.5915(12) . ? Se1 Cu3 2.442(3) 3 ? Se1 Cu1 2.4587(10) 10 ? Se1 In1 2.4587(10) 10 ? Se1 In1 2.4588(10) 5 ? Se1 Cu1 2.4588(10) 5 ? Se2 In2 2.5687(8) 5 ? Se3 C1 1.995(8) . ? Se3 C1 1.995(8) 13 ? Se3 Cu3 2.4523(13) . ? Se4 C13 2.088(10) 13 ? Se4 C13 2.088(10) . ? Se4 Cu2 2.4482(14) . ? Cu2 P1 2.295(5) . ? Cu2 Se4 2.4483(14) 5 ? Cu2 Se4 2.4484(14) 9 ? Cu3 Se1 2.442(3) 3 ? Cu3 Se3 2.4522(13) 8 ? Cu3 Se3 2.4522(12) 11 ? P1 C7 1.804(9) 17 ? P1 C7 1.804(9) 9 ? P1 C7 1.804(9) 21 ? P1 C7 1.804(9) . ? P1 C7 1.804(9) 13 ? P1 C7 1.804(9) 5 ? C1 C2 1.39 . ? C1 C6 1.39 . ? C1 C2 1.95(2) 23 ? C2 C2 0.68(2) 23 ? C2 C3 1.382(6) 23 ? C2 C3 1.39 . ? C2 C1 1.95(2) 23 ? C3 C3 0.05(3) 23 ? C3 C4 1.367(12) 23 ? C3 C2 1.382(5) 23 ? C3 C4 1.39 . ? C4 C4 1.09(3) 23 ? C4 C3 1.367(10) 23 ? C4 C5 1.39 . ? C5 C6 1.39 . ? C7 C7 0.94(2) 13 ? C7 C8 1.41 . ? C7 C12 1.39 . ? C8 C9 1.39 . ? C8 C9 1.387(9) 13 ? C8 C7 1.407(9) 13 ? C9 C9 0.84(3) 13 ? C9 C10 1.39 . ? C9 C10 2.02(3) 13 ? C10 C11 1.39 . ? C10 C9 2.02(2) 13 ? C11 C12 1.39 . ? C12 C12 1.52(2) 17 ? C13 C14 1.39 . ? C13 C18 1.39 . ? C14 C14 0.76(2) 17 ? C14 C15 1.39 . ? C14 C15 1.499(10) 17 ? C15 C15 0.41(3) 17 ? C15 C16 1.39 . ? C15 C14 1.499(9) 17 ? C15 C16 1.74(3) 17 ? C16 C17 1.39 . ? C16 C15 1.74(2) 17 ? C17 C18 1.39 . ? 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 Se1 In1 Se1 119.91(9) . 3 ? Se1 In1 Se2 109.76(2) . 3 ? Se1 In1 Se2 109.76(2) 3 3 ? Se1 In1 Se2 109.76(2) . . ? Se1 In1 Se2 109.76(2) 3 . ? Se2 In1 Se2 95.04(6) 3 . ? Se1 Cu1 Se1 119.91(9) . 3 ? Se1 Cu1 Se2 109.76(2) . 3 ? Se1 Cu1 Se2 109.76(2) 3 3 ? Se1 Cu1 Se2 109.76(2) . . ? Se1 Cu1 Se2 109.76(2) 3 . ? Se2 Cu1 Se2 95.04(6) 3 . ? Se2 In2 Se2 119.06(5) 9 . ? Se2 In2 Se4 107.43(3) 9 . ? Se2 In2 Se4 107.43(3) . . ? Se2 In2 Se3 107.51(3) 9 . ? Se2 In2 Se3 107.51(3) . . ? Se4 In2 Se3 107.40(4) . . ? Cu3 Se1 In1 114.69(4) 3 . ? Cu3 Se1 Cu1 114.69(4) 3 . ? In1 Se1 Cu1 0.00(5) . . ? Cu3 Se1 Cu1 114.69(4) 3 10 ? In1 Se1 Cu1 103.78(5) . 10 ? Cu1 Se1 Cu1 103.78(5) . 10 ? Cu3 Se1 In1 114.69(4) 3 10 ? In1 Se1 In1 103.78(5) . 10 ? Cu1 Se1 In1 103.78(5) . 10 ? Cu1 Se1 In1 0.00(5) 10 10 ? Cu3 Se1 In1 114.69(4) 3 5 ? In1 Se1 In1 103.78(5) . 5 ? Cu1 Se1 In1 103.78(5) . 5 ? Cu1 Se1 In1 103.78(5) 10 5 ? In1 Se1 In1 103.78(5) 10 5 ? Cu3 Se1 Cu1 114.69(4) 3 5 ? In1 Se1 Cu1 103.78(5) . 5 ? Cu1 Se1 Cu1 103.78(5) . 5 ? Cu1 Se1 Cu1 103.78(5) 10 5 ? In1 Se1 Cu1 103.78(5) 10 5 ? In1 Se1 Cu1 0.00(5) 5 5 ? Cu1 Se2 In1 0.00(4) . . ? Cu1 Se2 In2 103.34(3) . . ? In1 Se2 In2 103.34(3) . . ? Cu1 Se2 In2 103.34(3) . 5 ? In1 Se2 In2 103.34(3) . 5 ? In2 Se2 In2 103.30(4) . 5 ? C1 Se3 C1 144.9(6) . 13 ? C1 Se3 Cu3 105.3(3) . . ? C1 Se3 Cu3 105.3(3) 13 . ? C1 Se3 In2 93.7(3) . . ? C1 Se3 In2 93.7(3) 13 . ? Cu3 Se3 In2 106.20(6) . . ? C13 Se4 C13 139.0(8) 13 . ? C13 Se4 Cu2 108.2(4) 13 . ? C13 Se4 Cu2 108.2(4) . . ? C13 Se4 In2 92.7(4) 13 . ? C13 Se4 In2 92.7(4) . . ? Cu2 Se4 In2 109.17(6) . . ? P1 Cu2 Se4 108.94(5) . . ? P1 Cu2 Se4 108.94(5) . 5 ? Se4 Cu2 Se4 110.00(5) . 5 ? P1 Cu2 Se4 108.94(5) . 9 ? Se4 Cu2 Se4 110.00(5) . 9 ? Se4 Cu2 Se4 110.00(5) 5 9 ? Se1 Cu3 Se3 110.45(5) 3 8 ? Se1 Cu3 Se3 110.45(5) 3 11 ? Se3 Cu3 Se3 108.48(5) 8 11 ? Se1 Cu3 Se3 110.45(5) 3 . ? Se3 Cu3 Se3 108.48(5) 8 . ? Se3 Cu3 Se3 108.48(5) 11 . ? C7 P1 C7 30.1(8) 17 9 ? C7 P1 C7 103.5(5) 17 21 ? C7 P1 C7 77.0(7) 9 21 ? C7 P1 C7 77.0(7) 17 . ? C7 P1 C7 103.5(5) 9 . ? C7 P1 C7 123.8(8) 21 . ? C7 P1 C7 103.5(5) 17 13 ? C7 P1 C7 123.8(8) 9 13 ? C7 P1 C7 103.5(5) 21 13 ? C7 P1 C7 30.1(8) . 13 ? C7 P1 C7 123.8(8) 17 5 ? C7 P1 C7 103.5(5) 9 5 ? C7 P1 C7 30.1(8) 21 5 ? C7 P1 C7 103.5(5) . 5 ? C7 P1 C7 77.0(7) 13 5 ? C7 P1 Cu2 115.0(4) 17 . ? C7 P1 Cu2 115.0(4) 9 . ? C7 P1 Cu2 115.0(4) 21 . ? C7 P1 Cu2 115.0(4) . . ? C7 P1 Cu2 115.0(4) 13 . ? C7 P1 Cu2 115.0(4) 5 . ? C2 C1 C6 120.0 . . ? C2 C1 C2 13.3(3) . 23 ? C6 C1 C2 120.8 . 23 ? C2 C1 Se3 121.5(6) . . ? C6 C1 Se3 118.5(6) . . ? C2 C1 Se3 118.6(7) 23 . ? C2 C2 C3 76.8(11) 23 23 ? C2 C2 C3 74.9 23 . ? C3 C2 C3 2.0(11) 23 . ? C2 C2 C1 138.5 23 . ? C3 C2 C1 118.3(8) 23 . ? C3 C2 C1 119.7 . . ? C2 C2 C1 28.2(8) 23 23 ? C3 C2 C1 90.9(8) 23 23 ? C3 C2 C1 89.1(7) . 23 ? C1 C2 C1 110.3(8) . 23 ? C3 C3 C4 112.4(13) 23 23 ? C3 C3 C2 103.1(10) 23 23 ? C4 C3 C2 122.2(9) 23 23 ? C3 C3 C2 74.9(8) 23 . ? C4 C3 C2 135.6 23 . ? C2 C3 C2 28.3(8) 23 . ? C3 C3 C4 65.8(10) 23 . ? C4 C3 C4 46.6(13) 23 . ? C2 C3 C4 134.8(3) 23 . ? C2 C3 C4 119.9 . . ? C4 C4 C3 67.6(10) 23 23 ? C4 C4 C5 138.5 23 . ? C3 C4 C5 118.6(7) 23 . ? C4 C4 C3 65.8 23 . ? C3 C4 C3 1.9(10) 23 . ? C5 C4 C3 119.9 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C7 C7 C8 70.3(5) 13 . ? C7 C7 C12 128.4(6) 13 . ? C8 C7 C12 120.6 . . ? C7 C7 P1 75.0(4) 13 . ? C8 C7 P1 116.6(7) . . ? C12 C7 P1 122.6(7) . . ? C9 C8 C7 118.3 . . ? C9 C8 C9 35.1(12) . 13 ? C7 C8 C9 132.8(2) . 13 ? C9 C8 C7 132.8(3) . 13 ? C7 C8 C7 38.8(9) . 13 ? C9 C8 C7 119.0(10) 13 13 ? C9 C9 C8 72.2 13 . ? C9 C9 C10 128.4 13 . ? C8 C9 C10 121.1 . . ? C9 C9 C10 32.7(5) 13 13 ? C8 C9 C10 88.1(2) . 13 ? C10 C9 C10 95.7(5) . 13 ? C11 C10 C9 120.0 . . ? C11 C10 C9 118.70(7) . 13 ? C9 C10 C9 19.0(4) . 13 ? C12 C11 C10 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 C12 128.8 . 17 ? C7 C12 C12 105.2 . 17 ? C14 C13 C18 120.0 . . ? C14 C13 Se4 122.6(8) . . ? C18 C13 Se4 117.4(8) . . ? C14 C14 C15 82.8 17 . ? C14 C14 C13 156.5 17 . ? C15 C14 C13 120.0 . . ? C14 C14 C15 66.9(9) 17 17 ? C15 C14 C15 15.9(9) . 17 ? C13 C14 C15 135.8(9) . 17 ? C15 C15 C16 142.3 17 . ? C15 C15 C14 97.2 17 . ? C16 C15 C14 120.0 . . ? C15 C15 C14 66.9(8) 17 17 ? C16 C15 C14 150.0(8) . 17 ? C14 C15 C14 30.3(8) . 17 ? C15 C15 C16 29.3(6) 17 17 ? C16 C15 C16 113.0(6) . 17 ? C14 C15 C16 126.1(6) . 17 ? C14 C15 C16 95.9(11) 17 17 ? C15 C16 C17 120.0 . . ? C15 C16 C15 8.4(4) . 17 ? C17 C16 C15 128.2(4) . 17 ? C18 C17 C16 120.0 . . ? C17 C18 C13 120.0 . . ? _refine_diff_density_max 1.174 _refine_diff_density_min -0.633 _refine_diff_density_rms 0.162