# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Robert Davies' _publ_contact_author_address ; Dept of Chemistry Imperial College London Exhibition Road South Kensington London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email R.DAVIES@IMPERIAL.AC.UK _publ_section_title ; Discrete copper(I) clusters with Cu6P6Se6 and Cu6P4Se6 cores ; loop_ _publ_author_name 'Robert Davies' 'M. Giovanna Martinelli' 'Andrew J. P. White' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 604049' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C124 H112 Cl8 Cu6 P10 Se6' _chemical_formula_weight 3050.44 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.440(2) _cell_length_b 15.973(4) _cell_length_c 16.656(3) _cell_angle_alpha 62.152(13) _cell_angle_beta 64.756(10) _cell_angle_gamma 89.518(13) _cell_volume 3190.4(10) _cell_formula_units_Z 1 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 29 _cell_measurement_theta_min 4.77 _cell_measurement_theta_max 11.46 _exptl_crystal_description plates _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 3.033 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4127 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 24.64 _diffrn_reflns_number 8115 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.1078 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 22.50 _reflns_number_total 7770 _reflns_number_gt 5039 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0395P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7770 _refine_ls_number_parameters 634 _refine_ls_number_restraints 191 _refine_ls_R_factor_all 0.1046 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1095 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.41548(8) 0.40295(7) 0.55046(7) 0.0246(2) Uani 1 1 d . . . Se2 Se 0.32453(6) 0.31025(6) 0.73913(6) 0.0244(2) Uani 1 1 d . . . Cu3 Cu 0.37320(8) 0.44855(7) 0.75954(7) 0.0254(2) Uani 1 1 d . . . P4 P 0.33257(15) 0.57102(14) 0.65054(14) 0.0204(4) Uani 1 1 d . . . Se5 Se 0.40867(6) 0.57929(5) 0.49797(6) 0.0208(2) Uani 1 1 d . . . Cu6 Cu 0.41175(8) 0.66882(7) 0.32762(8) 0.0285(3) Uani 1 1 d . . . Se7 Se 0.45219(6) 0.53968(6) 0.28148(6) 0.0245(2) Uani 1 1 d . . . P8 P 0.37205(16) 0.40292(14) 0.43829(16) 0.0226(5) Uani 1 1 d . . . P9 P 0.43577(16) 0.23011(14) 0.77153(15) 0.0240(5) Uani 1 1 d . . . P10 P 0.2915(2) 0.38804(18) 0.93355(17) 0.0375(6) Uani 1 1 d . . . H10 H 0.3168 0.3062 0.9716 0.045 Uiso 1 1 calc R . . P11 P 0.26964(18) 0.70303(16) 0.33451(17) 0.0315(5) Uani 1 1 d . . . H11 H 0.2030 0.6224 0.4080 0.038 Uiso 1 1 calc R . . C1 C 0.2918(4) 0.7200(3) 0.6937(3) 0.035(2) Uani 1 1 d G . . H1A H 0.2382 0.6706 0.7564 0.042 Uiso 1 1 calc R . . C2 C 0.3063(4) 0.8148(4) 0.6740(4) 0.047(3) Uani 1 1 d G . . H2A H 0.2626 0.8303 0.7231 0.057 Uiso 1 1 calc R . . C3 C 0.3848(5) 0.8871(3) 0.5822(4) 0.043(2) Uani 1 1 d G . . H3A H 0.3948 0.9519 0.5687 0.051 Uiso 1 1 calc R . . C4 C 0.4489(4) 0.8644(3) 0.5103(3) 0.037(2) Uani 1 1 d G . . H4A H 0.5025 0.9138 0.4476 0.044 Uiso 1 1 calc R . . C5 C 0.4344(4) 0.7695(3) 0.5301(3) 0.030(2) Uani 1 1 d G . . H5A H 0.4781 0.7541 0.4809 0.036 Uiso 1 1 calc R . . C6 C 0.3559(4) 0.6973(3) 0.6218(4) 0.0237(18) Uani 1 1 d G . . C7 C 0.1353(4) 0.4640(3) 0.7727(4) 0.041(2) Uani 1 1 d G . . H7A H 0.1596 0.4131 0.8095 0.049 Uiso 1 1 calc R . . C8 C 0.0349(4) 0.4510(4) 0.8043(4) 0.058(3) Uani 1 1 d G . . H8A H -0.0095 0.3912 0.8627 0.069 Uiso 1 1 calc R . . C9 C -0.0006(3) 0.5255(5) 0.7504(5) 0.049(3) Uani 1 1 d G . . H9A H -0.0693 0.5166 0.7720 0.059 Uiso 1 1 calc R . . C10 C 0.0643(4) 0.6130(4) 0.6649(5) 0.043(2) Uani 1 1 d G . . H10A H 0.0401 0.6638 0.6281 0.052 Uiso 1 1 calc R . . C11 C 0.1648(4) 0.6259(3) 0.6333(4) 0.040(2) Uani 1 1 d G . . H11A H 0.2091 0.6857 0.5748 0.048 Uiso 1 1 calc R . . C12 C 0.2003(3) 0.5515(4) 0.6872(4) 0.0234(18) Uani 1 1 d G . . C13 C 0.1829(4) 0.4101(5) 0.5595(5) 0.044(2) Uani 1 1 d G . . H13A H 0.2100 0.4163 0.5987 0.052 Uiso 1 1 calc R . . C14 C 0.0835(4) 0.4066(6) 0.5892(5) 0.066(4) Uani 1 1 d G . . H14A H 0.0427 0.4103 0.6487 0.080 Uiso 1 1 calc R . . C15 C 0.0438(4) 0.3977(6) 0.5320(7) 0.064(4) Uani 1 1 d G . . H15A H -0.0241 0.3953 0.5523 0.077 Uiso 1 1 calc R . . C16 C 0.1036(5) 0.3922(6) 0.4451(6) 0.070(4) Uani 1 1 d G . . H16A H 0.0765 0.3861 0.4059 0.084 Uiso 1 1 calc R . . C17 C 0.2030(5) 0.3958(5) 0.4154(4) 0.053(3) Uani 1 1 d G . . H17A H 0.2438 0.3920 0.3559 0.064 Uiso 1 1 calc R . . C18 C 0.2427(3) 0.4047(5) 0.4726(4) 0.032(2) Uani 1 1 d G . . C19 C 0.4477(5) 0.3127(3) 0.3173(3) 0.040(2) Uani 1 1 d G . . H19A H 0.4916 0.3741 0.2622 0.048 Uiso 1 1 calc R . . C20 C 0.4497(5) 0.2331(4) 0.3037(4) 0.058(3) Uani 1 1 d G . . H20A H 0.4949 0.2401 0.2393 0.069 Uiso 1 1 calc R . . C21 C 0.3856(6) 0.1433(3) 0.3844(5) 0.055(3) Uani 1 1 d G . . H21A H 0.3869 0.0889 0.3750 0.066 Uiso 1 1 calc R . . C22 C 0.3194(5) 0.1331(3) 0.4787(4) 0.060(3) Uani 1 1 d G . . H22A H 0.2756 0.0718 0.5338 0.072 Uiso 1 1 calc R . . C23 C 0.3174(4) 0.2127(4) 0.4923(4) 0.044(3) Uani 1 1 d G . . H23A H 0.2722 0.2058 0.5567 0.053 Uiso 1 1 calc R . . C24 C 0.3816(4) 0.3025(3) 0.4116(4) 0.0263(19) Uani 1 1 d G . . C25 C 0.3383(4) 0.0928(4) 0.7536(5) 0.036(2) Uani 1 1 d G . . H25A H 0.2951 0.1345 0.7434 0.043 Uiso 1 1 calc R . . C26 C 0.3260(4) 0.0067(4) 0.7536(5) 0.050(3) Uani 1 1 d G . . H26A H 0.2743 -0.0104 0.7434 0.060 Uiso 1 1 calc R . . C27 C 0.3892(5) -0.0544(3) 0.7685(5) 0.050(3) Uani 1 1 d G . . H27A H 0.3807 -0.1133 0.7685 0.060 Uiso 1 1 calc R . . C28 C 0.4648(5) -0.0295(4) 0.7835(5) 0.051(3) Uani 1 1 d G . . H28A H 0.5080 -0.0712 0.7937 0.062 Uiso 1 1 calc R . . C29 C 0.4771(4) 0.0566(4) 0.7835(5) 0.042(2) Uani 1 1 d G . . H29A H 0.5288 0.0737 0.7937 0.050 Uiso 1 1 calc R . . C30 C 0.4139(4) 0.1177(3) 0.7686(5) 0.030(2) Uani 1 1 d G . . C31 C 0.2970(4) 0.1169(4) 0.9846(4) 0.045(3) Uani 1 1 d G . . H31A H 0.2546 0.1004 0.9637 0.054 Uiso 1 1 calc R . . C32 C 0.2656(5) 0.0801(5) 1.0889(4) 0.064(4) Uani 1 1 d G . . H32A H 0.2018 0.0384 1.1393 0.077 Uiso 1 1 calc R . . C33 C 0.3277(6) 0.1043(6) 1.1195(3) 0.071(4) Uani 1 1 d G . . H33A H 0.3062 0.0792 1.1908 0.085 Uiso 1 1 calc R . . C34 C 0.4211(6) 0.1653(6) 1.0458(5) 0.074(4) Uani 1 1 d G . . H34A H 0.4634 0.1818 1.0667 0.089 Uiso 1 1 calc R . . C35 C 0.4524(4) 0.2021(5) 0.9415(4) 0.048(3) Uani 1 1 d G . . H35A H 0.5162 0.2438 0.8911 0.057 Uiso 1 1 calc R . . C36 C 0.3904(4) 0.1779(4) 0.9109(3) 0.036(2) Uani 1 1 d G . . C37 C 0.1115(5) 0.2730(5) 1.0073(6) 0.058(3) Uani 1 1 d G . . H37A H 0.1509 0.2363 0.9816 0.070 Uiso 1 1 calc R . . C38 C 0.0096(5) 0.2476(5) 1.0503(7) 0.085(5) Uani 1 1 d G . . H38A H -0.0207 0.1935 1.0539 0.102 Uiso 1 1 calc R . . C39 C -0.0480(4) 0.3012(7) 1.0879(7) 0.081(4) Uani 1 1 d G . . H39A H -0.1176 0.2838 1.1173 0.097 Uiso 1 1 calc R . . C40 C -0.0036(5) 0.3804(6) 1.0825(7) 0.079(4) Uani 1 1 d G . . H40A H -0.0430 0.4171 1.1082 0.095 Uiso 1 1 calc R . . C41 C 0.0983(5) 0.4059(5) 1.0395(6) 0.066(4) Uani 1 1 d G . . H41A H 0.1286 0.4600 1.0359 0.080 Uiso 1 1 calc R . . C42 C 0.1559(4) 0.3522(5) 1.0019(5) 0.041(3) Uani 1 1 d G . . C43 C 0.3377(8) 0.4040(5) 1.0724(6) 0.078(4) Uani 1 1 d G . . H43A H 0.3302 0.3353 1.1047 0.094 Uiso 1 1 calc R . . C44 C 0.3628(8) 0.4548(8) 1.1110(6) 0.098(5) Uani 1 1 d GU . . H44A H 0.3725 0.4210 1.1698 0.118 Uiso 1 1 calc R . . C45 C 0.3737(9) 0.5553(8) 1.0636(8) 0.096(5) Uani 1 1 d GU . . H45A H 0.3909 0.5900 1.0900 0.115 Uiso 1 1 calc R . . C46 C 0.3595(8) 0.6048(5) 0.9776(7) 0.094(5) Uani 1 1 d G . . H46A H 0.3670 0.6734 0.9452 0.113 Uiso 1 1 calc R . . C47 C 0.3344(7) 0.5539(5) 0.9390(5) 0.059(3) Uani 1 1 d G . . H47A H 0.3247 0.5877 0.8802 0.071 Uiso 1 1 calc R . . C48 C 0.3235(6) 0.4535(5) 0.9864(5) 0.048(3) Uani 1 1 d G . . C49 C 0.2812(4) 0.8369(5) 0.3936(5) 0.045(3) Uani 1 1 d G . . H49A H 0.3400 0.8180 0.3927 0.054 Uiso 1 1 calc R . . C50 C 0.2499(6) 0.9058(5) 0.4212(6) 0.071(4) Uani 1 1 d G . . H50A H 0.2872 0.9340 0.4393 0.085 Uiso 1 1 calc R . . C51 C 0.1639(7) 0.9335(5) 0.4225(6) 0.071(4) Uani 1 1 d G . . H51A H 0.1425 0.9806 0.4414 0.085 Uiso 1 1 calc R . . C52 C 0.1093(5) 0.8923(6) 0.3962(6) 0.071(4) Uani 1 1 d G . . H52A H 0.0506 0.9113 0.3971 0.085 Uiso 1 1 calc R . . C53 C 0.1406(5) 0.8234(5) 0.3685(6) 0.052(3) Uani 1 1 d G . . H53A H 0.1033 0.7953 0.3505 0.063 Uiso 1 1 calc R . . C54 C 0.2266(5) 0.7957(4) 0.3672(5) 0.037(2) Uani 1 1 d G . . C55 C 0.2902(6) 0.8336(3) 0.1396(5) 0.045(3) Uani 1 1 d G . . H55A H 0.3202 0.8817 0.1442 0.054 Uiso 1 1 calc R . . C56 C 0.2821(6) 0.8594(4) 0.0515(4) 0.067(4) Uani 1 1 d G . . H56A H 0.3066 0.9251 -0.0042 0.080 Uiso 1 1 calc R . . C57 C 0.2383(7) 0.7890(5) 0.0447(4) 0.067(4) Uani 1 1 d G . . H57A H 0.2327 0.8067 -0.0156 0.080 Uiso 1 1 calc R . . C58 C 0.2025(6) 0.6929(4) 0.1260(5) 0.060(3) Uani 1 1 d G . . H58A H 0.1725 0.6448 0.1214 0.072 Uiso 1 1 calc R . . C59 C 0.2106(5) 0.6671(3) 0.2142(4) 0.048(3) Uani 1 1 d G . . H59A H 0.1862 0.6013 0.2698 0.058 Uiso 1 1 calc R . . C60 C 0.2545(5) 0.7374(4) 0.2210(4) 0.032(2) Uani 1 1 d G . . C70 C -0.007(3) 0.186(2) 0.296(3) 0.121(14) Uiso 0.53(2) 1 d PD A 1 H70A H -0.0589 0.2097 0.3351 0.145 Uiso 0.53(2) 1 calc PR A 1 H70B H 0.0187 0.2327 0.2216 0.145 Uiso 0.53(2) 1 calc PR A 1 Cl1 Cl -0.0563(14) 0.0699(9) 0.3281(10) 0.137(6) Uani 0.53(2) 1 d PDU A 1 Cl2 Cl 0.0903(13) 0.1837(11) 0.3269(14) 0.162(7) Uani 0.53(2) 1 d PDU A 1 C70' C 0.115(5) 0.211(4) 0.254(3) 0.18(3) Uiso 0.47(2) 1 d PD A 2 H70C H 0.0972 0.2735 0.2230 0.221 Uiso 0.47(2) 1 calc PR A 2 H70D H 0.1701 0.2072 0.1971 0.221 Uiso 0.47(2) 1 calc PR A 2 Cl1' Cl 0.013(2) 0.1135(16) 0.3165(15) 0.190(10) Uani 0.47(2) 1 d PDU A 2 Cl2' Cl 0.152(2) 0.2047(12) 0.3423(12) 0.172(10) Uani 0.47(2) 1 d PDU A 2 C80 C -0.039(3) 0.063(4) 0.831(5) 0.160(18) Uiso 0.370(4) 1 d PDU B 1 H80A H -0.0670 0.0052 0.9016 0.192 Uiso 0.370(4) 1 calc PR B 1 H80B H -0.0836 0.0622 0.8024 0.192 Uiso 0.370(4) 1 calc PR B 1 Cl3 Cl 0.079(2) 0.0567(17) 0.752(2) 0.167(10) Uani 0.370(4) 1 d PDU B 1 Cl4 Cl -0.0279(16) 0.1711(14) 0.8341(18) 0.164(7) Uani 0.370(4) 1 d PDU B 1 C80' C 0.085(5) 0.165(3) 0.795(3) 0.098(14) Uiso 0.33(2) 1 d PDU C 2 H80C H 0.1574 0.1886 0.7586 0.118 Uiso 0.33(2) 1 calc PR C 2 H80D H 0.0559 0.2229 0.7790 0.118 Uiso 0.33(2) 1 calc PR C 2 Cl3' Cl 0.051(3) 0.094(3) 0.752(2) 0.152(9) Uani 0.33(2) 1 d PDU C 2 Cl4' Cl 0.041(3) 0.093(3) 0.929(2) 0.197(11) Uani 0.33(2) 1 d PDU C 2 C80" C 0.058(3) 0.178(2) 0.833(3) 0.055(10) Uiso 0.30(2) 1 d PDU D 3 H80E H 0.1244 0.1883 0.8254 0.066 Uiso 0.30(2) 1 calc PR D 3 H80F H 0.0329 0.2372 0.8264 0.066 Uiso 0.30(2) 1 calc PR D 3 Cl3" Cl -0.023(4) 0.074(3) 0.955(2) 0.217(14) Uani 0.30(2) 1 d PDU . 3 Cl4" Cl 0.061(3) 0.156(3) 0.736(2) 0.214(17) Uani 0.30(2) 1 d PDU D 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 Cu1 0.0326(6) 0.0234(5) 0.0224(5) -0.0111(4) -0.0177(4) 0.0095(4) Se2 0.0288(5) 0.0172(4) 0.0222(4) -0.0066(3) -0.0123(3) 0.0060(3) Cu3 0.0356(6) 0.0207(5) 0.0195(5) -0.0086(4) -0.0149(4) 0.0092(4) P4 0.0256(12) 0.0160(10) 0.0193(10) -0.0082(8) -0.0114(9) 0.0043(8) Se5 0.0282(5) 0.0186(4) 0.0200(4) -0.0106(3) -0.0144(3) 0.0098(3) Cu6 0.0347(6) 0.0224(5) 0.0323(6) -0.0113(4) -0.0224(5) 0.0121(4) Se7 0.0352(5) 0.0202(4) 0.0229(4) -0.0102(3) -0.0186(4) 0.0084(4) P8 0.0297(12) 0.0192(10) 0.0273(11) -0.0134(9) -0.0188(9) 0.0083(9) P9 0.0337(12) 0.0160(10) 0.0181(10) -0.0044(8) -0.0139(9) 0.0078(9) P10 0.0544(16) 0.0350(13) 0.0191(11) -0.0121(10) -0.0165(11) 0.0177(12) P11 0.0381(14) 0.0252(11) 0.0318(12) -0.0096(10) -0.0229(11) 0.0119(10) C1 0.037(5) 0.027(5) 0.034(5) -0.015(4) -0.011(4) -0.002(4) C2 0.046(6) 0.055(7) 0.052(6) -0.044(6) -0.014(5) 0.018(5) C3 0.059(7) 0.024(5) 0.049(6) -0.020(5) -0.027(5) 0.006(5) C4 0.045(6) 0.031(6) 0.033(5) -0.017(4) -0.017(4) 0.004(4) C5 0.040(5) 0.027(5) 0.026(4) -0.015(4) -0.016(4) 0.004(4) C6 0.025(5) 0.021(4) 0.032(5) -0.016(4) -0.016(4) 0.008(4) C7 0.056(7) 0.022(5) 0.041(5) -0.011(4) -0.026(5) 0.010(4) C8 0.032(6) 0.053(7) 0.056(7) -0.008(5) -0.018(5) -0.010(5) C9 0.026(5) 0.059(7) 0.059(7) -0.028(6) -0.019(5) 0.004(5) C10 0.051(7) 0.040(5) 0.059(6) -0.029(5) -0.038(5) 0.019(5) C11 0.052(7) 0.035(5) 0.037(5) -0.015(4) -0.029(5) 0.012(5) C12 0.023(5) 0.026(4) 0.026(4) -0.017(4) -0.010(4) 0.006(4) C13 0.033(6) 0.048(6) 0.058(6) -0.041(5) -0.014(5) 0.008(5) C14 0.034(7) 0.066(8) 0.103(10) -0.061(8) -0.016(7) 0.011(6) C15 0.046(7) 0.040(6) 0.113(11) -0.034(7) -0.048(8) 0.021(5) C16 0.065(9) 0.065(8) 0.088(9) -0.022(7) -0.064(8) 0.015(6) C17 0.051(7) 0.060(7) 0.051(6) -0.025(5) -0.029(5) 0.008(5) C18 0.041(5) 0.019(4) 0.039(5) -0.011(4) -0.026(4) 0.013(4) C19 0.063(7) 0.027(5) 0.033(5) -0.020(4) -0.020(5) 0.009(5) C20 0.094(10) 0.034(6) 0.045(6) -0.026(5) -0.026(6) 0.015(6) C21 0.077(8) 0.033(6) 0.068(7) -0.036(6) -0.034(7) 0.012(5) C22 0.073(8) 0.022(6) 0.071(8) -0.021(5) -0.027(7) 0.006(5) C23 0.044(6) 0.024(5) 0.046(6) -0.015(4) -0.010(5) -0.001(4) C24 0.034(5) 0.020(4) 0.042(5) -0.017(4) -0.031(4) 0.010(4) C25 0.054(6) 0.023(5) 0.043(5) -0.021(4) -0.027(5) 0.020(4) C26 0.069(8) 0.030(6) 0.041(6) -0.012(4) -0.026(5) -0.003(5) C27 0.092(9) 0.020(5) 0.036(5) -0.013(4) -0.031(6) 0.013(5) C28 0.088(9) 0.031(6) 0.043(6) -0.019(5) -0.038(6) 0.028(6) C29 0.060(7) 0.031(6) 0.040(5) -0.016(4) -0.032(5) 0.020(5) C30 0.047(6) 0.015(4) 0.017(4) -0.003(3) -0.013(4) 0.005(4) C31 0.068(7) 0.024(5) 0.028(5) -0.008(4) -0.017(5) 0.016(5) C32 0.080(9) 0.037(6) 0.025(6) 0.002(5) -0.005(6) 0.016(6) C33 0.114(12) 0.063(8) 0.033(6) -0.018(6) -0.040(8) 0.045(8) C34 0.109(12) 0.091(9) 0.048(7) -0.032(7) -0.062(8) 0.047(9) C35 0.069(8) 0.050(6) 0.027(5) -0.014(5) -0.032(5) 0.022(5) C36 0.061(7) 0.030(5) 0.018(4) -0.012(4) -0.020(5) 0.024(5) C37 0.058(8) 0.047(7) 0.040(6) -0.015(5) -0.007(5) -0.006(6) C38 0.096(12) 0.049(7) 0.066(8) -0.026(7) -0.007(8) -0.013(8) C39 0.044(7) 0.071(9) 0.076(9) -0.034(7) 0.009(6) -0.005(7) C40 0.067(9) 0.082(10) 0.063(8) -0.044(7) -0.003(7) 0.024(8) C41 0.070(9) 0.057(7) 0.058(7) -0.042(6) -0.006(6) 0.020(6) C42 0.047(6) 0.029(5) 0.016(4) -0.002(4) -0.001(4) 0.007(5) C43 0.104(11) 0.110(11) 0.046(7) -0.048(8) -0.048(8) 0.050(9) C44 0.104(11) 0.159(14) 0.084(9) -0.083(10) -0.062(8) 0.050(10) C45 0.092(10) 0.151(13) 0.081(9) -0.086(10) -0.040(8) 0.020(9) C46 0.112(14) 0.099(11) 0.082(10) -0.068(10) -0.032(9) 0.018(10) C47 0.083(9) 0.058(7) 0.049(6) -0.037(6) -0.031(6) 0.025(6) C48 0.053(7) 0.074(8) 0.029(5) -0.031(5) -0.023(5) 0.024(6) C49 0.050(6) 0.033(5) 0.041(5) -0.011(5) -0.021(5) 0.013(5) C50 0.115(12) 0.042(7) 0.035(6) -0.016(5) -0.024(7) -0.002(7) C51 0.108(12) 0.060(8) 0.047(7) -0.038(6) -0.027(7) 0.047(8) C52 0.079(9) 0.063(8) 0.052(7) -0.025(6) -0.020(7) 0.040(7) C53 0.052(7) 0.051(6) 0.055(6) -0.031(5) -0.024(5) 0.027(5) C54 0.043(6) 0.029(5) 0.028(5) -0.006(4) -0.016(4) 0.012(4) C55 0.064(7) 0.031(5) 0.046(6) -0.012(5) -0.039(5) 0.011(5) C56 0.079(9) 0.054(7) 0.041(6) -0.001(5) -0.033(6) 0.014(6) C57 0.093(10) 0.061(8) 0.040(6) -0.013(6) -0.041(7) -0.003(7) C58 0.065(8) 0.060(7) 0.057(7) -0.025(6) -0.035(6) -0.006(6) C59 0.059(7) 0.038(6) 0.046(6) -0.016(5) -0.030(5) 0.001(5) C60 0.036(5) 0.029(5) 0.039(5) -0.015(4) -0.027(4) 0.016(4) Cl1 0.164(14) 0.085(7) 0.121(8) -0.045(6) -0.043(8) 0.045(7) Cl2 0.183(16) 0.126(10) 0.143(12) -0.063(9) -0.058(10) 0.053(10) Cl1' 0.22(2) 0.136(15) 0.143(12) -0.016(11) -0.091(13) 0.040(15) Cl2' 0.29(3) 0.104(9) 0.092(8) -0.040(7) -0.075(12) 0.034(13) Cl3 0.158(17) 0.126(13) 0.170(15) -0.080(12) -0.036(13) 0.048(12) Cl4 0.142(14) 0.144(13) 0.195(16) -0.070(12) -0.090(12) 0.060(11) Cl3' 0.165(18) 0.21(2) 0.164(14) -0.147(15) -0.091(13) 0.084(18) Cl4' 0.16(2) 0.22(2) 0.201(19) -0.121(16) -0.066(17) -0.004(18) Cl3" 0.20(2) 0.23(2) 0.20(2) -0.089(18) -0.105(19) 0.03(2) Cl4" 0.17(2) 0.19(2) 0.22(2) -0.07(2) -0.088(18) 0.07(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P8 2.238(2) . ? Cu1 Se2 2.4421(14) . ? Cu1 Se5 2.4565(14) 2_666 ? Cu1 Se5 2.5460(14) . ? Se2 P9 2.233(2) . ? Se2 Cu3 2.5510(14) . ? Cu3 P4 2.269(2) . ? Cu3 P10 2.283(2) . ? Cu3 Se7 2.4673(15) 2_666 ? P4 C6 1.841(4) . ? P4 C12 1.847(4) . ? P4 Se5 2.236(2) . ? Se5 Cu1 2.4565(14) 2_666 ? Se5 Cu6 2.4887(13) . ? Cu6 P11 2.225(3) . ? Cu6 P9 2.266(3) 2_666 ? Cu6 Se7 2.5072(14) . ? Se7 P8 2.255(2) . ? Se7 Cu3 2.4673(15) 2_666 ? P8 C18 1.833(5) . ? P8 C24 1.842(4) . ? P9 C36 1.841(4) . ? P9 C30 1.856(4) . ? P9 Cu6 2.266(3) 2_666 ? P10 C48 1.830(6) . ? P10 C42 1.840(6) . ? P11 C60 1.827(4) . ? P11 C54 1.833(5) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C70 Cl1 1.76(2) . ? C70 Cl2 1.77(2) . ? C70' Cl1' 1.76(2) . ? C70' Cl2' 1.76(2) . ? C80 Cl3 1.76(2) . ? C80 Cl4 1.77(2) . ? C80' Cl4' 1.77(2) . ? C80' Cl3' 1.78(2) . ? C80" Cl3" 1.78(2) . ? C80" Cl4" 1.79(2) . ? Cl3" Cl3" 2.43(9) 2_557 ? 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 P8 Cu1 Se2 128.58(8) . . ? P8 Cu1 Se5 116.99(7) . 2_666 ? Se2 Cu1 Se5 106.55(5) . 2_666 ? P8 Cu1 Se5 94.40(6) . . ? Se2 Cu1 Se5 105.67(5) . . ? Se5 Cu1 Se5 98.00(4) 2_666 . ? P9 Se2 Cu1 99.49(7) . . ? P9 Se2 Cu3 95.58(7) . . ? Cu1 Se2 Cu3 94.77(5) . . ? P4 Cu3 P10 121.50(10) . . ? P4 Cu3 Se7 119.16(7) . 2_666 ? P10 Cu3 Se7 103.60(8) . 2_666 ? P4 Cu3 Se2 99.92(7) . . ? P10 Cu3 Se2 104.48(8) . . ? Se7 Cu3 Se2 106.21(5) 2_666 . ? C6 P4 C12 99.1(3) . . ? C6 P4 Se5 105.91(17) . . ? C12 P4 Se5 105.0(2) . . ? C6 P4 Cu3 123.2(2) . . ? C12 P4 Cu3 115.01(18) . . ? Se5 P4 Cu3 107.07(9) . . ? P4 Se5 Cu1 106.40(7) . 2_666 ? P4 Se5 Cu6 137.83(7) . . ? Cu1 Se5 Cu6 102.86(5) 2_666 . ? P4 Se5 Cu1 102.42(6) . . ? Cu1 Se5 Cu1 82.00(4) 2_666 . ? Cu6 Se5 Cu1 111.24(4) . . ? P11 Cu6 P9 128.92(9) . 2_666 ? P11 Cu6 Se5 114.95(8) . . ? P9 Cu6 Se5 100.32(7) 2_666 . ? P11 Cu6 Se7 112.13(8) . . ? P9 Cu6 Se7 98.33(7) 2_666 . ? Se5 Cu6 Se7 96.60(4) . . ? P8 Se7 Cu3 103.43(7) . 2_666 ? P8 Se7 Cu6 101.27(7) . . ? Cu3 Se7 Cu6 102.13(5) 2_666 . ? C18 P8 C24 100.0(3) . . ? C18 P8 Cu1 114.1(2) . . ? C24 P8 Cu1 121.4(2) . . ? C18 P8 Se7 102.1(2) . . ? C24 P8 Se7 104.92(18) . . ? Cu1 P8 Se7 112.02(10) . . ? C36 P9 C30 100.4(3) . . ? C36 P9 Se2 104.8(2) . . ? C30 P9 Se2 105.85(19) . . ? C36 P9 Cu6 113.1(2) . 2_666 ? C30 P9 Cu6 120.2(2) . 2_666 ? Se2 P9 Cu6 110.97(9) . 2_666 ? C48 P10 C42 105.1(4) . . ? C48 P10 Cu3 119.5(3) . . ? C42 P10 Cu3 118.9(2) . . ? C60 P11 C54 103.0(3) . . ? C60 P11 Cu6 117.7(3) . . ? C54 P11 Cu6 119.0(2) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C3 C4 C5 120.0 . . ? C6 C5 C4 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 P4 121.6(3) . . ? C1 C6 P4 118.4(3) . . ? C8 C7 C12 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 P4 120.2(3) . . ? C7 C12 P4 119.7(3) . . ? C14 C13 C18 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 P8 120.4(3) . . ? C13 C18 P8 119.5(3) . . ? C20 C19 C24 120.0 . . ? C19 C20 C21 120.0 . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C22 C23 C24 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 P8 116.2(3) . . ? C19 C24 P8 123.8(3) . . ? C26 C25 C30 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 P9 116.6(3) . . ? C25 C30 P9 123.4(3) . . ? C32 C31 C36 120.0 . . ? C33 C32 C31 120.0 . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 P9 117.9(3) . . ? C31 C36 P9 122.1(3) . . ? C38 C37 C42 120.0 . . ? C37 C38 C39 120.0 . . ? C40 C39 C38 120.0 . . ? C39 C40 C41 120.0 . . ? C40 C41 C42 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 P10 122.4(4) . . ? C37 C42 P10 117.4(4) . . ? C44 C43 C48 120.0 . . ? C45 C44 C43 120.0 . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 P10 119.3(4) . . ? C43 C48 P10 120.7(4) . . ? C50 C49 C54 120.0 . . ? C49 C50 C51 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C53 120.0 . . ? C54 C53 C52 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 P11 121.8(4) . . ? C49 C54 P11 118.2(4) . . ? C56 C55 C60 120.0 . . ? C55 C56 C57 120.0 . . ? C58 C57 C56 120.0 . . ? C59 C58 C57 120.0 . . ? C58 C59 C60 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 P11 120.1(3) . . ? C55 C60 P11 119.8(3) . . ? Cl1 C70 Cl2 110.8(18) . . ? Cl1' C70' Cl2' 110.3(19) . . ? Cl3 C80 Cl4 108.9(18) . . ? Cl4' C80' Cl3' 108.7(18) . . ? Cl3" C80" Cl4" 107.2(17) . . ? C80" Cl3" Cl3" 126(4) . 2_557 ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.608 _refine_diff_density_min -0.560 _refine_diff_density_rms 0.114 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 604050' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H93 Cu6 P9 Se6' _chemical_formula_weight 2524.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.776(2) _cell_length_b 14.959(3) _cell_length_c 20.173(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.657(19) _cell_angle_gamma 90.00 _cell_volume 4990.6(19) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 80 _cell_measurement_theta_min 4.45 _cell_measurement_theta_max 19.96 _exptl_crystal_description plates _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.680 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2508 _exptl_absorpt_coefficient_mu 5.631 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3781 _exptl_absorpt_correction_T_max 0.7842 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7684 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0791 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 60.03 _reflns_number_total 7398 _reflns_number_gt 4589 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0804P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7398 _refine_ls_number_parameters 667 _refine_ls_number_restraints 664 _refine_ls_R_factor_all 0.1108 _refine_ls_R_factor_gt 0.0612 _refine_ls_wR_factor_ref 0.1679 _refine_ls_wR_factor_gt 0.1463 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 0.969 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.41165(9) 0.95378(9) -0.01389(7) 0.0657(4) Uani 1 1 d . . . Se2 Se 0.40299(6) 0.79837(6) 0.02410(5) 0.0631(3) Uani 1 1 d . . . Cu3' Cu 0.5433(3) 0.8165(2) 0.0262(3) 0.0668(11) Uani 0.50 1 d P . 1 Cu3 Cu 0.5524(3) 0.7748(3) 0.0296(2) 0.0689(11) Uani 0.50 1 d P . -2 P4 P 0.57281(15) 0.82051(14) -0.07443(11) 0.0599(6) Uani 1 1 d . . . Se5 Se 0.52812(6) 0.96162(6) -0.08611(5) 0.0622(3) Uani 1 1 d . . . Cu6 Cu 0.49624(9) 1.07756(9) -0.17575(7) 0.0665(4) Uani 1 1 d . . . Se7 Se 0.37940(6) 1.14581(6) -0.13139(5) 0.0603(3) Uani 1 1 d . . . P8 P 0.32281(14) 1.02489(15) -0.09258(11) 0.0563(5) Uani 1 1 d . . . P9 P 0.40606(15) 0.82226(15) 0.13429(12) 0.0614(6) Uani 1 1 d D . . P10 P 0.5710(4) 0.6170(4) 0.0506(3) 0.0831(17) Uani 0.50 1 d PD A -2 H10B H 0.5716 0.6111 0.1150 0.100 Uiso 0.35 1 d PR A -2 H10C H 0.5826 0.6067 0.1155 0.100 Uiso 0.15 1 d PR A -3 P11 P 0.45863(18) 1.03085(18) -0.28131(13) 0.0746(7) Uani 1 1 d D . . H11B H 0.4040 0.9711 -0.2751 0.090 Uiso 0.50 1 d PR B 1 H11C H 0.3930 0.9834 -0.2861 0.090 Uiso 0.50 1 d PR B 2 C1 C 0.7075(5) 0.7319(4) -0.1030(5) 0.097(4) Uani 1 1 d G . . H1A H 0.6800 0.6813 -0.0923 0.116 Uiso 1 1 calc R . . C2 C 0.7836(5) 0.7234(5) -0.1210(5) 0.129(6) Uani 1 1 d G . . H2A H 0.8069 0.6672 -0.1225 0.155 Uiso 1 1 calc R . . C3 C 0.8247(4) 0.7990(7) -0.1369(5) 0.116(5) Uani 1 1 d G . . H3A H 0.8756 0.7934 -0.1489 0.139 Uiso 1 1 calc R . . C4 C 0.7899(5) 0.8830(6) -0.1347(5) 0.124(5) Uani 1 1 d G . . H4A H 0.8174 0.9336 -0.1453 0.149 Uiso 1 1 calc R . . C5 C 0.7138(5) 0.8915(4) -0.1166(5) 0.100(4) Uani 1 1 d G . . H5A H 0.6905 0.9477 -0.1152 0.120 Uiso 1 1 calc R . . C6 C 0.6726(3) 0.8159(4) -0.1008(4) 0.065(2) Uani 1 1 d G . . C7 C 0.4677(5) 0.6861(5) -0.1303(3) 0.100(4) Uani 1 1 d G . . H7A H 0.4657 0.6705 -0.0859 0.120 Uiso 1 1 calc R . . C8 C 0.4240(6) 0.6371(5) -0.1827(4) 0.131(6) Uani 1 1 d G . . H8A H 0.3927 0.5888 -0.1734 0.158 Uiso 1 1 calc R . . C9 C 0.4270(5) 0.6604(5) -0.2489(3) 0.104(4) Uani 1 1 d G . . H9A H 0.3977 0.6276 -0.2840 0.125 Uiso 1 1 calc R . . C10 C 0.4737(5) 0.7326(6) -0.2628(2) 0.092(3) Uani 1 1 d G . . H10A H 0.4757 0.7482 -0.3071 0.110 Uiso 1 1 calc R . . C11 C 0.5174(5) 0.7816(4) -0.2103(3) 0.089(3) Uani 1 1 d G . . H11A H 0.5486 0.8299 -0.2196 0.107 Uiso 1 1 calc R . . C12 C 0.5144(4) 0.7583(4) -0.1441(3) 0.062(2) Uani 1 1 d G . . C13 C 0.3041(5) 0.8675(4) -0.1672(3) 0.103(4) Uani 1 1 d G . . H13A H 0.3321 0.8414 -0.1283 0.123 Uiso 1 1 calc R . . C14 C 0.2762(6) 0.8148(3) -0.2230(4) 0.123(5) Uani 1 1 d G . . H14A H 0.2857 0.7535 -0.2215 0.147 Uiso 1 1 calc R . . C15 C 0.2343(6) 0.8537(5) -0.2812(3) 0.100(4) Uani 1 1 d G . . H15A H 0.2156 0.8185 -0.3185 0.120 Uiso 1 1 calc R . . C16 C 0.2202(5) 0.9453(5) -0.2834(3) 0.098(4) Uani 1 1 d G . . H16A H 0.1921 0.9714 -0.3223 0.118 Uiso 1 1 calc R . . C17 C 0.2480(5) 0.9980(3) -0.2276(3) 0.088(3) Uani 1 1 d G . . H17A H 0.2386 1.0593 -0.2291 0.106 Uiso 1 1 calc R . . C18 C 0.2900(4) 0.9591(4) -0.1695(3) 0.062(2) Uani 1 1 d G . . C19 C 0.2106(4) 1.1538(4) -0.0632(4) 0.086(3) Uani 1 1 d G . . H19A H 0.2522 1.1952 -0.0622 0.104 Uiso 1 1 calc R . . C20 C 0.1353(5) 1.1813(4) -0.0509(5) 0.108(4) Uani 1 1 d G . . H20A H 0.1264 1.2411 -0.0417 0.130 Uiso 1 1 calc R . . C21 C 0.0732(3) 1.1195(6) -0.0524(4) 0.105(5) Uani 1 1 d G . . H21A H 0.0228 1.1378 -0.0442 0.126 Uiso 1 1 calc R . . C22 C 0.0864(4) 1.0301(6) -0.0661(5) 0.108(4) Uani 1 1 d G . . H22A H 0.0449 0.9888 -0.0671 0.130 Uiso 1 1 calc R . . C23 C 0.1617(4) 1.0027(4) -0.0784(4) 0.095(4) Uani 1 1 d G . . H23A H 0.1706 0.9429 -0.0876 0.114 Uiso 1 1 calc R . . C24 C 0.2238(3) 1.0645(4) -0.0769(3) 0.063(2) Uani 1 1 d G . . C25 C 0.2457(4) 0.8756(6) 0.0879(3) 0.085(3) Uani 1 1 d G . . H25A H 0.2620 0.8856 0.0467 0.102 Uiso 1 1 calc R . . C26 C 0.1664(4) 0.8927(6) 0.0956(4) 0.099(4) Uani 1 1 d G . . H26A H 0.1295 0.9142 0.0596 0.119 Uiso 1 1 calc R . . C27 C 0.1422(3) 0.8777(6) 0.1573(4) 0.098(4) Uani 1 1 d G . . H27A H 0.0891 0.8891 0.1625 0.118 Uiso 1 1 calc R . . C28 C 0.1973(5) 0.8455(6) 0.2112(3) 0.108(4) Uani 1 1 d G . . H28A H 0.1811 0.8355 0.2524 0.129 Uiso 1 1 calc R . . C29 C 0.2766(4) 0.8284(6) 0.2035(3) 0.097(4) Uani 1 1 d G . . H29A H 0.3135 0.8069 0.2395 0.116 Uiso 1 1 calc R . . C30 C 0.3009(3) 0.8434(5) 0.1418(3) 0.069(2) Uani 1 1 d G . . C31 C 0.3701(11) 0.6495(11) 0.1740(9) 0.094(7) Uani 0.50 1 d PGU . 1 H31A H 0.3196 0.6585 0.1478 0.113 Uiso 0.50 1 calc PR . 1 C32 C 0.3874(10) 0.5692(9) 0.2081(10) 0.108(7) Uani 0.50 1 d PGU . 1 H32A H 0.3484 0.5245 0.2048 0.129 Uiso 0.50 1 calc PR . 1 C33 C 0.4629(11) 0.5558(9) 0.2472(10) 0.091(7) Uani 0.50 1 d PGU . 1 H33A H 0.4744 0.5021 0.2701 0.109 Uiso 0.50 1 calc PR . 1 C34 C 0.5212(10) 0.6226(12) 0.2522(11) 0.084(7) Uani 0.50 1 d PGU . 1 H34A H 0.5717 0.6137 0.2784 0.101 Uiso 0.50 1 calc PR . 1 C35 C 0.5039(12) 0.7029(11) 0.2181(13) 0.067(6) Uani 0.50 1 d PGU . 1 H35A H 0.5429 0.7476 0.2214 0.081 Uiso 0.50 1 calc PR . 1 C36 C 0.4284(14) 0.7163(9) 0.1790(11) 0.067(6) Uani 0.50 1 d PGDU . 1 C31' C 0.3671(13) 0.6359(11) 0.1355(9) 0.100(7) Uani 0.50 1 d PGU . 2 H31B H 0.3263 0.6480 0.0993 0.120 Uiso 0.50 1 calc PR . 2 C32' C 0.3771(13) 0.5496(9) 0.1611(11) 0.109(7) Uani 0.50 1 d PGU . 2 H32B H 0.3432 0.5040 0.1421 0.130 Uiso 0.50 1 calc PR . 2 C33' C 0.4380(14) 0.5316(8) 0.2152(11) 0.110(8) Uani 0.50 1 d PGU . 2 H33B H 0.4447 0.4739 0.2324 0.132 Uiso 0.50 1 calc PR . 2 C34' C 0.4887(13) 0.5998(12) 0.2437(11) 0.092(7) Uani 0.50 1 d PGU . 2 H34B H 0.5295 0.5877 0.2799 0.110 Uiso 0.50 1 calc PR . 2 C35' C 0.4787(14) 0.6861(11) 0.2181(13) 0.080(7) Uani 0.50 1 d PGU . 2 H35B H 0.5126 0.7317 0.2371 0.096 Uiso 0.50 1 calc PR . 2 C36' C 0.4178(15) 0.7041(8) 0.1640(12) 0.075(7) Uani 0.50 1 d PGDU . 2 C37 C 0.4204(13) 0.5407(12) 0.0457(9) 0.108(8) Uani 0.50 1 d PG A -2 H37A H 0.4166 0.5767 0.0826 0.130 Uiso 0.50 1 calc PR A -2 C38 C 0.3566(12) 0.4848(14) 0.0195(10) 0.169(17) Uani 0.50 1 d PG A -2 H38A H 0.3102 0.4834 0.0390 0.203 Uiso 0.50 1 calc PR A -2 C39 C 0.3623(13) 0.4311(12) -0.0357(10) 0.086(7) Uani 0.50 1 d PGU A -2 H39A H 0.3196 0.3937 -0.0532 0.103 Uiso 0.50 1 calc PR A -2 C40 C 0.4318(15) 0.4332(14) -0.0648(9) 0.142(14) Uani 0.50 1 d PGU A -2 H40A H 0.4356 0.3973 -0.1017 0.170 Uiso 0.50 1 calc PR A -2 C41 C 0.4955(12) 0.4891(14) -0.0386(11) 0.109(11) Uani 0.50 1 d PGU A -2 H41A H 0.5420 0.4905 -0.0581 0.130 Uiso 0.50 1 calc PR A -2 C42 C 0.4899(11) 0.5428(11) 0.0166(10) 0.084(7) Uani 0.50 1 d PG A -2 C43 C 0.6701(12) 0.4680(16) 0.0436(16) 0.095(8) Uani 0.35 1 d PGU A -2 H43A H 0.6258 0.4346 0.0513 0.114 Uiso 0.35 1 calc PR A -2 C44 C 0.7414(15) 0.4253(12) 0.0355(15) 0.106(9) Uani 0.35 1 d PGU A -2 H44A H 0.7448 0.3632 0.0378 0.127 Uiso 0.35 1 calc PR A -2 C45 C 0.8076(11) 0.4752(17) 0.0239(14) 0.118(10) Uani 0.35 1 d PGU A -2 H45A H 0.8553 0.4466 0.0185 0.142 Uiso 0.35 1 calc PR A -2 C46 C 0.8025(12) 0.5679(17) 0.0205(13) 0.103(9) Uani 0.35 1 d PGU A -2 H46A H 0.8468 0.6013 0.0128 0.123 Uiso 0.35 1 calc PR A -2 C47 C 0.7312(15) 0.6106(12) 0.0286(14) 0.095(8) Uani 0.35 1 d PGU A -2 H47A H 0.7278 0.6726 0.0263 0.114 Uiso 0.35 1 calc PR A -2 C48 C 0.6650(12) 0.5607(16) 0.0401(16) 0.097(10) Uani 0.35 1 d PGDU A -2 C43' C 0.681(3) 0.478(4) 0.027(4) 0.106(12) Uiso 0.15 1 d PGU A -3 H43B H 0.6462 0.4362 0.0405 0.127 Uiso 0.15 1 calc PR A -3 C44' C 0.755(4) 0.451(3) 0.012(4) 0.102(13) Uiso 0.15 1 d PGU A -3 H44B H 0.7702 0.3909 0.0158 0.122 Uiso 0.15 1 calc PR A -3 C45' C 0.808(2) 0.513(5) -0.009(3) 0.120(15) Uiso 0.15 1 d PGU A -3 H45B H 0.8573 0.4950 -0.0184 0.144 Uiso 0.15 1 calc PR A -3 C46' C 0.786(3) 0.603(4) -0.014(3) 0.111(14) Uiso 0.15 1 d PGU A -3 H46B H 0.8205 0.6446 -0.0280 0.134 Uiso 0.15 1 calc PR A -3 C47' C 0.711(4) 0.630(3) 0.000(3) 0.102(14) Uiso 0.15 1 d PGU A -3 H47B H 0.6965 0.6899 -0.0034 0.123 Uiso 0.15 1 calc PR A -3 C48' C 0.659(3) 0.568(5) 0.021(4) 0.094(12) Uiso 0.15 1 d PGDU A -3 C49 C 0.6036(19) 0.961(3) -0.2996(12) 0.092(7) Uani 0.50 1 d PGU . 1 H49A H 0.6210 0.9829 -0.2565 0.110 Uiso 0.50 1 calc PR . 1 C50 C 0.6577(14) 0.917(3) -0.3337(12) 0.130(8) Uani 0.50 1 d PGU . 1 H50A H 0.7113 0.9101 -0.3134 0.156 Uiso 0.50 1 calc PR . 1 C51 C 0.6317(15) 0.884(2) -0.3982(10) 0.137(9) Uani 0.50 1 d PGU . 1 H51A H 0.6679 0.8553 -0.4210 0.165 Uiso 0.50 1 calc PR . 1 C52 C 0.5515(15) 0.895(2) -0.4285(9) 0.126(9) Uani 0.50 1 d PGU . 1 H52A H 0.5341 0.8733 -0.4717 0.151 Uiso 0.50 1 calc PR . 1 C53 C 0.4974(13) 0.939(2) -0.3945(12) 0.110(8) Uani 0.50 1 d PGU . 1 H53A H 0.4438 0.9462 -0.4148 0.132 Uiso 0.50 1 calc PR . 1 C54 C 0.5235(18) 0.972(3) -0.3300(14) 0.085(8) Uani 0.50 1 d PGDU . 1 C55 C 0.4508(9) 1.1767(11) -0.3635(9) 0.099(7) Uani 0.50 1 d PGU . 1 H55A H 0.5052 1.1804 -0.3445 0.119 Uiso 0.50 1 calc PR . 1 C56 C 0.4170(12) 1.2402(10) -0.4102(9) 0.110(7) Uani 0.50 1 d PGU . 1 H56A H 0.4487 1.2865 -0.4223 0.132 Uiso 0.50 1 calc PR . 1 C57 C 0.3357(12) 1.2347(11) -0.4387(8) 0.106(7) Uani 0.50 1 d PGU . 1 H57A H 0.3131 1.2773 -0.4699 0.127 Uiso 0.50 1 calc PR . 1 C58 C 0.2883(9) 1.1656(13) -0.4205(9) 0.119(8) Uani 0.50 1 d PGU . 1 H58A H 0.2340 1.1619 -0.4396 0.143 Uiso 0.50 1 calc PR . 1 C59 C 0.3222(9) 1.1021(11) -0.3739(9) 0.098(7) Uani 0.50 1 d PGU . 1 H59A H 0.2904 1.0559 -0.3618 0.117 Uiso 0.50 1 calc PR . 1 C60 C 0.4034(10) 1.1076(10) -0.3454(7) 0.078(6) Uani 0.50 1 d PGDU . 1 C49' C 0.6161(18) 0.969(3) -0.2844(15) 0.106(8) Uani 0.50 1 d PGU . 2 H49B H 0.6323 1.0035 -0.2463 0.127 Uiso 0.50 1 calc PR . 2 C50' C 0.6723(13) 0.916(3) -0.3096(13) 0.123(9) Uani 0.50 1 d PGU . 2 H50B H 0.7260 0.9153 -0.2884 0.148 Uiso 0.50 1 calc PR . 2 C51' C 0.6483(14) 0.864(2) -0.3665(12) 0.139(9) Uani 0.50 1 d PGU . 2 H51B H 0.6859 0.8283 -0.3833 0.166 Uiso 0.50 1 calc PR . 2 C52' C 0.5680(15) 0.8643(18) -0.3981(10) 0.120(8) Uani 0.50 1 d PGU . 2 H52B H 0.5519 0.8294 -0.4362 0.144 Uiso 0.50 1 calc PR . 2 C53' C 0.5118(12) 0.917(2) -0.3729(12) 0.097(8) Uani 0.50 1 d PGU . 2 H53B H 0.4581 0.9176 -0.3941 0.117 Uiso 0.50 1 calc PR . 2 C54' C 0.5359(17) 0.969(3) -0.3160(16) 0.081(7) Uani 0.50 1 d PGDU . 2 C55' C 0.4969(11) 1.1510(13) -0.3799(10) 0.118(8) Uani 0.50 1 d PGU . 2 H55B H 0.5453 1.1203 -0.3783 0.141 Uiso 0.50 1 calc PR . 2 C56' C 0.4788(13) 1.2227(13) -0.4237(10) 0.131(8) Uani 0.50 1 d PGU . 2 H56B H 0.5151 1.2399 -0.4514 0.157 Uiso 0.50 1 calc PR . 2 C57' C 0.4063(15) 1.2686(12) -0.4262(10) 0.122(8) Uani 0.50 1 d PGU . 2 H57B H 0.3942 1.3166 -0.4555 0.146 Uiso 0.50 1 calc PR . 2 C58' C 0.3520(12) 1.2429(13) -0.3848(11) 0.126(8) Uani 0.50 1 d PGU . 2 H58B H 0.3035 1.2736 -0.3864 0.151 Uiso 0.50 1 calc PR . 2 C59' C 0.3701(12) 1.1713(13) -0.3410(10) 0.117(7) Uani 0.50 1 d PGU . 2 H59B H 0.3337 1.1540 -0.3133 0.141 Uiso 0.50 1 calc PR . 2 C60' C 0.4425(13) 1.1253(11) -0.3385(9) 0.103(8) Uani 0.50 1 d PGDU . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0776(9) 0.0555(7) 0.0615(7) 0.0084(6) 0.0048(6) 0.0031(6) Se2 0.0727(6) 0.0518(5) 0.0673(6) 0.0013(4) 0.0187(5) -0.0050(4) Cu3' 0.080(2) 0.050(2) 0.074(2) -0.003(2) 0.0239(16) 0.000(2) Cu3 0.076(2) 0.079(3) 0.0535(18) -0.009(2) 0.0157(15) -0.006(3) P4 0.0764(15) 0.0451(11) 0.0590(12) 0.0013(9) 0.0135(11) 0.0011(10) Se5 0.0810(7) 0.0466(5) 0.0584(5) 0.0019(4) 0.0103(5) 0.0057(4) Cu6 0.0773(9) 0.0612(7) 0.0637(8) 0.0024(6) 0.0191(7) 0.0003(7) Se7 0.0687(6) 0.0526(5) 0.0605(5) 0.0053(4) 0.0135(4) 0.0044(4) P8 0.0615(13) 0.0526(12) 0.0541(11) 0.0026(9) 0.0075(10) 0.0019(10) P9 0.0701(15) 0.0520(12) 0.0657(13) 0.0112(10) 0.0220(11) -0.0005(10) P10 0.115(5) 0.069(4) 0.068(3) 0.001(3) 0.022(3) 0.011(3) P11 0.098(2) 0.0677(15) 0.0620(13) 0.0041(12) 0.0243(13) 0.0084(14) C1 0.095(9) 0.087(8) 0.118(10) -0.023(7) 0.044(7) -0.005(7) C2 0.111(11) 0.109(11) 0.183(16) -0.022(11) 0.073(11) 0.026(9) C3 0.095(9) 0.160(15) 0.102(9) -0.038(10) 0.043(8) -0.011(10) C4 0.108(11) 0.115(12) 0.165(15) 0.006(10) 0.067(11) -0.011(9) C5 0.102(9) 0.100(9) 0.107(9) -0.008(7) 0.045(7) -0.016(7) C6 0.067(6) 0.062(5) 0.067(5) -0.008(4) 0.021(5) 0.005(5) C7 0.135(11) 0.082(8) 0.083(7) -0.001(6) 0.017(7) -0.028(8) C8 0.194(17) 0.100(10) 0.096(9) -0.014(8) 0.013(10) -0.073(11) C9 0.119(10) 0.101(9) 0.089(8) -0.043(7) 0.007(7) -0.018(8) C10 0.116(9) 0.096(8) 0.063(6) -0.017(6) 0.014(6) -0.004(7) C11 0.114(9) 0.085(8) 0.069(6) -0.002(6) 0.013(6) -0.023(7) C12 0.069(6) 0.046(4) 0.067(5) -0.013(4) 0.005(4) -0.008(4) C13 0.153(12) 0.046(5) 0.092(8) -0.004(5) -0.027(8) 0.020(7) C14 0.142(13) 0.087(9) 0.125(12) -0.027(8) -0.015(10) 0.006(9) C15 0.095(9) 0.103(9) 0.096(8) -0.032(8) -0.002(7) -0.003(7) C16 0.115(10) 0.099(9) 0.071(7) -0.013(6) -0.012(7) 0.009(7) C17 0.110(9) 0.069(6) 0.083(7) -0.001(6) 0.012(7) 0.020(6) C18 0.065(6) 0.069(5) 0.052(5) -0.002(4) 0.012(4) -0.001(5) C19 0.070(7) 0.072(7) 0.117(9) -0.021(6) 0.013(6) 0.007(5) C20 0.074(8) 0.110(10) 0.143(12) -0.046(9) 0.024(8) 0.004(7) C21 0.055(7) 0.175(15) 0.088(8) -0.019(9) 0.024(6) 0.020(8) C22 0.085(9) 0.124(11) 0.122(10) 0.019(9) 0.036(8) 0.001(8) C23 0.071(7) 0.097(8) 0.125(10) 0.018(7) 0.042(7) 0.003(6) C24 0.062(5) 0.077(6) 0.052(5) 0.002(4) 0.022(4) 0.001(5) C25 0.069(7) 0.108(9) 0.079(7) 0.002(6) 0.016(6) 0.008(6) C26 0.085(8) 0.127(11) 0.085(8) 0.010(7) 0.011(6) 0.013(8) C27 0.075(8) 0.103(9) 0.114(10) -0.006(8) 0.005(7) -0.011(7) C28 0.123(11) 0.121(11) 0.093(8) -0.006(8) 0.058(8) 0.013(9) C29 0.090(8) 0.122(10) 0.092(8) 0.018(7) 0.052(7) 0.027(7) C30 0.063(6) 0.070(6) 0.081(6) 0.007(5) 0.028(5) -0.008(5) C31 0.118(13) 0.064(11) 0.101(15) 0.036(12) 0.018(14) -0.009(11) C32 0.121(16) 0.059(12) 0.146(18) 0.017(13) 0.026(16) -0.014(12) C33 0.107(16) 0.050(12) 0.117(16) 0.023(12) 0.019(13) -0.014(12) C34 0.082(16) 0.076(13) 0.091(13) 0.025(11) 0.010(12) -0.003(12) C35 0.075(14) 0.055(10) 0.080(11) 0.021(9) 0.037(10) -0.007(9) C36 0.084(14) 0.055(11) 0.068(11) 0.027(10) 0.027(11) -0.003(10) C31' 0.129(16) 0.063(12) 0.106(17) 0.006(13) 0.016(16) -0.012(12) C32' 0.137(16) 0.048(10) 0.139(18) 0.001(12) 0.020(16) -0.006(12) C33' 0.117(18) 0.057(13) 0.159(19) 0.024(14) 0.035(16) 0.005(12) C34' 0.091(17) 0.068(14) 0.116(14) 0.032(13) 0.018(13) -0.001(13) C35' 0.084(16) 0.060(11) 0.100(13) 0.027(11) 0.026(13) 0.003(11) C36' 0.078(13) 0.055(11) 0.098(14) 0.014(11) 0.033(12) 0.000(11) C37 0.11(2) 0.095(18) 0.12(2) -0.018(16) 0.020(17) -0.001(16) C38 0.25(5) 0.09(2) 0.15(3) 0.01(2) -0.01(3) -0.02(3) C39 0.109(15) 0.074(12) 0.073(12) -0.002(10) 0.013(12) -0.013(11) C40 0.14(2) 0.119(19) 0.16(2) 0.010(16) 0.014(16) -0.009(16) C41 0.117(17) 0.096(18) 0.114(17) -0.022(15) 0.022(14) -0.009(14) C42 0.12(2) 0.043(11) 0.092(17) -0.005(12) 0.030(15) 0.011(12) C43 0.111(15) 0.074(13) 0.097(16) -0.025(13) 0.008(13) 0.021(13) C44 0.110(17) 0.088(16) 0.116(18) -0.026(15) 0.011(15) 0.034(15) C45 0.117(18) 0.116(18) 0.121(18) 0.000(17) 0.016(16) 0.014(16) C46 0.104(17) 0.088(16) 0.111(17) 0.011(15) 0.005(15) 0.007(15) C47 0.089(15) 0.095(15) 0.098(15) 0.008(14) 0.004(14) -0.002(13) C48 0.098(10) 0.096(10) 0.097(10) 0.001(5) 0.016(5) 0.000(5) C49 0.110(15) 0.103(13) 0.067(13) -0.033(11) 0.027(13) 0.008(13) C50 0.117(15) 0.158(16) 0.117(18) -0.036(16) 0.022(15) 0.044(15) C51 0.143(18) 0.159(19) 0.111(18) -0.031(17) 0.022(18) 0.068(16) C52 0.147(17) 0.145(19) 0.087(17) -0.026(15) 0.022(15) 0.063(15) C53 0.136(16) 0.117(17) 0.075(16) -0.019(14) 0.012(14) 0.023(14) C54 0.104(14) 0.080(12) 0.071(16) 0.000(12) 0.017(13) 0.019(12) C55 0.142(16) 0.080(12) 0.073(11) 0.036(10) 0.012(12) 0.011(12) C56 0.146(17) 0.097(14) 0.086(13) 0.039(12) 0.016(13) 0.041(14) C57 0.146(17) 0.101(14) 0.070(11) 0.016(12) 0.017(13) 0.061(14) C58 0.124(18) 0.117(17) 0.107(15) 0.026(14) -0.008(14) 0.038(15) C59 0.080(13) 0.123(16) 0.089(13) 0.026(13) 0.012(11) 0.016(13) C60 0.095(15) 0.086(12) 0.053(10) 0.001(10) 0.008(10) 0.026(12) C49' 0.114(15) 0.112(15) 0.096(16) -0.018(14) 0.033(14) 0.027(14) C50' 0.131(14) 0.135(14) 0.104(14) -0.019(13) 0.024(12) 0.022(12) C51' 0.152(18) 0.155(19) 0.110(19) -0.032(17) 0.027(17) 0.037(17) C52' 0.153(17) 0.126(17) 0.083(15) -0.033(14) 0.023(15) 0.043(15) C53' 0.109(14) 0.105(16) 0.079(16) -0.016(14) 0.017(13) 0.022(12) C54' 0.103(15) 0.078(12) 0.063(13) -0.027(12) 0.022(13) 0.005(12) C55' 0.17(2) 0.109(17) 0.080(13) 0.020(13) 0.035(15) -0.014(16) C56' 0.18(2) 0.108(15) 0.106(15) 0.036(13) 0.023(16) 0.020(16) C57' 0.172(19) 0.091(15) 0.106(15) 0.036(13) 0.033(16) 0.044(15) C58' 0.162(17) 0.100(14) 0.119(15) 0.022(13) 0.035(14) 0.042(14) C59' 0.141(16) 0.104(14) 0.109(14) 0.038(12) 0.026(13) 0.029(13) C60' 0.142(19) 0.092(15) 0.076(13) 0.007(12) 0.023(13) 0.021(15) _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 Cu1 P8 2.254(3) . ? Cu1 Se5 2.4511(17) 3_675 ? Cu1 Se2 2.4598(16) . ? Cu1 Se5 2.6285(19) . ? Cu1 Cu3' 3.026(5) . ? Se2 P9 2.243(3) . ? Se2 Cu3' 2.364(6) . ? Se2 Cu3 2.515(5) . ? Cu3' P4 2.169(6) . ? Cu3' Se7 2.362(6) 3_675 ? Cu3 P4 2.287(5) . ? Cu3 P10 2.409(8) . ? Cu3 Se7 2.479(5) 3_675 ? P4 C12 1.827(5) . ? P4 C6 1.841(6) . ? P4 Se5 2.239(2) . ? Se5 Cu1 2.4511(17) 3_675 ? Se5 Cu6 2.4979(17) . ? Cu6 P11 2.229(3) . ? Cu6 P9 2.274(3) 3_675 ? Cu6 Se7 2.5048(17) . ? Se7 P8 2.244(2) . ? Se7 Cu3' 2.362(6) 3_675 ? Se7 Cu3 2.479(5) 3_675 ? P8 C24 1.839(5) . ? P8 C18 1.842(5) . ? P9 C30 1.824(5) . ? P9 C36 1.830(10) . ? P9 C36' 1.866(10) . ? P9 Cu6 2.274(3) 3_675 ? P10 C42 1.800(17) . ? P10 C48 1.831(12) . ? P10 C48' 1.839(15) . ? P11 C54 1.813(11) . ? P11 C60' 1.816(10) . ? P11 C54' 1.823(12) . ? P11 C60 1.856(9) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C7 C8 1.3900 . ? C7 C12 1.3900 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C14 C15 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C19 C20 1.3900 . ? C19 C24 1.3900 . ? C20 C21 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C27 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 C33 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C31' C32' 1.3900 . ? C31' C36' 1.3900 . ? C32' C33' 1.3900 . ? C33' C34' 1.3900 . ? C34' C35' 1.3900 . ? C35' C36' 1.3900 . ? C37 C38 1.3900 . ? C37 C42 1.3900 . ? C38 C39 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C43 C44 1.3900 . ? C43 C48 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C43' C44' 1.3900 . ? C43' C48' 1.3900 . ? C44' C45' 1.3900 . ? C45' C46' 1.3900 . ? C46' C47' 1.3900 . ? C47' C48' 1.3900 . ? C49 C50 1.3900 . ? C49 C54 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? C53 C54 1.3900 . ? C55 C56 1.3900 . ? C55 C60 1.3900 . ? C56 C57 1.3900 . ? C57 C58 1.3900 . ? C58 C59 1.3900 . ? C59 C60 1.3900 . ? C49' C50' 1.3900 . ? C49' C54' 1.3900 . ? C50' C51' 1.3900 . ? C51' C52' 1.3900 . ? C52' C53' 1.3900 . ? C53' C54' 1.3900 . ? C55' C56' 1.3900 . ? C55' C60' 1.3900 . ? C56' C57' 1.3900 . ? C57' C58' 1.3900 . ? C58' C59' 1.3900 . ? C59' C60' 1.3900 . ? 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 P8 Cu1 Se5 117.95(8) . 3_675 ? P8 Cu1 Se2 126.79(9) . . ? Se5 Cu1 Se2 105.62(6) 3_675 . ? P8 Cu1 Se5 93.08(8) . . ? Se5 Cu1 Se5 101.01(6) 3_675 . ? Se2 Cu1 Se5 107.65(6) . . ? P8 Cu1 Cu3' 151.12(13) . . ? Se5 Cu1 Cu3' 87.07(11) 3_675 . ? Se2 Cu1 Cu3' 49.75(10) . . ? Se5 Cu1 Cu3' 66.48(11) . . ? P9 Se2 Cu3' 96.14(15) . . ? P9 Se2 Cu1 99.52(7) . . ? Cu3' Se2 Cu1 77.67(10) . . ? P9 Se2 Cu3 96.97(13) . . ? Cu3' Se2 Cu3 14.70(10) . . ? Cu1 Se2 Cu3 92.04(12) . . ? P4 Cu3' Se7 131.1(3) . 3_675 ? P4 Cu3' Se2 111.7(2) . . ? Se7 Cu3' Se2 116.0(2) 3_675 . ? P4 Cu3' Cu1 90.11(17) . . ? Se7 Cu3' Cu1 110.11(15) 3_675 . ? Se2 Cu3' Cu1 52.58(10) . . ? P4 Cu3 P10 114.8(2) . . ? P4 Cu3 Se7 119.8(2) . 3_675 ? P10 Cu3 Se7 107.2(2) . 3_675 ? P4 Cu3 Se2 102.7(2) . . ? P10 Cu3 Se2 104.1(3) . . ? Se7 Cu3 Se2 106.72(17) 3_675 . ? C12 P4 C6 98.9(3) . . ? C12 P4 Cu3' 121.9(3) . . ? C6 P4 Cu3' 129.1(3) . . ? C12 P4 Se5 105.8(2) . . ? C6 P4 Se5 108.1(2) . . ? Cu3' P4 Se5 90.00(13) . . ? C12 P4 Cu3 114.2(3) . . ? C6 P4 Cu3 122.5(3) . . ? Cu3' P4 Cu3 16.29(10) . . ? Se5 P4 Cu3 106.21(15) . . ? P4 Se5 Cu1 108.40(8) . 3_675 ? P4 Se5 Cu6 139.28(8) . . ? Cu1 Se5 Cu6 104.24(6) 3_675 . ? P4 Se5 Cu1 99.58(8) . . ? Cu1 Se5 Cu1 78.99(6) 3_675 . ? Cu6 Se5 Cu1 110.09(6) . . ? P11 Cu6 P9 128.97(11) . 3_675 ? P11 Cu6 Se5 117.77(9) . . ? P9 Cu6 Se5 97.91(8) 3_675 . ? P11 Cu6 Se7 110.85(10) . . ? P9 Cu6 Se7 99.14(8) 3_675 . ? Se5 Cu6 Se7 96.30(6) . . ? P8 Se7 Cu3' 94.56(13) . 3_675 ? P8 Se7 Cu3 105.11(13) . 3_675 ? Cu3' Se7 Cu3 14.99(10) 3_675 3_675 ? P8 Se7 Cu6 101.44(8) . . ? Cu3' Se7 Cu6 94.25(13) 3_675 . ? Cu3 Se7 Cu6 102.17(13) 3_675 . ? C24 P8 C18 99.5(3) . . ? C24 P8 Se7 104.3(2) . . ? C18 P8 Se7 102.8(2) . . ? C24 P8 Cu1 122.7(2) . . ? C18 P8 Cu1 114.2(2) . . ? Se7 P8 Cu1 110.96(11) . . ? C30 P9 C36 103.3(8) . . ? C30 P9 C36' 100.9(9) . . ? C36 P9 C36' 11.5(13) . . ? C30 P9 Se2 104.4(2) . . ? C36 P9 Se2 108.6(8) . . ? C36' P9 Se2 98.7(8) . . ? C30 P9 Cu6 120.2(3) . 3_675 ? C36 P9 Cu6 108.3(7) . 3_675 ? C36' P9 Cu6 118.4(8) . 3_675 ? Se2 P9 Cu6 111.39(10) . 3_675 ? C42 P10 C48 106.4(11) . . ? C42 P10 C48' 103(3) . . ? C48 P10 C48' 12(3) . . ? C42 P10 Cu3 118.0(7) . . ? C48 P10 Cu3 121.3(10) . . ? C48' P10 Cu3 115(3) . . ? C54 P11 C60' 94.2(14) . . ? C54 P11 C54' 10.2(18) . . ? C60' P11 C54' 100.9(15) . . ? C54 P11 C60 101.5(12) . . ? C60' P11 C60 21.9(8) . . ? C54' P11 C60 110.4(13) . . ? C54 P11 Cu6 124.8(10) . . ? C60' P11 Cu6 110.6(7) . . ? C54' P11 Cu6 114.8(10) . . ? C60 P11 Cu6 120.0(6) . . ? C2 C1 C6 120.0 . . ? C3 C2 C1 120.0 . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 P4 123.2(4) . . ? C1 C6 P4 116.8(4) . . ? C8 C7 C12 120.0 . . ? C9 C8 C7 120.0 . . ? C8 C9 C10 120.0 . . ? C11 C10 C9 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 P4 120.7(4) . . ? C7 C12 P4 119.3(4) . . ? C14 C13 C18 120.0 . . ? C13 C14 C15 120.0 . . ? C16 C15 C14 120.0 . . ? C15 C16 C17 120.0 . . ? C16 C17 C18 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 P8 121.6(4) . . ? C13 C18 P8 118.3(4) . . ? C20 C19 C24 120.0 . . ? C19 C20 C21 120.0 . . ? C20 C21 C22 120.0 . . ? C23 C22 C21 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C19 120.0 . . ? C23 C24 P8 118.5(4) . . ? C19 C24 P8 121.5(4) . . ? C26 C25 C30 120.0 . . ? C25 C26 C27 120.0 . . ? C26 C27 C28 120.0 . . ? C29 C28 C27 120.0 . . ? C28 C29 C30 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 P9 118.6(4) . . ? C25 C30 P9 121.4(4) . . ? C32 C31 C36 120.0 . . ? C31 C32 C33 120.0 . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 P9 119.8(12) . . ? C31 C36 P9 120.2(12) . . ? C32' C31' C36' 120.0 . . ? C31' C32' C33' 120.0 . . ? C34' C33' C32' 120.0 . . ? C33' C34' C35' 120.0 . . ? C36' C35' C34' 120.0 . . ? C35' C36' C31' 120.0 . . ? C35' C36' P9 117.4(12) . . ? C31' C36' P9 122.6(12) . . ? C38 C37 C42 120.0 . . ? C39 C38 C37 120.0 . . ? C38 C39 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C37 120.0 . . ? C41 C42 P10 120.9(12) . . ? C37 C42 P10 119.1(12) . . ? C44 C43 C48 120.0 . . ? C45 C44 C43 120.0 . . ? C44 C45 C46 120.0 . . ? C45 C46 C47 120.0 . . ? C48 C47 C46 120.0 . . ? C47 C48 C43 120.0 . . ? C47 C48 P10 120.0(15) . . ? C43 C48 P10 120.0(15) . . ? C44' C43' C48' 120.0 . . ? C45' C44' C43' 120.0 . . ? C44' C45' C46' 120.0 . . ? C47' C46' C45' 120.0 . . ? C46' C47' C48' 120.0 . . ? C47' C48' C43' 120.0 . . ? C47' C48' P10 114(4) . . ? C43' C48' P10 125(4) . . ? C50 C49 C54 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C52 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C54 120.0 . . ? C53 C54 C49 120.0 . . ? C53 C54 P11 123.8(17) . . ? C49 C54 P11 116.2(17) . . ? C56 C55 C60 120.0 . . ? C57 C56 C55 120.0 . . ? C58 C57 C56 120.0 . . ? C57 C58 C59 120.0 . . ? C60 C59 C58 120.0 . . ? C59 C60 C55 120.0 . . ? C59 C60 P11 126.3(9) . . ? C55 C60 P11 113.7(9) . . ? C50' C49' C54' 120.0 . . ? C49' C50' C51' 120.0 . . ? C52' C51' C50' 120.0 . . ? C51' C52' C53' 120.0 . . ? C54' C53' C52' 120.0 . . ? C53' C54' C49' 120.0 . . ? C53' C54' P11 118.3(17) . . ? C49' C54' P11 121.6(17) . . ? C56' C55' C60' 120.0 . . ? C55' C56' C57' 120.0 . . ? C58' C57' C56' 120.0 . . ? C57' C58' C59' 120.0 . . ? C60' C59' C58' 120.0 . . ? C59' C60' C55' 120.0 . . ? C59' C60' P11 116.3(11) . . ? C55' C60' P11 123.7(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 60.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.547 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.095 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 604051' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H86 Cu6 P8 Se8' _chemical_formula_weight 2524.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.1362(12) _cell_length_b 22.2016(14) _cell_length_c 17.6252(14) _cell_angle_alpha 90.00 _cell_angle_beta 106.850(7) _cell_angle_gamma 90.00 _cell_volume 4919.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 11.09 _cell_measurement_theta_max 24.89 _exptl_crystal_description blocks _exptl_crystal_colour Orange/yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2480 _exptl_absorpt_coefficient_mu 6.372 _exptl_absorpt_correction_type Shelxa _exptl_absorpt_correction_T_min 0.2366 _exptl_absorpt_correction_T_max 0.6975 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/RA' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7626 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.29 _diffrn_reflns_theta_max 60.00 _reflns_number_total 7269 _reflns_number_gt 5605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0599P)^2^+15.9858P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7269 _refine_ls_number_parameters 445 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.1457 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.35324(10) 0.51073(5) 0.99901(7) 0.0553(3) Uani 1 1 d . . . Se2 Se 0.31104(8) 0.50197(4) 1.11914(6) 0.0581(2) Uani 1 1 d . . . Cu3 Cu 0.50532(10) 0.51254(5) 1.14824(7) 0.0522(3) Uani 1 1 d . . . P4 P 0.5721(2) 0.57403(11) 1.25353(13) 0.0630(6) Uani 1 1 d . . . Se5 Se 0.57015(7) 0.57383(4) 1.04965(5) 0.0472(2) Uani 1 1 d . . . Cu6 Cu 0.55937(10) 0.63548(5) 0.92723(7) 0.0512(3) Uani 1 1 d . . . Se7 Se 0.40979(7) 0.58825(4) 0.83023(5) 0.0493(2) Uani 1 1 d . . . P8 P 0.29865(16) 0.57863(9) 0.90406(12) 0.0476(5) Uani 1 1 d . . . P9 P 0.31045(19) 0.40170(10) 1.12092(14) 0.0568(5) Uani 1 1 d . . . Se10 Se 0.64509(12) 0.65382(5) 1.21194(7) 0.0856(4) Uani 1 1 d . . . P11 P 0.5478(2) 0.73160(10) 0.96127(15) 0.0615(6) Uani 1 1 d . . . H11 H 0.4700 0.7336 0.9930 0.074 Uiso 1 1 calc R . . C1 C 0.6896(8) 0.6088(4) 1.1292(6) 0.070(3) Uani 1 1 d . . . H1A H 0.7276 0.6362 1.1033 0.084 Uiso 1 1 calc R . . H1B H 0.7388 0.5766 1.1545 0.084 Uiso 1 1 calc R . . C2 C 0.4770(6) 0.6118(4) 1.2958(4) 0.072(3) Uani 1 1 d G . . C3 C 0.3871(8) 0.6369(5) 1.2431(4) 0.125(5) Uani 1 1 d GU . . H3A H 0.3792 0.6363 1.1884 0.150 Uiso 1 1 calc R . . C4 C 0.3088(7) 0.6627(5) 1.2714(7) 0.169(8) Uani 1 1 d GU . . H4A H 0.2479 0.6797 1.2357 0.203 Uiso 1 1 calc R . . C5 C 0.3204(8) 0.6635(6) 1.3523(7) 0.157(8) Uani 1 1 d G . . H5A H 0.2675 0.6810 1.3714 0.189 Uiso 1 1 calc R . . C6 C 0.4104(10) 0.6384(6) 1.4050(5) 0.154(8) Uani 1 1 d G . . H6A H 0.4182 0.6390 1.4597 0.184 Uiso 1 1 calc R . . C7 C 0.4887(7) 0.6126(5) 1.3768(4) 0.118(5) Uani 1 1 d G . . H7A H 0.5495 0.5956 1.4124 0.141 Uiso 1 1 calc R . . C8 C 0.6712(6) 0.5448(3) 1.3405(4) 0.074(3) Uani 1 1 d G . . C9 C 0.6460(7) 0.4910(3) 1.3713(4) 0.104(4) Uani 1 1 d G . . H9A H 0.5819 0.4712 1.3460 0.125 Uiso 1 1 calc R . . C10 C 0.7156(9) 0.4665(3) 1.4392(5) 0.126(5) Uani 1 1 d GU . . H10A H 0.6985 0.4302 1.4600 0.151 Uiso 1 1 calc R . . C11 C 0.8104(8) 0.4958(5) 1.4765(5) 0.137(6) Uani 1 1 d GU . . H11A H 0.8575 0.4793 1.5225 0.164 Uiso 1 1 calc R . . C12 C 0.8357(6) 0.5496(5) 1.4458(6) 0.146(7) Uani 1 1 d G . . H12A H 0.8998 0.5694 1.4710 0.175 Uiso 1 1 calc R . . C13 C 0.7661(7) 0.5741(3) 1.3778(5) 0.104(4) Uani 1 1 d G . . H13A H 0.7831 0.6104 1.3571 0.124 Uiso 1 1 calc R . . C14 C 0.2782(5) 0.65524(18) 0.9346(3) 0.0531(19) Uani 1 1 d G . . C15 C 0.3100(5) 0.6680(2) 1.0153(3) 0.062(2) Uani 1 1 d G . . H15A H 0.3387 0.6373 1.0521 0.074 Uiso 1 1 calc R . . C16 C 0.2995(5) 0.7260(3) 1.0416(3) 0.072(3) Uani 1 1 d G . . H16A H 0.3211 0.7346 1.0962 0.086 Uiso 1 1 calc R . . C17 C 0.2572(6) 0.7714(2) 0.9872(4) 0.076(3) Uani 1 1 d G . . H17A H 0.2501 0.8106 1.0050 0.091 Uiso 1 1 calc R . . C18 C 0.2253(6) 0.7586(2) 0.9065(4) 0.083(3) Uani 1 1 d G . . H18A H 0.1967 0.7893 0.8697 0.100 Uiso 1 1 calc R . . C19 C 0.2359(5) 0.7006(3) 0.8802(3) 0.071(3) Uani 1 1 d G . . H19A H 0.2143 0.6920 0.8257 0.086 Uiso 1 1 calc R . . C20 C 0.1696(4) 0.5601(3) 0.8348(4) 0.061(2) Uani 1 1 d G . . C21 C 0.1534(5) 0.5559(3) 0.7535(4) 0.082(3) Uani 1 1 d G . . H21A H 0.2110 0.5606 0.7324 0.098 Uiso 1 1 calc R . . C22 C 0.0521(7) 0.5448(4) 0.7034(4) 0.114(5) Uani 1 1 d G . . H22A H 0.0411 0.5419 0.6484 0.136 Uiso 1 1 calc R . . C23 C -0.0330(4) 0.5379(4) 0.7345(6) 0.118(5) Uani 1 1 d GU . . H23A H -0.1016 0.5303 0.7006 0.142 Uiso 1 1 calc R . . C24 C -0.0168(5) 0.5421(4) 0.8159(6) 0.122(5) Uani 1 1 d GU . . H24A H -0.0744 0.5374 0.8369 0.146 Uiso 1 1 calc R . . C25 C 0.0845(6) 0.5532(4) 0.8660(4) 0.102(5) Uani 1 1 d G . . H25A H 0.0954 0.5560 0.9210 0.123 Uiso 1 1 calc R . . C26 C 0.1713(4) 0.3810(3) 1.0714(4) 0.070(3) Uani 1 1 d G . . C27 C 0.1223(6) 0.4084(4) 0.9990(5) 0.110(5) Uani 1 1 d G . . H27A H 0.1578 0.4389 0.9798 0.132 Uiso 1 1 calc R . . C28 C 0.0208(7) 0.3906(5) 0.9552(4) 0.134(6) Uani 1 1 d G . . H28A H -0.0123 0.4091 0.9063 0.160 Uiso 1 1 calc R . . C29 C -0.0317(5) 0.3455(5) 0.9837(6) 0.118(5) Uani 1 1 d GU . . H29A H -0.1003 0.3335 0.9541 0.141 Uiso 1 1 calc R . . C30 C 0.0173(6) 0.3181(4) 1.0560(7) 0.118(5) Uani 1 1 d GU . . H30A H -0.0182 0.2876 1.0753 0.142 Uiso 1 1 calc R . . C31 C 0.1188(6) 0.3359(3) 1.0998(5) 0.098(4) Uani 1 1 d G . . H31A H 0.1519 0.3174 1.1487 0.118 Uiso 1 1 calc R . . C32 C 0.3310(6) 0.3812(3) 1.2257(3) 0.075(3) Uani 1 1 d G . . C33 C 0.3523(7) 0.3210(3) 1.2459(5) 0.100(4) Uani 1 1 d G . . H33A H 0.3527 0.2926 1.2065 0.120 Uiso 1 1 calc R . . C34 C 0.3730(8) 0.3030(4) 1.3244(6) 0.130(6) Uani 1 1 d G . . H34A H 0.3874 0.2623 1.3382 0.156 Uiso 1 1 calc R . . C35 C 0.3724(8) 0.3451(6) 1.3827(4) 0.139(6) Uani 1 1 d GU . . H35A H 0.3864 0.3328 1.4358 0.166 Uiso 1 1 calc R . . C36 C 0.3511(8) 0.4052(5) 1.3624(4) 0.130(6) Uani 1 1 d G . . H36A H 0.3507 0.4337 1.4018 0.156 Uiso 1 1 calc R . . C37 C 0.3304(7) 0.4233(3) 1.2839(5) 0.104(4) Uani 1 1 d G . . H37A H 0.3160 0.4640 1.2702 0.125 Uiso 1 1 calc R . . C38 C 0.6631(4) 0.7613(3) 1.0357(3) 0.064(2) Uani 1 1 d G . . C39 C 0.6556(5) 0.7940(3) 1.1011(4) 0.085(3) Uani 1 1 d G . . H39A H 0.5893 0.7987 1.1107 0.102 Uiso 1 1 calc R . . C40 C 0.7461(7) 0.8197(3) 1.1523(3) 0.090(4) Uani 1 1 d G . . H40A H 0.7411 0.8418 1.1966 0.107 Uiso 1 1 calc R . . C41 C 0.8442(5) 0.8127(3) 1.1381(4) 0.089(3) Uani 1 1 d G . . H41A H 0.9054 0.8300 1.1728 0.107 Uiso 1 1 calc R . . C42 C 0.8517(4) 0.7800(3) 1.0727(4) 0.082(3) Uani 1 1 d G . . H42A H 0.9179 0.7753 1.0631 0.098 Uiso 1 1 calc R . . C43 C 0.7611(5) 0.7543(3) 1.0215(3) 0.072(3) Uani 1 1 d G . . H43A H 0.7662 0.7322 0.9772 0.086 Uiso 1 1 calc R . . C44 C 0.5193(6) 0.7897(3) 0.8856(4) 0.065(2) Uani 1 1 d G . . C45 C 0.5569(7) 0.8482(3) 0.9027(4) 0.110(5) Uani 1 1 d G . . H45A H 0.5962 0.8585 0.9546 0.132 Uiso 1 1 calc R . . C46 C 0.5363(8) 0.8913(2) 0.8430(5) 0.132(6) Uani 1 1 d GU . . H46A H 0.5617 0.9308 0.8545 0.158 Uiso 1 1 calc R . . C47 C 0.4781(7) 0.8760(3) 0.7662(4) 0.096(4) Uani 1 1 d G . . H47A H 0.4642 0.9052 0.7258 0.115 Uiso 1 1 calc R . . C48 C 0.4406(7) 0.8176(3) 0.7491(3) 0.101(4) Uani 1 1 d G . . H48A H 0.4012 0.8072 0.6971 0.122 Uiso 1 1 calc R . . C49 C 0.4611(6) 0.7744(2) 0.8088(4) 0.089(4) Uani 1 1 d G . . H49A H 0.4357 0.7349 0.7972 0.107 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0525(7) 0.0557(7) 0.0579(7) 0.0052(5) 0.0162(6) -0.0003(6) Se2 0.0514(5) 0.0608(5) 0.0683(6) -0.0039(4) 0.0271(4) 0.0019(4) Cu3 0.0537(7) 0.0515(6) 0.0509(6) -0.0064(5) 0.0144(5) -0.0013(5) P4 0.0846(17) 0.0566(12) 0.0475(11) -0.0054(10) 0.0185(11) -0.0042(12) Se5 0.0476(5) 0.0494(4) 0.0435(4) -0.0015(3) 0.0112(3) -0.0073(4) Cu6 0.0490(7) 0.0487(6) 0.0569(7) 0.0001(5) 0.0168(5) -0.0046(5) Se7 0.0485(5) 0.0517(4) 0.0447(4) 0.0013(3) 0.0085(4) 0.0023(4) P8 0.0394(11) 0.0466(10) 0.0532(11) -0.0007(9) 0.0078(9) 0.0015(8) P9 0.0535(13) 0.0613(12) 0.0636(13) 0.0009(10) 0.0294(11) -0.0084(10) Se10 0.1323(11) 0.0649(6) 0.0624(6) -0.0148(5) 0.0325(7) -0.0286(7) P11 0.0624(15) 0.0510(12) 0.0748(15) -0.0022(10) 0.0260(12) -0.0046(10) C1 0.063(6) 0.059(5) 0.093(7) 0.002(5) 0.033(5) -0.011(5) C2 0.096(8) 0.063(6) 0.061(6) -0.008(4) 0.026(5) 0.007(5) C3 0.144(12) 0.129(10) 0.095(9) -0.019(8) 0.025(8) 0.067(9) C4 0.177(15) 0.179(14) 0.142(13) -0.037(11) 0.032(11) 0.084(12) C5 0.155(17) 0.176(18) 0.162(18) -0.058(15) 0.079(15) 0.043(14) C6 0.167(18) 0.21(2) 0.120(13) -0.026(13) 0.093(14) 0.026(16) C7 0.124(12) 0.156(14) 0.086(8) -0.026(9) 0.051(8) 0.024(10) C8 0.091(8) 0.063(6) 0.062(6) -0.011(5) 0.013(5) 0.001(5) C9 0.161(13) 0.080(7) 0.055(6) 0.006(5) 0.008(7) -0.004(8) C10 0.184(14) 0.095(9) 0.080(8) 0.014(7) 0.008(9) 0.013(9) C11 0.145(13) 0.119(10) 0.109(10) 0.006(9) -0.023(9) 0.026(10) C12 0.142(15) 0.117(12) 0.135(14) -0.005(11) -0.030(12) 0.018(11) C13 0.112(11) 0.085(8) 0.093(8) -0.009(7) -0.004(8) 0.013(8) C14 0.043(5) 0.050(4) 0.066(5) 0.002(4) 0.016(4) 0.002(4) C15 0.049(5) 0.072(6) 0.065(5) -0.010(4) 0.019(4) -0.012(4) C16 0.070(7) 0.077(6) 0.072(6) -0.020(5) 0.026(5) -0.002(5) C17 0.081(7) 0.051(5) 0.105(8) -0.011(5) 0.041(6) 0.004(5) C18 0.099(9) 0.056(6) 0.106(9) 0.011(6) 0.045(7) 0.018(6) C19 0.084(7) 0.055(5) 0.074(6) 0.006(5) 0.021(5) 0.010(5) C20 0.047(5) 0.045(4) 0.086(6) -0.010(4) 0.012(5) 0.001(4) C21 0.076(7) 0.068(6) 0.081(7) -0.003(5) -0.008(6) -0.014(5) C22 0.078(9) 0.108(10) 0.116(10) -0.027(8) -0.035(8) -0.008(8) C23 0.069(8) 0.111(9) 0.153(12) -0.050(9) -0.003(8) 0.002(7) C24 0.059(7) 0.129(10) 0.178(13) -0.056(10) 0.036(8) 0.003(7) C25 0.047(6) 0.109(9) 0.152(12) -0.059(9) 0.028(7) -0.013(6) C26 0.050(6) 0.077(6) 0.096(7) -0.023(6) 0.041(5) -0.015(5) C27 0.074(8) 0.167(14) 0.086(8) -0.035(9) 0.018(7) -0.047(9) C28 0.094(11) 0.189(18) 0.112(11) -0.054(12) 0.020(9) -0.034(11) C29 0.067(8) 0.155(12) 0.140(11) -0.066(10) 0.044(8) -0.028(8) C30 0.080(8) 0.107(9) 0.192(14) -0.042(9) 0.077(9) -0.036(7) C31 0.080(8) 0.077(7) 0.157(12) -0.027(7) 0.064(8) -0.030(6) C32 0.074(7) 0.090(7) 0.072(6) 0.014(6) 0.037(5) -0.008(6) C33 0.103(10) 0.107(9) 0.093(9) 0.034(7) 0.033(7) -0.016(8) C34 0.124(13) 0.148(14) 0.119(12) 0.055(11) 0.038(10) -0.027(11) C35 0.129(12) 0.193(15) 0.107(10) 0.054(11) 0.056(9) -0.012(11) C36 0.130(13) 0.193(18) 0.083(9) -0.001(10) 0.055(9) 0.001(13) C37 0.118(11) 0.135(11) 0.073(7) 0.010(8) 0.049(7) 0.015(9) C38 0.094(8) 0.049(5) 0.056(5) -0.004(4) 0.032(5) -0.011(5) C39 0.113(10) 0.075(7) 0.076(7) -0.007(6) 0.041(7) 0.001(6) C40 0.129(11) 0.076(7) 0.058(6) -0.020(5) 0.018(7) -0.021(7) C41 0.108(10) 0.075(7) 0.068(7) -0.008(5) 0.002(6) -0.001(7) C42 0.069(7) 0.091(7) 0.077(7) -0.005(6) 0.009(5) -0.012(6) C43 0.070(7) 0.071(6) 0.071(6) -0.019(5) 0.015(5) -0.016(5) C44 0.059(6) 0.052(5) 0.082(6) -0.001(4) 0.019(5) 0.001(4) C45 0.145(13) 0.065(7) 0.088(8) 0.003(6) -0.016(8) -0.021(7) C46 0.160(13) 0.071(7) 0.125(11) 0.010(7) -0.021(9) -0.015(8) C47 0.098(9) 0.072(7) 0.097(9) 0.019(6) -0.006(7) -0.006(6) C48 0.112(11) 0.079(8) 0.096(9) 0.006(7) 0.003(8) 0.013(7) C49 0.090(8) 0.055(6) 0.097(8) -0.011(5) -0.013(7) -0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 P8 2.212(2) . ? Cu1 Se2 2.3471(16) . ? Cu1 Se5 2.4027(15) 3_667 ? Cu1 Cu3 2.8043(18) . ? Se2 P9 2.226(3) . ? Se2 Cu3 2.4643(16) . ? Cu3 P4 2.266(3) . ? Cu3 Se7 2.4799(15) 3_667 ? Cu3 Se5 2.5404(14) . ? P4 C8 1.820(6) . ? P4 C2 1.833(6) . ? P4 Se10 2.236(3) . ? Se5 C1 1.937(10) . ? Se5 Cu1 2.4027(15) 3_667 ? Se5 Cu6 2.5244(14) . ? Cu6 P11 2.234(3) . ? Cu6 P9 2.273(3) 3_667 ? Cu6 Se7 2.4363(15) . ? Se7 P8 2.230(2) . ? Se7 Cu3 2.4799(15) 3_667 ? P8 C20 1.825(5) . ? P8 C14 1.827(4) . ? P9 C26 1.841(6) . ? P9 C32 1.844(6) . ? P9 Cu6 2.273(3) 3_667 ? Se10 C1 1.991(10) . ? P11 C44 1.816(5) . ? P11 C38 1.816(5) . ? C2 C3 1.3900 . ? C2 C7 1.3900 . ? C3 C4 1.3900 . ? C4 C5 1.3900 . ? C5 C6 1.3900 . ? C6 C7 1.3900 . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C14 C15 1.3900 . ? C14 C19 1.3900 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C20 C21 1.3900 . ? C20 C25 1.3900 . ? C21 C22 1.3900 . ? C22 C23 1.3900 . ? C23 C24 1.3900 . ? C24 C25 1.3900 . ? C26 C27 1.3900 . ? C26 C31 1.3900 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C29 C30 1.3900 . ? C30 C31 1.3900 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 C36 1.3900 . ? C36 C37 1.3900 . ? C38 C39 1.3900 . ? C38 C43 1.3900 . ? C39 C40 1.3900 . ? C40 C41 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C44 C45 1.3900 . ? C44 C49 1.3900 . ? C45 C46 1.3900 . ? C46 C47 1.3900 . ? C47 C48 1.3900 . ? C48 C49 1.3900 . ? 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 P8 Cu1 Se2 129.01(8) . . ? P8 Cu1 Se5 109.87(8) . 3_667 ? Se2 Cu1 Se5 119.36(6) . 3_667 ? P8 Cu1 Cu3 133.35(8) . . ? Se2 Cu1 Cu3 56.32(4) . . ? Se5 Cu1 Cu3 95.04(5) 3_667 . ? P9 Se2 Cu1 95.63(7) . . ? P9 Se2 Cu3 95.73(8) . . ? Cu1 Se2 Cu3 71.25(5) . . ? P4 Cu3 Se2 111.07(9) . . ? P4 Cu3 Se7 111.61(8) . 3_667 ? Se2 Cu3 Se7 109.79(5) . 3_667 ? P4 Cu3 Se5 96.35(8) . . ? Se2 Cu3 Se5 116.17(6) . . ? Se7 Cu3 Se5 111.28(5) 3_667 . ? P4 Cu3 Cu1 141.10(9) . . ? Se2 Cu3 Cu1 52.43(4) . . ? Se7 Cu3 Cu1 107.28(5) 3_667 . ? Se5 Cu3 Cu1 69.83(4) . . ? C8 P4 C2 103.1(4) . . ? C8 P4 Se10 106.8(3) . . ? C2 P4 Se10 100.3(3) . . ? C8 P4 Cu3 119.2(3) . . ? C2 P4 Cu3 117.5(3) . . ? Se10 P4 Cu3 108.04(10) . . ? C1 Se5 Cu1 103.7(3) . 3_667 ? C1 Se5 Cu6 103.6(3) . . ? Cu1 Se5 Cu6 92.52(5) 3_667 . ? C1 Se5 Cu3 94.7(3) . . ? Cu1 Se5 Cu3 94.81(5) 3_667 . ? Cu6 Se5 Cu3 158.15(6) . . ? P11 Cu6 P9 124.37(10) . 3_667 ? P11 Cu6 Se7 119.71(9) . . ? P9 Cu6 Se7 97.05(8) 3_667 . ? P11 Cu6 Se5 106.24(8) . . ? P9 Cu6 Se5 105.09(8) 3_667 . ? Se7 Cu6 Se5 101.56(5) . . ? P8 Se7 Cu6 99.39(7) . . ? P8 Se7 Cu3 99.54(7) . 3_667 ? Cu6 Se7 Cu3 92.61(5) . 3_667 ? C20 P8 C14 102.7(3) . . ? C20 P8 Cu1 112.8(2) . . ? C14 P8 Cu1 117.0(2) . . ? C20 P8 Se7 105.7(2) . . ? C14 P8 Se7 105.1(2) . . ? Cu1 P8 Se7 112.54(10) . . ? C26 P9 C32 104.5(4) . . ? C26 P9 Se2 104.5(3) . . ? C32 P9 Se2 105.1(3) . . ? C26 P9 Cu6 118.9(3) . 3_667 ? C32 P9 Cu6 112.1(3) . 3_667 ? Se2 P9 Cu6 110.60(10) . 3_667 ? C1 Se10 P4 95.0(3) . . ? C44 P11 C38 102.9(3) . . ? C44 P11 Cu6 119.8(2) . . ? C38 P11 Cu6 115.7(2) . . ? Se5 C1 Se10 112.5(5) . . ? C3 C2 C7 120.0 . . ? C3 C2 P4 117.3(5) . . ? C7 C2 P4 122.5(5) . . ? C2 C3 C4 120.0 . . ? C5 C4 C3 120.0 . . ? C4 C5 C6 120.0 . . ? C5 C6 C7 120.0 . . ? C6 C7 C2 120.0 . . ? C9 C8 C13 120.0 . . ? C9 C8 P4 116.2(5) . . ? C13 C8 P4 123.8(5) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C12 C11 C10 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C8 120.0 . . ? C15 C14 C19 120.0 . . ? C15 C14 P8 117.7(3) . . ? C19 C14 P8 122.3(3) . . ? C14 C15 C16 120.0 . . ? C15 C16 C17 120.0 . . ? C18 C17 C16 120.0 . . ? C17 C18 C19 120.0 . . ? C18 C19 C14 120.0 . . ? C21 C20 C25 120.0 . . ? C21 C20 P8 122.6(4) . . ? C25 C20 P8 117.3(4) . . ? C22 C21 C20 120.0 . . ? C21 C22 C23 120.0 . . ? C24 C23 C22 120.0 . . ? C23 C24 C25 120.0 . . ? C24 C25 C20 120.0 . . ? C27 C26 C31 120.0 . . ? C27 C26 P9 117.3(4) . . ? C31 C26 P9 122.5(4) . . ? C26 C27 C28 120.0 . . ? C27 C28 C29 120.0 . . ? C28 C29 C30 120.0 . . ? C31 C30 C29 120.0 . . ? C30 C31 C26 120.0 . . ? C33 C32 C37 120.0 . . ? C33 C32 P9 117.1(5) . . ? C37 C32 P9 122.9(5) . . ? C32 C33 C34 120.0 . . ? C35 C34 C33 120.0 . . ? C36 C35 C34 120.0 . . ? C37 C36 C35 120.0 . . ? C36 C37 C32 120.0 . . ? C39 C38 C43 120.0 . . ? C39 C38 P11 122.9(4) . . ? C43 C38 P11 116.9(4) . . ? C38 C39 C40 120.0 . . ? C39 C40 C41 120.0 . . ? C42 C41 C40 120.0 . . ? C41 C42 C43 120.0 . . ? C42 C43 C38 120.0 . . ? C45 C44 C49 120.0 . . ? C45 C44 P11 121.3(4) . . ? C49 C44 P11 118.7(4) . . ? C46 C45 C44 120.0 . . ? C45 C46 C47 120.0 . . ? C46 C47 C48 120.0 . . ? C49 C48 C47 120.0 . . ? C48 C49 C44 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 60.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.176 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.102 #===END