Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Dmitri Konarev' 'Philip Coppens' 'A. Yu. Kovalevsky' 'Dmitri V. Lopatin' 'Rimma N. Lyubovskaya' 'Gunzi Saito' 'Alexey V. Umrikhin' 'Evgeniya I. Yudanova' _publ_contact_author_name 'Dr Dmitri Konarev' _publ_contact_author_address ; Graduate Scool of Science Kyoto University Sakyo-ku 606-8502 Kyoto 606-8502 JAPAN ; _publ_contact_author_email KONAREV@KUCHEM.KYOTO-U.AC.JP _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Synthesis, crystal structure and photoconductivity of first fullerene[60] complex with metal diethyldithiocarbamate: {CuII(dedtc)2}2 C60 ; data_cus4c60a _database_code_depnum_ccdc_archive 'CCDC 260289' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H40 Cu2 N4 S8' _chemical_formula_weight 1440.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 16.1948(8) _cell_length_b 10.2552(5) _cell_length_c 17.2192(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.504(2) _cell_angle_gamma 90.00 _cell_volume 2791.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used **** _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 26.99 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 1.120 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6628 _exptl_absorpt_correction_T_max 0.7670 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25977 _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 27.06 _reflns_number_total 5683 _reflns_number_gt 4983 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0341P)^2^+8.2311P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0094(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5683 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _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 0.07888(2) 0.49329(3) 0.44368(2) 0.01367(12) Uani 1 1 d . . . S1 S 0.07896(4) 0.72101(7) 0.44296(4) 0.01470(17) Uani 1 1 d . . . S2 S 0.11010(5) 0.54523(7) 0.57674(5) 0.01469(17) Uani 1 1 d . . . S3 S 0.08841(4) 0.44141(7) 0.31610(4) 0.01419(17) Uani 1 1 d . . . S4 S 0.09666(4) 0.26858(7) 0.44921(4) 0.01440(17) Uani 1 1 d . . . N1 N 0.13959(16) 0.8011(2) 0.59383(15) 0.0155(5) Uani 1 1 d . . . N2 N 0.11060(15) 0.1844(2) 0.30428(15) 0.0145(5) Uani 1 1 d . . . C1 C 0.11229(17) 0.7042(3) 0.54442(18) 0.0133(6) Uani 1 1 d . . . C2 C 0.13612(19) 0.9384(3) 0.56685(19) 0.0173(6) Uani 1 1 d . . . H2A H 0.1166 0.9942 0.6062 0.021 Uiso 1 1 calc R . . H2B H 0.0947 0.9464 0.5155 0.021 Uiso 1 1 calc R . . C3 C 0.2222(2) 0.9856(3) 0.5567(2) 0.0226(7) Uani 1 1 d . . . H3A H 0.2179 1.0767 0.5392 0.034 Uiso 1 1 calc R . . H3B H 0.2410 0.9318 0.5168 0.034 Uiso 1 1 calc R . . H3C H 0.2631 0.9787 0.6076 0.034 Uiso 1 1 calc R . . C4 C 0.17553(19) 0.7795(3) 0.67915(19) 0.0190(7) Uani 1 1 d . . . H4A H 0.2144 0.8520 0.7000 0.023 Uiso 1 1 calc R . . H4B H 0.2087 0.6976 0.6859 0.023 Uiso 1 1 calc R . . C5 C 0.1070(2) 0.7712(3) 0.72647(19) 0.0196(7) Uani 1 1 d . . . H5A H 0.1329 0.7572 0.7828 0.029 Uiso 1 1 calc R . . H5B H 0.0691 0.6983 0.7067 0.029 Uiso 1 1 calc R . . H5C H 0.0746 0.8526 0.7205 0.029 Uiso 1 1 calc R . . C6 C 0.10076(16) 0.2832(3) 0.35060(18) 0.0132(6) Uani 1 1 d . . . C7 C 0.10230(19) 0.2026(3) 0.21842(19) 0.0183(6) Uani 1 1 d . . . H7A H 0.0575 0.2681 0.1996 0.022 Uiso 1 1 calc R . . H7B H 0.0833 0.1192 0.1913 0.022 Uiso 1 1 calc R . . C8 C 0.1823(2) 0.2461(3) 0.1934(2) 0.0225(7) Uani 1 1 d . . . H8A H 0.1709 0.2554 0.1354 0.034 Uiso 1 1 calc R . . H8B H 0.2268 0.1810 0.2103 0.034 Uiso 1 1 calc R . . H8C H 0.2008 0.3301 0.2183 0.034 Uiso 1 1 calc R . . C9 C 0.12294(19) 0.0501(3) 0.3351(2) 0.0181(6) Uani 1 1 d . . . H9A H 0.0803 -0.0075 0.3020 0.022 Uiso 1 1 calc R . . H9B H 0.1138 0.0480 0.3901 0.022 Uiso 1 1 calc R . . C10 C 0.2107(2) -0.0015(3) 0.3349(2) 0.0278(8) Uani 1 1 d . . . H10A H 0.2161 -0.0906 0.3561 0.042 Uiso 1 1 calc R . . H10B H 0.2531 0.0545 0.3683 0.042 Uiso 1 1 calc R . . H10C H 0.2195 -0.0018 0.2804 0.042 Uiso 1 1 calc R . . C11 C 0.58332(19) 0.2769(3) 0.65426(19) 0.0189(6) Uani 1 1 d . . . C12 C 0.6015(2) 0.5019(3) 0.70386(18) 0.0177(7) Uani 1 1 d . . . C13 C 0.4221(2) 0.5016(3) 0.6770(2) 0.0194(7) Uani 1 1 d . . . C14 C 0.69210(18) 0.6707(3) 0.5619(2) 0.0190(7) Uani 1 1 d . . . C15 C 0.4679(2) 0.6240(3) 0.68290(19) 0.0189(7) Uani 1 1 d . . . C16 C 0.34515(19) 0.5162(3) 0.6166(2) 0.0182(7) Uani 1 1 d . . . C17 C 0.30335(18) 0.5859(3) 0.37672(19) 0.0190(7) Uani 1 1 d . . . C18 C 0.5982(2) 0.7154(3) 0.65291(19) 0.0203(7) Uani 1 1 d . . . C19 C 0.34883(19) 0.7086(3) 0.3830(2) 0.0199(7) Uani 1 1 d . . . C20 C 0.67246(19) 0.5169(3) 0.6654(2) 0.0197(7) Uani 1 1 d . . . C21 C 0.43485(19) 0.2767(3) 0.63157(19) 0.0179(6) Uani 1 1 d . . . C22 C 0.4599(2) 0.8016(3) 0.5851(2) 0.0193(7) Uani 1 1 d . . . C23 C 0.4662(2) 0.3841(3) 0.68436(19) 0.0185(7) Uani 1 1 d . . . C24 C 0.49265(19) 0.7903(3) 0.3873(2) 0.0187(7) Uani 1 1 d . . . C25 C 0.5558(2) 0.6243(3) 0.69601(19) 0.0200(7) Uani 1 1 d . . . C26 C 0.35650(19) 0.2388(3) 0.4947(2) 0.0190(7) Uani 1 1 d . . . C27 C 0.35368(19) 0.7597(3) 0.4617(2) 0.0202(7) Uani 1 1 d . . . C28 C 0.41894(19) 0.7149(3) 0.62606(19) 0.0189(7) Uani 1 1 d . . . C29 C 0.5578(2) 0.3846(3) 0.69815(18) 0.0186(7) Uani 1 1 d . . . C30 C 0.4972(2) 0.8400(3) 0.4629(2) 0.0186(7) Uani 1 1 d . . . C31 C 0.5512(2) 0.8019(3) 0.5988(2) 0.0190(7) Uani 1 1 d . . . C32 C 0.34293(19) 0.6476(3) 0.5854(2) 0.0187(7) Uani 1 1 d . . . C33 C 0.5745(2) 0.8255(3) 0.5234(2) 0.0185(6) Uani 1 1 d . . . C34 C 0.28236(17) 0.4371(3) 0.4824(2) 0.0185(7) Uani 1 1 d . . . C35 C 0.67028(19) 0.6485(3) 0.63386(19) 0.0193(7) Uani 1 1 d . . . C36 C 0.42657(19) 0.8250(3) 0.5012(2) 0.0190(7) Uani 1 1 d . . . C37 C 0.31138(18) 0.6698(3) 0.5048(2) 0.0182(7) Uani 1 1 d . . . C38 C 0.36087(19) 0.2906(3) 0.5736(2) 0.0188(7) Uani 1 1 d . . . C39 C 0.31529(18) 0.4126(3) 0.56609(19) 0.0180(6) Uani 1 1 d . . . C40 C 0.28011(17) 0.5624(3) 0.4522(2) 0.0191(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01777(19) 0.01070(19) 0.0127(2) -0.00096(13) 0.00366(14) 0.00157(13) S1 0.0191(3) 0.0119(3) 0.0126(4) 0.0001(3) 0.0023(3) 0.0005(3) S2 0.0201(3) 0.0111(3) 0.0138(4) 0.0010(3) 0.0058(3) 0.0008(3) S3 0.0175(3) 0.0113(3) 0.0137(4) -0.0001(3) 0.0033(3) 0.0007(3) S4 0.0173(3) 0.0128(3) 0.0139(4) 0.0005(3) 0.0049(3) 0.0006(3) N1 0.0225(12) 0.0114(12) 0.0130(14) -0.0004(10) 0.0044(10) -0.0013(10) N2 0.0174(12) 0.0095(11) 0.0161(14) -0.0015(10) 0.0028(10) 0.0007(9) C1 0.0133(12) 0.0142(14) 0.0137(16) -0.0023(11) 0.0057(11) 0.0010(10) C2 0.0228(15) 0.0098(13) 0.0194(18) 0.0005(12) 0.0052(12) 0.0014(11) C3 0.0250(16) 0.0167(15) 0.028(2) 0.0023(13) 0.0096(14) -0.0005(12) C4 0.0179(14) 0.0196(15) 0.0185(18) -0.0027(13) 0.0019(12) -0.0020(11) C5 0.0228(15) 0.0198(16) 0.0159(18) 0.0003(13) 0.0036(13) 0.0005(12) C6 0.0083(12) 0.0142(14) 0.0169(16) 0.0002(12) 0.0023(11) 0.0004(10) C7 0.0209(14) 0.0172(15) 0.0148(17) -0.0018(12) -0.0008(12) 0.0017(12) C8 0.0267(16) 0.0237(16) 0.0177(18) -0.0011(14) 0.0060(13) 0.0010(13) C9 0.0259(15) 0.0102(14) 0.0174(17) -0.0003(12) 0.0029(13) 0.0024(11) C10 0.0242(16) 0.0171(16) 0.039(2) 0.0012(14) -0.0009(15) 0.0048(13) C11 0.0229(15) 0.0178(15) 0.0141(17) 0.0078(12) 0.0001(12) 0.0046(12) C12 0.0213(15) 0.0250(17) 0.0052(17) -0.0015(12) -0.0009(12) -0.0009(12) C13 0.0247(15) 0.0229(16) 0.0140(18) -0.0006(12) 0.0116(13) -0.0011(12) C14 0.0125(13) 0.0199(15) 0.0237(19) -0.0046(13) 0.0021(12) -0.0075(11) C15 0.0268(16) 0.0204(16) 0.0112(17) -0.0060(12) 0.0080(13) -0.0007(12) C16 0.0167(14) 0.0238(16) 0.0184(18) 0.0005(13) 0.0128(13) 0.0015(12) C17 0.0122(13) 0.0231(16) 0.0186(18) 0.0074(13) -0.0033(12) 0.0032(11) C18 0.0222(15) 0.0211(16) 0.0164(18) -0.0087(13) 0.0019(13) -0.0071(12) C19 0.0160(14) 0.0201(15) 0.0214(19) 0.0064(13) -0.0007(12) 0.0065(12) C20 0.0160(14) 0.0267(17) 0.0125(17) 0.0012(13) -0.0055(12) -0.0030(12) C21 0.0230(15) 0.0157(15) 0.0172(17) 0.0056(12) 0.0089(13) -0.0022(12) C22 0.0258(15) 0.0107(14) 0.0226(19) -0.0065(12) 0.0077(13) 0.0008(12) C23 0.0240(15) 0.0224(16) 0.0102(17) 0.0054(12) 0.0064(12) -0.0017(12) C24 0.0233(15) 0.0119(14) 0.0217(18) 0.0074(12) 0.0064(13) 0.0001(11) C25 0.0277(16) 0.0211(16) 0.0107(17) -0.0053(12) 0.0035(13) -0.0040(12) C26 0.0170(14) 0.0154(14) 0.0254(19) 0.0000(13) 0.0061(13) -0.0076(11) C27 0.0179(14) 0.0164(15) 0.0264(19) 0.0042(13) 0.0053(13) 0.0091(12) C28 0.0235(15) 0.0171(15) 0.0184(18) -0.0063(13) 0.0093(13) 0.0037(12) C29 0.0253(16) 0.0230(16) 0.0068(16) 0.0047(12) 0.0016(12) 0.0014(12) C30 0.0256(15) 0.0076(13) 0.0232(19) 0.0054(12) 0.0063(13) 0.0006(11) C31 0.0241(15) 0.0118(14) 0.0213(18) -0.0077(12) 0.0051(13) -0.0053(12) C32 0.0171(14) 0.0177(15) 0.0246(19) -0.0051(13) 0.0117(13) 0.0044(12) C33 0.0240(15) 0.0091(13) 0.0223(18) -0.0013(12) 0.0047(13) -0.0056(11) C34 0.0094(12) 0.0231(16) 0.0225(18) 0.0005(13) 0.0025(12) -0.0028(11) C35 0.0169(14) 0.0218(16) 0.0172(18) -0.0035(13) -0.0008(12) -0.0067(12) C36 0.0226(15) 0.0086(13) 0.0270(19) 0.0000(12) 0.0083(13) 0.0053(11) C37 0.0135(13) 0.0170(15) 0.0247(19) 0.0001(13) 0.0058(12) 0.0057(11) C38 0.0192(14) 0.0169(15) 0.0230(18) 0.0038(13) 0.0105(13) -0.0064(11) C39 0.0137(13) 0.0218(15) 0.0218(18) 0.0007(13) 0.0112(12) -0.0030(11) C40 0.0097(13) 0.0243(16) 0.0223(18) 0.0011(14) 0.0016(12) 0.0032(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 Cu1 S3 2.2978(8) . ? Cu1 S2 2.2994(9) . ? Cu1 S4 2.3218(8) . ? Cu1 S1 2.3354(8) . ? S1 C1 1.722(3) . ? S2 C1 1.725(3) . ? S3 C6 1.724(3) . ? S4 C6 1.720(3) . ? N1 C1 1.321(4) . ? N1 C4 1.475(4) . ? N1 C2 1.480(4) . ? N2 C6 1.320(4) . ? N2 C7 1.467(4) . ? N2 C9 1.474(4) . ? C2 C3 1.521(4) . ? C4 C5 1.516(4) . ? C7 C8 1.519(4) . ? C9 C10 1.516(4) . ? C11 C19 1.395(4) 3_666 ? C11 C29 1.448(4) . ? C11 C24 1.456(4) 3_666 ? C12 C29 1.388(4) . ? C12 C25 1.448(4) . ? C12 C20 1.454(4) . ? C13 C23 1.392(4) . ? C13 C16 1.448(5) . ? C13 C15 1.451(4) . ? C14 C35 1.379(5) . ? C14 C26 1.448(5) 3_666 ? C14 C34 1.453(4) 3_666 ? C15 C25 1.393(4) . ? C15 C28 1.456(5) . ? C16 C39 1.392(5) . ? C16 C32 1.448(4) . ? C17 C20 1.384(5) 3_666 ? C17 C40 1.449(5) . ? C17 C19 1.450(4) . ? C18 C31 1.388(5) . ? C18 C35 1.451(4) . ? C18 C25 1.454(4) . ? C19 C11 1.395(4) 3_666 ? C19 C27 1.439(5) . ? C20 C17 1.384(5) 3_666 ? C20 C35 1.453(4) . ? C21 C38 1.391(4) . ? C21 C23 1.449(4) . ? C21 C24 1.456(4) 3_666 ? C22 C28 1.389(4) . ? C22 C31 1.446(4) . ? C22 C36 1.448(5) . ? C23 C29 1.451(4) . ? C24 C30 1.385(5) . ? C24 C11 1.456(4) 3_666 ? C24 C21 1.456(4) 3_666 ? C26 C33 1.390(4) 3_666 ? C26 C38 1.446(5) . ? C26 C14 1.448(5) 3_666 ? C27 C36 1.399(5) . ? C27 C37 1.445(4) . ? C28 C32 1.452(4) . ? C30 C36 1.447(4) . ? C30 C33 1.453(4) . ? C31 C33 1.449(5) . ? C32 C37 1.391(5) . ? C33 C26 1.390(4) 3_666 ? C34 C40 1.384(5) . ? C34 C39 1.446(5) . ? C34 C14 1.453(4) 3_666 ? C37 C40 1.446(5) . ? C38 C39 1.445(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Cu1 S2 163.84(3) . . ? S3 Cu1 S4 77.06(3) . . ? S2 Cu1 S4 100.98(3) . . ? S3 Cu1 S1 103.07(3) . . ? S2 Cu1 S1 76.90(3) . . ? S4 Cu1 S1 173.00(3) . . ? C1 S1 Cu1 83.96(10) . . ? C1 S2 Cu1 85.00(10) . . ? C6 S3 Cu1 85.13(10) . . ? C6 S4 Cu1 84.47(10) . . ? C1 N1 C4 122.2(3) . . ? C1 N1 C2 121.9(3) . . ? C4 N1 C2 115.8(2) . . ? C6 N2 C7 121.0(3) . . ? C6 N2 C9 121.6(3) . . ? C7 N2 C9 117.2(2) . . ? N1 C1 S1 124.5(2) . . ? N1 C1 S2 122.1(2) . . ? S1 C1 S2 113.47(16) . . ? N1 C2 C3 111.4(2) . . ? N1 C4 C5 111.5(2) . . ? N2 C6 S4 124.4(2) . . ? N2 C6 S3 122.3(2) . . ? S4 C6 S3 113.33(17) . . ? N2 C7 C8 115.2(3) . . ? N2 C9 C10 112.3(3) . . ? C19 C11 C29 120.1(3) 3_666 . ? C19 C11 C24 119.4(3) 3_666 3_666 ? C29 C11 C24 108.2(3) . 3_666 ? C29 C12 C25 120.2(3) . . ? C29 C12 C20 120.0(3) . . ? C25 C12 C20 107.7(3) . . ? C23 C13 C16 120.0(3) . . ? C23 C13 C15 119.9(3) . . ? C16 C13 C15 107.9(3) . . ? C35 C14 C26 120.1(3) . 3_666 ? C35 C14 C34 120.3(3) . 3_666 ? C26 C14 C34 108.0(3) 3_666 3_666 ? C25 C15 C13 120.2(3) . . ? C25 C15 C28 119.7(3) . . ? C13 C15 C28 108.2(3) . . ? C39 C16 C13 119.9(3) . . ? C39 C16 C32 120.1(3) . . ? C13 C16 C32 108.2(3) . . ? C20 C17 C40 120.1(3) 3_666 . ? C20 C17 C19 120.2(3) 3_666 . ? C40 C17 C19 107.7(3) . . ? C31 C18 C35 120.1(3) . . ? C31 C18 C25 120.1(3) . . ? C35 C18 C25 107.7(3) . . ? C11 C19 C27 120.4(3) 3_666 . ? C11 C19 C17 119.7(3) 3_666 . ? C27 C19 C17 108.0(3) . . ? C17 C20 C35 119.9(3) 3_666 . ? C17 C20 C12 120.0(3) 3_666 . ? C35 C20 C12 108.1(3) . . ? C38 C21 C23 120.2(3) . . ? C38 C21 C24 119.9(3) . 3_666 ? C23 C21 C24 108.0(3) . 3_666 ? C28 C22 C31 120.1(3) . . ? C28 C22 C36 119.8(3) . . ? C31 C22 C36 108.0(3) . . ? C13 C23 C21 119.9(3) . . ? C13 C23 C29 119.9(3) . . ? C21 C23 C29 108.2(3) . . ? C30 C24 C11 120.2(3) . 3_666 ? C30 C24 C21 120.1(3) . 3_666 ? C11 C24 C21 107.7(3) 3_666 3_666 ? C15 C25 C12 119.8(3) . . ? C15 C25 C18 119.8(3) . . ? C12 C25 C18 108.5(3) . . ? C33 C26 C38 120.4(3) 3_666 . ? C33 C26 C14 120.0(3) 3_666 3_666 ? C38 C26 C14 107.8(3) . 3_666 ? C36 C27 C19 120.0(3) . . ? C36 C27 C37 120.0(3) . . ? C19 C27 C37 108.4(3) . . ? C22 C28 C32 120.5(3) . . ? C22 C28 C15 120.1(3) . . ? C32 C28 C15 107.5(3) . . ? C12 C29 C11 120.0(3) . . ? C12 C29 C23 120.1(3) . . ? C11 C29 C23 108.0(3) . . ? C24 C30 C36 120.2(3) . . ? C24 C30 C33 119.9(3) . . ? C36 C30 C33 107.8(3) . . ? C18 C31 C22 120.1(3) . . ? C18 C31 C33 119.8(3) . . ? C22 C31 C33 108.0(3) . . ? C37 C32 C16 119.8(3) . . ? C37 C32 C28 119.5(3) . . ? C16 C32 C28 108.2(3) . . ? C26 C33 C31 120.0(3) 3_666 . ? C26 C33 C30 119.8(3) 3_666 . ? C31 C33 C30 108.0(3) . . ? C40 C34 C39 120.6(3) . . ? C40 C34 C14 119.7(3) . 3_666 ? C39 C34 C14 107.8(3) . 3_666 ? C14 C35 C18 120.0(3) . . ? C14 C35 C20 119.9(3) . . ? C18 C35 C20 108.0(3) . . ? C27 C36 C30 119.8(3) . . ? C27 C36 C22 119.9(3) . . ? C30 C36 C22 108.2(3) . . ? C32 C37 C27 120.3(3) . . ? C32 C37 C40 120.3(3) . . ? C27 C37 C40 107.8(3) . . ? C21 C38 C39 119.8(3) . . ? C21 C38 C26 119.8(3) . . ? C39 C38 C26 108.3(3) . . ? C16 C39 C38 120.3(3) . . ? C16 C39 C34 119.6(3) . . ? C38 C39 C34 108.1(3) . . ? C34 C40 C37 119.7(3) . . ? C34 C40 C17 120.0(3) . . ? C37 C40 C17 108.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S3 Cu1 S1 C1 -158.21(9) . . . . ? S2 Cu1 S1 C1 5.20(9) . . . . ? S4 Cu1 S1 C1 -68.0(3) . . . . ? S3 Cu1 S2 C1 86.62(14) . . . . ? S4 Cu1 S2 C1 167.99(9) . . . . ? S1 Cu1 S2 C1 -5.18(9) . . . . ? S2 Cu1 S3 C6 84.20(14) . . . . ? S4 Cu1 S3 C6 -0.59(9) . . . . ? S1 Cu1 S3 C6 172.23(9) . . . . ? S3 Cu1 S4 C6 0.59(9) . . . . ? S2 Cu1 S4 C6 -163.01(9) . . . . ? S1 Cu1 S4 C6 -91.3(3) . . . . ? C4 N1 C1 S1 -173.6(2) . . . . ? C2 N1 C1 S1 6.2(4) . . . . ? C4 N1 C1 S2 4.3(4) . . . . ? C2 N1 C1 S2 -175.9(2) . . . . ? Cu1 S1 C1 N1 170.7(3) . . . . ? Cu1 S1 C1 S2 -7.37(13) . . . . ? Cu1 S2 C1 N1 -170.6(2) . . . . ? Cu1 S2 C1 S1 7.47(13) . . . . ? C1 N1 C2 C3 -101.6(3) . . . . ? C4 N1 C2 C3 78.3(3) . . . . ? C1 N1 C4 C5 -84.6(3) . . . . ? C2 N1 C4 C5 95.5(3) . . . . ? C7 N2 C6 S4 171.9(2) . . . . ? C9 N2 C6 S4 -2.8(4) . . . . ? C7 N2 C6 S3 -6.7(4) . . . . ? C9 N2 C6 S3 178.7(2) . . . . ? Cu1 S4 C6 N2 -179.5(2) . . . . ? Cu1 S4 C6 S3 -0.83(13) . . . . ? Cu1 S3 C6 N2 179.6(2) . . . . ? Cu1 S3 C6 S4 0.84(13) . . . . ? C6 N2 C7 C8 86.2(3) . . . . ? C9 N2 C7 C8 -98.9(3) . . . . ? C6 N2 C9 C10 -112.8(3) . . . . ? C7 N2 C9 C10 72.4(3) . . . . ? C23 C13 C15 C25 -0.2(5) . . . . ? C16 C13 C15 C25 -142.5(3) . . . . ? C23 C13 C15 C28 142.5(3) . . . . ? C16 C13 C15 C28 0.2(3) . . . . ? C23 C13 C16 C39 0.2(4) . . . . ? C15 C13 C16 C39 142.5(3) . . . . ? C23 C13 C16 C32 -142.6(3) . . . . ? C15 C13 C16 C32 -0.3(3) . . . . ? C20 C17 C19 C11 0.6(5) 3_666 . . 3_666 ? C40 C17 C19 C11 143.2(3) . . . 3_666 ? C20 C17 C19 C27 -142.5(3) 3_666 . . . ? C40 C17 C19 C27 0.2(3) . . . . ? C29 C12 C20 C17 -0.1(5) . . . 3_666 ? C25 C12 C20 C17 -142.7(3) . . . 3_666 ? C29 C12 C20 C35 142.5(3) . . . . ? C25 C12 C20 C35 -0.1(3) . . . . ? C16 C13 C23 C21 -0.2(4) . . . . ? C15 C13 C23 C21 -138.0(3) . . . . ? C16 C13 C23 C29 138.1(3) . . . . ? C15 C13 C23 C29 0.3(5) . . . . ? C38 C21 C23 C13 0.1(4) . . . . ? C24 C21 C23 C13 142.8(3) 3_666 . . . ? C38 C21 C23 C29 -142.5(3) . . . . ? C24 C21 C23 C29 0.2(3) 3_666 . . . ? C13 C15 C25 C12 -0.1(5) . . . . ? C28 C15 C25 C12 -138.5(3) . . . . ? C13 C15 C25 C18 138.4(3) . . . . ? C28 C15 C25 C18 0.0(4) . . . . ? C29 C12 C25 C15 0.2(5) . . . . ? C20 C12 C25 C15 142.6(3) . . . . ? C29 C12 C25 C18 -142.5(3) . . . . ? C20 C12 C25 C18 0.0(3) . . . . ? C31 C18 C25 C15 0.0(5) . . . . ? C35 C18 C25 C15 -142.5(3) . . . . ? C31 C18 C25 C12 142.7(3) . . . . ? C35 C18 C25 C12 0.2(3) . . . . ? C11 C19 C27 C36 0.3(4) 3_666 . . . ? C17 C19 C27 C36 143.1(3) . . . . ? C11 C19 C27 C37 -142.8(3) 3_666 . . . ? C17 C19 C27 C37 -0.1(3) . . . . ? C31 C22 C28 C32 -138.2(3) . . . . ? C36 C22 C28 C32 0.0(4) . . . . ? C31 C22 C28 C15 -0.1(4) . . . . ? C36 C22 C28 C15 138.1(3) . . . . ? C25 C15 C28 C22 0.0(4) . . . . ? C13 C15 C28 C22 -142.8(3) . . . . ? C25 C15 C28 C32 142.9(3) . . . . ? C13 C15 C28 C32 0.1(3) . . . . ? C25 C12 C29 C11 138.2(3) . . . . ? C20 C12 C29 C11 0.3(5) . . . . ? C25 C12 C29 C23 -0.1(5) . . . . ? C20 C12 C29 C23 -138.0(3) . . . . ? C19 C11 C29 C12 -0.7(5) 3_666 . . . ? C24 C11 C29 C12 -142.5(3) 3_666 . . . ? C19 C11 C29 C23 142.1(3) 3_666 . . . ? C24 C11 C29 C23 0.3(3) 3_666 . . . ? C13 C23 C29 C12 -0.2(5) . . . . ? C21 C23 C29 C12 142.4(3) . . . . ? C13 C23 C29 C11 -142.9(3) . . . . ? C21 C23 C29 C11 -0.3(3) . . . . ? C11 C24 C30 C36 0.3(4) 3_666 . . . ? C21 C24 C30 C36 -137.8(3) 3_666 . . . ? C11 C24 C30 C33 138.2(3) 3_666 . . . ? C21 C24 C30 C33 0.1(4) 3_666 . . . ? C35 C18 C31 C22 137.8(3) . . . . ? C25 C18 C31 C22 -0.1(5) . . . . ? C35 C18 C31 C33 -0.2(4) . . . . ? C25 C18 C31 C33 -138.1(3) . . . . ? C28 C22 C31 C18 0.1(4) . . . . ? C36 C22 C31 C18 -142.4(3) . . . . ? C28 C22 C31 C33 142.5(3) . . . . ? C36 C22 C31 C33 0.0(3) . . . . ? C39 C16 C32 C37 -0.4(4) . . . . ? C13 C16 C32 C37 142.3(3) . . . . ? C39 C16 C32 C28 -142.3(3) . . . . ? C13 C16 C32 C28 0.4(3) . . . . ? C22 C28 C32 C37 0.4(4) . . . . ? C15 C28 C32 C37 -142.3(3) . . . . ? C22 C28 C32 C16 142.4(3) . . . . ? C15 C28 C32 C16 -0.3(3) . . . . ? C18 C31 C33 C26 0.3(4) . . . 3_666 ? C22 C31 C33 C26 -142.2(3) . . . 3_666 ? C18 C31 C33 C30 142.6(3) . . . . ? C22 C31 C33 C30 0.1(3) . . . . ? C24 C30 C33 C26 -0.3(4) . . . 3_666 ? C36 C30 C33 C26 142.2(3) . . . 3_666 ? C24 C30 C33 C31 -142.6(3) . . . . ? C36 C30 C33 C31 -0.1(3) . . . . ? C26 C14 C35 C18 0.4(4) 3_666 . . . ? C34 C14 C35 C18 -138.5(3) 3_666 . . . ? C26 C14 C35 C20 138.6(3) 3_666 . . . ? C34 C14 C35 C20 -0.3(4) 3_666 . . . ? C31 C18 C35 C14 -0.1(4) . . . . ? C25 C18 C35 C14 142.4(3) . . . . ? C31 C18 C35 C20 -142.8(3) . . . . ? C25 C18 C35 C20 -0.2(3) . . . . ? C17 C20 C35 C14 0.2(4) 3_666 . . . ? C12 C20 C35 C14 -142.5(3) . . . . ? C17 C20 C35 C18 142.8(3) 3_666 . . . ? C12 C20 C35 C18 0.2(3) . . . . ? C19 C27 C36 C30 -0.5(4) . . . . ? C37 C27 C36 C30 138.5(3) . . . . ? C19 C27 C36 C22 -138.5(3) . . . . ? C37 C27 C36 C22 0.5(4) . . . . ? C24 C30 C36 C27 0.2(4) . . . . ? C33 C30 C36 C27 -142.2(3) . . . . ? C24 C30 C36 C22 142.5(3) . . . . ? C33 C30 C36 C22 0.1(3) . . . . ? C28 C22 C36 C27 -0.4(4) . . . . ? C31 C22 C36 C27 142.2(3) . . . . ? C28 C22 C36 C30 -142.7(3) . . . . ? C31 C22 C36 C30 -0.1(3) . . . . ? C16 C32 C37 C27 -138.0(3) . . . . ? C28 C32 C37 C27 -0.3(4) . . . . ? C16 C32 C37 C40 0.6(4) . . . . ? C28 C32 C37 C40 138.3(3) . . . . ? C36 C27 C37 C32 -0.1(4) . . . . ? C19 C27 C37 C32 143.1(3) . . . . ? C36 C27 C37 C40 -143.2(3) . . . . ? C19 C27 C37 C40 -0.1(3) . . . . ? C23 C21 C38 C39 0.0(4) . . . . ? C24 C21 C38 C39 -138.3(3) 3_666 . . . ? C23 C21 C38 C26 138.1(3) . . . . ? C24 C21 C38 C26 -0.3(4) 3_666 . . . ? C33 C26 C38 C21 0.5(4) 3_666 . . . ? C14 C26 C38 C21 -142.4(3) 3_666 . . . ? C33 C26 C38 C39 142.8(3) 3_666 . . . ? C14 C26 C38 C39 -0.1(3) 3_666 . . . ? C13 C16 C39 C38 -0.1(4) . . . . ? C32 C16 C39 C38 138.3(3) . . . . ? C13 C16 C39 C34 -138.2(3) . . . . ? C32 C16 C39 C34 0.2(4) . . . . ? C21 C38 C39 C16 0.0(4) . . . . ? C26 C38 C39 C16 -142.3(3) . . . . ? C21 C38 C39 C34 142.4(3) . . . . ? C26 C38 C39 C34 0.1(3) . . . . ? C40 C34 C39 C16 -0.1(4) . . . . ? C14 C34 C39 C16 142.6(3) 3_666 . . . ? C40 C34 C39 C38 -142.8(3) . . . . ? C14 C34 C39 C38 0.0(3) 3_666 . . . ? C39 C34 C40 C37 0.3(4) . . . . ? C14 C34 C40 C37 -138.1(3) 3_666 . . . ? C39 C34 C40 C17 138.3(3) . . . . ? C14 C34 C40 C17 -0.1(4) 3_666 . . . ? C32 C37 C40 C34 -0.5(4) . . . . ? C27 C37 C40 C34 142.6(3) . . . . ? C32 C37 C40 C17 -143.0(3) . . . . ? C27 C37 C40 C17 0.2(3) . . . . ? C20 C17 C40 C34 0.2(4) 3_666 . . . ? C19 C17 C40 C34 -142.5(3) . . . . ? C20 C17 C40 C37 142.5(3) 3_666 . . . ? C19 C17 C40 C37 -0.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.134 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.091