Electronic Supplementary Material for Journal of Materials Chemistry. This journal is © The Royal Society of Chemistry 2004. data_1 _publ_requested_journal 'Journal of Materials Chemistry' _publ_contact_author_name ; Sandrine Perruchas, Kamal Boubekeur and Pascale Auban-Senzier ; _publ_contact_author_address ; Institut des Materiaux Jean Rouxel 2 rue de la Houssiniere BP 32229 44322 nantes Cedex 3 FRANCE present address for S. Perruchas: Baker laboratories department of chemistry Cornell University Ithaca NY 14853 USA ; _publ_contact_author_email 'sp353@cornell.edu' _publ_section_title ; Radical cation salts of TTF derivatives incorporating the maleonitriledithiolate copper cluster anion [Cu8(i-mnt)6]4- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetrakis-tetrapropylamonium-hexa-iso-maleonitrile- octa-cuprate(I)bis-acetonitrile solvate ; _chemical_name_common '(TPA)4[Cu8(i-mnt)6],2MeCN' _chemical_formula_moiety 'C24 Cu8 N12 S12, 4(C12 H28 N), 2(C2 H3 N)' _chemical_formula_sum 'C76 H118 Cu8 N18 S12' _chemical_formula_weight 2176.92 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 P21/n _symmetry_space_group_name_Hall '-P 2yn' 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 15.1447(8) _cell_length_b 21.8075(12) _cell_length_c 15.6767(8) _cell_angle_alpha 90.00 _cell_angle_beta 107.160(6) _cell_angle_gamma 90.00 _cell_volume 4947.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 24.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 1.986 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6264 _exptl_absorpt_correction_T_max 0.7478 _exptl_absorpt_process_details 'stoe IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe IPDS' _diffrn_measurement_method 'oscillation phi. incr. = 1.1' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38693 _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_sigmaI/netI 0.2122 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 25.84 _reflns_number_total 9503 _reflns_number_gt 3566 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(6.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0000P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 9503 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0315 _refine_ls_wR_factor_ref 0.0926 _refine_ls_wR_factor_gt 0.0588 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.08303(5) 0.08777(4) 1.08058(5) 0.04393(19) Uani 1 1 d . . . Cu2 Cu -0.01828(5) 0.08684(4) 0.89468(5) 0.0435(2) Uani 1 1 d . . . Cu3 Cu 0.16448(5) -0.02391(4) 1.06285(5) 0.04270(19) Uani 1 1 d . . . Cu4 Cu -0.06058(5) 0.02826(4) 1.12135(5) 0.04249(19) Uani 1 1 d . . . S1 S 0.10728(9) 0.06626(7) 0.85300(10) 0.0389(4) Uani 1 1 d . . . S2 S 0.21857(10) 0.07078(7) 1.05229(10) 0.0396(4) Uani 1 1 d . . . C1 C 0.2047(3) 0.0851(2) 0.9385(4) 0.0350(12) Uani 1 1 d . . . C2 C 0.2772(3) 0.1130(3) 0.9168(4) 0.0393(14) Uani 1 1 d . . . C3 C 0.3606(4) 0.1299(3) 0.9829(5) 0.0486(16) Uani 1 1 d . . . C4 C 0.2710(4) 0.1290(3) 0.8281(5) 0.0477(16) Uani 1 1 d . . . N1 N 0.4285(4) 0.1448(3) 1.0316(4) 0.0705(18) Uani 1 1 d . . . N2 N 0.2700(4) 0.1441(3) 0.7585(4) 0.0719(19) Uani 1 1 d . . . S3 S 0.16904(9) -0.09300(7) 0.95688(10) 0.0406(3) Uani 1 1 d . . . S4 S 0.00957(10) -0.15973(7) 1.00212(11) 0.0421(4) Uani 1 1 d . . . C5 C 0.1181(4) -0.1590(2) 0.9845(3) 0.0363(13) Uani 1 1 d . . . C6 C 0.1656(4) -0.2130(3) 0.9932(4) 0.0411(14) Uani 1 1 d . . . C7 C 0.2554(5) -0.2169(3) 0.9792(4) 0.0525(17) Uani 1 1 d . . . C8 C 0.1285(5) -0.2676(3) 1.0191(4) 0.0505(17) Uani 1 1 d . . . N3 N 0.3262(4) -0.2198(3) 0.9692(5) 0.080(2) Uani 1 1 d . . . N4 N 0.0984(5) -0.3101(3) 1.0405(5) 0.0746(18) Uani 1 1 d . . . S5 S 0.07112(10) 0.06367(7) 1.21613(10) 0.0421(4) Uani 1 1 d . . . S6 S 0.15862(10) -0.06092(7) 1.19488(10) 0.0409(4) Uani 1 1 d . . . C9 C 0.1426(3) 0.0014(3) 1.2596(4) 0.0383(13) Uani 1 1 d . . . C10 C 0.1886(4) 0.0010(3) 1.3487(4) 0.0451(15) Uani 1 1 d . . . C11 C 0.1812(5) 0.0501(4) 1.4046(5) 0.069(2) Uani 1 1 d . . . C12 C 0.2509(5) -0.0471(4) 1.3898(5) 0.0556(19) Uani 1 1 d . . . N6 N 0.3035(4) -0.0833(3) 1.4230(4) 0.0774(19) Uani 1 1 d . . . N5 N 0.1752(6) 0.0896(4) 1.4495(5) 0.115(3) Uani 1 1 d . . . N1A N 0.5379(3) 0.1697(2) 0.7546(3) 0.0384(11) Uani 1 1 d . . . C1A C 0.5205(4) 0.1293(3) 0.6718(4) 0.0544(17) Uani 1 1 d . . . H1A1 H 0.5196 0.1555 0.6215 0.065 Uiso 1 1 calc R . . H1A2 H 0.5727 0.1018 0.6805 0.065 Uiso 1 1 calc R . . C2A C 0.4346(5) 0.0917(4) 0.6469(5) 0.070(2) Uani 1 1 d . . . H2A1 H 0.3813 0.1186 0.6348 0.084 Uiso 1 1 calc R . . H2A2 H 0.4339 0.0654 0.6966 0.084 Uiso 1 1 calc R . . C3A C 0.4283(6) 0.0533(3) 0.5664(5) 0.083(3) Uani 1 1 d . . . H3A1 H 0.3720 0.0300 0.5515 0.124 Uiso 1 1 calc R . . H3A2 H 0.4801 0.0259 0.5789 0.124 Uiso 1 1 calc R . . H3A3 H 0.4287 0.0793 0.5172 0.124 Uiso 1 1 calc R . . C4A C 0.6334(4) 0.1969(3) 0.7761(5) 0.0589(19) Uani 1 1 d . . . H4A1 H 0.6457 0.2186 0.8324 0.071 Uiso 1 1 calc R . . H4A2 H 0.6773 0.1634 0.7850 0.071 Uiso 1 1 calc R . . C5A C 0.6516(5) 0.2393(4) 0.7097(5) 0.087(3) Uani 1 1 d . . . H5A1 H 0.6085 0.2732 0.7002 0.104 Uiso 1 1 calc R . . H5A2 H 0.6412 0.2179 0.6533 0.104 Uiso 1 1 calc R . . C6A C 0.7490(6) 0.2640(5) 0.7386(6) 0.115(4) Uani 1 1 d . . . H6A1 H 0.7575 0.2914 0.6937 0.173 Uiso 1 1 calc R . . H6A2 H 0.7920 0.2306 0.7466 0.173 Uiso 1 1 calc R . . H6A3 H 0.7593 0.2858 0.7939 0.173 Uiso 1 1 calc R . . C7A C 0.4654(4) 0.2205(3) 0.7349(5) 0.0549(17) Uani 1 1 d . . . H7A1 H 0.4683 0.2421 0.6817 0.066 Uiso 1 1 calc R . . H7A2 H 0.4048 0.2017 0.7214 0.066 Uiso 1 1 calc R . . C8A C 0.4734(6) 0.2662(4) 0.8067(6) 0.084(3) Uani 1 1 d . . . H8A1 H 0.5333 0.2860 0.8206 0.100 Uiso 1 1 calc R . . H8A2 H 0.4690 0.2456 0.8601 0.100 Uiso 1 1 calc R . . C9A C 0.3996(6) 0.3133(4) 0.7794(6) 0.090(3) Uani 1 1 d . . . H9A1 H 0.4068 0.3426 0.8267 0.135 Uiso 1 1 calc R . . H9A2 H 0.3402 0.2939 0.7672 0.135 Uiso 1 1 calc R . . H9A3 H 0.4040 0.3339 0.7267 0.135 Uiso 1 1 calc R . . C10A C 0.5302(4) 0.1326(3) 0.8344(4) 0.0484(16) Uani 1 1 d . . . H10A H 0.5461 0.1591 0.8864 0.058 Uiso 1 1 calc R . . H10B H 0.4661 0.1206 0.8234 0.058 Uiso 1 1 calc R . . C11A C 0.5885(4) 0.0765(4) 0.8564(4) 0.0617(19) Uani 1 1 d . . . H11A H 0.6532 0.0879 0.8724 0.074 Uiso 1 1 calc R . . H11B H 0.5753 0.0500 0.8044 0.074 Uiso 1 1 calc R . . C12A C 0.5696(5) 0.0427(3) 0.9324(5) 0.069(2) Uani 1 1 d . . . H12A H 0.6070 0.0064 0.9452 0.104 Uiso 1 1 calc R . . H12B H 0.5055 0.0315 0.9165 0.104 Uiso 1 1 calc R . . H12C H 0.5843 0.0686 0.9843 0.104 Uiso 1 1 calc R . . N1B N 0.5812(3) 0.1703(2) 1.2872(3) 0.0418(12) Uani 1 1 d . . . C1B C 0.6485(4) 0.1224(3) 1.2768(5) 0.0621(19) Uani 1 1 d . . . H1B1 H 0.7083 0.1419 1.2868 0.074 Uiso 1 1 calc R . . H1B2 H 0.6548 0.0922 1.3236 0.074 Uiso 1 1 calc R . . C2B C 0.6267(5) 0.0895(4) 1.1907(5) 0.073(2) Uani 1 1 d . . . H2B1 H 0.6306 0.1177 1.1441 0.088 Uiso 1 1 calc R . . H2B2 H 0.5640 0.0739 1.1755 0.088 Uiso 1 1 calc R . . C3B C 0.6933(5) 0.0368(4) 1.1960(5) 0.075(2) Uani 1 1 d . . . H3B1 H 0.6781 0.0160 1.1396 0.112 Uiso 1 1 calc R . . H3B2 H 0.6888 0.0087 1.2416 0.112 Uiso 1 1 calc R . . H3B3 H 0.7552 0.0524 1.2102 0.112 Uiso 1 1 calc R . . C4B C 0.5771(5) 0.2220(3) 1.2208(5) 0.0625(19) Uani 1 1 d . . . H4B1 H 0.6393 0.2378 1.2310 0.075 Uiso 1 1 calc R . . H4B2 H 0.5581 0.2045 1.1612 0.075 Uiso 1 1 calc R . . C5B C 0.5155(6) 0.2744(4) 1.2224(6) 0.089(3) Uani 1 1 d . . . H5B1 H 0.5383 0.2958 1.2789 0.107 Uiso 1 1 calc R . . H5B2 H 0.4541 0.2592 1.2178 0.107 Uiso 1 1 calc R . . C6B C 0.5100(7) 0.3185(4) 1.1474(6) 0.107(3) Uani 1 1 d . . . H6B1 H 0.4712 0.3525 1.1516 0.160 Uiso 1 1 calc R . . H6B2 H 0.4844 0.2980 1.0913 0.160 Uiso 1 1 calc R . . H6B3 H 0.5708 0.3332 1.1513 0.160 Uiso 1 1 calc R . . C7B C 0.4865(4) 0.1434(3) 1.2731(5) 0.0528(17) Uani 1 1 d . . . H7B1 H 0.4492 0.1739 1.2915 0.063 Uiso 1 1 calc R . . H7B2 H 0.4592 0.1372 1.2095 0.063 Uiso 1 1 calc R . . C8B C 0.4779(5) 0.0862(4) 1.3177(5) 0.069(2) Uani 1 1 d . . . H8B1 H 0.5037 0.0913 1.3817 0.083 Uiso 1 1 calc R . . H8B2 H 0.5127 0.0544 1.2987 0.083 Uiso 1 1 calc R . . C9B C 0.3768(4) 0.0667(3) 1.2961(5) 0.0633(19) Uani 1 1 d . . . H9B1 H 0.3728 0.0293 1.3270 0.095 Uiso 1 1 calc R . . H9B2 H 0.3518 0.0603 1.2329 0.095 Uiso 1 1 calc R . . H9B3 H 0.3423 0.0982 1.3148 0.095 Uiso 1 1 calc R . . C10B C 0.6146(5) 0.1945(3) 1.3840(4) 0.0600(18) Uani 1 1 d . . . H10C H 0.5699 0.2242 1.3915 0.072 Uiso 1 1 calc R . . H10D H 0.6145 0.1605 1.4239 0.072 Uiso 1 1 calc R . . C11B C 0.7064(6) 0.2233(4) 1.4128(5) 0.087(3) Uani 1 1 d . . . H11C H 0.7071 0.2590 1.3760 0.104 Uiso 1 1 calc R . . H11D H 0.7524 0.1945 1.4052 0.104 Uiso 1 1 calc R . . C12B C 0.7297(6) 0.2420(4) 1.5082(5) 0.084(3) Uani 1 1 d . . . H12D H 0.7901 0.2603 1.5263 0.126 Uiso 1 1 calc R . . H12E H 0.7290 0.2067 1.5445 0.126 Uiso 1 1 calc R . . H12F H 0.6850 0.2713 1.5154 0.126 Uiso 1 1 calc R . . C1C C 0.9138(8) -0.0264(6) 1.3873(7) 0.146(5) Uani 1 1 d . . . H1C1 H 0.9503 -0.0484 1.4387 0.220 Uiso 1 1 calc R . . H1C2 H 0.9515 -0.0158 1.3499 0.220 Uiso 1 1 calc R . . H1C3 H 0.8634 -0.0518 1.3544 0.220 Uiso 1 1 calc R . . C2C C 0.8784(8) 0.0278(7) 1.4152(7) 0.110(3) Uani 1 1 d . . . N1C N 0.8516(8) 0.0705(5) 1.4385(7) 0.144(4) 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 0.0409(4) 0.0444(5) 0.0483(5) 0.0014(4) 0.0160(3) 0.0009(4) Cu2 0.0372(4) 0.0459(5) 0.0490(5) -0.0042(4) 0.0150(3) -0.0020(3) Cu3 0.0441(4) 0.0406(4) 0.0452(4) -0.0007(4) 0.0159(4) -0.0025(3) Cu4 0.0391(4) 0.0399(4) 0.0483(5) -0.0002(4) 0.0127(3) -0.0029(3) S1 0.0335(8) 0.0435(9) 0.0405(9) 0.0022(7) 0.0121(6) -0.0045(7) S2 0.0354(8) 0.0424(9) 0.0416(9) -0.0001(7) 0.0125(7) -0.0050(7) C1 0.034(3) 0.029(3) 0.044(3) -0.005(3) 0.015(2) 0.003(2) C2 0.027(3) 0.043(4) 0.050(4) -0.004(3) 0.015(3) -0.001(2) C3 0.037(4) 0.052(4) 0.060(4) -0.004(3) 0.019(3) -0.002(3) C4 0.038(4) 0.051(4) 0.061(5) 0.002(4) 0.025(3) -0.003(3) N1 0.045(3) 0.083(5) 0.082(5) 0.001(4) 0.017(3) -0.013(3) N2 0.055(4) 0.100(6) 0.068(4) 0.014(4) 0.029(3) -0.009(3) S3 0.0392(8) 0.0377(8) 0.0477(9) -0.0020(7) 0.0172(7) 0.0001(7) S4 0.0387(8) 0.0371(8) 0.0519(9) -0.0013(7) 0.0155(7) -0.0024(6) C5 0.039(3) 0.036(3) 0.027(3) -0.005(2) 0.000(2) 0.000(3) C6 0.046(3) 0.037(4) 0.040(3) -0.001(3) 0.013(3) 0.008(3) C7 0.066(5) 0.043(4) 0.048(4) -0.005(3) 0.018(4) 0.015(3) C8 0.060(4) 0.039(4) 0.046(4) -0.011(3) 0.005(3) 0.009(3) N3 0.068(4) 0.086(5) 0.093(5) 0.005(4) 0.034(4) 0.025(4) N4 0.096(5) 0.045(4) 0.082(5) 0.003(3) 0.025(4) -0.001(4) S5 0.0415(8) 0.0439(9) 0.0406(9) -0.0059(7) 0.0117(7) -0.0017(7) S6 0.0373(8) 0.0429(9) 0.0409(9) 0.0017(7) 0.0093(7) 0.0024(7) C9 0.031(3) 0.047(3) 0.039(3) 0.005(3) 0.012(2) -0.008(3) C10 0.040(3) 0.057(4) 0.038(3) 0.003(3) 0.011(3) -0.007(3) C11 0.079(5) 0.080(6) 0.043(4) -0.012(4) 0.008(4) 0.008(4) C12 0.052(4) 0.071(5) 0.040(4) 0.008(3) 0.007(3) 0.003(4) N6 0.074(4) 0.091(5) 0.066(4) 0.018(4) 0.018(3) 0.011(4) N5 0.138(7) 0.121(7) 0.073(5) -0.044(5) 0.010(5) 0.016(6) N1A 0.036(3) 0.046(3) 0.035(3) 0.003(2) 0.013(2) 0.001(2) C1A 0.062(4) 0.063(5) 0.035(3) -0.002(3) 0.010(3) 0.005(4) C2A 0.078(5) 0.067(5) 0.058(5) -0.010(4) 0.010(4) -0.006(4) C3A 0.115(7) 0.060(5) 0.055(5) 0.000(4) -0.004(5) -0.007(5) C4A 0.045(4) 0.072(5) 0.064(5) 0.008(4) 0.020(3) -0.002(3) C5A 0.084(6) 0.121(8) 0.057(5) 0.017(5) 0.021(4) -0.034(5) C6A 0.090(6) 0.162(10) 0.088(7) 0.005(6) 0.019(5) -0.080(7) C7A 0.051(4) 0.051(4) 0.063(5) 0.009(4) 0.019(3) 0.012(3) C8A 0.106(7) 0.060(5) 0.085(6) 0.001(5) 0.028(5) 0.030(5) C9A 0.120(7) 0.064(5) 0.101(7) 0.016(5) 0.056(6) 0.033(5) C10A 0.043(3) 0.057(4) 0.045(4) 0.001(3) 0.013(3) 0.010(3) C11A 0.054(4) 0.080(5) 0.052(4) 0.010(4) 0.017(3) 0.018(4) C12A 0.075(5) 0.061(5) 0.071(5) 0.022(4) 0.022(4) 0.017(4) N1B 0.041(3) 0.037(3) 0.050(3) -0.005(2) 0.020(2) -0.007(2) C1B 0.050(4) 0.055(4) 0.089(6) -0.004(4) 0.032(4) -0.002(3) C2B 0.078(5) 0.076(5) 0.070(5) -0.005(5) 0.028(4) 0.011(4) C3B 0.078(5) 0.072(6) 0.081(6) -0.014(4) 0.036(4) 0.016(4) C4B 0.083(5) 0.049(4) 0.056(5) 0.007(4) 0.021(4) -0.003(4) C5B 0.111(7) 0.045(5) 0.117(8) 0.014(5) 0.043(6) 0.006(5) C6B 0.125(8) 0.060(6) 0.116(8) 0.029(6) 0.006(6) 0.004(5) C7B 0.048(4) 0.045(4) 0.070(5) -0.007(3) 0.025(3) -0.001(3) C8B 0.071(5) 0.060(5) 0.086(6) 0.004(4) 0.037(4) -0.007(4) C9B 0.060(4) 0.060(5) 0.072(5) -0.007(4) 0.023(4) -0.016(4) C10B 0.068(5) 0.057(4) 0.059(4) -0.001(3) 0.025(4) -0.014(4) C11B 0.104(6) 0.090(6) 0.068(6) -0.017(5) 0.028(5) -0.046(5) C12B 0.106(6) 0.075(6) 0.066(5) -0.009(4) 0.018(5) -0.037(5) C1C 0.160(11) 0.186(13) 0.084(8) -0.022(8) 0.024(7) 0.062(10) C2C 0.120(8) 0.134(11) 0.075(7) 0.013(7) 0.027(6) 0.035(8) N1C 0.191(10) 0.125(9) 0.123(8) 0.013(7) 0.058(7) 0.047(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S4 2.2445(17) 3_557 ? Cu1 S5 2.2473(17) . ? Cu1 S2 2.2548(16) . ? Cu1 Cu4 2.7647(11) . ? Cu1 Cu3 2.7808(11) . ? Cu1 Cu2 2.8651(11) . ? Cu2 S1 2.2311(16) . ? Cu2 S4 2.2440(17) 3_557 ? Cu2 S6 2.2467(16) 3_557 ? Cu2 Cu4 2.8226(11) 3_557 ? Cu2 Cu3 2.8458(11) 3_557 ? Cu3 S2 2.2456(17) . ? Cu3 S6 2.2476(17) . ? Cu3 S3 2.2587(17) . ? Cu3 Cu2 2.8458(11) 3_557 ? Cu3 Cu4 2.8534(11) 3_557 ? Cu4 S3 2.2376(17) 3_557 ? Cu4 S5 2.2436(17) . ? Cu4 S1 2.2535(17) 3_557 ? Cu4 Cu2 2.8226(11) 3_557 ? Cu4 Cu3 2.8534(11) 3_557 ? S1 C1 1.724(5) . ? S1 Cu4 2.2535(17) 3_557 ? S2 C1 1.762(6) . ? C1 C2 1.383(7) . ? C2 C4 1.410(9) . ? C2 C3 1.426(8) . ? C3 N1 1.132(7) . ? C4 N2 1.135(8) . ? S3 C5 1.747(6) . ? S3 Cu4 2.2376(17) 3_557 ? S4 C5 1.745(6) . ? S4 Cu2 2.2440(17) 3_557 ? S4 Cu1 2.2445(17) 3_557 ? C5 C6 1.366(7) . ? C6 C8 1.427(9) . ? C6 C7 1.443(9) . ? C7 N3 1.129(8) . ? C8 N4 1.125(8) . ? S5 C9 1.745(6) . ? S6 C9 1.754(6) . ? S6 Cu2 2.2467(16) 3_557 ? C9 C10 1.366(8) . ? C10 C11 1.410(10) . ? C10 C12 1.429(9) . ? C11 N5 1.132(9) . ? C12 N6 1.133(8) . ? N1A C4A 1.506(7) . ? N1A C10A 1.522(7) . ? N1A C1A 1.527(7) . ? N1A C7A 1.527(7) . ? C1A C2A 1.489(9) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A C3A 1.494(10) . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A H3A1 0.9600 . ? C3A H3A2 0.9600 . ? C3A H3A3 0.9600 . ? C4A C5A 1.478(9) . ? C4A H4A1 0.9700 . ? C4A H4A2 0.9700 . ? C5A C6A 1.509(10) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C7A C8A 1.480(10) . ? C7A H7A1 0.9700 . ? C7A H7A2 0.9700 . ? C8A C9A 1.485(10) . ? C8A H8A1 0.9700 . ? C8A H8A2 0.9700 . ? C9A H9A1 0.9600 . ? C9A H9A2 0.9600 . ? C9A H9A3 0.9600 . ? C10A C11A 1.488(9) . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? C11A C12A 1.499(9) . ? C11A H11A 0.9700 . ? C11A H11B 0.9700 . ? C12A H12A 0.9600 . ? C12A H12B 0.9600 . ? C12A H12C 0.9600 . ? N1B C1B 1.502(8) . ? N1B C7B 1.505(7) . ? N1B C4B 1.523(8) . ? N1B C10B 1.544(8) . ? C1B C2B 1.477(9) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B C3B 1.515(9) . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B H3B1 0.9600 . ? C3B H3B2 0.9600 . ? C3B H3B3 0.9600 . ? C4B C5B 1.482(10) . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? C5B C6B 1.502(11) . ? C5B H5B1 0.9700 . ? C5B H5B2 0.9700 . ? C6B H6B1 0.9600 . ? C6B H6B2 0.9600 . ? C6B H6B3 0.9600 . ? C7B C8B 1.453(9) . ? C7B H7B1 0.9700 . ? C7B H7B2 0.9700 . ? C8B C9B 1.528(8) . ? C8B H8B1 0.9700 . ? C8B H8B2 0.9700 . ? C9B H9B1 0.9600 . ? C9B H9B2 0.9600 . ? C9B H9B3 0.9600 . ? C10B C11B 1.469(9) . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? C11B C12B 1.490(10) . ? C11B H11C 0.9700 . ? C11B H11D 0.9700 . ? C12B H12D 0.9600 . ? C12B H12E 0.9600 . ? C12B H12F 0.9600 . ? C1C C2C 1.420(15) . ? C1C H1C1 0.9600 . ? C1C H1C2 0.9600 . ? C1C H1C3 0.9600 . ? C2C N1C 1.118(13) . ? 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 S4 Cu1 S5 119.93(6) 3_557 . ? S4 Cu1 S2 116.82(6) 3_557 . ? S5 Cu1 S2 118.63(6) . . ? S4 Cu1 Cu4 93.53(5) 3_557 . ? S5 Cu1 Cu4 51.94(4) . . ? S2 Cu1 Cu4 142.40(5) . . ? S4 Cu1 Cu3 140.78(6) 3_557 . ? S5 Cu1 Cu3 92.94(5) . . ? S2 Cu1 Cu3 51.69(4) . . ? Cu4 Cu1 Cu3 90.83(3) . . ? S4 Cu1 Cu2 50.33(5) 3_557 . ? S5 Cu1 Cu2 142.36(5) . . ? S2 Cu1 Cu2 92.53(5) . . ? Cu4 Cu1 Cu2 90.58(3) . . ? Cu3 Cu1 Cu2 90.71(3) . . ? S1 Cu2 S4 118.67(6) . 3_557 ? S1 Cu2 S6 119.82(6) . 3_557 ? S4 Cu2 S6 118.19(6) 3_557 3_557 ? S1 Cu2 Cu4 51.35(4) . 3_557 ? S4 Cu2 Cu4 139.26(5) 3_557 3_557 ? S6 Cu2 Cu4 93.88(5) 3_557 3_557 ? S1 Cu2 Cu3 139.53(5) . 3_557 ? S4 Cu2 Cu3 93.28(5) 3_557 3_557 ? S6 Cu2 Cu3 50.73(4) 3_557 3_557 ? Cu4 Cu2 Cu3 88.33(3) 3_557 3_557 ? S1 Cu2 Cu1 93.00(5) . . ? S4 Cu2 Cu1 50.34(5) 3_557 . ? S6 Cu2 Cu1 139.59(5) 3_557 . ? Cu4 Cu2 Cu1 89.03(3) 3_557 . ? Cu3 Cu2 Cu1 89.17(3) 3_557 . ? S2 Cu3 S6 120.82(7) . . ? S2 Cu3 S3 117.92(6) . . ? S6 Cu3 S3 117.12(7) . . ? S2 Cu3 Cu1 51.99(4) . . ? S6 Cu3 Cu1 94.77(5) . . ? S3 Cu3 Cu1 140.21(5) . . ? S2 Cu3 Cu2 141.87(5) . 3_557 ? S6 Cu3 Cu2 50.70(4) . 3_557 ? S3 Cu3 Cu2 92.59(5) . 3_557 ? Cu1 Cu3 Cu2 90.02(3) . 3_557 ? S2 Cu3 Cu4 93.45(5) . 3_557 ? S6 Cu3 Cu4 139.48(5) . 3_557 ? S3 Cu3 Cu4 50.28(4) . 3_557 ? Cu1 Cu3 Cu4 90.10(3) . 3_557 ? Cu2 Cu3 Cu4 89.19(3) 3_557 3_557 ? S3 Cu4 S5 120.75(7) 3_557 . ? S3 Cu4 S1 117.17(6) 3_557 3_557 ? S5 Cu4 S1 117.46(6) . 3_557 ? S3 Cu4 Cu1 94.44(5) 3_557 . ? S5 Cu4 Cu1 52.06(5) . . ? S1 Cu4 Cu1 141.29(5) 3_557 . ? S3 Cu4 Cu2 140.69(5) 3_557 3_557 ? S5 Cu4 Cu2 92.76(5) . 3_557 ? S1 Cu4 Cu2 50.64(4) 3_557 3_557 ? Cu1 Cu4 Cu2 90.83(3) . 3_557 ? S3 Cu4 Cu3 50.94(4) 3_557 3_557 ? S5 Cu4 Cu3 143.00(5) . 3_557 ? S1 Cu4 Cu3 92.40(5) 3_557 3_557 ? Cu1 Cu4 Cu3 91.04(3) . 3_557 ? Cu2 Cu4 Cu3 90.11(3) 3_557 3_557 ? C1 S1 Cu2 109.39(18) . . ? C1 S1 Cu4 108.7(2) . 3_557 ? Cu2 S1 Cu4 78.01(5) . 3_557 ? C1 S2 Cu3 107.48(19) . . ? C1 S2 Cu1 109.05(18) . . ? Cu3 S2 Cu1 76.32(5) . . ? C2 C1 S1 118.3(4) . . ? C2 C1 S2 117.4(4) . . ? S1 C1 S2 124.3(3) . . ? C1 C2 C4 121.6(5) . . ? C1 C2 C3 122.2(6) . . ? C4 C2 C3 116.1(5) . . ? N1 C3 C2 176.0(7) . . ? N2 C4 C2 176.2(7) . . ? C5 S3 Cu4 110.44(18) . 3_557 ? C5 S3 Cu3 104.80(19) . . ? Cu4 S3 Cu3 78.78(6) 3_557 . ? C5 S4 Cu2 104.45(18) . 3_557 ? C5 S4 Cu1 111.06(19) . 3_557 ? Cu2 S4 Cu1 79.33(6) 3_557 3_557 ? C6 C5 S4 118.0(4) . . ? C6 C5 S3 118.5(4) . . ? S4 C5 S3 123.5(3) . . ? C5 C6 C8 120.5(5) . . ? C5 C6 C7 121.9(6) . . ? C8 C6 C7 117.6(5) . . ? N3 C7 C6 179.2(8) . . ? N4 C8 C6 178.7(8) . . ? C9 S5 Cu4 108.6(2) . . ? C9 S5 Cu1 109.73(19) . . ? Cu4 S5 Cu1 75.99(6) . . ? C9 S6 Cu2 106.81(18) . 3_557 ? C9 S6 Cu3 107.7(2) . . ? Cu2 S6 Cu3 78.57(6) 3_557 . ? C10 C9 S5 118.4(5) . . ? C10 C9 S6 118.1(5) . . ? S5 C9 S6 123.6(3) . . ? C9 C10 C11 121.4(6) . . ? C9 C10 C12 122.4(6) . . ? C11 C10 C12 116.1(6) . . ? N5 C11 C10 179.9(11) . . ? N6 C12 C10 176.9(8) . . ? C4A N1A C10A 109.1(4) . . ? C4A N1A C1A 109.2(5) . . ? C10A N1A C1A 110.9(5) . . ? C4A N1A C7A 110.2(5) . . ? C10A N1A C7A 109.1(4) . . ? C1A N1A C7A 108.3(5) . . ? C2A C1A N1A 117.2(5) . . ? C2A C1A H1A1 108.0 . . ? N1A C1A H1A1 108.0 . . ? C2A C1A H1A2 108.0 . . ? N1A C1A H1A2 108.0 . . ? H1A1 C1A H1A2 107.2 . . ? C1A C2A C3A 111.3(6) . . ? C1A C2A H2A1 109.4 . . ? C3A C2A H2A1 109.4 . . ? C1A C2A H2A2 109.4 . . ? C3A C2A H2A2 109.4 . . ? H2A1 C2A H2A2 108.0 . . ? C2A C3A H3A1 109.5 . . ? C2A C3A H3A2 109.5 . . ? H3A1 C3A H3A2 109.5 . . ? C2A C3A H3A3 109.5 . . ? H3A1 C3A H3A3 109.5 . . ? H3A2 C3A H3A3 109.5 . . ? C5A C4A N1A 117.1(6) . . ? C5A C4A H4A1 108.0 . . ? N1A C4A H4A1 108.0 . . ? C5A C4A H4A2 108.0 . . ? N1A C4A H4A2 108.0 . . ? H4A1 C4A H4A2 107.3 . . ? C4A C5A C6A 112.4(7) . . ? C4A C5A H5A1 109.1 . . ? C6A C5A H5A1 109.1 . . ? C4A C5A H5A2 109.1 . . ? C6A C5A H5A2 109.1 . . ? H5A1 C5A H5A2 107.9 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C8A C7A N1A 116.3(6) . . ? C8A C7A H7A1 108.2 . . ? N1A C7A H7A1 108.2 . . ? C8A C7A H7A2 108.2 . . ? N1A C7A H7A2 108.2 . . ? H7A1 C7A H7A2 107.4 . . ? C7A C8A C9A 111.2(7) . . ? C7A C8A H8A1 109.4 . . ? C9A C8A H8A1 109.4 . . ? C7A C8A H8A2 109.4 . . ? C9A C8A H8A2 109.4 . . ? H8A1 C8A H8A2 108.0 . . ? C8A C9A H9A1 109.5 . . ? C8A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C8A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C11A C10A N1A 116.3(5) . . ? C11A C10A H10A 108.2 . . ? N1A C10A H10A 108.2 . . ? C11A C10A H10B 108.2 . . ? N1A C10A H10B 108.2 . . ? H10A C10A H10B 107.4 . . ? C10A C11A C12A 110.5(5) . . ? C10A C11A H11A 109.6 . . ? C12A C11A H11A 109.6 . . ? C10A C11A H11B 109.6 . . ? C12A C11A H11B 109.6 . . ? H11A C11A H11B 108.1 . . ? C11A C12A H12A 109.5 . . ? C11A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? C11A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? C1B N1B C7B 111.2(5) . . ? C1B N1B C4B 109.4(5) . . ? C7B N1B C4B 110.1(5) . . ? C1B N1B C10B 108.0(5) . . ? C7B N1B C10B 107.4(5) . . ? C4B N1B C10B 110.7(5) . . ? C2B C1B N1B 117.5(6) . . ? C2B C1B H1B1 107.9 . . ? N1B C1B H1B1 107.9 . . ? C2B C1B H1B2 107.9 . . ? N1B C1B H1B2 107.9 . . ? H1B1 C1B H1B2 107.2 . . ? C1B C2B C3B 110.6(6) . . ? C1B C2B H2B1 109.5 . . ? C3B C2B H2B1 109.5 . . ? C1B C2B H2B2 109.5 . . ? C3B C2B H2B2 109.5 . . ? H2B1 C2B H2B2 108.1 . . ? C2B C3B H3B1 109.5 . . ? C2B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 109.5 . . ? C2B C3B H3B3 109.5 . . ? H3B1 C3B H3B3 109.5 . . ? H3B2 C3B H3B3 109.5 . . ? C5B C4B N1B 117.3(6) . . ? C5B C4B H4B1 108.0 . . ? N1B C4B H4B1 108.0 . . ? C5B C4B H4B2 108.0 . . ? N1B C4B H4B2 108.0 . . ? H4B1 C4B H4B2 107.2 . . ? C4B C5B C6B 111.7(8) . . ? C4B C5B H5B1 109.3 . . ? C6B C5B H5B1 109.3 . . ? C4B C5B H5B2 109.3 . . ? C6B C5B H5B2 109.3 . . ? H5B1 C5B H5B2 107.9 . . ? C5B C6B H6B1 109.5 . . ? C5B C6B H6B2 109.5 . . ? H6B1 C6B H6B2 109.5 . . ? C5B C6B H6B3 109.5 . . ? H6B1 C6B H6B3 109.5 . . ? H6B2 C6B H6B3 109.5 . . ? C8B C7B N1B 118.7(5) . . ? C8B C7B H7B1 107.6 . . ? N1B C7B H7B1 107.6 . . ? C8B C7B H7B2 107.6 . . ? N1B C7B H7B2 107.6 . . ? H7B1 C7B H7B2 107.1 . . ? C7B C8B C9B 111.0(6) . . ? C7B C8B H8B1 109.4 . . ? C9B C8B H8B1 109.4 . . ? C7B C8B H8B2 109.4 . . ? C9B C8B H8B2 109.4 . . ? H8B1 C8B H8B2 108.0 . . ? C8B C9B H9B1 109.5 . . ? C8B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C8B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C11B C10B N1B 117.0(6) . . ? C11B C10B H10C 108.0 . . ? N1B C10B H10C 108.0 . . ? C11B C10B H10D 108.0 . . ? N1B C10B H10D 108.0 . . ? H10C C10B H10D 107.3 . . ? C10B C11B C12B 110.4(7) . . ? C10B C11B H11C 109.6 . . ? C12B C11B H11C 109.6 . . ? C10B C11B H11D 109.6 . . ? C12B C11B H11D 109.6 . . ? H11C C11B H11D 108.1 . . ? C11B C12B H12D 109.5 . . ? C11B C12B H12E 109.5 . . ? H12D C12B H12E 109.5 . . ? C11B C12B H12F 109.5 . . ? H12D C12B H12F 109.5 . . ? H12E C12B H12F 109.5 . . ? C2C C1C H1C1 109.5 . . ? C2C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? C2C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? N1C C2C C1C 178.8(14) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.84 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.301 _refine_diff_density_min -0.249 _refine_diff_density_rms 0.050 #===END data_2 _publ_requested_journal 'Journal of Materials Chemistry' _publ_contact_author_name ; Sandrine Perruchas, Kamal Boubekeur and Pascale Auban-Senzier ; _publ_contact_author_address ; Institut des Materiaux Jean Rouxel 2 rue de la Houssiniere BP 32229 44322 nantes Cedex 3 FRANCE present address for S. Perruchas: Baker laboratories department of chemistry Cornell University Ithaca NY 14853 USA ; _publ_contact_author_email 'sp353@cornell.edu' _publ_section_title ; Radical cation salts of TTF derivatives incorporating the maleonitriledithiolate copper cluster anion [Cu8(i-mnt)6]4- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis-bisethylenedithiotetrathiafulvalenium-hexa-iso-maleonitrile- octa-cuprate(I)-tetrakis-dichloromethane solvate ; _chemical_name_common '(BEDT-TTF)6[Cu8(i-mnt)6](CH2Cl2)4' _chemical_formula_moiety 'C24 Cu8 N12 S12, 6(C10 H8 S8), 4(C H2 Cl2)' _chemical_formula_sum 'C44 H28 Cl4 Cu4 N6 S30' _chemical_formula_weight 1998.48 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' '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8019(11) _cell_length_b 16.5389(14) _cell_length_c 17.5845(17) _cell_angle_alpha 95.819(11) _cell_angle_beta 91.382(11) _cell_angle_gamma 109.792(10) _cell_volume 3478.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8002 _cell_measurement_theta_min 2 _cell_measurement_theta_max 25.9 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.908 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1996 _exptl_absorpt_coefficient_mu 2.302 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2151 _exptl_absorpt_correction_T_max 0.6531 _exptl_absorpt_process_details 'stoe IPDS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe IPDS' _diffrn_measurement_method 'oscillation phi. incr. = 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35512 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.89 _reflns_number_total 12562 _reflns_number_gt 9868 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1498P)^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 12562 _refine_ls_number_parameters 794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0920 _refine_ls_R_factor_gt 0.0828 _refine_ls_wR_factor_ref 0.2049 _refine_ls_wR_factor_gt 0.1957 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 1.09819(6) 0.90744(4) 0.93829(3) 0.03701(19) Uani 1 1 d . . . Cu2 Cu 0.94882(6) 0.97067(4) 0.86126(4) 0.03586(18) Uani 1 1 d . . . Cu3 Cu 0.95386(6) 0.86801(4) 1.05515(3) 0.03636(18) Uani 1 1 d . . . Cu4 Cu 1.21685(8) 1.08435(5) 1.01889(4) 0.0453(2) Uani 1 1 d . . . S1D S 1.25284(12) 0.95968(8) 1.01625(7) 0.0324(3) Uani 1 1 d . . . S2D S 1.09361(12) 0.90811(8) 1.14650(7) 0.0330(3) Uani 1 1 d . . . S3D S 0.80126(12) 0.84983(8) 0.86719(7) 0.0346(3) Uani 1 1 d . . . S4D S 0.96256(13) 0.78107(8) 0.95028(7) 0.0366(3) Uani 1 1 d . . . S5D S 0.78282(12) 0.85725(8) 1.09158(7) 0.0322(3) Uani 1 1 d . . . S6D S 0.89010(12) 1.04026(8) 1.17655(7) 0.0320(3) Uani 1 1 d . . . C1D C 1.2238(5) 0.9290(3) 1.1082(3) 0.0301(11) Uani 1 1 d . . . C2D C 1.3094(5) 0.9206(4) 1.1521(3) 0.0373(12) Uani 1 1 d . . . C3D C 1.4195(6) 0.9423(4) 1.1273(3) 0.0415(13) Uani 1 1 d . . . C4D C 1.2891(6) 0.8878(5) 1.2246(3) 0.0494(16) Uani 1 1 d . . . N2D N 1.5079(6) 0.9600(4) 1.1092(4) 0.0628(16) Uani 1 1 d . . . N1D N 1.2775(7) 0.8599(6) 1.2814(4) 0.083(2) Uani 1 1 d . . . C5D C 0.8541(5) 0.7681(3) 0.8820(3) 0.0335(12) Uani 1 1 d . . . C6D C 0.8095(5) 0.6890(4) 0.8376(3) 0.0403(13) Uani 1 1 d . . . C7D C 0.8452(6) 0.6178(4) 0.8471(3) 0.0482(16) Uani 1 1 d . . . C8D C 0.7224(6) 0.6750(4) 0.7795(3) 0.0468(15) Uani 1 1 d . . . N3D N 0.8756(6) 0.5613(4) 0.8566(4) 0.0647(17) Uani 1 1 d . . . N4D N 0.6517(6) 0.6631(4) 0.7347(3) 0.0639(16) Uani 1 1 d . . . C9D C 0.7846(5) 0.9399(3) 1.1629(3) 0.0307(11) Uani 1 1 d . . . C10D C 0.6977(5) 0.9236(4) 1.2102(3) 0.0360(12) Uani 1 1 d . . . C11D C 0.6917(6) 0.9869(4) 1.2698(3) 0.0445(14) Uani 1 1 d . . . C12D C 0.6055(5) 0.8432(4) 1.2018(3) 0.0423(13) Uani 1 1 d . . . N5D N 0.5327(6) 0.7792(4) 1.1978(4) 0.0612(15) Uani 1 1 d . . . N6D N 0.6882(6) 1.0359(5) 1.3204(4) 0.0702(19) Uani 1 1 d . . . S1A S 1.53210(16) 0.81172(10) 0.98376(10) 0.0524(4) Uani 1 1 d . . . S2A S 1.3859(2) 0.68043(15) 0.81717(11) 0.0755(7) Uani 1 1 d . . . S3A S 1.61291(14) 0.66796(9) 0.99895(8) 0.0424(3) Uani 1 1 d . . . S4A S 1.48578(15) 0.55711(9) 0.86493(8) 0.0456(4) Uani 1 1 d . . . S5A S 1.73107(15) 0.53111(10) 1.02647(9) 0.0482(4) Uani 1 1 d . . . S6A S 1.60545(14) 0.41666(9) 0.89387(8) 0.0407(3) Uani 1 1 d . . . S7A S 1.8652(2) 0.42084(15) 1.05799(12) 0.0709(6) Uani 1 1 d . . . S8A S 1.71743(17) 0.28729(10) 0.90301(10) 0.0539(4) Uani 1 1 d . . . C1A C 1.4502(13) 0.8348(7) 0.9128(6) 0.121(5) Uani 1 1 d . . . H1A1 H 1.4173 0.8743 0.9381 0.145 Uiso 1 1 calc R . . H1A2 H 1.5013 0.8669 0.8777 0.145 Uiso 1 1 calc R . . C2A C 1.3653(12) 0.7713(8) 0.8681(7) 0.111(4) Uani 1 1 d . . . H2A1 H 1.3382 0.8000 0.8308 0.133 Uiso 1 1 calc R . . H2A2 H 1.3052 0.7491 0.9013 0.133 Uiso 1 1 calc R . . C3A C 1.5314(5) 0.7102(4) 0.9463(3) 0.0392(12) Uani 1 1 d . . . C4A C 1.4730(6) 0.6579(4) 0.8832(3) 0.0471(15) Uani 1 1 d . . . C5A C 1.5800(6) 0.5714(4) 0.9402(3) 0.0401(13) Uani 1 1 d . . . C6A C 1.6323(5) 0.5122(3) 0.9516(3) 0.0382(12) Uani 1 1 d . . . C7A C 1.7597(6) 0.4365(4) 1.0039(3) 0.0440(13) Uani 1 1 d . . . C8A C 1.7021(6) 0.3829(4) 0.9418(3) 0.0410(13) Uani 1 1 d . . . C9A C 1.9229(9) 0.3732(7) 0.9799(8) 0.111(4) Uani 1 1 d . . . H9A1 H 1.9558 0.4181 0.9475 0.133 Uiso 1 1 calc R . . H9A2 H 1.9833 0.3584 1.0019 0.133 Uiso 1 1 calc R . . C10A C 1.8579(10) 0.3030(9) 0.9341(7) 0.108(4) Uani 1 1 d . . . H10A H 1.8553 0.2532 0.9596 0.130 Uiso 1 1 calc R . . H10B H 1.8973 0.2999 0.8881 0.130 Uiso 1 1 calc R . . S1B S 1.63308(16) 0.44308(12) 0.68515(11) 0.0577(5) Uani 1 1 d . . . S2B S 1.89073(16) 0.42223(12) 0.64568(11) 0.0583(5) Uani 1 1 d . . . S3B S 1.68524(14) 0.56354(10) 0.56726(9) 0.0450(4) Uani 1 1 d . . . S4B S 1.90269(14) 0.54850(10) 0.53825(9) 0.0444(4) Uani 1 1 d . . . S5B S 1.74864(15) 0.73247(10) 0.47545(10) 0.0472(4) Uani 1 1 d . . . S6B S 1.96417(14) 0.71507(10) 0.44526(9) 0.0454(4) Uani 1 1 d . . . S7B S 1.80476(19) 0.90789(13) 0.42817(14) 0.0715(6) Uani 1 1 d . . . S8B S 2.06028(18) 0.88407(15) 0.38756(15) 0.0752(6) Uani 1 1 d . . . C1B C 1.6794(6) 0.3524(4) 0.6958(4) 0.0484(15) Uani 1 1 d . . . H1B1 H 1.6356 0.3184 0.7332 0.058 Uiso 1 1 calc R . . H1B2 H 1.6653 0.3158 0.6473 0.058 Uiso 1 1 calc R . . C2B C 1.7987(7) 0.3776(4) 0.7203(4) 0.0536(17) Uani 1 1 d . . . H2B1 H 1.8133 0.3272 0.7348 0.064 Uiso 1 1 calc R . . H2B2 H 1.8153 0.4203 0.7650 0.064 Uiso 1 1 calc R . . C3B C 1.7288(5) 0.4970(4) 0.6218(3) 0.0408(13) Uani 1 1 d . . . C4B C 1.8256(5) 0.4884(4) 0.6083(3) 0.0404(13) Uani 1 1 d . . . C5B C 1.8122(5) 0.6043(4) 0.5253(3) 0.0366(12) Uani 1 1 d . . . C6B C 1.8377(5) 0.6745(4) 0.4862(3) 0.0365(12) Uani 1 1 d . . . C7B C 1.8501(6) 0.8215(4) 0.4433(3) 0.0424(14) Uani 1 1 d . . . C8B C 1.9477(6) 0.8133(4) 0.4286(3) 0.0440(14) Uani 1 1 d . . . C9B C 1.9256(7) 0.9844(5) 0.3932(5) 0.067(2) Uani 1 1 d . . . H9B1 H 1.9020 1.0243 0.3664 0.081 Uiso 1 1 calc R . . H9B2 H 1.9746 1.0177 0.4368 0.081 Uiso 1 1 calc R . . C10B C 1.9890(7) 0.9457(5) 0.3416(4) 0.066(2) Uani 1 1 d . . . H10C H 2.0435 0.9916 0.3187 0.079 Uiso 1 1 calc R . . H10D H 1.9385 0.9080 0.3006 0.079 Uiso 1 1 calc R . . S1C S 1.73601(17) 0.18824(12) 0.52932(12) 0.0636(5) Uani 1 1 d . . . S2C S 1.47300(17) 0.20095(16) 0.55399(14) 0.0764(7) Uani 1 1 d . . . S3C S 1.76321(15) 0.32855(11) 0.43329(10) 0.0495(4) Uani 1 1 d . . . S4C S 1.54275(15) 0.33977(12) 0.45558(11) 0.0566(5) Uani 1 1 d . . . S5C S 1.82336(14) 0.48282(10) 0.33146(9) 0.0453(4) Uani 1 1 d . . . S6C S 1.60762(15) 0.50428(11) 0.35438(10) 0.0519(4) Uani 1 1 d . . . S7C S 1.89422(19) 0.60896(13) 0.22084(12) 0.0667(6) Uani 1 1 d . . . S8C S 1.64656(17) 0.64378(12) 0.25329(13) 0.0649(5) Uani 1 1 d . . . C1C C 1.6089(8) 0.0990(5) 0.5378(5) 0.068(2) Uani 1 1 d . . . H1C1 H 1.5729 0.0762 0.4871 0.081 Uiso 1 1 calc R . . H1C2 H 1.6272 0.0532 0.5590 0.081 Uiso 1 1 calc R . . C2C C 1.5314(7) 0.1240(5) 0.5862(5) 0.067(2) Uani 1 1 d . . . H2C1 H 1.5693 0.1478 0.6362 0.080 Uiso 1 1 calc R . . H2C2 H 1.4703 0.0719 0.5933 0.080 Uiso 1 1 calc R . . C3C C 1.6780(5) 0.2576(4) 0.4906(3) 0.0409(13) Uani 1 1 d . . . C4C C 1.5771(6) 0.2626(4) 0.5008(3) 0.0464(14) Uani 1 1 d . . . C5C C 1.6697(6) 0.3802(4) 0.4150(3) 0.0436(13) Uani 1 1 d . . . C6C C 1.6949(6) 0.4467(4) 0.3712(3) 0.0424(13) Uani 1 1 d . . . C7C C 1.7902(6) 0.5568(4) 0.2800(3) 0.0454(14) Uani 1 1 d . . . C8C C 1.6938(6) 0.5680(4) 0.2917(3) 0.0441(14) Uani 1 1 d . . . C9C C 1.8598(8) 0.7028(5) 0.2022(5) 0.073(2) Uani 1 1 d . . . H9C1 H 1.9283 0.7521 0.2068 0.088 Uiso 1 1 calc R . . H9C2 H 1.8311 0.6937 0.1492 0.088 Uiso 1 1 calc R . . C10C C 1.7831(8) 0.7254(5) 0.2479(5) 0.066(2) Uani 1 1 d . . . H10E H 1.7721 0.7753 0.2292 0.079 Uiso 1 1 calc R . . H10F H 1.8169 0.7435 0.2995 0.079 Uiso 1 1 calc R . . C1E C 1.3692(12) 0.1420(10) 0.3036(7) 0.118(4) Uani 1 1 d . . . H1E1 H 1.3878 0.2043 0.3102 0.141 Uiso 1 1 calc R . . H1E2 H 1.3339 0.1203 0.2527 0.141 Uiso 1 1 calc R . . Cl1E Cl 1.4934(3) 0.1171(2) 0.31195(17) 0.1091(10) Uani 1 1 d . . . Cl2E Cl 1.2789(4) 0.0982(3) 0.3693(2) 0.1451(14) Uani 1 1 d . . . C1F C 1.0638(10) 0.7777(6) 0.6721(6) 0.092(3) Uani 1 1 d . . . H1F1 H 1.1231 0.8323 0.6877 0.111 Uiso 1 1 calc R . . H1F2 H 1.0778 0.7563 0.6214 0.111 Uiso 1 1 calc R . . Cl2F Cl 0.9390(3) 0.79640(18) 0.66714(15) 0.0928(7) Uani 1 1 d . . . Cl1F Cl 1.0687(4) 0.7044(3) 0.7351(2) 0.1350(14) 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 0.0404(5) 0.0281(3) 0.0426(3) 0.0075(3) -0.0007(3) 0.0111(3) Cu2 0.0341(5) 0.0240(3) 0.0507(4) 0.0055(3) 0.0015(3) 0.0114(3) Cu3 0.0372(5) 0.0280(3) 0.0444(3) 0.0029(2) 0.0003(3) 0.0122(3) Cu4 0.0727(6) 0.0305(4) 0.0415(3) 0.0058(3) 0.0008(3) 0.0289(4) S1D 0.0356(8) 0.0260(6) 0.0405(6) 0.0084(5) 0.0014(5) 0.0159(6) S2D 0.0357(8) 0.0276(6) 0.0405(6) 0.0105(5) 0.0023(5) 0.0151(6) S3D 0.0368(9) 0.0236(6) 0.0411(6) -0.0002(5) -0.0022(5) 0.0087(6) S4D 0.0441(9) 0.0190(6) 0.0467(6) 0.0011(5) -0.0015(5) 0.0120(6) S5D 0.0339(8) 0.0208(6) 0.0409(6) 0.0054(4) 0.0001(5) 0.0078(5) S6D 0.0330(8) 0.0242(6) 0.0381(6) 0.0029(4) 0.0011(5) 0.0090(5) C1D 0.037(3) 0.019(2) 0.040(2) 0.0058(18) 0.000(2) 0.016(2) C2D 0.040(4) 0.030(3) 0.046(3) 0.008(2) -0.004(2) 0.016(3) C3D 0.039(4) 0.041(3) 0.052(3) 0.010(2) -0.004(2) 0.023(3) C4D 0.050(5) 0.061(4) 0.049(3) 0.014(3) -0.003(3) 0.032(4) N2D 0.047(5) 0.061(4) 0.091(4) 0.020(3) 0.005(3) 0.029(3) N1D 0.085(6) 0.130(7) 0.065(4) 0.050(4) 0.016(3) 0.064(5) C5D 0.039(4) 0.015(2) 0.041(2) 0.0006(18) 0.007(2) 0.003(2) C6D 0.042(4) 0.027(3) 0.046(3) -0.003(2) 0.002(2) 0.006(3) C7D 0.055(5) 0.023(3) 0.058(3) -0.005(2) 0.010(3) 0.004(3) C8D 0.049(5) 0.026(3) 0.056(3) -0.010(2) 0.005(3) 0.004(3) N3D 0.079(5) 0.027(3) 0.087(4) -0.007(3) -0.002(3) 0.020(3) N4D 0.060(5) 0.054(4) 0.067(3) -0.014(3) -0.010(3) 0.013(3) C9D 0.034(3) 0.025(2) 0.038(2) 0.0078(18) -0.0002(19) 0.015(2) C10D 0.034(4) 0.032(3) 0.046(3) 0.010(2) 0.002(2) 0.014(2) C11D 0.037(4) 0.053(4) 0.052(3) 0.013(3) 0.009(2) 0.024(3) C12D 0.031(4) 0.038(3) 0.065(3) 0.018(3) 0.010(3) 0.017(3) N5D 0.041(4) 0.049(3) 0.095(4) 0.025(3) 0.010(3) 0.011(3) N6D 0.068(5) 0.071(4) 0.075(4) -0.006(3) 0.021(3) 0.031(4) S1A 0.0501(12) 0.0286(7) 0.0796(10) -0.0054(7) 0.0001(8) 0.0187(7) S2A 0.100(2) 0.0653(13) 0.0744(11) -0.0090(9) -0.0285(11) 0.0521(13) S3A 0.0422(10) 0.0254(6) 0.0587(8) -0.0057(5) -0.0037(6) 0.0136(6) S4A 0.0564(11) 0.0305(7) 0.0503(7) -0.0032(5) -0.0042(6) 0.0183(7) S5A 0.0457(11) 0.0347(7) 0.0628(8) -0.0072(6) -0.0080(7) 0.0163(7) S6A 0.0480(10) 0.0257(6) 0.0502(7) -0.0011(5) 0.0000(6) 0.0168(6) S7A 0.0601(15) 0.0711(13) 0.0872(12) 0.0120(10) -0.0170(10) 0.0306(12) S8A 0.0527(12) 0.0330(8) 0.0816(10) -0.0001(7) 0.0036(8) 0.0240(8) C1A 0.185(14) 0.071(6) 0.130(8) -0.018(6) -0.070(8) 0.089(9) C2A 0.133(12) 0.091(8) 0.134(8) -0.020(6) -0.050(7) 0.084(8) C3A 0.036(4) 0.027(3) 0.056(3) 0.004(2) 0.007(2) 0.013(2) C4A 0.053(5) 0.035(3) 0.056(3) 0.003(2) -0.002(3) 0.020(3) C5A 0.045(4) 0.026(3) 0.050(3) 0.000(2) 0.005(2) 0.013(3) C6A 0.036(4) 0.024(2) 0.052(3) -0.002(2) 0.003(2) 0.008(2) C7A 0.035(4) 0.035(3) 0.062(3) 0.004(2) 0.001(2) 0.013(3) C8A 0.041(4) 0.029(3) 0.055(3) 0.008(2) 0.003(2) 0.014(3) C9A 0.055(7) 0.076(7) 0.202(11) -0.044(7) -0.023(7) 0.043(6) C10A 0.071(9) 0.129(11) 0.133(8) -0.025(7) -0.001(6) 0.056(8) S1B 0.0504(12) 0.0595(10) 0.0817(10) 0.0397(9) 0.0283(9) 0.0322(9) S2B 0.0415(11) 0.0546(10) 0.0940(12) 0.0383(9) 0.0113(8) 0.0272(9) S3B 0.0392(10) 0.0398(8) 0.0687(9) 0.0233(7) 0.0171(7) 0.0242(7) S4B 0.0349(9) 0.0346(7) 0.0723(9) 0.0199(6) 0.0145(7) 0.0183(7) S5B 0.0388(10) 0.0348(7) 0.0771(9) 0.0231(7) 0.0163(7) 0.0188(7) S6B 0.0385(10) 0.0372(8) 0.0680(9) 0.0178(6) 0.0122(7) 0.0185(7) S7B 0.0636(14) 0.0498(10) 0.1224(16) 0.0493(11) 0.0339(12) 0.0341(10) S8B 0.0444(13) 0.0711(13) 0.1243(16) 0.0629(13) 0.0267(11) 0.0221(10) C1B 0.053(5) 0.035(3) 0.059(3) 0.014(3) 0.013(3) 0.013(3) C2B 0.063(5) 0.041(3) 0.064(4) 0.017(3) 0.004(3) 0.024(3) C3B 0.040(4) 0.029(3) 0.058(3) 0.014(2) 0.006(2) 0.015(3) C4B 0.034(4) 0.031(3) 0.058(3) 0.012(2) 0.006(2) 0.011(3) C5B 0.029(3) 0.027(3) 0.058(3) 0.007(2) 0.004(2) 0.014(2) C6B 0.035(4) 0.028(3) 0.047(3) 0.008(2) 0.005(2) 0.010(2) C7B 0.044(4) 0.032(3) 0.056(3) 0.018(2) 0.012(3) 0.015(3) C8B 0.042(4) 0.035(3) 0.059(3) 0.021(2) 0.004(3) 0.014(3) C9B 0.063(6) 0.041(4) 0.095(5) 0.035(4) 0.002(4) 0.006(4) C10B 0.064(6) 0.058(4) 0.081(5) 0.038(4) 0.016(4) 0.018(4) S1C 0.0481(12) 0.0470(9) 0.1009(13) 0.0417(9) -0.0052(9) 0.0144(9) S2C 0.0320(12) 0.0842(15) 0.1207(16) 0.0705(13) 0.0111(10) 0.0130(10) S3C 0.0447(11) 0.0432(8) 0.0732(9) 0.0299(7) 0.0166(7) 0.0243(8) S4C 0.0356(11) 0.0516(10) 0.0926(11) 0.0405(9) 0.0100(8) 0.0187(8) S5C 0.0399(10) 0.0398(8) 0.0645(8) 0.0250(7) 0.0089(6) 0.0187(7) S6C 0.0344(10) 0.0447(9) 0.0842(10) 0.0334(8) 0.0041(7) 0.0160(7) S7C 0.0699(15) 0.0604(11) 0.0886(12) 0.0450(10) 0.0333(10) 0.0345(11) S8C 0.0464(12) 0.0392(9) 0.1120(14) 0.0368(9) -0.0129(9) 0.0118(8) C1C 0.069(6) 0.034(3) 0.088(5) 0.019(3) -0.009(4) 0.000(4) C2C 0.064(6) 0.046(4) 0.088(5) 0.035(4) 0.004(4) 0.008(4) C3C 0.028(4) 0.034(3) 0.060(3) 0.021(2) -0.001(2) 0.005(3) C4C 0.040(4) 0.035(3) 0.061(3) 0.021(3) -0.006(3) 0.005(3) C5C 0.034(4) 0.034(3) 0.065(3) 0.018(3) 0.004(3) 0.012(3) C6C 0.037(4) 0.034(3) 0.059(3) 0.019(2) -0.001(2) 0.012(3) C7C 0.051(4) 0.027(3) 0.057(3) 0.017(2) 0.002(3) 0.010(3) C8C 0.039(4) 0.034(3) 0.063(3) 0.017(2) -0.003(3) 0.014(3) C9C 0.082(7) 0.039(4) 0.101(6) 0.034(4) 0.013(5) 0.017(4) C10C 0.068(6) 0.038(4) 0.091(5) 0.019(3) 0.002(4) 0.015(4) C1E 0.111(11) 0.142(12) 0.137(9) 0.025(8) -0.004(7) 0.087(10) Cl1E 0.097(2) 0.137(3) 0.1158(18) 0.0187(17) 0.0039(15) 0.068(2) Cl2E 0.101(3) 0.160(4) 0.175(3) -0.006(3) 0.021(2) 0.051(3) C1F 0.100(9) 0.053(5) 0.117(7) -0.002(5) 0.052(6) 0.017(5) Cl2F 0.081(2) 0.0795(16) 0.1050(16) -0.0088(12) 0.0015(12) 0.0164(14) Cl1F 0.163(4) 0.136(3) 0.147(3) 0.062(2) 0.065(3) 0.087(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S1D 2.2397(16) . ? Cu1 S4D 2.2532(16) . ? Cu1 S6D 2.2648(13) 2_777 ? Cu1 Cu3 2.7750(10) . ? Cu1 Cu2 2.8463(10) . ? Cu1 Cu4 2.9869(11) . ? Cu2 S6D 2.2408(16) 2_777 ? Cu2 S3D 2.2515(16) . ? Cu2 S2D 2.2633(14) 2_777 ? Cu2 Cu3 2.7743(10) 2_777 ? Cu2 Cu4 3.0110(11) 2_777 ? Cu3 S4D 2.2497(14) . ? Cu3 S2D 2.2501(16) . ? Cu3 S5D 2.2503(16) . ? Cu3 Cu2 2.7743(10) 2_777 ? Cu3 Cu4 2.8860(11) 2_777 ? Cu4 S3D 2.2368(14) 2_777 ? Cu4 S5D 2.2549(13) 2_777 ? Cu4 S1D 2.2562(14) . ? Cu4 Cu3 2.8860(11) 2_777 ? Cu4 Cu2 3.0110(11) 2_777 ? S1D C1D 1.755(5) . ? S2D C1D 1.750(6) . ? S2D Cu2 2.2633(14) 2_777 ? S3D C5D 1.742(6) . ? S3D Cu4 2.2368(14) 2_777 ? S4D C5D 1.754(6) . ? S5D C9D 1.752(5) . ? S5D Cu4 2.2549(13) 2_777 ? S6D C9D 1.739(6) . ? S6D Cu2 2.2408(16) 2_777 ? S6D Cu1 2.2648(13) 2_777 ? C1D C2D 1.378(8) . ? C2D C3D 1.423(9) . ? C2D C4D 1.431(8) . ? C3D N2D 1.131(9) . ? C4D N1D 1.134(8) . ? C5D C6D 1.383(7) . ? C6D C7D 1.422(9) . ? C6D C8D 1.436(9) . ? C7D N3D 1.153(9) . ? C8D N4D 1.138(9) . ? C9D C10D 1.375(8) . ? C10D C11D 1.427(8) . ? C10D C12D 1.439(9) . ? C11D N6D 1.154(9) . ? C12D N5D 1.144(9) . ? S1A C3A 1.736(6) . ? S1A C1A 1.762(9) . ? S2A C4A 1.742(7) . ? S2A C2A 1.772(10) . ? S3A C5A 1.728(5) . ? S3A C3A 1.736(6) . ? S4A C5A 1.710(6) . ? S4A C4A 1.728(6) . ? S5A C6A 1.731(6) . ? S5A C7A 1.734(6) . ? S6A C6A 1.714(5) . ? S6A C8A 1.751(6) . ? S7A C7A 1.738(7) . ? S7A C9A 1.809(11) . ? S8A C8A 1.733(6) . ? S8A C10A 1.790(12) . ? C1A C2A 1.385(16) . ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.367(9) . ? C5A C6A 1.387(8) . ? C7A C8A 1.359(9) . ? C9A C10A 1.347(16) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C10A H10A 0.9700 . ? C10A H10B 0.9700 . ? S1B C3B 1.750(6) . ? S1B C1B 1.814(7) . ? S2B C4B 1.749(6) . ? S2B C2B 1.826(7) . ? S3B C3B 1.746(6) . ? S3B C5B 1.748(6) . ? S4B C5B 1.732(6) . ? S4B C4B 1.767(6) . ? S5B C6B 1.738(6) . ? S5B C7B 1.756(6) . ? S6B C6B 1.735(6) . ? S6B C8B 1.760(6) . ? S7B C7B 1.755(6) . ? S7B C9B 1.803(8) . ? S8B C8B 1.745(6) . ? S8B C10B 1.813(8) . ? C1B C2B 1.480(11) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C3B C4B 1.319(9) . ? C5B C6B 1.358(7) . ? C7B C8B 1.330(9) . ? C9B C10B 1.470(12) . ? C9B H9B1 0.9700 . ? C9B H9B2 0.9700 . ? C10B H10C 0.9700 . ? C10B H10D 0.9700 . ? S1C C3C 1.744(6) . ? S1C C1C 1.811(8) . ? S2C C4C 1.739(6) . ? S2C C2C 1.809(8) . ? S3C C5C 1.731(6) . ? S3C C3C 1.734(5) . ? S4C C5C 1.736(6) . ? S4C C4C 1.739(6) . ? S5C C6C 1.739(7) . ? S5C C7C 1.748(6) . ? S6C C6C 1.733(6) . ? S6C C8C 1.746(6) . ? S7C C7C 1.752(6) . ? S7C C9C 1.809(8) . ? S8C C8C 1.748(6) . ? S8C C10C 1.823(9) . ? C1C C2C 1.459(13) . ? C1C H1C1 0.9700 . ? C1C H1C2 0.9700 . ? C2C H2C1 0.9700 . ? C2C H2C2 0.9700 . ? C3C C4C 1.338(9) . ? C5C C6C 1.361(8) . ? C7C C8C 1.327(9) . ? C9C C10C 1.405(12) . ? C9C H9C1 0.9700 . ? C9C H9C2 0.9700 . ? C10C H10E 0.9700 . ? C10C H10F 0.9700 . ? C1E Cl2E 1.692(14) . ? C1E Cl1E 1.778(12) . ? C1E H1E1 0.9700 . ? C1E H1E2 0.9700 . ? C1F Cl2F 1.728(12) . ? C1F Cl1F 1.739(11) . ? C1F H1F1 0.9700 . ? C1F H1F2 0.9700 . ? 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 S1D Cu1 S4D 122.70(5) . . ? S1D Cu1 S6D 115.70(6) . 2_777 ? S4D Cu1 S6D 118.19(6) . 2_777 ? S1D Cu1 Cu3 95.11(4) . . ? S4D Cu1 Cu3 51.90(4) . . ? S6D Cu1 Cu3 140.19(5) 2_777 . ? S1D Cu1 Cu2 138.57(4) . . ? S4D Cu1 Cu2 92.20(5) . . ? S6D Cu1 Cu2 50.45(4) 2_777 . ? Cu3 Cu1 Cu2 89.81(3) . . ? S1D Cu1 Cu4 48.60(4) . . ? S4D Cu1 Cu4 142.92(4) . . ? S6D Cu1 Cu4 91.30(4) 2_777 . ? Cu3 Cu1 Cu4 91.14(3) . . ? Cu2 Cu1 Cu4 90.28(3) . . ? S6D Cu2 S3D 119.60(6) 2_777 . ? S6D Cu2 S2D 122.09(6) 2_777 2_777 ? S3D Cu2 S2D 114.76(6) . 2_777 ? S6D Cu2 Cu3 94.83(4) 2_777 2_777 ? S3D Cu2 Cu3 138.10(4) . 2_777 ? S2D Cu2 Cu3 51.86(4) 2_777 2_777 ? S6D Cu2 Cu1 51.20(4) 2_777 . ? S3D Cu2 Cu1 93.70(4) . . ? S2D Cu2 Cu1 142.00(5) 2_777 . ? Cu3 Cu2 Cu1 90.16(3) 2_777 . ? S6D Cu2 Cu4 141.31(4) 2_777 2_777 ? S3D Cu2 Cu4 47.66(4) . 2_777 ? S2D Cu2 Cu4 90.91(4) 2_777 2_777 ? Cu3 Cu2 Cu4 90.65(3) 2_777 2_777 ? Cu1 Cu2 Cu4 90.61(3) . 2_777 ? S4D Cu3 S2D 118.78(6) . . ? S4D Cu3 S5D 116.61(6) . . ? S2D Cu3 S5D 117.83(5) . . ? S4D Cu3 Cu2 145.40(5) . 2_777 ? S2D Cu3 Cu2 52.29(4) . 2_777 ? S5D Cu3 Cu2 92.72(4) . 2_777 ? S4D Cu3 Cu1 52.01(4) . . ? S2D Cu3 Cu1 92.98(4) . . ? S5D Cu3 Cu1 144.76(4) . . ? Cu2 Cu3 Cu1 93.49(3) 2_777 . ? S4D Cu3 Cu4 91.81(5) . 2_777 ? S2D Cu3 Cu4 145.71(4) . 2_777 ? S5D Cu3 Cu4 50.23(4) . 2_777 ? Cu2 Cu3 Cu4 93.87(3) 2_777 2_777 ? Cu1 Cu3 Cu4 94.72(3) . 2_777 ? S3D Cu4 S5D 123.17(5) 2_777 2_777 ? S3D Cu4 S1D 118.07(5) 2_777 . ? S5D Cu4 S1D 118.50(5) 2_777 . ? S3D Cu4 Cu3 92.61(5) 2_777 2_777 ? S5D Cu4 Cu3 50.09(4) 2_777 2_777 ? S1D Cu4 Cu3 133.43(5) . 2_777 ? S3D Cu4 Cu1 132.64(5) 2_777 . ? S5D Cu4 Cu1 90.74(4) 2_777 . ? S1D Cu4 Cu1 48.13(4) . . ? Cu3 Cu4 Cu1 85.31(3) 2_777 . ? S3D Cu4 Cu2 48.07(4) 2_777 2_777 ? S5D Cu4 Cu2 134.66(5) 2_777 2_777 ? S1D Cu4 Cu2 91.07(4) . 2_777 ? Cu3 Cu4 Cu2 84.56(3) 2_777 2_777 ? Cu1 Cu4 Cu2 84.72(3) . 2_777 ? C1D S1D Cu1 110.2(2) . . ? C1D S1D Cu4 103.68(16) . . ? Cu1 S1D Cu4 83.27(5) . . ? C1D S2D Cu3 112.39(17) . . ? C1D S2D Cu2 105.36(16) . 2_777 ? Cu3 S2D Cu2 75.86(5) . 2_777 ? C5D S3D Cu4 108.64(16) . 2_777 ? C5D S3D Cu2 106.6(2) . . ? Cu4 S3D Cu2 84.27(5) 2_777 . ? C5D S4D Cu3 111.16(18) . . ? C5D S4D Cu1 107.73(17) . . ? Cu3 S4D Cu1 76.09(5) . . ? C9D S5D Cu3 112.7(2) . . ? C9D S5D Cu4 104.32(16) . 2_777 ? Cu3 S5D Cu4 79.67(5) . 2_777 ? C9D S6D Cu2 110.64(18) . 2_777 ? C9D S6D Cu1 105.56(16) . 2_777 ? Cu2 S6D Cu1 78.35(5) 2_777 2_777 ? C2D C1D S2D 118.7(4) . . ? C2D C1D S1D 117.3(4) . . ? S2D C1D S1D 124.0(3) . . ? C1D C2D C3D 122.1(5) . . ? C1D C2D C4D 120.3(6) . . ? C3D C2D C4D 117.6(5) . . ? N2D C3D C2D 178.5(7) . . ? N1D C4D C2D 176.2(7) . . ? C6D C5D S3D 118.8(5) . . ? C6D C5D S4D 117.9(4) . . ? S3D C5D S4D 123.3(3) . . ? C5D C6D C7D 122.7(6) . . ? C5D C6D C8D 120.6(6) . . ? C7D C6D C8D 116.7(5) . . ? N3D C7D C6D 178.2(7) . . ? N4D C8D C6D 178.5(8) . . ? C10D C9D S6D 118.9(4) . . ? C10D C9D S5D 117.7(4) . . ? S6D C9D S5D 123.5(3) . . ? C9D C10D C11D 121.7(6) . . ? C9D C10D C12D 122.7(5) . . ? C11D C10D C12D 115.5(5) . . ? N6D C11D C10D 176.9(7) . . ? N5D C12D C10D 177.6(7) . . ? C3A S1A C1A 101.4(4) . . ? C4A S2A C2A 100.7(4) . . ? C5A S3A C3A 95.7(3) . . ? C5A S4A C4A 95.5(3) . . ? C6A S5A C7A 95.9(3) . . ? C6A S6A C8A 96.0(3) . . ? C7A S7A C9A 97.1(4) . . ? C8A S8A C10A 102.0(5) . . ? C2A C1A S1A 123.1(8) . . ? C2A C1A H1A1 106.6 . . ? S1A C1A H1A1 106.6 . . ? C2A C1A H1A2 106.6 . . ? S1A C1A H1A2 106.6 . . ? H1A1 C1A H1A2 106.5 . . ? C1A C2A S2A 122.0(9) . . ? C1A C2A H2A1 106.8 . . ? S2A C2A H2A1 106.8 . . ? C1A C2A H2A2 106.8 . . ? S2A C2A H2A2 106.8 . . ? H2A1 C2A H2A2 106.7 . . ? C4A C3A S3A 115.6(4) . . ? C4A C3A S1A 129.3(5) . . ? S3A C3A S1A 115.0(3) . . ? C3A C4A S4A 117.4(5) . . ? C3A C4A S2A 127.7(5) . . ? S4A C4A S2A 114.9(4) . . ? C6A C5A S4A 122.9(4) . . ? C6A C5A S3A 121.2(5) . . ? S4A C5A S3A 115.8(3) . . ? C5A C6A S6A 123.3(5) . . ? C5A C6A S5A 121.4(4) . . ? S6A C6A S5A 115.3(3) . . ? C8A C7A S5A 116.8(5) . . ? C8A C7A S7A 125.0(5) . . ? S5A C7A S7A 118.0(4) . . ? C7A C8A S8A 127.2(5) . . ? C7A C8A S6A 116.0(4) . . ? S8A C8A S6A 116.7(3) . . ? C10A C9A S7A 120.5(9) . . ? C10A C9A H9A1 107.2 . . ? S7A C9A H9A1 107.2 . . ? C10A C9A H9A2 107.2 . . ? S7A C9A H9A2 107.2 . . ? H9A1 C9A H9A2 106.8 . . ? C9A C10A S8A 123.4(8) . . ? C9A C10A H10A 106.5 . . ? S8A C10A H10A 106.5 . . ? C9A C10A H10B 106.5 . . ? S8A C10A H10B 106.5 . . ? H10A C10A H10B 106.5 . . ? C3B S1B C1B 100.0(3) . . ? C4B S2B C2B 101.7(3) . . ? C3B S3B C5B 94.5(3) . . ? C5B S4B C4B 94.6(3) . . ? C6B S5B C7B 94.9(3) . . ? C6B S6B C8B 94.9(3) . . ? C7B S7B C9B 102.8(4) . . ? C8B S8B C10B 99.2(3) . . ? C2B C1B S1B 114.1(5) . . ? C2B C1B H1B1 108.7 . . ? S1B C1B H1B1 108.7 . . ? C2B C1B H1B2 108.7 . . ? S1B C1B H1B2 108.7 . . ? H1B1 C1B H1B2 107.6 . . ? C1B C2B S2B 113.0(4) . . ? C1B C2B H2B1 109.0 . . ? S2B C2B H2B1 109.0 . . ? C1B C2B H2B2 109.0 . . ? S2B C2B H2B2 109.0 . . ? H2B1 C2B H2B2 107.8 . . ? C4B C3B S3B 117.7(4) . . ? C4B C3B S1B 127.0(4) . . ? S3B C3B S1B 115.2(4) . . ? C3B C4B S2B 130.5(4) . . ? C3B C4B S4B 116.9(4) . . ? S2B C4B S4B 112.5(3) . . ? C6B C5B S4B 122.9(5) . . ? C6B C5B S3B 122.5(5) . . ? S4B C5B S3B 114.7(3) . . ? C5B C6B S6B 122.2(5) . . ? C5B C6B S5B 123.0(5) . . ? S6B C6B S5B 114.8(3) . . ? C8B C7B S7B 128.2(4) . . ? C8B C7B S5B 117.1(4) . . ? S7B C7B S5B 114.6(4) . . ? C7B C8B S8B 128.7(4) . . ? C7B C8B S6B 116.9(4) . . ? S8B C8B S6B 114.2(4) . . ? C10B C9B S7B 114.8(6) . . ? C10B C9B H9B1 108.6 . . ? S7B C9B H9B1 108.6 . . ? C10B C9B H9B2 108.6 . . ? S7B C9B H9B2 108.6 . . ? H9B1 C9B H9B2 107.5 . . ? C9B C10B S8B 114.4(5) . . ? C9B C10B H10C 108.7 . . ? S8B C10B H10C 108.7 . . ? C9B C10B H10D 108.7 . . ? S8B C10B H10D 108.7 . . ? H10C C10B H10D 107.6 . . ? C3C S1C C1C 98.5(4) . . ? C4C S2C C2C 102.8(3) . . ? C5C S3C C3C 95.5(3) . . ? C5C S4C C4C 95.2(3) . . ? C6C S5C C7C 94.5(3) . . ? C6C S6C C8C 94.9(3) . . ? C7C S7C C9C 103.0(4) . . ? C8C S8C C10C 96.6(3) . . ? C2C C1C S1C 112.7(6) . . ? C2C C1C H1C1 109.0 . . ? S1C C1C H1C1 109.0 . . ? C2C C1C H1C2 109.0 . . ? S1C C1C H1C2 109.0 . . ? H1C1 C1C H1C2 107.8 . . ? C1C C2C S2C 117.8(5) . . ? C1C C2C H2C1 107.8 . . ? S2C C2C H2C1 107.8 . . ? C1C C2C H2C2 107.8 . . ? S2C C2C H2C2 107.8 . . ? H2C1 C2C H2C2 107.2 . . ? C4C C3C S3C 117.1(4) . . ? C4C C3C S1C 127.5(4) . . ? S3C C3C S1C 115.3(4) . . ? C3C C4C S2C 128.3(4) . . ? C3C C4C S4C 117.2(4) . . ? S2C C4C S4C 114.5(4) . . ? C6C C5C S3C 121.7(5) . . ? C6C C5C S4C 123.3(5) . . ? S3C C5C S4C 115.0(3) . . ? C5C C6C S6C 123.9(5) . . ? C5C C6C S5C 120.7(5) . . ? S6C C6C S5C 115.3(3) . . ? C8C C7C S5C 117.4(4) . . ? C8C C7C S7C 128.8(4) . . ? S5C C7C S7C 113.7(4) . . ? C7C C8C S6C 117.3(4) . . ? C7C C8C S8C 126.2(5) . . ? S6C C8C S8C 116.5(4) . . ? C10C C9C S7C 118.4(5) . . ? C10C C9C H9C1 107.7 . . ? S7C C9C H9C1 107.7 . . ? C10C C9C H9C2 107.7 . . ? S7C C9C H9C2 107.7 . . ? H9C1 C9C H9C2 107.1 . . ? C9C C10C S8C 118.0(6) . . ? C9C C10C H10E 107.8 . . ? S8C C10C H10E 107.8 . . ? C9C C10C H10F 107.8 . . ? S8C C10C H10F 107.8 . . ? H10E C10C H10F 107.1 . . ? Cl2E C1E Cl1E 112.0(7) . . ? Cl2E C1E H1E1 109.2 . . ? Cl1E C1E H1E1 109.2 . . ? Cl2E C1E H1E2 109.2 . . ? Cl1E C1E H1E2 109.2 . . ? H1E1 C1E H1E2 107.9 . . ? Cl2F C1F Cl1F 114.3(5) . . ? Cl2F C1F H1F1 108.7 . . ? Cl1F C1F H1F1 108.7 . . ? Cl2F C1F H1F2 108.7 . . ? Cl1F C1F H1F2 108.7 . . ? H1F1 C1F H1F2 107.6 . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 2.398 _refine_diff_density_min -2.311 _refine_diff_density_rms 0.251 #===END data_3 _publ_requested_journal 'Journal of Materials Chemistry' _publ_contact_author_name ; Sandrine Perruchas, Kamal Boubekeur and Pascale Auban-Senzier ; _publ_contact_author_address ; Institut des Materiaux Jean Rouxel 2 rue de la Houssiniere BP 32229 44322 nantes Cedex 3 FRANCE present address for S. Perruchas: Baker laboratories department of chemistry Cornell University Ithaca NY 14853 USA ; _publ_contact_author_email 'sp353@cornell.edu' _publ_section_title ; Radical cation salts of TTF derivatives incorporating the maleonitriledithiolate copper cluster anion [Cu8(i-mnt)6]4- ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; hexakis-ethylenedithiotetrathiafulvalenium-hexa-iso-maleonitrile- octa-cuprate(I) ; _chemical_name_common '(EDT-TTF)6[Cu8(i-mnt)6]' _chemical_formula_moiety 'C24 Cu8 N12 S12, 6(C8 H6 S6)' _chemical_formula_sum 'C72 H36 Cu8 N12 S48' _chemical_formula_weight 3116.33 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8708(14) _cell_length_b 14.590(2) _cell_length_c 16.714(2) _cell_angle_alpha 76.930(16) _cell_angle_beta 77.497(14) _cell_angle_gamma 72.449(15) _cell_volume 2654.1(6) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8000 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 25.8 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.950 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 2.564 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4845 _exptl_absorpt_correction_T_max 0.860 _exptl_absorpt_process_details 'X-PREP' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'stoe IPDS' _diffrn_measurement_method 'oscillation phi. incr. = 1.4' _diffrn_detector_area_resol_mean 6.66 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26921 _diffrn_reflns_av_R_equivalents 0.1284 _diffrn_reflns_av_sigmaI/netI 0.1268 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.83 _reflns_number_total 9559 _reflns_number_gt 4343 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE [STOE-IPDS]' _computing_cell_refinement 'SELECT, CELL [STOE-IPDS]' _computing_data_reduction 'INTEGRATE [STOE-IPDS]' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND (Brandenburg, 1999)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.1209P)^2^+0.0000sin\q/\l] where P = 0.33333Fo^2^ + 0.66667Fc^2^ ; _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 9559 _refine_ls_number_parameters 628 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1509 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_ref 0.2154 _refine_ls_wR_factor_gt 0.1703 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _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 0.95903(13) 0.12267(10) 0.08338(7) 0.0423(4) Uani 1 1 d . . . Cu2 Cu 1.15930(13) -0.04053(10) 0.08116(7) 0.0418(4) Uani 1 1 d . . . Cu3 Cu 0.80645(14) 0.00745(11) 0.09780(7) 0.0448(4) Uani 1 1 d . . . Cu4 Cu 1.00478(13) -0.16036(11) 0.09681(7) 0.0449(4) Uani 1 1 d . . . S1 S 1.0491(3) 0.0296(2) 0.18986(13) 0.0406(7) Uani 1 1 d . . . S2 S 0.8805(3) -0.1006(2) 0.20697(13) 0.0406(7) Uani 1 1 d . . . C1 C 0.9586(10) -0.0446(8) 0.2490(5) 0.038(3) Uani 1 1 d . . . C2 C 0.9489(11) -0.0573(9) 0.3354(5) 0.044(3) Uani 1 1 d . . . C3 C 1.0065(11) -0.0111(10) 0.3731(6) 0.045(3) Uani 1 1 d . . . C4 C 0.8839(12) -0.1230(10) 0.3887(6) 0.051(3) Uani 1 1 d . . . N1 N 0.8320(11) -0.1741(9) 0.4333(6) 0.065(3) Uani 1 1 d . . . N2 N 1.0486(12) 0.0285(10) 0.4059(6) 0.075(4) Uani 1 1 d . . . S4 S 0.7236(3) -0.0436(2) 0.01210(13) 0.0377(6) Uani 1 1 d . . . S3 S 0.9430(3) -0.2225(2) 0.00768(14) 0.0399(7) Uani 1 1 d . . . C5 C 0.7881(10) -0.1696(8) 0.0189(5) 0.033(2) Uani 1 1 d . . . C6 C 0.7121(11) -0.2293(8) 0.0332(6) 0.040(3) Uani 1 1 d . . . C7 C 0.5872(13) -0.1914(10) 0.0462(6) 0.049(3) Uani 1 1 d . . . C8 C 0.7605(12) -0.3330(10) 0.0345(7) 0.051(3) Uani 1 1 d . . . N3 N 0.4864(13) -0.1610(9) 0.0583(6) 0.068(3) Uani 1 1 d . . . N4 N 0.7922(13) -0.4157(9) 0.0347(7) 0.073(4) Uani 1 1 d . . . S5 S 0.7584(3) 0.1706(2) 0.09415(14) 0.0400(7) Uani 1 1 d . . . S6 S 0.7979(3) 0.2054(2) -0.09750(13) 0.0395(7) Uani 1 1 d . . . C9 C 0.7167(10) 0.2372(8) -0.0014(5) 0.038(3) Uani 1 1 d . . . C10 C 0.6165(11) 0.3117(8) -0.0014(6) 0.039(3) Uani 1 1 d . . . C12 C 0.5387(12) 0.3325(9) 0.0736(7) 0.052(3) Uani 1 1 d . . . C11 C 0.5797(11) 0.3688(8) -0.0777(7) 0.045(3) Uani 1 1 d . . . N5 N 0.4699(12) 0.3464(9) 0.1319(7) 0.072(4) Uani 1 1 d . . . N6 N 0.5492(13) 0.4173(9) -0.1368(7) 0.076(4) Uani 1 1 d . . . S1A S 1.2603(3) 0.1196(3) 0.28072(17) 0.0588(9) Uani 1 1 d . . . S2A S 1.5526(3) -0.0129(3) 0.20582(15) 0.0576(9) Uani 1 1 d . . . S3A S 1.3159(3) 0.0081(2) 0.44238(14) 0.0453(7) Uani 1 1 d . . . S4A S 1.5593(3) -0.0976(2) 0.38118(14) 0.0446(7) Uani 1 1 d . . . S5A S 1.3447(3) -0.1055(2) 0.62777(15) 0.0478(8) Uani 1 1 d . . . S6A S 1.5875(3) -0.2140(2) 0.56842(15) 0.0477(8) Uani 1 1 d . . . C1A C 1.3479(16) 0.1356(11) 0.1790(7) 0.074(5) Uani 1 1 d . . . H1A1 H 1.2938 0.1675 0.1390 0.089 Uiso 1 1 calc R . . H1A2 H 1.3961 0.1792 0.1780 0.089 Uiso 1 1 calc R . . C2A C 1.4290(16) 0.0441(12) 0.1514(7) 0.074(5) Uani 1 1 d . . . H2A1 H 1.4596 0.0591 0.0926 0.089 Uiso 1 1 calc R . . H2A2 H 1.3823 -0.0021 0.1578 0.089 Uiso 1 1 calc R . . C3A C 1.3654(11) 0.0334(9) 0.3359(6) 0.045(3) Uani 1 1 d . . . C4A C 1.4769(11) -0.0164(8) 0.3080(6) 0.044(3) Uani 1 1 d . . . C5A C 1.4448(10) -0.0753(8) 0.4642(5) 0.040(3) Uani 1 1 d . . . C6A C 1.4607(11) -0.1272(8) 0.5444(6) 0.040(3) Uani 1 1 d . . . C7A C 1.4244(12) -0.1924(10) 0.6989(6) 0.058(4) Uani 1 1 d . . . H7A H 1.3908 -0.2034 0.7547 0.069 Uiso 1 1 calc R . . C8A C 1.5322(13) -0.2422(10) 0.6727(6) 0.056(4) Uani 1 1 d . . . H8A H 1.5773 -0.2907 0.7086 0.067 Uiso 1 1 calc R . . S1B S 1.1758(3) 0.3826(2) 0.23618(18) 0.0596(9) Uani 1 1 d . . . S2B S 0.9576(4) 0.6083(3) 0.19941(19) 0.0660(10) Uani 1 1 d . . . S4B S 0.8638(3) 0.5562(3) 0.37591(19) 0.0593(9) Uani 1 1 d . . . S3B S 1.0426(3) 0.3696(2) 0.40700(16) 0.0508(8) Uani 1 1 d . . . S5B S 0.9135(3) 0.3424(3) 0.60269(18) 0.0562(9) Uani 1 1 d . . . S6B S 0.7308(3) 0.5243(3) 0.56378(19) 0.0596(9) Uani 1 1 d . . . C1B C 1.1825(13) 0.4862(11) 0.1545(7) 0.064(4) Uani 1 1 d . . . H1B1 H 1.2113 0.5312 0.1744 0.076 Uiso 1 1 calc R . . H1B2 H 1.2406 0.4639 0.1077 0.076 Uiso 1 1 calc R . . C2B C 1.0672(15) 0.5402(10) 0.1245(7) 0.068(4) Uani 1 1 d . . . H2B1 H 1.0332 0.4941 0.1110 0.081 Uiso 1 1 calc R . . H2B2 H 1.0831 0.5853 0.0738 0.081 Uiso 1 1 calc R . . C4B C 0.9719(12) 0.5211(9) 0.2907(6) 0.050(3) Uani 1 1 d . . . C3B C 1.0540(11) 0.4361(9) 0.3060(6) 0.046(3) Uani 1 1 d . . . C5B C 0.9162(11) 0.4548(8) 0.4457(7) 0.044(3) Uani 1 1 d . . . C6B C 0.8609(11) 0.4404(9) 0.5281(7) 0.049(3) Uani 1 1 d . . . C8B C 0.7184(14) 0.4605(11) 0.6639(7) 0.063(4) Uani 1 1 d . . . H8B H 0.6541 0.4825 0.7041 0.075 Uiso 1 1 calc R . . C7B C 0.8031(14) 0.3788(11) 0.6824(8) 0.060(4) Uani 1 1 d . . . H7B H 0.8023 0.3433 0.7362 0.071 Uiso 1 1 calc R . . S3C S 0.5970(4) 0.3916(3) 0.4498(2) 0.0658(10) Uani 1 1 d . . . S6C S 0.7156(4) 0.1751(3) 0.6626(2) 0.0637(9) Uani 1 1 d . . . S2C S 0.9035(4) 0.2535(3) 0.2817(2) 0.0796(12) Uani 1 1 d . . . S4C S 0.8089(4) 0.2243(3) 0.4650(4) 0.0901(14) Uani 1 1 d . . . S5C S 0.4887(5) 0.3458(3) 0.6334(2) 0.0905(15) Uani 1 1 d . . . S1C S 0.6641(6) 0.4469(4) 0.2652(2) 0.111(2) Uani 1 1 d . . . C3C C 0.696(2) 0.3746(17) 0.3505(12) 0.055(6) Uiso 0.65(2) 1 d P . . C4C C 0.795(2) 0.2995(17) 0.3537(12) 0.042(5) Uiso 0.65(2) 1 d P . . C5C C 0.6797(17) 0.2952(12) 0.5044(10) 0.040(5) Uiso 0.65(2) 1 d P . . C6C C 0.644(2) 0.2730(17) 0.5856(10) 0.034(5) Uiso 0.65(2) 1 d P . . C3C' C 0.586(3) 0.313(2) 0.5677(17) 0.030(8) Uiso 0.35(2) 1 d P . . C6C' C 0.725(3) 0.309(2) 0.4222(16) 0.031(8) Uiso 0.35(2) 1 d P . . C5C' C 0.762(5) 0.337(3) 0.342(2) 0.042(9) Uiso 0.35(2) 1 d P . . C4C' C 0.679(4) 0.237(3) 0.582(2) 0.050(12) Uiso 0.35(2) 1 d P . . C1C C 0.758(3) 0.3899(15) 0.1817(10) 0.128(10) Uani 1 1 d . . . C7C C 0.509(2) 0.2806(13) 0.7317(8) 0.105(8) Uani 1 1 d . . . C2C C 0.8756(19) 0.3479(18) 0.1909(8) 0.093(6) Uani 1 1 d . . . C8C C 0.6113(18) 0.2179(15) 0.7447(8) 0.082(5) 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 0.0375(9) 0.0544(9) 0.0275(6) 0.0076(5) 0.0006(5) -0.0160(7) Cu2 0.0425(9) 0.0500(8) 0.0247(6) 0.0039(5) 0.0066(5) -0.0164(7) Cu3 0.0490(10) 0.0509(9) 0.0303(6) 0.0050(6) -0.0055(6) -0.0165(8) Cu4 0.0384(10) 0.0620(9) 0.0297(6) -0.0020(6) 0.0021(5) -0.0161(8) S1 0.0410(19) 0.0555(17) 0.0192(10) 0.0047(10) 0.0007(10) -0.0161(14) S2 0.0410(18) 0.0548(17) 0.0206(10) 0.0040(10) 0.0026(10) -0.0177(15) C1 0.037(7) 0.044(6) 0.020(4) 0.006(4) 0.006(4) -0.007(5) C2 0.045(8) 0.065(8) 0.012(4) 0.009(4) 0.002(4) -0.015(6) C3 0.037(8) 0.074(8) 0.012(4) -0.003(5) -0.002(4) -0.005(6) C4 0.045(8) 0.071(8) 0.020(5) 0.009(5) -0.001(5) -0.005(7) N1 0.057(8) 0.080(8) 0.036(5) 0.008(5) 0.017(5) -0.017(7) N2 0.089(10) 0.108(10) 0.022(5) 0.001(5) 0.003(5) -0.035(9) S4 0.0346(17) 0.0515(17) 0.0230(10) 0.0029(10) 0.0027(10) -0.0176(14) S3 0.0382(18) 0.0485(16) 0.0282(11) 0.0036(11) 0.0013(10) -0.0165(14) C5 0.036(7) 0.049(6) 0.016(4) 0.005(4) -0.001(4) -0.023(5) C6 0.046(8) 0.049(7) 0.029(5) 0.004(4) 0.001(4) -0.031(6) C7 0.044(9) 0.070(9) 0.033(5) -0.001(5) 0.008(5) -0.030(7) C8 0.054(9) 0.052(9) 0.043(6) 0.006(5) -0.001(5) -0.023(7) N3 0.066(10) 0.072(8) 0.053(6) 0.007(5) 0.011(6) -0.030(7) N4 0.086(11) 0.056(8) 0.070(7) 0.008(6) -0.005(6) -0.029(7) S5 0.0360(18) 0.0512(17) 0.0224(10) 0.0040(10) 0.0040(10) -0.0099(14) S6 0.0370(18) 0.0522(17) 0.0208(10) 0.0065(10) -0.0004(10) -0.0117(14) C9 0.037(7) 0.051(7) 0.024(4) 0.010(4) 0.000(4) -0.024(6) C10 0.038(8) 0.040(6) 0.031(5) 0.001(4) 0.001(4) -0.009(6) C12 0.041(8) 0.052(7) 0.038(6) 0.001(5) 0.008(5) 0.006(6) C11 0.038(8) 0.040(6) 0.042(6) 0.005(5) 0.001(5) 0.000(6) N5 0.065(9) 0.065(8) 0.052(6) 0.006(5) 0.017(6) 0.003(6) N6 0.102(12) 0.057(7) 0.054(6) 0.016(6) -0.029(7) -0.007(7) S1A 0.049(2) 0.073(2) 0.0392(14) 0.0192(14) -0.0100(13) -0.0124(18) S2A 0.056(2) 0.087(2) 0.0229(12) 0.0071(13) 0.0037(12) -0.0288(19) S3A 0.0403(19) 0.0626(19) 0.0228(11) 0.0037(11) 0.0008(10) -0.0110(15) S4A 0.0410(19) 0.0597(18) 0.0236(11) 0.0037(11) 0.0001(11) -0.0112(15) S5A 0.038(2) 0.066(2) 0.0295(12) 0.0026(12) 0.0031(11) -0.0142(16) S6A 0.050(2) 0.0534(18) 0.0273(12) 0.0060(11) -0.0017(11) -0.0076(15) C1A 0.098(13) 0.067(9) 0.036(6) 0.022(6) -0.003(7) -0.017(9) C2A 0.100(13) 0.094(12) 0.029(6) 0.003(6) -0.020(7) -0.028(10) C3A 0.048(8) 0.063(8) 0.024(5) 0.009(5) -0.004(5) -0.028(7) C4A 0.047(8) 0.049(7) 0.025(5) 0.012(4) -0.002(5) -0.014(6) C5A 0.041(7) 0.057(7) 0.018(4) 0.008(4) -0.007(4) -0.016(6) C6A 0.046(8) 0.048(7) 0.025(4) -0.002(4) -0.003(4) -0.017(6) C7A 0.047(9) 0.085(10) 0.029(5) 0.011(6) 0.005(5) -0.022(8) C8A 0.061(10) 0.066(8) 0.025(5) 0.023(5) -0.006(5) -0.017(7) S1B 0.060(3) 0.0536(19) 0.0411(15) 0.0078(13) 0.0045(14) -0.0003(17) S2B 0.071(3) 0.055(2) 0.0452(16) 0.0115(14) 0.0009(15) -0.0002(18) S4B 0.053(2) 0.057(2) 0.0473(16) 0.0062(14) 0.0070(14) -0.0071(17) S3B 0.050(2) 0.0530(18) 0.0376(14) 0.0063(12) 0.0000(12) -0.0109(16) S5B 0.060(2) 0.058(2) 0.0449(15) 0.0033(14) -0.0027(14) -0.0207(18) S6B 0.054(2) 0.063(2) 0.0480(16) -0.0025(15) 0.0065(14) -0.0118(18) C1B 0.062(10) 0.071(9) 0.039(6) 0.007(6) 0.006(6) -0.012(8) C2B 0.085(12) 0.059(8) 0.038(6) 0.013(6) -0.003(6) -0.007(8) C4B 0.056(9) 0.052(7) 0.034(5) 0.005(5) 0.002(5) -0.017(7) C3B 0.037(8) 0.047(7) 0.040(5) 0.000(5) 0.007(5) -0.006(6) C5B 0.032(8) 0.039(6) 0.048(6) 0.001(5) 0.002(5) -0.001(5) C6B 0.038(8) 0.050(7) 0.048(6) 0.001(5) 0.005(5) -0.012(6) C8B 0.062(11) 0.084(11) 0.036(6) -0.006(6) 0.014(6) -0.031(9) C7B 0.068(11) 0.064(9) 0.049(7) -0.007(6) 0.003(6) -0.032(8) S3C 0.054(3) 0.062(2) 0.0629(19) -0.0015(16) -0.0058(16) 0.0015(18) S6C 0.071(3) 0.057(2) 0.0602(18) -0.0042(16) -0.0168(17) -0.0124(19) S2C 0.075(3) 0.071(3) 0.073(2) -0.0083(19) 0.020(2) -0.015(2) S4C 0.055(3) 0.053(2) 0.161(5) -0.016(3) -0.030(3) -0.006(2) S5C 0.130(4) 0.092(3) 0.0400(17) -0.0022(18) 0.017(2) -0.044(3) S1C 0.190(6) 0.104(4) 0.0385(18) -0.009(2) 0.017(2) -0.068(4) C1C 0.24(3) 0.083(13) 0.042(8) -0.025(8) 0.011(13) -0.029(17) C7C 0.17(2) 0.077(11) 0.027(6) 0.003(7) 0.032(9) -0.019(13) C2C 0.097(14) 0.161(19) 0.026(6) -0.010(8) 0.026(7) -0.074(15) C8C 0.084(14) 0.119(15) 0.035(7) 0.009(8) 0.002(7) -0.037(12) _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 S1 2.238(3) . ? Cu1 S3 2.246(3) 2_755 ? Cu1 S5 2.249(3) . ? Cu1 Cu3 2.762(2) . ? Cu1 Cu2 2.813(2) . ? Cu1 Cu4 2.8966(17) 2_755 ? Cu2 S1 2.250(3) . ? Cu2 S4 2.257(3) 2_755 ? Cu2 S6 2.269(3) 2_755 ? Cu2 Cu4 2.830(2) . ? Cu2 Cu3 2.8782(17) 2_755 ? Cu3 S4 2.260(3) . ? Cu3 S5 2.264(3) . ? Cu3 S2 2.268(3) . ? Cu3 Cu4 2.840(2) . ? Cu3 Cu2 2.8782(17) 2_755 ? Cu4 S6 2.236(3) 2_755 ? Cu4 S3 2.250(3) . ? Cu4 S2 2.258(3) . ? Cu4 Cu1 2.8966(17) 2_755 ? S1 C1 1.750(10) . ? S2 C1 1.738(12) . ? C1 C2 1.398(12) . ? C2 C3 1.405(18) . ? C2 C4 1.439(16) . ? C3 N2 1.149(16) . ? C4 N1 1.148(16) . ? S4 C5 1.753(11) . ? S4 Cu2 2.257(3) 2_755 ? S3 C5 1.753(11) . ? S3 Cu1 2.246(3) 2_755 ? C5 C6 1.384(14) . ? C6 C7 1.404(19) . ? C6 C8 1.444(18) . ? C7 N3 1.134(17) . ? C8 N4 1.149(16) . ? S5 C9 1.759(10) . ? S6 C9 1.766(10) . ? S6 Cu4 2.236(3) 2_755 ? S6 Cu2 2.269(3) 2_755 ? C9 C10 1.348(16) . ? C10 C12 1.420(15) . ? C10 C11 1.432(15) . ? C12 N5 1.142(15) . ? C11 N6 1.137(15) . ? S1A C3A 1.737(13) . ? S1A C1A 1.797(13) . ? S2A C4A 1.746(10) . ? S2A C2A 1.781(15) . ? S3A C5A 1.695(12) . ? S3A C3A 1.740(10) . ? S4A C5A 1.732(10) . ? S4A C4A 1.738(11) . ? S5A C7A 1.731(13) . ? S5A C6A 1.744(11) . ? S6A C6A 1.706(12) . ? S6A C8A 1.727(10) . ? C1A C2A 1.49(2) . ? C1A N5 3.64(2) 1_655 ? C1A H1A1 0.9700 . ? C1A H1A2 0.9700 . ? C2A N3 3.607(16) 2_755 ? C2A H2A1 0.9700 . ? C2A H2A2 0.9700 . ? C3A C4A 1.343(17) . ? C5A C6A 1.404(13) . ? C7A C8A 1.303(18) . ? C7A H7A 0.9300 . ? C8A N5 3.273(14) 2_756 ? C8A H8A 0.9300 . ? S1B C3B 1.750(11) . ? S1B C1B 1.801(12) . ? S2B C4B 1.755(11) . ? S2B C2B 1.823(14) . ? S4B C5B 1.708(11) . ? S4B C4B 1.755(12) . ? S3B C5B 1.742(12) . ? S3B C3B 1.745(11) . ? S5B C7B 1.709(14) . ? S5B C6B 1.727(12) . ? S6B C8B 1.721(12) . ? S6B C6B 1.741(13) . ? C1B C2B 1.49(2) . ? C1B N4 3.468(18) 2_755 ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? C4B C3B 1.337(17) . ? C5B C6B 1.390(15) . ? C8B C7B 1.33(2) . ? C8B N6 3.528(17) 1_556 ? C8B H8B 0.9300 . ? C7B H7B 0.9300 . ? S3C C5C 1.658(18) . ? S3C C6C' 1.68(3) . ? S3C C3C 1.83(2) . ? S3C C3C' 2.04(3) . ? S6C C4C' 1.51(4) . ? S6C C8C 1.730(17) . ? S6C C6C 1.82(2) . ? S2C C4C 1.65(2) . ? S2C C2C 1.82(2) . ? S2C C5C' 1.98(5) . ? S4C C6C' 1.48(3) . ? S4C C5C 1.666(18) . ? S4C C4C 1.95(2) . ? S4C C4C' 2.21(4) . ? S5C C3C' 1.46(3) . ? S5C C7C 1.729(16) . ? S5C C6C 1.93(2) . ? S1C C3C 1.61(2) . ? S1C C1C 1.780(19) . ? S1C C5C' 2.03(5) . ? C3C C5C' 0.81(5) . ? C3C C4C 1.35(3) . ? C3C C6C' 1.39(3) . ? C4C C5C' 0.60(5) . ? C4C C6C' 1.27(3) . ? C5C C6C 1.33(2) . ? C5C C6C' 1.36(3) . ? C5C C3C' 1.37(3) . ? C5C C4C' 1.38(4) . ? C6C C4C' 0.58(5) . ? C6C C3C' 0.82(3) . ? C3C' C4C' 1.33(6) . ? C6C' C5C' 1.33(4) . ? C1C C2C 1.38(3) . ? C1C N4 3.37(2) 1_565 ? C7C C8C 1.31(3) . ? C7C N3 3.552(18) 2_656 ? C8C N3 3.250(16) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 S3 117.23(12) . 2_755 ? S1 Cu1 S5 121.43(10) . . ? S3 Cu1 S5 115.53(12) 2_755 . ? S1 Cu1 Cu3 93.89(9) . . ? S3 Cu1 Cu3 143.58(9) 2_755 . ? S5 Cu1 Cu3 52.50(9) . . ? S1 Cu1 Cu2 51.39(8) . . ? S3 Cu1 Cu2 93.85(10) 2_755 . ? S5 Cu1 Cu2 143.91(10) . . ? Cu3 Cu1 Cu2 91.43(6) . . ? S1 Cu1 Cu4 140.89(10) . 2_755 ? S3 Cu1 Cu4 49.96(8) 2_755 2_755 ? S5 Cu1 Cu4 93.25(8) . 2_755 ? Cu3 Cu1 Cu4 94.07(6) . 2_755 ? Cu2 Cu1 Cu4 90.19(6) . 2_755 ? S1 Cu2 S4 117.14(12) . 2_755 ? S1 Cu2 S6 117.13(10) . 2_755 ? S4 Cu2 S6 121.28(12) 2_755 2_755 ? S1 Cu2 Cu1 51.01(8) . . ? S4 Cu2 Cu1 93.04(9) 2_755 . ? S6 Cu2 Cu1 139.43(10) 2_755 . ? S1 Cu2 Cu4 92.21(9) . . ? S4 Cu2 Cu4 143.40(9) 2_755 . ? S6 Cu2 Cu4 50.56(9) 2_755 . ? Cu1 Cu2 Cu4 89.13(6) . . ? S1 Cu2 Cu3 140.87(10) . 2_755 ? S4 Cu2 Cu3 50.46(8) 2_755 2_755 ? S6 Cu2 Cu3 95.63(8) 2_755 2_755 ? Cu1 Cu2 Cu3 90.33(6) . 2_755 ? Cu4 Cu2 Cu3 93.03(6) . 2_755 ? S4 Cu3 S5 116.38(12) . . ? S4 Cu3 S2 119.07(12) . . ? S5 Cu3 S2 121.68(11) . . ? S4 Cu3 Cu1 137.57(8) . . ? S5 Cu3 Cu1 52.03(9) . . ? S2 Cu3 Cu1 94.26(9) . . ? S4 Cu3 Cu4 91.79(10) . . ? S5 Cu3 Cu4 141.96(10) . . ? S2 Cu3 Cu4 51.00(8) . . ? Cu1 Cu3 Cu4 89.96(6) . . ? S4 Cu3 Cu2 50.36(7) . 2_755 ? S5 Cu3 Cu2 89.51(8) . 2_755 ? S2 Cu3 Cu2 140.94(10) . 2_755 ? Cu1 Cu3 Cu2 87.25(5) . 2_755 ? Cu4 Cu3 Cu2 90.03(6) . 2_755 ? S6 Cu4 S3 115.57(12) 2_755 . ? S6 Cu4 S2 118.90(11) 2_755 . ? S3 Cu4 S2 122.47(12) . . ? S6 Cu4 Cu2 51.60(9) 2_755 . ? S3 Cu4 Cu2 135.14(8) . . ? S2 Cu4 Cu2 94.20(9) . . ? S6 Cu4 Cu3 140.83(10) 2_755 . ? S3 Cu4 Cu3 94.38(10) . . ? S2 Cu4 Cu3 51.31(8) . . ? Cu2 Cu4 Cu3 89.48(6) . . ? S6 Cu4 Cu1 91.45(8) 2_755 2_755 ? S3 Cu4 Cu1 49.82(7) . 2_755 ? S2 Cu4 Cu1 140.71(10) . 2_755 ? Cu2 Cu4 Cu1 85.63(5) . 2_755 ? Cu3 Cu4 Cu1 89.43(6) . 2_755 ? C1 S1 Cu1 108.6(4) . . ? C1 S1 Cu2 108.8(4) . . ? Cu1 S1 Cu2 77.60(9) . . ? C1 S2 Cu4 106.9(3) . . ? C1 S2 Cu3 107.3(3) . . ? Cu4 S2 Cu3 77.69(9) . . ? C2 C1 S2 119.2(8) . . ? C2 C1 S1 116.6(9) . . ? S2 C1 S1 124.2(5) . . ? C1 C2 C3 121.8(10) . . ? C1 C2 C4 120.3(11) . . ? C3 C2 C4 117.8(8) . . ? N2 C3 C2 176.9(13) . . ? N1 C4 C2 177.9(13) . . ? C5 S4 Cu2 110.8(3) . 2_755 ? C5 S4 Cu3 106.8(3) . . ? Cu2 S4 Cu3 79.18(10) 2_755 . ? C5 S3 Cu1 110.6(3) . 2_755 ? C5 S3 Cu4 104.2(3) . . ? Cu1 S3 Cu4 80.22(11) 2_755 . ? C6 C5 S3 119.0(9) . . ? C6 C5 S4 117.8(9) . . ? S3 C5 S4 123.1(6) . . ? C5 C6 C7 121.5(11) . . ? C5 C6 C8 120.2(12) . . ? C7 C6 C8 118.4(10) . . ? N3 C7 C6 178.7(12) . . ? N4 C8 C6 175.8(15) . . ? C9 S5 Cu1 110.1(4) . . ? C9 S5 Cu3 112.2(4) . . ? Cu1 S5 Cu3 75.46(11) . . ? C9 S6 Cu4 111.6(4) . 2_755 ? C9 S6 Cu2 106.3(4) . 2_755 ? Cu4 S6 Cu2 77.84(11) 2_755 2_755 ? C10 C9 S5 119.1(8) . . ? C10 C9 S6 118.9(7) . . ? S5 C9 S6 121.9(7) . . ? C9 C10 C12 121.6(10) . . ? C9 C10 C11 121.1(9) . . ? C12 C10 C11 117.2(11) . . ? N5 C12 C10 174.5(16) . . ? N6 C11 C10 177.2(13) . . ? C3A S1A C1A 100.9(6) . . ? C4A S2A C2A 99.5(6) . . ? C5A S3A C3A 95.2(5) . . ? C5A S4A C4A 94.1(5) . . ? C7A S5A C6A 93.5(6) . . ? C6A S6A C8A 95.3(6) . . ? C2A C1A S1A 115.4(9) . . ? C2A C1A N5 116.5(10) . 1_655 ? S1A C1A N5 114.3(7) . 1_655 ? C2A C1A H1A1 108.4 . . ? S1A C1A H1A1 108.4 . . ? N5 C1A H1A1 90.2 1_655 . ? C2A C1A H1A2 108.4 . . ? S1A C1A H1A2 108.4 . . ? N5 C1A H1A2 17.3 1_655 . ? H1A1 C1A H1A2 107.5 . . ? C1A C2A S2A 115.0(10) . . ? C1A C2A N3 94.8(8) . 2_755 ? S2A C2A N3 113.3(7) . 2_755 ? C1A C2A H2A1 108.5 . . ? S2A C2A H2A1 108.5 . . ? N3 C2A H2A1 14.1 2_755 . ? C1A C2A H2A2 108.5 . . ? S2A C2A H2A2 108.5 . . ? N3 C2A H2A2 116.3 2_755 . ? H2A1 C2A H2A2 107.5 . . ? C4A C3A S1A 129.3(8) . . ? C4A C3A S3A 116.5(8) . . ? S1A C3A S3A 114.1(7) . . ? C3A C4A S4A 117.3(7) . . ? C3A C4A S2A 128.8(8) . . ? S4A C4A S2A 113.9(7) . . ? C6A C5A S3A 123.4(8) . . ? C6A C5A S4A 119.8(9) . . ? S3A C5A S4A 116.8(5) . . ? C5A C6A S6A 124.8(8) . . ? C5A C6A S5A 119.7(9) . . ? S6A C6A S5A 115.5(5) . . ? C8A C7A S5A 118.8(8) . . ? C8A C7A H7A 120.6 . . ? S5A C7A H7A 120.6 . . ? C7A C8A S6A 116.9(9) . . ? C7A C8A N5 84.4(7) . 2_756 ? S6A C8A N5 158.5(8) . 2_756 ? C7A C8A H8A 121.5 . . ? S6A C8A H8A 121.5 . . ? N5 C8A H8A 37.2 2_756 . ? C3B S1B C1B 100.3(6) . . ? C4B S2B C2B 100.3(6) . . ? C5B S4B C4B 95.7(6) . . ? C5B S3B C3B 94.6(5) . . ? C7B S5B C6B 95.7(7) . . ? C8B S6B C6B 94.3(7) . . ? C2B C1B S1B 115.3(10) . . ? C2B C1B N4 75.2(8) . 2_755 ? S1B C1B N4 108.6(7) . 2_755 ? C2B C1B H1B1 108.5 . . ? S1B C1B H1B1 108.5 . . ? N4 C1B H1B1 136.2 2_755 . ? C2B C1B H1B2 108.5 . . ? S1B C1B H1B2 108.5 . . ? N4 C1B H1B2 37.6 2_755 . ? H1B1 C1B H1B2 107.5 . . ? C1B C2B S2B 113.9(9) . . ? C1B C2B H2B1 108.8 . . ? S2B C2B H2B1 108.8 . . ? C1B C2B H2B2 108.8 . . ? S2B C2B H2B2 108.8 . . ? H2B1 C2B H2B2 107.7 . . ? C3B C4B S4B 116.1(8) . . ? C3B C4B S2B 130.6(9) . . ? S4B C4B S2B 113.3(7) . . ? C4B C3B S3B 117.8(8) . . ? C4B C3B S1B 127.5(8) . . ? S3B C3B S1B 114.7(7) . . ? C6B C5B S4B 122.2(9) . . ? C6B C5B S3B 122.0(9) . . ? S4B C5B S3B 115.8(6) . . ? C5B C6B S5B 124.3(10) . . ? C5B C6B S6B 120.9(9) . . ? S5B C6B S6B 114.8(6) . . ? C7B C8B S6B 118.4(10) . . ? C7B C8B N6 90.7(8) . 1_556 ? S6B C8B N6 150.3(8) . 1_556 ? C7B C8B H8B 120.8 . . ? S6B C8B H8B 120.8 . . ? N6 C8B H8B 30.6 1_556 . ? C8B C7B S5B 116.8(10) . . ? C8B C7B H7B 121.6 . . ? S5B C7B H7B 121.6 . . ? C5C S3C C6C' 47.9(10) . . ? C5C S3C C3C 94.3(10) . . ? C6C' S3C C3C 46.4(12) . . ? C5C S3C C3C' 41.7(11) . . ? C6C' S3C C3C' 89.3(13) . . ? C3C S3C C3C' 135.4(12) . . ? C4C' S6C C8C 109(2) . . ? C4C' S6C C6C 16.8(17) . . ? C8C S6C C6C 93.0(9) . . ? C4C S2C C2C 101.5(11) . . ? C4C S2C C5C' 15.9(12) . . ? C2C S2C C5C' 85.6(14) . . ? C6C' S4C C5C 50.6(12) . . ? C6C' S4C C4C 40.8(13) . . ? C5C S4C C4C 91.4(9) . . ? C6C' S4C C4C' 88.8(16) . . ? C5C S4C C4C' 38.5(14) . . ? C4C S4C C4C' 129.5(14) . . ? C3C' S5C C7C 114.1(16) . . ? C3C' S5C C6C 23.1(12) . . ? C7C S5C C6C 91.3(9) . . ? C3C S1C C1C 107.2(12) . . ? C3C S1C C5C' 22.0(12) . . ? C1C S1C C5C' 86.4(15) . . ? C5C' C3C C4C 14(3) . . ? C5C' C3C C6C' 69(3) . . ? C4C C3C C6C' 55.2(17) . . ? C5C' C3C S1C 109(4) . . ? C4C C3C S1C 122.9(18) . . ? C6C' C3C S1C 177(2) . . ? C5C' C3C S3C 129(4) . . ? C4C C3C S3C 116.2(14) . . ? C6C' C3C S3C 61.0(15) . . ? S1C C3C S3C 120.9(16) . . ? C5C' C4C C6C' 83(5) . . ? C5C' C4C C3C 19(5) . . ? C6C' C4C C3C 64.1(19) . . ? C5C' C4C S2C 115(5) . . ? C6C' C4C S2C 162(2) . . ? C3C C4C S2C 133.1(17) . . ? C5C' C4C S4C 132(5) . . ? C6C' C4C S4C 49.5(15) . . ? C3C C4C S4C 113.6(14) . . ? S2C C4C S4C 113.1(13) . . ? C6C C5C C6C' 174(2) . . ? C6C C5C C3C' 35.5(14) . . ? C6C' C5C C3C' 150(2) . . ? C6C C5C C4C' 24.4(18) . . ? C6C' C5C C4C' 149(3) . . ? C3C' C5C C4C' 58(2) . . ? C6C C5C S3C 119.1(16) . . ? C6C' C5C S3C 66.9(14) . . ? C3C' C5C S3C 84.4(17) . . ? C4C' C5C S3C 142(2) . . ? C6C C5C S4C 116.4(16) . . ? C6C' C5C S4C 57.6(14) . . ? C3C' C5C S4C 150.6(19) . . ? C4C' C5C S4C 93(2) . . ? S3C C5C S4C 124.4(10) . . ? C4C' C6C C3C' 144(6) . . ? C4C' C6C C5C 83(5) . . ? C3C' C6C C5C 75(2) . . ? C4C' C6C S6C 49(5) . . ? C3C' C6C S6C 153(3) . . ? C5C C6C S6C 129.8(19) . . ? C4C' C6C S5C 151(5) . . ? C3C' C6C S5C 44(2) . . ? C5C C6C S5C 118.3(18) . . ? S6C C6C S5C 111.8(9) . . ? C6C C3C' C4C' 15(3) . . ? C6C C3C' C5C 70(3) . . ? C4C' C3C' C5C 61(2) . . ? C6C C3C' S5C 113(3) . . ? C4C' C3C' S5C 123(3) . . ? C5C C3C' S5C 172(2) . . ? C6C C3C' S3C 122(3) . . ? C4C' C3C' S3C 115(2) . . ? C5C C3C' S3C 53.9(12) . . ? S5C C3C' S3C 121(2) . . ? C4C C6C' C5C' 26(2) . . ? C4C C6C' C5C 161(3) . . ? C5C' C6C' C5C 171(3) . . ? C4C C6C' C3C 60.6(18) . . ? C5C' C6C' C3C 34(2) . . ? C5C C6C' C3C 138(3) . . ? C4C C6C' S4C 90(2) . . ? C5C' C6C' S4C 116(3) . . ? C5C C6C' S4C 71.8(15) . . ? C3C C6C' S4C 150(3) . . ? C4C C6C' S3C 133(2) . . ? C5C' C6C' S3C 107(3) . . ? C5C C6C' S3C 65.2(14) . . ? C3C C6C' S3C 72.6(18) . . ? S4C C6C' S3C 136.8(17) . . ? C4C C5C' C3C 146(8) . . ? C4C C5C' C6C' 71(5) . . ? C3C C5C' C6C' 77(4) . . ? C4C C5C' S2C 49(4) . . ? C3C C5C' S2C 160(4) . . ? C6C' C5C' S2C 120(4) . . ? C4C C5C' S1C 161(5) . . ? C3C C5C' S1C 48(3) . . ? C6C' C5C' S1C 125(4) . . ? S2C C5C' S1C 113.6(17) . . ? C6C C4C' C3C' 21(4) . . ? C6C C4C' C5C 73(5) . . ? C3C' C4C' C5C 60(2) . . ? C6C C4C' S6C 114(6) . . ? C3C' C4C' S6C 130(3) . . ? C5C C4C' S6C 163(4) . . ? C6C C4C' S4C 120(5) . . ? C3C' C4C' S4C 109(2) . . ? C5C C4C' S4C 48.7(15) . . ? S6C C4C' S4C 119(3) . . ? C2C C1C S1C 116.0(16) . . ? C2C C1C N4 98.9(16) . 1_565 ? S1C C1C N4 101.8(8) . 1_565 ? C8C C7C S5C 120.7(12) . . ? C8C C7C N3 66.1(8) . 2_656 ? S5C C7C N3 173.2(12) . 2_656 ? C1C C2C S2C 116.4(12) . . ? C7C C8C S6C 120.7(11) . . ? C7C C8C N3 92.3(9) . 2_656 ? S6C C8C N3 143.3(10) . 2_656 ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.83 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 1.026 _refine_diff_density_min -1.743 _refine_diff_density_rms 0.174 #===END