# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Iahcene Ouahab' 'Olivier Cador' 'Stephane Golhen' 'Akira Ota' 'Gunzi Saito' 'Yukihiro Yoshida' _publ_contact_author_name 'Dr Iahcene Ouahab' _publ_contact_author_address ; Institut de Chimie de Rennes CNRS - Universite de rennes 1 263 Av. general Leclerc RENNES cedex 35042 FRANCE ; _publ_contact_author_email LAHCENE.OUAHAB@UNIV-RENNES1.FR _publ_contact_author_phone '+33 (0)2 23 23 56 59' _publ_contact_author_fax '+33 (0)2 23 23 62 54' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Paramagnetic transition metal complexes with redox-active ligand: M(hfac)2(EDO-EDT-TTF-py)2; M = CuII, MnII and CuII(hfac)2(EDO-EDT-TTF-py) ; data_1 _database_code_depnum_ccdc_archive 'CCDC 275856' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common EDO-EDT-TTF-Py _chemical_melting_point ? _chemical_formula_moiety 'C15 H11 N O2 S6' _chemical_formula_sum 'C15 H11 N O2 S6' _chemical_formula_weight 429.61 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.4060(3) _cell_length_b 10.5093(3) _cell_length_c 11.5318(5) _cell_angle_alpha 64.758(2) _cell_angle_beta 86.923(2) _cell_angle_gamma 72.444(2) _cell_volume 875.22(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3467 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.630 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 440 _exptl_absorpt_coefficient_mu 0.790 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6367 _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3961 _reflns_number_gt 2953 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+0.6072P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3961 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1381 _refine_ls_wR_factor_gt 0.1236 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S4 S 0.13322(12) 0.33966(10) 0.33390(8) 0.0554(2) Uani 1 1 d . . . S6 S 0.21946(11) 0.52562(10) 0.47206(8) 0.0531(2) Uani 1 1 d . . . S3 S 0.35771(10) 0.44178(10) 0.13339(9) 0.0540(2) Uani 1 1 d . . . S5 S 0.43194(12) 0.63913(11) 0.26196(9) 0.0584(3) Uani 1 1 d . . . S1 S 0.23005(12) 0.34626(10) -0.04210(8) 0.0554(2) Uani 1 1 d . . . S2 S -0.04035(11) 0.23937(11) 0.18981(9) 0.0596(3) Uani 1 1 d . . . O1 O 0.4192(3) 0.8537(3) 0.3297(3) 0.0677(7) Uani 1 1 d . . . O2 O 0.2147(3) 0.7415(3) 0.5379(2) 0.0642(7) Uani 1 1 d . . . C10 C 0.2659(4) 0.4498(3) 0.2713(3) 0.0451(7) Uani 1 1 d . . . C3 C 0.2101(5) 0.1205(4) -0.0884(3) 0.0557(8) Uani 1 1 d . . . C7 C 0.0205(6) 0.1764(6) 0.0658(5) 0.0826(14) Uani 1 1 d . . . H7B H 0.0138 0.0766 0.0985 0.099 Uiso 1 1 calc R . . H7A H -0.0634 0.2377 -0.0067 0.099 Uiso 1 1 calc R . . C11 C 0.2997(4) 0.5291(3) 0.3273(3) 0.0445(6) Uani 1 1 d . . . C4 C 0.1286(5) 0.2007(4) -0.2104(4) 0.0662(10) Uani 1 1 d . . . H4 H 0.0530 0.2948 -0.2340 0.079 Uiso 1 1 calc R . . N1 N 0.2668(4) 0.0077(4) -0.2719(3) 0.0663(8) Uani 1 1 d . . . C8 C 0.2125(4) 0.3685(3) 0.0998(3) 0.0454(7) Uani 1 1 d . . . C1 C 0.3437(5) -0.0664(4) -0.1557(4) 0.0682(10) Uani 1 1 d . . . H1 H 0.4195 -0.1597 -0.1353 0.082 Uiso 1 1 calc R . . C13 C 0.2699(4) 0.6839(4) 0.4510(3) 0.0496(7) Uani 1 1 d . . . C9 C 0.1098(4) 0.3221(3) 0.1911(3) 0.0459(7) Uani 1 1 d . . . C12 C 0.3630(4) 0.7352(4) 0.3566(3) 0.0520(8) Uani 1 1 d . . . C2 C 0.3204(5) -0.0160(4) -0.0620(4) 0.0629(9) Uani 1 1 d . . . H2 H 0.3791 -0.0744 0.0186 0.075 Uiso 1 1 calc R . . C14 C 0.3938(6) 0.8941(5) 0.4344(5) 0.0822(13) Uani 1 1 d . . . H16B H 0.3930 0.9959 0.4027 0.099 Uiso 1 1 calc R . . H16A H 0.4889 0.8332 0.4980 0.099 Uiso 1 1 calc R . . C5 C 0.1610(5) 0.1391(5) -0.2970(4) 0.0693(10) Uani 1 1 d . . . H5 H 0.1042 0.1943 -0.3785 0.083 Uiso 1 1 calc R . . C15 C 0.2441(8) 0.8809(6) 0.4974(5) 0.1029(18) Uani 1 1 d . . . H15B H 0.1493 0.9575 0.4394 0.123 Uiso 1 1 calc R . . H15A H 0.2479 0.8999 0.5723 0.123 Uiso 1 1 calc R . . C6 C 0.1835(6) 0.1742(5) 0.0161(4) 0.0699(10) Uani 1 1 d . . . H6 H 0.2674 0.1022 0.0878 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S4 0.0771(6) 0.0672(5) 0.0444(4) -0.0340(4) 0.0187(4) -0.0401(5) S6 0.0723(5) 0.0634(5) 0.0443(4) -0.0326(4) 0.0174(4) -0.0371(4) S3 0.0582(5) 0.0707(5) 0.0594(5) -0.0459(4) 0.0221(4) -0.0318(4) S5 0.0670(5) 0.0759(6) 0.0608(5) -0.0458(5) 0.0277(4) -0.0401(5) S1 0.0763(6) 0.0630(5) 0.0470(4) -0.0364(4) 0.0204(4) -0.0324(4) S2 0.0658(5) 0.0811(6) 0.0647(6) -0.0515(5) 0.0258(4) -0.0409(5) O1 0.0891(18) 0.0740(17) 0.0730(17) -0.0457(14) 0.0291(14) -0.0526(15) O2 0.0851(17) 0.0777(17) 0.0661(16) -0.0540(14) 0.0310(13) -0.0442(14) C10 0.0499(16) 0.0511(17) 0.0453(16) -0.0292(14) 0.0095(13) -0.0189(14) C3 0.076(2) 0.062(2) 0.0499(19) -0.0372(16) 0.0179(16) -0.0327(18) C7 0.094(3) 0.113(3) 0.100(3) -0.084(3) 0.051(3) -0.063(3) C11 0.0521(17) 0.0493(16) 0.0406(15) -0.0255(13) 0.0080(13) -0.0187(14) C4 0.080(3) 0.057(2) 0.059(2) -0.0318(18) 0.0094(19) -0.0090(19) N1 0.0717(19) 0.086(2) 0.077(2) -0.062(2) 0.0238(17) -0.0355(18) C8 0.0506(16) 0.0518(17) 0.0474(17) -0.0335(14) 0.0103(13) -0.0171(14) C1 0.059(2) 0.064(2) 0.094(3) -0.051(2) 0.010(2) -0.0117(18) C13 0.0578(18) 0.0586(18) 0.0520(18) -0.0370(16) 0.0136(14) -0.0264(16) C9 0.0526(17) 0.0518(17) 0.0470(17) -0.0318(14) 0.0089(13) -0.0198(14) C12 0.0590(19) 0.0605(19) 0.0580(19) -0.0379(16) 0.0152(15) -0.0307(16) C2 0.063(2) 0.065(2) 0.065(2) -0.0330(19) -0.0042(17) -0.0167(18) C14 0.105(3) 0.090(3) 0.099(3) -0.068(3) 0.031(3) -0.057(3) C5 0.081(3) 0.087(3) 0.049(2) -0.038(2) 0.0062(18) -0.026(2) C15 0.164(5) 0.106(4) 0.105(4) -0.084(3) 0.065(4) -0.085(4) C6 0.103(3) 0.074(2) 0.062(2) -0.047(2) 0.029(2) -0.044(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S4 C10 1.756(3) . ? S4 C9 1.761(3) . ? S6 C13 1.754(3) . ? S6 C11 1.757(3) . ? S3 C10 1.754(3) . ? S3 C8 1.762(3) . ? S5 C12 1.750(3) . ? S5 C11 1.756(3) . ? S1 C8 1.742(3) . ? S1 C6 1.799(4) . ? S2 C9 1.739(3) . ? S2 C7 1.808(4) . ? O1 C12 1.371(4) . ? O1 C14 1.427(4) . ? O2 C13 1.373(3) . ? O2 C15 1.431(5) . ? C10 C11 1.346(4) . ? C3 C2 1.366(5) . ? C3 C4 1.380(5) . ? C3 C6 1.515(4) . ? C7 C6 1.454(5) . ? C4 C5 1.380(5) . ? N1 C1 1.311(5) . ? N1 C5 1.315(5) . ? C8 C9 1.345(4) . ? C1 C2 1.374(5) . ? C13 C12 1.323(4) . ? C14 C15 1.432(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 S4 C9 94.14(14) . . ? C13 S6 C11 92.61(14) . . ? C10 S3 C8 93.99(13) . . ? C12 S5 C11 92.62(14) . . ? C8 S1 C6 98.20(16) . . ? C9 S2 C7 102.87(16) . . ? C12 O1 C14 109.5(3) . . ? C13 O2 C15 110.0(3) . . ? C11 C10 S3 122.7(2) . . ? C11 C10 S4 122.9(2) . . ? S3 C10 S4 114.30(16) . . ? C2 C3 C4 116.8(3) . . ? C2 C3 C6 119.0(3) . . ? C4 C3 C6 124.1(3) . . ? C6 C7 S2 119.9(3) . . ? C10 C11 S5 121.9(2) . . ? C10 C11 S6 122.4(2) . . ? S5 C11 S6 115.62(16) . . ? C3 C4 C5 118.9(4) . . ? C1 N1 C5 115.8(3) . . ? C9 C8 S1 126.0(2) . . ? C9 C8 S3 117.2(2) . . ? S1 C8 S3 116.40(17) . . ? N1 C1 C2 124.6(4) . . ? C12 C13 O2 125.1(3) . . ? C12 C13 S6 118.0(2) . . ? O2 C13 S6 116.9(2) . . ? C8 C9 S2 128.3(2) . . ? C8 C9 S4 116.9(2) . . ? S2 C9 S4 114.70(17) . . ? C13 C12 O1 125.7(3) . . ? C13 C12 S5 118.1(2) . . ? O1 C12 S5 116.1(2) . . ? C3 C2 C1 119.4(4) . . ? O1 C14 C15 116.3(3) . . ? N1 C5 C4 124.4(4) . . ? C14 C15 O2 116.0(4) . . ? C7 C6 C3 112.1(3) . . ? C7 C6 S1 115.6(3) . . ? C3 C6 S1 108.6(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.845 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.066 data_2 _database_code_depnum_ccdc_archive 'CCDC 275857' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cu(hfac)2(EDO-EDT-TTF-Py)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H24 Cu F12 N2 O8 S12' _chemical_formula_weight 1336.87 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1085(4) _cell_length_b 11.1210(7) _cell_length_c 16.3628(11) _cell_angle_alpha 91.682(2) _cell_angle_beta 91.014(3) _cell_angle_gamma 93.547(2) _cell_volume 1290.26(14) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25538 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.350 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.721 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 671 _exptl_absorpt_coefficient_mu 1.004 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13073 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4743 _reflns_number_gt 2817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1337P)^2^+1.2437P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4743 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1305 _refine_ls_R_factor_gt 0.0817 _refine_ls_wR_factor_ref 0.2617 _refine_ls_wR_factor_gt 0.2219 _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 C1 C 0.9138(11) 0.6173(8) 0.3465(5) 0.092(2) Uani 1 1 d . . . H1 H 1.0408 0.6083 0.3370 0.110 Uiso 1 1 calc R . . C2 C 0.8095(13) 0.6750(9) 0.2883(5) 0.106(3) Uani 1 1 d . . . H2 H 0.8685 0.7056 0.2424 0.127 Uiso 1 1 calc R . . C3 C 0.6255(13) 0.6867(7) 0.2979(5) 0.090(2) Uani 1 1 d . . . C4 C 0.5512(11) 0.6420(10) 0.3665(7) 0.112(3) Uani 1 1 d . . . H4 H 0.4234 0.6476 0.3761 0.135 Uiso 1 1 calc R . . C5 C 0.6634(11) 0.5875(10) 0.4233(6) 0.106(3) Uani 1 1 d . . . H5 H 0.6077 0.5584 0.4704 0.127 Uiso 1 1 calc R . . C6 C 0.5052(16) 0.7520(9) 0.2384(6) 0.126(4) Uani 1 1 d . . . H6 H 0.6003 0.7767 0.1985 0.151 Uiso 1 1 calc R . . C7 C 0.445(2) 0.8598(10) 0.2608(8) 0.184(7) Uani 1 1 d . . . H7A H 0.5564 0.9087 0.2787 0.220 Uiso 1 1 calc R . . H7B H 0.3706 0.8463 0.3093 0.220 Uiso 1 1 calc R . . C8 C 0.1981(10) 0.7231(6) 0.1359(4) 0.0759(19) Uani 1 1 d . . . C9 C 0.1744(11) 0.8419(7) 0.1458(6) 0.096(3) Uani 1 1 d . . . C10 C -0.1002(10) 0.7621(6) 0.0529(4) 0.0772(19) Uani 1 1 d . . . C11 C -0.2557(10) 0.7516(7) 0.0037(4) 0.0761(18) Uani 1 1 d . . . C12 C -0.5293(9) 0.6776(7) -0.0913(5) 0.0784(19) Uani 1 1 d . . . C13 C -0.5516(10) 0.7912(8) -0.0785(6) 0.095(3) Uani 1 1 d . . . C14 C -0.7951(16) 0.6595(10) -0.1719(9) 0.156(5) Uani 1 1 d . . . H14A H -0.7936 0.6454 -0.2306 0.188 Uiso 1 1 calc R . . H14B H -0.9102 0.6189 -0.1529 0.188 Uiso 1 1 calc R . . C15 C -0.8115(18) 0.7768(12) -0.1591(10) 0.192(7) Uani 1 1 d . . . H15A H -0.9368 0.7845 -0.1378 0.231 Uiso 1 1 calc R . . H15B H -0.8123 0.8113 -0.2129 0.231 Uiso 1 1 calc R . . C16 C 1.2641(19) 0.8782(9) 0.5291(9) 0.127(4) Uani 1 1 d . . . C17 C 1.1386(12) 0.7647(7) 0.5448(5) 0.085(2) Uani 1 1 d . . . C18 C 0.9908(13) 0.7726(7) 0.5959(6) 0.095(2) Uani 1 1 d . . . H18 H 0.9756 0.8475 0.6209 0.114 Uiso 1 1 calc R . . C19 C 0.8628(10) 0.6816(7) 0.6142(4) 0.0761(18) Uani 1 1 d . . . C20 C 0.7128(15) 0.7058(10) 0.6747(7) 0.106(3) Uani 1 1 d . . . N1 N 0.8431(7) 0.5753(5) 0.4136(3) 0.0657(13) Uani 1 1 d . . . O1 O -0.6486(8) 0.6011(5) -0.1395(4) 0.1057(19) Uani 1 1 d . . . O2 O -0.6941(9) 0.8523(6) -0.1115(5) 0.133(3) Uani 1 1 d . . . O3 O 1.1901(7) 0.6735(5) 0.5053(3) 0.0842(14) Uani 1 1 d . . . O4 O 0.8513(7) 0.5741(4) 0.5876(3) 0.0755(12) Uani 1 1 d . . . F1 F 1.4355(12) 0.8585(7) 0.5087(7) 0.195(4) Uani 1 1 d . . . F2 F 1.2783(17) 0.9515(9) 0.5885(7) 0.259(6) Uani 1 1 d . . . F3 F 1.2073(15) 0.9339(8) 0.4664(7) 0.217(5) Uani 1 1 d . . . F4 F 0.7423(12) 0.6564(12) 0.7423(5) 0.222(5) Uani 1 1 d . . . F5 F 0.5490(9) 0.6649(8) 0.6519(5) 0.168(3) Uani 1 1 d . . . F6 F 0.6931(15) 0.8159(7) 0.6939(7) 0.239(5) Uani 1 1 d . . . S1 S 0.3698(4) 0.6408(2) 0.17928(17) 0.1259(11) Uani 1 1 d . . . S2 S 0.3162(5) 0.9510(2) 0.2001(2) 0.1553(15) Uani 1 1 d . . . S3 S 0.0347(3) 0.64005(18) 0.07449(14) 0.0973(7) Uani 1 1 d . . . S4 S -0.0233(4) 0.89820(18) 0.10178(18) 0.1131(9) Uani 1 1 d . . . S5 S -0.3373(3) 0.61412(18) -0.04383(13) 0.0911(7) Uani 1 1 d . . . S6 S -0.3888(4) 0.8742(2) -0.0143(2) 0.1334(12) Uani 1 1 d . . . Cu Cu 1.0000 0.5000 0.5000 0.0627(4) Uani 1 2 d S . . 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 C1 0.079(5) 0.123(7) 0.075(5) 0.026(4) -0.002(4) 0.014(4) C2 0.093(6) 0.141(8) 0.088(5) 0.040(5) -0.010(5) 0.023(5) C3 0.098(6) 0.081(5) 0.088(5) 0.004(4) -0.039(4) 0.002(4) C4 0.055(4) 0.156(9) 0.126(8) 0.021(7) -0.019(5) 0.005(5) C5 0.068(5) 0.156(9) 0.093(6) 0.039(6) -0.007(4) -0.008(5) C6 0.141(8) 0.104(7) 0.130(8) -0.006(6) -0.081(7) 0.020(6) C7 0.259(16) 0.090(7) 0.197(12) -0.040(7) -0.149(12) 0.036(9) C8 0.076(4) 0.074(4) 0.077(4) -0.011(3) -0.032(3) 0.017(3) C9 0.085(5) 0.084(5) 0.116(6) -0.026(4) -0.043(5) 0.016(4) C10 0.083(4) 0.066(4) 0.082(4) -0.003(3) -0.022(4) 0.016(3) C11 0.069(4) 0.079(4) 0.081(4) 0.003(3) -0.018(3) 0.015(3) C12 0.057(4) 0.082(5) 0.095(5) -0.007(4) -0.021(3) 0.008(3) C13 0.069(4) 0.085(5) 0.131(7) -0.003(5) -0.043(5) 0.013(4) C14 0.129(8) 0.110(8) 0.225(13) -0.023(8) -0.107(9) 0.018(7) C15 0.157(10) 0.143(10) 0.274(17) -0.064(11) -0.148(12) 0.057(9) C16 0.130(9) 0.076(6) 0.168(11) -0.007(7) -0.009(8) -0.031(6) C17 0.089(5) 0.067(4) 0.096(6) 0.000(4) -0.022(5) -0.008(4) C18 0.105(6) 0.066(5) 0.110(6) -0.015(4) -0.008(5) -0.003(4) C19 0.083(5) 0.076(5) 0.069(4) -0.008(3) -0.017(4) 0.014(4) C20 0.106(7) 0.108(7) 0.102(7) -0.021(5) 0.000(6) 0.010(5) N1 0.058(3) 0.071(3) 0.067(3) 0.005(3) -0.009(2) -0.001(2) O1 0.086(3) 0.097(4) 0.131(5) -0.028(3) -0.049(3) 0.015(3) O2 0.105(4) 0.090(4) 0.203(7) -0.015(4) -0.077(5) 0.029(3) O3 0.082(3) 0.077(3) 0.092(3) 0.007(3) -0.005(3) -0.009(2) O4 0.083(3) 0.067(3) 0.076(3) -0.001(2) -0.002(2) 0.006(2) F1 0.143(6) 0.123(5) 0.312(12) 0.007(6) 0.025(7) -0.060(5) F2 0.330(12) 0.170(7) 0.252(10) -0.104(7) 0.093(9) -0.161(8) F3 0.258(10) 0.149(7) 0.237(10) 0.096(7) -0.047(8) -0.068(6) F4 0.172(7) 0.406(17) 0.100(5) 0.034(7) 0.042(5) 0.087(9) F5 0.100(4) 0.202(7) 0.200(7) -0.063(6) 0.010(5) 0.021(5) F6 0.276(11) 0.127(6) 0.313(12) -0.085(7) 0.147(10) 0.009(6) S1 0.135(2) 0.0966(15) 0.145(2) -0.0453(15) -0.0874(17) 0.0529(15) S2 0.172(3) 0.0831(16) 0.206(3) -0.0288(18) -0.111(3) 0.0173(16) S3 0.1026(15) 0.0714(11) 0.1165(16) -0.0179(10) -0.0540(13) 0.0200(10) S4 0.1151(17) 0.0649(12) 0.157(2) -0.0091(12) -0.0634(16) 0.0157(11) S5 0.0907(13) 0.0771(12) 0.1049(15) -0.0148(10) -0.0405(11) 0.0192(10) S6 0.1153(18) 0.0734(13) 0.209(3) -0.0164(15) -0.089(2) 0.0245(12) Cu 0.0678(7) 0.0586(6) 0.0610(7) 0.0024(5) -0.0100(5) 0.0012(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.302(9) . ? C1 C2 1.393(10) . ? C2 C3 1.334(11) . ? C3 C4 1.345(12) . ? C3 C6 1.516(10) . ? C4 C5 1.391(11) . ? C5 N1 1.305(9) . ? C6 C7 1.341(13) . ? C6 S1 1.773(9) . ? C7 S2 1.730(10) . ? C8 C9 1.348(10) . ? C8 S1 1.725(6) . ? C8 S3 1.727(7) . ? C9 S4 1.728(7) . ? C9 S2 1.740(8) . ? C10 C11 1.352(9) . ? C10 S4 1.744(7) . ? C10 S3 1.750(7) . ? C11 S6 1.736(7) . ? C11 S5 1.756(8) . ? C12 C13 1.295(11) . ? C12 O1 1.384(8) . ? C12 S5 1.754(7) . ? C13 O2 1.366(8) . ? C13 S6 1.750(8) . ? C14 C15 1.327(14) . ? C14 O1 1.368(10) . ? C15 O2 1.364(12) . ? C16 F2 1.249(13) . ? C16 F3 1.286(14) . ? C16 F1 1.298(13) . ? C16 C17 1.531(12) . ? C17 O3 1.264(9) . ? C17 C18 1.359(11) . ? C18 C19 1.362(11) . ? C19 O4 1.257(8) . ? C19 C20 1.498(12) . ? C20 F5 1.268(11) . ? C20 F4 1.269(12) . ? C20 F6 1.272(11) . ? N1 Cu 2.018(5) . ? O3 Cu 2.285(5) . ? O4 Cu 1.986(5) . ? Cu O4 1.986(5) 2_766 ? Cu N1 2.018(5) 2_766 ? Cu O3 2.285(5) 2_766 ? 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 N1 C1 C2 123.6(7) . . ? C3 C2 C1 120.5(8) . . ? C2 C3 C4 116.2(7) . . ? C2 C3 C6 123.2(9) . . ? C4 C3 C6 120.5(9) . . ? C3 C4 C5 120.7(8) . . ? N1 C5 C4 123.1(8) . . ? C7 C6 C3 119.1(8) . . ? C7 C6 S1 124.3(8) . . ? C3 C6 S1 107.3(6) . . ? C6 C7 S2 125.8(8) . . ? C9 C8 S1 128.1(5) . . ? C9 C8 S3 117.0(5) . . ? S1 C8 S3 114.9(4) . . ? C8 C9 S4 118.1(5) . . ? C8 C9 S2 128.7(6) . . ? S4 C9 S2 113.2(4) . . ? C11 C10 S4 122.1(5) . . ? C11 C10 S3 122.8(6) . . ? S4 C10 S3 115.0(4) . . ? C10 C11 S6 121.3(6) . . ? C10 C11 S5 122.5(5) . . ? S6 C11 S5 116.2(4) . . ? C13 C12 O1 124.4(6) . . ? C13 C12 S5 118.6(5) . . ? O1 C12 S5 117.0(5) . . ? C12 C13 O2 124.8(7) . . ? C12 C13 S6 118.3(5) . . ? O2 C13 S6 116.9(6) . . ? C15 C14 O1 122.1(9) . . ? C14 C15 O2 125.9(9) . . ? F2 C16 F3 108.2(12) . . ? F2 C16 F1 106.0(11) . . ? F3 C16 F1 101.0(12) . . ? F2 C16 C17 113.8(11) . . ? F3 C16 C17 112.1(10) . . ? F1 C16 C17 114.8(9) . . ? O3 C17 C18 128.6(7) . . ? O3 C17 C16 112.2(9) . . ? C18 C17 C16 119.1(9) . . ? C17 C18 C19 126.4(8) . . ? O4 C19 C18 128.8(7) . . ? O4 C19 C20 112.2(7) . . ? C18 C19 C20 119.0(8) . . ? F5 C20 F4 104.7(11) . . ? F5 C20 F6 104.5(10) . . ? F4 C20 F6 104.6(10) . . ? F5 C20 C19 113.9(8) . . ? F4 C20 C19 111.8(9) . . ? F6 C20 C19 116.3(10) . . ? C1 N1 C5 116.0(6) . . ? C1 N1 Cu 122.8(5) . . ? C5 N1 Cu 121.2(5) . . ? C14 O1 C12 112.0(7) . . ? C15 O2 C13 110.7(7) . . ? C17 O3 Cu 119.5(5) . . ? C19 O4 Cu 128.1(5) . . ? C8 S1 C6 102.4(4) . . ? C7 S2 C9 100.1(5) . . ? C8 S3 C10 95.0(3) . . ? C9 S4 C10 94.6(3) . . ? C12 S5 C11 93.1(3) . . ? C11 S6 C13 93.8(4) . . ? O4 Cu O4 180.000(1) 2_766 . ? O4 Cu N1 89.3(2) 2_766 . ? O4 Cu N1 90.7(2) . . ? O4 Cu N1 90.7(2) 2_766 2_766 ? O4 Cu N1 89.3(2) . 2_766 ? N1 Cu N1 180.0(2) . 2_766 ? O4 Cu O3 92.86(19) 2_766 . ? O4 Cu O3 87.14(19) . . ? N1 Cu O3 87.98(19) . . ? N1 Cu O3 92.02(19) 2_766 . ? O4 Cu O3 87.14(19) 2_766 2_766 ? O4 Cu O3 92.86(19) . 2_766 ? N1 Cu O3 92.02(19) . 2_766 ? N1 Cu O3 87.98(19) 2_766 2_766 ? O3 Cu O3 180.0 . 2_766 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.279 _refine_diff_density_min -0.599 _refine_diff_density_rms 0.082 data_3 _database_code_depnum_ccdc_archive 'CCDC 275858' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Mn(hfac)2(EDO-EDT-TTF-Py)2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H24 F12 Mn N2 O8 S12' _chemical_formula_weight 1328.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.1013(9) _cell_length_b 11.1105(15) _cell_length_c 16.346(3) _cell_angle_alpha 91.662(6) _cell_angle_beta 91.036(7) _cell_angle_gamma 93.650(6) _cell_volume 1286.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17012 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 22.986 _exptl_crystal_description plate _exptl_crystal_colour 'pale red' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 667 _exptl_absorpt_coefficient_mu 0.839 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 KappaCCD _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9051 _diffrn_reflns_av_R_equivalents 0.1496 _diffrn_reflns_av_sigmaI/netI 0.1653 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 22.98 _reflns_number_total 3500 _reflns_number_gt 1522 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1714P)^2^+0.3381P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3500 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2125 _refine_ls_R_factor_gt 0.1056 _refine_ls_wR_factor_ref 0.3400 _refine_ls_wR_factor_gt 0.2637 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 C1 C 0.911(3) 0.6189(18) 0.3437(11) 0.122(6) Uani 1 1 d . . . H1 H 1.0366 0.6078 0.3323 0.146 Uiso 1 1 calc R . . C2 C 0.806(3) 0.6766(19) 0.2900(11) 0.125(6) Uani 1 1 d . . . H2 H 0.8644 0.7108 0.2451 0.150 Uiso 1 1 calc R . . C3 C 0.628(3) 0.6864(14) 0.2982(11) 0.099(5) Uani 1 1 d . . . C4 C 0.548(2) 0.6391(18) 0.3655(14) 0.123(6) Uani 1 1 d . . . H4 H 0.4187 0.6420 0.3731 0.148 Uiso 1 1 calc R . . C5 C 0.659(2) 0.5868(18) 0.4224(11) 0.121(6) Uani 1 1 d . . . H5 H 0.6027 0.5573 0.4694 0.146 Uiso 1 1 calc R . . C6 C 0.502(3) 0.749(2) 0.2384(14) 0.154(8) Uani 1 1 d . . . H6 H 0.5966 0.7748 0.1986 0.185 Uiso 1 1 calc R . . C7 C 0.441(4) 0.8630(17) 0.2632(17) 0.221(14) Uani 1 1 d . . . H7A H 0.5526 0.9118 0.2812 0.265 Uiso 1 1 calc R . . H7B H 0.3649 0.8500 0.3113 0.265 Uiso 1 1 calc R . . C8 C 0.1982(18) 0.7236(12) 0.1341(8) 0.084(4) Uani 1 1 d . . . C9 C 0.176(2) 0.8432(13) 0.1464(11) 0.107(5) Uani 1 1 d . . . C10 C -0.095(2) 0.7612(12) 0.0524(9) 0.083(4) Uani 1 1 d . . . C11 C -0.251(2) 0.7524(12) 0.0047(9) 0.083(4) Uani 1 1 d . . . C12 C -0.5266(18) 0.6776(14) -0.0898(9) 0.086(4) Uani 1 1 d . . . C13 C -0.545(2) 0.7905(16) -0.0787(11) 0.102(5) Uani 1 1 d . . . C14 C -0.799(3) 0.658(2) -0.1700(16) 0.162(9) Uani 1 1 d . . . H14A H -0.8043 0.6426 -0.2287 0.194 Uiso 1 1 calc R . . H14B H -0.9111 0.6168 -0.1482 0.194 Uiso 1 1 calc R . . C15 C -0.818(3) 0.776(3) -0.1579(17) 0.203(13) Uani 1 1 d . . . H15A H -0.9414 0.7842 -0.1349 0.244 Uiso 1 1 calc R . . H15B H -0.8213 0.8107 -0.2117 0.244 Uiso 1 1 calc R . . C16 C 1.261(4) 0.882(2) 0.524(2) 0.144(8) Uani 1 1 d . . . C17 C 1.140(2) 0.7660(15) 0.5435(11) 0.101(5) Uani 1 1 d . . . C18 C 0.990(3) 0.7741(16) 0.5956(12) 0.120(6) Uani 1 1 d . . . H18 H 0.9748 0.8492 0.6204 0.144 Uiso 1 1 calc R . . C19 C 0.863(2) 0.6823(15) 0.6141(9) 0.090(4) Uani 1 1 d . . . C20 C 0.707(4) 0.706(2) 0.6708(12) 0.133(7) Uani 1 1 d . . . N1 N 0.8384(17) 0.5768(9) 0.4133(7) 0.076(3) Uani 1 1 d . . . O1 O -0.6470(16) 0.6012(10) -0.1402(7) 0.115(4) Uani 1 1 d . . . O2 O -0.6937(18) 0.8493(11) -0.1111(9) 0.143(5) Uani 1 1 d . . . O3 O 1.1911(13) 0.6728(9) 0.5051(6) 0.093(3) Uani 1 1 d . . . O4 O 0.8517(13) 0.5743(9) 0.5895(5) 0.088(3) Uani 1 1 d . . . F1 F 1.433(2) 0.8609(13) 0.5132(14) 0.241(9) Uani 1 1 d . . . F2 F 1.275(3) 0.9526(14) 0.5888(11) 0.266(10) Uani 1 1 d . . . F3 F 1.202(3) 0.9305(16) 0.4644(14) 0.243(10) Uani 1 1 d . . . F4 F 0.742(2) 0.657(2) 0.7398(10) 0.244(10) Uani 1 1 d . . . F5 F 0.5424(18) 0.6590(14) 0.6513(9) 0.180(6) Uani 1 1 d . . . F6 F 0.690(2) 0.8150(13) 0.6908(12) 0.237(9) Uani 1 1 d . . . S1 S 0.3712(8) 0.6419(4) 0.1787(3) 0.141(2) Uani 1 1 d . . . S2 S 0.3164(9) 0.9503(5) 0.2008(5) 0.174(3) Uani 1 1 d . . . S3 S 0.0345(6) 0.6400(4) 0.0749(3) 0.1115(16) Uani 1 1 d . . . S4 S -0.0235(7) 0.8980(4) 0.1024(3) 0.1228(17) Uani 1 1 d . . . S5 S -0.3376(6) 0.6142(4) -0.0438(3) 0.1024(14) Uani 1 1 d . . . S6 S -0.3887(8) 0.8735(4) -0.0141(4) 0.146(2) Uani 1 1 d . . . Mn Mn 1.0000 0.5000 0.5000 0.0517(8) Uani 1 2 d S . . 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 C1 0.114(13) 0.169(18) 0.085(12) 0.035(12) 0.004(11) 0.013(12) C2 0.105(15) 0.176(19) 0.097(13) 0.051(12) -0.009(11) 0.021(13) C3 0.101(13) 0.084(10) 0.108(13) 0.004(9) -0.045(11) -0.003(9) C4 0.075(11) 0.153(17) 0.141(16) 0.044(14) -0.016(12) -0.010(11) C5 0.067(11) 0.190(19) 0.108(13) 0.061(12) -0.002(10) -0.013(11) C6 0.139(17) 0.142(18) 0.181(19) 0.011(15) -0.092(14) 0.022(13) C7 0.35(4) 0.061(12) 0.25(3) -0.014(15) -0.15(3) 0.028(17) C8 0.080(9) 0.078(9) 0.094(10) 0.006(8) -0.030(7) 0.013(7) C9 0.100(11) 0.071(10) 0.151(15) -0.005(9) -0.045(10) 0.014(8) C10 0.088(10) 0.073(9) 0.087(9) 0.003(7) -0.030(8) 0.010(7) C11 0.092(10) 0.066(8) 0.092(9) 0.011(7) -0.019(8) 0.012(7) C12 0.065(9) 0.090(11) 0.099(10) -0.014(9) -0.023(7) -0.006(8) C13 0.078(10) 0.093(12) 0.133(13) 0.003(10) -0.026(9) 0.008(9) C14 0.139(18) 0.104(16) 0.24(3) -0.008(16) -0.086(17) 0.010(13) C15 0.17(2) 0.17(2) 0.26(3) -0.05(2) -0.15(2) 0.046(18) C16 0.117(17) 0.084(14) 0.22(3) -0.014(17) -0.014(17) -0.042(13) C17 0.108(13) 0.082(11) 0.113(13) -0.003(10) -0.024(10) 0.020(10) C18 0.111(14) 0.096(13) 0.152(17) -0.012(12) 0.001(13) -0.002(11) C19 0.098(11) 0.087(11) 0.085(11) -0.010(9) 0.007(8) 0.007(9) C20 0.22(3) 0.110(16) 0.073(12) -0.021(11) 0.008(15) 0.001(16) N1 0.080(8) 0.077(7) 0.071(8) 0.007(6) -0.012(6) -0.003(6) O1 0.107(8) 0.109(8) 0.129(9) -0.019(7) -0.044(7) 0.028(7) O2 0.127(10) 0.110(9) 0.192(13) -0.020(9) -0.067(9) 0.031(8) O3 0.090(7) 0.086(7) 0.103(7) 0.013(6) 0.000(5) -0.001(5) O4 0.114(7) 0.080(6) 0.070(6) -0.004(5) -0.002(5) 0.004(5) F1 0.155(12) 0.136(11) 0.43(3) 0.022(14) 0.035(15) -0.054(10) F2 0.38(2) 0.163(12) 0.233(15) -0.092(12) 0.102(15) -0.164(14) F3 0.29(2) 0.164(14) 0.28(2) 0.126(14) -0.053(15) -0.012(12) F4 0.181(13) 0.44(3) 0.124(11) 0.032(14) 0.047(9) 0.086(15) F5 0.130(10) 0.199(13) 0.207(14) -0.058(11) 0.014(9) 0.003(9) F6 0.276(17) 0.123(10) 0.31(2) -0.066(13) 0.132(16) 0.008(11) S1 0.156(4) 0.102(3) 0.163(5) -0.048(3) -0.091(4) 0.049(3) S2 0.192(6) 0.097(4) 0.229(7) -0.037(4) -0.116(5) 0.021(4) S3 0.118(3) 0.078(3) 0.137(4) -0.016(2) -0.054(3) 0.019(2) S4 0.131(4) 0.072(3) 0.163(4) -0.005(3) -0.064(3) 0.012(2) S5 0.100(3) 0.082(3) 0.124(3) -0.012(2) -0.038(2) 0.017(2) S6 0.137(4) 0.076(3) 0.222(6) -0.012(3) -0.089(4) 0.024(3) Mn 0.0564(16) 0.0460(14) 0.0523(15) 0.0040(11) -0.0053(11) 0.0013(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 C1 N1 1.342(18) . ? C1 C2 1.34(2) . ? C2 C3 1.28(2) . ? C3 C4 1.35(2) . ? C3 C6 1.52(2) . ? C4 C5 1.37(2) . ? C5 N1 1.299(17) . ? C6 C7 1.42(2) . ? C6 S1 1.73(2) . ? C7 S2 1.70(2) . ? C8 C9 1.358(18) . ? C8 S3 1.709(13) . ? C8 S1 1.736(13) . ? C9 S2 1.718(15) . ? C9 S4 1.732(15) . ? C10 C11 1.336(18) . ? C10 S3 1.726(14) . ? C10 S4 1.747(13) . ? C11 S6 1.745(14) . ? C11 S5 1.777(14) . ? C12 C13 1.278(19) . ? C12 O1 1.405(15) . ? C12 S5 1.726(15) . ? C13 O2 1.379(18) . ? C13 S6 1.724(16) . ? C14 C15 1.34(3) . ? C14 O1 1.37(2) . ? C15 O2 1.37(2) . ? C16 F3 1.21(3) . ? C16 F1 1.27(2) . ? C16 F2 1.29(3) . ? C16 C17 1.55(3) . ? C17 O3 1.272(16) . ? C17 C18 1.38(2) . ? C18 C19 1.36(2) . ? C19 O4 1.251(16) . ? C19 C20 1.49(2) . ? C20 F6 1.26(2) . ? C20 F5 1.28(2) . ? C20 F4 1.30(2) . ? N1 Mn 2.046(11) . ? O3 Mn 2.278(9) . ? O4 Mn 2.006(9) . ? Mn O4 2.006(9) 2_766 ? Mn N1 2.046(11) 2_766 ? Mn O3 2.278(9) 2_766 ? 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 N1 C1 C2 121.4(17) . . ? C3 C2 C1 122.8(18) . . ? C2 C3 C4 117.3(17) . . ? C2 C3 C6 125(2) . . ? C4 C3 C6 117.9(19) . . ? C3 C4 C5 119.5(16) . . ? N1 C5 C4 122.8(16) . . ? C7 C6 C3 117.3(17) . . ? C7 C6 S1 125.0(15) . . ? C3 C6 S1 109.7(14) . . ? C6 C7 S2 123.3(17) . . ? C9 C8 S3 118.7(11) . . ? C9 C8 S1 126.1(11) . . ? S3 C8 S1 115.0(8) . . ? C8 C9 S2 129.7(12) . . ? C8 C9 S4 116.2(11) . . ? S2 C9 S4 114.1(8) . . ? C11 C10 S3 123.4(11) . . ? C11 C10 S4 120.4(11) . . ? S3 C10 S4 116.0(8) . . ? C10 C11 S6 123.5(11) . . ? C10 C11 S5 122.5(11) . . ? S6 C11 S5 114.0(8) . . ? C13 C12 O1 124.0(14) . . ? C13 C12 S5 118.9(11) . . ? O1 C12 S5 117.0(11) . . ? C12 C13 O2 123.5(14) . . ? C12 C13 S6 119.2(13) . . ? O2 C13 S6 117.2(12) . . ? C15 C14 O1 122.5(18) . . ? C14 C15 O2 123.2(19) . . ? F3 C16 F1 109(3) . . ? F3 C16 F2 114(2) . . ? F1 C16 F2 101(2) . . ? F3 C16 C17 112(2) . . ? F1 C16 C17 111(2) . . ? F2 C16 C17 109(2) . . ? O3 C17 C18 127.8(16) . . ? O3 C17 C16 113.3(18) . . ? C18 C17 C16 118.8(17) . . ? C19 C18 C17 126.0(16) . . ? O4 C19 C18 129.9(14) . . ? O4 C19 C20 110.6(15) . . ? C18 C19 C20 119.5(16) . . ? F6 C20 F5 108(2) . . ? F6 C20 F4 103.5(17) . . ? F5 C20 F4 103(2) . . ? F6 C20 C19 116(2) . . ? F5 C20 C19 117.2(15) . . ? F4 C20 C19 108(2) . . ? C5 N1 C1 116.1(14) . . ? C5 N1 Mn 121.7(11) . . ? C1 N1 Mn 122.2(11) . . ? C14 O1 C12 112.7(13) . . ? C15 O2 C13 113.8(15) . . ? C17 O3 Mn 120.1(10) . . ? C19 O4 Mn 127.1(9) . . ? C6 S1 C8 103.5(8) . . ? C7 S2 C9 101.5(9) . . ? C8 S3 C10 94.4(7) . . ? C9 S4 C10 94.3(7) . . ? C12 S5 C11 93.6(7) . . ? C13 S6 C11 94.2(8) . . ? O4 Mn O4 180.0(3) . 2_766 ? O4 Mn N1 89.5(4) . 2_766 ? O4 Mn N1 90.5(4) 2_766 2_766 ? O4 Mn N1 90.5(4) . . ? O4 Mn N1 89.5(4) 2_766 . ? N1 Mn N1 180.000(2) 2_766 . ? O4 Mn O3 87.3(4) . . ? O4 Mn O3 92.7(4) 2_766 . ? N1 Mn O3 91.8(4) 2_766 . ? N1 Mn O3 88.2(4) . . ? O4 Mn O3 92.7(4) . 2_766 ? O4 Mn O3 87.3(4) 2_766 2_766 ? N1 Mn O3 88.2(4) 2_766 2_766 ? N1 Mn O3 91.8(4) . 2_766 ? O3 Mn O3 180.000(1) . 2_766 ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 22.98 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.691 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.095 data_4 _database_code_depnum_ccdc_archive 'CCDC 275859' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cu(hfac)2(EDO-EDT-TTF-Py) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H13 Cu F12 N O6 S6' _chemical_formula_weight 907.26 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.29370(10) _cell_length_b 15.1897(2) _cell_length_c 24.3174(6) _cell_angle_alpha 92.4610(10) _cell_angle_beta 93.0480(10) _cell_angle_gamma 105.4910(10) _cell_volume 3297.63(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 11398 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 26.022 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1804 _exptl_absorpt_coefficient_mu 1.152 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22071 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0652 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12843 _reflns_number_gt 8037 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+4.4883P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12843 _refine_ls_number_parameters 919 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0632 _refine_ls_wR_factor_ref 0.1846 _refine_ls_wR_factor_gt 0.1553 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Cu1A Cu 0.54474(8) 0.15755(4) 0.20622(3) 0.05180(19) Uani 1 1 d . . . Cu1B Cu 0.97787(8) 0.30071(4) -0.19654(3) 0.0564(2) Uani 1 1 d . . . S2A S 1.08612(16) 0.61003(10) 0.41897(7) 0.0645(4) Uani 1 1 d . . . S1B S 0.75585(18) 0.03607(10) -0.45460(6) 0.0624(4) Uani 1 1 d . . . S4A S 0.99923(16) 0.73417(9) 0.49954(6) 0.0564(3) Uani 1 1 d . . . S4B S 0.49239(16) -0.23869(10) -0.51116(6) 0.0591(4) Uani 1 1 d . . . S3B S 0.77433(16) -0.10745(10) -0.53666(6) 0.0582(4) Uani 1 1 d . . . S5B S 0.79658(16) -0.24427(11) -0.64235(6) 0.0599(4) Uani 1 1 d . . . S3A S 0.71975(16) 0.60054(10) 0.52470(6) 0.0577(4) Uani 1 1 d . . . S2B S 0.42123(16) -0.11875(11) -0.42422(6) 0.0640(4) Uani 1 1 d . . . S1A S 0.75518(19) 0.45292(10) 0.44937(6) 0.0679(4) Uani 1 1 d . . . S6A S 0.97352(17) 0.86320(10) 0.60710(6) 0.0593(4) Uani 1 1 d . . . S5A S 0.69445(17) 0.72703(12) 0.63197(6) 0.0678(4) Uani 1 1 d . . . S6B S 0.51149(17) -0.37226(10) -0.61407(7) 0.0628(4) Uani 1 1 d . . . O6A O 0.4936(4) 0.2544(2) 0.16664(16) 0.0585(9) Uani 1 1 d . . . N1B N 0.8872(5) 0.2245(3) -0.26467(18) 0.0516(10) Uani 1 1 d . . . N1A N 0.6341(5) 0.2427(3) 0.27064(17) 0.0461(9) Uani 1 1 d . . . O3A O 0.5766(4) 0.0532(2) 0.24424(15) 0.0568(9) Uani 1 1 d . . . O6B O 0.9441(5) 0.4121(2) -0.22628(16) 0.0627(10) Uani 1 1 d . . . O4A O 0.4192(5) 0.0754(3) 0.14787(17) 0.0697(11) Uani 1 1 d . . . O3B O 1.0342(5) 0.1986(3) -0.16362(17) 0.0656(10) Uani 1 1 d . . . O4B O 1.0884(5) 0.3821(3) -0.13531(19) 0.0685(11) Uani 1 1 d . . . O5A O 0.7446(4) 0.1740(3) 0.15893(17) 0.0643(10) Uani 1 1 d . . . O5B O 0.7641(5) 0.2882(3) -0.15535(17) 0.0651(10) Uani 1 1 d . . . O2A O 1.0227(4) 0.9151(3) 0.71437(17) 0.0648(10) Uani 1 1 d . . . O1A O 0.7480(4) 0.7844(3) 0.73891(16) 0.0716(11) Uani 1 1 d . . . O2B O 0.4756(5) -0.4481(3) -0.7162(2) 0.0810(13) Uani 1 1 d . . . O1B O 0.7513(5) -0.3219(4) -0.74523(18) 0.0843(14) Uani 1 1 d . . . C12A C 0.8026(6) 0.7961(4) 0.6873(2) 0.0565(13) Uani 1 1 d . . . C10B C 0.6382(6) -0.2111(3) -0.5557(2) 0.0494(12) Uani 1 1 d . . . C9B C 0.5392(6) -0.1314(3) -0.4757(2) 0.0489(12) Uani 1 1 d . . . C25B C 0.6357(8) 0.3494(4) -0.0904(3) 0.0691(16) Uani 1 1 d . . . C13A C 0.9280(6) 0.8557(4) 0.6762(2) 0.0539(13) Uani 1 1 d . . . C1A C 0.7512(6) 0.2327(4) 0.3009(2) 0.0567(14) Uani 1 1 d . . . H1A H 0.7822 0.1800 0.2945 0.068 Uiso 1 1 calc R . . C5A C 0.5884(6) 0.3178(4) 0.2814(3) 0.0595(14) Uani 1 1 d . . . H5A H 0.5066 0.3265 0.2608 0.071 Uiso 1 1 calc R . . C19A C 0.4199(6) -0.0058(4) 0.1377(2) 0.0599(14) Uani 1 1 d . . . C17A C 0.5523(6) -0.0266(3) 0.2213(2) 0.0518(12) Uani 1 1 d . . . C10A C 0.8534(6) 0.7043(3) 0.5438(2) 0.0497(12) Uani 1 1 d . . . C4B C 0.8458(7) 0.0878(4) -0.3218(3) 0.0693(17) Uani 1 1 d . . . H4B H 0.8726 0.0342 -0.3302 0.083 Uiso 1 1 calc R . . C24B C 0.7399(6) 0.3601(4) -0.1374(2) 0.0530(13) Uani 1 1 d . . . C8B C 0.6681(6) -0.0718(3) -0.4870(2) 0.0491(12) Uani 1 1 d . . . C23B C 0.7991(7) 0.4484(4) -0.1546(2) 0.0606(15) Uani 1 1 d . . . H23B H 0.7749 0.4969 -0.1362 0.073 Uiso 1 1 calc R . . C2B C 0.7068(7) 0.1923(4) -0.3410(3) 0.0638(15) Uani 1 1 d . . . H2B H 0.6364 0.2115 -0.3625 0.077 Uiso 1 1 calc R . . C3A C 0.7852(6) 0.3739(4) 0.3522(2) 0.0604(14) Uani 1 1 d . . . C11A C 0.8422(6) 0.7581(4) 0.5882(2) 0.0510(12) Uani 1 1 d . . . C22A C 0.7441(6) 0.2063(4) 0.1132(2) 0.0576(14) Uani 1 1 d . . . C23A C 0.6437(6) 0.2524(4) 0.0903(2) 0.0621(15) Uani 1 1 d . . . H23A H 0.6557 0.2709 0.0545 0.074 Uiso 1 1 calc R . . C2A C 0.8288(7) 0.2962(4) 0.3411(2) 0.0636(15) Uani 1 1 d . . . H2A H 0.9111 0.2864 0.3608 0.076 Uiso 1 1 calc R . . C11B C 0.6471(6) -0.2674(3) -0.5988(2) 0.0508(12) Uani 1 1 d . . . C25A C 0.4275(9) 0.3202(6) 0.0887(3) 0.086(2) Uani 1 1 d . . . C21B C 0.9444(13) 0.5664(5) -0.2131(4) 0.105(3) Uani 1 1 d . . . C8A C 0.8334(6) 0.5634(4) 0.4785(2) 0.0508(12) Uani 1 1 d . . . C24A C 0.5298(6) 0.2714(4) 0.1179(2) 0.0567(13) Uani 1 1 d . . . C1B C 0.7847(7) 0.2471(4) -0.2966(3) 0.0633(15) Uani 1 1 d . . . H1B H 0.7641 0.3027 -0.2888 0.076 Uiso 1 1 calc R . . C20A C 0.3508(10) -0.0455(5) 0.0803(3) 0.087(2) Uani 1 1 d . . . C12B C 0.6938(6) -0.3236(4) -0.6943(2) 0.0576(14) Uani 1 1 d . . . C5B C 0.9192(7) 0.1461(4) -0.2775(3) 0.0649(16) Uani 1 1 d . . . H5B H 0.9930 0.1298 -0.2562 0.078 Uiso 1 1 calc R . . C18A C 0.4783(7) -0.0592(4) 0.1712(3) 0.0680(16) Uani 1 1 d . . . H18A H 0.4674 -0.1199 0.1597 0.082 Uiso 1 1 calc R . . C4A C 0.6605(7) 0.3827(4) 0.3224(3) 0.0663(16) Uani 1 1 d . . . H4A H 0.6241 0.4330 0.3300 0.080 Uiso 1 1 calc R . . C22B C 0.8916(7) 0.4670(4) -0.1974(2) 0.0635(15) Uani 1 1 d . . . C3B C 0.7337(6) 0.1090(4) -0.3533(2) 0.0545(13) Uani 1 1 d . . . C9A C 0.9597(6) 0.6240(3) 0.4667(2) 0.0485(12) Uani 1 1 d . . . C16A C 0.6196(7) -0.0896(4) 0.2549(3) 0.0643(15) Uani 1 1 d . . . C13B C 0.5676(7) -0.3803(4) -0.6815(2) 0.0603(14) Uani 1 1 d . . . C21A C 0.8670(9) 0.1935(7) 0.0784(3) 0.091(2) Uani 1 1 d . . . C6B C 0.6383(7) 0.0435(4) -0.3985(2) 0.0619(14) Uani 1 1 d . . . H6B H 0.5598 0.0706 -0.4122 0.074 Uiso 1 1 calc R . . C7B C 0.5627(7) -0.0474(4) -0.3759(2) 0.0626(15) Uani 1 1 d . . . H7B1 H 0.5171 -0.0365 -0.3422 0.075 Uiso 1 1 calc R . . H7B2 H 0.6375 -0.0794 -0.3668 0.075 Uiso 1 1 calc R . . C19B C 1.1216(6) 0.3570(4) -0.0890(3) 0.0638(15) Uani 1 1 d . . . C7A C 0.9551(8) 0.5301(5) 0.3712(3) 0.086(2) Uani 1 1 d . . . H7A1 H 0.8835 0.5602 0.3560 0.103 Uiso 1 1 calc R . . H7A2 H 1.0090 0.5139 0.3410 0.103 Uiso 1 1 calc R . . C6A C 0.8739(8) 0.4467(5) 0.3952(3) 0.0792(19) Uani 1 1 d . . . H6A H 0.9514 0.4210 0.4114 0.095 Uiso 1 1 calc R . . C18B C 1.1202(7) 0.2710(5) -0.0748(3) 0.0712(17) Uani 1 1 d . . . H18B H 1.1445 0.2610 -0.0384 0.085 Uiso 1 1 calc R . . C17B C 1.0828(7) 0.1982(4) -0.1142(3) 0.0633(15) Uani 1 1 d . . . C15A C 0.9694(12) 0.9021(7) 0.7676(3) 0.135(4) Uani 1 1 d . . . H15A H 1.0527 0.8961 0.7915 0.162 Uiso 1 1 calc R . . H15B H 0.9486 0.9589 0.7797 0.162 Uiso 1 1 calc R . . C16B C 1.1051(11) 0.1067(6) -0.0978(3) 0.092(2) Uani 1 1 d . . . C14A C 0.8542(11) 0.8366(8) 0.7784(3) 0.146(5) Uani 1 1 d . . . H14A H 0.7993 0.8635 0.8041 0.175 Uiso 1 1 calc R . . H14B H 0.8935 0.7936 0.7987 0.175 Uiso 1 1 calc R . . C15B C 0.5429(11) -0.4525(6) -0.7677(3) 0.108(3) Uani 1 1 d . . . H15C H 0.5906 -0.5020 -0.7667 0.130 Uiso 1 1 calc R . . H15D H 0.4628 -0.4696 -0.7966 0.130 Uiso 1 1 calc R . . C14B C 0.6427(13) -0.3790(12) -0.7826(5) 0.244(10) Uani 1 1 d . . . H14C H 0.5866 -0.3406 -0.7995 0.293 Uiso 1 1 calc R . . H14D H 0.6960 -0.3996 -0.8116 0.293 Uiso 1 1 calc R . . C20B C 1.1772(9) 0.4361(6) -0.0457(3) 0.085(2) Uani 1 1 d . . . F1A F 0.7552(4) -0.0880(3) 0.23868(19) 0.0962(13) Uani 1 1 d . . . F2A F 0.6353(6) -0.0683(3) 0.30784(17) 0.1025(14) Uani 1 1 d . . . F12A F 0.4625(5) 0.3416(4) 0.03863(19) 0.1180(18) Uani 1 1 d . . . F3A F 0.5401(5) -0.1760(3) 0.2486(2) 0.1074(15) Uani 1 1 d . . . F6A F 0.2439(5) -0.1213(3) 0.0834(2) 0.1153(16) Uani 1 1 d . . . F12B F 0.5841(7) 0.4178(4) -0.0802(3) 0.156(3) Uani 1 1 d . . . F11B F 0.5284(6) 0.2790(4) -0.0969(3) 0.165(3) Uani 1 1 d . . . F5A F 0.4502(7) -0.0692(5) 0.0511(2) 0.157(3) Uani 1 1 d . . . F7A F 0.9764(6) 0.1796(6) 0.1025(2) 0.175(3) Uani 1 1 d . . . F4A F 0.2970(8) 0.0090(4) 0.0525(2) 0.152(3) Uani 1 1 d . . . F2B F 1.0026(8) 0.0374(3) -0.1235(2) 0.136(2) Uani 1 1 d . . . F11A F 0.4281(10) 0.3958(5) 0.1146(2) 0.177(3) Uani 1 1 d . . . F8B F 0.8982(8) 0.5713(4) -0.2661(3) 0.148(2) Uani 1 1 d . . . F10B F 0.7069(7) 0.3401(6) -0.0448(2) 0.163(3) Uani 1 1 d . . . F10A F 0.2922(6) 0.2719(6) 0.0861(3) 0.189(4) Uani 1 1 d . . . F4B F 1.1148(10) 0.4979(5) -0.0499(3) 0.203(4) Uani 1 1 d . . . F9A F 0.8995(11) 0.2452(8) 0.0413(4) 0.258(6) Uani 1 1 d . . . F9B F 0.8948(11) 0.6223(3) -0.1848(3) 0.232(5) Uani 1 1 d . . . F8A F 0.8226(9) 0.1195(9) 0.0481(4) 0.251(6) Uani 1 1 d . . . F1B F 1.2309(8) 0.0973(5) -0.1124(3) 0.174(3) Uani 1 1 d . . . F6B F 1.1623(10) 0.4124(4) 0.0045(3) 0.186(3) Uani 1 1 d . . . F7B F 1.0883(9) 0.5945(4) -0.2136(4) 0.180(3) Uani 1 1 d . . . F5B F 1.3149(8) 0.4703(6) -0.0449(4) 0.244(5) Uani 1 1 d . . . F3B F 1.0920(7) 0.0941(3) -0.04538(19) 0.1283(19) 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 Cu1A 0.0666(4) 0.0420(3) 0.0440(4) 0.0013(3) -0.0016(3) 0.0110(3) Cu1B 0.0682(4) 0.0497(4) 0.0510(4) -0.0083(3) 0.0014(3) 0.0175(3) S2A 0.0590(8) 0.0618(9) 0.0625(10) -0.0147(7) 0.0177(7) -0.0009(7) S1B 0.0754(9) 0.0508(8) 0.0519(9) -0.0058(6) 0.0106(7) 0.0014(7) S4A 0.0628(8) 0.0452(7) 0.0557(9) -0.0043(6) 0.0117(6) 0.0047(6) S4B 0.0621(8) 0.0503(8) 0.0586(9) -0.0062(6) 0.0132(7) 0.0039(6) S3B 0.0584(8) 0.0536(8) 0.0582(9) -0.0048(6) 0.0156(7) 0.0065(6) S5B 0.0586(8) 0.0669(9) 0.0518(9) -0.0042(7) 0.0065(6) 0.0135(7) S3A 0.0568(8) 0.0584(8) 0.0532(9) -0.0053(6) 0.0116(6) 0.0069(6) S2B 0.0540(8) 0.0728(10) 0.0585(9) -0.0108(7) 0.0128(7) 0.0064(7) S1A 0.0860(10) 0.0498(8) 0.0544(9) -0.0066(6) 0.0177(8) -0.0061(7) S6A 0.0735(9) 0.0497(8) 0.0518(9) -0.0018(6) 0.0082(7) 0.0114(7) S5A 0.0595(9) 0.0860(11) 0.0490(9) -0.0118(7) 0.0062(7) 0.0062(8) S6B 0.0705(9) 0.0526(8) 0.0614(9) -0.0026(7) 0.0109(7) 0.0097(7) O6A 0.075(2) 0.057(2) 0.052(2) 0.0090(18) 0.0118(19) 0.0287(19) N1B 0.058(3) 0.047(2) 0.050(3) -0.0029(19) 0.006(2) 0.014(2) N1A 0.054(2) 0.042(2) 0.042(2) -0.0009(18) 0.0064(19) 0.0114(19) O3A 0.081(3) 0.0389(19) 0.047(2) -0.0018(16) -0.0056(18) 0.0123(18) O6B 0.088(3) 0.050(2) 0.052(2) -0.0033(17) 0.017(2) 0.019(2) O4A 0.086(3) 0.054(2) 0.062(3) 0.0004(19) -0.017(2) 0.012(2) O3B 0.088(3) 0.065(2) 0.050(2) -0.0062(19) 0.000(2) 0.035(2) O4B 0.075(3) 0.058(2) 0.069(3) -0.011(2) -0.001(2) 0.016(2) O5A 0.071(2) 0.075(3) 0.055(3) 0.006(2) 0.0035(19) 0.032(2) O5B 0.080(3) 0.049(2) 0.068(3) -0.0021(19) 0.017(2) 0.018(2) O2A 0.067(2) 0.065(2) 0.057(3) -0.0116(19) 0.0007(19) 0.011(2) O1A 0.062(2) 0.101(3) 0.044(2) -0.006(2) 0.0044(18) 0.009(2) O2B 0.074(3) 0.085(3) 0.076(3) -0.028(2) 0.000(2) 0.014(2) O1B 0.069(3) 0.128(4) 0.053(3) -0.019(3) 0.005(2) 0.025(3) C12A 0.054(3) 0.068(4) 0.046(3) -0.006(3) 0.003(2) 0.016(3) C10B 0.055(3) 0.047(3) 0.046(3) 0.003(2) 0.006(2) 0.013(2) C9B 0.049(3) 0.051(3) 0.044(3) -0.004(2) 0.002(2) 0.010(2) C25B 0.079(4) 0.064(4) 0.066(4) 0.003(3) 0.019(3) 0.020(3) C13A 0.061(3) 0.054(3) 0.046(3) -0.010(2) -0.001(3) 0.017(3) C1A 0.073(4) 0.048(3) 0.050(3) -0.003(2) 0.000(3) 0.020(3) C5A 0.057(3) 0.056(3) 0.065(4) -0.010(3) 0.005(3) 0.016(3) C19A 0.064(3) 0.051(3) 0.057(4) -0.005(3) 0.000(3) 0.003(3) C17A 0.055(3) 0.045(3) 0.053(3) 0.002(2) 0.011(2) 0.009(2) C10A 0.059(3) 0.046(3) 0.046(3) 0.004(2) 0.005(2) 0.016(2) C4B 0.084(4) 0.061(4) 0.069(4) -0.017(3) -0.002(3) 0.036(3) C24B 0.059(3) 0.052(3) 0.046(3) -0.002(2) 0.005(2) 0.012(3) C8B 0.054(3) 0.051(3) 0.043(3) -0.001(2) 0.004(2) 0.015(2) C23B 0.084(4) 0.048(3) 0.056(4) -0.001(3) 0.015(3) 0.027(3) C2B 0.073(4) 0.053(3) 0.065(4) -0.003(3) -0.012(3) 0.020(3) C3A 0.056(3) 0.060(3) 0.055(4) -0.007(3) 0.011(3) -0.001(3) C11A 0.053(3) 0.053(3) 0.047(3) 0.001(2) -0.001(2) 0.014(2) C22A 0.061(3) 0.059(3) 0.052(4) -0.001(3) -0.001(3) 0.016(3) C23A 0.071(4) 0.067(4) 0.051(3) 0.015(3) 0.008(3) 0.021(3) C2A 0.074(4) 0.060(3) 0.054(4) -0.008(3) -0.010(3) 0.017(3) C11B 0.059(3) 0.045(3) 0.047(3) 0.000(2) 0.005(2) 0.012(2) C25A 0.088(5) 0.110(6) 0.075(5) 0.033(4) 0.013(4) 0.048(5) C21B 0.165(9) 0.057(4) 0.101(7) 0.014(4) 0.064(6) 0.033(5) C8A 0.055(3) 0.049(3) 0.045(3) -0.003(2) 0.009(2) 0.009(2) C24A 0.067(3) 0.050(3) 0.054(4) 0.009(3) 0.005(3) 0.015(3) C1B 0.081(4) 0.046(3) 0.065(4) -0.004(3) -0.005(3) 0.022(3) C20A 0.103(6) 0.076(5) 0.068(5) -0.006(4) -0.008(4) 0.007(4) C12B 0.056(3) 0.071(4) 0.048(3) -0.005(3) 0.002(3) 0.021(3) C5B 0.065(4) 0.069(4) 0.065(4) -0.014(3) -0.007(3) 0.031(3) C18A 0.091(4) 0.049(3) 0.061(4) -0.013(3) -0.004(3) 0.018(3) C4A 0.075(4) 0.053(3) 0.071(4) -0.015(3) 0.017(3) 0.018(3) C22B 0.092(4) 0.045(3) 0.054(4) -0.004(3) 0.008(3) 0.021(3) C3B 0.061(3) 0.057(3) 0.043(3) -0.007(2) 0.002(2) 0.013(3) C9A 0.054(3) 0.048(3) 0.040(3) -0.004(2) 0.006(2) 0.007(2) C16A 0.075(4) 0.047(3) 0.075(4) 0.000(3) 0.005(3) 0.022(3) C13B 0.068(4) 0.061(3) 0.053(4) -0.014(3) -0.003(3) 0.023(3) C21A 0.092(5) 0.155(8) 0.044(4) 0.008(5) 0.014(4) 0.059(5) C6B 0.066(3) 0.064(4) 0.052(3) -0.006(3) 0.002(3) 0.013(3) C7B 0.069(4) 0.067(4) 0.045(3) -0.006(3) 0.005(3) 0.008(3) C19B 0.060(3) 0.072(4) 0.059(4) -0.017(3) 0.005(3) 0.022(3) C7A 0.105(5) 0.076(4) 0.053(4) -0.022(3) 0.024(4) -0.016(4) C6A 0.085(4) 0.070(4) 0.068(4) -0.017(3) 0.017(3) -0.004(3) C18B 0.081(4) 0.085(5) 0.049(4) -0.004(3) 0.001(3) 0.028(4) C17B 0.071(4) 0.071(4) 0.053(4) 0.002(3) 0.009(3) 0.027(3) C15A 0.152(8) 0.160(9) 0.039(4) -0.021(5) 0.003(5) -0.049(7) C16B 0.142(7) 0.089(6) 0.067(5) 0.007(4) 0.002(5) 0.068(6) C14A 0.122(7) 0.209(11) 0.043(5) -0.035(6) 0.012(4) -0.057(7) C15B 0.132(7) 0.116(7) 0.061(5) -0.021(5) -0.009(5) 0.014(6) C14B 0.140(9) 0.37(2) 0.105(9) -0.142(12) 0.061(7) -0.114(12) C20B 0.086(5) 0.098(6) 0.070(5) -0.029(4) -0.007(4) 0.030(5) F1A 0.077(2) 0.108(3) 0.117(4) 0.021(3) 0.018(2) 0.046(2) F2A 0.163(4) 0.109(3) 0.062(3) 0.011(2) 0.001(3) 0.083(3) F12A 0.130(4) 0.179(5) 0.080(3) 0.060(3) 0.021(3) 0.090(4) F3A 0.108(3) 0.054(2) 0.154(4) 0.025(2) -0.013(3) 0.012(2) F6A 0.124(4) 0.092(3) 0.099(4) -0.011(3) -0.028(3) -0.016(3) F12B 0.217(6) 0.114(4) 0.183(6) 0.048(4) 0.142(5) 0.095(4) F11B 0.133(4) 0.129(4) 0.194(6) -0.048(4) 0.105(4) -0.040(4) F5A 0.144(5) 0.247(7) 0.070(3) -0.045(4) 0.008(3) 0.044(5) F7A 0.099(4) 0.365(10) 0.097(4) 0.027(5) 0.020(3) 0.121(5) F4A 0.256(7) 0.093(3) 0.090(4) -0.007(3) -0.083(4) 0.038(4) F2B 0.239(7) 0.078(3) 0.102(4) -0.004(3) -0.017(4) 0.068(4) F11A 0.320(10) 0.175(6) 0.112(4) 0.022(4) 0.019(5) 0.197(7) F8B 0.241(7) 0.104(4) 0.124(5) 0.053(3) 0.054(5) 0.075(4) F10B 0.157(5) 0.286(9) 0.069(3) 0.053(4) 0.031(3) 0.088(6) F10A 0.077(3) 0.265(9) 0.241(8) 0.155(7) 0.010(4) 0.055(4) F4B 0.312(10) 0.173(6) 0.156(6) -0.111(5) -0.119(6) 0.164(7) F9A 0.273(9) 0.332(12) 0.298(10) 0.233(10) 0.233(9) 0.227(9) F9B 0.451(12) 0.051(3) 0.227(7) 0.036(3) 0.237(8) 0.080(5) F8A 0.158(6) 0.384(14) 0.205(9) -0.168(10) 0.022(6) 0.089(8) F1B 0.173(5) 0.188(6) 0.224(7) 0.079(5) 0.076(5) 0.138(5) F6B 0.314(10) 0.138(5) 0.077(4) -0.042(4) 0.003(5) 0.020(6) F7B 0.189(7) 0.084(4) 0.240(9) 0.029(4) 0.064(6) -0.024(4) F5B 0.113(5) 0.233(8) 0.320(12) -0.189(8) 0.035(6) -0.039(5) F3B 0.226(6) 0.111(4) 0.066(3) 0.014(3) 0.000(3) 0.076(4) _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 Cu1A O6A 1.939(4) . ? Cu1A O3A 1.950(3) . ? Cu1A O4A 1.956(4) . ? Cu1A N1A 1.982(4) . ? Cu1A O5A 2.200(4) . ? Cu1B O4B 1.950(4) . ? Cu1B O3B 1.954(4) . ? Cu1B O6B 1.961(4) . ? Cu1B N1B 1.990(4) . ? Cu1B O5B 2.239(4) . ? S2A C9A 1.740(5) . ? S2A C7A 1.800(6) . ? S1B C8B 1.755(5) . ? S1B C6B 1.811(6) . ? S4A C10A 1.752(5) . ? S4A C9A 1.761(5) . ? S4B C9B 1.747(5) . ? S4B C10B 1.753(5) . ? S3B C8B 1.755(5) . ? S3B C10B 1.762(5) . ? S5B C12B 1.757(6) . ? S5B C11B 1.761(5) . ? S3A C10A 1.753(5) . ? S3A C8A 1.756(5) . ? S2B C9B 1.744(5) . ? S2B C7B 1.803(6) . ? S1A C8A 1.744(5) . ? S1A C6A 1.778(7) . ? S6A C13A 1.756(6) . ? S6A C11A 1.757(5) . ? S5A C12A 1.759(6) . ? S5A C11A 1.759(6) . ? S6B C13B 1.756(6) . ? S6B C11B 1.758(5) . ? O6A C24A 1.269(6) . ? N1B C1B 1.322(7) . ? N1B C5B 1.332(7) . ? N1A C1A 1.327(7) . ? N1A C5A 1.341(6) . ? O3A C17A 1.270(6) . ? O6B C22B 1.277(6) . ? O4A C19A 1.250(7) . ? O3B C17B 1.262(7) . ? O4B C19B 1.254(7) . ? O5A C22A 1.235(7) . ? O5B C24B 1.238(6) . ? O2A C13A 1.366(6) . ? O2A C15A 1.413(8) . ? O1A C12A 1.379(7) . ? O1A C14A 1.393(8) . ? O2B C13B 1.372(7) . ? O2B C15B 1.435(9) . ? O1B C12B 1.373(7) . ? O1B C14B 1.402(10) . ? C12A C13A 1.319(8) . ? C10B C11B 1.345(7) . ? C9B C8B 1.344(7) . ? C25B F11B 1.251(8) . ? C25B F12B 1.275(7) . ? C25B F10B 1.292(8) . ? C25B C24B 1.523(8) . ? C1A C2A 1.371(8) . ? C5A C4A 1.380(8) . ? C19A C18A 1.364(8) . ? C19A C20A 1.534(9) . ? C17A C18A 1.370(8) . ? C17A C16A 1.521(8) . ? C10A C11A 1.351(7) . ? C4B C3B 1.376(8) . ? C4B C5B 1.387(8) . ? C24B C23B 1.398(7) . ? C23B C22B 1.376(8) . ? C2B C1B 1.377(8) . ? C2B C3B 1.378(7) . ? C3A C2A 1.368(8) . ? C3A C4A 1.374(8) . ? C3A C6A 1.521(8) . ? C22A C23A 1.413(8) . ? C22A C21A 1.506(9) . ? C23A C24A 1.369(8) . ? C25A F10A 1.272(9) . ? C25A F11A 1.284(10) . ? C25A F12A 1.309(8) . ? C25A C24A 1.518(8) . ? C21B F9B 1.265(8) . ? C21B F7B 1.292(11) . ? C21B F8B 1.349(11) . ? C21B C22B 1.529(9) . ? C8A C9A 1.337(7) . ? C20A F4A 1.274(9) . ? C20A F5A 1.308(9) . ? C20A F6A 1.313(8) . ? C12B C13B 1.318(8) . ? C3B C6B 1.521(7) . ? C16A F2A 1.304(7) . ? C16A F3A 1.321(7) . ? C16A F1A 1.334(7) . ? C21A F9A 1.219(9) . ? C21A F7A 1.218(8) . ? C21A F8A 1.275(12) . ? C6B C7B 1.514(8) . ? C19B C18B 1.362(9) . ? C19B C20B 1.524(9) . ? C7A C6A 1.454(9) . ? C18B C17B 1.389(8) . ? C17B C16B 1.526(9) . ? C15A C14A 1.300(11) . ? C16B F1B 1.281(9) . ? C16B F3B 1.304(8) . ? C16B F2B 1.324(10) . ? C15B C14B 1.326(14) . ? C20B F4B 1.233(9) . ? C20B F5B 1.245(9) . ? C20B F6B 1.291(10) . ? 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 O6A Cu1A O3A 174.54(17) . . ? O6A Cu1A O4A 85.03(17) . . ? O3A Cu1A O4A 90.65(16) . . ? O6A Cu1A N1A 91.89(17) . . ? O3A Cu1A N1A 91.71(16) . . ? O4A Cu1A N1A 168.75(18) . . ? O6A Cu1A O5A 89.42(15) . . ? O3A Cu1A O5A 94.06(16) . . ? O4A Cu1A O5A 91.71(18) . . ? N1A Cu1A O5A 99.09(16) . . ? O4B Cu1B O3B 89.46(17) . . ? O4B Cu1B O6B 85.09(17) . . ? O3B Cu1B O6B 173.36(18) . . ? O4B Cu1B N1B 172.67(18) . . ? O3B Cu1B N1B 92.18(17) . . ? O6B Cu1B N1B 92.75(17) . . ? O4B Cu1B O5B 90.19(16) . . ? O3B Cu1B O5B 98.03(16) . . ? O6B Cu1B O5B 85.81(15) . . ? N1B Cu1B O5B 96.65(16) . . ? C9A S2A C7A 97.6(3) . . ? C8B S1B C6B 102.9(3) . . ? C10A S4A C9A 94.2(2) . . ? C9B S4B C10B 95.2(2) . . ? C8B S3B C10B 94.5(2) . . ? C12B S5B C11B 92.4(3) . . ? C10A S3A C8A 94.1(2) . . ? C9B S2B C7B 97.3(3) . . ? C8A S1A C6A 102.3(3) . . ? C13A S6A C11A 91.5(3) . . ? C12A S5A C11A 91.7(3) . . ? C13B S6B C11B 92.1(3) . . ? C24A O6A Cu1A 122.9(3) . . ? C1B N1B C5B 117.7(5) . . ? C1B N1B Cu1B 120.7(4) . . ? C5B N1B Cu1B 121.5(4) . . ? C1A N1A C5A 117.6(5) . . ? C1A N1A Cu1A 121.2(3) . . ? C5A N1A Cu1A 120.7(4) . . ? C17A O3A Cu1A 123.5(4) . . ? C22B O6B Cu1B 121.7(4) . . ? C19A O4A Cu1A 124.8(4) . . ? C17B O3B Cu1B 125.2(4) . . ? C19B O4B Cu1B 125.0(4) . . ? C22A O5A Cu1A 118.5(4) . . ? C24B O5B Cu1B 117.1(4) . . ? C13A O2A C15A 110.4(5) . . ? C12A O1A C14A 109.5(5) . . ? C13B O2B C15B 109.7(6) . . ? C12B O1B C14B 108.4(6) . . ? C13A C12A O1A 125.2(5) . . ? C13A C12A S5A 117.7(4) . . ? O1A C12A S5A 117.1(4) . . ? C11B C10B S4B 122.0(4) . . ? C11B C10B S3B 123.7(4) . . ? S4B C10B S3B 114.2(3) . . ? C8B C9B S2B 127.4(4) . . ? C8B C9B S4B 117.1(4) . . ? S2B C9B S4B 115.2(3) . . ? F11B C25B F12B 108.5(7) . . ? F11B C25B F10B 105.0(7) . . ? F12B C25B F10B 104.8(7) . . ? F11B C25B C24B 113.0(6) . . ? F12B C25B C24B 115.0(6) . . ? F10B C25B C24B 109.9(6) . . ? C12A C13A O2A 124.8(5) . . ? C12A C13A S6A 118.0(4) . . ? O2A C13A S6A 117.1(4) . . ? N1A C1A C2A 123.3(5) . . ? N1A C5A C4A 121.3(5) . . ? O4A C19A C18A 126.9(6) . . ? O4A C19A C20A 114.2(6) . . ? C18A C19A C20A 118.8(6) . . ? O3A C17A C18A 128.1(5) . . ? O3A C17A C16A 113.0(5) . . ? C18A C17A C16A 118.9(5) . . ? C11A C10A S4A 122.8(4) . . ? C11A C10A S3A 122.5(4) . . ? S4A C10A S3A 114.6(3) . . ? C3B C4B C5B 120.2(5) . . ? O5B C24B C23B 127.4(5) . . ? O5B C24B C25B 115.1(5) . . ? C23B C24B C25B 117.5(5) . . ? C9B C8B S3B 117.6(4) . . ? C9B C8B S1B 128.6(4) . . ? S3B C8B S1B 113.6(3) . . ? C22B C23B C24B 123.2(5) . . ? C1B C2B C3B 119.7(5) . . ? C2A C3A C4A 116.8(5) . . ? C2A C3A C6A 120.6(6) . . ? C4A C3A C6A 122.7(6) . . ? C10A C11A S6A 123.0(4) . . ? C10A C11A S5A 122.1(4) . . ? S6A C11A S5A 114.9(3) . . ? O5A C22A C23A 128.2(5) . . ? O5A C22A C21A 114.4(5) . . ? C23A C22A C21A 117.4(6) . . ? C24A C23A C22A 123.8(6) . . ? C3A C2A C1A 120.0(6) . . ? C10B C11B S6B 121.6(4) . . ? C10B C11B S5B 123.1(4) . . ? S6B C11B S5B 115.2(3) . . ? F10A C25A F11A 105.5(8) . . ? F10A C25A F12A 108.1(8) . . ? F11A C25A F12A 105.6(7) . . ? F10A C25A C24A 110.9(7) . . ? F11A C25A C24A 112.2(7) . . ? F12A C25A C24A 114.1(6) . . ? F9B C21B F7B 110.6(10) . . ? F9B C21B F8B 106.7(9) . . ? F7B C21B F8B 102.9(7) . . ? F9B C21B C22B 114.8(7) . . ? F7B C21B C22B 112.2(8) . . ? F8B C21B C22B 108.8(8) . . ? C9A C8A S1A 128.4(4) . . ? C9A C8A S3A 117.5(4) . . ? S1A C8A S3A 113.8(3) . . ? O6A C24A C23A 129.3(5) . . ? O6A C24A C25A 111.7(5) . . ? C23A C24A C25A 119.1(6) . . ? N1B C1B C2B 123.3(5) . . ? F4A C20A F5A 107.6(8) . . ? F4A C20A F6A 107.8(7) . . ? F5A C20A F6A 105.0(7) . . ? F4A C20A C19A 114.1(6) . . ? F5A C20A C19A 110.6(6) . . ? F6A C20A C19A 111.2(6) . . ? C13B C12B O1B 125.0(5) . . ? C13B C12B S5B 117.6(4) . . ? O1B C12B S5B 117.4(4) . . ? N1B C5B C4B 122.1(5) . . ? C19A C18A C17A 122.4(5) . . ? C3A C4A C5A 120.9(5) . . ? O6B C22B C23B 128.7(5) . . ? O6B C22B C21B 113.6(6) . . ? C23B C22B C21B 117.7(5) . . ? C4B C3B C2B 116.8(5) . . ? C4B C3B C6B 122.7(5) . . ? C2B C3B C6B 120.4(5) . . ? C8A C9A S2A 127.9(4) . . ? C8A C9A S4A 117.0(4) . . ? S2A C9A S4A 114.9(3) . . ? F2A C16A F3A 106.5(6) . . ? F2A C16A F1A 106.9(5) . . ? F3A C16A F1A 105.9(5) . . ? F2A C16A C17A 114.1(5) . . ? F3A C16A C17A 112.7(5) . . ? F1A C16A C17A 110.2(5) . . ? C12B C13B O2B 125.5(6) . . ? C12B C13B S6B 118.6(4) . . ? O2B C13B S6B 115.9(5) . . ? F9A C21A F7A 112.7(9) . . ? F9A C21A F8A 97.1(9) . . ? F7A C21A F8A 99.6(9) . . ? F9A C21A C22A 116.6(7) . . ? F7A C21A C22A 116.9(6) . . ? F8A C21A C22A 110.5(8) . . ? C7B C6B C3B 110.9(5) . . ? C7B C6B S1B 114.6(4) . . ? C3B C6B S1B 107.8(4) . . ? C6B C7B S2B 112.3(4) . . ? O4B C19B C18B 128.1(6) . . ? O4B C19B C20B 113.2(6) . . ? C18B C19B C20B 118.7(6) . . ? C6A C7A S2A 114.5(5) . . ? C7A C6A C3A 113.1(6) . . ? C7A C6A S1A 119.7(5) . . ? C3A C6A S1A 107.5(4) . . ? C19B C18B C17B 120.6(6) . . ? O3B C17B C18B 127.5(6) . . ? O3B C17B C16B 114.5(6) . . ? C18B C17B C16B 118.0(6) . . ? C14A C15A O2A 123.6(7) . . ? F1B C16B F3B 110.7(7) . . ? F1B C16B F2B 105.3(7) . . ? F3B C16B F2B 105.2(8) . . ? F1B C16B C17B 111.0(7) . . ? F3B C16B C17B 113.1(6) . . ? F2B C16B C17B 111.2(6) . . ? C15A C14A O1A 124.7(8) . . ? C14B C15B O2B 119.0(8) . . ? C15B C14B O1B 122.7(12) . . ? F4B C20B F5B 108.6(9) . . ? F4B C20B F6B 105.3(7) . . ? F5B C20B F6B 101.1(8) . . ? F4B C20B C19B 114.3(7) . . ? F5B C20B C19B 112.4(6) . . ? F6B C20B C19B 114.0(7) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.885 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.078 #===END