# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_section_title ; Tetranuclear copper(I) clusters: impact of bridging carboxylate ligands on solid state structure and photoluminescence ; _publ_contact_author_name 'Marina A. Petrukhina' _publ_contact_author_address ; Department of Chemistry University at Albany, SUNY 1400 Washington Avenue Albany, NY 12222 ; _publ_contact_author_phone '(518) 4424406' _publ_contact_author_fax '(518) 4423462' _publ_contact_author_email marina@albany.edu loop_ _publ_author_name 'Yulia Sevryugina' 'Oleksandr Hietsoi' 'Marina A. Petrukhina' #===END data_[Cu4(O2C(3-F)C6H4)4]_(1) _database_code_depnum_ccdc_archive 'CCDC 648824' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra-(3-fluorobenzoato-O,O')-tetracopper(I,I,I,I) ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; [Cu4 (O2 C F C6 H4)4] ; _chemical_formula_sum 'C28 H16 Cu4 F4 O8' _chemical_formula_weight 810.57 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' 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' 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 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.1591(18) _cell_length_b 16.0078(16) _cell_length_c 12.3894(13) _cell_angle_alpha 90.00 _cell_angle_beta 129.578(1) _cell_angle_gamma 90.00 _cell_volume 2623.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2161 _cell_measurement_theta_min 3.08 _cell_measurement_theta_max 25.30 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.053 _exptl_crystal_density_method none _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 3.281 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.8531 _exptl_absorpt_correction_T_max 0.8799 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 9452 _diffrn_reflns_av_R_equivalents 0.0693 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.99 _reflns_number_total 2302 _reflns_number_gt 1535 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0602P)^2^+2.5595P] 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 noref _refine_ls_number_reflns 2302 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0933 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.05541(6) 0.37153(5) 0.89890(8) 0.0289(3) Uani 1 1 d . . . Cu2 Cu 0.14956(6) 0.37529(5) 0.78613(9) 0.0310(3) Uani 1 1 d . . . O1 O 0.0855(3) 0.2582(3) 0.9123(5) 0.0284(11) Uani 1 1 d . . . O2 O 0.0342(3) 0.4856(3) 0.9038(4) 0.0286(11) Uani 1 1 d . . . O3 O 0.1666(3) 0.2627(3) 0.8260(5) 0.0290(11) Uani 1 1 d . . . O4 O -0.1359(3) 0.4876(3) 0.7581(5) 0.0311(11) Uani 1 1 d . . . F1 F 0.0930(4) -0.0444(3) 1.0157(5) 0.0587(13) Uani 1 1 d . . . F2 F -0.2210(3) 0.7905(3) 0.6924(5) 0.0615(14) Uani 1 1 d . . . C1 C 0.1311(4) 0.2247(4) 0.8739(7) 0.0267(16) Uani 1 1 d . . . C2 C -0.0503(5) 0.5230(4) 0.8350(7) 0.0248(15) Uani 1 1 d . . . C3 C 0.1436(5) 0.1316(4) 0.8883(6) 0.0257(15) Uani 1 1 d . . . C4 C -0.0479(5) 0.6155(4) 0.8477(6) 0.0228(14) Uani 1 1 d . . . C5 C 0.1097(5) 0.0858(4) 0.9455(7) 0.0280(16) Uani 1 1 d . . . H5 H 0.0764 0.1119 0.9751 0.034 Uiso 1 1 calc R . . C6 C 0.1259(5) 0.0008(4) 0.9582(7) 0.0349(17) Uani 1 1 d . . . C7 C 0.1692(5) -0.0408(4) 0.9135(7) 0.0370(18) Uani 1 1 d . . . H7 H 0.1766 -0.0999 0.9219 0.044 Uiso 1 1 calc R . . C8 C 0.2022(6) 0.0048(5) 0.8556(8) 0.0419(19) Uani 1 1 d . . . H8 H 0.2328 -0.0227 0.8231 0.050 Uiso 1 1 calc R . . C9 C 0.1908(5) 0.0920(4) 0.8444(7) 0.0331(17) Uani 1 1 d . . . H9 H 0.2154 0.1237 0.8069 0.040 Uiso 1 1 calc R . . C10 C -0.1376(5) 0.6607(4) 0.7658(7) 0.0263(15) Uani 1 1 d . . . H10 H -0.2008 0.6328 0.7049 0.032 Uiso 1 1 calc R . . C11 C -0.1331(5) 0.7451(4) 0.7743(7) 0.0318(17) Uani 1 1 d . . . C12 C -0.0446(5) 0.7882(4) 0.8595(7) 0.0318(16) Uani 1 1 d . . . H12 H -0.0444 0.8476 0.8611 0.038 Uiso 1 1 calc R . . C13 C 0.0441(5) 0.7443(4) 0.9428(7) 0.0342(18) Uani 1 1 d . . . H13 H 0.1067 0.7728 1.0053 0.041 Uiso 1 1 calc R . . C14 C 0.0415(5) 0.6580(4) 0.9351(7) 0.0287(16) Uani 1 1 d . . . H14 H 0.1032 0.6276 0.9918 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0339(5) 0.0217(5) 0.0296(5) 0.0013(4) 0.0194(4) 0.0062(4) Cu2 0.0338(5) 0.0219(5) 0.0366(5) 0.0060(4) 0.0221(4) 0.0025(4) O1 0.028(3) 0.023(3) 0.034(3) 0.002(2) 0.020(2) 0.006(2) O2 0.031(3) 0.021(3) 0.029(3) -0.003(2) 0.016(2) 0.003(2) O3 0.031(3) 0.024(3) 0.035(3) 0.005(2) 0.022(3) 0.000(2) O4 0.032(3) 0.025(3) 0.033(3) -0.007(2) 0.019(2) -0.005(2) F1 0.096(4) 0.030(2) 0.071(3) 0.000(2) 0.064(3) -0.013(2) F2 0.041(3) 0.041(3) 0.089(4) 0.015(3) 0.035(3) 0.010(2) C1 0.016(3) 0.023(4) 0.021(4) -0.004(3) 0.003(3) 0.000(3) C2 0.040(4) 0.020(3) 0.026(4) 0.005(3) 0.027(4) 0.009(3) C3 0.021(3) 0.023(4) 0.021(3) -0.007(3) 0.007(3) -0.002(3) C4 0.030(4) 0.019(3) 0.026(3) 0.004(3) 0.021(3) 0.005(3) C5 0.039(4) 0.022(4) 0.030(4) -0.001(3) 0.025(4) 0.009(3) C6 0.040(4) 0.028(4) 0.035(4) 0.000(3) 0.023(4) -0.004(3) C7 0.045(5) 0.017(4) 0.031(4) -0.003(3) 0.016(4) 0.008(3) C8 0.045(5) 0.036(4) 0.041(5) -0.002(4) 0.026(4) 0.010(4) C9 0.031(4) 0.031(4) 0.039(4) -0.001(3) 0.023(4) 0.004(3) C10 0.027(4) 0.023(3) 0.030(4) 0.005(3) 0.018(3) -0.001(3) C11 0.029(4) 0.028(4) 0.040(4) 0.012(3) 0.023(4) 0.012(3) C12 0.038(4) 0.021(4) 0.036(4) -0.003(3) 0.024(4) -0.004(3) C13 0.032(4) 0.031(4) 0.032(4) 0.005(3) 0.017(4) 0.003(3) C14 0.029(4) 0.030(4) 0.026(4) 0.001(3) 0.017(3) 0.002(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 O1 1.865(4) . y Cu1 O2 1.870(4) . y Cu1 Cu2 2.7120(12) 2_556 y Cu1 Cu2 2.7280(11) . y Cu1 Cu1 2.8790(16) 2_556 y Cu2 O3 1.842(4) . y Cu2 O4 1.851(4) 2_556 y Cu2 Cu1 2.7120(12) 2_556 n Cu2 Cu2 4.6142(17) 2_556 y O1 C1 1.265(7) . n O2 C2 1.270(7) . n O3 C1 1.247(7) . n O4 C2 1.266(8) . n O4 Cu2 1.851(4) 2_556 n F1 C6 1.365(8) . n F2 C11 1.372(7) . n C1 C3 1.500(8) . n C2 C4 1.488(8) . n C3 C5 1.380(9) . n C3 C9 1.383(9) . n C4 C14 1.368(9) . n C4 C10 1.389(8) . n C5 C6 1.377(9) . n C6 C7 1.352(10) . n C7 C8 1.373(10) . n C8 C9 1.405(9) . n C10 C11 1.354(8) . n C11 C12 1.362(9) . n C12 C13 1.368(9) . n C13 C14 1.384(9) . n 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 O1 Cu1 O2 174.6(2) . . y O1 Cu1 Cu2 103.49(13) . 2_556 y O2 Cu1 Cu2 80.29(13) . 2_556 y O1 Cu1 Cu2 81.16(13) . . y O2 Cu1 Cu2 100.74(14) . . y Cu2 Cu1 Cu2 116.03(3) 2_556 . y O1 Cu1 Cu1 91.91(14) . 2_556 y O2 Cu1 Cu1 93.35(13) . 2_556 y Cu2 Cu1 Cu1 58.32(3) 2_556 2_556 y Cu2 Cu1 Cu1 57.78(3) . 2_556 y O3 Cu2 O4 176.8(2) . 2_556 y O3 Cu2 Cu1 95.96(13) . 2_556 y O4 Cu2 Cu1 85.40(14) 2_556 2_556 y O3 Cu2 Cu1 83.46(14) . . y O4 Cu2 Cu1 99.71(14) 2_556 . y Cu1 Cu2 Cu1 63.91(3) 2_556 . y O3 Cu2 Cu2 91.10(13) . 2_556 y O4 Cu2 Cu2 91.56(14) 2_556 2_556 y Cu1 Cu2 Cu2 32.09(2) 2_556 2_556 y Cu1 Cu2 Cu2 31.88(2) . 2_556 y C1 O1 Cu1 125.5(4) . . n C2 O2 Cu1 126.9(4) . . n C1 O3 Cu2 124.2(4) . . n C2 O4 Cu2 121.6(4) . 2_556 n O3 C1 O1 125.5(6) . . n O3 C1 C3 117.7(6) . . n O1 C1 C3 116.8(6) . . n O4 C2 O2 125.2(6) . . n O4 C2 C4 117.7(6) . . n O2 C2 C4 117.1(6) . . n C5 C3 C9 120.1(6) . . n C5 C3 C1 121.0(6) . . n C9 C3 C1 118.9(6) . . n C14 C4 C10 118.8(6) . . n C14 C4 C2 121.3(6) . . n C10 C4 C2 119.8(6) . . n C6 C5 C3 117.6(6) . . n C7 C6 F1 118.0(6) . . n C7 C6 C5 124.3(7) . . n F1 C6 C5 117.6(6) . . n C6 C7 C8 117.9(7) . . n C7 C8 C9 120.2(7) . . n C3 C9 C8 119.7(7) . . n C11 C10 C4 118.7(6) . . n C10 C11 C12 123.1(6) . . n C10 C11 F2 119.4(6) . . n C12 C11 F2 117.5(6) . . n C11 C12 C13 118.6(6) . . n C12 C13 C14 119.3(7) . . n C4 C14 C13 121.4(6) . . n _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.852 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.135 _chemical_name_common tetra-(3-fluorobenzoato-O,O')-tetracopper(I,I,I,I) #===END data_[Cu4(O2C(2,3,4-F)3C6H2)4]_(2) _database_code_depnum_ccdc_archive 'CCDC 648825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra-(2,3,4-trifluorobenzoato-O,O')-tetracopper(I,I,I,I) ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; [Cu4 (O2 C F3 C6 H2)4] ; _chemical_formula_sum 'C28 H8 Cu4 F12 O8' _chemical_formula_weight 954.50 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 15.7443(19) _cell_length_b 16.574(2) _cell_length_c 21.682(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5658.1(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5327 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 28.14 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.241 _exptl_crystal_density_method none _exptl_crystal_F_000 3712 _exptl_absorpt_coefficient_mu 3.100 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.7468 _exptl_absorpt_correction_T_max 0.8358 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 11397 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 28.21 _reflns_number_total 1706 _reflns_number_gt 1313 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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^)+(0.0710P)^2^+1.0464P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 1706 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0542 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1074 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 0.53203(3) 0.1250 0.1250 0.03673(18) Uani 1 2 d S . . Cu2 Cu 0.6250 0.1250 0.02094(2) 0.03591(18) Uani 1 2 d S . . O1 O 0.52581(13) 0.01552(11) 0.10732(9) 0.0377(4) Uani 1 1 d . . . O2 O 0.59993(13) 0.01610(11) 0.01892(9) 0.0358(4) Uani 1 1 d . . . F1 F 0.46772(15) -0.12372(10) 0.14736(10) 0.0622(6) Uani 1 1 d . . . F2 F 0.45573(15) -0.28164(11) 0.13094(9) 0.0638(6) Uani 1 1 d . . . F3 F 0.53463(12) -0.35516(10) 0.03761(10) 0.0535(5) Uani 1 1 d . . . C1 C 0.55935(16) -0.01852(15) 0.06180(12) 0.0316(5) Uani 1 1 d . . . C2 C 0.55192(16) -0.10845(15) 0.05643(12) 0.0304(5) Uani 1 1 d . . . C3 C 0.50680(19) -0.15519(16) 0.09833(13) 0.0360(6) Uani 1 1 d . . . C4 C 0.50113(19) -0.23768(16) 0.09085(13) 0.0387(6) Uani 1 1 d . . . C5 C 0.54135(18) -0.27458(16) 0.04285(14) 0.0381(6) Uani 1 1 d . . . C6 C 0.5864(2) -0.23059(17) 0.00051(15) 0.0436(7) Uani 1 1 d . . . C7 C 0.5906(2) -0.14807(18) 0.00757(14) 0.0389(6) Uani 1 1 d . . . H6 H 0.613(2) -0.254(2) -0.0303(16) 0.042(9) Uiso 1 1 d . . . H7 H 0.619(2) -0.117(2) -0.0197(17) 0.044(9) Uiso 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 0.0420(3) 0.0310(3) 0.0372(3) -0.00804(18) 0.000 0.000 Cu2 0.0454(3) 0.0289(3) 0.0334(3) 0.000 0.000 -0.00498(18) O1 0.0448(12) 0.0322(10) 0.0363(10) -0.0057(8) 0.0013(9) -0.0002(8) O2 0.0441(11) 0.0298(9) 0.0336(10) -0.0011(8) -0.0001(8) -0.0046(8) F1 0.0912(16) 0.0429(10) 0.0526(12) -0.0051(8) 0.0398(12) 0.0002(9) F2 0.0842(15) 0.0384(10) 0.0688(14) 0.0067(9) 0.0405(11) -0.0051(10) F3 0.0620(12) 0.0302(8) 0.0683(13) -0.0069(8) 0.0166(10) -0.0058(8) C1 0.0329(13) 0.0326(13) 0.0293(12) -0.0018(10) -0.0045(10) -0.0010(10) C2 0.0307(13) 0.0303(13) 0.0301(13) -0.0020(10) -0.0024(10) 0.0003(10) C3 0.0412(15) 0.0344(14) 0.0323(13) -0.0034(11) 0.0085(12) 0.0016(12) C4 0.0420(15) 0.0357(14) 0.0382(15) 0.0061(11) 0.0095(12) -0.0015(12) C5 0.0385(15) 0.0283(13) 0.0474(16) -0.0032(11) 0.0038(12) -0.0037(10) C6 0.0500(18) 0.0373(15) 0.0434(17) -0.0094(12) 0.0157(14) -0.0042(13) C7 0.0453(16) 0.0366(14) 0.0348(15) -0.0023(12) 0.0114(13) -0.0066(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 O1 1.8573(19) . y Cu1 O1 1.8573(19) 8_544 n Cu1 Cu2 2.6895(6) 11_554 y Cu1 Cu2 2.6895(6) . n Cu1 Cu1 2.9274(11) 14_545 y Cu2 O2 1.8482(18) 14_545 y Cu2 O2 1.8482(18) . n Cu2 Cu1 2.6895(6) 14_545 y Cu2 Cu2 4.5127(11) 11_554 y O1 C1 1.254(3) . n O2 C1 1.266(3) . n F1 C3 1.334(3) . n F2 C4 1.341(3) . n F3 C5 1.345(3) . n C1 C2 1.500(4) . n C2 C7 1.388(4) . n C2 C3 1.389(4) . n C3 C4 1.380(4) . n C4 C5 1.363(4) . n C5 C6 1.370(4) . n C6 C7 1.378(4) . n C6 H6 0.88(3) . n C7 H7 0.91(4) . n 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 O1 Cu1 O1 173.95(13) . 8_544 y O1 Cu1 Cu2 101.64(6) . 11_554 y O1 Cu1 Cu2 81.70(6) 8_544 11_554 n O1 Cu1 Cu2 81.70(6) . . y O1 Cu1 Cu2 101.64(6) 8_544 . n Cu2 Cu1 Cu2 114.06(2) 11_554 . y O1 Cu1 Cu1 93.02(6) . 14_545 y O1 Cu1 Cu1 93.02(6) 8_544 14_545 n Cu2 Cu1 Cu1 57.028(12) 11_554 14_545 n Cu2 Cu1 Cu1 57.028(12) . 14_545 y O2 Cu2 O2 177.29(12) 14_545 . y O2 Cu2 Cu1 84.47(6) 14_545 14_545 y O2 Cu2 Cu1 97.82(6) . 14_545 y O2 Cu2 Cu1 97.82(6) 14_545 . n O2 Cu2 Cu1 84.47(6) . . y Cu1 Cu2 Cu1 65.94(2) 14_545 . y O2 Cu2 Cu2 91.35(6) 14_545 11_554 n O2 Cu2 Cu2 91.35(6) . 11_554 y Cu1 Cu2 Cu2 32.972(12) 14_545 11_554 n Cu1 Cu2 Cu2 32.972(12) . 11_554 y C1 O1 Cu1 125.45(18) . . n C1 O2 Cu2 122.23(17) . . n O1 C1 O2 125.9(3) . . n O1 C1 C2 118.4(2) . . n O2 C1 C2 115.7(2) . . n C7 C2 C3 117.4(2) . . n C7 C2 C1 119.7(2) . . n C3 C2 C1 122.9(2) . . n F1 C3 C4 116.8(2) . . n F1 C3 C2 122.6(2) . . n C4 C3 C2 120.6(2) . . n F2 C4 C5 119.9(2) . . n F2 C4 C3 119.8(2) . . n C5 C4 C3 120.3(2) . . n F3 C5 C4 118.3(2) . . n F3 C5 C6 120.8(3) . . n C4 C5 C6 120.9(3) . . n C5 C6 C7 118.6(3) . . n C5 C6 H6 122(2) . . n C7 C6 H6 120(2) . . n C6 C7 C2 122.2(3) . . n C6 C7 H7 121(2) . . n C2 C7 H7 117(2) . . n _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.21 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.164 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.140 _chemical_name_common tetra-(2,3,4-trifluorobenzoato-O,O')-tetracopper(I,I,I,I) #===END data_[Cu4(O2CC6F5)2(O2CCF3)2]_(3) _database_code_depnum_ccdc_archive 'CCDC 648826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis-(pentafluorobenzoato-O,O')-bis-(trifluoroacetato-O,O')- tetracopper(I,I,I,I) ; _chemical_melting_point 'not measured' _chemical_formula_moiety ; [Cu4 (O2 C C6 F5)2 (O2 C C F3)2] ; _chemical_formula_sum 'C18 Cu4 F16 O8' _chemical_formula_weight 902.34 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' 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' 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 11.4301(8) _cell_length_b 14.4443(11) _cell_length_c 16.7589(12) _cell_angle_alpha 71.969(1) _cell_angle_beta 74.374(1) _cell_angle_gamma 70.565(1) _cell_volume 2438.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5905 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 22.59 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.458 _exptl_crystal_density_method none _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 3.611 _exptl_absorpt_correction_type 'multi-scan (SADABS)' _exptl_absorpt_correction_T_min 0.8125 _exptl_absorpt_correction_T_max 0.8690 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD' _diffrn_measurement_method '0.3 deg wide \w exposures' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'none (area detector data)' _diffrn_standards_interval_count na _diffrn_standards_interval_time na _diffrn_standards_decay_% 0 _diffrn_reflns_number 21451 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.39 _reflns_number_total 10984 _reflns_number_gt 6917 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement 'SMART, SAINT' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-01 (Sheldrick, 2001)' _computing_structure_refinement 'SHELXL-01 (Sheldrick, 2001)' _computing_molecular_graphics 'SHELXP-01 (Sheldrick, 2001)' _computing_publication_material 'SHELXCIF-01 (Sheldrick, 2001)' _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. Disorder of four CF3 groups was modeled using EXYZ and SAME restraints. ; _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^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens na _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef noref _refine_ls_number_reflns 10984 _refine_ls_number_parameters 865 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0538 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1062 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.986 _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 -0.00495(7) 0.32595(5) 0.00662(4) 0.02838(18) Uani 1 1 d . . . Cu2 Cu 0.17251(8) 0.16101(5) -0.04992(4) 0.02988(19) Uani 1 1 d . . . Cu3 Cu 0.22669(7) 0.24636(5) 0.05656(5) 0.02961(19) Uani 1 1 d . . . Cu4 Cu 0.05910(7) 0.42398(6) 0.10299(5) 0.03081(19) Uani 1 1 d . . . O1 O 0.0535(4) 0.3949(3) -0.1055(2) 0.0273(9) Uani 1 1 d . . . O2 O -0.0805(4) 0.2665(3) 0.1163(2) 0.0310(10) Uani 1 1 d . B . O3 O 0.1837(4) 0.2601(3) -0.1522(2) 0.0287(10) Uani 1 1 d . . . O4 O 0.1609(4) 0.0578(3) 0.0485(2) 0.0345(10) Uani 1 1 d . . . O5 O 0.3067(4) 0.3442(3) -0.0170(2) 0.0315(10) Uani 1 1 d . A . O6 O 0.1876(4) 0.1335(3) 0.1380(2) 0.0314(10) Uani 1 1 d . . . O7 O 0.1735(4) 0.4862(3) 0.0197(3) 0.0359(11) Uani 1 1 d . A . O8 O -0.0371(4) 0.3518(3) 0.1922(3) 0.0346(11) Uani 1 1 d . B . F1 F -0.0441(3) 0.5153(3) -0.2525(2) 0.0399(9) Uani 1 1 d . . . F2 F 0.0234(4) 0.6348(3) -0.4051(3) 0.0557(12) Uani 1 1 d . . . F3 F 0.2697(4) 0.6000(3) -0.4847(2) 0.0560(12) Uani 1 1 d . . . F4 F 0.4473(4) 0.4460(3) -0.4089(2) 0.0484(10) Uani 1 1 d . . . F5 F 0.3839(3) 0.3323(3) -0.2531(2) 0.0387(9) Uani 1 1 d . . . F6 F -0.0090(4) -0.0495(3) 0.1402(3) 0.0494(10) Uani 1 1 d . . . F7 F -0.0319(4) -0.2123(3) 0.2666(3) 0.0517(11) Uani 1 1 d . . . F8 F 0.1139(4) -0.2818(3) 0.3872(2) 0.0559(12) Uani 1 1 d . . . F9 F 0.2858(5) -0.1857(3) 0.3799(3) 0.0760(15) Uani 1 1 d . . . F10 F 0.3139(4) -0.0244(3) 0.2524(3) 0.0609(12) Uani 1 1 d . . . C1 C 0.1313(5) 0.3531(4) -0.1621(3) 0.0238(13) Uani 1 1 d . . . C2 C 0.1677(6) 0.0622(4) 0.1210(4) 0.0299(14) Uani 1 1 d . . . C3 C 0.2722(6) 0.4366(4) -0.0198(4) 0.0260(13) Uani 1 1 d . . . C4 C -0.0800(6) 0.2874(4) 0.1830(4) 0.0290(14) Uani 1 1 d . . . C5 C 0.1681(5) 0.4202(4) -0.2480(3) 0.0217(12) Uani 1 1 d . . . C6 C 0.1496(6) -0.0280(4) 0.1926(4) 0.0275(14) Uani 1 1 d . . . C7 C 0.3572(6) 0.5006(5) -0.0833(4) 0.0401(17) Uani 1 1 d D A 1 F11 F 0.3154(7) 0.5280(6) -0.1601(4) 0.0459(19) Uiso 0.65 1 d PD A 1 F12 F 0.4786(6) 0.4493(5) -0.0936(6) 0.045(2) Uiso 0.65 1 d PD A 1 F13 F 0.3444(8) 0.5843(5) -0.0623(6) 0.045(2) Uiso 0.65 1 d PD A 1 F11X F 0.388(4) 0.481(3) -0.1596(16) 0.066(13) Uiso 0.10 1 d PD A 2 F12X F 0.472(2) 0.457(2) -0.056(2) 0.031(9) Uiso 0.10 1 d PD A 2 F13X F 0.320(3) 0.5977(13) -0.093(2) 0.029(10) Uiso 0.10 1 d PD A 2 F11Y F 0.3149(16) 0.5625(13) -0.1504(10) 0.048(5) Uiso 0.25 1 d PD A 3 F12Y F 0.4659(12) 0.4452(10) -0.1203(9) 0.024(4) Uiso 0.25 1 d PD A 3 F13Y F 0.3762(18) 0.5620(13) -0.0408(11) 0.046(6) Uiso 0.25 1 d PD A 3 C8 C -0.1440(7) 0.2255(5) 0.2657(4) 0.0398(17) Uani 1 1 d D B 1 F14 F -0.2654(10) 0.2555(12) 0.2772(11) 0.040(4) Uiso 0.30 1 d PD B 1 F15 F -0.1035(16) 0.1281(8) 0.2595(10) 0.027(4) Uiso 0.30 1 d PD B 1 F16 F -0.1021(16) 0.2255(13) 0.3355(9) 0.054(7) Uiso 0.30 1 d PD B 1 F14X F -0.2556(10) 0.2210(11) 0.2685(11) 0.040(4) Uiso 0.35 1 d PD B 2 F15X F -0.0672(14) 0.1276(8) 0.2798(12) 0.042(5) Uiso 0.35 1 d PD B 2 F16X F -0.1381(16) 0.2494(11) 0.3364(6) 0.018(3) Uiso 0.35 1 d PD B 2 F14Y F -0.2731(9) 0.2467(11) 0.2523(8) 0.023(3) Uiso 0.35 1 d PD B 3 F15Y F -0.1006(18) 0.1289(8) 0.2814(13) 0.036(5) Uiso 0.35 1 d PD B 3 F16Y F -0.1799(13) 0.2697(10) 0.3302(8) 0.045(5) Uiso 0.35 1 d PD B 3 C9 C 0.0794(6) 0.4981(4) -0.2887(4) 0.0296(14) Uani 1 1 d . . . C10 C 0.1111(7) 0.5593(4) -0.3681(4) 0.0347(16) Uani 1 1 d . . . C11 C 0.2364(7) 0.5413(5) -0.4078(4) 0.0369(16) Uani 1 1 d . . . C12 C 0.3258(6) 0.4640(5) -0.3685(4) 0.0306(14) Uani 1 1 d . . . C13 C 0.2920(6) 0.4045(4) -0.2891(4) 0.0267(13) Uani 1 1 d . . . C14 C 0.0659(6) -0.0806(4) 0.1978(4) 0.0308(14) Uani 1 1 d . . . C15 C 0.0512(6) -0.1638(5) 0.2627(4) 0.0351(15) Uani 1 1 d . . . C16 C 0.1259(7) -0.1987(5) 0.3240(4) 0.0385(17) Uani 1 1 d . . . C17 C 0.2128(8) -0.1510(5) 0.3209(4) 0.0464(19) Uani 1 1 d . . . C18 C 0.2245(7) -0.0661(5) 0.2548(4) 0.0359(16) Uani 1 1 d . . . Cu5 Cu 0.25895(7) -0.00416(6) -0.29913(4) 0.02915(19) Uani 1 1 d . . . Cu6 Cu 0.43401(7) -0.10143(6) -0.42202(5) 0.03086(19) Uani 1 1 d . . . Cu7 Cu 0.50046(7) 0.02816(5) -0.36086(5) 0.02987(19) Uani 1 1 d . . . Cu8 Cu 0.31098(8) 0.14278(5) -0.25557(4) 0.02992(19) Uani 1 1 d . . . O9 O 0.1800(4) 0.0642(3) -0.3944(2) 0.0302(10) Uani 1 1 d . C . O10 O 0.2967(4) -0.0780(3) -0.1914(2) 0.0318(10) Uani 1 1 d . . . O11 O 0.3213(4) -0.0103(3) -0.4935(2) 0.0359(11) Uani 1 1 d . C . O12 O 0.5259(4) -0.1973(3) -0.3414(2) 0.0309(10) Uani 1 1 d . D . O13 O 0.4546(4) 0.1479(3) -0.4462(2) 0.0295(10) Uani 1 1 d . . . O14 O 0.5650(4) -0.0923(3) -0.2831(3) 0.0329(10) Uani 1 1 d . D . O15 O 0.3104(4) 0.2388(3) -0.3586(2) 0.0328(10) Uani 1 1 d . . . O16 O 0.3107(4) 0.0504(3) -0.1492(2) 0.0307(10) Uani 1 1 d . . . F23 F 0.5664(3) 0.2949(3) -0.5614(2) 0.0441(10) Uani 1 1 d . . . F24 F 0.5188(4) 0.4521(3) -0.6955(2) 0.0558(12) Uani 1 1 d . . . F25 F 0.2767(4) 0.5598(3) -0.7094(2) 0.0573(12) Uani 1 1 d . . . F26 F 0.0839(4) 0.5099(3) -0.5880(2) 0.0505(11) Uani 1 1 d . . . F27 F 0.1289(3) 0.3481(3) -0.4560(2) 0.0420(9) Uani 1 1 d . . . F28 F 0.5139(3) -0.0570(3) -0.0616(2) 0.0364(9) Uani 1 1 d . . . F29 F 0.5453(4) -0.1704(3) 0.0959(2) 0.0441(10) Uani 1 1 d . . . F30 F 0.3877(4) -0.2858(3) 0.1879(2) 0.0462(10) Uani 1 1 d . . . F31 F 0.1949(4) -0.2861(3) 0.1214(2) 0.0507(11) Uani 1 1 d . . . F32 F 0.1556(4) -0.1661(3) -0.0324(2) 0.0470(10) Uani 1 1 d . . . C19 C 0.2197(6) 0.0478(4) -0.4669(4) 0.0271(13) Uani 1 1 d . . . C20 C 0.5639(6) -0.1762(5) -0.2881(4) 0.0281(14) Uani 1 1 d . . . C21 C 0.3719(6) 0.2286(4) -0.4306(3) 0.0244(13) Uani 1 1 d . . . C22 C 0.3118(5) -0.0402(4) -0.1382(3) 0.0243(13) Uani 1 1 d . . . C23 C 0.1364(6) 0.1104(5) -0.5335(4) 0.0391(17) Uani 1 1 d D C 1 F17 F 0.1466(10) 0.0550(7) -0.5877(6) 0.036(2) Uiso 0.50 1 d PD C 1 F18 F 0.1844(11) 0.1923(7) -0.5793(8) 0.035(3) Uiso 0.50 1 d PD C 1 F19 F 0.0190(9) 0.1489(11) -0.5025(9) 0.034(4) Uiso 0.50 1 d PD C 1 F17X F 0.105(2) 0.0414(13) -0.5627(13) 0.038(6) Uiso 0.20 1 d PD C 2 F18X F 0.1765(18) 0.1693(14) -0.6030(10) 0.037(5) Uiso 0.20 1 d PD C 2 F19X F 0.0298(16) 0.1661(17) -0.4968(15) 0.031(8) Uiso 0.20 1 d PD C 2 F17Y F 0.1681(14) 0.0834(11) -0.6052(8) 0.040(4) Uiso 0.30 1 d PD C 3 F18Y F 0.167(2) 0.2023(13) -0.5623(14) 0.074(10) Uiso 0.30 1 d PD C 3 F19Y F 0.0158(11) 0.1207(13) -0.4994(11) 0.039(5) Uiso 0.30 1 d PD C 3 C24 C 0.6213(7) -0.2667(5) -0.2193(4) 0.0364(16) Uani 1 1 d D D 1 F20 F 0.5693(9) -0.2512(7) -0.1418(4) 0.034(2) Uiso 0.55 1 d PD D 1 F21 F 0.7481(7) -0.2763(8) -0.2299(6) 0.043(2) Uiso 0.55 1 d PD D 1 F22 F 0.6134(10) -0.3550(5) -0.2219(6) 0.046(2) Uiso 0.55 1 d PD D 1 F20X F 0.6116(14) -0.2419(10) -0.1482(7) 0.034(4) Uiso 0.30 1 d PD D 2 F21X F 0.7378(11) -0.3097(11) -0.2439(9) 0.046(4) Uiso 0.30 1 d PD D 2 F22X F 0.5566(13) -0.3401(9) -0.2022(8) 0.035(3) Uiso 0.30 1 d PD D 2 F20Y F 0.547(2) -0.282(2) -0.1437(12) 0.047(9) Uiso 0.15 1 d PD D 3 F21Y F 0.728(2) -0.253(2) -0.206(2) 0.051(10) Uiso 0.15 1 d PD D 3 F22Y F 0.677(2) -0.3528(13) -0.2460(13) 0.022(5) Uiso 0.15 1 d PD D 3 C25 C 0.3483(6) 0.3169(4) -0.5045(3) 0.0271(14) Uani 1 1 d . . . C26 C 0.3342(6) -0.1087(4) -0.0523(3) 0.0247(13) Uani 1 1 d . . . C27 C 0.4460(6) 0.3458(5) -0.5666(4) 0.0284(14) Uani 1 1 d . . . C28 C 0.4232(6) 0.4278(5) -0.6358(4) 0.0339(15) Uani 1 1 d . . . C29 C 0.3011(7) 0.4819(5) -0.6426(4) 0.0379(17) Uani 1 1 d . . . C30 C 0.2022(6) 0.4548(5) -0.5801(4) 0.0343(15) Uani 1 1 d . . . C31 C 0.2265(6) 0.3743(4) -0.5132(4) 0.0285(14) Uani 1 1 d . . . C32 C 0.4312(5) -0.1103(4) -0.0169(4) 0.0252(13) Uani 1 1 d . . . C33 C 0.4504(6) -0.1698(5) 0.0635(4) 0.0312(14) Uani 1 1 d . . . C34 C 0.3709(6) -0.2292(4) 0.1092(4) 0.0326(15) Uani 1 1 d . . . C35 C 0.2731(6) -0.2292(4) 0.0757(4) 0.0320(15) Uani 1 1 d . . . C36 C 0.2547(6) -0.1687(5) -0.0038(4) 0.0289(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 0.0350(4) 0.0285(4) 0.0203(4) -0.0066(3) -0.0006(3) -0.0097(3) Cu2 0.0458(5) 0.0223(4) 0.0173(4) -0.0035(3) -0.0015(3) -0.0085(3) Cu3 0.0361(5) 0.0226(4) 0.0268(4) -0.0028(3) -0.0039(3) -0.0082(3) Cu4 0.0368(5) 0.0276(4) 0.0273(4) -0.0095(3) 0.0057(3) -0.0145(3) O1 0.036(2) 0.021(2) 0.023(2) -0.0082(17) -0.0028(18) -0.0055(18) O2 0.040(3) 0.032(2) 0.024(2) -0.0098(19) 0.0017(19) -0.016(2) O3 0.041(3) 0.019(2) 0.019(2) -0.0081(17) -0.0026(18) 0.0007(18) O4 0.053(3) 0.025(2) 0.019(2) -0.0033(18) 0.001(2) -0.011(2) O5 0.035(3) 0.020(2) 0.029(2) -0.0046(18) 0.0003(19) -0.0008(19) O6 0.039(3) 0.026(2) 0.027(2) -0.0043(19) -0.0024(19) -0.010(2) O7 0.034(3) 0.030(2) 0.038(3) -0.016(2) 0.011(2) -0.011(2) O8 0.045(3) 0.029(2) 0.032(2) -0.013(2) 0.007(2) -0.020(2) F1 0.038(2) 0.037(2) 0.034(2) -0.0086(17) -0.0121(17) 0.0067(17) F2 0.080(3) 0.027(2) 0.048(2) 0.0065(18) -0.033(2) 0.003(2) F3 0.096(3) 0.046(2) 0.027(2) 0.0082(18) -0.012(2) -0.035(2) F4 0.046(2) 0.064(3) 0.035(2) -0.014(2) 0.0101(19) -0.027(2) F5 0.032(2) 0.042(2) 0.035(2) -0.0051(17) -0.0099(17) -0.0028(17) F6 0.044(2) 0.048(3) 0.050(2) 0.007(2) -0.019(2) -0.014(2) F7 0.046(3) 0.043(2) 0.063(3) -0.001(2) -0.003(2) -0.025(2) F8 0.091(3) 0.036(2) 0.034(2) 0.0063(18) -0.005(2) -0.027(2) F9 0.130(5) 0.056(3) 0.055(3) 0.020(2) -0.059(3) -0.040(3) F10 0.085(3) 0.053(3) 0.059(3) 0.009(2) -0.035(2) -0.041(3) C1 0.028(3) 0.025(3) 0.018(3) -0.005(2) -0.001(2) -0.009(3) C2 0.029(4) 0.024(3) 0.026(3) -0.007(3) 0.003(3) 0.000(3) C3 0.026(3) 0.025(3) 0.025(3) -0.007(3) -0.003(3) -0.006(3) C4 0.030(4) 0.024(3) 0.028(3) -0.003(3) 0.002(3) -0.010(3) C5 0.030(3) 0.020(3) 0.017(3) -0.005(2) -0.006(2) -0.006(3) C6 0.036(4) 0.019(3) 0.021(3) -0.005(2) 0.001(3) -0.005(3) C7 0.029(4) 0.042(4) 0.045(4) -0.015(3) 0.009(3) -0.012(3) C8 0.052(5) 0.042(4) 0.031(4) -0.014(3) 0.006(3) -0.025(4) C9 0.036(4) 0.022(3) 0.029(3) -0.011(3) -0.004(3) -0.003(3) C10 0.060(5) 0.016(3) 0.029(3) -0.001(3) -0.021(3) -0.005(3) C11 0.062(5) 0.030(4) 0.020(3) -0.003(3) -0.006(3) -0.019(3) C12 0.036(4) 0.038(4) 0.021(3) -0.009(3) 0.000(3) -0.016(3) C13 0.035(4) 0.026(3) 0.022(3) -0.009(3) -0.006(3) -0.007(3) C14 0.033(4) 0.025(3) 0.024(3) -0.001(3) -0.002(3) -0.002(3) C15 0.034(4) 0.031(4) 0.035(4) -0.009(3) 0.006(3) -0.011(3) C16 0.054(5) 0.022(3) 0.027(3) 0.005(3) 0.001(3) -0.012(3) C17 0.074(6) 0.037(4) 0.028(4) 0.003(3) -0.019(4) -0.017(4) C18 0.051(4) 0.027(3) 0.032(4) -0.002(3) -0.012(3) -0.014(3) Cu5 0.0372(5) 0.0303(4) 0.0202(4) -0.0070(3) -0.0068(3) -0.0075(3) Cu6 0.0355(5) 0.0302(4) 0.0255(4) -0.0103(3) -0.0120(3) 0.0011(3) Cu7 0.0367(5) 0.0241(4) 0.0271(4) -0.0056(3) -0.0094(3) -0.0038(3) Cu8 0.0450(5) 0.0228(4) 0.0175(4) -0.0032(3) -0.0039(3) -0.0066(3) O9 0.033(2) 0.030(2) 0.024(2) -0.0071(18) -0.0047(18) -0.0033(19) O10 0.044(3) 0.030(2) 0.023(2) -0.0095(19) -0.0076(19) -0.008(2) O11 0.038(3) 0.039(3) 0.024(2) -0.011(2) -0.0106(19) 0.005(2) O12 0.040(3) 0.029(2) 0.025(2) -0.0079(19) -0.0139(19) -0.004(2) O13 0.036(3) 0.025(2) 0.024(2) -0.0064(18) -0.0064(18) -0.0019(19) O14 0.040(3) 0.026(2) 0.033(2) -0.0063(19) -0.013(2) -0.006(2) O15 0.051(3) 0.023(2) 0.018(2) -0.0065(17) 0.0003(19) -0.005(2) O16 0.051(3) 0.018(2) 0.019(2) -0.0018(17) -0.0085(19) -0.0055(19) F23 0.034(2) 0.054(3) 0.041(2) -0.013(2) 0.0018(17) -0.0129(19) F24 0.071(3) 0.061(3) 0.036(2) -0.009(2) 0.014(2) -0.042(2) F25 0.093(3) 0.034(2) 0.031(2) 0.0103(18) -0.011(2) -0.018(2) F26 0.055(3) 0.037(2) 0.045(2) 0.0013(19) -0.015(2) 0.001(2) F27 0.035(2) 0.036(2) 0.042(2) 0.0020(18) -0.0011(18) -0.0082(18) F28 0.036(2) 0.040(2) 0.0313(19) 0.0002(17) -0.0059(16) -0.0166(18) F29 0.041(2) 0.048(2) 0.040(2) -0.0036(19) -0.0182(18) -0.0067(19) F30 0.060(3) 0.042(2) 0.0241(19) 0.0079(17) -0.0136(18) -0.008(2) F31 0.066(3) 0.051(3) 0.036(2) 0.0026(19) -0.002(2) -0.036(2) F32 0.055(3) 0.059(3) 0.039(2) -0.003(2) -0.0150(19) -0.033(2) C19 0.027(3) 0.028(3) 0.027(3) -0.008(3) -0.008(3) -0.006(3) C20 0.030(4) 0.027(3) 0.025(3) -0.008(3) -0.003(3) -0.006(3) C21 0.033(4) 0.020(3) 0.021(3) -0.007(2) -0.003(3) -0.009(3) C22 0.020(3) 0.026(3) 0.022(3) -0.008(3) 0.001(2) -0.001(2) C23 0.036(4) 0.046(4) 0.030(4) -0.019(3) -0.006(3) 0.005(3) C24 0.051(5) 0.038(4) 0.024(3) -0.013(3) -0.014(3) -0.005(3) C25 0.045(4) 0.021(3) 0.014(3) -0.007(2) -0.001(3) -0.009(3) C26 0.034(4) 0.015(3) 0.021(3) -0.005(2) -0.005(3) 0.000(2) C27 0.037(4) 0.033(3) 0.019(3) -0.013(3) 0.003(3) -0.014(3) C28 0.046(4) 0.034(4) 0.024(3) -0.014(3) 0.006(3) -0.020(3) C29 0.064(5) 0.023(3) 0.020(3) 0.000(3) -0.005(3) -0.010(3) C30 0.040(4) 0.032(4) 0.027(3) -0.005(3) -0.005(3) -0.008(3) C31 0.034(4) 0.024(3) 0.024(3) 0.000(3) -0.006(3) -0.008(3) C32 0.028(3) 0.022(3) 0.023(3) -0.005(2) -0.001(2) -0.007(3) C33 0.028(4) 0.033(4) 0.030(3) -0.010(3) -0.009(3) -0.001(3) C34 0.043(4) 0.023(3) 0.022(3) -0.005(3) -0.009(3) 0.004(3) C35 0.045(4) 0.019(3) 0.027(3) -0.002(3) -0.003(3) -0.008(3) C36 0.036(4) 0.030(3) 0.024(3) -0.008(3) -0.007(3) -0.010(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 O2 1.878(4) . y Cu1 O1 1.891(4) . y Cu1 O7 2.740(4) 2_565 y Cu1 Cu3 2.7577(11) . y Cu1 Cu2 2.799(1) . y Cu1 Cu4 2.8093(10) . y Cu2 O4 1.858(4) . y Cu2 O3 1.868(4) . y Cu2 O16 2.523(4) . y Cu2 Cu3 2.7483(10) . y Cu2 Cu4 4.8616(10) . y Cu3 O6 1.870(4) . y Cu3 O5 1.878(4) . y Cu3 Cu4 2.8319(10) . y Cu4 O8 1.856(4) . y Cu4 O7 1.868(4) . y Cu4 O1 2.511(4) 2_565 y O1 C1 1.263(6) . n O2 C4 1.248(7) . n O3 C1 1.253(6) . n O3 Cu8 2.610(4) . y O4 C2 1.261(7) . n O5 C3 1.249(6) . n O6 C2 1.252(7) . n O7 C3 1.256(7) . n O8 C4 1.248(7) . n F1 C9 1.349(7) . n F2 C10 1.329(7) . n F3 C11 1.342(7) . n F4 C12 1.348(7) . n F5 C13 1.333(6) . n F6 C14 1.338(7) . n F7 C15 1.334(7) . n F8 C16 1.350(7) . n F9 C17 1.336(8) . n F10 C18 1.335(7) . n C1 C5 1.507(7) . n C2 C6 1.503(8) . n C3 C7 1.537(8) . n C4 C8 1.542(8) . n C5 C13 1.373(8) . n C5 C9 1.378(8) . n C6 C14 1.378(9) . n C6 C18 1.391(8) . n C7 F13 1.313(8) . n C7 F12 1.331(8) . n C7 F11 1.389(9) . n C8 F14 1.287(12) . n C8 F15 1.355(11) . n C8 F16 1.378(12) . n C9 C10 1.382(8) . n C10 C11 1.381(9) . n C11 C12 1.369(9) . n C12 C13 1.377(8) . n C14 C15 1.371(8) . n C15 C16 1.380(9) . n C16 C17 1.366(10) . n C17 C18 1.392(9) . n Cu5 O10 1.872(4) . y Cu5 O9 1.884(4) . y Cu5 Cu8 2.7247(11) . y Cu5 Cu6 2.8142(10) . y Cu5 Cu7 2.8158(11) . y Cu6 O12 1.868(4) . y Cu6 O11 1.885(4) . y Cu6 O13 2.405(4) 2_654 y Cu6 Cu7 2.7721(11) . y Cu6 Cu8 4.7831(10) . y Cu7 O14 1.879(4) . y Cu7 O13 1.892(4) . y Cu7 O11 2.745(4) 2_654 y Cu7 Cu8 2.8122(10) . y Cu8 O15 1.850(4) . y Cu8 O16 1.867(4) . y O9 C19 1.244(6) . n O10 C22 1.253(6) . n O11 C19 1.248(7) . n O12 C20 1.242(7) . n O13 C21 1.282(6) . n O13 Cu6 2.405(4) 2_654 n O14 C20 1.244(7) . n O15 C21 1.247(6) . n O16 C22 1.259(7) . n F23 C27 1.340(7) . n F24 C28 1.329(7) . n F25 C29 1.333(7) . n F26 C30 1.339(7) . n F27 C31 1.338(7) . n F28 C32 1.339(6) . n F29 C33 1.334(7) . n F30 C34 1.345(6) . n F31 C35 1.339(7) . n F32 C36 1.329(7) . n C19 C23 1.531(8) . n C20 C24 1.541(8) . n C21 C25 1.485(8) . n C22 C26 1.506(8) . n C23 F19 1.300(10) . n C23 F17 1.345(9) . n C23 F18 1.390(10) . n C24 F22 1.323(9) . n C24 F20 1.329(8) . n C24 F21 1.377(9) . n C25 C31 1.383(8) . n C25 C27 1.385(8) . n C26 C32 1.381(8) . n C26 C36 1.388(8) . n C27 C28 1.387(8) . n C28 C29 1.370(9) . n C29 C30 1.389(9) . n C30 C31 1.354(8) . n C32 C33 1.386(8) . n C33 C34 1.373(9) . n C34 C35 1.380(9) . n C35 C36 1.375(8) . n 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 O2 Cu1 O1 173.80(18) . . y O2 Cu1 O7 100.03(15) . 2_565 y O1 Cu1 O7 74.45(14) . 2_565 y O2 Cu1 Cu3 89.42(13) . . y O1 Cu1 Cu3 96.50(12) . . y O7 Cu1 Cu3 135.09(10) 2_565 . y O2 Cu1 Cu2 103.44(13) . . y O1 Cu1 Cu2 81.28(11) . . y O7 Cu1 Cu2 152.73(9) 2_565 . y Cu3 Cu1 Cu2 59.28(3) . . y O2 Cu1 Cu4 80.53(12) . . y O1 Cu1 Cu4 100.69(12) . . y O7 Cu1 Cu4 77.15(9) 2_565 . y Cu3 Cu1 Cu4 61.15(3) . . y Cu2 Cu1 Cu4 120.19(4) . . y O4 Cu2 O3 176.88(17) . . y O4 Cu2 O16 97.01(15) . . y O3 Cu2 O16 80.54(14) . . y O4 Cu2 Cu3 82.35(13) . . y O3 Cu2 Cu3 100.72(12) . . y O16 Cu2 Cu3 132.42(10) . . y O4 Cu2 Cu1 100.81(13) . . y O3 Cu2 Cu1 81.33(11) . . y O16 Cu2 Cu1 160.07(9) . . y Cu3 Cu2 Cu1 59.61(3) . . y O4 Cu2 Cu4 94.44(12) . . y O3 Cu2 Cu4 88.54(11) . . y O16 Cu2 Cu4 156.47(10) . . y Cu3 Cu2 Cu4 29.89(2) . . y Cu1 Cu2 Cu4 29.96(2) . . y O6 Cu3 O5 165.26(18) . . y O6 Cu3 Cu2 81.79(13) . . y O5 Cu3 Cu2 104.79(13) . . y O6 Cu3 Cu1 95.94(13) . . y O5 Cu3 Cu1 98.78(13) . . y Cu2 Cu3 Cu1 61.11(3) . . y O6 Cu3 Cu4 108.86(13) . . y O5 Cu3 Cu4 79.34(12) . . y Cu2 Cu3 Cu4 121.19(4) . . y Cu1 Cu3 Cu4 60.33(3) . . y O8 Cu4 O7 172.7(2) . . y O8 Cu4 O1 103.61(16) . 2_565 y O7 Cu4 O1 80.87(15) . 2_565 y O8 Cu4 Cu1 82.39(13) . . y O7 Cu4 Cu1 100.33(13) . . y O1 Cu4 Cu1 121.04(9) 2_565 . y O8 Cu4 Cu3 92.76(13) . . y O7 Cu4 Cu3 83.06(13) . . y O1 Cu4 Cu3 163.50(9) 2_565 . y Cu1 Cu4 Cu3 58.53(3) . . y O8 Cu4 Cu2 90.01(12) . . y O7 Cu4 Cu2 89.17(12) . . y O1 Cu4 Cu2 146.54(9) 2_565 . y Cu1 Cu4 Cu2 29.84(2) . . y Cu3 Cu4 Cu2 28.92(2) . . y C1 O1 Cu1 125.1(4) . . n C4 O2 Cu1 124.3(4) . . n C1 O3 Cu2 126.3(4) . . n C1 O3 Cu8 134.5(3) . . n Cu2 O3 Cu8 98.85(15) . . n C2 O4 Cu2 124.3(4) . . n C3 O5 Cu3 126.5(4) . . n C2 O6 Cu3 124.5(4) . . n C3 O7 Cu4 122.1(4) . . n C4 O8 Cu4 122.9(4) . . n O3 C1 O1 125.4(5) . . n O3 C1 C5 116.7(5) . . n O1 C1 C5 117.9(5) . . n O6 C2 O4 126.3(6) . . n O6 C2 C6 118.3(5) . . n O4 C2 C6 115.3(5) . . n O5 C3 O7 128.8(6) . . n O5 C3 C7 116.6(5) . . n O7 C3 C7 114.5(5) . . n O2 C4 O8 129.5(6) . . n O2 C4 C8 114.6(5) . . n O8 C4 C8 115.9(5) . . n C13 C5 C9 117.7(5) . . n C13 C5 C1 120.8(5) . . n C9 C5 C1 121.5(5) . . n C14 C6 C18 116.6(6) . . n C14 C6 C2 123.1(5) . . n C18 C6 C2 120.2(6) . . n F13 C7 F12 109.1(8) . . n F13 C7 F11 107.5(8) . . n F12 C7 F11 109.5(7) . . n F13 C7 C3 112.9(6) . . n F12 C7 C3 112.6(6) . . n F11 C7 C3 105.0(6) . . n F14 C8 F15 109.8(11) . . n F14 C8 F16 110.6(11) . . n F15 C8 F16 105.5(11) . . n F14 C8 C4 113.1(10) . . n F15 C8 C4 106.6(8) . . n F16 C8 C4 110.8(9) . . n F1 C9 C5 120.3(5) . . n F1 C9 C10 117.3(5) . . n C5 C9 C10 122.3(6) . . n F2 C10 C11 120.6(6) . . n F2 C10 C9 120.8(6) . . n C11 C10 C9 118.6(6) . . n F3 C11 C12 120.4(6) . . n F3 C11 C10 119.7(6) . . n C12 C11 C10 119.9(6) . . n F4 C12 C11 119.3(6) . . n F4 C12 C13 120.3(6) . . n C11 C12 C13 120.4(6) . . n F5 C13 C5 121.4(5) . . n F5 C13 C12 117.6(5) . . n C5 C13 C12 121.0(6) . . n F6 C14 C15 116.7(6) . . n F6 C14 C6 120.5(5) . . n C15 C14 C6 122.8(6) . . n F7 C15 C14 121.3(6) . . n F7 C15 C16 119.6(6) . . n C14 C15 C16 119.0(6) . . n F8 C16 C17 119.8(6) . . n F8 C16 C15 119.4(6) . . n C17 C16 C15 120.8(6) . . n F9 C17 C16 120.6(6) . . n F9 C17 C18 120.5(7) . . n C16 C17 C18 118.9(6) . . n F10 C18 C6 121.3(6) . . n F10 C18 C17 116.8(6) . . n C6 C18 C17 121.9(6) . . n O10 Cu5 O9 165.21(19) . . n O10 Cu5 Cu8 81.85(13) . . n O9 Cu5 Cu8 104.78(13) . . n O10 Cu5 Cu6 108.14(12) . . n O9 Cu5 Cu6 80.43(12) . . n Cu8 Cu5 Cu6 119.43(4) . . n O10 Cu5 Cu7 92.87(13) . . n O9 Cu5 Cu7 101.91(13) . . n Cu8 Cu5 Cu7 60.98(3) . . n Cu6 Cu5 Cu7 58.99(3) . . n O12 Cu6 O11 171.96(19) . . n O12 Cu6 O13 103.33(15) . 2_654 n O11 Cu6 O13 81.44(15) . 2_654 n O12 Cu6 Cu7 81.06(12) . . n O11 Cu6 Cu7 102.05(14) . . n O13 Cu6 Cu7 121.89(10) 2_654 . n O12 Cu6 Cu5 93.18(12) . . n O11 Cu6 Cu5 82.11(12) . . n O13 Cu6 Cu5 163.48(10) 2_654 . n Cu7 Cu6 Cu5 60.53(3) . . n O12 Cu6 Cu8 90.99(12) . . n O11 Cu6 Cu8 88.12(12) . . n O13 Cu6 Cu8 147.55(10) 2_654 . n Cu7 Cu6 Cu8 31.32(2) . . n Cu5 Cu6 Cu8 29.75(2) . . n O14 Cu7 O13 173.46(19) . . n O14 Cu7 O11 101.53(16) . 2_654 n O13 Cu7 O11 72.51(15) . 2_654 n O14 Cu7 Cu6 82.62(13) . . n O13 Cu7 Cu6 98.41(12) . . n O11 Cu7 Cu6 77.36(10) 2_654 . n O14 Cu7 Cu8 103.26(13) . . n O13 Cu7 Cu8 82.03(12) . . n O11 Cu7 Cu8 152.33(9) 2_654 . n Cu6 Cu7 Cu8 117.85(4) . . n O14 Cu7 Cu5 88.93(14) . . n O13 Cu7 Cu5 97.21(13) . . n O11 Cu7 Cu5 134.90(10) 2_654 . n Cu6 Cu7 Cu5 60.47(3) . . n Cu8 Cu7 Cu5 57.91(3) . . n O15 Cu8 O16 177.46(17) . . n O15 Cu8 O3 99.50(15) . . n O16 Cu8 O3 78.21(14) . . n O15 Cu8 Cu5 99.70(13) . . n O16 Cu8 Cu5 82.72(12) . . n O3 Cu8 Cu5 132.64(10) . . n O15 Cu8 Cu7 80.44(12) . . n O16 Cu8 Cu7 101.50(12) . . n O3 Cu8 Cu7 165.43(10) . . n Cu5 Cu8 Cu7 61.11(3) . . n O15 Cu8 Cu6 86.03(12) . . n O16 Cu8 Cu6 96.48(12) . . n O3 Cu8 Cu6 163.40(10) . . n Cu5 Cu8 Cu6 30.83(2) . . n Cu7 Cu8 Cu6 30.82(2) . . n C19 O9 Cu5 125.6(4) . . n C22 O10 Cu5 124.1(4) . . n C19 O11 Cu6 123.2(4) . . n C20 O12 Cu6 124.1(4) . . n C21 O13 Cu7 123.6(4) . . n C21 O13 Cu6 131.8(3) . 2_654 n Cu7 O13 Cu6 104.20(16) . 2_654 n C20 O14 Cu7 121.9(4) . . n C21 O15 Cu8 128.5(4) . . n C22 O16 Cu8 122.9(4) . . n C22 O16 Cu2 123.7(4) . . n Cu8 O16 Cu2 101.93(16) . . n O9 C19 O11 128.4(5) . . n O9 C19 C23 116.1(5) . . n O11 C19 C23 115.4(5) . . n O12 C20 O14 129.5(6) . . n O12 C20 C24 115.8(5) . . n O14 C20 C24 114.7(5) . . n O15 C21 O13 125.2(5) . . n O15 C21 C25 117.7(5) . . n O13 C21 C25 117.0(5) . . n O10 C22 O16 126.6(5) . . n O10 C22 C26 117.6(5) . . n O16 C22 C26 115.8(5) . . n F19 C23 F17 111.3(10) . . n F19 C23 F18 105.8(9) . . n F17 C23 F18 108.4(9) . . n F19 C23 C19 115.1(8) . . n F17 C23 C19 109.5(6) . . n F18 C23 C19 106.5(7) . . n F22 C24 F20 109.4(8) . . n F22 C24 F21 105.8(8) . . n F20 C24 F21 106.6(8) . . n F22 C24 C20 114.5(6) . . n F20 C24 C20 110.7(6) . . n F21 C24 C20 109.5(6) . . n C31 C25 C27 117.4(5) . . n C31 C25 C21 120.7(5) . . n C27 C25 C21 122.0(6) . . n C32 C26 C36 117.5(5) . . n C32 C26 C22 121.0(5) . . n C36 C26 C22 121.4(5) . . n F23 C27 C25 120.6(5) . . n F23 C27 C28 117.7(5) . . n C25 C27 C28 121.7(6) . . n F24 C28 C29 120.6(6) . . n F24 C28 C27 120.2(6) . . n C29 C28 C27 119.2(6) . . n F25 C29 C28 120.3(6) . . n F25 C29 C30 119.8(6) . . n C28 C29 C30 119.9(6) . . n F26 C30 C31 121.5(6) . . n F26 C30 C29 118.5(6) . . n C31 C30 C29 120.0(6) . . n F27 C31 C30 118.4(6) . . n F27 C31 C25 119.6(5) . . n C30 C31 C25 121.9(6) . . n F28 C32 C26 120.4(5) . . n F28 C32 C33 117.6(5) . . n C26 C32 C33 122.0(6) . . n F29 C33 C34 120.3(6) . . n F29 C33 C32 120.7(6) . . n C34 C33 C32 119.0(6) . . n F30 C34 C33 119.3(6) . . n F30 C34 C35 120.3(6) . . n C33 C34 C35 120.5(6) . . n F31 C35 C36 120.3(6) . . n F31 C35 C34 120.0(6) . . n C36 C35 C34 119.7(6) . . n F32 C36 C35 118.3(6) . . n F32 C36 C26 120.2(5) . . n C35 C36 C26 121.4(6) . . n _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.905 _refine_diff_density_min -0.734 _refine_diff_density_rms 0.133 #===END _chemical_name_common ;bis-(pentafluorobenzoato-O,O')-bis-(trifluoroacetato-O,O')- tetracopper(I,I,I,I) ;