# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'H V Rasika Dias' _publ_contact_author_email DIAS@UTA.EDU _publ_section_title ; Organometallic Wheels Based on Coinage Metal Ions and Norbornene: Syntheses and Structural Characterization of [M(norbornene)3][SbF6] (M = Au, Ag, Cu) ; loop_ _publ_author_name 'H V Rasika Dias' 'Huixiong Dai.' 'Mauro Fianchini' # Attachment 'AuAgCu-Norb.cif' data_dias532s _database_code_depnum_ccdc_archive 'CCDC 741041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Au(C7H10)3SbF6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Au F6 Sb' _chemical_formula_weight 715.17 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 11.3842(3) _cell_length_b 11.3842(3) _cell_length_c 14.1889(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1592.52(10) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4996 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.26 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 8.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4646 _exptl_absorpt_correction_T_max 0.6837 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4623 _diffrn_reflns_av_R_equivalents 0.0174 _diffrn_reflns_av_sigmaI/netI 0.0170 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.52 _diffrn_reflns_theta_max 26.47 _reflns_number_total 1475 _reflns_number_gt 1475 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+2.7377P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(4) _refine_ls_number_reflns 1475 _refine_ls_number_parameters 96 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0156 _refine_ls_R_factor_gt 0.0156 _refine_ls_wR_factor_ref 0.0395 _refine_ls_wR_factor_gt 0.0395 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.052 _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 Au Au 0.6667 0.3333 0.1547 0.01575(7) Uani 1 3 d S . . Sb Sb 1.0000 0.0000 0.11463(3) 0.01526(10) Uani 1 3 d S . . C1 C 0.5726(4) 0.1021(4) 0.1688(3) 0.0184(7) Uani 1 1 d . . . C2 C 0.4696(4) 0.1298(4) 0.1524(2) 0.0163(7) Uani 1 1 d . . . C3 C 0.4142(4) 0.0744(4) 0.0548(3) 0.0181(7) Uani 1 1 d . . . H3 H 0.3637 0.1138 0.0225 0.022 Uiso 1 1 calc R . . C4 C 0.3355(4) -0.0817(4) 0.0699(3) 0.0193(7) Uani 1 1 d . . . H4A H 0.2725 -0.1072 0.1240 0.023 Uiso 1 1 calc R . . H4B H 0.2836 -0.1296 0.0128 0.023 Uiso 1 1 calc R . . C5 C 0.4502(4) -0.1142(4) 0.0900(3) 0.0211(8) Uani 1 1 d . . . H5A H 0.4508 -0.1773 0.0423 0.025 Uiso 1 1 calc R . . H5B H 0.4400 -0.1545 0.1534 0.025 Uiso 1 1 calc R . . C6 C 0.5824(4) 0.0278(4) 0.0838(3) 0.0193(7) Uani 1 1 d . . . H6 H 0.6696 0.0278 0.0753 0.023 Uiso 1 1 calc R . . C7 C 0.5410(4) 0.0912(4) 0.0038(3) 0.0205(7) Uani 1 1 d . . . H7A H 0.6094 0.1873 -0.0080 0.025 Uiso 1 1 calc R . . H7B H 0.5191 0.0386 -0.0555 0.025 Uiso 1 1 calc R . . F1 F 0.9436(3) 0.0973(3) 0.19028(18) 0.0367(6) Uani 1 1 d . . . F2 F 0.8480(2) -0.0538(3) 0.03688(17) 0.0303(5) Uani 1 1 d . . . H1 H 0.606(5) 0.087(4) 0.227(3) 0.013(10) Uiso 1 1 d . . . H2 H 0.414(5) 0.139(4) 0.195(3) 0.010(10) 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 Au 0.01614(8) 0.01614(8) 0.01497(10) 0.000 0.000 0.00807(4) Sb 0.01625(13) 0.01625(13) 0.01328(19) 0.000 0.000 0.00812(7) C1 0.0173(18) 0.0153(17) 0.0196(17) 0.0026(13) -0.0005(14) 0.0059(14) C2 0.0166(16) 0.0143(16) 0.0168(16) -0.0014(13) 0.0004(13) 0.0067(14) C3 0.0196(18) 0.0156(17) 0.0206(17) 0.0011(14) -0.0027(14) 0.0099(15) C4 0.0191(17) 0.0151(17) 0.0228(18) -0.0021(14) -0.0034(15) 0.0080(14) C5 0.0209(18) 0.0172(18) 0.027(2) -0.0017(15) 0.0003(16) 0.0108(16) C6 0.0189(17) 0.0177(17) 0.0225(18) -0.0025(14) -0.0011(14) 0.0100(15) C7 0.0227(18) 0.0205(17) 0.0157(16) -0.0021(14) 0.0010(14) 0.0089(15) F1 0.0543(18) 0.0443(16) 0.0260(13) -0.0031(11) 0.0098(12) 0.0354(14) F2 0.0196(11) 0.0433(15) 0.0258(12) 0.0029(10) -0.0049(9) 0.0140(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 Au C2 2.281(3) 2_655 ? Au C2 2.281(3) . ? Au C2 2.281(3) 3_665 ? Au C1 2.302(4) . ? Au C1 2.302(4) 2_655 ? Au C1 2.302(4) 3_665 ? Sb F1 1.872(3) 3_765 ? Sb F1 1.872(3) . ? Sb F1 1.872(3) 2_645 ? Sb F2 1.878(2) . ? Sb F2 1.878(2) 3_765 ? Sb F2 1.878(2) 2_645 ? C1 C2 1.378(5) . ? C1 C6 1.509(5) . ? C1 H1 0.96(5) . ? C2 C3 1.522(5) . ? C2 H2 0.92(5) . ? C3 C7 1.539(5) . ? C3 C4 1.554(5) . ? C3 H3 1.0000 . ? C4 C5 1.551(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.566(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.539(5) . ? C6 H6 1.0000 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 C2 Au C2 119.980(4) 2_655 . ? C2 Au C2 119.980(5) 2_655 3_665 ? C2 Au C2 119.980(5) . 3_665 ? C2 Au C1 85.55(13) 2_655 . ? C2 Au C1 34.99(13) . . ? C2 Au C1 154.24(13) 3_665 . ? C2 Au C1 34.99(13) 2_655 2_655 ? C2 Au C1 154.24(13) . 2_655 ? C2 Au C1 85.55(13) 3_665 2_655 ? C1 Au C1 119.25(3) . 2_655 ? C2 Au C1 154.24(13) 2_655 3_665 ? C2 Au C1 85.55(13) . 3_665 ? C2 Au C1 34.99(13) 3_665 3_665 ? C1 Au C1 119.25(3) . 3_665 ? C1 Au C1 119.25(3) 2_655 3_665 ? F1 Sb F1 90.39(12) 3_765 . ? F1 Sb F1 90.39(12) 3_765 2_645 ? F1 Sb F1 90.39(12) . 2_645 ? F1 Sb F2 178.80(12) 3_765 . ? F1 Sb F2 89.81(12) . . ? F1 Sb F2 90.79(12) 2_645 . ? F1 Sb F2 89.81(12) 3_765 3_765 ? F1 Sb F2 90.79(12) . 3_765 ? F1 Sb F2 178.80(11) 2_645 3_765 ? F2 Sb F2 89.00(11) . 3_765 ? F1 Sb F2 90.79(12) 3_765 2_645 ? F1 Sb F2 178.80(11) . 2_645 ? F1 Sb F2 89.81(12) 2_645 2_645 ? F2 Sb F2 89.00(11) . 2_645 ? F2 Sb F2 89.00(11) 3_765 2_645 ? C2 C1 C6 107.6(3) . . ? C2 C1 Au 71.7(2) . . ? C6 C1 Au 116.7(2) . . ? C2 C1 H1 130(3) . . ? C6 C1 H1 116(3) . . ? Au C1 H1 106(3) . . ? C1 C2 C3 106.4(3) . . ? C1 C2 Au 73.3(2) . . ? C3 C2 Au 115.3(2) . . ? C1 C2 H2 129(3) . . ? C3 C2 H2 119(3) . . ? Au C2 H2 105(3) . . ? C2 C3 C7 102.0(3) . . ? C2 C3 C4 103.4(3) . . ? C7 C3 C4 100.1(3) . . ? C2 C3 H3 116.3 . . ? C7 C3 H3 116.3 . . ? C4 C3 H3 116.3 . . ? C5 C4 C3 103.0(3) . . ? C5 C4 H4A 111.2 . . ? C3 C4 H4A 111.2 . . ? C5 C4 H4B 111.2 . . ? C3 C4 H4B 111.2 . . ? H4A C4 H4B 109.1 . . ? C4 C5 C6 103.5(3) . . ? C4 C5 H5A 111.1 . . ? C6 C5 H5A 111.1 . . ? C4 C5 H5B 111.1 . . ? C6 C5 H5B 111.1 . . ? H5A C5 H5B 109.0 . . ? C1 C6 C7 101.6(3) . . ? C1 C6 C5 103.4(3) . . ? C7 C6 C5 99.4(3) . . ? C1 C6 H6 116.6 . . ? C7 C6 H6 116.6 . . ? C5 C6 H6 116.6 . . ? C3 C7 C6 94.8(3) . . ? C3 C7 H7A 112.8 . . ? C6 C7 H7A 112.8 . . ? C3 C7 H7B 112.8 . . ? C6 C7 H7B 112.8 . . ? H7A C7 H7B 110.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.712 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.074 #===END data_dias581s _database_code_depnum_ccdc_archive 'CCDC 741042' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Ag(C7H10)3SbF6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Ag F6 Sb' _chemical_formula_weight 626.07 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ag Ag -0.8971 1.1015 '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 Hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 11.5119(3) _cell_length_b 11.5119(3) _cell_length_c 14.1244(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1621.04(10) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5271 _cell_measurement_theta_min 2.50 _cell_measurement_theta_max 28.29 _exptl_crystal_description parallelpipe _exptl_crystal_colour colorless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.924 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 2.211 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5664 _exptl_absorpt_correction_T_max 0.6538 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5260 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1797 _reflns_number_gt 1797 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+4.5630P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(2) _refine_ls_number_reflns 1797 _refine_ls_number_parameters 96 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0175 _refine_ls_R_factor_gt 0.0175 _refine_ls_wR_factor_ref 0.0449 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.002 _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 Ag Ag 1.0000 1.0000 1.00659(2) 0.01720(10) Uani 1 3 d S . . Sb Sb 0.3333 0.6667 0.957557(13) 0.01694(9) Uani 1 3 d S . . C1 C 0.8988(3) 0.7591(3) 1.0205(2) 0.0214(5) Uani 1 1 d . . . C2 C 0.7981(3) 0.7862(3) 1.0015(2) 0.0188(5) Uani 1 1 d . . . C3 C 0.7494(3) 0.7378(3) 0.9019(2) 0.0211(5) Uani 1 1 d . . . H3 H 0.7015 0.7788 0.8693 0.025 Uiso 1 1 calc R . . C4 C 0.6704(3) 0.5812(3) 0.9122(2) 0.0226(5) Uani 1 1 d . . . H4A H 0.6051 0.5525 0.9649 0.027 Uiso 1 1 calc R . . H4B H 0.6223 0.5376 0.8530 0.027 Uiso 1 1 calc R . . C5 C 0.7821(3) 0.5481(3) 0.9331(2) 0.0246(6) Uani 1 1 d . . . H5A H 0.7859 0.4894 0.8834 0.030 Uiso 1 1 calc R . . H5B H 0.7682 0.5035 0.9954 0.030 Uiso 1 1 calc R . . C6 C 0.9130(3) 0.6894(3) 0.9331(2) 0.0229(6) Uani 1 1 d . . . H6 H 0.9997 0.6900 0.9262 0.027 Uiso 1 1 calc R . . C7 C 0.8776(3) 0.7568(3) 0.8538(2) 0.0232(6) Uani 1 1 d . . . H7A H 0.8595 0.7085 0.7928 0.028 Uiso 1 1 calc R . . H7B H 0.9461 0.8525 0.8453 0.028 Uiso 1 1 calc R . . F1 F 0.4184(2) 0.81798(19) 0.87887(14) 0.0325(4) Uani 1 1 d . . . F2 F 0.2643(2) 0.7516(2) 1.03299(15) 0.0404(5) Uani 1 1 d . . . H1 H 0.939(4) 0.751(4) 1.087(2) 0.021(9) Uiso 1 1 d . . . H2 H 0.746(4) 0.814(4) 1.039(3) 0.038(11) 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 Ag 0.01715(13) 0.01715(13) 0.01729(19) 0.000 0.000 0.00858(7) Sb 0.01845(12) 0.01845(12) 0.01391(15) 0.000 0.000 0.00923(6) C1 0.0200(13) 0.0168(12) 0.0215(13) -0.0004(10) -0.0037(10) 0.0047(10) C2 0.0191(12) 0.0158(12) 0.0193(12) -0.0012(10) 0.0008(10) 0.0072(10) C3 0.0219(13) 0.0168(12) 0.0238(13) -0.0014(10) -0.0049(11) 0.0091(10) C4 0.0217(13) 0.0172(12) 0.0269(13) -0.0031(10) -0.0069(11) 0.0082(10) C5 0.0237(14) 0.0195(13) 0.0321(15) -0.0030(11) -0.0029(11) 0.0119(11) C6 0.0209(13) 0.0212(13) 0.0289(15) -0.0010(11) 0.0009(11) 0.0123(11) C7 0.0262(14) 0.0228(13) 0.0180(12) -0.0032(11) 0.0012(11) 0.0103(12) F1 0.0395(11) 0.0204(8) 0.0288(10) 0.0083(7) 0.0084(8) 0.0085(8) F2 0.0556(13) 0.0508(13) 0.0317(10) -0.0072(10) 0.0079(10) 0.0393(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 Ag C2 2.397(3) 2_765 ? Ag C2 2.397(3) . ? Ag C2 2.397(3) 3_675 ? Ag C1 2.420(3) 2_765 ? Ag C1 2.420(3) . ? Ag C1 2.420(3) 3_675 ? Sb F2 1.8714(19) . ? Sb F2 1.8714(19) 3_565 ? Sb F2 1.8714(19) 2_665 ? Sb F1 1.8769(18) 2_665 ? Sb F1 1.8769(18) . ? Sb F1 1.8769(18) 3_565 ? C1 C2 1.369(4) . ? C1 C6 1.525(4) . ? C1 H1 1.07(3) . ? C2 C3 1.513(4) . ? C2 H2 0.96(4) . ? C3 C7 1.537(4) . ? C3 C4 1.567(4) . ? C3 H3 1.0000 . ? C4 C5 1.542(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.570(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.529(4) . ? C6 H6 1.0000 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 C2 Ag C2 119.910(8) 2_765 . ? C2 Ag C2 119.910(9) 2_765 3_675 ? C2 Ag C2 119.910(8) . 3_675 ? C2 Ag C1 33.02(9) 2_765 2_765 ? C2 Ag C1 152.32(9) . 2_765 ? C2 Ag C1 87.73(9) 3_675 2_765 ? C2 Ag C1 87.73(9) 2_765 . ? C2 Ag C1 33.02(9) . . ? C2 Ag C1 152.32(10) 3_675 . ? C1 Ag C1 119.35(2) 2_765 . ? C2 Ag C1 152.32(10) 2_765 3_675 ? C2 Ag C1 87.73(9) . 3_675 ? C2 Ag C1 33.02(9) 3_675 3_675 ? C1 Ag C1 119.35(2) 2_765 3_675 ? C1 Ag C1 119.35(2) . 3_675 ? F2 Sb F2 90.79(10) . 3_565 ? F2 Sb F2 90.79(10) . 2_665 ? F2 Sb F2 90.79(10) 3_565 2_665 ? F2 Sb F1 89.94(10) . 2_665 ? F2 Sb F1 178.30(10) 3_565 2_665 ? F2 Sb F1 90.74(10) 2_665 2_665 ? F2 Sb F1 90.74(10) . . ? F2 Sb F1 89.94(10) 3_565 . ? F2 Sb F1 178.30(10) 2_665 . ? F1 Sb F1 88.51(9) 2_665 . ? F2 Sb F1 178.30(10) . 3_565 ? F2 Sb F1 90.74(10) 3_565 3_565 ? F2 Sb F1 89.94(10) 2_665 3_565 ? F1 Sb F1 88.51(9) 2_665 3_565 ? F1 Sb F1 88.51(9) . 3_565 ? C2 C1 C6 106.6(2) . . ? C2 C1 Ag 72.54(16) . . ? C6 C1 Ag 114.84(19) . . ? C2 C1 H1 130(2) . . ? C6 C1 H1 120.0(19) . . ? Ag C1 H1 100.8(19) . . ? C1 C2 C3 107.4(2) . . ? C1 C2 Ag 74.44(17) . . ? C3 C2 Ag 113.39(18) . . ? C1 C2 H2 134(3) . . ? C3 C2 H2 117(3) . . ? Ag C2 H2 95(3) . . ? C2 C3 C7 101.8(2) . . ? C2 C3 C4 103.5(2) . . ? C7 C3 C4 99.7(2) . . ? C2 C3 H3 116.4 . . ? C7 C3 H3 116.4 . . ? C4 C3 H3 116.4 . . ? C5 C4 C3 103.0(2) . . ? C5 C4 H4A 111.2 . . ? C3 C4 H4A 111.2 . . ? C5 C4 H4B 111.2 . . ? C3 C4 H4B 111.2 . . ? H4A C4 H4B 109.1 . . ? C4 C5 C6 103.4(2) . . ? C4 C5 H5A 111.1 . . ? C6 C5 H5A 111.1 . . ? C4 C5 H5B 111.1 . . ? C6 C5 H5B 111.1 . . ? H5A C5 H5B 109.1 . . ? C1 C6 C7 101.5(2) . . ? C1 C6 C5 104.2(2) . . ? C7 C6 C5 99.5(2) . . ? C1 C6 H6 116.4 . . ? C7 C6 H6 116.4 . . ? C5 C6 H6 116.4 . . ? C6 C7 C3 94.8(2) . . ? C6 C7 H7A 112.8 . . ? C3 C7 H7A 112.8 . . ? C6 C7 H7B 112.8 . . ? C3 C7 H7B 112.8 . . ? H7A C7 H7B 110.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.972 _refine_diff_density_min -0.854 _refine_diff_density_rms 0.079 #===END data_dias591s _database_code_depnum_ccdc_archive 'CCDC 741043' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cu(C7H10)3SbF6 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Cu F6 Sb' _chemical_formula_weight 581.74 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' 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Hexagonal _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 11.3580(3) _cell_length_b 11.3580(3) _cell_length_c 14.0341(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1567.90(10) _cell_formula_units_Z 3 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5044 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 28.29 _exptl_crystal_description parallelpipe _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 2.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7484 _exptl_absorpt_correction_T_max 0.7643 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4876 _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 28.29 _reflns_number_total 1723 _reflns_number_gt 1722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+10.8780P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 1723 _refine_ls_number_parameters 95 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0276 _refine_ls_R_factor_gt 0.0276 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.129 _refine_ls_restrained_S_all 1.129 _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 Cu Cu 0.3333 0.6667 0.25592(6) 0.0174(2) Uani 1 3 d S . . Sb Sb 0.3333 0.6667 0.9611 0.01540(11) Uani 1 3 d S . . C1 C 0.3352(4) 0.4742(4) 0.2593(3) 0.0190(8) Uani 1 1 d . . . C2 C 0.4645(5) 0.5771(5) 0.2378(3) 0.0205(9) Uani 1 1 d . . . C3 C 0.5564(4) 0.5911(4) 0.3202(3) 0.0203(8) Uani 1 1 d . . . H3 H 0.6440 0.6792 0.3252 0.024 Uiso 1 1 calc R . . C4 C 0.5665(5) 0.4589(5) 0.3160(4) 0.0225(9) Uani 1 1 d . . . H4A H 0.5932 0.4453 0.2515 0.027 Uiso 1 1 calc R . . H4B H 0.6331 0.4622 0.3629 0.027 Uiso 1 1 calc R . . C5 C 0.4206(4) 0.3450(4) 0.3409(3) 0.0217(8) Uani 1 1 d . . . H5A H 0.4202 0.2951 0.3988 0.026 Uiso 1 1 calc R . . H5B H 0.3796 0.2799 0.2876 0.026 Uiso 1 1 calc R . . C6 C 0.3435(4) 0.4239(4) 0.3582(3) 0.0209(8) Uani 1 1 d . . . H6 H 0.2561 0.3745 0.3944 0.025 Uiso 1 1 calc R . . C7 C 0.4562(4) 0.5539(5) 0.4043(3) 0.0215(8) Uani 1 1 d . . . H7A H 0.4911 0.5360 0.4640 0.026 Uiso 1 1 calc R . . H7B H 0.4285 0.6228 0.4155 0.026 Uiso 1 1 calc R . . F1 F 0.4878(4) 0.7423(4) 1.0407(2) 0.0310(8) Uani 1 1 d . . . F2 F 0.4136(4) 0.8227(4) 0.8853(2) 0.0350(8) Uani 1 1 d . . . H1 H 0.259(8) 0.425(8) 0.217(5) 0.050 Uiso 1 1 d . . . H2 H 0.517(10) 0.631(9) 0.185(7) 0.07(3) 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 Cu 0.0181(3) 0.0181(3) 0.0159(4) 0.000 0.000 0.00903(14) Sb 0.01624(13) 0.01624(13) 0.01371(18) 0.000 0.000 0.00812(7) C1 0.019(2) 0.0203(19) 0.0202(18) -0.0022(15) -0.0017(15) 0.0120(16) C2 0.031(2) 0.0161(19) 0.019(2) 0.0030(15) 0.0042(17) 0.0150(18) C3 0.0168(18) 0.0217(19) 0.023(2) 0.0005(15) 0.0007(15) 0.0098(16) C4 0.019(2) 0.020(2) 0.029(2) 0.0082(17) 0.0036(17) 0.0097(18) C5 0.024(2) 0.0210(19) 0.024(2) 0.0041(15) 0.0037(16) 0.0149(17) C6 0.0188(19) 0.022(2) 0.0231(19) 0.0040(16) 0.0025(15) 0.0112(16) C7 0.023(2) 0.025(2) 0.0179(18) -0.0003(15) -0.0008(15) 0.0128(17) F1 0.0239(17) 0.039(2) 0.0264(17) -0.0029(15) -0.0075(13) 0.0127(15) F2 0.046(2) 0.0242(18) 0.0276(18) 0.0148(14) 0.0069(17) 0.0120(16) _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 Cu C1 2.197(4) 3_565 ? Cu C1 2.197(4) 2_665 ? Cu C1 2.197(4) . ? Cu C2 2.199(4) 3_565 ? Cu C2 2.199(4) 2_665 ? Cu C2 2.199(4) . ? Sb F2 1.867(3) 2_665 ? Sb F2 1.867(3) . ? Sb F2 1.867(3) 3_565 ? Sb F1 1.886(3) 2_665 ? Sb F1 1.886(3) . ? Sb F1 1.886(3) 3_565 ? C1 C2 1.378(6) . ? C1 C6 1.522(6) . ? C1 H1 0.97(8) . ? C2 C3 1.511(6) . ? C2 H2 0.96(9) . ? C3 C7 1.545(6) . ? C3 C4 1.564(6) . ? C3 H3 1.0000 . ? C4 C5 1.548(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.554(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.532(6) . ? C6 H6 1.0000 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? 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 C1 Cu C1 119.953(9) 3_565 2_665 ? C1 Cu C1 119.953(9) 3_565 . ? C1 Cu C1 119.953(9) 2_665 . ? C1 Cu C2 36.53(16) 3_565 3_565 ? C1 Cu C2 155.22(16) 2_665 3_565 ? C1 Cu C2 84.45(16) . 3_565 ? C1 Cu C2 84.45(16) 3_565 2_665 ? C1 Cu C2 36.53(16) 2_665 2_665 ? C1 Cu C2 155.22(16) . 2_665 ? C2 Cu C2 118.69(5) 3_565 2_665 ? C1 Cu C2 155.22(16) 3_565 . ? C1 Cu C2 84.45(16) 2_665 . ? C1 Cu C2 36.53(16) . . ? C2 Cu C2 118.69(5) 3_565 . ? C2 Cu C2 118.69(5) 2_665 . ? F2 Sb F2 90.75(16) 2_665 . ? F2 Sb F2 90.75(16) 2_665 3_565 ? F2 Sb F2 90.75(16) . 3_565 ? F2 Sb F1 90.19(18) 2_665 2_665 ? F2 Sb F1 90.55(18) . 2_665 ? F2 Sb F1 178.39(19) 3_565 2_665 ? F2 Sb F1 178.39(19) 2_665 . ? F2 Sb F1 90.19(18) . . ? F2 Sb F1 90.55(18) 3_565 . ? F1 Sb F1 88.49(16) 2_665 . ? F2 Sb F1 90.55(18) 2_665 3_565 ? F2 Sb F1 178.4(2) . 3_565 ? F2 Sb F1 90.19(18) 3_565 3_565 ? F1 Sb F1 88.49(16) 2_665 3_565 ? F1 Sb F1 88.49(16) . 3_565 ? C2 C1 C6 106.2(4) . . ? C2 C1 Cu 71.8(2) . . ? C6 C1 Cu 115.2(3) . . ? C2 C1 H1 128(4) . . ? C6 C1 H1 124(4) . . ? Cu C1 H1 96(5) . . ? C1 C2 C3 108.0(4) . . ? C1 C2 Cu 71.7(2) . . ? C3 C2 Cu 117.1(3) . . ? C1 C2 H2 140(6) . . ? C3 C2 H2 111(6) . . ? Cu C2 H2 98(6) . . ? C2 C3 C7 100.4(3) . . ? C2 C3 C4 104.4(4) . . ? C7 C3 C4 99.4(3) . . ? C2 C3 H3 116.7 . . ? C7 C3 H3 116.7 . . ? C4 C3 H3 116.7 . . ? C5 C4 C3 103.4(3) . . ? C5 C4 H4A 111.1 . . ? C3 C4 H4A 111.1 . . ? C5 C4 H4B 111.1 . . ? C3 C4 H4B 111.1 . . ? H4A C4 H4B 109.0 . . ? C4 C5 C6 103.3(3) . . ? C4 C5 H5A 111.1 . . ? C6 C5 H5A 111.1 . . ? C4 C5 H5B 111.1 . . ? C6 C5 H5B 111.1 . . ? H5A C5 H5B 109.1 . . ? C1 C6 C7 101.6(3) . . ? C1 C6 C5 103.4(3) . . ? C7 C6 C5 100.5(3) . . ? C1 C6 H6 116.3 . . ? C7 C6 H6 116.3 . . ? C5 C6 H6 116.3 . . ? C6 C7 C3 95.0(3) . . ? C6 C7 H7A 112.7 . . ? C3 C7 H7A 112.7 . . ? C6 C7 H7B 112.7 . . ? C3 C7 H7B 112.7 . . ? H7A C7 H7B 110.2 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.830 _refine_diff_density_min -0.953 _refine_diff_density_rms 0.112 #===END