data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'H V Rasika Dias' _publ_contact_author_email DIAS@UTA.EDU _publ_section_title ; A Non-Classical Copper Carbonyl on a Tri-alkene Hydrocarbon Support ; loop_ _publ_author_name 'H V Rasika Dias' 'Thomas R Cundari' 'Nathan J. DeYonker' 'Mauro Fianchini' data_dias586s _database_code_depnum_ccdc_archive 'CCDC 712593' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cu(C12H18))(SbF6) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H18 Cu F6 Sb' _chemical_formula_weight 461.55 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 7.6618(4) _cell_length_b 11.4769(6) _cell_length_c 9.0706(5) _cell_angle_alpha 90.00 _cell_angle_beta 113.717(1) _cell_angle_gamma 90.00 _cell_volume 730.25(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6219 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.31 _exptl_crystal_description rods _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.099 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 448 _exptl_absorpt_coefficient_mu 3.357 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5532 _exptl_absorpt_correction_T_max 0.6694 _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 7159 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0163 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1903 _reflns_number_gt 1868 _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^)+(0.0361P)^2^+0.3723P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1903 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0198 _refine_ls_R_factor_gt 0.0194 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0527 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.03953(5) 0.2500 0.25834(4) 0.02952(9) Uani 1 2 d S . . Sb Sb 0.546260(19) 0.2500 0.702242(16) 0.02291(7) Uani 1 2 d S . . F1 F 0.5632(2) 0.13470(13) 0.56387(17) 0.0528(4) Uani 1 1 d . . . F2 F 0.2806(2) 0.2500 0.5854(3) 0.0560(5) Uani 1 2 d S . . F3 F 0.8107(2) 0.2500 0.8121(3) 0.0503(5) Uani 1 2 d S . . F4 F 0.5299(3) 0.13531(15) 0.84153(19) 0.0606(4) Uani 1 1 d . . . C1 C 0.1216(8) 0.3800(4) 0.1346(5) 0.0294(8) Uani 0.50 1 d P A -1 H1A H 0.0241 0.3989 0.0246 0.035 Uiso 0.50 1 calc PR A -1 C2 C 0.0933(5) 0.4323(3) 0.2571(5) 0.0279(7) Uani 0.50 1 d P A -1 H2A H 0.2089 0.4630 0.3479 0.034 Uiso 0.50 1 calc PR A -1 C3 C -0.0979(9) 0.4834(8) 0.2383(9) 0.0322(13) Uani 0.50 1 d P A -1 H3A H -0.1847 0.4848 0.1228 0.039 Uiso 0.50 1 calc PR A -1 H3B H -0.0793 0.5647 0.2783 0.039 Uiso 0.50 1 calc PR A -1 C4 C -0.1895(9) 0.4116(6) 0.3321(7) 0.0293(11) Uani 0.50 1 d P A -1 H4A H -0.1036 0.4102 0.4479 0.035 Uiso 0.50 1 calc PR A -1 H4B H -0.3113 0.4481 0.3211 0.035 Uiso 0.50 1 calc PR A -1 C5 C -0.2257(5) 0.2894(3) 0.2679(5) 0.0265(7) Uani 0.50 1 d P A -1 H5A H -0.3386 0.2806 0.1631 0.032 Uiso 0.50 1 calc PR A -1 C6 C -0.1626(6) 0.1887(4) 0.3499(6) 0.0334(8) Uani 0.50 1 d P A -1 H6A H -0.1211 0.1935 0.4693 0.040 Uiso 0.50 1 calc PR A -1 C7 C -0.2045(11) 0.0668(6) 0.2775(8) 0.0391(15) Uani 0.50 1 d P A -1 H7A H -0.2505 0.0175 0.3440 0.047 Uiso 0.50 1 calc PR A -1 H7B H -0.3073 0.0714 0.1680 0.047 Uiso 0.50 1 calc PR A -1 C8 C -0.0314(10) 0.0109(8) 0.2680(10) 0.0426(19) Uani 0.50 1 d P A -1 H8A H 0.0720 0.0059 0.3771 0.051 Uiso 0.50 1 calc PR A -1 H8B H -0.0632 -0.0692 0.2250 0.051 Uiso 0.50 1 calc PR A -1 C9 C 0.0354(7) 0.0810(4) 0.1604(6) 0.0360(9) Uani 0.50 1 d P A -1 H9A H -0.0456 0.0737 0.0426 0.043 Uiso 0.50 1 calc PR A -1 C10 C 0.2101(8) 0.1275(4) 0.1968(6) 0.0389(10) Uani 0.50 1 d P A -1 H10A H 0.3169 0.0909 0.2897 0.047 Uiso 0.50 1 calc PR A -1 C11 C 0.2684(9) 0.1998(7) 0.0847(7) 0.0443(15) Uani 0.50 1 d P A -1 H11A H 0.1665 0.1962 -0.0253 0.053 Uiso 0.50 1 calc PR A -1 H11B H 0.3855 0.1663 0.0808 0.053 Uiso 0.50 1 calc PR A -1 C12 C 0.3051(9) 0.3274(6) 0.1380(7) 0.0373(12) Uani 0.50 1 d P A -1 H12A H 0.4063 0.3321 0.2482 0.045 Uiso 0.50 1 calc PR A -1 H12B H 0.3482 0.3711 0.0646 0.045 Uiso 0.50 1 calc PR A -1 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 0.02545(17) 0.02664(17) 0.03861(19) 0.000 0.01512(14) 0.000 Sb 0.01860(10) 0.02611(10) 0.01852(10) 0.000 0.00171(7) 0.000 F1 0.0587(8) 0.0503(8) 0.0356(7) -0.0167(6) 0.0044(6) 0.0139(7) F2 0.0179(8) 0.0675(13) 0.0696(14) 0.000 0.0042(8) 0.000 F3 0.0208(8) 0.0617(12) 0.0485(11) 0.000 -0.0070(7) 0.000 F4 0.0762(11) 0.0572(9) 0.0459(8) 0.0193(7) 0.0217(8) -0.0135(8) C1 0.020(2) 0.039(2) 0.023(2) 0.0006(16) 0.0011(17) -0.0052(17) C2 0.0258(17) 0.0301(18) 0.0237(19) -0.0003(14) 0.0056(16) -0.0082(14) C3 0.032(3) 0.028(2) 0.029(3) -0.004(2) 0.004(3) 0.004(3) C4 0.029(2) 0.033(3) 0.027(3) -0.004(2) 0.013(2) 0.0000(19) C5 0.0200(15) 0.0351(17) 0.0237(17) -0.0019(13) 0.0080(14) -0.0035(12) C6 0.0245(18) 0.049(3) 0.0239(19) 0.0035(17) 0.0064(16) -0.0050(16) C7 0.049(3) 0.031(3) 0.030(3) 0.002(2) 0.008(3) -0.011(2) C8 0.049(5) 0.028(2) 0.031(3) -0.001(2) -0.004(3) 0.004(4) C9 0.036(2) 0.0292(19) 0.031(2) -0.0063(17) 0.000(2) 0.0078(18) C10 0.026(2) 0.044(2) 0.035(2) -0.0137(19) -0.0002(19) 0.0156(19) C11 0.022(3) 0.070(4) 0.036(3) -0.013(3) 0.007(3) 0.010(2) C12 0.021(3) 0.059(3) 0.031(3) -0.006(2) 0.010(2) -0.009(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 Cu C1 2.110(4) 4_565 ? Cu C1 2.110(4) . ? Cu C5 2.117(3) . ? Cu C5 2.117(3) 4_565 ? Cu C9 2.128(4) . ? Cu C9 2.128(4) 4_565 ? Cu C2 2.133(4) . ? Cu C2 2.133(4) 4_565 ? Cu C10 2.141(4) 4_565 ? Cu C10 2.141(4) . ? Cu C6 2.149(4) . ? Cu C6 2.149(4) 4_565 ? Sb F4 1.8633(14) 4_565 ? Sb F4 1.8633(14) . ? Sb F3 1.8640(17) . ? Sb F1 1.8640(13) . ? Sb F1 1.8640(13) 4_565 ? Sb F2 1.8789(18) . ? C1 C2 1.355(6) . ? C1 C12 1.519(9) . ? C1 H1A 1.0000 . ? C2 C3 1.522(8) . ? C2 H2A 1.0000 . ? C3 C4 1.542(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.501(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.354(5) . ? C5 H5A 1.0000 . ? C6 C7 1.524(8) . ? C6 H6A 1.0000 . ? C7 C8 1.507(12) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.504(12) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.353(7) . ? C9 H9A 1.0000 . ? C10 C11 1.512(9) . ? C10 H10A 1.0000 . ? C11 C12 1.532(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 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 90.0(3) 4_565 . ? C1 Cu C5 132.0(2) 4_565 . ? C1 Cu C5 111.54(19) . . ? C1 Cu C5 111.54(19) 4_565 4_565 ? C1 Cu C5 132.0(2) . 4_565 ? C5 Cu C5 24.7(2) . 4_565 ? C1 Cu C9 24.61(17) 4_565 . ? C1 Cu C9 112.3(2) . . ? C5 Cu C9 110.99(18) . . ? C5 Cu C9 88.22(18) 4_565 . ? C1 Cu C9 112.3(2) 4_565 4_565 ? C1 Cu C9 24.61(17) . 4_565 ? C5 Cu C9 88.22(18) . 4_565 ? C5 Cu C9 110.99(18) 4_565 4_565 ? C9 Cu C9 131.4(3) . 4_565 ? C1 Cu C2 126.26(19) 4_565 . ? C1 Cu C2 37.25(16) . . ? C5 Cu C2 88.92(14) . . ? C5 Cu C2 113.59(14) 4_565 . ? C9 Cu C2 149.6(2) . . ? C9 Cu C2 22.26(15) 4_565 . ? C1 Cu C2 37.25(16) 4_565 4_565 ? C1 Cu C2 126.26(19) . 4_565 ? C5 Cu C2 113.59(14) . 4_565 ? C5 Cu C2 88.92(14) 4_565 4_565 ? C9 Cu C2 22.26(15) . 4_565 ? C9 Cu C2 149.6(2) 4_565 4_565 ? C2 Cu C2 157.5(2) . 4_565 ? C1 Cu C10 89.0(2) 4_565 4_565 ? C1 Cu C10 18.71(13) . 4_565 ? C5 Cu C10 124.54(18) . 4_565 ? C5 Cu C10 147.94(19) 4_565 4_565 ? C9 Cu C10 113.5(2) . 4_565 ? C9 Cu C10 36.96(18) 4_565 4_565 ? C2 Cu C10 38.29(17) . 4_565 ? C2 Cu C10 120.22(18) 4_565 4_565 ? C1 Cu C10 18.71(13) 4_565 . ? C1 Cu C10 89.0(2) . . ? C5 Cu C10 147.94(19) . . ? C5 Cu C10 124.54(18) 4_565 . ? C9 Cu C10 36.96(18) . . ? C9 Cu C10 113.5(2) 4_565 . ? C2 Cu C10 120.22(18) . . ? C2 Cu C10 38.29(17) 4_565 . ? C10 Cu C10 82.1(3) 4_565 . ? C1 Cu C6 112.93(19) 4_565 . ? C1 Cu C6 148.5(2) . . ? C5 Cu C6 37.00(14) . . ? C5 Cu C6 20.21(13) 4_565 . ? C9 Cu C6 88.3(2) . . ? C9 Cu C6 124.6(2) 4_565 . ? C2 Cu C6 119.58(16) . . ? C2 Cu C6 81.47(16) 4_565 . ? C10 Cu C6 157.84(19) 4_565 . ? C10 Cu C6 119.75(19) . . ? C1 Cu C6 148.5(2) 4_565 4_565 ? C1 Cu C6 112.93(19) . 4_565 ? C5 Cu C6 20.21(13) . 4_565 ? C5 Cu C6 37.00(14) 4_565 4_565 ? C9 Cu C6 124.6(2) . 4_565 ? C9 Cu C6 88.3(2) 4_565 4_565 ? C2 Cu C6 81.47(16) . 4_565 ? C2 Cu C6 119.58(16) 4_565 4_565 ? C10 Cu C6 119.75(19) 4_565 4_565 ? C10 Cu C6 157.84(19) . 4_565 ? C6 Cu C6 38.2(2) . 4_565 ? F4 Sb F4 89.89(12) 4_565 . ? F4 Sb F3 89.58(8) 4_565 . ? F4 Sb F3 89.58(8) . . ? F4 Sb F1 179.68(6) 4_565 . ? F4 Sb F1 89.82(9) . . ? F3 Sb F1 90.26(7) . . ? F4 Sb F1 89.82(9) 4_565 4_565 ? F4 Sb F1 179.68(7) . 4_565 ? F3 Sb F1 90.26(7) . 4_565 ? F1 Sb F1 90.46(11) . 4_565 ? F4 Sb F2 91.69(8) 4_565 . ? F4 Sb F2 91.69(8) . . ? F3 Sb F2 178.20(9) . . ? F1 Sb F2 88.47(7) . . ? F1 Sb F2 88.47(7) 4_565 . ? C2 C1 C12 127.7(5) . . ? C2 C1 Cu 72.3(2) . . ? C12 C1 Cu 100.3(4) . . ? C2 C1 H1A 114.9 . . ? C12 C1 H1A 114.9 . . ? Cu C1 H1A 114.9 . . ? C1 C2 C3 122.9(5) . . ? C1 C2 Cu 70.4(2) . . ? C3 C2 Cu 101.5(4) . . ? C1 C2 H2A 116.8 . . ? C3 C2 H2A 116.8 . . ? Cu C2 H2A 116.8 . . ? C2 C3 C4 111.3(6) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 109.8(5) . . ? C5 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 . . ? C5 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C6 C5 C4 127.9(4) . . ? C6 C5 Cu 72.8(2) . . ? C4 C5 Cu 100.7(3) . . ? C6 C5 H5A 114.7 . . ? C4 C5 H5A 114.7 . . ? Cu C5 H5A 114.7 . . ? C5 C6 C7 125.4(4) . . ? C5 C6 Cu 70.2(2) . . ? C7 C6 Cu 101.2(4) . . ? C5 C6 H6A 115.9 . . ? C7 C6 H6A 115.9 . . ? Cu C6 H6A 115.9 . . ? C8 C7 C6 112.2(6) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 110.2(6) . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 127.9(5) . . ? C10 C9 Cu 72.1(2) . . ? C8 C9 Cu 99.7(4) . . ? C10 C9 H9A 114.9 . . ? C8 C9 H9A 114.9 . . ? Cu C9 H9A 114.9 . . ? C9 C10 C11 125.7(6) . . ? C9 C10 Cu 71.0(2) . . ? C11 C10 Cu 101.0(3) . . ? C9 C10 H10A 115.7 . . ? C11 C10 H10A 115.7 . . ? Cu C10 H10A 115.7 . . ? C10 C11 C12 112.3(6) . . ? C10 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C1 C12 C11 108.8(5) . . ? C1 C12 H12A 109.9 . . ? C11 C12 H12A 109.9 . . ? C1 C12 H12B 109.9 . . ? C11 C12 H12B 109.9 . . ? H12A C12 H12B 108.3 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.590 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.099 data_dias587s _database_code_depnum_ccdc_archive 'CCDC 712594' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (Cu(C12H18)CO)(SbF6) _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H18 Cu F6 O Sb' _chemical_formula_weight 489.56 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' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P2(1)3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' 'z, x, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x, y+1/2' '-z, x+1/2, -y+1/2' 'y, z, x' '-y, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x' '-y+1/2, -z, x+1/2' _cell_length_a 11.7046(12) _cell_length_b 11.7046(12) _cell_length_c 11.7046(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1603.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6785 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.31 _exptl_crystal_description blocks _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 3.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5517 _exptl_absorpt_correction_T_max 0.6081 _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 15645 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0113 _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 -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1340 _reflns_number_gt 1337 _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^)+(0.0232P)^2^+0.7740P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 1340 _refine_ls_number_parameters 103 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0168 _refine_ls_R_factor_gt 0.0168 _refine_ls_wR_factor_ref 0.0428 _refine_ls_wR_factor_gt 0.0428 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.109 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu 0.69867(2) 0.19867(2) 0.30133(2) 0.02362(10) Uani 1 3 d S . . Sb Sb 0.580890(12) 0.419110(12) 0.919110(12) 0.02804(7) Uani 1 3 d S . . O O 0.84997(15) 0.34997(15) 0.15003(15) 0.0410(7) Uani 1 3 d S . . C5 C 0.79445(18) 0.29445(18) 0.20555(18) 0.0270(7) Uani 1 3 d S A . F1 F 0.61834(16) 0.47506(16) 1.06451(14) 0.0513(4) Uani 1 1 d . . . F2 F 0.5374(2) 0.3616(2) 0.77760(15) 0.0712(6) Uani 1 1 d . . . C1A C 0.7453(4) 0.1528(4) 0.4836(4) 0.0231(8) Uani 0.50 1 d PD A 1 H1AA H 0.6940 0.0966 0.5226 0.028 Uiso 0.50 1 calc PR A 1 C2A C 0.7424(5) 0.2740(5) 0.5295(6) 0.0246(12) Uani 0.50 1 d PD A 1 H2AA H 0.7989 0.3213 0.4879 0.030 Uiso 0.50 1 calc PR A 1 H2AB H 0.7636 0.2738 0.6114 0.030 Uiso 0.50 1 calc PR A 1 C3A C 0.6233(5) 0.3259(5) 0.5154(5) 0.0291(11) Uani 0.50 1 d PD A 1 H3AA H 0.5679 0.2811 0.5610 0.035 Uiso 0.50 1 calc PR A 1 H3AB H 0.6237 0.4050 0.5452 0.035 Uiso 0.50 1 calc PR A 1 C4A C 0.5858(4) 0.3271(5) 0.3921(4) 0.0265(9) Uani 0.50 1 d PD A 1 H4AA H 0.5806 0.4042 0.3556 0.032 Uiso 0.50 1 calc PR A 1 C1B C 0.7834(4) 0.2171(5) 0.4733(4) 0.0338(10) Uani 0.50 1 d PD A 2 H1BA H 0.8633 0.2471 0.4716 0.041 Uiso 0.50 1 calc PR A 2 C2B C 0.7001(6) 0.2854(6) 0.5449(6) 0.0372(17) Uani 0.50 1 d PD A 2 H2BA H 0.7432 0.3397 0.5934 0.045 Uiso 0.50 1 calc PR A 2 H2BB H 0.6577 0.2330 0.5959 0.045 Uiso 0.50 1 calc PR A 2 C3B C 0.6156(5) 0.3515(5) 0.4714(6) 0.0343(13) Uani 0.50 1 d PD A 2 H3BA H 0.5621 0.3937 0.5214 0.041 Uiso 0.50 1 calc PR A 2 H3BB H 0.6575 0.4080 0.4245 0.041 Uiso 0.50 1 calc PR A 2 C4B C 0.5485(5) 0.2727(5) 0.3937(5) 0.0292(10) Uani 0.50 1 d PD A 2 H4BA H 0.4999 0.2154 0.4344 0.035 Uiso 0.50 1 calc PR A 2 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 0.02362(10) 0.02362(10) 0.02362(10) -0.00028(10) -0.00028(10) 0.00028(10) Sb 0.02804(7) 0.02804(7) 0.02804(7) -0.00186(6) 0.00186(6) 0.00186(6) O 0.0410(7) 0.0410(7) 0.0410(7) 0.0060(8) 0.0060(8) -0.0060(8) C5 0.0270(7) 0.0270(7) 0.0270(7) 0.0014(8) 0.0014(8) -0.0014(8) F1 0.0583(10) 0.0570(10) 0.0385(8) -0.0094(8) -0.0153(7) -0.0024(8) F2 0.0871(15) 0.0913(15) 0.0351(9) -0.0275(10) -0.0009(9) -0.0062(12) C1A 0.022(2) 0.022(2) 0.026(2) -0.0008(18) -0.0004(17) -0.0003(19) C2A 0.021(3) 0.027(2) 0.025(3) -0.003(2) -0.001(2) -0.003(2) C3A 0.031(3) 0.034(3) 0.023(3) -0.008(2) -0.001(2) 0.005(2) C4A 0.0230(19) 0.023(2) 0.033(3) -0.0027(17) -0.0006(19) 0.0033(19) C1B 0.029(2) 0.046(3) 0.026(2) 0.003(2) -0.0056(18) -0.003(2) C2B 0.040(4) 0.044(4) 0.027(3) -0.007(2) 0.008(3) -0.008(4) C3B 0.038(3) 0.035(3) 0.030(4) -0.002(3) 0.005(3) 0.000(2) C4B 0.024(2) 0.031(3) 0.033(3) -0.001(2) 0.0035(19) 0.001(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 Cu C5 1.942(4) . ? Cu C4B 2.238(5) 8_645 ? Cu C4B 2.238(5) . ? Cu C4B 2.238(5) 11_556 ? Cu C1B 2.254(5) 11_556 ? Cu C1B 2.254(5) . ? Cu C1B 2.254(5) 8_645 ? Cu C4A 2.266(4) 8_645 ? Cu C4A 2.266(4) . ? Cu C4A 2.266(4) 11_556 ? Cu C1A 2.267(5) 11_556 ? Cu C1A 2.267(5) . ? Sb F2 1.8590(17) . ? Sb F2 1.8590(17) 7_665 ? Sb F2 1.8590(17) 10_646 ? Sb F1 1.8754(16) . ? Sb F1 1.8754(16) 7_665 ? Sb F1 1.8754(16) 10_646 ? O C5 1.126(5) . ? C1A C4A 1.361(7) 11_556 ? C1A C2A 1.517(6) . ? C1A H1AA 1.0000 . ? C2A C3A 1.528(7) . ? C2A H2AA 0.9900 . ? C2A H2AB 0.9900 . ? C3A C4A 1.510(6) . ? C3A H3AA 0.9900 . ? C3A H3AB 0.9900 . ? C4A C1A 1.361(7) 8_645 ? C4A H4AA 1.0000 . ? C1B C4B 1.328(8) 11_556 ? C1B C2B 1.514(6) . ? C1B H1BA 1.0000 . ? C2B C3B 1.522(8) . ? C2B H2BA 0.9900 . ? C2B H2BB 0.9900 . ? C3B C4B 1.515(7) . ? C3B H3BA 0.9900 . ? C3B H3BB 0.9900 . ? C4B C1B 1.328(8) 8_645 ? C4B H4BA 1.0000 . ? 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 C5 Cu C4B 120.59(15) . 8_645 ? C5 Cu C4B 120.59(15) . . ? C4B Cu C4B 96.4(2) 8_645 . ? C5 Cu C4B 120.59(15) . 11_556 ? C4B Cu C4B 96.4(2) 8_645 11_556 ? C4B Cu C4B 96.4(2) . 11_556 ? C5 Cu C1B 101.92(14) . 11_556 ? C4B Cu C1B 34.4(2) 8_645 11_556 ? C4B Cu C1B 129.3(2) . 11_556 ? C4B Cu C1B 82.9(2) 11_556 11_556 ? C5 Cu C1B 101.92(14) . . ? C4B Cu C1B 129.3(2) 8_645 . ? C4B Cu C1B 82.9(2) . . ? C4B Cu C1B 34.4(2) 11_556 . ? C1B Cu C1B 115.85(10) 11_556 . ? C5 Cu C1B 101.92(14) . 8_645 ? C4B Cu C1B 82.9(2) 8_645 8_645 ? C4B Cu C1B 34.4(2) . 8_645 ? C4B Cu C1B 129.3(2) 11_556 8_645 ? C1B Cu C1B 115.85(10) 11_556 8_645 ? C1B Cu C1B 115.85(10) . 8_645 ? C5 Cu C4A 102.96(15) . 8_645 ? C4B Cu C4A 19.72(16) 8_645 8_645 ? C4B Cu C4A 100.3(2) . 8_645 ? C4B Cu C4A 114.9(2) 11_556 8_645 ? C1B Cu C4A 39.83(19) 11_556 8_645 ? C1B Cu C4A 148.7(2) . 8_645 ? C1B Cu C4A 76.98(18) 8_645 8_645 ? C5 Cu C4A 102.96(15) . . ? C4B Cu C4A 114.9(2) 8_645 . ? C4B Cu C4A 19.72(16) . . ? C4B Cu C4A 100.3(2) 11_556 . ? C1B Cu C4A 148.7(2) 11_556 . ? C1B Cu C4A 76.98(18) . . ? C1B Cu C4A 39.83(19) 8_645 . ? C4A Cu C4A 115.12(11) 8_645 . ? C5 Cu C4A 102.96(15) . 11_556 ? C4B Cu C4A 100.3(2) 8_645 11_556 ? C4B Cu C4A 114.9(2) . 11_556 ? C4B Cu C4A 19.72(16) 11_556 11_556 ? C1B Cu C4A 76.98(18) 11_556 11_556 ? C1B Cu C4A 39.83(19) . 11_556 ? C1B Cu C4A 148.7(2) 8_645 11_556 ? C4A Cu C4A 115.12(11) 8_645 11_556 ? C4A Cu C4A 115.12(11) . 11_556 ? C5 Cu C1A 122.77(12) . 11_556 ? C4B Cu C1A 18.79(15) 8_645 11_556 ? C4B Cu C1A 107.15(19) . 11_556 ? C4B Cu C1A 79.96(16) 11_556 11_556 ? C1B Cu C1A 22.51(16) 11_556 11_556 ? C1B Cu C1A 114.1(2) . 11_556 ? C1B Cu C1A 100.34(19) 8_645 11_556 ? C4A Cu C1A 34.95(18) 8_645 11_556 ? C4A Cu C1A 126.8(2) . 11_556 ? C4A Cu C1A 81.74(17) 11_556 11_556 ? C5 Cu C1A 122.77(12) . . ? C4B Cu C1A 107.15(19) 8_645 . ? C4B Cu C1A 79.96(16) . . ? C4B Cu C1A 18.79(15) 11_556 . ? C1B Cu C1A 100.34(19) 11_556 . ? C1B Cu C1A 22.51(16) . . ? C1B Cu C1A 114.1(2) 8_645 . ? C4A Cu C1A 126.8(2) 8_645 . ? C4A Cu C1A 81.74(16) . . ? C4A Cu C1A 34.95(18) 11_556 . ? C1A Cu C1A 93.47(16) 11_556 . ? F2 Sb F2 91.19(11) . 7_665 ? F2 Sb F2 91.19(11) . 10_646 ? F2 Sb F2 91.19(11) 7_665 10_646 ? F2 Sb F1 177.40(10) . . ? F2 Sb F1 91.41(10) 7_665 . ? F2 Sb F1 88.73(10) 10_646 . ? F2 Sb F1 88.73(10) . 7_665 ? F2 Sb F1 177.40(10) 7_665 7_665 ? F2 Sb F1 91.41(10) 10_646 7_665 ? F1 Sb F1 88.67(8) . 7_665 ? F2 Sb F1 91.41(10) . 10_646 ? F2 Sb F1 88.73(10) 7_665 10_646 ? F2 Sb F1 177.40(10) 10_646 10_646 ? F1 Sb F1 88.67(8) . 10_646 ? F1 Sb F1 88.67(8) 7_665 10_646 ? O C5 Cu 180.0(5) . . ? C4A C1A C2A 126.0(5) 11_556 . ? C4A C1A Cu 72.5(3) 11_556 . ? C2A C1A Cu 96.1(3) . . ? C4A C1A H1AA 116.1 11_556 . ? C2A C1A H1AA 116.1 . . ? Cu C1A H1AA 116.1 . . ? C1A C2A C3A 110.7(5) . . ? C1A C2A H2AA 109.5 . . ? C3A C2A H2AA 109.5 . . ? C1A C2A H2AB 109.5 . . ? C3A C2A H2AB 109.5 . . ? H2AA C2A H2AB 108.1 . . ? C4A C3A C2A 111.9(5) . . ? C4A C3A H3AA 109.2 . . ? C2A C3A H3AA 109.2 . . ? C4A C3A H3AB 109.2 . . ? C2A C3A H3AB 109.2 . . ? H3AA C3A H3AB 107.9 . . ? C1A C4A C3A 122.4(5) 8_645 . ? C1A C4A Cu 72.6(3) 8_645 . ? C3A C4A Cu 105.8(3) . . ? C1A C4A H4AA 115.7 8_645 . ? C3A C4A H4AA 115.7 . . ? Cu C4A H4AA 115.7 . . ? C4B C1B C2B 124.2(6) 11_556 . ? C4B C1B Cu 72.1(3) 11_556 . ? C2B C1B Cu 105.2(4) . . ? C4B C1B H1BA 115.3 11_556 . ? C2B C1B H1BA 115.3 . . ? Cu C1B H1BA 115.3 . . ? C1B C2B C3B 112.0(5) . . ? C1B C2B H2BA 109.2 . . ? C3B C2B H2BA 109.2 . . ? C1B C2B H2BB 109.2 . . ? C3B C2B H2BB 109.2 . . ? H2BA C2B H2BB 107.9 . . ? C4B C3B C2B 111.5(5) . . ? C4B C3B H3BA 109.3 . . ? C2B C3B H3BA 109.3 . . ? C4B C3B H3BB 109.3 . . ? C2B C3B H3BB 109.3 . . ? H3BA C3B H3BB 108.0 . . ? C1B C4B C3B 129.0(6) 8_645 . ? C1B C4B Cu 73.5(3) 8_645 . ? C3B C4B Cu 96.8(4) . . ? C1B C4B H4BA 114.7 8_645 . ? C3B C4B H4BA 114.7 . . ? Cu C4B H4BA 114.7 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.537 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.056 #===