Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Bolte, Michael' 'Green, Jennifer C.' 'Lerner, Hans-Wolfram' 'Scholz, Stefan' 'Wagner, Matthias' _publ_requested_journal 'Chemical Communications' #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Matthias Wagner' _publ_contact_author_address ; Contact Address Inorganic Chemistry Universität Frankfurt Marie-Curie-Str. 11 Frankfurt (Main) D-60439 GERMANY ; _publ_contact_author_phone '49 69 798 29136' _publ_contact_author_fax '49 69 798 29128' _publ_contact_author_email MATTHIAS.WAGNER@CHEMIE.UNI-FRANKFURT.DE _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission as deposition of data for the Cambridge Crystallographic Database. ; #============================================================================== # # 3. TITLE AND AUTHOR LIST _publ_section_title ; A novel multidecker sandwich complex from the reaction of ferrocene with GaCl3. ; data_wa73 _database_code_CSD 170258 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cl4 Fe Ga' _chemical_formula_weight 397.55 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, y, -z+1/2' 'x, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, -y, z-1/2' '-x, y-1/2, -z' 'x-1/2, -y-1/2, -z-1/2' _cell_length_a 13.7170(10) _cell_length_b 8.6001(6) _cell_length_c 12.014(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1417.3(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 474 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 20. _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 3.647 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3882 _exptl_absorpt_correction_T_max 0.7118 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 123 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12390 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.02 _reflns_number_total 1339 _reflns_number_gt 985 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1339 _refine_ls_number_parameters 82 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0804 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Fe1 Fe 0.50704(6) 0.2500 0.75182(6) 0.0253(3) Uani 1 2 d S . . C1 C 0.4781(4) 0.1680(6) 0.9095(3) 0.0500(14) Uani 1 1 d . . . H1 H 0.4248 0.1025 0.9282 0.060 Uiso 1 1 calc R . . C2 C 0.5703(4) 0.1202(6) 0.8772(4) 0.0549(16) Uani 1 1 d . . . H2 H 0.5915 0.0154 0.8705 0.066 Uiso 1 1 calc R . . C3 C 0.6260(5) 0.2500 0.8563(6) 0.058(2) Uani 1 2 d S . . H3 H 0.6918 0.2500 0.8316 0.070 Uiso 1 2 calc SR . . C4 C 0.4050(3) 0.1679(6) 0.6383(4) 0.0452(13) Uani 1 1 d . . . H4 H 0.3510 0.1030 0.6552 0.054 Uiso 1 1 calc R . . C5 C 0.4991(4) 0.1173(6) 0.6089(3) 0.0448(13) Uani 1 1 d . . . H5 H 0.5200 0.0122 0.6034 0.054 Uiso 1 1 calc R . . C6 C 0.5568(6) 0.2500 0.5891(5) 0.050(2) Uani 1 2 d S . . H6 H 0.6232 0.2500 0.5664 0.060 Uiso 1 2 calc SR . . Ga1 Ga 0.70904(5) 0.2500 0.21096(6) 0.0313(2) Uani 1 2 d S . . Cl1 Cl 0.76842(14) 0.2500 0.37850(15) 0.0545(6) Uani 1 2 d S . . Cl2 Cl 0.55131(13) 0.2500 0.22173(16) 0.0517(5) Uani 1 2 d S . . Cl3 Cl 0.75771(9) 0.04433(17) 0.12312(13) 0.0573(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0309(6) 0.0196(5) 0.0255(5) 0.000 -0.0002(4) 0.000 C1 0.064(4) 0.061(4) 0.025(3) 0.015(2) -0.002(2) -0.027(3) C2 0.088(5) 0.034(3) 0.043(3) 0.007(2) -0.014(3) 0.023(3) C3 0.038(5) 0.083(7) 0.054(5) 0.000 -0.016(4) 0.000 C4 0.045(3) 0.046(3) 0.044(3) -0.003(2) -0.016(2) -0.012(2) C5 0.067(4) 0.039(3) 0.029(3) -0.012(2) -0.006(2) -0.001(3) C6 0.061(5) 0.059(6) 0.030(4) 0.000 0.013(3) 0.000 Ga1 0.0321(4) 0.0201(4) 0.0416(5) 0.000 0.0004(3) 0.000 Cl1 0.0567(13) 0.0653(14) 0.0415(11) 0.000 -0.0048(8) 0.000 Cl2 0.0319(10) 0.0347(11) 0.0885(14) 0.000 0.0018(9) 0.000 Cl3 0.0523(9) 0.0411(8) 0.0785(10) -0.0242(7) 0.0046(7) 0.0071(6) _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 Fe1 C3 2.059(7) . ? Fe1 C1 2.060(4) 3 ? Fe1 C1 2.060(4) . ? Fe1 C5 2.065(4) 3 ? Fe1 C5 2.065(4) . ? Fe1 C2 2.066(5) . ? Fe1 C2 2.066(5) 3 ? Fe1 C6 2.070(6) . ? Fe1 C4 2.078(4) . ? Fe1 C4 2.078(4) 3 ? C1 C2 1.386(6) . ? C1 C1 1.410(10) 3 ? C1 H1 0.9500 . ? C2 C3 1.376(7) . ? C2 H2 0.9500 . ? C3 C2 1.376(7) 3 ? C3 H3 0.9500 . ? C4 C5 1.406(6) . ? C4 C4 1.413(10) 3 ? C4 H4 0.9500 . ? C5 C6 1.410(6) . ? C5 H5 0.9500 . ? C6 C5 1.410(6) 3 ? C6 H6 0.9500 . ? Ga1 Cl3 2.1652(14) 3 ? Ga1 Cl3 2.1652(14) . ? Ga1 Cl2 2.168(2) . ? Ga1 Cl1 2.171(2) . ? 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 C3 Fe1 C1 65.9(3) . 3 ? C3 Fe1 C1 65.9(3) . . ? C1 Fe1 C1 40.0(3) 3 . ? C3 Fe1 C5 123.3(2) . 3 ? C1 Fe1 C5 124.4(2) 3 3 ? C1 Fe1 C5 160.7(2) . 3 ? C3 Fe1 C5 123.3(2) . . ? C1 Fe1 C5 160.7(2) 3 . ? C1 Fe1 C5 124.4(2) . . ? C5 Fe1 C5 67.1(3) 3 . ? C3 Fe1 C2 38.96(19) . . ? C1 Fe1 C2 66.15(19) 3 . ? C1 Fe1 C2 39.26(18) . . ? C5 Fe1 C2 158.0(2) 3 . ? C5 Fe1 C2 109.2(2) . . ? C3 Fe1 C2 38.96(19) . 3 ? C1 Fe1 C2 39.26(18) 3 3 ? C1 Fe1 C2 66.15(19) . 3 ? C5 Fe1 C2 109.2(2) 3 3 ? C5 Fe1 C2 158.0(2) . 3 ? C2 Fe1 C2 65.4(3) . 3 ? C3 Fe1 C6 108.3(3) . . ? C1 Fe1 C6 158.71(17) 3 . ? C1 Fe1 C6 158.71(17) . . ? C5 Fe1 C6 39.87(16) 3 . ? C5 Fe1 C6 39.87(16) . . ? C2 Fe1 C6 123.3(2) . . ? C2 Fe1 C6 123.3(2) 3 . ? C3 Fe1 C4 159.07(16) . . ? C1 Fe1 C4 126.2(2) 3 . ? C1 Fe1 C4 110.9(2) . . ? C5 Fe1 C4 66.82(19) 3 . ? C5 Fe1 C4 39.69(18) . . ? C2 Fe1 C4 125.3(2) . . ? C2 Fe1 C4 160.9(2) 3 . ? C6 Fe1 C4 66.6(2) . . ? C3 Fe1 C4 159.07(16) . 3 ? C1 Fe1 C4 110.9(2) 3 3 ? C1 Fe1 C4 126.2(2) . 3 ? C5 Fe1 C4 39.69(18) 3 3 ? C5 Fe1 C4 66.82(19) . 3 ? C2 Fe1 C4 160.9(2) . 3 ? C2 Fe1 C4 125.3(2) 3 3 ? C6 Fe1 C4 66.6(2) . 3 ? C4 Fe1 C4 39.7(3) . 3 ? C2 C1 C1 107.3(3) . 3 ? C2 C1 Fe1 70.6(3) . . ? C1 C1 Fe1 69.99(14) 3 . ? C2 C1 H1 126.4 . . ? C1 C1 H1 126.4 3 . ? Fe1 C1 H1 124.7 . . ? C3 C2 C1 108.5(5) . . ? C3 C2 Fe1 70.2(4) . . ? C1 C2 Fe1 70.1(3) . . ? C3 C2 H2 125.8 . . ? C1 C2 H2 125.8 . . ? Fe1 C2 H2 125.5 . . ? C2 C3 C2 108.5(7) . 3 ? C2 C3 Fe1 70.8(3) . . ? C2 C3 Fe1 70.8(3) 3 . ? C2 C3 H3 125.8 . . ? C2 C3 H3 125.7 3 . ? Fe1 C3 H3 124.3 . . ? C5 C4 C4 108.0(3) . 3 ? C5 C4 Fe1 69.6(2) . . ? C4 C4 Fe1 70.13(13) 3 . ? C5 C4 H4 126.0 . . ? C4 C4 H4 126.0 3 . ? Fe1 C4 H4 125.8 . . ? C4 C5 C6 107.9(5) . . ? C4 C5 Fe1 70.7(3) . . ? C6 C5 Fe1 70.3(3) . . ? C4 C5 H5 126.0 . . ? C6 C5 H5 126.0 . . ? Fe1 C5 H5 124.6 . . ? C5 C6 C5 108.1(7) . 3 ? C5 C6 Fe1 69.8(3) . . ? C5 C6 Fe1 69.8(3) 3 . ? C5 C6 H6 125.9 . . ? C5 C6 H6 125.9 3 . ? Fe1 C6 H6 126.0 . . ? Cl3 Ga1 Cl3 109.55(9) 3 . ? Cl3 Ga1 Cl2 109.69(5) 3 . ? Cl3 Ga1 Cl2 109.69(5) . . ? Cl3 Ga1 Cl1 109.64(6) 3 . ? Cl3 Ga1 Cl1 109.64(6) . . ? Cl2 Ga1 Cl1 108.61(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Fe1 C1 C2 -37.0(3) . . . . ? C1 Fe1 C1 C2 -117.6(3) 3 . . . ? C5 Fe1 C1 C2 -159.9(6) 3 . . . ? C5 Fe1 C1 C2 78.1(4) . . . . ? C2 Fe1 C1 C2 -79.8(4) 3 . . . ? C6 Fe1 C1 C2 41.6(8) . . . . ? C4 Fe1 C1 C2 120.6(3) . . . . ? C4 Fe1 C1 C2 162.9(3) 3 . . . ? C3 Fe1 C1 C1 80.63(13) . . . 3 ? C5 Fe1 C1 C1 -42.3(5) 3 . . 3 ? C5 Fe1 C1 C1 -164.4(2) . . . 3 ? C2 Fe1 C1 C1 117.6(3) . . . 3 ? C2 Fe1 C1 C1 37.83(19) 3 . . 3 ? C6 Fe1 C1 C1 159.2(7) . . . 3 ? C4 Fe1 C1 C1 -121.79(18) . . . 3 ? C4 Fe1 C1 C1 -79.52(19) 3 . . 3 ? C1 C1 C2 C3 -0.7(5) 3 . . . ? Fe1 C1 C2 C3 60.0(4) . . . . ? C1 C1 C2 Fe1 -60.70(13) 3 . . . ? C1 Fe1 C2 C3 -80.6(4) 3 . . . ? C1 Fe1 C2 C3 -119.2(5) . . . . ? C5 Fe1 C2 C3 43.1(7) 3 . . . ? C5 Fe1 C2 C3 119.5(4) . . . . ? C2 Fe1 C2 C3 -37.4(4) 3 . . . ? C6 Fe1 C2 C3 77.6(4) . . . . ? C4 Fe1 C2 C3 160.8(4) . . . . ? C4 Fe1 C2 C3 -165.9(5) 3 . . . ? C3 Fe1 C2 C1 119.2(5) . . . . ? C1 Fe1 C2 C1 38.6(3) 3 . . . ? C5 Fe1 C2 C1 162.3(4) 3 . . . ? C5 Fe1 C2 C1 -121.3(3) . . . . ? C2 Fe1 C2 C1 81.8(3) 3 . . . ? C6 Fe1 C2 C1 -163.2(3) . . . . ? C4 Fe1 C2 C1 -80.0(4) . . . . ? C4 Fe1 C2 C1 -46.7(7) 3 . . . ? C1 C2 C3 C2 1.1(8) . . . 3 ? Fe1 C2 C3 C2 61.1(5) . . . 3 ? C1 C2 C3 Fe1 -59.9(4) . . . . ? C1 Fe1 C3 C2 81.3(4) 3 . . . ? C1 Fe1 C3 C2 37.2(3) . . . . ? C5 Fe1 C3 C2 -162.2(3) 3 . . . ? C5 Fe1 C3 C2 -79.3(5) . . . . ? C2 Fe1 C3 C2 118.5(7) 3 . . . ? C6 Fe1 C3 C2 -120.8(3) . . . . ? C4 Fe1 C3 C2 -48.6(9) . . . . ? C4 Fe1 C3 C2 167.1(5) 3 . . . ? C1 Fe1 C3 C2 -37.2(3) 3 . . 3 ? C1 Fe1 C3 C2 -81.3(4) . . . 3 ? C5 Fe1 C3 C2 79.3(5) 3 . . 3 ? C5 Fe1 C3 C2 162.2(3) . . . 3 ? C2 Fe1 C3 C2 -118.5(7) . . . 3 ? C6 Fe1 C3 C2 120.8(3) . . . 3 ? C4 Fe1 C3 C2 -167.1(5) . . . 3 ? C4 Fe1 C3 C2 48.6(9) 3 . . 3 ? C3 Fe1 C4 C5 -41.9(8) . . . . ? C1 Fe1 C4 C5 -161.7(3) 3 . . . ? C1 Fe1 C4 C5 -119.1(3) . . . . ? C5 Fe1 C4 C5 81.6(4) 3 . . . ? C2 Fe1 C4 C5 -77.3(4) . . . . ? C2 Fe1 C4 C5 163.5(5) 3 . . . ? C6 Fe1 C4 C5 38.0(3) . . . . ? C4 Fe1 C4 C5 119.0(3) 3 . . . ? C3 Fe1 C4 C4 -160.9(7) . . . 3 ? C1 Fe1 C4 C4 79.25(19) 3 . . 3 ? C1 Fe1 C4 C4 121.87(19) . . . 3 ? C5 Fe1 C4 C4 -37.41(17) 3 . . 3 ? C5 Fe1 C4 C4 -119.0(3) . . . 3 ? C2 Fe1 C4 C4 163.7(2) . . . 3 ? C2 Fe1 C4 C4 44.5(6) 3 . . 3 ? C6 Fe1 C4 C4 -80.99(11) . . . 3 ? C4 C4 C5 C6 -0.9(4) 3 . . . ? Fe1 C4 C5 C6 -60.7(4) . . . . ? C4 C4 C5 Fe1 59.87(13) 3 . . . ? C3 Fe1 C5 C4 163.4(3) . . . . ? C1 Fe1 C5 C4 49.9(7) 3 . . . ? C1 Fe1 C5 C4 81.5(4) . . . . ? C5 Fe1 C5 C4 -80.8(3) 3 . . . ? C2 Fe1 C5 C4 122.5(3) . . . . ? C2 Fe1 C5 C4 -165.7(5) 3 . . . ? C6 Fe1 C5 C4 -118.1(5) . . . . ? C4 Fe1 C5 C4 -37.5(3) 3 . . . ? C3 Fe1 C5 C6 -78.4(4) . . . . ? C1 Fe1 C5 C6 168.1(5) 3 . . . ? C1 Fe1 C5 C6 -160.3(4) . . . . ? C5 Fe1 C5 C6 37.4(4) 3 . . . ? C2 Fe1 C5 C6 -119.3(4) . . . . ? C2 Fe1 C5 C6 -47.5(7) 3 . . . ? C4 Fe1 C5 C6 118.1(5) . . . . ? C4 Fe1 C5 C6 80.7(4) 3 . . . ? C4 C5 C6 C5 1.4(7) . . . 3 ? Fe1 C5 C6 C5 -59.6(4) . . . 3 ? C4 C5 C6 Fe1 61.0(3) . . . . ? C3 Fe1 C6 C5 120.4(3) . . . . ? C1 Fe1 C6 C5 -169.1(5) 3 . . . ? C1 Fe1 C6 C5 49.9(9) . . . . ? C5 Fe1 C6 C5 -119.2(6) 3 . . . ? C2 Fe1 C6 C5 80.1(4) . . . . ? C2 Fe1 C6 C5 160.7(3) 3 . . . ? C4 Fe1 C6 C5 -37.9(3) . . . . ? C4 Fe1 C6 C5 -81.3(4) 3 . . . ? C3 Fe1 C6 C5 -120.4(3) . . . 3 ? C1 Fe1 C6 C5 -49.9(9) 3 . . 3 ? C1 Fe1 C6 C5 169.1(5) . . . 3 ? C5 Fe1 C6 C5 119.2(6) . . . 3 ? C2 Fe1 C6 C5 -160.7(3) . . . 3 ? C2 Fe1 C6 C5 -80.1(4) 3 . . 3 ? C4 Fe1 C6 C5 81.3(4) . . . 3 ? C4 Fe1 C6 C5 37.9(3) 3 . . 3 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.415 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.107 data_wa22 _database_code_CSD 153729 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H10 Cl4 Fe Ga2' _chemical_formula_weight 467.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.5689(1) _cell_length_b 14.5558(1) _cell_length_c 10.7524(1) _cell_angle_alpha 90.00 _cell_angle_beta 113.243(1) _cell_angle_gamma 90.00 _cell_volume 1519.89(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1 _cell_measurement_theta_max 25 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.042 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 5.138 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2058 _exptl_absorpt_correction_T_max 0.6840 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 360 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1200 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31849 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 27.88 _reflns_number_total 3612 _reflns_number_gt 3030 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens XTL-Plus)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0193P)^2^+1.1909P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3612 _refine_ls_number_parameters 154 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0575 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.63412(3) 0.200636(19) 0.71913(3) 0.02419(8) Uani 1 1 d . . . Cl1 Cl 0.58202(8) 0.25831(6) 0.87770(8) 0.04341(19) Uani 1 1 d . . . Cl2 Cl 0.77005(8) 0.08327(5) 0.79317(8) 0.04272(19) Uani 1 1 d . . . Cl3 Cl 0.74354(8) 0.30363(5) 0.64882(8) 0.03961(18) Uani 1 1 d . . . Cl4 Cl 0.44727(7) 0.16432(5) 0.54605(7) 0.03860(17) Uani 1 1 d . . . Ga2 Ga 0.54380(3) 0.27948(2) 0.34299(3) 0.03571(9) Uani 1 1 d . . . Fe1 Fe 0.74822(3) 0.53539(2) 0.24381(3) 0.01945(8) Uani 1 1 d . . . C1 C 0.7773(3) 0.67383(16) 0.2642(3) 0.0273(6) Uani 1 1 d . . . H1 H 0.7355 0.7145 0.3059 0.033 Uiso 1 1 calc R . . C2 C 0.7238(3) 0.64876(17) 0.1240(3) 0.0277(6) Uani 1 1 d . . . H2 H 0.6402 0.6701 0.0559 0.033 Uiso 1 1 calc R . . C3 C 0.8184(3) 0.58588(17) 0.1045(3) 0.0294(6) Uani 1 1 d . . . H3 H 0.8083 0.5579 0.0213 0.035 Uiso 1 1 calc R . . C4 C 0.9299(3) 0.57264(18) 0.2308(3) 0.0302(6) Uani 1 1 d . . . H4 H 1.0077 0.5346 0.2467 0.036 Uiso 1 1 calc R . . C5 C 0.9051(3) 0.62634(17) 0.3300(3) 0.0296(6) Uani 1 1 d . . . H5 H 0.9634 0.6299 0.4234 0.035 Uiso 1 1 calc R . . C11 C 0.6086(3) 0.50303(18) 0.3254(3) 0.0306(6) Uani 1 1 d . . . H11 H 0.5633 0.5449 0.3620 0.037 Uiso 1 1 calc R . . C12 C 0.5597(3) 0.47349(17) 0.1883(3) 0.0300(6) Uani 1 1 d . . . H12 H 0.4763 0.4922 0.1173 0.036 Uiso 1 1 calc R . . C13 C 0.6576(3) 0.41106(17) 0.1763(3) 0.0289(6) Uani 1 1 d . . . H13 H 0.6509 0.3805 0.0959 0.035 Uiso 1 1 calc R . . C14 C 0.7676(3) 0.40231(17) 0.3061(3) 0.0293(6) Uani 1 1 d . . . H14 H 0.8473 0.3652 0.3274 0.035 Uiso 1 1 calc R . . C15 C 0.7364(3) 0.45929(17) 0.3982(3) 0.0310(6) Uani 1 1 d . . . H15 H 0.7916 0.4666 0.4919 0.037 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 Ga1 0.02159(14) 0.02874(15) 0.02324(15) 0.00224(11) 0.00990(12) -0.00055(11) Cl1 0.0375(4) 0.0611(5) 0.0359(4) -0.0163(3) 0.0189(3) -0.0049(3) Cl2 0.0380(4) 0.0381(4) 0.0548(5) 0.0159(3) 0.0212(4) 0.0111(3) Cl3 0.0377(4) 0.0425(4) 0.0346(4) 0.0100(3) 0.0100(3) -0.0138(3) Cl4 0.0279(4) 0.0550(4) 0.0298(4) -0.0042(3) 0.0080(3) -0.0103(3) Ga2 0.03294(18) 0.04051(19) 0.03358(19) 0.00243(14) 0.01300(14) 0.00433(14) Fe1 0.02217(18) 0.01581(16) 0.02017(18) -0.00013(13) 0.00815(15) -0.00068(13) C1 0.0318(14) 0.0167(11) 0.0358(15) -0.0008(10) 0.0158(12) -0.0044(10) C2 0.0270(13) 0.0233(12) 0.0310(15) 0.0076(11) 0.0096(12) -0.0021(10) C3 0.0368(15) 0.0277(13) 0.0307(15) -0.0019(11) 0.0206(13) -0.0074(11) C4 0.0248(14) 0.0267(13) 0.0406(16) -0.0005(12) 0.0146(12) -0.0012(11) C5 0.0265(14) 0.0274(13) 0.0306(15) -0.0018(11) 0.0068(12) -0.0057(11) C11 0.0385(15) 0.0253(13) 0.0367(16) 0.0020(12) 0.0242(13) -0.0016(11) C12 0.0258(14) 0.0268(13) 0.0341(15) 0.0050(11) 0.0083(12) -0.0053(11) C13 0.0383(16) 0.0204(12) 0.0276(14) -0.0038(10) 0.0128(12) -0.0095(11) C14 0.0343(15) 0.0185(12) 0.0323(15) 0.0039(10) 0.0102(12) 0.0000(10) C15 0.0434(17) 0.0267(13) 0.0219(14) 0.0020(11) 0.0119(12) -0.0060(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 Ga1 Cl1 2.1578(7) . ? Ga1 Cl2 2.1710(8) . ? Ga1 Cl4 2.1776(7) . ? Ga1 Cl3 2.2014(7) . ? Fe1 C14 2.033(2) . ? Fe1 C1 2.037(2) . ? Fe1 C5 2.037(3) . ? Fe1 C15 2.040(3) . ? Fe1 C13 2.042(2) . ? Fe1 C2 2.046(2) . ? Fe1 C11 2.048(3) . ? Fe1 C12 2.050(3) . ? Fe1 C3 2.052(2) . ? Fe1 C4 2.053(3) . ? C1 C5 1.432(4) . ? C1 C2 1.433(4) . ? C1 H1 0.9500 . ? C2 C3 1.431(4) . ? C2 H2 0.9500 . ? C3 C4 1.416(4) . ? C3 H3 0.9500 . ? C4 C5 1.427(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C11 C15 1.417(4) . ? C11 C12 1.423(4) . ? C11 H11 0.9500 . ? C12 C13 1.421(4) . ? C12 H12 0.9500 . ? C13 C14 1.426(4) . ? C13 H13 0.9500 . ? C14 C15 1.427(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? 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 Cl1 Ga1 Cl2 110.77(3) . . ? Cl1 Ga1 Cl4 109.97(3) . . ? Cl2 Ga1 Cl4 111.60(3) . . ? Cl1 Ga1 Cl3 109.81(3) . . ? Cl2 Ga1 Cl3 107.49(3) . . ? Cl4 Ga1 Cl3 107.10(3) . . ? C14 Fe1 C1 156.30(11) . . ? C14 Fe1 C5 120.75(11) . . ? C1 Fe1 C5 41.16(10) . . ? C14 Fe1 C15 41.00(10) . . ? C1 Fe1 C15 120.30(11) . . ? C5 Fe1 C15 106.44(11) . . ? C14 Fe1 C13 40.97(11) . . ? C1 Fe1 C13 160.80(11) . . ? C5 Fe1 C13 157.10(11) . . ? C15 Fe1 C13 68.73(11) . . ? C14 Fe1 C2 161.25(11) . . ? C1 Fe1 C2 41.08(10) . . ? C5 Fe1 C2 68.91(11) . . ? C15 Fe1 C2 156.51(11) . . ? C13 Fe1 C2 124.46(11) . . ? C14 Fe1 C11 68.63(11) . . ? C1 Fe1 C11 106.56(11) . . ? C5 Fe1 C11 123.35(11) . . ? C15 Fe1 C11 40.57(11) . . ? C13 Fe1 C11 68.41(11) . . ? C2 Fe1 C11 121.47(11) . . ? C14 Fe1 C12 68.72(11) . . ? C1 Fe1 C12 123.65(11) . . ? C5 Fe1 C12 160.36(11) . . ? C15 Fe1 C12 68.51(11) . . ? C13 Fe1 C12 40.63(10) . . ? C2 Fe1 C12 107.72(10) . . ? C11 Fe1 C12 40.64(11) . . ? C14 Fe1 C3 124.28(11) . . ? C1 Fe1 C3 69.00(10) . . ? C5 Fe1 C3 68.60(11) . . ? C15 Fe1 C3 160.77(12) . . ? C13 Fe1 C3 108.19(11) . . ? C2 Fe1 C3 40.87(10) . . ? C11 Fe1 C3 157.61(11) . . ? C12 Fe1 C3 122.34(11) . . ? C14 Fe1 C4 107.39(11) . . ? C1 Fe1 C4 68.94(10) . . ? C5 Fe1 C4 40.85(10) . . ? C15 Fe1 C4 123.94(11) . . ? C13 Fe1 C4 122.02(11) . . ? C2 Fe1 C4 68.47(11) . . ? C11 Fe1 C4 160.39(11) . . ? C12 Fe1 C4 157.60(11) . . ? C3 Fe1 C4 40.36(11) . . ? C5 C1 C2 107.5(2) . . ? C5 C1 Fe1 69.41(14) . . ? C2 C1 Fe1 69.81(14) . . ? C5 C1 H1 126.3 . . ? C2 C1 H1 126.3 . . ? Fe1 C1 H1 126.1 . . ? C3 C2 C1 108.0(2) . . ? C3 C2 Fe1 69.78(14) . . ? C1 C2 Fe1 69.11(14) . . ? C3 C2 H2 126.0 . . ? C1 C2 H2 126.0 . . ? Fe1 C2 H2 126.7 . . ? C4 C3 C2 108.2(2) . . ? C4 C3 Fe1 69.83(15) . . ? C2 C3 Fe1 69.35(14) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe1 C3 H3 126.5 . . ? C3 C4 C5 108.3(2) . . ? C3 C4 Fe1 69.81(14) . . ? C5 C4 Fe1 68.98(15) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 126.9 . . ? C4 C5 C1 108.1(2) . . ? C4 C5 Fe1 70.16(15) . . ? C1 C5 Fe1 69.43(14) . . ? C4 C5 H5 125.9 . . ? C1 C5 H5 125.9 . . ? Fe1 C5 H5 126.0 . . ? C15 C11 C12 108.3(2) . . ? C15 C11 Fe1 69.44(15) . . ? C12 C11 Fe1 69.75(15) . . ? C15 C11 H11 125.9 . . ? C12 C11 H11 125.9 . . ? Fe1 C11 H11 126.5 . . ? C13 C12 C11 107.9(2) . . ? C13 C12 Fe1 69.41(14) . . ? C11 C12 Fe1 69.61(15) . . ? C13 C12 H12 126.0 . . ? C11 C12 H12 126.0 . . ? Fe1 C12 H12 126.5 . . ? C12 C13 C14 108.1(2) . . ? C12 C13 Fe1 69.96(14) . . ? C14 C13 Fe1 69.18(14) . . ? C12 C13 H13 126.0 . . ? C14 C13 H13 126.0 . . ? Fe1 C13 H13 126.5 . . ? C13 C14 C15 107.8(2) . . ? C13 C14 Fe1 69.85(14) . . ? C15 C14 Fe1 69.77(14) . . ? C13 C14 H14 126.1 . . ? C15 C14 H14 126.1 . . ? Fe1 C14 H14 125.8 . . ? C11 C15 C14 108.0(2) . . ? C11 C15 Fe1 69.99(15) . . ? C14 C15 Fe1 69.23(14) . . ? C11 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? Fe1 C15 H15 126.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Fe1 C1 C5 47.7(3) . . . . ? C15 Fe1 C1 C5 80.19(18) . . . . ? C13 Fe1 C1 C5 -166.2(3) . . . . ? C2 Fe1 C1 C5 -118.7(2) . . . . ? C11 Fe1 C1 C5 122.10(17) . . . . ? C12 Fe1 C1 C5 163.25(16) . . . . ? C3 Fe1 C1 C5 -81.10(17) . . . . ? C4 Fe1 C1 C5 -37.71(16) . . . . ? C14 Fe1 C1 C2 166.4(2) . . . . ? C5 Fe1 C1 C2 118.7(2) . . . . ? C15 Fe1 C1 C2 -161.12(15) . . . . ? C13 Fe1 C1 C2 -47.5(4) . . . . ? C11 Fe1 C1 C2 -119.20(16) . . . . ? C12 Fe1 C1 C2 -78.06(18) . . . . ? C3 Fe1 C1 C2 37.60(15) . . . . ? C4 Fe1 C1 C2 80.98(16) . . . . ? C5 C1 C2 C3 0.3(3) . . . . ? Fe1 C1 C2 C3 -59.16(17) . . . . ? C5 C1 C2 Fe1 59.43(17) . . . . ? C14 Fe1 C2 C3 -43.4(4) . . . . ? C1 Fe1 C2 C3 119.5(2) . . . . ? C5 Fe1 C2 C3 81.26(17) . . . . ? C15 Fe1 C2 C3 164.0(3) . . . . ? C13 Fe1 C2 C3 -77.61(18) . . . . ? C11 Fe1 C2 C3 -161.68(16) . . . . ? C12 Fe1 C2 C3 -119.27(16) . . . . ? C4 Fe1 C2 C3 37.26(15) . . . . ? C14 Fe1 C2 C1 -162.9(3) . . . . ? C5 Fe1 C2 C1 -38.23(15) . . . . ? C15 Fe1 C2 C1 44.5(3) . . . . ? C13 Fe1 C2 C1 162.90(15) . . . . ? C11 Fe1 C2 C1 78.83(18) . . . . ? C12 Fe1 C2 C1 121.24(16) . . . . ? C3 Fe1 C2 C1 -119.5(2) . . . . ? C4 Fe1 C2 C1 -82.23(16) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? Fe1 C2 C3 C4 -59.23(17) . . . . ? C1 C2 C3 Fe1 58.74(17) . . . . ? C14 Fe1 C3 C4 -75.92(18) . . . . ? C1 Fe1 C3 C4 81.80(16) . . . . ? C5 Fe1 C3 C4 37.50(15) . . . . ? C15 Fe1 C3 C4 -40.9(4) . . . . ? C13 Fe1 C3 C4 -118.37(16) . . . . ? C2 Fe1 C3 C4 119.6(2) . . . . ? C11 Fe1 C3 C4 164.3(3) . . . . ? C12 Fe1 C3 C4 -160.85(15) . . . . ? C14 Fe1 C3 C2 164.50(15) . . . . ? C1 Fe1 C3 C2 -37.78(15) . . . . ? C5 Fe1 C3 C2 -82.08(16) . . . . ? C15 Fe1 C3 C2 -160.5(3) . . . . ? C13 Fe1 C3 C2 122.05(16) . . . . ? C11 Fe1 C3 C2 44.7(3) . . . . ? C12 Fe1 C3 C2 79.57(18) . . . . ? C4 Fe1 C3 C2 -119.6(2) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? Fe1 C3 C4 C5 -58.41(18) . . . . ? C2 C3 C4 Fe1 58.93(17) . . . . ? C14 Fe1 C4 C3 122.87(16) . . . . ? C1 Fe1 C4 C3 -81.96(16) . . . . ? C5 Fe1 C4 C3 -119.9(2) . . . . ? C15 Fe1 C4 C3 164.93(15) . . . . ? C13 Fe1 C4 C3 80.37(18) . . . . ? C2 Fe1 C4 C3 -37.71(15) . . . . ? C11 Fe1 C4 C3 -162.1(3) . . . . ? C12 Fe1 C4 C3 46.6(3) . . . . ? C14 Fe1 C4 C5 -117.19(16) . . . . ? C1 Fe1 C4 C5 37.99(16) . . . . ? C15 Fe1 C4 C5 -75.13(19) . . . . ? C13 Fe1 C4 C5 -159.69(15) . . . . ? C2 Fe1 C4 C5 82.23(17) . . . . ? C11 Fe1 C4 C5 -42.2(4) . . . . ? C12 Fe1 C4 C5 166.6(2) . . . . ? C3 Fe1 C4 C5 119.9(2) . . . . ? C3 C4 C5 C1 -0.4(3) . . . . ? Fe1 C4 C5 C1 -59.27(17) . . . . ? C3 C4 C5 Fe1 58.92(18) . . . . ? C2 C1 C5 C4 0.1(3) . . . . ? Fe1 C1 C5 C4 59.73(17) . . . . ? C2 C1 C5 Fe1 -59.68(17) . . . . ? C14 Fe1 C5 C4 81.01(18) . . . . ? C1 Fe1 C5 C4 -119.2(2) . . . . ? C15 Fe1 C5 C4 123.28(17) . . . . ? C13 Fe1 C5 C4 49.1(3) . . . . ? C2 Fe1 C5 C4 -81.06(17) . . . . ? C11 Fe1 C5 C4 164.35(16) . . . . ? C12 Fe1 C5 C4 -164.8(3) . . . . ? C3 Fe1 C5 C4 -37.07(16) . . . . ? C14 Fe1 C5 C1 -159.77(15) . . . . ? C15 Fe1 C5 C1 -117.50(16) . . . . ? C13 Fe1 C5 C1 168.4(2) . . . . ? C2 Fe1 C5 C1 38.16(15) . . . . ? C11 Fe1 C5 C1 -76.43(19) . . . . ? C12 Fe1 C5 C1 -45.5(4) . . . . ? C3 Fe1 C5 C1 82.16(17) . . . . ? C4 Fe1 C5 C1 119.2(2) . . . . ? C14 Fe1 C11 C15 37.91(15) . . . . ? C1 Fe1 C11 C15 -117.53(16) . . . . ? C5 Fe1 C11 C15 -75.65(18) . . . . ? C13 Fe1 C11 C15 82.09(17) . . . . ? C2 Fe1 C11 C15 -159.79(15) . . . . ? C12 Fe1 C11 C15 119.7(2) . . . . ? C3 Fe1 C11 C15 167.5(2) . . . . ? C4 Fe1 C11 C15 -43.9(4) . . . . ? C14 Fe1 C11 C12 -81.81(16) . . . . ? C1 Fe1 C11 C12 122.76(16) . . . . ? C5 Fe1 C11 C12 164.63(15) . . . . ? C15 Fe1 C11 C12 -119.7(2) . . . . ? C13 Fe1 C11 C12 -37.62(15) . . . . ? C2 Fe1 C11 C12 80.50(18) . . . . ? C3 Fe1 C11 C12 47.8(3) . . . . ? C4 Fe1 C11 C12 -163.6(3) . . . . ? C15 C11 C12 C13 0.1(3) . . . . ? Fe1 C11 C12 C13 59.04(17) . . . . ? C15 C11 C12 Fe1 -58.92(18) . . . . ? C14 Fe1 C12 C13 -37.78(16) . . . . ? C1 Fe1 C12 C13 165.12(15) . . . . ? C5 Fe1 C12 C13 -160.5(3) . . . . ? C15 Fe1 C12 C13 -81.97(17) . . . . ? C2 Fe1 C12 C13 122.67(16) . . . . ? C11 Fe1 C12 C13 -119.3(2) . . . . ? C3 Fe1 C12 C13 80.17(18) . . . . ? C4 Fe1 C12 C13 46.3(3) . . . . ? C14 Fe1 C12 C11 81.56(17) . . . . ? C1 Fe1 C12 C11 -75.53(18) . . . . ? C5 Fe1 C12 C11 -41.2(4) . . . . ? C15 Fe1 C12 C11 37.38(15) . . . . ? C13 Fe1 C12 C11 119.3(2) . . . . ? C2 Fe1 C12 C11 -117.98(16) . . . . ? C3 Fe1 C12 C11 -160.48(15) . . . . ? C4 Fe1 C12 C11 165.6(3) . . . . ? C11 C12 C13 C14 -0.3(3) . . . . ? Fe1 C12 C13 C14 58.86(17) . . . . ? C11 C12 C13 Fe1 -59.17(17) . . . . ? C14 Fe1 C13 C12 119.5(2) . . . . ? C1 Fe1 C13 C12 -40.5(4) . . . . ? C5 Fe1 C13 C12 163.3(3) . . . . ? C15 Fe1 C13 C12 81.37(17) . . . . ? C2 Fe1 C13 C12 -76.53(19) . . . . ? C11 Fe1 C13 C12 37.64(16) . . . . ? C3 Fe1 C13 C12 -118.81(17) . . . . ? C4 Fe1 C13 C12 -161.04(16) . . . . ? C1 Fe1 C13 C14 -160.0(3) . . . . ? C5 Fe1 C13 C14 43.8(3) . . . . ? C15 Fe1 C13 C14 -38.10(16) . . . . ? C2 Fe1 C13 C14 164.00(15) . . . . ? C11 Fe1 C13 C14 -81.83(17) . . . . ? C12 Fe1 C13 C14 -119.5(2) . . . . ? C3 Fe1 C13 C14 121.72(16) . . . . ? C4 Fe1 C13 C14 79.49(18) . . . . ? C12 C13 C14 C15 0.4(3) . . . . ? Fe1 C13 C14 C15 59.72(17) . . . . ? C12 C13 C14 Fe1 -59.35(17) . . . . ? C1 Fe1 C14 C13 163.8(2) . . . . ? C5 Fe1 C14 C13 -161.73(15) . . . . ? C15 Fe1 C14 C13 118.8(2) . . . . ? C2 Fe1 C14 C13 -45.0(4) . . . . ? C11 Fe1 C14 C13 81.26(17) . . . . ? C12 Fe1 C14 C13 37.47(16) . . . . ? C3 Fe1 C14 C13 -77.95(19) . . . . ? C4 Fe1 C14 C13 -119.12(16) . . . . ? C1 Fe1 C14 C15 45.0(3) . . . . ? C5 Fe1 C14 C15 79.49(19) . . . . ? C13 Fe1 C14 C15 -118.8(2) . . . . ? C2 Fe1 C14 C15 -163.8(3) . . . . ? C11 Fe1 C14 C15 -37.52(16) . . . . ? C12 Fe1 C14 C15 -81.30(18) . . . . ? C3 Fe1 C14 C15 163.27(16) . . . . ? C4 Fe1 C14 C15 122.10(17) . . . . ? C12 C11 C15 C14 0.1(3) . . . . ? Fe1 C11 C15 C14 -59.01(17) . . . . ? C12 C11 C15 Fe1 59.11(17) . . . . ? C13 C14 C15 C11 -0.3(3) . . . . ? Fe1 C14 C15 C11 59.48(18) . . . . ? C13 C14 C15 Fe1 -59.77(17) . . . . ? C14 Fe1 C15 C11 -119.3(2) . . . . ? C1 Fe1 C15 C11 79.92(18) . . . . ? C5 Fe1 C15 C11 122.46(16) . . . . ? C13 Fe1 C15 C11 -81.23(17) . . . . ? C2 Fe1 C15 C11 47.7(3) . . . . ? C12 Fe1 C15 C11 -37.44(16) . . . . ? C3 Fe1 C15 C11 -165.5(3) . . . . ? C4 Fe1 C15 C11 163.70(15) . . . . ? C1 Fe1 C15 C14 -160.78(15) . . . . ? C5 Fe1 C15 C14 -118.24(16) . . . . ? C13 Fe1 C15 C14 38.07(16) . . . . ? C2 Fe1 C15 C14 167.0(2) . . . . ? C11 Fe1 C15 C14 119.3(2) . . . . ? C12 Fe1 C15 C14 81.86(17) . . . . ? C3 Fe1 C15 C14 -46.2(4) . . . . ? C4 Fe1 C15 C14 -77.00(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.343 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.083 data_wa36 _database_code_CSD 153730 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H16 Cl4 Co Ga' _chemical_formula_weight 478.74 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ga' 'Ga' 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 11.744(1) _cell_length_b 15.226(1) _cell_length_c 11.1345(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.851(5) _cell_angle_gamma 90.00 _cell_volume 1905.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 512 _cell_measurement_theta_min 1 _cell_measurement_theta_max 20 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 2.837 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5741 _exptl_absorpt_correction_T_max 0.7645 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _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 'Siemens CCD three-circle diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 123 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 1400 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11589 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0839 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 27.02 _reflns_number_total 3731 _reflns_number_gt 2718 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens XTL-Plus)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 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 0.412(13) _refine_ls_number_reflns 3731 _refine_ls_number_parameters 200 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0755 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0514 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ga1 Ga 0.64338(5) 0.61540(3) 0.65065(5) 0.03324(15) Uani 1 1 d . . . Cl1 Cl 0.55592(13) 0.72589(9) 0.53708(14) 0.0585(5) Uani 1 1 d . . . Cl2 Cl 0.51160(11) 0.53808(10) 0.70623(13) 0.0458(4) Uani 1 1 d . . . Cl3 Cl 0.72905(12) 0.53628(10) 0.53967(12) 0.0466(4) Uani 1 1 d . . . Cl4 Cl 0.77487(12) 0.66279(10) 0.81770(12) 0.0534(4) Uani 1 1 d . . . Co1 Co 0.62247(6) 0.25642(4) 0.62216(5) 0.02742(16) Uani 1 1 d . . . C1 C 0.4526(5) 0.2225(5) 0.6028(6) 0.0512(17) Uani 1 1 d . . . H1 H 0.4243 0.1942 0.6646 0.061 Uiso 1 1 calc R . . C2 C 0.4929(5) 0.1812(4) 0.5115(6) 0.0491(18) Uani 1 1 d . . . H2 H 0.4965 0.1196 0.4996 0.059 Uiso 1 1 calc R . . C3 C 0.5270(6) 0.2457(6) 0.4404(6) 0.061(2) Uani 1 1 d . . . H3 H 0.5585 0.2361 0.3720 0.074 Uiso 1 1 calc R . . C4 C 0.5069(6) 0.3261(4) 0.4872(6) 0.057(2) Uani 1 1 d . . . H4 H 0.5218 0.3816 0.4561 0.068 Uiso 1 1 calc R . . C5 C 0.4610(5) 0.3124(5) 0.5875(6) 0.0539(19) Uani 1 1 d . . . H5 H 0.4393 0.3567 0.6368 0.065 Uiso 1 1 calc R . . C11 C 0.7196(5) 0.2388(5) 0.8029(5) 0.0501(18) Uani 1 1 d . . . H11 H 0.6894 0.2255 0.8713 0.060 Uiso 1 1 calc R . . C12 C 0.7539(5) 0.1771(4) 0.7247(5) 0.0481(18) Uani 1 1 d . . . H12 H 0.7504 0.1149 0.7306 0.058 Uiso 1 1 calc R . . C13 C 0.7938(4) 0.2243(5) 0.6374(5) 0.0433(16) Uani 1 1 d . . . H13 H 0.8229 0.1995 0.5737 0.052 Uiso 1 1 calc R . . C14 C 0.7841(5) 0.3140(4) 0.6589(6) 0.0465(17) Uani 1 1 d . . . H14 H 0.8050 0.3603 0.6121 0.056 Uiso 1 1 calc R . . C15 C 0.7383(5) 0.3242(5) 0.7607(6) 0.056(2) Uani 1 1 d . . . H15 H 0.7226 0.3783 0.7953 0.067 Uiso 1 1 calc R . . C21 C 0.1943(8) 0.5855(4) 0.2794(8) 0.068(2) Uani 1 1 d . . . H21 H 0.2271 0.6280 0.2364 0.082 Uiso 1 1 calc R . . C22 C 0.0783(6) 0.5604(4) 0.2311(6) 0.0605(18) Uani 1 1 d . . . H22 H 0.0308 0.5855 0.1549 0.073 Uiso 1 1 calc R . . C23 C 0.0305(5) 0.4990(4) 0.2924(6) 0.0531(17) Uani 1 1 d . . . H23 H -0.0498 0.4808 0.2584 0.064 Uiso 1 1 calc R . . C24 C 0.0990(7) 0.4641(4) 0.4028(6) 0.0615(18) Uani 1 1 d . . . H24 H 0.0668 0.4224 0.4475 0.074 Uiso 1 1 calc R . . C25 C 0.2162(7) 0.4909(5) 0.4478(6) 0.069(2) Uani 1 1 d . . . H25 H 0.2653 0.4665 0.5237 0.083 Uiso 1 1 calc R . . C26 C 0.2621(6) 0.5508(5) 0.3863(8) 0.072(2) Uani 1 1 d . . . H26 H 0.3427 0.5685 0.4190 0.087 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 Ga1 0.0333(3) 0.0301(3) 0.0362(3) -0.0024(3) 0.0099(2) -0.0003(3) Cl1 0.0602(11) 0.0466(9) 0.0767(12) 0.0248(8) 0.0326(9) 0.0151(8) Cl2 0.0428(9) 0.0416(10) 0.0529(9) 0.0042(7) 0.0136(7) -0.0083(7) Cl3 0.0576(10) 0.0405(10) 0.0418(8) -0.0079(7) 0.0148(7) 0.0066(8) Cl4 0.0469(9) 0.0717(11) 0.0427(9) -0.0225(8) 0.0147(7) -0.0176(8) Co1 0.0270(4) 0.0284(4) 0.0261(4) -0.0007(3) 0.0064(3) 0.0007(4) C1 0.029(4) 0.067(5) 0.054(4) 0.014(4) 0.007(3) -0.004(4) C2 0.037(4) 0.029(4) 0.069(5) -0.013(3) -0.003(3) -0.004(3) C3 0.039(4) 0.112(8) 0.028(4) -0.015(4) 0.001(3) -0.010(4) C4 0.054(4) 0.037(5) 0.060(5) 0.020(4) -0.014(4) -0.007(3) C5 0.036(4) 0.056(5) 0.063(4) -0.022(4) 0.004(3) 0.013(3) C11 0.044(4) 0.077(6) 0.022(3) 0.012(3) -0.001(3) 0.011(4) C12 0.038(4) 0.042(5) 0.057(4) 0.016(3) 0.001(3) 0.008(3) C13 0.031(4) 0.051(5) 0.048(4) -0.001(3) 0.011(3) 0.002(3) C14 0.035(4) 0.052(5) 0.045(4) 0.011(3) 0.000(3) -0.010(3) C15 0.039(4) 0.063(6) 0.047(4) -0.021(4) -0.014(3) 0.008(4) C21 0.087(6) 0.047(5) 0.080(6) -0.003(4) 0.040(5) -0.004(4) C22 0.066(5) 0.067(5) 0.044(4) 0.005(4) 0.008(4) 0.025(4) C23 0.053(4) 0.058(5) 0.048(4) -0.017(4) 0.014(3) 0.001(4) C24 0.097(6) 0.045(4) 0.055(5) -0.003(3) 0.042(4) -0.001(4) C25 0.074(6) 0.076(6) 0.042(4) -0.006(4) -0.007(4) 0.033(5) C26 0.051(5) 0.071(6) 0.086(6) -0.050(5) 0.007(5) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ga1 Cl4 2.1679(14) . ? Ga1 Cl3 2.1705(15) . ? Ga1 Cl2 2.1723(15) . ? Ga1 Cl1 2.1751(14) . ? Co1 C4 2.011(5) . ? Co1 C1 2.011(5) . ? Co1 C5 2.012(6) . ? Co1 C2 2.015(5) . ? Co1 C3 2.016(6) . ? Co1 C15 2.019(5) . ? Co1 C14 2.022(6) . ? Co1 C11 2.023(5) . ? Co1 C13 2.030(5) . ? Co1 C12 2.031(5) . ? C1 C5 1.386(8) . ? C1 C2 1.390(8) . ? C1 H1 0.9500 . ? C2 C3 1.391(8) . ? C2 H2 0.9500 . ? C3 C4 1.377(8) . ? C3 H3 0.9500 . ? C4 C5 1.389(9) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C11 C12 1.418(8) . ? C11 C15 1.421(8) . ? C11 H11 0.9500 . ? C12 C13 1.395(7) . ? C12 H12 0.9500 . ? C13 C14 1.397(8) . ? C13 H13 0.9500 . ? C14 C15 1.397(9) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C21 C26 1.334(9) . ? C21 C22 1.366(9) . ? C21 H21 0.9500 . ? C22 C23 1.370(8) . ? C22 H22 0.9500 . ? C23 C24 1.367(8) . ? C23 H23 0.9500 . ? C24 C25 1.384(9) . ? C24 H24 0.9500 . ? C25 C26 1.343(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? 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 Cl4 Ga1 Cl3 109.92(6) . . ? Cl4 Ga1 Cl2 108.97(6) . . ? Cl3 Ga1 Cl2 110.34(5) . . ? Cl4 Ga1 Cl1 109.89(7) . . ? Cl3 Ga1 Cl1 108.48(6) . . ? Cl2 Ga1 Cl1 109.23(6) . . ? C4 Co1 C1 67.7(3) . . ? C4 Co1 C5 40.4(3) . . ? C1 Co1 C5 40.3(2) . . ? C4 Co1 C2 67.4(2) . . ? C1 Co1 C2 40.4(2) . . ? C5 Co1 C2 67.7(2) . . ? C4 Co1 C3 40.0(2) . . ? C1 Co1 C3 68.0(3) . . ? C5 Co1 C3 67.8(3) . . ? C2 Co1 C3 40.4(2) . . ? C4 Co1 C15 117.4(2) . . ? C1 Co1 C15 129.9(3) . . ? C5 Co1 C15 108.6(3) . . ? C2 Co1 C15 168.5(3) . . ? C3 Co1 C15 149.7(3) . . ? C4 Co1 C14 108.3(3) . . ? C1 Co1 C14 167.7(3) . . ? C5 Co1 C14 129.2(2) . . ? C2 Co1 C14 150.3(3) . . ? C3 Co1 C14 117.0(3) . . ? C15 Co1 C14 40.4(2) . . ? C4 Co1 C11 151.3(3) . . ? C1 Co1 C11 109.2(3) . . ? C5 Co1 C11 118.4(3) . . ? C2 Co1 C11 129.9(3) . . ? C3 Co1 C11 167.7(3) . . ? C15 Co1 C11 41.2(2) . . ? C14 Co1 C11 68.3(2) . . ? C4 Co1 C13 128.9(3) . . ? C1 Co1 C13 151.2(2) . . ? C5 Co1 C13 167.1(3) . . ? C2 Co1 C13 118.0(3) . . ? C3 Co1 C13 108.3(3) . . ? C15 Co1 C13 68.1(2) . . ? C14 Co1 C13 40.3(2) . . ? C11 Co1 C13 68.0(2) . . ? C4 Co1 C12 166.5(3) . . ? C1 Co1 C12 118.5(3) . . ? C5 Co1 C12 151.7(3) . . ? C2 Co1 C12 108.8(2) . . ? C3 Co1 C12 128.8(3) . . ? C15 Co1 C12 68.9(2) . . ? C14 Co1 C12 68.2(2) . . ? C11 Co1 C12 40.9(2) . . ? C13 Co1 C12 40.2(2) . . ? C5 C1 C2 107.8(6) . . ? C5 C1 Co1 69.9(3) . . ? C2 C1 Co1 69.9(3) . . ? C5 C1 H1 126.1 . . ? C2 C1 H1 126.1 . . ? Co1 C1 H1 125.7 . . ? C1 C2 C3 108.2(6) . . ? C1 C2 Co1 69.7(3) . . ? C3 C2 Co1 69.9(3) . . ? C1 C2 H2 125.9 . . ? C3 C2 H2 125.9 . . ? Co1 C2 H2 126.2 . . ? C4 C3 C2 107.6(7) . . ? C4 C3 Co1 69.8(3) . . ? C2 C3 Co1 69.8(3) . . ? C4 C3 H3 126.2 . . ? C2 C3 H3 126.2 . . ? Co1 C3 H3 125.8 . . ? C3 C4 C5 108.7(6) . . ? C3 C4 Co1 70.2(4) . . ? C5 C4 Co1 69.8(3) . . ? C3 C4 H4 125.6 . . ? C5 C4 H4 125.6 . . ? Co1 C4 H4 125.9 . . ? C1 C5 C4 107.7(6) . . ? C1 C5 Co1 69.8(3) . . ? C4 C5 Co1 69.8(4) . . ? C1 C5 H5 126.1 . . ? C4 C5 H5 126.1 . . ? Co1 C5 H5 125.9 . . ? C12 C11 C15 107.7(6) . . ? C12 C11 Co1 69.8(3) . . ? C15 C11 Co1 69.3(3) . . ? C12 C11 H11 126.1 . . ? C15 C11 H11 126.1 . . ? Co1 C11 H11 126.3 . . ? C13 C12 C11 107.4(6) . . ? C13 C12 Co1 69.9(3) . . ? C11 C12 Co1 69.2(3) . . ? C13 C12 H12 126.3 . . ? C11 C12 H12 126.3 . . ? Co1 C12 H12 126.2 . . ? C12 C13 C14 108.9(6) . . ? C12 C13 Co1 69.9(3) . . ? C14 C13 Co1 69.5(3) . . ? C12 C13 H13 125.5 . . ? C14 C13 H13 125.5 . . ? Co1 C13 H13 126.6 . . ? C15 C14 C13 108.5(6) . . ? C15 C14 Co1 69.7(3) . . ? C13 C14 Co1 70.1(3) . . ? C15 C14 H14 125.7 . . ? C13 C14 H14 125.7 . . ? Co1 C14 H14 126.0 . . ? C14 C15 C11 107.5(6) . . ? C14 C15 Co1 69.9(3) . . ? C11 C15 Co1 69.6(3) . . ? C14 C15 H15 126.3 . . ? C11 C15 H15 126.3 . . ? Co1 C15 H15 125.9 . . ? C26 C21 C22 120.6(7) . . ? C26 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C21 C22 C23 120.0(6) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C24 C23 C22 119.6(6) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 118.4(7) . . ? C23 C24 H24 120.8 . . ? C25 C24 H24 120.8 . . ? C26 C25 C24 121.3(7) . . ? C26 C25 H25 119.3 . . ? C24 C25 H25 119.3 . . ? C21 C26 C25 120.0(7) . . ? C21 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Co1 C1 C5 -37.9(4) . . . . ? C2 Co1 C1 C5 -118.7(6) . . . . ? C3 Co1 C1 C5 -81.2(4) . . . . ? C15 Co1 C1 C5 70.0(5) . . . . ? C14 Co1 C1 C5 35.4(12) . . . . ? C11 Co1 C1 C5 111.6(4) . . . . ? C13 Co1 C1 C5 -169.4(5) . . . . ? C12 Co1 C1 C5 155.4(4) . . . . ? C4 Co1 C1 C2 80.8(4) . . . . ? C5 Co1 C1 C2 118.7(6) . . . . ? C3 Co1 C1 C2 37.5(4) . . . . ? C15 Co1 C1 C2 -171.3(4) . . . . ? C14 Co1 C1 C2 154.1(10) . . . . ? C11 Co1 C1 C2 -129.7(4) . . . . ? C13 Co1 C1 C2 -50.7(7) . . . . ? C12 Co1 C1 C2 -85.9(4) . . . . ? C5 C1 C2 C3 0.4(7) . . . . ? Co1 C1 C2 C3 -59.4(4) . . . . ? C5 C1 C2 Co1 59.9(4) . . . . ? C4 Co1 C2 C1 -81.7(4) . . . . ? C5 Co1 C2 C1 -37.8(4) . . . . ? C3 Co1 C2 C1 -119.4(6) . . . . ? C15 Co1 C2 C1 35.5(14) . . . . ? C14 Co1 C2 C1 -169.2(4) . . . . ? C11 Co1 C2 C1 71.2(5) . . . . ? C13 Co1 C2 C1 155.0(3) . . . . ? C12 Co1 C2 C1 112.1(4) . . . . ? C4 Co1 C2 C3 37.7(4) . . . . ? C1 Co1 C2 C3 119.4(6) . . . . ? C5 Co1 C2 C3 81.5(4) . . . . ? C15 Co1 C2 C3 154.9(12) . . . . ? C14 Co1 C2 C3 -49.8(6) . . . . ? C11 Co1 C2 C3 -169.4(4) . . . . ? C13 Co1 C2 C3 -85.6(4) . . . . ? C12 Co1 C2 C3 -128.5(4) . . . . ? C1 C2 C3 C4 -0.5(7) . . . . ? Co1 C2 C3 C4 -59.8(4) . . . . ? C1 C2 C3 Co1 59.3(4) . . . . ? C1 Co1 C3 C4 81.1(5) . . . . ? C5 Co1 C3 C4 37.4(4) . . . . ? C2 Co1 C3 C4 118.6(6) . . . . ? C15 Co1 C3 C4 -51.7(6) . . . . ? C14 Co1 C3 C4 -86.5(5) . . . . ? C11 Co1 C3 C4 160.2(13) . . . . ? C13 Co1 C3 C4 -129.4(4) . . . . ? C12 Co1 C3 C4 -169.3(4) . . . . ? C4 Co1 C3 C2 -118.6(6) . . . . ? C1 Co1 C3 C2 -37.5(4) . . . . ? C5 Co1 C3 C2 -81.2(4) . . . . ? C15 Co1 C3 C2 -170.3(5) . . . . ? C14 Co1 C3 C2 154.9(4) . . . . ? C11 Co1 C3 C2 41.6(17) . . . . ? C13 Co1 C3 C2 112.0(4) . . . . ? C12 Co1 C3 C2 72.0(5) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? Co1 C3 C4 C5 -59.4(4) . . . . ? C2 C3 C4 Co1 59.8(4) . . . . ? C1 Co1 C4 C3 -81.9(4) . . . . ? C5 Co1 C4 C3 -119.7(6) . . . . ? C2 Co1 C4 C3 -38.0(4) . . . . ? C15 Co1 C4 C3 153.5(4) . . . . ? C14 Co1 C4 C3 110.6(4) . . . . ? C11 Co1 C4 C3 -171.4(6) . . . . ? C13 Co1 C4 C3 70.5(5) . . . . ? C12 Co1 C4 C3 38.1(13) . . . . ? C1 Co1 C4 C5 37.8(4) . . . . ? C2 Co1 C4 C5 81.7(4) . . . . ? C3 Co1 C4 C5 119.7(6) . . . . ? C15 Co1 C4 C5 -86.8(5) . . . . ? C14 Co1 C4 C5 -129.8(4) . . . . ? C11 Co1 C4 C5 -51.7(7) . . . . ? C13 Co1 C4 C5 -169.8(3) . . . . ? C12 Co1 C4 C5 157.8(10) . . . . ? C2 C1 C5 C4 -0.2(6) . . . . ? Co1 C1 C5 C4 59.7(4) . . . . ? C2 C1 C5 Co1 -59.9(4) . . . . ? C3 C4 C5 C1 -0.1(7) . . . . ? Co1 C4 C5 C1 -59.7(4) . . . . ? C3 C4 C5 Co1 59.7(4) . . . . ? C4 Co1 C5 C1 118.8(6) . . . . ? C2 Co1 C5 C1 37.9(4) . . . . ? C3 Co1 C5 C1 81.7(4) . . . . ? C15 Co1 C5 C1 -130.4(4) . . . . ? C14 Co1 C5 C1 -170.8(4) . . . . ? C11 Co1 C5 C1 -86.6(4) . . . . ? C13 Co1 C5 C1 156.6(10) . . . . ? C12 Co1 C5 C1 -50.5(7) . . . . ? C1 Co1 C5 C4 -118.8(6) . . . . ? C2 Co1 C5 C4 -80.9(4) . . . . ? C3 Co1 C5 C4 -37.1(4) . . . . ? C15 Co1 C5 C4 110.8(4) . . . . ? C14 Co1 C5 C4 70.4(5) . . . . ? C11 Co1 C5 C4 154.7(4) . . . . ? C13 Co1 C5 C4 37.8(12) . . . . ? C12 Co1 C5 C4 -169.3(5) . . . . ? C4 Co1 C11 C12 -169.9(5) . . . . ? C1 Co1 C11 C12 111.7(4) . . . . ? C5 Co1 C11 C12 154.8(4) . . . . ? C2 Co1 C11 C12 71.1(4) . . . . ? C3 Co1 C11 C12 37.1(17) . . . . ? C15 Co1 C11 C12 -119.0(6) . . . . ? C14 Co1 C11 C12 -81.2(4) . . . . ? C13 Co1 C11 C12 -37.6(4) . . . . ? C4 Co1 C11 C15 -50.9(6) . . . . ? C1 Co1 C11 C15 -129.3(4) . . . . ? C5 Co1 C11 C15 -86.2(5) . . . . ? C2 Co1 C11 C15 -169.8(4) . . . . ? C3 Co1 C11 C15 156.1(13) . . . . ? C14 Co1 C11 C15 37.8(4) . . . . ? C13 Co1 C11 C15 81.4(4) . . . . ? C12 Co1 C11 C15 119.0(6) . . . . ? C15 C11 C12 C13 0.5(6) . . . . ? Co1 C11 C12 C13 59.7(4) . . . . ? C15 C11 C12 Co1 -59.1(4) . . . . ? C4 Co1 C12 C13 40.2(13) . . . . ? C1 Co1 C12 C13 154.5(4) . . . . ? C5 Co1 C12 C13 -170.9(4) . . . . ? C2 Co1 C12 C13 111.4(4) . . . . ? C3 Co1 C12 C13 70.8(5) . . . . ? C15 Co1 C12 C13 -80.6(4) . . . . ? C14 Co1 C12 C13 -37.0(3) . . . . ? C11 Co1 C12 C13 -118.7(5) . . . . ? C4 Co1 C12 C11 158.9(10) . . . . ? C1 Co1 C12 C11 -86.9(4) . . . . ? C5 Co1 C12 C11 -52.2(7) . . . . ? C2 Co1 C12 C11 -129.9(4) . . . . ? C3 Co1 C12 C11 -170.5(4) . . . . ? C15 Co1 C12 C11 38.1(4) . . . . ? C14 Co1 C12 C11 81.7(4) . . . . ? C13 Co1 C12 C11 118.7(5) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? Co1 C12 C13 C14 58.8(4) . . . . ? C11 C12 C13 Co1 -59.3(4) . . . . ? C4 Co1 C13 C12 -168.8(4) . . . . ? C1 Co1 C13 C12 -51.8(7) . . . . ? C5 Co1 C13 C12 160.5(10) . . . . ? C2 Co1 C13 C12 -86.3(4) . . . . ? C3 Co1 C13 C12 -129.2(4) . . . . ? C15 Co1 C13 C12 82.9(4) . . . . ? C14 Co1 C13 C12 120.3(5) . . . . ? C11 Co1 C13 C12 38.3(4) . . . . ? C4 Co1 C13 C14 70.9(4) . . . . ? C1 Co1 C13 C14 -172.0(5) . . . . ? C5 Co1 C13 C14 40.2(12) . . . . ? C2 Co1 C13 C14 153.4(4) . . . . ? C3 Co1 C13 C14 110.5(4) . . . . ? C15 Co1 C13 C14 -37.4(4) . . . . ? C11 Co1 C13 C14 -82.0(4) . . . . ? C12 Co1 C13 C14 -120.3(5) . . . . ? C12 C13 C14 C15 0.3(6) . . . . ? Co1 C13 C14 C15 59.3(4) . . . . ? C12 C13 C14 Co1 -59.0(4) . . . . ? C4 Co1 C14 C15 111.2(4) . . . . ? C1 Co1 C14 C15 42.2(12) . . . . ? C5 Co1 C14 C15 71.2(5) . . . . ? C2 Co1 C14 C15 -172.6(5) . . . . ? C3 Co1 C14 C15 153.7(4) . . . . ? C11 Co1 C14 C15 -38.5(4) . . . . ? C13 Co1 C14 C15 -119.6(5) . . . . ? C12 Co1 C14 C15 -82.7(4) . . . . ? C4 Co1 C14 C13 -129.2(4) . . . . ? C1 Co1 C14 C13 161.8(10) . . . . ? C5 Co1 C14 C13 -169.3(4) . . . . ? C2 Co1 C14 C13 -53.0(6) . . . . ? C3 Co1 C14 C13 -86.8(4) . . . . ? C15 Co1 C14 C13 119.6(5) . . . . ? C11 Co1 C14 C13 81.1(4) . . . . ? C12 Co1 C14 C13 36.9(3) . . . . ? C13 C14 C15 C11 0.1(6) . . . . ? Co1 C14 C15 C11 59.7(4) . . . . ? C13 C14 C15 Co1 -59.6(4) . . . . ? C12 C11 C15 C14 -0.4(6) . . . . ? Co1 C11 C15 C14 -59.9(4) . . . . ? C12 C11 C15 Co1 59.5(4) . . . . ? C4 Co1 C15 C14 -86.3(5) . . . . ? C1 Co1 C15 C14 -169.2(3) . . . . ? C5 Co1 C15 C14 -129.3(4) . . . . ? C2 Co1 C15 C14 161.4(12) . . . . ? C3 Co1 C15 C14 -51.6(6) . . . . ? C11 Co1 C15 C14 118.5(5) . . . . ? C13 Co1 C15 C14 37.3(4) . . . . ? C12 Co1 C15 C14 80.7(4) . . . . ? C4 Co1 C15 C11 155.2(4) . . . . ? C1 Co1 C15 C11 72.2(5) . . . . ? C5 Co1 C15 C11 112.1(4) . . . . ? C2 Co1 C15 C11 42.8(14) . . . . ? C3 Co1 C15 C11 -170.2(5) . . . . ? C14 Co1 C15 C11 -118.5(5) . . . . ? C13 Co1 C15 C11 -81.2(4) . . . . ? C12 Co1 C15 C11 -37.9(4) . . . . ? C26 C21 C22 C23 -0.1(10) . . . . ? C21 C22 C23 C24 0.9(9) . . . . ? C22 C23 C24 C25 -1.4(9) . . . . ? C23 C24 C25 C26 1.1(10) . . . . ? C22 C21 C26 C25 -0.2(10) . . . . ? C24 C25 C26 C21 -0.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.346 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.082