data_all _publ_contact_author_name 'Dr. Andrew L. Johnson' _publ_contact_author_address ; Department of Chemistry, University of Bath. Claverton Down. Bath. BA2 7AY United Kingdon ; _publ_contact_author_email a.l.johnson@bath.ac.uk _publ_contact_author_phone '+44 (0) 1225 384467' _publ_contact_author_fax '+44 (0) 1225 386231' _publ_requested_journal 'Inorganic Chemistry' _publ_section_title ; Cobalt(I) olefin Complexes: Precursors for Metal-Organic Chemical Vapor Deposition of High Purity Cobalt Metal Thin Films ; loop_ _publ_author_name _publ_author_address 'Hamilton, J.A. ' ; Department of Chemistry, University of Bath. Claverton Down. Bath. BA2 7AY United Kingdon ; 'Pugh, T.' ; Department of Chemistry, University of Bath. Claverton Down. Bath. BA2 7AY United Kingdon ; 'Johnson, A. L.' ; Department of Chemistry, University of Bath. Claverton Down. Bath. BA2 7AY United Kingdon ; 'Kingsley, A.J.' ; SAFC-Hitech, Power Road, Bromborough, Wirral, CH62 3QF, United Kingdom ; 'Richards, S.P.' ; SAFC-Hitech, Power Road, Bromborough, Wirral, CH62 3QF, United Kingdom ; data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H15 Co' _chemical_formula_weight 206.16 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3760(3) _cell_length_b 7.5360(2) _cell_length_c 11.3800(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.335(2) _cell_angle_gamma 90.00 _cell_volume 956.57(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 19548 _cell_measurement_theta_min 8.18 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 432 _exptl_absorpt_coefficient_mu 1.734 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7810 _exptl_absorpt_correction_T_max 0.8810 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19548 _diffrn_reflns_av_R_equivalents 0.0754 _diffrn_reflns_av_sigmaI/netI 0.0461 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 8.18 _diffrn_reflns_theta_max 27.88 _reflns_number_total 2211 _reflns_number_gt 1704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0241P)^2^+0.1006P] 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 2211 _refine_ls_number_parameters 127 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0519 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Co1 Co 0.21871(2) 0.83791(3) 0.180596(19) 0.01727(9) Uani 1 1 d . . . C5 C 0.19027(18) 0.5725(2) 0.20886(19) 0.0329(5) Uani 1 1 d . . . H5 H 0.2510 0.4842 0.2202 0.040 Uiso 1 1 calc R . . C13 C 0.30024(15) 1.0587(2) 0.24798(15) 0.0191(4) Uani 1 1 d . . . C12 C 0.38543(15) 0.9217(2) 0.23751(15) 0.0195(4) Uani 1 1 d . . . C14 C 0.21681(19) 1.0993(3) 0.14018(18) 0.0254(4) Uani 1 1 d . . . C1 C 0.15268(16) 0.6714(2) 0.29995(16) 0.0253(4) Uani 1 1 d . . . H1 H 0.1821 0.6594 0.3837 0.030 Uiso 1 1 calc R . . C4 C 0.1214(2) 0.6283(3) 0.09718(19) 0.0384(5) Uani 1 1 d . . . H4 H 0.1270 0.5824 0.0207 0.046 Uiso 1 1 calc R . . C3 C 0.04409(17) 0.7623(3) 0.11928(19) 0.0367(5) Uani 1 1 d . . . H3 H -0.0121 0.8237 0.0605 0.044 Uiso 1 1 calc R . . C11 C 0.37453(17) 0.8465(3) 0.12025(17) 0.0267(4) Uani 1 1 d . . . C16 C 0.28940(18) 1.1395(3) 0.36567(18) 0.0286(4) Uani 1 1 d . . . H16A H 0.3049 1.0487 0.4284 0.043 Uiso 1 1 calc R . . H16B H 0.2083 1.1870 0.3602 0.043 Uiso 1 1 calc R . . H16C H 0.3480 1.2357 0.3854 0.043 Uiso 1 1 calc R . . C15 C 0.47172(16) 0.8471(3) 0.34291(17) 0.0286(4) Uani 1 1 d . . . H15A H 0.5485 0.9096 0.3520 0.043 Uiso 1 1 calc R . . H15B H 0.4840 0.7205 0.3298 0.043 Uiso 1 1 calc R . . H15C H 0.4389 0.8625 0.4157 0.043 Uiso 1 1 calc R . . C2 C 0.06407(16) 0.7908(3) 0.24515(18) 0.0279(4) Uani 1 1 d . . . H2 H 0.0244 0.8759 0.2851 0.033 Uiso 1 1 calc R . . H11A H 0.3633(18) 0.924(3) 0.0483(19) 0.035(5) Uiso 1 1 d . . . H11B H 0.4172(18) 0.735(3) 0.1178(17) 0.030(5) Uiso 1 1 d . . . H14A H 0.2446(18) 1.115(3) 0.0688(19) 0.028(5) Uiso 1 1 d . . . H14B H 0.145(2) 1.170(3) 0.1480(18) 0.032(5) 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 Co1 0.01763(14) 0.01620(13) 0.01774(13) -0.00120(10) 0.00287(9) -0.00266(10) C5 0.0350(12) 0.0141(9) 0.0534(14) 0.0001(9) 0.0177(10) -0.0065(8) C13 0.0185(9) 0.0157(8) 0.0224(9) -0.0003(7) 0.0024(7) -0.0043(7) C12 0.0162(9) 0.0199(9) 0.0232(9) -0.0007(7) 0.0052(7) -0.0048(7) C14 0.0293(11) 0.0199(9) 0.0253(10) 0.0026(8) 0.0010(9) -0.0022(8) C1 0.0271(10) 0.0254(9) 0.0235(9) 0.0041(8) 0.0050(8) -0.0084(8) C4 0.0504(14) 0.0371(12) 0.0295(11) -0.0171(9) 0.0117(10) -0.0270(10) C3 0.0223(10) 0.0446(13) 0.0374(12) 0.0118(10) -0.0083(9) -0.0152(10) C11 0.0261(10) 0.0293(10) 0.0270(10) -0.0036(9) 0.0109(8) -0.0033(9) C16 0.0254(10) 0.0292(11) 0.0301(10) -0.0106(8) 0.0031(8) 0.0021(8) C15 0.0213(10) 0.0314(10) 0.0312(11) -0.0010(8) 0.0007(8) 0.0010(8) C2 0.0187(9) 0.0293(10) 0.0378(12) 0.0009(8) 0.0109(8) -0.0032(8) _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 Co1 C12 1.9832(17) . ? Co1 C13 1.9843(17) . ? Co1 C14 2.0217(19) . ? Co1 C11 2.0240(18) . ? Co1 C4 2.0513(19) . ? Co1 C3 2.0525(19) . ? Co1 C5 2.0611(18) . ? Co1 C2 2.0659(18) . ? Co1 C1 2.0938(17) . ? C5 C1 1.410(3) . ? C5 C4 1.419(3) . ? C5 H5 0.9500 . ? C13 C14 1.429(3) . ? C13 C12 1.437(2) . ? C13 C16 1.498(3) . ? C12 C11 1.432(3) . ? C12 C15 1.502(3) . ? C14 H14A 0.94(2) . ? C14 H14B 0.99(2) . ? C1 C2 1.403(3) . ? C1 H1 0.9500 . ? C4 C3 1.394(3) . ? C4 H4 0.9500 . ? C3 C2 1.422(3) . ? C3 H3 0.9500 . ? C11 H11A 0.99(2) . ? C11 H11B 0.97(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C2 H2 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 C12 Co1 C13 42.47(7) . . ? C12 Co1 C14 74.38(8) . . ? C13 Co1 C14 41.78(7) . . ? C12 Co1 C11 41.88(7) . . ? C13 Co1 C11 74.35(7) . . ? C14 Co1 C11 82.09(9) . . ? C12 Co1 C4 142.26(9) . . ? C13 Co1 C4 173.32(8) . . ? C14 Co1 C4 131.62(9) . . ? C11 Co1 C4 107.26(8) . . ? C12 Co1 C3 177.49(8) . . ? C13 Co1 C3 135.39(8) . . ? C14 Co1 C3 103.11(9) . . ? C11 Co1 C3 138.35(8) . . ? C4 Co1 C3 39.71(9) . . ? C12 Co1 C5 115.31(8) . . ? C13 Co1 C5 146.01(8) . . ? C14 Co1 C5 170.31(8) . . ? C11 Co1 C5 105.00(9) . . ? C4 Co1 C5 40.38(9) . . ? C3 Co1 C5 67.20(9) . . ? C12 Co1 C2 139.92(7) . . ? C13 Co1 C2 111.87(7) . . ? C14 Co1 C2 106.04(8) . . ? C11 Co1 C2 171.86(8) . . ? C4 Co1 C2 67.21(8) . . ? C3 Co1 C2 40.39(8) . . ? C5 Co1 C2 66.87(8) . . ? C12 Co1 C1 114.90(7) . . ? C13 Co1 C1 116.86(7) . . ? C14 Co1 C1 137.91(8) . . ? C11 Co1 C1 133.56(9) . . ? C4 Co1 C1 66.99(8) . . ? C3 Co1 C1 66.89(8) . . ? C5 Co1 C1 39.66(8) . . ? C2 Co1 C1 39.41(7) . . ? C1 C5 C4 107.94(18) . . ? C1 C5 Co1 71.42(10) . . ? C4 C5 Co1 69.44(11) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Co1 C5 H5 124.7 . . ? C14 C13 C12 115.31(16) . . ? C14 C13 C16 121.55(16) . . ? C12 C13 C16 122.78(16) . . ? C14 C13 Co1 70.51(10) . . ? C12 C13 Co1 68.73(9) . . ? C16 C13 Co1 124.88(12) . . ? C11 C12 C13 115.16(16) . . ? C11 C12 C15 121.28(17) . . ? C13 C12 C15 123.25(15) . . ? C11 C12 Co1 70.59(10) . . ? C13 C12 Co1 68.81(9) . . ? C15 C12 Co1 125.07(12) . . ? C13 C14 Co1 67.71(10) . . ? C13 C14 H14A 119.5(13) . . ? Co1 C14 H14A 109.4(12) . . ? C13 C14 H14B 117.1(12) . . ? Co1 C14 H14B 118.3(12) . . ? H14A C14 H14B 115.7(17) . . ? C2 C1 C5 107.91(17) . . ? C2 C1 Co1 69.22(10) . . ? C5 C1 Co1 68.92(10) . . ? C2 C1 H1 126.0 . . ? C5 C1 H1 126.0 . . ? Co1 C1 H1 127.4 . . ? C3 C4 C5 108.05(18) . . ? C3 C4 Co1 70.19(11) . . ? C5 C4 Co1 70.18(11) . . ? C3 C4 H4 126.0 . . ? C5 C4 H4 126.0 . . ? Co1 C4 H4 125.2 . . ? C4 C3 C2 108.05(18) . . ? C4 C3 Co1 70.10(12) . . ? C2 C3 Co1 70.31(10) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Co1 C3 H3 125.2 . . ? C12 C11 Co1 67.54(10) . . ? C12 C11 H11A 120.6(12) . . ? Co1 C11 H11A 108.6(12) . . ? C12 C11 H11B 114.5(11) . . ? Co1 C11 H11B 117.3(12) . . ? H11A C11 H11B 117.9(17) . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C1 C2 C3 108.02(17) . . ? C1 C2 Co1 71.37(10) . . ? C3 C2 Co1 69.30(11) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Co1 C2 H2 124.9 . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.273 _refine_diff_density_min -0.283 _refine_diff_density_rms 0.063 #===END data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H26 Co2' _chemical_formula_weight 432.31 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.65600(10) _cell_length_b 5.8840(3) _cell_length_c 24.1690(4) _cell_angle_alpha 90.0000(10) _cell_angle_beta 131.6510(10) _cell_angle_gamma 90.0000(10) _cell_volume 3682.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30759 _cell_measurement_theta_min 8.52 _cell_measurement_theta_max 30.52 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.806 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7429 _exptl_absorpt_correction_T_max 0.8058 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30759 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -49 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 8.52 _diffrn_reflns_theta_max 30.52 _reflns_number_total 5499 _reflns_number_gt 4368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0319P)^2^+2.3393P] 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 SHELXL _refine_ls_extinction_coef 0.0021(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5499 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0434 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0645 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 Co1 Co 0.153895(7) 0.47631(3) 0.204764(10) 0.01889(7) Uani 1 1 d . . . Co2 Co 0.061822(7) 0.98939(3) 0.398740(10) 0.01898(7) Uani 1 1 d . . . C1 C 0.11539(7) 0.3861(3) 0.09588(8) 0.0321(3) Uani 1 1 d . . . H1 H 0.1105 0.2359 0.0778 0.038 Uiso 1 1 calc R . . C2 C 0.15731(7) 0.5317(3) 0.12360(9) 0.0273(3) Uani 1 1 d . . . H2 H 0.1862 0.4944 0.1287 0.033 Uiso 1 1 calc R . . C3 C 0.14889(6) 0.7431(3) 0.14253(8) 0.0263(3) Uani 1 1 d . . . H3 H 0.1708 0.8722 0.1615 0.032 Uiso 1 1 calc R . . C4 C 0.10266(6) 0.7282(3) 0.12839(9) 0.0307(3) Uani 1 1 d . . . H4 H 0.0877 0.8447 0.1362 0.037 Uiso 1 1 calc R . . C5 C 0.08207(7) 0.5061(3) 0.10018(9) 0.0340(4) Uani 1 1 d . . . H5 H 0.0512 0.4484 0.0866 0.041 Uiso 1 1 calc R . . C11 C 0.22424(6) 0.5042(3) 0.30576(8) 0.0243(3) Uani 1 1 d . . . C12 C 0.21544(6) 0.2809(3) 0.27848(9) 0.0284(3) Uani 1 1 d . . . C13 C 0.19235(7) 0.1515(3) 0.30554(9) 0.0327(3) Uani 1 1 d . . . H13 H 0.1929 -0.0183 0.3045 0.039 Uiso 1 1 calc R . . C14 C 0.13970(6) 0.2680(3) 0.25546(9) 0.0290(3) Uani 1 1 d . . . C15 C 0.14837(6) 0.4909(3) 0.28254(9) 0.0275(3) Uani 1 1 d . . . C16 C 0.20643(6) 0.5087(2) 0.34910(8) 0.0246(3) Uani 1 1 d . . . H16 H 0.2186 0.6377 0.3843 0.030 Uiso 1 1 calc R . . C17 C 0.21942(7) 0.2670(3) 0.38071(9) 0.0317(3) Uani 1 1 d . . . H17A H 0.2034 0.2281 0.4015 0.038 Uiso 1 1 calc R . . H17B H 0.2570 0.2370 0.4176 0.038 Uiso 1 1 calc R . . C21A C 0.01480(12) 0.9824(10) 0.4246(2) 0.0391(8) Uani 0.857(11) 1 d P A -1 H21A H 0.0216 0.9035 0.4646 0.047 Uiso 0.857(11) 1 calc PR A -1 C22A C -0.01094(19) 0.8954(8) 0.3519(3) 0.0517(16) Uani 0.857(11) 1 d P A -1 H22A H -0.0229 0.7437 0.3364 0.062 Uiso 0.857(11) 1 calc PR A -1 C23A C -0.01585(10) 1.0629(8) 0.30773(15) 0.0319(7) Uani 0.857(11) 1 d P A -1 H23A H -0.0326 1.0501 0.2569 0.038 Uiso 0.857(11) 1 calc PR A -1 C24A C 0.00896(10) 1.2567(4) 0.3529(3) 0.0309(7) Uani 0.857(11) 1 d P A -1 H24A H 0.0126 1.3983 0.3378 0.037 Uiso 0.857(11) 1 calc PR A -1 C25A C 0.02766(8) 1.2065(9) 0.42433(18) 0.0338(8) Uani 0.857(11) 1 d P A -1 H25A H 0.0459 1.3083 0.4652 0.041 Uiso 0.857(11) 1 calc PR A -1 C21B C 0.0100(6) 0.904(3) 0.4106(10) 0.021(3) Uiso 0.143(11) 1 d P A -2 H21B H 0.0166 0.7861 0.4428 0.025 Uiso 0.143(11) 1 calc PR A -2 C22B C -0.0148(9) 0.873(4) 0.3439(10) 0.012(4) Uiso 0.143(11) 1 d P A -2 H22B H -0.0323 0.7397 0.3151 0.014 Uiso 0.143(11) 1 calc PR A -2 C23B C -0.0095(7) 1.123(3) 0.3176(10) 0.016(3) Uiso 0.143(11) 1 d P A -2 H23B H -0.0209 1.1664 0.2709 0.019 Uiso 0.143(11) 1 calc PR A -2 C24B C 0.0144(5) 1.243(2) 0.3776(11) 0.017(3) Uiso 0.143(11) 1 d P A -2 H24B H 0.0222 1.4006 0.3816 0.021 Uiso 0.143(11) 1 calc PR A -2 C25B C 0.0265(5) 1.114(4) 0.4334(7) 0.019(3) Uiso 0.143(11) 1 d P A -2 H25B H 0.0445 1.1665 0.4823 0.022 Uiso 0.143(11) 1 calc PR A -2 C31 C 0.10631(6) 0.7108(2) 0.44137(8) 0.0243(3) Uani 1 1 d . A . C32 C 0.08765(6) 0.7553(2) 0.36981(8) 0.0231(3) Uani 1 1 d . A . C33 C 0.12852(5) 0.9053(2) 0.38086(8) 0.0226(3) Uani 1 1 d . . . H33 H 0.1275 0.9181 0.3386 0.027 Uiso 1 1 calc R A . C34 C 0.11835(5) 1.1212(2) 0.40486(8) 0.0230(3) Uani 1 1 d . A . C35 C 0.13677(6) 1.0774(3) 0.47591(9) 0.0258(3) Uani 1 1 d . A . C36 C 0.15823(6) 0.8348(3) 0.49513(8) 0.0257(3) Uani 1 1 d . . . H36 H 0.1820 0.7888 0.5484 0.031 Uiso 1 1 calc R A . C37 C 0.17858(6) 0.8159(3) 0.45495(8) 0.0260(3) Uani 1 1 d . A . H37A H 0.1866 0.6575 0.4517 0.031 Uiso 1 1 calc R . . H37B H 0.2087 0.9156 0.4765 0.031 Uiso 1 1 calc R . . H11 H 0.2463(8) 0.615(4) 0.3101(10) 0.036(5) Uiso 1 1 d . . . H31 H 0.0957(7) 0.592(3) 0.4568(10) 0.030(4) Uiso 1 1 d . . . H35 H 0.1438(8) 1.201(4) 0.5124(12) 0.045(5) Uiso 1 1 d . . . H32 H 0.0614(7) 0.677(3) 0.3254(11) 0.033(5) Uiso 1 1 d . . . H34 H 0.1109(8) 1.270(4) 0.3829(11) 0.040(5) Uiso 1 1 d . . . H15 H 0.1216(8) 0.597(4) 0.2709(11) 0.041(5) Uiso 1 1 d . . . H14 H 0.1068(8) 0.193(3) 0.2231(11) 0.037(5) Uiso 1 1 d . . . H12 H 0.2318(7) 0.209(3) 0.2609(10) 0.036(5) 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 Co1 0.01944(10) 0.02090(10) 0.01831(10) -0.00104(6) 0.01338(9) -0.00151(6) Co2 0.01674(10) 0.01958(10) 0.02119(11) -0.00180(6) 0.01285(9) -0.00055(6) C1 0.0400(9) 0.0285(8) 0.0204(7) -0.0030(6) 0.0170(7) -0.0052(6) C2 0.0333(8) 0.0320(8) 0.0229(7) 0.0016(6) 0.0213(7) 0.0024(6) C3 0.0303(8) 0.0250(7) 0.0239(7) 0.0018(5) 0.0182(6) -0.0016(6) C4 0.0311(8) 0.0319(8) 0.0303(8) 0.0089(6) 0.0210(7) 0.0091(6) C5 0.0224(7) 0.0460(10) 0.0225(8) 0.0062(6) 0.0102(6) -0.0055(6) C11 0.0191(6) 0.0337(8) 0.0197(7) 0.0002(5) 0.0127(6) -0.0045(5) C12 0.0256(7) 0.0351(8) 0.0240(8) 0.0021(6) 0.0163(7) 0.0082(6) C13 0.0412(9) 0.0232(7) 0.0297(8) 0.0024(6) 0.0219(8) -0.0015(6) C14 0.0286(8) 0.0334(8) 0.0261(8) 0.0000(6) 0.0187(7) -0.0100(6) C15 0.0271(7) 0.0381(8) 0.0255(7) 0.0015(6) 0.0210(7) 0.0023(6) C16 0.0275(7) 0.0288(7) 0.0207(7) -0.0025(5) 0.0174(6) -0.0036(5) C17 0.0331(8) 0.0349(8) 0.0259(8) 0.0047(6) 0.0191(7) -0.0026(6) C21A 0.0315(12) 0.054(2) 0.0458(16) 0.0163(16) 0.0314(12) 0.0116(14) C22A 0.0263(15) 0.0267(16) 0.097(4) -0.0181(16) 0.039(2) -0.0093(11) C23A 0.0159(10) 0.0425(17) 0.0264(12) -0.0101(11) 0.0095(9) 0.0010(10) C24A 0.0306(12) 0.0259(11) 0.0438(19) 0.0081(10) 0.0280(13) 0.0091(8) C25A 0.0250(10) 0.041(2) 0.0372(14) -0.0150(12) 0.0213(10) -0.0012(9) C31 0.0253(7) 0.0212(7) 0.0287(8) 0.0046(5) 0.0190(6) 0.0030(5) C32 0.0245(7) 0.0202(6) 0.0245(7) -0.0040(5) 0.0163(6) -0.0007(5) C33 0.0238(7) 0.0251(7) 0.0230(7) 0.0002(5) 0.0172(6) 0.0016(5) C34 0.0215(7) 0.0196(7) 0.0300(8) -0.0004(5) 0.0180(6) -0.0013(5) C35 0.0201(7) 0.0309(7) 0.0271(8) -0.0084(6) 0.0160(6) -0.0050(6) C36 0.0209(7) 0.0351(8) 0.0200(7) 0.0050(6) 0.0131(6) 0.0033(6) C37 0.0229(7) 0.0297(7) 0.0279(8) 0.0046(6) 0.0179(6) 0.0051(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C12 1.9986(15) . ? Co1 C11 2.0047(15) . ? Co1 C14 2.0118(15) . ? Co1 C15 2.0141(15) . ? Co1 C5 2.0622(16) . ? Co1 C2 2.0680(15) . ? Co1 C1 2.0785(15) . ? Co1 C4 2.0975(15) . ? Co1 C3 2.0998(15) . ? Co2 C31 2.0034(14) . ? Co2 C32 2.0047(14) . ? Co2 C35 2.0136(14) . ? Co2 C34 2.0190(14) . ? Co2 C24B 2.020(13) . ? Co2 C25B 2.023(13) . ? Co2 C23B 2.032(16) . ? Co2 C22A 2.038(5) . ? Co2 C21B 2.060(16) . ? Co2 C24A 2.088(2) . ? Co2 C25A 2.095(2) . ? Co2 C23A 2.098(2) . ? C1 C2 1.414(2) . ? C1 C5 1.415(3) . ? C1 H1 0.9500 . ? C2 C3 1.421(2) . ? C2 H2 0.9500 . ? C3 C4 1.402(2) . ? C3 H3 0.9500 . ? C4 C5 1.427(2) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C11 C12 1.410(2) . ? C11 C16 1.529(2) . ? C11 H11 0.95(2) . ? C12 C13 1.531(2) . ? C12 H12 1.00(2) . ? C13 C14 1.526(2) . ? C13 C17 1.542(2) . ? C13 H13 1.0000 . ? C14 C15 1.406(2) . ? C14 H14 0.96(2) . ? C15 C16 1.531(2) . ? C15 H15 0.99(2) . ? C16 C17 1.534(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C21A C25A 1.393(4) . ? C21A C22A 1.436(6) . ? C21A H21A 0.9500 . ? C22A C23A 1.378(6) . ? C22A H22A 0.9500 . ? C23A C24A 1.408(4) . ? C23A H23A 0.9500 . ? C24A C25A 1.415(4) . ? C24A H24A 0.9500 . ? C25A H25A 0.9500 . ? C21B C22B 1.24(3) . ? C21B C25B 1.318(19) . ? C21B H21B 0.9500 . ? C22B C23B 1.66(3) . ? C22B H22B 0.9500 . ? C23B C24B 1.30(2) . ? C23B H23B 0.9500 . ? C24B C25B 1.349(19) . ? C24B H24B 0.9500 . ? C25B H25B 0.9500 . ? C31 C32 1.411(2) . ? C31 C36 1.533(2) . ? C31 H31 0.97(2) . ? C32 C33 1.534(2) . ? C32 H32 0.947(19) . ? C33 C34 1.532(2) . ? C33 C37 1.537(2) . ? C33 H33 1.0000 . ? C34 C35 1.402(2) . ? C34 H34 0.97(2) . ? C35 C36 1.532(2) . ? C35 H35 1.04(2) . ? C36 C37 1.537(2) . ? C36 H36 1.0000 . ? C37 H37A 0.9900 . ? C37 H37B 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 C12 Co1 C11 41.23(6) . . ? C12 Co1 C14 69.80(7) . . ? C11 Co1 C14 84.26(6) . . ? C12 Co1 C15 84.24(6) . . ? C11 Co1 C15 69.70(6) . . ? C14 Co1 C15 40.90(7) . . ? C12 Co1 C5 147.69(7) . . ? C11 Co1 C5 170.39(7) . . ? C14 Co1 C5 102.34(7) . . ? C15 Co1 C5 110.75(7) . . ? C12 Co1 C2 103.67(6) . . ? C11 Co1 C2 110.62(6) . . ? C14 Co1 C2 149.89(7) . . ? C15 Co1 C2 168.38(6) . . ? C5 Co1 C2 66.89(7) . . ? C12 Co1 C1 112.86(7) . . ? C11 Co1 C1 143.18(7) . . ? C14 Co1 C1 113.85(7) . . ? C15 Co1 C1 144.42(7) . . ? C5 Co1 C1 39.96(7) . . ? C2 Co1 C1 39.88(7) . . ? C12 Co1 C4 165.62(7) . . ? C11 Co1 C4 130.30(7) . . ? C14 Co1 C4 124.04(7) . . ? C15 Co1 C4 103.95(6) . . ? C5 Co1 C4 40.10(7) . . ? C2 Co1 C4 66.59(6) . . ? C1 Co1 C4 67.08(7) . . ? C12 Co1 C3 126.85(6) . . ? C11 Co1 C3 105.40(6) . . ? C14 Co1 C3 162.65(6) . . ? C15 Co1 C3 128.52(6) . . ? C5 Co1 C3 66.47(6) . . ? C2 Co1 C3 39.86(6) . . ? C1 Co1 C3 66.81(6) . . ? C4 Co1 C3 39.01(6) . . ? C31 Co2 C32 41.23(6) . . ? C31 Co2 C35 69.88(6) . . ? C32 Co2 C35 84.24(6) . . ? C31 Co2 C34 84.21(6) . . ? C32 Co2 C34 69.70(6) . . ? C35 Co2 C34 40.69(6) . . ? C31 Co2 C24B 162.6(6) . . ? C32 Co2 C24B 153.8(6) . . ? C35 Co2 C24B 112.1(4) . . ? C34 Co2 C24B 108.7(5) . . ? C31 Co2 C25B 123.6(6) . . ? C32 Co2 C25B 157.8(7) . . ? C35 Co2 C25B 106.6(5) . . ? C34 Co2 C25B 130.9(7) . . ? C24B Co2 C25B 39.0(5) . . ? C31 Co2 C23B 147.0(5) . . ? C32 Co2 C23B 117.8(5) . . ? C35 Co2 C23B 142.0(5) . . ? C34 Co2 C23B 114.9(4) . . ? C24B Co2 C23B 37.5(6) . . ? C25B Co2 C23B 65.0(6) . . ? C31 Co2 C22A 108.00(15) . . ? C32 Co2 C22A 107.13(15) . . ? C35 Co2 C22A 160.51(18) . . ? C34 Co2 C22A 158.02(17) . . ? C24B Co2 C22A 64.0(4) . . ? C25B Co2 C22A 57.5(5) . . ? C23B Co2 C22A 46.0(4) . . ? C31 Co2 C21B 99.9(5) . . ? C32 Co2 C21B 120.9(5) . . ? C35 Co2 C21B 129.9(5) . . ? C34 Co2 C21B 167.6(6) . . ? C24B Co2 C21B 65.0(6) . . ? C25B Co2 C21B 37.6(6) . . ? C23B Co2 C21B 67.3(6) . . ? C22A Co2 C21B 30.6(5) . . ? C31 Co2 C24A 173.28(8) . . ? C32 Co2 C24A 140.35(15) . . ? C35 Co2 C24A 115.76(9) . . ? C34 Co2 C24A 102.46(9) . . ? C24B Co2 C24A 13.8(5) . . ? C25B Co2 C24A 52.3(5) . . ? C23B Co2 C24A 28.5(5) . . ? C22A Co2 C24A 65.43(15) . . ? C21B Co2 C24A 73.7(4) . . ? C31 Co2 C25A 137.71(15) . . ? C32 Co2 C25A 173.11(12) . . ? C35 Co2 C25A 101.77(8) . . ? C34 Co2 C25A 117.08(14) . . ? C24B Co2 C25A 25.7(5) . . ? C25B Co2 C25A 16.6(5) . . ? C23B Co2 C25A 59.1(5) . . ? C22A Co2 C25A 66.16(16) . . ? C21B Co2 C25A 52.6(5) . . ? C24A Co2 C25A 39.54(11) . . ? C31 Co2 C23A 136.09(14) . . ? C32 Co2 C23A 109.58(11) . . ? C35 Co2 C23A 152.20(15) . . ? C34 Co2 C23A 120.27(11) . . ? C24B Co2 C23A 47.2(5) . . ? C25B Co2 C23A 69.6(4) . . ? C23B Co2 C23A 10.9(4) . . ? C22A Co2 C23A 38.89(18) . . ? C21B Co2 C23A 64.3(5) . . ? C24A Co2 C23A 39.32(11) . . ? C25A Co2 C23A 66.47(11) . . ? C2 C1 C5 107.13(14) . . ? C2 C1 Co1 69.66(9) . . ? C5 C1 Co1 69.40(9) . . ? C2 C1 H1 126.4 . . ? C5 C1 H1 126.4 . . ? Co1 C1 H1 126.1 . . ? C1 C2 C3 108.47(14) . . ? C1 C2 Co1 70.46(9) . . ? C3 C2 Co1 71.28(8) . . ? C1 C2 H2 125.8 . . ? C3 C2 H2 125.8 . . ? Co1 C2 H2 124.1 . . ? C4 C3 C2 108.23(14) . . ? C4 C3 Co1 70.41(9) . . ? C2 C3 Co1 68.87(8) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Co1 C3 H3 126.4 . . ? C3 C4 C5 107.55(14) . . ? C3 C4 Co1 70.58(9) . . ? C5 C4 Co1 68.62(9) . . ? C3 C4 H4 126.2 . . ? C5 C4 H4 126.2 . . ? Co1 C4 H4 126.1 . . ? C1 C5 C4 108.59(14) . . ? C1 C5 Co1 70.64(9) . . ? C4 C5 Co1 71.28(9) . . ? C1 C5 H5 125.7 . . ? C4 C5 H5 125.7 . . ? Co1 C5 H5 124.0 . . ? C12 C11 C16 106.04(12) . . ? C12 C11 Co1 69.15(9) . . ? C16 C11 Co1 96.76(9) . . ? C12 C11 H11 126.5(12) . . ? C16 C11 H11 124.8(12) . . ? Co1 C11 H11 115.3(11) . . ? C11 C12 C13 106.01(13) . . ? C11 C12 Co1 69.61(9) . . ? C13 C12 Co1 96.65(10) . . ? C11 C12 H12 125.7(12) . . ? C13 C12 H12 125.2(11) . . ? Co1 C12 H12 115.7(11) . . ? C14 C13 C12 97.29(12) . . ? C14 C13 C17 101.95(13) . . ? C12 C13 C17 101.71(13) . . ? C14 C13 H13 117.5 . . ? C12 C13 H13 117.5 . . ? C17 C13 H13 117.5 . . ? C15 C14 C13 106.06(13) . . ? C15 C14 Co1 69.64(9) . . ? C13 C14 Co1 96.26(10) . . ? C15 C14 H14 125.4(12) . . ? C13 C14 H14 125.8(12) . . ? Co1 C14 H14 115.0(11) . . ? C14 C15 C16 106.13(13) . . ? C14 C15 Co1 69.47(9) . . ? C16 C15 Co1 96.31(9) . . ? C14 C15 H15 125.7(13) . . ? C16 C15 H15 125.8(12) . . ? Co1 C15 H15 114.5(12) . . ? C11 C16 C15 97.23(11) . . ? C11 C16 C17 101.92(12) . . ? C15 C16 C17 101.86(12) . . ? C11 C16 H16 117.5 . . ? C15 C16 H16 117.5 . . ? C17 C16 H16 117.5 . . ? C16 C17 C13 94.26(12) . . ? C16 C17 H17A 112.9 . . ? C13 C17 H17A 112.9 . . ? C16 C17 H17B 112.9 . . ? C13 C17 H17B 112.9 . . ? H17A C17 H17B 110.3 . . ? C25A C21A C22A 105.8(3) . . ? C25A C21A Co2 70.48(13) . . ? C22A C21A Co2 67.4(2) . . ? C25A C21A H21A 127.1 . . ? C22A C21A H21A 127.1 . . ? Co2 C21A H21A 126.5 . . ? C23A C22A C21A 110.5(3) . . ? C23A C22A Co2 72.9(2) . . ? C21A C22A Co2 72.0(2) . . ? C23A C22A H22A 124.8 . . ? C21A C22A H22A 124.8 . . ? Co2 C22A H22A 121.9 . . ? C22A C23A C24A 106.3(3) . . ? C22A C23A Co2 68.2(2) . . ? C24A C23A Co2 69.96(13) . . ? C22A C23A H23A 126.8 . . ? C24A C23A H23A 126.8 . . ? Co2 C23A H23A 126.6 . . ? C23A C24A C25A 109.0(2) . . ? C23A C24A Co2 70.72(14) . . ? C25A C24A Co2 70.51(13) . . ? C23A C24A H24A 125.5 . . ? C25A C24A H24A 125.5 . . ? Co2 C24A H24A 124.8 . . ? C21A C25A C24A 108.4(2) . . ? C21A C25A Co2 70.71(14) . . ? C24A C25A Co2 69.95(11) . . ? C21A C25A H25A 125.8 . . ? C24A C25A H25A 125.8 . . ? Co2 C25A H25A 125.1 . . ? C22B C21B C25B 114.6(17) . . ? C22B C21B Co2 76.6(13) . . ? C25B C21B Co2 69.7(9) . . ? C22B C21B H21B 122.7 . . ? C25B C21B H21B 122.7 . . ? Co2 C21B H21B 122.4 . . ? C21B C22B C23B 102.1(18) . . ? C21B C22B Co2 69.2(13) . . ? C23B C22B Co2 63.0(10) . . ? C21B C22B H22B 129.0 . . ? C23B C22B H22B 129.0 . . ? Co2 C22B H22B 130.0 . . ? C24B C23B C22B 102.0(13) . . ? C24B C23B Co2 70.7(9) . . ? C22B C23B Co2 70.2(10) . . ? C24B C23B H23B 129.0 . . ? C22B C23B H23B 129.0 . . ? Co2 C23B H23B 122.1 . . ? C23B C24B C25B 110.4(13) . . ? C23B C24B Co2 71.7(9) . . ? C25B C24B Co2 70.6(8) . . ? C23B C24B H24B 124.8 . . ? C25B C24B H24B 124.8 . . ? Co2 C24B H24B 124.5 . . ? C21B C25B C24B 110.6(14) . . ? C21B C25B Co2 72.7(10) . . ? C24B C25B Co2 70.4(8) . . ? C21B C25B H25B 124.7 . . ? C24B C25B H25B 124.7 . . ? Co2 C25B H25B 123.8 . . ? C32 C31 C36 105.91(12) . . ? C32 C31 Co2 69.43(8) . . ? C36 C31 Co2 96.61(9) . . ? C32 C31 H31 128.4(11) . . ? C36 C31 H31 123.2(11) . . ? Co2 C31 H31 115.3(11) . . ? C31 C32 C33 105.98(12) . . ? C31 C32 Co2 69.33(8) . . ? C33 C32 Co2 96.83(9) . . ? C31 C32 H32 127.6(11) . . ? C33 C32 H32 124.1(11) . . ? Co2 C32 H32 114.6(11) . . ? C34 C33 C32 97.16(11) . . ? C34 C33 C37 102.01(12) . . ? C32 C33 C37 101.70(12) . . ? C34 C33 H33 117.6 . . ? C32 C33 H33 117.6 . . ? C37 C33 H33 117.6 . . ? C35 C34 C33 106.21(12) . . ? C35 C34 Co2 69.45(8) . . ? C33 C34 Co2 96.31(9) . . ? C35 C34 H34 125.3(12) . . ? C33 C34 H34 126.0(12) . . ? Co2 C34 H34 114.6(12) . . ? C34 C35 C36 106.07(12) . . ? C34 C35 Co2 69.86(8) . . ? C36 C35 Co2 96.23(9) . . ? C34 C35 H35 124.7(12) . . ? C36 C35 H35 127.0(12) . . ? Co2 C35 H35 113.4(11) . . ? C35 C36 C31 97.28(11) . . ? C35 C36 C37 102.12(12) . . ? C31 C36 C37 101.71(12) . . ? C35 C36 H36 117.5 . . ? C31 C36 H36 117.5 . . ? C37 C36 H36 117.5 . . ? C36 C37 C33 94.28(11) . . ? C36 C37 H37A 112.9 . . ? C33 C37 H37A 112.9 . . ? C36 C37 H37B 112.9 . . ? C33 C37 H37B 112.9 . . ? H37A C37 H37B 110.3 . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.427 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.062 #===END data_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34 Co2' _chemical_formula_weight 464.39 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' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 11.3070(2) _cell_length_b 7.32500(10) _cell_length_c 12.6230(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.8830(10) _cell_angle_gamma 90.00 _cell_volume 1019.17(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 18476 _cell_measurement_theta_min 7.87 _cell_measurement_theta_max 30.50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 1.637 _exptl_absorpt_correction_type 'Multi-scan' _exptl_absorpt_correction_T_min 0.7355 _exptl_absorpt_correction_T_max 0.7627 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 Kappa CCD Diffractometer' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18476 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0300 _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 -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 7.87 _diffrn_reflns_theta_max 30.50 _reflns_number_total 3052 _reflns_number_gt 2636 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kappa CCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP 3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0262P)^2^+0.3761P] 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 3052 _refine_ls_number_parameters 134 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0607 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _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 Co1 Co 0.293533(15) 0.18037(2) 0.789363(14) 0.01469(6) Uani 1 1 d . . . C4 C 0.26132(13) 0.45043(17) 0.82657(12) 0.0218(3) Uani 1 1 d . . . H4 H 0.2384 0.5438 0.7738 0.026 Uiso 1 1 calc R . . C15 C 0.37987(13) 0.17901(18) 0.66496(12) 0.0201(3) Uani 1 1 d . . . C3 C 0.18085(13) 0.33479(18) 0.86644(12) 0.0204(3) Uani 1 1 d . . . H3 H 0.0947 0.3392 0.8475 0.024 Uiso 1 1 calc R . . C14 C 0.43177(13) -0.0067(2) 0.64480(12) 0.0233(3) Uani 1 1 d . . . H14A H 0.5166 0.0086 0.6376 0.028 Uiso 1 1 calc R . . H14B H 0.3842 -0.0579 0.5758 0.028 Uiso 1 1 calc R . . C13 C 0.42863(13) -0.14056(19) 0.73789(13) 0.0230(3) Uani 1 1 d . . . H13A H 0.4115 -0.2650 0.7078 0.028 Uiso 1 1 calc R . . H13B H 0.5091 -0.1426 0.7887 0.028 Uiso 1 1 calc R . . C18 C 0.16100(13) -0.0866(2) 0.62702(12) 0.0245(3) Uani 1 1 d . . . H18A H 0.0778 -0.1371 0.6135 0.029 Uiso 1 1 calc R . . H18B H 0.2128 -0.1746 0.5987 0.029 Uiso 1 1 calc R . . C12 C 0.33328(13) -0.08803(17) 0.79921(11) 0.0193(3) Uani 1 1 d . . . C17 C 0.15932(13) 0.0961(2) 0.56736(12) 0.0240(3) Uani 1 1 d . . . H17A H 0.1727 0.0739 0.4936 0.029 Uiso 1 1 calc R . . H17B H 0.0787 0.1538 0.5596 0.029 Uiso 1 1 calc R . . C11 C 0.20956(12) -0.06144(18) 0.74883(12) 0.0192(2) Uani 1 1 d . . . C16 C 0.25607(13) 0.22476(19) 0.62768(11) 0.0203(3) Uani 1 1 d . . . C1 C 0.37798(14) 0.2569(2) 0.94948(12) 0.0270(3) Uani 1 1 d . . . H1 H 0.4455 0.1986 0.9953 0.032 Uiso 1 1 calc R . . C5 C 0.38282(13) 0.4032(2) 0.87899(13) 0.0254(3) Uani 1 1 d . . . H5 H 0.4544 0.4608 0.8680 0.030 Uiso 1 1 calc R . . C2 C 0.25294(14) 0.21128(19) 0.93998(12) 0.0237(3) Uani 1 1 d . . . H2 H 0.2233 0.1144 0.9768 0.028 Uiso 1 1 calc R . . H11 H 0.1550 -0.0823 0.7952 0.026(4) Uiso 1 1 d R . . H12 H 0.3499 -0.1258 0.8771 0.020(4) Uiso 1 1 d R . . H16 H 0.2396 0.3554 0.6099 0.022(4) Uiso 1 1 d R . . H15 H 0.4402(18) 0.280(3) 0.6748(18) 0.034(5) 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 Co1 0.01572(10) 0.01341(9) 0.01476(10) 0.00042(6) 0.00305(6) -0.00030(6) C4 0.0271(7) 0.0130(5) 0.0247(7) -0.0023(5) 0.0042(5) 0.0007(5) C15 0.0228(6) 0.0200(6) 0.0193(6) 0.0005(5) 0.0088(5) -0.0034(5) C3 0.0195(6) 0.0206(6) 0.0219(7) -0.0036(5) 0.0063(5) 0.0010(5) C14 0.0207(6) 0.0265(7) 0.0242(7) -0.0037(5) 0.0083(5) 0.0000(5) C13 0.0207(6) 0.0195(6) 0.0285(7) -0.0027(5) 0.0047(5) 0.0025(5) C18 0.0211(7) 0.0272(7) 0.0242(7) -0.0052(5) 0.0032(5) -0.0064(5) C12 0.0229(6) 0.0131(5) 0.0217(6) 0.0010(5) 0.0044(5) 0.0002(5) C17 0.0219(7) 0.0316(7) 0.0170(6) -0.0014(5) 0.0010(5) 0.0029(5) C11 0.0211(6) 0.0160(6) 0.0218(6) -0.0015(5) 0.0073(5) -0.0045(5) C16 0.0255(7) 0.0213(6) 0.0143(6) 0.0037(5) 0.0045(5) 0.0015(5) C1 0.0280(7) 0.0308(7) 0.0181(7) -0.0066(6) -0.0036(5) 0.0063(6) C5 0.0223(7) 0.0245(7) 0.0293(8) -0.0110(6) 0.0055(6) -0.0060(5) C2 0.0332(8) 0.0227(6) 0.0170(6) -0.0003(5) 0.0091(6) 0.0021(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C12 2.0144(13) . ? Co1 C16 2.0162(13) . ? Co1 C11 2.0209(13) . ? Co1 C15 2.0256(14) . ? Co1 C2 2.0654(14) . ? Co1 C4 2.0839(13) . ? Co1 C3 2.0981(13) . ? Co1 C1 2.1096(14) . ? Co1 C5 2.1104(14) . ? C4 C3 1.415(2) . ? C4 C5 1.428(2) . ? C4 H4 0.9500 . ? C15 C16 1.414(2) . ? C15 C14 1.5252(19) . ? C15 H15 0.99(2) . ? C3 C2 1.417(2) . ? C3 H3 0.9500 . ? C14 C13 1.537(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C13 C12 1.511(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C18 C11 1.524(2) . ? C18 C17 1.534(2) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C12 C11 1.4152(19) . ? C12 H12 0.9986 . ? C17 C16 1.514(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C11 H11 0.9532 . ? C16 H16 0.9908 . ? C1 C5 1.402(2) . ? C1 C2 1.432(2) . ? C1 H1 0.9500 . ? C5 H5 0.9500 . ? C2 H2 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 C12 Co1 C16 102.33(6) . . ? C12 Co1 C11 41.06(6) . . ? C16 Co1 C11 84.51(6) . . ? C12 Co1 C15 84.47(6) . . ? C16 Co1 C15 40.96(6) . . ? C11 Co1 C15 94.58(6) . . ? C12 Co1 C2 98.19(6) . . ? C16 Co1 C2 150.99(6) . . ? C11 Co1 C2 98.10(6) . . ? C15 Co1 C2 163.47(6) . . ? C12 Co1 C4 163.81(6) . . ? C16 Co1 C4 93.86(6) . . ? C11 Co1 C4 142.49(5) . . ? C15 Co1 C4 108.55(6) . . ? C2 Co1 C4 66.58(6) . . ? C12 Co1 C3 130.37(6) . . ? C16 Co1 C3 111.73(6) . . ? C11 Co1 C3 106.87(5) . . ? C15 Co1 C3 144.06(6) . . ? C2 Co1 C3 39.78(6) . . ? C4 Co1 C3 39.56(5) . . ? C12 Co1 C1 98.81(6) . . ? C16 Co1 C1 151.05(6) . . ? C11 Co1 C1 124.21(6) . . ? C15 Co1 C1 123.41(6) . . ? C2 Co1 C1 40.09(6) . . ? C4 Co1 C1 66.19(6) . . ? C3 Co1 C1 66.70(6) . . ? C12 Co1 C5 130.41(6) . . ? C16 Co1 C5 112.67(6) . . ? C11 Co1 C5 162.78(6) . . ? C15 Co1 C5 99.43(6) . . ? C2 Co1 C5 66.40(6) . . ? C4 Co1 C5 39.81(6) . . ? C3 Co1 C5 66.54(6) . . ? C1 Co1 C5 38.80(6) . . ? C3 C4 C5 108.57(13) . . ? C3 C4 Co1 70.76(7) . . ? C5 C4 Co1 71.10(8) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Co1 C4 H4 124.0 . . ? C16 C15 C14 123.02(12) . . ? C16 C15 Co1 69.17(8) . . ? C14 C15 Co1 113.80(9) . . ? C16 C15 H15 117.9(12) . . ? C14 C15 H15 113.8(11) . . ? Co1 C15 H15 109.7(12) . . ? C4 C3 C2 107.08(12) . . ? C4 C3 Co1 69.68(8) . . ? C2 C3 Co1 68.87(8) . . ? C4 C3 H3 126.5 . . ? C2 C3 H3 126.5 . . ? Co1 C3 H3 126.5 . . ? C15 C14 C13 111.47(11) . . ? C15 C14 H14A 109.3 . . ? C13 C14 H14A 109.3 . . ? C15 C14 H14B 109.3 . . ? C13 C14 H14B 109.3 . . ? H14A C14 H14B 108.0 . . ? C12 C13 C14 111.72(11) . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C11 C18 C17 110.62(11) . . ? C11 C18 H18A 109.5 . . ? C17 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 108.1 . . ? C11 C12 C13 123.49(13) . . ? C11 C12 Co1 69.72(7) . . ? C13 C12 Co1 113.07(9) . . ? C11 C12 H12 115.5 . . ? C13 C12 H12 115.8 . . ? Co1 C12 H12 108.8 . . ? C16 C17 C18 111.57(11) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C12 C11 C18 122.30(12) . . ? C12 C11 Co1 69.22(7) . . ? C18 C11 Co1 113.86(9) . . ? C12 C11 H11 114.4 . . ? C18 C11 H11 117.6 . . ? Co1 C11 H11 108.5 . . ? C15 C16 C17 124.78(12) . . ? C15 C16 Co1 69.88(8) . . ? C17 C16 Co1 111.95(9) . . ? C15 C16 H16 115.2 . . ? C17 C16 H16 114.1 . . ? Co1 C16 H16 111.8 . . ? C5 C1 C2 107.63(13) . . ? C5 C1 Co1 70.63(8) . . ? C2 C1 Co1 68.29(8) . . ? C5 C1 H1 126.2 . . ? C2 C1 H1 126.2 . . ? Co1 C1 H1 126.5 . . ? C1 C5 C4 108.04(13) . . ? C1 C5 Co1 70.57(8) . . ? C4 C5 Co1 69.10(8) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Co1 C5 H5 125.9 . . ? C3 C2 C1 108.60(13) . . ? C3 C2 Co1 71.35(8) . . ? C1 C2 Co1 71.62(8) . . ? C3 C2 H2 125.7 . . ? C1 C2 H2 125.7 . . ? Co1 C2 H2 123.0 . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.385 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.061 #===END