# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2305 data_global _publ_contact_author_name 'F.A. Cotton' _publ_contact_author_address ; Laboratory for Molecular Structure and Bonding Dept. of Chemistry Texas A&M University, P.O. Box 30012 College Station, TX 77842-3012, USA ; _publ_contact_author_email cotton@tamu.edu _publ_contact_author_fax '(979) 845 9351' _publ_contact_author_phone '(979) 845 4432' _publ_requested_journal 'Dalton Transactions' data_1.CH2Cl2_at_111K _audit_creation_method SHELXL _chemical_formula_sum 'C41 H34 Br2 Cl2 Co3 N12' _chemical_formula_weight 1102.31 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.829(1) _cell_length_b 13.935(2) _cell_length_c 11.158(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1994.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 111(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.008 _cell_measurement_theta_max 24.467 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.835 _exptl_crystal_density_method ? _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 3.420 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.1241 _exptl_absorpt_correction_T_max 0.2006 _diffrn_ambient_temperature 111(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'Omega-theta scans' _diffrn_refln_scan_width 0.70 _diffrn_refln_scan_mode_backgd MO _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7650 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.14 _reflns_number_total 3570 _reflns_number_observed 3381 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 V5' _computing_cell_refinement 'CAD4 V5' _computing_data_reduction 'XCAD4 (Harms, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1213P)^2^+11.7412P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 3570 _refine_ls_number_parameters 281 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_obs 0.0591 _refine_ls_wR_factor_all 0.1799 _refine_ls_wR_factor_obs 0.1770 _refine_ls_goodness_of_fit_all 1.060 _refine_ls_goodness_of_fit_obs 1.073 _refine_ls_restrained_S_all 1.060 _refine_ls_restrained_S_obs 1.073 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.15516(6) 0.91511(5) 0.32327(10) 0.0097(2) Uani 1 d . . Co2 Co 0.0000 1.0000 0.3173(2) 0.0087(3) Uani 1 d S . Br1 Br 0.32828(7) 0.81513(6) 0.32493(11) 0.0349(3) Uani 1 d . . N1 N 0.1141(5) 0.8795(4) 0.4883(6) 0.0125(12) Uani 1 d . . N2 N 0.0712(5) 0.8075(4) 0.2608(6) 0.0151(13) Uani 1 d . . N3 N 0.2206(5) 1.0315(4) 0.3861(5) 0.0116(12) Uani 1 d . . N4 N 0.1747(5) 0.9662(4) 0.1580(6) 0.0131(13) Uani 1 d . . N5 N 0.0510(5) 1.0822(5) 0.1972(6) 0.0088(14) Uani 1 d . . N6 N 0.0555(6) 1.0843(5) 0.4368(6) 0.0107(14) Uani 1 d . . C1 C 0.0122(6) 0.8819(5) 0.5209(7) 0.0108(14) Uani 1 d . . C2 C -0.0170(6) 0.8579(6) 0.6394(8) 0.018(2) Uani 1 d . . H2 H -0.0877(6) 0.8620(6) 0.6639(8) 0.021 Uiso 1 calc R . C3 C 0.0581(7) 0.8287(7) 0.7179(7) 0.023(2) Uani 1 d . . H3 H 0.0385(7) 0.8085(7) 0.7961(7) 0.027 Uiso 1 calc R . C4 C 0.1625(6) 0.8281(7) 0.6856(8) 0.023(2) Uani 1 d . . H4 H 0.2152(6) 0.8099(7) 0.7410(8) 0.028 Uiso 1 calc R . C5 C 0.1875(6) 0.8551(6) 0.5682(7) 0.018(2) Uani 1 d . . H5 H 0.2586(6) 0.8562(6) 0.5445(7) 0.021 Uiso 1 calc R . C6 C -0.0171(6) 0.8246(6) 0.1978(7) 0.015(2) Uani 1 d . . C7 C -0.0724(6) 0.7462(5) 0.1458(8) 0.019(2) Uani 1 d . . H7 H -0.1328(6) 0.7583(5) 0.0989(8) 0.023 Uiso 1 calc R . C8 C -0.0396(7) 0.6542(7) 0.1626(10) 0.030(2) Uani 1 d . . H8 H -0.0767(7) 0.6022(7) 0.1278(10) 0.035 Uiso 1 calc R . C9 C 0.0493(7) 0.6372(6) 0.2317(11) 0.037(3) Uani 1 d . . H9 H 0.0737(7) 0.5738(6) 0.2455(11) 0.044 Uiso 1 calc R . C10 C 0.1001(7) 0.7149(6) 0.2789(9) 0.029(2) Uani 1 d . . H10 H 0.1595(7) 0.7032(6) 0.3276(9) 0.035 Uiso 1 calc R . C11 C 0.3240(6) 1.0464(6) 0.3757(8) 0.017(2) Uani 1 d . . H11 H 0.3646(6) 0.9985(6) 0.3370(8) 0.021 Uiso 1 calc R . C12 C 0.3744(7) 1.1274(6) 0.4182(8) 0.019(2) Uani 1 d . . H12 H 0.4475(7) 1.1356(6) 0.4098(8) 0.023 Uiso 1 calc R . C13 C 0.3118(7) 1.1968(6) 0.4744(9) 0.022(2) Uani 1 d . . H13 H 0.3431(7) 1.2527(6) 0.5072(9) 0.026 Uiso 1 calc R . C14 C 0.2062(6) 1.1845(5) 0.4823(8) 0.017(2) Uani 1 d . . H14 H 0.1640(6) 1.2335(5) 0.5164(8) 0.020 Uiso 1 calc R . C15 C 0.1596(5) 1.0989(6) 0.4396(7) 0.012(2) Uani 1 d . . C16 C 0.2401(6) 0.9224(5) 0.0809(7) 0.017(2) Uani 1 d . . H16 H 0.2777(6) 0.8682(5) 0.1088(7) 0.021 Uiso 1 calc R . C17 C 0.2560(7) 0.9513(6) -0.0366(7) 0.023(2) Uani 1 d . . H17 H 0.3042(7) 0.9187(6) -0.0868(7) 0.028 Uiso 1 calc R . C18 C 0.1997(7) 1.0289(7) -0.0785(8) 0.025(2) Uani 1 d . . H18 H 0.2078(7) 1.0498(7) -0.1590(8) 0.030 Uiso 1 calc R . C19 C 0.1316(7) 1.0759(6) -0.0030(7) 0.019(2) Uani 1 d . . H19 H 0.0927(7) 1.1294(6) -0.0309(7) 0.023 Uiso 1 calc R . C20 C 0.1204(6) 1.0441(6) 0.1150(7) 0.016(2) Uani 1 d . . C21 C -0.0111(15) 0.4681(13) 0.6206(17) 0.023(4) Uiso 0.50 d P . H21A H 0.0531(15) 0.4397(13) 0.6548(17) 0.028 Uiso 0.50 calc PR . H21B H -0.0586(15) 0.4727(13) 0.6903(17) 0.028 Uiso 0.50 calc PR . Cl2 Cl 0.0348(5) 0.5806(4) 0.5927(6) 0.0471(15) Uani 0.50 d P . Cl3 Cl -0.0160(4) 0.3930(4) 0.4946(5) 0.0363(11) Uani 0.50 d P . 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 0.0090(4) 0.0088(4) 0.0113(4) -0.0018(5) 0.0002(5) -0.0009(3) Co2 0.0082(6) 0.0084(5) 0.0096(6) 0.000 0.000 -0.0010(4) Br1 0.0325(5) 0.0344(5) 0.0378(5) -0.0027(5) -0.0007(6) 0.0020(3) N1 0.016(3) 0.008(3) 0.013(3) -0.001(2) -0.002(3) 0.000(2) N2 0.012(3) 0.013(3) 0.020(3) -0.003(3) 0.007(3) 0.001(3) N3 0.013(3) 0.015(3) 0.008(3) 0.002(2) 0.002(2) 0.000(3) N4 0.011(3) 0.007(3) 0.021(3) -0.005(2) 0.003(3) -0.004(2) N5 0.010(3) 0.010(3) 0.006(3) 0.001(2) 0.001(3) 0.000(3) N6 0.009(3) 0.006(3) 0.017(3) 0.000(3) -0.002(3) -0.001(3) C1 0.013(4) 0.004(3) 0.016(4) -0.003(3) 0.001(3) 0.001(3) C2 0.013(4) 0.018(4) 0.023(4) 0.005(3) 0.003(3) 0.001(3) C3 0.023(4) 0.034(5) 0.011(4) 0.012(3) 0.001(3) 0.002(4) C4 0.013(4) 0.041(5) 0.016(4) 0.003(4) -0.004(3) 0.006(3) C5 0.017(4) 0.015(4) 0.021(4) 0.003(3) 0.002(3) 0.002(3) C6 0.008(3) 0.019(4) 0.019(4) -0.003(3) 0.001(3) -0.003(3) C7 0.014(4) 0.015(4) 0.028(4) -0.016(3) 0.000(3) -0.003(3) C8 0.020(4) 0.021(4) 0.047(6) -0.011(4) -0.004(4) -0.006(4) C9 0.021(4) 0.013(4) 0.076(8) -0.011(4) -0.021(5) 0.003(4) C10 0.016(4) 0.018(4) 0.054(6) -0.003(4) -0.008(4) -0.001(3) C11 0.013(4) 0.021(4) 0.018(3) -0.002(3) 0.003(3) 0.000(3) C12 0.018(4) 0.017(4) 0.023(4) -0.003(3) -0.003(3) -0.006(3) C13 0.016(4) 0.018(4) 0.032(5) -0.008(4) 0.001(3) -0.006(3) C14 0.014(4) 0.015(3) 0.020(4) -0.007(3) -0.001(3) 0.000(3) C15 0.009(4) 0.014(3) 0.014(4) 0.002(3) -0.002(3) 0.003(3) C16 0.023(4) 0.015(4) 0.014(4) -0.006(3) 0.006(3) -0.006(3) C17 0.030(5) 0.025(4) 0.014(4) -0.008(3) 0.011(3) -0.009(4) C18 0.026(5) 0.034(5) 0.016(4) 0.002(4) 0.001(4) -0.009(4) C19 0.018(4) 0.023(4) 0.018(4) 0.003(3) 0.002(3) -0.001(3) C20 0.015(4) 0.016(4) 0.016(4) 0.001(3) 0.000(3) -0.006(3) Cl2 0.037(3) 0.041(3) 0.064(4) -0.026(3) -0.013(3) 0.008(3) Cl3 0.022(2) 0.045(3) 0.042(3) -0.003(2) -0.007(2) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.957(6) . ? Co1 N2 1.973(7) . ? Co1 N1 1.978(6) . ? Co1 N4 1.992(7) . ? Co1 Co2 2.3165(8) . ? Co1 Br1 2.6219(12) . ? Co2 N5 1.880(7) 2_575 ? Co2 N5 1.880(7) . ? Co2 N6 1.914(7) 2_575 ? Co2 N6 1.914(7) . ? Co2 Co1 2.3164(8) 2_575 ? N1 C5 1.341(11) . ? N1 C1 1.358(10) . ? N2 C6 1.355(11) . ? N2 C10 1.357(11) . ? N3 C11 1.347(10) . ? N3 C15 1.360(10) . ? N4 C16 1.347(10) . ? N4 C20 1.377(10) . ? N5 C6 1.370(11) 2_575 ? N5 C20 1.384(11) . ? N6 C15 1.352(10) . ? N6 C1 1.363(10) 2_575 ? C1 N6 1.363(10) 2_575 ? C1 C2 1.414(11) . ? C2 C3 1.364(12) . ? C3 C4 1.388(12) . ? C4 C5 1.400(12) . ? C6 N5 1.370(11) 2_575 ? C6 C7 1.426(11) . ? C7 C8 1.363(13) . ? C8 C9 1.396(14) . ? C9 C10 1.369(13) . ? C11 C12 1.385(12) . ? C12 C13 1.404(12) . ? C13 C14 1.369(12) . ? C14 C15 1.417(11) . ? C16 C17 1.386(11) . ? C17 C18 1.381(13) . ? C18 C19 1.379(12) . ? C19 C20 1.396(11) . ? C21 Cl2 0.81(2) 2_565 ? C21 C21 0.93(4) 2_565 ? C21 Cl2 1.70(2) . ? C21 Cl3 1.75(2) . ? Cl2 C21 0.81(2) 2_565 ? Cl2 Cl3 1.180(9) 2_565 ? Cl2 Cl2 2.416(13) 2_565 ? Cl3 Cl2 1.180(9) 2_565 ? 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 N3 Co1 N2 172.2(3) . . ? N3 Co1 N1 89.3(3) . . ? N2 Co1 N1 89.6(3) . . ? N3 Co1 N4 88.9(2) . . ? N2 Co1 N4 90.8(3) . . ? N1 Co1 N4 169.9(3) . . ? N3 Co1 Co2 87.5(2) . . ? N2 Co1 Co2 84.8(2) . . ? N1 Co1 Co2 85.8(2) . . ? N4 Co1 Co2 84.2(2) . . ? N3 Co1 Br1 94.3(2) . . ? N2 Co1 Br1 93.5(2) . . ? N1 Co1 Br1 94.9(2) . . ? N4 Co1 Br1 95.1(2) . . ? Co2 Co1 Br1 178.15(6) . . ? N5 Co2 N5 89.1(4) 2_575 . ? N5 Co2 N6 89.6(2) 2_575 2_575 ? N5 Co2 N6 178.3(4) . 2_575 ? N5 Co2 N6 178.3(4) 2_575 . ? N5 Co2 N6 89.6(2) . . ? N6 Co2 N6 91.7(4) 2_575 . ? N5 Co2 Co1 91.9(2) 2_575 2_575 ? N5 Co2 Co1 90.5(2) . 2_575 ? N6 Co2 Co1 88.5(2) 2_575 2_575 ? N6 Co2 Co1 89.2(2) . 2_575 ? N5 Co2 Co1 90.5(2) 2_575 . ? N5 Co2 Co1 91.9(2) . . ? N6 Co2 Co1 89.2(2) 2_575 . ? N6 Co2 Co1 88.5(2) . . ? Co1 Co2 Co1 176.71(10) 2_575 . ? C5 N1 C1 120.3(7) . . ? C5 N1 Co1 119.7(5) . . ? C1 N1 Co1 120.0(5) . . ? C6 N2 C10 118.2(7) . . ? C6 N2 Co1 120.4(5) . . ? C10 N2 Co1 121.4(6) . . ? C11 N3 C15 119.9(7) . . ? C11 N3 Co1 121.3(5) . . ? C15 N3 Co1 118.8(5) . . ? C16 N4 C20 116.7(7) . . ? C16 N4 Co1 120.6(5) . . ? C20 N4 Co1 122.7(5) . . ? C6 N5 C20 124.8(7) 2_575 . ? C6 N5 Co2 117.6(5) 2_575 . ? C20 N5 Co2 117.6(5) . . ? C15 N6 C1 124.2(7) . 2_575 ? C15 N6 Co2 118.4(6) . . ? C1 N6 Co2 117.0(5) 2_575 . ? N1 C1 N6 115.9(7) . 2_575 ? N1 C1 C2 120.0(7) . . ? N6 C1 C2 123.9(7) 2_575 . ? C3 C2 C1 119.0(8) . . ? C2 C3 C4 121.1(8) . . ? C3 C4 C5 117.5(7) . . ? N1 C5 C4 122.0(8) . . ? N2 C6 N5 115.8(7) . 2_575 ? N2 C6 C7 119.5(7) . . ? N5 C6 C7 124.5(7) 2_575 . ? C8 C7 C6 120.7(8) . . ? C7 C8 C9 119.2(8) . . ? C10 C9 C8 117.9(8) . . ? N2 C10 C9 124.4(9) . . ? N3 C11 C12 123.7(8) . . ? C11 C12 C13 116.5(7) . . ? C14 C13 C12 120.6(8) . . ? C13 C14 C15 120.0(7) . . ? N6 C15 N3 117.1(7) . . ? N6 C15 C14 123.4(7) . . ? N3 C15 C14 119.1(7) . . ? N4 C16 C17 124.4(8) . . ? C18 C17 C16 118.1(8) . . ? C19 C18 C17 119.7(8) . . ? C18 C19 C20 119.4(8) . . ? N4 C20 N5 113.3(7) . . ? N4 C20 C19 121.8(8) . . ? N5 C20 C19 124.8(7) . . ? Cl2 C21 C21 156.5(17) 2_565 2_565 ? Cl2 C21 Cl2 146.6(21) 2_565 . ? C21 C21 Cl2 10.9(8) 2_565 . ? Cl2 C21 Cl3 34.3(10) 2_565 . ? C21 C21 Cl3 125.4(8) 2_565 . ? Cl2 C21 Cl3 114.6(11) . . ? C21 Cl2 Cl3 123.0(15) 2_565 2_565 ? C21 Cl2 C21 12.6(10) 2_565 . ? Cl3 Cl2 C21 112.8(8) 2_565 . ? C21 Cl2 Cl2 22.8(14) 2_565 2_565 ? Cl3 Cl2 Cl2 102.4(4) 2_565 2_565 ? C21 Cl2 Cl2 10.6(7) . 2_565 ? Cl2 Cl3 C21 22.6(6) 2_565 . ? _refine_diff_density_max 1.151 _refine_diff_density_min -1.834 _refine_diff_density_rms 0.204 #===END data_1.CH2Cl2_at_147K _audit_creation_method SHELXL _chemical_formula_sum 'C41 H34 Br2 Cl2 Co3 N12' _chemical_formula_weight 1102.31 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P n n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.849(2) _cell_length_b 13.956(2) _cell_length_c 11.175(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2003.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 19.058 _cell_measurement_theta_max 22.467 _exptl_crystal_description plate _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.827 _exptl_crystal_density_method ? _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 3.405 _exptl_absorpt_correction_type '\s scans' _exptl_absorpt_correction_T_min 0.1302 _exptl_absorpt_correction_T_max 0.1893 _diffrn_ambient_temperature 147(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf Nonius CAD4' _diffrn_measurement_method 'Omega-theta scans' _diffrn_refln_scan_width 0.70 _diffrn_refln_scan_mode_backgd MO _diffrn_standards_number 3 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4708 _diffrn_reflns_av_R_equivalents 0.0491 _diffrn_reflns_av_sigmaI/netI 0.0340 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 26.04 _reflns_number_total 3965 _reflns_number_observed 3676 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 V5' _computing_cell_refinement 'CAD4 V5' _computing_data_reduction 'XCAD4 (Harms, 1993)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0918P)^2^+10.7297P] 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 ? _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 0.12(2) _refine_ls_number_reflns 3963 _refine_ls_number_parameters 281 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_obs 0.0597 _refine_ls_wR_factor_all 0.1746 _refine_ls_wR_factor_obs 0.1659 _refine_ls_goodness_of_fit_all 1.181 _refine_ls_goodness_of_fit_obs 1.190 _refine_ls_restrained_S_all 1.204 _refine_ls_restrained_S_obs 1.190 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.15492(6) 0.91500(5) 0.32319(10) 0.0109(2) Uani 1 d . . Co2 Co 0.0000 1.0000 0.31750(15) 0.0103(3) Uani 1 d S . Br1 Br 0.32805(6) 0.81497(6) 0.32485(11) 0.0372(2) Uani 1 d . . N1 N 0.1137(4) 0.8790(4) 0.4882(5) 0.0134(11) Uani 1 d . . N2 N 0.0708(5) 0.8080(4) 0.2596(6) 0.0163(12) Uani 1 d . . N3 N 0.2209(4) 1.0316(4) 0.3868(5) 0.0125(11) Uani 1 d . . N4 N 0.1743(5) 0.9663(4) 0.1574(6) 0.0141(12) Uani 1 d . . N5 N 0.0514(5) 1.0820(5) 0.1976(6) 0.0116(13) Uani 1 d . . N6 N 0.0557(5) 1.0839(4) 0.4375(6) 0.0115(13) Uani 1 d . . C1 C 0.0116(5) 0.8818(5) 0.5211(6) 0.0131(13) Uani 1 d . . C2 C -0.0170(6) 0.8588(6) 0.6393(7) 0.020(2) Uani 1 d . . H2 H -0.0875(6) 0.8642(6) 0.6643(7) 0.024 Uiso 1 calc R . C3 C 0.0579(7) 0.8286(7) 0.7179(7) 0.028(2) Uani 1 d . . H3 H 0.0384(7) 0.8078(7) 0.7957(7) 0.034 Uiso 1 calc R . C4 C 0.1623(6) 0.8279(7) 0.6850(7) 0.026(2) Uani 1 d . . H4 H 0.2148(6) 0.8095(7) 0.7402(7) 0.032 Uiso 1 calc R . C5 C 0.1874(6) 0.8551(6) 0.5680(7) 0.021(2) Uani 1 d . . H5 H 0.2584(6) 0.8566(6) 0.5444(7) 0.025 Uiso 1 calc R . C6 C -0.0179(6) 0.8245(5) 0.1970(7) 0.0168(14) Uani 1 d . . C7 C -0.0730(6) 0.7467(5) 0.1462(8) 0.023(2) Uani 1 d . . H7 H -0.1334(6) 0.7587(5) 0.0996(8) 0.027 Uiso 1 calc R . C8 C -0.0403(7) 0.6546(6) 0.1632(9) 0.031(2) Uani 1 d . . H8 H -0.0782(7) 0.6025(6) 0.1300(9) 0.038 Uiso 1 calc R . C9 C 0.0491(7) 0.6382(6) 0.2298(11) 0.040(3) Uani 1 d . . H9 H 0.0744(7) 0.5750(6) 0.2417(11) 0.048 Uiso 1 calc R . C10 C 0.1003(6) 0.7158(6) 0.2783(8) 0.027(2) Uani 1 d . . H10 H 0.1593(6) 0.7041(6) 0.3274(8) 0.032 Uiso 1 calc R . C11 C 0.3228(6) 1.0462(6) 0.3755(7) 0.0183(15) Uani 1 d . . H11 H 0.3634(6) 0.9990(6) 0.3360(7) 0.022 Uiso 1 calc R . C12 C 0.3721(6) 1.1268(6) 0.4185(8) 0.023(2) Uani 1 d . . H12 H 0.4453(6) 1.1346(6) 0.4107(8) 0.028 Uiso 1 calc R . C13 C 0.3110(6) 1.1968(6) 0.4741(8) 0.024(2) Uani 1 d . . H13 H 0.3425(6) 1.2529(6) 0.5059(8) 0.029 Uiso 1 calc R . C14 C 0.2065(6) 1.1843(5) 0.4825(7) 0.0195(15) Uani 1 d . . H14 H 0.1646(6) 1.2329(5) 0.5174(7) 0.023 Uiso 1 calc R . C15 C 0.1601(5) 1.1001(5) 0.4399(6) 0.0124(13) Uani 1 d . . C16 C 0.2408(6) 0.9231(5) 0.0804(7) 0.0196(15) Uani 1 d . . H16 H 0.2801(6) 0.8700(5) 0.1087(7) 0.024 Uiso 1 calc R . C17 C 0.2549(7) 0.9519(6) -0.0375(7) 0.026(2) Uani 1 d . . H17 H 0.3017(7) 0.9187(6) -0.0887(7) 0.031 Uiso 1 calc R . C18 C 0.2001(7) 1.0285(6) -0.0777(7) 0.027(2) Uani 1 d . . H18 H 0.2088(7) 1.0499(6) -0.1578(7) 0.033 Uiso 1 calc R . C19 C 0.1314(6) 1.0757(6) -0.0020(7) 0.022(2) Uani 1 d . . H19 H 0.0926(6) 1.1292(6) -0.0301(7) 0.026 Uiso 1 calc R . C20 C 0.1198(5) 1.0437(5) 0.1165(7) 0.0165(14) Uani 1 d . . C21 C -0.0122(16) 0.4669(14) 0.6201(17) 0.029(4) Uiso 0.50 d P . H21A H 0.0488(16) 0.4383(14) 0.6607(17) 0.035 Uiso 0.50 calc PR . H21B H -0.0641(16) 0.4735(14) 0.6851(17) 0.035 Uiso 0.50 calc PR . Cl2 Cl 0.0344(5) 0.5809(5) 0.5919(7) 0.060(2) Uani 0.50 d P . Cl3 Cl -0.0162(4) 0.3925(4) 0.4956(5) 0.0441(11) Uani 0.50 d P . 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 0.0099(4) 0.0102(4) 0.0126(4) -0.0016(5) -0.0001(4) -0.0009(3) Co2 0.0088(5) 0.0108(5) 0.0112(5) 0.000 0.000 -0.0009(4) Br1 0.0352(4) 0.0366(4) 0.0398(5) -0.0023(6) -0.0009(6) 0.0027(3) N1 0.013(3) 0.011(3) 0.017(3) -0.003(2) -0.002(2) 0.001(2) N2 0.009(3) 0.012(3) 0.027(3) -0.003(2) 0.004(2) 0.002(2) N3 0.013(3) 0.016(3) 0.009(3) 0.000(2) 0.002(2) 0.000(2) N4 0.011(3) 0.011(3) 0.020(3) -0.007(2) 0.001(2) -0.004(2) N5 0.007(3) 0.016(3) 0.012(3) -0.001(2) 0.002(3) 0.001(2) N6 0.009(3) 0.008(3) 0.018(3) 0.000(2) 0.001(3) -0.002(2) C1 0.016(3) 0.009(3) 0.015(3) -0.002(2) 0.002(3) 0.001(3) C2 0.017(4) 0.023(4) 0.020(4) 0.004(3) 0.002(3) 0.003(3) C3 0.029(4) 0.040(5) 0.014(4) 0.012(3) -0.001(3) 0.004(4) C4 0.020(4) 0.043(5) 0.016(4) 0.004(3) -0.002(3) 0.007(3) C5 0.018(4) 0.024(4) 0.020(4) 0.002(3) 0.001(3) 0.002(3) C6 0.015(3) 0.017(3) 0.019(3) -0.002(3) 0.002(3) 0.000(3) C7 0.018(4) 0.019(4) 0.032(4) -0.012(3) -0.001(3) -0.002(3) C8 0.023(4) 0.018(4) 0.053(6) -0.008(4) -0.008(4) -0.005(3) C9 0.030(5) 0.012(4) 0.078(8) -0.018(4) -0.020(5) 0.004(3) C10 0.018(4) 0.016(3) 0.047(5) -0.004(3) -0.013(3) 0.000(3) C11 0.013(3) 0.023(4) 0.019(3) 0.000(3) 0.002(3) -0.001(3) C12 0.019(4) 0.023(4) 0.028(4) -0.006(3) -0.004(3) -0.005(3) C13 0.018(4) 0.024(4) 0.031(4) -0.010(3) 0.000(3) -0.008(3) C14 0.018(4) 0.016(3) 0.024(4) -0.003(3) 0.002(3) -0.005(3) C15 0.011(3) 0.015(3) 0.011(3) 0.001(2) 0.000(2) -0.002(3) C16 0.021(4) 0.020(3) 0.018(3) -0.006(3) 0.004(3) -0.002(3) C17 0.027(4) 0.032(4) 0.018(4) -0.010(3) 0.012(3) -0.004(3) C18 0.032(4) 0.037(5) 0.013(3) 0.001(3) 0.001(3) -0.006(4) C19 0.021(4) 0.026(4) 0.019(4) 0.003(3) 0.003(3) -0.001(3) C20 0.013(3) 0.018(3) 0.018(3) 0.003(3) -0.002(3) -0.007(3) Cl2 0.049(3) 0.050(4) 0.080(5) -0.032(4) -0.017(3) 0.015(3) Cl3 0.031(2) 0.053(3) 0.048(3) -0.002(2) -0.006(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 1.968(6) . ? Co1 N2 1.976(6) . ? Co1 N1 1.983(6) . ? Co1 N4 2.002(6) . ? Co1 Co2 2.3182(8) . ? Co1 Br1 2.6263(11) . ? Co2 N5 1.881(7) 2_575 ? Co2 N5 1.881(7) . ? Co2 N6 1.918(7) 2_575 ? Co2 N6 1.919(7) . ? Co2 Co1 2.3182(8) 2_575 ? N1 C5 1.342(10) . ? N1 C1 1.363(9) . ? N2 C6 1.357(10) . ? N2 C10 1.358(10) . ? N3 C11 1.331(9) . ? N3 C15 1.370(9) . ? N4 C16 1.353(10) . ? N4 C20 1.366(10) . ? N5 C20 1.371(10) . ? N5 C6 1.375(10) 2_575 ? N6 C1 1.360(10) 2_575 ? N6 C15 1.361(9) . ? C1 N6 1.360(10) 2_575 ? C1 C2 1.409(10) . ? C2 C3 1.370(11) . ? C3 C4 1.390(12) . ? C4 C5 1.400(11) . ? C6 N5 1.375(10) 2_575 ? C6 C7 1.415(10) . ? C7 C8 1.366(12) . ? C8 C9 1.388(13) . ? C9 C10 1.378(11) . ? C11 C12 1.377(11) . ? C12 C13 1.400(11) . ? C13 C14 1.357(11) . ? C14 C15 1.402(10) . ? C16 C17 1.390(11) . ? C17 C18 1.356(12) . ? C18 C19 1.390(11) . ? C19 C20 1.406(10) . ? C21 Cl2 0.79(2) 2_565 ? C21 C21 0.98(4) 2_565 ? C21 Cl2 1.73(2) . ? C21 Cl3 1.74(2) . ? Cl2 C21 0.79(2) 2_565 ? Cl2 Cl3 1.162(9) 2_565 ? Cl2 Cl2 2.425(15) 2_565 ? Cl3 Cl2 1.162(9) 2_565 ? 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 N3 Co1 N2 172.2(2) . . ? N3 Co1 N1 89.3(2) . . ? N2 Co1 N1 89.8(3) . . ? N3 Co1 N4 89.1(2) . . ? N2 Co1 N4 90.3(3) . . ? N1 Co1 N4 169.9(2) . . ? N3 Co1 Co2 87.5(2) . . ? N2 Co1 Co2 84.7(2) . . ? N1 Co1 Co2 85.8(2) . . ? N4 Co1 Co2 84.2(2) . . ? N3 Co1 Br1 94.1(2) . . ? N2 Co1 Br1 93.7(2) . . ? N1 Co1 Br1 94.9(2) . . ? N4 Co1 Br1 95.2(2) . . ? Co2 Co1 Br1 178.24(5) . . ? N5 Co2 N5 89.2(4) 2_575 . ? N5 Co2 N6 89.7(2) 2_575 2_575 ? N5 Co2 N6 178.5(3) . 2_575 ? N5 Co2 N6 178.5(3) 2_575 . ? N5 Co2 N6 89.7(2) . . ? N6 Co2 N6 91.3(4) 2_575 . ? N5 Co2 Co1 90.6(2) 2_575 . ? N5 Co2 Co1 91.7(2) . . ? N6 Co2 Co1 89.4(2) 2_575 . ? N6 Co2 Co1 88.4(2) . . ? N5 Co2 Co1 91.7(2) 2_575 2_575 ? N5 Co2 Co1 90.6(2) . 2_575 ? N6 Co2 Co1 88.4(2) 2_575 2_575 ? N6 Co2 Co1 89.4(2) . 2_575 ? Co1 Co2 Co1 176.86(10) . 2_575 ? C5 N1 C1 120.5(6) . . ? C5 N1 Co1 119.5(5) . . ? C1 N1 Co1 120.0(5) . . ? C6 N2 C10 118.4(6) . . ? C6 N2 Co1 121.1(5) . . ? C10 N2 Co1 120.6(5) . . ? C11 N3 C15 119.6(6) . . ? C11 N3 Co1 121.1(5) . . ? C15 N3 Co1 119.2(5) . . ? C16 N4 C20 117.6(7) . . ? C16 N4 Co1 120.5(5) . . ? C20 N4 Co1 121.9(5) . . ? C20 N5 C6 124.6(7) . 2_575 ? C20 N5 Co2 117.3(5) . . ? C6 N5 Co2 118.1(5) 2_575 . ? C1 N6 C15 123.7(7) 2_575 . ? C1 N6 Co2 117.2(5) 2_575 . ? C15 N6 Co2 118.9(5) . . ? N6 C1 N1 115.9(6) 2_575 . ? N6 C1 C2 123.9(7) 2_575 . ? N1 C1 C2 119.8(6) . . ? C3 C2 C1 119.2(7) . . ? C2 C3 C4 120.7(7) . . ? C3 C4 C5 117.9(7) . . ? N1 C5 C4 121.7(7) . . ? N2 C6 N5 115.0(6) . 2_575 ? N2 C6 C7 119.8(7) . . ? N5 C6 C7 125.0(7) 2_575 . ? C8 C7 C6 120.8(8) . . ? C7 C8 C9 118.9(8) . . ? C10 C9 C8 118.5(8) . . ? N2 C10 C9 123.4(8) . . ? N3 C11 C12 123.0(7) . . ? C11 C12 C13 117.8(7) . . ? C14 C13 C12 119.8(7) . . ? C13 C14 C15 120.3(7) . . ? N6 C15 N3 116.0(6) . . ? N6 C15 C14 124.4(7) . . ? N3 C15 C14 119.4(6) . . ? N4 C16 C17 123.7(7) . . ? C18 C17 C16 118.3(7) . . ? C17 C18 C19 120.1(7) . . ? C18 C19 C20 119.3(7) . . ? N4 C20 N5 114.6(6) . . ? N4 C20 C19 120.8(7) . . ? N5 C20 C19 124.5(7) . . ? Cl2 C21 C21 156.1(17) 2_565 2_565 ? Cl2 C21 Cl2 145.9(22) 2_565 . ? C21 C21 Cl2 10.7(7) 2_565 . ? Cl2 C21 Cl3 33.5(11) 2_565 . ? C21 C21 Cl3 125.1(9) 2_565 . ? Cl2 C21 Cl3 114.4(12) . . ? C21 Cl2 Cl3 124.5(17) 2_565 2_565 ? C21 Cl2 C21 13.2(11) 2_565 . ? Cl3 Cl2 C21 113.1(8) 2_565 . ? C21 Cl2 Cl2 23.6(16) 2_565 2_565 ? Cl3 Cl2 Cl2 102.9(5) 2_565 2_565 ? C21 Cl2 Cl2 10.5(7) . 2_565 ? Cl2 Cl3 C21 22.1(7) 2_565 . ? _refine_diff_density_max 1.207 _refine_diff_density_min -1.792 _refine_diff_density_rms 0.203 #===END data_1.CH2Cl2_at_240K _audit_creation_method SHELXL _chemical_formula_structural 'Co3(dpa)4Br2 CH2Cl2' _chemical_formula_sum 'C41 H34 Br2 Cl2 Co3 N12' _chemical_formula_weight 1102.31 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.953(1) _cell_length_b 14.055(1) _cell_length_c 11.264(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2050.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 240(2) _cell_measurement_reflns_used 6336 _cell_measurement_theta_min 2.317 _cell_measurement_theta_max 27.449 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.785 _exptl_crystal_density_method ? _exptl_crystal_F_000 1098 _exptl_absorpt_coefficient_mu 3.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8014 _exptl_absorpt_correction_T_max 0.6550 _diffrn_ambient_temperature 240(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12505 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0315 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4575 _reflns_number_observed 3998 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINTPLUS _computing_data_reduction 'SAINTPLUS and SADABS' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0746P)^2^+6.2883P] 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 noref _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 0.12(2) _refine_ls_number_reflns 4575 _refine_ls_number_parameters 281 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_obs 0.0474 _refine_ls_wR_factor_all 0.1436 _refine_ls_wR_factor_obs 0.1370 _refine_ls_goodness_of_fit_all 1.075 _refine_ls_goodness_of_fit_obs 1.101 _refine_ls_restrained_S_all 1.075 _refine_ls_restrained_S_obs 1.101 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.84634(4) 0.08520(4) 0.67721(9) 0.0182(2) Uani 1 d . . Co2 Co 1.0000 0.0000 0.68143(13) 0.0172(2) Uani 1 d S . Br1 Br 0.67224(5) 0.18621(5) 0.67533(9) 0.0455(2) Uani 1 d . . N1 N 0.8875(3) 0.1214(3) 0.5126(4) 0.0215(9) Uani 1 d . . N2 N 0.9309(4) 0.1918(3) 0.7406(4) 0.0231(10) Uani 1 d . . N3 N 0.7815(4) -0.0313(3) 0.6144(4) 0.0200(9) Uani 1 d . . N4 N 0.8273(4) 0.0348(3) 0.8423(4) 0.0213(9) Uani 1 d . . N5 N 0.9479(4) -0.0817(4) 0.8012(5) 0.0205(12) Uani 1 d . . N6 N 0.9458(4) -0.0828(4) 0.5626(5) 0.0207(11) Uani 1 d . . C1 C 0.9887(4) 0.1171(4) 0.4802(5) 0.0214(11) Uani 1 d . . C2 C 1.0170(5) 0.1403(5) 0.3614(6) 0.0332(14) Uani 1 d . . H2 H 1.0860(5) 0.1349(5) 0.3366(6) 0.040 Uiso 1 calc R . C3 C 0.9424(6) 0.1705(6) 0.2836(6) 0.042(2) Uani 1 d . . H3 H 0.9616(6) 0.1912(6) 0.2074(6) 0.051 Uiso 1 calc R . C4 C 0.8396(5) 0.1708(6) 0.3159(6) 0.042(2) Uani 1 d . . H4 H 0.7877(5) 0.1879(6) 0.2615(6) 0.051 Uiso 1 calc R . C5 C 0.8153(5) 0.1447(5) 0.4334(6) 0.0317(14) Uani 1 d . . H5 H 0.7456(5) 0.1436(5) 0.4568(6) 0.038 Uiso 1 calc R . C6 C 1.0189(5) 0.1744(4) 0.8016(5) 0.0242(11) Uani 1 d . . C7 C 1.0738(5) 0.2517(5) 0.8522(7) 0.0344(14) Uani 1 d . . H7 H 1.1332(5) 0.2397(5) 0.8978(7) 0.041 Uiso 1 calc R . C8 C 1.0417(6) 0.3431(5) 0.8359(8) 0.046(2) Uani 1 d . . H8 H 1.0791(6) 0.3941(5) 0.8688(8) 0.055 Uiso 1 calc R . C9 C 0.9528(6) 0.3598(5) 0.7699(9) 0.052(2) Uani 1 d . . H9 H 0.9284(6) 0.4220(5) 0.7581(9) 0.062 Uiso 1 calc R . C10 C 0.9012(5) 0.2830(4) 0.7221(7) 0.036(2) Uani 1 d . . H10 H 0.8429(5) 0.2945(4) 0.6745(7) 0.044 Uiso 1 calc R . C11 C 0.6787(5) -0.0463(5) 0.6255(6) 0.0278(12) Uani 1 d . . H11 H 0.6390(5) 0.0000(5) 0.6648(6) 0.033 Uiso 1 calc R . C12 C 0.6296(5) -0.1254(5) 0.5826(6) 0.0336(14) Uani 1 d . . H12 H 0.5577(5) -0.1324(5) 0.5899(6) 0.040 Uiso 1 calc R . C13 C 0.6893(5) -0.1954(5) 0.5276(7) 0.0359(15) Uani 1 d . . H13 H 0.6581(5) -0.2508(5) 0.4977(7) 0.043 Uiso 1 calc R . C14 C 0.7936(5) -0.1824(4) 0.5178(6) 0.0318(14) Uani 1 d . . H14 H 0.8343(5) -0.2297(4) 0.4819(6) 0.038 Uiso 1 calc R . C15 C 0.8407(4) -0.0989(4) 0.5608(5) 0.0217(11) Uani 1 d . . C16 C 0.7631(5) 0.0784(4) 0.9198(6) 0.0285(12) Uani 1 d . . H16 H 0.7258(5) 0.1316(4) 0.8931(6) 0.034 Uiso 1 calc R . C17 C 0.7491(6) 0.0490(5) 1.0367(6) 0.040(2) Uani 1 d . . H17 H 0.7035(6) 0.0815(5) 1.0874(6) 0.048 Uiso 1 calc R . C18 C 0.8034(6) -0.0283(6) 1.0758(6) 0.040(2) Uani 1 d . . H18 H 0.7955(6) -0.0494(6) 1.1545(6) 0.048 Uiso 1 calc R . C19 C 0.8695(5) -0.0751(5) 1.0003(5) 0.0322(14) Uani 1 d . . H19 H 0.9070(5) -0.1279(5) 1.0278(5) 0.039 Uiso 1 calc R . C20 C 0.8812(4) -0.0445(4) 0.8820(5) 0.0229(11) Uani 1 d . . C21 C 1.0112(15) 0.5308(11) 0.3777(16) 0.045(4) Uiso 0.50 d P . H21A H 1.0623(15) 0.5250(11) 0.3139(16) 0.054 Uiso 0.50 calc PR . H21B H 0.9513(15) 0.5594(11) 0.3384(16) 0.054 Uiso 0.50 calc PR . Cl2 Cl 0.9652(6) 0.4192(6) 0.4096(9) 0.102(2) Uani 0.50 d P . Cl3 Cl 1.0162(4) 0.6064(5) 0.5022(7) 0.081(2) Uani 0.50 d P . 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 0.0158(3) 0.0173(3) 0.0214(3) -0.0019(4) -0.0002(4) -0.0009(2) Co2 0.0139(4) 0.0165(4) 0.0213(4) 0.000 0.000 -0.0006(3) Br1 0.0398(3) 0.0462(4) 0.0506(4) -0.0018(5) -0.0011(5) 0.0052(2) N1 0.020(2) 0.023(2) 0.022(2) 0.000(2) -0.001(2) 0.002(2) N2 0.017(2) 0.020(2) 0.032(3) -0.003(2) 0.002(2) 0.000(2) N3 0.017(2) 0.023(2) 0.020(2) -0.004(2) 0.001(2) -0.001(2) N4 0.016(2) 0.019(2) 0.029(2) -0.004(2) 0.000(2) -0.003(2) N5 0.019(3) 0.018(3) 0.024(3) 0.002(2) 0.003(2) -0.001(2) N6 0.017(3) 0.019(3) 0.027(3) -0.003(2) -0.002(2) -0.002(2) C1 0.023(3) 0.016(2) 0.025(3) 0.000(2) 0.001(2) 0.001(2) C2 0.025(3) 0.047(4) 0.028(3) 0.008(3) 0.004(3) 0.003(3) C3 0.038(4) 0.061(5) 0.027(3) 0.015(3) 0.000(3) 0.008(3) C4 0.030(3) 0.073(5) 0.023(3) 0.012(3) -0.003(3) 0.011(3) C5 0.025(3) 0.042(4) 0.028(3) 0.004(3) 0.001(3) 0.005(3) C6 0.021(3) 0.022(3) 0.029(3) -0.005(2) 0.003(2) -0.002(2) C7 0.025(3) 0.029(3) 0.049(4) -0.011(3) -0.006(3) -0.004(2) C8 0.038(4) 0.029(3) 0.071(5) -0.007(3) -0.016(4) -0.009(3) C9 0.040(4) 0.018(3) 0.099(7) -0.007(4) -0.019(4) 0.005(3) C10 0.023(3) 0.021(3) 0.065(4) -0.002(3) -0.015(3) 0.001(2) C11 0.018(3) 0.030(3) 0.035(3) -0.008(2) 0.005(2) -0.002(2) C12 0.019(3) 0.036(3) 0.046(4) -0.009(3) 0.001(3) -0.008(2) C13 0.022(3) 0.035(3) 0.050(4) -0.017(3) -0.003(3) -0.009(3) C14 0.027(3) 0.028(3) 0.041(3) -0.013(3) 0.002(3) -0.002(2) C15 0.018(3) 0.023(3) 0.025(3) -0.001(2) -0.001(2) -0.002(2) C16 0.028(3) 0.027(3) 0.030(3) -0.005(2) 0.001(3) 0.001(2) C17 0.043(4) 0.047(4) 0.030(3) -0.009(3) 0.015(3) 0.000(3) C18 0.046(4) 0.052(4) 0.022(3) 0.004(3) 0.007(3) -0.003(3) C19 0.033(3) 0.038(3) 0.026(3) 0.006(3) 0.003(3) 0.003(3) C20 0.019(3) 0.025(3) 0.025(3) 0.005(2) 0.001(2) -0.005(2) Cl2 0.088(5) 0.091(5) 0.127(7) -0.044(5) -0.029(5) 0.025(4) Cl3 0.054(3) 0.098(4) 0.090(4) -0.004(4) -0.012(3) 0.000(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.3234(6) . y Co2 Co1 2.3234(6) 2_755 y Co1 Br1 2.6648(9) . y Co1 N1 1.995(5) . y Co1 N2 1.988(5) . y Co1 N3 1.972(5) . y Co1 N4 2.005(5) . y Co2 N5 1.896(6) 2_755 ? Co2 N5 1.896(6) . y Co2 N6 1.908(6) . y Co2 N6 1.908(6) 2_755 ? N1 C5 1.333(8) . ? N1 C1 1.362(7) . ? N2 C6 1.354(8) . ? N2 C10 1.355(8) . ? N3 C11 1.354(7) . ? N3 C15 1.362(7) . ? N4 C16 1.353(8) . ? N4 C20 1.388(7) . ? N5 C20 1.360(8) . ? N5 C6 1.371(8) 2_755 ? N6 C1 1.347(8) 2_755 ? N6 C15 1.380(8) . ? C1 N6 1.347(8) 2_755 ? C1 C2 1.425(8) . ? C2 C3 1.370(10) . ? C3 C4 1.381(10) . ? C4 C5 1.410(9) . ? C6 N5 1.371(8) 2_755 ? C6 C7 1.418(8) . ? C7 C8 1.362(10) . ? C8 C9 1.391(11) . ? C9 C10 1.379(10) . ? C11 C12 1.369(9) . ? C12 C13 1.396(9) . ? C13 C14 1.368(9) . ? C14 C15 1.409(8) . ? C16 C17 1.391(9) . ? C17 C18 1.367(11) . ? C18 C19 1.375(9) . ? C19 C20 1.408(8) . ? C21 Cl2 0.85(2) 2_765 ? C21 C21 0.91(3) 2_765 ? C21 Cl2 1.72(2) . ? C21 Cl3 1.76(2) . ? Cl2 C21 0.85(2) 2_765 ? Cl2 Cl3 1.129(10) 2_765 ? Cl2 Cl2 2.44(2) 2_765 ? Cl3 Cl2 1.129(10) 2_765 ? 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 Co1 Co2 Co1 177.66(9) 2_755 . y Co2 Co1 Br1 178.64(4) . . y N2 Co1 N1 89.7(2) . . y N3 Co1 N1 89.5(2) . . y N1 Co1 N4 170.0(2) . . y N3 Co1 N4 89.3(2) . . y N3 Co1 N2 171.6(2) . . y N2 Co1 N4 90.1(2) . . y N3 Co1 Co2 86.81(14) . . ? N2 Co1 Co2 84.78(14) . . ? N1 Co1 Co2 85.50(14) . . ? N4 Co1 Co2 84.49(14) . . ? N1 Co1 Br1 94.75(14) . . y N2 Co1 Br1 93.88(14) . . y N3 Co1 Br1 94.52(14) . . y N4 Co1 Br1 95.27(14) . . y N5 Co2 N5 89.3(3) 2_755 . y N5 Co2 N6 179.1(3) 2_755 . y N5 Co2 N6 89.9(2) . . y N5 Co2 N6 89.9(2) 2_755 2_755 y N5 Co2 N6 179.1(3) . 2_755 y N6 Co2 N6 90.9(4) . 2_755 y N5 Co2 Co1 91.2(2) 2_755 2_755 ? N5 Co2 Co1 90.4(2) . 2_755 ? N6 Co2 Co1 89.2(2) . 2_755 ? N6 Co2 Co1 89.1(2) 2_755 2_755 ? N5 Co2 Co1 90.4(2) 2_755 . ? N5 Co2 Co1 91.2(2) . . ? N6 Co2 Co1 89.1(2) . . ? N6 Co2 Co1 89.2(2) 2_755 . ? C5 N1 C1 120.4(5) . . ? C5 N1 Co1 119.8(4) . . ? C1 N1 Co1 119.7(4) . . ? C6 N2 C10 119.2(5) . . ? C6 N2 Co1 120.7(4) . . ? C10 N2 Co1 120.1(4) . . ? C11 N3 C15 119.1(5) . . ? C11 N3 Co1 121.0(4) . . ? C15 N3 Co1 119.9(4) . . ? C16 N4 C20 117.7(5) . . ? C16 N4 Co1 120.9(4) . . ? C20 N4 Co1 121.4(4) . . ? C20 N5 C6 124.2(5) . 2_755 ? C20 N5 Co2 118.0(4) . . ? C6 N5 Co2 117.8(4) 2_755 . ? C1 N6 C15 123.6(5) 2_755 . ? C1 N6 Co2 118.0(4) 2_755 . ? C15 N6 Co2 118.2(4) . . ? N6 C1 N1 115.9(5) 2_755 . ? N6 C1 C2 124.5(6) 2_755 . ? N1 C1 C2 119.3(5) . . ? C3 C2 C1 119.3(6) . . ? C2 C3 C4 120.9(6) . . ? C3 C4 C5 117.5(6) . . ? N1 C5 C4 122.4(6) . . ? N2 C6 N5 115.7(5) . 2_755 ? N2 C6 C7 119.1(5) . . ? N5 C6 C7 124.9(6) 2_755 . ? C8 C7 C6 121.1(7) . . ? C7 C8 C9 118.9(6) . . ? C10 C9 C8 118.6(6) . . ? N2 C10 C9 122.9(6) . . ? N3 C11 C12 123.4(6) . . ? C11 C12 C13 118.2(6) . . ? C14 C13 C12 119.3(6) . . ? C13 C14 C15 120.7(6) . . ? N3 C15 N6 115.8(5) . . ? N3 C15 C14 119.3(5) . . ? N6 C15 C14 124.6(5) . . ? N4 C16 C17 123.8(6) . . ? C18 C17 C16 118.3(6) . . ? C17 C18 C19 120.1(6) . . ? C18 C19 C20 120.4(6) . . ? N5 C20 N4 114.3(5) . . ? N5 C20 C19 125.7(6) . . ? N4 C20 C19 119.7(6) . . ? Cl2 C21 C21 154.5(16) 2_765 2_765 ? Cl2 C21 Cl2 142.7(20) 2_765 . ? C21 C21 Cl2 12.3(8) 2_765 . ? Cl2 C21 Cl3 31.5(10) 2_765 . ? C21 C21 Cl3 125.7(8) 2_765 . ? Cl2 C21 Cl3 113.4(11) . . ? C21 Cl2 Cl3 125.4(16) 2_765 2_765 ? C21 Cl2 C21 13.2(9) 2_765 . ? Cl3 Cl2 C21 114.2(9) 2_765 . ? C21 Cl2 Cl2 25.2(14) 2_765 2_765 ? Cl3 Cl2 Cl2 102.5(6) 2_765 2_765 ? C21 Cl2 Cl2 12.1(7) . 2_765 ? Cl2 Cl3 C21 23.1(7) 2_765 . ? _refine_diff_density_max 0.837 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.135 #===END data_1.C6H12_at_110K _audit_creation_method SHELXL _chemical_formula_structural 'Co3dpa4Cl2.C6H12' _chemical_formula_sum 'C46 H44 Br2 Co3 N12' _chemical_formula_weight 1101.54 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 '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 1 2/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 12.9949(5) _cell_length_b 11.5683(5) _cell_length_c 14.2818(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.2290(10) _cell_angle_gamma 90.00 _cell_volume 2141.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8040 _cell_measurement_theta_min 2.268 _cell_measurement_theta_max 27.506 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.709 _exptl_crystal_density_method ? _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 3.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4156 _exptl_absorpt_correction_T_max 0.4915 _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13310 _diffrn_reflns_av_R_equivalents 0.0155 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4862 _reflns_number_observed 4141 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+1.3724P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4862 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_obs 0.0242 _refine_ls_wR_factor_all 0.0629 _refine_ls_wR_factor_obs 0.0604 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.104 _refine_ls_shift/esd_max -0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.89775(2) 0.18475(2) 0.16833(2) 0.01186(7) Uani 1 d . . Br1 Br 1.065893(14) 0.18477(2) 0.077424(13) 0.01741(6) Uani 1 d . . N1 N 0.80583(11) 0.12818(13) 0.06096(11) 0.0142(3) Uani 1 d . . C1 C 0.82805(14) 0.1475(2) -0.02833(13) 0.0171(4) Uani 1 d . . H1A H 0.88935(14) 0.1889(2) -0.03872(13) 0.021 Uiso 1 calc R . Co2 Co 0.7500 0.18474(3) 0.2500 0.01188(8) Uani 1 d S . N2 N 0.69190(11) 0.06967(13) 0.16774(10) 0.0143(3) Uani 1 d . . C2 C 0.7668(2) 0.1107(2) -0.10545(13) 0.0205(4) Uani 1 d . . H2A H 0.7857(2) 0.1258(2) -0.16726(13) 0.025 Uiso 1 calc R . N3 N 0.58633(11) 0.02263(13) 0.28481(10) 0.0140(3) Uani 1 d . . C3 C 0.6767(2) 0.0511(2) -0.09073(14) 0.0219(4) Uani 1 d . . H3A H 0.6332(2) 0.0240(2) -0.14244(14) 0.026 Uiso 1 calc R . N4 N 0.85699(12) 0.34625(13) 0.13352(11) 0.0139(3) Uani 1 d . . C4 C 0.65145(15) 0.0319(2) -0.00033(13) 0.0191(4) Uani 1 d . . H4A H 0.59002(15) -0.0089(2) 0.01060(13) 0.023 Uiso 1 calc R . N5 N 0.69147(12) 0.30067(13) 0.16939(11) 0.0140(3) Uani 1 d . . C5 C 0.71602(14) 0.0722(2) 0.07617(12) 0.0145(4) Uani 1 d . . N6 N 0.53201(12) 0.24127(13) 0.21206(10) 0.0140(3) Uani 1 d . . C6 C 0.63044(14) -0.0111(2) 0.20508(13) 0.0151(4) Uani 1 d . . C7 C 0.6198(2) -0.1258(2) 0.17241(14) 0.0213(4) Uani 1 d . . H7A H 0.6487(2) -0.1482(2) 0.11593(14) 0.026 Uiso 1 calc R . C8 C 0.5678(2) -0.2049(2) 0.2225(2) 0.0259(5) Uani 1 d . . H8A H 0.5597(2) -0.2822(2) 0.2007(2) 0.031 Uiso 1 calc R . C9 C 0.5268(2) -0.1714(2) 0.30550(15) 0.0234(4) Uani 1 d . . H9A H 0.4917(2) -0.2255(2) 0.34175(15) 0.028 Uiso 1 calc R . C10 C 0.53801(14) -0.0581(2) 0.33409(13) 0.0182(4) Uani 1 d . . H10A H 0.51049(14) -0.0356(2) 0.39115(13) 0.022 Uiso 1 calc R . C11 C 0.92754(14) 0.4256(2) 0.11045(13) 0.0170(4) Uani 1 d . . H11A H 0.99767(14) 0.4023(2) 0.11059(13) 0.020 Uiso 1 calc R . C12 C 0.90294(15) 0.5382(2) 0.08680(14) 0.0197(4) Uani 1 d . . H12A H 0.95449(15) 0.5902(2) 0.06883(14) 0.024 Uiso 1 calc R . C13 C 0.8013(2) 0.5741(2) 0.08977(14) 0.0222(4) Uani 1 d . . H13A H 0.7823(2) 0.6515(2) 0.07440(14) 0.027 Uiso 1 calc R . C14 C 0.72841(15) 0.4961(2) 0.11525(14) 0.0196(4) Uani 1 d . . H14A H 0.65880(15) 0.5199(2) 0.11848(14) 0.024 Uiso 1 calc R . C15 C 0.75678(14) 0.3812(2) 0.13654(12) 0.0148(4) Uani 1 d . . C16 C 0.58717(14) 0.2970(2) 0.14780(13) 0.0146(4) Uani 1 d . . C17 C 0.5380(2) 0.3351(2) 0.06218(14) 0.0197(4) Uani 1 d . . H17A H 0.5761(2) 0.3758(2) 0.01845(14) 0.024 Uiso 1 calc R . C18 C 0.4349(2) 0.3134(2) 0.04199(14) 0.0217(4) Uani 1 d . . H18A H 0.4017(2) 0.3388(2) -0.01582(14) 0.026 Uiso 1 calc R . C19 C 0.37912(15) 0.2540(2) 0.10635(14) 0.0202(4) Uani 1 d . . H19A H 0.30787(15) 0.2376(2) 0.09326(14) 0.024 Uiso 1 calc R . C20 C 0.43051(14) 0.2198(2) 0.18953(14) 0.0171(4) Uani 1 d . . H20A H 0.39289(14) 0.1789(2) 0.23353(14) 0.021 Uiso 1 calc R . C21 C 0.8687(3) 0.4729(5) 0.7440(3) 0.0270(13) Uiso 0.523(9) d P 1 H21A H 0.9377(3) 0.4403(5) 0.7350(3) 0.032 Uiso 0.523(9) calc PR 1 H21B H 0.8758(3) 0.5577(5) 0.7514(3) 0.032 Uiso 0.523(9) calc PR 1 C22 C 0.8264(4) 0.4209(5) 0.8313(3) 0.0319(13) Uiso 0.523(9) d P 1 H22A H 0.8662(4) 0.4522(5) 0.8874(3) 0.038 Uiso 0.523(9) calc PR 1 H22B H 0.8377(4) 0.3362(5) 0.8305(3) 0.038 Uiso 0.523(9) calc PR 1 C21' C 0.8490(5) 0.4155(7) 0.7509(4) 0.041(2) Uiso 0.477(9) d P 2 H21C H 0.9223(5) 0.4385(7) 0.7494(4) 0.050 Uiso 0.477(9) calc PR 2 H21D H 0.8472(5) 0.3305(7) 0.7584(4) 0.050 Uiso 0.477(9) calc PR 2 C22' C 0.8060(5) 0.4708(7) 0.8373(4) 0.041(2) Uiso 0.477(9) d P 2 H22C H 0.8449(5) 0.4420(7) 0.8948(4) 0.050 Uiso 0.477(9) calc PR 2 H22D H 0.8148(5) 0.5557(7) 0.8348(4) 0.050 Uiso 0.477(9) calc PR 2 C23 C 0.7052(2) 0.4454(3) 0.8409(2) 0.0451(6) Uiso 1 d . . H23A H 0.6772(2) 0.3766(3) 0.8716(2) 0.054 Uiso 1 calc R 1 H23B H 0.7009(2) 0.5105(3) 0.8854(2) 0.054 Uiso 1 calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01144(12) 0.01159(12) 0.01263(13) 0.00018(9) 0.00139(9) -0.00020(9) Br1 0.01459(10) 0.01913(10) 0.01904(10) 0.00029(7) 0.00477(7) -0.00016(7) N1 0.0138(7) 0.0135(7) 0.0154(7) -0.0005(6) 0.0020(6) 0.0009(6) C1 0.0161(9) 0.0195(9) 0.0161(9) 0.0014(7) 0.0034(7) 0.0006(7) Co2 0.0108(2) 0.0119(2) 0.0131(2) 0.000 0.00171(12) 0.000 N2 0.0139(7) 0.0145(7) 0.0147(7) -0.0007(6) 0.0023(6) -0.0016(6) C2 0.0225(10) 0.0258(10) 0.0134(9) 0.0004(8) 0.0024(7) 0.0005(8) N3 0.0131(7) 0.0141(7) 0.0149(8) 0.0003(6) 0.0013(6) 0.0004(6) C3 0.0230(10) 0.0247(10) 0.0174(10) -0.0023(8) -0.0034(8) -0.0018(8) N4 0.0131(7) 0.0148(7) 0.0136(7) -0.0004(6) 0.0008(6) -0.0011(6) C4 0.0162(9) 0.0210(10) 0.0202(10) -0.0013(8) 0.0012(7) -0.0036(7) N5 0.0120(7) 0.0146(7) 0.0155(7) 0.0003(6) 0.0013(6) -0.0007(6) C5 0.0158(9) 0.0124(8) 0.0155(9) -0.0003(7) 0.0025(7) 0.0020(7) N6 0.0136(7) 0.0131(7) 0.0154(8) -0.0015(6) 0.0012(6) 0.0006(6) C6 0.0125(8) 0.0166(9) 0.0161(9) 0.0009(7) 0.0009(7) 0.0001(7) C7 0.0255(10) 0.0179(10) 0.0213(10) -0.0046(8) 0.0080(8) -0.0024(8) C8 0.0327(12) 0.0162(10) 0.0299(12) -0.0056(8) 0.0108(9) -0.0058(8) C9 0.0279(11) 0.0178(10) 0.0258(11) 0.0024(8) 0.0108(9) -0.0041(8) C10 0.0171(9) 0.0187(9) 0.0194(9) 0.0010(7) 0.0058(7) -0.0006(7) C11 0.0146(9) 0.0188(9) 0.0179(9) -0.0007(7) 0.0023(7) -0.0025(7) C12 0.0193(9) 0.0177(9) 0.0222(10) 0.0031(8) 0.0020(8) -0.0045(7) C13 0.0238(10) 0.0148(9) 0.0276(11) 0.0048(8) -0.0007(8) -0.0003(8) C14 0.0147(9) 0.0178(9) 0.0261(10) 0.0029(8) 0.0006(7) 0.0025(7) C15 0.0152(9) 0.0167(9) 0.0126(8) 0.0009(7) 0.0007(7) -0.0013(7) C16 0.0135(8) 0.0131(9) 0.0172(9) -0.0016(7) 0.0012(7) 0.0011(7) C17 0.0194(9) 0.0203(10) 0.0192(10) 0.0040(7) 0.0001(7) -0.0019(7) C18 0.0197(10) 0.0237(10) 0.0208(10) 0.0033(8) -0.0037(8) 0.0008(8) C19 0.0136(9) 0.0205(10) 0.0259(10) -0.0020(8) -0.0015(7) -0.0007(7) C20 0.0153(9) 0.0156(9) 0.0206(10) -0.0020(7) 0.0027(7) -0.0019(7) _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 Co2 2.3188(2) . y Co2 Co1 2.3189(2) 2_655 y Co1 Br1 2.6227(3) . y Co1 N1 1.984(2) . y Co1 N3 1.9969(15) 2_655 y Co1 N4 1.995(2) . y Co1 N6 1.987(2) 2_655 y N1 C1 1.347(2) . ? N1 C5 1.366(2) . ? C1 C2 1.378(3) . ? Co2 N2 1.895(2) 2_655 y Co2 N2 1.895(2) . y Co2 N5 1.890(2) . y Co2 N5 1.890(2) 2_655 y N2 C6 1.363(2) . ? N2 C5 1.367(2) . ? C2 C3 1.387(3) . ? N3 C10 1.351(2) . ? N3 C6 1.369(2) . ? N3 Co1 1.9970(15) 2_655 ? C3 C4 1.374(3) . ? N4 C11 1.355(2) . ? N4 C15 1.367(2) . ? C4 C5 1.407(3) . ? N5 C15 1.366(2) . ? N5 C16 1.368(2) . ? N6 C20 1.357(2) . ? N6 C16 1.367(2) . ? N6 Co1 1.987(2) 2_655 ? C6 C7 1.410(3) . ? C7 C8 1.371(3) . ? C8 C9 1.389(3) . ? C9 C10 1.377(3) . ? C11 C12 1.377(3) . ? C12 C13 1.389(3) . ? C13 C14 1.376(3) . ? C14 C15 1.407(3) . ? C16 C17 1.408(3) . ? C17 C18 1.373(3) . ? C18 C19 1.393(3) . ? C19 C20 1.377(3) . ? C21 C22 1.523(7) . ? C21 C23 1.524(5) 2_656 ? C22 C23 1.616(6) . ? C21' C23 1.483(6) 2_656 ? C21' C22' 1.532(9) . ? C22' C23 1.346(6) . ? C23 C21' 1.483(6) 2_656 ? C23 C21 1.524(5) 2_656 ? 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 Co1 Co2 Co1 180.00(2) . 2_655 y Co2 Co1 Br1 179.475(11) . . y N1 Co1 N6 170.11(6) . 2_655 y N1 Co1 N3 89.48(6) . 2_655 y N1 Co1 N4 89.00(6) . . y N4 Co1 N3 169.16(6) . 2_655 y N6 Co1 N3 89.50(6) 2_655 2_655 y N6 Co1 N4 90.16(6) 2_655 . y N1 Co1 Co2 85.13(4) . . ? N6 Co1 Co2 84.98(4) 2_655 . ? N4 Co1 Co2 84.89(4) . . ? N3 Co1 Co2 84.29(4) 2_655 . ? N1 Co1 Br1 95.36(4) . . y N3 Co1 Br1 95.54(4) 2_655 . y N4 Co1 Br1 95.29(4) . . y N6 Co1 Br1 94.53(4) 2_655 . y C1 N1 C5 118.3(2) . . ? C1 N1 Co1 121.20(13) . . ? C5 N1 Co1 120.41(12) . . ? N1 C1 C2 123.6(2) . . ? N2 Co2 N2 90.76(9) 2_655 . y N5 Co2 N2 179.21(6) . 2_655 y N5 Co2 N2 89.81(7) 2_655 2_655 y N5 Co2 N2 89.82(7) . . y N5 Co2 N2 179.21(7) 2_655 . y N5 Co2 N5 89.62(9) . 2_655 y N5 Co2 Co1 90.26(5) . . ? N5 Co2 Co1 89.74(5) 2_655 . ? N2 Co2 Co1 90.29(4) 2_655 . ? N2 Co2 Co1 89.71(4) . . ? N5 Co2 Co1 89.74(5) . 2_655 ? N5 Co2 Co1 90.26(5) 2_655 2_655 ? N2 Co2 Co1 89.71(4) 2_655 2_655 ? N2 Co2 Co1 90.29(4) . 2_655 ? C6 N2 C5 124.8(2) . . ? C6 N2 Co2 117.20(12) . . ? C5 N2 Co2 117.96(12) . . ? C1 C2 C3 118.5(2) . . ? C10 N3 C6 118.4(2) . . ? C10 N3 Co1 120.98(12) . 2_655 ? C6 N3 Co1 120.48(12) . 2_655 ? C4 C3 C2 119.1(2) . . ? C11 N4 C15 118.1(2) . . ? C11 N4 Co1 121.54(12) . . ? C15 N4 Co1 120.33(12) . . ? C3 C4 C5 120.4(2) . . ? C15 N5 C16 125.0(2) . . ? C15 N5 Co2 117.42(12) . . ? C16 N5 Co2 117.56(12) . . ? N1 C5 N2 114.9(2) . . ? N1 C5 C4 120.1(2) . . ? N2 C5 C4 124.7(2) . . ? C20 N6 C16 118.4(2) . . ? C20 N6 Co1 121.34(13) . 2_655 ? C16 N6 Co1 120.13(12) . 2_655 ? N2 C6 N3 115.0(2) . . ? N2 C6 C7 124.2(2) . . ? N3 C6 C7 120.5(2) . . ? C8 C7 C6 119.7(2) . . ? C7 C8 C9 119.6(2) . . ? C10 C9 C8 118.6(2) . . ? N3 C10 C9 123.1(2) . . ? N4 C11 C12 123.5(2) . . ? C11 C12 C13 118.7(2) . . ? C14 C13 C12 119.1(2) . . ? C13 C14 C15 120.2(2) . . ? N5 C15 N4 115.3(2) . . ? N5 C15 C14 124.0(2) . . ? N4 C15 C14 120.5(2) . . ? N6 C16 N5 115.0(2) . . ? N6 C16 C17 120.3(2) . . ? N5 C16 C17 124.4(2) . . ? C18 C17 C16 119.9(2) . . ? C17 C18 C19 119.9(2) . . ? C20 C19 C18 117.9(2) . . ? N6 C20 C19 123.6(2) . . ? C22 C21 C23 108.9(4) . 2_656 ? C21 C22 C23 114.4(4) . . ? C23 C21' C22' 116.0(5) 2_656 . ? C23 C22' C21' 110.7(5) . . ? C22' C23 C21' 114.6(4) . 2_656 ? C21 C23 C22 122.0(3) 2_656 . ? _refine_diff_density_max 0.561 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.066 #===END data_1.C6H12_at_150K _audit_creation_method SHELXL _chemical_formula_structural 'Co3dpa4Br2.C6H12' _chemical_formula_sum 'C46 H44 Br2 Co3 N12' _chemical_formula_weight 1101.54 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 '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 1 2/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.0105(7) _cell_length_b 11.5955(6) _cell_length_c 14.3119(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.178(1) _cell_angle_gamma 90.00 _cell_volume 2153.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7582 _cell_measurement_theta_min 2.196 _cell_measurement_theta_max 27.544 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.699 _exptl_crystal_density_method ? _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 3.048 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4276 _exptl_absorpt_correction_T_max 0.5332 _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13174 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4923 _reflns_number_observed 4036 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+1.0649P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4923 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_obs 0.0252 _refine_ls_wR_factor_all 0.0679 _refine_ls_wR_factor_obs 0.0643 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.093 _refine_ls_restrained_S_all 1.039 _refine_ls_restrained_S_obs 1.093 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.89804(2) 0.18495(2) 0.16814(2) 0.01500(7) Uani 1 d . . Br1 Br 1.065726(14) 0.18509(2) 0.077428(14) 0.02174(6) Uani 1 d . . N1 N 0.80541(11) 0.12832(14) 0.06088(11) 0.0165(3) Uani 1 d . . C1 C 0.8275(2) 0.1472(2) -0.02839(13) 0.0208(4) Uani 1 d . . H1A H 0.8888(2) 0.1882(2) -0.03905(13) 0.025 Uiso 1 calc R . Co2 Co 0.7500 0.18506(3) 0.2500 0.01375(8) Uani 1 d S . N2 N 0.69206(11) 0.07005(13) 0.16791(11) 0.0163(3) Uani 1 d . . C2 C 0.7663(2) 0.1103(2) -0.10474(14) 0.0259(4) Uani 1 d . . H2A H 0.7851(2) 0.1251(2) -0.16651(14) 0.031 Uiso 1 calc R . N3 N 0.58652(12) 0.02263(13) 0.28451(11) 0.0168(3) Uani 1 d . . C3 C 0.6764(2) 0.0511(2) -0.08978(14) 0.0265(4) Uani 1 d . . H3A H 0.6327(2) 0.0241(2) -0.14126(14) 0.032 Uiso 1 calc R . N4 N 0.85656(12) 0.34685(13) 0.13365(11) 0.0164(3) Uani 1 d . . C4 C 0.6513(2) 0.0322(2) 0.00029(14) 0.0230(4) Uani 1 d . . H4A H 0.5900(2) -0.0085(2) 0.01131(14) 0.028 Uiso 1 calc R . N5 N 0.69151(12) 0.30080(13) 0.16960(11) 0.0162(3) Uani 1 d . . C5 C 0.71568(14) 0.0724(2) 0.07650(13) 0.0164(4) Uani 1 d . . N6 N 0.53211(12) 0.24157(13) 0.21181(11) 0.0165(3) Uani 1 d . . C6 C 0.63081(14) -0.0109(2) 0.20527(13) 0.0173(4) Uani 1 d . . C7 C 0.6209(2) -0.1254(2) 0.17282(15) 0.0254(4) Uani 1 d . . H7A H 0.6499(2) -0.1476(2) 0.11656(15) 0.030 Uiso 1 calc R . C8 C 0.5690(2) -0.2045(2) 0.2228(2) 0.0315(5) Uani 1 d . . H8A H 0.5616(2) -0.2817(2) 0.2013(2) 0.038 Uiso 1 calc R . C9 C 0.5274(2) -0.1707(2) 0.3053(2) 0.0290(5) Uani 1 d . . H9A H 0.4920(2) -0.2246(2) 0.3412(2) 0.035 Uiso 1 calc R . C10 C 0.53846(15) -0.0581(2) 0.33389(14) 0.0218(4) Uani 1 d . . H10A H 0.51109(15) -0.0358(2) 0.39094(14) 0.026 Uiso 1 calc R . C11 C 0.92678(15) 0.4259(2) 0.11018(14) 0.0206(4) Uani 1 d . . H11A H 0.99673(15) 0.4026(2) 0.10966(14) 0.025 Uiso 1 calc R . C12 C 0.9023(2) 0.5380(2) 0.08710(15) 0.0247(4) Uani 1 d . . H12A H 0.9537(2) 0.5900(2) 0.06927(15) 0.030 Uiso 1 calc R . C13 C 0.8006(2) 0.5739(2) 0.0903(2) 0.0274(5) Uani 1 d . . H13A H 0.7816(2) 0.6512(2) 0.0751(2) 0.033 Uiso 1 calc R . C14 C 0.7281(2) 0.4962(2) 0.11576(15) 0.0233(4) Uani 1 d . . H14A H 0.6586(2) 0.5199(2) 0.11929(15) 0.028 Uiso 1 calc R . C15 C 0.75651(14) 0.3813(2) 0.13663(13) 0.0169(4) Uani 1 d . . C16 C 0.58743(14) 0.2969(2) 0.14797(13) 0.0167(4) Uani 1 d . . C17 C 0.5387(2) 0.3352(2) 0.06226(15) 0.0239(4) Uani 1 d . . H17A H 0.5770(2) 0.3757(2) 0.01871(15) 0.029 Uiso 1 calc R . C18 C 0.4355(2) 0.3136(2) 0.0420(2) 0.0264(5) Uani 1 d . . H18A H 0.4024(2) 0.3389(2) -0.0157(2) 0.032 Uiso 1 calc R . C19 C 0.37989(15) 0.2545(2) 0.10614(15) 0.0243(4) Uani 1 d . . H19A H 0.30873(15) 0.2383(2) 0.09305(15) 0.029 Uiso 1 calc R . C20 C 0.43096(15) 0.2202(2) 0.18925(14) 0.0210(4) Uani 1 d . . H20A H 0.39322(15) 0.1795(2) 0.23306(14) 0.025 Uiso 1 calc R . C21 C 0.8674(4) 0.4720(6) 0.7436(3) 0.0355(15) Uiso 0.538(11) d P 1 H21A H 0.9363(4) 0.4395(6) 0.7342(3) 0.043 Uiso 0.538(11) calc PR 1 H21B H 0.8745(4) 0.5565(6) 0.7512(3) 0.043 Uiso 0.538(11) calc PR 1 C22 C 0.8261(4) 0.4200(6) 0.8305(4) 0.041(2) Uiso 0.538(11) d P 1 H22A H 0.8664(4) 0.4507(6) 0.8864(4) 0.049 Uiso 0.538(11) calc PR 1 H22B H 0.8368(4) 0.3355(6) 0.8293(4) 0.049 Uiso 0.538(11) calc PR 1 C21' C 0.8494(5) 0.4146(8) 0.7498(5) 0.050(2) Uiso 0.462(11) d P 2 H21C H 0.9225(5) 0.4371(8) 0.7477(5) 0.060 Uiso 0.462(11) calc PR 2 H21D H 0.8471(5) 0.3298(8) 0.7577(5) 0.060 Uiso 0.462(11) calc PR 2 C22' C 0.8058(6) 0.4720(8) 0.8366(5) 0.051(2) Uiso 0.462(11) d P 2 H22C H 0.8454(6) 0.4454(8) 0.8942(5) 0.061 Uiso 0.462(11) calc PR 2 H22D H 0.8134(6) 0.5568(8) 0.8325(5) 0.061 Uiso 0.462(11) calc PR 2 C23 C 0.7063(2) 0.4451(3) 0.8409(2) 0.0558(8) Uiso 1 d . . H23A H 0.6782(2) 0.3771(3) 0.8722(2) 0.067 Uiso 1 calc R 1 H23B H 0.7026(2) 0.5106(3) 0.8849(2) 0.067 Uiso 1 calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01624(13) 0.01344(13) 0.01529(13) 0.00032(9) 0.00091(10) -0.00026(10) Br1 0.01941(10) 0.02296(11) 0.02352(11) 0.00036(8) 0.00617(7) -0.00002(8) N1 0.0165(7) 0.0153(8) 0.0179(8) -0.0005(6) 0.0028(6) 0.0008(6) C1 0.0218(10) 0.0218(10) 0.0193(10) 0.0012(8) 0.0044(7) -0.0003(8) Co2 0.0132(2) 0.0131(2) 0.0150(2) 0.000 0.00177(13) 0.000 N2 0.0165(7) 0.0150(8) 0.0177(8) -0.0009(6) 0.0024(6) -0.0019(6) C2 0.0317(11) 0.0291(11) 0.0174(10) 0.0009(8) 0.0045(8) -0.0011(9) N3 0.0159(7) 0.0159(8) 0.0188(8) 0.0006(6) 0.0031(6) -0.0005(6) C3 0.0309(11) 0.0278(11) 0.0199(10) -0.0035(8) -0.0038(8) -0.0037(9) N4 0.0165(8) 0.0162(8) 0.0166(8) 0.0004(6) 0.0019(6) -0.0013(6) C4 0.0221(10) 0.0238(11) 0.0230(10) -0.0019(8) 0.0012(8) -0.0056(8) N5 0.0146(7) 0.0153(8) 0.0186(8) 0.0011(6) 0.0012(6) 0.0003(6) C5 0.0178(9) 0.0133(9) 0.0184(9) -0.0009(7) 0.0025(7) 0.0011(7) N6 0.0161(7) 0.0138(8) 0.0196(8) -0.0009(6) 0.0011(6) 0.0004(6) C6 0.0156(9) 0.0167(9) 0.0198(9) 0.0004(7) 0.0022(7) -0.0015(7) C7 0.0337(11) 0.0187(10) 0.0252(11) -0.0054(8) 0.0113(9) -0.0041(9) C8 0.0428(13) 0.0177(11) 0.0358(13) -0.0060(9) 0.0154(10) -0.0087(9) C9 0.0357(12) 0.0208(11) 0.0326(12) 0.0020(9) 0.0159(10) -0.0054(9) C10 0.0220(10) 0.0212(10) 0.0232(10) 0.0015(8) 0.0080(8) -0.0011(8) C11 0.0195(9) 0.0201(10) 0.0223(10) -0.0008(8) 0.0018(7) -0.0034(8) C12 0.0234(10) 0.0213(10) 0.0294(11) 0.0032(8) 0.0030(8) -0.0080(8) C13 0.0288(11) 0.0175(10) 0.0355(12) 0.0063(9) -0.0009(9) -0.0010(8) C14 0.0184(9) 0.0196(10) 0.0316(11) 0.0045(8) -0.0001(8) 0.0024(8) C15 0.0174(9) 0.0176(9) 0.0155(9) 0.0009(7) 0.0003(7) -0.0018(7) C16 0.0152(9) 0.0131(9) 0.0216(10) -0.0007(7) 0.0013(7) 0.0014(7) C17 0.0223(10) 0.0244(11) 0.0247(11) 0.0057(8) -0.0009(8) -0.0019(8) C18 0.0239(10) 0.0274(11) 0.0267(11) 0.0043(9) -0.0060(8) 0.0017(9) C19 0.0161(9) 0.0238(11) 0.0326(11) -0.0027(9) -0.0023(8) -0.0005(8) C20 0.0184(9) 0.0183(10) 0.0265(10) -0.0029(8) 0.0033(8) -0.0029(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 Co2 2.3262(3) . ? Co2 Co1 2.3263(3) 2_655 ? Co1 Br1 2.6187(3) . ? Co1 N1 1.993(2) . ? Co1 N3 2.006(2) 2_655 ? Co1 N4 2.005(2) . ? Co1 N6 1.995(2) 2_655 ? Co2 N5 1.891(2) 2_655 ? Co2 N5 1.891(2) . ? Co2 N2 1.897(2) . ? Co2 N2 1.897(2) 2_655 ? N1 C1 1.348(2) . ? N1 C5 1.368(2) . ? C1 C2 1.373(3) . ? N2 C6 1.365(2) . ? N2 C5 1.366(2) . ? C2 C3 1.387(3) . ? N3 C10 1.353(2) . ? N3 C6 1.365(2) . ? N3 Co1 2.006(2) 2_655 ? C3 C4 1.370(3) . ? N4 C11 1.354(2) . ? N4 C15 1.365(2) . ? C4 C5 1.406(3) . ? N5 C15 1.366(2) . ? N5 C16 1.368(2) . ? N6 C20 1.355(2) . ? N6 C16 1.364(2) . ? N6 Co1 1.995(2) 2_655 ? C6 C7 1.409(3) . ? C7 C8 1.371(3) . ? C8 C9 1.390(3) . ? C9 C10 1.373(3) . ? C11 C12 1.372(3) . ? C12 C13 1.390(3) . ? C13 C14 1.373(3) . ? C14 C15 1.408(3) . ? C16 C17 1.411(3) . ? C17 C18 1.376(3) . ? C18 C19 1.390(3) . ? C19 C20 1.378(3) . ? C21 C22 1.516(8) . ? C21 C23 1.520(6) 2_656 ? C22 C23 1.603(7) . ? C21' C23 1.483(7) 2_656 ? C21' C22' 1.552(11) . ? C22' C23 1.338(7) . ? C23 C21' 1.483(7) 2_656 ? C23 C21 1.520(6) 2_656 ? 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 N1 Co1 N6 169.65(6) . 2_655 ? N1 Co1 N4 88.97(6) . . ? N6 Co1 N4 90.08(6) 2_655 . ? N1 Co1 N3 89.49(7) . 2_655 ? N6 Co1 N3 89.41(6) 2_655 2_655 ? N4 Co1 N3 168.63(6) . 2_655 ? N1 Co1 Co2 84.93(4) . . ? N6 Co1 Co2 84.72(4) 2_655 . ? N4 Co1 Co2 84.58(5) . . ? N3 Co1 Co2 84.06(4) 2_655 . ? N1 Co1 Br1 95.58(4) . . ? N6 Co1 Br1 94.77(4) 2_655 . ? N4 Co1 Br1 95.53(4) . . ? N3 Co1 Br1 95.83(4) 2_655 . ? Co2 Co1 Br1 179.479(12) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Co1 121.20(13) . . ? C5 N1 Co1 120.38(12) . . ? N1 C1 C2 123.6(2) . . ? N5 Co2 N5 89.60(10) 2_655 . ? N5 Co2 N2 179.20(7) 2_655 . ? N5 Co2 N2 89.88(7) . . ? N5 Co2 N2 89.88(7) 2_655 2_655 ? N5 Co2 N2 179.20(7) . 2_655 ? N2 Co2 N2 90.66(10) . 2_655 ? N5 Co2 Co1 89.75(5) 2_655 . ? N5 Co2 Co1 90.30(5) . . ? N2 Co2 Co1 89.65(5) . . ? N2 Co2 Co1 90.30(5) 2_655 . ? N5 Co2 Co1 90.29(5) 2_655 2_655 ? N5 Co2 Co1 89.75(5) . 2_655 ? N2 Co2 Co1 90.30(5) . 2_655 ? N2 Co2 Co1 89.65(5) 2_655 2_655 ? Co1 Co2 Co1 179.93(2) . 2_655 ? C6 N2 C5 124.6(2) . . ? C6 N2 Co2 117.24(13) . . ? C5 N2 Co2 118.17(12) . . ? C1 C2 C3 118.6(2) . . ? C10 N3 C6 118.4(2) . . ? C10 N3 Co1 120.76(13) . 2_655 ? C6 N3 Co1 120.65(12) . 2_655 ? C4 C3 C2 119.1(2) . . ? C11 N4 C15 118.1(2) . . ? C11 N4 Co1 121.39(13) . . ? C15 N4 Co1 120.42(12) . . ? C3 C4 C5 120.5(2) . . ? C15 N5 C16 124.9(2) . . ? C15 N5 Co2 117.59(12) . . ? C16 N5 Co2 117.53(12) . . ? N2 C5 N1 114.9(2) . . ? N2 C5 C4 125.0(2) . . ? N1 C5 C4 119.9(2) . . ? C20 N6 C16 118.5(2) . . ? C20 N6 Co1 121.25(13) . 2_655 ? C16 N6 Co1 120.14(12) . 2_655 ? N2 C6 N3 115.0(2) . . ? N2 C6 C7 124.1(2) . . ? N3 C6 C7 120.5(2) . . ? C8 C7 C6 119.7(2) . . ? C7 C8 C9 119.5(2) . . ? C10 C9 C8 118.8(2) . . ? N3 C10 C9 123.0(2) . . ? N4 C11 C12 123.5(2) . . ? C11 C12 C13 118.7(2) . . ? C14 C13 C12 119.0(2) . . ? C13 C14 C15 120.2(2) . . ? N4 C15 N5 115.2(2) . . ? N4 C15 C14 120.4(2) . . ? N5 C15 C14 124.0(2) . . ? N6 C16 N5 115.2(2) . . ? N6 C16 C17 120.3(2) . . ? N5 C16 C17 124.1(2) . . ? C18 C17 C16 119.7(2) . . ? C17 C18 C19 119.9(2) . . ? C20 C19 C18 118.1(2) . . ? N6 C20 C19 123.5(2) . . ? C22 C21 C23 109.3(4) . 2_656 ? C21 C22 C23 114.2(4) . . ? C23 C21' C22' 114.5(6) 2_656 . ? C23 C22' C21' 110.4(6) . . ? C22' C23 C21' 115.3(5) . 2_656 ? C21 C23 C22 121.6(3) 2_656 . ? _refine_diff_density_max 0.487 _refine_diff_density_min -0.444 _refine_diff_density_rms 0.066 #===END data_1.C6H12_at_213K _audit_creation_method SHELXL _chemical_formula_sum 'C46 H44 Br2 Co3 N12' _chemical_formula_weight 1101.54 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 '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 1 2/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y, -z-1/2' _cell_length_a 13.0226(6) _cell_length_b 11.6749(5) _cell_length_c 14.3720(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.958(1) _cell_angle_gamma 90.00 _cell_volume 2179.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 6732 _cell_measurement_theta_min 2.187 _cell_measurement_theta_max 27.495 _exptl_crystal_description block _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.678 _exptl_crystal_density_method ? _exptl_crystal_F_000 1110 _exptl_absorpt_coefficient_mu 3.011 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3824 _exptl_absorpt_correction_T_max 0.5330 _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13357 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4976 _reflns_number_observed 3829 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.8094P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4976 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_obs 0.0263 _refine_ls_wR_factor_all 0.0708 _refine_ls_wR_factor_obs 0.0658 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.89993(2) 0.18556(2) 0.16708(2) 0.02318(8) Uani 1 d . . Br1 Br 1.06581(2) 0.18595(2) 0.07713(2) 0.03116(7) Uani 1 d . . N1 N 0.80436(12) 0.12849(14) 0.06037(12) 0.0224(4) Uani 1 d . . C1 C 0.8260(2) 0.1462(2) -0.02878(15) 0.0293(5) Uani 1 d . . H1A H 0.8865(2) 0.1862(2) -0.04002(15) 0.035 Uiso 1 calc R . Co2 Co 0.7500 0.18572(3) 0.2500 0.01786(9) Uani 1 d S . N2 N 0.69203(12) 0.07102(14) 0.16814(11) 0.0214(3) Uani 1 d . . C2 C 0.7646(2) 0.1091(2) -0.1040(2) 0.0364(5) Uani 1 d . . H2A H 0.7828(2) 0.1231(2) -0.1651(2) 0.044 Uiso 1 calc R . N3 N 0.58669(12) 0.02228(14) 0.28452(12) 0.0233(4) Uani 1 d . . C3 C 0.6752(2) 0.0505(2) -0.0881(2) 0.0376(5) Uani 1 d . . H3A H 0.6320(2) 0.0232(2) -0.1383(2) 0.045 Uiso 1 calc R . N4 N 0.85590(12) 0.34836(14) 0.13351(12) 0.0227(4) Uani 1 d . . C4 C 0.6502(2) 0.0327(2) 0.0018(2) 0.0321(5) Uani 1 d . . H4A H 0.5895(2) -0.0068(2) 0.0134(2) 0.039 Uiso 1 calc R . N5 N 0.69136(12) 0.30088(14) 0.16985(12) 0.0213(3) Uani 1 d . . C5 C 0.71510(15) 0.0733(2) 0.07682(14) 0.0223(4) Uani 1 d . . N6 N 0.53159(12) 0.24235(14) 0.21103(12) 0.0232(4) Uani 1 d . . C6 C 0.63185(15) -0.0103(2) 0.20574(14) 0.0228(4) Uani 1 d . . C7 C 0.6230(2) -0.1239(2) 0.1735(2) 0.0350(5) Uani 1 d . . H7A H 0.6523(2) -0.1456(2) 0.1182(2) 0.042 Uiso 1 calc R . C8 C 0.5714(2) -0.2026(2) 0.2233(2) 0.0440(6) Uani 1 d . . H8A H 0.5647(2) -0.2786(2) 0.2020(2) 0.053 Uiso 1 calc R . C9 C 0.5292(2) -0.1699(2) 0.3049(2) 0.0409(6) Uani 1 d . . H9A H 0.4944(2) -0.2234(2) 0.3403(2) 0.049 Uiso 1 calc R . C10 C 0.5389(2) -0.0585(2) 0.3331(2) 0.0316(5) Uani 1 d . . H10A H 0.5109(2) -0.0369(2) 0.3891(2) 0.038 Uiso 1 calc R . C11 C 0.9252(2) 0.4274(2) 0.10993(15) 0.0290(5) Uani 1 d . . H11A H 0.9945(2) 0.4050(2) 0.10900(15) 0.035 Uiso 1 calc R . C12 C 0.9002(2) 0.5386(2) 0.0872(2) 0.0350(5) Uani 1 d . . H12A H 0.9507(2) 0.5901(2) 0.0693(2) 0.042 Uiso 1 calc R . C13 C 0.7989(2) 0.5732(2) 0.0914(2) 0.0382(6) Uani 1 d . . H13A H 0.7795(2) 0.6490(2) 0.0767(2) 0.046 Uiso 1 calc R . C14 C 0.7271(2) 0.4955(2) 0.1171(2) 0.0325(5) Uani 1 d . . H14A H 0.6584(2) 0.5185(2) 0.1212(2) 0.039 Uiso 1 calc R . C15 C 0.75605(15) 0.3816(2) 0.13718(14) 0.0223(4) Uani 1 d . . C16 C 0.58755(15) 0.2970(2) 0.14781(15) 0.0227(4) Uani 1 d . . C17 C 0.5397(2) 0.3345(2) 0.0623(2) 0.0332(5) Uani 1 d . . H17A H 0.5781(2) 0.3738(2) 0.0194(2) 0.040 Uiso 1 calc R . C18 C 0.4372(2) 0.3134(2) 0.0421(2) 0.0377(5) Uani 1 d . . H18A H 0.4050(2) 0.3384(2) -0.0149(2) 0.045 Uiso 1 calc R . C19 C 0.3809(2) 0.2554(2) 0.1055(2) 0.0348(5) Uani 1 d . . H19A H 0.3106(2) 0.2395(2) 0.0923(2) 0.042 Uiso 1 calc R . C20 C 0.4307(2) 0.2219(2) 0.1880(2) 0.0297(5) Uani 1 d . . H20A H 0.3927(2) 0.1826(2) 0.2312(2) 0.036 Uiso 1 calc R . C21 C 0.8651(4) 0.4696(7) 0.7424(4) 0.053(2) Uiso 0.572(13) d P 1 H21A H 0.8731(4) 0.5526(7) 0.7496(4) 0.064 Uiso 0.572(13) calc PR 1 H21B H 0.9329(4) 0.4368(7) 0.7329(4) 0.064 Uiso 0.572(13) calc PR 1 C22 C 0.8242(5) 0.4194(8) 0.8299(4) 0.063(2) Uiso 0.572(13) d P 1 H22A H 0.8642(5) 0.4506(8) 0.8844(4) 0.075 Uiso 0.572(13) calc PR 1 H22B H 0.8348(5) 0.3363(8) 0.8296(4) 0.075 Uiso 0.572(13) calc PR 1 C21' C 0.8491(7) 0.4106(12) 0.7496(6) 0.071(3) Uiso 0.428(13) d P 2 H21C H 0.9225(7) 0.4282(12) 0.7471(6) 0.085 Uiso 0.428(13) calc PR 2 H21D H 0.8422(7) 0.3279(12) 0.7591(6) 0.085 Uiso 0.428(13) calc PR 2 C22' C 0.8046(7) 0.4772(11) 0.8341(6) 0.067(3) Uiso 0.428(13) d P 2 H22C H 0.8454(7) 0.4596(11) 0.8921(6) 0.081 Uiso 0.428(13) calc PR 2 H22D H 0.8075(7) 0.5600(11) 0.8234(6) 0.081 Uiso 0.428(13) calc PR 2 C23 C 0.7072(3) 0.4442(4) 0.8404(3) 0.0790(10) Uiso 1 d . . H23A H 0.6794(3) 0.3777(4) 0.8719(3) 0.095 Uiso 1 calc R 1 H23B H 0.7037(3) 0.5091(4) 0.8832(3) 0.095 Uiso 1 calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0283(2) 0.01880(14) 0.02207(15) 0.00030(11) -0.00073(11) -0.00019(12) Br1 0.02897(12) 0.03255(13) 0.03296(13) 0.00054(9) 0.00940(9) 0.00016(9) N1 0.0227(8) 0.0212(9) 0.0235(9) -0.0002(7) 0.0045(7) -0.0002(7) C1 0.0315(11) 0.0311(12) 0.0262(11) 0.0034(9) 0.0079(9) -0.0012(9) Co2 0.0182(2) 0.0170(2) 0.0185(2) 0.000 0.00242(13) 0.000 N2 0.0220(8) 0.0195(9) 0.0230(8) -0.0019(7) 0.0035(6) -0.0031(7) C2 0.0464(14) 0.0419(14) 0.0217(11) 0.0016(10) 0.0079(10) -0.0022(11) N3 0.0220(8) 0.0233(9) 0.0250(9) 0.0008(7) 0.0045(7) 0.0009(7) C3 0.0452(14) 0.0403(14) 0.0263(12) -0.0052(10) -0.0046(10) -0.0053(11) N4 0.0226(8) 0.0220(9) 0.0237(9) -0.0007(7) 0.0022(7) -0.0018(7) C4 0.0312(11) 0.0350(13) 0.0300(12) -0.0021(10) 0.0015(9) -0.0103(10) N5 0.0211(8) 0.0198(9) 0.0230(9) 0.0024(7) 0.0025(6) 0.0011(7) C5 0.0251(10) 0.0185(10) 0.0237(10) -0.0015(8) 0.0046(8) 0.0001(8) N6 0.0234(8) 0.0193(9) 0.0271(9) -0.0013(7) 0.0037(7) 0.0005(7) C6 0.0218(9) 0.0224(10) 0.0246(10) -0.0010(8) 0.0035(8) -0.0027(8) C7 0.0458(14) 0.0264(12) 0.0347(13) -0.0076(10) 0.0166(10) -0.0088(10) C8 0.061(2) 0.0247(13) 0.049(2) -0.0067(11) 0.0205(13) -0.0134(12) C9 0.0507(15) 0.0289(13) 0.0460(15) 0.0043(11) 0.0232(12) -0.0086(11) C10 0.0334(12) 0.0290(12) 0.0338(12) 0.0039(10) 0.0128(9) -0.0002(10) C11 0.0248(10) 0.0299(12) 0.0326(12) -0.0020(9) 0.0034(9) -0.0060(9) C12 0.0347(12) 0.0299(13) 0.0406(14) 0.0062(10) 0.0049(10) -0.0110(10) C13 0.0382(13) 0.0247(12) 0.051(2) 0.0108(11) -0.0015(11) -0.0023(10) C14 0.0267(11) 0.0249(11) 0.0455(14) 0.0088(10) -0.0006(10) 0.0027(9) C15 0.0229(10) 0.0233(11) 0.0204(10) 0.0024(8) -0.0001(7) -0.0018(8) C16 0.0209(9) 0.0177(10) 0.0295(11) -0.0003(8) 0.0022(8) 0.0027(8) C17 0.0298(11) 0.0346(13) 0.0349(13) 0.0101(10) -0.0005(9) -0.0015(10) C18 0.0327(12) 0.0377(14) 0.0411(14) 0.0066(11) -0.0099(10) 0.0011(11) C19 0.0213(10) 0.0348(13) 0.0474(15) -0.0031(11) -0.0032(10) -0.0019(10) C20 0.0248(10) 0.0277(12) 0.0373(13) -0.0047(9) 0.0063(9) -0.0049(9) _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 Co2 2.3566(3) . y Co2 Co1 2.3566(3) 4_756 y Co1 Br1 2.5928(4) . y Co1 N1 2.020(2) . y Co1 N3 2.033(2) 4_756 y Co1 N4 2.034(2) . y Co1 N6 2.022(2) 4_756 y Co2 N2 1.904(2) . y Co2 N2 1.904(2) 4_756 y Co2 N5 1.896(2) 4_756 y Co2 N5 1.896(2) . y N1 C1 1.347(3) . ? N1 C5 1.364(2) . ? C1 C2 1.370(3) . ? N2 C6 1.366(2) . ? N2 C5 1.367(2) . ? C2 C3 1.383(3) . ? N3 C10 1.351(3) . ? N3 C6 1.365(3) . ? N3 Co1 2.033(2) 4_756 ? C3 C4 1.370(3) . ? N4 C11 1.350(3) . ? N4 C15 1.362(3) . ? C4 C5 1.405(3) . ? N5 C16 1.368(2) . ? N5 C15 1.369(2) . ? N6 C20 1.353(3) . ? N6 C16 1.362(3) . ? N6 Co1 2.022(2) 4_756 ? C6 C7 1.407(3) . ? C7 C8 1.369(3) . ? C8 C9 1.384(3) . ? C9 C10 1.366(3) . ? C11 C12 1.372(3) . ? C12 C13 1.385(3) . ? C13 C14 1.370(3) . ? C14 C15 1.407(3) . ? C16 C17 1.408(3) . ? C17 C18 1.370(3) . ? C18 C19 1.387(3) . ? C19 C20 1.369(3) . ? C21 C23 1.496(7) 4_757 ? C21 C22 1.516(10) . ? C22 C23 1.568(8) . ? C21' C23 1.495(10) 4_757 ? C21' C22' 1.59(2) . ? C22' C23 1.335(8) . ? C23 C21' 1.495(10) 4_757 ? C23 C21 1.496(7) 4_757 ? 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 N1 Co1 N6 167.86(7) . 4_756 ? N1 Co1 N3 89.10(7) . 4_756 ? N6 Co1 N3 89.35(7) 4_756 4_756 ? N1 Co1 N4 88.82(7) . . ? N6 Co1 N4 89.96(7) 4_756 . ? N3 Co1 N4 166.86(7) 4_756 . ? N1 Co1 Co2 84.01(5) . . ? N6 Co1 Co2 83.85(5) 4_756 . ? N3 Co1 Co2 83.23(5) 4_756 . ? N4 Co1 Co2 83.65(5) . . ? N1 Co1 Br1 96.48(5) . . ? N6 Co1 Br1 95.66(5) 4_756 . ? N3 Co1 Br1 96.75(5) 4_756 . ? N4 Co1 Br1 96.37(5) . . ? Co2 Co1 Br1 179.506(13) . . ? C1 N1 C5 118.3(2) . . ? C1 N1 Co1 120.89(14) . . ? C5 N1 Co1 120.79(13) . . ? N1 C1 C2 123.6(2) . . ? N5 Co2 N5 89.69(10) 4_756 . ? N5 Co2 N2 179.21(7) 4_756 . ? N5 Co2 N2 89.85(7) . . ? N5 Co2 N2 89.85(7) 4_756 4_756 ? N5 Co2 N2 179.21(7) . 4_756 ? N2 Co2 N2 90.61(10) . 4_756 ? N5 Co2 Co1 89.70(5) 4_756 . ? N5 Co2 Co1 90.36(5) . . ? N2 Co2 Co1 89.66(5) . . ? N2 Co2 Co1 90.28(5) 4_756 . ? N5 Co2 Co1 90.36(5) 4_756 4_756 ? N5 Co2 Co1 89.70(5) . 4_756 ? N2 Co2 Co1 90.28(5) . 4_756 ? N2 Co2 Co1 89.66(5) 4_756 4_756 ? Co1 Co2 Co1 179.91(2) . 4_756 ? C6 N2 C5 124.3(2) . . ? C6 N2 Co2 117.27(13) . . ? C5 N2 Co2 118.40(13) . . ? C1 C2 C3 118.6(2) . . ? C10 N3 C6 118.4(2) . . ? C10 N3 Co1 120.61(14) . 4_756 ? C6 N3 Co1 120.88(13) . 4_756 ? C4 C3 C2 119.2(2) . . ? C11 N4 C15 118.1(2) . . ? C11 N4 Co1 121.05(14) . . ? C15 N4 Co1 120.78(13) . . ? C3 C4 C5 120.2(2) . . ? C16 N5 C15 124.4(2) . . ? C16 N5 Co2 117.86(13) . . ? C15 N5 Co2 117.72(13) . . ? N1 C5 N2 115.0(2) . . ? N1 C5 C4 120.1(2) . . ? N2 C5 C4 124.7(2) . . ? C20 N6 C16 118.3(2) . . ? C20 N6 Co1 121.09(14) . 4_756 ? C16 N6 Co1 120.49(13) . 4_756 ? N3 C6 N2 115.2(2) . . ? N3 C6 C7 120.3(2) . . ? N2 C6 C7 124.1(2) . . ? C8 C7 C6 119.6(2) . . ? C7 C8 C9 119.7(2) . . ? C10 C9 C8 118.7(2) . . ? N3 C10 C9 123.2(2) . . ? N4 C11 C12 123.7(2) . . ? C11 C12 C13 118.5(2) . . ? C14 C13 C12 119.2(2) . . ? C13 C14 C15 120.2(2) . . ? N4 C15 N5 115.4(2) . . ? N4 C15 C14 120.3(2) . . ? N5 C15 C14 124.0(2) . . ? N6 C16 N5 115.3(2) . . ? N6 C16 C17 120.2(2) . . ? N5 C16 C17 124.2(2) . . ? C18 C17 C16 119.7(2) . . ? C17 C18 C19 120.0(2) . . ? C20 C19 C18 117.9(2) . . ? N6 C20 C19 123.8(2) . . ? C23 C21 C22 110.2(5) 4_757 . ? C21 C22 C23 114.1(6) . . ? C23 C21' C22' 110.5(8) 4_757 . ? C23 C22' C21' 108.0(9) . . ? C22' C23 C21' 115.4(6) . 4_757 ? C21 C23 C22 121.5(4) 4_757 . ? _refine_diff_density_max 0.489 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.063 #===END data_1.C6H12_at_298K _audit_creation_method SHELXL _chemical_formula_structural 'Co3(dpa)4Br2.C6H14' _chemical_formula_sum 'C46 H46 Br2 Co3 N12' _chemical_formula_weight 1103.56 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 '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 1 2/n 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.0483(7) _cell_length_b 11.7668(6) _cell_length_c 14.4367(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.7810(10) _cell_angle_gamma 90.00 _cell_volume 2211.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5434 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.657 _exptl_crystal_density_method ? _exptl_crystal_F_000 1114 _exptl_absorpt_coefficient_mu 2.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.389 _exptl_absorpt_correction_T_max 0.533 _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w-scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13620 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5060 _reflns_number_observed 3468 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0401P)^2^+0.2191P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5060 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_obs 0.0292 _refine_ls_wR_factor_all 0.0813 _refine_ls_wR_factor_obs 0.0731 _refine_ls_goodness_of_fit_all 1.030 _refine_ls_goodness_of_fit_obs 1.134 _refine_ls_restrained_S_all 1.030 _refine_ls_restrained_S_obs 1.134 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.90132(2) 0.18644(3) 0.16617(2) 0.03483(9) Uani 1 d . . Br1 Br 1.06540(2) 0.18704(2) 0.07712(2) 0.04704(9) Uani 1 d . . N1 N 0.80302(14) 0.1287(2) 0.06020(13) 0.0327(4) Uani 1 d . . C1 C 0.8245(2) 0.1446(2) -0.0289(2) 0.0431(6) Uani 1 d . . H1A H 0.8843(2) 0.1836(2) -0.0407(2) 0.052 Uiso 1 calc R . Co2 Co 0.7500 0.18652(3) 0.2500 0.02569(10) Uani 1 d S . N2 N 0.69206(13) 0.0721(2) 0.16866(13) 0.0301(4) Uani 1 d . . C2 C 0.7635(2) 0.1070(3) -0.1026(2) 0.0541(7) Uani 1 d . . H2A H 0.7816(2) 0.1193(3) -0.1630(2) 0.065 Uiso 1 calc R . N3 N 0.58709(14) 0.0227(2) 0.28439(13) 0.0332(4) Uani 1 d . . C3 C 0.6744(2) 0.0503(3) -0.0857(2) 0.0556(7) Uani 1 d . . H3A H 0.6314(2) 0.0232(3) -0.1348(2) 0.067 Uiso 1 calc R . N4 N 0.85503(14) 0.3494(2) 0.13352(13) 0.0326(4) Uani 1 d . . C4 C 0.6498(2) 0.0342(2) 0.0036(2) 0.0462(7) Uani 1 d . . H4A H 0.5896(2) -0.0038(2) 0.0156(2) 0.055 Uiso 1 calc R . N5 N 0.69145(13) 0.3009(2) 0.17020(13) 0.0303(4) Uani 1 d . . C5 C 0.7145(2) 0.0744(2) 0.0774(2) 0.0315(5) Uani 1 d . . N6 N 0.53164(14) 0.2431(2) 0.21039(13) 0.0336(4) Uani 1 d . . C6 C 0.6325(2) -0.0090(2) 0.2062(2) 0.0328(5) Uani 1 d . . C7 C 0.6254(2) -0.1218(2) 0.1746(2) 0.0502(7) Uani 1 d . . H7A H 0.6553(2) -0.1430(2) 0.1204(2) 0.060 Uiso 1 calc R . C8 C 0.5743(3) -0.2002(2) 0.2240(2) 0.0627(9) Uani 1 d . . H8A H 0.5684(3) -0.2749(2) 0.2033(2) 0.075 Uiso 1 calc R . C9 C 0.5315(2) -0.1680(2) 0.3049(2) 0.0589(8) Uani 1 d . . H9A H 0.4973(2) -0.2206(2) 0.3398(2) 0.071 Uiso 1 calc R . C10 C 0.5403(2) -0.0578(2) 0.3325(2) 0.0454(6) Uani 1 d . . H10A H 0.5125(2) -0.0370(2) 0.3877(2) 0.054 Uiso 1 calc R . C11 C 0.9237(2) 0.4284(2) 0.1097(2) 0.0412(6) Uani 1 d . . H11A H 0.9921(2) 0.4068(2) 0.1078(2) 0.049 Uiso 1 calc R . C12 C 0.8980(2) 0.5383(2) 0.0881(2) 0.0504(7) Uani 1 d . . H12A H 0.9475(2) 0.5895(2) 0.0705(2) 0.060 Uiso 1 calc R . C13 C 0.7972(2) 0.5720(2) 0.0928(2) 0.0537(7) Uani 1 d . . H13A H 0.7778(2) 0.6465(2) 0.0789(2) 0.064 Uiso 1 calc R . C14 C 0.7261(2) 0.4945(2) 0.1183(2) 0.0469(7) Uani 1 d . . H14A H 0.6581(2) 0.5166(2) 0.1227(2) 0.056 Uiso 1 calc R . C15 C 0.7553(2) 0.3817(2) 0.1378(2) 0.0322(5) Uani 1 d . . C16 C 0.5880(2) 0.2970(2) 0.1477(2) 0.0325(5) Uani 1 d . . C17 C 0.5415(2) 0.3338(2) 0.0624(2) 0.0473(7) Uani 1 d . . H17A H 0.5800(2) 0.3720(2) 0.0203(2) 0.057 Uiso 1 calc R . C18 C 0.4392(2) 0.3132(2) 0.0416(2) 0.0544(7) Uani 1 d . . H18A H 0.4079(2) 0.3373(2) -0.0147(2) 0.065 Uiso 1 calc R . C19 C 0.3827(2) 0.2560(2) 0.1051(2) 0.0514(7) Uani 1 d . . H19A H 0.3134(2) 0.2404(2) 0.0919(2) 0.062 Uiso 1 calc R . C20 C 0.4312(2) 0.2235(2) 0.1871(2) 0.0435(6) Uani 1 d . . H20A H 0.3930(2) 0.1855(2) 0.2296(2) 0.052 Uiso 1 calc R . C21 C 0.8622(5) 0.4661(10) 0.7416(5) 0.088(3) Uiso 0.640(15) d P 1 H21A H 0.8729(5) 0.5475(10) 0.7469(5) 0.106 Uiso 0.640(15) calc PR 1 H21B H 0.9281(5) 0.4308(10) 0.7330(5) 0.106 Uiso 0.640(15) calc PR 1 C22 C 0.8211(5) 0.4223(10) 0.8298(5) 0.094(3) Uiso 0.640(15) d P 1 H22A H 0.8341(5) 0.3412(10) 0.8335(5) 0.112 Uiso 0.640(15) calc PR 1 H22B H 0.8596(5) 0.4576(10) 0.8819(5) 0.112 Uiso 0.640(15) calc PR 1 C21' C 0.8483(10) 0.3988(18) 0.7512(9) 0.095(5) Uiso 0.360(15) d P 2 H21C H 0.9222(10) 0.4051(18) 0.7490(9) 0.114 Uiso 0.360(15) calc PR 2 H21D H 0.8302(10) 0.3208(18) 0.7647(9) 0.114 Uiso 0.360(15) calc PR 2 C22' C 0.8017(10) 0.4920(17) 0.8302(9) 0.096(5) Uiso 0.360(15) d P 2 H22C H 0.8440(10) 0.4934(17) 0.8881(9) 0.115 Uiso 0.360(15) calc PR 2 H22D H 0.7946(10) 0.5684(17) 0.8055(9) 0.115 Uiso 0.360(15) calc PR 2 C23 C 0.7090(4) 0.4421(5) 0.8401(4) 0.124(2) Uiso 1 d . . H23A H 0.6829(4) 0.3754(5) 0.8704(4) 0.149 Uiso 1 calc R 1 H23B H 0.7037(4) 0.5051(5) 0.8829(4) 0.149 Uiso 1 calc R 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0414(2) 0.0297(2) 0.0329(2) 0.00055(14) -0.00118(14) -0.00013(15) Br1 0.0422(2) 0.0505(2) 0.0500(2) 0.00088(13) 0.01510(12) 0.00016(12) N1 0.0322(10) 0.0333(11) 0.0331(11) 0.0008(8) 0.0067(8) -0.0003(9) C1 0.0442(15) 0.049(2) 0.0368(15) 0.0047(12) 0.0098(11) -0.0047(12) Co2 0.0252(2) 0.0256(2) 0.0264(2) 0.000 0.0030(2) 0.000 N2 0.0293(9) 0.0306(10) 0.0308(10) -0.0024(8) 0.0057(8) -0.0040(8) C2 0.066(2) 0.066(2) 0.0310(15) 0.0020(13) 0.0094(13) -0.006(2) N3 0.0303(10) 0.0348(11) 0.0352(11) 0.0016(9) 0.0083(8) -0.0003(8) C3 0.066(2) 0.063(2) 0.037(2) -0.0064(13) -0.0061(14) -0.011(2) N4 0.0317(10) 0.0319(11) 0.0345(11) 0.0005(8) 0.0037(8) -0.0019(8) C4 0.0451(15) 0.054(2) 0.040(2) -0.0039(12) 0.0009(12) -0.0152(13) N5 0.0280(9) 0.0300(11) 0.0330(10) 0.0050(8) 0.0019(8) 0.0012(8) C5 0.0343(12) 0.0286(12) 0.0320(12) -0.0030(9) 0.0052(10) -0.0003(10) N6 0.0306(10) 0.0315(11) 0.0390(11) -0.0025(9) 0.0052(8) -0.0012(8) C6 0.0306(12) 0.0319(13) 0.0363(13) -0.0008(10) 0.0051(10) -0.0039(10) C7 0.067(2) 0.038(2) 0.048(2) -0.0109(12) 0.0227(14) -0.0133(13) C8 0.087(2) 0.037(2) 0.067(2) -0.0089(14) 0.028(2) -0.019(2) C9 0.075(2) 0.040(2) 0.065(2) 0.0035(14) 0.035(2) -0.0133(15) C10 0.049(2) 0.044(2) 0.046(2) 0.0034(12) 0.0193(12) 0.0000(13) C11 0.0340(13) 0.043(2) 0.047(2) -0.0008(12) 0.0056(11) -0.0066(11) C12 0.048(2) 0.042(2) 0.061(2) 0.0094(13) 0.0064(13) -0.0151(13) C13 0.052(2) 0.036(2) 0.072(2) 0.0166(14) -0.0027(14) -0.0037(13) C14 0.0386(14) 0.0367(15) 0.065(2) 0.0137(13) 0.0003(13) 0.0048(11) C15 0.0320(12) 0.0338(13) 0.0307(12) 0.0055(10) 0.0011(9) -0.0007(10) C16 0.0299(12) 0.0285(13) 0.0390(13) 0.0006(10) 0.0025(10) 0.0032(10) C17 0.0394(14) 0.053(2) 0.049(2) 0.0145(13) -0.0038(12) -0.0030(12) C18 0.045(2) 0.058(2) 0.057(2) 0.0094(15) -0.0157(13) 0.0035(14) C19 0.0306(13) 0.055(2) 0.068(2) -0.0016(15) -0.0048(13) -0.0032(13) C20 0.0331(13) 0.041(2) 0.057(2) -0.0058(12) 0.0069(12) -0.0062(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.3830(3) . ? Co1 Br1 2.5689(4) . ? Co1 N1 2.047(2) . ? Co1 N3 2.057(2) 2_655 ? Co1 N4 2.056(2) . ? Co1 N6 2.044(2) 2_655 ? N1 C1 1.348(3) . ? N1 C5 1.356(3) . ? C1 C2 1.360(4) . ? Co2 N5 1.899(2) 2_655 ? Co2 N5 1.899(2) . ? Co2 N2 1.909(2) 2_655 ? Co2 N2 1.909(2) . ? Co2 Co1 2.3830(3) 2_655 ? N2 C6 1.366(3) . ? N2 C5 1.368(3) . ? C2 C3 1.377(4) . ? N3 C10 1.345(3) . ? N3 C6 1.361(3) . ? N3 Co1 2.057(2) 2_655 ? C3 C4 1.363(4) . ? N4 C11 1.352(3) . ? N4 C15 1.361(3) . ? C4 C5 1.398(3) . ? N5 C15 1.366(3) . ? N5 C16 1.368(3) . ? N6 C20 1.351(3) . ? N6 C16 1.360(3) . ? N6 Co1 2.044(2) 2_655 ? C6 C7 1.405(3) . ? C7 C8 1.367(4) . ? C8 C9 1.380(4) . ? C9 C10 1.359(4) . ? C11 C12 1.367(4) . ? C12 C13 1.381(4) . ? C13 C14 1.368(4) . ? C14 C15 1.405(3) . ? C16 C17 1.405(3) . ? C17 C18 1.370(3) . ? C18 C19 1.388(4) . ? C19 C20 1.360(4) . ? C21 C23 1.481(8) 2_656 ? C21 C22 1.504(12) . ? C22 C23 1.499(9) . ? C21' C23 1.558(14) 2_656 ? C21' C22' 1.72(3) . ? C22' C23 1.361(12) . ? C23 C21 1.481(8) 2_656 ? C23 C21' 1.558(14) 2_656 ? 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 N6 Co1 N1 166.14(7) 2_655 . ? N6 Co1 N4 89.90(8) 2_655 . ? N1 Co1 N4 88.75(8) . . ? N6 Co1 N3 89.16(8) 2_655 2_655 ? N1 Co1 N3 88.65(8) . 2_655 ? N4 Co1 N3 165.26(7) . 2_655 ? N6 Co1 Co2 83.01(5) 2_655 . ? N1 Co1 Co2 83.13(5) . . ? N4 Co1 Co2 82.84(5) . . ? N3 Co1 Co2 82.45(5) 2_655 . ? N6 Co1 Br1 96.46(5) 2_655 . ? N1 Co1 Br1 97.40(5) . . ? N4 Co1 Br1 97.16(5) . . ? N3 Co1 Br1 97.56(5) 2_655 . ? Co2 Co1 Br1 179.476(15) . . ? C1 N1 C5 118.3(2) . . ? C1 N1 Co1 120.5(2) . . ? C5 N1 Co1 121.20(15) . . ? N1 C1 C2 123.6(2) . . ? N5 Co2 N5 89.72(11) 2_655 . ? N5 Co2 N2 89.98(8) 2_655 2_655 ? N5 Co2 N2 179.34(8) . 2_655 ? N5 Co2 N2 179.34(8) 2_655 . ? N5 Co2 N2 89.98(8) . . ? N2 Co2 N2 90.33(11) 2_655 . ? N5 Co2 Co1 89.70(5) 2_655 . ? N5 Co2 Co1 90.34(6) . . ? N2 Co2 Co1 90.25(5) 2_655 . ? N2 Co2 Co1 89.72(5) . . ? N5 Co2 Co1 90.34(6) 2_655 2_655 ? N5 Co2 Co1 89.70(6) . 2_655 ? N2 Co2 Co1 89.72(5) 2_655 2_655 ? N2 Co2 Co1 90.25(5) . 2_655 ? Co1 Co2 Co1 179.95(2) . 2_655 ? C6 N2 C5 124.1(2) . . ? C6 N2 Co2 117.5(2) . . ? C5 N2 Co2 118.45(15) . . ? C1 C2 C3 118.5(3) . . ? C10 N3 C6 118.2(2) . . ? C10 N3 Co1 120.4(2) . 2_655 ? C6 N3 Co1 121.26(15) . 2_655 ? C4 C3 C2 119.3(3) . . ? C11 N4 C15 118.1(2) . . ? C11 N4 Co1 120.7(2) . . ? C15 N4 Co1 121.15(15) . . ? C3 C4 C5 120.4(2) . . ? C15 N5 C16 123.8(2) . . ? C15 N5 Co2 118.09(14) . . ? C16 N5 Co2 118.09(15) . . ? N1 C5 N2 115.2(2) . . ? N1 C5 C4 119.9(2) . . ? N2 C5 C4 124.7(2) . . ? C20 N6 C16 118.2(2) . . ? C20 N6 Co1 120.9(2) . 2_655 ? C16 N6 Co1 120.87(15) . 2_655 ? N3 C6 N2 115.3(2) . . ? N3 C6 C7 120.5(2) . . ? N2 C6 C7 123.9(2) . . ? C8 C7 C6 119.4(3) . . ? C7 C8 C9 119.7(3) . . ? C10 C9 C8 118.6(2) . . ? N3 C10 C9 123.6(2) . . ? N4 C11 C12 123.5(2) . . ? C11 C12 C13 118.7(2) . . ? C14 C13 C12 119.2(3) . . ? C13 C14 C15 120.3(2) . . ? N4 C15 N5 115.3(2) . . ? N4 C15 C14 120.1(2) . . ? N5 C15 C14 124.2(2) . . ? N6 C16 N5 115.2(2) . . ? N6 C16 C17 120.4(2) . . ? N5 C16 C17 124.0(2) . . ? C18 C17 C16 119.7(3) . . ? C17 C18 C19 119.6(3) . . ? C20 C19 C18 118.3(2) . . ? N6 C20 C19 123.8(2) . . ? C23 C21 C22 111.6(7) 2_656 . ? C23 C22 C21 115.8(7) . . ? C23 C21' C22' 100.5(12) 2_656 . ? C23 C22' C21' 98.6(14) . . ? C21 C23 C22 121.0(6) 2_656 . ? C22' C23 C21' 115.6(9) . 2_656 ? _refine_diff_density_max 0.468 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.058 #===END data_1-1.75C7H8.0.5C6H14_at_110K _audit_creation_method SHELXL _chemical_formula_structural 'Co3(dpa)4Br2 1.75Toluene 0.5Hexane' _chemical_formula_sum 'C55.25 H53 Br2 Co3 N12' _chemical_formula_weight 1221.71 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.835(1) _cell_length_b 18.060(2) _cell_length_c 19.243(2) _cell_angle_alpha 81.636(2) _cell_angle_beta 82.881(2) _cell_angle_gamma 62.516(1) _cell_volume 5124.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 5318 _cell_measurement_theta_min 2.365 _cell_measurement_theta_max 27.425 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method ? _exptl_crystal_F_000 2478 _exptl_absorpt_coefficient_mu 2.571 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_correction_T_min 0.4054 _exptl_absorpt_correction_T_max 0.7684 _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method \w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35137 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0754 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.53 _reflns_number_total 22686 _reflns_number_observed 14609 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction 'SAINTPLUS and XPREP' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0601P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22686 _refine_ls_number_parameters 1198 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_obs 0.0484 _refine_ls_wR_factor_all 0.1308 _refine_ls_wR_factor_obs 0.1158 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.145 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max 0.012 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.05297(4) 0.72660(4) 0.08794(3) 0.01941(13) Uani 1 d . -1 Co2 Co -0.00832(4) 0.67870(3) 0.18749(3) 0.01661(13) Uani 1 d . -1 Co3 Co -0.07482(4) 0.63040(4) 0.28923(3) 0.02156(14) Uani 1 d . -1 Co4 Co 0.71299(4) 0.17837(3) 0.52297(3) 0.01662(13) Uani 1 d . -1 Co5 Co 0.61884(4) 0.21332(3) 0.43268(3) 0.01510(12) Uani 1 d . -1 Co6 Co 0.53101(4) 0.24068(3) 0.33958(3) 0.01647(13) Uani 1 d . -1 Br1 Br 0.12112(3) 0.78017(3) -0.02397(3) 0.03371(13) Uani 1 d . -1 Br2 Br -0.14614(3) 0.57369(3) 0.39993(3) 0.03041(12) Uani 1 d . -1 Br3 Br 0.81300(3) 0.13643(3) 0.62767(3) 0.02671(11) Uani 1 d . -1 Br4 Br 0.42624(3) 0.27833(3) 0.23607(3) 0.02801(12) Uani 1 d . -1 N1 N -0.0277(2) 0.8403(2) 0.1153(2) 0.0224(8) Uani 1 d . -1 N2 N -0.1133(2) 0.7830(2) 0.1819(2) 0.0202(8) Uani 1 d . -1 N3 N -0.1935(2) 0.7221(2) 0.2535(2) 0.0234(8) Uani 1 d . -1 N4 N 0.1427(2) 0.7168(2) 0.1503(2) 0.0209(8) Uani 1 d . -1 N5 N 0.0407(2) 0.7229(2) 0.2448(2) 0.0168(8) Uani 1 d . -1 N6 N -0.0590(2) 0.7162(2) 0.3366(2) 0.0178(8) Uani 1 d . -1 N7 N -0.0444(2) 0.7285(2) 0.0385(2) 0.0223(8) Uani 1 d . -1 N8 N -0.0569(2) 0.6351(2) 0.1292(2) 0.0201(8) Uani 1 d . -1 N9 N -0.0707(2) 0.5474(2) 0.2252(2) 0.0207(8) Uani 1 d . -1 N10 N 0.1276(2) 0.6058(2) 0.0758(2) 0.0213(8) Uani 1 d . -1 N11 N 0.0973(2) 0.5750(2) 0.1935(2) 0.0189(8) Uani 1 d . -1 N12 N 0.0558(2) 0.5539(2) 0.3107(2) 0.0197(8) Uani 1 d . -1 N13 N 0.8113(2) 0.1131(2) 0.4558(2) 0.0185(8) Uani 1 d . -1 N14 N 0.7026(2) 0.1122(2) 0.3939(2) 0.0162(7) Uani 1 d . -1 N15 N 0.5882(2) 0.1187(2) 0.3353(2) 0.0170(7) Uani 1 d . -1 N16 N 0.6873(2) 0.0810(2) 0.5475(2) 0.0183(8) Uani 1 d . -1 N17 N 0.5598(2) 0.1553(2) 0.4863(2) 0.0166(7) Uani 1 d . -1 N18 N 0.4419(2) 0.2290(2) 0.4148(2) 0.0204(8) Uani 1 d . -1 N19 N 0.5972(2) 0.2544(2) 0.5761(2) 0.0186(8) Uani 1 d . -1 N20 N 0.5337(2) 0.3138(2) 0.4697(2) 0.0177(8) Uani 1 d . -1 N21 N 0.4879(2) 0.3596(2) 0.3565(2) 0.0188(8) Uani 1 d . -1 N22 N 0.7295(2) 0.2783(2) 0.4835(2) 0.0201(8) Uani 1 d . -1 N23 N 0.6788(2) 0.2714(2) 0.3799(2) 0.0173(8) Uani 1 d . -1 N24 N 0.6332(2) 0.2477(2) 0.2807(2) 0.0187(8) Uani 1 d . -1 C1 C -0.0092(3) 0.9061(3) 0.0953(3) 0.0291(11) Uani 1 d . -1 H1A H 0.0444(3) 0.8965(3) 0.0671(3) 0.035 Uiso 1 calc R -1 C2 C -0.0639(4) 0.9864(3) 0.1136(3) 0.0348(12) Uani 1 d . -1 H2A H -0.0491(4) 1.0310(3) 0.0976(3) 0.042 Uiso 1 calc R -1 C3 C -0.1410(4) 0.9995(3) 0.1559(3) 0.0349(12) Uani 1 d . -1 H3A H -0.1801(4) 1.0541(3) 0.1691(3) 0.042 Uiso 1 calc R -1 C4 C -0.1615(3) 0.9343(3) 0.1790(3) 0.0276(11) Uani 1 d . -1 H4A H -0.2138(3) 0.9431(3) 0.2089(3) 0.033 Uiso 1 calc R -1 C5 C -0.1031(3) 0.8536(3) 0.1577(2) 0.0212(10) Uani 1 d . -1 C6 C -0.1944(3) 0.7849(3) 0.2036(2) 0.0212(10) Uani 1 d . -1 C7 C -0.2756(3) 0.8447(3) 0.1750(3) 0.0269(11) Uani 1 d . -1 H7A H -0.2753(3) 0.8861(3) 0.1384(3) 0.032 Uiso 1 calc R -1 C8 C -0.3556(3) 0.8435(3) 0.1999(3) 0.0346(13) Uani 1 d . -1 H8A H -0.4104(3) 0.8837(3) 0.1808(3) 0.042 Uiso 1 calc R -1 C9 C -0.3544(3) 0.7828(3) 0.2530(3) 0.0363(13) Uani 1 d . -1 H9A H -0.4088(3) 0.7824(3) 0.2728(3) 0.044 Uiso 1 calc R -1 C10 C -0.2732(3) 0.7228(3) 0.2769(3) 0.0323(12) Uani 1 d . -1 H10A H -0.2730(3) 0.6796(3) 0.3116(3) 0.039 Uiso 1 calc R -1 C11 C 0.2255(3) 0.7040(3) 0.1249(3) 0.0253(10) Uani 1 d . -1 H11A H 0.2402(3) 0.6987(3) 0.0760(3) 0.030 Uiso 1 calc R -1 C12 C 0.2902(3) 0.6981(3) 0.1656(3) 0.0283(11) Uani 1 d . -1 H12A H 0.3474(3) 0.6908(3) 0.1451(3) 0.034 Uiso 1 calc R -1 C13 C 0.2698(3) 0.7032(3) 0.2374(3) 0.0242(10) Uani 1 d . -1 H13A H 0.3128(3) 0.6999(3) 0.2669(3) 0.029 Uiso 1 calc R -1 C14 C 0.1875(3) 0.7130(3) 0.2653(2) 0.0207(10) Uani 1 d . -1 H14A H 0.1736(3) 0.7152(3) 0.3145(2) 0.025 Uiso 1 calc R -1 C15 C 0.1226(3) 0.7198(3) 0.2213(2) 0.0189(9) Uani 1 d . -1 C16 C -0.0019(3) 0.7492(3) 0.3080(2) 0.0175(9) Uani 1 d . -1 C17 C 0.0076(3) 0.8078(3) 0.3431(2) 0.0209(9) Uani 1 d . -1 H17A H 0.0450(3) 0.8325(3) 0.3223(2) 0.025 Uiso 1 calc R -1 C18 C -0.0371(3) 0.8289(3) 0.4071(2) 0.0226(10) Uani 1 d . -1 H18A H -0.0295(3) 0.8672(3) 0.4313(2) 0.027 Uiso 1 calc R -1 C19 C -0.0940(3) 0.7940(3) 0.4368(2) 0.0242(10) Uani 1 d . -1 H19A H -0.1254(3) 0.8076(3) 0.4813(2) 0.029 Uiso 1 calc R -1 C20 C -0.1028(3) 0.7393(3) 0.3991(2) 0.0222(10) Uani 1 d . -1 H20A H -0.1423(3) 0.7164(3) 0.4186(2) 0.027 Uiso 1 calc R -1 C21 C -0.0757(3) 0.7809(3) -0.0198(2) 0.0296(11) Uani 1 d . -1 H21A H -0.0523(3) 0.8197(3) -0.0358(2) 0.035 Uiso 1 calc R -1 C22 C -0.1402(4) 0.7807(3) -0.0576(3) 0.0383(13) Uani 1 d . -1 H22A H -0.1611(4) 0.8190(3) -0.0984(3) 0.046 Uiso 1 calc R -1 C23 C -0.1741(4) 0.7236(3) -0.0350(3) 0.0379(13) Uani 1 d . -1 H23A H -0.2160(4) 0.7201(3) -0.0615(3) 0.045 Uiso 1 calc R -1 C24 C -0.1463(3) 0.6726(3) 0.0260(3) 0.0284(11) Uani 1 d . -1 H24A H -0.1704(3) 0.6345(3) 0.0429(3) 0.034 Uiso 1 calc R -1 C25 C -0.0814(3) 0.6764(3) 0.0642(2) 0.0208(9) Uani 1 d . -1 C26 C -0.0621(3) 0.5624(3) 0.1534(2) 0.0209(9) Uani 1 d . -1 C27 C -0.0498(3) 0.5004(3) 0.1105(3) 0.0269(11) Uani 1 d . -1 H27A H -0.0425(3) 0.5102(3) 0.0608(3) 0.032 Uiso 1 calc R -1 C28 C -0.0485(3) 0.4261(3) 0.1400(3) 0.0332(12) Uani 1 d . -1 H28A H -0.0406(3) 0.3845(3) 0.1112(3) 0.040 Uiso 1 calc R -1 C29 C -0.0589(3) 0.4125(3) 0.2130(3) 0.0329(12) Uani 1 d . -1 H29A H -0.0597(3) 0.3621(3) 0.2348(3) 0.039 Uiso 1 calc R -1 C30 C -0.0681(3) 0.4738(3) 0.2527(3) 0.0275(11) Uani 1 d . -1 H30A H -0.0728(3) 0.4634(3) 0.3025(3) 0.033 Uiso 1 calc R -1 C31 C 0.1656(3) 0.5790(3) 0.0114(2) 0.0256(11) Uani 1 d . -1 H31A H 0.1504(3) 0.6194(3) -0.0286(2) 0.031 Uiso 1 calc R -1 C32 C 0.2240(3) 0.4979(3) 0.0013(3) 0.0323(12) Uani 1 d . -1 H32A H 0.2480(3) 0.4820(3) -0.0446(3) 0.039 Uiso 1 calc R -1 C33 C 0.2476(3) 0.4387(3) 0.0599(3) 0.0333(12) Uani 1 d . -1 H33A H 0.2908(3) 0.3824(3) 0.0546(3) 0.040 Uiso 1 calc R -1 C34 C 0.2085(3) 0.4617(3) 0.1253(3) 0.0296(11) Uani 1 d . -1 H34A H 0.2227(3) 0.4212(3) 0.1652(3) 0.035 Uiso 1 calc R -1 C35 C 0.1465(3) 0.5470(3) 0.1328(3) 0.0231(10) Uani 1 d . -1 C36 C 0.1238(3) 0.5388(2) 0.2599(2) 0.0183(9) Uani 1 d . -1 C37 C 0.2136(3) 0.4970(3) 0.2786(2) 0.0229(10) Uani 1 d . -1 H37A H 0.2612(3) 0.4868(3) 0.2433(2) 0.028 Uiso 1 calc R -1 C38 C 0.2323(3) 0.4710(3) 0.3479(3) 0.0253(10) Uani 1 d . -1 H38A H 0.2929(3) 0.4429(3) 0.3605(3) 0.030 Uiso 1 calc R -1 C39 C 0.1635(3) 0.4855(3) 0.3994(3) 0.0259(10) Uani 1 d . -1 H39A H 0.1753(3) 0.4670(3) 0.4475(3) 0.031 Uiso 1 calc R -1 C40 C 0.0766(3) 0.5278(3) 0.3784(2) 0.0233(10) Uani 1 d . -1 H40A H 0.0287(3) 0.5392(3) 0.4136(2) 0.028 Uiso 1 calc R -1 C41 C 0.8969(3) 0.0980(3) 0.4610(3) 0.0217(10) Uani 1 d . -1 H41A H 0.9099(3) 0.1183(3) 0.4988(3) 0.026 Uiso 1 calc R -1 C42 C 0.9661(3) 0.0546(3) 0.4139(2) 0.0233(10) Uani 1 d . -1 H42A H 1.0258(3) 0.0435(3) 0.4200(2) 0.028 Uiso 1 calc R -1 C43 C 0.9470(3) 0.0272(3) 0.3573(3) 0.0253(10) Uani 1 d . -1 H43A H 0.9936(3) -0.0023(3) 0.3238(3) 0.030 Uiso 1 calc R -1 C44 C 0.8609(3) 0.0428(3) 0.3501(2) 0.0220(10) Uani 1 d . -1 H44A H 0.8474(3) 0.0243(3) 0.3114(2) 0.026 Uiso 1 calc R -1 C45 C 0.7918(3) 0.0865(2) 0.4001(2) 0.0170(9) Uani 1 d . -1 C46 C 0.6705(3) 0.0708(3) 0.3612(2) 0.0173(9) Uani 1 d . -1 C47 C 0.7118(3) -0.0173(3) 0.3595(2) 0.0195(9) Uani 1 d . -1 H47A H 0.7694(3) -0.0509(3) 0.3772(2) 0.023 Uiso 1 calc R -1 C48 C 0.6689(3) -0.0541(3) 0.3322(2) 0.0216(10) Uani 1 d . -1 H48A H 0.6974(3) -0.1129(3) 0.3296(2) 0.026 Uiso 1 calc R -1 C49 C 0.5839(3) -0.0052(3) 0.3087(2) 0.0239(10) Uani 1 d . -1 H49A H 0.5521(3) -0.0301(3) 0.2916(2) 0.029 Uiso 1 calc R -1 C50 C 0.5462(3) 0.0803(3) 0.3105(2) 0.0215(10) Uani 1 d . -1 H50A H 0.4882(3) 0.1140(3) 0.2936(2) 0.026 Uiso 1 calc R -1 C51 C 0.7482(3) 0.0062(3) 0.5771(2) 0.0239(10) Uani 1 d . -1 H51A H 0.8044(3) 0.0015(3) 0.5868(2) 0.029 Uiso 1 calc R -1 C52 C 0.7332(3) -0.0631(3) 0.5937(3) 0.0283(11) Uani 1 d . -1 H52A H 0.7785(3) -0.1143(3) 0.6136(3) 0.034 Uiso 1 calc R -1 C53 C 0.6502(3) -0.0571(3) 0.5811(3) 0.0274(11) Uani 1 d . -1 H53A H 0.6366(3) -0.1030(3) 0.5945(3) 0.033 Uiso 1 calc R -1 C54 C 0.5885(3) 0.0175(3) 0.5486(2) 0.0242(10) Uani 1 d . -1 H54A H 0.5319(3) 0.0230(3) 0.5391(2) 0.029 Uiso 1 calc R -1 C55 C 0.6086(3) 0.0856(3) 0.5295(2) 0.0187(9) Uani 1 d . -1 C56 C 0.4702(3) 0.1852(3) 0.4781(2) 0.0195(9) Uani 1 d . -1 C57 C 0.4089(3) 0.1796(3) 0.5326(3) 0.0293(11) Uani 1 d . -1 H57A H 0.4296(3) 0.1489(3) 0.5765(3) 0.035 Uiso 1 calc R -1 C58 C 0.3195(3) 0.2187(3) 0.5221(3) 0.0376(13) Uani 1 d . -1 H58A H 0.2774(3) 0.2150(3) 0.5584(3) 0.045 Uiso 1 calc R -1 C59 C 0.2906(3) 0.2639(3) 0.4577(3) 0.0344(12) Uani 1 d . -1 H59A H 0.2285(3) 0.2921(3) 0.4497(3) 0.041 Uiso 1 calc R -1 C60 C 0.3526(3) 0.2674(3) 0.4058(3) 0.0234(10) Uani 1 d . -1 H60A H 0.3323(3) 0.2980(3) 0.3617(3) 0.028 Uiso 1 calc R -1 C61 C 0.5906(3) 0.2479(3) 0.6468(2) 0.0246(10) Uani 1 d . -1 H61A H 0.6402(3) 0.2055(3) 0.6710(2) 0.030 Uiso 1 calc R -1 C62 C 0.5159(3) 0.2993(3) 0.6865(3) 0.0303(11) Uani 1 d . -1 H62A H 0.5150(3) 0.2937(3) 0.7364(3) 0.036 Uiso 1 calc R -1 C63 C 0.4419(3) 0.3597(3) 0.6508(3) 0.0297(11) Uani 1 d . -1 H63A H 0.3894(3) 0.3960(3) 0.6762(3) 0.036 Uiso 1 calc R -1 C64 C 0.4460(3) 0.3659(3) 0.5784(3) 0.0256(10) Uani 1 d . -1 H64A H 0.3950(3) 0.4053(3) 0.5539(3) 0.031 Uiso 1 calc R -1 C65 C 0.5251(3) 0.3144(3) 0.5403(2) 0.0208(10) Uani 1 d . -1 C66 C 0.4884(3) 0.3804(3) 0.4218(2) 0.0213(10) Uani 1 d . -1 C67 C 0.4533(3) 0.4653(3) 0.4327(3) 0.0239(10) Uani 1 d . -1 H67A H 0.4488(3) 0.4807(3) 0.4787(3) 0.029 Uiso 1 calc R -1 C68 C 0.4255(3) 0.5262(3) 0.3771(3) 0.0272(11) Uani 1 d . -1 H68A H 0.4017(3) 0.5837(3) 0.3844(3) 0.033 Uiso 1 calc R -1 C69 C 0.4323(3) 0.5033(3) 0.3105(3) 0.0257(10) Uani 1 d . -1 H69A H 0.4160(3) 0.5444(3) 0.2711(3) 0.031 Uiso 1 calc R -1 C70 C 0.4631(3) 0.4201(3) 0.3023(3) 0.0228(10) Uani 1 d . -1 H70A H 0.4671(3) 0.4045(3) 0.2564(3) 0.027 Uiso 1 calc R -1 C71 C 0.7576(3) 0.3171(3) 0.5228(3) 0.0262(11) Uani 1 d . -1 H71A H 0.7667(3) 0.2969(3) 0.5711(3) 0.031 Uiso 1 calc R -1 C72 C 0.7738(3) 0.3852(3) 0.4960(3) 0.0325(12) Uani 1 d . -1 H72A H 0.7960(3) 0.4092(3) 0.5247(3) 0.039 Uiso 1 calc R -1 C73 C 0.7567(3) 0.4171(3) 0.4262(3) 0.0292(11) Uani 1 d . -1 H73A H 0.7665(3) 0.4638(3) 0.4065(3) 0.035 Uiso 1 calc R -1 C74 C 0.7255(3) 0.3804(3) 0.3862(3) 0.0275(11) Uani 1 d . -1 H74A H 0.7118(3) 0.4029(3) 0.3390(3) 0.033 Uiso 1 calc R -1 C75 C 0.7137(3) 0.3094(3) 0.4145(2) 0.0193(9) Uani 1 d . -1 C76 C 0.6921(3) 0.2651(3) 0.3090(2) 0.0197(9) Uani 1 d . -1 C77 C 0.7665(3) 0.2671(3) 0.2670(3) 0.0261(10) Uani 1 d . -1 H77A H 0.8077(3) 0.2791(3) 0.2867(3) 0.031 Uiso 1 calc R -1 C78 C 0.7788(3) 0.2517(3) 0.1982(3) 0.0301(11) Uani 1 d . -1 H78A H 0.8281(3) 0.2540(3) 0.1697(3) 0.036 Uiso 1 calc R -1 C79 C 0.7190(3) 0.2327(3) 0.1698(3) 0.0307(11) Uani 1 d . -1 H79A H 0.7267(3) 0.2215(3) 0.1220(3) 0.037 Uiso 1 calc R -1 C80 C 0.6489(3) 0.2306(3) 0.2129(2) 0.0225(10) Uani 1 d . -1 H80A H 0.6088(3) 0.2164(3) 0.1940(2) 0.027 Uiso 1 calc R -1 C1S C -0.4187(7) 0.6414(6) 0.1168(6) 0.068(5) Uiso 0.40 d PG 1 C2S C -0.4331(6) 0.5709(7) 0.1335(7) 0.029(4) Uiso 0.40 d PGD 1 C3S C -0.3736(8) 0.5017(6) 0.1743(7) 0.072(6) Uiso 0.40 d PG 1 C4S C -0.2998(7) 0.5030(6) 0.1982(6) 0.047(4) Uiso 0.40 d PG 1 C5S C -0.2855(6) 0.5736(7) 0.1815(6) 0.040(3) Uiso 0.40 d PG 1 C6S C -0.3449(8) 0.6428(6) 0.1408(7) 0.058(5) Uiso 0.40 d PGD 1 C7S C -0.4766(12) 0.7056(11) 0.0744(10) 0.067(5) Uiso 0.40 d PD 1 C1' C -0.3931(6) 0.6709(4) 0.1071(4) 0.069(3) Uiso 0.60 d PG 2 C2' C -0.4493(5) 0.6350(6) 0.1019(5) 0.056(3) Uiso 0.60 d PG 2 C3' C -0.4343(6) 0.5589(6) 0.1403(6) 0.088(7) Uiso 0.60 d PG 2 C4' C -0.3632(7) 0.5186(5) 0.1838(6) 0.078(4) Uiso 0.60 d PG 2 C5' C -0.3071(5) 0.5545(5) 0.1890(4) 0.076(4) Uiso 0.60 d PG 2 C6' C -0.3220(5) 0.6307(5) 0.1506(5) 0.040(3) Uiso 0.60 d PG 2 C7' C -0.4076(9) 0.7461(9) 0.0654(7) 0.081(4) Uiso 0.60 d P 2 C8S C -0.0010(6) 0.2449(7) 0.3737(5) 0.077(4) Uiso 0.60 d PG 1 C9S C 0.0419(7) 0.1984(5) 0.3169(6) 0.066(3) Uiso 0.60 d PG 1 C10S C 0.1099(7) 0.2104(6) 0.2762(4) 0.079(4) Uiso 0.60 d PG 1 C11S C 0.1351(6) 0.2690(7) 0.2922(5) 0.078(4) Uiso 0.60 d PG 1 C12S C 0.0922(8) 0.3154(6) 0.3490(6) 0.070(4) Uiso 0.60 d PG 1 C13S C 0.0241(7) 0.3034(6) 0.3898(4) 0.069(4) Uiso 0.60 d PG 1 C14S C 0.1868(13) 0.2930(13) 0.2596(11) 0.109(6) Uiso 0.50 d P 1 C8' C 0.0869(6) 0.2012(5) 0.2879(5) 0.018(2) Uiso 0.40 d PG 3 C9' C 0.0223(6) 0.2242(6) 0.3437(5) 0.028(3) Uiso 0.40 d PGD 3 C10' C 0.0142(6) 0.2850(6) 0.3846(4) 0.033(3) Uiso 0.40 d PG 3 C11' C 0.0708(7) 0.3229(5) 0.3697(5) 0.023(3) Uiso 0.40 d PG 3 C12' C 0.1353(6) 0.2999(6) 0.3138(5) 0.033(3) Uiso 0.40 d PG 3 C13' C 0.1434(6) 0.2391(6) 0.2730(4) 0.038(3) Uiso 0.40 d PGD 3 C14' C 0.0910(9) 0.1328(9) 0.2445(8) 0.064(4) Uiso 0.50 d PD 3 C15S C 0.1441(16) -0.0519(16) 0.1749(14) 0.151(9) Uiso 0.50 d P 1 C16S C 0.1660(12) -0.0143(11) 0.1017(11) 0.081(5) Uiso 0.50 d P 1 C17S C 0.2365(14) -0.0834(14) 0.0668(12) 0.105(6) Uiso 0.50 d P 1 C18S C 0.2759(11) -0.0588(10) -0.0053(9) 0.050(4) Uiso 0.50 d P 1 C19S C 0.3715(11) -0.1235(11) -0.0591(10) 0.075(5) Uiso 0.50 d P 1 C20S C 0.4115(10) -0.1164(9) -0.0954(8) 0.061(4) Uiso 0.50 d P 1 C15' C 0.3763(8) -0.0463(8) -0.0799(7) 0.048(3) Uiso 0.50 d P 2 C16' C 0.2973(7) -0.0112(7) -0.0289(6) 0.041(3) Uiso 0.50 d P 2 C17' C 0.2544(11) -0.0570(10) 0.0139(9) 0.047(4) Uiso 0.50 d P 2 C18' C 0.3768(10) -0.1770(10) -0.0472(8) 0.064(4) Uiso 0.50 d P 2 C19' C 0.1784(12) -0.0251(11) 0.0607(10) 0.073(5) Uiso 0.50 d P 2 C20' C 0.3091(8) -0.1460(7) -0.0029(6) 0.045(3) Uiso 0.50 d P 2 C21S C 0.4912(8) 0.4644(7) 0.0298(6) 0.039(3) Uiso 0.50 d P . C22S C 0.4135(9) 0.5363(8) 0.0170(8) 0.039(2) Uiso 0.50 d PD . C23S C 0.4103(9) 0.5979(8) -0.0380(7) 0.053(3) Uiso 0.50 d P . C24S C 0.4815(12) 0.5942(10) -0.0817(9) 0.064(5) Uiso 0.50 d P . C25S C 0.5739(10) 0.5114(9) -0.0665(8) 0.061(4) Uiso 0.50 d P . C26S C 0.5719(9) 0.4493(9) -0.0062(8) 0.039(2) Uiso 0.50 d PD . C27S C 0.4821(10) 0.4097(10) 0.0870(9) 0.058(4) Uiso 0.50 d PD . C28S C 0.3860(12) 0.1125(7) 0.1578(8) 0.066(6) Uiso 0.40 d PG 1 C29S C 0.4098(11) 0.0667(9) 0.1000(6) 0.075(7) Uiso 0.40 d PG 1 C30S C 0.4085(10) -0.0104(8) 0.1068(6) 0.037(4) Uiso 0.40 d PG 1 C31S C 0.3834(9) -0.0418(7) 0.1714(6) 0.047(4) Uiso 0.40 d PG 1 C32S C 0.3595(10) 0.0040(8) 0.2292(5) 0.052(5) Uiso 0.40 d PG 1 C33S C 0.3608(11) 0.0811(8) 0.2224(6) 0.052(5) Uiso 0.40 d PG 1 C34S C 0.3719(9) -0.1285(9) 0.1787(8) 0.064(4) Uiso 0.50 d P 1 C28' C 0.3935(6) -0.0665(4) 0.1828(4) 0.059(4) Uiso 0.60 d PG 2 C29' C 0.4063(6) -0.0311(5) 0.1159(4) 0.038(3) Uiso 0.60 d PG 2 C30' C 0.3992(7) 0.0494(5) 0.1067(4) 0.055(3) Uiso 0.60 d PG 2 C31' C 0.3792(7) 0.0946(4) 0.1645(5) 0.061(4) Uiso 0.60 d PG 2 C32' C 0.3663(7) 0.0592(5) 0.2314(4) 0.044(3) Uiso 0.60 d PG 2 C33' C 0.3735(6) -0.0213(5) 0.2405(3) 0.050(3) Uiso 0.60 d PG 2 C34' C 0.3967(9) 0.0937(9) 0.0312(8) 0.065(4) Uiso 0.50 d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0203(3) 0.0230(3) 0.0154(3) -0.0032(2) 0.0005(2) -0.0101(3) Co2 0.0167(3) 0.0164(3) 0.0158(3) -0.0034(2) -0.0002(2) -0.0064(2) Co3 0.0247(3) 0.0193(3) 0.0195(3) -0.0049(3) -0.0036(3) -0.0076(3) Co4 0.0142(3) 0.0158(3) 0.0197(3) -0.0047(2) -0.0004(2) -0.0060(2) Co5 0.0132(3) 0.0130(3) 0.0182(3) -0.0031(2) -0.0002(2) -0.0050(2) Co6 0.0155(3) 0.0129(3) 0.0196(3) -0.0020(2) -0.0019(2) -0.0049(2) Br1 0.0374(3) 0.0467(3) 0.0211(3) -0.0026(2) 0.0048(2) -0.0242(2) Br2 0.0413(3) 0.0362(3) 0.0239(3) -0.0047(2) 0.0047(2) -0.0273(2) Br3 0.0229(2) 0.0303(3) 0.0268(3) -0.0078(2) -0.0066(2) -0.0093(2) Br4 0.0271(3) 0.0247(2) 0.0294(3) -0.0020(2) -0.0099(2) -0.0076(2) N1 0.030(2) 0.023(2) 0.019(2) -0.001(2) -0.004(2) -0.016(2) N2 0.020(2) 0.016(2) 0.023(2) -0.002(2) 0.000(2) -0.0063(15) N3 0.025(2) 0.024(2) 0.025(2) -0.009(2) 0.003(2) -0.013(2) N4 0.019(2) 0.020(2) 0.022(2) -0.005(2) -0.001(2) -0.006(2) N5 0.016(2) 0.018(2) 0.018(2) -0.0040(15) 0.0000(15) -0.0080(15) N6 0.015(2) 0.020(2) 0.017(2) -0.002(2) 0.0014(15) -0.0075(15) N7 0.020(2) 0.024(2) 0.020(2) -0.004(2) 0.001(2) -0.007(2) N8 0.024(2) 0.020(2) 0.017(2) -0.006(2) -0.001(2) -0.010(2) N9 0.020(2) 0.020(2) 0.019(2) -0.003(2) -0.001(2) -0.007(2) N10 0.021(2) 0.026(2) 0.018(2) -0.007(2) 0.000(2) -0.011(2) N11 0.020(2) 0.016(2) 0.019(2) -0.005(2) -0.001(2) -0.0066(15) N12 0.021(2) 0.019(2) 0.021(2) -0.003(2) -0.001(2) -0.010(2) N13 0.015(2) 0.014(2) 0.026(2) -0.001(2) -0.003(2) -0.0062(14) N14 0.018(2) 0.016(2) 0.014(2) -0.0028(14) -0.0019(15) -0.0064(14) N15 0.018(2) 0.016(2) 0.018(2) -0.0031(15) 0.0002(15) -0.0081(15) N16 0.015(2) 0.018(2) 0.019(2) -0.004(2) -0.0010(15) -0.0047(15) N17 0.015(2) 0.016(2) 0.018(2) -0.0054(15) -0.0010(15) -0.0061(14) N18 0.019(2) 0.016(2) 0.028(2) -0.004(2) -0.002(2) -0.0076(15) N19 0.020(2) 0.020(2) 0.019(2) -0.005(2) 0.004(2) -0.012(2) N20 0.017(2) 0.017(2) 0.018(2) -0.005(2) 0.0001(15) -0.0060(15) N21 0.015(2) 0.018(2) 0.021(2) -0.004(2) 0.002(2) -0.0057(15) N22 0.014(2) 0.020(2) 0.027(2) -0.010(2) 0.003(2) -0.0061(15) N23 0.017(2) 0.018(2) 0.017(2) -0.0045(15) 0.0017(15) -0.0086(15) N24 0.020(2) 0.013(2) 0.021(2) 0.0002(15) -0.001(2) -0.0062(15) C1 0.040(3) 0.034(3) 0.022(3) -0.001(2) 0.000(2) -0.025(2) C2 0.054(3) 0.024(3) 0.030(3) 0.000(2) 0.000(3) -0.022(2) C3 0.050(3) 0.019(2) 0.030(3) -0.005(2) 0.001(3) -0.011(2) C4 0.032(3) 0.020(2) 0.027(3) -0.004(2) 0.000(2) -0.008(2) C5 0.025(2) 0.021(2) 0.018(2) -0.003(2) -0.002(2) -0.010(2) C6 0.019(2) 0.022(2) 0.021(2) -0.011(2) 0.001(2) -0.007(2) C7 0.025(2) 0.020(2) 0.034(3) -0.010(2) -0.003(2) -0.006(2) C8 0.023(3) 0.037(3) 0.047(3) -0.021(3) -0.004(2) -0.011(2) C9 0.026(3) 0.047(3) 0.047(3) -0.023(3) 0.007(2) -0.021(2) C10 0.034(3) 0.037(3) 0.037(3) -0.019(2) 0.008(2) -0.024(2) C11 0.026(2) 0.026(2) 0.024(3) -0.005(2) 0.007(2) -0.013(2) C12 0.019(2) 0.029(3) 0.034(3) -0.004(2) 0.004(2) -0.011(2) C13 0.018(2) 0.019(2) 0.035(3) -0.006(2) -0.005(2) -0.006(2) C14 0.024(2) 0.020(2) 0.019(2) -0.004(2) -0.003(2) -0.009(2) C15 0.021(2) 0.016(2) 0.018(2) 0.000(2) -0.002(2) -0.006(2) C16 0.014(2) 0.017(2) 0.020(2) -0.001(2) -0.002(2) -0.006(2) C17 0.018(2) 0.019(2) 0.025(2) -0.005(2) -0.001(2) -0.007(2) C18 0.020(2) 0.020(2) 0.025(2) -0.009(2) -0.002(2) -0.005(2) C19 0.022(2) 0.026(2) 0.020(2) -0.005(2) 0.004(2) -0.008(2) C20 0.020(2) 0.025(2) 0.020(2) -0.003(2) 0.004(2) -0.010(2) C21 0.039(3) 0.031(3) 0.021(3) 0.004(2) -0.006(2) -0.018(2) C22 0.043(3) 0.045(3) 0.028(3) 0.006(2) -0.013(2) -0.020(3) C23 0.042(3) 0.044(3) 0.035(3) 0.006(3) -0.018(3) -0.025(3) C24 0.031(3) 0.032(3) 0.027(3) -0.005(2) -0.004(2) -0.018(2) C25 0.020(2) 0.023(2) 0.019(2) -0.006(2) 0.000(2) -0.009(2) C26 0.017(2) 0.021(2) 0.022(2) -0.004(2) 0.000(2) -0.006(2) C27 0.033(3) 0.025(2) 0.024(3) -0.006(2) -0.005(2) -0.012(2) C28 0.036(3) 0.026(3) 0.039(3) -0.006(2) -0.013(2) -0.011(2) C29 0.038(3) 0.017(2) 0.042(3) 0.005(2) -0.013(3) -0.011(2) C30 0.030(3) 0.021(2) 0.026(3) 0.003(2) -0.003(2) -0.008(2) C31 0.021(2) 0.040(3) 0.018(2) -0.014(2) 0.003(2) -0.014(2) C32 0.031(3) 0.039(3) 0.032(3) -0.018(2) 0.003(2) -0.017(2) C33 0.027(3) 0.032(3) 0.042(3) -0.023(3) 0.007(2) -0.011(2) C34 0.030(3) 0.022(2) 0.035(3) -0.010(2) -0.001(2) -0.009(2) C35 0.017(2) 0.028(2) 0.027(3) -0.010(2) 0.002(2) -0.011(2) C36 0.020(2) 0.012(2) 0.022(2) -0.005(2) 0.003(2) -0.006(2) C37 0.021(2) 0.019(2) 0.028(3) -0.005(2) -0.002(2) -0.006(2) C38 0.022(2) 0.019(2) 0.033(3) 0.001(2) -0.008(2) -0.007(2) C39 0.030(3) 0.021(2) 0.027(3) 0.001(2) -0.008(2) -0.012(2) C40 0.028(2) 0.022(2) 0.022(2) -0.003(2) -0.003(2) -0.012(2) C41 0.015(2) 0.019(2) 0.031(3) -0.003(2) -0.003(2) -0.007(2) C42 0.014(2) 0.024(2) 0.030(3) 0.000(2) 0.001(2) -0.009(2) C43 0.019(2) 0.022(2) 0.031(3) -0.003(2) 0.004(2) -0.008(2) C44 0.025(2) 0.018(2) 0.022(2) -0.006(2) -0.002(2) -0.008(2) C45 0.017(2) 0.013(2) 0.019(2) 0.001(2) 0.000(2) -0.007(2) C46 0.016(2) 0.017(2) 0.018(2) -0.004(2) 0.001(2) -0.006(2) C47 0.017(2) 0.015(2) 0.022(2) -0.003(2) 0.000(2) -0.003(2) C48 0.020(2) 0.016(2) 0.027(3) -0.006(2) 0.002(2) -0.006(2) C49 0.026(2) 0.024(2) 0.028(3) -0.006(2) -0.002(2) -0.016(2) C50 0.020(2) 0.022(2) 0.022(2) -0.005(2) -0.001(2) -0.009(2) C51 0.017(2) 0.027(2) 0.022(2) -0.003(2) 0.000(2) -0.006(2) C52 0.026(3) 0.023(2) 0.027(3) 0.005(2) -0.005(2) -0.005(2) C53 0.031(3) 0.023(2) 0.029(3) 0.003(2) -0.002(2) -0.014(2) C54 0.024(2) 0.024(2) 0.028(3) -0.002(2) -0.002(2) -0.013(2) C55 0.018(2) 0.021(2) 0.015(2) -0.003(2) 0.004(2) -0.008(2) C56 0.016(2) 0.013(2) 0.028(3) -0.002(2) -0.004(2) -0.005(2) C57 0.018(2) 0.031(3) 0.034(3) 0.002(2) 0.001(2) -0.009(2) C58 0.016(2) 0.032(3) 0.055(4) 0.008(3) 0.007(2) -0.008(2) C59 0.013(2) 0.027(3) 0.052(4) 0.003(2) 0.000(2) -0.003(2) C60 0.013(2) 0.015(2) 0.038(3) 0.001(2) -0.005(2) -0.003(2) C61 0.029(3) 0.030(3) 0.024(3) -0.005(2) 0.001(2) -0.021(2) C62 0.034(3) 0.040(3) 0.023(3) -0.014(2) 0.003(2) -0.021(2) C63 0.028(3) 0.029(3) 0.033(3) -0.016(2) 0.012(2) -0.013(2) C64 0.020(2) 0.022(2) 0.032(3) -0.006(2) 0.002(2) -0.007(2) C65 0.015(2) 0.018(2) 0.030(3) -0.009(2) 0.003(2) -0.007(2) C66 0.014(2) 0.018(2) 0.029(3) -0.005(2) 0.004(2) -0.006(2) C67 0.020(2) 0.020(2) 0.030(3) -0.006(2) 0.001(2) -0.007(2) C68 0.020(2) 0.013(2) 0.043(3) -0.005(2) 0.003(2) -0.004(2) C69 0.022(2) 0.018(2) 0.034(3) 0.001(2) -0.002(2) -0.007(2) C70 0.016(2) 0.019(2) 0.029(3) 0.001(2) -0.005(2) -0.004(2) C71 0.020(2) 0.026(2) 0.034(3) -0.015(2) 0.000(2) -0.008(2) C72 0.028(3) 0.030(3) 0.047(3) -0.016(3) 0.000(2) -0.017(2) C73 0.026(3) 0.023(2) 0.044(3) -0.010(2) 0.008(2) -0.016(2) C74 0.023(2) 0.019(2) 0.037(3) -0.006(2) 0.005(2) -0.007(2) C75 0.013(2) 0.020(2) 0.022(2) -0.008(2) 0.005(2) -0.006(2) C76 0.019(2) 0.015(2) 0.022(2) -0.002(2) 0.001(2) -0.006(2) C77 0.030(3) 0.026(2) 0.027(3) -0.006(2) 0.006(2) -0.018(2) C78 0.030(3) 0.031(3) 0.031(3) -0.004(2) 0.006(2) -0.017(2) C79 0.042(3) 0.026(3) 0.022(3) -0.002(2) 0.004(2) -0.016(2) C80 0.025(2) 0.020(2) 0.019(2) 0.002(2) -0.004(2) -0.008(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.3097(9) . y Co2 Co3 2.3892(9) . y Co1 Br1 2.5877(8) . y Co3 Br2 2.6259(8) . y Co1 N1 1.976(4) . y Co1 N4 1.974(4) . y Co1 N7 1.979(4) . y Co1 N10 1.985(4) . y Co2 N2 1.897(3) . y Co2 N5 1.902(3) . y Co2 N8 1.905(3) . y Co2 N11 1.897(3) . y Co3 N3 2.040(4) . y Co3 N6 2.039(3) . y Co3 N9 2.047(3) . y Co3 N12 2.042(4) . y Co4 N13 1.978(3) . y Co4 N16 1.977(4) . y Co4 N19 2.043(3) . y Co4 N22 1.981(4) . y Co4 Co5 2.3173(8) . y Co5 Co6 2.3162(8) . y Co4 Br3 2.5861(7) . y Co6 Br4 2.6288(7) . y Co5 N14 1.907(3) . y Co5 N17 1.883(4) . y Co5 N20 1.892(3) . y Co5 N23 1.888(4) . y Co6 N15 1.966(3) . y Co6 N18 2.012(4) . y Co6 N21 1.988(3) . y Co6 N24 1.983(4) . y N1 C1 1.354(6) . ? N1 C5 1.362(5) . ? N2 C6 1.363(5) . ? N2 C5 1.371(6) . ? N3 C10 1.355(6) . ? N3 C6 1.373(6) . ? N4 C11 1.342(5) . ? N4 C15 1.369(5) . ? N5 C16 1.363(5) . ? N5 C15 1.376(5) . ? N6 C20 1.345(5) . ? N6 C16 1.372(5) . ? N7 C21 1.346(6) . ? N7 C25 1.360(6) . ? N8 C25 1.365(6) . ? N8 C26 1.366(6) . ? N9 C30 1.339(6) . ? N9 C26 1.370(6) . ? N10 C31 1.367(5) . ? N10 C35 1.367(6) . ? N11 C35 1.361(5) . ? N11 C36 1.373(6) . ? N12 C40 1.349(6) . ? N12 C36 1.361(5) . ? N13 C41 1.352(5) . ? N13 C45 1.368(5) . ? N14 C46 1.358(5) . ? N14 C45 1.366(5) . ? N15 C50 1.355(5) . ? N15 C46 1.363(5) . ? N16 C51 1.358(5) . ? N16 C55 1.373(5) . ? N17 C55 1.363(5) . ? N17 C56 1.369(5) . ? N18 C60 1.356(5) . ? N18 C56 1.362(6) . ? N19 C61 1.343(6) . ? N19 C65 1.377(5) . ? N20 C65 1.350(6) . ? N20 C66 1.371(6) . ? N21 C70 1.346(6) . ? N21 C66 1.364(6) . ? N22 C71 1.355(5) . ? N22 C75 1.372(6) . ? N23 C75 1.364(5) . ? N23 C76 1.368(5) . ? N24 C80 1.350(5) . ? N24 C76 1.361(5) . ? C1 C2 1.381(6) . ? C2 C3 1.383(7) . ? C3 C4 1.374(7) . ? C4 C5 1.418(6) . ? C6 C7 1.411(6) . ? C7 C8 1.381(7) . ? C8 C9 1.381(8) . ? C9 C10 1.378(7) . ? C11 C12 1.377(6) . ? C12 C13 1.388(7) . ? C13 C14 1.362(6) . ? C14 C15 1.412(6) . ? C16 C17 1.411(6) . ? C17 C18 1.367(6) . ? C18 C19 1.399(6) . ? C19 C20 1.375(6) . ? C21 C22 1.382(7) . ? C22 C23 1.389(7) . ? C23 C24 1.368(7) . ? C24 C25 1.421(6) . ? C26 C27 1.412(6) . ? C27 C28 1.371(7) . ? C28 C29 1.393(7) . ? C29 C30 1.377(6) . ? C31 C32 1.364(6) . ? C32 C33 1.393(7) . ? C33 C34 1.372(7) . ? C34 C35 1.423(6) . ? C36 C37 1.411(6) . ? C37 C38 1.372(6) . ? C38 C39 1.381(6) . ? C39 C40 1.383(6) . ? C41 C42 1.376(6) . ? C42 C43 1.386(6) . ? C43 C44 1.364(6) . ? C44 C45 1.413(6) . ? C46 C47 1.416(5) . ? C47 C48 1.370(6) . ? C48 C49 1.383(6) . ? C49 C50 1.377(6) . ? C51 C52 1.374(6) . ? C52 C53 1.400(6) . ? C53 C54 1.382(6) . ? C54 C55 1.408(6) . ? C56 C57 1.404(6) . ? C57 C58 1.364(6) . ? C58 C59 1.388(7) . ? C59 C60 1.370(7) . ? C61 C62 1.385(6) . ? C62 C63 1.397(7) . ? C63 C64 1.376(7) . ? C64 C65 1.412(6) . ? C66 C67 1.405(6) . ? C67 C68 1.371(7) . ? C68 C69 1.378(7) . ? C69 C70 1.372(6) . ? C71 C72 1.394(7) . ? C72 C73 1.392(7) . ? C73 C74 1.371(6) . ? C74 C75 1.409(6) . ? C76 C77 1.415(6) . ? C77 C78 1.362(7) . ? C78 C79 1.393(7) . ? C79 C80 1.369(6) . ? C1S C7S 1.36(2) . ? C1S C2S 1.39 . ? C1S C6S 1.39 . ? C2S C3S 1.39 . ? C3S C4S 1.39 . ? C4S C5S 1.39 . ? C5S C6S 1.39 . ? C1' C2' 1.39 . ? C1' C6' 1.39 . ? C1' C7' 1.405(15) . ? C2' C3' 1.39 . ? C3' C4' 1.39 . ? C4' C5' 1.39 . ? C5' C6' 1.39 . ? C8S C9S 1.39 . ? C8S C13S 1.39 . ? C9S C10S 1.39 . ? C10S C11S 1.39 . ? C11S C14S 1.21(2) . ? C11S C12S 1.39 . ? C12S C13S 1.39 . ? C8' C9' 1.39 . ? C8' C13' 1.39 . ? C8' C14' 1.561(14) . ? C9' C10' 1.39 . ? C10' C11' 1.39 . ? C11' C12' 1.39 . ? C12' C13' 1.39 . ? C15S C16S 1.55(3) . ? C16S C17S 1.45(3) . ? C17S C18S 1.56(3) . ? C18S C19S 1.80(2) . ? C19S C20S 0.95(2) . ? C15' C16' 1.49(2) . ? C16' C17' 1.44(2) . ? C17' C19' 1.40(2) . ? C17' C20' 1.50(2) . ? C18' C20' 1.28(2) . ? C21S C25S 1.16(2) 2_665 ? C21S C24S 1.30(2) 2_665 ? C21S C22S 1.37(2) . ? C21S C26S 1.37(2) . ? C21S C27S 1.41(2) . ? C21S C26S 1.47(2) 2_665 ? C21S C23S 1.53(2) 2_665 ? C21S C21S 1.70(2) 2_665 ? C21S C22S 1.74(2) 2_665 ? C22S C26S 0.45(2) 2_665 ? C22S C25S 1.16(2) 2_665 ? C22S C23S 1.41(2) . ? C22S C21S 1.74(2) 2_665 ? C23S C26S 1.07(2) 2_665 ? C23S C24S 1.36(2) . ? C23S C21S 1.53(2) 2_665 ? C23S C27S 1.89(2) 2_665 ? C24S C27S 0.58(2) 2_665 ? C24S C21S 1.30(2) 2_665 ? C24S C25S 1.61(2) . ? C25S C22S 1.16(2) 2_665 ? C25S C21S 1.16(2) 2_665 ? C25S C27S 1.33(2) 2_665 ? C25S C26S 1.50(2) . ? C26S C22S 0.45(2) 2_665 ? C26S C23S 1.07(2) 2_665 ? C26S C21S 1.47(2) 2_665 ? C27S C24S 0.58(2) 2_665 ? C27S C25S 1.33(2) 2_665 ? C27S C23S 1.89(2) 2_665 ? C28S C29S 1.39 . ? C28S C33S 1.39 . ? C29S C30S 1.39 . ? C30S C31S 1.39 . ? C31S C32S 1.39 . ? C31S C34S 1.65(2) . ? C32S C33S 1.39 . ? C28' C29' 1.39 . ? C28' C33' 1.39 . ? C29' C30' 1.39 . ? C30' C31' 1.39 . ? C30' C34' 1.55(2) . ? C31' C32' 1.39 . ? C32' C33' 1.39 . ? 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 Co1 Co2 Co3 178.72(3) . . y Co2 Co1 Br1 179.71(3) . . y Co2 Co3 Br2 178.60(3) . . y N4 Co1 N1 89.95(14) . . y N1 Co1 N7 90.12(15) . . y N4 Co1 N10 87.83(14) . . y N1 Co1 N10 170.6(2) . . y N4 Co1 N7 170.9(2) . . y N7 Co1 N10 90.63(14) . . y N2 Co2 N5 89.52(15) . . y N2 Co2 N8 90.40(15) . . y N11 Co2 N2 179.3(2) . . y N5 Co2 N8 179.3(2) . . y N11 Co2 N5 89.81(14) . . y N11 Co2 N8 90.26(15) . . y N6 Co3 N3 90.05(14) . . y N3 Co3 N9 92.53(14) . . y N3 Co3 N12 167.3(2) . . y N6 Co3 N9 167.34(15) . . y N6 Co3 N12 84.52(13) . . y N12 Co3 N9 90.38(14) . . y N1 Co1 Br1 93.99(11) . . y N4 Co1 Br1 95.07(11) . . y N7 Co1 Br1 93.98(12) . . y N10 Co1 Br1 95.33(11) . . y N3 Co3 Br2 95.81(11) . . y N6 Co3 Br2 97.22(10) . . y N9 Co3 Br2 94.85(11) . . y N12 Co3 Br2 96.30(11) . . y N4 Co1 Co2 85.21(12) . . ? N1 Co1 Co2 86.06(11) . . ? N7 Co1 Co2 85.74(12) . . ? N10 Co1 Co2 84.63(11) . . ? N11 Co2 Co1 90.79(12) . . ? N2 Co2 Co1 89.07(12) . . ? N5 Co2 Co1 90.00(11) . . ? N8 Co2 Co1 89.34(12) . . ? N11 Co2 Co3 90.14(12) . . ? N2 Co2 Co3 90.01(12) . . ? N5 Co2 Co3 90.89(11) . . ? N8 Co2 Co3 89.77(12) . . ? N6 Co3 Co2 83.97(10) . . ? N3 Co3 Co2 84.90(11) . . ? N12 Co3 Co2 83.08(11) . . ? N9 Co3 Co2 83.91(11) . . ? Co6 Co5 Co4 176.48(3) . . y Co5 Co4 Br3 177.10(3) . . y Co5 Co6 Br4 177.39(3) . . y N16 Co4 N13 89.18(14) . . y N13 Co4 N19 169.13(15) . . y N13 Co4 N22 88.09(14) . . y N16 Co4 N19 91.67(14) . . y N16 Co4 N22 170.44(15) . . y N22 Co4 N19 89.31(14) . . y N17 Co5 N14 89.88(15) . . y N20 Co5 N14 178.64(15) . . y N23 Co5 N14 90.23(15) . . y N17 Co5 N20 89.81(15) . . y N17 Co5 N23 179.3(2) . . y N23 Co5 N20 90.10(15) . . y N15 Co6 N18 89.16(14) . . y N15 Co6 N21 170.12(15) . . y N15 Co6 N24 90.18(14) . . y N21 Co6 N18 90.80(14) . . y N24 Co6 N18 169.02(15) . . y N24 Co6 N21 87.98(14) . . y N16 Co4 Br3 92.67(10) . . y N13 Co4 Br3 95.39(10) . . y N22 Co4 Br3 96.70(11) . . y N19 Co4 Br3 95.40(10) . . y N15 Co6 Br4 95.82(10) . . y N18 Co6 Br4 94.56(11) . . y N21 Co6 Br4 94.03(10) . . y N24 Co6 Br4 96.41(11) . . y N16 Co4 Co5 84.93(10) . . ? N13 Co4 Co5 86.23(10) . . ? N22 Co4 Co5 85.75(11) . . ? N19 Co4 Co5 83.05(10) . . ? N17 Co5 Co6 90.41(11) . . ? N23 Co5 Co6 90.33(11) . . ? N20 Co5 Co6 90.76(11) . . ? N14 Co5 Co6 87.91(10) . . ? N17 Co5 Co4 89.57(11) . . ? N23 Co5 Co4 89.70(11) . . ? N20 Co5 Co4 92.76(11) . . ? N14 Co5 Co4 88.57(10) . . ? N15 Co6 Co5 86.60(10) . . ? N24 Co6 Co5 84.56(11) . . ? N21 Co6 Co5 83.57(10) . . ? N18 Co6 Co5 84.46(11) . . ? C1 N1 C5 118.0(4) . . ? C1 N1 Co1 122.2(3) . . ? C5 N1 Co1 119.7(3) . . ? C6 N2 C5 123.1(4) . . ? C6 N2 Co2 119.1(3) . . ? C5 N2 Co2 117.7(3) . . ? C10 N3 C6 117.9(4) . . ? C10 N3 Co3 122.0(3) . . ? C6 N3 Co3 120.1(3) . . ? C11 N4 C15 118.4(4) . . ? C11 N4 Co1 121.1(3) . . ? C15 N4 Co1 120.4(3) . . ? C16 N5 C15 123.5(3) . . ? C16 N5 Co2 119.9(3) . . ? C15 N5 Co2 116.5(3) . . ? C20 N6 C16 118.3(4) . . ? C20 N6 Co3 119.6(3) . . ? C16 N6 Co3 122.0(3) . . ? C21 N7 C25 118.9(4) . . ? C21 N7 Co1 121.5(3) . . ? C25 N7 Co1 119.5(3) . . ? C25 N8 C26 123.5(4) . . ? C25 N8 Co2 118.1(3) . . ? C26 N8 Co2 118.3(3) . . ? C30 N9 C26 118.6(4) . . ? C30 N9 Co3 120.4(3) . . ? C26 N9 Co3 120.7(3) . . ? C31 N10 C35 117.9(4) . . ? C31 N10 Co1 121.6(3) . . ? C35 N10 Co1 120.4(3) . . ? C35 N11 C36 124.7(4) . . ? C35 N11 Co2 118.1(3) . . ? C36 N11 Co2 116.7(3) . . ? C40 N12 C36 118.6(4) . . ? C40 N12 Co3 119.1(3) . . ? C36 N12 Co3 121.5(3) . . ? C41 N13 C45 118.7(4) . . ? C41 N13 Co4 121.8(3) . . ? C45 N13 Co4 119.4(3) . . ? C46 N14 C45 123.9(3) . . ? C46 N14 Co5 118.3(3) . . ? C45 N14 Co5 117.7(3) . . ? C50 N15 C46 119.0(4) . . ? C50 N15 Co6 121.9(3) . . ? C46 N15 Co6 119.0(3) . . ? C51 N16 C55 117.6(4) . . ? C51 N16 Co4 122.2(3) . . ? C55 N16 Co4 120.0(3) . . ? C55 N17 C56 124.1(4) . . ? C55 N17 Co5 118.5(3) . . ? C56 N17 Co5 117.3(3) . . ? C60 N18 C56 118.1(4) . . ? C60 N18 Co6 121.8(3) . . ? C56 N18 Co6 120.1(3) . . ? C61 N19 C65 118.7(4) . . ? C61 N19 Co4 120.5(3) . . ? C65 N19 Co4 120.8(3) . . ? C65 N20 C66 126.1(3) . . ? C65 N20 Co5 117.3(3) . . ? C66 N20 Co5 116.6(3) . . ? C70 N21 C66 119.2(4) . . ? C70 N21 Co6 119.9(3) . . ? C66 N21 Co6 120.8(3) . . ? C71 N22 C75 118.2(4) . . ? C71 N22 Co4 121.7(3) . . ? C75 N22 Co4 120.1(3) . . ? C75 N23 C76 124.0(4) . . ? C75 N23 Co5 119.0(3) . . ? C76 N23 Co5 116.7(3) . . ? C80 N24 C76 118.3(4) . . ? C80 N24 Co6 120.9(3) . . ? C76 N24 Co6 120.6(3) . . ? N1 C1 C2 123.8(5) . . ? C1 C2 C3 117.8(5) . . ? C4 C3 C2 120.6(4) . . ? C3 C4 C5 118.9(5) . . ? N1 C5 N2 115.2(4) . . ? N1 C5 C4 120.9(4) . . ? N2 C5 C4 123.7(4) . . ? N2 C6 N3 116.4(4) . . ? N2 C6 C7 123.4(4) . . ? N3 C6 C7 120.1(4) . . ? C8 C7 C6 120.4(5) . . ? C7 C8 C9 118.8(5) . . ? C10 C9 C8 119.0(5) . . ? N3 C10 C9 123.6(5) . . ? N4 C11 C12 123.7(4) . . ? C11 C12 C13 118.2(4) . . ? C14 C13 C12 119.5(4) . . ? C13 C14 C15 120.4(4) . . ? N4 C15 N5 115.2(4) . . ? N4 C15 C14 119.7(4) . . ? N5 C15 C14 124.9(4) . . ? N5 C16 N6 115.3(4) . . ? N5 C16 C17 124.7(4) . . ? N6 C16 C17 120.0(4) . . ? C18 C17 C16 120.0(4) . . ? C17 C18 C19 119.9(4) . . ? C20 C19 C18 117.5(4) . . ? N6 C20 C19 124.2(4) . . ? N7 C21 C22 122.9(5) . . ? C21 C22 C23 118.8(5) . . ? C24 C23 C22 119.1(5) . . ? C23 C24 C25 120.1(5) . . ? N7 C25 N8 115.6(4) . . ? N7 C25 C24 119.9(4) . . ? N8 C25 C24 124.3(4) . . ? N8 C26 N9 115.5(4) . . ? N8 C26 C27 124.4(4) . . ? N9 C26 C27 119.8(4) . . ? C28 C27 C26 120.4(5) . . ? C27 C28 C29 119.1(4) . . ? C30 C29 C28 118.4(5) . . ? N9 C30 C29 123.8(5) . . ? C32 C31 N10 123.9(5) . . ? C31 C32 C33 118.3(5) . . ? C34 C33 C32 120.1(4) . . ? C33 C34 C35 119.3(5) . . ? N11 C35 N10 115.3(4) . . ? N11 C35 C34 124.1(5) . . ? N10 C35 C34 120.4(4) . . ? N12 C36 N11 115.1(4) . . ? N12 C36 C37 119.8(4) . . ? N11 C36 C37 124.7(4) . . ? C38 C37 C36 120.0(4) . . ? C37 C38 C39 120.2(4) . . ? C38 C39 C40 117.5(4) . . ? N12 C40 C39 123.8(4) . . ? N13 C41 C42 122.9(4) . . ? C41 C42 C43 118.8(4) . . ? C44 C43 C42 119.5(4) . . ? C43 C44 C45 120.2(4) . . ? N14 C45 N13 115.3(4) . . ? N14 C45 C44 124.5(4) . . ? N13 C45 C44 119.9(4) . . ? N14 C46 N15 115.5(3) . . ? N14 C46 C47 124.6(4) . . ? N15 C46 C47 119.6(4) . . ? C48 C47 C46 120.1(4) . . ? C47 C48 C49 119.8(4) . . ? C50 C49 C48 118.5(4) . . ? N15 C50 C49 123.0(4) . . ? N16 C51 C52 123.8(4) . . ? C51 C52 C53 119.1(4) . . ? C54 C53 C52 118.0(4) . . ? C53 C54 C55 120.7(4) . . ? N17 C55 N16 114.5(4) . . ? N17 C55 C54 124.7(4) . . ? N16 C55 C54 120.4(4) . . ? N18 C56 N17 115.1(4) . . ? N18 C56 C57 121.1(4) . . ? N17 C56 C57 123.4(4) . . ? C58 C57 C56 119.6(5) . . ? C57 C58 C59 119.2(5) . . ? C60 C59 C58 119.4(4) . . ? N18 C60 C59 122.6(5) . . ? N19 C61 C62 123.9(5) . . ? C61 C62 C63 117.9(5) . . ? C64 C63 C62 119.3(4) . . ? C63 C64 C65 120.5(4) . . ? N20 C65 N19 115.7(3) . . ? N20 C65 C64 124.4(4) . . ? N19 C65 C64 119.6(4) . . ? N21 C66 N20 115.0(4) . . ? N21 C66 C67 119.3(4) . . ? N20 C66 C67 125.3(4) . . ? C68 C67 C66 120.2(4) . . ? C67 C68 C69 119.5(4) . . ? C70 C69 C68 118.7(5) . . ? N21 C70 C69 122.7(4) . . ? N22 C71 C72 123.3(5) . . ? C73 C72 C71 118.3(4) . . ? C74 C73 C72 119.3(5) . . ? C73 C74 C75 120.5(5) . . ? N23 C75 N22 114.8(4) . . ? N23 C75 C74 124.6(4) . . ? N22 C75 C74 120.3(4) . . ? N24 C76 N23 115.4(4) . . ? N24 C76 C77 120.0(4) . . ? N23 C76 C77 124.2(4) . . ? C78 C77 C76 119.9(4) . . ? C77 C78 C79 119.9(5) . . ? C80 C79 C78 117.8(4) . . ? N24 C80 C79 124.0(4) . . ? C7S C1S C2S 117.5(9) . . ? C7S C1S C6S 122.4(9) . . ? C2S C1S C6S 120.0 . . ? C1S C2S C3S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C2' C1' C6' 120.0 . . ? C2' C1' C7' 118.7(8) . . ? C6' C1' C7' 121.3(8) . . ? C3' C2' C1' 120.0 . . ? C2' C3' C4' 120.0 . . ? C5' C4' C3' 120.0 . . ? C4' C5' C6' 120.0 . . ? C5' C6' C1' 120.0 . . ? C9S C8S C13S 120.0 . . ? C8S C9S C10S 120.0 . . ? C9S C10S C11S 120.0 . . ? C14S C11S C10S 129.1(14) . . ? C14S C11S C12S 110.5(14) . . ? C10S C11S C12S 120.0 . . ? C13S C12S C11S 120.0 . . ? C12S C13S C8S 120.0 . . ? C9' C8' C13' 120.0 . . ? C9' C8' C14' 116.6(7) . . ? C13' C8' C14' 123.4(7) . . ? C8' C9' C10' 120.0 . . ? C9' C10' C11' 120.0 . . ? C12' C11' C10' 120.0 . . ? C13' C12' C11' 120.0 . . ? C12' C13' C8' 120.0 . . ? C17S C16S C15S 106.8(18) . . ? C16S C17S C18S 115.6(18) . . ? C17S C18S C19S 129.1(14) . . ? C20S C19S C18S 138.0(20) . . ? C17' C16' C15' 126.5(12) . . ? C19' C17' C16' 127.7(14) . . ? C19' C17' C20' 127.7(15) . . ? C16' C17' C20' 104.7(13) . . ? C18' C20' C17' 129.6(14) . . ? C25S C21S C24S 81.4(13) 2_665 2_665 ? C25S C21S C22S 53.6(10) 2_665 . ? C24S C21S C22S 135.0(14) 2_665 . ? C25S C21S C26S 166.1(13) 2_665 . ? C24S C21S C26S 99.9(12) 2_665 . ? C22S C21S C26S 123.3(12) . . ? C25S C21S C27S 61.3(10) 2_665 . ? C24S C21S C27S 24.3(9) 2_665 . ? C22S C21S C27S 113.8(12) . . ? C26S C21S C27S 122.8(12) . . ? C25S C21S C26S 68.5(11) 2_665 2_665 ? C24S C21S C26S 147.4(14) 2_665 2_665 ? C22S C21S C26S 17.8(8) . 2_665 ? C26S C21S C26S 106.4(10) . 2_665 ? C27S C21S C26S 129.8(12) . 2_665 ? C25S C21S C23S 136.2(13) 2_665 2_665 ? C24S C21S C23S 56.8(10) 2_665 2_665 ? C22S C21S C23S 163.1(12) . 2_665 ? C26S C21S C23S 43.1(8) . 2_665 ? C27S C21S C23S 80.1(10) . 2_665 ? C26S C21S C23S 145.5(12) 2_665 2_665 ? C25S C21S C21S 117.8(13) 2_665 2_665 ? C24S C21S C21S 149.7(15) 2_665 2_665 ? C22S C21S C21S 67.8(9) . 2_665 ? C26S C21S C21S 55.7(9) . 2_665 ? C27S C21S C21S 170.9(13) . 2_665 ? C26S C21S C21S 50.6(7) 2_665 2_665 ? C23S C21S C21S 97.0(11) 2_665 2_665 ? C25S C21S C22S 157.8(12) 2_665 2_665 ? C24S C21S C22S 106.8(12) 2_665 2_665 ? C22S C21S C22S 114.7(9) . 2_665 ? C26S C21S C22S 9.8(9) . 2_665 ? C27S C21S C22S 130.6(11) . 2_665 ? C26S C21S C22S 97.4(9) 2_665 2_665 ? C23S C21S C22S 50.5(8) 2_665 2_665 ? C21S C21S C22S 47.0(7) 2_665 2_665 ? C26S C22S C25S 133.4(39) 2_665 2_665 ? C26S C22S C21S 93.4(33) 2_665 . ? C25S C22S C21S 53.9(10) 2_665 . ? C26S C22S C23S 35.9(30) 2_665 . ? C25S C22S C23S 168.9(16) 2_665 . ? C21S C22S C23S 121.5(12) . . ? C26S C22S C21S 31.2(28) 2_665 2_665 ? C25S C22S C21S 115.7(13) 2_665 2_665 ? C21S C22S C21S 65.3(9) . 2_665 ? C23S C22S C21S 57.0(8) . 2_665 ? C26S C23S C24S 113.9(15) 2_665 . ? C26S C23S C22S 14.2(11) 2_665 . ? C24S C23S C22S 124.9(13) . . ? C26S C23S C21S 60.7(10) 2_665 2_665 ? C24S C23S C21S 53.1(9) . 2_665 ? C22S C23S C21S 72.5(10) . 2_665 ? C26S C23S C27S 107.7(13) 2_665 2_665 ? C24S C23S C27S 8.3(10) . 2_665 ? C22S C23S C27S 119.7(11) . 2_665 ? C21S C23S C27S 47.3(7) 2_665 2_665 ? C27S C24S C21S 88.7(30) 2_665 2_665 ? C27S C24S C23S 152.1(36) 2_665 . ? C21S C24S C23S 70.1(12) 2_665 . ? C27S C24S C25S 51.8(25) 2_665 . ? C21S C24S C25S 45.6(9) 2_665 . ? C23S C24S C25S 114.4(14) . . ? C22S C25S C21S 72.5(13) 2_665 2_665 ? C22S C25S C27S 139.3(17) 2_665 2_665 ? C21S C25S C27S 68.7(11) 2_665 2_665 ? C22S C25S C26S 12.6(11) 2_665 . ? C21S C25S C26S 65.5(11) 2_665 . ? C27S C25S C26S 134.1(14) 2_665 . ? C22S C25S C24S 125.6(15) 2_665 . ? C21S C25S C24S 53.0(10) 2_665 . ? C27S C25S C24S 20.1(10) 2_665 . ? C26S C25S C24S 117.3(13) . . ? C22S C26S C23S 129.9(39) 2_665 2_665 ? C22S C26S C21S 139.0(36) 2_665 . ? C23S C26S C21S 76.1(12) 2_665 . ? C22S C26S C21S 68.8(31) 2_665 2_665 ? C23S C26S C21S 144.2(15) 2_665 2_665 ? C21S C26S C21S 73.6(10) . 2_665 ? C22S C26S C25S 34.0(30) 2_665 . ? C23S C26S C25S 163.6(15) 2_665 . ? C21S C26S C25S 118.4(12) . . ? C21S C26S C25S 46.0(8) 2_665 . ? C24S C27S C25S 108.1(31) 2_665 2_665 ? C24S C27S C21S 67.0(28) 2_665 . ? C25S C27S C21S 50.0(9) 2_665 . ? C24S C27S C23S 19.6(26) 2_665 2_665 ? C25S C27S C23S 100.2(12) 2_665 2_665 ? C21S C27S C23S 52.7(8) . 2_665 ? C29S C28S C33S 120.0 . . ? C30S C29S C28S 120.0 . . ? C29S C30S C31S 120.0 . . ? C30S C31S C32S 120.0 . . ? C30S C31S C34S 120.7(9) . . ? C32S C31S C34S 119.1(9) . . ? C31S C32S C33S 120.0 . . ? C32S C33S C28S 120.0 . . ? C29' C28' C33' 120.0 . . ? C28' C29' C30' 120.0 . . ? C31' C30' C29' 120.0 . . ? C31' C30' C34' 120.0(7) . . ? C29' C30' C34' 119.1(7) . . ? C30' C31' C32' 120.0 . . ? C31' C32' C33' 120.0 . . ? C32' C33' C28' 120.0 . . ? _refine_diff_density_max 1.483 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.111 #===END data_1-1.75C7H8.0.5C6H14_at_170K _audit_creation_method SHELXL _chemical_formula_structural 'Co3(dpa)4Br2.1.75Tol.0.5Hex' _chemical_formula_sum 'C55.25 H53 Br2 Co3 N12' _chemical_formula_weight 1221.71 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.927(1) _cell_length_b 18.155(1) _cell_length_c 19.293(1) _cell_angle_alpha 81.395(1) _cell_angle_beta 82.475(2) _cell_angle_gamma 62.438(1) _cell_volume 5183.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 4908 _cell_measurement_theta_min 2.363 _cell_measurement_theta_max 27.497 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method ? _exptl_crystal_F_000 2478 _exptl_absorpt_coefficient_mu 2.541 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.4128 _exptl_absorpt_correction_T_max 0.7728 _diffrn_ambient_temperature 170(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35531 _diffrn_reflns_av_R_equivalents 0.0379 _diffrn_reflns_av_sigmaI/netI 0.0807 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.52 _reflns_number_total 22927 _reflns_number_observed 13681 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0601P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22926 _refine_ls_number_parameters 1198 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0993 _refine_ls_R_factor_obs 0.0491 _refine_ls_wR_factor_all 0.1352 _refine_ls_wR_factor_obs 0.1160 _refine_ls_goodness_of_fit_all 1.012 _refine_ls_goodness_of_fit_obs 1.142 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.143 _refine_ls_shift/esd_max -0.011 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.05316(4) 0.72577(4) 0.08895(3) 0.02630(15) Uani 1 d . -1 Co2 Co -0.00846(4) 0.67905(4) 0.18876(3) 0.02175(14) Uani 1 d . -1 Co3 Co -0.07640(4) 0.62933(4) 0.29175(3) 0.0287(2) Uani 1 d . -1 Br1 Br 0.12182(4) 0.77836(4) -0.02330(3) 0.0465(2) Uani 1 d . -1 Br2 Br -0.14683(4) 0.57441(3) 0.40079(3) 0.03838(13) Uani 1 d . -1 Br3 Br 0.42955(3) 0.27884(3) 0.23831(3) 0.03736(13) Uani 1 d . -1 Co4 Co 0.53302(4) 0.24113(4) 0.34128(3) 0.02181(14) Uani 1 d . -1 Co5 Co 0.62040(4) 0.21298(4) 0.43367(3) 0.02004(13) Uani 1 d . -1 Co6 Co 0.71456(4) 0.17782(4) 0.52541(3) 0.02473(15) Uani 1 d . -1 N13 N 0.4443(2) 0.2294(2) 0.4163(2) 0.0246(8) Uani 1 d . -1 N14 N 0.5613(2) 0.1549(2) 0.4872(2) 0.0211(8) Uani 1 d . -1 N15 N 0.6871(2) 0.0797(2) 0.5490(2) 0.0260(9) Uani 1 d . -1 N16 N 0.5900(2) 0.1196(2) 0.3369(2) 0.0234(8) Uani 1 d . -1 N17 N 0.7044(2) 0.1127(2) 0.3948(2) 0.0211(8) Uani 1 d . -1 N18 N 0.8127(2) 0.1126(2) 0.4555(2) 0.0245(8) Uani 1 d . -1 N19 N 0.6347(2) 0.2482(2) 0.2821(2) 0.0245(8) Uani 1 d . -1 N20 N 0.6800(2) 0.2714(2) 0.3810(2) 0.0225(8) Uani 1 d . -1 N21 N 0.7299(2) 0.2794(2) 0.4837(2) 0.0283(9) Uani 1 d . -1 N22 N 0.4899(2) 0.3593(2) 0.3585(2) 0.0245(8) Uani 1 d . -1 N23 N 0.5348(2) 0.3131(2) 0.4708(2) 0.0213(8) Uani 1 d . -1 N24 N 0.5965(2) 0.2554(2) 0.5777(2) 0.0256(9) Uani 1 d . -1 C41 C 0.3552(3) 0.2678(3) 0.4078(3) 0.0308(11) Uani 1 d . -1 H41A H 0.3348(3) 0.2988(3) 0.3641(3) 0.037 Uiso 1 calc R -1 C42 C 0.2938(3) 0.2636(3) 0.4596(3) 0.0401(13) Uani 1 d . -1 H42A H 0.2320(3) 0.2916(3) 0.4516(3) 0.048 Uiso 1 calc R -1 C43 C 0.3217(3) 0.2186(3) 0.5237(3) 0.0440(14) Uani 1 d . -1 H43A H 0.2797(3) 0.2150(3) 0.5601(3) 0.053 Uiso 1 calc R -1 C44 C 0.4109(3) 0.1795(3) 0.5336(3) 0.0354(12) Uani 1 d . -1 H44A H 0.4315(3) 0.1486(3) 0.5774(3) 0.043 Uiso 1 calc R -1 C45 C 0.4720(3) 0.1849(3) 0.4792(3) 0.0240(10) Uani 1 d . -1 C46 C 0.6097(3) 0.0851(3) 0.5298(2) 0.0256(10) Uani 1 d . -1 C47 C 0.5893(3) 0.0172(3) 0.5482(3) 0.0309(11) Uani 1 d . -1 H47A H 0.5333(3) 0.0228(3) 0.5380(3) 0.037 Uiso 1 calc R -1 C48 C 0.6495(3) -0.0568(3) 0.5808(3) 0.0385(13) Uani 1 d . -1 H48A H 0.6357(3) -0.1024(3) 0.5934(3) 0.046 Uiso 1 calc R -1 C49 C 0.7318(3) -0.0634(3) 0.5949(3) 0.0390(13) Uani 1 d . -1 H49A H 0.7763(3) -0.1144(3) 0.6153(3) 0.047 Uiso 1 calc R -1 C50 C 0.7468(3) 0.0054(3) 0.5788(3) 0.0329(12) Uani 1 d . -1 H50A H 0.8024(3) 0.0006(3) 0.5891(3) 0.039 Uiso 1 calc R -1 C51 C 0.5485(3) 0.0814(3) 0.3120(2) 0.0287(11) Uani 1 d . -1 H51A H 0.4907(3) 0.1150(3) 0.2954(2) 0.034 Uiso 1 calc R -1 C52 C 0.5859(3) -0.0033(3) 0.3095(3) 0.0323(11) Uani 1 d . -1 H52A H 0.5546(3) -0.0278(3) 0.2921(3) 0.039 Uiso 1 calc R -1 C53 C 0.6708(3) -0.0523(3) 0.3332(3) 0.0299(11) Uani 1 d . -1 H53A H 0.6989(3) -0.1110(3) 0.3310(3) 0.036 Uiso 1 calc R -1 C54 C 0.7135(3) -0.0162(3) 0.3596(2) 0.0248(10) Uani 1 d . -1 H54A H 0.7713(3) -0.0497(3) 0.3762(2) 0.030 Uiso 1 calc R -1 C55 C 0.6717(3) 0.0718(3) 0.3623(2) 0.0215(9) Uani 1 d . -1 C56 C 0.7931(3) 0.0868(3) 0.4001(2) 0.0234(10) Uani 1 d . -1 C57 C 0.8612(3) 0.0443(3) 0.3494(3) 0.0294(11) Uani 1 d . -1 H57A H 0.8473(3) 0.0265(3) 0.3108(3) 0.035 Uiso 1 calc R -1 C58 C 0.9473(3) 0.0286(3) 0.3560(3) 0.0348(12) Uani 1 d . -1 H58A H 0.9933(3) 0.0003(3) 0.3218(3) 0.042 Uiso 1 calc R -1 C59 C 0.9667(3) 0.0542(3) 0.4125(3) 0.0342(12) Uani 1 d . -1 H59A H 1.0264(3) 0.0424(3) 0.4185(3) 0.041 Uiso 1 calc R -1 C60 C 0.8983(3) 0.0971(3) 0.4602(3) 0.0325(12) Uani 1 d . -1 H60A H 0.9117(3) 0.1167(3) 0.4979(3) 0.039 Uiso 1 calc R -1 C61 C 0.6505(3) 0.2312(3) 0.2143(2) 0.0299(11) Uani 1 d . -1 H61A H 0.6106(3) 0.2174(3) 0.1954(2) 0.036 Uiso 1 calc R -1 C62 C 0.7212(3) 0.2329(3) 0.1714(3) 0.0373(12) Uani 1 d . -1 H62A H 0.7292(3) 0.2218(3) 0.1238(3) 0.045 Uiso 1 calc R -1 C63 C 0.7803(3) 0.2511(3) 0.1995(3) 0.0400(13) Uani 1 d . -1 H63A H 0.8302(3) 0.2522(3) 0.1712(3) 0.048 Uiso 1 calc R -1 C64 C 0.7671(3) 0.2674(3) 0.2675(3) 0.0320(11) Uani 1 d . -1 H64A H 0.8077(3) 0.2802(3) 0.2867(3) 0.038 Uiso 1 calc R -1 C65 C 0.6936(3) 0.2655(3) 0.3099(2) 0.0246(10) Uani 1 d . -1 C66 C 0.7142(3) 0.3098(3) 0.4151(2) 0.0249(10) Uani 1 d . -1 C67 C 0.7251(3) 0.3806(3) 0.3862(3) 0.0387(13) Uani 1 d . -1 H67A H 0.7114(3) 0.4028(3) 0.3391(3) 0.046 Uiso 1 calc R -1 C68 C 0.7554(3) 0.4175(3) 0.4257(3) 0.0427(14) Uani 1 d . -1 H68A H 0.7644(3) 0.4645(3) 0.4058(3) 0.051 Uiso 1 calc R -1 C69 C 0.7731(4) 0.3862(3) 0.4950(3) 0.0465(15) Uani 1 d . -1 H69A H 0.7952(4) 0.4105(3) 0.5231(3) 0.056 Uiso 1 calc R -1 C70 C 0.7579(3) 0.3191(3) 0.5221(3) 0.0376(13) Uani 1 d . -1 H70A H 0.7674(3) 0.2993(3) 0.5702(3) 0.045 Uiso 1 calc R -1 C71 C 0.4653(3) 0.4198(3) 0.3044(3) 0.0321(11) Uani 1 d . -1 H71A H 0.4694(3) 0.4043(3) 0.2587(3) 0.038 Uiso 1 calc R -1 C72 C 0.4346(3) 0.5026(3) 0.3124(3) 0.0345(12) Uani 1 d . -1 H72A H 0.4187(3) 0.5436(3) 0.2730(3) 0.041 Uiso 1 calc R -1 C73 C 0.4275(3) 0.5248(3) 0.3787(3) 0.0386(13) Uani 1 d . -1 H73A H 0.4038(3) 0.5820(3) 0.3860(3) 0.046 Uiso 1 calc R -1 C74 C 0.4545(3) 0.4646(3) 0.4342(3) 0.0321(11) Uani 1 d . -1 H74A H 0.4492(3) 0.4801(3) 0.4801(3) 0.038 Uiso 1 calc R -1 C75 C 0.4902(3) 0.3797(3) 0.4237(3) 0.0256(10) Uani 1 d . -1 C76 C 0.5249(3) 0.3138(3) 0.5420(3) 0.0253(10) Uani 1 d . -1 C77 C 0.4456(3) 0.3649(3) 0.5792(3) 0.0343(12) Uani 1 d . -1 H77A H 0.3953(3) 0.4037(3) 0.5544(3) 0.041 Uiso 1 calc R -1 C78 C 0.4403(4) 0.3593(3) 0.6511(3) 0.0397(13) Uani 1 d . -1 H78A H 0.3872(4) 0.3950(3) 0.6761(3) 0.048 Uiso 1 calc R -1 C79 C 0.5136(4) 0.3008(3) 0.6870(3) 0.0407(13) Uani 1 d . -1 H79A H 0.5118(4) 0.2961(3) 0.7368(3) 0.049 Uiso 1 calc R -1 C80 C 0.5893(3) 0.2494(3) 0.6481(3) 0.0335(12) Uani 1 d . -1 H80A H 0.6385(3) 0.2078(3) 0.6727(3) 0.040 Uiso 1 calc R -1 Br4 Br 0.81313(3) 0.13659(3) 0.62852(3) 0.03654(13) Uani 1 d . -1 N1 N -0.0264(3) 0.8388(2) 0.1155(2) 0.0304(9) Uani 1 d . -1 N2 N -0.1133(2) 0.7830(2) 0.1829(2) 0.0249(8) Uani 1 d . -1 N3 N -0.1949(3) 0.7237(2) 0.2544(2) 0.0286(9) Uani 1 d . -1 N4 N 0.1422(2) 0.7157(2) 0.1510(2) 0.0271(9) Uani 1 d . -1 N5 N 0.0398(2) 0.7236(2) 0.2454(2) 0.0225(8) Uani 1 d . -1 N6 N -0.0589(2) 0.7175(2) 0.3376(2) 0.0228(8) Uani 1 d . -1 N7 N -0.0437(3) 0.7281(2) 0.0402(2) 0.0307(9) Uani 1 d . -1 N8 N -0.0558(2) 0.6346(2) 0.1307(2) 0.0263(9) Uani 1 d . -1 N9 N -0.0704(2) 0.5467(2) 0.2253(2) 0.0273(9) Uani 1 d . -1 N10 N 0.1269(2) 0.6057(2) 0.0768(2) 0.0291(9) Uani 1 d . -1 N11 N 0.0971(2) 0.5760(2) 0.1948(2) 0.0251(9) Uani 1 d . -1 N12 N 0.0568(2) 0.5535(2) 0.3118(2) 0.0274(9) Uani 1 d . -1 C1 C -0.0073(4) 0.9040(3) 0.0957(3) 0.0397(13) Uani 1 d . -1 H1A H 0.0468(4) 0.8942(3) 0.0681(3) 0.048 Uiso 1 calc R -1 C2 C -0.0623(4) 0.9839(3) 0.1136(3) 0.049(2) Uani 1 d . -1 H2A H -0.0472(4) 1.0282(3) 0.0975(3) 0.059 Uiso 1 calc R -1 C3 C -0.1395(4) 0.9982(3) 0.1554(3) 0.0454(14) Uani 1 d . -1 H3A H -0.1784(4) 1.0529(3) 0.1680(3) 0.054 Uiso 1 calc R -1 C4 C -0.1603(3) 0.9338(3) 0.1788(3) 0.0365(12) Uani 1 d . -1 H4A H -0.2127(3) 0.9430(3) 0.2086(3) 0.044 Uiso 1 calc R -1 C5 C -0.1020(3) 0.8528(3) 0.1579(2) 0.0271(10) Uani 1 d . -1 C6 C -0.1945(3) 0.7858(3) 0.2042(2) 0.0262(10) Uani 1 d . -1 C7 C -0.2745(3) 0.8460(3) 0.1749(3) 0.0346(12) Uani 1 d . -1 H7A H -0.2732(3) 0.8869(3) 0.1384(3) 0.041 Uiso 1 calc R -1 C8 C -0.3541(3) 0.8453(3) 0.1993(3) 0.0419(14) Uani 1 d . -1 H8A H -0.4082(3) 0.8855(3) 0.1797(3) 0.050 Uiso 1 calc R -1 C9 C -0.3551(4) 0.7857(4) 0.2524(3) 0.047(2) Uani 1 d . -1 H9A H -0.4099(4) 0.7861(4) 0.2718(3) 0.056 Uiso 1 calc R -1 C10 C -0.2750(3) 0.7257(3) 0.2769(3) 0.0379(13) Uani 1 d . -1 H10A H -0.2759(3) 0.6831(3) 0.3117(3) 0.045 Uiso 1 calc R -1 C11 C 0.2247(3) 0.7026(3) 0.1251(3) 0.0355(12) Uani 1 d . -1 H11A H 0.2393(3) 0.6974(3) 0.0762(3) 0.043 Uiso 1 calc R -1 C12 C 0.2893(3) 0.6962(3) 0.1654(3) 0.0402(13) Uani 1 d . -1 H12A H 0.3466(3) 0.6881(3) 0.1448(3) 0.048 Uiso 1 calc R -1 C13 C 0.2680(3) 0.7021(3) 0.2373(3) 0.0350(12) Uani 1 d . -1 H13A H 0.3105(3) 0.6990(3) 0.2667(3) 0.042 Uiso 1 calc R -1 C14 C 0.1864(3) 0.7123(3) 0.2647(3) 0.0293(11) Uani 1 d . -1 H14A H 0.1724(3) 0.7146(3) 0.3139(3) 0.035 Uiso 1 calc R -1 C15 C 0.1220(3) 0.7197(3) 0.2219(2) 0.0237(10) Uani 1 d . -1 C16 C -0.0025(3) 0.7501(3) 0.3088(2) 0.0220(9) Uani 1 d . -1 C17 C 0.0068(3) 0.8085(3) 0.3428(3) 0.0274(10) Uani 1 d . -1 H17A H 0.0440(3) 0.8331(3) 0.3214(3) 0.033 Uiso 1 calc R -1 C18 C -0.0374(3) 0.8299(3) 0.4064(3) 0.0300(11) Uani 1 d . -1 H18A H -0.0298(3) 0.8682(3) 0.4301(3) 0.036 Uiso 1 calc R -1 C19 C -0.0935(3) 0.7955(3) 0.4367(3) 0.0337(12) Uani 1 d . -1 H19A H -0.1247(3) 0.8094(3) 0.4812(3) 0.040 Uiso 1 calc R -1 C20 C -0.1026(3) 0.7409(3) 0.4002(2) 0.0290(11) Uani 1 d . -1 H20A H -0.1419(3) 0.7181(3) 0.4203(2) 0.035 Uiso 1 calc R -1 C21 C -0.0744(4) 0.7798(3) -0.0179(3) 0.0408(13) Uani 1 d . -1 H21A H -0.0503(4) 0.8178(3) -0.0344(3) 0.049 Uiso 1 calc R -1 C22 C -0.1394(4) 0.7806(4) -0.0547(3) 0.052(2) Uani 1 d . -1 H22A H -0.1605(4) 0.8190(4) -0.0952(3) 0.062 Uiso 1 calc R -1 C23 C -0.1734(4) 0.7242(4) -0.0316(3) 0.049(2) Uani 1 d . -1 H23A H -0.2159(4) 0.7214(4) -0.0574(3) 0.059 Uiso 1 calc R -1 C24 C -0.1450(3) 0.6731(3) 0.0284(3) 0.0389(13) Uani 1 d . -1 H24A H -0.1687(3) 0.6349(3) 0.0452(3) 0.047 Uiso 1 calc R -1 C25 C -0.0809(3) 0.6763(3) 0.0658(2) 0.0276(11) Uani 1 d . -1 C26 C -0.0604(3) 0.5618(3) 0.1541(3) 0.0281(11) Uani 1 d . -1 C27 C -0.0475(3) 0.5014(3) 0.1105(3) 0.0371(13) Uani 1 d . -1 H27A H -0.0395(3) 0.5118(3) 0.0610(3) 0.045 Uiso 1 calc R -1 C28 C -0.0466(4) 0.4271(3) 0.1394(3) 0.0439(14) Uani 1 d . -1 H28A H -0.0380(4) 0.3860(3) 0.1100(3) 0.053 Uiso 1 calc R -1 C29 C -0.0584(4) 0.4127(3) 0.2115(3) 0.0448(14) Uani 1 d . -1 H29A H -0.0599(4) 0.3625(3) 0.2324(3) 0.054 Uiso 1 calc R -1 C30 C -0.0677(3) 0.4720(3) 0.2518(3) 0.0376(12) Uani 1 d . -1 H30A H -0.0727(3) 0.4605(3) 0.3014(3) 0.045 Uiso 1 calc R -1 C31 C 0.1639(3) 0.5786(3) 0.0125(3) 0.0340(12) Uani 1 d . -1 H31A H 0.1485(3) 0.6185(3) -0.0276(3) 0.041 Uiso 1 calc R -1 C32 C 0.2216(3) 0.4976(4) 0.0026(3) 0.0439(15) Uani 1 d . -1 H32A H 0.2452(3) 0.4815(4) -0.0432(3) 0.053 Uiso 1 calc R -1 C33 C 0.2448(4) 0.4396(4) 0.0611(3) 0.0444(15) Uani 1 d . -1 H33A H 0.2872(4) 0.3834(4) 0.0558(3) 0.053 Uiso 1 calc R -1 C34 C 0.2071(3) 0.4626(3) 0.1265(3) 0.0369(12) Uani 1 d . -1 H34A H 0.2218(3) 0.4223(3) 0.1664(3) 0.044 Uiso 1 calc R -1 C35 C 0.1459(3) 0.5473(3) 0.1340(3) 0.0294(11) Uani 1 d . -1 C36 C 0.1238(3) 0.5395(3) 0.2609(2) 0.0241(10) Uani 1 d . -1 C37 C 0.2139(3) 0.4985(3) 0.2781(3) 0.0319(11) Uani 1 d . -1 H37A H 0.2608(3) 0.4891(3) 0.2424(3) 0.038 Uiso 1 calc R -1 C38 C 0.2328(3) 0.4721(3) 0.3476(3) 0.0364(12) Uani 1 d . -1 H38A H 0.2931(3) 0.4445(3) 0.3597(3) 0.044 Uiso 1 calc R -1 C39 C 0.1650(3) 0.4856(3) 0.3993(3) 0.0355(12) Uani 1 d . -1 H39A H 0.1774(3) 0.4674(3) 0.4472(3) 0.043 Uiso 1 calc R -1 C40 C 0.0779(3) 0.5269(3) 0.3793(3) 0.0295(11) Uani 1 d . -1 H40A H 0.0306(3) 0.5369(3) 0.4148(3) 0.035 Uiso 1 calc R -1 C1S C -0.4178(8) 0.6450(6) 0.1143(7) 0.079(6) Uiso 0.40 d PG 1 C2S C -0.4330(6) 0.5753(7) 0.1309(7) 0.032(3) Uiso 0.40 d PGD 1 C3S C -0.3751(9) 0.5063(6) 0.1722(8) 0.107(10) Uiso 0.40 d PG 1 C4S C -0.3020(7) 0.5071(6) 0.1969(7) 0.056(4) Uiso 0.40 d PG 1 C5S C -0.2867(6) 0.5769(7) 0.1803(6) 0.037(3) Uiso 0.40 d PG 1 C6S C -0.3446(9) 0.6459(6) 0.1390(8) 0.051(5) Uiso 0.40 d PGD 1 C7S C -0.4748(11) 0.7073(11) 0.0717(10) 0.070(5) Uiso 0.40 d PD 1 C1' C -0.3917(9) 0.6679(6) 0.1112(6) 0.135(7) Uiso 0.60 d PG 2 C2' C -0.4468(7) 0.6320(8) 0.1043(6) 0.084(4) Uiso 0.60 d PG 2 C3' C -0.4307(9) 0.5545(8) 0.1400(8) 0.135(8) Uiso 0.60 d PG 2 C4' C -0.3595(10) 0.5129(6) 0.1826(8) 0.100(6) Uiso 0.60 d PG 2 C5' C -0.3044(7) 0.5487(8) 0.1896(6) 0.132(6) Uiso 0.60 d PG 2 C6' C -0.3205(7) 0.6262(8) 0.1539(7) 0.058(3) Uiso 0.60 d PG 2 C7' C -0.4084(12) 0.7404(12) 0.0730(10) 0.135(6) Uiso 0.60 d P 2 C8S C 0.0012(7) 0.2459(9) 0.3731(7) 0.103(5) Uiso 0.60 d PG 1 C9S C 0.0428(9) 0.1997(7) 0.3162(8) 0.088(4) Uiso 0.60 d PG 1 C10S C 0.1113(9) 0.2105(8) 0.2750(6) 0.107(6) Uiso 0.60 d PG 1 C11S C 0.1381(7) 0.2674(9) 0.2908(7) 0.098(5) Uiso 0.60 d PG 1 C12S C 0.0965(10) 0.3136(7) 0.3477(8) 0.085(4) Uiso 0.60 d PG 1 C13S C 0.0281(9) 0.3029(8) 0.3889(6) 0.101(6) Uiso 0.60 d PG 1 C14S C 0.1891(13) 0.2899(12) 0.2612(11) 0.115(7) Uiso 0.50 d P 1 C8' C 0.0873(9) 0.2030(7) 0.2889(6) 0.035(3) Uiso 0.40 d PG 2 C9' C 0.0228(8) 0.2257(8) 0.3448(7) 0.054(4) Uiso 0.40 d PGD 2 C10' C 0.0148(8) 0.2858(9) 0.3858(6) 0.066(6) Uiso 0.40 d PG 2 C11' C 0.0715(9) 0.3232(7) 0.3711(7) 0.043(4) Uiso 0.40 d PG 2 C12' C 0.1360(8) 0.3005(8) 0.3153(7) 0.052(4) Uiso 0.40 d PG 2 C13' C 0.1439(8) 0.2404(9) 0.2742(6) 0.083(6) Uiso 0.40 d PGD 2 C14' C 0.0909(12) 0.1340(12) 0.2441(10) 0.108(6) Uiso 0.50 d PD 2 C15S C 0.1436(21) -0.0390(21) 0.1710(19) 0.215(13) Uiso 0.50 d P 1 C16S C 0.1683(16) -0.0143(15) 0.1002(14) 0.115(8) Uiso 0.50 d P 1 C17S C 0.2406(16) -0.0843(16) 0.0588(13) 0.128(8) Uiso 0.50 d P 1 C18S C 0.2817(18) -0.0737(18) -0.0081(15) 0.122(10) Uiso 0.50 d P 1 C19S C 0.3703(15) -0.1233(15) -0.0621(13) 0.109(7) Uiso 0.50 d P 1 C20S C 0.4076(12) -0.1181(11) -0.0964(10) 0.084(5) Uiso 0.50 d P 1 C15' C 0.3714(10) -0.0498(9) -0.0804(8) 0.069(4) Uiso 0.50 d P 2 C16' C 0.2959(9) -0.0141(8) -0.0274(7) 0.058(3) Uiso 0.50 d P 2 C17' C 0.2564(11) -0.0520(10) 0.0086(9) 0.050(4) Uiso 0.50 d P 2 C18' C 0.3724(11) -0.1756(11) -0.0450(9) 0.082(5) Uiso 0.50 d P 2 C19' C 0.1775(16) -0.0265(15) 0.0639(13) 0.105(7) Uiso 0.50 d P 2 C20' C 0.3037(10) -0.1461(10) -0.0014(8) 0.069(4) Uiso 0.50 d P 2 C21S C 0.4885(10) 0.4679(9) 0.0301(8) 0.066(4) Uiso 0.50 d P . C22S C 0.4107(10) 0.5374(10) 0.0197(9) 0.057(2) Uiso 0.50 d PD . C23S C 0.4077(11) 0.5971(10) -0.0375(9) 0.078(4) Uiso 0.50 d P . C24S C 0.4765(13) 0.5981(11) -0.0805(10) 0.081(5) Uiso 0.50 d P . C25S C 0.5755(12) 0.5116(12) -0.0659(10) 0.084(5) Uiso 0.50 d P . C26S C 0.5692(10) 0.4526(10) -0.0028(9) 0.057(2) Uiso 0.50 d PD . C27S C 0.4783(12) 0.4174(11) 0.0868(10) 0.077(5) Uiso 0.50 d PD . C28S C 0.3855(12) 0.1276(8) 0.1488(10) 0.087(6) Uiso 0.40 d PG 1 C29S C 0.4039(13) 0.0828(11) 0.0913(7) 0.143(12) Uiso 0.40 d PG 1 C30S C 0.4048(12) 0.0050(10) 0.1004(7) 0.072(5) Uiso 0.40 d PG 1 C31S C 0.3871(12) -0.0280(8) 0.1669(9) 0.097(7) Uiso 0.40 d PG 1 C32S C 0.3687(13) 0.0168(11) 0.2244(7) 0.109(8) Uiso 0.40 d PG 1 C33S C 0.3678(12) 0.0946(10) 0.2153(8) 0.085(6) Uiso 0.40 d PG 1 C34S C 0.3747(13) -0.1276(13) 0.1820(11) 0.113(6) Uiso 0.50 d P 1 C28' C 0.3936(6) -0.0658(4) 0.1793(5) 0.083(4) Uiso 0.60 d PG 2 C29' C 0.4088(6) -0.0298(5) 0.1133(4) 0.047(3) Uiso 0.60 d PG 2 C30' C 0.4049(7) 0.0491(6) 0.1062(4) 0.089(4) Uiso 0.60 d PG 2 C31' C 0.3858(7) 0.0920(5) 0.1649(5) 0.079(4) Uiso 0.60 d PG 2 C32' C 0.3706(7) 0.0560(6) 0.2308(4) 0.064(3) Uiso 0.60 d PG 2 C33' C 0.3745(7) -0.0229(6) 0.2380(4) 0.071(3) Uiso 0.60 d PG 2 C34' C 0.3999(13) 0.0924(12) 0.0326(11) 0.113(6) Uiso 0.50 d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0279(3) 0.0320(4) 0.0208(3) -0.0055(3) 0.0022(3) -0.0152(3) Co2 0.0213(3) 0.0229(3) 0.0206(3) -0.0048(2) 0.0004(2) -0.0093(2) Co3 0.0298(3) 0.0277(3) 0.0272(4) -0.0073(3) -0.0032(3) -0.0103(3) Br1 0.0534(4) 0.0628(4) 0.0293(3) -0.0054(3) 0.0095(3) -0.0342(3) Br2 0.0479(3) 0.0436(3) 0.0321(3) -0.0044(2) 0.0062(2) -0.0299(3) Br3 0.0352(3) 0.0364(3) 0.0370(3) -0.0014(2) -0.0110(2) -0.0118(2) Co4 0.0198(3) 0.0181(3) 0.0256(3) -0.0029(3) -0.0014(3) -0.0068(2) Co5 0.0172(3) 0.0186(3) 0.0235(3) -0.0045(2) 0.0002(2) -0.0071(2) Co6 0.0212(3) 0.0239(3) 0.0295(4) -0.0079(3) 0.0015(3) -0.0098(3) N13 0.025(2) 0.019(2) 0.032(2) -0.005(2) -0.002(2) -0.011(2) N14 0.016(2) 0.022(2) 0.024(2) -0.005(2) -0.001(2) -0.0059(15) N15 0.020(2) 0.028(2) 0.027(2) -0.006(2) -0.003(2) -0.006(2) N16 0.021(2) 0.022(2) 0.027(2) -0.003(2) -0.001(2) -0.010(2) N17 0.020(2) 0.021(2) 0.023(2) -0.007(2) 0.000(2) -0.008(2) N18 0.019(2) 0.021(2) 0.031(2) -0.002(2) -0.005(2) -0.007(2) N19 0.026(2) 0.018(2) 0.026(2) 0.000(2) -0.002(2) -0.008(2) N20 0.023(2) 0.024(2) 0.022(2) -0.005(2) 0.005(2) -0.012(2) N21 0.021(2) 0.030(2) 0.035(2) -0.014(2) 0.003(2) -0.011(2) N22 0.019(2) 0.024(2) 0.029(2) -0.002(2) -0.002(2) -0.009(2) N23 0.020(2) 0.019(2) 0.024(2) -0.004(2) 0.000(2) -0.008(2) N24 0.026(2) 0.032(2) 0.025(2) -0.008(2) 0.003(2) -0.018(2) C41 0.016(2) 0.023(2) 0.047(3) -0.001(2) -0.004(2) -0.003(2) C42 0.016(2) 0.036(3) 0.060(4) 0.001(3) -0.002(2) -0.007(2) C43 0.020(3) 0.045(3) 0.055(4) 0.009(3) 0.007(3) -0.011(2) C44 0.025(3) 0.036(3) 0.038(3) 0.004(2) -0.002(2) -0.010(2) C45 0.020(2) 0.018(2) 0.033(3) -0.003(2) 0.000(2) -0.008(2) C46 0.024(2) 0.028(2) 0.022(2) -0.007(2) 0.004(2) -0.010(2) C47 0.031(3) 0.029(3) 0.037(3) 0.000(2) -0.004(2) -0.018(2) C48 0.044(3) 0.029(3) 0.041(3) 0.003(2) -0.001(3) -0.018(2) C49 0.036(3) 0.030(3) 0.038(3) 0.004(2) -0.006(2) -0.005(2) C50 0.027(3) 0.032(3) 0.032(3) -0.005(2) -0.006(2) -0.006(2) C51 0.026(2) 0.028(2) 0.031(3) -0.006(2) -0.003(2) -0.010(2) C52 0.038(3) 0.035(3) 0.034(3) -0.009(2) -0.002(2) -0.023(2) C53 0.027(2) 0.021(2) 0.039(3) -0.008(2) 0.002(2) -0.009(2) C54 0.024(2) 0.019(2) 0.028(3) -0.003(2) 0.000(2) -0.007(2) C55 0.020(2) 0.023(2) 0.021(2) -0.003(2) 0.001(2) -0.010(2) C56 0.023(2) 0.016(2) 0.029(3) 0.001(2) -0.001(2) -0.007(2) C57 0.025(2) 0.024(2) 0.037(3) -0.009(2) 0.000(2) -0.007(2) C58 0.028(3) 0.030(3) 0.042(3) -0.005(2) 0.006(2) -0.011(2) C59 0.017(2) 0.036(3) 0.047(3) 0.000(2) 0.000(2) -0.012(2) C60 0.023(2) 0.030(3) 0.046(3) -0.003(2) -0.005(2) -0.013(2) C61 0.035(3) 0.027(3) 0.024(3) -0.002(2) -0.002(2) -0.011(2) C62 0.043(3) 0.042(3) 0.027(3) -0.003(2) 0.004(2) -0.020(3) C63 0.037(3) 0.046(3) 0.035(3) -0.005(3) 0.011(2) -0.021(3) C64 0.033(3) 0.036(3) 0.034(3) -0.007(2) 0.008(2) -0.024(2) C65 0.021(2) 0.021(2) 0.030(3) 0.001(2) -0.002(2) -0.008(2) C66 0.019(2) 0.027(2) 0.030(3) -0.008(2) 0.005(2) -0.011(2) C67 0.037(3) 0.031(3) 0.048(3) -0.007(3) 0.006(3) -0.017(2) C68 0.040(3) 0.035(3) 0.063(4) -0.016(3) 0.013(3) -0.026(3) C69 0.044(3) 0.045(3) 0.064(4) -0.023(3) 0.000(3) -0.027(3) C70 0.034(3) 0.040(3) 0.043(3) -0.020(3) -0.004(2) -0.016(2) C71 0.025(3) 0.027(3) 0.039(3) 0.000(2) -0.002(2) -0.008(2) C72 0.036(3) 0.023(2) 0.041(3) 0.007(2) -0.004(2) -0.013(2) C73 0.029(3) 0.020(2) 0.061(4) -0.005(3) 0.004(3) -0.007(2) C74 0.028(3) 0.026(2) 0.041(3) -0.006(2) 0.001(2) -0.011(2) C75 0.018(2) 0.025(2) 0.035(3) -0.005(2) 0.001(2) -0.011(2) C76 0.022(2) 0.024(2) 0.031(3) -0.008(2) 0.002(2) -0.011(2) C77 0.030(3) 0.034(3) 0.037(3) -0.013(2) 0.006(2) -0.012(2) C78 0.041(3) 0.034(3) 0.043(3) -0.016(3) 0.019(3) -0.019(2) C79 0.052(3) 0.051(3) 0.033(3) -0.015(3) 0.009(3) -0.035(3) C80 0.040(3) 0.040(3) 0.030(3) -0.003(2) -0.001(2) -0.027(2) Br4 0.0306(3) 0.0434(3) 0.0369(3) -0.0107(2) -0.0084(2) -0.0143(2) N1 0.038(2) 0.032(2) 0.025(2) -0.003(2) 0.000(2) -0.020(2) N2 0.025(2) 0.022(2) 0.027(2) -0.002(2) 0.000(2) -0.010(2) N3 0.033(2) 0.030(2) 0.028(2) -0.010(2) 0.004(2) -0.018(2) N4 0.026(2) 0.028(2) 0.029(2) -0.006(2) 0.000(2) -0.013(2) N5 0.023(2) 0.027(2) 0.021(2) -0.005(2) 0.001(2) -0.014(2) N6 0.018(2) 0.028(2) 0.021(2) -0.005(2) 0.001(2) -0.009(2) N7 0.031(2) 0.033(2) 0.026(2) -0.005(2) -0.001(2) -0.012(2) N8 0.030(2) 0.028(2) 0.025(2) -0.008(2) -0.001(2) -0.015(2) N9 0.028(2) 0.029(2) 0.025(2) -0.005(2) -0.003(2) -0.012(2) N10 0.030(2) 0.034(2) 0.025(2) -0.011(2) 0.004(2) -0.016(2) N11 0.020(2) 0.023(2) 0.028(2) -0.010(2) 0.002(2) -0.006(2) N12 0.029(2) 0.024(2) 0.029(2) -0.004(2) -0.001(2) -0.012(2) C1 0.048(3) 0.043(3) 0.036(3) -0.003(3) 0.002(3) -0.029(3) C2 0.072(4) 0.035(3) 0.046(4) -0.003(3) 0.007(3) -0.034(3) C3 0.060(4) 0.026(3) 0.044(4) -0.007(3) 0.003(3) -0.016(3) C4 0.040(3) 0.030(3) 0.037(3) -0.007(2) -0.001(2) -0.013(2) C5 0.032(3) 0.028(2) 0.022(2) -0.001(2) -0.004(2) -0.013(2) C6 0.027(2) 0.030(2) 0.023(3) -0.011(2) 0.002(2) -0.012(2) C7 0.030(3) 0.028(3) 0.042(3) -0.007(2) -0.007(2) -0.008(2) C8 0.029(3) 0.047(3) 0.053(4) -0.020(3) -0.007(3) -0.014(2) C9 0.031(3) 0.062(4) 0.056(4) -0.026(3) 0.007(3) -0.025(3) C10 0.038(3) 0.046(3) 0.044(3) -0.019(3) 0.010(3) -0.030(3) C11 0.032(3) 0.040(3) 0.036(3) -0.008(2) 0.007(2) -0.019(2) C12 0.028(3) 0.044(3) 0.048(4) -0.010(3) 0.008(3) -0.018(2) C13 0.028(3) 0.031(3) 0.048(3) -0.011(2) -0.006(2) -0.011(2) C14 0.029(3) 0.033(3) 0.028(3) -0.006(2) 0.000(2) -0.016(2) C15 0.023(2) 0.021(2) 0.028(3) -0.009(2) 0.002(2) -0.010(2) C16 0.018(2) 0.024(2) 0.022(2) 0.000(2) -0.002(2) -0.009(2) C17 0.027(2) 0.026(2) 0.030(3) -0.005(2) -0.003(2) -0.012(2) C18 0.030(3) 0.027(2) 0.031(3) -0.009(2) -0.004(2) -0.009(2) C19 0.034(3) 0.036(3) 0.026(3) -0.010(2) 0.007(2) -0.011(2) C20 0.025(2) 0.031(3) 0.028(3) -0.003(2) 0.004(2) -0.013(2) C21 0.053(3) 0.042(3) 0.033(3) 0.004(3) -0.010(3) -0.026(3) C22 0.066(4) 0.051(4) 0.040(3) 0.011(3) -0.022(3) -0.028(3) C23 0.056(4) 0.059(4) 0.045(4) 0.004(3) -0.022(3) -0.034(3) C24 0.043(3) 0.043(3) 0.037(3) -0.001(3) -0.010(3) -0.024(3) C25 0.029(3) 0.028(2) 0.024(3) -0.005(2) -0.002(2) -0.010(2) C26 0.024(2) 0.031(3) 0.031(3) -0.008(2) 0.001(2) -0.013(2) C27 0.051(3) 0.031(3) 0.031(3) -0.004(2) -0.010(3) -0.018(2) C28 0.054(4) 0.036(3) 0.045(4) -0.009(3) -0.017(3) -0.019(3) C29 0.052(3) 0.025(3) 0.057(4) 0.009(3) -0.019(3) -0.017(2) C30 0.039(3) 0.030(3) 0.037(3) 0.005(2) -0.008(2) -0.011(2) C31 0.034(3) 0.052(3) 0.021(3) -0.016(2) 0.006(2) -0.023(2) C32 0.039(3) 0.056(4) 0.041(3) -0.031(3) 0.013(3) -0.022(3) C33 0.039(3) 0.043(3) 0.055(4) -0.028(3) 0.009(3) -0.018(3) C34 0.036(3) 0.028(3) 0.043(3) -0.009(2) -0.001(2) -0.011(2) C35 0.024(2) 0.034(3) 0.035(3) -0.011(2) 0.003(2) -0.016(2) C36 0.026(2) 0.017(2) 0.028(3) -0.004(2) 0.000(2) -0.009(2) C37 0.027(3) 0.027(3) 0.040(3) -0.004(2) -0.002(2) -0.011(2) C38 0.034(3) 0.027(3) 0.046(3) 0.002(2) -0.010(3) -0.011(2) C39 0.041(3) 0.029(3) 0.037(3) 0.001(2) -0.009(3) -0.016(2) C40 0.032(3) 0.035(3) 0.025(3) -0.003(2) 0.000(2) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.3062(9) . y Co2 Co3 2.4313(9) . y Co1 Br1 2.5887(9) . y Co3 Br2 2.5800(9) . y Co1 N1 1.965(4) . y Co1 N4 1.973(4) . y Co1 N7 1.976(4) . y Co1 N10 1.980(4) . y Co2 N2 1.901(4) . y Co2 N5 1.904(3) . y Co2 N8 1.910(4) . y Co2 N11 1.898(3) . y Co3 N3 2.075(4) . y Co3 N6 2.088(4) . y Co3 N9 2.074(4) . y Co3 N12 2.079(4) . y Co4 Co5 2.3118(8) . y Co5 Co6 2.3536(9) . y Br3 Co4 2.6226(8) . y Co6 Br4 2.5632(8) . y Co4 N16 1.968(4) . y Co4 N19 1.982(4) . y Co4 N22 1.986(4) . y Co4 N13 2.008(4) . y Co5 N14 1.887(4) . y Co5 N17 1.906(3) . y Co5 N20 1.890(4) . y Co5 N23 1.897(3) . y Co6 N15 2.016(4) . y Co6 N18 2.013(4) . y Co6 N21 2.015(4) . y Co6 N24 2.070(4) . y N13 C41 1.358(5) . ? N13 C45 1.361(6) . ? N14 C46 1.362(6) . ? N14 C45 1.370(5) . ? N15 C50 1.352(6) . ? N15 C46 1.365(5) . ? N16 C55 1.358(5) . ? N16 C51 1.359(5) . ? N17 C56 1.363(5) . ? N17 C55 1.363(5) . ? N18 C60 1.355(5) . ? N18 C56 1.365(5) . ? N19 C61 1.352(6) . ? N19 C65 1.364(5) . ? N20 C66 1.367(5) . ? N20 C65 1.373(6) . ? N21 C70 1.364(6) . ? N21 C66 1.365(6) . ? N22 C71 1.348(6) . ? N22 C75 1.365(6) . ? N23 C76 1.362(6) . ? N23 C75 1.365(6) . ? N24 C80 1.342(6) . ? N24 C76 1.371(6) . ? C41 C42 1.364(7) . ? C42 C43 1.384(8) . ? C43 C44 1.365(6) . ? C44 C45 1.400(6) . ? C46 C47 1.413(6) . ? C47 C48 1.373(7) . ? C48 C49 1.402(7) . ? C49 C50 1.370(7) . ? C51 C52 1.370(6) . ? C52 C53 1.390(6) . ? C53 C54 1.359(6) . ? C54 C55 1.423(6) . ? C56 C57 1.410(6) . ? C57 C58 1.369(6) . ? C58 C59 1.378(7) . ? C59 C60 1.375(6) . ? C61 C62 1.372(6) . ? C62 C63 1.381(7) . ? C63 C64 1.355(7) . ? C64 C65 1.409(6) . ? C66 C67 1.405(7) . ? C67 C68 1.366(7) . ? C68 C69 1.386(8) . ? C69 C70 1.374(8) . ? C71 C72 1.371(6) . ? C72 C73 1.373(7) . ? C73 C74 1.366(7) . ? C74 C75 1.407(6) . ? C76 C77 1.404(6) . ? C77 C78 1.369(7) . ? C78 C79 1.390(7) . ? C79 C80 1.388(7) . ? N1 C1 1.356(6) . ? N1 C5 1.362(6) . ? N2 C6 1.362(6) . ? N2 C5 1.377(6) . ? N3 C10 1.354(6) . ? N3 C6 1.373(6) . ? N4 C11 1.343(6) . ? N4 C15 1.369(6) . ? N5 C16 1.366(5) . ? N5 C15 1.378(5) . ? N6 C20 1.348(5) . ? N6 C16 1.362(5) . ? N7 C21 1.339(6) . ? N7 C25 1.360(6) . ? N8 C26 1.365(6) . ? N8 C25 1.371(6) . ? N9 C30 1.358(6) . ? N9 C26 1.365(6) . ? N10 C31 1.367(6) . ? N10 C35 1.368(6) . ? N11 C35 1.364(6) . ? N11 C36 1.375(6) . ? N12 C40 1.354(6) . ? N12 C36 1.354(6) . ? C1 C2 1.381(7) . ? C2 C3 1.378(7) . ? C3 C4 1.370(7) . ? C4 C5 1.425(6) . ? C6 C7 1.412(6) . ? C7 C8 1.374(7) . ? C8 C9 1.378(8) . ? C9 C10 1.377(8) . ? C11 C12 1.375(7) . ? C12 C13 1.395(7) . ? C13 C14 1.351(6) . ? C14 C15 1.399(6) . ? C16 C17 1.405(6) . ? C17 C18 1.360(6) . ? C18 C19 1.389(7) . ? C19 C20 1.371(6) . ? C21 C22 1.381(7) . ? C22 C23 1.384(8) . ? C23 C24 1.358(7) . ? C24 C25 1.408(6) . ? C26 C27 1.403(6) . ? C27 C28 1.374(7) . ? C28 C29 1.383(8) . ? C29 C30 1.360(7) . ? C31 C32 1.363(7) . ? C32 C33 1.384(8) . ? C33 C34 1.369(7) . ? C34 C35 1.419(6) . ? C36 C37 1.414(6) . ? C37 C38 1.381(7) . ? C38 C39 1.372(7) . ? C39 C40 1.388(6) . ? C1S C7S 1.34(2) . ? C1S C2S 1.39 . ? C1S C6S 1.39 . ? C2S C3S 1.39 . ? C3S C4S 1.39 . ? C4S C5S 1.39 . ? C5S C6S 1.39 . ? C1' C7' 1.33(2) . ? C1' C2' 1.39 . ? C1' C6' 1.39 . ? C2' C3' 1.39 . ? C3' C4' 1.39 . ? C4' C5' 1.39 . ? C5' C6' 1.39 . ? C8S C9S 1.39 . ? C8S C13S 1.39 . ? C9S C10S 1.39 . ? C10S C11S 1.39 . ? C11S C14S 1.17(2) . ? C11S C12S 1.39 . ? C12S C13S 1.39 . ? C8' C9' 1.39 . ? C8' C13' 1.39 . ? C8' C14' 1.60(2) . ? C9' C10' 1.39 . ? C10' C11' 1.39 . ? C11' C12' 1.39 . ? C12' C13' 1.39 . ? C15S C16S 1.44(4) . ? C16S C17S 1.54(3) . ? C17S C18S 1.41(3) . ? C18S C19S 1.66(3) . ? C19S C20S 0.88(3) . ? C15' C16' 1.48(2) . ? C16' C17' 1.25(2) . ? C17' C19' 1.53(3) . ? C17' C20' 1.55(2) . ? C18' C20' 1.28(2) . ? C21S C25S 1.14(2) 2_665 ? C21S C26S 1.35(2) . ? C21S C22S 1.35(2) . ? C21S C27S 1.37(2) . ? C21S C24S 1.37(2) 2_665 ? C21S C26S 1.38(2) 2_665 ? C21S C23S 1.61(2) 2_665 ? C21S C21S 1.66(3) 2_665 ? C21S C22S 1.81(2) 2_665 ? C22S C26S 0.52(2) 2_665 ? C22S C25S 1.13(2) 2_665 ? C22S C23S 1.41(2) . ? C22S C21S 1.81(2) 2_665 ? C23S C26S 1.05(2) 2_665 ? C23S C24S 1.34(2) . ? C23S C21S 1.61(2) 2_665 ? C23S C27S 1.96(2) 2_665 ? C24S C27S 0.68(2) 2_665 ? C24S C21S 1.37(2) 2_665 ? C24S C25S 1.71(2) . ? C24S C26S 1.98(2) 2_665 ? C25S C22S 1.13(2) 2_665 ? C25S C21S 1.14(2) 2_665 ? C25S C27S 1.23(2) 2_665 ? C25S C26S 1.52(2) . ? C26S C22S 0.52(2) 2_665 ? C26S C23S 1.05(2) 2_665 ? C26S C21S 1.38(2) 2_665 ? C26S C24S 1.98(2) 2_665 ? C27S C24S 0.68(2) 2_665 ? C27S C25S 1.23(2) 2_665 ? C27S C23S 1.96(2) 2_665 ? C28S C29S 1.39 . ? C28S C33S 1.39 . ? C29S C30S 1.39 . ? C30S C31S 1.39 . ? C31S C32S 1.39 . ? C31S C34S 1.89(2) . ? C32S C33S 1.39 . ? C28' C29' 1.39 . ? C28' C33' 1.39 . ? C29' C30' 1.39 . ? C30' C31' 1.39 . ? C30' C34' 1.51(2) . ? C31' C32' 1.39 . ? C32' C33' 1.39 . ? 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 Co1 Co2 Co3 178.24(3) . . y Co2 Co1 Br1 179.80(4) . . y Co2 Co3 Br2 179.18(3) . . y N1 Co1 N4 90.1(2) . . y N1 Co1 N7 90.0(2) . . y N1 Co1 N10 170.9(2) . . y N4 Co1 N7 170.8(2) . . y N4 Co1 N10 88.0(2) . . y N7 Co1 N10 90.6(2) . . y N2 Co2 N5 89.5(2) . . y N2 Co2 N8 90.6(2) . . y N11 Co2 N2 179.3(2) . . y N5 Co2 N8 179.2(2) . . y N11 Co2 N5 89.8(2) . . y N11 Co2 N8 90.0(2) . . y N3 Co3 N6 89.26(14) . . y N9 Co3 N3 92.91(14) . . y N3 Co3 N12 164.6(2) . . y N9 Co3 N6 164.7(2) . . y N12 Co3 N6 83.75(14) . . y N9 Co3 N12 90.36(14) . . y N1 Co1 Br1 93.82(12) . . y N4 Co1 Br1 95.22(12) . . y N7 Co1 Br1 93.99(13) . . y N10 Co1 Br1 95.16(12) . . y N3 Co3 Br2 96.93(11) . . y N6 Co3 Br2 98.46(11) . . y N9 Co3 Br2 96.35(11) . . y N12 Co3 Br2 97.63(12) . . y N1 Co1 Co2 86.13(12) . . ? N4 Co1 Co2 84.98(12) . . ? N7 Co1 Co2 85.82(12) . . ? N10 Co1 Co2 84.89(12) . . ? N11 Co2 Co1 90.40(12) . . ? N2 Co2 Co1 89.28(12) . . ? N5 Co2 Co1 90.10(11) . . ? N8 Co2 Co1 89.08(12) . . ? N11 Co2 Co3 90.12(12) . . ? N2 Co2 Co3 90.22(12) . . ? N5 Co2 Co3 91.58(11) . . ? N8 Co2 Co3 89.24(12) . . ? N9 Co3 Co2 83.11(11) . . ? N3 Co3 Co2 83.72(11) . . ? N12 Co3 Co2 81.76(11) . . ? N6 Co3 Co2 82.04(11) . . ? Co4 Co5 Co6 177.06(3) . . y Co5 Co4 Br3 177.71(3) . . y Co5 Co6 Br4 177.51(4) . . y N16 Co4 N13 89.13(15) . . y N19 Co4 N13 169.2(2) . . y N22 Co4 N13 90.68(15) . . y N16 Co4 N19 90.18(15) . . y N16 Co4 N22 170.1(2) . . y N19 Co4 N22 88.15(15) . . y N14 Co5 N17 90.00(15) . . y N14 Co5 N20 179.3(2) . . y N14 Co5 N23 89.75(15) . . y N20 Co5 N17 90.27(15) . . y N23 Co5 N17 178.61(15) . . y N20 Co5 N23 89.99(15) . . y N18 Co6 N15 89.05(15) . . y N21 Co6 N15 168.4(2) . . y N15 Co6 N24 91.77(14) . . y N18 Co6 N24 167.03(15) . . y N18 Co6 N21 87.78(15) . . y N21 Co6 N24 88.84(14) . . y N13 Co4 Br3 94.62(11) . . y N16 Co4 Br3 95.81(11) . . y N19 Co4 Br3 96.18(11) . . y N22 Co4 Br3 94.09(11) . . y N15 Co6 Br4 93.91(11) . . y N18 Co6 Br4 96.40(10) . . y N21 Co6 Br4 97.58(11) . . y N24 Co6 Br4 96.46(11) . . y N16 Co4 Co5 86.32(11) . . ? N19 Co4 Co5 84.63(11) . . ? N22 Co4 Co5 83.78(11) . . ? N13 Co4 Co5 84.57(11) . . ? N14 Co5 Co4 90.28(11) . . ? N20 Co5 Co4 90.34(12) . . ? N23 Co5 Co4 90.31(11) . . ? N17 Co5 Co4 88.32(11) . . ? N14 Co5 Co6 89.61(11) . . ? N20 Co5 Co6 89.79(11) . . ? N23 Co5 Co6 92.63(11) . . ? N17 Co5 Co6 88.74(11) . . ? N18 Co6 Co5 84.84(11) . . ? N21 Co6 Co5 84.62(11) . . ? N15 Co6 Co5 83.94(11) . . ? N24 Co6 Co5 82.37(11) . . ? C41 N13 C45 117.7(4) . . ? C41 N13 Co4 122.0(3) . . ? C45 N13 Co4 120.2(3) . . ? C46 N14 C45 124.1(4) . . ? C46 N14 Co5 118.6(3) . . ? C45 N14 Co5 117.3(3) . . ? C50 N15 C46 118.1(4) . . ? C50 N15 Co6 121.7(3) . . ? C46 N15 Co6 120.0(3) . . ? C55 N16 C51 118.8(4) . . ? C55 N16 Co4 119.2(3) . . ? C51 N16 Co4 122.0(3) . . ? C56 N17 C55 124.0(3) . . ? C56 N17 Co5 118.4(3) . . ? C55 N17 Co5 117.6(3) . . ? C60 N18 C56 118.6(4) . . ? C60 N18 Co6 121.2(3) . . ? C56 N18 Co6 120.0(3) . . ? C61 N19 C65 118.2(4) . . ? C61 N19 Co4 120.9(3) . . ? C65 N19 Co4 120.7(3) . . ? C66 N20 C65 123.5(4) . . ? C66 N20 Co5 119.6(3) . . ? C65 N20 Co5 116.6(3) . . ? C70 N21 C66 117.7(4) . . ? C70 N21 Co6 121.6(4) . . ? C66 N21 Co6 120.7(3) . . ? C71 N22 C75 119.2(4) . . ? C71 N22 Co4 119.8(3) . . ? C75 N22 Co4 120.9(3) . . ? C76 N23 C75 125.3(4) . . ? C76 N23 Co5 117.6(3) . . ? C75 N23 Co5 117.1(3) . . ? C80 N24 C76 118.6(4) . . ? C80 N24 Co6 119.8(3) . . ? C76 N24 Co6 121.6(3) . . ? N13 C41 C42 122.7(5) . . ? C41 C42 C43 119.8(5) . . ? C44 C43 C42 118.7(5) . . ? C43 C44 C45 119.9(5) . . ? N13 C45 N14 114.9(4) . . ? N13 C45 C44 121.2(4) . . ? N14 C45 C44 123.4(4) . . ? N14 C46 N15 115.3(4) . . ? N14 C46 C47 124.5(4) . . ? N15 C46 C47 119.9(4) . . ? C48 C47 C46 120.8(5) . . ? C47 C48 C49 118.3(5) . . ? C50 C49 C48 118.6(5) . . ? N15 C50 C49 123.9(5) . . ? N16 C51 C52 123.2(4) . . ? C51 C52 C53 118.4(4) . . ? C54 C53 C52 119.9(4) . . ? C53 C54 C55 120.0(4) . . ? N16 C55 N17 115.7(4) . . ? N16 C55 C54 119.7(4) . . ? N17 C55 C54 124.4(4) . . ? N17 C56 N18 115.1(4) . . ? N17 C56 C57 124.4(4) . . ? N18 C56 C57 120.1(4) . . ? C58 C57 C56 119.9(4) . . ? C57 C58 C59 119.5(5) . . ? C60 C59 C58 119.0(4) . . ? N18 C60 C59 122.7(5) . . ? N19 C61 C62 123.5(5) . . ? C61 C62 C63 118.2(5) . . ? C64 C63 C62 119.9(5) . . ? C63 C64 C65 120.4(5) . . ? N19 C65 N20 115.0(4) . . ? N19 C65 C64 119.8(4) . . ? N20 C65 C64 124.9(4) . . ? N21 C66 N20 114.9(4) . . ? N21 C66 C67 120.5(4) . . ? N20 C66 C67 124.3(5) . . ? C68 C67 C66 120.2(5) . . ? C67 C68 C69 119.7(5) . . ? C70 C69 C68 118.2(5) . . ? N21 C70 C69 123.6(5) . . ? N22 C71 C72 123.0(5) . . ? C71 C72 C73 118.3(5) . . ? C74 C73 C72 119.9(5) . . ? C73 C74 C75 120.4(5) . . ? N22 C75 N23 114.5(4) . . ? N22 C75 C74 118.8(4) . . ? N23 C75 C74 126.3(4) . . ? N23 C76 N24 115.5(4) . . ? N23 C76 C77 124.3(4) . . ? N24 C76 C77 120.0(4) . . ? C78 C77 C76 120.5(5) . . ? C77 C78 C79 119.2(5) . . ? C80 C79 C78 118.2(5) . . ? N24 C80 C79 123.4(5) . . ? C1 N1 C5 117.7(4) . . ? C1 N1 Co1 122.4(3) . . ? C5 N1 Co1 119.9(3) . . ? C6 N2 C5 123.2(4) . . ? C6 N2 Co2 119.9(3) . . ? C5 N2 Co2 116.9(3) . . ? C10 N3 C6 117.3(4) . . ? C10 N3 Co3 121.8(4) . . ? C6 N3 Co3 120.8(3) . . ? C11 N4 C15 118.5(4) . . ? C11 N4 Co1 120.8(3) . . ? C15 N4 Co1 120.7(3) . . ? C16 N5 C15 123.2(4) . . ? C16 N5 Co2 120.2(3) . . ? C15 N5 Co2 116.3(3) . . ? C20 N6 C16 118.0(4) . . ? C20 N6 Co3 118.6(3) . . ? C16 N6 Co3 123.3(3) . . ? C21 N7 C25 118.7(4) . . ? C21 N7 Co1 121.6(4) . . ? C25 N7 Co1 119.7(3) . . ? C26 N8 C25 122.8(4) . . ? C26 N8 Co2 119.2(3) . . ? C25 N8 Co2 117.9(3) . . ? C30 N9 C26 117.8(4) . . ? C30 N9 Co3 120.6(3) . . ? C26 N9 Co3 121.3(3) . . ? C31 N10 C35 117.8(4) . . ? C31 N10 Co1 121.9(4) . . ? C35 N10 Co1 120.3(3) . . ? C35 N11 C36 124.2(4) . . ? C35 N11 Co2 118.3(3) . . ? C36 N11 Co2 117.2(3) . . ? C40 N12 C36 118.6(4) . . ? C40 N12 Co3 118.6(3) . . ? C36 N12 Co3 122.1(3) . . ? N1 C1 C2 123.4(5) . . ? C3 C2 C1 118.7(5) . . ? C4 C3 C2 120.1(5) . . ? C3 C4 C5 118.9(5) . . ? N1 C5 N2 115.5(4) . . ? N1 C5 C4 121.1(4) . . ? N2 C5 C4 123.2(4) . . ? N2 C6 N3 116.3(4) . . ? N2 C6 C7 123.0(5) . . ? N3 C6 C7 120.6(4) . . ? C8 C7 C6 119.8(5) . . ? C7 C8 C9 119.5(5) . . ? C10 C9 C8 118.5(5) . . ? N3 C10 C9 124.0(5) . . ? N4 C11 C12 123.6(5) . . ? C11 C12 C13 117.9(5) . . ? C14 C13 C12 119.3(5) . . ? C13 C14 C15 121.1(5) . . ? N4 C15 N5 114.9(4) . . ? N4 C15 C14 119.5(4) . . ? N5 C15 C14 125.4(4) . . ? N6 C16 N5 115.1(4) . . ? N6 C16 C17 120.3(4) . . ? N5 C16 C17 124.6(4) . . ? C18 C17 C16 120.0(4) . . ? C17 C18 C19 119.9(4) . . ? C20 C19 C18 117.8(4) . . ? N6 C20 C19 123.9(5) . . ? N7 C21 C22 123.0(5) . . ? C21 C22 C23 118.7(5) . . ? C24 C23 C22 119.0(5) . . ? C23 C24 C25 120.4(5) . . ? N7 C25 N8 115.2(4) . . ? N7 C25 C24 120.0(5) . . ? N8 C25 C24 124.7(5) . . ? N9 C26 N8 115.3(4) . . ? N9 C26 C27 120.3(4) . . ? N8 C26 C27 124.1(5) . . ? C28 C27 C26 120.0(5) . . ? C27 C28 C29 119.5(5) . . ? C30 C29 C28 118.4(5) . . ? N9 C30 C29 123.9(5) . . ? C32 C31 N10 123.8(5) . . ? C31 C32 C33 118.1(5) . . ? C34 C33 C32 120.6(5) . . ? C33 C34 C35 119.2(5) . . ? N11 C35 N10 115.0(4) . . ? N11 C35 C34 124.5(5) . . ? N10 C35 C34 120.3(4) . . ? N12 C36 N11 115.2(4) . . ? N12 C36 C37 120.5(4) . . ? N11 C36 C37 123.9(4) . . ? C38 C37 C36 119.2(5) . . ? C39 C38 C37 120.5(5) . . ? C38 C39 C40 117.8(5) . . ? N12 C40 C39 123.4(5) . . ? C7S C1S C2S 115.9(9) . . ? C7S C1S C6S 124.0(9) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C4S C3S C2S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C7' C1' C2' 116.8(14) . . ? C7' C1' C6' 123.1(14) . . ? C2' C1' C6' 120.0 . . ? C3' C2' C1' 120.0 . . ? C2' C3' C4' 120.0 . . ? C5' C4' C3' 120.0 . . ? C4' C5' C6' 120.0 . . ? C5' C6' C1' 120.0 . . ? C9S C8S C13S 120.0 . . ? C8S C9S C10S 120.0 . . ? C11S C10S C9S 120.0 . . ? C14S C11S C10S 131.2(17) . . ? C14S C11S C12S 108.6(17) . . ? C10S C11S C12S 120.0 . . ? C11S C12S C13S 120.0 . . ? C12S C13S C8S 120.0 . . ? C9' C8' C13' 120.0 . . ? C9' C8' C14' 116.5(9) . . ? C13' C8' C14' 123.5(9) . . ? C8' C9' C10' 120.0 . . ? C11' C10' C9' 120.0 . . ? C12' C11' C10' 120.0 . . ? C11' C12' C13' 120.0 . . ? C12' C13' C8' 120.0 . . ? C15S C16S C17S 116.4(25) . . ? C18S C17S C16S 126.1(26) . . ? C17S C18S C19S 141.9(26) . . ? C20S C19S C18S 146.1(32) . . ? C17' C16' C15' 125.7(14) . . ? C16' C17' C19' 133.7(17) . . ? C16' C17' C20' 111.7(15) . . ? C19' C17' C20' 114.4(15) . . ? C18' C20' C17' 120.4(16) . . ? C25S C21S C26S 167.1(17) 2_665 . ? C25S C21S C22S 52.9(12) 2_665 . ? C26S C21S C22S 126.9(16) . . ? C25S C21S C27S 57.9(12) 2_665 . ? C26S C21S C27S 122.2(16) . . ? C22S C21S C27S 110.3(14) . . ? C25S C21S C24S 85.1(16) 2_665 2_665 ? C26S C21S C24S 93.4(15) . 2_665 ? C22S C21S C24S 138.0(17) . 2_665 ? C27S C21S C24S 28.9(10) . 2_665 ? C25S C21S C26S 73.6(14) 2_665 2_665 ? C26S C21S C26S 105.2(14) . 2_665 ? C22S C21S C26S 21.7(10) . 2_665 ? C27S C21S C26S 131.4(16) . 2_665 ? C24S C21S C26S 156.8(17) 2_665 2_665 ? C25S C21S C23S 136.3(17) 2_665 2_665 ? C26S C21S C23S 40.6(9) . 2_665 ? C22S C21S C23S 164.4(14) . 2_665 ? C27S C21S C23S 81.7(12) . 2_665 ? C24S C21S C23S 52.9(10) 2_665 2_665 ? C26S C21S C23S 143.9(15) 2_665 2_665 ? C25S C21S C21S 123.8(19) 2_665 2_665 ? C26S C21S C21S 53.6(12) . 2_665 ? C22S C21S C21S 73.3(12) . 2_665 ? C27S C21S C21S 170.2(17) . 2_665 ? C24S C21S C21S 144.7(19) 2_665 2_665 ? C26S C21S C21S 51.6(10) 2_665 2_665 ? C23S C21S C21S 93.3(14) 2_665 2_665 ? C25S C21S C22S 163.3(16) 2_665 2_665 ? C26S C21S C22S 8.2(11) . 2_665 ? C22S C21S C22S 118.8(11) . 2_665 ? C27S C21S C22S 130.0(13) . 2_665 ? C24S C21S C22S 101.1(13) 2_665 2_665 ? C26S C21S C22S 97.1(12) 2_665 2_665 ? C23S C21S C22S 48.3(10) 2_665 2_665 ? C21S C21S C22S 45.5(9) 2_665 2_665 ? C26S C22S C25S 133.0(39) 2_665 2_665 ? C26S C22S C21S 82.9(32) 2_665 . ? C25S C22S C21S 53.9(12) 2_665 . ? C26S C22S C23S 37.8(29) 2_665 . ? C25S C22S C23S 170.6(19) 2_665 . ? C21S C22S C23S 118.6(15) . . ? C26S C22S C21S 21.8(29) 2_665 2_665 ? C25S C22S C21S 113.1(15) 2_665 2_665 ? C21S C22S C21S 61.2(11) . 2_665 ? C23S C22S C21S 58.3(9) . 2_665 ? C26S C23S C24S 110.5(17) 2_665 . ? C26S C23S C22S 17.5(12) 2_665 . ? C24S C23S C22S 127.6(16) . . ? C26S C23S C21S 56.2(12) 2_665 2_665 ? C24S C23S C21S 54.3(11) . 2_665 ? C22S C23S C21S 73.4(12) . 2_665 ? C26S C23S C27S 99.9(15) 2_665 2_665 ? C24S C23S C27S 10.8(11) . 2_665 ? C22S C23S C27S 117.1(13) . 2_665 ? C21S C23S C27S 43.7(8) 2_665 2_665 ? C27S C24S C23S 147.7(34) 2_665 . ? C27S C24S C21S 75.3(26) 2_665 2_665 ? C23S C24S C21S 72.8(14) . 2_665 ? C27S C24S C25S 36.7(23) 2_665 . ? C23S C24S C25S 113.5(16) . . ? C21S C24S C25S 41.8(9) 2_665 . ? C27S C24S C26S 118.0(30) 2_665 2_665 ? C23S C24S C26S 29.9(9) . 2_665 ? C21S C24S C26S 42.9(10) 2_665 2_665 ? C25S C24S C26S 84.0(11) . 2_665 ? C22S C25S C21S 73.2(16) 2_665 2_665 ? C22S C25S C27S 142.6(21) 2_665 2_665 ? C21S C25S C27S 70.3(14) 2_665 2_665 ? C22S C25S C26S 14.3(12) 2_665 . ? C21S C25S C26S 60.6(13) 2_665 . ? C27S C25S C26S 130.9(17) 2_665 . ? C22S C25S C24S 126.3(18) 2_665 . ? C21S C25S C24S 53.1(12) 2_665 . ? C27S C25S C24S 19.4(12) 2_665 . ? C26S C25S C24S 113.1(14) . . ? C22S C26S C23S 124.7(38) 2_665 2_665 ? C22S C26S C21S 150.1(39) 2_665 . ? C23S C26S C21S 83.2(15) 2_665 . ? C22S C26S C21S 75.4(32) 2_665 2_665 ? C23S C26S C21S 153.9(19) 2_665 2_665 ? C21S C26S C21S 74.7(14) . 2_665 ? C22S C26S C25S 32.6(29) 2_665 . ? C23S C26S C25S 157.3(18) 2_665 . ? C21S C26S C25S 119.3(16) . . ? C21S C26S C25S 45.8(9) 2_665 . ? C22S C26S C24S 162.2(37) 2_665 2_665 ? C23S C26S C24S 39.5(11) 2_665 2_665 ? C21S C26S C24S 43.7(9) . 2_665 ? C21S C26S C24S 117.2(13) 2_665 2_665 ? C25S C26S C24S 162.9(14) . 2_665 ? C24S C27S C25S 123.8(32) 2_665 2_665 ? C24S C27S C21S 75.8(27) 2_665 . ? C25S C27S C21S 51.8(11) 2_665 . ? C24S C27S C23S 21.5(24) 2_665 2_665 ? C25S C27S C23S 104.6(15) 2_665 2_665 ? C21S C27S C23S 54.6(10) . 2_665 ? C29S C28S C33S 120.0 . . ? C28S C29S C30S 120.0 . . ? C29S C30S C31S 120.0 . . ? C32S C31S C30S 120.0 . . ? C32S C31S C34S 117.3(12) . . ? C30S C31S C34S 122.4(12) . . ? C33S C32S C31S 120.0 . . ? C32S C33S C28S 120.0 . . ? C29' C28' C33' 120.0 . . ? C30' C29' C28' 120.0 . . ? C29' C30' C31' 120.0 . . ? C29' C30' C34' 116.7(9) . . ? C31' C30' C34' 121.7(9) . . ? C32' C31' C30' 120.0 . . ? C33' C32' C31' 120.0 . . ? C32' C33' C28' 120.0 . . ? _refine_diff_density_max 1.306 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.103 #===END data_1-1.75C7H8.0.5C6H14_at_213K _audit_creation_method SHELXL _chemical_formula_structural 'Co3(dpa)4Br2.1.75Tol.0.5Hex' _chemical_formula_sum 'C55.25 H53 Br2 Co3 N12' _chemical_formula_weight 1221.71 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.007(1) _cell_length_b 18.228(1) _cell_length_c 19.321(2) _cell_angle_alpha 81.220(2) _cell_angle_beta 82.232(2) _cell_angle_gamma 62.411(1) _cell_volume 5232.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 4125 _cell_measurement_theta_min 2.351 _cell_measurement_theta_max 27.297 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method ? _exptl_crystal_F_000 2478 _exptl_absorpt_coefficient_mu 2.518 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.4139 _exptl_absorpt_correction_T_max 0.7726 _diffrn_ambient_temperature 213(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36033 _diffrn_reflns_av_R_equivalents 0.0460 _diffrn_reflns_av_sigmaI/netI 0.0978 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.53 _reflns_number_total 23143 _reflns_number_observed 12280 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0531P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23143 _refine_ls_number_parameters 1199 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1170 _refine_ls_R_factor_obs 0.0515 _refine_ls_wR_factor_all 0.1385 _refine_ls_wR_factor_obs 0.1159 _refine_ls_goodness_of_fit_all 1.002 _refine_ls_goodness_of_fit_obs 1.175 _refine_ls_restrained_S_all 1.003 _refine_ls_restrained_S_obs 1.176 _refine_ls_shift/esd_max 0.005 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.05356(4) 0.72523(4) 0.08941(4) 0.0329(2) Uani 1 d . -1 Co2 Co -0.00846(4) 0.67934(4) 0.18935(4) 0.0270(2) Uani 1 d . -1 Co3 Co -0.07701(4) 0.62910(4) 0.29303(4) 0.0339(2) Uani 1 d . -1 Br1 Br 0.12270(4) 0.77703(4) -0.02287(3) 0.0584(2) Uani 1 d . -1 Br2 Br -0.14709(4) 0.57517(4) 0.40115(3) 0.0464(2) Uani 1 d . -1 N1 N -0.0261(3) 0.8380(3) 0.1163(2) 0.0353(10) Uani 1 d . -1 N2 N -0.1126(3) 0.7834(2) 0.1832(2) 0.0296(10) Uani 1 d . -1 N3 N -0.1946(3) 0.7247(3) 0.2541(2) 0.0342(10) Uani 1 d . -1 N4 N 0.1418(3) 0.7156(3) 0.1514(2) 0.0347(10) Uani 1 d . -1 N5 N 0.0396(3) 0.7237(2) 0.2453(2) 0.0288(9) Uani 1 d . -1 N6 N -0.0595(2) 0.7184(2) 0.3379(2) 0.0281(9) Uani 1 d . -1 N7 N -0.0428(3) 0.7277(3) 0.0409(2) 0.0360(11) Uani 1 d . -1 N8 N -0.0553(3) 0.6351(3) 0.1314(2) 0.0321(10) Uani 1 d . -1 N9 N -0.0703(3) 0.5468(3) 0.2255(2) 0.0334(10) Uani 1 d . -1 N10 N 0.1269(3) 0.6054(3) 0.0771(2) 0.0353(11) Uani 1 d . -1 N11 N 0.0967(3) 0.5762(2) 0.1952(2) 0.0313(10) Uani 1 d . -1 N12 N 0.0570(3) 0.5532(2) 0.3124(2) 0.0329(10) Uani 1 d . -1 C1 C -0.0068(4) 0.9031(4) 0.0955(3) 0.049(2) Uani 1 d . -1 H1A H 0.0466(4) 0.8931(4) 0.0681(3) 0.059 Uiso 1 calc R -1 C2 C -0.0617(4) 0.9829(4) 0.1126(3) 0.058(2) Uani 1 d . -1 H2A H -0.0473(4) 1.0267(4) 0.0958(3) 0.070 Uiso 1 calc R -1 C3 C -0.1379(4) 0.9965(4) 0.1548(3) 0.058(2) Uani 1 d . -1 H3A H -0.1761(4) 1.0503(4) 0.1676(3) 0.070 Uiso 1 calc R -1 C4 C -0.1586(4) 0.9332(3) 0.1782(3) 0.0422(14) Uani 1 d . -1 H4A H -0.2106(4) 0.9427(3) 0.2075(3) 0.051 Uiso 1 calc R -1 C5 C -0.1014(3) 0.8524(3) 0.1582(3) 0.0334(12) Uani 1 d . -1 C6 C -0.1936(3) 0.7868(3) 0.2041(3) 0.0307(12) Uani 1 d . -1 C7 C -0.2729(3) 0.8461(3) 0.1747(3) 0.0403(14) Uani 1 d . -1 H7A H -0.2713(3) 0.8860(3) 0.1382(3) 0.048 Uiso 1 calc R -1 C8 C -0.3536(4) 0.8460(4) 0.1993(3) 0.049(2) Uani 1 d . -1 H8A H -0.4067(4) 0.8860(4) 0.1801(3) 0.058 Uiso 1 calc R -1 C9 C -0.3545(4) 0.7872(4) 0.2517(4) 0.052(2) Uani 1 d . -1 H9A H -0.4086(4) 0.7876(4) 0.2708(4) 0.062 Uiso 1 calc R -1 C10 C -0.2749(4) 0.7269(4) 0.2765(3) 0.0449(15) Uani 1 d . -1 H10A H -0.2763(4) 0.6850(4) 0.3109(3) 0.054 Uiso 1 calc R -1 C11 C 0.2244(4) 0.7012(3) 0.1262(3) 0.0442(14) Uani 1 d . -1 H11A H 0.2394(4) 0.6953(3) 0.0780(3) 0.053 Uiso 1 calc R -1 C12 C 0.2882(4) 0.6948(4) 0.1660(3) 0.052(2) Uani 1 d . -1 H12A H 0.3446(4) 0.6867(4) 0.1455(3) 0.062 Uiso 1 calc R -1 C13 C 0.2677(3) 0.7005(3) 0.2374(3) 0.0429(14) Uani 1 d . -1 H13A H 0.3101(3) 0.6965(3) 0.2663(3) 0.052 Uiso 1 calc R -1 C14 C 0.1853(3) 0.7120(3) 0.2652(3) 0.0356(13) Uani 1 d . -1 H14A H 0.1711(3) 0.7151(3) 0.3137(3) 0.043 Uiso 1 calc R -1 C15 C 0.1217(3) 0.7192(3) 0.2221(3) 0.0291(11) Uani 1 d . -1 C16 C -0.0031(3) 0.7502(3) 0.3087(3) 0.0286(11) Uani 1 d . -1 C17 C 0.0061(3) 0.8093(3) 0.3425(3) 0.0329(12) Uani 1 d . -1 H17A H 0.0429(3) 0.8333(3) 0.3209(3) 0.039 Uiso 1 calc R -1 C18 C -0.0380(3) 0.8314(3) 0.4057(3) 0.0377(13) Uani 1 d . -1 H18A H -0.0306(3) 0.8695(3) 0.4287(3) 0.045 Uiso 1 calc R -1 C19 C -0.0944(3) 0.7972(3) 0.4365(3) 0.0420(14) Uani 1 d . -1 H19A H -0.1251(3) 0.8111(3) 0.4805(3) 0.050 Uiso 1 calc R -1 C20 C -0.1033(3) 0.7426(3) 0.4004(3) 0.0367(13) Uani 1 d . -1 H20A H -0.1425(3) 0.7207(3) 0.4204(3) 0.044 Uiso 1 calc R -1 C21 C -0.0732(4) 0.7794(4) -0.0167(3) 0.049(2) Uani 1 d . -1 H21A H -0.0496(4) 0.8170(4) -0.0329(3) 0.059 Uiso 1 calc R -1 C22 C -0.1377(5) 0.7803(4) -0.0539(4) 0.065(2) Uani 1 d . -1 H22A H -0.1581(5) 0.8180(4) -0.0940(4) 0.078 Uiso 1 calc R -1 C23 C -0.1718(4) 0.7241(4) -0.0303(4) 0.061(2) Uani 1 d . -1 H23A H -0.2134(4) 0.7210(4) -0.0556(4) 0.073 Uiso 1 calc R -1 C24 C -0.1442(4) 0.6741(4) 0.0296(3) 0.0475(15) Uani 1 d . -1 H24A H -0.1682(4) 0.6370(4) 0.0467(3) 0.057 Uiso 1 calc R -1 C25 C -0.0800(3) 0.6766(3) 0.0668(3) 0.0333(12) Uani 1 d . -1 C26 C -0.0594(3) 0.5620(3) 0.1544(3) 0.0324(12) Uani 1 d . -1 C27 C -0.0470(4) 0.5023(3) 0.1108(3) 0.0450(15) Uani 1 d . -1 H27A H -0.0395(4) 0.5129(3) 0.0618(3) 0.054 Uiso 1 calc R -1 C28 C -0.0458(4) 0.4283(4) 0.1395(4) 0.053(2) Uani 1 d . -1 H28A H -0.0364(4) 0.3876(4) 0.1104(4) 0.064 Uiso 1 calc R -1 C29 C -0.0586(4) 0.4140(4) 0.2110(4) 0.054(2) Uani 1 d . -1 H29A H -0.0609(4) 0.3648(4) 0.2316(4) 0.065 Uiso 1 calc R -1 C30 C -0.0678(4) 0.4729(3) 0.2512(3) 0.0442(14) Uani 1 d . -1 H30A H -0.0728(4) 0.4612(3) 0.3003(3) 0.053 Uiso 1 calc R -1 C31 C 0.1629(3) 0.5783(4) 0.0133(3) 0.0422(14) Uani 1 d . -1 H31A H 0.1476(3) 0.6175(4) -0.0265(3) 0.051 Uiso 1 calc R -1 C32 C 0.2196(4) 0.4978(4) 0.0036(4) 0.055(2) Uani 1 d . -1 H32A H 0.2431(4) 0.4819(4) -0.0416(4) 0.066 Uiso 1 calc R -1 C33 C 0.2419(4) 0.4402(4) 0.0615(4) 0.054(2) Uani 1 d . -1 H33A H 0.2826(4) 0.3844(4) 0.0564(4) 0.065 Uiso 1 calc R -1 C34 C 0.2050(4) 0.4639(3) 0.1268(3) 0.0466(15) Uani 1 d . -1 H34A H 0.2200(4) 0.4243(3) 0.1664(3) 0.056 Uiso 1 calc R -1 C35 C 0.1445(3) 0.5479(3) 0.1349(3) 0.0357(13) Uani 1 d . -1 C36 C 0.1237(3) 0.5400(3) 0.2610(3) 0.0306(12) Uani 1 d . -1 C37 C 0.2131(3) 0.4992(3) 0.2782(3) 0.0370(13) Uani 1 d . -1 H37A H 0.2592(3) 0.4903(3) 0.2426(3) 0.044 Uiso 1 calc R -1 C38 C 0.2328(4) 0.4727(3) 0.3469(3) 0.0452(15) Uani 1 d . -1 H38A H 0.2923(4) 0.4457(3) 0.3585(3) 0.054 Uiso 1 calc R -1 C39 C 0.1650(4) 0.4858(3) 0.3991(3) 0.0446(15) Uani 1 d . -1 H39A H 0.1772(4) 0.4671(3) 0.4463(3) 0.053 Uiso 1 calc R -1 C40 C 0.0785(3) 0.5274(3) 0.3792(3) 0.0363(13) Uani 1 d . -1 H40A H 0.0320(3) 0.5381(3) 0.4146(3) 0.044 Uiso 1 calc R -1 Co4 Co 0.53423(4) 0.24146(4) 0.34255(4) 0.0272(2) Uani 1 d . -1 Co5 Co 0.62156(4) 0.21275(4) 0.43436(4) 0.02453(15) Uani 1 d . -1 Co6 Co 0.71638(4) 0.17708(4) 0.52754(4) 0.0325(2) Uani 1 d . -1 Br3 Br 0.43165(4) 0.27912(4) 0.24010(3) 0.0456(2) Uani 1 d . -1 Br4 Br 0.81344(4) 0.13675(4) 0.62909(3) 0.0456(2) Uani 1 d . -1 N13 N 0.4459(2) 0.2296(2) 0.4177(2) 0.0293(10) Uani 1 d . -1 N14 N 0.5628(2) 0.1543(2) 0.4880(2) 0.0255(9) Uani 1 d . -1 N15 N 0.6873(2) 0.0786(2) 0.5497(2) 0.0296(10) Uani 1 d . -1 N16 N 0.5915(2) 0.1200(2) 0.3378(2) 0.0280(9) Uani 1 d . -1 N17 N 0.7056(2) 0.1131(2) 0.3952(2) 0.0267(9) Uani 1 d . -1 N18 N 0.8144(2) 0.1119(2) 0.4551(2) 0.0314(10) Uani 1 d . -1 N19 N 0.6356(3) 0.2478(2) 0.2835(2) 0.0300(10) Uani 1 d . -1 N20 N 0.6804(2) 0.2715(2) 0.3819(2) 0.0292(10) Uani 1 d . -1 N21 N 0.7302(3) 0.2808(3) 0.4833(2) 0.0344(10) Uani 1 d . -1 N22 N 0.4914(2) 0.3589(2) 0.3590(2) 0.0305(10) Uani 1 d . -1 N23 N 0.5354(2) 0.3123(2) 0.4719(2) 0.0274(9) Uani 1 d . -1 N24 N 0.5955(3) 0.2562(2) 0.5789(2) 0.0317(10) Uani 1 d . -1 C41 C 0.3568(3) 0.2682(3) 0.4098(3) 0.0383(13) Uani 1 d . -1 H41A H 0.3366(3) 0.2990(3) 0.3667(3) 0.046 Uiso 1 calc R -1 C42 C 0.2956(3) 0.2641(3) 0.4618(3) 0.047(2) Uani 1 d . -1 H42A H 0.2347(3) 0.2921(3) 0.4544(3) 0.056 Uiso 1 calc R -1 C43 C 0.3237(3) 0.2189(4) 0.5251(3) 0.052(2) Uani 1 d . -1 H43A H 0.2824(3) 0.2150(4) 0.5612(3) 0.062 Uiso 1 calc R -1 C44 C 0.4127(3) 0.1796(3) 0.5348(3) 0.0417(14) Uani 1 d . -1 H44A H 0.4329(3) 0.1490(3) 0.5780(3) 0.050 Uiso 1 calc R -1 C45 C 0.4737(3) 0.1849(3) 0.4800(3) 0.0283(11) Uani 1 d . -1 C46 C 0.6108(3) 0.0836(3) 0.5304(3) 0.0282(11) Uani 1 d . -1 C47 C 0.5899(3) 0.0166(3) 0.5474(3) 0.0379(13) Uani 1 d . -1 H47A H 0.5351(3) 0.0223(3) 0.5363(3) 0.045 Uiso 1 calc R -1 C48 C 0.6493(4) -0.0568(3) 0.5800(3) 0.0465(15) Uani 1 d . -1 H48A H 0.6359(4) -0.1019(3) 0.5917(3) 0.056 Uiso 1 calc R -1 C49 C 0.7305(4) -0.0635(3) 0.5955(3) 0.048(2) Uani 1 d . -1 H49A H 0.7738(4) -0.1139(3) 0.6160(3) 0.058 Uiso 1 calc R -1 C50 C 0.7456(3) 0.0046(3) 0.5803(3) 0.0403(14) Uani 1 d . -1 H50A H 0.7999(3) -0.0002(3) 0.5917(3) 0.048 Uiso 1 calc R -1 C51 C 0.5498(3) 0.0826(3) 0.3135(3) 0.0354(13) Uani 1 d . -1 H51A H 0.4924(3) 0.1157(3) 0.2980(3) 0.042 Uiso 1 calc R -1 C52 C 0.5881(4) -0.0019(3) 0.3104(3) 0.0411(14) Uani 1 d . -1 H52A H 0.5576(4) -0.0261(3) 0.2930(3) 0.049 Uiso 1 calc R -1 C53 C 0.6723(3) -0.0506(3) 0.3334(3) 0.0383(13) Uani 1 d . -1 H53A H 0.7002(3) -0.1084(3) 0.3309(3) 0.046 Uiso 1 calc R -1 C54 C 0.7142(3) -0.0144(3) 0.3596(3) 0.0314(12) Uani 1 d . -1 H54A H 0.7710(3) -0.0475(3) 0.3761(3) 0.038 Uiso 1 calc R -1 C55 C 0.6733(3) 0.0728(3) 0.3625(3) 0.0272(11) Uani 1 d . -1 C56 C 0.7940(3) 0.0872(3) 0.3993(3) 0.0274(11) Uani 1 d . -1 C57 C 0.8608(3) 0.0457(3) 0.3481(3) 0.0377(13) Uani 1 d . -1 H57A H 0.8466(3) 0.0290(3) 0.3098(3) 0.045 Uiso 1 calc R -1 C58 C 0.9472(3) 0.0295(3) 0.3543(3) 0.0416(14) Uani 1 d . -1 H58A H 0.9923(3) 0.0018(3) 0.3202(3) 0.050 Uiso 1 calc R -1 C59 C 0.9669(3) 0.0540(3) 0.4108(3) 0.0456(15) Uani 1 d . -1 H59A H 1.0259(3) 0.0420(3) 0.4165(3) 0.055 Uiso 1 calc R -1 C60 C 0.8992(3) 0.0965(3) 0.4588(3) 0.0391(13) Uani 1 d . -1 H60A H 0.9128(3) 0.1155(3) 0.4959(3) 0.047 Uiso 1 calc R -1 C61 C 0.6515(4) 0.2317(3) 0.2157(3) 0.0378(13) Uani 1 d . -1 H61A H 0.6121(4) 0.2185(3) 0.1969(3) 0.045 Uiso 1 calc R -1 C62 C 0.7218(4) 0.2336(4) 0.1725(3) 0.0478(15) Uani 1 d . -1 H62A H 0.7298(4) 0.2226(4) 0.1254(3) 0.057 Uiso 1 calc R -1 C63 C 0.7807(4) 0.2521(4) 0.2003(3) 0.049(2) Uani 1 d . -1 H63A H 0.8298(4) 0.2535(4) 0.1723(3) 0.059 Uiso 1 calc R -1 C64 C 0.7669(3) 0.2682(3) 0.2680(3) 0.0404(14) Uani 1 d . -1 H64A H 0.8065(3) 0.2811(3) 0.2869(3) 0.049 Uiso 1 calc R -1 C65 C 0.6941(3) 0.2659(3) 0.3107(3) 0.0303(12) Uani 1 d . -1 C66 C 0.7136(3) 0.3104(3) 0.4152(3) 0.0327(12) Uani 1 d . -1 C67 C 0.7240(3) 0.3818(3) 0.3857(3) 0.0446(15) Uani 1 d . -1 H67A H 0.7097(3) 0.4039(3) 0.3393(3) 0.053 Uiso 1 calc R -1 C68 C 0.7545(4) 0.4186(4) 0.4242(4) 0.054(2) Uani 1 d . -1 H68A H 0.7634(4) 0.4647(4) 0.4041(4) 0.065 Uiso 1 calc R -1 C69 C 0.7723(4) 0.3877(4) 0.4929(4) 0.058(2) Uani 1 d . -1 H69A H 0.7936(4) 0.4122(4) 0.5203(4) 0.070 Uiso 1 calc R -1 C70 C 0.7584(3) 0.3204(4) 0.5208(3) 0.046(2) Uani 1 d . -1 H70A H 0.7688(3) 0.3007(4) 0.5682(3) 0.055 Uiso 1 calc R -1 C71 C 0.4662(3) 0.4199(3) 0.3061(3) 0.0375(13) Uani 1 d . -1 H71A H 0.4693(3) 0.4055(3) 0.2607(3) 0.045 Uiso 1 calc R -1 C72 C 0.4362(3) 0.5021(3) 0.3146(3) 0.0441(14) Uani 1 d . -1 H72A H 0.4213(3) 0.5427(3) 0.2757(3) 0.053 Uiso 1 calc R -1 C73 C 0.4284(3) 0.5238(3) 0.3806(3) 0.046(2) Uani 1 d . -1 H73A H 0.4043(3) 0.5801(3) 0.3882(3) 0.056 Uiso 1 calc R -1 C74 C 0.4557(3) 0.4632(3) 0.4356(3) 0.0382(13) Uani 1 d . -1 H74A H 0.4506(3) 0.4780(3) 0.4812(3) 0.046 Uiso 1 calc R -1 C75 C 0.4916(3) 0.3790(3) 0.4246(3) 0.0299(12) Uani 1 d . -1 C76 C 0.5247(3) 0.3136(3) 0.5431(3) 0.0311(12) Uani 1 d . -1 C77 C 0.4452(3) 0.3638(3) 0.5797(3) 0.0393(13) Uani 1 d . -1 H77A H 0.3957(3) 0.4013(3) 0.5548(3) 0.047 Uiso 1 calc R -1 C78 C 0.4388(4) 0.3590(4) 0.6512(3) 0.047(2) Uani 1 d . -1 H78A H 0.3857(4) 0.3937(4) 0.6756(3) 0.057 Uiso 1 calc R -1 C79 C 0.5116(4) 0.3022(4) 0.6874(3) 0.052(2) Uani 1 d . -1 H79A H 0.5094(4) 0.2986(4) 0.7367(3) 0.062 Uiso 1 calc R -1 C80 C 0.5878(4) 0.2507(4) 0.6495(3) 0.0416(14) Uani 1 d . -1 H80A H 0.6361(4) 0.2103(4) 0.6741(3) 0.050 Uiso 1 calc R -1 C1S C -0.4161(8) 0.6471(6) 0.1122(7) 0.091(7) Uiso 0.40 d PG 1 C2S C -0.4316(7) 0.5777(8) 0.1291(7) 0.036(3) Uiso 0.40 d PGD 1 C3S C -0.3748(10) 0.5094(7) 0.1711(9) 0.152(17) Uiso 0.40 d PG 1 C4S C -0.3026(9) 0.5105(7) 0.1963(8) 0.074(6) Uiso 0.40 d PG 1 C5S C -0.2871(7) 0.5799(8) 0.1795(7) 0.043(4) Uiso 0.40 d PG 1 C6S C -0.3439(9) 0.6482(7) 0.1374(8) 0.048(5) Uiso 0.40 d PGD 1 C7S C -0.4741(12) 0.7097(11) 0.0697(10) 0.074(5) Uiso 0.40 d PD 1 C1' C -0.3917(11) 0.6657(6) 0.1136(8) 0.201(11) Uiso 0.60 d PG 2 C2' C -0.4460(7) 0.6298(10) 0.1060(7) 0.095(4) Uiso 0.60 d PG 2 C3' C -0.4289(10) 0.5516(10) 0.1401(9) 0.163(9) Uiso 0.60 d PG 2 C4' C -0.3574(12) 0.5092(6) 0.1818(9) 0.107(7) Uiso 0.60 d PG 2 C5' C -0.3030(8) 0.5451(10) 0.1895(7) 0.159(8) Uiso 0.60 d PG 2 C6' C -0.3201(9) 0.6233(10) 0.1554(8) 0.068(4) Uiso 0.60 d PG 2 C7' C -0.4062(14) 0.7349(14) 0.0778(12) 0.167(8) Uiso 0.60 d P 2 C8S C 0.0000(10) 0.2458(12) 0.3725(9) 0.111(7) Uiso 0.498(15) d PG 1 C9S C 0.0417(12) 0.2004(9) 0.3152(10) 0.093(6) Uiso 0.498(15) d PG 1 C10S C 0.1106(12) 0.2109(12) 0.2749(8) 0.118(9) Uiso 0.498(15) d PG 1 C11S C 0.1378(10) 0.2667(13) 0.2917(9) 0.097(7) Uiso 0.498(15) d PG 1 C12S C 0.0961(13) 0.3120(10) 0.3489(10) 0.089(6) Uiso 0.498(15) d PG 1 C13S C 0.0272(13) 0.3016(12) 0.3893(9) 0.117(9) Uiso 0.498(15) d PG 1 C14S C 0.1914(14) 0.2853(13) 0.2622(11) 0.126(9) Uiso 0.498(15) d P 1 C12' C 0.1368(10) 0.3013(10) 0.3159(9) 0.085(5) Uiso 0.502(15) d PG 2 C13' C 0.1446(10) 0.2418(11) 0.2746(8) 0.150(10) Uiso 0.502(15) d PGD 2 C8' C 0.0882(11) 0.2046(9) 0.2893(8) 0.065(5) Uiso 0.502(15) d PG 2 C9' C 0.0240(10) 0.2269(10) 0.3453(9) 0.098(6) Uiso 0.502(15) d PGD 2 C10' C 0.0162(11) 0.2864(12) 0.3866(8) 0.127(10) Uiso 0.502(15) d PG 2 C11' C 0.0726(12) 0.3236(9) 0.3719(8) 0.087(6) Uiso 0.502(15) d PG 2 C14' C 0.0919(14) 0.1372(14) 0.2437(12) 0.148(10) Uiso 0.502(15) d PD 2 C15S C 0.1399(24) -0.0255(23) 0.1697(22) 0.255(16) Uiso 0.50 d P 1 C16S C 0.1730(18) -0.0173(17) 0.0987(17) 0.129(10) Uiso 0.50 d P 1 C17S C 0.2440(19) -0.0837(18) 0.0521(15) 0.143(9) Uiso 0.50 d P 1 C18S C 0.3111(23) -0.0948(25) -0.0272(18) 0.187(12) Uiso 0.50 d P 1 C19S C 0.3939(17) -0.1396(17) -0.0730(15) 0.120(8) Uiso 0.50 d P 1 C20S C 0.3932(18) -0.1005(20) -0.1020(15) 0.142(11) Uiso 0.50 d P 1 C15' C 0.3671(13) -0.0506(12) -0.0756(11) 0.097(6) Uiso 0.50 d P 2 C16' C 0.2909(10) -0.0158(10) -0.0241(8) 0.074(4) Uiso 0.50 d P 2 C17' C 0.2589(9) -0.0565(9) 0.0076(8) 0.053(3) Uiso 0.50 d P 2 C18' C 0.3614(14) -0.1728(13) -0.0401(12) 0.102(6) Uiso 0.50 d P 2 C19' C 0.1801(22) -0.0283(20) 0.0644(16) 0.143(11) Uiso 0.50 d P 2 C20' C 0.2965(12) -0.1435(12) 0.0039(10) 0.092(5) Uiso 0.50 d P 2 C21S C 0.4846(11) 0.4707(10) 0.0317(9) 0.077(5) Uiso 0.50 d P . C22S C 0.4087(10) 0.5379(10) 0.0205(9) 0.064(3) Uiso 0.50 d PD . C23S C 0.4083(12) 0.5956(12) -0.0360(11) 0.092(5) Uiso 0.50 d P . C24S C 0.4742(13) 0.5968(11) -0.0778(10) 0.081(5) Uiso 0.50 d P . C25S C 0.5793(13) 0.5110(13) -0.0680(11) 0.095(5) Uiso 0.50 d P . C26S C 0.5649(11) 0.4546(11) -0.0004(9) 0.064(3) Uiso 0.50 d PD . C27S C 0.4743(13) 0.4200(12) 0.0885(10) 0.088(6) Uiso 0.50 d PD . C28S C 0.3981(13) 0.1254(11) 0.0960(10) 0.131(9) Uiso 0.40 d PG 1 C29S C 0.4074(15) 0.0552(14) 0.0689(7) 0.163(14) Uiso 0.40 d PG 1 C30S C 0.4012(13) -0.0095(10) 0.1137(9) 0.077(8) Uiso 0.40 d PG 1 C31S C 0.3857(11) -0.0040(9) 0.1857(8) 0.095(7) Uiso 0.40 d PG 1 C32S C 0.3764(12) 0.0662(11) 0.2128(7) 0.080(8) Uiso 0.40 d PG 1 C33S C 0.3826(12) 0.1309(9) 0.1680(11) 0.106(8) Uiso 0.40 d PG 1 C34S C 0.3776(20) -0.1178(21) 0.1878(17) 0.217(13) Uiso 0.50 d P 1 C28' C 0.3967(8) -0.0660(6) 0.1791(7) 0.106(5) Uiso 0.60 d PG 2 C29' C 0.4116(10) -0.0292(8) 0.1135(5) 0.109(8) Uiso 0.60 d PG 2 C30' C 0.4070(9) 0.0497(8) 0.1071(5) 0.125(6) Uiso 0.60 d PG 2 C31' C 0.3875(9) 0.0917(6) 0.1663(7) 0.107(5) Uiso 0.60 d PG 2 C32' C 0.3726(9) 0.0549(7) 0.2318(6) 0.125(8) Uiso 0.60 d PG 2 C33' C 0.3772(7) -0.0240(7) 0.2383(5) 0.088(4) Uiso 0.60 d PG 2 C34' C 0.3999(18) 0.1007(18) 0.0313(15) 0.176(10) Uiso 0.50 d P 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0344(4) 0.0405(4) 0.0269(4) -0.0074(3) 0.0036(3) -0.0199(3) Co2 0.0266(3) 0.0294(4) 0.0251(4) -0.0056(3) 0.0008(3) -0.0127(3) Co3 0.0340(4) 0.0343(4) 0.0328(4) -0.0076(3) -0.0021(3) -0.0138(3) Br1 0.0677(4) 0.0778(5) 0.0376(4) -0.0080(3) 0.0140(3) -0.0436(4) Br2 0.0554(4) 0.0511(4) 0.0400(3) -0.0040(3) 0.0074(3) -0.0334(3) N1 0.041(3) 0.043(3) 0.026(2) -0.005(2) 0.002(2) -0.023(2) N2 0.028(2) 0.028(2) 0.031(2) -0.003(2) 0.000(2) -0.012(2) N3 0.031(2) 0.038(3) 0.036(3) -0.013(2) 0.004(2) -0.017(2) N4 0.031(2) 0.037(3) 0.039(3) -0.008(2) 0.005(2) -0.018(2) N5 0.030(2) 0.033(2) 0.026(2) -0.005(2) -0.001(2) -0.016(2) N6 0.024(2) 0.033(2) 0.027(2) -0.007(2) 0.003(2) -0.013(2) N7 0.039(3) 0.041(3) 0.027(2) -0.004(2) -0.003(2) -0.017(2) N8 0.035(2) 0.038(3) 0.027(2) -0.010(2) -0.001(2) -0.018(2) N9 0.032(2) 0.034(2) 0.031(3) -0.004(2) -0.001(2) -0.012(2) N10 0.039(2) 0.047(3) 0.027(2) -0.015(2) 0.004(2) -0.024(2) N11 0.028(2) 0.033(2) 0.032(3) -0.011(2) 0.001(2) -0.012(2) N12 0.035(2) 0.031(2) 0.035(3) -0.003(2) -0.003(2) -0.017(2) C1 0.059(4) 0.048(4) 0.049(4) -0.003(3) 0.006(3) -0.035(3) C2 0.077(5) 0.041(4) 0.060(4) -0.003(3) 0.012(4) -0.035(3) C3 0.071(4) 0.037(3) 0.061(5) -0.012(3) 0.005(4) -0.019(3) C4 0.044(3) 0.037(3) 0.042(4) -0.007(3) 0.001(3) -0.016(3) C5 0.037(3) 0.037(3) 0.025(3) 0.000(2) -0.002(2) -0.016(2) C6 0.034(3) 0.030(3) 0.028(3) -0.007(2) -0.003(2) -0.014(2) C7 0.039(3) 0.030(3) 0.049(4) -0.006(3) -0.008(3) -0.012(2) C8 0.035(3) 0.048(4) 0.062(4) -0.019(3) -0.005(3) -0.015(3) C9 0.035(3) 0.063(4) 0.066(5) -0.021(4) 0.002(3) -0.026(3) C10 0.049(4) 0.053(4) 0.048(4) -0.013(3) 0.006(3) -0.035(3) C11 0.039(3) 0.055(4) 0.042(4) -0.012(3) 0.009(3) -0.025(3) C12 0.033(3) 0.065(4) 0.059(4) -0.015(4) 0.013(3) -0.025(3) C13 0.031(3) 0.045(3) 0.055(4) -0.015(3) -0.005(3) -0.016(3) C14 0.033(3) 0.036(3) 0.040(3) -0.008(3) 0.000(3) -0.017(2) C15 0.029(3) 0.030(3) 0.031(3) -0.006(2) 0.001(2) -0.015(2) C16 0.025(3) 0.030(3) 0.029(3) -0.003(2) -0.003(2) -0.011(2) C17 0.030(3) 0.035(3) 0.035(3) -0.008(2) 0.000(2) -0.015(2) C18 0.035(3) 0.032(3) 0.043(3) -0.012(3) -0.005(3) -0.010(2) C19 0.042(3) 0.042(3) 0.036(3) -0.013(3) 0.003(3) -0.013(3) C20 0.032(3) 0.039(3) 0.035(3) -0.006(3) 0.005(2) -0.014(2) C21 0.065(4) 0.050(4) 0.042(4) 0.003(3) -0.008(3) -0.034(3) C22 0.082(5) 0.066(5) 0.050(4) 0.010(4) -0.029(4) -0.035(4) C23 0.067(4) 0.073(5) 0.056(4) 0.008(4) -0.027(4) -0.042(4) C24 0.056(4) 0.050(4) 0.044(4) -0.003(3) -0.012(3) -0.030(3) C25 0.034(3) 0.038(3) 0.028(3) -0.009(2) 0.000(2) -0.015(2) C26 0.027(3) 0.035(3) 0.035(3) -0.005(3) -0.002(2) -0.014(2) C27 0.059(4) 0.042(3) 0.037(3) -0.007(3) -0.014(3) -0.023(3) C28 0.061(4) 0.043(4) 0.058(4) -0.014(3) -0.013(4) -0.020(3) C29 0.064(4) 0.032(3) 0.066(5) 0.005(3) -0.021(4) -0.020(3) C30 0.049(3) 0.038(3) 0.042(4) 0.005(3) -0.007(3) -0.018(3) C31 0.045(3) 0.060(4) 0.030(3) -0.019(3) 0.008(3) -0.029(3) C32 0.055(4) 0.072(5) 0.049(4) -0.036(4) 0.020(3) -0.034(4) C33 0.048(4) 0.048(4) 0.070(5) -0.031(4) 0.014(3) -0.022(3) C34 0.046(3) 0.039(3) 0.052(4) -0.014(3) 0.004(3) -0.016(3) C35 0.026(3) 0.045(3) 0.041(3) -0.015(3) 0.005(2) -0.020(2) C36 0.030(3) 0.025(3) 0.037(3) -0.007(2) -0.001(2) -0.012(2) C37 0.032(3) 0.032(3) 0.044(3) -0.005(3) -0.002(3) -0.012(2) C38 0.037(3) 0.034(3) 0.065(4) 0.001(3) -0.010(3) -0.016(3) C39 0.049(4) 0.041(3) 0.046(4) 0.005(3) -0.014(3) -0.022(3) C40 0.038(3) 0.037(3) 0.036(3) -0.001(3) -0.002(3) -0.019(3) Co4 0.0244(3) 0.0232(3) 0.0314(4) -0.0039(3) -0.0005(3) -0.0086(3) Co5 0.0214(3) 0.0224(3) 0.0287(4) -0.0053(3) 0.0005(3) -0.0089(3) Co6 0.0276(4) 0.0311(4) 0.0395(4) -0.0096(3) 0.0015(3) -0.0132(3) Br3 0.0428(3) 0.0462(4) 0.0438(4) -0.0020(3) -0.0112(3) -0.0155(3) Br4 0.0378(3) 0.0539(4) 0.0472(4) -0.0137(3) -0.0103(3) -0.0182(3) N13 0.026(2) 0.025(2) 0.036(3) -0.006(2) -0.002(2) -0.010(2) N14 0.020(2) 0.027(2) 0.028(2) -0.005(2) -0.002(2) -0.009(2) N15 0.028(2) 0.030(2) 0.029(2) -0.004(2) -0.005(2) -0.010(2) N16 0.027(2) 0.024(2) 0.033(2) -0.005(2) 0.001(2) -0.012(2) N17 0.024(2) 0.025(2) 0.030(2) -0.006(2) -0.002(2) -0.010(2) N18 0.024(2) 0.027(2) 0.040(3) 0.000(2) -0.007(2) -0.010(2) N19 0.032(2) 0.022(2) 0.032(2) 0.000(2) -0.001(2) -0.011(2) N20 0.026(2) 0.031(2) 0.034(3) -0.009(2) 0.003(2) -0.015(2) N21 0.027(2) 0.037(3) 0.040(3) -0.016(2) 0.003(2) -0.013(2) N22 0.027(2) 0.028(2) 0.034(3) -0.003(2) -0.002(2) -0.011(2) N23 0.025(2) 0.025(2) 0.032(2) -0.008(2) 0.001(2) -0.011(2) N24 0.035(2) 0.033(2) 0.031(2) -0.008(2) 0.001(2) -0.018(2) C41 0.026(3) 0.034(3) 0.049(4) -0.005(3) -0.007(3) -0.007(2) C42 0.019(3) 0.042(3) 0.065(4) 0.006(3) -0.003(3) -0.006(2) C43 0.025(3) 0.054(4) 0.063(4) 0.009(3) 0.009(3) -0.015(3) C44 0.032(3) 0.043(3) 0.041(3) 0.003(3) -0.001(3) -0.013(3) C45 0.023(3) 0.022(2) 0.037(3) -0.004(2) -0.002(2) -0.007(2) C46 0.026(3) 0.031(3) 0.026(3) -0.007(2) 0.003(2) -0.011(2) C47 0.038(3) 0.033(3) 0.046(3) 0.001(3) -0.005(3) -0.021(3) C48 0.052(4) 0.035(3) 0.052(4) 0.002(3) -0.006(3) -0.020(3) C49 0.048(4) 0.034(3) 0.047(4) 0.010(3) -0.008(3) -0.009(3) C50 0.030(3) 0.042(3) 0.039(3) -0.003(3) -0.006(3) -0.007(3) C51 0.029(3) 0.038(3) 0.041(3) -0.007(3) -0.003(2) -0.016(2) C52 0.047(3) 0.046(3) 0.043(4) -0.015(3) 0.000(3) -0.029(3) C53 0.039(3) 0.026(3) 0.045(3) -0.007(3) 0.002(3) -0.010(2) C54 0.031(3) 0.023(3) 0.036(3) -0.004(2) -0.002(2) -0.009(2) C55 0.024(2) 0.025(3) 0.029(3) -0.004(2) 0.001(2) -0.009(2) C56 0.028(3) 0.018(2) 0.034(3) 0.001(2) -0.001(2) -0.010(2) C57 0.033(3) 0.033(3) 0.041(3) -0.014(3) 0.004(3) -0.009(2) C58 0.028(3) 0.038(3) 0.051(4) -0.009(3) 0.008(3) -0.010(2) C59 0.024(3) 0.049(4) 0.062(4) 0.002(3) 0.000(3) -0.018(3) C60 0.031(3) 0.037(3) 0.054(4) -0.006(3) -0.005(3) -0.019(2) C61 0.044(3) 0.038(3) 0.029(3) -0.004(3) -0.004(3) -0.016(3) C62 0.053(4) 0.053(4) 0.032(3) -0.006(3) 0.006(3) -0.021(3) C63 0.047(4) 0.051(4) 0.044(4) -0.004(3) 0.013(3) -0.023(3) C64 0.038(3) 0.048(3) 0.040(3) -0.009(3) 0.009(3) -0.025(3) C65 0.026(3) 0.024(3) 0.038(3) 0.002(2) 0.000(2) -0.011(2) C66 0.021(2) 0.037(3) 0.041(3) -0.012(3) 0.008(2) -0.013(2) C67 0.041(3) 0.038(3) 0.056(4) -0.005(3) 0.007(3) -0.022(3) C68 0.048(4) 0.047(4) 0.080(5) -0.023(4) 0.015(4) -0.032(3) C69 0.061(4) 0.054(4) 0.080(5) -0.024(4) -0.001(4) -0.039(3) C70 0.040(3) 0.052(4) 0.052(4) -0.025(3) 0.001(3) -0.021(3) C71 0.031(3) 0.034(3) 0.041(3) 0.004(3) -0.004(3) -0.011(2) C72 0.044(3) 0.027(3) 0.051(4) 0.007(3) -0.001(3) -0.011(3) C73 0.036(3) 0.023(3) 0.074(5) -0.006(3) 0.002(3) -0.010(2) C74 0.034(3) 0.032(3) 0.048(4) -0.012(3) 0.005(3) -0.015(2) C75 0.019(2) 0.026(3) 0.041(3) -0.006(2) 0.005(2) -0.009(2) C76 0.032(3) 0.026(3) 0.038(3) -0.012(2) 0.002(2) -0.014(2) C77 0.032(3) 0.037(3) 0.043(4) -0.012(3) 0.007(3) -0.010(2) C78 0.044(3) 0.045(4) 0.050(4) -0.017(3) 0.014(3) -0.019(3) C79 0.065(4) 0.070(4) 0.038(4) -0.019(3) 0.011(3) -0.046(4) C80 0.052(4) 0.048(3) 0.036(3) -0.004(3) 0.001(3) -0.033(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 Co2 2.3052(10) . y Co2 Co3 2.4512(10) . y Co1 Br1 2.5874(10) . y Co3 Br2 2.5566(10) . y Co1 N1 1.972(4) . y Co1 N4 1.973(4) . y Co1 N7 1.974(4) . y Co1 N10 1.984(4) . y Co2 N2 1.904(4) . y Co2 N5 1.900(4) . y Co2 N8 1.911(4) . y Co2 N11 1.902(4) . y Co3 N3 2.092(4) . y Co3 N6 2.108(4) . y Co3 N9 2.089(4) . y Co3 N12 2.097(4) . y N1 C5 1.355(6) . ? N1 C1 1.362(7) . ? N2 C6 1.358(6) . ? N2 C5 1.365(6) . ? N3 C10 1.360(6) . ? N3 C6 1.376(6) . ? N4 C11 1.339(6) . ? N4 C15 1.367(6) . ? N5 C16 1.370(6) . ? N5 C15 1.376(6) . ? N6 C20 1.349(6) . ? N6 C16 1.356(6) . ? N7 C21 1.334(7) . ? N7 C25 1.356(6) . ? N8 C25 1.366(6) . ? N8 C26 1.369(6) . ? N9 C30 1.347(6) . ? N9 C26 1.363(6) . ? N10 C31 1.357(6) . ? N10 C35 1.370(7) . ? N11 C35 1.352(6) . ? N11 C36 1.372(6) . ? N12 C40 1.344(6) . ? N12 C36 1.360(6) . ? C1 C2 1.379(8) . ? C2 C3 1.372(8) . ? C3 C4 1.355(8) . ? C4 C5 1.417(7) . ? C6 C7 1.406(7) . ? C7 C8 1.391(7) . ? C8 C9 1.362(8) . ? C9 C10 1.381(8) . ? C11 C12 1.366(7) . ? C12 C13 1.382(8) . ? C13 C14 1.362(7) . ? C14 C15 1.399(6) . ? C16 C17 1.417(6) . ? C17 C18 1.357(7) . ? C18 C19 1.396(7) . ? C19 C20 1.371(7) . ? C21 C22 1.383(8) . ? C22 C23 1.389(9) . ? C23 C24 1.348(8) . ? C24 C25 1.406(7) . ? C26 C27 1.400(7) . ? C27 C28 1.370(8) . ? C28 C29 1.373(8) . ? C29 C30 1.359(7) . ? C31 C32 1.357(8) . ? C32 C33 1.373(9) . ? C33 C34 1.369(8) . ? C34 C35 1.413(7) . ? C36 C37 1.410(7) . ? C37 C38 1.373(8) . ? C38 C39 1.379(7) . ? C39 C40 1.385(7) . ? Co4 Co5 2.3099(9) . y Co5 Co6 2.3917(10) . y Co4 Br3 2.6158(9) . y Co6 Br4 2.5350(9) . y Co4 N13 2.007(4) . y Co4 N16 1.974(4) . y Co4 N19 1.976(4) . y Co4 N22 1.979(4) . y Co5 N14 1.892(4) . y Co5 N17 1.908(4) . y Co5 N20 1.887(4) . y Co5 N23 1.902(4) . y Co6 N15 2.045(4) . y Co6 N18 2.048(4) . y Co6 N21 2.055(4) . y Co6 N24 2.105(4) . y N13 C45 1.353(6) . ? N13 C41 1.363(6) . ? N14 C46 1.372(6) . ? N14 C45 1.374(5) . ? N15 C50 1.352(6) . ? N15 C46 1.361(6) . ? N16 C51 1.350(6) . ? N16 C55 1.359(6) . ? N17 C55 1.360(6) . ? N17 C56 1.361(6) . ? N18 C60 1.345(6) . ? N18 C56 1.370(6) . ? N19 C61 1.350(6) . ? N19 C65 1.368(6) . ? N20 C66 1.357(6) . ? N20 C65 1.376(6) . ? N21 C66 1.358(7) . ? N21 C70 1.360(6) . ? N22 C71 1.340(6) . ? N22 C75 1.372(6) . ? N23 C76 1.365(6) . ? N23 C75 1.370(6) . ? N24 C80 1.344(6) . ? N24 C76 1.364(6) . ? C41 C42 1.366(7) . ? C42 C43 1.374(8) . ? C43 C44 1.367(7) . ? C44 C45 1.405(7) . ? C46 C47 1.404(7) . ? C47 C48 1.368(7) . ? C48 C49 1.399(7) . ? C49 C50 1.362(8) . ? C51 C52 1.374(7) . ? C52 C53 1.382(7) . ? C53 C54 1.355(6) . ? C54 C55 1.417(6) . ? C56 C57 1.404(6) . ? C57 C58 1.376(7) . ? C58 C59 1.376(8) . ? C59 C60 1.375(7) . ? C61 C62 1.373(7) . ? C62 C63 1.385(8) . ? C63 C64 1.350(7) . ? C64 C65 1.406(6) . ? C66 C67 1.419(7) . ? C67 C68 1.361(7) . ? C68 C69 1.376(9) . ? C69 C70 1.373(8) . ? C71 C72 1.370(7) . ? C72 C73 1.364(8) . ? C73 C74 1.366(8) . ? C74 C75 1.403(6) . ? C76 C77 1.401(6) . ? C77 C78 1.364(8) . ? C78 C79 1.386(8) . ? C79 C80 1.387(7) . ? C1S C7S 1.36(2) . ? C1S C2S 1.39 . ? C1S C6S 1.39 . ? C2S C3S 1.39 . ? C3S C4S 1.39 . ? C4S C5S 1.39 . ? C5S C6S 1.39 . ? C1' C7' 1.27(2) . ? C1' C2' 1.39 . ? C1' C6' 1.39 . ? C2' C3' 1.39 . ? C3' C4' 1.39 . ? C4' C5' 1.39 . ? C5' C6' 1.39 . ? C8S C9S 1.39 . ? C8S C13S 1.39 . ? C9S C10S 1.39 . ? C10S C11S 1.39 . ? C11S C14S 1.16(2) . ? C11S C12S 1.39 . ? C12S C13S 1.39 . ? C12' C13' 1.39 . ? C12' C11' 1.39 . ? C13' C8' 1.39 . ? C8' C9' 1.39 . ? C8' C14' 1.59(2) . ? C9' C10' 1.39 . ? C10' C11' 1.39 . ? C15S C16S 1.42(4) . ? C16S C17S 1.55(4) . ? C17S C18S 1.76(4) . ? C18S C19S 1.50(4) . ? C18S C20S 1.85(4) . ? C19S C20S 0.83(4) . ? C15' C16' 1.47(2) . ? C16' C17' 1.17(2) . ? C17' C20' 1.42(2) . ? C17' C19' 1.55(3) . ? C18' C20' 1.25(2) . ? C21S C25S 1.15(2) 2_665 ? C21S C22S 1.32(2) . ? C21S C26S 1.32(2) 2_665 ? C21S C26S 1.34(2) . ? C21S C24S 1.35(2) 2_665 ? C21S C27S 1.37(2) . ? C21S C23S 1.66(2) 2_665 ? C21S C21S 1.69(3) 2_665 ? C21S C22S 1.90(2) 2_665 ? C22S C25S 1.15(2) 2_665 ? C22S C23S 1.39(2) . ? C22S C21S 1.90(2) 2_665 ? C23S C26S 1.02(2) 2_665 ? C23S C24S 1.30(2) . ? C23S C21S 1.66(2) 2_665 ? C24S C21S 1.35(2) 2_665 ? C24S C25S 1.76(3) . ? C24S C26S 1.86(2) 2_665 ? C25S C22S 1.15(2) 2_665 ? C25S C21S 1.15(2) 2_665 ? C25S C27S 1.21(2) 2_665 ? C25S C26S 1.60(3) . ? C26S C23S 1.02(2) 2_665 ? C26S C21S 1.32(2) 2_665 ? C26S C24S 1.86(2) 2_665 ? C27S C25S 1.21(2) 2_665 ? C27S C23S 2.03(2) 2_665 ? C28S C29S 1.39 . ? C28S C33S 1.39 . ? C29S C30S 1.39 . ? C30S C31S 1.39 . ? C31S C32S 1.39 . ? C32S C33S 1.39 . ? C28' C29' 1.39 . ? C28' C33' 1.39 . ? C29' C30' 1.39 . ? C30' C31' 1.39 . ? C30' C34' 1.60(3) . ? C31' C32' 1.39 . ? C32' C33' 1.39 . ? 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 Co1 Co2 Co3 178.02(4) . . y Co2 Co1 Br1 179.83(4) . . y Co2 Co3 Br2 179.39(4) . . y N1 Co1 N4 89.8(2) . . y N1 Co1 N7 89.9(2) . . y N1 Co1 N10 170.8(2) . . y N4 Co1 N7 170.8(2) . . y N4 Co1 N10 88.3(2) . . y N7 Co1 N10 90.4(2) . . y N3 Co3 N6 88.69(15) . . y N5 Co2 N2 89.4(2) . . y N2 Co2 N8 90.8(2) . . y N11 Co2 N2 179.1(2) . . y N5 Co2 N8 178.8(2) . . y N5 Co2 N11 90.0(2) . . y N11 Co2 N8 89.8(2) . . y N9 Co3 N3 92.8(2) . . y N3 Co3 N12 163.2(2) . . y N9 Co3 N6 163.6(2) . . y N9 Co3 N12 90.2(2) . . y N12 Co3 N6 83.89(15) . . y N1 Co1 Br1 94.25(13) . . y N4 Co1 Br1 95.16(13) . . y N7 Co1 Br1 94.06(14) . . y N10 Co1 Br1 94.91(13) . . y N3 Co3 Br2 97.82(12) . . y N6 Co3 Br2 99.02(11) . . y N9 Co3 Br2 97.00(12) . . y N12 Co3 Br2 98.19(12) . . y N1 Co1 Co2 85.65(13) . . ? N4 Co1 Co2 84.97(13) . . ? N7 Co1 Co2 85.80(13) . . ? N10 Co1 Co2 85.20(13) . . ? N5 Co2 Co1 89.96(13) . . ? N11 Co2 Co1 90.17(13) . . ? N2 Co2 Co1 89.24(13) . . ? N8 Co2 Co1 88.87(13) . . ? N5 Co2 Co3 92.01(13) . . ? N11 Co2 Co3 90.05(13) . . ? N2 Co2 Co3 90.57(13) . . ? N8 Co2 Co3 89.16(13) . . ? N9 Co3 Co2 82.69(12) . . ? N3 Co3 Co2 82.73(12) . . ? N12 Co3 Co2 81.29(12) . . ? N6 Co3 Co2 81.26(11) . . ? C5 N1 C1 117.8(5) . . ? C5 N1 Co1 120.3(3) . . ? C1 N1 Co1 121.9(4) . . ? C6 N2 C5 122.8(4) . . ? C6 N2 Co2 119.9(3) . . ? C5 N2 Co2 117.3(3) . . ? C10 N3 C6 117.4(5) . . ? C10 N3 Co3 121.1(4) . . ? C6 N3 Co3 121.5(3) . . ? C11 N4 C15 117.8(5) . . ? C11 N4 Co1 121.2(4) . . ? C15 N4 Co1 120.9(3) . . ? C16 N5 C15 123.4(4) . . ? C16 N5 Co2 119.7(3) . . ? C15 N5 Co2 116.5(3) . . ? C20 N6 C16 118.1(4) . . ? C20 N6 Co3 118.6(3) . . ? C16 N6 Co3 123.2(3) . . ? C21 N7 C25 118.7(5) . . ? C21 N7 Co1 121.5(4) . . ? C25 N7 Co1 119.7(4) . . ? C25 N8 C26 122.6(4) . . ? C25 N8 Co2 118.0(3) . . ? C26 N8 Co2 119.4(3) . . ? C30 N9 C26 117.6(4) . . ? C30 N9 Co3 120.6(4) . . ? C26 N9 Co3 121.5(3) . . ? C31 N10 C35 118.4(5) . . ? C31 N10 Co1 122.2(4) . . ? C35 N10 Co1 119.4(3) . . ? C35 N11 C36 124.1(4) . . ? C35 N11 Co2 118.2(4) . . ? C36 N11 Co2 117.4(3) . . ? C40 N12 C36 118.4(4) . . ? C40 N12 Co3 118.7(3) . . ? C36 N12 Co3 122.1(3) . . ? N1 C1 C2 123.3(6) . . ? C3 C2 C1 118.2(6) . . ? C4 C3 C2 120.5(6) . . ? C3 C4 C5 119.6(5) . . ? N1 C5 N2 115.2(4) . . ? N1 C5 C4 120.6(5) . . ? N2 C5 C4 124.0(5) . . ? N2 C6 N3 116.1(4) . . ? N2 C6 C7 123.7(5) . . ? N3 C6 C7 120.1(5) . . ? C8 C7 C6 120.4(6) . . ? C9 C8 C7 119.0(6) . . ? C8 C9 C10 119.0(6) . . ? N3 C10 C9 123.8(6) . . ? N4 C11 C12 124.1(5) . . ? C11 C12 C13 118.3(5) . . ? C14 C13 C12 119.1(5) . . ? C13 C14 C15 120.6(5) . . ? N4 C15 N5 114.5(4) . . ? N4 C15 C14 120.0(4) . . ? N5 C15 C14 125.3(5) . . ? N6 C16 N5 115.8(4) . . ? N6 C16 C17 120.1(4) . . ? N5 C16 C17 124.1(5) . . ? C18 C17 C16 120.3(5) . . ? C17 C18 C19 119.5(5) . . ? C20 C19 C18 117.8(5) . . ? N6 C20 C19 124.2(5) . . ? N7 C21 C22 123.2(6) . . ? C21 C22 C23 118.2(6) . . ? C24 C23 C22 119.0(6) . . ? C23 C24 C25 120.9(6) . . ? N7 C25 N8 115.2(4) . . ? N7 C25 C24 119.8(5) . . ? N8 C25 C24 124.9(5) . . ? N9 C26 N8 115.2(4) . . ? N9 C26 C27 120.2(5) . . ? N8 C26 C27 124.5(5) . . ? C28 C27 C26 120.0(6) . . ? C27 C28 C29 119.5(6) . . ? C30 C29 C28 118.2(6) . . ? N9 C30 C29 124.3(6) . . ? N10 C31 C32 123.9(6) . . ? C31 C32 C33 118.3(6) . . ? C34 C33 C32 120.1(6) . . ? C33 C34 C35 120.1(6) . . ? N11 C35 N10 115.9(4) . . ? N11 C35 C34 124.9(5) . . ? N10 C35 C34 119.1(5) . . ? N12 C36 N11 115.1(4) . . ? N12 C36 C37 120.1(5) . . ? N11 C36 C37 124.4(5) . . ? C38 C37 C36 120.0(5) . . ? C37 C38 C39 119.9(5) . . ? C38 C39 C40 117.6(5) . . ? N12 C40 C39 124.0(5) . . ? Co4 Co5 Co6 177.41(4) . . y Co5 Co4 Br3 177.98(3) . . y Co5 Co6 Br4 177.82(4) . . y N16 Co4 N13 89.3(2) . . y N19 Co4 N13 169.1(2) . . y N22 Co4 N13 90.9(2) . . y N16 Co4 N19 89.7(2) . . y N16 Co4 N22 170.4(2) . . y N19 Co4 N22 88.3(2) . . y N14 Co5 N17 90.0(2) . . y N20 Co5 N14 179.2(2) . . y N14 Co5 N23 89.5(2) . . y N20 Co5 N17 90.4(2) . . y N23 Co5 N17 178.4(2) . . y N20 Co5 N23 90.1(2) . . y N15 Co6 N18 88.8(2) . . y N15 Co6 N21 165.9(2) . . y N15 Co6 N24 91.7(2) . . y N18 Co6 N21 87.4(2) . . y N18 Co6 N24 164.9(2) . . y N21 Co6 N24 88.4(2) . . y N16 Co4 Br3 95.76(12) . . y N19 Co4 Br3 96.24(12) . . y N22 Co4 Br3 93.82(12) . . y N13 Co4 Br3 94.68(12) . . y N15 Co6 Br4 95.32(11) . . y N18 Co6 Br4 97.37(11) . . y N21 Co6 Br4 98.60(12) . . y N24 Co6 Br4 97.61(12) . . y N16 Co4 Co5 86.15(12) . . ? N19 Co4 Co5 84.41(12) . . ? N22 Co4 Co5 84.28(12) . . ? N13 Co4 Co5 84.67(12) . . ? N20 Co5 Co4 90.39(13) . . ? N14 Co5 Co4 90.25(12) . . ? N23 Co5 Co4 89.87(12) . . ? N17 Co5 Co4 88.61(12) . . ? N20 Co5 Co6 89.89(13) . . ? N14 Co5 Co6 89.49(12) . . ? N23 Co5 Co6 92.70(12) . . ? N17 Co5 Co6 88.82(12) . . ? N15 Co6 Co5 82.81(11) . . ? N18 Co6 Co5 83.72(11) . . ? N21 Co6 Co5 83.31(12) . . ? N24 Co6 Co5 81.37(12) . . ? C45 N13 C41 117.7(4) . . ? C45 N13 Co4 120.1(3) . . ? C41 N13 Co4 122.2(4) . . ? C46 N14 C45 124.0(4) . . ? C46 N14 Co5 119.2(3) . . ? C45 N14 Co5 116.8(3) . . ? C50 N15 C46 117.4(4) . . ? C50 N15 Co6 121.3(3) . . ? C46 N15 Co6 121.1(3) . . ? C51 N16 C55 119.4(4) . . ? C51 N16 Co4 121.6(3) . . ? C55 N16 Co4 118.9(3) . . ? C55 N17 C56 123.4(4) . . ? C55 N17 Co5 117.5(3) . . ? C56 N17 Co5 119.0(3) . . ? C60 N18 C56 118.5(4) . . ? C60 N18 Co6 120.9(4) . . ? C56 N18 Co6 120.4(3) . . ? C61 N19 C65 117.6(4) . . ? C61 N19 Co4 121.4(4) . . ? C65 N19 Co4 120.9(3) . . ? C66 N20 C65 123.1(4) . . ? C66 N20 Co5 120.1(3) . . ? C65 N20 Co5 116.5(3) . . ? C66 N21 C70 118.2(5) . . ? C66 N21 Co6 120.8(3) . . ? C70 N21 Co6 121.0(4) . . ? C71 N22 C75 118.5(4) . . ? C71 N22 Co4 121.0(3) . . ? C75 N22 Co4 120.4(3) . . ? C76 N23 C75 124.8(4) . . ? C76 N23 Co5 118.3(3) . . ? C75 N23 Co5 116.8(3) . . ? C80 N24 C76 118.6(4) . . ? C80 N24 Co6 119.1(4) . . ? C76 N24 Co6 122.3(3) . . ? N13 C41 C42 122.8(5) . . ? C41 C42 C43 119.6(5) . . ? C44 C43 C42 119.0(5) . . ? C43 C44 C45 119.8(5) . . ? N13 C45 N14 115.4(4) . . ? N13 C45 C44 121.1(4) . . ? N14 C45 C44 123.0(5) . . ? N15 C46 N14 114.5(4) . . ? N15 C46 C47 121.0(5) . . ? N14 C46 C47 124.1(4) . . ? C48 C47 C46 119.9(5) . . ? C47 C48 C49 118.8(5) . . ? C50 C49 C48 118.6(5) . . ? N15 C50 C49 124.0(5) . . ? N16 C51 C52 122.5(5) . . ? C51 C52 C53 118.9(5) . . ? C54 C53 C52 119.4(5) . . ? C53 C54 C55 120.7(5) . . ? N16 C55 N17 116.1(4) . . ? N16 C55 C54 119.0(4) . . ? N17 C55 C54 124.5(4) . . ? N17 C56 N18 114.9(4) . . ? N17 C56 C57 124.6(5) . . ? N18 C56 C57 120.3(4) . . ? C58 C57 C56 119.7(5) . . ? C59 C58 C57 119.5(5) . . ? C60 C59 C58 119.1(5) . . ? N18 C60 C59 122.9(5) . . ? N19 C61 C62 124.0(5) . . ? C61 C62 C63 118.1(5) . . ? C64 C63 C62 119.3(5) . . ? C63 C64 C65 121.0(5) . . ? N19 C65 N20 114.6(4) . . ? N19 C65 C64 119.9(5) . . ? N20 C65 C64 125.1(5) . . ? N20 C66 N21 115.4(5) . . ? N20 C66 C67 124.6(5) . . ? N21 C66 C67 119.8(5) . . ? C68 C67 C66 120.3(6) . . ? C67 C68 C69 119.6(6) . . ? C70 C69 C68 118.7(6) . . ? N21 C70 C69 123.3(6) . . ? N22 C71 C72 123.4(5) . . ? C73 C72 C71 118.6(6) . . ? C72 C73 C74 119.6(5) . . ? C73 C74 C75 120.4(5) . . ? N23 C75 N22 114.6(4) . . ? N23 C75 C74 126.1(5) . . ? N22 C75 C74 119.0(5) . . ? N24 C76 N23 115.5(4) . . ? N24 C76 C77 120.1(5) . . ? N23 C76 C77 124.2(5) . . ? C78 C77 C76 120.6(5) . . ? C77 C78 C79 119.1(5) . . ? C78 C79 C80 118.5(6) . . ? N24 C80 C79 122.9(6) . . ? C7S C1S C2S 115.6(10) . . ? C7S C1S C6S 124.4(10) . . ? C2S C1S C6S 120.0 . . ? C3S C2S C1S 120.0 . . ? C2S C3S C4S 120.0 . . ? C3S C4S C5S 120.0 . . ? C6S C5S C4S 120.0 . . ? C5S C6S C1S 120.0 . . ? C7' C1' C2' 117.8(17) . . ? C7' C1' C6' 122.0(17) . . ? C2' C1' C6' 120.0 . . ? C1' C2' C3' 120.0 . . ? C4' C3' C2' 120.0 . . ? C3' C4' C5' 120.0 . . ? C6' C5' C4' 120.0 . . ? C5' C6' C1' 120.0 . . ? C9S C8S C13S 120.0 . . ? C8S C9S C10S 120.0 . . ? C11S C10S C9S 120.0 . . ? C14S C11S C10S 128.9(20) . . ? C14S C11S C12S 111.0(20) . . ? C10S C11S C12S 120.0 . . ? C13S C12S C11S 120.0 . . ? C12S C13S C8S 120.0 . . ? C13' C12' C11' 120.0 . . ? C12' C13' C8' 120.0 . . ? C9' C8' C13' 120.0 . . ? C9' C8' C14' 117.0(10) . . ? C13' C8' C14' 123.0(10) . . ? C8' C9' C10' 120.0 . . ? C11' C10' C9' 120.0 . . ? C10' C11' C12' 120.0 . . ? C15S C16S C17S 130.7(29) . . ? C16S C17S C18S 142.5(28) . . ? C19S C18S C17S 153.1(32) . . ? C19S C18S C20S 26.3(15) . . ? C17S C18S C20S 169.6(23) . . ? C20S C19S C18S 100.8(37) . . ? C19S C20S C18S 52.9(29) . . ? C17' C16' C15' 121.6(16) . . ? C16' C17' C20' 122.1(17) . . ? C16' C17' C19' 126.8(19) . . ? C20' C17' C19' 110.8(18) . . ? C18' C20' C17' 115.9(19) . . ? C25S C21S C22S 54.8(13) 2_665 . ? C25S C21S C26S 80.4(17) 2_665 2_665 ? C22S C21S C26S 26.4(11) . 2_665 ? C25S C21S C26S 168.1(19) 2_665 . ? C22S C21S C26S 127.5(19) . . ? C26S C21S C26S 101.1(17) 2_665 . ? C25S C21S C24S 88.9(18) 2_665 2_665 ? C22S C21S C24S 143.6(19) . 2_665 ? C26S C21S C24S 166.4(18) 2_665 2_665 ? C26S C21S C24S 87.6(16) . 2_665 ? C25S C21S C27S 56.4(13) 2_665 . ? C22S C21S C27S 110.8(16) . . ? C26S C21S C27S 136.8(18) 2_665 . ? C26S C21S C27S 121.3(18) . . ? C24S C21S C27S 33.7(10) 2_665 . ? C25S C21S C23S 137.3(19) 2_665 2_665 ? C22S C21S C23S 163.9(17) . 2_665 ? C26S C21S C23S 138.2(18) 2_665 2_665 ? C26S C21S C23S 37.9(10) . 2_665 ? C24S C21S C23S 49.7(11) 2_665 2_665 ? C27S C21S C23S 83.4(14) . 2_665 ? C25S C21S C21S 130.0(21) 2_665 2_665 ? C22S C21S C21S 77.3(15) . 2_665 ? C26S C21S C21S 50.9(11) 2_665 2_665 ? C26S C21S C21S 50.2(12) . 2_665 ? C24S C21S C21S 136.8(20) 2_665 2_665 ? C27S C21S C21S 169.1(19) . 2_665 ? C23S C21S C21S 87.7(15) 2_665 2_665 ? C25S C21S C22S 166.3(17) 2_665 2_665 ? C22S C21S C22S 119.9(13) . 2_665 ? C26S C21S C22S 93.5(13) 2_665 2_665 ? C26S C21S C22S 7.6(12) . 2_665 ? C24S C21S C22S 95.1(14) 2_665 2_665 ? C27S C21S C22S 128.8(14) . 2_665 ? C23S C21S C22S 45.4(10) 2_665 2_665 ? C21S C21S C22S 42.6(9) 2_665 2_665 ? C26S C22S C25S 129.7(35) 2_665 2_665 ? C26S C22S C21S 77.1(27) 2_665 . ? C25S C22S C21S 54.8(13) 2_665 . ? C26S C22S C23S 41.4(25) 2_665 . ? C25S C22S C23S 170.4(20) 2_665 . ? C21S C22S C23S 117.6(17) . . ? C26S C22S C21S 17.1(26) 2_665 2_665 ? C25S C22S C21S 113.4(16) 2_665 2_665 ? C21S C22S C21S 60.1(13) . 2_665 ? C23S C22S C21S 58.0(10) . 2_665 ? C26S C23S C24S 106.4(19) 2_665 . ? C26S C23S C22S 23.0(13) 2_665 . ? C24S C23S C22S 129.3(19) . . ? C26S C23S C21S 53.6(13) 2_665 2_665 ? C24S C23S C21S 52.8(11) . 2_665 ? C22S C23S C21S 76.6(14) . 2_665 ? C26S C23S C27S 95.8(16) 2_665 2_665 ? C24S C23S C27S 10.7(11) . 2_665 ? C22S C23S C27S 118.7(15) . 2_665 ? C21S C23S C27S 42.2(9) 2_665 2_665 ? C27S C24S C23S 151.5(30) 2_665 . ? C27S C24S C21S 74.2(22) 2_665 2_665 ? C23S C24S C21S 77.5(16) . 2_665 ? C27S C24S C25S 35.6(19) 2_665 . ? C23S C24S C25S 117.4(17) . . ? C21S C24S C25S 40.7(10) 2_665 . ? C27S C24S C26S 119.9(26) 2_665 2_665 ? C23S C24S C26S 31.7(10) . 2_665 ? C21S C24S C26S 45.8(10) 2_665 2_665 ? C25S C24S C26S 86.0(12) . 2_665 ? C22S C25S C21S 70.4(17) 2_665 2_665 ? C22S C25S C27S 140.8(23) 2_665 2_665 ? C21S C25S C27S 71.2(16) 2_665 2_665 ? C22S C25S C26S 16.9(12) 2_665 . ? C21S C25S C26S 54.7(13) 2_665 . ? C27S C25S C26S 125.9(19) 2_665 . ? C22S C25S C24S 120.8(18) 2_665 . ? C21S C25S C24S 50.4(13) 2_665 . ? C27S C25S C24S 22.4(12) 2_665 . ? C26S C25S C24S 104.7(14) . . ? C22S C26S C23S 115.6(34) 2_665 2_665 ? C22S C26S C21S 76.4(28) 2_665 2_665 ? C23S C26S C21S 163.6(22) 2_665 2_665 ? C22S C26S C21S 155.3(37) 2_665 . ? C23S C26S C21S 88.4(18) 2_665 . ? C21S C26S C21S 78.9(17) 2_665 . ? C22S C26S C25S 33.4(25) 2_665 . ? C23S C26S C25S 148.8(20) 2_665 . ? C21S C26S C25S 44.9(10) 2_665 . ? C21S C26S C25S 122.7(18) . . ? C22S C26S C24S 157.0(33) 2_665 2_665 ? C23S C26S C24S 41.9(13) 2_665 2_665 ? C21S C26S C24S 124.6(16) 2_665 2_665 ? C21S C26S C24S 46.5(10) . 2_665 ? C25S C26S C24S 169.3(15) . 2_665 ? C24S C27S C25S 122.0(29) 2_665 2_665 ? C24S C27S C21S 72.1(22) 2_665 . ? C25S C27S C21S 52.4(12) 2_665 . ? C24S C27S C23S 17.8(20) 2_665 2_665 ? C25S C27S C23S 105.5(16) 2_665 2_665 ? C21S C27S C23S 54.5(11) . 2_665 ? C29S C28S C33S 120.0 . . ? C28S C29S C30S 120.0 . . ? C29S C30S C31S 120.0 . . ? C32S C31S C30S 120.0 . . ? C31S C32S C33S 120.0 . . ? C32S C33S C28S 120.0 . . ? C29' C28' C33' 120.0 . . ? C28' C29' C30' 120.0 . . ? C29' C30' C31' 120.0 . . ? C29' C30' C34' 119.5(13) . . ? C31' C30' C34' 118.8(13) . . ? C32' C31' C30' 120.0 . . ? C33' C32' C31' 120.0 . . ? C32' C33' C28' 120.0 . . ? _refine_diff_density_max 1.199 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.100 #===END data_1-1.75C7H8.0.5C6H14_at_295K _audit_creation_method SHELXL _chemical_formula_structural 'Co3(dpa)4Br2.1.75Tol.0.5Hex' _chemical_formula_sum 'C55.25 H53 Br2 Co3 N12' _chemical_formula_weight 1221.71 _chemical_compound_source synthesis 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' 'N' 'N' 0.0061 0.0033 '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' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 17.200(5) _cell_length_b 18.383(6) _cell_length_c 19.385(6) _cell_angle_alpha 81.049(6) _cell_angle_beta 82.046(7) _cell_angle_gamma 62.464(5) _cell_volume 5353.5(28) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 6372 _cell_measurement_theta_min 2.332 _cell_measurement_theta_max 25.652 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method ? _exptl_crystal_F_000 2478 _exptl_absorpt_coefficient_mu 2.461 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.4275 _exptl_absorpt_correction_T_max 0.7765 _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1000' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30543 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.23 _reflns_number_total 18590 _reflns_number_observed 9083 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SADABS _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0441P)^2^] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18590 _refine_ls_number_parameters 1181 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_obs 0.0527 _refine_ls_wR_factor_all 0.1352 _refine_ls_wR_factor_obs 0.1128 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.273 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.276 _refine_ls_shift/esd_max -0.013 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.05513(6) 0.72509(6) 0.09047(5) 0.0517(3) Uani 1 d . -1 Co2 Co -0.00837(5) 0.68034(5) 0.19001(4) 0.0396(2) Uani 1 d . -1 Co3 Co -0.07749(5) 0.62997(5) 0.29381(5) 0.0469(2) Uani 1 d . -1 Br1 Br 0.12607(6) 0.77553(6) -0.02121(4) 0.0905(3) Uani 1 d . -1 Br2 Br -0.14843(5) 0.57717(5) 0.40050(4) 0.0660(2) Uani 1 d . -1 N1 N -0.0240(4) 0.8379(3) 0.1166(3) 0.0534(15) Uani 1 d . -1 N2 N -0.1107(3) 0.7836(3) 0.1834(3) 0.0422(13) Uani 1 d . -1 N3 N -0.1940(3) 0.7258(3) 0.2533(3) 0.0481(14) Uani 1 d . -1 N4 N 0.1410(3) 0.7147(3) 0.1537(3) 0.0501(14) Uani 1 d . -1 N5 N 0.0394(3) 0.7245(3) 0.2460(3) 0.0396(13) Uani 1 d . -1 N6 N -0.0607(3) 0.7200(3) 0.3379(3) 0.0420(13) Uani 1 d . -1 N7 N -0.0402(4) 0.7274(4) 0.0416(3) 0.060(2) Uani 1 d . -1 N8 N -0.0548(3) 0.6370(3) 0.1320(3) 0.0459(13) Uani 1 d . -1 N9 N -0.0701(3) 0.5487(3) 0.2245(3) 0.0469(14) Uani 1 d . -1 N10 N 0.1263(3) 0.6061(3) 0.0790(3) 0.0520(15) Uani 1 d . -1 N11 N 0.0952(3) 0.5772(3) 0.1969(3) 0.0461(14) Uani 1 d . -1 N12 N 0.0565(3) 0.5551(3) 0.3132(3) 0.0453(13) Uani 1 d . -1 C1 C -0.0059(5) 0.9030(5) 0.0965(4) 0.075(2) Uani 1 d . -1 H1A H 0.0468(5) 0.8931(5) 0.0702(4) 0.090 Uiso 1 calc R -1 C2 C -0.0596(6) 0.9820(5) 0.1122(5) 0.085(3) Uani 1 d . -1 H2A H -0.0451(6) 1.0248(5) 0.0953(5) 0.102 Uiso 1 calc R -1 C3 C -0.1356(6) 0.9960(5) 0.1538(4) 0.080(2) Uani 1 d . -1 H3A H -0.1733(6) 1.0488(5) 0.1659(4) 0.096 Uiso 1 calc R -1 C4 C -0.1556(5) 0.9326(4) 0.1771(4) 0.065(2) Uani 1 d . -1 H4A H -0.2068(5) 0.9420(4) 0.2057(4) 0.078 Uiso 1 calc R -1 C5 C -0.0989(4) 0.8520(4) 0.1579(3) 0.048(2) Uani 1 d . -1 C6 C -0.1923(4) 0.7869(4) 0.2035(3) 0.045(2) Uani 1 d . -1 C7 C -0.2709(4) 0.8465(4) 0.1734(4) 0.058(2) Uani 1 d . -1 H7A H -0.2693(4) 0.8859(4) 0.1376(4) 0.070 Uiso 1 calc R -1 C8 C -0.3490(5) 0.8454(5) 0.1976(4) 0.066(2) Uani 1 d . -1 H8A H -0.4006(5) 0.8845(5) 0.1782(4) 0.079 Uiso 1 calc R -1 C9 C -0.3519(5) 0.7881(5) 0.2495(5) 0.070(2) Uani 1 d . -1 H9A H -0.4053(5) 0.7893(5) 0.2681(5) 0.085 Uiso 1 calc R -1 C10 C -0.2745(5) 0.7287(4) 0.2738(4) 0.059(2) Uani 1 d . -1 H10A H -0.2766(5) 0.6869(4) 0.3067(4) 0.071 Uiso 1 calc R -1 C11 C 0.2241(5) 0.6994(4) 0.1292(4) 0.070(2) Uani 1 d . -1 H11A H 0.2395(5) 0.6929(4) 0.0818(4) 0.085 Uiso 1 calc R -1 C12 C 0.2867(5) 0.6927(5) 0.1691(5) 0.079(2) Uani 1 d . -1 H12A H 0.3422(5) 0.6841(5) 0.1491(5) 0.095 Uiso 1 calc R -1 C13 C 0.2657(5) 0.6991(4) 0.2399(5) 0.068(2) Uani 1 d . -1 H13A H 0.3066(5) 0.6955(4) 0.2686(5) 0.082 Uiso 1 calc R -1 C14 C 0.1833(4) 0.7107(4) 0.2671(4) 0.056(2) Uani 1 d . -1 H14A H 0.1691(4) 0.7127(4) 0.3151(4) 0.067 Uiso 1 calc R -1 C15 C 0.1210(4) 0.7195(3) 0.2238(3) 0.042(2) Uani 1 d . -1 C16 C -0.0036(4) 0.7506(4) 0.3090(3) 0.042(2) Uani 1 d . -1 C17 C 0.0047(4) 0.8098(4) 0.3424(3) 0.045(2) Uani 1 d . -1 H17A H 0.0413(4) 0.8330(4) 0.3217(3) 0.054 Uiso 1 calc R -1 C18 C -0.0403(4) 0.8322(4) 0.4041(4) 0.055(2) Uani 1 d . -1 H18A H -0.0337(4) 0.8700(4) 0.4265(4) 0.066 Uiso 1 calc R -1 C19 C -0.0963(5) 0.7996(4) 0.4346(4) 0.062(2) Uani 1 d . -1 H19A H -0.1269(5) 0.8141(4) 0.4777(4) 0.074 Uiso 1 calc R -1 C20 C -0.1053(4) 0.7455(4) 0.3994(3) 0.049(2) Uani 1 d . -1 H20A H -0.1446(4) 0.7249(4) 0.4190(3) 0.059 Uiso 1 calc R -1 C21 C -0.0692(5) 0.7781(5) -0.0160(4) 0.075(2) Uani 1 d . -1 H21A H -0.0452(5) 0.8144(5) -0.0319(4) 0.090 Uiso 1 calc R -1 C22 C -0.1329(6) 0.7805(6) -0.0538(5) 0.101(3) Uani 1 d . -1 H22A H -0.1508(6) 0.8164(6) -0.0943(5) 0.121 Uiso 1 calc R -1 C23 C -0.1686(6) 0.7273(6) -0.0289(5) 0.101(3) Uani 1 d . -1 H23A H -0.2111(6) 0.7264(6) -0.0532(5) 0.121 Uiso 1 calc R -1 C24 C -0.1422(5) 0.6759(5) 0.0310(4) 0.073(2) Uani 1 d . -1 H24A H -0.1661(5) 0.6397(5) 0.0476(4) 0.088 Uiso 1 calc R -1 C25 C -0.0787(4) 0.6783(4) 0.0675(4) 0.051(2) Uani 1 d . -1 C26 C -0.0589(4) 0.5645(4) 0.1547(4) 0.046(2) Uani 1 d . -1 C27 C -0.0469(4) 0.5055(5) 0.1107(4) 0.066(2) Uani 1 d . -1 H27A H -0.0391(4) 0.5164(5) 0.0625(4) 0.079 Uiso 1 calc R -1 C28 C -0.0466(5) 0.4326(5) 0.1381(5) 0.081(3) Uani 1 d . -1 H28A H -0.0385(5) 0.3938(5) 0.1088(5) 0.098 Uiso 1 calc R -1 C29 C -0.0584(5) 0.4167(4) 0.2097(5) 0.079(3) Uani 1 d . -1 H29A H -0.0595(5) 0.3676(4) 0.2294(5) 0.095 Uiso 1 calc R -1 C30 C -0.0684(4) 0.4751(4) 0.2512(4) 0.066(2) Uani 1 d . -1 H30A H -0.0743(4) 0.4638(4) 0.2996(4) 0.079 Uiso 1 calc R -1 C31 C 0.1619(5) 0.5792(5) 0.0150(4) 0.068(2) Uani 1 d . -1 H31A H 0.1482(5) 0.6181(5) -0.0240(4) 0.082 Uiso 1 calc R -1 C32 C 0.2166(5) 0.4988(6) 0.0048(5) 0.084(3) Uani 1 d . -1 H32A H 0.2391(5) 0.4829(6) -0.0398(5) 0.101 Uiso 1 calc R -1 C33 C 0.2372(5) 0.4421(5) 0.0630(5) 0.084(3) Uani 1 d . -1 H33A H 0.2765(5) 0.3873(5) 0.0580(5) 0.101 Uiso 1 calc R -1 C34 C 0.2008(4) 0.4651(4) 0.1287(4) 0.067(2) Uani 1 d . -1 H34A H 0.2141(4) 0.4263(4) 0.1678(4) 0.081 Uiso 1 calc R -1 C35 C 0.1422(4) 0.5497(4) 0.1355(4) 0.052(2) Uani 1 d . -1 C36 C 0.1218(4) 0.5415(4) 0.2620(4) 0.042(2) Uani 1 d . -1 C37 C 0.2100(4) 0.5003(4) 0.2787(4) 0.056(2) Uani 1 d . -1 H37A H 0.2549(4) 0.4917(4) 0.2434(4) 0.067 Uiso 1 calc R -1 C38 C 0.2298(5) 0.4730(4) 0.3471(4) 0.062(2) Uani 1 d . -1 H38A H 0.2881(5) 0.4454(4) 0.3583(4) 0.075 Uiso 1 calc R -1 C39 C 0.1628(5) 0.4867(4) 0.3986(4) 0.064(2) Uani 1 d . -1 H39A H 0.1749(5) 0.4681(4) 0.4452(4) 0.077 Uiso 1 calc R -1 C40 C 0.0769(5) 0.5288(4) 0.3800(4) 0.055(2) Uani 1 d . -1 H40A H 0.0314(5) 0.5393(4) 0.4151(4) 0.066 Uiso 1 calc R -1 Co4 Co 0.53493(5) 0.24144(5) 0.34326(5) 0.0416(2) Uani 1 d . -1 Co5 Co 0.62317(5) 0.21201(5) 0.43433(4) 0.0357(2) Uani 1 d . -1 Co6 Co 0.71882(5) 0.17620(5) 0.52840(5) 0.0476(2) Uani 1 d . -1 Br3 Br 0.43285(5) 0.27878(5) 0.24241(4) 0.0676(2) Uani 1 d . -1 Br4 Br 0.81515(5) 0.13726(5) 0.62738(4) 0.0685(2) Uani 1 d . -1 N13 N 0.4484(3) 0.2283(3) 0.4198(3) 0.0400(13) Uani 1 d . -1 N14 N 0.5654(3) 0.1535(3) 0.4878(3) 0.0370(12) Uani 1 d . -1 N15 N 0.6883(3) 0.0776(3) 0.5494(3) 0.0423(13) Uani 1 d . -1 N16 N 0.5926(3) 0.1201(3) 0.3386(3) 0.0412(13) Uani 1 d . -1 N17 N 0.7061(3) 0.1139(3) 0.3938(3) 0.0390(13) Uani 1 d . -1 N18 N 0.8154(3) 0.1117(3) 0.4532(3) 0.0434(13) Uani 1 d . -1 N19 N 0.6352(3) 0.2490(3) 0.2833(3) 0.0457(14) Uani 1 d . -1 N20 N 0.6805(3) 0.2721(3) 0.3813(3) 0.0393(12) Uani 1 d . -1 N21 N 0.7300(3) 0.2821(3) 0.4819(3) 0.0492(14) Uani 1 d . -1 N22 N 0.4928(3) 0.3582(3) 0.3605(3) 0.0434(13) Uani 1 d . -1 N23 N 0.5371(3) 0.3106(3) 0.4729(3) 0.0386(12) Uani 1 d . -1 N24 N 0.5965(3) 0.2552(3) 0.5790(3) 0.0463(13) Uani 1 d . -1 C41 C 0.3604(4) 0.2673(4) 0.4127(4) 0.052(2) Uani 1 d . -1 H41A H 0.3404(4) 0.2979(4) 0.3703(4) 0.062 Uiso 1 calc R -1 C42 C 0.2998(4) 0.2635(4) 0.4651(4) 0.066(2) Uani 1 d . -1 H42A H 0.2399(4) 0.2918(4) 0.4588(4) 0.079 Uiso 1 calc R -1 C43 C 0.3290(5) 0.2173(5) 0.5270(4) 0.070(2) Uani 1 d . -1 H43A H 0.2889(5) 0.2137(5) 0.5631(4) 0.084 Uiso 1 calc R -1 C44 C 0.4169(4) 0.1764(4) 0.5359(4) 0.058(2) Uani 1 d . -1 H44A H 0.4369(4) 0.1446(4) 0.5779(4) 0.070 Uiso 1 calc R -1 C45 C 0.4772(4) 0.1829(3) 0.4808(3) 0.039(2) Uani 1 d . -1 C46 C 0.6125(4) 0.0829(4) 0.5290(3) 0.040(2) Uani 1 d . -1 C47 C 0.5929(4) 0.0156(4) 0.5455(4) 0.056(2) Uani 1 d . -1 H47A H 0.5402(4) 0.0204(4) 0.5332(4) 0.067 Uiso 1 calc R -1 C48 C 0.6501(5) -0.0567(4) 0.5795(4) 0.067(2) Uani 1 d . -1 H48A H 0.6366(5) -0.1008(4) 0.5914(4) 0.080 Uiso 1 calc R -1 C49 C 0.7300(5) -0.0627(5) 0.5961(4) 0.073(2) Uani 1 d . -1 H49A H 0.7723(5) -0.1117(5) 0.6168(4) 0.087 Uiso 1 calc R -1 C50 C 0.7436(4) 0.0057(5) 0.5809(4) 0.061(2) Uani 1 d . -1 H50A H 0.7957(4) 0.0018(5) 0.5935(4) 0.073 Uiso 1 calc R -1 C51 C 0.5518(4) 0.0830(4) 0.3145(3) 0.054(2) Uani 1 d . -1 H51A H 0.4956(4) 0.1155(4) 0.2997(3) 0.064 Uiso 1 calc R -1 C52 C 0.5892(5) -0.0004(4) 0.3107(4) 0.061(2) Uani 1 d . -1 H52A H 0.5591(5) -0.0241(4) 0.2939(4) 0.074 Uiso 1 calc R -1 C53 C 0.6728(4) -0.0483(4) 0.3325(4) 0.057(2) Uani 1 d . -1 H53A H 0.7001(4) -0.1049(4) 0.3298(4) 0.068 Uiso 1 calc R -1 C54 C 0.7153(4) -0.0127(4) 0.3579(3) 0.048(2) Uani 1 d . -1 H54A H 0.7716(4) -0.0451(4) 0.3726(3) 0.057 Uiso 1 calc R -1 C55 C 0.6740(4) 0.0737(4) 0.3622(3) 0.039(2) Uani 1 d . -1 C56 C 0.7946(4) 0.0882(3) 0.3986(4) 0.043(2) Uani 1 d . -1 C57 C 0.8591(4) 0.0480(4) 0.3461(4) 0.056(2) Uani 1 d . -1 H57A H 0.8438(4) 0.0332(4) 0.3082(4) 0.067 Uiso 1 calc R -1 C58 C 0.9453(4) 0.0305(4) 0.3513(4) 0.064(2) Uani 1 d . -1 H58A H 0.9889(4) 0.0032(4) 0.3173(4) 0.076 Uiso 1 calc R -1 C59 C 0.9657(4) 0.0542(4) 0.4078(4) 0.067(2) Uani 1 d . -1 H59A H 1.0234(4) 0.0422(4) 0.4130(4) 0.080 Uiso 1 calc R -1 C60 C 0.8999(4) 0.0954(4) 0.4559(4) 0.058(2) Uani 1 d . -1 H60A H 0.9140(4) 0.1133(4) 0.4925(4) 0.069 Uiso 1 calc R -1 C61 C 0.6516(5) 0.2331(4) 0.2158(4) 0.058(2) Uani 1 d . -1 H61A H 0.6132(5) 0.2200(4) 0.1972(4) 0.070 Uiso 1 calc R -1 C62 C 0.7218(5) 0.2350(4) 0.1726(4) 0.071(2) Uani 1 d . -1 H62A H 0.7305(5) 0.2233(4) 0.1264(4) 0.085 Uiso 1 calc R -1 C63 C 0.7775(5) 0.2543(5) 0.1995(4) 0.074(2) Uani 1 d . -1 H63A H 0.8239(5) 0.2579(5) 0.1709(4) 0.089 Uiso 1 calc R -1 C64 C 0.7665(4) 0.2685(4) 0.2679(4) 0.062(2) Uani 1 d . -1 H64A H 0.8064(4) 0.2797(4) 0.2863(4) 0.074 Uiso 1 calc R -1 C65 C 0.6942(4) 0.2660(3) 0.3108(4) 0.046(2) Uani 1 d . -1 C66 C 0.7131(4) 0.3117(4) 0.4134(4) 0.046(2) Uani 1 d . -1 C67 C 0.7210(4) 0.3831(4) 0.3838(4) 0.062(2) Uani 1 d . -1 H67A H 0.7064(4) 0.4047(4) 0.3381(4) 0.074 Uiso 1 calc R -1 C68 C 0.7497(5) 0.4202(5) 0.4220(5) 0.077(3) Uani 1 d . -1 H68A H 0.7564(5) 0.4666(5) 0.4018(5) 0.092 Uiso 1 calc R -1 C69 C 0.7691(5) 0.3907(5) 0.4894(6) 0.083(3) Uani 1 d . -1 H69A H 0.7899(5) 0.4157(5) 0.5153(6) 0.100 Uiso 1 calc R -1 C70 C 0.7571(4) 0.3229(5) 0.5184(4) 0.069(2) Uani 1 d . -1 H70A H 0.7681(4) 0.3040(5) 0.5651(4) 0.083 Uiso 1 calc R -1 C71 C 0.4666(4) 0.4193(4) 0.3086(4) 0.052(2) Uani 1 d . -1 H71A H 0.4695(4) 0.4056(4) 0.2638(4) 0.063 Uiso 1 calc R -1 C72 C 0.4360(4) 0.5006(4) 0.3172(4) 0.065(2) Uani 1 d . -1 H72A H 0.4194(4) 0.5411(4) 0.2793(4) 0.077 Uiso 1 calc R -1 C73 C 0.4305(4) 0.5202(4) 0.3835(5) 0.067(2) Uani 1 d . -1 H73A H 0.4071(4) 0.5752(4) 0.3916(5) 0.080 Uiso 1 calc R -1 C74 C 0.4590(4) 0.4601(4) 0.4375(4) 0.056(2) Uani 1 d . -1 H74A H 0.4556(4) 0.4740(4) 0.4823(4) 0.067 Uiso 1 calc R -1 C75 C 0.4936(4) 0.3766(4) 0.4258(4) 0.042(2) Uani 1 d . -1 C76 C 0.5269(4) 0.3116(4) 0.5433(4) 0.043(2) Uani 1 d . -1 C77 C 0.4468(4) 0.3610(4) 0.5790(4) 0.058(2) Uani 1 d . -1 H77A H 0.3986(4) 0.3972(4) 0.5540(4) 0.070 Uiso 1 calc R -1 C78 C 0.4398(5) 0.3558(5) 0.6506(4) 0.067(2) Uani 1 d . -1 H78A H 0.3874(5) 0.3891(5) 0.6745(4) 0.081 Uiso 1 calc R -1 C79 C 0.5122(6) 0.2999(5) 0.6875(4) 0.071(2) Uani 1 d . -1 H79A H 0.5096(6) 0.2959(5) 0.7361(4) 0.085 Uiso 1 calc R -1 C80 C 0.5890(5) 0.2497(4) 0.6488(4) 0.061(2) Uani 1 d . -1 H80A H 0.6368(5) 0.2109(4) 0.6729(4) 0.073 Uiso 1 calc R -1 C1S C -0.4170(10) 0.6476(9) 0.1113(9) 0.108(9) Uiso 0.40 d PG 1 C2S C -0.4305(10) 0.5780(10) 0.1313(10) 0.057(5) Uiso 0.40 d PGD 1 C3S C -0.3726(14) 0.5123(10) 0.1737(13) 0.167(26) Uiso 0.40 d PG 1 C4S C -0.3012(12) 0.5160(10) 0.1960(11) 0.107(9) Uiso 0.40 d PG 1 C5S C -0.2878(10) 0.5856(11) 0.1760(10) 0.067(6) Uiso 0.40 d PG 1 C6S C -0.3457(12) 0.6513(9) 0.1336(11) 0.078(8) Uiso 0.40 d PGD 1 C7S C -0.4751(13) 0.7088(13) 0.0673(11) 0.086(6) Uiso 0.40 d PD 1 C1' C -0.3944(15) 0.6643(8) 0.1121(11) 0.329(23) Uiso 0.60 d PG 2 C2' C -0.4468(10) 0.6269(13) 0.1054(9) 0.114(6) Uiso 0.60 d PG 2 C3' C -0.4281(14) 0.5492(14) 0.1400(12) 0.239(15) Uiso 0.60 d PG 2 C4' C -0.3570(18) 0.5088(9) 0.1812(12) 0.151(15) Uiso 0.60 d PG 2 C5' C -0.3046(11) 0.5461(14) 0.1879(9) 0.194(11) Uiso 0.60 d PG 2 C6' C -0.3233(13) 0.6239(15) 0.1533(11) 0.102(5) Uiso 0.60 d PG 2 C7' C -0.3989(16) 0.7276(17) 0.0789(14) 0.200(10) Uiso 0.60 d P 2 C8S C -0.0116(7) 0.2521(8) 0.3824(7) 0.113(6) Uiso 0.60 d PG 1 C9S C 0.0325(9) 0.2106(7) 0.3240(8) 0.113(6) Uiso 0.60 d PG 1 C10S C 0.1008(9) 0.2239(8) 0.2872(6) 0.168(10) Uiso 0.60 d PG 1 C11S C 0.1251(7) 0.2788(8) 0.3086(7) 0.097(5) Uiso 0.60 d PG 1 C12S C 0.0810(9) 0.3203(7) 0.3669(7) 0.124(6) Uiso 0.60 d PG 1 C13S C 0.0127(8) 0.3070(8) 0.4038(6) 0.128(6) Uiso 0.60 d PG 1 C14S C 0.1906(25) 0.2707(23) 0.2520(23) 0.241(20) Uiso 0.50 d P 1 C8' C 0.0879(10) 0.2038(9) 0.2874(8) 0.076(7) Uiso 0.40 d PG 2 C9' C 0.0397(9) 0.2437(10) 0.3455(8) 0.092(7) Uiso 0.40 d PGD 2 C10' C 0.0591(11) 0.3002(10) 0.3700(8) 0.113(9) Uiso 0.40 d PG 2 C11' C 0.1267(12) 0.3169(10) 0.3362(10) 0.071(6) Uiso 0.40 d PG 2 C12' C 0.1750(11) 0.2771(12) 0.2781(10) 0.155(18) Uiso 0.40 d PG 2 C13' C 0.1556(10) 0.2205(11) 0.2537(8) 0.098(7) Uiso 0.40 d PGD 2 C14' C 0.0715(22) 0.1534(25) 0.2557(19) 0.290(18) Uiso 0.50 d PD 2 C15S C 0.1360(32) -0.0070(30) 0.1804(27) 0.305(21) Uiso 0.50 d P 1 C16S C 0.2122(43) -0.0635(41) 0.1502(35) 0.358(30) Uiso 0.50 d P 1 C17S C 0.2458(27) -0.0931(26) 0.0648(26) 0.217(16) Uiso 0.50 d P 1 C18S C 0.2607(18) -0.0579(18) 0.0095(15) 0.123(8) Uiso 0.50 d P 1 C19S C 0.3363(31) -0.0914(34) -0.0585(25) 0.242(18) Uiso 0.50 d P 1 C20S C 0.4135(23) -0.1320(25) -0.0916(19) 0.210(14) Uiso 0.50 d P 1 C15' C 0.3806(27) -0.0554(24) -0.0803(20) 0.221(15) Uiso 0.50 d P 2 C16' C 0.2984(18) -0.0225(17) -0.0230(15) 0.150(9) Uiso 0.50 d P 2 C17' C 0.1894(36) -0.0337(33) 0.0540(27) 0.223(19) Uiso 0.50 d P 2 C18' C 0.3684(22) -0.1690(20) -0.0444(17) 0.173(11) Uiso 0.50 d P 2 C19' C 0.1658(30) -0.0109(28) 0.0970(32) 0.236(20) Uiso 0.50 d P 2 C20' C 0.2981(19) -0.1359(18) 0.0006(16) 0.148(9) Uiso 0.50 d P 2 C21S C 0.4914(11) 0.4705(10) 0.0292(9) 0.139(9) Uiso 0.50 d PG . C22S C 0.4161(8) 0.5417(10) 0.0109(9) 0.122(4) Uiso 0.50 d PGD . C23S C 0.4212(10) 0.5977(8) -0.0445(9) 0.127(7) Uiso 0.50 d PG . C24S C 0.5015(13) 0.5825(9) -0.0815(7) 0.176(22) Uiso 0.50 d PG . C25S C 0.5767(9) 0.5113(10) -0.0632(8) 0.113(7) Uiso 0.50 d PG . C26S C 0.5717(9) 0.4553(8) -0.0078(9) 0.122(4) Uiso 0.50 d PGD . C27S C 0.4818(21) 0.4105(23) 0.0853(22) 0.242(29) Uiso 0.50 d PD . C28S C 0.3923(15) 0.1330(12) 0.1465(16) 0.128(10) Uiso 0.40 d PG 1 C29S C 0.4029(22) 0.1082(19) 0.0803(12) 0.272(30) Uiso 0.40 d PG 1 C30S C 0.4043(25) 0.0335(22) 0.0731(12) 0.221(18) Uiso 0.40 d PG 1 C31S C 0.3950(20) -0.0163(15) 0.1322(17) 0.226(20) Uiso 0.40 d PGD 1 C32S C 0.3844(17) 0.0086(15) 0.1984(13) 0.128(10) Uiso 0.40 d PG 1 C33S C 0.3830(17) 0.0833(17) 0.2056(11) 0.162(13) Uiso 0.40 d PG 1 C34S C 0.3567(44) -0.0731(36) 0.1945(27) 0.446(39) Uiso 0.50 d PD 1 C28' C 0.4030(17) -0.0757(12) 0.1781(23) 0.265(7) Uiso 0.60 d PG 2 C29' C 0.4179(18) -0.0363(24) 0.1141(15) 0.265(7) Uiso 0.60 d PG 2 C30' C 0.4131(18) 0.0417(24) 0.1109(15) 0.265(7) Uiso 0.60 d PGD 2 C31' C 0.3934(17) 0.0803(12) 0.1717(25) 0.265(7) Uiso 0.60 d PG 2 C32' C 0.3785(17) 0.0409(23) 0.2356(16) 0.265(7) Uiso 0.60 d PG 2 C33' C 0.3833(16) -0.0372(23) 0.2388(14) 0.265(7) Uiso 0.60 d PG 2 C34' C 0.4200(61) 0.1151(38) 0.0577(33) 0.558(64) Uiso 0.50 d PD 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0546(6) 0.0637(6) 0.0415(6) -0.0138(5) 0.0080(5) -0.0312(5) Co2 0.0387(5) 0.0445(5) 0.0361(5) -0.0106(4) 0.0031(4) -0.0189(4) Co3 0.0454(5) 0.0503(6) 0.0455(6) -0.0109(5) 0.0003(5) -0.0212(4) Br1 0.1081(7) 0.1192(8) 0.0569(5) -0.0152(5) 0.0265(5) -0.0688(6) Br2 0.0753(5) 0.0710(5) 0.0587(5) -0.0058(4) 0.0122(4) -0.0439(4) N1 0.062(4) 0.057(4) 0.047(4) 0.000(3) 0.001(3) -0.034(3) N2 0.041(3) 0.036(3) 0.046(3) -0.001(3) -0.002(3) -0.016(3) N3 0.045(3) 0.055(4) 0.048(4) -0.013(3) 0.007(3) -0.026(3) N4 0.045(3) 0.059(4) 0.053(4) -0.013(3) 0.016(3) -0.033(3) N5 0.041(3) 0.046(3) 0.037(3) -0.010(3) 0.004(3) -0.023(3) N6 0.031(3) 0.049(3) 0.043(3) -0.012(3) 0.005(3) -0.015(3) N7 0.069(4) 0.076(4) 0.036(4) -0.001(3) -0.002(3) -0.035(4) N8 0.052(3) 0.052(4) 0.038(3) -0.009(3) -0.002(3) -0.026(3) N9 0.043(3) 0.049(4) 0.052(4) -0.012(3) -0.001(3) -0.022(3) N10 0.054(4) 0.071(4) 0.036(3) -0.019(3) 0.011(3) -0.032(3) N11 0.043(3) 0.047(3) 0.046(4) -0.016(3) 0.005(3) -0.017(3) N12 0.041(3) 0.049(3) 0.046(4) -0.006(3) -0.001(3) -0.021(3) C1 0.082(6) 0.091(7) 0.072(6) -0.015(5) 0.016(5) -0.059(5) C2 0.105(7) 0.063(6) 0.097(7) -0.015(5) 0.018(6) -0.052(5) C3 0.094(6) 0.053(5) 0.086(7) -0.013(5) 0.005(6) -0.028(5) C4 0.067(5) 0.054(5) 0.075(6) -0.013(4) 0.006(4) -0.028(4) C5 0.050(4) 0.052(4) 0.039(4) 0.006(3) -0.009(4) -0.021(4) C6 0.045(4) 0.043(4) 0.045(4) -0.015(3) -0.002(4) -0.015(3) C7 0.053(5) 0.045(4) 0.065(5) -0.003(4) -0.008(4) -0.011(4) C8 0.045(5) 0.066(6) 0.082(6) -0.016(5) -0.007(4) -0.018(4) C9 0.043(5) 0.082(6) 0.091(7) -0.025(5) -0.006(5) -0.027(5) C10 0.058(5) 0.061(5) 0.071(5) -0.019(4) 0.009(4) -0.037(4) C11 0.057(5) 0.081(6) 0.073(6) -0.017(5) 0.011(5) -0.032(4) C12 0.047(5) 0.097(7) 0.087(7) -0.025(5) 0.017(5) -0.029(5) C13 0.047(5) 0.070(5) 0.094(7) -0.020(5) -0.013(5) -0.025(4) C14 0.049(4) 0.061(5) 0.065(5) -0.022(4) 0.005(4) -0.028(4) C15 0.043(4) 0.039(4) 0.044(4) -0.007(3) 0.000(4) -0.019(3) C16 0.039(4) 0.045(4) 0.039(4) -0.005(3) -0.004(3) -0.017(3) C17 0.048(4) 0.049(4) 0.043(4) -0.015(3) 0.006(3) -0.025(3) C18 0.055(4) 0.048(4) 0.065(5) -0.021(4) 0.000(4) -0.021(4) C19 0.068(5) 0.068(5) 0.046(5) -0.029(4) 0.007(4) -0.023(4) C20 0.034(4) 0.061(4) 0.051(5) -0.014(4) 0.012(3) -0.022(3) C21 0.100(7) 0.087(6) 0.056(5) -0.001(5) -0.012(5) -0.058(5) C22 0.134(9) 0.121(8) 0.061(6) 0.022(6) -0.031(6) -0.072(7) C23 0.123(8) 0.137(9) 0.073(7) 0.017(6) -0.045(6) -0.082(7) C24 0.088(6) 0.085(6) 0.061(5) -0.003(5) -0.018(5) -0.050(5) C25 0.056(5) 0.060(5) 0.040(4) -0.013(4) -0.002(4) -0.026(4) C26 0.043(4) 0.052(4) 0.046(4) -0.010(4) -0.004(4) -0.023(3) C27 0.086(6) 0.066(5) 0.058(5) -0.022(4) -0.008(4) -0.041(5) C28 0.104(7) 0.070(6) 0.083(7) -0.028(5) -0.013(6) -0.043(5) C29 0.099(6) 0.038(5) 0.102(7) -0.006(5) -0.030(6) -0.027(4) C30 0.065(5) 0.059(5) 0.072(6) 0.002(5) -0.018(4) -0.025(4) C31 0.070(5) 0.094(6) 0.046(5) -0.029(5) 0.016(4) -0.041(5) C32 0.085(6) 0.108(8) 0.074(7) -0.054(6) 0.029(6) -0.053(6) C33 0.083(6) 0.072(6) 0.102(7) -0.049(6) 0.027(6) -0.037(5) C34 0.071(5) 0.055(5) 0.069(5) -0.026(4) 0.013(4) -0.022(4) C35 0.048(4) 0.064(5) 0.054(5) -0.023(4) 0.008(4) -0.033(4) C36 0.039(4) 0.034(4) 0.052(5) -0.015(3) 0.004(4) -0.016(3) C37 0.047(4) 0.046(4) 0.069(5) -0.010(4) 0.000(4) -0.017(3) C38 0.051(5) 0.048(5) 0.082(6) 0.002(4) -0.014(5) -0.018(4) C39 0.073(5) 0.054(5) 0.060(5) 0.003(4) -0.020(5) -0.023(4) C40 0.061(5) 0.058(5) 0.043(5) -0.004(4) -0.003(4) -0.024(4) Co4 0.0368(5) 0.0358(5) 0.0474(6) -0.0075(4) 0.0021(4) -0.0129(4) Co5 0.0305(4) 0.0322(5) 0.0429(5) -0.0089(4) 0.0022(4) -0.0126(4) Co6 0.0391(5) 0.0472(6) 0.0579(6) -0.0146(5) 0.0013(5) -0.0192(4) Br3 0.0633(5) 0.0711(5) 0.0634(5) -0.0049(4) -0.0148(4) -0.0241(4) Br4 0.0559(5) 0.0809(6) 0.0722(6) -0.0208(5) -0.0155(4) -0.0272(4) N13 0.035(3) 0.031(3) 0.052(4) -0.009(3) -0.001(3) -0.012(2) N14 0.028(3) 0.033(3) 0.048(3) -0.005(3) -0.004(3) -0.011(2) N15 0.037(3) 0.035(3) 0.045(3) -0.005(3) -0.006(3) -0.008(2) N16 0.039(3) 0.037(3) 0.046(3) -0.008(3) 0.002(3) -0.016(3) N17 0.030(3) 0.037(3) 0.046(3) -0.012(3) -0.001(3) -0.010(2) N18 0.032(3) 0.040(3) 0.057(4) -0.004(3) -0.009(3) -0.014(2) N19 0.046(3) 0.039(3) 0.044(4) -0.006(3) 0.003(3) -0.013(3) N20 0.034(3) 0.044(3) 0.041(3) -0.011(3) 0.007(3) -0.019(2) N21 0.035(3) 0.050(3) 0.067(4) -0.023(3) 0.005(3) -0.020(3) N22 0.037(3) 0.039(3) 0.049(4) -0.002(3) 0.000(3) -0.015(2) N23 0.038(3) 0.032(3) 0.045(3) -0.009(3) 0.002(3) -0.015(2) N24 0.054(3) 0.051(4) 0.042(3) -0.011(3) 0.003(3) -0.030(3) C41 0.036(4) 0.045(4) 0.064(5) -0.002(4) -0.009(4) -0.010(3) C42 0.027(4) 0.068(5) 0.089(6) -0.004(5) 0.002(4) -0.012(4) C43 0.045(5) 0.072(5) 0.075(6) 0.012(5) 0.006(4) -0.021(4) C44 0.041(4) 0.054(4) 0.063(5) 0.009(4) -0.003(4) -0.013(4) C45 0.035(4) 0.029(3) 0.050(4) -0.004(3) 0.002(3) -0.013(3) C46 0.035(4) 0.043(4) 0.040(4) -0.013(3) 0.005(3) -0.016(3) C47 0.059(4) 0.049(4) 0.066(5) 0.004(4) -0.015(4) -0.030(4) C48 0.071(5) 0.038(4) 0.087(6) 0.005(4) -0.011(5) -0.023(4) C49 0.077(6) 0.055(5) 0.071(6) 0.015(4) -0.021(5) -0.019(4) C50 0.049(4) 0.062(5) 0.063(5) -0.009(4) -0.010(4) -0.015(4) C51 0.044(4) 0.053(5) 0.064(5) -0.009(4) -0.009(4) -0.020(4) C52 0.064(5) 0.063(5) 0.069(5) -0.021(4) -0.003(4) -0.036(4) C53 0.056(5) 0.043(4) 0.067(5) -0.019(4) 0.005(4) -0.017(4) C54 0.044(4) 0.035(4) 0.056(4) -0.008(3) 0.001(3) -0.011(3) C55 0.032(3) 0.039(4) 0.043(4) -0.016(3) 0.009(3) -0.012(3) C56 0.040(4) 0.030(4) 0.051(4) 0.000(3) 0.006(4) -0.011(3) C57 0.041(4) 0.049(4) 0.067(5) -0.023(4) 0.004(4) -0.009(3) C58 0.045(5) 0.059(5) 0.076(6) -0.015(4) 0.013(4) -0.017(4) C59 0.032(4) 0.067(5) 0.095(7) 0.000(5) 0.001(4) -0.021(4) C60 0.044(4) 0.058(5) 0.076(6) -0.008(4) -0.004(4) -0.027(4) C61 0.061(5) 0.059(5) 0.041(4) -0.008(4) -0.001(4) -0.016(4) C62 0.071(6) 0.076(6) 0.054(5) -0.007(4) 0.008(5) -0.027(5) C63 0.069(5) 0.090(6) 0.061(6) -0.014(5) 0.028(5) -0.040(5) C64 0.056(5) 0.071(5) 0.061(5) -0.014(4) 0.014(4) -0.034(4) C65 0.040(4) 0.031(4) 0.058(5) 0.000(3) -0.001(4) -0.011(3) C66 0.029(4) 0.051(4) 0.054(5) -0.012(4) 0.008(3) -0.017(3) C67 0.062(5) 0.055(5) 0.075(6) -0.006(4) 0.009(4) -0.036(4) C68 0.071(6) 0.060(5) 0.112(8) -0.024(6) 0.014(6) -0.042(5) C69 0.078(6) 0.075(6) 0.123(9) -0.035(6) 0.000(6) -0.051(5) C70 0.058(5) 0.085(6) 0.074(6) -0.037(5) 0.004(4) -0.034(4) C71 0.042(4) 0.049(4) 0.055(5) 0.000(4) 0.001(4) -0.015(3) C72 0.066(5) 0.042(5) 0.068(6) 0.012(4) 0.001(4) -0.016(4) C73 0.062(5) 0.032(4) 0.099(7) -0.010(5) 0.004(5) -0.018(4) C74 0.056(4) 0.039(4) 0.069(5) -0.015(4) 0.007(4) -0.018(3) C75 0.031(3) 0.037(4) 0.055(5) -0.014(4) 0.009(3) -0.014(3) C76 0.041(4) 0.039(4) 0.051(5) -0.016(3) 0.004(4) -0.018(3) C77 0.054(4) 0.053(4) 0.061(5) -0.016(4) 0.011(4) -0.020(4) C78 0.060(5) 0.063(5) 0.071(6) -0.024(5) 0.017(5) -0.023(4) C79 0.099(6) 0.093(6) 0.045(5) -0.024(5) 0.018(5) -0.065(6) C80 0.063(5) 0.073(5) 0.058(5) -0.005(4) -0.002(4) -0.042(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 Co1 Co2 2.3123(13) . y Co2 Co3 2.4690(13) . y Co1 Br1 2.5935(13) . y Co3 Br2 2.5456(13) . y Co1 N1 1.984(5) . y Co1 N4 1.972(5) . y Co1 N7 1.985(6) . y Co1 N10 1.984(5) . y Co2 N2 1.901(5) . y Co2 N5 1.911(5) . y Co2 N8 1.911(5) . y Co2 N11 1.911(5) . y Co3 N3 2.116(5) . y Co3 N6 2.123(5) . y Co3 N9 2.110(5) . y Co3 N12 2.119(5) . y N1 C5 1.355(7) . ? N1 C1 1.359(8) . ? N2 C5 1.371(7) . ? N2 C6 1.380(7) . ? N3 C10 1.365(7) . ? N3 C6 1.371(8) . ? N4 C11 1.352(8) . ? N4 C15 1.361(7) . ? N5 C16 1.367(7) . ? N5 C15 1.376(7) . ? N6 C20 1.348(7) . ? N6 C16 1.362(7) . ? N7 C21 1.330(9) . ? N7 C25 1.350(8) . ? N8 C25 1.367(8) . ? N8 C26 1.369(7) . ? N9 C26 1.345(8) . ? N9 C30 1.361(8) . ? N10 C35 1.348(8) . ? N10 C31 1.362(7) . ? N11 C36 1.363(8) . ? N11 C35 1.367(7) . ? N12 C40 1.345(8) . ? N12 C36 1.348(7) . ? C1 C2 1.370(9) . ? C2 C3 1.373(9) . ? C3 C4 1.358(9) . ? C4 C5 1.422(8) . ? C6 C7 1.420(8) . ? C7 C8 1.369(9) . ? C8 C9 1.353(10) . ? C9 C10 1.363(9) . ? C11 C12 1.361(10) . ? C12 C13 1.379(10) . ? C13 C14 1.371(8) . ? C14 C15 1.388(8) . ? C16 C17 1.419(8) . ? C17 C18 1.342(8) . ? C18 C19 1.378(8) . ? C19 C20 1.365(8) . ? C21 C22 1.381(10) . ? C22 C23 1.375(11) . ? C23 C24 1.363(10) . ? C24 C25 1.402(9) . ? C26 C27 1.406(8) . ? C27 C28 1.360(10) . ? C28 C29 1.381(10) . ? C29 C30 1.374(9) . ? C31 C32 1.366(10) . ? C32 C33 1.374(11) . ? C33 C34 1.376(10) . ? C34 C35 1.424(9) . ? C36 C37 1.405(8) . ? C37 C38 1.373(9) . ? C38 C39 1.372(9) . ? C39 C40 1.385(9) . ? Co4 Co5 2.3234(13) . y Co5 Co6 2.4333(13) . y Co4 Br3 2.6065(13) . y Co6 Br4 2.5090(13) . y Co4 N13 2.021(5) . y Co4 N16 1.989(5) . y Co4 N19 1.991(5) . y Co4 N22 1.991(5) . y Co5 N14 1.892(5) . y Co5 N17 1.913(4) . y Co5 N20 1.903(5) . y Co5 N23 1.915(4) . y Co6 N15 2.079(5) . y Co6 N18 2.083(5) . y Co6 N21 2.096(5) . y Co6 N24 2.131(5) . y N13 C45 1.345(7) . ? N13 C41 1.360(7) . ? N14 C46 1.364(7) . ? N14 C45 1.373(7) . ? N15 C50 1.330(8) . ? N15 C46 1.371(7) . ? N16 C51 1.344(7) . ? N16 C55 1.358(7) . ? N17 C55 1.356(7) . ? N17 C56 1.380(7) . ? N18 C60 1.349(7) . ? N18 C56 1.351(7) . ? N19 C61 1.347(7) . ? N19 C65 1.380(7) . ? N20 C66 1.361(7) . ? N20 C65 1.367(8) . ? N21 C70 1.364(8) . ? N21 C66 1.369(8) . ? N22 C71 1.335(7) . ? N22 C75 1.362(7) . ? N23 C76 1.354(7) . ? N23 C75 1.368(7) . ? N24 C80 1.334(8) . ? N24 C76 1.358(7) . ? C41 C42 1.370(8) . ? C42 C43 1.366(9) . ? C43 C44 1.364(8) . ? C44 C45 1.415(8) . ? C46 C47 1.407(8) . ? C47 C48 1.367(8) . ? C48 C49 1.406(9) . ? C49 C50 1.363(9) . ? C51 C52 1.373(8) . ? C52 C53 1.379(8) . ? C53 C54 1.358(8) . ? C54 C55 1.420(7) . ? C56 C57 1.405(8) . ? C57 C58 1.380(8) . ? C58 C59 1.381(9) . ? C59 C60 1.363(9) . ? C61 C62 1.382(9) . ? C62 C63 1.350(9) . ? C63 C64 1.362(9) . ? C64 C65 1.412(8) . ? C66 C67 1.407(9) . ? C67 C68 1.353(9) . ? C68 C69 1.358(11) . ? C69 C70 1.379(10) . ? C71 C72 1.365(8) . ? C72 C73 1.367(9) . ? C73 C74 1.355(9) . ? C74 C75 1.410(8) . ? C76 C77 1.406(8) . ? C77 C78 1.370(9) . ? C78 C79 1.397(10) . ? C79 C80 1.405(9) . ? C1S C7S 1.37(2) . ? C1S C2S 1.39 . ? C1S C6S 1.39 . ? C2S C3S 1.39 . ? C3S C4S 1.39 . ? C4S C5S 1.39 . ? C5S C6S 1.39 . ? C1' C7' 1.21(3) . ? C1' C2' 1.39 . ? C1' C6' 1.39 . ? C2' C3' 1.39 . ? C3' C4' 1.39 . ? C4' C5' 1.39 . ? C5' C6' 1.39 . ? C8S C9S 1.39 . ? C8S C13S 1.39 . ? C9S C10S 1.39 . ? C10S C11S 1.39 . ? C11S C12S 1.39 . ? C11S C14S 1.43(4) . ? C12S C13S 1.39 . ? C8' C14' 1.34(4) . ? C8' C9' 1.39 . ? C8' C13' 1.39 . ? C9' C10' 1.39 . ? C10' C11' 1.39 . ? C11' C12' 1.39 . ? C12' C13' 1.39 . ? C15S C16S 1.36(7) . ? C16S C17S 1.76(6) . ? C17S C18S 1.22(5) . ? C18S C19S 1.69(5) . ? C19S C20S 1.31(5) . ? C15' C16' 1.61(4) . ? C17' C19' 0.94(6) . ? C18' C20' 1.34(3) . ? C21S C25S 1.19(3) 2_665 ? C21S C24S 1.27(2) 2_665 ? C21S C26S 1.34(3) 2_665 ? C21S C22S 1.39 . ? C21S C26S 1.39 . ? C21S C27S 1.47(4) . ? C21S C23S 1.48(3) 2_665 ? C21S C21S 1.54(2) 2_665 ? C21S C22S 1.60(3) 2_665 ? C22S C26S 0.24(3) 2_665 ? C22S C25S 1.27(3) 2_665 ? C22S C23S 1.39 . ? C22S C21S 1.60(3) 2_665 ? C23S C26S 1.27(3) 2_665 ? C23S C24S 1.39 . ? C23S C21S 1.48(2) 2_665 ? C23S C27S 1.70(4) 2_665 ? C24S C27S 0.36(5) 2_665 ? C24S C21S 1.27(2) 2_665 ? C24S C25S 1.39 . ? C25S C21S 1.19(3) 2_665 ? C25S C22S 1.27(3) 2_665 ? C25S C27S 1.36(4) 2_665 ? C25S C26S 1.39 . ? C26S C22S 0.24(3) 2_665 ? C26S C23S 1.27(3) 2_665 ? C26S C21S 1.34(2) 2_665 ? C27S C24S 0.36(6) 2_665 ? C27S C25S 1.36(5) 2_665 ? C27S C23S 1.70(5) 2_665 ? C28S C29S 1.39 . ? C28S C33S 1.39 . ? C29S C30S 1.39 . ? C30S C31S 1.39 . ? C31S C32S 1.39 . ? C31S C34S 1.74(3) . ? C32S C33S 1.39 . ? C32S C34S 1.79(6) . ? C28' C29' 1.39 . ? C28' C33' 1.39 . ? C29' C30' 1.39 . ? C30' C31' 1.39 . ? C30' C34' 1.61(3) . ? C31' C32' 1.39 . ? C32' C33' 1.39 . ? 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 Co1 Co2 Co3 178.05(5) . . y Co2 Co1 Br1 179.89(4) . . y Co2 Co3 Br2 179.63(4) . . y N4 Co1 N1 90.0(2) . . y N1 Co1 N7 90.0(2) . . y N10 Co1 N1 170.6(2) . . y N4 Co1 N7 169.8(2) . . y N4 Co1 N10 88.5(2) . . y N10 Co1 N7 89.9(2) . . y N2 Co2 N5 89.3(2) . . y N2 Co2 N8 90.7(2) . . y N2 Co2 N11 179.3(2) . . y N5 Co2 N8 178.6(2) . . y N5 Co2 N11 90.1(2) . . y N11 Co2 N8 89.9(2) . . y N3 Co3 N6 88.3(2) . . y N9 Co3 N3 92.2(2) . . y N3 Co3 N12 162.2(2) . . y N9 Co3 N6 162.4(2) . . y N12 Co3 N6 83.8(2) . . y N9 Co3 N12 90.6(2) . . y N1 Co1 Br1 94.2(2) . . y N4 Co1 Br1 95.6(2) . . y N7 Co1 Br1 94.6(2) . . y N10 Co1 Br1 95.1(2) . . y N3 Co3 Br2 97.9(2) . . y N6 Co3 Br2 99.74(14) . . y N9 Co3 Br2 97.6(2) . . y N12 Co3 Br2 99.2(2) . . y N4 Co1 Co2 84.5(2) . . ? N10 Co1 Co2 85.0(2) . . ? N1 Co1 Co2 85.7(2) . . ? N7 Co1 Co2 85.4(2) . . ? N2 Co2 Co1 89.5(2) . . ? N5 Co2 Co1 89.6(2) . . ? N11 Co2 Co1 90.3(2) . . ? N8 Co2 Co1 89.0(2) . . ? N2 Co2 Co3 90.9(2) . . ? N5 Co2 Co3 92.3(2) . . ? N11 Co2 Co3 89.4(2) . . ? N8 Co2 Co3 89.0(2) . . ? N9 Co3 Co2 82.0(2) . . ? N3 Co3 Co2 82.3(2) . . ? N12 Co3 Co2 80.70(15) . . ? N6 Co3 Co2 80.60(14) . . ? C5 N1 C1 117.1(6) . . ? C5 N1 Co1 119.8(4) . . ? C1 N1 Co1 123.0(5) . . ? C5 N2 C6 123.1(5) . . ? C5 N2 Co2 117.3(4) . . ? C6 N2 Co2 119.6(4) . . ? C10 N3 C6 116.5(6) . . ? C10 N3 Co3 121.8(5) . . ? C6 N3 Co3 121.7(4) . . ? C11 N4 C15 117.0(6) . . ? C11 N4 Co1 120.9(5) . . ? C15 N4 Co1 122.1(4) . . ? C16 N5 C15 123.3(5) . . ? C16 N5 Co2 119.3(4) . . ? C15 N5 Co2 117.0(4) . . ? C20 N6 C16 118.0(5) . . ? C20 N6 Co3 118.7(4) . . ? C16 N6 Co3 123.3(4) . . ? C21 N7 C25 118.3(7) . . ? C21 N7 Co1 121.3(6) . . ? C25 N7 Co1 120.3(5) . . ? C25 N8 C26 122.6(6) . . ? C25 N8 Co2 118.0(5) . . ? C26 N8 Co2 119.4(4) . . ? C26 N9 C30 119.0(6) . . ? C26 N9 Co3 121.6(4) . . ? C30 N9 Co3 119.1(5) . . ? C35 N10 C31 118.4(6) . . ? C35 N10 Co1 120.0(4) . . ? C31 N10 Co1 121.6(5) . . ? C36 N11 C35 124.8(6) . . ? C36 N11 Co2 117.9(4) . . ? C35 N11 Co2 116.8(5) . . ? C40 N12 C36 119.2(6) . . ? C40 N12 Co3 118.2(4) . . ? C36 N12 Co3 122.1(4) . . ? N1 C1 C2 124.8(7) . . ? C1 C2 C3 117.7(7) . . ? C4 C3 C2 119.9(7) . . ? C3 C4 C5 120.3(7) . . ? N1 C5 N2 115.8(6) . . ? N1 C5 C4 120.1(6) . . ? N2 C5 C4 124.0(6) . . ? N3 C6 N2 116.0(6) . . ? N3 C6 C7 120.2(6) . . ? N2 C6 C7 123.8(6) . . ? C8 C7 C6 119.5(7) . . ? C9 C8 C7 120.7(7) . . ? C8 C9 C10 118.1(7) . . ? C9 C10 N3 124.9(7) . . ? N4 C11 C12 124.5(7) . . ? C11 C12 C13 118.3(7) . . ? C14 C13 C12 118.7(7) . . ? C13 C14 C15 120.7(7) . . ? N4 C15 N5 113.5(6) . . ? N4 C15 C14 120.7(6) . . ? N5 C15 C14 125.4(6) . . ? N6 C16 N5 116.3(5) . . ? N6 C16 C17 119.7(6) . . ? N5 C16 C17 123.9(6) . . ? C18 C17 C16 119.9(6) . . ? C17 C18 C19 120.6(6) . . ? C20 C19 C18 117.8(6) . . ? N6 C20 C19 124.0(6) . . ? N7 C21 C22 124.1(8) . . ? C23 C22 C21 117.1(8) . . ? C24 C23 C22 120.5(8) . . ? C23 C24 C25 119.2(8) . . ? N7 C25 N8 115.0(6) . . ? N7 C25 C24 120.6(7) . . ? N8 C25 C24 124.2(7) . . ? N9 C26 N8 115.7(6) . . ? N9 C26 C27 119.8(6) . . ? N8 C26 C27 124.4(6) . . ? C28 C27 C26 120.6(7) . . ? C27 C28 C29 119.6(7) . . ? C30 C29 C28 118.3(8) . . ? N9 C30 C29 122.8(7) . . ? N10 C31 C32 124.0(8) . . ? C31 C32 C33 117.4(8) . . ? C32 C33 C34 121.2(8) . . ? C33 C34 C35 118.5(8) . . ? N10 C35 N11 116.6(6) . . ? N10 C35 C34 120.3(6) . . ? N11 C35 C34 122.9(7) . . ? N12 C36 N11 115.2(5) . . ? N12 C36 C37 120.1(6) . . ? N11 C36 C37 124.4(6) . . ? C38 C37 C36 120.1(7) . . ? C39 C38 C37 119.3(7) . . ? C38 C39 C40 118.7(7) . . ? N12 C40 C39 122.6(7) . . ? Co4 Co5 Co6 177.93(5) . . y Co5 Co4 Br3 178.28(4) . . y Co5 Co6 Br4 178.40(5) . . y N16 Co4 N13 89.1(2) . . y N19 Co4 N13 168.6(2) . . y N22 Co4 N13 91.1(2) . . y N16 Co4 N19 89.9(2) . . y N16 Co4 N22 169.6(2) . . y N22 Co4 N19 88.0(2) . . y N14 Co5 N17 90.3(2) . . y N14 Co5 N20 179.3(2) . . y N14 Co5 N23 89.2(2) . . y N20 Co5 N17 90.4(2) . . y N17 Co5 N23 178.0(2) . . y N20 Co5 N23 90.1(2) . . y N15 Co6 N18 88.5(2) . . y N15 Co6 N21 163.6(2) . . y N15 Co6 N24 91.2(2) . . y N18 Co6 N21 87.5(2) . . y N18 Co6 N24 162.7(2) . . y N21 Co6 N24 88.0(2) . . y N13 Co4 Br3 94.97(15) . . y N16 Co4 Br3 96.11(15) . . y N19 Co4 Br3 96.4(2) . . y N22 Co4 Br3 94.2(2) . . y N15 Co6 Br4 97.02(14) . . y N18 Co6 Br4 98.15(14) . . y N21 Co6 Br4 99.3(2) . . y N24 Co6 Br4 99.1(2) . . y N16 Co4 Co5 85.52(15) . . ? N22 Co4 Co5 84.1(2) . . ? N19 Co4 Co5 84.2(2) . . ? N13 Co4 Co5 84.49(15) . . ? N14 Co5 Co4 89.83(15) . . ? N20 Co5 Co4 90.3(2) . . ? N17 Co5 Co4 88.53(15) . . ? N23 Co5 Co4 89.5(2) . . ? N14 Co5 Co6 89.76(15) . . ? N20 Co5 Co6 90.1(2) . . ? N17 Co5 Co6 89.44(15) . . ? N23 Co5 Co6 92.5(2) . . ? N15 Co6 Co5 81.56(14) . . ? N18 Co6 Co5 82.58(14) . . ? N21 Co6 Co5 82.1(2) . . ? N24 Co6 Co5 80.2(2) . . ? C45 N13 C41 118.4(5) . . ? C45 N13 Co4 120.0(4) . . ? C41 N13 Co4 121.6(5) . . ? C46 N14 C45 122.8(5) . . ? C46 N14 Co5 119.6(4) . . ? C45 N14 Co5 117.5(4) . . ? C50 N15 C46 117.6(6) . . ? C50 N15 Co6 120.9(5) . . ? C46 N15 Co6 121.5(4) . . ? C51 N16 C55 119.4(5) . . ? C51 N16 Co4 121.4(4) . . ? C55 N16 Co4 119.1(4) . . ? C55 N17 C56 124.1(5) . . ? C55 N17 Co5 117.5(4) . . ? C56 N17 Co5 118.3(4) . . ? C60 N18 C56 118.0(6) . . ? C60 N18 Co6 120.9(5) . . ? C56 N18 Co6 121.0(4) . . ? C61 N19 C65 117.2(6) . . ? C61 N19 Co4 121.9(5) . . ? C65 N19 Co4 120.8(4) . . ? C66 N20 C65 122.6(5) . . ? C66 N20 Co5 120.9(4) . . ? C65 N20 Co5 116.2(4) . . ? C70 N21 C66 117.4(6) . . ? C70 N21 Co6 120.8(5) . . ? C66 N21 Co6 121.7(4) . . ? C71 N22 C75 118.7(5) . . ? C71 N22 Co4 121.3(4) . . ? C75 N22 Co4 120.0(4) . . ? C76 N23 C75 125.0(5) . . ? C76 N23 Co5 118.7(4) . . ? C75 N23 Co5 116.3(4) . . ? C80 N24 C76 118.8(6) . . ? C80 N24 Co6 118.2(5) . . ? C76 N24 Co6 123.0(4) . . ? N13 C41 C42 122.9(7) . . ? C43 C42 C41 118.6(6) . . ? C44 C43 C42 120.3(7) . . ? C43 C44 C45 119.3(7) . . ? N13 C45 N14 115.5(6) . . ? N13 C45 C44 120.5(5) . . ? N14 C45 C44 123.6(6) . . ? N14 C46 N15 114.6(5) . . ? N14 C46 C47 125.2(6) . . ? N15 C46 C47 119.9(6) . . ? C48 C47 C46 120.9(6) . . ? C47 C48 C49 118.2(7) . . ? C50 C49 C48 117.9(7) . . ? N15 C50 C49 125.3(7) . . ? N16 C51 C52 123.2(6) . . ? C51 C52 C53 118.2(6) . . ? C54 C53 C52 120.0(6) . . ? C53 C54 C55 120.3(6) . . ? N17 C55 N16 116.0(5) . . ? N17 C55 C54 124.9(6) . . ? N16 C55 C54 118.9(5) . . ? N18 C56 N17 116.1(5) . . ? N18 C56 C57 121.0(6) . . ? N17 C56 C57 122.6(6) . . ? C58 C57 C56 119.6(7) . . ? C57 C58 C59 118.7(7) . . ? C60 C59 C58 119.1(6) . . ? N18 C60 C59 123.5(7) . . ? N19 C61 C62 124.2(7) . . ? C63 C62 C61 118.1(7) . . ? C62 C63 C64 120.9(7) . . ? C63 C64 C65 119.7(7) . . ? N20 C65 N19 114.8(6) . . ? N20 C65 C64 125.0(6) . . ? N19 C65 C64 119.9(6) . . ? N20 C66 N21 114.7(6) . . ? N20 C66 C67 124.7(7) . . ? N21 C66 C67 120.3(6) . . ? C68 C67 C66 119.7(8) . . ? C67 C68 C69 120.9(8) . . ? C68 C69 C70 118.4(8) . . ? N21 C70 C69 123.1(8) . . ? N22 C71 C72 124.1(7) . . ? C71 C72 C73 117.4(7) . . ? C74 C73 C72 120.6(7) . . ? C73 C74 C75 120.1(7) . . ? N22 C75 N23 115.6(5) . . ? N22 C75 C74 118.8(6) . . ? N23 C75 C74 125.3(6) . . ? N23 C76 N24 115.8(5) . . ? N23 C76 C77 122.9(6) . . ? N24 C76 C77 120.9(6) . . ? C78 C77 C76 119.9(7) . . ? C77 C78 C79 119.3(7) . . ? C78 C79 C80 117.8(7) . . ? N24 C80 C79 123.1(7) . . ? C7S C1S C2S 116.7(11) . . ? C7S C1S C6S 123.3(11) . . ? C2S C1S C6S 120.0 . . ? C1S C2S C3S 120.0 . . ? C2S C3S C4S 120.0 . . ? C5S C4S C3S 120.0 . . ? C4S C5S C6S 120.0 . . ? C5S C6S C1S 120.0 . . ? C7' C1' C2' 125.6(23) . . ? C7' C1' C6' 114.0(23) . . ? C2' C1' C6' 120.0 . . ? C3' C2' C1' 120.0 . . ? C4' C3' C2' 120.0 . . ? C5' C4' C3' 120.0 . . ? C6' C5' C4' 120.0 . . ? C5' C6' C1' 120.0 . . ? C9S C8S C13S 120.0 . . ? C10S C9S C8S 120.0 . . ? C9S C10S C11S 120.0 . . ? C10S C11S C12S 120.0 . . ? C10S C11S C14S 95.2(18) . . ? C12S C11S C14S 144.7(18) . . ? C13S C12S C11S 120.0 . . ? C12S C13S C8S 120.0 . . ? C14' C8' C9' 125.7(11) . . ? C14' C8' C13' 114.1(11) . . ? C9' C8' C13' 120.0 . . ? C8' C9' C10' 120.0 . . ? C11' C10' C9' 120.0 . . ? C10' C11' C12' 120.0 . . ? C11' C12' C13' 120.0 . . ? C12' C13' C8' 120.0 . . ? C15S C16S C17S 133.7(58) . . ? C18S C17S C16S 132.7(40) . . ? C17S C18S C19S 132.6(37) . . ? C20S C19S C18S 158.4(38) . . ? C25S C21S C24S 68.9(13) 2_665 2_665 ? C25S C21S C26S 66.5(16) 2_665 2_665 ? C24S C21S C26S 134.9(26) 2_665 2_665 ? C25S C21S C22S 58.3(20) 2_665 . ? C24S C21S C22S 127.2(24) 2_665 . ? C26S C21S C22S 9.8(12) 2_665 . ? C25S C21S C26S 174.4(25) 2_665 . ? C24S C21S C26S 112.6(24) 2_665 . ? C26S C21S C26S 111.3(11) 2_665 . ? C22S C21S C26S 120.0 . . ? C25S C21S C27S 60.4(18) 2_665 . ? C24S C21S C27S 12.5(23) 2_665 . ? C26S C21S C27S 126.7(15) 2_665 . ? C22S C21S C27S 118.0(11) . . ? C26S C21S C27S 121.9(11) . . ? C25S C21S C23S 128.8(18) 2_665 2_665 ? C24S C21S C23S 60.2(12) 2_665 2_665 ? C26S C21S C23S 161.4(25) 2_665 2_665 ? C22S C21S C23S 171.2(18) . 2_665 ? C26S C21S C23S 52.4(17) . 2_665 ? C27S C21S C23S 70.1(16) . 2_665 ? C25S C21S C21S 123.5(26) 2_665 2_665 ? C24S C21S C21S 163.9(35) 2_665 2_665 ? C26S C21S C21S 57.3(12) 2_665 2_665 ? C22S C21S C21S 66.1(9) . 2_665 ? C26S C21S C21S 54.1(9) . 2_665 ? C27S C21S C21S 175.9(17) . 2_665 ? C23S C21S C21S 105.8(23) 2_665 2_665 ? C25S C21S C22S 170.2(35) 2_665 2_665 ? C24S C21S C22S 113.5(22) 2_665 2_665 ? C26S C21S C22S 109.6(15) 2_665 2_665 ? C22S C21S C22S 118.6(10) . 2_665 ? C26S C21S C22S 4.2(13) . 2_665 ? C27S C21S C22S 123.5(13) . 2_665 ? C23S C21S C22S 53.5(11) 2_665 2_665 ? C21S C21S C22S 52.5(12) 2_665 2_665 ? C26S C22S C25S 116.2(89) 2_665 2_665 ? C26S C22S C23S 54.9(74) 2_665 . ? C25S C22S C23S 171.1(20) 2_665 . ? C26S C22S C21S 72.6(72) 2_665 . ? C25S C22S C21S 52.8(18) 2_665 . ? C23S C22S C21S 120.0 . . ? C26S C22S C21S 25.0(63) 2_665 2_665 ? C25S C22S C21S 113.5(22) 2_665 2_665 ? C23S C22S C21S 58.7(8) . 2_665 ? C21S C22S C21S 61.4(8) . 2_665 ? C26S C23S C22S 8.9(12) 2_665 . ? C26S C23S C24S 112.6(11) 2_665 . ? C22S C23S C24S 120.0 . . ? C26S C23S C21S 60.2(9) 2_665 2_665 ? C22S C23S C21S 67.8(9) . 2_665 ? C24S C23S C21S 52.4(9) . 2_665 ? C26S C23S C27S 114.5(18) 2_665 2_665 ? C22S C23S C27S 122.5(14) . 2_665 ? C24S C23S C27S 7.2(18) . 2_665 ? C21S C23S C27S 54.8(13) 2_665 2_665 ? C27S C24S C21S 118.1(74) 2_665 2_665 ? C27S C24S C25S 77.9(57) 2_665 . ? C21S C24S C25S 52.8(11) 2_665 . ? C27S C24S C23S 143.9(72) 2_665 . ? C21S C24S C23S 67.4(11) 2_665 . ? C25S C24S C23S 120.0 . . ? C21S C25S C22S 68.9(13) 2_665 2_665 ? C21S C25S C27S 70.2(19) 2_665 2_665 ? C22S C25S C27S 137.9(26) 2_665 2_665 ? C21S C25S C24S 58.3(10) 2_665 . ? C22S C25S C24S 127.2(12) 2_665 . ? C27S C25S C24S 15.0(20) 2_665 . ? C21S C25S C26S 62.0(11) 2_665 . ? C22S C25S C26S 8.9(14) 2_665 . ? C27S C25S C26S 132.0(19) 2_665 . ? C24S C25S C26S 120.0 . . ? C22S C26S C23S 116.2(71) 2_665 2_665 ? C22S C26S C21S 97.6(65) 2_665 2_665 ? C23S C26S C21S 134.9(28) 2_665 2_665 ? C22S C26S C25S 54.9(69) 2_665 . ? C23S C26S C25S 171.2(22) 2_665 . ? C21S C26S C25S 51.6(10) 2_665 . ? C22S C26S C21S 150.8(81) 2_665 . ? C23S C26S C21S 67.4(20) 2_665 . ? C21S C26S C21S 68.7(10) 2_665 . ? C25S C26S C21S 120.0 . . ? C24S C27S C25S 87.0(74) 2_665 2_665 ? C24S C27S C21S 49.4(69) 2_665 . ? C25S C27S C21S 49.4(19) 2_665 . ? C24S C27S C23S 28.9(61) 2_665 2_665 ? C25S C27S C23S 103.4(30) 2_665 2_665 ? C21S C27S C23S 55.1(15) . 2_665 ? C29S C28S C33S 120.0 . . ? C30S C29S C28S 120.0 . . ? C29S C30S C31S 120.0 . . ? C32S C31S C30S 120.0 . . ? C32S C31S C34S 68.8(25) . . ? C30S C31S C34S 163.4(26) . . ? C31S C32S C33S 120.0 . . ? C31S C32S C34S 64.8(18) . . ? C33S C32S C34S 165.4(24) . . ? C32S C33S C28S 120.0 . . ? C31S C34S C32S 46.4(10) . . ? C29' C28' C33' 120.0 . . ? C28' C29' C30' 120.0 . . ? C31' C30' C29' 120.0 . . ? C31' C30' C34' 96.9(41) . . ? C29' C30' C34' 143.1(41) . . ? C32' C31' C30' 120.0 . . ? C31' C32' C33' 120.0 . . ? C32' C33' C28' 120.0 . . ? _refine_diff_density_max 0.773 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.086 #===END