# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hundal, Maninder' _publ_contact_author_email 'Hundal chem@yahoo.com' loop_ _publ_author_name M.Hundal G.Hundal A.P.Pannu P.Kapoor R.Kapoor C.Montserrat N.Aliaga-Alcalde data_shelxl _database_code_depnum_ccdc_archive 'CCDC 808174' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H22 Cl2 Co N2 O' _chemical_formula_sum 'C14 H22 Cl2 Co N2 O' _chemical_formula_weight 364.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3915(4) _cell_length_b 7.3850(3) _cell_length_c 13.1072(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.658(2) _cell_angle_gamma 90.00 _cell_volume 856.08(6) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 53 _cell_measurement_theta_min 12 _cell_measurement_theta_max 20 _exptl_crystal_description needles _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.413 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 378 _exptl_absorpt_coefficient_mu 10.701 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.220 _exptl_absorpt_correction_T_max 0.238 _exptl_absorpt_process_details 'R. H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius kappa CCD2000' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3327 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0601 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 64.76 _reflns_number_total 1771 _reflns_number_gt 1751 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CAD4 Express Software (Enraf-Nonius)' _computing_cell_refinement 'CAD4 Express Software (Enraf-Nonius)' _computing_data_reduction 'CAD4 Express Software (Enraf-Nonius)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ' ORTEP3 for Windows (Farrugia,1997)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.1513P] 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 none _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 0.015(7) _refine_ls_number_reflns 1771 _refine_ls_number_parameters 181 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0396 _refine_ls_wR_factor_ref 0.0986 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.262 _refine_ls_restrained_S_all 1.261 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3374(6) -0.2357(8) 0.2380(4) 0.0135(12) Uani 1 1 d . . . C2 C 0.3747(6) -0.1336(10) 0.3316(4) 0.0179(12) Uani 1 1 d . . . H2 H 0.3514 -0.1759 0.3910 0.021 Uiso 1 1 calc R . . C3 C 0.4460(7) 0.0300(8) 0.3373(4) 0.0169(13) Uani 1 1 d . . . H3 H 0.4699 0.0972 0.4009 0.020 Uiso 1 1 calc R . . C4 C 0.4491(6) -0.0045(9) 0.1624(4) 0.0157(13) Uani 1 1 d . . . H4 H 0.4737 0.0399 0.1040 0.019 Uiso 1 1 calc R . . C5 C 0.3796(6) -0.1719(8) 0.1527(4) 0.0158(13) Uani 1 1 d . . . H5 H 0.3614 -0.2404 0.0901 0.019 Uiso 1 1 calc R . . C6 C 0.2576(6) -0.4142(8) 0.2318(4) 0.0131(12) Uani 1 1 d . . . C7 C 0.0224(7) -0.2610(8) 0.2265(4) 0.0184(12) Uani 1 1 d . . . H7A H 0.0843 -0.1526 0.2440 0.022 Uiso 1 1 calc R . . H7B H -0.0319 -0.2699 0.2775 0.022 Uiso 1 1 calc R . . C8 C -0.0917(7) -0.2425(9) 0.1121(5) 0.0232(14) Uani 1 1 d . . . H8 H -0.1457 -0.3577 0.0920 0.028 Uiso 1 1 calc R . . C9 C -0.0153(7) -0.2005(9) 0.0303(4) 0.0268(14) Uani 1 1 d . . . H9A H 0.0549 -0.2953 0.0309 0.040 Uiso 1 1 calc R . . H9B H 0.0379 -0.0876 0.0485 0.040 Uiso 1 1 calc R . . H9C H -0.0900 -0.1918 -0.0406 0.040 Uiso 1 1 calc R . . C10 C -0.2067(7) -0.0953(11) 0.1123(5) 0.0369(18) Uani 1 1 d . . . H10A H -0.2800 -0.0842 0.0410 0.055 Uiso 1 1 calc R . . H10B H -0.1553 0.0181 0.1335 0.055 Uiso 1 1 calc R . . H10C H -0.2568 -0.1276 0.1626 0.055 Uiso 1 1 calc R . . C11 C 0.0557(6) -0.5951(8) 0.2559(4) 0.0169(13) Uani 1 1 d . . . H11A H 0.1164 -0.6927 0.2428 0.020 Uiso 1 1 calc R . . H11B H -0.0455 -0.6062 0.2036 0.020 Uiso 1 1 calc R . . C12 C 0.0482(6) -0.6146(10) 0.3708(4) 0.0210(12) Uani 1 1 d . . . H12 H -0.0236 -0.5251 0.3799 0.025 Uiso 1 1 calc R . . C13 C -0.0113(8) -0.8026(10) 0.3811(5) 0.0305(16) Uani 1 1 d . . . H13A H -0.0176 -0.8172 0.4523 0.046 Uiso 1 1 calc R . . H13B H 0.0561 -0.8920 0.3697 0.046 Uiso 1 1 calc R . . H13C H -0.1099 -0.8175 0.3279 0.046 Uiso 1 1 calc R . . C14 C 0.2013(7) -0.5808(9) 0.4569(4) 0.0250(15) Uani 1 1 d . . . H14A H 0.1923 -0.5921 0.5274 0.038 Uiso 1 1 calc R . . H14B H 0.2353 -0.4610 0.4483 0.038 Uiso 1 1 calc R . . H14C H 0.2729 -0.6679 0.4492 0.038 Uiso 1 1 calc R . . N1 N 0.4827(5) 0.0968(7) 0.2530(3) 0.0145(10) Uani 1 1 d . . . N2 N 0.1212(5) -0.4196(6) 0.2393(3) 0.0119(10) Uani 1 1 d . . . O1 O 0.3253(4) -0.5578(6) 0.2222(3) 0.0166(8) Uani 1 1 d . . . Cl1 Cl 0.66746(16) -0.5394(2) 0.41870(10) 0.0257(4) Uani 1 1 d . . . Cl2 Cl 0.62530(15) -0.59178(18) 0.11646(9) 0.0200(4) Uani 1 1 d . . . Co1 Co 0.53862(9) -0.63467(12) 0.25286(6) 0.0119(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.008(3) 0.017(3) 0.018(3) 0.004(2) 0.008(2) 0.000(2) C2 0.019(3) 0.021(3) 0.017(2) 0.006(3) 0.010(2) 0.002(3) C3 0.014(3) 0.021(3) 0.014(2) -0.001(2) 0.002(2) 0.002(2) C4 0.010(3) 0.024(4) 0.018(3) 0.001(2) 0.011(2) -0.002(2) C5 0.016(3) 0.014(3) 0.019(3) -0.002(2) 0.009(2) 0.001(2) C6 0.013(3) 0.014(3) 0.012(2) 0.002(2) 0.004(2) 0.000(2) C7 0.018(3) 0.015(3) 0.024(3) 0.004(2) 0.009(2) 0.000(2) C8 0.015(3) 0.022(4) 0.032(3) 0.010(3) 0.007(3) -0.001(3) C9 0.029(4) 0.027(4) 0.021(3) 0.003(3) 0.005(2) 0.007(3) C10 0.024(4) 0.042(5) 0.042(3) 0.011(4) 0.007(3) 0.015(3) C11 0.014(3) 0.016(4) 0.023(2) 0.000(2) 0.009(2) 0.003(2) C12 0.024(3) 0.025(3) 0.020(2) 0.008(3) 0.015(2) 0.002(3) C13 0.032(4) 0.030(4) 0.037(3) 0.012(3) 0.022(3) 0.001(3) C14 0.033(4) 0.021(4) 0.022(2) 0.005(3) 0.010(2) 0.003(3) N1 0.009(2) 0.015(3) 0.018(2) 0.0036(19) 0.0026(19) 0.0011(19) N2 0.012(3) 0.012(3) 0.014(2) 0.0004(18) 0.0076(18) -0.0019(19) O1 0.010(2) 0.015(2) 0.0261(18) -0.0015(16) 0.0076(15) 0.0016(16) Cl1 0.0254(8) 0.0344(9) 0.0169(6) -0.0052(6) 0.0064(5) -0.0074(7) Cl2 0.0191(7) 0.0249(9) 0.0204(6) 0.0025(5) 0.0125(5) -0.0036(5) Co1 0.0099(4) 0.0110(5) 0.0161(4) -0.0009(4) 0.0060(3) -0.0023(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 C1 C2 1.382(8) . ? C1 C5 1.388(7) . ? C1 C6 1.505(8) . ? C2 C3 1.371(9) . ? C2 H2 0.9300 . ? C3 N1 1.356(7) . ? C3 H3 0.9300 . ? C4 N1 1.348(7) . ? C4 C5 1.383(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 O1 1.264(7) . ? C6 N2 1.318(7) . ? C7 N2 1.469(7) . ? C7 C8 1.528(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.510(8) . ? C8 C10 1.533(9) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.482(7) . ? C11 C12 1.538(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C14 1.520(8) . ? C12 C13 1.520(10) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? N1 Co1 2.052(5) 1_565 ? O1 Co1 1.989(4) . ? Cl1 Co1 2.2169(15) . ? Cl2 Co1 2.2222(13) . ? Co1 N1 2.052(5) 1_545 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 118.3(5) . . ? C2 C1 C6 119.9(5) . . ? C5 C1 C6 121.8(5) . . ? C3 C2 C1 120.2(5) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? N1 C3 C2 122.0(5) . . ? N1 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? N1 C4 C5 122.7(5) . . ? N1 C4 H4 118.7 . . ? C5 C4 H4 118.7 . . ? C4 C5 C1 118.9(5) . . ? C4 C5 H5 120.5 . . ? C1 C5 H5 120.5 . . ? O1 C6 N2 121.1(5) . . ? O1 C6 C1 118.8(5) . . ? N2 C6 C1 120.1(5) . . ? N2 C7 C8 113.0(5) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C9 C8 C7 111.8(5) . . ? C9 C8 C10 111.1(5) . . ? C7 C8 C10 108.8(5) . . ? C9 C8 H8 108.3 . . ? C7 C8 H8 108.3 . . ? C10 C8 H8 108.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 112.6(5) . . ? N2 C11 H11A 109.1 . . ? C12 C11 H11A 109.1 . . ? N2 C11 H11B 109.1 . . ? C12 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C14 C12 C13 111.6(5) . . ? C14 C12 C11 111.6(4) . . ? C13 C12 C11 108.2(5) . . ? C14 C12 H12 108.5 . . ? C13 C12 H12 108.5 . . ? C11 C12 H12 108.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C4 N1 C3 117.9(5) . . ? C4 N1 Co1 121.3(4) . 1_565 ? C3 N1 Co1 119.2(4) . 1_565 ? C6 N2 C7 124.1(5) . . ? C6 N2 C11 119.9(5) . . ? C7 N2 C11 115.9(4) . . ? C6 O1 Co1 136.5(4) . . ? O1 Co1 N1 92.02(18) . 1_545 ? O1 Co1 Cl1 106.75(11) . . ? N1 Co1 Cl1 111.19(13) 1_545 . ? O1 Co1 Cl2 114.41(11) . . ? N1 Co1 Cl2 107.56(13) 1_545 . ? Cl1 Co1 Cl2 121.11(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 2.6(8) . . . . ? C6 C1 C2 C3 -179.3(5) . . . . ? C1 C2 C3 N1 -0.2(8) . . . . ? N1 C4 C5 C1 2.4(8) . . . . ? C2 C1 C5 C4 -3.7(8) . . . . ? C6 C1 C5 C4 178.3(5) . . . . ? C2 C1 C6 O1 -115.0(6) . . . . ? C5 C1 C6 O1 63.0(7) . . . . ? C2 C1 C6 N2 63.3(7) . . . . ? C5 C1 C6 N2 -118.7(6) . . . . ? N2 C7 C8 C9 -67.0(7) . . . . ? N2 C7 C8 C10 169.9(5) . . . . ? N2 C11 C12 C14 -53.4(7) . . . . ? N2 C11 C12 C13 -176.6(5) . . . . ? C5 C4 N1 C3 0.0(8) . . . . ? C5 C4 N1 Co1 -165.4(4) . . . 1_565 ? C2 C3 N1 C4 -1.1(8) . . . . ? C2 C3 N1 Co1 164.6(4) . . . 1_565 ? O1 C6 N2 C7 -165.8(5) . . . . ? C1 C6 N2 C7 15.9(7) . . . . ? O1 C6 N2 C11 10.8(7) . . . . ? C1 C6 N2 C11 -167.5(4) . . . . ? C8 C7 N2 C6 96.3(6) . . . . ? C8 C7 N2 C11 -80.5(6) . . . . ? C12 C11 N2 C6 108.2(5) . . . . ? C12 C11 N2 C7 -74.9(6) . . . . ? N2 C6 O1 Co1 -156.4(4) . . . . ? C1 C6 O1 Co1 21.9(7) . . . . ? C6 O1 Co1 N1 160.2(5) . . . 1_545 ? C6 O1 Co1 Cl1 47.3(5) . . . . ? C6 O1 Co1 Cl2 -89.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 64.76 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 0.461 _refine_diff_density_min -0.464 _refine_diff_density_rms 0.088 # Attachment '- 2 .cif' data_shelxl2 _database_code_depnum_ccdc_archive 'CCDC 808175' #TrackingRef '- 2 .cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H52 Co N4 O6, 2(C14 H22 Br3 Co N2 O), 2(H2 O)' _chemical_formula_sum 'C56 H100 Br6 Co3 N8 O10' _chemical_formula_weight 1701.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2900 2.4600 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3490 0.9720 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8031(3) _cell_length_b 11.8076(5) _cell_length_c 15.7629(7) _cell_angle_alpha 92.503(4) _cell_angle_beta 91.003(3) _cell_angle_gamma 91.025(3) _cell_volume 1822.23(12) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10157 _cell_measurement_theta_min 5.0751 _cell_measurement_theta_max 32.7024 _exptl_crystal_description plates _exptl_crystal_colour blue _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 863 _exptl_absorpt_coefficient_mu 4.018 _exptl_absorpt_correction_T_min 0.402 _exptl_absorpt_correction_T_max 0.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Ruby, Gemini' _diffrn_detector_area_resol_mean 10.5081 _diffrn_reflns_av_R_equivalents 0.0420 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23039 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 5.09 _diffrn_reflns_theta_max 32.78 _reflns_number_total 12016 _reflns_number_gt 7521 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The cif shows A level error due to the missing hydrogens of the lattice water molecules. Their are other A level errors due to residual electron density peaks of 4.6 eA-3 and lesser, all very close to the heavy atoms (Co and Br). All our attempts to treat them as disordered atoms failed. These are due to the poor crystal quality, which were probably twinned. A number of crystals were tried before collecting data on this one. The presence of non-merohedral twinning is indicated (P. Muller et al., " Crystal structure refinement, A crystallographer's guide to SHELXL" IUCr, Oxford Univ. Press, 2006) clearly by (i) the strange residual intensity near the heavy metal ions which is not due to disorder or solvent (ii) Fobs being greater than Fcalc. for almost all those reflections showing disagreement between the two (iii) high R values although data seem to be good. A B level error occurs due to a relatively large ratio Ueq(max.)/Ueq(min.) for some of the terminal C atoms of the isobutyl group. These terminal isobutyl groups usually have large thermal parameters due to disorder although none was evident in the present data set. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12016 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1531 _refine_ls_R_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.3707 _refine_ls_wR_factor_gt 0.3458 _refine_ls_goodness_of_fit_ref 1.332 _refine_ls_restrained_S_all 1.332 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3258(6) 0.0264(6) 0.9640(4) 0.0137(13) Uani 1 1 d . . . H1 H 0.3709 -0.0284 0.9939 0.016 Uiso 1 1 calc R . . C2 C 0.3749(6) 0.0553(6) 0.8848(4) 0.0123(12) Uani 1 1 d . . . H2 H 0.4496 0.0192 0.8612 0.015 Uiso 1 1 calc R . . C3 C 0.3076(6) 0.1405(5) 0.8424(4) 0.0086(11) Uani 1 1 d . . . C4 C 0.1901(6) 0.1873(5) 0.8771(4) 0.0093(11) Uani 1 1 d . . . H4 H 0.1412 0.2415 0.8489 0.011 Uiso 1 1 calc R . . C5 C 0.1494(6) 0.1505(5) 0.9540(4) 0.0087(11) Uani 1 1 d . . . H5 H 0.0700 0.1803 0.9766 0.010 Uiso 1 1 calc R . . C6 C 0.3718(6) 0.1865(6) 0.7644(4) 0.0100(11) Uani 1 1 d . . . C7 C 0.4329(6) 0.1712(6) 0.6172(4) 0.0135(12) Uani 1 1 d . . . H7A H 0.4209 0.2525 0.6157 0.016 Uiso 1 1 calc R . . H7B H 0.3954 0.1368 0.5646 0.016 Uiso 1 1 calc R . . C8 C 0.5856(7) 0.1465(6) 0.6232(5) 0.0173(14) Uani 1 1 d . . . H8 H 0.6243 0.1852 0.6746 0.021 Uiso 1 1 calc R . . C9 C 0.6152(9) 0.0203(8) 0.6255(6) 0.0299(18) Uani 1 1 d . . . H9A H 0.7120 0.0100 0.6294 0.045 Uiso 1 1 calc R . . H9B H 0.5797 -0.0179 0.5746 0.045 Uiso 1 1 calc R . . H9C H 0.5726 -0.0106 0.6740 0.045 Uiso 1 1 calc R . . C10 C 0.6500(9) 0.1987(9) 0.5444(6) 0.032(2) Uani 1 1 d . . . H10A H 0.7465 0.1862 0.5451 0.047 Uiso 1 1 calc R . . H10B H 0.6337 0.2786 0.5456 0.047 Uiso 1 1 calc R . . H10C H 0.6097 0.1635 0.4937 0.047 Uiso 1 1 calc R . . C11 C 0.2602(7) 0.0345(6) 0.6740(4) 0.0143(12) Uani 1 1 d . . . H11A H 0.2282 0.0104 0.7284 0.017 Uiso 1 1 calc R . . H11B H 0.3065 -0.0290 0.6469 0.017 Uiso 1 1 calc R . . C12 C 0.1378(7) 0.0630(7) 0.6194(5) 0.0182(14) Uani 1 1 d . . . H12 H 0.1701 0.0841 0.5637 0.022 Uiso 1 1 calc R . . C13 C 0.0576(9) 0.1634(8) 0.6592(6) 0.032(2) Uani 1 1 d . . . H13A H -0.0189 0.1792 0.6231 0.048 Uiso 1 1 calc R . . H13B H 0.1164 0.2293 0.6652 0.048 Uiso 1 1 calc R . . H13C H 0.0257 0.1440 0.7141 0.048 Uiso 1 1 calc R . . C14 C 0.0464(8) -0.0427(7) 0.6073(5) 0.0244(17) Uani 1 1 d . . . H14A H -0.0318 -0.0257 0.5729 0.037 Uiso 1 1 calc R . . H14B H 0.0169 -0.0663 0.6617 0.037 Uiso 1 1 calc R . . H14C H 0.0965 -0.1025 0.5797 0.037 Uiso 1 1 calc R . . C15 C 0.2911(6) 0.5837(6) 0.1288(5) 0.0134(12) Uani 1 1 d . . . H15 H 0.3551 0.6424 0.1376 0.016 Uiso 1 1 calc R . . C16 C 0.1766(6) 0.5837(6) 0.1794(5) 0.0140(13) Uani 1 1 d . . . H16 H 0.1653 0.6406 0.2212 0.017 Uiso 1 1 calc R . . C17 C 0.0779(6) 0.4967(5) 0.1664(4) 0.0090(11) Uani 1 1 d . . . C18 C 0.0999(7) 0.4166(6) 0.1007(6) 0.0198(15) Uani 1 1 d . . . H18 H 0.0356 0.3593 0.0879 0.024 Uiso 1 1 calc R . . C19 C 0.2184(7) 0.4234(6) 0.0546(5) 0.0175(14) Uani 1 1 d . . . H19 H 0.2323 0.3686 0.0116 0.021 Uiso 1 1 calc R . . C20 C -0.0518(6) 0.5036(5) 0.2133(4) 0.0103(11) Uani 1 1 d . . . C21 C 0.0343(6) 0.3679(6) 0.3165(5) 0.0139(13) Uani 1 1 d . . . H21A H 0.1070 0.3593 0.2759 0.017 Uiso 1 1 calc R . . H21B H -0.0093 0.2941 0.3213 0.017 Uiso 1 1 calc R . . C22 C 0.0970(7) 0.4052(6) 0.4026(5) 0.0175(14) Uani 1 1 d . . . H22 H 0.0235 0.4109 0.4438 0.021 Uiso 1 1 calc R . . C23 C 0.1706(9) 0.5188(7) 0.4024(6) 0.0278(18) Uani 1 1 d . . . H23A H 0.1083 0.5755 0.3852 0.042 Uiso 1 1 calc R . . H23B H 0.2448 0.5144 0.3635 0.042 Uiso 1 1 calc R . . H23C H 0.2056 0.5385 0.4585 0.042 Uiso 1 1 calc R . . C24 C 0.1943(9) 0.3128(8) 0.4302(6) 0.0294(19) Uani 1 1 d . . . H24A H 0.1457 0.2415 0.4303 0.044 Uiso 1 1 calc R . . H24B H 0.2296 0.3320 0.4863 0.044 Uiso 1 1 calc R . . H24C H 0.2683 0.3071 0.3913 0.044 Uiso 1 1 calc R . . C25 C -0.1952(7) 0.4613(7) 0.3306(5) 0.0216(15) Uani 1 1 d . . . H25A H -0.2185 0.5408 0.3323 0.026 Uiso 1 1 calc R . . H25B H -0.1807 0.4393 0.3886 0.026 Uiso 1 1 calc R . . C26 C -0.3183(10) 0.3888(9) 0.2890(7) 0.037(2) Uani 1 1 d . . . H26 H -0.3250 0.4049 0.2287 0.044 Uiso 1 1 calc R . . C27 C -0.3047(11) 0.2653(9) 0.2965(8) 0.040(2) Uani 1 1 d . . . H27A H -0.2247 0.2403 0.2674 0.060 Uiso 1 1 calc R . . H27B H -0.3838 0.2269 0.2715 0.060 Uiso 1 1 calc R . . H27C H -0.2969 0.2482 0.3553 0.060 Uiso 1 1 calc R . . C28 C -0.4495(10) 0.4327(11) 0.3337(11) 0.065(4) Uani 1 1 d . . . H28A H -0.4556 0.5131 0.3280 0.098 Uiso 1 1 calc R . . H28B H -0.4450 0.4165 0.3928 0.098 Uiso 1 1 calc R . . H28C H -0.5285 0.3956 0.3077 0.098 Uiso 1 1 calc R . . O1 O 0.4394(5) 0.2766(4) 0.7722(3) 0.0118(9) Uani 1 1 d . . . O2 O -0.1429(5) 0.5649(4) 0.1844(4) 0.0175(11) Uani 1 1 d . . . O3 O 0.6079(5) 0.5627(4) 0.1075(3) 0.0155(10) Uani 1 1 d . . . O4 O 0.5302(5) 0.3315(4) 0.0348(4) 0.0181(11) Uani 1 1 d . . . O5 O 0.7894(5) 0.2579(5) 0.0258(4) 0.0221(12) Uani 1 1 d . . . Br1 Br 0.23025(12) -0.12143(10) 1.15937(8) 0.0451(3) Uani 1 1 d . . . Br2 Br 0.35110(9) 0.19581(8) 1.18416(6) 0.0311(3) Uani 1 1 d . . . Br3 Br -0.03405(11) 0.11487(11) 1.15598(8) 0.0458(3) Uani 1 1 d . . . N1 N 0.2154(5) 0.0754(5) 0.9983(4) 0.0110(10) Uani 1 1 d . . . N2 N 0.3580(5) 0.1275(5) 0.6890(4) 0.0100(10) Uani 1 1 d . . . N3 N 0.3143(5) 0.5047(4) 0.0686(4) 0.0079(9) Uani 1 1 d . . . N4 N -0.0666(5) 0.4461(5) 0.2831(4) 0.0145(11) Uani 1 1 d . . . Co1 Co 0.18545(8) 0.06396(7) 1.12673(6) 0.0092(2) Uani 1 1 d . . . Co2 Co 0.5000 0.5000 0.0000 0.0058(2) Uani 1 2 d S . . 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 C1 0.009(3) 0.021(3) 0.012(3) 0.005(2) -0.003(2) 0.004(2) C2 0.010(3) 0.018(3) 0.009(3) 0.004(2) -0.001(2) 0.004(2) C3 0.007(2) 0.011(3) 0.008(3) 0.000(2) -0.003(2) 0.0017(19) C4 0.010(3) 0.009(3) 0.009(3) -0.001(2) 0.001(2) 0.0014(19) C5 0.011(3) 0.008(3) 0.006(3) -0.004(2) 0.000(2) 0.003(2) C6 0.009(3) 0.015(3) 0.005(3) -0.002(2) -0.002(2) 0.001(2) C7 0.012(3) 0.021(3) 0.007(3) -0.002(2) 0.002(2) -0.002(2) C8 0.014(3) 0.025(4) 0.013(3) -0.004(3) 0.002(2) -0.005(3) C9 0.029(4) 0.036(5) 0.025(5) -0.005(4) 0.004(3) 0.006(3) C10 0.023(4) 0.049(6) 0.022(4) -0.003(4) 0.015(3) -0.015(4) C11 0.016(3) 0.014(3) 0.013(3) -0.002(2) -0.002(2) -0.007(2) C12 0.016(3) 0.024(4) 0.014(3) 0.000(3) -0.003(2) -0.009(3) C13 0.023(4) 0.036(5) 0.037(5) -0.002(4) -0.010(4) 0.007(3) C14 0.023(4) 0.031(4) 0.018(4) 0.002(3) -0.005(3) -0.017(3) C15 0.007(3) 0.015(3) 0.018(3) -0.006(2) 0.002(2) -0.005(2) C16 0.008(3) 0.013(3) 0.019(3) -0.007(2) 0.003(2) -0.006(2) C17 0.004(2) 0.007(3) 0.016(3) 0.003(2) 0.001(2) -0.0008(18) C18 0.013(3) 0.010(3) 0.036(5) -0.009(3) 0.013(3) -0.007(2) C19 0.010(3) 0.011(3) 0.030(4) -0.011(3) 0.007(3) -0.007(2) C20 0.007(2) 0.006(3) 0.019(3) 0.001(2) 0.001(2) -0.0020(19) C21 0.006(3) 0.018(3) 0.019(3) 0.006(3) 0.002(2) -0.001(2) C22 0.012(3) 0.024(4) 0.017(4) 0.008(3) 0.003(2) -0.002(2) C23 0.031(4) 0.023(4) 0.029(5) -0.002(3) -0.013(3) -0.004(3) C24 0.024(4) 0.032(5) 0.033(5) 0.015(4) -0.009(3) 0.001(3) C25 0.012(3) 0.036(4) 0.018(4) 0.003(3) 0.004(3) 0.005(3) C26 0.031(5) 0.043(6) 0.037(6) 0.010(4) 0.011(4) -0.003(4) C27 0.033(5) 0.038(5) 0.048(7) -0.003(5) 0.005(4) -0.001(4) C28 0.020(5) 0.062(8) 0.112(12) -0.027(8) 0.034(6) -0.015(5) O1 0.015(2) 0.010(2) 0.010(2) -0.0039(16) 0.0045(17) -0.0033(16) O2 0.008(2) 0.012(2) 0.033(3) 0.009(2) 0.0001(19) 0.0039(16) O3 0.012(2) 0.019(2) 0.015(2) -0.0072(19) -0.0037(18) 0.0059(17) O4 0.019(2) 0.010(2) 0.026(3) 0.006(2) 0.006(2) 0.0027(18) O5 0.017(2) 0.022(3) 0.028(3) 0.004(2) 0.002(2) 0.010(2) Br1 0.0543(7) 0.0378(6) 0.0435(7) 0.0040(5) -0.0018(5) 0.0072(5) Br2 0.0263(4) 0.0357(5) 0.0308(5) 0.0034(4) -0.0061(3) -0.0105(3) Br3 0.0383(6) 0.0536(7) 0.0453(7) 0.0018(5) 0.0010(5) 0.0009(5) N1 0.009(2) 0.016(3) 0.008(3) -0.002(2) -0.0013(18) 0.0004(19) N2 0.010(2) 0.013(3) 0.007(3) -0.0001(19) -0.0004(18) -0.0033(18) N3 0.006(2) 0.003(2) 0.015(3) -0.0004(18) 0.0003(18) -0.0013(16) N4 0.006(2) 0.024(3) 0.014(3) 0.001(2) 0.0030(19) 0.003(2) Co1 0.0091(4) 0.0122(4) 0.0063(4) 0.0007(3) -0.0006(3) -0.0005(3) Co2 0.0044(5) 0.0033(5) 0.0096(6) -0.0008(4) 0.0009(4) 0.0004(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 C1 N1 1.347(8) . ? C1 C2 1.400(9) . ? C1 H1 0.9300 . ? C2 C3 1.401(8) . ? C2 H2 0.9300 . ? C3 C4 1.397(8) . ? C3 C6 1.509(9) . ? C4 C5 1.368(9) . ? C4 H4 0.9300 . ? C5 N1 1.324(8) . ? C5 H5 0.9300 . ? C6 O1 1.243(8) . ? C6 N2 1.354(8) . ? C7 N2 1.468(9) . ? C7 C8 1.532(9) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.525(12) . ? C8 C10 1.550(11) . ? C8 H8 0.9800 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 N2 1.453(8) . ? C11 C12 1.516(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C14 1.526(10) . ? C12 C13 1.551(12) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 N3 1.327(8) . ? C15 C16 1.389(9) . ? C15 H15 0.9300 . ? C16 C17 1.405(8) . ? C16 H16 0.9300 . ? C17 C18 1.393(10) . ? C17 C20 1.483(9) . ? C18 C19 1.384(9) . ? C18 H18 0.9300 . ? C19 N3 1.340(8) . ? C19 H19 0.9300 . ? C20 O2 1.251(7) . ? C20 N4 1.328(9) . ? C21 N4 1.471(8) . ? C21 C22 1.524(11) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.511(11) . ? C22 C24 1.534(11) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N4 1.486(9) . ? C25 C26 1.583(13) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 C27 1.476(15) . ? C26 C28 1.563(14) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? O3 Co2 2.082(5) . ? O4 Co2 2.112(5) . ? Br1 Co1 2.3182(14) . ? Br2 Co1 2.3696(12) . ? Br3 Co1 2.2937(14) . ? N1 Co1 2.061(6) . ? N3 Co2 2.134(5) . ? Co2 O3 2.082(5) 2_665 ? Co2 O4 2.112(5) 2_665 ? Co2 N3 2.134(5) 2_665 ? 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 C1 C2 122.0(6) . . ? N1 C1 H1 119.0 . . ? C2 C1 H1 119.0 . . ? C1 C2 C3 117.7(6) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 119.4(6) . . ? C4 C3 C6 121.7(5) . . ? C2 C3 C6 118.6(5) . . ? C5 C4 C3 117.7(6) . . ? C5 C4 H4 121.2 . . ? C3 C4 H4 121.2 . . ? N1 C5 C4 124.4(6) . . ? N1 C5 H5 117.8 . . ? C4 C5 H5 117.8 . . ? O1 C6 N2 122.1(6) . . ? O1 C6 C3 118.4(6) . . ? N2 C6 C3 119.5(6) . . ? N2 C7 C8 112.0(6) . . ? N2 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N2 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C9 C8 C7 113.2(6) . . ? C9 C8 C10 110.9(7) . . ? C7 C8 C10 105.8(6) . . ? C9 C8 H8 109.0 . . ? C7 C8 H8 109.0 . . ? C10 C8 H8 109.0 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N2 C11 C12 114.3(6) . . ? N2 C11 H11A 108.7 . . ? C12 C11 H11A 108.7 . . ? N2 C11 H11B 108.7 . . ? C12 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C11 C12 C14 108.6(6) . . ? C11 C12 C13 111.7(6) . . ? C14 C12 C13 110.8(7) . . ? C11 C12 H12 108.5 . . ? C14 C12 H12 108.5 . . ? C13 C12 H12 108.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 C16 123.6(6) . . ? N3 C15 H15 118.2 . . ? C16 C15 H15 118.2 . . ? C15 C16 C17 119.1(6) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 117.0(6) . . ? C18 C17 C20 123.2(6) . . ? C16 C17 C20 119.1(6) . . ? C19 C18 C17 119.3(6) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? N3 C19 C18 123.6(6) . . ? N3 C19 H19 118.2 . . ? C18 C19 H19 118.2 . . ? O2 C20 N4 123.0(6) . . ? O2 C20 C17 117.5(6) . . ? N4 C20 C17 119.6(5) . . ? N4 C21 C22 114.6(6) . . ? N4 C21 H21A 108.6 . . ? C22 C21 H21A 108.6 . . ? N4 C21 H21B 108.6 . . ? C22 C21 H21B 108.6 . . ? H21A C21 H21B 107.6 . . ? C23 C22 C21 113.4(6) . . ? C23 C22 C24 110.6(6) . . ? C21 C22 C24 108.2(7) . . ? C23 C22 H22 108.2 . . ? C21 C22 H22 108.2 . . ? C24 C22 H22 108.2 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 C26 112.4(7) . . ? N4 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N4 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.9 . . ? C27 C26 C28 111.3(9) . . ? C27 C26 C25 114.0(8) . . ? C28 C26 C25 106.0(8) . . ? C27 C26 H26 108.5 . . ? C28 C26 H26 108.5 . . ? C25 C26 H26 108.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C5 N1 C1 118.5(6) . . ? C5 N1 Co1 121.0(4) . . ? C1 N1 Co1 118.5(4) . . ? C6 N2 C11 123.2(6) . . ? C6 N2 C7 116.9(5) . . ? C11 N2 C7 119.4(5) . . ? C15 N3 C19 117.3(6) . . ? C15 N3 Co2 122.2(4) . . ? C19 N3 Co2 120.4(4) . . ? C20 N4 C21 124.8(5) . . ? C20 N4 C25 117.4(6) . . ? C21 N4 C25 117.7(6) . . ? N1 Co1 Br3 108.63(15) . . ? N1 Co1 Br1 106.82(16) . . ? Br3 Co1 Br1 112.87(6) . . ? N1 Co1 Br2 101.49(16) . . ? Br3 Co1 Br2 113.10(5) . . ? Br1 Co1 Br2 113.01(5) . . ? O3 Co2 O3 179.999(2) 2_665 . ? O3 Co2 O4 88.9(2) 2_665 . ? O3 Co2 O4 91.1(2) . . ? O3 Co2 O4 91.1(2) 2_665 2_665 ? O3 Co2 O4 88.9(2) . 2_665 ? O4 Co2 O4 180.0 . 2_665 ? O3 Co2 N3 90.4(2) 2_665 2_665 ? O3 Co2 N3 89.6(2) . 2_665 ? O4 Co2 N3 89.78(19) . 2_665 ? O4 Co2 N3 90.22(19) 2_665 2_665 ? O3 Co2 N3 89.6(2) 2_665 . ? O3 Co2 N3 90.4(2) . . ? O4 Co2 N3 90.22(19) . . ? O4 Co2 N3 89.78(19) 2_665 . ? N3 Co2 N3 180.0 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 1.9(10) . . . . ? C1 C2 C3 C4 -4.5(10) . . . . ? C1 C2 C3 C6 170.1(6) . . . . ? C2 C3 C4 C5 3.0(9) . . . . ? C6 C3 C4 C5 -171.4(6) . . . . ? C3 C4 C5 N1 1.4(10) . . . . ? C4 C3 C6 O1 76.3(8) . . . . ? C2 C3 C6 O1 -98.1(7) . . . . ? C4 C3 C6 N2 -105.7(7) . . . . ? C2 C3 C6 N2 79.9(8) . . . . ? N2 C7 C8 C9 59.1(8) . . . . ? N2 C7 C8 C10 -179.3(6) . . . . ? N2 C11 C12 C14 178.6(6) . . . . ? N2 C11 C12 C13 -58.9(9) . . . . ? N3 C15 C16 C17 -0.8(11) . . . . ? C15 C16 C17 C18 -2.0(10) . . . . ? C15 C16 C17 C20 -173.0(6) . . . . ? C16 C17 C18 C19 2.8(11) . . . . ? C20 C17 C18 C19 173.4(7) . . . . ? C17 C18 C19 N3 -1.1(12) . . . . ? C18 C17 C20 O2 -89.3(8) . . . . ? C16 C17 C20 O2 81.1(8) . . . . ? C18 C17 C20 N4 90.9(9) . . . . ? C16 C17 C20 N4 -98.6(8) . . . . ? N4 C21 C22 C23 -59.5(8) . . . . ? N4 C21 C22 C24 177.4(6) . . . . ? N4 C25 C26 C27 68.9(10) . . . . ? N4 C25 C26 C28 -168.4(9) . . . . ? C4 C5 N1 C1 -4.0(10) . . . . ? C4 C5 N1 Co1 159.8(5) . . . . ? C2 C1 N1 C5 2.2(10) . . . . ? C2 C1 N1 Co1 -161.9(5) . . . . ? O1 C6 N2 C11 -168.2(6) . . . . ? C3 C6 N2 C11 14.0(9) . . . . ? O1 C6 N2 C7 3.3(9) . . . . ? C3 C6 N2 C7 -174.6(5) . . . . ? C12 C11 N2 C6 106.2(7) . . . . ? C12 C11 N2 C7 -65.0(8) . . . . ? C8 C7 N2 C6 75.6(7) . . . . ? C8 C7 N2 C11 -112.7(7) . . . . ? C16 C15 N3 C19 2.5(10) . . . . ? C16 C15 N3 Co2 -174.4(5) . . . . ? C18 C19 N3 C15 -1.6(11) . . . . ? C18 C19 N3 Co2 175.4(6) . . . . ? O2 C20 N4 C21 176.2(6) . . . . ? C17 C20 N4 C21 -4.0(10) . . . . ? O2 C20 N4 C25 -3.3(10) . . . . ? C17 C20 N4 C25 176.5(6) . . . . ? C22 C21 N4 C20 115.2(7) . . . . ? C22 C21 N4 C25 -65.3(8) . . . . ? C26 C25 N4 C20 79.8(9) . . . . ? C26 C25 N4 C21 -99.8(8) . . . . ? C5 N1 Co1 Br3 30.6(5) . . . . ? C1 N1 Co1 Br3 -165.7(5) . . . . ? C5 N1 Co1 Br1 152.6(5) . . . . ? C1 N1 Co1 Br1 -43.7(5) . . . . ? C5 N1 Co1 Br2 -88.8(5) . . . . ? C1 N1 Co1 Br2 74.9(5) . . . . ? C15 N3 Co2 O3 -146.3(5) . . . 2_665 ? C19 N3 Co2 O3 36.9(6) . . . 2_665 ? C15 N3 Co2 O3 33.7(5) . . . . ? C19 N3 Co2 O3 -143.1(6) . . . . ? C15 N3 Co2 O4 124.8(5) . . . . ? C19 N3 Co2 O4 -52.0(6) . . . . ? C15 N3 Co2 O4 -55.2(5) . . . 2_665 ? C19 N3 Co2 O4 128.0(6) . . . 2_665 ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.656 _refine_diff_density_min -4.362 _refine_diff_density_rms 0.327