# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Jonas Peters' _publ_contact_author_email JONAS.PETERS@GMAIL.COM _publ_section_title ; Hydrogen Evolution by Cobalt Tetraimine Catalysts Adsorbed on Electrode Surfaces ; loop_ _publ_author_name 'Jonas Peters' 'Louise A. Berben' # Attachment 'Combined_cif_revision.CIF' data_08113 _database_code_depnum_ccdc_archive 'CCDC 735555' #TrackingRef 'Combined_cif_revision.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H22 B Br2 Co F2 N4 O2' _chemical_formula_sum 'C20 H22 B Br2 Co F2 N4 O2' _chemical_formula_weight 617.98 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 12.2153(8) _cell_length_b 13.1102(8) _cell_length_c 28.6077(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4581.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_absorpt_coefficient_mu 4.279 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4143 _exptl_absorpt_correction_T_max 0.5662 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEX2 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85831 _diffrn_reflns_av_R_equivalents 0.1098 _diffrn_reflns_av_sigmaI/netI 0.0425 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 27.72 _reflns_number_total 5361 _reflns_number_gt 4251 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0416P)^2^+3.2325P] 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 5361 _refine_ls_number_parameters 293 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0803 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.010 _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 Co1 Co 0.54006(3) 0.00860(3) 0.618873(14) 0.01268(10) Uani 1 1 d . . . Br1 Br 0.55128(3) 0.13624(2) 0.678186(11) 0.01952(9) Uani 1 1 d . . . Br2 Br 0.51361(3) -0.11509(2) 0.559629(11) 0.01843(9) Uani 1 1 d . . . N1 N 0.6485(2) 0.0782(2) 0.58353(9) 0.0172(6) Uani 1 1 d . . . N2 N 0.6421(2) -0.0821(2) 0.64729(9) 0.0164(5) Uani 1 1 d . . . N3 N 0.4408(2) -0.06639(19) 0.66143(9) 0.0136(5) Uani 1 1 d . . . N4 N 0.4455(2) 0.10468(19) 0.58449(8) 0.0128(5) Uani 1 1 d . . . C1 C 0.1504(3) 0.1530(2) 0.60697(12) 0.0216(7) Uani 1 1 d . . . H1 H 0.1051 0.1877 0.6288 0.026 Uiso 1 1 calc R . . C2 C 0.1379(3) -0.0789(3) 0.65176(12) 0.0248(8) Uani 1 1 d . . . H2 H 0.0836 -0.1080 0.6321 0.030 Uiso 1 1 calc R . . C3 C 0.1685(3) 0.0535(3) 0.53703(12) 0.0213(7) Uani 1 1 d . . . H3 H 0.1359 0.0191 0.5113 0.026 Uiso 1 1 calc R . . C4 C 0.2965(3) 0.0054(2) 0.71026(11) 0.0222(7) Uani 1 1 d . . . H4 H 0.3507 0.0340 0.7301 0.027 Uiso 1 1 calc R . . C5 C 0.1031(3) 0.1034(3) 0.56932(12) 0.0228(7) Uani 1 1 d . . . H5 H 0.0259 0.1035 0.5656 0.027 Uiso 1 1 calc R . . C6 C 0.2484(3) -0.0905(2) 0.64079(11) 0.0177(6) Uani 1 1 d . . . H6 H 0.2700 -0.1265 0.6135 0.021 Uiso 1 1 calc R . . C7 C 0.1069(3) -0.0247(3) 0.69157(13) 0.0298(9) Uani 1 1 d . . . H7 H 0.0316 -0.0163 0.6988 0.036 Uiso 1 1 calc R . . C8 C 0.2815(3) 0.0537(2) 0.54220(11) 0.0169(6) Uani 1 1 d . . . H8 H 0.3266 0.0204 0.5199 0.020 Uiso 1 1 calc R . . C9 C 0.1859(3) 0.0168(3) 0.72045(12) 0.0284(8) Uani 1 1 d . . . H9 H 0.1643 0.0536 0.7476 0.034 Uiso 1 1 calc R . . C10 C 0.2629(3) 0.1528(2) 0.61324(11) 0.0181(6) Uani 1 1 d . . . H10 H 0.2948 0.1858 0.6395 0.022 Uiso 1 1 calc R . . C11 C 0.3283(2) 0.1034(2) 0.58050(10) 0.0136(6) Uani 1 1 d . . . C12 C 0.3263(2) -0.0487(2) 0.67041(10) 0.0148(6) Uani 1 1 d . . . C13 C 0.4998(2) 0.1749(2) 0.56260(10) 0.0146(6) Uani 1 1 d . . . C14 C 0.4902(3) -0.1344(2) 0.68701(10) 0.0157(6) Uani 1 1 d . . . C15 C 0.6194(3) 0.1596(2) 0.56108(11) 0.0172(6) Uani 1 1 d . . . C16 C 0.6078(3) -0.1454(2) 0.67890(11) 0.0181(7) Uani 1 1 d . . . C17 C 0.6954(3) 0.2266(3) 0.53472(12) 0.0237(7) Uani 1 1 d . . . H17A H 0.7711 0.2096 0.5429 0.036 Uiso 1 1 calc R . . H17B H 0.6808 0.2980 0.5427 0.036 Uiso 1 1 calc R . . H17C H 0.6845 0.2165 0.5011 0.036 Uiso 1 1 calc R . . C18 C 0.6773(3) -0.2228(3) 0.70249(12) 0.0253(8) Uani 1 1 d . . . H18A H 0.6670 -0.2892 0.6874 0.038 Uiso 1 1 calc R . . H18B H 0.6564 -0.2276 0.7355 0.038 Uiso 1 1 calc R . . H18C H 0.7544 -0.2026 0.7002 0.038 Uiso 1 1 calc R . . C19 C 0.4354(3) -0.2019(3) 0.72223(11) 0.0221(7) Uani 1 1 d . . . H19A H 0.4547 -0.1792 0.7538 0.033 Uiso 1 1 calc R . . H19B H 0.4599 -0.2724 0.7178 0.033 Uiso 1 1 calc R . . H19C H 0.3559 -0.1982 0.7181 0.033 Uiso 1 1 calc R . . C20 C 0.4517(3) 0.2664(2) 0.53946(11) 0.0174(6) Uani 1 1 d . . . H20A H 0.3724 0.2674 0.5446 0.026 Uiso 1 1 calc R . . H20B H 0.4667 0.2637 0.5058 0.026 Uiso 1 1 calc R . . H20C H 0.4844 0.3282 0.5527 0.026 Uiso 1 1 calc R . . O1 O 0.75411(18) 0.04922(18) 0.57819(8) 0.0248(5) Uani 1 1 d . . . O2 O 0.74618(18) -0.09745(18) 0.63255(8) 0.0227(5) Uani 1 1 d . . . B1 B 0.8086(3) -0.0074(3) 0.61662(14) 0.0217(8) Uani 1 1 d . . . F1 F 0.82948(17) 0.05637(16) 0.65371(8) 0.0356(5) Uani 1 1 d . . . F2 F 0.90306(16) -0.04614(15) 0.59701(8) 0.0303(5) 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 Co1 0.0143(2) 0.0122(2) 0.0115(2) 0.00083(16) -0.00041(15) -0.00003(15) Br1 0.02745(18) 0.01612(17) 0.01498(16) -0.00173(12) -0.00550(12) -0.00062(12) Br2 0.02346(17) 0.01709(17) 0.01473(16) -0.00271(12) 0.00179(12) 0.00020(12) N1 0.0121(13) 0.0207(15) 0.0190(14) 0.0004(11) 0.0012(10) -0.0007(11) N2 0.0140(13) 0.0175(14) 0.0178(14) -0.0012(11) 0.0016(10) 0.0015(10) N3 0.0169(13) 0.0125(13) 0.0114(12) -0.0022(10) 0.0007(10) 0.0002(10) N4 0.0189(13) 0.0109(13) 0.0084(12) -0.0015(9) -0.0002(9) -0.0010(10) C1 0.0226(17) 0.0195(18) 0.0225(17) 0.0055(13) 0.0054(13) 0.0055(13) C2 0.0232(18) 0.0203(18) 0.031(2) 0.0117(15) -0.0006(15) 0.0001(14) C3 0.0187(17) 0.0233(18) 0.0219(17) 0.0074(14) -0.0075(13) -0.0035(13) C4 0.0308(19) 0.0212(18) 0.0147(16) -0.0009(13) 0.0041(13) 0.0060(14) C5 0.0144(16) 0.0241(18) 0.0300(19) 0.0122(15) 0.0011(13) 0.0030(13) C6 0.0197(16) 0.0130(16) 0.0204(16) 0.0042(12) 0.0002(12) -0.0007(12) C7 0.0215(18) 0.029(2) 0.038(2) 0.0167(17) 0.0139(15) 0.0088(15) C8 0.0224(16) 0.0147(16) 0.0136(15) 0.0030(12) -0.0005(12) 0.0003(12) C9 0.038(2) 0.026(2) 0.0212(18) 0.0062(15) 0.0156(15) 0.0112(16) C10 0.0239(17) 0.0125(15) 0.0178(16) 0.0008(12) 0.0001(13) 0.0025(13) C11 0.0171(15) 0.0120(15) 0.0116(14) 0.0061(11) 0.0001(11) -0.0010(12) C12 0.0162(15) 0.0130(16) 0.0152(15) 0.0047(12) 0.0053(11) 0.0016(12) C13 0.0193(15) 0.0156(16) 0.0088(14) -0.0016(11) -0.0016(12) -0.0005(12) C14 0.0218(16) 0.0131(15) 0.0122(15) -0.0010(11) -0.0025(12) 0.0014(12) C15 0.0193(16) 0.0167(16) 0.0157(16) 0.0018(12) -0.0017(12) -0.0030(12) C16 0.0214(17) 0.0146(16) 0.0182(16) -0.0010(13) -0.0037(13) 0.0026(12) C17 0.0227(18) 0.0233(19) 0.0251(18) 0.0068(14) 0.0025(13) -0.0038(14) C18 0.0251(18) 0.0240(19) 0.0267(19) 0.0049(15) -0.0057(14) 0.0079(14) C19 0.0275(18) 0.0190(17) 0.0199(17) 0.0083(13) 0.0024(13) -0.0002(14) C20 0.0218(16) 0.0149(16) 0.0156(15) 0.0033(12) -0.0001(12) 0.0000(12) O1 0.0139(11) 0.0291(14) 0.0314(14) 0.0061(11) 0.0044(9) 0.0024(10) O2 0.0141(11) 0.0229(12) 0.0310(14) 0.0025(10) 0.0031(9) 0.0053(9) B1 0.0169(17) 0.019(2) 0.029(2) 0.0006(16) -0.0025(15) -0.0006(15) F1 0.0331(12) 0.0318(13) 0.0419(13) -0.0110(10) -0.0118(10) 0.0013(10) F2 0.0188(10) 0.0267(11) 0.0454(13) 0.0023(10) 0.0043(9) 0.0024(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 N1 1.900(3) . ? Co1 N2 1.905(3) . ? Co1 N4 1.972(2) . ? Co1 N3 1.980(3) . ? Co1 Br2 2.3678(5) . ? Co1 Br1 2.3870(5) . ? N1 C15 1.295(4) . ? N1 O1 1.353(3) . ? N2 C16 1.297(4) . ? N2 O2 1.354(3) . ? N3 C14 1.302(4) . ? N3 C12 1.441(4) . ? N4 C13 1.296(4) . ? N4 C11 1.437(4) . ? C1 C5 1.385(5) . ? C1 C10 1.385(4) . ? C2 C7 1.395(5) . ? C2 C6 1.395(5) . ? C3 C5 1.385(5) . ? C3 C8 1.389(4) . ? C4 C9 1.391(5) . ? C4 C12 1.391(4) . ? C6 C12 1.387(4) . ? C7 C9 1.381(5) . ? C8 C11 1.397(4) . ? C10 C11 1.391(4) . ? C13 C15 1.475(4) . ? C13 C20 1.491(4) . ? C14 C16 1.462(4) . ? C14 C19 1.499(4) . ? C15 C17 1.484(4) . ? C16 C18 1.485(4) . ? O1 B1 1.484(4) . ? O2 B1 1.477(4) . ? B1 F1 1.375(4) . ? B1 F2 1.380(4) . ? 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 N2 94.02(11) . . ? N1 Co1 N4 80.59(11) . . ? N2 Co1 N4 174.23(11) . . ? N1 Co1 N3 173.13(11) . . ? N2 Co1 N3 80.12(11) . . ? N4 Co1 N3 105.38(11) . . ? N1 Co1 Br2 92.47(8) . . ? N2 Co1 Br2 88.13(8) . . ? N4 Co1 Br2 90.03(7) . . ? N3 Co1 Br2 90.95(7) . . ? N1 Co1 Br1 90.10(8) . . ? N2 Co1 Br1 95.54(8) . . ? N4 Co1 Br1 86.58(7) . . ? N3 Co1 Br1 86.91(7) . . ? Br2 Co1 Br1 175.37(2) . . ? C15 N1 O1 115.9(3) . . ? C15 N1 Co1 117.9(2) . . ? O1 N1 Co1 126.2(2) . . ? C16 N2 O2 115.2(3) . . ? C16 N2 Co1 119.0(2) . . ? O2 N2 Co1 125.05(19) . . ? C14 N3 C12 117.4(3) . . ? C14 N3 Co1 113.7(2) . . ? C12 N3 Co1 128.62(19) . . ? C13 N4 C11 118.7(3) . . ? C13 N4 Co1 113.3(2) . . ? C11 N4 Co1 128.02(19) . . ? C5 C1 C10 120.9(3) . . ? C7 C2 C6 120.1(3) . . ? C5 C3 C8 120.1(3) . . ? C9 C4 C12 118.7(3) . . ? C1 C5 C3 120.0(3) . . ? C12 C6 C2 118.9(3) . . ? C9 C7 C2 120.0(3) . . ? C3 C8 C11 119.4(3) . . ? C7 C9 C4 120.7(3) . . ? C1 C10 C11 118.9(3) . . ? C10 C11 C8 120.7(3) . . ? C10 C11 N4 120.9(3) . . ? C8 C11 N4 118.4(3) . . ? C6 C12 C4 121.5(3) . . ? C6 C12 N3 119.5(3) . . ? C4 C12 N3 118.8(3) . . ? N4 C13 C15 115.1(3) . . ? N4 C13 C20 125.8(3) . . ? C15 C13 C20 119.1(3) . . ? N3 C14 C16 115.7(3) . . ? N3 C14 C19 125.1(3) . . ? C16 C14 C19 119.2(3) . . ? N1 C15 C13 111.7(3) . . ? N1 C15 C17 124.6(3) . . ? C13 C15 C17 123.6(3) . . ? N2 C16 C14 111.4(3) . . ? N2 C16 C18 124.7(3) . . ? C14 C16 C18 123.8(3) . . ? N1 O1 B1 118.9(2) . . ? N2 O2 B1 117.5(2) . . ? F1 B1 F2 112.5(3) . . ? F1 B1 O2 110.1(3) . . ? F2 B1 O2 105.3(3) . . ? F1 B1 O1 110.5(3) . . ? F2 B1 O1 104.9(3) . . ? O2 B1 O1 113.4(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.72 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.881 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.108 #===END data_lab18 _database_code_depnum_ccdc_archive 'CCDC 735556' #TrackingRef 'Combined_cif_revision.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H27 Br2 Co N4 O4' _chemical_formula_sum 'C22 H27 Br2 Co N4 O4' _chemical_formula_weight 630.23 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' O O 0.0106 0.0060 '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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6425(11) _cell_length_b 12.4200(10) _cell_length_c 14.1086(11) _cell_angle_alpha 90.00 _cell_angle_beta 95.3260(10) _cell_angle_gamma 90.00 _cell_volume 2380.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.759 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 4.115 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3715 _exptl_absorpt_correction_T_max 0.4933 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEX2 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 55558 _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_sigmaI/netI 0.0554 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 31.73 _reflns_number_total 7641 _reflns_number_gt 5517 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0322P)^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 7641 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.216795(19) 0.74260(2) 0.028461(19) 0.01258(6) Uani 1 1 d . . . Br1 Br 0.116931(15) 0.694293(17) 0.151327(14) 0.01740(6) Uani 1 1 d . . . Br2 Br 0.316923(15) 0.788612(18) -0.095669(14) 0.01927(6) Uani 1 1 d . . . N1 N 0.28492(12) 0.84976(14) 0.10753(12) 0.0158(4) Uani 1 1 d . . . N2 N 0.11549(12) 0.83724(13) -0.02398(12) 0.0156(4) Uani 1 1 d . . . N3 N 0.32433(12) 0.65328(14) 0.09246(11) 0.0147(3) Uani 1 1 d . . . N4 N 0.14191(12) 0.64347(13) -0.06063(11) 0.0135(3) Uani 1 1 d . . . C1 C 0.40608(17) 0.15060(18) 0.01664(17) 0.0274(5) Uani 1 1 d . . . H1A H 0.3733 0.1727 -0.0450 0.041 Uiso 1 1 calc R . . H1B H 0.3989 0.0727 0.0243 0.041 Uiso 1 1 calc R . . H1C H 0.4761 0.1690 0.0194 0.041 Uiso 1 1 calc R . . C2 C 0.16324(17) 0.13028(17) -0.10263(16) 0.0244(5) Uani 1 1 d . . . H2A H 0.1962 0.1311 -0.0379 0.037 Uiso 1 1 calc R . . H2B H 0.1749 0.0609 -0.1327 0.037 Uiso 1 1 calc R . . H2C H 0.0923 0.1408 -0.1001 0.037 Uiso 1 1 calc R . . C3 C -0.00200(15) 0.63007(18) -0.18189(15) 0.0188(4) Uani 1 1 d . . . H3A H 0.0182 0.6434 -0.2457 0.028 Uiso 1 1 calc R . . H3B H -0.0691 0.6569 -0.1783 0.028 Uiso 1 1 calc R . . H3C H 0.0000 0.5526 -0.1689 0.028 Uiso 1 1 calc R . . C4 C 0.42867(16) 0.89880(18) 0.21721(16) 0.0241(5) Uani 1 1 d . . . H4A H 0.3981 0.9702 0.2139 0.036 Uiso 1 1 calc R . . H4B H 0.4937 0.9027 0.1932 0.036 Uiso 1 1 calc R . . H4C H 0.4357 0.8741 0.2835 0.036 Uiso 1 1 calc R . . C5 C 0.47311(15) 0.65990(18) 0.20753(15) 0.0215(5) Uani 1 1 d . . . H5A H 0.4580 0.6507 0.2736 0.032 Uiso 1 1 calc R . . H5B H 0.5294 0.7085 0.2056 0.032 Uiso 1 1 calc R . . H5C H 0.4892 0.5898 0.1811 0.032 Uiso 1 1 calc R . . C6 C -0.02983(16) 0.86730(17) -0.13856(15) 0.0205(5) Uani 1 1 d . . . H6A H -0.0223 0.9423 -0.1175 0.031 Uiso 1 1 calc R . . H6B H -0.0937 0.8399 -0.1230 0.031 Uiso 1 1 calc R . . H6C H -0.0262 0.8634 -0.2075 0.031 Uiso 1 1 calc R . . C7 C 0.20647(15) 0.50676(16) -0.16297(14) 0.0154(4) Uani 1 1 d . . . H7 H 0.2273 0.5620 -0.2031 0.018 Uiso 1 1 calc R . . C8 C 0.13271(15) 0.45318(16) -0.02190(14) 0.0162(4) Uani 1 1 d . . . H8 H 0.1038 0.4719 0.0346 0.019 Uiso 1 1 calc R . . C9 C 0.39034(15) 0.37772(17) 0.01555(15) 0.0189(4) Uani 1 1 d . . . H9 H 0.4211 0.3443 -0.0345 0.023 Uiso 1 1 calc R . . C10 C 0.30331(16) 0.47632(18) 0.16394(15) 0.0197(5) Uani 1 1 d . . . H10 H 0.2743 0.5099 0.2150 0.024 Uiso 1 1 calc R . . C11 C 0.37811(15) 0.48901(17) 0.01650(15) 0.0176(4) Uani 1 1 d . . . H11 H 0.3994 0.5312 -0.0338 0.021 Uiso 1 1 calc R . . C12 C 0.31408(16) 0.36547(18) 0.16257(15) 0.0208(5) Uani 1 1 d . . . H12 H 0.2919 0.3233 0.2125 0.025 Uiso 1 1 calc R . . C13 C 0.21981(15) 0.39993(17) -0.18590(14) 0.0165(4) Uani 1 1 d . . . H13 H 0.2505 0.3816 -0.2415 0.020 Uiso 1 1 calc R . . C14 C 0.14495(15) 0.34567(17) -0.04495(15) 0.0174(4) Uani 1 1 d . . . H14 H 0.1240 0.2906 -0.0047 0.021 Uiso 1 1 calc R . . C15 C 0.35717(16) 0.31552(17) 0.08851(16) 0.0198(5) Uani 1 1 d . . . C16 C 0.18816(16) 0.31924(16) -0.12734(15) 0.0174(4) Uani 1 1 d . . . C17 C 0.33509(15) 0.53876(16) 0.09033(14) 0.0156(4) Uani 1 1 d . . . C18 C 0.16256(14) 0.53307(16) -0.08113(14) 0.0141(4) Uani 1 1 d . . . C19 C 0.36547(15) 0.82161(17) 0.15802(14) 0.0171(4) Uani 1 1 d . . . C20 C 0.38544(15) 0.70677(17) 0.14987(14) 0.0168(4) Uani 1 1 d . . . C21 C 0.05070(15) 0.80064(16) -0.08918(14) 0.0160(4) Uani 1 1 d . . . C22 C 0.06690(15) 0.68735(16) -0.10949(14) 0.0155(4) Uani 1 1 d . . . O1 O 0.36152(12) 0.20592(12) 0.09245(12) 0.0260(4) Uani 1 1 d . . . O2 O 0.20173(12) 0.21534(12) -0.15710(11) 0.0233(3) Uani 1 1 d . . . O3 O 0.10795(11) 0.93880(12) 0.00366(11) 0.0218(3) Uani 1 1 d . . . O4 O 0.25670(11) 0.95180(11) 0.10942(10) 0.0209(3) Uani 1 1 d . . . H60 H 0.175(2) 0.954(2) 0.057(2) 0.066(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01176(14) 0.01491(14) 0.01084(13) -0.00035(10) -0.00017(10) -0.00017(11) Br1 0.01589(11) 0.02322(11) 0.01347(10) -0.00036(8) 0.00349(8) -0.00018(8) Br2 0.01730(11) 0.02680(12) 0.01398(10) 0.00166(8) 0.00283(8) -0.00436(9) N1 0.0166(9) 0.0175(9) 0.0136(8) -0.0007(7) 0.0029(7) -0.0018(7) N2 0.0156(9) 0.0159(8) 0.0155(8) 0.0002(7) 0.0019(7) 0.0003(7) N3 0.0137(9) 0.0180(9) 0.0125(8) 0.0001(7) 0.0021(7) 0.0003(7) N4 0.0142(9) 0.0160(8) 0.0107(8) 0.0004(7) 0.0027(7) -0.0015(7) C1 0.0224(12) 0.0222(12) 0.0369(14) -0.0023(10) -0.0018(11) 0.0010(10) C2 0.0320(13) 0.0171(11) 0.0240(12) 0.0009(9) 0.0024(10) -0.0031(10) C3 0.0170(11) 0.0224(11) 0.0166(10) 0.0010(8) -0.0013(9) -0.0035(9) C4 0.0203(12) 0.0276(12) 0.0233(12) -0.0044(10) -0.0040(9) -0.0042(9) C5 0.0168(11) 0.0306(12) 0.0164(11) -0.0012(9) -0.0017(9) 0.0044(9) C6 0.0192(11) 0.0228(11) 0.0188(11) 0.0012(9) -0.0010(9) 0.0039(9) C7 0.0156(10) 0.0185(10) 0.0120(9) 0.0011(8) 0.0009(8) -0.0031(8) C8 0.0146(10) 0.0205(11) 0.0135(10) -0.0014(8) 0.0016(8) -0.0007(8) C9 0.0150(10) 0.0244(11) 0.0170(11) -0.0019(9) 0.0007(8) 0.0009(9) C10 0.0182(11) 0.0263(12) 0.0143(10) 0.0016(9) -0.0004(9) 0.0016(9) C11 0.0139(10) 0.0240(11) 0.0148(10) 0.0029(8) 0.0002(8) -0.0011(8) C12 0.0210(11) 0.0250(11) 0.0159(11) 0.0053(9) 0.0002(9) -0.0019(9) C13 0.0176(11) 0.0210(11) 0.0109(9) -0.0023(8) 0.0011(8) -0.0016(8) C14 0.0163(10) 0.0185(10) 0.0170(10) 0.0034(8) -0.0001(8) -0.0034(8) C15 0.0150(11) 0.0199(11) 0.0237(11) 0.0002(9) -0.0039(9) 0.0001(8) C16 0.0167(11) 0.0174(10) 0.0176(10) -0.0019(8) -0.0019(9) -0.0008(8) C17 0.0116(10) 0.0186(10) 0.0158(10) 0.0012(8) -0.0024(8) 0.0006(8) C18 0.0126(10) 0.0167(10) 0.0126(9) -0.0016(8) -0.0011(8) -0.0016(8) C19 0.0153(11) 0.0232(11) 0.0127(10) -0.0017(8) 0.0008(8) -0.0030(8) C20 0.0130(10) 0.0248(11) 0.0128(10) 0.0002(8) 0.0024(8) -0.0006(8) C21 0.0144(10) 0.0200(11) 0.0135(10) 0.0018(8) 0.0014(8) 0.0002(8) C22 0.0145(10) 0.0199(11) 0.0122(9) 0.0013(8) 0.0026(8) -0.0030(8) O1 0.0297(9) 0.0193(8) 0.0284(9) 0.0020(7) -0.0004(7) -0.0001(7) O2 0.0332(9) 0.0165(8) 0.0210(8) -0.0021(6) 0.0070(7) -0.0009(7) O3 0.0237(9) 0.0158(8) 0.0248(8) -0.0028(6) -0.0039(7) 0.0044(6) O4 0.0247(9) 0.0156(7) 0.0215(8) -0.0033(6) -0.0026(7) 0.0003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.9103(17) . ? Co1 N1 1.9201(17) . ? Co1 N4 1.9751(16) . ? Co1 N3 1.9881(17) . ? Co1 Br1 2.3789(4) . ? Co1 Br2 2.3883(4) . ? N1 C19 1.301(3) . ? N1 O4 1.326(2) . ? N2 C21 1.297(3) . ? N2 O3 1.327(2) . ? N3 C20 1.291(3) . ? N3 C17 1.430(3) . ? N4 C22 1.299(3) . ? N4 C18 1.435(2) . ? C1 O1 1.451(3) . ? C2 O2 1.434(2) . ? C3 C22 1.502(3) . ? C4 C19 1.492(3) . ? C5 C20 1.500(3) . ? C6 C21 1.495(3) . ? C7 C13 1.382(3) . ? C7 C18 1.388(3) . ? C8 C18 1.383(3) . ? C8 C14 1.388(3) . ? C9 C11 1.393(3) . ? C9 C15 1.396(3) . ? C10 C12 1.385(3) . ? C10 C17 1.397(3) . ? C11 C17 1.387(3) . ? C12 C15 1.392(3) . ? C13 C16 1.393(3) . ? C14 C16 1.391(3) . ? C15 O1 1.363(2) . ? C16 O2 1.375(2) . ? C19 C20 1.459(3) . ? C21 C22 1.457(3) . ? 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 N2 Co1 N1 95.30(7) . . ? N2 Co1 N4 79.87(7) . . ? N1 Co1 N4 174.65(7) . . ? N2 Co1 N3 174.94(7) . . ? N1 Co1 N3 79.97(7) . . ? N4 Co1 N3 104.92(7) . . ? N2 Co1 Br1 89.70(5) . . ? N1 Co1 Br1 91.75(5) . . ? N4 Co1 Br1 90.52(5) . . ? N3 Co1 Br1 88.67(5) . . ? N2 Co1 Br2 90.64(5) . . ? N1 Co1 Br2 88.92(5) . . ? N4 Co1 Br2 88.84(5) . . ? N3 Co1 Br2 91.05(5) . . ? Br1 Co1 Br2 179.214(15) . . ? C19 N1 O4 118.56(17) . . ? C19 N1 Co1 118.08(14) . . ? O4 N1 Co1 123.27(13) . . ? C21 N2 O3 118.36(17) . . ? C21 N2 Co1 118.68(14) . . ? O3 N2 Co1 122.96(13) . . ? C20 N3 C17 117.60(17) . . ? C20 N3 Co1 113.83(14) . . ? C17 N3 Co1 128.18(13) . . ? C22 N4 C18 116.98(17) . . ? C22 N4 Co1 114.30(14) . . ? C18 N4 Co1 128.64(13) . . ? C13 C7 C18 119.81(19) . . ? C18 C8 C14 120.01(19) . . ? C11 C9 C15 119.7(2) . . ? C12 C10 C17 120.1(2) . . ? C17 C11 C9 120.6(2) . . ? C10 C12 C15 120.4(2) . . ? C7 C13 C16 119.82(19) . . ? C8 C14 C16 119.50(19) . . ? O1 C15 C12 115.7(2) . . ? O1 C15 C9 124.5(2) . . ? C12 C15 C9 119.7(2) . . ? O2 C16 C14 123.81(19) . . ? O2 C16 C13 115.86(18) . . ? C14 C16 C13 120.33(19) . . ? C11 C17 C10 119.54(19) . . ? C11 C17 N3 120.67(18) . . ? C10 C17 N3 119.79(18) . . ? C8 C18 C7 120.52(19) . . ? C8 C18 N4 119.31(17) . . ? C7 C18 N4 120.04(18) . . ? N1 C19 C20 111.97(18) . . ? N1 C19 C4 123.3(2) . . ? C20 C19 C4 124.75(19) . . ? N3 C20 C19 115.99(19) . . ? N3 C20 C5 125.2(2) . . ? C19 C20 C5 118.82(19) . . ? N2 C21 C22 111.83(18) . . ? N2 C21 C6 123.99(19) . . ? C22 C21 C6 124.16(19) . . ? N4 C22 C21 115.29(18) . . ? N4 C22 C3 125.07(19) . . ? C21 C22 C3 119.63(18) . . ? C15 O1 C1 117.53(18) . . ? C16 O2 C2 117.47(17) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 31.73 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.848 _refine_diff_density_min -0.510 _refine_diff_density_rms 0.107 #===END data_08105 _database_code_depnum_ccdc_archive 'CCDC 735557' #TrackingRef 'Combined_cif_revision.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 B Br2 Co F2 N4 O4' _chemical_formula_sum 'C22 H26 B Br2 Co F2 N4 O4' _chemical_formula_weight 678.03 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.3248(16) _cell_length_b 11.816(2) _cell_length_c 18.730(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.463(3) _cell_angle_gamma 90.00 _cell_volume 2504.0(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 30.4 _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.799 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 3.929 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3852 _exptl_absorpt_correction_T_max 0.6947 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEX2 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7513 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 30.14 _reflns_number_total 4239 _reflns_number_gt 3071 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(14) _refine_ls_number_reflns 4239 _refine_ls_number_parameters 601 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1064 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.576 _refine_ls_restrained_S_all 0.576 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co -2.17216(15) -0.83744(9) -0.11881(8) 0.0111(3) Uani 1 1 d . . . Br1 Br -1.97418(10) -0.90550(7) -0.10820(6) 0.0153(3) Uani 1 1 d . . . Br2 Br -2.37398(10) -0.77867(7) -0.12919(6) 0.0151(3) Uani 1 1 d . . . N1 N -2.2168(9) -0.9379(6) -0.0406(5) 0.013(2) Uani 1 1 d . . . N2 N -2.1409(9) -0.7278(6) -0.1893(5) 0.0098(17) Uiso 1 1 d . . . N3 N -2.1463(9) -0.7362(6) -0.0405(5) 0.0121(17) Uiso 1 1 d . . . N4 N -2.1930(9) -0.9299(6) -0.2053(5) 0.0146(19) Uiso 1 1 d . . . O1 O -2.1153(8) -0.6264(5) -0.0452(4) 0.020(2) Uani 1 1 d . . . O2 O -2.1221(7) -0.6155(5) -0.1749(4) 0.016(2) Uani 1 1 d . . . O3 O -2.2751(7) -1.3914(6) -0.2393(4) 0.021(2) Uani 1 1 d . . . O4 O -2.4091(8) -1.3707(5) -0.0432(5) 0.024(2) Uani 1 1 d . . . C1 C -2.1808(11) -0.8753(7) -0.2632(6) 0.015(2) Uiso 1 1 d . . . C2 C -2.1564(10) -0.7549(7) -0.2543(6) 0.011(3) Uani 1 1 d . . . C3 C -2.2091(11) -0.8900(8) 0.0215(6) 0.015(2) Uiso 1 1 d . . . C4 C -2.1665(10) -0.7719(7) 0.0225(5) 0.012(3) Uani 1 1 d . . . C5 C -2.2633(11) -1.2777(8) -0.2290(6) 0.014(3) Uani 1 1 d . . . C6 C -2.2169(11) -1.0505(7) -0.2100(6) 0.011(2) Uiso 1 1 d . . . C7 C -2.3553(11) -1.2665(7) -0.0440(6) 0.014(3) Uani 1 1 d . . . C8 C -2.2659(12) -1.0520(7) -0.0440(5) 0.012(3) Uani 1 1 d . . . C9 C -2.2487(12) -0.9404(7) 0.0900(6) 0.019(3) Uani 1 1 d . . . H9A H -2.2436 -1.0231 0.0874 0.029 Uiso 1 1 calc R . . H9B H -2.3306 -0.9181 0.0973 0.029 Uiso 1 1 calc R . . H9C H -2.1978 -0.9130 0.1299 0.029 Uiso 1 1 calc R . . C10 C -2.1931(11) -0.9262(8) -0.3362(6) 0.015(3) Uani 1 1 d . . . H10A H -2.2652 -0.8975 -0.3608 0.022 Uiso 1 1 calc R . . H10B H -2.1978 -1.0088 -0.3322 0.022 Uiso 1 1 calc R . . H10C H -2.1244 -0.9057 -0.3635 0.022 Uiso 1 1 calc R . . C11 C -2.1548(12) -0.6753(8) -0.3155(6) 0.022(3) Uani 1 1 d . . . H11A H -2.1484 -0.5975 -0.2976 0.033 Uiso 1 1 calc R . . H11B H -2.2279 -0.6836 -0.3449 0.033 Uiso 1 1 calc R . . H11C H -2.0869 -0.6923 -0.3444 0.033 Uiso 1 1 calc R . . C12 C -2.1542(11) -0.7042(7) 0.0881(6) 0.017(3) Uani 1 1 d . . . H12A H -2.2320 -0.6940 0.1081 0.025 Uiso 1 1 calc R . . H12B H -2.1207 -0.6302 0.0770 0.025 Uiso 1 1 calc R . . H12C H -2.1017 -0.7434 0.1229 0.025 Uiso 1 1 calc R . . C13 C -2.3321(12) -1.4676(8) -0.0485(7) 0.023(3) Uani 1 1 d . . . H13A H -2.2759 -1.4691 -0.0072 0.034 Uiso 1 1 calc R . . H13B H -2.2887 -1.4623 -0.0925 0.034 Uiso 1 1 calc R . . H13C H -2.3794 -1.5371 -0.0493 0.034 Uiso 1 1 calc R . . C14 C -2.3919(12) -1.4354(8) -0.2412(6) 0.020(3) Uani 1 1 d . . . H14A H -2.4390 -1.3989 -0.2797 0.031 Uiso 1 1 calc R . . H14B H -2.4278 -1.4206 -0.1954 0.031 Uiso 1 1 calc R . . H14C H -2.3895 -1.5172 -0.2496 0.031 Uiso 1 1 calc R . . C15 C -2.1474(11) -1.2397(7) -0.2249(7) 0.016(3) Uani 1 1 d . . . H15 H -2.0841 -1.2920 -0.2279 0.020 Uiso 1 1 calc R . . C16 C -2.4328(11) -1.1747(7) -0.0375(6) 0.017(3) Uani 1 1 d . . . H16 H -2.5151 -1.1860 -0.0326 0.020 Uiso 1 1 calc R . . C17 C -2.3840(12) -1.0658(7) -0.0383(6) 0.020(3) Uani 1 1 d . . . H17 H -2.4337 -1.0014 -0.0350 0.024 Uiso 1 1 calc R . . C18 C -2.3585(12) -1.2035(7) -0.2222(6) 0.018(3) Uani 1 1 d . . . H18 H -2.4378 -1.2300 -0.2243 0.022 Uiso 1 1 calc R . . C19 C -2.1238(11) -1.1246(7) -0.2165(6) 0.012(3) Uani 1 1 d . . . H19 H -2.0447 -1.0976 -0.2153 0.015 Uiso 1 1 calc R . . C20 C -2.3322(11) -1.0891(7) -0.2122(6) 0.014(3) Uani 1 1 d . . . H20 H -2.3948 -1.0366 -0.2068 0.017 Uiso 1 1 calc R . . C21 C -2.2382(12) -1.2499(7) -0.0489(6) 0.019(3) Uani 1 1 d . . . H21 H -2.1875 -1.3134 -0.0528 0.023 Uiso 1 1 calc R . . C22 C -2.1901(12) -1.1414(8) -0.0482(6) 0.014(3) Uani 1 1 d . . . H22 H -2.1073 -1.1300 -0.0506 0.017 Uiso 1 1 calc R . . B1 B -2.0524(13) -0.5890(8) -0.1087(7) 0.014(2) Uiso 1 1 d . . . F1 F -2.0501(6) -0.4724(4) -0.1053(4) 0.0196(17) Uani 1 1 d . . . F2 F -1.9433(6) -0.6353(5) -0.1085(4) 0.0190(16) Uani 1 1 d . . . Co2 Co -1.67460(15) -1.83270(9) -0.36692(8) 0.0116(4) Uani 1 1 d . . . Br3 Br -1.87578(11) -1.89173(7) -0.36385(6) 0.0165(3) Uani 1 1 d . . . Br4 Br -1.47939(11) -1.75855(7) -0.37066(6) 0.0155(3) Uani 1 1 d . . . N5 N -1.6518(10) -1.9392(7) -0.4410(6) 0.023(3) Uani 1 1 d . . . N6 N -1.6322(9) -1.9366(6) -0.2918(5) 0.014(2) Uani 1 1 d . . . N7 N -1.6997(9) -1.7361(6) -0.2837(5) 0.013(2) Uani 1 1 d . . . N8 N -1.7176(9) -1.7379(6) -0.4507(5) 0.014(2) Uani 1 1 d . . . O5 O -1.6063(7) -2.0472(5) -0.3009(4) 0.0142(19) Uani 1 1 d . . . O7 O -1.8791(8) -1.2989(5) -0.2745(5) 0.025(2) Uani 1 1 d . . . O6 O -1.6269(8) -2.0502(5) -0.4312(5) 0.021(2) Uani 1 1 d . . . O8 O -1.8181(9) -1.2797(7) -0.4772(5) 0.039(3) Uani 1 1 d . . . C23 C -1.6782(11) -1.9115(8) -0.5062(6) 0.021(3) Uani 1 1 d . . . C24 C -1.7151(11) -1.7901(8) -0.5114(6) 0.017(3) Uani 1 1 d . . . C25 C -1.6434(11) -1.9050(8) -0.2268(6) 0.019(2) Uiso 1 1 d . . . C26 C -1.6807(10) -1.7860(7) -0.2226(5) 0.0109(18) Uiso 1 1 d . . . C27 C -1.8258(11) -1.4032(8) -0.2774(5) 0.013(3) Uani 1 1 d . . . C28 C -1.7442(12) -1.6217(7) -0.2829(6) 0.014(3) Uani 1 1 d . . . C29 C -1.7992(13) -1.3934(9) -0.4687(6) 0.026(3) Uani 1 1 d . . . C30 C -1.7447(12) -1.6184(7) -0.4535(6) 0.019(3) Uani 1 1 d . . . C31 C -1.6334(11) -1.9790(8) -0.1622(6) 0.015(3) Uani 1 1 d . . . H31A H -1.6231 -2.0578 -0.1770 0.023 Uiso 1 1 calc R . . H31B H -1.7055 -1.9723 -0.1354 0.023 Uiso 1 1 calc R . . H31C H -1.5651 -1.9554 -0.1319 0.023 Uiso 1 1 calc R . . C32 C -1.6813(13) -1.9898(10) -0.5671(7) 0.034(4) Uani 1 1 d . . . H32A H -1.7623 -2.0169 -0.5763 0.051 Uiso 1 1 calc R . . H32B H -1.6292 -2.0543 -0.5561 0.051 Uiso 1 1 calc R . . H32C H -1.6544 -1.9505 -0.6095 0.051 Uiso 1 1 calc R . . C33 C -1.7438(11) -1.7417(8) -0.5839(6) 0.019(3) Uani 1 1 d . . . H33A H -1.7928 -1.6740 -0.5792 0.029 Uiso 1 1 calc R . . H33B H -1.7870 -1.7980 -0.6132 0.029 Uiso 1 1 calc R . . H33C H -1.6704 -1.7216 -0.6067 0.029 Uiso 1 1 calc R . . C34 C -1.6910(11) -1.7331(7) -0.1521(6) 0.013(3) Uani 1 1 d . . . H34A H -1.7688 -1.7500 -0.1339 0.019 Uiso 1 1 calc R . . H34B H -1.6816 -1.6509 -0.1565 0.019 Uiso 1 1 calc R . . H34C H -1.6293 -1.7630 -0.1190 0.019 Uiso 1 1 calc R . . C35 C -1.9278(14) -1.2360(9) -0.4616(8) 0.037(4) Uani 1 1 d . . . H35A H -1.9439 -1.2522 -0.4116 0.056 Uiso 1 1 calc R . . H35B H -1.9890 -1.2709 -0.4929 0.056 Uiso 1 1 calc R . . H35C H -1.9279 -1.1539 -0.4692 0.056 Uiso 1 1 calc R . . C36 C -1.8051(12) -1.2046(7) -0.2864(7) 0.027(4) Uani 1 1 d . . . H36A H -1.7664 -1.2142 -0.3318 0.041 Uiso 1 1 calc R . . H36B H -1.7448 -1.1989 -0.2474 0.041 Uiso 1 1 calc R . . H36C H -1.8527 -1.1353 -0.2882 0.041 Uiso 1 1 calc R . . C37 C -1.8543(12) -1.5822(8) -0.4380(7) 0.024(3) Uani 1 1 d . . . H37 H -1.9101 -1.6347 -0.4209 0.028 Uiso 1 1 calc R . . C38 C -1.6722(12) -1.5327(8) -0.3013(6) 0.019(3) Uani 1 1 d . . . H38 H -1.5939 -1.5467 -0.3153 0.023 Uiso 1 1 calc R . . C39 C -1.6579(14) -1.5434(8) -0.4772(6) 0.025(3) Uani 1 1 d . . . H39 H -1.5816 -1.5696 -0.4886 0.030 Uiso 1 1 calc R . . C40 C -1.8860(14) -1.4693(9) -0.4469(7) 0.028(4) Uani 1 1 d . . . H40 H -1.9639 -1.4443 -0.4385 0.034 Uiso 1 1 calc R . . C41 C -1.9004(10) -1.4944(7) -0.2608(5) 0.0103(18) Uiso 1 1 d . . . H41 H -1.9793 -1.4806 -0.2480 0.012 Uiso 1 1 calc R . . C42 C -1.6882(14) -1.4295(8) -0.4834(7) 0.035(4) Uani 1 1 d . . . H42 H -1.6311 -1.3763 -0.4979 0.042 Uiso 1 1 calc R . . C43 C -1.7151(11) -1.4232(8) -0.2992(6) 0.015(2) Uiso 1 1 d . . . H43 H -1.6670 -1.3618 -0.3131 0.019 Uiso 1 1 calc R . . C44 C -1.8580(11) -1.6034(7) -0.2634(6) 0.013(2) Uiso 1 1 d . . . H44 H -1.9070 -1.6653 -0.2518 0.016 Uiso 1 1 calc R . . B2 B -1.5528(15) -2.0814(9) -0.3682(7) 0.019(4) Uani 1 1 d . . . F3 F -1.4417(6) -2.0338(5) -0.3713(4) 0.0194(16) Uani 1 1 d . . . F4 F -1.5488(6) -2.1972(4) -0.3662(4) 0.0234(18) 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 Co1 0.0132(11) 0.0095(5) 0.0105(7) 0.0011(4) 0.0006(6) -0.0003(5) Br1 0.0120(8) 0.0146(4) 0.0192(6) 0.0005(3) -0.0016(5) 0.0018(4) Br2 0.0091(8) 0.0155(4) 0.0207(6) 0.0017(3) 0.0001(5) 0.0013(4) N1 0.021(8) 0.010(3) 0.008(5) 0.003(2) -0.004(5) 0.000(3) O1 0.022(6) 0.012(3) 0.026(5) -0.004(3) 0.005(4) -0.004(3) O2 0.023(6) 0.007(3) 0.019(5) 0.006(2) -0.005(4) -0.002(3) O3 0.019(6) 0.014(3) 0.029(5) 0.000(3) -0.002(4) -0.004(3) O4 0.025(7) 0.010(3) 0.039(6) -0.001(3) 0.010(5) -0.006(3) C2 0.004(8) 0.019(4) 0.012(6) 0.001(3) 0.000(5) 0.003(4) C4 0.010(8) 0.013(4) 0.013(5) -0.003(3) -0.005(5) 0.001(4) C5 0.006(9) 0.018(5) 0.018(6) -0.004(4) -0.006(5) -0.005(4) C7 0.006(9) 0.013(4) 0.022(6) 0.003(3) 0.001(6) 0.003(4) C8 0.018(10) 0.012(4) 0.004(5) 0.003(3) -0.004(5) -0.004(4) C9 0.028(9) 0.020(4) 0.009(6) 0.002(3) 0.002(6) -0.006(4) C10 0.003(8) 0.031(5) 0.010(6) 0.003(3) -0.001(5) -0.002(4) C11 0.022(10) 0.027(5) 0.015(7) 0.007(4) -0.004(6) -0.013(5) C12 0.022(9) 0.017(4) 0.012(6) -0.001(3) -0.006(6) -0.006(4) C13 0.022(9) 0.013(4) 0.034(8) -0.001(4) 0.018(6) -0.005(4) C14 0.024(10) 0.029(5) 0.008(7) -0.001(3) -0.006(6) -0.010(5) C15 0.007(9) 0.015(4) 0.028(7) 0.001(3) 0.004(6) -0.001(4) C16 0.020(9) 0.011(4) 0.020(7) 0.002(3) 0.006(6) 0.000(4) C17 0.031(10) 0.011(4) 0.018(7) 0.001(3) 0.010(6) -0.002(4) C18 0.030(10) 0.015(4) 0.008(6) 0.006(3) -0.004(6) -0.001(4) C19 0.005(9) 0.015(4) 0.017(6) 0.001(3) 0.005(5) 0.002(4) C20 0.023(9) 0.010(4) 0.010(6) -0.003(3) 0.002(5) 0.003(4) C21 0.034(11) 0.012(4) 0.012(6) -0.006(3) 0.002(6) 0.004(4) C22 0.007(9) 0.020(5) 0.015(6) 0.003(3) 0.003(6) 0.006(4) F1 0.021(5) 0.014(3) 0.025(4) 0.000(2) 0.002(3) -0.005(2) F2 0.012(5) 0.024(3) 0.021(4) 0.002(2) -0.004(3) 0.003(3) Co2 0.0132(11) 0.0115(5) 0.0101(7) -0.0018(4) 0.0011(6) -0.0014(5) Br3 0.0108(9) 0.0185(5) 0.0202(6) 0.0000(3) -0.0004(5) -0.0018(4) Br4 0.0106(8) 0.0169(4) 0.0191(6) -0.0011(3) 0.0016(5) -0.0029(4) N5 0.026(8) 0.018(4) 0.024(7) -0.007(3) 0.004(5) 0.006(4) N6 0.021(7) 0.008(3) 0.013(5) -0.002(2) 0.007(5) 0.001(3) N7 0.011(7) 0.009(4) 0.020(6) 0.000(3) 0.000(5) 0.001(3) N8 0.010(7) 0.016(4) 0.015(6) -0.001(3) 0.002(5) -0.001(3) O5 0.014(6) 0.008(3) 0.021(5) -0.003(2) 0.004(4) 0.001(3) O7 0.030(7) 0.013(3) 0.033(6) 0.001(3) 0.014(4) -0.003(3) O6 0.020(7) 0.018(3) 0.023(5) -0.004(3) -0.004(4) 0.007(3) O8 0.062(8) 0.021(4) 0.034(6) 0.001(3) -0.003(5) 0.012(4) C23 0.025(9) 0.014(5) 0.024(7) -0.008(4) -0.005(6) 0.004(4) C24 0.011(9) 0.030(5) 0.011(7) -0.001(4) 0.007(6) 0.005(4) C27 0.014(9) 0.013(4) 0.011(5) 0.007(3) -0.003(5) 0.005(4) C28 0.019(9) 0.014(4) 0.010(6) 0.004(3) 0.004(5) 0.004(4) C29 0.038(12) 0.027(6) 0.013(7) -0.004(4) -0.006(6) 0.008(5) C30 0.026(10) 0.014(4) 0.018(7) 0.003(3) 0.004(6) 0.008(4) C31 0.005(8) 0.024(5) 0.018(6) 0.003(4) 0.004(5) 0.002(4) C32 0.044(12) 0.037(6) 0.021(8) -0.022(5) -0.007(7) 0.014(6) C33 0.019(9) 0.031(5) 0.007(6) -0.002(3) -0.002(6) -0.006(4) C34 0.007(9) 0.024(5) 0.008(6) 0.001(3) 0.001(5) 0.003(4) C35 0.056(13) 0.028(6) 0.028(9) -0.005(4) -0.006(8) 0.019(6) C36 0.041(11) 0.009(4) 0.034(8) 0.004(4) 0.022(7) 0.000(4) C37 0.024(10) 0.014(4) 0.030(8) -0.001(4) -0.019(7) -0.003(4) C38 0.019(9) 0.016(5) 0.023(7) -0.004(4) 0.007(6) 0.003(4) C39 0.040(11) 0.017(5) 0.018(7) 0.001(4) 0.003(6) 0.006(5) C40 0.040(12) 0.037(6) 0.008(7) 0.001(4) -0.011(7) 0.015(5) C42 0.057(13) 0.016(5) 0.032(9) 0.006(4) -0.004(8) -0.008(5) B2 0.031(12) 0.023(5) 0.003(6) -0.002(4) -0.001(6) 0.015(5) F3 0.013(5) 0.022(3) 0.023(4) 0.000(2) 0.006(3) 0.001(2) F4 0.027(5) 0.014(3) 0.029(4) -0.002(2) -0.001(4) 0.000(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 N2 1.893(8) . ? Co1 N3 1.905(9) . ? Co1 N4 1.959(9) . ? Co1 N1 1.969(8) . ? Co1 Br1 2.382(2) . ? Co1 Br2 2.389(2) . ? N1 C3 1.293(13) . ? N1 C8 1.458(12) . ? N2 C2 1.265(13) . ? N2 O2 1.369(9) . ? N3 C4 1.284(13) . ? N3 O1 1.349(9) . ? N4 C1 1.276(14) . ? N4 C6 1.453(11) . ? O1 B1 1.480(14) . ? O2 B1 1.475(15) . ? O3 C5 1.363(11) . ? O3 C14 1.421(14) . ? O4 C7 1.375(12) . ? O4 C13 1.446(13) . ? C1 C2 1.458(12) . ? C1 C10 1.494(15) . ? C2 C11 1.482(14) . ? C3 C4 1.476(13) . ? C3 C9 1.500(14) . ? C4 C12 1.467(13) . ? C5 C15 1.386(17) . ? C5 C18 1.400(16) . ? C6 C19 1.380(15) . ? C6 C20 1.383(16) . ? C7 C21 1.347(17) . ? C7 C16 1.404(14) . ? C8 C17 1.356(17) . ? C8 C22 1.366(15) . ? C15 C19 1.393(12) . ? C16 C17 1.401(13) . ? C18 C20 1.395(12) . ? C21 C22 1.392(14) . ? B1 F2 1.351(15) . ? B1 F1 1.380(11) . ? Co2 N5 1.898(9) . ? Co2 N6 1.913(9) . ? Co2 N7 1.963(9) . ? Co2 N8 1.972(9) . ? Co2 Br4 2.382(2) . ? Co2 Br3 2.386(2) . ? N5 C23 1.287(15) . ? N5 O6 1.353(10) . ? N6 C25 1.284(13) . ? N6 O5 1.351(9) . ? N7 C26 1.297(13) . ? N7 C28 1.442(11) . ? N8 C24 1.295(14) . ? N8 C30 1.445(11) . ? O5 B2 1.479(14) . ? O7 C27 1.374(12) . ? O7 C36 1.418(12) . ? O6 B2 1.465(16) . ? O8 C29 1.369(13) . ? O8 C35 1.387(17) . ? C23 C32 1.467(14) . ? C23 C24 1.497(14) . ? C24 C33 1.495(16) . ? C25 C26 1.471(13) . ? C25 C31 1.493(14) . ? C26 C34 1.469(14) . ? C27 C43 1.355(16) . ? C27 C41 1.411(14) . ? C28 C44 1.372(17) . ? C28 C38 1.383(15) . ? C29 C42 1.367(19) . ? C29 C40 1.40(2) . ? C30 C37 1.356(18) . ? C30 C39 1.409(17) . ? C37 C40 1.390(14) . ? C38 C43 1.384(13) . ? C39 C42 1.393(14) . ? C41 C44 1.376(12) . ? B2 F4 1.370(12) . ? B2 F3 1.382(17) . ? 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 N2 Co1 N3 94.6(4) . . ? N2 Co1 N4 79.9(4) . . ? N3 Co1 N4 174.4(4) . . ? N2 Co1 N1 173.2(4) . . ? N3 Co1 N1 80.9(4) . . ? N4 Co1 N1 104.7(3) . . ? N2 Co1 Br1 94.9(3) . . ? N3 Co1 Br1 92.0(3) . . ? N4 Co1 Br1 87.7(3) . . ? N1 Co1 Br1 90.3(3) . . ? N2 Co1 Br2 87.2(3) . . ? N3 Co1 Br2 89.7(3) . . ? N4 Co1 Br2 90.8(3) . . ? N1 Co1 Br2 87.7(3) . . ? Br1 Co1 Br2 177.16(6) . . ? C3 N1 C8 117.0(8) . . ? C3 N1 Co1 113.3(6) . . ? C8 N1 Co1 129.4(7) . . ? C2 N2 O2 116.6(8) . . ? C2 N2 Co1 118.4(6) . . ? O2 N2 Co1 124.0(6) . . ? C4 N3 O1 115.7(8) . . ? C4 N3 Co1 118.3(6) . . ? O1 N3 Co1 125.9(7) . . ? C1 N4 C6 118.1(9) . . ? C1 N4 Co1 114.1(7) . . ? C6 N4 Co1 127.8(7) . . ? N3 O1 B1 118.3(7) . . ? N2 O2 B1 116.4(7) . . ? C5 O3 C14 116.8(8) . . ? C7 O4 C13 116.1(10) . . ? N4 C1 C2 115.0(9) . . ? N4 C1 C10 124.4(8) . . ? C2 C1 C10 120.5(9) . . ? N2 C2 C1 112.0(9) . . ? N2 C2 C11 125.3(9) . . ? C1 C2 C11 122.6(9) . . ? N1 C3 C4 115.7(9) . . ? N1 C3 C9 125.7(9) . . ? C4 C3 C9 118.3(9) . . ? N3 C4 C12 125.2(9) . . ? N3 C4 C3 111.7(8) . . ? C12 C4 C3 123.0(9) . . ? O3 C5 C15 114.5(9) . . ? O3 C5 C18 124.0(10) . . ? C15 C5 C18 121.6(9) . . ? C19 C6 C20 120.9(9) . . ? C19 C6 N4 119.1(10) . . ? C20 C6 N4 119.9(9) . . ? C21 C7 O4 124.7(9) . . ? C21 C7 C16 121.0(9) . . ? O4 C7 C16 114.3(11) . . ? C17 C8 C22 122.4(9) . . ? C17 C8 N1 118.9(9) . . ? C22 C8 N1 118.6(12) . . ? C5 C15 C19 119.9(10) . . ? C17 C16 C7 117.4(12) . . ? C8 C17 C16 120.2(10) . . ? C20 C18 C5 117.3(11) . . ? C6 C19 C15 119.0(11) . . ? C6 C20 C18 121.3(10) . . ? C7 C21 C22 121.3(10) . . ? C8 C22 C21 117.8(12) . . ? F2 B1 F1 112.9(10) . . ? F2 B1 O2 111.9(9) . . ? F1 B1 O2 105.0(8) . . ? F2 B1 O1 110.4(9) . . ? F1 B1 O1 105.6(8) . . ? O2 B1 O1 110.7(10) . . ? N5 Co2 N6 94.3(4) . . ? N5 Co2 N7 174.1(4) . . ? N6 Co2 N7 80.2(3) . . ? N5 Co2 N8 80.3(4) . . ? N6 Co2 N8 174.5(3) . . ? N7 Co2 N8 105.2(3) . . ? N5 Co2 Br4 93.8(4) . . ? N6 Co2 Br4 93.1(3) . . ? N7 Co2 Br4 88.6(3) . . ? N8 Co2 Br4 88.0(3) . . ? N5 Co2 Br3 89.1(4) . . ? N6 Co2 Br3 90.3(3) . . ? N7 Co2 Br3 88.8(3) . . ? N8 Co2 Br3 89.0(3) . . ? Br4 Co2 Br3 175.40(7) . . ? C23 N5 O6 114.4(8) . . ? C23 N5 Co2 119.5(7) . . ? O6 N5 Co2 125.3(8) . . ? C25 N6 O5 115.6(8) . . ? C25 N6 Co2 118.6(7) . . ? O5 N6 Co2 125.2(6) . . ? C26 N7 C28 117.4(9) . . ? C26 N7 Co2 114.4(6) . . ? C28 N7 Co2 128.0(7) . . ? C24 N8 C30 116.5(9) . . ? C24 N8 Co2 114.5(7) . . ? C30 N8 Co2 128.9(7) . . ? N6 O5 B2 118.1(7) . . ? C27 O7 C36 115.8(10) . . ? N5 O6 B2 117.5(8) . . ? C29 O8 C35 118.6(11) . . ? N5 C23 C32 125.1(10) . . ? N5 C23 C24 111.0(9) . . ? C32 C23 C24 123.8(11) . . ? N8 C24 C33 127.1(9) . . ? N8 C24 C23 114.6(10) . . ? C33 C24 C23 118.4(9) . . ? N6 C25 C26 111.7(9) . . ? N6 C25 C31 126.2(9) . . ? C26 C25 C31 121.8(9) . . ? N7 C26 C34 125.6(8) . . ? N7 C26 C25 115.0(8) . . ? C34 C26 C25 119.3(8) . . ? C43 C27 O7 125.5(9) . . ? C43 C27 C41 120.2(9) . . ? O7 C27 C41 114.1(10) . . ? C44 C28 C38 121.1(9) . . ? C44 C28 N7 118.9(9) . . ? C38 C28 N7 120.0(11) . . ? C42 C29 O8 115.1(12) . . ? C42 C29 C40 121.3(11) . . ? O8 C29 C40 123.6(12) . . ? C37 C30 C39 121.8(9) . . ? C37 C30 N8 119.7(10) . . ? C39 C30 N8 118.4(10) . . ? C30 C37 C40 120.7(12) . . ? C28 C38 C43 119.5(12) . . ? C42 C39 C30 117.4(13) . . ? C37 C40 C29 117.9(13) . . ? C44 C41 C27 119.6(11) . . ? C29 C42 C39 120.7(12) . . ? C27 C43 C38 120.1(10) . . ? C28 C44 C41 119.4(9) . . ? F4 B2 F3 112.3(10) . . ? F4 B2 O6 106.8(9) . . ? F3 B2 O6 110.8(10) . . ? F4 B2 O5 105.3(9) . . ? F3 B2 O5 109.4(10) . . ? O6 B2 O5 112.1(10) . . ? _diffrn_measured_fraction_theta_max 0.549 _diffrn_reflns_theta_full 30.14 _diffrn_measured_fraction_theta_full 0.549 _refine_diff_density_max 0.533 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.099 #===ENDw data_lab23a _database_code_depnum_ccdc_archive 'CCDC 735558' #TrackingRef 'Combined_cif_revision.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H41 Br2 Co N6 O8' _chemical_formula_weight 832.4 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' Br Br -0.2901 2.4595 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.774(2) _cell_length_b 12.7834(13) _cell_length_c 14.289(2) _cell_angle_alpha 90.00 _cell_angle_beta 116.198(2) _cell_angle_gamma 90.00 _cell_volume 3404.8(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 2.909 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.422 _exptl_absorpt_correction_T_max 0.483 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39442 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 31.59 _reflns_number_total 5475 _reflns_number_gt 4378 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1000P)^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 5475 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0792 _refine_ls_goodness_of_fit_ref 0.626 _refine_ls_restrained_S_all 0.626 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.420920(8) 0.526857(11) 0.330131(11) 0.01630(6) Uani 1 1 d . . . Co1 Co 0.5000 0.529029(19) 0.2500 0.01073(7) Uani 1 2 d S . . O1 O 0.45375(6) 0.73262(8) 0.16133(9) 0.0198(2) Uani 1 1 d . . . O3 O 0.38679(6) -0.05364(9) -0.07363(9) 0.0204(2) Uani 1 1 d . . . H3 H 0.3502 -0.0761 -0.1249 0.031 Uiso 1 1 d R . . O5 O 0.31639(6) -0.06892(9) 0.00758(9) 0.0213(2) Uani 1 1 d . . . N1 N 0.44130(6) 0.63014(9) 0.14996(9) 0.0143(2) Uani 1 1 d . . . N2 N 0.43358(6) 0.43473(9) 0.13994(9) 0.0122(2) Uani 1 1 d . . . C1 C 0.38704(7) 0.59662(11) 0.06648(11) 0.0147(3) Uani 1 1 d . . . C2 C 0.38229(8) 0.48298(11) 0.06351(11) 0.0133(3) Uani 1 1 d . . . C5 C 0.33773(8) 0.66641(13) -0.01837(12) 0.0223(3) Uani 1 1 d . . . H5A H 0.3389 0.7367 0.0096 0.033 Uiso 1 1 calc R . . H5B H 0.2888 0.6387 -0.0465 0.033 Uiso 1 1 calc R . . H5C H 0.3531 0.6697 -0.0740 0.033 Uiso 1 1 calc R . . C6 C 0.31975(7) 0.43173(12) -0.02344(11) 0.0169(3) Uani 1 1 d . . . H6A H 0.3224 0.3559 -0.0124 0.025 Uiso 1 1 calc R . . H6B H 0.3208 0.4472 -0.0899 0.025 Uiso 1 1 calc R . . H6C H 0.2751 0.4585 -0.0251 0.025 Uiso 1 1 calc R . . C9 C 0.40966(7) 0.26040(11) 0.18863(11) 0.0140(3) Uani 1 1 d . . . H9 H 0.3916 0.2912 0.2327 0.017 Uiso 1 1 calc R . . C10 C 0.40971(7) 0.15222(11) 0.17806(11) 0.0145(3) Uani 1 1 d . . . H10 H 0.3906 0.1093 0.2139 0.017 Uiso 1 1 calc R . . C11 C 0.46464(8) 0.17019(11) 0.06182(11) 0.0155(3) Uani 1 1 d . . . H11 H 0.4841 0.1394 0.0194 0.019 Uiso 1 1 calc R . . C12 C 0.46339(7) 0.27856(11) 0.07005(11) 0.0144(3) Uani 1 1 d . . . H12 H 0.4809 0.3218 0.0323 0.017 Uiso 1 1 calc R . . C17 C 0.43759(7) 0.10625(11) 0.11532(11) 0.0143(3) Uani 1 1 d . . . C19 C 0.43876(9) -0.01197(11) 0.10612(13) 0.0182(3) Uani 1 1 d . . . H19A H 0.4832 -0.0338 0.1022 0.022 Uiso 1 1 calc R . . H19B H 0.4384 -0.0447 0.1687 0.022 Uiso 1 1 calc R . . C21 C 0.37397(8) -0.04838(11) 0.00930(12) 0.0158(3) Uani 1 1 d . . . C23 C 0.43619(7) 0.32283(11) 0.13428(11) 0.0122(2) Uani 1 1 d . . . O7 O 0.28786(6) 0.14756(9) 0.26800(9) 0.0223(2) Uani 1 1 d . . . N5 N 0.20741(7) 0.28101(11) 0.22350(10) 0.0180(3) Uani 1 1 d . . . C40 C 0.23867(8) 0.19492(12) 0.27656(11) 0.0180(3) Uani 1 1 d . . . H40 H 0.2222 0.1680 0.3241 0.022 Uiso 1 1 calc R . . C41 C 0.15131(9) 0.33425(16) 0.23988(14) 0.0293(4) Uani 1 1 d . . . H41A H 0.1424 0.2968 0.2928 0.044 Uiso 1 1 calc R . . H41B H 0.1072 0.3359 0.1743 0.044 Uiso 1 1 calc R . . H41C H 0.1665 0.4060 0.2636 0.044 Uiso 1 1 calc R . . C42 C 0.22986(9) 0.32842(13) 0.15001(13) 0.0226(3) Uani 1 1 d . . . H42A H 0.2533 0.3956 0.1777 0.034 Uiso 1 1 calc R . . H42B H 0.1878 0.3399 0.0832 0.034 Uiso 1 1 calc R . . H42C H 0.2636 0.2817 0.1397 0.034 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.01684(9) 0.01763(9) 0.01567(9) -0.00109(5) 0.00831(6) 0.00165(5) Co1 0.01196(13) 0.00818(13) 0.01020(13) 0.000 0.00321(10) 0.000 O1 0.0244(5) 0.0071(4) 0.0214(5) 0.0013(4) 0.0043(4) -0.0001(4) O3 0.0176(5) 0.0239(6) 0.0181(5) -0.0055(4) 0.0065(4) -0.0043(4) O5 0.0195(5) 0.0209(6) 0.0237(6) -0.0037(5) 0.0097(5) -0.0015(4) N1 0.0167(6) 0.0095(5) 0.0151(6) 0.0010(4) 0.0057(5) 0.0011(4) N2 0.0133(5) 0.0104(5) 0.0122(5) -0.0008(4) 0.0049(4) -0.0002(4) C1 0.0162(6) 0.0124(6) 0.0128(6) 0.0024(5) 0.0040(5) 0.0022(5) C2 0.0134(6) 0.0136(6) 0.0120(6) -0.0008(5) 0.0048(5) 0.0004(5) C5 0.0232(7) 0.0176(7) 0.0180(7) 0.0041(6) 0.0016(6) 0.0035(6) C6 0.0151(6) 0.0170(7) 0.0130(6) -0.0014(5) 0.0011(5) 0.0005(5) C9 0.0133(6) 0.0138(6) 0.0146(6) -0.0020(5) 0.0059(5) -0.0001(5) C10 0.0137(6) 0.0133(6) 0.0147(6) 0.0004(5) 0.0047(5) -0.0012(5) C11 0.0158(6) 0.0160(7) 0.0129(6) -0.0026(5) 0.0046(5) 0.0018(5) C12 0.0151(6) 0.0150(6) 0.0123(6) 0.0004(5) 0.0055(5) 0.0003(5) C17 0.0128(6) 0.0116(6) 0.0140(6) -0.0014(5) 0.0020(5) 0.0008(5) C19 0.0194(7) 0.0104(6) 0.0184(7) -0.0020(5) 0.0025(6) 0.0019(5) C21 0.0179(6) 0.0079(6) 0.0190(7) -0.0006(5) 0.0056(6) 0.0016(5) C23 0.0114(6) 0.0104(6) 0.0117(6) -0.0013(5) 0.0024(5) -0.0003(5) O7 0.0239(6) 0.0244(6) 0.0153(5) 0.0029(4) 0.0058(4) 0.0057(5) N5 0.0154(6) 0.0216(6) 0.0148(6) 0.0000(5) 0.0048(5) 0.0007(5) C40 0.0181(6) 0.0202(7) 0.0120(6) -0.0021(5) 0.0034(5) -0.0033(6) C41 0.0270(8) 0.0372(10) 0.0258(9) 0.0047(7) 0.0133(7) 0.0118(7) C42 0.0215(7) 0.0245(8) 0.0213(8) 0.0056(6) 0.0089(6) 0.0015(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Co1 2.3815(2) . ? Co1 N1 1.9136(12) 2_655 ? Co1 N1 1.9136(12) . ? Co1 N2 1.9784(12) . ? Co1 N2 1.9784(12) 2_655 ? Co1 Br1 2.3815(2) 2_655 ? O1 N1 1.3312(15) . ? O3 C21 1.3259(19) . ? O3 H3 0.8399 . ? O5 C21 1.2142(18) . ? N1 C1 1.3000(18) . ? N2 C2 1.2965(18) . ? N2 C23 1.4351(18) . ? C1 C2 1.455(2) . ? C1 C5 1.4894(19) . ? C2 C6 1.4952(19) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C9 C23 1.3861(19) . ? C9 C10 1.391(2) . ? C9 H9 0.9500 . ? C10 C17 1.394(2) . ? C10 H10 0.9500 . ? C11 C12 1.391(2) . ? C11 C17 1.396(2) . ? C11 H11 0.9500 . ? C12 C23 1.3928(19) . ? C12 H12 0.9500 . ? C17 C19 1.518(2) . ? C19 C21 1.516(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? O7 C40 1.2394(19) . ? N5 C40 1.332(2) . ? N5 C42 1.456(2) . ? N5 C41 1.455(2) . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 N1 95.02(7) 2_655 . ? N1 Co1 N2 174.95(5) 2_655 . ? N1 Co1 N2 80.04(5) . . ? N1 Co1 N2 80.04(5) 2_655 2_655 ? N1 Co1 N2 174.95(5) . 2_655 ? N2 Co1 N2 104.92(7) . 2_655 ? N1 Co1 Br1 91.13(4) 2_655 2_655 ? N1 Co1 Br1 89.77(4) . 2_655 ? N2 Co1 Br1 89.87(3) . 2_655 ? N2 Co1 Br1 89.31(3) 2_655 2_655 ? N1 Co1 Br1 89.77(4) 2_655 . ? N1 Co1 Br1 91.13(4) . . ? N2 Co1 Br1 89.31(3) . . ? N2 Co1 Br1 89.87(3) 2_655 . ? Br1 Co1 Br1 178.664(13) 2_655 . ? C21 O3 H3 109.5 . . ? C1 N1 O1 118.64(12) . . ? C1 N1 Co1 118.11(10) . . ? O1 N1 Co1 123.24(9) . . ? C2 N2 C23 117.65(12) . . ? C2 N2 Co1 113.90(10) . . ? C23 N2 Co1 128.44(9) . . ? N1 C1 C2 112.08(12) . . ? N1 C1 C5 123.75(13) . . ? C2 C1 C5 124.11(13) . . ? N2 C2 C1 115.49(12) . . ? N2 C2 C6 125.52(13) . . ? C1 C2 C6 118.97(12) . . ? C1 C5 H5A 109.5 . . ? C1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C2 C6 H6A 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C23 C9 C10 119.47(13) . . ? C23 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C17 120.63(13) . . ? C9 C10 H10 119.7 . . ? C17 C10 H10 119.7 . . ? C12 C11 C17 120.64(13) . . ? C12 C11 H11 119.7 . . ? C17 C11 H11 119.7 . . ? C11 C12 C23 119.24(13) . . ? C11 C12 H12 120.4 . . ? C23 C12 H12 120.4 . . ? C10 C17 C11 119.17(13) . . ? C10 C17 C19 120.17(13) . . ? C11 C17 C19 120.65(13) . . ? C21 C19 C17 110.06(12) . . ? C21 C19 H19A 109.6 . . ? C17 C19 H19A 109.6 . . ? C21 C19 H19B 109.6 . . ? C17 C19 H19B 109.6 . . ? H19A C19 H19B 108.2 . . ? O5 C21 O3 123.75(14) . . ? O5 C21 C19 123.68(15) . . ? O3 C21 C19 112.55(13) . . ? C9 C23 C12 120.83(13) . . ? C9 C23 N2 120.53(12) . . ? C12 C23 N2 118.59(12) . . ? C40 N5 C42 121.59(13) . . ? C40 N5 C41 121.26(14) . . ? C42 N5 C41 117.11(14) . . ? O7 C40 N5 124.30(15) . . ? O7 C40 H40 117.8 . . ? N5 C40 H40 117.8 . . ? N5 C41 H41A 109.5 . . ? N5 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 H42A 109.5 . . ? N5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 31.59 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.508 _refine_diff_density_min -0.394 _refine_diff_density_rms 0.078 #===END data_08119 _database_code_depnum_ccdc_archive 'CCDC 735559' #TrackingRef 'Combined_cif_revision.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32.25 H30 Br2 Co N4 O2.50' _chemical_formula_weight 732.35 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.4891(15) _cell_length_b 14.3245(17) _cell_length_c 17.501(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.195(2) _cell_angle_gamma 90.00 _cell_volume 3021.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1474 _exptl_absorpt_coefficient_mu 3.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3563 _exptl_absorpt_correction_T_max 0.4421 _exptl_absorpt_process_details 'Blessing, Acta. Cryst.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type APEX2 _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58638 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0421 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 29.57 _reflns_number_total 8481 _reflns_number_gt 6499 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.1000P)^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 8481 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0599 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1075 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19819(3) -0.06669(2) 0.22542(2) 0.01707(9) Uani 1 1 d . . . Br1 Br 0.33498(2) -0.13444(2) 0.333352(16) 0.02351(9) Uani 1 1 d . . . Br2 Br 0.05045(2) 0.01181(2) 0.132420(16) 0.02131(8) Uani 1 1 d . . . N1 N 0.23891(19) 0.05145(17) 0.27419(13) 0.0205(5) Uani 1 1 d . . . N2 N 0.30755(19) -0.02277(16) 0.16508(13) 0.0189(5) Uani 1 1 d . . . N3 N 0.09310(19) -0.09625(17) 0.28466(13) 0.0198(5) Uani 1 1 d . . . N4 N 0.15371(18) -0.19749(16) 0.18425(13) 0.0187(4) Uani 1 1 d . . . C1 C 0.3097(2) 0.10277(19) 0.25027(16) 0.0210(5) Uani 1 1 d . . . C2 C 0.3452(2) 0.06065(19) 0.18561(16) 0.0200(5) Uani 1 1 d . . . C3 C 0.0898(2) -0.23803(19) 0.22201(15) 0.0196(5) Uani 1 1 d . . . C4 C 0.0489(2) -0.1783(2) 0.27636(16) 0.0202(5) Uani 1 1 d . . . C5 C 0.3444(3) 0.1965(2) 0.2852(2) 0.0300(7) Uani 1 1 d . . . H5A H 0.2878 0.2427 0.2611 0.045 Uiso 1 1 calc R . . H5B H 0.4152 0.2139 0.2750 0.045 Uiso 1 1 calc R . . H5C H 0.3529 0.1943 0.3425 0.045 Uiso 1 1 calc R . . C6 C -0.0320(3) -0.2109(2) 0.32099(18) 0.0271(6) Uani 1 1 d . . . H6A H 0.0051 -0.2550 0.3624 0.041 Uiso 1 1 calc R . . H6B H -0.0948 -0.2419 0.2844 0.041 Uiso 1 1 calc R . . H6C H -0.0588 -0.1572 0.3453 0.041 Uiso 1 1 calc R . . C7 C 0.0590(3) -0.3383(2) 0.21901(17) 0.0248(6) Uani 1 1 d . . . H7A H -0.0198 -0.3453 0.1917 0.037 Uiso 1 1 calc R . . H7B H 0.0728 -0.3628 0.2730 0.037 Uiso 1 1 calc R . . H7C H 0.1038 -0.3731 0.1903 0.037 Uiso 1 1 calc R . . C8 C 0.4187(2) 0.1166(2) 0.14757(19) 0.0256(6) Uani 1 1 d . . . H8A H 0.4937 0.1190 0.1830 0.038 Uiso 1 1 calc R . . H8B H 0.3892 0.1801 0.1373 0.038 Uiso 1 1 calc R . . H8C H 0.4211 0.0872 0.0975 0.038 Uiso 1 1 calc R . . C9 C 0.3350(2) -0.06827(19) 0.09857(16) 0.0203(5) Uani 1 1 d . . . C10 C 0.1960(2) -0.2556(2) 0.13120(16) 0.0209(5) Uani 1 1 d . . . C11 C 0.1259(2) -0.2980(2) 0.06404(16) 0.0227(6) Uani 1 1 d . . . C12 C 0.4444(2) -0.0931(2) 0.09783(17) 0.0229(6) Uani 1 1 d . . . C13 C 0.0029(2) -0.2886(2) 0.03945(15) 0.0221(6) Uani 1 1 d . . . C14 C 0.5461(2) -0.07419(19) 0.16205(18) 0.0224(6) Uani 1 1 d . . . C15 C -0.2288(3) -0.2776(3) -0.0080(2) 0.0364(8) Uani 1 1 d . . . H15 H -0.3075 -0.2739 -0.0235 0.044 Uiso 1 1 calc R . . C16 C -0.1656(3) -0.1971(3) 0.0060(2) 0.0363(8) Uani 1 1 d . . . H16 H -0.2012 -0.1379 -0.0003 0.044 Uiso 1 1 calc R . . C17 C 0.3564(3) -0.3321(2) 0.10614(19) 0.0270(6) Uani 1 1 d . . . H17 H 0.4340 -0.3437 0.1207 0.032 Uiso 1 1 calc R . . C18 C 0.2886(3) -0.3742(2) 0.03869(19) 0.0283(7) Uani 1 1 d . . . H18 H 0.3197 -0.4143 0.0069 0.034 Uiso 1 1 calc R . . C19 C 0.2615(3) -0.1312(2) -0.03295(18) 0.0295(7) Uani 1 1 d . . . H19 H 0.2004 -0.1431 -0.0772 0.035 Uiso 1 1 calc R . . C20 C 0.2450(3) -0.0865(2) 0.03345(16) 0.0243(6) Uani 1 1 d . . . H20 H 0.1724 -0.0682 0.0347 0.029 Uiso 1 1 calc R . . C21 C 0.4564(3) -0.1389(2) 0.02970(19) 0.0275(6) Uani 1 1 d . . . H21 H 0.5286 -0.1573 0.0274 0.033 Uiso 1 1 calc R . . C22 C 0.1758(3) -0.3569(2) 0.01870(18) 0.0270(6) Uani 1 1 d . . . H22 H 0.1302 -0.3856 -0.0273 0.032 Uiso 1 1 calc R . . C23 C 0.3102(2) -0.2731(2) 0.15208(17) 0.0234(6) Uani 1 1 d . . . H23 H 0.3565 -0.2446 0.1979 0.028 Uiso 1 1 calc R . . C24 C 0.3672(3) -0.1585(2) -0.03452(19) 0.0322(7) Uani 1 1 d . . . H24 H 0.3786 -0.1905 -0.0793 0.039 Uiso 1 1 calc R . . C25 C -0.0617(3) -0.3696(2) 0.02412(17) 0.0269(6) Uani 1 1 d . . . H25 H -0.0266 -0.4290 0.0298 0.032 Uiso 1 1 calc R . . C26 C -0.0503(3) -0.2021(2) 0.02943(18) 0.0294(7) Uani 1 1 d . . . H26 H -0.0076 -0.1463 0.0386 0.035 Uiso 1 1 calc R . . C27 C -0.1765(3) -0.3640(2) 0.00079(18) 0.0318(7) Uani 1 1 d . . . H27 H -0.2196 -0.4195 -0.0092 0.038 Uiso 1 1 calc R . . C28 C 0.7418(3) -0.0390(2) 0.2815(2) 0.0348(7) Uani 1 1 d . . . H28 H 0.8076 -0.0263 0.3218 0.042 Uiso 1 1 calc R . . C29 C 0.6453(3) -0.0486(2) 0.1436(2) 0.0291(6) Uani 1 1 d . . . H29 H 0.6460 -0.0419 0.0897 0.035 Uiso 1 1 calc R . . C30 C 0.5486(2) -0.0820(2) 0.24225(18) 0.0249(6) Uani 1 1 d . . . H30 H 0.4833 -0.0999 0.2567 0.030 Uiso 1 1 calc R . . C31 C 0.6454(3) -0.0637(2) 0.3011(2) 0.0307(7) Uani 1 1 d . . . H31 H 0.6453 -0.0683 0.3552 0.037 Uiso 1 1 calc R . . C32 C 0.7419(3) -0.0330(2) 0.2025(2) 0.0363(8) Uani 1 1 d . . . H32 H 0.8086 -0.0181 0.1888 0.044 Uiso 1 1 calc R . . O1 O 0.19953(18) 0.08368(15) 0.33224(12) 0.0264(4) Uani 1 1 d . . . O2 O 0.06565(17) -0.03682(15) 0.33478(12) 0.0250(4) Uani 1 1 d . . . O3 O 0.5460(11) -0.3779(10) -0.0019(8) 0.062(3) Uiso 0.25 1 d P . . C50 C 0.5486(10) -0.4408(10) 0.0129(8) 0.029(3) Uiso 0.25 1 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 0.02474(19) 0.01482(19) 0.01289(17) 0.00034(13) 0.00717(14) -0.00038(13) Br1 0.02929(16) 0.02650(16) 0.01544(14) 0.00475(10) 0.00710(11) 0.00358(11) Br2 0.02703(15) 0.01900(15) 0.01765(14) 0.00165(10) 0.00540(11) 0.00129(10) N1 0.0277(11) 0.0177(11) 0.0163(11) -0.0015(9) 0.0059(9) 0.0024(9) N2 0.0243(11) 0.0185(12) 0.0145(10) 0.0010(9) 0.0060(9) -0.0020(9) N3 0.0264(11) 0.0202(12) 0.0144(10) 0.0004(9) 0.0083(9) 0.0025(9) N4 0.0260(11) 0.0180(11) 0.0137(10) 0.0018(9) 0.0078(9) 0.0011(9) C1 0.0273(13) 0.0156(13) 0.0191(13) -0.0004(10) 0.0041(10) 0.0020(10) C2 0.0234(13) 0.0174(13) 0.0191(13) 0.0040(10) 0.0050(10) 0.0000(10) C3 0.0254(13) 0.0191(13) 0.0145(12) 0.0021(10) 0.0057(10) -0.0003(10) C4 0.0258(13) 0.0200(14) 0.0165(12) 0.0031(10) 0.0084(10) 0.0048(10) C5 0.0318(15) 0.0218(15) 0.0353(17) -0.0088(13) 0.0071(13) -0.0034(12) C6 0.0317(15) 0.0281(16) 0.0258(15) 0.0003(12) 0.0154(12) -0.0005(12) C7 0.0362(15) 0.0198(14) 0.0208(13) 0.0005(11) 0.0118(12) -0.0051(12) C8 0.0286(14) 0.0199(14) 0.0290(15) 0.0054(12) 0.0089(12) -0.0038(11) C9 0.0313(14) 0.0168(13) 0.0152(12) 0.0012(10) 0.0102(10) -0.0052(10) C10 0.0352(15) 0.0159(13) 0.0155(12) 0.0002(10) 0.0134(11) -0.0033(11) C11 0.0351(15) 0.0192(14) 0.0161(12) 0.0005(10) 0.0109(11) -0.0065(11) C12 0.0353(15) 0.0177(13) 0.0196(13) 0.0008(11) 0.0143(11) -0.0036(11) C13 0.0330(14) 0.0227(14) 0.0117(12) -0.0007(10) 0.0079(10) -0.0041(11) C14 0.0294(14) 0.0152(13) 0.0252(14) 0.0007(11) 0.0116(11) -0.0002(10) C15 0.0356(17) 0.038(2) 0.0304(17) 0.0035(14) -0.0006(14) -0.0036(14) C16 0.0388(17) 0.0305(18) 0.0343(18) 0.0045(14) 0.0004(14) 0.0030(14) C17 0.0322(15) 0.0252(15) 0.0289(15) -0.0004(12) 0.0174(12) -0.0025(12) C18 0.0432(18) 0.0202(15) 0.0279(15) -0.0020(12) 0.0206(13) -0.0043(12) C19 0.0437(18) 0.0303(17) 0.0159(13) -0.0022(11) 0.0105(12) -0.0154(13) C20 0.0355(15) 0.0240(15) 0.0158(12) -0.0027(11) 0.0108(11) -0.0110(12) C21 0.0406(17) 0.0214(15) 0.0276(15) -0.0019(12) 0.0214(13) -0.0050(12) C22 0.0427(17) 0.0225(15) 0.0207(14) -0.0032(11) 0.0169(12) -0.0077(12) C23 0.0307(14) 0.0219(14) 0.0208(13) -0.0006(11) 0.0124(11) -0.0037(11) C24 0.054(2) 0.0253(16) 0.0239(15) -0.0040(13) 0.0228(14) -0.0114(14) C25 0.0405(17) 0.0216(15) 0.0196(14) -0.0015(11) 0.0095(12) -0.0055(12) C26 0.0389(16) 0.0228(15) 0.0238(15) 0.0002(12) 0.0033(12) -0.0035(12) C27 0.0419(18) 0.0296(17) 0.0208(14) 0.0017(12) 0.0024(13) -0.0077(13) C28 0.0285(15) 0.0275(17) 0.044(2) 0.0019(15) 0.0024(14) -0.0004(13) C29 0.0342(16) 0.0207(14) 0.0367(17) 0.0018(13) 0.0170(13) -0.0021(12) C30 0.0286(14) 0.0203(14) 0.0268(15) 0.0014(11) 0.0088(12) 0.0040(11) C31 0.0355(16) 0.0267(17) 0.0282(16) -0.0008(13) 0.0052(13) 0.0043(12) C32 0.0306(16) 0.0285(17) 0.052(2) 0.0012(15) 0.0152(15) -0.0040(13) O1 0.0360(11) 0.0246(11) 0.0217(10) -0.0070(8) 0.0132(9) 0.0011(9) O2 0.0375(11) 0.0223(10) 0.0207(10) -0.0029(8) 0.0178(9) 0.0028(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 N1 1.904(2) . ? Co1 N3 1.921(2) . ? Co1 N4 2.032(2) . ? Co1 N2 2.033(2) . ? Co1 Br1 2.3951(5) . ? Co1 Br2 2.3967(5) . ? N1 C1 1.301(4) . ? N1 O1 1.323(3) . ? N2 C2 1.300(4) . ? N2 C9 1.451(3) . ? N3 C4 1.290(4) . ? N3 O2 1.330(3) . ? N4 C3 1.300(3) . ? N4 C10 1.446(3) . ? C1 C2 1.450(4) . ? C1 C5 1.491(4) . ? C2 C8 1.499(4) . ? C3 C4 1.467(4) . ? C3 C7 1.485(4) . ? C4 C6 1.504(4) . ? C9 C20 1.399(4) . ? C9 C12 1.415(4) . ? C10 C23 1.399(4) . ? C10 C11 1.406(4) . ? C11 C22 1.410(4) . ? C11 C13 1.489(4) . ? C12 C21 1.403(4) . ? C12 C14 1.483(4) . ? C13 C26 1.396(4) . ? C13 C25 1.399(4) . ? C14 C30 1.400(4) . ? C14 C29 1.409(4) . ? C15 C16 1.383(5) . ? C15 C27 1.389(5) . ? C16 C26 1.392(5) . ? C17 C23 1.392(4) . ? C17 C18 1.397(4) . ? C18 C22 1.382(5) . ? C19 C24 1.383(5) . ? C19 C20 1.389(4) . ? C21 C24 1.388(5) . ? C25 C27 1.386(5) . ? C28 C32 1.384(5) . ? C28 C31 1.382(5) . ? C29 C32 1.385(5) . ? C30 C31 1.393(4) . ? O3 C50 0.935(16) . ? 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 N3 95.39(10) . . ? N1 Co1 N4 174.20(9) . . ? N3 Co1 N4 79.99(10) . . ? N1 Co1 N2 79.68(10) . . ? N3 Co1 N2 174.69(10) . . ? N4 Co1 N2 105.05(9) . . ? N1 Co1 Br1 87.42(7) . . ? N3 Co1 Br1 86.10(7) . . ? N4 Co1 Br1 88.76(6) . . ? N2 Co1 Br1 95.61(7) . . ? N1 Co1 Br2 87.42(7) . . ? N3 Co1 Br2 87.51(7) . . ? N4 Co1 Br2 95.83(6) . . ? N2 Co1 Br2 90.26(7) . . ? Br1 Co1 Br2 171.383(19) . . ? C1 N1 O1 118.1(2) . . ? C1 N1 Co1 118.84(19) . . ? O1 N1 Co1 123.05(18) . . ? C2 N2 C9 119.3(2) . . ? C2 N2 Co1 112.62(19) . . ? C9 N2 Co1 127.57(18) . . ? C4 N3 O2 118.7(2) . . ? C4 N3 Co1 118.23(19) . . ? O2 N3 Co1 123.06(18) . . ? C3 N4 C10 116.5(2) . . ? C3 N4 Co1 112.28(19) . . ? C10 N4 Co1 130.29(18) . . ? N1 C1 C2 112.9(2) . . ? N1 C1 C5 121.7(3) . . ? C2 C1 C5 125.4(3) . . ? N2 C2 C1 115.8(2) . . ? N2 C2 C8 126.0(3) . . ? C1 C2 C8 118.2(2) . . ? N4 C3 C4 115.7(2) . . ? N4 C3 C7 127.0(3) . . ? C4 C3 C7 117.2(2) . . ? N3 C4 C3 113.1(2) . . ? N3 C4 C6 123.4(2) . . ? C3 C4 C6 123.4(3) . . ? C20 C9 C12 121.1(3) . . ? C20 C9 N2 115.4(2) . . ? C12 C9 N2 123.5(2) . . ? C23 C10 C11 120.6(3) . . ? C23 C10 N4 117.0(2) . . ? C11 C10 N4 122.2(3) . . ? C10 C11 C22 117.3(3) . . ? C10 C11 C13 124.9(3) . . ? C22 C11 C13 117.8(3) . . ? C21 C12 C9 116.3(3) . . ? C21 C12 C14 117.9(3) . . ? C9 C12 C14 125.7(3) . . ? C26 C13 C25 118.7(3) . . ? C26 C13 C11 122.6(3) . . ? C25 C13 C11 118.7(3) . . ? C30 C14 C29 117.4(3) . . ? C30 C14 C12 122.3(3) . . ? C29 C14 C12 120.2(3) . . ? C16 C15 C27 119.6(3) . . ? C15 C16 C26 120.5(3) . . ? C23 C17 C18 119.9(3) . . ? C22 C18 C17 119.2(3) . . ? C24 C19 C20 119.9(3) . . ? C19 C20 C9 120.2(3) . . ? C24 C21 C12 122.8(3) . . ? C18 C22 C11 122.5(3) . . ? C17 C23 C10 120.5(3) . . ? C19 C24 C21 119.6(3) . . ? C27 C25 C13 120.6(3) . . ? C16 C26 C13 120.3(3) . . ? C25 C27 C15 120.3(3) . . ? C32 C28 C31 119.5(3) . . ? C32 C29 C14 121.2(3) . . ? C31 C30 C14 120.9(3) . . ? C28 C31 C30 120.6(3) . . ? C28 C32 C29 120.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.182 _refine_diff_density_min -0.581 _refine_diff_density_rms 0.113 #===END