# Supplementary Material (ESI) for Catalysis Science & Technology # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full Cat.Sci.Tech. _journal_coden_cambridge 1486 #TrackingRef 'CIF.CIF' #SUBMISSION DETAILS: _publ_contact_author ; Dr. Wen-Hua Sun Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; loop_ _publ_author_name _publ_author_address 'Tianpengfei Xiao' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Jingjuan Lai' ; Center of Analysis and Measurement Shanxi Datong University Datong 037009 China ; 'Shu Zhang' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Xiang Hao' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; 'Wen-Hua Sun' ; Institute of Chemistry Chinese Academy of Sciences Beijing 100190 China ; _publ_contact_author_name 'Dr. Wen-Hua Sun' data_C2 _database_code_depnum_ccdc_archive 'CCDC 805826' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24 Cl2 Co N2' _chemical_formula_weight 446.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.337(2) _cell_length_b 15.712(3) _cell_length_c 11.611(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.49(3) _cell_angle_gamma 90.00 _cell_volume 2058.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6953 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.127 _exptl_crystal_size_min 0.116 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 1.102 _exptl_absorpt_correction_type Numerical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.7869 _exptl_absorpt_correction_T_max 0.9109 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 18079 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0401 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.45 _reflns_number_total 4682 _reflns_number_gt 4441 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0505P)^2^+1.8370P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4682 _refine_ls_number_parameters 272 _refine_ls_number_restraints 82 _refine_ls_R_factor_ref 0.0616 _refine_ls_R_factor_gt 0.0574 _refine_ls_wR_factor_ref 0.1336 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 1.200 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.58405(3) 0.08563(3) 0.46203(3) 0.02575(13) Uani 1 1 d . . . N1 N 0.7708(2) 0.11389(16) 0.4746(2) 0.0272(5) Uani 1 1 d . . . Cl2 Cl 0.37511(6) 0.05376(5) 0.47384(7) 0.03323(19) Uani 1 1 d . . . N2 N 0.6047(2) 0.17150(16) 0.5967(2) 0.0297(5) Uani 1 1 d . . . Cl1 Cl 0.55625(7) 0.14044(6) 0.28007(7) 0.0436(2) Uani 1 1 d . . . C1 C 0.8034(3) 0.1731(2) 0.5531(3) 0.0297(6) Uani 1 1 d . . . C16 C 0.7070(3) 0.2061(2) 0.6203(3) 0.0324(7) Uani 1 1 d . . . C9 C 0.8541(3) 0.0783(2) 0.4128(3) 0.0291(6) Uani 1 1 d . . . C3 C 1.0064(3) 0.1654(2) 0.5144(3) 0.0390(8) Uani 1 1 d . . . H3A H 1.0864 0.1838 0.5278 0.047 Uiso 1 1 calc R . . C2 C 0.9215(3) 0.2005(2) 0.5762(3) 0.0377(7) Uani 1 1 d . . . H2A H 0.9420 0.2425 0.6335 0.045 Uiso 1 1 calc R . . C8 C 0.8213(3) 0.0147(2) 0.3300(3) 0.0334(7) Uani 1 1 d . . . H8A H 0.7406 -0.0017 0.3156 0.040 Uiso 1 1 calc R . . C10 C 0.5064(3) 0.1924(2) 0.6621(3) 0.0311(7) Uani 1 1 d . B . C5 C 1.0601(3) 0.0617(2) 0.3680(3) 0.0404(8) Uani 1 1 d . . . H5A H 1.1412 0.0776 0.3799 0.048 Uiso 1 1 calc R . . C15 C 0.4216(3) 0.2510(2) 0.6164(3) 0.0387(8) Uani 1 1 d . B . C17 C 0.7342(3) 0.2763(2) 0.7055(3) 0.0410(8) Uani 1 1 d . . . H17A H 0.8065 0.2615 0.7562 0.049 Uiso 1 1 calc R . . H17B H 0.6680 0.2818 0.7548 0.049 Uiso 1 1 calc R . . C6 C 1.0260(3) 0.0005(3) 0.2910(3) 0.0437(8) Uani 1 1 d . . . H6A H 1.0836 -0.0270 0.2497 0.052 Uiso 1 1 calc R . . C4 C 0.9752(3) 0.1026(2) 0.4317(3) 0.0329(7) Uani 1 1 d . . . C18 C 0.7531(3) 0.3614(2) 0.6467(4) 0.0474(9) Uani 1 1 d . . . H18A H 0.7706 0.4054 0.7057 0.071 Uiso 1 1 calc R . . H18B H 0.6811 0.3769 0.5976 0.071 Uiso 1 1 calc R . . H18C H 0.8196 0.3566 0.5991 0.071 Uiso 1 1 calc R . . C7 C 0.9054(3) -0.0235(2) 0.2705(3) 0.0412(8) Uani 1 1 d . . . H7A H 0.8828 -0.0663 0.2151 0.049 Uiso 1 1 calc R . . C20 C 0.4339(4) 0.2974(3) 0.5048(4) 0.0585(11) Uani 1 1 d D . . H20A H 0.5169 0.2918 0.4862 0.070 Uiso 1 1 calc R A 1 H20B H 0.3830 0.2686 0.4425 0.070 Uiso 1 1 calc R A 1 C11 C 0.4920(3) 0.1458(2) 0.7616(3) 0.0432(8) Uani 1 1 d D . . C14 C 0.3223(3) 0.2637(3) 0.6771(4) 0.0475(9) Uani 1 1 d . . . H14A H 0.2644 0.3045 0.6494 0.057 Uiso 1 1 calc R B . C13 C 0.3069(4) 0.2188(3) 0.7753(4) 0.0536(10) Uani 1 1 d . B . H13A H 0.2381 0.2277 0.8145 0.064 Uiso 1 1 calc R . . C12 C 0.3909(4) 0.1607(3) 0.8174(4) 0.0542(10) Uani 1 1 d . B . H12A H 0.3796 0.1301 0.8861 0.065 Uiso 1 1 calc R . . C19 C 0.5988(8) 0.0918(6) 0.8100(8) 0.052(3) Uani 0.581(13) 1 d PDU B 1 H19A H 0.6138 0.0470 0.7531 0.063 Uiso 0.581(13) 1 calc PR B 1 H19B H 0.6700 0.1285 0.8204 0.063 Uiso 0.581(13) 1 calc PR B 1 C21 C 0.5795(9) 0.0501(6) 0.9251(6) 0.064(3) Uani 0.581(13) 1 d PDU B 1 H21A H 0.6503 0.0176 0.9531 0.096 Uiso 0.581(13) 1 calc PR B 1 H21B H 0.5112 0.0117 0.9145 0.096 Uiso 0.581(13) 1 calc PR B 1 H21C H 0.5646 0.0942 0.9817 0.096 Uiso 0.581(13) 1 calc PR B 1 C22 C 0.4025(17) 0.3898(6) 0.5032(18) 0.117(7) Uani 0.581(13) 1 d PDU B 1 H22A H 0.4131 0.4136 0.4269 0.175 Uiso 0.581(13) 1 calc PR B 1 H22B H 0.4542 0.4198 0.5623 0.175 Uiso 0.581(13) 1 calc PR B 1 H22C H 0.3198 0.3966 0.5193 0.175 Uiso 0.581(13) 1 calc PR B 1 C19' C 0.5641(10) 0.0683(5) 0.8056(10) 0.039(3) Uani 0.419(13) 1 d PDU B 2 H19C H 0.5100 0.0216 0.8235 0.047 Uiso 0.419(13) 1 calc PR B 2 H19D H 0.6132 0.0480 0.7451 0.047 Uiso 0.419(13) 1 calc PR B 2 C21' C 0.6438(11) 0.0920(8) 0.9143(10) 0.072(4) Uani 0.419(13) 1 d PDU B 2 H21D H 0.6914 0.0425 0.9411 0.108 Uiso 0.419(13) 1 calc PR B 2 H21E H 0.5947 0.1099 0.9750 0.108 Uiso 0.419(13) 1 calc PR B 2 H21F H 0.6963 0.1387 0.8966 0.108 Uiso 0.419(13) 1 calc PR B 2 C22' C 0.4388(14) 0.3927(5) 0.5181(13) 0.044(3) Uani 0.419(13) 1 d PDU B 2 H22D H 0.4468 0.4190 0.4427 0.066 Uiso 0.419(13) 1 calc PR B 2 H22E H 0.5069 0.4083 0.5724 0.066 Uiso 0.419(13) 1 calc PR B 2 H22F H 0.3657 0.4128 0.5479 0.066 Uiso 0.419(13) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0216(2) 0.0281(2) 0.0273(2) -0.00062(15) 0.00135(15) -0.00280(15) N1 0.0237(12) 0.0305(13) 0.0269(12) 0.0030(10) -0.0012(10) -0.0023(10) Cl2 0.0234(4) 0.0328(4) 0.0436(4) 0.0017(3) 0.0040(3) -0.0023(3) N2 0.0267(13) 0.0286(13) 0.0340(13) -0.0031(10) 0.0029(10) 0.0003(10) Cl1 0.0306(4) 0.0602(6) 0.0391(5) 0.0184(4) -0.0014(3) -0.0021(4) C1 0.0261(15) 0.0291(15) 0.0328(16) 0.0007(12) -0.0026(12) -0.0026(12) C16 0.0331(17) 0.0294(16) 0.0338(16) -0.0008(13) -0.0012(13) -0.0038(13) C9 0.0277(15) 0.0321(16) 0.0276(14) 0.0076(12) 0.0030(12) -0.0007(12) C3 0.0240(16) 0.0434(19) 0.048(2) 0.0073(15) -0.0027(14) -0.0050(14) C2 0.0305(17) 0.0362(18) 0.0449(19) -0.0026(15) -0.0047(14) -0.0070(14) C8 0.0286(16) 0.0406(18) 0.0317(16) 0.0031(13) 0.0063(12) -0.0022(13) C10 0.0294(16) 0.0316(16) 0.0327(16) -0.0090(12) 0.0050(12) -0.0008(12) C5 0.0234(16) 0.052(2) 0.047(2) 0.0126(16) 0.0083(14) -0.0020(14) C15 0.0383(18) 0.0364(18) 0.0406(18) -0.0085(14) -0.0001(14) 0.0060(15) C17 0.0400(19) 0.046(2) 0.0376(18) -0.0123(15) 0.0043(14) -0.0102(15) C6 0.0349(18) 0.057(2) 0.0415(19) 0.0049(17) 0.0169(15) 0.0026(16) C4 0.0237(15) 0.0385(17) 0.0361(16) 0.0107(13) 0.0015(12) -0.0012(13) C18 0.046(2) 0.0326(18) 0.063(2) -0.0107(17) 0.0012(18) -0.0037(16) C7 0.0407(19) 0.049(2) 0.0349(17) -0.0046(15) 0.0097(14) 0.0013(16) C20 0.073(3) 0.056(3) 0.046(2) 0.0024(19) 0.001(2) 0.026(2) C11 0.055(2) 0.0400(19) 0.0364(18) -0.0036(14) 0.0134(16) 0.0090(16) C14 0.0349(19) 0.048(2) 0.059(2) -0.0191(18) 0.0017(17) 0.0089(16) C13 0.045(2) 0.053(2) 0.065(3) -0.025(2) 0.0209(19) -0.0031(18) C12 0.075(3) 0.045(2) 0.047(2) -0.0075(17) 0.027(2) 0.000(2) C19 0.078(6) 0.034(4) 0.046(4) 0.003(3) 0.015(4) 0.008(4) C21 0.086(6) 0.052(5) 0.054(4) 0.005(3) 0.003(4) 0.005(4) C22 0.137(11) 0.106(9) 0.108(10) 0.022(7) 0.015(8) 0.027(7) C19' 0.052(6) 0.031(5) 0.037(5) 0.006(4) 0.016(4) -0.001(4) C21' 0.064(7) 0.069(7) 0.079(7) 0.000(5) -0.015(5) -0.009(5) C22' 0.054(6) 0.033(5) 0.044(5) 0.008(4) -0.007(4) 0.011(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 2.061(3) . ? Co1 N1 2.154(2) . ? Co1 Cl1 2.2753(10) . ? Co1 Cl2 2.3451(10) 3_656 ? Co1 Cl2 2.4376(9) . ? N1 C1 1.330(4) . ? N1 C9 1.360(4) . ? Cl2 Co1 2.3451(10) 3_656 ? N2 C16 1.286(4) . ? N2 C10 1.446(4) . ? C1 C2 1.408(4) . ? C1 C16 1.494(4) . ? C16 C17 1.494(4) . ? C9 C8 1.411(4) . ? C9 C4 1.422(4) . ? C3 C2 1.370(5) . ? C3 C4 1.399(5) . ? C3 H3A 0.9500 . ? C2 H2A 0.9500 . ? C8 C7 1.369(5) . ? C8 H8A 0.9500 . ? C10 C11 1.391(5) . ? C10 C15 1.398(5) . ? C5 C6 1.344(5) . ? C5 C4 1.422(5) . ? C5 H5A 0.9500 . ? C15 C14 1.398(5) . ? C15 C20 1.505(5) . ? C17 C18 1.526(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C6 C7 1.416(5) . ? C6 H6A 0.9500 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C7 H7A 0.9500 . ? C20 C22 1.495(9) . ? C20 C22' 1.506(8) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C11 C12 1.389(5) . ? C11 C19' 1.527(8) . ? C11 C19 1.540(7) . ? C14 C13 1.367(6) . ? C14 H14A 0.9500 . ? C13 C12 1.375(6) . ? C13 H13A 0.9500 . ? C12 H12A 0.9500 . ? C19 C21 1.523(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C19' C21' 1.526(10) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 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 N2 Co1 N1 76.95(10) . . ? N2 Co1 Cl1 116.88(8) . . ? N1 Co1 Cl1 91.88(7) . . ? N2 Co1 Cl2 111.46(8) . 3_656 ? N1 Co1 Cl2 90.46(7) . 3_656 ? Cl1 Co1 Cl2 130.83(4) . 3_656 ? N2 Co1 Cl2 97.60(8) . . ? N1 Co1 Cl2 172.92(7) . . ? Cl1 Co1 Cl2 94.64(4) . . ? Cl2 Co1 Cl2 87.35(3) 3_656 . ? C1 N1 C9 119.2(3) . . ? C1 N1 Co1 113.4(2) . . ? C9 N1 Co1 127.4(2) . . ? Co1 Cl2 Co1 92.65(3) 3_656 . ? C16 N2 C10 121.1(3) . . ? C16 N2 Co1 118.2(2) . . ? C10 N2 Co1 120.66(19) . . ? N1 C1 C2 122.8(3) . . ? N1 C1 C16 115.5(3) . . ? C2 C1 C16 121.7(3) . . ? N2 C16 C17 125.3(3) . . ? N2 C16 C1 115.6(3) . . ? C17 C16 C1 119.1(3) . . ? N1 C9 C8 119.9(3) . . ? N1 C9 C4 121.2(3) . . ? C8 C9 C4 118.9(3) . . ? C2 C3 C4 120.0(3) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C2 C1 118.7(3) . . ? C3 C2 H2A 120.6 . . ? C1 C2 H2A 120.6 . . ? C7 C8 C9 120.2(3) . . ? C7 C8 H8A 119.9 . . ? C9 C8 H8A 119.9 . . ? C11 C10 C15 122.1(3) . . ? C11 C10 N2 118.3(3) . . ? C15 C10 N2 119.1(3) . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C10 C15 C14 117.4(3) . . ? C10 C15 C20 122.0(3) . . ? C14 C15 C20 120.6(3) . . ? C16 C17 C18 112.3(3) . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.9 . . ? C5 C6 C7 120.9(3) . . ? C5 C6 H6A 119.6 . . ? C7 C6 H6A 119.6 . . ? C3 C4 C9 118.2(3) . . ? C3 C4 C5 122.5(3) . . ? C9 C4 C5 119.3(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C7 C6 120.5(3) . . ? C8 C7 H7A 119.8 . . ? C6 C7 H7A 119.8 . . ? C22 C20 C15 116.1(9) . . ? C22 C20 C22' 16.6(11) . . ? C15 C20 C22' 113.5(7) . . ? C22 C20 H20A 108.3 . . ? C15 C20 H20A 108.3 . . ? C22' C20 H20A 94.8 . . ? C22 C20 H20B 108.3 . . ? C15 C20 H20B 108.3 . . ? C22' C20 H20B 122.8 . . ? H20A C20 H20B 107.4 . . ? C12 C11 C10 117.7(3) . . ? C12 C11 C19' 114.7(6) . . ? C10 C11 C19' 126.7(6) . . ? C12 C11 C19 125.3(4) . . ? C10 C11 C19 116.3(4) . . ? C19' C11 C19 20.2(5) . . ? C13 C14 C15 121.3(4) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C14 C13 C12 120.0(4) . . ? C14 C13 H13A 120.0 . . ? C12 C13 H13A 120.0 . . ? C13 C12 C11 121.4(4) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C21 C19 C11 112.5(6) . . ? C21 C19 H19A 109.1 . . ? C11 C19 H19A 109.1 . . ? C21 C19 H19B 109.1 . . ? C11 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21' C19' C11 109.7(7) . . ? C21' C19' H19C 109.7 . . ? C11 C19' H19C 109.7 . . ? C21' C19' H19D 109.7 . . ? C11 C19' H19D 109.7 . . ? H19C C19' H19D 108.2 . . ? C19' C21' H21D 109.5 . . ? C19' C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19' C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C20 C22' H22D 109.5 . . ? C20 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C20 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? 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 N2 Co1 N1 C1 -3.9(2) . . . . ? Cl1 Co1 N1 C1 113.3(2) . . . . ? Cl2 Co1 N1 C1 -115.8(2) 3_656 . . . ? Cl2 Co1 N1 C1 -43.9(7) . . . . ? N2 Co1 N1 C9 176.1(3) . . . . ? Cl1 Co1 N1 C9 -66.8(2) . . . . ? Cl2 Co1 N1 C9 64.1(2) 3_656 . . . ? Cl2 Co1 N1 C9 136.0(5) . . . . ? N2 Co1 Cl2 Co1 -111.30(8) . . . 3_656 ? N1 Co1 Cl2 Co1 -72.1(6) . . . 3_656 ? Cl1 Co1 Cl2 Co1 130.76(4) . . . 3_656 ? Cl2 Co1 Cl2 Co1 0.0 3_656 . . 3_656 ? N1 Co1 N2 C16 5.2(2) . . . . ? Cl1 Co1 N2 C16 -80.2(2) . . . . ? Cl2 Co1 N2 C16 90.5(2) 3_656 . . . ? Cl2 Co1 N2 C16 -179.4(2) . . . . ? N1 Co1 N2 C10 -175.1(2) . . . . ? Cl1 Co1 N2 C10 99.5(2) . . . . ? Cl2 Co1 N2 C10 -89.8(2) 3_656 . . . ? Cl2 Co1 N2 C10 0.3(2) . . . . ? C9 N1 C1 C2 -0.6(5) . . . . ? Co1 N1 C1 C2 179.3(2) . . . . ? C9 N1 C1 C16 -177.6(3) . . . . ? Co1 N1 C1 C16 2.3(3) . . . . ? C10 N2 C16 C17 -6.9(5) . . . . ? Co1 N2 C16 C17 172.8(3) . . . . ? C10 N2 C16 C1 174.7(3) . . . . ? Co1 N2 C16 C1 -5.6(4) . . . . ? N1 C1 C16 N2 2.0(4) . . . . ? C2 C1 C16 N2 -175.1(3) . . . . ? N1 C1 C16 C17 -176.5(3) . . . . ? C2 C1 C16 C17 6.4(5) . . . . ? C1 N1 C9 C8 179.3(3) . . . . ? Co1 N1 C9 C8 -0.6(4) . . . . ? C1 N1 C9 C4 0.9(4) . . . . ? Co1 N1 C9 C4 -179.1(2) . . . . ? C4 C3 C2 C1 -1.1(5) . . . . ? N1 C1 C2 C3 0.7(5) . . . . ? C16 C1 C2 C3 177.5(3) . . . . ? N1 C9 C8 C7 -177.6(3) . . . . ? C4 C9 C8 C7 0.8(5) . . . . ? C16 N2 C10 C11 -88.1(4) . . . . ? Co1 N2 C10 C11 92.2(3) . . . . ? C16 N2 C10 C15 99.6(4) . . . . ? Co1 N2 C10 C15 -80.1(3) . . . . ? C11 C10 C15 C14 2.3(5) . . . . ? N2 C10 C15 C14 174.3(3) . . . . ? C11 C10 C15 C20 -176.2(4) . . . . ? N2 C10 C15 C20 -4.2(5) . . . . ? N2 C16 C17 C18 -106.7(4) . . . . ? C1 C16 C17 C18 71.6(4) . . . . ? C4 C5 C6 C7 0.9(5) . . . . ? C2 C3 C4 C9 1.3(5) . . . . ? C2 C3 C4 C5 -177.7(3) . . . . ? N1 C9 C4 C3 -1.2(4) . . . . ? C8 C9 C4 C3 -179.7(3) . . . . ? N1 C9 C4 C5 177.8(3) . . . . ? C8 C9 C4 C5 -0.6(4) . . . . ? C6 C5 C4 C3 178.8(3) . . . . ? C6 C5 C4 C9 -0.2(5) . . . . ? C9 C8 C7 C6 -0.2(5) . . . . ? C5 C6 C7 C8 -0.7(6) . . . . ? C10 C15 C20 C22 -137.9(9) . . . . ? C14 C15 C20 C22 43.7(10) . . . . ? C10 C15 C20 C22' -119.9(7) . . . . ? C14 C15 C20 C22' 61.7(8) . . . . ? C15 C10 C11 C12 -1.7(5) . . . . ? N2 C10 C11 C12 -173.8(3) . . . . ? C15 C10 C11 C19' 166.6(6) . . . . ? N2 C10 C11 C19' -5.5(7) . . . . ? C15 C10 C11 C19 -172.9(6) . . . . ? N2 C10 C11 C19 15.0(7) . . . . ? C10 C15 C14 C13 -2.0(5) . . . . ? C20 C15 C14 C13 176.5(4) . . . . ? C15 C14 C13 C12 1.1(6) . . . . ? C14 C13 C12 C11 -0.5(6) . . . . ? C10 C11 C12 C13 0.8(6) . . . . ? C19' C11 C12 C13 -168.9(5) . . . . ? C19 C11 C12 C13 171.1(7) . . . . ? C12 C11 C19 C21 3.9(13) . . . . ? C10 C11 C19 C21 174.3(7) . . . . ? C19' C11 C19 C21 -59.9(17) . . . . ? C12 C11 C19' C21' -82.0(12) . . . . ? C10 C11 C19' C21' 109.3(11) . . . . ? C19 C11 C19' C21' 44.3(16) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.402 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.069 #==END data_C3 _database_code_depnum_ccdc_archive 'CCDC 805827' #TrackingRef 'CIF.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H28 Cl2 Co N2' _chemical_formula_weight 474.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.125(2) _cell_length_b 16.885(3) _cell_length_c 13.533(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.01(3) _cell_angle_gamma 90.00 _cell_volume 2313.7(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7127 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 27.51 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.985 _exptl_absorpt_correction_type Numerical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.8600 _exptl_absorpt_correction_T_max 0.9695 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 18838 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5245 _reflns_number_gt 4837 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART & SAINT' _computing_data_reduction 'Siemens XPREP' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0290P)^2^+3.1724P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5245 _refine_ls_number_parameters 282 _refine_ls_number_restraints 42 _refine_ls_R_factor_ref 0.0595 _refine_ls_R_factor_gt 0.0537 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.134 _refine_ls_shift/su_max 0.010 _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 0.79709(4) 0.18003(2) 0.85133(3) 0.02639(11) Uani 1 1 d . . . Cl1 Cl 0.89562(8) 0.11542(5) 0.72893(6) 0.03838(18) Uani 1 1 d . . . Cl2 Cl 0.58561(7) 0.20691(5) 0.82942(6) 0.03850(19) Uani 1 1 d . . . N2 N 0.9104(2) 0.26638(13) 0.91316(17) 0.0246(5) Uani 1 1 d . . . N1 N 0.8491(2) 0.12404(13) 0.97969(17) 0.0255(5) Uani 1 1 d . . . C4 C 0.8676(3) 0.01496(16) 1.0953(2) 0.0274(6) Uani 1 1 d . . . C1 C 0.9409(3) 0.16358(15) 1.0301(2) 0.0252(5) Uani 1 1 d . . . C2 C 1.0044(3) 0.13079(17) 1.1125(2) 0.0315(6) Uani 1 1 d . . . H2A H 1.0709 0.1597 1.1464 0.038 Uiso 1 1 calc R . . C16 C 0.9687(3) 0.24627(16) 0.9940(2) 0.0267(6) Uani 1 1 d . . . C10 C 0.9230(3) 0.34559(15) 0.8730(2) 0.0275(6) Uani 1 1 d . . . C9 C 0.8090(3) 0.05114(15) 1.0118(2) 0.0270(6) Uani 1 1 d . . . C12 C 1.0269(3) 0.43667(19) 0.7628(3) 0.0408(7) Uani 1 1 d . . . H12A H 1.0920 0.4484 0.7144 0.049 Uiso 1 1 calc R . . C3 C 0.9694(3) 0.05646(17) 1.1435(2) 0.0340(6) Uani 1 1 d . . . H3A H 1.0140 0.0329 1.1978 0.041 Uiso 1 1 calc R . . C14 C 0.8461(4) 0.47890(18) 0.8625(2) 0.0415(8) Uani 1 1 d . . . H14A H 0.7873 0.5197 0.8827 0.050 Uiso 1 1 calc R . . C6 C 0.7145(3) -0.09323(18) 1.0816(3) 0.0421(8) Uani 1 1 d . . . H6A H 0.6796 -0.1417 1.1058 0.051 Uiso 1 1 calc R . . C11 C 1.0190(3) 0.36018(17) 0.8010(2) 0.0342(7) Uani 1 1 d . B . C5 C 0.8178(3) -0.05878(17) 1.1286(2) 0.0351(7) Uani 1 1 d . . . H5A H 0.8569 -0.0841 1.1840 0.042 Uiso 1 1 calc R . . C15 C 0.8332(3) 0.40366(16) 0.9030(2) 0.0313(6) Uani 1 1 d . . . C13 C 0.9424(4) 0.49548(18) 0.7935(3) 0.0447(8) Uani 1 1 d . . . H13A H 0.9503 0.5474 0.7673 0.054 Uiso 1 1 calc R . . C17 C 1.0563(3) 0.29909(18) 1.0538(2) 0.0390(7) Uani 1 1 d . . . H17A H 1.0295 0.2960 1.1240 0.047 Uiso 1 1 calc R . . H17B H 1.0442 0.3545 1.0317 0.047 Uiso 1 1 calc R . . C8 C 0.7048(3) 0.01249(18) 0.9619(2) 0.0375(7) Uani 1 1 d . . . H8A H 0.6672 0.0354 0.9042 0.045 Uiso 1 1 calc R . . C19 C 1.1109(4) 0.2970(2) 0.7622(3) 0.0619(12) Uani 1 1 d D . . H19A H 1.0885 0.2469 0.7977 0.074 Uiso 1 1 calc R A 1 C7 C 0.6585(3) -0.05791(19) 0.9969(3) 0.0449(8) Uani 1 1 d . . . H7A H 0.5876 -0.0835 0.9639 0.054 Uiso 1 1 calc R . . C20 C 0.7229(3) 0.38733(19) 0.9771(2) 0.0392(7) Uani 1 1 d . . . H20A H 0.7237 0.3294 0.9922 0.047 Uiso 1 1 calc R . . C23 C 0.5876(3) 0.4077(2) 0.9343(3) 0.0503(9) Uani 1 1 d . . . H23A H 0.5740 0.3781 0.8728 0.075 Uiso 1 1 calc R . . H23B H 0.5832 0.4646 0.9206 0.075 Uiso 1 1 calc R . . H23C H 0.5187 0.3934 0.9819 0.075 Uiso 1 1 calc R . . C18 C 1.2019(4) 0.2772(3) 1.0451(3) 0.0655(12) Uani 1 1 d . . . H18A H 1.2547 0.3134 1.0857 0.098 Uiso 1 1 calc R . . H18B H 1.2296 0.2814 0.9759 0.098 Uiso 1 1 calc R . . H18C H 1.2149 0.2227 1.0682 0.098 Uiso 1 1 calc R . . C24 C 0.7448(4) 0.4320(3) 1.0743(3) 0.0666(12) Uani 1 1 d . . . H24A H 0.8318 0.4185 1.1011 0.100 Uiso 1 1 calc R . . H24B H 0.6762 0.4169 1.1218 0.100 Uiso 1 1 calc R . . H24C H 0.7403 0.4891 1.0621 0.100 Uiso 1 1 calc R . . C21 C 1.0831(11) 0.2825(3) 0.6512(4) 0.088(2) Uani 0.92(2) 1 d PDU B 1 H21A H 0.9917 0.2646 0.6428 0.131 Uiso 0.92(2) 1 calc PR B 1 H21B H 1.1435 0.2419 0.6262 0.131 Uiso 0.92(2) 1 calc PR B 1 H21C H 1.0963 0.3318 0.6145 0.131 Uiso 0.92(2) 1 calc PR B 1 C21' C 1.156(12) 0.285(6) 0.654(3) 0.086(11) Uani 0.08(2) 1 d PDU B 2 H21D H 1.0806 0.2679 0.6141 0.128 Uiso 0.08(2) 1 calc PR B 2 H21E H 1.2256 0.2451 0.6516 0.128 Uiso 0.08(2) 1 calc PR B 2 H21F H 1.1898 0.3355 0.6280 0.128 Uiso 0.08(2) 1 calc PR B 2 C22 C 1.2610(8) 0.2984(13) 0.7499(15) 0.050(5) Uani 0.27(2) 1 d PDU B 1 H22A H 1.2865 0.2625 0.6963 0.075 Uiso 0.27(2) 1 calc PR B 1 H22B H 1.3030 0.2812 0.8115 0.075 Uiso 0.27(2) 1 calc PR B 1 H22C H 1.2898 0.3523 0.7339 0.075 Uiso 0.27(2) 1 calc PR B 1 C22' C 1.2538(5) 0.3256(6) 0.7908(10) 0.085(3) Uani 0.73(2) 1 d PDU B 2 H22D H 1.2483 0.3635 0.8455 0.127 Uiso 0.73(2) 1 calc PR B 2 H22E H 1.2951 0.3511 0.7336 0.127 Uiso 0.73(2) 1 calc PR B 2 H22F H 1.3070 0.2799 0.8111 0.127 Uiso 0.73(2) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0263(2) 0.0236(2) 0.0293(2) 0.00245(15) -0.00583(15) -0.00096(14) Cl1 0.0414(4) 0.0394(4) 0.0343(4) -0.0043(3) -0.0045(3) 0.0080(3) Cl2 0.0281(4) 0.0391(4) 0.0482(5) -0.0035(3) -0.0094(3) 0.0030(3) N2 0.0231(11) 0.0212(11) 0.0294(12) 0.0010(9) 0.0010(9) -0.0005(8) N1 0.0249(11) 0.0229(11) 0.0286(12) 0.0023(9) -0.0019(9) 0.0000(9) C4 0.0290(14) 0.0229(13) 0.0304(14) 0.0014(11) 0.0043(11) 0.0049(10) C1 0.0258(13) 0.0237(13) 0.0260(14) -0.0022(10) -0.0002(10) 0.0004(10) C2 0.0341(15) 0.0306(15) 0.0298(15) -0.0006(12) -0.0075(12) 0.0006(12) C16 0.0278(14) 0.0246(13) 0.0276(14) -0.0020(11) -0.0005(11) -0.0016(10) C10 0.0292(13) 0.0205(12) 0.0329(15) 0.0033(11) -0.0059(11) -0.0013(10) C9 0.0248(13) 0.0227(13) 0.0333(15) 0.0031(11) 0.0028(11) 0.0023(10) C12 0.0430(18) 0.0340(16) 0.0452(19) 0.0096(14) -0.0033(14) -0.0079(13) C3 0.0407(16) 0.0319(15) 0.0294(15) 0.0035(12) -0.0044(12) 0.0062(12) C14 0.059(2) 0.0243(15) 0.0418(18) -0.0002(13) -0.0094(15) 0.0107(14) C6 0.0407(17) 0.0286(15) 0.057(2) 0.0119(15) 0.0090(15) -0.0011(13) C11 0.0310(15) 0.0280(14) 0.0435(18) 0.0108(13) 0.0025(13) -0.0036(11) C5 0.0403(16) 0.0290(15) 0.0359(16) 0.0079(12) 0.0066(13) 0.0058(12) C15 0.0361(15) 0.0253(14) 0.0324(15) -0.0013(12) -0.0081(12) 0.0032(11) C13 0.060(2) 0.0232(15) 0.051(2) 0.0099(14) -0.0172(17) -0.0049(14) C17 0.053(2) 0.0299(15) 0.0344(17) -0.0028(13) -0.0124(14) -0.0094(14) C8 0.0312(15) 0.0321(15) 0.0490(19) 0.0070(14) -0.0092(13) -0.0022(12) C19 0.054(2) 0.049(2) 0.083(3) 0.033(2) 0.043(2) 0.0188(18) C7 0.0375(17) 0.0306(16) 0.067(2) 0.0051(15) -0.0054(16) -0.0061(13) C20 0.0402(17) 0.0373(17) 0.0401(17) -0.0037(14) -0.0001(14) 0.0089(13) C23 0.0417(19) 0.0434(19) 0.066(2) -0.0035(17) -0.0018(17) 0.0075(15) C18 0.048(2) 0.081(3) 0.068(3) -0.014(2) -0.016(2) -0.027(2) C24 0.057(2) 0.098(3) 0.045(2) -0.022(2) 0.0029(18) 0.002(2) C21 0.129(6) 0.055(3) 0.079(3) 0.012(2) 0.067(3) 0.026(3) C21' 0.090(14) 0.079(13) 0.087(13) -0.001(9) 0.014(9) 0.001(9) C22 0.044(6) 0.059(8) 0.046(8) 0.010(6) 0.027(5) 0.014(6) C22' 0.042(3) 0.091(5) 0.121(7) 0.043(5) 0.046(4) 0.032(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 2.035(2) . ? Co1 N1 2.047(2) . ? Co1 Cl2 2.2087(9) . ? Co1 Cl1 2.2202(10) . ? N2 C16 1.288(3) . ? N2 C10 1.449(3) . ? N1 C1 1.332(3) . ? N1 C9 1.367(3) . ? C4 C3 1.406(4) . ? C4 C9 1.415(4) . ? C4 C5 1.417(4) . ? C1 C2 1.400(4) . ? C1 C16 1.506(4) . ? C2 C3 1.370(4) . ? C2 H2A 0.9500 . ? C16 C17 1.496(4) . ? C10 C15 1.397(4) . ? C10 C11 1.399(4) . ? C9 C8 1.413(4) . ? C12 C13 1.375(5) . ? C12 C11 1.394(4) . ? C12 H12A 0.9500 . ? C3 H3A 0.9500 . ? C14 C13 1.378(5) . ? C14 C15 1.390(4) . ? C14 H14A 0.9500 . ? C6 C5 1.355(5) . ? C6 C7 1.410(5) . ? C6 H6A 0.9500 . ? C11 C19 1.509(5) . ? C5 H5A 0.9500 . ? C15 C20 1.526(4) . ? C13 H13A 0.9500 . ? C17 C18 1.524(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C8 C7 1.363(4) . ? C8 H8A 0.9500 . ? C19 C22 1.529(8) . ? C19 C21' 1.545(9) . ? C19 C21 1.548(6) . ? C19 C22' 1.574(7) . ? C19 H19A 1.0000 . ? C7 H7A 0.9500 . ? C20 C23 1.527(4) . ? C20 C24 1.532(5) . ? C20 H20A 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 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 N2 Co1 N1 80.62(9) . . ? N2 Co1 Cl2 117.03(7) . . ? N1 Co1 Cl2 117.26(7) . . ? N2 Co1 Cl1 113.91(7) . . ? N1 Co1 Cl1 106.90(7) . . ? Cl2 Co1 Cl1 115.88(4) . . ? C16 N2 C10 121.4(2) . . ? C16 N2 Co1 114.74(18) . . ? C10 N2 Co1 123.80(17) . . ? C1 N1 C9 119.7(2) . . ? C1 N1 Co1 112.50(18) . . ? C9 N1 Co1 127.56(18) . . ? C3 C4 C9 117.6(3) . . ? C3 C4 C5 123.4(3) . . ? C9 C4 C5 118.9(3) . . ? N1 C1 C2 122.0(2) . . ? N1 C1 C16 115.4(2) . . ? C2 C1 C16 122.6(2) . . ? C3 C2 C1 119.2(3) . . ? C3 C2 H2A 120.4 . . ? C1 C2 H2A 120.4 . . ? N2 C16 C17 125.0(3) . . ? N2 C16 C1 115.7(2) . . ? C17 C16 C1 119.2(2) . . ? C15 C10 C11 122.1(3) . . ? C15 C10 N2 118.8(2) . . ? C11 C10 N2 119.0(2) . . ? N1 C9 C8 119.0(2) . . ? N1 C9 C4 121.2(2) . . ? C8 C9 C4 119.7(3) . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12A 119.3 . . ? C11 C12 H12A 119.3 . . ? C2 C3 C4 120.2(3) . . ? C2 C3 H3A 119.9 . . ? C4 C3 H3A 119.9 . . ? C13 C14 C15 121.3(3) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C5 C6 C7 120.7(3) . . ? C5 C6 H6A 119.7 . . ? C7 C6 H6A 119.7 . . ? C12 C11 C10 117.5(3) . . ? C12 C11 C19 119.4(3) . . ? C10 C11 C19 123.1(3) . . ? C6 C5 C4 120.2(3) . . ? C6 C5 H5A 119.9 . . ? C4 C5 H5A 119.9 . . ? C14 C15 C10 117.8(3) . . ? C14 C15 C20 119.5(3) . . ? C10 C15 C20 122.7(3) . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13A 120.1 . . ? C14 C13 H13A 120.1 . . ? C16 C17 C18 112.8(3) . . ? C16 C17 H17A 109.0 . . ? C18 C17 H17A 109.0 . . ? C16 C17 H17B 109.0 . . ? C18 C17 H17B 109.0 . . ? H17A C17 H17B 107.8 . . ? C7 C8 C9 119.5(3) . . ? C7 C8 H8A 120.2 . . ? C9 C8 H8A 120.2 . . ? C11 C19 C22 129.8(9) . . ? C11 C19 C21' 127(4) . . ? C22 C19 C21' 67(5) . . ? C11 C19 C21 109.7(4) . . ? C22 C19 C21 94.4(9) . . ? C21' C19 C21 28(4) . . ? C11 C19 C22' 105.4(5) . . ? C22 C19 C22' 26.9(6) . . ? C21' C19 C22' 90(4) . . ? C21 C19 C22' 117.0(7) . . ? C11 C19 H19A 106.9 . . ? C22 C19 H19A 106.9 . . ? C21' C19 H19A 114.4 . . ? C21 C19 H19A 106.9 . . ? C22' C19 H19A 110.5 . . ? C8 C7 C6 120.9(3) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C15 C20 C23 111.5(3) . . ? C15 C20 C24 111.7(3) . . ? C23 C20 C24 110.2(3) . . ? C15 C20 H20A 107.8 . . ? C23 C20 H20A 107.8 . . ? C24 C20 H20A 107.8 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C21' H21D 109.5 . . ? C19 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19 C21' H21F 109.4 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C22' H22D 109.5 . . ? C19 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C19 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? 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 Co1 N2 C16 5.5(2) . . . . ? Cl2 Co1 N2 C16 121.44(18) . . . . ? Cl1 Co1 N2 C16 -98.89(19) . . . . ? N1 Co1 N2 C10 -172.5(2) . . . . ? Cl2 Co1 N2 C10 -56.6(2) . . . . ? Cl1 Co1 N2 C10 83.1(2) . . . . ? N2 Co1 N1 C1 -8.96(19) . . . . ? Cl2 Co1 N1 C1 -124.62(17) . . . . ? Cl1 Co1 N1 C1 103.33(18) . . . . ? N2 Co1 N1 C9 176.9(2) . . . . ? Cl2 Co1 N1 C9 61.2(2) . . . . ? Cl1 Co1 N1 C9 -70.9(2) . . . . ? C9 N1 C1 C2 4.0(4) . . . . ? Co1 N1 C1 C2 -170.7(2) . . . . ? C9 N1 C1 C16 -174.5(2) . . . . ? Co1 N1 C1 C16 10.8(3) . . . . ? N1 C1 C2 C3 -1.4(4) . . . . ? C16 C1 C2 C3 177.1(3) . . . . ? C10 N2 C16 C17 -1.5(4) . . . . ? Co1 N2 C16 C17 -179.5(2) . . . . ? C10 N2 C16 C1 176.6(2) . . . . ? Co1 N2 C16 C1 -1.4(3) . . . . ? N1 C1 C16 N2 -6.5(4) . . . . ? C2 C1 C16 N2 175.0(3) . . . . ? N1 C1 C16 C17 171.7(3) . . . . ? C2 C1 C16 C17 -6.8(4) . . . . ? C16 N2 C10 C15 -88.9(3) . . . . ? Co1 N2 C10 C15 89.0(3) . . . . ? C16 N2 C10 C11 95.1(3) . . . . ? Co1 N2 C10 C11 -87.0(3) . . . . ? C1 N1 C9 C8 175.4(3) . . . . ? Co1 N1 C9 C8 -10.8(4) . . . . ? C1 N1 C9 C4 -3.0(4) . . . . ? Co1 N1 C9 C4 170.8(2) . . . . ? C3 C4 C9 N1 -0.5(4) . . . . ? C5 C4 C9 N1 176.8(2) . . . . ? C3 C4 C9 C8 -178.9(3) . . . . ? C5 C4 C9 C8 -1.6(4) . . . . ? C1 C2 C3 C4 -2.3(4) . . . . ? C9 C4 C3 C2 3.1(4) . . . . ? C5 C4 C3 C2 -174.0(3) . . . . ? C13 C12 C11 C10 -0.9(5) . . . . ? C13 C12 C11 C19 177.8(3) . . . . ? C15 C10 C11 C12 3.0(4) . . . . ? N2 C10 C11 C12 178.9(3) . . . . ? C15 C10 C11 C19 -175.6(3) . . . . ? N2 C10 C11 C19 0.3(5) . . . . ? C7 C6 C5 C4 2.4(5) . . . . ? C3 C4 C5 C6 176.3(3) . . . . ? C9 C4 C5 C6 -0.8(4) . . . . ? C13 C14 C15 C10 1.2(5) . . . . ? C13 C14 C15 C20 -178.4(3) . . . . ? C11 C10 C15 C14 -3.2(4) . . . . ? N2 C10 C15 C14 -179.1(3) . . . . ? C11 C10 C15 C20 176.4(3) . . . . ? N2 C10 C15 C20 0.5(4) . . . . ? C11 C12 C13 C14 -1.0(5) . . . . ? C15 C14 C13 C12 0.8(5) . . . . ? N2 C16 C17 C18 -106.9(4) . . . . ? C1 C16 C17 C18 75.1(4) . . . . ? N1 C9 C8 C7 -175.9(3) . . . . ? C4 C9 C8 C7 2.5(5) . . . . ? C12 C11 C19 C22 50.6(10) . . . . ? C10 C11 C19 C22 -130.8(9) . . . . ? C12 C11 C19 C21' -39(5) . . . . ? C10 C11 C19 C21' 140(5) . . . . ? C12 C11 C19 C21 -63.3(5) . . . . ? C10 C11 C19 C21 115.3(5) . . . . ? C12 C11 C19 C22' 63.5(5) . . . . ? C10 C11 C19 C22' -117.9(5) . . . . ? C9 C8 C7 C6 -0.9(5) . . . . ? C5 C6 C7 C8 -1.5(5) . . . . ? C14 C15 C20 C23 56.0(4) . . . . ? C10 C15 C20 C23 -123.6(3) . . . . ? C14 C15 C20 C24 -67.7(4) . . . . ? C10 C15 C20 C24 112.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.423 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.067 _publ_section_references ; Sheldrick G.M.(1996), SADABS, Absorption Correction Program, University of Goeltingen, German Siemens(1994), SAINT Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1996), SMART Software Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA Siemens(1994), SHELXTL^TM^ Version 5 Reference Manual, Siemens Energy & Automation Inc., Madison, Wisconsin, USA ;