# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'George Britovsek' _publ_contact_author_address ; Building RCS1, room 314 Frankland Road South Kensington London SW7 2AY ; _publ_contact_author_email g.britovsek@imperial.ac.uk'' loop_ _publ_author_name G.Britovsek R.Cariou J.Chirinos V.Gibson A.Tomov A.White ; G.Jacobsen ; data_1 _database_code_depnum_ccdc_archive 'CCDC 762753' #TrackingRef '- Dalton04-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 Cl2 Co N5, C3 H7 N O, 0.5(C4 H10 O)' _chemical_formula_sum 'C21 H27 Cl2 Co N6 O1.50' _chemical_formula_weight 517.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 22.6305(3) _cell_length_b 8.25098(10) _cell_length_c 28.3753(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.2954(15) _cell_angle_gamma 90.00 _cell_volume 4902.24(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6822 _cell_measurement_theta_min 3.1533 _cell_measurement_theta_max 71.2341 _exptl_crystal_description shards _exptl_crystal_colour Blue _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 7.716 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.70645 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54248 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16165 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 71.46 _reflns_number_total 4673 _reflns_number_gt 3714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0410P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4673 _refine_ls_number_parameters 317 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.0422 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0714 _refine_ls_wR_factor_gt 0.0662 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.976 _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 Co Co 0.625562(13) 0.54835(4) 0.575418(11) 0.03231(9) Uani 1 1 d . . . Cl1 Cl 0.55174(2) 0.73746(6) 0.524437(18) 0.03947(12) Uani 1 1 d . . . Cl2 Cl 0.66117(2) 0.69240(6) 0.650638(18) 0.04228(13) Uani 1 1 d . . . N1 N 0.59449(7) 0.3858(2) 0.50477(6) 0.0369(4) Uani 1 1 d D . . H1 H 0.5523(2) 0.400(3) 0.4877(7) 0.054(7) Uiso 1 1 d D . . C2 C 0.62945(9) 0.4352(3) 0.47293(7) 0.0442(5) Uani 1 1 d . . . H2A H 0.6056 0.5210 0.4488 0.053 Uiso 1 1 calc R . . H2B H 0.6349 0.3416 0.4531 0.053 Uiso 1 1 calc R . . C3 C 0.69285(9) 0.4971(3) 0.50744(8) 0.0389(5) Uani 1 1 d . . . N4 N 0.70360(7) 0.5452(2) 0.55443(6) 0.0348(4) Uani 1 1 d . . . C5 C 0.76706(9) 0.5968(2) 0.57436(8) 0.0360(4) Uani 1 1 d . . . C6 C 0.80446(9) 0.6549(3) 0.62226(8) 0.0421(5) Uani 1 1 d . . . H6A H 0.7879 0.6677 0.6482 0.050 Uiso 1 1 calc R . . C7 C 0.86735(10) 0.6936(3) 0.63042(10) 0.0529(6) Uani 1 1 d . . . H7A H 0.8945 0.7330 0.6629 0.064 Uiso 1 1 calc R . . C8 C 0.89188(11) 0.6764(3) 0.59258(10) 0.0575(7) Uani 1 1 d . . . H8A H 0.9351 0.7053 0.5998 0.069 Uiso 1 1 calc R . . C9 C 0.85517(10) 0.6188(3) 0.54501(10) 0.0513(6) Uani 1 1 d . . . H9A H 0.8718 0.6074 0.5191 0.062 Uiso 1 1 calc R . . C10 C 0.79270(10) 0.5781(3) 0.53685(8) 0.0413(5) Uani 1 1 d . . . N11 N 0.74403(8) 0.5141(2) 0.49472(7) 0.0428(4) Uani 1 1 d D . . H11 H 0.7447(11) 0.484(3) 0.4644(4) 0.062(8) Uiso 1 1 d D . . C12 C 0.60646(9) 0.2173(3) 0.52236(8) 0.0395(5) Uani 1 1 d . . . H12A H 0.6509 0.1863 0.5279 0.047 Uiso 1 1 calc R . . H12B H 0.5770 0.1436 0.4966 0.047 Uiso 1 1 calc R . . C13 C 0.59596(8) 0.2056(2) 0.57077(8) 0.0369(5) Uani 1 1 d . . . N14 N 0.59887(7) 0.3351(2) 0.59903(6) 0.0361(4) Uani 1 1 d . . . C15 C 0.58768(10) 0.2783(3) 0.64125(8) 0.0423(5) Uani 1 1 d . . . C16 C 0.58395(12) 0.3602(3) 0.68274(9) 0.0583(6) Uani 1 1 d . . . H16A H 0.5896 0.4743 0.6862 0.070 Uiso 1 1 calc R . . C17 C 0.57178(15) 0.2691(4) 0.71853(11) 0.0794(9) Uani 1 1 d . . . H17A H 0.5690 0.3217 0.7474 0.095 Uiso 1 1 calc R . . C18 C 0.56328(15) 0.1010(4) 0.71380(12) 0.0812(9) Uani 1 1 d . . . H18A H 0.5550 0.0427 0.7395 0.097 Uiso 1 1 calc R . . C19 C 0.56658(12) 0.0186(3) 0.67289(11) 0.0652(7) Uani 1 1 d . . . H19A H 0.5609 -0.0955 0.6696 0.078 Uiso 1 1 calc R . . C20 C 0.57859(10) 0.1101(3) 0.63676(9) 0.0452(5) Uani 1 1 d . . . N21 N 0.58425(8) 0.0689(2) 0.59127(7) 0.0435(4) Uani 1 1 d D . . H21 H 0.5819(11) -0.0302(12) 0.5774(8) 0.057(7) Uiso 1 1 d D . . O30 O 0.74551(7) 0.38746(19) 0.40616(5) 0.0481(4) Uani 1 1 d . . . C30 C 0.75235(9) 0.4434(3) 0.36810(8) 0.0416(5) Uani 1 1 d . . . H30A H 0.7631 0.5549 0.3688 0.050 Uiso 1 1 calc R . . N31 N 0.74600(8) 0.3611(2) 0.32660(6) 0.0421(4) Uani 1 1 d . . . C32 C 0.73067(12) 0.1898(3) 0.32212(9) 0.0594(7) Uani 1 1 d . . . H32A H 0.7220 0.1546 0.3518 0.089 Uiso 1 1 calc R . . H32B H 0.7668 0.1282 0.3204 0.089 Uiso 1 1 calc R . . H32C H 0.6929 0.1708 0.2911 0.089 Uiso 1 1 calc R . . C33 C 0.75505(12) 0.4366(3) 0.28361(8) 0.0589(6) Uani 1 1 d . . . H33A H 0.7656 0.5514 0.2911 0.088 Uiso 1 1 calc R . . H33B H 0.7157 0.4270 0.2532 0.088 Uiso 1 1 calc R . . H33C H 0.7900 0.3823 0.2775 0.088 Uiso 1 1 calc R . . O40 O 0.5046(3) 0.2757(6) 0.2429(2) 0.0678(18) Uiso 0.370(5) 1 d PDU A -1 C41 C 0.5167(4) 0.3485(13) 0.2909(3) 0.082(3) Uiso 0.370(5) 1 d PDU A -1 H41A H 0.4865 0.3051 0.3055 0.099 Uiso 0.370(5) 1 calc PR A -1 H41B H 0.5100 0.4670 0.2867 0.099 Uiso 0.370(5) 1 calc PR A -1 C42 C 0.5810(5) 0.316(2) 0.3250(4) 0.113(4) Uiso 0.370(5) 1 d PDU A -1 H42A H 0.5887 0.3665 0.3581 0.170 Uiso 0.370(5) 1 calc PR A -1 H42B H 0.6108 0.3607 0.3107 0.170 Uiso 0.370(5) 1 calc PR A -1 H42C H 0.5873 0.1987 0.3294 0.170 Uiso 0.370(5) 1 calc PR A -1 C43 C 0.4455(5) 0.3437(16) 0.2088(4) 0.092(3) Uiso 0.370(5) 1 d PDU A -1 H43A H 0.4515 0.4583 0.2013 0.110 Uiso 0.370(5) 1 calc PR A -1 H43B H 0.4127 0.3387 0.2240 0.110 Uiso 0.370(5) 1 calc PR A -1 C44 C 0.4261(5) 0.2453(13) 0.1621(3) 0.082(3) Uiso 0.370(5) 1 d PDU A -1 H44A H 0.3857 0.2868 0.1373 0.122 Uiso 0.370(5) 1 calc PR A -1 H44B H 0.4205 0.1323 0.1702 0.122 Uiso 0.370(5) 1 calc PR A -1 H44C H 0.4591 0.2513 0.1477 0.122 Uiso 0.370(5) 1 calc PR A -1 O40' O 0.5057(8) 0.3651(19) 0.2414(5) 0.072(5) Uiso 0.130(5) 1 d PDU A -2 C41' C 0.5593(11) 0.301(4) 0.2789(9) 0.103(8) Uiso 0.130(5) 1 d PDU A -2 H41C H 0.5961 0.3076 0.2681 0.123 Uiso 0.130(5) 1 calc PR A -2 H41D H 0.5519 0.1858 0.2844 0.123 Uiso 0.130(5) 1 calc PR A -2 C42' C 0.5735(15) 0.392(4) 0.3262(8) 0.092(8) Uiso 0.130(5) 1 d PDU A -2 H42D H 0.6092 0.3405 0.3536 0.138 Uiso 0.130(5) 1 calc PR A -2 H42E H 0.5358 0.3927 0.3352 0.138 Uiso 0.130(5) 1 calc PR A -2 H42F H 0.5850 0.5036 0.3215 0.138 Uiso 0.130(5) 1 calc PR A -2 C43' C 0.4659(12) 0.255(3) 0.2077(7) 0.087(6) Uiso 0.130(5) 1 d PDU A -2 H43C H 0.4297 0.2280 0.2178 0.104 Uiso 0.130(5) 1 calc PR A -2 H43D H 0.4896 0.1536 0.2081 0.104 Uiso 0.130(5) 1 calc PR A -2 C44' C 0.4420(10) 0.324(4) 0.1568(6) 0.063(5) Uiso 0.130(5) 1 d PDU A -2 H44D H 0.4156 0.2435 0.1324 0.095 Uiso 0.130(5) 1 calc PR A -2 H44E H 0.4780 0.3549 0.1476 0.095 Uiso 0.130(5) 1 calc PR A -2 H44F H 0.4161 0.4198 0.1560 0.095 Uiso 0.130(5) 1 calc PR A -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 Co 0.03332(15) 0.03115(19) 0.03339(17) -0.00318(14) 0.01370(12) -0.00162(13) Cl1 0.0354(2) 0.0371(3) 0.0428(3) -0.0005(2) 0.01134(19) 0.0019(2) Cl2 0.0514(3) 0.0378(3) 0.0362(3) -0.0071(2) 0.0150(2) -0.0038(2) N1 0.0342(8) 0.0357(10) 0.0380(9) -0.0030(8) 0.0106(7) 0.0019(7) C2 0.0507(11) 0.0478(14) 0.0342(11) -0.0043(10) 0.0164(9) 0.0013(10) C3 0.0466(11) 0.0360(12) 0.0392(11) 0.0008(10) 0.0221(9) 0.0027(9) N4 0.0361(8) 0.0356(10) 0.0350(8) -0.0015(8) 0.0159(7) -0.0005(7) C5 0.0379(10) 0.0273(11) 0.0466(11) 0.0019(9) 0.0203(9) 0.0006(8) C6 0.0399(10) 0.0372(12) 0.0493(12) -0.0006(10) 0.0173(9) -0.0020(9) C7 0.0417(11) 0.0450(14) 0.0672(15) -0.0026(12) 0.0152(11) -0.0064(10) C8 0.0421(12) 0.0454(15) 0.0905(19) -0.0001(14) 0.0314(13) -0.0035(11) C9 0.0517(12) 0.0384(13) 0.0779(17) -0.0004(13) 0.0404(12) 0.0004(11) C10 0.0475(11) 0.0304(12) 0.0528(13) 0.0034(10) 0.0266(10) 0.0025(9) N11 0.0531(10) 0.0405(11) 0.0455(10) -0.0019(9) 0.0306(9) 0.0009(8) C12 0.0370(10) 0.0360(12) 0.0422(11) -0.0088(10) 0.0111(8) 0.0017(9) C13 0.0295(9) 0.0341(12) 0.0436(11) -0.0024(10) 0.0100(8) -0.0005(8) N14 0.0380(8) 0.0310(9) 0.0409(9) -0.0051(8) 0.0166(7) -0.0039(7) C15 0.0429(11) 0.0415(13) 0.0477(12) 0.0003(10) 0.0231(9) -0.0038(9) C16 0.0784(16) 0.0490(15) 0.0629(15) -0.0048(13) 0.0443(14) -0.0059(13) C17 0.119(3) 0.072(2) 0.076(2) 0.0028(17) 0.0689(19) 0.0004(18) C18 0.109(2) 0.070(2) 0.097(2) 0.0196(18) 0.075(2) 0.0014(18) C19 0.0738(16) 0.0441(15) 0.097(2) 0.0122(15) 0.0541(16) -0.0011(13) C20 0.0437(11) 0.0401(13) 0.0586(14) 0.0016(11) 0.0272(10) -0.0003(10) N21 0.0405(9) 0.0299(10) 0.0611(12) -0.0029(9) 0.0204(8) -0.0021(8) O30 0.0559(8) 0.0514(10) 0.0409(8) 0.0014(8) 0.0226(7) 0.0040(8) C30 0.0449(11) 0.0373(12) 0.0391(11) 0.0000(10) 0.0121(9) 0.0035(9) N31 0.0536(10) 0.0362(10) 0.0338(9) -0.0013(8) 0.0136(8) -0.0021(8) C32 0.0829(17) 0.0398(14) 0.0553(15) -0.0078(12) 0.0262(13) -0.0066(13) C33 0.0789(16) 0.0597(16) 0.0353(12) -0.0004(12) 0.0184(11) -0.0112(13) _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 Co N14 2.0535(17) . ? Co N4 2.0668(15) . ? Co N1 2.2895(17) . ? Co Cl2 2.3049(6) . ? Co Cl1 2.3420(6) . ? N1 C2 1.466(3) . ? N1 C12 1.467(3) . ? C2 C3 1.487(3) . ? C3 N4 1.322(3) . ? C3 N11 1.345(2) . ? N4 C5 1.395(2) . ? C5 C6 1.386(3) . ? C5 C10 1.401(3) . ? C6 C7 1.390(3) . ? C7 C8 1.390(3) . ? C8 C9 1.374(3) . ? C9 C10 1.384(3) . ? C10 N11 1.386(3) . ? C12 C13 1.483(3) . ? C13 N14 1.323(3) . ? C13 N21 1.341(3) . ? N14 C15 1.396(3) . ? C15 C16 1.388(3) . ? C15 C20 1.402(3) . ? C16 C17 1.373(3) . ? C17 C18 1.399(4) . ? C18 C19 1.371(4) . ? C19 C20 1.381(3) . ? C20 N21 1.387(3) . ? O30 C30 1.237(2) . ? C30 N31 1.319(3) . ? N31 C32 1.450(3) . ? N31 C33 1.452(3) . ? O40 C41 1.417(9) . ? O40 C43 1.435(10) . ? C41 C42 1.433(11) . ? C43 C44 1.472(11) . ? O40' C43' 1.379(15) . ? O40' C41' 1.380(15) . ? C41' C42' 1.463(16) . ? C43' C44' 1.453(15) . ? 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 N14 Co N4 118.19(6) . . ? N14 Co N1 75.71(6) . . ? N4 Co N1 75.67(6) . . ? N14 Co Cl2 100.51(5) . . ? N4 Co Cl2 103.68(5) . . ? N1 Co Cl2 175.00(5) . . ? N14 Co Cl1 122.90(5) . . ? N4 Co Cl1 108.52(5) . . ? N1 Co Cl1 86.52(4) . . ? Cl2 Co Cl1 98.35(2) . . ? C2 N1 C12 113.56(16) . . ? C2 N1 Co 108.57(12) . . ? C12 N1 Co 107.54(12) . . ? N1 C2 C3 107.52(16) . . ? N4 C3 N11 113.04(18) . . ? N4 C3 C2 121.96(17) . . ? N11 C3 C2 124.98(18) . . ? C3 N4 C5 105.51(16) . . ? C3 N4 Co 116.35(13) . . ? C5 N4 Co 137.73(13) . . ? C6 C5 N4 130.89(18) . . ? C6 C5 C10 120.55(18) . . ? N4 C5 C10 108.55(18) . . ? C5 C6 C7 116.7(2) . . ? C6 C7 C8 122.1(2) . . ? C9 C8 C7 121.6(2) . . ? C8 C9 C10 116.5(2) . . ? C9 C10 N11 131.6(2) . . ? C9 C10 C5 122.5(2) . . ? N11 C10 C5 105.92(17) . . ? C3 N11 C10 106.98(17) . . ? N1 C12 C13 107.66(17) . . ? N14 C13 N21 112.91(18) . . ? N14 C13 C12 121.33(19) . . ? N21 C13 C12 125.75(19) . . ? C13 N14 C15 105.40(17) . . ? C13 N14 Co 116.59(13) . . ? C15 N14 Co 137.66(14) . . ? C16 C15 N14 130.8(2) . . ? C16 C15 C20 120.4(2) . . ? N14 C15 C20 108.81(19) . . ? C17 C16 C15 117.0(2) . . ? C16 C17 C18 122.1(3) . . ? C19 C18 C17 121.5(3) . . ? C18 C19 C20 116.5(2) . . ? C19 C20 N21 132.1(2) . . ? C19 C20 C15 122.5(2) . . ? N21 C20 C15 105.38(19) . . ? C13 N21 C20 107.50(18) . . ? O30 C30 N31 125.4(2) . . ? C30 N31 C32 121.45(19) . . ? C30 N31 C33 121.81(19) . . ? C32 N31 C33 116.73(18) . . ? C41 O40 C43 105.8(7) . . ? O40 C41 C42 110.1(9) . . ? O40 C43 C44 106.0(9) . . ? C43' O40' C41' 115.7(17) . . ? O40' C41' C42' 109.5(16) . . ? O40' C43' C44' 109.2(15) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 71.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.258 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.040 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 762754' #TrackingRef '- Dalton04-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H19 Cl2 Co N5, C3 H7 N O' _chemical_formula_sum 'C25 H26 Cl2 Co N6 O' _chemical_formula_weight 556.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 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 8.04885(4) _cell_length_b 17.64238(8) _cell_length_c 18.51859(9) _cell_angle_alpha 90.00 _cell_angle_beta 97.2342(5) _cell_angle_gamma 90.00 _cell_volume 2608.72(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 21235 _cell_measurement_theta_min 2.5017 _cell_measurement_theta_max 71.1818 _exptl_crystal_description needles _exptl_crystal_colour Blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 7.281 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.271 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur PX Ultra' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.2556 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40033 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.47 _diffrn_reflns_theta_max 71.32 _reflns_number_total 5050 _reflns_number_gt 4457 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0552P)^2^+0.1417P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5050 _refine_ls_number_parameters 326 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0281 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.109 _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 Co Co 0.93146(3) 0.352718(15) 0.694905(14) 0.03397(9) Uani 1 1 d . . . Cl1 Cl 1.10104(5) 0.26977(2) 0.64680(2) 0.04456(12) Uani 1 1 d . . . Cl2 Cl 1.11301(5) 0.41232(2) 0.78348(2) 0.04142(11) Uani 1 1 d . . . N1 N 0.66817(17) 0.29585(8) 0.60110(7) 0.0332(3) Uani 1 1 d . . . C2 C 0.7071(3) 0.33556(10) 0.53560(9) 0.0405(4) Uani 1 1 d . . . H2A H 0.6049 0.3389 0.4999 0.049 Uiso 1 1 calc R . . H2B H 0.7925 0.3067 0.5130 0.049 Uiso 1 1 calc R . . C3 C 0.7710(2) 0.41333(10) 0.55460(9) 0.0360(4) Uani 1 1 d . . . N4 N 0.86215(18) 0.43123(8) 0.61698(7) 0.0355(3) Uani 1 1 d . . . C5 C 0.9018(2) 0.50818(9) 0.61059(9) 0.0379(4) Uani 1 1 d . . . C6 C 0.9933(3) 0.55734(10) 0.65903(10) 0.0459(4) Uani 1 1 d . . . H6A H 1.0431 0.5407 0.7056 0.055 Uiso 1 1 calc R . . C7 C 1.0089(3) 0.63184(11) 0.63641(12) 0.0537(5) Uani 1 1 d . . . H7A H 1.0710 0.6668 0.6682 0.064 Uiso 1 1 calc R . . C8 C 0.9360(3) 0.65661(11) 0.56842(13) 0.0552(5) Uani 1 1 d . . . H8A H 0.9481 0.7082 0.5553 0.066 Uiso 1 1 calc R . . C9 C 0.8467(3) 0.60846(11) 0.51965(11) 0.0498(5) Uani 1 1 d . . . H9A H 0.7989 0.6252 0.4728 0.060 Uiso 1 1 calc R . . C10 C 0.8299(2) 0.53385(10) 0.54239(10) 0.0405(4) Uani 1 1 d . . . N11 N 0.7477(2) 0.47207(9) 0.50854(8) 0.0402(3) Uani 1 1 d D . . H11 H 0.686(2) 0.4694(11) 0.4646(5) 0.047(6) Uiso 1 1 d D . . C12 C 0.5368(2) 0.33421(10) 0.63548(9) 0.0352(3) Uani 1 1 d . . . H12A H 0.4289 0.3076 0.6225 0.042 Uiso 1 1 calc R . . H12B H 0.5239 0.3869 0.6171 0.042 Uiso 1 1 calc R . . C13 C 0.5802(2) 0.33512(9) 0.71636(9) 0.0330(3) Uani 1 1 d . . . N14 N 0.73462(17) 0.33214(8) 0.75062(7) 0.0324(3) Uani 1 1 d . . . C15 C 0.7185(2) 0.33881(9) 0.82520(8) 0.0324(3) Uani 1 1 d . . . C16 C 0.8369(2) 0.33720(10) 0.88636(9) 0.0389(4) Uani 1 1 d . . . H16A H 0.9521 0.3293 0.8824 0.047 Uiso 1 1 calc R . . C17 C 0.7814(3) 0.34752(10) 0.95333(10) 0.0427(4) Uani 1 1 d . . . H17A H 0.8601 0.3466 0.9961 0.051 Uiso 1 1 calc R . . C18 C 0.6119(3) 0.35932(10) 0.95957(9) 0.0423(4) Uani 1 1 d . . . H18A H 0.5788 0.3678 1.0064 0.051 Uiso 1 1 calc R . . C19 C 0.4919(2) 0.35895(10) 0.89959(10) 0.0407(4) Uani 1 1 d . . . H19A H 0.3766 0.3662 0.9037 0.049 Uiso 1 1 calc R . . C20 C 0.5492(2) 0.34732(9) 0.83230(9) 0.0343(3) Uani 1 1 d . . . N21 N 0.46471(18) 0.34320(8) 0.76236(8) 0.0368(3) Uani 1 1 d D . . H21 H 0.3533(5) 0.3436(11) 0.7490(11) 0.043(6) Uiso 1 1 d D . . C22 C 0.6491(2) 0.21542(10) 0.59498(9) 0.0353(3) Uani 1 1 d . . . C23 C 0.7278(3) 0.17319(11) 0.54595(11) 0.0470(4) Uani 1 1 d . . . H23A H 0.7961 0.1981 0.5150 0.056 Uiso 1 1 calc R . . C24 C 0.7084(3) 0.09537(11) 0.54136(12) 0.0542(5) Uani 1 1 d . . . H24A H 0.7635 0.0678 0.5072 0.065 Uiso 1 1 calc R . . C25 C 0.6110(3) 0.05704(11) 0.58520(11) 0.0536(5) Uani 1 1 d . . . H25A H 0.5979 0.0036 0.5816 0.064 Uiso 1 1 calc R . . C26 C 0.5327(3) 0.09818(12) 0.63452(11) 0.0567(5) Uani 1 1 d . . . H26A H 0.4660 0.0726 0.6657 0.068 Uiso 1 1 calc R . . C27 C 0.5496(3) 0.17612(12) 0.63936(10) 0.0500(5) Uani 1 1 d . . . H27A H 0.4931 0.2033 0.6732 0.060 Uiso 1 1 calc R . . O30 O 0.54126(19) 0.47386(10) 0.38244(7) 0.0612(4) Uani 1 1 d . . . C30 C 0.5699(3) 0.47238(12) 0.31866(11) 0.0519(5) Uani 1 1 d . . . H30A H 0.6384 0.5117 0.3036 0.062 Uiso 1 1 calc R . . N31 N 0.5153(2) 0.42207(10) 0.26987(9) 0.0505(4) Uani 1 1 d . . . C32 C 0.4178(5) 0.35791(18) 0.2893(2) 0.1072(13) Uani 1 1 d U . . H32A H 0.3418 0.3743 0.3237 0.161 Uiso 1 1 calc R . . H32B H 0.4932 0.3186 0.3120 0.161 Uiso 1 1 calc R . . H32C H 0.3524 0.3374 0.2454 0.161 Uiso 1 1 calc R . . C33 C 0.5521(4) 0.42805(17) 0.19530(13) 0.0774(8) Uani 1 1 d . . . H33A H 0.6295 0.4703 0.1914 0.116 Uiso 1 1 calc R . . H33B H 0.4480 0.4371 0.1629 0.116 Uiso 1 1 calc R . . H33C H 0.6035 0.3808 0.1813 0.116 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 Co 0.03223(16) 0.03714(16) 0.03401(15) 0.00605(11) 0.00997(11) 0.00421(11) Cl1 0.0389(2) 0.0419(2) 0.0557(3) 0.00029(18) 0.01655(18) 0.00582(16) Cl2 0.0342(2) 0.0484(2) 0.0419(2) -0.00043(17) 0.00560(16) 0.00051(16) N1 0.0352(7) 0.0374(7) 0.0282(6) 0.0020(5) 0.0088(5) -0.0002(6) C2 0.0512(11) 0.0432(9) 0.0280(8) 0.0025(7) 0.0086(7) -0.0053(8) C3 0.0391(9) 0.0393(9) 0.0314(8) 0.0042(6) 0.0111(7) 0.0024(7) N4 0.0423(8) 0.0327(7) 0.0322(7) 0.0031(5) 0.0078(6) 0.0014(6) C5 0.0427(9) 0.0339(8) 0.0390(9) 0.0038(7) 0.0127(7) 0.0038(7) C6 0.0563(11) 0.0376(9) 0.0449(10) -0.0008(8) 0.0107(8) 0.0006(8) C7 0.0656(14) 0.0366(9) 0.0611(13) -0.0026(9) 0.0167(10) -0.0049(9) C8 0.0655(14) 0.0342(10) 0.0702(14) 0.0078(9) 0.0250(11) 0.0033(9) C9 0.0541(12) 0.0436(10) 0.0546(11) 0.0171(9) 0.0177(9) 0.0075(9) C10 0.0433(10) 0.0375(9) 0.0428(9) 0.0065(7) 0.0138(7) 0.0044(7) N11 0.0453(8) 0.0433(8) 0.0330(7) 0.0091(6) 0.0086(6) 0.0024(6) C12 0.0328(8) 0.0443(9) 0.0286(8) 0.0030(7) 0.0046(6) 0.0024(7) C13 0.0327(8) 0.0370(8) 0.0299(8) 0.0012(6) 0.0066(6) 0.0020(6) N14 0.0310(7) 0.0391(7) 0.0278(6) 0.0013(5) 0.0059(5) 0.0013(6) C15 0.0366(9) 0.0341(8) 0.0270(8) 0.0015(6) 0.0062(6) -0.0014(6) C16 0.0367(9) 0.0451(9) 0.0344(8) 0.0030(7) 0.0025(7) -0.0043(7) C17 0.0501(11) 0.0477(10) 0.0295(8) 0.0022(7) 0.0019(8) -0.0066(8) C18 0.0544(12) 0.0446(10) 0.0293(8) 0.0002(7) 0.0106(8) -0.0021(8) C19 0.0428(10) 0.0480(10) 0.0338(9) 0.0023(7) 0.0143(7) 0.0035(7) C20 0.0382(9) 0.0361(8) 0.0294(8) 0.0020(6) 0.0080(7) 0.0016(6) N21 0.0283(7) 0.0509(8) 0.0315(7) 0.0025(6) 0.0058(6) 0.0035(6) C22 0.0367(9) 0.0392(9) 0.0297(8) 0.0018(6) 0.0025(6) -0.0021(7) C23 0.0490(11) 0.0425(10) 0.0531(11) 0.0015(8) 0.0204(9) 0.0000(8) C24 0.0610(13) 0.0439(11) 0.0605(12) -0.0043(9) 0.0190(10) 0.0031(9) C25 0.0723(14) 0.0375(9) 0.0499(11) 0.0029(8) 0.0039(10) -0.0049(9) C26 0.0859(16) 0.0478(11) 0.0386(10) 0.0037(8) 0.0161(10) -0.0171(11) C27 0.0718(14) 0.0475(10) 0.0333(9) -0.0026(8) 0.0168(9) -0.0131(10) O30 0.0567(9) 0.0851(11) 0.0411(7) -0.0134(7) 0.0031(6) -0.0034(8) C30 0.0518(12) 0.0495(11) 0.0540(12) -0.0069(9) 0.0052(9) -0.0049(9) N31 0.0526(10) 0.0503(9) 0.0481(9) -0.0131(7) 0.0049(7) -0.0050(7) C32 0.126(3) 0.095(2) 0.113(3) -0.0422(19) 0.063(2) -0.057(2) C33 0.091(2) 0.0909(19) 0.0515(13) -0.0207(13) 0.0144(13) -0.0135(15) _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 Co N4 2.0271(14) . ? Co N14 2.0293(14) . ? Co Cl1 2.2593(5) . ? Co Cl2 2.3082(5) . ? Co N1 2.7546(14) . ? N1 C22 1.430(2) . ? N1 C12 1.467(2) . ? N1 C2 1.468(2) . ? C2 C3 1.492(2) . ? C3 N4 1.326(2) . ? C3 N11 1.340(2) . ? N4 C5 1.403(2) . ? C5 C6 1.390(3) . ? C5 C10 1.397(2) . ? C6 C7 1.390(3) . ? C7 C8 1.391(3) . ? C8 C9 1.375(3) . ? C9 C10 1.394(2) . ? C10 N11 1.384(2) . ? N11 O30 2.690(2) . ? C12 C13 1.495(2) . ? C13 N14 1.323(2) . ? C13 N21 1.345(2) . ? N14 C15 1.408(2) . ? C15 C16 1.386(2) . ? C15 C20 1.393(2) . ? C16 C17 1.382(2) . ? C17 C18 1.399(3) . ? C18 C19 1.377(3) . ? C19 C20 1.397(2) . ? C20 N21 1.387(2) . ? C22 C23 1.387(3) . ? C22 C27 1.401(3) . ? C23 C24 1.383(3) . ? C24 C25 1.375(3) . ? C25 C26 1.380(3) . ? C26 C27 1.384(3) . ? O30 C30 1.232(2) . ? C30 N31 1.303(3) . ? N31 C32 1.448(3) . ? N31 C33 1.452(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 N4 Co N14 108.76(6) . . ? N4 Co Cl1 106.72(4) . . ? N14 Co Cl1 129.32(4) . . ? N4 Co Cl2 106.70(4) . . ? N14 Co Cl2 100.67(4) . . ? Cl1 Co Cl2 102.442(19) . . ? N4 Co N1 71.28(5) . . ? N14 Co N1 70.58(5) . . ? Cl1 Co N1 88.31(3) . . ? Cl2 Co N1 169.10(3) . . ? C22 N1 C12 114.61(14) . . ? C22 N1 C2 116.09(13) . . ? C12 N1 C2 112.25(14) . . ? C22 N1 Co 118.53(10) . . ? C12 N1 Co 95.60(9) . . ? C2 N1 Co 96.90(10) . . ? N1 C2 C3 110.31(14) . . ? N4 C3 N11 112.84(15) . . ? N4 C3 C2 124.12(14) . . ? N11 C3 C2 122.99(16) . . ? C3 N4 C5 105.28(13) . . ? C3 N4 Co 122.00(11) . . ? C5 N4 Co 132.54(12) . . ? C6 C5 C10 120.44(16) . . ? C6 C5 N4 131.05(16) . . ? C10 C5 N4 108.51(15) . . ? C7 C6 C5 117.14(18) . . ? C6 C7 C8 121.7(2) . . ? C9 C8 C7 121.78(18) . . ? C8 C9 C10 116.59(19) . . ? N11 C10 C9 131.76(18) . . ? N11 C10 C5 105.92(15) . . ? C9 C10 C5 122.32(18) . . ? C3 N11 C10 107.46(15) . . ? C3 N11 O30 125.68(13) . . ? C10 N11 O30 126.29(12) . . ? N1 C12 C13 110.46(13) . . ? N14 C13 N21 112.51(14) . . ? N14 C13 C12 124.54(15) . . ? N21 C13 C12 122.86(15) . . ? C13 N14 C15 105.66(13) . . ? C13 N14 Co 119.69(11) . . ? C15 N14 Co 131.14(11) . . ? C16 C15 C20 120.34(15) . . ? C16 C15 N14 131.38(16) . . ? C20 C15 N14 108.27(14) . . ? C17 C16 C15 117.65(17) . . ? C16 C17 C18 121.49(17) . . ? C19 C18 C17 121.65(16) . . ? C18 C19 C20 116.34(17) . . ? N21 C20 C15 106.06(14) . . ? N21 C20 C19 131.50(17) . . ? C15 C20 C19 122.43(16) . . ? C13 N21 C20 107.46(14) . . ? C23 C22 C27 117.37(17) . . ? C23 C22 N1 122.11(15) . . ? C27 C22 N1 120.51(16) . . ? C24 C23 C22 121.06(18) . . ? C25 C24 C23 121.33(19) . . ? C24 C25 C26 118.31(19) . . ? C25 C26 C27 121.07(19) . . ? C26 C27 C22 120.85(19) . . ? C30 O30 N11 131.49(14) . . ? O30 C30 N31 126.3(2) . . ? C30 N31 C32 120.4(2) . . ? C30 N31 C33 121.2(2) . . ? C32 N31 C33 118.4(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 71.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.407 _refine_diff_density_min -0.307 _refine_diff_density_rms 0.040 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 762755' #TrackingRef '- Dalton04-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H21 Cl Co N7, Cl, 2(C3 H7 N O), 0.25(C4 H10 O)' _chemical_formula_sum 'C31 H37.50 Cl2 Co N9 O2.25' _chemical_formula_weight 702.03 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' 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3900(4) _cell_length_b 15.7696(4) _cell_length_c 15.8027(4) _cell_angle_alpha 68.049(2) _cell_angle_beta 70.125(2) _cell_angle_gamma 77.034(2) _cell_volume 3324.43(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 15079 _cell_measurement_theta_min 4.1021 _cell_measurement_theta_max 31.9706 _exptl_crystal_description 'blocky needles' _exptl_crystal_colour Purple _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1462 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.768 _exptl_absorpt_correction_T_max 0.924 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45498 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0815 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.11 _diffrn_reflns_theta_max 32.05 _reflns_number_total 20849 _reflns_number_gt 11658 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0321P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20849 _refine_ls_number_parameters 935 _refine_ls_number_restraints 323 _refine_ls_R_factor_all 0.0800 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0655 _refine_ls_goodness_of_fit_ref 0.806 _refine_ls_restrained_S_all 0.811 _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 Co Co 0.592926(14) 0.252652(13) 0.327781(13) 0.02385(5) Uani 1 1 d . . . Cl Cl 0.60780(3) 0.11244(3) 0.44122(3) 0.03281(9) Uani 1 1 d . . . N1 N 0.57476(8) 0.39852(8) 0.21061(8) 0.0252(3) Uani 1 1 d . . . C2 C 0.48818(11) 0.44764(10) 0.25439(10) 0.0299(3) Uani 1 1 d . . . H2A H 0.4345 0.4326 0.2437 0.036 Uiso 1 1 calc R . . H2B H 0.4909 0.5149 0.2257 0.036 Uiso 1 1 calc R . . C3 C 0.47754(11) 0.41831(10) 0.35863(10) 0.0280(3) Uani 1 1 d . . . N4 N 0.52055(9) 0.33984(9) 0.40273(8) 0.0277(3) Uani 1 1 d . . . C5 C 0.49397(11) 0.33592(11) 0.49842(10) 0.0296(4) Uani 1 1 d . . . C6 C 0.51854(12) 0.26951(12) 0.57648(11) 0.0359(4) Uani 1 1 d . . . H6A H 0.5591 0.2155 0.5710 0.043 Uiso 1 1 calc R . . C7 C 0.48091(13) 0.28601(13) 0.66274(11) 0.0429(5) Uani 1 1 d . . . H7A H 0.4964 0.2424 0.7176 0.052 Uiso 1 1 calc R . . C8 C 0.42123(14) 0.36452(13) 0.67111(12) 0.0475(5) Uani 1 1 d . . . H8A H 0.3974 0.3733 0.7315 0.057 Uiso 1 1 calc R . . C9 C 0.39567(13) 0.42969(13) 0.59504(12) 0.0431(5) Uani 1 1 d . . . H9A H 0.3541 0.4829 0.6014 0.052 Uiso 1 1 calc R . . C10 C 0.43373(11) 0.41413(11) 0.50754(11) 0.0332(4) Uani 1 1 d . . . N11 N 0.42463(10) 0.46504(9) 0.41767(9) 0.0321(3) Uani 1 1 d D . . H11 H 0.3903(10) 0.5197(6) 0.4019(11) 0.042(5) Uiso 1 1 d D . . C12 C 0.57037(11) 0.38011(10) 0.12749(10) 0.0283(3) Uani 1 1 d . . . H12A H 0.6334 0.3766 0.0830 0.034 Uiso 1 1 calc R . . H12B H 0.5306 0.4305 0.0935 0.034 Uiso 1 1 calc R . . C13 C 0.53114(10) 0.29152(10) 0.16094(10) 0.0247(3) Uani 1 1 d . . . N14 N 0.52992(8) 0.22930(8) 0.24557(8) 0.0249(3) Uani 1 1 d . . . C15 C 0.49286(10) 0.15446(10) 0.24865(10) 0.0258(3) Uani 1 1 d . . . C16 C 0.47336(11) 0.07090(11) 0.32003(11) 0.0323(4) Uani 1 1 d . . . H16A H 0.4862 0.0556 0.3790 0.039 Uiso 1 1 calc R . . C17 C 0.43459(13) 0.01107(12) 0.30165(12) 0.0418(4) Uani 1 1 d . . . H17A H 0.4203 -0.0464 0.3493 0.050 Uiso 1 1 calc R . . C18 C 0.41572(13) 0.03253(12) 0.21501(12) 0.0428(4) Uani 1 1 d . . . H18A H 0.3898 -0.0109 0.2048 0.051 Uiso 1 1 calc R . . C19 C 0.43397(11) 0.11541(11) 0.14413(11) 0.0344(4) Uani 1 1 d . . . H19A H 0.4204 0.1308 0.0854 0.041 Uiso 1 1 calc R . . C20 C 0.47300(10) 0.17510(10) 0.16272(10) 0.0271(3) Uani 1 1 d . . . N21 N 0.49834(9) 0.26281(9) 0.10877(8) 0.0272(3) Uani 1 1 d D . . H21 H 0.4865(11) 0.2953(10) 0.0527(6) 0.041(5) Uiso 1 1 d D . . C22 C 0.65841(11) 0.44190(10) 0.18963(11) 0.0295(3) Uani 1 1 d . . . H22A H 0.6492 0.4738 0.2359 0.035 Uiso 1 1 calc R . . H22B H 0.6711 0.4877 0.1249 0.035 Uiso 1 1 calc R . . C23 C 0.73766(11) 0.36794(10) 0.19634(10) 0.0259(3) Uani 1 1 d . . . N24 N 0.72498(8) 0.28293(8) 0.25446(8) 0.0254(3) Uani 1 1 d . . . C25 C 0.81310(10) 0.23382(10) 0.24313(10) 0.0249(3) Uani 1 1 d . . . C26 C 0.84214(11) 0.14129(10) 0.28468(11) 0.0298(3) Uani 1 1 d . . . H26A H 0.7989 0.0998 0.3295 0.036 Uiso 1 1 calc R . . C27 C 0.93493(12) 0.11271(11) 0.25854(12) 0.0374(4) Uani 1 1 d . . . H27A H 0.9562 0.0501 0.2859 0.045 Uiso 1 1 calc R . . C28 C 0.99974(12) 0.17306(12) 0.19248(12) 0.0406(4) Uani 1 1 d . . . H28A H 1.0638 0.1505 0.1766 0.049 Uiso 1 1 calc R . . C29 C 0.97235(12) 0.26476(12) 0.15001(11) 0.0354(4) Uani 1 1 d . . . H29A H 1.0159 0.3059 0.1050 0.042 Uiso 1 1 calc R . . C30 C 0.87825(11) 0.29336(10) 0.17641(10) 0.0266(3) Uani 1 1 d . . . N31 N 0.82734(9) 0.37819(9) 0.14893(9) 0.0283(3) Uani 1 1 d D . . H31 H 0.8485(12) 0.4263(8) 0.0977(8) 0.056(6) Uiso 1 1 d D . . Co' Co 0.930324(15) 0.272852(14) 0.724032(14) 0.02648(5) Uani 1 1 d . . . Cl' Cl 1.01742(3) 0.14894(3) 0.68296(3) 0.04173(11) Uani 1 1 d . . . N1' N 0.83211(9) 0.39815(8) 0.76691(8) 0.0266(3) Uani 1 1 d . . . C2' C 0.85175(12) 0.48107(10) 0.68308(10) 0.0316(4) Uani 1 1 d . . . H2'A H 0.9029 0.5093 0.6835 0.038 Uiso 1 1 calc R . . H2'B H 0.7959 0.5268 0.6838 0.038 Uiso 1 1 calc R . . C3' C 0.87869(11) 0.45317(10) 0.59695(10) 0.0285(3) Uani 1 1 d . . . N4' N 0.92005(9) 0.37028(9) 0.59646(8) 0.0286(3) Uani 1 1 d . . . C5' C 0.93745(11) 0.37198(11) 0.50218(10) 0.0282(3) Uani 1 1 d . . . C6' C 0.97936(12) 0.30470(12) 0.45942(11) 0.0372(4) Uani 1 1 d . . . H6'A H 1.0037 0.2459 0.4939 0.045 Uiso 1 1 calc R . . C7' C 0.98418(13) 0.32672(13) 0.36477(11) 0.0418(4) Uani 1 1 d . . . H7'A H 1.0128 0.2822 0.3336 0.050 Uiso 1 1 calc R . . C8' C 0.94789(13) 0.41303(13) 0.31370(12) 0.0441(5) Uani 1 1 d . . . H8'A H 0.9519 0.4254 0.2489 0.053 Uiso 1 1 calc R . . C9' C 0.90666(13) 0.48014(12) 0.35506(11) 0.0408(4) Uani 1 1 d . . . H9'A H 0.8820 0.5387 0.3204 0.049 Uiso 1 1 calc R . . C10' C 0.90262(11) 0.45871(11) 0.45020(10) 0.0314(4) Uani 1 1 d . . . N11' N 0.86658(10) 0.50841(9) 0.51217(9) 0.0328(3) Uani 1 1 d D . . H11' H 0.8351(10) 0.5649(5) 0.5055(11) 0.042(5) Uiso 1 1 d D . . C12' C 0.85504(11) 0.40384(11) 0.84791(10) 0.0303(4) Uani 1 1 d . . . H12C H 0.8138 0.3684 0.9086 0.036 Uiso 1 1 calc R . . H12D H 0.8460 0.4687 0.8457 0.036 Uiso 1 1 calc R . . C13' C 0.95397(10) 0.36533(10) 0.84166(10) 0.0258(3) Uani 1 1 d . . . N14' N 0.99836(9) 0.30636(8) 0.79505(8) 0.0263(3) Uani 1 1 d . . . C15' C 1.08560(10) 0.28089(10) 0.81190(10) 0.0264(3) Uani 1 1 d . . . C16' C 1.16044(11) 0.22080(11) 0.78125(11) 0.0330(4) Uani 1 1 d . . . H16B H 1.1577 0.1884 0.7424 0.040 Uiso 1 1 calc R . . C17' C 1.23836(12) 0.21022(12) 0.80944(12) 0.0397(4) Uani 1 1 d . . . H17B H 1.2903 0.1692 0.7899 0.048 Uiso 1 1 calc R . . C18' C 1.24378(12) 0.25797(12) 0.86613(12) 0.0377(4) Uani 1 1 d . . . H18B H 1.2992 0.2488 0.8838 0.045 Uiso 1 1 calc R . . C19' C 1.17023(11) 0.31806(11) 0.89679(11) 0.0338(4) Uani 1 1 d . . . H19B H 1.1735 0.3509 0.9350 0.041 Uiso 1 1 calc R . . C20' C 1.09130(11) 0.32798(10) 0.86887(10) 0.0268(3) Uani 1 1 d . . . N21' N 1.00600(9) 0.38101(9) 0.88648(8) 0.0279(3) Uani 1 1 d D . . H21' H 0.9864(11) 0.4238(8) 0.9159(10) 0.043(5) Uiso 1 1 d D . . C22' C 0.73605(11) 0.37711(11) 0.79191(11) 0.0312(4) Uani 1 1 d . . . H22C H 0.7136 0.4016 0.7346 0.037 Uiso 1 1 calc R . . H22D H 0.6944 0.4061 0.8393 0.037 Uiso 1 1 calc R . . C23' C 0.73541(11) 0.27569(11) 0.83193(10) 0.0286(3) Uani 1 1 d . . . N24' N 0.81142(9) 0.21760(8) 0.81861(8) 0.0275(3) Uani 1 1 d . . . C25' C 0.78245(11) 0.12978(11) 0.86541(10) 0.0298(4) Uani 1 1 d . . . C26' C 0.83239(12) 0.04274(11) 0.87749(11) 0.0358(4) Uani 1 1 d . . . H26B H 0.8977 0.0354 0.8499 0.043 Uiso 1 1 calc R . . C27' C 0.78331(13) -0.03246(12) 0.93117(12) 0.0425(4) Uani 1 1 d . . . H27B H 0.8158 -0.0925 0.9408 0.051 Uiso 1 1 calc R . . C28' C 0.68736(14) -0.02245(13) 0.97147(12) 0.0456(5) Uani 1 1 d . . . H28B H 0.6561 -0.0758 1.0085 0.055 Uiso 1 1 calc R . . C29' C 0.63683(13) 0.06306(13) 0.95883(12) 0.0412(4) Uani 1 1 d . . . H29B H 0.5712 0.0699 0.9851 0.049 Uiso 1 1 calc R . . C30' C 0.68621(11) 0.13889(11) 0.90582(11) 0.0318(4) Uani 1 1 d . . . N31' N 0.65872(9) 0.23237(10) 0.88279(9) 0.0320(3) Uani 1 1 d D . . H31' H 0.6007(5) 0.2607(10) 0.8975(11) 0.044(5) Uiso 1 1 d D . . Cl2 Cl 0.89008(3) 0.53676(3) -0.03494(3) 0.03309(9) Uani 1 1 d . . . Cl3 Cl 0.45501(3) 0.32677(3) 0.91510(3) 0.03681(10) Uani 1 1 d . . . O40 O 0.3123(5) 0.62862(18) 0.3903(3) 0.0461(9) Uani 0.911(3) 1 d PDU A 1 C40 C 0.28099(13) 0.66275(14) 0.45502(15) 0.0402(5) Uani 0.911(3) 1 d PDU A 1 H40 H 0.2770 0.6222 0.5179 0.048 Uiso 0.911(3) 1 calc PR A 1 N41 N 0.2528(6) 0.7502(2) 0.4444(2) 0.0370(8) Uani 0.911(3) 1 d PDU A 1 C42 C 0.25507(19) 0.81581(15) 0.35161(15) 0.0598(7) Uani 0.911(3) 1 d PD A 1 H42A H 0.2921 0.7875 0.3029 0.090 Uiso 0.911(3) 1 calc PR A 1 H42B H 0.2831 0.8696 0.3427 0.090 Uiso 0.911(3) 1 calc PR A 1 H42C H 0.1916 0.8350 0.3460 0.090 Uiso 0.911(3) 1 calc PR A 1 C43 C 0.21691(17) 0.78410(18) 0.52506(16) 0.0558(7) Uani 0.911(3) 1 d PDU A 1 H43A H 0.2149 0.7323 0.5841 0.084 Uiso 0.911(3) 1 calc PR A 1 H43B H 0.1541 0.8157 0.5267 0.084 Uiso 0.911(3) 1 calc PR A 1 H43C H 0.2576 0.8272 0.5187 0.084 Uiso 0.911(3) 1 calc PR A 1 O40' O 0.301(5) 0.6270(16) 0.405(3) 0.029(6) Uiso 0.089(3) 1 d PDU A 2 C40' C 0.2879(15) 0.7139(14) 0.3768(14) 0.053(6) Uiso 0.089(3) 1 d PDU A 2 H40' H 0.3066 0.7468 0.3106 0.063 Uiso 0.089(3) 1 calc PR A 2 N41' N 0.248(7) 0.760(2) 0.438(2) 0.037(9) Uiso 0.089(3) 1 d PDU A 2 C42' C 0.2482(19) 0.7179(17) 0.5368(12) 0.064(8) Uiso 0.089(3) 1 d PD A 2 H42D H 0.2471 0.6514 0.5555 0.096 Uiso 0.089(3) 1 calc PR A 2 H42E H 0.1931 0.7438 0.5769 0.096 Uiso 0.089(3) 1 calc PR A 2 H42F H 0.3043 0.7298 0.5448 0.096 Uiso 0.089(3) 1 calc PR A 2 C43' C 0.222(2) 0.8585(13) 0.4062(18) 0.082(7) Uiso 0.089(3) 1 d PDU A 2 H43D H 0.2699 0.8908 0.4050 0.122 Uiso 0.089(3) 1 calc PR A 2 H43E H 0.1626 0.8737 0.4497 0.122 Uiso 0.089(3) 1 calc PR A 2 H43F H 0.2149 0.8774 0.3421 0.122 Uiso 0.089(3) 1 calc PR A 2 O50 O 0.7798(3) 0.68003(19) 0.5036(3) 0.0593(9) Uani 0.713(4) 1 d PDU B 1 C50 C 0.72842(19) 0.73494(17) 0.45652(18) 0.0456(8) Uani 0.713(4) 1 d PDU B 1 H50A H 0.7010 0.7110 0.4258 0.055 Uiso 0.713(4) 1 calc PR B 1 N51 N 0.7085(2) 0.82342(16) 0.44542(19) 0.0364(7) Uani 0.713(4) 1 d PDU B 1 C52 C 0.7523(2) 0.8672(3) 0.4860(2) 0.0563(9) Uani 0.713(4) 1 d PD B 1 H52A H 0.7971 0.8217 0.5161 0.084 Uiso 0.713(4) 1 calc PR B 1 H52B H 0.7044 0.8909 0.5337 0.084 Uiso 0.713(4) 1 calc PR B 1 H52C H 0.7846 0.9181 0.4353 0.084 Uiso 0.713(4) 1 calc PR B 1 C53 C 0.64338(19) 0.8820(2) 0.3956(2) 0.0511(8) Uani 0.713(4) 1 d PD B 1 H53A H 0.6216 0.8468 0.3686 0.077 Uiso 0.713(4) 1 calc PR B 1 H53B H 0.6737 0.9338 0.3443 0.077 Uiso 0.713(4) 1 calc PR B 1 H53C H 0.5904 0.9053 0.4399 0.077 Uiso 0.713(4) 1 calc PR B 1 O50' O 0.7615(7) 0.6690(6) 0.4937(7) 0.047(2) Uiso 0.287(4) 1 d PDU B 2 C50' C 0.7879(4) 0.7421(4) 0.4807(4) 0.0333(16) Uiso 0.287(4) 1 d PDU B 2 H50B H 0.8495 0.7427 0.4807 0.040 Uiso 0.287(4) 1 calc PR B 2 N51' N 0.7301(5) 0.8225(5) 0.4662(6) 0.0317(19) Uiso 0.287(4) 1 d PDU B 2 C52' C 0.6364(6) 0.8223(7) 0.4744(8) 0.098(4) Uiso 0.287(4) 1 d PD B 2 H52D H 0.6318 0.8150 0.4172 0.147 Uiso 0.287(4) 1 calc PR B 2 H52E H 0.6014 0.8806 0.4814 0.147 Uiso 0.287(4) 1 calc PR B 2 H52F H 0.6107 0.7712 0.5304 0.147 Uiso 0.287(4) 1 calc PR B 2 C53' C 0.7613(7) 0.9073(6) 0.4462(8) 0.082(4) Uiso 0.287(4) 1 d PD B 2 H53D H 0.7264 0.9332 0.4972 0.123 Uiso 0.287(4) 1 calc PR B 2 H53E H 0.7514 0.9500 0.3857 0.123 Uiso 0.287(4) 1 calc PR B 2 H53F H 0.8277 0.8977 0.4416 0.123 Uiso 0.287(4) 1 calc PR B 2 O60 O 0.7602(5) 0.2573(4) 1.0420(5) 0.0443(12) Uani 0.531(3) 1 d PDU C 1 C60 C 0.7524(3) 0.1704(3) 1.0837(2) 0.0504(11) Uani 0.531(3) 1 d PDU C 1 H60A H 0.6929 0.1495 1.1163 0.060 Uiso 0.531(3) 1 calc PR C 1 N61 N 0.8285(6) 0.1109(4) 1.0804(9) 0.0392(17) Uani 0.531(3) 1 d PDU C 1 C62 C 0.9167(2) 0.1407(3) 1.0187(3) 0.0514(11) Uani 0.531(3) 1 d PD C 1 H62A H 0.9311 0.1260 0.9601 0.077 Uiso 0.531(3) 1 calc PR C 1 H62B H 0.9651 0.1091 1.0507 0.077 Uiso 0.531(3) 1 calc PR C 1 H62C H 0.9141 0.2073 1.0033 0.077 Uiso 0.531(3) 1 calc PR C 1 C63 C 0.8253(4) 0.0128(2) 1.1318(3) 0.0715(15) Uani 0.531(3) 1 d PDU C 1 H63A H 0.7606 0.0008 1.1661 0.107 Uiso 0.531(3) 1 calc PR C 1 H63B H 0.8619 -0.0068 1.1772 0.107 Uiso 0.531(3) 1 calc PR C 1 H63C H 0.8511 -0.0216 1.0866 0.107 Uiso 0.531(3) 1 calc PR C 1 O60' O 0.7421(6) 0.2489(5) 1.0421(7) 0.045(2) Uiso 0.469(3) 1 d PDU C 2 C60' C 0.8207(3) 0.1949(3) 1.0418(3) 0.0439(11) Uiso 0.469(3) 1 d PDU C 2 H60B H 0.8790 0.2186 1.0099 0.053 Uiso 0.469(3) 1 calc PR C 2 N61' N 0.8150(7) 0.1050(6) 1.0882(12) 0.044(2) Uiso 0.469(3) 1 d PDU C 2 C62' C 0.7282(3) 0.0726(3) 1.1505(3) 0.0649(14) Uiso 0.469(3) 1 d PD C 2 H62D H 0.7313 0.0486 1.2164 0.097 Uiso 0.469(3) 1 calc PR C 2 H62E H 0.7156 0.0236 1.1337 0.097 Uiso 0.469(3) 1 calc PR C 2 H62F H 0.6782 0.1235 1.1440 0.097 Uiso 0.469(3) 1 calc PR C 2 C63' C 0.8987(4) 0.0395(4) 1.0841(4) 0.0685(15) Uiso 0.469(3) 1 d PDU C 2 H63D H 0.9522 0.0712 1.0384 0.103 Uiso 0.469(3) 1 calc PR C 2 H63E H 0.8910 -0.0095 1.0640 0.103 Uiso 0.469(3) 1 calc PR C 2 H63F H 0.9090 0.0127 1.1472 0.103 Uiso 0.469(3) 1 calc PR C 2 O70 O 0.66103(9) 0.56168(9) 0.84929(10) 0.0563(4) Uani 1 1 d . . . C70 C 0.69346(12) 0.60930(12) 0.87453(14) 0.0401(4) Uani 1 1 d . . . H70A H 0.6916 0.5892 0.9397 0.048 Uiso 1 1 calc R . . N71 N 0.73101(10) 0.68665(10) 0.81855(10) 0.0421(4) Uani 1 1 d . . . C72 C 0.73718(15) 0.72146(15) 0.71790(14) 0.0609(6) Uani 1 1 d . . . H72A H 0.8021 0.7130 0.6808 0.091 Uiso 1 1 calc R . . H72B H 0.7142 0.7871 0.6999 0.091 Uiso 1 1 calc R . . H72C H 0.6994 0.6878 0.7051 0.091 Uiso 1 1 calc R . . C73 C 0.77102(14) 0.73620(13) 0.85422(15) 0.0556(5) Uani 1 1 d . . . H73A H 0.7547 0.7109 0.9238 0.083 Uiso 1 1 calc R . . H73B H 0.7467 0.8014 0.8350 0.083 Uiso 1 1 calc R . . H73C H 0.8388 0.7299 0.8280 0.083 Uiso 1 1 calc R . . O80 O 1.0185(5) -0.0290(5) 0.4942(6) 0.107(2) Uiso 0.386(4) 1 d PDU D -1 C81 C 1.0580(8) 0.0543(8) 0.4485(8) 0.128(4) Uiso 0.386(4) 1 d PDU D -1 H81A H 1.0733 0.0723 0.4950 0.154 Uiso 0.386(4) 1 calc PR D -1 H81B H 1.0130 0.1035 0.4210 0.154 Uiso 0.386(4) 1 calc PR D -1 C82 C 1.1424(9) 0.0433(10) 0.3730(9) 0.145(6) Uiso 0.386(4) 1 d PDU D -1 H82A H 1.1684 0.1022 0.3388 0.218 Uiso 0.386(4) 1 calc PR D -1 H82B H 1.1272 0.0230 0.3287 0.218 Uiso 0.386(4) 1 calc PR D -1 H82C H 1.1881 -0.0028 0.4010 0.218 Uiso 0.386(4) 1 calc PR D -1 C83 C 0.9247(7) -0.0324(11) 0.5133(8) 0.154(5) Uiso 0.386(4) 1 d PDU D -1 H83A H 0.9165 -0.0748 0.4843 0.185 Uiso 0.386(4) 1 calc PR D -1 H83B H 0.8959 0.0296 0.4831 0.185 Uiso 0.386(4) 1 calc PR D -1 C84 C 0.8779(9) -0.0617(9) 0.6116(8) 0.108(4) Uiso 0.386(4) 1 d PDU D -1 H84A H 0.8179 -0.0807 0.6214 0.161 Uiso 0.386(4) 1 calc PR D -1 H84B H 0.8677 -0.0109 0.6367 0.161 Uiso 0.386(4) 1 calc PR D -1 H84C H 0.9157 -0.1137 0.6449 0.161 Uiso 0.386(4) 1 calc PR D -1 O80' O 1.0592(12) 0.0005(13) 0.4518(14) 0.071(5) Uiso 0.114(4) 1 d PDU D -2 C81' C 1.1144(19) 0.0716(16) 0.426(3) 0.115(7) Uiso 0.114(4) 1 d PDU D -2 H81C H 1.0828 0.1154 0.4610 0.138 Uiso 0.114(4) 1 calc PR D -2 H81D H 1.1278 0.1056 0.3565 0.138 Uiso 0.114(4) 1 calc PR D -2 C82' C 1.1989(19) 0.025(3) 0.450(3) 0.183(11) Uiso 0.114(4) 1 d PDU D -2 H82D H 1.2452 0.0684 0.4248 0.275 Uiso 0.114(4) 1 calc PR D -2 H82E H 1.2231 -0.0255 0.4237 0.275 Uiso 0.114(4) 1 calc PR D -2 H82F H 1.1856 -0.0001 0.5199 0.275 Uiso 0.114(4) 1 calc PR D -2 C83' C 0.9664(13) 0.039(2) 0.4769(16) 0.097(7) Uiso 0.114(4) 1 d PDU D -2 H83C H 0.9280 0.0176 0.4516 0.117 Uiso 0.114(4) 1 calc PR D -2 H83D H 0.9628 0.1073 0.4495 0.117 Uiso 0.114(4) 1 calc PR D -2 C84' C 0.932(2) 0.012(3) 0.5801(16) 0.134(11) Uiso 0.114(4) 1 d PDU D -2 H84D H 0.8844 -0.0297 0.6027 0.201 Uiso 0.114(4) 1 calc PR D -2 H84E H 0.9050 0.0666 0.5995 0.201 Uiso 0.114(4) 1 calc PR D -2 H84F H 0.9835 -0.0196 0.6076 0.201 Uiso 0.114(4) 1 calc PR D -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 Co 0.02665(11) 0.02227(11) 0.01959(10) -0.00294(8) -0.00756(8) -0.00209(8) Cl 0.0388(2) 0.0269(2) 0.02690(19) 0.00239(16) -0.01341(16) -0.00547(17) N1 0.0282(7) 0.0234(6) 0.0223(6) -0.0056(5) -0.0081(5) -0.0015(5) C2 0.0330(9) 0.0241(8) 0.0299(8) -0.0068(7) -0.0117(7) 0.0026(7) C3 0.0285(9) 0.0274(8) 0.0279(8) -0.0093(7) -0.0062(6) -0.0050(7) N4 0.0305(7) 0.0270(7) 0.0229(6) -0.0068(5) -0.0065(5) -0.0021(6) C5 0.0292(9) 0.0344(9) 0.0257(8) -0.0093(7) -0.0043(6) -0.0107(7) C6 0.0404(10) 0.0385(10) 0.0269(8) -0.0061(7) -0.0076(7) -0.0120(8) C7 0.0578(12) 0.0461(11) 0.0244(8) -0.0050(8) -0.0090(8) -0.0204(10) C8 0.0655(14) 0.0497(12) 0.0275(9) -0.0159(9) 0.0024(9) -0.0254(10) C9 0.0529(12) 0.0403(10) 0.0352(9) -0.0197(8) 0.0017(8) -0.0124(9) C10 0.0369(10) 0.0329(9) 0.0295(8) -0.0098(7) -0.0045(7) -0.0120(7) N11 0.0345(8) 0.0271(8) 0.0332(7) -0.0122(6) -0.0071(6) -0.0004(6) C12 0.0340(9) 0.0259(8) 0.0208(7) -0.0029(6) -0.0089(6) -0.0018(7) C13 0.0250(8) 0.0251(8) 0.0217(7) -0.0069(6) -0.0080(6) 0.0027(6) N14 0.0280(7) 0.0230(6) 0.0197(6) -0.0024(5) -0.0081(5) -0.0009(5) C15 0.0259(8) 0.0252(8) 0.0249(7) -0.0068(6) -0.0082(6) -0.0009(6) C16 0.0385(10) 0.0300(9) 0.0267(8) -0.0030(7) -0.0137(7) -0.0046(7) C17 0.0569(12) 0.0324(9) 0.0362(9) -0.0016(8) -0.0175(8) -0.0151(9) C18 0.0542(12) 0.0384(10) 0.0440(10) -0.0128(9) -0.0191(9) -0.0139(9) C19 0.0382(10) 0.0387(10) 0.0293(8) -0.0114(8) -0.0128(7) -0.0045(8) C20 0.0259(8) 0.0279(8) 0.0240(7) -0.0065(7) -0.0066(6) -0.0005(6) N21 0.0322(7) 0.0276(7) 0.0192(6) -0.0040(6) -0.0104(5) 0.0001(6) C22 0.0357(9) 0.0216(8) 0.0284(8) -0.0027(6) -0.0111(7) -0.0038(7) C23 0.0319(9) 0.0243(8) 0.0209(7) -0.0048(6) -0.0090(6) -0.0044(6) N24 0.0287(7) 0.0201(6) 0.0233(6) -0.0025(5) -0.0075(5) -0.0025(5) C25 0.0277(8) 0.0256(8) 0.0223(7) -0.0087(6) -0.0073(6) -0.0026(6) C26 0.0312(9) 0.0259(8) 0.0299(8) -0.0071(7) -0.0082(7) -0.0028(7) C27 0.0383(10) 0.0279(9) 0.0454(10) -0.0141(8) -0.0140(8) 0.0045(7) C28 0.0286(9) 0.0411(10) 0.0509(11) -0.0216(9) -0.0070(8) 0.0032(8) C29 0.0310(9) 0.0394(10) 0.0350(9) -0.0142(8) -0.0026(7) -0.0091(7) C30 0.0290(9) 0.0271(8) 0.0254(7) -0.0107(7) -0.0074(6) -0.0029(6) N31 0.0306(8) 0.0249(7) 0.0249(7) -0.0035(6) -0.0042(6) -0.0081(6) Co' 0.03195(12) 0.02286(11) 0.02406(10) -0.00971(9) -0.00810(9) 0.00196(9) Cl' 0.0528(3) 0.0283(2) 0.0385(2) -0.01690(18) -0.00697(19) 0.00734(19) N1' 0.0303(7) 0.0256(7) 0.0246(6) -0.0095(5) -0.0099(5) 0.0010(5) C2' 0.0391(10) 0.0241(8) 0.0326(8) -0.0114(7) -0.0129(7) 0.0027(7) C3' 0.0338(9) 0.0253(8) 0.0273(8) -0.0074(7) -0.0106(7) -0.0037(7) N4' 0.0329(7) 0.0268(7) 0.0264(7) -0.0109(6) -0.0083(5) -0.0005(6) C5' 0.0307(9) 0.0313(9) 0.0229(7) -0.0094(7) -0.0053(6) -0.0068(7) C6' 0.0407(10) 0.0386(10) 0.0320(9) -0.0140(8) -0.0082(7) -0.0027(8) C7' 0.0503(12) 0.0464(11) 0.0320(9) -0.0205(9) -0.0055(8) -0.0081(9) C8' 0.0586(12) 0.0514(12) 0.0255(8) -0.0093(8) -0.0098(8) -0.0210(10) C9' 0.0536(12) 0.0383(10) 0.0286(9) 0.0000(8) -0.0149(8) -0.0154(9) C10' 0.0376(10) 0.0298(9) 0.0259(8) -0.0051(7) -0.0084(7) -0.0099(7) N11' 0.0426(9) 0.0232(7) 0.0298(7) -0.0031(6) -0.0132(6) -0.0033(6) C12' 0.0315(9) 0.0338(9) 0.0288(8) -0.0171(7) -0.0105(7) 0.0054(7) C13' 0.0297(9) 0.0251(8) 0.0199(7) -0.0068(6) -0.0076(6) 0.0022(6) N14' 0.0279(7) 0.0244(7) 0.0243(6) -0.0089(5) -0.0065(5) 0.0020(5) C15' 0.0274(8) 0.0243(8) 0.0234(7) -0.0057(6) -0.0051(6) -0.0019(6) C16' 0.0303(9) 0.0301(9) 0.0381(9) -0.0169(7) -0.0056(7) 0.0009(7) C17' 0.0279(9) 0.0371(10) 0.0520(11) -0.0193(9) -0.0088(8) 0.0046(7) C18' 0.0299(9) 0.0393(10) 0.0445(10) -0.0121(8) -0.0142(8) -0.0019(8) C19' 0.0360(10) 0.0338(9) 0.0314(8) -0.0087(7) -0.0113(7) -0.0040(7) C20' 0.0293(9) 0.0235(8) 0.0231(7) -0.0048(6) -0.0062(6) -0.0009(6) N21' 0.0322(8) 0.0260(7) 0.0254(7) -0.0106(6) -0.0088(6) 0.0021(6) C22' 0.0324(9) 0.0310(9) 0.0334(8) -0.0153(7) -0.0141(7) 0.0062(7) C23' 0.0325(9) 0.0322(9) 0.0252(8) -0.0135(7) -0.0115(7) 0.0007(7) N24' 0.0309(7) 0.0250(7) 0.0273(6) -0.0114(6) -0.0084(5) 0.0012(6) C25' 0.0375(10) 0.0300(9) 0.0244(8) -0.0110(7) -0.0095(7) -0.0033(7) C26' 0.0414(10) 0.0323(9) 0.0307(8) -0.0103(7) -0.0090(7) -0.0003(8) C27' 0.0579(13) 0.0295(9) 0.0372(9) -0.0099(8) -0.0117(9) -0.0040(8) C28' 0.0569(13) 0.0396(11) 0.0393(10) -0.0116(9) -0.0065(9) -0.0170(9) C29' 0.0388(10) 0.0483(11) 0.0382(9) -0.0162(9) -0.0064(8) -0.0111(9) C30' 0.0363(10) 0.0353(9) 0.0275(8) -0.0142(7) -0.0099(7) -0.0026(7) N31' 0.0284(8) 0.0371(8) 0.0323(7) -0.0158(6) -0.0091(6) 0.0016(6) Cl2 0.0420(2) 0.02399(19) 0.03003(19) -0.00794(16) -0.00906(17) -0.00071(16) Cl3 0.0337(2) 0.0454(2) 0.02592(19) -0.00440(18) -0.01328(16) 0.00101(18) O40 0.049(3) 0.0453(12) 0.056(2) -0.0285(11) -0.022(2) 0.0037(9) C40 0.0416(12) 0.0413(12) 0.0428(12) -0.0107(10) -0.0189(9) -0.0084(9) N41 0.0399(16) 0.0426(15) 0.0392(13) -0.0215(11) -0.0179(11) -0.0005(14) C42 0.0918(19) 0.0438(14) 0.0550(14) -0.0197(12) -0.0376(13) 0.0037(12) C43 0.0539(15) 0.0731(18) 0.0575(14) -0.0421(13) -0.0112(11) -0.0105(13) O50 0.086(2) 0.0275(14) 0.0618(17) -0.0106(11) -0.0332(16) 0.0111(13) C50 0.0536(19) 0.0304(15) 0.0431(15) -0.0095(12) -0.0054(13) -0.0035(12) N51 0.0420(17) 0.0273(12) 0.0341(14) -0.0094(10) -0.0045(12) -0.0036(10) C52 0.062(2) 0.059(2) 0.0421(18) -0.0173(18) -0.0221(15) 0.0163(17) C53 0.0457(17) 0.0503(18) 0.0587(19) -0.0217(15) -0.0173(14) 0.0032(13) O60 0.048(3) 0.041(2) 0.041(2) -0.0144(15) -0.013(2) 0.003(2) C60 0.058(3) 0.058(3) 0.0343(19) -0.0140(19) -0.0077(18) -0.015(2) N61 0.053(4) 0.033(2) 0.036(3) -0.0153(18) -0.017(3) 0.002(2) C62 0.047(2) 0.054(2) 0.048(2) -0.0149(19) -0.0127(18) -0.0024(18) C63 0.124(4) 0.036(2) 0.056(2) -0.006(2) -0.034(3) -0.012(2) O70 0.0471(8) 0.0482(8) 0.0930(10) -0.0409(8) -0.0340(7) 0.0108(6) C70 0.0295(10) 0.0377(10) 0.0553(11) -0.0207(9) -0.0169(8) 0.0092(8) N71 0.0354(9) 0.0429(9) 0.0491(9) -0.0149(8) -0.0185(7) 0.0038(7) C72 0.0511(13) 0.0690(15) 0.0538(13) -0.0182(11) -0.0150(10) 0.0077(11) C73 0.0529(13) 0.0393(11) 0.0826(15) -0.0139(11) -0.0375(11) -0.0024(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 Co N24 2.0302(12) . ? Co N14 2.0342(12) . ? Co N4 2.0414(13) . ? Co Cl 2.2899(4) . ? Co N1 2.3826(12) . ? N1 C2 1.4714(19) . ? N1 C12 1.4728(18) . ? N1 C22 1.4732(19) . ? C2 C3 1.495(2) . ? C3 N4 1.3253(19) . ? C3 N11 1.3433(19) . ? N4 C5 1.4067(18) . ? C5 C10 1.389(2) . ? C5 C6 1.391(2) . ? C6 C7 1.386(2) . ? C7 C8 1.387(3) . ? C8 C9 1.368(3) . ? C9 C10 1.398(2) . ? C10 N11 1.383(2) . ? C12 C13 1.485(2) . ? C13 N14 1.3273(17) . ? C13 N21 1.3429(19) . ? N14 C15 1.4004(19) . ? C15 C16 1.391(2) . ? C15 C20 1.397(2) . ? C16 C17 1.381(2) . ? C17 C18 1.398(2) . ? C18 C19 1.378(2) . ? C19 C20 1.383(2) . ? C20 N21 1.3880(19) . ? C22 C23 1.489(2) . ? C23 N24 1.3244(18) . ? C23 N31 1.3412(19) . ? N24 C25 1.3922(19) . ? C25 C26 1.397(2) . ? C25 C30 1.401(2) . ? C26 C27 1.365(2) . ? C27 C28 1.402(2) . ? C28 C29 1.383(2) . ? C29 C30 1.383(2) . ? C30 N31 1.385(2) . ? Co' N14' 2.0312(13) . ? Co' N24' 2.0552(12) . ? Co' N4' 2.0595(12) . ? Co' Cl' 2.2842(5) . ? Co' N1' 2.3690(12) . ? N1' C2' 1.4718(18) . ? N1' C22' 1.4754(19) . ? N1' C12' 1.4759(18) . ? C2' C3' 1.483(2) . ? C3' N4' 1.3209(19) . ? C3' N11' 1.3465(19) . ? N4' C5' 1.4123(18) . ? C5' C6' 1.390(2) . ? C5' C10' 1.401(2) . ? C6' C7' 1.382(2) . ? C7' C8' 1.400(3) . ? C8' C9' 1.373(2) . ? C9' C10' 1.394(2) . ? C10' N11' 1.375(2) . ? C12' C13' 1.492(2) . ? C13' N14' 1.3261(18) . ? C13' N21' 1.3452(19) . ? N14' C15' 1.3987(19) . ? C15' C16' 1.390(2) . ? C15' C20' 1.397(2) . ? C16' C17' 1.372(2) . ? C17' C18' 1.400(2) . ? C18' C19' 1.379(2) . ? C19' C20' 1.387(2) . ? C20' N21' 1.3903(19) . ? C22' C23' 1.485(2) . ? C23' N24' 1.3220(19) . ? C23' N31' 1.3460(19) . ? N24' C25' 1.3968(19) . ? C25' C26' 1.393(2) . ? C25' C30' 1.397(2) . ? C26' C27' 1.382(2) . ? C27' C28' 1.394(3) . ? C28' C29' 1.377(3) . ? C29' C30' 1.391(2) . ? C30' N31' 1.381(2) . ? O40 C40 1.237(4) . ? C40 N41 1.313(3) . ? N41 C42 1.439(3) . ? N41 C43 1.454(3) . ? O40' C40' 1.264(15) . ? C40' N41' 1.335(14) . ? N41' C43' 1.445(13) . ? N41' C42' 1.446(14) . ? O50 C50 1.241(4) . ? C50 N51 1.317(3) . ? N51 C53 1.434(4) . ? N51 C52 1.475(4) . ? O50' C50' 1.231(9) . ? C50' N51' 1.366(8) . ? N51' C52' 1.404(9) . ? N51' C53' 1.409(9) . ? O60 C60 1.293(7) . ? C60 N61 1.326(7) . ? N61 C62 1.434(9) . ? N61 C63 1.457(7) . ? O60' C60' 1.313(8) . ? C60' N61' 1.337(9) . ? N61' C62' 1.432(10) . ? N61' C63' 1.458(9) . ? O70 C70 1.224(2) . ? C70 N71 1.329(2) . ? N71 C73 1.445(2) . ? N71 C72 1.452(2) . ? O80 C83 1.380(8) . ? O80 C81 1.403(8) . ? C81 C82 1.464(9) . ? C83 C84 1.413(9) . ? O80' C83' 1.405(10) . ? O80' C81' 1.410(10) . ? C81' C82' 1.446(10) . ? C83' C84' 1.455(10) . ? 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 N24 Co N14 111.31(5) . . ? N24 Co N4 112.69(5) . . ? N14 Co N4 117.25(5) . . ? N24 Co Cl 105.28(4) . . ? N14 Co Cl 104.16(3) . . ? N4 Co Cl 104.79(4) . . ? N24 Co N1 75.65(4) . . ? N14 Co N1 75.38(4) . . ? N4 Co N1 74.80(4) . . ? Cl Co N1 179.07(3) . . ? C2 N1 C12 112.94(12) . . ? C2 N1 C22 113.43(12) . . ? C12 N1 C22 111.97(11) . . ? C2 N1 Co 106.05(8) . . ? C12 N1 Co 106.65(8) . . ? C22 N1 Co 105.06(9) . . ? N1 C2 C3 108.05(12) . . ? N4 C3 N11 112.72(13) . . ? N4 C3 C2 121.60(14) . . ? N11 C3 C2 125.67(14) . . ? C3 N4 C5 105.29(13) . . ? C3 N4 Co 118.40(10) . . ? C5 N4 Co 135.94(11) . . ? C10 C5 C6 121.16(14) . . ? C10 C5 N4 108.43(13) . . ? C6 C5 N4 130.41(15) . . ? C7 C6 C5 116.71(17) . . ? C6 C7 C8 121.76(17) . . ? C9 C8 C7 122.00(16) . . ? C8 C9 C10 116.75(18) . . ? N11 C10 C5 106.28(13) . . ? N11 C10 C9 132.10(17) . . ? C5 C10 C9 121.61(16) . . ? C3 N11 C10 107.27(13) . . ? N1 C12 C13 108.64(11) . . ? N14 C13 N21 112.57(13) . . ? N14 C13 C12 122.45(13) . . ? N21 C13 C12 124.88(12) . . ? C13 N14 C15 105.50(12) . . ? C13 N14 Co 118.38(10) . . ? C15 N14 Co 135.47(9) . . ? C16 C15 C20 120.06(14) . . ? C16 C15 N14 131.24(14) . . ? C20 C15 N14 108.68(12) . . ? C17 C16 C15 117.30(15) . . ? C16 C17 C18 121.93(15) . . ? C19 C18 C17 121.28(16) . . ? C18 C19 C20 116.63(15) . . ? C19 C20 N21 131.47(14) . . ? C19 C20 C15 122.80(14) . . ? N21 C20 C15 105.71(13) . . ? C13 N21 C20 107.53(12) . . ? N1 C22 C23 107.74(12) . . ? N24 C23 N31 112.67(13) . . ? N24 C23 C22 121.41(13) . . ? N31 C23 C22 125.90(13) . . ? C23 N24 C25 105.56(12) . . ? C23 N24 Co 118.36(10) . . ? C25 N24 Co 135.95(9) . . ? N24 C25 C26 131.18(13) . . ? N24 C25 C30 108.78(13) . . ? C26 C25 C30 120.03(14) . . ? C27 C26 C25 117.59(14) . . ? C26 C27 C28 121.96(16) . . ? C29 C28 C27 121.36(16) . . ? C30 C29 C28 116.49(15) . . ? C29 C30 N31 131.97(14) . . ? C29 C30 C25 122.56(15) . . ? N31 C30 C25 105.47(13) . . ? C23 N31 C30 107.51(12) . . ? N14' Co' N24' 108.97(5) . . ? N14' Co' N4' 115.57(5) . . ? N24' Co' N4' 117.79(5) . . ? N14' Co' Cl' 106.60(4) . . ? N24' Co' Cl' 101.99(4) . . ? N4' Co' Cl' 104.25(4) . . ? N14' Co' N1' 76.37(5) . . ? N24' Co' N1' 75.30(5) . . ? N4' Co' N1' 75.55(5) . . ? Cl' Co' N1' 176.62(3) . . ? C2' N1' C22' 111.52(12) . . ? C2' N1' C12' 111.84(12) . . ? C22' N1' C12' 112.79(11) . . ? C2' N1' Co' 107.06(8) . . ? C22' N1' Co' 106.08(9) . . ? C12' N1' Co' 107.12(9) . . ? N1' C2' C3' 107.90(12) . . ? N4' C3' N11' 113.36(13) . . ? N4' C3' C2' 121.92(13) . . ? N11' C3' C2' 124.70(14) . . ? C3' N4' C5' 104.82(12) . . ? C3' N4' Co' 118.13(10) . . ? C5' N4' Co' 136.64(10) . . ? C6' C5' C10' 120.66(14) . . ? C6' C5' N4' 130.99(15) . . ? C10' C5' N4' 108.34(14) . . ? C7' C6' C5' 117.38(16) . . ? C6' C7' C8' 121.64(17) . . ? C9' C8' C7' 121.51(16) . . ? C8' C9' C10' 117.10(16) . . ? N11' C10' C9' 132.11(15) . . ? N11' C10' C5' 106.18(13) . . ? C9' C10' C5' 121.70(16) . . ? C3' N11' C10' 107.28(13) . . ? N1' C12' C13' 108.43(12) . . ? N14' C13' N21' 112.55(13) . . ? N14' C13' C12' 122.54(14) . . ? N21' C13' C12' 124.77(13) . . ? C13' N14' C15' 105.52(13) . . ? C13' N14' Co' 118.31(10) . . ? C15' N14' Co' 136.14(10) . . ? C16' C15' C20' 120.33(15) . . ? C16' C15' N14' 130.78(14) . . ? C20' C15' N14' 108.89(13) . . ? C17' C16' C15' 117.29(15) . . ? C16' C17' C18' 122.09(16) . . ? C19' C18' C17' 121.26(16) . . ? C18' C19' C20' 116.50(16) . . ? C19' C20' N21' 131.96(15) . . ? C19' C20' C15' 122.52(15) . . ? N21' C20' C15' 105.51(13) . . ? C13' N21' C20' 107.52(12) . . ? N1' C22' C23' 108.43(12) . . ? N24' C23' N31' 112.40(14) . . ? N24' C23' C22' 122.83(14) . . ? N31' C23' C22' 124.74(14) . . ? C23' N24' C25' 105.75(12) . . ? C23' N24' Co' 116.86(10) . . ? C25' N24' Co' 136.50(10) . . ? C26' C25' N24' 131.28(15) . . ? C26' C25' C30' 120.21(15) . . ? N24' C25' C30' 108.50(14) . . ? C27' C26' C25' 117.52(16) . . ? C26' C27' C28' 121.72(17) . . ? C29' C28' C27' 121.44(17) . . ? C28' C29' C30' 116.96(17) . . ? N31' C30' C29' 132.02(16) . . ? N31' C30' C25' 105.82(14) . . ? C29' C30' C25' 122.15(16) . . ? C23' N31' C30' 107.51(14) . . ? O40 C40 N41 125.7(3) . . ? C40 N41 C42 120.6(2) . . ? C40 N41 C43 121.8(3) . . ? C42 N41 C43 117.6(2) . . ? O40' C40' N41' 121.4(19) . . ? C40' N41' C43' 121.3(16) . . ? C40' N41' C42' 120.4(16) . . ? C43' N41' C42' 117.2(15) . . ? O50 C50 N51 125.7(3) . . ? C50 N51 C53 122.9(3) . . ? C50 N51 C52 120.7(3) . . ? C53 N51 C52 116.4(2) . . ? O50' C50' N51' 121.1(7) . . ? C50' N51' C52' 120.5(7) . . ? C50' N51' C53' 121.5(7) . . ? C52' N51' C53' 118.0(7) . . ? O60 C60 N61 119.3(5) . . ? C60 N61 C62 120.2(5) . . ? C60 N61 C63 122.1(7) . . ? C62 N61 C63 117.5(5) . . ? O60' C60' N61' 117.1(6) . . ? C60' N61' C62' 120.6(7) . . ? C60' N61' C63' 120.5(8) . . ? C62' N61' C63' 118.7(7) . . ? O70 C70 N71 125.60(18) . . ? C70 N71 C73 121.54(16) . . ? C70 N71 C72 120.54(17) . . ? C73 N71 C72 117.85(16) . . ? C83 O80 C81 121.7(9) . . ? O80 C81 C82 109.2(9) . . ? O80 C83 C84 113.3(9) . . ? C83' O80' C81' 106.0(14) . . ? O80' C81' C82' 104.6(14) . . ? O80' C83' C84' 108.5(14) . . ? _diffrn_measured_fraction_theta_max 0.899 _diffrn_reflns_theta_full 30.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.353 _refine_diff_density_min -0.278 _refine_diff_density_rms 0.050 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 762756' #TrackingRef '- Dalton04-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H13 Cl2 Co N5, C3 H7 N O' _chemical_formula_sum 'C22 H20 Cl2 Co N6 O' _chemical_formula_weight 514.27 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' 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 14.6250(2) _cell_length_b 7.70335(12) _cell_length_c 19.6751(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.3472(16) _cell_angle_gamma 90.00 _cell_volume 2165.36(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13535 _cell_measurement_theta_min 4.1214 _cell_measurement_theta_max 31.9218 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1052 _exptl_absorpt_coefficient_mu 1.068 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.964 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31789 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 32.01 _reflns_number_total 7005 _reflns_number_gt 4932 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0380P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7005 _refine_ls_number_parameters 299 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0280 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _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 Co Co 0.701564(12) 0.75368(2) 0.487136(9) 0.01752(5) Uani 1 1 d . . . Cl1 Cl 0.71107(2) 1.00139(5) 0.420976(18) 0.02749(8) Uani 1 1 d . . . Cl2 Cl 0.84218(3) 0.69036(6) 0.559114(19) 0.03516(10) Uani 1 1 d . . . N1 N 0.55783(7) 0.68399(14) 0.45212(5) 0.0178(2) Uani 1 1 d . . . C2 C 0.49374(9) 0.73840(16) 0.48659(6) 0.0176(2) Uani 1 1 d . . . C3 C 0.39928(9) 0.69881(17) 0.46449(7) 0.0216(3) Uani 1 1 d . . . H3A H 0.3544 0.7389 0.4893 0.026 Uiso 1 1 calc R . . C4 C 0.37277(9) 0.59854(18) 0.40476(7) 0.0233(3) Uani 1 1 d . . . H4A H 0.3086 0.5720 0.3875 0.028 Uiso 1 1 calc R . . C5 C 0.43978(9) 0.53687(17) 0.37010(7) 0.0220(3) Uani 1 1 d . . . H5A H 0.4226 0.4661 0.3299 0.026 Uiso 1 1 calc R . . C6 C 0.53255(9) 0.58202(17) 0.39615(6) 0.0185(3) Uani 1 1 d . . . C7 C 0.53874(9) 0.83382(16) 0.54939(6) 0.0177(2) Uani 1 1 d . . . N8 N 0.63132(7) 0.85444(14) 0.56361(5) 0.0180(2) Uani 1 1 d . . . C9 C 0.65144(9) 0.94363(17) 0.62639(6) 0.0190(3) Uani 1 1 d . . . C10 C 0.73668(10) 1.00743(18) 0.66456(7) 0.0236(3) Uani 1 1 d . . . H10A H 0.7937 0.9889 0.6499 0.028 Uiso 1 1 calc R . . C11 C 0.73388(11) 1.09851(19) 0.72448(7) 0.0285(3) Uani 1 1 d . . . H11A H 0.7903 1.1457 0.7511 0.034 Uiso 1 1 calc R . . C12 C 0.65032(11) 1.12362(19) 0.74740(7) 0.0299(3) Uani 1 1 d . . . H12A H 0.6519 1.1850 0.7895 0.036 Uiso 1 1 calc R . . C13 C 0.56601(10) 1.06132(19) 0.71024(7) 0.0265(3) Uani 1 1 d . . . H13A H 0.5093 1.0777 0.7257 0.032 Uiso 1 1 calc R . . C14 C 0.56841(9) 0.97319(17) 0.64897(7) 0.0200(3) Uani 1 1 d . . . N15 N 0.49780(8) 0.89954(14) 0.59895(6) 0.0200(2) Uani 1 1 d D . . H15 H 0.4361(2) 0.910(2) 0.5973(8) 0.035(4) Uiso 1 1 d D . . C16 C 0.61486(9) 0.52213(16) 0.37193(6) 0.0183(3) Uani 1 1 d . . . N17 N 0.69969(7) 0.56371(15) 0.40777(5) 0.0191(2) Uani 1 1 d . . . C18 C 0.76116(9) 0.48700(16) 0.37216(6) 0.0186(3) Uani 1 1 d . . . C19 C 0.85883(9) 0.48914(18) 0.38553(7) 0.0235(3) Uani 1 1 d . . . H19A H 0.8945 0.5489 0.4245 0.028 Uiso 1 1 calc R . . C20 C 0.90123(10) 0.40096(19) 0.33980(8) 0.0280(3) Uani 1 1 d . . . H20A H 0.9676 0.3996 0.3475 0.034 Uiso 1 1 calc R . . C21 C 0.84870(11) 0.3132(2) 0.28207(8) 0.0313(3) Uani 1 1 d . . . H21A H 0.8806 0.2544 0.2515 0.038 Uiso 1 1 calc R . . C22 C 0.75253(11) 0.3093(2) 0.26822(7) 0.0287(3) Uani 1 1 d . . . H22A H 0.7171 0.2493 0.2291 0.034 Uiso 1 1 calc R . . C23 C 0.71006(9) 0.39801(17) 0.31448(7) 0.0210(3) Uani 1 1 d . . . N24 N 0.61660(8) 0.42215(15) 0.31593(6) 0.0210(2) Uani 1 1 d D . . H24 H 0.5670(8) 0.384(2) 0.2840(7) 0.048(5) Uiso 1 1 d D . . O30 O 0.46528(7) 0.30573(16) 0.22357(5) 0.0362(3) Uani 1 1 d . . . C30 C 0.43693(10) 0.25928(19) 0.16256(7) 0.0271(3) Uani 1 1 d . . . H30A H 0.3919 0.1686 0.1545 0.032 Uiso 1 1 calc R . . N31 N 0.46291(8) 0.32292(16) 0.10782(6) 0.0274(3) Uani 1 1 d . . . C32 C 0.53196(14) 0.4602(2) 0.11410(10) 0.0484(5) Uani 1 1 d . . . H32A H 0.5556 0.4876 0.1634 0.073 Uiso 1 1 calc R . . H32B H 0.5031 0.5638 0.0897 0.073 Uiso 1 1 calc R . . H32C H 0.5839 0.4219 0.0935 0.073 Uiso 1 1 calc R . . C33 C 0.42047(14) 0.2657(2) 0.03767(8) 0.0436(4) Uani 1 1 d . . . H33A H 0.3813 0.1636 0.0400 0.065 Uiso 1 1 calc R . . H33B H 0.4697 0.2356 0.0129 0.065 Uiso 1 1 calc R . . H33C H 0.3818 0.3593 0.0128 0.065 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 Co 0.01522(8) 0.02012(9) 0.01669(8) -0.00167(7) 0.00224(6) 0.00058(7) Cl1 0.02291(15) 0.02732(17) 0.03466(19) 0.00778(14) 0.01151(14) 0.00178(13) Cl2 0.02452(17) 0.0508(2) 0.02550(17) -0.00773(16) -0.00514(14) 0.01413(16) N1 0.0179(5) 0.0174(5) 0.0179(5) 0.0004(4) 0.0034(4) -0.0002(4) C2 0.0186(5) 0.0154(6) 0.0187(6) 0.0036(5) 0.0040(5) 0.0010(5) C3 0.0182(6) 0.0211(6) 0.0255(7) 0.0041(5) 0.0049(5) 0.0018(5) C4 0.0182(6) 0.0223(7) 0.0274(7) 0.0045(5) 0.0003(5) -0.0013(5) C5 0.0228(6) 0.0211(7) 0.0197(6) 0.0018(5) -0.0009(5) -0.0021(5) C6 0.0208(6) 0.0171(6) 0.0170(6) 0.0020(5) 0.0025(5) 0.0000(5) C7 0.0184(6) 0.0163(6) 0.0188(6) 0.0028(5) 0.0047(5) 0.0022(5) N8 0.0177(5) 0.0192(5) 0.0172(5) 0.0004(4) 0.0039(4) 0.0009(4) C9 0.0231(6) 0.0181(6) 0.0155(6) 0.0019(5) 0.0037(5) 0.0027(5) C10 0.0224(6) 0.0240(7) 0.0224(6) 0.0007(5) 0.0002(5) 0.0029(5) C11 0.0316(8) 0.0281(8) 0.0217(7) -0.0008(6) -0.0032(6) 0.0019(6) C12 0.0440(9) 0.0270(8) 0.0180(6) -0.0029(6) 0.0048(6) 0.0031(6) C13 0.0344(8) 0.0259(7) 0.0219(7) 0.0011(6) 0.0121(6) 0.0040(6) C14 0.0241(6) 0.0181(6) 0.0182(6) 0.0032(5) 0.0057(5) 0.0011(5) N15 0.0188(5) 0.0216(6) 0.0208(5) 0.0012(4) 0.0069(4) 0.0018(4) C16 0.0212(6) 0.0175(6) 0.0159(6) -0.0002(5) 0.0029(5) -0.0008(5) N17 0.0177(5) 0.0217(5) 0.0171(5) -0.0010(4) 0.0022(4) 0.0002(4) C18 0.0238(6) 0.0157(6) 0.0167(6) 0.0014(5) 0.0054(5) 0.0013(5) C19 0.0235(6) 0.0234(7) 0.0231(7) -0.0001(5) 0.0038(5) 0.0003(5) C20 0.0249(7) 0.0285(8) 0.0324(8) 0.0011(6) 0.0103(6) 0.0015(6) C21 0.0346(8) 0.0300(8) 0.0334(8) -0.0062(6) 0.0166(7) 0.0016(6) C22 0.0345(8) 0.0279(7) 0.0246(7) -0.0078(6) 0.0085(6) -0.0015(6) C23 0.0249(6) 0.0183(6) 0.0203(6) 0.0004(5) 0.0058(5) -0.0006(5) N24 0.0219(5) 0.0229(6) 0.0176(5) -0.0033(4) 0.0026(4) -0.0017(5) O30 0.0319(6) 0.0498(7) 0.0249(5) -0.0063(5) 0.0021(5) -0.0117(5) C30 0.0237(6) 0.0280(7) 0.0271(7) -0.0015(6) 0.0000(5) -0.0048(6) N31 0.0298(6) 0.0244(6) 0.0262(6) 0.0017(5) 0.0018(5) -0.0026(5) C32 0.0511(11) 0.0455(11) 0.0471(10) 0.0102(8) 0.0069(9) -0.0192(9) C33 0.0533(11) 0.0501(11) 0.0230(7) 0.0021(7) -0.0013(7) -0.0043(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 Co N17 2.1359(11) . ? Co N1 2.1360(10) . ? Co N8 2.1407(11) . ? Co Cl2 2.2862(4) . ? Co Cl1 2.3308(4) . ? N1 C2 1.3363(16) . ? N1 C6 1.3388(16) . ? C2 C3 1.3907(17) . ? C2 C7 1.4671(17) . ? C3 C4 1.3903(19) . ? C4 C5 1.392(2) . ? C5 C6 1.3882(17) . ? C6 C16 1.4608(18) . ? C7 N8 1.3322(15) . ? C7 N15 1.3474(16) . ? N8 C9 1.3888(16) . ? C9 C14 1.3980(18) . ? C9 C10 1.3998(18) . ? C10 C11 1.3801(19) . ? C11 C12 1.404(2) . ? C12 C13 1.378(2) . ? C13 C14 1.3905(19) . ? C14 N15 1.3865(17) . ? C16 N17 1.3285(16) . ? C16 N24 1.3491(16) . ? N17 C18 1.3848(17) . ? C18 C19 1.3962(18) . ? C18 C23 1.3978(17) . ? C19 C20 1.376(2) . ? C20 C21 1.402(2) . ? C21 C22 1.375(2) . ? C22 C23 1.3866(19) . ? C23 N24 1.3857(17) . ? O30 C30 1.2362(16) . ? C30 N31 1.3113(19) . ? N31 C32 1.449(2) . ? N31 C33 1.4555(19) . ? 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 N17 Co N1 74.58(4) . . ? N17 Co N8 146.01(4) . . ? N1 Co N8 74.38(4) . . ? N17 Co Cl2 100.13(3) . . ? N1 Co Cl2 147.04(3) . . ? N8 Co Cl2 98.35(3) . . ? N17 Co Cl1 98.37(3) . . ? N1 Co Cl1 101.41(3) . . ? N8 Co Cl1 100.99(3) . . ? Cl2 Co Cl1 111.558(16) . . ? C2 N1 C6 120.08(11) . . ? C2 N1 Co 120.41(8) . . ? C6 N1 Co 119.49(9) . . ? N1 C2 C3 122.02(12) . . ? N1 C2 C7 110.34(11) . . ? C3 C2 C7 127.59(12) . . ? C4 C3 C2 117.71(13) . . ? C3 C4 C5 120.36(12) . . ? C6 C5 C4 117.95(12) . . ? N1 C6 C5 121.79(12) . . ? N1 C6 C16 110.60(11) . . ? C5 C6 C16 127.51(12) . . ? N8 C7 N15 113.09(11) . . ? N8 C7 C2 119.30(11) . . ? N15 C7 C2 127.52(11) . . ? C7 N8 C9 104.97(11) . . ? C7 N8 Co 115.35(8) . . ? C9 N8 Co 139.66(9) . . ? N8 C9 C14 109.27(11) . . ? N8 C9 C10 130.23(12) . . ? C14 C9 C10 120.45(12) . . ? C11 C10 C9 116.82(13) . . ? C10 C11 C12 122.10(13) . . ? C13 C12 C11 121.55(13) . . ? C12 C13 C14 116.38(14) . . ? N15 C14 C13 131.46(13) . . ? N15 C14 C9 105.88(11) . . ? C13 C14 C9 122.66(12) . . ? C7 N15 C14 106.77(11) . . ? N17 C16 N24 113.11(11) . . ? N17 C16 C6 119.46(11) . . ? N24 C16 C6 127.41(11) . . ? C16 N17 C18 105.20(10) . . ? C16 N17 Co 114.69(9) . . ? C18 N17 Co 138.94(9) . . ? N17 C18 C19 130.42(12) . . ? N17 C18 C23 109.14(11) . . ? C19 C18 C23 120.44(12) . . ? C20 C19 C18 117.18(13) . . ? C19 C20 C21 121.50(14) . . ? C22 C21 C20 122.09(14) . . ? C21 C22 C23 116.26(13) . . ? N24 C23 C22 131.45(12) . . ? N24 C23 C18 106.02(11) . . ? C22 C23 C18 122.53(13) . . ? C16 N24 C23 106.52(11) . . ? O30 C30 N31 126.40(14) . . ? C30 N31 C32 121.46(13) . . ? C30 N31 C33 121.72(13) . . ? C32 N31 C33 116.74(14) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 31.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.353 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.059 #===END data_1_2 _database_code_depnum_ccdc_archive 'CCDC 762757' #TrackingRef '- Dalton04-10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H23 Cl2 Co N5, 2(C3 H7 N O)' _chemical_formula_sum 'C30 H37 Cl2 Co N7 O2' _chemical_formula_weight 657.50 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' 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 8.94991(11) _cell_length_b 17.56344(19) _cell_length_c 20.0433(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.4273(11) _cell_angle_gamma 90.00 _cell_volume 3130.83(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 19154 _cell_measurement_theta_min 4.1553 _cell_measurement_theta_max 32.4603 _exptl_crystal_description needles _exptl_crystal_colour Blue _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1372 _exptl_absorpt_coefficient_mu 0.758 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.957 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET) (compiled Sep 15 2009,11:49:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9825 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 50546 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 4.17 _diffrn_reflns_theta_max 32.54 _reflns_number_total 10513 _reflns_number_gt 7218 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0426P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10513 _refine_ls_number_parameters 393 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0771 _refine_ls_wR_factor_gt 0.0739 _refine_ls_goodness_of_fit_ref 0.922 _refine_ls_restrained_S_all 0.922 _refine_ls_shift/su_max 0.003 _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 Co Co 0.225627(18) 0.435132(9) 0.801254(8) 0.02062(5) Uani 1 1 d . . . Cl1 Cl 0.31944(4) 0.317116(18) 0.818464(18) 0.03504(8) Uani 1 1 d . . . Cl2 Cl -0.01696(3) 0.447291(18) 0.818735(16) 0.02814(7) Uani 1 1 d . . . N1 N 0.54758(12) 0.56777(6) 0.73771(6) 0.0269(2) Uani 1 1 d . . . C2 C 0.56832(14) 0.51005(7) 0.78963(6) 0.0246(2) Uani 1 1 d . . . H2A H 0.6771 0.5032 0.8036 0.030 Uiso 1 1 calc R . . H2B H 0.5277 0.4610 0.7713 0.030 Uiso 1 1 calc R . . C3 C 0.49087(13) 0.53139(7) 0.84972(6) 0.0228(2) Uani 1 1 d . . . N4 N 0.35750(11) 0.50509(6) 0.86179(5) 0.0217(2) Uani 1 1 d . . . C5 C 0.33228(14) 0.53512(7) 0.92418(6) 0.0223(2) Uani 1 1 d . . . C6 C 0.21429(15) 0.52367(8) 0.96305(6) 0.0281(3) Uani 1 1 d . . . H6A H 0.1305 0.4926 0.9477 0.034 Uiso 1 1 calc R . . C7 C 0.22462(16) 0.55939(8) 1.02471(7) 0.0326(3) Uani 1 1 d . . . H7A H 0.1460 0.5529 1.0524 0.039 Uiso 1 1 calc R . . C8 C 0.34872(17) 0.60509(8) 1.04755(7) 0.0333(3) Uani 1 1 d . . . H8A H 0.3519 0.6286 1.0904 0.040 Uiso 1 1 calc R . . C9 C 0.46520(16) 0.61672(7) 1.00995(7) 0.0307(3) Uani 1 1 d . . . H9A H 0.5491 0.6475 1.0256 0.037 Uiso 1 1 calc R . . C10 C 0.45430(14) 0.58098(7) 0.94742(6) 0.0247(3) Uani 1 1 d . . . N11 N 0.55195(12) 0.57783(6) 0.89881(5) 0.0252(2) Uani 1 1 d D . . H11 H 0.6405(8) 0.6018(8) 0.8978(8) 0.039(4) Uiso 1 1 d D . . C12 C 0.39424(14) 0.58330(7) 0.70906(7) 0.0244(2) Uani 1 1 d . . . H12A H 0.3957 0.6257 0.6766 0.029 Uiso 1 1 calc R . . H12B H 0.3358 0.6004 0.7454 0.029 Uiso 1 1 calc R . . C13 C 0.31477(13) 0.51669(7) 0.67398(6) 0.0230(2) Uani 1 1 d . . . N14 N 0.24348(11) 0.46218(6) 0.70394(5) 0.0234(2) Uani 1 1 d . . . C15 C 0.18396(14) 0.41351(7) 0.65226(6) 0.0243(2) Uani 1 1 d . . . C16 C 0.09790(15) 0.34789(8) 0.65451(7) 0.0309(3) Uani 1 1 d . . . H16A H 0.0697 0.3289 0.6957 0.037 Uiso 1 1 calc R . . C17 C 0.05512(17) 0.31143(8) 0.59420(7) 0.0368(3) Uani 1 1 d . . . H17A H -0.0033 0.2662 0.5940 0.044 Uiso 1 1 calc R . . C18 C 0.09592(17) 0.33957(9) 0.53352(7) 0.0376(3) Uani 1 1 d . . . H18A H 0.0646 0.3129 0.4931 0.045 Uiso 1 1 calc R . . C19 C 0.18026(16) 0.40493(8) 0.53068(7) 0.0325(3) Uani 1 1 d . . . H19A H 0.2070 0.4243 0.4894 0.039 Uiso 1 1 calc R . . C20 C 0.22409(14) 0.44088(7) 0.59145(6) 0.0253(3) Uani 1 1 d . . . N21 N 0.30622(12) 0.50626(6) 0.60704(5) 0.0265(2) Uani 1 1 d D . . H21 H 0.3556(16) 0.5349(7) 0.5794(6) 0.043(4) Uiso 1 1 d D . . C22 C 0.67282(13) 0.59441(7) 0.70640(6) 0.0221(2) Uani 1 1 d . . . C23 C 0.70850(15) 0.67211(7) 0.71130(7) 0.0276(3) Uani 1 1 d . . . C24 C 0.83663(17) 0.69793(8) 0.68496(7) 0.0373(3) Uani 1 1 d . . . H24A H 0.8617 0.7505 0.6877 0.045 Uiso 1 1 calc R . . C25 C 0.92740(17) 0.64827(10) 0.65496(7) 0.0421(4) Uani 1 1 d . . . H25A H 1.0163 0.6664 0.6385 0.051 Uiso 1 1 calc R . . C26 C 0.88989(16) 0.57236(9) 0.64868(7) 0.0374(3) Uani 1 1 d . . . H26A H 0.9529 0.5388 0.6273 0.045 Uiso 1 1 calc R . . C27 C 0.76121(15) 0.54386(8) 0.67311(7) 0.0277(3) Uani 1 1 d . . . C28 C 0.61337(18) 0.72719(8) 0.74578(8) 0.0396(3) Uani 1 1 d . . . H28A H 0.5211 0.7384 0.7163 0.059 Uiso 1 1 calc R . . H28B H 0.6697 0.7744 0.7558 0.059 Uiso 1 1 calc R . . H28C H 0.5874 0.7046 0.7877 0.059 Uiso 1 1 calc R . . C29 C 0.71885(18) 0.46162(8) 0.66224(8) 0.0389(3) Uani 1 1 d . . . H29A H 0.7475 0.4329 0.7036 0.058 Uiso 1 1 calc R . . H29B H 0.7714 0.4407 0.6260 0.058 Uiso 1 1 calc R . . H29C H 0.6100 0.4576 0.6500 0.058 Uiso 1 1 calc R . . O30 O 0.79634(12) 0.66739(6) 0.89792(5) 0.0410(3) Uani 1 1 d . . . C30 C 0.90773(16) 0.65085(8) 0.86920(7) 0.0322(3) Uani 1 1 d . . . H30A H 0.9197 0.5990 0.8572 0.039 Uiso 1 1 calc R . . N31 N 1.01079(13) 0.69942(6) 0.85399(6) 0.0300(2) Uani 1 1 d . . . C32 C 0.9999(2) 0.78022(8) 0.86788(10) 0.0476(4) Uani 1 1 d . . . H32A H 0.9023 0.7911 0.8836 0.071 Uiso 1 1 calc R . . H32B H 1.0094 0.8092 0.8268 0.071 Uiso 1 1 calc R . . H32C H 1.0806 0.7949 0.9026 0.071 Uiso 1 1 calc R . . C33 C 1.13937(17) 0.67403(9) 0.82112(8) 0.0397(3) Uani 1 1 d . . . H33A H 1.2316 0.6799 0.8520 0.060 Uiso 1 1 calc R . . H33B H 1.1468 0.7048 0.7808 0.060 Uiso 1 1 calc R . . H33C H 1.1262 0.6204 0.8084 0.060 Uiso 1 1 calc R . . O40 O 0.49012(12) 0.58846(6) 0.53456(5) 0.0399(2) Uani 1 1 d . . . C40 C 0.52701(16) 0.65528(8) 0.54656(7) 0.0324(3) Uani 1 1 d . . . H40A H 0.6313 0.6656 0.5565 0.039 Uiso 1 1 calc R . . N41 N 0.43393(14) 0.71345(6) 0.54680(6) 0.0332(3) Uani 1 1 d . . . C42 C 0.27338(18) 0.70391(9) 0.52966(9) 0.0446(4) Uani 1 1 d . . . H42A H 0.2518 0.6509 0.5168 0.067 Uiso 1 1 calc R . . H42B H 0.2386 0.7375 0.4921 0.067 Uiso 1 1 calc R . . H42C H 0.2211 0.7169 0.5686 0.067 Uiso 1 1 calc R . . C43 C 0.4891(2) 0.79025(8) 0.56054(9) 0.0482(4) Uani 1 1 d . . . H43A H 0.5989 0.7892 0.5703 0.072 Uiso 1 1 calc R . . H43B H 0.4449 0.8108 0.5993 0.072 Uiso 1 1 calc R . . H43C H 0.4609 0.8225 0.5213 0.072 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 Co 0.01965(8) 0.02287(8) 0.01989(8) 0.00013(6) 0.00456(6) -0.00104(6) Cl1 0.0407(2) 0.02805(16) 0.03621(19) -0.00095(13) 0.00369(14) 0.00961(14) Cl2 0.01965(15) 0.03507(17) 0.03027(16) 0.00024(12) 0.00528(12) 0.00041(11) N1 0.0170(5) 0.0348(6) 0.0294(6) 0.0114(5) 0.0049(4) -0.0005(4) C2 0.0204(6) 0.0292(6) 0.0247(6) 0.0051(5) 0.0044(5) -0.0001(5) C3 0.0204(6) 0.0240(6) 0.0238(6) 0.0040(5) 0.0015(5) -0.0002(4) N4 0.0193(5) 0.0256(5) 0.0205(5) 0.0014(4) 0.0032(4) -0.0008(4) C5 0.0228(6) 0.0233(6) 0.0205(6) 0.0009(5) 0.0011(4) 0.0022(5) C6 0.0248(7) 0.0335(7) 0.0262(7) 0.0010(5) 0.0039(5) -0.0005(5) C7 0.0321(7) 0.0398(8) 0.0269(7) -0.0001(6) 0.0081(5) 0.0074(6) C8 0.0402(8) 0.0329(7) 0.0263(7) -0.0054(6) 0.0011(6) 0.0079(6) C9 0.0343(8) 0.0261(6) 0.0299(7) -0.0031(5) -0.0038(6) -0.0006(5) C10 0.0246(6) 0.0237(6) 0.0252(6) 0.0026(5) -0.0002(5) 0.0011(5) N11 0.0222(5) 0.0274(5) 0.0257(5) 0.0005(4) 0.0012(4) -0.0058(4) C12 0.0202(6) 0.0262(6) 0.0270(6) 0.0038(5) 0.0036(5) 0.0010(4) C13 0.0180(6) 0.0282(6) 0.0231(6) 0.0035(5) 0.0031(5) 0.0026(5) N14 0.0207(5) 0.0275(5) 0.0224(5) 0.0006(4) 0.0033(4) -0.0018(4) C15 0.0214(6) 0.0304(6) 0.0212(6) 0.0005(5) 0.0022(5) 0.0014(5) C16 0.0294(7) 0.0370(7) 0.0262(7) 0.0008(6) 0.0030(5) -0.0064(5) C17 0.0356(8) 0.0395(8) 0.0346(8) -0.0036(6) 0.0005(6) -0.0100(6) C18 0.0379(9) 0.0477(9) 0.0260(7) -0.0084(6) -0.0013(6) -0.0032(7) C19 0.0318(8) 0.0442(8) 0.0216(6) 0.0000(6) 0.0033(5) 0.0024(6) C20 0.0217(6) 0.0316(6) 0.0227(6) 0.0019(5) 0.0032(5) 0.0022(5) N21 0.0258(6) 0.0324(6) 0.0216(5) 0.0047(4) 0.0048(4) -0.0006(4) C22 0.0189(6) 0.0279(6) 0.0198(6) 0.0016(5) 0.0031(4) -0.0027(5) C23 0.0297(7) 0.0292(6) 0.0235(6) 0.0010(5) 0.0007(5) -0.0040(5) C24 0.0368(8) 0.0401(8) 0.0340(8) 0.0102(6) -0.0009(6) -0.0162(6) C25 0.0245(7) 0.0703(11) 0.0320(8) 0.0145(7) 0.0057(6) -0.0118(7) C26 0.0250(7) 0.0644(10) 0.0239(7) 0.0042(7) 0.0081(5) 0.0089(7) C27 0.0258(7) 0.0363(7) 0.0208(6) -0.0007(5) 0.0022(5) 0.0034(5) C28 0.0500(10) 0.0286(7) 0.0393(9) -0.0038(6) 0.0012(7) 0.0023(6) C29 0.0436(9) 0.0353(7) 0.0373(8) -0.0087(6) 0.0024(7) 0.0089(6) O30 0.0339(6) 0.0425(6) 0.0487(7) -0.0085(5) 0.0138(5) -0.0139(4) C30 0.0342(8) 0.0282(7) 0.0340(8) 0.0000(6) 0.0025(6) -0.0049(5) N31 0.0282(6) 0.0280(6) 0.0347(6) 0.0019(5) 0.0070(5) -0.0019(4) C32 0.0500(10) 0.0305(8) 0.0665(12) -0.0084(7) 0.0244(9) -0.0105(7) C33 0.0349(8) 0.0405(8) 0.0454(9) 0.0082(7) 0.0126(7) 0.0065(6) O40 0.0451(7) 0.0315(5) 0.0460(6) 0.0006(5) 0.0174(5) -0.0046(4) C40 0.0314(8) 0.0386(8) 0.0286(7) 0.0021(6) 0.0091(6) -0.0041(6) N41 0.0326(7) 0.0327(6) 0.0343(7) -0.0024(5) 0.0040(5) -0.0041(5) C42 0.0316(9) 0.0502(9) 0.0517(10) 0.0014(8) 0.0036(7) 0.0003(7) C43 0.0583(12) 0.0320(8) 0.0536(11) -0.0057(7) 0.0033(8) -0.0091(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N4 2.0135(10) . ? Co N14 2.0312(10) . ? Co Cl2 2.2478(3) . ? Co Cl1 2.2484(4) . ? N1 C22 1.4237(15) . ? N1 C2 1.4499(15) . ? N1 C12 1.4530(16) . ? C2 C3 1.5028(17) . ? C3 N4 1.3272(15) . ? C3 N11 1.3460(16) . ? N4 C5 1.3986(15) . ? C5 C10 1.3943(18) . ? C5 C6 1.3952(17) . ? C6 C7 1.3799(18) . ? C7 C8 1.405(2) . ? C8 C9 1.368(2) . ? C9 C10 1.3954(18) . ? C10 N11 1.3809(17) . ? C12 C13 1.5022(17) . ? C13 N14 1.3304(15) . ? C13 N21 1.3479(15) . ? N14 C15 1.4014(16) . ? C15 C16 1.3898(18) . ? C15 C20 1.3941(17) . ? C16 C17 1.3835(19) . ? C17 C18 1.399(2) . ? C18 C19 1.379(2) . ? C19 C20 1.3888(18) . ? C20 N21 1.3802(16) . ? C22 C23 1.4025(18) . ? C22 C27 1.4062(18) . ? C23 C24 1.3910(19) . ? C23 C28 1.5067(19) . ? C24 C25 1.375(2) . ? C25 C26 1.377(2) . ? C26 C27 1.3939(19) . ? C27 C29 1.503(2) . ? O30 C30 1.2401(17) . ? C30 N31 1.3170(17) . ? N31 C32 1.4515(17) . ? N31 C33 1.4584(17) . ? O40 C40 1.2354(17) . ? C40 N41 1.3187(18) . ? N41 C42 1.449(2) . ? N41 C43 1.4521(18) . ? 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 N4 Co N14 109.40(4) . . ? N4 Co Cl2 111.06(3) . . ? N14 Co Cl2 107.98(3) . . ? N4 Co Cl1 106.65(3) . . ? N14 Co Cl1 107.14(3) . . ? Cl2 Co Cl1 114.474(14) . . ? C22 N1 C2 120.16(10) . . ? C22 N1 C12 121.30(10) . . ? C2 N1 C12 117.02(10) . . ? N1 C2 C3 111.55(10) . . ? N4 C3 N11 112.19(11) . . ? N4 C3 C2 124.35(11) . . ? N11 C3 C2 123.43(11) . . ? C3 N4 C5 105.67(10) . . ? C3 N4 Co 125.52(8) . . ? C5 N4 Co 128.80(8) . . ? C10 C5 C6 120.68(12) . . ? C10 C5 N4 108.53(11) . . ? C6 C5 N4 130.75(11) . . ? C7 C6 C5 117.10(12) . . ? C6 C7 C8 121.52(13) . . ? C9 C8 C7 121.95(13) . . ? C8 C9 C10 116.52(13) . . ? N11 C10 C5 105.97(11) . . ? N11 C10 C9 131.73(12) . . ? C5 C10 C9 122.23(12) . . ? C3 N11 C10 107.62(10) . . ? N1 C12 C13 114.56(10) . . ? N14 C13 N21 112.01(11) . . ? N14 C13 C12 125.11(11) . . ? N21 C13 C12 122.88(11) . . ? C13 N14 C15 105.50(10) . . ? C13 N14 Co 134.02(9) . . ? C15 N14 Co 120.19(8) . . ? C16 C15 C20 120.82(12) . . ? C16 C15 N14 130.40(11) . . ? C20 C15 N14 108.79(11) . . ? C17 C16 C15 117.11(12) . . ? C16 C17 C18 121.50(13) . . ? C19 C18 C17 121.85(13) . . ? C18 C19 C20 116.39(12) . . ? N21 C20 C19 131.89(12) . . ? N21 C20 C15 105.77(11) . . ? C19 C20 C15 122.33(12) . . ? C13 N21 C20 107.93(10) . . ? C23 C22 C27 120.79(11) . . ? C23 C22 N1 118.24(11) . . ? C27 C22 N1 120.95(11) . . ? C24 C23 C22 118.78(12) . . ? C24 C23 C28 119.80(12) . . ? C22 C23 C28 121.40(12) . . ? C25 C24 C23 120.77(13) . . ? C24 C25 C26 120.27(13) . . ? C25 C26 C27 121.21(13) . . ? C26 C27 C22 118.08(13) . . ? C26 C27 C29 119.94(13) . . ? C22 C27 C29 121.97(12) . . ? O30 C30 N31 125.17(13) . . ? C30 N31 C32 121.67(12) . . ? C30 N31 C33 121.00(12) . . ? C32 N31 C33 117.32(12) . . ? O40 C40 N41 125.57(14) . . ? C40 N41 C42 121.30(12) . . ? C40 N41 C43 121.25(13) . . ? C42 N41 C43 117.36(13) . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 31.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.319 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.051 #===END