Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _publ_contact_author_email P.BROTHERS@AUCKLAND.AC.NZ _publ_contact_author_name 'Prof Penelope Brothers' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry University of Auckland Private Bag 92019 Auckland NEW ZEALAND ; _publ_section_title ; Anionic carbonato and oxalato cobalt(III) nitrogen mustard complexes ; _publ_requested_category metalorganic loop_ _publ_author_name 'Penelope Brothers' 'George R. Clark' 'Peter R. Craig' 'William A. Denny' 'David C. Ware' 'William R. Wilson' data_prc51 _database_code_depnum_ccdc_archive 'CCDC 219491' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H48 B Co N4 O6 S4' _chemical_formula_sum 'C36 H48 B Co N4 O6 S4' _chemical_formula_weight 830.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.3348(10) _cell_length_b 12.7206(9) _cell_length_c 22.4320(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.979(2) _cell_angle_gamma 90.00 _cell_volume 4080.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 19.99 _exptl_crystal_description Tablet _exptl_crystal_colour Green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1744 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8716 _exptl_absorpt_correction_T_max 0.9608 _exptl_absorpt_process_details ; North, A.C.T., Phillips, D.C. & Mathews, F.S. (1968). Acta Cryst., A24, 351-359. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 5331 _diffrn_reflns_av_R_equivalents 0.1950 _diffrn_reflns_av_sigmaI/netI 0.1950 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5331 _reflns_number_gt 2607 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1994a)' _computing_cell_refinement 'Siemens SMART (Siemens, 1994a)' _computing_data_reduction 'Siemens SHELXTL (Siemens, 1994b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994b)' _computing_publication_material 'Siemens SHELXTL (Siemens, 1994b)' _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^)+(0.0936P)^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 5331 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1836 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2200 _refine_ls_wR_factor_gt 0.1729 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.27164(9) 0.36140(11) 0.33625(6) 0.0286(4) Uani 1 1 d . . . S1 S 0.36460(18) 0.4381(2) 0.27131(11) 0.0320(7) Uani 1 1 d . . . S2 S 0.38722(19) 0.2415(2) 0.32759(11) 0.0340(7) Uani 1 1 d . . . S3 S 0.18115(18) 0.5065(2) 0.34893(11) 0.0327(7) Uani 1 1 d . . . S4 S 0.34236(18) 0.4395(2) 0.41734(11) 0.0347(8) Uani 1 1 d . . . N1 N 0.2012(5) 0.2674(7) 0.3868(3) 0.038(2) Uani 1 1 d . . . H1A H 0.2411 0.2350 0.4143 0.045 Uiso 1 1 calc R . . H1B H 0.1593 0.3054 0.4067 0.045 Uiso 1 1 calc R . . N2 N 0.1897(5) 0.3037(6) 0.2706(3) 0.031(2) Uani 1 1 d . . . H2A H 0.1678 0.3568 0.2463 0.037 Uiso 1 1 calc R . . H2B H 0.2229 0.2590 0.2485 0.037 Uiso 1 1 calc R . . N3 N 0.5107(6) 0.3092(6) 0.2509(3) 0.026(2) Uani 1 1 d . . . N4 N 0.2505(5) 0.6171(7) 0.4456(3) 0.028(2) Uani 1 1 d . . . O1 O 0.5456(5) 0.2764(6) 0.1216(3) 0.050(2) Uani 1 1 d . . . H1C H 0.5092 0.2278 0.1283 0.075 Uiso 1 1 calc R . . O2 O 0.7016(5) 0.2776(6) 0.3125(3) 0.041(2) Uani 1 1 d . . . H2C H 0.6970 0.3264 0.3366 0.062 Uiso 1 1 calc R . . O3 O 0.3479(5) 0.5841(6) 0.6028(3) 0.051(2) Uani 1 1 d . . . H3A H 0.3270 0.6268 0.6265 0.077 Uiso 1 1 calc R . . O4 O 0.2668(5) 0.8155(6) 0.3833(3) 0.052(2) Uani 1 1 d . . . H4A H 0.3207 0.7971 0.3946 0.077 Uiso 1 1 calc R . . C1 C 0.1518(7) 0.1885(8) 0.3487(5) 0.039(3) Uani 1 1 d . . . H1D H 0.1018 0.1555 0.3699 0.047 Uiso 1 1 calc R . . H1E H 0.1951 0.1338 0.3372 0.047 Uiso 1 1 calc R . . C2 C 0.1111(7) 0.2475(9) 0.2939(4) 0.034(3) Uani 1 1 d . . . H2D H 0.0835 0.1983 0.2640 0.041 Uiso 1 1 calc R . . H2E H 0.0627 0.2969 0.3048 0.041 Uiso 1 1 calc R . . C3 C 0.4335(7) 0.3302(8) 0.2786(4) 0.029(3) Uani 1 1 d . . . C4 C 0.5452(7) 0.3900(8) 0.2099(4) 0.034(3) Uani 1 1 d . . . H4B H 0.6138 0.3895 0.2132 0.041 Uiso 1 1 calc R . . H4C H 0.5246 0.4594 0.2225 0.041 Uiso 1 1 calc R . . C5 C 0.5108(8) 0.3725(9) 0.1441(4) 0.044(3) Uani 1 1 d . . . H5A H 0.4423 0.3712 0.1407 0.052 Uiso 1 1 calc R . . H5B H 0.5315 0.4312 0.1200 0.052 Uiso 1 1 calc R . . C6 C 0.5616(6) 0.2112(9) 0.2589(4) 0.034(3) Uani 1 1 d . . . H6A H 0.5996 0.2006 0.2248 0.041 Uiso 1 1 calc R . . H6B H 0.5167 0.1532 0.2593 0.041 Uiso 1 1 calc R . . C7 C 0.6248(7) 0.2077(9) 0.3162(4) 0.036(3) Uani 1 1 d . . . H7A H 0.5890 0.2274 0.3502 0.043 Uiso 1 1 calc R . . H7B H 0.6482 0.1359 0.3230 0.043 Uiso 1 1 calc R . . C8 C 0.2580(6) 0.5350(8) 0.4106(4) 0.026(3) Uiso 1 1 d . . . C9 C 0.3168(7) 0.6252(8) 0.4998(4) 0.033(3) Uani 1 1 d . . . H9A H 0.3269 0.6995 0.5099 0.040 Uiso 1 1 calc R . . H9B H 0.3772 0.5950 0.4909 0.040 Uiso 1 1 calc R . . C10 C 0.2803(7) 0.5682(9) 0.5533(4) 0.042(3) Uani 1 1 d . . . H10A H 0.2195 0.5968 0.5625 0.051 Uiso 1 1 calc R . . H10B H 0.2730 0.4930 0.5447 0.051 Uiso 1 1 calc R . . C11 C 0.1747(7) 0.6945(8) 0.4383(4) 0.035(3) Uani 1 1 d . . . H11A H 0.1377 0.6914 0.4734 0.041 Uiso 1 1 calc R . . H11B H 0.1336 0.6754 0.4033 0.041 Uiso 1 1 calc R . . C12 C 0.2075(7) 0.8038(9) 0.4309(5) 0.038(3) Uani 1 1 d . . . H12A H 0.1530 0.8498 0.4237 0.045 Uiso 1 1 calc R . . H12B H 0.2412 0.8266 0.4682 0.045 Uiso 1 1 calc R . . B B -0.1556(8) 0.7816(9) 0.4250(5) 0.027(3) Uani 1 1 d . . . C21 C -0.2478(7) 0.8164(8) 0.4610(4) 0.023(2) Uani 1 1 d . . . C22 C -0.2489(7) 0.9114(9) 0.4913(4) 0.041(3) Uani 1 1 d . . . H22A H -0.1970 0.9562 0.4899 0.049 Uiso 1 1 calc R . . C23 C -0.3238(8) 0.9437(9) 0.5242(5) 0.045(3) Uani 1 1 d . . . H23A H -0.3223 1.0095 0.5433 0.054 Uiso 1 1 calc R . . C24 C -0.3990(8) 0.8785(10) 0.5280(5) 0.049(3) Uani 1 1 d . . . H24A H -0.4494 0.8999 0.5497 0.059 Uiso 1 1 calc R . . C25 C -0.4015(7) 0.7835(9) 0.5009(4) 0.032(3) Uani 1 1 d . . . H25A H -0.4530 0.7387 0.5040 0.039 Uiso 1 1 calc R . . C26 C -0.3253(7) 0.7524(8) 0.4678(4) 0.031(3) Uani 1 1 d . . . H26A H -0.3272 0.6858 0.4496 0.037 Uiso 1 1 calc R . . C31 C -0.1234(7) 0.8733(8) 0.3804(4) 0.025(2) Uani 1 1 d . . . C32 C -0.1804(7) 0.9567(8) 0.3592(4) 0.028(3) Uani 1 1 d . . . H32A H -0.2408 0.9621 0.3728 0.034 Uiso 1 1 calc R . . C33 C -0.1523(7) 1.0317(8) 0.3193(4) 0.032(3) Uani 1 1 d . . . H33A H -0.1921 1.0880 0.3079 0.038 Uiso 1 1 calc R . . C34 C -0.0656(7) 1.0235(9) 0.2963(4) 0.037(3) Uani 1 1 d . . . H34A H -0.0472 1.0720 0.2677 0.044 Uiso 1 1 calc R . . C35 C -0.0071(8) 0.9440(9) 0.3156(4) 0.040(3) Uani 1 1 d . . . H35A H 0.0533 0.9392 0.3019 0.049 Uiso 1 1 calc R . . C36 C -0.0376(7) 0.8697(8) 0.3559(4) 0.032(3) Uani 1 1 d . . . H36A H 0.0028 0.8137 0.3670 0.038 Uiso 1 1 calc R . . C41 C -0.1746(7) 0.6812(8) 0.3796(4) 0.027(3) Uani 1 1 d . . . C42 C -0.2594(7) 0.6667(8) 0.3444(4) 0.035(3) Uani 1 1 d . . . H42A H -0.3098 0.7122 0.3500 0.043 Uiso 1 1 calc R . . C43 C -0.2708(8) 0.5873(9) 0.3018(4) 0.036(3) Uani 1 1 d . . . H43A H -0.3286 0.5797 0.2799 0.043 Uiso 1 1 calc R . . C44 C -0.1981(8) 0.5190(9) 0.2912(4) 0.040(3) Uani 1 1 d . . . H44A H -0.2058 0.4662 0.2619 0.049 Uiso 1 1 calc R . . C45 C -0.1153(8) 0.5306(9) 0.3243(4) 0.040(3) Uani 1 1 d . . . H45A H -0.0655 0.4848 0.3180 0.048 Uiso 1 1 calc R . . C46 C -0.1036(7) 0.6094(9) 0.3675(4) 0.037(3) Uani 1 1 d . . . H46A H -0.0455 0.6148 0.3895 0.044 Uiso 1 1 calc R . . C51 C -0.0743(6) 0.7573(8) 0.4786(4) 0.024(3) Uani 1 1 d . . . C52 C -0.0170(7) 0.8359(8) 0.5028(4) 0.031(3) Uani 1 1 d . . . H52A H -0.0206 0.9025 0.4846 0.037 Uiso 1 1 calc R . . C53 C 0.0464(7) 0.8225(10) 0.5529(5) 0.041(3) Uani 1 1 d . . . H53A H 0.0819 0.8796 0.5684 0.049 Uiso 1 1 calc R . . C54 C 0.0559(7) 0.7255(10) 0.5790(4) 0.037(3) Uani 1 1 d . . . H54A H 0.0983 0.7151 0.6123 0.044 Uiso 1 1 calc R . . C55 C 0.0019(7) 0.6425(9) 0.5554(4) 0.036(3) Uani 1 1 d . . . H55A H 0.0083 0.5754 0.5728 0.044 Uiso 1 1 calc R . . C56 C -0.0623(7) 0.6582(8) 0.5059(4) 0.032(3) Uani 1 1 d . . . H56A H -0.0979 0.6010 0.4906 0.039 Uiso 1 1 calc R . . O5 O 0.1817(6) 0.7550(7) 0.2783(3) 0.062(2) Uani 1 1 d . . . O6 O 0.4711(5) 0.4279(7) 0.6227(4) 0.082(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0308(9) 0.0430(10) 0.0123(7) 0.0002(7) 0.0038(6) -0.0003(8) S1 0.0314(16) 0.045(2) 0.0209(15) 0.0034(13) 0.0076(12) 0.0007(14) S2 0.0361(17) 0.044(2) 0.0223(15) 0.0058(13) 0.0073(13) 0.0008(14) S3 0.0331(17) 0.049(2) 0.0161(15) -0.0031(13) 0.0020(12) 0.0001(14) S4 0.0365(17) 0.050(2) 0.0171(15) -0.0005(13) -0.0003(13) 0.0044(15) N1 0.036(5) 0.061(7) 0.016(5) -0.002(4) 0.007(4) 0.002(5) N2 0.032(5) 0.042(6) 0.019(5) -0.008(4) 0.004(4) 0.003(5) N3 0.033(5) 0.028(6) 0.018(5) -0.002(4) 0.009(4) -0.004(4) N4 0.037(5) 0.035(6) 0.012(4) -0.005(4) 0.006(4) -0.008(4) O1 0.063(5) 0.066(6) 0.023(4) -0.002(4) 0.008(4) -0.010(5) O2 0.036(4) 0.054(6) 0.035(5) -0.013(4) 0.009(4) -0.005(4) O3 0.065(5) 0.082(7) 0.007(4) -0.015(4) 0.003(4) 0.001(5) O4 0.034(5) 0.067(6) 0.057(5) 0.005(4) 0.018(4) 0.001(4) C1 0.043(7) 0.039(8) 0.038(7) -0.001(6) 0.024(6) -0.011(6) C2 0.032(7) 0.047(8) 0.026(6) 0.000(5) 0.008(5) -0.008(6) C3 0.030(6) 0.040(8) 0.018(6) 0.005(5) 0.003(5) -0.007(5) C4 0.030(6) 0.036(8) 0.039(7) 0.002(5) 0.015(6) 0.005(5) C5 0.053(8) 0.049(9) 0.031(7) 0.009(6) 0.013(6) 0.012(7) C6 0.017(6) 0.050(9) 0.038(7) -0.012(5) 0.009(5) 0.003(5) C7 0.036(7) 0.046(8) 0.025(7) 0.002(5) -0.003(5) 0.001(6) C9 0.045(7) 0.033(7) 0.021(6) -0.011(5) -0.007(5) -0.005(6) C10 0.052(8) 0.063(9) 0.011(6) 0.000(5) -0.003(5) -0.020(7) C11 0.032(7) 0.044(8) 0.030(7) -0.012(5) 0.010(5) 0.001(6) C12 0.034(7) 0.044(8) 0.035(7) -0.010(6) 0.005(6) 0.002(6) B 0.027(7) 0.034(8) 0.018(7) 0.005(5) -0.001(6) -0.002(6) C21 0.043(7) 0.017(7) 0.009(5) 0.008(4) 0.001(5) -0.001(5) C22 0.045(8) 0.043(9) 0.037(7) 0.001(6) 0.017(6) -0.024(6) C23 0.060(8) 0.039(9) 0.039(7) -0.010(6) 0.011(7) -0.006(7) C24 0.046(8) 0.069(11) 0.033(7) -0.005(7) 0.014(6) -0.005(7) C25 0.029(7) 0.038(8) 0.030(6) 0.003(5) 0.006(5) -0.006(5) C26 0.042(7) 0.035(8) 0.015(6) 0.002(5) -0.008(5) -0.003(6) C31 0.022(6) 0.044(8) 0.008(5) -0.004(5) -0.002(4) -0.003(5) C32 0.027(6) 0.043(8) 0.014(6) -0.005(5) 0.000(5) -0.005(5) C33 0.029(7) 0.044(8) 0.020(6) 0.010(5) -0.003(5) 0.004(6) C34 0.041(7) 0.063(9) 0.006(6) 0.011(5) -0.010(5) -0.008(6) C35 0.034(7) 0.067(10) 0.022(6) 0.000(6) 0.005(5) -0.009(7) C36 0.029(6) 0.048(8) 0.017(6) 0.009(5) 0.000(5) 0.006(6) C41 0.040(7) 0.023(7) 0.018(6) 0.005(5) -0.001(5) -0.002(5) C42 0.034(7) 0.049(9) 0.022(6) 0.000(5) -0.003(5) -0.002(6) C43 0.046(8) 0.044(8) 0.016(6) 0.005(5) -0.009(5) -0.012(6) C44 0.057(8) 0.045(9) 0.019(6) -0.009(5) 0.000(6) -0.016(7) C45 0.054(8) 0.048(8) 0.019(6) 0.002(5) 0.008(6) 0.000(6) C46 0.037(7) 0.054(9) 0.019(6) 0.002(6) 0.007(5) -0.004(6) C51 0.018(6) 0.041(8) 0.013(6) -0.003(5) 0.001(5) 0.006(5) C52 0.047(7) 0.034(8) 0.012(6) 0.006(5) 0.002(5) 0.004(6) C53 0.044(8) 0.058(9) 0.021(6) -0.010(6) 0.005(6) -0.006(6) C54 0.027(6) 0.073(10) 0.011(6) -0.008(6) 0.004(5) 0.003(7) C55 0.037(7) 0.058(9) 0.016(6) 0.018(6) 0.012(5) 0.023(7) C56 0.039(7) 0.041(8) 0.018(6) 0.001(5) 0.008(5) 0.014(6) O5 0.072(6) 0.085(7) 0.031(5) -0.013(4) 0.019(4) -0.003(5) O6 0.035(5) 0.078(7) 0.132(9) 0.008(6) -0.006(5) -0.003(5) _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 N2 1.962(7) . ? Co N1 1.974(8) . ? Co S4 2.251(3) . ? Co S1 2.263(3) . ? Co S2 2.270(3) . ? Co S3 2.285(3) . ? S1 C3 1.693(10) . ? S2 C3 1.738(10) . ? S3 C8 1.746(10) . ? S4 C8 1.714(10) . ? N1 C1 1.467(12) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N2 C2 1.461(11) . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N3 C3 1.334(11) . ? N3 C6 1.449(12) . ? N3 C4 1.486(12) . ? N4 C8 1.315(11) . ? N4 C11 1.467(12) . ? N4 C9 1.494(11) . ? O1 C5 1.427(12) . ? O1 H1C 0.8300 . ? O2 C7 1.422(11) . ? O2 H2C 0.8300 . ? O3 C10 1.436(10) . ? O3 H3A 0.8300 . ? O4 C12 1.419(11) . ? O4 H4A 0.8300 . ? C1 C2 1.522(13) . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C4 C5 1.539(13) . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C6 C7 1.521(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C9 C10 1.525(13) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C11 C12 1.480(13) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? B C31 1.624(14) . ? B C51 1.645(13) . ? B C41 1.644(15) . ? B C21 1.656(14) . ? C21 C22 1.387(13) . ? C21 C26 1.394(12) . ? C22 C23 1.405(14) . ? C22 H22A 0.9400 . ? C23 C24 1.367(14) . ? C23 H23A 0.9400 . ? C24 C25 1.352(14) . ? C24 H24A 0.9400 . ? C25 C26 1.419(13) . ? C25 H25A 0.9400 . ? C26 H26A 0.9400 . ? C31 C36 1.383(12) . ? C31 C32 1.402(13) . ? C32 C33 1.388(13) . ? C32 H32A 0.9400 . ? C33 C34 1.382(13) . ? C33 H33A 0.9400 . ? C34 C35 1.366(14) . ? C34 H34A 0.9400 . ? C35 C36 1.399(13) . ? C35 H35A 0.9400 . ? C36 H36A 0.9400 . ? C41 C46 1.408(13) . ? C41 C42 1.415(12) . ? C42 C43 1.392(13) . ? C42 H42A 0.9400 . ? C43 C44 1.390(14) . ? C43 H43A 0.9400 . ? C44 C45 1.364(14) . ? C44 H44A 0.9400 . ? C45 C46 1.396(14) . ? C45 H45A 0.9400 . ? C46 H46A 0.9400 . ? C51 C52 1.381(13) . ? C51 C56 1.407(13) . ? C52 C53 1.405(13) . ? C52 H52A 0.9400 . ? C53 C54 1.368(14) . ? C53 H53A 0.9400 . ? C54 C55 1.391(14) . ? C54 H54A 0.9400 . ? C55 C56 1.407(12) . ? C55 H55A 0.9400 . ? C56 H56A 0.9400 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Co N1 84.3(3) . . ? N2 Co S4 169.9(2) . . ? N1 Co S4 91.3(2) . . ? N2 Co S1 91.5(2) . . ? N1 Co S1 168.2(3) . . ? S4 Co S1 94.44(11) . . ? N2 Co S2 95.0(2) . . ? N1 Co S2 92.7(3) . . ? S4 Co S2 94.31(11) . . ? S1 Co S2 76.63(10) . . ? N2 Co S3 94.6(2) . . ? N1 Co S3 95.8(3) . . ? S4 Co S3 76.74(10) . . ? S1 Co S3 95.52(11) . . ? S2 Co S3 167.76(12) . . ? C3 S1 Co 87.3(3) . . ? C3 S2 Co 86.0(4) . . ? C8 S3 Co 86.2(3) . . ? C8 S4 Co 88.1(3) . . ? C1 N1 Co 109.0(6) . . ? C1 N1 H1A 109.9 . . ? Co N1 H1A 109.9 . . ? C1 N1 H1B 109.9 . . ? Co N1 H1B 109.9 . . ? H1A N1 H1B 108.3 . . ? C2 N2 Co 110.5(6) . . ? C2 N2 H2A 109.5 . . ? Co N2 H2A 109.5 . . ? C2 N2 H2B 109.5 . . ? Co N2 H2B 109.5 . . ? H2A N2 H2B 108.1 . . ? C3 N3 C6 122.7(8) . . ? C3 N3 C4 118.2(8) . . ? C6 N3 C4 119.0(8) . . ? C8 N4 C11 123.9(8) . . ? C8 N4 C9 117.8(8) . . ? C11 N4 C9 118.0(7) . . ? C5 O1 H1C 109.5 . . ? C7 O2 H2C 109.5 . . ? C10 O3 H3A 109.5 . . ? C12 O4 H4A 109.5 . . ? N1 C1 C2 106.0(9) . . ? N1 C1 H1D 110.5 . . ? C2 C1 H1D 110.5 . . ? N1 C1 H1E 110.5 . . ? C2 C1 H1E 110.5 . . ? H1D C1 H1E 108.7 . . ? N2 C2 C1 105.6(8) . . ? N2 C2 H2D 110.6 . . ? C1 C2 H2D 110.6 . . ? N2 C2 H2E 110.6 . . ? C1 C2 H2E 110.6 . . ? H2D C2 H2E 108.8 . . ? N3 C3 S1 127.9(8) . . ? N3 C3 S2 122.0(8) . . ? S1 C3 S2 110.0(6) . . ? N3 C4 C5 113.2(8) . . ? N3 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? N3 C4 H4C 108.9 . . ? C5 C4 H4C 108.9 . . ? H4B C4 H4C 107.7 . . ? O1 C5 C4 111.5(8) . . ? O1 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? O1 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? N3 C6 C7 113.4(8) . . ? N3 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? N3 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O2 C7 C6 110.5(8) . . ? O2 C7 H7A 109.6 . . ? C6 C7 H7A 109.6 . . ? O2 C7 H7B 109.6 . . ? C6 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N4 C8 S4 126.6(8) . . ? N4 C8 S3 124.4(8) . . ? S4 C8 S3 109.0(5) . . ? N4 C9 C10 111.9(8) . . ? N4 C9 H9A 109.2 . . ? C10 C9 H9A 109.2 . . ? N4 C9 H9B 109.2 . . ? C10 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? O3 C10 C9 106.9(8) . . ? O3 C10 H10A 110.3 . . ? C9 C10 H10A 110.3 . . ? O3 C10 H10B 110.3 . . ? C9 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? N4 C11 C12 113.9(8) . . ? N4 C11 H11A 108.8 . . ? C12 C11 H11A 108.8 . . ? N4 C11 H11B 108.8 . . ? C12 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? O4 C12 C11 113.2(8) . . ? O4 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? O4 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C31 B C51 111.6(8) . . ? C31 B C41 102.6(8) . . ? C51 B C41 112.7(9) . . ? C31 B C21 112.2(8) . . ? C51 B C21 104.0(7) . . ? C41 B C21 113.9(8) . . ? C22 C21 C26 114.7(9) . . ? C22 C21 B 120.6(9) . . ? C26 C21 B 124.5(9) . . ? C21 C22 C23 123.2(10) . . ? C21 C22 H22A 118.4 . . ? C23 C22 H22A 118.4 . . ? C24 C23 C22 119.4(11) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C25 C24 C23 120.7(11) . . ? C25 C24 H24A 119.7 . . ? C23 C24 H24A 119.7 . . ? C24 C25 C26 119.2(10) . . ? C24 C25 H25A 120.4 . . ? C26 C25 H25A 120.4 . . ? C21 C26 C25 122.9(10) . . ? C21 C26 H26A 118.6 . . ? C25 C26 H26A 118.6 . . ? C36 C31 C32 113.8(9) . . ? C36 C31 B 121.3(9) . . ? C32 C31 B 124.7(9) . . ? C33 C32 C31 123.4(9) . . ? C33 C32 H32A 118.3 . . ? C31 C32 H32A 118.3 . . ? C34 C33 C32 119.9(10) . . ? C34 C33 H33A 120.1 . . ? C32 C33 H33A 120.1 . . ? C35 C34 C33 119.1(10) . . ? C35 C34 H34A 120.5 . . ? C33 C34 H34A 120.5 . . ? C34 C35 C36 119.6(10) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C31 C36 C35 124.1(10) . . ? C31 C36 H36A 117.9 . . ? C35 C36 H36A 117.9 . . ? C46 C41 C42 114.4(9) . . ? C46 C41 B 122.1(9) . . ? C42 C41 B 123.1(9) . . ? C43 C42 C41 122.2(10) . . ? C43 C42 H42A 118.9 . . ? C41 C42 H42A 118.9 . . ? C44 C43 C42 121.2(10) . . ? C44 C43 H43A 119.4 . . ? C42 C43 H43A 119.4 . . ? C45 C44 C43 118.2(10) . . ? C45 C44 H44A 120.9 . . ? C43 C44 H44A 120.9 . . ? C44 C45 C46 121.0(11) . . ? C44 C45 H45A 119.5 . . ? C46 C45 H45A 119.5 . . ? C45 C46 C41 123.0(10) . . ? C45 C46 H46A 118.5 . . ? C41 C46 H46A 118.5 . . ? C52 C51 C56 115.2(9) . . ? C52 C51 B 121.6(9) . . ? C56 C51 B 123.1(9) . . ? C51 C52 C53 124.1(10) . . ? C51 C52 H52A 118.0 . . ? C53 C52 H52A 118.0 . . ? C54 C53 C52 119.4(10) . . ? C54 C53 H53A 120.3 . . ? C52 C53 H53A 120.3 . . ? C53 C54 C55 119.1(10) . . ? C53 C54 H54A 120.5 . . ? C55 C54 H54A 120.5 . . ? C54 C55 C56 120.5(11) . . ? C54 C55 H55A 119.7 . . ? C56 C55 H55A 119.7 . . ? C51 C56 C55 121.6(10) . . ? C51 C56 H56A 119.2 . . ? C55 C56 H56A 119.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.739 _refine_diff_density_min -0.732 _refine_diff_density_rms 0.112 data_prc3a _database_code_depnum_ccdc_archive 'CCDC 219492' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H26 Cl Co N4 O9' _chemical_formula_sum 'C18 H26 Cl Co N4 O9' _chemical_formula_weight 536.81 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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 26.6696(1) _cell_length_b 41.0358(2) _cell_length_c 7.9862(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8740.17(12) _cell_formula_units_Z 16 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 3571 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 26.36 _exptl_crystal_id 'Compound 8' _exptl_crystal_description tablet _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4448 _exptl_absorpt_coefficient_mu 0.967 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; North, A.C.T., Phillips, D.C. & Mathews, F.S. (1968). Acta Cryst., A24,351-359. ; _exptl_absorpt_correction_T_min 0.6984 _exptl_absorpt_correction_T_max 0.7941 _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 3571 _diffrn_reflns_av_R_equivalents 0.03 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 50 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.36 _reflns_number_total 3571 _reflns_number_gt 3514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART (Siemens, 1994a)' _computing_cell_refinement 'Siemens SMART (Siemens, 1994a)' _computing_data_reduction 'Siemens SHELXTL (Siemens, 1994b)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL (Siemens, 1994b)' _computing_publication_material 'Siemens SHELXTL (Siemens, 1994b)' _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^)+(0.0576P)^2^+59.6566P] 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 SHELXL _refine_ls_extinction_coef 0.00119(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.011(19) _refine_ls_number_reflns 3571 _refine_ls_number_parameters 285 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1097 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.022 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.114948(17) 0.084389(11) 0.08801(7) 0.01651(16) Uani 1 1 d . . . Cl1 Cl 0.08204(4) 0.24023(2) -0.30186(16) 0.0332(3) Uani 1 1 d . . . O1 O 0.06368(10) 0.07499(6) -0.0696(4) 0.0205(6) Uani 1 1 d . . . O2 O -0.01392(11) 0.05532(8) -0.0937(5) 0.0321(7) Uani 1 1 d . . . O3 O 0.16334(11) 0.09447(6) 0.2528(4) 0.0217(6) Uani 1 1 d . . . O4 O 0.19215(11) 0.13569(7) 0.4099(4) 0.0281(7) Uani 1 1 d . . . O5 O 0.0955(3) 0.2398(2) -0.1369(14) 0.133(3) Uiso 1 1 d . . . O6 O 0.0526(2) 0.21311(13) -0.3454(8) 0.0774(15) Uiso 1 1 d . . . O7 O 0.05816(18) 0.27038(11) -0.3400(7) 0.0646(12) Uiso 1 1 d . . . O8 O 0.12700(16) 0.23709(11) -0.4037(7) 0.0605(11) Uiso 1 1 d . . . O9 O 0.33244(15) 0.25424(10) 0.1281(7) 0.0554(12) Uani 1 1 d D . . H9A H 0.315(2) 0.2698(12) 0.153(9) 0.082 Uiso 1 1 d D . . H9B H 0.349(3) 0.2571(18) 0.043(6) 0.082 Uiso 1 1 d D . . N1 N 0.14321(12) 0.04102(7) 0.0657(5) 0.0225(7) Uani 1 1 d . . . HN1A H 0.1551 0.0343 0.1668 0.027 Uiso 1 1 calc R . . HN1B H 0.1187 0.0269 0.0337 0.027 Uiso 1 1 calc R . . N2 N 0.16122(12) 0.09763(8) -0.1060(4) 0.0202(7) Uani 1 1 d . . . N3 N 0.08960(12) 0.12769(8) 0.1350(4) 0.0200(7) Uani 1 1 d . . . N4 N 0.06803(13) 0.06625(7) 0.2477(5) 0.0200(7) Uani 1 1 d . . . C1 C 0.02300(15) 0.06196(9) -0.0089(6) 0.0225(9) Uani 1 1 d . . . C2 C 0.02496(15) 0.05640(9) 0.1766(6) 0.0218(8) Uani 1 1 d . . . C3 C -0.01334(16) 0.04262(10) 0.2699(6) 0.0255(9) Uani 1 1 d . . . H3 H -0.0432 0.0358 0.2182 0.031 Uiso 1 1 calc R . . C4 C -0.00670(12) 0.03916(7) 0.4416(5) 0.0289(10) Uani 1 1 d . . . H4 H -0.0324 0.0303 0.5081 0.035 Uiso 1 1 calc R . . C5 C 0.03772(12) 0.04872(7) 0.5134(5) 0.0287(9) Uani 1 1 d R . . H5 H 0.0431 0.0461 0.6289 0.034 Uiso 1 1 calc R . . C6 C 0.07468(16) 0.06234(10) 0.4124(6) 0.0251(9) Uani 1 1 d . . . H6 H 0.1051 0.0690 0.4612 0.030 Uiso 1 1 calc R . . C7 C 0.16190(13) 0.12426(9) 0.3112(5) 0.0189(8) Uani 1 1 d . . . C8 C 0.11830(14) 0.14364(9) 0.2487(6) 0.0203(8) Uani 1 1 d . . . C9 C 0.10639(16) 0.17473(10) 0.3049(6) 0.0264(9) Uani 1 1 d . . . H9 H 0.1267 0.1856 0.3834 0.032 Uiso 1 1 calc R . . C10 C 0.06296(17) 0.18945(10) 0.2406(7) 0.0326(10) Uani 1 1 d . . . H10 H 0.0539 0.2106 0.2747 0.039 Uiso 1 1 calc R . . C11 C 0.03387(16) 0.17297(10) 0.1283(7) 0.0304(10) Uani 1 1 d . . . H11 H 0.0043 0.1825 0.0870 0.037 Uiso 1 1 calc R . . C12 C 0.04816(14) 0.14197(9) 0.0750(6) 0.0244(8) Uani 1 1 d . . . H12 H 0.0284 0.1309 -0.0042 0.029 Uiso 1 1 calc R . . C13 C 0.18401(16) 0.04030(10) -0.0579(6) 0.0288(10) Uani 1 1 d . . . H13A H 0.1870 0.0185 -0.1076 0.035 Uiso 1 1 calc R . . H13B H 0.2160 0.0460 -0.0050 0.035 Uiso 1 1 calc R . . C14 C 0.17034(16) 0.06500(10) -0.1893(6) 0.0278(9) Uani 1 1 d . . . H14A H 0.1400 0.0580 -0.2487 0.033 Uiso 1 1 calc R . . H14B H 0.1976 0.0669 -0.2710 0.033 Uiso 1 1 calc R . . C15 C 0.21038(14) 0.11196(10) -0.0493(6) 0.0248(9) Uani 1 1 d . . . H15A H 0.2244 0.0980 0.0385 0.030 Uiso 1 1 calc R . . H15B H 0.2039 0.1334 0.0005 0.030 Uiso 1 1 calc R . . C16 C 0.24967(16) 0.11591(11) -0.1885(6) 0.0323(10) Uani 1 1 d . . . H16A H 0.2628 0.0947 -0.2190 0.048 Uiso 1 1 calc R . . H16B H 0.2768 0.1296 -0.1488 0.048 Uiso 1 1 calc R . . H16C H 0.2342 0.1259 -0.2857 0.048 Uiso 1 1 calc R . . C17 C 0.13678(17) 0.11892(12) -0.2349(7) 0.0308(10) Uani 1 1 d . . . H17A H 0.1014 0.1127 -0.2427 0.037 Uiso 1 1 calc R . . H17B H 0.1522 0.1142 -0.3436 0.037 Uiso 1 1 calc R . . C18 C 0.1393(2) 0.15576(12) -0.2061(7) 0.0402(13) Uani 1 1 d . . . H18A H 0.1277 0.1607 -0.0939 0.060 Uiso 1 1 calc R . . H18B H 0.1181 0.1668 -0.2872 0.060 Uiso 1 1 calc R . . H18C H 0.1736 0.1631 -0.2191 0.060 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 0.0167(2) 0.0166(2) 0.0163(3) 0.0004(2) -0.0016(2) -0.00163(17) Cl1 0.0360(6) 0.0282(5) 0.0354(7) 0.0046(4) -0.0013(5) 0.0027(4) O1 0.0206(13) 0.0243(13) 0.0165(15) -0.0002(11) -0.0010(11) -0.0039(10) O2 0.0250(16) 0.0377(17) 0.0335(19) -0.0002(14) -0.0067(14) -0.0101(12) O3 0.0225(14) 0.0207(13) 0.0218(16) -0.0018(12) -0.0044(12) -0.0008(10) O4 0.0274(15) 0.0343(15) 0.0228(17) -0.0039(12) -0.0068(13) -0.0044(11) O9 0.053(2) 0.042(2) 0.072(4) 0.016(2) 0.010(2) 0.0200(17) N1 0.0260(16) 0.0192(14) 0.022(2) -0.0010(14) 0.0003(15) 0.0008(11) N2 0.0167(15) 0.0217(16) 0.0223(19) -0.0015(13) -0.0001(13) -0.0033(11) N3 0.0196(15) 0.0212(14) 0.0191(18) -0.0017(12) -0.0009(13) -0.0032(12) N4 0.0256(17) 0.0150(14) 0.0193(18) -0.0019(13) -0.0002(14) 0.0006(12) C1 0.022(2) 0.0206(18) 0.026(2) -0.0022(16) 0.0000(17) -0.0017(14) C2 0.0211(18) 0.0179(17) 0.026(2) 0.0020(15) 0.0051(17) -0.0007(13) C3 0.021(2) 0.0222(18) 0.033(2) 0.0028(17) 0.0067(17) -0.0025(14) C4 0.027(2) 0.0240(19) 0.036(3) 0.0075(18) 0.015(2) 0.0033(15) C5 0.041(3) 0.030(2) 0.016(2) 0.0015(16) 0.0064(19) 0.0057(18) C6 0.028(2) 0.0248(18) 0.023(2) 0.0010(16) -0.0002(17) -0.0007(15) C7 0.0205(18) 0.0240(17) 0.012(2) 0.0011(15) 0.0016(15) -0.0045(13) C8 0.0189(18) 0.0195(18) 0.023(2) 0.0018(15) 0.0002(16) -0.0027(13) C9 0.033(2) 0.0225(18) 0.024(2) -0.0042(16) -0.0004(18) -0.0047(15) C10 0.035(2) 0.0212(18) 0.041(3) -0.0005(18) 0.005(2) 0.0043(16) C11 0.028(2) 0.0253(18) 0.038(3) 0.0043(18) -0.0010(19) 0.0051(16) C12 0.0190(17) 0.0263(19) 0.028(2) -0.0002(18) -0.0027(18) -0.0014(13) C13 0.024(2) 0.0249(19) 0.038(3) -0.0028(18) 0.007(2) 0.0024(14) C14 0.027(2) 0.032(2) 0.024(2) -0.0058(18) 0.0064(18) -0.0070(15) C15 0.0201(19) 0.030(2) 0.025(2) 0.0008(17) -0.0020(18) -0.0070(15) C16 0.025(2) 0.042(2) 0.030(3) 0.004(2) 0.004(2) -0.0053(17) C17 0.025(2) 0.043(3) 0.025(2) 0.0117(19) -0.0019(18) -0.0027(17) C18 0.042(3) 0.034(2) 0.044(4) 0.019(2) 0.013(2) 0.0044(19) _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 O3 1.889(3) . ? Co O1 1.898(3) . ? Co N4 1.935(4) . ? Co N3 1.938(3) . ? Co N1 1.941(3) . ? Co N2 2.054(3) . ? Cl1 O5 1.365(11) . ? Cl1 O6 1.406(5) . ? Cl1 O7 1.424(5) . ? Cl1 O8 1.455(5) . ? O1 C1 1.303(5) . ? O2 C1 1.226(5) . ? O3 C7 1.309(5) . ? O4 C7 1.221(5) . ? O9 H9A 0.81(2) . ? O9 H9B 0.82(2) . ? N1 C13 1.469(6) . ? N1 HN1A 0.9100 . ? N1 HN1B 0.9100 . ? N2 C15 1.507(5) . ? N2 C14 1.515(5) . ? N2 C17 1.499(6) . ? N3 C12 1.339(5) . ? N3 C8 1.356(5) . ? N4 C6 1.337(6) . ? N4 C2 1.344(6) . ? C1 C2 1.500(6) . ? C2 C3 1.385(6) . ? C3 C4 1.390(6) . ? C3 H3 0.9400 . ? C4 C5 1.3733 . ? C4 H4 0.9400 . ? C5 C6 1.391(5) . ? C5 H5 0.9400 . ? C6 H6 0.9400 . ? C7 C8 1.494(5) . ? C8 C9 1.389(6) . ? C9 C10 1.404(6) . ? C9 H9 0.9400 . ? C10 C11 1.365(7) . ? C10 H10 0.9400 . ? C11 C12 1.395(6) . ? C11 H11 0.9400 . ? C12 H12 0.9400 . ? C13 C14 1.504(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.536(6) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C17 C18 1.531(7) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C18 H18C 0.9700 . ? 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 O3 Co O1 177.00(13) . . ? O3 Co N4 93.84(15) . . ? O1 Co N4 83.86(13) . . ? O3 Co N3 84.41(13) . . ? O1 Co N3 93.64(13) . . ? N4 Co N3 89.98(14) . . ? O3 Co N1 89.97(14) . . ? O1 Co N1 91.86(14) . . ? N4 Co N1 87.65(14) . . ? N3 Co N1 173.75(16) . . ? O3 Co N2 93.28(12) . . ? O1 Co N2 89.20(13) . . ? N4 Co N2 170.81(14) . . ? N3 Co N2 96.49(14) . . ? N1 Co N2 86.55(14) . . ? O5 Cl1 O6 112.1(5) . . ? O5 Cl1 O7 109.5(4) . . ? O6 Cl1 O7 112.6(3) . . ? O5 Cl1 O8 108.8(4) . . ? O6 Cl1 O8 104.6(3) . . ? O7 Cl1 O8 109.0(3) . . ? C1 O1 Co 115.9(3) . . ? C7 O3 Co 115.6(2) . . ? H9A O9 H9B 113(4) . . ? C13 N1 Co 111.6(2) . . ? C13 N1 HN1A 109.3 . . ? Co N1 HN1A 109.3 . . ? C13 N1 HN1B 109.3 . . ? Co N1 HN1B 109.3 . . ? HN1A N1 HN1B 108.0 . . ? C15 N2 C14 109.7(3) . . ? C15 N2 C17 110.9(3) . . ? C14 N2 C17 106.5(4) . . ? C15 N2 Co 113.5(3) . . ? C14 N2 Co 101.2(2) . . ? C17 N2 Co 114.3(3) . . ? C12 N3 C8 119.6(3) . . ? C12 N3 Co 128.3(3) . . ? C8 N3 Co 112.0(3) . . ? C6 N4 C2 119.5(4) . . ? C6 N4 Co 127.5(3) . . ? C2 N4 Co 113.0(3) . . ? O2 C1 O1 123.7(4) . . ? O2 C1 C2 122.7(4) . . ? O1 C1 C2 113.6(4) . . ? N4 C2 C3 121.7(4) . . ? N4 C2 C1 113.7(4) . . ? C3 C2 C1 124.6(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 H3 120.7 . . ? C4 C3 H3 120.7 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 119.0(2) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? N4 C6 C5 121.6(4) . . ? N4 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? O4 C7 O3 124.7(4) . . ? O4 C7 C8 121.7(3) . . ? O3 C7 C8 113.6(3) . . ? N3 C8 C9 122.0(4) . . ? N3 C8 C7 114.0(3) . . ? C9 C8 C7 124.0(4) . . ? C10 C9 C8 117.7(4) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C11 C10 C9 119.8(4) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 119.8(4) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? N3 C12 C11 121.0(4) . . ? N3 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? N1 C13 C14 106.0(3) . . ? N1 C13 H13A 110.5 . . ? C14 C13 H13A 110.5 . . ? N1 C13 H13B 110.5 . . ? C14 C13 H13B 110.5 . . ? H13A C13 H13B 108.7 . . ? C13 C14 N2 109.2(4) . . ? C13 C14 H14A 109.9 . . ? N2 C14 H14A 109.9 . . ? C13 C14 H14B 109.8 . . ? N2 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? N2 C15 C16 114.7(4) . . ? N2 C15 H15A 108.6 . . ? C16 C15 H15A 108.6 . . ? N2 C15 H15B 108.6 . . ? C16 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N2 C17 C18 117.0(4) . . ? N2 C17 H17A 108.1 . . ? C18 C17 H17A 108.1 . . ? N2 C17 H17B 108.1 . . ? C18 C17 H17B 108.1 . . ? H17A C17 H17B 107.3 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.956 _refine_diff_density_min -0.617 _refine_diff_density_rms 0.092