Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Trevor Hambley' _publ_contact_author_address ; School of Chemistry, Building F11 University of Sydney Sydney NSW 2006 AUSTRALIA ; _publ_contact_author_email T.HAMBLEY@CHEM.USYD.EDU.AU _publ_section_title ; Models of hypoxia activated prodrugs: Co(III) complexes of hydroxamic acids ; loop_ _publ_author_name 'T. Hambley' 'Timothy W. Failes' data_twf31 _database_code_depnum_ccdc_archive 'CCDC 282771' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(mmst)tpa]ClO4' _chemical_formula_sum 'C33 H53 Cl Co N7 O13' _chemical_formula_weight 850.21 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5889(13) _cell_length_b 18.950(3) _cell_length_c 12.6315(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.277(3) _cell_angle_gamma 90.00 _cell_volume 2039.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhomb _exptl_crystal_colour green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.555 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18214 _diffrn_reflns_av_R_equivalents 0.0160 _diffrn_reflns_av_sigmaI/netI 0.0358 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9225 _reflns_number_gt 8891 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.0518P)^2^+0.0984P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(7) _refine_ls_number_reflns 9225 _refine_ls_number_parameters 538 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.031 _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 O1W O -0.3781(3) 0.85109(13) 0.2771(2) 0.0566(5) Uani 1 1 d . . . O2W O 0.3947(3) 0.94623(11) 0.30108(19) 0.0556(5) Uani 1 1 d . . . O3W O 0.0732(3) 0.85423(14) 0.4116(2) 0.0658(6) Uani 1 1 d . . . O4W O 0.3697(3) 0.90624(13) 0.50130(19) 0.0689(6) Uani 1 1 d . . . H1W H 0.341(2) 0.9481(10) 0.3477(15) 0.000(4) Uiso 1 1 d . . . H2N H 0.173(3) 0.9724(14) 0.187(2) 0.036(7) Uiso 1 1 d . . . H2W H 0.415(6) 0.999(3) 0.259(4) 0.114(15) Uiso 1 1 d . . . H3N H 0.136(3) 1.1695(13) 0.057(2) 0.030(6) Uiso 1 1 d . . . H3O H -0.033(3) 0.8395(16) 0.249(2) 0.037(9) Uiso 1 1 d . . . H3W H 0.114(3) 0.8637(15) 0.373(2) 0.022(8) Uiso 1 1 d D . . H4W H 0.140(5) 0.877(2) 0.473(3) 0.096(14) Uiso 1 1 d D . . H5W H -0.268(6) 0.860(2) 0.258(3) 0.091(13) Uiso 1 1 d . . . H6W H -0.365(5) 0.880(2) 0.324(4) 0.084(15) Uiso 1 1 d . . . C1 C 0.0377(2) 0.73812(9) 0.14620(13) 0.0190(3) Uani 1 1 d . . . C2 C -0.0193(2) 0.81206(9) 0.11834(14) 0.0214(3) Uani 1 1 d . . . H2 H -0.1029 0.8089 0.0580 0.026 Uiso 1 1 calc R . . C3 C 0.1129(2) 0.85798(9) 0.08361(14) 0.0207(3) Uani 1 1 d . . . H3 H 0.2016 0.8592 0.1406 0.025 Uiso 1 1 calc R . . C4 C 0.1673(2) 0.82859(9) -0.01914(15) 0.0257(4) Uani 1 1 d . . . H4A H 0.2101 0.7818 -0.0042 0.031 Uiso 1 1 calc R . . H4B H 0.0762 0.8237 -0.0725 0.031 Uiso 1 1 calc R . . C5 C 0.2906(2) 0.87307(10) -0.06684(17) 0.0303(4) Uani 1 1 d . . . H5 H 0.2496 0.9212 -0.0774 0.036 Uiso 1 1 calc R . . C6 C 0.3161(3) 0.84317(14) -0.17632(19) 0.0440(5) Uani 1 1 d . . . H6A H 0.3533 0.7955 -0.1681 0.066 Uiso 1 1 calc R . . H6B H 0.3923 0.8714 -0.2064 0.066 Uiso 1 1 calc R . . H6C H 0.2187 0.8439 -0.2229 0.066 Uiso 1 1 calc R . . C7 C 0.4452(3) 0.87672(14) 0.0070(2) 0.0438(5) Uani 1 1 d . . . H7A H 0.4293 0.9011 0.0714 0.066 Uiso 1 1 calc R . . H7B H 0.5216 0.9016 -0.0280 0.066 Uiso 1 1 calc R . . H7C H 0.4822 0.8298 0.0242 0.066 Uiso 1 1 calc R . . C8 C 0.0480(2) 0.93247(9) 0.06304(14) 0.0209(3) Uani 1 1 d . . . C9 C 0.0603(2) 1.05531(9) 0.13014(14) 0.0227(3) Uani 1 1 d . . . H9 H 0.0169 1.0659 0.0563 0.027 Uiso 1 1 calc R . . C10 C -0.0662(3) 1.07434(10) 0.20393(15) 0.0297(4) Uani 1 1 d . . . C11 C -0.1116(3) 1.15250(11) 0.1900(2) 0.0401(5) Uani 1 1 d . . . H11A H -0.2019 1.1619 0.2254 0.060 Uiso 1 1 calc R . . H11B H -0.1357 1.1630 0.1153 0.060 Uiso 1 1 calc R . . H11C H -0.0256 1.1814 0.2204 0.060 Uiso 1 1 calc R . . C12 C -0.0062(4) 1.05990(16) 0.32158(19) 0.0508(6) Uani 1 1 d . . . H12A H 0.0799 1.0909 0.3444 0.076 Uiso 1 1 calc R . . H12B H 0.0282 1.0118 0.3296 0.076 Uiso 1 1 calc R . . H12C H -0.0894 1.0680 0.3643 0.076 Uiso 1 1 calc R . . C13 C -0.2131(3) 1.02995(13) 0.1696(2) 0.0420(5) Uani 1 1 d . . . H13A H -0.2923 1.0411 0.2142 0.063 Uiso 1 1 calc R . . H13B H -0.1871 0.9808 0.1766 0.063 Uiso 1 1 calc R . . H13C H -0.2519 1.0402 0.0966 0.063 Uiso 1 1 calc R . . C14 C 0.2116(2) 1.09801(10) 0.15686(15) 0.0256(4) Uani 1 1 d . . . C15 C 0.3517(3) 1.20656(11) 0.12668(18) 0.0363(5) Uani 1 1 d . . . H15A H 0.3554 1.2259 0.1972 0.054 Uiso 1 1 calc R . . H15B H 0.3411 1.2442 0.0753 0.054 Uiso 1 1 calc R . . H15C H 0.4467 1.1810 0.1210 0.054 Uiso 1 1 calc R . . C16 C -0.1036(2) 0.65789(11) 0.36916(15) 0.0274(4) Uani 1 1 d . . . H16 H -0.0809 0.7058 0.3681 0.033 Uiso 1 1 calc R . . C17 C -0.2247(2) 0.63494(15) 0.42343(15) 0.0340(4) Uani 1 1 d . . . H17 H -0.2838 0.6670 0.4573 0.041 Uiso 1 1 calc R . . C18 C -0.2559(2) 0.56339(13) 0.42626(17) 0.0353(5) Uani 1 1 d . . . H18 H -0.3347 0.5468 0.4639 0.042 Uiso 1 1 calc R . . C19 C -0.1691(2) 0.51633(11) 0.37262(15) 0.0284(4) Uani 1 1 d . . . H19 H -0.1897 0.4682 0.3732 0.034 Uiso 1 1 calc R . . C20 C -0.0521(2) 0.54262(10) 0.31873(14) 0.0223(3) Uani 1 1 d . . . C21 C 0.0512(2) 0.49869(9) 0.25741(15) 0.0212(3) Uani 1 1 d . . . H21A H 0.0090 0.4971 0.1825 0.025 Uiso 1 1 calc R . . H21B H 0.0581 0.4508 0.2848 0.025 Uiso 1 1 calc R . . C22 C 0.2998(2) 0.70538(10) 0.45257(16) 0.0271(4) Uani 1 1 d . . . H22 H 0.2645 0.7472 0.4193 0.033 Uiso 1 1 calc R . . C23 C 0.3734(2) 0.70712(11) 0.55671(16) 0.0314(4) Uani 1 1 d . . . H23 H 0.3882 0.7497 0.5931 0.038 Uiso 1 1 calc R . . C24 C 0.4243(2) 0.64474(12) 0.60550(15) 0.0315(4) Uani 1 1 d . . . H24 H 0.4749 0.6450 0.6751 0.038 Uiso 1 1 calc R . . C25 C 0.4000(2) 0.58189(11) 0.55044(15) 0.0265(4) Uani 1 1 d . . . H25 H 0.4323 0.5394 0.5828 0.032 Uiso 1 1 calc R . . C26 C 0.3265(2) 0.58313(10) 0.44611(14) 0.0204(3) Uani 1 1 d . . . C27 C 0.2973(2) 0.51760(9) 0.37963(14) 0.0250(4) Uani 1 1 d . . . H27A H 0.2370 0.4845 0.4165 0.030 Uiso 1 1 calc R . . H27B H 0.3970 0.4956 0.3713 0.030 Uiso 1 1 calc R . . C28 C 0.4594(2) 0.69287(10) 0.19134(15) 0.0263(4) Uani 1 1 d . . . H28 H 0.4240 0.7371 0.2094 0.032 Uiso 1 1 calc R . . C29 C 0.6057(2) 0.68630(12) 0.15681(16) 0.0313(4) Uani 1 1 d . . . H29 H 0.6682 0.7260 0.1520 0.038 Uiso 1 1 calc R . . C30 C 0.6583(2) 0.62074(11) 0.12966(15) 0.0313(5) Uani 1 1 d . . . H30 H 0.7561 0.6157 0.1064 0.038 Uiso 1 1 calc R . . C31 C 0.5631(2) 0.56255(11) 0.13757(16) 0.0283(4) Uani 1 1 d . . . H31 H 0.5964 0.5179 0.1198 0.034 Uiso 1 1 calc R . . C32 C 0.4184(2) 0.57152(10) 0.17214(14) 0.0223(4) Uani 1 1 d . . . C33 C 0.3033(2) 0.51288(9) 0.18329(14) 0.0215(3) Uani 1 1 d . . . H33A H 0.2343 0.5067 0.1170 0.026 Uiso 1 1 calc R . . H33B H 0.3587 0.4689 0.2004 0.026 Uiso 1 1 calc R . . N1 N -0.00277(17) 0.68708(7) 0.08172(11) 0.0194(3) Uani 1 1 d . . . N2 N 0.10352(19) 0.98090(8) 0.13622(13) 0.0236(3) Uani 1 1 d . . . N3 N 0.2177(2) 1.15897(8) 0.10610(13) 0.0265(3) Uani 1 1 d . . . N4 N -0.01866(17) 0.61301(8) 0.31834(12) 0.0201(3) Uani 1 1 d . . . N5 N 0.27858(16) 0.64416(8) 0.39878(11) 0.0198(3) Uani 1 1 d . . . N6 N 0.36791(15) 0.63576(10) 0.19898(10) 0.0207(2) Uani 1 1 d . . . N7 N 0.21029(18) 0.53287(8) 0.27119(12) 0.0186(3) Uani 1 1 d . . . O1 O 0.06221(14) 0.62182(6) 0.11902(9) 0.0192(2) Uani 1 1 d . . . O2 O 0.12988(16) 0.73008(6) 0.23831(10) 0.0217(2) Uani 1 1 d . . . O3 O -0.08448(19) 0.84272(8) 0.20597(13) 0.0299(3) Uani 1 1 d . . . O4 O -0.04833(16) 0.94530(7) -0.01462(10) 0.0278(3) Uani 1 1 d . . . O5 O 0.32226(19) 1.07665(8) 0.22224(13) 0.0384(4) Uani 1 1 d . . . Co1 Co 0.17014(2) 0.633573(12) 0.255949(15) 0.01677(6) Uani 1 1 d . . . O6 O 0.6789(4) 0.80389(16) 0.4926(2) 0.0948(9) Uani 1 1 d . . . O7 O 0.6625(4) 0.85023(12) 0.6623(3) 0.0958(10) Uani 1 1 d . . . O8 O 0.7958(5) 0.74692(13) 0.6392(2) 0.0971(10) Uani 1 1 d . . . O9 O 0.8948(4) 0.85713(18) 0.5869(3) 0.1077(12) Uani 1 1 d . . . Cl1 Cl 0.76201(9) 0.81478(3) 0.59755(6) 0.05227(16) 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 O1W 0.0472(11) 0.0614(14) 0.0601(13) 0.0118(11) 0.0027(10) 0.0015(9) O2W 0.0600(12) 0.0402(10) 0.0615(13) 0.0081(9) -0.0119(11) 0.0008(9) O3W 0.0673(15) 0.0733(16) 0.0533(14) -0.0229(12) -0.0057(13) 0.0076(12) O4W 0.0692(14) 0.0687(14) 0.0709(14) -0.0020(11) 0.0176(11) 0.0107(11) C1 0.0201(8) 0.0184(8) 0.0179(8) 0.0040(6) 0.0004(6) 0.0001(6) C2 0.0240(8) 0.0180(8) 0.0218(8) 0.0018(6) 0.0012(6) 0.0028(6) C3 0.0222(8) 0.0154(7) 0.0238(8) 0.0013(6) -0.0005(6) 0.0006(6) C4 0.0334(9) 0.0165(8) 0.0283(9) -0.0005(7) 0.0074(7) -0.0017(7) C5 0.0320(10) 0.0236(9) 0.0371(11) 0.0066(8) 0.0117(8) 0.0017(7) C6 0.0472(13) 0.0476(14) 0.0409(12) 0.0061(10) 0.0197(11) -0.0005(10) C7 0.0332(11) 0.0478(14) 0.0512(14) 0.0044(11) 0.0086(10) -0.0040(9) C8 0.0239(8) 0.0168(8) 0.0218(8) 0.0034(6) 0.0027(6) 0.0003(6) C9 0.0297(9) 0.0151(8) 0.0220(8) 0.0004(6) -0.0015(7) 0.0002(6) C10 0.0406(11) 0.0229(9) 0.0267(9) -0.0004(7) 0.0076(8) 0.0040(8) C11 0.0510(13) 0.0235(10) 0.0491(13) 0.0001(8) 0.0190(10) 0.0076(8) C12 0.0685(17) 0.0580(16) 0.0268(11) 0.0025(10) 0.0103(11) 0.0098(13) C13 0.0392(12) 0.0342(11) 0.0559(14) -0.0060(10) 0.0186(10) -0.0032(9) C14 0.0331(10) 0.0184(9) 0.0230(8) -0.0030(7) -0.0060(7) 0.0000(7) C15 0.0384(11) 0.0298(10) 0.0371(11) 0.0037(8) -0.0091(9) -0.0115(8) C16 0.0300(10) 0.0271(9) 0.0238(9) -0.0041(7) -0.0012(7) 0.0056(7) C17 0.0286(9) 0.0454(11) 0.0286(8) -0.0085(10) 0.0058(7) 0.0090(10) C18 0.0271(10) 0.0514(13) 0.0291(10) -0.0014(9) 0.0094(8) -0.0010(9) C19 0.0261(9) 0.0329(10) 0.0263(9) 0.0018(8) 0.0037(7) -0.0032(7) C20 0.0208(8) 0.0237(8) 0.0217(8) 0.0008(6) 0.0006(6) 0.0008(6) C21 0.0217(8) 0.0165(8) 0.0254(8) 0.0007(6) 0.0025(6) -0.0030(6) C22 0.0318(10) 0.0214(9) 0.0263(9) -0.0018(7) -0.0030(8) -0.0001(7) C23 0.0349(10) 0.0320(10) 0.0256(9) -0.0069(8) -0.0028(8) -0.0002(8) C24 0.0310(9) 0.0405(13) 0.0210(8) -0.0030(8) -0.0050(7) 0.0030(8) C25 0.0258(9) 0.0320(10) 0.0213(8) 0.0053(7) 0.0011(7) 0.0072(7) C26 0.0174(8) 0.0230(8) 0.0205(8) 0.0011(7) 0.0014(6) 0.0012(6) C27 0.0289(9) 0.0204(9) 0.0238(9) 0.0031(7) -0.0044(7) 0.0031(7) C28 0.0300(10) 0.0223(9) 0.0249(9) 0.0035(7) -0.0038(7) -0.0048(7) C29 0.0244(9) 0.0367(11) 0.0315(10) 0.0084(8) -0.0017(8) -0.0113(8) C30 0.0216(8) 0.0436(14) 0.0288(9) 0.0056(8) 0.0038(7) -0.0018(8) C31 0.0236(9) 0.0323(10) 0.0291(9) -0.0013(8) 0.0030(7) 0.0009(7) C32 0.0219(8) 0.0240(9) 0.0203(8) -0.0012(7) 0.0004(7) 0.0000(7) C33 0.0220(8) 0.0183(8) 0.0248(8) -0.0027(6) 0.0047(7) 0.0008(6) N1 0.0208(7) 0.0164(7) 0.0203(7) 0.0039(5) 0.0000(5) 0.0000(5) N2 0.0292(8) 0.0163(7) 0.0234(7) 0.0015(6) -0.0047(6) 0.0022(6) N3 0.0294(8) 0.0222(7) 0.0251(8) 0.0020(6) -0.0073(6) -0.0045(6) N4 0.0206(7) 0.0213(7) 0.0178(6) 0.0009(5) -0.0002(5) 0.0019(5) N5 0.0220(6) 0.0166(8) 0.0199(6) 0.0013(5) -0.0005(5) 0.0007(5) N6 0.0198(6) 0.0222(6) 0.0194(6) 0.0017(7) -0.0008(5) -0.0015(7) N7 0.0188(6) 0.0148(7) 0.0216(7) 0.0009(5) 0.0004(5) 0.0007(6) O1 0.0231(6) 0.0163(7) 0.0171(5) 0.0000(4) -0.0019(4) 0.0010(4) O2 0.0286(6) 0.0159(6) 0.0188(6) 0.0003(5) -0.0040(5) 0.0006(5) O3 0.0381(8) 0.0258(7) 0.0265(8) 0.0018(6) 0.0074(7) 0.0087(6) O4 0.0358(7) 0.0203(6) 0.0247(6) 0.0014(5) -0.0060(5) 0.0028(5) O5 0.0451(9) 0.0228(7) 0.0401(8) 0.0034(6) -0.0218(7) -0.0020(6) Co1 0.01936(10) 0.01349(10) 0.01656(10) 0.00061(8) -0.00125(7) 0.00015(8) O6 0.125(2) 0.0898(19) 0.0617(15) 0.0300(14) -0.0209(15) -0.0306(18) O7 0.134(2) 0.0398(12) 0.129(2) 0.0002(13) 0.077(2) 0.0042(14) O8 0.167(3) 0.0538(14) 0.0644(14) -0.0005(11) -0.0100(16) 0.0435(16) O9 0.0869(19) 0.102(2) 0.143(3) -0.081(2) 0.0448(19) -0.0299(16) Cl1 0.0688(4) 0.0300(3) 0.0556(4) -0.0045(2) -0.0014(3) 0.0022(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.284(2) . ? C1 O2 1.331(2) . ? C1 C2 1.511(2) . ? C2 O3 1.426(2) . ? C2 C3 1.538(2) . ? C3 C8 1.528(2) . ? C3 C4 1.538(3) . ? C4 C5 1.535(3) . ? C5 C7 1.525(3) . ? C5 C6 1.536(3) . ? C8 O4 1.225(2) . ? C8 N2 1.346(2) . ? C9 N2 1.458(2) . ? C9 C14 1.532(3) . ? C9 C10 1.560(3) . ? C10 C13 1.533(3) . ? C10 C12 1.535(3) . ? C10 C11 1.536(3) . ? C14 O5 1.245(2) . ? C14 N3 1.325(2) . ? C15 N3 1.459(2) . ? C16 N4 1.337(2) . ? C16 C17 1.386(3) . ? C17 C18 1.383(4) . ? C18 C19 1.392(3) . ? C19 C20 1.376(3) . ? C20 N4 1.365(2) . ? C20 C21 1.502(2) . ? C21 N7 1.502(2) . ? C22 N5 1.345(2) . ? C22 C23 1.386(3) . ? C23 C24 1.379(3) . ? C24 C25 1.382(3) . ? C25 C26 1.387(3) . ? C26 N5 1.342(2) . ? C26 C27 1.502(3) . ? C27 N7 1.503(2) . ? C28 N6 1.348(2) . ? C28 C29 1.387(3) . ? C29 C30 1.380(3) . ? C30 C31 1.383(3) . ? C31 C32 1.379(3) . ? C32 N6 1.350(3) . ? C32 C33 1.506(2) . ? C33 N7 1.497(2) . ? N1 O1 1.4128(18) . ? N4 Co1 1.9304(15) . ? N5 Co1 1.9332(14) . ? N6 Co1 1.9273(13) . ? N7 Co1 1.9444(15) . ? O1 Co1 1.8693(12) . ? O2 Co1 1.8693(13) . ? O6 Cl1 1.439(3) . ? O7 Cl1 1.424(3) . ? O8 Cl1 1.406(2) . ? O9 Cl1 1.415(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 N1 C1 O2 123.49(15) . . ? N1 C1 C2 119.82(15) . . ? O2 C1 C2 116.69(14) . . ? O3 C2 C1 110.16(14) . . ? O3 C2 C3 111.56(14) . . ? C1 C2 C3 111.20(14) . . ? C8 C3 C4 109.53(14) . . ? C8 C3 C2 107.72(14) . . ? C4 C3 C2 110.49(14) . . ? C5 C4 C3 115.51(15) . . ? C7 C5 C4 112.06(18) . . ? C7 C5 C6 110.78(19) . . ? C4 C5 C6 109.57(17) . . ? O4 C8 N2 123.98(16) . . ? O4 C8 C3 120.97(16) . . ? N2 C8 C3 115.05(15) . . ? N2 C9 C14 107.20(15) . . ? N2 C9 C10 112.60(15) . . ? C14 C9 C10 112.44(15) . . ? C13 C10 C12 109.8(2) . . ? C13 C10 C11 107.98(19) . . ? C12 C10 C11 109.42(19) . . ? C13 C10 C9 108.34(16) . . ? C12 C10 C9 111.33(18) . . ? C11 C10 C9 109.89(16) . . ? O5 C14 N3 122.07(18) . . ? O5 C14 C9 121.95(17) . . ? N3 C14 C9 115.97(16) . . ? N4 C16 C17 121.81(19) . . ? C18 C17 C16 118.72(19) . . ? C17 C18 C19 119.84(19) . . ? C20 C19 C18 118.58(19) . . ? N4 C20 C19 121.53(17) . . ? N4 C20 C21 113.67(15) . . ? C19 C20 C21 124.79(17) . . ? C20 C21 N7 106.83(14) . . ? N5 C22 C23 121.09(18) . . ? C24 C23 C22 118.99(18) . . ? C23 C24 C25 119.66(17) . . ? C24 C25 C26 119.03(18) . . ? N5 C26 C25 120.96(17) . . ? N5 C26 C27 116.31(15) . . ? C25 C26 C27 122.73(17) . . ? C26 C27 N7 112.26(14) . . ? N6 C28 C29 120.64(19) . . ? C30 C29 C28 119.80(18) . . ? C29 C30 C31 119.00(17) . . ? C32 C31 C30 119.26(19) . . ? N6 C32 C31 121.46(17) . . ? N6 C32 C33 113.97(15) . . ? C31 C32 C33 124.57(17) . . ? N7 C33 C32 107.53(14) . . ? C1 N1 O1 112.59(13) . . ? C8 N2 C9 123.89(15) . . ? C14 N3 C15 122.06(17) . . ? C16 N4 C20 119.49(16) . . ? C16 N4 Co1 127.26(13) . . ? C20 N4 Co1 112.77(12) . . ? C26 N5 C22 120.26(15) . . ? C26 N5 Co1 114.23(12) . . ? C22 N5 Co1 125.41(13) . . ? C28 N6 C32 119.83(15) . . ? C28 N6 Co1 126.37(14) . . ? C32 N6 Co1 113.64(13) . . ? C33 N7 C21 111.61(14) . . ? C33 N7 C27 112.13(14) . . ? C21 N7 C27 111.25(13) . . ? C33 N7 Co1 106.24(10) . . ? C21 N7 Co1 105.33(10) . . ? C27 N7 Co1 109.92(11) . . ? N1 O1 Co1 109.44(9) . . ? C1 O2 Co1 107.27(10) . . ? O1 Co1 O2 86.77(5) . . ? O1 Co1 N6 90.82(5) . . ? O2 Co1 N6 95.33(7) . . ? O1 Co1 N4 90.57(6) . . ? O2 Co1 N4 95.39(6) . . ? N6 Co1 N4 169.25(7) . . ? O1 Co1 N5 178.68(6) . . ? O2 Co1 N5 94.00(6) . . ? N6 Co1 N5 90.17(6) . . ? N4 Co1 N5 88.29(6) . . ? O1 Co1 N7 92.04(6) . . ? O2 Co1 N7 178.80(7) . . ? N6 Co1 N7 84.52(7) . . ? N4 Co1 N7 84.78(6) . . ? N5 Co1 N7 87.19(6) . . ? O8 Cl1 O9 115.1(2) . . ? O8 Cl1 O7 109.09(18) . . ? O9 Cl1 O7 109.66(16) . . ? O8 Cl1 O6 105.57(17) . . ? O9 Cl1 O6 107.8(2) . . ? O7 Cl1 O6 109.5(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 O3 130.31(17) . . . . ? O2 C1 C2 O3 -50.1(2) . . . . ? N1 C1 C2 C3 -105.47(18) . . . . ? O2 C1 C2 C3 74.16(19) . . . . ? O3 C2 C3 C8 -53.49(18) . . . . ? C1 C2 C3 C8 -176.91(14) . . . . ? O3 C2 C3 C4 -173.10(15) . . . . ? C1 C2 C3 C4 63.47(18) . . . . ? C8 C3 C4 C5 57.0(2) . . . . ? C2 C3 C4 C5 175.52(15) . . . . ? C3 C4 C5 C7 64.5(2) . . . . ? C3 C4 C5 C6 -172.09(17) . . . . ? C4 C3 C8 O4 49.1(2) . . . . ? C2 C3 C8 O4 -71.1(2) . . . . ? C4 C3 C8 N2 -131.48(17) . . . . ? C2 C3 C8 N2 108.30(17) . . . . ? N2 C9 C10 C13 -59.7(2) . . . . ? C14 C9 C10 C13 179.04(17) . . . . ? N2 C9 C10 C12 61.1(2) . . . . ? C14 C9 C10 C12 -60.1(2) . . . . ? N2 C9 C10 C11 -177.49(17) . . . . ? C14 C9 C10 C11 61.3(2) . . . . ? N2 C9 C14 O5 -33.7(2) . . . . ? C10 C9 C14 O5 90.5(2) . . . . ? N2 C9 C14 N3 146.20(16) . . . . ? C10 C9 C14 N3 -89.5(2) . . . . ? N4 C16 C17 C18 1.1(3) . . . . ? C16 C17 C18 C19 -1.8(3) . . . . ? C17 C18 C19 C20 0.7(3) . . . . ? C18 C19 C20 N4 1.0(3) . . . . ? C18 C19 C20 C21 179.98(18) . . . . ? N4 C20 C21 N7 34.05(19) . . . . ? C19 C20 C21 N7 -144.99(18) . . . . ? N5 C22 C23 C24 -0.4(3) . . . . ? C22 C23 C24 C25 -0.6(3) . . . . ? C23 C24 C25 C26 1.0(3) . . . . ? C24 C25 C26 N5 -0.4(3) . . . . ? C24 C25 C26 C27 179.06(18) . . . . ? N5 C26 C27 N7 -2.9(2) . . . . ? C25 C26 C27 N7 177.70(16) . . . . ? N6 C28 C29 C30 0.2(3) . . . . ? C28 C29 C30 C31 0.0(3) . . . . ? C29 C30 C31 C32 0.1(3) . . . . ? C30 C31 C32 N6 -0.4(3) . . . . ? C30 C31 C32 C33 179.40(17) . . . . ? N6 C32 C33 N7 -29.8(2) . . . . ? C31 C32 C33 N7 150.38(18) . . . . ? O2 C1 N1 O1 -0.4(2) . . . . ? C2 C1 N1 O1 179.17(14) . . . . ? O4 C8 N2 C9 -2.3(3) . . . . ? C3 C8 N2 C9 178.25(16) . . . . ? C14 C9 N2 C8 -135.25(18) . . . . ? C10 C9 N2 C8 100.6(2) . . . . ? O5 C14 N3 C15 -2.6(3) . . . . ? C9 C14 N3 C15 177.46(19) . . . . ? C17 C16 N4 C20 0.6(3) . . . . ? C17 C16 N4 Co1 -170.89(14) . . . . ? C19 C20 N4 C16 -1.7(3) . . . . ? C21 C20 N4 C16 179.24(15) . . . . ? C19 C20 N4 Co1 170.97(14) . . . . ? C21 C20 N4 Co1 -8.11(19) . . . . ? C25 C26 N5 C22 -0.7(3) . . . . ? C27 C26 N5 C22 179.87(17) . . . . ? C25 C26 N5 Co1 -177.16(13) . . . . ? C27 C26 N5 Co1 3.38(19) . . . . ? C23 C22 N5 C26 1.1(3) . . . . ? C23 C22 N5 Co1 177.13(15) . . . . ? C29 C28 N6 C32 -0.4(3) . . . . ? C29 C28 N6 Co1 174.61(13) . . . . ? C31 C32 N6 C28 0.5(3) . . . . ? C33 C32 N6 C28 -179.26(15) . . . . ? C31 C32 N6 Co1 -175.12(14) . . . . ? C33 C32 N6 Co1 5.09(18) . . . . ? C32 C33 N7 C21 153.70(14) . . . . ? C32 C33 N7 C27 -80.71(17) . . . . ? C32 C33 N7 Co1 39.39(16) . . . . ? C20 C21 N7 C33 -157.55(14) . . . . ? C20 C21 N7 C27 76.37(17) . . . . ? C20 C21 N7 Co1 -42.68(15) . . . . ? C26 C27 N7 C33 118.89(16) . . . . ? C26 C27 N7 C21 -115.32(16) . . . . ? C26 C27 N7 Co1 0.95(18) . . . . ? C1 N1 O1 Co1 4.94(16) . . . . ? N1 C1 O2 Co1 -4.3(2) . . . . ? C2 C1 O2 Co1 176.13(12) . . . . ? N1 O1 Co1 O2 -5.81(10) . . . . ? N1 O1 Co1 N6 -101.10(10) . . . . ? N1 O1 Co1 N4 89.56(10) . . . . ? N1 O1 Co1 N5 120(3) . . . . ? N1 O1 Co1 N7 174.36(10) . . . . ? C1 O2 Co1 O1 5.42(11) . . . . ? C1 O2 Co1 N6 95.94(11) . . . . ? C1 O2 Co1 N4 -84.85(11) . . . . ? C1 O2 Co1 N5 -173.51(11) . . . . ? C1 O2 Co1 N7 13(3) . . . . ? C28 N6 Co1 O1 107.80(14) . . . . ? C32 N6 Co1 O1 -76.87(12) . . . . ? C28 N6 Co1 O2 20.97(14) . . . . ? C32 N6 Co1 O2 -163.71(12) . . . . ? C28 N6 Co1 N4 -154.8(3) . . . . ? C32 N6 Co1 N4 20.5(4) . . . . ? C28 N6 Co1 N5 -73.06(14) . . . . ? C32 N6 Co1 N5 102.26(12) . . . . ? C28 N6 Co1 N7 -160.22(14) . . . . ? C32 N6 Co1 N7 15.10(12) . . . . ? C16 N4 Co1 O1 -110.38(15) . . . . ? C20 N4 Co1 O1 77.66(12) . . . . ? C16 N4 Co1 O2 -23.57(16) . . . . ? C20 N4 Co1 O2 164.47(12) . . . . ? C16 N4 Co1 N6 152.2(3) . . . . ? C20 N4 Co1 N6 -19.8(4) . . . . ? C16 N4 Co1 N5 70.28(15) . . . . ? C20 N4 Co1 N5 -101.67(13) . . . . ? C16 N4 Co1 N7 157.62(16) . . . . ? C20 N4 Co1 N7 -14.34(12) . . . . ? C26 N5 Co1 O1 52(3) . . . . ? C22 N5 Co1 O1 -124(3) . . . . ? C26 N5 Co1 O2 177.88(12) . . . . ? C22 N5 Co1 O2 1.60(16) . . . . ? C26 N5 Co1 N6 -86.76(13) . . . . ? C22 N5 Co1 N6 96.96(16) . . . . ? C26 N5 Co1 N4 82.59(12) . . . . ? C22 N5 Co1 N4 -93.68(16) . . . . ? C26 N5 Co1 N7 -2.26(12) . . . . ? C22 N5 Co1 N7 -178.54(16) . . . . ? C33 N7 Co1 O1 60.14(11) . . . . ? C21 N7 Co1 O1 -58.39(11) . . . . ? C27 N7 Co1 O1 -178.33(11) . . . . ? C33 N7 Co1 O2 52(3) . . . . ? C21 N7 Co1 O2 -66(3) . . . . ? C27 N7 Co1 O2 174(3) . . . . ? C33 N7 Co1 N6 -30.48(11) . . . . ? C21 N7 Co1 N6 -149.02(11) . . . . ? C27 N7 Co1 N6 91.04(11) . . . . ? C33 N7 Co1 N4 150.53(11) . . . . ? C21 N7 Co1 N4 31.99(11) . . . . ? C27 N7 Co1 N4 -87.95(12) . . . . ? C33 N7 Co1 N5 -120.93(12) . . . . ? C21 N7 Co1 N5 120.54(11) . . . . ? C27 N7 Co1 N5 0.60(11) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.798 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.052 # Attachment '1c.cif' data_twf33 _database_code_depnum_ccdc_archive 'CCDC 282772' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(aha)tpa][Co(aha-H)tpa](ClO4)3' _chemical_formula_sum 'C40 H47 Cl3 Co2 N10 O18' _chemical_formula_weight 1180.09 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)/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 16.339(9) _cell_length_b 18.173(10) _cell_length_c 16.754(9) _cell_angle_alpha 90.00 _cell_angle_beta 102.061(10) _cell_angle_gamma 90.00 _cell_volume 4865(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour grey/green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27305 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0859 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 28.35 _reflns_number_total 11238 _reflns_number_gt 6540 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.0701P)^2^+14.4387P] 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 11238 _refine_ls_number_parameters 674 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1278 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1393 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 C1 C 0.4243(3) 0.3584(3) 0.7740(3) 0.0248(10) Uani 1 1 d . . . H1 H 0.4388 0.4022 0.8023 0.030 Uiso 1 1 calc R . . C2 C 0.3886(3) 0.3609(3) 0.6919(3) 0.0318(12) Uani 1 1 d . . . H2 H 0.3783 0.4058 0.6652 0.038 Uiso 1 1 calc R . . C3 C 0.3681(3) 0.2957(3) 0.6498(3) 0.0353(13) Uani 1 1 d . . . H3 H 0.3455 0.2964 0.5940 0.042 Uiso 1 1 calc R . . C4 C 0.3815(4) 0.2299(3) 0.6911(3) 0.0404(14) Uani 1 1 d . . . H4 H 0.3671 0.1857 0.6637 0.048 Uiso 1 1 calc R . . C5 C 0.4165(3) 0.2303(3) 0.7733(3) 0.0307(11) Uani 1 1 d . . . C6 C 0.4278(4) 0.1636(3) 0.8277(3) 0.0367(13) Uani 1 1 d . . . H6A H 0.3769 0.1543 0.8473 0.044 Uiso 1 1 calc R . . H6B H 0.4392 0.1208 0.7972 0.044 Uiso 1 1 calc R . . C7 C 0.6454(3) 0.3546(3) 0.9155(3) 0.0284(11) Uani 1 1 d . . . H7 H 0.6206 0.3975 0.9293 0.034 Uiso 1 1 calc R . . C8 C 0.7259(3) 0.3569(3) 0.9047(3) 0.0347(12) Uani 1 1 d . . . H8 H 0.7554 0.4011 0.9101 0.042 Uiso 1 1 calc R . . C9 C 0.7634(3) 0.2921(4) 0.8856(3) 0.0409(14) Uani 1 1 d . . . H9 H 0.8182 0.2924 0.8783 0.049 Uiso 1 1 calc R . . C10 C 0.7180(3) 0.2275(3) 0.8777(3) 0.0369(13) Uani 1 1 d . . . H10 H 0.7423 0.1837 0.8657 0.044 Uiso 1 1 calc R . . C11 C 0.6370(3) 0.2285(3) 0.8877(3) 0.0249(10) Uani 1 1 d . . . C12 C 0.5809(4) 0.1621(3) 0.8769(3) 0.0364(13) Uani 1 1 d . . . H12A H 0.5716 0.1461 0.8205 0.044 Uiso 1 1 calc R . . H12B H 0.6087 0.1224 0.9107 0.044 Uiso 1 1 calc R . . C13 C 0.5757(3) 0.2913(3) 1.0985(3) 0.0264(11) Uani 1 1 d . . . H13 H 0.5778 0.3419 1.0909 0.032 Uiso 1 1 calc R . . C14 C 0.6106(3) 0.2613(3) 1.1744(3) 0.0321(12) Uani 1 1 d . . . H14 H 0.6355 0.2914 1.2175 0.039 Uiso 1 1 calc R . . C15 C 0.6077(3) 0.1867(3) 1.1846(3) 0.0363(13) Uani 1 1 d . . . H15 H 0.6311 0.1657 1.2348 0.044 Uiso 1 1 calc R . . C16 C 0.5700(3) 0.1426(3) 1.1204(3) 0.0318(12) Uani 1 1 d . . . H16 H 0.5680 0.0918 1.1267 0.038 Uiso 1 1 calc R . . C17 C 0.5354(3) 0.1749(3) 1.0465(3) 0.0254(10) Uani 1 1 d . . . C18 C 0.4892(3) 0.1343(3) 0.9730(3) 0.0297(11) Uani 1 1 d . . . H18A H 0.4304 0.1303 0.9749 0.036 Uiso 1 1 calc R . . H18B H 0.5118 0.0851 0.9717 0.036 Uiso 1 1 calc R . . C19 C 0.4146(3) 0.3844(3) 0.9892(3) 0.0235(10) Uani 1 1 d . . . C20 C 0.4018(3) 0.4564(3) 1.0279(3) 0.0340(12) Uani 1 1 d . . . H20A H 0.3849 0.4929 0.9862 0.051 Uiso 1 1 calc R . . H20B H 0.4532 0.4715 1.0632 0.051 Uiso 1 1 calc R . . H20C H 0.3592 0.4512 1.0592 0.051 Uiso 1 1 calc R . . C21 C 0.1403(3) 0.3310(3) 0.2063(3) 0.0251(10) Uani 1 1 d . . . H21 H 0.1204 0.3733 0.1775 0.030 Uiso 1 1 calc R . . C22 C 0.1805(3) 0.3371(3) 0.2868(3) 0.0320(12) Uani 1 1 d . . . H22 H 0.1877 0.3829 0.3120 0.038 Uiso 1 1 calc R . . C23 C 0.2100(3) 0.2743(3) 0.3297(3) 0.0344(12) Uani 1 1 d . . . H23 H 0.2374 0.2774 0.3841 0.041 Uiso 1 1 calc R . . C24 C 0.1982(3) 0.2066(3) 0.2909(3) 0.0344(12) Uani 1 1 d . . . H24 H 0.2174 0.1637 0.3191 0.041 Uiso 1 1 calc R . . C25 C 0.1576(3) 0.2034(3) 0.2095(3) 0.0275(11) Uani 1 1 d . . . C26 C 0.1480(3) 0.1349(3) 0.1587(3) 0.0329(12) Uani 1 1 d . . . H26A H 0.2003 0.1239 0.1425 0.039 Uiso 1 1 calc R . . H26B H 0.1342 0.0938 0.1904 0.039 Uiso 1 1 calc R . . C27 C -0.0768(3) 0.3144(3) 0.0769(3) 0.0300(11) Uani 1 1 d . . . H27 H -0.0550 0.3593 0.0645 0.036 Uiso 1 1 calc R . . C28 C -0.1552(3) 0.3122(3) 0.0937(3) 0.0378(13) Uani 1 1 d . . . H28 H -0.1862 0.3551 0.0936 0.045 Uiso 1 1 calc R . . C29 C -0.1879(3) 0.2450(4) 0.1107(3) 0.0436(15) Uani 1 1 d . . . H29 H -0.2416 0.2426 0.1209 0.052 Uiso 1 1 calc R . . C30 C -0.1406(3) 0.1816(3) 0.1127(3) 0.0362(13) Uani 1 1 d . . . H30 H -0.1618 0.1362 0.1241 0.043 Uiso 1 1 calc R . . C31 C -0.0611(3) 0.1877(3) 0.0971(3) 0.0249(10) Uani 1 1 d . . . C32 C -0.0039(3) 0.1231(3) 0.0982(3) 0.0308(11) Uani 1 1 d . . . H32A H 0.0029 0.0983 0.1505 0.037 Uiso 1 1 calc R . . H32B H -0.0292 0.0885 0.0561 0.037 Uiso 1 1 calc R . . C33 C -0.0076(3) 0.2530(3) -0.1165(3) 0.0260(10) Uani 1 1 d . . . H33 H -0.0159 0.3031 -0.1101 0.031 Uiso 1 1 calc R . . C34 C -0.0387(3) 0.2202(3) -0.1914(3) 0.0354(12) Uani 1 1 d . . . H34 H -0.0676 0.2480 -0.2349 0.042 Uiso 1 1 calc R . . C35 C -0.0263(4) 0.1462(3) -0.2008(3) 0.0403(14) Uani 1 1 d . . . H35 H -0.0476 0.1234 -0.2504 0.048 Uiso 1 1 calc R . . C36 C 0.0180(4) 0.1060(3) -0.1362(3) 0.0370(13) Uani 1 1 d . . . H36 H 0.0279 0.0561 -0.1422 0.044 Uiso 1 1 calc R . . C37 C 0.0474(3) 0.1407(3) -0.0624(3) 0.0266(11) Uani 1 1 d . . . C38 C 0.0979(3) 0.1054(3) 0.0121(3) 0.0298(11) Uani 1 1 d . . . H38A H 0.1571 0.1083 0.0115 0.036 Uiso 1 1 calc R . . H38B H 0.0827 0.0539 0.0143 0.036 Uiso 1 1 calc R . . C39 C 0.1470(3) 0.3660(3) 0.0066(3) 0.0235(10) Uani 1 1 d . . . C40 C 0.1601(3) 0.4428(3) -0.0194(3) 0.0353(12) Uani 1 1 d . . . H40A H 0.2130 0.4462 -0.0356 0.053 Uiso 1 1 calc R . . H40B H 0.1596 0.4759 0.0252 0.053 Uiso 1 1 calc R . . H40C H 0.1160 0.4559 -0.0647 0.053 Uiso 1 1 calc R . . N1 N 0.4387(2) 0.2943(2) 0.8140(2) 0.0231(8) Uani 1 1 d . . . N2 N 0.6009(2) 0.2914(2) 0.9066(2) 0.0213(8) Uani 1 1 d . . . N3 N 0.5392(2) 0.2485(2) 1.0366(2) 0.0209(8) Uani 1 1 d . . . N4 N 0.4990(3) 0.1765(2) 0.8983(2) 0.0269(9) Uani 1 1 d . . . N5 N 0.3625(2) 0.3314(2) 0.9879(2) 0.0239(9) Uani 1 1 d . . . N6 N 0.1289(2) 0.2656(2) 0.1681(2) 0.0222(8) Uani 1 1 d . . . N7 N -0.0306(2) 0.2529(2) 0.0781(2) 0.0225(8) Uani 1 1 d . . . N8 N 0.0340(2) 0.2137(2) -0.0534(2) 0.0226(8) Uani 1 1 d . . . N9 N 0.0801(2) 0.1455(2) 0.0845(2) 0.0235(8) Uani 1 1 d . . . N10 N 0.2044(3) 0.3168(2) 0.0117(2) 0.0244(9) Uani 1 1 d . . . O1 O 0.3851(2) 0.26659(17) 0.95054(19) 0.0242(7) Uani 1 1 d . . . O2 O 0.48211(19) 0.37793(16) 0.95822(19) 0.0217(7) Uani 1 1 d . . . O1W O -0.1454(3) 0.0673(3) -0.0723(3) 0.0623(13) Uani 1 1 d . . . O3 O 0.18633(19) 0.24554(17) 0.0334(2) 0.0235(7) Uani 1 1 d . . . O2W O 0.7069(5) 0.4964(5) 0.7723(5) 0.151(3) Uani 1 1 d . . . O4 O 0.07639(19) 0.34813(16) 0.02420(19) 0.0219(7) Uani 1 1 d . . . Co1 Co 0.49020(4) 0.28000(3) 0.92718(4) 0.01920(16) Uani 1 1 d . . . Co2 Co 0.07877(4) 0.24870(3) 0.05539(4) 0.01877(15) Uani 1 1 d . . . H10N H 0.254(5) 0.324(4) 0.006(4) 0.07(2) Uiso 1 1 d . . . O5 O 0.3689(5) 0.5529(3) 0.7745(5) 0.132(3) Uani 1 1 d . . . O6 O 0.2955(3) 0.5677(3) 0.8748(3) 0.0692(14) Uani 1 1 d . . . O7 O 0.2704(3) 0.4675(3) 0.7897(4) 0.0742(16) Uani 1 1 d . . . O8 O 0.2299(5) 0.5876(4) 0.7451(4) 0.142(3) Uani 1 1 d . . . O9 O -0.0042(3) 0.5936(3) 0.2060(3) 0.0703(15) Uani 1 1 d . . . O10 O 0.0147(3) 0.4789(2) 0.1532(3) 0.0721(15) Uani 1 1 d . . . O11 O 0.1029(4) 0.5745(3) 0.1391(4) 0.103(2) Uani 1 1 d . . . O12 O 0.1081(4) 0.5197(3) 0.2679(4) 0.0858(18) Uani 1 1 d . . . O13 O 0.2680(9) 0.5470(6) 0.4736(7) 0.130(5) Uani 0.67 1 d P . . O13A O 0.2125(7) 0.4961(8) 0.4239(9) 0.053(4) Uani 0.33 1 d P . . O14 O 0.3462(3) 0.4830(3) 0.3986(3) 0.0715(15) Uani 1 1 d . . . O15 O 0.2857(4) 0.4116(3) 0.4848(4) 0.103(2) Uani 1 1 d . . . O16 O 0.3761(7) 0.4970(4) 0.5347(4) 0.160(4) Uani 1 1 d . . . Cl1 Cl 0.28965(10) 0.54226(8) 0.79297(10) 0.0452(4) Uani 1 1 d . . . Cl2 Cl 0.05795(11) 0.54168(8) 0.19095(10) 0.0481(4) Uani 1 1 d . . . Cl3 Cl 0.30632(11) 0.48354(8) 0.46671(10) 0.0518(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.023(2) 0.030(3) 0.022(2) 0.002(2) 0.0070(19) 0.001(2) C2 0.025(3) 0.045(3) 0.025(3) 0.010(2) 0.005(2) 0.002(2) C3 0.029(3) 0.058(4) 0.018(2) -0.002(2) 0.004(2) 0.000(3) C4 0.041(3) 0.046(3) 0.030(3) -0.012(3) -0.003(2) -0.003(3) C5 0.033(3) 0.030(3) 0.027(3) -0.004(2) 0.001(2) -0.001(2) C6 0.056(4) 0.025(3) 0.026(3) -0.005(2) 0.001(2) -0.008(2) C7 0.023(3) 0.035(3) 0.027(3) -0.007(2) 0.006(2) -0.003(2) C8 0.026(3) 0.047(3) 0.032(3) -0.010(2) 0.008(2) -0.007(2) C9 0.017(3) 0.070(4) 0.034(3) -0.006(3) 0.003(2) 0.004(3) C10 0.032(3) 0.050(3) 0.028(3) -0.004(2) 0.006(2) 0.017(3) C11 0.030(3) 0.029(3) 0.016(2) -0.0005(19) 0.0066(19) 0.006(2) C12 0.051(3) 0.024(3) 0.040(3) -0.002(2) 0.022(3) 0.005(2) C13 0.022(2) 0.036(3) 0.023(2) -0.003(2) 0.0077(19) 0.001(2) C14 0.029(3) 0.048(3) 0.020(2) 0.000(2) 0.007(2) -0.002(2) C15 0.034(3) 0.051(4) 0.026(3) 0.010(3) 0.010(2) 0.007(3) C16 0.034(3) 0.032(3) 0.033(3) 0.010(2) 0.015(2) 0.008(2) C17 0.023(2) 0.028(3) 0.028(3) 0.003(2) 0.011(2) 0.002(2) C18 0.040(3) 0.018(2) 0.034(3) 0.005(2) 0.012(2) 0.001(2) C19 0.024(2) 0.025(2) 0.022(2) -0.0018(19) 0.0049(19) 0.000(2) C20 0.036(3) 0.025(3) 0.046(3) -0.008(2) 0.019(3) 0.001(2) C21 0.025(2) 0.027(3) 0.024(2) 0.001(2) 0.0053(19) 0.004(2) C22 0.032(3) 0.035(3) 0.030(3) -0.003(2) 0.006(2) -0.002(2) C23 0.029(3) 0.045(3) 0.025(3) 0.001(2) -0.002(2) 0.002(2) C24 0.035(3) 0.038(3) 0.030(3) 0.009(2) 0.004(2) 0.005(2) C25 0.025(3) 0.028(3) 0.029(3) 0.004(2) 0.005(2) 0.005(2) C26 0.037(3) 0.025(3) 0.032(3) 0.006(2) -0.002(2) 0.006(2) C27 0.028(3) 0.035(3) 0.027(3) -0.003(2) 0.007(2) 0.008(2) C28 0.028(3) 0.056(4) 0.032(3) 0.001(3) 0.011(2) 0.014(3) C29 0.020(3) 0.080(5) 0.034(3) -0.002(3) 0.012(2) 0.001(3) C30 0.027(3) 0.052(4) 0.031(3) -0.003(3) 0.009(2) -0.009(3) C31 0.028(3) 0.030(3) 0.018(2) -0.002(2) 0.0076(19) -0.007(2) C32 0.032(3) 0.030(3) 0.035(3) 0.002(2) 0.018(2) -0.006(2) C33 0.025(2) 0.030(3) 0.023(2) -0.001(2) 0.0052(19) 0.003(2) C34 0.037(3) 0.046(3) 0.024(3) 0.000(2) 0.007(2) 0.000(3) C35 0.054(4) 0.044(3) 0.024(3) -0.012(2) 0.014(3) -0.017(3) C36 0.048(3) 0.036(3) 0.030(3) -0.009(2) 0.015(3) -0.012(3) C37 0.030(3) 0.025(2) 0.028(3) -0.004(2) 0.014(2) -0.004(2) C38 0.039(3) 0.018(2) 0.035(3) -0.002(2) 0.014(2) 0.007(2) C39 0.025(2) 0.024(2) 0.021(2) 0.0013(19) 0.0046(19) 0.001(2) C40 0.036(3) 0.028(3) 0.043(3) 0.007(2) 0.010(2) 0.000(2) N1 0.021(2) 0.026(2) 0.023(2) -0.0044(16) 0.0054(16) 0.0000(16) N2 0.025(2) 0.024(2) 0.0150(18) -0.0012(15) 0.0042(15) 0.0060(16) N3 0.0212(19) 0.024(2) 0.0192(19) -0.0003(16) 0.0079(15) 0.0007(16) N4 0.039(2) 0.017(2) 0.025(2) -0.0048(16) 0.0074(18) 0.0007(17) N5 0.023(2) 0.019(2) 0.031(2) -0.0020(17) 0.0094(17) -0.0003(16) N6 0.0194(19) 0.023(2) 0.024(2) 0.0014(16) 0.0039(15) 0.0030(15) N7 0.0201(19) 0.030(2) 0.0166(19) -0.0011(16) 0.0019(15) 0.0027(17) N8 0.020(2) 0.026(2) 0.023(2) 0.0013(17) 0.0093(16) 0.0000(16) N9 0.026(2) 0.023(2) 0.023(2) 0.0015(16) 0.0081(16) 0.0001(16) N10 0.022(2) 0.026(2) 0.026(2) 0.0035(17) 0.0069(17) -0.0018(18) O1 0.0246(17) 0.0217(17) 0.0264(18) -0.0037(13) 0.0054(14) -0.0042(13) O2 0.0223(17) 0.0185(16) 0.0253(17) -0.0015(13) 0.0075(13) -0.0016(13) O1W 0.049(3) 0.063(3) 0.074(3) 0.027(3) 0.011(2) 0.001(2) O3 0.0226(17) 0.0175(16) 0.0323(18) 0.0038(14) 0.0099(14) 0.0023(13) O2W 0.125(7) 0.215(10) 0.115(6) 0.063(6) 0.030(5) -0.010(6) O4 0.0219(17) 0.0179(16) 0.0268(17) 0.0021(13) 0.0072(13) 0.0013(13) Co1 0.0220(3) 0.0182(3) 0.0177(3) -0.0015(2) 0.0050(2) 0.0001(2) Co2 0.0178(3) 0.0186(3) 0.0205(3) 0.0012(2) 0.0053(2) 0.0021(2) O5 0.156(7) 0.062(4) 0.230(9) -0.019(5) 0.156(7) -0.021(4) O6 0.069(3) 0.071(3) 0.068(3) -0.024(3) 0.015(3) 0.007(3) O7 0.078(4) 0.042(3) 0.108(4) -0.020(3) 0.032(3) -0.018(2) O8 0.199(8) 0.145(7) 0.072(4) 0.037(4) 0.005(5) 0.107(6) O9 0.106(4) 0.054(3) 0.059(3) 0.003(2) 0.037(3) 0.029(3) O10 0.072(3) 0.038(3) 0.098(4) -0.006(3) 0.000(3) 0.003(2) O11 0.099(5) 0.089(4) 0.149(6) 0.012(4) 0.089(5) -0.005(4) O12 0.079(4) 0.064(3) 0.101(5) 0.010(3) -0.011(3) -0.001(3) O13 0.191(12) 0.119(9) 0.105(8) 0.053(7) 0.089(8) 0.131(9) O13A 0.021(6) 0.077(10) 0.063(9) 0.048(8) 0.015(6) 0.029(6) O14 0.090(4) 0.061(3) 0.075(4) 0.018(3) 0.044(3) 0.020(3) O15 0.075(4) 0.086(4) 0.157(6) 0.049(4) 0.046(4) -0.010(3) O16 0.284(12) 0.104(6) 0.082(5) -0.029(4) 0.018(6) -0.079(7) Cl1 0.0564(9) 0.0330(7) 0.0497(9) 0.0045(6) 0.0190(7) 0.0057(7) Cl2 0.0631(10) 0.0306(7) 0.0519(9) 0.0039(7) 0.0149(8) 0.0030(7) Cl3 0.0732(11) 0.0362(8) 0.0510(9) 0.0006(7) 0.0241(8) 0.0012(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.341(6) . ? C1 C2 1.378(6) . ? C2 C3 1.384(8) . ? C3 C4 1.377(8) . ? C4 C5 1.376(7) . ? C5 N1 1.360(6) . ? C5 C6 1.505(7) . ? C6 N4 1.495(6) . ? C7 N2 1.350(6) . ? C7 C8 1.366(7) . ? C8 C9 1.395(8) . ? C9 C10 1.379(8) . ? C10 C11 1.369(7) . ? C11 N2 1.355(6) . ? C11 C12 1.503(7) . ? C12 N4 1.479(7) . ? C13 N3 1.333(6) . ? C13 C14 1.391(7) . ? C14 C15 1.369(8) . ? C15 C16 1.380(8) . ? C16 C17 1.379(7) . ? C17 N3 1.352(6) . ? C17 C18 1.497(7) . ? C18 N4 1.504(6) . ? C19 N5 1.283(6) . ? C19 O2 1.319(5) . ? C19 C20 1.494(6) . ? C21 N6 1.344(6) . ? C21 C22 1.375(7) . ? C22 C23 1.381(7) . ? C23 C24 1.386(7) . ? C24 C25 1.388(7) . ? C25 N6 1.357(6) . ? C25 C26 1.497(7) . ? C26 N9 1.495(6) . ? C27 N7 1.347(6) . ? C27 C28 1.369(7) . ? C28 C29 1.384(8) . ? C29 C30 1.384(8) . ? C30 C31 1.382(7) . ? C31 N7 1.349(6) . ? C31 C32 1.499(7) . ? C32 N9 1.496(6) . ? C33 N8 1.339(6) . ? C33 C34 1.386(7) . ? C34 C35 1.373(8) . ? C35 C36 1.378(8) . ? C36 C37 1.382(7) . ? C37 N8 1.358(6) . ? C37 C38 1.491(7) . ? C38 N9 1.495(6) . ? C39 N10 1.286(6) . ? C39 O4 1.291(5) . ? C39 C40 1.491(7) . ? N1 Co1 1.924(4) . ? N2 Co1 1.922(4) . ? N3 Co1 1.927(4) . ? N4 Co1 1.955(4) . ? N5 O1 1.418(5) . ? N6 Co2 1.920(4) . ? N7 Co2 1.905(4) . ? N8 Co2 1.924(4) . ? N9 Co2 1.936(4) . ? N10 O3 1.393(5) . ? O1 Co1 1.855(3) . ? O2 Co1 1.867(3) . ? O3 Co2 1.870(3) . ? O4 Co2 1.879(3) . ? O5 Cl1 1.407(6) . ? O6 Cl1 1.431(5) . ? O7 Cl1 1.394(5) . ? O8 Cl1 1.396(6) . ? O9 Cl2 1.446(5) . ? O10 Cl2 1.418(5) . ? O11 Cl2 1.384(6) . ? O12 Cl2 1.433(6) . ? O13 Cl3 1.329(8) . ? O13 O13A 1.434(18) . ? O13A Cl3 1.567(11) . ? O14 Cl3 1.428(5) . ? O15 Cl3 1.399(6) . ? O16 Cl3 1.454(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.4(5) . . ? C1 C2 C3 119.3(5) . . ? C4 C3 C2 119.4(5) . . ? C5 C4 C3 119.2(5) . . ? N1 C5 C4 121.2(5) . . ? N1 C5 C6 113.5(4) . . ? C4 C5 C6 125.1(5) . . ? N4 C6 C5 109.3(4) . . ? N2 C7 C8 121.5(5) . . ? C7 C8 C9 119.0(5) . . ? C10 C9 C8 119.2(5) . . ? C11 C10 C9 119.4(5) . . ? N2 C11 C10 121.2(5) . . ? N2 C11 C12 115.0(4) . . ? C10 C11 C12 123.8(5) . . ? N4 C12 C11 112.9(4) . . ? N3 C13 C14 120.9(5) . . ? C15 C14 C13 119.0(5) . . ? C14 C15 C16 119.9(5) . . ? C17 C16 C15 119.0(5) . . ? N3 C17 C16 120.7(5) . . ? N3 C17 C18 114.5(4) . . ? C16 C17 C18 124.8(5) . . ? C17 C18 N4 108.1(4) . . ? N5 C19 O2 122.2(4) . . ? N5 C19 C20 120.9(4) . . ? O2 C19 C20 116.9(4) . . ? N6 C21 C22 121.9(4) . . ? C21 C22 C23 119.2(5) . . ? C22 C23 C24 119.4(5) . . ? C23 C24 C25 119.2(5) . . ? N6 C25 C24 120.8(5) . . ? N6 C25 C26 114.7(4) . . ? C24 C25 C26 124.4(4) . . ? N9 C26 C25 109.7(4) . . ? N7 C27 C28 121.2(5) . . ? C27 C28 C29 119.1(5) . . ? C30 C29 C28 120.1(5) . . ? C31 C30 C29 118.0(5) . . ? N7 C31 C30 121.6(5) . . ? N7 C31 C32 115.5(4) . . ? C30 C31 C32 122.8(5) . . ? N9 C32 C31 111.9(4) . . ? N8 C33 C34 121.0(5) . . ? C35 C34 C33 119.3(5) . . ? C34 C35 C36 119.7(5) . . ? C35 C36 C37 119.2(5) . . ? N8 C37 C36 120.8(5) . . ? N8 C37 C38 113.7(4) . . ? C36 C37 C38 125.5(5) . . ? C37 C38 N9 107.5(4) . . ? N10 C39 O4 119.0(4) . . ? N10 C39 C40 121.6(4) . . ? O4 C39 C40 119.4(4) . . ? C1 N1 C5 119.5(4) . . ? C1 N1 Co1 127.2(3) . . ? C5 N1 Co1 113.3(3) . . ? C7 N2 C11 119.6(4) . . ? C7 N2 Co1 125.2(3) . . ? C11 N2 Co1 115.0(3) . . ? C13 N3 C17 120.4(4) . . ? C13 N3 Co1 126.6(3) . . ? C17 N3 Co1 113.0(3) . . ? C12 N4 C6 111.9(4) . . ? C12 N4 C18 111.8(4) . . ? C6 N4 C18 112.2(4) . . ? C12 N4 Co1 110.3(3) . . ? C6 N4 Co1 105.1(3) . . ? C18 N4 Co1 105.0(3) . . ? C19 N5 O1 113.5(4) . . ? C21 N6 C25 119.6(4) . . ? C21 N6 Co2 126.7(3) . . ? C25 N6 Co2 113.6(3) . . ? C27 N7 C31 119.9(4) . . ? C27 N7 Co2 125.2(4) . . ? C31 N7 Co2 114.9(3) . . ? C33 N8 C37 120.0(4) . . ? C33 N8 Co2 127.0(3) . . ? C37 N8 Co2 112.9(3) . . ? C26 N9 C38 112.0(4) . . ? C26 N9 C32 112.5(4) . . ? C38 N9 C32 109.4(4) . . ? C26 N9 Co2 107.5(3) . . ? C38 N9 Co2 105.2(3) . . ? C32 N9 Co2 109.9(3) . . ? C39 N10 O3 118.2(4) . . ? N5 O1 Co1 108.8(2) . . ? C19 O2 Co1 108.0(3) . . ? N10 O3 Co2 106.4(2) . . ? C39 O4 Co2 109.7(3) . . ? O1 Co1 O2 86.78(14) . . ? O1 Co1 N2 177.71(15) . . ? O2 Co1 N2 94.07(15) . . ? O1 Co1 N1 89.57(15) . . ? O2 Co1 N1 95.98(15) . . ? N2 Co1 N1 92.45(16) . . ? O1 Co1 N3 88.79(15) . . ? O2 Co1 N3 93.29(15) . . ? N2 Co1 N3 89.04(16) . . ? N1 Co1 N3 170.48(16) . . ? O1 Co1 N4 92.58(16) . . ? O2 Co1 N4 178.15(15) . . ? N2 Co1 N4 86.50(17) . . ? N1 Co1 N4 85.75(17) . . ? N3 Co1 N4 84.96(16) . . ? O3 Co2 O4 86.59(13) . . ? O3 Co2 N7 179.45(16) . . ? O4 Co2 N7 92.94(15) . . ? O3 Co2 N6 88.46(15) . . ? O4 Co2 N6 95.73(15) . . ? N7 Co2 N6 91.30(16) . . ? O3 Co2 N8 89.44(15) . . ? O4 Co2 N8 94.16(15) . . ? N7 Co2 N8 90.89(16) . . ? N6 Co2 N8 169.75(16) . . ? O3 Co2 N9 93.35(15) . . ? O4 Co2 N9 178.48(15) . . ? N7 Co2 N9 87.13(17) . . ? N6 Co2 N9 85.79(16) . . ? N8 Co2 N9 84.32(16) . . ? Cl3 O13 O13A 69.0(7) . . ? O13 O13A Cl3 52.4(5) . . ? O7 Cl1 O8 115.3(5) . . ? O7 Cl1 O5 109.7(3) . . ? O8 Cl1 O5 111.0(5) . . ? O7 Cl1 O6 108.8(3) . . ? O8 Cl1 O6 105.0(4) . . ? O5 Cl1 O6 106.6(4) . . ? O11 Cl2 O10 110.3(4) . . ? O11 Cl2 O12 114.0(4) . . ? O10 Cl2 O12 108.4(3) . . ? O11 Cl2 O9 108.2(3) . . ? O10 Cl2 O9 107.4(3) . . ? O12 Cl2 O9 108.3(3) . . ? O13 Cl3 O15 130.7(6) . . ? O13 Cl3 O14 112.2(5) . . ? O15 Cl3 O14 109.8(4) . . ? O13 Cl3 O16 95.3(7) . . ? O15 Cl3 O16 99.9(4) . . ? O14 Cl3 O16 102.3(5) . . ? O13 Cl3 O13A 58.7(7) . . ? O15 Cl3 O13A 88.7(6) . . ? O14 Cl3 O13A 101.6(6) . . ? O16 Cl3 O13A 150.0(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.8(7) . . . . ? C1 C2 C3 C4 1.9(8) . . . . ? C2 C3 C4 C5 -1.2(8) . . . . ? C3 C4 C5 N1 -0.7(8) . . . . ? C3 C4 C5 C6 174.3(5) . . . . ? N1 C5 C6 N4 -30.5(6) . . . . ? C4 C5 C6 N4 154.1(5) . . . . ? N2 C7 C8 C9 -1.2(8) . . . . ? C7 C8 C9 C10 0.3(8) . . . . ? C8 C9 C10 C11 0.8(8) . . . . ? C9 C10 C11 N2 -1.1(7) . . . . ? C9 C10 C11 C12 177.2(5) . . . . ? N2 C11 C12 N4 -6.6(6) . . . . ? C10 C11 C12 N4 174.9(4) . . . . ? N3 C13 C14 C15 0.6(7) . . . . ? C13 C14 C15 C16 -0.5(8) . . . . ? C14 C15 C16 C17 -0.2(8) . . . . ? C15 C16 C17 N3 0.9(7) . . . . ? C15 C16 C17 C18 -177.0(5) . . . . ? N3 C17 C18 N4 29.8(6) . . . . ? C16 C17 C18 N4 -152.2(5) . . . . ? N6 C21 C22 C23 -0.1(8) . . . . ? C21 C22 C23 C24 -0.2(8) . . . . ? C22 C23 C24 C25 0.4(8) . . . . ? C23 C24 C25 N6 -0.4(8) . . . . ? C23 C24 C25 C26 174.1(5) . . . . ? N6 C25 C26 N9 -22.7(6) . . . . ? C24 C25 C26 N9 162.5(5) . . . . ? N7 C27 C28 C29 -1.1(8) . . . . ? C27 C28 C29 C30 1.6(8) . . . . ? C28 C29 C30 C31 -0.1(8) . . . . ? C29 C30 C31 N7 -2.0(7) . . . . ? C29 C30 C31 C32 179.5(5) . . . . ? N7 C31 C32 N9 4.9(6) . . . . ? C30 C31 C32 N9 -176.4(4) . . . . ? N8 C33 C34 C35 -0.1(8) . . . . ? C33 C34 C35 C36 -1.1(8) . . . . ? C34 C35 C36 C37 1.5(8) . . . . ? C35 C36 C37 N8 -0.8(8) . . . . ? C35 C36 C37 C38 -178.3(5) . . . . ? N8 C37 C38 N9 30.7(6) . . . . ? C36 C37 C38 N9 -151.7(5) . . . . ? C2 C1 N1 C5 -1.1(7) . . . . ? C2 C1 N1 Co1 178.4(4) . . . . ? C4 C5 N1 C1 1.9(7) . . . . ? C6 C5 N1 C1 -173.7(4) . . . . ? C4 C5 N1 Co1 -177.7(4) . . . . ? C6 C5 N1 Co1 6.7(6) . . . . ? C8 C7 N2 C11 1.0(7) . . . . ? C8 C7 N2 Co1 175.7(4) . . . . ? C10 C11 N2 C7 0.2(7) . . . . ? C12 C11 N2 C7 -178.2(4) . . . . ? C10 C11 N2 Co1 -175.0(4) . . . . ? C12 C11 N2 Co1 6.5(5) . . . . ? C14 C13 N3 C17 0.0(7) . . . . ? C14 C13 N3 Co1 -178.4(3) . . . . ? C16 C17 N3 C13 -0.8(7) . . . . ? C18 C17 N3 C13 177.3(4) . . . . ? C16 C17 N3 Co1 177.8(4) . . . . ? C18 C17 N3 Co1 -4.1(5) . . . . ? C11 C12 N4 C6 120.3(5) . . . . ? C11 C12 N4 C18 -112.8(5) . . . . ? C11 C12 N4 Co1 3.6(5) . . . . ? C5 C6 N4 C12 -81.7(5) . . . . ? C5 C6 N4 C18 151.6(4) . . . . ? C5 C6 N4 Co1 38.0(5) . . . . ? C17 C18 N4 C12 79.9(5) . . . . ? C17 C18 N4 C6 -153.4(4) . . . . ? C17 C18 N4 Co1 -39.7(4) . . . . ? O2 C19 N5 O1 0.0(6) . . . . ? C20 C19 N5 O1 -178.6(4) . . . . ? C22 C21 N6 C25 0.0(7) . . . . ? C22 C21 N6 Co2 -177.0(4) . . . . ? C24 C25 N6 C21 0.2(7) . . . . ? C26 C25 N6 C21 -174.8(4) . . . . ? C24 C25 N6 Co2 177.6(4) . . . . ? C26 C25 N6 Co2 2.6(5) . . . . ? C28 C27 N7 C31 -0.9(7) . . . . ? C28 C27 N7 Co2 179.7(4) . . . . ? C30 C31 N7 C27 2.5(7) . . . . ? C32 C31 N7 C27 -178.8(4) . . . . ? C30 C31 N7 Co2 -178.0(4) . . . . ? C32 C31 N7 Co2 0.6(5) . . . . ? C34 C33 N8 C37 0.8(7) . . . . ? C34 C33 N8 Co2 -178.1(4) . . . . ? C36 C37 N8 C33 -0.3(7) . . . . ? C38 C37 N8 C33 177.4(4) . . . . ? C36 C37 N8 Co2 178.7(4) . . . . ? C38 C37 N8 Co2 -3.6(5) . . . . ? C25 C26 N9 C38 146.2(4) . . . . ? C25 C26 N9 C32 -90.1(5) . . . . ? C25 C26 N9 Co2 31.1(5) . . . . ? C37 C38 N9 C26 -158.7(4) . . . . ? C37 C38 N9 C32 75.9(5) . . . . ? C37 C38 N9 Co2 -42.2(4) . . . . ? C31 C32 N9 C26 112.0(4) . . . . ? C31 C32 N9 C38 -122.9(4) . . . . ? C31 C32 N9 Co2 -7.9(5) . . . . ? O4 C39 N10 O3 2.2(6) . . . . ? C40 C39 N10 O3 -177.6(4) . . . . ? C19 N5 O1 Co1 6.4(4) . . . . ? N5 C19 O2 Co1 -6.3(5) . . . . ? C20 C19 O2 Co1 172.4(4) . . . . ? C39 N10 O3 Co2 -3.7(5) . . . . ? N10 C39 O4 Co2 0.6(5) . . . . ? C40 C39 O4 Co2 -179.6(4) . . . . ? N5 O1 Co1 O2 -7.8(3) . . . . ? N5 O1 Co1 N2 104(4) . . . . ? N5 O1 Co1 N1 -103.8(3) . . . . ? N5 O1 Co1 N3 85.6(3) . . . . ? N5 O1 Co1 N4 170.5(3) . . . . ? C19 O2 Co1 O1 7.7(3) . . . . ? C19 O2 Co1 N2 -170.2(3) . . . . ? C19 O2 Co1 N1 96.9(3) . . . . ? C19 O2 Co1 N3 -80.9(3) . . . . ? C19 O2 Co1 N4 -62(5) . . . . ? C7 N2 Co1 O1 -112(4) . . . . ? C11 N2 Co1 O1 63(4) . . . . ? C7 N2 Co1 O2 -0.3(4) . . . . ? C11 N2 Co1 O2 174.6(3) . . . . ? C7 N2 Co1 N1 95.9(4) . . . . ? C11 N2 Co1 N1 -89.2(3) . . . . ? C7 N2 Co1 N3 -93.5(4) . . . . ? C11 N2 Co1 N3 81.4(3) . . . . ? C7 N2 Co1 N4 -178.5(4) . . . . ? C11 N2 Co1 N4 -3.6(3) . . . . ? C1 N1 Co1 O1 100.9(4) . . . . ? C5 N1 Co1 O1 -79.6(3) . . . . ? C1 N1 Co1 O2 14.2(4) . . . . ? C5 N1 Co1 O2 -166.3(3) . . . . ? C1 N1 Co1 N2 -80.2(4) . . . . ? C5 N1 Co1 N2 99.4(4) . . . . ? C1 N1 Co1 N3 -179(56) . . . . ? C5 N1 Co1 N3 0.5(12) . . . . ? C1 N1 Co1 N4 -166.5(4) . . . . ? C5 N1 Co1 N4 13.0(4) . . . . ? C13 N3 Co1 O1 -105.0(4) . . . . ? C17 N3 Co1 O1 76.5(3) . . . . ? C13 N3 Co1 O2 -18.3(4) . . . . ? C17 N3 Co1 O2 163.2(3) . . . . ? C13 N3 Co1 N2 75.7(4) . . . . ? C17 N3 Co1 N2 -102.8(3) . . . . ? C13 N3 Co1 N1 174.8(8) . . . . ? C17 N3 Co1 N1 -3.7(11) . . . . ? C13 N3 Co1 N4 162.3(4) . . . . ? C17 N3 Co1 N4 -16.2(3) . . . . ? C12 N4 Co1 O1 -178.1(3) . . . . ? C6 N4 Co1 O1 61.0(3) . . . . ? C18 N4 Co1 O1 -57.5(3) . . . . ? C12 N4 Co1 O2 -108(5) . . . . ? C6 N4 Co1 O2 131(5) . . . . ? C18 N4 Co1 O2 12(5) . . . . ? C12 N4 Co1 N2 -0.2(3) . . . . ? C6 N4 Co1 N2 -121.1(3) . . . . ? C18 N4 Co1 N2 120.4(3) . . . . ? C12 N4 Co1 N1 92.5(3) . . . . ? C6 N4 Co1 N1 -28.4(3) . . . . ? C18 N4 Co1 N1 -146.9(3) . . . . ? C12 N4 Co1 N3 -89.6(3) . . . . ? C6 N4 Co1 N3 149.6(3) . . . . ? C18 N4 Co1 N3 31.1(3) . . . . ? N10 O3 Co2 O4 3.1(3) . . . . ? N10 O3 Co2 N7 -29(17) . . . . ? N10 O3 Co2 N6 -92.7(3) . . . . ? N10 O3 Co2 N8 97.3(3) . . . . ? N10 O3 Co2 N9 -178.4(3) . . . . ? C39 O4 Co2 O3 -2.2(3) . . . . ? C39 O4 Co2 N7 177.5(3) . . . . ? C39 O4 Co2 N6 85.9(3) . . . . ? C39 O4 Co2 N8 -91.4(3) . . . . ? C39 O4 Co2 N9 -90(6) . . . . ? C27 N7 Co2 O3 25(17) . . . . ? C31 N7 Co2 O3 -154(16) . . . . ? C27 N7 Co2 O4 -6.4(4) . . . . ? C31 N7 Co2 O4 174.1(3) . . . . ? C27 N7 Co2 N6 89.4(4) . . . . ? C31 N7 Co2 N6 -90.1(3) . . . . ? C27 N7 Co2 N8 -100.6(4) . . . . ? C31 N7 Co2 N8 79.9(3) . . . . ? C27 N7 Co2 N9 175.1(4) . . . . ? C31 N7 Co2 N9 -4.3(3) . . . . ? C21 N6 Co2 O3 96.8(4) . . . . ? C25 N6 Co2 O3 -80.4(3) . . . . ? C21 N6 Co2 O4 10.3(4) . . . . ? C25 N6 Co2 O4 -166.9(3) . . . . ? C21 N6 Co2 N7 -82.7(4) . . . . ? C25 N6 Co2 N7 100.1(3) . . . . ? C21 N6 Co2 N8 175.0(8) . . . . ? C25 N6 Co2 N8 -2.2(11) . . . . ? C21 N6 Co2 N9 -169.8(4) . . . . ? C25 N6 Co2 N9 13.0(3) . . . . ? C33 N8 Co2 O3 -105.3(4) . . . . ? C37 N8 Co2 O3 75.7(3) . . . . ? C33 N8 Co2 O4 -18.8(4) . . . . ? C37 N8 Co2 O4 162.3(3) . . . . ? C33 N8 Co2 N7 74.3(4) . . . . ? C37 N8 Co2 N7 -104.7(3) . . . . ? C33 N8 Co2 N6 176.5(8) . . . . ? C37 N8 Co2 N6 -2.4(11) . . . . ? C33 N8 Co2 N9 161.3(4) . . . . ? C37 N8 Co2 N9 -17.7(3) . . . . ? C26 N9 Co2 O3 63.7(3) . . . . ? C38 N9 Co2 O3 -55.9(3) . . . . ? C32 N9 Co2 O3 -173.5(3) . . . . ? C26 N9 Co2 O4 151(6) . . . . ? C38 N9 Co2 O4 32(6) . . . . ? C32 N9 Co2 O4 -86(6) . . . . ? C26 N9 Co2 N7 -116.1(3) . . . . ? C38 N9 Co2 N7 124.4(3) . . . . ? C32 N9 Co2 N7 6.7(3) . . . . ? C26 N9 Co2 N6 -24.6(3) . . . . ? C38 N9 Co2 N6 -144.1(3) . . . . ? C32 N9 Co2 N6 98.2(3) . . . . ? C26 N9 Co2 N8 152.8(3) . . . . ? C38 N9 Co2 N8 33.2(3) . . . . ? C32 N9 Co2 N8 -84.5(3) . . . . ? O13A O13 Cl3 O15 -56.1(9) . . . . ? O13A O13 Cl3 O14 90.4(8) . . . . ? O13A O13 Cl3 O16 -164.0(7) . . . . ? O13 O13A Cl3 O15 141.0(7) . . . . ? O13 O13A Cl3 O14 -109.0(6) . . . . ? O13 O13A Cl3 O16 33.2(13) . . . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 1.327 _refine_diff_density_min -0.838 _refine_diff_density_rms 0.112 # Attachment '2a.cif' data_twf36 _database_code_depnum_ccdc_archive 'CCDC 282773' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(pha-H)tpa](ClO4)0.5' _chemical_formula_sum 'C21 H31 Cl0.5 Co N5 O8' _chemical_formula_weight 558.16 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' S S 0.1246 0.1234 '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 10.819(2) _cell_length_b 14.213(3) _cell_length_c 32.478(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.463(4) _cell_angle_gamma 90.00 _cell_volume 4994.1(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhomb _exptl_crystal_colour blue/green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.847 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21504 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 28.27 _reflns_number_total 5904 _reflns_number_gt 5144 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.0719P)^2^+24.7697P] 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 5904 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1600 _refine_ls_wR_factor_gt 0.1552 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.154 _refine_ls_shift/su_mean 0.008 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5242(3) 1.0557(3) 0.87151(13) 0.0386(8) Uani 1 1 d . . . H1 H 0.5627 1.0583 0.8460 0.046 Uiso 1 1 calc R . . C2 C 0.4707(4) 1.1365(3) 0.88723(17) 0.0563(13) Uani 1 1 d . . . H2 H 0.4729 1.1927 0.8726 0.068 Uiso 1 1 calc R . . C3 C 0.4143(5) 1.1321(4) 0.92489(19) 0.0697(17) Uani 1 1 d . . . H3 H 0.3801 1.1860 0.9364 0.084 Uiso 1 1 calc R . . C4 C 0.4083(5) 1.0474(4) 0.94571(16) 0.0658(16) Uani 1 1 d . . . H4 H 0.3666 1.0433 0.9706 0.079 Uiso 1 1 calc R . . C5 C 0.4653(4) 0.9680(3) 0.92910(12) 0.0483(10) Uani 1 1 d . . . C6 C 0.4734(5) 0.8733(4) 0.94906(12) 0.0572(12) Uani 1 1 d . . . H6A H 0.4015 0.8627 0.9661 0.069 Uiso 1 1 calc R . . H6B H 0.5466 0.8699 0.9664 0.069 Uiso 1 1 calc R . . C7 C 0.4279(3) 0.8775(2) 0.79915(9) 0.0245(6) Uani 1 1 d . . . H7 H 0.4941 0.9104 0.7881 0.029 Uiso 1 1 calc R . . C8 C 0.3226(3) 0.8639(3) 0.77541(10) 0.0323(7) Uani 1 1 d . . . H8 H 0.3172 0.8879 0.7488 0.039 Uiso 1 1 calc R . . C9 C 0.2251(3) 0.8138(3) 0.79217(12) 0.0352(7) Uani 1 1 d . . . H9 H 0.1546 0.8018 0.7765 0.042 Uiso 1 1 calc R . . C10 C 0.2332(3) 0.7821(2) 0.83217(11) 0.0317(7) Uani 1 1 d . . . H10 H 0.1680 0.7491 0.8438 0.038 Uiso 1 1 calc R . . C11 C 0.3395(3) 0.7998(2) 0.85483(10) 0.0256(6) Uani 1 1 d . . . C12 C 0.3540(3) 0.7749(3) 0.89930(11) 0.0396(8) Uani 1 1 d . . . H12A H 0.3405 0.7079 0.9027 0.047 Uiso 1 1 calc R . . H12B H 0.2916 0.8078 0.9150 0.047 Uiso 1 1 calc R . . C13 C 0.6802(3) 0.6912(3) 0.82793(13) 0.0379(8) Uani 1 1 d . . . H13 H 0.6977 0.7321 0.8064 0.045 Uiso 1 1 calc R . . C14 C 0.7102(3) 0.5965(3) 0.82414(18) 0.0535(12) Uani 1 1 d . . . H14 H 0.7489 0.5742 0.8006 0.064 Uiso 1 1 calc R . . C15 C 0.6812(4) 0.5365(3) 0.8560(2) 0.0617(15) Uani 1 1 d . . . H15 H 0.7002 0.4729 0.8540 0.074 Uiso 1 1 calc R . . C16 C 0.6237(4) 0.5709(3) 0.89092(18) 0.0590(14) Uani 1 1 d . . . H16 H 0.6027 0.5306 0.9123 0.071 Uiso 1 1 calc R . . C17 C 0.5982(3) 0.6662(3) 0.89346(14) 0.0428(9) Uani 1 1 d . . . C18 C 0.5450(4) 0.7132(3) 0.93025(13) 0.0502(11) Uani 1 1 d . . . H18A H 0.4876 0.6713 0.9439 0.060 Uiso 1 1 calc R . . H18B H 0.6103 0.7295 0.9496 0.060 Uiso 1 1 calc R . . C19 C 0.7986(3) 0.9040(2) 0.84647(10) 0.0277(6) Uani 1 1 d . . . C20 C 0.8983(3) 0.9336(3) 0.81738(11) 0.0360(8) Uani 1 1 d . . . H20A H 0.8943 0.8948 0.7928 0.043 Uiso 1 1 calc R . . H20B H 0.9783 0.9239 0.8303 0.043 Uiso 1 1 calc R . . C21 C 0.8849(4) 1.0370(3) 0.80526(15) 0.0523(11) Uani 1 1 d . . . H21A H 0.8086 1.0457 0.7905 0.078 Uiso 1 1 calc R . . H21B H 0.9527 1.0549 0.7881 0.078 Uiso 1 1 calc R . . H21C H 0.8849 1.0752 0.8296 0.078 Uiso 1 1 calc R . . N1 N 0.5219(3) 0.9737(2) 0.89206(9) 0.0336(6) Uani 1 1 d . . . N2 N 0.4369(2) 0.84418(17) 0.83788(8) 0.0206(5) Uani 1 1 d . . . N3 N 0.6263(2) 0.7249(2) 0.86199(9) 0.0321(6) Uani 1 1 d . . . N4 N 0.4796(3) 0.7999(2) 0.91605(9) 0.0364(7) Uani 1 1 d . . . N5 N 0.8272(3) 0.8826(3) 0.88370(9) 0.0386(7) Uani 1 1 d . . . O1 O 0.7199(2) 0.8614(2) 0.90733(7) 0.0440(7) Uani 1 1 d . . . O2 O 0.68310(18) 0.90213(15) 0.83205(6) 0.0221(4) Uani 1 1 d . . . O1W O 0.0675(3) 0.8515(2) 0.91893(12) 0.0607(9) Uani 1 1 d . . . O3 O 0.5426(3) 0.1947(2) 0.71704(9) 0.0440(6) Uani 1 1 d . . . O2W O 0.0440(4) 0.9828(3) 0.99576(11) 0.0673(11) Uani 1 1 d . . . O4 O 0.4008(3) 0.0777(2) 0.73578(10) 0.0507(7) Uani 1 1 d . . . O3W O 0.7870(5) 0.8377(5) 0.98776(14) 0.119(2) Uani 1 1 d . . . O4W O 0.1566(6) 0.7169(4) 0.97451(17) 0.0467(13) Uani 0.50 1 d P . . O5W O 0.1777(5) 0.8597(9) 0.9992(2) 0.105(4) Uani 0.50 1 d P . . O6W O 0.2648(9) 0.5453(8) 0.9483(4) 0.266(7) Uani 1 1 d . . . Cl1 Cl 0.5000 0.13626(7) 0.7500 0.0266(2) Uani 1 2 d S . . Co1 Co 0.58103(4) 0.85363(3) 0.872974(12) 0.02366(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0306(17) 0.0324(18) 0.053(2) -0.0150(16) 0.0137(15) -0.0107(14) C2 0.043(2) 0.037(2) 0.089(4) -0.029(2) 0.025(2) -0.0148(17) C3 0.059(3) 0.054(3) 0.097(4) -0.048(3) 0.037(3) -0.023(2) C4 0.059(3) 0.085(4) 0.054(3) -0.044(3) 0.027(2) -0.025(3) C5 0.050(2) 0.068(3) 0.0278(18) -0.0182(18) 0.0121(16) -0.014(2) C6 0.066(3) 0.086(3) 0.0203(17) -0.0012(19) 0.0135(17) -0.006(2) C7 0.0219(14) 0.0300(15) 0.0216(14) 0.0000(11) 0.0020(11) -0.0050(11) C8 0.0249(15) 0.046(2) 0.0257(15) -0.0003(14) -0.0026(12) -0.0061(14) C9 0.0230(15) 0.0403(19) 0.0422(19) -0.0048(15) -0.0044(13) -0.0087(14) C10 0.0218(14) 0.0283(16) 0.0451(19) 0.0019(14) 0.0067(13) -0.0064(12) C11 0.0235(14) 0.0214(14) 0.0322(16) 0.0037(12) 0.0089(12) 0.0014(11) C12 0.0287(17) 0.055(2) 0.0355(18) 0.0161(16) 0.0120(14) -0.0002(16) C13 0.0208(15) 0.0314(17) 0.062(2) 0.0005(16) 0.0084(15) 0.0012(13) C14 0.0217(16) 0.0324(19) 0.106(4) -0.007(2) 0.006(2) 0.0007(14) C15 0.0225(17) 0.0285(19) 0.134(5) 0.012(2) -0.007(2) -0.0002(15) C16 0.0271(18) 0.042(2) 0.108(4) 0.040(3) -0.014(2) -0.0059(17) C17 0.0257(16) 0.041(2) 0.061(3) 0.0264(18) -0.0044(16) -0.0024(15) C18 0.038(2) 0.068(3) 0.045(2) 0.036(2) -0.0036(16) -0.0055(19) C19 0.0225(14) 0.0322(16) 0.0284(15) -0.0021(12) -0.0022(12) -0.0011(12) C20 0.0200(14) 0.050(2) 0.0378(18) -0.0016(16) -0.0010(13) -0.0068(14) C21 0.0313(19) 0.064(3) 0.061(3) 0.029(2) -0.0060(18) -0.0107(18) N1 0.0322(14) 0.0422(16) 0.0264(14) -0.0127(12) 0.0061(11) -0.0073(12) N2 0.0192(11) 0.0205(11) 0.0223(12) -0.0007(9) 0.0040(9) -0.0003(9) N3 0.0216(12) 0.0308(14) 0.0440(16) 0.0108(12) 0.0017(11) 0.0021(11) N4 0.0360(15) 0.0512(18) 0.0220(13) 0.0102(12) 0.0048(11) -0.0007(13) N5 0.0258(14) 0.059(2) 0.0311(15) 0.0059(14) -0.0075(11) -0.0057(13) O1 0.0329(13) 0.078(2) 0.0214(11) 0.0109(12) -0.0065(10) -0.0105(13) O2 0.0175(9) 0.0292(11) 0.0197(10) 0.0011(8) -0.0013(7) -0.0023(8) O1W 0.0351(15) 0.0516(18) 0.095(3) 0.0147(17) -0.0139(16) -0.0021(13) O3 0.0419(15) 0.0411(15) 0.0490(16) 0.0140(12) 0.0099(12) 0.0061(12) O2W 0.092(3) 0.059(2) 0.0503(19) -0.0084(16) -0.032(2) -0.003(2) O4 0.0392(15) 0.0544(18) 0.0583(18) -0.0121(14) -0.0062(13) -0.0191(13) O3W 0.116(4) 0.188(6) 0.054(3) 0.005(3) -0.016(3) -0.027(4) O4W 0.052(3) 0.055(3) 0.033(3) 0.012(2) 0.001(2) -0.016(3) O5W 0.022(3) 0.255(13) 0.038(3) 0.022(5) 0.017(2) 0.045(5) O6W 0.180(8) 0.288(12) 0.327(13) -0.232(11) -0.094(9) 0.033(8) Cl1 0.0213(5) 0.0243(5) 0.0343(5) 0.000 -0.0031(4) 0.000 Co1 0.0233(2) 0.0306(2) 0.0171(2) 0.00253(15) 0.00059(15) -0.00063(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.343(5) . ? C1 C2 1.386(5) . ? C2 C3 1.373(7) . ? C3 C4 1.383(8) . ? C4 C5 1.397(7) . ? C5 N1 1.357(5) . ? C5 C6 1.496(7) . ? C6 N4 1.498(6) . ? C7 N2 1.347(4) . ? C7 C8 1.385(4) . ? C8 C9 1.388(5) . ? C9 C10 1.377(5) . ? C10 C11 1.384(5) . ? C11 N2 1.348(4) . ? C11 C12 1.494(5) . ? C12 N4 1.502(5) . ? C13 N3 1.342(5) . ? C13 C14 1.390(5) . ? C14 C15 1.378(7) . ? C15 C16 1.387(8) . ? C16 C17 1.385(6) . ? C17 N3 1.355(5) . ? C17 C18 1.488(7) . ? C18 N4 1.492(5) . ? C19 N5 1.282(4) . ? C19 O2 1.331(4) . ? C19 C20 1.500(5) . ? C20 C21 1.527(6) . ? N1 Co1 1.927(3) . ? N2 Co1 1.929(3) . ? N3 Co1 1.929(3) . ? N4 Co1 1.942(3) . ? N5 O1 1.429(4) . ? O1 Co1 1.867(2) . ? O2 Co1 1.867(2) . ? O3 Cl1 1.434(3) . ? O2W O2W 1.108(7) 5_577 ? O4 Cl1 1.432(3) . ? Cl1 O4 1.432(3) 2_656 ? Cl1 O3 1.434(3) 2_656 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.8(4) . . ? C3 C2 C1 118.7(5) . . ? C2 C3 C4 119.9(4) . . ? C3 C4 C5 119.5(4) . . ? N1 C5 C4 119.8(5) . . ? N1 C5 C6 114.4(4) . . ? C4 C5 C6 125.7(4) . . ? C5 C6 N4 108.6(3) . . ? N2 C7 C8 121.6(3) . . ? C7 C8 C9 118.6(3) . . ? C10 C9 C8 119.7(3) . . ? C9 C10 C11 119.2(3) . . ? N2 C11 C10 121.1(3) . . ? N2 C11 C12 115.4(3) . . ? C10 C11 C12 123.4(3) . . ? C11 C12 N4 112.4(3) . . ? N3 C13 C14 121.4(4) . . ? C15 C14 C13 118.6(5) . . ? C14 C15 C16 120.1(4) . . ? C17 C16 C15 119.0(4) . . ? N3 C17 C16 120.7(4) . . ? N3 C17 C18 114.9(3) . . ? C16 C17 C18 124.4(4) . . ? N4 C18 C17 107.9(3) . . ? N5 C19 O2 123.1(3) . . ? N5 C19 C20 119.4(3) . . ? O2 C19 C20 117.5(3) . . ? C19 C20 C21 111.4(3) . . ? C1 N1 C5 120.2(3) . . ? C1 N1 Co1 126.9(2) . . ? C5 N1 Co1 112.6(3) . . ? C7 N2 C11 119.7(3) . . ? C7 N2 Co1 125.4(2) . . ? C11 N2 Co1 115.0(2) . . ? C13 N3 C17 120.3(3) . . ? C13 N3 Co1 127.1(2) . . ? C17 N3 Co1 112.6(3) . . ? C18 N4 C6 112.2(3) . . ? C18 N4 C12 110.0(3) . . ? C6 N4 C12 112.2(3) . . ? C18 N4 Co1 106.2(2) . . ? C6 N4 Co1 105.7(3) . . ? C12 N4 Co1 110.3(2) . . ? C19 N5 O1 111.4(3) . . ? N5 O1 Co1 110.18(18) . . ? C19 O2 Co1 108.41(19) . . ? O4 Cl1 O4 108.9(3) . 2_656 ? O4 Cl1 O3 109.90(18) . . ? O4 Cl1 O3 109.46(17) 2_656 . ? O4 Cl1 O3 109.46(17) . 2_656 ? O4 Cl1 O3 109.90(18) 2_656 2_656 ? O3 Cl1 O3 109.2(2) . 2_656 ? O1 Co1 O2 85.75(10) . . ? O1 Co1 N1 91.30(13) . . ? O2 Co1 N1 95.84(11) . . ? O1 Co1 N3 87.85(13) . . ? O2 Co1 N3 93.79(11) . . ? N1 Co1 N3 170.24(13) . . ? O1 Co1 N2 179.26(12) . . ? O2 Co1 N2 94.89(10) . . ? N1 Co1 N2 89.01(11) . . ? N3 Co1 N2 91.73(11) . . ? O1 Co1 N4 92.83(12) . . ? O2 Co1 N4 177.89(12) . . ? N1 Co1 N4 85.74(14) . . ? N3 Co1 N4 84.59(13) . . ? N2 Co1 N4 86.52(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.2(7) . . . . ? C1 C2 C3 C4 -2.1(8) . . . . ? C2 C3 C4 C5 3.2(8) . . . . ? C3 C4 C5 N1 -2.4(7) . . . . ? C3 C4 C5 C6 176.1(5) . . . . ? N1 C5 C6 N4 -30.0(5) . . . . ? C4 C5 C6 N4 151.4(4) . . . . ? N2 C7 C8 C9 -0.7(5) . . . . ? C7 C8 C9 C10 2.4(5) . . . . ? C8 C9 C10 C11 -0.8(5) . . . . ? C9 C10 C11 N2 -2.8(5) . . . . ? C9 C10 C11 C12 175.2(3) . . . . ? N2 C11 C12 N4 -3.3(4) . . . . ? C10 C11 C12 N4 178.6(3) . . . . ? N3 C13 C14 C15 1.3(6) . . . . ? C13 C14 C15 C16 -0.2(6) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C15 C16 C17 N3 1.4(6) . . . . ? C15 C16 C17 C18 -175.6(4) . . . . ? N3 C17 C18 N4 28.2(4) . . . . ? C16 C17 C18 N4 -154.7(4) . . . . ? N5 C19 C20 C21 -112.8(4) . . . . ? O2 C19 C20 C21 66.7(4) . . . . ? C2 C1 N1 C5 0.6(6) . . . . ? C2 C1 N1 Co1 175.2(3) . . . . ? C4 C5 N1 C1 0.6(6) . . . . ? C6 C5 N1 C1 -178.1(4) . . . . ? C4 C5 N1 Co1 -174.8(3) . . . . ? C6 C5 N1 Co1 6.5(4) . . . . ? C8 C7 N2 C11 -2.8(5) . . . . ? C8 C7 N2 Co1 177.0(2) . . . . ? C10 C11 N2 C7 4.5(4) . . . . ? C12 C11 N2 C7 -173.6(3) . . . . ? C10 C11 N2 Co1 -175.3(2) . . . . ? C12 C11 N2 Co1 6.5(4) . . . . ? C14 C13 N3 C17 -1.0(5) . . . . ? C14 C13 N3 Co1 178.8(3) . . . . ? C16 C17 N3 C13 -0.4(5) . . . . ? C18 C17 N3 C13 176.9(3) . . . . ? C16 C17 N3 Co1 179.7(3) . . . . ? C18 C17 N3 Co1 -3.0(4) . . . . ? C17 C18 N4 C6 -153.8(3) . . . . ? C17 C18 N4 C12 80.5(4) . . . . ? C17 C18 N4 Co1 -38.8(4) . . . . ? C5 C6 N4 C18 153.1(4) . . . . ? C5 C6 N4 C12 -82.5(4) . . . . ? C5 C6 N4 Co1 37.8(4) . . . . ? C11 C12 N4 C18 -118.1(3) . . . . ? C11 C12 N4 C6 116.2(4) . . . . ? C11 C12 N4 Co1 -1.4(4) . . . . ? O2 C19 N5 O1 -2.7(5) . . . . ? C20 C19 N5 O1 176.7(3) . . . . ? C19 N5 O1 Co1 9.3(4) . . . . ? N5 C19 O2 Co1 -5.2(4) . . . . ? C20 C19 O2 Co1 175.3(2) . . . . ? N5 O1 Co1 O2 -9.8(2) . . . . ? N5 O1 Co1 N1 -105.6(3) . . . . ? N5 O1 Co1 N3 84.2(3) . . . . ? N5 O1 Co1 N2 140(10) . . . . ? N5 O1 Co1 N4 168.6(3) . . . . ? C19 O2 Co1 O1 8.3(2) . . . . ? C19 O2 Co1 N1 99.1(2) . . . . ? C19 O2 Co1 N3 -79.3(2) . . . . ? C19 O2 Co1 N2 -171.4(2) . . . . ? C19 O2 Co1 N4 -40(3) . . . . ? C1 N1 Co1 O1 105.5(3) . . . . ? C5 N1 Co1 O1 -79.5(3) . . . . ? C1 N1 Co1 O2 19.7(3) . . . . ? C5 N1 Co1 O2 -165.4(3) . . . . ? C1 N1 Co1 N3 -169.6(6) . . . . ? C5 N1 Co1 N3 5.4(9) . . . . ? C1 N1 Co1 N2 -75.2(3) . . . . ? C5 N1 Co1 N2 99.8(3) . . . . ? C1 N1 Co1 N4 -161.7(3) . . . . ? C5 N1 Co1 N4 13.2(3) . . . . ? C13 N3 Co1 O1 -103.3(3) . . . . ? C17 N3 Co1 O1 76.5(2) . . . . ? C13 N3 Co1 O2 -17.7(3) . . . . ? C17 N3 Co1 O2 162.1(2) . . . . ? C13 N3 Co1 N1 171.5(6) . . . . ? C17 N3 Co1 N1 -8.7(9) . . . . ? C13 N3 Co1 N2 77.3(3) . . . . ? C17 N3 Co1 N2 -102.9(2) . . . . ? C13 N3 Co1 N4 163.6(3) . . . . ? C17 N3 Co1 N4 -16.6(2) . . . . ? C7 N2 Co1 O1 -157(10) . . . . ? C11 N2 Co1 O1 23(10) . . . . ? C7 N2 Co1 O2 -7.4(3) . . . . ? C11 N2 Co1 O2 172.5(2) . . . . ? C7 N2 Co1 N1 88.4(3) . . . . ? C11 N2 Co1 N1 -91.7(2) . . . . ? C7 N2 Co1 N3 -101.3(3) . . . . ? C11 N2 Co1 N3 78.5(2) . . . . ? C7 N2 Co1 N4 174.2(3) . . . . ? C11 N2 Co1 N4 -6.0(2) . . . . ? C18 N4 Co1 O1 -56.7(3) . . . . ? C6 N4 Co1 O1 62.6(3) . . . . ? C12 N4 Co1 O1 -175.9(3) . . . . ? C18 N4 Co1 O2 -9(3) . . . . ? C6 N4 Co1 O2 110(3) . . . . ? C12 N4 Co1 O2 -128(3) . . . . ? C18 N4 Co1 N1 -147.8(3) . . . . ? C6 N4 Co1 N1 -28.5(3) . . . . ? C12 N4 Co1 N1 93.0(3) . . . . ? C18 N4 Co1 N3 30.9(3) . . . . ? C6 N4 Co1 N3 150.2(3) . . . . ? C12 N4 Co1 N3 -88.3(3) . . . . ? C18 N4 Co1 N2 123.0(3) . . . . ? C6 N4 Co1 N2 -117.7(3) . . . . ? C12 N4 Co1 N2 3.8(3) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 0.856 _refine_diff_density_min -0.814 _refine_diff_density_rms 0.092 data_twf26 _database_code_depnum_ccdc_archive 'CCDC 282774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(pha)tpa](ClO4)1.5' _chemical_formula_sum 'C21 H24 Cl1.50 Co N5 O8' _chemical_formula_weight 586.56 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 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 19.720(7) _cell_length_b 18.459(7) _cell_length_c 17.196(6) _cell_angle_alpha 90.00 _cell_angle_beta 124.426(6) _cell_angle_gamma 90.00 _cell_volume 5163(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour grey/green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 0.874 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22888 _diffrn_reflns_av_R_equivalents 0.0973 _diffrn_reflns_av_sigmaI/netI 0.0907 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.39 _reflns_number_total 6069 _reflns_number_gt 2549 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-86 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.1329P)^2^+28.8445P] 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 6069 _refine_ls_number_parameters 336 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.2021 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.3149 _refine_ls_wR_factor_gt 0.2141 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3218(5) 0.6672(6) 0.4596(6) 0.074(2) Uani 1 1 d . . . C2 C 0.2752(7) 0.5996(7) 0.4504(10) 0.124(4) Uani 1 1 d . . . H2A H 0.2457 0.6082 0.4794 0.149 Uiso 1 1 calc R . . H2B H 0.2348 0.5902 0.3839 0.149 Uiso 1 1 calc R . . C3 C 0.3271(11) 0.5345(8) 0.4936(13) 0.177(7) Uani 1 1 d . . . H3A H 0.3631 0.5410 0.5606 0.266 Uiso 1 1 calc R . . H3B H 0.3593 0.5272 0.4683 0.266 Uiso 1 1 calc R . . H3C H 0.2928 0.4930 0.4799 0.266 Uiso 1 1 calc R . . C4 C 0.3995(6) 0.9008(5) 0.4095(7) 0.090(3) Uani 1 1 d . . . H4A H 0.3688 0.9164 0.4349 0.108 Uiso 1 1 calc R . . H4B H 0.4208 0.9435 0.3971 0.108 Uiso 1 1 calc R . . C5 C 0.3451(5) 0.8596(5) 0.3209(6) 0.073(2) Uani 1 1 d . . . C6 C 0.2950(6) 0.8920(6) 0.2317(8) 0.104(3) Uani 1 1 d . . . H6 H 0.2964 0.9418 0.2243 0.124 Uiso 1 1 calc R . . C7 C 0.2439(7) 0.8482(8) 0.1557(8) 0.109(4) Uani 1 1 d . . . H7 H 0.2094 0.8679 0.0957 0.130 Uiso 1 1 calc R . . C8 C 0.2447(6) 0.7763(7) 0.1692(6) 0.094(3) Uani 1 1 d . . . H8 H 0.2095 0.7466 0.1181 0.112 Uiso 1 1 calc R . . C9 C 0.2958(5) 0.7460(5) 0.2560(5) 0.069(2) Uani 1 1 d . . . H9 H 0.2962 0.6960 0.2633 0.083 Uiso 1 1 calc R . . C10 C 0.5379(5) 0.8530(5) 0.4649(6) 0.073(2) Uani 1 1 d . . . H10A H 0.5279 0.8907 0.4202 0.087 Uiso 1 1 calc R . . H10B H 0.5890 0.8642 0.5244 0.087 Uiso 1 1 calc R . . C11 C 0.5460(4) 0.7823(5) 0.4299(5) 0.0624(19) Uani 1 1 d . . . C12 C 0.5996(5) 0.7701(6) 0.4051(6) 0.080(3) Uani 1 1 d . . . H12 H 0.6317 0.8077 0.4066 0.097 Uiso 1 1 calc R . . C13 C 0.6059(6) 0.7014(7) 0.3779(7) 0.095(3) Uani 1 1 d . . . H13 H 0.6426 0.6923 0.3613 0.114 Uiso 1 1 calc R . . C14 C 0.5587(6) 0.6479(6) 0.3754(7) 0.090(3) Uani 1 1 d . . . H14 H 0.5634 0.6012 0.3585 0.108 Uiso 1 1 calc R . . C15 C 0.5034(5) 0.6623(4) 0.3979(6) 0.068(2) Uani 1 1 d . . . H15 H 0.4692 0.6255 0.3937 0.081 Uiso 1 1 calc R . . C16 C 0.5006(6) 0.8694(7) 0.5787(7) 0.103(4) Uani 1 1 d . . . H16A H 0.5418 0.9072 0.6022 0.123 Uiso 1 1 calc R . . H16B H 0.4560 0.8868 0.5823 0.123 Uiso 1 1 calc R . . C17 C 0.5366(7) 0.8045(8) 0.6369(7) 0.098(3) Uani 1 1 d U . . C18 C 0.5965(9) 0.7999(9) 0.7361(10) 0.140(5) Uani 1 1 d U . . H18 H 0.6207 0.8413 0.7726 0.168 Uiso 1 1 calc R . . C19 C 0.6155(11) 0.7360(11) 0.7730(12) 0.155(6) Uani 1 1 d U . . H19 H 0.6505 0.7347 0.8384 0.186 Uiso 1 1 calc R . . C20 C 0.5926(9) 0.6728(10) 0.7312(10) 0.143(5) Uani 1 1 d U . . H20 H 0.6137 0.6289 0.7625 0.172 Uiso 1 1 calc R . . C21 C 0.5329(6) 0.6786(7) 0.6341(7) 0.098(3) Uani 1 1 d U . . H21 H 0.5111 0.6362 0.5992 0.118 Uiso 1 1 calc R . . N1 N 0.3454(3) 0.7882(3) 0.3309(4) 0.0543(14) Uani 1 1 d . . . N2 N 0.4977(4) 0.7285(4) 0.4257(4) 0.0600(16) Uani 1 1 d . . . N3 N 0.5060(4) 0.7416(5) 0.5893(5) 0.082(2) Uani 1 1 d . . . N4 N 0.4687(4) 0.8527(4) 0.4784(5) 0.0681(18) Uani 1 1 d . . . N5 N 0.3075(4) 0.7266(5) 0.4846(5) 0.083(2) Uani 1 1 d . . . H5 H 0.2722 0.7293 0.4989 0.100 Uiso 1 1 calc R . . O1 O 0.3768(3) 0.6649(3) 0.4412(4) 0.0680(14) Uani 1 1 d . . . O2 O 0.3509(3) 0.7873(3) 0.4883(4) 0.0731(15) Uani 1 1 d . . . O3 O 0.2063(5) 0.4332(5) 0.6802(7) 0.147(3) Uani 1 1 d . . . O4 O 0.3429(5) 0.4320(6) 0.7247(7) 0.172(4) Uani 1 1 d . . . O5 O 0.2588(6) 0.5221(4) 0.6314(7) 0.149(4) Uani 1 1 d . . . O6 O 0.2395(6) 0.4004(6) 0.5771(8) 0.169(4) Uani 1 1 d . . . Cl1 Cl 0.26113(16) 0.44787(15) 0.6545(2) 0.0991(9) Uani 1 1 d . . . Cl2 Cl 0.0000 0.4818(3) 0.2500 0.1238(15) Uani 1 2 d S . . O11 O 0.0000 0.4072(10) 0.2500 0.255(11) Uani 1 2 d S . . O12 O 0.0556(12) 0.5106(17) 0.245(2) 0.318(18) Uani 0.75 1 d P . . O13 O 0.039(3) 0.4962(11) 0.3385(16) 0.36(2) Uani 0.75 1 d P . . Co1 Co 0.42332(6) 0.75632(6) 0.45806(7) 0.0565(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(5) 0.108(7) 0.060(5) 0.012(5) 0.033(4) 0.004(5) C2 0.088(7) 0.124(10) 0.164(11) 0.050(9) 0.074(8) -0.001(7) C3 0.230(18) 0.127(13) 0.24(2) -0.001(13) 0.171(17) -0.026(13) C4 0.084(6) 0.055(5) 0.123(8) -0.017(5) 0.054(6) 0.004(5) C5 0.066(5) 0.062(5) 0.081(6) 0.000(4) 0.035(5) 0.008(4) C6 0.082(7) 0.087(7) 0.108(8) 0.017(7) 0.033(7) 0.015(6) C7 0.094(8) 0.125(10) 0.086(8) 0.031(7) 0.039(7) 0.027(8) C8 0.071(6) 0.128(9) 0.057(5) -0.007(6) 0.022(5) 0.004(6) C9 0.055(4) 0.092(6) 0.054(4) -0.012(4) 0.027(4) -0.003(4) C10 0.056(5) 0.086(6) 0.080(5) -0.004(5) 0.041(4) -0.006(4) C11 0.050(4) 0.078(5) 0.059(4) 0.009(4) 0.030(4) 0.008(4) C12 0.073(6) 0.108(7) 0.081(6) 0.018(5) 0.056(5) 0.015(5) C13 0.082(6) 0.121(9) 0.108(8) 0.000(7) 0.069(6) 0.014(6) C14 0.090(7) 0.102(8) 0.092(7) 0.004(6) 0.059(6) 0.030(6) C15 0.070(5) 0.066(5) 0.070(5) -0.001(4) 0.042(4) 0.013(4) C16 0.083(6) 0.140(10) 0.106(8) -0.068(8) 0.067(6) -0.051(7) C17 0.095(6) 0.138(7) 0.069(5) -0.015(5) 0.051(5) -0.024(6) C18 0.131(8) 0.165(9) 0.111(8) -0.019(7) 0.061(6) -0.038(7) C19 0.172(10) 0.182(10) 0.115(8) 0.012(7) 0.084(7) -0.018(8) C20 0.142(8) 0.174(9) 0.121(8) 0.047(7) 0.078(7) -0.010(7) C21 0.074(5) 0.144(8) 0.076(6) 0.020(5) 0.041(5) -0.003(5) N1 0.049(3) 0.058(4) 0.056(3) 0.000(3) 0.030(3) 0.007(3) N2 0.048(3) 0.077(4) 0.053(3) 0.002(3) 0.028(3) 0.012(3) N3 0.050(4) 0.144(7) 0.053(4) -0.004(5) 0.030(3) -0.011(4) N4 0.056(4) 0.080(5) 0.071(4) -0.027(3) 0.038(3) -0.009(3) N5 0.056(4) 0.135(7) 0.067(4) -0.010(4) 0.039(4) -0.005(4) O1 0.058(3) 0.080(4) 0.069(3) 0.003(3) 0.038(3) -0.003(3) O2 0.060(3) 0.096(4) 0.076(4) -0.020(3) 0.047(3) -0.010(3) O3 0.143(7) 0.141(7) 0.217(10) 0.014(7) 0.139(8) -0.010(6) O4 0.087(5) 0.207(11) 0.153(8) 0.038(7) 0.028(6) 0.033(6) O5 0.191(9) 0.081(5) 0.223(10) 0.057(6) 0.146(9) 0.046(5) O6 0.154(8) 0.155(9) 0.198(10) -0.058(8) 0.100(8) -0.012(7) Cl1 0.0839(17) 0.0841(18) 0.131(2) 0.0200(16) 0.0623(17) 0.0176(13) Cl2 0.174(5) 0.124(4) 0.124(4) 0.000 0.115(4) 0.000 O11 0.47(4) 0.142(15) 0.155(14) 0.000 0.17(2) 0.000 O12 0.159(14) 0.48(4) 0.32(3) 0.25(3) 0.138(18) 0.037(19) O13 0.76(7) 0.148(15) 0.181(19) -0.016(14) 0.27(3) 0.03(3) Co1 0.0468(5) 0.0766(8) 0.0495(6) -0.0080(5) 0.0292(4) -0.0014(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 C1 N5 1.268(11) . ? C1 O1 1.289(9) . ? C1 C2 1.503(14) . ? C2 C3 1.478(18) . ? C4 C5 1.484(12) . ? C4 N4 1.492(11) . ? C5 N1 1.328(10) . ? C5 C6 1.405(13) . ? C6 C7 1.375(15) . ? C7 C8 1.347(15) . ? C8 C9 1.362(12) . ? C9 N1 1.341(10) . ? C10 C11 1.483(11) . ? C10 N4 1.509(9) . ? C11 N2 1.350(10) . ? C11 C12 1.364(10) . ? C12 C13 1.382(14) . ? C13 C14 1.341(14) . ? C14 C15 1.375(11) . ? C15 N2 1.339(9) . ? C16 C17 1.462(15) . ? C16 N4 1.496(11) . ? C17 N3 1.350(13) . ? C17 C18 1.426(16) . ? C18 C19 1.29(2) . ? C19 C20 1.31(2) . ? C20 C21 1.401(16) . ? C21 N3 1.330(13) . ? N1 Co1 1.922(6) . ? N2 Co1 1.910(6) . ? N3 Co1 1.914(7) . ? N4 Co1 1.933(7) . ? N5 O2 1.390(10) . ? O1 Co1 1.863(5) . ? O2 Co1 1.863(5) . ? O3 Cl1 1.407(8) . ? O4 Cl1 1.393(8) . ? O5 Cl1 1.421(8) . ? O6 Cl1 1.441(10) . ? Cl2 O12 1.265(18) . ? Cl2 O12 1.265(18) 2 ? Cl2 O13 1.29(2) . ? Cl2 O13 1.29(2) 2 ? Cl2 O11 1.378(18) . ? O12 O13 1.61(4) 2 ? O13 O12 1.61(4) 2 ? 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 N5 C1 O1 119.4(9) . . ? N5 C1 C2 120.9(9) . . ? O1 C1 C2 119.7(10) . . ? C3 C2 C1 114.4(10) . . ? C5 C4 N4 108.4(7) . . ? N1 C5 C6 120.9(9) . . ? N1 C5 C4 115.4(8) . . ? C6 C5 C4 123.8(9) . . ? C7 C6 C5 118.2(10) . . ? C8 C7 C6 119.0(10) . . ? C7 C8 C9 121.5(10) . . ? N1 C9 C8 120.0(9) . . ? C11 C10 N4 111.9(7) . . ? N2 C11 C12 120.6(8) . . ? N2 C11 C10 115.8(7) . . ? C12 C11 C10 123.5(8) . . ? C11 C12 C13 119.5(9) . . ? C14 C13 C12 119.6(9) . . ? C13 C14 C15 119.6(9) . . ? N2 C15 C14 121.2(9) . . ? C17 C16 N4 110.2(8) . . ? N3 C17 C18 117.3(12) . . ? N3 C17 C16 114.3(9) . . ? C18 C17 C16 128.3(12) . . ? C19 C18 C17 117.1(15) . . ? C18 C19 C20 129.1(17) . . ? C19 C20 C21 112.5(15) . . ? N3 C21 C20 123.3(12) . . ? C5 N1 C9 120.4(7) . . ? C5 N1 Co1 113.2(5) . . ? C9 N1 Co1 126.5(6) . . ? C15 N2 C11 119.5(7) . . ? C15 N2 Co1 125.6(6) . . ? C11 N2 Co1 114.9(5) . . ? C21 N3 C17 120.4(9) . . ? C21 N3 Co1 127.0(8) . . ? C17 N3 Co1 112.6(8) . . ? C4 N4 C16 113.1(7) . . ? C4 N4 C10 112.1(7) . . ? C16 N4 C10 110.5(6) . . ? C4 N4 Co1 106.4(5) . . ? C16 N4 Co1 104.4(6) . . ? C10 N4 Co1 110.0(5) . . ? C1 N5 O2 117.6(7) . . ? C1 O1 Co1 110.0(6) . . ? N5 O2 Co1 106.9(5) . . ? O4 Cl1 O3 113.9(7) . . ? O4 Cl1 O5 106.4(6) . . ? O3 Cl1 O5 111.4(5) . . ? O4 Cl1 O6 105.5(7) . . ? O3 Cl1 O6 107.0(6) . . ? O5 Cl1 O6 112.5(7) . . ? O12 Cl2 O12 130(3) . 2 ? O12 Cl2 O13 91.6(17) . . ? O12 Cl2 O13 78.4(16) 2 . ? O12 Cl2 O13 78.4(16) . 2 ? O12 Cl2 O13 91.6(17) 2 2 ? O13 Cl2 O13 156.2(18) . 2 ? O12 Cl2 O11 114.8(15) . . ? O12 Cl2 O11 114.8(15) 2 . ? O13 Cl2 O11 101.9(9) . . ? O13 Cl2 O11 101.9(9) 2 . ? Cl2 O12 O13 51.3(11) . 2 ? Cl2 O13 O12 50.2(12) . 2 ? O1 Co1 O2 86.2(2) . . ? O1 Co1 N2 95.9(3) . . ? O2 Co1 N2 177.7(3) . . ? O1 Co1 N3 94.1(3) . . ? O2 Co1 N3 89.4(3) . . ? N2 Co1 N3 91.3(3) . . ? O1 Co1 N1 95.4(2) . . ? O2 Co1 N1 88.7(2) . . ? N2 Co1 N1 90.1(2) . . ? N3 Co1 N1 170.2(3) . . ? O1 Co1 N4 177.0(2) . . ? O2 Co1 N4 90.9(3) . . ? N2 Co1 N4 87.0(3) . . ? N3 Co1 N4 85.3(3) . . ? N1 Co1 N4 85.1(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 C1 C2 C3 -134.2(12) . . . . ? O1 C1 C2 C3 46.2(16) . . . . ? N4 C4 C5 N1 27.1(11) . . . . ? N4 C4 C5 C6 -153.9(9) . . . . ? N1 C5 C6 C7 2.5(15) . . . . ? C4 C5 C6 C7 -176.4(9) . . . . ? C5 C6 C7 C8 -0.9(17) . . . . ? C6 C7 C8 C9 -1.1(18) . . . . ? C7 C8 C9 N1 1.7(15) . . . . ? N4 C10 C11 N2 -6.7(10) . . . . ? N4 C10 C11 C12 174.9(7) . . . . ? N2 C11 C12 C13 -1.7(12) . . . . ? C10 C11 C12 C13 176.7(8) . . . . ? C11 C12 C13 C14 0.5(14) . . . . ? C12 C13 C14 C15 1.5(15) . . . . ? C13 C14 C15 N2 -2.5(14) . . . . ? N4 C16 C17 N3 -25.8(11) . . . . ? N4 C16 C17 C18 156.9(10) . . . . ? N3 C17 C18 C19 -1.3(19) . . . . ? C16 C17 C18 C19 176.0(13) . . . . ? C17 C18 C19 C20 6(3) . . . . ? C18 C19 C20 C21 -7(3) . . . . ? C19 C20 C21 N3 3.1(19) . . . . ? C6 C5 N1 C9 -2.1(12) . . . . ? C4 C5 N1 C9 177.0(7) . . . . ? C6 C5 N1 Co1 176.6(7) . . . . ? C4 C5 N1 Co1 -4.3(9) . . . . ? C8 C9 N1 C5 0.0(12) . . . . ? C8 C9 N1 Co1 -178.5(6) . . . . ? C14 C15 N2 C11 1.4(12) . . . . ? C14 C15 N2 Co1 179.5(6) . . . . ? C12 C11 N2 C15 0.7(11) . . . . ? C10 C11 N2 C15 -177.8(7) . . . . ? C12 C11 N2 Co1 -177.6(6) . . . . ? C10 C11 N2 Co1 3.9(8) . . . . ? C20 C21 N3 C17 0.7(15) . . . . ? C20 C21 N3 Co1 -178.6(8) . . . . ? C18 C17 N3 C21 -1.7(14) . . . . ? C16 C17 N3 C21 -179.4(8) . . . . ? C18 C17 N3 Co1 177.7(8) . . . . ? C16 C17 N3 Co1 0.0(10) . . . . ? C5 C4 N4 C16 -149.8(8) . . . . ? C5 C4 N4 C10 84.5(9) . . . . ? C5 C4 N4 Co1 -35.7(8) . . . . ? C17 C16 N4 C4 152.9(8) . . . . ? C17 C16 N4 C10 -80.6(9) . . . . ? C17 C16 N4 Co1 37.6(8) . . . . ? C11 C10 N4 C4 -111.9(8) . . . . ? C11 C10 N4 C16 120.9(8) . . . . ? C11 C10 N4 Co1 6.2(8) . . . . ? O1 C1 N5 O2 1.9(11) . . . . ? C2 C1 N5 O2 -177.7(8) . . . . ? N5 C1 O1 Co1 0.1(9) . . . . ? C2 C1 O1 Co1 179.7(7) . . . . ? C1 N5 O2 Co1 -2.7(8) . . . . ? O12 Cl2 O12 O13 -82.1(12) 2 . . 2 ? O13 Cl2 O12 O13 -158.2(18) . . . 2 ? O11 Cl2 O12 O13 97.9(12) . . . 2 ? O12 Cl2 O13 O12 131(3) . . . 2 ? O13 Cl2 O13 O12 66.7(17) 2 . . 2 ? O11 Cl2 O13 O12 -113.3(17) . . . 2 ? C1 O1 Co1 O2 -1.3(5) . . . . ? C1 O1 Co1 N2 179.6(5) . . . . ? C1 O1 Co1 N3 87.9(5) . . . . ? C1 O1 Co1 N1 -89.7(5) . . . . ? C1 O1 Co1 N4 10(5) . . . . ? N5 O2 Co1 O1 2.1(4) . . . . ? N5 O2 Co1 N2 158(6) . . . . ? N5 O2 Co1 N3 -92.0(5) . . . . ? N5 O2 Co1 N1 97.6(5) . . . . ? N5 O2 Co1 N4 -177.4(5) . . . . ? C15 N2 Co1 O1 2.2(6) . . . . ? C11 N2 Co1 O1 -179.6(5) . . . . ? C15 N2 Co1 O2 -153(6) . . . . ? C11 N2 Co1 O2 25(6) . . . . ? C15 N2 Co1 N3 96.4(7) . . . . ? C11 N2 Co1 N3 -85.4(6) . . . . ? C15 N2 Co1 N1 -93.2(6) . . . . ? C11 N2 Co1 N1 84.9(5) . . . . ? C15 N2 Co1 N4 -178.3(6) . . . . ? C11 N2 Co1 N4 -0.1(5) . . . . ? C21 N3 Co1 O1 20.7(8) . . . . ? C17 N3 Co1 O1 -158.6(6) . . . . ? C21 N3 Co1 O2 106.9(8) . . . . ? C17 N3 Co1 O2 -72.5(6) . . . . ? C21 N3 Co1 N2 -75.3(8) . . . . ? C17 N3 Co1 N2 105.4(6) . . . . ? C21 N3 Co1 N1 -173.8(12) . . . . ? C17 N3 Co1 N1 6.8(18) . . . . ? C21 N3 Co1 N4 -162.2(8) . . . . ? C17 N3 Co1 N4 18.5(6) . . . . ? C5 N1 Co1 O1 163.0(5) . . . . ? C9 N1 Co1 O1 -18.4(6) . . . . ? C5 N1 Co1 O2 76.9(5) . . . . ? C9 N1 Co1 O2 -104.5(6) . . . . ? C5 N1 Co1 N2 -101.1(6) . . . . ? C9 N1 Co1 N2 77.5(6) . . . . ? C5 N1 Co1 N3 -2.4(17) . . . . ? C9 N1 Co1 N3 176.2(13) . . . . ? C5 N1 Co1 N4 -14.1(5) . . . . ? C9 N1 Co1 N4 164.5(6) . . . . ? C4 N4 Co1 O1 -72(5) . . . . ? C16 N4 Co1 O1 48(5) . . . . ? C10 N4 Co1 O1 167(5) . . . . ? C4 N4 Co1 O2 -60.9(5) . . . . ? C16 N4 Co1 O2 59.0(6) . . . . ? C10 N4 Co1 O2 177.5(5) . . . . ? C4 N4 Co1 N2 118.1(5) . . . . ? C16 N4 Co1 N2 -122.0(6) . . . . ? C10 N4 Co1 N2 -3.5(5) . . . . ? C4 N4 Co1 N3 -150.3(6) . . . . ? C16 N4 Co1 N3 -30.4(6) . . . . ? C10 N4 Co1 N3 88.1(5) . . . . ? C4 N4 Co1 N1 27.7(5) . . . . ? C16 N4 Co1 N1 147.6(6) . . . . ? C10 N4 Co1 N1 -93.9(5) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 28.39 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.669 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.101 data_twf35 _database_code_depnum_ccdc_archive 'CCDC 282775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(bha-H)tpa]Cl' _chemical_formula_sum 'C25 H35 Cl Co N5 O8' _chemical_formula_weight 627.96 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)/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 15.043(2) _cell_length_b 13.3573(17) _cell_length_c 14.6063(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.440(2) _cell_angle_gamma 90.00 _cell_volume 2854.6(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 0.749 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26969 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0167 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.27 _reflns_number_total 6733 _reflns_number_gt 6062 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.1033P)^2^+4.2383P] 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 6733 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1718 _refine_ls_wR_factor_gt 0.1661 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.39795(18) 0.09896(18) 0.13010(19) 0.0265(5) Uani 1 1 d . . . H1 H 0.4550 0.0857 0.1691 0.032 Uiso 1 1 calc R . . C2 C 0.3893(2) 0.1087(2) 0.0335(2) 0.0323(6) Uani 1 1 d . . . H2 H 0.4405 0.1034 0.0082 0.039 Uiso 1 1 calc R . . C3 C 0.3041(2) 0.1265(2) -0.0246(2) 0.0335(6) Uani 1 1 d . . . H3 H 0.2973 0.1329 -0.0892 0.040 Uiso 1 1 calc R . . C4 C 0.22875(19) 0.1345(2) 0.01488(18) 0.0298(5) Uani 1 1 d . . . H4 H 0.1706 0.1447 -0.0230 0.036 Uiso 1 1 calc R . . C5 C 0.24173(18) 0.12710(19) 0.11160(18) 0.0254(5) Uani 1 1 d . . . C6 C 0.16723(17) 0.1450(2) 0.16271(17) 0.0271(5) Uani 1 1 d . . . H6A H 0.1615 0.2161 0.1738 0.033 Uiso 1 1 calc R . . H6B H 0.1093 0.1209 0.1254 0.033 Uiso 1 1 calc R . . C7 C 0.4055(2) -0.0913(2) 0.3402(2) 0.0319(6) Uani 1 1 d . . . H7 H 0.4613 -0.0582 0.3580 0.038 Uiso 1 1 calc R . . C8 C 0.4032(2) -0.1939(2) 0.3489(2) 0.0409(7) Uani 1 1 d . . . H8 H 0.4567 -0.2297 0.3722 0.049 Uiso 1 1 calc R . . C9 C 0.3205(3) -0.2428(2) 0.3227(2) 0.0459(8) Uani 1 1 d . . . H9 H 0.3176 -0.3120 0.3284 0.055 Uiso 1 1 calc R . . C10 C 0.2420(2) -0.1884(2) 0.2880(2) 0.0408(7) Uani 1 1 d . . . H10 H 0.1857 -0.2203 0.2699 0.049 Uiso 1 1 calc R . . C11 C 0.24862(19) -0.0847(2) 0.28045(18) 0.0291(5) Uani 1 1 d . . . C12 C 0.16866(19) -0.0187(2) 0.2403(2) 0.0344(6) Uani 1 1 d . . . H12A H 0.1191 -0.0345 0.2701 0.041 Uiso 1 1 calc R . . H12B H 0.1477 -0.0322 0.1735 0.041 Uiso 1 1 calc R . . C13 C 0.3632(2) 0.11000(19) 0.50505(19) 0.0301(6) Uani 1 1 d . . . H13 H 0.4248 0.1057 0.5045 0.036 Uiso 1 1 calc R . . C14 C 0.3383(2) 0.1135(2) 0.5903(2) 0.0374(7) Uani 1 1 d . . . H14 H 0.3826 0.1137 0.6465 0.045 Uiso 1 1 calc R . . C15 C 0.2469(2) 0.1167(2) 0.5911(2) 0.0380(7) Uani 1 1 d . . . H15 H 0.2289 0.1170 0.6478 0.046 Uiso 1 1 calc R . . C16 C 0.1818(2) 0.1196(2) 0.5062(2) 0.0345(6) Uani 1 1 d . . . H16 H 0.1198 0.1213 0.5052 0.041 Uiso 1 1 calc R . . C17 C 0.21102(19) 0.1198(2) 0.42307(19) 0.0284(5) Uani 1 1 d . . . C18 C 0.14918(18) 0.1363(2) 0.32695(18) 0.0316(6) Uani 1 1 d . . . H18A H 0.0900 0.1060 0.3241 0.038 Uiso 1 1 calc R . . H18B H 0.1403 0.2074 0.3149 0.038 Uiso 1 1 calc R . . C19 C 0.47086(16) 0.21646(18) 0.34673(16) 0.0225(4) Uani 1 1 d . . . C20 C 0.56867(16) 0.24030(19) 0.38423(16) 0.0240(5) Uani 1 1 d . . . C21 C 0.60006(18) 0.3378(2) 0.4053(2) 0.0308(5) Uani 1 1 d . . . H21 H 0.5590 0.3909 0.3945 0.037 Uiso 1 1 calc R . . C22 C 0.6926(2) 0.3557(2) 0.4425(2) 0.0370(6) Uani 1 1 d . . . H22 H 0.7131 0.4209 0.4562 0.044 Uiso 1 1 calc R . . C23 C 0.75421(19) 0.2769(2) 0.4591(2) 0.0392(7) Uani 1 1 d . . . H23 H 0.8160 0.2891 0.4839 0.047 Uiso 1 1 calc R . . C24 C 0.7236(2) 0.1802(2) 0.4387(3) 0.0411(7) Uani 1 1 d . . . H24 H 0.7648 0.1272 0.4499 0.049 Uiso 1 1 calc R . . C25 C 0.63134(19) 0.1618(2) 0.4015(2) 0.0338(6) Uani 1 1 d . . . H25 H 0.6112 0.0964 0.3880 0.041 Uiso 1 1 calc R . . N1 N 0.32467(15) 0.10844(14) 0.16763(15) 0.0229(4) Uani 1 1 d . . . N2 N 0.32934(14) -0.03795(17) 0.30650(14) 0.0249(4) Uani 1 1 d . . . N3 N 0.30027(16) 0.11269(15) 0.42262(15) 0.0249(4) Uani 1 1 d . . . N4 N 0.19196(14) 0.09005(17) 0.25436(15) 0.0245(4) Uani 1 1 d . . . N5 N 0.40976(14) 0.28584(16) 0.32202(14) 0.0238(4) Uani 1 1 d . . . O1 O 0.32071(11) 0.24700(13) 0.29281(11) 0.0235(4) Uani 1 1 d . . . O2 O 0.44945(12) 0.12006(13) 0.34159(13) 0.0251(4) Uani 1 1 d . . . O1W O 0.9375(2) 0.1167(3) 0.4110(3) 0.0906(12) Uani 1 1 d . . . O2W O 0.0010(7) -0.1943(6) 0.1267(6) 0.058(2) Uani 0.50 1 d P . . O3W O 0.1849(2) 0.5419(3) 0.2596(3) 0.0836(10) Uani 1 1 d . . . O4W O -0.0645(3) 0.1346(4) 0.1504(3) 0.1011(13) Uani 1 1 d . . . O5W O 0.0096(3) 0.3575(3) 0.1608(4) 0.0453(11) Uani 0.50 1 d P . . O6W O 0.0847(4) 0.3669(4) 0.2494(5) 0.0608(15) Uani 0.50 1 d P . . O7W O -0.0460(3) 0.3925(8) 0.0919(4) 0.238(6) Uani 1 1 d . . . O8W O 0.0081(6) -0.1755(9) 0.0926(10) 0.131(6) Uani 0.50 1 d P . . Cl1 Cl 0.0000 0.0000 0.0000 0.0963(7) Uani 1 2 d S . . Cl2 Cl 0.38705(15) 0.50094(15) 0.30808(16) 0.0618(5) Uani 0.50 1 d P . . Co1 Co 0.32377(2) 0.10685(2) 0.29888(2) 0.02058(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0269(12) 0.0240(11) 0.0303(13) -0.0011(9) 0.0098(10) -0.0005(9) C2 0.0366(15) 0.0304(13) 0.0344(14) -0.0018(10) 0.0171(12) -0.0019(10) C3 0.0448(16) 0.0335(13) 0.0246(12) 0.0007(10) 0.0128(11) -0.0016(12) C4 0.0339(13) 0.0316(13) 0.0231(12) 0.0006(10) 0.0051(10) 0.0000(10) C5 0.0263(12) 0.0262(11) 0.0228(11) -0.0005(9) 0.0041(9) -0.0009(9) C6 0.0227(11) 0.0368(13) 0.0204(11) 0.0007(10) 0.0020(9) 0.0021(10) C7 0.0369(14) 0.0280(13) 0.0296(13) -0.0005(10) 0.0055(11) 0.0037(11) C8 0.0524(18) 0.0280(13) 0.0410(16) 0.0008(12) 0.0083(13) 0.0090(12) C9 0.067(2) 0.0239(13) 0.0470(17) -0.0011(12) 0.0141(16) -0.0019(13) C10 0.0511(18) 0.0305(14) 0.0421(16) -0.0046(12) 0.0133(14) -0.0117(13) C11 0.0362(14) 0.0288(12) 0.0233(11) -0.0025(10) 0.0088(10) -0.0072(10) C12 0.0284(13) 0.0344(14) 0.0387(15) -0.0016(11) 0.0044(11) -0.0098(11) C13 0.0337(14) 0.0323(13) 0.0216(12) 0.0006(9) 0.0011(10) 0.0055(10) C14 0.0487(18) 0.0391(15) 0.0219(13) 0.0014(10) 0.0031(12) 0.0086(12) C15 0.0543(19) 0.0386(15) 0.0240(13) 0.0033(10) 0.0149(13) 0.0084(13) C16 0.0384(15) 0.0395(15) 0.0285(13) 0.0001(11) 0.0141(12) 0.0020(11) C17 0.0304(13) 0.0310(12) 0.0240(12) -0.0005(9) 0.0068(10) -0.0001(10) C18 0.0238(12) 0.0482(16) 0.0234(12) -0.0022(11) 0.0066(10) 0.0029(11) C19 0.0229(11) 0.0253(11) 0.0195(10) -0.0014(8) 0.0051(8) -0.0002(9) C20 0.0221(11) 0.0281(12) 0.0216(10) -0.0005(9) 0.0048(8) -0.0009(9) C21 0.0266(12) 0.0276(12) 0.0375(14) 0.0020(10) 0.0060(10) -0.0016(10) C22 0.0287(13) 0.0346(14) 0.0458(16) 0.0008(12) 0.0045(12) -0.0078(11) C23 0.0229(12) 0.0460(17) 0.0461(16) -0.0028(13) 0.0026(11) -0.0038(11) C24 0.0252(13) 0.0402(16) 0.0552(19) -0.0038(13) 0.0036(12) 0.0064(11) C25 0.0260(12) 0.0301(13) 0.0436(15) -0.0068(11) 0.0045(11) 0.0009(10) N1 0.0242(10) 0.0222(10) 0.0225(10) -0.0012(7) 0.0058(8) 0.0002(7) N2 0.0282(11) 0.0265(11) 0.0200(9) -0.0007(7) 0.0055(8) -0.0002(8) N3 0.0292(11) 0.0249(10) 0.0199(10) -0.0004(7) 0.0039(8) 0.0007(8) N4 0.0215(10) 0.0322(11) 0.0197(9) -0.0005(8) 0.0046(8) -0.0009(8) N5 0.0215(9) 0.0254(10) 0.0237(10) -0.0013(8) 0.0039(7) 0.0001(8) O1 0.0204(8) 0.0244(8) 0.0238(8) -0.0007(6) 0.0014(6) 0.0012(6) O2 0.0203(8) 0.0236(8) 0.0290(9) 0.0001(7) 0.0010(7) 0.0006(6) O1W 0.0522(19) 0.099(3) 0.125(4) -0.002(2) 0.029(2) 0.0113(17) O2W 0.075(5) 0.048(3) 0.053(4) 0.016(3) 0.017(3) -0.016(3) O3W 0.073(2) 0.070(2) 0.113(3) -0.001(2) 0.033(2) 0.0108(17) O4W 0.067(2) 0.130(4) 0.109(3) 0.025(3) 0.025(2) -0.003(2) O5W 0.054(3) 0.041(2) 0.056(3) 0.000(2) 0.046(2) 0.013(2) O6W 0.047(3) 0.047(3) 0.090(4) 0.023(3) 0.020(3) 0.010(2) O7W 0.054(3) 0.570(17) 0.088(4) -0.094(6) 0.011(2) 0.031(5) O8W 0.037(4) 0.145(10) 0.177(12) -0.125(9) -0.040(5) 0.042(5) Cl1 0.1163(16) 0.0846(12) 0.0692(10) -0.0037(9) -0.0166(10) -0.0434(12) Cl2 0.0725(13) 0.0482(10) 0.0661(12) 0.0018(8) 0.0189(10) -0.0029(9) Co1 0.01947(19) 0.0228(2) 0.01856(19) -0.00053(10) 0.00266(13) 0.00049(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.346(3) . ? C1 C2 1.393(4) . ? C2 C3 1.384(4) . ? C3 C4 1.390(4) . ? C4 C5 1.384(4) . ? C5 N1 1.347(3) . ? C5 C6 1.503(3) . ? C6 N4 1.496(3) . ? C7 N2 1.342(4) . ? C7 C8 1.378(4) . ? C8 C9 1.378(5) . ? C9 C10 1.378(5) . ? C10 C11 1.395(4) . ? C11 N2 1.340(3) . ? C11 C12 1.497(4) . ? C12 N4 1.498(3) . ? C13 N3 1.348(3) . ? C13 C14 1.383(4) . ? C14 C15 1.378(5) . ? C15 C16 1.391(4) . ? C16 C17 1.384(4) . ? C17 N3 1.348(4) . ? C17 C18 1.509(4) . ? C18 N4 1.496(3) . ? C19 N5 1.296(3) . ? C19 O2 1.325(3) . ? C19 C20 1.481(3) . ? C20 C25 1.394(4) . ? C20 C21 1.394(4) . ? C21 C22 1.392(4) . ? C22 C23 1.387(4) . ? C23 C24 1.380(4) . ? C24 C25 1.390(4) . ? N1 Co1 1.920(2) . ? N2 Co1 1.938(2) . ? N3 Co1 1.922(2) . ? N4 Co1 1.951(2) . ? N5 O1 1.407(3) . ? O1 Co1 1.8742(18) . ? O2 Co1 1.8564(18) . ? O2W O8W 0.590(19) . ? O5W O7W 1.241(8) . ? O5W O6W 1.512(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 120.8(3) . . ? C3 C2 C1 119.4(3) . . ? C2 C3 C4 119.2(3) . . ? C5 C4 C3 118.9(3) . . ? N1 C5 C4 121.6(2) . . ? N1 C5 C6 114.8(2) . . ? C4 C5 C6 123.4(2) . . ? N4 C6 C5 107.9(2) . . ? N2 C7 C8 121.6(3) . . ? C7 C8 C9 119.1(3) . . ? C8 C9 C10 119.6(3) . . ? C9 C10 C11 118.8(3) . . ? N2 C11 C10 121.1(3) . . ? N2 C11 C12 115.4(2) . . ? C10 C11 C12 123.4(3) . . ? C11 C12 N4 112.1(2) . . ? N3 C13 C14 121.5(3) . . ? C15 C14 C13 119.2(3) . . ? C14 C15 C16 119.4(3) . . ? C17 C16 C15 118.8(3) . . ? N3 C17 C16 121.6(3) . . ? N3 C17 C18 113.9(2) . . ? C16 C17 C18 124.3(3) . . ? N4 C18 C17 109.0(2) . . ? N5 C19 O2 122.1(2) . . ? N5 C19 C20 121.9(2) . . ? O2 C19 C20 116.0(2) . . ? C25 C20 C21 118.9(2) . . ? C25 C20 C19 118.5(2) . . ? C21 C20 C19 122.6(2) . . ? C22 C21 C20 120.2(3) . . ? C23 C22 C21 120.3(3) . . ? C24 C23 C22 119.8(3) . . ? C23 C24 C25 120.2(3) . . ? C24 C25 C20 120.6(3) . . ? C1 N1 C5 120.0(2) . . ? C1 N1 Co1 127.00(19) . . ? C5 N1 Co1 112.84(17) . . ? C11 N2 C7 119.8(3) . . ? C11 N2 Co1 115.14(18) . . ? C7 N2 Co1 124.97(19) . . ? C17 N3 C13 119.4(2) . . ? C17 N3 Co1 114.12(18) . . ? C13 N3 Co1 126.4(2) . . ? C18 N4 C6 111.9(2) . . ? C18 N4 C12 111.9(2) . . ? C6 N4 C12 110.6(2) . . ? C18 N4 Co1 106.72(15) . . ? C6 N4 Co1 105.30(15) . . ? C12 N4 Co1 110.17(17) . . ? C19 N5 O1 112.6(2) . . ? N5 O1 Co1 110.05(13) . . ? C19 O2 Co1 109.06(15) . . ? O7W O5W O6W 153.0(7) . . ? O2 Co1 O1 86.15(7) . . ? O2 Co1 N1 95.25(9) . . ? O1 Co1 N1 86.99(8) . . ? O2 Co1 N3 94.34(9) . . ? O1 Co1 N3 89.77(8) . . ? N1 Co1 N3 169.65(9) . . ? O2 Co1 N2 92.78(8) . . ? O1 Co1 N2 178.90(8) . . ? N1 Co1 N2 93.33(8) . . ? N3 Co1 N2 90.09(8) . . ? O2 Co1 N4 178.84(9) . . ? O1 Co1 N4 95.01(8) . . ? N1 Co1 N4 84.89(9) . . ? N3 Co1 N4 85.60(9) . . ? N2 Co1 N4 86.07(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -1.3(4) . . . . ? C1 C2 C3 C4 0.2(4) . . . . ? C2 C3 C4 C5 1.6(4) . . . . ? C3 C4 C5 N1 -2.6(4) . . . . ? C3 C4 C5 C6 173.5(3) . . . . ? N1 C5 C6 N4 -27.5(3) . . . . ? C4 C5 C6 N4 156.1(2) . . . . ? N2 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 0.3(5) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C9 C10 C11 N2 -0.2(4) . . . . ? C9 C10 C11 C12 177.5(3) . . . . ? N2 C11 C12 N4 -11.1(3) . . . . ? C10 C11 C12 N4 171.0(3) . . . . ? N3 C13 C14 C15 2.0(4) . . . . ? C13 C14 C15 C16 -2.0(4) . . . . ? C14 C15 C16 C17 -0.5(4) . . . . ? C15 C16 C17 N3 3.1(4) . . . . ? C15 C16 C17 C18 -171.7(3) . . . . ? N3 C17 C18 N4 28.7(3) . . . . ? C16 C17 C18 N4 -156.1(3) . . . . ? N5 C19 C20 C25 -174.5(2) . . . . ? O2 C19 C20 C25 6.7(3) . . . . ? N5 C19 C20 C21 7.4(4) . . . . ? O2 C19 C20 C21 -171.5(2) . . . . ? C25 C20 C21 C22 0.4(4) . . . . ? C19 C20 C21 C22 178.5(3) . . . . ? C20 C21 C22 C23 -0.2(5) . . . . ? C21 C22 C23 C24 -0.1(5) . . . . ? C22 C23 C24 C25 0.1(5) . . . . ? C23 C24 C25 C20 0.0(5) . . . . ? C21 C20 C25 C24 -0.3(4) . . . . ? C19 C20 C25 C24 -178.5(3) . . . . ? C2 C1 N1 C5 0.3(4) . . . . ? C2 C1 N1 Co1 -175.34(18) . . . . ? C4 C5 N1 C1 1.6(4) . . . . ? C6 C5 N1 C1 -174.8(2) . . . . ? C4 C5 N1 Co1 177.9(2) . . . . ? C6 C5 N1 Co1 1.4(3) . . . . ? C10 C11 N2 C7 0.3(4) . . . . ? C12 C11 N2 C7 -177.6(2) . . . . ? C10 C11 N2 Co1 -176.0(2) . . . . ? C12 C11 N2 Co1 6.1(3) . . . . ? C8 C7 N2 C11 -0.1(4) . . . . ? C8 C7 N2 Co1 175.8(2) . . . . ? C16 C17 N3 C13 -3.2(4) . . . . ? C18 C17 N3 C13 172.1(2) . . . . ? C16 C17 N3 Co1 176.6(2) . . . . ? C18 C17 N3 Co1 -8.1(3) . . . . ? C14 C13 N3 C17 0.6(4) . . . . ? C14 C13 N3 Co1 -179.2(2) . . . . ? C17 C18 N4 C6 -149.2(2) . . . . ? C17 C18 N4 C12 86.0(3) . . . . ? C17 C18 N4 Co1 -34.5(3) . . . . ? C5 C6 N4 C18 154.5(2) . . . . ? C5 C6 N4 C12 -80.1(3) . . . . ? C5 C6 N4 Co1 38.9(2) . . . . ? C11 C12 N4 C18 -107.9(3) . . . . ? C11 C12 N4 C6 126.6(2) . . . . ? C11 C12 N4 Co1 10.6(3) . . . . ? O2 C19 N5 O1 1.7(3) . . . . ? C20 C19 N5 O1 -177.02(19) . . . . ? C19 N5 O1 Co1 -0.8(2) . . . . ? N5 C19 O2 Co1 -1.7(3) . . . . ? C20 C19 O2 Co1 177.14(16) . . . . ? C19 O2 Co1 O1 0.82(16) . . . . ? C19 O2 Co1 N1 87.43(16) . . . . ? C19 O2 Co1 N3 -88.66(16) . . . . ? C19 O2 Co1 N2 -178.96(16) . . . . ? C19 O2 Co1 N4 -176(100) . . . . ? N5 O1 Co1 O2 0.00(14) . . . . ? N5 O1 Co1 N1 -95.47(14) . . . . ? N5 O1 Co1 N3 94.36(15) . . . . ? N5 O1 Co1 N2 12(4) . . . . ? N5 O1 Co1 N4 179.93(14) . . . . ? C1 N1 Co1 O2 12.8(2) . . . . ? C5 N1 Co1 O2 -163.15(17) . . . . ? C1 N1 Co1 O1 98.6(2) . . . . ? C5 N1 Co1 O1 -77.31(17) . . . . ? C1 N1 Co1 N3 170.6(4) . . . . ? C5 N1 Co1 N3 -5.3(6) . . . . ? C1 N1 Co1 N2 -80.3(2) . . . . ? C5 N1 Co1 N2 103.74(18) . . . . ? C1 N1 Co1 N4 -166.1(2) . . . . ? C5 N1 Co1 N4 18.00(17) . . . . ? C17 N3 Co1 O2 170.94(18) . . . . ? C13 N3 Co1 O2 -9.3(2) . . . . ? C17 N3 Co1 O1 84.82(18) . . . . ? C13 N3 Co1 O1 -95.4(2) . . . . ? C17 N3 Co1 N1 13.1(6) . . . . ? C13 N3 Co1 N1 -167.1(4) . . . . ? C17 N3 Co1 N2 -96.27(18) . . . . ? C13 N3 Co1 N2 83.5(2) . . . . ? C17 N3 Co1 N4 -10.22(18) . . . . ? C13 N3 Co1 N4 169.6(2) . . . . ? C11 N2 Co1 O2 -179.92(18) . . . . ? C7 N2 Co1 O2 4.1(2) . . . . ? C11 N2 Co1 O1 169(4) . . . . ? C7 N2 Co1 O1 -7(4) . . . . ? C11 N2 Co1 N1 -84.49(18) . . . . ? C7 N2 Co1 N1 99.5(2) . . . . ? C11 N2 Co1 N3 85.73(18) . . . . ? C7 N2 Co1 N3 -90.3(2) . . . . ? C11 N2 Co1 N4 0.15(18) . . . . ? C7 N2 Co1 N4 -175.9(2) . . . . ? C18 N4 Co1 O2 112(4) . . . . ? C6 N4 Co1 O2 -129(4) . . . . ? C12 N4 Co1 O2 -9(4) . . . . ? C18 N4 Co1 O1 -64.30(18) . . . . ? C6 N4 Co1 O1 54.79(16) . . . . ? C12 N4 Co1 O1 174.07(17) . . . . ? C18 N4 Co1 N1 -150.81(18) . . . . ? C6 N4 Co1 N1 -31.73(16) . . . . ? C12 N4 Co1 N1 87.56(17) . . . . ? C18 N4 Co1 N3 25.09(18) . . . . ? C6 N4 Co1 N3 144.18(17) . . . . ? C12 N4 Co1 N3 -96.54(18) . . . . ? C18 N4 Co1 N2 115.48(18) . . . . ? C6 N4 Co1 N2 -125.43(17) . . . . ? C12 N4 Co1 N2 -6.15(17) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 1.273 _refine_diff_density_min -1.735 _refine_diff_density_rms 0.111 # Attachment '1a.cif' data_twf00 _database_code_depnum_ccdc_archive 'CCDC 282776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[Co(aha-H)tpa]ClO4' _chemical_formula_sum 'C20 H22 Cl Co N5 O6.50' _chemical_formula_weight 530.81 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 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 12.2788(16) _cell_length_b 12.2789(16) _cell_length_c 34.654(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.468(2) _cell_angle_gamma 90.00 _cell_volume 5201.0(12) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rhomb _exptl_crystal_colour blue/green _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21859 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.24 _reflns_number_total 5995 _reflns_number_gt 4928 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART _computing_data_reduction SAINT _computing_structure_solution SHELXS-86 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics WINGX _computing_publication_material ORTEP _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^)+(0.0682P)^2^+10.5456P] 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 ? _refine_ls_extinction_expression ; Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ ; _refine_ls_number_reflns 5995 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0607 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1371 _refine_ls_wR_factor_gt 0.1318 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0207(2) 0.3370(3) 0.65772(11) 0.0467(8) Uani 1 1 d . . . H1 H 0.0425 0.3113 0.6825 0.056 Uiso 1 1 calc R . . C2 C -0.0123(3) 0.4452(3) 0.65283(16) 0.0678(12) Uani 1 1 d . . . H2 H -0.0136 0.4918 0.6739 0.081 Uiso 1 1 calc R . . C3 C -0.0432(3) 0.4810(3) 0.61535(19) 0.0804(16) Uani 1 1 d . . . H3 H -0.0653 0.5528 0.6112 0.096 Uiso 1 1 calc R . . C4 C -0.0415(3) 0.4126(4) 0.58486(15) 0.0695(12) Uani 1 1 d . . . H4 H -0.0619 0.4372 0.5598 0.083 Uiso 1 1 calc R . . C5 C -0.0090(2) 0.3051(3) 0.59118(11) 0.0496(8) Uani 1 1 d . . . C6 C -0.0056(3) 0.2202(3) 0.56047(9) 0.0550(9) Uani 1 1 d . . . H6A H -0.0751 0.1823 0.5568 0.066 Uiso 1 1 calc R . . H6B H 0.0083 0.2538 0.5361 0.066 Uiso 1 1 calc R . . C7 C 0.2833(2) 0.1929(2) 0.66917(9) 0.0368(6) Uani 1 1 d . . . H7 H 0.2555 0.1702 0.6919 0.044 Uiso 1 1 calc R . . C8 C 0.3862(3) 0.2395(3) 0.67101(11) 0.0523(8) Uani 1 1 d . . . H8 H 0.4277 0.2469 0.6947 0.063 Uiso 1 1 calc R . . C9 C 0.4262(3) 0.2744(3) 0.63778(12) 0.0574(10) Uani 1 1 d . . . H9 H 0.4947 0.3072 0.6389 0.069 Uiso 1 1 calc R . . C10 C 0.3653(3) 0.2611(2) 0.60268(11) 0.0486(8) Uani 1 1 d . . . H10 H 0.3920 0.2846 0.5799 0.058 Uiso 1 1 calc R . . C11 C 0.2627(2) 0.2117(2) 0.60200(8) 0.0334(6) Uani 1 1 d . . . C12 C 0.1934(2) 0.1875(3) 0.56548(9) 0.0446(7) Uani 1 1 d . . . H12A H 0.2309 0.1354 0.5504 0.054 Uiso 1 1 calc R . . H12B H 0.1827 0.2537 0.5504 0.054 Uiso 1 1 calc R . . C13 C 0.1862(2) -0.0851(2) 0.64737(9) 0.0346(6) Uani 1 1 d . . . H13 H 0.1944 -0.0620 0.6730 0.042 Uiso 1 1 calc R . . C14 C 0.2266(3) -0.1864(2) 0.63800(12) 0.0501(8) Uani 1 1 d . . . H14 H 0.2608 -0.2312 0.6571 0.060 Uiso 1 1 calc R . . C15 C 0.2151(3) -0.2189(3) 0.59999(13) 0.0591(10) Uani 1 1 d . . . H15 H 0.2413 -0.2866 0.5931 0.071 Uiso 1 1 calc R . . C16 C 0.1650(3) -0.1517(3) 0.57198(11) 0.0545(9) Uani 1 1 d . . . H16 H 0.1575 -0.1730 0.5461 0.065 Uiso 1 1 calc R . . C17 C 0.1256(2) -0.0505(2) 0.58303(9) 0.0388(6) Uani 1 1 d . . . C18 C 0.0658(3) 0.0309(3) 0.55604(8) 0.0463(8) Uani 1 1 d . . . H18A H 0.0934 0.0277 0.5307 0.056 Uiso 1 1 calc R . . H18B H -0.0117 0.0142 0.5530 0.056 Uiso 1 1 calc R . . C19 C -0.1004(2) 0.0499(2) 0.65505(8) 0.0334(6) Uani 1 1 d . . . C20 C -0.2178(2) 0.0110(3) 0.65551(11) 0.0472(8) Uani 1 1 d . . . H20A H -0.2667 0.0715 0.6507 0.071 Uiso 1 1 calc R . . H20B H -0.2275 -0.0200 0.6804 0.071 Uiso 1 1 calc R . . H20C H -0.2332 -0.0431 0.6357 0.071 Uiso 1 1 calc R . . N1 N 0.02175(18) 0.26955(19) 0.62756(7) 0.0362(5) Uani 1 1 d . . . N2 N 0.22282(17) 0.17993(17) 0.63506(7) 0.0296(5) Uani 1 1 d . . . N3 N 0.13572(17) -0.02005(18) 0.62040(6) 0.0303(5) Uani 1 1 d . . . N4 N 0.08378(18) 0.1420(2) 0.57307(7) 0.0366(5) Uani 1 1 d . . . N5 N -0.04022(19) 0.0620(2) 0.68722(7) 0.0378(5) Uani 1 1 d . . . O1 O 0.06649(15) 0.10163(15) 0.68120(5) 0.0333(4) Uani 1 1 d . . . O2 O -0.06638(14) 0.06973(16) 0.62121(5) 0.0335(4) Uani 1 1 d . . . O1W O 0.0000 0.9106(5) 0.7500 0.190(6) Uani 1 2 d S . . O3 O 0.1529(3) 0.4501(4) 0.49553(13) 0.143(2) Uani 1 1 d . . . O4 O 0.3195(3) 0.4294(4) 0.52818(10) 0.0935(11) Uani 1 1 d . . . O5 O 0.1761(3) 0.4897(5) 0.55990(11) 0.1282(17) Uani 1 1 d . . . O6 O 0.2561(6) 0.6003(4) 0.51918(17) 0.179(3) Uani 1 1 d . . . Cl1 Cl 0.21977(7) 0.49874(8) 0.52511(2) 0.0540(2) Uani 1 1 d . . . Co1 Co 0.07744(3) 0.12297(3) 0.628642(9) 0.02595(12) Uani 1 1 d . . . H1W H 0.064(3) 0.945(3) 0.7551(12) 0.049(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0310(14) 0.0370(15) 0.073(2) -0.0091(15) 0.0115(14) -0.0012(12) C2 0.0383(18) 0.0383(18) 0.128(4) -0.013(2) 0.015(2) 0.0045(14) C3 0.042(2) 0.045(2) 0.156(5) 0.027(3) 0.017(2) 0.0134(16) C4 0.0400(19) 0.062(2) 0.106(4) 0.039(2) 0.006(2) 0.0105(17) C5 0.0310(14) 0.0535(19) 0.066(2) 0.0222(16) 0.0114(14) 0.0064(13) C6 0.0421(17) 0.084(3) 0.0389(17) 0.0218(17) 0.0012(13) 0.0078(17) C7 0.0324(14) 0.0310(13) 0.0461(16) -0.0045(12) -0.0020(11) -0.0036(11) C8 0.0353(16) 0.0457(18) 0.074(2) -0.0142(16) -0.0064(15) -0.0084(13) C9 0.0327(16) 0.0467(19) 0.093(3) -0.0089(18) 0.0070(17) -0.0167(14) C10 0.0391(16) 0.0359(15) 0.074(2) 0.0005(15) 0.0234(16) -0.0084(13) C11 0.0282(13) 0.0254(12) 0.0481(16) 0.0012(11) 0.0105(11) 0.0015(10) C12 0.0400(16) 0.0556(19) 0.0406(16) 0.0075(14) 0.0166(13) -0.0079(14) C13 0.0304(13) 0.0297(13) 0.0443(15) 0.0013(11) 0.0060(11) -0.0041(10) C14 0.0422(17) 0.0308(15) 0.080(2) 0.0022(15) 0.0189(16) 0.0003(13) C15 0.059(2) 0.0340(16) 0.090(3) -0.0153(18) 0.033(2) -0.0033(15) C16 0.054(2) 0.054(2) 0.060(2) -0.0291(17) 0.0300(17) -0.0165(16) C17 0.0340(14) 0.0440(16) 0.0407(15) -0.0138(12) 0.0157(12) -0.0134(12) C18 0.0416(16) 0.072(2) 0.0266(14) -0.0125(14) 0.0072(12) -0.0149(15) C19 0.0292(13) 0.0293(13) 0.0438(15) 0.0021(11) 0.0145(11) 0.0007(10) C20 0.0338(15) 0.0438(17) 0.067(2) 0.0036(15) 0.0223(14) -0.0038(13) N1 0.0245(11) 0.0337(12) 0.0512(14) 0.0040(10) 0.0077(10) 0.0020(9) N2 0.0242(10) 0.0239(10) 0.0409(12) -0.0008(9) 0.0047(9) -0.0002(8) N3 0.0249(10) 0.0312(11) 0.0360(12) -0.0064(9) 0.0091(9) -0.0072(8) N4 0.0296(11) 0.0512(14) 0.0293(11) 0.0048(10) 0.0051(9) -0.0036(10) N5 0.0395(13) 0.0389(13) 0.0379(13) 0.0000(10) 0.0189(10) -0.0036(10) O1 0.0358(10) 0.0364(10) 0.0281(9) -0.0034(7) 0.0057(7) -0.0040(8) O2 0.0243(9) 0.0430(11) 0.0339(10) 0.0002(8) 0.0058(7) -0.0048(8) O1W 0.461(19) 0.048(3) 0.053(3) 0.000 -0.016(6) 0.000 O3 0.110(3) 0.179(4) 0.124(3) -0.089(3) -0.071(3) 0.065(3) O4 0.0639(19) 0.136(3) 0.079(2) 0.000(2) -0.0020(16) 0.009(2) O5 0.102(3) 0.221(5) 0.069(2) -0.001(3) 0.050(2) -0.017(3) O6 0.282(8) 0.096(3) 0.170(5) 0.032(3) 0.076(5) -0.052(4) Cl1 0.0513(5) 0.0782(6) 0.0334(4) 0.0003(4) 0.0080(3) -0.0200(4) Co1 0.02361(18) 0.02881(19) 0.02591(18) -0.00049(13) 0.00478(12) -0.00197(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 C1 N1 1.334(4) . ? C1 C2 1.395(5) . ? C2 C3 1.389(7) . ? C3 C4 1.352(7) . ? C4 C5 1.390(5) . ? C5 N1 1.354(4) . ? C5 C6 1.493(5) . ? C6 N4 1.492(4) . ? C7 N2 1.344(4) . ? C7 C8 1.382(4) . ? C8 C9 1.364(5) . ? C9 C10 1.375(5) . ? C10 C11 1.397(4) . ? C11 N2 1.346(3) . ? C11 C12 1.486(4) . ? C12 N4 1.504(4) . ? C13 N3 1.336(4) . ? C13 C14 1.389(4) . ? C14 C15 1.371(5) . ? C15 C16 1.375(6) . ? C16 C17 1.400(4) . ? C17 N3 1.342(4) . ? C17 C18 1.510(5) . ? C18 N4 1.495(4) . ? C19 N5 1.286(4) . ? C19 O2 1.305(3) . ? C19 C20 1.519(4) . ? N1 Co1 1.924(2) . ? N2 Co1 1.910(2) . ? N3 Co1 1.928(2) . ? N4 Co1 1.949(2) . ? N5 O1 1.431(3) . ? O1 Co1 1.8575(19) . ? O2 Co1 1.8778(18) . ? O3 Cl1 1.386(3) . ? O4 Cl1 1.487(4) . ? O5 Cl1 1.370(3) . ? O6 Cl1 1.347(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.4(4) . . ? C3 C2 C1 117.7(4) . . ? C4 C3 C2 120.7(4) . . ? C3 C4 C5 119.5(4) . . ? N1 C5 C4 120.2(4) . . ? N1 C5 C6 114.5(3) . . ? C4 C5 C6 125.3(4) . . ? N4 C6 C5 108.1(3) . . ? N2 C7 C8 121.0(3) . . ? C9 C8 C7 119.5(3) . . ? C8 C9 C10 120.0(3) . . ? C9 C10 C11 118.7(3) . . ? N2 C11 C10 120.8(3) . . ? N2 C11 C12 116.2(2) . . ? C10 C11 C12 122.9(3) . . ? C11 C12 N4 112.0(2) . . ? N3 C13 C14 121.6(3) . . ? C15 C14 C13 118.6(3) . . ? C14 C15 C16 120.1(3) . . ? C15 C16 C17 118.9(3) . . ? N3 C17 C16 120.6(3) . . ? N3 C17 C18 114.1(3) . . ? C16 C17 C18 125.3(3) . . ? N4 C18 C17 108.4(2) . . ? N5 C19 O2 123.4(2) . . ? N5 C19 C20 119.7(3) . . ? O2 C19 C20 117.0(3) . . ? C1 N1 C5 120.4(3) . . ? C1 N1 Co1 126.5(2) . . ? C5 N1 Co1 112.8(2) . . ? C7 N2 C11 119.9(2) . . ? C7 N2 Co1 125.29(19) . . ? C11 N2 Co1 114.74(18) . . ? C13 N3 C17 120.2(3) . . ? C13 N3 Co1 126.51(19) . . ? C17 N3 Co1 113.3(2) . . ? C6 N4 C18 113.3(3) . . ? C6 N4 C12 110.8(3) . . ? C18 N4 C12 111.8(2) . . ? C6 N4 Co1 105.61(18) . . ? C18 N4 Co1 105.22(18) . . ? C12 N4 Co1 109.76(18) . . ? C19 N5 O1 111.8(2) . . ? N5 O1 Co1 110.10(15) . . ? C19 O2 Co1 108.63(17) . . ? O6 Cl1 O5 111.9(3) . . ? O6 Cl1 O3 117.9(4) . . ? O5 Cl1 O3 111.2(3) . . ? O6 Cl1 O4 105.0(4) . . ? O5 Cl1 O4 106.2(3) . . ? O3 Cl1 O4 103.4(2) . . ? O1 Co1 O2 86.01(8) . . ? O1 Co1 N2 95.26(9) . . ? O2 Co1 N2 178.41(9) . . ? O1 Co1 N1 95.29(10) . . ? O2 Co1 N1 89.72(9) . . ? N2 Co1 N1 89.21(9) . . ? O1 Co1 N3 94.55(9) . . ? O2 Co1 N3 91.15(9) . . ? N2 Co1 N3 89.70(9) . . ? N1 Co1 N3 170.16(10) . . ? O1 Co1 N4 177.77(9) . . ? O2 Co1 N4 91.82(9) . . ? N2 Co1 N4 86.92(10) . . ? N1 Co1 N4 85.20(11) . . ? N3 Co1 N4 84.98(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.7(5) . . . . ? C1 C2 C3 C4 0.3(6) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C3 C4 C5 N1 -0.7(5) . . . . ? C3 C4 C5 C6 178.6(3) . . . . ? N1 C5 C6 N4 -31.0(4) . . . . ? C4 C5 C6 N4 149.7(3) . . . . ? N2 C7 C8 C9 1.0(5) . . . . ? C7 C8 C9 C10 -1.3(5) . . . . ? C8 C9 C10 C11 0.1(5) . . . . ? C9 C10 C11 N2 1.5(4) . . . . ? C9 C10 C11 C12 -176.2(3) . . . . ? N2 C11 C12 N4 6.5(4) . . . . ? C10 C11 C12 N4 -175.7(3) . . . . ? N3 C13 C14 C15 0.7(4) . . . . ? C13 C14 C15 C16 0.4(5) . . . . ? C14 C15 C16 C17 -0.5(5) . . . . ? C15 C16 C17 N3 -0.5(4) . . . . ? C15 C16 C17 C18 -178.0(3) . . . . ? N3 C17 C18 N4 28.7(3) . . . . ? C16 C17 C18 N4 -153.7(3) . . . . ? C2 C1 N1 C5 0.4(4) . . . . ? C2 C1 N1 Co1 173.8(2) . . . . ? C4 C5 N1 C1 0.3(4) . . . . ? C6 C5 N1 C1 -179.0(3) . . . . ? C4 C5 N1 Co1 -174.0(2) . . . . ? C6 C5 N1 Co1 6.7(3) . . . . ? C8 C7 N2 C11 0.5(4) . . . . ? C8 C7 N2 Co1 -177.1(2) . . . . ? C10 C11 N2 C7 -1.8(4) . . . . ? C12 C11 N2 C7 176.0(3) . . . . ? C10 C11 N2 Co1 176.0(2) . . . . ? C12 C11 N2 Co1 -6.1(3) . . . . ? C14 C13 N3 C17 -1.8(4) . . . . ? C14 C13 N3 Co1 -179.0(2) . . . . ? C16 C17 N3 C13 1.7(4) . . . . ? C18 C17 N3 C13 179.4(2) . . . . ? C16 C17 N3 Co1 179.2(2) . . . . ? C18 C17 N3 Co1 -3.0(3) . . . . ? C5 C6 N4 C18 153.7(3) . . . . ? C5 C6 N4 C12 -79.7(3) . . . . ? C5 C6 N4 Co1 39.1(3) . . . . ? C17 C18 N4 C6 -153.9(2) . . . . ? C17 C18 N4 C12 80.0(3) . . . . ? C17 C18 N4 Co1 -39.1(2) . . . . ? C11 C12 N4 C6 112.6(3) . . . . ? C11 C12 N4 C18 -120.0(3) . . . . ? C11 C12 N4 Co1 -3.7(3) . . . . ? O2 C19 N5 O1 1.2(4) . . . . ? C20 C19 N5 O1 -178.6(2) . . . . ? C19 N5 O1 Co1 0.9(3) . . . . ? N5 C19 O2 Co1 -2.6(3) . . . . ? C20 C19 O2 Co1 177.2(2) . . . . ? N5 O1 Co1 O2 -1.78(15) . . . . ? N5 O1 Co1 N2 177.26(15) . . . . ? N5 O1 Co1 N1 87.57(16) . . . . ? N5 O1 Co1 N3 -92.62(16) . . . . ? N5 O1 Co1 N4 -15(3) . . . . ? C19 O2 Co1 O1 2.31(17) . . . . ? C19 O2 Co1 N2 -141(3) . . . . ? C19 O2 Co1 N1 -93.01(18) . . . . ? C19 O2 Co1 N3 96.79(18) . . . . ? C19 O2 Co1 N4 -178.20(18) . . . . ? C7 N2 Co1 O1 0.4(2) . . . . ? C11 N2 Co1 O1 -177.35(18) . . . . ? C7 N2 Co1 O2 143(3) . . . . ? C11 N2 Co1 O2 -34(3) . . . . ? C7 N2 Co1 N1 95.6(2) . . . . ? C11 N2 Co1 N1 -82.11(19) . . . . ? C7 N2 Co1 N3 -94.2(2) . . . . ? C11 N2 Co1 N3 88.11(18) . . . . ? C7 N2 Co1 N4 -179.2(2) . . . . ? C11 N2 Co1 N4 3.12(18) . . . . ? C1 N1 Co1 O1 22.0(2) . . . . ? C5 N1 Co1 O1 -164.2(2) . . . . ? C1 N1 Co1 O2 107.9(2) . . . . ? C5 N1 Co1 O2 -78.2(2) . . . . ? C1 N1 Co1 N2 -73.2(2) . . . . ? C5 N1 Co1 N2 100.6(2) . . . . ? C1 N1 Co1 N3 -156.9(5) . . . . ? C5 N1 Co1 N3 16.9(6) . . . . ? C1 N1 Co1 N4 -160.2(2) . . . . ? C5 N1 Co1 N4 13.7(2) . . . . ? C13 N3 Co1 O1 -21.5(2) . . . . ? C17 N3 Co1 O1 161.15(18) . . . . ? C13 N3 Co1 O2 -107.6(2) . . . . ? C17 N3 Co1 O2 75.06(18) . . . . ? C13 N3 Co1 N2 73.7(2) . . . . ? C17 N3 Co1 N2 -103.60(18) . . . . ? C13 N3 Co1 N1 157.4(5) . . . . ? C17 N3 Co1 N1 -19.9(6) . . . . ? C13 N3 Co1 N4 160.7(2) . . . . ? C17 N3 Co1 N4 -16.66(18) . . . . ? C6 N4 Co1 O1 73(3) . . . . ? C18 N4 Co1 O1 -47(3) . . . . ? C12 N4 Co1 O1 -167(2) . . . . ? C6 N4 Co1 O2 60.1(2) . . . . ? C18 N4 Co1 O2 -60.04(18) . . . . ? C12 N4 Co1 O2 179.6(2) . . . . ? C6 N4 Co1 N2 -119.0(2) . . . . ? C18 N4 Co1 N2 120.93(18) . . . . ? C12 N4 Co1 N2 0.5(2) . . . . ? C6 N4 Co1 N1 -29.5(2) . . . . ? C18 N4 Co1 N1 -149.61(18) . . . . ? C12 N4 Co1 N1 90.0(2) . . . . ? C6 N4 Co1 N3 151.1(2) . . . . ? C18 N4 Co1 N3 30.95(18) . . . . ? C12 N4 Co1 N3 -89.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 0.714 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.076