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 'Fenton Heirtzler' _publ_contact_author_address ; Department of Chemistry University of Alberta 11227 Saskatchewan Drive Edmonton Alberta T6G 2G2 CANADA ; _publ_contact_author_email FENTONH@UALBERTA.CA _publ_section_title ; Formation of a solubilized cobalt block oligomer from a ML2-type double helicate ; loop_ _publ_author_name 'Fenton Heirtzler' 'Kevin Howland' 'Saverio Santi' 'Thomas Weyhermuller' # Attachment '4474.CIF' data_ST4474 _database_code_depnum_ccdc_archive 'CCDC 229005' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[C52 H40 Co2 N14]4+, 4 (Cl O4)-, 4 MeCN' _chemical_formula_sum 'C60 H52 Cl4 Co2 N18 O16' _chemical_formula_weight 1540.86 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 18.5148(6) _cell_length_b 16.7629(6) _cell_length_c 21.3319(8) _cell_angle_alpha 90.00 _cell_angle_beta 94.460(10) _cell_angle_gamma 90.00 _cell_volume 6600.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3152 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type 'Gaussian, face-indexed' _exptl_absorpt_correction_T_min 0.7064 _exptl_absorpt_correction_T_max 0.8773 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '763 images at 1.0 deg. in \w, 50 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65778 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 30.97 _reflns_number_total 10473 _reflns_number_gt 9436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+7.5945P] 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 10473 _refine_ls_number_parameters 481 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0793 _refine_ls_wR_factor_gt 0.0765 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 2.027 _refine_ls_shift/su_mean 0.004 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.0000 0.756950(12) 0.2500 0.01104(5) Uani 1 d S . . Co2 Co 0.0000 0.329629(12) 0.2500 0.01107(5) Uani 1 d S . . N1 N 0.05775(5) 0.85822(5) 0.20762(5) 0.01409(17) Uani 1 d . . . C2 C 0.07714(6) 0.92669(7) 0.23701(6) 0.0170(2) Uani 1 d . . . H2 H 0.0724 0.9307 0.2809 0.020 Uiso 1 calc R . . C3 C 0.10384(6) 0.99191(7) 0.20589(6) 0.0196(2) Uani 1 d . . . H3 H 0.1169 1.0396 0.2281 0.023 Uiso 1 calc R . . C4 C 0.11106(6) 0.98610(7) 0.14194(6) 0.0205(2) Uani 1 d . . . H4 H 0.1273 1.0305 0.1192 0.025 Uiso 1 calc R . . C5 C 0.09424(6) 0.91448(7) 0.11136(6) 0.0187(2) Uani 1 d . . . H5 H 0.0999 0.9086 0.0677 0.022 Uiso 1 calc R . . C6 C 0.06878(6) 0.85133(6) 0.14617(5) 0.01419(18) Uani 1 d . . . C7 C 0.05599(6) 0.77028(6) 0.11998(5) 0.01353(18) Uani 1 d . . . N8 N 0.04135(5) 0.71551(5) 0.16276(4) 0.01223(16) Uani 1 d . . . C9 C 0.03184(6) 0.63882(6) 0.14530(5) 0.01278(18) Uani 1 d . . . C10 C 0.03113(6) 0.61538(7) 0.08265(5) 0.0163(2) Uani 1 d . . . H10 H 0.0206 0.5618 0.0706 0.020 Uiso 1 calc R . . C11 C 0.04624(7) 0.67268(7) 0.03801(6) 0.0194(2) Uani 1 d . . . H11 H 0.0466 0.6584 -0.0051 0.023 Uiso 1 calc R . . C12 C 0.06067(7) 0.75058(7) 0.05691(5) 0.0182(2) Uani 1 d . . . H12 H 0.0735 0.7897 0.0275 0.022 Uiso 1 calc R . . C13 C 0.01962(6) 0.58532(6) 0.19900(5) 0.01198(17) Uani 1 d . . . N13 N 0.0000 0.62392(8) 0.2500 0.0123(2) Uani 1 d S . . N14 N 0.0000 0.46271(7) 0.2500 0.0120(2) Uani 1 d S . . C14 C 0.02671(6) 0.50148(6) 0.20198(5) 0.01227(18) Uani 1 d . . . C15 C 0.06112(6) 0.44703(6) 0.15800(5) 0.01276(18) Uani 1 d . . . C16 C 0.11857(6) 0.46661(7) 0.12238(5) 0.0160(2) Uani 1 d . . . H16 H 0.1382 0.5190 0.1233 0.019 Uiso 1 calc R . . C17 C 0.14655(7) 0.40728(7) 0.08523(6) 0.0193(2) Uani 1 d . . . H17 H 0.1860 0.4188 0.0608 0.023 Uiso 1 calc R . . C18 C 0.11645(7) 0.33122(7) 0.08407(6) 0.0186(2) Uani 1 d . . . H18 H 0.1330 0.2910 0.0573 0.022 Uiso 1 calc R . . C19 C 0.06126(6) 0.31556(6) 0.12336(5) 0.01398(18) Uani 1 d . . . N20 N 0.03547(5) 0.37221(5) 0.15996(4) 0.01280(16) Uani 1 d . . . C21 C 0.02518(6) 0.23732(6) 0.12953(5) 0.01444(19) Uani 1 d . . . C22 C 0.02402(7) 0.17825(7) 0.08354(6) 0.0187(2) Uani 1 d . . . H22 H 0.0521 0.1836 0.0484 0.022 Uiso 1 calc R . . C23 C -0.01913(7) 0.11126(7) 0.09013(6) 0.0213(2) Uani 1 d . . . H23 H -0.0207 0.0699 0.0596 0.026 Uiso 1 calc R . . C24 C -0.05977(7) 0.10560(7) 0.14186(6) 0.0203(2) Uani 1 d . . . H24 H -0.0912 0.0615 0.1465 0.024 Uiso 1 calc R . . C25 C -0.05355(6) 0.16587(7) 0.18690(6) 0.0177(2) Uani 1 d . . . H25 H -0.0805 0.1613 0.2229 0.021 Uiso 1 calc R . . N26 N -0.01111(5) 0.23013(6) 0.18165(5) 0.01453(17) Uani 1 d . . . N30 N 0.09877(5) 0.74856(6) 0.31057(5) 0.01685(18) Uani 1 d . . . C31 C 0.14337(7) 0.73256(8) 0.34808(6) 0.0202(2) Uani 1 d . . . C32 C 0.19994(9) 0.71042(11) 0.39667(8) 0.0398(4) Uani 1 d . . . H32A H 0.2150 0.7577 0.4213 0.060 Uiso 1 calc R . . H32B H 0.2416 0.6885 0.3768 0.060 Uiso 1 calc R . . H32C H 0.1811 0.6702 0.4244 0.060 Uiso 1 calc R . . N40 N 0.11576(5) 0.33374(6) 0.26897(5) 0.01732(18) Uani 1 d . . . C41 C 0.17714(6) 0.33738(7) 0.26819(6) 0.0183(2) Uani 1 d . . . C42 C 0.25542(7) 0.34288(9) 0.26561(8) 0.0310(3) Uani 1 d . . . H42A H 0.2760 0.2891 0.2641 0.046 Uiso 1 calc R . . H42B H 0.2765 0.3707 0.3031 0.046 Uiso 1 calc R . . H42C H 0.2664 0.3725 0.2279 0.046 Uiso 1 calc R . . Cl70 Cl 0.14094(7) 0.90896(8) 0.45894(7) 0.01793(10) Uani 0.864(4) d PD A 1 O71 O 0.16767(11) 0.93408(10) 0.40072(8) 0.0369(4) Uani 0.864(4) d PD A 1 O72 O 0.08366(9) 0.85235(13) 0.44612(7) 0.0481(5) Uani 0.864(4) d PD A 1 O73 O 0.11451(11) 0.97630(10) 0.49250(7) 0.0432(5) Uani 0.864(4) d PD A 1 O74 O 0.19851(10) 0.87176(11) 0.49771(8) 0.0410(4) Uani 0.864(4) d PD A 1 Cl75 Cl 0.1391(5) 0.9154(5) 0.4597(4) 0.01793(10) Uani 0.136(4) d PD A 2 O71X O 0.1708(7) 0.9122(7) 0.4003(5) 0.0369(4) Uani 0.136(4) d PD A 2 O72X O 0.0634(4) 0.8969(8) 0.4505(4) 0.0481(5) Uani 0.136(4) d PD A 2 O73X O 0.1474(6) 0.9938(5) 0.4855(5) 0.0432(5) Uani 0.136(4) d PD A 2 O74X O 0.1738(6) 0.8581(6) 0.5017(5) 0.0410(4) Uani 0.136(4) d PD A 2 Cl80 Cl 0.229123(17) 0.59949(2) 0.233882(15) 0.02440(7) Uani 1 d . . . O81 O 0.17768(7) 0.56025(9) 0.27041(7) 0.0483(3) Uani 1 d . . . O82 O 0.19055(6) 0.65253(7) 0.19022(6) 0.0366(3) Uani 1 d . . . O83 O 0.28018(6) 0.64368(7) 0.27510(5) 0.0342(2) Uani 1 d . . . O84 O 0.26770(6) 0.54146(7) 0.19939(6) 0.0368(3) Uani 1 d . . . N50 N 0.08599(8) 0.52631(10) -0.05532(9) 0.0456(4) Uani 1 d . . . C51 C 0.14261(8) 0.52480(9) -0.07235(7) 0.0288(3) Uani 1 d . . . C52 C 0.21554(9) 0.52303(11) -0.09359(8) 0.0362(3) Uani 1 d . . . H52A H 0.2346 0.5775 -0.0947 0.054 Uiso 1 calc R . . H52B H 0.2141 0.4997 -0.1358 0.054 Uiso 1 calc R . . H52C H 0.2470 0.4907 -0.0645 0.054 Uiso 1 calc R . . N60 N 0.1871(4) 0.2724(2) 0.4239(2) 0.0713(14) Uani 0.555(5) d PD B 1 C61 C 0.2080(3) 0.2094(2) 0.4329(2) 0.0393(9) Uani 0.555(5) d PD B 1 C62 C 0.23775(10) 0.12963(11) 0.44384(8) 0.0391(4) Uani 0.555(5) d PD B 1 H62A H 0.2898 0.1335 0.4559 0.059 Uiso 0.555(5) calc PR B 1 H62B H 0.2299 0.0980 0.4053 0.059 Uiso 0.555(5) calc PR B 1 H62C H 0.2135 0.1038 0.4777 0.059 Uiso 0.555(5) calc PR B 1 N60X N 0.2324(5) 0.2802(3) 0.4138(3) 0.0713(14) Uani 0.445(5) d PD B 2 C61X C 0.2359(3) 0.2144(3) 0.4261(3) 0.0393(9) Uani 0.445(5) d PD B 2 C62X C 0.23775(10) 0.12963(11) 0.44384(8) 0.0391(4) Uani 0.445(5) d PD B 2 H62D H 0.1942 0.1164 0.4650 0.059 Uiso 0.445(5) calc PR B 2 H62E H 0.2808 0.1192 0.4724 0.059 Uiso 0.445(5) calc PR B 2 H62F H 0.2395 0.0968 0.4060 0.059 Uiso 0.445(5) calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.01104(9) 0.00892(9) 0.01303(9) 0.000 0.00005(7) 0.000 Co2 0.01169(9) 0.00852(9) 0.01315(9) 0.000 0.00204(7) 0.000 N1 0.0119(4) 0.0108(4) 0.0194(4) -0.0003(3) 0.0001(3) -0.0001(3) C2 0.0128(4) 0.0140(5) 0.0241(5) -0.0031(4) 0.0002(4) -0.0008(4) C3 0.0136(5) 0.0113(5) 0.0335(6) -0.0021(4) 0.0006(4) -0.0008(4) C4 0.0166(5) 0.0118(5) 0.0334(6) 0.0046(4) 0.0028(4) -0.0006(4) C5 0.0193(5) 0.0136(5) 0.0232(5) 0.0046(4) 0.0023(4) -0.0013(4) C6 0.0123(4) 0.0106(4) 0.0195(5) 0.0019(4) 0.0000(4) 0.0001(3) C7 0.0133(4) 0.0110(4) 0.0161(5) 0.0019(4) 0.0000(3) 0.0003(3) N8 0.0116(4) 0.0105(4) 0.0144(4) 0.0009(3) 0.0004(3) 0.0000(3) C9 0.0135(4) 0.0106(4) 0.0142(4) 0.0006(3) 0.0008(3) -0.0001(3) C10 0.0206(5) 0.0128(5) 0.0153(5) -0.0006(4) -0.0003(4) -0.0008(4) C11 0.0266(6) 0.0174(5) 0.0138(5) 0.0005(4) -0.0002(4) 0.0002(4) C12 0.0233(5) 0.0154(5) 0.0161(5) 0.0032(4) 0.0015(4) -0.0004(4) C13 0.0120(4) 0.0102(4) 0.0137(4) 0.0000(3) 0.0003(3) -0.0006(3) N13 0.0125(5) 0.0102(5) 0.0141(6) 0.000 0.0000(4) 0.000 N14 0.0118(5) 0.0097(5) 0.0145(6) 0.000 0.0015(4) 0.000 C14 0.0123(4) 0.0105(4) 0.0140(4) -0.0006(3) 0.0012(3) -0.0006(3) C15 0.0135(4) 0.0110(4) 0.0140(4) 0.0001(3) 0.0021(3) 0.0003(3) C16 0.0159(5) 0.0149(5) 0.0176(5) 0.0005(4) 0.0044(4) -0.0017(4) C17 0.0193(5) 0.0193(5) 0.0202(5) 0.0001(4) 0.0074(4) 0.0003(4) C18 0.0206(5) 0.0173(5) 0.0188(5) -0.0020(4) 0.0072(4) 0.0026(4) C19 0.0158(5) 0.0121(4) 0.0141(4) -0.0009(3) 0.0014(4) 0.0013(4) N20 0.0137(4) 0.0105(4) 0.0143(4) -0.0002(3) 0.0015(3) 0.0005(3) C21 0.0161(5) 0.0111(4) 0.0159(5) -0.0012(4) 0.0001(4) 0.0021(3) C22 0.0242(5) 0.0144(5) 0.0172(5) -0.0032(4) 0.0005(4) 0.0028(4) C23 0.0282(6) 0.0132(5) 0.0214(5) -0.0046(4) -0.0052(4) 0.0019(4) C24 0.0236(5) 0.0120(5) 0.0243(6) -0.0008(4) -0.0048(4) -0.0018(4) C25 0.0199(5) 0.0121(5) 0.0209(5) 0.0003(4) 0.0001(4) -0.0017(4) N26 0.0164(4) 0.0110(4) 0.0160(4) -0.0005(3) 0.0004(3) 0.0000(3) N30 0.0154(4) 0.0167(4) 0.0184(4) -0.0005(3) 0.0010(3) -0.0009(3) C31 0.0191(5) 0.0208(5) 0.0201(5) -0.0045(4) -0.0012(4) 0.0028(4) C32 0.0369(8) 0.0490(10) 0.0306(7) -0.0120(7) -0.0172(6) 0.0222(7) N40 0.0172(4) 0.0158(4) 0.0188(4) 0.0017(3) 0.0006(3) 0.0004(3) C41 0.0176(5) 0.0154(5) 0.0217(5) -0.0011(4) -0.0004(4) 0.0000(4) C42 0.0136(5) 0.0324(7) 0.0468(9) -0.0078(6) 0.0017(5) -0.0021(5) Cl70 0.01770(14) 0.0188(3) 0.01732(13) 0.00063(16) 0.00177(10) 0.00100(16) O71 0.0501(7) 0.0336(9) 0.0290(6) 0.0097(6) 0.0168(5) -0.0001(8) O72 0.0411(8) 0.0723(13) 0.0328(7) -0.0192(8) 0.0141(6) -0.0352(9) O73 0.0581(12) 0.0381(8) 0.0338(7) -0.0078(6) 0.0052(7) 0.0255(8) O74 0.0426(10) 0.0426(8) 0.0352(7) 0.0014(6) -0.0129(7) 0.0193(8) Cl75 0.01770(14) 0.0188(3) 0.01732(13) 0.00063(16) 0.00177(10) 0.00100(16) O71X 0.0501(7) 0.0336(9) 0.0290(6) 0.0097(6) 0.0168(5) -0.0001(8) O72X 0.0411(8) 0.0723(13) 0.0328(7) -0.0192(8) 0.0141(6) -0.0352(9) O73X 0.0581(12) 0.0381(8) 0.0338(7) -0.0078(6) 0.0052(7) 0.0255(8) O74X 0.0426(10) 0.0426(8) 0.0352(7) 0.0014(6) -0.0129(7) 0.0193(8) Cl80 0.01989(13) 0.02877(15) 0.02372(14) -0.00298(11) -0.00350(10) 0.00707(11) O81 0.0372(7) 0.0638(9) 0.0441(7) 0.0115(6) 0.0047(5) -0.0080(6) O82 0.0306(5) 0.0433(6) 0.0345(6) 0.0042(5) -0.0057(4) 0.0176(5) O83 0.0277(5) 0.0349(6) 0.0382(6) -0.0144(5) -0.0093(4) 0.0071(4) O84 0.0368(6) 0.0389(6) 0.0331(6) -0.0137(5) -0.0078(5) 0.0170(5) N50 0.0357(7) 0.0403(8) 0.0621(10) -0.0192(7) 0.0125(7) -0.0129(6) C51 0.0311(7) 0.0238(6) 0.0313(7) -0.0057(5) 0.0010(5) -0.0051(5) C52 0.0312(7) 0.0466(9) 0.0313(7) -0.0039(7) 0.0058(6) -0.0008(7) N60 0.128(4) 0.0428(13) 0.0394(16) -0.0040(11) -0.018(3) 0.014(2) C61 0.055(3) 0.0396(11) 0.0222(13) -0.0026(8) -0.0035(19) -0.0022(17) C62 0.0494(10) 0.0392(9) 0.0283(7) -0.0009(6) 0.0005(7) 0.0029(7) N60X 0.128(4) 0.0428(13) 0.0394(16) -0.0040(11) -0.018(3) 0.014(2) C61X 0.055(3) 0.0396(11) 0.0222(13) -0.0026(8) -0.0035(19) -0.0022(17) C62X 0.0494(10) 0.0392(9) 0.0283(7) -0.0009(6) 0.0005(7) 0.0029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N30 2.1602(10) . ? Co1 N30 2.1602(10) 2 ? Co1 N8 2.1803(9) . ? Co1 N8 2.1803(9) 2 ? Co1 N13 2.2300(13) . ? Co1 N1 2.2344(10) . ? Co1 N1 2.2344(9) 2 ? Co2 N40 2.1511(10) . ? Co2 N40 2.1511(10) 2 ? Co2 N20 2.1969(9) . ? Co2 N20 2.1969(9) 2 ? Co2 N26 2.2143(10) . ? Co2 N26 2.2143(10) 2 ? Co2 N14 2.2307(13) . ? N1 C2 1.3433(14) . ? N1 C6 1.3470(15) . ? C2 C3 1.3898(17) . ? C3 C4 1.3844(19) . ? C4 C5 1.3900(17) . ? C5 C6 1.3960(15) . ? C6 C7 1.4811(15) . ? C7 N8 1.3370(14) . ? C7 C12 1.3947(16) . ? N8 C9 1.3460(13) . ? C9 C10 1.3923(15) . ? C9 C13 1.4860(14) . ? C10 C11 1.3960(16) . ? C11 C12 1.3865(16) . ? C13 N13 1.3400(12) . ? C13 C14 1.4124(14) . ? N13 C13 1.3400(12) 2 ? N14 C14 1.3399(12) . ? N14 C14 1.3399(12) 2 ? C14 C15 1.4873(14) . ? C15 N20 1.3430(13) . ? C15 C16 1.3935(15) . ? C16 C17 1.3962(16) . ? C17 C18 1.3909(17) . ? C18 C19 1.3960(15) . ? C19 N20 1.3406(13) . ? C19 C21 1.4823(15) . ? C21 N26 1.3485(14) . ? C21 C22 1.3929(15) . ? C22 C23 1.3915(17) . ? C23 C24 1.3865(19) . ? C24 C25 1.3927(16) . ? C25 N26 1.3432(14) . ? N30 C31 1.1363(16) . ? C31 C32 1.4629(18) . ? N40 C41 1.1396(16) . ? C41 C42 1.4575(17) . ? Cl70 O72 1.4335(17) . ? Cl70 O71 1.4354(16) . ? Cl70 O74 1.4394(16) . ? Cl70 O73 1.4425(16) . ? Cl75 O73X 1.428(6) . ? Cl75 O74X 1.431(6) . ? Cl75 O72X 1.433(6) . ? Cl75 O71X 1.438(6) . ? Cl80 O81 1.4361(13) . ? Cl80 O82 1.4368(11) . ? Cl80 O84 1.4420(11) . ? Cl80 O83 1.4444(11) . ? N50 C51 1.136(2) . ? C51 C52 1.458(2) . ? N60 C61 1.137(4) . ? C61 C62 1.457(4) . ? N60X C61X 1.135(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 N30 Co1 N30 172.54(5) . 2 ? N30 Co1 N8 98.78(4) . . ? N30 Co1 N8 78.80(4) 2 . ? N30 Co1 N8 78.80(4) . 2 ? N30 Co1 N8 98.78(4) 2 2 ? N8 Co1 N8 142.84(5) . 2 ? N30 Co1 N13 86.27(3) . . ? N30 Co1 N13 86.27(3) 2 . ? N8 Co1 N13 71.42(2) . . ? N8 Co1 N13 71.42(2) 2 . ? N30 Co1 N1 83.23(4) . . ? N30 Co1 N1 102.53(4) 2 . ? N8 Co1 N1 71.69(3) . . ? N8 Co1 N1 142.97(3) 2 . ? N13 Co1 N1 139.44(2) . . ? N30 Co1 N1 102.53(4) . 2 ? N30 Co1 N1 83.22(4) 2 2 ? N8 Co1 N1 142.97(3) . 2 ? N8 Co1 N1 71.69(3) 2 2 ? N13 Co1 N1 139.44(2) . 2 ? N1 Co1 N1 81.12(5) . 2 ? N40 Co2 N40 176.33(5) . 2 ? N40 Co2 N20 78.05(4) . . ? N40 Co2 N20 100.73(4) 2 . ? N40 Co2 N20 100.73(4) . 2 ? N40 Co2 N20 78.05(4) 2 2 ? N20 Co2 N20 142.08(5) . 2 ? N40 Co2 N26 100.85(4) . . ? N40 Co2 N26 81.95(4) 2 . ? N20 Co2 N26 71.81(3) . . ? N20 Co2 N26 143.29(4) 2 . ? N40 Co2 N26 81.95(4) . 2 ? N40 Co2 N26 100.85(4) 2 2 ? N20 Co2 N26 143.29(3) . 2 ? N20 Co2 N26 71.81(3) 2 2 ? N26 Co2 N26 82.26(5) . 2 ? N40 Co2 N14 88.16(3) . . ? N40 Co2 N14 88.16(3) 2 . ? N20 Co2 N14 71.04(2) . . ? N20 Co2 N14 71.04(2) 2 . ? N26 Co2 N14 138.87(2) . . ? N26 Co2 N14 138.87(2) 2 . ? C2 N1 C6 118.17(10) . . ? C2 N1 Co1 125.40(8) . . ? C6 N1 Co1 116.24(7) . . ? N1 C2 C3 122.78(11) . . ? C4 C3 C2 118.71(11) . . ? C3 C4 C5 119.21(11) . . ? C4 C5 C6 118.54(11) . . ? N1 C6 C5 122.39(10) . . ? N1 C6 C7 114.44(9) . . ? C5 C6 C7 123.07(10) . . ? N8 C7 C12 121.80(10) . . ? N8 C7 C6 114.05(10) . . ? C12 C7 C6 124.13(10) . . ? C7 N8 C9 119.74(9) . . ? C7 N8 Co1 117.84(7) . . ? C9 N8 Co1 119.56(7) . . ? N8 C9 C10 121.76(10) . . ? N8 C9 C13 112.81(9) . . ? C10 C9 C13 125.39(10) . . ? C9 C10 C11 118.24(10) . . ? C12 C11 C10 119.61(11) . . ? C11 C12 C7 118.59(11) . . ? N13 C13 C14 118.30(10) . . ? N13 C13 C9 113.68(9) . . ? C14 C13 C9 128.03(10) . . ? C13 N13 C13 122.26(13) . 2 ? C13 N13 Co1 118.87(6) . . ? C13 N13 Co1 118.87(6) 2 . ? C14 N14 C14 121.96(13) . 2 ? C14 N14 Co2 119.02(6) . . ? C14 N14 Co2 119.02(6) 2 . ? N14 C14 C13 118.59(10) . . ? N14 C14 C15 112.72(9) . . ? C13 C14 C15 128.69(9) . . ? N20 C15 C16 121.58(10) . . ? N20 C15 C14 112.56(9) . . ? C16 C15 C14 125.59(10) . . ? C15 C16 C17 118.32(10) . . ? C18 C17 C16 119.81(10) . . ? C17 C18 C19 118.21(10) . . ? N20 C19 C18 121.80(10) . . ? N20 C19 C21 113.06(9) . . ? C18 C19 C21 125.14(10) . . ? C19 N20 C15 120.04(9) . . ? C19 N20 Co2 115.04(7) . . ? C15 N20 Co2 117.46(7) . . ? N26 C21 C22 122.40(10) . . ? N26 C21 C19 114.15(9) . . ? C22 C21 C19 123.28(10) . . ? C23 C22 C21 118.68(11) . . ? C24 C23 C22 119.15(11) . . ? C23 C24 C25 118.59(11) . . ? N26 C25 C24 122.81(11) . . ? C25 N26 C21 118.20(10) . . ? C25 N26 Co2 125.04(8) . . ? C21 N26 Co2 116.67(7) . . ? C31 N30 Co1 166.31(10) . . ? N30 C31 C32 178.79(15) . . ? C41 N40 Co2 168.28(10) . . ? N40 C41 C42 178.57(14) . . ? O72 Cl70 O71 109.20(12) . . ? O72 Cl70 O74 109.07(13) . . ? O71 Cl70 O74 109.53(12) . . ? O72 Cl70 O73 109.77(14) . . ? O71 Cl70 O73 110.67(12) . . ? O74 Cl70 O73 108.57(12) . . ? O73X Cl75 O74X 110.3(6) . . ? O73X Cl75 O72X 109.0(6) . . ? O74X Cl75 O72X 109.2(6) . . ? O73X Cl75 O71X 109.5(6) . . ? O74X Cl75 O71X 109.4(6) . . ? O72X Cl75 O71X 109.4(6) . . ? O81 Cl80 O82 108.54(8) . . ? O81 Cl80 O84 110.10(9) . . ? O82 Cl80 O84 109.12(7) . . ? O81 Cl80 O83 109.56(8) . . ? O82 Cl80 O83 110.25(7) . . ? O84 Cl80 O83 109.26(7) . . ? N50 C51 C52 179.45(17) . . ? N60 C61 C62 177.7(5) . . ? _diffrn_measured_fraction_theta_max 0.483 _diffrn_reflns_theta_full 30.97 _diffrn_measured_fraction_theta_full 0.483 _refine_diff_density_max 0.494 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.057