# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1685 data_z _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common Co2DPD _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H86 Cl2 Co2 N8 O3' _chemical_formula_weight 1384.32 _chemical_melting_point ? _chemical_compound_source ? 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' 'Co' 'Co' 0.3494 0.9721 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9872(2) _cell_length_b 13.0824(2) _cell_length_c 27.21270(10) _cell_angle_alpha 84.68 _cell_angle_beta 87.2850(10) _cell_angle_gamma 71.8840(10) _cell_volume 3700.93(9) _cell_formula_units_Z 2 _cell_measurement_temperature 183(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 1.242 _exptl_crystal_density_method ? _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.572 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7339 _exptl_absorpt_correction_T_max 0.8647 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15393 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 23.68 _reflns_number_total 10494 _reflns_number_observed 9358 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 4 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1589P)^2^+21.3106P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0114(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10490 _refine_ls_number_parameters 879 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_obs 0.0977 _refine_ls_wR_factor_all 0.2889 _refine_ls_wR_factor_obs 0.2714 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 1.080 _refine_ls_restrained_S_all 1.083 _refine_ls_restrained_S_obs 1.080 _refine_ls_shift/esd_max -0.756 _refine_ls_shift/esd_mean 0.031 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co -0.06102(8) 0.86127(7) 0.90751(3) 0.0284(3) Uani 1 d . . Co2 Co -0.06706(7) 0.83799(6) 0.59195(3) 0.0267(3) Uani 1 d . . N1 N -0.2059(5) 0.8202(4) 0.8844(2) 0.0316(12) Uani 1 d . . N2 N -0.1562(5) 1.0140(4) 0.8885(2) 0.0306(12) Uani 1 d . . N3 N 0.0716(5) 0.9047(4) 0.9396(2) 0.0322(12) Uani 1 d . . N4 N 0.0309(5) 0.7091(4) 0.9296(2) 0.0331(13) Uani 1 d . . N5 N -0.2108(5) 0.7882(4) 0.6200(2) 0.0306(12) Uani 1 d . . N6 N -0.1647(5) 0.9860(4) 0.6075(2) 0.0277(11) Uani 1 d . . N7 N 0.0697(5) 0.8892(4) 0.5588(2) 0.0282(12) Uani 1 d . . N8 N 0.0241(5) 0.6922(4) 0.5709(2) 0.0324(12) Uani 1 d . . O1 O -0.4474(4) 1.0166(3) 0.75044(15) 0.0290(10) Uani 1 d . . C1 C -0.2154(7) 0.7171(6) 0.8881(3) 0.037(2) Uani 1 d . . C2A C -0.3823(8) 0.6208(7) 0.8723(3) 0.054(2) Uani 1 d . . H2AA H -0.3264(8) 0.5606(7) 0.8936(3) 0.065 Uiso 1 calc R . H2AB H -0.4705(8) 0.6372(7) 0.8862(3) 0.065 Uiso 1 calc R . C2 C -0.3383(7) 0.7184(6) 0.8735(3) 0.039(2) Uani 1 d . . C2B C -0.3804(13) 0.5862(8) 0.8225(4) 0.090(4) Uani 1 d . . H2BA H -0.4100(13) 0.5226(8) 0.8240(4) 0.136 Uiso 1 calc R . H2BB H -0.2929(13) 0.5680(8) 0.8088(4) 0.136 Uiso 1 calc R . H2BC H -0.4370(13) 0.6448(8) 0.8014(4) 0.136 Uiso 1 calc R . C3 C -0.4068(6) 0.8218(6) 0.8612(3) 0.037(2) Uani 1 d . . C3A C -0.5448(7) 0.8545(7) 0.8468(3) 0.052(2) Uani 1 d . . H3AA H -0.5762(7) 0.9329(7) 0.8392(3) 0.078 Uiso 1 calc R . H3AB H -0.5958(7) 0.8336(7) 0.8741(3) 0.078 Uiso 1 calc R . H3AC H -0.5523(7) 0.8185(7) 0.8176(3) 0.078 Uiso 1 calc R . C4 C -0.3229(6) 0.8867(6) 0.8663(2) 0.0322(15) Uani 1 d . . C5 C -0.3495(6) 0.9960(6) 0.8546(2) 0.0324(15) Uani 1 d . . C6 C -0.2682(6) 1.0564(5) 0.8624(2) 0.0314(14) Uani 1 d . . C7 C -0.2945(7) 1.1705(6) 0.8503(3) 0.038(2) Uani 1 d . . C7A C -0.3953(8) 1.2481(6) 0.8182(3) 0.055(2) Uani 1 d . . H7AA H -0.4517(8) 1.2107(6) 0.8065(3) 0.082 Uiso 1 calc R . H7AB H -0.3543(8) 1.2769(6) 0.7898(3) 0.082 Uiso 1 calc R . H7AC H -0.4458(8) 1.3076(6) 0.8372(3) 0.082 Uiso 1 calc R . C8 C -0.2029(7) 1.1993(6) 0.8716(3) 0.039(2) Uani 1 d . . C8A C -0.1877(7) 1.3084(6) 0.8718(3) 0.052(2) Uani 1 d . . H8AA H -0.1557(7) 1.3153(6) 0.9043(3) 0.062 Uiso 1 calc R . H8AB H -0.2726(7) 1.3634(6) 0.8674(3) 0.062 Uiso 1 calc R . C8B C -0.0976(10) 1.3310(8) 0.8322(5) 0.080(3) Uani 1 d . . H8BA H -0.0917(10) 1.4037(8) 0.8343(5) 0.119 Uiso 1 calc R . H8BB H -0.1297(10) 1.3261(8) 0.7998(5) 0.119 Uiso 1 calc R . H8BC H -0.0127(10) 1.2779(8) 0.8367(5) 0.119 Uiso 1 calc R . C9 C -0.1169(6) 1.1014(5) 0.8954(2) 0.035(2) Uani 1 d . . C10 C -0.0142(6) 1.0988(6) 0.9221(3) 0.036(2) Uani 1 d . . H10A H -0.0007(6) 1.1660(6) 0.9257(3) 0.043 Uiso 1 calc R . C11 C 0.0721(6) 1.0079(5) 0.9444(2) 0.0322(15) Uani 1 d . . C12 C 0.1791(6) 1.0095(5) 0.9725(2) 0.0325(15) Uani 1 d . . C12A C 0.2057(7) 1.1072(6) 0.9863(3) 0.040(2) Uani 1 d . . H12A H 0.1418(7) 1.1717(6) 0.9716(3) 0.060 Uiso 1 calc R . H12B H 0.2914(7) 1.1064(6) 0.9741(3) 0.060 Uiso 1 calc R . H12C H 0.2016(7) 1.1083(6) 1.0223(3) 0.060 Uiso 1 calc R . C13 C 0.2443(6) 0.9044(5) 0.9852(2) 0.0338(15) Uani 1 d . . C13A C 0.3637(6) 0.8613(6) 1.0150(3) 0.038(2) Uani 1 d . . H13A H 0.3671(6) 0.9161(6) 1.0372(3) 0.046 Uiso 1 calc R . H13B H 0.3596(6) 0.7962(6) 1.0359(3) 0.046 Uiso 1 calc R . C13B C 0.4835(7) 0.8328(8) 0.9840(3) 0.059(2) Uani 1 d . . H13C H 0.5579(7) 0.8052(8) 1.0054(3) 0.088 Uiso 1 calc R . H13D H 0.4893(7) 0.8972(8) 0.9638(3) 0.088 Uiso 1 calc R . H13E H 0.4818(7) 0.7772(8) 0.9624(3) 0.088 Uiso 1 calc R . C14 C 0.1779(6) 0.8396(5) 0.9643(2) 0.0322(15) Uani 1 d . . C15 C 0.2145(6) 0.7296(6) 0.9693(3) 0.037(2) Uani 1 d . . H15A H 0.2932(6) 0.6931(6) 0.9852(3) 0.044 Uiso 1 calc R . C16 C 0.1462(6) 0.6672(6) 0.9530(2) 0.037(2) Uani 1 d . . C17 C 0.1820(7) 0.5519(6) 0.9603(3) 0.040(2) Uani 1 d . . C17A C 0.3040(8) 0.4792(6) 0.9837(4) 0.056(2) Uani 1 d . . H17A H 0.2876(8) 0.4142(6) 1.0005(4) 0.067 Uiso 1 calc R . H17B H 0.3301(8) 0.5176(6) 1.0090(4) 0.067 Uiso 1 calc R . C17B C 0.4131(9) 0.4444(9) 0.9461(5) 0.094(4) Uani 1 d . . H17C H 0.4899(9) 0.3975(9) 0.9630(5) 0.141 Uiso 1 calc R . H17D H 0.4311(9) 0.5083(9) 0.9298(5) 0.141 Uiso 1 calc R . H17E H 0.3886(9) 0.4049(9) 0.9214(5) 0.141 Uiso 1 calc R . C18A C 0.0796(9) 0.4104(6) 0.9412(4) 0.057(2) Uani 1 d . . H18A H 0.0001(9) 0.4136(6) 0.9254(4) 0.086 Uiso 1 calc R . H18B H 0.0799(9) 0.3777(6) 0.9751(4) 0.086 Uiso 1 calc R . H18C H 0.1531(9) 0.3667(6) 0.9227(4) 0.086 Uiso 1 calc R . C18 C 0.0885(7) 0.5219(6) 0.9420(3) 0.043(2) Uani 1 d . . C19 C -0.0056(6) 0.6198(5) 0.9230(3) 0.035(2) Uani 1 d . . C20 C -0.1206(7) 0.6252(6) 0.9043(3) 0.041(2) Uani 1 d . . H20A H -0.1369(7) 0.5586(6) 0.9023(3) 0.049 Uiso 1 calc R . C21 C -0.2171(6) 0.6857(5) 0.6214(3) 0.038(2) Uani 1 d . . C22 C -0.3332(7) 0.6773(6) 0.6460(3) 0.048(2) Uani 1 d . . C22A C -0.3795(13) 0.5761(8) 0.6485(6) 0.108(5) Uani 1 d . . H22A H -0.4730(13) 0.5980(8) 0.6434(6) 0.130 Uiso 1 calc R . H22B H -0.3359(13) 0.5288(8) 0.6224(6) 0.130 Uiso 1 calc R . C22B C -0.3520(17) 0.5255(16) 0.6917(8) 0.155(8) Uani 1 d . . H22C H -0.3797(17) 0.4608(16) 0.6943(8) 0.232 Uiso 1 calc R . H22D H -0.3963(17) 0.5729(16) 0.7172(8) 0.232 Uiso 1 calc R . H22E H -0.2593(17) 0.5045(16) 0.6964(8) 0.232 Uiso 1 calc R . C23 C -0.3972(6) 0.7749(6) 0.6592(3) 0.041(2) Uani 1 d . . C23A C -0.5220(8) 0.8012(7) 0.6894(4) 0.062(2) Uani 1 d . . H23A H -0.5512(8) 0.8783(7) 0.6946(4) 0.092 Uiso 1 calc R . H23B H -0.5078(8) 0.7588(7) 0.7214(4) 0.092 Uiso 1 calc R . H23C H -0.5873(8) 0.7834(7) 0.6716(4) 0.092 Uiso 1 calc R . C24 C -0.3232(6) 0.8468(5) 0.6425(2) 0.0303(14) Uani 1 d . . C25 C -0.3586(6) 0.9569(5) 0.6469(2) 0.0303(14) Uani 1 d . . C26 C -0.2839(6) 1.0233(5) 0.6308(2) 0.0283(14) Uani 1 d . . C27 C -0.3165(7) 1.1387(5) 0.6355(3) 0.037(2) Uani 1 d . . C27A C -0.4318(7) 1.2149(6) 0.6589(3) 0.051(2) Uani 1 d . . H27A H -0.4909(7) 1.1755(6) 0.6717(3) 0.076 Uiso 1 calc R . H27B H -0.4752(7) 1.2727(6) 0.6343(3) 0.076 Uiso 1 calc R . H27C H -0.4046(7) 1.2463(6) 0.6862(3) 0.076 Uiso 1 calc R . C28 C -0.2182(6) 1.1699(5) 0.6147(3) 0.036(2) Uani 1 d . . C28A C -0.1980(8) 1.2778(6) 0.6129(3) 0.051(2) Uani 1 d . . H28A H -0.2820(8) 1.3348(6) 0.6137(3) 0.061 Uiso 1 calc R . H28B H -0.1531(8) 1.2906(6) 0.5817(3) 0.061 Uiso 1 calc R . C28B C -0.1197(11) 1.2838(8) 0.6562(4) 0.078(3) Uani 1 d . . H28C H -0.1074(11) 1.3551(8) 0.6544(4) 0.117 Uiso 1 calc R . H28D H -0.0362(11) 1.2281(8) 0.6551(4) 0.117 Uiso 1 calc R . H28E H -0.1649(11) 1.2722(8) 0.6871(4) 0.117 Uiso 1 calc R . C29 C -0.1262(6) 1.0756(5) 0.5968(2) 0.0301(14) Uani 1 d . . C30 C -0.0162(6) 1.0792(5) 0.5711(2) 0.0334(15) Uani 1 d . . H30A H -0.0025(6) 1.1476(5) 0.5655(2) 0.040 Uiso 1 calc R . C31 C 0.0743(6) 0.9936(5) 0.5532(2) 0.0288(14) Uani 1 d . . C32 C 0.1906(6) 1.0001(5) 0.5271(2) 0.0313(15) Uani 1 d . . C32A C 0.2222(7) 1.1009(6) 0.5123(3) 0.040(2) Uani 1 d . . H32A H 0.1550(7) 1.1623(6) 0.5246(3) 0.060 Uiso 1 calc R . H32B H 0.2282(7) 1.1106(6) 0.4763(3) 0.060 Uiso 1 calc R . H32C H 0.3044(7) 1.0963(6) 0.5264(3) 0.060 Uiso 1 calc R . C33 C 0.2579(6) 0.8981(5) 0.5176(2) 0.0320(15) Uani 1 d . . C33A C 0.3862(7) 0.8592(6) 0.4934(3) 0.042(2) Uani 1 d . . H33A H 0.4052(7) 0.9210(6) 0.4744(3) 0.050 Uiso 1 calc R . H33B H 0.3845(7) 0.8065(6) 0.4697(3) 0.050 Uiso 1 calc R . C33B C 0.4923(8) 0.8064(8) 0.5299(3) 0.058(2) Uani 1 d . . H33C H 0.5745(8) 0.7825(8) 0.5120(3) 0.087 Uiso 1 calc R . H33D H 0.4751(8) 0.7441(8) 0.5483(3) 0.087 Uiso 1 calc R . H33E H 0.4958(8) 0.8586(8) 0.5530(3) 0.087 Uiso 1 calc R . C34 C 0.1814(6) 0.8301(5) 0.5370(2) 0.0329(15) Uani 1 d . . C35 C 0.2148(7) 0.7218(6) 0.5314(3) 0.038(2) Uani 1 d . . H35A H 0.2950(7) 0.6890(6) 0.5158(3) 0.046 Uiso 1 calc R . C36 C 0.1402(6) 0.6572(6) 0.5468(3) 0.038(2) Uani 1 d . . C37 C 0.1729(7) 0.5458(6) 0.5383(3) 0.047(2) Uani 1 d . . C37A C 0.2948(8) 0.4811(7) 0.5136(4) 0.060(2) Uani 1 d . . H37A H 0.2777(8) 0.4225(7) 0.4973(4) 0.072 Uiso 1 calc R . H37B H 0.3213(8) 0.5285(7) 0.4876(4) 0.072 Uiso 1 calc R . C37B C 0.4017(9) 0.4331(9) 0.5482(5) 0.084(3) Uani 1 d . . H37C H 0.4778(9) 0.3922(9) 0.5301(5) 0.125 Uiso 1 calc R . H37D H 0.3771(9) 0.3846(9) 0.5736(5) 0.125 Uiso 1 calc R . H37E H 0.4209(9) 0.4907(9) 0.5639(5) 0.125 Uiso 1 calc R . C38A C 0.0658(9) 0.3992(6) 0.5595(4) 0.063(3) Uani 1 d . . H38A H -0.0142(9) 0.3976(6) 0.5766(4) 0.094 Uiso 1 calc R . H38B H 0.1385(9) 0.3478(6) 0.5771(4) 0.094 Uiso 1 calc R . H38C H 0.0657(9) 0.3793(6) 0.5257(4) 0.094 Uiso 1 calc R . C38 C 0.0773(7) 0.5094(6) 0.5583(3) 0.045(2) Uani 1 d . . C39 C -0.0152(7) 0.6016(6) 0.5779(3) 0.039(2) Uani 1 d . . C40 C -0.1268(7) 0.6003(6) 0.6014(3) 0.045(2) Uani 1 d . . H40A H -0.1447(7) 0.5334(6) 0.6042(3) 0.054 Uiso 1 calc R . C41 C -0.5234(6) 1.0630(5) 0.7902(2) 0.0321(15) Uani 1 d . . C42 C -0.4821(6) 1.0583(6) 0.8372(2) 0.035(2) Uani 1 d . . C43 C -0.5736(7) 1.1111(7) 0.8701(3) 0.047(2) Uani 1 d . . H43A H -0.5499(7) 1.1106(7) 0.9032(3) 0.057 Uiso 1 calc R . C44 C -0.7001(7) 1.1656(8) 0.8569(3) 0.062(3) Uani 1 d . . H44A H -0.7595(7) 1.2026(8) 0.8807(3) 0.075 Uiso 1 calc R . C45 C -0.7389(7) 1.1659(8) 0.8101(3) 0.058(2) Uani 1 d . . H45A H -0.8253(7) 1.2012(8) 0.8012(3) 0.069 Uiso 1 calc R . C46 C -0.6498(6) 1.1140(6) 0.7757(2) 0.038(2) Uani 1 d . . C47 C -0.6539(6) 1.0970(6) 0.7246(3) 0.038(2) Uani 1 d . . C48 C -0.7497(7) 1.1239(7) 0.6900(3) 0.050(2) Uani 1 d . . H48A H -0.8358(7) 1.1608(7) 0.6989(3) 0.060 Uiso 1 calc R . C49 C -0.7178(7) 1.0962(8) 0.6430(3) 0.055(2) Uani 1 d . . H49A H -0.7823(7) 1.1138(8) 0.6188(3) 0.066 Uiso 1 calc R . C50 C -0.5913(7) 1.0422(6) 0.6301(3) 0.043(2) Uani 1 d . . H50A H -0.5717(7) 1.0257(6) 0.5968(3) 0.052 Uiso 1 calc R . C51 C -0.4926(6) 1.0115(5) 0.6638(2) 0.0311(15) Uani 1 d . . C52 C -0.5298(6) 1.0387(5) 0.7108(2) 0.0308(14) Uani 1 d . . C1S C 0.1186(16) 0.9136(19) 0.8206(6) 0.178(10) Uani 1 d . . H1SA H 0.1832(109) 0.8806(81) 0.7959(51) 0.267 Uiso 1 calc R . H1SB H 0.1612(132) 0.9179(124) 0.8509(16) 0.267 Uiso 1 calc R . H1SC H 0.0688(31) 0.9864(47) 0.8078(63) 0.267 Uiso 1 calc R . O1S O 0.0366(5) 0.8507(5) 0.8311(2) 0.0549(14) Uani 1 d . . H1SD H 0.0778(24) 0.7905(33) 0.8449(37) 0.082 Uiso 1 calc R . C2S C 0.1512(11) 0.8178(13) 0.6690(4) 0.100(4) Uani 1 d . . H2SA H 0.1899(42) 0.7822(71) 0.7002(17) 0.150 Uiso 1 calc R . H2SB H 0.1428(14) 0.8948(13) 0.6675(37) 0.150 Uiso 1 calc R . H2SC H 0.2058(31) 0.7853(71) 0.6414(22) 0.150 Uiso 1 calc R . O2S O 0.0312(5) 0.8052(5) 0.6658(2) 0.0509(14) Uani 1 d . . H2SD H 0.0310(29) 0.7686(71) 0.6421(24) 0.076 Uiso 1 calc R . C3S C -0.7716(29) 1.5883(20) 0.8233(9) 0.098(8) Uani 0.50 d P . H3SA H -0.8633(29) 1.6292(20) 0.8189(9) 0.118 Uiso 0.50 calc PR . H3SB H -0.7495(29) 1.6003(20) 0.8566(9) 0.118 Uiso 0.50 calc PR . Cl1S Cl -0.6953(9) 1.6431(10) 0.7860(4) 0.155(4) Uani 0.50 d P . Cl2S Cl -0.7597(12) 1.4565(8) 0.8242(3) 0.154(4) Uani 0.50 d P . C4S C 0.1632(38) 0.5011(28) 0.6885(10) 0.152(16) Uani 0.50 d P . H4SA H 0.1390(38) 0.5160(28) 0.6533(10) 0.182 Uiso 0.50 calc PR . H4SB H 0.1504(38) 0.5720(28) 0.7014(10) 0.182 Uiso 0.50 calc PR . Cl3S Cl 0.0480(11) 0.4461(9) 0.7195(4) 0.161(4) Uani 0.50 d P . Cl4S Cl 0.2986(13) 0.4465(13) 0.6890(5) 0.248(9) Uani 0.50 d P . 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 0.0218(5) 0.0311(5) 0.0320(5) -0.0032(4) -0.0082(4) -0.0066(4) Co2 0.0225(5) 0.0284(5) 0.0299(5) -0.0040(4) 0.0008(3) -0.0087(4) N1 0.029(3) 0.037(3) 0.030(3) -0.004(2) -0.009(2) -0.011(2) N2 0.027(3) 0.034(3) 0.031(3) -0.001(2) -0.009(2) -0.008(2) N3 0.025(3) 0.036(3) 0.036(3) -0.001(2) -0.010(2) -0.009(2) N4 0.031(3) 0.030(3) 0.038(3) -0.003(2) -0.010(2) -0.008(2) N5 0.025(3) 0.033(3) 0.034(3) -0.004(2) -0.002(2) -0.009(2) N6 0.025(3) 0.032(3) 0.028(3) -0.005(2) -0.001(2) -0.010(2) N7 0.027(3) 0.029(3) 0.028(3) -0.003(2) 0.002(2) -0.008(2) N8 0.027(3) 0.030(3) 0.039(3) -0.005(2) 0.003(2) -0.008(2) O1 0.017(2) 0.041(3) 0.026(2) -0.003(2) -0.005(2) -0.003(2) C1 0.035(4) 0.037(4) 0.042(4) -0.004(3) -0.010(3) -0.013(3) C2A 0.046(5) 0.051(5) 0.074(6) 0.008(4) -0.028(4) -0.027(4) C2 0.035(4) 0.047(4) 0.040(4) 0.000(3) -0.010(3) -0.018(3) C2B 0.128(10) 0.054(6) 0.100(8) -0.004(6) -0.055(8) -0.035(6) C3 0.026(3) 0.052(5) 0.037(4) -0.005(3) -0.007(3) -0.016(3) C3A 0.030(4) 0.059(5) 0.072(6) 0.004(4) -0.014(4) -0.022(4) C4 0.026(3) 0.045(4) 0.027(3) -0.006(3) -0.006(3) -0.012(3) C5 0.026(3) 0.044(4) 0.024(3) -0.008(3) -0.004(3) -0.005(3) C6 0.027(3) 0.034(4) 0.030(3) -0.004(3) -0.007(3) -0.004(3) C7 0.033(4) 0.045(4) 0.033(4) -0.003(3) -0.010(3) -0.007(3) C7A 0.060(5) 0.036(4) 0.065(5) 0.005(4) -0.020(4) -0.011(4) C8 0.032(4) 0.034(4) 0.048(4) 0.000(3) -0.007(3) -0.007(3) C8A 0.040(4) 0.044(4) 0.070(6) 0.003(4) -0.023(4) -0.009(3) C8B 0.070(7) 0.056(6) 0.112(9) 0.001(6) 0.012(6) -0.023(5) C9 0.032(4) 0.035(4) 0.036(4) 0.001(3) -0.008(3) -0.008(3) C10 0.034(4) 0.034(4) 0.044(4) -0.002(3) -0.011(3) -0.015(3) C11 0.028(3) 0.033(4) 0.037(4) -0.002(3) -0.007(3) -0.012(3) C12 0.031(3) 0.042(4) 0.028(3) -0.003(3) -0.005(3) -0.015(3) C12A 0.034(4) 0.055(5) 0.035(4) -0.001(3) -0.010(3) -0.018(3) C13 0.031(3) 0.039(4) 0.033(4) -0.005(3) -0.008(3) -0.011(3) C13A 0.030(4) 0.049(4) 0.039(4) -0.006(3) -0.014(3) -0.014(3) C13B 0.032(4) 0.081(6) 0.063(5) -0.002(5) -0.009(4) -0.016(4) C14 0.025(3) 0.039(4) 0.034(4) -0.006(3) -0.007(3) -0.010(3) C15 0.024(3) 0.042(4) 0.041(4) -0.003(3) -0.010(3) -0.006(3) C16 0.030(4) 0.045(4) 0.034(4) 0.000(3) -0.007(3) -0.010(3) C17 0.036(4) 0.034(4) 0.048(4) -0.001(3) -0.009(3) -0.009(3) C17A 0.048(5) 0.037(4) 0.080(6) 0.011(4) -0.029(4) -0.009(4) C17B 0.038(5) 0.080(7) 0.147(11) 0.029(7) -0.006(6) -0.002(5) C18A 0.059(5) 0.038(4) 0.075(6) -0.004(4) -0.017(4) -0.014(4) C18 0.041(4) 0.032(4) 0.054(5) 0.000(3) -0.006(3) -0.009(3) C19 0.032(4) 0.034(4) 0.039(4) -0.004(3) -0.008(3) -0.009(3) C20 0.041(4) 0.035(4) 0.050(4) -0.007(3) -0.007(3) -0.016(3) C21 0.031(4) 0.033(4) 0.048(4) -0.001(3) 0.004(3) -0.010(3) C22 0.030(4) 0.039(4) 0.080(6) -0.009(4) 0.015(4) -0.018(3) C22A 0.109(9) 0.042(5) 0.141(12) 0.013(6) 0.086(9) 0.005(5) C22B 0.119(14) 0.173(18) 0.203(20) -0.104(16) 0.040(14) -0.070(13) C23 0.023(3) 0.045(4) 0.056(5) -0.002(3) 0.002(3) -0.013(3) C23A 0.037(4) 0.057(5) 0.094(7) -0.011(5) 0.026(4) -0.022(4) C24 0.022(3) 0.036(4) 0.034(3) -0.005(3) -0.002(3) -0.008(3) C25 0.022(3) 0.035(4) 0.032(3) -0.003(3) -0.005(3) -0.004(3) C26 0.020(3) 0.034(3) 0.029(3) -0.003(3) -0.002(3) -0.005(3) C27 0.035(4) 0.033(4) 0.039(4) -0.009(3) 0.002(3) -0.005(3) C27A 0.043(4) 0.040(4) 0.067(5) -0.011(4) 0.009(4) -0.007(3) C28 0.029(4) 0.032(4) 0.046(4) -0.007(3) 0.000(3) -0.006(3) C28A 0.045(4) 0.032(4) 0.075(6) -0.010(4) 0.007(4) -0.010(3) C28B 0.090(8) 0.061(6) 0.096(8) -0.027(5) -0.005(6) -0.038(6) C29 0.029(3) 0.029(3) 0.033(3) -0.005(3) -0.001(3) -0.009(3) C30 0.035(4) 0.033(4) 0.034(4) -0.002(3) -0.006(3) -0.013(3) C31 0.026(3) 0.037(4) 0.026(3) -0.002(3) -0.001(3) -0.013(3) C32 0.030(3) 0.041(4) 0.027(3) 0.001(3) -0.001(3) -0.019(3) C32A 0.039(4) 0.050(4) 0.039(4) 0.000(3) -0.001(3) -0.025(3) C33 0.028(3) 0.040(4) 0.032(3) -0.005(3) 0.002(3) -0.016(3) C33A 0.034(4) 0.049(4) 0.044(4) -0.005(3) 0.012(3) -0.016(3) C33B 0.036(4) 0.073(6) 0.069(6) -0.018(5) 0.000(4) -0.021(4) C34 0.028(3) 0.038(4) 0.034(4) -0.001(3) 0.001(3) -0.012(3) C35 0.033(4) 0.040(4) 0.040(4) -0.011(3) 0.012(3) -0.010(3) C36 0.029(4) 0.039(4) 0.044(4) -0.006(3) 0.001(3) -0.009(3) C37 0.036(4) 0.039(4) 0.064(5) -0.013(4) 0.010(4) -0.008(3) C37A 0.045(5) 0.047(5) 0.085(7) -0.023(4) 0.024(5) -0.010(4) C37B 0.048(6) 0.086(8) 0.102(9) -0.018(6) 0.006(5) 0.003(5) C38A 0.058(5) 0.036(4) 0.098(7) -0.022(4) 0.023(5) -0.017(4) C38 0.039(4) 0.034(4) 0.061(5) -0.009(3) 0.006(4) -0.010(3) C39 0.036(4) 0.036(4) 0.045(4) -0.008(3) 0.003(3) -0.013(3) C40 0.036(4) 0.031(4) 0.069(5) -0.006(3) 0.004(4) -0.013(3) C41 0.021(3) 0.042(4) 0.031(4) -0.008(3) -0.002(3) -0.004(3) C42 0.027(3) 0.042(4) 0.030(4) -0.003(3) -0.006(3) -0.004(3) C43 0.037(4) 0.065(5) 0.031(4) -0.013(4) -0.009(3) 0.000(4) C44 0.030(4) 0.097(7) 0.040(4) -0.024(4) -0.003(3) 0.013(4) C45 0.026(4) 0.090(7) 0.040(4) -0.015(4) -0.008(3) 0.010(4) C46 0.020(3) 0.056(4) 0.031(4) -0.005(3) -0.004(3) 0.000(3) C47 0.017(3) 0.059(5) 0.034(4) -0.005(3) -0.004(3) -0.003(3) C48 0.024(4) 0.080(6) 0.036(4) -0.013(4) -0.007(3) 0.001(4) C49 0.030(4) 0.089(6) 0.040(4) -0.013(4) -0.014(3) -0.003(4) C50 0.032(4) 0.061(5) 0.034(4) -0.014(3) -0.005(3) -0.006(3) C51 0.022(3) 0.039(4) 0.031(4) -0.004(3) -0.002(3) -0.009(3) C52 0.018(3) 0.037(4) 0.034(4) -0.007(3) -0.005(3) -0.003(3) C1S 0.160(15) 0.356(29) 0.112(11) -0.113(15) 0.083(11) -0.202(19) O1S 0.042(3) 0.072(4) 0.053(3) -0.015(3) 0.008(3) -0.019(3) C2S 0.071(7) 0.185(14) 0.066(7) 0.024(8) -0.020(6) -0.077(8) O2S 0.040(3) 0.076(4) 0.040(3) 0.002(3) -0.012(2) -0.022(3) C3S 0.127(22) 0.088(17) 0.069(14) -0.018(12) 0.024(14) -0.019(15) Cl1S 0.126(7) 0.207(11) 0.162(8) -0.056(8) 0.041(6) -0.091(7) Cl2S 0.221(11) 0.144(8) 0.098(6) -0.016(5) 0.019(6) -0.058(7) C4S 0.245(40) 0.170(28) 0.085(18) 0.072(19) -0.111(24) -0.137(29) Cl3S 0.198(10) 0.190(10) 0.147(8) 0.023(7) -0.063(7) -0.134(9) Cl4S 0.174(11) 0.286(17) 0.151(9) 0.008(10) 0.065(9) 0.104(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 Co1 N1 1.978(5) . ? Co1 N2 1.978(5) . ? Co1 N4 1.983(5) . ? Co1 N3 1.984(5) . ? Co2 N6 1.974(5) . ? Co2 N7 1.977(5) . ? Co2 N8 1.982(5) . ? Co2 N5 1.983(5) . ? N1 C1 1.378(9) . ? N1 C4 1.392(8) . ? N2 C9 1.373(9) . ? N2 C6 1.383(8) . ? N3 C11 1.370(9) . ? N3 C14 1.374(8) . ? N4 C19 1.377(9) . ? N4 C16 1.375(8) . ? N5 C21 1.360(9) . ? N5 C24 1.384(8) . ? N6 C29 1.368(8) . ? N6 C26 1.392(8) . ? N7 C34 1.372(8) . ? N7 C31 1.376(8) . ? N8 C36 1.372(9) . ? N8 C39 1.377(9) . ? O1 C52 1.393(7) . ? O1 C41 1.399(8) . ? C1 C20 1.376(10) . ? C1 C2 1.420(10) . ? C2A C2B 1.466(14) . ? C2A C2 1.503(10) . ? C2 C3 1.347(10) . ? C3 C4 1.452(9) . ? C3 C3A 1.502(9) . ? C4 C5 1.377(10) . ? C5 C6 1.399(10) . ? C5 C42 1.505(9) . ? C6 C7 1.438(10) . ? C7 C8 1.351(10) . ? C7 C7A 1.500(10) . ? C8 C9 1.450(10) . ? C8 C8A 1.488(11) . ? C8A C8B 1.499(13) . ? C9 C10 1.361(10) . ? C10 C11 1.379(10) . ? C11 C12 1.439(9) . ? C12 C13 1.359(10) . ? C12 C12A 1.481(10) . ? C13 C14 1.446(9) . ? C13 C13A 1.500(9) . ? C13A C13B 1.494(11) . ? C14 C15 1.364(10) . ? C15 C16 1.381(10) . ? C16 C17 1.432(10) . ? C17 C18 1.340(10) . ? C17 C17A 1.511(10) . ? C17A C17B 1.524(15) . ? C18A C18 1.494(11) . ? C18 C19 1.443(10) . ? C19 C20 1.362(10) . ? C21 C40 1.380(10) . ? C21 C22 1.442(10) . ? C22 C23 1.325(11) . ? C22 C22A 1.554(14) . ? C22A C22B 1.30(2) . ? C23 C24 1.454(9) . ? C23 C23A 1.525(10) . ? C24 C25 1.386(9) . ? C25 C26 1.400(9) . ? C25 C51 1.493(9) . ? C26 C27 1.456(9) . ? C27 C28 1.351(10) . ? C27 C27A 1.504(10) . ? C28 C29 1.439(9) . ? C28 C28A 1.492(10) . ? C28A C28B 1.513(13) . ? C29 C30 1.379(9) . ? C30 C31 1.358(9) . ? C31 C32 1.455(9) . ? C32 C33 1.351(10) . ? C32 C32A 1.481(9) . ? C33 C34 1.453(9) . ? C33 C33A 1.486(9) . ? C33A C33B 1.518(11) . ? C34 C35 1.370(10) . ? C35 C36 1.376(10) . ? C36 C37 1.427(10) . ? C37 C38 1.355(11) . ? C37 C37A 1.510(10) . ? C37A C37B 1.483(14) . ? C38A C38 1.482(11) . ? C38 C39 1.442(10) . ? C39 C40 1.360(10) . ? C41 C42 1.367(9) . ? C41 C46 1.399(9) . ? C42 C43 1.373(10) . ? C43 C44 1.397(10) . ? C44 C45 1.362(11) . ? C45 C46 1.382(10) . ? C46 C47 1.434(10) . ? C47 C48 1.386(10) . ? C47 C52 1.393(9) . ? C48 C49 1.363(11) . ? C49 C50 1.394(10) . ? C50 C51 1.391(9) . ? C51 C52 1.369(9) . ? C1S O1S 1.402(14) . ? C2S O2S 1.386(11) . ? C3S Cl1S 1.55(3) . ? C3S Cl2S 1.69(3) . ? C4S Cl4S 1.44(4) . ? C4S Cl3S 1.78(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 Co1 N2 88.8(2) . . ? N1 Co1 N4 91.3(2) . . ? N2 Co1 N4 177.4(2) . . ? N1 Co1 N3 172.1(2) . . ? N2 Co1 N3 91.0(2) . . ? N4 Co1 N3 88.6(2) . . ? N6 Co2 N7 91.1(2) . . ? N6 Co2 N8 175.2(2) . . ? N7 Co2 N8 88.5(2) . . ? N6 Co2 N5 89.1(2) . . ? N7 Co2 N5 175.4(2) . . ? N8 Co2 N5 90.9(2) . . ? C1 N1 C4 105.5(5) . . ? C1 N1 Co1 125.5(4) . . ? C4 N1 Co1 128.7(4) . . ? C9 N2 C6 104.7(5) . . ? C9 N2 Co1 125.9(4) . . ? C6 N2 Co1 129.2(4) . . ? C11 N3 C14 105.0(5) . . ? C11 N3 Co1 126.7(4) . . ? C14 N3 Co1 128.2(4) . . ? C19 N4 C16 104.0(5) . . ? C19 N4 Co1 127.0(4) . . ? C16 N4 Co1 129.0(5) . . ? C21 N5 C24 105.3(5) . . ? C21 N5 Co2 125.9(4) . . ? C24 N5 Co2 128.8(4) . . ? C29 N6 C26 105.0(5) . . ? C29 N6 Co2 125.7(4) . . ? C26 N6 Co2 129.3(4) . . ? C34 N7 C31 104.4(5) . . ? C34 N7 Co2 128.6(4) . . ? C31 N7 Co2 127.0(4) . . ? C36 N8 C39 103.8(5) . . ? C36 N8 Co2 128.8(5) . . ? C39 N8 Co2 127.4(4) . . ? C52 O1 C41 105.4(4) . . ? C20 C1 N1 125.3(6) . . ? C20 C1 C2 124.0(7) . . ? N1 C1 C2 110.6(6) . . ? C2B C2A C2 113.1(8) . . ? C3 C2 C1 107.8(6) . . ? C3 C2 C2A 126.8(6) . . ? C1 C2 C2A 125.4(7) . . ? C2 C3 C4 106.9(6) . . ? C2 C3 C3A 122.6(7) . . ? C4 C3 C3A 130.5(7) . . ? C5 C4 N1 123.6(6) . . ? C5 C4 C3 127.3(6) . . ? N1 C4 C3 109.1(6) . . ? C4 C5 C6 125.4(6) . . ? C4 C5 C42 117.6(6) . . ? C6 C5 C42 116.6(6) . . ? N2 C6 C5 122.6(6) . . ? N2 C6 C7 111.0(6) . . ? C5 C6 C7 126.0(6) . . ? C8 C7 C6 106.7(6) . . ? C8 C7 C7A 122.8(7) . . ? C6 C7 C7A 130.3(6) . . ? C7 C8 C9 106.7(6) . . ? C7 C8 C8A 128.7(6) . . ? C9 C8 C8A 124.5(6) . . ? C8 C8A C8B 113.4(8) . . ? C10 C9 N2 125.4(6) . . ? C10 C9 C8 123.8(6) . . ? N2 C9 C8 110.7(6) . . ? C9 C10 C11 126.1(6) . . ? N3 C11 C10 124.1(6) . . ? N3 C11 C12 111.7(6) . . ? C10 C11 C12 124.0(6) . . ? C13 C12 C11 105.7(6) . . ? C13 C12 C12A 128.3(6) . . ? C11 C12 C12A 125.9(6) . . ? C12 C13 C14 107.2(6) . . ? C12 C13 C13A 127.3(6) . . ? C14 C13 C13A 125.4(6) . . ? C13B C13A C13 113.2(6) . . ? C15 C14 N3 125.1(6) . . ? C15 C14 C13 124.5(6) . . ? N3 C14 C13 110.3(6) . . ? C14 C15 C16 125.0(6) . . ? N4 C16 C15 123.7(6) . . ? N4 C16 C17 111.3(6) . . ? C15 C16 C17 124.9(6) . . ? C18 C17 C16 107.2(6) . . ? C18 C17 C17A 127.2(7) . . ? C16 C17 C17A 125.7(6) . . ? C17 C17A C17B 112.5(8) . . ? C17 C18 C19 106.4(6) . . ? C17 C18 C18A 128.0(7) . . ? C19 C18 C18A 125.6(7) . . ? C20 C19 N4 123.7(6) . . ? C20 C19 C18 125.0(7) . . ? N4 C19 C18 111.2(6) . . ? C19 C20 C1 126.8(7) . . ? N5 C21 C40 125.4(6) . . ? N5 C21 C22 111.2(6) . . ? C40 C21 C22 123.4(6) . . ? C23 C22 C21 106.6(6) . . ? C23 C22 C22A 128.0(7) . . ? C21 C22 C22A 124.8(7) . . ? C22B C22A C22 107.6(16) . . ? C22 C23 C24 107.8(6) . . ? C22 C23 C23A 124.3(7) . . ? C24 C23 C23A 127.8(7) . . ? N5 C24 C25 124.4(6) . . ? N5 C24 C23 109.1(6) . . ? C25 C24 C23 126.5(6) . . ? C24 C25 C26 124.8(6) . . ? C24 C25 C51 117.7(6) . . ? C26 C25 C51 117.0(6) . . ? N6 C26 C25 123.5(6) . . ? N6 C26 C27 110.0(5) . . ? C25 C26 C27 126.5(6) . . ? C28 C27 C26 106.5(6) . . ? C28 C27 C27A 123.1(6) . . ? C26 C27 C27A 130.3(6) . . ? C27 C28 C29 107.1(6) . . ? C27 C28 C28A 128.7(6) . . ? C29 C28 C28A 124.0(6) . . ? C28 C28A C28B 110.5(7) . . ? N6 C29 C30 126.0(6) . . ? N6 C29 C28 111.3(6) . . ? C30 C29 C28 122.7(6) . . ? C31 C30 C29 125.7(6) . . ? C30 C31 N7 124.4(6) . . ? C30 C31 C32 124.2(6) . . ? N7 C31 C32 111.4(5) . . ? C33 C32 C31 106.2(6) . . ? C33 C32 C32A 128.3(6) . . ? C31 C32 C32A 125.4(6) . . ? C32 C33 C34 106.5(6) . . ? C32 C33 C33A 128.2(6) . . ? C34 C33 C33A 125.2(6) . . ? C33 C33A C33B 112.9(6) . . ? C35 C34 N7 124.9(6) . . ? C35 C34 C33 123.5(6) . . ? N7 C34 C33 111.5(6) . . ? C34 C35 C36 124.5(6) . . ? N8 C36 C35 124.4(6) . . ? N8 C36 C37 111.6(6) . . ? C35 C36 C37 123.9(6) . . ? C38 C37 C36 107.2(6) . . ? C38 C37 C37A 127.2(7) . . ? C36 C37 C37A 125.5(7) . . ? C37B C37A C37 113.3(8) . . ? C37 C38 C39 105.6(6) . . ? C37 C38 C38A 128.4(7) . . ? C39 C38 C38A 126.1(7) . . ? C40 C39 N8 123.4(6) . . ? C40 C39 C38 124.8(7) . . ? N8 C39 C38 111.7(6) . . ? C39 C40 C21 126.9(7) . . ? C42 C41 O1 125.4(6) . . ? C42 C41 C46 123.9(6) . . ? O1 C41 C46 110.7(5) . . ? C41 C42 C43 115.1(6) . . ? C41 C42 C5 124.7(6) . . ? C43 C42 C5 120.1(6) . . ? C42 C43 C44 122.9(7) . . ? C45 C44 C43 120.4(7) . . ? C44 C45 C46 118.6(7) . . ? C45 C46 C41 119.0(6) . . ? C45 C46 C47 134.7(6) . . ? C41 C46 C47 106.3(6) . . ? C48 C47 C52 119.1(6) . . ? C48 C47 C46 134.5(6) . . ? C52 C47 C46 106.4(6) . . ? C49 C48 C47 118.6(7) . . ? C48 C49 C50 120.5(7) . . ? C51 C50 C49 122.9(7) . . ? C52 C51 C50 114.4(6) . . ? C52 C51 C25 125.6(6) . . ? C50 C51 C25 119.9(6) . . ? C51 C52 O1 124.5(5) . . ? C51 C52 C47 124.3(6) . . ? O1 C52 C47 111.1(5) . . ? Cl1S C3S Cl2S 122.8(15) . . ? Cl4S C4S Cl3S 123.3(19) . . ? _refine_diff_density_max 2.626 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.184 #===END data_i _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common Co2DPX _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C79 H82 Co2 N8 O' _chemical_formula_weight 1277.39 _chemical_melting_point ? _chemical_compound_source ? 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' '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 24.1310(5) _cell_length_b 10.6260(2) _cell_length_c 50.27170(10) _cell_angle_alpha 90.00 _cell_angle_beta 99.5120(10) _cell_angle_gamma 90.00 _cell_volume 12713.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method ? _exptl_crystal_F_000 5392 _exptl_absorpt_coefficient_mu 0.577 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25472 _diffrn_reflns_av_R_equivalents 0.1088 _diffrn_reflns_av_sigmaI/netI 0.1148 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -56 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 23.42 _reflns_number_total 9225 _reflns_number_observed 5810 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1105P)^2^+53.5971P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9212 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1554 _refine_ls_R_factor_obs 0.0848 _refine_ls_wR_factor_all 0.2646 _refine_ls_wR_factor_obs 0.2003 _refine_ls_goodness_of_fit_all 1.224 _refine_ls_goodness_of_fit_obs 1.198 _refine_ls_restrained_S_all 1.233 _refine_ls_restrained_S_obs 1.198 _refine_ls_shift/esd_max -0.009 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Co1 Co 0.30993(5) 0.06877(11) 0.12763(2) 0.0262(3) Uani 1 d . . Co2 Co 0.25465(4) -0.32904(11) 0.09966(2) 0.0254(3) Uani 1 d . . O O 0.3517(2) -0.3502(5) 0.19880(10) 0.0279(13) Uani 1 d . . N8 N 0.3322(3) -0.3254(6) 0.11882(12) 0.025(2) Uani 1 d . . N7 N 0.3522(3) 0.1985(6) 0.11171(12) 0.028(2) Uani 1 d . . N6 N 0.2668(3) -0.0545(6) 0.14452(13) 0.025(2) Uani 1 d . . N5 N 0.3762(3) 0.0268(6) 0.15400(13) 0.029(2) Uani 1 d . . N4 N 0.2378(3) -0.4589(6) 0.12500(13) 0.026(2) Uani 1 d . . N3 N 0.1778(3) -0.3402(7) 0.07885(13) 0.031(2) Uani 1 d . . N2 N 0.2713(3) -0.1978(7) 0.07434(13) 0.030(2) Uani 1 d . . C80 C 0.3611(3) -0.5445(8) 0.1788(2) 0.026(2) Uani 1 d . . C79 C 0.3791(3) -0.0465(8) 0.1773(2) 0.025(2) Uani 1 d . . C78 C 0.4187(3) -0.3778(8) 0.1453(2) 0.027(2) Uani 1 d . . C77 C 0.4099(4) 0.2124(8) 0.1162(2) 0.031(2) Uani 1 d . . C76 C 0.3533(3) -0.2734(8) 0.2207(2) 0.026(2) Uani 1 d . . C75 C 0.2331(3) -0.1851(7) 0.1753(2) 0.026(2) Uani 1 d . . N1 N 0.2437(3) 0.1138(7) 0.10175(14) 0.031(2) Uani 1 d . . C74 C 0.3871(3) -0.5238(8) 0.2277(2) 0.032(2) Uani 1 d . . C73 C 0.3662(3) -0.3159(8) 0.2470(2) 0.030(2) Uani 1 d . . C72 C 0.2722(3) -0.5109(8) 0.1472(2) 0.027(2) Uani 1 d . . C71 C 0.1821(3) -0.0534(8) 0.1104(2) 0.029(2) Uani 1 d . . H71A H 0.1496(3) -0.0979(8) 0.1037(2) 0.035 Uiso 1 calc R . C70 C 0.2800(3) -0.1120(8) 0.1697(2) 0.029(2) Uani 1 d . . C69 C 0.1859(3) -0.5113(8) 0.1257(2) 0.028(2) Uani 1 d . . C68 C 0.3200(3) -0.1314(8) 0.0763(2) 0.031(2) Uani 1 d . . C67 C 0.2380(4) -0.1516(8) 0.0517(2) 0.033(2) Uani 1 d . . C66 C 0.1339(3) -0.4116(8) 0.0850(2) 0.029(2) Uani 1 d . . C65 C 0.3298(3) -0.4857(7) 0.1533(2) 0.024(2) Uani 1 d . . C64 C 0.3825(4) -0.4522(8) 0.2533(2) 0.033(2) Uani 1 d . . C63 C 0.4459(4) 0.1460(8) 0.1346(2) 0.032(2) Uani 1 d . . H63A H 0.4842(4) 0.1584(8) 0.1348(2) 0.038 Uiso 1 calc R . C62 C 0.3750(3) -0.2465(8) 0.1137(2) 0.027(2) Uani 1 d . . C61 C 0.1378(4) -0.6639(9) 0.1557(2) 0.039(2) Uani 1 d . . H61A H 0.1369(4) -0.6523(9) 0.1748(2) 0.047 Uiso 1 calc R . H61B H 0.1033(4) -0.6288(9) 0.1458(2) 0.047 Uiso 1 calc R . C60 C 0.3672(3) -0.4736(7) 0.2024(2) 0.022(2) Uani 1 d . . C59 C 0.3172(4) -0.0380(8) 0.0546(2) 0.031(2) Uani 1 d . . C58 C 0.4375(3) -0.0567(8) 0.1903(2) 0.027(2) Uani 1 d . . C57 C 0.3389(4) -0.0627(9) 0.2351(2) 0.036(2) Uani 1 d . . H57A H 0.3307(4) 0.0215(9) 0.2313(2) 0.043 Uiso 1 calc R . C56 C 0.4828(4) -0.2167(8) 0.1269(2) 0.032(2) Uani 1 d . . H56A H 0.5088(4) -0.2272(8) 0.1437(2) 0.039 Uiso 1 calc R . H56B H 0.4769(4) -0.1272(8) 0.1239(2) 0.039 Uiso 1 calc R . C55 C 0.4308(3) 0.0626(8) 0.1528(2) 0.028(2) Uani 1 d . . C54 C 0.2354(4) 0.2177(9) 0.0851(2) 0.033(2) Uani 1 d . . C53 C 0.1347(3) -0.2318(9) 0.1488(2) 0.035(2) Uani 1 d . . H53A H 0.1348(3) -0.3119(9) 0.1581(2) 0.042 Uiso 1 calc R . H53B H 0.1223(3) -0.2469(9) 0.1298(2) 0.042 Uiso 1 calc R . C52 C 0.1800(4) 0.2170(9) 0.0695(2) 0.034(2) Uani 1 d . . C51 C 0.4684(3) 0.0107(8) 0.1751(2) 0.029(2) Uani 1 d . . C5 C 0.3723(4) 0.4804(9) 0.0691(2) 0.045(3) Uani 1 d . . H5A H 0.3992(4) 0.5439(9) 0.0767(2) 0.054 Uiso 1 calc R . H5B H 0.3350(4) 0.5163(9) 0.0679(2) 0.054 Uiso 1 calc R . C50 C 0.2656(4) -0.0525(8) 0.0392(2) 0.032(2) Uani 1 d . . C49 C 0.2396(3) -0.5922(8) 0.1619(2) 0.027(2) Uani 1 d . . C48 C 0.3796(4) -0.6683(9) 0.1803(2) 0.038(2) Uani 1 d . . H48A H 0.3767(4) -0.7171(9) 0.1647(2) 0.045 Uiso 1 calc R . C47 C 0.1866(4) -0.5924(8) 0.1485(2) 0.028(2) Uani 1 d . . C46 C 0.3629(4) 0.0502(9) 0.0504(2) 0.042(2) Uani 1 d . . H46A H 0.3945(4) 0.0389(9) 0.0645(2) 0.063 Uiso 1 calc R . H46B H 0.3496(4) 0.1352(9) 0.0506(2) 0.063 Uiso 1 calc R . H46C H 0.3740(4) 0.0332(9) 0.0333(2) 0.063 Uiso 1 calc R . C45 C 0.1930(3) -0.1803(8) 0.1530(2) 0.028(2) Uani 1 d . . C44 C 0.4255(4) 0.3171(9) 0.1002(2) 0.033(2) Uani 1 d . . C43 C 0.5306(3) 0.0334(8) 0.1815(2) 0.033(2) Uani 1 d . . H43A H 0.5441(3) 0.0601(8) 0.1652(2) 0.039 Uiso 1 calc R . H43B H 0.5495(3) -0.0447(8) 0.1875(2) 0.039 Uiso 1 calc R . C42 C 0.1944(4) 0.0469(8) 0.0961(2) 0.029(2) Uani 1 d . . C41 C 0.1381(4) -0.4896(8) 0.1069(2) 0.031(2) Uani 1 d . . H41A H 0.1057(4) -0.5321(8) 0.1094(2) 0.038 Uiso 1 calc R . C40 C 0.0839(4) -0.3922(10) 0.0657(2) 0.043(2) Uani 1 d . . C38 C 0.3412(3) -0.1475(8) 0.2142(2) 0.028(2) Uani 1 d . . C37 C 0.3578(3) -0.4024(8) 0.1392(2) 0.025(2) Uani 1 d . . C36 C 0.2132(3) -0.0965(8) 0.1343(2) 0.028(2) Uani 1 d . . C35 C 0.3321(3) 0.2928(8) 0.0939(2) 0.032(2) Uani 1 d . . C34 C 0.4023(4) -0.7179(9) 0.2050(2) 0.041(2) Uani 1 d . . H34A H 0.4159(4) -0.8000(9) 0.2060(2) 0.049 Uiso 1 calc R . C33 C 0.3327(3) -0.0999(7) 0.1855(2) 0.024(2) Uani 1 d . . C32 C 0.3644(4) -0.2277(9) 0.2672(2) 0.037(2) Uani 1 d . . H32A H 0.3739(4) -0.2524(9) 0.2851(2) 0.045 Uiso 1 calc R . C31 C 0.4051(4) -0.6494(9) 0.2277(2) 0.041(2) Uani 1 d . . H31A H 0.4196(4) -0.6870(9) 0.2441(2) 0.049 Uiso 1 calc R . C30 C 0.1392(4) -0.8010(9) 0.1500(2) 0.058(3) Uani 1 d . . H30A H 0.1068(4) -0.8408(9) 0.1551(2) 0.087 Uiso 1 calc R . H30B H 0.1727(4) -0.8371(9) 0.1600(2) 0.087 Uiso 1 calc R . H30C H 0.1390(4) -0.8136(9) 0.1310(2) 0.087 Uiso 1 calc R . C29 C 0.1550(4) 0.1080(9) 0.0753(2) 0.034(2) Uani 1 d . . C28 C 0.0969(4) -0.3101(9) 0.0474(2) 0.041(2) Uani 1 d . . C27 C 0.2765(4) 0.3039(8) 0.0827(2) 0.033(2) Uani 1 d . . H27A H 0.2658(4) 0.3760(8) 0.0727(2) 0.039 Uiso 1 calc R . C26 C 0.1553(4) -0.2768(9) 0.0555(2) 0.034(2) Uani 1 d . . C25 C 0.3489(4) -0.1042(9) 0.2615(2) 0.043(3) Uani 1 d . . H25A H 0.3451(4) -0.0490(9) 0.2754(2) 0.051 Uiso 1 calc R . C24 C 0.2268(3) -0.2623(9) 0.1996(2) 0.033(2) Uani 1 d . . H24A H 0.2597(3) -0.2527(9) 0.2130(2) 0.050 Uiso 1 calc R . H24B H 0.2224(3) -0.3493(9) 0.1945(2) 0.050 Uiso 1 calc R . H24C H 0.1944(3) -0.2345(9) 0.2067(2) 0.050 Uiso 1 calc R . C23 C 0.3676(4) -0.1500(8) 0.0947(2) 0.035(2) Uani 1 d . . H23A H 0.3972(4) -0.0940(8) 0.0946(2) 0.042 Uiso 1 calc R . C22 C 0.3772(4) 0.3685(8) 0.0877(2) 0.035(2) Uani 1 d . . C21 C 0.1833(4) -0.1911(9) 0.0428(2) 0.034(2) Uani 1 d . . H21A H 0.1644(4) -0.1562(9) 0.0269(2) 0.041 Uiso 1 calc R . C20 C 0.0287(4) -0.4554(10) 0.0665(2) 0.055(3) Uani 1 d . . H20A H 0.0321(4) -0.5093(10) 0.0820(2) 0.083 Uiso 1 calc R . H20B H 0.0183(4) -0.5046(10) 0.0504(2) 0.083 Uiso 1 calc R . H20C H 0.0005(4) -0.3928(10) 0.0676(2) 0.083 Uiso 1 calc R . C19 C 0.2426(4) 0.0134(10) 0.0136(2) 0.046(3) Uani 1 d . . H19A H 0.2589(4) 0.0969(10) 0.0138(2) 0.055 Uiso 1 calc R . H19B H 0.2023(4) 0.0228(10) 0.0124(2) 0.055 Uiso 1 calc R . C18 C 0.4638(3) -0.4460(9) 0.1636(2) 0.041(2) Uani 1 d . . H18A H 0.4474(3) -0.5127(9) 0.1726(2) 0.062 Uiso 1 calc R . H18B H 0.4829(3) -0.3885(9) 0.1768(2) 0.062 Uiso 1 calc R . H18C H 0.4901(3) -0.4806(9) 0.1532(2) 0.062 Uiso 1 calc R . C17 C 0.3363(4) -0.5149(10) 0.2667(2) 0.048(3) Uani 1 d . . H17A H 0.3327(4) -0.4709(10) 0.2830(2) 0.072 Uiso 1 calc R . H17B H 0.3462(4) -0.6010(10) 0.2708(2) 0.072 Uiso 1 calc R . H17C H 0.3012(4) -0.5118(10) 0.2545(2) 0.072 Uiso 1 calc R . C16 C 0.0938(3) -0.1436(9) 0.1591(2) 0.039(2) Uani 1 d . . H16A H 0.0569(3) -0.1802(9) 0.1560(2) 0.059 Uiso 1 calc R . H16B H 0.0931(3) -0.0647(9) 0.1498(2) 0.059 Uiso 1 calc R . H16C H 0.1055(3) -0.1299(9) 0.1781(2) 0.059 Uiso 1 calc R . C15 C 0.0978(4) 0.0606(10) 0.0642(2) 0.046(3) Uani 1 d . . H15A H 0.0919(4) -0.0192(10) 0.0722(2) 0.069 Uiso 1 calc R . H15B H 0.0944(4) 0.0509(10) 0.0450(2) 0.069 Uiso 1 calc R . H15C H 0.0702(4) 0.1196(10) 0.0682(2) 0.069 Uiso 1 calc R . C14 C 0.4272(3) -0.2784(8) 0.1296(2) 0.030(2) Uani 1 d . . C13 C 0.4625(4) -0.1320(10) 0.2143(2) 0.045(3) Uani 1 d . . H13A H 0.4331(4) -0.1719(10) 0.2219(2) 0.067 Uiso 1 calc R . H13B H 0.4837(4) -0.0777(10) 0.2274(2) 0.067 Uiso 1 calc R . H13C H 0.4869(4) -0.1951(10) 0.2089(2) 0.067 Uiso 1 calc R . C12 C 0.2559(4) -0.6654(11) 0.1877(2) 0.054(3) Uani 1 d . . H12A H 0.2952(4) -0.6538(11) 0.1943(2) 0.081 Uiso 1 calc R . H12B H 0.2483(4) -0.7532(11) 0.1842(2) 0.081 Uiso 1 calc R . H12C H 0.2344(4) -0.6360(11) 0.2009(2) 0.081 Uiso 1 calc R . C11 C 0.4384(4) -0.4570(10) 0.2732(2) 0.050(3) Uani 1 d . . H11A H 0.4346(4) -0.4114(10) 0.2893(2) 0.074 Uiso 1 calc R . H11B H 0.4676(4) -0.4196(10) 0.2650(2) 0.074 Uiso 1 calc R . H11C H 0.4479(4) -0.5430(10) 0.2777(2) 0.074 Uiso 1 calc R . C10 C 0.0597(4) -0.2594(11) 0.0221(2) 0.056(3) Uani 1 d . . H10A H 0.0209(4) -0.2602(11) 0.0249(2) 0.067 Uiso 1 calc R . H10B H 0.0700(4) -0.1727(11) 0.0193(2) 0.067 Uiso 1 calc R . C9 C 0.1535(4) 0.3177(10) 0.0502(2) 0.052(3) Uani 1 d . . H9A H 0.1156(4) 0.3330(10) 0.0535(2) 0.063 Uiso 1 calc R . H9B H 0.1747(4) 0.3951(10) 0.0540(2) 0.063 Uiso 1 calc R . C8 C 0.5455(4) 0.1326(10) 0.2031(2) 0.053(3) Uani 1 d . . H8A H 0.5855(4) 0.1444(10) 0.2066(2) 0.079 Uiso 1 calc R . H8B H 0.5330(4) 0.1058(10) 0.2193(2) 0.079 Uiso 1 calc R . H8C H 0.5275(4) 0.2105(10) 0.1971(2) 0.079 Uiso 1 calc R . C7 C 0.5084(4) -0.2729(10) 0.1039(2) 0.049(3) Uani 1 d . . H7A H 0.5434(4) -0.2317(10) 0.1028(2) 0.074 Uiso 1 calc R . H7B H 0.4830(4) -0.2614(10) 0.0872(2) 0.074 Uiso 1 calc R . H7C H 0.5149(4) -0.3612(10) 0.1070(2) 0.074 Uiso 1 calc R . C6 C 0.2552(5) -0.0584(12) -0.0112(2) 0.066(3) Uani 1 d . . H6A H 0.2397(5) -0.0133(12) -0.0272(2) 0.099 Uiso 1 calc R . H6B H 0.2386(5) -0.1406(12) -0.0116(2) 0.099 Uiso 1 calc R . H6C H 0.2951(5) -0.0663(12) -0.0102(2) 0.099 Uiso 1 calc R . C5 C 0.4845(4) 0.3556(10) 0.0988(2) 0.049(3) Uani 1 d . . H5C H 0.5101(4) 0.3011(10) 0.1100(2) 0.073 Uiso 1 calc R . H5D H 0.4903(4) 0.4408(10) 0.1049(2) 0.073 Uiso 1 calc R . H5E H 0.4909(4) 0.3495(10) 0.0805(2) 0.073 Uiso 1 calc R . C4 C 0.1513(6) 0.2860(12) 0.0214(2) 0.085(4) Uani 1 d . . H4A H 0.1341(6) 0.3539(12) 0.0105(2) 0.127 Uiso 1 calc R . H4B H 0.1296(6) 0.2107(12) 0.0173(2) 0.127 Uiso 1 calc R . H4C H 0.1887(6) 0.2729(12) 0.0178(2) 0.127 Uiso 1 calc R . C3 C 0.3826(5) 0.4471(11) 0.0410(2) 0.065(3) Uani 1 d . . H3A H 0.3789(5) 0.5213(11) 0.0299(2) 0.097 Uiso 1 calc R . H3B H 0.3556(5) 0.3855(11) 0.0332(2) 0.097 Uiso 1 calc R . H3C H 0.4198(5) 0.4135(11) 0.0420(2) 0.097 Uiso 1 calc R . C2 C 0.0648(6) -0.3349(13) -0.0028(2) 0.090(5) Uani 1 d . . H2A H 0.0408(6) -0.2993(13) -0.0180(2) 0.134 Uiso 1 calc R . H2B H 0.0539(6) -0.4203(13) -0.0003(2) 0.134 Uiso 1 calc R . H2C H 0.1031(6) -0.3330(13) -0.0058(2) 0.134 Uiso 1 calc R . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0291(7) 0.0256(7) 0.0238(6) 0.0013(5) 0.0041(5) -0.0014(5) Co2 0.0233(6) 0.0292(7) 0.0233(6) -0.0004(5) 0.0022(5) -0.0031(5) O 0.042(4) 0.017(3) 0.026(3) 0.001(3) 0.007(3) 0.001(3) N8 0.029(4) 0.028(4) 0.017(3) 0.003(3) 0.000(3) 0.004(3) N7 0.041(5) 0.024(4) 0.018(4) 0.002(3) -0.001(3) -0.004(3) N6 0.021(4) 0.020(4) 0.035(4) -0.001(3) 0.007(3) 0.003(3) N5 0.034(4) 0.027(4) 0.027(4) -0.009(3) 0.003(3) -0.002(3) N4 0.027(4) 0.023(4) 0.028(4) -0.007(3) 0.007(3) 0.000(3) N3 0.028(4) 0.035(4) 0.029(4) -0.006(4) -0.001(3) 0.000(4) N2 0.033(4) 0.031(4) 0.024(4) -0.004(3) 0.003(3) 0.002(3) C80 0.024(5) 0.029(5) 0.025(5) -0.003(4) 0.003(4) -0.003(4) C79 0.027(5) 0.024(5) 0.022(4) 0.004(4) -0.001(4) -0.002(4) C78 0.032(5) 0.024(5) 0.026(5) 0.005(4) 0.005(4) 0.004(4) C77 0.036(6) 0.025(5) 0.033(5) 0.001(4) 0.004(4) -0.009(4) C76 0.025(5) 0.025(5) 0.028(5) -0.008(4) 0.003(4) 0.005(4) C75 0.031(5) 0.015(5) 0.033(5) -0.002(4) 0.005(4) 0.002(4) N1 0.028(4) 0.026(4) 0.039(4) -0.001(4) 0.011(3) -0.001(3) C74 0.029(5) 0.035(6) 0.032(5) 0.004(4) 0.007(4) 0.001(4) C73 0.027(5) 0.034(5) 0.027(5) 0.004(4) 0.000(4) -0.003(4) C72 0.026(5) 0.028(5) 0.024(5) -0.005(4) -0.004(4) -0.002(4) C71 0.027(5) 0.029(5) 0.030(5) -0.008(4) -0.004(4) 0.001(4) C70 0.031(5) 0.018(5) 0.041(5) 0.003(4) 0.012(4) 0.000(4) C69 0.023(5) 0.029(5) 0.032(5) -0.015(4) 0.005(4) -0.005(4) C68 0.026(5) 0.031(5) 0.034(5) -0.004(4) 0.002(4) -0.003(4) C67 0.036(6) 0.036(6) 0.026(5) 0.001(4) 0.007(4) 0.007(4) C66 0.020(5) 0.037(6) 0.027(5) -0.004(4) -0.003(4) -0.003(4) C65 0.029(5) 0.021(5) 0.024(4) -0.013(4) 0.006(4) 0.000(4) C64 0.036(5) 0.038(6) 0.026(5) 0.007(4) 0.007(4) 0.005(4) C63 0.030(5) 0.041(6) 0.023(5) 0.000(4) 0.004(4) -0.004(4) C62 0.031(5) 0.032(5) 0.021(4) -0.006(4) 0.011(4) -0.008(4) C61 0.030(5) 0.052(7) 0.038(5) 0.002(5) 0.013(4) 0.006(5) C60 0.018(4) 0.019(5) 0.029(5) 0.002(4) 0.002(4) 0.004(3) C59 0.043(6) 0.025(5) 0.025(5) 0.011(4) 0.005(4) -0.006(4) C58 0.036(5) 0.024(5) 0.021(4) -0.003(4) 0.003(4) 0.003(4) C57 0.054(6) 0.027(5) 0.026(5) -0.002(4) 0.007(4) -0.001(5) C56 0.037(5) 0.028(5) 0.032(5) -0.003(4) 0.006(4) -0.009(4) C55 0.029(5) 0.033(5) 0.020(4) -0.006(4) 0.001(4) -0.004(4) C54 0.036(5) 0.041(6) 0.023(5) 0.008(4) 0.003(4) 0.009(5) C53 0.034(5) 0.036(6) 0.034(5) 0.002(4) 0.003(4) -0.010(4) C52 0.034(5) 0.040(6) 0.028(5) 0.001(4) 0.004(4) 0.005(5) C51 0.027(5) 0.021(5) 0.038(5) -0.006(4) 0.001(4) -0.002(4) C5 0.058(7) 0.032(6) 0.043(6) -0.002(5) 0.007(5) -0.006(5) C50 0.044(6) 0.033(5) 0.020(4) 0.003(4) 0.005(4) -0.001(4) C49 0.030(5) 0.026(5) 0.027(5) 0.001(4) 0.008(4) -0.008(4) C48 0.038(6) 0.036(6) 0.040(6) 0.005(5) 0.011(4) 0.001(5) C47 0.037(6) 0.018(5) 0.030(5) 0.001(4) 0.011(4) -0.007(4) C46 0.043(6) 0.042(6) 0.041(6) 0.011(5) 0.006(5) -0.007(5) C45 0.028(5) 0.025(5) 0.032(5) 0.004(4) 0.005(4) -0.005(4) C44 0.038(6) 0.036(6) 0.025(5) 0.004(4) 0.002(4) -0.007(4) C43 0.027(5) 0.038(6) 0.031(5) 0.002(4) 0.001(4) 0.000(4) C42 0.034(5) 0.031(5) 0.025(5) -0.003(4) 0.011(4) 0.005(4) C41 0.028(5) 0.029(5) 0.036(5) -0.007(4) 0.002(4) -0.007(4) C40 0.023(5) 0.051(7) 0.054(6) 0.000(5) 0.004(5) -0.001(5) C38 0.029(5) 0.025(5) 0.030(5) -0.004(4) 0.008(4) -0.001(4) C37 0.029(5) 0.026(5) 0.022(4) -0.013(4) 0.008(4) 0.000(4) C36 0.025(5) 0.028(5) 0.029(5) -0.004(4) 0.004(4) -0.001(4) C35 0.026(5) 0.032(6) 0.037(5) -0.004(4) 0.005(4) -0.002(4) C34 0.047(6) 0.030(6) 0.049(6) -0.008(5) 0.018(5) 0.007(5) C33 0.025(5) 0.020(5) 0.028(5) -0.006(4) 0.004(4) 0.003(4) C32 0.051(6) 0.036(6) 0.024(5) 0.004(4) 0.003(4) -0.004(5) C31 0.045(6) 0.042(7) 0.036(6) 0.019(5) 0.006(4) 0.000(5) C30 0.054(7) 0.035(7) 0.091(9) -0.006(6) 0.030(6) -0.012(5) C29 0.030(5) 0.048(6) 0.022(5) -0.002(4) -0.004(4) 0.004(5) C28 0.033(6) 0.045(6) 0.043(6) -0.003(5) 0.000(4) 0.003(5) C27 0.043(6) 0.022(5) 0.033(5) 0.001(4) 0.006(4) 0.002(4) C26 0.032(5) 0.039(6) 0.031(5) 0.000(4) 0.007(4) 0.002(4) C25 0.060(7) 0.047(7) 0.022(5) -0.015(5) 0.008(5) -0.003(5) C24 0.029(5) 0.041(6) 0.032(5) -0.001(4) 0.011(4) -0.001(4) C23 0.037(6) 0.031(6) 0.037(5) -0.005(4) 0.009(4) -0.008(4) C22 0.047(6) 0.032(6) 0.024(5) -0.005(4) 0.003(4) -0.015(5) C21 0.034(5) 0.039(6) 0.027(5) -0.005(4) -0.004(4) 0.010(5) C20 0.031(6) 0.062(8) 0.070(7) -0.003(6) -0.002(5) -0.004(5) C19 0.050(6) 0.051(7) 0.035(6) 0.012(5) 0.006(5) 0.006(5) C18 0.024(5) 0.053(7) 0.046(6) 0.008(5) 0.004(4) -0.002(5) C17 0.063(7) 0.048(7) 0.034(5) 0.008(5) 0.008(5) -0.009(5) C16 0.019(5) 0.040(6) 0.057(6) 0.003(5) 0.002(4) -0.009(4) C15 0.039(6) 0.063(7) 0.036(5) 0.002(5) 0.005(5) 0.010(5) C14 0.017(5) 0.038(6) 0.035(5) -0.004(4) 0.005(4) -0.003(4) C13 0.025(5) 0.064(7) 0.042(6) 0.013(5) -0.007(4) -0.002(5) C12 0.040(6) 0.079(8) 0.043(6) 0.024(6) 0.007(5) -0.015(6) C11 0.057(7) 0.053(7) 0.034(5) -0.003(5) -0.010(5) 0.010(5) C10 0.042(6) 0.069(8) 0.053(7) -0.004(6) -0.003(5) 0.003(6) C9 0.058(7) 0.049(7) 0.048(6) 0.014(5) 0.002(5) 0.012(6) C8 0.030(6) 0.058(7) 0.067(7) -0.006(6) -0.003(5) -0.011(5) C7 0.053(7) 0.051(7) 0.048(6) -0.015(5) 0.019(5) -0.022(5) C6 0.073(8) 0.086(9) 0.038(6) 0.008(6) 0.005(6) 0.013(7) C5 0.046(6) 0.049(7) 0.052(6) 0.010(5) 0.006(5) -0.015(5) C4 0.152(13) 0.062(9) 0.040(7) 0.009(6) 0.016(8) 0.018(9) C3 0.082(9) 0.071(9) 0.038(6) 0.013(6) 0.002(6) 0.004(7) C2 0.112(11) 0.094(11) 0.048(7) -0.019(7) -0.030(7) 0.018(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.946(7) . ? Co1 N6 1.952(7) . ? Co1 N5 1.953(7) . ? Co1 N7 1.962(7) . ? Co2 N8 1.959(6) . ? Co2 N4 1.965(7) . ? Co2 N2 1.974(7) . ? Co2 N3 1.976(7) . ? O C76 1.366(9) . ? O C60 1.367(9) . ? N8 C37 1.376(10) . ? N8 C62 1.387(10) . ? N7 C35 1.377(10) . ? N7 C77 1.383(11) . ? N6 C36 1.385(10) . ? N6 C70 1.393(10) . ? N5 C55 1.381(10) . ? N5 C79 1.400(10) . ? N4 C69 1.377(10) . ? N4 C72 1.390(10) . ? N3 C66 1.378(10) . ? N3 C26 1.384(11) . ? N2 C68 1.361(10) . ? N2 C67 1.372(10) . ? C80 C48 1.387(12) . ? C80 C60 1.391(11) . ? C80 C65 1.511(11) . ? C79 C33 1.376(11) . ? C79 C58 1.457(11) . ? C78 C14 1.357(11) . ? C78 C37 1.473(11) . ? C78 C18 1.491(11) . ? C77 C63 1.358(11) . ? C77 C44 1.456(12) . ? C76 C73 1.382(11) . ? C76 C38 1.396(12) . ? C75 C45 1.357(11) . ? C75 C70 1.438(11) . ? C75 C24 1.499(11) . ? N1 C42 1.375(11) . ? N1 C54 1.379(11) . ? C74 C60 1.391(11) . ? C74 C31 1.404(13) . ? C74 C64 1.516(12) . ? C73 C32 1.389(12) . ? C73 C64 1.521(12) . ? C72 C65 1.400(11) . ? C72 C49 1.451(11) . ? C71 C42 1.348(12) . ? C71 C36 1.383(11) . ? C70 C33 1.391(11) . ? C69 C41 1.384(11) . ? C69 C47 1.430(11) . ? C68 C23 1.365(11) . ? C68 C59 1.467(11) . ? C67 C21 1.388(12) . ? C67 C50 1.444(12) . ? C66 C41 1.371(12) . ? C66 C40 1.430(12) . ? C65 C37 1.379(11) . ? C64 C11 1.542(12) . ? C64 C17 1.543(12) . ? C63 C55 1.368(11) . ? C62 C23 1.393(12) . ? C62 C14 1.416(11) . ? C61 C30 1.487(13) . ? C61 C47 1.497(11) . ? C59 C50 1.361(12) . ? C59 C46 1.489(12) . ? C58 C51 1.358(11) . ? C58 C13 1.486(11) . ? C57 C25 1.381(12) . ? C57 C38 1.391(11) . ? C56 C14 1.518(11) . ? C56 C7 1.524(12) . ? C55 C51 1.430(11) . ? C54 C27 1.370(12) . ? C54 C52 1.435(12) . ? C53 C45 1.492(11) . ? C53 C16 1.513(12) . ? C52 C29 1.361(12) . ? C52 C9 1.511(12) . ? C51 C43 1.503(11) . ? C5 C22 1.504(12) . ? C5 C3 1.520(13) . ? C50 C19 1.488(12) . ? C49 C47 1.344(11) . ? C49 C12 1.505(12) . ? C48 C34 1.378(12) . ? C45 C36 1.437(11) . ? C44 C22 1.345(12) . ? C44 C5 1.495(12) . ? C43 C8 1.514(12) . ? C42 C29 1.444(11) . ? C40 C28 1.342(13) . ? C40 C20 1.498(13) . ? C38 C33 1.510(11) . ? C35 C27 1.371(12) . ? C35 C22 1.429(12) . ? C34 C31 1.347(12) . ? C32 C25 1.382(13) . ? C29 C15 1.488(12) . ? C28 C26 1.444(12) . ? C28 C10 1.528(13) . ? C26 C21 1.355(12) . ? C19 C6 1.533(13) . ? C10 C2 1.508(14) . ? C9 C4 1.478(13) . ? 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 Co1 N6 91.0(3) . . ? N1 Co1 N5 178.8(3) . . ? N6 Co1 N5 89.3(3) . . ? N1 Co1 N7 88.8(3) . . ? N6 Co1 N7 177.4(3) . . ? N5 Co1 N7 90.9(3) . . ? N8 Co2 N4 88.7(3) . . ? N8 Co2 N2 91.3(3) . . ? N4 Co2 N2 179.6(3) . . ? N8 Co2 N3 176.6(3) . . ? N4 Co2 N3 91.4(3) . . ? N2 Co2 N3 88.5(3) . . ? C76 O C60 119.8(6) . . ? C37 N8 C62 104.0(6) . . ? C37 N8 Co2 129.0(6) . . ? C62 N8 Co2 126.9(5) . . ? C35 N7 C77 105.3(7) . . ? C35 N7 Co1 128.8(6) . . ? C77 N7 Co1 125.9(5) . . ? C36 N6 C70 104.7(6) . . ? C36 N6 Co1 126.0(5) . . ? C70 N6 Co1 129.1(5) . . ? C55 N5 C79 105.9(7) . . ? C55 N5 Co1 126.0(6) . . ? C79 N5 Co1 128.1(5) . . ? C69 N4 C72 104.0(7) . . ? C69 N4 Co2 125.9(6) . . ? C72 N4 Co2 129.8(5) . . ? C66 N3 C26 104.4(7) . . ? C66 N3 Co2 127.1(5) . . ? C26 N3 Co2 128.5(6) . . ? C68 N2 C67 104.7(7) . . ? C68 N2 Co2 125.9(6) . . ? C67 N2 Co2 129.4(6) . . ? C48 C80 C60 118.8(8) . . ? C48 C80 C65 123.2(7) . . ? C60 C80 C65 117.8(7) . . ? C33 C79 N5 123.3(7) . . ? C33 C79 C58 127.5(7) . . ? N5 C79 C58 109.1(7) . . ? C14 C78 C37 105.0(7) . . ? C14 C78 C18 124.9(8) . . ? C37 C78 C18 130.0(8) . . ? C63 C77 N7 124.7(8) . . ? C63 C77 C44 125.3(8) . . ? N7 C77 C44 109.7(7) . . ? O C76 C73 123.1(8) . . ? O C76 C38 114.0(7) . . ? C73 C76 C38 122.9(8) . . ? C45 C75 C70 107.1(7) . . ? C45 C75 C24 122.6(7) . . ? C70 C75 C24 130.2(7) . . ? C42 N1 C54 104.7(7) . . ? C42 N1 Co1 126.7(6) . . ? C54 N1 Co1 128.6(6) . . ? C60 C74 C31 115.1(8) . . ? C60 C74 C64 121.5(8) . . ? C31 C74 C64 122.9(8) . . ? C76 C73 C32 116.7(8) . . ? C76 C73 C64 121.5(8) . . ? C32 C73 C64 121.8(7) . . ? N4 C72 C65 122.6(8) . . ? N4 C72 C49 110.2(7) . . ? C65 C72 C49 127.2(8) . . ? C42 C71 C36 126.1(8) . . ? C33 C70 N6 122.0(7) . . ? C33 C70 C75 127.7(8) . . ? N6 C70 C75 110.3(7) . . ? N4 C69 C41 125.0(8) . . ? N4 C69 C47 112.0(7) . . ? C41 C69 C47 123.0(8) . . ? N2 C68 C23 126.3(8) . . ? N2 C68 C59 111.3(7) . . ? C23 C68 C59 122.3(8) . . ? N2 C67 C21 123.7(8) . . ? N2 C67 C50 111.9(8) . . ? C21 C67 C50 124.3(8) . . ? C41 C66 N3 123.7(7) . . ? C41 C66 C40 125.0(8) . . ? N3 C66 C40 111.3(8) . . ? C37 C65 C72 124.3(8) . . ? C37 C65 C80 118.8(7) . . ? C72 C65 C80 116.6(7) . . ? C74 C64 C73 110.6(7) . . ? C74 C64 C11 110.7(7) . . ? C73 C64 C11 109.6(7) . . ? C74 C64 C17 108.2(7) . . ? C73 C64 C17 108.8(7) . . ? C11 C64 C17 108.8(7) . . ? C77 C63 C55 125.6(8) . . ? N8 C62 C23 123.9(8) . . ? N8 C62 C14 111.7(7) . . ? C23 C62 C14 124.4(8) . . ? C30 C61 C47 113.9(7) . . ? O C60 C74 122.3(7) . . ? O C60 C80 114.8(7) . . ? C74 C60 C80 123.0(8) . . ? C50 C59 C68 105.8(7) . . ? C50 C59 C46 128.2(8) . . ? C68 C59 C46 125.9(8) . . ? C51 C58 C79 106.7(7) . . ? C51 C58 C13 123.6(8) . . ? C79 C58 C13 129.5(8) . . ? C25 C57 C38 119.7(9) . . ? C14 C56 C7 111.8(7) . . ? C63 C55 N5 124.7(8) . . ? C63 C55 C51 124.7(8) . . ? N5 C55 C51 110.3(7) . . ? C27 C54 N1 123.5(8) . . ? C27 C54 C52 125.4(8) . . ? N1 C54 C52 111.0(8) . . ? C45 C53 C16 112.2(7) . . ? C29 C52 C54 106.9(8) . . ? C29 C52 C9 125.9(9) . . ? C54 C52 C9 127.1(9) . . ? C58 C51 C55 108.0(7) . . ? C58 C51 C43 126.0(8) . . ? C55 C51 C43 125.9(8) . . ? C22 C5 C3 112.6(8) . . ? C59 C50 C67 106.2(7) . . ? C59 C50 C19 127.8(8) . . ? C67 C50 C19 125.9(8) . . ? C47 C49 C72 107.2(7) . . ? C47 C49 C12 121.5(7) . . ? C72 C49 C12 131.3(8) . . ? C34 C48 C80 119.1(9) . . ? C49 C47 C69 106.6(7) . . ? C49 C47 C61 126.9(8) . . ? C69 C47 C61 126.5(8) . . ? C75 C45 C36 106.9(7) . . ? C75 C45 C53 129.0(8) . . ? C36 C45 C53 123.5(7) . . ? C22 C44 C77 106.7(8) . . ? C22 C44 C5 128.6(8) . . ? C77 C44 C5 124.7(8) . . ? C51 C43 C8 112.1(7) . . ? C71 C42 N1 123.9(8) . . ? C71 C42 C29 124.4(8) . . ? N1 C42 C29 111.2(8) . . ? C66 C41 C69 126.4(8) . . ? C28 C40 C66 106.9(8) . . ? C28 C40 C20 128.2(9) . . ? C66 C40 C20 124.9(9) . . ? C57 C38 C76 118.5(8) . . ? C57 C38 C33 119.2(7) . . ? C76 C38 C33 122.3(7) . . ? N8 C37 C65 124.6(7) . . ? N8 C37 C78 111.0(7) . . ? C65 C37 C78 124.3(7) . . ? C71 C36 N6 123.7(8) . . ? C71 C36 C45 125.2(8) . . ? N6 C36 C45 110.8(7) . . ? C27 C35 N7 122.9(8) . . ? C27 C35 C22 126.2(8) . . ? N7 C35 C22 110.7(7) . . ? C31 C34 C48 121.0(9) . . ? C79 C33 C70 125.4(7) . . ? C79 C33 C38 115.7(7) . . ? C70 C33 C38 118.9(7) . . ? C25 C32 C73 121.9(8) . . ? C34 C31 C74 122.8(9) . . ? C52 C29 C42 106.0(8) . . ? C52 C29 C15 128.5(8) . . ? C42 C29 C15 125.4(9) . . ? C40 C28 C26 107.1(8) . . ? C40 C28 C10 128.9(9) . . ? C26 C28 C10 124.0(9) . . ? C54 C27 C35 125.6(8) . . ? C21 C26 N3 124.8(8) . . ? C21 C26 C28 124.8(8) . . ? N3 C26 C28 110.3(8) . . ? C57 C25 C32 120.1(8) . . ? C68 C23 C62 124.8(8) . . ? C44 C22 C35 107.5(8) . . ? C44 C22 C5 125.9(8) . . ? C35 C22 C5 126.6(8) . . ? C26 C21 C67 125.0(8) . . ? C50 C19 C6 111.8(8) . . ? C78 C14 C62 108.0(7) . . ? C78 C14 C56 127.4(8) . . ? C62 C14 C56 124.3(8) . . ? C2 C10 C28 112.6(9) . . ? C4 C9 C52 114.2(9) . . ? _refine_diff_density_max 0.729 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.307