data_asb261 _audit_creation_method SHELXTL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H49 Cl2 Co N4 O7 S3' _chemical_formula_weight 851.78 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.6668(4) _cell_length_b 14.8717(8) _cell_length_c 17.4049(9) _cell_angle_alpha 92.5600(7) _cell_angle_beta 96.5047(7) _cell_angle_gamma 101.7540(7) _cell_volume 1925.67(18) _cell_formula_units_Z 2 _cell_measurement_temperature 88(2) _cell_measurement_reflns_used 7077 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 28.27 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.799 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8032 _exptl_absorpt_correction_T_max 0.9718 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 88(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22893 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 28.29 _reflns_number_total 9099 _reflns_number_gt 6795 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0359P)^2^+1.2323P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'difmap & geom' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9099 _refine_ls_number_parameters 477 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0639 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.0894 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 Co1 Co 0.77917(4) 0.81423(2) 0.301041(18) 0.00971(8) Uani 1 1 d . . . S1 S 0.65265(8) 0.61492(4) 0.19992(3) 0.01361(12) Uani 1 1 d . . . S2 S 0.62765(7) 0.97603(4) 0.21021(3) 0.01080(12) Uani 1 1 d . . . S3 S 0.70767(7) 0.80463(4) 0.48277(3) 0.01180(12) Uani 1 1 d . . . O1 O 0.4746(2) 0.62717(11) 0.21280(10) 0.0186(4) Uani 1 1 d . . . O2 O 0.7034(2) 0.53446(11) 0.23067(10) 0.0187(4) Uani 1 1 d . . . O3 O 0.4522(2) 0.92662(11) 0.22205(9) 0.0143(3) Uani 1 1 d . . . O4 O 0.6598(2) 0.98522(11) 0.13059(9) 0.0149(3) Uani 1 1 d . . . O5 O 0.5203(2) 0.78006(11) 0.44792(9) 0.0147(3) Uani 1 1 d . . . O6 O 0.7539(2) 0.88663(11) 0.53414(9) 0.0163(4) Uani 1 1 d . . . O7 O 0.5218(2) 0.77784(12) 0.29984(10) 0.0127(3) Uani 1 1 d . . . H1 H 0.488(5) 0.726(3) 0.275(2) 0.056(12) Uiso 1 1 d . . . H2 H 0.502(4) 0.771(2) 0.349(2) 0.038(9) Uiso 1 1 d . . . N1 N 1.0400(2) 0.84761(12) 0.30403(11) 0.0107(4) Uani 1 1 d . . . N2 N 0.7949(2) 0.70781(12) 0.23463(11) 0.0116(4) Uani 1 1 d . . . N3 N 0.7807(2) 0.93018(12) 0.25570(11) 0.0107(4) Uani 1 1 d . . . N4 N 0.8308(2) 0.81203(13) 0.41379(11) 0.0119(4) Uani 1 1 d . . . C1 C 1.0900(3) 0.79824(15) 0.23531(14) 0.0130(5) Uani 1 1 d . . . H1A H 1.2198 0.7980 0.2431 0.016 Uiso 1 1 calc R . . H1B H 1.0650 0.8303 0.1879 0.016 Uiso 1 1 calc R . . C2 C 0.9820(3) 0.70070(15) 0.22612(14) 0.0142(5) Uani 1 1 d . . . H2A H 0.9884 0.6717 0.1745 0.017 Uiso 1 1 calc R . . H2B H 1.0275 0.6634 0.2664 0.017 Uiso 1 1 calc R . . C3 C 0.6639(3) 0.60970(15) 0.09806(13) 0.0145(5) Uani 1 1 d . . . C4 C 0.7384(3) 0.54214(16) 0.06136(14) 0.0161(5) Uani 1 1 d . . . C5 C 0.7509(3) 0.54631(17) -0.01782(15) 0.0195(5) Uani 1 1 d . . . H5A H 0.7985 0.5006 -0.0433 0.023 Uiso 1 1 calc R . . C6 C 0.6974(3) 0.61392(17) -0.06083(14) 0.0205(5) Uani 1 1 d . . . C7 C 0.6229(3) 0.67835(17) -0.02353(15) 0.0221(6) Uani 1 1 d . . . H7A H 0.5842 0.7247 -0.0527 0.027 Uiso 1 1 calc R . . C8 C 0.6023(3) 0.67808(16) 0.05490(14) 0.0179(5) Uani 1 1 d . . . C9 C 0.8056(4) 0.46436(17) 0.10046(15) 0.0223(5) Uani 1 1 d . . . H9A H 0.8507 0.4274 0.0623 0.033 Uiso 1 1 calc R . . H9B H 0.7069 0.4254 0.1224 0.033 Uiso 1 1 calc R . . H9C H 0.9027 0.4900 0.1420 0.033 Uiso 1 1 calc R . . C10 C 0.7198(4) 0.6180(2) -0.14589(15) 0.0293(6) Uani 1 1 d . . . H10A H 0.7147 0.5558 -0.1685 0.044 Uiso 1 1 calc R . . H10B H 0.8360 0.6574 -0.1516 0.044 Uiso 1 1 calc R . . H10C H 0.6231 0.6433 -0.1727 0.044 Uiso 1 1 calc R . . C11 C 0.5151(4) 0.75107(18) 0.08835(16) 0.0279(6) Uani 1 1 d . . . H11A H 0.4962 0.7945 0.0491 0.042 Uiso 1 1 calc R . . H11B H 0.5933 0.7841 0.1336 0.042 Uiso 1 1 calc R . . H11C H 0.3992 0.7218 0.1040 0.042 Uiso 1 1 calc R . . C12 C 1.0932(3) 0.94977(15) 0.29890(13) 0.0120(4) Uani 1 1 d . . . H12A H 1.2162 0.9665 0.2843 0.014 Uiso 1 1 calc R . . H12B H 1.0910 0.9822 0.3496 0.014 Uiso 1 1 calc R . . C13 C 0.9609(3) 0.97652(15) 0.23826(13) 0.0121(5) Uani 1 1 d . . . H13A H 0.9727 1.0442 0.2409 0.015 Uiso 1 1 calc R . . H13B H 0.9812 0.9558 0.1858 0.015 Uiso 1 1 calc R . . C14 C 0.6600(3) 1.08925(15) 0.25675(13) 0.0119(4) Uani 1 1 d . . . C15 C 0.6333(3) 1.09609(16) 0.33567(14) 0.0138(5) Uani 1 1 d . . . C16 C 0.6434(3) 1.18312(16) 0.37108(14) 0.0167(5) Uani 1 1 d . . . H16A H 0.6247 1.1883 0.4240 0.020 Uiso 1 1 calc R . . C17 C 0.6799(3) 1.26271(16) 0.33170(15) 0.0186(5) Uani 1 1 d . . . C18 C 0.7105(3) 1.25406(16) 0.25490(15) 0.0176(5) Uani 1 1 d . . . H18A H 0.7365 1.3082 0.2277 0.021 Uiso 1 1 calc R . . C19 C 0.7047(3) 1.16924(16) 0.21579(14) 0.0150(5) Uani 1 1 d . . . C20 C 0.5987(3) 1.01570(16) 0.38591(14) 0.0165(5) Uani 1 1 d . . . H20A H 0.5308 1.0306 0.4274 0.025 Uiso 1 1 calc R . . H20B H 0.7135 1.0031 0.4086 0.025 Uiso 1 1 calc R . . H20C H 0.5294 0.9612 0.3543 0.025 Uiso 1 1 calc R . . C21 C 0.6883(4) 1.35587(17) 0.37120(17) 0.0275(6) Uani 1 1 d . . . H21A H 0.6885 1.4015 0.3323 0.041 Uiso 1 1 calc R . . H21B H 0.7982 1.3732 0.4079 0.041 Uiso 1 1 calc R . . H21C H 0.5835 1.3535 0.3991 0.041 Uiso 1 1 calc R . . C22 C 0.7503(3) 1.17203(17) 0.13337(14) 0.0202(5) Uani 1 1 d . . . H22A H 0.7879 1.2362 0.1210 0.030 Uiso 1 1 calc R . . H22B H 0.6443 1.1420 0.0976 0.030 Uiso 1 1 calc R . . H22C H 0.8481 1.1397 0.1282 0.030 Uiso 1 1 calc R . . C23 C 1.1240(3) 0.81902(16) 0.37792(13) 0.0148(5) Uani 1 1 d . . . H23A H 1.2519 0.8508 0.3881 0.018 Uiso 1 1 calc R . . H23B H 1.1179 0.7518 0.3740 0.018 Uiso 1 1 calc R . . C24 C 1.0246(3) 0.84379(16) 0.44350(13) 0.0147(5) Uani 1 1 d . . . H24A H 1.0563 0.8122 0.4903 0.018 Uiso 1 1 calc R . . H24B H 1.0540 0.9111 0.4566 0.018 Uiso 1 1 calc R . . C25 C 0.7505(3) 0.70912(15) 0.53603(13) 0.0125(5) Uani 1 1 d . . . C26 C 0.7163(3) 0.62154(16) 0.49527(14) 0.0159(5) Uani 1 1 d . . . C27 C 0.7489(3) 0.54710(16) 0.53592(14) 0.0186(5) Uani 1 1 d . . . H27A H 0.7265 0.4881 0.5090 0.022 Uiso 1 1 calc R . . C28 C 0.8129(3) 0.55553(17) 0.61445(14) 0.0181(5) Uani 1 1 d . . . C29 C 0.8435(3) 0.64170(16) 0.65275(14) 0.0168(5) Uani 1 1 d . . . H29A H 0.8859 0.6481 0.7066 0.020 Uiso 1 1 calc R . . C30 C 0.8148(3) 0.72015(16) 0.61573(13) 0.0133(5) Uani 1 1 d . . . C31 C 0.6476(4) 0.60310(16) 0.41039(14) 0.0229(6) Uani 1 1 d . . . H31A H 0.6231 0.5367 0.3967 0.034 Uiso 1 1 calc R . . H31B H 0.7382 0.6346 0.3797 0.034 Uiso 1 1 calc R . . H31C H 0.5368 0.6260 0.3994 0.034 Uiso 1 1 calc R . . C32 C 0.8508(4) 0.47382(17) 0.65673(16) 0.0251(6) Uani 1 1 d . . . H32A H 0.9754 0.4877 0.6816 0.038 Uiso 1 1 calc R . . H32B H 0.8321 0.4200 0.6198 0.038 Uiso 1 1 calc R . . H32C H 0.7695 0.4607 0.6963 0.038 Uiso 1 1 calc R . . C33 C 0.8560(3) 0.80903(16) 0.66590(14) 0.0189(5) Uani 1 1 d . . . H33A H 0.8932 0.7969 0.7195 0.028 Uiso 1 1 calc R . . H33B H 0.7485 0.8354 0.6639 0.028 Uiso 1 1 calc R . . H33C H 0.9531 0.8525 0.6469 0.028 Uiso 1 1 calc R . . C34 C 0.7358(4) 1.0042(2) -0.04494(16) 0.0384(8) Uani 1 1 d . . . H34A H 0.6199 1.0235 -0.0564 0.046 Uiso 1 1 calc R . . H34B H 0.7392 0.9794 0.0069 0.046 Uiso 1 1 calc R . . Cl1 Cl 0.74831(9) 0.91583(5) -0.11532(4) 0.03306(17) Uani 1 1 d . . . Cl2 Cl 0.91343(10) 1.10121(6) -0.04336(4) 0.03681(18) 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 Co1 0.00751(14) 0.00987(15) 0.01166(16) 0.00167(11) 0.00136(11) 0.00135(11) S1 0.0136(3) 0.0114(3) 0.0143(3) -0.0001(2) 0.0019(2) -0.0007(2) S2 0.0096(3) 0.0104(3) 0.0127(3) 0.0018(2) 0.0013(2) 0.0025(2) S3 0.0123(3) 0.0117(3) 0.0120(3) 0.0016(2) 0.0021(2) 0.0034(2) O1 0.0128(8) 0.0189(9) 0.0216(9) -0.0036(7) 0.0033(7) -0.0023(7) O2 0.0254(9) 0.0125(8) 0.0169(9) 0.0028(7) 0.0027(7) 0.0010(7) O3 0.0094(8) 0.0137(8) 0.0202(9) 0.0034(7) 0.0006(6) 0.0032(6) O4 0.0173(8) 0.0159(8) 0.0119(8) 0.0020(7) 0.0010(7) 0.0045(7) O5 0.0104(8) 0.0206(9) 0.0139(8) 0.0028(7) 0.0028(6) 0.0044(6) O6 0.0235(9) 0.0118(8) 0.0143(8) -0.0004(7) 0.0027(7) 0.0051(7) O7 0.0096(8) 0.0144(9) 0.0140(9) 0.0022(7) 0.0019(7) 0.0016(6) N1 0.0080(9) 0.0101(9) 0.0145(10) 0.0013(7) 0.0016(7) 0.0026(7) N2 0.0082(9) 0.0104(9) 0.0149(10) -0.0006(7) 0.0010(7) -0.0008(7) N3 0.0073(9) 0.0107(9) 0.0141(10) 0.0014(7) 0.0014(7) 0.0020(7) N4 0.0093(9) 0.0140(9) 0.0122(10) 0.0012(8) 0.0016(7) 0.0021(7) C1 0.0101(11) 0.0119(11) 0.0177(12) -0.0004(9) 0.0041(9) 0.0029(8) C2 0.0115(11) 0.0131(11) 0.0182(12) 0.0000(9) 0.0028(9) 0.0032(9) C3 0.0136(11) 0.0135(11) 0.0141(12) -0.0006(9) 0.0004(9) -0.0014(9) C4 0.0133(11) 0.0153(12) 0.0184(12) 0.0010(10) 0.0029(9) -0.0007(9) C5 0.0160(12) 0.0199(12) 0.0207(13) -0.0049(10) 0.0035(10) 0.0003(10) C6 0.0200(13) 0.0213(13) 0.0156(12) -0.0024(10) 0.0025(10) -0.0057(10) C7 0.0269(14) 0.0171(12) 0.0190(13) 0.0037(10) -0.0024(11) -0.0006(10) C8 0.0217(13) 0.0132(11) 0.0168(12) -0.0014(9) -0.0010(10) 0.0014(9) C9 0.0269(14) 0.0201(13) 0.0219(14) 0.0000(10) 0.0036(11) 0.0094(11) C10 0.0338(16) 0.0353(16) 0.0168(13) 0.0014(12) 0.0061(12) 0.0009(12) C11 0.0422(17) 0.0220(14) 0.0213(14) -0.0007(11) -0.0054(12) 0.0166(12) C12 0.0090(10) 0.0095(10) 0.0176(12) 0.0003(9) 0.0037(9) 0.0010(8) C13 0.0080(10) 0.0117(11) 0.0167(12) 0.0013(9) 0.0038(9) 0.0009(8) C14 0.0085(10) 0.0129(11) 0.0148(11) 0.0011(9) -0.0001(9) 0.0043(8) C15 0.0092(11) 0.0154(11) 0.0174(12) 0.0027(9) 0.0022(9) 0.0034(9) C16 0.0115(11) 0.0196(12) 0.0193(13) -0.0013(10) 0.0055(9) 0.0030(9) C17 0.0127(11) 0.0148(12) 0.0289(14) -0.0018(10) 0.0063(10) 0.0029(9) C18 0.0139(12) 0.0137(11) 0.0257(14) 0.0039(10) 0.0050(10) 0.0022(9) C19 0.0128(11) 0.0143(11) 0.0187(12) 0.0029(9) 0.0041(9) 0.0033(9) C20 0.0205(12) 0.0175(12) 0.0134(12) 0.0020(9) 0.0040(10) 0.0069(10) C21 0.0301(15) 0.0146(13) 0.0385(17) -0.0047(11) 0.0142(13) 0.0023(11) C22 0.0255(14) 0.0152(12) 0.0205(13) 0.0052(10) 0.0070(11) 0.0024(10) C23 0.0092(11) 0.0161(12) 0.0182(12) 0.0034(9) -0.0010(9) 0.0019(9) C24 0.0113(11) 0.0182(12) 0.0134(12) 0.0023(9) -0.0003(9) 0.0008(9) C25 0.0118(11) 0.0118(11) 0.0143(11) 0.0033(9) 0.0035(9) 0.0022(8) C26 0.0181(12) 0.0148(12) 0.0146(12) 0.0010(9) 0.0039(9) 0.0023(9) C27 0.0266(14) 0.0106(11) 0.0183(13) 0.0013(9) 0.0031(10) 0.0031(10) C28 0.0195(12) 0.0171(12) 0.0184(13) 0.0053(10) 0.0037(10) 0.0042(10) C29 0.0165(12) 0.0189(12) 0.0140(12) 0.0039(10) 0.0016(9) 0.0011(9) C30 0.0106(11) 0.0152(11) 0.0138(11) 0.0023(9) 0.0021(9) 0.0015(9) C31 0.0401(16) 0.0111(12) 0.0144(13) -0.0009(10) -0.0003(11) 0.0005(11) C32 0.0328(15) 0.0170(13) 0.0253(14) 0.0077(11) -0.0001(12) 0.0058(11) C33 0.0239(13) 0.0172(12) 0.0143(12) 0.0020(10) -0.0032(10) 0.0041(10) C34 0.0226(15) 0.078(2) 0.0192(15) 0.0092(15) 0.0079(12) 0.0168(15) Cl1 0.0226(3) 0.0437(4) 0.0337(4) 0.0160(3) 0.0064(3) 0.0044(3) Cl2 0.0424(4) 0.0524(5) 0.0197(3) 0.0025(3) 0.0051(3) 0.0188(4) _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 N3 1.9266(18) . ? Co1 O7 1.9343(16) . ? Co1 N2 1.9495(19) . ? Co1 N1 1.9540(18) . ? Co1 N4 1.9605(19) . ? S1 O2 1.4385(17) . ? S1 O1 1.4542(17) . ? S1 N2 1.6201(18) . ? S1 C3 1.784(2) . ? S2 O3 1.4372(16) . ? S2 O4 1.4426(16) . ? S2 N3 1.6226(19) . ? S2 C14 1.793(2) . ? S3 O6 1.4376(16) . ? S3 O5 1.4606(16) . ? S3 N4 1.6037(19) . ? S3 C25 1.795(2) . ? O1 H1 1.77(4) . ? O5 H2 1.71(3) . ? O7 H1 0.84(4) . ? O7 H2 0.89(3) . ? N1 C23 1.491(3) . ? N1 C12 1.500(3) . ? N1 C1 1.502(3) . ? N2 C2 1.483(3) . ? N3 C13 1.484(3) . ? N4 C24 1.488(3) . ? C1 C2 1.508(3) . ? C3 C4 1.415(3) . ? C3 C8 1.416(3) . ? C4 C5 1.396(3) . ? C4 C9 1.517(3) . ? C5 C6 1.380(4) . ? C6 C7 1.385(4) . ? C6 C10 1.512(3) . ? C7 C8 1.392(3) . ? C8 C11 1.514(3) . ? C12 C13 1.503(3) . ? C14 C15 1.414(3) . ? C14 C19 1.416(3) . ? C15 C16 1.392(3) . ? C15 C20 1.510(3) . ? C16 C17 1.389(3) . ? C17 C18 1.388(3) . ? C17 C21 1.505(3) . ? C18 C19 1.396(3) . ? C19 C22 1.515(3) . ? C23 C24 1.514(3) . ? C25 C30 1.409(3) . ? C25 C26 1.416(3) . ? C26 C27 1.390(3) . ? C26 C31 1.505(3) . ? C27 C28 1.390(3) . ? C28 C29 1.381(3) . ? C28 C32 1.509(3) . ? C29 C30 1.402(3) . ? C30 C33 1.508(3) . ? C34 Cl2 1.768(3) . ? C34 Cl1 1.781(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 N3 Co1 O7 96.78(7) . . ? N3 Co1 N2 118.78(8) . . ? O7 Co1 N2 94.07(8) . . ? N3 Co1 N1 85.01(8) . . ? O7 Co1 N1 178.20(8) . . ? N2 Co1 N1 85.21(7) . . ? N3 Co1 N4 119.48(8) . . ? O7 Co1 N4 94.35(8) . . ? N2 Co1 N4 119.43(8) . . ? N1 Co1 N4 84.59(8) . . ? O2 S1 O1 115.36(10) . . ? O2 S1 N2 111.20(10) . . ? O1 S1 N2 107.56(10) . . ? O2 S1 C3 108.53(11) . . ? O1 S1 C3 108.31(11) . . ? N2 S1 C3 105.39(10) . . ? O3 S2 O4 115.95(10) . . ? O3 S2 N3 110.08(9) . . ? O4 S2 N3 109.57(10) . . ? O3 S2 C14 107.54(10) . . ? O4 S2 C14 108.18(10) . . ? N3 S2 C14 104.91(10) . . ? O6 S3 O5 115.25(10) . . ? O6 S3 N4 111.20(10) . . ? O5 S3 N4 107.72(10) . . ? O6 S3 C25 108.77(10) . . ? O5 S3 C25 106.75(10) . . ? N4 S3 C25 106.73(10) . . ? S1 O1 H1 110.8(12) . . ? S3 O5 H2 111.8(10) . . ? H1 O7 H2 108(3) . . ? H1 O7 Co1 107(2) . . ? H2 O7 Co1 107(2) . . ? C23 N1 C12 111.07(17) . . ? C23 N1 C1 110.91(17) . . ? C12 N1 C1 110.05(17) . . ? C23 N1 Co1 108.60(13) . . ? C12 N1 Co1 108.32(13) . . ? C1 N1 Co1 107.79(13) . . ? C2 N2 S1 111.49(14) . . ? C2 N2 Co1 113.44(13) . . ? S1 N2 Co1 133.83(11) . . ? C13 N3 S2 109.95(14) . . ? C13 N3 Co1 113.27(13) . . ? S2 N3 Co1 134.17(11) . . ? C24 N4 S3 111.62(15) . . ? C24 N4 Co1 113.54(14) . . ? S3 N4 Co1 133.28(11) . . ? N1 C1 C2 109.07(18) . . ? N2 C2 C1 105.65(17) . . ? C4 C3 C8 120.5(2) . . ? C4 C3 S1 121.67(18) . . ? C8 C3 S1 117.79(18) . . ? C5 C4 C3 117.8(2) . . ? C5 C4 C9 116.5(2) . . ? C3 C4 C9 125.7(2) . . ? C6 C5 C4 123.0(2) . . ? C5 C6 C7 117.9(2) . . ? C5 C6 C10 121.2(2) . . ? C7 C6 C10 120.9(2) . . ? C6 C7 C8 122.8(2) . . ? C7 C8 C3 118.0(2) . . ? C7 C8 C11 117.7(2) . . ? C3 C8 C11 124.3(2) . . ? N1 C12 C13 107.48(17) . . ? N3 C13 C12 105.82(17) . . ? C15 C14 C19 120.8(2) . . ? C15 C14 S2 117.52(17) . . ? C19 C14 S2 121.64(17) . . ? C16 C15 C14 118.4(2) . . ? C16 C15 C20 116.8(2) . . ? C14 C15 C20 124.9(2) . . ? C17 C16 C15 122.3(2) . . ? C18 C17 C16 118.1(2) . . ? C18 C17 C21 120.8(2) . . ? C16 C17 C21 121.1(2) . . ? C17 C18 C19 122.9(2) . . ? C18 C19 C14 117.5(2) . . ? C18 C19 C22 116.3(2) . . ? C14 C19 C22 126.1(2) . . ? N1 C23 C24 109.00(18) . . ? N4 C24 C23 105.06(18) . . ? C30 C25 C26 120.8(2) . . ? C30 C25 S3 121.56(17) . . ? C26 C25 S3 117.67(17) . . ? C27 C26 C25 118.2(2) . . ? C27 C26 C31 117.3(2) . . ? C25 C26 C31 124.6(2) . . ? C26 C27 C28 122.6(2) . . ? C29 C28 C27 117.9(2) . . ? C29 C28 C32 120.7(2) . . ? C27 C28 C32 121.4(2) . . ? C28 C29 C30 122.9(2) . . ? C29 C30 C25 117.7(2) . . ? C29 C30 C33 116.1(2) . . ? C25 C30 C33 126.2(2) . . ? Cl2 C34 Cl1 112.27(15) . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.442 _refine_diff_density_min -0.474 _refine_diff_density_rms 0.078 _iucr_refine_instructions_details ; TITL asb261 in P-1 CELL 0.71073 7.6668 14.8717 17.4049 92.5600 96.5047 101.7540 ZERR 2.00 0.0004 0.0008 0.0009 0.0007 0.0007 0.0007 LATT 1 SFAC C H N O S CL CO UNIT 68 98 8 14 6 4 2 TEMP -185.000 SIZE 0.036 0.097 0.287 rem David Lacy 60s ccd1 rem APEX2 2011.4-1, SAINT 7.68a, SADABS 2008/1, SHELXTL 2008/4 OMIT 0 0 1 OMIT 0 1 0 L.S. 12 ACTA 51 BOND H1 BOND H2 BIND H1 O1 H2 O5 BIND O7 H1 O7 H2 WGHT 0.035900 1.232300 FVAR 0.16966 CO1 7 0.779170 0.814225 0.301041 11.00000 0.00751 0.00987 = 0.01166 0.00167 0.00136 0.00135 S1 5 0.652655 0.614920 0.199922 11.00000 0.01365 0.01142 = 0.01425 -0.00006 0.00189 -0.00073 S2 5 0.627651 0.976026 0.210212 11.00000 0.00957 0.01042 = 0.01265 0.00179 0.00125 0.00249 S3 5 0.707668 0.804628 0.482771 11.00000 0.01227 0.01174 = 0.01200 0.00157 0.00215 0.00341 O1 4 0.474566 0.627171 0.212798 11.00000 0.01276 0.01891 = 0.02160 -0.00362 0.00330 -0.00231 O2 4 0.703397 0.534462 0.230674 11.00000 0.02544 0.01253 = 0.01689 0.00275 0.00273 0.00101 O3 4 0.452181 0.926625 0.222050 11.00000 0.00936 0.01372 = 0.02017 0.00335 0.00063 0.00323 O4 4 0.659844 0.985219 0.130586 11.00000 0.01728 0.01590 = 0.01190 0.00205 0.00104 0.00446 O5 4 0.520330 0.780060 0.447921 11.00000 0.01041 0.02060 = 0.01389 0.00277 0.00281 0.00440 O6 4 0.753857 0.886629 0.534137 11.00000 0.02349 0.01179 = 0.01428 -0.00038 0.00273 0.00514 O7 4 0.521799 0.777841 0.299843 11.00000 0.00957 0.01440 = 0.01402 0.00223 0.00195 0.00165 H1 2 0.488360 0.726357 0.275131 11.00000 0.05647 H2 2 0.501939 0.771119 0.349098 11.00000 0.03847 N1 3 1.040010 0.847607 0.304034 11.00000 0.00796 0.01006 = 0.01452 0.00126 0.00160 0.00256 N2 3 0.794866 0.707813 0.234633 11.00000 0.00818 0.01041 = 0.01486 -0.00057 0.00103 -0.00075 N3 3 0.780741 0.930178 0.255698 11.00000 0.00733 0.01075 = 0.01408 0.00141 0.00136 0.00204 N4 3 0.830846 0.812028 0.413788 11.00000 0.00927 0.01399 = 0.01225 0.00119 0.00160 0.00212 C1 1 1.089986 0.798237 0.235311 11.00000 0.01010 0.01189 = 0.01767 -0.00039 0.00414 0.00294 AFIX 23 H1A 2 1.219811 0.797978 0.243054 11.00000 -1.20000 H1B 2 1.064992 0.830273 0.187936 11.00000 -1.20000 AFIX 0 C2 1 0.981957 0.700704 0.226119 11.00000 0.01153 0.01312 = 0.01820 -0.00004 0.00278 0.00324 AFIX 23 H2A 2 0.988427 0.671692 0.174496 11.00000 -1.20000 H2B 2 1.027539 0.663435 0.266447 11.00000 -1.20000 AFIX 0 C3 1 0.663863 0.609701 0.098059 11.00000 0.01360 0.01347 = 0.01413 -0.00064 0.00043 -0.00135 C4 1 0.738368 0.542136 0.061355 11.00000 0.01327 0.01529 = 0.01840 0.00100 0.00293 -0.00073 C5 1 0.750936 0.546313 -0.017820 11.00000 0.01600 0.01995 = 0.02073 -0.00491 0.00352 0.00026 AFIX 43 H5A 2 0.798456 0.500560 -0.043267 11.00000 -1.20000 AFIX 0 C6 1 0.697437 0.613924 -0.060828 11.00000 0.01999 0.02132 = 0.01558 -0.00239 0.00247 -0.00573 C7 1 0.622906 0.678346 -0.023528 11.00000 0.02694 0.01713 = 0.01898 0.00369 -0.00241 -0.00063 AFIX 43 H7A 2 0.584159 0.724715 -0.052720 11.00000 -1.20000 AFIX 0 C8 1 0.602320 0.678079 0.054904 11.00000 0.02173 0.01325 = 0.01684 -0.00140 -0.00103 0.00142 C9 1 0.805629 0.464357 0.100457 11.00000 0.02687 0.02010 = 0.02194 -0.00002 0.00361 0.00944 AFIX 137 H9A 2 0.850687 0.427382 0.062262 11.00000 -1.50000 H9B 2 0.706924 0.425396 0.122373 11.00000 -1.50000 H9C 2 0.902730 0.490043 0.141998 11.00000 -1.50000 AFIX 0 C10 1 0.719784 0.617954 -0.145890 11.00000 0.03376 0.03531 = 0.01678 0.00135 0.00612 0.00086 AFIX 137 H10A 2 0.714707 0.555784 -0.168485 11.00000 -1.50000 H10B 2 0.836015 0.657405 -0.151594 11.00000 -1.50000 H10C 2 0.623115 0.643286 -0.172725 11.00000 -1.50000 AFIX 0 C11 1 0.515073 0.751071 0.088351 11.00000 0.04215 0.02204 = 0.02132 -0.00073 -0.00540 0.01663 AFIX 137 H11A 2 0.496188 0.794515 0.049093 11.00000 -1.50000 H11B 2 0.593329 0.784142 0.133607 11.00000 -1.50000 H11C 2 0.399227 0.721802 0.104002 11.00000 -1.50000 AFIX 0 C12 1 1.093219 0.949769 0.298899 11.00000 0.00905 0.00948 = 0.01762 0.00032 0.00373 0.00098 AFIX 23 H12A 2 1.216225 0.966538 0.284312 11.00000 -1.20000 H12B 2 1.090952 0.982198 0.349587 11.00000 -1.20000 AFIX 0 C13 1 0.960942 0.976517 0.238258 11.00000 0.00796 0.01168 = 0.01672 0.00127 0.00384 0.00094 AFIX 23 H13A 2 0.972715 1.044158 0.240916 11.00000 -1.20000 H13B 2 0.981172 0.955766 0.185776 11.00000 -1.20000 AFIX 0 C14 1 0.660018 1.089247 0.256747 11.00000 0.00850 0.01290 = 0.01481 0.00111 -0.00007 0.00433 C15 1 0.633283 1.096088 0.335672 11.00000 0.00924 0.01543 = 0.01740 0.00267 0.00219 0.00343 C16 1 0.643429 1.183116 0.371079 11.00000 0.01153 0.01964 = 0.01932 -0.00128 0.00548 0.00296 AFIX 43 H16A 2 0.624745 1.188261 0.423990 11.00000 -1.20000 AFIX 0 C17 1 0.679940 1.262707 0.331696 11.00000 0.01273 0.01482 = 0.02886 -0.00184 0.00628 0.00294 C18 1 0.710520 1.254061 0.254898 11.00000 0.01389 0.01373 = 0.02570 0.00385 0.00503 0.00222 AFIX 43 H18A 2 0.736539 1.308239 0.227731 11.00000 -1.20000 AFIX 0 C19 1 0.704733 1.169240 0.215794 11.00000 0.01280 0.01428 = 0.01868 0.00289 0.00413 0.00332 C20 1 0.598730 1.015702 0.385906 11.00000 0.02047 0.01749 = 0.01343 0.00199 0.00402 0.00691 AFIX 137 H20A 2 0.530815 1.030597 0.427428 11.00000 -1.50000 H20B 2 0.713509 1.003129 0.408615 11.00000 -1.50000 H20C 2 0.529444 0.961215 0.354275 11.00000 -1.50000 AFIX 0 C21 1 0.688281 1.355870 0.371195 11.00000 0.03007 0.01458 = 0.03846 -0.00468 0.01423 0.00234 AFIX 137 H21A 2 0.688528 1.401523 0.332286 11.00000 -1.50000 H21B 2 0.798220 1.373205 0.407933 11.00000 -1.50000 H21C 2 0.583525 1.353545 0.399086 11.00000 -1.50000 AFIX 0 C22 1 0.750291 1.172026 0.133367 11.00000 0.02547 0.01524 = 0.02053 0.00522 0.00697 0.00241 AFIX 137 H22A 2 0.787911 1.236204 0.121032 11.00000 -1.50000 H22B 2 0.644302 1.141974 0.097586 11.00000 -1.50000 H22C 2 0.848130 1.139702 0.128159 11.00000 -1.50000 AFIX 0 C23 1 1.123980 0.819022 0.377924 11.00000 0.00923 0.01611 = 0.01824 0.00338 -0.00105 0.00190 AFIX 23 H23A 2 1.251867 0.850755 0.388100 11.00000 -1.20000 H23B 2 1.117872 0.751809 0.373999 11.00000 -1.20000 AFIX 0 C24 1 1.024609 0.843787 0.443501 11.00000 0.01125 0.01820 = 0.01337 0.00227 -0.00033 0.00083 AFIX 23 H24A 2 1.056302 0.812201 0.490339 11.00000 -1.20000 H24B 2 1.054046 0.911073 0.456588 11.00000 -1.20000 AFIX 0 C25 1 0.750461 0.709123 0.536029 11.00000 0.01180 0.01183 = 0.01426 0.00335 0.00351 0.00217 C26 1 0.716278 0.621543 0.495268 11.00000 0.01811 0.01480 = 0.01461 0.00099 0.00391 0.00234 C27 1 0.748877 0.547100 0.535919 11.00000 0.02655 0.01063 = 0.01827 0.00127 0.00308 0.00311 AFIX 43 H27A 2 0.726497 0.488116 0.508978 11.00000 -1.20000 AFIX 0 C28 1 0.812942 0.555534 0.614452 11.00000 0.01946 0.01715 = 0.01844 0.00529 0.00370 0.00421 C29 1 0.843498 0.641696 0.652751 11.00000 0.01651 0.01891 = 0.01405 0.00389 0.00163 0.00114 AFIX 43 H29A 2 0.885851 0.648076 0.706571 11.00000 -1.20000 AFIX 0 C30 1 0.814786 0.720152 0.615725 11.00000 0.01062 0.01517 = 0.01377 0.00227 0.00210 0.00148 C31 1 0.647613 0.603099 0.410389 11.00000 0.04006 0.01106 = 0.01441 -0.00086 -0.00033 0.00052 AFIX 137 H31A 2 0.623063 0.536697 0.396710 11.00000 -1.50000 H31B 2 0.738232 0.634618 0.379748 11.00000 -1.50000 H31C 2 0.536820 0.625967 0.399420 11.00000 -1.50000 AFIX 0 C32 1 0.850809 0.473820 0.656734 11.00000 0.03281 0.01697 = 0.02535 0.00773 -0.00014 0.00583 AFIX 137 H32A 2 0.975402 0.487651 0.681599 11.00000 -1.50000 H32B 2 0.832124 0.420049 0.619769 11.00000 -1.50000 H32C 2 0.769489 0.460702 0.696288 11.00000 -1.50000 AFIX 0 C33 1 0.856008 0.809034 0.665903 11.00000 0.02385 0.01723 = 0.01432 0.00198 -0.00317 0.00415 AFIX 137 H33A 2 0.893227 0.796943 0.719527 11.00000 -1.50000 H33B 2 0.748488 0.835374 0.663859 11.00000 -1.50000 H33C 2 0.953098 0.852548 0.646932 11.00000 -1.50000 AFIX 0 C34 1 0.735765 1.004194 -0.044938 11.00000 0.02256 0.07795 = 0.01916 0.00923 0.00791 0.01682 AFIX 23 H34A 2 0.619893 1.023482 -0.056412 11.00000 -1.20000 H34B 2 0.739153 0.979407 0.006938 11.00000 -1.20000 AFIX 0 CL1 6 0.748308 0.915834 -0.115315 11.00000 0.02257 0.04368 = 0.03372 0.01605 0.00641 0.00436 CL2 6 0.913429 1.101209 -0.043356 11.00000 0.04236 0.05240 = 0.01974 0.00247 0.00509 0.01878 HKLF 4 REM asb261 in P-1 REM R1 = 0.0382 for 6795 Fo > 4sig(Fo) and 0.0639 for all 9099 data REM 477 parameters refined using 0 restraints END WGHT 0.0359 1.2321 REM Highest difference peak 0.442, deepest hole -0.474, 1-sigma level 0.078 Q1 1 1.0186 0.9617 0.2680 11.00000 0.05 0.44 Q2 1 0.7519 0.7474 0.5105 11.00000 0.05 0.40 Q3 1 0.8233 0.9196 -0.0678 11.00000 0.05 0.40 Q4 1 0.6262 0.6410 0.0777 11.00000 0.05 0.39 Q5 1 0.8497 0.8053 0.2696 11.00000 0.05 0.39 Q6 1 0.5219 0.9514 0.2204 11.00000 0.05 0.39 Q7 1 0.7096 0.9462 0.2339 11.00000 0.05 0.37 Q8 1 1.0858 0.8403 0.4107 11.00000 0.05 0.36 Q9 1 0.6076 1.0546 0.3625 11.00000 0.05 0.35 Q10 1 0.6365 1.1247 0.2360 11.00000 0.05 0.35 Q11 1 1.0395 0.7532 0.2290 11.00000 0.05 0.35 Q12 1 0.7093 0.5795 -0.0381 11.00000 0.05 0.34 Q13 1 0.7826 0.8094 0.3794 11.00000 0.05 0.34 Q14 1 0.7264 0.6706 -0.1607 11.00000 0.05 0.33 Q15 1 0.8726 0.6865 0.6290 11.00000 0.05 0.33 Q16 1 0.7649 0.5128 0.0803 11.00000 0.05 0.32 Q17 1 1.0390 0.8186 0.2011 11.00000 0.05 0.32 Q18 1 0.8687 0.9692 0.2484 11.00000 0.05 0.32 Q19 1 0.8167 0.7600 0.1993 11.00000 0.05 0.32 Q20 1 0.6001 1.0586 0.2373 11.00000 0.05 0.31 ;