# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Li, Dong-Sheng' _publ_contact_author_email lidongsheng1@126.com _publ_author_name 'Dong-Sheng Li' data_d _database_code_depnum_ccdc_archive 'CCDC 778541' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H34 N4 Ni2 O13 S4, H2 O, 0.2(O)' _chemical_formula_sum 'C48 H36 N4 Ni2 O14.20 S4' _chemical_formula_weight 1141.67 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' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 11.4666(10) _cell_length_b 39.891(3) _cell_length_c 43.067(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19699(3) _cell_formula_units_Z 16 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9533 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.64 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9368 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32432 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.2211 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4575 _reflns_number_gt 2080 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4575 _refine_ls_number_parameters 351 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1151 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_ref 0.1884 _refine_ls_wR_factor_gt 0.1730 _refine_ls_goodness_of_fit_ref 0.811 _refine_ls_restrained_S_all 0.810 _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 N1 N -0.3944(6) 0.3290(2) 0.4712(2) 0.045(4) Uani 0.62 1 d PGU . 1 C1 C -0.3727(7) 0.3326(2) 0.43964(19) 0.045(3) Uani 0.62 1 d PG . 1 H1 H -0.4317 0.3400 0.4265 0.054 Uiso 0.62 1 calc PR . 1 C2 C -0.2630(8) 0.3252(3) 0.42774(16) 0.067(5) Uani 0.62 1 d PG . 1 H2 H -0.2486 0.3277 0.4066 0.081 Uiso 0.62 1 calc PR . 1 C3 C -0.1749(6) 0.3142(3) 0.4474(2) 0.043(3) Uani 0.62 1 d PGD . 1 C4 C -0.1966(7) 0.3106(3) 0.4790(2) 0.099(6) Uani 0.62 1 d PG . 1 H4 H -0.1376 0.3032 0.4922 0.118 Uiso 0.62 1 calc PR . 1 C5 C -0.3063(9) 0.3180(3) 0.49090(16) 0.071(5) Uani 0.62 1 d PG . 1 H5 H -0.3207 0.3156 0.5120 0.085 Uiso 0.62 1 calc PR . 1 S1 S -0.0349(10) 0.3069(4) 0.4310(4) 0.064(4) Uani 0.62 1 d PD . 1 N2 N 0.0555(7) 0.20896(17) 0.4806(2) 0.027(2) Uani 0.62 1 d PGU . 1 C6 C 0.1173(7) 0.2380(2) 0.48733(18) 0.045(3) Uani 0.62 1 d PGU . 1 H6 H 0.1759 0.2377 0.5023 0.054 Uiso 0.62 1 calc PR . 1 C7 C 0.0917(7) 0.26763(18) 0.4717(2) 0.049(3) Uani 0.62 1 d PGU . 1 H7 H 0.1331 0.2871 0.4762 0.059 Uiso 0.62 1 calc PR . 1 C8 C 0.0042(8) 0.2681(2) 0.4494(2) 0.038(3) Uani 0.62 1 d PGD . 1 C9 C -0.0576(7) 0.2391(3) 0.4427(2) 0.056(5) Uani 0.62 1 d PG . 1 H9 H -0.1162 0.2394 0.4277 0.068 Uiso 0.62 1 calc PR . 1 C10 C -0.0320(7) 0.2095(2) 0.4583(3) 0.044(4) Uani 0.62 1 d PG . 1 H10 H -0.0734 0.1900 0.4538 0.053 Uiso 0.62 1 calc PR . 1 Ni1 Ni 0.07500(9) 0.16658(2) 0.51064(2) 0.0357(3) Uani 1 1 d . . . N1' N -0.4238(9) 0.3266(3) 0.4675(3) 0.024(5) Uani 0.38 1 d PGU . 2 C1' C -0.3494(11) 0.3527(2) 0.4594(3) 0.045(3) Uani 0.38 1 d PG . 2 H1' H -0.3734 0.3748 0.4618 0.054 Uiso 0.38 1 calc PR . 2 C2' C -0.2392(10) 0.3457(3) 0.4476(3) 0.038(5) Uani 0.38 1 d PG . 2 H2' H -0.1894 0.3632 0.4422 0.045 Uiso 0.38 1 calc PR . 2 C3' C -0.2033(9) 0.3127(3) 0.4440(3) 0.043(3) Uani 0.38 1 d PGD . 2 C4' C -0.2777(10) 0.2866(2) 0.4521(3) 0.024(4) Uani 0.38 1 d PG . 2 H4' H -0.2537 0.2645 0.4496 0.029 Uiso 0.38 1 calc PR . 2 C5' C -0.3880(10) 0.2936(3) 0.4638(3) 0.045(3) Uani 0.38 1 d PG . 2 H5' H -0.4377 0.2761 0.4693 0.054 Uiso 0.38 1 calc PR . 2 S1' S -0.0663(17) 0.3027(6) 0.4266(7) 0.067(7) Uani 0.38 1 d PD . 2 N2' N 0.0276(12) 0.2106(3) 0.4847(4) 0.027(2) Uani 0.38 1 d PG . 2 C6' C 0.0067(13) 0.2412(3) 0.4991(3) 0.045(3) Uani 0.38 1 d PG . 2 H6' H 0.0131 0.2431 0.5205 0.054 Uiso 0.38 1 calc PR . 2 C7' C -0.0237(13) 0.2690(3) 0.4814(3) 0.049(3) Uani 0.38 1 d PG . 2 H7' H -0.0377 0.2895 0.4910 0.059 Uiso 0.38 1 calc PR . 2 C8' C -0.0332(16) 0.2662(4) 0.4493(3) 0.038(3) Uani 0.38 1 d PGD . 2 C9' C -0.0123(16) 0.2356(6) 0.4349(3) 0.062(10) Uani 0.38 1 d PG . 2 H9' H -0.0186 0.2337 0.4135 0.074 Uiso 0.38 1 calc PR . 2 C10' C 0.0181(14) 0.2078(4) 0.4526(4) 0.044(4) Uani 0.38 1 d PG . 2 H10' H 0.0321 0.1873 0.4430 0.053 Uiso 0.38 1 calc PR . 2 S2 S 0.40098(17) 0.30919(5) 0.63744(5) 0.0401(5) Uani 1 1 d . . . O1 O 0.1369(5) 0.19784(12) 0.54567(12) 0.0480(14) Uani 1 1 d . . . O2 O 0.2326(6) 0.16268(13) 0.57636(12) 0.0636(18) Uani 1 1 d . . . O3 O 0.4218(4) 0.33325(13) 0.61326(12) 0.0548(15) Uani 1 1 d . . . O4 O 0.4956(4) 0.29646(13) 0.65582(12) 0.0555(16) Uani 1 1 d . . . O5 O 0.0026(4) 0.38907(12) 0.72611(10) 0.0356(12) Uani 1 1 d . . . O6 O -0.0115(4) 0.33555(12) 0.74249(11) 0.0416(13) Uani 1 1 d . . . O7 O 0.1250 0.1250 0.53720(14) 0.0401(19) Uani 1 2 d S . . H7A H 0.1729 0.1339 0.5488 0.048 Uiso 1 1 d R . . C11 C 0.1972(7) 0.19113(19) 0.56887(17) 0.0390(19) Uani 1 1 d . . . C12 C 0.2359(6) 0.22062(17) 0.58847(15) 0.0332(18) Uani 1 1 d . . . C13 C 0.2083(7) 0.25240(19) 0.58030(17) 0.042(2) Uani 1 1 d . . . H13 H 0.1559 0.2560 0.5642 0.051 Uiso 1 1 calc R . . C14 C 0.2567(7) 0.27992(19) 0.59552(17) 0.042(2) Uani 1 1 d . . . H14 H 0.2392 0.3016 0.5892 0.051 Uiso 1 1 calc R . . C15 C 0.3309(6) 0.27433(18) 0.62004(16) 0.0319(17) Uani 1 1 d . . . C16 C 0.3572(7) 0.24258(18) 0.62967(16) 0.041(2) Uani 1 1 d . . . H16 H 0.4076 0.2392 0.6463 0.050 Uiso 1 1 calc R . . C17 C 0.3079(7) 0.21552(18) 0.61434(16) 0.041(2) Uani 1 1 d . . . H17 H 0.3227 0.1938 0.6213 0.049 Uiso 1 1 calc R . . C18 C 0.0310(6) 0.3588(2) 0.72590(16) 0.0333(18) Uani 1 1 d . . . C19 C 0.1262(6) 0.34829(17) 0.70361(15) 0.0307(17) Uani 1 1 d . . . C20 C 0.1889(8) 0.3200(2) 0.71062(18) 0.055(2) Uani 1 1 d . . . H20 H 0.1724 0.3081 0.7286 0.065 Uiso 1 1 calc R . . C21 C 0.2765(8) 0.3093(2) 0.69101(18) 0.055(2) Uani 1 1 d . . . H21 H 0.3228 0.2912 0.6966 0.065 Uiso 1 1 calc R . . C22 C 0.2956(6) 0.32553(18) 0.66321(16) 0.0337(18) Uani 1 1 d . . . C23 C 0.2300(6) 0.35343(18) 0.65568(17) 0.0364(19) Uani 1 1 d . . . H23 H 0.2413 0.3642 0.6368 0.044 Uiso 1 1 calc R . . C24 C 0.1475(6) 0.36525(18) 0.67640(17) 0.0360(19) Uani 1 1 d . . . H24 H 0.1063 0.3847 0.6719 0.043 Uiso 1 1 calc R . . O1W O 0.3551(8) 0.1250 0.6250 0.092(3) Uani 1 2 d S . . H1A H 0.3214 0.1360 0.6116 0.110 Uiso 1 1 d R . . O2W O 0.6250 0.1250 0.6250 0.075(10) Uani 0.40 4 d SP . . 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 N1 0.039(6) 0.048(8) 0.049(8) -0.001(6) 0.001(6) 0.016(6) C1 0.032(6) 0.049(7) 0.055(7) 0.008(5) 0.004(5) 0.011(5) C2 0.033(9) 0.102(14) 0.066(11) 0.020(10) 0.018(8) -0.004(9) C3 0.043(7) 0.041(6) 0.043(5) 0.010(4) 0.007(6) 0.006(5) C4 0.058(12) 0.138(18) 0.100(14) 0.053(13) 0.010(10) 0.023(11) C5 0.040(9) 0.101(13) 0.072(11) 0.016(10) 0.007(8) 0.006(9) S1 0.048(5) 0.045(4) 0.100(8) 0.028(4) 0.025(5) 0.010(4) N2 0.019(4) 0.027(3) 0.037(4) -0.006(3) 0.006(3) 0.007(3) C6 0.050(5) 0.044(5) 0.042(4) -0.002(4) -0.014(4) -0.002(4) C7 0.056(5) 0.042(5) 0.051(5) -0.005(4) -0.004(4) -0.005(4) C8 0.016(9) 0.032(5) 0.065(6) 0.006(4) 0.025(5) -0.003(6) C9 0.048(12) 0.033(10) 0.089(13) 0.017(9) -0.011(10) 0.006(8) C10 0.023(10) 0.035(6) 0.075(8) 0.000(6) -0.008(8) 0.006(7) Ni1 0.0496(7) 0.0246(5) 0.0328(5) -0.0030(4) -0.0015(5) -0.0017(5) N1' 0.027(8) 0.024(9) 0.021(8) -0.001(6) -0.006(6) -0.013(7) C1' 0.032(6) 0.049(7) 0.055(7) 0.008(5) 0.004(5) 0.011(5) C2' 0.039(13) 0.017(11) 0.057(14) 0.015(10) -0.004(11) -0.006(9) C3' 0.043(7) 0.041(6) 0.043(5) 0.010(4) 0.007(6) 0.006(5) C4' 0.029(11) 0.014(9) 0.028(10) 0.000(8) 0.003(8) 0.007(8) C5' 0.032(6) 0.049(7) 0.055(7) 0.008(5) 0.004(5) 0.011(5) S1' 0.064(12) 0.060(10) 0.077(8) 0.028(8) 0.024(10) 0.028(10) N2' 0.019(4) 0.027(3) 0.037(4) -0.006(3) 0.006(3) 0.007(3) C6' 0.050(5) 0.044(5) 0.042(4) -0.002(4) -0.014(4) -0.002(4) C7' 0.056(5) 0.042(5) 0.051(5) -0.005(4) -0.004(4) -0.005(4) C8' 0.016(9) 0.032(5) 0.065(6) 0.006(4) 0.025(5) -0.003(6) C9' 0.07(2) 0.07(2) 0.046(16) 0.002(15) 0.018(15) 0.025(17) C10' 0.023(10) 0.035(6) 0.075(8) 0.000(6) -0.008(8) 0.006(7) S2 0.0324(12) 0.0365(12) 0.0515(13) -0.0129(10) 0.0026(10) -0.0037(10) O1 0.070(4) 0.031(3) 0.043(3) -0.005(3) -0.020(3) -0.001(3) O2 0.108(5) 0.028(3) 0.055(4) -0.004(3) -0.033(3) -0.002(3) O3 0.057(4) 0.039(3) 0.068(4) -0.009(3) 0.021(3) -0.020(3) O4 0.031(3) 0.060(4) 0.075(4) -0.021(3) -0.014(3) 0.010(3) O5 0.043(3) 0.026(3) 0.038(3) -0.005(2) 0.004(2) 0.001(3) O6 0.049(3) 0.030(3) 0.046(3) 0.004(3) 0.002(3) 0.001(3) O7 0.051(5) 0.029(4) 0.040(4) 0.000 0.000 -0.016(4) C11 0.054(5) 0.030(5) 0.033(4) -0.002(4) -0.002(4) -0.004(4) C12 0.045(5) 0.028(4) 0.027(4) -0.007(3) -0.002(4) -0.004(4) C13 0.049(5) 0.036(5) 0.041(5) -0.011(4) -0.016(4) 0.011(4) C14 0.049(5) 0.031(5) 0.047(5) -0.008(4) -0.012(4) 0.013(4) C15 0.028(4) 0.030(4) 0.038(4) -0.008(3) 0.002(4) 0.002(4) C16 0.058(6) 0.031(5) 0.035(4) -0.004(4) -0.008(4) 0.000(4) C17 0.056(6) 0.024(4) 0.043(5) 0.006(4) -0.007(4) 0.000(4) C18 0.031(5) 0.034(5) 0.035(4) -0.006(4) -0.006(4) 0.005(4) C19 0.034(4) 0.027(4) 0.031(4) -0.006(3) -0.004(3) 0.004(4) C20 0.073(6) 0.051(6) 0.039(5) 0.016(4) 0.006(5) 0.034(5) C21 0.075(7) 0.045(5) 0.044(5) 0.003(4) 0.009(5) 0.028(5) C22 0.038(5) 0.028(4) 0.035(4) -0.007(4) -0.002(4) -0.002(4) C23 0.036(5) 0.033(5) 0.041(5) 0.003(4) 0.002(4) -0.008(4) C24 0.036(5) 0.028(4) 0.044(5) 0.004(4) 0.000(4) 0.008(4) O1W 0.111(8) 0.083(7) 0.081(7) 0.033(6) 0.000 0.000 O2W 0.10(3) 0.028(17) 0.09(2) 0.000 0.000 0.000 _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 N1 C1 1.3900 . ? N1 C5 1.3900 . ? N1 Ni1 2.221(6) 29_456 ? C1 C2 1.3900 . ? C1 H1 0.9300 . ? C2 C3 1.3900 . ? C2 H2 0.9300 . ? C3 C4 1.3900 . ? C3 S1 1.779(9) . ? C4 C5 1.3900 . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? S1 C8 1.792(9) . ? N2 C6 1.3900 . ? N2 C10 1.3900 . ? N2 Ni1 2.140(8) . ? C6 C7 1.3900 . ? C6 H6 0.9300 . ? C7 C8 1.3900 . ? C7 H7 0.9300 . ? C8 C9 1.3900 . ? C9 C10 1.3900 . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? Ni1 N1' 1.991(9) 29_456 ? Ni1 O6 2.034(5) 32 ? Ni1 O5 2.051(5) 19 ? Ni1 O1 2.082(5) . ? Ni1 O7 2.095(4) . ? Ni1 N2' 2.152(13) . ? Ni1 N1 2.221(6) 29_456 ? N1' C1' 1.3900 . ? N1' C5' 1.3900 . ? N1' Ni1 1.991(9) 29_456 ? C1' C2' 1.3900 . ? C1' H1' 0.9300 . ? C2' C3' 1.3900 . ? C2' H2' 0.9300 . ? C3' C4' 1.3900 . ? C3' S1' 1.785(13) . ? C4' C5' 1.3900 . ? C4' H4' 0.9300 . ? C5' H5' 0.9300 . ? S1' C8' 1.793(13) . ? N2' C6' 1.3900 . ? N2' C10' 1.3900 . ? C6' C7' 1.3900 . ? C6' H6' 0.9300 . ? C7' C8' 1.3900 . ? C7' H7' 0.9300 . ? C8' C9' 1.3900 . ? C9' C10' 1.3900 . ? C9' H9' 0.9300 . ? C10' H10' 0.9300 . ? S2 O4 1.436(5) . ? S2 O3 1.436(5) . ? S2 C22 1.765(7) . ? S2 C15 1.772(7) . ? O1 C11 1.245(8) . ? O2 C11 1.247(8) . ? O5 C18 1.252(8) . ? O5 Ni1 2.051(5) 23 ? O6 C18 1.267(8) . ? O6 Ni1 2.034(5) 24 ? O7 Ni1 2.095(4) 2 ? O7 H7A 0.8215 . ? C11 C12 1.514(9) . ? C12 C13 1.353(9) . ? C12 C17 1.402(9) . ? C13 C14 1.394(10) . ? C13 H13 0.9300 . ? C14 C15 1.374(9) . ? C14 H14 0.9300 . ? C15 C16 1.366(9) . ? C16 C17 1.386(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.512(9) . ? C19 C20 1.370(9) . ? C19 C24 1.375(9) . ? C20 C21 1.380(10) . ? C20 H20 0.9300 . ? C21 C22 1.378(10) . ? C21 H21 0.9300 . ? C22 C23 1.382(9) . ? C23 C24 1.383(9) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? O1W H1A 0.8209 . ? 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 C1 N1 C5 120.0 . . ? C1 N1 Ni1 120.2(5) . 29_456 ? C5 N1 Ni1 119.2(5) . 29_456 ? C2 C1 N1 120.0 . . ? C2 C1 H1 120.0 . . ? N1 C1 H1 120.0 . . ? C3 C2 C1 120.0 . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 S1 117.8(8) . . ? C4 C3 S1 122.2(8) . . ? C3 C4 C5 120.0 . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 N1 120.0 . . ? C4 C5 H5 120.0 . . ? N1 C5 H5 120.0 . . ? C3 S1 C8 101.1(7) . . ? C6 N2 C10 120.0 . . ? C6 N2 Ni1 118.7(5) . . ? C10 N2 Ni1 120.4(5) . . ? C7 C6 N2 120.0 . . ? C7 C6 H6 120.0 . . ? N2 C6 H6 120.0 . . ? C8 C7 C6 120.0 . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 120.0 . . ? C7 C8 S1 119.9(9) . . ? C9 C8 S1 120.0(9) . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 N2 120.0 . . ? C9 C10 H10 120.0 . . ? N2 C10 H10 120.0 . . ? N1' Ni1 O6 172.0(4) 29_456 32 ? N1' Ni1 O5 92.2(4) 29_456 19 ? O6 Ni1 O5 95.68(19) 32 19 ? N1' Ni1 O1 82.7(4) 29_456 . ? O6 Ni1 O1 89.4(2) 32 . ? O5 Ni1 O1 173.5(2) 19 . ? N1' Ni1 O7 95.0(4) 29_456 . ? O6 Ni1 O7 85.66(16) 32 . ? O5 Ni1 O7 95.21(18) 19 . ? O1 Ni1 O7 89.16(19) . . ? N1' Ni1 N2 95.0(4) 29_456 . ? O6 Ni1 N2 84.1(2) 32 . ? O5 Ni1 N2 86.5(3) 19 . ? O1 Ni1 N2 90.0(3) . . ? O7 Ni1 N2 169.7(2) . . ? N1' Ni1 N2' 85.1(5) 29_456 . ? O6 Ni1 N2' 93.9(4) 32 . ? O5 Ni1 N2' 87.2(4) 19 . ? O1 Ni1 N2' 88.5(5) . . ? O7 Ni1 N2' 177.6(4) . . ? N2 Ni1 N2' 9.9(5) . . ? N1' Ni1 N1 8.5(5) 29_456 29_456 ? O6 Ni1 N1 177.1(3) 32 29_456 ? O5 Ni1 N1 83.8(3) 19 29_456 ? O1 Ni1 N1 90.9(3) . 29_456 ? O7 Ni1 N1 97.2(3) . 29_456 ? N2 Ni1 N1 93.0(3) . 29_456 ? N2' Ni1 N1 83.3(5) . 29_456 ? C1' N1' C5' 120.0 . . ? C1' N1' Ni1 123.5(7) . 29_456 ? C5' N1' Ni1 116.1(7) . 29_456 ? N1' C1' C2' 120.0 . . ? N1' C1' H1' 120.0 . . ? C2' C1' H1' 120.0 . . ? C1' C2' C3' 120.0 . . ? C1' C2' H2' 120.0 . . ? C3' C2' H2' 120.0 . . ? C4' C3' C2' 120.0 . . ? C4' C3' S1' 118.6(11) . . ? C2' C3' S1' 121.3(10) . . ? C3' C4' C5' 120.0 . . ? C3' C4' H4' 120.0 . . ? C5' C4' H4' 120.0 . . ? C4' C5' N1' 120.0 . . ? C4' C5' H5' 120.0 . . ? N1' C5' H5' 120.0 . . ? C3' S1' C8' 98.0(11) . . ? C6' N2' C10' 120.0 . . ? C6' N2' Ni1 122.0(9) . . ? C10' N2' Ni1 118.0(9) . . ? N2' C6' C7' 120.0 . . ? N2' C6' H6' 120.0 . . ? C7' C6' H6' 120.0 . . ? C8' C7' C6' 120.0 . . ? C8' C7' H7' 120.0 . . ? C6' C7' H7' 120.0 . . ? C7' C8' C9' 120.0 . . ? C7' C8' S1' 119.5(15) . . ? C9' C8' S1' 120.4(15) . . ? C10' C9' C8' 120.0 . . ? C10' C9' H9' 120.0 . . ? C8' C9' H9' 120.0 . . ? C9' C10' N2' 120.0 . . ? C9' C10' H10' 120.0 . . ? N2' C10' H10' 120.0 . . ? O4 S2 O3 120.7(3) . . ? O4 S2 C22 107.5(3) . . ? O3 S2 C22 108.9(3) . . ? O4 S2 C15 107.3(3) . . ? O3 S2 C15 107.1(3) . . ? C22 S2 C15 104.2(3) . . ? C11 O1 Ni1 130.0(5) . . ? C18 O5 Ni1 129.4(5) . 23 ? C18 O6 Ni1 127.0(5) . 24 ? Ni1 O7 Ni1 113.8(3) 2 . ? Ni1 O7 H7A 119.2 2 . ? Ni1 O7 H7A 100.0 . . ? O1 C11 O2 125.7(7) . . ? O1 C11 C12 116.3(7) . . ? O2 C11 C12 117.9(7) . . ? C13 C12 C17 118.7(7) . . ? C13 C12 C11 121.0(7) . . ? C17 C12 C11 120.2(7) . . ? C12 C13 C14 121.5(7) . . ? C12 C13 H13 119.2 . . ? C14 C13 H13 119.2 . . ? C15 C14 C13 118.7(7) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 C14 121.4(7) . . ? C16 C15 S2 119.9(6) . . ? C14 C15 S2 118.6(6) . . ? C15 C16 C17 119.1(7) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C16 C17 C12 120.4(7) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? O5 C18 O6 127.0(7) . . ? O5 C18 C19 117.3(7) . . ? O6 C18 C19 115.7(6) . . ? C20 C19 C24 120.0(7) . . ? C20 C19 C18 117.8(7) . . ? C24 C19 C18 122.2(6) . . ? C19 C20 C21 120.1(7) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 120.2(7) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 119.6(7) . . ? C21 C22 S2 118.8(6) . . ? C23 C22 S2 121.5(6) . . ? C22 C23 C24 119.7(7) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C19 C24 C23 120.2(7) . . ? C19 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 N1 C1 C2 0.0 . . . . ? Ni1 N1 C1 C2 -170.9(6) 29_456 . . . ? N1 C1 C2 C3 0.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C1 C2 C3 S1 -177.4(10) . . . . ? C2 C3 C4 C5 0.0 . . . . ? S1 C3 C4 C5 177.3(10) . . . . ? C3 C4 C5 N1 0.0 . . . . ? C1 N1 C5 C4 0.0 . . . . ? Ni1 N1 C5 C4 171.0(6) 29_456 . . . ? C2 C3 S1 C8 -136.9(9) . . . . ? C4 C3 S1 C8 45.7(14) . . . . ? C10 N2 C6 C7 0.0 . . . . ? Ni1 N2 C6 C7 -168.8(5) . . . . ? N2 C6 C7 C8 0.0 . . . . ? C6 C7 C8 C9 0.0 . . . . ? C6 C7 C8 S1 176.1(8) . . . . ? C3 S1 C8 C7 -109.4(9) . . . . ? C3 S1 C8 C9 66.7(13) . . . . ? C7 C8 C9 C10 0.0 . . . . ? S1 C8 C9 C10 -176.1(8) . . . . ? C8 C9 C10 N2 0.0 . . . . ? C6 N2 C10 C9 0.0 . . . . ? Ni1 N2 C10 C9 168.6(6) . . . . ? C6 N2 Ni1 N1' 102.6(6) . . . 29_456 ? C10 N2 Ni1 N1' -66.2(6) . . . 29_456 ? C6 N2 Ni1 O6 -69.5(4) . . . 32 ? C10 N2 Ni1 O6 121.8(4) . . . 32 ? C6 N2 Ni1 O5 -165.6(4) . . . 19 ? C10 N2 Ni1 O5 25.7(4) . . . 19 ? C6 N2 Ni1 O1 19.9(4) . . . . ? C10 N2 Ni1 O1 -148.8(4) . . . . ? C6 N2 Ni1 O7 -65.5(17) . . . . ? C10 N2 Ni1 O7 125.7(15) . . . . ? C6 N2 Ni1 N2' 101(4) . . . . ? C6 N2 Ni1 N1 110.8(5) . . . 29_456 ? C10 N2 Ni1 N1 -57.9(5) . . . 29_456 ? C5' N1' C1' C2' 0.0 . . . . ? Ni1 N1' C1' C2' 172.1(10) 29_456 . . . ? N1' C1' C2' C3' 0.0 . . . . ? C1' C2' C3' C4' 0.0 . . . . ? C1' C2' C3' S1' 175.9(16) . . . . ? C2' C3' C4' C5' 0.0 . . . . ? S1' C3' C4' C5' -176.0(15) . . . . ? C3' C4' C5' N1' 0.0 . . . . ? C1' N1' C5' C4' 0.0 . . . . ? Ni1 N1' C5' C4' -172.7(9) 29_456 . . . ? C2' C3' S1' C8' 145.6(11) . . . . ? N1' Ni1 N2' C6' 59.0(9) 29_456 . . . ? O6 Ni1 N2' C6' -113.1(8) 32 . . . ? O5 Ni1 N2' C6' 151.4(8) 19 . . . ? O1 Ni1 N2' C6' -23.8(8) . . . . ? N1 Ni1 N2' C6' 67.3(8) 29_456 . . . ? N1' Ni1 N2' C10' -121.0(9) 29_456 . . . ? O6 Ni1 N2' C10' 67.0(8) 32 . . . ? O5 Ni1 N2' C10' -28.5(8) 19 . . . ? O1 Ni1 N2' C10' 156.3(8) . . . . ? N1 Ni1 N2' C10' -112.7(8) 29_456 . . . ? C10' N2' C6' C7' 0.0 . . . . ? Ni1 N2' C6' C7' -180.0(10) . . . . ? N2' C6' C7' C8' 0.0 . . . . ? C6' C7' C8' C9' 0.0 . . . . ? C6' C7' C8' S1' -177.3(15) . . . . ? C3' S1' C8' C9' 122.9(14) . . . . ? C7' C8' C9' C10' 0.0 . . . . ? S1' C8' C9' C10' 177.3(15) . . . . ? C8' C9' C10' N2' 0.0 . . . . ? C6' N2' C10' C9' 0.0 . . . . ? N1' Ni1 O1 C11 106.5(8) 29_456 . . . ? O6 Ni1 O1 C11 -74.4(7) 32 . . . ? O7 Ni1 O1 C11 11.3(7) . . . . ? N2 Ni1 O1 C11 -158.4(7) . . . . ? N2' Ni1 O1 C11 -168.2(8) . . . . ? N1 Ni1 O1 C11 108.5(7) 29_456 . . . ? N1' Ni1 O7 Ni1 128.6(4) 29_456 . . 2 ? O6 Ni1 O7 Ni1 -59.36(14) 32 . . 2 ? O5 Ni1 O7 Ni1 35.96(13) 19 . . 2 ? O1 Ni1 O7 Ni1 -148.82(16) . . . 2 ? N2 Ni1 O7 Ni1 -63.3(16) . . . 2 ? N1 Ni1 O7 Ni1 120.4(3) 29_456 . . 2 ? Ni1 O1 C11 O2 -1.5(12) . . . . ? Ni1 O1 C11 C12 174.9(5) . . . . ? O1 C11 C12 C13 -1.9(11) . . . . ? O2 C11 C12 C13 174.8(7) . . . . ? O1 C11 C12 C17 -177.5(7) . . . . ? O2 C11 C12 C17 -0.8(11) . . . . ? C17 C12 C13 C14 4.9(12) . . . . ? C11 C12 C13 C14 -170.8(7) . . . . ? C12 C13 C14 C15 -2.3(12) . . . . ? C13 C14 C15 C16 -0.2(11) . . . . ? C13 C14 C15 S2 175.3(6) . . . . ? O4 S2 C15 C16 11.5(7) . . . . ? O3 S2 C15 C16 142.4(6) . . . . ? C22 S2 C15 C16 -102.4(6) . . . . ? O4 S2 C15 C14 -164.1(6) . . . . ? O3 S2 C15 C14 -33.2(7) . . . . ? C22 S2 C15 C14 82.1(6) . . . . ? C14 C15 C16 C17 0.0(11) . . . . ? S2 C15 C16 C17 -175.4(6) . . . . ? C15 C16 C17 C12 2.7(11) . . . . ? C13 C12 C17 C16 -5.1(11) . . . . ? C11 C12 C17 C16 170.6(7) . . . . ? Ni1 O5 C18 O6 23.4(11) 23 . . . ? Ni1 O5 C18 C19 -156.5(4) 23 . . . ? Ni1 O6 C18 O5 27.8(10) 24 . . . ? Ni1 O6 C18 C19 -152.3(4) 24 . . . ? O5 C18 C19 C20 155.4(7) . . . . ? O6 C18 C19 C20 -24.5(10) . . . . ? O5 C18 C19 C24 -27.4(10) . . . . ? O6 C18 C19 C24 152.7(7) . . . . ? C24 C19 C20 C21 2.6(12) . . . . ? C18 C19 C20 C21 179.8(8) . . . . ? C19 C20 C21 C22 -4.8(13) . . . . ? C20 C21 C22 C23 2.9(12) . . . . ? C20 C21 C22 S2 -175.3(7) . . . . ? O4 S2 C22 C21 -36.7(7) . . . . ? O3 S2 C22 C21 -169.0(6) . . . . ? C15 S2 C22 C21 77.0(7) . . . . ? O4 S2 C22 C23 145.3(6) . . . . ? O3 S2 C22 C23 12.9(7) . . . . ? C15 S2 C22 C23 -101.0(6) . . . . ? C21 C22 C23 C24 1.3(11) . . . . ? S2 C22 C23 C24 179.4(6) . . . . ? C20 C19 C24 C23 1.6(11) . . . . ? C18 C19 C24 C23 -175.5(7) . . . . ? C22 C23 C24 C19 -3.6(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C10 H10 O5 0.93 2.39 2.931(11) 116.9 19 C23 H23 O3 0.93 2.53 3.314(9) 142.0 14 C9 H9 O4 0.93 2.33 3.101(9) 139.5 32_455 O1W H1A O2 0.82 2.12 2.936(7) 177.8 . O7 H7A O2 0.82 1.79 2.574(6) 159.2 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.599 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.079 _vrf_PLAT213_d ; PROBLEM: Atom C8 has ADP max/min Ratio ..... 4.10 prola RESPONSE: This alert results from the disorder of the dsa molecule. ; _vrf_PLAT220_d ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.13 Ratio RESPONSE: This alert results from the disorder of the dsa molecule. ; _vrf_PLAT242_d ; PROBLEM: Check Low Ueq as Compared to Neighbors for C3 RESPONSE: This alert results from the disorder of the dsa molecule. ; # Attachment '- 2.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 778542' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H34 Co2 N4 O13 S4, H2 O, 0.2(O)' _chemical_formula_sum 'C48 H36 Co2 N4 O14.20 S4' _chemical_formula_weight 1142.15 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Fddd loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 11.4184(10) _cell_length_b 40.061(4) _cell_length_c 42.963(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 19653(3) _cell_formula_units_Z 16 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3441 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 22.28 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.544 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9337.6 _exptl_absorpt_coefficient_mu 0.917 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30570 _diffrn_reflns_av_R_equivalents 0.0718 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 48 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4574 _reflns_number_gt 3360 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0330P)^2^+69.5337P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4574 _refine_ls_number_parameters 366 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.066 _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 0.07528(4) 0.167220(10) 0.510534(10) 0.02998(13) Uani 1 1 d . . . N1 N -0.4017(2) 0.32649(7) 0.46936(6) 0.0419(7) Uani 1 1 d D . . C1 C -0.3737(6) 0.33323(14) 0.44090(15) 0.048(2) Uani 0.574(7) 1 d PD A 1 H1 H -0.4315 0.3426 0.4284 0.058 Uiso 0.574(7) 1 calc PR A 1 C2 C -0.2663(6) 0.32774(16) 0.42744(16) 0.049(2) Uani 0.574(7) 1 d PD A 1 H2 H -0.2527 0.3339 0.4069 0.059 Uiso 0.574(7) 1 calc PR A 1 C3 C -0.1799(3) 0.31318(8) 0.44460(8) 0.0468(9) Uani 1 1 d D . . C4 C -0.2027(6) 0.3065(2) 0.47519(17) 0.076(3) Uani 0.574(7) 1 d PD A 1 H4 H -0.1450 0.2975 0.4879 0.092 Uiso 0.574(7) 1 calc PR A 1 C5 C -0.3116(6) 0.3134(2) 0.48682(18) 0.076(3) Uani 0.574(7) 1 d PD A 1 H5 H -0.3257 0.3089 0.5077 0.091 Uiso 0.574(7) 1 calc PR A 1 C1' C -0.3342(8) 0.3500(2) 0.4581(2) 0.064(4) Uani 0.426(7) 1 d PD A 2 H1' H -0.3615 0.3719 0.4586 0.077 Uiso 0.426(7) 1 calc PR A 2 C2' C -0.2263(8) 0.3443(2) 0.4456(2) 0.071(4) Uani 0.426(7) 1 d PD A 2 H2' H -0.1837 0.3621 0.4376 0.085 Uiso 0.426(7) 1 calc PR A 2 C4' C -0.2503(8) 0.2873(2) 0.4557(2) 0.054(3) Uani 0.426(7) 1 d PD A 2 H4' H -0.2242 0.2653 0.4550 0.065 Uiso 0.426(7) 1 calc PR A 2 C5' C -0.3592(8) 0.2948(2) 0.4677(2) 0.058(3) Uani 0.426(7) 1 d PD A 2 H5' H -0.4058 0.2774 0.4749 0.070 Uiso 0.426(7) 1 calc PR A 2 S1 S -0.04044(10) 0.30612(3) 0.42743(3) 0.0692(4) Uani 1 1 d . A . S2 S 0.40375(8) 0.31007(2) 0.63685(2) 0.0391(2) Uani 1 1 d . . . O1 O 0.1347(2) 0.19880(5) 0.54619(5) 0.0387(6) Uani 1 1 d . . . O2 O 0.2281(3) 0.16383(6) 0.57792(6) 0.0565(7) Uani 1 1 d . . . O3 O 0.4235(2) 0.33411(6) 0.61275(6) 0.0519(7) Uani 1 1 d . . . O4 O 0.5003(2) 0.29738(6) 0.65467(6) 0.0558(7) Uani 1 1 d . . . O5 O 0.0041(2) 0.38906(5) 0.72641(5) 0.0382(6) Uani 1 1 d . . . O6 O -0.0059(2) 0.33609(5) 0.74305(5) 0.0383(5) Uani 1 1 d . . . O7 O 0.1250 0.1250 0.53885(6) 0.0332(7) Uani 1 2 d S . . H7A H 0.1729 0.1339 0.5504 0.040 Uiso 1 1 d R . . N2 N 0.0511(2) 0.21044(6) 0.48011(6) 0.0349(7) Uani 1 1 d . A . C6 C 0.1002(4) 0.23967(9) 0.48724(8) 0.0480(9) Uani 1 1 d . . . H6 H 0.1514 0.2404 0.5040 0.058 Uiso 1 1 calc R . . C7 C 0.0793(3) 0.26898(9) 0.47109(9) 0.0495(10) Uani 1 1 d . A . H7 H 0.1176 0.2886 0.4765 0.059 Uiso 1 1 calc R . . C8 C 0.0006(3) 0.26849(9) 0.44677(9) 0.0425(9) Uani 1 1 d . . . C9 C -0.0412(4) 0.23829(10) 0.43752(10) 0.0599(11) Uani 1 1 d . A . H9 H -0.0878 0.2366 0.4198 0.072 Uiso 1 1 calc R . . C10 C -0.0140(4) 0.21033(9) 0.45452(9) 0.0537(10) Uani 1 1 d . . . H10 H -0.0432 0.1900 0.4477 0.064 Uiso 1 1 calc R A . C11 C 0.1947(3) 0.19226(8) 0.57004(7) 0.0347(8) Uani 1 1 d . . . C12 C 0.2336(3) 0.22160(8) 0.58950(7) 0.0316(7) Uani 1 1 d . . . C13 C 0.2072(3) 0.25382(8) 0.58034(8) 0.0413(9) Uani 1 1 d . . . H13 H 0.1551 0.2573 0.5640 0.050 Uiso 1 1 calc R . . C14 C 0.2570(3) 0.28085(9) 0.59510(8) 0.0417(9) Uani 1 1 d . . . H14 H 0.2411 0.3024 0.5883 0.050 Uiso 1 1 calc R . . C15 C 0.3306(3) 0.27552(8) 0.62000(7) 0.0333(7) Uani 1 1 d . . . C16 C 0.3529(3) 0.24367(8) 0.63055(8) 0.0411(9) Uani 1 1 d . . . H16 H 0.4006 0.2403 0.6478 0.049 Uiso 1 1 calc R . . C17 C 0.3040(3) 0.21686(8) 0.61540(7) 0.0397(8) Uani 1 1 d . . . H17 H 0.3184 0.1953 0.6226 0.048 Uiso 1 1 calc R . . C18 C 0.0358(3) 0.35898(8) 0.72637(7) 0.0324(7) Uani 1 1 d . . . C19 C 0.1314(3) 0.34898(8) 0.70427(7) 0.0327(7) Uani 1 1 d . . . C20 C 0.2025(4) 0.32221(10) 0.71171(8) 0.0576(12) Uani 1 1 d . . . H20 H 0.1923 0.3115 0.7307 0.069 Uiso 1 1 calc R . . C21 C 0.2875(4) 0.31111(10) 0.69175(9) 0.0560(11) Uani 1 1 d . . . H21 H 0.3357 0.2933 0.6973 0.067 Uiso 1 1 calc R . . C22 C 0.3008(3) 0.32657(8) 0.66344(7) 0.0338(8) Uani 1 1 d . . . C23 C 0.2314(3) 0.35331(8) 0.65547(7) 0.0366(8) Uani 1 1 d . . . H23 H 0.2407 0.3636 0.6362 0.044 Uiso 1 1 calc R . . C24 C 0.1477(3) 0.36487(8) 0.67611(7) 0.0358(8) Uani 1 1 d . . . H24 H 0.1025 0.3834 0.6710 0.043 Uiso 1 1 calc R . . O1W O 0.3492(4) 0.1250 0.6250 0.0915(15) Uani 1 2 d S . . H1A H 0.3154 0.1360 0.6116 0.110 Uiso 1 1 d R . . O2W O 0.6250 0.1250 0.6250 0.104(6) Uani 0.40 4 d SP . . 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 0.0316(2) 0.0254(2) 0.0329(2) -0.00197(18) -0.00121(19) 0.00185(19) N1 0.0360(17) 0.0432(18) 0.0465(18) 0.0001(14) 0.0044(14) 0.0083(14) C1 0.039(4) 0.062(5) 0.044(4) 0.011(4) 0.000(3) 0.021(4) C2 0.043(4) 0.066(5) 0.039(4) 0.013(4) 0.008(3) 0.012(4) C3 0.042(2) 0.040(2) 0.059(2) 0.0115(18) 0.0135(19) 0.0101(17) C4 0.039(4) 0.136(9) 0.054(5) 0.028(6) 0.006(4) 0.039(5) C5 0.045(5) 0.132(9) 0.050(5) 0.029(5) 0.005(4) 0.027(5) C1' 0.051(7) 0.037(6) 0.104(10) 0.023(6) 0.023(7) 0.014(5) C2' 0.046(7) 0.042(6) 0.125(11) 0.031(7) 0.036(7) 0.003(5) C4' 0.052(6) 0.040(5) 0.070(7) 0.004(5) 0.019(5) 0.012(5) C5' 0.048(6) 0.038(5) 0.089(8) -0.002(5) 0.023(6) -0.001(5) S1 0.0528(7) 0.0554(7) 0.0992(9) 0.0384(6) 0.0350(6) 0.0235(5) S2 0.0353(5) 0.0357(5) 0.0463(5) -0.0127(4) 0.0057(4) -0.0028(4) O1 0.0466(14) 0.0324(12) 0.0370(13) -0.0056(10) -0.0075(11) 0.0030(11) O2 0.081(2) 0.0317(14) 0.0564(16) -0.0032(12) -0.0289(15) 0.0029(13) O3 0.0623(17) 0.0409(15) 0.0525(15) -0.0098(12) 0.0219(13) -0.0156(13) O4 0.0353(14) 0.0589(17) 0.0730(18) -0.0243(14) -0.0089(13) 0.0044(13) O5 0.0465(15) 0.0284(13) 0.0398(13) -0.0019(10) 0.0098(11) -0.0003(11) O6 0.0389(14) 0.0303(12) 0.0458(13) 0.0044(11) 0.0095(11) 0.0009(11) O7 0.0342(18) 0.0311(17) 0.0344(17) 0.000 0.000 -0.0028(14) N2 0.0403(17) 0.0274(15) 0.0371(16) -0.0025(12) -0.0029(13) 0.0016(13) C6 0.062(3) 0.045(2) 0.037(2) 0.0011(17) -0.0060(18) -0.0078(19) C7 0.062(3) 0.034(2) 0.052(2) -0.0030(17) 0.010(2) -0.0102(19) C8 0.032(2) 0.039(2) 0.057(2) 0.0093(17) 0.0126(18) 0.0085(16) C9 0.062(3) 0.049(2) 0.069(3) 0.018(2) -0.024(2) -0.004(2) C10 0.068(3) 0.035(2) 0.057(2) 0.0004(18) -0.023(2) -0.0052(19) C11 0.0353(19) 0.0339(19) 0.0349(19) -0.0030(15) 0.0010(15) -0.0022(16) C12 0.0323(18) 0.0308(18) 0.0316(17) -0.0036(14) 0.0023(14) -0.0014(14) C13 0.044(2) 0.036(2) 0.043(2) -0.0080(16) -0.0073(17) 0.0104(16) C14 0.048(2) 0.0305(19) 0.047(2) -0.0052(16) -0.0065(18) 0.0100(16) C15 0.0342(19) 0.0291(17) 0.0366(18) -0.0077(14) 0.0035(15) 0.0015(14) C16 0.048(2) 0.038(2) 0.0375(19) -0.0025(16) -0.0095(17) -0.0024(17) C17 0.052(2) 0.0301(19) 0.0374(19) 0.0032(15) -0.0027(17) -0.0013(16) C18 0.0328(18) 0.0311(19) 0.0334(17) -0.0027(15) -0.0044(15) 0.0000(15) C19 0.0373(19) 0.0272(17) 0.0337(18) -0.0022(14) 0.0053(15) -0.0013(15) C20 0.074(3) 0.060(3) 0.039(2) 0.0189(19) 0.016(2) 0.031(2) C21 0.062(3) 0.054(2) 0.051(2) 0.0104(19) 0.012(2) 0.030(2) C22 0.0362(19) 0.0306(18) 0.0345(18) -0.0080(14) 0.0043(15) -0.0018(15) C23 0.045(2) 0.0303(18) 0.0349(18) 0.0005(14) 0.0053(16) -0.0016(16) C24 0.039(2) 0.0274(18) 0.0409(19) 0.0010(15) 0.0051(16) 0.0068(15) O1W 0.120(4) 0.081(3) 0.073(3) 0.025(3) 0.000 0.000 O2W 0.155(18) 0.077(12) 0.080(12) 0.000 0.000 0.000 _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 O5 2.060(2) 19 ? Co1 O6 2.073(2) 32 ? Co1 O1 2.100(2) . ? Co1 O7 2.1593(16) . ? Co1 N1 2.177(3) 29_456 ? Co1 N2 2.187(3) . ? N1 C1 1.292(7) . ? N1 C1' 1.311(9) . ? N1 C5' 1.362(8) . ? N1 C5 1.377(7) . ? N1 Co1 2.177(3) 29_456 ? C1 C2 1.374(8) . ? C1 H1 0.9300 . ? C2 C3 1.363(7) . ? C2 H2 0.9300 . ? C3 C2' 1.356(9) . ? C3 C4 1.366(7) . ? C3 C4' 1.397(9) . ? C3 S1 1.777(4) . ? C4 C5 1.368(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C1' C2' 1.362(11) . ? C1' H1' 0.9300 . ? C2' H2' 0.9300 . ? C4' C5' 1.379(10) . ? C4' H4' 0.9300 . ? C5' H5' 0.9300 . ? S1 C8 1.784(4) . ? S2 O3 1.432(3) . ? S2 O4 1.435(3) . ? S2 C22 1.767(3) . ? S2 C15 1.771(3) . ? O1 C11 1.260(4) . ? O2 C11 1.248(4) . ? O5 C18 1.258(4) . ? O5 Co1 2.060(2) 23 ? O6 C18 1.258(4) . ? O6 Co1 2.073(2) 24 ? O7 Co1 2.1593(16) 2 ? O7 H7A 0.8198 . ? N2 C10 1.328(4) . ? N2 C6 1.334(4) . ? C6 C7 1.385(5) . ? C6 H6 0.9300 . ? C7 C8 1.378(5) . ? C7 H7 0.9300 . ? C8 C9 1.360(5) . ? C9 C10 1.373(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.509(4) . ? C12 C13 1.383(4) . ? C12 C17 1.386(4) . ? C13 C14 1.377(5) . ? C13 H13 0.9300 . ? C14 C15 1.377(4) . ? C14 H14 0.9300 . ? C15 C16 1.378(4) . ? C16 C17 1.374(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.501(4) . ? C19 C24 1.380(4) . ? C19 C20 1.382(5) . ? C20 C21 1.370(5) . ? C20 H20 0.9300 . ? C21 C22 1.374(5) . ? C21 H21 0.9300 . ? C22 C23 1.376(4) . ? C23 C24 1.383(4) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? O1W H1A 0.8202 . ? 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 O5 Co1 O6 96.69(9) 19 32 ? O5 Co1 O1 172.54(9) 19 . ? O6 Co1 O1 90.12(9) 32 . ? O5 Co1 O7 95.04(8) 19 . ? O6 Co1 O7 84.80(7) 32 . ? O1 Co1 O7 88.62(8) . . ? O5 Co1 N1 86.85(10) 19 29_456 ? O6 Co1 N1 176.26(10) 32 29_456 ? O1 Co1 N1 86.29(10) . 29_456 ? O7 Co1 N1 96.12(8) . 29_456 ? O5 Co1 N2 87.29(9) 19 . ? O6 Co1 N2 87.22(10) 32 . ? O1 Co1 N2 89.99(9) . . ? O7 Co1 N2 171.90(8) . . ? N1 Co1 N2 91.76(10) 29_456 . ? C1 N1 C1' 49.7(3) . . ? C1 N1 C5' 93.2(4) . . ? C1' N1 C5' 116.2(6) . . ? C1 N1 C5 114.3(5) . . ? C1' N1 C5 92.2(4) . . ? C5' N1 C5 53.6(4) . . ? C1 N1 Co1 125.2(3) . 29_456 ? C1' N1 Co1 126.8(4) . 29_456 ? C5' N1 Co1 117.0(4) . 29_456 ? C5 N1 Co1 120.5(3) . 29_456 ? N1 C1 C2 125.8(6) . . ? N1 C1 H1 117.1 . . ? C2 C1 H1 117.1 . . ? C3 C2 C1 119.1(6) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2' C3 C2 48.7(4) . . ? C2' C3 C4 94.2(5) . . ? C2 C3 C4 117.8(5) . . ? C2' C3 C4' 116.6(6) . . ? C2 C3 C4' 94.9(5) . . ? C4 C3 C4' 54.3(4) . . ? C2' C3 S1 120.7(5) . . ? C2 C3 S1 119.5(4) . . ? C4 C3 S1 122.6(4) . . ? C4' C3 S1 122.6(4) . . ? C3 C4 C5 119.1(6) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 N1 123.8(6) . . ? C4 C5 H5 118.1 . . ? N1 C5 H5 118.1 . . ? N1 C1' C2' 123.8(8) . . ? N1 C1' H1' 118.1 . . ? C2' C1' H1' 118.1 . . ? C3 C2' C1' 121.4(8) . . ? C3 C2' H2' 119.3 . . ? C1' C2' H2' 119.3 . . ? C5' C4' C3 119.0(7) . . ? C5' C4' H4' 120.5 . . ? C3 C4' H4' 120.5 . . ? N1 C5' C4' 123.0(8) . . ? N1 C5' H5' 118.5 . . ? C4' C5' H5' 118.5 . . ? C3 S1 C8 100.17(16) . . ? O3 S2 O4 120.19(17) . . ? O3 S2 C22 108.72(15) . . ? O4 S2 C22 107.35(15) . . ? O3 S2 C15 107.73(15) . . ? O4 S2 C15 107.66(15) . . ? C22 S2 C15 104.05(15) . . ? C11 O1 Co1 130.1(2) . . ? C18 O5 Co1 130.7(2) . 23 ? C18 O6 Co1 127.2(2) . 24 ? Co1 O7 Co1 111.43(12) 2 . ? Co1 O7 H7A 120.3 2 . ? Co1 O7 H7A 100.2 . . ? C10 N2 C6 115.3(3) . . ? C10 N2 Co1 124.3(2) . . ? C6 N2 Co1 120.3(2) . . ? N2 C6 C7 123.9(3) . . ? N2 C6 H6 118.1 . . ? C7 C6 H6 118.1 . . ? C8 C7 C6 118.7(3) . . ? C8 C7 H7 120.7 . . ? C6 C7 H7 120.7 . . ? C9 C8 C7 117.6(3) . . ? C9 C8 S1 121.6(3) . . ? C7 C8 S1 120.8(3) . . ? C8 C9 C10 119.4(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 124.4(4) . . ? N2 C10 H10 117.8 . . ? C9 C10 H10 117.8 . . ? O2 C11 O1 125.2(3) . . ? O2 C11 C12 118.1(3) . . ? O1 C11 C12 116.7(3) . . ? C13 C12 C17 118.9(3) . . ? C13 C12 C11 120.3(3) . . ? C17 C12 C11 120.6(3) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 120.8(3) . . ? C14 C15 S2 118.9(3) . . ? C16 C15 S2 120.2(3) . . ? C17 C16 C15 119.6(3) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C12 120.6(3) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? O6 C18 O5 126.1(3) . . ? O6 C18 C19 116.2(3) . . ? O5 C18 C19 117.8(3) . . ? C24 C19 C20 118.8(3) . . ? C24 C19 C18 122.0(3) . . ? C20 C19 C18 119.2(3) . . ? C21 C20 C19 121.6(3) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 119.1(3) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C21 C22 C23 120.5(3) . . ? C21 C22 S2 118.5(3) . . ? C23 C22 S2 120.9(2) . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C19 C24 C23 120.1(3) . . ? C19 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1' N1 C1 C2 72.3(6) . . . . ? C5' N1 C1 C2 -49.8(4) . . . . ? C5 N1 C1 C2 1.5(3) . . . . ? Co1 N1 C1 C2 -176.3(2) 29_456 . . . ? N1 C1 C2 C3 1.7(3) . . . . ? C1 C2 C3 C2' -73.3(6) . . . . ? C1 C2 C3 C4 -3.8(6) . . . . ? C1 C2 C3 C4' 48.1(4) . . . . ? C1 C2 C3 S1 -179.8(2) . . . . ? C2' C3 C4 C5 47.6(7) . . . . ? C2 C3 C4 C5 2.8(8) . . . . ? C4' C3 C4 C5 -72.3(7) . . . . ? S1 C3 C4 C5 178.6(4) . . . . ? C3 C4 C5 N1 0.5(9) . . . . ? C1 N1 C5 C4 -2.6(7) . . . . ? C1' N1 C5 C4 -48.8(7) . . . . ? C5' N1 C5 C4 72.6(7) . . . . ? Co1 N1 C5 C4 175.3(5) 29_456 . . . ? C1 N1 C1' C2' -71.6(6) . . . . ? C5' N1 C1' C2' -1.1(3) . . . . ? C5 N1 C1' C2' 48.9(3) . . . . ? Co1 N1 C1' C2' -179.6(3) 29_456 . . . ? C2 C3 C2' C1' 74.6(6) . . . . ? C4 C3 C2' C1' -49.2(5) . . . . ? C4' C3 C2' C1' 2.7(6) . . . . ? S1 C3 C2' C1' 178.5(3) . . . . ? N1 C1' C2' C3 -1.2(3) . . . . ? C2' C3 C4' C5' -1.9(8) . . . . ? C2 C3 C4' C5' -47.7(6) . . . . ? C4 C3 C4' C5' 73.2(7) . . . . ? S1 C3 C4' C5' -177.7(5) . . . . ? C1 N1 C5' C4' 47.9(6) . . . . ? C1' N1 C5' C4' 1.9(7) . . . . ? C5 N1 C5' C4' -70.0(7) . . . . ? Co1 N1 C5' C4' -179.5(5) 29_456 . . . ? C3 C4' C5' N1 -0.3(9) . . . . ? C2' C3 S1 C8 156.3(5) . . . . ? C2 C3 S1 C8 -146.8(4) . . . . ? C4 C3 S1 C8 37.5(5) . . . . ? C4' C3 S1 C8 -28.2(5) . . . . ? O6 Co1 O1 C11 -72.9(3) 32 . . . ? O7 Co1 O1 C11 11.9(3) . . . . ? N1 Co1 O1 C11 108.2(3) 29_456 . . . ? N2 Co1 O1 C11 -160.1(3) . . . . ? O5 Co1 O7 Co1 36.42(7) 19 . . 2 ? O6 Co1 O7 Co1 -59.86(6) 32 . . 2 ? O1 Co1 O7 Co1 -150.10(7) . . . 2 ? N1 Co1 O7 Co1 123.78(7) 29_456 . . 2 ? O5 Co1 N2 C10 10.7(3) 19 . . . ? O6 Co1 N2 C10 107.5(3) 32 . . . ? O1 Co1 N2 C10 -162.4(3) . . . . ? N1 Co1 N2 C10 -76.1(3) 29_456 . . . ? O5 Co1 N2 C6 -171.6(3) 19 . . . ? O6 Co1 N2 C6 -74.8(3) 32 . . . ? O1 Co1 N2 C6 15.4(3) . . . . ? N1 Co1 N2 C6 101.6(3) 29_456 . . . ? C10 N2 C6 C7 5.0(5) . . . . ? Co1 N2 C6 C7 -173.0(3) . . . . ? N2 C6 C7 C8 2.1(6) . . . . ? C6 C7 C8 C9 -8.0(5) . . . . ? C6 C7 C8 S1 174.1(3) . . . . ? C3 S1 C8 C9 80.1(4) . . . . ? C3 S1 C8 C7 -102.0(3) . . . . ? C7 C8 C9 C10 6.9(6) . . . . ? S1 C8 C9 C10 -175.2(3) . . . . ? C6 N2 C10 C9 -6.3(6) . . . . ? Co1 N2 C10 C9 171.5(3) . . . . ? C8 C9 C10 N2 0.4(7) . . . . ? Co1 O1 C11 O2 -3.0(5) . . . . ? Co1 O1 C11 C12 173.8(2) . . . . ? O2 C11 C12 C13 174.6(3) . . . . ? O1 C11 C12 C13 -2.4(5) . . . . ? O2 C11 C12 C17 -0.2(5) . . . . ? O1 C11 C12 C17 -177.2(3) . . . . ? C17 C12 C13 C14 5.0(5) . . . . ? C11 C12 C13 C14 -169.9(3) . . . . ? C12 C13 C14 C15 -2.4(5) . . . . ? C13 C14 C15 C16 -1.2(5) . . . . ? C13 C14 C15 S2 174.9(3) . . . . ? O3 S2 C15 C14 -30.7(3) . . . . ? O4 S2 C15 C14 -161.6(3) . . . . ? C22 S2 C15 C14 84.6(3) . . . . ? O3 S2 C15 C16 145.5(3) . . . . ? O4 S2 C15 C16 14.5(3) . . . . ? C22 S2 C15 C16 -99.2(3) . . . . ? C14 C15 C16 C17 2.1(5) . . . . ? S2 C15 C16 C17 -173.9(3) . . . . ? C15 C16 C17 C12 0.6(5) . . . . ? C13 C12 C17 C16 -4.1(5) . . . . ? C11 C12 C17 C16 170.8(3) . . . . ? Co1 O6 C18 O5 29.0(5) 24 . . . ? Co1 O6 C18 C19 -150.4(2) 24 . . . ? Co1 O5 C18 O6 24.7(5) 23 . . . ? Co1 O5 C18 C19 -155.9(2) 23 . . . ? O6 C18 C19 C24 149.2(3) . . . . ? O5 C18 C19 C24 -30.2(5) . . . . ? O6 C18 C19 C20 -28.2(5) . . . . ? O5 C18 C19 C20 152.4(3) . . . . ? C24 C19 C20 C21 -0.5(6) . . . . ? C18 C19 C20 C21 177.0(4) . . . . ? C19 C20 C21 C22 -1.3(7) . . . . ? C20 C21 C22 C23 1.4(6) . . . . ? C20 C21 C22 S2 -175.5(3) . . . . ? O3 S2 C22 C21 -166.1(3) . . . . ? O4 S2 C22 C21 -34.6(3) . . . . ? C15 S2 C22 C21 79.3(3) . . . . ? O3 S2 C22 C23 17.0(3) . . . . ? O4 S2 C22 C23 148.4(3) . . . . ? C15 S2 C22 C23 -97.6(3) . . . . ? C21 C22 C23 C24 0.2(5) . . . . ? S2 C22 C23 C24 177.1(3) . . . . ? C20 C19 C24 C23 2.1(5) . . . . ? C18 C19 C24 C23 -175.3(3) . . . . ? C22 C23 C24 C19 -2.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7A O2 0.82 1.80 2.574(3) 157.1 . O1W H1A O2 0.82 2.08 2.902(3) 179.4 . C6 H6 O1 0.93 2.47 3.042(4) 120.0 . C9 H9 O4 0.93 2.39 3.115(5) 135.1 32_455 C10 H10 O5 0.93 2.43 3.008(4) 120.7 19 C23 H23 O3 0.93 2.52 3.291(4) 140.2 14 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.374 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.065