# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1974 data_cobzl7a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Co8 N107 O32 S24 C193 H308' _chemical_formula_sum 'C193 H308 Co8 N107 O32 S24' _chemical_formula_weight 5880.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 53.242(11) _cell_length_b 33.671(7) _cell_length_c 33.537(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 60122(21) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Green _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.58 _exptl_crystal_size_min 0.51 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 24568 _exptl_absorpt_coefficient_mu 5.539 _exptl_absorpt_correction_type 'Face-indexed' _exptl_absorpt_correction_T_min 0.062 _exptl_absorpt_correction_T_max 0.157 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5 _diffrn_reflns_number 23565 _diffrn_reflns_av_R_equivalents 0.0630 _diffrn_reflns_av_sigmaI/netI 0.2939 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 40.00 _reflns_number_total 18245 _reflns_number_gt 7035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000031(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 18245 _refine_ls_number_parameters 1762 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.2941 _refine_ls_R_factor_gt 0.1373 _refine_ls_wR_factor_ref 0.4236 _refine_ls_wR_factor_gt 0.3361 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.28151(11) 0.82786(16) 0.83667(18) 0.0429(19) Uani 1 1 d . . . Co2 Co 0.24618(10) 0.58875(15) 0.99769(17) 0.0364(18) Uani 1 1 d . . . Co3 Co 0.31993(10) 0.82370(16) 1.12304(18) 0.0427(19) Uani 1 1 d . . . Co4 Co 0.05691(11) 0.14156(17) 0.86609(19) 0.049(2) Uani 1 1 d . . . Co5 Co 0.14255(10) 0.82805(16) 1.02975(18) 0.0423(19) Uani 1 1 d . . . Co6 Co 0.04018(11) -0.61652(18) 1.3821(2) 0.058(2) Uani 1 1 d . . . Co7 Co -0.08271(11) -0.40568(16) 1.31400(19) 0.045(2) Uani 1 1 d . . . Co8 Co 0.08320(12) 0.09539(19) 1.1868(2) 0.070(2) Uani 1 1 d . . . S1 S 0.31669(17) 0.8022(3) 0.8088(3) 0.049(3) Uani 1 1 d . . . N1A N 0.3066(5) 0.8224(7) 0.8788(9) 0.028(8) Uiso 1 1 d D . . C1A C 0.3245(7) 0.8050(8) 0.8596(11) 0.044(12) Uiso 1 1 d D . . N1B N 0.3460(5) 0.7896(7) 0.8761(9) 0.039(9) Uiso 1 1 d D . . C1B C 0.3474(7) 0.7933(10) 0.9145(13) 0.051(12) Uiso 1 1 d D . . N1C N 0.3287(5) 0.8115(7) 0.9366(8) 0.031(8) Uiso 1 1 d D . . H1CA H 0.3299 0.8135 0.9621 0.037 Uiso 1 1 calc R . . C1C C 0.3087(7) 0.8260(10) 0.9167(13) 0.036(12) Uiso 1 1 d D . . O1 O 0.2927(4) 0.8430(6) 0.9372(7) 0.044(7) Uani 1 1 d . . . N1D N 0.3677(5) 0.7804(8) 0.9331(9) 0.035(9) Uiso 1 1 d . . . C1D C 0.3866(6) 0.7563(10) 0.9125(11) 0.049(12) Uiso 1 1 d . . . H1DA H 0.3791 0.7438 0.8894 0.059 Uiso 1 1 calc R . . H1DB H 0.3925 0.7355 0.9302 0.059 Uiso 1 1 calc R . . C1E C 0.4081(8) 0.7811(13) 0.8998(13) 0.113(18) Uiso 1 1 d . . . H1EA H 0.4197 0.7651 0.8850 0.169 Uiso 1 1 calc R . . H1EB H 0.4163 0.7919 0.9228 0.169 Uiso 1 1 calc R . . H1EC H 0.4021 0.8024 0.8832 0.169 Uiso 1 1 calc R . . C1F C 0.3734(7) 0.7858(11) 0.9733(12) 0.065(13) Uiso 1 1 d . . . H1FA H 0.3872 0.7684 0.9804 0.078 Uiso 1 1 calc R . . H1FB H 0.3589 0.7779 0.9890 0.078 Uiso 1 1 calc R . . C1G C 0.3806(8) 0.8298(11) 0.9848(13) 0.097(17) Uiso 1 1 d . . . H1GA H 0.3832 0.8316 1.0131 0.145 Uiso 1 1 calc R . . H1GB H 0.3673 0.8474 0.9770 0.145 Uiso 1 1 calc R . . H1GC H 0.3958 0.8372 0.9712 0.145 Uiso 1 1 calc R . . S2 S 0.25351(18) 0.8185(3) 0.7857(3) 0.048(3) Uani 1 1 d . . . N2A N 0.2666(4) 0.7751(8) 0.8439(8) 0.027(8) Uiso 1 1 d . . . C2A C 0.2497(7) 0.7769(11) 0.8105(11) 0.045(11) Uiso 1 1 d . . . N2B N 0.2339(5) 0.7462(9) 0.8026(9) 0.050(9) Uiso 1 1 d . . . C2B C 0.2357(6) 0.7158(11) 0.8286(11) 0.035(11) Uiso 1 1 d . . . N2C N 0.2506(5) 0.7152(8) 0.8599(8) 0.042(9) Uiso 1 1 d . . . H2CA H 0.2495 0.6952 0.8758 0.051 Uiso 1 1 calc R . . C2C C 0.2687(7) 0.7455(12) 0.8697(12) 0.037(12) Uiso 1 1 d . . . O2 O 0.2839(4) 0.7405(7) 0.8946(7) 0.051(8) Uani 1 1 d . . . N2D N 0.2222(5) 0.6826(9) 0.8209(9) 0.046(9) Uiso 1 1 d . . . C2D C 0.2051(6) 0.6813(11) 0.7860(11) 0.059(13) Uiso 1 1 d . . . H2DA H 0.2041 0.6541 0.7766 0.071 Uiso 1 1 calc R . . H2DB H 0.2123 0.6971 0.7648 0.071 Uiso 1 1 calc R . . C2E C 0.1793(7) 0.6960(11) 0.7946(12) 0.091(16) Uiso 1 1 d . . . H2EA H 0.1700 0.6977 0.7702 0.136 Uiso 1 1 calc R . . H2EB H 0.1803 0.7218 0.8067 0.136 Uiso 1 1 calc R . . H2EC H 0.1711 0.6779 0.8125 0.136 Uiso 1 1 calc R . . C2F C 0.2208(6) 0.6485(10) 0.8492(11) 0.050(12) Uiso 1 1 d . . . H2FA H 0.2212 0.6583 0.8764 0.060 Uiso 1 1 calc R . . H2FB H 0.2052 0.6343 0.8453 0.060 Uiso 1 1 calc R . . C2G C 0.2414(6) 0.6226(10) 0.8428(11) 0.072(14) Uiso 1 1 d . . . H2GA H 0.2411 0.6018 0.8623 0.108 Uiso 1 1 calc R . . H2GB H 0.2568 0.6372 0.8451 0.108 Uiso 1 1 calc R . . H2GC H 0.2402 0.6113 0.8166 0.108 Uiso 1 1 calc R . . S3 S 0.28943(17) 0.8940(3) 0.8301(3) 0.046(3) Uani 1 1 d . . . N3A N 0.2563(5) 0.8573(8) 0.8650(8) 0.027(8) Uiso 1 1 d . . . C3A C 0.2644(7) 0.8941(12) 0.8620(12) 0.056(13) Uiso 1 1 d . . . N3B N 0.2531(6) 0.9274(9) 0.8774(9) 0.054(10) Uiso 1 1 d . . . C3B C 0.2333(7) 0.9209(12) 0.9004(12) 0.050(12) Uiso 1 1 d . . . N3C N 0.2247(5) 0.8841(8) 0.9047(8) 0.038(9) Uiso 1 1 d . . . H3CA H 0.2115 0.8806 0.9191 0.046 Uiso 1 1 calc R . . C3C C 0.2358(7) 0.8506(12) 0.8872(11) 0.033(11) Uiso 1 1 d . . . O3 O 0.2248(4) 0.8176(7) 0.8907(7) 0.050(8) Uani 1 1 d . . . N3D N 0.2220(6) 0.9500(9) 0.9171(9) 0.051(10) Uiso 1 1 d . . . C3D C 0.2324(6) 0.9899(9) 0.9142(11) 0.044(11) Uiso 1 1 d . . . H3D1 H 0.2349 1.0007 0.9407 0.053 Uiso 1 1 calc R . . H3D2 H 0.2485 0.9890 0.9008 0.053 Uiso 1 1 calc R . . C3E C 0.2154(7) 1.0144(12) 0.8924(12) 0.095(16) Uiso 1 1 d . . . H3EA H 0.2223 1.0406 0.8901 0.142 Uiso 1 1 calc R . . H3EB H 0.1996 1.0156 0.9062 0.142 Uiso 1 1 calc R . . H3EC H 0.2129 1.0034 0.8663 0.142 Uiso 1 1 calc R . . C3F C 0.2010(6) 0.9448(10) 0.9426(11) 0.046(12) Uiso 1 1 d . . . H3FA H 0.1991 0.9683 0.9591 0.055 Uiso 1 1 calc R . . H3FB H 0.2043 0.9225 0.9602 0.055 Uiso 1 1 calc R . . C3G C 0.1768(7) 0.9375(12) 0.9203(13) 0.099(17) Uiso 1 1 d . . . H3GA H 0.1632 0.9357 0.9390 0.148 Uiso 1 1 calc R . . H3GB H 0.1780 0.9131 0.9057 0.148 Uiso 1 1 calc R . . H3GC H 0.1738 0.9590 0.9022 0.148 Uiso 1 1 calc R . . S4 S 0.22809(18) 0.5574(3) 1.0518(3) 0.046(3) Uani 1 1 d . . . N4A N 0.2548(6) 0.6186(9) 1.0451(9) 0.059(10) Uiso 1 1 d . . . C4A C 0.2428(7) 0.5976(12) 1.0745(14) 0.065(14) Uiso 1 1 d . . . N4B N 0.2417(5) 0.6050(9) 1.1134(10) 0.049(9) Uiso 1 1 d . . . C4B C 0.2544(7) 0.6373(11) 1.1240(12) 0.041(11) Uiso 1 1 d . . . N4C N 0.2672(5) 0.6586(8) 1.0971(8) 0.037(8) Uiso 1 1 d . . . H4CA H 0.2741 0.6798 1.1063 0.044 Uiso 1 1 calc R . . C4C C 0.2716(6) 0.6513(10) 1.0529(11) 0.018(10) Uiso 1 1 d . . . O4 O 0.2850(4) 0.6680(7) 1.0329(7) 0.046(8) Uani 1 1 d . . . N4D N 0.2556(5) 0.6484(9) 1.1626(10) 0.049(9) Uiso 1 1 d . . . C4D C 0.2457(8) 0.6209(13) 1.1934(13) 0.088(16) Uiso 1 1 d . . . H4DA H 0.2459 0.5936 1.1839 0.105 Uiso 1 1 calc R . . H4DB H 0.2555 0.6226 1.2177 0.105 Uiso 1 1 calc R . . C4E C 0.2237(11) 0.6327(17) 1.1990(18) 0.18(3) Uiso 1 1 d . . . H4EA H 0.2162 0.6178 1.2204 0.276 Uiso 1 1 calc R . . H4EB H 0.2141 0.6289 1.1751 0.276 Uiso 1 1 calc R . . H4EC H 0.2239 0.6604 1.2059 0.276 Uiso 1 1 calc R . . C4F C 0.2662(6) 0.6854(10) 1.1777(11) 0.056(13) Uiso 1 1 d . . . H4FA H 0.2578 0.6929 1.2022 0.068 Uiso 1 1 calc R . . H4FB H 0.2637 0.7064 1.1584 0.068 Uiso 1 1 calc R . . C4G C 0.2934(7) 0.6803(11) 1.1853(12) 0.083(15) Uiso 1 1 d . . . H4GA H 0.3005 0.7051 1.1939 0.124 Uiso 1 1 calc R . . H4GB H 0.3016 0.6718 1.1613 0.124 Uiso 1 1 calc R . . H4GC H 0.2959 0.6607 1.2058 0.124 Uiso 1 1 calc R . . S5 S 0.28395(17) 0.5568(3) 0.9978(3) 0.041(3) Uani 1 1 d . . . N5A N 0.2683(5) 0.6187(7) 0.9610(8) 0.025(8) Uiso 1 1 d . . . C5A C 0.2911(6) 0.5953(10) 0.9649(10) 0.033(11) Uiso 1 1 d . . . N5B N 0.3127(5) 0.6040(8) 0.9483(8) 0.031(8) Uiso 1 1 d . . . C5B C 0.3119(7) 0.6365(11) 0.9255(11) 0.036(11) Uiso 1 1 d . . . N5C N 0.2916(5) 0.6592(8) 0.9202(8) 0.046(9) Uiso 1 1 d . . . H5CA H 0.2931 0.6807 0.9065 0.055 Uiso 1 1 calc R . . C5C C 0.2682(8) 0.6498(12) 0.9356(11) 0.037(12) Uiso 1 1 d . . . O5 O 0.2501(4) 0.6694(6) 0.9310(6) 0.036(7) Uani 1 1 d . . . N5D N 0.3329(5) 0.6462(8) 0.9068(8) 0.041(9) Uiso 1 1 d . . . C5D C 0.3550(7) 0.6208(11) 0.9120(11) 0.063(13) Uiso 1 1 d . . . H5DA H 0.3545 0.6089 0.9383 0.076 Uiso 1 1 calc R . . H5DB H 0.3700 0.6370 0.9102 0.076 Uiso 1 1 calc R . . C5E C 0.3563(7) 0.5886(11) 0.8813(12) 0.092(16) Uiso 1 1 d . . . H5EA H 0.3706 0.5721 0.8864 0.137 Uiso 1 1 calc R . . H5EB H 0.3578 0.6002 0.8553 0.137 Uiso 1 1 calc R . . H5EC H 0.3413 0.5728 0.8825 0.137 Uiso 1 1 calc R . . C5F C 0.3354(7) 0.6799(11) 0.8813(12) 0.064(13) Uiso 1 1 d . . . H5F1 H 0.3528 0.6880 0.8811 0.077 Uiso 1 1 calc R . . H5F2 H 0.3256 0.7016 0.8925 0.077 Uiso 1 1 calc R . . C5G C 0.3273(7) 0.6734(11) 0.8402(12) 0.088(15) Uiso 1 1 d . . . H5GA H 0.3290 0.6976 0.8254 0.132 Uiso 1 1 calc R . . H5GB H 0.3100 0.6651 0.8400 0.132 Uiso 1 1 calc R . . H5GC H 0.3375 0.6531 0.8282 0.132 Uiso 1 1 calc R . . S6 S 0.22771(18) 0.5569(3) 0.9449(3) 0.045(3) Uani 1 1 d . . . N6A N 0.2159(4) 0.6180(7) 0.9840(8) 0.021(8) Uiso 1 1 d . . . C6A C 0.2083(6) 0.5949(9) 0.9517(10) 0.025(10) Uiso 1 1 d . . . N6B N 0.1880(5) 0.6044(9) 0.9302(9) 0.050(10) Uiso 1 1 d . . . C6B C 0.1736(7) 0.6375(11) 0.9377(12) 0.046(12) Uiso 1 1 d . . . N6C N 0.1831(5) 0.6577(8) 0.9725(8) 0.035(8) Uiso 1 1 d . . . H6CA H 0.1756 0.6797 0.9776 0.042 Uiso 1 1 calc R . . C6C C 0.2019(7) 0.6489(12) 0.9994(13) 0.037(13) Uiso 1 1 d . . . O6 O 0.2078(4) 0.6685(7) 1.0261(8) 0.056(8) Uani 1 1 d . . . N6D N 0.1546(6) 0.6474(9) 0.9197(10) 0.052(10) Uiso 1 1 d . . . C6D C 0.1475(6) 0.6255(10) 0.8821(11) 0.052(12) Uiso 1 1 d . . . H6D1 H 0.1394 0.6436 0.8637 0.062 Uiso 1 1 calc R . . H6D2 H 0.1626 0.6153 0.8693 0.062 Uiso 1 1 calc R . . C6E C 0.1307(7) 0.5927(12) 0.8911(13) 0.097(16) Uiso 1 1 d . . . H6EA H 0.1253 0.5804 0.8668 0.146 Uiso 1 1 calc R . . H6EB H 0.1163 0.6026 0.9053 0.146 Uiso 1 1 calc R . . H6EC H 0.1393 0.5736 0.9073 0.146 Uiso 1 1 calc R . . C6F C 0.1378(8) 0.6820(12) 0.9282(13) 0.088(16) Uiso 1 1 d . . . H6FA H 0.1478 0.7052 0.9347 0.106 Uiso 1 1 calc R . . H6FB H 0.1277 0.6881 0.9050 0.106 Uiso 1 1 calc R . . C6G C 0.1222(10) 0.6719(16) 0.9608(17) 0.18(3) Uiso 1 1 d . . . H6GA H 0.1119 0.6942 0.9677 0.264 Uiso 1 1 calc R . . H6GB H 0.1324 0.6646 0.9833 0.264 Uiso 1 1 calc R . . H6GC H 0.1117 0.6499 0.9536 0.264 Uiso 1 1 calc R . . S7 S 0.32002(19) 0.8901(3) 1.1369(3) 0.049(3) Uani 1 1 d . . . N7A N 0.3173(5) 0.8522(8) 1.0727(9) 0.043(9) Uiso 1 1 d . . . C7A C 0.3152(6) 0.8896(12) 1.0866(11) 0.044(12) Uiso 1 1 d . . . N7B N 0.3129(5) 0.9223(8) 1.0640(10) 0.047(9) Uiso 1 1 d . . . C7B C 0.3090(6) 0.9143(11) 1.0252(12) 0.042(11) Uiso 1 1 d . . . N7C N 0.3093(5) 0.8760(8) 1.0097(9) 0.044(9) Uiso 1 1 d . . . H7CA H 0.3059 0.8723 0.9849 0.053 Uiso 1 1 calc R . . C7C C 0.3151(7) 0.8428(13) 1.0343(13) 0.045(12) Uiso 1 1 d . . . O7 O 0.3170(4) 0.8105(7) 1.0185(7) 0.055(8) Uani 1 1 d . . . N7D N 0.3049(5) 0.9439(8) 0.9979(9) 0.042(9) Uiso 1 1 d . . . C7D C 0.3035(7) 0.9832(11) 1.0142(12) 0.077(15) Uiso 1 1 d . . . H7DA H 0.3007 0.9817 1.0428 0.092 Uiso 1 1 calc R . . H7DB H 0.2894 0.9973 1.0025 0.092 Uiso 1 1 calc R . . C7E C 0.3285(7) 1.0061(12) 1.0055(12) 0.090(16) Uiso 1 1 d . . . H7EA H 0.3277 1.0320 1.0175 0.134 Uiso 1 1 calc R . . H7EB H 0.3306 1.0088 0.9772 0.134 Uiso 1 1 calc R . . H7EC H 0.3424 0.9916 1.0165 0.134 Uiso 1 1 calc R . . C7F C 0.3011(6) 0.9385(10) 0.9533(11) 0.052(12) Uiso 1 1 d . . . H7FA H 0.2943 0.9627 0.9419 0.062 Uiso 1 1 calc R . . H7FB H 0.2891 0.9173 0.9487 0.062 Uiso 1 1 calc R . . C7G C 0.3259(7) 0.9284(11) 0.9333(12) 0.081(15) Uiso 1 1 d . . . H7GA H 0.3232 0.9243 0.9053 0.121 Uiso 1 1 calc R . . H7GB H 0.3327 0.9046 0.9449 0.121 Uiso 1 1 calc R . . H7GC H 0.3375 0.9499 0.9371 0.121 Uiso 1 1 calc R . . S8 S 0.31491(17) 0.7989(3) 1.1863(3) 0.050(3) Uani 1 1 d . . . N8A N 0.2839(5) 0.8187(7) 1.1345(8) 0.029(8) Uiso 1 1 d . . . C8A C 0.2829(7) 0.8022(11) 1.1717(12) 0.051(12) Uiso 1 1 d . . . N8B N 0.2631(5) 0.7893(7) 1.1901(8) 0.033(8) Uiso 1 1 d . . . C8B C 0.2420(7) 0.7953(9) 1.1730(11) 0.028(10) Uiso 1 1 d . . . N8C N 0.2420(5) 0.8103(8) 1.1341(9) 0.050(9) Uiso 1 1 d . . . H8CA H 0.2279 0.8093 1.1216 0.060 Uiso 1 1 calc R . . C8C C 0.2630(6) 0.8273(10) 1.1125(12) 0.023(11) Uiso 1 1 d . . . O8 O 0.2593(4) 0.8421(6) 1.0815(7) 0.031(7) Uani 1 1 d . . . N8D N 0.2209(5) 0.7862(8) 1.1886(9) 0.044(9) Uiso 1 1 d . . . C8D C 0.2219(7) 0.7667(11) 1.2284(11) 0.062(13) Uiso 1 1 d . . . H8DA H 0.2387 0.7569 1.2336 0.074 Uiso 1 1 calc R . . H8DB H 0.2103 0.7446 1.2295 0.074 Uiso 1 1 calc R . . C8E C 0.2146(6) 0.7987(10) 1.2598(11) 0.060(13) Uiso 1 1 d . . . H8EA H 0.2152 0.7873 1.2860 0.090 Uiso 1 1 calc R . . H8EB H 0.1979 0.8080 1.2546 0.090 Uiso 1 1 calc R . . H8EC H 0.2261 0.8206 1.2583 0.090 Uiso 1 1 calc R . . C8F C 0.1958(6) 0.7924(10) 1.1723(11) 0.052(12) Uiso 1 1 d . . . H8FA H 0.1839 0.7772 1.1881 0.062 Uiso 1 1 calc R . . H8FB H 0.1954 0.7818 1.1454 0.062 Uiso 1 1 calc R . . C8G C 0.1872(7) 0.8339(10) 1.1711(11) 0.072(14) Uiso 1 1 d . . . H8GA H 0.1707 0.8350 1.1593 0.108 Uiso 1 1 calc R . . H8GB H 0.1986 0.8494 1.1554 0.108 Uiso 1 1 calc R . . H8GC H 0.1865 0.8444 1.1977 0.108 Uiso 1 1 calc R . . S9 S 0.36218(18) 0.8119(3) 1.1150(3) 0.053(3) Uani 1 1 d . . . N9A N 0.3237(5) 0.7717(8) 1.1025(8) 0.035(8) Uiso 1 1 d . . . C9A C 0.3490(6) 0.7693(10) 1.0968(10) 0.037(11) Uiso 1 1 d . . . N9B N 0.3626(5) 0.7383(9) 1.0804(9) 0.049(9) Uiso 1 1 d . . . C9B C 0.3469(7) 0.7080(10) 1.0684(10) 0.034(11) Uiso 1 1 d . . . N9C N 0.3220(5) 0.7093(8) 1.0719(8) 0.031(8) Uiso 1 1 d . . . H9CA H 0.3138 0.6899 1.0617 0.037 Uiso 1 1 calc R . . C9C C 0.3085(9) 0.7381(13) 1.0899(12) 0.055(14) Uiso 1 1 d . . . O9 O 0.2866(4) 0.7383(6) 1.0966(6) 0.041(7) Uani 1 1 d . . . N9D N 0.3593(5) 0.6759(9) 1.0526(9) 0.051(10) Uiso 1 1 d . . . C9D C 0.3871(7) 0.6739(12) 1.0473(13) 0.086(15) Uiso 1 1 d . . . H9DA H 0.3950 0.6932 1.0648 0.103 Uiso 1 1 calc R . . H9DB H 0.3929 0.6477 1.0553 0.103 Uiso 1 1 calc R . . C9E C 0.3944(7) 0.6807(12) 1.0104(13) 0.090(16) Uiso 1 1 d . . . H9EA H 0.4124 0.6780 1.0087 0.135 Uiso 1 1 calc R . . H9EB H 0.3897 0.7071 1.0028 0.135 Uiso 1 1 calc R . . H9EC H 0.3866 0.6619 0.9929 0.135 Uiso 1 1 calc R . . C9F C 0.3451(6) 0.6420(9) 1.0379(10) 0.033(10) Uiso 1 1 d . . . H9FA H 0.3553 0.6270 1.0192 0.039 Uiso 1 1 calc R . . H9FB H 0.3302 0.6512 1.0239 0.039 Uiso 1 1 calc R . . C9G C 0.3371(7) 0.6144(11) 1.0734(11) 0.078(15) Uiso 1 1 d . . . H9GA H 0.3274 0.5925 1.0634 0.117 Uiso 1 1 calc R . . H9GB H 0.3272 0.6293 1.0921 0.117 Uiso 1 1 calc R . . H9GC H 0.3519 0.6044 1.0865 0.117 Uiso 1 1 calc R . . S10 S 0.04314(19) 0.1983(3) 0.8952(3) 0.059(3) Uani 1 1 d . . . N10A N 0.0247(5) 0.1315(9) 0.8836(9) 0.049(10) Uiso 1 1 d . . . C10A C 0.0186(7) 0.1669(12) 0.8986(12) 0.055(13) Uiso 1 1 d . . . N10B N -0.0041(5) 0.1787(8) 0.9157(9) 0.049(9) Uiso 1 1 d . . . C10B C -0.0213(7) 0.1484(11) 0.9166(11) 0.039(11) Uiso 1 1 d . . . N10C N -0.0173(6) 0.1134(9) 0.9016(9) 0.057(10) Uiso 1 1 d . . . H10B H -0.0289 0.0955 0.9016 0.068 Uiso 1 1 calc R . . C10C C 0.0067(10) 0.1057(15) 0.8855(14) 0.077(16) Uiso 1 1 d . . . O10 O 0.0086(4) 0.0713(7) 0.8722(8) 0.062(8) Uani 1 1 d . . . N10D N -0.0440(6) 0.1579(9) 0.9328(9) 0.061(10) Uiso 1 1 d . . . C10D C -0.0657(7) 0.1314(10) 0.9300(11) 0.058(13) Uiso 1 1 d . . . H10D H -0.0645 0.1153 0.9062 0.070 Uiso 1 1 calc R . . H10E H -0.0811 0.1468 0.9288 0.070 Uiso 1 1 calc R . . C10E C -0.0656(7) 0.1044(11) 0.9681(12) 0.087(16) Uiso 1 1 d . . . H10F H -0.0795 0.0863 0.9669 0.131 Uiso 1 1 calc R . . H10G H -0.0671 0.1207 0.9915 0.131 Uiso 1 1 calc R . . H10H H -0.0502 0.0897 0.9692 0.131 Uiso 1 1 calc R . . C10F C -0.0468(8) 0.1950(12) 0.9582(13) 0.088(16) Uiso 1 1 d . . . H10I H -0.0579 0.1901 0.9806 0.106 Uiso 1 1 calc R . . H10J H -0.0306 0.2035 0.9683 0.106 Uiso 1 1 calc R . . C10G C -0.0574(8) 0.2253(12) 0.9318(13) 0.097(17) Uiso 1 1 d . . . H10K H -0.0599 0.2494 0.9465 0.145 Uiso 1 1 calc R . . H10L H -0.0733 0.2162 0.9216 0.145 Uiso 1 1 calc R . . H10M H -0.0461 0.2300 0.9100 0.145 Uiso 1 1 calc R . . S11 S 0.09216(17) 0.1688(3) 0.8388(3) 0.051(3) Uani 1 1 d . . . N11A N 0.0492(5) 0.1588(7) 0.8123(8) 0.037(9) Uiso 1 1 d . . . C11A C 0.0714(7) 0.1710(10) 0.8020(12) 0.046(12) Uiso 1 1 d . . . N11B N 0.0761(5) 0.1841(7) 0.7650(9) 0.038(9) Uiso 1 1 d . . . C11B C 0.0566(8) 0.1827(12) 0.7371(14) 0.067(14) Uiso 1 1 d . . . N11C N 0.0340(5) 0.1675(7) 0.7493(8) 0.028(8) Uiso 1 1 d . . . H11B H 0.0225 0.1649 0.7316 0.033 Uiso 1 1 calc R . . C11C C 0.0282(9) 0.1558(11) 0.7888(13) 0.046(13) Uiso 1 1 d . . . O11 O 0.0078(4) 0.1448(7) 0.7970(7) 0.051(8) Uani 1 1 d . . . N11D N 0.0588(5) 0.1962(8) 0.6994(10) 0.051(10) Uiso 1 1 d . . . C11D C 0.0838(7) 0.2066(10) 0.6862(12) 0.064(13) Uiso 1 1 d . . . H11C H 0.0878 0.1920 0.6621 0.077 Uiso 1 1 calc R . . H11D H 0.0959 0.1991 0.7065 0.077 Uiso 1 1 calc R . . C11E C 0.0861(8) 0.2499(12) 0.6782(13) 0.105(17) Uiso 1 1 d . . . H11E H 0.1029 0.2557 0.6694 0.157 Uiso 1 1 calc R . . H11F H 0.0826 0.2644 0.7022 0.157 Uiso 1 1 calc R . . H11G H 0.0743 0.2574 0.6579 0.157 Uiso 1 1 calc R . . C11F C 0.0379(6) 0.1970(10) 0.6722(11) 0.046(12) Uiso 1 1 d . . . H11H H 0.0289 0.1721 0.6741 0.056 Uiso 1 1 calc R . . H11I H 0.0443 0.1993 0.6451 0.056 Uiso 1 1 calc R . . C11G C 0.0200(7) 0.2309(11) 0.6801(12) 0.084(15) Uiso 1 1 d . . . H11J H 0.0071 0.2310 0.6601 0.126 Uiso 1 1 calc R . . H11K H 0.0290 0.2556 0.6793 0.126 Uiso 1 1 calc R . . H11L H 0.0125 0.2275 0.7059 0.126 Uiso 1 1 calc R . . S12 S 0.07321(18) 0.1146(3) 0.9224(3) 0.054(3) Uani 1 1 d . . . N12A N 0.0676(5) 0.0875(9) 0.8557(11) 0.055(10) Uiso 1 1 d . . . C12A C 0.0747(6) 0.0759(11) 0.8901(12) 0.042(12) Uiso 1 1 d . . . N12B N 0.0822(5) 0.0409(10) 0.8996(10) 0.064(10) Uiso 1 1 d . . . C12B C 0.0840(8) 0.0150(13) 0.8668(15) 0.072(14) Uiso 1 1 d . . . N12C N 0.0758(5) 0.0243(9) 0.8304(9) 0.049(9) Uiso 1 1 d . . . H12B H 0.0755 0.0070 0.8115 0.059 Uiso 1 1 calc R . . C12C C 0.0677(7) 0.0622(12) 0.8246(14) 0.043(13) Uiso 1 1 d . . . O12 O 0.0641(4) 0.0708(7) 0.7883(7) 0.048(7) Uani 1 1 d . . . N12D N 0.0926(7) -0.0226(12) 0.8763(12) 0.102(13) Uiso 1 1 d . . . C12D C 0.1068(10) -0.0317(16) 0.9180(17) 0.15(2) Uiso 1 1 d . . . H12C H 0.1202 -0.0512 0.9156 0.185 Uiso 1 1 calc R . . H12D H 0.1128 -0.0080 0.9315 0.185 Uiso 1 1 calc R . . C12E C 0.0851(11) -0.0468(17) 0.9340(18) 0.18(3) Uiso 1 1 d . . . H12E H 0.0882 -0.0561 0.9606 0.273 Uiso 1 1 calc R . . H12F H 0.0793 -0.0685 0.9178 0.273 Uiso 1 1 calc R . . H12G H 0.0725 -0.0264 0.9346 0.273 Uiso 1 1 calc R . . C12F C 0.0982(8) -0.0524(13) 0.8447(14) 0.093(16) Uiso 1 1 d . . . H12H H 0.0841 -0.0525 0.8264 0.112 Uiso 1 1 calc R . . H12I H 0.0986 -0.0783 0.8574 0.112 Uiso 1 1 calc R . . C12G C 0.1221(11) -0.0488(18) 0.8198(19) 0.22(3) Uiso 1 1 d . . . H12J H 0.1218 -0.0681 0.7988 0.328 Uiso 1 1 calc R . . H12K H 0.1365 -0.0532 0.8364 0.328 Uiso 1 1 calc R . . H12L H 0.1230 -0.0226 0.8084 0.328 Uiso 1 1 calc R . . S13 S 0.10929(17) 0.8078(3) 0.9919(3) 0.052(3) Uani 1 1 d . . . N13A N 0.1536(6) 0.8266(8) 0.9753(9) 0.046(9) Uiso 1 1 d . . . C13A C 0.1326(8) 0.8111(11) 0.9592(13) 0.060(13) Uiso 1 1 d . . . N13B N 0.1295(5) 0.8044(8) 0.9194(10) 0.046(9) Uiso 1 1 d . . . C13B C 0.1509(7) 0.8097(10) 0.8975(12) 0.045(12) Uiso 1 1 d . . . N13C N 0.1732(6) 0.8202(8) 0.9142(10) 0.056(10) Uiso 1 1 d . . . H13A H 0.1867 0.8204 0.9002 0.067 Uiso 1 1 calc R . . C13C C 0.1740(9) 0.8307(12) 0.9550(14) 0.054(15) Uiso 1 1 d . . . O13 O 0.1929(5) 0.8451(8) 0.9649(7) 0.066(9) Uani 1 1 d . . . N13D N 0.1504(6) 0.8040(8) 0.8577(10) 0.056(10) Uiso 1 1 d . . . C13D C 0.1263(8) 0.7937(12) 0.8372(14) 0.101(17) Uiso 1 1 d . . . H13B H 0.1129 0.8090 0.8496 0.121 Uiso 1 1 calc R . . H13C H 0.1275 0.8024 0.8097 0.121 Uiso 1 1 calc R . . C13E C 0.1184(8) 0.7512(12) 0.8370(13) 0.107(17) Uiso 1 1 d . . . H13C H 0.1020 0.7489 0.8252 0.161 Uiso 1 1 calc R . . H13D H 0.1179 0.7414 0.8639 0.161 Uiso 1 1 calc R . . H13E H 0.1302 0.7359 0.8219 0.161 Uiso 1 1 calc R . . C13F C 0.1717(7) 0.8050(11) 0.8309(12) 0.068(14) Uiso 1 1 d . . . H13F H 0.1686 0.7878 0.8082 0.082 Uiso 1 1 calc R . . H13G H 0.1866 0.7954 0.8446 0.082 Uiso 1 1 calc R . . C13G C 0.1764(9) 0.8499(14) 0.8157(16) 0.15(2) Uiso 1 1 d . . . H13H H 0.1904 0.8504 0.7977 0.232 Uiso 1 1 calc R . . H13I H 0.1798 0.8667 0.8381 0.232 Uiso 1 1 calc R . . H13J H 0.1616 0.8593 0.8022 0.232 Uiso 1 1 calc R . . S14 S 0.12654(18) 0.8174(3) 1.0923(3) 0.050(3) Uani 1 1 d . . . N14A N 0.1522(5) 0.7728(9) 1.0438(10) 0.052(10) Uiso 1 1 d . . . C14A C 0.1415(7) 0.7747(11) 1.0802(13) 0.055(13) Uiso 1 1 d . . . N14B N 0.1414(5) 0.7426(9) 1.1078(9) 0.047(9) Uiso 1 1 d . . . C14B C 0.1550(7) 0.7100(12) 1.0948(12) 0.050(12) Uiso 1 1 d . . . N14C N 0.1665(5) 0.7116(8) 1.0573(9) 0.045(9) Uiso 1 1 d . . . H14B H 0.1756 0.6913 1.0516 0.054 Uiso 1 1 calc R . . C14C C 0.1655(7) 0.7424(11) 1.0258(13) 0.035(12) Uiso 1 1 d . . . O14 O 0.1721(5) 0.7398(7) 0.9945(7) 0.066(9) Uani 1 1 d . . . N14D N 0.1568(5) 0.6767(8) 1.1181(9) 0.038(9) Uiso 1 1 d . . . C14D C 0.1423(7) 0.6733(12) 1.1545(12) 0.077(14) Uiso 1 1 d . . . H14C H 0.1389 0.6455 1.1603 0.092 Uiso 1 1 calc R . . H14D H 0.1264 0.6870 1.1517 0.092 Uiso 1 1 calc R . . C14E C 0.1584(8) 0.6927(13) 1.1899(14) 0.124(19) Uiso 1 1 d . . . H14E H 0.1487 0.6926 1.2140 0.186 Uiso 1 1 calc R . . H14F H 0.1626 0.7196 1.1830 0.186 Uiso 1 1 calc R . . H14G H 0.1735 0.6777 1.1938 0.186 Uiso 1 1 calc R . . C14F C 0.1712(6) 0.6444(10) 1.1059(11) 0.054(12) Uiso 1 1 d . . . H14H H 0.1766 0.6300 1.1294 0.065 Uiso 1 1 calc R . . H14I H 0.1861 0.6543 1.0926 0.065 Uiso 1 1 calc R . . C14G C 0.1586(7) 0.6167(11) 1.0793(12) 0.084(15) Uiso 1 1 d . . . H14J H 0.1697 0.5951 1.0730 0.126 Uiso 1 1 calc R . . H14K H 0.1539 0.6302 1.0551 0.126 Uiso 1 1 calc R . . H14L H 0.1437 0.6066 1.0920 0.126 Uiso 1 1 calc R . . S15 S 0.13659(18) 0.8949(3) 1.0262(3) 0.058(4) Uani 1 1 d . . . N15A N 0.1716(5) 0.8537(8) 1.0517(8) 0.040(9) Uiso 1 1 d . . . C15A C 0.1662(7) 0.8920(13) 1.0461(12) 0.060(13) Uiso 1 1 d . . . N15B N 0.1801(6) 0.9240(9) 1.0521(9) 0.056(10) Uiso 1 1 d . . . C15B C 0.2040(7) 0.9145(11) 1.0652(11) 0.043(12) Uiso 1 1 d . . . N15C N 0.2106(5) 0.8754(8) 1.0717(8) 0.039(9) Uiso 1 1 d . . . H15B H 0.2257 0.8705 1.0790 0.047 Uiso 1 1 calc R . . C15C C 0.1943(7) 0.8434(12) 1.0671(10) 0.028(11) Uiso 1 1 d . . . O15 O 0.2015(4) 0.8110(7) 1.0739(7) 0.044(8) Uani 1 1 d . . . N15D N 0.2214(6) 0.9440(9) 1.0746(9) 0.059(10) Uiso 1 1 d . . . C15D C 0.2139(8) 0.9837(11) 1.0648(12) 0.081(15) Uiso 1 1 d . . . H15C H 0.1993 0.9825 1.0476 0.097 Uiso 1 1 calc R . . H15D H 0.2273 0.9963 1.0499 0.097 Uiso 1 1 calc R . . C15E C 0.2077(8) 1.0093(13) 1.1006(14) 0.123(19) Uiso 1 1 d . . . H15E H 0.2025 1.0351 1.0918 0.185 Uiso 1 1 calc R . . H15F H 0.2223 1.0118 1.1172 0.185 Uiso 1 1 calc R . . H15G H 0.1944 0.9971 1.1156 0.185 Uiso 1 1 calc R . . C15F C 0.2466(7) 0.9352(11) 1.0852(11) 0.061(13) Uiso 1 1 d . . . H15H H 0.2575 0.9571 1.0779 0.073 Uiso 1 1 calc R . . H15I H 0.2522 0.9115 1.0713 0.073 Uiso 1 1 calc R . . C15G C 0.2475(10) 0.9282(16) 1.1321(16) 0.17(2) Uiso 1 1 d . . . H15J H 0.2642 0.9213 1.1399 0.250 Uiso 1 1 calc R . . H15K H 0.2362 0.9070 1.1390 0.250 Uiso 1 1 calc R . . H15L H 0.2424 0.9520 1.1455 0.250 Uiso 1 1 calc R . . S16 S 0.0134(2) -0.6543(4) 1.4187(4) 0.082(4) Uani 1 1 d . . . N16A N 0.0158(5) -0.6397(9) 1.3475(11) 0.053(10) Uiso 1 1 d . . . C16A C 0.0014(9) -0.6596(12) 1.3722(14) 0.074(14) Uiso 1 1 d . . . N16B N -0.0199(7) -0.6805(10) 1.3633(12) 0.085(12) Uiso 1 1 d . . . C16B C -0.0277(9) -0.6784(13) 1.3248(15) 0.074(15) Uiso 1 1 d . . . N16C N -0.0120(5) -0.6570(8) 1.2979(9) 0.048(9) Uiso 1 1 d . . . H16B H -0.0165 -0.6561 1.2733 0.057 Uiso 1 1 calc R . . C16C C 0.0108(8) -0.6369(12) 1.3087(15) 0.051(13) Uiso 1 1 d . . . O16 O 0.0234(5) -0.6258(7) 1.2802(7) 0.064(9) Uani 1 1 d . . . N16D N -0.0464(9) -0.6985(12) 1.3092(14) 0.124(16) Uiso 1 1 d D . . C16D C -0.0671(10) -0.7069(18) 1.337(2) 0.30(4) Uiso 1 1 d D . . H16A H -0.0826 -0.7079 1.3215 0.357 Uiso 1 1 calc R . . H16C H -0.0684 -0.6853 1.3555 0.357 Uiso 1 1 calc R . . C16E C -0.0640(12) -0.7457(18) 1.3593(18) 0.28(4) Uiso 1 1 d D . . H16D H -0.0774 -0.7483 1.3783 0.426 Uiso 1 1 calc R . . H16E H -0.0482 -0.7457 1.3729 0.426 Uiso 1 1 calc R . . H16F H -0.0646 -0.7676 1.3409 0.426 Uiso 1 1 calc R . . C16F C -0.0549(7) -0.6977(12) 1.2684(13) 0.081(15) Uiso 1 1 d . . . H16H H -0.0522 -0.6714 1.2573 0.097 Uiso 1 1 calc R . . H16I H -0.0728 -0.7032 1.2676 0.097 Uiso 1 1 calc R . . C16G C -0.0413(7) -0.7274(12) 1.2445(13) 0.102(17) Uiso 1 1 d . . . H16J H -0.0459 -0.7246 1.2169 0.153 Uiso 1 1 calc R . . H16K H -0.0456 -0.7536 1.2535 0.153 Uiso 1 1 calc R . . H16L H -0.0236 -0.7234 1.2473 0.153 Uiso 1 1 calc R . . S17 S 0.0600(2) -0.5859(3) 1.4338(3) 0.067(4) Uani 1 1 d . . . N17A N 0.0221(5) -0.5686(8) 1.3957(9) 0.051(10) Uiso 1 1 d . . . C17A C 0.0364(6) -0.5531(10) 1.4236(11) 0.031(11) Uiso 1 1 d . . . N17B N 0.0335(6) -0.5185(9) 1.4441(9) 0.055(10) Uiso 1 1 d . . . C17B C 0.0157(7) -0.4979(12) 1.4291(13) 0.055(13) Uiso 1 1 d . . . N17C N 0.0003(5) -0.5098(8) 1.3999(9) 0.049(9) Uiso 1 1 d . . . H17B H -0.0106 -0.4927 1.3922 0.059 Uiso 1 1 calc R . . C17C C -0.0003(7) -0.5481(11) 1.3794(12) 0.030(12) Uiso 1 1 d . . . O17 O -0.0141(5) -0.5589(8) 1.3551(8) 0.068(9) Uani 1 1 d . . . N17D N 0.0088(6) -0.4636(10) 1.4439(10) 0.074(11) Uiso 1 1 d D . . C17D C 0.0200(9) -0.4507(14) 1.4816(10) 0.14(2) Uiso 1 1 d D . . H17A H 0.0269 -0.4736 1.4953 0.167 Uiso 1 1 calc R . . H17C H 0.0070 -0.4395 1.4984 0.167 Uiso 1 1 calc R . . C17E C 0.0407(9) -0.4199(16) 1.4762(16) 0.22(3) Uiso 1 1 d D . . H17D H 0.0492 -0.4160 1.5011 0.337 Uiso 1 1 calc R . . H17E H 0.0334 -0.3953 1.4676 0.337 Uiso 1 1 calc R . . H17F H 0.0524 -0.4291 1.4565 0.337 Uiso 1 1 calc R . . C17F C -0.0126(7) -0.4376(11) 1.4344(12) 0.071(14) Uiso 1 1 d . . . H17A H -0.0090 -0.4113 1.4448 0.085 Uiso 1 1 calc R . . H17C H -0.0139 -0.4354 1.4057 0.085 Uiso 1 1 calc R . . C17G C -0.0368(8) -0.4502(13) 1.4498(14) 0.116(19) Uiso 1 1 d . . . H17H H -0.0497 -0.4328 1.4401 0.174 Uiso 1 1 calc R . . H17I H -0.0365 -0.4494 1.4784 0.174 Uiso 1 1 calc R . . H17J H -0.0402 -0.4768 1.4411 0.174 Uiso 1 1 calc R . . S18 S 0.07027(19) -0.6628(3) 1.3676(3) 0.065(4) Uani 1 1 d . . . N18A N 0.0631(5) -0.5940(10) 1.3429(9) 0.055(10) Uiso 1 1 d . . . C18A C 0.0787(7) -0.6251(11) 1.3361(12) 0.050(12) Uiso 1 1 d . . . N18B N 0.0971(6) -0.6249(9) 1.3112(10) 0.060(10) Uiso 1 1 d . . . C18B C 0.1004(7) -0.5945(12) 1.2881(12) 0.051(12) Uiso 1 1 d . . . N18C N 0.0851(5) -0.5615(8) 1.2916(8) 0.039(9) Uiso 1 1 d . . . H18B H 0.0867 -0.5414 1.2761 0.047 Uiso 1 1 calc R . . C18C C 0.0675(7) -0.5624(13) 1.3204(13) 0.046(13) Uiso 1 1 d . . . O18 O 0.0544(4) -0.5307(7) 1.3268(7) 0.058(8) Uani 1 1 d . . . N18D N 0.1178(7) -0.5903(10) 1.2621(12) 0.086(12) Uiso 1 1 d . . . C18D C 0.1348(7) -0.6268(10) 1.2515(12) 0.060(13) Uiso 1 1 d . . . H18D H 0.1513 -0.6171 1.2442 0.072 Uiso 1 1 calc R . . H18E H 0.1368 -0.6430 1.2752 0.072 Uiso 1 1 calc R . . C18E C 0.1255(7) -0.6518(10) 1.2195(11) 0.068(14) Uiso 1 1 d . . . H18F H 0.1361 -0.6746 1.2168 0.102 Uiso 1 1 calc R . . H18G H 0.1255 -0.6370 1.1951 0.102 Uiso 1 1 calc R . . H18H H 0.1087 -0.6602 1.2256 0.102 Uiso 1 1 calc R . . C18F C 0.1178(9) -0.5612(13) 1.2289(14) 0.109(18) Uiso 1 1 d . . . H18I H 0.1229 -0.5730 1.2038 0.131 Uiso 1 1 calc R . . H18J H 0.1016 -0.5483 1.2258 0.131 Uiso 1 1 calc R . . C18G C 0.1370(12) -0.5342(17) 1.2451(19) 0.21(3) Uiso 1 1 d . . . H18K H 0.1373 -0.5101 1.2298 0.321 Uiso 1 1 calc R . . H18L H 0.1532 -0.5468 1.2438 0.321 Uiso 1 1 calc R . . H18M H 0.1331 -0.5281 1.2724 0.321 Uiso 1 1 calc R . . S19 S -0.11985(17) -0.4341(3) 1.3310(3) 0.054(3) Uani 1 1 d . . . N19A N -0.0764(6) -0.4545(8) 1.3398(9) 0.055(10) Uiso 1 1 d . . . C19A C -0.1000(6) -0.4713(10) 1.3472(10) 0.036(11) Uiso 1 1 d . . . N19B N -0.1049(5) -0.5065(9) 1.3635(9) 0.047(9) Uiso 1 1 d . . . C19B C -0.0852(8) -0.5275(13) 1.3692(12) 0.061(13) Uiso 1 1 d . . . N19C N -0.0611(6) -0.5164(9) 1.3609(9) 0.063(10) Uiso 1 1 d . . . H19B H -0.0492 -0.5335 1.3634 0.075 Uiso 1 1 calc R . . C19C C -0.0552(8) -0.4771(11) 1.3482(11) 0.043(12) Uiso 1 1 d . . . O19 O -0.0330(4) -0.4679(7) 1.3457(8) 0.059(8) Uani 1 1 d . . . N19D N -0.0885(6) -0.5626(10) 1.3807(10) 0.069(11) Uiso 1 1 d . . . C19D C -0.1137(7) -0.5795(12) 1.3883(12) 0.076(14) Uiso 1 1 d . . . H19C H -0.1130 -0.6082 1.3863 0.091 Uiso 1 1 calc R . . H19D H -0.1254 -0.5698 1.3685 0.091 Uiso 1 1 calc R . . C19E C -0.1225(10) -0.5677(16) 1.4298(17) 0.17(3) Uiso 1 1 d . . . H19E H -0.1393 -0.5770 1.4339 0.262 Uiso 1 1 calc R . . H19F H -0.1221 -0.5393 1.4323 0.262 Uiso 1 1 calc R . . H19G H -0.1116 -0.5792 1.4494 0.262 Uiso 1 1 calc R . . C19F C -0.0693(9) -0.5957(15) 1.3805(16) 0.13(2) Uiso 1 1 d . . . H19H H -0.0562 -0.5920 1.3608 0.153 Uiso 1 1 calc R . . H19I H -0.0768 -0.6219 1.3780 0.153 Uiso 1 1 calc R . . C19G C -0.0610(12) -0.5859(18) 1.4225(19) 0.21(3) Uiso 1 1 d . . . H19J H -0.0476 -0.6035 1.4302 0.319 Uiso 1 1 calc R . . H19K H -0.0749 -0.5891 1.4405 0.319 Uiso 1 1 calc R . . H19L H -0.0552 -0.5589 1.4235 0.319 Uiso 1 1 calc R . . S20 S -0.09623(19) -0.3567(3) 1.2722(3) 0.054(3) Uani 1 1 d . . . N20A N -0.0841(5) -0.4270(9) 1.2604(8) 0.040(9) Uiso 1 1 d . . . C20A C -0.0914(6) -0.3951(11) 1.2380(12) 0.042(12) Uiso 1 1 d . . . N20B N -0.0915(5) -0.3908(9) 1.2000(10) 0.046(9) Uiso 1 1 d . . . C20B C -0.0866(6) -0.4234(12) 1.1801(13) 0.046(12) Uiso 1 1 d . . . N20C N -0.0794(5) -0.4569(8) 1.1996(9) 0.040(9) Uiso 1 1 d . . . H20B H -0.0745 -0.4764 1.1850 0.047 Uiso 1 1 calc R . . C20C C -0.0792(8) -0.4633(14) 1.2417(14) 0.058(15) Uiso 1 1 d . . . O20 O -0.0745(4) -0.4930(7) 1.2586(8) 0.056(8) Uani 1 1 d . . . N20D N -0.0870(5) -0.4275(9) 1.1418(10) 0.045(9) Uiso 1 1 d . . . C20D C -0.0953(7) -0.3921(12) 1.1204(13) 0.078(15) Uiso 1 1 d . . . H20C H -0.0877 -0.3922 1.0941 0.094 Uiso 1 1 calc R . . H20D H -0.0890 -0.3689 1.1344 0.094 Uiso 1 1 calc R . . C20E C -0.1228(8) -0.3881(13) 1.1159(14) 0.13(2) Uiso 1 1 d . . . H20E H -0.1266 -0.3634 1.1029 0.188 Uiso 1 1 calc R . . H20F H -0.1306 -0.3886 1.1418 0.188 Uiso 1 1 calc R . . H20G H -0.1291 -0.4097 1.1002 0.188 Uiso 1 1 calc R . . C20F C -0.0810(7) -0.4614(11) 1.1183(12) 0.069(14) Uiso 1 1 d . . . H20H H -0.0662 -0.4744 1.1289 0.083 Uiso 1 1 calc R . . H20I H -0.0775 -0.4534 1.0910 0.083 Uiso 1 1 calc R . . C20G C -0.1035(7) -0.4905(12) 1.1190(13) 0.110(18) Uiso 1 1 d . . . H20J H -0.0992 -0.5141 1.1046 0.164 Uiso 1 1 calc R . . H20K H -0.1178 -0.4781 1.1068 0.164 Uiso 1 1 calc R . . H20L H -0.1074 -0.4972 1.1461 0.164 Uiso 1 1 calc R . . S21 S -0.07615(18) -0.3685(3) 1.3697(3) 0.054(3) Uani 1 1 d . . . N21A N -0.0492(5) -0.3825(8) 1.3121(10) 0.052(10) Uiso 1 1 d . . . C21A C -0.0499(7) -0.3645(11) 1.3484(12) 0.052(12) Uiso 1 1 d . . . N21B N -0.0281(5) -0.3435(8) 1.3583(9) 0.042(9) Uiso 1 1 d . . . C21B C -0.0077(7) -0.3446(10) 1.3368(12) 0.046(12) Uiso 1 1 d . . . N21C N -0.0079(6) -0.3628(8) 1.3011(10) 0.061(10) Uiso 1 1 d . . . H21B H 0.0055 -0.3627 1.2869 0.073 Uiso 1 1 calc R . . C21C C -0.0294(8) -0.3820(12) 1.2864(14) 0.049(13) Uiso 1 1 d . . . O21 O -0.0303(4) -0.3952(6) 1.2517(8) 0.041(7) Uani 1 1 d . . . N21D N 0.0137(6) -0.3249(9) 1.3456(10) 0.056(10) Uiso 1 1 d . . . C21D C 0.0135(7) -0.3030(10) 1.3829(11) 0.058(13) Uiso 1 1 d . . . H21C H 0.0231 -0.2788 1.3795 0.070 Uiso 1 1 calc R . . H21D H -0.0037 -0.2955 1.3889 0.070 Uiso 1 1 calc R . . C21E C 0.0235(8) -0.3247(13) 1.4161(14) 0.115(19) Uiso 1 1 d . . . H21E H 0.0224 -0.3087 1.4397 0.172 Uiso 1 1 calc R . . H21F H 0.0407 -0.3312 1.4110 0.172 Uiso 1 1 calc R . . H21G H 0.0140 -0.3487 1.4197 0.172 Uiso 1 1 calc R . . C21F C 0.0375(8) -0.3288(12) 1.3216(13) 0.092(16) Uiso 1 1 d . . . H21H H 0.0520 -0.3267 1.3390 0.110 Uiso 1 1 calc R . . H21I H 0.0380 -0.3545 1.3085 0.110 Uiso 1 1 calc R . . C21G C 0.0379(8) -0.2970(12) 1.2918(13) 0.104(17) Uiso 1 1 d . . . H21J H 0.0534 -0.2982 1.2770 0.157 Uiso 1 1 calc R . . H21K H 0.0367 -0.2717 1.3049 0.157 Uiso 1 1 calc R . . H21L H 0.0240 -0.3002 1.2739 0.157 Uiso 1 1 calc R . . S22 S 0.1066(2) 0.1226(3) 1.2372(4) 0.074(4) Uani 1 1 d . . . N22A N 0.0603(6) 0.1113(9) 1.2296(10) 0.059(10) Uiso 1 1 d . . . C22A C 0.0780(7) 0.1267(11) 1.2549(13) 0.059(13) Uiso 1 1 d . . . N22B N 0.0712(6) 0.1436(9) 1.2901(10) 0.058(10) Uiso 1 1 d . . . C22B C 0.0475(8) 0.1446(11) 1.3012(13) 0.051(12) Uiso 1 1 d . . . N22C N 0.0303(6) 0.1271(8) 1.2750(10) 0.065(11) Uiso 1 1 d . . . H22A H 0.0149 0.1263 1.2826 0.078 Uiso 1 1 calc R . . C22C C 0.0358(9) 0.1104(12) 1.2368(14) 0.061(15) Uiso 1 1 d . . . O22 O 0.0191(5) 0.0983(8) 1.2150(7) 0.063(9) Uani 1 1 d . . . N22D N 0.0376(6) 0.1604(9) 1.3310(10) 0.060(10) Uiso 1 1 d . . . C22D C 0.0562(8) 0.1828(12) 1.3547(13) 0.083(15) Uiso 1 1 d . . . H22B H 0.0712 0.1875 1.3389 0.100 Uiso 1 1 calc R . . H22C H 0.0493 0.2082 1.3625 0.100 Uiso 1 1 calc R . . C22E C 0.0625(8) 0.1604(13) 1.3892(14) 0.109(18) Uiso 1 1 d . . . H22D H 0.0739 0.1754 1.4055 0.164 Uiso 1 1 calc R . . H22E H 0.0703 0.1359 1.3814 0.164 Uiso 1 1 calc R . . H22F H 0.0476 0.1547 1.4042 0.164 Uiso 1 1 calc R . . S23 S 0.1136(2) 0.0690(3) 1.1485(4) 0.088(4) Uani 1 1 d . . . N23A N 0.0893(6) 0.0413(9) 1.2031(10) 0.057(10) Uiso 1 1 d . . . C23A C 0.1056(8) 0.0289(13) 1.1762(13) 0.066(14) Uiso 1 1 d . . . N23B N 0.1157(6) -0.0075(12) 1.1747(11) 0.087(12) Uiso 1 1 d . . . C23B C 0.1073(8) -0.0359(14) 1.2011(14) 0.066(14) Uiso 1 1 d . . . N23C N 0.0912(5) -0.0245(9) 1.2276(10) 0.058(10) Uiso 1 1 d . . . H23C H 0.0862 -0.0414 1.2451 0.069 Uiso 1 1 calc R . . C23C C 0.0819(9) 0.0135(16) 1.2290(16) 0.082(17) Uiso 1 1 d . . . O23 O 0.0678(5) 0.0233(7) 1.2595(9) 0.067(9) Uani 1 1 d . . . N23D N 0.1176(6) -0.0701(10) 1.1997(10) 0.064(10) Uiso 1 1 d . . . C23D C 0.1308(9) -0.0855(15) 1.1596(16) 0.12(2) Uiso 1 1 d . . . H23C H 0.1290 -0.1139 1.1558 0.149 Uiso 1 1 calc R . . H23D H 0.1250 -0.0714 1.1361 0.149 Uiso 1 1 calc R . . C23E C 0.1535(12) -0.0750(19) 1.171(2) 0.22(3) Uiso 1 1 d . . . H23E H 0.1652 -0.0809 1.1497 0.323 Uiso 1 1 calc R . . H23F H 0.1581 -0.0895 1.1943 0.323 Uiso 1 1 calc R . . H23G H 0.1538 -0.0471 1.1763 0.323 Uiso 1 1 calc R . . C22F C 0.0125(7) 0.1601(11) 1.3434(12) 0.065(13) Uiso 1 1 d . . . H22G H 0.0122 0.1614 1.3723 0.078 Uiso 1 1 calc R . . H22H H 0.0052 0.1348 1.3357 0.078 Uiso 1 1 calc R . . C22G C -0.0034(7) 0.1915(11) 1.3280(12) 0.090(16) Uiso 1 1 d . . . H22I H -0.0199 0.1890 1.3392 0.135 Uiso 1 1 calc R . . H22J H -0.0044 0.1895 1.2995 0.135 Uiso 1 1 calc R . . H22K H 0.0036 0.2168 1.3352 0.135 Uiso 1 1 calc R . . C23F C 0.1105(7) -0.1026(11) 1.2266(11) 0.065(13) Uiso 1 1 d . . . H23H H 0.1128 -0.1278 1.2132 0.078 Uiso 1 1 calc R . . H23I H 0.0929 -0.1001 1.2335 0.078 Uiso 1 1 calc R . . C23G C 0.1261(8) -0.1016(13) 1.2640(13) 0.112(18) Uiso 1 1 d . . . H23J H 0.1201 -0.1213 1.2823 0.168 Uiso 1 1 calc R . . H23K H 0.1249 -0.0758 1.2760 0.168 Uiso 1 1 calc R . . H23L H 0.1433 -0.1070 1.2575 0.168 Uiso 1 1 calc R . . S24 S 0.0768(2) 0.1519(3) 1.1512(4) 0.068(4) Uani 1 1 d . . . N24A N 0.0574(5) 0.0843(9) 1.1470(9) 0.054(10) Uiso 1 1 d . . . C24A C 0.0565(7) 0.1217(11) 1.1303(12) 0.047(12) Uiso 1 1 d . . . N24B N 0.0410(7) 0.1291(10) 1.1007(11) 0.084(12) Uiso 1 1 d . . . C24B C 0.0248(9) 0.1015(15) 1.0870(15) 0.080(16) Uiso 1 1 d . . . N24C N 0.0270(6) 0.0671(10) 1.1054(10) 0.070(11) Uiso 1 1 d . . . H24A H 0.0168 0.0491 1.0970 0.084 Uiso 1 1 calc R . . C24C C 0.0427(8) 0.0546(14) 1.1354(13) 0.053(14) Uiso 1 1 d . . . O24 O 0.0420(5) 0.0206(8) 1.1504(8) 0.082(10) Uani 1 1 d . . . N24D N 0.0085(8) 0.1078(12) 1.0612(12) 0.100(14) Uiso 1 1 d . . . C24D C 0.0085(9) 0.1494(13) 1.0394(14) 0.111(18) Uiso 1 1 d . . . H24B H -0.0073 0.1533 1.0257 0.133 Uiso 1 1 calc R . . H24C H 0.0105 0.1705 1.0588 0.133 Uiso 1 1 calc R . . C24E C 0.0287(8) 0.1506(13) 1.0114(13) 0.112(18) Uiso 1 1 d . . . H24D H 0.0290 0.1761 0.9985 0.167 Uiso 1 1 calc R . . H24E H 0.0264 0.1302 0.9918 0.167 Uiso 1 1 calc R . . H24F H 0.0443 0.1465 1.0251 0.167 Uiso 1 1 calc R . . C24F C -0.0137(10) 0.0831(16) 1.0512(16) 0.15(2) Uiso 1 1 d . . . H24G H -0.0283 0.0993 1.0451 0.175 Uiso 1 1 calc R . . H24H H -0.0177 0.0646 1.0724 0.175 Uiso 1 1 calc R . . C24G C -0.0030(9) 0.0601(14) 1.0112(16) 0.15(2) Uiso 1 1 d . . . H24I H -0.0149 0.0403 1.0029 0.224 Uiso 1 1 calc R . . H24J H 0.0128 0.0477 1.0173 0.224 Uiso 1 1 calc R . . H24K H -0.0006 0.0790 0.9901 0.224 Uiso 1 1 calc R . . N1S N 0.2493(5) 0.9101(8) 0.9953(9) 0.051(9) Uiso 1 1 d D . . C1S C 0.2480(7) 0.8766(8) 0.9939(12) 0.066(14) Uiso 1 1 d D . . C2S C 0.2474(7) 0.8329(8) 0.9948(11) 0.065(13) Uiso 1 1 d D . . H2S1 H 0.2599 0.8234 1.0132 0.098 Uiso 1 1 calc R . . H2S2 H 0.2509 0.8228 0.9687 0.098 Uiso 1 1 calc R . . H2S3 H 0.2311 0.8241 1.0033 0.098 Uiso 1 1 calc R . . N2S N -0.0277(6) -0.4229(10) 1.1419(12) 0.088(13) Uiso 1 1 d . . . C3S C -0.0226(7) -0.4416(12) 1.1674(13) 0.052(13) Uiso 1 1 d . . . C4S C -0.0137(6) -0.4684(10) 1.2000(11) 0.062(13) Uiso 1 1 d . . . H4S1 H -0.0188 -0.4952 1.1944 0.093 Uiso 1 1 calc R . . H4S2 H -0.0209 -0.4601 1.2249 0.093 Uiso 1 1 calc R . . H4S3 H 0.0043 -0.4672 1.2017 0.093 Uiso 1 1 calc R . . N3S N 0.3302(6) 0.7150(8) 0.9739(9) 0.052(10) Uiso 1 1 d . . . C5S C 0.3115(7) 0.7293(10) 0.9782(10) 0.036(11) Uiso 1 1 d . . . C6S C 0.2874(6) 0.7425(10) 0.9859(10) 0.046(12) Uiso 1 1 d . . . H6S1 H 0.2771 0.7204 0.9934 0.068 Uiso 1 1 calc R . . H6S2 H 0.2806 0.7547 0.9624 0.068 Uiso 1 1 calc R . . H6S3 H 0.2878 0.7615 1.0072 0.068 Uiso 1 1 calc R . . N4S N 0.1476(8) 0.7933(12) 1.2402(13) 0.125(16) Uiso 1 1 d . . . C7S C 0.1358(9) 0.7693(14) 1.2592(14) 0.087(16) Uiso 1 1 d . . . C8S C 0.1217(7) 0.7419(11) 1.2846(12) 0.083(15) Uiso 1 1 d . . . H8S1 H 0.1305 0.7381 1.3092 0.124 Uiso 1 1 calc R . . H8S2 H 0.1198 0.7169 1.2712 0.124 Uiso 1 1 calc R . . H8S3 H 0.1054 0.7529 1.2901 0.124 Uiso 1 1 calc R . . N5S N 0.0328(8) -0.0667(14) 0.8561(15) 0.141(18) Uiso 1 1 d . . . C9S C 0.0248(9) -0.0425(16) 0.8339(17) 0.097(18) Uiso 1 1 d . . . C10S C 0.0143(8) -0.0195(13) 0.8094(13) 0.101(18) Uiso 1 1 d . . . H10A H 0.0114 -0.0333 0.7848 0.152 Uiso 1 1 calc R . . H10C H 0.0249 0.0030 0.8046 0.152 Uiso 1 1 calc R . . H10N H -0.0015 -0.0107 0.8201 0.152 Uiso 1 1 calc R . . N6S N 0.1838(9) 0.5689(16) 0.8156(16) 0.16(2) Uiso 1 1 d . . . C11S C 0.1889(11) 0.545(2) 0.830(2) 0.14(2) Uiso 1 1 d . . . C12S C 0.1883(10) 0.5092(16) 0.8640(17) 0.17(3) Uiso 1 1 d . . . H12A H 0.1712 0.5012 0.8685 0.259 Uiso 1 1 calc R . . H12M H 0.1954 0.5187 0.8885 0.259 Uiso 1 1 calc R . . H12N H 0.1978 0.4870 0.8545 0.259 Uiso 1 1 calc R . . N7S N 0.0612(7) -0.1048(11) 1.1742(11) 0.096(14) Uiso 1 1 d . . . C13S C 0.0457(9) -0.0863(13) 1.1864(14) 0.084(16) Uiso 1 1 d . . . C14S C 0.0265(9) -0.0644(13) 1.2096(14) 0.13(2) Uiso 1 1 d . . . H14A H 0.0133 -0.0822 1.2173 0.189 Uiso 1 1 calc R . . H14M H 0.0197 -0.0434 1.1936 0.189 Uiso 1 1 calc R . . H14N H 0.0341 -0.0533 1.2331 0.189 Uiso 1 1 calc R . . N8S N 0.1895(5) 0.7252(8) 0.8961(9) 0.045(9) Uiso 1 1 d . . . C15S C 0.2045(7) 0.7354(11) 0.9191(13) 0.051(13) Uiso 1 1 d . . . C16S C 0.2196(6) 0.7472(9) 0.9467(10) 0.037(11) Uiso 1 1 d . . . H16G H 0.2101 0.7572 0.9688 0.055 Uiso 1 1 calc R . . H16M H 0.2302 0.7679 0.9365 0.055 Uiso 1 1 calc R . . H16N H 0.2298 0.7253 0.9554 0.055 Uiso 1 1 calc R . . N9S N -0.0663(7) -0.6000(10) 1.2968(11) 0.081(12) Uiso 1 1 d . . . C17S C -0.0507(8) -0.5797(12) 1.2875(12) 0.061(14) Uiso 1 1 d . . . C18S C -0.0302(6) -0.5504(10) 1.2729(11) 0.065(13) Uiso 1 1 d . . . H18A H -0.0145 -0.5568 1.2853 0.098 Uiso 1 1 calc R . . H18C H -0.0350 -0.5238 1.2798 0.098 Uiso 1 1 calc R . . H18N H -0.0286 -0.5525 1.2444 0.098 Uiso 1 1 calc R . . N10S N 0.2162(6) 0.7142(9) 1.1222(10) 0.063(11) Uiso 1 1 d . . . C19S C 0.2246(7) 0.7224(11) 1.0924(13) 0.050(13) Uiso 1 1 d . . . C20S C 0.2344(6) 0.7400(10) 1.0560(10) 0.048(12) Uiso 1 1 d . . . H20A H 0.2215 0.7553 1.0432 0.072 Uiso 1 1 calc R . . H20M H 0.2399 0.7193 1.0383 0.072 Uiso 1 1 calc R . . H20N H 0.2483 0.7569 1.0623 0.072 Uiso 1 1 calc R . . N11S N -0.1742(10) -0.4931(16) 1.3736(18) 0.20(2) Uiso 1 1 d . . . C21S C -0.1900(12) -0.4826(19) 1.342(2) 0.16(3) Uiso 1 1 d . . . C22S C -0.1951(10) -0.4748(16) 1.3059(18) 0.17(3) Uiso 1 1 d . . . H22L H -0.1958 -0.4991 1.2909 0.256 Uiso 1 1 calc R . . H22M H -0.1824 -0.4578 1.2950 0.256 Uiso 1 1 calc R . . H22N H -0.2111 -0.4617 1.3044 0.256 Uiso 1 1 calc R . . O1M O 0.1469(6) -0.4448(12) 1.2955(13) 0.181(19) Uani 1 1 d D . . C1M C 0.1563(12) -0.4140(17) 1.2690(18) 0.20(4) Uiso 1 1 d D . . H1M1 H 0.1430 -0.4048 1.2522 0.295 Uiso 1 1 calc R . . H1M2 H 0.1696 -0.4246 1.2529 0.295 Uiso 1 1 calc R . . H1M3 H 0.1626 -0.3923 1.2846 0.295 Uiso 1 1 calc R . . O2M O 0.0306(9) 0.2381(11) 1.4443(14) 0.20(2) Uani 1 1 d D . . C2M C 0.0546(10) 0.258(2) 1.443(2) 0.24(4) Uiso 1 1 d D . . H2M1 H 0.0622 0.2575 1.4690 0.364 Uiso 1 1 calc R . . H2M2 H 0.0522 0.2853 1.4349 0.364 Uiso 1 1 calc R . . H2M3 H 0.0654 0.2450 1.4243 0.364 Uiso 1 1 calc R . . O3M O 0.3646(8) 0.7094(12) 1.1890(13) 0.194(18) Uani 1 1 d DU . . C3M C 0.3803(11) 0.7306(17) 1.2172(17) 0.19(3) Uiso 1 1 d DU . . H3M1 H 0.3711 0.7528 1.2279 0.282 Uiso 1 1 calc R . . H3M2 H 0.3951 0.7401 1.2039 0.282 Uiso 1 1 calc R . . H3M3 H 0.3850 0.7131 1.2385 0.282 Uiso 1 1 calc R . . OW1 O -0.0445(5) 0.0418(8) 0.9033(10) 0.110(12) Uani 1 1 d . . . OW2 O -0.0039(7) -0.0039(10) 1.0822(11) 0.166(15) 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 0.057(4) 0.040(4) 0.031(5) 0.002(4) 0.005(4) 0.003(4) Co2 0.048(4) 0.029(4) 0.031(4) 0.004(4) 0.000(4) -0.004(3) Co3 0.045(4) 0.041(4) 0.042(5) -0.003(4) 0.002(4) 0.001(4) Co4 0.050(4) 0.053(5) 0.045(5) -0.002(4) 0.001(4) 0.000(4) Co5 0.042(4) 0.041(4) 0.043(5) -0.003(4) 0.011(4) 0.004(4) Co6 0.057(5) 0.047(5) 0.071(6) 0.016(4) 0.001(4) 0.003(4) Co7 0.048(4) 0.035(4) 0.052(5) -0.002(4) -0.001(4) 0.003(4) Co8 0.074(5) 0.054(5) 0.081(6) 0.014(5) 0.017(5) 0.014(4) S1 0.050(7) 0.056(7) 0.042(8) -0.017(7) -0.002(6) -0.010(6) O1 0.064(18) 0.025(16) 0.043(19) 0.021(14) 0.020(16) 0.009(15) S2 0.065(8) 0.043(7) 0.037(8) 0.017(6) -0.006(7) 0.002(6) O2 0.045(17) 0.055(19) 0.05(2) 0.022(16) -0.010(17) 0.005(15) S3 0.050(7) 0.038(7) 0.049(8) 0.013(6) 0.015(6) 0.009(6) O3 0.064(18) 0.037(17) 0.05(2) -0.017(15) 0.012(16) -0.011(15) S4 0.060(7) 0.030(7) 0.046(8) 0.000(6) 0.002(7) -0.006(6) O4 0.046(17) 0.056(18) 0.036(18) 0.029(16) 0.037(16) -0.027(15) S5 0.061(7) 0.024(6) 0.037(8) 0.007(6) -0.009(7) 0.013(6) O5 0.025(15) 0.048(17) 0.037(18) -0.002(14) 0.005(14) 0.007(15) S6 0.059(7) 0.023(7) 0.055(8) -0.001(6) -0.006(7) -0.006(6) O6 0.036(17) 0.057(19) 0.07(2) -0.029(19) -0.023(16) 0.015(15) S7 0.067(8) 0.039(7) 0.040(8) -0.008(6) -0.002(7) 0.000(6) O7 0.08(2) 0.029(17) 0.06(2) -0.017(16) 0.017(16) 0.016(15) S8 0.048(7) 0.066(8) 0.037(8) 0.009(7) 0.001(6) -0.002(6) O8 0.060(18) 0.030(16) 0.005(16) 0.013(14) -0.020(13) 0.010(13) S9 0.056(7) 0.052(8) 0.052(9) -0.009(7) -0.007(7) 0.005(6) O9 0.042(18) 0.060(18) 0.019(17) -0.017(14) 0.004(14) 0.004(15) S10 0.068(8) 0.058(8) 0.051(9) 0.000(7) 0.010(7) -0.007(7) O10 0.067(19) 0.044(18) 0.07(2) 0.021(18) 0.004(17) -0.032(16) S11 0.038(7) 0.072(8) 0.044(8) 0.006(7) -0.009(6) 0.000(6) O11 0.036(18) 0.09(2) 0.028(19) 0.030(16) 0.006(15) -0.007(16) S12 0.058(8) 0.063(8) 0.040(8) -0.005(7) -0.011(7) 0.003(6) O12 0.058(18) 0.062(19) 0.02(2) -0.001(16) 0.021(15) 0.005(15) S13 0.041(7) 0.067(8) 0.048(8) -0.003(7) 0.007(7) -0.002(6) O13 0.06(2) 0.10(2) 0.04(2) -0.018(18) 0.025(17) -0.019(19) S14 0.063(8) 0.038(7) 0.049(8) -0.001(6) 0.014(7) 0.006(6) O14 0.11(2) 0.08(2) 0.005(19) 0.011(16) 0.042(17) 0.037(18) S15 0.045(7) 0.055(8) 0.074(9) 0.012(7) -0.003(7) 0.008(6) O15 0.052(17) 0.022(17) 0.06(2) 0.015(15) 0.011(15) 0.018(14) S16 0.088(9) 0.094(10) 0.062(10) 0.025(8) 0.007(8) -0.009(8) O16 0.10(2) 0.07(2) 0.018(19) 0.016(16) 0.006(18) -0.009(18) S17 0.070(8) 0.078(9) 0.053(9) 0.011(8) -0.005(7) 0.009(7) O17 0.07(2) 0.09(2) 0.04(2) -0.015(18) -0.022(18) -0.010(18) S18 0.072(8) 0.049(8) 0.073(10) 0.035(7) 0.021(8) 0.010(7) O18 0.055(18) 0.059(19) 0.06(2) -0.003(17) 0.021(16) -0.014(16) S19 0.045(7) 0.046(7) 0.072(10) 0.003(7) -0.003(7) 0.001(6) O19 0.039(18) 0.062(19) 0.07(2) 0.014(17) -0.003(17) 0.005(15) S20 0.063(8) 0.036(7) 0.063(9) -0.010(7) 0.002(7) 0.007(6) O20 0.069(19) 0.043(18) 0.06(2) -0.002(17) -0.003(17) 0.005(16) S21 0.054(8) 0.059(8) 0.050(9) -0.010(7) 0.013(7) -0.003(6) O21 0.057(18) 0.030(16) 0.04(2) -0.005(15) -0.006(15) 0.003(14) S22 0.058(8) 0.071(9) 0.092(11) -0.003(8) 0.013(8) -0.011(7) O22 0.058(19) 0.10(2) 0.03(2) -0.012(18) -0.007(17) -0.005(18) S23 0.090(9) 0.065(9) 0.108(12) 0.015(9) 0.037(9) 0.018(8) O23 0.07(2) 0.044(18) 0.09(3) -0.005(18) 0.02(2) 0.008(16) S24 0.085(9) 0.043(8) 0.076(10) 0.010(7) 0.003(8) -0.006(7) O24 0.14(3) 0.06(2) 0.04(2) -0.009(18) 0.02(2) 0.00(2) O1M 0.10(3) 0.20(4) 0.25(5) -0.05(4) -0.01(3) 0.09(3) O2M 0.24(5) 0.11(3) 0.25(5) -0.03(3) 0.03(4) 0.08(3) O3M 0.19(4) 0.19(4) 0.21(4) 0.08(3) 0.02(4) 0.04(3) OW1 0.10(2) 0.07(2) 0.15(3) 0.01(2) 0.01(2) -0.032(19) OW2 0.20(4) 0.13(3) 0.17(4) 0.06(3) -0.02(3) -0.02(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3A 1.92(3) . ? Co1 N1A 1.95(3) . ? Co1 N2A 1.96(3) . ? Co1 S1 2.263(11) . ? Co1 S3 2.277(11) . ? Co1 S2 2.289(11) . ? Co2 N4A 1.94(3) . ? Co2 N6A 1.94(2) . ? Co2 N5A 1.98(3) . ? Co2 S5 2.280(11) . ? Co2 S6 2.292(11) . ? Co2 S4 2.311(11) . ? Co3 N9A 1.89(3) . ? Co3 N7A 1.95(3) . ? Co3 N8A 1.96(3) . ? Co3 S7 2.284(11) . ? Co3 S8 2.296(12) . ? Co3 S9 2.300(11) . ? Co4 N10A 1.84(3) . ? Co4 N12A 1.94(3) . ? Co4 N11A 1.94(3) . ? Co4 S12 2.267(12) . ? Co4 S10 2.268(12) . ? Co4 S11 2.280(11) . ? Co4 C10A 2.46(4) . ? Co4 C11A 2.49(4) . ? Co5 N13A 1.92(3) . ? Co5 N15A 1.92(3) . ? Co5 N14A 1.99(3) . ? Co5 S15 2.277(11) . ? Co5 S13 2.283(11) . ? Co5 S14 2.293(12) . ? Co5 C14A 2.47(4) . ? Co5 C13A 2.49(5) . ? Co6 N16A 1.91(3) . ? Co6 N17A 1.93(3) . ? Co6 N18A 1.95(3) . ? Co6 S16 2.269(13) . ? Co6 S17 2.276(13) . ? Co6 S18 2.286(12) . ? Co7 N19A 1.89(3) . ? Co7 N20A 1.94(3) . ? Co7 N21A 1.95(3) . ? Co7 S19 2.270(11) . ? Co7 S21 2.276(12) . ? Co7 S20 2.281(12) . ? Co7 C21A 2.51(4) . ? Co8 N23A 1.93(3) . ? Co8 N24A 1.95(3) . ? Co8 N22A 1.96(3) . ? Co8 S23 2.249(13) . ? Co8 S24 2.272(12) . ? Co8 S22 2.290(14) . ? S1 C1A 1.75(4) . ? N1A C1C 1.28(4) . ? N1A C1A 1.29(4) . ? C1A N1B 1.38(4) . ? N1B C1B 1.29(4) . ? C1B N1D 1.32(4) . ? C1B N1C 1.38(4) . ? N1C C1C 1.35(4) . ? C1C O1 1.24(4) . ? N1D C1F 1.39(4) . ? N1D C1D 1.46(4) . ? C1D C1E 1.48(4) . ? C1F C1G 1.58(4) . ? S2 C2A 1.64(4) . ? N2A C2C 1.32(4) . ? N2A C2A 1.44(4) . ? C2A N2B 1.36(4) . ? N2B C2B 1.35(4) . ? C2B N2C 1.32(4) . ? C2B N2D 1.35(4) . ? N2C C2C 1.44(4) . ? C2C O2 1.18(4) . ? N2D C2D 1.48(4) . ? N2D C2F 1.49(4) . ? C2D C2E 1.49(4) . ? C2F C2G 1.42(4) . ? S3 C3A 1.71(4) . ? N3A C3A 1.32(4) . ? N3A C3C 1.34(4) . ? C3A N3B 1.37(4) . ? N3B C3B 1.33(4) . ? C3B N3D 1.28(4) . ? C3B N3C 1.33(4) . ? N3C C3C 1.40(4) . ? C3C O3 1.26(4) . ? N3D C3F 1.42(4) . ? N3D C3D 1.45(4) . ? C3D C3E 1.42(4) . ? C3F C3G 1.51(4) . ? S4 C4A 1.74(4) . ? N4A C4A 1.37(4) . ? N4A C4C 1.44(4) . ? C4A N4B 1.33(4) . ? N4B C4B 1.33(4) . ? C4B N4C 1.34(4) . ? C4B N4D 1.35(4) . ? N4C C4C 1.52(4) . ? C4C O4 1.13(3) . ? N4D C4F 1.46(4) . ? N4D C4D 1.48(4) . ? C4D C4E 1.25(6) . ? C4F C4G 1.48(4) . ? S5 C5A 1.74(3) . ? N5A C5C 1.35(4) . ? N5A C5A 1.45(3) . ? C5A N5B 1.31(3) . ? N5B C5B 1.34(4) . ? C5B N5D 1.32(4) . ? C5B N5C 1.34(3) . ? N5C C5C 1.39(4) . ? C5C O5 1.18(4) . ? N5D C5F 1.43(4) . ? N5D C5D 1.47(4) . ? C5D C5E 1.50(4) . ? C5F C5G 1.46(4) . ? S6 C6A 1.66(3) . ? N6A C6C 1.38(4) . ? N6A C6A 1.39(3) . ? C6A N6B 1.34(3) . ? N6B C6B 1.38(4) . ? C6B N6D 1.22(4) . ? C6B N6C 1.45(4) . ? N6C C6C 1.38(4) . ? C6C O6 1.16(4) . ? N6D C6F 1.50(4) . ? N6D C6D 1.51(4) . ? C6D C6E 1.45(4) . ? C6F C6G 1.42(6) . ? S7 C7A 1.70(4) . ? N7A C7C 1.33(4) . ? N7A C7A 1.35(4) . ? C7A N7B 1.34(4) . ? N7B C7B 1.35(4) . ? C7B N7D 1.37(4) . ? C7B N7C 1.39(4) . ? N7C C7C 1.42(4) . ? C7C O7 1.21(4) . ? N7D C7D 1.43(4) . ? N7D C7F 1.52(4) . ? C7D C7E 1.57(4) . ? C7F C7G 1.52(4) . ? S8 C8A 1.77(4) . ? N8A C8C 1.37(4) . ? N8A C8A 1.37(4) . ? C8A N8B 1.30(4) . ? N8B C8B 1.28(3) . ? C8B N8D 1.28(3) . ? C8B N8C 1.40(4) . ? N8C C8C 1.45(4) . ? C8C O8 1.17(4) . ? N8D C8F 1.46(4) . ? N8D C8D 1.49(4) . ? C8D C8E 1.56(4) . ? C8F C8G 1.47(4) . ? S9 C9A 1.71(3) . ? N9A C9A 1.36(3) . ? N9A C9C 1.45(4) . ? C9A N9B 1.38(4) . ? N9B C9B 1.38(4) . ? C9B N9C 1.33(3) . ? C9B N9D 1.37(4) . ? N9C C9C 1.35(4) . ? C9C O9 1.19(4) . ? N9D C9F 1.46(3) . ? N9D C9D 1.49(4) . ? C9D C9E 1.32(5) . ? C9F C9G 1.57(4) . ? S10 C10A 1.68(4) . ? N10A C10C 1.29(5) . ? N10A C10A 1.33(4) . ? C10A N10B 1.40(4) . ? N10B C10B 1.37(4) . ? C10B N10C 1.30(4) . ? C10B N10D 1.36(4) . ? N10C C10C 1.41(5) . ? C10C O10 1.25(4) . ? N10D C10D 1.46(4) . ? N10D C10F 1.52(4) . ? C10D C10E 1.57(4) . ? C10F C10G 1.46(5) . ? S11 C11A 1.66(4) . ? N11A C11A 1.30(4) . ? N11A C11C 1.37(4) . ? C11A N11B 1.34(4) . ? N11B C11B 1.40(4) . ? C11B N11D 1.35(4) . ? C11B N11C 1.37(4) . ? N11C C11C 1.42(4) . ? C11C O11 1.18(4) . ? N11D C11F 1.44(4) . ? N11D C11D 1.45(4) . ? C11D C11E 1.49(4) . ? C11F C11G 1.51(4) . ? S12 C12A 1.70(4) . ? N12A C12A 1.27(4) . ? N12A C12C 1.35(4) . ? C12A N12B 1.29(4) . ? N12B C12B 1.41(4) . ? C12B N12C 1.34(4) . ? C12B N12D 1.38(4) . ? N12C C12C 1.36(4) . ? C12C O12 1.27(4) . ? N12D C12F 1.49(5) . ? N12D C12D 1.62(6) . ? C12D C12E 1.37(6) . ? C12F C12G 1.53(6) . ? S13 C13A 1.66(4) . ? N13A C13C 1.29(4) . ? N13A C13A 1.35(4) . ? C13A N13B 1.36(4) . ? N13B C13B 1.37(4) . ? C13B N13D 1.35(4) . ? C13B N13C 1.36(4) . ? N13C C13C 1.41(4) . ? C13C O13 1.16(4) . ? N13D C13F 1.45(4) . ? N13D C13D 1.50(4) . ? C13D C13E 1.49(5) . ? C13F C13G 1.61(5) . ? S14 C14A 1.69(4) . ? N14A C14A 1.35(4) . ? N14A C14C 1.38(4) . ? C14A N14B 1.42(4) . ? N14B C14B 1.38(4) . ? C14B N14D 1.37(4) . ? C14B N14C 1.40(4) . ? N14C C14C 1.48(4) . ? C14C O14 1.11(4) . ? N14D C14F 1.39(3) . ? N14D C14D 1.45(4) . ? C14D C14E 1.60(5) . ? C14F C14G 1.46(4) . ? S15 C15A 1.71(4) . ? N15A C15A 1.34(4) . ? N15A C15C 1.36(4) . ? C15A N15B 1.32(4) . ? N15B C15B 1.38(4) . ? C15B N15C 1.38(4) . ? C15B N15D 1.40(4) . ? N15C C15C 1.39(4) . ? C15C O15 1.18(3) . ? N15D C15F 1.42(4) . ? N15D C15D 1.43(4) . ? C15D C15E 1.51(5) . ? C15F C15G 1.59(5) . ? S16 C16A 1.70(5) . ? N16A C16A 1.31(4) . ? N16A C16C 1.33(4) . ? C16A N16B 1.37(4) . ? N16B C16B 1.36(5) . ? C16B N16D 1.31(5) . ? C16B N16C 1.43(4) . ? N16C C16C 1.44(4) . ? C16C O16 1.23(4) . ? N16D C16F 1.44(5) . ? N16D C16D 1.46(2) . ? C16D C16E 1.52(2) . ? C16F C16G 1.47(5) . ? S17 C17A 1.71(3) . ? N17A C17A 1.31(4) . ? N17A C17C 1.49(4) . ? C17A N17B 1.36(4) . ? N17B C17B 1.28(4) . ? C17B N17D 1.31(4) . ? C17B N17C 1.34(4) . ? N17C C17C 1.46(4) . ? C17C O17 1.15(4) . ? N17D C17D 1.465(19) . ? N17D C17F 1.47(4) . ? C17D C17E 1.52(2) . ? C17F C17G 1.45(4) . ? S18 C18A 1.71(4) . ? N18A C18C 1.32(4) . ? N18A C18A 1.36(4) . ? C18A N18B 1.29(4) . ? N18B C18B 1.29(4) . ? C18B N18D 1.28(4) . ? C18B N18C 1.38(4) . ? N18C C18C 1.35(4) . ? C18C O18 1.30(4) . ? N18D C18F 1.48(5) . ? N18D C18D 1.57(4) . ? C18D C18E 1.45(4) . ? C18F C18G 1.48(6) . ? S19 C19A 1.73(3) . ? N19A C19C 1.39(4) . ? N19A C19A 1.40(4) . ? C19A N19B 1.33(4) . ? N19B C19B 1.28(4) . ? C19B N19D 1.26(4) . ? C19B N19C 1.36(4) . ? N19C C19C 1.42(4) . ? C19C O19 1.22(4) . ? N19D C19D 1.48(4) . ? N19D C19F 1.51(5) . ? C19D C19E 1.52(6) . ? C19F C19G 1.51(7) . ? S20 C20A 1.75(4) . ? N20A C20A 1.37(4) . ? N20A C20C 1.40(4) . ? C20A N20B 1.28(4) . ? N20B C20B 1.31(4) . ? C20B N20D 1.29(4) . ? C20B N20C 1.36(4) . ? N20C C20C 1.43(4) . ? C20C O20 1.18(4) . ? N20D C20F 1.43(4) . ? N20D C20D 1.46(4) . ? C20D C20E 1.48(5) . ? C20F C20G 1.55(4) . ? S21 C21A 1.58(4) . ? N21A C21A 1.36(4) . ? N21A C21C 1.36(4) . ? C21A N21B 1.40(4) . ? N21B C21B 1.30(4) . ? C21B N21C 1.34(4) . ? C21B N21D 1.35(4) . ? N21C C21C 1.40(4) . ? C21C O21 1.25(4) . ? N21D C21D 1.45(4) . ? N21D C21F 1.51(4) . ? C21D C21E 1.43(5) . ? C21F C21G 1.47(5) . ? S22 C22A 1.64(4) . ? N22A C22C 1.33(4) . ? N22A C22A 1.37(4) . ? C22A N22B 1.36(4) . ? N22B C22B 1.31(4) . ? C22B N22D 1.25(4) . ? C22B N22C 1.40(4) . ? N22C C22C 1.43(4) . ? C22C O22 1.22(4) . ? N22D C22F 1.40(4) . ? N22D C22D 1.48(4) . ? C22D C22E 1.42(5) . ? S23 C23A 1.69(4) . ? N23A C23A 1.32(4) . ? N23A C23C 1.34(5) . ? C23A N23B 1.34(4) . ? N23B C23B 1.38(4) . ? C23B N23D 1.28(4) . ? C23B N23C 1.29(4) . ? N23C C23C 1.37(5) . ? C23C O23 1.31(5) . ? N23D C23F 1.47(4) . ? N23D C23D 1.60(5) . ? C23D C23E 1.32(6) . ? C22F C22G 1.45(4) . ? C23F C23G 1.50(5) . ? S24 C24A 1.64(4) . ? N24A C24C 1.33(4) . ? N24A C24A 1.38(4) . ? C24A N24B 1.31(4) . ? N24B C24B 1.35(5) . ? C24B N24D 1.24(5) . ? C24B N24C 1.32(5) . ? N24C C24C 1.37(4) . ? C24C O24 1.25(4) . ? N24D C24F 1.48(5) . ? N24D C24D 1.58(5) . ? C24D C24E 1.43(5) . ? C24F C24G 1.65(6) . ? N1S C1S 1.131(10) . ? C1S C2S 1.473(10) . ? N2S C3S 1.09(4) . ? C3S C4S 1.50(5) . ? N3S C5S 1.12(3) . ? C5S C6S 1.38(4) . ? N4S C7S 1.21(5) . ? C7S C8S 1.46(5) . ? N5S C9S 1.18(6) . ? C9S C10S 1.26(6) . ? N6S C11S 0.98(7) . ? C11S C12S 1.65(7) . ? N7S C13S 1.11(5) . ? C13S C14S 1.48(5) . ? N8S C15S 1.16(4) . ? C15S C16S 1.29(4) . ? N9S C17S 1.12(4) . ? C17S C18S 1.55(5) . ? N10S C19S 1.13(4) . ? C19S C20S 1.45(4) . ? N11S C21S 1.38(7) . ? C21S C22S 1.29(8) . ? O1M C1M 1.45(2) . ? O2M C2M 1.45(2) . ? O3M C3M 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3A Co1 N1A 99.7(12) . . ? N3A Co1 N2A 97.0(11) . . ? N1A Co1 N2A 95.9(10) . . ? N3A Co1 S1 168.3(9) . . ? N1A Co1 S1 72.3(9) . . ? N2A Co1 S1 92.4(8) . . ? N3A Co1 S3 70.9(9) . . ? N1A Co1 S3 92.1(7) . . ? N2A Co1 S3 166.6(8) . . ? S1 Co1 S3 100.3(4) . . ? N3A Co1 S2 89.1(8) . . ? N1A Co1 S2 166.5(8) . . ? N2A Co1 S2 72.8(9) . . ? S1 Co1 S2 100.3(4) . . ? S3 Co1 S2 100.5(4) . . ? N4A Co2 N6A 97.3(12) . . ? N4A Co2 N5A 96.0(12) . . ? N6A Co2 N5A 95.1(10) . . ? N4A Co2 S5 92.0(9) . . ? N6A Co2 S5 166.0(8) . . ? N5A Co2 S5 73.5(8) . . ? N4A Co2 S6 168.2(10) . . ? N6A Co2 S6 72.5(8) . . ? N5A Co2 S6 90.8(8) . . ? S5 Co2 S6 99.1(4) . . ? N4A Co2 S4 72.0(10) . . ? N6A Co2 S4 94.1(8) . . ? N5A Co2 S4 165.8(8) . . ? S5 Co2 S4 98.7(4) . . ? S6 Co2 S4 102.4(4) . . ? N9A Co3 N7A 98.5(12) . . ? N9A Co3 N8A 95.6(11) . . ? N7A Co3 N8A 98.2(12) . . ? N9A Co3 S7 168.4(9) . . ? N7A Co3 S7 72.2(10) . . ? N8A Co3 S7 92.6(8) . . ? N9A Co3 S8 90.7(9) . . ? N7A Co3 S8 166.5(9) . . ? N8A Co3 S8 71.0(9) . . ? S7 Co3 S8 99.7(4) . . ? N9A Co3 S9 72.1(9) . . ? N7A Co3 S9 93.0(9) . . ? N8A Co3 S9 164.6(9) . . ? S7 Co3 S9 101.0(4) . . ? S8 Co3 S9 99.2(4) . . ? N10A Co4 N12A 99.1(13) . . ? N10A Co4 N11A 98.9(13) . . ? N12A Co4 N11A 100.1(13) . . ? N10A Co4 S12 91.0(10) . . ? N12A Co4 S12 70.2(11) . . ? N11A Co4 S12 167.3(9) . . ? N10A Co4 S10 73.6(10) . . ? N12A Co4 S10 164.5(11) . . ? N11A Co4 S10 94.5(8) . . ? S12 Co4 S10 95.9(4) . . ? N10A Co4 S11 165.3(10) . . ? N12A Co4 S11 93.7(9) . . ? N11A Co4 S11 71.4(9) . . ? S12 Co4 S11 100.4(4) . . ? S10 Co4 S11 95.7(4) . . ? N10A Co4 C10A 32.2(11) . . ? N12A Co4 C10A 130.4(13) . . ? N11A Co4 C10A 97.6(12) . . ? S12 Co4 C10A 95.0(9) . . ? S10 Co4 C10A 41.5(9) . . ? S11 Co4 C10A 136.0(10) . . ? N10A Co4 C11A 129.5(13) . . ? N12A Co4 C11A 97.3(13) . . ? N11A Co4 C11A 31.0(10) . . ? S12 Co4 C11A 139.5(9) . . ? S10 Co4 C11A 97.8(9) . . ? S11 Co4 C11A 40.5(9) . . ? C10A Co4 C11A 120.0(12) . . ? N13A Co5 N15A 97.3(13) . . ? N13A Co5 N14A 97.1(13) . . ? N15A Co5 N14A 97.0(12) . . ? N13A Co5 S15 91.1(9) . . ? N15A Co5 S15 71.7(9) . . ? N14A Co5 S15 167.0(10) . . ? N13A Co5 S13 72.6(10) . . ? N15A Co5 S13 166.6(10) . . ? N14A Co5 S13 93.1(9) . . ? S15 Co5 S13 99.1(4) . . ? N13A Co5 S14 168.8(10) . . ? N15A Co5 S14 91.1(9) . . ? N14A Co5 S14 74.5(10) . . ? S15 Co5 S14 98.6(4) . . ? S13 Co5 S14 100.0(4) . . ? N13A Co5 C14A 129.9(12) . . ? N15A Co5 C14A 94.8(12) . . ? N14A Co5 C14A 33.0(11) . . ? S15 Co5 C14A 138.8(10) . . ? S13 Co5 C14A 98.4(9) . . ? S14 Co5 C14A 41.5(9) . . ? N13A Co5 C13A 32.4(11) . . ? N15A Co5 C13A 129.6(13) . . ? N14A Co5 C13A 93.8(13) . . ? S15 Co5 C13A 98.5(9) . . ? S13 Co5 C13A 40.4(9) . . ? S14 Co5 C13A 139.0(10) . . ? C14A Co5 C13A 118.6(13) . . ? N16A Co6 N17A 98.5(13) . . ? N16A Co6 N18A 100.0(14) . . ? N17A Co6 N18A 98.3(13) . . ? N16A Co6 S16 70.9(11) . . ? N17A Co6 S16 91.6(9) . . ? N18A Co6 S16 167.5(10) . . ? N16A Co6 S17 164.6(11) . . ? N17A Co6 S17 70.9(10) . . ? N18A Co6 S17 92.7(9) . . ? S16 Co6 S17 97.7(5) . . ? N16A Co6 S18 93.9(9) . . ? N17A Co6 S18 165.2(10) . . ? N18A Co6 S18 71.5(10) . . ? S16 Co6 S18 100.0(4) . . ? S17 Co6 S18 98.4(5) . . ? N19A Co7 N20A 96.2(13) . . ? N19A Co7 N21A 101.6(13) . . ? N20A Co7 N21A 98.9(13) . . ? N19A Co7 S19 70.9(10) . . ? N20A Co7 S19 92.4(8) . . ? N21A Co7 S19 167.2(11) . . ? N19A Co7 S21 94.4(10) . . ? N20A Co7 S21 166.3(9) . . ? N21A Co7 S21 70.5(10) . . ? S19 Co7 S21 99.2(4) . . ? N19A Co7 S20 165.3(10) . . ? N20A Co7 S20 71.7(9) . . ? N21A Co7 S20 88.8(9) . . ? S19 Co7 S20 100.6(4) . . ? S21 Co7 S20 98.9(4) . . ? N19A Co7 C21A 98.4(12) . . ? N20A Co7 C21A 131.1(12) . . ? N21A Co7 C21A 32.5(11) . . ? S19 Co7 C21A 136.4(10) . . ? S21 Co7 C21A 38.1(9) . . ? S20 Co7 C21A 95.9(9) . . ? N23A Co8 N24A 97.6(13) . . ? N23A Co8 N22A 99.0(14) . . ? N24A Co8 N22A 96.8(13) . . ? N23A Co8 S23 70.6(11) . . ? N24A Co8 S23 92.2(9) . . ? N22A Co8 S23 167.1(10) . . ? N23A Co8 S24 164.7(11) . . ? N24A Co8 S24 72.2(10) . . ? N22A Co8 S24 93.7(9) . . ? S23 Co8 S24 97.9(5) . . ? N23A Co8 S22 94.4(10) . . ? N24A Co8 S22 164.6(10) . . ? N22A Co8 S22 71.7(11) . . ? S23 Co8 S22 100.9(5) . . ? S24 Co8 S22 97.7(5) . . ? C1A S1 Co1 77.0(14) . . ? C1C N1A C1A 118(4) . . ? C1C N1A Co1 140(3) . . ? C1A N1A Co1 101(3) . . ? N1A C1A N1B 126(4) . . ? N1A C1A S1 110(3) . . ? N1B C1A S1 125(3) . . ? C1B N1B C1A 114(3) . . ? N1B C1B N1D 119(4) . . ? N1B C1B N1C 122(4) . . ? N1D C1B N1C 119(4) . . ? C1C N1C C1B 117(4) . . ? O1 C1C N1A 122(4) . . ? O1 C1C N1C 116(4) . . ? N1A C1C N1C 122(4) . . ? C1B N1D C1F 126(4) . . ? C1B N1D C1D 121(3) . . ? C1F N1D C1D 112(3) . . ? N1D C1D C1E 111(3) . . ? N1D C1F C1G 114(3) . . ? C2A S2 Co1 79.6(14) . . ? C2C N2A C2A 126(3) . . ? C2C N2A Co1 137(3) . . ? C2A N2A Co1 97(2) . . ? N2B C2A N2A 120(3) . . ? N2B C2A S2 129(3) . . ? N2A C2A S2 111(3) . . ? C2B N2B C2A 114(3) . . ? N2C C2B N2B 125(4) . . ? N2C C2B N2D 118(4) . . ? N2B C2B N2D 118(4) . . ? C2B N2C C2C 125(3) . . ? O2 C2C N2A 129(4) . . ? O2 C2C N2C 121(4) . . ? N2A C2C N2C 109(4) . . ? C2B N2D C2D 120(3) . . ? C2B N2D C2F 123(3) . . ? C2D N2D C2F 117(3) . . ? N2D C2D C2E 114(3) . . ? C2G C2F N2D 110(3) . . ? C3A S3 Co1 78.2(15) . . ? C3A N3A C3C 118(3) . . ? C3A N3A Co1 103(2) . . ? C3C N3A Co1 139(3) . . ? N3A C3A N3B 127(4) . . ? N3A C3A S3 108(3) . . ? N3B C3A S3 125(3) . . ? C3B N3B C3A 116(3) . . ? N3D C3B N3B 120(4) . . ? N3D C3B N3C 120(4) . . ? N3B C3B N3C 119(4) . . ? C3B N3C C3C 124(3) . . ? O3 C3C N3A 125(4) . . ? O3 C3C N3C 118(3) . . ? N3A C3C N3C 116(4) . . ? C3B N3D C3F 123(3) . . ? C3B N3D C3D 120(3) . . ? C3F N3D C3D 117(3) . . ? C3E C3D N3D 109(3) . . ? N3D C3F C3G 113(3) . . ? C4A S4 Co2 78.5(16) . . ? C4A N4A C4C 123(3) . . ? C4A N4A Co2 102(3) . . ? C4C N4A Co2 134(3) . . ? N4B C4A N4A 129(4) . . ? N4B C4A S4 123(3) . . ? N4A C4A S4 107(3) . . ? C4A N4B C4B 113(4) . . ? N4B C4B N4C 121(4) . . ? N4B C4B N4D 120(4) . . ? N4C C4B N4D 118(4) . . ? C4B N4C C4C 130(3) . . ? O4 C4C N4A 132(4) . . ? O4 C4C N4C 126(3) . . ? N4A C4C N4C 102(3) . . ? C4B N4D C4F 126(3) . . ? C4B N4D C4D 119(3) . . ? C4F N4D C4D 115(3) . . ? C4E C4D N4D 104(4) . . ? N4D C4F C4G 110(3) . . ? C5A S5 Co2 80.9(12) . . ? C5C N5A C5A 119(3) . . ? C5C N5A Co2 142(3) . . ? C5A N5A Co2 99(2) . . ? N5B C5A N5A 125(3) . . ? N5B C5A S5 129(3) . . ? N5A C5A S5 106(2) . . ? C5A N5B C5B 113(3) . . ? N5D C5B N5C 119(3) . . ? N5D C5B N5B 117(3) . . ? N5C C5B N5B 125(3) . . ? C5B N5C C5C 123(3) . . ? O5 C5C N5A 122(4) . . ? O5 C5C N5C 124(4) . . ? N5A C5C N5C 114(4) . . ? C5B N5D C5F 124(3) . . ? C5B N5D C5D 119(3) . . ? C5F N5D C5D 117(3) . . ? N5D C5D C5E 112(3) . . ? N5D C5F C5G 115(3) . . ? C6A S6 Co2 78.4(13) . . ? C6C N6A C6A 124(3) . . ? C6C N6A Co2 138(3) . . ? C6A N6A Co2 98(2) . . ? N6B C6A N6A 121(3) . . ? N6B C6A S6 128(3) . . ? N6A C6A S6 111(2) . . ? C6A N6B C6B 123(3) . . ? N6D C6B N6B 126(4) . . ? N6D C6B N6C 124(4) . . ? N6B C6B N6C 109(3) . . ? C6C N6C C6B 133(3) . . ? O6 C6C N6C 125(4) . . ? O6 C6C N6A 125(4) . . ? N6C C6C N6A 108(4) . . ? C6B N6D C6F 128(4) . . ? C6B N6D C6D 119(3) . . ? C6F N6D C6D 113(3) . . ? C6E C6D N6D 111(3) . . ? C6G C6F N6D 108(4) . . ? C7A S7 Co3 77.9(14) . . ? C7C N7A C7A 123(4) . . ? C7C N7A Co3 137(3) . . ? C7A N7A Co3 100(3) . . ? N7B C7A N7A 125(4) . . ? N7B C7A S7 124(3) . . ? N7A C7A S7 110(3) . . ? C7A N7B C7B 113(3) . . ? N7B C7B N7D 122(4) . . ? N7B C7B N7C 123(4) . . ? N7D C7B N7C 115(3) . . ? C7B N7C C7C 121(3) . . ? O7 C7C N7A 129(4) . . ? O7 C7C N7C 118(4) . . ? N7A C7C N7C 113(4) . . ? C7B N7D C7D 115(3) . . ? C7B N7D C7F 126(3) . . ? C7D N7D C7F 119(3) . . ? N7D C7D C7E 110(3) . . ? N7D C7F C7G 110(3) . . ? C8A S8 Co3 80.5(14) . . ? C8C N8A C8A 123(3) . . ? C8C N8A Co3 132(2) . . ? C8A N8A Co3 105(2) . . ? N8B C8A N8A 127(3) . . ? N8B C8A S8 129(3) . . ? N8A C8A S8 104(3) . . ? C8B N8B C8A 117(3) . . ? N8B C8B N8D 123(4) . . ? N8B C8B N8C 119(3) . . ? N8D C8B N8C 118(3) . . ? C8B N8C C8C 127(3) . . ? O8 C8C N8A 135(4) . . ? O8 C8C N8C 119(3) . . ? N8A C8C N8C 106(3) . . ? C8B N8D C8F 128(3) . . ? C8B N8D C8D 116(3) . . ? C8F N8D C8D 116(3) . . ? N8D C8D C8E 107(3) . . ? N8D C8F C8G 116(3) . . ? C9A S9 Co3 77.6(13) . . ? C9A N9A C9C 118(3) . . ? C9A N9A Co3 102(2) . . ? C9C N9A Co3 140(3) . . ? N9A C9A N9B 128(3) . . ? N9A C9A S9 108(3) . . ? N9B C9A S9 124(3) . . ? C9B N9B C9A 111(3) . . ? N9C C9B N9D 123(3) . . ? N9C C9B N9B 124(3) . . ? N9D C9B N9B 114(3) . . ? C9B N9C C9C 126(3) . . ? O9 C9C N9C 128(4) . . ? O9 C9C N9A 119(4) . . ? N9C C9C N9A 113(4) . . ? C9B N9D C9F 120(3) . . ? C9B N9D C9D 124(3) . . ? C9F N9D C9D 116(3) . . ? C9E C9D N9D 113(4) . . ? N9D C9F C9G 110(3) . . ? C10A S10 Co4 75.5(15) . . ? C10C N10A C10A 114(4) . . ? C10C N10A Co4 146(3) . . ? C10A N10A Co4 100(3) . . ? N10A C10A N10B 128(4) . . ? N10A C10A S10 110(3) . . ? N10B C10A S10 121(3) . . ? N10A C10A Co4 47(2) . . ? N10B C10A Co4 175(3) . . ? S10 C10A Co4 63.0(13) . . ? C10B N10B C10A 112(3) . . ? N10C C10B N10D 121(4) . . ? N10C C10B N10B 124(4) . . ? N10D C10B N10B 115(3) . . ? C10B N10C C10C 117(4) . . ? O10 C10C N10A 123(5) . . ? O10 C10C N10C 112(5) . . ? N10A C10C N10C 125(5) . . ? C10B N10D C10D 122(3) . . ? C10B N10D C10F 120(3) . . ? C10D N10D C10F 117(3) . . ? N10D C10D C10E 107(3) . . ? C10G C10F N10D 106(3) . . ? C11A S11 Co4 76.6(14) . . ? C11A N11A C11C 128(4) . . ? C11A N11A Co4 99(3) . . ? C11C N11A Co4 133(3) . . ? N11A C11A N11B 122(4) . . ? N11A C11A S11 113(3) . . ? N11B C11A S11 125(3) . . ? N11A C11A Co4 50(2) . . ? N11B C11A Co4 171(3) . . ? S11 C11A Co4 62.9(13) . . ? C11A N11B C11B 118(3) . . ? N11D C11B N11C 119(4) . . ? N11D C11B N11B 124(4) . . ? N11C C11B N11B 118(4) . . ? C11B N11C C11C 125(3) . . ? O11 C11C N11A 130(4) . . ? O11 C11C N11C 120(4) . . ? N11A C11C N11C 110(4) . . ? C11B N11D C11F 122(3) . . ? C11B N11D C11D 117(3) . . ? C11F N11D C11D 121(3) . . ? N11D C11D C11E 112(3) . . ? N11D C11F C11G 113(3) . . ? C12A S12 Co4 78.0(15) . . ? C12A N12A C12C 120(4) . . ? C12A N12A Co4 102(3) . . ? C12C N12A Co4 137(3) . . ? N12A C12A N12B 127(4) . . ? N12A C12A S12 109(3) . . ? N12B C12A S12 124(3) . . ? C12A N12B C12B 113(4) . . ? N12C C12B N12D 122(5) . . ? N12C C12B N12B 123(4) . . ? N12D C12B N12B 114(4) . . ? C12B N12C C12C 117(4) . . ? O12 C12C N12A 127(4) . . ? O12 C12C N12C 113(4) . . ? N12A C12C N12C 119(4) . . ? C12B N12D C12F 121(4) . . ? C12B N12D C12D 122(4) . . ? C12F N12D C12D 113(4) . . ? C12E C12D N12D 91(4) . . ? N12D C12F C12G 120(4) . . ? C13A S13 Co5 76.5(16) . . ? C13C N13A C13A 122(4) . . ? C13C N13A Co5 139(3) . . ? C13A N13A Co5 98(3) . . ? N13A C13A N13B 124(4) . . ? N13A C13A S13 112(3) . . ? N13B C13A S13 123(3) . . ? N13A C13A Co5 50(2) . . ? N13B C13A Co5 173(3) . . ? S13 C13A Co5 63.0(15) . . ? C13A N13B C13B 114(3) . . ? N13D C13B N13C 118(4) . . ? N13D C13B N13B 120(4) . . ? N13C C13B N13B 123(4) . . ? C13B N13C C13C 119(4) . . ? O13 C13C N13A 129(5) . . ? O13 C13C N13C 114(5) . . ? N13A C13C N13C 117(4) . . ? C13B N13D C13F 127(3) . . ? C13B N13D C13D 120(4) . . ? C13F N13D C13D 113(3) . . ? C13E C13D N13D 118(4) . . ? N13D C13F C13G 110(3) . . ? C14A S14 Co5 74.8(15) . . ? C14A N14A C14C 130(4) . . ? C14A N14A Co5 94(3) . . ? C14C N14A Co5 136(3) . . ? N14A C14A N14B 124(3) . . ? N14A C14A S14 117(3) . . ? N14B C14A S14 119(3) . . ? N14A C14A Co5 53(2) . . ? N14B C14A Co5 177(3) . . ? S14 C14A Co5 63.7(13) . . ? C14B N14B C14A 113(3) . . ? N14D C14B N14B 121(4) . . ? N14D C14B N14C 121(4) . . ? N14B C14B N14C 119(3) . . ? C14B N14C C14C 131(3) . . ? O14 C14C N14A 129(4) . . ? O14 C14C N14C 127(4) . . ? N14A C14C N14C 103(3) . . ? C14B N14D C14F 121(3) . . ? C14B N14D C14D 120(3) . . ? C14F N14D C14D 119(3) . . ? N14D C14D C14E 108(3) . . ? N14D C14F C14G 115(3) . . ? C15A S15 Co5 78.2(15) . . ? C15A N15A C15C 120(3) . . ? C15A N15A Co5 102(3) . . ? C15C N15A Co5 138(3) . . ? N15B C15A N15A 130(4) . . ? N15B C15A S15 122(3) . . ? N15A C15A S15 108(3) . . ? C15A N15B C15B 112(3) . . ? N15C C15B N15B 120(3) . . ? N15C C15B N15D 118(3) . . ? N15B C15B N15D 121(3) . . ? C15B N15C C15C 124(3) . . ? O15 C15C N15A 127(4) . . ? O15 C15C N15C 120(3) . . ? N15A C15C N15C 113(3) . . ? C15B N15D C15F 122(3) . . ? C15B N15D C15D 115(3) . . ? C15F N15D C15D 121(3) . . ? N15D C15D C15E 114(4) . . ? N15D C15F C15G 108(3) . . ? C16A S16 Co6 78.5(17) . . ? C16A N16A C16C 122(4) . . ? C16A N16A Co6 103(3) . . ? C16C N16A Co6 135(3) . . ? N16A C16A N16B 128(4) . . ? N16A C16A S16 108(4) . . ? N16B C16A S16 125(4) . . ? C16B N16B C16A 116(4) . . ? N16D C16B N16B 126(5) . . ? N16D C16B N16C 117(5) . . ? N16B C16B N16C 117(4) . . ? C16B N16C C16C 125(4) . . ? O16 C16C N16A 132(4) . . ? O16 C16C N16C 114(4) . . ? N16A C16C N16C 113(4) . . ? C16B N16D C16F 128(4) . . ? C16B N16D C16D 115(6) . . ? C16F N16D C16D 111(5) . . ? N16D C16D C16E 113.7(18) . . ? N16D C16F C16G 110(4) . . ? C17A S17 Co6 78.4(13) . . ? C17A N17A C17C 123(3) . . ? C17A N17A Co6 102(2) . . ? C17C N17A Co6 134(3) . . ? N17A C17A N17B 130(3) . . ? N17A C17A S17 108(3) . . ? N17B C17A S17 122(3) . . ? C17B N17B C17A 110(4) . . ? N17B C17B N17D 122(4) . . ? N17B C17B N17C 125(4) . . ? N17D C17B N17C 112(4) . . ? C17B N17C C17C 129(4) . . ? O17 C17C N17C 129(4) . . ? O17 C17C N17A 129(4) . . ? N17C C17C N17A 102(3) . . ? C17B N17D C17D 118(4) . . ? C17B N17D C17F 131(4) . . ? C17D N17D C17F 109(4) . . ? N17D C17D C17E 113.2(17) . . ? C17G C17F N17D 116(3) . . ? C18A S18 Co6 79.1(14) . . ? C18C N18A C18A 114(4) . . ? C18C N18A Co6 144(3) . . ? C18A N18A Co6 101(3) . . ? N18B C18A N18A 125(4) . . ? N18B C18A S18 127(3) . . ? N18A C18A S18 108(3) . . ? C18A N18B C18B 119(4) . . ? N18D C18B N18B 126(4) . . ? N18D C18B N18C 113(4) . . ? N18B C18B N18C 120(4) . . ? C18C N18C C18B 117(4) . . ? O18 C18C N18A 118(4) . . ? O18 C18C N18C 118(4) . . ? N18A C18C N18C 123(4) . . ? C18B N18D C18F 126(4) . . ? C18B N18D C18D 119(4) . . ? C18F N18D C18D 110(4) . . ? C18E C18D N18D 115(3) . . ? C18G C18F N18D 97(4) . . ? C19A S19 Co7 81.4(12) . . ? C19C N19A C19A 118(3) . . ? C19C N19A Co7 136(3) . . ? C19A N19A Co7 106(2) . . ? N19B C19A N19A 128(3) . . ? N19B C19A S19 131(3) . . ? N19A C19A S19 102(3) . . ? C19B N19B C19A 113(3) . . ? N19D C19B N19B 117(4) . . ? N19D C19B N19C 117(4) . . ? N19B C19B N19C 126(4) . . ? C19B N19C C19C 122(4) . . ? O19 C19C N19A 129(4) . . ? O19 C19C N19C 118(4) . . ? N19A C19C N19C 113(4) . . ? C19B N19D C19D 123(4) . . ? C19B N19D C19F 127(4) . . ? C19D N19D C19F 109(3) . . ? N19D C19D C19E 110(4) . . ? N19D C19F C19G 92(4) . . ? C20A S20 Co7 79.8(14) . . ? C20A N20A C20C 120(3) . . ? C20A N20A Co7 103(2) . . ? C20C N20A Co7 137(3) . . ? N20B C20A N20A 129(4) . . ? N20B C20A S20 125(3) . . ? N20A C20A S20 105(3) . . ? C20A N20B C20B 114(4) . . ? N20D C20B N20B 126(4) . . ? N20D C20B N20C 113(4) . . ? N20B C20B N20C 120(4) . . ? C20B N20C C20C 127(4) . . ? O20 C20C N20A 124(4) . . ? O20 C20C N20C 127(4) . . ? N20A C20C N20C 108(4) . . ? C20B N20D C20F 129(4) . . ? C20B N20D C20D 114(4) . . ? C20F N20D C20D 117(3) . . ? N20D C20D C20E 115(4) . . ? N20D C20F C20G 109(3) . . ? C21A S21 Co7 79.1(16) . . ? C21A N21A C21C 126(4) . . ? C21A N21A Co7 97(3) . . ? C21C N21A Co7 137(3) . . ? N21A C21A N21B 114(3) . . ? N21A C21A S21 113(3) . . ? N21B C21A S21 132(3) . . ? N21A C21A Co7 50(2) . . ? N21B C21A Co7 165(3) . . ? S21 C21A Co7 62.8(14) . . ? C21B N21B C21A 123(3) . . ? N21B C21B N21C 120(4) . . ? N21B C21B N21D 125(4) . . ? N21C C21B N21D 115(4) . . ? C21B N21C C21C 122(4) . . ? O21 C21C N21A 124(4) . . ? O21 C21C N21C 122(4) . . ? N21A C21C N21C 114(4) . . ? C21B N21D C21D 115(3) . . ? C21B N21D C21F 123(3) . . ? C21D N21D C21F 121(3) . . ? C21E C21D N21D 114(3) . . ? C21G C21F N21D 108(3) . . ? C22A S22 Co8 78.3(17) . . ? C22C N22A C22A 125(4) . . ? C22C N22A Co8 138(3) . . ? C22A N22A Co8 97(3) . . ? N22B C22A N22A 121(4) . . ? N22B C22A S22 127(3) . . ? N22A C22A S22 112(3) . . ? C22B N22B C22A 121(4) . . ? N22D C22B N22B 130(4) . . ? N22D C22B N22C 114(4) . . ? N22B C22B N22C 116(4) . . ? C22B N22C C22C 127(4) . . ? O22 C22C N22A 128(5) . . ? O22 C22C N22C 121(4) . . ? N22A C22C N22C 111(4) . . ? C22B N22D C22F 130(4) . . ? C22B N22D C22D 111(4) . . ? C22F N22D C22D 119(4) . . ? C22E C22D N22D 109(4) . . ? C23A S23 Co8 79.7(17) . . ? C23A N23A C23C 115(4) . . ? C23A N23A Co8 102(3) . . ? C23C N23A Co8 143(4) . . ? N23A C23A N23B 125(4) . . ? N23A C23A S23 107(3) . . ? N23B C23A S23 127(4) . . ? C23A N23B C23B 119(4) . . ? N23D C23B N23C 125(5) . . ? N23D C23B N23B 118(5) . . ? N23C C23B N23B 117(4) . . ? C23B N23C C23C 123(4) . . ? O23 C23C N23A 120(5) . . ? O23 C23C N23C 118(5) . . ? N23A C23C N23C 121(5) . . ? C23B N23D C23F 123(4) . . ? C23B N23D C23D 121(4) . . ? C23F N23D C23D 113(3) . . ? C23E C23D N23D 95(5) . . ? N22D C22F C22G 116(3) . . ? N23D C23F C23G 111(3) . . ? C24A S24 Co8 78.8(15) . . ? C24C N24A C24A 123(4) . . ? C24C N24A Co8 139(3) . . ? C24A N24A Co8 97(3) . . ? N24B C24A N24A 120(4) . . ? N24B C24A S24 128(4) . . ? N24A C24A S24 112(3) . . ? C24A N24B C24B 122(4) . . ? N24D C24B N24C 123(5) . . ? N24D C24B N24B 125(5) . . ? N24C C24B N24B 113(5) . . ? C24B N24C C24C 132(4) . . ? O24 C24C N24A 126(4) . . ? O24 C24C N24C 124(4) . . ? N24A C24C N24C 110(4) . . ? C24B N24D C24F 128(5) . . ? C24B N24D C24D 118(5) . . ? C24F N24D C24D 113(4) . . ? C24E C24D N24D 109(4) . . ? N24D C24F C24G 100(4) . . ? N1S C1S C2S 176(5) . . ? N2S C3S C4S 175(5) . . ? N3S C5S C6S 173(4) . . ? N4S C7S C8S 176(5) . . ? N5S C9S C10S 173(6) . . ? N6S C11S C12S 159(8) . . ? N7S C13S C14S 170(5) . . ? N8S C15S C16S 175(4) . . ? N9S C17S C18S 177(5) . . ? N10S C19S C20S 170(4) . . ? C22S C21S N11S 154(7) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 40.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.594 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.146 data_nidh70 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 N8 Ni S4' _chemical_formula_weight 487.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.5234(15) _cell_length_b 16.689(3) _cell_length_c 16.472(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.145(17) _cell_angle_gamma 90.00 _cell_volume 2029.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 48 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Plae-yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.595 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 5.381 _exptl_absorpt_correction_type 'Optimised numerical' _exptl_absorpt_correction_T_min 0.425 _exptl_absorpt_correction_T_max 0.769 _exptl_absorpt_process_details x-shape _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% +/-1 _diffrn_reflns_number 6005 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0513 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 70.01 _reflns_number_total 3575 _reflns_number_gt 2542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution DIRDIF _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1471P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3575 _refine_ls_number_parameters 326 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1875 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.063 _refine_ls_shift/su_mean 0.003 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_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.16230(13) 0.05668(7) 0.45831(6) 0.0333(3) Uani 0.90 1 d PD A 1 N1A N 0.2916(7) 0.0535(3) 0.5652(3) 0.0380(11) Uani 0.90 1 d PD A 1 C2A C 0.2767(8) 0.1287(4) 0.5925(4) 0.0359(13) Uani 0.90 1 d PD A 1 S2A S 0.1432(3) 0.17928(12) 0.51124(11) 0.0406(4) Uani 0.90 1 d PD A 1 N3A N 0.3516(8) 0.1558(3) 0.6667(3) 0.0374(12) Uani 0.90 1 d PD A 1 C4A C 0.4491(9) 0.0984(4) 0.7153(4) 0.0381(14) Uani 0.90 1 d PD A 1 N41A N 0.5212(8) 0.1212(4) 0.7929(3) 0.0446(13) Uani 0.90 1 d PD A 1 C42A C 0.4811(12) 0.2008(5) 0.8234(5) 0.057(2) Uani 0.90 1 d PD A 1 H42A H 0.4791 0.2403 0.7793 0.069 Uiso 0.90 1 calc PR A 1 H42B H 0.5778 0.2160 0.8697 0.069 Uiso 0.90 1 calc PR A 1 C43A C 0.3042(15) 0.2027(7) 0.8513(6) 0.080(3) Uani 0.90 1 d PD A 1 H43A H 0.2821 0.2564 0.8698 0.120 Uiso 0.90 1 calc PR A 1 H43B H 0.3073 0.1653 0.8966 0.120 Uiso 0.90 1 calc PR A 1 H43C H 0.2080 0.1878 0.8057 0.120 Uiso 0.90 1 calc PR A 1 C44A C 0.6301(10) 0.0671(5) 0.8520(4) 0.059(2) Uani 0.90 1 d PD A 1 H44A H 0.6429 0.0169 0.8251 0.071 Uiso 0.45 1 d PR A 1 H44B H 0.5696 0.0569 0.8972 0.071 Uiso 0.45 1 d PR A 1 H44C H 0.7455 0.0914 0.8728 0.071 Uiso 0.45 1 d PR A 1 H44D H 0.6512 0.0187 0.8237 0.071 Uiso 0.45 1 d PR A 1 C45A C 0.815(2) 0.1021(11) 0.8848(11) 0.069(5) Uiso 0.45 1 d PD A 1 H45A H 0.8726 0.1163 0.8389 0.104 Uiso 0.45 1 calc PR A 1 H45B H 0.8893 0.0629 0.9195 0.104 Uiso 0.45 1 calc PR A 1 H45C H 0.8030 0.1497 0.9172 0.104 Uiso 0.45 1 calc PR A 1 C46A C 0.542(3) 0.0445(13) 0.9229(11) 0.093(6) Uiso 0.45 1 d PD A 1 H46A H 0.4246 0.0210 0.9018 0.139 Uiso 0.45 1 calc PR A 1 H46B H 0.5277 0.0920 0.9550 0.139 Uiso 0.45 1 calc PR A 1 H46C H 0.6178 0.0060 0.9578 0.139 Uiso 0.45 1 calc PR A 1 N5A N 0.4809(8) 0.0231(4) 0.6918(3) 0.0371(12) Uani 0.90 1 d PD A 1 C6A C 0.3967(9) 0.0040(4) 0.6159(3) 0.0341(13) Uani 0.90 1 d PD A 1 N1B N 0.2048(6) -0.0526(3) 0.4326(3) 0.0327(11) Uani 0.90 1 d PD A 1 C2B C 0.1266(8) -0.0849(4) 0.3572(3) 0.0337(13) Uani 0.90 1 d PD A 1 S2B S -0.0061(2) -0.02450(12) 0.28388(10) 0.0444(4) Uani 0.90 1 d PD A 1 S3B S 0.0082(2) 0.08583(10) 0.33940(9) 0.0431(4) Uani 0.90 1 d PD A 1 N3B N 0.1384(7) -0.1583(3) 0.3323(3) 0.0373(12) Uani 0.90 1 d PD A 1 C4B C 0.2407(8) -0.2086(4) 0.3886(4) 0.0378(14) Uani 0.90 1 d PD A 1 N41B N 0.2504(8) -0.2846(3) 0.3686(3) 0.0422(13) Uani 0.90 1 d PD A 1 C42B C 0.1346(9) -0.3168(4) 0.2935(4) 0.0448(16) Uani 0.90 1 d PD A 1 H42C H 0.1921 -0.3643 0.2749 0.054 Uiso 0.90 1 calc PR A 1 H42D H 0.1210 -0.2766 0.2494 0.054 Uiso 0.90 1 calc PR A 1 C43B C -0.0507(9) -0.3392(6) 0.3100(5) 0.056(2) Uani 0.90 1 d PD A 1 H43D H -0.1243 -0.3609 0.2599 0.084 Uiso 0.90 1 calc PR A 1 H43E H -0.1089 -0.2919 0.3270 0.084 Uiso 0.90 1 calc PR A 1 H43F H -0.0373 -0.3791 0.3535 0.084 Uiso 0.90 1 calc PR A 1 C44B C 0.3556(11) -0.3427(5) 0.4255(5) 0.0516(17) Uani 0.90 1 d PD A 1 H44E H 0.2849 -0.3918 0.4266 0.062 Uiso 0.90 1 calc PR A 1 H44F H 0.3822 -0.3204 0.4816 0.062 Uiso 0.90 1 calc PR A 1 C45B C 0.5337(11) -0.3621(6) 0.3969(5) 0.063(2) Uani 0.90 1 d PD A 1 H45D H 0.6028 -0.4004 0.4347 0.095 Uiso 0.90 1 calc PR A 1 H45E H 0.6037 -0.3134 0.3963 0.095 Uiso 0.90 1 calc PR A 1 H45F H 0.5068 -0.3849 0.3417 0.095 Uiso 0.90 1 calc PR A 1 N5B N 0.3314(7) -0.1819(3) 0.4633(3) 0.0348(11) Uani 0.90 1 d PD A 1 C6B C 0.3070(8) -0.1088(4) 0.4823(3) 0.0333(13) Uani 0.90 1 d PD A 1 S6AB S 0.4368(3) -0.09292(12) 0.58303(11) 0.0349(4) Uani 0.90 1 d PD A 1 Ni2 Ni 0.153(2) 0.0189(8) 0.4357(8) 0.071(5) Uiso 0.10 1 d PD B 2 N1C N 0.236(8) -0.0849(15) 0.436(2) 0.114(7) Uiso 0.10 1 d PD B 2 C2C C 0.150(11) -0.1139(18) 0.363(3) 0.114(7) Uiso 0.10 1 d PD B 2 S2C S 0.033(5) -0.0334(14) 0.3120(13) 0.114(7) Uiso 0.10 1 d PD B 2 N3C N 0.157(13) -0.1888(18) 0.338(3) 0.114(7) Uiso 0.10 1 d PD B 2 C4C C 0.245(11) -0.2381(14) 0.399(3) 0.114(7) Uiso 0.10 1 d PD B 2 N41C N 0.260(11) -0.3150(15) 0.377(3) 0.114(7) Uiso 0.10 1 d PD B 2 C42C C 0.160(12) -0.345(3) 0.296(4) 0.114(7) Uiso 0.10 1 d PD B 2 H42E H 0.1712 -0.4030 0.2947 0.137 Uiso 0.10 1 calc PR B 2 H42F H 0.2156 -0.3224 0.2520 0.137 Uiso 0.10 1 calc PR B 2 C43C C -0.035(10) -0.322(9) 0.281(6) 0.114(7) Uiso 0.10 1 d PD B 2 H43D H -0.0909 -0.3360 0.2248 0.172 Uiso 0.10 1 calc PR B 2 H43E H -0.0465 -0.2652 0.2896 0.172 Uiso 0.10 1 calc PR B 2 H43F H -0.0948 -0.3514 0.3193 0.172 Uiso 0.10 1 calc PR B 2 C44C C 0.386(13) -0.370(3) 0.427(4) 0.114(7) Uiso 0.10 1 d PD B 2 H44G H 0.3194 -0.4164 0.4419 0.137 Uiso 0.10 1 calc PR B 2 H44H H 0.4449 -0.3433 0.4777 0.137 Uiso 0.10 1 calc PR B 2 C45C C 0.528(13) -0.398(7) 0.380(8) 0.114(7) Uiso 0.10 1 d PD B 2 H45D H 0.6064 -0.4373 0.4129 0.172 Uiso 0.10 1 calc PR B 2 H45E H 0.6003 -0.3531 0.3683 0.172 Uiso 0.10 1 calc PR B 2 H45F H 0.4699 -0.4229 0.3281 0.172 Uiso 0.10 1 calc PR B 2 N5C N 0.334(13) -0.2150(14) 0.474(3) 0.114(7) Uiso 0.10 1 d PD B 2 C6C C 0.333(8) -0.1367(15) 0.487(2) 0.114(7) Uiso 0.10 1 d PD B 2 N1D N 0.268(9) 0.0431(17) 0.5471(18) 0.114(7) Uiso 0.10 1 d PD B 2 C2D C 0.260(11) 0.119(2) 0.579(2) 0.114(7) Uiso 0.10 1 d PD B 2 S2D S 0.140(7) 0.1930(14) 0.5169(19) 0.114(7) Uiso 0.10 1 d PD B 2 S3D S 0.046(4) 0.1357(10) 0.4070(13) 0.114(7) Uiso 0.10 1 d PD B 2 N3D N 0.347(15) 0.147(2) 0.649(3) 0.114(7) Uiso 0.10 1 d PD B 2 C4D C 0.444(14) 0.091(3) 0.701(3) 0.114(7) Uiso 0.10 1 d PD B 2 N41D N 0.516(9) 0.113(3) 0.776(2) 0.114(7) Uiso 0.10 1 d PD B 2 C42D C 0.464(12) 0.189(3) 0.810(3) 0.114(7) Uiso 0.10 1 d PD B 2 H42G H 0.3988 0.2224 0.7647 0.137 Uiso 0.10 1 calc PR B 2 H42H H 0.5731 0.2183 0.8363 0.137 Uiso 0.10 1 calc PR B 2 C43D C 0.344(19) 0.175(8) 0.873(7) 0.114(7) Uiso 0.10 1 d PD B 2 H43G H 0.3423 0.2227 0.9062 0.172 Uiso 0.10 1 calc PR B 2 H43H H 0.3920 0.1304 0.9084 0.172 Uiso 0.10 1 calc PR B 2 H43I H 0.2223 0.1625 0.8444 0.172 Uiso 0.10 1 calc PR B 2 C44D C 0.674(11) 0.072(4) 0.825(4) 0.114(7) Uiso 0.10 1 d PD B 2 H44I H 0.7253 0.0349 0.7890 0.137 Uiso 0.10 1 calc PR B 2 H44J H 0.6368 0.0400 0.8689 0.137 Uiso 0.10 1 calc PR B 2 C45D C 0.818(9) 0.133(6) 0.863(7) 0.114(7) Uiso 0.10 1 d PD B 2 H45G H 0.9069 0.1079 0.9056 0.172 Uiso 0.10 1 calc PR B 2 H45H H 0.7598 0.1768 0.8873 0.172 Uiso 0.10 1 calc PR B 2 H45I H 0.8770 0.1546 0.8203 0.172 Uiso 0.10 1 calc PR B 2 N5D N 0.464(15) 0.014(3) 0.675(3) 0.114(7) Uiso 0.10 1 d PD B 2 C6D C 0.381(14) -0.005(3) 0.602(3) 0.114(7) Uiso 0.10 1 d PD B 2 S6CD S 0.448(6) -0.1046(18) 0.5847(19) 0.114(7) Uiso 0.10 1 d PD B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0218(6) 0.0458(7) 0.0308(5) 0.0004(5) 0.0016(4) -0.0006(4) N1A 0.032(3) 0.049(3) 0.033(2) 0.003(2) 0.006(2) -0.002(2) C2A 0.020(3) 0.052(4) 0.035(3) -0.003(3) 0.006(2) -0.002(3) S2A 0.0327(8) 0.0483(10) 0.0392(8) 0.0025(7) 0.0026(6) 0.0024(7) N3A 0.027(3) 0.047(3) 0.039(3) -0.001(2) 0.008(2) -0.003(2) C4A 0.026(3) 0.055(4) 0.033(3) -0.003(3) 0.007(2) -0.004(3) N41A 0.033(3) 0.059(4) 0.038(3) -0.008(2) -0.002(2) 0.001(2) C42A 0.060(5) 0.064(5) 0.042(4) -0.020(3) -0.004(3) 0.000(4) C43A 0.081(7) 0.090(8) 0.071(6) -0.026(5) 0.018(5) 0.021(5) C44A 0.053(5) 0.081(6) 0.037(4) -0.011(4) -0.006(3) 0.010(4) N5A 0.023(3) 0.057(3) 0.030(2) -0.006(2) 0.001(2) -0.001(2) C6A 0.020(3) 0.055(4) 0.027(3) -0.002(2) 0.002(2) -0.003(2) N1B 0.019(2) 0.047(3) 0.031(2) -0.005(2) 0.0014(18) -0.003(2) C2B 0.020(3) 0.053(4) 0.028(3) 0.000(2) 0.004(2) -0.006(3) S2B 0.0332(9) 0.0584(11) 0.0372(8) 0.0017(7) -0.0045(7) -0.0005(7) S3B 0.0341(9) 0.0526(10) 0.0380(8) 0.0054(7) -0.0042(6) 0.0017(7) N3B 0.021(3) 0.054(3) 0.036(3) -0.005(2) 0.004(2) 0.000(2) C4B 0.019(3) 0.054(4) 0.039(3) -0.003(3) 0.004(2) -0.002(3) N41B 0.030(3) 0.053(3) 0.042(3) -0.015(3) 0.004(2) -0.001(3) C42B 0.037(4) 0.048(4) 0.047(4) -0.012(3) 0.003(3) 0.005(3) C43B 0.030(4) 0.081(6) 0.054(4) -0.018(4) 0.003(3) -0.004(3) C44B 0.050(4) 0.048(4) 0.054(4) -0.005(3) 0.004(3) 0.008(3) C45B 0.043(4) 0.080(6) 0.065(5) -0.010(4) 0.004(4) 0.014(4) N5B 0.016(2) 0.056(3) 0.030(2) -0.003(2) -0.0015(18) 0.001(2) C6B 0.017(3) 0.050(4) 0.035(3) -0.003(3) 0.010(2) -0.003(2) S6AB 0.0209(7) 0.0491(9) 0.0327(7) -0.0022(6) -0.0002(5) 0.0020(6) _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 Ni1 N1A 1.841(5) . ? Ni1 N1B 1.913(5) . ? Ni1 S3B 2.1307(18) . ? Ni1 S2A 2.240(2) . ? Ni1 C2A 2.518(6) . ? N1A C6A 1.323(8) . ? N1A C2A 1.345(8) . ? C2A N3A 1.323(7) . ? C2A S2A 1.730(6) . ? N3A C4A 1.367(8) . ? C4A N41A 1.344(7) . ? C4A N5A 1.350(8) . ? N41A C44A 1.459(9) . ? N41A C42A 1.473(9) . ? C42A C43A 1.489(12) . ? C44A C46A 1.496(16) . ? C44A C45A 1.512(16) . ? N5A C6A 1.325(7) . ? C6A S6AB 1.751(7) . ? N1B C6B 1.378(8) . ? N1B C2B 1.378(7) . ? C2B N3B 1.300(8) . ? C2B S2B 1.733(6) . ? S2B S3B 2.049(3) . ? N3B C4B 1.372(8) . ? C4B N41B 1.316(8) . ? C4B N5B 1.362(7) . ? N41B C44B 1.469(9) . ? N41B C42B 1.470(8) . ? C42B C43B 1.517(10) . ? C44B C45B 1.538(10) . ? N5B C6B 1.282(8) . ? C6B S6AB 1.775(6) . ? Ni2 N1C 1.840(7) . ? Ni2 N1D 1.914(7) . ? Ni2 S3D 2.130(5) . ? Ni2 S2C 2.241(5) . ? Ni2 C2C 2.517(7) . ? N1C C6C 1.323(9) . ? N1C C2C 1.346(9) . ? C2C N3C 1.322(9) . ? C2C S2C 1.730(8) . ? N3C C4C 1.367(9) . ? C4C N41C 1.344(9) . ? C4C N5C 1.351(10) . ? N41C C44C 1.459(10) . ? N41C C42C 1.473(10) . ? C42C C43C 1.490(13) . ? C44C C45C 1.512(17) . ? N5C C6C 1.325(8) . ? C6C S6CD 1.751(8) . ? N1D C6D 1.378(9) . ? N1D C2D 1.379(8) . ? C2D N3D 1.301(10) . ? C2D S2D 1.733(8) . ? S2D S3D 2.049(5) . ? N3D C4D 1.372(9) . ? C4D N41D 1.316(10) . ? C4D N5D 1.361(9) . ? N41D C44D 1.470(10) . ? N41D C42D 1.470(9) . ? C42D C43D 1.517(11) . ? C44D C45D 1.539(12) . ? N5D C6D 1.282(9) . ? C6D S6CD 1.775(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Ni1 N1B 96.0(2) . . ? N1A Ni1 S3B 168.27(19) . . ? N1B Ni1 S3B 95.68(15) . . ? N1A Ni1 S2A 73.47(18) . . ? N1B Ni1 S2A 169.46(15) . . ? S3B Ni1 S2A 94.86(8) . . ? N1A Ni1 C2A 31.3(2) . . ? N1B Ni1 C2A 127.3(2) . . ? S3B Ni1 C2A 136.98(17) . . ? S2A Ni1 C2A 42.15(15) . . ? C6A N1A C2A 116.7(5) . . ? C6A N1A Ni1 139.7(5) . . ? C2A N1A Ni1 103.3(4) . . ? N3A C2A N1A 125.4(6) . . ? N3A C2A S2A 129.0(5) . . ? N1A C2A S2A 105.7(4) . . ? N3A C2A Ni1 170.7(5) . . ? N1A C2A Ni1 45.4(3) . . ? S2A C2A Ni1 60.30(19) . . ? C2A S2A Ni1 77.5(2) . . ? C2A N3A C4A 112.7(5) . . ? N41A C4A N5A 118.4(6) . . ? N41A C4A N3A 115.5(6) . . ? N5A C4A N3A 126.1(5) . . ? C4A N41A C44A 122.1(6) . . ? C4A N41A C42A 120.6(6) . . ? C44A N41A C42A 117.2(5) . . ? N41A C42A C43A 112.2(7) . . ? N41A C44A C46A 113.7(9) . . ? N41A C44A C45A 111.0(9) . . ? C46A C44A C45A 109.5(12) . . ? C6A N5A C4A 114.5(5) . . ? N1A C6A N5A 124.3(6) . . ? N1A C6A S6AB 120.0(4) . . ? N5A C6A S6AB 115.7(5) . . ? C6B N1B C2B 111.2(5) . . ? C6B N1B Ni1 128.0(4) . . ? C2B N1B Ni1 120.8(4) . . ? N3B C2B N1B 127.6(6) . . ? N3B C2B S2B 113.1(4) . . ? N1B C2B S2B 119.3(5) . . ? C2B S2B S3B 103.8(2) . . ? S2B S3B Ni1 100.21(9) . . ? C2B N3B C4B 115.3(5) . . ? N41B C4B N5B 120.0(6) . . ? N41B C4B N3B 118.2(5) . . ? N5B C4B N3B 121.9(6) . . ? C4B N41B C44B 121.7(5) . . ? C4B N41B C42B 120.7(5) . . ? C44B N41B C42B 117.0(6) . . ? N41B C42B C43B 110.9(5) . . ? N41B C44B C45B 109.7(6) . . ? C6B N5B C4B 117.5(5) . . ? N5B C6B N1B 126.4(5) . . ? N5B C6B S6AB 107.0(4) . . ? N1B C6B S6AB 126.6(5) . . ? C6A S6AB C6B 109.3(3) . . ? N1C Ni2 N1D 96.1(4) . . ? N1C Ni2 S3D 167.6(9) . . ? N1D Ni2 S3D 95.8(3) . . ? N1C Ni2 S2C 73.4(3) . . ? N1D Ni2 S2C 169.3(6) . . ? S3D Ni2 S2C 94.8(3) . . ? N1C Ni2 C2C 31.4(3) . . ? N1D Ni2 C2C 127.2(4) . . ? S3D Ni2 C2C 137.0(3) . . ? S2C Ni2 C2C 42.2(2) . . ? C6C N1C C2C 116.7(8) . . ? C6C N1C Ni2 139.5(9) . . ? C2C N1C Ni2 103.2(5) . . ? N3C C2C N1C 125.3(9) . . ? N3C C2C S2C 129.1(8) . . ? N1C C2C S2C 105.6(6) . . ? N3C C2C Ni2 170(2) . . ? N1C C2C Ni2 45.4(4) . . ? S2C C2C Ni2 60.4(3) . . ? C2C S2C Ni2 77.5(3) . . ? C2C N3C C4C 112.4(9) . . ? N41C C4C N5C 118.0(10) . . ? N41C C4C N3C 115.4(10) . . ? N5C C4C N3C 126.2(9) . . ? C4C N41C C44C 121.9(10) . . ? C4C N41C C42C 120.6(10) . . ? C44C N41C C42C 117.2(9) . . ? N41C C42C C43C 112.3(11) . . ? N41C C44C C45C 111.0(12) . . ? C6C N5C C4C 114.4(8) . . ? N1C C6C N5C 124.1(11) . . ? N1C C6C S6CD 119.9(7) . . ? N5C C6C S6CD 115.6(9) . . ? C6D N1D C2D 110.9(8) . . ? C6D N1D Ni2 128.0(7) . . ? C2D N1D Ni2 120.7(6) . . ? N3D C2D N1D 127.5(10) . . ? N3D C2D S2D 112.8(8) . . ? N1D C2D S2D 119.4(7) . . ? C2D S2D S3D 103.8(4) . . ? S2D S3D Ni2 100.3(3) . . ? C2D N3D C4D 115.4(10) . . ? N41D C4D N5D 120.3(10) . . ? N41D C4D N3D 118.1(9) . . ? N5D C4D N3D 121.6(9) . . ? C4D N41D C44D 121.7(11) . . ? C4D N41D C42D 120.5(10) . . ? C44D N41D C42D 116.7(10) . . ? N41D C42D C43D 110.8(10) . . ? N41D C44D C45D 109.7(10) . . ? C6D N5D C4D 117.6(9) . . ? N5D C6D N1D 126.5(8) . . ? N5D C6D S6CD 106.8(8) . . ? N1D C6D S6CD 126.6(7) . . ? C6C S6CD C6D 109.3(6) . . ? _diffrn_measured_fraction_theta_max 0.929 _diffrn_reflns_theta_full 70.01 _diffrn_measured_fraction_theta_full 0.929 _refine_diff_density_max 1.148 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.130 data_s2dh45 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 N4 S2' _chemical_formula_weight 216.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.030(2) _cell_length_b 13.949(4) _cell_length_c 9.394(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.079(13) _cell_angle_gamma 90.00 _cell_volume 1104.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 4.083 _exptl_absorpt_correction_type Shelxa _exptl_absorpt_correction_T_min 0.054 _exptl_absorpt_correction_T_max 0.483 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2950 _diffrn_reflns_av_R_equivalents 0.0150 _diffrn_reflns_av_sigmaI/netI 0.0232 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 5.25 _diffrn_reflns_theta_max 69.99 _reflns_number_total 1925 _reflns_number_gt 1568 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1783P)^2^+2.4654P] 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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1925 _refine_ls_number_parameters 116 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.1113 _refine_ls_R_factor_gt 0.0989 _refine_ls_wR_factor_ref 0.3011 _refine_ls_wR_factor_gt 0.2872 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.024 _refine_ls_shift/su_mean 0.003 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 0.5821(5) 0.1382(4) -0.0186(5) 0.0477(12) Uani 1 1 d . . . H1 H 0.5190 0.0921 -0.0623 0.057 Uiso 1 1 calc R . . C2 C 0.5695(7) 0.2187(5) -0.0984(6) 0.0516(15) Uani 1 1 d . . . S2 S 0.4359(2) 0.23575(16) -0.27142(19) 0.0744(8) Uani 1 1 d . . . N3 N 0.6755(6) 0.2893(4) -0.0222(5) 0.0562(14) Uani 1 1 d . . . H3 H 0.6719 0.3443 -0.0647 0.067 Uiso 1 1 calc R . . C4 C 0.7864(8) 0.2732(5) 0.1201(7) 0.0611(17) Uani 1 1 d . A . N41 N 0.8886(8) 0.3420(4) 0.1860(6) 0.087(2) Uani 1 1 d DU . . C42 C 1.0413(12) 0.3149(8) 0.3179(10) 0.064(3) Uiso 0.640(17) 1 d PDU A 1 H42A H 1.0428 0.2467 0.3382 0.077 Uiso 0.640(17) 1 calc PR A 1 H42B H 1.1333 0.3306 0.2923 0.077 Uiso 0.640(17) 1 calc PR A 1 C43 C 1.0440(17) 0.3703(11) 0.4544(14) 0.094(5) Uiso 0.640(17) 1 d PDU A 1 H43A H 1.1383 0.3546 0.5394 0.141 Uiso 0.640(17) 1 calc PR A 1 H43B H 0.9522 0.3543 0.4784 0.141 Uiso 0.640(17) 1 calc PR A 1 H43C H 1.0433 0.4377 0.4333 0.141 Uiso 0.640(17) 1 calc PR A 1 C44 C 0.9052(18) 0.4320(9) 0.1063(16) 0.085(4) Uiso 0.640(17) 1 d PDU A 1 H44A H 1.0109 0.4586 0.1533 0.102 Uiso 0.640(17) 1 calc PR A 1 H44B H 0.8857 0.4195 -0.0005 0.102 Uiso 0.640(17) 1 calc PR A 1 C45 C 0.783(2) 0.4992(10) 0.123(2) 0.110(6) Uiso 0.640(17) 1 d PDU A 1 H45A H 0.7903 0.5596 0.0767 0.165 Uiso 0.640(17) 1 calc PR A 1 H45B H 0.8020 0.5087 0.2292 0.165 Uiso 0.640(17) 1 calc PR A 1 H45C H 0.6794 0.4725 0.0733 0.165 Uiso 0.640(17) 1 calc PR A 1 C42' C 0.965(2) 0.3422(15) 0.3595(12) 0.072(6) Uiso 0.360(17) 1 d PDU A 2 H42C H 0.9793 0.4071 0.3991 0.087 Uiso 0.360(17) 1 calc PR A 2 H42D H 0.9004 0.3069 0.4049 0.087 Uiso 0.360(17) 1 calc PR A 2 C43' C 1.121(3) 0.294(2) 0.391(3) 0.112(10) Uiso 0.360(17) 1 d PDU A 2 H43D H 1.1774 0.2909 0.4989 0.168 Uiso 0.360(17) 1 calc PR A 2 H43E H 1.1820 0.3298 0.3440 0.168 Uiso 0.360(17) 1 calc PR A 2 H43F H 1.1036 0.2303 0.3495 0.168 Uiso 0.360(17) 1 calc PR A 2 C44' C 0.8611(19) 0.4459(8) 0.1283(16) 0.042(4) Uiso 0.360(17) 1 d PDU A 2 H44C H 0.9575 0.4826 0.1763 0.050 Uiso 0.360(17) 1 calc PR A 2 H44D H 0.8371 0.4466 0.0190 0.050 Uiso 0.360(17) 1 calc PR A 2 C45' C 0.729(3) 0.4917(15) 0.162(3) 0.093(8) Uiso 0.360(17) 1 d PDU A 2 H45D H 0.7152 0.5561 0.1232 0.139 Uiso 0.360(17) 1 calc PR A 2 H45E H 0.7541 0.4928 0.2700 0.139 Uiso 0.360(17) 1 calc PR A 2 H45F H 0.6335 0.4559 0.1136 0.139 Uiso 0.360(17) 1 calc PR A 2 N5 N 0.7932(6) 0.1906(4) 0.1947(5) 0.0527(13) Uani 1 1 d . . . C6 C 0.6866(6) 0.1223(5) 0.1267(6) 0.0480(14) Uani 1 1 d . A . S6 S 0.67608(19) 0.02117(11) 0.21665(18) 0.0608(7) 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 N1 0.049(2) 0.049(3) 0.052(2) -0.003(2) 0.026(2) -0.007(2) C2 0.044(3) 0.067(4) 0.052(3) -0.006(3) 0.028(2) -0.013(3) S2 0.0685(12) 0.0862(15) 0.0604(11) 0.0145(9) 0.0135(8) -0.0302(9) N3 0.061(3) 0.060(3) 0.053(3) 0.003(2) 0.027(2) -0.020(2) C4 0.063(4) 0.075(5) 0.052(3) -0.005(3) 0.029(3) -0.024(3) N41 0.099(5) 0.086(5) 0.061(3) 0.011(3) 0.010(3) -0.058(4) N5 0.054(3) 0.058(3) 0.051(2) 0.001(2) 0.024(2) -0.013(2) C6 0.043(3) 0.055(4) 0.054(3) -0.009(3) 0.027(2) -0.004(2) S6 0.0662(11) 0.0446(11) 0.0649(10) -0.0008(7) 0.0153(8) -0.0027(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C2 1.332(8) . ? N1 C6 1.370(7) . ? C2 N3 1.380(8) . ? C2 S2 1.656(6) . ? N3 C4 1.370(8) . ? C4 N41 1.321(8) . ? C4 N5 1.339(9) . ? N41 C44 1.497(9) . ? N41 C42' 1.524(10) . ? N41 C42 1.533(8) . ? N41 C44' 1.536(9) . ? C42 C43 1.489(13) . ? C44 C45 1.496(14) . ? C42' C43' 1.492(14) . ? C44' C45' 1.479(14) . ? N5 C6 1.342(7) . ? C6 S6 1.664(6) . ? 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 C2 N1 C6 125.9(5) . . ? N1 C2 N3 114.0(5) . . ? N1 C2 S2 123.9(4) . . ? N3 C2 S2 122.1(5) . . ? C4 N3 C2 121.1(6) . . ? N41 C4 N5 119.1(6) . . ? N41 C4 N3 118.8(6) . . ? N5 C4 N3 122.1(6) . . ? C4 N41 C44 123.6(7) . . ? C4 N41 C42' 118.3(10) . . ? C44 N41 C42' 116.5(11) . . ? C4 N41 C42 118.3(7) . . ? C44 N41 C42 112.9(8) . . ? C42' N41 C42 37.5(7) . . ? C4 N41 C44' 121.5(7) . . ? C44 N41 C44' 20.7(6) . . ? C42' N41 C44' 109.2(9) . . ? C42 N41 C44' 120.1(8) . . ? C43 C42 N41 107.4(8) . . ? C45 C44 N41 105.3(10) . . ? C43' C42' N41 103.9(11) . . ? C45' C44' N41 111.9(11) . . ? C4 N5 C6 118.2(5) . . ? N5 C6 N1 118.5(5) . . ? N5 C6 S6 121.5(4) . . ? N1 C6 S6 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.920 _diffrn_reflns_theta_full 69.99 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 0.557 _refine_diff_density_min -0.588 _refine_diff_density_rms 0.114 data_sodh43 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C7 H12 N4 O S' _chemical_formula_weight 200.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.789(3) _cell_length_b 7.043(2) _cell_length_c 17.452(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.36(4) _cell_angle_gamma 90.00 _cell_volume 955.7(7) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 32 _cell_measurement_theta_min 20 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 424 _exptl_absorpt_coefficient_mu 2.764 _exptl_absorpt_correction_type Psi-scans _exptl_absorpt_correction_T_min 0.101 _exptl_absorpt_correction_T_max 0.319 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method Omega-theta _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 2683 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 5.08 _diffrn_reflns_theta_max 70.13 _reflns_number_total 1647 _reflns_number_gt 1446 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe DIF4' _computing_cell_refinement 'Stoe DIF4' _computing_data_reduction 'Stoe REDU4' _computing_structure_solution SHELXS-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics SHELXTL _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1475P)^2^+1.3044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geometric _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0031(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1647 _refine_ls_number_parameters 156 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0817 _refine_ls_R_factor_gt 0.0758 _refine_ls_wR_factor_ref 0.2224 _refine_ls_wR_factor_gt 0.2155 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.7391(4) -0.1266(5) 0.52369(17) 0.0325(8) Uani 1 d . . . H1 H 0.6423 -0.1237 0.4962 0.039 Uiso 1 calc R . . C2 C 0.8484(5) -0.2747(5) 0.5136(2) 0.0306(9) Uani 1 d . . . O2 O 0.8152(4) -0.4001(4) 0.46729(17) 0.0432(8) Uani 1 d . . . N3 N 0.9973(4) -0.2693(5) 0.55879(19) 0.0351(8) Uani 1 d . . . H3 H 1.0719 -0.3604 0.5553 0.042 Uiso 1 calc R . . C4 C 1.0322(5) -0.1244(6) 0.6095(2) 0.0411(10) Uani 1 d . . . N41 N 1.1770(6) -0.1272(6) 0.6525(3) 0.0713(16) Uani 1 d D . . C42 C 1.3292(9) -0.2536(10) 0.6367(5) 0.047(2) Uani 0.620(10) d PD A 1 H42A H 1.3220 -0.2963 0.5832 0.056 Uiso 0.620(10) calc PR A 1 H42B H 1.4376 -0.1847 0.6466 0.056 Uiso 0.620(10) calc PR A 1 C43 C 1.3198(12) -0.4199(13) 0.6901(4) 0.058(2) Uani 0.620(10) d PD A 1 H43A H 1.4150 -0.5053 0.6825 0.086 Uiso 0.620(10) calc PR A 1 H43B H 1.2121 -0.4866 0.6795 0.086 Uiso 0.620(10) calc PR A 1 H43C H 1.3262 -0.3752 0.7428 0.086 Uiso 0.620(10) calc PR A 1 C44 C 1.2392(8) 0.0561(10) 0.6907(4) 0.0372(18) Uani 0.620(10) d PD A 1 H44A H 1.3650 0.0578 0.6977 0.045 Uiso 0.620(10) calc PR A 1 H44B H 1.2014 0.1665 0.6600 0.045 Uiso 0.620(10) calc PR A 1 C45 C 1.1588(11) 0.0563(15) 0.7669(4) 0.057(2) Uani 0.620(10) d PD A 1 H45A H 1.1931 0.1700 0.7952 0.085 Uiso 0.620(10) calc PR A 1 H45B H 1.1967 -0.0548 0.7961 0.085 Uiso 0.620(10) calc PR A 1 H45C H 1.0345 0.0537 0.7587 0.085 Uiso 0.620(10) calc PR A 1 C42' C 1.2659(13) -0.3166(13) 0.6740(6) 0.041(3) Uani 0.380(10) d PD A 2 H42C H 1.2899 -0.3255 0.7297 0.049 Uiso 0.380(10) calc PR A 2 H42D H 1.1933 -0.4242 0.6571 0.049 Uiso 0.380(10) calc PR A 2 C43' C 1.4305(14) -0.3157(19) 0.6330(8) 0.053(4) Uani 0.380(10) d PD A 2 H43D H 1.4926 -0.4330 0.6438 0.080 Uiso 0.380(10) calc PR A 2 H43E H 1.5007 -0.2088 0.6506 0.080 Uiso 0.380(10) calc PR A 2 H43F H 1.4042 -0.3047 0.5782 0.080 Uiso 0.380(10) calc PR A 2 C44' C 1.1738(16) -0.0239(15) 0.7314(6) 0.053(4) Uani 0.380(10) d PD A 2 H44C H 1.0564 -0.0177 0.7487 0.063 Uiso 0.380(10) calc PR A 2 H44D H 1.2472 -0.0897 0.7705 0.063 Uiso 0.380(10) calc PR A 2 C45' C 1.2417(19) 0.1715(16) 0.7167(9) 0.056(4) Uani 0.380(10) d PD A 2 H45D H 1.2421 0.2457 0.7636 0.085 Uiso 0.380(10) calc PR A 2 H45E H 1.1688 0.2329 0.6771 0.085 Uiso 0.380(10) calc PR A 2 H45F H 1.3579 0.1621 0.7000 0.085 Uiso 0.380(10) calc PR A 2 N5 N 0.9239(4) 0.0200(5) 0.6166(2) 0.0431(10) Uani 1 d . . . C6 C 0.7740(5) 0.0185(5) 0.5751(2) 0.0300(9) Uani 1 d . . . S6 S 0.62747(12) 0.19166(15) 0.58195(6) 0.0404(5) Uani 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 N1 0.0318(15) 0.0255(19) 0.0393(16) -0.0100(14) -0.0056(12) 0.0104(13) C2 0.0364(18) 0.019(2) 0.0354(18) -0.0064(16) -0.0024(14) 0.0092(15) O2 0.0442(15) 0.0300(17) 0.0533(17) -0.0219(14) -0.0148(12) 0.0163(12) N3 0.0359(16) 0.0236(18) 0.0446(18) -0.0102(15) -0.0072(13) 0.0134(13) C4 0.043(2) 0.026(2) 0.052(2) -0.0119(19) -0.0121(17) 0.0099(17) N41 0.059(2) 0.049(3) 0.100(3) -0.050(3) -0.044(2) 0.033(2) C42 0.035(4) 0.036(5) 0.068(5) -0.016(4) -0.013(3) 0.008(4) C43 0.064(5) 0.061(6) 0.048(4) -0.006(4) -0.004(4) 0.027(5) C44 0.035(3) 0.032(5) 0.044(4) -0.007(4) -0.001(3) 0.001(3) C45 0.065(5) 0.056(6) 0.048(4) -0.001(4) -0.002(4) 0.013(5) C42' 0.039(6) 0.035(8) 0.046(7) -0.010(6) -0.021(5) 0.021(5) C43' 0.033(6) 0.045(8) 0.082(9) 0.000(7) -0.001(6) 0.006(6) C44' 0.054(7) 0.029(8) 0.071(10) -0.027(7) -0.028(7) 0.021(6) C45' 0.066(8) 0.032(8) 0.070(9) -0.010(7) -0.003(7) 0.004(6) N5 0.0466(19) 0.0231(19) 0.057(2) -0.0193(16) -0.0199(16) 0.0164(15) C6 0.0338(17) 0.019(2) 0.0361(18) -0.0051(16) -0.0041(13) 0.0078(14) S6 0.0414(6) 0.0283(7) 0.0499(7) -0.0183(4) -0.0114(4) 0.0170(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 N1 C2 1.364(5) . ? N1 C6 1.377(5) . ? C2 O2 1.215(5) . ? C2 N3 1.365(5) . ? N3 C4 1.368(5) . ? C4 N41 1.318(6) . ? C4 N5 1.332(5) . ? N41 C44 1.519(7) . ? N41 C42 1.521(7) . ? N41 C42' 1.540(8) . ? N41 C44' 1.559(8) . ? C42 C43 1.501(9) . ? C44 C45 1.503(8) . ? C42' C43' 1.504(9) . ? C44' C45' 1.502(10) . ? N5 C6 1.337(5) . ? C6 S6 1.679(4) . ? 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 C2 N1 C6 123.4(3) . . ? O2 C2 N1 122.1(3) . . ? O2 C2 N3 123.0(3) . . ? N1 C2 N3 114.9(3) . . ? C2 N3 C4 121.6(3) . . ? N41 C4 N5 118.9(4) . . ? N41 C4 N3 119.3(4) . . ? N5 C4 N3 121.8(3) . . ? C4 N41 C44 118.5(4) . . ? C4 N41 C42 123.7(4) . . ? C44 N41 C42 110.2(4) . . ? C4 N41 C42' 120.6(5) . . ? C44 N41 C42' 120.1(5) . . ? C42 N41 C42' 36.1(5) . . ? C4 N41 C44' 116.1(5) . . ? C44 N41 C44' 40.3(5) . . ? C42 N41 C44' 119.1(6) . . ? C42' N41 C44' 102.7(6) . . ? C43 C42 N41 106.1(6) . . ? C45 C44 N41 104.5(6) . . ? C43' C42' N41 105.3(8) . . ? C45' C44' N41 104.6(9) . . ? C4 N5 C6 118.8(3) . . ? N5 C6 N1 119.4(3) . . ? N5 C6 S6 122.1(3) . . ? N1 C6 S6 118.4(3) . . ? _diffrn_measured_fraction_theta_max 0.831 _diffrn_reflns_theta_full 70.13 _diffrn_measured_fraction_theta_full 0.831 _refine_diff_density_max 0.552 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.105 data_codh77 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Co(ii)4Co(iii)2NaO(LS)7(L2S)2(OBz)2(H2O)2].8MeCN _chemical_formula_sum 'C107 H155 Co6 N52 Na O18 S9' _chemical_formula_weight 3122.94 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' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.6882(8) _cell_length_b 19.7229(8) _cell_length_c 39.7227(18) _cell_angle_alpha 90.00 _cell_angle_beta 94.844(2) _cell_angle_gamma 90.00 _cell_volume 15369.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description flake _exptl_crystal_colour Blue _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.025 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6488 _exptl_absorpt_coefficient_mu 0.830 _exptl_absorpt_correction_type Sortav _exptl_absorpt_correction_T_min 0.994 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details ? _exptl_special_details ; Data collected at Southampton by Simon Coles. Only data to 45deg used. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Kappa-CCD _diffrn_measurement_method Omega-phi _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 124909 _diffrn_reflns_av_R_equivalents 0.3291 _diffrn_reflns_av_sigmaI/netI 0.3609 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 22.50 _reflns_number_total 19775 _reflns_number_gt 6930 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometric; NH and OH based on H-bonding' _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19775 _refine_ls_number_parameters 979 _refine_ls_number_restraints 877 _refine_ls_R_factor_all 0.2824 _refine_ls_R_factor_gt 0.0998 _refine_ls_wR_factor_ref 0.3073 _refine_ls_wR_factor_gt 0.2219 _refine_ls_goodness_of_fit_ref 0.961 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.040 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.34048(10) 0.89647(10) 0.07745(5) 0.0379(6) Uani 1 1 d . . . Co2 Co 0.34127(10) 0.78059(10) 0.02176(5) 0.0408(6) Uani 1 1 d . . . Co3 Co 0.19300(10) 0.64009(10) 0.06018(5) 0.0374(6) Uani 1 1 d . . . Co4 Co 0.18826(10) 0.85855(10) 0.04008(5) 0.0365(6) Uani 1 1 d . . . Co5 Co 0.32896(10) 0.85334(10) 0.21160(5) 0.0398(6) Uani 1 1 d . . . Co6 Co -0.06798(10) 0.63724(10) 0.09336(5) 0.0368(6) Uani 1 1 d . . . Na1 Na 0.1269(3) 0.7532(3) 0.11065(15) 0.0419(16) Uani 1 1 d . . . O124 O 0.2799(4) 0.8168(4) 0.0543(2) 0.035(3) Uani 1 1 d . . . O1W O 0.1496(4) 0.5765(5) 0.0215(2) 0.045(3) Uani 1 1 d . . . H1WA H 0.1809 0.5532 0.0136 0.068 Uiso 1 1 d R . . H1WB H 0.1301 0.6009 0.0059 0.068 Uiso 1 1 d R . . O2W O 0.2352(4) 0.5533(4) 0.0832(2) 0.038(3) Uani 1 1 d . . . H2WA H 0.2749 0.5605 0.0927 0.046 Uiso 1 1 d R . . H2WB H 0.2363 0.5202 0.0695 0.046 Uiso 1 1 d R . . N1A N 0.3544(6) 0.8505(5) -0.0139(3) 0.041(3) Uiso 1 1 d D . . C2A C 0.3503(7) 0.8477(6) -0.0470(4) 0.045(4) Uiso 1 1 d D . . S2AB S 0.3369(2) 0.7716(2) -0.07077(11) 0.0590(14) Uani 1 1 d D . . N3A N 0.3565(6) 0.8988(5) -0.0684(3) 0.041(3) Uiso 1 1 d D . . C4A C 0.3703(7) 0.9574(7) -0.0519(3) 0.042(4) Uiso 1 1 d D . . N41A N 0.3767(6) 1.0140(6) -0.0724(3) 0.050(4) Uiso 1 1 d D . . C42A C 0.3952(7) 1.0804(7) -0.0563(4) 0.051(5) Uiso 1 1 d D . . H42A H 0.3827 1.1173 -0.0725 0.061 Uiso 1 1 calc R . . H42B H 0.3688 1.0868 -0.0363 0.061 Uiso 1 1 calc R . . C43A C 0.4686(7) 1.0844(7) -0.0456(4) 0.051(5) Uiso 1 1 d D . . H43A H 0.4788 1.1285 -0.0349 0.076 Uiso 1 1 calc R . . H43B H 0.4948 1.0794 -0.0653 0.076 Uiso 1 1 calc R . . H43C H 0.4810 1.0481 -0.0293 0.076 Uiso 1 1 calc R . . C44A C 0.3738(7) 1.0088(8) -0.1097(4) 0.058(5) Uiso 1 1 d D . . H44A H 0.3805 0.9609 -0.1162 0.070 Uiso 1 1 calc R . . H44B H 0.4112 1.0359 -0.1181 0.070 Uiso 1 1 calc R . . C45A C 0.3074(8) 1.0334(9) -0.1258(4) 0.085(6) Uiso 1 1 d D . . H45A H 0.3071 1.0295 -0.1504 0.127 Uiso 1 1 calc R . . H45B H 0.3009 1.0810 -0.1197 0.127 Uiso 1 1 calc R . . H45C H 0.2703 1.0060 -0.1179 0.127 Uiso 1 1 calc R . . N5A N 0.3776(6) 0.9687(5) -0.0188(3) 0.039(3) Uiso 1 1 d D . . C6A C 0.3692(8) 0.9136(7) -0.0002(4) 0.044(5) Uiso 1 1 d D . . O6A O 0.3758(5) 0.9184(4) 0.0319(2) 0.042(3) Uani 1 1 d D . . N1B N 0.3125(6) 0.7081(5) -0.0119(3) 0.040(3) Uiso 1 1 d D . . C2B C 0.3159(7) 0.7030(7) -0.0450(3) 0.044(4) Uiso 1 1 d D . . N3B N 0.3035(6) 0.6477(6) -0.0636(3) 0.049(4) Uiso 1 1 d D . . C4B C 0.2837(7) 0.5938(7) -0.0459(4) 0.045(4) Uiso 1 1 d D . . N41B N 0.2759(6) 0.5340(6) -0.0627(3) 0.056(4) Uiso 1 1 d D . . C42B C 0.2576(8) 0.4722(8) -0.0448(4) 0.068(6) Uiso 1 1 d D . . H42C H 0.2390 0.4387 -0.0617 0.082 Uiso 1 1 calc R . . H42D H 0.2209 0.4834 -0.0302 0.082 Uiso 1 1 calc R . . C43B C 0.3144(9) 0.4403(9) -0.0238(5) 0.094(7) Uiso 1 1 d D . . H43D H 0.2975 0.4002 -0.0125 0.141 Uiso 1 1 calc R . . H43E H 0.3331 0.4727 -0.0068 0.141 Uiso 1 1 calc R . . H43F H 0.3501 0.4267 -0.0381 0.141 Uiso 1 1 calc R . . C44B C 0.2738(9) 0.5306(9) -0.1000(4) 0.087(7) Uiso 1 1 d D . . H44C H 0.2801 0.5765 -0.1095 0.105 Uiso 1 1 calc R . . H44D H 0.2293 0.5128 -0.1095 0.105 Uiso 1 1 calc R . . C45B C 0.3302(11) 0.4846(11) -0.1090(6) 0.140(10) Uiso 1 1 d D . . H45D H 0.3300 0.4817 -0.1336 0.210 Uiso 1 1 calc R . . H45E H 0.3233 0.4394 -0.0997 0.210 Uiso 1 1 calc R . . H45F H 0.3740 0.5028 -0.0995 0.210 Uiso 1 1 calc R . . N5B N 0.2730(6) 0.5936(6) -0.0132(3) 0.046(4) Uiso 1 1 d D . . C6B C 0.2877(7) 0.6509(7) 0.0040(4) 0.034(4) Uiso 1 1 d D . . O6B O 0.2791(4) 0.6592(4) 0.0348(2) 0.038(3) Uani 1 1 d D . . N1C N 0.2161(5) 0.9410(5) 0.0137(3) 0.037(3) Uiso 1 1 d D . . C2C C 0.2005(7) 0.9584(7) -0.0177(3) 0.043(4) Uiso 1 1 d D . . S2CD S 0.1678(2) 0.9025(2) -0.05030(10) 0.0460(12) Uani 1 1 d D . . N3C N 0.2111(6) 1.0178(6) -0.0314(3) 0.043(3) Uiso 1 1 d D . . C4C C 0.2353(7) 1.0640(6) -0.0087(3) 0.038(4) Uiso 1 1 d D . . N41C N 0.2421(6) 1.1278(5) -0.0222(3) 0.045(4) Uiso 1 1 d D . . C42C C 0.2751(8) 1.1831(8) -0.0017(4) 0.073(6) Uiso 1 1 d D . . H42E H 0.2931 1.1652 0.0205 0.087 Uiso 1 1 calc R . . H42F H 0.3137 1.2016 -0.0133 0.087 Uiso 1 1 calc R . . C43C C 0.2262(11) 1.2365(10) 0.0030(6) 0.130(9) Uiso 1 1 d D . . H43G H 0.2487 1.2732 0.0163 0.195 Uiso 1 1 calc R . . H43H H 0.1886 1.2183 0.0149 0.195 Uiso 1 1 calc R . . H43I H 0.2084 1.2541 -0.0191 0.195 Uiso 1 1 calc R . . C44C C 0.2229(7) 1.1392(8) -0.0589(4) 0.056(5) Uiso 1 1 d D . . H44E H 0.2445 1.1816 -0.0661 0.067 Uiso 1 1 calc R . . H44F H 0.2408 1.1014 -0.0720 0.067 Uiso 1 1 calc R . . C45C C 0.1482(7) 1.1441(8) -0.0670(4) 0.053(5) Uiso 1 1 d D . . H45G H 0.1383 1.1514 -0.0914 0.080 Uiso 1 1 calc R . . H45H H 0.1302 1.1822 -0.0546 0.080 Uiso 1 1 calc R . . H45I H 0.1265 1.1019 -0.0605 0.080 Uiso 1 1 calc R . . N5C N 0.2545(5) 1.0541(5) 0.0242(3) 0.038(3) Uiso 1 1 d D . . C6C C 0.2457(7) 0.9904(7) 0.0344(3) 0.036(4) Uiso 1 1 d D . . O6C O 0.2646(4) 0.9728(4) 0.0647(2) 0.037(3) Uani 1 1 d D . . N1D N 0.1551(6) 0.8074(5) -0.0023(3) 0.040(3) Uiso 1 1 d D . . C2D C 0.1532(7) 0.8212(6) -0.0348(3) 0.035(4) Uiso 1 1 d D . . N3D N 0.1384(6) 0.7776(5) -0.0598(3) 0.040(3) Uiso 1 1 d D . . C4D C 0.1231(7) 0.7144(7) -0.0490(3) 0.041(4) Uiso 1 1 d D . . N41D N 0.1061(6) 0.6683(6) -0.0740(3) 0.051(4) Uiso 1 1 d D . . C42D C 0.0929(7) 0.5966(7) -0.0649(4) 0.058(5) Uiso 1 1 d D . . H42G H 0.1028 0.5668 -0.0839 0.069 Uiso 1 1 calc R . . H42H H 0.1240 0.5838 -0.0450 0.069 Uiso 1 1 calc R . . C43D C 0.0216(7) 0.5858(8) -0.0569(4) 0.070(6) Uiso 1 1 d D . . H43J H 0.0154 0.5383 -0.0508 0.106 Uiso 1 1 calc R . . H43K H -0.0093 0.5970 -0.0768 0.106 Uiso 1 1 calc R . . H43L H 0.0117 0.6151 -0.0380 0.106 Uiso 1 1 calc R . . C44D C 0.0978(8) 0.6886(8) -0.1095(4) 0.060(5) Uiso 1 1 d D . . H44G H 0.0881 0.7378 -0.1112 0.072 Uiso 1 1 calc R . . H44H H 0.0590 0.6639 -0.1213 0.072 Uiso 1 1 calc R . . C45D C 0.1629(8) 0.6727(9) -0.1260(4) 0.080(6) Uiso 1 1 d D . . H45J H 0.1576 0.6866 -0.1498 0.120 Uiso 1 1 calc R . . H45K H 0.1718 0.6238 -0.1247 0.120 Uiso 1 1 calc R . . H45L H 0.2011 0.6973 -0.1143 0.120 Uiso 1 1 calc R . . N5D N 0.1261(6) 0.6938(5) -0.0171(3) 0.039(3) Uiso 1 1 d D . . C6D C 0.1434(7) 0.7401(7) 0.0071(4) 0.036(4) Uiso 1 1 d D . . O6D O 0.1488(4) 0.7281(4) 0.0380(2) 0.037(3) Uani 1 1 d D . . N1E N -0.0363(5) 0.7026(5) 0.0615(3) 0.033(3) Uiso 1 1 d D . . C2E C -0.0572(7) 0.6753(5) 0.0317(3) 0.035(4) Uiso 1 1 d D . . S2E S -0.0898(2) 0.5958(2) 0.03937(11) 0.0495(12) Uani 1 1 d D . . N3E N -0.0541(6) 0.7039(5) 0.0015(3) 0.046(4) Uiso 1 1 d D . . C4E C -0.0273(7) 0.7666(6) 0.0033(3) 0.042(4) Uiso 1 1 d D . . N41E N -0.0257(6) 0.8033(5) -0.0255(3) 0.049(4) Uiso 1 1 d D . . C42E C -0.0106(7) 0.8781(6) -0.0257(4) 0.049(5) Uiso 1 1 d D . . H42I H 0.0283 0.8878 -0.0089 0.059 Uiso 1 1 calc R . . H42J H 0.0028 0.8913 -0.0482 0.059 Uiso 1 1 calc R . . C43E C -0.0705(7) 0.9199(7) -0.0175(4) 0.063(5) Uiso 1 1 d D . . H43M H -0.0583 0.9681 -0.0178 0.094 Uiso 1 1 calc R . . H43N H -0.0836 0.9076 0.0050 0.094 Uiso 1 1 calc R . . H43O H -0.1089 0.9114 -0.0343 0.094 Uiso 1 1 calc R . . C44E C -0.0567(8) 0.7732(8) -0.0579(3) 0.071(6) Uiso 1 1 d D . . H44I H -0.0456 0.7242 -0.0581 0.085 Uiso 1 1 calc R . . H44J H -0.1069 0.7774 -0.0585 0.085 Uiso 1 1 calc R . . C45E C -0.0333(10) 0.8052(10) -0.0889(4) 0.110(8) Uiso 1 1 d D . . H45M H -0.0556 0.7830 -0.1089 0.165 Uiso 1 1 calc R . . H45N H 0.0162 0.8002 -0.0889 0.165 Uiso 1 1 calc R . . H45O H -0.0452 0.8535 -0.0892 0.165 Uiso 1 1 calc R . . N5E N -0.0012(5) 0.7949(5) 0.0320(2) 0.034(3) Uiso 1 1 d D . . H5E H 0.0184 0.8350 0.0314 0.040 Uiso 1 1 calc R . . C6E C -0.0045(7) 0.7629(6) 0.0622(3) 0.041(4) Uiso 1 1 d D . . O6E O 0.0196(5) 0.7905(4) 0.0889(2) 0.043(3) Uani 1 1 d D . . N1F N 0.0148(5) 0.5862(5) 0.1053(3) 0.034(3) Uiso 1 1 d D . . C2F C -0.0082(5) 0.5351(7) 0.1236(4) 0.047(5) Uiso 1 1 d D . . S2F S -0.09561(19) 0.5460(2) 0.12473(11) 0.0450(12) Uani 1 1 d D . . N3F N 0.0281(5) 0.4874(5) 0.1398(3) 0.039(3) Uiso 1 1 d D . . C4F C 0.0956(6) 0.4928(7) 0.1356(4) 0.052(5) Uiso 1 1 d D . . N41F N 0.1393(5) 0.4491(5) 0.1524(3) 0.051(4) Uiso 1 1 d D . . C42F C 0.2133(6) 0.4476(7) 0.1502(4) 0.056(5) Uiso 1 1 d D . . H42K H 0.2232 0.4538 0.1264 0.067 Uiso 1 1 calc R . . H42L H 0.2312 0.4027 0.1578 0.067 Uiso 1 1 calc R . . C43F C 0.2490(8) 0.5019(8) 0.1715(4) 0.070(6) Uiso 1 1 d D . . H43P H 0.2980 0.4998 0.1691 0.105 Uiso 1 1 calc R . . H43Q H 0.2407 0.4950 0.1952 0.105 Uiso 1 1 calc R . . H43R H 0.2314 0.5465 0.1640 0.105 Uiso 1 1 calc R . . C44F C 0.1113(7) 0.3978(6) 0.1750(3) 0.051(5) Uiso 1 1 d D . . H44K H 0.0703 0.4165 0.1844 0.061 Uiso 1 1 calc R . . H44L H 0.1456 0.3882 0.1941 0.061 Uiso 1 1 calc R . . C45F C 0.0929(8) 0.3330(7) 0.1567(4) 0.070(6) Uiso 1 1 d D . . H45P H 0.0746 0.3006 0.1723 0.105 Uiso 1 1 calc R . . H45Q H 0.1337 0.3138 0.1478 0.105 Uiso 1 1 calc R . . H45R H 0.0585 0.3422 0.1379 0.105 Uiso 1 1 calc R . . N5F N 0.1236(5) 0.5417(5) 0.1174(3) 0.034(3) Uiso 1 1 d D . . H5F H 0.1676 0.5417 0.1150 0.040 Uiso 1 1 calc R . . C6F C 0.0826(6) 0.5910(6) 0.1027(3) 0.038(4) Uiso 1 1 d D . . O6F O 0.1081(4) 0.6384(4) 0.0870(2) 0.038(3) Uani 1 1 d D . . N1G N -0.0623(5) 0.6986(5) 0.1313(3) 0.034(3) Uiso 1 1 d D . . C2G C -0.1256(6) 0.7253(7) 0.1295(3) 0.042(4) Uiso 1 1 d D . . S2G S -0.17192(19) 0.6874(2) 0.09604(11) 0.0458(12) Uani 1 1 d D . . N3G N -0.1494(5) 0.7723(5) 0.1491(3) 0.040(3) Uiso 1 1 d D . . C4G C -0.1025(6) 0.7938(7) 0.1730(3) 0.051(5) Uiso 1 1 d D . . N41G N -0.1209(6) 0.8445(6) 0.1937(3) 0.065(4) Uiso 1 1 d D . . C42G C -0.0752(8) 0.8730(8) 0.2220(4) 0.083(6) Uiso 1 1 d D . . H42M H -0.0909 0.9191 0.2275 0.099 Uiso 1 1 calc R . . H42N H -0.0283 0.8768 0.2149 0.099 Uiso 1 1 calc R . . C43G C -0.0748(10) 0.8287(10) 0.2527(4) 0.118(8) Uiso 1 1 d D . . H43S H -0.0437 0.8477 0.2708 0.177 Uiso 1 1 calc R . . H43T H -0.0596 0.7830 0.2472 0.177 Uiso 1 1 calc R . . H43U H -0.1210 0.8264 0.2602 0.177 Uiso 1 1 calc R . . C44G C -0.1915(8) 0.8763(9) 0.1876(5) 0.106(8) Uiso 1 1 d D . . H44M H -0.1899 0.9240 0.1955 0.127 Uiso 1 1 calc R . . H44N H -0.2059 0.8762 0.1631 0.127 Uiso 1 1 calc R . . C45G C -0.2413(11) 0.8378(13) 0.2059(7) 0.174(12) Uiso 1 1 d D . . H45S H -0.2866 0.8584 0.2017 0.261 Uiso 1 1 calc R . . H45T H -0.2275 0.8388 0.2302 0.261 Uiso 1 1 calc R . . H45U H -0.2429 0.7907 0.1980 0.261 Uiso 1 1 calc R . . N5G N -0.0369(5) 0.7738(5) 0.1756(3) 0.047(4) Uiso 1 1 d D . . H5G H -0.0079 0.7923 0.1910 0.056 Uiso 1 1 calc R . . C6G C -0.0149(6) 0.7251(6) 0.1545(3) 0.035(4) Uiso 1 1 d D . . O6G O 0.0472(4) 0.7082(5) 0.1564(2) 0.043(3) Uani 1 1 d D . . N1H N 0.3195(5) 0.7407(5) 0.1399(3) 0.035(3) Uiso 1 1 d D . . H1H H 0.2964 0.7784 0.1424 0.042 Uiso 1 1 calc R . . C2H C 0.3777(6) 0.7308(6) 0.1588(3) 0.037(4) Uiso 1 1 d D . . S2H S 0.4095(2) 0.7919(2) 0.18711(11) 0.0464(12) Uani 1 1 d D . . N3H N 0.4165(5) 0.6775(5) 0.1552(3) 0.044(4) Uiso 1 1 d D . . C4H C 0.3928(6) 0.6334(7) 0.1311(4) 0.053(5) Uiso 1 1 d D . . N41H N 0.4338(6) 0.5815(6) 0.1241(3) 0.072(5) Uiso 1 1 d D . . C42H C 0.4157(9) 0.5304(8) 0.0975(4) 0.078(6) Uiso 1 1 d D . . H42O H 0.4444 0.4896 0.1017 0.093 Uiso 1 1 calc R . . H42P H 0.3675 0.5169 0.0983 0.093 Uiso 1 1 calc R . . C43H C 0.4258(11) 0.5577(10) 0.0635(4) 0.117(8) Uiso 1 1 d D . . H43V H 0.4124 0.5234 0.0464 0.176 Uiso 1 1 calc R . . H43W H 0.4740 0.5693 0.0624 0.176 Uiso 1 1 calc R . . H43$ H 0.3978 0.5984 0.0594 0.176 Uiso 1 1 calc R . . C44H C 0.5087(8) 0.5831(10) 0.1374(5) 0.117(8) Uiso 1 1 d D . . H44O H 0.5382 0.5657 0.1204 0.140 Uiso 1 1 calc R . . H44P H 0.5233 0.6297 0.1439 0.140 Uiso 1 1 calc R . . C45H C 0.5109(11) 0.5381(12) 0.1672(5) 0.150(10) Uiso 1 1 d D . . H45V H 0.5577 0.5356 0.1777 0.225 Uiso 1 1 calc R . . H45W H 0.4954 0.4927 0.1602 0.225 Uiso 1 1 calc R . . H45$ H 0.4810 0.5562 0.1836 0.225 Uiso 1 1 calc R . . N5H N 0.3319(5) 0.6372(5) 0.1134(3) 0.037(3) Uiso 1 1 d D . . C6H C 0.2951(6) 0.6940(6) 0.1171(3) 0.036(4) Uiso 1 1 d D . . O6H O 0.2390(4) 0.7038(4) 0.0992(2) 0.038(3) Uani 1 1 d D . . N1I N 0.2590(5) 0.7827(5) 0.2083(3) 0.037(3) Uiso 1 1 d D . . C2I C 0.2719(6) 0.7501(6) 0.2382(3) 0.042(4) Uiso 1 1 d D . . S2I S 0.3438(2) 0.7857(2) 0.25869(10) 0.0461(12) Uani 1 1 d D . . N3I N 0.2374(5) 0.6988(5) 0.2497(3) 0.041(3) Uiso 1 1 d D . . C4I C 0.1833(7) 0.6810(7) 0.2286(3) 0.052(5) Uiso 1 1 d D . . N41I N 0.1428(6) 0.6307(6) 0.2384(3) 0.069(4) Uiso 1 1 d D . . C42I C 0.0958(9) 0.5897(10) 0.2123(5) 0.118(8) Uiso 1 1 d D . . H42Q H 0.1030 0.6026 0.1888 0.141 Uiso 1 1 calc R . . H42R H 0.1025 0.5402 0.2151 0.141 Uiso 1 1 calc R . . C43I C 0.0287(10) 0.6114(13) 0.2218(7) 0.164(11) Uiso 1 1 d D . . H43$ H -0.0071 0.5893 0.2071 0.246 Uiso 1 1 calc R . . H43 H 0.0246 0.6607 0.2194 0.246 Uiso 1 1 calc R . . H43C H 0.0239 0.5987 0.2454 0.246 Uiso 1 1 calc R . . C44I C 0.1559(8) 0.6012(7) 0.2728(3) 0.064(5) Uiso 1 1 d D . . H44Q H 0.1321 0.5570 0.2734 0.076 Uiso 1 1 calc R . . H44R H 0.2054 0.5924 0.2771 0.076 Uiso 1 1 calc R . . C45I C 0.1337(9) 0.6446(8) 0.3002(4) 0.078(6) Uiso 1 1 d D . . H45$ H 0.1447 0.6222 0.3220 0.117 Uiso 1 1 calc R . . H45 H 0.0844 0.6519 0.2967 0.117 Uiso 1 1 calc R . . H45C H 0.1573 0.6883 0.3000 0.117 Uiso 1 1 calc R . . N5I N 0.1677(5) 0.7106(5) 0.1985(3) 0.043(3) Uiso 1 1 d D . . H5I H 0.1331 0.6949 0.1853 0.051 Uiso 1 1 calc R . . C6I C 0.2039(6) 0.7644(6) 0.1878(3) 0.030(4) Uiso 1 1 d D . . O6I O 0.1870(4) 0.7922(4) 0.1602(2) 0.038(3) Uani 1 1 d D . . N1J N 0.4244(5) 0.9433(5) 0.1573(2) 0.041(3) Uiso 1 1 d D . . H1J H 0.4069 0.9025 0.1542 0.049 Uiso 1 1 calc R . . C2J C 0.4453(7) 0.9635(6) 0.1888(3) 0.046(5) Uiso 1 1 d D . . S2J S 0.4197(2) 0.9235(2) 0.22480(11) 0.0470(12) Uani 1 1 d D . . N3J N 0.4846(6) 1.0189(6) 0.1938(3) 0.050(4) Uiso 1 1 d D . . C4J C 0.4956(7) 1.0525(7) 0.1651(3) 0.058(5) Uiso 1 1 d D . . N41J N 0.5395(6) 1.1059(6) 0.1685(3) 0.061(4) Uiso 1 1 d D . . C42J C 0.5511(8) 1.1529(7) 0.1403(4) 0.066(5) Uiso 1 1 d D . . H42S H 0.5456 1.1277 0.1187 0.079 Uiso 1 1 calc R . . H42T H 0.5984 1.1701 0.1432 0.079 Uiso 1 1 calc R . . C43J C 0.5028(9) 1.2117(8) 0.1385(5) 0.085(6) Uiso 1 1 d D . . H43$ H 0.5121 1.2409 0.1195 0.128 Uiso 1 1 calc R . . H43 H 0.5090 1.2378 0.1596 0.128 Uiso 1 1 calc R . . H43C H 0.4558 1.1950 0.1353 0.128 Uiso 1 1 calc R . . C44J C 0.5798(8) 1.1199(8) 0.2015(4) 0.081(6) Uiso 1 1 d D . . H44S H 0.5926 1.1684 0.2029 0.097 Uiso 1 1 calc R . . H44T H 0.5519 1.1094 0.2204 0.097 Uiso 1 1 calc R . . C45J C 0.6425(9) 1.0767(10) 0.2039(5) 0.116(8) Uiso 1 1 d D . . H45$ H 0.6691 1.0854 0.2254 0.174 Uiso 1 1 calc R . . H45 H 0.6701 1.0876 0.1852 0.174 Uiso 1 1 calc R . . H45C H 0.6294 1.0287 0.2026 0.174 Uiso 1 1 calc R . . N5J N 0.4658(6) 1.0430(6) 0.1341(3) 0.052(4) Uiso 1 1 d D . . C6J C 0.4296(7) 0.9842(7) 0.1303(3) 0.042(4) Uiso 1 1 d D . . O6J O 0.4016(5) 0.9706(5) 0.1012(2) 0.044(3) Uani 1 1 d D . . N1K N 0.2835(5) 0.9136(5) 0.1775(3) 0.038(3) Uiso 1 1 d D . . C2K C 0.2500(7) 0.9564(6) 0.1965(3) 0.037(4) Uiso 1 1 d D . . S2K S 0.2599(2) 0.9290(2) 0.23765(10) 0.0445(12) Uani 1 1 d D . . N3K N 0.2199(5) 1.0138(5) 0.1870(3) 0.038(3) Uiso 1 1 d D . . C4K C 0.2231(7) 1.0266(6) 0.1540(3) 0.046(5) Uiso 1 1 d D . . N41K N 0.2035(6) 1.0880(5) 0.1420(3) 0.048(4) Uiso 1 1 d D . . C42K C 0.2132(7) 1.1104(8) 0.1070(3) 0.060(5) Uiso 1 1 d D . . H42U H 0.2026 1.0723 0.0912 0.072 Uiso 1 1 calc R . . H42V H 0.1811 1.1478 0.1006 0.072 Uiso 1 1 calc R . . C43K C 0.2842(7) 1.1337(8) 0.1038(4) 0.067(5) Uiso 1 1 d D . . H43$ H 0.2889 1.1480 0.0805 0.100 Uiso 1 1 calc R . . H43 H 0.3160 1.0965 0.1097 0.100 Uiso 1 1 calc R . . H43C H 0.2945 1.1720 0.1191 0.100 Uiso 1 1 calc R . . C44K C 0.1798(7) 1.1412(7) 0.1652(4) 0.059(5) Uiso 1 1 d D . . H44U H 0.2085 1.1397 0.1869 0.071 Uiso 1 1 calc R . . H44V H 0.1855 1.1865 0.1550 0.071 Uiso 1 1 calc R . . C45K C 0.1074(7) 1.1319(8) 0.1718(4) 0.075(6) Uiso 1 1 d D . . H45$ H 0.0941 1.1672 0.1873 0.113 Uiso 1 1 calc R . . H45 H 0.1015 1.0872 0.1820 0.113 Uiso 1 1 calc R . . H45C H 0.0786 1.1350 0.1505 0.113 Uiso 1 1 calc R . . N5K N 0.2478(5) 0.9823(5) 0.1321(3) 0.036(3) Uiso 1 1 d D . . H5K H 0.2445 0.9914 0.1104 0.043 Uiso 1 1 calc R . . C6K C 0.2780(7) 0.9234(6) 0.1437(3) 0.035(4) Uiso 1 1 d D . . O6K O 0.2989(4) 0.8806(4) 0.1237(2) 0.034(3) Uani 1 1 d D . . O11 O 0.4127(4) 0.8245(5) 0.0928(2) 0.041(3) Uani 1 1 d D . . O21 O 0.4262(5) 0.7567(5) 0.0481(3) 0.046(3) Uani 1 1 d D . . C11 C 0.4459(7) 0.7843(7) 0.0765(4) 0.036(4) Uiso 1 1 d D . . C21 C 0.5183(6) 0.7667(7) 0.0908(4) 0.042(4) Uiso 1 1 d D . . C31 C 0.5388(7) 0.7897(7) 0.1229(4) 0.051(5) Uiso 1 1 d D . . H31 H 0.5074 0.8119 0.1360 0.061 Uiso 1 1 calc R . . C41 C 0.6072(8) 0.7796(8) 0.1359(4) 0.067(5) Uiso 1 1 d D . . H41 H 0.6234 0.7977 0.1572 0.080 Uiso 1 1 calc R . . C51 C 0.6496(8) 0.7429(8) 0.1169(4) 0.061(5) Uiso 1 1 d D . . H51 H 0.6946 0.7329 0.1262 0.073 Uiso 1 1 calc R . . C61 C 0.6287(7) 0.7203(8) 0.0851(4) 0.057(5) Uiso 1 1 d D . . H61 H 0.6604 0.6983 0.0719 0.069 Uiso 1 1 calc R . . C71 C 0.5614(7) 0.7294(8) 0.0717(4) 0.055(5) Uiso 1 1 d D . . H71 H 0.5455 0.7107 0.0504 0.066 Uiso 1 1 calc R . . O12 O 0.0767(5) 0.9153(4) 0.0464(2) 0.042(3) Uani 1 1 d D . . O22 O 0.1504(4) 0.8693(4) 0.0852(2) 0.035(3) Uani 1 1 d D . . C12 C 0.0973(7) 0.9056(7) 0.0763(4) 0.038(4) Uiso 1 1 d D . . C22 C 0.0597(6) 0.9357(7) 0.1047(3) 0.031(4) Uiso 1 1 d D . . C32 C 0.0023(7) 0.9748(7) 0.0962(4) 0.052(5) Uiso 1 1 d D . . H32 H -0.0123 0.9833 0.0732 0.063 Uiso 1 1 calc R . . C42 C -0.0342(8) 1.0019(8) 0.1223(4) 0.064(5) Uiso 1 1 d D . . H42 H -0.0740 1.0282 0.1169 0.077 Uiso 1 1 calc R . . C52 C -0.0118(8) 0.9899(8) 0.1559(4) 0.064(5) Uiso 1 1 d D . . H52 H -0.0366 1.0078 0.1734 0.076 Uiso 1 1 calc R . . C62 C 0.0461(8) 0.9522(8) 0.1640(4) 0.063(5) Uiso 1 1 d D . . H62 H 0.0614 0.9447 0.1871 0.076 Uiso 1 1 calc R . . C72 C 0.0830(7) 0.9246(7) 0.1382(3) 0.047(5) Uiso 1 1 d D . . H72 H 0.1232 0.8988 0.1437 0.056 Uiso 1 1 calc R . . C1O C 0.3585(10) 0.5869(10) 0.2374(5) 0.108(8) Uiso 1 1 d D . . H1O1 H 0.3197 0.5744 0.2501 0.163 Uiso 1 1 d R . . H1O2 H 0.3437 0.5888 0.2133 0.163 Uiso 1 1 d R . . H1O3 H 0.3758 0.6314 0.2450 0.163 Uiso 1 1 d R . . C2O C 0.4080(10) 0.5400(10) 0.2428(5) 0.088(7) Uiso 1 1 d D . . N3O N 0.4464(9) 0.4944(9) 0.2478(5) 0.117(7) Uiso 1 1 d D . . C1P C 0.4388(8) 0.0817(8) 0.0467(4) 0.069(6) Uiso 1 1 d D . . H1P1 H 0.4520 0.0579 0.0266 0.103 Uiso 1 1 d R . . H1P2 H 0.3901 0.0746 0.0489 0.103 Uiso 1 1 d R . . H1P3 H 0.4652 0.0639 0.0668 0.103 Uiso 1 1 d R . . C2P C 0.4511(12) 0.1481(11) 0.0438(6) 0.122(9) Uiso 1 1 d D . . N3P N 0.4617(12) 0.2060(11) 0.0365(6) 0.182(10) Uiso 1 1 d D . . C1Q C 0.1658(9) 0.4072(9) 0.0513(5) 0.089(7) Uiso 1 1 d D . . H1Q1 H 0.1407 0.4392 0.0644 0.133 Uiso 1 1 d R . . H1Q2 H 0.1362 0.3915 0.0317 0.133 Uiso 1 1 d R . . H1Q3 H 0.2059 0.4297 0.0434 0.133 Uiso 1 1 d R . . C2Q C 0.1858(12) 0.3532(11) 0.0710(6) 0.125(9) Uiso 1 1 d D . . N3Q N 0.2034(10) 0.3079(10) 0.0898(5) 0.133(7) Uiso 1 1 d D . . C1R C 0.1403(9) 0.8470(9) 0.2873(4) 0.084(6) Uiso 1 1 d D . . H1R1 H 0.1776 0.8154 0.2938 0.126 Uiso 1 1 d R . . H1R2 H 0.1086 0.8482 0.3051 0.126 Uiso 1 1 d R . . H1R3 H 0.1589 0.8924 0.2843 0.126 Uiso 1 1 d R . . C2R C 0.1063(9) 0.8257(10) 0.2576(4) 0.079(6) Uiso 1 1 d D . . N3R N 0.0772(7) 0.8099(7) 0.2316(4) 0.075(5) Uiso 1 1 d D . . C1S C 0.5163(13) 0.3618(13) 0.0125(6) 0.097(9) Uiso 0.75 1 d PD . . H1S1 H 0.5426 0.3199 0.0164 0.145 Uiso 0.75 1 d PR . . H1S2 H 0.5297 0.3840 -0.0080 0.145 Uiso 0.75 1 d PR . . H1S3 H 0.4676 0.3509 0.0097 0.145 Uiso 0.75 1 d PR . . C2S C 0.5287(15) 0.4036(13) 0.0388(7) 0.106(10) Uiso 0.75 1 d PD . . N3S N 0.5308(15) 0.4069(14) 0.0697(7) 0.160(12) Uiso 0.75 1 d PD . . C1T C 0.7735(11) 0.6203(11) 0.1826(6) 0.068(7) Uiso 0.75 1 d PD . . H1T1 H 0.7318 0.6381 0.1911 0.102 Uiso 0.75 1 d PR . . H1T2 H 0.7726 0.5706 0.1831 0.102 Uiso 0.75 1 d PR . . H1T3 H 0.7765 0.6358 0.1593 0.102 Uiso 0.75 1 d PR . . C2T C 0.8273(12) 0.6425(12) 0.2019(6) 0.074(8) Uiso 0.75 1 d PD . . N3T N 0.8776(12) 0.6641(14) 0.2170(7) 0.141(10) Uiso 0.75 1 d PD . . C1U C 0.3752(16) 0.3262(16) 0.0776(7) 0.059(10) Uiso 0.50 1 d PD . . H1U1 H 0.3423 0.3554 0.0647 0.088 Uiso 0.50 1 d PR . . H1U2 H 0.3608 0.2788 0.0751 0.088 Uiso 0.50 1 d PR . . H1U3 H 0.4203 0.3317 0.0692 0.088 Uiso 0.50 1 d PR . . C2U C 0.3782(16) 0.3437(16) 0.1097(8) 0.060(10) Uiso 0.50 1 d PD . . N3U N 0.3933(17) 0.3737(16) 0.1352(8) 0.105(12) Uiso 0.50 1 d PD . . C1V C 0.7955(16) 0.1459(15) 0.1418(8) 0.059(10) Uiso 0.50 1 d PD . . H1V1 H 0.7711 0.1185 0.1241 0.088 Uiso 0.50 1 d PR . . H1V2 H 0.8305 0.1730 0.1320 0.088 Uiso 0.50 1 d PR . . H1V3 H 0.7634 0.1760 0.1520 0.088 Uiso 0.50 1 d PR . . C2V C 0.8249(18) 0.1049(18) 0.1656(8) 0.082(12) Uiso 0.50 1 d PD . . N3V N 0.8393(15) 0.0693(15) 0.1900(7) 0.090(11) Uiso 0.50 1 d PD . . C1X C 0.6809(16) 0.2749(15) 0.1720(8) 0.071(11) Uiso 0.50 1 d PD . . H1X1 H 0.6476 0.2421 0.1791 0.106 Uiso 0.50 1 d PR . . H1X2 H 0.7117 0.2883 0.1915 0.106 Uiso 0.50 1 d PR . . H1X3 H 0.7073 0.2541 0.1549 0.106 Uiso 0.50 1 d PR . . C2X C 0.6483(15) 0.3297(14) 0.1590(8) 0.049(9) Uiso 0.50 1 d PD . . N3X N 0.6025(16) 0.3696(15) 0.1521(9) 0.106(12) Uiso 0.50 1 d PD . . C1Y C 0.7947(14) 0.4432(18) 0.2056(9) 0.079(12) Uiso 0.50 1 d PD . . H1Y1 H 0.7806 0.4895 0.2108 0.118 Uiso 0.50 1 d PR . . H1Y2 H 0.7752 0.4114 0.2212 0.118 Uiso 0.50 1 d PR . . H1Y3 H 0.7784 0.4319 0.1823 0.118 Uiso 0.50 1 d PR . . C2Y C 0.8616(14) 0.4391(19) 0.2090(10) 0.080(12) Uiso 0.50 1 d PD . . N3Y N 0.9224(13) 0.4336(14) 0.2085(7) 0.071(9) Uiso 0.50 1 d PD . . C1Z C 0.952(2) 0.187(2) 0.2569(10) 0.113(16) Uiso 0.50 1 d PD . . H1Z1 H 0.9361 0.1413 0.2513 0.170 Uiso 0.50 1 d PR . . H1Z2 H 0.9207 0.2095 0.2712 0.170 Uiso 0.50 1 d PR . . H1Z3 H 0.9977 0.1849 0.2691 0.170 Uiso 0.50 1 d PR . . C2Z C 0.956(2) 0.223(2) 0.2283(10) 0.097(14) Uiso 0.50 1 d PD . . N3Z N 0.947(2) 0.242(2) 0.1995(9) 0.134(15) Uiso 0.50 1 d PD . . 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 0.0403(14) 0.0348(13) 0.0390(15) -0.0017(11) 0.0065(11) -0.0029(11) Co2 0.0433(14) 0.0385(14) 0.0415(15) -0.0010(11) 0.0086(11) -0.0049(11) Co3 0.0419(14) 0.0303(13) 0.0406(15) -0.0013(11) 0.0071(11) -0.0018(11) Co4 0.0396(14) 0.0339(13) 0.0360(14) 0.0014(11) 0.0040(11) -0.0037(11) Co5 0.0391(14) 0.0410(14) 0.0391(15) -0.0035(11) 0.0015(11) -0.0019(11) Co6 0.0371(13) 0.0341(13) 0.0394(15) 0.0028(11) 0.0039(11) -0.0040(11) Na1 0.044(4) 0.035(4) 0.045(4) 0.002(3) -0.001(3) 0.001(3) O124 0.030(6) 0.037(6) 0.040(7) -0.003(5) 0.010(5) -0.004(5) O1W 0.042(7) 0.051(7) 0.039(7) -0.005(5) -0.010(5) 0.002(5) O2W 0.043(6) 0.031(6) 0.040(7) -0.008(5) 0.000(5) 0.002(5) S2AB 0.085(4) 0.047(3) 0.047(3) -0.007(2) 0.022(3) -0.019(3) O6A 0.047(7) 0.040(7) 0.040(8) -0.002(5) 0.003(6) -0.010(5) O6B 0.032(6) 0.042(7) 0.041(7) -0.008(5) 0.004(5) 0.001(5) S2CD 0.059(3) 0.040(3) 0.040(3) 0.004(2) 0.007(2) -0.004(2) O6C 0.046(7) 0.036(6) 0.027(7) 0.002(5) -0.001(5) 0.001(5) O6D 0.042(6) 0.038(6) 0.030(7) 0.011(5) 0.003(5) -0.003(5) S2E 0.061(3) 0.040(3) 0.047(3) -0.001(2) -0.001(2) -0.008(2) O6E 0.042(7) 0.040(7) 0.048(8) 0.001(6) 0.002(6) -0.005(5) S2F 0.041(3) 0.040(3) 0.054(3) 0.006(2) 0.007(2) -0.005(2) O6F 0.039(6) 0.037(6) 0.040(7) 0.002(5) 0.010(5) -0.007(5) S2G 0.036(3) 0.042(3) 0.059(3) 0.008(2) -0.001(2) 0.005(2) O6G 0.034(7) 0.049(7) 0.045(7) 0.004(6) 0.005(5) -0.004(5) S2H 0.041(3) 0.043(3) 0.053(3) -0.011(2) -0.003(2) -0.001(2) O6H 0.041(7) 0.025(6) 0.047(7) -0.004(5) 0.003(5) 0.000(5) S2I 0.050(3) 0.048(3) 0.039(3) 0.001(2) -0.005(2) -0.003(2) O6I 0.037(6) 0.037(6) 0.041(7) 0.006(5) -0.002(5) -0.007(5) S2J 0.047(3) 0.047(3) 0.046(3) -0.007(2) 0.001(2) -0.006(2) O6J 0.048(7) 0.048(7) 0.039(7) -0.002(6) 0.010(6) -0.008(5) S2K 0.049(3) 0.047(3) 0.038(3) -0.006(2) 0.007(2) 0.004(2) O6K 0.034(6) 0.031(6) 0.037(7) -0.003(5) 0.002(5) 0.000(5) O11 0.041(7) 0.040(7) 0.043(7) -0.011(5) 0.006(5) -0.003(5) O21 0.044(7) 0.041(7) 0.052(8) -0.003(6) 0.003(6) -0.008(5) O12 0.056(7) 0.037(7) 0.034(7) 0.010(5) 0.003(6) 0.001(5) O22 0.035(6) 0.031(6) 0.040(7) -0.003(5) -0.002(5) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O6A 2.039(10) . ? Co1 O11 2.066(9) . ? Co1 O6J 2.069(9) . ? Co1 O6K 2.096(9) . ? Co1 O124 2.132(9) . ? Co1 O6C 2.152(9) . ? Co2 O21 1.954(10) . ? Co2 O124 1.977(9) . ? Co2 N1B 2.006(11) . ? Co2 N1A 2.009(11) . ? Co3 O6F 2.058(9) . ? Co3 O6B 2.080(9) . ? Co3 O2W 2.080(9) . ? Co3 O6D 2.101(9) . ? Co3 O1W 2.109(9) . ? Co3 O6H 2.136(9) . ? Co3 Na1 3.336(6) . ? Co4 O22 2.010(9) . ? Co4 O124 2.021(9) . ? Co4 N1D 2.023(11) . ? Co4 N1C 2.035(11) . ? Co5 N1I 1.956(10) . ? Co5 N1K 1.960(10) . ? Co5 S2H 2.277(5) . ? Co5 S2J 2.286(4) . ? Co5 S2I 2.296(5) . ? Co5 S2K 2.320(4) . ? Co6 N1G 1.929(10) . ? Co6 N1F 1.939(10) . ? Co6 N1E 1.945(10) . ? Co6 S2F 2.280(4) . ? Co6 S2G 2.283(4) . ? Co6 S2E 2.302(5) . ? Na1 O6E 2.333(10) . ? Na1 O6I 2.339(10) . ? Na1 O6F 2.468(10) . ? Na1 O6H 2.488(10) . ? Na1 O22 2.560(10) . ? Na1 O6G 2.652(11) . ? Na1 O6D 2.995(11) . ? Na1 C6E 3.098(14) . ? N1A C2A 1.310(14) . ? N1A C6A 1.380(14) . ? C2A N3A 1.331(14) . ? C2A S2AB 1.782(13) . ? S2AB C2B 1.767(13) . ? N3A C4A 1.344(14) . ? C4A N5A 1.331(14) . ? C4A N41A 1.392(14) . ? N41A C44A 1.484(14) . ? N41A C42A 1.489(14) . ? C42A C43A 1.474(15) . ? C44A C45A 1.488(16) . ? N5A C6A 1.332(14) . ? C6A O6A 1.274(13) . ? N1B C2B 1.323(14) . ? N1B C6B 1.401(14) . ? C2B N3B 1.329(14) . ? N3B C4B 1.350(14) . ? C4B N5B 1.333(14) . ? C4B N41B 1.357(14) . ? N41B C42B 1.471(15) . ? N41B C44B 1.482(16) . ? C42B C43B 1.479(17) . ? C44B C45B 1.499(19) . ? N5B C6B 1.339(14) . ? C6B O6B 1.260(13) . ? N1C C2C 1.305(14) . ? N1C C6C 1.372(14) . ? C2C N3C 1.316(14) . ? C2C S2CD 1.778(13) . ? S2CD C2D 1.751(12) . ? N3C C4C 1.340(14) . ? C4C N5C 1.344(14) . ? C4C N41C 1.379(14) . ? N41C C42C 1.477(15) . ? N41C C44C 1.493(14) . ? C42C C43C 1.449(17) . ? C44C C45C 1.482(15) . ? N5C C6C 1.335(14) . ? C6C O6C 1.279(13) . ? N1D C2D 1.315(13) . ? N1D C6D 1.404(14) . ? C2D N3D 1.330(13) . ? N3D C4D 1.361(14) . ? C4D N5D 1.328(14) . ? C4D N41D 1.370(14) . ? N41D C44D 1.460(15) . ? N41D C42D 1.487(15) . ? C42D C43D 1.479(16) . ? C44D C45D 1.521(17) . ? N5D C6D 1.347(14) . ? C6D O6D 1.247(13) . ? N1E C2E 1.334(11) . ? N1E C6E 1.343(11) . ? C2E N3E 1.333(11) . ? C2E S2E 1.731(10) . ? N3E C4E 1.345(11) . ? C4E N5E 1.331(11) . ? C4E N41E 1.359(11) . ? N41E C44E 1.499(12) . ? N41E C42E 1.505(12) . ? C42E C43E 1.496(13) . ? C44E C45E 1.490(14) . ? N5E C6E 1.361(11) . ? C6E O6E 1.251(11) . ? N1F C2F 1.343(11) . ? N1F C6F 1.351(11) . ? C2F N3F 1.319(11) . ? C2F S2F 1.739(11) . ? N3F C4F 1.357(11) . ? C4F N5F 1.351(11) . ? C4F N41F 1.353(11) . ? N41F C42F 1.467(12) . ? N41F C44F 1.490(12) . ? C42F C43F 1.502(13) . ? C44F C45F 1.501(13) . ? N5F C6F 1.363(11) . ? C6F O6F 1.251(11) . ? N1G C2G 1.350(11) . ? N1G C6G 1.360(11) . ? C2G N3G 1.320(11) . ? C2G S2G 1.718(10) . ? N3G C4G 1.336(11) . ? C4G N5G 1.347(11) . ? C4G N41G 1.364(12) . ? N41G C42G 1.489(12) . ? N41G C44G 1.526(13) . ? C42G C43G 1.501(14) . ? C44G C45G 1.479(15) . ? N5G C6G 1.370(11) . ? C6G O6G 1.263(11) . ? N1H C2H 1.328(11) . ? N1H C6H 1.352(11) . ? C2H N3H 1.315(11) . ? C2H S2H 1.730(10) . ? N3H C4H 1.347(11) . ? C4H N5H 1.339(11) . ? C4H N41H 1.347(12) . ? N41H C42H 1.483(12) . ? N41H C44H 1.525(13) . ? C42H C43H 1.480(14) . ? C44H C45H 1.478(15) . ? N5H C6H 1.349(11) . ? C6H O6H 1.279(11) . ? N1I C6I 1.352(11) . ? N1I C2I 1.355(11) . ? C2I N3I 1.320(11) . ? C2I S2I 1.722(10) . ? N3I C4I 1.344(11) . ? C4I N5I 1.343(11) . ? C4I N41I 1.350(11) . ? N41I C44I 1.489(12) . ? N41I C42I 1.556(13) . ? C42I C43I 1.469(15) . ? C44I C45I 1.480(13) . ? N5I C6I 1.365(11) . ? C6I O6I 1.245(11) . ? N1J C2J 1.342(11) . ? N1J C6J 1.356(11) . ? C2J N3J 1.343(11) . ? C2J S2J 1.745(11) . ? N3J C4J 1.350(12) . ? C4J N5J 1.332(12) . ? C4J N41J 1.362(12) . ? N41J C42J 1.486(12) . ? N41J C44J 1.500(12) . ? C42J C43J 1.497(13) . ? C44J C45J 1.497(14) . ? N5J C6J 1.363(11) . ? C6J O6J 1.266(11) . ? N1K C2K 1.342(11) . ? N1K C6K 1.352(11) . ? C2K N3K 1.318(11) . ? C2K S2K 1.719(10) . ? N3K C4K 1.341(11) . ? C4K N41K 1.347(11) . ? C4K N5K 1.350(11) . ? N41K C42K 1.488(12) . ? N41K C44K 1.496(12) . ? C42K C43K 1.487(13) . ? C44K C45K 1.484(13) . ? N5K C6K 1.366(11) . ? C6K O6K 1.254(11) . ? O11 C11 1.242(13) . ? O21 C11 1.286(13) . ? C11 C21 1.528(15) . ? C21 C31 1.381(15) . ? C21 C71 1.394(15) . ? C31 C41 1.415(16) . ? C41 C51 1.377(16) . ? C51 C61 1.371(16) . ? C61 C71 1.398(16) . ? O12 C12 1.240(13) . ? O22 C12 1.292(13) . ? C12 C22 1.520(15) . ? C22 C32 1.385(15) . ? C22 C72 1.389(15) . ? C32 C42 1.415(16) . ? C42 C52 1.389(16) . ? C52 C62 1.376(16) . ? C62 C72 1.415(16) . ? C1O C2O 1.348(14) . ? C2O N3O 1.180(14) . ? C1P C2P 1.340(15) . ? C2P N3P 1.200(15) . ? C1Q C2Q 1.360(15) . ? C2Q N3Q 1.197(14) . ? C1R C2R 1.372(14) . ? C2R N3R 1.182(13) . ? C1S C2S 1.337(16) . ? C2S N3S 1.227(16) . ? C1T C2T 1.327(15) . ? C2T N3T 1.194(15) . ? C1U C2U 1.316(16) . ? C2U N3U 1.190(16) . ? C1V C2V 1.336(16) . ? C2V N3V 1.210(16) . ? C1X C2X 1.338(16) . ? C2X N3X 1.211(16) . ? C1Y C2Y 1.315(16) . ? C2Y N3Y 1.204(16) . ? C1Z C2Z 1.342(16) . ? C2Z N3Z 1.201(16) . ? 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 O6A Co1 O11 97.5(4) . . ? O6A Co1 O6J 91.4(4) . . ? O11 Co1 O6J 89.5(4) . . ? O6A Co1 O6K 175.4(4) . . ? O11 Co1 O6K 87.1(4) . . ? O6J Co1 O6K 87.9(4) . . ? O6A Co1 O124 89.7(3) . . ? O11 Co1 O124 88.1(3) . . ? O6J Co1 O124 177.5(4) . . ? O6K Co1 O124 91.2(3) . . ? O6A Co1 O6C 85.7(4) . . ? O11 Co1 O6C 176.4(4) . . ? O6J Co1 O6C 88.8(4) . . ? O6K Co1 O6C 89.7(3) . . ? O124 Co1 O6C 93.6(3) . . ? O21 Co2 O124 106.2(4) . . ? O21 Co2 N1B 111.4(4) . . ? O124 Co2 N1B 122.7(4) . . ? O21 Co2 N1A 112.8(4) . . ? O124 Co2 N1A 109.6(4) . . ? N1B Co2 N1A 93.7(4) . . ? O6F Co3 O6B 170.4(4) . . ? O6F Co3 O2W 94.0(4) . . ? O6B Co3 O2W 92.9(4) . . ? O6F Co3 O6D 84.6(4) . . ? O6B Co3 O6D 88.4(4) . . ? O2W Co3 O6D 178.5(4) . . ? O6F Co3 O1W 94.1(4) . . ? O6B Co3 O1W 92.9(4) . . ? O2W Co3 O1W 87.3(4) . . ? O6D Co3 O1W 93.3(4) . . ? O6F Co3 O6H 86.9(4) . . ? O6B Co3 O6H 86.1(4) . . ? O2W Co3 O6H 92.1(3) . . ? O6D Co3 O6H 87.3(3) . . ? O1W Co3 O6H 178.9(4) . . ? O6F Co3 Na1 47.5(3) . . ? O6B Co3 Na1 123.1(3) . . ? O2W Co3 Na1 116.6(3) . . ? O6D Co3 Na1 62.0(3) . . ? O1W Co3 Na1 132.9(3) . . ? O6H Co3 Na1 48.2(3) . . ? O22 Co4 O124 100.5(4) . . ? O22 Co4 N1D 132.6(4) . . ? O124 Co4 N1D 104.4(4) . . ? O22 Co4 N1C 120.8(4) . . ? O124 Co4 N1C 101.3(4) . . ? N1D Co4 N1C 93.0(4) . . ? N1I Co5 N1K 96.2(4) . . ? N1I Co5 S2H 96.0(3) . . ? N1K Co5 S2H 108.7(3) . . ? N1I Co5 S2J 168.3(3) . . ? N1K Co5 S2J 95.4(3) . . ? S2H Co5 S2J 82.04(16) . . ? N1I Co5 S2I 71.4(3) . . ? N1K Co5 S2I 159.2(3) . . ? S2H Co5 S2I 89.62(17) . . ? S2J Co5 S2I 96.99(16) . . ? N1I Co5 S2K 93.0(3) . . ? N1K Co5 S2K 70.6(3) . . ? S2H Co5 S2K 171.01(17) . . ? S2J Co5 S2K 89.08(16) . . ? S2I Co5 S2K 92.85(17) . . ? N1G Co6 N1F 98.2(4) . . ? N1G Co6 N1E 95.3(4) . . ? N1F Co6 N1E 101.2(4) . . ? N1G Co6 S2F 93.9(3) . . ? N1F Co6 S2F 72.0(3) . . ? N1E Co6 S2F 169.3(3) . . ? N1G Co6 S2G 71.6(3) . . ? N1F Co6 S2G 162.0(3) . . ? N1E Co6 S2G 94.6(3) . . ? S2F Co6 S2G 93.46(16) . . ? N1G Co6 S2E 161.0(3) . . ? N1F Co6 S2E 97.4(4) . . ? N1E Co6 S2E 71.0(3) . . ? S2F Co6 S2E 101.22(16) . . ? S2G Co6 S2E 95.76(17) . . ? O6E Na1 O6I 125.8(4) . . ? O6E Na1 O6F 92.7(4) . . ? O6I Na1 O6F 132.1(4) . . ? O6E Na1 O6H 147.7(4) . . ? O6I Na1 O6H 83.7(3) . . ? O6F Na1 O6H 71.2(3) . . ? O6E Na1 O22 76.2(3) . . ? O6I Na1 O22 86.7(3) . . ? O6F Na1 O22 134.2(4) . . ? O6H Na1 O22 94.9(3) . . ? O6E Na1 O6G 77.8(3) . . ? O6I Na1 O6G 79.6(3) . . ? O6F Na1 O6G 82.8(3) . . ? O6H Na1 O6G 125.4(4) . . ? O22 Na1 O6G 135.0(4) . . ? O6E Na1 O6D 84.0(3) . . ? O6I Na1 O6D 139.6(4) . . ? O6F Na1 O6D 60.7(3) . . ? O6H Na1 O6D 63.7(3) . . ? O22 Na1 O6D 73.9(3) . . ? O6G Na1 O6D 138.2(3) . . ? O6E Na1 C6E 21.2(3) . . ? O6I Na1 C6E 147.0(4) . . ? O6F Na1 C6E 74.3(3) . . ? O6H Na1 C6E 128.1(4) . . ? O22 Na1 C6E 82.5(3) . . ? O6G Na1 C6E 86.3(3) . . ? O6D Na1 C6E 65.9(3) . . ? O6E Na1 Co3 112.0(3) . . ? O6I Na1 Co3 122.1(3) . . ? O6F Na1 Co3 37.9(2) . . ? O6H Na1 Co3 39.8(2) . . ? O22 Na1 Co3 105.6(3) . . ? O6G Na1 Co3 118.1(3) . . ? O6D Na1 Co3 38.29(18) . . ? C6E Na1 Co3 90.9(3) . . ? Co2 O124 Co4 123.0(5) . . ? Co2 O124 Co1 101.4(4) . . ? Co4 O124 Co1 105.9(4) . . ? C2A N1A C6A 115.2(11) . . ? C2A N1A Co2 132.6(9) . . ? C6A N1A Co2 112.1(9) . . ? N1A C2A N3A 127.4(12) . . ? N1A C2A S2AB 124.1(10) . . ? N3A C2A S2AB 108.4(10) . . ? C2B S2AB C2A 111.6(7) . . ? C2A N3A C4A 111.4(11) . . ? N5A C4A N3A 128.7(12) . . ? N5A C4A N41A 115.8(12) . . ? N3A C4A N41A 115.5(12) . . ? C4A N41A C44A 122.0(12) . . ? C4A N41A C42A 119.1(12) . . ? C44A N41A C42A 118.5(11) . . ? C43A C42A N41A 111.7(11) . . ? N41A C44A C45A 111.4(12) . . ? C6A N5A C4A 113.8(12) . . ? O6A C6A N5A 119.1(13) . . ? O6A C6A N1A 117.5(12) . . ? N5A C6A N1A 123.3(13) . . ? C6A O6A Co1 149.2(9) . . ? C2B N1B C6B 115.7(11) . . ? C2B N1B Co2 132.9(9) . . ? C6B N1B Co2 111.2(9) . . ? N1B C2B N3B 126.3(12) . . ? N1B C2B S2AB 123.4(10) . . ? N3B C2B S2AB 110.3(10) . . ? C2B N3B C4B 113.8(12) . . ? N5B C4B N3B 126.0(13) . . ? N5B C4B N41B 117.1(12) . . ? N3B C4B N41B 116.9(13) . . ? C4B N41B C42B 120.4(13) . . ? C4B N41B C44B 121.6(13) . . ? C42B N41B C44B 117.3(13) . . ? N41B C42B C43B 114.9(14) . . ? N41B C44B C45B 107.9(14) . . ? C4B N5B C6B 116.6(12) . . ? O6B C6B N5B 124.2(12) . . ? O6B C6B N1B 114.4(12) . . ? N5B C6B N1B 121.3(12) . . ? C6B O6B Co3 129.0(9) . . ? C2C N1C C6C 116.1(11) . . ? C2C N1C Co4 130.5(9) . . ? C6C N1C Co4 112.2(9) . . ? N1C C2C N3C 126.4(12) . . ? N1C C2C S2CD 125.1(10) . . ? N3C C2C S2CD 108.2(10) . . ? C2D S2CD C2C 111.7(7) . . ? C2C N3C C4C 112.9(12) . . ? N3C C4C N5C 127.5(12) . . ? N3C C4C N41C 113.5(12) . . ? N5C C4C N41C 118.9(12) . . ? C4C N41C C42C 120.8(12) . . ? C4C N41C C44C 119.5(11) . . ? C42C N41C C44C 119.4(12) . . ? C43C C42C N41C 110.0(14) . . ? C45C C44C N41C 112.8(12) . . ? C6C N5C C4C 113.5(11) . . ? O6C C6C N5C 120.4(12) . . ? O6C C6C N1C 116.5(12) . . ? N5C C6C N1C 123.1(12) . . ? C6C O6C Co1 123.5(9) . . ? C2D N1D C6D 117.6(11) . . ? C2D N1D Co4 133.9(9) . . ? C6D N1D Co4 107.4(9) . . ? N1D C2D N3D 125.9(12) . . ? N1D C2D S2CD 122.9(10) . . ? N3D C2D S2CD 111.1(10) . . ? C2D N3D C4D 113.3(11) . . ? N5D C4D N3D 126.2(12) . . ? N5D C4D N41D 118.6(12) . . ? N3D C4D N41D 115.2(12) . . ? C4D N41D C44D 121.2(12) . . ? C4D N41D C42D 119.4(12) . . ? C44D N41D C42D 119.3(12) . . ? C43D C42D N41D 112.2(12) . . ? N41D C44D C45D 109.3(12) . . ? C4D N5D C6D 117.3(12) . . ? O6D C6D N5D 124.6(12) . . ? O6D C6D N1D 116.0(12) . . ? N5D C6D N1D 119.4(12) . . ? C6D O6D Co3 124.6(9) . . ? C6D O6D Na1 155.6(9) . . ? Co3 O6D Na1 79.7(3) . . ? C2E N1E C6E 118.9(10) . . ? C2E N1E Co6 102.6(7) . . ? C6E N1E Co6 138.5(8) . . ? N3E C2E N1E 126.5(10) . . ? N3E C2E S2E 125.9(9) . . ? N1E C2E S2E 107.5(8) . . ? C2E S2E Co6 78.4(4) . . ? C2E N3E C4E 112.8(10) . . ? N5E C4E N3E 123.6(10) . . ? N5E C4E N41E 117.7(10) . . ? N3E C4E N41E 118.7(10) . . ? C4E N41E C44E 118.4(10) . . ? C4E N41E C42E 122.9(10) . . ? C44E N41E C42E 116.9(10) . . ? C43E C42E N41E 112.3(11) . . ? C45E C44E N41E 114.1(12) . . ? C4E N5E C6E 121.0(10) . . ? O6E C6E N1E 122.9(11) . . ? O6E C6E N5E 120.3(11) . . ? N1E C6E N5E 116.8(10) . . ? O6E C6E Na1 42.4(7) . . ? N1E C6E Na1 108.7(8) . . ? N5E C6E Na1 118.5(8) . . ? C6E O6E Na1 116.4(9) . . ? C2F N1F C6F 118.2(10) . . ? C2F N1F Co6 101.9(7) . . ? C6F N1F Co6 139.6(8) . . ? N3F C2F N1F 127.4(10) . . ? N3F C2F S2F 124.9(9) . . ? N1F C2F S2F 107.5(8) . . ? C2F S2F Co6 78.5(4) . . ? C2F N3F C4F 112.3(10) . . ? N5F C4F N41F 116.6(10) . . ? N5F C4F N3F 124.8(10) . . ? N41F C4F N3F 118.5(11) . . ? C4F N41F C42F 125.3(11) . . ? C4F N41F C44F 118.5(10) . . ? C42F N41F C44F 116.2(10) . . ? N41F C42F C43F 111.9(11) . . ? N41F C44F C45F 111.8(11) . . ? C4F N5F C6F 119.0(10) . . ? O6F C6F N1F 122.0(11) . . ? O6F C6F N5F 119.8(11) . . ? N1F C6F N5F 118.1(10) . . ? C6F O6F Co3 130.4(9) . . ? C6F O6F Na1 123.3(9) . . ? Co3 O6F Na1 94.6(3) . . ? C2G N1G C6G 117.7(10) . . ? C2G N1G Co6 102.2(7) . . ? C6G N1G Co6 139.6(8) . . ? N3G C2G N1G 127.9(10) . . ? N3G C2G S2G 124.7(9) . . ? N1G C2G S2G 107.4(8) . . ? C2G S2G Co6 78.8(4) . . ? C2G N3G C4G 112.5(10) . . ? N3G C4G N5G 124.3(11) . . ? N3G C4G N41G 117.4(11) . . ? N5G C4G N41G 117.9(11) . . ? C4G N41G C42G 124.0(12) . . ? C4G N41G C44G 119.3(12) . . ? C42G N41G C44G 116.7(12) . . ? N41G C42G C43G 110.8(13) . . ? C45G C44G N41G 110.1(15) . . ? C4G N5G C6G 120.6(11) . . ? O6G C6G N1G 123.0(11) . . ? O6G C6G N5G 120.3(11) . . ? N1G C6G N5G 116.7(10) . . ? C6G O6G Na1 119.8(9) . . ? C2H N1H C6H 121.1(10) . . ? N3H C2H N1H 122.6(10) . . ? N3H C2H S2H 116.4(9) . . ? N1H C2H S2H 120.8(9) . . ? C2H S2H Co5 115.0(5) . . ? C2H N3H C4H 115.0(10) . . ? N5H C4H N41H 117.3(11) . . ? N5H C4H N3H 125.4(11) . . ? N41H C4H N3H 117.3(11) . . ? C4H N41H C42H 123.5(11) . . ? C4H N41H C44H 119.5(12) . . ? C42H N41H C44H 115.4(12) . . ? C43H C42H N41H 111.2(13) . . ? C45H C44H N41H 103.1(14) . . ? C4H N5H C6H 117.0(10) . . ? O6H C6H N5H 120.8(10) . . ? O6H C6H N1H 120.7(10) . . ? N5H C6H N1H 118.4(10) . . ? C6H O6H Co3 127.5(8) . . ? C6H O6H Na1 134.0(8) . . ? Co3 O6H Na1 92.0(3) . . ? C6I N1I C2I 118.9(10) . . ? C6I N1I Co5 139.1(8) . . ? C2I N1I Co5 101.6(7) . . ? N3I C2I N1I 127.0(10) . . ? N3I C2I S2I 125.1(9) . . ? N1I C2I S2I 107.8(8) . . ? C2I S2I Co5 79.0(4) . . ? C2I N3I C4I 112.9(10) . . ? N5I C4I N3I 123.3(11) . . ? N5I C4I N41I 118.6(11) . . ? N3I C4I N41I 118.1(11) . . ? C4I N41I C44I 119.3(11) . . ? C4I N41I C42I 121.6(12) . . ? C44I N41I C42I 117.1(12) . . ? C43I C42I N41I 100.0(14) . . ? C45I C44I N41I 114.2(12) . . ? C4I N5I C6I 122.1(10) . . ? O6I C6I N1I 123.7(11) . . ? O6I C6I N5I 120.7(11) . . ? N1I C6I N5I 115.6(10) . . ? C6I O6I Na1 132.3(8) . . ? C2J N1J C6J 121.6(10) . . ? N1J C2J N3J 120.4(10) . . ? N1J C2J S2J 122.8(9) . . ? N3J C2J S2J 116.7(9) . . ? C2J S2J Co5 111.1(5) . . ? C2J N3J C4J 113.9(10) . . ? N5J C4J N3J 128.4(11) . . ? N5J C4J N41J 115.1(11) . . ? N3J C4J N41J 116.3(11) . . ? C4J N41J C42J 123.1(11) . . ? C4J N41J C44J 120.7(11) . . ? C42J N41J C44J 116.2(11) . . ? N41J C42J C43J 112.5(12) . . ? C45J C44J N41J 108.9(13) . . ? C4J N5J C6J 114.1(11) . . ? O6J C6J N1J 122.8(11) . . ? O6J C6J N5J 117.8(11) . . ? N1J C6J N5J 119.4(11) . . ? C6J O6J Co1 139.2(9) . . ? C2K N1K C6K 117.7(10) . . ? C2K N1K Co5 102.2(7) . . ? C6K N1K Co5 140.1(8) . . ? N3K C2K N1K 127.6(10) . . ? N3K C2K S2K 123.7(9) . . ? N1K C2K S2K 108.4(8) . . ? C2K S2K Co5 78.5(4) . . ? C2K N3K C4K 112.6(10) . . ? N3K C4K N41K 118.5(11) . . ? N3K C4K N5K 123.7(11) . . ? N41K C4K N5K 117.6(11) . . ? C4K N41K C42K 122.7(11) . . ? C4K N41K C44K 120.6(11) . . ? C42K N41K C44K 116.1(11) . . ? C43K C42K N41K 111.5(11) . . ? C45K C44K N41K 112.1(12) . . ? C4K N5K C6K 120.2(10) . . ? O6K C6K N1K 122.0(11) . . ? O6K C6K N5K 121.1(11) . . ? N1K C6K N5K 116.9(10) . . ? C6K O6K Co1 128.9(8) . . ? C11 O11 Co1 131.6(10) . . ? C11 O21 Co2 123.3(9) . . ? O11 C11 O21 126.5(13) . . ? O11 C11 C21 117.9(12) . . ? O21 C11 C21 115.6(12) . . ? C31 C21 C71 122.1(13) . . ? C31 C21 C11 117.2(12) . . ? C71 C21 C11 120.7(12) . . ? C21 C31 C41 119.1(14) . . ? C51 C41 C31 118.5(15) . . ? C61 C51 C41 121.8(15) . . ? C51 C61 C71 120.7(15) . . ? C21 C71 C61 117.5(13) . . ? C12 O22 Co4 99.6(8) . . ? C12 O22 Na1 115.7(8) . . ? Co4 O22 Na1 110.5(4) . . ? O12 C12 O22 122.7(13) . . ? O12 C12 C22 120.7(13) . . ? O22 C12 C22 116.7(12) . . ? C32 C22 C72 121.2(12) . . ? C32 C22 C12 118.4(12) . . ? C72 C22 C12 120.4(12) . . ? C22 C32 C42 119.0(14) . . ? C52 C42 C32 120.0(15) . . ? C62 C52 C42 120.5(15) . . ? C52 C62 C72 120.2(15) . . ? C22 C72 C62 119.1(13) . . ? N3O C2O C1O 174(2) . . ? N3P C2P C1P 171(3) . . ? N3Q C2Q C1Q 176(3) . . ? N3R C2R C1R 178(2) . . ? N3S C2S C1S 143(3) . . ? N3T C2T C1T 175(3) . . ? N3U C2U C1U 161(4) . . ? N3V C2V C1V 167(4) . . ? N3X C2X C1X 159(4) . . ? N3Y C2Y C1Y 173(4) . . ? N3Z C2Z C1Z 162(5) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.977 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.121