# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Paul O'Brien" _publ_contact_author_email PAUL.OBRIEN@MANCHESTER.AC.UK _publ_section_title ; Metal Complexes of Thiobiurets and Dithiobiurets: Novel Single Source Precursors for Metal Sulfide Thin Film Nanostructures ; loop_ _publ_author_name "Paul O'Brien" 'Mohammad A. Malik' 'James Raftery' 'Karthik Ramasamy' # Attachment 's2949m.cif' data_s2949m _database_code_depnum_ccdc_archive 'CCDC 692257' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 N6 S4 Zn' _chemical_formula_weight 558.19 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 9.0920(8) _cell_length_b 11.5052(10) _cell_length_c 26.955(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.799(2) _cell_angle_gamma 90.00 _cell_volume 2786.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3247 _cell_measurement_theta_min 2.338 _cell_measurement_theta_max 23.681 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 1.200 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23865 _diffrn_reflns_av_R_equivalents 0.0642 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 28.29 _reflns_number_total 6650 _reflns_number_gt 4163 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6650 _refine_ls_number_parameters 288 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0360 _refine_ls_wR_factor_ref 0.0541 _refine_ls_wR_factor_gt 0.0492 _refine_ls_goodness_of_fit_ref 0.743 _refine_ls_restrained_S_all 0.743 _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 C1 C 0.4063(3) 0.4859(2) 0.25276(9) 0.0325(7) Uani 1 1 d . . . H1A H 0.4094 0.4315 0.2250 0.049 Uiso 1 1 calc R . . H1B H 0.4617 0.4533 0.2837 0.049 Uiso 1 1 calc R . . H1C H 0.4514 0.5599 0.2452 0.049 Uiso 1 1 calc R . . C2 C 0.2467(3) 0.5061(2) 0.25963(8) 0.0233(6) Uani 1 1 d . . . H2A H 0.2073 0.4340 0.2728 0.028 Uiso 1 1 calc R . . H2B H 0.2439 0.5679 0.2850 0.028 Uiso 1 1 calc R . . C3 C 0.0723(3) 0.46271(19) 0.18190(9) 0.0214(6) Uani 1 1 d . . . C4 C -0.0828(3) 0.45175(19) 0.10221(9) 0.0211(5) Uani 1 1 d . . . C5 C -0.3138(3) 0.4290(2) 0.04247(9) 0.0289(6) Uani 1 1 d . . . H5A H -0.4196 0.4287 0.0473 0.035 Uiso 1 1 calc R . . H5B H -0.2824 0.3472 0.0395 0.035 Uiso 1 1 calc R . . C6 C -0.3002(3) 0.4919(2) -0.00571(9) 0.0365(7) Uani 1 1 d . . . H6A H -0.3317 0.5729 -0.0032 0.055 Uiso 1 1 calc R . . H6B H -0.3636 0.4539 -0.0337 0.055 Uiso 1 1 calc R . . H6C H -0.1964 0.4898 -0.0115 0.055 Uiso 1 1 calc R . . C7 C 0.1439(3) 0.66349(18) 0.20002(9) 0.0265(6) Uani 1 1 d . . . H7A H 0.1716 0.7099 0.2310 0.032 Uiso 1 1 calc R . . H7B H 0.0404 0.6842 0.1856 0.032 Uiso 1 1 calc R . . C8 C 0.2460(3) 0.6959(2) 0.16280(9) 0.0372(7) Uani 1 1 d . . . H8A H 0.3497 0.6838 0.1782 0.056 Uiso 1 1 calc R . . H8B H 0.2310 0.7777 0.1533 0.056 Uiso 1 1 calc R . . H8C H 0.2235 0.6470 0.1328 0.056 Uiso 1 1 calc R . . C9 C -0.2988(3) 0.56803(19) 0.11343(9) 0.0288(6) Uani 1 1 d . . . H9A H -0.3769 0.6071 0.0896 0.035 Uiso 1 1 calc R . . H9B H -0.2254 0.6276 0.1274 0.035 Uiso 1 1 calc R . . C10 C -0.3686(3) 0.5153(2) 0.15557(10) 0.0467(8) Uani 1 1 d . . . H10A H -0.4433 0.4578 0.1418 0.070 Uiso 1 1 calc R . . H10B H -0.4163 0.5766 0.1727 0.070 Uiso 1 1 calc R . . H10C H -0.2915 0.4773 0.1795 0.070 Uiso 1 1 calc R . . C11 C -0.0526(3) -0.23297(19) 0.05857(8) 0.0296(6) Uani 1 1 d . . . H11A H 0.0092 -0.3015 0.0552 0.044 Uiso 1 1 calc R . . H11B H -0.1551 -0.2485 0.0428 0.044 Uiso 1 1 calc R . . H11C H -0.0511 -0.2155 0.0942 0.044 Uiso 1 1 calc R . . C12 C 0.0084(2) -0.12947(19) 0.03293(8) 0.0233(6) Uani 1 1 d . . . H12A H 0.0053 -0.1474 -0.0031 0.028 Uiso 1 1 calc R . . H12B H -0.0566 -0.0614 0.0355 0.028 Uiso 1 1 calc R . . C13 C 0.1972(3) -0.01716(19) 0.09002(8) 0.0200(5) Uani 1 1 d . . . C14 C 0.4191(3) 0.08616(19) 0.12330(8) 0.0203(6) Uani 1 1 d . . . C15 C 0.6631(2) 0.1570(2) 0.16795(9) 0.0274(6) Uani 1 1 d . . . H15A H 0.6505 0.2190 0.1422 0.033 Uiso 1 1 calc R . . H15B H 0.7627 0.1221 0.1683 0.033 Uiso 1 1 calc R . . C16 C 0.6552(3) 0.2106(2) 0.21904(9) 0.0385(7) Uani 1 1 d . . . H16A H 0.5630 0.2554 0.2175 0.058 Uiso 1 1 calc R . . H16B H 0.7408 0.2621 0.2284 0.058 Uiso 1 1 calc R . . H16C H 0.6568 0.1488 0.2441 0.058 Uiso 1 1 calc R . . C17 C 0.2784(3) -0.16591(19) 0.03608(9) 0.0268(6) Uani 1 1 d . . . H17A H 0.2402 -0.2442 0.0258 0.032 Uiso 1 1 calc R . . H17B H 0.3636 -0.1755 0.0634 0.032 Uiso 1 1 calc R . . C18 C 0.3315(3) -0.1062(2) -0.00828(9) 0.0383(7) Uani 1 1 d . . . H18A H 0.2497 -0.1029 -0.0365 0.057 Uiso 1 1 calc R . . H18B H 0.4146 -0.1502 -0.0182 0.057 Uiso 1 1 calc R . . H18C H 0.3645 -0.0272 0.0013 0.057 Uiso 1 1 calc R . . C19 C 0.5888(3) -0.04911(19) 0.17377(9) 0.0275(6) Uani 1 1 d . . . H19A H 0.4966 -0.0928 0.1765 0.033 Uiso 1 1 calc R . . H19B H 0.6465 -0.0422 0.2079 0.033 Uiso 1 1 calc R . . C20 C 0.6791(3) -0.1164(2) 0.14105(10) 0.0413(8) Uani 1 1 d . . . H20A H 0.6201 -0.1281 0.1078 0.062 Uiso 1 1 calc R . . H20B H 0.7065 -0.1920 0.1565 0.062 Uiso 1 1 calc R . . H20C H 0.7696 -0.0728 0.1376 0.062 Uiso 1 1 calc R . . N1 N 0.1492(2) 0.53979(15) 0.21327(7) 0.0205(5) Uani 1 1 d . . . N2 N -0.0163(2) 0.50546(15) 0.14324(7) 0.0222(5) Uani 1 1 d . . . N3 N -0.2246(2) 0.48121(15) 0.08642(7) 0.0222(5) Uani 1 1 d . . . N4 N 0.1613(2) -0.09941(15) 0.05473(7) 0.0203(5) Uani 1 1 d . . . N5 N 0.3410(2) -0.00660(15) 0.10811(7) 0.0215(5) Uani 1 1 d . . . N6 N 0.5491(2) 0.06746(16) 0.15421(7) 0.0225(5) Uani 1 1 d . . . S1 S 0.08420(7) 0.31433(5) 0.19774(2) 0.02555(16) Uani 1 1 d . . . S2 S 0.00446(7) 0.36221(5) 0.06408(2) 0.02707(16) Uani 1 1 d . . . S3 S 0.05207(7) 0.05193(5) 0.11366(2) 0.02168(15) Uani 1 1 d . . . S4 S 0.37664(6) 0.22841(5) 0.10291(2) 0.02606(15) Uani 1 1 d . . . Zn1 Zn 0.13824(3) 0.24103(2) 0.122504(10) 0.02077(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 C1 0.0343(17) 0.0376(16) 0.0249(15) 0.0002(13) 0.0028(13) 0.0066(13) C2 0.0300(15) 0.0237(14) 0.0162(14) -0.0037(11) 0.0039(12) -0.0012(11) C3 0.0222(14) 0.0196(14) 0.0240(14) -0.0028(11) 0.0090(11) 0.0008(11) C4 0.0225(14) 0.0154(13) 0.0257(14) 0.0022(11) 0.0045(11) -0.0015(11) C5 0.0207(14) 0.0223(14) 0.0413(17) -0.0099(13) -0.0025(12) -0.0001(11) C6 0.0296(16) 0.0384(17) 0.0364(17) -0.0058(14) -0.0116(13) 0.0031(13) C7 0.0320(16) 0.0180(14) 0.0274(15) -0.0032(11) -0.0025(12) 0.0012(12) C8 0.0440(18) 0.0276(15) 0.0390(17) 0.0086(13) 0.0027(14) -0.0071(13) C9 0.0232(14) 0.0215(14) 0.0429(17) -0.0081(12) 0.0086(13) 0.0029(11) C10 0.050(2) 0.0339(17) 0.064(2) -0.0132(15) 0.0355(17) -0.0077(14) C11 0.0335(15) 0.0262(15) 0.0292(14) -0.0014(12) 0.0054(12) -0.0074(12) C12 0.0235(14) 0.0258(14) 0.0206(14) -0.0060(11) 0.0031(11) -0.0061(11) C13 0.0248(14) 0.0162(13) 0.0192(13) 0.0050(10) 0.0043(11) -0.0010(11) C14 0.0219(14) 0.0210(14) 0.0195(13) -0.0032(11) 0.0079(11) 0.0013(11) C15 0.0164(14) 0.0258(15) 0.0392(16) -0.0056(12) 0.0015(12) -0.0003(11) C16 0.0433(17) 0.0307(16) 0.0395(17) -0.0086(13) -0.0003(14) -0.0051(13) C17 0.0265(15) 0.0224(14) 0.0314(15) -0.0118(12) 0.0044(12) -0.0003(12) C18 0.0322(17) 0.0394(17) 0.0476(19) -0.0153(14) 0.0200(14) -0.0080(13) C19 0.0239(15) 0.0229(14) 0.0338(16) 0.0015(12) -0.0021(12) 0.0015(12) C20 0.0321(17) 0.0251(15) 0.066(2) -0.0073(15) 0.0054(15) 0.0044(13) N1 0.0239(12) 0.0184(11) 0.0187(11) -0.0026(9) 0.0021(9) -0.0005(9) N2 0.0258(12) 0.0168(11) 0.0225(12) -0.0026(9) -0.0013(10) 0.0017(9) N3 0.0198(11) 0.0198(11) 0.0266(12) -0.0066(9) 0.0026(9) -0.0006(9) N4 0.0214(12) 0.0179(11) 0.0218(11) -0.0044(9) 0.0043(9) -0.0019(9) N5 0.0209(12) 0.0179(11) 0.0251(12) -0.0047(9) 0.0011(9) -0.0005(9) N6 0.0191(11) 0.0174(11) 0.0298(12) -0.0015(9) -0.0003(9) -0.0001(9) S1 0.0375(4) 0.0183(3) 0.0210(3) -0.0012(3) 0.0049(3) 0.0003(3) S2 0.0280(4) 0.0311(4) 0.0214(3) -0.0024(3) 0.0012(3) 0.0112(3) S3 0.0227(3) 0.0213(3) 0.0216(3) -0.0039(3) 0.0054(3) -0.0026(3) S4 0.0223(3) 0.0195(3) 0.0367(4) 0.0042(3) 0.0054(3) 0.0003(3) Zn1 0.02219(16) 0.01825(15) 0.02144(15) -0.00233(13) 0.00196(11) 0.00137(13) _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 C1 C2 1.509(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 N1 1.469(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.312(3) . ? C3 N1 1.345(3) . ? C3 S1 1.759(2) . ? C4 N2 1.329(3) . ? C4 N3 1.338(3) . ? C4 S2 1.731(2) . ? C5 N3 1.459(3) . ? C5 C6 1.508(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N1 1.466(3) . ? C7 C8 1.514(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N3 1.460(3) . ? C9 C10 1.511(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.523(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N4 1.466(3) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N5 1.329(3) . ? C13 N4 1.346(3) . ? C13 S3 1.742(2) . ? C14 N5 1.313(3) . ? C14 N6 1.355(3) . ? C14 S4 1.751(2) . ? C15 N6 1.468(3) . ? C15 C16 1.520(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 N4 1.461(3) . ? C17 C18 1.520(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N6 1.466(3) . ? C19 C20 1.507(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? S1 Zn1 2.3174(7) . ? S2 Zn1 2.3058(7) . ? S3 Zn1 2.3124(7) . ? S4 Zn1 2.3126(7) . ? 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 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 C1 113.74(18) . . ? N1 C2 H2A 108.8 . . ? C1 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C1 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N2 C3 N1 116.7(2) . . ? N2 C3 S1 124.34(18) . . ? N1 C3 S1 118.73(17) . . ? N2 C4 N3 116.1(2) . . ? N2 C4 S2 125.41(18) . . ? N3 C4 S2 117.94(17) . . ? N3 C5 C6 113.11(19) . . ? N3 C5 H5A 109.0 . . ? C6 C5 H5A 109.0 . . ? N3 C5 H5B 109.0 . . ? C6 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C7 C8 113.54(19) . . ? N1 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N1 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 112.30(19) . . ? N3 C9 H9A 109.1 . . ? C10 C9 H9A 109.1 . . ? N3 C9 H9B 109.1 . . ? C10 C9 H9B 109.1 . . ? H9A C9 H9B 107.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4 C12 C11 113.04(19) . . ? N4 C12 H12A 109.0 . . ? C11 C12 H12A 109.0 . . ? N4 C12 H12B 109.0 . . ? C11 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? N5 C13 N4 116.2(2) . . ? N5 C13 S3 125.55(18) . . ? N4 C13 S3 117.66(17) . . ? N5 C14 N6 116.3(2) . . ? N5 C14 S4 125.39(18) . . ? N6 C14 S4 118.13(17) . . ? N6 C15 C16 112.58(19) . . ? N6 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? N6 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N4 C17 C18 111.71(19) . . ? N4 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? N4 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 112.7(2) . . ? N6 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N6 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C3 N1 C7 119.49(19) . . ? C3 N1 C2 123.26(19) . . ? C7 N1 C2 117.17(18) . . ? C3 N2 C4 129.3(2) . . ? C4 N3 C5 122.90(19) . . ? C4 N3 C9 120.71(19) . . ? C5 N3 C9 116.39(18) . . ? C13 N4 C17 120.04(19) . . ? C13 N4 C12 124.16(19) . . ? C17 N4 C12 115.80(18) . . ? C14 N5 C13 130.1(2) . . ? C14 N6 C19 120.67(19) . . ? C14 N6 C15 124.01(19) . . ? C19 N6 C15 115.21(18) . . ? C3 S1 Zn1 98.86(8) . . ? C4 S2 Zn1 101.31(8) . . ? C13 S3 Zn1 101.74(8) . . ? C14 S4 Zn1 99.01(8) . . ? S2 Zn1 S3 111.31(2) . . ? S2 Zn1 S4 107.27(2) . . ? S3 Zn1 S4 103.41(2) . . ? S2 Zn1 S1 102.55(2) . . ? S3 Zn1 S1 108.59(2) . . ? S4 Zn1 S1 123.66(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C3 N1 C7 -6.9(3) . . . . ? S1 C3 N1 C7 178.35(16) . . . . ? N2 C3 N1 C2 176.6(2) . . . . ? S1 C3 N1 C2 1.9(3) . . . . ? C8 C7 N1 C3 -80.0(3) . . . . ? C8 C7 N1 C2 96.7(2) . . . . ? C1 C2 N1 C3 91.3(3) . . . . ? C1 C2 N1 C7 -85.2(2) . . . . ? N1 C3 N2 C4 166.3(2) . . . . ? S1 C3 N2 C4 -19.3(4) . . . . ? N3 C4 N2 C3 137.7(2) . . . . ? S2 C4 N2 C3 -50.7(3) . . . . ? N2 C4 N3 C5 -179.03(19) . . . . ? S2 C4 N3 C5 8.7(3) . . . . ? N2 C4 N3 C9 0.2(3) . . . . ? S2 C4 N3 C9 -172.06(16) . . . . ? C6 C5 N3 C4 -88.5(3) . . . . ? C6 C5 N3 C9 92.2(2) . . . . ? C10 C9 N3 C4 -87.2(3) . . . . ? C10 C9 N3 C5 92.1(2) . . . . ? N5 C13 N4 C17 -3.9(3) . . . . ? S3 C13 N4 C17 -175.72(16) . . . . ? N5 C13 N4 C12 175.56(19) . . . . ? S3 C13 N4 C12 3.8(3) . . . . ? C18 C17 N4 C13 -88.7(2) . . . . ? C18 C17 N4 C12 91.8(2) . . . . ? C11 C12 N4 C13 -95.6(2) . . . . ? C11 C12 N4 C17 83.8(2) . . . . ? N6 C14 N5 C13 159.5(2) . . . . ? S4 C14 N5 C13 -26.1(3) . . . . ? N4 C13 N5 C14 146.0(2) . . . . ? S3 C13 N5 C14 -43.0(3) . . . . ? N5 C14 N6 C19 -7.0(3) . . . . ? S4 C14 N6 C19 178.13(16) . . . . ? N5 C14 N6 C15 168.9(2) . . . . ? S4 C14 N6 C15 -5.9(3) . . . . ? C20 C19 N6 C14 92.0(3) . . . . ? C20 C19 N6 C15 -84.3(2) . . . . ? C16 C15 N6 C14 99.0(3) . . . . ? C16 C15 N6 C19 -84.8(2) . . . . ? N2 C3 S1 Zn1 55.7(2) . . . . ? N1 C3 S1 Zn1 -129.97(16) . . . . ? N2 C4 S2 Zn1 48.8(2) . . . . ? N3 C4 S2 Zn1 -139.68(16) . . . . ? N5 C13 S3 Zn1 47.2(2) . . . . ? N4 C13 S3 Zn1 -141.80(15) . . . . ? N5 C14 S4 Zn1 56.0(2) . . . . ? N6 C14 S4 Zn1 -129.63(16) . . . . ? C4 S2 Zn1 S3 113.97(8) . . . . ? C4 S2 Zn1 S4 -133.57(8) . . . . ? C4 S2 Zn1 S1 -1.97(8) . . . . ? C13 S3 Zn1 S2 109.33(8) . . . . ? C13 S3 Zn1 S4 -5.55(8) . . . . ? C13 S3 Zn1 S1 -138.50(8) . . . . ? C14 S4 Zn1 S2 -148.16(8) . . . . ? C14 S4 Zn1 S3 -30.41(8) . . . . ? C14 S4 Zn1 S1 93.13(8) . . . . ? C3 S1 Zn1 S2 -34.76(8) . . . . ? C3 S1 Zn1 S3 -152.65(8) . . . . ? C3 S1 Zn1 S4 86.16(8) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.860 _refine_diff_density_min -0.443 _refine_diff_density_rms 0.066 # Attachment 's2983m.cif' data_s2983m _database_code_depnum_ccdc_archive 'CCDC 715960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 N6 Ni O2 S2' _chemical_formula_weight 631.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_cell_setting monoclinic 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 21.787 _cell_length_b 13.777 _cell_length_c 11.925 _cell_angle_alpha 90.00 _cell_angle_beta 90.99 _cell_angle_gamma 90.00 _cell_volume 3578.9 _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2715 _cell_measurement_theta_min 2.5036 _cell_measurement_theta_max 28.3384 _exptl_absorpt_correction_T_min 0.74814 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_crystal_description plate _exptl_crystal_colour violet _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16324 _diffrn_reflns_av_R_equivalents 0.1107 _diffrn_reflns_av_sigmaI/netI 0.2717 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6984 _reflns_number_gt 2961 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _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^)+(0.0978P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6984 _refine_ls_number_parameters 345 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1877 _refine_ls_R_factor_gt 0.0781 _refine_ls_wR_factor_ref 0.2183 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 0.939 _refine_ls_restrained_S_all 0.939 _refine_ls_shift/su_max 0.036 _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 C1 C 0.42524(17) -0.0366(3) 0.3898(4) 0.0441(13) Uani 1 1 d . . . H1 H 0.4663 -0.0692 0.3922 0.053 Uiso 1 1 calc R . . C2 C 0.43386(19) 0.0548(3) 0.3260(4) 0.0573(15) Uani 1 1 d . . . H2A H 0.4539 0.0404 0.2549 0.086 Uiso 1 1 calc R . . H2B H 0.4596 0.0994 0.3702 0.086 Uiso 1 1 calc R . . H2C H 0.3938 0.0848 0.3108 0.086 Uiso 1 1 calc R . . C3 C 0.4078(2) -0.0201(4) 0.5131(4) 0.0675(17) Uani 1 1 d . . . H3A H 0.3701 0.0185 0.5159 0.101 Uiso 1 1 calc R . . H3B H 0.4411 0.0145 0.5522 0.101 Uiso 1 1 calc R . . H3C H 0.4011 -0.0829 0.5495 0.101 Uiso 1 1 calc R . . C4 C 0.41061(18) -0.1926(3) 0.2850(4) 0.0471(14) Uani 1 1 d . . . H4 H 0.3768 -0.2277 0.2443 0.056 Uiso 1 1 calc R . . C5 C 0.4355(2) -0.2617(4) 0.3751(4) 0.0777(18) Uani 1 1 d . . . H5A H 0.4700 -0.2309 0.4152 0.117 Uiso 1 1 calc R . . H5B H 0.4495 -0.3218 0.3398 0.117 Uiso 1 1 calc R . . H5C H 0.4030 -0.2767 0.4282 0.117 Uiso 1 1 calc R . . C6 C 0.4592(2) -0.1688(3) 0.1988(4) 0.0637(17) Uani 1 1 d . . . H6A H 0.4417 -0.1255 0.1416 0.096 Uiso 1 1 calc R . . H6B H 0.4732 -0.2289 0.1633 0.096 Uiso 1 1 calc R . . H6C H 0.4941 -0.1367 0.2362 0.096 Uiso 1 1 calc R . . C7 C 0.32250(17) -0.0866(2) 0.3230(3) 0.0287(11) Uani 1 1 d . . . C8 C 0.22768(17) -0.1555(3) 0.2664(3) 0.0269(10) Uani 1 1 d . A . C9 C 0.23573(18) -0.2838(3) 0.1216(3) 0.0342(11) Uani 1 1 d . . . H9 H 0.2046 -0.3191 0.0744 0.041 Uiso 1 1 calc R . . C10 C 0.27784(19) -0.2342(3) 0.0406(4) 0.0488(14) Uani 1 1 d . . . H10A H 0.2546 -0.1857 -0.0028 0.073 Uiso 1 1 calc R . . H10B H 0.2950 -0.2824 -0.0104 0.073 Uiso 1 1 calc R . . H10C H 0.3112 -0.2021 0.0824 0.073 Uiso 1 1 calc R . . C11 C 0.2681(2) -0.3616(3) 0.1926(4) 0.0464(13) Uani 1 1 d . . . H11A H 0.3036 -0.3329 0.2319 0.070 Uiso 1 1 calc R . . H11B H 0.2821 -0.4141 0.1438 0.070 Uiso 1 1 calc R . . H11C H 0.2395 -0.3877 0.2475 0.070 Uiso 1 1 calc R . . C12 C 0.13276(18) -0.2208(3) 0.1781(4) 0.0424(13) Uani 1 1 d . . . H12 H 0.1146 -0.1723 0.2304 0.051 Uiso 1 1 calc R . . C13 C 0.1142(2) -0.1907(3) 0.0592(4) 0.0597(16) Uani 1 1 d . . . H13A H 0.1332 -0.1282 0.0414 0.090 Uiso 1 1 calc R . . H13B H 0.0694 -0.1845 0.0538 0.090 Uiso 1 1 calc R . . H13C H 0.1279 -0.2400 0.0060 0.090 Uiso 1 1 calc R . . C14 C 0.10819(18) -0.3194(3) 0.2103(4) 0.0491(14) Uani 1 1 d . . . H14A H 0.1225 -0.3682 0.1569 0.074 Uiso 1 1 calc R . . H14B H 0.0632 -0.3178 0.2087 0.074 Uiso 1 1 calc R . . H14C H 0.1229 -0.3361 0.2859 0.074 Uiso 1 1 calc R . . C15 C 0.0456(2) 0.1208(5) 0.6558(4) 0.117(2) Uani 1 1 d . . . H15 H 0.0646 0.0616 0.6224 0.140 Uiso 1 1 calc R . . N4 N 0.09789(14) 0.1910(2) 0.6328(3) 0.0449(11) Uani 1 1 d G . . C20 C 0.0691(3) 0.3625(2) 0.5916(6) 0.090(2) Uani 1 1 d GD . . H20A H 0.0594 0.4226 0.6315 0.136 Uiso 1 1 calc R . . H20B H 0.0322 0.3386 0.5524 0.136 Uiso 1 1 calc R . . H20C H 0.1013 0.3753 0.5371 0.136 Uiso 1 1 calc R . . C21 C 0.14795(17) 0.1663(3) 0.5742(3) 0.0360(12) Uani 1 1 d . A . C22 C 0.24147(18) 0.2220(3) 0.4995(3) 0.0329(11) Uani 1 1 d . A . N6 N 0.27363(12) 0.30448(16) 0.4713(2) 0.0368(10) Uani 1 1 d G . . C23 C 0.24015(16) 0.39315(19) 0.5071(3) 0.096(2) Uani 1 1 d G A . H23 H 0.2047 0.3720 0.5532 0.115 Uiso 1 1 calc R . . C24 C 0.2143(2) 0.4478(3) 0.4046(4) 0.097(2) Uani 1 1 d G A . H24A H 0.2479 0.4644 0.3545 0.146 Uiso 1 1 calc R . . H24B H 0.1940 0.5074 0.4293 0.146 Uiso 1 1 calc R . . H24C H 0.1845 0.4065 0.3647 0.146 Uiso 1 1 calc R . . C25 C 0.2832(3) 0.4565(2) 0.5832(4) 0.118(3) Uani 1 1 d G A . H25A H 0.2974 0.4182 0.6477 0.177 Uiso 1 1 calc R . . H25B H 0.2605 0.5134 0.6095 0.177 Uiso 1 1 calc R . . H25C H 0.3186 0.4779 0.5400 0.177 Uiso 1 1 calc R . . N1 N 0.38364(14) -0.1044(2) 0.3324(3) 0.0331(9) Uani 1 1 d . . . N2 N 0.28829(13) -0.1543(2) 0.2701(2) 0.0263(9) Uani 1 1 d . . . N3 N 0.20025(13) -0.2154(2) 0.1926(3) 0.0300(9) Uani 1 1 d . . . N5 N 0.18679(14) 0.2366(2) 0.5478(3) 0.0363(10) Uani 1 1 d . . . Ni1 Ni 0.23067(2) 0.02668(3) 0.43056(4) 0.02485(12) Uani 1 1 d . A . O1 O 0.30496(11) -0.00503(17) 0.3611(2) 0.0319(7) Uani 1 1 d . . . O2 O 0.26805(11) 0.14203(17) 0.4783(2) 0.0299(7) Uani 1 1 d . . . S1 S 0.17928(4) -0.08761(7) 0.35330(9) 0.0304(3) Uani 1 1 d . . . S2 S 0.15332(5) 0.04502(8) 0.53491(9) 0.0368(3) Uani 1 1 d . . . C26 C 0.33086(19) 0.2999(3) 0.4113(3) 0.0445(13) Uani 0.625(4) 1 d PD A 3 H26 H 0.3419 0.3691 0.3965 0.053 Uiso 0.625(4) 1 calc PR A 3 C27 C 0.3824(3) 0.2615(5) 0.4816(5) 0.0437(13) Uani 0.625(4) 1 d PD A 3 H27A H 0.3843 0.2968 0.5529 0.066 Uiso 0.625(4) 1 calc PR A 3 H27B H 0.4211 0.2701 0.4420 0.066 Uiso 0.625(4) 1 calc PR A 3 H27C H 0.3758 0.1923 0.4961 0.066 Uiso 0.625(4) 1 calc PR A 3 C28 C 0.3185(3) 0.2576(4) 0.2992(5) 0.0437(13) Uani 0.625(4) 1 d PD A 3 H28A H 0.3068 0.1893 0.3073 0.066 Uiso 0.625(4) 1 calc PR A 3 H28B H 0.3556 0.2621 0.2540 0.066 Uiso 0.625(4) 1 calc PR A 3 H28C H 0.2850 0.2933 0.2620 0.066 Uiso 0.625(4) 1 calc PR A 3 C26S C 0.33086(19) 0.2999(3) 0.4113(3) 0.0445(13) Uani 0.375(4) 1 d P A 4 H26S H 0.3369 0.2280 0.4086 0.053 Uiso 0.375(4) 1 calc PR A 4 C27S C 0.3888(4) 0.3295(8) 0.4735(9) 0.0437(13) Uani 0.375(4) 1 d PD A 4 H27D H 0.3890 0.4001 0.4838 0.066 Uiso 0.375(4) 1 calc PR A 4 H27E H 0.4246 0.3101 0.4301 0.066 Uiso 0.375(4) 1 calc PR A 4 H27F H 0.3903 0.2976 0.5469 0.066 Uiso 0.375(4) 1 calc PR A 4 C28S C 0.3343(5) 0.3235(8) 0.2882(6) 0.0437(13) Uani 0.375(4) 1 d PD A 4 H28D H 0.2968 0.3008 0.2497 0.066 Uiso 0.375(4) 1 calc PR A 4 H28E H 0.3700 0.2910 0.2563 0.066 Uiso 0.375(4) 1 calc PR A 4 H28F H 0.3382 0.3938 0.2786 0.066 Uiso 0.375(4) 1 calc PR A 4 C18 C 0.0903(2) 0.2908(4) 0.6706(4) 0.0698(16) Uiso 1 1 d D . . H18 H 0.0497 0.2804 0.7064 0.084 Uiso 1 1 calc R . . C17 C 0.0415(3) 0.0859(4) 0.7677(5) 0.094(2) Uiso 1 1 d . . . H17A H 0.0312 0.1397 0.8177 0.142 Uiso 1 1 calc R . . H17B H 0.0811 0.0579 0.7913 0.142 Uiso 1 1 calc R . . H17C H 0.0096 0.0360 0.7712 0.142 Uiso 1 1 calc R . . C16 C -0.0034(3) 0.1306(5) 0.5782(5) 0.108(2) Uiso 1 1 d . . . H16A H -0.0293 0.0724 0.5806 0.162 Uiso 1 1 calc R . . H16B H 0.0128 0.1384 0.5026 0.162 Uiso 1 1 calc R . . H16C H -0.0280 0.1877 0.5974 0.162 Uiso 1 1 calc R . . C19 C 0.1226(4) 0.3155(6) 0.7709(6) 0.161(3) Uiso 1 1 d D . . H19A H 0.1628 0.3425 0.7525 0.241 Uiso 1 1 calc R . . H19B H 0.1282 0.2572 0.8171 0.241 Uiso 1 1 calc R . . H19C H 0.0990 0.3638 0.8125 0.241 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0184(18) 0.060(3) 0.054(3) -0.012(2) 0.002(2) -0.013(2) C2 0.036(2) 0.055(3) 0.081(4) -0.022(3) 0.012(3) -0.012(2) C3 0.034(2) 0.117(4) 0.051(3) -0.025(3) -0.013(2) -0.015(3) C4 0.025(2) 0.058(3) 0.058(3) 0.008(2) 0.004(2) 0.012(2) C5 0.064(3) 0.084(3) 0.085(4) 0.025(3) 0.023(3) 0.046(3) C6 0.051(3) 0.063(3) 0.078(4) -0.009(3) 0.018(3) -0.004(3) C7 0.034(2) 0.0160(19) 0.036(2) 0.0018(18) 0.0087(19) 0.0056(16) C8 0.034(2) 0.027(2) 0.0199(19) 0.0011(17) 0.0023(18) -0.0009(17) C9 0.032(2) 0.027(2) 0.044(2) -0.0151(19) -0.008(2) -0.0011(17) C10 0.038(2) 0.057(3) 0.051(3) -0.002(2) 0.003(2) -0.004(2) C11 0.050(3) 0.030(2) 0.059(3) -0.013(2) 0.003(2) 0.007(2) C12 0.031(2) 0.033(2) 0.063(3) -0.018(2) 0.002(2) 0.0018(18) C13 0.038(3) 0.066(3) 0.074(3) -0.001(3) -0.027(3) 0.008(2) C14 0.035(2) 0.054(3) 0.058(3) -0.022(2) 0.006(2) -0.007(2) C15 0.021(2) 0.263(7) 0.067(3) -0.098(4) 0.008(2) -0.037(3) N4 0.0321(19) 0.068(2) 0.035(2) -0.0163(19) -0.0044(18) 0.0068(18) C20 0.132(5) 0.040(3) 0.098(4) 0.035(3) -0.015(4) -0.025(3) C21 0.023(2) 0.062(3) 0.023(2) -0.012(2) -0.0067(18) 0.0073(19) C22 0.036(2) 0.042(2) 0.021(2) -0.0003(19) -0.0072(19) -0.0081(19) N6 0.0389(18) 0.0190(16) 0.053(2) -0.0109(16) 0.0051(18) -0.0076(15) C23 0.124(5) 0.036(3) 0.127(5) -0.024(3) -0.039(5) 0.004(3) C24 0.174(6) 0.041(3) 0.078(4) -0.002(3) 0.023(5) 0.032(3) C25 0.211(8) 0.059(4) 0.082(4) -0.017(3) -0.017(5) 0.040(4) N1 0.0233(16) 0.0327(18) 0.043(2) -0.0004(16) 0.0007(16) 0.0057(14) N2 0.0238(15) 0.0277(17) 0.0273(17) -0.0063(15) 0.0005(15) -0.0021(14) N3 0.0228(16) 0.0279(17) 0.0394(19) -0.0088(15) 0.0043(16) 0.0028(14) N5 0.0283(17) 0.048(2) 0.0326(19) -0.0090(17) -0.0036(16) -0.0007(16) Ni1 0.0239(2) 0.0255(2) 0.0250(2) 0.0007(2) -0.0021(2) -0.0022(2) O1 0.0229(13) 0.0361(15) 0.0366(15) -0.0040(12) -0.0026(13) -0.0044(11) O2 0.0291(13) 0.0249(14) 0.0358(15) -0.0091(12) 0.0085(13) 0.0036(11) S1 0.0237(5) 0.0305(5) 0.0370(6) -0.0047(5) 0.0001(5) -0.0028(4) S2 0.0326(5) 0.0447(6) 0.0332(6) 0.0053(5) 0.0057(5) -0.0062(5) C26 0.059(3) 0.031(2) 0.043(3) 0.001(2) 0.002(2) -0.022(2) C27 0.046(2) 0.037(3) 0.048(3) -0.004(3) 0.007(2) -0.017(2) C28 0.046(2) 0.037(3) 0.048(3) -0.004(3) 0.007(2) -0.017(2) C26S 0.059(3) 0.031(2) 0.043(3) 0.001(2) 0.002(2) -0.022(2) C27S 0.046(2) 0.037(3) 0.048(3) -0.004(3) 0.007(2) -0.017(2) C28S 0.046(2) 0.037(3) 0.048(3) -0.004(3) 0.007(2) -0.017(2) _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 C1 N1 1.462(5) . ? C1 C2 1.485(6) . ? C1 C3 1.542(6) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.468(5) . ? C4 C6 1.525(6) . ? C4 C5 1.528(6) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 O1 1.273(4) . ? C7 N2 1.344(4) . ? C7 N1 1.357(5) . ? C8 N2 1.320(5) . ? C8 N3 1.340(5) . ? C8 S1 1.760(4) . ? C9 N3 1.492(5) . ? C9 C10 1.508(6) . ? C9 C11 1.530(5) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N3 1.479(5) . ? C12 C14 1.512(6) . ? C12 C13 1.526(6) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.408(8) . ? C15 C17 1.423(8) . ? C15 N4 1.523(6) . ? C15 H15 1.0000 . ? N4 C21 1.349(5) . ? N4 C18 1.457(5) . ? C20 C18 1.435(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N5 1.328(5) . ? C21 S2 1.740(4) . ? C22 O2 1.271(4) . ? C22 N5 1.348(5) . ? C22 N6 1.380(4) . ? N6 C26 1.449(5) . ? N6 C23 1.4892 . ? C23 C24 1.5335 . ? C23 C25 1.5604 . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? Ni1 O2 1.870(2) . ? Ni1 O1 1.882(2) . ? Ni1 S2 2.1271(11) . ? Ni1 S1 2.1321(11) . ? C26 C28 1.479(6) . ? C26 C27 1.487(7) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C27S H27D 0.9800 . ? C27S H27E 0.9800 . ? C27S H27F 0.9800 . ? C28S H28D 0.9800 . ? C28S H28E 0.9800 . ? C28S H28F 0.9800 . ? C18 C19 1.419(8) . ? C18 H18 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.6(3) . . ? N1 C1 C3 112.3(3) . . ? C2 C1 C3 113.5(4) . . ? N1 C1 H1 105.9 . . ? C2 C1 H1 105.9 . . ? C3 C1 H1 105.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C6 111.6(3) . . ? N1 C4 C5 112.6(4) . . ? C6 C4 C5 111.5(4) . . ? N1 C4 H4 106.9 . . ? C6 C4 H4 106.9 . . ? C5 C4 H4 106.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O1 C7 N2 127.8(3) . . ? O1 C7 N1 115.5(3) . . ? N2 C7 N1 116.7(3) . . ? N2 C8 N3 117.6(3) . . ? N2 C8 S1 125.6(3) . . ? N3 C8 S1 116.7(3) . . ? N3 C9 C10 113.8(3) . . ? N3 C9 C11 111.6(3) . . ? C10 C9 C11 113.1(3) . . ? N3 C9 H9 105.9 . . ? C10 C9 H9 105.9 . . ? C11 C9 H9 105.9 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C14 111.8(3) . . ? N3 C12 C13 110.0(3) . . ? C14 C12 C13 113.0(4) . . ? N3 C12 H12 107.2 . . ? C14 C12 H12 107.2 . . ? C13 C12 H12 107.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 126.1(5) . . ? C16 C15 N4 112.5(5) . . ? C17 C15 N4 116.3(4) . . ? C16 C15 H15 97.5 . . ? C17 C15 H15 97.5 . . ? N4 C15 H15 97.5 . . ? C21 N4 C18 119.7(3) . . ? C21 N4 C15 123.1(4) . . ? C18 N4 C15 117.0(4) . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 N4 117.6(4) . . ? N5 C21 S2 126.2(3) . . ? N4 C21 S2 116.2(3) . . ? O2 C22 N5 128.6(3) . . ? O2 C22 N6 115.5(3) . . ? N5 C22 N6 115.9(3) . . ? C22 N6 C26 121.9(3) . . ? C22 N6 C23 110.7(2) . . ? C26 N6 C23 127.4(2) . . ? N6 C23 C24 110.4 . . ? N6 C23 C25 109.5 . . ? C24 C23 C25 113.4 . . ? N6 C23 H23 107.8 . . ? C24 C23 H23 107.8 . . ? C25 C23 H23 107.8 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C7 N1 C1 121.5(3) . . ? C7 N1 C4 121.1(3) . . ? C1 N1 C4 117.4(3) . . ? C8 N2 C7 124.8(3) . . ? C8 N3 C12 122.6(3) . . ? C8 N3 C9 122.2(3) . . ? C12 N3 C9 115.2(3) . . ? C21 N5 C22 124.3(3) . . ? O2 Ni1 O1 87.59(10) . . ? O2 Ni1 S2 93.79(8) . . ? O1 Ni1 S2 168.81(9) . . ? O2 Ni1 S1 169.05(8) . . ? O1 Ni1 S1 95.02(8) . . ? S2 Ni1 S1 85.70(4) . . ? C7 O1 Ni1 128.9(2) . . ? C22 O2 Ni1 126.8(2) . . ? C8 S1 Ni1 109.35(13) . . ? C21 S2 Ni1 109.24(13) . . ? N6 C26 C28 108.6(4) . . ? N6 C26 C27 112.6(4) . . ? C28 C26 C27 119.5(4) . . ? N6 C26 H26 104.9 . . ? C28 C26 H26 104.9 . . ? C27 C26 H26 104.9 . . ? C19 C18 C20 122.5(5) . . ? C19 C18 N4 115.4(5) . . ? C20 C18 N4 118.9(4) . . ? C19 C18 H18 95.9 . . ? C20 C18 H18 95.9 . . ? N4 C18 H18 95.9 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 C15 N4 C21 -96.4(6) . . . . ? C17 C15 N4 C21 107.2(5) . . . . ? C16 C15 N4 C18 79.5(5) . . . . ? C17 C15 N4 C18 -76.9(6) . . . . ? C18 N4 C21 N5 -3.9(5) . . . . ? C15 N4 C21 N5 171.9(4) . . . . ? C18 N4 C21 S2 179.0(3) . . . . ? C15 N4 C21 S2 -5.2(5) . . . . ? O2 C22 N6 C26 6.0(5) . . . . ? N5 C22 N6 C26 -175.3(3) . . . . ? O2 C22 N6 C23 -176.0(3) . . . . ? N5 C22 N6 C23 2.6(4) . . . . ? C22 N6 C23 C24 -109.6(3) . . . . ? C26 N6 C23 C24 68.2(3) . . . . ? C22 N6 C23 C25 124.8(3) . . . . ? C26 N6 C23 C25 -57.3(3) . . . . ? O1 C7 N1 C1 4.1(5) . . . . ? N2 C7 N1 C1 -179.1(3) . . . . ? O1 C7 N1 C4 -175.8(3) . . . . ? N2 C7 N1 C4 1.1(5) . . . . ? C2 C1 N1 C7 -70.4(5) . . . . ? C3 C1 N1 C7 59.2(5) . . . . ? C2 C1 N1 C4 109.5(4) . . . . ? C3 C1 N1 C4 -120.9(4) . . . . ? C6 C4 N1 C7 120.8(4) . . . . ? C5 C4 N1 C7 -113.0(4) . . . . ? C6 C4 N1 C1 -59.1(5) . . . . ? C5 C4 N1 C1 67.2(5) . . . . ? N3 C8 N2 C7 166.8(3) . . . . ? S1 C8 N2 C7 -15.2(5) . . . . ? O1 C7 N2 C8 -13.2(6) . . . . ? N1 C7 N2 C8 170.4(3) . . . . ? N2 C8 N3 C12 -177.9(3) . . . . ? S1 C8 N3 C12 3.8(5) . . . . ? N2 C8 N3 C9 4.1(5) . . . . ? S1 C8 N3 C9 -174.1(3) . . . . ? C14 C12 N3 C8 -115.9(4) . . . . ? C13 C12 N3 C8 117.6(4) . . . . ? C14 C12 N3 C9 62.1(5) . . . . ? C13 C12 N3 C9 -64.3(4) . . . . ? C10 C9 N3 C8 -63.8(5) . . . . ? C11 C9 N3 C8 65.7(4) . . . . ? C10 C9 N3 C12 118.2(4) . . . . ? C11 C9 N3 C12 -112.4(4) . . . . ? N4 C21 N5 C22 173.2(3) . . . . ? S2 C21 N5 C22 -10.0(6) . . . . ? O2 C22 N5 C21 -5.8(6) . . . . ? N6 C22 N5 C21 175.7(3) . . . . ? N2 C7 O1 Ni1 37.2(5) . . . . ? N1 C7 O1 Ni1 -146.4(3) . . . . ? O2 Ni1 O1 C7 165.5(3) . . . . ? S2 Ni1 O1 C7 68.1(6) . . . . ? S1 Ni1 O1 C7 -25.1(3) . . . . ? N5 C22 O2 Ni1 37.0(5) . . . . ? N6 C22 O2 Ni1 -144.5(3) . . . . ? O1 Ni1 O2 C22 152.8(3) . . . . ? S2 Ni1 O2 C22 -38.3(3) . . . . ? S1 Ni1 O2 C22 48.7(6) . . . . ? N2 C8 S1 Ni1 16.8(4) . . . . ? N3 C8 S1 Ni1 -165.2(2) . . . . ? O2 Ni1 S1 C8 104.0(4) . . . . ? O1 Ni1 S1 C8 0.59(15) . . . . ? S2 Ni1 S1 C8 -168.21(13) . . . . ? N5 C21 S2 Ni1 -2.4(4) . . . . ? N4 C21 S2 Ni1 174.4(2) . . . . ? O2 Ni1 S2 C21 19.33(16) . . . . ? O1 Ni1 S2 C21 116.1(4) . . . . ? S1 Ni1 S2 C21 -149.71(14) . . . . ? C22 N6 C26 C28 63.5(5) . . . . ? C23 N6 C26 C28 -114.1(4) . . . . ? C22 N6 C26 C27 -71.2(5) . . . . ? C23 N6 C26 C27 111.2(4) . . . . ? C21 N4 C18 C19 -82.0(6) . . . . ? C15 N4 C18 C19 101.9(6) . . . . ? C21 N4 C18 C20 78.5(6) . . . . ? C15 N4 C18 C20 -97.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.379 _refine_diff_density_min -0.994 _refine_diff_density_rms 0.107 #start Validation Reply Form _vrf_PLAT220_s2983m ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.96 Ratio RESPONSE: Disordered side chain ; _vrf_PLAT222_s2983m ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.88 Ratio RESPONSE: Vide ultra ; # end Validation Reply Form # Attachment 's2987n.cif' data_s2987n _database_code_depnum_ccdc_archive 'CCDC 715962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H87 Co N10 O3 S3' _chemical_formula_weight 959.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 14.0552(17) _cell_length_b 15.7278(19) _cell_length_c 25.394(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.686(2) _cell_angle_gamma 90.00 _cell_volume 5575.5(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2946 _cell_measurement_theta_min 2.4215 _cell_measurement_theta_max 21.9875 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.463 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43979 _diffrn_reflns_av_R_equivalents 0.1028 _diffrn_reflns_av_sigmaI/netI 0.1567 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 26.37 _reflns_number_total 11407 _reflns_number_gt 6078 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11407 _refine_ls_number_parameters 562 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1308 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2235 _refine_ls_wR_factor_gt 0.2003 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 1.026 _refine_ls_shift/su_mean 0.011 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 C1 C 1.1354(4) 0.1778(4) -0.0077(2) 0.0286(15) Uani 1 1 d . . . H1 H 1.1669 0.1551 -0.0381 0.034 Uiso 1 1 calc R . . C2 C 1.1675(5) 0.2699(4) -0.0015(3) 0.0348(16) Uani 1 1 d . . . H2A H 1.1394 0.3027 -0.0322 0.052 Uiso 1 1 calc R . . H2B H 1.2375 0.2727 0.0009 0.052 Uiso 1 1 calc R . . H2C H 1.1463 0.2936 0.0309 0.052 Uiso 1 1 calc R . . C3 C 1.1713(4) 0.1216(4) 0.0399(2) 0.0324(16) Uani 1 1 d . . . H3A H 1.1414 0.1399 0.0710 0.049 Uiso 1 1 calc R . . H3B H 1.2410 0.1267 0.0473 0.049 Uiso 1 1 calc R . . H3C H 1.1543 0.0622 0.0317 0.049 Uiso 1 1 calc R . . C4 C 1.0035(4) 0.1296(4) -0.0762(2) 0.0270(14) Uani 1 1 d . . . H4 H 0.9319 0.1291 -0.0822 0.032 Uiso 1 1 calc R . . C5 C 1.0381(5) 0.1833(4) -0.1207(3) 0.0409(18) Uani 1 1 d . . . H5A H 1.0204 0.2428 -0.1161 0.061 Uiso 1 1 calc R . . H5B H 1.0081 0.1626 -0.1551 0.061 Uiso 1 1 calc R . . H5C H 1.1078 0.1786 -0.1192 0.061 Uiso 1 1 calc R . . C6 C 1.0364(5) 0.0366(4) -0.0779(3) 0.0396(18) Uani 1 1 d . . . H6A H 1.1064 0.0341 -0.0709 0.059 Uiso 1 1 calc R . . H6B H 1.0159 0.0126 -0.1130 0.059 Uiso 1 1 calc R . . H6C H 1.0081 0.0038 -0.0509 0.059 Uiso 1 1 calc R . . C7 C 0.9661(4) 0.1916(4) 0.0093(2) 0.0198(13) Uani 1 1 d . . . C8 C 0.9465(4) 0.2759(3) 0.0833(2) 0.0180(12) Uani 1 1 d . . . C9 C 1.0947(4) 0.2905(4) 0.1465(2) 0.0215(13) Uani 1 1 d . . . H9 H 1.1186 0.2532 0.1190 0.026 Uiso 1 1 calc R . . C10 C 1.1549(5) 0.3718(4) 0.1497(3) 0.0439(19) Uani 1 1 d . . . H10A H 1.1467 0.4007 0.1152 0.066 Uiso 1 1 calc R . . H10B H 1.2225 0.3574 0.1590 0.066 Uiso 1 1 calc R . . H10C H 1.1338 0.4096 0.1768 0.066 Uiso 1 1 calc R . . C11 C 1.1067(5) 0.2421(5) 0.1980(3) 0.0410(18) Uani 1 1 d . . . H11A H 1.0845 0.2772 0.2261 0.062 Uiso 1 1 calc R . . H11B H 1.1744 0.2279 0.2074 0.062 Uiso 1 1 calc R . . H11C H 1.0688 0.1897 0.1942 0.062 Uiso 1 1 calc R . . C12 C 0.9435(4) 0.3685(4) 0.1610(2) 0.0231(13) Uani 1 1 d . . . H12 H 0.9912 0.3845 0.1917 0.028 Uiso 1 1 calc R . . C13 C 0.9145(5) 0.4512(4) 0.1322(3) 0.0376(17) Uani 1 1 d . . . H13A H 0.9717 0.4799 0.1223 0.056 Uiso 1 1 calc R . . H13B H 0.8822 0.4883 0.1555 0.056 Uiso 1 1 calc R . . H13C H 0.8708 0.4387 0.1001 0.056 Uiso 1 1 calc R . . C14 C 0.8590(4) 0.3269(4) 0.1847(2) 0.0273(15) Uani 1 1 d . . . H14A H 0.8042 0.3220 0.1573 0.041 Uiso 1 1 calc R . . H14B H 0.8412 0.3619 0.2139 0.041 Uiso 1 1 calc R . . H14C H 0.8778 0.2701 0.1980 0.041 Uiso 1 1 calc R . . C15 C 0.8206(4) 0.0294(4) 0.1992(2) 0.0274(15) Uani 1 1 d . . . H15 H 0.8411 0.0241 0.1629 0.033 Uiso 1 1 calc R . . C16 C 0.9059(4) 0.0628(4) 0.2355(3) 0.045(2) Uani 1 1 d . . . H16A H 0.9251 0.1183 0.2227 0.068 Uiso 1 1 calc R . . H16B H 0.9595 0.0228 0.2358 0.068 Uiso 1 1 calc R . . H16C H 0.8883 0.0689 0.2715 0.068 Uiso 1 1 calc R . . C17 C 0.7921(5) -0.0594(4) 0.2162(3) 0.0356(17) Uani 1 1 d . . . H17A H 0.7807 -0.0582 0.2535 0.053 Uiso 1 1 calc R . . H17B H 0.8438 -0.0996 0.2116 0.053 Uiso 1 1 calc R . . H17C H 0.7335 -0.0774 0.1943 0.053 Uiso 1 1 calc R . . C18 C 0.6911(4) 0.1010(4) 0.2435(2) 0.0279(15) Uani 1 1 d . . . H18 H 0.7266 0.0638 0.2711 0.034 Uiso 1 1 calc R . . C19 C 0.6977(4) 0.1907(4) 0.2664(2) 0.0305(15) Uani 1 1 d . . . H19A H 0.7633 0.2120 0.2666 0.046 Uiso 1 1 calc R . . H19B H 0.6806 0.1898 0.3027 0.046 Uiso 1 1 calc R . . H19C H 0.6534 0.2281 0.2445 0.046 Uiso 1 1 calc R . . C20 C 0.5883(4) 0.0663(4) 0.2354(2) 0.0286(15) Uani 1 1 d . . . H20A H 0.5514 0.0970 0.2062 0.043 Uiso 1 1 calc R . . H20B H 0.5582 0.0740 0.2680 0.043 Uiso 1 1 calc R . . H20C H 0.5897 0.0056 0.2267 0.043 Uiso 1 1 calc R . . C21 C 0.7189(4) 0.1397(4) 0.1518(2) 0.0202(13) Uani 1 1 d . . . C22 C 0.6232(4) 0.2560(3) 0.1188(2) 0.0185(12) Uani 1 1 d . . . C23 C 0.4732(4) 0.2676(4) 0.1608(2) 0.0259(14) Uani 1 1 d . . . H23 H 0.5045 0.2184 0.1809 0.031 Uiso 1 1 calc R . . C24 C 0.4528(5) 0.3352(4) 0.2018(2) 0.0346(16) Uani 1 1 d . . . H24A H 0.5135 0.3589 0.2185 0.052 Uiso 1 1 calc R . . H24B H 0.4183 0.3091 0.2290 0.052 Uiso 1 1 calc R . . H24C H 0.4138 0.3808 0.1841 0.052 Uiso 1 1 calc R . . C25 C 0.3822(5) 0.2350(5) 0.1301(3) 0.046(2) Uani 1 1 d . . . H25A H 0.3507 0.2813 0.1089 0.069 Uiso 1 1 calc R . . H25B H 0.3393 0.2136 0.1548 0.069 Uiso 1 1 calc R . . H25C H 0.3976 0.1889 0.1065 0.069 Uiso 1 1 calc R . . C26 C 0.5108(4) 0.3737(4) 0.0914(2) 0.0265(14) Uani 1 1 d . . . H26 H 0.4477 0.3924 0.1019 0.032 Uiso 1 1 calc R . . C27 C 0.4946(5) 0.3557(4) 0.0323(2) 0.0326(16) Uani 1 1 d . . . H27A H 0.5563 0.3462 0.0190 0.049 Uiso 1 1 calc R . . H27B H 0.4623 0.4044 0.0140 0.049 Uiso 1 1 calc R . . H27C H 0.4545 0.3049 0.0260 0.049 Uiso 1 1 calc R . . C28 C 0.5793(5) 0.4476(4) 0.1033(3) 0.0375(17) Uani 1 1 d . . . H28A H 0.5880 0.4583 0.1416 0.056 Uiso 1 1 calc R . . H28B H 0.5529 0.4985 0.0848 0.056 Uiso 1 1 calc R . . H28C H 0.6413 0.4337 0.0914 0.056 Uiso 1 1 calc R . . C29 C 0.4655(4) 0.0824(4) -0.0587(2) 0.0234(13) Uani 1 1 d . . . H29 H 0.5152 0.0580 -0.0315 0.028 Uiso 1 1 calc R . . C30 C 0.4471(5) 0.0165(4) -0.1023(2) 0.0333(16) Uani 1 1 d . . . H30A H 0.3958 0.0365 -0.1289 0.050 Uiso 1 1 calc R . . H30B H 0.4278 -0.0372 -0.0871 0.050 Uiso 1 1 calc R . . H30C H 0.5057 0.0077 -0.1191 0.050 Uiso 1 1 calc R . . C31 C 0.3771(4) 0.1000(4) -0.0307(3) 0.0367(17) Uani 1 1 d . . . H31A H 0.3935 0.1406 -0.0018 0.055 Uiso 1 1 calc R . . H31B H 0.3548 0.0468 -0.0161 0.055 Uiso 1 1 calc R . . H31C H 0.3262 0.1238 -0.0561 0.055 Uiso 1 1 calc R . . C32 C 0.4462(4) 0.2055(4) -0.1220(2) 0.0282(15) Uani 1 1 d . . . H32 H 0.3847 0.1730 -0.1271 0.034 Uiso 1 1 calc R . . C33 C 0.4865(5) 0.2009(4) -0.1747(2) 0.0328(16) Uani 1 1 d . . . H33A H 0.5446 0.2357 -0.1731 0.049 Uiso 1 1 calc R . . H33B H 0.4389 0.2222 -0.2028 0.049 Uiso 1 1 calc R . . H33C H 0.5022 0.1417 -0.1822 0.049 Uiso 1 1 calc R . . C34 C 0.4191(5) 0.2947(4) -0.1066(3) 0.0358(17) Uani 1 1 d . . . H34A H 0.3925 0.2929 -0.0727 0.054 Uiso 1 1 calc R . . H34B H 0.3712 0.3178 -0.1340 0.054 Uiso 1 1 calc R . . H34C H 0.4762 0.3310 -0.1033 0.054 Uiso 1 1 calc R . . C35 C 0.5893(4) 0.1955(4) -0.0551(2) 0.0191(12) Uani 1 1 d . . . C36 C 0.6977(4) 0.3092(4) -0.0579(2) 0.0192(12) Uani 1 1 d . . . C37 C 0.7111(4) 0.3585(4) -0.1494(2) 0.0266(14) Uani 1 1 d . . . H37 H 0.6747 0.3044 -0.1573 0.032 Uiso 1 1 calc R . . C38 C 0.6452(5) 0.4309(5) -0.1693(3) 0.047(2) Uani 1 1 d . . . H38A H 0.5901 0.4325 -0.1490 0.070 Uiso 1 1 calc R . . H38B H 0.6227 0.4221 -0.2069 0.070 Uiso 1 1 calc R . . H38C H 0.6801 0.4848 -0.1649 0.070 Uiso 1 1 calc R . . C39 C 0.7992(5) 0.3544(4) -0.1787(2) 0.0355(17) Uani 1 1 d . . . H39A H 0.8309 0.4100 -0.1770 0.053 Uiso 1 1 calc R . . H39B H 0.7801 0.3392 -0.2158 0.053 Uiso 1 1 calc R . . H39C H 0.8435 0.3114 -0.1622 0.053 Uiso 1 1 calc R . . C40 C 0.8010(4) 0.4334(4) -0.0704(2) 0.0266(14) Uani 1 1 d . . . H40 H 0.8147 0.4674 -0.1018 0.032 Uiso 1 1 calc R . . C41 C 0.7495(5) 0.4937(4) -0.0352(3) 0.0418(18) Uani 1 1 d . . . H41A H 0.6870 0.5094 -0.0538 0.063 Uiso 1 1 calc R . . H41B H 0.7883 0.5449 -0.0276 0.063 Uiso 1 1 calc R . . H41C H 0.7406 0.4650 -0.0019 0.063 Uiso 1 1 calc R . . C42 C 0.8979(4) 0.4028(4) -0.0434(2) 0.0314(16) Uani 1 1 d . . . H42A H 0.8887 0.3726 -0.0106 0.047 Uiso 1 1 calc R . . H42B H 0.9400 0.4518 -0.0350 0.047 Uiso 1 1 calc R . . H42C H 0.9272 0.3644 -0.0673 0.047 Uiso 1 1 calc R . . Co1 Co 0.75543(5) 0.22628(5) 0.04142(3) 0.0159(2) Uani 1 1 d . . . N1 N 1.0307(3) 0.1681(3) -0.02339(19) 0.0225(11) Uani 1 1 d . . . N2 N 1.0000(3) 0.2289(3) 0.05395(18) 0.0196(10) Uani 1 1 d . . . N3 N 0.9929(3) 0.3100(3) 0.12859(18) 0.0211(11) Uani 1 1 d . . . N4 N 0.7405(3) 0.0909(3) 0.19545(18) 0.0202(11) Uani 1 1 d . . . N5 N 0.6435(3) 0.1892(3) 0.15191(17) 0.0185(10) Uani 1 1 d . . . N6 N 0.5404(3) 0.2983(3) 0.12440(19) 0.0227(11) Uani 1 1 d . . . N7 N 0.5061(3) 0.1619(3) -0.07819(18) 0.0217(11) Uani 1 1 d . . . N8 N 0.6276(3) 0.2575(3) -0.08055(18) 0.0199(11) Uani 1 1 d . . . N9 N 0.7375(3) 0.3619(3) -0.09136(18) 0.0227(11) Uani 1 1 d . . . O1 O 0.8589(3) 0.2973(2) 0.07296(14) 0.0180(9) Uani 1 1 d . . . O2 O 0.6745(3) 0.2868(2) 0.08541(14) 0.0198(9) Uani 1 1 d . . . O3 O 0.7259(3) 0.3177(2) -0.00864(14) 0.0182(9) Uani 1 1 d . . . S1 S 0.84644(10) 0.16224(9) -0.01132(6) 0.0192(3) Uani 1 1 d . . . S2 S 0.79147(10) 0.12594(9) 0.10069(6) 0.0188(3) Uani 1 1 d . . . S3 S 0.63585(10) 0.14807(9) 0.00573(6) 0.0201(3) Uani 1 1 d . . . C44 C 0.7115(8) 0.0377(7) 0.8640(5) 0.061(4) Uiso 0.582(9) 1 d PG A 1 H44A H 0.7423 0.0276 0.9001 0.091 Uiso 0.582(9) 1 calc PR A 1 H44B H 0.6892 -0.0165 0.8479 0.091 Uiso 0.582(9) 1 calc PR A 1 H44C H 0.6569 0.0760 0.8652 0.091 Uiso 0.582(9) 1 calc PR A 1 C45 C 0.7798(5) 0.0760(5) 0.8327(3) 0.38(4) Uiso 0.582(9) 1 d PG A 1 N10 N 0.8332(6) 0.1066(6) 0.8083(3) 0.060(4) Uiso 0.582(9) 1 d PG A 1 C46 C 0.7487(7) 0.1347(5) 0.8419(4) 0.027(4) Uiso 0.418(9) 1 d PG A 2 H46A H 0.7064 0.1072 0.8649 0.041 Uiso 0.418(9) 1 calc PR A 2 H46B H 0.7106 0.1706 0.8159 0.041 Uiso 0.418(9) 1 calc PR A 2 H46C H 0.7958 0.1699 0.8635 0.041 Uiso 0.418(9) 1 calc PR A 2 C47 C 0.7980(5) 0.0705(5) 0.8146(3) 0.28(3) Uiso 0.418(9) 1 d PG A 2 N11 N 0.8372(8) 0.0201(7) 0.7936(5) 0.061(5) Uiso 0.418(9) 1 d PG A 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 C1 0.017(3) 0.038(4) 0.032(4) -0.006(3) 0.008(3) -0.003(3) C2 0.028(4) 0.041(4) 0.036(4) -0.008(3) 0.008(3) -0.007(3) C3 0.023(3) 0.035(4) 0.038(4) -0.009(3) -0.003(3) 0.006(3) C4 0.023(3) 0.036(4) 0.023(3) -0.013(3) 0.005(3) 0.002(3) C5 0.042(4) 0.050(5) 0.032(4) -0.004(3) 0.008(3) 0.005(4) C6 0.042(4) 0.036(4) 0.041(4) -0.014(3) 0.007(3) 0.002(3) C7 0.018(3) 0.018(3) 0.025(3) 0.001(2) 0.005(3) 0.000(2) C8 0.016(3) 0.019(3) 0.019(3) 0.001(2) 0.001(2) -0.006(2) C9 0.013(3) 0.026(3) 0.025(3) -0.003(3) 0.002(2) -0.005(2) C10 0.031(4) 0.040(4) 0.062(5) -0.016(4) 0.009(4) -0.012(3) C11 0.030(4) 0.057(5) 0.035(4) 0.009(4) 0.001(3) 0.007(3) C12 0.019(3) 0.029(3) 0.021(3) -0.007(3) 0.000(2) -0.005(3) C13 0.045(4) 0.027(4) 0.040(4) -0.012(3) 0.004(3) 0.003(3) C14 0.020(3) 0.042(4) 0.020(3) -0.008(3) 0.003(3) 0.003(3) C15 0.022(3) 0.038(4) 0.023(3) 0.007(3) 0.004(3) 0.012(3) C16 0.024(4) 0.036(4) 0.074(6) 0.021(4) -0.005(4) -0.005(3) C17 0.031(4) 0.028(4) 0.046(4) 0.002(3) -0.006(3) 0.004(3) C18 0.025(3) 0.037(4) 0.022(3) 0.006(3) 0.003(3) 0.007(3) C19 0.032(4) 0.040(4) 0.020(3) -0.002(3) 0.005(3) -0.002(3) C20 0.028(3) 0.032(4) 0.027(4) 0.007(3) 0.008(3) 0.000(3) C21 0.016(3) 0.021(3) 0.022(3) -0.001(2) -0.004(2) -0.006(2) C22 0.017(3) 0.021(3) 0.017(3) -0.005(2) -0.001(2) 0.000(2) C23 0.017(3) 0.033(4) 0.029(3) 0.002(3) 0.008(3) 0.002(3) C24 0.029(4) 0.048(4) 0.028(4) 0.001(3) 0.008(3) 0.007(3) C25 0.024(4) 0.056(5) 0.061(5) -0.016(4) 0.017(4) -0.008(3) C26 0.028(3) 0.025(3) 0.028(3) 0.003(3) 0.004(3) 0.013(3) C27 0.030(4) 0.043(4) 0.024(3) 0.004(3) 0.000(3) 0.017(3) C28 0.048(4) 0.027(4) 0.038(4) 0.003(3) 0.008(3) 0.009(3) C29 0.022(3) 0.021(3) 0.026(3) 0.003(3) 0.000(3) -0.004(3) C30 0.037(4) 0.034(4) 0.029(4) -0.006(3) 0.005(3) -0.013(3) C31 0.028(4) 0.040(4) 0.045(4) 0.003(3) 0.015(3) -0.002(3) C32 0.023(3) 0.030(4) 0.029(4) 0.007(3) -0.008(3) -0.003(3) C33 0.037(4) 0.040(4) 0.019(3) 0.002(3) -0.004(3) -0.006(3) C34 0.032(4) 0.040(4) 0.033(4) 0.007(3) -0.008(3) 0.007(3) C35 0.019(3) 0.021(3) 0.017(3) -0.001(2) 0.001(2) 0.005(2) C36 0.019(3) 0.018(3) 0.020(3) 0.000(2) 0.004(2) 0.006(2) C37 0.026(3) 0.035(4) 0.018(3) 0.004(3) -0.001(3) -0.006(3) C38 0.043(4) 0.060(5) 0.036(4) 0.014(4) -0.004(3) 0.008(4) C39 0.044(4) 0.043(4) 0.020(3) 0.000(3) 0.005(3) -0.015(3) C40 0.038(4) 0.022(3) 0.019(3) 0.001(3) 0.001(3) -0.009(3) C41 0.066(5) 0.022(4) 0.039(4) -0.004(3) 0.012(4) -0.003(4) C42 0.031(4) 0.032(4) 0.031(4) 0.000(3) 0.001(3) -0.015(3) Co1 0.0154(4) 0.0160(4) 0.0161(4) 0.0004(3) 0.0008(3) 0.0014(3) N1 0.016(3) 0.028(3) 0.024(3) -0.005(2) 0.005(2) 0.002(2) N2 0.017(2) 0.024(3) 0.018(3) -0.002(2) 0.001(2) 0.001(2) N3 0.019(3) 0.025(3) 0.019(3) -0.004(2) 0.002(2) -0.001(2) N4 0.018(3) 0.026(3) 0.017(3) 0.006(2) 0.004(2) 0.004(2) N5 0.012(2) 0.025(3) 0.018(3) 0.004(2) 0.0011(19) 0.004(2) N6 0.018(3) 0.026(3) 0.025(3) 0.001(2) 0.003(2) 0.006(2) N7 0.016(3) 0.032(3) 0.017(3) 0.000(2) -0.003(2) -0.005(2) N8 0.019(3) 0.024(3) 0.017(3) 0.003(2) 0.001(2) -0.001(2) N9 0.027(3) 0.023(3) 0.017(3) 0.002(2) 0.001(2) -0.003(2) O1 0.014(2) 0.019(2) 0.021(2) -0.0041(16) 0.0001(16) -0.0019(16) O2 0.021(2) 0.021(2) 0.019(2) 0.0000(17) 0.0060(17) 0.0045(17) O3 0.024(2) 0.015(2) 0.015(2) 0.0033(16) 0.0000(17) -0.0005(17) S1 0.0176(7) 0.0208(8) 0.0192(8) -0.0029(6) 0.0021(6) -0.0009(6) S2 0.0180(7) 0.0208(8) 0.0179(7) 0.0027(6) 0.0033(6) 0.0035(6) S3 0.0179(8) 0.0215(8) 0.0202(8) 0.0027(6) -0.0012(6) -0.0019(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 C1 N1 1.488(7) . ? C1 C2 1.518(8) . ? C1 C3 1.534(8) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.481(7) . ? C4 C5 1.533(9) . ? C4 C6 1.536(9) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N2 1.316(7) . ? C7 N1 1.352(7) . ? C7 S1 1.763(6) . ? C8 O1 1.274(6) . ? C8 N2 1.342(7) . ? C8 N3 1.364(7) . ? C9 N3 1.482(7) . ? C9 C11 1.507(8) . ? C9 C10 1.531(8) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N3 1.462(7) . ? C12 C13 1.524(8) . ? C12 C14 1.539(8) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 N4 1.479(7) . ? C15 C16 1.520(8) . ? C15 C17 1.529(8) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 N4 1.482(7) . ? C18 C19 1.524(8) . ? C18 C20 1.536(8) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 N5 1.316(7) . ? C21 N4 1.354(7) . ? C21 S2 1.755(6) . ? C22 O2 1.270(6) . ? C22 N5 1.356(7) . ? C22 N6 1.362(7) . ? C23 N6 1.479(7) . ? C23 C25 1.508(8) . ? C23 C24 1.538(8) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N6 1.484(7) . ? C26 C28 1.516(9) . ? C26 C27 1.516(8) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N7 1.483(7) . ? C29 C30 1.516(8) . ? C29 C31 1.527(8) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 N7 1.482(7) . ? C32 C33 1.515(8) . ? C32 C34 1.516(8) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 N8 1.319(7) . ? C35 N7 1.354(7) . ? C35 S3 1.770(6) . ? C36 O3 1.275(6) . ? C36 N8 1.352(7) . ? C36 N9 1.354(7) . ? C37 N9 1.479(7) . ? C37 C38 1.517(9) . ? C37 C39 1.518(8) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 N9 1.494(7) . ? C40 C42 1.529(8) . ? C40 C41 1.539(8) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? Co1 O1 1.932(4) . ? Co1 O3 1.932(4) . ? Co1 O2 1.935(4) . ? Co1 S3 2.1920(16) . ? Co1 S2 2.1987(16) . ? Co1 S1 2.2008(16) . ? C44 C45 1.4465 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 N10 1.1339 . ? C46 C47 1.4465 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N11 1.1339 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 113.5(5) . . ? N1 C1 C3 112.1(5) . . ? C2 C1 C3 113.7(5) . . ? N1 C1 H1 105.5 . . ? C2 C1 H1 105.5 . . ? C3 C1 H1 105.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 111.8(5) . . ? N1 C4 C6 111.5(5) . . ? C5 C4 C6 112.4(5) . . ? N1 C4 H4 106.9 . . ? C5 C4 H4 106.9 . . ? C6 C4 H4 106.9 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 N1 116.7(5) . . ? N2 C7 S1 127.6(4) . . ? N1 C7 S1 115.6(4) . . ? O1 C8 N2 128.5(5) . . ? O1 C8 N3 115.2(5) . . ? N2 C8 N3 116.2(5) . . ? N3 C9 C11 112.1(5) . . ? N3 C9 C10 110.5(5) . . ? C11 C9 C10 111.8(5) . . ? N3 C9 H9 107.4 . . ? C11 C9 H9 107.4 . . ? C10 C9 H9 107.4 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C13 112.6(5) . . ? N3 C12 C14 113.0(5) . . ? C13 C12 C14 112.1(5) . . ? N3 C12 H12 106.2 . . ? C13 C12 H12 106.2 . . ? C14 C12 H12 106.2 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N4 C15 C16 110.8(5) . . ? N4 C15 C17 113.1(5) . . ? C16 C15 C17 111.0(5) . . ? N4 C15 H15 107.2 . . ? C16 C15 H15 107.2 . . ? C17 C15 H15 107.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C19 113.6(5) . . ? N4 C18 C20 111.9(5) . . ? C19 C18 C20 113.3(5) . . ? N4 C18 H18 105.8 . . ? C19 C18 H18 105.8 . . ? C20 C18 H18 105.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N5 C21 N4 115.9(5) . . ? N5 C21 S2 127.8(4) . . ? N4 C21 S2 116.2(4) . . ? O2 C22 N5 128.0(5) . . ? O2 C22 N6 116.2(5) . . ? N5 C22 N6 115.6(5) . . ? N6 C23 C25 110.6(5) . . ? N6 C23 C24 112.3(5) . . ? C25 C23 C24 111.8(5) . . ? N6 C23 H23 107.2 . . ? C25 C23 H23 107.2 . . ? C24 C23 H23 107.2 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 C28 111.7(5) . . ? N6 C26 C27 114.2(5) . . ? C28 C26 C27 111.1(5) . . ? N6 C26 H26 106.4 . . ? C28 C26 H26 106.4 . . ? C27 C26 H26 106.4 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N7 C29 C30 111.8(5) . . ? N7 C29 C31 111.6(5) . . ? C30 C29 C31 112.6(5) . . ? N7 C29 H29 106.8 . . ? C30 C29 H29 106.8 . . ? C31 C29 H29 106.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N7 C32 C33 113.8(5) . . ? N7 C32 C34 111.9(5) . . ? C33 C32 C34 113.8(5) . . ? N7 C32 H32 105.5 . . ? C33 C32 H32 105.5 . . ? C34 C32 H32 105.5 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N8 C35 N7 117.2(5) . . ? N8 C35 S3 127.5(4) . . ? N7 C35 S3 115.2(4) . . ? O3 C36 N8 127.4(5) . . ? O3 C36 N9 116.6(5) . . ? N8 C36 N9 115.8(5) . . ? N9 C37 C38 112.2(5) . . ? N9 C37 C39 111.4(5) . . ? C38 C37 C39 111.7(5) . . ? N9 C37 H37 107.1 . . ? C38 C37 H37 107.1 . . ? C39 C37 H37 107.1 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N9 C40 C42 112.8(5) . . ? N9 C40 C41 111.7(5) . . ? C42 C40 C41 112.9(5) . . ? N9 C40 H40 106.3 . . ? C42 C40 H40 106.3 . . ? C41 C40 H40 106.3 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 Co1 O3 86.35(16) . . ? O1 Co1 O2 86.62(16) . . ? O3 Co1 O2 85.29(16) . . ? O1 Co1 S3 178.73(12) . . ? O3 Co1 S3 92.85(12) . . ? O2 Co1 S3 92.33(12) . . ? O1 Co1 S2 91.66(12) . . ? O3 Co1 S2 177.75(12) . . ? O2 Co1 S2 93.55(12) . . ? S3 Co1 S2 89.12(6) . . ? O1 Co1 S1 93.11(12) . . ? O3 Co1 S1 92.06(12) . . ? O2 Co1 S1 177.35(12) . . ? S3 Co1 S1 87.91(6) . . ? S2 Co1 S1 89.09(6) . . ? C7 N1 C4 123.1(5) . . ? C7 N1 C1 121.5(5) . . ? C4 N1 C1 115.4(5) . . ? C7 N2 C8 123.6(5) . . ? C8 N3 C12 120.7(5) . . ? C8 N3 C9 121.8(5) . . ? C12 N3 C9 117.6(4) . . ? C21 N4 C15 121.3(5) . . ? C21 N4 C18 122.2(5) . . ? C15 N4 C18 116.3(4) . . ? C21 N5 C22 124.6(5) . . ? C22 N6 C23 121.5(5) . . ? C22 N6 C26 121.1(5) . . ? C23 N6 C26 117.2(5) . . ? C35 N7 C32 122.0(5) . . ? C35 N7 C29 122.1(5) . . ? C32 N7 C29 115.8(4) . . ? C35 N8 C36 123.7(5) . . ? C36 N9 C37 121.9(5) . . ? C36 N9 C40 120.7(5) . . ? C37 N9 C40 117.0(5) . . ? C8 O1 Co1 126.5(3) . . ? C22 O2 Co1 128.0(4) . . ? C36 O3 Co1 125.9(4) . . ? C7 S1 Co1 107.5(2) . . ? C21 S2 Co1 108.1(2) . . ? C35 S3 Co1 108.2(2) . . ? N10 C45 C44 179.4 . . ? C47 C46 H46A 109.5 . . ? C47 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C47 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N11 C47 C46 179.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C7 N1 C4 -176.8(5) . . . . ? S1 C7 N1 C4 7.3(7) . . . . ? N2 C7 N1 C1 4.5(8) . . . . ? S1 C7 N1 C1 -171.5(4) . . . . ? C5 C4 N1 C7 120.2(6) . . . . ? C6 C4 N1 C7 -113.0(6) . . . . ? C5 C4 N1 C1 -61.0(7) . . . . ? C6 C4 N1 C1 65.8(7) . . . . ? C2 C1 N1 C7 -65.8(7) . . . . ? C3 C1 N1 C7 64.7(7) . . . . ? C2 C1 N1 C4 115.3(6) . . . . ? C3 C1 N1 C4 -114.1(6) . . . . ? N1 C7 N2 C8 161.2(5) . . . . ? S1 C7 N2 C8 -23.4(8) . . . . ? O1 C8 N2 C7 -4.7(9) . . . . ? N3 C8 N2 C7 180.0(5) . . . . ? O1 C8 N3 C12 -1.6(7) . . . . ? N2 C8 N3 C12 174.4(5) . . . . ? O1 C8 N3 C9 179.3(5) . . . . ? N2 C8 N3 C9 -4.8(8) . . . . ? C13 C12 N3 C8 -64.6(7) . . . . ? C14 C12 N3 C8 63.6(7) . . . . ? C13 C12 N3 C9 114.6(6) . . . . ? C14 C12 N3 C9 -117.2(5) . . . . ? C11 C9 N3 C8 -114.7(6) . . . . ? C10 C9 N3 C8 119.8(6) . . . . ? C11 C9 N3 C12 66.1(7) . . . . ? C10 C9 N3 C12 -59.4(7) . . . . ? N5 C21 N4 C15 177.0(5) . . . . ? S2 C21 N4 C15 -0.3(7) . . . . ? N5 C21 N4 C18 -8.3(8) . . . . ? S2 C21 N4 C18 174.4(4) . . . . ? C16 C15 N4 C21 104.7(6) . . . . ? C17 C15 N4 C21 -129.9(6) . . . . ? C16 C15 N4 C18 -70.3(7) . . . . ? C17 C15 N4 C18 55.1(7) . . . . ? C19 C18 N4 C21 -56.5(7) . . . . ? C20 C18 N4 C21 73.3(7) . . . . ? C19 C18 N4 C15 118.5(6) . . . . ? C20 C18 N4 C15 -111.7(6) . . . . ? N4 C21 N5 C22 163.8(5) . . . . ? S2 C21 N5 C22 -19.3(8) . . . . ? O2 C22 N5 C21 -5.9(9) . . . . ? N6 C22 N5 C21 178.6(5) . . . . ? O2 C22 N6 C23 178.3(5) . . . . ? N5 C22 N6 C23 -5.7(7) . . . . ? O2 C22 N6 C26 2.7(8) . . . . ? N5 C22 N6 C26 178.7(5) . . . . ? C25 C23 N6 C22 -110.4(6) . . . . ? C24 C23 N6 C22 123.8(6) . . . . ? C25 C23 N6 C26 65.4(7) . . . . ? C24 C23 N6 C26 -60.4(7) . . . . ? C28 C26 N6 C22 -65.8(7) . . . . ? C27 C26 N6 C22 61.3(7) . . . . ? C28 C26 N6 C23 118.4(6) . . . . ? C27 C26 N6 C23 -114.5(6) . . . . ? N8 C35 N7 C32 -16.0(8) . . . . ? S3 C35 N7 C32 165.7(4) . . . . ? N8 C35 N7 C29 168.6(5) . . . . ? S3 C35 N7 C29 -9.7(7) . . . . ? C33 C32 N7 C35 74.7(7) . . . . ? C34 C32 N7 C35 -56.0(7) . . . . ? C33 C32 N7 C29 -109.6(6) . . . . ? C34 C32 N7 C29 119.7(6) . . . . ? C30 C29 N7 C35 -125.0(6) . . . . ? C31 C29 N7 C35 107.8(6) . . . . ? C30 C29 N7 C32 59.3(7) . . . . ? C31 C29 N7 C32 -67.9(6) . . . . ? N7 C35 N8 C36 165.1(5) . . . . ? S3 C35 N8 C36 -16.8(8) . . . . ? O3 C36 N8 C35 -13.5(9) . . . . ? N9 C36 N8 C35 171.6(5) . . . . ? O3 C36 N9 C37 180.0(5) . . . . ? N8 C36 N9 C37 -4.6(8) . . . . ? O3 C36 N9 C40 -7.7(8) . . . . ? N8 C36 N9 C40 167.7(5) . . . . ? C38 C37 N9 C36 103.9(6) . . . . ? C39 C37 N9 C36 -130.0(6) . . . . ? C38 C37 N9 C40 -68.6(7) . . . . ? C39 C37 N9 C40 57.4(7) . . . . ? C42 C40 N9 C36 70.9(7) . . . . ? C41 C40 N9 C36 -57.4(7) . . . . ? C42 C40 N9 C37 -116.5(6) . . . . ? C41 C40 N9 C37 115.2(6) . . . . ? N2 C8 O1 Co1 40.9(8) . . . . ? N3 C8 O1 Co1 -143.8(4) . . . . ? O3 Co1 O1 C8 -128.5(4) . . . . ? O2 Co1 O1 C8 146.0(4) . . . . ? S3 Co1 O1 C8 -180(100) . . . . ? S2 Co1 O1 C8 52.6(4) . . . . ? S1 Co1 O1 C8 -36.6(4) . . . . ? N5 C22 O2 Co1 37.1(8) . . . . ? N6 C22 O2 Co1 -147.4(4) . . . . ? O1 Co1 O2 C22 -123.8(4) . . . . ? O3 Co1 O2 C22 149.5(5) . . . . ? S3 Co1 O2 C22 56.9(4) . . . . ? S2 Co1 O2 C22 -32.4(4) . . . . ? S1 Co1 O2 C22 152(2) . . . . ? N8 C36 O3 Co1 47.7(8) . . . . ? N9 C36 O3 Co1 -137.4(4) . . . . ? O1 Co1 O3 C36 142.0(4) . . . . ? O2 Co1 O3 C36 -131.1(4) . . . . ? S3 Co1 O3 C36 -39.0(4) . . . . ? S2 Co1 O3 C36 170(3) . . . . ? S1 Co1 O3 C36 49.0(4) . . . . ? N2 C7 S1 Co1 13.8(6) . . . . ? N1 C7 S1 Co1 -170.8(4) . . . . ? O1 Co1 S1 C7 10.4(2) . . . . ? O3 Co1 S1 C7 96.9(2) . . . . ? O2 Co1 S1 C7 94(3) . . . . ? S3 Co1 S1 C7 -170.4(2) . . . . ? S2 Co1 S1 C7 -81.2(2) . . . . ? N5 C21 S2 Co1 12.1(6) . . . . ? N4 C21 S2 Co1 -171.0(4) . . . . ? O1 Co1 S2 C21 95.3(2) . . . . ? O3 Co1 S2 C21 67(3) . . . . ? O2 Co1 S2 C21 8.6(2) . . . . ? S3 Co1 S2 C21 -83.72(19) . . . . ? S1 Co1 S2 C21 -171.64(19) . . . . ? N8 C35 S3 Co1 11.3(6) . . . . ? N7 C35 S3 Co1 -170.5(4) . . . . ? O1 Co1 S3 C35 62(6) . . . . ? O3 Co1 S3 C35 10.7(2) . . . . ? O2 Co1 S3 C35 96.1(2) . . . . ? S2 Co1 S3 C35 -170.4(2) . . . . ? S1 Co1 S3 C35 -81.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.250 _refine_diff_density_min -0.601 _refine_diff_density_rms 0.117 # start Validation Reply Form _vrf_SHFSU01_s2987n ; PROBLEM: The absolute value of parameter shift to su ratio > 0.20 RESPONSE:The disordered MeCN,to obtain a formally correct electron count,had the Hs placed in calculated positions. ; _vrf_PLAT080_s2987n ; PROBLEM: Maximum Shift/Error ............................ 1.03 RESPONSE:Vide ultra ; _vrf_PLAT221_s2987n ; PROBLEM: Large Solvent/Anion C Ueq(max)/Ueq(min) ... 10.00 Ratio RESPONSE:MeCN disordered solvent. ; # end Validation Reply Form # Attachment 's2995abs.cif' data_z:\s2995\work\s2995abs _database_code_depnum_ccdc_archive 'CCDC 715963' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H40 N6 Ni S4' _chemical_formula_weight 551.53 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4941(15) _cell_length_b 11.4556(17) _cell_length_c 13.758(2) _cell_angle_alpha 89.628(3) _cell_angle_beta 89.726(3) _cell_angle_gamma 67.548(3) _cell_volume 1382.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 955 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.57 _exptl_crystal_description plate _exptl_crystal_colour brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_absorpt_coefficient_mu 1.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8092 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 26.43 _reflns_number_total 5529 _reflns_number_gt 4311 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0312P)^2^+1.8406P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5529 _refine_ls_number_parameters 291 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0651 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0991 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _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 Ni1 Ni 0.5000 0.0000 0.5000 0.01300(15) Uani 1 2 d S . . S1 S 0.35524(10) 0.17290(8) 0.42863(6) 0.0183(2) Uani 1 1 d . . . S2 S 0.34261(10) -0.09386(8) 0.48747(6) 0.0187(2) Uani 1 1 d . . . N1 N 0.1856(3) 0.2411(3) 0.2719(2) 0.0202(7) Uani 1 1 d . . . N2 N 0.2014(3) 0.0503(3) 0.3253(2) 0.0177(6) Uani 1 1 d . . . N3 N 0.1410(3) -0.1157(3) 0.3675(2) 0.0195(7) Uani 1 1 d . . . C1 C 0.2425(4) 0.1478(3) 0.3381(2) 0.0163(7) Uani 1 1 d . . . C2 C 0.2044(4) 0.3616(4) 0.2776(3) 0.0262(9) Uani 1 1 d . . . H2A H 0.1968 0.3981 0.2115 0.031 Uiso 1 1 calc R . . H2B H 0.3073 0.3468 0.3029 0.031 Uiso 1 1 calc R . . C3 C 0.0858(5) 0.4554(4) 0.3427(3) 0.0336(10) Uani 1 1 d . . . H3A H -0.0163 0.4647 0.3214 0.050 Uiso 1 1 calc R . . H3B H 0.0956 0.5374 0.3387 0.050 Uiso 1 1 calc R . . H3C H 0.1015 0.4248 0.4100 0.050 Uiso 1 1 calc R . . C4 C 0.0916(4) 0.2285(4) 0.1910(3) 0.0254(9) Uani 1 1 d . . . H4A H 0.0216 0.3135 0.1696 0.031 Uiso 1 1 calc R . . H4B H 0.0292 0.1814 0.2137 0.031 Uiso 1 1 calc R . . C5 C 0.1900(5) 0.1596(4) 0.1058(3) 0.0363(10) Uani 1 1 d . . . H5A H 0.2530 0.2055 0.0840 0.054 Uiso 1 1 calc R . . H5B H 0.1246 0.1549 0.0524 0.054 Uiso 1 1 calc R . . H5C H 0.2560 0.0741 0.1262 0.054 Uiso 1 1 calc R . . C6 C 0.2244(4) -0.0458(3) 0.3864(2) 0.0171(7) Uani 1 1 d . . . C7 C 0.0129(4) -0.0699(4) 0.2991(3) 0.0227(8) Uani 1 1 d . . . H7A H -0.0297 0.0236 0.2990 0.027 Uiso 1 1 calc R . . H7B H -0.0680 -0.0982 0.3217 0.027 Uiso 1 1 calc R . . C8 C 0.0580(5) -0.1162(4) 0.1959(3) 0.0366(10) Uani 1 1 d . . . H8A H 0.1325 -0.0831 0.1712 0.055 Uiso 1 1 calc R . . H8B H -0.0326 -0.0865 0.1544 0.055 Uiso 1 1 calc R . . H8C H 0.1031 -0.2087 0.1957 0.055 Uiso 1 1 calc R . . C9 C 0.1632(4) -0.2350(3) 0.4163(3) 0.0239(8) Uani 1 1 d . . . H9A H 0.2708 -0.2751 0.4374 0.029 Uiso 1 1 calc R . . H9B H 0.1441 -0.2922 0.3693 0.029 Uiso 1 1 calc R . . C10 C 0.0606(4) -0.2202(4) 0.5039(3) 0.0299(9) Uani 1 1 d . . . H10A H 0.0804 -0.1652 0.5516 0.045 Uiso 1 1 calc R . . H10B H 0.0813 -0.3033 0.5333 0.045 Uiso 1 1 calc R . . H10C H -0.0462 -0.1828 0.4835 0.045 Uiso 1 1 calc R . . Ni2 Ni 1.0000 0.5000 0.0000 0.01430(15) Uani 1 2 d S . . S3 S 0.88691(10) 0.62741(9) 0.11653(6) 0.0200(2) Uani 1 1 d . . . S4 S 0.82038(10) 0.42878(9) -0.02065(6) 0.0198(2) Uani 1 1 d . . . N4 N 0.6810(3) 0.6655(3) 0.2535(2) 0.0194(6) Uani 1 1 d . . . N5 N 0.7098(3) 0.4906(3) 0.1667(2) 0.0164(6) Uani 1 1 d . . . N6 N 0.6737(3) 0.3286(3) 0.0940(2) 0.0185(6) Uani 1 1 d . . . C11 C 0.7507(4) 0.5896(3) 0.1792(2) 0.0170(7) Uani 1 1 d . . . C12 C 0.7180(4) 0.7729(3) 0.2845(3) 0.0244(8) Uani 1 1 d . . . H12A H 0.8268 0.7541 0.2704 0.029 Uiso 1 1 calc R . . H12B H 0.7032 0.7831 0.3557 0.029 Uiso 1 1 calc R . . C13 C 0.6222(4) 0.8951(4) 0.2351(3) 0.0307(9) Uani 1 1 d . . . H13A H 0.6404 0.8872 0.1648 0.046 Uiso 1 1 calc R . . H13B H 0.6497 0.9636 0.2599 0.046 Uiso 1 1 calc R . . H13C H 0.5142 0.9141 0.2483 0.046 Uiso 1 1 calc R . . C14 C 0.5608(4) 0.6449(3) 0.3095(3) 0.0241(8) Uani 1 1 d . . . H14A H 0.5050 0.6086 0.2664 0.029 Uiso 1 1 calc R . . H14B H 0.4875 0.7272 0.3333 0.029 Uiso 1 1 calc R . . C15 C 0.6238(5) 0.5568(4) 0.3956(3) 0.0333(10) Uani 1 1 d . . . H15A H 0.6908 0.4733 0.3721 0.050 Uiso 1 1 calc R . . H15B H 0.5394 0.5491 0.4328 0.050 Uiso 1 1 calc R . . H15C H 0.6819 0.5910 0.4375 0.050 Uiso 1 1 calc R . . C16 C 0.7328(4) 0.4192(3) 0.0886(2) 0.0172(7) Uani 1 1 d . . . C17 C 0.5769(4) 0.3247(4) 0.1770(3) 0.0228(8) Uani 1 1 d . . . H17A H 0.4999 0.2921 0.1549 0.027 Uiso 1 1 calc R . . H17B H 0.5223 0.4116 0.2015 0.027 Uiso 1 1 calc R . . C18 C 0.6690(4) 0.2420(4) 0.2587(3) 0.0303(9) Uani 1 1 d . . . H18A H 0.7284 0.1574 0.2338 0.045 Uiso 1 1 calc R . . H18B H 0.6000 0.2362 0.3100 0.045 Uiso 1 1 calc R . . H18C H 0.7382 0.2789 0.2853 0.045 Uiso 1 1 calc R . . C19 C 0.7010(4) 0.2295(3) 0.0217(3) 0.0228(8) Uani 1 1 d . . . H19A H 0.7072 0.1508 0.0548 0.027 Uiso 1 1 calc R . . H19B H 0.8003 0.2130 -0.0105 0.027 Uiso 1 1 calc R . . C20 C 0.5774(4) 0.2642(4) -0.0549(3) 0.0312(9) Uani 1 1 d . . . H20A H 0.4775 0.2899 -0.0231 0.047 Uiso 1 1 calc R . . H20B H 0.5933 0.1910 -0.0963 0.047 Uiso 1 1 calc R . . H20C H 0.5812 0.3342 -0.0947 0.047 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0112(3) 0.0138(3) 0.0147(3) 0.0006(2) -0.0006(2) -0.0056(2) S1 0.0183(4) 0.0176(5) 0.0206(5) 0.0015(4) -0.0042(3) -0.0087(4) S2 0.0172(4) 0.0206(5) 0.0210(5) 0.0042(4) -0.0033(3) -0.0104(4) N1 0.0175(15) 0.0207(16) 0.0215(16) 0.0028(13) 0.0001(12) -0.0064(13) N2 0.0161(15) 0.0220(16) 0.0161(15) -0.0009(12) -0.0006(12) -0.0084(13) N3 0.0171(15) 0.0199(16) 0.0229(16) -0.0044(13) 0.0015(12) -0.0085(13) C1 0.0119(16) 0.0193(18) 0.0155(17) 0.0000(14) 0.0029(13) -0.0036(14) C2 0.026(2) 0.027(2) 0.029(2) 0.0089(17) -0.0032(16) -0.0146(17) C3 0.037(2) 0.022(2) 0.043(3) 0.0007(18) -0.0025(19) -0.0115(18) C4 0.025(2) 0.028(2) 0.023(2) 0.0088(16) -0.0088(16) -0.0095(17) C5 0.044(3) 0.037(3) 0.023(2) 0.0006(18) -0.0023(18) -0.011(2) C6 0.0126(16) 0.0187(18) 0.0192(18) -0.0071(14) 0.0029(13) -0.0051(14) C7 0.0188(18) 0.029(2) 0.025(2) -0.0046(16) -0.0021(15) -0.0142(16) C8 0.043(3) 0.049(3) 0.025(2) -0.0081(19) -0.0032(19) -0.025(2) C9 0.0192(18) 0.0189(19) 0.036(2) -0.0071(16) 0.0036(16) -0.0093(15) C10 0.022(2) 0.032(2) 0.039(2) 0.0046(18) 0.0039(17) -0.0138(17) Ni2 0.0130(3) 0.0164(3) 0.0141(3) -0.0005(2) 0.0029(2) -0.0062(3) S3 0.0206(4) 0.0221(5) 0.0205(5) -0.0050(4) 0.0086(4) -0.0117(4) S4 0.0199(4) 0.0260(5) 0.0174(5) -0.0040(4) 0.0053(3) -0.0132(4) N4 0.0187(15) 0.0203(16) 0.0197(16) -0.0051(12) 0.0066(12) -0.0080(13) N5 0.0130(14) 0.0193(16) 0.0182(15) -0.0013(12) 0.0022(11) -0.0074(12) N6 0.0160(15) 0.0204(16) 0.0195(16) 0.0008(12) 0.0012(12) -0.0076(12) C11 0.0117(16) 0.0192(18) 0.0176(18) 0.0022(14) -0.0007(13) -0.0033(14) C12 0.0215(19) 0.029(2) 0.025(2) -0.0093(16) 0.0081(15) -0.0116(16) C13 0.030(2) 0.025(2) 0.039(2) -0.0079(18) 0.0051(18) -0.0125(18) C14 0.0224(19) 0.025(2) 0.026(2) -0.0066(16) 0.0129(16) -0.0098(16) C15 0.038(2) 0.034(2) 0.028(2) 0.0021(18) 0.0114(18) -0.0141(19) C16 0.0110(16) 0.0180(18) 0.0189(18) 0.0018(14) 0.0006(13) -0.0015(14) C17 0.0195(18) 0.027(2) 0.027(2) 0.0014(16) 0.0023(15) -0.0137(16) C18 0.025(2) 0.038(2) 0.031(2) 0.0103(18) 0.0053(17) -0.0161(18) C19 0.0214(18) 0.021(2) 0.028(2) -0.0013(16) -0.0019(15) -0.0105(16) C20 0.025(2) 0.039(2) 0.032(2) -0.0029(19) -0.0008(17) -0.0134(18) _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 S2 2.1565(9) . ? Ni1 S2 2.1565(9) 2_656 ? Ni1 S1 2.1643(9) 2_656 ? Ni1 S1 2.1644(9) . ? S1 C1 1.741(3) . ? S2 C6 1.740(3) . ? N1 C1 1.347(4) . ? N1 C2 1.460(5) . ? N1 C4 1.471(4) . ? N2 C1 1.329(4) . ? N2 C6 1.332(4) . ? N3 C6 1.350(4) . ? N3 C9 1.460(5) . ? N3 C7 1.469(4) . ? C2 C3 1.517(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.519(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.519(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.515(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? Ni2 S3 2.1611(9) . ? Ni2 S3 2.1612(9) 2_765 ? Ni2 S4 2.1737(9) 2_765 ? Ni2 S4 2.1737(9) . ? S3 C11 1.736(3) . ? S4 C16 1.737(3) . ? N4 C11 1.344(4) . ? N4 C14 1.465(4) . ? N4 C12 1.468(5) . ? N5 C16 1.321(4) . ? N5 C11 1.344(4) . ? N6 C16 1.356(4) . ? N6 C19 1.461(4) . ? N6 C17 1.472(4) . ? C12 C13 1.508(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.521(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C18 1.513(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.515(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 S2 Ni1 S2 180.0 . 2_656 ? S2 Ni1 S1 84.35(3) . 2_656 ? S2 Ni1 S1 95.65(3) 2_656 2_656 ? S2 Ni1 S1 95.65(3) . . ? S2 Ni1 S1 84.35(3) 2_656 . ? S1 Ni1 S1 180.0 2_656 . ? C1 S1 Ni1 112.89(12) . . ? C6 S2 Ni1 113.43(12) . . ? C1 N1 C2 123.5(3) . . ? C1 N1 C4 120.5(3) . . ? C2 N1 C4 115.9(3) . . ? C1 N2 C6 126.9(3) . . ? C6 N3 C9 123.8(3) . . ? C6 N3 C7 120.6(3) . . ? C9 N3 C7 115.5(3) . . ? N2 C1 N1 114.6(3) . . ? N2 C1 S1 129.4(3) . . ? N1 C1 S1 116.0(3) . . ? N1 C2 C3 112.3(3) . . ? N1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? N1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 111.2(3) . . ? N1 C4 H4A 109.4 . . ? C5 C4 H4A 109.4 . . ? N1 C4 H4B 109.4 . . ? C5 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 N3 114.7(3) . . ? N2 C6 S2 130.1(3) . . ? N3 C6 S2 115.2(3) . . ? N3 C7 C8 113.1(3) . . ? N3 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N3 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 113.5(3) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? S3 Ni2 S3 180.00(3) . 2_765 ? S3 Ni2 S4 84.45(3) . 2_765 ? S3 Ni2 S4 95.55(3) 2_765 2_765 ? S3 Ni2 S4 95.55(3) . . ? S3 Ni2 S4 84.45(3) 2_765 . ? S4 Ni2 S4 179.999(1) 2_765 . ? C11 S3 Ni2 114.97(12) . . ? C16 S4 Ni2 111.65(12) . . ? C11 N4 C14 121.0(3) . . ? C11 N4 C12 123.5(3) . . ? C14 N4 C12 115.5(3) . . ? C16 N5 C11 126.9(3) . . ? C16 N6 C19 123.9(3) . . ? C16 N6 C17 120.4(3) . . ? C19 N6 C17 115.7(3) . . ? N4 C11 N5 114.8(3) . . ? N4 C11 S3 116.3(3) . . ? N5 C11 S3 128.8(3) . . ? N4 C12 C13 113.1(3) . . ? N4 C12 H12A 109.0 . . ? C13 C12 H12A 109.0 . . ? N4 C12 H12B 109.0 . . ? C13 C12 H12B 109.0 . . ? H12A C12 H12B 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 112.3(3) . . ? N4 C14 H14A 109.2 . . ? C15 C14 H14A 109.2 . . ? N4 C14 H14B 109.2 . . ? C15 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 N6 114.5(3) . . ? N5 C16 S4 129.4(3) . . ? N6 C16 S4 116.0(3) . . ? N6 C17 C18 111.9(3) . . ? N6 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N6 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 112.6(3) . . ? N6 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N6 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Ni1 S1 C1 -32.97(12) . . . . ? S2 Ni1 S1 C1 147.03(12) 2_656 . . . ? S1 Ni1 S1 C1 -160(19) 2_656 . . . ? S2 Ni1 S2 C6 11(7) 2_656 . . . ? S1 Ni1 S2 C6 -150.73(12) 2_656 . . . ? S1 Ni1 S2 C6 29.27(12) . . . . ? C6 N2 C1 N1 -170.6(3) . . . . ? C6 N2 C1 S1 8.0(5) . . . . ? C2 N1 C1 N2 174.0(3) . . . . ? C4 N1 C1 N2 -2.5(4) . . . . ? C2 N1 C1 S1 -4.8(4) . . . . ? C4 N1 C1 S1 178.7(2) . . . . ? Ni1 S1 C1 N2 20.8(3) . . . . ? Ni1 S1 C1 N1 -160.6(2) . . . . ? C1 N1 C2 C3 -83.9(4) . . . . ? C4 N1 C2 C3 92.7(4) . . . . ? C1 N1 C4 C5 -85.9(4) . . . . ? C2 N1 C4 C5 97.3(4) . . . . ? C1 N2 C6 N3 164.9(3) . . . . ? C1 N2 C6 S2 -14.0(5) . . . . ? C9 N3 C6 N2 171.1(3) . . . . ? C7 N3 C6 N2 -12.9(4) . . . . ? C9 N3 C6 S2 -9.8(4) . . . . ? C7 N3 C6 S2 166.2(2) . . . . ? Ni1 S2 C6 N2 -10.9(4) . . . . ? Ni1 S2 C6 N3 170.2(2) . . . . ? C6 N3 C7 C8 93.1(4) . . . . ? C9 N3 C7 C8 -90.6(4) . . . . ? C6 N3 C9 C10 93.9(4) . . . . ? C7 N3 C9 C10 -82.3(4) . . . . ? S3 Ni2 S3 C11 140(100) 2_765 . . . ? S4 Ni2 S3 C11 -157.40(13) 2_765 . . . ? S4 Ni2 S3 C11 22.60(13) . . . . ? S3 Ni2 S4 C16 -34.68(13) . . . . ? S3 Ni2 S4 C16 145.32(13) 2_765 . . . ? S4 Ni2 S4 C16 -178(14) 2_765 . . . ? C14 N4 C11 N5 -5.0(5) . . . . ? C12 N4 C11 N5 174.9(3) . . . . ? C14 N4 C11 S3 178.1(3) . . . . ? C12 N4 C11 S3 -2.0(4) . . . . ? C16 N5 C11 N4 163.6(3) . . . . ? C16 N5 C11 S3 -20.0(5) . . . . ? Ni2 S3 C11 N4 178.5(2) . . . . ? Ni2 S3 C11 N5 2.1(4) . . . . ? C11 N4 C12 C13 91.2(4) . . . . ? C14 N4 C12 C13 -88.9(4) . . . . ? C11 N4 C14 C15 89.7(4) . . . . ? C12 N4 C14 C15 -90.2(4) . . . . ? C11 N5 C16 N6 -177.3(3) . . . . ? C11 N5 C16 S4 -0.1(5) . . . . ? C19 N6 C16 N5 -172.3(3) . . . . ? C17 N6 C16 N5 7.0(4) . . . . ? C19 N6 C16 S4 10.2(4) . . . . ? C17 N6 C16 S4 -170.6(2) . . . . ? Ni2 S4 C16 N5 31.7(3) . . . . ? Ni2 S4 C16 N6 -151.1(2) . . . . ? C16 N6 C17 C18 -91.3(4) . . . . ? C19 N6 C17 C18 88.1(4) . . . . ? C16 N6 C19 C20 -94.2(4) . . . . ? C17 N6 C19 C20 86.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.553 _refine_diff_density_min -0.326 _refine_diff_density_rms 0.080 # Attachment 's3006p.cif' data_s3006p _database_code_depnum_ccdc_archive 'CCDC 715965' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 Cu N6 O2 S2' _chemical_formula_weight 636.45 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.952(2) _cell_length_b 11.127(3) _cell_length_c 11.142(3) _cell_angle_alpha 65.992(6) _cell_angle_beta 72.469(5) _cell_angle_gamma 79.123(6) _cell_volume 856.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 241 _cell_measurement_theta_min 2.2785 _cell_measurement_theta_max 16.307 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 343 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5384 _diffrn_reflns_av_R_equivalents 0.0877 _diffrn_reflns_av_sigmaI/netI 0.4533 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.35 _reflns_number_total 3796 _reflns_number_gt 1131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3796 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1681 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 0.491 _refine_ls_restrained_S_all 0.491 _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 C1 C 0.2304(6) 0.4803(4) -0.3312(4) 0.0254(13) Uani 1 1 d . . . H1 H 0.3509 0.5104 -0.3542 0.030 Uiso 1 1 calc R . . C2 C 0.2353(6) 0.4185(5) -0.4297(4) 0.0367(15) Uani 1 1 d . . . H2A H 0.3229 0.3425 -0.4186 0.055 Uiso 1 1 calc R . . H2B H 0.2677 0.4834 -0.5226 0.055 Uiso 1 1 calc R . . H2C H 0.1184 0.3893 -0.4121 0.055 Uiso 1 1 calc R . . C3 C 0.1009(6) 0.6025(4) -0.3446(5) 0.0404(15) Uani 1 1 d . . . H3A H -0.0197 0.5774 -0.3226 0.061 Uiso 1 1 calc R . . H3B H 0.1310 0.6670 -0.4379 0.061 Uiso 1 1 calc R . . H3C H 0.1081 0.6416 -0.2819 0.061 Uiso 1 1 calc R . . C4 C 0.0264(6) 0.3229(4) -0.1373(5) 0.0234(12) Uani 1 1 d . . . H4 H -0.0361 0.3657 -0.2118 0.028 Uiso 1 1 calc R . . C5 C 0.0467(6) 0.1758(4) -0.1105(5) 0.0377(15) Uani 1 1 d . . . H5A H 0.1332 0.1597 -0.1873 0.057 Uiso 1 1 calc R . . H5B H -0.0676 0.1463 -0.0992 0.057 Uiso 1 1 calc R . . H5C H 0.0878 0.1267 -0.0276 0.057 Uiso 1 1 calc R . . C6 C -0.0937(6) 0.3538(5) -0.0166(4) 0.0335(14) Uani 1 1 d . . . H6A H -0.0491 0.3022 0.0642 0.050 Uiso 1 1 calc R . . H6B H -0.2139 0.3310 -0.0005 0.050 Uiso 1 1 calc R . . H6C H -0.0955 0.4481 -0.0357 0.050 Uiso 1 1 calc R . . C7 C 0.3059(6) 0.3606(4) -0.1088(5) 0.0221(12) Uani 1 1 d . . . C8 C 0.3420(6) 0.2521(5) 0.1129(5) 0.0236(13) Uani 1 1 d . . . C9 C 0.4174(6) 0.1082(4) 0.3272(4) 0.0231(12) Uani 1 1 d . . . H9 H 0.4120 0.0117 0.3835 0.028 Uiso 1 1 calc R . . C10 C 0.6115(6) 0.1358(4) 0.2894(5) 0.0329(14) Uani 1 1 d . . . H10A H 0.6820 0.0910 0.2287 0.049 Uiso 1 1 calc R . . H10B H 0.6542 0.1030 0.3718 0.049 Uiso 1 1 calc R . . H10C H 0.6229 0.2310 0.2433 0.049 Uiso 1 1 calc R . . C11 C 0.3011(6) 0.1787(4) 0.4187(4) 0.0276(13) Uani 1 1 d . . . H11A H 0.3184 0.2732 0.3750 0.041 Uiso 1 1 calc R . . H11B H 0.3331 0.1427 0.5057 0.041 Uiso 1 1 calc R . . H11C H 0.1767 0.1654 0.4342 0.041 Uiso 1 1 calc R . . C12 C 0.2908(6) 0.0164(4) 0.2039(5) 0.0222(12) Uani 1 1 d . . . H12 H 0.2543 0.0480 0.1169 0.027 Uiso 1 1 calc R . . C13 C 0.4365(6) -0.0947(4) 0.2013(5) 0.0407(15) Uani 1 1 d . . . H13A H 0.5424 -0.0585 0.1309 0.061 Uiso 1 1 calc R . . H13B H 0.3956 -0.1609 0.1816 0.061 Uiso 1 1 calc R . . H13C H 0.4649 -0.1361 0.2898 0.061 Uiso 1 1 calc R . . C14 C 0.1290(6) -0.0334(4) 0.3182(4) 0.0364(15) Uani 1 1 d . . . H14A H 0.1611 -0.0691 0.4052 0.055 Uiso 1 1 calc R . . H14B H 0.0836 -0.1029 0.3066 0.055 Uiso 1 1 calc R . . H14C H 0.0377 0.0395 0.3168 0.055 Uiso 1 1 calc R . . Cu1 Cu 0.5000 0.5000 0.0000 0.0199(3) Uani 1 2 d S . . N1 N 0.1969(5) 0.3842(3) -0.1895(4) 0.0189(10) Uani 1 1 d . . . N2 N 0.2687(5) 0.2654(3) 0.0128(4) 0.0214(10) Uani 1 1 d . . . N3 N 0.3526(5) 0.1294(4) 0.2091(4) 0.0205(10) Uani 1 1 d . . . O1 O 0.3907(4) 0.3450(3) 0.1315(3) 0.0256(9) Uani 1 1 d . . . S1 S 0.49703(16) 0.44868(12) -0.17691(12) 0.0239(4) 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 C1 0.027(3) 0.033(3) 0.017(3) -0.005(3) -0.011(3) -0.005(3) C2 0.044(4) 0.043(4) 0.023(3) -0.012(3) -0.015(3) 0.005(3) C3 0.054(4) 0.025(3) 0.043(4) -0.008(3) -0.024(3) 0.003(3) C4 0.026(3) 0.023(3) 0.022(3) -0.003(3) -0.017(3) 0.001(2) C5 0.041(4) 0.032(3) 0.045(4) -0.007(3) -0.025(3) -0.005(3) C6 0.019(3) 0.045(4) 0.036(3) -0.011(3) -0.011(3) -0.004(3) C7 0.023(3) 0.012(3) 0.032(3) -0.007(2) -0.011(3) 0.001(2) C8 0.010(3) 0.025(3) 0.027(3) -0.005(3) -0.004(2) 0.003(2) C9 0.025(3) 0.019(3) 0.024(3) -0.004(2) -0.010(3) -0.002(2) C10 0.029(4) 0.030(3) 0.033(3) 0.000(3) -0.014(3) -0.005(3) C11 0.029(3) 0.027(3) 0.024(3) -0.006(3) -0.011(3) 0.003(2) C12 0.023(3) 0.019(3) 0.029(3) -0.009(2) -0.013(3) 0.000(2) C13 0.049(4) 0.021(3) 0.058(4) -0.020(3) -0.025(3) 0.013(3) C14 0.040(4) 0.037(3) 0.039(4) -0.013(3) -0.016(3) -0.010(3) Cu1 0.0190(6) 0.0161(6) 0.0252(6) -0.0052(5) -0.0112(5) 0.0007(5) N1 0.019(3) 0.019(2) 0.018(2) -0.0046(19) -0.007(2) -0.0013(19) N2 0.017(3) 0.023(3) 0.026(3) -0.008(2) -0.010(2) -0.0028(19) N3 0.021(3) 0.016(2) 0.025(3) -0.004(2) -0.012(2) -0.0001(19) O1 0.027(2) 0.015(2) 0.035(2) -0.0018(17) -0.0158(18) -0.0072(16) S1 0.0217(9) 0.0276(9) 0.0245(8) -0.0087(7) -0.0079(7) -0.0054(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 C1 N1 1.479(5) . ? C1 C2 1.502(5) . ? C1 C3 1.527(6) . ? C1 H1 1.0000 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 N1 1.481(5) . ? C4 C6 1.522(6) . ? C4 C5 1.525(5) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 N2 1.324(5) . ? C7 N1 1.349(5) . ? C7 S1 1.763(4) . ? C8 O1 1.280(5) . ? C8 N2 1.352(5) . ? C8 N3 1.357(5) . ? C9 N3 1.471(5) . ? C9 C11 1.522(6) . ? C9 C10 1.528(6) . ? C9 H9 1.0000 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N3 1.461(5) . ? C12 C14 1.514(6) . ? C12 C13 1.530(6) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? Cu1 O1 1.902(3) . ? Cu1 O1 1.902(3) 2_665 ? Cu1 S1 2.2717(13) 2_665 ? Cu1 S1 2.2717(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 112.2(4) . . ? N1 C1 C3 111.2(4) . . ? C2 C1 C3 113.0(4) . . ? N1 C1 H1 106.7 . . ? C2 C1 H1 106.7 . . ? C3 C1 H1 106.7 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C6 112.7(4) . . ? N1 C4 C5 113.6(4) . . ? C6 C4 C5 112.4(4) . . ? N1 C4 H4 105.8 . . ? C6 C4 H4 105.8 . . ? C5 C4 H4 105.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 N1 117.4(4) . . ? N2 C7 S1 124.4(3) . . ? N1 C7 S1 118.0(3) . . ? O1 C8 N2 126.5(4) . . ? O1 C8 N3 116.5(4) . . ? N2 C8 N3 116.8(4) . . ? N3 C9 C11 114.0(4) . . ? N3 C9 C10 113.1(4) . . ? C11 C9 C10 111.7(4) . . ? N3 C9 H9 105.8 . . ? C11 C9 H9 105.8 . . ? C10 C9 H9 105.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N3 C12 C14 111.4(4) . . ? N3 C12 C13 112.5(4) . . ? C14 C12 C13 111.3(4) . . ? N3 C12 H12 107.1 . . ? C14 C12 H12 107.1 . . ? C13 C12 H12 107.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 Cu1 O1 180.00(13) . 2_665 ? O1 Cu1 S1 86.90(10) . 2_665 ? O1 Cu1 S1 93.10(9) 2_665 2_665 ? O1 Cu1 S1 93.10(10) . . ? O1 Cu1 S1 86.90(9) 2_665 . ? S1 Cu1 S1 179.999(1) 2_665 . ? C7 N1 C1 123.1(4) . . ? C7 N1 C4 121.5(4) . . ? C1 N1 C4 115.2(3) . . ? C7 N2 C8 122.6(4) . . ? C8 N3 C12 121.7(4) . . ? C8 N3 C9 120.3(4) . . ? C12 N3 C9 117.9(4) . . ? C8 O1 Cu1 128.8(3) . . ? C7 S1 Cu1 101.14(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C7 N1 C1 -175.2(4) . . . . ? S1 C7 N1 C1 -0.3(6) . . . . ? N2 C7 N1 C4 10.2(7) . . . . ? S1 C7 N1 C4 -174.9(3) . . . . ? C2 C1 N1 C7 124.1(5) . . . . ? C3 C1 N1 C7 -108.4(5) . . . . ? C2 C1 N1 C4 -61.0(5) . . . . ? C3 C1 N1 C4 66.5(5) . . . . ? C6 C4 N1 C7 56.8(6) . . . . ? C5 C4 N1 C7 -72.5(6) . . . . ? C6 C4 N1 C1 -118.2(4) . . . . ? C5 C4 N1 C1 112.5(4) . . . . ? N1 C7 N2 C8 -164.8(4) . . . . ? S1 C7 N2 C8 20.7(7) . . . . ? O1 C8 N2 C7 30.8(7) . . . . ? N3 C8 N2 C7 -154.6(4) . . . . ? O1 C8 N3 C12 176.2(4) . . . . ? N2 C8 N3 C12 1.1(6) . . . . ? O1 C8 N3 C9 0.0(6) . . . . ? N2 C8 N3 C9 -175.1(4) . . . . ? C14 C12 N3 C8 -112.0(5) . . . . ? C13 C12 N3 C8 122.2(5) . . . . ? C14 C12 N3 C9 64.2(5) . . . . ? C13 C12 N3 C9 -61.5(5) . . . . ? C11 C9 N3 C8 63.6(5) . . . . ? C10 C9 N3 C8 -65.3(6) . . . . ? C11 C9 N3 C12 -112.8(4) . . . . ? C10 C9 N3 C12 118.3(4) . . . . ? N2 C8 O1 Cu1 -37.9(7) . . . . ? N3 C8 O1 Cu1 147.5(3) . . . . ? O1 Cu1 O1 C8 64(5) 2_665 . . . ? S1 Cu1 O1 C8 -179.2(4) 2_665 . . . ? S1 Cu1 O1 C8 0.8(4) . . . . ? N2 C7 S1 Cu1 -47.4(4) . . . . ? N1 C7 S1 Cu1 138.1(3) . . . . ? O1 Cu1 S1 C7 30.66(18) . . . . ? O1 Cu1 S1 C7 -149.34(18) 2_665 . . . ? S1 Cu1 S1 C7 151(27) 2_665 . . . ? _diffrn_measured_fraction_theta_max 0.887 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.445 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.071 # Attachment 's3096abs.cif' data_z:\s3096\work\s3096abs _database_code_depnum_ccdc_archive 'CCDC 715969' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H86 Fe2 N12 O6 S4' _chemical_formula_weight 1095.17 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' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.4666(18) _cell_length_b 25.355(4) _cell_length_c 10.3281(17) _cell_angle_alpha 90.00 _cell_angle_beta 95.442(3) _cell_angle_gamma 90.00 _cell_volume 2728.5(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 864 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.24 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.834 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15681 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5558 _reflns_number_gt 4890 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+4.1092P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5558 _refine_ls_number_parameters 309 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 Fe1 Fe 0.48506(4) 0.446249(15) 0.07326(4) 0.01467(12) Uani 1 1 d . . . S1 S 0.36796(7) 0.42143(3) 0.25548(7) 0.02009(17) Uani 1 1 d . . . S2 S 0.29935(7) 0.41930(3) -0.07433(7) 0.02026(17) Uani 1 1 d . . . O1 O 0.63814(19) 0.45646(8) 0.20099(18) 0.0202(4) Uani 1 1 d . . . O2 O 0.55224(19) 0.37401(8) 0.03666(19) 0.0200(4) Uani 1 1 d . . . O3 O 0.41546(17) 0.51923(7) 0.06037(18) 0.0150(4) Uani 1 1 d . . . N1 N 0.7986(2) 0.42798(11) 0.3441(2) 0.0240(6) Uani 1 1 d . . . N2 N 0.5986(2) 0.42812(10) 0.4105(2) 0.0213(5) Uani 1 1 d . . . N3 N 0.4163(2) 0.43039(10) 0.5103(2) 0.0217(5) Uani 1 1 d . . . N4 N 0.5728(2) 0.28843(10) -0.0117(2) 0.0198(5) Uani 1 1 d . . . N5 N 0.3711(2) 0.31939(9) 0.0042(2) 0.0201(5) Uani 1 1 d . . . N6 N 0.1585(2) 0.33805(10) -0.0117(2) 0.0221(5) Uani 1 1 d . . . C1 C 0.6721(3) 0.43750(11) 0.3141(3) 0.0199(6) Uani 1 1 d . . . C2 C 0.8497(3) 0.40831(13) 0.4719(3) 0.0275(7) Uani 1 1 d . . . H2A H 0.7949 0.4210 0.5384 0.033 Uiso 1 1 calc R . . H2B H 0.9371 0.4227 0.4935 0.033 Uiso 1 1 calc R . . C3 C 0.8552(3) 0.34850(13) 0.4759(3) 0.0316(8) Uani 1 1 d . . . H3A H 0.7686 0.3341 0.4560 0.047 Uiso 1 1 calc R . . H3B H 0.8896 0.3370 0.5629 0.047 Uiso 1 1 calc R . . H3C H 0.9110 0.3358 0.4115 0.047 Uiso 1 1 calc R . . C4 C 0.8904(3) 0.43401(13) 0.2463(3) 0.0258(7) Uani 1 1 d . . . H4A H 0.8445 0.4295 0.1587 0.031 Uiso 1 1 calc R . . H4B H 0.9558 0.4058 0.2588 0.031 Uiso 1 1 calc R . . C5 C 0.9575(3) 0.48688(14) 0.2523(4) 0.0366(8) Uani 1 1 d . . . H5A H 0.8940 0.5150 0.2339 0.055 Uiso 1 1 calc R . . H5B H 1.0201 0.4879 0.1877 0.055 Uiso 1 1 calc R . . H5C H 1.0017 0.4920 0.3394 0.055 Uiso 1 1 calc R . . C6 C 0.4716(3) 0.42837(11) 0.3981(3) 0.0191(6) Uani 1 1 d . . . C7 C 0.2773(3) 0.42725(14) 0.5183(3) 0.0299(7) Uani 1 1 d . . . H7A H 0.2328 0.4444 0.4406 0.036 Uiso 1 1 calc R . . H7B H 0.2556 0.4471 0.5958 0.036 Uiso 1 1 calc R . . C8 C 0.2282(3) 0.37130(16) 0.5269(4) 0.0399(9) Uani 1 1 d . . . H8A H 0.2528 0.3509 0.4526 0.060 Uiso 1 1 calc R . . H8B H 0.1344 0.3718 0.5256 0.060 Uiso 1 1 calc R . . H8C H 0.2654 0.3551 0.6079 0.060 Uiso 1 1 calc R . . C9 C 0.4966(3) 0.43338(12) 0.6356(3) 0.0236(7) Uani 1 1 d . . . H9A H 0.4453 0.4490 0.7017 0.028 Uiso 1 1 calc R . . H9B H 0.5701 0.4571 0.6258 0.028 Uiso 1 1 calc R . . C10 C 0.5470(3) 0.38036(13) 0.6836(3) 0.0286(7) Uani 1 1 d . . . H10A H 0.4749 0.3561 0.6894 0.043 Uiso 1 1 calc R . . H10B H 0.5940 0.3844 0.7696 0.043 Uiso 1 1 calc R . . H10C H 0.6046 0.3662 0.6227 0.043 Uiso 1 1 calc R . . C11 C 0.4967(3) 0.33009(11) 0.0093(3) 0.0183(6) Uani 1 1 d . . . C12 C 0.7113(3) 0.29483(13) -0.0066(3) 0.0243(7) Uani 1 1 d . . . H12A H 0.7312 0.3308 -0.0359 0.029 Uiso 1 1 calc R . . H12B H 0.7461 0.2694 -0.0670 0.029 Uiso 1 1 calc R . . C13 C 0.7759(3) 0.28607(16) 0.1294(3) 0.0379(9) Uani 1 1 d . . . H13A H 0.7445 0.3122 0.1887 0.057 Uiso 1 1 calc R . . H13B H 0.8690 0.2898 0.1285 0.057 Uiso 1 1 calc R . . H13C H 0.7559 0.2505 0.1589 0.057 Uiso 1 1 calc R . . C14 C 0.5201(3) 0.23615(11) -0.0416(3) 0.0229(6) Uani 1 1 d . . . H14A H 0.4429 0.2310 0.0055 0.027 Uiso 1 1 calc R . . H14B H 0.5841 0.2092 -0.0103 0.027 Uiso 1 1 calc R . . C15 C 0.4842(4) 0.22831(15) -0.1854(3) 0.0359(8) Uani 1 1 d . . . H15A H 0.4181 0.2539 -0.2161 0.054 Uiso 1 1 calc R . . H15B H 0.4511 0.1925 -0.2008 0.054 Uiso 1 1 calc R . . H15C H 0.5603 0.2334 -0.2325 0.054 Uiso 1 1 calc R . . C16 C 0.2794(3) 0.35479(12) -0.0213(3) 0.0204(6) Uani 1 1 d . . . C17 C 0.1342(3) 0.28394(13) 0.0282(3) 0.0294(7) Uani 1 1 d . . . H17A H 0.1982 0.2602 -0.0059 0.035 Uiso 1 1 calc R . . H17B H 0.0481 0.2729 -0.0101 0.035 Uiso 1 1 calc R . . C18 C 0.1412(3) 0.27838(16) 0.1741(4) 0.0401(9) Uani 1 1 d . . . H18A H 0.2274 0.2879 0.2122 0.060 Uiso 1 1 calc R . . H18B H 0.1227 0.2418 0.1966 0.060 Uiso 1 1 calc R . . H18C H 0.0779 0.3018 0.2083 0.060 Uiso 1 1 calc R . . C19 C 0.0448(3) 0.37181(13) -0.0357(3) 0.0249(7) Uani 1 1 d . . . H19A H 0.0698 0.4089 -0.0175 0.030 Uiso 1 1 calc R . . H19B H -0.0190 0.3618 0.0247 0.030 Uiso 1 1 calc R . . C20 C -0.0164(3) 0.36750(14) -0.1746(3) 0.0319(8) Uani 1 1 d . . . H20A H 0.0445 0.3797 -0.2346 0.048 Uiso 1 1 calc R . . H20B H -0.0938 0.3894 -0.1850 0.048 Uiso 1 1 calc R . . H20C H -0.0393 0.3307 -0.1938 0.048 Uiso 1 1 calc R . . C21 C 0.2898(3) 0.53469(12) 0.0854(3) 0.0211(6) Uani 1 1 d . . . H21A H 0.2267 0.5137 0.0314 0.032 Uiso 1 1 calc R . . H21B H 0.2775 0.5722 0.0646 0.032 Uiso 1 1 calc R . . H21C H 0.2786 0.5288 0.1774 0.032 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0180(2) 0.0148(2) 0.0116(2) 0.00028(15) 0.00333(15) 0.00091(16) S1 0.0198(4) 0.0257(4) 0.0149(3) 0.0018(3) 0.0025(3) -0.0014(3) S2 0.0207(4) 0.0202(4) 0.0194(4) 0.0007(3) -0.0008(3) -0.0011(3) O1 0.0205(10) 0.0247(11) 0.0150(10) 0.0010(8) -0.0002(8) 0.0011(8) O2 0.0219(11) 0.0172(10) 0.0212(10) -0.0021(8) 0.0046(8) -0.0006(8) O3 0.0145(10) 0.0174(10) 0.0135(9) -0.0003(7) 0.0039(7) 0.0015(8) N1 0.0220(13) 0.0323(15) 0.0175(12) 0.0028(11) 0.0019(10) -0.0011(11) N2 0.0256(13) 0.0258(13) 0.0124(11) -0.0001(10) 0.0014(10) -0.0001(11) N3 0.0237(13) 0.0247(13) 0.0170(12) -0.0021(10) 0.0037(10) 0.0004(11) N4 0.0194(13) 0.0198(13) 0.0199(12) -0.0003(10) 0.0009(10) -0.0016(10) N5 0.0228(13) 0.0186(12) 0.0190(12) -0.0004(10) 0.0021(10) 0.0000(10) N6 0.0197(13) 0.0215(13) 0.0254(13) -0.0001(11) 0.0033(10) 0.0011(10) C1 0.0234(15) 0.0179(14) 0.0185(14) -0.0011(11) 0.0029(12) -0.0001(12) C2 0.0224(16) 0.0372(19) 0.0222(16) 0.0011(14) -0.0011(12) -0.0015(14) C3 0.0289(17) 0.0368(19) 0.0279(17) 0.0083(14) -0.0042(14) -0.0034(15) C4 0.0219(16) 0.0340(18) 0.0215(15) 0.0022(13) 0.0028(12) 0.0042(13) C5 0.0266(18) 0.040(2) 0.045(2) 0.0068(17) 0.0082(16) -0.0006(15) C6 0.0234(15) 0.0191(14) 0.0146(13) -0.0005(11) 0.0006(11) 0.0021(12) C7 0.0250(17) 0.041(2) 0.0250(16) -0.0014(14) 0.0091(13) 0.0037(14) C8 0.0266(19) 0.050(2) 0.043(2) 0.0078(18) 0.0065(16) -0.0050(17) C9 0.0322(17) 0.0235(16) 0.0153(14) -0.0014(12) 0.0036(12) -0.0018(13) C10 0.041(2) 0.0260(17) 0.0181(15) -0.0002(13) -0.0006(14) -0.0036(14) C11 0.0273(16) 0.0178(14) 0.0101(12) 0.0006(11) 0.0026(11) -0.0018(12) C12 0.0205(15) 0.0267(16) 0.0260(16) -0.0010(13) 0.0041(12) 0.0009(13) C13 0.0236(17) 0.056(2) 0.0333(19) 0.0016(17) -0.0035(14) -0.0009(16) C14 0.0242(16) 0.0172(14) 0.0275(16) 0.0018(12) 0.0039(13) 0.0010(12) C15 0.039(2) 0.0345(19) 0.0345(19) -0.0128(15) 0.0065(16) -0.0115(16) C16 0.0270(16) 0.0209(15) 0.0133(13) -0.0022(11) 0.0020(11) 0.0010(12) C17 0.0223(16) 0.0243(16) 0.042(2) -0.0015(14) 0.0044(14) -0.0023(13) C18 0.0272(18) 0.048(2) 0.045(2) 0.0198(18) 0.0010(16) -0.0057(16) C19 0.0188(15) 0.0300(17) 0.0266(16) -0.0010(13) 0.0065(12) 0.0036(13) C20 0.0264(17) 0.039(2) 0.0303(18) 0.0003(15) 0.0028(14) 0.0033(15) C21 0.0184(15) 0.0244(15) 0.0211(14) -0.0009(12) 0.0051(12) 0.0004(12) _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 Fe1 O3 1.9886(19) . ? Fe1 O1 1.993(2) . ? Fe1 O3 2.0069(19) 3_665 ? Fe1 O2 2.011(2) . ? Fe1 S1 2.4242(8) . ? Fe1 S2 2.4508(9) . ? S1 C6 1.753(3) . ? S2 C16 1.744(3) . ? O1 C1 1.282(3) . ? O2 C11 1.275(3) . ? O3 C21 1.419(3) . ? O3 Fe1 2.0070(18) 3_665 ? N1 C1 1.353(4) . ? N1 C2 1.463(4) . ? N1 C4 1.468(4) . ? N2 C6 1.323(4) . ? N2 C1 1.336(4) . ? N3 C6 1.345(4) . ? N3 C7 1.467(4) . ? N3 C9 1.477(4) . ? N4 C11 1.353(4) . ? N4 C12 1.454(4) . ? N4 C14 1.458(4) . ? N5 C16 1.321(4) . ? N5 C11 1.339(4) . ? N6 C16 1.348(4) . ? N6 C17 1.462(4) . ? N6 C19 1.467(4) . ? C2 C3 1.518(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.512(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C7 C8 1.515(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.510(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C12 C13 1.517(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.510(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 C18 1.508(5) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.518(4) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? 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 O3 Fe1 O1 100.94(8) . . ? O3 Fe1 O3 76.04(8) . 3_665 ? O1 Fe1 O3 87.80(8) . 3_665 ? O3 Fe1 O2 165.37(8) . . ? O1 Fe1 O2 88.24(8) . . ? O3 Fe1 O2 93.12(8) 3_665 . ? O3 Fe1 S1 94.85(6) . . ? O1 Fe1 S1 87.35(6) . . ? O3 Fe1 S1 168.67(6) 3_665 . ? O2 Fe1 S1 96.95(6) . . ? O3 Fe1 S2 87.36(6) . . ? O1 Fe1 S2 171.15(6) . . ? O3 Fe1 S2 97.26(6) 3_665 . ? O2 Fe1 S2 84.26(6) . . ? S1 Fe1 S2 88.91(3) . . ? C6 S1 Fe1 107.93(10) . . ? C16 S2 Fe1 100.22(10) . . ? C1 O1 Fe1 133.64(19) . . ? C11 O2 Fe1 132.62(19) . . ? C21 O3 Fe1 125.78(17) . . ? C21 O3 Fe1 123.70(17) . 3_665 ? Fe1 O3 Fe1 103.96(8) . 3_665 ? C1 N1 C2 122.3(2) . . ? C1 N1 C4 121.0(2) . . ? C2 N1 C4 116.7(2) . . ? C6 N2 C1 124.8(3) . . ? C6 N3 C7 123.8(3) . . ? C6 N3 C9 120.1(3) . . ? C7 N3 C9 116.0(2) . . ? C11 N4 C12 120.5(3) . . ? C11 N4 C14 121.8(2) . . ? C12 N4 C14 117.7(2) . . ? C16 N5 C11 124.2(3) . . ? C16 N6 C17 120.4(3) . . ? C16 N6 C19 123.8(3) . . ? C17 N6 C19 115.8(2) . . ? O1 C1 N2 128.1(3) . . ? O1 C1 N1 117.2(3) . . ? N2 C1 N1 114.7(3) . . ? N1 C2 C3 112.0(3) . . ? N1 C2 H2A 109.2 . . ? C3 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C3 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 113.3(3) . . ? N1 C4 H4A 108.9 . . ? C5 C4 H4A 108.9 . . ? N1 C4 H4B 108.9 . . ? C5 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 N3 115.3(3) . . ? N2 C6 S1 128.1(2) . . ? N3 C6 S1 116.4(2) . . ? N3 C7 C8 113.5(3) . . ? N3 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? N3 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N3 C9 C10 113.2(2) . . ? N3 C9 H9A 108.9 . . ? C10 C9 H9A 108.9 . . ? N3 C9 H9B 108.9 . . ? C10 C9 H9B 108.9 . . ? H9A C9 H9B 107.8 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 N5 127.6(3) . . ? O2 C11 N4 117.0(3) . . ? N5 C11 N4 115.3(3) . . ? N4 C12 C13 111.9(3) . . ? N4 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N4 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 C15 112.4(3) . . ? N4 C14 H14A 109.1 . . ? C15 C14 H14A 109.1 . . ? N4 C14 H14B 109.1 . . ? C15 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N5 C16 N6 116.1(3) . . ? N5 C16 S2 126.4(2) . . ? N6 C16 S2 117.3(2) . . ? N6 C17 C18 112.1(3) . . ? N6 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? N6 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N6 C19 C20 112.4(3) . . ? N6 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? N6 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O3 C21 H21A 109.5 . . ? O3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Fe1 S1 C6 -97.91(12) . . . . ? O1 Fe1 S1 C6 2.85(12) . . . . ? O3 Fe1 S1 C6 -61.9(3) 3_665 . . . ? O2 Fe1 S1 C6 90.75(12) . . . . ? S2 Fe1 S1 C6 174.83(10) . . . . ? O3 Fe1 S2 C16 -149.63(11) . . . . ? O1 Fe1 S2 C16 10.3(4) . . . . ? O3 Fe1 S2 C16 134.81(11) 3_665 . . . ? O2 Fe1 S2 C16 42.38(11) . . . . ? S1 Fe1 S2 C16 -54.72(10) . . . . ? O3 Fe1 O1 C1 119.2(3) . . . . ? O3 Fe1 O1 C1 -165.4(3) 3_665 . . . ? O2 Fe1 O1 C1 -72.2(3) . . . . ? S1 Fe1 O1 C1 24.8(3) . . . . ? S2 Fe1 O1 C1 -40.3(6) . . . . ? O3 Fe1 O2 C11 -85.8(4) . . . . ? O1 Fe1 O2 C11 144.9(2) . . . . ? O3 Fe1 O2 C11 -127.4(2) 3_665 . . . ? S1 Fe1 O2 C11 57.8(2) . . . . ? S2 Fe1 O2 C11 -30.4(2) . . . . ? O1 Fe1 O3 C21 -123.0(2) . . . . ? O3 Fe1 O3 C21 152.1(2) 3_665 . . . ? O2 Fe1 O3 C21 109.0(3) . . . . ? S1 Fe1 O3 C21 -34.7(2) . . . . ? S2 Fe1 O3 C21 54.0(2) . . . . ? O1 Fe1 O3 Fe1 84.93(9) . . . 3_665 ? O3 Fe1 O3 Fe1 0.0 3_665 . . 3_665 ? O2 Fe1 O3 Fe1 -43.1(3) . . . 3_665 ? S1 Fe1 O3 Fe1 173.16(7) . . . 3_665 ? S2 Fe1 O3 Fe1 -98.16(7) . . . 3_665 ? Fe1 O1 C1 N2 -39.6(4) . . . . ? Fe1 O1 C1 N1 144.1(2) . . . . ? C6 N2 C1 O1 12.5(5) . . . . ? C6 N2 C1 N1 -171.1(3) . . . . ? C2 N1 C1 O1 177.6(3) . . . . ? C4 N1 C1 O1 -6.2(4) . . . . ? C2 N1 C1 N2 0.8(4) . . . . ? C4 N1 C1 N2 177.0(3) . . . . ? C1 N1 C2 C3 91.3(4) . . . . ? C4 N1 C2 C3 -85.1(3) . . . . ? C1 N1 C4 C5 96.4(3) . . . . ? C2 N1 C4 C5 -87.1(3) . . . . ? C1 N2 C6 N3 -165.0(3) . . . . ? C1 N2 C6 S1 20.2(4) . . . . ? C7 N3 C6 N2 -175.5(3) . . . . ? C9 N3 C6 N2 1.4(4) . . . . ? C7 N3 C6 S1 -0.1(4) . . . . ? C9 N3 C6 S1 176.8(2) . . . . ? Fe1 S1 C6 N2 -22.7(3) . . . . ? Fe1 S1 C6 N3 162.5(2) . . . . ? C6 N3 C7 C8 87.7(4) . . . . ? C9 N3 C7 C8 -89.3(3) . . . . ? C6 N3 C9 C10 -81.7(3) . . . . ? C7 N3 C9 C10 95.4(3) . . . . ? Fe1 O2 C11 N5 -4.1(4) . . . . ? Fe1 O2 C11 N4 179.10(18) . . . . ? C16 N5 C11 O2 26.7(4) . . . . ? C16 N5 C11 N4 -156.5(3) . . . . ? C12 N4 C11 O2 -1.8(4) . . . . ? C14 N4 C11 O2 179.0(2) . . . . ? C12 N4 C11 N5 -179.0(2) . . . . ? C14 N4 C11 N5 1.8(4) . . . . ? C11 N4 C12 C13 89.6(3) . . . . ? C14 N4 C12 C13 -91.1(3) . . . . ? C11 N4 C14 C15 87.4(3) . . . . ? C12 N4 C14 C15 -91.8(3) . . . . ? C11 N5 C16 N6 -174.6(3) . . . . ? C11 N5 C16 S2 9.2(4) . . . . ? C17 N6 C16 N5 1.6(4) . . . . ? C19 N6 C16 N5 179.7(3) . . . . ? C17 N6 C16 S2 178.1(2) . . . . ? C19 N6 C16 S2 -3.8(4) . . . . ? Fe1 S2 C16 N5 -45.3(3) . . . . ? Fe1 S2 C16 N6 138.6(2) . . . . ? C16 N6 C17 C18 86.8(3) . . . . ? C19 N6 C17 C18 -91.4(3) . . . . ? C16 N6 C19 C20 94.3(3) . . . . ? C17 N6 C19 C20 -87.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.677 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.084