# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dr Rong Cao' _publ_contact_author_email rcao@fjirsm.ac.cn _publ_section_title ; Systematic Investigation on the Coordination Chemistry of a Sulfonated Monoazo Dye: Ligand Dominated d- and f-Block Derivatives ; loop_ _publ_author_name 'Jian Lu' 'Shui-Ying Gao' 'Jing-Xiang Lin' 'Lin-Xi Shi' 'Rong Cao' 'Stuart R. Batten' # Attachment 'crystal.cif' data_compd1 _database_code_depnum_ccdc_archive 'CCDC 682495' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H30 N6 O10 S2' _chemical_formula_weight 626.66 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' _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 8.049(4) _cell_length_b 11.470(5) _cell_length_c 16.228(8) _cell_angle_alpha 85.964(15) _cell_angle_beta 84.380(14) _cell_angle_gamma 70.814(13) _cell_volume 1407.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6382 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.50 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.479 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11014 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6382 _reflns_number_gt 4390 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 6382 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1566 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.230 _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 S1 S 0.79863(8) 0.34195(5) 0.35624(3) 0.02732(19) Uani 1 1 d . . . S2 S 0.71205(8) 0.15686(5) 0.64022(3) 0.02745(19) Uani 1 1 d . . . C18 C 0.8357(4) 0.0091(2) 0.77657(14) 0.0348(6) Uani 1 1 d . . . H18A H 0.9133 -0.0444 0.7390 0.042 Uiso 1 1 calc R . . C2 C 0.7694(4) 0.2923(2) 0.19661(15) 0.0373(6) Uani 1 1 d . . . H2A H 0.7631 0.2166 0.2185 0.045 Uiso 1 1 calc R . . C8 C 0.6934(4) 0.4942(2) -0.16916(15) 0.0351(6) Uani 1 1 d . . . H8A H 0.6808 0.4212 -0.1451 0.042 Uiso 1 1 calc R . . C20 C 0.6709(4) 0.0027(2) 1.16963(15) 0.0362(6) Uani 1 1 d . . . H20A H 0.5914 0.0741 1.1478 0.043 Uiso 1 1 calc R . . C12 C 0.7373(4) 0.6894(2) -0.15614(15) 0.0390(6) Uani 1 1 d . . . H12A H 0.7521 0.7476 -0.1230 0.047 Uiso 1 1 calc R . . C14 C 0.5970(4) 0.2001(2) 0.80339(15) 0.0366(6) Uani 1 1 d . . . H14A H 0.5166 0.2729 0.7838 0.044 Uiso 1 1 calc R . . C6 C 0.8031(4) 0.4898(2) 0.21551(15) 0.0371(6) Uani 1 1 d . . . H6A H 0.8205 0.5451 0.2503 0.045 Uiso 1 1 calc R . . C24 C 0.9074(4) -0.1894(2) 1.14955(15) 0.0380(6) Uani 1 1 d . . . H24A H 0.9852 -0.2470 1.1144 0.046 Uiso 1 1 calc R . . C21 C 0.6690(3) -0.0195(2) 1.25414(15) 0.0356(6) Uani 1 1 d . . . H21A H 0.5884 0.0360 1.2896 0.043 Uiso 1 1 calc R . . C17 C 0.8371(4) -0.0197(2) 0.86057(14) 0.0362(6) Uani 1 1 d . . . H17A H 0.9170 -0.0927 0.8803 0.043 Uiso 1 1 calc R . . C9 C 0.6844(3) 0.5178(2) -0.25334(15) 0.0339(6) Uani 1 1 d . . . H9A H 0.6637 0.4616 -0.2862 0.041 Uiso 1 1 calc R . . C11 C 0.7312(4) 0.7129(2) -0.24102(15) 0.0370(6) Uani 1 1 d . . . H11A H 0.7438 0.7858 -0.2652 0.044 Uiso 1 1 calc R . . C3 C 0.7573(4) 0.3210(3) 0.11253(16) 0.0413(7) Uani 1 1 d . . . H3A H 0.7421 0.2650 0.0776 0.050 Uiso 1 1 calc R . . C15 C 0.5990(4) 0.1709(3) 0.88761(15) 0.0413(7) Uani 1 1 d . . . H15A H 0.5211 0.2243 0.9251 0.050 Uiso 1 1 calc R . . N3 N 0.7366(3) 0.5615(2) -0.03272(13) 0.0394(5) Uani 1 1 d . . . C5 C 0.7891(4) 0.5200(2) 0.13188(15) 0.0396(6) Uani 1 1 d . . . H5A H 0.7938 0.5962 0.1102 0.048 Uiso 1 1 calc R . . O3 O 0.9139(2) 0.40264(17) 0.38501(10) 0.0343(4) Uani 1 1 d . . . C23 C 0.9065(4) -0.2111(2) 1.23509(15) 0.0370(6) Uani 1 1 d . . . H23A H 0.9847 -0.2826 1.2576 0.044 Uiso 1 1 calc R . . O6 O 0.5959(2) 0.09753(16) 0.60982(10) 0.0333(4) Uani 1 1 d . . . N1 N 0.7015(3) 0.6465(2) -0.37858(13) 0.0302(5) Uani 1 1 d . . . N6 N 0.8027(3) -0.0646(2) 1.02821(13) 0.0388(5) Uani 1 1 d . . . O5 O 0.6409(3) 0.29093(17) 0.63179(11) 0.0410(5) Uani 1 1 d . . . N2 N 0.7528(3) 0.4556(2) -0.00686(13) 0.0414(6) Uani 1 1 d . . . O4 O 0.8921(2) 0.10747(19) 0.60525(11) 0.0412(5) Uani 1 1 d . . . O2 O 0.8688(3) 0.20851(17) 0.36508(11) 0.0391(5) Uani 1 1 d . . . C4 C 0.7680(4) 0.4346(2) 0.08082(15) 0.0346(6) Uani 1 1 d . . . N5 N 0.7095(3) 0.0403(2) 1.00371(13) 0.0416(6) Uani 1 1 d . . . C1 C 0.7910(3) 0.3765(2) 0.24763(14) 0.0278(5) Uani 1 1 d . . . N4 N 0.7903(3) -0.1453(2) 1.37612(13) 0.0300(5) Uani 1 1 d . . . C10 C 0.7063(3) 0.6262(2) -0.28893(14) 0.0275(5) Uani 1 1 d . . . C7 C 0.7213(3) 0.5799(2) -0.12034(14) 0.0315(5) Uani 1 1 d . . . O1 O 0.6191(2) 0.39232(18) 0.39137(11) 0.0391(5) Uani 1 1 d . . . C13 C 0.7146(3) 0.1208(2) 0.74883(14) 0.0285(5) Uani 1 1 d . . . C22 C 0.7893(3) -0.1261(2) 1.28567(14) 0.0292(5) Uani 1 1 d . . . C16 C 0.7188(4) 0.0607(2) 0.91548(15) 0.0342(6) Uani 1 1 d . . . C19 C 0.7907(3) -0.0808(2) 1.11686(14) 0.0325(6) Uani 1 1 d . . . O1W O 0.8006(4) 0.8500(2) -0.43904(14) 0.0428(5) Uani 1 1 d . . . O2W O 0.6113(3) 0.1000(2) 0.43192(13) 0.0425(5) Uani 1 1 d . . . O3W O 0.8929(3) 0.4048(2) 0.56521(14) 0.0422(5) Uani 1 1 d . . . O4W O 0.6975(3) -0.3493(2) 1.43226(15) 0.0470(5) Uani 1 1 d . . . H1C H 0.603(5) 0.106(3) 0.482(2) 0.050(10) Uiso 1 1 d . . . H1E H 0.907(5) 0.404(3) 0.516(2) 0.052(10) Uiso 1 1 d . . . H1H H 0.815(5) 0.380(3) 0.579(2) 0.036(9) Uiso 1 1 d . . . H1X H 0.771(6) -0.422(4) 1.424(3) 0.089(15) Uiso 1 1 d . . . H1A H 0.890(7) 0.847(4) -0.431(3) 0.088(17) Uiso 1 1 d . . . H1D H 0.691(5) 0.113(3) 0.413(2) 0.046(10) Uiso 1 1 d . . . H1Y H 0.601(6) -0.368(4) 1.424(3) 0.080(14) Uiso 1 1 d . . . H1B H 0.746(7) 0.917(5) -0.433(3) 0.097(18) Uiso 1 1 d . . . H4A H 0.727(3) 0.705(2) -0.3939(15) 0.014(6) Uiso 1 1 d . . . H4B H 0.767(4) 0.577(3) -0.4024(17) 0.029(7) Uiso 1 1 d . . . H4D H 0.731(4) -0.087(3) 1.3993(19) 0.037(9) Uiso 1 1 d . . . H4E H 0.752(4) -0.216(3) 1.3901(18) 0.040(8) Uiso 1 1 d . . . H4C H 0.580(4) 0.659(3) -0.3943(19) 0.043(8) Uiso 1 1 d . . . H4F H 0.906(5) -0.165(3) 1.392(2) 0.054(10) Uiso 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 S1 0.0269(3) 0.0318(3) 0.0249(3) -0.0003(2) -0.0026(2) -0.0118(3) S2 0.0301(3) 0.0320(3) 0.0238(3) -0.0001(2) -0.0028(2) -0.0149(3) C18 0.0371(14) 0.0347(14) 0.0290(12) -0.0036(10) 0.0010(10) -0.0072(11) C2 0.0509(16) 0.0295(13) 0.0354(13) 0.0015(10) -0.0079(12) -0.0174(12) C8 0.0440(15) 0.0334(14) 0.0309(12) 0.0039(10) -0.0037(11) -0.0176(12) C20 0.0402(15) 0.0367(14) 0.0302(12) 0.0019(10) -0.0025(11) -0.0112(12) C12 0.0517(17) 0.0397(15) 0.0337(13) -0.0054(11) -0.0056(12) -0.0243(13) C14 0.0398(15) 0.0363(14) 0.0306(12) 0.0011(10) -0.0055(11) -0.0078(11) C6 0.0503(16) 0.0356(14) 0.0320(12) -0.0010(11) -0.0089(11) -0.0213(12) C24 0.0416(15) 0.0362(14) 0.0329(12) -0.0041(11) 0.0011(11) -0.0087(12) C21 0.0344(14) 0.0377(14) 0.0334(12) -0.0016(11) -0.0006(10) -0.0104(11) C17 0.0450(16) 0.0327(14) 0.0285(12) 0.0021(10) -0.0024(11) -0.0102(12) C9 0.0395(14) 0.0362(14) 0.0320(12) -0.0040(10) -0.0029(10) -0.0197(11) C11 0.0453(16) 0.0348(14) 0.0348(13) 0.0009(11) -0.0030(11) -0.0189(12) C3 0.0604(19) 0.0366(15) 0.0311(13) -0.0045(11) -0.0088(12) -0.0195(13) C15 0.0460(17) 0.0385(15) 0.0315(12) -0.0030(11) 0.0028(11) -0.0042(12) N3 0.0504(14) 0.0434(14) 0.0265(10) 0.0012(9) -0.0059(10) -0.0177(11) C5 0.0553(18) 0.0333(14) 0.0355(13) 0.0026(11) -0.0076(12) -0.0211(13) O3 0.0330(10) 0.0429(11) 0.0313(9) -0.0021(7) -0.0037(7) -0.0179(8) C23 0.0383(14) 0.0336(14) 0.0371(13) -0.0015(11) -0.0017(11) -0.0094(11) O6 0.0335(10) 0.0408(10) 0.0303(8) -0.0040(7) -0.0030(7) -0.0179(8) N1 0.0295(12) 0.0368(13) 0.0266(10) 0.0033(9) -0.0044(8) -0.0142(10) N6 0.0500(14) 0.0412(13) 0.0245(10) 0.0011(9) -0.0036(9) -0.0142(11) O5 0.0574(13) 0.0309(10) 0.0381(10) 0.0031(8) -0.0090(9) -0.0181(9) N2 0.0564(16) 0.0402(13) 0.0272(11) 0.0014(9) -0.0042(10) -0.0156(11) O4 0.0308(10) 0.0617(13) 0.0357(9) -0.0042(9) 0.0025(8) -0.0221(9) O2 0.0482(12) 0.0347(10) 0.0353(9) 0.0080(8) -0.0093(8) -0.0148(9) C4 0.0408(15) 0.0372(14) 0.0266(12) -0.0016(10) -0.0019(10) -0.0139(11) N5 0.0525(15) 0.0429(13) 0.0271(11) 0.0008(9) -0.0026(10) -0.0129(11) C1 0.0289(12) 0.0296(13) 0.0253(11) -0.0013(9) -0.0026(9) -0.0097(10) N4 0.0297(12) 0.0370(13) 0.0250(10) 0.0007(9) -0.0049(9) -0.0125(10) C10 0.0252(12) 0.0349(13) 0.0241(11) 0.0006(9) -0.0025(9) -0.0120(10) C7 0.0354(14) 0.0314(13) 0.0267(11) 0.0014(10) -0.0048(10) -0.0096(11) O1 0.0275(10) 0.0518(12) 0.0388(10) -0.0049(9) 0.0008(8) -0.0145(9) C13 0.0334(13) 0.0320(13) 0.0239(11) -0.0003(9) -0.0036(9) -0.0153(10) C22 0.0292(12) 0.0375(14) 0.0253(11) 0.0012(10) -0.0027(9) -0.0170(11) C16 0.0426(15) 0.0333(14) 0.0280(12) -0.0035(10) -0.0015(11) -0.0139(11) C19 0.0348(14) 0.0384(14) 0.0271(12) 0.0003(10) -0.0038(10) -0.0154(11) O1W 0.0416(13) 0.0357(12) 0.0528(12) 0.0029(9) -0.0114(10) -0.0137(10) O2W 0.0501(14) 0.0550(13) 0.0299(10) -0.0026(9) -0.0027(10) -0.0272(11) O3W 0.0467(13) 0.0489(12) 0.0368(11) -0.0045(9) -0.0007(9) -0.0236(10) O4W 0.0458(13) 0.0319(11) 0.0648(14) 0.0011(10) -0.0108(11) -0.0135(10) _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 S1 O1 1.443(2) . ? S1 O2 1.449(2) . ? S1 O3 1.4552(18) . ? S1 C1 1.782(2) . ? S2 O4 1.445(2) . ? S2 O5 1.455(2) . ? S2 O6 1.4617(18) . ? S2 C13 1.782(2) . ? C18 C17 1.380(3) . ? C18 C13 1.406(3) . ? C2 C1 1.378(3) . ? C2 C3 1.386(3) . ? C8 C9 1.378(3) . ? C8 C7 1.391(3) . ? C20 C21 1.377(3) . ? C20 C19 1.388(4) . ? C12 C7 1.386(4) . ? C12 C11 1.387(3) . ? C14 C13 1.375(3) . ? C14 C15 1.384(3) . ? C6 C5 1.383(3) . ? C6 C1 1.396(3) . ? C24 C23 1.393(3) . ? C24 C19 1.397(4) . ? C21 C22 1.387(3) . ? C17 C16 1.387(4) . ? C9 C10 1.390(3) . ? C11 C10 1.380(3) . ? C3 C4 1.393(4) . ? C15 C16 1.391(4) . ? N3 N2 1.226(3) . ? N3 C7 1.434(3) . ? C5 C4 1.388(4) . ? C23 C22 1.368(3) . ? N1 C10 1.459(3) . ? N6 N5 1.251(3) . ? N6 C19 1.435(3) . ? N2 C4 1.437(3) . ? N5 C16 1.433(3) . ? N4 C22 1.469(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 S1 O2 113.35(12) . . ? O1 S1 O3 112.20(11) . . ? O2 S1 O3 112.79(11) . . ? O1 S1 C1 105.72(11) . . ? O2 S1 C1 105.61(11) . . ? O3 S1 C1 106.43(11) . . ? O4 S2 O5 113.17(12) . . ? O4 S2 O6 112.59(11) . . ? O5 S2 O6 111.95(11) . . ? O4 S2 C13 106.72(12) . . ? O5 S2 C13 105.77(11) . . ? O6 S2 C13 105.98(11) . . ? C17 C18 C13 118.8(2) . . ? C1 C2 C3 119.7(2) . . ? C9 C8 C7 119.7(2) . . ? C21 C20 C19 120.4(2) . . ? C7 C12 C11 120.5(2) . . ? C13 C14 C15 119.6(2) . . ? C5 C6 C1 120.0(2) . . ? C23 C24 C19 119.6(2) . . ? C20 C21 C22 119.0(2) . . ? C18 C17 C16 119.7(2) . . ? C8 C9 C10 119.7(2) . . ? C10 C11 C12 118.8(2) . . ? C2 C3 C4 119.3(2) . . ? C14 C15 C16 119.3(2) . . ? N2 N3 C7 113.7(2) . . ? C6 C5 C4 118.9(2) . . ? C22 C23 C24 119.2(2) . . ? N5 N6 C19 112.6(2) . . ? N3 N2 C4 114.9(2) . . ? C5 C4 C3 121.3(2) . . ? C5 C4 N2 123.7(2) . . ? C3 C4 N2 115.0(2) . . ? N6 N5 C16 114.4(2) . . ? C2 C1 C6 120.8(2) . . ? C2 C1 S1 119.67(19) . . ? C6 C1 S1 119.52(18) . . ? C11 C10 C9 121.1(2) . . ? C11 C10 N1 120.6(2) . . ? C9 C10 N1 118.3(2) . . ? C12 C7 C8 120.0(2) . . ? C12 C7 N3 116.5(2) . . ? C8 C7 N3 123.4(2) . . ? C14 C13 C18 121.4(2) . . ? C14 C13 S2 120.00(19) . . ? C18 C13 S2 118.60(18) . . ? C23 C22 C21 121.8(2) . . ? C23 C22 N4 120.1(2) . . ? C21 C22 N4 118.1(2) . . ? C17 C16 C15 121.3(2) . . ? C17 C16 N5 124.3(2) . . ? C15 C16 N5 114.4(2) . . ? C20 C19 C24 119.8(2) . . ? C20 C19 N6 124.1(2) . . ? C24 C19 N6 116.1(2) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.464 _refine_diff_density_min -0.424 _refine_diff_density_rms 0.074 #===end data_compd2 _database_code_depnum_ccdc_archive 'CCDC 682496' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 N6 Na O8 S2' _chemical_formula_weight 612.61 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' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 33.554(15) _cell_length_b 11.965(4) _cell_length_c 14.577(5) _cell_angle_alpha 90.00 _cell_angle_beta 115.300(4) _cell_angle_gamma 90.00 _cell_volume 5291(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5966 _cell_measurement_theta_min 3.34 _cell_measurement_theta_max 27.49 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2544 _exptl_absorpt_coefficient_mu 0.280 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.935 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 19967 _diffrn_reflns_av_R_equivalents 0.0308 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5966 _reflns_number_gt 5126 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 5966 _refine_ls_number_parameters 470 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1428 _refine_ls_wR_factor_gt 0.1350 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.188446(13) 0.72746(3) 0.00094(3) 0.02509(14) Uani 1 1 d . . . S2 S 0.683380(13) 0.28657(3) 0.53387(3) 0.02608(14) Uani 1 1 d . . . O6 O 0.69433(4) 0.28569(10) 0.44805(11) 0.0347(3) Uani 1 1 d . . . O3 O 0.19005(4) 0.84901(10) 0.00182(10) 0.0335(3) Uani 1 1 d . . . O2 O 0.21454(4) 0.67952(11) 0.10030(10) 0.0366(3) Uani 1 1 d . . . O1 O 0.19883(4) 0.68028(10) -0.07857(10) 0.0340(3) Uani 1 1 d . . . C13 C 0.62704(5) 0.32351(13) 0.48588(13) 0.0251(3) Uani 1 1 d . . . N6 N 0.49297(5) 0.40346(12) 0.36943(13) 0.0362(4) Uani 1 1 d . . . O5 O 0.70778(4) 0.37165(10) 0.60840(10) 0.0351(3) Uani 1 1 d . . . C22 C 0.35016(5) 0.58485(14) 0.24471(13) 0.0281(4) Uani 1 1 d . . . O4 O 0.68698(4) 0.17646(10) 0.57842(12) 0.0440(4) Uani 1 1 d . . . C2 C 0.10786(6) 0.75651(14) 0.00318(17) 0.0351(4) Uani 1 1 d . . . C8 C -0.08244(6) 0.54536(15) -0.13500(15) 0.0347(4) Uani 1 1 d . . . C18 C 0.59562(6) 0.24117(14) 0.46646(16) 0.0325(4) Uani 1 1 d . . . C7 C -0.05352(5) 0.48025(13) -0.15795(14) 0.0280(3) Uani 1 1 d . . . N1 N -0.18753(5) 0.39708(14) -0.27431(15) 0.0384(4) Uani 1 1 d . . . C16 C 0.53929(5) 0.38144(14) 0.40822(14) 0.0309(4) Uani 1 1 d . . . C11 C -0.11313(6) 0.35533(14) -0.25341(15) 0.0311(4) Uani 1 1 d . . . N5 N 0.48356(5) 0.50416(13) 0.36129(14) 0.0376(4) Uani 1 1 d . . . N4 N 0.30345(5) 0.61580(14) 0.20326(13) 0.0313(3) Uani 1 1 d . . . N2 N -0.00874(5) 0.50683(12) -0.13028(12) 0.0320(3) Uani 1 1 d . . . N3 N 0.00258(5) 0.60324(12) -0.09496(13) 0.0335(3) Uani 1 1 d . . . C1 C 0.13308(5) 0.69038(13) -0.02946(13) 0.0260(3) Uani 1 1 d . . . C15 C 0.57081(6) 0.46316(14) 0.42536(17) 0.0376(4) Uani 1 1 d . . . C6 C 0.11601(6) 0.59257(15) -0.08231(16) 0.0372(4) Uani 1 1 d . . . C24 C 0.40548(6) 0.44420(15) 0.30216(16) 0.0379(4) Uani 1 1 d . . . C19 C 0.43746(6) 0.52642(14) 0.32229(15) 0.0323(4) Uani 1 1 d . . . C10 C -0.14219(5) 0.42103(14) -0.23221(14) 0.0293(4) Uani 1 1 d . . . C5 C 0.07332(6) 0.56163(15) -0.10338(16) 0.0373(4) Uani 1 1 d . . . C12 C -0.06884(6) 0.38377(13) -0.21525(15) 0.0310(4) Uani 1 1 d . . . C14 C 0.61489(6) 0.43495(14) 0.46419(16) 0.0359(4) Uani 1 1 d . . . C17 C 0.55144(6) 0.27040(15) 0.42748(17) 0.0361(4) Uani 1 1 d . . . C23 C 0.36163(6) 0.47393(15) 0.26314(17) 0.0370(4) Uani 1 1 d . . . C4 C 0.04749(5) 0.62859(13) -0.07268(14) 0.0288(4) Uani 1 1 d . . . C3 C 0.06471(6) 0.72644(14) -0.01950(17) 0.0375(5) Uani 1 1 d . . . C20 C 0.42548(6) 0.63755(15) 0.30460(18) 0.0416(5) Uani 1 1 d . . . C9 C -0.12617(6) 0.51555(15) -0.17044(16) 0.0355(4) Uani 1 1 d . . . C21 C 0.38124(6) 0.66716(15) 0.26452(17) 0.0392(4) Uani 1 1 d . . . Na2 Na 0.25390(2) 0.96306(6) 0.09801(6) 0.03406(19) Uani 1 1 d . . . O1W O 0.74623(5) 0.45867(11) 0.44401(11) 0.0364(3) Uani 1 1 d . . . O2W O 0.24350(8) 0.87622(17) 0.23034(14) 0.0604(5) Uani 1 1 d . . . H11A H -0.1242(7) 0.2884(16) -0.2960(17) 0.033(5) Uiso 1 1 d . . . H18A H 0.6042(7) 0.1655(18) 0.4799(17) 0.041(6) Uiso 1 1 d . . . H12A H -0.0497(7) 0.3394(17) -0.2344(17) 0.041(5) Uiso 1 1 d . . . H1C H 0.2949(7) 0.6222(17) 0.2556(19) 0.043(6) Uiso 1 1 d . . . H3A H 0.0490(9) 0.7685(19) 0.006(2) 0.057(7) Uiso 1 1 d . . . H17A H 0.5288(9) 0.216(2) 0.413(2) 0.064(8) Uiso 1 1 d . . . H6A H 0.1320(8) 0.5464(18) -0.1101(19) 0.053(6) Uiso 1 1 d . . . H14A H 0.6370(9) 0.492(2) 0.483(2) 0.063(7) Uiso 1 1 d . . . H20A H 0.4456(8) 0.6975(18) 0.3189(19) 0.049(6) Uiso 1 1 d . . . H9A H -0.1457(8) 0.5617(19) -0.1538(19) 0.055(7) Uiso 1 1 d . . . H24A H 0.4135(7) 0.3697(18) 0.3164(17) 0.043(6) Uiso 1 1 d . . . H8A H -0.0726(6) 0.6103(16) -0.0965(16) 0.031(5) Uiso 1 1 d . . . H23A H 0.3397(8) 0.4221(19) 0.2501(19) 0.054(7) Uiso 1 1 d . . . H15A H 0.5619(8) 0.5386(19) 0.409(2) 0.056(7) Uiso 1 1 d . . . H1A H -0.1964(8) 0.399(2) -0.226(2) 0.055(7) Uiso 1 1 d . . . H2A H 0.1204(7) 0.8233(18) 0.0437(18) 0.045(6) Uiso 1 1 d . . . H21A H 0.3732(8) 0.7438(18) 0.247(2) 0.049(6) Uiso 1 1 d . . . H1E H 0.7309(8) 0.399(2) 0.4371(17) 0.043(6) Uiso 1 1 d . . . H5A H 0.0594(9) 0.496(2) -0.146(2) 0.063(7) Uiso 1 1 d . . . H1G H -0.1940(8) 0.334(2) -0.311(2) 0.046(6) Uiso 1 1 d . . . H1D H 0.7691(9) 0.433(2) 0.445(2) 0.055(7) Uiso 1 1 d . . . H1I H 0.2673(9) 0.849(2) 0.261(2) 0.051(8) Uiso 1 1 d . . . H1F H 0.2842(9) 0.563(2) 0.155(2) 0.073(8) Uiso 1 1 d . . . H1X H 0.2998(8) 0.680(2) 0.172(2) 0.045(6) Uiso 1 1 d . . . H1H H 0.2348(13) 0.807(3) 0.207(3) 0.098(12) Uiso 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 S1 0.0164(2) 0.0277(2) 0.0310(3) -0.00026(15) 0.00998(18) 0.00022(14) S2 0.0161(2) 0.0283(2) 0.0316(3) 0.00200(15) 0.00809(18) 0.00002(14) O6 0.0264(6) 0.0422(7) 0.0383(8) -0.0083(5) 0.0164(6) -0.0048(5) O3 0.0231(6) 0.0282(6) 0.0467(8) -0.0020(5) 0.0124(6) -0.0024(5) O2 0.0238(6) 0.0456(7) 0.0367(8) 0.0070(6) 0.0094(6) 0.0036(5) O1 0.0268(6) 0.0402(6) 0.0395(8) -0.0029(6) 0.0186(6) 0.0012(5) C13 0.0176(7) 0.0308(8) 0.0263(9) 0.0000(6) 0.0088(6) 0.0011(6) N6 0.0192(7) 0.0364(8) 0.0479(10) 0.0021(7) 0.0095(7) 0.0044(6) O5 0.0235(6) 0.0465(7) 0.0324(7) -0.0073(6) 0.0090(5) -0.0054(5) C22 0.0187(7) 0.0368(8) 0.0263(9) 0.0005(7) 0.0073(7) 0.0056(6) O4 0.0255(6) 0.0379(7) 0.0636(10) 0.0197(7) 0.0143(7) 0.0049(6) C2 0.0247(9) 0.0282(8) 0.0534(12) -0.0114(8) 0.0177(9) -0.0047(7) C8 0.0273(9) 0.0367(9) 0.0393(11) -0.0088(8) 0.0134(8) -0.0046(7) C18 0.0223(8) 0.0273(8) 0.0448(11) 0.0045(7) 0.0114(8) 0.0012(7) C7 0.0213(8) 0.0322(8) 0.0294(9) 0.0006(7) 0.0097(7) -0.0027(6) N1 0.0233(8) 0.0441(9) 0.0445(10) -0.0002(8) 0.0113(7) -0.0080(7) C16 0.0179(8) 0.0353(8) 0.0357(10) 0.0014(7) 0.0079(7) 0.0036(7) C11 0.0267(8) 0.0291(8) 0.0335(10) -0.0009(7) 0.0090(7) -0.0039(7) N5 0.0198(7) 0.0383(8) 0.0494(10) 0.0017(7) 0.0097(7) 0.0036(6) N4 0.0211(7) 0.0395(8) 0.0307(9) 0.0011(7) 0.0087(6) 0.0069(6) N2 0.0232(7) 0.0353(7) 0.0364(9) -0.0014(6) 0.0116(7) -0.0039(6) N3 0.0219(7) 0.0340(7) 0.0439(10) -0.0038(7) 0.0134(7) -0.0048(6) C1 0.0195(7) 0.0288(7) 0.0298(9) 0.0015(6) 0.0108(7) 0.0005(6) C15 0.0256(9) 0.0274(8) 0.0541(13) 0.0023(8) 0.0116(9) 0.0042(7) C6 0.0310(9) 0.0382(9) 0.0491(12) -0.0147(8) 0.0234(9) -0.0062(7) C24 0.0251(9) 0.0312(8) 0.0514(13) 0.0026(8) 0.0106(9) 0.0042(7) C19 0.0215(8) 0.0349(8) 0.0368(10) 0.0013(7) 0.0090(7) 0.0036(7) C10 0.0230(8) 0.0320(8) 0.0300(9) 0.0052(7) 0.0086(7) -0.0029(6) C5 0.0302(9) 0.0391(9) 0.0467(12) -0.0164(9) 0.0203(9) -0.0100(8) C12 0.0255(8) 0.0287(8) 0.0386(10) 0.0003(7) 0.0135(8) 0.0013(7) C14 0.0216(8) 0.0288(8) 0.0532(12) 0.0008(8) 0.0120(8) -0.0028(7) C17 0.0208(8) 0.0331(9) 0.0493(13) 0.0020(8) 0.0100(8) -0.0043(7) C23 0.0227(8) 0.0350(9) 0.0478(12) 0.0031(8) 0.0098(8) -0.0008(7) C4 0.0214(7) 0.0319(8) 0.0333(10) -0.0001(7) 0.0119(7) -0.0015(6) C3 0.0251(9) 0.0337(9) 0.0585(14) -0.0101(8) 0.0223(10) -0.0004(7) C20 0.0242(9) 0.0330(9) 0.0582(14) -0.0009(9) 0.0088(9) -0.0022(7) C9 0.0247(8) 0.0395(9) 0.0440(11) -0.0072(8) 0.0163(8) -0.0009(7) C21 0.0274(9) 0.0298(8) 0.0532(13) 0.0016(8) 0.0103(9) 0.0066(7) Na2 0.0310(4) 0.0352(4) 0.0345(4) -0.0003(3) 0.0126(3) 0.0000(3) O1W 0.0355(7) 0.0357(7) 0.0431(8) -0.0010(6) 0.0217(7) -0.0012(6) O2W 0.0730(13) 0.0651(12) 0.0347(10) 0.0015(8) 0.0149(9) -0.0067(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O2 1.4525(14) . ? S1 O3 1.4552(13) . ? S1 O1 1.4590(13) . ? S1 C1 1.7722(18) . ? S2 O6 1.4468(15) . ? S2 O4 1.4508(13) . ? S2 O5 1.4583(13) . ? S2 C13 1.7687(17) . ? O3 Na2 2.4186(15) . ? O1 Na2 2.4334(14) 7_565 ? C13 C18 1.381(2) . ? C13 C14 1.391(2) . ? N6 N5 1.238(2) . ? N6 C16 1.433(2) . ? O5 Na2 2.5552(15) 8_566 ? C22 C21 1.372(3) . ? C22 C23 1.376(2) . ? C22 N4 1.466(2) . ? C2 C1 1.383(2) . ? C2 C3 1.388(2) . ? C8 C9 1.378(2) . ? C8 C7 1.392(2) . ? C18 C17 1.387(2) . ? C7 C12 1.388(2) . ? C7 N2 1.415(2) . ? N1 C10 1.405(2) . ? N1 Na2 2.6460(19) 8_465 ? C16 C15 1.383(2) . ? C16 C17 1.383(2) . ? C11 C12 1.388(2) . ? C11 C10 1.386(2) . ? N5 C19 1.427(2) . ? N2 N3 1.254(2) . ? N3 C4 1.432(2) . ? C1 C6 1.383(2) . ? C15 C14 1.381(2) . ? C6 C5 1.381(3) . ? C24 C23 1.378(3) . ? C24 C19 1.391(2) . ? C19 C20 1.381(2) . ? C10 C9 1.402(3) . ? C5 C4 1.388(2) . ? C4 C3 1.387(2) . ? C20 C21 1.389(3) . ? Na2 O1W 2.3428(17) 8_465 ? Na2 O2W 2.345(2) . ? Na2 O1 2.4334(14) 7_565 ? Na2 O5 2.5552(15) 8_465 ? Na2 N1 2.6460(19) 8_566 ? O1W Na2 2.3428(17) 8_566 ? 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 O2 S1 O3 112.43(8) . . ? O2 S1 O1 113.11(8) . . ? O3 S1 O1 111.91(7) . . ? O2 S1 C1 105.74(8) . . ? O3 S1 C1 106.46(7) . . ? O1 S1 C1 106.57(8) . . ? O6 S2 O4 112.15(8) . . ? O6 S2 O5 112.34(8) . . ? O4 S2 O5 112.81(9) . . ? O6 S2 C13 106.46(8) . . ? O4 S2 C13 105.93(8) . . ? O5 S2 C13 106.57(7) . . ? S1 O3 Na2 126.11(7) . . ? S1 O1 Na2 138.94(8) . 7_565 ? C18 C13 C14 120.90(15) . . ? C18 C13 S2 119.74(13) . . ? C14 C13 S2 119.30(12) . . ? N5 N6 C16 113.93(14) . . ? S2 O5 Na2 131.12(8) . 8_566 ? C21 C22 C23 121.81(16) . . ? C21 C22 N4 119.20(15) . . ? C23 C22 N4 118.99(15) . . ? C1 C2 C3 119.94(16) . . ? C9 C8 C7 120.32(17) . . ? C13 C18 C17 119.52(16) . . ? C12 C7 C8 119.55(15) . . ? C12 C7 N2 115.67(14) . . ? C8 C7 N2 124.74(15) . . ? C10 N1 Na2 121.22(11) . 8_465 ? C15 C16 C17 120.42(16) . . ? C15 C16 N6 123.94(15) . . ? C17 C16 N6 115.64(15) . . ? C12 C11 C10 120.40(16) . . ? N6 N5 C19 114.10(15) . . ? N3 N2 C7 114.96(14) . . ? N2 N3 C4 113.13(14) . . ? C2 C1 C6 120.47(15) . . ? C2 C1 S1 120.06(13) . . ? C6 C1 S1 119.42(12) . . ? C14 C15 C16 120.26(16) . . ? C5 C6 C1 119.59(16) . . ? C23 C24 C19 119.71(17) . . ? C20 C19 C24 120.30(16) . . ? C20 C19 N5 115.70(15) . . ? C24 C19 N5 124.00(15) . . ? C11 C10 C9 119.18(15) . . ? C11 C10 N1 121.35(17) . . ? C9 C10 N1 119.43(16) . . ? C6 C5 C4 120.34(17) . . ? C11 C12 C7 120.17(16) . . ? C15 C14 C13 119.09(16) . . ? C16 C17 C18 119.76(16) . . ? C22 C23 C24 119.32(17) . . ? C5 C4 C3 119.96(15) . . ? C5 C4 N3 123.13(15) . . ? C3 C4 N3 116.90(14) . . ? C2 C3 C4 119.68(16) . . ? C19 C20 C21 119.84(17) . . ? C8 C9 C10 120.28(16) . . ? C22 C21 C20 119.01(17) . . ? O1W Na2 O2W 166.27(8) 8_465 . ? O1W Na2 O3 87.86(6) 8_465 . ? O2W Na2 O3 79.67(7) . . ? O1W Na2 O1 88.87(5) 8_465 7_565 ? O2W Na2 O1 96.72(7) . 7_565 ? O3 Na2 O1 89.70(5) . 7_565 ? O1W Na2 O5 85.76(5) 8_465 8_465 ? O2W Na2 O5 89.28(7) . 8_465 ? O3 Na2 O5 93.57(5) . 8_465 ? O1 Na2 O5 173.60(5) 7_565 8_465 ? O1W Na2 N1 99.53(7) 8_465 8_566 ? O2W Na2 N1 91.63(8) . 8_566 ? O3 Na2 N1 166.47(6) . 8_566 ? O1 Na2 N1 101.68(6) 7_565 8_566 ? O5 Na2 N1 75.84(5) 8_465 8_566 ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.675 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.055 #===end data_Compd3a _database_code_depnum_ccdc_archive 'CCDC 682497' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Mn N6 O8 S2' _chemical_formula_weight 643.55 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' Mn Mn 0.3368 0.7283 '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 6.0026(18) _cell_length_b 7.049(2) _cell_length_c 15.438(5) _cell_angle_alpha 100.329(9) _cell_angle_beta 100.032(15) _cell_angle_gamma 96.299(12) _cell_volume 626.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2782 _cell_measurement_theta_min 2.97 _cell_measurement_theta_max 27.48 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.707 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 331 _exptl_absorpt_coefficient_mu 0.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.833 _exptl_absorpt_correction_T_max 0.859 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4849 _diffrn_reflns_av_R_equivalents 0.0177 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2782 _reflns_number_gt 2401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0800P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2782 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0351 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mn1 Mn 1.0000 0.0000 1.0000 0.01908(13) Uani 1 2 d S . . S1 S 1.18170(7) 0.28137(5) 0.86087(2) 0.02008(13) Uani 1 1 d . . . O1W O 0.7286(2) 0.18764(19) 1.00006(9) 0.0274(3) Uani 1 1 d . . . O1 O 1.0941(2) 0.09866(17) 0.88415(8) 0.0271(3) Uani 1 1 d . . . O3 O 1.4289(2) 0.3142(2) 0.87479(9) 0.0355(3) Uani 1 1 d . . . O2 O 1.0878(3) 0.44456(19) 0.90610(9) 0.0366(3) Uani 1 1 d . . . N1 N 0.7455(3) -0.2591(2) 0.90817(10) 0.0247(3) Uani 1 1 d . . . C2 C 1.2205(3) 0.3040(3) 0.68892(12) 0.0249(4) Uani 1 1 d . . . C1 C 1.0752(3) 0.2556(2) 0.74496(10) 0.0188(3) Uani 1 1 d . . . C6 C 0.8425(3) 0.1939(3) 0.71170(12) 0.0255(4) Uani 1 1 d . . . C4 C 0.8988(3) 0.2369(2) 0.56569(11) 0.0233(3) Uani 1 1 d . . . C5 C 0.7544(3) 0.1853(3) 0.62180(12) 0.0262(4) Uani 1 1 d . . . C3 C 1.1328(3) 0.2902(3) 0.59871(12) 0.0287(4) Uani 1 1 d . . . H2A H 1.365(4) 0.343(3) 0.7143(15) 0.031(5) Uiso 1 1 d . . . H5A H 0.605(5) 0.134(4) 0.6005(18) 0.049(7) Uiso 1 1 d . . . H1D H 0.644(4) -0.267(3) 0.9346(17) 0.039(7) Uiso 1 1 d . . . H6A H 0.743(4) 0.154(3) 0.7474(16) 0.035(6) Uiso 1 1 d . . . H1C H 0.826(4) -0.361(4) 0.9060(17) 0.045(7) Uiso 1 1 d . . . H3A H 1.231(4) 0.309(4) 0.5540(17) 0.051(7) Uiso 1 1 d . . . H1B H 0.768(4) 0.310(4) 1.0276(18) 0.040(6) Uiso 1 1 d . . . H1A H 0.636(5) 0.186(4) 0.9499(19) 0.046(7) Uiso 1 1 d . . . C10 C 0.3469(3) 0.2549(2) 0.18329(11) 0.0207(3) Uani 1 1 d . . . N3 N 0.6130(3) 0.2533(2) 0.45342(10) 0.0264(3) Uani 1 1 d . . . N2 N 0.8214(3) 0.2365(2) 0.47264(10) 0.0280(3) Uani 1 1 d . . . C11 C 0.2275(3) 0.3119(2) 0.25067(12) 0.0248(3) Uani 1 1 d . . . C8 C 0.6488(3) 0.1861(2) 0.29297(11) 0.0242(3) Uani 1 1 d . . . C7 C 0.5315(3) 0.2487(2) 0.36062(11) 0.0230(3) Uani 1 1 d . . . C9 C 0.5561(3) 0.1886(2) 0.20469(11) 0.0238(3) Uani 1 1 d . . . C12 C 0.3186(3) 0.3082(3) 0.33884(12) 0.0266(4) Uani 1 1 d . . . H11A H 0.079(4) 0.365(3) 0.2412(16) 0.038(6) Uiso 1 1 d . . . H12A H 0.246(4) 0.353(3) 0.3850(15) 0.030(5) Uiso 1 1 d . . . H8A H 0.807(4) 0.141(3) 0.3088(16) 0.035(6) Uiso 1 1 d . . . H9A H 0.631(4) 0.151(3) 0.1613(15) 0.026(5) Uiso 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 Mn1 0.0218(2) 0.02174(19) 0.01380(19) 0.00581(13) 0.00183(13) 0.00276(14) S1 0.0246(2) 0.0223(2) 0.0125(2) 0.00550(15) -0.00037(15) 0.00340(16) O1W 0.0268(7) 0.0309(7) 0.0241(7) 0.0081(5) -0.0003(5) 0.0069(5) O1 0.0393(7) 0.0275(6) 0.0168(6) 0.0109(5) 0.0058(5) 0.0034(5) O3 0.0252(7) 0.0517(8) 0.0287(7) 0.0180(6) -0.0047(5) 0.0008(6) O2 0.0538(9) 0.0290(7) 0.0239(7) -0.0016(5) 0.0010(6) 0.0146(6) N1 0.0265(8) 0.0294(8) 0.0161(7) 0.0074(5) -0.0016(6) -0.0006(6) C2 0.0188(8) 0.0357(9) 0.0198(8) 0.0096(7) 0.0002(7) 0.0012(7) C1 0.0232(8) 0.0197(7) 0.0136(7) 0.0063(5) 0.0005(6) 0.0042(6) C6 0.0240(8) 0.0338(9) 0.0188(8) 0.0101(7) 0.0026(7) -0.0005(7) C4 0.0279(9) 0.0266(8) 0.0146(7) 0.0064(6) -0.0001(6) 0.0033(7) C5 0.0218(8) 0.0329(9) 0.0219(8) 0.0098(7) -0.0022(7) -0.0019(7) C3 0.0255(9) 0.0419(10) 0.0198(8) 0.0116(7) 0.0040(7) 0.0021(7) C10 0.0231(8) 0.0215(7) 0.0148(7) 0.0053(6) -0.0018(6) -0.0019(6) N3 0.0304(8) 0.0318(8) 0.0166(7) 0.0080(6) 0.0004(6) 0.0046(6) N2 0.0292(8) 0.0377(8) 0.0158(7) 0.0085(6) -0.0016(6) 0.0034(6) C11 0.0235(8) 0.0287(8) 0.0226(8) 0.0069(6) 0.0016(7) 0.0073(7) C8 0.0237(8) 0.0289(8) 0.0198(8) 0.0069(6) 0.0006(7) 0.0052(7) C7 0.0266(8) 0.0248(8) 0.0168(8) 0.0075(6) 0.0000(6) 0.0022(6) C9 0.0243(8) 0.0306(8) 0.0171(8) 0.0049(6) 0.0041(7) 0.0059(7) C12 0.0287(9) 0.0335(9) 0.0192(8) 0.0056(7) 0.0061(7) 0.0083(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 Mn1 O1 2.1710(12) 2_757 ? Mn1 O1 2.1710(12) . ? Mn1 O1W 2.2083(14) 2_757 ? Mn1 O1W 2.2083(14) . ? Mn1 N1 2.3204(16) . ? Mn1 N1 2.3204(16) 2_757 ? S1 O3 1.4482(14) . ? S1 O2 1.4561(13) . ? S1 O1 1.4655(12) . ? S1 C1 1.7615(17) . ? N1 C10 1.431(2) 2_656 ? C2 C3 1.382(2) . ? C2 C1 1.389(2) . ? C1 C6 1.393(2) . ? C6 C5 1.384(2) . ? C4 C5 1.393(2) . ? C4 C3 1.393(3) . ? C4 N2 1.430(2) . ? C10 C11 1.390(2) . ? C10 C9 1.394(2) . ? C10 N1 1.431(2) 2_656 ? N3 N2 1.258(2) . ? N3 C7 1.424(2) . ? C11 C12 1.382(2) . ? C8 C9 1.383(2) . ? C8 C7 1.393(2) . ? C7 C12 1.393(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mn1 O1 180.000(1) 2_757 . ? O1 Mn1 O1W 90.52(5) 2_757 2_757 ? O1 Mn1 O1W 89.48(5) . 2_757 ? O1 Mn1 O1W 89.48(5) 2_757 . ? O1 Mn1 O1W 90.52(5) . . ? O1W Mn1 O1W 180.000(1) 2_757 . ? O1 Mn1 N1 88.71(5) 2_757 . ? O1 Mn1 N1 91.29(5) . . ? O1W Mn1 N1 88.89(6) 2_757 . ? O1W Mn1 N1 91.11(6) . . ? O1 Mn1 N1 91.29(5) 2_757 2_757 ? O1 Mn1 N1 88.71(5) . 2_757 ? O1W Mn1 N1 91.11(6) 2_757 2_757 ? O1W Mn1 N1 88.89(6) . 2_757 ? N1 Mn1 N1 180.0 . 2_757 ? O3 S1 O2 113.05(9) . . ? O3 S1 O1 112.63(8) . . ? O2 S1 O1 110.90(8) . . ? O3 S1 C1 107.36(8) . . ? O2 S1 C1 106.65(8) . . ? O1 S1 C1 105.72(7) . . ? S1 O1 Mn1 138.22(8) . . ? C10 N1 Mn1 121.22(10) 2_656 . ? C3 C2 C1 119.43(16) . . ? C2 C1 C6 121.03(15) . . ? C2 C1 S1 120.10(13) . . ? C6 C1 S1 118.82(12) . . ? C5 C6 C1 119.30(15) . . ? C5 C4 C3 120.38(16) . . ? C5 C4 N2 123.50(16) . . ? C3 C4 N2 116.11(15) . . ? C6 C5 C4 119.85(17) . . ? C2 C3 C4 119.89(15) . . ? C11 C10 C9 119.68(15) . . ? C11 C10 N1 120.58(16) . 2_656 ? C9 C10 N1 119.72(15) . 2_656 ? N2 N3 C7 113.91(14) . . ? N3 N2 C4 113.10(14) . . ? C12 C11 C10 120.16(16) . . ? C9 C8 C7 119.77(16) . . ? C12 C7 C8 119.90(15) . . ? C12 C7 N3 115.99(14) . . ? C8 C7 N3 124.10(15) . . ? C8 C9 C10 120.32(15) . . ? C11 C12 C7 120.11(15) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.379 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.052 #===end data_Compd3b _database_code_depnum_ccdc_archive 'CCDC 682498' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Co N6 O8 P0 S2' _chemical_formula_weight 647.54 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' P P 0.1023 0.0942 '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' S S 0.1246 0.1234 '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 5.9988(2) _cell_length_b 6.9651(2) _cell_length_c 15.3459(2) _cell_angle_alpha 99.851(9) _cell_angle_beta 100.327(12) _cell_angle_gamma 97.087(9) _cell_volume 613.60(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2764 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.48 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.752 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 333 _exptl_absorpt_coefficient_mu 0.936 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.799 _exptl_absorpt_correction_T_max 0.829 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4723 _diffrn_reflns_av_R_equivalents 0.0161 _diffrn_reflns_av_sigmaI/netI 0.0247 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2764 _reflns_number_gt 2492 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1628P)^2^+0.3694P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2764 _refine_ls_number_parameters 203 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0546 _refine_ls_R_factor_gt 0.0395 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1154 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _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 O1 O -0.5870(5) 0.0552(3) -0.40857(16) 0.0317(6) Uani 1 1 d . . . O2 O -0.9281(4) 0.1897(4) -0.37819(16) 0.0310(6) Uani 1 1 d . . . O3 O -0.5843(4) 0.4071(3) -0.38501(14) 0.0227(5) Uani 1 1 d . . . O1W O -0.7600(4) 0.6775(3) -0.50010(16) 0.0230(5) Uani 1 1 d . . . N1 N -0.7496(4) 0.2483(4) -0.58708(17) 0.0201(5) Uani 1 1 d . . . N2 N -0.3227(5) 0.2625(4) 0.02787(18) 0.0262(6) Uani 1 1 d . . . N3 N -0.1137(5) 0.2458(4) 0.04786(17) 0.0241(5) Uani 1 1 d . . . C6 C -0.3399(5) 0.3028(5) -0.2129(2) 0.0234(6) Uani 1 1 d . . . H6A H -0.2430 0.3359 -0.2508 0.028 Uiso 1 1 calc R . . H2A H -0.870(7) 0.677(6) -0.553(3) 0.025(9) Uiso 1 1 d . . . H1D H -0.847(7) 0.242(5) -0.557(3) 0.016(8) Uiso 1 1 d . . . C10 C 0.1561(5) 0.2509(4) 0.32049(19) 0.0188(6) Uani 1 1 d . . . H1C H -0.655(8) 0.136(7) -0.576(3) 0.040(12) Uiso 1 1 d . . . C8 C -0.1492(5) 0.3146(5) 0.2093(2) 0.0220(6) Uani 1 1 d . . . H8A H -0.2905 0.3555 0.1943 0.026 Uiso 1 1 calc R . . H1A H -0.727(7) 0.802(7) -0.466(3) 0.031(11) Uiso 1 1 d . . . C1 C -0.5747(5) 0.2441(4) -0.24647(18) 0.0166(5) Uani 1 1 d . . . C4 C -0.3989(5) 0.2623(4) -0.06604(19) 0.0214(6) Uani 1 1 d . . . C12 C 0.1832(5) 0.1947(5) 0.1643(2) 0.0244(6) Uani 1 1 d . . . H12A H 0.2634 0.1578 0.1192 0.029 Uiso 1 1 calc R . . C11 C 0.2764(5) 0.1923(5) 0.2532(2) 0.0228(6) Uani 1 1 d . . . H11A H 0.4182 0.1521 0.2681 0.027 Uiso 1 1 calc R . . C5 C -0.2529(5) 0.3110(5) -0.1222(2) 0.0249(6) Uani 1 1 d . . . H5A H -0.0965 0.3493 -0.0989 0.030 Uiso 1 1 calc R . . C7 C -0.0305(5) 0.2523(4) 0.14208(19) 0.0203(6) Uani 1 1 d . . . C3 C -0.6341(6) 0.2106(5) -0.0994(2) 0.0257(7) Uani 1 1 d . . . H3A H -0.7320 0.1848 -0.0607 0.031 Uiso 1 1 calc R . . C9 C -0.0543(5) 0.3149(4) 0.2992(2) 0.0212(6) Uani 1 1 d . . . H9A H -0.1310 0.3575 0.3447 0.025 Uiso 1 1 calc R . . C2 C -0.7218(5) 0.1976(5) -0.1904(2) 0.0235(6) Uani 1 1 d . . . H2B H -0.8781 0.1580 -0.2137 0.028 Uiso 1 1 calc R . . S1 S -0.67974(12) 0.22042(10) -0.36330(4) 0.0174(2) Uani 1 1 d . . . Co1 Co -0.5000 0.5000 -0.5000 0.0152(2) Uani 1 2 d S . . 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 O1 0.0471(15) 0.0229(11) 0.0232(12) -0.0007(9) 0.0028(10) 0.0123(10) O2 0.0208(11) 0.0445(14) 0.0244(12) 0.0132(10) -0.0070(9) 0.0008(10) O3 0.0337(11) 0.0202(10) 0.0151(10) 0.0063(8) 0.0065(8) 0.0017(8) O1W 0.0200(10) 0.0236(11) 0.0243(11) 0.0064(9) -0.0017(8) 0.0062(8) N1 0.0222(12) 0.0235(12) 0.0124(11) 0.0052(9) -0.0010(9) -0.0005(9) N2 0.0268(13) 0.0352(15) 0.0157(12) 0.0078(11) -0.0003(10) 0.0045(11) N3 0.0276(13) 0.0300(13) 0.0136(12) 0.0063(10) -0.0001(10) 0.0034(10) C6 0.0219(14) 0.0310(15) 0.0178(14) 0.0094(12) 0.0036(11) 0.0010(11) C10 0.0233(13) 0.0167(12) 0.0140(13) 0.0035(10) -0.0009(10) -0.0002(10) C8 0.0208(13) 0.0267(14) 0.0183(14) 0.0057(11) 0.0006(11) 0.0057(11) C1 0.0215(13) 0.0173(12) 0.0103(12) 0.0047(10) 0.0000(10) 0.0030(10) C4 0.0264(15) 0.0234(14) 0.0122(13) 0.0037(10) -0.0010(11) 0.0028(11) C12 0.0250(14) 0.0289(15) 0.0193(14) 0.0033(11) 0.0052(11) 0.0061(12) C11 0.0219(14) 0.0265(14) 0.0201(14) 0.0055(11) 0.0013(11) 0.0078(11) C5 0.0180(13) 0.0318(15) 0.0224(15) 0.0100(12) -0.0028(11) -0.0022(11) C7 0.0233(14) 0.0229(13) 0.0126(13) 0.0039(10) -0.0005(10) 0.0016(10) C3 0.0258(15) 0.0375(17) 0.0159(14) 0.0092(12) 0.0070(12) 0.0032(12) C9 0.0209(14) 0.0271(14) 0.0145(13) 0.0029(11) 0.0019(10) 0.0041(11) C2 0.0192(13) 0.0322(15) 0.0187(15) 0.0088(12) 0.0008(11) 0.0012(11) S1 0.0218(4) 0.0178(4) 0.0116(4) 0.0042(3) -0.0005(3) 0.0029(3) Co1 0.0180(3) 0.0163(3) 0.0109(3) 0.0037(2) 0.0013(2) 0.0030(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 O1 S1 1.463(2) . ? O2 S1 1.449(2) . ? O3 S1 1.470(2) . ? O3 Co1 2.102(2) . ? O1W Co1 2.106(2) . ? N1 C10 1.434(3) 1_454 ? N1 Co1 2.221(3) . ? N2 N3 1.261(4) . ? N2 C4 1.431(4) . ? N3 C7 1.433(4) . ? C6 C5 1.385(4) . ? C6 C1 1.394(4) . ? C10 C9 1.392(4) . ? C10 C11 1.396(4) . ? C10 N1 1.434(3) 1_656 ? C8 C7 1.395(4) . ? C8 C9 1.394(4) . ? C1 C2 1.386(4) . ? C1 S1 1.762(3) . ? C4 C3 1.391(4) . ? C4 C5 1.386(4) . ? C12 C11 1.383(4) . ? C12 C7 1.392(4) . ? C3 C2 1.384(4) . ? Co1 O3 2.102(2) 2_464 ? Co1 O1W 2.106(2) 2_464 ? Co1 N1 2.221(3) 2_464 ? 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 S1 O3 Co1 136.25(14) . . ? C10 N1 Co1 121.31(17) 1_454 . ? N3 N2 C4 112.9(3) . . ? N2 N3 C7 114.1(3) . . ? C5 C6 C1 119.1(3) . . ? C9 C10 C11 120.8(3) . . ? C9 C10 N1 119.2(3) . 1_656 ? C11 C10 N1 120.0(3) . 1_656 ? C7 C8 C9 119.5(3) . . ? C2 C1 C6 121.1(3) . . ? C2 C1 S1 120.5(2) . . ? C6 C1 S1 118.4(2) . . ? C3 C4 C5 120.6(3) . . ? C3 C4 N2 115.8(3) . . ? C5 C4 N2 123.6(3) . . ? C11 C12 C7 120.1(3) . . ? C12 C11 C10 119.5(3) . . ? C6 C5 C4 120.0(3) . . ? C12 C7 C8 120.5(3) . . ? C12 C7 N3 115.7(3) . . ? C8 C7 N3 123.8(3) . . ? C2 C3 C4 119.7(3) . . ? C10 C9 C8 119.6(3) . . ? C3 C2 C1 119.4(3) . . ? O2 S1 O1 113.76(16) . . ? O2 S1 O3 112.85(14) . . ? O1 S1 O3 110.71(14) . . ? O2 S1 C1 107.31(14) . . ? O1 S1 C1 106.55(14) . . ? O3 S1 C1 105.01(13) . . ? O3 Co1 O3 180.000(1) . 2_464 ? O3 Co1 O1W 89.24(9) . . ? O3 Co1 O1W 90.76(9) 2_464 . ? O3 Co1 O1W 90.76(9) . 2_464 ? O3 Co1 O1W 89.24(9) 2_464 2_464 ? O1W Co1 O1W 180.00(13) . 2_464 ? O3 Co1 N1 90.47(9) . 2_464 ? O3 Co1 N1 89.53(9) 2_464 2_464 ? O1W Co1 N1 89.63(9) . 2_464 ? O1W Co1 N1 90.37(9) 2_464 2_464 ? O3 Co1 N1 89.53(9) . . ? O3 Co1 N1 90.47(9) 2_464 . ? O1W Co1 N1 90.37(9) . . ? O1W Co1 N1 89.63(10) 2_464 . ? N1 Co1 N1 180.0 2_464 . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.859 _refine_diff_density_min -1.173 _refine_diff_density_rms 0.265 #===end data_Compd3c _database_code_depnum_ccdc_archive 'CCDC 682499' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cu N6 O8 S2' _chemical_formula_weight 652.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 5.933(2) _cell_length_b 6.985(2) _cell_length_c 15.325(6) _cell_angle_alpha 102.104(10) _cell_angle_beta 98.278(13) _cell_angle_gamma 95.670(10) _cell_volume 609.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2728 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.49 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 335 _exptl_absorpt_coefficient_mu 1.135 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.762 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4765 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 2728 _reflns_number_gt 2219 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0540P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2728 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0379 _refine_ls_R_factor_gt 0.0302 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Cu1 Cu 0.5000 0.5000 1.0000 0.01797(12) Uani 1 2 d S . . O1W O 0.2422(3) 0.6727(2) 1.00441(11) 0.0241(3) Uani 1 1 d . . . N1 N 0.6479(4) 0.6515(3) 0.91780(11) 0.0205(4) Uani 1 1 d . . . C10 C 0.6528(3) 0.5589(3) 0.82467(12) 0.0173(4) Uani 1 1 d . . . C7 C 0.6680(4) 0.3846(3) 0.64630(12) 0.0203(4) Uani 1 1 d . . . C11 C 0.4648(4) 0.5525(3) 0.75798(13) 0.0220(4) Uani 1 1 d . . . N3 N 0.6609(3) 0.3008(3) 0.55240(11) 0.0246(4) Uani 1 1 d . . . C8 C 0.8530(4) 0.3862(3) 0.71342(13) 0.0220(4) Uani 1 1 d . . . C9 C 0.8457(4) 0.4738(3) 0.80269(13) 0.0210(4) Uani 1 1 d . . . C12 C 0.4732(4) 0.4652(3) 0.66902(14) 0.0239(4) Uani 1 1 d . . . H8A H 0.981(4) 0.321(3) 0.6962(15) 0.025(6) Uiso 1 1 d . . . H11A H 0.327(4) 0.610(3) 0.7731(16) 0.031(6) Uiso 1 1 d . . . H1B H 0.591(5) 0.751(4) 0.9163(17) 0.029(7) Uiso 1 1 d . . . H12A H 0.355(4) 0.462(4) 0.6265(17) 0.027(6) Uiso 1 1 d . . . H1A H 0.773(5) 0.679(4) 0.9380(17) 0.024(7) Uiso 1 1 d . . . H1D H 0.254(5) 0.758(4) 0.975(2) 0.046(9) Uiso 1 1 d . . . H1C H 0.211(5) 0.728(4) 1.0509(19) 0.034(7) Uiso 1 1 d . . . H9A H 0.971(4) 0.480(3) 0.8500(17) 0.027(6) Uiso 1 1 d . . . N2 N 0.8529(3) 0.2674(3) 0.53197(11) 0.0258(4) Uani 1 1 d . . . C4 C 0.8418(4) 0.1785(3) 0.43832(12) 0.0216(4) Uani 1 1 d . . . S1 S 0.83976(9) -0.06212(7) 0.14000(3) 0.02007(13) Uani 1 1 d . . . O1 O 0.7311(3) -0.2652(2) 0.11872(9) 0.0277(3) Uani 1 1 d . . . C5 C 0.6430(4) 0.0738(3) 0.38268(14) 0.0254(5) Uani 1 1 d . . . H5A H 0.5060 0.0551 0.4069 0.030 Uiso 1 1 calc R . . C1 C 0.8463(4) 0.0272(3) 0.25757(12) 0.0185(4) Uani 1 1 d . . . O2 O 1.0755(3) -0.0425(2) 0.12462(10) 0.0346(4) Uani 1 1 d . . . O3 O 0.6988(3) 0.0604(2) 0.09505(10) 0.0366(4) Uani 1 1 d . . . C3 C 1.0449(4) 0.2014(3) 0.40396(14) 0.0262(5) Uani 1 1 d . . . C2 C 1.0459(4) 0.1288(3) 0.31254(13) 0.0238(4) Uani 1 1 d . . . H2A H 1.1823 0.1487 0.2880 0.029 Uiso 1 1 calc R . . C6 C 0.6447(4) -0.0032(3) 0.29199(14) 0.0242(4) Uani 1 1 d . . . H6A H 0.514(5) -0.077(4) 0.2567(17) 0.029(6) Uiso 1 1 d . . . H3A H 1.175(5) 0.261(3) 0.4411(17) 0.033(7) Uiso 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 Cu1 0.0208(2) 0.0211(2) 0.01265(17) 0.00316(13) 0.00432(13) 0.00510(14) O1W 0.0283(8) 0.0239(8) 0.0212(7) 0.0034(7) 0.0076(6) 0.0077(6) N1 0.0238(10) 0.0209(9) 0.0151(8) -0.0001(7) 0.0049(7) 0.0016(8) C10 0.0228(10) 0.0160(9) 0.0125(8) 0.0021(7) 0.0051(7) -0.0001(8) C7 0.0245(10) 0.0207(10) 0.0133(8) -0.0005(7) 0.0035(7) 0.0011(8) C11 0.0206(10) 0.0251(10) 0.0202(9) 0.0033(8) 0.0045(8) 0.0055(9) N3 0.0298(10) 0.0265(9) 0.0151(8) -0.0005(7) 0.0048(7) 0.0026(8) C8 0.0217(10) 0.0256(11) 0.0187(9) 0.0023(8) 0.0061(8) 0.0054(9) C9 0.0211(10) 0.0250(10) 0.0159(9) 0.0039(8) 0.0007(8) 0.0030(8) C12 0.0214(11) 0.0302(11) 0.0175(9) 0.0032(8) -0.0019(8) 0.0036(9) N2 0.0300(10) 0.0300(10) 0.0142(8) -0.0015(7) 0.0049(7) 0.0011(8) C4 0.0265(11) 0.0230(10) 0.0135(9) -0.0001(8) 0.0037(8) 0.0035(9) S1 0.0276(3) 0.0206(3) 0.0114(2) 0.00065(18) 0.00397(19) 0.0060(2) O1 0.0359(9) 0.0229(8) 0.0187(7) -0.0018(6) -0.0022(6) 0.0013(7) C5 0.0233(11) 0.0297(11) 0.0204(9) -0.0015(8) 0.0083(8) -0.0012(9) C1 0.0252(10) 0.0161(9) 0.0134(8) 0.0002(7) 0.0037(7) 0.0047(8) O2 0.0342(9) 0.0419(10) 0.0255(8) -0.0031(7) 0.0151(7) 0.0036(8) O3 0.0549(11) 0.0383(9) 0.0231(8) 0.0126(7) 0.0081(7) 0.0233(8) C3 0.0224(11) 0.0319(12) 0.0184(9) -0.0026(8) -0.0002(8) -0.0024(9) C2 0.0212(10) 0.0279(11) 0.0201(9) 0.0002(8) 0.0057(8) 0.0002(9) C6 0.0233(11) 0.0259(11) 0.0198(10) -0.0001(8) 0.0027(8) -0.0013(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1W 2.0396(16) 2_667 ? Cu1 O1W 2.0396(16) . ? Cu1 N1 2.0423(19) . ? Cu1 N1 2.0423(19) 2_667 ? Cu1 O1 2.3380(16) 2_656 ? Cu1 O1 2.3380(16) 1_566 ? N1 C10 1.444(2) . ? C10 C11 1.390(3) . ? C10 C9 1.392(3) . ? C7 C12 1.392(3) . ? C7 C8 1.389(3) . ? C7 N3 1.428(2) . ? C11 C12 1.382(3) . ? N3 N2 1.255(3) . ? C8 C9 1.385(3) . ? N2 C4 1.428(2) . ? C4 C5 1.390(3) . ? C4 C3 1.391(3) . ? S1 O1 1.4487(16) . ? S1 O2 1.4496(18) . ? S1 O3 1.4591(16) . ? S1 C1 1.7720(19) . ? O1 Cu1 2.3380(16) 1_544 ? C5 C6 1.383(3) . ? C1 C2 1.383(3) . ? C1 C6 1.391(3) . ? C3 C2 1.388(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1W Cu1 O1W 180.00(9) 2_667 . ? O1W Cu1 N1 88.93(8) 2_667 . ? O1W Cu1 N1 91.07(8) . . ? O1W Cu1 N1 91.07(8) 2_667 2_667 ? O1W Cu1 N1 88.93(8) . 2_667 ? N1 Cu1 N1 180.000(1) . 2_667 ? O1W Cu1 O1 90.08(6) 2_667 2_656 ? O1W Cu1 O1 89.92(6) . 2_656 ? N1 Cu1 O1 94.92(7) . 2_656 ? N1 Cu1 O1 85.08(7) 2_667 2_656 ? O1W Cu1 O1 89.92(6) 2_667 1_566 ? O1W Cu1 O1 90.08(6) . 1_566 ? N1 Cu1 O1 85.08(7) . 1_566 ? N1 Cu1 O1 94.92(7) 2_667 1_566 ? O1 Cu1 O1 180.000(1) 2_656 1_566 ? C10 N1 Cu1 121.10(14) . . ? C11 C10 C9 120.50(17) . . ? C11 C10 N1 120.12(18) . . ? C9 C10 N1 119.38(18) . . ? C12 C7 C8 120.10(18) . . ? C12 C7 N3 115.99(18) . . ? C8 C7 N3 123.90(18) . . ? C12 C11 C10 119.38(19) . . ? N2 N3 C7 114.00(17) . . ? C9 C8 C7 119.78(18) . . ? C8 C9 C10 119.83(18) . . ? C11 C12 C7 120.36(19) . . ? N3 N2 C4 113.29(17) . . ? C5 C4 C3 120.36(18) . . ? C5 C4 N2 123.50(19) . . ? C3 C4 N2 116.14(19) . . ? O1 S1 O2 113.34(10) . . ? O1 S1 O3 111.13(10) . . ? O2 S1 O3 112.94(10) . . ? O1 S1 C1 105.93(9) . . ? O2 S1 C1 107.06(10) . . ? O3 S1 C1 105.81(9) . . ? S1 O1 Cu1 140.70(9) . 1_544 ? C6 C5 C4 120.0(2) . . ? C2 C1 C6 121.36(18) . . ? C2 C1 S1 120.42(16) . . ? C6 C1 S1 118.20(16) . . ? C2 C3 C4 119.8(2) . . ? C1 C2 C3 119.3(2) . . ? C5 C6 C1 119.1(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.410 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.064 #===end data_Compd3d _database_code_depnum_ccdc_archive 'CCDC 682500' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 N6 O8 S2 Zn' _chemical_formula_weight 653.98 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' Zn Zn 0.2839 1.4301 '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 5.9751(16) _cell_length_b 6.9775(19) _cell_length_c 15.374(5) _cell_angle_alpha 99.920(9) _cell_angle_beta 100.404(16) _cell_angle_gamma 96.932(13) _cell_volume 613.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2728 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.47 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 336 _exptl_absorpt_coefficient_mu 1.238 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.781 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4734 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2728 _reflns_number_gt 2459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0550P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2728 _refine_ls_number_parameters 235 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.5000 0.5000 1.0000 0.01762(9) Uani 1 2 d S . . S1 S 0.67968(6) 0.78478(5) 0.86272(2) 0.01788(10) Uani 1 1 d . . . O1 O 0.5900(2) 0.59833(15) 0.88504(7) 0.0238(2) Uani 1 1 d . . . O3 O 0.9287(2) 0.81987(19) 0.87759(8) 0.0323(3) Uani 1 1 d . . . O1W O 0.2334(2) 0.67879(17) 0.99997(8) 0.0241(2) Uani 1 1 d . . . N1 N 0.2536(2) 0.25690(19) 0.91469(8) 0.0209(3) Uani 1 1 d . . . O2 O 0.5847(2) 0.94799(16) 0.90735(7) 0.0320(3) Uani 1 1 d . . . C2 C 0.7210(3) 0.8062(2) 0.69006(10) 0.0243(3) Uani 1 1 d . . . C1 C 0.5736(2) 0.7602(2) 0.74560(9) 0.0173(3) Uani 1 1 d . . . C5 C 0.2500(3) 0.6904(2) 0.62153(10) 0.0246(3) Uani 1 1 d . . . C4 C 0.3976(3) 0.7393(2) 0.56513(9) 0.0217(3) Uani 1 1 d . . . C6 C 0.3390(3) 0.6996(2) 0.71194(10) 0.0234(3) Uani 1 1 d . . . C3 C 0.6329(3) 0.7924(3) 0.59874(11) 0.0269(3) Uani 1 1 d . . . H5A H 0.090(4) 0.646(3) 0.5981(14) 0.030(5) Uiso 1 1 d . . . H2B H 0.866(4) 0.842(3) 0.7098(13) 0.029(5) Uiso 1 1 d . . . H6A H 0.244(3) 0.665(3) 0.7498(13) 0.031(5) Uiso 1 1 d . . . H3A H 0.727(4) 0.821(3) 0.5643(14) 0.035(5) Uiso 1 1 d . . . H2A H 0.288(4) 0.799(4) 1.0257(16) 0.044(6) Uiso 1 1 d . . . H1A H 0.154(4) 0.686(3) 0.9510(16) 0.039(6) Uiso 1 1 d . . . H1D H 0.313(3) 0.152(3) 0.9159(14) 0.031(5) Uiso 1 1 d . . . H1C H 0.145(4) 0.246(3) 0.9395(13) 0.027(5) Uiso 1 1 d . . . N3 N 0.1113(2) 0.75338(19) 0.45099(8) 0.0250(3) Uani 1 1 d . . . C10 C -0.1583(3) 0.7431(2) 0.17810(9) 0.0185(3) Uani 1 1 d . . . C7 C 0.0285(3) 0.7456(2) 0.35728(9) 0.0208(3) Uani 1 1 d . . . N2 N 0.3196(2) 0.7371(2) 0.47128(8) 0.0268(3) Uani 1 1 d . . . C12 C -0.1854(3) 0.8035(2) 0.33413(10) 0.0239(3) Uani 1 1 d . . . C11 C -0.2792(3) 0.8033(2) 0.24476(10) 0.0227(3) Uani 1 1 d . . . C8 C 0.1463(3) 0.6808(2) 0.28995(10) 0.0222(3) Uani 1 1 d . . . C9 C 0.0523(3) 0.6793(2) 0.20100(10) 0.0213(3) Uani 1 1 d . . . H11A H -0.419(3) 0.853(3) 0.2305(12) 0.024(4) Uiso 1 1 d . . . H8A H 0.286(3) 0.649(2) 0.3076(11) 0.017(4) Uiso 1 1 d . . . H9A H 0.135(3) 0.635(3) 0.1538(13) 0.031(5) Uiso 1 1 d . . . H12A H -0.266(4) 0.850(3) 0.3776(14) 0.038(5) Uiso 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 Zn1 0.01965(14) 0.01902(14) 0.01316(13) 0.00403(9) 0.00004(9) 0.00276(9) S1 0.0219(2) 0.01913(18) 0.01136(17) 0.00467(13) -0.00148(13) 0.00316(14) O1 0.0343(6) 0.0220(5) 0.0159(5) 0.0075(4) 0.0042(4) 0.0036(4) O3 0.0233(6) 0.0465(7) 0.0245(6) 0.0140(5) -0.0057(5) 0.0010(5) O1W 0.0243(6) 0.0257(6) 0.0220(6) 0.0067(5) -0.0002(4) 0.0073(5) N1 0.0224(7) 0.0239(6) 0.0144(6) 0.0060(5) -0.0020(5) 0.0010(5) O2 0.0468(8) 0.0247(6) 0.0220(6) -0.0011(4) 0.0020(5) 0.0121(5) C2 0.0179(7) 0.0338(8) 0.0203(7) 0.0095(6) -0.0004(6) 0.0013(6) C1 0.0218(7) 0.0179(6) 0.0120(6) 0.0054(5) -0.0001(5) 0.0038(5) C5 0.0192(7) 0.0322(8) 0.0199(7) 0.0095(6) -0.0033(6) -0.0013(6) C4 0.0265(8) 0.0244(7) 0.0127(6) 0.0050(5) -0.0015(6) 0.0046(6) C6 0.0211(7) 0.0304(8) 0.0191(7) 0.0099(6) 0.0030(6) -0.0004(6) C3 0.0245(8) 0.0400(9) 0.0178(7) 0.0111(6) 0.0052(6) 0.0017(7) N3 0.0283(7) 0.0299(7) 0.0151(6) 0.0065(5) -0.0011(5) 0.0038(6) C10 0.0210(7) 0.0175(6) 0.0148(6) 0.0041(5) -0.0011(5) 0.0000(5) C7 0.0237(7) 0.0226(7) 0.0145(7) 0.0056(5) -0.0010(5) 0.0016(6) N2 0.0264(7) 0.0371(7) 0.0150(6) 0.0083(5) -0.0025(5) 0.0030(6) C12 0.0262(8) 0.0288(7) 0.0177(7) 0.0040(6) 0.0056(6) 0.0077(6) C11 0.0205(7) 0.0269(7) 0.0207(7) 0.0057(6) 0.0008(6) 0.0076(6) C8 0.0189(7) 0.0259(7) 0.0209(7) 0.0062(6) -0.0007(6) 0.0051(6) C9 0.0205(7) 0.0255(7) 0.0176(7) 0.0037(5) 0.0030(6) 0.0043(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 Zn1 O1 2.1344(11) 2_667 ? Zn1 O1 2.1344(11) . ? Zn1 O1W 2.1388(12) . ? Zn1 O1W 2.1388(12) 2_667 ? Zn1 N1 2.1676(14) 2_667 ? Zn1 N1 2.1676(14) . ? S1 O3 1.4477(13) . ? S1 O2 1.4551(12) . ? S1 O1 1.4660(11) . ? S1 C1 1.7687(15) . ? N1 C10 1.4374(18) 2_566 ? C2 C1 1.380(2) . ? C2 C3 1.390(2) . ? C1 C6 1.390(2) . ? C5 C6 1.383(2) . ? C5 C4 1.397(2) . ? C4 C3 1.388(2) . ? C4 N2 1.4306(18) . ? N3 N2 1.2512(19) . ? N3 C7 1.4257(18) . ? C10 C9 1.391(2) . ? C10 C11 1.393(2) . ? C10 N1 1.4374(18) 2_566 ? C7 C12 1.390(2) . ? C7 C8 1.397(2) . ? C12 C11 1.387(2) . ? C8 C9 1.379(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 180.000(1) 2_667 . ? O1 Zn1 O1W 89.02(5) 2_667 . ? O1 Zn1 O1W 90.98(5) . . ? O1 Zn1 O1W 90.98(5) 2_667 2_667 ? O1 Zn1 O1W 89.02(5) . 2_667 ? O1W Zn1 O1W 180.00(7) . 2_667 ? O1 Zn1 N1 91.36(5) 2_667 2_667 ? O1 Zn1 N1 88.64(5) . 2_667 ? O1W Zn1 N1 90.37(6) . 2_667 ? O1W Zn1 N1 89.63(6) 2_667 2_667 ? O1 Zn1 N1 88.64(5) 2_667 . ? O1 Zn1 N1 91.36(5) . . ? O1W Zn1 N1 89.63(6) . . ? O1W Zn1 N1 90.37(6) 2_667 . ? N1 Zn1 N1 180.0 2_667 . ? O3 S1 O2 113.24(8) . . ? O3 S1 O1 112.76(7) . . ? O2 S1 O1 111.15(7) . . ? O3 S1 C1 107.13(7) . . ? O2 S1 C1 106.45(7) . . ? O1 S1 C1 105.52(7) . . ? S1 O1 Zn1 137.29(6) . . ? C10 N1 Zn1 122.22(9) 2_566 . ? C1 C2 C3 119.35(15) . . ? C2 C1 C6 121.30(13) . . ? C2 C1 S1 120.26(11) . . ? C6 C1 S1 118.42(11) . . ? C6 C5 C4 119.56(14) . . ? C3 C4 C5 120.49(13) . . ? C3 C4 N2 116.29(13) . . ? C5 C4 N2 123.21(14) . . ? C5 C6 C1 119.46(14) . . ? C4 C3 C2 119.76(15) . . ? N2 N3 C7 114.22(13) . . ? C9 C10 C11 120.10(13) . . ? C9 C10 N1 119.96(13) . 2_566 ? C11 C10 N1 119.93(13) . 2_566 ? C12 C7 C8 119.88(13) . . ? C12 C7 N3 116.10(13) . . ? C8 C7 N3 124.01(14) . . ? N3 N2 C4 113.35(13) . . ? C7 C12 C11 120.36(14) . . ? C12 C11 C10 119.49(14) . . ? C9 C8 C7 119.76(14) . . ? C8 C9 C10 120.36(14) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.418 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.053 #===end data_Compd3e _database_code_depnum_ccdc_archive 'CCDC 682501' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 Cd N6 O8 S2' _chemical_formula_weight 700.95 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' Cd Cd -0.8075 1.2024 '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' _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 5.9899(15) _cell_length_b 7.103(2) _cell_length_c 15.529(5) _cell_angle_alpha 101.441(6) _cell_angle_beta 99.923(13) _cell_angle_gamma 95.931(9) _cell_volume 631.4(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3625 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 27.47 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 346 _exptl_absorpt_coefficient_mu 1.094 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 0.803 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 4921 _diffrn_reflns_av_R_equivalents 0.0158 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.47 _reflns_number_total 2834 _reflns_number_gt 2708 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef none _refine_ls_number_reflns 3625 _refine_ls_number_parameters 370 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 0.949 _refine_ls_restrained_S_all 0.948 _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 Cd1 Cd 0.5000 0.5000 0.0000 0.01957(11) Uani 1 2 d S . . S1 S 0.32088(9) 0.21808(7) 0.14287(3) 0.02056(13) Uani 1 1 d . . . O1 O 0.0736(3) 0.1801(3) 0.12900(12) 0.0374(4) Uani 1 1 d . . . O1W O 0.7879(3) 0.3005(2) -0.00080(11) 0.0286(3) Uani 1 1 d . . . O2 O 0.4193(3) 0.0592(3) 0.09617(12) 0.0387(4) Uani 1 1 d . . . O3 O 0.4020(3) 0.4028(2) 0.12288(10) 0.0283(3) Uani 1 1 d . . . N1 N 1.2441(3) 0.2382(3) 0.90726(12) 0.0246(4) Uani 1 1 d . . . N2 N 0.8887(3) 0.2474(3) 0.54820(12) 0.0273(4) Uani 1 1 d . . . N3 N 0.6816(3) 0.2637(3) 0.52889(13) 0.0290(4) Uani 1 1 d . . . C1 C 1.1540(3) 0.2443(3) 0.81623(13) 0.0214(4) Uani 1 1 d . . . C2 C 0.9458(4) 0.3122(3) 0.79548(14) 0.0255(4) Uani 1 1 d . . . H2A H 0.8664 0.3565 0.8418 0.031 Uiso 1 1 calc R . . C3 C 0.8541(4) 0.3157(3) 0.70804(15) 0.0252(4) Uani 1 1 d . . . H3A H 0.7115 0.3614 0.6943 0.030 Uiso 1 1 calc R . . C4 C 0.9703(4) 0.2524(3) 0.64005(14) 0.0238(4) Uani 1 1 d . . . C5 C 1.1844(4) 0.1930(3) 0.66147(15) 0.0277(4) Uani 1 1 d . . . H5A H 1.2682 0.1561 0.6157 0.033 Uiso 1 1 calc R . . C6 C 1.2748(4) 0.1876(3) 0.74889(15) 0.0265(4) Uani 1 1 d . . . H6A H 1.4193 0.1452 0.7630 0.032 Uiso 1 1 calc R . . C7 C 0.6047(4) 0.2623(3) 0.43668(14) 0.0250(4) Uani 1 1 d . . . C8 C 0.3692(4) 0.2072(4) 0.40356(15) 0.0295(5) Uani 1 1 d . . . H8A H 0.2701 0.1794 0.4424 0.035 Uiso 1 1 calc R . . C9 C 0.2817(4) 0.1936(4) 0.31310(15) 0.0272(4) Uani 1 1 d . . . H9A H 0.1236 0.1508 0.2891 0.033 Uiso 1 1 calc R . . C10 C 0.4272(4) 0.2430(3) 0.25850(13) 0.0205(4) Uani 1 1 d . . . C11 C 0.6586(4) 0.3058(3) 0.29229(15) 0.0271(4) Uani 1 1 d . . . H11A H 0.7558 0.3420 0.2542 0.032 Uiso 1 1 calc R . . C12 C 0.7467(4) 0.3154(3) 0.38120(15) 0.0277(5) Uani 1 1 d . . . H12A H 0.9051 0.3584 0.4046 0.033 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 Cd1 0.02274(15) 0.02065(14) 0.01431(14) 0.00447(9) 0.00095(9) 0.00189(9) S1 0.0250(3) 0.0212(3) 0.0142(2) 0.00528(19) -0.00072(19) 0.0028(2) O1 0.0246(8) 0.0556(12) 0.0303(9) 0.0199(8) -0.0062(7) -0.0028(8) O1W 0.0269(8) 0.0312(8) 0.0282(8) 0.0089(7) 0.0015(6) 0.0090(6) O2 0.0542(12) 0.0293(9) 0.0275(9) -0.0025(7) 0.0011(8) 0.0119(8) O3 0.0409(9) 0.0264(8) 0.0206(7) 0.0110(6) 0.0087(7) 0.0032(7) N1 0.0275(9) 0.0255(9) 0.0173(8) 0.0065(7) -0.0030(7) -0.0023(7) N2 0.0308(10) 0.0301(9) 0.0193(9) 0.0068(7) -0.0003(7) 0.0026(8) N3 0.0296(10) 0.0359(10) 0.0200(9) 0.0086(8) -0.0013(7) 0.0032(8) C1 0.0228(10) 0.0195(9) 0.0182(9) 0.0040(7) -0.0032(7) -0.0006(7) C2 0.0251(10) 0.0293(11) 0.0211(10) 0.0032(8) 0.0036(8) 0.0062(8) C3 0.0213(10) 0.0289(10) 0.0242(10) 0.0065(8) -0.0001(8) 0.0053(8) C4 0.0266(10) 0.0240(10) 0.0191(9) 0.0057(8) -0.0001(8) 0.0015(8) C5 0.0285(11) 0.0330(11) 0.0218(10) 0.0036(9) 0.0060(8) 0.0079(9) C6 0.0235(10) 0.0291(11) 0.0253(11) 0.0053(8) -0.0005(8) 0.0066(8) C7 0.0288(11) 0.0255(10) 0.0192(10) 0.0061(8) -0.0007(8) 0.0032(8) C8 0.0272(11) 0.0411(13) 0.0218(11) 0.0119(9) 0.0053(9) 0.0014(9) C9 0.0223(10) 0.0357(12) 0.0220(10) 0.0089(9) -0.0005(8) 0.0003(9) C10 0.0250(10) 0.0193(9) 0.0163(9) 0.0053(7) -0.0001(7) 0.0032(7) C11 0.0241(11) 0.0327(11) 0.0241(10) 0.0106(9) 0.0027(8) -0.0022(8) C12 0.0215(10) 0.0334(11) 0.0250(11) 0.0094(9) -0.0032(8) -0.0034(8) _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 Cd1 O3 2.2995(16) . ? Cd1 O3 2.2995(16) 2_665 ? Cd1 N1 2.3389(19) 2_766 ? Cd1 N1 2.3389(19) 1_454 ? Cd1 O1W 2.3427(16) . ? Cd1 O1W 2.3427(16) 2_665 ? S1 O1 1.4485(18) . ? S1 O2 1.4514(17) . ? S1 O3 1.4613(16) . ? S1 C10 1.766(2) . ? N1 C1 1.435(3) . ? N1 Cd1 2.3389(18) 1_656 ? N2 N3 1.248(3) . ? N2 C4 1.418(3) . ? N3 C7 1.424(3) . ? C1 C6 1.391(3) . ? C1 C2 1.392(3) . ? C2 C3 1.380(3) . ? C2 H2A 0.9500 . ? C3 C4 1.390(3) . ? C3 H3A 0.9500 . ? C4 C5 1.398(3) . ? C5 C6 1.382(3) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.387(3) . ? C7 C8 1.401(3) . ? C8 C9 1.392(3) . ? C8 H8A 0.9500 . ? C9 C10 1.382(3) . ? C9 H9A 0.9500 . ? C10 C11 1.387(3) . ? C11 C12 1.376(3) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? 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 Cd1 O3 180.00(7) . 2_665 ? O3 Cd1 N1 90.84(6) . 2_766 ? O3 Cd1 N1 89.16(6) 2_665 2_766 ? O3 Cd1 N1 89.16(6) . 1_454 ? O3 Cd1 N1 90.84(6) 2_665 1_454 ? N1 Cd1 N1 180.0 2_766 1_454 ? O3 Cd1 O1W 90.58(6) . . ? O3 Cd1 O1W 89.42(6) 2_665 . ? N1 Cd1 O1W 91.38(6) 2_766 . ? N1 Cd1 O1W 88.62(6) 1_454 . ? O3 Cd1 O1W 89.42(6) . 2_665 ? O3 Cd1 O1W 90.58(6) 2_665 2_665 ? N1 Cd1 O1W 88.62(6) 2_766 2_665 ? N1 Cd1 O1W 91.38(6) 1_454 2_665 ? O1W Cd1 O1W 180.0 . 2_665 ? O1 S1 O2 112.92(12) . . ? O1 S1 O3 112.63(11) . . ? O2 S1 O3 111.60(11) . . ? O1 S1 C10 106.99(10) . . ? O2 S1 C10 106.74(10) . . ? O3 S1 C10 105.37(10) . . ? S1 O3 Cd1 135.57(10) . . ? C1 N1 Cd1 119.83(13) . 1_656 ? N3 N2 C4 114.41(19) . . ? N2 N3 C7 113.43(19) . . ? C6 C1 C2 119.67(19) . . ? C6 C1 N1 120.73(19) . . ? C2 C1 N1 119.59(19) . . ? C3 C2 C1 120.4(2) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 120.05(19) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C3 C4 C5 119.5(2) . . ? C3 C4 N2 124.3(2) . . ? C5 C4 N2 116.24(19) . . ? C6 C5 C4 120.4(2) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C1 119.9(2) . . ? C5 C6 H6A 120.1 . . ? C1 C6 H6A 120.1 . . ? C12 C7 C8 120.2(2) . . ? C12 C7 N3 123.9(2) . . ? C8 C7 N3 115.8(2) . . ? C9 C8 C7 119.4(2) . . ? C9 C8 H8A 120.3 . . ? C7 C8 H8A 120.3 . . ? C10 C9 C8 119.4(2) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 C11 121.1(2) . . ? C9 C10 S1 119.88(16) . . ? C11 C10 S1 118.95(16) . . ? C12 C11 C10 119.7(2) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C7 120.1(2) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.733 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.078 #===end data_Compd3f _database_code_depnum_ccdc_archive 'CCDC 682502' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H24 N6 O8 Pb S2' _chemical_formula_weight 795.74 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' Pb Pb -3.3944 10.1111 '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' _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 6.0295(16) _cell_length_b 7.2837(19) _cell_length_c 15.683(5) _cell_angle_alpha 101.514(8) _cell_angle_beta 100.351(15) _cell_angle_gamma 94.611(12) _cell_volume 659.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 3763 _cell_measurement_theta_min 3.96 _cell_measurement_theta_max 27.480 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.985 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 6.620 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.223 _exptl_absorpt_correction_T_max 0.266 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 5082 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2933 _reflns_number_gt 2679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2933 _refine_ls_number_parameters 187 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0676 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Pb1 Pb 0.5000 1.0000 1.0000 0.04043(10) Uani 1 2 d S . . S1 S 0.16442(15) 0.58627(12) 0.84922(6) 0.03212(18) Uani 1 1 d . . . O1 O 0.2624(5) 0.7836(4) 0.8670(2) 0.0472(7) Uani 1 1 d . . . O1W O 0.1891(6) 1.2222(5) 0.9954(2) 0.0601(9) Uani 1 1 d . . . O2 O 0.3125(7) 0.4815(6) 0.8997(2) 0.0603(9) Uani 1 1 d . . . O3 O -0.0673(5) 0.5664(5) 0.8607(2) 0.0515(8) Uani 1 1 d . . . N1 N 0.3507(6) -0.1958(5) 0.1101(2) 0.0425(8) Uani 1 1 d . . . N2 N 0.3443(5) 0.2035(4) 0.4553(2) 0.0322(6) Uani 1 1 d . . . N3 N 0.1546(5) 0.2364(5) 0.4722(2) 0.0337(6) Uani 1 1 d . . . C1 C 0.3490(6) -0.0914(5) 0.1967(2) 0.0306(7) Uani 1 1 d . . . C2 C 0.1589(6) -0.0036(6) 0.2126(3) 0.0357(7) Uani 1 1 d . . . H2A H 0.0334 -0.0116 0.1652 0.043 Uiso 1 1 calc R . . C3 C 0.1517(6) 0.0950(5) 0.2968(3) 0.0327(7) Uani 1 1 d . . . H3A H 0.0205 0.1524 0.3076 0.039 Uiso 1 1 calc R . . C4 C 0.3379(6) 0.1098(5) 0.3659(2) 0.0282(6) Uani 1 1 d . . . C5 C 0.5322(6) 0.0304(5) 0.3489(3) 0.0343(7) Uani 1 1 d . . . H5A H 0.6618 0.0458 0.3954 0.041 Uiso 1 1 calc R . . C6 C 0.5377(6) -0.0704(5) 0.2652(3) 0.0330(7) Uani 1 1 d . . . H6A H 0.6703 -0.1254 0.2542 0.040 Uiso 1 1 calc R . . C7 C 0.1648(6) 0.3316(5) 0.5618(2) 0.0303(7) Uani 1 1 d . . . C8 C -0.0327(6) 0.3101(6) 0.5943(3) 0.0370(8) Uani 1 1 d . . . H8A H -0.1667 0.2411 0.5563 0.044 Uiso 1 1 calc R . . C9 C -0.0348(6) 0.3892(5) 0.6822(3) 0.0333(7) Uani 1 1 d . . . H9A H -0.1684 0.3718 0.7052 0.040 Uiso 1 1 calc R . . C10 C 0.1603(6) 0.4941(4) 0.7360(2) 0.0284(6) Uani 1 1 d . . . C11 C 0.3567(6) 0.5240(5) 0.7030(3) 0.0340(7) Uani 1 1 d . . . H11A H 0.4875 0.6001 0.7399 0.041 Uiso 1 1 calc R . . C12 C 0.3591(6) 0.4418(5) 0.6160(3) 0.0336(7) Uani 1 1 d . . . H12A H 0.4926 0.4600 0.5929 0.040 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 Pb1 0.05986(15) 0.03395(12) 0.02184(12) 0.00860(7) -0.00478(8) -0.00463(8) S1 0.0406(4) 0.0353(4) 0.0202(4) 0.0053(3) 0.0049(3) 0.0073(3) O1 0.0565(16) 0.0425(15) 0.0340(16) -0.0017(12) 0.0016(13) -0.0033(13) O1W 0.071(2) 0.065(2) 0.0375(18) -0.0062(15) 0.0187(16) -0.0069(17) O2 0.084(2) 0.075(2) 0.0320(17) 0.0255(16) 0.0118(16) 0.038(2) O3 0.0514(16) 0.0645(19) 0.0355(17) -0.0024(14) 0.0190(14) -0.0017(14) N1 0.0500(18) 0.0441(17) 0.0298(18) -0.0029(14) 0.0137(14) -0.0004(14) N2 0.0390(15) 0.0345(14) 0.0240(15) 0.0089(11) 0.0064(12) 0.0034(12) N3 0.0370(15) 0.0390(15) 0.0242(15) 0.0048(12) 0.0069(12) 0.0021(12) C1 0.0366(16) 0.0288(14) 0.0274(17) 0.0067(13) 0.0106(14) -0.0005(13) C2 0.0343(17) 0.0451(19) 0.0255(18) 0.0067(15) 0.0008(14) 0.0057(14) C3 0.0330(16) 0.0361(16) 0.0295(18) 0.0075(14) 0.0058(14) 0.0059(13) C4 0.0340(16) 0.0294(14) 0.0216(16) 0.0083(12) 0.0046(13) 0.0023(12) C5 0.0336(16) 0.0395(17) 0.0306(19) 0.0118(14) 0.0027(14) 0.0063(14) C6 0.0323(16) 0.0358(16) 0.0339(19) 0.0107(14) 0.0093(14) 0.0078(13) C7 0.0386(17) 0.0304(15) 0.0226(16) 0.0084(13) 0.0054(14) 0.0036(13) C8 0.0321(16) 0.0460(19) 0.0274(19) 0.0018(15) 0.0027(14) -0.0040(14) C9 0.0317(16) 0.0405(17) 0.0265(18) 0.0063(14) 0.0059(14) -0.0006(14) C10 0.0379(16) 0.0270(14) 0.0211(16) 0.0080(12) 0.0048(13) 0.0052(12) C11 0.0350(16) 0.0345(16) 0.0286(18) 0.0033(14) 0.0041(14) -0.0052(13) C12 0.0353(16) 0.0363(16) 0.0292(18) 0.0072(14) 0.0095(14) -0.0020(14) _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 Pb1 O1 2.478(3) . ? Pb1 O1 2.478(3) 2_677 ? Pb1 O1W 2.574(4) 2_677 ? Pb1 O1W 2.574(4) . ? Pb1 N1 2.676(4) 2_666 ? Pb1 N1 2.676(4) 1_566 ? S1 O3 1.440(3) . ? S1 O2 1.450(3) . ? S1 O1 1.462(3) . ? S1 C10 1.764(4) . ? N1 C1 1.420(5) . ? N1 Pb1 2.676(4) 1_544 ? N2 N3 1.251(4) . ? N2 C4 1.423(4) . ? N3 C7 1.425(5) . ? C1 C6 1.393(5) . ? C1 C2 1.393(5) . ? C2 C3 1.382(5) . ? C2 H2A 0.9500 . ? C3 C4 1.393(5) . ? C3 H3A 0.9500 . ? C4 C5 1.392(5) . ? C5 C6 1.379(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.387(5) . ? C7 C12 1.400(5) . ? C8 C9 1.386(5) . ? C8 H8A 0.9500 . ? C9 C10 1.385(5) . ? C9 H9A 0.9500 . ? C10 C11 1.394(5) . ? C11 C12 1.379(5) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? 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 O1 Pb1 O1 180.000(1) . 2_677 ? O1 Pb1 O1W 91.47(11) . 2_677 ? O1 Pb1 O1W 88.53(11) 2_677 2_677 ? O1 Pb1 O1W 88.53(11) . . ? O1 Pb1 O1W 91.47(11) 2_677 . ? O1W Pb1 O1W 180.00(17) 2_677 . ? O1 Pb1 N1 87.53(11) . 2_666 ? O1 Pb1 N1 92.47(11) 2_677 2_666 ? O1W Pb1 N1 97.11(12) 2_677 2_666 ? O1W Pb1 N1 82.89(12) . 2_666 ? O1 Pb1 N1 92.47(11) . 1_566 ? O1 Pb1 N1 87.53(11) 2_677 1_566 ? O1W Pb1 N1 82.89(12) 2_677 1_566 ? O1W Pb1 N1 97.11(12) . 1_566 ? N1 Pb1 N1 180.000(1) 2_666 1_566 ? O3 S1 O2 114.0(2) . . ? O3 S1 O1 112.6(2) . . ? O2 S1 O1 110.1(2) . . ? O3 S1 C10 106.82(18) . . ? O2 S1 C10 106.95(18) . . ? O1 S1 C10 105.83(18) . . ? S1 O1 Pb1 133.1(2) . . ? C1 N1 Pb1 116.1(2) . 1_544 ? N3 N2 C4 114.5(3) . . ? N2 N3 C7 113.6(3) . . ? C6 C1 C2 119.6(3) . . ? C6 C1 N1 120.8(3) . . ? C2 C1 N1 119.6(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C2 C3 C4 119.7(3) . . ? C2 C3 H3A 120.2 . . ? C4 C3 H3A 120.2 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 N2 116.3(3) . . ? C3 C4 N2 123.9(3) . . ? C6 C5 C4 120.4(3) . . ? C6 C5 H5A 119.8 . . ? C4 C5 H5A 119.8 . . ? C5 C6 C1 120.0(3) . . ? C5 C6 H6A 120.0 . . ? C1 C6 H6A 120.0 . . ? C8 C7 C12 120.2(3) . . ? C8 C7 N3 116.1(3) . . ? C12 C7 N3 123.7(3) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 121.2(3) . . ? C9 C10 S1 119.7(3) . . ? C11 C10 S1 119.0(3) . . ? C12 C11 C10 119.2(3) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C7 119.9(3) . . ? C11 C12 H12A 120.0 . . ? C7 C12 H12A 120.0 . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.062 _refine_diff_density_min -2.387 _refine_diff_density_rms 0.119 #===end data_Compd4 _database_code_depnum_ccdc_archive 'CCDC 682503' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Ag N3 O3 S' _chemical_formula_weight 384.16 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' Ag Ag -0.8971 1.1015 '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 14.813(5) _cell_length_b 9.088(3) _cell_length_c 9.457(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.837(5) _cell_angle_gamma 90.00 _cell_volume 1271.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2886 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.48 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.759 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.662 _exptl_absorpt_correction_T_max 0.703 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 9617 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2886 _reflns_number_gt 2467 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 2886 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 0.789 _refine_ls_restrained_S_all 0.789 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.478601(13) 0.20471(2) 0.10153(2) 0.04097(12) Uani 1 1 d . . . S1 S 0.39050(4) -0.11598(6) 0.15019(6) 0.02635(15) Uani 1 1 d . . . C1 C 0.27491(15) -0.1123(2) 0.1863(2) 0.0269(4) Uani 1 1 d . . . C6 C 0.24530(18) -0.1805(3) 0.3083(3) 0.0350(5) Uani 1 1 d . . . C2 C 0.21473(17) -0.0367(3) 0.0969(3) 0.0351(5) Uani 1 1 d . . . O1 O 0.43428(13) -0.0064(2) 0.24389(19) 0.0390(4) Uani 1 1 d . . . N3 N -0.02571(14) -0.1351(2) 0.3813(2) 0.0345(4) Uani 1 1 d . . . C7 C -0.12044(16) -0.1196(3) 0.3968(3) 0.0306(5) Uani 1 1 d . . . C4 C 0.09408(16) -0.1002(3) 0.2467(3) 0.0325(5) Uani 1 1 d . . . C8 C -0.17854(17) -0.0512(3) 0.2981(3) 0.0334(5) Uani 1 1 d . . . N2 N -0.00052(14) -0.0866(3) 0.2659(2) 0.0383(5) Uani 1 1 d . . . C10 C -0.30353(16) -0.1010(2) 0.4424(2) 0.0270(5) Uani 1 1 d . . . C3 C 0.12392(18) -0.0313(3) 0.1269(3) 0.0384(6) Uani 1 1 d . . . C12 C -0.15417(19) -0.1764(3) 0.5201(3) 0.0352(5) Uani 1 1 d . . . C11 C -0.24574(18) -0.1677(3) 0.5426(3) 0.0329(5) Uani 1 1 d . . . C9 C -0.26980(17) -0.0423(3) 0.3195(3) 0.0339(5) Uani 1 1 d . . . C5 C 0.15478(19) -0.1746(3) 0.3384(3) 0.0365(6) Uani 1 1 d . . . N1 N -0.39838(14) -0.0927(2) 0.4627(2) 0.0315(4) Uani 1 1 d . . . O3 O 0.42349(13) -0.2640(2) 0.1809(2) 0.0397(4) Uani 1 1 d . . . O2 O 0.39646(12) -0.0754(2) 0.00202(18) 0.0403(4) Uani 1 1 d . . . H11A H -0.271(2) -0.204(3) 0.632(3) 0.036(8) Uiso 1 1 d . . . H12A H -0.122(2) -0.218(3) 0.578(3) 0.033(8) Uiso 1 1 d . . . H2A H 0.235(2) 0.030(3) 0.022(4) 0.052(9) Uiso 1 1 d . . . H5A H 0.132(3) -0.210(3) 0.417(4) 0.059(12) Uiso 1 1 d . . . H8A H -0.158(2) -0.017(3) 0.222(3) 0.039(8) Uiso 1 1 d . . . H6A H 0.285(2) -0.228(3) 0.368(3) 0.039(8) Uiso 1 1 d . . . H1B H -0.422(2) -0.030(3) 0.404(4) 0.044(8) Uiso 1 1 d . . . H1A H -0.403(3) -0.092(4) 0.559(4) 0.064(11) Uiso 1 1 d . . . H9A H -0.309(3) -0.009(3) 0.241(4) 0.053(9) Uiso 1 1 d . . . H3A H 0.074(3) 0.025(4) 0.066(4) 0.058(10) Uiso 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 Ag1 0.02958(16) 0.04419(17) 0.04926(17) 0.00619(8) 0.00308(10) 0.00383(8) S1 0.0180(3) 0.0324(3) 0.0288(3) -0.0008(2) 0.0035(2) -0.0011(2) C1 0.0210(11) 0.0293(11) 0.0307(10) -0.0018(8) 0.0053(8) -0.0007(8) C6 0.0247(13) 0.0409(13) 0.0396(13) 0.0109(10) 0.0040(10) 0.0060(10) C2 0.0249(12) 0.0473(14) 0.0334(11) 0.0084(10) 0.0050(9) 0.0032(10) O1 0.0318(9) 0.0464(10) 0.0391(9) -0.0077(8) 0.0045(7) -0.0112(8) N3 0.0222(10) 0.0401(11) 0.0418(11) 0.0001(9) 0.0067(8) 0.0020(9) C7 0.0220(11) 0.0314(11) 0.0386(12) -0.0035(9) 0.0053(9) -0.0005(9) C4 0.0209(11) 0.0366(12) 0.0404(12) -0.0015(10) 0.0061(9) 0.0002(9) C8 0.0265(12) 0.0419(13) 0.0327(11) 0.0048(10) 0.0096(9) 0.0033(10) N2 0.0219(11) 0.0477(11) 0.0458(12) 0.0023(10) 0.0069(9) 0.0025(9) C10 0.0230(11) 0.0265(10) 0.0320(11) -0.0052(8) 0.0066(8) 0.0004(8) C3 0.0240(12) 0.0536(16) 0.0377(12) 0.0094(11) 0.0039(10) 0.0054(11) C12 0.0272(13) 0.0404(13) 0.0377(13) 0.0058(11) 0.0012(11) 0.0040(11) C11 0.0265(12) 0.0385(12) 0.0343(11) 0.0052(10) 0.0075(9) 0.0013(10) C9 0.0244(12) 0.0420(13) 0.0355(12) 0.0063(10) 0.0039(9) 0.0054(10) C5 0.0287(13) 0.0405(13) 0.0417(13) 0.0109(11) 0.0141(11) 0.0044(11) N1 0.0206(10) 0.0381(11) 0.0364(11) 0.0012(9) 0.0065(8) 0.0017(8) O3 0.0297(10) 0.0354(9) 0.0544(11) 0.0005(8) 0.0052(8) 0.0073(8) O2 0.0272(9) 0.0640(11) 0.0303(8) 0.0056(8) 0.0074(7) 0.0035(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.259(2) 2 ? Ag1 O2 2.4383(19) 3_655 ? Ag1 O1 2.452(2) . ? Ag1 O3 2.474(2) 2_655 ? S1 O3 1.455(2) . ? S1 O2 1.4560(18) . ? S1 O1 1.4632(19) . ? S1 C1 1.763(2) . ? C1 C2 1.381(3) . ? C1 C6 1.399(3) . ? C6 C5 1.385(4) . ? C2 C3 1.389(3) . ? N3 N2 1.250(3) . ? N3 C7 1.425(3) . ? C7 C12 1.390(4) . ? C7 C8 1.385(4) . ? C4 C3 1.386(3) . ? C4 C5 1.393(4) . ? C4 N2 1.427(3) . ? C8 C9 1.379(3) . ? C10 C11 1.385(4) . ? C10 C9 1.394(3) . ? C10 N1 1.430(3) . ? C12 C11 1.386(4) . ? N1 Ag1 2.259(2) 2_545 ? O3 Ag1 2.474(2) 2_645 ? O2 Ag1 2.4383(19) 3_655 ? 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 Ag1 O2 133.22(7) 2 3_655 ? N1 Ag1 O1 129.35(7) 2 . ? O2 Ag1 O1 94.16(7) 3_655 . ? N1 Ag1 O3 114.13(8) 2 2_655 ? O2 Ag1 O3 87.94(7) 3_655 2_655 ? O1 Ag1 O3 78.19(6) . 2_655 ? O3 S1 O2 113.00(12) . . ? O3 S1 O1 111.94(12) . . ? O2 S1 O1 111.36(12) . . ? O3 S1 C1 107.37(11) . . ? O2 S1 C1 106.71(11) . . ? O1 S1 C1 105.98(11) . . ? C2 C1 C6 120.4(2) . . ? C2 C1 S1 119.62(17) . . ? C6 C1 S1 119.91(19) . . ? C5 C6 C1 119.9(2) . . ? C1 C2 C3 119.6(2) . . ? S1 O1 Ag1 108.83(10) . . ? N2 N3 C7 113.1(2) . . ? C12 C7 C8 119.6(2) . . ? C12 C7 N3 116.5(2) . . ? C8 C7 N3 123.9(2) . . ? C3 C4 C5 120.4(2) . . ? C3 C4 N2 114.8(2) . . ? C5 C4 N2 124.8(2) . . ? C7 C8 C9 120.6(2) . . ? N3 N2 C4 114.7(2) . . ? C11 C10 C9 120.2(2) . . ? C11 C10 N1 120.6(2) . . ? C9 C10 N1 119.1(2) . . ? C4 C3 C2 120.1(2) . . ? C7 C12 C11 120.2(2) . . ? C10 C11 C12 119.8(2) . . ? C10 C9 C8 119.6(2) . . ? C6 C5 C4 119.5(2) . . ? C10 N1 Ag1 115.35(14) . 2_545 ? S1 O3 Ag1 116.72(11) . 2_645 ? S1 O2 Ag1 110.35(11) . 3_655 ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.520 _refine_diff_density_min -0.686 _refine_diff_density_rms 0.072 #===end data_Compd5a _database_code_depnum_ccdc_archive 'CCDC 682504' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 Gd N13 O13 S3' _chemical_formula_weight 1418.48 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.812(8) _cell_length_b 11.0386(17) _cell_length_c 30.430(6) _cell_angle_alpha 90.00 _cell_angle_beta 117.098(2) _cell_angle_gamma 90.00 _cell_volume 11905(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 13548 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.46 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.567 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5656 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.740 _exptl_absorpt_correction_T_max 0.772 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 44206 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0392 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 51 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.46 _reflns_number_total 13548 _reflns_number_gt 11553 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 13548 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.251 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.155335(5) -0.693973(16) 0.163994(6) 0.03795(9) Uani 1 1 d . . . S2 S 0.19978(3) -0.41424(9) 0.24017(4) 0.0483(2) Uani 1 1 d . . . S3 S 0.10662(3) -0.44251(11) 0.07694(5) 0.0582(3) Uani 1 1 d . . . S1 S 0.07811(3) -0.92302(10) 0.12456(4) 0.0539(3) Uani 1 1 d . . . O6 O 0.20213(13) -0.3102(3) 0.21383(18) 0.0718(11) Uani 1 1 d . . . O4 O 0.18176(9) -0.5151(3) 0.20661(13) 0.0623(8) Uani 1 1 d . . . O1 O 0.11252(9) -0.8509(3) 0.13764(13) 0.0578(8) Uani 1 1 d . . . O1W O 0.19020(8) -0.8829(3) 0.18096(13) 0.0592(8) Uani 1 1 d . . . N11 N 0.21884(11) -0.6601(3) 0.16146(15) 0.0513(8) Uani 1 1 d . . . O3 O 0.08305(11) -1.0449(3) 0.11158(15) 0.0750(10) Uani 1 1 d . . . O5 O 0.23566(9) -0.4487(3) 0.28024(14) 0.0661(9) Uani 1 1 d . . . O9 O 0.06875(10) -0.4553(4) 0.03751(16) 0.0896(13) Uani 1 1 d . . . O8 O 0.11313(13) -0.3359(4) 0.1072(2) 0.0839(12) Uani 1 1 d . . . O7 O 0.11776(10) -0.5548(3) 0.10674(13) 0.0639(8) Uani 1 1 d . . . C48 C 0.22093(15) -0.6819(4) 0.1196(2) 0.0548(11) Uani 1 1 d . . . N12 N 0.17714(10) -0.7349(4) 0.25446(14) 0.0525(8) Uani 1 1 d . . . N13 N 0.10779(10) -0.6366(3) 0.19649(15) 0.0525(8) Uani 1 1 d . . . C59 C 0.15538(13) -0.7050(3) 0.27584(18) 0.0501(10) Uani 1 1 d . . . C22 C 0.16982(12) -0.3801(4) 0.26713(18) 0.0526(10) Uani 1 1 d . . . N9 N 0.20993(13) -0.4321(4) -0.01762(16) 0.0677(11) Uani 1 1 d . . . C46 C 0.24996(12) -0.6209(4) 0.2001(2) 0.0599(11) Uani 1 1 d . . . H46A H 0.2489 -0.6079 0.2296 0.072 Uiso 1 1 calc R . . C11 C 0.04420(12) -0.8816(5) 0.1838(2) 0.0615(12) Uani 1 1 d . . . H11A H 0.0246 -0.8465 0.1563 0.074 Uiso 1 1 calc R . . C60 C 0.11892(12) -0.6559(4) 0.24703(18) 0.0505(10) Uani 1 1 d . . . C10 C 0.07488(12) -0.9321(4) 0.18016(18) 0.0537(10) Uani 1 1 d . . . O2 O 0.04507(10) -0.8615(5) 0.08895(15) 0.0883(12) Uani 1 1 d . . . N8 N 0.24400(13) -0.4127(4) 0.01189(17) 0.0689(11) Uani 1 1 d . . . C1 C 0.05023(16) -0.8359(6) 0.4600(2) 0.0751(15) Uani 1 1 d . . . N2 N 0.05566(11) -0.8544(4) 0.32474(17) 0.0649(10) Uani 1 1 d . . . N10 N 0.15589(12) -0.7450(4) 0.08264(14) 0.0592(9) Uani 1 1 d . . . C45 C 0.28399(14) -0.5981(4) 0.1989(2) 0.0682(13) Uani 1 1 d . . . H45A H 0.3049 -0.5710 0.2269 0.082 Uiso 1 1 calc R . . C21 C 0.18195(15) -0.4020(5) 0.3168(2) 0.0657(13) Uani 1 1 d . . . H21A H 0.2062 -0.4317 0.3356 0.079 Uiso 1 1 calc R . . C23 C 0.13417(14) -0.3347(4) 0.2387(2) 0.0649(13) Uani 1 1 d . . . H23A H 0.1257 -0.3185 0.2053 0.078 Uiso 1 1 calc R . . C12 C 0.04289(13) -0.8837(5) 0.2281(2) 0.0644(12) Uani 1 1 d . . . H12A H 0.0228 -0.8469 0.2306 0.077 Uiso 1 1 calc R . . N3 N 0.07213(12) -0.9441(4) 0.31683(17) 0.0654(10) Uani 1 1 d . . . C43 C 0.25420(16) -0.6597(5) 0.1143(2) 0.0681(14) Uani 1 1 d . . . C47 C 0.18767(15) -0.7251(4) 0.07765(19) 0.0577(11) Uani 1 1 d . . . C6 C 0.04477(17) -0.7351(6) 0.4300(2) 0.0777(16) Uani 1 1 d . . . H6A H 0.0397 -0.6603 0.4397 0.093 Uiso 1 1 calc R . . C16 C 0.04921(17) -0.2931(5) 0.3417(2) 0.0727(15) Uani 1 1 d . . . C4 C 0.05490(13) -0.8559(5) 0.3704(2) 0.0612(12) Uani 1 1 d . . . N1 N 0.05034(19) -0.8271(6) 0.5043(2) 0.1005(19) Uani 1 1 d . . . C34 C 0.13707(13) -0.4358(4) 0.04852(18) 0.0572(11) Uani 1 1 d . . . N5 N 0.07268(17) -0.2910(5) 0.3142(2) 0.0979(19) Uani 1 1 d . . . C7 C 0.07090(13) -0.9399(4) 0.26903(19) 0.0590(11) Uani 1 1 d . . . C55 C 0.09566(15) -0.6240(5) 0.2686(2) 0.0635(12) Uani 1 1 d . . . C44 C 0.28591(15) -0.6160(5) 0.1565(2) 0.0742(15) Uani 1 1 d . . . H44A H 0.3082 -0.5995 0.1549 0.089 Uiso 1 1 calc R . . C5 C 0.04685(16) -0.7451(6) 0.3858(3) 0.0757(15) Uani 1 1 d . . . H5A H 0.0428 -0.6768 0.3661 0.091 Uiso 1 1 calc R . . C28 C 0.26953(15) -0.4174(4) -0.0088(2) 0.0627(12) Uani 1 1 d . . . C9 C 0.10288(14) -0.9904(5) 0.2209(2) 0.0667(13) Uani 1 1 d . . . H9A H 0.1231 -1.0264 0.2185 0.080 Uiso 1 1 calc R . . C58 C 0.07410(13) -0.5895(4) 0.1688(2) 0.0646(12) Uani 1 1 d . . . H58A H 0.0664 -0.5782 0.1353 0.078 Uiso 1 1 calc R . . C3 C 0.05884(17) -0.9572(6) 0.3990(2) 0.0805(16) Uani 1 1 d . . . H3A H 0.0631 -1.0320 0.3884 0.097 Uiso 1 1 calc R . . C49 C 0.21177(16) -0.7722(6) 0.2832(2) 0.0700(14) Uani 1 1 d . . . H49A H 0.2268 -0.7922 0.2682 0.084 Uiso 1 1 calc R . . C52 C 0.16813(18) -0.7187(5) 0.3280(2) 0.0646(13) Uani 1 1 d . . . C56 C 0.06029(15) -0.5739(5) 0.2377(3) 0.0763(16) Uani 1 1 d . . . H56A H 0.0441 -0.5530 0.2509 0.092 Uiso 1 1 calc R . . C30 C 0.28842(19) -0.4436(6) -0.0722(2) 0.0779(16) Uani 1 1 d . . . H30A H 0.2821 -0.4631 -0.1047 0.093 Uiso 1 1 calc R . . C2 C 0.05658(18) -0.9507(6) 0.4430(2) 0.0849(17) Uani 1 1 d . . . H2A H 0.0592 -1.0204 0.4614 0.102 Uiso 1 1 calc R . . C29 C 0.26059(16) -0.4459(5) -0.0569(2) 0.0715(13) Uani 1 1 d . . . H29A H 0.2360 -0.4666 -0.0791 0.086 Uiso 1 1 calc R . . C31 C 0.18635(14) -0.4302(5) 0.00632(19) 0.0636(12) Uani 1 1 d . . . C25 C 0.32529(17) -0.4132(5) -0.0404(2) 0.0714(14) Uani 1 1 d . . . N7 N 0.35274(16) -0.4093(5) -0.0566(2) 0.0971(17) Uani 1 1 d . . . C24 C 0.11068(17) -0.3136(4) 0.2616(3) 0.084(2) Uani 1 1 d . . . H24A H 0.0865 -0.2826 0.2435 0.101 Uiso 1 1 calc R . . C57 C 0.04921(16) -0.5553(5) 0.1888(3) 0.0772(16) Uani 1 1 d . . . H57A H 0.0258 -0.5209 0.1688 0.093 Uiso 1 1 calc R . . C53 C 0.1443(2) -0.6887(4) 0.3482(2) 0.0716(16) Uani 1 1 d . . . H53A H 0.1526 -0.7003 0.3818 0.086 Uiso 1 1 calc R . . N6 N 0.10181(18) -0.3333(5) 0.3393(2) 0.0885(16) Uani 1 1 d . . . C8 C 0.10092(16) -0.9953(5) 0.2648(2) 0.0716(14) Uani 1 1 d . . . H8A H 0.1196 -1.0354 0.2917 0.086 Uiso 1 1 calc R . . C35 C 0.12433(15) -0.4625(5) -0.0004(2) 0.0715(14) Uani 1 1 d . . . H35A H 0.0991 -0.4825 -0.0196 0.086 Uiso 1 1 calc R . . C51 C 0.20498(19) -0.7591(6) 0.3557(2) 0.0791(16) Uani 1 1 d . . . H51A H 0.2145 -0.7695 0.3896 0.095 Uiso 1 1 calc R . . C54 C 0.10835(19) -0.6419(5) 0.3197(2) 0.0729(15) Uani 1 1 d . . . H54A H 0.0929 -0.6225 0.3342 0.088 Uiso 1 1 calc R . . C36 C 0.14878(16) -0.4601(5) -0.0221(2) 0.0753(15) Uani 1 1 d . . . H36A H 0.1398 -0.4785 -0.0554 0.090 Uiso 1 1 calc R . . C15 C 0.05641(17) -0.3547(7) 0.3845(2) 0.0905(19) Uani 1 1 d . . . H15A H 0.0779 -0.4028 0.3995 0.109 Uiso 1 1 calc R . . C32 C 0.19862(14) -0.4017(5) 0.0553(2) 0.0705(14) Uani 1 1 d . . . H32A H 0.2237 -0.3803 0.0745 0.085 Uiso 1 1 calc R . . C33 C 0.17438(15) -0.4041(5) 0.0767(2) 0.0709(13) Uani 1 1 d . . . H33A H 0.1833 -0.3844 0.1098 0.085 Uiso 1 1 calc R . . C27 C 0.30690(17) -0.3921(6) 0.0238(2) 0.0823(16) Uani 1 1 d . . . H27A H 0.3135 -0.3767 0.0567 0.099 Uiso 1 1 calc R . . C50 C 0.2273(2) -0.7837(6) 0.3336(2) 0.0871(18) Uani 1 1 d . . . H50A H 0.2523 -0.8075 0.3520 0.104 Uiso 1 1 calc R . . C13 C -0.00020(18) -0.2725(7) 0.3844(3) 0.0831(17) Uani 1 1 d . . . C19 C 0.1245(2) -0.3401(5) 0.3118(3) 0.0759(16) Uani 1 1 d . . . C20 C 0.15973(18) -0.3820(6) 0.3389(3) 0.0815(16) Uani 1 1 d . . . H20A H 0.1687 -0.3969 0.3725 0.098 Uiso 1 1 calc R . . C40 C 0.1885(2) -0.7443(6) 0.0320(2) 0.0831(17) Uani 1 1 d . . . C37 C 0.1249(2) -0.7808(5) 0.0437(2) 0.0768(16) Uani 1 1 d . . . H37A H 0.1031 -0.7944 0.0471 0.092 Uiso 1 1 calc R . . C18 C -0.00681(19) -0.2138(6) 0.3419(3) 0.0880(19) Uani 1 1 d . . . H18A H -0.0282 -0.1653 0.3269 0.106 Uiso 1 1 calc R . . C26 C 0.33374(17) -0.3895(6) 0.0084(3) 0.0897(18) Uani 1 1 d . . . H26A H 0.3585 -0.3715 0.0310 0.108 Uiso 1 1 calc R . . C38 C 0.1240(2) -0.7990(5) -0.0031(2) 0.091(2) Uani 1 1 d . . . H38A H 0.1018 -0.8229 -0.0301 0.109 Uiso 1 1 calc R . . C42 C 0.2539(2) -0.6797(7) 0.0689(3) 0.100(2) Uani 1 1 d . . . H42A H 0.2758 -0.6657 0.0658 0.120 Uiso 1 1 calc R . . C14 C 0.03184(19) -0.3455(8) 0.4054(3) 0.100(2) Uani 1 1 d . . . H14A H 0.0369 -0.3890 0.4339 0.120 Uiso 1 1 calc R . . C41 C 0.2226(3) -0.7189(7) 0.0293(3) 0.103(2) Uani 1 1 d . . . H41A H 0.2234 -0.7297 -0.0006 0.124 Uiso 1 1 calc R . . C39 C 0.1557(2) -0.7811(6) -0.0081(3) 0.091(2) Uani 1 1 d . . . H39A H 0.1554 -0.7937 -0.0384 0.110 Uiso 1 1 calc R . . C17 C 0.0169(2) -0.2235(7) 0.3203(3) 0.099(2) Uani 1 1 d . . . H17A H 0.0110 -0.1827 0.2909 0.119 Uiso 1 1 calc R . . N4 N -0.02385(18) -0.2645(7) 0.4051(3) 0.115(2) Uani 1 1 d . . . O2W O 0.16050(10) -0.1069(4) 0.16474(14) 0.0770(11) Uani 1 1 d . . . O3W O 0.0215(2) -0.6621(8) 0.0165(3) 0.193(4) Uani 1 1 d . . . O4W O 0.1442(4) -1.0732(19) 0.3870(6) 0.374(10) 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 Gd1 0.03444(13) 0.03537(13) 0.04320(14) 0.00305(6) 0.01697(10) -0.00002(6) S2 0.0389(5) 0.0390(5) 0.0672(6) -0.0061(4) 0.0242(5) -0.0064(4) S3 0.0460(6) 0.0553(6) 0.0659(7) 0.0222(5) 0.0191(5) 0.0087(5) S1 0.0386(5) 0.0550(6) 0.0644(6) -0.0060(5) 0.0202(5) -0.0087(4) O6 0.078(3) 0.052(2) 0.104(3) 0.0091(17) 0.058(3) -0.0037(15) O4 0.0486(17) 0.0556(18) 0.085(2) -0.0186(17) 0.0318(17) -0.0119(14) O1 0.0480(17) 0.0537(17) 0.076(2) -0.0130(16) 0.0314(16) -0.0168(14) O1W 0.0473(16) 0.0458(16) 0.082(2) 0.0039(16) 0.0278(16) 0.0071(13) N11 0.057(2) 0.0390(17) 0.066(2) 0.0040(16) 0.035(2) 0.0047(15) O3 0.076(2) 0.0573(19) 0.098(3) -0.0252(19) 0.045(2) -0.0243(17) O5 0.0403(16) 0.076(2) 0.073(2) -0.0073(18) 0.0181(16) -0.0024(15) O9 0.0470(19) 0.123(3) 0.082(3) 0.046(2) 0.0147(19) 0.004(2) O8 0.091(3) 0.054(2) 0.119(4) -0.004(2) 0.058(3) 0.002(2) O7 0.066(2) 0.0618(19) 0.0612(19) 0.0199(16) 0.0265(17) 0.0138(15) C48 0.060(3) 0.040(2) 0.078(3) 0.0054(19) 0.043(3) 0.0081(17) N12 0.054(2) 0.052(2) 0.053(2) 0.0091(17) 0.0257(18) 0.0044(17) N13 0.051(2) 0.0445(19) 0.069(2) -0.0033(17) 0.0332(19) -0.0043(15) C59 0.054(2) 0.037(2) 0.060(3) 0.0039(17) 0.026(2) -0.0033(16) C22 0.046(2) 0.0376(19) 0.078(3) -0.006(2) 0.031(2) -0.0077(16) N9 0.066(3) 0.072(3) 0.063(2) -0.001(2) 0.028(2) -0.006(2) C46 0.043(2) 0.054(2) 0.082(3) 0.001(2) 0.028(2) 0.0016(19) C11 0.039(2) 0.069(3) 0.075(3) 0.003(2) 0.025(2) 0.002(2) C60 0.054(2) 0.041(2) 0.069(3) -0.012(2) 0.038(2) -0.0101(18) C10 0.042(2) 0.044(2) 0.071(3) -0.002(2) 0.023(2) -0.0069(16) O2 0.048(2) 0.125(3) 0.081(3) 0.015(3) 0.0198(19) 0.008(2) N8 0.072(3) 0.064(3) 0.069(3) -0.003(2) 0.031(2) -0.006(2) C1 0.057(3) 0.097(4) 0.063(3) -0.017(3) 0.020(3) 0.003(3) N2 0.051(2) 0.066(2) 0.079(3) -0.015(2) 0.031(2) -0.0081(19) N10 0.069(3) 0.051(2) 0.055(2) -0.0032(18) 0.025(2) -0.0078(19) C45 0.049(3) 0.055(3) 0.103(4) 0.003(3) 0.037(3) 0.002(2) C21 0.066(3) 0.060(3) 0.079(3) -0.013(2) 0.039(3) -0.014(2) C23 0.054(3) 0.048(2) 0.096(4) 0.001(3) 0.037(3) -0.002(2) C12 0.046(2) 0.075(3) 0.080(3) -0.003(3) 0.035(2) 0.003(2) N3 0.061(2) 0.060(2) 0.078(3) -0.004(2) 0.034(2) 0.0041(18) C43 0.074(3) 0.054(3) 0.099(4) 0.014(3) 0.060(3) 0.012(2) C47 0.074(3) 0.043(2) 0.072(3) 0.004(2) 0.046(3) 0.005(2) C6 0.070(3) 0.074(3) 0.091(4) -0.026(3) 0.038(3) -0.001(3) C16 0.059(3) 0.085(4) 0.079(4) -0.029(3) 0.035(3) -0.006(2) C4 0.044(2) 0.065(3) 0.072(3) -0.014(3) 0.024(2) -0.005(2) N1 0.102(4) 0.123(5) 0.073(3) -0.027(3) 0.037(3) 0.011(3) C34 0.047(2) 0.053(2) 0.062(3) 0.017(2) 0.016(2) 0.0017(18) N5 0.073(4) 0.081(4) 0.108(5) -0.016(3) 0.014(3) 0.011(3) C7 0.055(3) 0.052(2) 0.075(3) -0.004(2) 0.034(2) -0.0055(19) C55 0.065(3) 0.056(3) 0.084(3) -0.013(2) 0.046(3) -0.011(2) C44 0.057(3) 0.065(3) 0.115(5) 0.007(3) 0.051(3) 0.003(2) C5 0.065(3) 0.068(3) 0.097(4) -0.013(3) 0.039(3) -0.003(3) C28 0.065(3) 0.056(3) 0.070(3) 0.002(2) 0.034(3) -0.001(2) C9 0.052(3) 0.072(3) 0.080(3) 0.010(3) 0.033(3) 0.019(2) C58 0.045(2) 0.061(3) 0.087(4) 0.005(3) 0.029(2) -0.001(2) C3 0.081(4) 0.078(4) 0.086(4) -0.013(3) 0.041(3) 0.012(3) C49 0.066(3) 0.083(3) 0.058(3) 0.015(3) 0.026(3) 0.022(3) C52 0.086(4) 0.053(3) 0.059(3) -0.004(2) 0.037(3) -0.011(2) C56 0.058(3) 0.063(3) 0.121(5) -0.017(3) 0.052(3) -0.007(2) C30 0.092(4) 0.084(4) 0.063(3) 0.010(3) 0.040(3) 0.011(3) C2 0.092(4) 0.084(4) 0.077(4) -0.004(3) 0.037(3) 0.026(3) C29 0.067(3) 0.083(4) 0.060(3) 0.008(3) 0.025(3) 0.002(3) C31 0.063(3) 0.063(3) 0.060(3) 0.001(2) 0.024(2) -0.006(2) C25 0.077(4) 0.060(3) 0.086(4) 0.010(3) 0.046(3) 0.012(2) N7 0.096(4) 0.096(4) 0.120(5) 0.020(3) 0.068(4) 0.014(3) C24 0.049(3) 0.052(3) 0.153(7) -0.011(3) 0.047(4) 0.000(2) C57 0.055(3) 0.065(3) 0.112(5) -0.001(3) 0.039(3) -0.001(2) C53 0.104(5) 0.063(3) 0.061(3) -0.003(2) 0.048(3) -0.010(3) N6 0.097(4) 0.074(3) 0.082(4) -0.016(3) 0.030(3) 0.009(3) C8 0.068(3) 0.070(3) 0.078(3) 0.014(3) 0.034(3) 0.019(3) C35 0.055(3) 0.080(4) 0.064(3) 0.012(3) 0.014(2) -0.007(2) C51 0.094(4) 0.083(4) 0.053(3) 0.014(3) 0.027(3) 0.014(3) C54 0.102(4) 0.062(3) 0.076(3) -0.020(3) 0.059(3) -0.019(3) C36 0.068(3) 0.087(4) 0.055(3) 0.000(3) 0.015(3) -0.016(3) C15 0.060(3) 0.124(5) 0.081(4) -0.010(4) 0.026(3) 0.035(4) C32 0.051(3) 0.079(3) 0.071(3) -0.010(3) 0.020(2) -0.020(2) C33 0.056(3) 0.082(4) 0.064(3) -0.008(3) 0.018(2) -0.010(2) C27 0.074(4) 0.099(4) 0.073(4) -0.020(3) 0.034(3) -0.010(3) C50 0.077(4) 0.114(5) 0.064(3) 0.023(3) 0.026(3) 0.021(3) C13 0.066(4) 0.105(4) 0.080(4) -0.021(4) 0.034(3) 0.015(3) C19 0.092(4) 0.057(3) 0.100(5) -0.022(3) 0.063(4) -0.018(3) C20 0.085(4) 0.080(4) 0.096(4) -0.017(3) 0.055(4) -0.015(3) C40 0.116(5) 0.071(4) 0.084(4) -0.007(3) 0.064(4) 0.008(3) C37 0.097(5) 0.068(3) 0.064(3) -0.007(3) 0.035(3) -0.019(3) C18 0.068(4) 0.100(5) 0.094(5) -0.005(4) 0.036(4) 0.026(3) C26 0.060(3) 0.102(5) 0.098(5) -0.027(4) 0.028(3) -0.004(3) C38 0.114(6) 0.079(4) 0.064(4) -0.019(3) 0.028(4) -0.027(3) C42 0.094(5) 0.124(6) 0.114(6) 0.006(5) 0.075(5) 0.012(4) C14 0.088(5) 0.141(6) 0.080(4) 0.014(4) 0.046(4) 0.050(4) C41 0.116(6) 0.131(6) 0.104(6) -0.014(5) 0.086(5) 0.019(5) C39 0.131(6) 0.081(4) 0.074(4) -0.016(3) 0.057(4) -0.015(4) C17 0.097(5) 0.110(5) 0.102(5) 0.014(4) 0.056(5) 0.028(4) N4 0.095(4) 0.148(5) 0.131(5) 0.002(5) 0.077(4) 0.040(4) O2W 0.064(2) 0.054(2) 0.107(3) 0.0009(17) 0.033(2) -0.0048(15) O3W 0.137(6) 0.245(9) 0.141(6) 0.050(6) 0.016(5) -0.082(6) O4W 0.256(13) 0.62(3) 0.324(16) 0.172(18) 0.201(13) 0.133(17) _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 Gd1 O7 2.293(3) . ? Gd1 O1 2.303(3) . ? Gd1 O4 2.334(3) . ? Gd1 O1W 2.427(3) . ? Gd1 N12 2.522(4) . ? Gd1 N10 2.549(4) . ? Gd1 N13 2.582(3) . ? Gd1 N11 2.591(4) . ? S2 O6 1.428(4) . ? S2 O5 1.444(4) . ? S2 O4 1.459(3) . ? S2 C22 1.769(4) . ? S3 O8 1.444(4) . ? S3 O9 1.444(4) . ? S3 O7 1.480(3) . ? S3 C34 1.783(5) . ? S1 O2 1.438(4) . ? S1 O3 1.441(4) . ? S1 O1 1.474(3) . ? S1 C10 1.757(5) . ? N11 C48 1.336(6) . ? N11 C46 1.333(6) . ? C48 C47 1.439(8) . ? C48 C43 1.426(7) . ? N12 C49 1.318(6) . ? N12 C59 1.340(6) . ? N13 C58 1.323(6) . ? N13 C60 1.409(6) . ? C59 C60 1.418(6) . ? C59 C52 1.436(7) . ? C22 C23 1.377(7) . ? C22 C21 1.382(7) . ? N9 N8 1.258(6) . ? N9 C31 1.427(7) . ? C46 C45 1.395(6) . ? C11 C12 1.372(7) . ? C11 C10 1.392(6) . ? C60 C55 1.401(6) . ? C10 C9 1.392(7) . ? N8 C28 1.418(6) . ? C1 N1 1.349(8) . ? C1 C2 1.435(8) . ? C1 C6 1.392(9) . ? N2 N3 1.270(6) . ? N2 C4 1.403(7) . ? N10 C37 1.323(7) . ? N10 C47 1.359(6) . ? C45 C44 1.339(8) . ? C21 C20 1.352(7) . ? C23 C24 1.417(8) . ? C12 C7 1.384(7) . ? N3 C7 1.434(6) . ? C43 C42 1.396(10) . ? C43 C44 1.415(8) . ? C47 C40 1.421(7) . ? C6 C5 1.391(8) . ? C16 C17 1.381(9) . ? C16 C15 1.379(9) . ? C16 N5 1.510(9) . ? C4 C5 1.398(8) . ? C4 C3 1.382(8) . ? C34 C35 1.368(7) . ? C34 C33 1.380(7) . ? N5 N6 1.157(7) . ? C7 C8 1.399(7) . ? C55 C56 1.403(8) . ? C55 C54 1.415(8) . ? C28 C29 1.378(7) . ? C28 C27 1.389(8) . ? C9 C8 1.373(8) . ? C58 C57 1.429(7) . ? C3 C2 1.383(8) . ? C49 C50 1.372(8) . ? C52 C51 1.391(8) . ? C52 C53 1.386(8) . ? C56 C57 1.360(9) . ? C30 C29 1.383(8) . ? C30 C25 1.382(8) . ? C31 C32 1.376(7) . ? C31 C36 1.384(7) . ? C25 N7 1.389(7) . ? C25 C26 1.389(8) . ? C24 C19 1.399(10) . ? C53 C54 1.392(9) . ? N6 C19 1.487(8) . ? C35 C36 1.403(8) . ? C51 C50 1.366(9) . ? C15 C14 1.392(8) . ? C32 C33 1.389(7) . ? C27 C26 1.348(8) . ? C13 N4 1.352(8) . ? C13 C18 1.361(10) . ? C13 C14 1.394(9) . ? C19 C20 1.344(9) . ? C40 C39 1.381(10) . ? C40 C41 1.426(10) . ? C37 C38 1.424(9) . ? C18 C17 1.378(10) . ? C38 C39 1.351(11) . ? C42 C41 1.350(11) . ? 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 O7 Gd1 O1 96.66(13) . . ? O7 Gd1 O4 80.11(13) . . ? O1 Gd1 O4 154.81(11) . . ? O7 Gd1 O1W 148.13(13) . . ? O1 Gd1 O1W 71.86(12) . . ? O4 Gd1 O1W 122.66(12) . . ? O7 Gd1 N12 136.92(12) . . ? O1 Gd1 N12 94.46(12) . . ? O4 Gd1 N12 72.60(13) . . ? O1W Gd1 N12 74.62(12) . . ? O7 Gd1 N10 72.62(13) . . ? O1 Gd1 N10 80.10(12) . . ? O4 Gd1 N10 121.70(12) . . ? O1W Gd1 N10 76.09(13) . . ? N12 Gd1 N10 150.44(13) . . ? O7 Gd1 N13 77.78(12) . . ? O1 Gd1 N13 76.25(11) . . ? O4 Gd1 N13 78.66(11) . . ? O1W Gd1 N13 125.26(11) . . ? N12 Gd1 N13 64.76(12) . . ? N10 Gd1 N13 139.32(13) . . ? O7 Gd1 N11 100.86(12) . . ? O1 Gd1 N11 132.50(11) . . ? O4 Gd1 N11 72.26(11) . . ? O1W Gd1 N11 70.07(11) . . ? N12 Gd1 N11 101.71(12) . . ? N10 Gd1 N11 64.07(13) . . ? N13 Gd1 N11 150.62(12) . . ? O6 S2 O5 113.2(2) . . ? O6 S2 O4 110.9(2) . . ? O5 S2 O4 111.8(2) . . ? O6 S2 C22 108.6(2) . . ? O5 S2 C22 106.3(2) . . ? O4 S2 C22 105.49(19) . . ? O8 S3 O9 115.2(3) . . ? O8 S3 O7 112.1(3) . . ? O9 S3 O7 109.6(2) . . ? O8 S3 C34 108.1(2) . . ? O9 S3 C34 106.5(2) . . ? O7 S3 C34 104.6(2) . . ? O2 S1 O3 115.3(3) . . ? O2 S1 O1 111.5(2) . . ? O3 S1 O1 110.6(2) . . ? O2 S1 C10 108.0(2) . . ? O3 S1 C10 106.8(2) . . ? O1 S1 C10 103.7(2) . . ? S2 O4 Gd1 171.1(2) . . ? S1 O1 Gd1 161.8(2) . . ? C48 N11 C46 117.5(4) . . ? C48 N11 Gd1 119.2(3) . . ? C46 N11 Gd1 123.3(3) . . ? S3 O7 Gd1 159.5(2) . . ? N11 C48 C47 118.3(4) . . ? N11 C48 C43 122.8(5) . . ? C47 C48 C43 118.9(5) . . ? C49 N12 C59 117.8(4) . . ? C49 N12 Gd1 121.1(3) . . ? C59 N12 Gd1 120.6(3) . . ? C58 N13 C60 118.5(4) . . ? C58 N13 Gd1 124.1(3) . . ? C60 N13 Gd1 117.4(3) . . ? N12 C59 C60 120.0(4) . . ? N12 C59 C52 121.9(5) . . ? C60 C59 C52 118.0(5) . . ? C23 C22 C21 119.9(5) . . ? C23 C22 S2 120.4(4) . . ? C21 C22 S2 119.7(4) . . ? N8 N9 C31 112.3(4) . . ? N11 C46 C45 124.0(5) . . ? C12 C11 C10 119.9(5) . . ? C55 C60 N13 121.8(4) . . ? C55 C60 C59 121.0(5) . . ? N13 C60 C59 117.2(4) . . ? C11 C10 C9 119.3(5) . . ? C11 C10 S1 120.3(4) . . ? C9 C10 S1 120.3(4) . . ? N9 N8 C28 115.8(4) . . ? N1 C1 C2 120.3(6) . . ? N1 C1 C6 121.7(6) . . ? C2 C1 C6 118.0(6) . . ? N3 N2 C4 115.1(5) . . ? C37 N10 C47 119.0(5) . . ? C37 N10 Gd1 121.2(4) . . ? C47 N10 Gd1 119.5(3) . . ? C44 C45 C46 118.7(5) . . ? C20 C21 C22 122.3(6) . . ? C22 C23 C24 118.3(6) . . ? C11 C12 C7 121.1(4) . . ? N2 N3 C7 112.6(4) . . ? C42 C43 C44 123.7(6) . . ? C42 C43 C48 119.8(6) . . ? C44 C43 C48 116.5(5) . . ? N10 C47 C48 118.8(4) . . ? N10 C47 C40 121.5(5) . . ? C48 C47 C40 119.7(5) . . ? C5 C6 C1 120.8(5) . . ? C17 C16 C15 117.9(6) . . ? C17 C16 N5 114.2(6) . . ? C15 C16 N5 127.9(6) . . ? C5 C4 C3 118.3(5) . . ? C5 C4 N2 115.7(6) . . ? C3 C4 N2 125.9(5) . . ? C35 C34 C33 119.4(5) . . ? C35 C34 S3 121.5(4) . . ? C33 C34 S3 119.1(4) . . ? N6 N5 C16 108.5(7) . . ? C12 C7 C8 119.0(5) . . ? C12 C7 N3 124.7(4) . . ? C8 C7 N3 116.3(5) . . ? C60 C55 C56 117.5(5) . . ? C60 C55 C54 119.9(5) . . ? C56 C55 C54 122.6(5) . . ? C45 C44 C43 120.4(5) . . ? C4 C5 C6 121.2(6) . . ? C29 C28 C27 118.5(5) . . ? C29 C28 N8 126.1(5) . . ? C27 C28 N8 115.3(5) . . ? C8 C9 C10 120.5(4) . . ? N13 C58 C57 122.1(5) . . ? C2 C3 C4 121.9(6) . . ? N12 C49 C50 125.0(6) . . ? C51 C52 C53 123.5(5) . . ? C51 C52 C59 116.7(5) . . ? C53 C52 C59 119.8(6) . . ? C57 C56 C55 121.2(5) . . ? C29 C30 C25 121.8(5) . . ? C3 C2 C1 119.7(6) . . ? C30 C29 C28 119.6(5) . . ? C32 C31 C36 118.7(5) . . ? C32 C31 N9 124.3(5) . . ? C36 C31 N9 117.0(5) . . ? N7 C25 C30 121.0(6) . . ? N7 C25 C26 121.8(6) . . ? C30 C25 C26 117.2(5) . . ? C23 C24 C19 118.8(6) . . ? C56 C57 C58 118.9(5) . . ? C54 C53 C52 122.0(5) . . ? N5 N6 C19 109.5(7) . . ? C9 C8 C7 120.1(5) . . ? C34 C35 C36 121.0(5) . . ? C52 C51 C50 120.5(5) . . ? C53 C54 C55 119.1(5) . . ? C31 C36 C35 119.7(5) . . ? C14 C15 C16 120.6(6) . . ? C31 C32 C33 121.6(5) . . ? C34 C33 C32 119.6(5) . . ? C26 C27 C28 121.2(6) . . ? C49 C50 C51 117.9(6) . . ? N4 C13 C18 122.5(6) . . ? N4 C13 C14 120.7(7) . . ? C18 C13 C14 116.8(6) . . ? C20 C19 C24 121.7(6) . . ? C20 C19 N6 113.7(6) . . ? C24 C19 N6 124.5(6) . . ? C19 C20 C21 119.1(6) . . ? C39 C40 C47 118.2(6) . . ? C39 C40 C41 123.4(6) . . ? C47 C40 C41 118.3(7) . . ? N10 C37 C38 121.7(6) . . ? C13 C18 C17 122.6(6) . . ? C27 C26 C25 121.5(6) . . ? C39 C38 C37 119.5(7) . . ? C41 C42 C43 121.5(7) . . ? C15 C14 C13 121.3(7) . . ? C42 C41 C40 121.9(6) . . ? C38 C39 C40 120.0(6) . . ? C16 C17 C18 120.7(7) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.744 _refine_diff_density_min -1.387 _refine_diff_density_rms 0.254 #===end data_Compd5c _database_code_depnum_ccdc_archive 'CCDC 682505' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H54 Ho N13 O13 S3' _chemical_formula_weight 1426.16 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' Ho Ho -0.2175 4.6783 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.773(13) _cell_length_b 10.995(3) _cell_length_c 30.390(10) _cell_angle_alpha 90.00 _cell_angle_beta 117.052(4) _cell_angle_gamma 90.00 _cell_volume 11835(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13404 _cell_measurement_theta_min 2.10 _cell_measurement_theta_max 27.45 _exptl_crystal_description trunk _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5680 _exptl_absorpt_coefficient_mu 1.520 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 173(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 ; Mercury70 (2x2 bin mode) ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 44624 _diffrn_reflns_av_R_equivalents 0.0571 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 27.45 _reflns_number_total 13404 _reflns_number_gt 10718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1227P)^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 none _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 13404 _refine_ls_number_parameters 806 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.2135 _refine_ls_wR_factor_gt 0.1541 _refine_ls_goodness_of_fit_ref 1.169 _refine_ls_restrained_S_all 1.169 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.155825(6) 0.19322(2) 0.663951(9) 0.03406(12) Uani 1 1 d . . . S1 S 0.19933(4) -0.08540(13) 0.73974(6) 0.0427(3) Uani 1 1 d . . . S2 S 0.07864(4) 0.41856(15) 0.62410(6) 0.0470(3) Uani 1 1 d . . . S3 S 0.10722(4) -0.05733(15) 0.57828(6) 0.0499(4) Uani 1 1 d . . . O1W O 0.19000(11) 0.3808(4) 0.67925(17) 0.0486(10) Uani 1 1 d . . . O1 O 0.18120(12) 0.0158(4) 0.70638(18) 0.0535(11) Uani 1 1 d . . . O2 O 0.23536(12) -0.0500(5) 0.78001(18) 0.0556(11) Uani 1 1 d . . . O3 O 0.20156(17) -0.1898(4) 0.7127(2) 0.0632(14) Uani 1 1 d . . . O3W O 0.0203(2) 0.1591(11) 0.5163(3) 0.156(4) Uani 1 1 d . . . O4 O 0.11383(12) 0.3486(4) 0.63786(17) 0.0491(10) Uani 1 1 d . . . O4W O 0.16020(14) 0.6061(5) 0.6650(2) 0.0705(15) Uani 1 1 d . . . O5 O 0.04596(14) 0.3530(6) 0.5890(2) 0.0739(15) Uani 1 1 d . . . O6 O 0.08283(14) 0.5408(5) 0.6101(2) 0.0639(13) Uani 1 1 d . . . O7 O 0.11813(13) 0.0556(4) 0.60766(18) 0.0569(11) Uani 1 1 d . . . O8 O 0.06916(13) -0.0464(6) 0.5395(2) 0.0746(16) Uani 1 1 d . . . O9 O 0.11403(18) -0.1628(5) 0.6089(3) 0.0742(16) Uani 1 1 d . . . N1 N -0.0242(3) -0.2348(11) 0.9063(4) 0.106(3) Uani 1 1 d . . . N2 N 0.0722(2) -0.2089(7) 0.8145(4) 0.089(2) Uani 1 1 d . . . N3 N 0.1013(3) -0.1638(7) 0.8398(3) 0.083(2) Uani 1 1 d . . . N4 N 0.0507(3) 0.3242(8) 1.0043(3) 0.088(2) Uani 1 1 d . . . N5 N 0.05572(16) 0.3553(6) 0.8240(2) 0.0573(14) Uani 1 1 d . . . N6 N 0.07226(16) 0.4455(6) 0.8162(2) 0.0594(14) Uani 1 1 d . . . N7 N 0.3528(2) -0.0900(8) 0.4437(3) 0.089(2) Uani 1 1 d . . . N8 N 0.24406(17) -0.0871(6) 0.5118(2) 0.0621(15) Uani 1 1 d . . . N9 N 0.21012(17) -0.0668(6) 0.4834(2) 0.0603(14) Uani 1 1 d . . . N10 N 0.17767(14) 0.2341(5) 0.75347(19) 0.0451(11) Uani 1 1 d . . . N11 N 0.10831(13) 0.1370(5) 0.69579(19) 0.0441(11) Uani 1 1 d . . . N12 N 0.21855(14) 0.1597(5) 0.6621(2) 0.0459(11) Uani 1 1 d . . . N13 N 0.15541(16) 0.2425(5) 0.5830(2) 0.0512(12) Uani 1 1 d . . . C1 C -0.0006(2) -0.2274(9) 0.8842(3) 0.070(2) Uani 1 1 d . . . C2 C -0.0069(3) -0.2866(10) 0.8429(4) 0.085(3) Uani 1 1 d . . . H2A H -0.0284 -0.3378 0.8281 0.102 Uiso 1 1 calc R . . C3 C 0.0169(3) -0.2767(10) 0.8207(4) 0.086(3) Uani 1 1 d . . . H3A H 0.0111 -0.3185 0.7907 0.103 Uiso 1 1 calc R . . C4 C 0.0489(2) -0.2061(8) 0.8424(3) 0.071(2) Uani 1 1 d . . . C5 C 0.0555(2) -0.1427(10) 0.8841(3) 0.081(3) Uani 1 1 d . . . H5A H 0.0770 -0.0915 0.8989 0.097 Uiso 1 1 calc R . . C6 C 0.0311(3) -0.1521(11) 0.9051(4) 0.090(3) Uani 1 1 d . . . H6A H 0.0361 -0.1070 0.9341 0.108 Uiso 1 1 calc R . . C7 C 0.1244(3) -0.1595(8) 0.8123(4) 0.070(2) Uani 1 1 d . . . C8 C 0.1105(2) -0.1858(6) 0.7619(4) 0.074(3) Uani 1 1 d . . . H8A H 0.0857 -0.2174 0.7437 0.089 Uiso 1 1 calc R . . C9 C 0.1333(2) -0.1652(6) 0.7381(3) 0.0587(17) Uani 1 1 d . . . H9A H 0.1245 -0.1819 0.7039 0.070 Uiso 1 1 calc R . . C10 C 0.16967(16) -0.1191(5) 0.7672(2) 0.0459(13) Uani 1 1 d . . . C11 C 0.1822(2) -0.0973(6) 0.8170(3) 0.0587(17) Uani 1 1 d . . . H11A H 0.2071 -0.0677 0.8363 0.070 Uiso 1 1 calc R . . C12 C 0.1592(2) -0.1176(8) 0.8392(3) 0.071(2) Uani 1 1 d . . . H12A H 0.1681 -0.1018 0.8734 0.085 Uiso 1 1 calc R . . C13 C 0.0505(2) 0.3337(8) 0.9598(3) 0.0641(19) Uani 1 1 d . . . C14 C 0.0444(2) 0.2338(8) 0.9288(3) 0.0645(19) Uani 1 1 d . . . H14A H 0.0388 0.1567 0.9380 0.077 Uiso 1 1 calc R . . C15 C 0.0464(2) 0.2462(7) 0.8850(3) 0.0661(19) Uani 1 1 d . . . H15A H 0.0418 0.1770 0.8644 0.079 Uiso 1 1 calc R . . C16 C 0.05491(18) 0.3557(7) 0.8698(3) 0.0535(15) Uani 1 1 d . . . C17 C 0.0595(2) 0.4571(8) 0.8991(3) 0.070(2) Uani 1 1 d . . . H17A H 0.0643 0.5341 0.8890 0.084 Uiso 1 1 calc R . . C18 C 0.0571(3) 0.4476(8) 0.9429(3) 0.077(2) Uani 1 1 d . . . H18A H 0.0598 0.5185 0.9621 0.093 Uiso 1 1 calc R . . C19 C 0.07129(18) 0.4403(6) 0.7683(3) 0.0504(14) Uani 1 1 d . . . C20 C 0.04233(19) 0.3853(7) 0.7272(3) 0.0574(16) Uani 1 1 d . . . H20A H 0.0213 0.3514 0.7297 0.069 Uiso 1 1 calc R . . C21 C 0.04389(16) 0.3798(7) 0.6831(3) 0.0533(15) Uani 1 1 d . . . H21A H 0.0241 0.3422 0.6551 0.064 Uiso 1 1 calc R . . C22 C 0.07513(15) 0.4305(6) 0.6798(2) 0.0476(13) Uani 1 1 d . . . C23 C 0.10274(18) 0.4889(7) 0.7199(3) 0.0574(16) Uani 1 1 d . . . H23A H 0.1233 0.5256 0.7170 0.069 Uiso 1 1 calc R . . C24 C 0.1011(2) 0.4953(8) 0.7643(3) 0.0649(19) Uani 1 1 d . . . H24A H 0.1202 0.5367 0.7917 0.078 Uiso 1 1 calc R . . C25 C 0.3250(2) -0.0840(7) 0.4591(3) 0.0666(19) Uani 1 1 d . . . C26 C 0.2879(3) -0.0557(8) 0.4275(3) 0.073(2) Uani 1 1 d . . . H26A H 0.2812 -0.0363 0.3941 0.088 Uiso 1 1 calc R . . C27 C 0.2606(2) -0.0548(7) 0.4431(3) 0.0619(17) Uani 1 1 d . . . H27A H 0.2353 -0.0356 0.4203 0.074 Uiso 1 1 calc R . . C28 C 0.26943(19) -0.0815(7) 0.4915(3) 0.0573(16) Uani 1 1 d . . . C29 C 0.3071(2) -0.1083(9) 0.5244(3) 0.079(2) Uani 1 1 d . . . H29A H 0.3138 -0.1261 0.5579 0.094 Uiso 1 1 calc R . . C30 C 0.3344(2) -0.1094(9) 0.5086(4) 0.081(3) Uani 1 1 d . . . H30A H 0.3598 -0.1273 0.5314 0.097 Uiso 1 1 calc R . . C31 C 0.1865(2) -0.0703(7) 0.5071(3) 0.0564(16) Uani 1 1 d . . . C32 C 0.1488(2) -0.0400(8) 0.4787(3) 0.067(2) Uani 1 1 d . . . H32A H 0.1395 -0.0205 0.4447 0.080 Uiso 1 1 calc R . . C33 C 0.1247(2) -0.0383(7) 0.5005(3) 0.0613(17) Uani 1 1 d . . . H33A H 0.0988 -0.0185 0.4809 0.074 Uiso 1 1 calc R . . C34 C 0.13728(18) -0.0643(6) 0.5490(2) 0.0514(14) Uani 1 1 d . . . C35 C 0.17510(19) -0.0954(8) 0.5778(3) 0.0631(18) Uani 1 1 d . . . H35A H 0.1845 -0.1128 0.6120 0.076 Uiso 1 1 calc R . . C36 C 0.1985(2) -0.1002(8) 0.5557(3) 0.067(2) Uani 1 1 d . . . H36A H 0.2239 -0.1252 0.5749 0.080 Uiso 1 1 calc R . . C37 C 0.2126(2) 0.2718(8) 0.7823(3) 0.0620(18) Uani 1 1 d . . . H37A H 0.2281 0.2911 0.7671 0.074 Uiso 1 1 calc R . . C38 C 0.2276(3) 0.2846(9) 0.8322(3) 0.079(3) Uani 1 1 d . . . H38A H 0.2528 0.3115 0.8510 0.095 Uiso 1 1 calc R . . C39 C 0.2053(2) 0.2577(8) 0.8550(3) 0.069(2) Uani 1 1 d . . . H39A H 0.2153 0.2650 0.8898 0.082 Uiso 1 1 calc R . . C40 C 0.1684(2) 0.2201(6) 0.8267(3) 0.0537(15) Uani 1 1 d . . . C41 C 0.1439(3) 0.1888(6) 0.8467(3) 0.0609(19) Uani 1 1 d . . . H41A H 0.1521 0.2002 0.8811 0.073 Uiso 1 1 calc R . . C42 C 0.1093(2) 0.1433(7) 0.8190(3) 0.065(2) Uani 1 1 d . . . H42A H 0.0936 0.1228 0.8339 0.078 Uiso 1 1 calc R . . C43 C 0.09608(19) 0.1257(7) 0.7672(3) 0.0561(17) Uani 1 1 d . . . C44 C 0.0606(2) 0.0758(7) 0.7365(3) 0.0636(19) Uani 1 1 d . . . H44A H 0.0441 0.0552 0.7501 0.076 Uiso 1 1 calc R . . C45 C 0.0494(2) 0.0563(7) 0.6873(3) 0.065(2) Uani 1 1 d . . . H45A H 0.0255 0.0209 0.6667 0.078 Uiso 1 1 calc R . . C46 C 0.07451(18) 0.0907(6) 0.6680(3) 0.0553(16) Uani 1 1 d . . . H46A H 0.0667 0.0800 0.6337 0.066 Uiso 1 1 calc R . . C47 C 0.15595(18) 0.2054(5) 0.7754(2) 0.0434(13) Uani 1 1 d . . . C48 C 0.11912(17) 0.1561(5) 0.7455(2) 0.0421(12) Uani 1 1 d . . . C49 C 0.24950(18) 0.1201(6) 0.7009(3) 0.0552(16) Uani 1 1 d . . . H49A H 0.2483 0.1055 0.7310 0.066 Uiso 1 1 calc R . . C50 C 0.28365(18) 0.0988(6) 0.6996(3) 0.0614(18) Uani 1 1 d . . . H50A H 0.3052 0.0716 0.7283 0.074 Uiso 1 1 calc R . . C51 C 0.2856(2) 0.1178(7) 0.6565(3) 0.068(2) Uani 1 1 d . . . H51A H 0.3084 0.1018 0.6547 0.082 Uiso 1 1 calc R . . C52 C 0.2546(2) 0.1603(7) 0.6158(3) 0.0614(18) Uani 1 1 d . . . C53 C 0.2533(3) 0.1808(10) 0.5681(4) 0.089(3) Uani 1 1 d . . . H53A H 0.2753 0.1664 0.5640 0.107 Uiso 1 1 calc R . . C54 C 0.2223(3) 0.2190(10) 0.5302(4) 0.087(3) Uani 1 1 d . . . H54A H 0.2228 0.2317 0.4995 0.104 Uiso 1 1 calc R . . C55 C 0.1882(3) 0.2423(8) 0.5330(3) 0.075(2) Uani 1 1 d . . . C56 C 0.1546(3) 0.2815(9) 0.4926(4) 0.080(2) Uani 1 1 d . . . H56A H 0.1546 0.2964 0.4618 0.096 Uiso 1 1 calc R . . C57 C 0.1230(3) 0.2981(7) 0.4967(3) 0.080(3) Uani 1 1 d . . . H57A H 0.1004 0.3232 0.4692 0.096 Uiso 1 1 calc R . . C58 C 0.1243(2) 0.2768(7) 0.5439(3) 0.0662(19) Uani 1 1 d . . . H58A H 0.1019 0.2878 0.5473 0.079 Uiso 1 1 calc R . . C59 C 0.2207(2) 0.1819(5) 0.6199(3) 0.0484(15) Uani 1 1 d . . . C60 C 0.1872(2) 0.2247(6) 0.5780(3) 0.0537(16) Uani 1 1 d . . . O2W O 0.1435(5) 0.5777(18) 0.8875(7) 0.270(8) Uiso 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 Ho1 0.03260(17) 0.03222(17) 0.03782(17) -0.00232(8) 0.01641(12) 0.00002(8) S1 0.0376(7) 0.0347(7) 0.0574(8) 0.0052(6) 0.0232(6) 0.0052(5) S2 0.0364(7) 0.0475(8) 0.0544(8) 0.0027(7) 0.0184(6) 0.0066(6) S3 0.0407(7) 0.0468(9) 0.0557(9) -0.0164(7) 0.0162(7) -0.0061(6) O1W 0.044(2) 0.038(2) 0.065(3) -0.0056(19) 0.025(2) -0.0062(17) O1 0.047(2) 0.048(2) 0.069(3) 0.017(2) 0.029(2) 0.0096(19) O2 0.037(2) 0.062(3) 0.060(3) 0.007(2) 0.015(2) -0.0002(19) O3 0.072(3) 0.048(3) 0.090(4) -0.006(2) 0.055(3) 0.003(2) O3W 0.106(6) 0.181(9) 0.109(6) -0.044(6) -0.014(5) 0.066(6) O4 0.045(2) 0.043(2) 0.065(3) 0.011(2) 0.030(2) 0.0124(18) O4W 0.070(3) 0.041(3) 0.098(5) -0.001(2) 0.036(3) 0.005(2) O5 0.048(3) 0.096(4) 0.070(3) -0.020(3) 0.020(3) -0.010(3) O6 0.066(3) 0.050(3) 0.078(3) 0.018(2) 0.035(3) 0.019(2) O7 0.059(3) 0.048(3) 0.062(3) -0.018(2) 0.027(2) -0.014(2) O8 0.040(2) 0.095(4) 0.072(3) -0.034(3) 0.011(2) 0.001(2) O9 0.088(4) 0.046(3) 0.103(5) 0.006(3) 0.057(4) -0.004(3) N1 0.092(6) 0.140(8) 0.120(7) 0.000(7) 0.077(6) -0.032(6) N2 0.069(5) 0.077(5) 0.100(6) 0.016(4) 0.019(5) -0.004(4) N3 0.099(6) 0.069(4) 0.071(5) 0.014(4) 0.031(4) -0.011(4) N4 0.093(6) 0.099(6) 0.071(5) 0.022(4) 0.036(4) -0.013(4) N5 0.051(3) 0.055(3) 0.070(4) 0.012(3) 0.031(3) 0.007(3) N6 0.056(3) 0.060(4) 0.063(3) 0.006(3) 0.028(3) -0.002(3) N7 0.093(5) 0.090(6) 0.115(6) -0.018(5) 0.076(5) -0.016(4) N8 0.062(4) 0.059(4) 0.068(4) 0.008(3) 0.031(3) 0.002(3) N9 0.062(4) 0.061(4) 0.057(3) 0.002(3) 0.026(3) 0.006(3) N10 0.045(3) 0.044(3) 0.042(3) -0.003(2) 0.016(2) -0.008(2) N11 0.035(2) 0.044(3) 0.050(3) -0.001(2) 0.017(2) 0.001(2) N12 0.049(3) 0.034(2) 0.062(3) -0.003(2) 0.032(3) -0.001(2) N13 0.058(3) 0.045(3) 0.050(3) -0.001(2) 0.025(3) 0.009(2) C1 0.060(4) 0.082(5) 0.077(5) 0.014(5) 0.040(4) -0.009(4) C2 0.064(5) 0.096(7) 0.096(7) 0.002(5) 0.037(5) -0.025(5) C3 0.080(6) 0.108(8) 0.074(6) -0.002(5) 0.040(5) -0.018(5) C4 0.056(4) 0.095(6) 0.072(5) 0.028(4) 0.039(4) 0.011(4) C5 0.056(4) 0.106(7) 0.081(6) 0.014(5) 0.031(4) -0.022(5) C6 0.081(6) 0.121(8) 0.073(6) -0.001(6) 0.038(5) -0.038(6) C7 0.088(6) 0.058(4) 0.088(6) 0.023(4) 0.061(5) 0.019(4) C8 0.051(4) 0.041(4) 0.131(9) 0.008(4) 0.042(5) 0.001(3) C9 0.053(4) 0.038(3) 0.087(5) -0.002(3) 0.033(4) -0.004(3) C10 0.044(3) 0.036(3) 0.063(4) 0.004(3) 0.029(3) 0.006(2) C11 0.068(4) 0.054(4) 0.065(4) 0.006(3) 0.040(4) 0.009(3) C12 0.084(5) 0.064(5) 0.082(6) 0.016(4) 0.053(5) 0.017(4) C13 0.051(4) 0.081(5) 0.057(4) 0.014(4) 0.021(3) -0.004(4) C14 0.059(4) 0.058(4) 0.073(5) 0.015(4) 0.028(4) 0.001(3) C15 0.063(4) 0.052(4) 0.086(6) 0.006(4) 0.036(4) 0.000(3) C16 0.043(3) 0.058(4) 0.060(4) 0.011(3) 0.024(3) 0.002(3) C17 0.077(5) 0.066(5) 0.069(5) 0.008(4) 0.035(4) -0.019(4) C18 0.095(6) 0.068(5) 0.066(5) -0.004(4) 0.034(5) -0.025(4) C19 0.054(3) 0.038(3) 0.066(4) 0.000(3) 0.033(3) 0.003(2) C20 0.048(3) 0.057(4) 0.074(5) -0.001(3) 0.034(3) -0.001(3) C21 0.035(3) 0.065(4) 0.059(4) 0.001(3) 0.020(3) 0.001(3) C22 0.036(3) 0.043(3) 0.060(4) -0.003(3) 0.018(3) 0.006(2) C23 0.051(3) 0.065(4) 0.059(4) -0.007(3) 0.026(3) -0.017(3) C24 0.060(4) 0.071(5) 0.068(5) -0.014(4) 0.032(4) -0.018(4) C25 0.076(5) 0.058(4) 0.081(5) -0.012(4) 0.048(4) -0.013(4) C26 0.089(6) 0.085(6) 0.056(4) -0.011(4) 0.043(4) -0.009(5) C27 0.064(4) 0.067(5) 0.053(4) -0.002(3) 0.025(3) 0.002(3) C28 0.058(4) 0.053(4) 0.064(4) 0.006(3) 0.032(3) 0.003(3) C29 0.078(5) 0.083(6) 0.075(5) 0.025(5) 0.036(5) 0.012(4) C30 0.051(4) 0.099(7) 0.086(6) 0.020(5) 0.026(4) 0.004(4) C31 0.062(4) 0.053(4) 0.055(4) 0.004(3) 0.027(3) 0.006(3) C32 0.060(4) 0.089(6) 0.041(3) 0.002(3) 0.013(3) 0.013(4) C33 0.048(3) 0.071(5) 0.057(4) -0.002(3) 0.017(3) 0.008(3) C34 0.047(3) 0.053(4) 0.048(3) -0.011(3) 0.017(3) 0.004(3) C35 0.049(4) 0.078(5) 0.051(4) 0.010(3) 0.014(3) 0.008(3) C36 0.045(4) 0.084(6) 0.063(4) 0.019(4) 0.018(3) 0.014(3) C37 0.055(4) 0.082(5) 0.051(4) -0.013(4) 0.026(3) -0.018(4) C38 0.066(5) 0.113(7) 0.049(4) -0.022(4) 0.019(4) -0.022(5) C39 0.086(5) 0.066(5) 0.042(4) -0.012(3) 0.019(4) -0.002(4) C40 0.069(4) 0.045(3) 0.050(4) -0.001(3) 0.030(3) 0.003(3) C41 0.086(6) 0.053(4) 0.057(4) 0.003(3) 0.045(4) 0.008(3) C42 0.093(6) 0.053(4) 0.079(5) 0.011(4) 0.066(5) 0.020(4) C43 0.054(4) 0.058(4) 0.069(4) 0.019(3) 0.039(3) 0.013(3) C44 0.057(4) 0.051(4) 0.095(6) 0.010(4) 0.045(4) 0.002(3) C45 0.043(3) 0.058(4) 0.096(6) -0.006(4) 0.034(4) -0.005(3) C46 0.049(3) 0.052(4) 0.069(4) -0.006(3) 0.031(3) -0.004(3) C47 0.049(3) 0.037(3) 0.044(3) -0.002(2) 0.021(3) 0.007(2) C48 0.046(3) 0.031(3) 0.053(3) 0.005(2) 0.026(3) 0.007(2) C49 0.046(3) 0.045(3) 0.072(4) -0.002(3) 0.024(3) -0.002(3) C50 0.043(3) 0.053(4) 0.093(5) -0.001(4) 0.035(4) -0.001(3) C51 0.050(4) 0.060(4) 0.108(6) -0.015(4) 0.048(4) -0.005(3) C52 0.067(4) 0.053(4) 0.086(5) -0.009(4) 0.054(4) -0.010(3) C53 0.086(7) 0.114(9) 0.105(8) -0.006(6) 0.075(7) -0.014(5) C54 0.098(7) 0.110(8) 0.086(7) 0.004(6) 0.071(6) -0.009(6) C55 0.100(6) 0.069(5) 0.074(5) 0.014(4) 0.055(5) -0.002(5) C56 0.108(7) 0.081(6) 0.062(5) 0.008(4) 0.047(5) 0.003(5) C57 0.107(7) 0.066(5) 0.057(5) 0.007(4) 0.028(5) 0.027(5) C58 0.076(5) 0.064(4) 0.049(4) 0.005(3) 0.020(4) 0.018(4) C59 0.054(4) 0.041(3) 0.061(4) -0.003(3) 0.035(3) -0.008(2) C60 0.071(4) 0.043(3) 0.063(4) -0.001(3) 0.044(4) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ho1 O4 2.266(4) . ? Ho1 O7 2.265(4) . ? Ho1 O1 2.303(4) . ? Ho1 O1W 2.396(4) . ? Ho1 N10 2.492(5) . ? Ho1 N13 2.513(6) . ? Ho1 N12 2.547(5) . ? Ho1 N11 2.560(5) . ? S1 O3 1.438(5) . ? S1 O2 1.452(5) . ? S1 O1 1.456(4) . ? S1 C10 1.767(6) . ? S2 O6 1.442(5) . ? S2 O5 1.444(5) . ? S2 O4 1.481(4) . ? S2 C22 1.766(7) . ? S3 O9 1.433(6) . ? S3 O8 1.439(5) . ? S3 O7 1.475(5) . ? S3 C34 1.787(7) . ? N1 C1 1.381(10) . ? N2 N3 1.171(10) . ? N2 C4 1.514(12) . ? N3 C7 1.496(11) . ? N4 C13 1.352(11) . ? N5 N6 1.271(8) . ? N5 C16 1.406(9) . ? N6 C19 1.438(9) . ? N7 C25 1.384(9) . ? N8 N9 1.248(8) . ? N8 C28 1.403(8) . ? N9 C31 1.418(9) . ? N10 C37 1.326(8) . ? N10 C47 1.347(8) . ? N11 C46 1.322(8) . ? N11 C48 1.385(8) . ? N12 C49 1.332(9) . ? N12 C59 1.347(9) . ? N13 C58 1.322(9) . ? N13 C60 1.356(8) . ? C1 C2 1.331(14) . ? C1 C6 1.398(12) . ? C2 C3 1.397(13) . ? C3 C4 1.373(13) . ? C4 C5 1.363(13) . ? C5 C6 1.385(12) . ? C7 C12 1.330(13) . ? C7 C8 1.401(14) . ? C8 C9 1.412(11) . ? C9 C10 1.402(9) . ? C10 C11 1.383(10) . ? C11 C12 1.378(10) . ? C13 C14 1.396(12) . ? C13 C18 1.421(11) . ? C14 C15 1.376(11) . ? C15 C16 1.384(10) . ? C16 C17 1.387(12) . ? C17 C18 1.381(11) . ? C19 C24 1.387(9) . ? C19 C20 1.395(10) . ? C20 C21 1.371(10) . ? C21 C22 1.406(8) . ? C22 C23 1.373(9) . ? C23 C24 1.381(10) . ? C25 C26 1.379(12) . ? C25 C30 1.405(12) . ? C26 C27 1.367(10) . ? C27 C28 1.381(10) . ? C28 C29 1.403(11) . ? C29 C30 1.372(11) . ? C31 C36 1.373(10) . ? C31 C32 1.389(10) . ? C32 C33 1.392(10) . ? C33 C34 1.355(10) . ? C34 C35 1.395(9) . ? C35 C36 1.371(10) . ? C37 C38 1.362(11) . ? C38 C39 1.381(12) . ? C39 C40 1.386(11) . ? C40 C41 1.404(10) . ? C40 C47 1.415(9) . ? C41 C42 1.340(12) . ? C42 C43 1.429(11) . ? C43 C48 1.391(8) . ? C43 C44 1.401(11) . ? C44 C45 1.369(12) . ? C45 C46 1.423(9) . ? C47 C48 1.434(9) . ? C49 C50 1.397(9) . ? C50 C51 1.363(11) . ? C51 C52 1.371(12) . ? C52 C59 1.428(9) . ? C52 C53 1.446(13) . ? C53 C54 1.315(15) . ? C54 C55 1.420(13) . ? C55 C60 1.399(10) . ? C55 C56 1.409(13) . ? C56 C57 1.331(14) . ? C57 C58 1.433(12) . ? C59 C60 1.441(10) . ? 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 O4 Ho1 O7 96.31(18) . . ? O4 Ho1 O1 154.21(15) . . ? O7 Ho1 O1 80.09(18) . . ? O4 Ho1 O1W 71.45(16) . . ? O7 Ho1 O1W 147.53(17) . . ? O1 Ho1 O1W 123.71(16) . . ? O4 Ho1 N10 94.69(17) . . ? O7 Ho1 N10 136.67(17) . . ? O1 Ho1 N10 72.24(18) . . ? O1W Ho1 N10 75.39(16) . . ? O4 Ho1 N13 79.59(17) . . ? O7 Ho1 N13 72.36(19) . . ? O1 Ho1 N13 122.47(17) . . ? O1W Ho1 N13 75.82(17) . . ? N10 Ho1 N13 150.97(19) . . ? O4 Ho1 N12 132.46(16) . . ? O7 Ho1 N12 101.85(17) . . ? O1 Ho1 N12 72.86(16) . . ? O1W Ho1 N12 69.75(15) . . ? N10 Ho1 N12 101.02(17) . . ? N13 Ho1 N12 65.17(18) . . ? O4 Ho1 N11 76.15(16) . . ? O7 Ho1 N11 77.02(17) . . ? O1 Ho1 N11 78.17(15) . . ? O1W Ho1 N11 125.84(16) . . ? N10 Ho1 N11 65.26(16) . . ? N13 Ho1 N11 138.17(17) . . ? N12 Ho1 N11 150.70(17) . . ? O3 S1 O2 113.7(3) . . ? O3 S1 O1 110.6(3) . . ? O2 S1 O1 111.6(3) . . ? O3 S1 C10 109.3(3) . . ? O2 S1 C10 105.8(3) . . ? O1 S1 C10 105.3(3) . . ? O6 S2 O5 115.6(4) . . ? O6 S2 O4 110.3(3) . . ? O5 S2 O4 111.5(3) . . ? O6 S2 C22 106.4(3) . . ? O5 S2 C22 108.0(3) . . ? O4 S2 C22 104.2(3) . . ? O9 S3 O8 114.6(4) . . ? O9 S3 O7 111.8(4) . . ? O8 S3 O7 109.6(3) . . ? O9 S3 C34 108.5(3) . . ? O8 S3 C34 106.8(3) . . ? O7 S3 C34 105.0(3) . . ? S1 O1 Ho1 171.5(3) . . ? S2 O4 Ho1 160.4(3) . . ? S3 O7 Ho1 158.6(3) . . ? N3 N2 C4 107.5(9) . . ? N2 N3 C7 108.8(9) . . ? N6 N5 C16 115.5(6) . . ? N5 N6 C19 112.4(6) . . ? N9 N8 C28 117.1(6) . . ? N8 N9 C31 113.6(6) . . ? C37 N10 C47 117.4(6) . . ? C37 N10 Ho1 121.2(4) . . ? C47 N10 Ho1 121.0(4) . . ? C46 N11 C48 118.5(5) . . ? C46 N11 Ho1 124.2(4) . . ? C48 N11 Ho1 117.3(4) . . ? C49 N12 C59 118.0(6) . . ? C49 N12 Ho1 123.2(4) . . ? C59 N12 Ho1 118.8(4) . . ? C58 N13 C60 118.8(7) . . ? C58 N13 Ho1 121.8(5) . . ? C60 N13 Ho1 119.2(4) . . ? C2 C1 N1 123.5(9) . . ? C2 C1 C6 117.5(8) . . ? N1 C1 C6 119.1(9) . . ? C1 C2 C3 122.7(9) . . ? C4 C3 C2 119.6(10) . . ? C5 C4 C3 118.8(8) . . ? C5 C4 N2 128.4(8) . . ? C3 C4 N2 112.8(9) . . ? C4 C5 C6 120.7(8) . . ? C5 C6 C1 120.8(10) . . ? C12 C7 C8 121.7(7) . . ? C12 C7 N3 113.5(8) . . ? C8 C7 N3 124.6(9) . . ? C7 C8 C9 120.1(8) . . ? C10 C9 C8 117.0(8) . . ? C11 C10 C9 120.5(6) . . ? C11 C10 S1 119.7(5) . . ? C9 C10 S1 119.8(6) . . ? C12 C11 C10 121.2(8) . . ? C7 C12 C11 119.6(8) . . ? N4 C13 C14 122.2(8) . . ? N4 C13 C18 120.8(9) . . ? C14 C13 C18 117.0(7) . . ? C15 C14 C13 120.4(7) . . ? C14 C15 C16 122.6(8) . . ? C15 C16 C17 117.7(7) . . ? C15 C16 N5 116.5(7) . . ? C17 C16 N5 125.6(7) . . ? C18 C17 C16 120.8(7) . . ? C17 C18 C13 121.3(8) . . ? C24 C19 C20 120.1(7) . . ? C24 C19 N6 116.2(6) . . ? C20 C19 N6 123.7(6) . . ? C21 C20 C19 120.6(6) . . ? C20 C21 C22 119.1(6) . . ? C23 C22 C21 119.9(6) . . ? C23 C22 S2 120.3(5) . . ? C21 C22 S2 119.7(5) . . ? C22 C23 C24 121.1(6) . . ? C23 C24 C19 119.1(7) . . ? C26 C25 N7 122.8(8) . . ? C26 C25 C30 118.1(7) . . ? N7 C25 C30 119.1(8) . . ? C27 C26 C25 121.7(7) . . ? C26 C27 C28 120.8(7) . . ? C27 C28 N8 126.4(7) . . ? C27 C28 C29 118.3(7) . . ? N8 C28 C29 115.3(7) . . ? C30 C29 C28 120.9(8) . . ? C29 C30 C25 120.2(8) . . ? C36 C31 C32 118.2(7) . . ? C36 C31 N9 124.7(6) . . ? C32 C31 N9 117.1(6) . . ? C31 C32 C33 119.5(7) . . ? C34 C33 C32 121.3(7) . . ? C33 C34 C35 119.6(7) . . ? C33 C34 S3 122.2(5) . . ? C35 C34 S3 118.2(5) . . ? C36 C35 C34 118.7(7) . . ? C35 C36 C31 122.6(7) . . ? N10 C37 C38 124.4(7) . . ? C37 C38 C39 118.7(8) . . ? C38 C39 C40 119.6(7) . . ? C39 C40 C41 123.6(7) . . ? C39 C40 C47 117.2(7) . . ? C41 C40 C47 119.0(7) . . ? C42 C41 C40 122.4(7) . . ? C41 C42 C43 120.0(6) . . ? C48 C43 C44 117.3(7) . . ? C48 C43 C42 119.9(7) . . ? C44 C43 C42 122.8(6) . . ? C45 C44 C43 121.2(6) . . ? C44 C45 C46 117.9(7) . . ? N11 C46 C45 122.6(7) . . ? N10 C47 C40 122.6(6) . . ? N10 C47 C48 118.3(5) . . ? C40 C47 C48 119.1(6) . . ? N11 C48 C43 122.4(6) . . ? N11 C48 C47 118.0(5) . . ? C43 C48 C47 119.5(6) . . ? N12 C49 C50 123.2(7) . . ? C51 C50 C49 118.9(7) . . ? C50 C51 C52 119.8(6) . . ? C51 C52 C59 118.4(7) . . ? C51 C52 C53 124.4(7) . . ? C59 C52 C53 117.2(8) . . ? C54 C53 C52 121.4(8) . . ? C53 C54 C55 123.0(9) . . ? C60 C55 C56 117.1(8) . . ? C60 C55 C54 119.1(9) . . ? C56 C55 C54 123.8(9) . . ? C57 C56 C55 121.5(9) . . ? C56 C57 C58 117.9(9) . . ? N13 C58 C57 122.5(8) . . ? N12 C59 C52 121.6(7) . . ? N12 C59 C60 117.9(6) . . ? C52 C59 C60 120.4(7) . . ? N13 C60 C55 122.2(8) . . ? N13 C60 C59 118.8(6) . . ? C55 C60 C59 119.0(7) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.516 _refine_diff_density_min -2.546 _refine_diff_density_rms 0.340 #===end