data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Fei, Honghan' 'Oliver, Scott' _publ_contact_author_name 'Oliver Scott' _publ_contact_author_address ; Santa Cruz 95064 ; _publ_contact_author_email soliver@chemistry.ucsc.edu # Attachment '- SLUG-23.cif' data_xsc1002 _database_code_depnum_ccdc_archive 'CCDC 790077' #TrackingRef '- SLUG-23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H52 Cd3 N10 O18 S6' _chemical_formula_weight 1682.73 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 8.4243(9) _cell_length_b 11.6368(12) _cell_length_c 15.7095(16) _cell_angle_alpha 95.4940(10) _cell_angle_beta 104.7250(10) _cell_angle_gamma 99.1220(10) _cell_volume 1455.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8442 _cell_measurement_theta_min 4.788 _cell_measurement_theta_max 59.314 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.075 _exptl_crystal_size_mid 0.050 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.920 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 1.387 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6724 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 14904 _diffrn_reflns_av_R_equivalents 0.0206 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 26.73 _reflns_number_total 6107 _reflns_number_gt 5395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-II v2.1-4' _computing_cell_refinement 'Bruker SAINT v7.34' _computing_data_reduction 'Bruker SAINT v7.34' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.6428P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6107 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0230 _refine_ls_wR_factor_ref 0.0603 _refine_ls_wR_factor_gt 0.0578 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _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 Cd1 Cd 0.5000 0.5000 0.0000 0.00965(6) Uani 1 2 d S . . Cd2 Cd 0.476744(19) 0.449920(13) 0.323826(10) 0.01056(5) Uani 1 1 d . . . S1 S 0.22371(7) 0.44746(5) 0.47608(3) 0.01285(11) Uani 1 1 d . . . S3 S 0.17708(6) 0.42777(5) 0.10648(3) 0.01180(11) Uani 1 1 d . . . S4 S 0.79757(7) 0.53008(5) 0.22081(3) 0.01239(11) Uani 1 1 d . . . O1 O 0.25217(19) 0.43635(14) 0.38788(10) 0.0160(3) Uani 1 1 d . . . O2 O 0.2153(2) 0.33925(15) 0.51353(11) 0.0203(4) Uani 1 1 d . . . O3 O 0.34285(19) 0.54641(14) 0.53633(10) 0.0169(3) Uani 1 1 d . . . O7 O 0.2789(2) 0.50316(15) 0.06300(11) 0.0191(4) Uani 1 1 d . . . O8 O 0.2791(2) 0.38616(15) 0.18256(10) 0.0184(4) Uani 1 1 d . . . O9 O 0.05828(19) 0.33351(14) 0.04503(10) 0.0180(3) Uani 1 1 d . . . O10 O 0.7036(2) 0.55454(15) 0.13468(10) 0.0201(4) Uani 1 1 d . . . O11 O 0.6942(2) 0.44825(15) 0.25950(12) 0.0216(4) Uani 1 1 d . . . O12 O 0.8855(2) 0.63552(14) 0.28050(10) 0.0192(4) Uani 1 1 d . . . N1 N 0.4990(2) 0.69505(16) 0.00412(12) 0.0125(4) Uani 1 1 d . . . N7 N 0.4497(2) 0.63981(16) 0.31202(12) 0.0131(4) Uani 1 1 d . . . N8 N 0.4556(2) 0.25077(16) 0.31465(12) 0.0135(4) Uani 1 1 d . . . C1 C 0.0249(3) 0.4898(2) 0.45709(14) 0.0155(5) Uani 1 1 d . . . H1A H 0.0285 0.5629 0.4295 0.023 Uiso 1 1 calc R . . H1B H -0.0605 0.4275 0.4151 0.023 Uiso 1 1 calc R . . C3 C 0.0563(3) 0.5200(2) 0.14805(15) 0.0138(4) Uani 1 1 d . . . H3A H 0.1314 0.5888 0.1883 0.021 Uiso 1 1 calc R . . H3B H -0.0166 0.5491 0.0981 0.021 Uiso 1 1 calc R . . C4 C 0.9497(3) 0.4514(2) 0.19828(15) 0.0149(5) Uani 1 1 d . . . H4A H 1.0223 0.4368 0.2549 0.022 Uiso 1 1 calc R . . H4B H 0.8932 0.3743 0.1624 0.022 Uiso 1 1 calc R . . C11 C 0.4814(3) 0.6941(2) 0.24486(14) 0.0151(5) Uani 1 1 d . . . H11A H 0.5124 0.6506 0.1994 0.018 Uiso 1 1 calc R . . C12 C 0.4036(3) 0.7036(2) 0.37454(15) 0.0183(5) Uani 1 1 d . . . H12A H 0.3801 0.6667 0.4225 0.022 Uiso 1 1 calc R . . C13 C 0.3887(3) 0.8197(2) 0.37271(15) 0.0181(5) Uani 1 1 d . . . H13A H 0.3526 0.8601 0.4177 0.022 Uiso 1 1 calc R . . C14 C 0.4711(3) 0.8103(2) 0.23876(14) 0.0151(5) Uani 1 1 d . . . H14A H 0.4942 0.8445 0.1896 0.018 Uiso 1 1 calc R . . C15 C 0.4270(3) 0.87797(19) 0.30402(14) 0.0130(4) Uani 1 1 d . . . C16 C 0.4302(3) 1.00538(19) 0.30535(14) 0.0134(4) Uani 1 1 d . . . C17 C 0.3851(3) 1.0714(2) 0.37123(15) 0.0166(5) Uani 1 1 d . . . H17A H 0.3445 1.0336 0.4145 0.025 Uiso 1 1 calc R . . C18 C 0.4848(3) 1.0680(2) 0.24298(15) 0.0179(5) Uani 1 1 d . . . H18A H 0.5145 1.0274 0.1957 0.027 Uiso 1 1 calc R . . C20 C 0.3991(3) 0.1912(2) 0.37370(15) 0.0171(5) Uani 1 1 d . . . H20A H 0.3674 0.2339 0.4193 0.026 Uiso 1 1 calc R . . C21 C 0.6469(3) 0.8912(2) 0.01364(15) 0.0155(5) Uani 1 1 d . . . H21A H 0.7508 0.9423 0.0213 0.019 Uiso 1 1 calc R . . C22 C 0.3518(3) 0.8557(2) -0.00800(15) 0.0142(4) Uani 1 1 d . . . H22A H 0.2484 0.8817 -0.0155 0.017 Uiso 1 1 calc R . . C23 C 0.4996(3) 0.93680(19) 0.00115(14) 0.0111(4) Uani 1 1 d . . . C27 C 0.6411(3) 0.7726(2) 0.01485(15) 0.0159(5) Uani 1 1 d . . . H27A H 0.7428 0.7442 0.0237 0.019 Uiso 1 1 calc R . . C28 C 0.3571(3) 0.7379(2) -0.00600(15) 0.0146(4) Uani 1 1 d . . . H28A H 0.2557 0.6846 -0.0121 0.017 Uiso 1 1 calc R . . C41 C 0.4955(3) 0.1882(2) 0.24994(15) 0.0174(5) Uani 1 1 d . . . H41A H 0.5330 0.2284 0.2067 0.026 Uiso 1 1 calc R . . N11 N 0.1023(2) -0.03140(18) 0.09568(13) 0.0193(4) Uani 1 1 d . . . N12 N -0.2128(3) 0.04727(19) 0.47470(13) 0.0223(4) Uani 1 1 d . . . C91 C 0.0593(3) -0.1208(2) 0.13790(16) 0.0200(5) Uani 1 1 d . . . H91A H 0.0716 -0.1968 0.1158 0.024 Uiso 1 1 calc R . . C92 C 0.0826(3) 0.0743(2) 0.12877(16) 0.0216(5) Uani 1 1 d . . . C93 C -0.1968(3) -0.0583(2) 0.44004(16) 0.0207(5) Uani 1 1 d . . . H93A H -0.2301 -0.1242 0.4671 0.025 Uiso 1 1 calc R . . C94 C -0.1599(3) 0.1381(2) 0.43613(17) 0.0250(6) Uani 1 1 d . . . H94A H -0.1670 0.2146 0.4602 0.030 Uiso 1 1 calc R . . C95 C -0.0019(3) -0.1103(2) 0.21152(15) 0.0200(5) Uani 1 1 d . . . H95A H -0.0306 -0.1775 0.2384 0.024 Uiso 1 1 calc R . . C96 C 0.0225(3) 0.0941(2) 0.20206(16) 0.0199(5) Uani 1 1 d . . . H96A H 0.0111 0.1711 0.2224 0.024 Uiso 1 1 calc R . . C97 C -0.0211(3) 0.0006(2) 0.24594(15) 0.0169(5) Uani 1 1 d . . . C98 C -0.0843(3) 0.0166(2) 0.32623(15) 0.0171(5) Uani 1 1 d . . . C99 C -0.1351(3) -0.0780(2) 0.36740(15) 0.0194(5) Uani 1 1 d . . . H99A H -0.1274 -0.1554 0.3458 0.023 Uiso 1 1 calc R . . C100 C -0.0961(3) 0.1280(2) 0.36407(16) 0.0238(5) Uani 1 1 d . . . H10A H -0.0602 0.1961 0.3400 0.029 Uiso 1 1 calc R . . H92 H 0.117(4) 0.139(3) 0.1003(19) 0.035(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 Cd1 0.01120(11) 0.00673(11) 0.01258(11) 0.00219(8) 0.00513(8) 0.00273(8) Cd2 0.01238(9) 0.00807(9) 0.01275(9) 0.00247(6) 0.00511(6) 0.00310(6) S1 0.0126(3) 0.0141(3) 0.0133(3) 0.0021(2) 0.0051(2) 0.0040(2) S3 0.0115(3) 0.0126(3) 0.0129(3) 0.0029(2) 0.0053(2) 0.0035(2) S4 0.0126(3) 0.0132(3) 0.0131(3) 0.0022(2) 0.0058(2) 0.0040(2) O1 0.0138(8) 0.0200(9) 0.0150(8) 0.0001(6) 0.0048(6) 0.0055(6) O2 0.0246(9) 0.0169(9) 0.0232(9) 0.0065(7) 0.0104(7) 0.0070(7) O3 0.0154(8) 0.0189(9) 0.0150(8) 0.0013(7) 0.0032(6) 0.0018(7) O7 0.0208(9) 0.0176(9) 0.0257(9) 0.0077(7) 0.0154(7) 0.0065(7) O8 0.0199(8) 0.0194(9) 0.0169(8) 0.0033(7) 0.0029(7) 0.0095(7) O9 0.0152(8) 0.0193(9) 0.0183(8) -0.0019(7) 0.0042(6) 0.0032(7) O10 0.0188(8) 0.0276(10) 0.0156(8) 0.0036(7) 0.0037(7) 0.0107(7) O11 0.0230(9) 0.0168(9) 0.0314(10) 0.0065(7) 0.0181(8) 0.0039(7) O12 0.0228(9) 0.0158(9) 0.0184(8) -0.0007(7) 0.0060(7) 0.0034(7) N1 0.0136(9) 0.0103(9) 0.0147(9) 0.0025(7) 0.0050(7) 0.0033(7) N7 0.0155(9) 0.0085(9) 0.0153(9) 0.0010(7) 0.0041(7) 0.0027(7) N8 0.0162(9) 0.0097(9) 0.0149(9) 0.0022(7) 0.0044(7) 0.0030(7) C1 0.0133(11) 0.0207(12) 0.0128(11) 0.0015(9) 0.0029(9) 0.0062(9) C3 0.0148(11) 0.0135(11) 0.0159(11) 0.0031(9) 0.0077(9) 0.0044(9) C4 0.0156(11) 0.0165(12) 0.0165(11) 0.0041(9) 0.0084(9) 0.0064(9) C11 0.0178(11) 0.0141(12) 0.0135(10) -0.0002(9) 0.0047(9) 0.0035(9) C12 0.0266(13) 0.0131(12) 0.0195(12) 0.0052(9) 0.0126(10) 0.0041(10) C13 0.0281(13) 0.0113(12) 0.0195(12) 0.0030(9) 0.0138(10) 0.0050(10) C14 0.0202(12) 0.0125(11) 0.0135(10) 0.0029(9) 0.0061(9) 0.0030(9) C15 0.0138(11) 0.0090(11) 0.0149(11) 0.0013(8) 0.0022(9) 0.0017(8) C16 0.0140(11) 0.0111(11) 0.0138(10) 0.0010(8) 0.0016(8) 0.0026(8) C17 0.0232(12) 0.0127(12) 0.0185(11) 0.0044(9) 0.0115(10) 0.0057(9) C18 0.0284(13) 0.0131(12) 0.0162(11) 0.0020(9) 0.0126(10) 0.0049(10) C20 0.0234(12) 0.0145(12) 0.0166(11) 0.0032(9) 0.0094(9) 0.0061(9) C21 0.0129(11) 0.0093(11) 0.0257(12) 0.0032(9) 0.0076(9) 0.0017(8) C22 0.0101(10) 0.0137(12) 0.0206(11) 0.0047(9) 0.0050(9) 0.0047(8) C23 0.0130(10) 0.0102(11) 0.0111(10) 0.0024(8) 0.0049(8) 0.0026(8) C27 0.0126(11) 0.0133(12) 0.0232(12) 0.0034(9) 0.0064(9) 0.0034(9) C28 0.0123(11) 0.0112(11) 0.0188(11) 0.0035(9) 0.0025(9) 0.0006(8) C41 0.0242(12) 0.0142(12) 0.0166(11) 0.0040(9) 0.0095(10) 0.0039(9) N11 0.0192(10) 0.0215(11) 0.0182(10) 0.0031(8) 0.0061(8) 0.0049(8) N12 0.0222(11) 0.0260(12) 0.0193(10) 0.0035(9) 0.0078(8) 0.0032(9) C91 0.0218(12) 0.0160(12) 0.0202(12) 0.0003(10) 0.0026(10) 0.0044(10) C92 0.0242(13) 0.0194(13) 0.0230(13) 0.0076(10) 0.0074(10) 0.0051(10) C93 0.0165(12) 0.0230(13) 0.0213(12) 0.0056(10) 0.0044(9) 0.0001(10) C94 0.0307(14) 0.0186(13) 0.0259(13) -0.0008(10) 0.0110(11) 0.0023(11) C95 0.0228(12) 0.0174(13) 0.0194(12) 0.0035(10) 0.0055(10) 0.0022(10) C96 0.0221(12) 0.0151(12) 0.0233(12) 0.0040(10) 0.0062(10) 0.0053(10) C97 0.0130(11) 0.0194(12) 0.0169(11) 0.0027(9) 0.0025(9) 0.0016(9) C98 0.0139(11) 0.0184(12) 0.0170(11) 0.0028(9) 0.0026(9) 0.0001(9) C99 0.0192(12) 0.0181(13) 0.0194(12) 0.0026(10) 0.0032(9) 0.0031(9) C100 0.0296(14) 0.0187(13) 0.0245(13) 0.0038(10) 0.0110(11) 0.0022(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 Cd1 N1 2.2659(19) 2_665 ? Cd1 N1 2.2660(19) . ? Cd1 O10 2.3183(16) . ? Cd1 O10 2.3183(16) 2_665 ? Cd1 O7 2.3240(15) 2_665 ? Cd1 O7 2.3240(15) . ? Cd2 N7 2.2773(18) . ? Cd2 N8 2.2837(19) . ? Cd2 O11 2.3077(16) . ? Cd2 O3 2.3242(15) 2_666 ? Cd2 O1 2.3495(15) . ? Cd2 O8 2.3797(16) . ? S1 O2 1.4392(17) . ? S1 O1 1.4624(16) . ? S1 O3 1.4734(16) . ? S1 C1 1.782(2) . ? S3 O9 1.4473(16) . ? S3 O8 1.4566(16) . ? S3 O7 1.4651(16) . ? S3 C3 1.779(2) . ? S4 O12 1.4393(17) . ? S4 O10 1.4625(16) . ? S4 O11 1.4668(17) . ? S4 C4 1.774(2) . ? O3 Cd2 2.3242(15) 2_666 ? N1 C27 1.342(3) . ? N1 C28 1.346(3) . ? N7 C11 1.342(3) . ? N7 C12 1.346(3) . ? N8 C41 1.337(3) . ? N8 C20 1.345(3) . ? C1 C1 1.519(4) 2_566 ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C4 1.524(3) 1_455 ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C3 1.524(3) 1_655 ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C11 C14 1.379(3) . ? C11 H11A 0.9500 . ? C12 C13 1.378(3) . ? C12 H12A 0.9500 . ? C13 C15 1.406(3) . ? C13 H13A 0.9500 . ? C14 C15 1.393(3) . ? C14 H14A 0.9500 . ? C15 C16 1.477(3) . ? C16 C17 1.395(3) . ? C16 C18 1.400(3) . ? C17 C20 1.376(3) 1_565 ? C17 H17A 0.9500 . ? C18 C41 1.380(3) 1_565 ? C18 H18A 0.9500 . ? C20 C17 1.376(3) 1_545 ? C20 H20A 0.9500 . ? C21 C27 1.375(3) . ? C21 C23 1.401(3) . ? C21 H21A 0.9500 . ? C22 C28 1.381(3) . ? C22 C23 1.404(3) . ? C22 H22A 0.9500 . ? C23 C23 1.474(4) 2_675 ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C41 C18 1.380(3) 1_545 ? C41 H41A 0.9500 . ? N11 C91 1.337(3) . ? N11 C92 1.341(3) . ? N12 C93 1.336(3) . ? N12 C94 1.339(3) . ? C91 C95 1.384(3) . ? C91 H91A 0.9500 . ? C92 C96 1.384(3) . ? C92 H92 0.95(3) . ? C93 C99 1.384(3) . ? C93 H93A 0.9500 . ? C94 C100 1.374(3) . ? C94 H94A 0.9500 . ? C95 C97 1.400(3) . ? C95 H95A 0.9500 . ? C96 C97 1.393(3) . ? C96 H96A 0.9500 . ? C97 C98 1.496(3) . ? C98 C99 1.393(3) . ? C98 C100 1.402(3) . ? C99 H99A 0.9500 . ? C100 H10A 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 N1 Cd1 N1 180.00(9) 2_665 . ? N1 Cd1 O10 95.01(6) 2_665 . ? N1 Cd1 O10 84.99(6) . . ? N1 Cd1 O10 84.99(6) 2_665 2_665 ? N1 Cd1 O10 95.01(6) . 2_665 ? O10 Cd1 O10 180.0 . 2_665 ? N1 Cd1 O7 82.90(6) 2_665 2_665 ? N1 Cd1 O7 97.10(6) . 2_665 ? O10 Cd1 O7 85.76(6) . 2_665 ? O10 Cd1 O7 94.23(6) 2_665 2_665 ? N1 Cd1 O7 97.10(6) 2_665 . ? N1 Cd1 O7 82.90(6) . . ? O10 Cd1 O7 94.24(6) . . ? O10 Cd1 O7 85.77(6) 2_665 . ? O7 Cd1 O7 180.0 2_665 . ? N7 Cd2 N8 168.84(6) . . ? N7 Cd2 O11 97.37(6) . . ? N8 Cd2 O11 86.38(6) . . ? N7 Cd2 O3 105.96(6) . 2_666 ? N8 Cd2 O3 84.42(6) . 2_666 ? O11 Cd2 O3 90.73(6) . 2_666 ? N7 Cd2 O1 86.72(6) . . ? N8 Cd2 O1 89.40(6) . . ? O11 Cd2 O1 175.76(6) . . ? O3 Cd2 O1 89.20(5) 2_666 . ? N7 Cd2 O8 90.45(6) . . ? N8 Cd2 O8 78.98(6) . . ? O11 Cd2 O8 90.56(6) . . ? O3 Cd2 O8 163.23(6) 2_666 . ? O1 Cd2 O8 88.29(5) . . ? O2 S1 O1 113.62(10) . . ? O2 S1 O3 113.17(10) . . ? O1 S1 O3 111.30(9) . . ? O2 S1 C1 108.78(11) . . ? O1 S1 C1 103.66(9) . . ? O3 S1 C1 105.50(10) . . ? O9 S3 O8 112.72(10) . . ? O9 S3 O7 112.96(10) . . ? O8 S3 O7 112.05(10) . . ? O9 S3 C3 106.06(10) . . ? O8 S3 C3 107.15(10) . . ? O7 S3 C3 105.24(10) . . ? O12 S4 O10 112.58(10) . . ? O12 S4 O11 113.88(10) . . ? O10 S4 O11 111.94(10) . . ? O12 S4 C4 107.41(10) . . ? O10 S4 C4 105.83(10) . . ? O11 S4 C4 104.40(10) . . ? S1 O1 Cd2 139.09(9) . . ? S1 O3 Cd2 129.92(10) . 2_666 ? S3 O7 Cd1 139.98(10) . . ? S3 O8 Cd2 143.27(10) . . ? S4 O10 Cd1 152.13(11) . . ? S4 O11 Cd2 137.98(10) . . ? C27 N1 C28 117.20(19) . . ? C27 N1 Cd1 120.83(14) . . ? C28 N1 Cd1 121.95(15) . . ? C11 N7 C12 116.92(19) . . ? C11 N7 Cd2 122.60(15) . . ? C12 N7 Cd2 120.46(15) . . ? C41 N8 C20 117.2(2) . . ? C41 N8 Cd2 121.78(15) . . ? C20 N8 Cd2 121.02(15) . . ? C1 C1 S1 111.6(2) 2_566 . ? C1 C1 H1A 109.3 2_566 . ? S1 C1 H1A 109.3 . . ? C1 C1 H1B 109.3 2_566 . ? S1 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? C4 C3 S3 109.79(16) 1_455 . ? C4 C3 H3A 109.7 1_455 . ? S3 C3 H3A 109.7 . . ? C4 C3 H3B 109.7 1_455 . ? S3 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C3 C4 S4 110.86(16) 1_655 . ? C3 C4 H4A 109.5 1_655 . ? S4 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 1_655 . ? S4 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? N7 C11 C14 123.0(2) . . ? N7 C11 H11A 118.5 . . ? C14 C11 H11A 118.5 . . ? N7 C12 C13 123.5(2) . . ? N7 C12 H12A 118.2 . . ? C13 C12 H12A 118.2 . . ? C12 C13 C15 119.7(2) . . ? C12 C13 H13A 120.1 . . ? C15 C13 H13A 120.1 . . ? C11 C14 C15 120.6(2) . . ? C11 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C14 C15 C13 116.2(2) . . ? C14 C15 C16 122.7(2) . . ? C13 C15 C16 121.1(2) . . ? C17 C16 C18 116.0(2) . . ? C17 C16 C15 121.7(2) . . ? C18 C16 C15 122.2(2) . . ? C20 C17 C16 120.3(2) 1_565 . ? C20 C17 H17A 119.9 1_565 . ? C16 C17 H17A 119.9 . . ? C41 C18 C16 120.3(2) 1_565 . ? C41 C18 H18A 119.9 1_565 . ? C16 C18 H18A 119.9 . . ? N8 C20 C17 123.1(2) . 1_545 ? N8 C20 H20A 118.4 . . ? C17 C20 H20A 118.4 1_545 . ? C27 C21 C23 120.1(2) . . ? C27 C21 H21A 120.0 . . ? C23 C21 H21A 120.0 . . ? C28 C22 C23 119.9(2) . . ? C28 C22 H22A 120.1 . . ? C23 C22 H22A 120.1 . . ? C21 C23 C22 116.3(2) . . ? C21 C23 C23 121.7(2) . 2_675 ? C22 C23 C23 122.0(2) . 2_675 ? N1 C27 C21 123.4(2) . . ? N1 C27 H27A 118.3 . . ? C21 C27 H27A 118.3 . . ? N1 C28 C22 123.1(2) . . ? N1 C28 H28A 118.4 . . ? C22 C28 H28A 118.4 . . ? N8 C41 C18 123.1(2) . 1_545 ? N8 C41 H41A 118.5 . . ? C18 C41 H41A 118.5 1_545 . ? C91 N11 C92 115.9(2) . . ? C93 N12 C94 115.8(2) . . ? N11 C91 C95 124.5(2) . . ? N11 C91 H91A 117.7 . . ? C95 C91 H91A 117.7 . . ? N11 C92 C96 124.0(2) . . ? N11 C92 H92 116.1(18) . . ? C96 C92 H92 119.9(18) . . ? N12 C93 C99 124.4(2) . . ? N12 C93 H93A 117.8 . . ? C99 C93 H93A 117.8 . . ? N12 C94 C100 124.4(2) . . ? N12 C94 H94A 117.8 . . ? C100 C94 H94A 117.8 . . ? C91 C95 C97 119.2(2) . . ? C91 C95 H95A 120.4 . . ? C97 C95 H95A 120.4 . . ? C92 C96 C97 119.7(2) . . ? C92 C96 H96A 120.1 . . ? C97 C96 H96A 120.1 . . ? C96 C97 C95 116.6(2) . . ? C96 C97 C98 122.2(2) . . ? C95 C97 C98 121.1(2) . . ? C99 C98 C100 116.3(2) . . ? C99 C98 C97 122.0(2) . . ? C100 C98 C97 121.7(2) . . ? C93 C99 C98 119.5(2) . . ? C93 C99 H99A 120.3 . . ? C98 C99 H99A 120.3 . . ? C94 C100 C98 119.7(2) . . ? C94 C100 H10A 120.2 . . ? C98 C100 H10A 120.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 O1 Cd2 -88.65(16) . . . . ? O3 S1 O1 Cd2 40.51(18) . . . . ? C1 S1 O1 Cd2 153.45(14) . . . . ? N7 Cd2 O1 S1 -95.11(15) . . . . ? N8 Cd2 O1 S1 95.36(15) . . . . ? O11 Cd2 O1 S1 100.1(8) . . . . ? O3 Cd2 O1 S1 10.93(15) 2_666 . . . ? O8 Cd2 O1 S1 174.34(15) . . . . ? O2 S1 O3 Cd2 3.35(15) . . . 2_666 ? O1 S1 O3 Cd2 -126.04(11) . . . 2_666 ? C1 S1 O3 Cd2 122.18(12) . . . 2_666 ? O9 S3 O7 Cd1 -73.89(17) . . . . ? O8 S3 O7 Cd1 54.73(18) . . . . ? C3 S3 O7 Cd1 170.84(15) . . . . ? N1 Cd1 O7 S3 11.74(17) 2_665 . . . ? N1 Cd1 O7 S3 -168.26(17) . . . . ? O10 Cd1 O7 S3 -83.86(16) . . . . ? O10 Cd1 O7 S3 96.14(16) 2_665 . . . ? O7 Cd1 O7 S3 -29(51) 2_665 . . . ? O9 S3 O8 Cd2 -170.61(14) . . . . ? O7 S3 O8 Cd2 60.64(18) . . . . ? C3 S3 O8 Cd2 -54.31(18) . . . . ? N7 Cd2 O8 S3 4.18(17) . . . . ? N8 Cd2 O8 S3 -179.40(17) . . . . ? O11 Cd2 O8 S3 -93.20(17) . . . . ? O3 Cd2 O8 S3 172.41(14) 2_666 . . . ? O1 Cd2 O8 S3 90.88(17) . . . . ? O12 S4 O10 Cd1 -163.27(19) . . . . ? O11 S4 O10 Cd1 -33.5(2) . . . . ? C4 S4 O10 Cd1 79.7(2) . . . . ? N1 Cd1 O10 S4 -24.1(2) 2_665 . . . ? N1 Cd1 O10 S4 155.9(2) . . . . ? O10 Cd1 O10 S4 -76(7) 2_665 . . . ? O7 Cd1 O10 S4 -106.6(2) 2_665 . . . ? O7 Cd1 O10 S4 73.4(2) . . . . ? O12 S4 O11 Cd2 57.44(18) . . . . ? O10 S4 O11 Cd2 -71.70(17) . . . . ? C4 S4 O11 Cd2 174.28(15) . . . . ? N7 Cd2 O11 S4 0.35(17) . . . . ? N8 Cd2 O11 S4 169.79(16) . . . . ? O3 Cd2 O11 S4 -105.85(16) 2_666 . . . ? O1 Cd2 O11 S4 165.1(7) . . . . ? O8 Cd2 O11 S4 90.88(16) . . . . ? N1 Cd1 N1 C27 -131(6) 2_665 . . . ? O10 Cd1 N1 C27 53.93(16) . . . . ? O10 Cd1 N1 C27 -126.07(16) 2_665 . . . ? O7 Cd1 N1 C27 -31.16(17) 2_665 . . . ? O7 Cd1 N1 C27 148.84(17) . . . . ? N1 Cd1 N1 C28 47(6) 2_665 . . . ? O10 Cd1 N1 C28 -127.61(17) . . . . ? O10 Cd1 N1 C28 52.39(17) 2_665 . . . ? O7 Cd1 N1 C28 147.30(17) 2_665 . . . ? O7 Cd1 N1 C28 -32.70(17) . . . . ? N8 Cd2 N7 C11 -77.0(4) . . . . ? O11 Cd2 N7 C11 32.03(18) . . . . ? O3 Cd2 N7 C11 124.92(17) 2_666 . . . ? O1 Cd2 N7 C11 -146.85(17) . . . . ? O8 Cd2 N7 C11 -58.59(17) . . . . ? N8 Cd2 N7 C12 104.4(3) . . . . ? O11 Cd2 N7 C12 -146.56(17) . . . . ? O3 Cd2 N7 C12 -53.67(18) 2_666 . . . ? O1 Cd2 N7 C12 34.56(17) . . . . ? O8 Cd2 N7 C12 122.82(17) . . . . ? N7 Cd2 N8 C41 79.6(4) . . . . ? O11 Cd2 N8 C41 -30.51(17) . . . . ? O3 Cd2 N8 C41 -121.60(17) 2_666 . . . ? O1 Cd2 N8 C41 149.14(17) . . . . ? O8 Cd2 N8 C41 60.77(17) . . . . ? N7 Cd2 N8 C20 -99.2(4) . . . . ? O11 Cd2 N8 C20 150.73(17) . . . . ? O3 Cd2 N8 C20 59.64(17) 2_666 . . . ? O1 Cd2 N8 C20 -29.62(17) . . . . ? O8 Cd2 N8 C20 -117.99(17) . . . . ? O2 S1 C1 C1 60.8(3) . . . 2_566 ? O1 S1 C1 C1 -178.0(2) . . . 2_566 ? O3 S1 C1 C1 -60.9(3) . . . 2_566 ? O9 S3 C3 C4 62.31(18) . . . 1_455 ? O8 S3 C3 C4 -58.32(18) . . . 1_455 ? O7 S3 C3 C4 -177.74(15) . . . 1_455 ? O12 S4 C4 C3 -65.02(18) . . . 1_655 ? O10 S4 C4 C3 55.47(18) . . . 1_655 ? O11 S4 C4 C3 173.75(16) . . . 1_655 ? C12 N7 C11 C14 1.0(3) . . . . ? Cd2 N7 C11 C14 -177.65(17) . . . . ? C11 N7 C12 C13 -0.3(3) . . . . ? Cd2 N7 C12 C13 178.40(19) . . . . ? N7 C12 C13 C15 -1.8(4) . . . . ? N7 C11 C14 C15 0.4(3) . . . . ? C11 C14 C15 C13 -2.3(3) . . . . ? C11 C14 C15 C16 173.8(2) . . . . ? C12 C13 C15 C14 3.0(3) . . . . ? C12 C13 C15 C16 -173.3(2) . . . . ? C14 C15 C16 C17 179.8(2) . . . . ? C13 C15 C16 C17 -4.2(3) . . . . ? C14 C15 C16 C18 -2.8(3) . . . . ? C13 C15 C16 C18 173.2(2) . . . . ? C18 C16 C17 C20 -1.5(3) . . . 1_565 ? C15 C16 C17 C20 176.0(2) . . . 1_565 ? C17 C16 C18 C41 1.6(3) . . . 1_565 ? C15 C16 C18 C41 -176.0(2) . . . 1_565 ? C41 N8 C20 C17 1.6(3) . . . 1_545 ? Cd2 N8 C20 C17 -179.60(18) . . . 1_545 ? C27 C21 C23 C22 1.1(3) . . . . ? C27 C21 C23 C23 -179.6(2) . . . 2_675 ? C28 C22 C23 C21 -1.1(3) . . . . ? C28 C22 C23 C23 179.6(2) . . . 2_675 ? C28 N1 C27 C21 -1.7(3) . . . . ? Cd1 N1 C27 C21 176.81(17) . . . . ? C23 C21 C27 N1 0.3(4) . . . . ? C27 N1 C28 C22 1.7(3) . . . . ? Cd1 N1 C28 C22 -176.82(16) . . . . ? C23 C22 C28 N1 -0.3(3) . . . . ? C20 N8 C41 C18 -1.5(3) . . . 1_545 ? Cd2 N8 C41 C18 179.65(18) . . . 1_545 ? C92 N11 C91 C95 -0.2(3) . . . . ? C91 N11 C92 C96 0.2(4) . . . . ? C94 N12 C93 C99 -1.9(4) . . . . ? C93 N12 C94 C100 1.6(4) . . . . ? N11 C91 C95 C97 -0.2(4) . . . . ? N11 C92 C96 C97 0.1(4) . . . . ? C92 C96 C97 C95 -0.5(3) . . . . ? C92 C96 C97 C98 179.1(2) . . . . ? C91 C95 C97 C96 0.5(3) . . . . ? C91 C95 C97 C98 -179.0(2) . . . . ? C96 C97 C98 C99 177.0(2) . . . . ? C95 C97 C98 C99 -3.5(3) . . . . ? C96 C97 C98 C100 -2.8(3) . . . . ? C95 C97 C98 C100 176.7(2) . . . . ? N12 C93 C99 C98 0.3(4) . . . . ? C100 C98 C99 C93 1.6(3) . . . . ? C97 C98 C99 C93 -178.2(2) . . . . ? N12 C94 C100 C98 0.3(4) . . . . ? C99 C98 C100 C94 -1.9(4) . . . . ? C97 C98 C100 C94 177.9(2) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.73 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.642 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.081 # Attachment '- SLUG-24.cif' data_xsc1009a _database_code_depnum_ccdc_archive 'CCDC 790078' #TrackingRef '- SLUG-24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19.50 H27 Cd1.50 N3 O15 S3' _chemical_formula_weight 808.22 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 11.7810(10) _cell_length_b 11.7810(10) _cell_length_c 12.6868(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1524.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8126 _cell_measurement_theta_min 5.121 _cell_measurement_theta_max 58.634 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.760 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 810 _exptl_absorpt_coefficient_mu 1.332 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6571 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 1432 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 28.24 _reflns_number_total 1432 _reflns_number_gt 1401 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-II v2.1-4' _computing_cell_refinement 'Bruker SAINT v7.34' _computing_data_reduction 'Bruker SAINT v7.34' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+0.5225P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1432 _refine_ls_number_parameters 142 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0176 _refine_ls_R_factor_gt 0.0169 _refine_ls_wR_factor_ref 0.0412 _refine_ls_wR_factor_gt 0.0409 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Cd1 Cd 0.552075(19) 0.0000 0.1667 0.01217(7) Uani 1 2 d S . . S3 S 0.68126(7) 0.52177(7) 0.17508(5) 0.01594(14) Uani 1 1 d . . . C3 C 0.1127(3) 0.0000 0.1667 0.0162(8) Uani 1 2 d S . . N1 N 0.3510(3) 0.0000 0.1667 0.0140(7) Uani 1 2 d S . . O1 O 0.66062(19) 0.20861(17) 0.09550(14) 0.0172(4) Uani 1 1 d . . . H1B H 0.6545 0.2611 0.1367 0.026 Uiso 1 1 calc R . . C2 C 0.1164(3) -0.1158(3) 0.1536(2) 0.0190(6) Uani 1 1 d . . . H2A H 0.0375 -0.1971 0.1453 0.023 Uiso 1 1 calc R . . C1 C 0.2371(3) -0.1104(3) 0.1529(2) 0.0182(6) Uani 1 1 d . . . H1A H 0.2384 -0.1895 0.1422 0.022 Uiso 1 1 calc R . . C7 C 0.5987(4) 0.5987(4) 0.0000 0.0249(9) Uani 1 2 d S . . N2 N 0.7493(2) 0.0000 0.1667 0.0147(7) Uani 1 2 d S . . C8 C 0.5675(3) 0.4807(3) 0.0694(2) 0.0219(6) Uani 1 1 d . . . H8A H 0.5687 0.4118 0.0255 0.026 Uiso 1 1 calc R . . H8B H 0.4781 0.4446 0.0987 0.026 Uiso 1 1 calc R . . O2 O 0.4797(2) -0.0980(2) 0.00822(15) 0.0231(4) Uani 1 1 d . . . H2B H 0.5346 -0.1159 -0.0176 0.035 Uiso 1 1 calc R . . C4 C 0.8589(3) 0.1012(3) 0.1280(2) 0.0192(6) Uani 1 1 d . . . H4A H 0.8548 0.1741 0.1006 0.023 Uiso 1 1 calc R . . O3 O 0.6502(2) 0.39530(19) 0.22271(15) 0.0205(4) Uani 1 1 d . . . O4 O 0.8128(2) 0.5903(2) 0.12991(16) 0.0228(4) Uani 1 1 d . . . O5 O 0.65763(19) 0.60267(18) 0.24759(14) 0.0191(4) Uani 1 1 d . . . C5 C 0.9777(3) 0.1047(3) 0.1262(2) 0.0203(6) Uani 1 1 d . . . H5A H 1.0528 0.1783 0.0973 0.024 Uiso 1 1 calc R . . C6 C 0.9868(3) 0.0000 0.1667 0.0148(7) Uani 1 2 d S . . H8 H 0.619(3) 0.673(3) 0.044(2) 0.031(10) Uiso 1 1 d . . . H2 H 0.458(4) -0.043(5) -0.025(3) 0.049(12) Uiso 1 1 d . . . H1 H 0.642(4) 0.221(4) 0.031(3) 0.042(11) 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 Cd1 0.01004(9) 0.01262(13) 0.01471(11) 0.00014(10) 0.00007(5) 0.00631(6) S3 0.0186(3) 0.0159(3) 0.0146(3) 0.0004(2) 0.0013(2) 0.0095(3) C3 0.0133(13) 0.018(2) 0.0188(19) 0.0041(15) 0.0020(8) 0.0090(10) N1 0.0127(11) 0.0143(17) 0.0155(15) 0.0004(12) 0.0002(6) 0.0071(8) O1 0.0210(10) 0.0149(9) 0.0177(9) 0.0012(7) 0.0009(8) 0.0105(8) C2 0.0128(13) 0.0141(13) 0.0292(16) -0.0034(11) -0.0017(11) 0.0062(11) C1 0.0159(13) 0.0162(14) 0.0248(15) 0.0006(11) 0.0004(11) 0.0097(11) C7 0.0237(15) 0.0237(15) 0.024(2) 0.0033(9) -0.0033(9) 0.0098(18) N2 0.0107(12) 0.0142(15) 0.0205(16) 0.0003(12) 0.0001(6) 0.0071(7) C8 0.0254(14) 0.0200(14) 0.0181(13) 0.0010(10) -0.0048(11) 0.0098(11) O2 0.0298(11) 0.0299(11) 0.0192(10) -0.0043(8) -0.0036(8) 0.0221(9) C4 0.0146(12) 0.0164(13) 0.0277(14) 0.0047(11) 0.0020(11) 0.0087(11) O3 0.0301(11) 0.0166(10) 0.0174(9) 0.0002(8) -0.0005(8) 0.0136(9) O4 0.0204(10) 0.0257(11) 0.0238(10) 0.0018(8) 0.0055(8) 0.0127(9) O5 0.0225(10) 0.0170(9) 0.0184(9) 0.0004(7) 0.0051(8) 0.0103(8) C5 0.0156(13) 0.0146(13) 0.0284(16) 0.0039(11) 0.0020(11) 0.0057(11) C6 0.0101(12) 0.0207(19) 0.0171(18) -0.0035(15) -0.0017(8) 0.0103(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 Cd1 O2 2.2618(19) 5 ? Cd1 O2 2.2618(19) . ? Cd1 O1 2.3125(18) 5 ? Cd1 O1 2.3125(18) . ? Cd1 N2 2.323(3) . ? Cd1 N1 2.369(3) . ? S3 O5 1.4483(19) . ? S3 O4 1.459(2) . ? S3 O3 1.474(2) . ? S3 C8 1.783(3) . ? C3 C2 1.396(3) 5 ? C3 C2 1.396(3) . ? C3 C6 1.484(5) 1_455 ? N1 C1 1.333(3) 5 ? N1 C1 1.333(3) . ? C2 C1 1.392(4) . ? C7 C8 1.526(4) . ? C7 C8 1.527(4) 4 ? N2 C4 1.338(3) 5 ? N2 C4 1.338(3) . ? C4 C5 1.379(4) . ? C5 C6 1.389(3) . ? C6 C5 1.389(3) 5 ? C6 C3 1.484(5) 1_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 O2 Cd1 O2 166.03(10) 5 . ? O2 Cd1 O1 93.57(7) 5 5 ? O2 Cd1 O1 86.73(7) . 5 ? O2 Cd1 O1 86.73(7) 5 . ? O2 Cd1 O1 93.57(7) . . ? O1 Cd1 O1 177.52(9) 5 . ? O2 Cd1 N2 96.98(5) 5 . ? O2 Cd1 N2 96.98(5) . . ? O1 Cd1 N2 88.76(5) 5 . ? O1 Cd1 N2 88.76(5) . . ? O2 Cd1 N1 83.02(5) 5 . ? O2 Cd1 N1 83.02(5) . . ? O1 Cd1 N1 91.24(5) 5 . ? O1 Cd1 N1 91.24(5) . . ? N2 Cd1 N1 180.0 . . ? O5 S3 O4 112.67(12) . . ? O5 S3 O3 111.87(11) . . ? O4 S3 O3 112.24(12) . . ? O5 S3 C8 106.90(13) . . ? O4 S3 C8 107.49(13) . . ? O3 S3 C8 105.14(12) . . ? C2 C3 C2 117.4(4) 5 . ? C2 C3 C6 121.3(2) 5 1_455 ? C2 C3 C6 121.3(2) . 1_455 ? C1 N1 C1 117.6(4) 5 . ? C1 N1 Cd1 121.2(2) 5 . ? C1 N1 Cd1 121.2(2) . . ? C1 C2 C3 119.1(3) . . ? N1 C1 C2 123.4(3) . . ? C8 C7 C8 109.7(4) . 4 ? C4 N2 C4 117.3(3) 5 . ? C4 N2 Cd1 121.33(17) 5 . ? C4 N2 Cd1 121.33(17) . . ? C7 C8 S3 112.4(2) . . ? N2 C4 C5 123.1(3) . . ? C4 C5 C6 119.7(3) . . ? C5 C6 C5 117.2(4) 5 . ? C5 C6 C3 121.42(18) 5 1_655 ? C5 C6 C3 121.42(18) . 1_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Cd1 N1 C1 54.78(15) 5 . . 5 ? O2 Cd1 N1 C1 -125.22(15) . . . 5 ? O1 Cd1 N1 C1 148.23(14) 5 . . 5 ? O1 Cd1 N1 C1 -31.77(14) . . . 5 ? N2 Cd1 N1 C1 0(17) . . . 5 ? O2 Cd1 N1 C1 -125.22(15) 5 . . . ? O2 Cd1 N1 C1 54.78(15) . . . . ? O1 Cd1 N1 C1 -31.77(14) 5 . . . ? O1 Cd1 N1 C1 148.23(14) . . . . ? N2 Cd1 N1 C1 0(100) . . . . ? C2 C3 C2 C1 -0.8(2) 5 . . . ? C6 C3 C2 C1 179.2(2) 1_455 . . . ? C1 N1 C1 C2 -0.8(2) 5 . . . ? Cd1 N1 C1 C2 179.2(2) . . . . ? C3 C2 C1 N1 1.6(4) . . . . ? O2 Cd1 N2 C4 91.05(15) 5 . . 5 ? O2 Cd1 N2 C4 -88.95(15) . . . 5 ? O1 Cd1 N2 C4 -2.39(15) 5 . . 5 ? O1 Cd1 N2 C4 177.60(15) . . . 5 ? N1 Cd1 N2 C4 0(100) . . . 5 ? O2 Cd1 N2 C4 -88.95(15) 5 . . . ? O2 Cd1 N2 C4 91.05(15) . . . . ? O1 Cd1 N2 C4 177.61(15) 5 . . . ? O1 Cd1 N2 C4 -2.40(15) . . . . ? N1 Cd1 N2 C4 0(28) . . . . ? C8 C7 C8 S3 -164.9(2) 4 . . . ? O5 S3 C8 C7 69.8(2) . . . . ? O4 S3 C8 C7 -51.4(2) . . . . ? O3 S3 C8 C7 -171.18(17) . . . . ? C4 N2 C4 C5 0.3(2) 5 . . . ? Cd1 N2 C4 C5 -179.7(2) . . . . ? N2 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C5 0.3(2) . . . 5 ? C4 C5 C6 C3 -179.7(2) . . . 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O3 0.84 1.94 2.780(3) 174.6 . O2 H2B O4 0.84 1.93 2.691(3) 150.4 4_545 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.274 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.067 # Attachment '- SLUG-25.cif' data_xsc1010a _database_code_depnum_ccdc_archive 'CCDC 790079' #TrackingRef '- SLUG-25.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H30 Cd1.50 N3 O15 S3' _chemical_formula_weight 829.26 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M P3(2)21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 11.8001(8) _cell_length_b 11.8001(8) _cell_length_c 12.7024(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1531.75(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 5.115 _cell_measurement_theta_max 59.216 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 1.328 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6542 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II' _diffrn_measurement_method \w/2\q-scans _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number . _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% . _diffrn_reflns_number 17382 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0143 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 28.28 _reflns_number_total 2546 _reflns_number_gt 2535 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX-II v2.1-4' _computing_cell_refinement 'Bruker SAINT v7.34' _computing_data_reduction 'Bruker SAINT v7.34' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0251P)^2^+1.0233P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2546 _refine_ls_number_parameters 150 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0180 _refine_ls_R_factor_gt 0.0179 _refine_ls_wR_factor_ref 0.0472 _refine_ls_wR_factor_gt 0.0471 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.007 _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 Cd1 Cd 0.532768(15) 0.0000 0.1667 0.01228(5) Uani 1 2 d S . . C3 C 0.9677(2) 0.0000 0.1667 0.0139(6) Uani 1 2 d S . . S3 S 1.18257(5) 0.45634(5) 0.12903(4) 0.01891(11) Uani 1 1 d . . . N1 N 0.7296(2) 0.0000 0.1667 0.0159(4) Uani 1 2 d S . . O2 O 1.24876(18) 0.59838(17) 0.11118(14) 0.0266(4) Uani 1 1 d . . . O3 O 1.21070(16) 0.42306(18) 0.23261(12) 0.0245(3) Uani 1 1 d . . . C2 C 0.8505(2) -0.1113(2) 0.13733(16) 0.0165(4) Uani 1 1 d . . . H2A H 0.8502 -0.1885 0.1158 0.020 Uiso 1 1 calc R . . C4 C 1.0933(2) 0.0000 0.1667 0.0144(5) Uani 1 2 d S . . N2 N 0.3319(2) 0.0000 0.1667 0.0147(5) Uani 1 2 d S . . O1 O 1.04266(16) 0.39241(16) 0.10875(13) 0.0236(3) Uani 1 1 d . . . C8 C 1.2460(2) 0.3913(2) 0.03398(18) 0.0241(4) Uani 1 1 d . . . H8A H 1.2001 0.2949 0.0416 0.029 Uiso 1 1 calc R . . H8B H 1.2267 0.4112 -0.0373 0.029 Uiso 1 1 calc R . . C1 C 0.7346(2) -0.1075(2) 0.13994(16) 0.0171(4) Uani 1 1 d . . . H1A H 0.6553 -0.1846 0.1220 0.021 Uiso 1 1 calc R . . C7 C 1.3928(2) 0.4446(3) 0.0434(2) 0.0292(5) Uani 1 1 d . . . H7A H 1.4120 0.4199 0.1128 0.035 Uiso 1 1 calc R . . H7B H 1.4389 0.5413 0.0397 0.035 Uiso 1 1 calc R . . O4 O 0.64730(17) 0.20957(15) 0.09915(13) 0.0209(3) Uani 1 1 d . . . H4A H 0.6434 0.2621 0.1416 0.031 Uiso 1 1 calc R . . O5 O 0.56529(16) 0.09307(18) 0.32698(12) 0.0238(3) Uani 1 1 d . . . H5B H 0.6441 0.1246 0.3443 0.036 Uiso 1 1 calc R . . C5 C 1.1106(2) -0.0893(2) 0.10646(17) 0.0177(4) Uani 1 1 d . . . C6 C 0.2303(2) -0.0852(2) 0.10840(16) 0.0173(4) Uani 1 1 d . . . H6 H 0.244(3) -0.141(3) 0.064(2) 0.027(7) Uiso 1 1 d . . . H5 H 1.046(3) -0.147(3) 0.064(2) 0.028(8) Uiso 1 1 d . . . H4B H 0.646(3) 0.227(3) 0.042(3) 0.032(8) Uiso 1 1 d . . . H5A H 0.511(4) 0.054(3) 0.370(3) 0.035(9) 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 Cd1 0.00952(7) 0.01386(10) 0.01492(8) -0.00013(7) -0.00007(4) 0.00693(5) C3 0.0091(8) 0.0187(15) 0.0170(12) 0.0022(10) 0.0011(5) 0.0093(7) S3 0.0176(2) 0.0189(3) 0.0183(2) -0.00129(19) -0.00389(18) 0.0077(2) N1 0.0117(7) 0.0160(10) 0.0214(11) 0.0019(8) 0.0010(4) 0.0080(5) O2 0.0290(9) 0.0169(8) 0.0266(8) -0.0012(6) -0.0026(7) 0.0059(7) O3 0.0193(8) 0.0300(9) 0.0184(7) 0.0030(7) -0.0043(6) 0.0079(7) C2 0.0139(9) 0.0144(9) 0.0221(10) 0.0003(7) 0.0007(7) 0.0077(7) C4 0.0126(9) 0.0155(13) 0.0161(12) 0.0024(10) 0.0012(5) 0.0078(7) N2 0.0119(8) 0.0179(12) 0.0163(11) 0.0021(9) 0.0010(5) 0.0090(6) O1 0.0189(7) 0.0204(8) 0.0315(8) -0.0019(7) -0.0086(6) 0.0098(6) C8 0.0229(11) 0.0263(11) 0.0246(10) -0.0059(9) -0.0042(9) 0.0134(9) C1 0.0125(9) 0.0163(10) 0.0233(9) 0.0006(8) -0.0005(7) 0.0078(8) C7 0.0219(10) 0.0270(12) 0.0353(12) -0.0067(10) -0.0012(9) 0.0097(10) O4 0.0253(8) 0.0149(7) 0.0217(7) 0.0024(6) 0.0009(6) 0.0095(6) O5 0.0149(7) 0.0326(9) 0.0172(7) -0.0043(6) -0.0006(6) 0.0068(7) C5 0.0134(9) 0.0189(10) 0.0207(9) -0.0034(8) -0.0031(8) 0.0080(8) C6 0.0150(9) 0.0197(10) 0.0201(9) -0.0019(8) 0.0001(8) 0.0110(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 O5 2.2536(15) 5 ? Cd1 O5 2.2536(15) . ? Cd1 O4 2.3098(15) 5 ? Cd1 O4 2.3098(15) . ? Cd1 N1 2.323(3) . ? Cd1 N2 2.370(2) . ? C3 C2 1.400(2) . ? C3 C2 1.400(2) 5 ? C3 C4 1.482(4) . ? S3 O1 1.4546(16) . ? S3 O3 1.4580(16) . ? S3 O2 1.4703(18) . ? S3 C8 1.783(2) . ? N1 C1 1.343(2) 5 ? N1 C1 1.343(2) . ? C2 C1 1.391(3) . ? C4 C5 1.397(3) 5 ? C4 C5 1.397(3) . ? N2 C6 1.339(3) 5 ? N2 C6 1.339(3) . ? C8 C7 1.524(3) . ? C7 C7 1.528(5) 4_645 ? C5 C6 1.389(3) 1_655 ? C6 C5 1.389(3) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Cd1 O5 171.58(8) 5 . ? O5 Cd1 O4 87.01(6) 5 5 ? O5 Cd1 O4 93.41(6) . 5 ? O5 Cd1 O4 93.41(6) 5 . ? O5 Cd1 O4 87.01(6) . . ? O4 Cd1 O4 174.29(9) 5 . ? O5 Cd1 N1 94.21(4) 5 . ? O5 Cd1 N1 94.21(4) . . ? O4 Cd1 N1 87.14(4) 5 . ? O4 Cd1 N1 87.14(4) . . ? O5 Cd1 N2 85.79(4) 5 . ? O5 Cd1 N2 85.79(4) . . ? O4 Cd1 N2 92.86(4) 5 . ? O4 Cd1 N2 92.86(4) . . ? N1 Cd1 N2 180.0 . . ? C2 C3 C2 117.5(2) . 5 ? C2 C3 C4 121.27(12) . . ? C2 C3 C4 121.27(12) 5 . ? O1 S3 O3 111.86(10) . . ? O1 S3 O2 112.47(10) . . ? O3 S3 O2 112.55(11) . . ? O1 S3 C8 105.57(10) . . ? O3 S3 C8 107.10(11) . . ? O2 S3 C8 106.76(11) . . ? C1 N1 C1 117.9(3) 5 . ? C1 N1 Cd1 121.07(13) 5 . ? C1 N1 Cd1 121.07(13) . . ? C1 C2 C3 119.4(2) . . ? C5 C4 C5 116.9(3) 5 . ? C5 C4 C3 121.54(13) 5 . ? C5 C4 C3 121.54(13) . . ? C6 N2 C6 117.3(2) 5 . ? C6 N2 Cd1 121.37(12) 5 . ? C6 N2 Cd1 121.37(12) . . ? C7 C8 S3 113.84(16) . . ? N1 C1 C2 123.0(2) . . ? C8 C7 C7 112.22(17) . 4_645 ? C6 C5 C4 119.6(2) 1_655 . ? N2 C6 C5 123.3(2) . 1_455 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Cd1 N1 C1 132.20(11) 5 . . 5 ? O5 Cd1 N1 C1 -47.80(11) . . . 5 ? O4 Cd1 N1 C1 -141.01(11) 5 . . 5 ? O4 Cd1 N1 C1 38.99(11) . . . 5 ? N2 Cd1 N1 C1 0(19) . . . 5 ? O5 Cd1 N1 C1 -47.80(11) 5 . . . ? O5 Cd1 N1 C1 132.20(11) . . . . ? O4 Cd1 N1 C1 38.99(11) 5 . . . ? O4 Cd1 N1 C1 -141.01(11) . . . . ? N2 Cd1 N1 C1 0(100) . . . . ? C2 C3 C2 C1 -0.93(14) 5 . . . ? C4 C3 C2 C1 179.07(14) . . . . ? C2 C3 C4 C5 -158.18(14) . . . 5 ? C2 C3 C4 C5 21.82(14) 5 . . 5 ? C2 C3 C4 C5 21.82(14) . . . . ? C2 C3 C4 C5 -158.18(14) 5 . . . ? O5 Cd1 N2 C6 -155.39(12) 5 . . 5 ? O5 Cd1 N2 C6 24.61(12) . . . 5 ? O4 Cd1 N2 C6 117.82(12) 5 . . 5 ? O4 Cd1 N2 C6 -62.18(12) . . . 5 ? N1 Cd1 N2 C6 0(33) . . . 5 ? O5 Cd1 N2 C6 24.61(12) 5 . . . ? O5 Cd1 N2 C6 -155.39(12) . . . . ? O4 Cd1 N2 C6 -62.18(12) 5 . . . ? O4 Cd1 N2 C6 117.82(12) . . . . ? N1 Cd1 N2 C6 0(100) . . . . ? O1 S3 C8 C7 -178.88(18) . . . . ? O3 S3 C8 C7 -59.5(2) . . . . ? O2 S3 C8 C7 61.2(2) . . . . ? C1 N1 C1 C2 -1.01(15) 5 . . . ? Cd1 N1 C1 C2 178.99(15) . . . . ? C3 C2 C1 N1 2.0(3) . . . . ? S3 C8 C7 C7 -176.6(2) . . . 4_645 ? C5 C4 C5 C6 -0.37(15) 5 . . 1_655 ? C3 C4 C5 C6 179.63(15) . . . 1_655 ? C6 N2 C6 C5 -0.40(17) 5 . . 1_455 ? Cd1 N2 C6 C5 179.60(17) . . . 1_455 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O2 0.84 1.90 2.738(2) 171.1 5_565 O5 H5B O3 0.84 1.88 2.664(2) 154.8 6_765 O4 H4B O2 0.75(3) 2.08(3) 2.820(2) 168(3) 4_545 O5 H5A O1 0.79(4) 1.89(4) 2.664(2) 165(3) 3_665 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.538 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.056