Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Lisa Berreau' 'Russell A. Allred' 'Atta M. Arif' 'Sara A. Heufner' _publ_contact_author_name 'Lisa Berreau' _publ_contact_author_address ; Department of Chemistry Utah State University 0300 Old Main Hill Logan Utah 84322-0300 UNITED STATES OF AMERICA ; _publ_contact_author_email BERREAU@CC.USU.EDU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; A cadmium hydroxide complex of a N3S-donor ligand containing two hydrogen bond donors: Synthesis, characterization, and CO2 reactivity ; # Attachment 'usu064.cif' data_usu06 _database_code_depnum_ccdc_archive 'CCDC 619640' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H89.50 Cd2 Cl2 N10.50 O10 S2' _chemical_formula_weight 1393.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8238(2) _cell_length_b 16.8615(2) _cell_length_c 15.0661(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.7013(6) _cell_angle_gamma 90.00 _cell_volume 3257.48(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 6806 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1446 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8141 _exptl_absorpt_correction_T_max 0.8609 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi plus Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.0 _diffrn_reflns_number 13004 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 27.48 _reflns_number_total 7397 _reflns_number_gt 5914 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _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^)+(0.0453P)^2^+3.1822P] 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 7397 _refine_ls_number_parameters 410 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.1049 _refine_ls_wR_factor_gt 0.0945 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.099413(15) 0.055476(11) 0.043728(13) 0.03232(8) Uani 1 1 d . . . Cl1 Cl -0.05765(8) -0.23464(7) 0.25819(7) 0.0746(3) Uani 1 1 d . . . S1 S 0.21593(11) 0.07363(8) 0.20253(9) 0.0314(3) Uani 0.50 1 d P A 1 C1 C 0.2233(5) -0.0535(4) 0.3083(4) 0.117(2) Uani 1 1 d . . . H1A H 0.2094 -0.0157 0.3561 0.175 Uiso 1 1 calc R B 1 H1B H 0.2614 -0.0992 0.3323 0.175 Uiso 1 1 calc R B 1 H1C H 0.1570 -0.0714 0.2820 0.175 Uiso 1 1 calc R B 1 C2 C 0.2889(5) -0.0131(4) 0.2369(5) 0.0478(15) Uani 0.50 1 d P A 1 H2A H 0.2994 -0.0492 0.1860 0.057 Uiso 0.50 1 calc PR A 1 H2B H 0.3579 0.0024 0.2614 0.057 Uiso 0.50 1 calc PR A 1 S1' S 0.27175(13) 0.02696(11) 0.16074(12) 0.0504(4) Uani 0.50 1 d P A 2 C2' C 0.2366(10) 0.0428(7) 0.2732(7) 0.101(4) Uani 0.50 1 d P A 2 H2C H 0.2921 0.0709 0.3068 0.121 Uiso 0.50 1 calc PR A 2 H2D H 0.1704 0.0726 0.2777 0.121 Uiso 0.50 1 calc PR A 2 O1 O 0.01511(18) -0.05347(13) 0.06990(16) 0.0454(6) Uani 1 1 d . . . H1 H 0.015(3) -0.078(2) 0.111(2) 0.037(9) Uiso 1 1 d . . . O2 O -0.0160(3) -0.1745(2) 0.2056(2) 0.1003(12) Uani 1 1 d . C . O3 O -0.0091(2) -0.23921(19) 0.3421(2) 0.0790(9) Uani 1 1 d . C . O4 O -0.1607(8) -0.2422(6) 0.2580(10) 0.109(5) Uani 0.50 1 d P C 1 O5 O -0.0189(6) -0.3145(3) 0.2136(4) 0.0707(16) Uani 0.50 1 d P C 1 O4' O -0.1666(8) -0.1939(7) 0.2827(9) 0.103(4) Uani 0.50 1 d P C 2 O5' O -0.0920(12) -0.2961(8) 0.2124(9) 0.163(5) Uiso 0.50 1 d P C 2 N1 N 0.2018(2) 0.17168(15) 0.01916(18) 0.0434(6) Uani 1 1 d . A . N2 N 0.0168(2) 0.16228(16) 0.11526(18) 0.0460(6) Uani 1 1 d . A . N3 N -0.0824(3) 0.0828(2) 0.2057(2) 0.0573(8) Uani 1 1 d . . . H3N H -0.051(3) 0.048(2) 0.183(3) 0.058(13) Uiso 1 1 d . . . N4 N 0.24429(18) 0.01415(15) -0.03794(18) 0.0399(6) Uani 1 1 d . A . N5 N 0.2222(2) -0.11828(16) -0.0063(2) 0.0475(7) Uani 1 1 d . . . H5N H 0.169(3) -0.103(2) 0.018(2) 0.044(10) Uiso 1 1 d . . . C3 C 0.3218(4) 0.1239(3) 0.1380(4) 0.0931(18) Uani 1 1 d . . . H3A H 0.3783 0.1420 0.1786 0.112 Uiso 0.50 1 calc PR A 1 H3B H 0.3518 0.0868 0.0943 0.112 Uiso 0.50 1 calc PR A 1 H3C H 0.3434 0.1449 0.1968 0.112 Uiso 0.50 1 calc PR A 2 H3D H 0.3873 0.1142 0.1057 0.112 Uiso 0.50 1 calc PR A 2 C4 C 0.2745(3) 0.1912(2) 0.0928(3) 0.0614(10) Uani 1 1 d . A . H4A H 0.3309 0.2250 0.0692 0.074 Uiso 1 1 calc R . . H4B H 0.2364 0.2231 0.1371 0.074 Uiso 1 1 calc R . . C5 C 0.1230(3) 0.23506(18) 0.0104(3) 0.0508(8) Uani 1 1 d . . . H5A H 0.0847 0.2285 -0.0466 0.061 Uiso 1 1 calc R A . H5B H 0.1587 0.2871 0.0091 0.061 Uiso 1 1 calc R . . C6 C 0.0462(3) 0.23428(19) 0.0855(2) 0.0495(8) Uani 1 1 d . A . C7 C 0.0044(3) 0.3037(2) 0.1177(3) 0.0601(10) Uani 1 1 d . . . H7 H 0.0277 0.3539 0.0972 0.072 Uiso 1 1 calc R A . C8 C -0.0736(3) 0.2977(2) 0.1815(3) 0.0617(10) Uani 1 1 d . A . H8 H -0.1052 0.3444 0.2038 0.074 Uiso 1 1 calc R . . C9 C -0.1047(3) 0.2257(2) 0.2120(2) 0.0551(9) Uani 1 1 d . . . H9 H -0.1576 0.2220 0.2554 0.066 Uiso 1 1 calc R A . C10 C -0.0576(3) 0.1570(2) 0.1784(2) 0.0485(8) Uani 1 1 d . A . C11 C -0.1726(3) 0.0610(2) 0.2593(3) 0.0563(9) Uani 1 1 d . . . H11A H -0.2045 0.0127 0.2332 0.068 Uiso 1 1 calc R . . H11B H -0.2248 0.1041 0.2543 0.068 Uiso 1 1 calc R . . C12 C -0.1517(3) 0.04549(19) 0.3569(3) 0.0528(8) Uani 1 1 d . . . C13 C -0.1203(4) 0.1219(3) 0.4053(3) 0.0813(14) Uani 1 1 d . . . H13A H -0.0555 0.1425 0.3802 0.122 Uiso 1 1 calc R . . H13B H -0.1096 0.1107 0.4686 0.122 Uiso 1 1 calc R . . H13C H -0.1757 0.1615 0.3979 0.122 Uiso 1 1 calc R . . C14 C -0.2540(4) 0.0159(3) 0.3969(4) 0.0967(17) Uani 1 1 d . . . H14A H -0.3101 0.0536 0.3830 0.145 Uiso 1 1 calc R . . H14B H -0.2458 0.0114 0.4615 0.145 Uiso 1 1 calc R . . H14C H -0.2716 -0.0361 0.3719 0.145 Uiso 1 1 calc R . . C15 C -0.0672(5) -0.0159(3) 0.3696(5) 0.111(2) Uani 1 1 d . . . H15A H -0.0861 -0.0642 0.3371 0.166 Uiso 1 1 calc R . . H15B H -0.0594 -0.0282 0.4330 0.166 Uiso 1 1 calc R . . H15C H -0.0012 0.0048 0.3472 0.166 Uiso 1 1 calc R . . C16 C 0.2541(2) 0.15620(19) -0.0661(2) 0.0464(8) Uani 1 1 d . . . H16A H 0.3108 0.1954 -0.0735 0.056 Uiso 1 1 calc R A . H16B H 0.2031 0.1644 -0.1152 0.056 Uiso 1 1 calc R . . C17 C 0.2992(2) 0.0745(2) -0.0740(2) 0.0445(7) Uani 1 1 d . A . C18 C 0.3890(3) 0.0615(2) -0.1205(3) 0.0552(9) Uani 1 1 d . . . H18 H 0.4267 0.1045 -0.1451 0.066 Uiso 1 1 calc R A . C19 C 0.4234(3) -0.0162(3) -0.1308(3) 0.0635(10) Uani 1 1 d . A . H19 H 0.4845 -0.0265 -0.1640 0.076 Uiso 1 1 calc R . . C20 C 0.3703(3) -0.0776(2) -0.0938(3) 0.0559(9) Uani 1 1 d . . . H20 H 0.3944 -0.1306 -0.1001 0.067 Uiso 1 1 calc R A . C21 C 0.2792(2) -0.06111(18) -0.0460(2) 0.0430(7) Uani 1 1 d . A . C22 C 0.2394(2) -0.20309(17) -0.0138(2) 0.0422(7) Uani 1 1 d . . . H22A H 0.2796 -0.2132 -0.0684 0.051 Uiso 1 1 calc R . . H22B H 0.1709 -0.2295 -0.0212 0.051 Uiso 1 1 calc R . . C23 C 0.2973(3) -0.24165(19) 0.0649(2) 0.0472(8) Uani 1 1 d . . . C24 C 0.2329(4) -0.2317(3) 0.1479(3) 0.0845(14) Uani 1 1 d . . . H24A H 0.2683 -0.2578 0.1980 0.127 Uiso 1 1 calc R . . H24B H 0.1641 -0.2558 0.1385 0.127 Uiso 1 1 calc R . . H24C H 0.2246 -0.1751 0.1609 0.127 Uiso 1 1 calc R . . C25 C 0.4054(3) -0.2055(2) 0.0769(3) 0.0713(12) Uani 1 1 d . . . H25A H 0.4389 -0.2279 0.1301 0.107 Uiso 1 1 calc R . . H25B H 0.3991 -0.1479 0.0836 0.107 Uiso 1 1 calc R . . H25C H 0.4476 -0.2175 0.0248 0.107 Uiso 1 1 calc R . . C26 C 0.3087(3) -0.3296(2) 0.0419(3) 0.0674(11) Uani 1 1 d . . . H26A H 0.3485 -0.3350 -0.0129 0.101 Uiso 1 1 calc R . . H26B H 0.2394 -0.3531 0.0334 0.101 Uiso 1 1 calc R . . H26C H 0.3454 -0.3569 0.0904 0.101 Uiso 1 1 calc R . . N6 N 0.544(2) -0.0208(19) 0.5691(14) 0.141(9) Uiso 0.25 1 d PD D -1 C27 C 0.5000 0.0000 0.5000 0.136(7) Uiso 0.50 2 d SPD D -1 C28 C 0.475(4) 0.058(2) 0.418(2) 0.20(2) Uiso 0.25 1 d PD D -1 H28A H 0.4251 0.0328 0.3771 0.307 Uiso 0.25 1 calc PR D -1 H28B H 0.5398 0.0696 0.3860 0.307 Uiso 0.25 1 calc PR D -1 H28C H 0.4455 0.1080 0.4398 0.307 Uiso 0.25 1 calc PR D -1 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 0.02708(12) 0.03171(12) 0.03801(13) 0.00293(8) -0.00639(8) -0.00721(7) Cl1 0.0642(6) 0.0934(8) 0.0657(6) 0.0342(6) -0.0202(5) -0.0233(5) S1 0.0308(7) 0.0322(7) 0.0311(7) -0.0038(5) -0.0065(5) 0.0011(5) C1 0.112(5) 0.154(6) 0.084(4) 0.045(4) 0.002(3) -0.002(4) C2 0.046(4) 0.043(4) 0.054(4) 0.009(3) -0.001(3) 0.011(3) S1' 0.0407(9) 0.0510(9) 0.0591(10) -0.0005(8) -0.0161(8) 0.0009(7) C2' 0.114(9) 0.127(10) 0.062(6) -0.044(6) -0.012(6) 0.034(7) O1 0.0448(13) 0.0456(13) 0.0452(13) 0.0213(11) -0.0192(10) -0.0213(10) O2 0.085(2) 0.116(3) 0.100(3) 0.060(2) -0.0012(19) -0.020(2) O3 0.079(2) 0.088(2) 0.0700(18) 0.0147(16) -0.0241(15) 0.0188(16) O4 0.041(4) 0.126(8) 0.158(12) 0.077(8) -0.016(6) 0.006(6) O5 0.087(4) 0.059(3) 0.066(4) -0.010(3) -0.023(3) -0.007(3) O4' 0.040(4) 0.169(11) 0.100(6) 0.028(8) -0.001(3) 0.009(7) N1 0.0396(14) 0.0419(14) 0.0483(15) 0.0064(12) -0.0108(11) -0.0153(11) N2 0.0466(15) 0.0415(14) 0.0500(15) -0.0085(12) -0.0001(12) -0.0083(12) N3 0.0521(18) 0.0521(18) 0.068(2) -0.0093(16) 0.0190(16) -0.0071(15) N4 0.0256(12) 0.0388(14) 0.0554(16) 0.0097(12) -0.0028(11) -0.0050(10) N5 0.0278(13) 0.0365(14) 0.078(2) 0.0073(13) 0.0069(13) 0.0019(11) C3 0.092(3) 0.067(3) 0.118(4) 0.035(3) -0.077(3) -0.043(2) C4 0.053(2) 0.064(2) 0.066(2) 0.0075(19) -0.0221(18) -0.0270(18) C5 0.056(2) 0.0315(16) 0.064(2) -0.0001(15) -0.0039(17) -0.0118(14) C6 0.0519(19) 0.0397(17) 0.057(2) -0.0096(15) -0.0097(16) -0.0076(14) C7 0.073(3) 0.0411(18) 0.066(2) -0.0109(17) -0.018(2) -0.0025(17) C8 0.077(3) 0.054(2) 0.053(2) -0.0187(18) -0.0159(19) 0.0183(19) C9 0.058(2) 0.060(2) 0.0469(19) -0.0086(17) -0.0103(16) 0.0129(17) C10 0.0415(17) 0.0515(19) 0.0523(19) -0.0113(16) -0.0053(15) -0.0019(14) C11 0.0384(18) 0.061(2) 0.070(2) -0.0148(18) 0.0073(17) -0.0100(15) C12 0.050(2) 0.0396(17) 0.069(2) 0.0031(16) 0.0045(17) -0.0008(14) C13 0.129(4) 0.058(2) 0.056(2) 0.006(2) -0.023(3) -0.016(3) C14 0.093(4) 0.098(4) 0.100(4) -0.004(3) 0.048(3) -0.019(3) C15 0.107(4) 0.078(3) 0.148(5) 0.039(4) 0.016(4) 0.040(3) C16 0.0367(16) 0.0467(18) 0.0558(19) 0.0187(15) -0.0034(14) -0.0105(13) C17 0.0281(15) 0.0510(18) 0.0541(19) 0.0142(15) -0.0065(13) -0.0091(13) C18 0.0274(16) 0.068(2) 0.070(2) 0.0242(19) 0.0006(15) -0.0089(15) C19 0.0288(17) 0.083(3) 0.079(3) 0.017(2) 0.0108(17) 0.0060(17) C20 0.0321(16) 0.056(2) 0.080(3) 0.0071(19) 0.0049(16) 0.0071(15) C21 0.0265(14) 0.0448(17) 0.0575(19) 0.0050(14) -0.0046(13) -0.0017(12) C22 0.0350(16) 0.0361(15) 0.0554(19) -0.0055(14) -0.0072(14) -0.0001(12) C23 0.056(2) 0.0387(17) 0.0463(18) -0.0050(14) -0.0052(15) 0.0103(14) C24 0.121(4) 0.073(3) 0.059(3) 0.001(2) 0.015(3) 0.023(3) C25 0.059(2) 0.065(2) 0.089(3) -0.004(2) -0.039(2) 0.0080(19) C26 0.079(3) 0.0403(19) 0.082(3) -0.0023(19) -0.006(2) 0.0144(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.170(2) . ? Cd1 O1 2.242(2) 3 ? Cd1 N4 2.347(3) . ? Cd1 N2 2.357(3) . ? Cd1 N1 2.390(2) . ? Cd1 S1 2.8218(13) . ? Cd1 S1' 2.8509(16) . ? Cd1 Cd1 3.4139(4) 3 ? Cl1 O5' 1.317(14) . ? Cl1 O4 1.328(11) . ? Cl1 O2 1.397(3) . ? Cl1 O3 1.404(3) . ? Cl1 O5 1.588(6) . ? Cl1 O4' 1.604(11) . ? S1 C2 1.808(6) . ? S1 C3 1.882(5) . ? C1 C2 1.533(8) . ? C1 C2' 1.716(13) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? S1' C2' 1.778(10) . ? S1' C3 1.791(4) . ? C2' H2C 0.9900 . ? C2' H2D 0.9900 . ? O1 Cd1 2.242(2) 3 ? O1 H1 0.74(3) . ? N1 C5 1.475(4) . ? N1 C4 1.478(4) . ? N1 C16 1.480(4) . ? N2 C6 1.349(4) . ? N2 C10 1.359(4) . ? N3 C10 1.357(5) . ? N3 C11 1.466(5) . ? N3 H3N 0.79(4) . ? N4 C21 1.351(4) . ? N4 C17 1.355(4) . ? N5 C21 1.353(4) . ? N5 C22 1.452(4) . ? N5 H5N 0.82(4) . ? C3 C4 1.452(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 H3C 0.9900 . ? C3 H3D 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.510(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.378(5) . ? C7 C8 1.400(6) . ? C7 H7 0.9500 . ? C8 C9 1.358(6) . ? C8 H8 0.9500 . ? C9 C10 1.403(5) . ? C9 H9 0.9500 . ? C11 C12 1.514(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C15 1.509(6) . ? C12 C13 1.532(5) . ? C12 C14 1.534(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.499(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.373(5) . ? C18 C19 1.392(5) . ? C18 H18 0.9500 . ? C19 C20 1.363(5) . ? C19 H19 0.9500 . ? C20 C21 1.409(5) . ? C20 H20 0.9500 . ? C22 C23 1.537(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.516(5) . ? C23 C25 1.522(5) . ? C23 C26 1.530(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? N6 C27 1.227(17) . ? C27 C28 1.612(19) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 O1 78.63(9) . 3 ? O1 Cd1 N4 104.08(9) . . ? O1 Cd1 N4 96.35(9) 3 . ? O1 Cd1 N2 109.64(10) . . ? O1 Cd1 N2 93.83(9) 3 . ? N4 Cd1 N2 146.07(9) . . ? O1 Cd1 N1 176.37(9) . . ? O1 Cd1 N1 104.47(8) 3 . ? N4 Cd1 N1 73.88(9) . . ? N2 Cd1 N1 72.25(10) . . ? O1 Cd1 S1 101.40(7) . . ? O1 Cd1 S1 169.76(7) 3 . ? N4 Cd1 S1 93.57(7) . . ? N2 Cd1 S1 76.45(7) . . ? N1 Cd1 S1 75.89(7) . . ? O1 Cd1 S1' 97.41(7) . . ? O1 Cd1 S1' 164.83(8) 3 . ? N4 Cd1 S1' 70.21(7) . . ? N2 Cd1 S1' 101.27(8) . . ? N1 Cd1 S1' 79.10(7) . . ? S1 Cd1 S1' 25.26(5) . . ? O1 Cd1 Cd1 40.08(6) . 3 ? O1 Cd1 Cd1 38.55(5) 3 3 ? N4 Cd1 Cd1 103.14(6) . 3 ? N2 Cd1 Cd1 104.92(6) . 3 ? N1 Cd1 Cd1 142.99(6) . 3 ? S1 Cd1 Cd1 140.52(3) . 3 ? S1' Cd1 Cd1 135.72(4) . 3 ? O5' Cl1 O4 66.2(7) . . ? O5' Cl1 O2 113.6(6) . . ? O4 Cl1 O2 117.1(5) . . ? O5' Cl1 O3 124.7(6) . . ? O4 Cl1 O3 115.3(6) . . ? O2 Cl1 O3 112.5(2) . . ? O5' Cl1 O5 38.3(6) . . ? O4 Cl1 O5 103.6(6) . . ? O2 Cl1 O5 104.6(3) . . ? O3 Cl1 O5 101.3(3) . . ? O5' Cl1 O4' 99.8(8) . . ? O4 Cl1 O4' 34.1(6) . . ? O2 Cl1 O4' 99.2(5) . . ? O3 Cl1 O4' 101.2(5) . . ? O5 Cl1 O4' 137.6(5) . . ? C2 S1 C3 98.0(3) . . ? C2 S1 Cd1 114.9(2) . . ? C3 S1 Cd1 89.35(13) . . ? C2 C1 C2' 46.1(4) . . ? C2 C1 H1A 109.5 . . ? C2' C1 H1A 68.4 . . ? C2 C1 H1B 109.5 . . ? C2' C1 H1B 143.8 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? C2' C1 H1C 104.8 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 S1 105.9(4) . . ? C1 C2 H2A 110.6 . . ? S1 C2 H2A 110.6 . . ? C1 C2 H2B 110.6 . . ? S1 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? C2' S1' C3 98.1(5) . . ? C2' S1' Cd1 111.1(4) . . ? C3 S1' Cd1 90.27(13) . . ? C1 C2' S1' 100.3(5) . . ? C1 C2' H2C 111.7 . . ? S1' C2' H2C 111.7 . . ? C1 C2' H2D 111.7 . . ? S1' C2' H2D 111.7 . . ? H2C C2' H2D 109.5 . . ? Cd1 O1 Cd1 101.37(9) . 3 ? Cd1 O1 H1 130(3) . . ? Cd1 O1 H1 128(3) 3 . ? C5 N1 C4 109.3(3) . . ? C5 N1 C16 111.5(3) . . ? C4 N1 C16 113.7(3) . . ? C5 N1 Cd1 103.37(18) . . ? C4 N1 Cd1 114.2(2) . . ? C16 N1 Cd1 104.22(18) . . ? C6 N2 C10 119.5(3) . . ? C6 N2 Cd1 114.0(2) . . ? C10 N2 Cd1 126.4(2) . . ? C10 N3 C11 126.0(3) . . ? C10 N3 H3N 116(3) . . ? C11 N3 H3N 117(3) . . ? C21 N4 C17 119.7(3) . . ? C21 N4 Cd1 126.2(2) . . ? C17 N4 Cd1 113.9(2) . . ? C21 N5 C22 125.7(3) . . ? C21 N5 H5N 116(2) . . ? C22 N5 H5N 118(2) . . ? C4 C3 S1' 130.9(3) . . ? C4 C3 S1 107.1(4) . . ? S1' C3 S1 39.38(12) . . ? C4 C3 H3A 110.3 . . ? S1' C3 H3A 115.1 . . ? S1 C3 H3A 110.3 . . ? C4 C3 H3B 110.3 . . ? S1' C3 H3B 72.1 . . ? S1 C3 H3B 110.3 . . ? H3A C3 H3B 108.5 . . ? C4 C3 H3C 104.5 . . ? S1' C3 H3C 104.5 . . ? S1 C3 H3C 83.9 . . ? H3A C3 H3C 31.1 . . ? H3B C3 H3C 135.6 . . ? C4 C3 H3D 104.5 . . ? S1' C3 H3D 104.5 . . ? S1 C3 H3D 143.3 . . ? H3A C3 H3D 74.7 . . ? H3B C3 H3D 39.6 . . ? H3C C3 H3D 105.7 . . ? C3 C4 N1 115.7(3) . . ? C3 C4 H4A 108.4 . . ? N1 C4 H4A 108.4 . . ? C3 C4 H4B 108.4 . . ? N1 C4 H4B 108.4 . . ? H4A C4 H4B 107.4 . . ? N1 C5 C6 112.3(3) . . ? N1 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? N1 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N2 C6 C7 122.4(3) . . ? N2 C6 C5 116.4(3) . . ? C7 C6 C5 121.1(3) . . ? C6 C7 C8 117.6(4) . . ? C6 C7 H7 121.2 . . ? C8 C7 H7 121.2 . . ? C9 C8 C7 120.8(3) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.1(4) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? N3 C10 N2 116.2(3) . . ? N3 C10 C9 123.3(3) . . ? N2 C10 C9 120.5(3) . . ? N3 C11 C12 116.5(3) . . ? N3 C11 H11A 108.2 . . ? C12 C11 H11A 108.2 . . ? N3 C11 H11B 108.2 . . ? C12 C11 H11B 108.2 . . ? H11A C11 H11B 107.3 . . ? C15 C12 C11 111.1(4) . . ? C15 C12 C13 109.4(4) . . ? C11 C12 C13 111.0(3) . . ? C15 C12 C14 110.1(4) . . ? C11 C12 C14 107.2(4) . . ? C13 C12 C14 107.9(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N1 C16 C17 114.2(3) . . ? N1 C16 H16A 108.7 . . ? C17 C16 H16A 108.7 . . ? N1 C16 H16B 108.7 . . ? C17 C16 H16B 108.7 . . ? H16A C16 H16B 107.6 . . ? N4 C17 C18 121.8(3) . . ? N4 C17 C16 117.1(3) . . ? C18 C17 C16 121.0(3) . . ? C17 C18 C19 118.5(3) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C20 C19 C18 120.6(3) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 118.8(3) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? N4 C21 N5 116.6(3) . . ? N4 C21 C20 120.6(3) . . ? N5 C21 C20 122.8(3) . . ? N5 C22 C23 115.4(3) . . ? N5 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? N5 C22 H22B 108.4 . . ? C23 C22 H22B 108.4 . . ? H22A C22 H22B 107.5 . . ? C24 C23 C25 111.2(4) . . ? C24 C23 C26 110.4(3) . . ? C25 C23 C26 109.0(3) . . ? C24 C23 C22 109.1(3) . . ? C25 C23 C22 110.7(3) . . ? C26 C23 C22 106.3(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 C28 156(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 S1 C2 50.7(3) . . . . ? O1 Cd1 S1 C2 139.8(4) 3 . . . ? N4 Cd1 S1 C2 -54.4(3) . . . . ? N2 Cd1 S1 C2 158.4(3) . . . . ? N1 Cd1 S1 C2 -126.8(3) . . . . ? S1' Cd1 S1 C2 -32.5(3) . . . . ? Cd1 Cd1 S1 C2 61.3(3) 3 . . . ? O1 Cd1 S1 C3 149.19(19) . . . . ? O1 Cd1 S1 C3 -121.7(4) 3 . . . ? N4 Cd1 S1 C3 44.05(19) . . . . ? N2 Cd1 S1 C3 -103.10(19) . . . . ? N1 Cd1 S1 C3 -28.34(19) . . . . ? S1' Cd1 S1 C3 66.0(2) . . . . ? Cd1 Cd1 S1 C3 159.77(17) 3 . . . ? C2' C1 C2 S1 -28.3(6) . . . . ? C3 S1 C2 C1 167.6(5) . . . . ? Cd1 S1 C2 C1 -99.4(5) . . . . ? O1 Cd1 S1' C2' -75.9(5) . . . . ? O1 Cd1 S1' C2' -149.7(5) 3 . . . ? N4 Cd1 S1' C2' -178.3(5) . . . . ? N2 Cd1 S1' C2' 35.9(5) . . . . ? N1 Cd1 S1' C2' 105.1(5) . . . . ? S1 Cd1 S1' C2' 25.1(4) . . . . ? Cd1 Cd1 S1' C2' -89.6(4) 3 . . . ? O1 Cd1 S1' C3 -174.7(2) . . . . ? O1 Cd1 S1' C3 111.5(3) 3 . . . ? N4 Cd1 S1' C3 82.9(2) . . . . ? N2 Cd1 S1' C3 -62.9(2) . . . . ? N1 Cd1 S1' C3 6.3(2) . . . . ? S1 Cd1 S1' C3 -73.7(2) . . . . ? Cd1 Cd1 S1' C3 171.6(2) 3 . . . ? C2 C1 C2' S1' 28.1(5) . . . . ? C3 S1' C2' C1 -163.6(5) . . . . ? Cd1 S1' C2' C1 103.0(5) . . . . ? O1 Cd1 O1 Cd1 0.0 3 . . 3 ? N4 Cd1 O1 Cd1 -93.77(10) . . . 3 ? N2 Cd1 O1 Cd1 90.03(11) . . . 3 ? N1 Cd1 O1 Cd1 -149.1(15) . . . 3 ? S1 Cd1 O1 Cd1 169.56(8) . . . 3 ? S1' Cd1 O1 Cd1 -165.15(9) . . . 3 ? O1 Cd1 N1 C5 -157.5(15) . . . . ? O1 Cd1 N1 C5 53.8(2) 3 . . . ? N4 Cd1 N1 C5 146.3(2) . . . . ? N2 Cd1 N1 C5 -35.6(2) . . . . ? S1 Cd1 N1 C5 -115.6(2) . . . . ? S1' Cd1 N1 C5 -141.3(2) . . . . ? Cd1 Cd1 N1 C5 55.8(2) 3 . . . ? O1 Cd1 N1 C4 -38.9(16) . . . . ? O1 Cd1 N1 C4 172.4(2) 3 . . . ? N4 Cd1 N1 C4 -95.0(3) . . . . ? N2 Cd1 N1 C4 83.0(3) . . . . ? S1 Cd1 N1 C4 3.0(2) . . . . ? S1' Cd1 N1 C4 -22.7(2) . . . . ? Cd1 Cd1 N1 C4 174.4(2) 3 . . . ? O1 Cd1 N1 C16 85.8(15) . . . . ? O1 Cd1 N1 C16 -62.9(2) 3 . . . ? N4 Cd1 N1 C16 29.62(18) . . . . ? N2 Cd1 N1 C16 -152.3(2) . . . . ? S1 Cd1 N1 C16 127.64(19) . . . . ? S1' Cd1 N1 C16 101.97(18) . . . . ? Cd1 Cd1 N1 C16 -60.9(2) 3 . . . ? O1 Cd1 N2 C6 -164.0(2) . . . . ? O1 Cd1 N2 C6 -84.7(2) 3 . . . ? N4 Cd1 N2 C6 22.6(3) . . . . ? N1 Cd1 N2 C6 19.3(2) . . . . ? S1 Cd1 N2 C6 98.5(2) . . . . ? S1' Cd1 N2 C6 93.8(2) . . . . ? Cd1 Cd1 N2 C6 -122.2(2) 3 . . . ? O1 Cd1 N2 C10 13.2(3) . . . . ? O1 Cd1 N2 C10 92.5(3) 3 . . . ? N4 Cd1 N2 C10 -160.2(2) . . . . ? N1 Cd1 N2 C10 -163.5(3) . . . . ? S1 Cd1 N2 C10 -84.3(3) . . . . ? S1' Cd1 N2 C10 -89.0(3) . . . . ? Cd1 Cd1 N2 C10 55.0(3) 3 . . . ? O1 Cd1 N4 C21 -14.9(3) . . . . ? O1 Cd1 N4 C21 -94.8(3) 3 . . . ? N2 Cd1 N4 C21 158.6(2) . . . . ? N1 Cd1 N4 C21 162.0(3) . . . . ? S1 Cd1 N4 C21 87.8(3) . . . . ? S1' Cd1 N4 C21 78.0(3) . . . . ? Cd1 Cd1 N4 C21 -56.2(3) 3 . . . ? O1 Cd1 N4 C17 169.8(2) . . . . ? O1 Cd1 N4 C17 89.9(2) 3 . . . ? N2 Cd1 N4 C17 -16.7(3) . . . . ? N1 Cd1 N4 C17 -13.4(2) . . . . ? S1 Cd1 N4 C17 -87.6(2) . . . . ? S1' Cd1 N4 C17 -97.3(2) . . . . ? Cd1 Cd1 N4 C17 128.5(2) 3 . . . ? C2' S1' C3 C4 -99.8(7) . . . . ? Cd1 S1' C3 C4 11.6(6) . . . . ? C2' S1' C3 S1 -35.9(4) . . . . ? Cd1 S1' C3 S1 75.43(10) . . . . ? C2 S1 C3 C4 171.9(4) . . . . ? Cd1 S1 C3 C4 56.8(3) . . . . ? C2 S1 C3 S1' 37.2(3) . . . . ? Cd1 S1 C3 S1' -77.92(11) . . . . ? S1' C3 C4 N1 -33.5(8) . . . . ? S1 C3 C4 N1 -70.1(5) . . . . ? C5 N1 C4 C3 151.4(4) . . . . ? C16 N1 C4 C3 -83.3(4) . . . . ? Cd1 N1 C4 C3 36.2(5) . . . . ? C4 N1 C5 C6 -71.7(3) . . . . ? C16 N1 C5 C6 161.7(3) . . . . ? Cd1 N1 C5 C6 50.3(3) . . . . ? C10 N2 C6 C7 0.8(5) . . . . ? Cd1 N2 C6 C7 178.2(3) . . . . ? C10 N2 C6 C5 -175.4(3) . . . . ? Cd1 N2 C6 C5 2.1(4) . . . . ? N1 C5 C6 N2 -37.7(4) . . . . ? N1 C5 C6 C7 146.1(3) . . . . ? N2 C6 C7 C8 -2.0(5) . . . . ? C5 C6 C7 C8 174.0(3) . . . . ? C6 C7 C8 C9 1.6(5) . . . . ? C7 C8 C9 C10 -0.1(5) . . . . ? C11 N3 C10 N2 -167.5(3) . . . . ? C11 N3 C10 C9 12.4(6) . . . . ? C6 N2 C10 N3 -179.3(3) . . . . ? Cd1 N2 C10 N3 3.6(4) . . . . ? C6 N2 C10 C9 0.7(5) . . . . ? Cd1 N2 C10 C9 -176.3(2) . . . . ? C8 C9 C10 N3 179.0(3) . . . . ? C8 C9 C10 N2 -1.1(5) . . . . ? C10 N3 C11 C12 -102.1(4) . . . . ? N3 C11 C12 C15 -54.1(5) . . . . ? N3 C11 C12 C13 67.9(4) . . . . ? N3 C11 C12 C14 -174.4(4) . . . . ? C5 N1 C16 C17 -155.6(3) . . . . ? C4 N1 C16 C17 80.2(3) . . . . ? Cd1 N1 C16 C17 -44.7(3) . . . . ? C21 N4 C17 C18 1.4(5) . . . . ? Cd1 N4 C17 C18 177.0(3) . . . . ? C21 N4 C17 C16 177.5(3) . . . . ? Cd1 N4 C17 C16 -6.9(4) . . . . ? N1 C16 C17 N4 37.3(4) . . . . ? N1 C16 C17 C18 -146.5(3) . . . . ? N4 C17 C18 C19 0.3(5) . . . . ? C16 C17 C18 C19 -175.7(3) . . . . ? C17 C18 C19 C20 -1.4(6) . . . . ? C18 C19 C20 C21 0.9(6) . . . . ? C17 N4 C21 N5 178.2(3) . . . . ? Cd1 N4 C21 N5 3.2(4) . . . . ? C17 N4 C21 C20 -1.9(5) . . . . ? Cd1 N4 C21 C20 -177.0(2) . . . . ? C22 N5 C21 N4 173.5(3) . . . . ? C22 N5 C21 C20 -6.3(5) . . . . ? C19 C20 C21 N4 0.9(6) . . . . ? C19 C20 C21 N5 -179.3(4) . . . . ? C21 N5 C22 C23 100.5(4) . . . . ? N5 C22 C23 C24 62.2(4) . . . . ? N5 C22 C23 C25 -60.5(4) . . . . ? N5 C22 C23 C26 -178.7(3) . . . . ? 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 H1 O2 0.74(3) 2.20(4) 2.919(4) 163(3) . N3 H3N O1 0.79(4) 2.57(4) 3.330(4) 163(4) . N5 H5N O1 0.82(4) 2.29(4) 3.105(4) 173(3) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.713 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.076