Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Bermejo, M. R.' 'Garcia-Deibe, A.' 'Lodeiro, C.' 'Mahia, Jose' 'Sanmartin, Jesus' 'Vazquez, Miguel' _publ_contact_author_name 'M R Bermejo' _publ_contact_author_address ; Departamento de Quimica Inorganica Universidade de Santiago Facultade de Quimica Santiago de Compostela E-15706 SPAIN ; _publ_contact_author_email 'QISUSO@USC.ES' _publ_section_title ; Metal complexes with a chiral N4 symmetrical Schiff base. Crystal structures of the ligand and its Cu(II) and Ni(II) "mono-helicates" ; data_rrH2cyTs _database_code_CSD 155428 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36.50 N4 O4.25 S2' _chemical_formula_weight 633.29 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 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.4723(2) _cell_length_b 15.3201(3) _cell_length_c 19.1700(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.2860(10) _cell_angle_gamma 90.00 _cell_volume 3363.72(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8140 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 0.201 _exptl_absorpt_correction_type 'Sadabs' _exptl_absorpt_correction_T_min 0.709694 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 'Siemens CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number '50 first frames' _diffrn_standards_interval_count 'end of measurement' _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.11 _diffrn_reflns_number 14383 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11278 _reflns_number_gt 8455 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _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^)+(0.0396P)^2^+0.7157P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(6) _refine_ls_number_reflns 11278 _refine_ls_number_parameters 806 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1213 _refine_ls_wR_factor_gt 0.1052 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 C1A C 0.4434(6) 0.5339(5) -0.1838(3) 0.153(3) Uani 1 1 d . . . H1A1 H 0.3656 0.5108 -0.1890 0.229 Uiso 1 1 calc R . . H1A2 H 0.4955 0.4968 -0.2077 0.229 Uiso 1 1 calc R . . H1A3 H 0.4448 0.5915 -0.2034 0.229 Uiso 1 1 calc R . . C2A C 0.4819(5) 0.5379(3) -0.1070(3) 0.0894(14) Uani 1 1 d . . . C3A C 0.4106(4) 0.5080(3) -0.0573(3) 0.0903(14) Uani 1 1 d . . . H3A H 0.3391 0.4831 -0.0713 0.108 Uiso 1 1 calc R . . C4A C 0.4425(3) 0.5139(3) 0.0130(2) 0.0737(11) Uani 1 1 d . . . H4A1 H 0.3928 0.4936 0.0461 0.088 Uiso 1 1 calc R . . C5A C 0.5488(3) 0.5502(2) 0.0338(2) 0.0614(9) Uani 1 1 d . . . C6A C 0.6215(3) 0.5787(3) -0.0152(2) 0.0771(11) Uani 1 1 d . . . H6A H 0.6941 0.6021 -0.0016 0.093 Uiso 1 1 calc R . . C7A C 0.5869(4) 0.5727(3) -0.0852(3) 0.0917(14) Uani 1 1 d . . . H7A H 0.6365 0.5930 -0.1183 0.110 Uiso 1 1 calc R . . S1A S 0.59340(9) 0.55994(8) 0.12323(6) 0.0789(3) Uani 1 1 d . . . O1A O 0.4969(3) 0.5368(3) 0.16168(17) 0.1152(12) Uani 1 1 d . . . O2A O 0.6507(3) 0.6429(2) 0.13545(19) 0.1109(12) Uani 1 1 d . . . N1A N 0.6982(2) 0.48931(19) 0.13702(16) 0.0653(8) Uani 1 1 d . . . H1A H 0.7619 0.5080 0.1577 0.078 Uiso 1 1 calc R . . C8A C 0.6943(3) 0.4000(2) 0.11814(18) 0.0594(9) Uani 1 1 d . . . C9A C 0.5903(3) 0.3548(3) 0.1102(2) 0.0814(12) Uani 1 1 d . . . H9A H 0.5204 0.3822 0.1191 0.098 Uiso 1 1 calc R . . C10A C 0.5907(4) 0.2697(3) 0.0892(3) 0.1000(16) Uani 1 1 d . . . H10A H 0.5201 0.2402 0.0826 0.120 Uiso 1 1 calc R . . C11A C 0.6928(5) 0.2266(3) 0.0774(3) 0.1034(16) Uani 1 1 d . . . H11A H 0.6918 0.1686 0.0632 0.124 Uiso 1 1 calc R . . C12A C 0.7963(4) 0.2711(3) 0.0872(2) 0.0787(11) Uani 1 1 d . . . H12A H 0.8660 0.2425 0.0797 0.094 Uiso 1 1 calc R . . C13A C 0.7993(3) 0.3583(2) 0.10809(17) 0.0539(8) Uani 1 1 d . . . C14A C 0.9136(3) 0.4002(2) 0.11737(18) 0.0557(9) Uani 1 1 d . . . H14A H 0.9785 0.3680 0.1058 0.067 Uiso 1 1 calc R . . N2A N 0.9305(2) 0.47677(18) 0.13994(14) 0.0525(7) Uani 1 1 d . . . C15A C 1.0518(3) 0.5065(2) 0.14927(17) 0.0531(8) Uani 1 1 d . . . H15A H 1.0998 0.4730 0.1182 0.064 Uiso 1 1 calc R . . C16A C 1.0976(3) 0.4921(3) 0.22479(19) 0.0719(10) Uani 1 1 d . . . H16A H 1.0487 0.5233 0.2560 0.086 Uiso 1 1 calc R . . H16B H 1.0941 0.4305 0.2360 0.086 Uiso 1 1 calc R . . C17A C 1.2233(3) 0.5241(3) 0.2356(2) 0.0829(12) Uani 1 1 d . . . H17A H 1.2490 0.5179 0.2845 0.099 Uiso 1 1 calc R . . H17B H 1.2736 0.4883 0.2083 0.099 Uiso 1 1 calc R . . C18A C 1.2344(3) 0.6184(3) 0.2141(2) 0.0792(12) Uani 1 1 d . . . H18A H 1.3161 0.6351 0.2176 0.095 Uiso 1 1 calc R . . H18B H 1.1933 0.6549 0.2459 0.095 Uiso 1 1 calc R . . C19A C 1.1852(3) 0.6340(3) 0.1400(2) 0.0712(11) Uani 1 1 d . . . H19A H 1.2323 0.6031 0.1076 0.085 Uiso 1 1 calc R . . H19B H 1.1889 0.6958 0.1294 0.085 Uiso 1 1 calc R . . C20A C 1.0591(3) 0.6031(2) 0.13062(17) 0.0561(9) Uani 1 1 d . . . H20A H 1.0104 0.6370 0.1610 0.067 Uiso 1 1 calc R . . N3A N 1.0177(2) 0.61573(19) 0.05739(14) 0.0563(7) Uani 1 1 d . . . C21A C 0.9477(3) 0.6770(2) 0.04235(19) 0.0604(9) Uani 1 1 d . . . H21A H 0.9241 0.7118 0.0787 0.072 Uiso 1 1 calc R . . C22A C 0.9006(3) 0.6975(2) -0.02840(18) 0.0597(9) Uani 1 1 d . . . C23A C 0.8241(3) 0.7678(3) -0.0365(2) 0.0747(11) Uani 1 1 d . . . H23A H 0.8066 0.8008 0.0023 0.090 Uiso 1 1 calc R . . C24A C 0.7733(4) 0.7894(3) -0.1018(3) 0.0862(13) Uani 1 1 d . . . H24A H 0.7219 0.8362 -0.1068 0.103 Uiso 1 1 calc R . . C25A C 0.8004(4) 0.7406(3) -0.1590(3) 0.0899(14) Uani 1 1 d . . . H25A H 0.7669 0.7553 -0.2028 0.108 Uiso 1 1 calc R . . C26A C 0.8758(4) 0.6705(3) -0.1530(2) 0.0789(11) Uani 1 1 d . . . H26A H 0.8929 0.6384 -0.1924 0.095 Uiso 1 1 calc R . . C27A C 0.9264(3) 0.6479(3) -0.0873(2) 0.0642(10) Uani 1 1 d . . . N4A N 1.0074(3) 0.5797(2) -0.07745(15) 0.0679(8) Uani 1 1 d . . . H4A H 1.0538 0.5830 -0.0407 0.081 Uiso 1 1 calc R . . S2A S 1.02395(10) 0.49519(7) -0.12735(6) 0.0769(3) Uani 1 1 d . . . O3A O 1.0486(3) 0.5220(2) -0.19616(15) 0.1074(11) Uani 1 1 d . . . O4A O 1.1076(3) 0.4422(2) -0.08830(18) 0.0964(9) Uani 1 1 d . . . C28A C 0.8894(4) 0.4420(2) -0.13238(18) 0.0637(10) Uani 1 1 d . . . C29A C 0.8316(5) 0.4226(3) -0.1956(2) 0.1067(17) Uani 1 1 d . . . H29A H 0.8632 0.4399 -0.2370 0.128 Uiso 1 1 calc R . . C30A C 0.7279(5) 0.3780(4) -0.1976(3) 0.1147(19) Uani 1 1 d . . . H30A H 0.6911 0.3643 -0.2407 0.138 Uiso 1 1 calc R . . C31A C 0.6772(4) 0.3532(3) -0.1381(3) 0.0793(11) Uani 1 1 d . . . C32A C 0.7341(4) 0.3743(3) -0.0765(2) 0.0858(12) Uani 1 1 d . . . H32A H 0.7009 0.3589 -0.0351 0.103 Uiso 1 1 calc R . . C33A C 0.8383(4) 0.4174(3) -0.0730(2) 0.0825(12) Uani 1 1 d . . . H33A H 0.8748 0.4301 -0.0296 0.099 Uiso 1 1 calc R . . C34A C 0.5632(4) 0.3032(3) -0.1410(3) 0.1119(18) Uani 1 1 d . . . H34A H 0.5311 0.3014 -0.1883 0.168 Uiso 1 1 calc R . . H34B H 0.5092 0.3317 -0.1120 0.168 Uiso 1 1 calc R . . H34C H 0.5771 0.2448 -0.1244 0.168 Uiso 1 1 calc R . . C1B C 0.5751(6) 0.2253(4) 0.6500(2) 0.138(2) Uani 1 1 d . . . H1B1 H 0.6581 0.2170 0.6517 0.208 Uiso 1 1 calc R . . H1B2 H 0.5387 0.1751 0.6694 0.208 Uiso 1 1 calc R . . H1B3 H 0.5571 0.2762 0.6767 0.208 Uiso 1 1 calc R . . C2B C 0.5300(5) 0.2374(3) 0.5753(2) 0.0852(13) Uani 1 1 d . . . C3B C 0.5946(4) 0.2151(3) 0.5216(3) 0.0856(13) Uani 1 1 d . . . H3B H 0.6696 0.1937 0.5314 0.103 Uiso 1 1 calc R . . C4B C 0.5540(3) 0.2226(3) 0.4528(2) 0.0731(11) Uani 1 1 d . . . H4B1 H 0.5998 0.2048 0.4170 0.088 Uiso 1 1 calc R . . C5B C 0.4450(3) 0.2565(2) 0.4382(2) 0.0621(9) Uani 1 1 d . . . C6B C 0.3779(3) 0.2811(3) 0.4917(3) 0.0820(12) Uani 1 1 d . . . H6B H 0.3036 0.3040 0.4819 0.098 Uiso 1 1 calc R . . C7B C 0.4204(5) 0.2719(3) 0.5598(3) 0.0965(14) Uani 1 1 d . . . H7B H 0.3748 0.2892 0.5959 0.116 Uiso 1 1 calc R . . N1B N 0.2812(2) 0.1950(2) 0.34363(16) 0.0659(8) Uani 1 1 d . . . H1B H 0.2145 0.2154 0.3288 0.079 Uiso 1 1 calc R . . S1B S 0.38791(8) 0.26454(8) 0.35064(6) 0.0805(3) Uani 1 1 d . . . O1B O 0.4777(2) 0.2378(3) 0.30725(16) 0.1161(13) Uani 1 1 d . . . O2B O 0.3320(3) 0.3467(2) 0.3405(2) 0.1132(12) Uani 1 1 d . . . C8B C 0.2848(3) 0.1055(2) 0.35892(17) 0.0560(9) Uani 1 1 d . . . C9B C 0.3880(3) 0.0573(3) 0.3633(2) 0.0751(11) Uani 1 1 d . . . H9B H 0.4582 0.0838 0.3537 0.090 Uiso 1 1 calc R . . C10B C 0.3863(4) -0.0291(3) 0.3819(3) 0.0891(14) Uani 1 1 d . . . H10B H 0.4563 -0.0598 0.3864 0.107 Uiso 1 1 calc R . . C11B C 0.2845(4) -0.0711(3) 0.3939(3) 0.0960(15) Uani 1 1 d . . . H11B H 0.2844 -0.1298 0.4062 0.115 Uiso 1 1 calc R . . C12B C 0.1819(4) -0.0244(3) 0.3874(2) 0.0796(12) Uani 1 1 d . . . H12B H 0.1118 -0.0528 0.3943 0.096 Uiso 1 1 calc R . . C13B C 0.1797(3) 0.0642(2) 0.37078(17) 0.0554(8) Uani 1 1 d . . . C14B C 0.0670(3) 0.1092(2) 0.36827(18) 0.0550(8) Uani 1 1 d . . . H14B H 0.0014 0.0767 0.3782 0.066 Uiso 1 1 calc R . . N2B N 0.0526(2) 0.18877(19) 0.35364(14) 0.0512(7) Uani 1 1 d . . . C15B C -0.0661(3) 0.2249(2) 0.35239(17) 0.0511(8) Uani 1 1 d . . . H15B H -0.1114 0.1930 0.3859 0.061 Uiso 1 1 calc R . . C16B C -0.1243(3) 0.2143(3) 0.27937(18) 0.0620(9) Uani 1 1 d . . . H16C H -0.1284 0.1528 0.2674 0.074 Uiso 1 1 calc R . . H16D H -0.0777 0.2433 0.2457 0.074 Uiso 1 1 calc R . . C17B C -0.2471(3) 0.2528(3) 0.2757(2) 0.0722(11) Uani 1 1 d . . . H17C H -0.2807 0.2484 0.2282 0.087 Uiso 1 1 calc R . . H17D H -0.2959 0.2198 0.3058 0.087 Uiso 1 1 calc R . . C18B C -0.2446(3) 0.3471(3) 0.2979(2) 0.0819(12) Uani 1 1 d . . . H18C H -0.3240 0.3687 0.2986 0.098 Uiso 1 1 calc R . . H18D H -0.2044 0.3812 0.2641 0.098 Uiso 1 1 calc R . . C19B C -0.1838(3) 0.3588(3) 0.3696(2) 0.0717(11) Uani 1 1 d . . . H19C H -0.2293 0.3307 0.4043 0.086 Uiso 1 1 calc R . . H19D H -0.1790 0.4205 0.3807 0.086 Uiso 1 1 calc R . . C20B C -0.0611(3) 0.3199(2) 0.37258(18) 0.0561(9) Uani 1 1 d . . . H20B H -0.0131 0.3516 0.3403 0.067 Uiso 1 1 calc R . . N3B N -0.0100(2) 0.32932(19) 0.44414(15) 0.0582(7) Uani 1 1 d . . . C21B C 0.0626(3) 0.3901(2) 0.4572(2) 0.0631(9) Uani 1 1 d . . . H21B H 0.0828 0.4252 0.4203 0.076 Uiso 1 1 calc R . . C22B C 0.1170(3) 0.4090(3) 0.5265(2) 0.0669(10) Uani 1 1 d . . . C23B C 0.1930(4) 0.4794(3) 0.5331(3) 0.0863(13) Uani 1 1 d . . . H23B H 0.2068 0.5130 0.4940 0.104 Uiso 1 1 calc R . . C24B C 0.2480(4) 0.5002(4) 0.5963(3) 0.1078(17) Uani 1 1 d . . . H24B H 0.3000 0.5468 0.5997 0.129 Uiso 1 1 calc R . . C25B C 0.2261(5) 0.4525(4) 0.6543(3) 0.1099(18) Uani 1 1 d . . . H25B H 0.2632 0.4670 0.6971 0.132 Uiso 1 1 calc R . . C26B C 0.1493(4) 0.3827(3) 0.6501(2) 0.0913(14) Uani 1 1 d . . . H26B H 0.1348 0.3507 0.6899 0.110 Uiso 1 1 calc R . . C27B C 0.0940(3) 0.3607(3) 0.5861(2) 0.0676(10) Uani 1 1 d . . . N4B N 0.0129(3) 0.2918(2) 0.57824(17) 0.0720(9) Uani 1 1 d . . . H4B H -0.0367 0.2953 0.5430 0.086 Uiso 1 1 calc R . . S2B S 0.00224(10) 0.20591(8) 0.62824(6) 0.0834(3) Uani 1 1 d . . . O3B O -0.0074(3) 0.2332(3) 0.69911(16) 0.1151(12) Uani 1 1 d . . . O4B O -0.0897(2) 0.1560(2) 0.59408(17) 0.1042(10) Uani 1 1 d . . . C28B C 0.1338(3) 0.1499(3) 0.6232(2) 0.0695(10) Uani 1 1 d . . . C29B C 0.2071(4) 0.1327(3) 0.6814(2) 0.0858(13) Uani 1 1 d . . . H29B H 0.1876 0.1529 0.7250 0.103 Uiso 1 1 calc R . . C30B C 0.3084(4) 0.0862(3) 0.6754(3) 0.0879(14) Uani 1 1 d . . . H30B H 0.3554 0.0743 0.7154 0.106 Uiso 1 1 calc R . . C31B C 0.3421(4) 0.0570(3) 0.6122(3) 0.0806(12) Uani 1 1 d . . . C32B C 0.2705(4) 0.0742(3) 0.5544(2) 0.0839(12) Uani 1 1 d . . . H32B H 0.2913 0.0543 0.5110 0.101 Uiso 1 1 calc R . . C33B C 0.1675(4) 0.1206(3) 0.5591(2) 0.0821(12) Uani 1 1 d . . . H33B H 0.1208 0.1321 0.5189 0.099 Uiso 1 1 calc R . . C34B C 0.4523(4) 0.0045(3) 0.6067(3) 0.1086(16) Uani 1 1 d . . . H341 H 0.5013 0.0323 0.5744 0.163 Uiso 1 1 calc R . . H342 H 0.4327 -0.0532 0.5905 0.163 Uiso 1 1 calc R . . H343 H 0.4930 0.0010 0.6518 0.163 Uiso 1 1 calc R . . O1W O 0.7448(17) 0.8146(10) 0.1879(11) 0.331(11) Uani 0.50 1 d P . . H1W H 0.6850 0.7827 0.1780 0.100 Uiso 0.50 1 d P . . H2W H 0.7817 0.8525 0.1597 0.100 Uiso 0.50 1 d P . . 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 C1A 0.221(7) 0.142(6) 0.089(4) -0.012(4) -0.044(4) 0.057(5) C2A 0.112(4) 0.062(3) 0.091(3) -0.001(2) -0.017(3) 0.025(3) C3A 0.076(3) 0.066(3) 0.124(4) -0.002(3) -0.032(3) 0.003(2) C4A 0.058(2) 0.061(3) 0.101(3) 0.012(2) -0.006(2) 0.0073(18) C5A 0.0472(19) 0.057(2) 0.079(2) 0.0050(19) -0.0024(18) 0.0104(17) C6A 0.062(2) 0.066(3) 0.104(3) 0.002(2) 0.001(2) 0.001(2) C7A 0.103(4) 0.082(3) 0.092(3) 0.024(3) 0.020(3) 0.015(3) S1A 0.0661(6) 0.0861(8) 0.0836(7) -0.0100(6) -0.0047(5) 0.0278(6) O1A 0.0759(19) 0.174(4) 0.098(2) -0.002(2) 0.0175(17) 0.041(2) O2A 0.117(2) 0.067(2) 0.142(3) -0.0410(19) -0.044(2) 0.0298(18) N1A 0.0530(16) 0.062(2) 0.080(2) -0.0049(16) -0.0104(15) 0.0118(15) C8A 0.053(2) 0.064(3) 0.061(2) 0.0100(18) -0.0022(16) -0.0061(18) C9A 0.051(2) 0.078(3) 0.113(3) 0.026(3) -0.009(2) -0.009(2) C10A 0.079(3) 0.078(3) 0.140(4) 0.031(3) -0.025(3) -0.036(3) C11A 0.109(4) 0.058(3) 0.140(4) 0.003(3) -0.015(3) -0.024(3) C12A 0.079(3) 0.053(2) 0.104(3) -0.009(2) -0.004(2) -0.002(2) C13A 0.053(2) 0.046(2) 0.062(2) 0.0086(16) -0.0006(16) -0.0044(16) C14A 0.054(2) 0.053(2) 0.060(2) 0.0018(18) 0.0021(16) 0.0058(16) N2A 0.0497(15) 0.0524(18) 0.0552(16) 0.0024(13) 0.0019(12) -0.0024(13) C15A 0.0445(18) 0.056(2) 0.059(2) 0.0013(17) 0.0003(15) -0.0039(15) C16A 0.064(2) 0.085(3) 0.066(2) 0.017(2) -0.0047(18) -0.009(2) C17A 0.060(2) 0.106(4) 0.081(3) 0.009(2) -0.014(2) -0.009(2) C18A 0.062(2) 0.100(3) 0.074(3) -0.013(2) -0.009(2) -0.014(2) C19A 0.066(2) 0.073(3) 0.074(3) -0.006(2) -0.002(2) -0.022(2) C20A 0.057(2) 0.059(2) 0.053(2) -0.0021(16) 0.0068(16) -0.0069(16) N3A 0.0590(17) 0.0525(17) 0.0568(17) 0.0030(14) -0.0007(14) -0.0111(14) C21A 0.062(2) 0.055(2) 0.064(2) -0.0014(18) 0.0042(18) -0.0075(18) C22A 0.059(2) 0.057(2) 0.063(2) 0.0070(18) -0.0027(17) -0.0103(17) C23A 0.077(2) 0.064(3) 0.083(3) 0.008(2) -0.004(2) -0.006(2) C24A 0.078(3) 0.069(3) 0.109(4) 0.022(3) -0.014(3) -0.001(2) C25A 0.094(3) 0.090(4) 0.083(3) 0.015(3) -0.021(3) -0.018(3) C26A 0.086(3) 0.078(3) 0.071(3) 0.007(2) -0.005(2) -0.019(2) C27A 0.065(2) 0.061(2) 0.065(2) 0.009(2) -0.0050(19) -0.0209(19) N4A 0.079(2) 0.060(2) 0.0625(19) -0.0008(15) -0.0068(16) -0.0115(17) S2A 0.0915(7) 0.0709(7) 0.0697(6) -0.0022(6) 0.0183(6) -0.0100(6) O3A 0.149(3) 0.102(2) 0.0760(19) -0.0016(17) 0.0451(19) -0.029(2) O4A 0.086(2) 0.085(2) 0.119(2) -0.0010(19) 0.0072(18) 0.0105(17) C28A 0.095(3) 0.049(2) 0.047(2) -0.0026(16) 0.009(2) -0.0023(19) C29A 0.163(5) 0.099(4) 0.058(3) -0.006(2) 0.003(3) -0.039(4) C30A 0.153(5) 0.104(4) 0.084(4) -0.012(3) -0.022(3) -0.046(4) C31A 0.088(3) 0.054(2) 0.095(3) -0.008(2) -0.002(3) -0.002(2) C32A 0.099(3) 0.088(3) 0.071(3) -0.006(2) 0.016(2) -0.018(3) C33A 0.095(3) 0.094(3) 0.058(2) 0.000(2) 0.005(2) -0.022(3) C34A 0.092(3) 0.084(3) 0.158(5) -0.026(3) -0.004(3) -0.015(3) C1B 0.198(6) 0.134(5) 0.078(3) 0.021(3) -0.038(4) -0.082(5) C2B 0.109(4) 0.071(3) 0.073(3) 0.010(2) -0.014(3) -0.039(3) C3B 0.074(3) 0.075(3) 0.104(4) 0.009(3) -0.024(3) -0.009(2) C4B 0.051(2) 0.082(3) 0.085(3) 0.003(2) -0.0078(19) -0.0009(19) C5B 0.0487(19) 0.060(2) 0.077(2) 0.0087(19) -0.0023(18) -0.0101(17) C6B 0.060(2) 0.078(3) 0.108(4) -0.001(3) 0.004(2) 0.000(2) C7B 0.107(4) 0.096(4) 0.088(3) -0.020(3) 0.016(3) -0.025(3) N1B 0.0413(15) 0.076(2) 0.079(2) 0.0158(17) -0.0064(14) -0.0035(14) S1B 0.0548(6) 0.0956(8) 0.0894(7) 0.0351(7) -0.0112(5) -0.0201(6) O1B 0.0567(16) 0.206(4) 0.086(2) 0.031(2) 0.0070(15) -0.031(2) O2B 0.090(2) 0.081(2) 0.163(3) 0.059(2) -0.043(2) -0.0260(17) C8B 0.056(2) 0.059(2) 0.052(2) -0.0004(17) -0.0062(16) 0.0076(17) C9B 0.054(2) 0.086(3) 0.085(3) -0.015(2) -0.0060(19) 0.014(2) C10B 0.077(3) 0.080(3) 0.109(4) -0.017(3) -0.007(2) 0.038(3) C11B 0.097(3) 0.061(3) 0.128(4) -0.003(3) -0.008(3) 0.024(3) C12B 0.075(3) 0.056(3) 0.107(3) -0.003(2) 0.000(2) 0.003(2) C13B 0.054(2) 0.055(2) 0.057(2) -0.0076(17) -0.0010(16) 0.0065(17) C14B 0.0486(18) 0.053(2) 0.064(2) -0.0026(18) 0.0041(16) -0.0016(16) N2B 0.0451(14) 0.0543(19) 0.0541(16) -0.0008(13) 0.0031(12) 0.0017(13) C15B 0.0426(17) 0.054(2) 0.0572(19) 0.0005(16) 0.0038(15) 0.0033(15) C16B 0.0524(19) 0.069(2) 0.064(2) -0.0093(19) 0.0051(16) 0.0065(17) C17B 0.0456(18) 0.098(3) 0.073(2) -0.005(2) -0.0008(17) 0.008(2) C18B 0.072(3) 0.092(3) 0.080(3) -0.004(2) -0.010(2) 0.031(2) C19B 0.073(2) 0.069(3) 0.073(3) -0.006(2) 0.000(2) 0.024(2) C20B 0.055(2) 0.057(2) 0.057(2) 0.0024(16) 0.0031(17) 0.0049(16) N3B 0.0568(17) 0.0534(18) 0.0645(18) -0.0034(14) 0.0039(14) 0.0046(15) C21B 0.063(2) 0.055(2) 0.072(2) 0.0004(19) 0.0083(19) 0.0038(18) C22B 0.060(2) 0.061(2) 0.079(3) -0.013(2) 0.001(2) 0.0033(18) C23B 0.083(3) 0.064(3) 0.110(4) -0.011(2) -0.007(3) -0.005(2) C24B 0.094(3) 0.081(4) 0.145(5) -0.025(4) -0.018(4) -0.015(3) C25B 0.108(4) 0.101(4) 0.115(4) -0.032(4) -0.044(3) -0.001(3) C26B 0.097(3) 0.095(4) 0.079(3) -0.016(3) -0.017(3) 0.005(3) C27B 0.061(2) 0.064(2) 0.077(3) -0.014(2) -0.004(2) 0.0083(19) N4B 0.0690(19) 0.074(2) 0.072(2) 0.0036(17) -0.0077(16) -0.0005(16) S2B 0.0827(7) 0.0957(9) 0.0729(7) 0.0123(6) 0.0149(6) -0.0063(6) O3B 0.124(3) 0.152(3) 0.073(2) 0.002(2) 0.0369(18) 0.008(2) O4B 0.0840(19) 0.113(3) 0.115(3) 0.017(2) 0.0006(18) -0.0377(19) C28B 0.084(3) 0.066(2) 0.058(2) 0.0144(19) 0.004(2) -0.011(2) C29B 0.106(3) 0.089(3) 0.062(3) 0.014(2) 0.002(2) -0.013(3) C30B 0.098(3) 0.080(3) 0.083(3) 0.032(3) -0.019(3) -0.007(3) C31B 0.096(3) 0.052(2) 0.094(3) 0.017(2) 0.005(3) -0.009(2) C32B 0.105(3) 0.073(3) 0.074(3) 0.007(2) 0.007(2) 0.013(3) C33B 0.101(3) 0.085(3) 0.060(3) 0.012(2) -0.001(2) 0.005(3) C34B 0.101(3) 0.074(3) 0.151(5) 0.018(3) 0.007(3) 0.009(3) O1W 0.39(2) 0.191(13) 0.40(3) 0.003(14) -0.149(19) -0.070(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 C1A C2A 1.514(6) . ? C1A H1A1 0.9600 . ? C1A H1A2 0.9600 . ? C1A H1A3 0.9600 . ? C2A C7A 1.360(6) . ? C2A C3A 1.370(7) . ? C3A C4A 1.380(6) . ? C3A H3A 0.9300 . ? C4A C5A 1.378(5) . ? C4A H4A1 0.9300 . ? C5A C6A 1.364(5) . ? C5A S1A 1.767(4) . ? C6A C7A 1.381(6) . ? C6A H6A 0.9300 . ? C7A H7A 0.9300 . ? S1A O1A 1.410(3) . ? S1A O2A 1.444(3) . ? S1A N1A 1.628(3) . ? N1A C8A 1.415(5) . ? N1A H1A 0.8600 . ? C8A C9A 1.380(5) . ? C8A C13A 1.387(5) . ? C9A C10A 1.364(7) . ? C9A H9A 0.9300 . ? C10A C11A 1.374(6) . ? C10A H10A 0.9300 . ? C11A C12A 1.373(6) . ? C11A H11A 0.9300 . ? C12A C13A 1.394(5) . ? C12A H12A 0.9300 . ? C13A C14A 1.461(5) . ? C14A N2A 1.262(4) . ? C14A H14A 0.9300 . ? N2A C15A 1.465(4) . ? C15A C20A 1.525(5) . ? C15A C16A 1.528(5) . ? C15A H15A 0.9800 . ? C16A C17A 1.526(5) . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C17A C18A 1.510(6) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C18A C19A 1.517(5) . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C19A C20A 1.524(4) . ? C19A H19A 0.9700 . ? C19A H19B 0.9700 . ? C20A N3A 1.469(4) . ? C20A H20A 0.9800 . ? N3A C21A 1.259(4) . ? C21A C22A 1.464(5) . ? C21A H21A 0.9300 . ? C22A C23A 1.394(5) . ? C22A C27A 1.406(5) . ? C23A C24A 1.391(6) . ? C23A H23A 0.9300 . ? C24A C25A 1.377(6) . ? C24A H24A 0.9300 . ? C25A C26A 1.381(6) . ? C25A H25A 0.9300 . ? C26A C27A 1.399(5) . ? C26A H26A 0.9300 . ? C27A N4A 1.404(5) . ? N4A S2A 1.628(3) . ? N4A H4A 0.8600 . ? S2A O3A 1.425(3) . ? S2A O4A 1.435(3) . ? S2A C28A 1.743(4) . ? C28A C33A 1.364(5) . ? C28A C29A 1.380(6) . ? C29A C30A 1.371(7) . ? C29A H29A 0.9300 . ? C30A C31A 1.364(6) . ? C30A H30A 0.9300 . ? C31A C32A 1.356(6) . ? C31A C34A 1.513(6) . ? C32A C33A 1.364(5) . ? C32A H32A 0.9300 . ? C33A H33A 0.9300 . ? C34A H34A 0.9600 . ? C34A H34B 0.9600 . ? C34A H34C 0.9600 . ? C1B C2B 1.507(6) . ? C1B H1B1 0.9600 . ? C1B H1B2 0.9600 . ? C1B H1B3 0.9600 . ? C2B C3B 1.346(6) . ? C2B C7B 1.380(6) . ? C3B C4B 1.378(6) . ? C3B H3B 0.9300 . ? C4B C5B 1.369(5) . ? C4B H4B1 0.9300 . ? C5B C6B 1.370(5) . ? C5B S1B 1.771(4) . ? C6B C7B 1.374(6) . ? C6B H6B 0.9300 . ? C7B H7B 0.9300 . ? N1B C8B 1.403(4) . ? N1B S1B 1.623(3) . ? N1B H1B 0.8600 . ? S1B O2B 1.420(3) . ? S1B O1B 1.421(3) . ? C8B C13B 1.392(5) . ? C8B C9B 1.393(5) . ? C9B C10B 1.370(6) . ? C9B H9B 0.9300 . ? C10B C11B 1.365(6) . ? C10B H10B 0.9300 . ? C11B C12B 1.377(6) . ? C11B H11B 0.9300 . ? C12B C13B 1.395(5) . ? C12B H12B 0.9300 . ? C13B C14B 1.463(5) . ? C14B N2B 1.260(4) . ? C14B H14B 0.9300 . ? N2B C15B 1.469(4) . ? C15B C20B 1.506(5) . ? C15B C16B 1.525(4) . ? C15B H15B 0.9800 . ? C16B C17B 1.526(5) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17B C18B 1.505(6) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18B C19B 1.516(5) . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C19B C20B 1.527(5) . ? C19B H19C 0.9700 . ? C19B H19D 0.9700 . ? C20B N3B 1.468(4) . ? C20B H20B 0.9800 . ? N3B C21B 1.264(4) . ? C21B C22B 1.463(5) . ? C21B H21B 0.9300 . ? C22B C23B 1.388(5) . ? C22B C27B 1.399(6) . ? C23B C24B 1.372(7) . ? C23B H23B 0.9300 . ? C24B C25B 1.366(7) . ? C24B H24B 0.9300 . ? C25B C26B 1.385(7) . ? C25B H25B 0.9300 . ? C26B C27B 1.390(5) . ? C26B H26B 0.9300 . ? C27B N4B 1.409(5) . ? N4B S2B 1.637(3) . ? N4B H4B 0.8600 . ? S2B O4B 1.431(3) . ? S2B O3B 1.432(3) . ? S2B C28B 1.744(4) . ? C28B C29B 1.383(5) . ? C28B C33B 1.384(5) . ? C29B C30B 1.374(6) . ? C29B H29B 0.9300 . ? C30B C31B 1.367(6) . ? C30B H30B 0.9300 . ? C31B C32B 1.366(6) . ? C31B C34B 1.508(6) . ? C32B C33B 1.386(6) . ? C32B H32B 0.9300 . ? C33B H33B 0.9300 . ? C34B H341 0.9600 . ? C34B H342 0.9600 . ? C34B H343 0.9600 . ? O1W H1W 0.8544 . ? O1W H2W 0.9140 . ? 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 C2A C1A H1A1 109.5 . . ? C2A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? C2A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C7A C2A C3A 118.2(4) . . ? C7A C2A C1A 121.2(6) . . ? C3A C2A C1A 120.7(5) . . ? C2A C3A C4A 121.4(4) . . ? C2A C3A H3A 119.3 . . ? C4A C3A H3A 119.3 . . ? C5A C4A C3A 119.3(4) . . ? C5A C4A H4A1 120.3 . . ? C3A C4A H4A1 120.3 . . ? C6A C5A C4A 119.8(4) . . ? C6A C5A S1A 119.1(3) . . ? C4A C5A S1A 121.1(3) . . ? C5A C6A C7A 119.6(4) . . ? C5A C6A H6A 120.2 . . ? C7A C6A H6A 120.2 . . ? C2A C7A C6A 121.6(5) . . ? C2A C7A H7A 119.2 . . ? C6A C7A H7A 119.2 . . ? O1A S1A O2A 120.0(2) . . ? O1A S1A N1A 110.1(2) . . ? O2A S1A N1A 103.50(17) . . ? O1A S1A C5A 107.06(18) . . ? O2A S1A C5A 109.6(2) . . ? N1A S1A C5A 105.78(16) . . ? C8A N1A S1A 126.1(2) . . ? C8A N1A H1A 117.0 . . ? S1A N1A H1A 117.0 . . ? C9A C8A C13A 120.4(4) . . ? C9A C8A N1A 121.9(4) . . ? C13A C8A N1A 117.8(3) . . ? C10A C9A C8A 119.6(4) . . ? C10A C9A H9A 120.2 . . ? C8A C9A H9A 120.2 . . ? C9A C10A C11A 121.6(4) . . ? C9A C10A H10A 119.2 . . ? C11A C10A H10A 119.2 . . ? C12A C11A C10A 118.5(4) . . ? C12A C11A H11A 120.7 . . ? C10A C11A H11A 120.7 . . ? C11A C12A C13A 121.4(4) . . ? C11A C12A H12A 119.3 . . ? C13A C12A H12A 119.3 . . ? C8A C13A C12A 118.3(3) . . ? C8A C13A C14A 124.1(3) . . ? C12A C13A C14A 117.5(3) . . ? N2A C14A C13A 124.7(3) . . ? N2A C14A H14A 117.6 . . ? C13A C14A H14A 117.6 . . ? C14A N2A C15A 117.2(3) . . ? N2A C15A C20A 109.7(3) . . ? N2A C15A C16A 110.1(3) . . ? C20A C15A C16A 110.0(3) . . ? N2A C15A H15A 109.0 . . ? C20A C15A H15A 109.0 . . ? C16A C15A H15A 109.0 . . ? C17A C16A C15A 110.7(3) . . ? C17A C16A H16A 109.5 . . ? C15A C16A H16A 109.5 . . ? C17A C16A H16B 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 108.1 . . ? C18A C17A C16A 111.3(3) . . ? C18A C17A H17A 109.4 . . ? C16A C17A H17A 109.4 . . ? C18A C17A H17B 109.4 . . ? C16A C17A H17B 109.4 . . ? H17A C17A H17B 108.0 . . ? C17A C18A C19A 112.0(3) . . ? C17A C18A H18A 109.2 . . ? C19A C18A H18A 109.2 . . ? C17A C18A H18B 109.2 . . ? C19A C18A H18B 109.2 . . ? H18A C18A H18B 107.9 . . ? C18A C19A C20A 111.2(3) . . ? C18A C19A H19A 109.4 . . ? C20A C19A H19A 109.4 . . ? C18A C19A H19B 109.4 . . ? C20A C19A H19B 109.4 . . ? H19A C19A H19B 108.0 . . ? N3A C20A C19A 109.0(3) . . ? N3A C20A C15A 109.5(3) . . ? C19A C20A C15A 109.8(3) . . ? N3A C20A H20A 109.5 . . ? C19A C20A H20A 109.5 . . ? C15A C20A H20A 109.5 . . ? C21A N3A C20A 119.0(3) . . ? N3A C21A C22A 124.6(4) . . ? N3A C21A H21A 117.7 . . ? C22A C21A H21A 117.7 . . ? C23A C22A C27A 119.2(3) . . ? C23A C22A C21A 117.7(4) . . ? C27A C22A C21A 123.1(3) . . ? C24A C23A C22A 120.8(4) . . ? C24A C23A H23A 119.6 . . ? C22A C23A H23A 119.6 . . ? C25A C24A C23A 119.1(4) . . ? C25A C24A H24A 120.4 . . ? C23A C24A H24A 120.4 . . ? C24A C25A C26A 121.7(4) . . ? C24A C25A H25A 119.2 . . ? C26A C25A H25A 119.2 . . ? C25A C26A C27A 119.5(4) . . ? C25A C26A H26A 120.2 . . ? C27A C26A H26A 120.2 . . ? C26A C27A N4A 122.8(4) . . ? C26A C27A C22A 119.6(4) . . ? N4A C27A C22A 117.4(3) . . ? C27A N4A S2A 127.7(3) . . ? C27A N4A H4A 116.2 . . ? S2A N4A H4A 116.2 . . ? O3A S2A O4A 118.9(2) . . ? O3A S2A N4A 110.51(18) . . ? O4A S2A N4A 103.95(18) . . ? O3A S2A C28A 107.8(2) . . ? O4A S2A C28A 109.15(19) . . ? N4A S2A C28A 105.77(17) . . ? C33A C28A C29A 117.7(4) . . ? C33A C28A S2A 120.3(3) . . ? C29A C28A S2A 121.9(3) . . ? C30A C29A C28A 120.3(4) . . ? C30A C29A H29A 119.8 . . ? C28A C29A H29A 119.8 . . ? C31A C30A C29A 121.8(4) . . ? C31A C30A H30A 119.1 . . ? C29A C30A H30A 119.1 . . ? C32A C31A C30A 117.1(4) . . ? C32A C31A C34A 121.6(5) . . ? C30A C31A C34A 121.3(5) . . ? C31A C32A C33A 122.3(4) . . ? C31A C32A H32A 118.8 . . ? C33A C32A H32A 118.8 . . ? C28A C33A C32A 120.7(4) . . ? C28A C33A H33A 119.6 . . ? C32A C33A H33A 119.6 . . ? C31A C34A H34A 109.5 . . ? C31A C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C31A C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C2B C1B H1B1 109.5 . . ? C2B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? C2B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C3B C2B C7B 117.9(4) . . ? C3B C2B C1B 121.5(5) . . ? C7B C2B C1B 120.7(5) . . ? C2B C3B C4B 122.7(4) . . ? C2B C3B H3B 118.7 . . ? C4B C3B H3B 118.7 . . ? C5B C4B C3B 118.9(4) . . ? C5B C4B H4B1 120.6 . . ? C3B C4B H4B1 120.6 . . ? C4B C5B C6B 119.8(4) . . ? C4B C5B S1B 120.3(3) . . ? C6B C5B S1B 119.8(3) . . ? C5B C6B C7B 119.9(4) . . ? C5B C6B H6B 120.0 . . ? C7B C6B H6B 120.0 . . ? C6B C7B C2B 120.9(4) . . ? C6B C7B H7B 119.6 . . ? C2B C7B H7B 119.6 . . ? C8B N1B S1B 127.7(2) . . ? C8B N1B H1B 116.2 . . ? S1B N1B H1B 116.2 . . ? O2B S1B O1B 120.8(2) . . ? O2B S1B N1B 103.76(16) . . ? O1B S1B N1B 109.4(2) . . ? O2B S1B C5B 109.3(2) . . ? O1B S1B C5B 107.10(17) . . ? N1B S1B C5B 105.62(16) . . ? C13B C8B C9B 119.4(4) . . ? C13B C8B N1B 117.5(3) . . ? C9B C8B N1B 123.1(3) . . ? C10B C9B C8B 120.2(4) . . ? C10B C9B H9B 119.9 . . ? C8B C9B H9B 119.9 . . ? C11B C10B C9B 121.6(4) . . ? C11B C10B H10B 119.2 . . ? C9B C10B H10B 119.2 . . ? C10B C11B C12B 118.4(4) . . ? C10B C11B H11B 120.8 . . ? C12B C11B H11B 120.8 . . ? C11B C12B C13B 122.0(4) . . ? C11B C12B H12B 119.0 . . ? C13B C12B H12B 119.0 . . ? C8B C13B C12B 118.4(3) . . ? C8B C13B C14B 123.6(3) . . ? C12B C13B C14B 118.0(3) . . ? N2B C14B C13B 124.5(3) . . ? N2B C14B H14B 117.7 . . ? C13B C14B H14B 117.7 . . ? C14B N2B C15B 118.5(3) . . ? N2B C15B C20B 109.8(3) . . ? N2B C15B C16B 109.4(3) . . ? C20B C15B C16B 110.3(3) . . ? N2B C15B H15B 109.1 . . ? C20B C15B H15B 109.1 . . ? C16B C15B H15B 109.1 . . ? C15B C16B C17B 110.9(3) . . ? C15B C16B H16C 109.5 . . ? C17B C16B H16C 109.5 . . ? C15B C16B H16D 109.5 . . ? C17B C16B H16D 109.5 . . ? H16C C16B H16D 108.1 . . ? C18B C17B C16B 110.9(3) . . ? C18B C17B H17C 109.5 . . ? C16B C17B H17C 109.5 . . ? C18B C17B H17D 109.5 . . ? C16B C17B H17D 109.5 . . ? H17C C17B H17D 108.1 . . ? C17B C18B C19B 111.8(3) . . ? C17B C18B H18C 109.3 . . ? C19B C18B H18C 109.3 . . ? C17B C18B H18D 109.3 . . ? C19B C18B H18D 109.3 . . ? H18C C18B H18D 107.9 . . ? C18B C19B C20B 111.2(3) . . ? C18B C19B H19C 109.4 . . ? C20B C19B H19C 109.4 . . ? C18B C19B H19D 109.4 . . ? C20B C19B H19D 109.4 . . ? H19C C19B H19D 108.0 . . ? N3B C20B C15B 110.0(3) . . ? N3B C20B C19B 108.3(3) . . ? C15B C20B C19B 110.3(3) . . ? N3B C20B H20B 109.4 . . ? C15B C20B H20B 109.4 . . ? C19B C20B H20B 109.4 . . ? C21B N3B C20B 118.8(3) . . ? N3B C21B C22B 124.6(4) . . ? N3B C21B H21B 117.7 . . ? C22B C21B H21B 117.7 . . ? C23B C22B C27B 118.9(4) . . ? C23B C22B C21B 118.0(4) . . ? C27B C22B C21B 123.1(4) . . ? C24B C23B C22B 121.1(5) . . ? C24B C23B H23B 119.5 . . ? C22B C23B H23B 119.5 . . ? C25B C24B C23B 119.8(5) . . ? C25B C24B H24B 120.1 . . ? C23B C24B H24B 120.1 . . ? C24B C25B C26B 120.8(5) . . ? C24B C25B H25B 119.6 . . ? C26B C25B H25B 119.6 . . ? C25B C26B C27B 119.6(5) . . ? C25B C26B H26B 120.2 . . ? C27B C26B H26B 120.2 . . ? C26B C27B C22B 119.7(4) . . ? C26B C27B N4B 122.7(4) . . ? C22B C27B N4B 117.5(3) . . ? C27B N4B S2B 127.6(3) . . ? C27B N4B H4B 116.2 . . ? S2B N4B H4B 116.2 . . ? O4B S2B O3B 119.7(2) . . ? O4B S2B N4B 103.90(19) . . ? O3B S2B N4B 109.5(2) . . ? O4B S2B C28B 109.2(2) . . ? O3B S2B C28B 108.1(2) . . ? N4B S2B C28B 105.61(17) . . ? C29B C28B C33B 117.8(4) . . ? C29B C28B S2B 122.5(3) . . ? C33B C28B S2B 119.7(3) . . ? C30B C29B C28B 120.7(4) . . ? C30B C29B H29B 119.7 . . ? C28B C29B H29B 119.7 . . ? C31B C30B C29B 121.8(4) . . ? C31B C30B H30B 119.1 . . ? C29B C30B H30B 119.1 . . ? C32B C31B C30B 118.0(4) . . ? C32B C31B C34B 120.9(5) . . ? C30B C31B C34B 121.1(5) . . ? C31B C32B C33B 121.4(4) . . ? C31B C32B H32B 119.3 . . ? C33B C32B H32B 119.3 . . ? C28B C33B C32B 120.5(4) . . ? C28B C33B H33B 119.8 . . ? C32B C33B H33B 119.8 . . ? C31B C34B H341 109.5 . . ? C31B C34B H342 109.5 . . ? H341 C34B H342 109.5 . . ? C31B C34B H343 109.5 . . ? H341 C34B H343 109.5 . . ? H342 C34B H343 109.5 . . ? H1W O1W H2W 128.7 . . ? 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 C7A C2A C3A C4A 1.0(7) . . . . ? C1A C2A C3A C4A -177.7(4) . . . . ? C2A C3A C4A C5A -0.4(6) . . . . ? C3A C4A C5A C6A -0.9(6) . . . . ? C3A C4A C5A S1A 179.6(3) . . . . ? C4A C5A C6A C7A 1.5(6) . . . . ? S1A C5A C6A C7A -179.0(3) . . . . ? C3A C2A C7A C6A -0.4(7) . . . . ? C1A C2A C7A C6A 178.3(4) . . . . ? C5A C6A C7A C2A -0.8(7) . . . . ? C6A C5A S1A O1A 172.3(3) . . . . ? C4A C5A S1A O1A -8.2(4) . . . . ? C6A C5A S1A O2A 40.7(4) . . . . ? C4A C5A S1A O2A -139.8(3) . . . . ? C6A C5A S1A N1A -70.3(3) . . . . ? C4A C5A S1A N1A 109.2(3) . . . . ? O1A S1A N1A C8A 64.6(4) . . . . ? O2A S1A N1A C8A -165.9(3) . . . . ? C5A S1A N1A C8A -50.7(4) . . . . ? S1A N1A C8A C9A -25.3(5) . . . . ? S1A N1A C8A C13A 155.1(3) . . . . ? C13A C8A C9A C10A -3.1(6) . . . . ? N1A C8A C9A C10A 177.3(4) . . . . ? C8A C9A C10A C11A 1.9(7) . . . . ? C9A C10A C11A C12A -0.1(8) . . . . ? C10A C11A C12A C13A -0.4(7) . . . . ? C9A C8A C13A C12A 2.5(5) . . . . ? N1A C8A C13A C12A -177.9(3) . . . . ? C9A C8A C13A C14A -178.1(3) . . . . ? N1A C8A C13A C14A 1.5(5) . . . . ? C11A C12A C13A C8A -0.8(6) . . . . ? C11A C12A C13A C14A 179.8(4) . . . . ? C8A C13A C14A N2A 5.0(5) . . . . ? C12A C13A C14A N2A -175.6(4) . . . . ? C13A C14A N2A C15A 176.9(3) . . . . ? C14A N2A C15A C20A 143.9(3) . . . . ? C14A N2A C15A C16A -94.9(4) . . . . ? N2A C15A C16A C17A -179.2(3) . . . . ? C20A C15A C16A C17A -58.1(4) . . . . ? C15A C16A C17A C18A 55.3(5) . . . . ? C16A C17A C18A C19A -53.8(5) . . . . ? C17A C18A C19A C20A 55.1(5) . . . . ? C18A C19A C20A N3A -177.3(3) . . . . ? C18A C19A C20A C15A -57.4(4) . . . . ? N2A C15A C20A N3A -60.2(3) . . . . ? C16A C15A C20A N3A 178.5(3) . . . . ? N2A C15A C20A C19A -179.8(3) . . . . ? C16A C15A C20A C19A 59.0(4) . . . . ? C19A C20A N3A C21A -105.9(4) . . . . ? C15A C20A N3A C21A 134.0(3) . . . . ? C20A N3A C21A C22A 179.3(3) . . . . ? N3A C21A C22A C23A -179.8(3) . . . . ? N3A C21A C22A C27A 2.2(5) . . . . ? C27A C22A C23A C24A -0.1(5) . . . . ? C21A C22A C23A C24A -178.1(3) . . . . ? C22A C23A C24A C25A -0.5(6) . . . . ? C23A C24A C25A C26A 0.5(7) . . . . ? C24A C25A C26A C27A 0.1(6) . . . . ? C25A C26A C27A N4A -177.4(3) . . . . ? C25A C26A C27A C22A -0.6(5) . . . . ? C23A C22A C27A C26A 0.6(5) . . . . ? C21A C22A C27A C26A 178.5(3) . . . . ? C23A C22A C27A N4A 177.6(3) . . . . ? C21A C22A C27A N4A -4.5(5) . . . . ? C26A C27A N4A S2A -23.9(5) . . . . ? C22A C27A N4A S2A 159.2(3) . . . . ? C27A N4A S2A O3A 58.3(4) . . . . ? C27A N4A S2A O4A -173.0(3) . . . . ? C27A N4A S2A C28A -58.1(3) . . . . ? O3A S2A C28A C33A -173.1(3) . . . . ? O4A S2A C28A C33A 56.4(4) . . . . ? N4A S2A C28A C33A -54.9(4) . . . . ? O3A S2A C28A C29A 7.5(4) . . . . ? O4A S2A C28A C29A -122.9(4) . . . . ? N4A S2A C28A C29A 125.8(4) . . . . ? C33A C28A C29A C30A -1.7(8) . . . . ? S2A C28A C29A C30A 177.7(4) . . . . ? C28A C29A C30A C31A 1.5(9) . . . . ? C29A C30A C31A C32A -0.2(8) . . . . ? C29A C30A C31A C34A -179.4(5) . . . . ? C30A C31A C32A C33A -0.8(7) . . . . ? C34A C31A C32A C33A 178.3(4) . . . . ? C29A C28A C33A C32A 0.6(7) . . . . ? S2A C28A C33A C32A -178.8(4) . . . . ? C31A C32A C33A C28A 0.6(7) . . . . ? C7B C2B C3B C4B -2.2(7) . . . . ? C1B C2B C3B C4B 177.6(4) . . . . ? C2B C3B C4B C5B 2.0(6) . . . . ? C3B C4B C5B C6B -1.0(6) . . . . ? C3B C4B C5B S1B -178.3(3) . . . . ? C4B C5B C6B C7B 0.3(6) . . . . ? S1B C5B C6B C7B 177.6(3) . . . . ? C5B C6B C7B C2B -0.6(7) . . . . ? C3B C2B C7B C6B 1.5(7) . . . . ? C1B C2B C7B C6B -178.4(4) . . . . ? C8B N1B S1B O2B -170.1(3) . . . . ? C8B N1B S1B O1B 59.8(4) . . . . ? C8B N1B S1B C5B -55.2(4) . . . . ? C4B C5B S1B O2B -137.2(3) . . . . ? C6B C5B S1B O2B 45.5(4) . . . . ? C4B C5B S1B O1B -4.8(4) . . . . ? C6B C5B S1B O1B 177.9(3) . . . . ? C4B C5B S1B N1B 111.7(3) . . . . ? C6B C5B S1B N1B -65.6(4) . . . . ? S1B N1B C8B C13B 159.8(3) . . . . ? S1B N1B C8B C9B -19.5(5) . . . . ? C13B C8B C9B C10B -2.5(6) . . . . ? N1B C8B C9B C10B 176.8(4) . . . . ? C8B C9B C10B C11B 2.5(7) . . . . ? C9B C10B C11B C12B -0.4(8) . . . . ? C10B C11B C12B C13B -1.7(7) . . . . ? C9B C8B C13B C12B 0.6(5) . . . . ? N1B C8B C13B C12B -178.8(3) . . . . ? C9B C8B C13B C14B 179.2(3) . . . . ? N1B C8B C13B C14B -0.1(5) . . . . ? C11B C12B C13B C8B 1.5(6) . . . . ? C11B C12B C13B C14B -177.2(4) . . . . ? C8B C13B C14B N2B 1.7(5) . . . . ? C12B C13B C14B N2B -179.6(4) . . . . ? C13B C14B N2B C15B 179.4(3) . . . . ? C14B N2B C15B C20B 149.7(3) . . . . ? C14B N2B C15B C16B -89.1(4) . . . . ? N2B C15B C16B C17B -178.8(3) . . . . ? C20B C15B C16B C17B -58.0(4) . . . . ? C15B C16B C17B C18B 55.9(4) . . . . ? C16B C17B C18B C19B -54.5(5) . . . . ? C17B C18B C19B C20B 55.0(5) . . . . ? N2B C15B C20B N3B -62.1(4) . . . . ? C16B C15B C20B N3B 177.4(2) . . . . ? N2B C15B C20B C19B 178.5(3) . . . . ? C16B C15B C20B C19B 57.9(4) . . . . ? C18B C19B C20B N3B -177.0(3) . . . . ? C18B C19B C20B C15B -56.5(4) . . . . ? C15B C20B N3B C21B 138.0(3) . . . . ? C19B C20B N3B C21B -101.3(4) . . . . ? C20B N3B C21B C22B 177.7(3) . . . . ? N3B C21B C22B C23B -178.4(3) . . . . ? N3B C21B C22B C27B 0.1(6) . . . . ? C27B C22B C23B C24B 2.1(6) . . . . ? C21B C22B C23B C24B -179.3(4) . . . . ? C22B C23B C24B C25B -1.5(7) . . . . ? C23B C24B C25B C26B 0.4(8) . . . . ? C24B C25B C26B C27B 0.2(8) . . . . ? C25B C26B C27B C22B 0.4(6) . . . . ? C25B C26B C27B N4B -178.5(4) . . . . ? C23B C22B C27B C26B -1.5(6) . . . . ? C21B C22B C27B C26B 180.0(4) . . . . ? C23B C22B C27B N4B 177.5(3) . . . . ? C21B C22B C27B N4B -1.0(5) . . . . ? C26B C27B N4B S2B -24.3(5) . . . . ? C22B C27B N4B S2B 156.7(3) . . . . ? C27B N4B S2B O4B -176.9(3) . . . . ? C27B N4B S2B O3B 54.1(4) . . . . ? C27B N4B S2B C28B -62.0(4) . . . . ? O4B S2B C28B C29B -127.8(3) . . . . ? O3B S2B C28B C29B 3.9(4) . . . . ? N4B S2B C28B C29B 121.0(3) . . . . ? O4B S2B C28B C33B 51.8(4) . . . . ? O3B S2B C28B C33B -176.4(3) . . . . ? N4B S2B C28B C33B -59.3(4) . . . . ? C33B C28B C29B C30B -1.5(6) . . . . ? S2B C28B C29B C30B 178.1(3) . . . . ? C28B C29B C30B C31B 1.5(7) . . . . ? C29B C30B C31B C32B -1.1(7) . . . . ? C29B C30B C31B C34B -178.7(4) . . . . ? C30B C31B C32B C33B 0.8(7) . . . . ? C34B C31B C32B C33B 178.4(4) . . . . ? C29B C28B C33B C32B 1.2(6) . . . . ? S2B C28B C33B C32B -178.5(3) . . . . ? C31B C32B C33B C28B -0.9(7) . . . . ? 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 N1A H1A N2A 0.86 2.04 2.669(4) 129.3 . N4A H4A N3A 0.86 2.01 2.639(4) 129.0 . N1B H1B N2B 0.86 1.99 2.642(4) 132.2 . N4B H4B N3B 0.86 2.01 2.632(4) 128.9 . O1W H1W O2A 0.85 2.32 2.995(15) 136.4 . O1W H2W O4A 0.91 2.36 3.27(2) 174.8 2_755 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.249 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.035 data_H2cyts _database_code_CSD 155429 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H36 N4 O4 S2' _chemical_formula_weight 628.79 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 '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 11.2798(3) _cell_length_b 15.2754(4) _cell_length_c 18.9152(3) _cell_angle_alpha 90.00 _cell_angle_beta 92.9210(10) _cell_angle_gamma 90.00 _cell_volume 3254.92(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 107 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Pale brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.283 _exptl_crystal_density_method ? _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.207 _exptl_absorpt_correction_type 'Sadabs' _exptl_absorpt_correction_T_min 0.676211 _exptl_absorpt_correction_T_max 0.977511 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens CCD' _diffrn_measurement_method '\w scans' _diffrn_standards_number '50 first frames' _diffrn_standards_interval_count 'end of measurement' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13155 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0857 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5722 _reflns_number_gt 2823 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _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^)+(0.0453P)^2^+0.9227P] 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 5722 _refine_ls_number_parameters 454 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1532 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1127 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0906(5) 0.3323(3) 0.4314(3) 0.121(2) Uani 1 1 d . . . H1C H 1.1758 0.3310 0.4323 0.181 Uiso 1 1 calc R . . H1D H 1.0615 0.2769 0.4470 0.181 Uiso 1 1 calc R . . H1E H 1.0652 0.3778 0.4622 0.181 Uiso 1 1 calc R . . C2 C 1.0422(4) 0.3500(3) 0.3567(3) 0.0752(12) Uani 1 1 d . . . C3 C 1.1068(4) 0.3294(3) 0.2995(3) 0.0871(14) Uani 1 1 d . . . H3B H 1.1821 0.3053 0.3069 0.104 Uiso 1 1 calc R . . C4 C 1.0624(4) 0.3434(3) 0.2321(3) 0.0759(12) Uani 1 1 d . . . H4C H 1.1081 0.3289 0.1943 0.091 Uiso 1 1 calc R . . C5 C 0.9511(3) 0.3786(2) 0.2191(2) 0.0556(10) Uani 1 1 d . . . C6 C 0.8862(3) 0.4015(2) 0.2761(2) 0.0669(11) Uani 1 1 d . . . H6A H 0.8116 0.4267 0.2688 0.080 Uiso 1 1 calc R . . C7 C 0.9325(4) 0.3870(3) 0.3441(2) 0.0768(12) Uani 1 1 d . . . H7A H 0.8882 0.4026 0.3822 0.092 Uiso 1 1 calc R . . S1 S 0.89242(11) 0.39826(8) 0.13325(6) 0.0770(4) Uani 1 1 d . . . O1 O 0.8331(3) 0.48177(18) 0.13218(15) 0.0950(10) Uani 1 1 d . . . O2 O 0.9837(3) 0.3803(2) 0.08581(16) 0.1087(11) Uani 1 1 d . . . N1 N 0.7851(3) 0.3282(2) 0.11965(15) 0.0686(9) Uani 1 1 d . . . H1B H 0.7155 0.3503 0.1123 0.082 Uiso 1 1 calc R . . C8 C 0.7908(3) 0.2367(2) 0.11828(17) 0.0552(9) Uani 1 1 d . . . C9 C 0.8963(4) 0.1902(3) 0.1202(2) 0.0791(12) Uani 1 1 d . . . H9A H 0.9684 0.2198 0.1209 0.095 Uiso 1 1 calc R . . C10 C 0.8946(4) 0.1004(3) 0.1212(3) 0.0984(15) Uani 1 1 d . . . H10A H 0.9661 0.0699 0.1239 0.118 Uiso 1 1 calc R . . C11 C 0.7901(5) 0.0546(3) 0.1185(3) 0.0988(16) Uani 1 1 d . . . H11A H 0.7904 -0.0062 0.1195 0.119 Uiso 1 1 calc R . . C12 C 0.6853(4) 0.0996(3) 0.1142(2) 0.0725(11) Uani 1 1 d . . . H12A H 0.6142 0.0687 0.1110 0.087 Uiso 1 1 calc R . . C13 C 0.6828(3) 0.1905(2) 0.11447(17) 0.0531(9) Uani 1 1 d . . . C14 C 0.5681(3) 0.2332(2) 0.11008(17) 0.0551(10) Uani 1 1 d . A . H14A H 0.5009 0.1980 0.1116 0.066 Uiso 1 1 calc R . . N2 N 0.5528(3) 0.3151(2) 0.10431(15) 0.0596(8) Uani 1 1 d . . . C15 C 0.4364(7) 0.3470(6) 0.0948(4) 0.051(2) Uani 0.793(10) 1 d P A 1 H15A H 0.3855 0.3156 0.1268 0.061 Uiso 0.793(10) 1 calc PR A 1 C16 C 0.3856(6) 0.3368(5) 0.0199(4) 0.065(2) Uani 0.793(10) 1 d P A 1 H16A H 0.3804 0.2750 0.0084 0.077 Uiso 0.793(10) 1 calc PR A 1 H16B H 0.4388 0.3639 -0.0123 0.077 Uiso 0.793(10) 1 calc PR A 1 C17 C 0.2603(7) 0.3789(5) 0.0092(4) 0.078(2) Uani 0.793(10) 1 d P A 1 H17A H 0.2347 0.3759 -0.0405 0.094 Uiso 0.793(10) 1 calc PR A 1 H17B H 0.2042 0.3459 0.0358 0.094 Uiso 0.793(10) 1 calc PR A 1 C18 C 0.2601(7) 0.4732(5) 0.0331(4) 0.081(2) Uani 0.793(10) 1 d P A 1 H18A H 0.3061 0.5080 0.0015 0.097 Uiso 0.793(10) 1 calc PR A 1 H18B H 0.1793 0.4951 0.0304 0.097 Uiso 0.793(10) 1 calc PR A 1 C19 C 0.3112(6) 0.4832(4) 0.1076(3) 0.072(2) Uani 0.793(10) 1 d P A 1 H19A H 0.2608 0.4532 0.1398 0.086 Uiso 0.793(10) 1 calc PR A 1 H19B H 0.3130 0.5447 0.1202 0.086 Uiso 0.793(10) 1 calc PR A 1 C20 C 0.4398(7) 0.4448(6) 0.1156(5) 0.054(2) Uani 0.793(10) 1 d P A 1 H20A H 0.4928 0.4770 0.0854 0.064 Uiso 0.793(10) 1 calc PR A 1 C15' C 0.398(3) 0.356(3) 0.1181(16) 0.065(10) Uani 0.207(10) 1 d P A 2 H15B H 0.3695 0.3247 0.1591 0.077 Uiso 0.207(10) 1 calc PR A 2 C16' C 0.317(3) 0.3284(17) 0.0535(16) 0.097(12) Uani 0.207(10) 1 d P A 2 H16C H 0.3287 0.2668 0.0436 0.116 Uiso 0.207(10) 1 calc PR A 2 H16D H 0.2348 0.3377 0.0633 0.116 Uiso 0.207(10) 1 calc PR A 2 C17' C 0.347(3) 0.379(2) -0.0046(14) 0.077(9) Uani 0.207(10) 1 d P A 2 H17C H 0.2950 0.3638 -0.0453 0.092 Uiso 0.207(10) 1 calc PR A 2 H17D H 0.4280 0.3661 -0.0163 0.092 Uiso 0.207(10) 1 calc PR A 2 C18' C 0.334(3) 0.482(2) 0.0141(14) 0.082(9) Uani 0.207(10) 1 d P A 2 H18C H 0.3555 0.5175 -0.0257 0.098 Uiso 0.207(10) 1 calc PR A 2 H18D H 0.2522 0.4952 0.0242 0.098 Uiso 0.207(10) 1 calc PR A 2 C19' C 0.416(3) 0.5016(17) 0.0783(11) 0.085(9) Uani 0.207(10) 1 d P A 2 H19C H 0.4975 0.4927 0.0669 0.102 Uiso 0.207(10) 1 calc PR A 2 H19D H 0.4061 0.5620 0.0927 0.102 Uiso 0.207(10) 1 calc PR A 2 C20' C 0.387(2) 0.446(2) 0.1323(17) 0.045(8) Uani 0.207(10) 1 d P A 2 H20B H 0.3078 0.4598 0.1486 0.054 Uiso 0.207(10) 1 calc PR A 2 N3 N 0.4789(3) 0.45551(19) 0.19108(17) 0.0654(9) Uani 1 1 d . . . C21 C 0.5536(3) 0.5158(2) 0.2044(2) 0.0669(11) Uani 1 1 d . A . H21A H 0.5760 0.5508 0.1672 0.080 Uiso 1 1 calc R . . C22 C 0.6071(3) 0.5336(2) 0.2754(2) 0.0595(10) Uani 1 1 d . . . C23 C 0.6870(4) 0.6031(3) 0.2824(3) 0.0822(13) Uani 1 1 d . A . H23A H 0.7025 0.6369 0.2431 0.099 Uiso 1 1 calc R . . C24 C 0.7436(4) 0.6225(3) 0.3473(3) 0.0962(15) Uani 1 1 d . . . H24A H 0.7971 0.6687 0.3518 0.115 Uiso 1 1 calc R A . C25 C 0.7192(4) 0.5725(4) 0.4045(3) 0.0955(16) Uani 1 1 d . A . H25A H 0.7574 0.5852 0.4481 0.115 Uiso 1 1 calc R . . C26 C 0.6404(4) 0.5042(3) 0.4002(2) 0.0789(12) Uani 1 1 d . . . H26A H 0.6247 0.4717 0.4403 0.095 Uiso 1 1 calc R A . C27 C 0.5846(3) 0.4841(2) 0.3352(2) 0.0592(10) Uani 1 1 d . A . N4 N 0.5018(3) 0.4155(2) 0.32654(16) 0.0656(9) Uani 1 1 d . . . H4B H 0.4519 0.4195 0.2908 0.079 Uiso 1 1 calc R A . S2 S 0.48975(9) 0.32936(7) 0.37643(6) 0.0706(3) Uani 1 1 d . A . O3 O 0.3968(2) 0.27953(19) 0.34146(16) 0.0915(9) Uani 1 1 d . . . O4 O 0.4807(3) 0.3560(2) 0.44876(14) 0.0945(10) Uani 1 1 d . . . C28 C 0.6230(3) 0.2710(2) 0.3708(2) 0.0558(9) Uani 1 1 d . . . C29 C 0.6987(4) 0.2575(3) 0.42907(19) 0.0652(11) Uani 1 1 d . A . H29A H 0.6811 0.2815 0.4725 0.078 Uiso 1 1 calc R . . C30 C 0.7999(4) 0.2088(3) 0.4236(2) 0.0707(12) Uani 1 1 d . . . H30A H 0.8489 0.1991 0.4639 0.085 Uiso 1 1 calc R A . C31 C 0.8306(4) 0.1743(2) 0.3606(2) 0.0671(11) Uani 1 1 d . A . C32 C 0.7540(4) 0.1880(3) 0.3021(2) 0.0742(12) Uani 1 1 d . . . H32A H 0.7725 0.1642 0.2588 0.089 Uiso 1 1 calc R A . C33 C 0.6514(4) 0.2359(3) 0.3062(2) 0.0673(11) Uani 1 1 d . A . H33A H 0.6017 0.2447 0.2661 0.081 Uiso 1 1 calc R . . C34 C 0.9415(4) 0.1198(3) 0.3542(3) 0.1037(16) Uani 1 1 d . . . H34A H 0.9812 0.1134 0.4001 0.156 Uiso 1 1 calc R A . H34B H 0.9935 0.1483 0.3228 0.156 Uiso 1 1 calc R . . H34C H 0.9203 0.0631 0.3357 0.156 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.136(4) 0.120(4) 0.101(4) 0.025(3) -0.056(3) -0.042(4) C2 0.074(3) 0.061(3) 0.086(4) 0.006(2) -0.035(3) -0.014(2) C3 0.055(3) 0.083(3) 0.120(4) -0.002(3) -0.028(3) 0.003(2) C4 0.055(3) 0.080(3) 0.093(4) -0.014(3) 0.002(2) -0.007(2) C5 0.049(2) 0.051(2) 0.066(3) -0.0004(19) -0.007(2) -0.0116(19) C6 0.055(2) 0.064(3) 0.081(3) 0.007(2) -0.007(2) 0.001(2) C7 0.085(3) 0.070(3) 0.075(3) -0.001(2) 0.000(3) -0.015(3) S1 0.0812(8) 0.0753(8) 0.0729(8) 0.0103(6) -0.0114(6) -0.0296(7) O1 0.115(2) 0.0572(19) 0.108(2) 0.0222(16) -0.0422(18) -0.0228(17) O2 0.103(2) 0.146(3) 0.078(2) 0.000(2) 0.0186(18) -0.048(2) N1 0.069(2) 0.055(2) 0.079(2) 0.0062(17) -0.0213(16) -0.0155(17) C8 0.063(3) 0.057(3) 0.045(2) -0.0030(18) -0.0027(18) -0.002(2) C9 0.066(3) 0.077(3) 0.095(3) -0.009(3) 0.000(2) -0.002(3) C10 0.078(4) 0.087(4) 0.129(4) -0.018(3) -0.003(3) 0.022(3) C11 0.094(4) 0.056(3) 0.146(5) -0.002(3) 0.008(3) 0.014(3) C12 0.080(3) 0.049(3) 0.088(3) 0.004(2) 0.003(2) 0.002(2) C13 0.059(3) 0.053(3) 0.047(2) 0.0018(18) -0.0017(17) 0.002(2) C14 0.066(3) 0.046(2) 0.052(2) 0.0023(18) -0.0035(18) -0.010(2) N2 0.069(2) 0.046(2) 0.062(2) -0.0033(15) -0.0183(15) 0.0010(16) C15 0.051(5) 0.040(4) 0.061(5) -0.016(3) 0.000(3) 0.014(3) C16 0.060(5) 0.078(4) 0.053(5) -0.016(3) -0.025(4) 0.024(4) C17 0.053(5) 0.092(5) 0.087(5) -0.011(4) -0.027(3) 0.026(4) C18 0.076(5) 0.090(5) 0.074(5) -0.006(4) -0.021(4) 0.034(5) C19 0.073(5) 0.071(4) 0.071(4) -0.008(3) -0.014(4) 0.033(4) C20 0.053(6) 0.053(4) 0.054(6) -0.003(4) -0.006(4) 0.016(4) C15' 0.07(2) 0.084(19) 0.040(17) -0.047(16) -0.033(14) 0.064(18) C16' 0.11(3) 0.072(17) 0.11(3) -0.022(17) 0.06(2) 0.006(17) C17' 0.047(19) 0.11(2) 0.068(19) -0.042(17) -0.049(14) 0.005(17) C18' 0.09(2) 0.091(19) 0.061(16) 0.017(13) -0.003(16) 0.027(19) C19' 0.12(2) 0.090(18) 0.045(14) 0.029(12) -0.036(14) -0.030(15) C20' 0.023(16) 0.061(15) 0.050(18) -0.018(12) -0.009(12) 0.018(15) N3 0.077(2) 0.049(2) 0.068(2) -0.0098(17) -0.0225(17) 0.0081(17) C21 0.082(3) 0.050(2) 0.067(3) 0.002(2) -0.013(2) 0.008(2) C22 0.059(2) 0.049(2) 0.069(3) -0.006(2) -0.010(2) 0.007(2) C23 0.081(3) 0.061(3) 0.103(4) -0.005(3) -0.015(3) 0.000(2) C24 0.084(3) 0.074(3) 0.127(5) -0.019(3) -0.035(3) -0.007(3) C25 0.091(4) 0.093(4) 0.098(4) -0.023(3) -0.040(3) 0.008(3) C26 0.081(3) 0.084(3) 0.068(3) -0.010(2) -0.021(2) 0.008(3) C27 0.048(2) 0.053(2) 0.074(3) -0.011(2) -0.010(2) 0.0115(19) N4 0.057(2) 0.064(2) 0.075(2) 0.0033(17) -0.0120(16) 0.0067(17) S2 0.0590(7) 0.0806(8) 0.0727(8) 0.0064(6) 0.0072(5) 0.0036(6) O3 0.0561(18) 0.098(2) 0.120(3) 0.0160(18) -0.0047(16) -0.0144(16) O4 0.102(2) 0.122(3) 0.0613(19) -0.0026(17) 0.0301(16) 0.0226(19) C28 0.060(2) 0.056(2) 0.051(3) 0.005(2) 0.0018(19) 0.0004(19) C29 0.073(3) 0.080(3) 0.042(2) 0.001(2) -0.004(2) 0.002(2) C30 0.072(3) 0.072(3) 0.067(3) 0.016(2) -0.016(2) 0.002(2) C31 0.076(3) 0.051(2) 0.074(3) 0.014(2) 0.001(2) 0.004(2) C32 0.099(3) 0.068(3) 0.056(3) -0.001(2) 0.009(2) 0.017(3) C33 0.080(3) 0.070(3) 0.051(3) 0.004(2) -0.007(2) 0.015(2) C34 0.085(3) 0.080(3) 0.146(5) 0.019(3) 0.008(3) 0.023(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 C1 C2 1.512(6) . ? C1 H1C 0.9600 . ? C1 H1D 0.9600 . ? C1 H1E 0.9600 . ? C2 C7 1.370(5) . ? C2 C3 1.371(6) . ? C3 C4 1.363(6) . ? C3 H3B 0.9300 . ? C4 C5 1.377(5) . ? C4 H4C 0.9300 . ? C5 C6 1.379(5) . ? C5 S1 1.747(4) . ? C6 C7 1.380(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? S1 O2 1.426(3) . ? S1 O1 1.440(3) . ? S1 N1 1.626(3) . ? N1 C8 1.398(4) . ? N1 H1B 0.8600 . ? C8 C9 1.386(5) . ? C8 C13 1.407(5) . ? C9 C10 1.372(6) . ? C9 H9A 0.9300 . ? C10 C11 1.370(6) . ? C10 H10A 0.9300 . ? C11 C12 1.366(5) . ? C11 H11A 0.9300 . ? C12 C13 1.389(5) . ? C12 H12A 0.9300 . ? C13 C14 1.447(5) . ? C14 N2 1.267(4) . ? C14 H14A 0.9300 . ? N2 C15 1.405(8) . ? N2 C15' 1.89(3) . ? C15 C16 1.508(11) . ? C15 C20 1.544(13) . ? C15 H15A 0.9800 . ? C16 C17 1.557(10) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.509(10) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.503(8) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.565(10) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 N3 1.482(9) . ? C20 H20A 0.9800 . ? C15' C20' 1.41(5) . ? C15' C16' 1.54(5) . ? C15' H15B 0.9800 . ? C16' C17' 1.39(4) . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C17' C18' 1.63(4) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' C19' 1.52(3) . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19' C20' 1.38(4) . ? C19' H19C 0.9700 . ? C19' H19D 0.9700 . ? C20' N3 1.49(3) . ? C20' H20B 0.9800 . ? N3 C21 1.266(4) . ? C21 C22 1.468(5) . ? C21 H21A 0.9300 . ? C22 C23 1.393(5) . ? C22 C27 1.396(5) . ? C23 C24 1.387(6) . ? C23 H23A 0.9300 . ? C24 C25 1.364(6) . ? C24 H24A 0.9300 . ? C25 C26 1.370(6) . ? C25 H25A 0.9300 . ? C26 C27 1.386(5) . ? C26 H26A 0.9300 . ? C27 N4 1.408(4) . ? N4 S2 1.629(3) . ? N4 H4B 0.8600 . ? S2 O3 1.431(3) . ? S2 O4 1.436(3) . ? S2 C28 1.755(4) . ? C28 C29 1.375(5) . ? C28 C33 1.386(5) . ? C29 C30 1.371(5) . ? C29 H29A 0.9300 . ? C30 C31 1.364(5) . ? C30 H30A 0.9300 . ? C31 C32 1.384(5) . ? C31 C34 1.513(5) . ? C32 C33 1.374(5) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1C 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 109.5 . . ? C2 C1 H1E 109.5 . . ? H1C C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? C7 C2 C3 117.9(4) . . ? C7 C2 C1 121.1(5) . . ? C3 C2 C1 121.0(5) . . ? C4 C3 C2 121.1(4) . . ? C4 C3 H3B 119.4 . . ? C2 C3 H3B 119.4 . . ? C3 C4 C5 121.2(4) . . ? C3 C4 H4C 119.4 . . ? C5 C4 H4C 119.4 . . ? C4 C5 C6 118.3(4) . . ? C4 C5 S1 122.2(3) . . ? C6 C5 S1 119.5(3) . . ? C5 C6 C7 119.8(4) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C2 C7 C6 121.6(4) . . ? C2 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? O2 S1 O1 120.8(2) . . ? O2 S1 N1 109.18(19) . . ? O1 S1 N1 103.84(17) . . ? O2 S1 C5 107.5(2) . . ? O1 S1 C5 108.59(18) . . ? N1 S1 C5 106.10(16) . . ? C8 N1 S1 128.8(3) . . ? C8 N1 H1B 115.6 . . ? S1 N1 H1B 115.6 . . ? C9 C8 N1 123.5(4) . . ? C9 C8 C13 119.0(4) . . ? N1 C8 C13 117.6(3) . . ? C10 C9 C8 120.0(4) . . ? C10 C9 H9A 120.0 . . ? C8 C9 H9A 120.0 . . ? C11 C10 C9 121.5(4) . . ? C11 C10 H10A 119.2 . . ? C9 C10 H10A 119.2 . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 121.3(4) . . ? C11 C12 H12A 119.3 . . ? C13 C12 H12A 119.3 . . ? C12 C13 C8 119.0(4) . . ? C12 C13 C14 117.9(4) . . ? C8 C13 C14 123.1(3) . . ? N2 C14 C13 124.5(3) . . ? N2 C14 H14A 117.7 . . ? C13 C14 H14A 117.7 . . ? C14 N2 C15 118.4(5) . . ? C14 N2 C15' 116.0(14) . . ? C15 N2 C15' 15.3(11) . . ? N2 C15 C16 113.1(5) . . ? N2 C15 C20 107.0(6) . . ? C16 C15 C20 110.0(7) . . ? N2 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C20 C15 H15A 108.9 . . ? C15 C16 C17 112.2(6) . . ? C15 C16 H16A 109.2 . . ? C17 C16 H16A 109.2 . . ? C15 C16 H16B 109.2 . . ? C17 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? C18 C17 C16 111.8(6) . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C17 111.8(6) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C18 C19 C20 111.2(5) . . ? C18 C19 H19A 109.4 . . ? C20 C19 H19A 109.4 . . ? C18 C19 H19B 109.4 . . ? C20 C19 H19B 109.4 . . ? H19A C19 H19B 108.0 . . ? N3 C20 C15 110.8(7) . . ? N3 C20 C19 106.3(6) . . ? C15 C20 C19 109.1(7) . . ? N3 C20 H20A 110.2 . . ? C15 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? C20' C15' C16' 111(3) . . ? C20' C15' N2 116(3) . . ? C16' C15' N2 108.2(18) . . ? C20' C15' H15B 106.9 . . ? C16' C15' H15B 106.9 . . ? N2 C15' H15B 106.9 . . ? C17' C16' C15' 109(3) . . ? C17' C16' H16C 110.0 . . ? C15' C16' H16C 110.0 . . ? C17' C16' H16D 110.0 . . ? C15' C16' H16D 110.0 . . ? H16C C16' H16D 108.3 . . ? C16' C17' C18' 109(2) . . ? C16' C17' H17C 109.8 . . ? C18' C17' H17C 109.8 . . ? C16' C17' H17D 109.8 . . ? C18' C17' H17D 109.8 . . ? H17C C17' H17D 108.2 . . ? C19' C18' C17' 108(2) . . ? C19' C18' H18C 110.1 . . ? C17' C18' H18C 110.1 . . ? C19' C18' H18D 110.1 . . ? C17' C18' H18D 110.1 . . ? H18C C18' H18D 108.4 . . ? C20' C19' C18' 108(2) . . ? C20' C19' H19C 110.0 . . ? C18' C19' H19C 110.0 . . ? C20' C19' H19D 110.0 . . ? C18' C19' H19D 110.0 . . ? H19C C19' H19D 108.4 . . ? C19' C20' C15' 116(3) . . ? C19' C20' N3 108(2) . . ? C15' C20' N3 100(2) . . ? C19' C20' H20B 110.9 . . ? C15' C20' H20B 110.9 . . ? N3 C20' H20B 110.9 . . ? C21 N3 C20 115.8(5) . . ? C21 N3 C20' 130.5(14) . . ? C20 N3 C20' 26.9(9) . . ? N3 C21 C22 123.8(4) . . ? N3 C21 H21A 118.1 . . ? C22 C21 H21A 118.1 . . ? C23 C22 C27 118.6(4) . . ? C23 C22 C21 117.5(4) . . ? C27 C22 C21 123.9(4) . . ? C24 C23 C22 121.0(4) . . ? C24 C23 H23A 119.5 . . ? C22 C23 H23A 119.5 . . ? C25 C24 C23 118.6(5) . . ? C25 C24 H24A 120.7 . . ? C23 C24 H24A 120.7 . . ? C24 C25 C26 122.4(5) . . ? C24 C25 H25A 118.8 . . ? C26 C25 H25A 118.8 . . ? C25 C26 C27 119.1(4) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C26 C27 C22 120.4(4) . . ? C26 C27 N4 122.5(4) . . ? C22 C27 N4 117.1(3) . . ? C27 N4 S2 127.5(3) . . ? C27 N4 H4B 116.3 . . ? S2 N4 H4B 116.3 . . ? O3 S2 O4 120.35(18) . . ? O3 S2 N4 104.04(17) . . ? O4 S2 N4 109.57(18) . . ? O3 S2 C28 108.16(18) . . ? O4 S2 C28 107.75(18) . . ? N4 S2 C28 106.13(16) . . ? C29 C28 C33 119.1(3) . . ? C29 C28 S2 121.7(3) . . ? C33 C28 S2 119.2(3) . . ? C30 C29 C28 120.5(4) . . ? C30 C29 H29A 119.8 . . ? C28 C29 H29A 119.8 . . ? C31 C30 C29 121.6(4) . . ? C31 C30 H30A 119.2 . . ? C29 C30 H30A 119.2 . . ? C30 C31 C32 117.7(4) . . ? C30 C31 C34 122.0(4) . . ? C32 C31 C34 120.3(4) . . ? C33 C32 C31 121.9(4) . . ? C33 C32 H32A 119.0 . . ? C31 C32 H32A 119.0 . . ? C32 C33 C28 119.3(4) . . ? C32 C33 H33A 120.4 . . ? C28 C33 H33A 120.4 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 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 C7 C2 C3 C4 -1.3(6) . . . . ? C1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C6 1.6(6) . . . . ? C3 C4 C5 S1 179.4(3) . . . . ? C4 C5 C6 C7 -1.5(5) . . . . ? S1 C5 C6 C7 -179.4(3) . . . . ? C3 C2 C7 C6 1.4(6) . . . . ? C1 C2 C7 C6 -178.4(4) . . . . ? C5 C6 C7 C2 0.0(6) . . . . ? C4 C5 S1 O2 -6.0(4) . . . . ? C6 C5 S1 O2 171.8(3) . . . . ? C4 C5 S1 O1 -138.2(3) . . . . ? C6 C5 S1 O1 39.6(3) . . . . ? C4 C5 S1 N1 110.7(3) . . . . ? C6 C5 S1 N1 -71.5(3) . . . . ? O2 S1 N1 C8 52.8(4) . . . . ? O1 S1 N1 C8 -177.1(3) . . . . ? C5 S1 N1 C8 -62.7(4) . . . . ? S1 N1 C8 C9 -8.3(5) . . . . ? S1 N1 C8 C13 171.9(3) . . . . ? N1 C8 C9 C10 177.7(4) . . . . ? C13 C8 C9 C10 -2.5(6) . . . . ? C8 C9 C10 C11 1.7(7) . . . . ? C9 C10 C11 C12 0.4(8) . . . . ? C10 C11 C12 C13 -1.7(7) . . . . ? C11 C12 C13 C8 0.9(6) . . . . ? C11 C12 C13 C14 -179.7(4) . . . . ? C9 C8 C13 C12 1.2(5) . . . . ? N1 C8 C13 C12 -179.0(3) . . . . ? C9 C8 C13 C14 -178.1(3) . . . . ? N1 C8 C13 C14 1.7(5) . . . . ? C12 C13 C14 N2 -174.3(3) . . . . ? C8 C13 C14 N2 5.1(5) . . . . ? C13 C14 N2 C15 174.9(4) . . . . ? C13 C14 N2 C15' -168.1(10) . . . . ? C14 N2 C15 C16 -78.3(7) . . . . ? C15' N2 C15 C16 -163(7) . . . . ? C14 N2 C15 C20 160.4(5) . . . . ? C15' N2 C15 C20 76(6) . . . . ? N2 C15 C16 C17 -175.6(7) . . . . ? C20 C15 C16 C17 -56.1(9) . . . . ? C15 C16 C17 C18 53.3(10) . . . . ? C16 C17 C18 C19 -52.9(10) . . . . ? C17 C18 C19 C20 56.4(9) . . . . ? N2 C15 C20 N3 -62.1(7) . . . . ? C16 C15 C20 N3 174.7(6) . . . . ? N2 C15 C20 C19 -178.7(6) . . . . ? C16 C15 C20 C19 58.1(8) . . . . ? C18 C19 C20 N3 -178.1(6) . . . . ? C18 C19 C20 C15 -58.6(9) . . . . ? C14 N2 C15' C20' 162(2) . . . . ? C15 N2 C15' C20' -95(7) . . . . ? C14 N2 C15' C16' -72(3) . . . . ? C15 N2 C15' C16' 31(4) . . . . ? C20' C15' C16' C17' 57(4) . . . . ? N2 C15' C16' C17' -71(4) . . . . ? C15' C16' C17' C18' -57(4) . . . . ? C16' C17' C18' C19' 59(4) . . . . ? C17' C18' C19' C20' -56(3) . . . . ? C18' C19' C20' C15' 60(4) . . . . ? C18' C19' C20' N3 171(2) . . . . ? C16' C15' C20' C19' -60(4) . . . . ? N2 C15' C20' C19' 65(3) . . . . ? C16' C15' C20' N3 -175(2) . . . . ? N2 C15' C20' N3 -51(3) . . . . ? C15 C20 N3 C21 136.3(5) . . . . ? C19 C20 N3 C21 -105.4(6) . . . . ? C15 C20 N3 C20' -94(4) . . . . ? C19 C20 N3 C20' 25(3) . . . . ? C19' C20' N3 C21 19(3) . . . . ? C15' C20' N3 C21 140(2) . . . . ? C19' C20' N3 C20 -46(3) . . . . ? C15' C20' N3 C20 75(3) . . . . ? C20 N3 C21 C22 -176.9(4) . . . . ? C20' N3 C21 C22 156.0(13) . . . . ? N3 C21 C22 C23 -179.1(4) . . . . ? N3 C21 C22 C27 2.4(6) . . . . ? C27 C22 C23 C24 0.4(6) . . . . ? C21 C22 C23 C24 -178.2(4) . . . . ? C22 C23 C24 C25 -0.3(7) . . . . ? C23 C24 C25 C26 -0.4(7) . . . . ? C24 C25 C26 C27 1.0(7) . . . . ? C25 C26 C27 C22 -0.9(6) . . . . ? C25 C26 C27 N4 -179.4(4) . . . . ? C23 C22 C27 C26 0.2(5) . . . . ? C21 C22 C27 C26 178.8(3) . . . . ? C23 C22 C27 N4 178.9(3) . . . . ? C21 C22 C27 N4 -2.6(5) . . . . ? C26 C27 N4 S2 -23.5(5) . . . . ? C22 C27 N4 S2 157.9(3) . . . . ? C27 N4 S2 O3 -176.8(3) . . . . ? C27 N4 S2 O4 53.3(3) . . . . ? C27 N4 S2 C28 -62.8(3) . . . . ? O3 S2 C28 C29 -131.7(3) . . . . ? O4 S2 C28 C29 -0.1(4) . . . . ? N4 S2 C28 C29 117.2(3) . . . . ? O3 S2 C28 C33 46.8(3) . . . . ? O4 S2 C28 C33 178.4(3) . . . . ? N4 S2 C28 C33 -64.3(3) . . . . ? C33 C28 C29 C30 -1.0(6) . . . . ? S2 C28 C29 C30 177.5(3) . . . . ? C28 C29 C30 C31 1.7(6) . . . . ? C29 C30 C31 C32 -1.7(6) . . . . ? C29 C30 C31 C34 -179.4(4) . . . . ? C30 C31 C32 C33 1.1(6) . . . . ? C34 C31 C32 C33 178.9(4) . . . . ? C31 C32 C33 C28 -0.5(6) . . . . ? C29 C28 C33 C32 0.4(6) . . . . ? S2 C28 C33 C32 -178.1(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 N1 H1B N2 0.86 1.91 2.629(4) 140.1 . N4 H4B N3 0.86 2.00 2.634(4) 129.5 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.164 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.045 #===END data_nicyts _database_code_CSD 168560 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 N4 Ni O4 S2, C2 H3 N' _chemical_formula_sum 'C36 H37 N5 Ni O4 S2' _chemical_formula_weight 726.54 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting '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 12.673(3) _cell_length_b 28.740(7) _cell_length_c 10.0593(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.726(16) _cell_angle_gamma 90.00 _cell_volume 3543.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.711 _exptl_absorpt_correction_type 'Sadabs' _exptl_absorpt_correction_T_min 0.321385 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'Siemens CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% -5.03 _diffrn_reflns_number 14866 _diffrn_reflns_av_R_equivalents 0.0834 _diffrn_reflns_av_sigmaI/netI 0.1054 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.11 _reflns_number_total 6282 _reflns_number_gt 3767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _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^)+(0.0658P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6282 _refine_ls_number_parameters 435 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1476 _refine_ls_wR_factor_gt 0.1251 _refine_ls_goodness_of_fit_ref 0.964 _refine_ls_restrained_S_all 0.964 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.02218(4) 0.144947(17) 0.39566(5) 0.03322(18) Uani 1 1 d . . . N1 N -0.1143(3) 0.16881(11) 0.2861(4) 0.0368(9) Uani 1 1 d . . . N2 N 0.0329(3) 0.19410(11) 0.5222(3) 0.0334(8) Uani 1 1 d . . . N3 N 0.1370(3) 0.11766(11) 0.5270(4) 0.0339(8) Uani 1 1 d . . . N4 N 0.0411(3) 0.09994(11) 0.2628(4) 0.0366(9) Uani 1 1 d . . . C1 C -0.4027(6) 0.0812(3) -0.3263(6) 0.100(2) Uani 1 1 d . . . H1A H -0.3726 0.0518 -0.3428 0.150 Uiso 1 1 calc R . . H1B H -0.3819 0.1046 -0.3829 0.150 Uiso 1 1 calc R . . H1C H -0.4808 0.0790 -0.3483 0.150 Uiso 1 1 calc R . . C2 C -0.3597(5) 0.09436(19) -0.1757(6) 0.0627(15) Uani 1 1 d . . . C3 C -0.4191(5) 0.1190(2) -0.1057(7) 0.087(2) Uani 1 1 d . . . H3A H -0.4898 0.1276 -0.1511 0.105 Uiso 1 1 calc R . . C4 C -0.3791(4) 0.1319(2) 0.0310(6) 0.0762(18) Uani 1 1 d . . . H4A H -0.4230 0.1480 0.0765 0.091 Uiso 1 1 calc R . . C5 C -0.2755(4) 0.12059(14) 0.0971(5) 0.0385(11) Uani 1 1 d . . . C6 C -0.2133(4) 0.09513(18) 0.0298(5) 0.0584(14) Uani 1 1 d . . . H6A H -0.1430 0.0862 0.0755 0.070 Uiso 1 1 calc R . . C7 C -0.2557(4) 0.08292(19) -0.1059(6) 0.0661(16) Uani 1 1 d . . . H7A H -0.2121 0.0664 -0.1512 0.079 Uiso 1 1 calc R . . S1 S -0.21876(9) 0.13555(4) 0.27342(12) 0.0406(3) Uani 1 1 d . . . O1 O -0.1771(3) 0.09283(10) 0.3425(3) 0.0536(9) Uani 1 1 d . . . O2 O -0.3054(3) 0.15915(11) 0.3171(3) 0.0533(9) Uani 1 1 d . . . C8 C -0.1345(3) 0.21722(14) 0.2643(5) 0.0360(10) Uani 1 1 d . . . C9 C -0.2053(4) 0.23438(15) 0.1447(5) 0.0436(12) Uani 1 1 d . . . H9A H -0.2404 0.2137 0.0766 0.052 Uiso 1 1 calc R . . C10 C -0.2241(4) 0.28142(16) 0.1257(5) 0.0502(13) Uani 1 1 d . . . H10A H -0.2710 0.2922 0.0449 0.060 Uiso 1 1 calc R . . C11 C -0.1731(4) 0.31277(16) 0.2268(5) 0.0533(13) Uani 1 1 d . . . H11A H -0.1864 0.3445 0.2143 0.064 Uiso 1 1 calc R . . C12 C -0.1034(4) 0.29679(15) 0.3446(5) 0.0471(12) Uani 1 1 d . . . H12A H -0.0694 0.3179 0.4120 0.057 Uiso 1 1 calc R . . C13 C -0.0822(4) 0.24885(14) 0.3656(5) 0.0364(11) Uani 1 1 d . . . C14 C -0.0079(4) 0.23478(15) 0.4934(4) 0.0381(11) Uani 1 1 d . . . H14A H 0.0122 0.2574 0.5613 0.046 Uiso 1 1 calc R . . C15 C 0.1037(3) 0.18279(14) 0.6592(4) 0.0357(10) Uani 1 1 d . . . H15A H 0.0594 0.1651 0.7085 0.043 Uiso 1 1 calc R . . C16 C 0.1547(4) 0.22284(15) 0.7511(5) 0.0428(11) Uani 1 1 d . . . H16A H 0.2020 0.2404 0.7075 0.051 Uiso 1 1 calc R . . H16B H 0.0981 0.2435 0.7651 0.051 Uiso 1 1 calc R . . C17 C 0.2201(4) 0.20437(17) 0.8881(5) 0.0547(14) Uani 1 1 d . . . H17A H 0.1710 0.1899 0.9357 0.066 Uiso 1 1 calc R . . H17B H 0.2562 0.2301 0.9440 0.066 Uiso 1 1 calc R . . C18 C 0.3053(4) 0.16903(18) 0.8714(5) 0.0586(14) Uani 1 1 d . . . H18A H 0.3400 0.1557 0.9605 0.070 Uiso 1 1 calc R . . H18B H 0.3611 0.1847 0.8377 0.070 Uiso 1 1 calc R . . C19 C 0.2556(4) 0.13004(17) 0.7723(5) 0.0514(13) Uani 1 1 d . . . H19A H 0.3131 0.1100 0.7575 0.062 Uiso 1 1 calc R . . H19B H 0.2074 0.1114 0.8117 0.062 Uiso 1 1 calc R . . C20 C 0.1922(3) 0.15019(14) 0.6362(4) 0.0369(10) Uani 1 1 d . . . H20A H 0.2431 0.1689 0.5997 0.044 Uiso 1 1 calc R . . C21 C 0.1598(4) 0.07395(14) 0.5337(4) 0.0392(11) Uani 1 1 d . . . H21A H 0.2115 0.0635 0.6111 0.047 Uiso 1 1 calc R . . C22 C 0.1116(3) 0.03952(13) 0.4303(5) 0.0365(11) Uani 1 1 d . . . C23 C 0.1276(4) -0.00732(14) 0.4661(5) 0.0458(12) Uani 1 1 d . . . H23A H 0.1669 -0.0155 0.5543 0.055 Uiso 1 1 calc R . . C24 C 0.0858(4) -0.04139(15) 0.3719(5) 0.0498(13) Uani 1 1 d . . . H24A H 0.0953 -0.0726 0.3967 0.060 Uiso 1 1 calc R . . C25 C 0.0300(4) -0.02935(15) 0.2413(5) 0.0484(13) Uani 1 1 d . . . H25A H 0.0017 -0.0526 0.1778 0.058 Uiso 1 1 calc R . . C26 C 0.0151(4) 0.01680(15) 0.2023(5) 0.0441(12) Uani 1 1 d . . . H26A H -0.0220 0.0244 0.1128 0.053 Uiso 1 1 calc R . . C27 C 0.0555(3) 0.05191(13) 0.2968(4) 0.0326(10) Uani 1 1 d . . . S2 S 0.09547(10) 0.11978(4) 0.14564(11) 0.0394(3) Uani 1 1 d . . . O3 O 0.0994(3) 0.16937(10) 0.1616(3) 0.0534(9) Uani 1 1 d . . . O4 O 0.0420(3) 0.10267(11) 0.0108(3) 0.0528(9) Uani 1 1 d . . . C28 C 0.2313(4) 0.09813(16) 0.1798(5) 0.0441(12) Uani 1 1 d . . . C29 C 0.3141(5) 0.1199(2) 0.2760(6) 0.0646(15) Uani 1 1 d . . . H29A H 0.2991 0.1465 0.3207 0.077 Uiso 1 1 calc R . . C30 C 0.4185(5) 0.1024(2) 0.3057(7) 0.0780(19) Uani 1 1 d . . . H30A H 0.4739 0.1177 0.3691 0.094 Uiso 1 1 calc R . . C31 C 0.4426(4) 0.0624(3) 0.2430(8) 0.084(2) Uani 1 1 d . . . C32 C 0.3591(5) 0.0412(2) 0.1450(8) 0.084(2) Uani 1 1 d . . . H32A H 0.3742 0.0147 0.1000 0.101 Uiso 1 1 calc R . . C33 C 0.2536(4) 0.05874(18) 0.1131(6) 0.0608(15) Uani 1 1 d . . . H33A H 0.1985 0.0441 0.0475 0.073 Uiso 1 1 calc R . . C34 C 0.5574(5) 0.0414(3) 0.2769(10) 0.135(4) Uani 1 1 d . . . H34A H 0.5607 0.0175 0.2113 0.203 Uiso 1 1 calc R . . H34B H 0.5740 0.0283 0.3675 0.203 Uiso 1 1 calc R . . H34C H 0.6094 0.0653 0.2730 0.203 Uiso 1 1 calc R . . N1S N 0.4432(7) 0.2056(4) 0.5599(9) 0.162(3) Uani 1 1 d . . . C1S C 0.4844(8) 0.2269(4) 0.6543(11) 0.124(3) Uani 1 1 d . . . C2S C 0.5418(9) 0.2523(4) 0.7797(11) 0.199(6) Uani 1 1 d . . . H2S1 H 0.5924 0.2317 0.8390 0.299 Uiso 1 1 calc R . . H2S2 H 0.4897 0.2634 0.8267 0.299 Uiso 1 1 calc R . . H2S3 H 0.5807 0.2782 0.7548 0.299 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0388(3) 0.0258(3) 0.0292(3) -0.0037(2) -0.0020(2) 0.0032(3) N1 0.041(2) 0.0254(19) 0.038(2) 0.0004(15) -0.0017(17) 0.0007(16) N2 0.035(2) 0.026(2) 0.034(2) -0.0053(15) 0.0002(16) 0.0002(16) N3 0.035(2) 0.029(2) 0.033(2) -0.0055(15) -0.0003(16) -0.0002(16) N4 0.053(2) 0.0224(19) 0.032(2) -0.0012(15) 0.0064(18) 0.0055(17) C1 0.106(5) 0.117(6) 0.055(4) -0.021(4) -0.020(4) -0.003(5) C2 0.066(4) 0.062(4) 0.048(4) -0.010(3) -0.008(3) -0.009(3) C3 0.059(4) 0.110(5) 0.069(5) -0.026(4) -0.027(3) 0.027(4) C4 0.054(3) 0.093(4) 0.065(4) -0.027(3) -0.014(3) 0.025(3) C5 0.038(3) 0.031(2) 0.040(3) 0.000(2) -0.004(2) -0.002(2) C6 0.043(3) 0.073(4) 0.051(4) -0.014(3) -0.004(3) 0.010(3) C7 0.056(3) 0.080(4) 0.059(4) -0.027(3) 0.007(3) 0.003(3) S1 0.0432(7) 0.0351(7) 0.0372(7) -0.0004(5) -0.0015(5) -0.0008(5) O1 0.062(2) 0.0342(18) 0.054(2) 0.0113(15) -0.0053(17) -0.0044(16) O2 0.053(2) 0.056(2) 0.049(2) -0.0071(16) 0.0095(17) -0.0027(17) C8 0.037(3) 0.031(2) 0.037(3) -0.0028(19) 0.004(2) 0.000(2) C9 0.047(3) 0.037(3) 0.041(3) -0.004(2) 0.000(2) 0.003(2) C10 0.057(3) 0.043(3) 0.045(3) 0.012(2) 0.001(3) 0.009(2) C11 0.064(3) 0.031(3) 0.062(4) 0.007(2) 0.010(3) 0.012(2) C12 0.053(3) 0.031(3) 0.054(3) -0.006(2) 0.006(3) -0.001(2) C13 0.042(3) 0.029(2) 0.037(3) -0.0011(19) 0.007(2) 0.002(2) C14 0.043(3) 0.030(3) 0.038(3) -0.012(2) 0.004(2) -0.003(2) C15 0.040(2) 0.035(2) 0.028(3) -0.0039(19) -0.0002(19) -0.003(2) C16 0.050(3) 0.039(3) 0.036(3) -0.011(2) 0.005(2) 0.000(2) C17 0.065(3) 0.055(3) 0.038(3) -0.012(2) 0.002(3) -0.002(3) C18 0.058(3) 0.061(3) 0.045(3) -0.007(3) -0.010(3) -0.002(3) C19 0.051(3) 0.052(3) 0.041(3) -0.006(2) -0.007(2) 0.005(2) C20 0.037(2) 0.034(2) 0.034(3) -0.0063(19) -0.0023(19) -0.001(2) C21 0.044(3) 0.034(3) 0.034(3) 0.000(2) -0.001(2) 0.006(2) C22 0.043(3) 0.023(2) 0.039(3) -0.0009(19) 0.005(2) 0.003(2) C23 0.061(3) 0.032(3) 0.041(3) 0.003(2) 0.008(2) 0.009(2) C24 0.073(4) 0.023(2) 0.053(3) -0.002(2) 0.015(3) 0.002(2) C25 0.069(3) 0.026(3) 0.049(3) -0.014(2) 0.012(3) -0.005(2) C26 0.061(3) 0.038(3) 0.028(3) -0.008(2) 0.001(2) 0.006(2) C27 0.040(2) 0.022(2) 0.035(3) -0.0038(18) 0.007(2) 0.0013(19) S2 0.0539(7) 0.0308(6) 0.0278(7) 0.0010(5) 0.0000(5) 0.0017(6) O3 0.082(2) 0.0263(18) 0.050(2) 0.0076(14) 0.0123(19) 0.0006(17) O4 0.067(2) 0.057(2) 0.0269(19) -0.0010(15) -0.0015(16) 0.0047(17) C28 0.046(3) 0.040(3) 0.046(3) 0.005(2) 0.009(2) -0.005(2) C29 0.061(4) 0.073(4) 0.050(4) -0.001(3) -0.004(3) -0.014(3) C30 0.051(4) 0.087(5) 0.084(5) 0.014(4) -0.004(3) -0.013(4) C31 0.040(3) 0.081(5) 0.126(6) 0.037(4) 0.013(4) -0.006(3) C32 0.067(4) 0.053(4) 0.136(7) -0.001(4) 0.033(4) 0.006(3) C33 0.058(3) 0.049(3) 0.072(4) -0.006(3) 0.012(3) -0.001(3) C34 0.050(4) 0.104(6) 0.241(11) 0.041(6) 0.018(5) 0.008(4) N1S 0.138(7) 0.212(10) 0.122(8) -0.034(7) 0.009(6) -0.022(6) C1S 0.124(8) 0.148(8) 0.104(8) -0.005(6) 0.037(7) -0.031(6) C2S 0.250(14) 0.220(11) 0.157(11) -0.084(9) 0.105(10) -0.156(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 Ni1 N3 1.871(3) . ? Ni1 N2 1.883(3) . ? Ni1 N4 1.919(3) . ? Ni1 N1 1.925(3) . ? N1 C8 1.422(5) . ? N1 S1 1.611(3) . ? N2 C14 1.281(5) . ? N2 C15 1.477(5) . ? N3 C21 1.287(5) . ? N3 C20 1.476(5) . ? N4 C27 1.423(5) . ? N4 S2 1.613(4) . ? C1 C2 1.521(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.354(8) . ? C2 C7 1.367(7) . ? C3 C4 1.390(8) . ? C3 H3A 0.9300 . ? C4 C5 1.352(7) . ? C4 H4A 0.9300 . ? C5 C6 1.373(6) . ? C5 S1 1.788(5) . ? C6 C7 1.379(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? S1 O1 1.443(3) . ? S1 O2 1.451(3) . ? C8 C9 1.395(6) . ? C8 C13 1.401(6) . ? C9 C10 1.378(6) . ? C9 H9A 0.9300 . ? C10 C11 1.389(7) . ? C10 H10A 0.9300 . ? C11 C12 1.365(7) . ? C11 H11A 0.9300 . ? C12 C13 1.409(6) . ? C12 H12A 0.9300 . ? C13 C14 1.445(6) . ? C14 H14A 0.9300 . ? C15 C16 1.515(6) . ? C15 C20 1.524(6) . ? C15 H15A 0.9800 . ? C16 C17 1.512(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.522(7) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.526(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.515(6) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9800 . ? C21 C22 1.453(6) . ? C21 H21A 0.9300 . ? C22 C23 1.395(6) . ? C22 C27 1.397(6) . ? C23 C24 1.372(6) . ? C23 H23A 0.9300 . ? C24 C25 1.369(7) . ? C24 H24A 0.9300 . ? C25 C26 1.382(6) . ? C25 H25A 0.9300 . ? C26 C27 1.391(6) . ? C26 H26A 0.9300 . ? S2 O3 1.434(3) . ? S2 O4 1.440(3) . ? S2 C28 1.779(5) . ? C28 C33 1.381(7) . ? C28 C29 1.383(7) . ? C29 C30 1.377(8) . ? C29 H29A 0.9300 . ? C30 C31 1.382(9) . ? C30 H30A 0.9300 . ? C31 C32 1.390(9) . ? C31 C34 1.531(8) . ? C32 C33 1.388(7) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N1S C1S 1.138(11) . ? C1S C2S 1.479(12) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? 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 N3 Ni1 N2 85.84(14) . . ? N3 Ni1 N4 89.83(14) . . ? N2 Ni1 N4 167.53(15) . . ? N3 Ni1 N1 167.88(15) . . ? N2 Ni1 N1 91.13(14) . . ? N4 Ni1 N1 95.42(15) . . ? C8 N1 S1 117.1(3) . . ? C8 N1 Ni1 122.5(3) . . ? S1 N1 Ni1 115.75(18) . . ? C14 N2 C15 121.7(3) . . ? C14 N2 Ni1 125.2(3) . . ? C15 N2 Ni1 112.8(2) . . ? C21 N3 C20 121.4(4) . . ? C21 N3 Ni1 124.8(3) . . ? C20 N3 Ni1 113.4(3) . . ? C27 N4 S2 117.8(3) . . ? C27 N4 Ni1 121.2(3) . . ? S2 N4 Ni1 115.03(18) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 C7 116.7(5) . . ? C3 C2 C1 122.8(6) . . ? C7 C2 C1 120.4(6) . . ? C2 C3 C4 122.9(5) . . ? C2 C3 H3A 118.6 . . ? C4 C3 H3A 118.6 . . ? C5 C4 C3 119.2(5) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 119.5(5) . . ? C4 C5 S1 121.7(4) . . ? C6 C5 S1 118.8(3) . . ? C5 C6 C7 119.8(5) . . ? C5 C6 H6A 120.1 . . ? C7 C6 H6A 120.1 . . ? C2 C7 C6 122.0(5) . . ? C2 C7 H7A 119.0 . . ? C6 C7 H7A 119.0 . . ? O1 S1 O2 117.7(2) . . ? O1 S1 N1 105.91(18) . . ? O2 S1 N1 111.65(18) . . ? O1 S1 C5 106.2(2) . . ? O2 S1 C5 105.6(2) . . ? N1 S1 C5 109.6(2) . . ? C9 C8 C13 118.7(4) . . ? C9 C8 N1 122.0(4) . . ? C13 C8 N1 119.3(4) . . ? C10 C9 C8 121.2(4) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C9 C10 C11 120.2(5) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C12 C11 C10 119.7(4) . . ? C12 C11 H11A 120.2 . . ? C10 C11 H11A 120.2 . . ? C11 C12 C13 121.1(4) . . ? C11 C12 H12A 119.5 . . ? C13 C12 H12A 119.5 . . ? C8 C13 C12 119.2(4) . . ? C8 C13 C14 123.2(4) . . ? C12 C13 C14 117.6(4) . . ? N2 C14 C13 126.2(4) . . ? N2 C14 H14A 116.9 . . ? C13 C14 H14A 116.9 . . ? N2 C15 C16 117.8(4) . . ? N2 C15 C20 106.8(3) . . ? C16 C15 C20 110.1(4) . . ? N2 C15 H15A 107.2 . . ? C16 C15 H15A 107.2 . . ? C20 C15 H15A 107.2 . . ? C17 C16 C15 109.9(4) . . ? C17 C16 H16A 109.7 . . ? C15 C16 H16A 109.7 . . ? C17 C16 H16B 109.7 . . ? C15 C16 H16B 109.7 . . ? H16A C16 H16B 108.2 . . ? C16 C17 C18 111.9(4) . . ? C16 C17 H17A 109.2 . . ? C18 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? C18 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C17 C18 C19 112.1(4) . . ? C17 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 110.2(4) . . ? C20 C19 H19A 109.6 . . ? C18 C19 H19A 109.6 . . ? C20 C19 H19B 109.6 . . ? C18 C19 H19B 109.6 . . ? H19A C19 H19B 108.1 . . ? N3 C20 C19 118.2(4) . . ? N3 C20 C15 105.9(3) . . ? C19 C20 C15 109.9(4) . . ? N3 C20 H20A 107.5 . . ? C19 C20 H20A 107.5 . . ? C15 C20 H20A 107.5 . . ? N3 C21 C22 125.4(4) . . ? N3 C21 H21A 117.3 . . ? C22 C21 H21A 117.3 . . ? C23 C22 C27 119.9(4) . . ? C23 C22 C21 117.7(4) . . ? C27 C22 C21 122.2(4) . . ? C24 C23 C22 120.3(5) . . ? C24 C23 H23A 119.8 . . ? C22 C23 H23A 119.8 . . ? C25 C24 C23 119.8(4) . . ? C25 C24 H24A 120.1 . . ? C23 C24 H24A 120.1 . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C27 120.2(4) . . ? C25 C26 H26A 119.9 . . ? C27 C26 H26A 119.9 . . ? C26 C27 C22 118.7(4) . . ? C26 C27 N4 122.5(4) . . ? C22 C27 N4 118.8(3) . . ? O3 S2 O4 116.08(19) . . ? O3 S2 N4 106.17(19) . . ? O4 S2 N4 112.4(2) . . ? O3 S2 C28 108.8(2) . . ? O4 S2 C28 105.2(2) . . ? N4 S2 C28 107.9(2) . . ? C33 C28 C29 119.9(5) . . ? C33 C28 S2 120.0(4) . . ? C29 C28 S2 120.1(4) . . ? C30 C29 C28 120.2(6) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C31 121.1(6) . . ? C29 C30 H30A 119.5 . . ? C31 C30 H30A 119.5 . . ? C30 C31 C32 118.2(5) . . ? C30 C31 C34 122.2(7) . . ? C32 C31 C34 119.6(7) . . ? C33 C32 C31 121.3(6) . . ? C33 C32 H32A 119.4 . . ? C31 C32 H32A 119.4 . . ? C28 C33 C32 119.3(5) . . ? C28 C33 H33A 120.4 . . ? C32 C33 H33A 120.4 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1S C1S C2S 176.8(14) . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 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 N3 Ni1 N1 C8 113.7(7) . . . . ? N2 Ni1 N1 C8 38.3(3) . . . . ? N4 Ni1 N1 C8 -131.0(3) . . . . ? N3 Ni1 N1 S1 -41.5(8) . . . . ? N2 Ni1 N1 S1 -116.8(2) . . . . ? N4 Ni1 N1 S1 73.8(2) . . . . ? N3 Ni1 N2 C14 163.2(4) . . . . ? N4 Ni1 N2 C14 93.2(7) . . . . ? N1 Ni1 N2 C14 -28.6(4) . . . . ? N3 Ni1 N2 C15 -11.1(3) . . . . ? N4 Ni1 N2 C15 -81.1(7) . . . . ? N1 Ni1 N2 C15 157.1(3) . . . . ? N2 Ni1 N3 C21 158.3(4) . . . . ? N4 Ni1 N3 C21 -33.4(4) . . . . ? N1 Ni1 N3 C21 82.5(8) . . . . ? N2 Ni1 N3 C20 -14.0(3) . . . . ? N4 Ni1 N3 C20 154.3(3) . . . . ? N1 Ni1 N3 C20 -89.9(7) . . . . ? N3 Ni1 N4 C27 45.1(3) . . . . ? N2 Ni1 N4 C27 114.7(7) . . . . ? N1 Ni1 N4 C27 -124.0(3) . . . . ? N3 Ni1 N4 S2 -107.0(2) . . . . ? N2 Ni1 N4 S2 -37.5(8) . . . . ? N1 Ni1 N4 S2 83.9(2) . . . . ? C7 C2 C3 C4 -1.0(10) . . . . ? C1 C2 C3 C4 -178.6(6) . . . . ? C2 C3 C4 C5 1.8(11) . . . . ? C3 C4 C5 C6 -2.5(9) . . . . ? C3 C4 C5 S1 -179.4(5) . . . . ? C4 C5 C6 C7 2.5(8) . . . . ? S1 C5 C6 C7 179.6(4) . . . . ? C3 C2 C7 C6 1.0(9) . . . . ? C1 C2 C7 C6 178.6(6) . . . . ? C5 C6 C7 C2 -1.8(9) . . . . ? C8 N1 S1 O1 -161.5(3) . . . . ? Ni1 N1 S1 O1 -4.9(3) . . . . ? C8 N1 S1 O2 -32.2(4) . . . . ? Ni1 N1 S1 O2 124.3(2) . . . . ? C8 N1 S1 C5 84.4(3) . . . . ? Ni1 N1 S1 C5 -119.1(2) . . . . ? C4 C5 S1 O1 126.4(4) . . . . ? C6 C5 S1 O1 -50.5(4) . . . . ? C4 C5 S1 O2 0.8(5) . . . . ? C6 C5 S1 O2 -176.2(4) . . . . ? C4 C5 S1 N1 -119.6(4) . . . . ? C6 C5 S1 N1 63.4(4) . . . . ? S1 N1 C8 C9 -54.8(5) . . . . ? Ni1 N1 C8 C9 150.4(3) . . . . ? S1 N1 C8 C13 125.2(4) . . . . ? Ni1 N1 C8 C13 -29.7(5) . . . . ? C13 C8 C9 C10 -0.1(7) . . . . ? N1 C8 C9 C10 179.8(4) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C9 C10 C11 C12 0.7(8) . . . . ? C10 C11 C12 C13 0.0(8) . . . . ? C9 C8 C13 C12 0.7(7) . . . . ? N1 C8 C13 C12 -179.2(4) . . . . ? C9 C8 C13 C14 179.6(4) . . . . ? N1 C8 C13 C14 -0.3(7) . . . . ? C11 C12 C13 C8 -0.7(7) . . . . ? C11 C12 C13 C14 -179.6(4) . . . . ? C15 N2 C14 C13 -176.7(4) . . . . ? Ni1 N2 C14 C13 9.5(6) . . . . ? C8 C13 C14 N2 11.7(7) . . . . ? C12 C13 C14 N2 -169.4(4) . . . . ? C14 N2 C15 C16 -18.0(6) . . . . ? Ni1 N2 C15 C16 156.5(3) . . . . ? C14 N2 C15 C20 -142.4(4) . . . . ? Ni1 N2 C15 C20 32.2(4) . . . . ? N2 C15 C16 C17 177.7(4) . . . . ? C20 C15 C16 C17 -59.5(5) . . . . ? C15 C16 C17 C18 55.4(5) . . . . ? C16 C17 C18 C19 -53.0(6) . . . . ? C17 C18 C19 C20 53.8(6) . . . . ? C21 N3 C20 C19 -14.7(6) . . . . ? Ni1 N3 C20 C19 157.9(3) . . . . ? C21 N3 C20 C15 -138.4(4) . . . . ? Ni1 N3 C20 C15 34.2(4) . . . . ? C18 C19 C20 N3 -179.4(4) . . . . ? C18 C19 C20 C15 -57.7(5) . . . . ? N2 C15 C20 N3 -41.0(4) . . . . ? C16 C15 C20 N3 -169.9(4) . . . . ? N2 C15 C20 C19 -169.7(4) . . . . ? C16 C15 C20 C19 61.3(5) . . . . ? C20 N3 C21 C22 -178.7(4) . . . . ? Ni1 N3 C21 C22 9.6(7) . . . . ? N3 C21 C22 C23 -166.6(4) . . . . ? N3 C21 C22 C27 16.6(7) . . . . ? C27 C22 C23 C24 -1.9(7) . . . . ? C21 C22 C23 C24 -178.8(4) . . . . ? C22 C23 C24 C25 1.4(8) . . . . ? C23 C24 C25 C26 0.1(8) . . . . ? C24 C25 C26 C27 -1.0(8) . . . . ? C25 C26 C27 C22 0.5(7) . . . . ? C25 C26 C27 N4 -179.1(4) . . . . ? C23 C22 C27 C26 0.9(7) . . . . ? C21 C22 C27 C26 177.7(4) . . . . ? C23 C22 C27 N4 -179.5(4) . . . . ? C21 C22 C27 N4 -2.7(6) . . . . ? S2 N4 C27 C26 -62.7(5) . . . . ? Ni1 N4 C27 C26 145.9(4) . . . . ? S2 N4 C27 C22 117.7(4) . . . . ? Ni1 N4 C27 C22 -33.7(5) . . . . ? C27 N4 S2 O3 -162.2(3) . . . . ? Ni1 N4 S2 O3 -9.1(3) . . . . ? C27 N4 S2 O4 69.8(4) . . . . ? Ni1 N4 S2 O4 -137.0(2) . . . . ? C27 N4 S2 C28 -45.8(4) . . . . ? Ni1 N4 S2 C28 107.4(2) . . . . ? O3 S2 C28 C33 -149.0(4) . . . . ? O4 S2 C28 C33 -24.0(4) . . . . ? N4 S2 C28 C33 96.3(4) . . . . ? O3 S2 C28 C29 32.8(5) . . . . ? O4 S2 C28 C29 157.9(4) . . . . ? N4 S2 C28 C29 -81.9(4) . . . . ? C33 C28 C29 C30 -0.2(8) . . . . ? S2 C28 C29 C30 178.0(4) . . . . ? C28 C29 C30 C31 -1.4(9) . . . . ? C29 C30 C31 C32 2.3(10) . . . . ? C29 C30 C31 C34 -178.4(6) . . . . ? C30 C31 C32 C33 -1.7(10) . . . . ? C34 C31 C32 C33 179.0(6) . . . . ? C29 C28 C33 C32 0.8(8) . . . . ? S2 C28 C33 C32 -177.4(4) . . . . ? C31 C32 C33 C28 0.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.11 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.445 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.157 data_cucyts _database_code_CSD 168561 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 Cu N4 O4 S2, C2 H3 N' _chemical_formula_sum 'C36 H37 Cu N5 O4 S2' _chemical_formula_weight 731.37 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 '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 12.6852(2) _cell_length_b 28.7169(3) _cell_length_c 10.2814(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.6670(10) _cell_angle_gamma 90.00 _cell_volume 3587.96(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'Prism' _exptl_crystal_colour 'Dark green' _exptl_crystal_size_max 0.85 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1524 _exptl_absorpt_coefficient_mu 0.770 _exptl_absorpt_correction_type 'Sadabs' _exptl_absorpt_correction_T_min 0.676777 _exptl_absorpt_correction_T_max 0.842770 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 'Siemens CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15058 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 25.03 _reflns_number_total 6325 _reflns_number_gt 4663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'Siemens SMART' _computing_data_reduction 'Siemens SAINT' _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^)+(0.0709P)^2^+1.4080P] 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 6325 _refine_ls_number_parameters 480 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0771 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1456 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.139 _refine_ls_restrained_S_all 1.139 _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 Cu1 Cu 0.52763(4) 0.145284(13) 0.38604(4) 0.04601(16) Uani 1 1 d . A . N1 N 0.5616(3) 0.09778(9) 0.2673(3) 0.0504(8) Uani 1 1 d . . . N2 N 0.6299(3) 0.11402(11) 0.5414(3) 0.0663(10) Uani 1 1 d . . . N3 N 0.5513(3) 0.19869(11) 0.5084(3) 0.0622(9) Uani 1 1 d . . . N4 N 0.3881(3) 0.17212(10) 0.2754(3) 0.0499(8) Uani 1 1 d . . . C1 C 1.0690(5) 0.0393(3) 0.2624(10) 0.168(4) Uani 1 1 d . . . H1A H 1.0832 0.0199 0.3415 0.252 Uiso 1 1 calc R . . H1B H 1.1216 0.0642 0.2787 0.252 Uiso 1 1 calc R . . H1C H 1.0752 0.0211 0.1865 0.252 Uiso 1 1 calc R . . C2 C 0.9532(5) 0.0594(2) 0.2312(8) 0.102(2) Uani 1 1 d . . . C3 C 0.9317(5) 0.0987(2) 0.2993(6) 0.0982(18) Uani 1 1 d . . . H3A H 0.9894 0.1133 0.3632 0.118 Uiso 1 1 calc R . . C4 C 0.8278(4) 0.11620(18) 0.2738(5) 0.0767(13) Uani 1 1 d . . . H4A H 0.8148 0.1422 0.3209 0.092 Uiso 1 1 calc R . . C5 C 0.7416(3) 0.09504(14) 0.1775(4) 0.0555(10) Uani 1 1 d . . . C6 C 0.7613(4) 0.05714(15) 0.1059(5) 0.0729(13) Uani 1 1 d . . . H6A H 0.7043 0.0434 0.0390 0.088 Uiso 1 1 calc R . . C7 C 0.8683(5) 0.03954(19) 0.1353(7) 0.0978(18) Uani 1 1 d . . . H7A H 0.8818 0.0136 0.0882 0.117 Uiso 1 1 calc R . . S1 S 0.60613(9) 0.11664(3) 0.14719(9) 0.0497(3) Uani 1 1 d . . . O1 O 0.6119(3) 0.16666(9) 0.1638(3) 0.0658(8) Uani 1 1 d . . . O2 O 0.5460(2) 0.09988(10) 0.0148(3) 0.0646(8) Uani 1 1 d . . . C8 C 0.5704(3) 0.05006(11) 0.3023(4) 0.0442(8) Uani 1 1 d . A . C9 C 0.5356(4) 0.01431(13) 0.2078(4) 0.0582(10) Uani 1 1 d . . . H9A H 0.5048 0.0218 0.1168 0.070 Uiso 1 1 calc R . . C10 C 0.5460(4) -0.03182(13) 0.2466(5) 0.0637(11) Uani 1 1 d . . . H10A H 0.5210 -0.0550 0.1817 0.076 Uiso 1 1 calc R . . C11 C 0.5929(4) -0.04402(13) 0.3801(4) 0.0613(11) Uani 1 1 d . . . H11A H 0.6009 -0.0752 0.4056 0.074 Uiso 1 1 calc R . . C12 C 0.6274(4) -0.00979(12) 0.4745(4) 0.0561(10) Uani 1 1 d . A . H12A H 0.6591 -0.0180 0.5647 0.067 Uiso 1 1 calc R . . C13 C 0.6163(3) 0.03751(12) 0.4395(4) 0.0481(9) Uani 1 1 d . . . C14 C 0.6532(4) 0.07048(13) 0.5478(4) 0.0652(12) Uani 1 1 d . A . H14A H 0.6979 0.0593 0.6300 0.078 Uiso 1 1 calc R . . C16 C 0.7489(5) 0.12825(17) 0.7847(5) 0.0791(14) Uani 1 1 d . . . H16A H 0.8020 0.1043 0.7809 0.095 Uiso 0.527(15) 1 calc PR A 1 H16B H 0.6915 0.1142 0.8169 0.095 Uiso 0.527(15) 1 calc PR A 1 H16C H 0.7427 0.0968 0.8162 0.095 Uiso 0.473(15) 1 calc PR A 2 H16D H 0.8121 0.1297 0.7495 0.095 Uiso 0.473(15) 1 calc PR A 2 C19 C 0.6734(5) 0.22503(16) 0.7437(5) 0.0848(16) Uani 1 1 d . . . H19A H 0.6246 0.2507 0.7471 0.102 Uiso 0.527(15) 1 calc PR A 1 H19B H 0.7299 0.2360 0.7047 0.102 Uiso 0.527(15) 1 calc PR A 1 H19C H 0.6747 0.2574 0.7170 0.102 Uiso 0.473(15) 1 calc PR A 2 H19D H 0.6145 0.2207 0.7855 0.102 Uiso 0.473(15) 1 calc PR A 2 C15 C 0.6993(9) 0.1493(4) 0.6437(10) 0.051(2) Uani 0.527(15) 1 d P A 1 H15 H 0.7550 0.1645 0.6092 0.061 Uiso 0.527(15) 1 calc PR A 1 C17 C 0.8055(12) 0.1675(6) 0.8811(16) 0.065(4) Uani 0.527(15) 1 d P A 1 H17A H 0.8387 0.1547 0.9708 0.078 Uiso 0.527(15) 1 calc PR A 1 H17B H 0.8637 0.1808 0.8490 0.078 Uiso 0.527(15) 1 calc PR A 1 C18 C 0.7264(11) 0.2046(4) 0.8898(10) 0.065(3) Uani 0.527(15) 1 d P A 1 H18A H 0.7642 0.2290 0.9505 0.078 Uiso 0.527(15) 1 calc PR A 1 H18B H 0.6695 0.1918 0.9255 0.078 Uiso 0.527(15) 1 calc PR A 1 C20 C 0.6086(8) 0.1845(3) 0.6596(9) 0.048(2) Uani 0.527(15) 1 d P A 1 H20 H 0.5571 0.1701 0.7029 0.057 Uiso 0.527(15) 1 calc PR A 1 C15' C 0.6392(17) 0.1425(3) 0.6693(11) 0.073(5) Uani 0.473(15) 1 d P A 2 H15' H 0.5730 0.1408 0.7001 0.088 Uiso 0.473(15) 1 calc PR A 2 C17' C 0.761(2) 0.1622(10) 0.898(2) 0.117(9) Uani 0.473(15) 1 d P A 2 H17C H 0.8221 0.1534 0.9756 0.140 Uiso 0.473(15) 1 calc PR A 2 H17D H 0.6947 0.1637 0.9258 0.140 Uiso 0.473(15) 1 calc PR A 2 C18' C 0.7849(15) 0.2101(5) 0.8399(17) 0.104(6) Uani 0.473(15) 1 d P A 2 H18C H 0.8111 0.2326 0.9122 0.125 Uiso 0.473(15) 1 calc PR A 2 H18D H 0.8395 0.2068 0.7910 0.125 Uiso 0.473(15) 1 calc PR A 2 C20' C 0.6595(15) 0.1915(4) 0.6189(11) 0.066(4) Uani 0.473(15) 1 d P A 2 H20' H 0.7233 0.1923 0.5832 0.079 Uiso 0.473(15) 1 calc PR A 2 C21 C 0.5064(4) 0.23856(13) 0.4823(4) 0.0595(11) Uani 1 1 d . A . H21A H 0.5265 0.2610 0.5502 0.071 Uiso 1 1 calc R . . C22 C 0.4274(3) 0.25209(12) 0.3572(4) 0.0478(9) Uani 1 1 d . . . C23 C 0.4063(4) 0.29982(13) 0.3364(4) 0.0616(11) Uani 1 1 d . A . H23A H 0.4417 0.3207 0.4040 0.074 Uiso 1 1 calc R . . C24 C 0.3353(4) 0.31652(14) 0.2199(5) 0.0703(12) Uani 1 1 d . . . H24A H 0.3232 0.3484 0.2083 0.084 Uiso 1 1 calc R A . C25 C 0.2815(4) 0.28606(14) 0.1193(5) 0.0699(12) Uani 1 1 d . A . H25A H 0.2340 0.2974 0.0391 0.084 Uiso 1 1 calc R . . C26 C 0.2980(4) 0.23840(13) 0.1372(4) 0.0603(11) Uani 1 1 d . . . H26A H 0.2602 0.2181 0.0693 0.072 Uiso 1 1 calc R A . S2 S 0.28540(9) 0.13842(3) 0.26221(10) 0.0505(3) Uani 1 1 d . A . O3 O 0.3326(3) 0.09659(9) 0.3333(3) 0.0665(8) Uani 1 1 d . . . O4 O 0.1988(3) 0.16094(10) 0.3024(3) 0.0686(8) Uani 1 1 d . . . C27 C 0.3703(3) 0.22055(12) 0.2553(4) 0.0473(9) Uani 1 1 d . A . C28 C 0.2268(3) 0.12184(12) 0.0894(4) 0.0499(9) Uani 1 1 d . . . C29 C 0.1218(4) 0.13345(19) 0.0213(5) 0.0893(17) Uani 1 1 d . A . H29A H 0.0789 0.1508 0.0633 0.107 Uiso 1 1 calc R . . C30 C 0.0795(5) 0.1188(2) -0.1130(6) 0.104(2) Uani 1 1 d . . . H30A H 0.0076 0.1268 -0.1599 0.125 Uiso 1 1 calc R A . C31 C 0.1393(4) 0.09348(17) -0.1779(5) 0.0747(13) Uani 1 1 d . A . C32 C 0.2426(4) 0.08191(19) -0.1063(5) 0.0836(15) Uani 1 1 d . . . H32A H 0.2848 0.0640 -0.1478 0.100 Uiso 1 1 calc R A . C33 C 0.2879(4) 0.09571(17) 0.0267(4) 0.0700(12) Uani 1 1 d . A . H33A H 0.3596 0.0873 0.0733 0.084 Uiso 1 1 calc R . . C34 C 0.0917(6) 0.0784(3) -0.3265(5) 0.120(2) Uani 1 1 d . . . H34A H 0.0943 0.1041 -0.3852 0.180 Uiso 1 1 calc R A . H34B H 0.0167 0.0687 -0.3418 0.180 Uiso 1 1 calc R . . H34C H 0.1342 0.0530 -0.3456 0.180 Uiso 1 1 calc R . . N1S N 0.9525(7) 0.2031(3) 0.5590(8) 0.162(3) Uani 1 1 d . B . C1S C 0.9935(8) 0.2238(3) 0.6475(9) 0.130(3) Uani 1 1 d . . . C2S C 1.028(6) 0.258(2) 0.758(4) 0.23(2) Uani 0.61(7) 1 d P B . H2S4 H 0.9823 0.2852 0.7350 0.349 Uiso 0.61(7) 1 calc PR . . H2S5 H 1.1032 0.2664 0.7696 0.349 Uiso 0.61(7) 1 calc PR . . H2S6 H 1.0204 0.2446 0.8402 0.349 Uiso 0.61(7) 1 calc PR . . C2S' C 1.074(3) 0.2384(14) 0.783(2) 0.103(11) Uani 0.39(7) 1 d P B 3 H2S1 H 1.0422 0.2322 0.8552 0.154 Uiso 0.39(7) 1 calc PR B 3 H2S2 H 1.0895 0.2711 0.7806 0.154 Uiso 0.39(7) 1 calc PR B 3 H2S3 H 1.1413 0.2211 0.7977 0.154 Uiso 0.39(7) 1 calc PR B 3 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 0.0582(3) 0.0334(2) 0.0390(3) -0.00422(18) 0.0022(2) 0.0032(2) N1 0.073(2) 0.0331(14) 0.0441(17) -0.0013(13) 0.0144(16) 0.0055(15) N2 0.095(3) 0.0403(17) 0.0460(19) -0.0046(15) -0.0085(18) 0.0071(17) N3 0.079(2) 0.0391(17) 0.0509(19) -0.0128(14) -0.0101(17) 0.0084(16) N4 0.0564(19) 0.0348(15) 0.0483(17) -0.0024(13) -0.0014(14) 0.0009(14) C1 0.072(4) 0.138(6) 0.296(12) 0.077(7) 0.057(6) 0.020(4) C2 0.059(3) 0.096(4) 0.151(6) 0.050(4) 0.028(4) 0.002(3) C3 0.067(4) 0.115(5) 0.095(4) 0.023(4) -0.006(3) -0.024(3) C4 0.073(3) 0.086(3) 0.061(3) -0.001(2) 0.003(2) -0.016(3) C5 0.063(3) 0.053(2) 0.047(2) 0.0109(18) 0.0101(19) -0.003(2) C6 0.069(3) 0.058(3) 0.090(3) -0.004(2) 0.019(3) -0.001(2) C7 0.080(4) 0.067(3) 0.157(6) 0.008(3) 0.050(4) 0.009(3) S1 0.0656(6) 0.0414(5) 0.0368(5) 0.0038(4) 0.0065(4) 0.0036(4) O1 0.095(2) 0.0429(14) 0.0558(17) 0.0111(13) 0.0161(16) 0.0034(15) O2 0.0733(19) 0.0731(18) 0.0378(14) -0.0019(13) 0.0004(13) 0.0038(15) C8 0.051(2) 0.0358(17) 0.045(2) -0.0026(15) 0.0139(17) 0.0051(16) C9 0.075(3) 0.050(2) 0.047(2) -0.0046(17) 0.013(2) 0.005(2) C10 0.083(3) 0.040(2) 0.069(3) -0.013(2) 0.022(2) 0.000(2) C11 0.080(3) 0.0355(19) 0.071(3) 0.0021(19) 0.025(2) 0.0026(19) C12 0.072(3) 0.0401(19) 0.054(2) 0.0073(17) 0.014(2) 0.0075(19) C13 0.053(2) 0.0363(18) 0.052(2) 0.0023(16) 0.0098(18) 0.0057(16) C14 0.086(3) 0.043(2) 0.051(2) 0.0018(18) -0.005(2) 0.009(2) C16 0.100(4) 0.065(3) 0.056(3) 0.003(2) -0.005(3) 0.010(3) C19 0.100(4) 0.055(3) 0.078(3) -0.012(2) -0.009(3) 0.009(3) C15 0.056(6) 0.041(5) 0.050(5) -0.001(4) 0.006(4) -0.003(4) C17 0.076(8) 0.053(7) 0.053(7) 0.013(5) -0.004(6) 0.001(7) C18 0.073(7) 0.060(6) 0.052(5) -0.001(4) 0.001(5) -0.004(5) C20 0.044(5) 0.068(6) 0.032(4) -0.005(4) 0.012(3) -0.008(4) C15' 0.117(13) 0.033(5) 0.047(6) 0.010(4) -0.013(7) -0.016(7) C17' 0.17(2) 0.116(15) 0.067(9) -0.001(8) 0.034(13) -0.058(15) C18' 0.091(11) 0.114(12) 0.086(10) 0.001(8) -0.011(8) -0.051(9) C20' 0.097(10) 0.048(6) 0.035(5) -0.002(4) -0.012(6) 0.019(6) C21 0.073(3) 0.042(2) 0.054(2) -0.0178(18) 0.003(2) 0.000(2) C22 0.056(2) 0.0365(18) 0.052(2) -0.0052(16) 0.0159(18) -0.0016(16) C23 0.075(3) 0.038(2) 0.070(3) -0.0048(19) 0.018(2) 0.001(2) C24 0.089(3) 0.038(2) 0.082(3) 0.009(2) 0.020(3) 0.010(2) C25 0.085(3) 0.052(2) 0.065(3) 0.017(2) 0.008(2) 0.010(2) C26 0.074(3) 0.046(2) 0.053(2) 0.0024(18) 0.005(2) 0.002(2) S2 0.0599(6) 0.0398(5) 0.0463(5) -0.0012(4) 0.0066(4) -0.0015(4) O3 0.084(2) 0.0438(14) 0.0591(17) 0.0111(13) 0.0006(15) -0.0032(14) O4 0.074(2) 0.0685(18) 0.0661(18) -0.0096(15) 0.0238(16) -0.0035(16) C27 0.053(2) 0.0390(18) 0.050(2) 0.0000(16) 0.0147(18) 0.0026(17) C28 0.053(2) 0.0401(19) 0.047(2) -0.0031(16) 0.0004(18) -0.0043(17) C29 0.068(3) 0.099(4) 0.082(3) -0.031(3) -0.008(3) 0.024(3) C30 0.075(4) 0.114(5) 0.090(4) -0.016(3) -0.031(3) 0.017(3) C31 0.084(3) 0.070(3) 0.056(3) -0.008(2) -0.002(3) -0.014(3) C32 0.078(3) 0.100(4) 0.071(3) -0.033(3) 0.018(3) -0.005(3) C33 0.051(2) 0.085(3) 0.064(3) -0.023(2) 0.003(2) -0.001(2) C34 0.139(6) 0.132(5) 0.063(3) -0.021(3) -0.011(3) -0.022(4) N1S 0.144(6) 0.194(8) 0.127(6) -0.024(6) 0.007(5) 0.000(5) C1S 0.143(7) 0.133(7) 0.119(6) -0.010(5) 0.043(6) -0.036(6) C2S 0.28(5) 0.16(3) 0.29(3) -0.06(2) 0.14(3) -0.13(3) C2S' 0.111(17) 0.13(2) 0.080(17) -0.028(11) 0.045(11) -0.062(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 Cu1 N3 1.952(3) . ? Cu1 N1 1.960(3) . ? Cu1 N2 1.963(3) . ? Cu1 N4 1.966(3) . ? N1 C8 1.413(4) . ? N1 S1 1.593(3) . ? N2 C14 1.282(5) . ? N2 C15' 1.523(14) . ? N2 C15 1.542(10) . ? N3 C21 1.273(5) . ? N3 C20' 1.524(12) . ? N3 C20 1.569(9) . ? N4 C27 1.415(4) . ? N4 S2 1.597(3) . ? C1 C2 1.526(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C7 1.359(9) . ? C2 C3 1.395(9) . ? C3 C4 1.364(8) . ? C3 H3A 0.9300 . ? C4 C5 1.388(6) . ? C4 H4A 0.9300 . ? C5 C6 1.376(6) . ? C5 S1 1.768(4) . ? C6 C7 1.399(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? S1 O2 1.439(3) . ? S1 O1 1.446(3) . ? C8 C9 1.395(5) . ? C8 C13 1.409(5) . ? C9 C10 1.379(5) . ? C9 H9A 0.9300 . ? C10 C11 1.376(6) . ? C10 H10A 0.9300 . ? C11 C12 1.362(5) . ? C11 H11A 0.9300 . ? C12 C13 1.402(5) . ? C12 H12A 0.9300 . ? C13 C14 1.434(5) . ? C14 H14A 0.9300 . ? C16 C17' 1.49(3) . ? C16 C15 1.529(11) . ? C16 C17 1.536(19) . ? C16 C15' 1.601(15) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 H16C 0.9700 . ? C16 H16D 0.9700 . ? C19 C18' 1.537(15) . ? C19 C20 1.540(10) . ? C19 C18 1.573(11) . ? C19 C20' 1.574(11) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 H19C 0.9700 . ? C19 H19D 0.9700 . ? C15 C20 1.575(15) . ? C15 H15 0.9800 . ? C17 C18 1.48(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C20 H20 0.9800 . ? C15' C20' 1.55(2) . ? C15' H15' 0.9800 . ? C17' C18' 1.56(3) . ? C17' H17C 0.9700 . ? C17' H17D 0.9700 . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C20' H20' 0.9800 . ? C21 C22 1.439(5) . ? C21 H21A 0.9300 . ? C22 C23 1.401(5) . ? C22 C27 1.417(5) . ? C23 C24 1.363(6) . ? C23 H23A 0.9300 . ? C24 C25 1.376(6) . ? C24 H24A 0.9300 . ? C25 C26 1.389(5) . ? C25 H25A 0.9300 . ? C26 C27 1.393(5) . ? C26 H26A 0.9300 . ? S2 O4 1.434(3) . ? S2 O3 1.444(3) . ? S2 C28 1.783(4) . ? C28 C29 1.356(6) . ? C28 C33 1.366(6) . ? C29 C30 1.395(7) . ? C29 H29A 0.9300 . ? C30 C31 1.357(7) . ? C30 H30A 0.9300 . ? C31 C32 1.348(7) . ? C31 C34 1.536(6) . ? C32 C33 1.380(6) . ? C32 H32A 0.9300 . ? C33 H33A 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? N1S C1S 1.087(9) . ? C1S C2S 1.47(3) . ? C1S C2S' 1.53(3) . ? C2S H2S4 0.9600 . ? C2S H2S5 0.9600 . ? C2S H2S6 0.9600 . ? C2S' H2S1 0.9600 . ? C2S' H2S2 0.9600 . ? C2S' H2S3 0.9600 . ? 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 N3 Cu1 N1 158.16(15) . . ? N3 Cu1 N2 83.74(13) . . ? N1 Cu1 N2 88.67(13) . . ? N3 Cu1 N4 90.66(13) . . ? N1 Cu1 N4 103.57(13) . . ? N2 Cu1 N4 157.72(16) . . ? C8 N1 S1 120.5(2) . . ? C8 N1 Cu1 122.1(2) . . ? S1 N1 Cu1 115.88(16) . . ? C14 N2 C15' 121.3(5) . . ? C14 N2 C15 121.9(5) . . ? C15' N2 C15 34.0(6) . . ? C14 N2 Cu1 125.2(3) . . ? C15' N2 Cu1 109.1(5) . . ? C15 N2 Cu1 111.7(4) . . ? C21 N3 C20' 122.2(5) . . ? C21 N3 C20 119.7(4) . . ? C20' N3 C20 33.3(6) . . ? C21 N3 Cu1 126.5(3) . . ? C20' N3 Cu1 108.2(4) . . ? C20 N3 Cu1 112.1(4) . . ? C27 N4 S2 119.4(3) . . ? C27 N4 Cu1 123.3(2) . . ? S2 N4 Cu1 112.87(16) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C7 C2 C3 118.4(5) . . ? C7 C2 C1 120.5(7) . . ? C3 C2 C1 121.1(7) . . ? C4 C3 C2 121.2(5) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 119.8(5) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 S1 120.0(3) . . ? C4 C5 S1 120.0(4) . . ? C5 C6 C7 119.0(5) . . ? C5 C6 H6A 120.5 . . ? C7 C6 H6A 120.5 . . ? C2 C7 C6 121.5(6) . . ? C2 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? O2 S1 O1 116.05(17) . . ? O2 S1 N1 114.18(17) . . ? O1 S1 N1 105.27(16) . . ? O2 S1 C5 105.90(18) . . ? O1 S1 C5 108.32(19) . . ? N1 S1 C5 106.68(17) . . ? C9 C8 C13 117.8(3) . . ? C9 C8 N1 123.4(3) . . ? C13 C8 N1 118.9(3) . . ? C10 C9 C8 121.4(4) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10A 119.6 . . ? C9 C10 H10A 119.6 . . ? C12 C11 C10 119.1(4) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C13 121.9(4) . . ? C11 C12 H12A 119.1 . . ? C13 C12 H12A 119.1 . . ? C12 C13 C8 119.1(3) . . ? C12 C13 C14 117.0(3) . . ? C8 C13 C14 123.9(3) . . ? N2 C14 C13 125.8(4) . . ? N2 C14 H14A 117.1 . . ? C13 C14 H14A 117.1 . . ? C17' C16 C15 113.8(11) . . ? C17' C16 C17 24.7(9) . . ? C15 C16 C17 108.1(7) . . ? C17' C16 C15' 106.7(13) . . ? C15 C16 C15' 33.2(5) . . ? C17 C16 C15' 115.9(7) . . ? C17' C16 H16A 125.0 . . ? C15 C16 H16A 110.1 . . ? C17 C16 H16A 110.1 . . ? C15' C16 H16A 128.0 . . ? C17' C16 H16B 85.9 . . ? C15 C16 H16B 110.1 . . ? C17 C16 H16B 110.1 . . ? C15' C16 H16B 77.4 . . ? H16A C16 H16B 108.4 . . ? C17' C16 H16C 110.4 . . ? C15 C16 H16C 129.4 . . ? C17 C16 H16C 122.3 . . ? C15' C16 H16C 110.4 . . ? H16A C16 H16C 58.6 . . ? H16B C16 H16C 50.0 . . ? C17' C16 H16D 110.4 . . ? C15 C16 H16D 77.8 . . ? C17 C16 H16D 85.8 . . ? C15' C16 H16D 110.4 . . ? H16A C16 H16D 50.0 . . ? H16B C16 H16D 157.8 . . ? H16C C16 H16D 108.6 . . ? C18' C19 C20 113.3(7) . . ? C18' C19 C18 38.6(6) . . ? C20 C19 C18 105.5(7) . . ? C18' C19 C20' 102.7(10) . . ? C20 C19 C20' 33.1(5) . . ? C18 C19 C20' 117.8(6) . . ? C18' C19 H19A 131.9 . . ? C20 C19 H19A 110.6 . . ? C18 C19 H19A 110.6 . . ? C20' C19 H19A 124.9 . . ? C18' C19 H19B 72.8 . . ? C20 C19 H19B 110.6 . . ? C18 C19 H19B 110.6 . . ? C20' C19 H19B 77.6 . . ? H19A C19 H19B 108.8 . . ? C18' C19 H19C 111.2 . . ? C20 C19 H19C 127.9 . . ? C18 C19 H19C 126.2 . . ? C20' C19 H19C 111.2 . . ? H19A C19 H19C 49.1 . . ? H19B C19 H19C 59.7 . . ? C18' C19 H19D 111.2 . . ? C20 C19 H19D 78.3 . . ? C18 C19 H19D 72.6 . . ? C20' C19 H19D 111.2 . . ? H19A C19 H19D 60.2 . . ? H19B C19 H19D 168.4 . . ? H19C C19 H19D 109.1 . . ? C16 C15 N2 112.7(8) . . ? C16 C15 C20 105.6(8) . . ? N2 C15 C20 101.6(7) . . ? C16 C15 H15 112.1 . . ? N2 C15 H15 112.1 . . ? C20 C15 H15 112.1 . . ? C18 C17 C16 111.5(11) . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C19 108.8(10) . . ? C17 C18 H18A 109.9 . . ? C19 C18 H18A 109.9 . . ? C17 C18 H18B 109.9 . . ? C19 C18 H18B 109.9 . . ? H18A C18 H18B 108.3 . . ? C19 C20 N3 112.4(7) . . ? C19 C20 C15 104.8(8) . . ? N3 C20 C15 102.0(7) . . ? C19 C20 H20 112.3 . . ? N3 C20 H20 112.3 . . ? C15 C20 H20 112.3 . . ? N2 C15' C20' 100.3(11) . . ? N2 C15' C16 109.8(12) . . ? C20' C15' C16 106.7(13) . . ? N2 C15' H15' 113.0 . . ? C20' C15' H15' 113.0 . . ? C16 C15' H15' 113.0 . . ? C16 C17' C18' 105.5(17) . . ? C16 C17' H17C 110.6 . . ? C18' C17' H17C 110.6 . . ? C16 C17' H17D 110.6 . . ? C18' C17' H17D 110.6 . . ? H17C C17' H17D 108.8 . . ? C19 C18' C17' 104.5(16) . . ? C19 C18' H18C 110.8 . . ? C17' C18' H18C 110.8 . . ? C19 C18' H18D 110.8 . . ? C17' C18' H18D 110.8 . . ? H18C C18' H18D 108.9 . . ? N3 C20' C15' 99.9(13) . . ? N3 C20' C19 113.0(9) . . ? C15' C20' C19 106.0(12) . . ? N3 C20' H20' 112.4 . . ? C15' C20' H20' 112.4 . . ? C19 C20' H20' 112.4 . . ? N3 C21 C22 125.9(3) . . ? N3 C21 H21A 117.1 . . ? C22 C21 H21A 117.1 . . ? C23 C22 C27 118.5(4) . . ? C23 C22 C21 117.0(3) . . ? C27 C22 C21 124.4(3) . . ? C24 C23 C22 121.9(4) . . ? C24 C23 H23A 119.1 . . ? C22 C23 H23A 119.1 . . ? C23 C24 C25 119.8(4) . . ? C23 C24 H24A 120.1 . . ? C25 C24 H24A 120.1 . . ? C24 C25 C26 120.3(4) . . ? C24 C25 H25A 119.9 . . ? C26 C25 H25A 119.9 . . ? C25 C26 C27 121.0(4) . . ? C25 C26 H26A 119.5 . . ? C27 C26 H26A 119.5 . . ? O4 S2 O3 118.02(19) . . ? O4 S2 N4 112.10(17) . . ? O3 S2 N4 104.56(17) . . ? O4 S2 C28 105.82(19) . . ? O3 S2 C28 106.04(17) . . ? N4 S2 C28 110.08(17) . . ? C26 C27 N4 121.8(3) . . ? C26 C27 C22 118.6(3) . . ? N4 C27 C22 119.6(3) . . ? C29 C28 C33 119.9(4) . . ? C29 C28 S2 121.1(3) . . ? C33 C28 S2 119.1(3) . . ? C28 C29 C30 118.6(5) . . ? C28 C29 H29A 120.7 . . ? C30 C29 H29A 120.7 . . ? C31 C30 C29 122.5(5) . . ? C31 C30 H30A 118.7 . . ? C29 C30 H30A 118.7 . . ? C32 C31 C30 117.2(4) . . ? C32 C31 C34 121.2(5) . . ? C30 C31 C34 121.7(5) . . ? C31 C32 C33 122.3(5) . . ? C31 C32 H32A 118.9 . . ? C33 C32 H32A 118.9 . . ? C28 C33 C32 119.5(4) . . ? C28 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N1S C1S C2S 168(4) . . ? N1S C1S C2S' 161(2) . . ? C2S C1S C2S' 31(3) . . ? C1S C2S H2S4 109.5 . . ? C1S C2S H2S5 109.5 . . ? H2S4 C2S H2S5 109.5 . . ? C1S C2S H2S6 109.5 . . ? H2S4 C2S H2S6 109.5 . . ? H2S5 C2S H2S6 109.5 . . ? C1S C2S' H2S1 109.5 . . ? C1S C2S' H2S2 109.5 . . ? H2S1 C2S' H2S2 109.5 . . ? C1S C2S' H2S3 109.5 . . ? H2S1 C2S' H2S3 109.5 . . ? H2S2 C2S' H2S3 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 N3 Cu1 N1 C8 112.0(4) . . . . ? N2 Cu1 N1 C8 42.5(3) . . . . ? N4 Cu1 N1 C8 -118.7(3) . . . . ? N3 Cu1 N1 S1 -54.2(4) . . . . ? N2 Cu1 N1 S1 -123.6(2) . . . . ? N4 Cu1 N1 S1 75.2(2) . . . . ? N3 Cu1 N2 C14 172.7(4) . . . . ? N1 Cu1 N2 C14 -27.8(4) . . . . ? N4 Cu1 N2 C14 96.4(5) . . . . ? N3 Cu1 N2 C15' 16.3(9) . . . . ? N1 Cu1 N2 C15' 175.7(8) . . . . ? N4 Cu1 N2 C15' -60.0(9) . . . . ? N3 Cu1 N2 C15 -20.0(6) . . . . ? N1 Cu1 N2 C15 139.5(6) . . . . ? N4 Cu1 N2 C15 -96.3(6) . . . . ? N1 Cu1 N3 C21 111.2(5) . . . . ? N2 Cu1 N3 C21 -178.4(4) . . . . ? N4 Cu1 N3 C21 -20.0(4) . . . . ? N1 Cu1 N3 C20' -48.9(9) . . . . ? N2 Cu1 N3 C20' 21.5(8) . . . . ? N4 Cu1 N3 C20' 179.9(8) . . . . ? N1 Cu1 N3 C20 -84.2(6) . . . . ? N2 Cu1 N3 C20 -13.8(5) . . . . ? N4 Cu1 N3 C20 144.6(5) . . . . ? N3 Cu1 N4 C27 33.6(3) . . . . ? N1 Cu1 N4 C27 -129.7(3) . . . . ? N2 Cu1 N4 C27 108.5(4) . . . . ? N3 Cu1 N4 S2 -122.7(2) . . . . ? N1 Cu1 N4 S2 74.1(2) . . . . ? N2 Cu1 N4 S2 -47.7(4) . . . . ? C7 C2 C3 C4 1.9(9) . . . . ? C1 C2 C3 C4 -178.5(6) . . . . ? C2 C3 C4 C5 -0.7(8) . . . . ? C3 C4 C5 C6 -1.3(7) . . . . ? C3 C4 C5 S1 178.4(4) . . . . ? C4 C5 C6 C7 2.2(7) . . . . ? S1 C5 C6 C7 -177.5(4) . . . . ? C3 C2 C7 C6 -1.1(9) . . . . ? C1 C2 C7 C6 179.4(6) . . . . ? C5 C6 C7 C2 -1.0(8) . . . . ? C8 N1 S1 O2 66.8(3) . . . . ? Cu1 N1 S1 O2 -126.82(19) . . . . ? C8 N1 S1 O1 -164.7(3) . . . . ? Cu1 N1 S1 O1 1.6(2) . . . . ? C8 N1 S1 C5 -49.8(3) . . . . ? Cu1 N1 S1 C5 116.6(2) . . . . ? C6 C5 S1 O2 -20.8(4) . . . . ? C4 C5 S1 O2 159.5(3) . . . . ? C6 C5 S1 O1 -145.9(3) . . . . ? C4 C5 S1 O1 34.4(4) . . . . ? C6 C5 S1 N1 101.2(4) . . . . ? C4 C5 S1 N1 -78.5(4) . . . . ? S1 N1 C8 C9 -50.6(5) . . . . ? Cu1 N1 C8 C9 143.9(3) . . . . ? S1 N1 C8 C13 129.6(3) . . . . ? Cu1 N1 C8 C13 -35.9(5) . . . . ? C13 C8 C9 C10 -0.3(6) . . . . ? N1 C8 C9 C10 179.9(4) . . . . ? C8 C9 C10 C11 -1.1(7) . . . . ? C9 C10 C11 C12 1.2(7) . . . . ? C10 C11 C12 C13 0.1(7) . . . . ? C11 C12 C13 C8 -1.4(6) . . . . ? C11 C12 C13 C14 178.6(4) . . . . ? C9 C8 C13 C12 1.4(6) . . . . ? N1 C8 C13 C12 -178.7(4) . . . . ? C9 C8 C13 C14 -178.5(4) . . . . ? N1 C8 C13 C14 1.4(6) . . . . ? C15' N2 C14 C13 159.2(10) . . . . ? C15 N2 C14 C13 -160.6(7) . . . . ? Cu1 N2 C14 C13 5.5(7) . . . . ? C12 C13 C14 N2 -164.7(5) . . . . ? C8 C13 C14 N2 15.2(7) . . . . ? C17' C16 C15 N2 -148.3(11) . . . . ? C17 C16 C15 N2 -174.1(8) . . . . ? C15' C16 C15 N2 -64.1(13) . . . . ? C17' C16 C15 C20 -38.3(17) . . . . ? C17 C16 C15 C20 -64.1(13) . . . . ? C15' C16 C15 C20 45.9(10) . . . . ? C14 N2 C15 C16 -32.1(11) . . . . ? C15' N2 C15 C16 67.8(13) . . . . ? Cu1 N2 C15 C16 160.1(5) . . . . ? C14 N2 C15 C20 -144.7(7) . . . . ? C15' N2 C15 C20 -44.8(9) . . . . ? Cu1 N2 C15 C20 47.5(10) . . . . ? C17' C16 C17 C18 -48(3) . . . . ? C15 C16 C17 C18 60.0(15) . . . . ? C15' C16 C17 C18 25.1(19) . . . . ? C16 C17 C18 C19 -59.0(15) . . . . ? C18' C19 C18 C17 -44.1(12) . . . . ? C20 C19 C18 C17 63.9(14) . . . . ? C20' C19 C18 C17 30.7(19) . . . . ? C18' C19 C20 N3 -138.8(10) . . . . ? C18 C19 C20 N3 -179.0(6) . . . . ? C20' C19 C20 N3 -61.5(10) . . . . ? C18' C19 C20 C15 -28.8(17) . . . . ? C18 C19 C20 C15 -69.0(12) . . . . ? C20' C19 C20 C15 48.5(9) . . . . ? C21 N3 C20 C19 -40.0(9) . . . . ? C20' N3 C20 C19 64.4(10) . . . . ? Cu1 N3 C20 C19 154.3(5) . . . . ? C21 N3 C20 C15 -151.7(7) . . . . ? C20' N3 C20 C15 -47.3(10) . . . . ? Cu1 N3 C20 C15 42.6(9) . . . . ? C16 C15 C20 C19 70.6(11) . . . . ? N2 C15 C20 C19 -171.7(5) . . . . ? C16 C15 C20 N3 -172.1(6) . . . . ? N2 C15 C20 N3 -54.4(10) . . . . ? C14 N2 C15' C20' 153.7(10) . . . . ? C15 N2 C15' C20' 51.9(11) . . . . ? Cu1 N2 C15' C20' -48.8(16) . . . . ? C14 N2 C15' C16 41.6(15) . . . . ? C15 N2 C15' C16 -60.2(16) . . . . ? Cu1 N2 C15' C16 -160.9(7) . . . . ? C17' C16 C15' N2 171.5(9) . . . . ? C15 C16 C15' N2 63.3(16) . . . . ? C17 C16 C15' N2 146.9(8) . . . . ? C17' C16 C15' C20' 64(2) . . . . ? C15 C16 C15' C20' -44.5(11) . . . . ? C17 C16 C15' C20' 39(2) . . . . ? C15 C16 C17' C18' -32(2) . . . . ? C17 C16 C17' C18' 49(2) . . . . ? C15' C16 C17' C18' -67(2) . . . . ? C20 C19 C18' C17' -40(2) . . . . ? C18 C19 C18' C17' 45.7(14) . . . . ? C20' C19 C18' C17' -73(2) . . . . ? C16 C17' C18' C19 74(2) . . . . ? C21 N3 C20' C15' 145.9(10) . . . . ? C20 N3 C20' C15' 49.7(15) . . . . ? Cu1 N3 C20' C15' -53.0(15) . . . . ? C21 N3 C20' C19 33.7(16) . . . . ? C20 N3 C20' C19 -62.5(13) . . . . ? Cu1 N3 C20' C19 -165.2(9) . . . . ? N2 C15' C20' N3 63.5(17) . . . . ? C16 C15' C20' N3 178.0(8) . . . . ? N2 C15' C20' C19 -178.9(8) . . . . ? C16 C15' C20' C19 -64.4(19) . . . . ? C18' C19 C20' N3 178.5(9) . . . . ? C20 C19 C20' N3 65.3(15) . . . . ? C18 C19 C20' N3 140.4(8) . . . . ? C18' C19 C20' C15' 70(2) . . . . ? C20 C19 C20' C15' -43.1(14) . . . . ? C18 C19 C20' C15' 32(2) . . . . ? C20' N3 C21 C22 158.6(10) . . . . ? C20 N3 C21 C22 -162.5(6) . . . . ? Cu1 N3 C21 C22 1.0(7) . . . . ? N3 C21 C22 C23 -166.0(4) . . . . ? N3 C21 C22 C27 14.1(7) . . . . ? C27 C22 C23 C24 -2.0(6) . . . . ? C21 C22 C23 C24 178.1(4) . . . . ? C22 C23 C24 C25 0.5(7) . . . . ? C23 C24 C25 C26 1.1(8) . . . . ? C24 C25 C26 C27 -1.2(7) . . . . ? C27 N4 S2 O4 -31.4(3) . . . . ? Cu1 N4 S2 O4 125.90(19) . . . . ? C27 N4 S2 O3 -160.4(3) . . . . ? Cu1 N4 S2 O3 -3.1(2) . . . . ? C27 N4 S2 C28 86.1(3) . . . . ? Cu1 N4 S2 C28 -116.60(19) . . . . ? C25 C26 C27 N4 180.0(4) . . . . ? C25 C26 C27 C22 -0.2(6) . . . . ? S2 N4 C27 C26 -54.8(5) . . . . ? Cu1 N4 C27 C26 150.4(3) . . . . ? S2 N4 C27 C22 125.4(3) . . . . ? Cu1 N4 C27 C22 -29.4(5) . . . . ? C23 C22 C27 C26 1.8(6) . . . . ? C21 C22 C27 C26 -178.3(4) . . . . ? C23 C22 C27 N4 -178.4(4) . . . . ? C21 C22 C27 N4 1.5(6) . . . . ? O4 S2 C28 C29 3.6(4) . . . . ? O3 S2 C28 C29 129.7(4) . . . . ? N4 S2 C28 C29 -117.7(4) . . . . ? O4 S2 C28 C33 -174.2(3) . . . . ? O3 S2 C28 C33 -48.1(4) . . . . ? N4 S2 C28 C33 64.5(4) . . . . ? C33 C28 C29 C30 -1.0(8) . . . . ? S2 C28 C29 C30 -178.9(4) . . . . ? C28 C29 C30 C31 0.1(10) . . . . ? C29 C30 C31 C32 1.1(9) . . . . ? C29 C30 C31 C34 -179.1(6) . . . . ? C30 C31 C32 C33 -1.3(9) . . . . ? C34 C31 C32 C33 178.9(5) . . . . ? C29 C28 C33 C32 0.9(7) . . . . ? S2 C28 C33 C32 178.7(4) . . . . ? C31 C32 C33 C28 0.3(8) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.341 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.102 #===END