# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_2003be15 _database_code_depnum_ccdc_archive 'CCDC 877814' #TrackingRef '- 1.cif' _audit_creation_date 2012-02-24T15:20:46-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H23 N3 O3 S ' _chemical_formula_sum 'C25 H23 N3 O3 S ' _chemical_formula_weight 445.53 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5395(18) _cell_length_b 14.248(3) _cell_length_c 14.5284(17) _cell_angle_alpha 75.654(13) _cell_angle_beta 78.072(8) _cell_angle_gamma 77.710(19) _cell_volume 2231.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 23 _cell_measurement_theta_min 18.59 _cell_measurement_theta_max 42.11 _cell_measurement_wavelength 1.5418 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 936 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.553 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7824 _exptl_absorpt_correction_T_max 0.8792 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 6 Theta correction was applied. Averaged transmission function was used. Fourier smoothing - Window value 1 ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_unetI/netI 0.0555 _diffrn_reflns_number 9254 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 72.93 _diffrn_reflns_theta_full 72.93 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8886 _reflns_number_gt 5768 _reflns_threshold_expression >2\s(I) _diffrn_standards_number 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 -6 -4 1 -3 -1 -6 -1 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 1 _diffrn_standards_decay_corr_max 1.049 _diffrn_standards_decay_corr_min 0.977 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 0.030434 _diffrn_orient_matrix_UB_12 -0.070997 _diffrn_orient_matrix_UB_13 -0.000953 _diffrn_orient_matrix_UB_21 -0.079407 _diffrn_orient_matrix_UB_22 -0.006297 _diffrn_orient_matrix_UB_23 -0.013097 _diffrn_orient_matrix_UB_31 0.029165 _diffrn_orient_matrix_UB_32 0.018076 _diffrn_orient_matrix_UB_33 -0.070803 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR-97 (Giacovazzo et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0954P)^2^+0.0656P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8886 _refine_ls_number_parameters 589 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.051 _refine_ls_wR_factor_ref 0.1566 _refine_ls_wR_factor_gt 0.1338 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.21 _refine_diff_density_min -0.763 _refine_diff_density_rms 0.063 _iucr_refine_instructions_details ; TITL 2003be15 in P -1 CELL 1.54180 11.5395 14.2480 14.5284 75.654 78.072 77.710 ZERR 2.00 0.0018 0.0030 0.0017 0.013 0.008 0.019 LATT 1 SFAC C H N O S UNIT 100 92 12 12 4 MERG 2 OMIT -2 -4 3 OMIT 7 2 8 OMIT 10 -4 1 OMIT 3 1 3 OMIT 4 9 15 OMIT 1 -11 10 EQIV $2 1-x,-y, 1-z HTAB O4 N4 HTAB O1 N1 HTAB N2 O4_$2 HTAB N5 O1_$2 DFIX 0.85 N2 H2N DFIX 0.85 N5 H5N DFIX 0.85 O1 H1O DFIX 0.85 O4 H4O FMAP 2 PLAN 20 ACTA BOND $H CONF L.S. 14 WGHT 0.095400 0.065600 FVAR 0.78679 O1 4 0.583426 0.139550 0.225703 11.00000 0.03953 0.04442 = 0.06074 -0.00619 -0.00450 -0.00606 H1O 2 0.635636 0.172483 0.182754 11.00000 -1.50000 C1 1 0.474029 0.199064 0.228951 11.00000 0.03755 0.04430 = 0.04650 -0.01542 -0.00635 -0.00776 C2 1 0.378099 0.167270 0.295024 11.00000 0.05394 0.05387 = 0.05528 -0.01391 0.00439 -0.01645 AFIX 43 H2 2 0.389284 0.107076 0.338158 11.00000 -1.20000 AFIX 0 C3 1 0.265908 0.225006 0.296781 11.00000 0.04339 0.07189 = 0.07313 -0.02824 0.01264 -0.01917 AFIX 43 H3 2 0.201555 0.202882 0.340938 11.00000 -1.20000 AFIX 0 C4 1 0.247237 0.314928 0.234341 11.00000 0.03517 0.07410 = 0.07861 -0.02960 0.00047 -0.00615 AFIX 43 H4 2 0.171036 0.353232 0.236340 11.00000 -1.20000 AFIX 0 C5 1 0.342130 0.347300 0.169285 11.00000 0.04108 0.05420 = 0.06231 -0.01915 -0.01072 0.00068 AFIX 43 H5 2 0.329775 0.408057 0.127187 11.00000 -1.20000 AFIX 0 C6 1 0.457170 0.290631 0.165068 11.00000 0.03287 0.04636 = 0.04538 -0.01664 -0.00536 -0.00589 C7 1 0.552794 0.325619 0.092039 11.00000 0.04090 0.04355 = 0.04410 -0.00820 -0.00962 -0.00638 AFIX 43 H7 2 0.535920 0.387047 0.051948 11.00000 -1.20000 AFIX 0 N1 3 0.660114 0.276718 0.079170 11.00000 0.03196 0.04734 = 0.03805 -0.00611 -0.00745 -0.00873 C8 1 0.739963 0.316166 -0.002309 11.00000 0.03739 0.04127 = 0.03806 -0.00723 -0.00557 -0.00492 C9 1 0.702853 0.352649 -0.091429 11.00000 0.04730 0.06441 = 0.04298 -0.00746 -0.01357 -0.00190 AFIX 43 H9 2 0.626206 0.347516 -0.098258 11.00000 -1.20000 AFIX 0 C10 1 0.777574 0.396325 -0.169933 11.00000 0.06565 0.06259 = 0.04074 -0.00082 -0.00939 -0.00229 AFIX 43 H10 2 0.750995 0.421566 -0.228841 11.00000 -1.20000 AFIX 0 C11 1 0.891240 0.402193 -0.160367 11.00000 0.06816 0.05483 = 0.04277 -0.00463 0.00892 -0.01267 AFIX 43 H11 2 0.940735 0.434157 -0.212279 11.00000 -1.20000 AFIX 0 C12 1 0.933368 0.360610 -0.073387 11.00000 0.04961 0.05442 = 0.04836 -0.01157 0.00224 -0.01501 AFIX 43 H12 2 1.012072 0.361890 -0.068456 11.00000 -1.20000 AFIX 0 C13 1 0.857937 0.317341 0.005776 11.00000 0.03734 0.03875 = 0.04067 -0.00802 -0.00530 -0.00553 N2 3 0.901071 0.276573 0.094975 11.00000 0.04150 0.04201 = 0.04467 -0.00176 -0.01243 -0.01329 H2N 2 0.874098 0.226954 0.132171 11.00000 -1.20000 S1 5 0.922052 0.350901 0.157444 11.00000 0.04192 0.05385 = 0.05065 -0.00573 -0.01674 -0.01739 O2 4 0.958850 0.288841 0.243889 11.00000 0.05426 0.07000 = 0.05744 -0.00310 -0.03200 -0.01052 O3 4 0.999841 0.414397 0.095851 11.00000 0.05138 0.06379 = 0.07336 -0.00757 -0.01041 -0.03006 C14 1 0.780287 0.424898 0.184900 11.00000 0.05068 0.04380 = 0.04298 -0.00762 -0.01599 -0.01587 C15 1 0.762405 0.516982 0.125346 11.00000 0.05801 0.04863 = 0.04748 -0.00136 -0.01027 -0.01859 AFIX 43 H15 2 0.823197 0.537090 0.075942 11.00000 -1.20000 AFIX 0 C16 1 0.651592 0.580249 0.139860 11.00000 0.07185 0.04372 = 0.04817 0.00559 -0.01434 -0.01454 AFIX 43 H16 2 0.638651 0.641760 0.099085 11.00000 -1.20000 AFIX 0 C17 1 0.563491 0.551754 0.213230 11.00000 0.06007 0.04334 = 0.04573 -0.00273 -0.01671 -0.00719 AFIX 43 H17 2 0.491505 0.595008 0.222495 11.00000 -1.20000 AFIX 0 C18 1 0.578267 0.457723 0.276192 11.00000 0.05369 0.04166 = 0.03215 -0.00577 -0.01537 -0.01238 C23 1 0.688559 0.390368 0.260131 11.00000 0.05208 0.04235 = 0.03584 -0.00573 -0.01663 -0.01365 C19 1 0.483687 0.428083 0.351995 11.00000 0.05720 0.05051 = 0.03428 -0.01000 -0.01405 -0.01363 C20 1 0.497709 0.331834 0.403264 11.00000 0.06671 0.05426 = 0.03649 -0.00001 -0.00597 -0.02193 AFIX 43 H20 2 0.436009 0.310761 0.451228 11.00000 -1.20000 AFIX 0 C21 1 0.603371 0.265821 0.383947 11.00000 0.06966 0.04290 = 0.04667 0.00535 -0.01572 -0.01405 AFIX 43 H21 2 0.609690 0.201147 0.418638 11.00000 -1.20000 AFIX 0 C22 1 0.696817 0.293117 0.316289 11.00000 0.05742 0.04343 = 0.04616 -0.00017 -0.01731 -0.00795 AFIX 43 H22 2 0.766833 0.247845 0.306573 11.00000 -1.20000 AFIX 0 N3 3 0.377323 0.497018 0.367654 11.00000 0.05988 0.05453 = 0.04519 -0.01231 -0.00399 -0.01242 C24 1 0.269937 0.456200 0.415248 11.00000 0.06550 0.08798 = 0.06035 -0.01596 0.00706 -0.02079 AFIX 33 H24A 2 0.203357 0.508676 0.422547 11.00000 -1.50000 H24B 2 0.282492 0.416879 0.477510 11.00000 -1.50000 H24C 2 0.252910 0.416039 0.377177 11.00000 -1.50000 AFIX 0 C25 1 0.388315 0.577040 0.409840 11.00000 0.09517 0.06325 = 0.07936 -0.03134 0.00069 -0.01574 AFIX 33 H25A 2 0.311936 0.619487 0.417819 11.00000 -1.50000 H25B 2 0.446665 0.613907 0.368035 11.00000 -1.50000 H25C 2 0.413571 0.550343 0.471405 11.00000 -1.50000 AFIX 0 O4 4 0.145505 -0.079696 0.798109 11.00000 0.04404 0.04435 = 0.08226 -0.01334 -0.01766 -0.00420 H4O 2 0.190225 -0.051464 0.820854 11.00000 -1.50000 C26 1 0.038492 -0.017394 0.791825 11.00000 0.03624 0.04492 = 0.05141 -0.00201 -0.00597 -0.00889 C27 1 -0.049929 -0.045128 0.757260 11.00000 0.05100 0.06051 = 0.06758 -0.00530 -0.01476 -0.01742 AFIX 43 H27 2 -0.036110 -0.105411 0.739448 11.00000 -1.20000 AFIX 0 C28 1 -0.157322 0.016712 0.749595 11.00000 0.04814 0.07772 = 0.07910 0.00246 -0.01984 -0.02216 AFIX 43 H28 2 -0.216691 -0.002449 0.727240 11.00000 -1.20000 AFIX 0 C29 1 -0.179275 0.106964 0.774388 11.00000 0.03558 0.07759 = 0.09525 -0.00176 -0.01152 -0.00520 AFIX 43 H29 2 -0.251896 0.149096 0.767085 11.00000 -1.20000 AFIX 0 C30 1 -0.093081 0.133996 0.809889 11.00000 0.03998 0.06100 = 0.08694 -0.01557 -0.00343 -0.00272 AFIX 43 H30 2 -0.108577 0.194153 0.828154 11.00000 -1.20000 AFIX 0 C31 1 0.017822 0.072653 0.819128 11.00000 0.03661 0.04676 = 0.05296 -0.00362 -0.00100 -0.00780 C32 1 0.106726 0.103217 0.857634 11.00000 0.04407 0.04645 = 0.05797 -0.01399 -0.00083 -0.01008 AFIX 43 H32 2 0.085726 0.161363 0.879918 11.00000 -1.20000 AFIX 0 N4 3 0.212516 0.054082 0.862406 11.00000 0.03960 0.04803 = 0.04519 -0.00695 -0.00487 -0.01147 C33 1 0.289564 0.086094 0.908494 11.00000 0.05286 0.04339 = 0.04026 -0.00600 -0.00777 -0.01432 C34 1 0.249006 0.115058 0.996015 11.00000 0.07010 0.07543 = 0.04601 -0.01796 0.00234 -0.02092 AFIX 43 H34 2 0.169039 0.115273 1.024583 11.00000 -1.20000 AFIX 0 C35 1 0.326243 0.143481 1.040891 11.00000 0.10275 0.07204 = 0.04513 -0.01887 -0.01521 -0.02217 AFIX 43 H35 2 0.297999 0.163094 1.099141 11.00000 -1.20000 AFIX 0 C36 1 0.445415 0.142816 0.999358 11.00000 0.09385 0.06405 = 0.05585 -0.01318 -0.03145 -0.02391 AFIX 43 H36 2 0.497364 0.162224 1.029402 11.00000 -1.20000 AFIX 0 C37 1 0.486836 0.113389 0.913558 11.00000 0.05881 0.05224 = 0.05302 -0.00382 -0.02268 -0.01554 AFIX 43 H37 2 0.567328 0.111956 0.886132 11.00000 -1.20000 AFIX 0 C38 1 0.409747 0.085832 0.867542 11.00000 0.04953 0.03484 = 0.03882 -0.00228 -0.01316 -0.00973 N5 3 0.457971 0.055344 0.778044 11.00000 0.04221 0.04341 = 0.04278 -0.00598 -0.00968 -0.01053 H5N 2 0.434813 0.007132 0.770196 11.00000 -1.20000 S2 5 0.481410 0.138312 0.679569 11.00000 0.03547 0.05419 = 0.04543 -0.00069 -0.00494 -0.01282 O5 4 0.539388 0.207840 0.701089 11.00000 0.04817 0.05956 = 0.07460 0.00604 -0.01659 -0.02696 O6 4 0.540854 0.086122 0.606027 11.00000 0.05100 0.07748 = 0.05192 -0.01122 0.00921 -0.00322 C39 1 0.336596 0.201297 0.655320 11.00000 0.04077 0.05096 = 0.03527 -0.00256 -0.00663 -0.00940 C40 1 0.296354 0.285667 0.688344 11.00000 0.04912 0.05746 = 0.04631 -0.01386 -0.00913 -0.01263 AFIX 43 H40 2 0.347075 0.309841 0.715468 11.00000 -1.20000 AFIX 0 C41 1 0.178560 0.336888 0.681905 11.00000 0.05357 0.06710 = 0.05853 -0.02955 -0.00744 -0.00074 AFIX 43 H41 2 0.150580 0.393053 0.707097 11.00000 -1.20000 AFIX 0 C42 1 0.106269 0.303983 0.638879 11.00000 0.04273 0.07362 = 0.04552 -0.02136 -0.00947 0.00250 AFIX 43 H42 2 0.028453 0.337916 0.635272 11.00000 -1.20000 AFIX 0 C43 1 0.146640 0.218653 0.599044 11.00000 0.04222 0.05912 = 0.03280 -0.00877 -0.00522 -0.00917 C44 1 0.070063 0.186429 0.551667 11.00000 0.04511 0.07281 = 0.03549 -0.00909 -0.00610 -0.01234 C45 1 0.106184 0.096128 0.527395 11.00000 0.06938 0.07735 = 0.05827 -0.01952 -0.02025 -0.02129 AFIX 43 H45 2 0.055447 0.072191 0.500069 11.00000 -1.20000 AFIX 0 C46 1 0.218231 0.039646 0.543200 11.00000 0.08458 0.06118 = 0.07049 -0.01826 -0.02635 -0.01383 AFIX 43 H46 2 0.239839 -0.021535 0.526779 11.00000 -1.20000 AFIX 0 C47 1 0.295469 0.071342 0.581439 11.00000 0.06537 0.05226 = 0.05805 -0.01065 -0.01910 -0.00412 AFIX 43 H47 2 0.370678 0.033421 0.588393 11.00000 -1.20000 AFIX 0 C48 1 0.262792 0.162541 0.611312 11.00000 0.04145 0.04991 = 0.03285 -0.00554 -0.00445 -0.00988 N6 3 -0.039753 0.248624 0.532823 11.00000 0.04649 0.09834 = 0.04913 -0.02095 -0.01581 -0.00852 C49 1 -0.026284 0.340355 0.461453 11.00000 0.06559 0.09287 = 0.05946 -0.01894 -0.02223 0.01192 AFIX 33 H49A 2 -0.104267 0.378114 0.452914 11.00000 -1.50000 H49B 2 0.015824 0.325268 0.401198 11.00000 -1.50000 H49C 2 0.018399 0.377658 0.483584 11.00000 -1.50000 AFIX 0 C50 1 -0.129335 0.201251 0.512153 11.00000 0.05854 0.14177 = 0.07827 -0.03445 -0.02574 -0.02203 AFIX 33 H50A 2 -0.199921 0.249061 0.500138 11.00000 -1.50000 H50B 2 -0.150086 0.150022 0.566340 11.00000 -1.50000 H50C 2 -0.096781 0.173584 0.456418 11.00000 -1.50000 HKLF 4 REM 2003be15 in P -1 REM R1 = 0.0510 for 5768 Fo > 4sig(Fo) and 0.1078 for all 8886 data REM 589 parameters refined using 4 restraints END WGHT 0.0954 0.0657 REM Highest difference peak 0.210, deepest hole -0.763, 1-sigma level 0.063 Q1 1 0.5041 0.5860 0.3863 11.00000 0.05 0.21 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.58343(15) 0.13955(13) 0.22570(14) 0.0499(4) Uani 1 1 d D . . H1O H 0.636(3) 0.172(2) 0.183(2) 0.075 Uiso 1 1 d D . . C1 C 0.4740(2) 0.19906(18) 0.22895(18) 0.0417(5) Uani 1 1 d . . . C2 C 0.3781(3) 0.1673(2) 0.2950(2) 0.0548(7) Uani 1 1 d . . . H2 H 0.3893 0.1071 0.3382 0.066 Uiso 1 1 calc R . . C3 C 0.2659(3) 0.2250(2) 0.2968(2) 0.0624(8) Uani 1 1 d . . . H3 H 0.2016 0.2029 0.3409 0.075 Uiso 1 1 calc R . . C4 C 0.2472(2) 0.3149(2) 0.2343(3) 0.0622(8) Uani 1 1 d . . . H4 H 0.171 0.3532 0.2363 0.075 Uiso 1 1 calc R . . C5 C 0.3421(2) 0.3473(2) 0.1693(2) 0.0523(7) Uani 1 1 d . . . H5 H 0.3298 0.4081 0.1272 0.063 Uiso 1 1 calc R . . C6 C 0.4572(2) 0.29063(18) 0.16507(18) 0.0406(5) Uani 1 1 d . . . C7 C 0.5528(2) 0.32562(19) 0.09204(18) 0.0428(5) Uani 1 1 d . . . H7 H 0.5359 0.387 0.0519 0.051 Uiso 1 1 calc R . . N1 N 0.66011(17) 0.27672(15) 0.07917(14) 0.0391(4) Uani 1 1 d . . . C8 C 0.7400(2) 0.31617(18) -0.00231(17) 0.0395(5) Uani 1 1 d . . . C9 C 0.7029(2) 0.3526(2) -0.09143(19) 0.0525(7) Uani 1 1 d . . . H9 H 0.6262 0.3475 -0.0983 0.063 Uiso 1 1 calc R . . C10 C 0.7776(3) 0.3963(2) -0.1699(2) 0.0594(7) Uani 1 1 d . . . H10 H 0.751 0.4216 -0.2288 0.071 Uiso 1 1 calc R . . C11 C 0.8912(3) 0.4022(2) -0.1604(2) 0.0586(7) Uani 1 1 d . . . H11 H 0.9407 0.4342 -0.2123 0.07 Uiso 1 1 calc R . . C12 C 0.9334(3) 0.3606(2) -0.0734(2) 0.0513(6) Uani 1 1 d . . . H12 H 1.0121 0.3619 -0.0685 0.062 Uiso 1 1 calc R . . C13 C 0.8579(2) 0.31734(17) 0.00578(18) 0.0393(5) Uani 1 1 d . . . N2 N 0.90107(18) 0.27657(15) 0.09498(15) 0.0423(5) Uani 1 1 d D . . H2N H 0.874(2) 0.2270(16) 0.1322(18) 0.051 Uiso 1 1 d D . . S1 S 0.92205(6) 0.35090(5) 0.15744(5) 0.04699(17) Uani 1 1 d . . . O2 O 0.95885(17) 0.28884(15) 0.24389(15) 0.0590(5) Uani 1 1 d . . . O3 O 0.99984(17) 0.41440(15) 0.09585(16) 0.0610(5) Uani 1 1 d . . . C14 C 0.7803(2) 0.42490(18) 0.18490(18) 0.0437(6) Uani 1 1 d . . . C15 C 0.7624(3) 0.5170(2) 0.1253(2) 0.0513(6) Uani 1 1 d . . . H15 H 0.8232 0.5371 0.0759 0.062 Uiso 1 1 calc R . . C16 C 0.6516(3) 0.5802(2) 0.1399(2) 0.0560(7) Uani 1 1 d . . . H16 H 0.6387 0.6418 0.0991 0.067 Uiso 1 1 calc R . . C17 C 0.5635(3) 0.55175(19) 0.21323(19) 0.0500(6) Uani 1 1 d . . . H17 H 0.4915 0.595 0.2225 0.06 Uiso 1 1 calc R . . C18 C 0.5783(2) 0.45772(18) 0.27619(17) 0.0410(5) Uani 1 1 d . . . C23 C 0.6886(2) 0.39037(18) 0.26013(17) 0.0416(5) Uani 1 1 d . . . C19 C 0.4837(2) 0.4281(2) 0.35200(18) 0.0455(6) Uani 1 1 d . . . C20 C 0.4977(3) 0.3318(2) 0.40326(19) 0.0528(7) Uani 1 1 d . . . H20 H 0.436 0.3108 0.4512 0.063 Uiso 1 1 calc R . . C21 C 0.6034(3) 0.2658(2) 0.3839(2) 0.0541(7) Uani 1 1 d . . . H21 H 0.6097 0.2011 0.4186 0.065 Uiso 1 1 calc R . . C22 C 0.6968(3) 0.29312(19) 0.31629(19) 0.0495(6) Uani 1 1 d . . . H22 H 0.7668 0.2478 0.3066 0.059 Uiso 1 1 calc R . . N3 N 0.3773(2) 0.49702(17) 0.36765(17) 0.0532(6) Uani 1 1 d . . . C24 C 0.2699(3) 0.4562(3) 0.4152(3) 0.0727(9) Uani 1 1 d . . . H24A H 0.2034 0.5087 0.4225 0.109 Uiso 1 1 calc R . . H24B H 0.2825 0.4169 0.4775 0.109 Uiso 1 1 calc R . . H24C H 0.2529 0.416 0.3772 0.109 Uiso 1 1 calc R . . C25 C 0.3883(4) 0.5770(3) 0.4098(3) 0.0782(10) Uani 1 1 d . . . H25A H 0.3119 0.6195 0.4178 0.117 Uiso 1 1 calc R . . H25B H 0.4467 0.6139 0.368 0.117 Uiso 1 1 calc R . . H25C H 0.4136 0.5503 0.4714 0.117 Uiso 1 1 calc R . . O4 O 0.14550(17) -0.07970(14) 0.79811(17) 0.0563(5) Uani 1 1 d D . . H4O H 0.190(3) -0.051(2) 0.821(3) 0.084 Uiso 1 1 d D . . C26 C 0.0385(2) -0.01739(19) 0.79183(19) 0.0456(6) Uani 1 1 d . . . C27 C -0.0499(3) -0.0451(2) 0.7573(2) 0.0592(7) Uani 1 1 d . . . H27 H -0.0361 -0.1054 0.7394 0.071 Uiso 1 1 calc R . . C28 C -0.1573(3) 0.0167(3) 0.7496(3) 0.0686(9) Uani 1 1 d . . . H28 H -0.2167 -0.0024 0.7272 0.082 Uiso 1 1 calc R . . C29 C -0.1793(3) 0.1070(3) 0.7744(3) 0.0730(10) Uani 1 1 d . . . H29 H -0.2519 0.1491 0.7671 0.088 Uiso 1 1 calc R . . C30 C -0.0931(3) 0.1340(2) 0.8099(3) 0.0646(8) Uani 1 1 d . . . H30 H -0.1086 0.1942 0.8282 0.078 Uiso 1 1 calc R . . C31 C 0.0178(2) 0.07265(19) 0.8191(2) 0.0475(6) Uani 1 1 d . . . C32 C 0.1067(2) 0.1032(2) 0.8576(2) 0.0497(6) Uani 1 1 d . . . H32 H 0.0857 0.1614 0.8799 0.06 Uiso 1 1 calc R . . N4 N 0.21252(18) 0.05408(16) 0.86241(16) 0.0445(5) Uani 1 1 d . . . C33 C 0.2896(2) 0.08609(19) 0.90849(18) 0.0451(6) Uani 1 1 d . . . C34 C 0.2490(3) 0.1151(2) 0.9960(2) 0.0634(8) Uani 1 1 d . . . H34 H 0.169 0.1153 1.0246 0.076 Uiso 1 1 calc R . . C35 C 0.3262(4) 0.1435(3) 1.0409(2) 0.0706(9) Uani 1 1 d . . . H35 H 0.298 0.1631 1.0991 0.085 Uiso 1 1 calc R . . C36 C 0.4454(3) 0.1428(2) 0.9994(2) 0.0667(9) Uani 1 1 d . . . H36 H 0.4974 0.1622 1.0294 0.08 Uiso 1 1 calc R . . C37 C 0.4868(3) 0.1134(2) 0.9136(2) 0.0531(7) Uani 1 1 d . . . H37 H 0.5673 0.112 0.8861 0.064 Uiso 1 1 calc R . . C38 C 0.4097(2) 0.08583(17) 0.86754(17) 0.0408(5) Uani 1 1 d . . . N5 N 0.45797(19) 0.05534(15) 0.77804(15) 0.0425(5) Uani 1 1 d D . . H5N H 0.435(2) 0.0071(16) 0.770(2) 0.051 Uiso 1 1 d D . . S2 S 0.48141(5) 0.13831(5) 0.67957(5) 0.04627(17) Uani 1 1 d . . . O5 O 0.53939(17) 0.20784(14) 0.70109(16) 0.0607(5) Uani 1 1 d . . . O6 O 0.54085(18) 0.08612(16) 0.60603(15) 0.0644(6) Uani 1 1 d . . . C39 C 0.3366(2) 0.20130(19) 0.65532(17) 0.0432(6) Uani 1 1 d . . . C40 C 0.2964(2) 0.2857(2) 0.68834(19) 0.0497(6) Uani 1 1 d . . . H40 H 0.3471 0.3098 0.7155 0.06 Uiso 1 1 calc R . . C41 C 0.1786(3) 0.3369(2) 0.6819(2) 0.0585(7) Uani 1 1 d . . . H41 H 0.1506 0.3931 0.7071 0.07 Uiso 1 1 calc R . . C42 C 0.1063(2) 0.3040(2) 0.6389(2) 0.0540(7) Uani 1 1 d . . . H42 H 0.0285 0.3379 0.6353 0.065 Uiso 1 1 calc R . . C43 C 0.1466(2) 0.2187(2) 0.59904(17) 0.0449(6) Uani 1 1 d . . . C44 C 0.0701(2) 0.1864(2) 0.55167(19) 0.0513(6) Uani 1 1 d . . . C45 C 0.1062(3) 0.0961(3) 0.5274(2) 0.0646(8) Uani 1 1 d . . . H45 H 0.0554 0.0722 0.5001 0.078 Uiso 1 1 calc R . . C46 C 0.2182(3) 0.0396(2) 0.5432(2) 0.0690(9) Uani 1 1 d . . . H46 H 0.2398 -0.0215 0.5268 0.083 Uiso 1 1 calc R . . C47 C 0.2955(3) 0.0713(2) 0.5814(2) 0.0583(7) Uani 1 1 d . . . H47 H 0.3707 0.0334 0.5884 0.07 Uiso 1 1 calc R . . C48 C 0.2628(2) 0.16254(19) 0.61131(17) 0.0419(5) Uani 1 1 d . . . N6 N -0.0398(2) 0.2486(2) 0.53282(18) 0.0631(7) Uani 1 1 d . . . C49 C -0.0263(3) 0.3404(3) 0.4615(2) 0.0743(10) Uani 1 1 d . . . H49A H -0.1043 0.3781 0.4529 0.111 Uiso 1 1 calc R . . H49B H 0.0158 0.3253 0.4012 0.111 Uiso 1 1 calc R . . H49C H 0.0184 0.3777 0.4836 0.111 Uiso 1 1 calc R . . C50 C -0.1293(3) 0.2013(3) 0.5122(3) 0.0879(12) Uani 1 1 d . . . H50A H -0.1999 0.2491 0.5001 0.132 Uiso 1 1 calc R . . H50B H -0.1501 0.15 0.5663 0.132 Uiso 1 1 calc R . . H50C H -0.0968 0.1736 0.4564 0.132 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 O1 0.0395(9) 0.0444(10) 0.0607(12) -0.0062(9) -0.0045(8) -0.0061(8) C1 0.0375(12) 0.0443(13) 0.0465(13) -0.0154(11) -0.0063(10) -0.0078(10) C2 0.0539(16) 0.0539(16) 0.0553(16) -0.0139(13) 0.0044(13) -0.0164(13) C3 0.0434(15) 0.072(2) 0.073(2) -0.0282(17) 0.0126(14) -0.0192(14) C4 0.0352(13) 0.074(2) 0.079(2) -0.0296(18) 0.0005(13) -0.0061(13) C5 0.0411(13) 0.0542(15) 0.0623(17) -0.0191(14) -0.0107(12) 0.0007(12) C6 0.0329(11) 0.0464(13) 0.0454(13) -0.0166(11) -0.0054(10) -0.0059(10) C7 0.0409(13) 0.0435(13) 0.0441(13) -0.0082(11) -0.0096(10) -0.0064(10) N1 0.0320(9) 0.0473(11) 0.0381(10) -0.0061(9) -0.0075(8) -0.0087(8) C8 0.0374(12) 0.0413(12) 0.0381(12) -0.0072(10) -0.0056(9) -0.0049(10) C9 0.0473(14) 0.0644(17) 0.0430(14) -0.0075(13) -0.0136(11) -0.0019(13) C10 0.0657(18) 0.0626(18) 0.0407(14) -0.0008(13) -0.0094(13) -0.0023(14) C11 0.0682(19) 0.0548(16) 0.0428(15) -0.0046(12) 0.0089(13) -0.0127(14) C12 0.0496(14) 0.0544(16) 0.0484(15) -0.0116(12) 0.0022(12) -0.0150(12) C13 0.0373(12) 0.0388(12) 0.0407(12) -0.0080(10) -0.0053(9) -0.0055(9) N2 0.0415(11) 0.0420(11) 0.0447(12) -0.0018(9) -0.0124(9) -0.0133(9) S1 0.0419(3) 0.0539(4) 0.0507(4) -0.0057(3) -0.0167(3) -0.0174(3) O2 0.0543(11) 0.0700(13) 0.0574(12) -0.0031(10) -0.0320(9) -0.0105(10) O3 0.0514(11) 0.0638(12) 0.0734(14) -0.0076(11) -0.0104(10) -0.0301(10) C14 0.0507(14) 0.0438(13) 0.0430(13) -0.0076(11) -0.0160(11) -0.0159(11) C15 0.0580(16) 0.0486(15) 0.0475(15) -0.0014(12) -0.0103(12) -0.0186(12) C16 0.0719(19) 0.0437(15) 0.0482(15) 0.0056(12) -0.0143(13) -0.0145(13) C17 0.0601(16) 0.0433(14) 0.0457(14) -0.0027(11) -0.0167(12) -0.0072(12) C18 0.0537(14) 0.0417(13) 0.0322(11) -0.0058(10) -0.0154(10) -0.0124(11) C23 0.0521(14) 0.0423(13) 0.0358(12) -0.0057(10) -0.0166(10) -0.0136(11) C19 0.0572(15) 0.0505(14) 0.0343(12) -0.0100(11) -0.0140(11) -0.0136(12) C20 0.0667(18) 0.0543(16) 0.0365(13) 0.0000(12) -0.0060(12) -0.0219(14) C21 0.0697(18) 0.0429(14) 0.0467(15) 0.0054(12) -0.0157(13) -0.0141(13) C22 0.0574(16) 0.0434(14) 0.0462(14) -0.0002(11) -0.0173(12) -0.0079(12) N3 0.0599(14) 0.0545(13) 0.0452(12) -0.0123(10) -0.0040(10) -0.0124(11) C24 0.066(2) 0.088(2) 0.060(2) -0.0160(18) 0.0071(16) -0.0208(18) C25 0.095(3) 0.063(2) 0.079(2) -0.0313(18) 0.001(2) -0.0157(19) O4 0.0440(10) 0.0443(10) 0.0823(15) -0.0133(10) -0.0177(10) -0.0042(8) C26 0.0362(12) 0.0449(14) 0.0514(15) -0.0020(11) -0.0060(11) -0.0089(10) C27 0.0510(16) 0.0605(18) 0.0676(19) -0.0053(15) -0.0148(14) -0.0174(14) C28 0.0481(16) 0.078(2) 0.079(2) 0.0025(18) -0.0198(15) -0.0222(15) C29 0.0356(15) 0.078(2) 0.095(3) -0.002(2) -0.0115(15) -0.0052(14) C30 0.0400(14) 0.0610(18) 0.087(2) -0.0156(17) -0.0034(14) -0.0027(13) C31 0.0366(12) 0.0468(14) 0.0530(15) -0.0036(12) -0.0010(11) -0.0078(11) C32 0.0441(14) 0.0465(14) 0.0580(16) -0.0140(12) -0.0008(12) -0.0101(11) N4 0.0396(11) 0.0480(12) 0.0452(12) -0.0069(9) -0.0049(9) -0.0115(9) C33 0.0529(14) 0.0434(13) 0.0403(13) -0.0060(11) -0.0078(11) -0.0143(11) C34 0.0701(19) 0.075(2) 0.0460(16) -0.0180(15) 0.0023(14) -0.0209(16) C35 0.103(3) 0.072(2) 0.0451(16) -0.0189(15) -0.0152(17) -0.0222(19) C36 0.094(3) 0.064(2) 0.0559(18) -0.0132(15) -0.0314(17) -0.0239(18) C37 0.0588(16) 0.0522(15) 0.0530(16) -0.0038(12) -0.0227(13) -0.0155(13) C38 0.0495(13) 0.0348(12) 0.0388(12) -0.0023(10) -0.0132(10) -0.0097(10) N5 0.0422(11) 0.0434(11) 0.0428(11) -0.0060(9) -0.0097(9) -0.0105(9) S2 0.0355(3) 0.0542(4) 0.0454(3) -0.0007(3) -0.0049(2) -0.0128(3) O5 0.0482(10) 0.0596(12) 0.0746(14) 0.0060(10) -0.0166(10) -0.0270(9) O6 0.0510(11) 0.0775(14) 0.0519(12) -0.0112(11) 0.0092(9) -0.0032(10) C39 0.0408(12) 0.0510(14) 0.0353(12) -0.0026(11) -0.0066(10) -0.0094(11) C40 0.0491(14) 0.0575(16) 0.0463(14) -0.0139(12) -0.0091(11) -0.0126(12) C41 0.0536(16) 0.0671(19) 0.0585(17) -0.0296(15) -0.0074(13) -0.0007(14) C42 0.0427(14) 0.0736(19) 0.0455(15) -0.0214(14) -0.0095(11) 0.0025(13) C43 0.0422(13) 0.0591(16) 0.0328(12) -0.0088(11) -0.0052(10) -0.0092(11) C44 0.0451(14) 0.0728(18) 0.0355(13) -0.0091(12) -0.0061(10) -0.0123(13) C45 0.069(2) 0.077(2) 0.0583(18) -0.0195(16) -0.0202(15) -0.0213(17) C46 0.085(2) 0.0612(19) 0.070(2) -0.0183(16) -0.0264(18) -0.0138(17) C47 0.0654(18) 0.0523(16) 0.0581(18) -0.0107(13) -0.0191(14) -0.0041(14) C48 0.0414(12) 0.0499(14) 0.0328(12) -0.0055(10) -0.0044(9) -0.0099(11) N6 0.0465(13) 0.098(2) 0.0491(14) -0.0209(14) -0.0158(11) -0.0085(13) C49 0.066(2) 0.093(3) 0.059(2) -0.0189(18) -0.0222(16) 0.0119(18) C50 0.059(2) 0.142(4) 0.078(2) -0.034(3) -0.0257(18) -0.022(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.362(3) . ? O1 H1O 0.890(18) . ? C1 C2 1.382(4) . ? C1 C6 1.403(3) . ? C2 C3 1.377(4) . ? C2 H2 0.93 . ? C3 C4 1.378(5) . ? C3 H3 0.93 . ? C4 C5 1.370(4) . ? C4 H4 0.93 . ? C5 C6 1.397(3) . ? C5 H5 0.93 . ? C6 C7 1.442(3) . ? C7 N1 1.287(3) . ? C7 H7 0.93 . ? N1 C8 1.416(3) . ? C8 C9 1.390(3) . ? C8 C13 1.394(3) . ? C9 C10 1.379(4) . ? C9 H9 0.93 . ? C10 C11 1.369(4) . ? C10 H10 0.93 . ? C11 C12 1.394(4) . ? C11 H11 0.93 . ? C12 C13 1.387(3) . ? C12 H12 0.93 . ? C13 N2 1.427(3) . ? N2 S1 1.637(2) . ? N2 H2N 0.851(17) . ? S1 O3 1.4274(19) . ? S1 O2 1.4317(19) . ? S1 C14 1.775(3) . ? C14 C15 1.382(3) . ? C14 C23 1.426(3) . ? C15 C16 1.409(4) . ? C15 H15 0.93 . ? C16 C17 1.359(4) . ? C16 H16 0.93 . ? C17 C18 1.421(3) . ? C17 H17 0.93 . ? C18 C19 1.432(4) . ? C18 C23 1.436(4) . ? C23 C22 1.418(3) . ? C19 C20 1.382(4) . ? C19 N3 1.416(4) . ? C20 C21 1.397(4) . ? C20 H20 0.93 . ? C21 C22 1.353(4) . ? C21 H21 0.93 . ? C22 H22 0.93 . ? N3 C24 1.451(4) . ? N3 C25 1.460(4) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? O4 C26 1.364(3) . ? O4 H4O 0.873(18) . ? C26 C27 1.390(4) . ? C26 C31 1.394(4) . ? C27 C28 1.367(4) . ? C27 H27 0.93 . ? C28 C29 1.379(5) . ? C28 H28 0.93 . ? C29 C30 1.370(5) . ? C29 H29 0.93 . ? C30 C31 1.399(4) . ? C30 H30 0.93 . ? C31 C32 1.450(4) . ? C32 N4 1.278(3) . ? C32 H32 0.93 . ? N4 C33 1.420(3) . ? C33 C38 1.391(3) . ? C33 C34 1.392(4) . ? C34 C35 1.381(5) . ? C34 H34 0.93 . ? C35 C36 1.382(5) . ? C35 H35 0.93 . ? C36 C37 1.373(4) . ? C36 H36 0.93 . ? C37 C38 1.385(3) . ? C37 H37 0.93 . ? C38 N5 1.438(3) . ? N5 S2 1.630(2) . ? N5 H5N 0.828(17) . ? S2 O6 1.428(2) . ? S2 O5 1.431(2) . ? S2 C39 1.781(3) . ? C39 C40 1.359(4) . ? C39 C48 1.428(3) . ? C40 C41 1.409(4) . ? C40 H40 0.93 . ? C41 C42 1.354(4) . ? C41 H41 0.93 . ? C42 C43 1.423(4) . ? C42 H42 0.93 . ? C43 C48 1.428(3) . ? C43 C44 1.430(4) . ? C44 C45 1.374(4) . ? C44 N6 1.418(4) . ? C45 C46 1.400(4) . ? C45 H45 0.93 . ? C46 C47 1.344(4) . ? C46 H46 0.93 . ? C47 C48 1.422(4) . ? C47 H47 0.93 . ? N6 C50 1.463(4) . ? N6 C49 1.468(4) . ? C49 H49A 0.96 . ? C49 H49B 0.96 . ? C49 H49C 0.96 . ? C50 H50A 0.96 . ? C50 H50B 0.96 . ? C50 H50C 0.96 . ? 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 C1 O1 H1O 108(2) . . ? O1 C1 C2 119.1(2) . . ? O1 C1 C6 121.0(2) . . ? C2 C1 C6 119.9(2) . . ? C3 C2 C1 119.8(3) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 121.2(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C5 C4 C3 119.3(3) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 118.6(2) . . ? C5 C6 C7 119.0(2) . . ? C1 C6 C7 122.3(2) . . ? N1 C7 C6 123.8(2) . . ? N1 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? C7 N1 C8 116.8(2) . . ? C9 C8 C13 119.1(2) . . ? C9 C8 N1 120.8(2) . . ? C13 C8 N1 120.1(2) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C11 C10 C9 119.4(3) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 120.5(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 120.0(3) . . ? C13 C12 H12 120 . . ? C11 C12 H12 120 . . ? C12 C13 C8 119.5(2) . . ? C12 C13 N2 119.7(2) . . ? C8 C13 N2 120.8(2) . . ? C13 N2 S1 118.98(17) . . ? C13 N2 H2N 119(2) . . ? S1 N2 H2N 111(2) . . ? O3 S1 O2 119.22(12) . . ? O3 S1 N2 107.55(12) . . ? O2 S1 N2 105.58(12) . . ? O3 S1 C14 107.29(13) . . ? O2 S1 C14 110.06(13) . . ? N2 S1 C14 106.45(11) . . ? C15 C14 C23 122.0(3) . . ? C15 C14 S1 115.4(2) . . ? C23 C14 S1 122.56(19) . . ? C14 C15 C16 119.6(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.3(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 121.9(3) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 121.2(2) . . ? C17 C18 C23 118.8(2) . . ? C19 C18 C23 120.0(2) . . ? C22 C23 C14 124.4(2) . . ? C22 C23 C18 118.2(2) . . ? C14 C23 C18 117.3(2) . . ? C20 C19 N3 122.8(3) . . ? C20 C19 C18 118.5(3) . . ? N3 C19 C18 118.6(2) . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C22 C21 C20 122.0(3) . . ? C22 C21 H21 119 . . ? C20 C21 H21 119 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C19 N3 C24 116.0(2) . . ? C19 N3 C25 115.7(2) . . ? C24 N3 C25 110.6(3) . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 O4 H4O 107(2) . . ? O4 C26 C27 118.8(3) . . ? O4 C26 C31 120.9(2) . . ? C27 C26 C31 120.3(3) . . ? C28 C27 C26 119.6(3) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 121.2(3) . . ? C27 C28 H28 119.4 . . ? C29 C28 H28 119.4 . . ? C30 C29 C28 119.4(3) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 121.1(3) . . ? C29 C30 H30 119.4 . . ? C31 C30 H30 119.4 . . ? C26 C31 C30 118.3(3) . . ? C26 C31 C32 122.0(2) . . ? C30 C31 C32 119.7(3) . . ? N4 C32 C31 123.1(3) . . ? N4 C32 H32 118.4 . . ? C31 C32 H32 118.4 . . ? C32 N4 C33 118.7(2) . . ? C38 C33 C34 118.5(3) . . ? C38 C33 N4 119.8(2) . . ? C34 C33 N4 121.6(3) . . ? C35 C34 C33 120.7(3) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 120.1(3) . . ? C34 C35 H35 120 . . ? C36 C35 H35 120 . . ? C37 C36 C35 119.7(3) . . ? C37 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C36 C37 C38 120.5(3) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C33 120.4(2) . . ? C37 C38 N5 118.2(2) . . ? C33 C38 N5 121.4(2) . . ? C38 N5 S2 119.35(17) . . ? C38 N5 H5N 117(2) . . ? S2 N5 H5N 114(2) . . ? O6 S2 O5 119.18(13) . . ? O6 S2 N5 106.30(12) . . ? O5 S2 N5 107.21(12) . . ? O6 S2 C39 110.62(13) . . ? O5 S2 C39 106.82(12) . . ? N5 S2 C39 105.95(11) . . ? C40 C39 C48 121.6(2) . . ? C40 C39 S2 115.4(2) . . ? C48 C39 S2 122.7(2) . . ? C39 C40 C41 120.7(3) . . ? C39 C40 H40 119.7 . . ? C41 C40 H40 119.7 . . ? C42 C41 C40 119.7(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C43 121.5(3) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C42 C43 C48 119.0(2) . . ? C42 C43 C44 120.7(2) . . ? C48 C43 C44 120.2(2) . . ? C45 C44 N6 123.2(3) . . ? C45 C44 C43 118.3(3) . . ? N6 C44 C43 118.5(3) . . ? C44 C45 C46 121.0(3) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C47 C46 C45 121.9(3) . . ? C47 C46 H46 119.1 . . ? C45 C46 H46 119.1 . . ? C46 C47 C48 120.4(3) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C47 C48 C39 124.7(2) . . ? C47 C48 C43 118.0(2) . . ? C39 C48 C43 117.2(2) . . ? C44 N6 C50 115.7(3) . . ? C44 N6 C49 114.6(3) . . ? C50 N6 C49 110.5(3) . . ? N6 C49 H49A 109.5 . . ? N6 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N6 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N6 C50 H50A 109.5 . . ? N6 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N6 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -177.6(3) . . . . ? C6 C1 C2 C3 1.0(4) . . . . ? C1 C2 C3 C4 -0.7(5) . . . . ? C2 C3 C4 C5 0.1(5) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C4 C5 C6 C7 176.8(3) . . . . ? O1 C1 C6 C5 177.8(2) . . . . ? C2 C1 C6 C5 -0.8(4) . . . . ? O1 C1 C6 C7 1.3(4) . . . . ? C2 C1 C6 C7 -177.3(2) . . . . ? C5 C6 C7 N1 -176.4(2) . . . . ? C1 C6 C7 N1 0.1(4) . . . . ? C6 C7 N1 C8 173.1(2) . . . . ? C7 N1 C8 C9 -44.5(3) . . . . ? C7 N1 C8 C13 136.5(2) . . . . ? C13 C8 C9 C10 -4.8(4) . . . . ? N1 C8 C9 C10 176.2(3) . . . . ? C8 C9 C10 C11 1.3(5) . . . . ? C9 C10 C11 C12 2.9(5) . . . . ? C10 C11 C12 C13 -3.4(4) . . . . ? C11 C12 C13 C8 -0.2(4) . . . . ? C11 C12 C13 N2 -178.9(2) . . . . ? C9 C8 C13 C12 4.2(4) . . . . ? N1 C8 C13 C12 -176.8(2) . . . . ? C9 C8 C13 N2 -177.2(2) . . . . ? N1 C8 C13 N2 1.8(4) . . . . ? C12 C13 N2 S1 71.9(3) . . . . ? C8 C13 N2 S1 -106.6(2) . . . . ? C13 N2 S1 O3 -54.6(2) . . . . ? C13 N2 S1 O2 177.07(18) . . . . ? C13 N2 S1 C14 60.1(2) . . . . ? O3 S1 C14 C15 16.5(2) . . . . ? O2 S1 C14 C15 147.6(2) . . . . ? N2 S1 C14 C15 -98.4(2) . . . . ? O3 S1 C14 C23 -166.5(2) . . . . ? O2 S1 C14 C23 -35.3(2) . . . . ? N2 S1 C14 C23 78.6(2) . . . . ? C23 C14 C15 C16 1.4(4) . . . . ? S1 C14 C15 C16 178.4(2) . . . . ? C14 C15 C16 C17 1.3(4) . . . . ? C15 C16 C17 C18 -1.3(4) . . . . ? C16 C17 C18 C19 -178.8(3) . . . . ? C16 C17 C18 C23 -1.5(4) . . . . ? C15 C14 C23 C22 172.6(2) . . . . ? S1 C14 C23 C22 -4.2(3) . . . . ? C15 C14 C23 C18 -4.0(3) . . . . ? S1 C14 C23 C18 179.16(17) . . . . ? C17 C18 C23 C22 -172.9(2) . . . . ? C19 C18 C23 C22 4.5(3) . . . . ? C17 C18 C23 C14 4.0(3) . . . . ? C19 C18 C23 C14 -178.7(2) . . . . ? C17 C18 C19 C20 172.2(2) . . . . ? C23 C18 C19 C20 -5.1(3) . . . . ? C17 C18 C19 N3 -4.4(3) . . . . ? C23 C18 C19 N3 178.3(2) . . . . ? N3 C19 C20 C21 178.6(2) . . . . ? C18 C19 C20 C21 2.2(4) . . . . ? C19 C20 C21 C22 1.3(4) . . . . ? C20 C21 C22 C23 -2.0(4) . . . . ? C14 C23 C22 C21 -177.6(2) . . . . ? C18 C23 C22 C21 -1.0(4) . . . . ? C20 C19 N3 C24 -20.2(4) . . . . ? C18 C19 N3 C24 156.2(3) . . . . ? C20 C19 N3 C25 111.8(3) . . . . ? C18 C19 N3 C25 -71.8(3) . . . . ? O4 C26 C27 C28 -179.4(3) . . . . ? C31 C26 C27 C28 0.4(4) . . . . ? C26 C27 C28 C29 0.8(5) . . . . ? C27 C28 C29 C30 -1.8(5) . . . . ? C28 C29 C30 C31 1.6(5) . . . . ? O4 C26 C31 C30 179.2(3) . . . . ? C27 C26 C31 C30 -0.6(4) . . . . ? O4 C26 C31 C32 -1.7(4) . . . . ? C27 C26 C31 C32 178.5(3) . . . . ? C29 C30 C31 C26 -0.4(5) . . . . ? C29 C30 C31 C32 -179.6(3) . . . . ? C26 C31 C32 N4 5.5(4) . . . . ? C30 C31 C32 N4 -175.4(3) . . . . ? C31 C32 N4 C33 -174.9(2) . . . . ? C32 N4 C33 C38 -137.4(3) . . . . ? C32 N4 C33 C34 44.8(4) . . . . ? C38 C33 C34 C35 0.4(5) . . . . ? N4 C33 C34 C35 178.3(3) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C34 C35 C36 C37 -0.3(5) . . . . ? C35 C36 C37 C38 1.0(5) . . . . ? C36 C37 C38 C33 -1.0(4) . . . . ? C36 C37 C38 N5 -179.8(2) . . . . ? C34 C33 C38 C37 0.3(4) . . . . ? N4 C33 C38 C37 -177.6(2) . . . . ? C34 C33 C38 N5 179.0(2) . . . . ? N4 C33 C38 N5 1.1(4) . . . . ? C37 C38 N5 S2 -78.4(3) . . . . ? C33 C38 N5 S2 102.9(2) . . . . ? C38 N5 S2 O6 173.84(18) . . . . ? C38 N5 S2 O5 45.4(2) . . . . ? C38 N5 S2 C39 -68.4(2) . . . . ? O6 S2 C39 C40 -149.9(2) . . . . ? O5 S2 C39 C40 -18.7(2) . . . . ? N5 S2 C39 C40 95.3(2) . . . . ? O6 S2 C39 C48 35.1(2) . . . . ? O5 S2 C39 C48 166.2(2) . . . . ? N5 S2 C39 C48 -79.7(2) . . . . ? C48 C39 C40 C41 1.3(4) . . . . ? S2 C39 C40 C41 -173.8(2) . . . . ? C39 C40 C41 C42 -2.7(5) . . . . ? C40 C41 C42 C43 -0.4(5) . . . . ? C41 C42 C43 C48 4.8(4) . . . . ? C41 C42 C43 C44 -178.4(3) . . . . ? C42 C43 C44 C45 -170.4(3) . . . . ? C48 C43 C44 C45 6.4(4) . . . . ? C42 C43 C44 N6 9.0(4) . . . . ? C48 C43 C44 N6 -174.2(2) . . . . ? N6 C44 C45 C46 176.8(3) . . . . ? C43 C44 C45 C46 -3.8(4) . . . . ? C44 C45 C46 C47 -0.8(5) . . . . ? C45 C46 C47 C48 2.9(5) . . . . ? C46 C47 C48 C39 178.0(3) . . . . ? C46 C47 C48 C43 -0.2(4) . . . . ? C40 C39 C48 C47 -175.3(3) . . . . ? S2 C39 C48 C47 -0.5(4) . . . . ? C40 C39 C48 C43 3.0(4) . . . . ? S2 C39 C48 C43 177.74(18) . . . . ? C42 C43 C48 C47 172.4(2) . . . . ? C44 C43 C48 C47 -4.4(4) . . . . ? C42 C43 C48 C39 -5.9(3) . . . . ? C44 C43 C48 C39 177.2(2) . . . . ? C45 C44 N6 C50 17.4(4) . . . . ? C43 C44 N6 C50 -162.0(3) . . . . ? C45 C44 N6 C49 -113.1(3) . . . . ? C43 C44 N6 C49 67.5(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 O4 H4O N4 0.873(18) 1.84(2) 2.629(3) 150(3) . O1 H1O N1 0.890(18) 1.86(2) 2.652(3) 148(3) . N2 H2N O4 0.851(17) 2.129(19) 2.951(3) 162(3) 2_656 N5 H5N O1 0.828(17) 2.130(18) 2.931(3) 163(3) 2_656 # END of CIF # Attachment '- 6.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-03-01 at 12:55:27 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : 2003be17 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_NiOH _database_code_depnum_ccdc_archive 'CCDC 877817' #TrackingRef '- 6.cif' _audit_creation_date 2012-03-01T12:55:27-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H27 N3 Ni O6 S, C4 H10 O, H2 O' _chemical_formula_sum 'C29 H39 N3 Ni O8 S' _chemical_formula_weight 648.4 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3061(11) _cell_length_b 11.4223(19) _cell_length_c 12.998(3) _cell_angle_alpha 67.060(14) _cell_angle_beta 80.500(10) _cell_angle_gamma 77.410(8) _cell_volume 1502.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.83 _cell_measurement_theta_max 45.14 _cell_measurement_wavelength 1.54184 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_correction_type psi-scan _exptl_absorpt_coefficient_mu 2.038 _exptl_absorpt_factor_muR 0.107 _exptl_absorpt_process_details ; North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351 Number of psi-scan sets used was 7 Theta correction was applied. Weighted transmission curves were used. No Fourier smoothing was applied. ; _exptl_absorpt_correction_T_min 0.6872 _exptl_absorpt_correction_T_max 0.8850 _exptl_absorpt_correction_T_ave 0.8104 _exptl_absorpt_Rmerge_before 0.0421 _exptl_absorpt_Rmerge_after 0.0421 _exptl_absorpt_theta_corr_max 1.0000 _exptl_absorpt_theta_corr_min 0.9967 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_type Cuk\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_wavelength 1.54184 _diffrn_source 'Enraf Nonius FR590' _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius TurboCAD4' _diffrn_measurement_method 'non-profiled omega/2theta scans' _diffrn_standards_number 3 _diffrn_reflns_av_R_equivalents 0.054 _diffrn_reflns_av_unetI/netI 0.0282 _diffrn_reflns_number 6363 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 73.42 _diffrn_reflns_theta_full 73.42 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6038 _reflns_number_gt 4945 _reflns_threshold_expression >2\s(I) loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 1 -4 0 3 3 -3 -1 -2 _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 5 _diffrn_standards_decay_corr_max 1.061 _diffrn_standards_decay_corr_min 0.979 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_UB_11 0.010432 _diffrn_orient_matrix_UB_12 0.016494 _diffrn_orient_matrix_UB_13 -0.082110 _diffrn_orient_matrix_UB_21 -0.031587 _diffrn_orient_matrix_UB_22 0.093776 _diffrn_orient_matrix_UB_23 -0.016586 _diffrn_orient_matrix_UB_31 0.084693 _diffrn_orient_matrix_UB_32 0.015424 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'DIRDIF-99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.1305P)^2^+0.3017P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 6038 _refine_ls_number_parameters 407 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0741 _refine_ls_R_factor_gt 0.0592 _refine_ls_wR_factor_ref 0.1685 _refine_ls_wR_factor_gt 0.1558 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.998 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.11 _iucr_refine_instructions_details ; TITL NiOH CELL 1.54184 11.3061 11.4223 12.9980 67.060 80.500 77.410 ZERR 2.00 0.0011 0.0019 0.0030 0.014 0.010 0.008 LATT 1 SFAC C H N NI O S UNIT 58 78 6 2 16 2 MERG 2 DFIX 0.820 0.020 O4 H4A DFIX 0.820 0.050 O4 H4B DFIX 0.820 0.020 O5 H5A DFIX 0.820 0.020 O6 H6A DFIX 0.820 0.020 O6 H6B DFIX 0.820 0.020 O8 H8A DFIX 0.820 0.020 O8 H8B EQIV $2 2-x, 2-y, 1-z EQIV $3 1+x, y, z EQIV $4 x, 1+y, z EQIV $5 2-x, 1-y, 2-z HTAB O4 O1_$2 HTAB O4 O3 HTAB O5 N3_$3 HTAB O5 O8 HTAB O6 O1_$2 HTAB O6 O7_$4 HTAB O8 O2 HTAB O8 O2_$5 HTAB O8 O3_$5 DFIX 2.150 0.020 H5A O8 OMIT -5 1 0 OMIT 1 2 5 OMIT 3 0 0 OMIT -3 2 12 OMIT 1 -4 1 OMIT 0 1 0 FMAP 2 PLAN 5 SIZE 0.06 0.32 0.80 ACTA HTAB 2.00000 BOND $H CONF LIST 4 WPDB -2 L.S. 14 TEMP 20.00 WGHT 0.130500 0.301700 FVAR 1.78145 NI1 4 0.985259 0.924931 0.705796 11.00000 0.02987 0.03529 = 0.03022 -0.01485 0.00274 -0.01233 O1 5 1.107358 1.016469 0.589577 11.00000 0.04426 0.05847 = 0.03600 -0.02426 0.00809 -0.02803 C1 1 1.169115 1.095941 0.600702 11.00000 0.03157 0.03980 = 0.03369 -0.01073 -0.00030 -0.01484 C2 1 1.259695 1.143832 0.515313 11.00000 0.03918 0.06183 = 0.04136 -0.01918 0.00632 -0.02292 AFIX 43 H2 2 1.275886 1.115595 0.455492 11.00000 -1.20000 AFIX 0 C3 1 1.325040 1.230966 0.517389 11.00000 0.04123 0.05694 = 0.05241 -0.01181 0.00642 -0.02517 AFIX 43 H3 2 1.383331 1.261660 0.458742 11.00000 -1.20000 AFIX 0 C4 1 1.304950 1.273529 0.605955 11.00000 0.04580 0.04587 = 0.06832 -0.01615 0.00088 -0.02705 AFIX 43 H4 2 1.349673 1.332031 0.607625 11.00000 -1.20000 AFIX 0 C5 1 1.217466 1.227689 0.691688 11.00000 0.04626 0.04567 = 0.05451 -0.02097 -0.00225 -0.02144 AFIX 43 H5 2 1.204308 1.255454 0.751690 11.00000 -1.20000 AFIX 0 C6 1 1.147436 1.140003 0.691011 11.00000 0.03457 0.03493 = 0.03560 -0.01067 -0.00327 -0.01227 C7 1 1.052635 1.107385 0.782830 11.00000 0.04097 0.03492 = 0.03549 -0.01708 -0.00077 -0.01160 AFIX 43 H7 2 1.048833 1.141117 0.838106 11.00000 -1.20000 AFIX 0 N1 3 0.973937 1.036604 0.794705 11.00000 0.03022 0.03350 = 0.03012 -0.01166 -0.00018 -0.00909 C8 1 0.878473 1.019371 0.882818 11.00000 0.03250 0.03733 = 0.02791 -0.01313 -0.00015 -0.00554 C9 1 0.843739 1.098558 0.945255 11.00000 0.04365 0.04561 = 0.04202 -0.02218 0.00004 -0.00864 AFIX 43 H9 2 0.886778 1.164268 0.932812 11.00000 -1.20000 AFIX 0 C10 1 0.745446 1.079955 1.025769 11.00000 0.05023 0.06048 = 0.03784 -0.02744 0.00274 -0.00193 AFIX 43 H10 2 0.723414 1.132006 1.068174 11.00000 -1.20000 AFIX 0 C11 1 0.680443 0.983847 1.042706 11.00000 0.04178 0.07357 = 0.03673 -0.02554 0.01109 -0.00980 AFIX 43 H11 2 0.613771 0.972360 1.095978 11.00000 -1.20000 AFIX 0 C12 1 0.713208 0.904097 0.981323 11.00000 0.04034 0.05658 = 0.03579 -0.01672 0.00830 -0.01594 AFIX 43 H12 2 0.668357 0.839788 0.993891 11.00000 -1.20000 AFIX 0 C13 1 0.813425 0.919624 0.900448 11.00000 0.03008 0.03878 = 0.02782 -0.01149 -0.00053 -0.00748 N2 3 0.853713 0.845736 0.831899 11.00000 0.02852 0.03573 = 0.03255 -0.01240 0.00180 -0.01069 S1 6 0.806290 0.716899 0.857413 11.00000 0.02619 0.03151 = 0.03652 -0.00715 -0.00317 -0.00948 O2 5 0.797618 0.638723 0.976294 11.00000 0.04783 0.04922 = 0.03822 0.00366 -0.01305 -0.02061 O3 5 0.882747 0.650123 0.789266 11.00000 0.03006 0.03598 = 0.06285 -0.02282 0.00323 -0.00739 C14 1 0.657454 0.754527 0.811998 11.00000 0.02577 0.03266 = 0.03185 -0.01005 0.00093 -0.00959 C15 1 0.611019 0.880962 0.758272 11.00000 0.03278 0.03077 = 0.04091 -0.00977 -0.00343 -0.01029 AFIX 43 H15 2 0.656510 0.944147 0.747605 11.00000 -1.20000 AFIX 0 C16 1 0.494789 0.917040 0.718684 11.00000 0.03516 0.02941 = 0.04847 -0.00975 -0.00460 -0.00454 AFIX 43 H16 2 0.461728 1.003793 0.686001 11.00000 -1.20000 AFIX 0 C17 1 0.430664 0.823846 0.728519 11.00000 0.02631 0.03387 = 0.04196 -0.01033 -0.00293 -0.00482 AFIX 43 H17 2 0.354495 0.848251 0.701165 11.00000 -1.20000 AFIX 0 C18 1 0.477924 0.691167 0.779450 11.00000 0.02658 0.03298 = 0.02961 -0.01123 0.00319 -0.00890 C19 1 0.412692 0.592974 0.786835 11.00000 0.02883 0.03565 = 0.03169 -0.01364 0.00138 -0.00999 N3 3 0.305431 0.631537 0.728757 11.00000 0.03086 0.04080 = 0.03648 -0.01229 -0.00323 -0.01181 C20 1 0.454572 0.466331 0.849281 11.00000 0.03765 0.03350 = 0.04677 -0.01457 -0.00010 -0.01204 AFIX 43 H20 2 0.409769 0.403059 0.858567 11.00000 -1.20000 AFIX 0 C21 1 0.564917 0.431496 0.899404 11.00000 0.04028 0.02882 = 0.04670 -0.00927 -0.00319 -0.00589 AFIX 43 H21 2 0.591115 0.345482 0.942368 11.00000 -1.20000 AFIX 0 C22 1 0.633691 0.520923 0.886238 11.00000 0.03077 0.03322 = 0.04224 -0.00929 -0.00397 -0.00575 AFIX 43 H22 2 0.708394 0.495249 0.916414 11.00000 -1.20000 AFIX 0 C23 1 0.591697 0.653589 0.826452 11.00000 0.02579 0.03061 = 0.03208 -0.01170 0.00105 -0.00721 C24 1 0.228150 0.532530 0.760540 11.00000 0.04373 0.04881 = 0.05975 -0.01536 -0.01185 -0.01890 AFIX 137 H24A 2 0.270556 0.462816 0.737798 11.00000 -1.50000 H24B 2 0.154198 0.569539 0.724192 11.00000 -1.50000 H24C 2 0.209220 0.500570 0.840387 11.00000 -1.50000 AFIX 0 C25 1 0.332246 0.680171 0.605791 11.00000 0.05606 0.07146 = 0.03807 -0.01736 -0.00532 -0.01815 AFIX 137 H25A 2 0.372655 0.753269 0.582687 11.00000 -1.50000 H25B 2 0.257630 0.705426 0.570676 11.00000 -1.50000 H25C 2 0.383903 0.613464 0.583993 11.00000 -1.50000 AFIX 0 C26 1 0.894914 0.444060 0.653405 11.00000 0.10194 0.08142 = 0.09849 -0.04384 -0.00641 -0.02999 AFIX 137 H26A 2 0.822933 0.498306 0.670290 11.00000 -1.50000 H26B 2 0.957807 0.494803 0.616617 11.00000 -1.50000 H26C 2 0.921764 0.377354 0.721702 11.00000 -1.50000 AFIX 0 C27 1 0.867270 0.384485 0.578095 11.00000 0.08718 0.06075 = 0.06827 -0.02684 0.00085 -0.01716 AFIX 23 H27A 2 0.828295 0.452218 0.515031 11.00000 -1.20000 H27B 2 0.943361 0.345561 0.548703 11.00000 -1.20000 AFIX 0 O7 5 0.791354 0.289316 0.630126 11.00000 0.07444 0.05038 = 0.05903 -0.02629 -0.00598 -0.00408 C28 1 0.672479 0.336954 0.667402 11.00000 0.07823 0.06186 = 0.07861 -0.03845 -0.00161 0.00063 AFIX 23 H28A 2 0.632314 0.403673 0.604535 11.00000 -1.20000 H28B 2 0.676809 0.374234 0.721888 11.00000 -1.20000 AFIX 0 C29 1 0.602400 0.229155 0.719116 11.00000 0.06851 0.07794 = 0.09519 -0.04460 -0.00941 -0.00607 AFIX 137 H29A 2 0.594656 0.195749 0.663706 11.00000 -1.50000 H29B 2 0.522977 0.259899 0.747679 11.00000 -1.50000 H29C 2 0.644210 0.162046 0.779435 11.00000 -1.50000 AFIX 0 O4 5 1.001563 0.808595 0.611678 11.00000 0.04144 0.04485 = 0.03885 -0.01968 -0.00062 -0.01360 H4A 2 0.968676 0.852208 0.553542 11.00000 -1.20000 H4B 2 0.972232 0.745589 0.645794 11.00000 -1.20000 O5 5 1.122101 0.796298 0.806179 11.00000 0.03221 0.04960 = 0.04595 -0.02165 -0.00171 -0.00372 H5A 2 1.102811 0.744562 0.868228 11.00000 -1.20000 H5B 2 1.184407 0.744279 0.781070 11.00000 -1.20000 O6 5 0.843118 1.049406 0.604603 11.00000 0.04309 0.03913 = 0.03393 -0.01235 -0.00247 -0.00761 H6A 2 0.832627 1.124978 0.597936 11.00000 -1.20000 H6B 2 0.842530 1.055036 0.541761 11.00000 -1.20000 O8 5 1.035857 0.641400 1.039367 11.00000 0.05951 0.05744 = 0.09689 -0.00915 -0.03160 -0.01452 H8A 2 0.966716 0.641136 1.029708 11.00000 -1.20000 H8B 2 1.069508 0.566656 1.056171 11.00000 -1.20000 HKLF 4 REM XYZN file = SHELXL INS file, from DIRDIF output for 2003BE REM R1 = 0.0592 for 4945 Fo > 4sig(Fo) and 0.0741 for all 6038 data REM 407 parameters refined using 8 restraints END WGHT 0.1307 0.1781 REM Highest difference peak 0.998, deepest hole -1.047, 1-sigma level 0.110 Q1 1 0.9744 0.8351 0.7297 11.00000 0.05 1.00 Q2 1 0.9879 1.0191 0.6768 11.00000 0.05 1.00 Q3 1 0.8289 0.7944 0.8362 11.00000 0.05 0.89 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.98526(4) 0.92493(4) 0.70580(3) 0.03046(15) Uani 1 1 d . . . O1 O 1.10736(18) 1.0165(2) 0.58958(16) 0.0423(5) Uani 1 1 d . . . C1 C 1.1691(2) 1.0959(3) 0.6007(2) 0.0348(5) Uani 1 1 d . . . C2 C 1.2597(3) 1.1438(3) 0.5153(3) 0.0462(7) Uani 1 1 d . . . H2 H 1.2759 1.1156 0.4555 0.055 Uiso 1 1 calc R . . C3 C 1.3250(3) 1.2310(3) 0.5174(3) 0.0513(7) Uani 1 1 d . . . H3 H 1.3833 1.2617 0.4587 0.062 Uiso 1 1 calc R . . C4 C 1.3049(3) 1.2735(3) 0.6060(3) 0.0524(8) Uani 1 1 d . . . H4 H 1.3497 1.332 0.6076 0.063 Uiso 1 1 calc R . . C5 C 1.2175(3) 1.2277(3) 0.6917(3) 0.0460(7) Uani 1 1 d . . . H5 H 1.2043 1.2555 0.7517 0.055 Uiso 1 1 calc R . . C6 C 1.1474(2) 1.1400(2) 0.6910(2) 0.0347(5) Uani 1 1 d . . . C7 C 1.0526(2) 1.1074(2) 0.7828(2) 0.0353(5) Uani 1 1 d . . . H7 H 1.0488 1.1411 0.8381 0.042 Uiso 1 1 calc R . . N1 N 0.97394(19) 1.0366(2) 0.79470(17) 0.0310(4) Uani 1 1 d . . . C8 C 0.8785(2) 1.0194(2) 0.8828(2) 0.0326(5) Uani 1 1 d . . . C9 C 0.8437(3) 1.0986(3) 0.9453(2) 0.0422(6) Uani 1 1 d . . . H9 H 0.8868 1.1643 0.9328 0.051 Uiso 1 1 calc R . . C10 C 0.7454(3) 1.0800(3) 1.0258(2) 0.0486(7) Uani 1 1 d . . . H10 H 0.7234 1.132 1.0682 0.058 Uiso 1 1 calc R . . C11 C 0.6804(3) 0.9838(4) 1.0427(2) 0.0508(7) Uani 1 1 d . . . H11 H 0.6138 0.9724 1.096 0.061 Uiso 1 1 calc R . . C12 C 0.7132(3) 0.9041(3) 0.9813(2) 0.0445(6) Uani 1 1 d . . . H12 H 0.6684 0.8398 0.9939 0.053 Uiso 1 1 calc R . . C13 C 0.8134(2) 0.9196(2) 0.9004(2) 0.0324(5) Uani 1 1 d . . . N2 N 0.85371(18) 0.8457(2) 0.83190(17) 0.0320(4) Uani 1 1 d . . . S1 S 0.80629(5) 0.71690(6) 0.85741(5) 0.03227(17) Uani 1 1 d . . . O2 O 0.79762(19) 0.6387(2) 0.97629(17) 0.0481(5) Uani 1 1 d . . . O3 O 0.88275(17) 0.65012(18) 0.78927(19) 0.0421(4) Uani 1 1 d . . . C14 C 0.6575(2) 0.7545(2) 0.8120(2) 0.0303(5) Uani 1 1 d . . . C15 C 0.6110(2) 0.8810(2) 0.7583(2) 0.0351(5) Uani 1 1 d . . . H15 H 0.6565 0.9441 0.7476 0.042 Uiso 1 1 calc R . . C16 C 0.4948(2) 0.9170(2) 0.7187(2) 0.0391(6) Uani 1 1 d . . . H16 H 0.4617 1.0038 0.686 0.047 Uiso 1 1 calc R . . C17 C 0.4307(2) 0.8238(2) 0.7285(2) 0.0352(5) Uani 1 1 d . . . H17 H 0.3545 0.8483 0.7012 0.042 Uiso 1 1 calc R . . C18 C 0.4779(2) 0.6912(2) 0.77945(19) 0.0299(5) Uani 1 1 d . . . C19 C 0.4127(2) 0.5930(2) 0.7868(2) 0.0314(5) Uani 1 1 d . . . N3 N 0.3054(2) 0.6315(2) 0.72876(18) 0.0357(5) Uani 1 1 d . . . C20 C 0.4546(2) 0.4663(3) 0.8493(2) 0.0388(6) Uani 1 1 d . . . H20 H 0.4098 0.4031 0.8586 0.047 Uiso 1 1 calc R . . C21 C 0.5649(3) 0.4315(3) 0.8994(2) 0.0401(6) Uani 1 1 d . . . H21 H 0.5911 0.3455 0.9424 0.048 Uiso 1 1 calc R . . C22 C 0.6337(2) 0.5209(2) 0.8862(2) 0.0367(5) Uani 1 1 d . . . H22 H 0.7084 0.4952 0.9164 0.044 Uiso 1 1 calc R . . C23 C 0.5917(2) 0.6536(2) 0.8265(2) 0.0295(5) Uani 1 1 d . . . C24 C 0.2281(3) 0.5325(3) 0.7605(3) 0.0495(7) Uani 1 1 d . . . H24A H 0.2706 0.4628 0.7378 0.074 Uiso 1 1 calc R . . H24B H 0.1542 0.5695 0.7242 0.074 Uiso 1 1 calc R . . H24C H 0.2092 0.5006 0.8404 0.074 Uiso 1 1 calc R . . C25 C 0.3322(3) 0.6802(4) 0.6058(3) 0.0547(8) Uani 1 1 d . . . H25A H 0.3727 0.7533 0.5827 0.082 Uiso 1 1 calc R . . H25B H 0.2576 0.7054 0.5707 0.082 Uiso 1 1 calc R . . H25C H 0.3839 0.6135 0.584 0.082 Uiso 1 1 calc R . . C26 C 0.8949(5) 0.4441(5) 0.6534(5) 0.0885(14) Uani 1 1 d . . . H26A H 0.8229 0.4983 0.6703 0.133 Uiso 1 1 calc R . . H26B H 0.9578 0.4948 0.6166 0.133 Uiso 1 1 calc R . . H26C H 0.9218 0.3774 0.7217 0.133 Uiso 1 1 calc R . . C27 C 0.8673(4) 0.3845(4) 0.5781(4) 0.0713(11) Uani 1 1 d . . . H27A H 0.8283 0.4522 0.515 0.086 Uiso 1 1 calc R . . H27B H 0.9434 0.3456 0.5487 0.086 Uiso 1 1 calc R . . O7 O 0.7914(3) 0.2893(2) 0.6301(2) 0.0604(6) Uani 1 1 d . . . C28 C 0.6725(4) 0.3370(4) 0.6674(4) 0.0717(11) Uani 1 1 d . . . H28A H 0.6323 0.4037 0.6045 0.086 Uiso 1 1 calc R . . H28B H 0.6768 0.3742 0.7219 0.086 Uiso 1 1 calc R . . C29 C 0.6024(4) 0.2292(5) 0.7191(4) 0.0773(12) Uani 1 1 d . . . H29A H 0.5947 0.1957 0.6637 0.116 Uiso 1 1 calc R . . H29B H 0.523 0.2599 0.7477 0.116 Uiso 1 1 calc R . . H29C H 0.6442 0.162 0.7794 0.116 Uiso 1 1 calc R . . O4 O 1.00156(19) 0.8086(2) 0.61168(17) 0.0397(4) Uani 1 1 d D . . H4A H 0.969(3) 0.852(3) 0.554(2) 0.048 Uiso 1 1 d D . . H4B H 0.972(3) 0.746(3) 0.646(3) 0.048 Uiso 1 1 d D . . O5 O 1.12210(18) 0.7963(2) 0.80618(18) 0.0421(4) Uani 1 1 d D . . H5A H 1.103(3) 0.745(3) 0.8682(16) 0.05 Uiso 1 1 d D . . H5B H 1.184(4) 0.744(4) 0.781(3) 0.05 Uiso 1 1 d . . . O6 O 0.84312(19) 1.04941(19) 0.60460(16) 0.0391(4) Uani 1 1 d D . . H6A H 0.833(3) 1.125(2) 0.598(3) 0.047 Uiso 1 1 d D . . H6B H 0.843(3) 1.055(3) 0.5418(18) 0.047 Uiso 1 1 d D . . O8 O 1.0359(3) 0.6414(3) 1.0394(3) 0.0735(8) Uani 1 1 d D . . H8A H 0.967(2) 0.641(5) 1.030(4) 0.088 Uiso 1 1 d D . . H8B H 1.070(4) 0.567(2) 1.056(4) 0.088 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0299(2) 0.0353(3) 0.0302(2) -0.01485(18) 0.00274(16) -0.01233(17) O1 0.0443(11) 0.0585(12) 0.0360(9) -0.0243(9) 0.0081(8) -0.0280(9) C1 0.0316(12) 0.0398(13) 0.0337(12) -0.0107(10) -0.0003(9) -0.0148(10) C2 0.0392(14) 0.0618(18) 0.0414(14) -0.0192(13) 0.0063(11) -0.0229(13) C3 0.0412(15) 0.0569(18) 0.0524(17) -0.0118(14) 0.0064(13) -0.0252(13) C4 0.0458(16) 0.0459(16) 0.068(2) -0.0162(15) 0.0009(14) -0.0271(13) C5 0.0463(16) 0.0457(15) 0.0545(17) -0.0210(13) -0.0022(13) -0.0214(13) C6 0.0346(12) 0.0349(12) 0.0356(12) -0.0107(10) -0.0033(10) -0.0123(10) C7 0.0410(13) 0.0349(12) 0.0355(12) -0.0171(10) -0.0008(10) -0.0116(10) N1 0.0302(10) 0.0335(10) 0.0301(9) -0.0117(8) -0.0002(8) -0.0091(8) C8 0.0325(12) 0.0373(12) 0.0279(11) -0.0131(9) -0.0001(9) -0.0055(9) C9 0.0437(15) 0.0456(15) 0.0420(14) -0.0222(12) 0.0000(11) -0.0086(12) C10 0.0502(17) 0.0605(18) 0.0378(14) -0.0274(13) 0.0027(12) -0.0019(14) C11 0.0418(15) 0.074(2) 0.0367(14) -0.0255(14) 0.0111(11) -0.0098(14) C12 0.0403(15) 0.0566(17) 0.0358(13) -0.0167(12) 0.0083(11) -0.0159(12) C13 0.0301(12) 0.0388(12) 0.0278(11) -0.0115(9) -0.0005(9) -0.0075(10) N2 0.0285(10) 0.0357(10) 0.0325(10) -0.0124(8) 0.0018(8) -0.0107(8) S1 0.0262(3) 0.0315(3) 0.0365(3) -0.0072(2) -0.0032(2) -0.0095(2) O2 0.0478(11) 0.0492(11) 0.0382(10) 0.0037(9) -0.0131(8) -0.0206(9) O3 0.0301(9) 0.0360(9) 0.0629(12) -0.0228(9) 0.0032(8) -0.0074(7) C14 0.0258(11) 0.0327(11) 0.0319(11) -0.0100(9) 0.0009(8) -0.0096(9) C15 0.0328(12) 0.0308(12) 0.0409(13) -0.0098(10) -0.0034(10) -0.0103(9) C16 0.0352(13) 0.0294(12) 0.0485(15) -0.0098(11) -0.0046(11) -0.0045(10) C17 0.0263(11) 0.0339(12) 0.0420(13) -0.0103(10) -0.0029(9) -0.0048(9) C18 0.0266(11) 0.0330(11) 0.0296(11) -0.0112(9) 0.0032(8) -0.0089(9) C19 0.0288(11) 0.0357(12) 0.0317(11) -0.0136(9) 0.0014(9) -0.0100(9) N3 0.0309(10) 0.0408(11) 0.0365(11) -0.0123(9) -0.0032(8) -0.0118(9) C20 0.0377(13) 0.0335(12) 0.0468(14) -0.0146(11) -0.0001(11) -0.0120(10) C21 0.0403(14) 0.0288(12) 0.0467(14) -0.0093(10) -0.0032(11) -0.0059(10) C22 0.0308(12) 0.0332(12) 0.0422(13) -0.0093(10) -0.0040(10) -0.0057(9) C23 0.0258(11) 0.0306(11) 0.0321(11) -0.0117(9) 0.0010(8) -0.0072(9) C24 0.0437(16) 0.0488(16) 0.0597(18) -0.0154(14) -0.0118(13) -0.0189(13) C25 0.0561(19) 0.071(2) 0.0381(15) -0.0174(14) -0.0053(13) -0.0182(16) C26 0.102(4) 0.081(3) 0.098(4) -0.044(3) -0.006(3) -0.030(3) C27 0.087(3) 0.061(2) 0.068(2) -0.0268(19) 0.001(2) -0.017(2) O7 0.0744(16) 0.0504(13) 0.0590(14) -0.0263(11) -0.0060(12) -0.0041(11) C28 0.078(3) 0.062(2) 0.079(3) -0.038(2) -0.002(2) 0.0006(19) C29 0.069(3) 0.078(3) 0.095(3) -0.045(2) -0.009(2) -0.006(2) O4 0.0414(10) 0.0448(11) 0.0388(10) -0.0197(8) -0.0006(8) -0.0136(8) O5 0.0322(9) 0.0496(11) 0.0460(11) -0.0216(9) -0.0017(8) -0.0037(8) O6 0.0431(10) 0.0391(10) 0.0339(9) -0.0123(8) -0.0025(8) -0.0076(8) O8 0.0595(16) 0.0574(15) 0.097(2) -0.0092(15) -0.0316(15) -0.0145(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.9976(19) . ? Ni1 N1 2.002(2) . ? Ni1 N2 2.084(2) . ? Ni1 O4 2.093(2) . ? Ni1 O5 2.106(2) . ? Ni1 O6 2.140(2) . ? O1 C1 1.321(3) . ? C1 C2 1.406(4) . ? C1 C6 1.415(4) . ? C2 C3 1.373(4) . ? C2 H2 0.93 . ? C3 C4 1.384(5) . ? C3 H3 0.93 . ? C4 C5 1.379(4) . ? C4 H4 0.93 . ? C5 C6 1.409(4) . ? C5 H5 0.93 . ? C6 C7 1.455(4) . ? C7 N1 1.281(3) . ? C7 H7 0.93 . ? N1 C8 1.423(3) . ? C8 C9 1.394(4) . ? C8 C13 1.413(3) . ? C9 C10 1.386(4) . ? C9 H9 0.93 . ? C10 C11 1.380(5) . ? C10 H10 0.93 . ? C11 C12 1.388(4) . ? C11 H11 0.93 . ? C12 C13 1.403(3) . ? C12 H12 0.93 . ? C13 N2 1.414(3) . ? N2 S1 1.571(2) . ? S1 O3 1.449(2) . ? S1 O2 1.452(2) . ? S1 C14 1.783(2) . ? C14 C15 1.361(3) . ? C14 C23 1.441(3) . ? C15 C16 1.408(4) . ? C15 H15 0.93 . ? C16 C17 1.369(4) . ? C16 H16 0.93 . ? C17 C18 1.415(3) . ? C17 H17 0.93 . ? C18 C23 1.424(3) . ? C18 C19 1.437(3) . ? C19 C20 1.374(4) . ? C19 N3 1.430(3) . ? N3 C24 1.470(3) . ? N3 C25 1.475(4) . ? C20 C21 1.410(4) . ? C20 H20 0.93 . ? C21 C22 1.358(4) . ? C21 H21 0.93 . ? C22 C23 1.420(3) . ? C22 H22 0.93 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? C26 C27 1.494(6) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 O7 1.421(5) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? O7 C28 1.417(5) . ? C28 C29 1.483(6) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? O4 H4A 0.822(18) . ? O4 H4B 0.79(3) . ? O5 H5A 0.821(14) . ? O5 H5B 0.92(4) . ? O6 H6A 0.817(18) . ? O6 H6B 0.795(18) . ? O8 H8A 0.813(19) . ? O8 H8B 0.814(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 N1 93.14(8) . . ? O1 Ni1 N2 174.15(8) . . ? N1 Ni1 N2 81.29(8) . . ? O1 Ni1 O4 85.69(8) . . ? N1 Ni1 O4 178.60(8) . . ? N2 Ni1 O4 99.90(8) . . ? O1 Ni1 O5 92.08(9) . . ? N1 Ni1 O5 87.81(9) . . ? N2 Ni1 O5 89.51(8) . . ? O4 Ni1 O5 91.48(8) . . ? O1 Ni1 O6 89.40(9) . . ? N1 Ni1 O6 93.74(8) . . ? N2 Ni1 O6 89.17(8) . . ? O4 Ni1 O6 87.01(8) . . ? O5 Ni1 O6 177.80(8) . . ? C1 O1 Ni1 124.92(16) . . ? O1 C1 C2 118.0(2) . . ? O1 C1 C6 124.4(2) . . ? C2 C1 C6 117.5(2) . . ? C3 C2 C1 122.1(3) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.8(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.9(3) . . ? C4 C5 H5 119 . . ? C6 C5 H5 119 . . ? C5 C6 C1 119.0(2) . . ? C5 C6 C7 115.7(2) . . ? C1 C6 C7 125.2(2) . . ? N1 C7 C6 126.1(2) . . ? N1 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? C7 N1 C8 121.7(2) . . ? C7 N1 Ni1 123.74(18) . . ? C8 N1 Ni1 114.18(16) . . ? C9 C8 C13 120.4(2) . . ? C9 C8 N1 123.8(2) . . ? C13 C8 N1 115.8(2) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C11 C10 C9 119.7(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 120.9(3) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C13 120.6(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 N2 125.5(2) . . ? C12 C13 C8 118.1(2) . . ? N2 C13 C8 116.5(2) . . ? C13 N2 S1 121.51(17) . . ? C13 N2 Ni1 111.38(15) . . ? S1 N2 Ni1 127.03(12) . . ? O3 S1 O2 113.55(13) . . ? O3 S1 N2 108.23(11) . . ? O2 S1 N2 112.46(12) . . ? O3 S1 C14 105.95(12) . . ? O2 S1 C14 107.26(11) . . ? N2 S1 C14 109.13(11) . . ? C15 C14 C23 121.3(2) . . ? C15 C14 S1 117.83(18) . . ? C23 C14 S1 120.78(18) . . ? C14 C15 C16 120.7(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 119.7 . . ? C17 C16 C15 119.7(2) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 121.3(2) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C23 119.4(2) . . ? C17 C18 C19 121.6(2) . . ? C23 C18 C19 119.0(2) . . ? C20 C19 N3 122.4(2) . . ? C20 C19 C18 119.3(2) . . ? N3 C19 C18 118.3(2) . . ? C19 N3 C24 115.2(2) . . ? C19 N3 C25 112.6(2) . . ? C24 N3 C25 108.5(2) . . ? C19 C20 C21 120.6(2) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C22 C21 C20 121.4(2) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22 120 . . ? C23 C22 H22 120 . . ? C22 C23 C18 119.3(2) . . ? C22 C23 C14 123.4(2) . . ? C18 C23 C14 117.3(2) . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 H26A 109.5 . . ? C27 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C27 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O7 C27 C26 114.7(4) . . ? O7 C27 H27A 108.6 . . ? C26 C27 H27A 108.6 . . ? O7 C27 H27B 108.6 . . ? C26 C27 H27B 108.6 . . ? H27A C27 H27B 107.6 . . ? C28 O7 C27 114.2(3) . . ? O7 C28 C29 109.0(3) . . ? O7 C28 H28A 109.9 . . ? C29 C28 H28A 109.9 . . ? O7 C28 H28B 109.9 . . ? C29 C28 H28B 109.9 . . ? H28A C28 H28B 108.3 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? Ni1 O4 H4A 108(2) . . ? Ni1 O4 H4B 112(3) . . ? H4A O4 H4B 111(4) . . ? Ni1 O5 H5A 119(3) . . ? Ni1 O5 H5B 123(2) . . ? H5A O5 H5B 100(3) . . ? Ni1 O6 H6A 115(3) . . ? Ni1 O6 H6B 121(3) . . ? H6A O6 H6B 102(4) . . ? H8A O8 H8B 105(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 N1 Ni1 O1 C1 14.3(2) . . . . ? O4 Ni1 O1 C1 -165.0(2) . . . . ? O5 Ni1 O1 C1 -73.7(2) . . . . ? O6 Ni1 O1 C1 108.0(2) . . . . ? Ni1 O1 C1 C2 174.4(2) . . . . ? Ni1 O1 C1 C6 -8.0(4) . . . . ? O1 C1 C2 C3 177.3(3) . . . . ? C6 C1 C2 C3 -0.5(5) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C4 C5 C6 C1 1.2(5) . . . . ? C4 C5 C6 C7 -175.7(3) . . . . ? O1 C1 C6 C5 -178.2(3) . . . . ? C2 C1 C6 C5 -0.6(4) . . . . ? O1 C1 C6 C7 -1.7(4) . . . . ? C2 C1 C6 C7 176.0(3) . . . . ? C5 C6 C7 N1 175.3(3) . . . . ? C1 C6 C7 N1 -1.3(5) . . . . ? C6 C7 N1 C8 -174.6(2) . . . . ? C6 C7 N1 Ni1 13.2(4) . . . . ? O1 Ni1 N1 C7 -16.7(2) . . . . ? N2 Ni1 N1 C7 165.1(2) . . . . ? O5 Ni1 N1 C7 75.3(2) . . . . ? O6 Ni1 N1 C7 -106.3(2) . . . . ? O1 Ni1 N1 C8 170.68(17) . . . . ? N2 Ni1 N1 C8 -7.52(17) . . . . ? O5 Ni1 N1 C8 -97.36(17) . . . . ? O6 Ni1 N1 C8 81.07(17) . . . . ? C7 N1 C8 C9 16.1(4) . . . . ? Ni1 N1 C8 C9 -171.1(2) . . . . ? C7 N1 C8 C13 -167.6(2) . . . . ? Ni1 N1 C8 C13 5.2(3) . . . . ? C13 C8 C9 C10 0.4(4) . . . . ? N1 C8 C9 C10 176.5(3) . . . . ? C8 C9 C10 C11 -1.1(5) . . . . ? C9 C10 C11 C12 1.0(5) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 N2 -178.9(3) . . . . ? C11 C12 C13 C8 -0.7(4) . . . . ? C9 C8 C13 C12 0.6(4) . . . . ? N1 C8 C13 C12 -175.8(2) . . . . ? C9 C8 C13 N2 178.9(2) . . . . ? N1 C8 C13 N2 2.4(3) . . . . ? C12 C13 N2 S1 -13.5(4) . . . . ? C8 C13 N2 S1 168.34(18) . . . . ? C12 C13 N2 Ni1 169.7(2) . . . . ? C8 C13 N2 Ni1 -8.4(3) . . . . ? N1 Ni1 N2 C13 8.62(16) . . . . ? O4 Ni1 N2 C13 -172.11(16) . . . . ? O5 Ni1 N2 C13 96.47(17) . . . . ? O6 Ni1 N2 C13 -85.30(17) . . . . ? N1 Ni1 N2 S1 -167.95(16) . . . . ? O4 Ni1 N2 S1 11.33(17) . . . . ? O5 Ni1 N2 S1 -80.09(15) . . . . ? O6 Ni1 N2 S1 98.14(15) . . . . ? C13 N2 S1 O3 -167.5(2) . . . . ? Ni1 N2 S1 O3 8.74(18) . . . . ? C13 N2 S1 O2 -41.2(2) . . . . ? Ni1 N2 S1 O2 135.00(15) . . . . ? C13 N2 S1 C14 77.6(2) . . . . ? Ni1 N2 S1 C14 -106.12(15) . . . . ? O3 S1 C14 C15 -112.4(2) . . . . ? O2 S1 C14 C15 126.0(2) . . . . ? N2 S1 C14 C15 4.0(2) . . . . ? O3 S1 C14 C23 64.3(2) . . . . ? O2 S1 C14 C23 -57.3(2) . . . . ? N2 S1 C14 C23 -179.37(18) . . . . ? C23 C14 C15 C16 2.3(4) . . . . ? S1 C14 C15 C16 179.0(2) . . . . ? C14 C15 C16 C17 -3.8(4) . . . . ? C15 C16 C17 C18 1.0(4) . . . . ? C16 C17 C18 C23 3.2(4) . . . . ? C16 C17 C18 C19 -178.0(2) . . . . ? C17 C18 C19 C20 -171.8(2) . . . . ? C23 C18 C19 C20 7.0(3) . . . . ? C17 C18 C19 N3 7.9(3) . . . . ? C23 C18 C19 N3 -173.3(2) . . . . ? C20 C19 N3 C24 13.4(4) . . . . ? C18 C19 N3 C24 -166.3(2) . . . . ? C20 C19 N3 C25 -111.8(3) . . . . ? C18 C19 N3 C25 68.6(3) . . . . ? N3 C19 C20 C21 176.0(2) . . . . ? C18 C19 C20 C21 -4.4(4) . . . . ? C19 C20 C21 C22 -1.0(4) . . . . ? C20 C21 C22 C23 3.7(4) . . . . ? C21 C22 C23 C18 -0.9(4) . . . . ? C21 C22 C23 C14 177.9(2) . . . . ? C17 C18 C23 C22 174.4(2) . . . . ? C19 C18 C23 C22 -4.4(3) . . . . ? C17 C18 C23 C14 -4.5(3) . . . . ? C19 C18 C23 C14 176.7(2) . . . . ? C15 C14 C23 C22 -177.0(2) . . . . ? S1 C14 C23 C22 6.4(3) . . . . ? C15 C14 C23 C18 1.8(3) . . . . ? S1 C14 C23 C18 -174.76(17) . . . . ? C26 C27 O7 C28 64.0(5) . . . . ? C27 O7 C28 C29 179.6(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4 H4A O1 0.822(18) 2.059(19) 2.875(3) 172(3) 2_776 O4 H4B O3 0.79(3) 1.99(3) 2.681(3) 145(4) . O5 H5B N3 0.92(4) 1.90(4) 2.817(3) 176(3) 1_655 O5 H5A O8 0.821(14) 2.168(14) 2.977(4) 169(3) . O6 H6B O1 0.795(18) 2.11(2) 2.843(3) 152(3) 2_776 O6 H6A O7 0.817(18) 2.02(2) 2.812(3) 163(4) 1_565 O8 H8A O2 0.813(19) 2.15(2) 2.952(3) 170(5) . O8 H8B O3 0.814(19) 2.52(3) 3.233(3) 147(5) 2_767 # END of CIF # Attachment '- 9.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-02-24 at 16:33:06 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : be20mj1n41 struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_CuSALDS _database_code_depnum_ccdc_archive 'CCDC 877819' #TrackingRef '- 9.cif' _audit_creation_date 2012-02-24T16:33:06-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H27 Cu N3 O4 S2, C H Cl3' _chemical_formula_sum 'C28 H28 Cl3 Cu N3 O4 S2' _chemical_formula_weight 704.54 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8609(11) _cell_length_b 11.5049(13) _cell_length_c 14.1875(16) _cell_angle_alpha 98.616(2) _cell_angle_beta 103.423(2) _cell_angle_gamma 94.643(2) _cell_volume 1536.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2987 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.39 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.73 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 722 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.8078 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\W scans' _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 29485 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.8 _diffrn_reflns_theta_max 26.43 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6269 _reflns_number_gt 4508 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'SMART (Bruker AXS)' _computing_cell_refinement 'SAINT+ (Bruker AXS)' _computing_data_reduction 'SAINT+ (Bruker AXS)' _computing_structure_solution 'DIRDIF96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0651P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6269 _refine_ls_number_parameters 390 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0645 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1165 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.55 _refine_diff_density_min -0.4 _refine_diff_density_rms 0.061 _iucr_refine_instructions_details ; TITL CuSALDS CELL 0.71073 9.8609 11.5049 14.1875 98.616 103.423 94.643 ZERR 2.00 0.0011 0.0013 0.0016 0.002 0.002 0.002 LATT 1 SFAC C H CU N O S CL UNIT 56 56 2 6 8 4 6 MERG 2 OMIT 6 2 3 OMIT 0 0 1 OMIT 8 4 1 OMIT -11 -3 10 OMIT 4 1 0 OMIT 1 4 2 OMIT -10 -2 13 OMIT -4 -4 4 OMIT -3 0 6 OMIT -3 -4 2 EADP S2 S2B EADP C26 C26B EADP C27 C27B EADP CL3 CL3B EADP CL1 CL1B EADP CL2 CL2B MORE 3 FMAP 2 PLAN 10 SIZE 0.13 0.22 0.73 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 10 TEMP 293.00 WGHT 0.065100 FVAR 0.50906 0.87273 CU1 3 0.168582 0.481933 0.328254 11.00000 0.03914 0.05049 = 0.03277 0.00858 0.01008 0.01497 O1 5 0.065126 0.605544 0.356811 11.00000 0.07099 0.06737 = 0.04906 0.02149 0.02526 0.03925 C1 1 0.054602 0.652742 0.445380 11.00000 0.04829 0.04409 = 0.06452 0.01454 0.02998 0.01590 C2 1 -0.040745 0.738312 0.451861 11.00000 0.06816 0.06017 = 0.08901 0.02714 0.04124 0.02911 AFIX 43 H2 2 -0.092567 0.759444 0.394690 11.00000 -1.20000 AFIX 0 C3 1 -0.057045 0.789975 0.541552 11.00000 0.07615 0.04837 = 0.10969 0.01293 0.05905 0.02353 AFIX 43 H3 2 -0.118269 0.847090 0.544144 11.00000 -1.20000 C4 1 0.014033 0.759696 0.626497 11.00000 0.06995 0.05806 = 0.07983 -0.01085 0.04225 0.00187 AFIX 43 H4 2 -0.000226 0.794217 0.686474 11.00000 -1.20000 AFIX 0 O4 5 0.027207 0.417023 0.204104 11.00000 0.04912 0.08973 = 0.04839 0.00706 -0.00450 0.01556 C5 1 0.107160 0.677715 0.623240 11.00000 0.06293 0.05167 = 0.05605 -0.00822 0.02969 -0.00011 AFIX 43 H5 2 0.156573 0.657986 0.681764 11.00000 -1.20000 AFIX 0 C6 1 0.129842 0.622767 0.533783 11.00000 0.04108 0.03724 = 0.04780 0.00072 0.02104 -0.00055 C7 1 0.228939 0.537975 0.539154 11.00000 0.03914 0.04335 = 0.03389 0.00070 0.00971 -0.00087 AFIX 43 H7 2 0.275611 0.526244 0.601307 11.00000 -1.20000 AFIX 0 N1 4 0.258193 0.476583 0.463868 11.00000 0.03516 0.03583 = 0.03255 0.00519 0.01151 0.00425 C8 1 0.356347 0.392340 0.472795 11.00000 0.03149 0.03916 = 0.03252 0.00402 0.00570 0.00333 C9 1 0.417267 0.353694 0.558594 11.00000 0.04678 0.05972 = 0.03464 0.00831 0.00718 0.01143 AFIX 43 H9 2 0.397030 0.385227 0.617360 11.00000 -1.20000 AFIX 0 C10 1 0.507832 0.268711 0.557645 11.00000 0.05585 0.06876 = 0.04806 0.02477 0.00450 0.02275 AFIX 43 H10 2 0.548649 0.243046 0.615659 11.00000 -1.20000 AFIX 0 C11 1 0.538004 0.221616 0.470457 11.00000 0.05328 0.05265 = 0.05964 0.01554 0.01237 0.02064 AFIX 43 H11 2 0.599025 0.164119 0.469823 11.00000 -1.20000 AFIX 0 C12 1 0.477683 0.259774 0.384142 11.00000 0.04334 0.04686 = 0.04326 0.00198 0.01106 0.01114 AFIX 43 H12 2 0.498061 0.227393 0.325643 11.00000 -1.20000 AFIX 0 C13 1 0.387326 0.345645 0.383992 11.00000 0.03032 0.03790 = 0.03558 0.00353 0.00606 0.00075 N2 4 0.315099 0.389046 0.300616 11.00000 0.03913 0.04814 = 0.02945 0.00481 0.01212 0.01040 S1 6 0.377579 0.398424 0.208225 11.00000 0.03589 0.03879 = 0.03302 0.00248 0.01114 0.00275 O2 5 0.312610 0.489206 0.161031 11.00000 0.06736 0.03947 = 0.04676 0.01053 0.02411 0.01313 O3 5 0.528706 0.409140 0.233321 11.00000 0.03576 0.06750 = 0.04138 -0.00408 0.01139 -0.00564 C14 1 0.318015 0.263490 0.122525 11.00000 0.02997 0.03642 = 0.03076 0.00645 0.00650 0.00545 C15 1 0.228853 0.179484 0.143572 11.00000 0.04359 0.05051 = 0.03550 0.00641 0.01516 -0.00211 AFIX 43 H15 2 0.203212 0.191320 0.203056 11.00000 -1.20000 AFIX 0 C16 1 0.176087 0.075110 0.074892 11.00000 0.04775 0.04832 = 0.05056 0.00721 0.01591 -0.01305 AFIX 43 H16 2 0.113822 0.018764 0.088687 11.00000 -1.20000 AFIX 0 C17 1 0.214848 0.055567 -0.011223 11.00000 0.04107 0.04031 = 0.04380 0.00259 0.00939 -0.00447 AFIX 43 H17 2 0.177547 -0.013654 -0.055944 11.00000 -1.20000 AFIX 0 C18 1 0.310944 0.138281 -0.034604 11.00000 0.02769 0.03861 = 0.03409 0.00455 0.00468 0.00471 C19 1 0.353817 0.117825 -0.124914 11.00000 0.03282 0.04624 = 0.03648 0.00115 0.00824 0.01159 C20 1 0.434046 0.206531 -0.148292 11.00000 0.04508 0.05828 = 0.04312 0.00527 0.02311 0.00654 AFIX 43 H20 2 0.457361 0.195616 -0.208616 11.00000 -1.20000 AFIX 0 C21 1 0.481580 0.313426 -0.082870 11.00000 0.04649 0.04998 = 0.05262 0.01152 0.02621 0.00060 AFIX 43 H21 2 0.536800 0.371976 -0.100334 11.00000 -1.20000 AFIX 0 C22 1 0.448968 0.333653 0.005495 11.00000 0.03926 0.03669 = 0.04379 0.00495 0.01579 0.00066 AFIX 43 H22 2 0.484181 0.404483 0.048600 11.00000 -1.20000 AFIX 0 C23 1 0.361221 0.246942 0.032290 11.00000 0.02803 0.03614 = 0.03229 0.00892 0.00806 0.00687 N3 4 0.307814 0.005988 -0.187655 11.00000 0.04314 0.05106 = 0.03868 -0.00657 0.00862 0.00881 C24 1 0.313381 0.003636 -0.289835 11.00000 0.06241 0.07823 = 0.04550 -0.01122 0.01878 0.00269 AFIX 137 H24A 2 0.265987 0.066496 -0.314812 11.00000 -1.50000 H24B 2 0.268232 -0.071043 -0.328591 11.00000 -1.50000 H24C 2 0.409584 0.013910 -0.293304 11.00000 -1.50000 AFIX 0 C25 1 0.378102 -0.090461 -0.149294 11.00000 0.09118 0.04988 = 0.06778 -0.00355 0.00905 0.02429 AFIX 137 H25A 2 0.473971 -0.082229 -0.153738 11.00000 -1.50000 H25B 2 0.330916 -0.164961 -0.187209 11.00000 -1.50000 H25C 2 0.375566 -0.087512 -0.081750 11.00000 -1.50000 AFIX 0 PART 1 S2 6 -0.037238 0.478500 0.124353 21.00000 0.05216 0.13036 = 0.07398 0.05637 -0.00935 -0.00756 C26 1 -0.129914 0.364182 0.029196 21.00000 0.13408 0.20964 = 0.05880 0.02374 -0.03839 -0.00620 AFIX 137 H26A 2 -0.066636 0.309976 0.012518 21.00000 -1.50000 H26B 2 -0.171077 0.397235 -0.027508 21.00000 -1.50000 H26C 2 -0.202656 0.322886 0.050596 21.00000 -1.50000 AFIX 0 C27 1 -0.187890 0.538987 0.155520 21.00000 0.06916 0.18454 = 0.21277 0.06620 -0.00262 0.06410 AFIX 137 H27A 2 -0.248437 0.477220 0.168880 21.00000 -1.50000 H27B 2 -0.238215 0.572136 0.101456 21.00000 -1.50000 H27C 2 -0.157036 0.599733 0.212777 21.00000 -1.50000 AFIX 0 PART 2 SAME S2 C26 C27 S2B 6 -0.100637 0.416554 0.168050 -21.00000 0.05216 0.13036 = 0.07398 0.05637 -0.00935 -0.00756 C26B 1 -0.149060 0.310414 0.059708 -21.00000 0.13408 0.20964 = 0.05880 0.02374 -0.03839 -0.00620 AFIX 33 H26D 2 -0.087624 0.249802 0.064741 -21.00000 -1.50000 H26E 2 -0.141951 0.347716 0.004595 -21.00000 -1.50000 H26F 2 -0.244074 0.275704 0.050564 -21.00000 -1.50000 AFIX 0 C27B 1 -0.139732 0.547831 0.116160 -21.00000 0.06916 0.18454 = 0.21277 0.06620 -0.00262 0.06410 AFIX 33 H27D 2 -0.224661 0.572594 0.130233 -21.00000 -1.50000 H27E 2 -0.151526 0.530616 0.046204 -21.00000 -1.50000 H27F 2 -0.063771 0.610006 0.144486 -21.00000 -1.50000 AFIX 0 PART 0 C28 1 0.159105 0.858242 0.294245 11.00000 0.04728 0.07044 = 0.07871 0.02938 0.01754 0.02021 PART 1 H28 2 10.144021 10.807396 10.343246 21.00000 -1.20000 PART 2 H28B 2 10.154854 10.783475 10.322132 -21.00000 -1.20000 PART 1 CL1 7 0.282567 0.982381 0.356642 21.00000 0.07276 0.06137 = 0.12338 0.00843 0.01918 0.00905 CL2 7 0.227111 0.777639 0.206477 21.00000 0.08031 0.15034 = 0.10017 -0.05305 0.00871 0.03046 CL3 7 0.000019 0.908556 0.245084 21.00000 0.04601 0.11407 = 0.10035 0.05210 0.02120 0.02531 PART 2 CL1B 7 0.229156 0.952143 0.383840 -21.00000 0.07276 0.06137 = 0.12338 0.00843 0.01918 0.00905 CL2B 7 0.266139 0.836105 0.216998 -21.00000 0.08031 0.15034 = 0.10017 -0.05305 0.00871 0.03046 CL3B 7 -0.014514 0.841751 0.198984 -21.00000 0.04601 0.11407 = 0.10035 0.05210 0.02120 0.02531 HKLF 4 REM XYZN file = SHELXL INS file, from DIRDIF output for BE20MJ REM R1 = 0.0434 for 4508 Fo > 4sig(Fo) and 0.0645 for all 6269 data REM 390 parameters refined using 3 restraints END WGHT 0.0654 0.0000 REM Highest difference peak 0.550, deepest hole -0.400, 1-sigma level 0.061 Q1 1 0.1681 0.7724 0.1624 11.00000 0.05 0.50 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.16858(4) 0.48193(3) 0.32825(2) 0.03992(12) Uani 1 1 d . A . O1 O 0.0651(2) 0.6055(2) 0.35681(15) 0.0578(6) Uani 1 1 d . . . C1 C 0.0546(3) 0.6527(3) 0.4454(2) 0.0485(8) Uani 1 1 d . . . C2 C -0.0407(4) 0.7383(3) 0.4519(3) 0.0661(10) Uani 1 1 d . . . H2 H -0.0926 0.7594 0.3947 0.079 Uiso 1 1 calc R . . C3 C -0.0570(3) 0.7900(2) 0.5416(3) 0.0712(11) Uani 1 1 d . . . H3 H -0.1183 0.8471 0.5441 0.085 Uiso 1 1 calc R . . C4 C 0.0140(3) 0.7597(2) 0.6265(3) 0.0681(10) Uani 1 1 d R . . H4 H -0.0002 0.7942 0.6865 0.082 Uiso 1 1 calc R . . O4 O 0.0272(2) 0.4170(2) 0.20410(16) 0.0653(6) Uani 1 1 d . . . C5 C 0.1072(4) 0.6777(3) 0.6232(3) 0.0566(9) Uani 1 1 d . . . H5 H 0.1566 0.658 0.6818 0.068 Uiso 1 1 calc R . . C6 C 0.1298(3) 0.6228(2) 0.5338(2) 0.0414(7) Uani 1 1 d . . . C7 C 0.2289(3) 0.5380(2) 0.5392(2) 0.0397(6) Uani 1 1 d . A . H7 H 0.2756 0.5262 0.6013 0.048 Uiso 1 1 calc R . . N1 N 0.2582(2) 0.47658(19) 0.46387(15) 0.0341(5) Uani 1 1 d . . . C8 C 0.3563(3) 0.3923(2) 0.47280(18) 0.0351(6) Uani 1 1 d . A . C9 C 0.4173(3) 0.3537(3) 0.5586(2) 0.0472(7) Uani 1 1 d . . . H9 H 0.397 0.3852 0.6174 0.057 Uiso 1 1 calc R A . C10 C 0.5078(4) 0.2687(3) 0.5576(2) 0.0565(9) Uani 1 1 d . A . H10 H 0.5486 0.243 0.6157 0.068 Uiso 1 1 calc R . . C11 C 0.5380(3) 0.2216(3) 0.4705(2) 0.0540(8) Uani 1 1 d . . . H11 H 0.599 0.1641 0.4698 0.065 Uiso 1 1 calc R A . C12 C 0.4777(3) 0.2598(3) 0.3841(2) 0.0447(7) Uani 1 1 d . A . H12 H 0.4981 0.2274 0.3256 0.054 Uiso 1 1 calc R . . C13 C 0.3873(3) 0.3456(2) 0.38399(19) 0.0354(6) Uani 1 1 d . . . N2 N 0.3151(2) 0.3890(2) 0.30062(15) 0.0382(5) Uani 1 1 d . A . S1 S 0.37758(7) 0.39842(6) 0.20822(5) 0.03596(17) Uani 1 1 d . . . O2 O 0.3126(2) 0.48921(16) 0.16103(14) 0.0488(5) Uani 1 1 d . A . O3 O 0.5287(2) 0.40914(19) 0.23332(14) 0.0500(5) Uani 1 1 d . A . C14 C 0.3180(3) 0.2635(2) 0.12253(18) 0.0324(6) Uani 1 1 d . A . C15 C 0.2289(3) 0.1795(3) 0.1436(2) 0.0429(7) Uani 1 1 d . . . H15 H 0.2032 0.1913 0.2031 0.051 Uiso 1 1 calc R A . C16 C 0.1761(3) 0.0751(3) 0.0749(2) 0.0495(8) Uani 1 1 d . A . H16 H 0.1138 0.0188 0.0887 0.059 Uiso 1 1 calc R . . C17 C 0.2148(3) 0.0556(2) -0.0112(2) 0.0429(7) Uani 1 1 d . . . H17 H 0.1775 -0.0137 -0.0559 0.052 Uiso 1 1 calc R A . C18 C 0.3109(3) 0.1383(2) -0.03460(19) 0.0341(6) Uani 1 1 d . A . C19 C 0.3538(3) 0.1178(2) -0.12491(19) 0.0388(6) Uani 1 1 d . . . C20 C 0.4340(3) 0.2065(3) -0.1483(2) 0.0472(7) Uani 1 1 d . A . H20 H 0.4574 0.1956 -0.2086 0.057 Uiso 1 1 calc R . . C21 C 0.4816(3) 0.3134(3) -0.0829(2) 0.0474(7) Uani 1 1 d . . . H21 H 0.5368 0.372 -0.1003 0.057 Uiso 1 1 calc R A . C22 C 0.4490(3) 0.3337(2) 0.0055(2) 0.0394(6) Uani 1 1 d . A . H22 H 0.4842 0.4045 0.0486 0.047 Uiso 1 1 calc R . . C23 C 0.3612(3) 0.2469(2) 0.03229(18) 0.0316(6) Uani 1 1 d . . . N3 N 0.3078(3) 0.0060(2) -0.18765(17) 0.0459(6) Uani 1 1 d . A . C24 C 0.3134(4) 0.0036(3) -0.2898(2) 0.0638(9) Uani 1 1 d . . . H24A H 0.266 0.0665 -0.3148 0.096 Uiso 1 1 calc R A . H24B H 0.2682 -0.071 -0.3286 0.096 Uiso 1 1 calc R . . H24C H 0.4096 0.0139 -0.2933 0.096 Uiso 1 1 calc R . . C25 C 0.3781(4) -0.0905(3) -0.1493(3) 0.0720(11) Uani 1 1 d . . . H25A H 0.474 -0.0822 -0.1537 0.108 Uiso 1 1 calc R A . H25B H 0.3309 -0.165 -0.1872 0.108 Uiso 1 1 calc R . . H25C H 0.3756 -0.0875 -0.0818 0.108 Uiso 1 1 calc R . . S2 S -0.03724(13) 0.47850(13) 0.12435(9) 0.0866(4) Uani 0.8727(16) 1 d PD A 1 C26 C -0.1299(9) 0.3642(7) 0.0292(4) 0.146(3) Uani 0.8727(16) 1 d PD A 1 H26A H -0.0666 0.31 0.0125 0.219 Uiso 0.8727(16) 1 calc PR A 1 H26B H -0.1711 0.3972 -0.0275 0.219 Uiso 0.8727(16) 1 calc PR A 1 H26C H -0.2027 0.3229 0.0506 0.219 Uiso 0.8727(16) 1 calc PR A 1 C27 C -0.1879(7) 0.5390(8) 0.1555(7) 0.156(4) Uani 0.8727(16) 1 d PD A 1 H27A H -0.2484 0.4772 0.1689 0.233 Uiso 0.8727(16) 1 calc PR A 1 H27B H -0.2382 0.5721 0.1015 0.233 Uiso 0.8727(16) 1 calc PR A 1 H27C H -0.157 0.5997 0.2128 0.233 Uiso 0.8727(16) 1 calc PR A 1 S2B S -0.1006(9) 0.4166(9) 0.1680(6) 0.0866(4) Uani 0.1273(16) 1 d PD A 2 C26B C -0.149(8) 0.310(4) 0.060(2) 0.146(3) Uani 0.1273(16) 1 d PD A 2 H26D H -0.0876 0.2498 0.0647 0.219 Uiso 0.1273(16) 1 calc PR A 2 H26E H -0.142 0.3477 0.0046 0.219 Uiso 0.1273(16) 1 calc PR A 2 H26F H -0.2441 0.2757 0.0506 0.219 Uiso 0.1273(16) 1 calc PR A 2 C27B C -0.140(6) 0.548(3) 0.116(5) 0.156(4) Uani 0.1273(16) 1 d PD A 2 H27D H -0.2247 0.5726 0.1302 0.233 Uiso 0.1273(16) 1 calc PR A 2 H27E H -0.1515 0.5306 0.0462 0.233 Uiso 0.1273(16) 1 calc PR A 2 H27F H -0.0638 0.61 0.1445 0.233 Uiso 0.1273(16) 1 calc PR A 2 C28 C 0.1591(4) 0.8582(3) 0.2942(3) 0.0627(9) Uani 1 1 d . . . H28 H 0.144 0.8074 0.3432 0.075 Uiso 0.8727(16) 1 d P A 1 H28B H 0.1549 0.7835 0.3221 0.075 Uiso 0.1273(16) 1 d P A 2 Cl1 Cl 0.28257(16) 0.98238(12) 0.35664(12) 0.0875(4) Uani 0.8727(16) 1 d P A 1 Cl2 Cl 0.2271(2) 0.77764(18) 0.20648(14) 0.1196(7) Uani 0.8727(16) 1 d P A 1 Cl3 Cl 0.00002(12) 0.90856(15) 0.24508(11) 0.0819(4) Uani 0.8727(16) 1 d P A 1 Cl1B Cl 0.2292(12) 0.9521(9) 0.3838(9) 0.0875(4) Uani 0.1273(16) 1 d P A 2 Cl2B Cl 0.2661(15) 0.8361(14) 0.2170(12) 0.1196(7) Uani 0.1273(16) 1 d P A 2 Cl3B Cl -0.0145(10) 0.8418(11) 0.1990(8) 0.0819(4) Uani 0.1273(16) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0391(2) 0.0505(2) 0.03277(19) 0.00858(15) 0.01008(14) 0.01497(16) O1 0.0710(16) 0.0674(14) 0.0491(13) 0.0215(11) 0.0253(11) 0.0392(12) C1 0.0483(19) 0.0441(17) 0.065(2) 0.0145(15) 0.0300(16) 0.0159(14) C2 0.068(2) 0.060(2) 0.089(3) 0.0271(19) 0.041(2) 0.0291(18) C3 0.076(3) 0.048(2) 0.110(3) 0.013(2) 0.059(3) 0.0235(19) C4 0.070(3) 0.058(2) 0.080(3) -0.011(2) 0.042(2) 0.0019(19) O4 0.0491(14) 0.0897(18) 0.0484(13) 0.0071(12) -0.0045(10) 0.0156(12) C5 0.063(2) 0.0517(19) 0.056(2) -0.0082(15) 0.0297(17) -0.0001(16) C6 0.0411(17) 0.0372(15) 0.0478(17) 0.0007(13) 0.0210(13) -0.0006(12) C7 0.0391(16) 0.0433(16) 0.0339(15) 0.0007(12) 0.0097(12) -0.0009(12) N1 0.0352(13) 0.0358(12) 0.0325(12) 0.0052(9) 0.0115(9) 0.0042(9) C8 0.0315(15) 0.0392(15) 0.0325(14) 0.0040(11) 0.0057(11) 0.0033(11) C9 0.0468(18) 0.0597(19) 0.0346(15) 0.0083(13) 0.0072(13) 0.0114(15) C10 0.056(2) 0.069(2) 0.0481(19) 0.0248(16) 0.0045(15) 0.0228(17) C11 0.053(2) 0.0527(19) 0.060(2) 0.0155(16) 0.0124(15) 0.0206(16) C12 0.0433(17) 0.0469(17) 0.0433(16) 0.0020(13) 0.0111(13) 0.0111(13) C13 0.0303(14) 0.0379(15) 0.0356(14) 0.0035(11) 0.0061(11) 0.0008(11) N2 0.0391(13) 0.0481(14) 0.0294(11) 0.0048(10) 0.0121(10) 0.0104(10) S1 0.0359(4) 0.0388(4) 0.0330(4) 0.0025(3) 0.0111(3) 0.0027(3) O2 0.0674(15) 0.0395(11) 0.0468(12) 0.0105(9) 0.0241(10) 0.0131(10) O3 0.0358(12) 0.0675(14) 0.0414(11) -0.0041(10) 0.0114(9) -0.0056(10) C14 0.0300(14) 0.0364(14) 0.0308(13) 0.0065(11) 0.0065(10) 0.0054(11) C15 0.0436(17) 0.0505(17) 0.0355(15) 0.0064(13) 0.0152(13) -0.0021(13) C16 0.0478(19) 0.0483(18) 0.0506(18) 0.0072(14) 0.0159(14) -0.0130(14) C17 0.0411(17) 0.0403(16) 0.0438(16) 0.0026(12) 0.0094(13) -0.0045(12) C18 0.0277(14) 0.0386(15) 0.0341(14) 0.0045(11) 0.0047(10) 0.0047(11) C19 0.0328(15) 0.0462(16) 0.0365(15) 0.0012(12) 0.0082(11) 0.0116(12) C20 0.0451(18) 0.0583(19) 0.0431(16) 0.0053(14) 0.0231(14) 0.0065(14) C21 0.0465(18) 0.0500(18) 0.0526(18) 0.0115(14) 0.0262(15) 0.0006(14) C22 0.0393(16) 0.0367(15) 0.0438(16) 0.0050(12) 0.0158(13) 0.0007(12) C23 0.0280(14) 0.0361(14) 0.0323(13) 0.0089(11) 0.0081(10) 0.0069(11) N3 0.0431(15) 0.0511(15) 0.0387(13) -0.0066(11) 0.0086(11) 0.0088(11) C24 0.062(2) 0.078(2) 0.0455(18) -0.0112(17) 0.0188(16) 0.0027(18) C25 0.091(3) 0.050(2) 0.068(2) -0.0035(17) 0.009(2) 0.024(2) S2 0.0522(7) 0.1304(11) 0.0740(8) 0.0564(7) -0.0094(5) -0.0076(7) C26 0.134(6) 0.210(8) 0.059(4) 0.024(4) -0.038(4) -0.006(6) C27 0.069(5) 0.185(7) 0.213(10) 0.066(6) -0.003(5) 0.064(5) S2B 0.0522(7) 0.1304(11) 0.0740(8) 0.0564(7) -0.0094(5) -0.0076(7) C26B 0.134(6) 0.210(8) 0.059(4) 0.024(4) -0.038(4) -0.006(6) C27B 0.069(5) 0.185(7) 0.213(10) 0.066(6) -0.003(5) 0.064(5) C28 0.047(2) 0.070(2) 0.079(2) 0.0294(19) 0.0175(17) 0.0202(17) Cl1 0.0728(10) 0.0614(8) 0.1234(12) 0.0084(7) 0.0192(7) 0.0090(6) Cl2 0.0803(12) 0.1503(18) 0.1002(10) -0.0531(12) 0.0087(9) 0.0305(11) Cl3 0.0460(6) 0.1141(12) 0.1004(11) 0.0521(8) 0.0212(6) 0.0253(7) Cl1B 0.0728(10) 0.0614(8) 0.1234(12) 0.0084(7) 0.0192(7) 0.0090(6) Cl2B 0.0803(12) 0.1503(18) 0.1002(10) -0.0531(12) 0.0087(9) 0.0305(11) Cl3B 0.0460(6) 0.1141(12) 0.1004(11) 0.0521(8) 0.0212(6) 0.0253(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.866(2) . ? Cu1 N1 1.934(2) . ? Cu1 N2 1.942(2) . ? Cu1 O4 1.975(2) . ? O1 C1 1.323(4) . ? C1 C6 1.408(4) . ? C1 C2 1.423(4) . ? C2 C3 1.372(4) . ? C2 H2 0.93 . ? C3 C4 1.3558 . ? C3 H3 0.93 . ? C4 C5 1.372(4) . ? C4 H4 0.93 . ? O4 S2B 1.245(8) . ? O4 S2 1.471(2) . ? C5 C6 1.405(4) . ? C5 H5 0.93 . ? C6 C7 1.433(4) . ? C7 N1 1.293(3) . ? C7 H7 0.93 . ? N1 C8 1.423(3) . ? C8 C9 1.381(4) . ? C8 C13 1.404(4) . ? C9 C10 1.377(4) . ? C9 H9 0.93 . ? C10 C11 1.381(5) . ? C10 H10 0.93 . ? C11 C12 1.383(4) . ? C11 H11 0.93 . ? C12 C13 1.383(4) . ? C12 H12 0.93 . ? C13 N2 1.414(3) . ? N2 S1 1.586(2) . ? S1 O2 1.438(2) . ? S1 O3 1.440(2) . ? S1 C14 1.786(3) . ? C14 C15 1.366(4) . ? C14 C23 1.432(3) . ? C15 C16 1.405(4) . ? C15 H15 0.93 . ? C16 C17 1.356(4) . ? C16 H16 0.93 . ? C17 C18 1.417(4) . ? C17 H17 0.93 . ? C18 C23 1.427(4) . ? C18 C19 1.433(4) . ? C19 C20 1.367(4) . ? C19 N3 1.424(4) . ? C20 C21 1.399(4) . ? C20 H20 0.93 . ? C21 C22 1.357(4) . ? C21 H21 0.93 . ? C22 C23 1.420(3) . ? C22 H22 0.93 . ? N3 C24 1.460(4) . ? N3 C25 1.462(4) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? S2 C26 1.757(6) . ? S2 C27 1.807(6) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? S2B C26B 1.756(19) . ? S2B C27B 1.81(2) . ? C26B H26D 0.96 . ? C26B H26E 0.96 . ? C26B H26F 0.96 . ? C27B H27D 0.96 . ? C27B H27E 0.96 . ? C27B H27F 0.96 . ? C28 Cl1B 1.523(12) . ? C28 Cl2B 1.696(17) . ? C28 Cl2 1.733(4) . ? C28 Cl3 1.744(3) . ? C28 Cl1 1.773(4) . ? C28 Cl3B 1.895(11) . ? C28 H28 1.002(3) . ? C28 H28B 1.001(3) . ? Cl1B H28 1.753(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N1 95.56(9) . . ? O1 Cu1 N2 164.27(11) . . ? N1 Cu1 N2 83.71(9) . . ? O1 Cu1 O4 91.87(10) . . ? N1 Cu1 O4 151.13(10) . . ? N2 Cu1 O4 96.30(9) . . ? C1 O1 Cu1 126.00(19) . . ? O1 C1 C6 124.4(3) . . ? O1 C1 C2 117.9(3) . . ? C6 C1 C2 117.6(3) . . ? C3 C2 C1 120.7(4) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 121.5(2) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C3 C4 C5 119.4(2) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? S2B O4 S2 53.3(4) . . ? S2B O4 Cu1 138.7(5) . . ? S2 O4 Cu1 128.95(17) . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? C5 C6 C1 118.9(3) . . ? C5 C6 C7 116.9(3) . . ? C1 C6 C7 124.1(3) . . ? N1 C7 C6 124.8(3) . . ? N1 C7 H7 117.6 . . ? C6 C7 H7 117.6 . . ? C7 N1 C8 122.8(2) . . ? C7 N1 Cu1 124.6(2) . . ? C8 N1 Cu1 112.54(16) . . ? C9 C8 C13 120.0(3) . . ? C9 C8 N1 125.6(2) . . ? C13 C8 N1 114.4(2) . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.0(3) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C13 C12 C11 120.6(3) . . ? C13 C12 H12 119.7 . . ? C11 C12 H12 119.7 . . ? C12 C13 C8 118.9(2) . . ? C12 C13 N2 126.2(2) . . ? C8 C13 N2 114.9(2) . . ? C13 N2 S1 122.85(19) . . ? C13 N2 Cu1 112.42(16) . . ? S1 N2 Cu1 121.77(13) . . ? O2 S1 O3 117.08(13) . . ? O2 S1 N2 106.97(12) . . ? O3 S1 N2 112.30(12) . . ? O2 S1 C14 105.81(12) . . ? O3 S1 C14 106.54(12) . . ? N2 S1 C14 107.61(12) . . ? C15 C14 C23 121.4(2) . . ? C15 C14 S1 119.0(2) . . ? C23 C14 S1 119.52(19) . . ? C14 C15 C16 119.7(3) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.8(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 121.5(3) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C23 118.6(2) . . ? C17 C18 C19 121.9(2) . . ? C23 C18 C19 119.5(2) . . ? C20 C19 N3 122.8(3) . . ? C20 C19 C18 119.1(2) . . ? N3 C19 C18 118.1(2) . . ? C19 C20 C21 121.0(3) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 121.5(3) . . ? C22 C21 H21 119.2 . . ? C20 C21 H21 119.2 . . ? C21 C22 C23 120.1(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 118.6(2) . . ? C22 C23 C14 123.4(2) . . ? C18 C23 C14 117.9(2) . . ? C19 N3 C24 115.1(3) . . ? C19 N3 C25 113.1(2) . . ? C24 N3 C25 109.9(3) . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4 S2 C26 104.4(3) . . ? O4 S2 C27 107.6(3) . . ? C26 S2 C27 97.3(4) . . ? O4 S2B C26B 108(2) . . ? O4 S2B C27B 112.5(19) . . ? C26B S2B C27B 99.3(18) . . ? S2B C26B H26D 109.5 . . ? S2B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? S2B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? S2B C27B H27D 109.5 . . ? S2B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? S2B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? Cl1B C28 Cl2B 111.0(6) . . ? Cl2 C28 Cl3 113.5(2) . . ? Cl2 C28 Cl1 108.9(2) . . ? Cl3 C28 Cl1 108.6(2) . . ? Cl1B C28 Cl3B 133.0(6) . . ? Cl2B C28 Cl3B 98.7(6) . . ? Cl2 C28 H28 109.0(3) . . ? Cl3 C28 H28 108.3(3) . . ? Cl1 C28 H28 108.5(3) . . ? Cl1B C28 H28B 103.5(5) . . ? Cl2B C28 H28B 104.3(7) . . ? Cl3B C28 H28B 103.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 O1 C1 -7.5(3) . . . . ? N2 Cu1 O1 C1 -94.1(4) . . . . ? O4 Cu1 O1 C1 144.6(3) . . . . ? Cu1 O1 C1 C6 5.3(4) . . . . ? Cu1 O1 C1 C2 -173.7(2) . . . . ? O1 C1 C2 C3 179.6(3) . . . . ? C6 C1 C2 C3 0.6(5) . . . . ? C1 C2 C3 C4 -1.5(4) . . . . ? C2 C3 C4 C5 1.7(2) . . . . ? O1 Cu1 O4 S2B -25.9(7) . . . . ? N1 Cu1 O4 S2B 79.2(7) . . . . ? N2 Cu1 O4 S2B 167.6(7) . . . . ? O1 Cu1 O4 S2 49.9(2) . . . . ? N1 Cu1 O4 S2 154.99(18) . . . . ? N2 Cu1 O4 S2 -116.6(2) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? C4 C5 C6 C7 -179.6(3) . . . . ? O1 C1 C6 C5 -178.7(3) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? O1 C1 C6 C7 0.7(5) . . . . ? C2 C1 C6 C7 179.7(3) . . . . ? C5 C6 C7 N1 177.4(3) . . . . ? C1 C6 C7 N1 -2.1(5) . . . . ? C6 C7 N1 C8 -179.3(3) . . . . ? C6 C7 N1 Cu1 -2.6(4) . . . . ? O1 Cu1 N1 C7 6.2(2) . . . . ? N2 Cu1 N1 C7 170.4(2) . . . . ? O4 Cu1 N1 C7 -98.0(3) . . . . ? O1 Cu1 N1 C8 -176.85(18) . . . . ? N2 Cu1 N1 C8 -12.65(18) . . . . ? O4 Cu1 N1 C8 79.0(3) . . . . ? C7 N1 C8 C9 9.2(4) . . . . ? Cu1 N1 C8 C9 -167.8(2) . . . . ? C7 N1 C8 C13 -172.3(2) . . . . ? Cu1 N1 C8 C13 10.7(3) . . . . ? C13 C8 C9 C10 -0.5(5) . . . . ? N1 C8 C9 C10 177.9(3) . . . . ? C8 C9 C10 C11 -0.1(5) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C10 C11 C12 C13 0.3(5) . . . . ? C11 C12 C13 C8 -0.8(4) . . . . ? C11 C12 C13 N2 -177.5(3) . . . . ? C9 C8 C13 C12 0.9(4) . . . . ? N1 C8 C13 C12 -177.6(3) . . . . ? C9 C8 C13 N2 178.0(3) . . . . ? N1 C8 C13 N2 -0.6(3) . . . . ? C12 C13 N2 S1 -32.1(4) . . . . ? C8 C13 N2 S1 151.1(2) . . . . ? C12 C13 N2 Cu1 167.1(2) . . . . ? C8 C13 N2 Cu1 -9.7(3) . . . . ? O1 Cu1 N2 C13 100.5(4) . . . . ? N1 Cu1 N2 C13 12.33(18) . . . . ? O4 Cu1 N2 C13 -138.62(19) . . . . ? O1 Cu1 N2 S1 -60.5(4) . . . . ? N1 Cu1 N2 S1 -148.69(16) . . . . ? O4 Cu1 N2 S1 60.36(17) . . . . ? C13 N2 S1 O2 -155.1(2) . . . . ? Cu1 N2 S1 O2 3.89(19) . . . . ? C13 N2 S1 O3 -25.4(3) . . . . ? Cu1 N2 S1 O3 133.65(15) . . . . ? C13 N2 S1 C14 91.6(2) . . . . ? Cu1 N2 S1 C14 -109.42(15) . . . . ? O2 S1 C14 C15 -111.2(2) . . . . ? O3 S1 C14 C15 123.5(2) . . . . ? N2 S1 C14 C15 2.9(3) . . . . ? O2 S1 C14 C23 67.0(2) . . . . ? O3 S1 C14 C23 -58.3(2) . . . . ? N2 S1 C14 C23 -178.88(19) . . . . ? C23 C14 C15 C16 -1.0(4) . . . . ? S1 C14 C15 C16 177.2(2) . . . . ? C14 C15 C16 C17 1.4(5) . . . . ? C15 C16 C17 C18 0.9(5) . . . . ? C16 C17 C18 C23 -3.4(4) . . . . ? C16 C17 C18 C19 179.3(3) . . . . ? C17 C18 C19 C20 172.6(3) . . . . ? C23 C18 C19 C20 -4.7(4) . . . . ? C17 C18 C19 N3 -6.0(4) . . . . ? C23 C18 C19 N3 176.7(2) . . . . ? N3 C19 C20 C21 -177.5(3) . . . . ? C18 C19 C20 C21 4.0(4) . . . . ? C19 C20 C21 C22 -0.7(5) . . . . ? C20 C21 C22 C23 -2.0(5) . . . . ? C21 C22 C23 C18 1.1(4) . . . . ? C21 C22 C23 C14 -177.7(3) . . . . ? C17 C18 C23 C22 -175.2(2) . . . . ? C19 C18 C23 C22 2.1(4) . . . . ? C17 C18 C23 C14 3.6(4) . . . . ? C19 C18 C23 C14 -179.0(2) . . . . ? C15 C14 C23 C22 177.3(3) . . . . ? S1 C14 C23 C22 -0.9(4) . . . . ? C15 C14 C23 C18 -1.5(4) . . . . ? S1 C14 C23 C18 -179.67(19) . . . . ? C20 C19 N3 C24 -18.2(4) . . . . ? C18 C19 N3 C24 160.4(3) . . . . ? C20 C19 N3 C25 109.3(3) . . . . ? C18 C19 N3 C25 -72.2(3) . . . . ? S2B O4 S2 C26 -62.5(7) . . . . ? Cu1 O4 S2 C26 170.5(4) . . . . ? S2B O4 S2 C27 40.2(7) . . . . ? Cu1 O4 S2 C27 -86.8(4) . . . . ? S2 O4 S2B C26B 82(2) . . . . ? Cu1 O4 S2B C26B -168(2) . . . . ? S2 O4 S2B C27B -27(2) . . . . ? Cu1 O4 S2B C27B 83(2) . . . . ? # END of CIF # Attachment '- 12.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-06-19 at 12:54:25 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : be67mj1n struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_ZnSALDS _database_code_depnum_ccdc_archive 'CCDC 877815' #TrackingRef '- 12.cif' _audit_creation_date 2012-06-19T12:54:25-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C100 H86 N12 O14 S4 Zn5, 5(C2 H3 N)' _chemical_formula_sum 'C110 H101 N17 O14 S4 Zn5' _chemical_formula_weight 2340.17 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 19.4209(5) _cell_length_b 22.3669(5) _cell_length_c 23.7524(6) _cell_angle_alpha 90 _cell_angle_beta 94.3730(10) _cell_angle_gamma 90 _cell_volume 10287.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 23.18 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4824 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.304 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.6526 _exptl_absorpt_correction_T_max 0.8878 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0758 _diffrn_reflns_av_unetI/netI 0.0925 _diffrn_reflns_number 114014 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.68 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 19514 _reflns_number_gt 12664 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR-97 (Giacovazzo et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0406P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 19514 _refine_ls_number_parameters 1372 _refine_ls_number_restraints 97 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0469 _refine_ls_wR_factor_ref 0.1017 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.978 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.813 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.084 _iucr_refine_instructions_details ; TITL be67mj1n in P 1 21/n 1 CELL 0.71073 19.4209 22.3669 23.7524 90.000 94.373 90.000 ZERR 4.00 0.0005 0.0005 0.0006 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O S ZN UNIT 440 404 68 56 16 20 MERG 2 OMIT -1 0 1 OMIT -1 2 2 OMIT -4 6 2 OMIT 2 2 1 OMIT 2 1 2 OMIT -1 13 1 DFIX 0.82 H14O O14 HTAB O13 O2 HTAB O14 O9 ISOR 0.005 C109 C110 N17 C103 C104 N14 DELU 0.005 0.0005 C103 C104 N14 SIMU 0.010 0.0050 1.700 C103 C104 N14 DELU 0.005 0.0005 C105 C106 N15 SIMU 0.010 0.0050 1.700 C105 C106 N15 DELU 0.005 0.0005 C107 C108 N16 SIMU 0.010 0.0050 1.700 C107 C108 N16 DELU 0.005 0.0005 C109 C110 N17 SIMU 0.010 0.0050 1.700 C109 C110 N17 FMAP 2 PLAN 1 SIZE 0.07 0.12 0.20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 14 TEMP -173.00 WGHT 0.040600 FVAR 0.03557 C1 1 0.788457 0.586665 0.405627 11.00000 0.02410 0.02605 = 0.01907 0.00044 -0.00227 -0.01063 C2 1 0.723323 0.580074 0.377156 11.00000 0.02262 0.02815 = 0.03318 0.00322 -0.00005 -0.00333 AFIX 43 H2 2 0.687242 0.606957 0.384582 11.00000 -1.20000 AFIX 0 C3 1 0.710875 0.534088 0.337736 11.00000 0.03402 0.03610 = 0.01662 0.00501 -0.00685 -0.01696 AFIX 43 H3 2 0.666413 0.529936 0.318519 11.00000 -1.20000 AFIX 0 C4 1 0.762873 0.494753 0.326647 11.00000 0.04205 0.03048 = 0.02565 -0.00476 -0.00103 -0.01505 AFIX 43 H4 2 0.754312 0.463182 0.300285 11.00000 -1.20000 AFIX 0 C5 1 0.826627 0.501724 0.353947 11.00000 0.03707 0.02633 = 0.02639 -0.00563 0.00292 -0.00480 AFIX 43 H5 2 0.862205 0.474587 0.345898 11.00000 -1.20000 AFIX 0 C6 1 0.841949 0.547557 0.393647 11.00000 0.02918 0.02077 = 0.01583 -0.00191 0.00403 -0.00283 C7 1 0.910758 0.549275 0.420677 11.00000 0.02818 0.02038 = 0.02331 -0.00130 0.00466 -0.00203 AFIX 43 H7 2 0.939283 0.515947 0.413856 11.00000 -1.20000 AFIX 0 C8 1 1.007234 0.585633 0.477951 11.00000 0.01793 0.01864 = 0.02355 0.00354 0.00205 0.00075 C9 1 1.056177 0.546145 0.459206 11.00000 0.03012 0.01971 = 0.02642 0.00073 0.00787 -0.00101 AFIX 43 H9 2 1.044099 0.520358 0.428237 11.00000 -1.20000 AFIX 0 C10 1 1.121971 0.544358 0.485395 11.00000 0.02349 0.02111 = 0.04074 0.00225 0.00929 0.00564 AFIX 43 H10 2 1.154926 0.517006 0.472806 11.00000 -1.20000 AFIX 0 C11 1 1.139954 0.582338 0.529930 11.00000 0.01408 0.02371 = 0.03527 0.00856 -0.00012 0.00151 AFIX 43 H11 2 1.185573 0.581373 0.547459 11.00000 -1.20000 AFIX 0 C12 1 1.092225 0.621795 0.549300 11.00000 0.02344 0.02010 = 0.02653 0.00018 0.00151 -0.00104 AFIX 43 H12 2 1.105175 0.647537 0.580117 11.00000 -1.20000 AFIX 0 C13 1 1.024899 0.623928 0.523649 11.00000 0.01774 0.01604 = 0.01622 0.00482 0.00213 -0.00168 C14 1 1.039027 0.766685 0.573400 11.00000 0.01708 0.02040 = 0.01895 -0.00267 -0.00435 0.00277 C15 1 1.064582 0.767642 0.521680 11.00000 0.02947 0.02363 = 0.01891 -0.00040 -0.00526 0.00064 AFIX 43 H15 2 1.050261 0.738045 0.494584 11.00000 -1.20000 AFIX 0 C16 1 1.112008 0.811917 0.507705 11.00000 0.02959 0.03274 = 0.02346 0.00506 -0.00046 -0.00459 AFIX 43 H16 2 1.130267 0.811496 0.471723 11.00000 -1.20000 AFIX 0 C17 1 1.131718 0.855477 0.545978 11.00000 0.03309 0.02668 = 0.03136 0.00674 -0.00802 -0.00721 AFIX 43 H17 2 1.163805 0.885124 0.536317 11.00000 -1.20000 AFIX 0 C18 1 1.105060 0.857078 0.599749 11.00000 0.02273 0.02263 = 0.02497 0.00155 -0.00736 0.00414 C19 1 1.127473 0.902303 0.640031 11.00000 0.02550 0.01940 = 0.03060 -0.00184 -0.00568 0.00291 C20 1 1.105203 0.899392 0.693137 11.00000 0.03747 0.02737 = 0.03862 -0.01102 -0.00724 -0.00193 AFIX 43 H20 2 1.121680 0.927819 0.720671 11.00000 -1.20000 AFIX 0 C21 1 1.058076 0.854874 0.707953 11.00000 0.04364 0.02584 = 0.03017 -0.00570 0.00277 -0.00181 AFIX 43 H21 2 1.043108 0.853977 0.745100 11.00000 -1.20000 AFIX 0 C22 1 1.033858 0.813097 0.669266 11.00000 0.02858 0.01875 = 0.02793 -0.00097 0.00139 -0.00099 AFIX 43 H22 2 1.000432 0.784694 0.679086 11.00000 -1.20000 AFIX 0 C23 1 1.058293 0.812045 0.614951 11.00000 0.02289 0.01770 = 0.02180 -0.00269 -0.00704 0.00412 C24 1 1.139034 0.993541 0.587678 11.00000 0.04450 0.03505 = 0.06757 0.01462 -0.02316 -0.01281 AFIX 137 H24A 2 1.107685 1.016319 0.609995 11.00000 -1.50000 H24B 2 1.112620 0.974765 0.555602 11.00000 -1.50000 H24C 2 1.173671 1.020526 0.573737 11.00000 -1.50000 AFIX 0 C25 1 1.218017 0.973832 0.668448 11.00000 0.03933 0.03783 = 0.04683 0.00020 -0.01078 -0.01501 AFIX 137 H25A 2 1.240091 0.942269 0.692075 11.00000 -1.50000 H25B 2 1.190234 0.999267 0.691526 11.00000 -1.50000 H25C 2 1.253579 0.998081 0.652217 11.00000 -1.50000 AFIX 0 C26 1 0.940026 0.760093 0.404163 11.00000 0.01537 0.03568 = 0.01874 0.00520 -0.00258 0.00889 C27 1 0.963598 0.720517 0.363659 11.00000 0.03944 0.02766 = 0.02197 0.00300 0.00173 0.00784 AFIX 43 H27 2 0.946832 0.680605 0.362054 11.00000 -1.20000 AFIX 0 C28 1 1.010147 0.738373 0.326574 11.00000 0.04764 0.04577 = 0.02513 0.00190 0.00582 0.01898 AFIX 43 H28 2 1.024300 0.710969 0.299161 11.00000 -1.20000 AFIX 0 C29 1 1.037190 0.796387 0.328446 11.00000 0.03833 0.04822 = 0.02913 0.00771 0.00995 0.01246 AFIX 43 H29 2 1.069898 0.808571 0.302972 11.00000 -1.20000 AFIX 0 C30 1 1.015345 0.834954 0.367801 11.00000 0.03006 0.04093 = 0.02792 0.00525 0.00402 0.00218 AFIX 43 H30 2 1.033286 0.874485 0.369116 11.00000 -1.20000 AFIX 0 C31 1 0.967620 0.818769 0.406334 11.00000 0.02730 0.02665 = 0.02032 0.00203 0.00077 0.00543 C32 1 0.952885 0.862306 0.448086 11.00000 0.02313 0.02641 = 0.03174 0.00096 -0.00371 0.00030 AFIX 43 H32 2 0.977551 0.898948 0.447441 11.00000 -1.20000 AFIX 0 C33 1 0.904417 0.903697 0.527192 11.00000 0.02624 0.01897 = 0.02458 0.00167 0.00183 -0.00205 C34 1 0.957484 0.943703 0.541832 11.00000 0.02838 0.02867 = 0.03275 -0.00144 0.00752 -0.00109 AFIX 43 H34 2 1.000219 0.940117 0.525147 11.00000 -1.20000 AFIX 0 C35 1 0.948595 0.988572 0.580392 11.00000 0.03728 0.02529 = 0.03522 -0.00134 0.00556 -0.01220 AFIX 43 H35 2 0.985000 1.015946 0.590033 11.00000 -1.20000 AFIX 0 C36 1 0.887229 0.993625 0.604771 11.00000 0.03522 0.02167 = 0.03540 -0.00671 0.00244 -0.00229 AFIX 43 H36 2 0.880284 1.025813 0.629811 11.00000 -1.20000 AFIX 0 C37 1 0.835257 0.952118 0.593150 11.00000 0.02531 0.02442 = 0.02330 -0.00217 0.00470 -0.00274 AFIX 43 H37 2 0.793268 0.955613 0.610953 11.00000 -1.20000 AFIX 0 C38 1 0.843728 0.905377 0.555753 11.00000 0.01919 0.02356 = 0.02379 0.00175 0.00329 0.00151 C39 1 0.756295 0.842496 0.650309 11.00000 0.02283 0.02059 = 0.01684 -0.00461 -0.00038 -0.00103 C40 1 0.823897 0.826789 0.663894 11.00000 0.02263 0.02734 = 0.01970 -0.00048 0.00386 0.00589 AFIX 43 H40 2 0.853414 0.819019 0.634637 11.00000 -1.20000 AFIX 0 C41 1 0.849743 0.822111 0.720225 11.00000 0.02121 0.03597 = 0.02128 0.00018 -0.00235 0.00251 AFIX 43 H41 2 0.897135 0.813005 0.728954 11.00000 -1.20000 AFIX 0 C42 1 0.807411 0.830525 0.762786 11.00000 0.02831 0.03162 = 0.01887 -0.00151 -0.00252 -0.00141 AFIX 43 H42 2 0.825906 0.828139 0.800916 11.00000 -1.20000 AFIX 0 C43 1 0.736475 0.842731 0.750924 11.00000 0.02267 0.01869 = 0.02223 -0.00418 -0.00084 -0.00369 C44 1 0.691825 0.849219 0.796018 11.00000 0.02660 0.02045 = 0.02398 -0.00260 0.00338 -0.00489 C45 1 0.626719 0.871861 0.783907 11.00000 0.02925 0.02730 = 0.03483 -0.00498 0.00859 -0.00162 AFIX 43 H45 2 0.598556 0.880670 0.813833 11.00000 -1.20000 AFIX 0 C46 1 0.601441 0.882074 0.728406 11.00000 0.02331 0.02893 = 0.03488 0.00002 0.00548 0.00502 AFIX 43 H46 2 0.556056 0.897562 0.721336 11.00000 -1.20000 AFIX 0 C47 1 0.639815 0.870543 0.683542 11.00000 0.02296 0.02574 = 0.02563 -0.00126 -0.00311 0.00053 AFIX 43 H47 2 0.620017 0.874802 0.645934 11.00000 -1.20000 AFIX 0 C48 1 0.709935 0.852047 0.694130 11.00000 0.02272 0.01492 = 0.02304 -0.00278 0.00175 -0.00181 C49 1 0.682344 0.858687 0.897526 11.00000 0.04469 0.04453 = 0.02996 -0.00550 0.01166 -0.00601 AFIX 137 H49A 2 0.636795 0.839772 0.897155 11.00000 -1.50000 H49B 2 0.676741 0.901973 0.892714 11.00000 -1.50000 H49C 2 0.708464 0.850446 0.933631 11.00000 -1.50000 AFIX 0 C50 1 0.732520 0.771037 0.860335 11.00000 0.04057 0.04511 = 0.02773 0.00646 0.00010 0.00138 AFIX 137 H50A 2 0.757047 0.755233 0.828985 11.00000 -1.50000 H50B 2 0.688485 0.749957 0.861999 11.00000 -1.50000 H50C 2 0.760767 0.765135 0.895876 11.00000 -1.50000 AFIX 0 C51 1 0.696383 0.579883 0.579184 11.00000 0.03270 0.02374 = 0.01778 -0.00492 -0.00414 0.00540 C52 1 0.765479 0.574332 0.599312 11.00000 0.03771 0.02489 = 0.03791 -0.00514 -0.00576 0.00539 AFIX 43 H52 2 0.799102 0.599336 0.584264 11.00000 -1.20000 AFIX 0 C53 1 0.786208 0.532901 0.641008 11.00000 0.03981 0.02932 = 0.03718 -0.00687 -0.00938 0.01506 AFIX 43 H53 2 0.833467 0.530003 0.654339 11.00000 -1.20000 AFIX 0 C54 1 0.737486 0.495809 0.663038 11.00000 0.06018 0.02751 = 0.02867 -0.00243 -0.00999 0.01717 AFIX 43 H54 2 0.750936 0.467533 0.691635 11.00000 -1.20000 AFIX 0 C55 1 0.670146 0.500695 0.642930 11.00000 0.04726 0.02548 = 0.02329 -0.00135 0.00155 0.00515 AFIX 43 H55 2 0.637361 0.474618 0.657688 11.00000 -1.20000 AFIX 0 C56 1 0.646487 0.542573 0.601218 11.00000 0.03710 0.01766 = 0.02041 -0.00351 -0.00326 0.00526 C57 1 0.574319 0.539822 0.581756 11.00000 0.03869 0.02014 = 0.01720 -0.00382 0.00450 -0.00149 AFIX 43 H57 2 0.548152 0.508097 0.596002 11.00000 -1.20000 AFIX 0 C58 1 0.471307 0.568377 0.527635 11.00000 0.02487 0.01802 = 0.02353 -0.00277 0.00561 0.00102 C59 1 0.424295 0.534974 0.556606 11.00000 0.03422 0.02177 = 0.02650 0.00230 0.00821 -0.00058 AFIX 43 H59 2 0.439430 0.514828 0.590528 11.00000 -1.20000 AFIX 0 C60 1 0.356026 0.531243 0.536009 11.00000 0.02864 0.02872 = 0.03533 -0.00545 0.01604 -0.00628 AFIX 43 H60 2 0.324365 0.507957 0.555309 11.00000 -1.20000 AFIX 0 C61 1 0.333952 0.561406 0.487361 11.00000 0.02121 0.02383 = 0.03907 -0.00718 0.00807 -0.00317 AFIX 43 H61 2 0.286897 0.559041 0.473334 11.00000 -1.20000 AFIX 0 C62 1 0.379750 0.595070 0.458824 11.00000 0.02418 0.01800 = 0.02826 -0.00320 0.00542 -0.00109 AFIX 43 H62 2 0.363544 0.616144 0.425700 11.00000 -1.20000 AFIX 0 C63 1 0.449135 0.598616 0.477773 11.00000 0.02080 0.01321 = 0.02863 -0.00488 0.00809 -0.00278 C64 1 0.437067 0.732069 0.409699 11.00000 0.01622 0.01927 = 0.01670 -0.00355 0.00056 -0.00355 C65 1 0.416715 0.738998 0.462843 11.00000 0.01985 0.01887 = 0.02117 0.00050 -0.00104 -0.00117 AFIX 43 H65 2 0.428607 0.709626 0.490799 11.00000 -1.20000 AFIX 0 C66 1 0.377912 0.789747 0.476695 11.00000 0.02068 0.02595 = 0.01598 -0.00428 0.00159 -0.00299 AFIX 43 H66 2 0.363494 0.794317 0.513783 11.00000 -1.20000 AFIX 0 C67 1 0.361377 0.831841 0.436837 11.00000 0.02510 0.02162 = 0.02514 -0.00480 -0.00198 0.00273 AFIX 43 H67 2 0.336193 0.866212 0.446694 11.00000 -1.20000 AFIX 0 C68 1 0.380824 0.825713 0.380806 11.00000 0.02299 0.02000 = 0.02270 0.00032 0.00030 -0.00281 C69 1 0.362251 0.870494 0.338607 11.00000 0.03453 0.01916 = 0.02920 -0.00468 -0.00114 0.00382 C70 1 0.386243 0.864972 0.286381 11.00000 0.04634 0.02421 = 0.02594 0.00608 -0.00001 0.00338 AFIX 43 H70 2 0.375439 0.895062 0.258890 11.00000 -1.20000 AFIX 0 C71 1 0.426512 0.815891 0.272293 11.00000 0.03667 0.02551 = 0.02453 -0.00216 0.00590 -0.00369 AFIX 43 H71 2 0.442017 0.812876 0.235421 11.00000 -1.20000 AFIX 0 C72 1 0.443644 0.772186 0.311489 11.00000 0.02639 0.01995 = 0.02591 -0.00084 0.00179 -0.00359 AFIX 43 H72 2 0.471113 0.739267 0.301488 11.00000 -1.20000 AFIX 0 C73 1 0.420944 0.775572 0.366454 11.00000 0.02000 0.01957 = 0.01940 -0.00312 0.00067 -0.00702 C74 1 0.325628 0.973515 0.320318 11.00000 0.08823 0.02596 = 0.03733 0.00382 0.00423 0.02019 AFIX 137 H74A 2 0.299836 0.966996 0.283747 11.00000 -1.50000 H74B 2 0.373976 0.982327 0.314399 11.00000 -1.50000 H74C 2 0.305469 1.007275 0.339593 11.00000 -1.50000 AFIX 0 C75 1 0.250470 0.903885 0.363810 11.00000 0.04808 0.03427 = 0.04628 -0.01121 -0.00904 0.02155 AFIX 137 H75A 2 0.248678 0.863714 0.380105 11.00000 -1.50000 H75B 2 0.222963 0.904789 0.327473 11.00000 -1.50000 H75C 2 0.231761 0.932848 0.389584 11.00000 -1.50000 AFIX 0 C76 1 0.533146 0.742035 0.589000 11.00000 0.01368 0.02953 = 0.01899 -0.00614 -0.00255 -0.00641 C77 1 0.526303 0.702413 0.633187 11.00000 0.02772 0.02520 = 0.01757 0.00298 -0.00204 -0.00251 AFIX 43 H77 2 0.547010 0.664012 0.631815 11.00000 -1.20000 AFIX 0 C78 1 0.490449 0.717174 0.678812 11.00000 0.02933 0.03573 = 0.02089 0.00421 -0.00005 -0.00970 AFIX 43 H78 2 0.487144 0.689176 0.708561 11.00000 -1.20000 AFIX 0 C79 1 0.458899 0.772808 0.681856 11.00000 0.02858 0.04695 = 0.02521 -0.00048 0.01270 -0.00405 AFIX 43 H79 2 0.433661 0.782867 0.713246 11.00000 -1.20000 AFIX 0 C80 1 0.464858 0.813051 0.638623 11.00000 0.02347 0.03193 = 0.02806 -0.00578 0.00134 0.00016 AFIX 43 H80 2 0.442940 0.850903 0.640399 11.00000 -1.20000 AFIX 0 C81 1 0.502405 0.799709 0.592009 11.00000 0.01624 0.03072 = 0.01277 -0.00276 0.00006 -0.00470 C82 1 0.505379 0.845662 0.549226 11.00000 0.01656 0.02090 = 0.02608 -0.00589 -0.00086 -0.00169 AFIX 43 H82 2 0.477555 0.880121 0.553160 11.00000 -1.20000 AFIX 0 C83 1 0.540078 0.890940 0.465387 11.00000 0.01841 0.01953 = 0.01856 -0.00247 -0.00121 -0.00158 C84 1 0.488708 0.933985 0.459744 11.00000 0.02433 0.02117 = 0.03059 -0.00445 0.00378 -0.00101 AFIX 43 H84 2 0.452329 0.933164 0.484298 11.00000 -1.20000 AFIX 0 C85 1 0.489424 0.977900 0.419224 11.00000 0.02874 0.02136 = 0.03258 -0.00377 -0.00161 0.00605 AFIX 43 H85 2 0.454127 1.007377 0.415963 11.00000 -1.20000 AFIX 0 C86 1 0.542228 0.978550 0.383304 11.00000 0.03732 0.01940 = 0.03023 0.00381 -0.00502 0.00024 AFIX 43 H86 2 0.543359 1.009098 0.355601 11.00000 -1.20000 AFIX 0 C87 1 0.593534 0.935314 0.387098 11.00000 0.02493 0.02317 = 0.02127 0.00301 0.00058 -0.00056 AFIX 43 H87 2 0.629222 0.936325 0.361896 11.00000 -1.20000 AFIX 0 C88 1 0.592993 0.890158 0.427907 11.00000 0.02358 0.02445 = 0.01511 -0.00323 -0.00124 0.00036 C89 1 0.694325 0.826604 0.332647 11.00000 0.01937 0.02076 = 0.01331 0.00098 0.00186 -0.00023 C90 1 0.630082 0.804762 0.315911 11.00000 0.01702 0.02818 = 0.02094 0.00268 0.00558 -0.00291 AFIX 43 H90 2 0.597285 0.798670 0.343052 11.00000 -1.20000 AFIX 0 C91 1 0.612597 0.791451 0.259392 11.00000 0.02272 0.04359 = 0.02160 -0.00063 0.00181 -0.00890 AFIX 43 H91 2 0.567627 0.777109 0.248034 11.00000 -1.20000 AFIX 0 C92 1 0.659723 0.798899 0.220222 11.00000 0.02652 0.03437 = 0.01191 0.00060 -0.00183 -0.00510 AFIX 43 H92 2 0.646578 0.790590 0.181672 11.00000 -1.20000 AFIX 0 C93 1 0.727321 0.818596 0.235599 11.00000 0.01896 0.01596 = 0.01912 0.00273 0.00039 0.00196 C94 1 0.777486 0.825444 0.194413 11.00000 0.02133 0.01662 = 0.02006 0.00442 0.00332 0.00637 C95 1 0.839575 0.851634 0.210382 11.00000 0.02405 0.02603 = 0.02462 0.00284 0.01030 -0.00041 AFIX 43 H95 2 0.871220 0.859835 0.182784 11.00000 -1.20000 AFIX 0 C96 1 0.857017 0.866490 0.266940 11.00000 0.01817 0.03407 = 0.02648 -0.00545 0.00416 -0.00708 AFIX 43 H96 2 0.901034 0.883571 0.276980 11.00000 -1.20000 AFIX 0 C97 1 0.813028 0.857277 0.307969 11.00000 0.02326 0.02972 = 0.01813 -0.00388 -0.00123 -0.00153 AFIX 43 H97 2 0.827103 0.866118 0.346246 11.00000 -1.20000 AFIX 0 C98 1 0.746186 0.834441 0.293246 11.00000 0.02294 0.01617 = 0.01887 0.00141 0.00039 0.00000 C99 1 0.752190 0.741763 0.130923 11.00000 0.04226 0.04701 = 0.02787 -0.01223 0.00001 -0.00753 AFIX 137 H99A 2 0.726633 0.724853 0.161183 11.00000 -1.50000 H99B 2 0.798495 0.724145 0.132395 11.00000 -1.50000 H99C 2 0.727631 0.732881 0.094300 11.00000 -1.50000 AFIX 0 C100 1 0.799909 0.831601 0.095489 11.00000 0.04002 0.05171 = 0.02442 0.00374 0.00715 -0.00476 AFIX 137 H10A 2 0.846883 0.815530 0.101013 11.00000 -1.50000 H10B 2 0.801397 0.875264 0.098785 11.00000 -1.50000 H10C 2 0.779674 0.820468 0.057892 11.00000 -1.50000 AFIX 0 C101 1 0.561625 0.467320 0.755040 11.00000 0.05695 0.05719 = 0.03211 0.00608 -0.00352 -0.00757 AFIX 137 H10D 2 0.573566 0.434539 0.730198 11.00000 -1.50000 H10E 2 0.547541 0.450883 0.790643 11.00000 -1.50000 H10F 2 0.601886 0.493296 0.762705 11.00000 -1.50000 AFIX 0 C102 1 0.505337 0.501638 0.727832 11.00000 0.04236 0.07113 = 0.03796 -0.00452 0.00922 0.00240 C103 1 0.705173 0.693664 0.687300 11.00000 0.07567 0.05048 = 0.06546 -0.01388 -0.00715 -0.00512 AFIX 137 H10G 2 0.692403 0.690940 0.646662 11.00000 -1.50000 H10H 2 0.754993 0.687254 0.694423 11.00000 -1.50000 H10I 2 0.693104 0.733370 0.700953 11.00000 -1.50000 AFIX 0 C104 1 0.668708 0.649043 0.716289 11.00000 0.06233 0.04049 = 0.05128 -0.00946 -0.00949 0.00873 C105 1 0.049760 0.564016 0.737318 11.00000 0.04868 0.05759 = 0.03831 -0.01494 0.00303 0.00231 AFIX 137 H10J 2 0.088604 0.538283 0.750335 11.00000 -1.50000 H10K 2 0.029260 0.581458 0.769999 11.00000 -1.50000 H10L 2 0.066256 0.596080 0.713652 11.00000 -1.50000 AFIX 0 C106 1 -0.000469 0.529742 0.705551 11.00000 0.04003 0.06980 = 0.04122 -0.01838 0.00755 -0.00315 C107 1 0.302283 0.986384 0.504904 11.00000 0.07857 0.03865 = 0.04567 -0.00759 -0.01524 0.01367 AFIX 137 H10M 2 0.326713 0.982271 0.470502 11.00000 -1.50000 H10N 2 0.315527 1.024133 0.523678 11.00000 -1.50000 H10O 2 0.252357 0.986180 0.495042 11.00000 -1.50000 AFIX 0 C108 1 0.320340 0.937116 0.542470 11.00000 0.04902 0.03082 = 0.03817 -0.00892 0.00010 0.00768 C109 1 0.193402 0.323265 0.718834 11.00000 0.07169 0.08816 = 0.07916 0.04354 0.00244 -0.01307 AFIX 137 H10P 2 0.177667 0.284469 0.732105 11.00000 -1.50000 H10Q 2 0.240799 0.330613 0.734490 11.00000 -1.50000 H10R 2 0.192056 0.323082 0.677506 11.00000 -1.50000 AFIX 0 C110 1 0.149033 0.369557 0.736983 11.00000 0.07306 0.07062 = 0.07238 0.03260 -0.00179 -0.02532 N1 3 0.938525 0.590216 0.452899 11.00000 0.02230 0.01541 = 0.02088 -0.00289 0.00563 -0.00344 N2 3 0.972466 0.663960 0.538417 11.00000 0.01809 0.01838 = 0.02019 -0.00477 0.00036 -0.00082 N3 3 1.173786 0.946979 0.623294 11.00000 0.02564 0.02362 = 0.04215 0.00020 -0.01452 -0.00673 N4 3 0.909070 0.856894 0.486964 11.00000 0.02113 0.02607 = 0.02255 0.00420 0.00140 0.00112 N5 3 0.797859 0.856805 0.544706 11.00000 0.01945 0.02112 = 0.01773 -0.00440 0.00541 -0.00140 N6 3 0.719510 0.834736 0.851615 11.00000 0.03316 0.03358 = 0.02148 -0.00296 0.00352 -0.00450 N7 3 0.541919 0.576084 0.547025 11.00000 0.03018 0.01788 = 0.01782 0.00102 0.00255 0.00251 N8 3 0.500965 0.631671 0.452200 11.00000 0.01834 0.02103 = 0.01818 0.00160 0.00294 0.00056 N9 3 0.322020 0.919243 0.355268 11.00000 0.04266 0.02308 = 0.03536 0.00092 0.00306 0.01067 N10 3 0.542596 0.844153 0.505912 11.00000 0.01875 0.02308 = 0.01745 0.00077 0.00032 -0.00487 N11 3 0.641306 0.842858 0.434846 11.00000 0.01740 0.02234 = 0.01506 0.00304 0.00344 0.00080 N12 3 0.757930 0.807120 0.138287 11.00000 0.02627 0.03525 = 0.01413 0.00010 0.00668 -0.00101 N13 3 0.461079 0.526996 0.705225 11.00000 0.05723 0.10967 = 0.06353 -0.01096 -0.00769 0.02492 N14 3 0.638833 0.613766 0.740104 11.00000 0.06410 0.05508 = 0.05921 -0.00430 -0.00893 0.00683 N15 3 -0.039946 0.501953 0.678906 11.00000 0.05743 0.09717 = 0.06285 -0.02463 -0.00048 -0.01647 N16 3 0.334783 0.898046 0.571196 11.00000 0.05550 0.04359 = 0.04393 0.00079 0.00951 0.01105 N17 3 0.110204 0.404570 0.752041 11.00000 0.08714 0.06932 = 0.08374 0.02574 -0.00124 -0.02364 O1 4 0.798650 0.630143 0.444621 11.00000 0.02481 0.02800 = 0.03197 -0.01541 -0.00288 0.00167 O2 4 0.916989 0.734830 0.599379 11.00000 0.01884 0.03540 = 0.02939 -0.01418 -0.00210 0.00370 O3 4 1.016019 0.678156 0.640532 11.00000 0.02325 0.02735 = 0.02009 0.00068 -0.00067 -0.00260 O4 4 0.893871 0.742477 0.439240 11.00000 0.02544 0.02308 = 0.02514 0.00011 0.00240 0.00265 O5 4 0.685849 0.902968 0.571435 11.00000 0.02228 0.02330 = 0.02781 0.00019 0.00084 0.00374 O6 4 0.698061 0.794664 0.559067 11.00000 0.02036 0.02096 = 0.01766 -0.00291 -0.00068 -0.00336 O7 4 0.678568 0.620579 0.538463 11.00000 0.02292 0.02564 = 0.03157 0.00797 -0.00461 0.00334 O8 4 0.443580 0.633086 0.352462 11.00000 0.02030 0.02478 = 0.01876 -0.00509 -0.00382 -0.00082 O9 4 0.550966 0.686942 0.376240 11.00000 0.01867 0.02774 = 0.01857 0.00253 0.00016 -0.00312 O10 4 0.568451 0.726381 0.545436 11.00000 0.02217 0.02220 = 0.01573 0.00014 0.00444 -0.00049 O11 4 0.746106 0.900588 0.409878 11.00000 0.02289 0.02388 = 0.02043 -0.00314 0.00201 -0.00221 O12 4 0.752586 0.793208 0.428866 11.00000 0.01848 0.02486 = 0.01609 -0.00025 0.00132 0.00264 O13 4 0.814822 0.713517 0.520945 11.00000 0.02321 0.02306 = 0.02111 -0.00387 -0.00346 -0.00045 H13O 2 0.824462 0.716110 0.552753 11.00000 0.03150 O14 4 0.646063 0.704073 0.463500 11.00000 0.01590 0.02291 = 0.01714 -0.00032 -0.00067 -0.00039 H14O 2 0.633121 0.704766 0.431423 11.00000 0.03899 S1 5 0.983190 0.707276 0.591552 11.00000 0.01949 0.02192 = 0.01929 -0.00332 -0.00211 0.00019 S2 5 0.730361 0.851409 0.577691 11.00000 0.02034 0.02169 = 0.01968 -0.00164 -0.00013 0.00007 S3 5 0.485320 0.666576 0.394250 11.00000 0.01874 0.01989 = 0.01816 -0.00029 -0.00006 -0.00088 S4 5 0.711329 0.844072 0.405431 11.00000 0.01989 0.02138 = 0.01628 -0.00119 0.00032 -0.00167 ZN1 6 0.890192 0.665400 0.479578 11.00000 0.01910 0.01894 = 0.02219 -0.00452 -0.00260 0.00076 ZN2 6 0.832962 0.794992 0.489011 11.00000 0.02143 0.02101 = 0.02033 -0.00293 0.00048 0.00083 ZN3 6 0.619593 0.783940 0.496731 11.00000 0.01792 0.01978 = 0.01671 0.00026 0.00133 -0.00028 ZN4 6 0.582563 0.648017 0.508746 11.00000 0.02108 0.01926 = 0.01964 0.00193 -0.00053 -0.00025 ZN5 6 0.733663 0.670112 0.490812 11.00000 0.01806 0.02617 = 0.02915 -0.00180 -0.00143 0.00076 HKLF 4 REM be67mj1n in P 1 21/n 1 REM R1 = 0.0469 for 12664 Fo > 4sig(Fo) and 0.0871 for all 19514 data REM 1372 parameters refined using 97 restraints END WGHT 0.0418 0.0000 REM Highest difference peak 0.813, deepest hole -0.578, 1-sigma level 0.084 Q1 1 0.7486 0.7095 0.4803 11.00000 0.05 0.81 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7885(2) 0.58666(15) 0.40563(16) 0.0233(9) Uani 1 1 d . . . C2 C 0.7233(2) 0.58007(15) 0.37716(17) 0.0281(10) Uani 1 1 d . . . H2 H 0.6872 0.607 0.3846 0.034 Uiso 1 1 calc R . . C3 C 0.7109(2) 0.53409(16) 0.33774(16) 0.0294(10) Uani 1 1 d . . . H3 H 0.6664 0.5299 0.3185 0.035 Uiso 1 1 calc R . . C4 C 0.7629(2) 0.49475(17) 0.32665(18) 0.0329(11) Uani 1 1 d . . . H4 H 0.7543 0.4632 0.3003 0.039 Uiso 1 1 calc R . . C5 C 0.8266(2) 0.50172(15) 0.35395(17) 0.0299(10) Uani 1 1 d . . . H5 H 0.8622 0.4746 0.3459 0.036 Uiso 1 1 calc R . . C6 C 0.8419(2) 0.54756(14) 0.39365(16) 0.0218(9) Uani 1 1 d . . . C7 C 0.9108(2) 0.54927(15) 0.42068(16) 0.0238(10) Uani 1 1 d . . . H7 H 0.9393 0.5159 0.4139 0.029 Uiso 1 1 calc R . . C8 C 1.0072(2) 0.58563(14) 0.47795(16) 0.0200(9) Uani 1 1 d . . . C9 C 1.0562(2) 0.54615(14) 0.45921(17) 0.0251(10) Uani 1 1 d . . . H9 H 1.0441 0.5204 0.4282 0.03 Uiso 1 1 calc R . . C10 C 1.1220(2) 0.54436(15) 0.48539(18) 0.0281(10) Uani 1 1 d . . . H10 H 1.1549 0.517 0.4728 0.034 Uiso 1 1 calc R . . C11 C 1.1400(2) 0.58234(14) 0.52993(17) 0.0245(10) Uani 1 1 d . . . H11 H 1.1856 0.5814 0.5475 0.029 Uiso 1 1 calc R . . C12 C 1.0922(2) 0.62179(14) 0.54930(17) 0.0234(9) Uani 1 1 d . . . H12 H 1.1052 0.6475 0.5801 0.028 Uiso 1 1 calc R . . C13 C 1.02490(19) 0.62393(14) 0.52365(15) 0.0166(9) Uani 1 1 d . . . C14 C 1.03903(19) 0.76669(14) 0.57340(16) 0.0191(9) Uani 1 1 d . . . C15 C 1.0646(2) 0.76764(15) 0.52168(17) 0.0244(10) Uani 1 1 d . . . H15 H 1.0503 0.738 0.4946 0.029 Uiso 1 1 calc R . . C16 C 1.1120(2) 0.81192(16) 0.50770(17) 0.0287(10) Uani 1 1 d . . . H16 H 1.1303 0.8115 0.4717 0.034 Uiso 1 1 calc R . . C17 C 1.1317(2) 0.85548(16) 0.54598(18) 0.0309(11) Uani 1 1 d . . . H17 H 1.1638 0.8851 0.5363 0.037 Uiso 1 1 calc R . . C18 C 1.1051(2) 0.85708(15) 0.59975(17) 0.0239(10) Uani 1 1 d . . . C19 C 1.1275(2) 0.90230(15) 0.64003(18) 0.0256(10) Uani 1 1 d . . . C20 C 1.1052(2) 0.89939(16) 0.69314(19) 0.0350(11) Uani 1 1 d . . . H20 H 1.1217 0.9278 0.7207 0.042 Uiso 1 1 calc R . . C21 C 1.0581(2) 0.85487(15) 0.70795(18) 0.0332(11) Uani 1 1 d . . . H21 H 1.0431 0.854 0.7451 0.04 Uiso 1 1 calc R . . C22 C 1.0339(2) 0.81310(15) 0.66927(17) 0.0251(10) Uani 1 1 d . . . H22 H 1.0004 0.7847 0.6791 0.03 Uiso 1 1 calc R . . C23 C 1.0583(2) 0.81205(14) 0.61495(16) 0.0212(9) Uani 1 1 d . . . C24 C 1.1390(2) 0.99354(17) 0.5877(2) 0.0504(14) Uani 1 1 d . . . H24A H 1.1077 1.0163 0.61 0.076 Uiso 1 1 calc R . . H24B H 1.1126 0.9748 0.5556 0.076 Uiso 1 1 calc R . . H24C H 1.1737 1.0205 0.5737 0.076 Uiso 1 1 calc R . . C25 C 1.2180(2) 0.97383(17) 0.66845(19) 0.0421(13) Uani 1 1 d . . . H25A H 1.2401 0.9423 0.6921 0.063 Uiso 1 1 calc R . . H25B H 1.1902 0.9993 0.6915 0.063 Uiso 1 1 calc R . . H25C H 1.2536 0.9981 0.6522 0.063 Uiso 1 1 calc R . . C26 C 0.9400(2) 0.76009(16) 0.40416(17) 0.0235(9) Uani 1 1 d . . . C27 C 0.9636(2) 0.72052(16) 0.36366(17) 0.0297(10) Uani 1 1 d . . . H27 H 0.9468 0.6806 0.3621 0.036 Uiso 1 1 calc R . . C28 C 1.0101(2) 0.73837(18) 0.32657(19) 0.0394(12) Uani 1 1 d . . . H28 H 1.0243 0.711 0.2992 0.047 Uiso 1 1 calc R . . C29 C 1.0372(2) 0.79639(18) 0.32845(18) 0.0382(12) Uani 1 1 d . . . H29 H 1.0699 0.8086 0.303 0.046 Uiso 1 1 calc R . . C30 C 1.0153(2) 0.83495(18) 0.36780(18) 0.0329(11) Uani 1 1 d . . . H30 H 1.0333 0.8745 0.3691 0.039 Uiso 1 1 calc R . . C31 C 0.9676(2) 0.81877(15) 0.40633(17) 0.0248(10) Uani 1 1 d . . . C32 C 0.9529(2) 0.86231(16) 0.44809(18) 0.0274(10) Uani 1 1 d . . . H32 H 0.9776 0.8989 0.4474 0.033 Uiso 1 1 calc R . . C33 C 0.9044(2) 0.90370(14) 0.52719(17) 0.0233(9) Uani 1 1 d . . . C34 C 0.9575(2) 0.94370(15) 0.54183(17) 0.0297(10) Uani 1 1 d . . . H34 H 1.0002 0.9401 0.5251 0.036 Uiso 1 1 calc R . . C35 C 0.9486(2) 0.98857(16) 0.58039(18) 0.0325(11) Uani 1 1 d . . . H35 H 0.985 1.0159 0.59 0.039 Uiso 1 1 calc R . . C36 C 0.8872(2) 0.99362(15) 0.60477(18) 0.0308(11) Uani 1 1 d . . . H36 H 0.8803 1.0258 0.6298 0.037 Uiso 1 1 calc R . . C37 C 0.8353(2) 0.95212(14) 0.59315(16) 0.0242(10) Uani 1 1 d . . . H37 H 0.7933 0.9556 0.611 0.029 Uiso 1 1 calc R . . C38 C 0.8437(2) 0.90538(15) 0.55575(16) 0.0221(9) Uani 1 1 d . . . C39 C 0.7563(2) 0.84250(14) 0.65031(16) 0.0202(9) Uani 1 1 d . . . C40 C 0.8239(2) 0.82679(14) 0.66389(16) 0.0231(9) Uani 1 1 d . . . H40 H 0.8534 0.819 0.6346 0.028 Uiso 1 1 calc R . . C41 C 0.8497(2) 0.82211(15) 0.72023(17) 0.0264(10) Uani 1 1 d . . . H41 H 0.8971 0.813 0.729 0.032 Uiso 1 1 calc R . . C42 C 0.8074(2) 0.83052(15) 0.76279(17) 0.0265(10) Uani 1 1 d . . . H42 H 0.8259 0.8281 0.8009 0.032 Uiso 1 1 calc R . . C43 C 0.7365(2) 0.84273(14) 0.75092(16) 0.0213(9) Uani 1 1 d . . . C44 C 0.6918(2) 0.84922(14) 0.79602(17) 0.0236(9) Uani 1 1 d . . . C45 C 0.6267(2) 0.87186(15) 0.78391(18) 0.0301(10) Uani 1 1 d . . . H45 H 0.5986 0.8807 0.8138 0.036 Uiso 1 1 calc R . . C46 C 0.6014(2) 0.88207(15) 0.72841(18) 0.0289(10) Uani 1 1 d . . . H46 H 0.5561 0.8976 0.7213 0.035 Uiso 1 1 calc R . . C47 C 0.6398(2) 0.87054(14) 0.68354(18) 0.0250(10) Uani 1 1 d . . . H47 H 0.62 0.8748 0.6459 0.03 Uiso 1 1 calc R . . C48 C 0.7099(2) 0.85205(14) 0.69413(16) 0.0202(9) Uani 1 1 d . . . C49 C 0.6823(2) 0.85869(17) 0.89753(18) 0.0393(12) Uani 1 1 d . . . H49A H 0.6368 0.8398 0.8972 0.059 Uiso 1 1 calc R . . H49B H 0.6767 0.902 0.8927 0.059 Uiso 1 1 calc R . . H49C H 0.7085 0.8504 0.9336 0.059 Uiso 1 1 calc R . . C50 C 0.7325(2) 0.77104(16) 0.86033(18) 0.0379(11) Uani 1 1 d . . . H50A H 0.757 0.7552 0.829 0.057 Uiso 1 1 calc R . . H50B H 0.6885 0.75 0.862 0.057 Uiso 1 1 calc R . . H50C H 0.7608 0.7651 0.8959 0.057 Uiso 1 1 calc R . . C51 C 0.6964(2) 0.57988(15) 0.57918(16) 0.0250(10) Uani 1 1 d . . . C52 C 0.7655(2) 0.57433(16) 0.59931(18) 0.0339(11) Uani 1 1 d . . . H52 H 0.7991 0.5993 0.5843 0.041 Uiso 1 1 calc R . . C53 C 0.7862(2) 0.53290(16) 0.64101(18) 0.0361(12) Uani 1 1 d . . . H53 H 0.8335 0.53 0.6543 0.043 Uiso 1 1 calc R . . C54 C 0.7375(3) 0.49581(17) 0.66304(18) 0.0395(12) Uani 1 1 d . . . H54 H 0.7509 0.4675 0.6916 0.047 Uiso 1 1 calc R . . C55 C 0.6701(2) 0.50069(16) 0.64293(17) 0.0321(11) Uani 1 1 d . . . H55 H 0.6374 0.4746 0.6577 0.038 Uiso 1 1 calc R . . C56 C 0.6465(2) 0.54257(15) 0.60122(16) 0.0253(10) Uani 1 1 d . . . C57 C 0.5743(2) 0.53982(15) 0.58176(16) 0.0252(10) Uani 1 1 d . . . H57 H 0.5482 0.5081 0.596 0.03 Uiso 1 1 calc R . . C58 C 0.4713(2) 0.56838(14) 0.52764(17) 0.0219(9) Uani 1 1 d . . . C59 C 0.4243(2) 0.53497(15) 0.55661(17) 0.0272(10) Uani 1 1 d . . . H59 H 0.4394 0.5148 0.5905 0.033 Uiso 1 1 calc R . . C60 C 0.3560(2) 0.53124(16) 0.53601(18) 0.0302(10) Uani 1 1 d . . . H60 H 0.3244 0.508 0.5553 0.036 Uiso 1 1 calc R . . C61 C 0.3340(2) 0.56141(15) 0.48736(18) 0.0277(10) Uani 1 1 d . . . H61 H 0.2869 0.559 0.4733 0.033 Uiso 1 1 calc R . . C62 C 0.3798(2) 0.59507(14) 0.45882(17) 0.0233(9) Uani 1 1 d . . . H62 H 0.3635 0.6161 0.4257 0.028 Uiso 1 1 calc R . . C63 C 0.4491(2) 0.59862(14) 0.47777(16) 0.0206(9) Uani 1 1 d . . . C64 C 0.43707(19) 0.73207(14) 0.40970(16) 0.0174(9) Uani 1 1 d . . . C65 C 0.41672(19) 0.73900(14) 0.46284(16) 0.0201(9) Uani 1 1 d . . . H65 H 0.4286 0.7096 0.4908 0.024 Uiso 1 1 calc R . . C66 C 0.37791(19) 0.78975(14) 0.47670(16) 0.0209(9) Uani 1 1 d . . . H66 H 0.3635 0.7943 0.5138 0.025 Uiso 1 1 calc R . . C67 C 0.3614(2) 0.83184(15) 0.43684(17) 0.0242(10) Uani 1 1 d . . . H67 H 0.3362 0.8662 0.4467 0.029 Uiso 1 1 calc R . . C68 C 0.3808(2) 0.82571(14) 0.38081(16) 0.0220(9) Uani 1 1 d . . . C69 C 0.3623(2) 0.87049(15) 0.33861(18) 0.0278(10) Uani 1 1 d . . . C70 C 0.3862(2) 0.86497(15) 0.28638(18) 0.0323(11) Uani 1 1 d . . . H70 H 0.3754 0.8951 0.2589 0.039 Uiso 1 1 calc R . . C71 C 0.4265(2) 0.81589(15) 0.27229(18) 0.0287(10) Uani 1 1 d . . . H71 H 0.442 0.8129 0.2354 0.034 Uiso 1 1 calc R . . C72 C 0.4436(2) 0.77219(15) 0.31149(17) 0.0241(10) Uani 1 1 d . . . H72 H 0.4711 0.7393 0.3015 0.029 Uiso 1 1 calc R . . C73 C 0.42094(19) 0.77557(14) 0.36645(16) 0.0197(9) Uani 1 1 d . . . C74 C 0.3256(3) 0.97352(16) 0.32032(19) 0.0505(15) Uani 1 1 d . . . H74A H 0.2998 0.967 0.2837 0.076 Uiso 1 1 calc R . . H74B H 0.374 0.9823 0.3144 0.076 Uiso 1 1 calc R . . H74C H 0.3055 1.0073 0.3396 0.076 Uiso 1 1 calc R . . C75 C 0.2505(2) 0.90389(17) 0.36381(19) 0.0435(13) Uani 1 1 d . . . H75A H 0.2487 0.8637 0.3801 0.065 Uiso 1 1 calc R . . H75B H 0.223 0.9048 0.3275 0.065 Uiso 1 1 calc R . . H75C H 0.2318 0.9328 0.3896 0.065 Uiso 1 1 calc R . . C76 C 0.53315(19) 0.74203(15) 0.58900(16) 0.0209(9) Uani 1 1 d . . . C77 C 0.5263(2) 0.70241(15) 0.63319(16) 0.0237(9) Uani 1 1 d . . . H77 H 0.547 0.664 0.6318 0.028 Uiso 1 1 calc R . . C78 C 0.4904(2) 0.71717(16) 0.67881(17) 0.0287(10) Uani 1 1 d . . . H78 H 0.4871 0.6892 0.7086 0.034 Uiso 1 1 calc R . . C79 C 0.4589(2) 0.77281(17) 0.68186(18) 0.0330(11) Uani 1 1 d . . . H79 H 0.4337 0.7829 0.7132 0.04 Uiso 1 1 calc R . . C80 C 0.4649(2) 0.81305(16) 0.63862(17) 0.0279(10) Uani 1 1 d . . . H80 H 0.4429 0.8509 0.6404 0.033 Uiso 1 1 calc R . . C81 C 0.50241(19) 0.79971(15) 0.59201(16) 0.0200(9) Uani 1 1 d . . . C82 C 0.5054(2) 0.84566(14) 0.54923(17) 0.0213(9) Uani 1 1 d . . . H82 H 0.4776 0.8801 0.5532 0.026 Uiso 1 1 calc R . . C83 C 0.54008(19) 0.89094(14) 0.46539(16) 0.0190(9) Uani 1 1 d . . . C84 C 0.4887(2) 0.93399(14) 0.45974(17) 0.0253(10) Uani 1 1 d . . . H84 H 0.4523 0.9332 0.4843 0.03 Uiso 1 1 calc R . . C85 C 0.4894(2) 0.97790(15) 0.41922(17) 0.0278(10) Uani 1 1 d . . . H85 H 0.4541 1.0074 0.416 0.033 Uiso 1 1 calc R . . C86 C 0.5422(2) 0.97855(15) 0.38330(18) 0.0294(11) Uani 1 1 d . . . H86 H 0.5434 1.0091 0.3556 0.035 Uiso 1 1 calc R . . C87 C 0.5935(2) 0.93531(14) 0.38710(16) 0.0232(9) Uani 1 1 d . . . H87 H 0.6292 0.9363 0.3619 0.028 Uiso 1 1 calc R . . C88 C 0.5930(2) 0.89016(15) 0.42791(16) 0.0212(9) Uani 1 1 d . . . C89 C 0.6943(2) 0.82660(14) 0.33265(15) 0.0178(9) Uani 1 1 d . . . C90 C 0.6301(2) 0.80476(15) 0.31591(16) 0.0218(9) Uani 1 1 d . . . H90 H 0.5973 0.7987 0.3431 0.026 Uiso 1 1 calc R . . C91 C 0.6126(2) 0.79145(16) 0.25939(17) 0.0293(10) Uani 1 1 d . . . H91 H 0.5676 0.7771 0.248 0.035 Uiso 1 1 calc R . . C92 C 0.6597(2) 0.79890(15) 0.22022(16) 0.0244(9) Uani 1 1 d . . . H92 H 0.6466 0.7906 0.1817 0.029 Uiso 1 1 calc R . . C93 C 0.7273(2) 0.81860(13) 0.23560(16) 0.0181(9) Uani 1 1 d . . . C94 C 0.7775(2) 0.82544(14) 0.19441(16) 0.0192(9) Uani 1 1 d . . . C95 C 0.8396(2) 0.85163(14) 0.21038(17) 0.0245(9) Uani 1 1 d . . . H95 H 0.8712 0.8598 0.1828 0.029 Uiso 1 1 calc R . . C96 C 0.8570(2) 0.86649(15) 0.26694(17) 0.0261(10) Uani 1 1 d . . . H96 H 0.901 0.8836 0.277 0.031 Uiso 1 1 calc R . . C97 C 0.8130(2) 0.85728(15) 0.30797(17) 0.0238(9) Uani 1 1 d . . . H97 H 0.8271 0.8661 0.3462 0.029 Uiso 1 1 calc R . . C98 C 0.7462(2) 0.83444(14) 0.29325(16) 0.0194(9) Uani 1 1 d . . . C99 C 0.7522(2) 0.74176(17) 0.13092(18) 0.0392(12) Uani 1 1 d . . . H99A H 0.7266 0.7249 0.1612 0.059 Uiso 1 1 calc R . . H99B H 0.7985 0.7241 0.1324 0.059 Uiso 1 1 calc R . . H99C H 0.7276 0.7329 0.0943 0.059 Uiso 1 1 calc R . . C100 C 0.7999(2) 0.83160(18) 0.09549(18) 0.0385(11) Uani 1 1 d . . . H10A H 0.8469 0.8155 0.101 0.058 Uiso 1 1 calc R . . H10B H 0.8014 0.8753 0.0988 0.058 Uiso 1 1 calc R . . H10C H 0.7797 0.8205 0.0579 0.058 Uiso 1 1 calc R . . C101 C 0.5616(3) 0.46732(19) 0.75504(19) 0.0491(13) Uani 1 1 d . . . H10D H 0.5736 0.4345 0.7302 0.074 Uiso 1 1 calc R . . H10E H 0.5475 0.4509 0.7906 0.074 Uiso 1 1 calc R . . H10F H 0.6019 0.4933 0.7627 0.074 Uiso 1 1 calc R . . C102 C 0.5053(3) 0.5016(2) 0.7278(2) 0.0502(14) Uani 1 1 d . . . C103 C 0.7052(3) 0.6937(2) 0.6873(2) 0.0645(13) Uani 1 1 d U . . H10G H 0.6924 0.6909 0.6467 0.097 Uiso 1 1 calc R . . H10H H 0.755 0.6873 0.6944 0.097 Uiso 1 1 calc R . . H10I H 0.6931 0.7334 0.701 0.097 Uiso 1 1 calc R . . C104 C 0.6687(3) 0.6490(2) 0.7163(2) 0.0521(12) Uani 1 1 d U . . C105 C 0.0498(2) 0.56402(19) 0.7373(2) 0.0482(12) Uani 1 1 d U . . H10J H 0.0886 0.5383 0.7503 0.072 Uiso 1 1 calc R . . H10K H 0.0293 0.5815 0.77 0.072 Uiso 1 1 calc R . . H10L H 0.0663 0.5961 0.7137 0.072 Uiso 1 1 calc R . . C106 C -0.0005(3) 0.5297(2) 0.7056(2) 0.0501(12) Uani 1 1 d U . . C107 C 0.3023(3) 0.98638(18) 0.5049(2) 0.0553(13) Uani 1 1 d U . . H10M H 0.3267 0.9823 0.4705 0.083 Uiso 1 1 calc R . . H10N H 0.3155 1.0241 0.5237 0.083 Uiso 1 1 calc R . . H10O H 0.2524 0.9862 0.495 0.083 Uiso 1 1 calc R . . C108 C 0.3203(2) 0.93712(17) 0.54247(19) 0.0395(11) Uani 1 1 d U . . C109 C 0.1934(3) 0.3233(2) 0.7188(3) 0.0798(15) Uani 1 1 d U . . H10P H 0.1777 0.2845 0.7321 0.12 Uiso 1 1 calc R . . H10Q H 0.2408 0.3306 0.7345 0.12 Uiso 1 1 calc R . . H10R H 0.1921 0.3231 0.6775 0.12 Uiso 1 1 calc R . . C110 C 0.1490(3) 0.3696(3) 0.7370(3) 0.0724(15) Uani 1 1 d U . . N1 N 0.93852(16) 0.59022(11) 0.45290(13) 0.0193(7) Uani 1 1 d . . . N2 N 0.97247(16) 0.66396(11) 0.53842(13) 0.0189(7) Uani 1 1 d . . . N3 N 1.17379(17) 0.94698(12) 0.62329(15) 0.0313(9) Uani 1 1 d . . . N4 N 0.90907(17) 0.85689(12) 0.48696(14) 0.0233(8) Uani 1 1 d . . . N5 N 0.79786(16) 0.85681(11) 0.54471(13) 0.0192(7) Uani 1 1 d . . . N6 N 0.71951(18) 0.83474(13) 0.85162(14) 0.0293(8) Uani 1 1 d . . . N7 N 0.54192(17) 0.57608(11) 0.54702(13) 0.0219(8) Uani 1 1 d . . . N8 N 0.50097(16) 0.63167(11) 0.45220(13) 0.0191(7) Uani 1 1 d . . . N9 N 0.3220(2) 0.91924(13) 0.35527(14) 0.0337(9) Uani 1 1 d . . . N10 N 0.54260(16) 0.84415(12) 0.50591(13) 0.0198(7) Uani 1 1 d . . . N11 N 0.64131(16) 0.84286(11) 0.43485(12) 0.0182(7) Uani 1 1 d . . . N12 N 0.75793(17) 0.80712(13) 0.13829(13) 0.0250(8) Uani 1 1 d . . . N13 N 0.4611(3) 0.5270(2) 0.7052(2) 0.0774(16) Uani 1 1 d . . . N14 N 0.6388(2) 0.61377(18) 0.74010(19) 0.0602(11) Uani 1 1 d U . . N15 N -0.0399(2) 0.5020(2) 0.6789(2) 0.0727(13) Uani 1 1 d U . . N16 N 0.3348(2) 0.89805(15) 0.57120(16) 0.0474(10) Uani 1 1 d U . . N17 N 0.1102(3) 0.4046(2) 0.7520(2) 0.0805(14) Uani 1 1 d U . . O1 O 0.79865(13) 0.63014(10) 0.44462(11) 0.0285(7) Uani 1 1 d . . . O2 O 0.91699(13) 0.73483(10) 0.59938(11) 0.0281(7) Uani 1 1 d . . . O3 O 1.01602(13) 0.67816(10) 0.64053(11) 0.0237(6) Uani 1 1 d . . . O4 O 0.89387(14) 0.74248(10) 0.43924(11) 0.0245(6) Uani 1 1 d . . . O5 O 0.68585(13) 0.90297(9) 0.57144(11) 0.0245(6) Uani 1 1 d . . . O6 O 0.69806(13) 0.79466(9) 0.55907(10) 0.0198(6) Uani 1 1 d . . . O7 O 0.67857(13) 0.62058(10) 0.53846(11) 0.0271(7) Uani 1 1 d . . . O8 O 0.44358(13) 0.63309(9) 0.35246(10) 0.0216(6) Uani 1 1 d . . . O9 O 0.55097(13) 0.68694(10) 0.37624(10) 0.0217(6) Uani 1 1 d . . . O10 O 0.56845(13) 0.72638(9) 0.54544(10) 0.0199(6) Uani 1 1 d . . . O11 O 0.74611(13) 0.90059(9) 0.40988(10) 0.0224(6) Uani 1 1 d . . . O12 O 0.75259(13) 0.79321(9) 0.42887(10) 0.0198(6) Uani 1 1 d . . . O13 O 0.81482(15) 0.71352(10) 0.52095(13) 0.0227(7) Uani 1 1 d . . . H13O H 0.824(2) 0.7161(17) 0.5528(17) 0.032(14) Uiso 1 1 d . . . O14 O 0.64606(14) 0.70407(10) 0.46350(12) 0.0188(6) Uani 1 1 d D . . H14O H 0.633(2) 0.7048(17) 0.4314(9) 0.039(15) Uiso 1 1 d D . . S1 S 0.98319(5) 0.70728(4) 0.59155(4) 0.0204(2) Uani 1 1 d . . . S2 S 0.73036(5) 0.85141(4) 0.57769(4) 0.0207(2) Uani 1 1 d . . . S3 S 0.48532(5) 0.66658(4) 0.39425(4) 0.0190(2) Uani 1 1 d . . . S4 S 0.71133(5) 0.84407(4) 0.40543(4) 0.0192(2) Uani 1 1 d . . . Zn1 Zn 0.89019(2) 0.665400(17) 0.479578(19) 0.02029(11) Uani 1 1 d . . . Zn2 Zn 0.83296(2) 0.794992(17) 0.489011(19) 0.02098(12) Uani 1 1 d . . . Zn3 Zn 0.61959(2) 0.783940(16) 0.496731(18) 0.01814(11) Uani 1 1 d . . . Zn4 Zn 0.58256(2) 0.648017(16) 0.508746(19) 0.02010(11) Uani 1 1 d . . . Zn5 Zn 0.73366(2) 0.670112(18) 0.49081(2) 0.02462(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(3) 0.0260(19) 0.019(2) 0.0004(17) -0.0023(19) -0.0106(17) C2 0.023(3) 0.028(2) 0.033(3) 0.0032(18) 0.000(2) -0.0033(18) C3 0.034(3) 0.036(2) 0.017(2) 0.0050(18) -0.007(2) -0.017(2) C4 0.042(3) 0.030(2) 0.026(3) -0.0048(18) -0.001(2) -0.015(2) C5 0.037(3) 0.026(2) 0.026(3) -0.0056(18) 0.003(2) -0.0048(19) C6 0.029(3) 0.0208(18) 0.016(2) -0.0019(16) 0.0040(19) -0.0028(17) C7 0.028(3) 0.0204(18) 0.023(2) -0.0013(16) 0.005(2) -0.0020(17) C8 0.018(2) 0.0186(17) 0.024(2) 0.0035(16) 0.0021(19) 0.0007(16) C9 0.030(3) 0.0197(18) 0.026(3) 0.0007(17) 0.008(2) -0.0010(17) C10 0.023(3) 0.0211(19) 0.041(3) 0.0022(18) 0.009(2) 0.0056(17) C11 0.014(2) 0.0237(19) 0.035(3) 0.0086(18) 0.000(2) 0.0015(16) C12 0.023(3) 0.0201(18) 0.027(3) 0.0002(16) 0.002(2) -0.0010(17) C13 0.018(2) 0.0160(16) 0.016(2) 0.0048(15) 0.0021(18) -0.0017(15) C14 0.017(2) 0.0204(17) 0.019(2) -0.0027(16) -0.0044(18) 0.0028(16) C15 0.029(3) 0.0236(19) 0.019(2) -0.0004(16) -0.005(2) 0.0006(17) C16 0.030(3) 0.033(2) 0.023(3) 0.0051(18) 0.000(2) -0.0046(19) C17 0.033(3) 0.027(2) 0.031(3) 0.0067(19) -0.008(2) -0.0072(18) C18 0.023(2) 0.0226(18) 0.025(3) 0.0015(17) -0.007(2) 0.0041(17) C19 0.025(3) 0.0194(18) 0.031(3) -0.0018(17) -0.006(2) 0.0029(17) C20 0.037(3) 0.027(2) 0.039(3) -0.0110(19) -0.007(2) -0.0019(19) C21 0.044(3) 0.026(2) 0.030(3) -0.0057(18) 0.003(2) -0.0018(19) C22 0.029(3) 0.0187(18) 0.028(3) -0.0010(17) 0.001(2) -0.0010(17) C23 0.023(2) 0.0177(17) 0.022(2) -0.0027(16) -0.0070(19) 0.0041(16) C24 0.045(3) 0.035(2) 0.068(4) 0.015(2) -0.023(3) -0.013(2) C25 0.039(3) 0.038(2) 0.047(3) 0.000(2) -0.011(3) -0.015(2) C26 0.015(2) 0.036(2) 0.019(2) 0.0052(18) -0.0026(19) 0.0089(18) C27 0.039(3) 0.028(2) 0.022(3) 0.0030(18) 0.002(2) 0.0078(19) C28 0.048(3) 0.046(3) 0.025(3) 0.002(2) 0.006(2) 0.019(2) C29 0.038(3) 0.048(3) 0.029(3) 0.008(2) 0.010(2) 0.012(2) C30 0.030(3) 0.041(2) 0.028(3) 0.005(2) 0.004(2) 0.002(2) C31 0.027(3) 0.027(2) 0.020(2) 0.0020(17) 0.001(2) 0.0054(17) C32 0.023(3) 0.026(2) 0.032(3) 0.0010(18) -0.004(2) 0.0003(18) C33 0.026(3) 0.0190(18) 0.025(2) 0.0017(16) 0.002(2) -0.0021(17) C34 0.028(3) 0.029(2) 0.033(3) -0.0014(18) 0.008(2) -0.0011(18) C35 0.037(3) 0.025(2) 0.035(3) -0.0013(19) 0.006(2) -0.0122(19) C36 0.035(3) 0.0217(19) 0.035(3) -0.0067(18) 0.002(2) -0.0023(18) C37 0.025(3) 0.0244(19) 0.023(2) -0.0022(17) 0.005(2) -0.0027(17) C38 0.019(2) 0.0236(18) 0.024(2) 0.0017(17) 0.0033(19) 0.0015(17) C39 0.023(2) 0.0206(18) 0.017(2) -0.0046(15) -0.0004(19) -0.0010(16) C40 0.023(3) 0.0273(19) 0.020(2) -0.0005(17) 0.0039(19) 0.0059(17) C41 0.021(3) 0.036(2) 0.021(3) 0.0002(18) -0.002(2) 0.0025(18) C42 0.028(3) 0.032(2) 0.019(2) -0.0015(17) -0.003(2) -0.0014(18) C43 0.023(2) 0.0187(18) 0.022(2) -0.0042(16) -0.001(2) -0.0037(16) C44 0.027(3) 0.0205(18) 0.024(2) -0.0026(17) 0.003(2) -0.0049(17) C45 0.029(3) 0.027(2) 0.035(3) -0.0050(19) 0.009(2) -0.0016(18) C46 0.023(3) 0.029(2) 0.035(3) 0.0000(19) 0.005(2) 0.0050(18) C47 0.023(3) 0.0257(19) 0.026(3) -0.0013(17) -0.003(2) 0.0005(17) C48 0.023(2) 0.0149(16) 0.023(2) -0.0028(16) 0.0017(19) -0.0018(16) C49 0.045(3) 0.045(2) 0.030(3) -0.006(2) 0.012(2) -0.006(2) C50 0.041(3) 0.045(2) 0.028(3) 0.006(2) 0.000(2) 0.001(2) C51 0.033(3) 0.0237(19) 0.018(2) -0.0049(17) -0.004(2) 0.0054(18) C52 0.038(3) 0.025(2) 0.038(3) -0.0051(19) -0.006(2) 0.0054(19) C53 0.040(3) 0.029(2) 0.037(3) -0.007(2) -0.009(2) 0.015(2) C54 0.060(4) 0.028(2) 0.029(3) -0.0024(19) -0.010(3) 0.017(2) C55 0.047(3) 0.025(2) 0.023(3) -0.0013(18) 0.002(2) 0.005(2) C56 0.037(3) 0.0177(18) 0.020(2) -0.0035(16) -0.003(2) 0.0053(18) C57 0.039(3) 0.0201(18) 0.017(2) -0.0038(16) 0.004(2) -0.0015(18) C58 0.025(3) 0.0180(17) 0.024(2) -0.0028(16) 0.006(2) 0.0010(17) C59 0.034(3) 0.0218(19) 0.026(3) 0.0023(17) 0.008(2) -0.0006(18) C60 0.029(3) 0.029(2) 0.035(3) -0.0054(19) 0.016(2) -0.0063(19) C61 0.021(3) 0.0238(19) 0.039(3) -0.0072(19) 0.008(2) -0.0032(17) C62 0.024(3) 0.0180(18) 0.028(3) -0.0032(16) 0.005(2) -0.0011(17) C63 0.021(2) 0.0132(16) 0.029(3) -0.0049(16) 0.008(2) -0.0028(16) C64 0.016(2) 0.0193(17) 0.017(2) -0.0036(15) 0.0006(18) -0.0036(16) C65 0.020(2) 0.0189(17) 0.021(2) 0.0005(16) -0.0010(19) -0.0012(16) C66 0.021(2) 0.0260(19) 0.016(2) -0.0043(16) 0.0016(18) -0.0030(16) C67 0.025(3) 0.0216(18) 0.025(3) -0.0048(17) -0.002(2) 0.0027(17) C68 0.023(2) 0.0200(18) 0.023(2) 0.0003(16) 0.0003(19) -0.0028(16) C69 0.035(3) 0.0192(18) 0.029(3) -0.0047(17) -0.001(2) 0.0038(17) C70 0.046(3) 0.024(2) 0.026(3) 0.0061(18) 0.000(2) 0.0034(19) C71 0.037(3) 0.026(2) 0.025(3) -0.0022(17) 0.006(2) -0.0037(18) C72 0.026(3) 0.0200(18) 0.026(3) -0.0008(16) 0.002(2) -0.0036(17) C73 0.020(2) 0.0196(17) 0.019(2) -0.0031(16) 0.0007(18) -0.0070(16) C74 0.088(4) 0.026(2) 0.037(3) 0.004(2) 0.004(3) 0.020(2) C75 0.048(4) 0.034(2) 0.046(3) -0.011(2) -0.009(3) 0.022(2) C76 0.014(2) 0.0295(19) 0.019(2) -0.0061(17) -0.0025(19) -0.0064(16) C77 0.028(3) 0.0252(19) 0.018(2) 0.0030(17) -0.002(2) -0.0025(17) C78 0.029(3) 0.036(2) 0.021(3) 0.0042(18) 0.000(2) -0.0097(19) C79 0.029(3) 0.047(2) 0.025(3) 0.000(2) 0.013(2) -0.004(2) C80 0.023(3) 0.032(2) 0.028(3) -0.0058(18) 0.001(2) 0.0002(18) C81 0.016(2) 0.0307(19) 0.013(2) -0.0028(16) 0.0001(18) -0.0047(17) C82 0.017(2) 0.0209(18) 0.026(3) -0.0059(17) -0.001(2) -0.0017(16) C83 0.018(2) 0.0195(17) 0.019(2) -0.0025(16) -0.0012(19) -0.0016(16) C84 0.024(3) 0.0212(18) 0.031(3) -0.0044(17) 0.004(2) -0.0010(17) C85 0.029(3) 0.0214(19) 0.033(3) -0.0038(18) -0.002(2) 0.0061(17) C86 0.037(3) 0.0194(18) 0.030(3) 0.0038(17) -0.005(2) 0.0002(18) C87 0.025(3) 0.0232(18) 0.021(2) 0.0030(16) 0.0006(19) -0.0006(17) C88 0.024(3) 0.0245(18) 0.015(2) -0.0032(16) -0.0012(19) 0.0004(17) C89 0.019(2) 0.0208(17) 0.013(2) 0.0010(15) 0.0019(18) -0.0002(16) C90 0.017(2) 0.0282(19) 0.021(2) 0.0027(17) 0.0056(19) -0.0029(17) C91 0.023(3) 0.044(2) 0.022(3) -0.0006(19) 0.002(2) -0.0089(19) C92 0.027(3) 0.034(2) 0.012(2) 0.0006(17) -0.0018(19) -0.0051(18) C93 0.019(2) 0.0160(17) 0.019(2) 0.0027(15) 0.0004(19) 0.0020(15) C94 0.021(2) 0.0166(17) 0.020(2) 0.0044(16) 0.0033(19) 0.0064(16) C95 0.024(3) 0.0260(19) 0.025(3) 0.0028(17) 0.010(2) -0.0004(17) C96 0.018(2) 0.034(2) 0.026(3) -0.0054(18) 0.004(2) -0.0071(18) C97 0.023(3) 0.030(2) 0.018(2) -0.0039(17) -0.001(2) -0.0015(18) C98 0.023(2) 0.0162(17) 0.019(2) 0.0014(15) 0.0004(19) 0.0000(16) C99 0.042(3) 0.047(2) 0.028(3) -0.012(2) 0.000(2) -0.008(2) C100 0.040(3) 0.052(3) 0.024(3) 0.004(2) 0.007(2) -0.005(2) C101 0.057(4) 0.057(3) 0.032(3) 0.006(2) -0.004(3) -0.008(3) C102 0.042(4) 0.071(3) 0.038(3) -0.005(3) 0.009(3) 0.002(3) C103 0.076(3) 0.050(2) 0.065(3) -0.014(2) -0.007(2) -0.005(2) C104 0.062(3) 0.040(2) 0.051(3) -0.0095(19) -0.009(2) 0.0087(19) C105 0.049(3) 0.058(3) 0.038(3) -0.015(2) 0.003(2) 0.002(2) C106 0.040(3) 0.070(3) 0.041(3) -0.018(2) 0.008(2) -0.003(2) C107 0.079(3) 0.039(2) 0.046(3) -0.0076(17) -0.015(3) 0.014(2) C108 0.049(3) 0.0308(19) 0.038(3) -0.0089(17) 0.000(2) 0.0077(19) C109 0.072(3) 0.088(3) 0.079(3) 0.044(2) 0.002(3) -0.013(2) C110 0.073(3) 0.071(3) 0.072(3) 0.033(2) -0.002(2) -0.025(2) N1 0.022(2) 0.0154(14) 0.0209(19) -0.0029(13) 0.0056(15) -0.0034(13) N2 0.0181(19) 0.0184(14) 0.0202(19) -0.0048(13) 0.0004(15) -0.0008(13) N3 0.026(2) 0.0236(16) 0.042(2) 0.0002(15) -0.0145(18) -0.0067(15) N4 0.021(2) 0.0261(16) 0.023(2) 0.0042(14) 0.0014(17) 0.0011(14) N5 0.0195(19) 0.0211(15) 0.0177(19) -0.0044(13) 0.0054(15) -0.0014(13) N6 0.033(2) 0.0336(18) 0.021(2) -0.0030(15) 0.0035(17) -0.0045(16) N7 0.030(2) 0.0179(15) 0.0178(19) 0.0010(13) 0.0026(16) 0.0025(14) N8 0.0183(19) 0.0210(15) 0.0182(19) 0.0016(13) 0.0029(15) 0.0006(13) N9 0.043(3) 0.0231(16) 0.035(2) 0.0009(15) 0.003(2) 0.0107(16) N10 0.019(2) 0.0231(15) 0.0175(19) 0.0008(13) 0.0003(16) -0.0049(13) N11 0.0174(19) 0.0223(15) 0.0151(18) 0.0030(13) 0.0034(15) 0.0008(13) N12 0.026(2) 0.0353(17) 0.0141(19) 0.0001(14) 0.0067(16) -0.0010(15) N13 0.057(4) 0.110(4) 0.064(4) -0.011(3) -0.008(3) 0.025(3) N14 0.064(3) 0.055(2) 0.059(3) -0.0043(18) -0.009(2) 0.0068(18) N15 0.057(3) 0.097(3) 0.063(3) -0.025(2) 0.000(2) -0.016(2) N16 0.056(3) 0.0436(19) 0.044(3) 0.0008(15) 0.010(2) 0.0111(19) N17 0.087(3) 0.069(2) 0.084(3) 0.026(2) -0.001(2) -0.024(2) O1 0.0248(17) 0.0280(13) 0.0320(18) -0.0154(12) -0.0029(14) 0.0017(12) O2 0.0188(16) 0.0354(14) 0.0294(18) -0.0142(12) -0.0021(13) 0.0037(12) O3 0.0233(17) 0.0273(13) 0.0201(16) 0.0007(11) -0.0007(13) -0.0026(11) O4 0.0254(17) 0.0231(13) 0.0251(17) 0.0001(11) 0.0024(14) 0.0026(12) O5 0.0223(17) 0.0233(12) 0.0278(17) 0.0002(11) 0.0008(13) 0.0037(11) O6 0.0204(16) 0.0210(12) 0.0177(15) -0.0029(11) -0.0007(12) -0.0034(11) O7 0.0229(17) 0.0256(13) 0.0316(18) 0.0080(12) -0.0046(14) 0.0033(12) O8 0.0203(16) 0.0248(13) 0.0188(16) -0.0051(11) -0.0038(12) -0.0008(11) O9 0.0187(16) 0.0277(13) 0.0186(16) 0.0025(11) 0.0002(12) -0.0031(11) O10 0.0222(16) 0.0222(12) 0.0157(15) 0.0001(11) 0.0044(13) -0.0005(11) O11 0.0229(17) 0.0239(12) 0.0204(16) -0.0031(11) 0.0020(13) -0.0022(11) O12 0.0185(16) 0.0249(12) 0.0161(15) -0.0002(11) 0.0013(12) 0.0026(11) O13 0.0232(18) 0.0231(13) 0.0211(18) -0.0039(13) -0.0035(14) -0.0005(11) O14 0.0159(16) 0.0229(13) 0.0171(17) -0.0003(12) -0.0007(13) -0.0004(11) S1 0.0195(6) 0.0219(4) 0.0193(6) -0.0033(4) -0.0021(5) 0.0002(4) S2 0.0203(6) 0.0217(4) 0.0197(6) -0.0016(4) -0.0001(5) 0.0001(4) S3 0.0187(6) 0.0199(4) 0.0182(6) -0.0003(4) -0.0001(4) -0.0009(4) S4 0.0199(6) 0.0214(4) 0.0163(6) -0.0012(4) 0.0003(4) -0.0017(4) Zn1 0.0191(3) 0.0189(2) 0.0222(3) -0.00452(18) -0.0026(2) 0.00076(18) Zn2 0.0214(3) 0.0210(2) 0.0203(3) -0.00293(18) 0.0005(2) 0.00083(18) Zn3 0.0179(3) 0.0198(2) 0.0167(3) 0.00026(18) 0.0013(2) -0.00028(18) Zn4 0.0211(3) 0.0193(2) 0.0196(3) 0.00193(18) -0.0005(2) -0.00025(18) Zn5 0.0181(3) 0.0262(2) 0.0291(3) -0.0018(2) -0.0014(2) 0.00076(19) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 O1 1.347(4) . ? C1 C2 1.396(5) . ? C1 C6 1.404(5) . ? C2 C3 1.399(5) . ? C2 H2 0.95 . ? C3 C4 1.380(6) . ? C3 H3 0.95 . ? C4 C5 1.362(5) . ? C4 H4 0.95 . ? C5 C6 1.409(5) . ? C5 H5 0.95 . ? C6 C7 1.438(5) . ? C7 N1 1.285(4) . ? C7 H7 0.95 . ? C8 C9 1.395(5) . ? C8 C13 1.405(5) . ? C8 N1 1.423(5) . ? C9 C10 1.378(5) . ? C9 H9 0.95 . ? C10 C11 1.381(5) . ? C10 H10 0.95 . ? C11 C12 1.384(5) . ? C11 H11 0.95 . ? C12 C13 1.401(5) . ? C12 H12 0.95 . ? C13 N2 1.420(4) . ? C14 C15 1.360(5) . ? C14 C23 1.445(5) . ? C14 S1 1.789(4) . ? C15 C16 1.409(5) . ? C15 H15 0.95 . ? C16 C17 1.367(5) . ? C16 H16 0.95 . ? C17 C18 1.415(6) . ? C17 H17 0.95 . ? C18 C23 1.421(5) . ? C18 C19 1.437(5) . ? C19 C20 1.366(6) . ? C19 N3 1.421(5) . ? C20 C21 1.415(5) . ? C20 H20 0.95 . ? C21 C22 1.369(5) . ? C21 H21 0.95 . ? C22 C23 1.408(5) . ? C22 H22 0.95 . ? C24 N3 1.473(5) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 N3 1.452(5) . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 O4 1.329(4) . ? C26 C27 1.409(5) . ? C26 C31 1.417(5) . ? C27 C28 1.369(6) . ? C27 H27 0.95 . ? C28 C29 1.399(6) . ? C28 H28 0.95 . ? C29 C30 1.363(5) . ? C29 H29 0.95 . ? C30 C31 1.399(5) . ? C30 H30 0.95 . ? C31 C32 1.434(5) . ? C32 N4 1.308(5) . ? C32 H32 0.95 . ? C33 C34 1.389(5) . ? C33 C38 1.405(5) . ? C33 N4 1.425(4) . ? C34 C35 1.378(5) . ? C34 H34 0.95 . ? C35 C36 1.369(6) . ? C35 H35 0.95 . ? C36 C37 1.384(5) . ? C36 H36 0.95 . ? C37 C38 1.390(5) . ? C37 H37 0.95 . ? C38 N5 1.417(4) . ? C39 C40 1.374(5) . ? C39 C48 1.443(5) . ? C39 S2 1.771(4) . ? C40 C41 1.397(5) . ? C40 H40 0.95 . ? C41 C42 1.364(5) . ? C41 H41 0.95 . ? C42 C43 1.412(5) . ? C42 H42 0.95 . ? C43 C48 1.422(5) . ? C43 C44 1.436(5) . ? C44 C45 1.372(5) . ? C44 N6 1.425(5) . ? C45 C46 1.390(5) . ? C45 H45 0.95 . ? C46 C47 1.371(5) . ? C46 H46 0.95 . ? C47 C48 1.427(5) . ? C47 H47 0.95 . ? C49 N6 1.455(5) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 N6 1.459(4) . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 O7 1.354(4) . ? C51 C52 1.395(5) . ? C51 C56 1.409(5) . ? C52 C53 1.393(5) . ? C52 H52 0.95 . ? C53 C54 1.390(6) . ? C53 H53 0.95 . ? C54 C55 1.362(6) . ? C54 H54 0.95 . ? C55 C56 1.414(5) . ? C55 H55 0.95 . ? C56 C57 1.443(5) . ? C57 N7 1.287(4) . ? C57 H57 0.95 . ? C58 C59 1.400(5) . ? C58 C63 1.403(5) . ? C58 N7 1.423(5) . ? C59 C60 1.380(5) . ? C59 H59 0.95 . ? C60 C61 1.378(5) . ? C60 H60 0.95 . ? C61 C62 1.382(5) . ? C61 H61 0.95 . ? C62 C63 1.390(5) . ? C62 H62 0.95 . ? C63 N8 1.422(4) . ? C64 C65 1.360(5) . ? C64 C73 1.432(5) . ? C64 S3 1.792(3) . ? C65 C66 1.415(5) . ? C65 H65 0.95 . ? C66 C67 1.356(5) . ? C66 H66 0.95 . ? C67 C68 1.418(5) . ? C67 H67 0.95 . ? C68 C73 1.422(5) . ? C68 C69 1.443(5) . ? C69 C70 1.364(5) . ? C69 N9 1.415(5) . ? C70 C71 1.403(5) . ? C70 H70 0.95 . ? C71 C72 1.373(5) . ? C71 H71 0.95 . ? C72 C73 1.411(5) . ? C72 H72 0.95 . ? C74 N9 1.475(5) . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? C75 N9 1.460(5) . ? C75 H75A 0.98 . ? C75 H75B 0.98 . ? C75 H75C 0.98 . ? C76 O10 1.331(4) . ? C76 C77 1.388(5) . ? C76 C81 1.426(5) . ? C77 C78 1.372(5) . ? C77 H77 0.95 . ? C78 C79 1.391(5) . ? C78 H78 0.95 . ? C79 C80 1.377(5) . ? C79 H79 0.95 . ? C80 C81 1.403(5) . ? C80 H80 0.95 . ? C81 C82 1.450(5) . ? C82 N10 1.302(5) . ? C82 H82 0.95 . ? C83 C84 1.386(5) . ? C83 C88 1.410(5) . ? C83 N10 1.420(4) . ? C84 C85 1.376(5) . ? C84 H84 0.95 . ? C85 C86 1.383(6) . ? C85 H85 0.95 . ? C86 C87 1.387(5) . ? C86 H86 0.95 . ? C87 C88 1.400(5) . ? C87 H87 0.95 . ? C88 N11 1.415(4) . ? C89 C90 1.370(5) . ? C89 C98 1.437(5) . ? C89 S4 1.779(4) . ? C90 C91 1.392(5) . ? C90 H90 0.95 . ? C91 C92 1.364(5) . ? C91 H91 0.95 . ? C92 C93 1.406(5) . ? C92 H92 0.95 . ? C93 C98 1.435(5) . ? C93 C94 1.440(5) . ? C94 C95 1.368(5) . ? C94 N12 1.419(5) . ? C95 C96 1.400(5) . ? C95 H95 0.95 . ? C96 C97 1.360(5) . ? C96 H96 0.95 . ? C97 C98 1.414(5) . ? C97 H97 0.95 . ? C99 N12 1.475(4) . ? C99 H99A 0.98 . ? C99 H99B 0.98 . ? C99 H99C 0.98 . ? C100 N12 1.457(5) . ? C100 H10A 0.98 . ? C100 H10B 0.98 . ? C100 H10C 0.98 . ? C101 C102 1.447(6) . ? C101 H10D 0.98 . ? C101 H10E 0.98 . ? C101 H10F 0.98 . ? C102 N13 1.131(6) . ? C103 C104 1.430(7) . ? C103 H10G 0.98 . ? C103 H10H 0.98 . ? C103 H10I 0.98 . ? C104 N14 1.153(6) . ? C105 C106 1.413(6) . ? C105 H10J 0.98 . ? C105 H10K 0.98 . ? C105 H10L 0.98 . ? C106 N15 1.140(5) . ? C107 C108 1.444(6) . ? C107 H10M 0.98 . ? C107 H10N 0.98 . ? C107 H10O 0.98 . ? C108 N16 1.131(5) . ? C109 C110 1.434(8) . ? C109 H10P 0.98 . ? C109 H10Q 0.98 . ? C109 H10R 0.98 . ? C110 N17 1.162(7) . ? N1 Zn1 2.050(3) . ? N2 S1 1.592(3) . ? N2 Zn1 2.041(3) . ? N4 Zn2 2.029(3) . ? N5 S2 1.582(3) . ? N5 Zn2 2.065(3) . ? N7 Zn4 2.037(3) . ? N8 S3 1.591(3) . ? N8 Zn4 2.031(3) . ? N10 Zn3 2.036(3) . ? N11 S4 1.576(3) . ? N11 Zn3 2.042(3) . ? O1 Zn5 1.951(3) . ? O1 Zn1 2.061(3) . ? O2 S1 1.450(3) . ? O3 S1 1.439(3) . ? O4 Zn1 1.976(2) . ? O4 Zn2 2.095(3) . ? O5 S2 1.442(2) . ? O6 S2 1.469(2) . ? O6 Zn3 2.056(2) . ? O7 Zn5 1.959(3) . ? O7 Zn4 2.037(3) . ? O8 S3 1.442(2) . ? O9 S3 1.449(3) . ? O10 Zn4 1.986(2) . ? O10 Zn3 2.039(2) . ? O11 S4 1.433(2) . ? O12 S4 1.476(2) . ? O12 Zn2 2.034(2) . ? O13 Zn5 1.941(3) . ? O13 Zn2 2.015(3) . ? O13 Zn1 2.118(3) . ? O13 H13O 0.77(4) . ? O14 Zn5 1.930(3) . ? O14 Zn3 2.035(2) . ? O14 Zn4 2.109(3) . ? O14 H14O 0.784(19) . ? Zn1 Zn5 3.0736(6) . ? Zn1 Zn2 3.1185(5) . ? Zn3 Zn4 3.1421(5) . ? Zn4 Zn5 3.0377(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 119.3(4) . . ? O1 C1 C6 121.1(3) . . ? C2 C1 C6 119.6(3) . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 120.3(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.2(4) . . ? C5 C4 H4 120.4 . . ? C3 C4 H4 120.4 . . ? C4 C5 C6 122.7(4) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 117.9(4) . . ? C1 C6 C7 124.7(3) . . ? C5 C6 C7 117.4(4) . . ? N1 C7 C6 128.2(4) . . ? N1 C7 H7 115.9 . . ? C6 C7 H7 115.9 . . ? C9 C8 C13 120.0(4) . . ? C9 C8 N1 123.5(3) . . ? C13 C8 N1 116.4(3) . . ? C10 C9 C8 120.3(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.0(4) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C11 C12 C13 120.3(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C8 118.7(3) . . ? C12 C13 N2 125.3(3) . . ? C8 C13 N2 116.0(3) . . ? C15 C14 C23 120.9(3) . . ? C15 C14 S1 120.0(3) . . ? C23 C14 S1 119.2(3) . . ? C14 C15 C16 120.9(4) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C17 C16 C15 119.9(4) . . ? C17 C16 H16 120 . . ? C15 C16 H16 120 . . ? C16 C17 C18 121.0(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C23 119.8(3) . . ? C17 C18 C19 120.4(4) . . ? C23 C18 C19 119.8(4) . . ? C20 C19 N3 122.9(3) . . ? C20 C19 C18 118.7(4) . . ? N3 C19 C18 118.3(4) . . ? C19 C20 C21 121.3(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C22 C21 C20 120.6(4) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 119.2(3) . . ? C22 C23 C14 123.3(3) . . ? C18 C23 C14 117.5(4) . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O4 C26 C27 120.8(3) . . ? O4 C26 C31 121.5(3) . . ? C27 C26 C31 117.7(4) . . ? C28 C27 C26 121.4(4) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.3 . . ? C27 C28 C29 121.0(4) . . ? C27 C28 H28 119.5 . . ? C29 C28 H28 119.5 . . ? C30 C29 C28 118.2(4) . . ? C30 C29 H29 120.9 . . ? C28 C29 H29 120.9 . . ? C29 C30 C31 122.8(4) . . ? C29 C30 H30 118.6 . . ? C31 C30 H30 118.6 . . ? C30 C31 C26 118.9(4) . . ? C30 C31 C32 117.0(4) . . ? C26 C31 C32 124.0(4) . . ? N4 C32 C31 126.9(4) . . ? N4 C32 H32 116.6 . . ? C31 C32 H32 116.6 . . ? C34 C33 C38 119.7(4) . . ? C34 C33 N4 123.9(4) . . ? C38 C33 N4 116.2(3) . . ? C35 C34 C33 120.5(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C36 C35 C34 119.9(4) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C35 C36 C37 120.4(4) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 120.8(4) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C33 118.3(3) . . ? C37 C38 N5 126.3(4) . . ? C33 C38 N5 115.4(3) . . ? C40 C39 C48 120.4(4) . . ? C40 C39 S2 117.0(3) . . ? C48 C39 S2 122.6(3) . . ? C39 C40 C41 120.8(4) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 120.5(4) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.9(4) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C42 C43 C48 119.7(4) . . ? C42 C43 C44 120.4(4) . . ? C48 C43 C44 119.8(4) . . ? C45 C44 N6 123.7(4) . . ? C45 C44 C43 118.7(4) . . ? N6 C44 C43 117.5(4) . . ? C44 C45 C46 120.8(4) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? C47 C46 C45 122.2(4) . . ? C47 C46 H46 118.9 . . ? C45 C46 H46 118.9 . . ? C46 C47 C48 119.1(4) . . ? C46 C47 H47 120.5 . . ? C48 C47 H47 120.5 . . ? C43 C48 C47 118.8(4) . . ? C43 C48 C39 117.5(4) . . ? C47 C48 C39 123.7(4) . . ? N6 C49 H49A 109.5 . . ? N6 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N6 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N6 C50 H50A 109.5 . . ? N6 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N6 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O7 C51 C52 119.4(4) . . ? O7 C51 C56 121.2(4) . . ? C52 C51 C56 119.4(4) . . ? C53 C52 C51 121.4(4) . . ? C53 C52 H52 119.3 . . ? C51 C52 H52 119.3 . . ? C54 C53 C52 119.8(4) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C55 C54 C53 118.9(4) . . ? C55 C54 H54 120.6 . . ? C53 C54 H54 120.6 . . ? C54 C55 C56 123.4(4) . . ? C54 C55 H55 118.3 . . ? C56 C55 H55 118.3 . . ? C51 C56 C55 117.2(4) . . ? C51 C56 C57 125.8(3) . . ? C55 C56 C57 116.9(4) . . ? N7 C57 C56 126.4(4) . . ? N7 C57 H57 116.8 . . ? C56 C57 H57 116.8 . . ? C59 C58 C63 120.2(4) . . ? C59 C58 N7 123.6(4) . . ? C63 C58 N7 116.2(3) . . ? C60 C59 C58 120.2(4) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C61 C60 C59 119.8(4) . . ? C61 C60 H60 120.1 . . ? C59 C60 H60 120.1 . . ? C60 C61 C62 120.5(4) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C61 C62 C63 121.1(4) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C62 C63 C58 118.3(4) . . ? C62 C63 N8 126.3(3) . . ? C58 C63 N8 115.4(3) . . ? C65 C64 C73 121.7(3) . . ? C65 C64 S3 118.5(3) . . ? C73 C64 S3 119.8(3) . . ? C64 C65 C66 120.3(3) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C67 C66 C65 119.8(4) . . ? C67 C66 H66 120.1 . . ? C65 C66 H66 120.1 . . ? C66 C67 C68 121.5(3) . . ? C66 C67 H67 119.3 . . ? C68 C67 H67 119.3 . . ? C67 C68 C73 119.4(3) . . ? C67 C68 C69 121.0(3) . . ? C73 C68 C69 119.6(4) . . ? C70 C69 N9 123.9(3) . . ? C70 C69 C68 119.0(3) . . ? N9 C69 C68 117.0(4) . . ? C69 C70 C71 121.5(4) . . ? C69 C70 H70 119.2 . . ? C71 C70 H70 119.2 . . ? C72 C71 C70 120.4(4) . . ? C72 C71 H71 119.8 . . ? C70 C71 H71 119.8 . . ? C71 C72 C73 120.8(4) . . ? C71 C72 H72 119.6 . . ? C73 C72 H72 119.6 . . ? C72 C73 C68 118.7(3) . . ? C72 C73 C64 124.1(3) . . ? C68 C73 C64 117.2(3) . . ? N9 C74 H74A 109.5 . . ? N9 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? N9 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? N9 C75 H75A 109.5 . . ? N9 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? N9 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? O10 C76 C77 120.3(3) . . ? O10 C76 C81 121.3(3) . . ? C77 C76 C81 118.4(4) . . ? C78 C77 C76 121.8(4) . . ? C78 C77 H77 119.1 . . ? C76 C77 H77 119.1 . . ? C77 C78 C79 120.5(4) . . ? C77 C78 H78 119.7 . . ? C79 C78 H78 119.7 . . ? C80 C79 C78 118.9(4) . . ? C80 C79 H79 120.5 . . ? C78 C79 H79 120.5 . . ? C79 C80 C81 121.8(4) . . ? C79 C80 H80 119.1 . . ? C81 C80 H80 119.1 . . ? C80 C81 C76 118.5(3) . . ? C80 C81 C82 116.9(3) . . ? C76 C81 C82 124.6(4) . . ? N10 C82 C81 126.1(3) . . ? N10 C82 H82 116.9 . . ? C81 C82 H82 116.9 . . ? C84 C83 C88 120.1(3) . . ? C84 C83 N10 124.4(4) . . ? C88 C83 N10 115.4(3) . . ? C85 C84 C83 121.2(4) . . ? C85 C84 H84 119.4 . . ? C83 C84 H84 119.4 . . ? C84 C85 C86 119.1(4) . . ? C84 C85 H85 120.4 . . ? C86 C85 H85 120.4 . . ? C85 C86 C87 121.0(4) . . ? C85 C86 H86 119.5 . . ? C87 C86 H86 119.5 . . ? C86 C87 C88 120.3(4) . . ? C86 C87 H87 119.8 . . ? C88 C87 H87 119.8 . . ? C87 C88 C83 118.2(3) . . ? C87 C88 N11 125.4(4) . . ? C83 C88 N11 116.4(3) . . ? C90 C89 C98 121.5(3) . . ? C90 C89 S4 117.2(3) . . ? C98 C89 S4 121.3(3) . . ? C89 C90 C91 120.4(4) . . ? C89 C90 H90 119.8 . . ? C91 C90 H90 119.8 . . ? C92 C91 C90 120.3(4) . . ? C92 C91 H91 119.8 . . ? C90 C91 H91 119.8 . . ? C91 C92 C93 121.5(4) . . ? C91 C92 H92 119.2 . . ? C93 C92 H92 119.2 . . ? C92 C93 C98 119.4(4) . . ? C92 C93 C94 121.5(3) . . ? C98 C93 C94 119.0(3) . . ? C95 C94 N12 123.5(4) . . ? C95 C94 C93 119.0(4) . . ? N12 C94 C93 117.5(3) . . ? C94 C95 C96 120.8(4) . . ? C94 C95 H95 119.6 . . ? C96 C95 H95 119.6 . . ? C97 C96 C95 122.2(4) . . ? C97 C96 H96 118.9 . . ? C95 C96 H96 118.9 . . ? C96 C97 C98 119.5(4) . . ? C96 C97 H97 120.2 . . ? C98 C97 H97 120.2 . . ? C97 C98 C93 119.2(4) . . ? C97 C98 C89 124.0(3) . . ? C93 C98 C89 116.8(3) . . ? N12 C99 H99A 109.5 . . ? N12 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? N12 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? N12 C100 H10A 109.5 . . ? N12 C100 H10B 109.5 . . ? H10A C100 H10B 109.5 . . ? N12 C100 H10C 109.5 . . ? H10A C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C102 C101 H10D 109.5 . . ? C102 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C102 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? N13 C102 C101 177.7(6) . . ? C104 C103 H10G 109.5 . . ? C104 C103 H10H 109.5 . . ? H10G C103 H10H 109.5 . . ? C104 C103 H10I 109.5 . . ? H10G C103 H10I 109.5 . . ? H10H C103 H10I 109.5 . . ? N14 C104 C103 178.9(6) . . ? C106 C105 H10J 109.5 . . ? C106 C105 H10K 109.5 . . ? H10J C105 H10K 109.5 . . ? C106 C105 H10L 109.5 . . ? H10J C105 H10L 109.5 . . ? H10K C105 H10L 109.5 . . ? N15 C106 C105 178.3(6) . . ? C108 C107 H10M 109.5 . . ? C108 C107 H10N 109.5 . . ? H10M C107 H10N 109.5 . . ? C108 C107 H10O 109.5 . . ? H10M C107 H10O 109.5 . . ? H10N C107 H10O 109.5 . . ? N16 C108 C107 178.9(5) . . ? C110 C109 H10P 109.5 . . ? C110 C109 H10Q 109.5 . . ? H10P C109 H10Q 109.5 . . ? C110 C109 H10R 109.5 . . ? H10P C109 H10R 109.5 . . ? H10Q C109 H10R 109.5 . . ? N17 C110 C109 176.1(6) . . ? C7 N1 C8 122.4(3) . . ? C7 N1 Zn1 126.0(3) . . ? C8 N1 Zn1 111.5(2) . . ? C13 N2 S1 121.8(2) . . ? C13 N2 Zn1 112.3(2) . . ? S1 N2 Zn1 125.55(17) . . ? C19 N3 C25 115.8(3) . . ? C19 N3 C24 112.7(3) . . ? C25 N3 C24 110.6(3) . . ? C32 N4 C33 118.9(3) . . ? C32 N4 Zn2 126.5(3) . . ? C33 N4 Zn2 113.7(3) . . ? C38 N5 S2 120.0(2) . . ? C38 N5 Zn2 113.5(2) . . ? S2 N5 Zn2 126.34(16) . . ? C44 N6 C49 115.9(3) . . ? C44 N6 C50 113.7(3) . . ? C49 N6 C50 110.1(3) . . ? C57 N7 C58 122.9(3) . . ? C57 N7 Zn4 126.7(3) . . ? C58 N7 Zn4 110.4(2) . . ? C63 N8 S3 122.0(3) . . ? C63 N8 Zn4 110.7(2) . . ? S3 N8 Zn4 124.86(16) . . ? C69 N9 C75 114.1(3) . . ? C69 N9 C74 115.2(3) . . ? C75 N9 C74 111.0(3) . . ? C82 N10 C83 121.6(3) . . ? C82 N10 Zn3 123.9(2) . . ? C83 N10 Zn3 113.7(2) . . ? C88 N11 S4 121.5(2) . . ? C88 N11 Zn3 113.3(2) . . ? S4 N11 Zn3 124.25(16) . . ? C94 N12 C100 115.0(3) . . ? C94 N12 C99 114.2(3) . . ? C100 N12 C99 109.3(3) . . ? C1 O1 Zn5 130.5(2) . . ? C1 O1 Zn1 129.1(2) . . ? Zn5 O1 Zn1 99.98(10) . . ? C26 O4 Zn1 127.8(2) . . ? C26 O4 Zn2 128.6(2) . . ? Zn1 O4 Zn2 99.94(12) . . ? S2 O6 Zn3 126.42(14) . . ? C51 O7 Zn5 132.2(3) . . ? C51 O7 Zn4 128.9(3) . . ? Zn5 O7 Zn4 98.93(10) . . ? C76 O10 Zn4 132.1(2) . . ? C76 O10 Zn3 125.2(2) . . ? Zn4 O10 Zn3 102.64(11) . . ? S4 O12 Zn2 127.96(14) . . ? Zn5 O13 Zn2 118.29(14) . . ? Zn5 O13 Zn1 98.35(11) . . ? Zn2 O13 Zn1 97.94(13) . . ? Zn5 O13 H13O 122(3) . . ? Zn2 O13 H13O 105(3) . . ? Zn1 O13 H13O 112(3) . . ? Zn5 O14 Zn3 117.23(13) . . ? Zn5 O14 Zn4 97.44(11) . . ? Zn3 O14 Zn4 98.59(12) . . ? Zn5 O14 H14O 123(3) . . ? Zn3 O14 H14O 107(3) . . ? Zn4 O14 H14O 111(3) . . ? O3 S1 O2 115.54(17) . . ? O3 S1 N2 112.86(15) . . ? O2 S1 N2 107.25(16) . . ? O3 S1 C14 106.96(16) . . ? O2 S1 C14 105.95(16) . . ? N2 S1 C14 107.82(17) . . ? O5 S2 O6 114.90(15) . . ? O5 S2 N5 113.62(15) . . ? O6 S2 N5 105.53(15) . . ? O5 S2 C39 108.31(16) . . ? O6 S2 C39 106.22(15) . . ? N5 S2 C39 107.82(18) . . ? O8 S3 O9 114.90(15) . . ? O8 S3 N8 113.62(15) . . ? O9 S3 N8 107.18(15) . . ? O8 S3 C64 106.87(16) . . ? O9 S3 C64 106.81(15) . . ? N8 S3 C64 106.99(16) . . ? O11 S4 O12 114.38(15) . . ? O11 S4 N11 113.59(15) . . ? O12 S4 N11 106.35(15) . . ? O11 S4 C89 108.48(15) . . ? O12 S4 C89 104.63(15) . . ? N11 S4 C89 108.94(17) . . ? O4 Zn1 N2 106.88(11) . . ? O4 Zn1 N1 122.10(11) . . ? N2 Zn1 N1 81.12(12) . . ? O4 Zn1 O1 101.56(10) . . ? N2 Zn1 O1 151.17(11) . . ? N1 Zn1 O1 87.87(11) . . ? O4 Zn1 O13 80.41(11) . . ? N2 Zn1 O13 102.88(12) . . ? N1 Zn1 O13 155.41(11) . . ? O1 Zn1 O13 77.05(10) . . ? O4 Zn1 Zn5 94.86(8) . . ? N2 Zn1 Zn5 131.98(9) . . ? N1 Zn1 Zn5 122.29(9) . . ? O1 Zn1 Zn5 38.70(7) . . ? O13 Zn1 Zn5 38.67(7) . . ? O4 Zn1 Zn2 41.43(8) . . ? N2 Zn1 Zn2 103.31(7) . . ? N1 Zn1 Zn2 163.52(8) . . ? O1 Zn1 Zn2 94.78(7) . . ? O13 Zn1 Zn2 39.79(7) . . ? Zn5 Zn1 Zn2 66.523(14) . . ? O13 Zn2 N4 140.79(12) . . ? O13 Zn2 O12 95.73(10) . . ? N4 Zn2 O12 121.20(11) . . ? O13 Zn2 N5 106.77(12) . . ? N4 Zn2 N5 80.51(12) . . ? O12 Zn2 N5 100.95(11) . . ? O13 Zn2 O4 80.09(10) . . ? N4 Zn2 O4 85.72(11) . . ? O12 Zn2 O4 91.65(10) . . ? N5 Zn2 O4 164.80(11) . . ? O13 Zn2 Zn1 42.27(8) . . ? N4 Zn2 Zn1 111.61(9) . . ? O12 Zn2 Zn1 100.95(6) . . ? N5 Zn2 Zn1 143.63(8) . . ? O4 Zn2 Zn1 38.62(7) . . ? O14 Zn3 N10 146.25(11) . . ? O14 Zn3 O10 79.29(10) . . ? N10 Zn3 O10 87.90(11) . . ? O14 Zn3 N11 102.43(11) . . ? N10 Zn3 N11 81.02(12) . . ? O10 Zn3 N11 162.21(11) . . ? O14 Zn3 O6 100.75(10) . . ? N10 Zn3 O6 110.84(11) . . ? O10 Zn3 O6 91.80(10) . . ? N11 Zn3 O6 105.11(11) . . ? O14 Zn3 Zn4 41.59(8) . . ? N10 Zn3 Zn4 117.07(8) . . ? O10 Zn3 Zn4 38.07(7) . . ? N11 Zn3 Zn4 138.68(8) . . ? O6 Zn3 Zn4 102.10(6) . . ? O10 Zn4 N8 108.80(11) . . ? O10 Zn4 N7 115.48(11) . . ? N8 Zn4 N7 81.00(12) . . ? O10 Zn4 O7 105.49(10) . . ? N8 Zn4 O7 145.31(11) . . ? N7 Zn4 O7 89.02(11) . . ? O10 Zn4 O14 78.73(10) . . ? N8 Zn4 O14 103.12(11) . . ? N7 Zn4 O14 163.44(11) . . ? O7 Zn4 O14 78.49(10) . . ? O10 Zn4 Zn5 94.88(7) . . ? N8 Zn4 Zn5 130.54(9) . . ? N7 Zn4 Zn5 127.05(9) . . ? O7 Zn4 Zn5 39.58(7) . . ? O14 Zn4 Zn5 39.04(7) . . ? O10 Zn4 Zn3 39.29(7) . . ? N8 Zn4 Zn3 106.65(7) . . ? N7 Zn4 Zn3 154.70(8) . . ? O7 Zn4 Zn3 96.50(7) . . ? O14 Zn4 Zn3 39.82(7) . . ? Zn5 Zn4 Zn3 66.397(14) . . ? O14 Zn5 O13 126.68(10) . . ? O14 Zn5 O1 125.65(11) . . ? O13 Zn5 O1 83.95(11) . . ? O14 Zn5 O7 84.86(11) . . ? O13 Zn5 O7 122.26(12) . . ? O1 Zn5 O7 118.10(10) . . ? O14 Zn5 Zn4 43.52(8) . . ? O13 Zn5 Zn4 142.72(9) . . ? O1 Zn5 Zn4 132.65(7) . . ? O7 Zn5 Zn4 41.49(7) . . ? O14 Zn5 Zn1 146.80(8) . . ? O13 Zn5 Zn1 42.98(8) . . ? O1 Zn5 Zn1 41.33(7) . . ? O7 Zn5 Zn1 128.18(7) . . ? Zn4 Zn5 Zn1 168.238(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -178.0(3) . . . . ? C6 C1 C2 C3 1.3(6) . . . . ? C1 C2 C3 C4 0.1(6) . . . . ? C2 C3 C4 C5 -0.9(6) . . . . ? C3 C4 C5 C6 0.4(6) . . . . ? O1 C1 C6 C5 177.5(3) . . . . ? C2 C1 C6 C5 -1.7(5) . . . . ? O1 C1 C6 C7 0.2(6) . . . . ? C2 C1 C6 C7 -179.1(4) . . . . ? C4 C5 C6 C1 1.0(6) . . . . ? C4 C5 C6 C7 178.5(4) . . . . ? C1 C6 C7 N1 -11.3(6) . . . . ? C5 C6 C7 N1 171.3(4) . . . . ? C13 C8 C9 C10 0.1(5) . . . . ? N1 C8 C9 C10 179.7(3) . . . . ? C8 C9 C10 C11 -0.9(6) . . . . ? C9 C10 C11 C12 1.0(6) . . . . ? C10 C11 C12 C13 -0.4(6) . . . . ? C11 C12 C13 C8 -0.4(5) . . . . ? C11 C12 C13 N2 -177.5(3) . . . . ? C9 C8 C13 C12 0.5(5) . . . . ? N1 C8 C13 C12 -179.1(3) . . . . ? C9 C8 C13 N2 177.9(3) . . . . ? N1 C8 C13 N2 -1.7(5) . . . . ? C23 C14 C15 C16 1.8(6) . . . . ? S1 C14 C15 C16 -176.0(3) . . . . ? C14 C15 C16 C17 -1.5(6) . . . . ? C15 C16 C17 C18 -0.2(6) . . . . ? C16 C17 C18 C23 1.5(6) . . . . ? C16 C17 C18 C19 178.5(4) . . . . ? C17 C18 C19 C20 -174.4(4) . . . . ? C23 C18 C19 C20 2.6(6) . . . . ? C17 C18 C19 N3 3.5(5) . . . . ? C23 C18 C19 N3 -179.5(3) . . . . ? N3 C19 C20 C21 178.8(4) . . . . ? C18 C19 C20 C21 -3.4(6) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C23 3.2(6) . . . . ? C21 C22 C23 C18 -3.9(6) . . . . ? C21 C22 C23 C14 175.3(4) . . . . ? C17 C18 C23 C22 178.0(3) . . . . ? C19 C18 C23 C22 0.9(5) . . . . ? C17 C18 C23 C14 -1.2(5) . . . . ? C19 C18 C23 C14 -178.2(3) . . . . ? C15 C14 C23 C22 -179.6(4) . . . . ? S1 C14 C23 C22 -1.7(5) . . . . ? C15 C14 C23 C18 -0.4(5) . . . . ? S1 C14 C23 C18 177.4(3) . . . . ? O4 C26 C27 C28 178.8(4) . . . . ? C31 C26 C27 C28 -1.7(6) . . . . ? C26 C27 C28 C29 1.4(6) . . . . ? C27 C28 C29 C30 -0.7(6) . . . . ? C28 C29 C30 C31 0.4(6) . . . . ? C29 C30 C31 C26 -0.7(6) . . . . ? C29 C30 C31 C32 175.6(4) . . . . ? O4 C26 C31 C30 -179.1(3) . . . . ? C27 C26 C31 C30 1.4(5) . . . . ? O4 C26 C31 C32 4.8(6) . . . . ? C27 C26 C31 C32 -174.7(4) . . . . ? C30 C31 C32 N4 178.3(4) . . . . ? C26 C31 C32 N4 -5.5(6) . . . . ? C38 C33 C34 C35 -6.1(6) . . . . ? N4 C33 C34 C35 178.8(3) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? C34 C35 C36 C37 3.3(6) . . . . ? C35 C36 C37 C38 -1.3(6) . . . . ? C36 C37 C38 C33 -4.3(6) . . . . ? C36 C37 C38 N5 173.0(4) . . . . ? C34 C33 C38 C37 7.9(5) . . . . ? N4 C33 C38 C37 -176.6(3) . . . . ? C34 C33 C38 N5 -169.7(3) . . . . ? N4 C33 C38 N5 5.8(5) . . . . ? C48 C39 C40 C41 -2.6(5) . . . . ? S2 C39 C40 C41 176.4(3) . . . . ? C39 C40 C41 C42 2.9(5) . . . . ? C40 C41 C42 C43 1.5(5) . . . . ? C41 C42 C43 C48 -6.1(5) . . . . ? C41 C42 C43 C44 177.6(3) . . . . ? C42 C43 C44 C45 168.0(3) . . . . ? C48 C43 C44 C45 -8.4(5) . . . . ? C42 C43 C44 N6 -8.5(5) . . . . ? C48 C43 C44 N6 175.1(3) . . . . ? N6 C44 C45 C46 -176.5(3) . . . . ? C43 C44 C45 C46 7.1(5) . . . . ? C44 C45 C46 C47 -0.4(6) . . . . ? C45 C46 C47 C48 -5.2(5) . . . . ? C42 C43 C48 C47 -173.4(3) . . . . ? C44 C43 C48 C47 3.0(5) . . . . ? C42 C43 C48 C39 6.1(5) . . . . ? C44 C43 C48 C39 -177.5(3) . . . . ? C46 C47 C48 C43 3.7(5) . . . . ? C46 C47 C48 C39 -175.8(3) . . . . ? C40 C39 C48 C43 -1.9(5) . . . . ? S2 C39 C48 C43 179.2(2) . . . . ? C40 C39 C48 C47 177.6(3) . . . . ? S2 C39 C48 C47 -1.3(5) . . . . ? O7 C51 C52 C53 -179.7(3) . . . . ? C56 C51 C52 C53 -0.4(6) . . . . ? C51 C52 C53 C54 0.4(6) . . . . ? C52 C53 C54 C55 0.4(6) . . . . ? C53 C54 C55 C56 -1.2(6) . . . . ? O7 C51 C56 C55 178.9(3) . . . . ? C52 C51 C56 C55 -0.4(5) . . . . ? O7 C51 C56 C57 4.4(6) . . . . ? C52 C51 C56 C57 -175.0(3) . . . . ? C54 C55 C56 C51 1.3(6) . . . . ? C54 C55 C56 C57 176.3(4) . . . . ? C51 C56 C57 N7 -10.3(6) . . . . ? C55 C56 C57 N7 175.2(4) . . . . ? C63 C58 C59 C60 0.5(5) . . . . ? N7 C58 C59 C60 177.8(3) . . . . ? C58 C59 C60 C61 -1.2(6) . . . . ? C59 C60 C61 C62 0.4(6) . . . . ? C60 C61 C62 C63 1.1(5) . . . . ? C61 C62 C63 C58 -1.7(5) . . . . ? C61 C62 C63 N8 -179.9(3) . . . . ? C59 C58 C63 C62 0.9(5) . . . . ? N7 C58 C63 C62 -176.6(3) . . . . ? C59 C58 C63 N8 179.3(3) . . . . ? N7 C58 C63 N8 1.8(5) . . . . ? C73 C64 C65 C66 0.7(5) . . . . ? S3 C64 C65 C66 -179.3(3) . . . . ? C64 C65 C66 C67 -0.4(5) . . . . ? C65 C66 C67 C68 1.4(6) . . . . ? C66 C67 C68 C73 -2.6(6) . . . . ? C66 C67 C68 C69 179.3(4) . . . . ? C67 C68 C69 C70 175.3(4) . . . . ? C73 C68 C69 C70 -2.8(6) . . . . ? C67 C68 C69 N9 -2.1(6) . . . . ? C73 C68 C69 N9 179.7(3) . . . . ? N9 C69 C70 C71 179.4(4) . . . . ? C68 C69 C70 C71 2.1(6) . . . . ? C69 C70 C71 C72 -0.9(6) . . . . ? C70 C71 C72 C73 0.3(6) . . . . ? C71 C72 C73 C68 -1.0(5) . . . . ? C71 C72 C73 C64 -179.5(4) . . . . ? C67 C68 C73 C72 -175.9(3) . . . . ? C69 C68 C73 C72 2.2(5) . . . . ? C67 C68 C73 C64 2.7(5) . . . . ? C69 C68 C73 C64 -179.1(3) . . . . ? C65 C64 C73 C72 176.7(4) . . . . ? S3 C64 C73 C72 -3.2(5) . . . . ? C65 C64 C73 C68 -1.9(5) . . . . ? S3 C64 C73 C68 178.2(3) . . . . ? O10 C76 C77 C78 179.8(3) . . . . ? C81 C76 C77 C78 0.7(6) . . . . ? C76 C77 C78 C79 0.7(6) . . . . ? C77 C78 C79 C80 -0.7(6) . . . . ? C78 C79 C80 C81 -0.7(6) . . . . ? C79 C80 C81 C76 2.0(6) . . . . ? C79 C80 C81 C82 -179.7(4) . . . . ? O10 C76 C81 C80 178.9(3) . . . . ? C77 C76 C81 C80 -2.0(5) . . . . ? O10 C76 C81 C82 0.8(5) . . . . ? C77 C76 C81 C82 179.9(3) . . . . ? C80 C81 C82 N10 173.1(4) . . . . ? C76 C81 C82 N10 -8.7(6) . . . . ? C88 C83 C84 C85 -2.4(5) . . . . ? N10 C83 C84 C85 -179.6(3) . . . . ? C83 C84 C85 C86 0.5(6) . . . . ? C84 C85 C86 C87 0.9(6) . . . . ? C85 C86 C87 C88 -0.4(6) . . . . ? C86 C87 C88 C83 -1.4(5) . . . . ? C86 C87 C88 N11 178.2(3) . . . . ? C84 C83 C88 C87 2.8(5) . . . . ? N10 C83 C88 C87 -179.7(3) . . . . ? C84 C83 C88 N11 -176.8(3) . . . . ? N10 C83 C88 N11 0.6(5) . . . . ? C98 C89 C90 C91 -2.2(5) . . . . ? S4 C89 C90 C91 178.5(3) . . . . ? C89 C90 C91 C92 1.3(6) . . . . ? C90 C91 C92 C93 1.6(6) . . . . ? C91 C92 C93 C98 -3.5(5) . . . . ? C91 C92 C93 C94 178.9(3) . . . . ? C92 C93 C94 C95 172.0(3) . . . . ? C98 C93 C94 C95 -5.6(5) . . . . ? C92 C93 C94 N12 -4.8(5) . . . . ? C98 C93 C94 N12 177.6(3) . . . . ? N12 C94 C95 C96 -177.3(3) . . . . ? C93 C94 C95 C96 6.0(5) . . . . ? C94 C95 C96 C97 -1.8(6) . . . . ? C95 C96 C97 C98 -2.9(5) . . . . ? C96 C97 C98 C93 3.1(5) . . . . ? C96 C97 C98 C89 -175.9(3) . . . . ? C92 C93 C98 C97 -176.6(3) . . . . ? C94 C93 C98 C97 1.1(5) . . . . ? C92 C93 C98 C89 2.5(5) . . . . ? C94 C93 C98 C89 -179.8(3) . . . . ? C90 C89 C98 C97 179.4(3) . . . . ? S4 C89 C98 C97 -1.4(5) . . . . ? C90 C89 C98 C93 0.3(5) . . . . ? S4 C89 C98 C93 179.5(2) . . . . ? C6 C7 N1 C8 178.7(4) . . . . ? C6 C7 N1 Zn1 3.5(6) . . . . ? C9 C8 N1 C7 17.5(5) . . . . ? C13 C8 N1 C7 -162.9(3) . . . . ? C9 C8 N1 Zn1 -166.7(3) . . . . ? C13 C8 N1 Zn1 12.9(4) . . . . ? C12 C13 N2 S1 -6.6(5) . . . . ? C8 C13 N2 S1 176.2(2) . . . . ? C12 C13 N2 Zn1 166.8(3) . . . . ? C8 C13 N2 Zn1 -10.4(4) . . . . ? C20 C19 N3 C25 24.4(5) . . . . ? C18 C19 N3 C25 -153.4(4) . . . . ? C20 C19 N3 C24 -104.3(5) . . . . ? C18 C19 N3 C24 77.9(4) . . . . ? C31 C32 N4 C33 176.2(4) . . . . ? C31 C32 N4 Zn2 -15.6(6) . . . . ? C34 C33 N4 C32 -24.3(5) . . . . ? C38 C33 N4 C32 160.4(3) . . . . ? C34 C33 N4 Zn2 166.1(3) . . . . ? C38 C33 N4 Zn2 -9.3(4) . . . . ? C37 C38 N5 S2 -1.7(5) . . . . ? C33 C38 N5 S2 175.7(3) . . . . ? C37 C38 N5 Zn2 -177.0(3) . . . . ? C33 C38 N5 Zn2 0.3(4) . . . . ? C45 C44 N6 C49 -14.8(5) . . . . ? C43 C44 N6 C49 161.5(3) . . . . ? C45 C44 N6 C50 114.3(4) . . . . ? C43 C44 N6 C50 -69.3(4) . . . . ? C56 C57 N7 C58 176.6(3) . . . . ? C56 C57 N7 Zn4 0.3(5) . . . . ? C59 C58 N7 C57 22.3(5) . . . . ? C63 C58 N7 C57 -160.3(3) . . . . ? C59 C58 N7 Zn4 -160.9(3) . . . . ? C63 C58 N7 Zn4 16.5(4) . . . . ? C62 C63 N8 S3 -4.1(5) . . . . ? C58 C63 N8 S3 177.7(2) . . . . ? C62 C63 N8 Zn4 158.9(3) . . . . ? C58 C63 N8 Zn4 -19.3(4) . . . . ? C70 C69 N9 C75 111.0(5) . . . . ? C68 C69 N9 C75 -71.7(5) . . . . ? C70 C69 N9 C74 -19.1(6) . . . . ? C68 C69 N9 C74 158.2(4) . . . . ? C81 C82 N10 C83 178.0(3) . . . . ? C81 C82 N10 Zn3 -12.5(5) . . . . ? C84 C83 N10 C82 -15.7(5) . . . . ? C88 C83 N10 C82 166.9(3) . . . . ? C84 C83 N10 Zn3 173.8(3) . . . . ? C88 C83 N10 Zn3 -3.5(4) . . . . ? C87 C88 N11 S4 13.9(5) . . . . ? C83 C88 N11 S4 -166.5(3) . . . . ? C87 C88 N11 Zn3 -177.1(3) . . . . ? C83 C88 N11 Zn3 2.5(4) . . . . ? C95 C94 N12 C100 -15.4(5) . . . . ? C93 C94 N12 C100 161.4(3) . . . . ? C95 C94 N12 C99 112.2(4) . . . . ? C93 C94 N12 C99 -71.1(4) . . . . ? C2 C1 O1 Zn5 25.4(5) . . . . ? C6 C1 O1 Zn5 -153.8(3) . . . . ? C2 C1 O1 Zn1 -163.5(3) . . . . ? C6 C1 O1 Zn1 17.2(5) . . . . ? C27 C26 O4 Zn1 41.9(5) . . . . ? C31 C26 O4 Zn1 -137.6(3) . . . . ? C27 C26 O4 Zn2 -163.9(3) . . . . ? C31 C26 O4 Zn2 16.6(5) . . . . ? C52 C51 O7 Zn5 10.0(5) . . . . ? C56 C51 O7 Zn5 -169.3(3) . . . . ? C52 C51 O7 Zn4 -170.1(3) . . . . ? C56 C51 O7 Zn4 10.6(5) . . . . ? C77 C76 O10 Zn4 31.7(5) . . . . ? C81 C76 O10 Zn4 -149.2(3) . . . . ? C77 C76 O10 Zn3 -151.6(3) . . . . ? C81 C76 O10 Zn3 27.5(5) . . . . ? C13 N2 S1 O3 -43.1(3) . . . . ? Zn1 N2 S1 O3 144.47(18) . . . . ? C13 N2 S1 O2 -171.4(3) . . . . ? Zn1 N2 S1 O2 16.1(2) . . . . ? C13 N2 S1 C14 74.8(3) . . . . ? Zn1 N2 S1 C14 -97.6(2) . . . . ? C15 C14 S1 O3 120.6(3) . . . . ? C23 C14 S1 O3 -57.2(3) . . . . ? C15 C14 S1 O2 -115.6(3) . . . . ? C23 C14 S1 O2 66.6(3) . . . . ? C15 C14 S1 N2 -1.0(3) . . . . ? C23 C14 S1 N2 -178.9(3) . . . . ? Zn3 O6 S2 O5 29.3(2) . . . . ? Zn3 O6 S2 N5 -96.7(2) . . . . ? Zn3 O6 S2 C39 149.03(19) . . . . ? C38 N5 S2 O5 57.1(3) . . . . ? Zn2 N5 S2 O5 -128.22(19) . . . . ? C38 N5 S2 O6 -176.1(3) . . . . ? Zn2 N5 S2 O6 -1.5(2) . . . . ? C38 N5 S2 C39 -62.9(3) . . . . ? Zn2 N5 S2 C39 111.7(2) . . . . ? C40 C39 S2 O5 -139.2(3) . . . . ? C48 C39 S2 O5 39.7(3) . . . . ? C40 C39 S2 O6 96.8(3) . . . . ? C48 C39 S2 O6 -84.3(3) . . . . ? C40 C39 S2 N5 -15.9(3) . . . . ? C48 C39 S2 N5 163.0(3) . . . . ? C63 N8 S3 O8 -43.1(3) . . . . ? Zn4 N8 S3 O8 156.38(17) . . . . ? C63 N8 S3 O9 -171.1(2) . . . . ? Zn4 N8 S3 O9 28.3(2) . . . . ? C63 N8 S3 C64 74.6(3) . . . . ? Zn4 N8 S3 C64 -85.9(2) . . . . ? C65 C64 S3 O8 116.2(3) . . . . ? C73 C64 S3 O8 -63.9(3) . . . . ? C65 C64 S3 O9 -120.3(3) . . . . ? C73 C64 S3 O9 59.6(3) . . . . ? C65 C64 S3 N8 -5.8(3) . . . . ? C73 C64 S3 N8 174.1(3) . . . . ? Zn2 O12 S4 O11 24.2(2) . . . . ? Zn2 O12 S4 N11 -102.0(2) . . . . ? Zn2 O12 S4 C89 142.74(19) . . . . ? C88 N11 S4 O11 44.7(3) . . . . ? Zn3 N11 S4 O11 -123.03(18) . . . . ? C88 N11 S4 O12 171.4(3) . . . . ? Zn3 N11 S4 O12 3.7(2) . . . . ? C88 N11 S4 C89 -76.3(3) . . . . ? Zn3 N11 S4 C89 115.94(19) . . . . ? C90 C89 S4 O11 -135.8(3) . . . . ? C98 C89 S4 O11 45.0(3) . . . . ? C90 C89 S4 O12 101.7(3) . . . . ? C98 C89 S4 O12 -77.5(3) . . . . ? C90 C89 S4 N11 -11.7(3) . . . . ? C98 C89 S4 N11 169.1(3) . . . . ? C26 O4 Zn1 N2 68.7(3) . . . . ? Zn2 O4 Zn1 N2 -91.13(12) . . . . ? C26 O4 Zn1 N1 -21.3(3) . . . . ? Zn2 O4 Zn1 N1 178.87(11) . . . . ? C26 O4 Zn1 O1 -116.1(3) . . . . ? Zn2 O4 Zn1 O1 84.08(11) . . . . ? C26 O4 Zn1 O13 169.4(3) . . . . ? Zn2 O4 Zn1 O13 9.54(11) . . . . ? C26 O4 Zn1 Zn5 -154.6(3) . . . . ? Zn2 O4 Zn1 Zn5 45.53(9) . . . . ? C26 O4 Zn1 Zn2 159.8(3) . . . . ? C13 N2 Zn1 O4 -107.6(2) . . . . ? S1 N2 Zn1 O4 65.5(2) . . . . ? C13 N2 Zn1 N1 13.4(2) . . . . ? S1 N2 Zn1 N1 -173.5(2) . . . . ? C13 N2 Zn1 O1 82.2(3) . . . . ? S1 N2 Zn1 O1 -104.7(2) . . . . ? C13 N2 Zn1 O13 168.7(2) . . . . ? S1 N2 Zn1 O13 -18.2(2) . . . . ? C13 N2 Zn1 Zn5 139.36(19) . . . . ? S1 N2 Zn1 Zn5 -47.6(2) . . . . ? C13 N2 Zn1 Zn2 -150.4(2) . . . . ? S1 N2 Zn1 Zn2 22.7(2) . . . . ? C7 N1 Zn1 O4 -94.2(3) . . . . ? C8 N1 Zn1 O4 90.2(3) . . . . ? C7 N1 Zn1 N2 161.4(3) . . . . ? C8 N1 Zn1 N2 -14.2(2) . . . . ? C7 N1 Zn1 O1 8.2(3) . . . . ? C8 N1 Zn1 O1 -167.4(2) . . . . ? C7 N1 Zn1 O13 59.8(5) . . . . ? C8 N1 Zn1 O13 -115.8(3) . . . . ? C7 N1 Zn1 Zn5 26.8(3) . . . . ? C8 N1 Zn1 Zn5 -148.8(2) . . . . ? C7 N1 Zn1 Zn2 -91.5(4) . . . . ? C8 N1 Zn1 Zn2 92.9(4) . . . . ? C1 O1 Zn1 O4 103.6(3) . . . . ? Zn5 O1 Zn1 O4 -83.28(12) . . . . ? C1 O1 Zn1 N2 -85.9(4) . . . . ? Zn5 O1 Zn1 N2 87.2(2) . . . . ? C1 O1 Zn1 N1 -18.8(3) . . . . ? Zn5 O1 Zn1 N1 154.36(12) . . . . ? C1 O1 Zn1 O13 -179.2(3) . . . . ? Zn5 O1 Zn1 O13 -6.07(11) . . . . ? C1 O1 Zn1 Zn5 -173.1(4) . . . . ? C1 O1 Zn1 Zn2 144.9(3) . . . . ? Zn5 O1 Zn1 Zn2 -41.94(10) . . . . ? Zn5 O13 Zn1 O4 110.40(13) . . . . ? Zn2 O13 Zn1 O4 -9.87(11) . . . . ? Zn5 O13 Zn1 N2 -144.32(12) . . . . ? Zn2 O13 Zn1 N2 95.41(13) . . . . ? Zn5 O13 Zn1 N1 -47.5(3) . . . . ? Zn2 O13 Zn1 N1 -167.7(2) . . . . ? Zn5 O13 Zn1 O1 6.08(11) . . . . ? Zn2 O13 Zn1 O1 -114.19(13) . . . . ? Zn2 O13 Zn1 Zn5 -120.27(17) . . . . ? Zn5 O13 Zn1 Zn2 120.27(17) . . . . ? Zn5 O13 Zn2 N4 -165.15(16) . . . . ? Zn1 O13 Zn2 N4 -61.2(2) . . . . ? Zn5 O13 Zn2 O12 -3.99(17) . . . . ? Zn1 O13 Zn2 O12 99.99(11) . . . . ? Zn5 O13 Zn2 N5 99.28(17) . . . . ? Zn1 O13 Zn2 N5 -156.74(11) . . . . ? Zn5 O13 Zn2 O4 -94.67(16) . . . . ? Zn1 O13 Zn2 O4 9.31(10) . . . . ? Zn5 O13 Zn2 Zn1 -103.98(19) . . . . ? C32 N4 Zn2 O13 93.4(3) . . . . ? C33 N4 Zn2 O13 -97.8(3) . . . . ? C32 N4 Zn2 O12 -64.5(3) . . . . ? C33 N4 Zn2 O12 104.2(2) . . . . ? C32 N4 Zn2 N5 -161.6(3) . . . . ? C33 N4 Zn2 N5 7.1(2) . . . . ? C32 N4 Zn2 O4 24.8(3) . . . . ? C33 N4 Zn2 O4 -166.4(2) . . . . ? C32 N4 Zn2 Zn1 54.1(3) . . . . ? C33 N4 Zn2 Zn1 -137.2(2) . . . . ? S4 O12 Zn2 O13 149.0(2) . . . . ? S4 O12 Zn2 N4 -44.8(2) . . . . ? S4 O12 Zn2 N5 40.6(2) . . . . ? S4 O12 Zn2 O4 -130.83(19) . . . . ? S4 O12 Zn2 Zn1 -168.60(17) . . . . ? C38 N5 Zn2 O13 136.2(2) . . . . ? S2 N5 Zn2 O13 -38.7(2) . . . . ? C38 N5 Zn2 N4 -4.1(2) . . . . ? S2 N5 Zn2 N4 -179.1(2) . . . . ? C38 N5 Zn2 O12 -124.3(2) . . . . ? S2 N5 Zn2 O12 60.7(2) . . . . ? C38 N5 Zn2 O4 21.2(6) . . . . ? S2 N5 Zn2 O4 -153.8(3) . . . . ? C38 N5 Zn2 Zn1 109.6(2) . . . . ? S2 N5 Zn2 Zn1 -65.3(3) . . . . ? C26 O4 Zn2 O13 -169.6(3) . . . . ? Zn1 O4 Zn2 O13 -10.04(11) . . . . ? C26 O4 Zn2 N4 -26.3(3) . . . . ? Zn1 O4 Zn2 N4 133.27(12) . . . . ? C26 O4 Zn2 O12 94.8(3) . . . . ? Zn1 O4 Zn2 O12 -105.57(11) . . . . ? C26 O4 Zn2 N5 -51.3(6) . . . . ? Zn1 O4 Zn2 N5 108.3(4) . . . . ? C26 O4 Zn2 Zn1 -159.6(4) . . . . ? O4 Zn1 Zn2 O13 165.21(17) . . . . ? N2 Zn1 Zn2 O13 -94.25(15) . . . . ? N1 Zn1 Zn2 O13 161.8(3) . . . . ? O1 Zn1 Zn2 O13 63.14(14) . . . . ? Zn5 Zn1 Zn2 O13 36.04(12) . . . . ? O4 Zn1 Zn2 N4 -51.35(15) . . . . ? N2 Zn1 Zn2 N4 49.19(13) . . . . ? N1 Zn1 Zn2 N4 -54.7(3) . . . . ? O1 Zn1 Zn2 N4 -153.43(13) . . . . ? O13 Zn1 Zn2 N4 143.44(16) . . . . ? Zn5 Zn1 Zn2 N4 179.47(10) . . . . ? O4 Zn1 Zn2 O12 78.75(13) . . . . ? N2 Zn1 Zn2 O12 179.29(11) . . . . ? N1 Zn1 Zn2 O12 75.4(3) . . . . ? O1 Zn1 Zn2 O12 -23.33(11) . . . . ? O13 Zn1 Zn2 O12 -86.46(14) . . . . ? Zn5 Zn1 Zn2 O12 -50.43(7) . . . . ? O4 Zn1 Zn2 N5 -155.18(18) . . . . ? N2 Zn1 Zn2 N5 -54.64(17) . . . . ? N1 Zn1 Zn2 N5 -158.6(3) . . . . ? O1 Zn1 Zn2 N5 102.75(16) . . . . ? O13 Zn1 Zn2 N5 39.61(19) . . . . ? Zn5 Zn1 Zn2 N5 75.65(15) . . . . ? N2 Zn1 Zn2 O4 100.54(14) . . . . ? N1 Zn1 Zn2 O4 -3.4(3) . . . . ? O1 Zn1 Zn2 O4 -102.07(14) . . . . ? O13 Zn1 Zn2 O4 -165.21(17) . . . . ? Zn5 Zn1 Zn2 O4 -129.17(11) . . . . ? Zn5 O14 Zn3 N10 -166.14(16) . . . . ? Zn4 O14 Zn3 N10 -63.1(2) . . . . ? Zn5 O14 Zn3 O10 -96.63(15) . . . . ? Zn4 O14 Zn3 O10 6.37(10) . . . . ? Zn5 O14 Zn3 N11 101.45(16) . . . . ? Zn4 O14 Zn3 N11 -155.55(11) . . . . ? Zn5 O14 Zn3 O6 -6.82(16) . . . . ? Zn4 O14 Zn3 O6 96.18(11) . . . . ? Zn5 O14 Zn3 Zn4 -103.00(17) . . . . ? C82 N10 Zn3 O14 94.6(3) . . . . ? C83 N10 Zn3 O14 -95.2(3) . . . . ? C82 N10 Zn3 O10 27.5(3) . . . . ? C83 N10 Zn3 O10 -162.3(2) . . . . ? C82 N10 Zn3 N11 -166.4(3) . . . . ? C83 N10 Zn3 N11 3.8(2) . . . . ? C82 N10 Zn3 O6 -63.6(3) . . . . ? C83 N10 Zn3 O6 106.6(2) . . . . ? C82 N10 Zn3 Zn4 52.9(3) . . . . ? C83 N10 Zn3 Zn4 -136.9(2) . . . . ? C76 O10 Zn3 O14 175.6(3) . . . . ? Zn4 O10 Zn3 O14 -6.86(11) . . . . ? C76 O10 Zn3 N10 -35.8(3) . . . . ? Zn4 O10 Zn3 N10 141.75(12) . . . . ? C76 O10 Zn3 N11 -87.1(4) . . . . ? Zn4 O10 Zn3 N11 90.5(3) . . . . ? C76 O10 Zn3 O6 75.0(3) . . . . ? Zn4 O10 Zn3 O6 -107.46(11) . . . . ? C76 O10 Zn3 Zn4 -177.5(3) . . . . ? C88 N11 Zn3 O14 142.4(2) . . . . ? S4 N11 Zn3 O14 -49.0(2) . . . . ? C88 N11 Zn3 N10 -3.4(2) . . . . ? S4 N11 Zn3 N10 165.2(2) . . . . ? C88 N11 Zn3 O10 48.7(5) . . . . ? S4 N11 Zn3 O10 -142.6(3) . . . . ? C88 N11 Zn3 O6 -112.7(2) . . . . ? S4 N11 Zn3 O6 56.0(2) . . . . ? C88 N11 Zn3 Zn4 117.8(2) . . . . ? S4 N11 Zn3 Zn4 -73.5(2) . . . . ? S2 O6 Zn3 O14 145.30(19) . . . . ? S2 O6 Zn3 N10 -46.8(2) . . . . ? S2 O6 Zn3 O10 -135.26(19) . . . . ? S2 O6 Zn3 N11 39.1(2) . . . . ? S2 O6 Zn3 Zn4 -172.25(17) . . . . ? C76 O10 Zn4 N8 83.7(3) . . . . ? Zn3 O10 Zn4 N8 -93.55(13) . . . . ? C76 O10 Zn4 N7 -5.1(3) . . . . ? Zn3 O10 Zn4 N7 177.64(11) . . . . ? C76 O10 Zn4 O7 -101.5(3) . . . . ? Zn3 O10 Zn4 O7 81.18(12) . . . . ? C76 O10 Zn4 O14 -176.1(3) . . . . ? Zn3 O10 Zn4 O14 6.63(10) . . . . ? C76 O10 Zn4 Zn5 -140.4(3) . . . . ? Zn3 O10 Zn4 Zn5 42.35(9) . . . . ? C76 O10 Zn4 Zn3 177.3(4) . . . . ? C63 N8 Zn4 O10 -92.1(2) . . . . ? S3 N8 Zn4 O10 70.3(2) . . . . ? C63 N8 Zn4 N7 21.9(2) . . . . ? S3 N8 Zn4 N7 -175.7(2) . . . . ? C63 N8 Zn4 O7 96.9(3) . . . . ? S3 N8 Zn4 O7 -100.7(2) . . . . ? C63 N8 Zn4 O14 -174.4(2) . . . . ? S3 N8 Zn4 O14 -12.0(2) . . . . ? C63 N8 Zn4 Zn5 153.77(17) . . . . ? S3 N8 Zn4 Zn5 -43.8(2) . . . . ? C63 N8 Zn4 Zn3 -133.33(19) . . . . ? S3 N8 Zn4 Zn3 29.1(2) . . . . ? C57 N7 Zn4 O10 -97.6(3) . . . . ? C58 N7 Zn4 O10 85.8(2) . . . . ? C57 N7 Zn4 N8 155.8(3) . . . . ? C58 N7 Zn4 N8 -20.9(2) . . . . ? C57 N7 Zn4 O7 9.2(3) . . . . ? C58 N7 Zn4 O7 -167.5(2) . . . . ? C57 N7 Zn4 O14 49.9(6) . . . . ? C58 N7 Zn4 O14 -126.8(4) . . . . ? C57 N7 Zn4 Zn5 21.0(4) . . . . ? C58 N7 Zn4 Zn5 -155.69(19) . . . . ? C57 N7 Zn4 Zn3 -94.1(4) . . . . ? C58 N7 Zn4 Zn3 89.3(3) . . . . ? C51 O7 Zn4 O10 101.4(3) . . . . ? Zn5 O7 Zn4 O10 -78.65(12) . . . . ? C51 O7 Zn4 N8 -87.4(3) . . . . ? Zn5 O7 Zn4 N8 92.56(19) . . . . ? C51 O7 Zn4 N7 -14.8(3) . . . . ? Zn5 O7 Zn4 N7 165.13(12) . . . . ? C51 O7 Zn4 O14 176.2(3) . . . . ? Zn5 O7 Zn4 O14 -3.92(10) . . . . ? C51 O7 Zn4 Zn5 -179.9(3) . . . . ? C51 O7 Zn4 Zn3 140.5(3) . . . . ? Zn5 O7 Zn4 Zn3 -39.62(9) . . . . ? Zn5 O14 Zn4 O10 112.55(12) . . . . ? Zn3 O14 Zn4 O10 -6.56(10) . . . . ? Zn5 O14 Zn4 N8 -140.54(11) . . . . ? Zn3 O14 Zn4 N8 100.36(12) . . . . ? Zn5 O14 Zn4 N7 -37.8(5) . . . . ? Zn3 O14 Zn4 N7 -156.9(4) . . . . ? Zn5 O14 Zn4 O7 3.97(10) . . . . ? Zn3 O14 Zn4 O7 -115.13(12) . . . . ? Zn3 O14 Zn4 Zn5 -119.10(15) . . . . ? Zn5 O14 Zn4 Zn3 119.10(15) . . . . ? O14 Zn3 Zn4 O10 169.82(16) . . . . ? N10 Zn3 Zn4 O10 -44.01(15) . . . . ? N11 Zn3 Zn4 O10 -152.43(17) . . . . ? O6 Zn3 Zn4 O10 77.20(13) . . . . ? O14 Zn3 Zn4 N8 -90.65(15) . . . . ? N10 Zn3 Zn4 N8 55.52(13) . . . . ? O10 Zn3 Zn4 N8 99.54(14) . . . . ? N11 Zn3 Zn4 N8 -52.90(16) . . . . ? O6 Zn3 Zn4 N8 176.73(12) . . . . ? O14 Zn3 Zn4 N7 164.8(2) . . . . ? N10 Zn3 Zn4 N7 -49.0(2) . . . . ? O10 Zn3 Zn4 N7 -5.0(2) . . . . ? N11 Zn3 Zn4 N7 -157.4(3) . . . . ? O6 Zn3 Zn4 N7 72.2(2) . . . . ? O14 Zn3 Zn4 O7 63.23(14) . . . . ? N10 Zn3 Zn4 O7 -150.59(12) . . . . ? O10 Zn3 Zn4 O7 -106.58(14) . . . . ? N11 Zn3 Zn4 O7 100.99(15) . . . . ? O6 Zn3 Zn4 O7 -29.38(11) . . . . ? N10 Zn3 Zn4 O14 146.17(15) . . . . ? O10 Zn3 Zn4 O14 -169.82(16) . . . . ? N11 Zn3 Zn4 O14 37.75(17) . . . . ? O6 Zn3 Zn4 O14 -92.62(13) . . . . ? O14 Zn3 Zn4 Zn5 36.92(11) . . . . ? N10 Zn3 Zn4 Zn5 -176.91(10) . . . . ? O10 Zn3 Zn4 Zn5 -132.90(11) . . . . ? N11 Zn3 Zn4 Zn5 74.67(13) . . . . ? O6 Zn3 Zn4 Zn5 -55.70(7) . . . . ? Zn3 O14 Zn5 O13 -27.3(2) . . . . ? Zn4 O14 Zn5 O13 -131.03(13) . . . . ? Zn3 O14 Zn5 O1 -139.22(13) . . . . ? Zn4 O14 Zn5 O1 117.10(12) . . . . ? Zn3 O14 Zn5 O7 99.62(15) . . . . ? Zn4 O14 Zn5 O7 -4.06(11) . . . . ? Zn3 O14 Zn5 Zn4 103.68(18) . . . . ? Zn3 O14 Zn5 Zn1 -85.5(2) . . . . ? Zn4 O14 Zn5 Zn1 170.82(5) . . . . ? Zn2 O13 Zn5 O14 -33.2(2) . . . . ? Zn1 O13 Zn5 O14 -136.98(12) . . . . ? Zn2 O13 Zn5 O1 97.45(16) . . . . ? Zn1 O13 Zn5 O1 -6.29(11) . . . . ? Zn2 O13 Zn5 O7 -143.01(14) . . . . ? Zn1 O13 Zn5 O7 113.26(13) . . . . ? Zn2 O13 Zn5 Zn4 -92.29(19) . . . . ? Zn1 O13 Zn5 Zn4 163.97(4) . . . . ? Zn2 O13 Zn5 Zn1 103.7(2) . . . . ? C1 O1 Zn5 O14 -49.0(3) . . . . ? Zn1 O1 Zn5 O14 138.05(11) . . . . ? C1 O1 Zn5 O13 179.5(3) . . . . ? Zn1 O1 Zn5 O13 6.50(11) . . . . ? C1 O1 Zn5 O7 56.0(3) . . . . ? Zn1 O1 Zn5 O7 -117.00(11) . . . . ? C1 O1 Zn5 Zn4 7.5(4) . . . . ? Zn1 O1 Zn5 Zn4 -165.50(4) . . . . ? C1 O1 Zn5 Zn1 173.0(4) . . . . ? C51 O7 Zn5 O14 -175.9(3) . . . . ? Zn4 O7 Zn5 O14 4.22(11) . . . . ? C51 O7 Zn5 O13 -45.1(3) . . . . ? Zn4 O7 Zn5 O13 134.96(11) . . . . ? C51 O7 Zn5 O1 56.2(3) . . . . ? Zn4 O7 Zn5 O1 -123.76(11) . . . . ? C51 O7 Zn5 Zn4 179.9(4) . . . . ? C51 O7 Zn5 Zn1 7.7(3) . . . . ? Zn4 O7 Zn5 Zn1 -172.22(4) . . . . ? O10 Zn4 Zn5 O14 -65.38(13) . . . . ? N8 Zn4 Zn5 O14 54.54(15) . . . . ? N7 Zn4 Zn5 O14 167.36(16) . . . . ? O7 Zn4 Zn5 O14 -173.89(16) . . . . ? Zn3 Zn4 Zn5 O14 -37.63(11) . . . . ? O10 Zn4 Zn5 O13 27.43(15) . . . . ? N8 Zn4 Zn5 O13 147.34(16) . . . . ? N7 Zn4 Zn5 O13 -99.84(17) . . . . ? O7 Zn4 Zn5 O13 -81.08(17) . . . . ? O14 Zn4 Zn5 O13 92.81(18) . . . . ? Zn3 Zn4 Zn5 O13 55.18(13) . . . . ? O10 Zn4 Zn5 O1 -165.79(13) . . . . ? N8 Zn4 Zn5 O1 -45.87(14) . . . . ? N7 Zn4 Zn5 O1 66.95(15) . . . . ? O7 Zn4 Zn5 O1 85.70(15) . . . . ? O14 Zn4 Zn5 O1 -100.41(16) . . . . ? Zn3 Zn4 Zn5 O1 -138.04(11) . . . . ? O10 Zn4 Zn5 O7 108.51(13) . . . . ? N8 Zn4 Zn5 O7 -131.57(15) . . . . ? N7 Zn4 Zn5 O7 -18.75(15) . . . . ? O14 Zn4 Zn5 O7 173.89(16) . . . . ? Zn3 Zn4 Zn5 O7 136.26(11) . . . . ? O10 Zn4 Zn5 Zn1 140.00(12) . . . . ? N8 Zn4 Zn5 Zn1 -100.09(14) . . . . ? N7 Zn4 Zn5 Zn1 12.73(16) . . . . ? O7 Zn4 Zn5 Zn1 31.49(15) . . . . ? O14 Zn4 Zn5 Zn1 -154.63(15) . . . . ? Zn3 Zn4 Zn5 Zn1 167.74(10) . . . . ? O4 Zn1 Zn5 O14 19.69(16) . . . . ? N2 Zn1 Zn5 O14 137.62(17) . . . . ? N1 Zn1 Zn5 O14 -113.53(17) . . . . ? O1 Zn1 Zn5 O14 -82.76(18) . . . . ? O13 Zn1 Zn5 O14 87.74(19) . . . . ? Zn2 Zn1 Zn5 O14 50.68(14) . . . . ? O4 Zn1 Zn5 O13 -68.05(14) . . . . ? N2 Zn1 Zn5 O13 49.89(16) . . . . ? N1 Zn1 Zn5 O13 158.74(16) . . . . ? O1 Zn1 Zn5 O13 -170.50(17) . . . . ? Zn2 Zn1 Zn5 O13 -37.06(12) . . . . ? O4 Zn1 Zn5 O1 102.45(14) . . . . ? N2 Zn1 Zn5 O1 -139.61(15) . . . . ? N1 Zn1 Zn5 O1 -30.76(15) . . . . ? O13 Zn1 Zn5 O1 170.50(17) . . . . ? Zn2 Zn1 Zn5 O1 133.44(12) . . . . ? O4 Zn1 Zn5 O7 -166.80(12) . . . . ? N2 Zn1 Zn5 O7 -48.87(14) . . . . ? N1 Zn1 Zn5 O7 59.98(14) . . . . ? O1 Zn1 Zn5 O7 90.75(15) . . . . ? O13 Zn1 Zn5 O7 -98.75(16) . . . . ? Zn2 Zn1 Zn5 O7 -135.81(10) . . . . ? O4 Zn1 Zn5 Zn4 167.08(12) . . . . ? N2 Zn1 Zn5 Zn4 -74.98(14) . . . . ? N1 Zn1 Zn5 Zn4 33.87(15) . . . . ? O1 Zn1 Zn5 Zn4 64.63(15) . . . . ? O13 Zn1 Zn5 Zn4 -124.87(16) . . . . ? Zn2 Zn1 Zn5 Zn4 -161.93(10) . . . . ? 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 O13 H13O O2 0.77(4) 2.08(4) 2.659(4) 133(4) . O14 H14O O9 0.784(19) 2.03(3) 2.696(4) 143(4) . # END of CIF # Attachment '- 14.cif' #\#CIF_1.1 # CIF produced by WinGX routine CIF_UPDATE # Created on 2012-02-24 at 15:50:13 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.4 # Request file : h:\monocristal\wingx\files\archive.reqdat # CIF files read : be28mj1n struct #------------------ SECTION 1. GLOBAL INFORMATION ---------------------------# data_CdSALDS _database_code_depnum_ccdc_archive 'CCDC 877816' #TrackingRef '- 14.cif' _audit_creation_date 2012-02-24T15:50:13-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C58 H66 Cd2 N6 O10 S6, 2(C3 H6 O)' _chemical_formula_sum 'C64 H78 Cd2 N6 O12 S6' _chemical_formula_weight 1540.56 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7654(13) _cell_length_b 12.5139(19) _cell_length_c 16.216(2) _cell_angle_alpha 92.087(3) _cell_angle_beta 96.528(3) _cell_angle_gamma 101.086(3) _cell_volume 1731.1(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 1016 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 26 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.478 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.857 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.761682 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromador graphite _diffrn_measurement_device_type 'Smart-CCD-1000 BRUKER' _diffrn_measurement_method 'omega scans' _diffrn_reflns_av_R_equivalents 0.0533 _diffrn_reflns_av_unetI/netI 0.0726 _diffrn_reflns_number 17473 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.44 _diffrn_reflns_theta_full 26.44 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 7009 _reflns_number_gt 4444 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'BRUKER Smart' _computing_cell_refinement 'BRUKER Smart' _computing_data_reduction 'BRUKER Saint' _computing_structure_solution 'DIRDIF99 (Beurskens et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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^)+(0.0290P)^2^+2.9309P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7009 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.07 _refine_ls_restrained_S_all 1.07 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.829 _refine_diff_density_min -1.25 _refine_diff_density_rms 0.096 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd1 Cd 0.95795(5) 0.87519(3) 0.94211(2) 0.03996(13) Uani 1 1 d . . . O1 O 0.8771(4) 0.9657(3) 1.0507(2) 0.0414(8) Uani 1 1 d . . . C1 C 0.8229(6) 0.9170(4) 1.1161(3) 0.0404(12) Uani 1 1 d . . . C2 C 0.8600(7) 0.9695(5) 1.1957(3) 0.0527(15) Uani 1 1 d . . . H2 H 0.9253 1.038 1.202 0.063 Uiso 1 1 calc R . . C3 C 0.8036(7) 0.9238(5) 1.2646(4) 0.0641(17) Uani 1 1 d . . . H3 H 0.8328 0.961 1.3164 0.077 Uiso 1 1 calc R . . C4 C 0.7039(8) 0.8231(5) 1.2577(4) 0.0715(19) Uani 1 1 d . . . H4 H 0.6634 0.7927 1.3041 0.086 Uiso 1 1 calc R . . C5 C 0.6668(7) 0.7699(5) 1.1819(4) 0.0615(17) Uani 1 1 d . . . H5 H 0.6002 0.7019 1.1773 0.074 Uiso 1 1 calc R . . C6 C 0.7237(6) 0.8119(4) 1.1094(3) 0.0439(13) Uani 1 1 d . . . C7 C 0.6822(6) 0.7411(4) 1.0353(3) 0.0456(13) Uani 1 1 d . . . H7 H 0.6093 0.6773 1.0393 0.055 Uiso 1 1 calc R . . N1 N 0.7322(5) 0.7539(3) 0.9642(3) 0.0417(10) Uani 1 1 d . . . C8 C 0.6801(6) 0.6715(4) 0.8998(3) 0.0417(12) Uani 1 1 d . . . C9 C 0.5269(6) 0.6129(4) 0.8854(4) 0.0533(15) Uani 1 1 d . . . H9 H 0.4542 0.6279 0.9195 0.064 Uiso 1 1 calc R . . C10 C 0.4806(7) 0.5335(5) 0.8223(4) 0.0599(16) Uani 1 1 d . . . H10 H 0.3784 0.4938 0.8146 0.072 Uiso 1 1 calc R . . C11 C 0.5862(7) 0.5131(5) 0.7705(4) 0.0581(16) Uani 1 1 d . . . H11 H 0.556 0.4584 0.7282 0.07 Uiso 1 1 calc R . . C12 C 0.7377(7) 0.5737(4) 0.7809(3) 0.0489(14) Uani 1 1 d . . . H12 H 0.8072 0.5605 0.7443 0.059 Uiso 1 1 calc R . . C13 C 0.7875(6) 0.6537(4) 0.8447(3) 0.0423(12) Uani 1 1 d . . . N2 N 0.9378(5) 0.7221(3) 0.8587(2) 0.0398(10) Uani 1 1 d . . . S1 S 1.08132(15) 0.70253(11) 0.81415(8) 0.0432(3) Uani 1 1 d . . . O2 O 1.2161(4) 0.7761(3) 0.8550(2) 0.0514(10) Uani 1 1 d . . . O3 O 1.0922(4) 0.5889(3) 0.8072(2) 0.0536(10) Uani 1 1 d . . . C14 C 1.0527(6) 0.7446(4) 0.7101(3) 0.0422(12) Uani 1 1 d . . . C15 C 0.9211(6) 0.7832(4) 0.6840(3) 0.0488(14) Uani 1 1 d . . . H15 H 0.8475 0.7876 0.7204 0.059 Uiso 1 1 calc R . . C16 C 0.8960(7) 0.8161(5) 0.6029(4) 0.0588(16) Uani 1 1 d . . . H16 H 0.8033 0.8385 0.5847 0.071 Uiso 1 1 calc R . . C17 C 1.0064(7) 0.8156(5) 0.5505(4) 0.0579(16) Uani 1 1 d . . . H17 H 0.9881 0.8381 0.4969 0.07 Uiso 1 1 calc R . . C18 C 1.1478(7) 0.7818(4) 0.5755(3) 0.0475(13) Uani 1 1 d . . . C19 C 1.2669(8) 0.7825(5) 0.5212(3) 0.0573(16) Uani 1 1 d . . . C20 C 1.3945(8) 0.7389(5) 0.5460(4) 0.0644(17) Uani 1 1 d . . . H20 H 1.4709 0.7385 0.5107 0.077 Uiso 1 1 calc R . . C21 C 1.4122(7) 0.6945(5) 0.6241(4) 0.0632(17) Uani 1 1 d . . . H21 H 1.4989 0.6635 0.6391 0.076 Uiso 1 1 calc R . . C22 C 1.3046(6) 0.6961(4) 0.6780(3) 0.0520(14) Uani 1 1 d . . . H22 H 1.3198 0.668 0.7299 0.062 Uiso 1 1 calc R . . C23 C 1.1702(6) 0.7401(4) 0.6558(3) 0.0430(13) Uani 1 1 d . . . N3 N 1.2424(7) 0.8260(5) 0.4420(3) 0.0736(16) Uani 1 1 d . . . C24 C 1.2495(10) 0.9430(6) 0.4425(5) 0.104(3) Uani 1 1 d . . . H24A H 1.3569 0.9804 0.4505 0.156 Uiso 1 1 calc R . . H24B H 1.1964 0.9651 0.4869 0.156 Uiso 1 1 calc R . . H24C H 1.1998 0.9609 0.3904 0.156 Uiso 1 1 calc R . . C25 C 1.3315(11) 0.7919(7) 0.3790(4) 0.113(3) Uani 1 1 d . . . H25A H 1.3205 0.7139 0.3771 0.169 Uiso 1 1 calc R . . H25B H 1.4401 0.8253 0.3925 0.169 Uiso 1 1 calc R . . H25C H 1.2929 0.8138 0.3257 0.169 Uiso 1 1 calc R . . O4 O 1.1011(5) 0.7995(3) 1.0483(2) 0.0578(10) Uani 1 1 d . . . S2 S 1.0501(2) 0.68088(14) 1.06488(11) 0.0520(5) Uani 0.8664(19) 1 d P A 1 C26 C 1.076(2) 0.6801(16) 1.1756(8) 0.087(5) Uani 0.8664(19) 1 d P A 1 H26A H 1.0142 0.7271 1.1983 0.13 Uiso 0.8664(19) 1 calc PR A 1 H26B H 1.1841 0.7056 1.1961 0.13 Uiso 0.8664(19) 1 calc PR A 1 H26C H 1.042 0.6072 1.1919 0.13 Uiso 0.8664(19) 1 calc PR A 1 C27 C 1.2084(11) 0.6171(11) 1.0450(7) 0.091(4) Uani 0.8664(19) 1 d P A 1 H27A H 1.3026 0.6541 1.0783 0.136 Uiso 0.8664(19) 1 calc PR A 1 H27B H 1.2224 0.6205 0.9873 0.136 Uiso 0.8664(19) 1 calc PR A 1 H27C H 1.1855 0.5422 1.0588 0.136 Uiso 0.8664(19) 1 calc PR A 1 S2B S 1.1754(14) 0.7203(9) 1.0997(7) 0.0520(5) Uani 0.1336(19) 1 d P A 2 C26B C 1.037(17) 0.662(12) 1.154(7) 0.087(5) Uani 0.1336(19) 1 d P A 2 H26D H 1.0766 0.6117 1.1896 0.13 Uiso 0.1336(19) 1 calc PR A 2 H26E H 0.9492 0.623 1.1162 0.13 Uiso 0.1336(19) 1 calc PR A 2 H26F H 1.0036 0.7166 1.1863 0.13 Uiso 0.1336(19) 1 calc PR A 2 C27B C 1.137(9) 0.608(8) 1.033(6) 0.091(4) Uani 0.1336(19) 1 d P A 2 H27D H 1.189 0.6239 0.9848 0.136 Uiso 0.1336(19) 1 calc PR A 2 H27E H 1.0258 0.5876 1.0168 0.136 Uiso 0.1336(19) 1 calc PR A 2 H27F H 1.1735 0.5492 1.0601 0.136 Uiso 0.1336(19) 1 calc PR A 2 O5 O 0.7936(5) 0.9376(4) 0.8358(2) 0.0733(13) Uani 1 1 d . . . S3 S 0.6787(2) 1.00877(15) 0.82116(11) 0.0592(5) Uani 0.8664(19) 1 d P A 1 C28 C 0.5822(11) 1.0081(10) 0.9110(8) 0.075(3) Uani 0.8664(19) 1 d P A 1 H28A H 0.6528 1.048 0.9563 0.113 Uiso 0.8664(19) 1 calc PR A 1 H28B H 0.5483 0.9343 0.9253 0.113 Uiso 0.8664(19) 1 calc PR A 1 H28C H 0.4929 1.0418 0.9003 0.113 Uiso 0.8664(19) 1 calc PR A 1 C29 C 0.5328(11) 0.9337(18) 0.7528(12) 0.108(4) Uani 0.8664(19) 1 d P A 1 H29A H 0.4926 0.8661 0.7762 0.161 Uiso 0.8664(19) 1 calc PR A 1 H29B H 0.5732 0.9188 0.7019 0.161 Uiso 0.8664(19) 1 calc PR A 1 H29C H 0.4503 0.9736 0.7417 0.161 Uiso 0.8664(19) 1 calc PR A 1 S3B S 0.6049(14) 0.9002(10) 0.8317(8) 0.0592(5) Uani 0.1336(19) 1 d P A 2 C28B C 0.534(9) 0.969(8) 0.910(6) 0.075(3) Uani 0.1336(19) 1 d P A 2 H28D H 0.6122 0.9836 0.9581 0.113 Uiso 0.1336(19) 1 calc PR A 2 H28E H 0.4408 0.9239 0.9251 0.113 Uiso 0.1336(19) 1 calc PR A 2 H28F H 0.5111 1.036 0.8909 0.113 Uiso 0.1336(19) 1 calc PR A 2 C29B C 0.481(11) 0.936(14) 0.748(9) 0.108(4) Uani 0.1336(19) 1 d P A 2 H29D H 0.5159 0.9167 0.696 0.161 Uiso 0.1336(19) 1 calc PR A 2 H29E H 0.485 1.0135 0.7516 0.161 Uiso 0.1336(19) 1 calc PR A 2 H29F H 0.3756 0.8982 0.7493 0.161 Uiso 0.1336(19) 1 calc PR A 2 O6 O 0.6394(7) 0.6366(6) 0.4200(4) 0.118(2) Uani 1 1 d . . . C30 C 0.7411(10) 0.5926(6) 0.4355(5) 0.074(2) Uani 1 1 d . . . C31 C 0.8707(9) 0.5967(7) 0.3809(5) 0.104(3) Uani 1 1 d . . . H31A H 0.9649 0.6422 0.4083 0.156 Uiso 1 1 calc R . . H31B H 0.8408 0.6261 0.329 0.156 Uiso 1 1 calc R . . H31C H 0.8886 0.5243 0.3706 0.156 Uiso 1 1 calc R . . C32 C 0.7687(11) 0.5411(6) 0.5173(5) 0.111(3) Uani 1 1 d . . . H32A H 0.6746 0.5307 0.5436 0.167 Uiso 1 1 calc R . . H32B H 0.8517 0.588 0.5528 0.167 Uiso 1 1 calc R . . H32C H 0.7972 0.4718 0.5075 0.167 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cd1 0.0411(2) 0.0339(2) 0.0458(2) 0.00307(16) 0.01450(16) 0.00434(16) O1 0.050(2) 0.035(2) 0.0421(19) 0.0057(16) 0.0175(16) 0.0076(16) C1 0.037(3) 0.041(3) 0.050(3) 0.009(3) 0.021(2) 0.013(2) C2 0.060(4) 0.050(4) 0.052(3) 0.007(3) 0.021(3) 0.010(3) C3 0.083(5) 0.068(4) 0.047(3) 0.002(3) 0.029(3) 0.017(4) C4 0.096(5) 0.065(5) 0.063(4) 0.022(4) 0.046(4) 0.015(4) C5 0.066(4) 0.051(4) 0.072(4) 0.015(3) 0.036(3) 0.004(3) C6 0.042(3) 0.038(3) 0.057(3) 0.012(3) 0.020(3) 0.009(2) C7 0.041(3) 0.035(3) 0.061(4) 0.010(3) 0.017(3) 0.000(2) N1 0.038(2) 0.036(2) 0.054(3) 0.008(2) 0.018(2) 0.006(2) C8 0.043(3) 0.033(3) 0.049(3) 0.004(2) 0.006(2) 0.006(2) C9 0.041(3) 0.044(3) 0.076(4) 0.007(3) 0.011(3) 0.008(3) C10 0.047(4) 0.042(4) 0.083(5) 0.005(3) -0.010(3) -0.001(3) C11 0.066(4) 0.041(3) 0.060(4) -0.002(3) -0.013(3) 0.006(3) C12 0.054(4) 0.045(3) 0.047(3) 0.000(3) 0.001(3) 0.010(3) C13 0.042(3) 0.039(3) 0.046(3) 0.003(2) 0.004(2) 0.010(2) N2 0.038(2) 0.037(2) 0.044(2) -0.0003(19) 0.0114(19) 0.005(2) S1 0.0434(8) 0.0446(8) 0.0448(8) 0.0027(6) 0.0100(6) 0.0139(6) O2 0.043(2) 0.063(3) 0.047(2) 0.0000(19) 0.0071(17) 0.0081(19) O3 0.063(2) 0.047(2) 0.060(2) 0.0095(19) 0.016(2) 0.026(2) C14 0.050(3) 0.032(3) 0.047(3) 0.001(2) 0.010(3) 0.012(2) C15 0.049(3) 0.049(3) 0.053(3) 0.002(3) 0.015(3) 0.018(3) C16 0.062(4) 0.064(4) 0.056(4) 0.013(3) 0.001(3) 0.029(3) C17 0.076(4) 0.053(4) 0.048(3) 0.009(3) 0.007(3) 0.022(3) C18 0.064(4) 0.038(3) 0.044(3) 0.001(2) 0.012(3) 0.016(3) C19 0.080(4) 0.048(4) 0.047(3) 0.001(3) 0.023(3) 0.013(3) C20 0.072(4) 0.064(4) 0.065(4) 0.005(3) 0.033(3) 0.019(4) C21 0.059(4) 0.072(4) 0.069(4) 0.009(3) 0.023(3) 0.029(3) C22 0.057(4) 0.053(4) 0.053(3) 0.009(3) 0.015(3) 0.022(3) C23 0.050(3) 0.034(3) 0.048(3) 0.000(2) 0.011(3) 0.012(2) N3 0.104(4) 0.076(4) 0.053(3) 0.019(3) 0.033(3) 0.029(3) C24 0.153(8) 0.073(6) 0.098(6) 0.032(5) 0.043(6) 0.031(5) C25 0.165(9) 0.138(8) 0.054(4) 0.021(5) 0.041(5) 0.057(7) O4 0.066(3) 0.049(2) 0.056(2) 0.0124(19) -0.002(2) 0.010(2) S2 0.0528(10) 0.0444(10) 0.0600(11) 0.0111(8) 0.0019(8) 0.0136(8) C26 0.121(13) 0.087(10) 0.063(9) 0.026(8) 0.024(7) 0.038(9) C27 0.108(10) 0.110(7) 0.081(6) 0.026(5) 0.024(8) 0.078(9) S2B 0.0528(10) 0.0444(10) 0.0600(11) 0.0111(8) 0.0019(8) 0.0136(8) C26B 0.121(13) 0.087(10) 0.063(9) 0.026(8) 0.024(7) 0.038(9) C27B 0.108(10) 0.110(7) 0.081(6) 0.026(5) 0.024(8) 0.078(9) O5 0.066(3) 0.106(4) 0.065(3) 0.024(2) 0.017(2) 0.052(3) S3 0.0557(11) 0.0594(12) 0.0643(11) 0.0130(9) 0.0094(9) 0.0127(9) C28 0.053(7) 0.104(11) 0.079(5) 0.007(7) 0.022(6) 0.032(6) C29 0.054(8) 0.163(9) 0.096(7) -0.038(6) -0.015(8) 0.019(10) S3B 0.0557(11) 0.0594(12) 0.0643(11) 0.0130(9) 0.0094(9) 0.0127(9) C28B 0.053(7) 0.104(11) 0.079(5) 0.007(7) 0.022(6) 0.032(6) C29B 0.054(8) 0.163(9) 0.096(7) -0.038(6) -0.015(8) 0.019(10) O6 0.109(5) 0.163(6) 0.101(4) 0.030(4) 0.027(4) 0.060(4) C30 0.087(6) 0.068(5) 0.071(5) 0.001(4) 0.009(4) 0.026(4) C31 0.097(6) 0.102(7) 0.117(7) -0.002(5) 0.021(5) 0.027(5) C32 0.145(8) 0.082(6) 0.095(6) 0.014(5) -0.015(6) 0.009(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.215(3) 2_777 ? Cd1 N2 2.271(4) . ? Cd1 O1 2.310(3) . ? Cd1 N1 2.322(4) . ? Cd1 O4 2.350(4) . ? Cd1 O5 2.371(4) . ? O1 C1 1.330(5) . ? O1 Cd1 2.215(3) 2_777 ? C1 C2 1.401(7) . ? C1 C6 1.424(7) . ? C2 C3 1.372(7) . ? C2 H2 0.93 . ? C3 C4 1.382(8) . ? C3 H3 0.93 . ? C4 C5 1.352(8) . ? C4 H4 0.93 . ? C5 C6 1.408(7) . ? C5 H5 0.93 . ? C6 C7 1.436(7) . ? C7 N1 1.284(6) . ? C7 H7 0.93 . ? N1 C8 1.413(6) . ? C8 C9 1.390(7) . ? C8 C13 1.411(7) . ? C9 C10 1.369(8) . ? C9 H9 0.93 . ? C10 C11 1.371(8) . ? C10 H10 0.93 . ? C11 C12 1.386(7) . ? C11 H11 0.93 . ? C12 C13 1.385(7) . ? C12 H12 0.93 . ? C13 N2 1.416(6) . ? N2 S1 1.574(4) . ? S1 O2 1.429(4) . ? S1 O3 1.445(4) . ? S1 C14 1.791(5) . ? C14 C15 1.364(7) . ? C14 C23 1.436(7) . ? C15 C16 1.399(7) . ? C15 H15 0.93 . ? C16 C17 1.359(8) . ? C16 H16 0.93 . ? C17 C18 1.406(8) . ? C17 H17 0.93 . ? C18 C23 1.428(7) . ? C18 C19 1.439(7) . ? C19 C20 1.363(8) . ? C19 N3 1.423(7) . ? C20 C21 1.405(8) . ? C20 H20 0.93 . ? C21 C22 1.360(7) . ? C21 H21 0.93 . ? C22 C23 1.410(7) . ? C22 H22 0.93 . ? N3 C24 1.454(8) . ? N3 C25 1.455(8) . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? C25 H25A 0.96 . ? C25 H25B 0.96 . ? C25 H25C 0.96 . ? O4 S2 1.508(4) . ? O4 S2B 1.511(11) . ? S2 C27 1.782(9) . ? S2 C26 1.784(13) . ? C26 H26A 0.96 . ? C26 H26B 0.96 . ? C26 H26C 0.96 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? S2B C26B 1.65(15) . ? S2B C27B 1.70(10) . ? C26B H26D 0.96 . ? C26B H26E 0.96 . ? C26B H26F 0.96 . ? C27B H27D 0.96 . ? C27B H27E 0.96 . ? C27B H27F 0.96 . ? O5 S3 1.473(4) . ? O5 S3B 1.623(12) . ? S3 C29 1.699(14) . ? S3 C28 1.766(11) . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? S3B C28B 1.74(10) . ? S3B C29B 1.77(12) . ? C28B H28D 0.96 . ? C28B H28E 0.96 . ? C28B H28F 0.96 . ? C29B H29D 0.96 . ? C29B H29E 0.96 . ? C29B H29F 0.96 . ? O6 C30 1.144(8) . ? C30 C31 1.512(10) . ? C30 C32 1.512(9) . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N2 130.94(13) 2_777 . ? O1 Cd1 O1 78.97(12) 2_777 . ? N2 Cd1 O1 150.04(13) . . ? O1 Cd1 N1 156.41(13) 2_777 . ? N2 Cd1 N1 71.83(14) . . ? O1 Cd1 N1 78.75(13) . . ? O1 Cd1 O4 95.62(13) 2_777 . ? N2 Cd1 O4 90.05(14) . . ? O1 Cd1 O4 84.23(13) . . ? N1 Cd1 O4 89.78(14) . . ? O1 Cd1 O5 89.68(15) 2_777 . ? N2 Cd1 O5 87.35(15) . . ? O1 Cd1 O5 95.67(13) . . ? N1 Cd1 O5 84.88(15) . . ? O4 Cd1 O5 174.57(15) . . ? C1 O1 Cd1 124.5(3) . 2_777 ? C1 O1 Cd1 123.8(3) . . ? Cd1 O1 Cd1 101.03(12) 2_777 . ? O1 C1 C2 120.5(5) . . ? O1 C1 C6 122.8(5) . . ? C2 C1 C6 116.8(5) . . ? C3 C2 C1 122.6(6) . . ? C3 C2 H2 118.7 . . ? C1 C2 H2 118.7 . . ? C2 C3 C4 120.7(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? C4 C5 C6 123.5(6) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C5 C6 C1 118.2(5) . . ? C5 C6 C7 116.2(5) . . ? C1 C6 C7 125.5(5) . . ? N1 C7 C6 128.6(5) . . ? N1 C7 H7 115.7 . . ? C6 C7 H7 115.7 . . ? C7 N1 C8 119.5(4) . . ? C7 N1 Cd1 124.3(4) . . ? C8 N1 Cd1 113.5(3) . . ? C9 C8 C13 119.1(5) . . ? C9 C8 N1 123.1(5) . . ? C13 C8 N1 117.6(4) . . ? C10 C9 C8 121.5(6) . . ? C10 C9 H9 119.2 . . ? C8 C9 H9 119.2 . . ? C9 C10 C11 119.5(6) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 120.3(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C13 C12 C11 121.2(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 118.2(5) . . ? C12 C13 N2 125.4(5) . . ? C8 C13 N2 116.4(4) . . ? C13 N2 S1 123.8(3) . . ? C13 N2 Cd1 115.8(3) . . ? S1 N2 Cd1 120.2(2) . . ? O2 S1 O3 116.5(2) . . ? O2 S1 N2 106.7(2) . . ? O3 S1 N2 112.9(2) . . ? O2 S1 C14 106.2(2) . . ? O3 S1 C14 106.4(2) . . ? N2 S1 C14 107.7(2) . . ? C15 C14 C23 120.8(5) . . ? C15 C14 S1 119.4(4) . . ? C23 C14 S1 119.8(4) . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C17 C16 C15 120.4(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C18 121.6(5) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C17 C18 C23 118.8(5) . . ? C17 C18 C19 122.2(5) . . ? C23 C18 C19 118.9(5) . . ? C20 C19 N3 122.9(5) . . ? C20 C19 C18 119.4(5) . . ? N3 C19 C18 117.7(6) . . ? C19 C20 C21 121.0(5) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C22 C21 C20 121.0(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120.6(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C22 C23 C18 119.0(5) . . ? C22 C23 C14 123.2(5) . . ? C18 C23 C14 117.8(5) . . ? C19 N3 C24 115.9(5) . . ? C19 N3 C25 115.9(5) . . ? C24 N3 C25 110.4(6) . . ? N3 C24 H24A 109.5 . . ? N3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S2 O4 S2B 46.1(5) . . ? S2 O4 Cd1 119.3(2) . . ? S2B O4 Cd1 162.8(5) . . ? O4 S2 C27 105.9(5) . . ? O4 S2 C26 103.8(6) . . ? C27 S2 C26 98.1(7) . . ? O4 S2B C26B 105(5) . . ? O4 S2B C27B 101(3) . . ? C26B S2B C27B 90(6) . . ? S2B C26B H26D 109.5 . . ? S2B C26B H26E 109.5 . . ? H26D C26B H26E 109.5 . . ? S2B C26B H26F 109.5 . . ? H26D C26B H26F 109.5 . . ? H26E C26B H26F 109.5 . . ? S2B C27B H27D 109.5 . . ? S2B C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? S2B C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? S3 O5 S3B 54.0(4) . . ? S3 O5 Cd1 142.7(3) . . ? S3B O5 Cd1 119.4(5) . . ? O5 S3 C29 104.3(7) . . ? O5 S3 C28 106.5(5) . . ? C29 S3 C28 100.1(7) . . ? O5 S3B C28B 111(3) . . ? O5 S3B C29B 120(5) . . ? C28B S3B C29B 97(6) . . ? S3B C28B H28D 109.5 . . ? S3B C28B H28E 109.5 . . ? H28D C28B H28E 109.5 . . ? S3B C28B H28F 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? S3B C29B H29D 109.5 . . ? S3B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? S3B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? O6 C30 C31 121.8(7) . . ? O6 C30 C32 122.6(8) . . ? C31 C30 C32 115.0(7) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cd1 O1 C1 -145.5(4) 2_777 . . . ? N2 Cd1 O1 C1 31.4(5) . . . . ? N1 Cd1 O1 C1 42.3(4) . . . . ? O4 Cd1 O1 C1 -48.6(4) . . . . ? O5 Cd1 O1 C1 125.9(4) . . . . ? O1 Cd1 O1 Cd1 0 2_777 . . 2_777 ? N2 Cd1 O1 Cd1 176.9(2) . . . 2_777 ? N1 Cd1 O1 Cd1 -172.18(16) . . . 2_777 ? O4 Cd1 O1 Cd1 96.89(14) . . . 2_777 ? O5 Cd1 O1 Cd1 -88.57(15) . . . 2_777 ? Cd1 O1 C1 C2 4.8(6) 2_777 . . . ? Cd1 O1 C1 C2 142.4(4) . . . . ? Cd1 O1 C1 C6 -176.5(3) 2_777 . . . ? Cd1 O1 C1 C6 -38.9(6) . . . . ? O1 C1 C2 C3 178.3(5) . . . . ? C6 C1 C2 C3 -0.5(8) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C2 C3 C4 C5 1.7(10) . . . . ? C3 C4 C5 C6 -0.4(10) . . . . ? C4 C5 C6 C1 -1.3(9) . . . . ? C4 C5 C6 C7 175.4(6) . . . . ? O1 C1 C6 C5 -177.1(5) . . . . ? C2 C1 C6 C5 1.7(7) . . . . ? O1 C1 C6 C7 6.6(8) . . . . ? C2 C1 C6 C7 -174.7(5) . . . . ? C5 C6 C7 N1 -171.4(5) . . . . ? C1 C6 C7 N1 5.1(9) . . . . ? C6 C7 N1 C8 177.5(5) . . . . ? C6 C7 N1 Cd1 17.5(8) . . . . ? O1 Cd1 N1 C7 -51.0(6) 2_777 . . . ? N2 Cd1 N1 C7 142.8(4) . . . . ? O1 Cd1 N1 C7 -31.5(4) . . . . ? O4 Cd1 N1 C7 52.7(4) . . . . ? O5 Cd1 N1 C7 -128.3(4) . . . . ? O1 Cd1 N1 C8 147.9(3) 2_777 . . . ? N2 Cd1 N1 C8 -18.4(3) . . . . ? O1 Cd1 N1 C8 167.4(3) . . . . ? O4 Cd1 N1 C8 -108.5(3) . . . . ? O5 Cd1 N1 C8 70.5(3) . . . . ? C7 N1 C8 C9 39.1(7) . . . . ? Cd1 N1 C8 C9 -158.8(4) . . . . ? C7 N1 C8 C13 -145.1(5) . . . . ? Cd1 N1 C8 C13 17.0(6) . . . . ? C13 C8 C9 C10 4.2(8) . . . . ? N1 C8 C9 C10 179.9(5) . . . . ? C8 C9 C10 C11 -1.8(9) . . . . ? C9 C10 C11 C12 -1.2(9) . . . . ? C10 C11 C12 C13 1.9(8) . . . . ? C11 C12 C13 C8 0.5(8) . . . . ? C11 C12 C13 N2 -177.8(5) . . . . ? C9 C8 C13 C12 -3.5(7) . . . . ? N1 C8 C13 C12 -179.4(5) . . . . ? C9 C8 C13 N2 175.0(5) . . . . ? N1 C8 C13 N2 -1.0(7) . . . . ? C12 C13 N2 S1 -12.3(7) . . . . ? C8 C13 N2 S1 169.4(4) . . . . ? C12 C13 N2 Cd1 162.1(4) . . . . ? C8 C13 N2 Cd1 -16.2(6) . . . . ? O1 Cd1 N2 C13 -154.4(3) 2_777 . . . ? O1 Cd1 N2 C13 29.6(5) . . . . ? N1 Cd1 N2 C13 18.3(3) . . . . ? O4 Cd1 N2 C13 108.1(3) . . . . ? O5 Cd1 N2 C13 -67.2(3) . . . . ? O1 Cd1 N2 S1 20.2(3) 2_777 . . . ? O1 Cd1 N2 S1 -155.8(2) . . . . ? N1 Cd1 N2 S1 -167.1(3) . . . . ? O4 Cd1 N2 S1 -77.3(3) . . . . ? O5 Cd1 N2 S1 107.5(3) . . . . ? C13 N2 S1 O2 -170.0(4) . . . . ? Cd1 N2 S1 O2 15.8(3) . . . . ? C13 N2 S1 O3 -40.8(5) . . . . ? Cd1 N2 S1 O3 145.0(2) . . . . ? C13 N2 S1 C14 76.3(4) . . . . ? Cd1 N2 S1 C14 -97.9(3) . . . . ? O2 S1 C14 C15 -115.0(4) . . . . ? O3 S1 C14 C15 120.3(4) . . . . ? N2 S1 C14 C15 -1.0(5) . . . . ? O2 S1 C14 C23 63.3(5) . . . . ? O3 S1 C14 C23 -61.4(5) . . . . ? N2 S1 C14 C23 177.3(4) . . . . ? C23 C14 C15 C16 1.9(8) . . . . ? S1 C14 C15 C16 -179.8(4) . . . . ? C14 C15 C16 C17 -3.5(9) . . . . ? C15 C16 C17 C18 0.3(9) . . . . ? C16 C17 C18 C23 4.3(9) . . . . ? C16 C17 C18 C19 -178.9(6) . . . . ? C17 C18 C19 C20 -173.6(6) . . . . ? C23 C18 C19 C20 3.1(8) . . . . ? C17 C18 C19 N3 4.2(9) . . . . ? C23 C18 C19 N3 -179.1(5) . . . . ? N3 C19 C20 C21 -178.5(6) . . . . ? C18 C19 C20 C21 -0.8(9) . . . . ? C19 C20 C21 C22 -1.6(10) . . . . ? C20 C21 C22 C23 1.6(9) . . . . ? C21 C22 C23 C18 0.7(8) . . . . ? C21 C22 C23 C14 -179.8(5) . . . . ? C17 C18 C23 C22 173.8(5) . . . . ? C19 C18 C23 C22 -3.1(8) . . . . ? C17 C18 C23 C14 -5.7(8) . . . . ? C19 C18 C23 C14 177.5(5) . . . . ? C15 C14 C23 C22 -176.8(5) . . . . ? S1 C14 C23 C22 5.0(7) . . . . ? C15 C14 C23 C18 2.7(8) . . . . ? S1 C14 C23 C18 -175.6(4) . . . . ? C20 C19 N3 C24 -113.2(7) . . . . ? C18 C19 N3 C24 69.0(8) . . . . ? C20 C19 N3 C25 18.7(9) . . . . ? C18 C19 N3 C25 -159.1(6) . . . . ? O1 Cd1 O4 S2 -172.9(2) 2_777 . . . ? N2 Cd1 O4 S2 -41.8(3) . . . . ? O1 Cd1 O4 S2 108.8(3) . . . . ? N1 Cd1 O4 S2 30.1(3) . . . . ? O1 Cd1 O4 S2B -143.8(17) 2_777 . . . ? N2 Cd1 O4 S2B -12.6(17) . . . . ? O1 Cd1 O4 S2B 137.9(17) . . . . ? N1 Cd1 O4 S2B 59.2(17) . . . . ? S2B O4 S2 C27 -50.6(7) . . . . ? Cd1 O4 S2 C27 117.8(4) . . . . ? S2B O4 S2 C26 52.1(9) . . . . ? Cd1 O4 S2 C26 -139.4(7) . . . . ? S2 O4 S2B C26B -48(5) . . . . ? Cd1 O4 S2B C26B -84(5) . . . . ? S2 O4 S2B C27B 44(3) . . . . ? Cd1 O4 S2B C27B 8(4) . . . . ? O1 Cd1 O5 S3 -76.0(5) 2_777 . . . ? N2 Cd1 O5 S3 153.0(5) . . . . ? O1 Cd1 O5 S3 2.9(5) . . . . ? N1 Cd1 O5 S3 81.1(5) . . . . ? O1 Cd1 O5 S3B -144.1(6) 2_777 . . . ? N2 Cd1 O5 S3B 84.9(6) . . . . ? O1 Cd1 O5 S3B -65.2(6) . . . . ? N1 Cd1 O5 S3B 12.9(6) . . . . ? S3B O5 S3 C29 -43.2(9) . . . . ? Cd1 O5 S3 C29 -136.0(8) . . . . ? S3B O5 S3 C28 62.1(7) . . . . ? Cd1 O5 S3 C28 -30.7(6) . . . . ? S3 O5 S3B C28B -62(4) . . . . ? Cd1 O5 S3B C28B 74(4) . . . . ? S3 O5 S3B C29B 49(6) . . . . ? Cd1 O5 S3B C29B -175(6) . . . . ? # END of CIF