# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_AW1001_revised_p21n _database_code_depnum_ccdc_archive 'CCDC 848195' #TrackingRef 'web_deposit_cif_file_0_CarstenStreb_1360754958.AW1001_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C26 H28 N2 O6 S2' _chemical_formula_sum 'C26 H28 N2 O6 S2' _chemical_melting_point ? _exptl_crystal_description block _exptl_crystal_colour colourless _diffrn_ambient_temperature 150(2) _chemical_formula_weight 528.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? 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 8.2852(8) _cell_length_b 11.1495(18) _cell_length_c 27.839(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.240(11) _cell_angle_gamma 90.00 _cell_volume 2560.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 287 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 23.1 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.946 _exptl_absorpt_correction_T_max 0.971 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa Nonius CCD' _diffrn_measurement_method 'Omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41449 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5223 _reflns_number_gt 3919 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Kappa-Nonius SUPERGUI' _computing_cell_refinement 'Kappa-Nonius SUPERGUI' _computing_data_reduction 'Kappa-Nonius SUPERGUI' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-3 _computing_publication_material WINGX _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^)+(0.0697P)^2^+4.0086P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 5223 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1453 _refine_ls_wR_factor_gt 0.1316 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.31023(9) 0.04245(7) 0.18469(3) 0.02226(19) Uani 1 1 d . . . S2 S 0.79632(9) 0.32959(7) 0.22601(3) 0.02225(19) Uani 1 1 d . . . O6 O 0.0919(2) 0.68183(18) 0.01020(8) 0.0247(5) Uani 1 1 d . . . O3 O 0.1404(2) 0.89755(17) -0.02834(7) 0.0222(5) Uani 1 1 d . . . N1 N 0.3652(3) 0.6602(2) 0.02901(8) 0.0158(5) Uani 1 1 d . . . H1 H 0.4574 0.6939 0.0263 0.019 Uiso 1 1 calc R . . O2 O 0.2920(2) 0.28695(18) -0.05258(7) 0.0208(4) Uani 1 1 d . . . N2 N 0.2046(3) 0.4604(2) -0.01872(8) 0.0155(5) Uani 1 1 d . . . H2 H 0.1479 0.5241 -0.0248 0.019 Uiso 1 1 calc R . . O5 O 0.0233(3) 0.50680(19) -0.10219(7) 0.0263(5) Uani 1 1 d . . . O1 O 0.1296(2) 0.34461(19) -0.13643(7) 0.0241(5) Uani 1 1 d . . . O4 O 0.4022(3) 0.89058(19) 0.00245(8) 0.0301(5) Uani 1 1 d . . . C26 C 0.2122(3) 0.3790(2) -0.05423(10) 0.0159(6) Uani 1 1 d . . . C5 C 0.2850(3) 0.4467(2) 0.02810(9) 0.0159(6) Uani 1 1 d . . . C2 C 0.4619(3) 0.4170(3) 0.11831(10) 0.0170(6) Uani 1 1 d . . . C3 C 0.4532(3) 0.5284(3) 0.09569(10) 0.0173(6) Uani 1 1 d . . . H3 H 0.5073 0.5933 0.1107 0.021 Uiso 1 1 calc R . . C7 C 0.3609(3) 0.2021(3) 0.12200(10) 0.0170(6) Uani 1 1 d . . . C25 C 0.1081(3) 0.4193(3) -0.10034(10) 0.0190(6) Uani 1 1 d . . . C1 C 0.3710(3) 0.3204(2) 0.09687(10) 0.0172(6) Uani 1 1 d . . . C4 C 0.3650(3) 0.5451(2) 0.05095(10) 0.0159(6) Uani 1 1 d . . . C19 C 0.2307(3) 0.7200(2) 0.01215(9) 0.0166(6) Uani 1 1 d . . . C13 C 0.7012(3) 0.3263(3) 0.16778(10) 0.0185(6) Uani 1 1 d . . . C14 C 0.5709(3) 0.4022(2) 0.16381(9) 0.0175(6) Uani 1 1 d . . . C6 C 0.2860(3) 0.3365(3) 0.05192(10) 0.0180(6) Uani 1 1 d . . . H6 H 0.2285 0.2724 0.0374 0.022 Uiso 1 1 calc R . . C8 C 0.2973(3) 0.1907(3) 0.16536(10) 0.0194(6) Uani 1 1 d . . . C12 C 0.2195(4) 0.2841(3) 0.19396(11) 0.0272(7) Uani 1 1 d . . . H12A H 0.1865 0.2489 0.2230 0.041 Uiso 1 1 calc R . . H12B H 0.1264 0.3161 0.1752 0.041 Uiso 1 1 calc R . . H12C H 0.2956 0.3475 0.2021 0.041 Uiso 1 1 calc R . . C20 C 0.2694(3) 0.8467(2) -0.00524(9) 0.0164(6) Uani 1 1 d . . . C15 C 0.5515(3) 0.4652(3) 0.20777(10) 0.0217(6) Uani 1 1 d . . . H15 H 0.4700 0.5214 0.2107 0.026 Uiso 1 1 calc R . . C21 C 0.1610(4) 1.0202(3) -0.04559(12) 0.0280(7) Uani 1 1 d . . . H21A H 0.2606 1.0267 -0.0612 0.034 Uiso 1 1 calc R . . H21B H 0.1660 1.0761 -0.0188 0.034 Uiso 1 1 calc R . . C10 C 0.3993(3) -0.0047(3) 0.13410(10) 0.0206(6) Uani 1 1 d . . . C16 C 0.6626(4) 0.4358(3) 0.24470(10) 0.0227(6) Uani 1 1 d . . . C9 C 0.4159(3) 0.0900(3) 0.10429(10) 0.0191(6) Uani 1 1 d . . . H9 H 0.4594 0.0827 0.0748 0.023 Uiso 1 1 calc R . . C18 C 0.7685(4) 0.2523(3) 0.12928(10) 0.0235(6) Uani 1 1 d . . . H18A H 0.8610 0.2082 0.1430 0.035 Uiso 1 1 calc R . . H18B H 0.8005 0.3041 0.1043 0.035 Uiso 1 1 calc R . . H18C H 0.6871 0.1974 0.1159 0.035 Uiso 1 1 calc R . . C24 C 0.0363(4) 0.3734(3) -0.18233(10) 0.0275(7) Uani 1 1 d . . . H24A H 0.0877 0.3371 -0.2087 0.033 Uiso 1 1 calc R . . H24B H 0.0347 0.4596 -0.1871 0.033 Uiso 1 1 calc R . . C11 C 0.4438(4) -0.1338(3) 0.12802(12) 0.0292(7) Uani 1 1 d . . . H11A H 0.4172 -0.1787 0.1556 0.044 Uiso 1 1 calc R . . H11B H 0.5580 -0.1400 0.1250 0.044 Uiso 1 1 calc R . . H11C H 0.3848 -0.1653 0.0995 0.044 Uiso 1 1 calc R . . C22 C 0.0184(4) 1.0478(3) -0.08069(11) 0.0297(7) Uani 1 1 d . . . H22A H 0.0282 1.1279 -0.0927 0.045 Uiso 1 1 calc R . . H22B H -0.0793 1.0412 -0.0648 0.045 Uiso 1 1 calc R . . H22C H 0.0149 0.9920 -0.1070 0.045 Uiso 1 1 calc R . . C23 C -0.1342(4) 0.3277(4) -0.18243(12) 0.0398(9) Uani 1 1 d . . . H23A H -0.1937 0.3470 -0.2126 0.060 Uiso 1 1 calc R . . H23B H -0.1854 0.3646 -0.1566 0.060 Uiso 1 1 calc R . . H23C H -0.1325 0.2423 -0.1781 0.060 Uiso 1 1 calc R . . C17 C 0.6792(4) 0.4808(3) 0.29567(11) 0.0342(8) Uani 1 1 d . . . H17A H 0.7704 0.4428 0.3132 0.051 Uiso 1 1 calc R . . H17B H 0.5825 0.4622 0.3107 0.051 Uiso 1 1 calc R . . H17C H 0.6952 0.5660 0.2957 0.051 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 S1 0.0271(4) 0.0206(4) 0.0194(4) 0.0053(3) 0.0040(3) -0.0012(3) S2 0.0198(4) 0.0290(4) 0.0174(3) 0.0008(3) -0.0015(3) 0.0036(3) O6 0.0140(10) 0.0185(11) 0.0418(13) 0.0058(9) 0.0029(9) -0.0012(8) O3 0.0194(10) 0.0172(11) 0.0295(11) 0.0056(9) 0.0002(9) -0.0001(8) N1 0.0151(11) 0.0126(11) 0.0196(11) 0.0025(9) 0.0004(9) -0.0031(9) O2 0.0187(10) 0.0197(11) 0.0234(10) 0.0003(8) -0.0010(8) 0.0015(8) N2 0.0146(11) 0.0137(11) 0.0177(11) 0.0030(9) -0.0010(9) 0.0009(9) O5 0.0289(11) 0.0253(12) 0.0237(11) 0.0031(9) -0.0034(9) 0.0061(10) O1 0.0267(11) 0.0280(12) 0.0170(10) -0.0018(9) -0.0014(8) 0.0032(9) O4 0.0222(11) 0.0239(12) 0.0429(13) 0.0109(10) -0.0051(10) -0.0079(9) C26 0.0125(13) 0.0161(14) 0.0189(13) 0.0042(11) 0.0006(10) -0.0053(11) C5 0.0130(13) 0.0183(14) 0.0162(13) 0.0015(11) 0.0001(10) 0.0003(11) C2 0.0152(13) 0.0207(14) 0.0151(13) -0.0001(11) 0.0017(10) 0.0015(11) C3 0.0151(13) 0.0172(14) 0.0195(14) -0.0034(11) 0.0010(11) -0.0012(11) C7 0.0151(13) 0.0181(14) 0.0172(13) 0.0025(11) -0.0022(11) -0.0011(11) C25 0.0162(14) 0.0204(15) 0.0202(14) 0.0020(11) 0.0001(11) -0.0032(12) C1 0.0169(13) 0.0162(14) 0.0187(13) 0.0019(11) 0.0028(11) 0.0000(11) C4 0.0151(13) 0.0133(13) 0.0197(13) 0.0012(11) 0.0036(11) 0.0017(11) C19 0.0161(14) 0.0173(14) 0.0162(13) -0.0014(11) 0.0015(11) -0.0009(11) C13 0.0188(14) 0.0189(14) 0.0174(13) 0.0010(11) -0.0002(11) -0.0032(11) C14 0.0203(14) 0.0156(14) 0.0164(13) 0.0001(11) 0.0018(11) -0.0031(11) C6 0.0162(13) 0.0179(14) 0.0196(14) -0.0008(11) 0.0011(11) -0.0027(11) C8 0.0188(14) 0.0197(15) 0.0193(14) 0.0030(11) 0.0000(11) -0.0008(12) C12 0.0290(17) 0.0267(17) 0.0271(16) 0.0029(13) 0.0086(13) 0.0039(13) C20 0.0167(14) 0.0167(14) 0.0160(13) -0.0006(11) 0.0027(11) 0.0002(11) C15 0.0181(14) 0.0241(16) 0.0226(15) -0.0039(12) 0.0005(11) 0.0017(12) C21 0.0301(17) 0.0167(16) 0.0369(18) 0.0101(13) 0.0011(14) -0.0009(13) C10 0.0214(14) 0.0182(14) 0.0215(14) 0.0010(12) -0.0006(11) -0.0017(12) C16 0.0222(15) 0.0275(17) 0.0184(14) -0.0036(12) 0.0018(12) -0.0003(13) C9 0.0211(14) 0.0183(14) 0.0180(14) -0.0005(11) 0.0022(11) -0.0047(12) C18 0.0230(15) 0.0265(16) 0.0211(14) -0.0012(12) 0.0025(12) 0.0007(13) C24 0.0351(18) 0.0332(18) 0.0137(14) 0.0006(13) -0.0007(12) -0.0010(15) C11 0.0376(18) 0.0193(16) 0.0313(17) 0.0024(13) 0.0068(14) -0.0005(14) C22 0.0358(18) 0.0270(17) 0.0263(16) 0.0062(13) 0.0036(14) 0.0041(15) C23 0.038(2) 0.053(2) 0.0272(17) 0.0004(16) -0.0071(15) -0.0059(18) C17 0.0328(18) 0.047(2) 0.0221(16) -0.0100(15) -0.0018(14) 0.0031(16) _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 S1 C10 1.730(3) . ? S1 C8 1.739(3) . ? S2 C16 1.734(3) . ? S2 C13 1.737(3) . ? O6 C19 1.223(3) . ? O3 C20 1.323(3) . ? O3 C21 1.464(3) . ? N1 C19 1.346(3) . ? N1 C4 1.421(3) . ? N1 H1 0.8600 . ? O2 C26 1.219(3) . ? N2 C26 1.348(4) . ? N2 C5 1.417(3) . ? N2 H2 0.8600 . ? O5 C25 1.201(4) . ? O1 C25 1.330(3) . ? O1 C24 1.467(3) . ? O4 C20 1.205(3) . ? C26 C25 1.547(4) . ? C5 C6 1.396(4) . ? C5 C4 1.404(4) . ? C2 C3 1.392(4) . ? C2 C1 1.415(4) . ? C2 C14 1.496(4) . ? C3 C4 1.398(4) . ? C3 H3 0.9300 . ? C7 C8 1.366(4) . ? C7 C9 1.434(4) . ? C7 C1 1.499(4) . ? C1 C6 1.390(4) . ? C19 C20 1.537(4) . ? C13 C14 1.368(4) . ? C13 C18 1.499(4) . ? C14 C15 1.433(4) . ? C6 H6 0.9300 . ? C8 C12 1.492(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C15 C16 1.356(4) . ? C15 H15 0.9300 . ? C21 C22 1.494(4) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C10 C9 1.357(4) . ? C10 C11 1.499(4) . ? C16 C17 1.499(4) . ? C9 H9 0.9300 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C24 C23 1.501(5) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 S1 C8 93.20(14) . . ? C16 S2 C13 92.68(14) . . ? C20 O3 C21 116.5(2) . . ? C19 N1 C4 124.3(2) . . ? C19 N1 H1 117.9 . . ? C4 N1 H1 117.9 . . ? C26 N2 C5 123.6(2) . . ? C26 N2 H2 118.2 . . ? C5 N2 H2 118.2 . . ? C25 O1 C24 115.1(2) . . ? O2 C26 N2 126.9(2) . . ? O2 C26 C25 122.4(2) . . ? N2 C26 C25 110.7(2) . . ? C6 C5 C4 119.4(2) . . ? C6 C5 N2 120.9(2) . . ? C4 C5 N2 119.7(2) . . ? C3 C2 C1 119.0(2) . . ? C3 C2 C14 119.0(2) . . ? C1 C2 C14 122.0(2) . . ? C2 C3 C4 121.6(3) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C8 C7 C9 112.5(3) . . ? C8 C7 C1 122.5(3) . . ? C9 C7 C1 125.0(2) . . ? O5 C25 O1 126.5(3) . . ? O5 C25 C26 123.5(3) . . ? O1 C25 C26 110.0(2) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 C7 119.2(2) . . ? C2 C1 C7 121.5(2) . . ? C3 C4 C5 119.1(2) . . ? C3 C4 N1 118.8(2) . . ? C5 C4 N1 122.0(2) . . ? O6 C19 N1 126.1(3) . . ? O6 C19 C20 121.9(2) . . ? N1 C19 C20 112.0(2) . . ? C14 C13 C18 128.7(3) . . ? C14 C13 S2 110.5(2) . . ? C18 C13 S2 120.8(2) . . ? C13 C14 C15 112.6(2) . . ? C13 C14 C2 123.2(2) . . ? C15 C14 C2 124.2(3) . . ? C1 C6 C5 121.4(3) . . ? C1 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C7 C8 C12 128.8(3) . . ? C7 C8 S1 110.1(2) . . ? C12 C8 S1 121.1(2) . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O4 C20 O3 126.6(3) . . ? O4 C20 C19 122.0(2) . . ? O3 C20 C19 111.4(2) . . ? C16 C15 C14 114.1(3) . . ? C16 C15 H15 123.0 . . ? C14 C15 H15 123.0 . . ? O3 C21 C22 107.3(2) . . ? O3 C21 H21A 110.2 . . ? C22 C21 H21A 110.2 . . ? O3 C21 H21B 110.2 . . ? C22 C21 H21B 110.2 . . ? H21A C21 H21B 108.5 . . ? C9 C10 C11 129.6(3) . . ? C9 C10 S1 109.6(2) . . ? C11 C10 S1 120.7(2) . . ? C15 C16 C17 129.4(3) . . ? C15 C16 S2 110.2(2) . . ? C17 C16 S2 120.4(2) . . ? C10 C9 C7 114.5(3) . . ? C10 C9 H9 122.8 . . ? C7 C9 H9 122.8 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C24 C23 110.4(2) . . ? O1 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? O1 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C24 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.596 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.073 data_MAK65_revised _database_code_depnum_ccdc_archive 'CCDC 848406' #TrackingRef 'web_deposit_cif_file_1_CarstenStreb_1360754958.MAK65_revised.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 N2 Ni O4 S2, 2(C16 H36 N), 1(H2O)' _chemical_formula_sum 'C64 H98 N4 Ni O5 S2' _chemical_formula_weight 1126.28 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 21.123(4) _cell_length_b 13.088(3) _cell_length_c 22.600(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.40(3) _cell_angle_gamma 90.00 _cell_volume 6181(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 412 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 23.1 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.913 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa Nonius CCD' _diffrn_measurement_method 'Omega and Phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 80283 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0442 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 5.84 _diffrn_reflns_theta_max 26.37 _reflns_number_total 12470 _reflns_number_gt 9281 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Kappa-Nonius SUPERGUI' _computing_cell_refinement 'Kappa-Nonius SUPERGUI' _computing_data_reduction 'Kappa-Nonius SUPERGUI' _computing_structure_solution SHELXS-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP-3 _computing_publication_material WINGX _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^)+(0.1104P)^2^+6.1718P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12470 _refine_ls_number_parameters 700 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0895 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2088 _refine_ls_wR_factor_gt 0.1895 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.48470(15) 0.1353(3) 0.76003(13) 0.0343(7) Uani 1 1 d . . . C2 C 0.43906(15) 0.2046(3) 0.73131(13) 0.0335(7) Uani 1 1 d . . . C3 C 0.38197(14) 0.1738(3) 0.68716(14) 0.0334(7) Uani 1 1 d . . . C4 C 0.33734(13) 0.0543(2) 0.61053(12) 0.0248(6) Uani 1 1 d . . . C5 C 0.34714(13) -0.0429(2) 0.58626(12) 0.0230(6) Uani 1 1 d . . . C6 C 0.42192(13) -0.1830(2) 0.59318(13) 0.0253(6) Uani 1 1 d . . . C7 C 0.46918(14) -0.2483(3) 0.63167(14) 0.0304(7) Uani 1 1 d . . . C8 C 0.49292(16) -0.2267(3) 0.69195(14) 0.0337(7) Uani 1 1 d . . . C9 C 0.53491(19) -0.3001(3) 0.72353(17) 0.0467(9) Uani 1 1 d . . . H9 H 0.5510 -0.2876 0.7634 0.056 Uiso 1 1 calc R . . C10 C 0.5525(2) -0.3875(3) 0.69769(19) 0.0546(11) Uani 1 1 d . . . H10 H 0.5791 -0.4344 0.7200 0.065 Uiso 1 1 calc R . . C11 C 0.5302(2) -0.4063(3) 0.6373(2) 0.0576(11) Uani 1 1 d . . . H11 H 0.5431 -0.4645 0.6188 0.069 Uiso 1 1 calc R . . C12 C 0.48901(17) -0.3379(3) 0.60582(16) 0.0407(8) Uani 1 1 d . . . H12 H 0.4737 -0.3515 0.5659 0.049 Uiso 1 1 calc R . . C13 C 0.30466(14) -0.0770(2) 0.53672(12) 0.0252(6) Uani 1 1 d . . . H13 H 0.3109 -0.1411 0.5208 0.030 Uiso 1 1 calc R . . C14 C 0.25325(13) -0.0175(2) 0.51052(12) 0.0255(6) Uani 1 1 d . . . C15 C 0.20898(14) -0.0597(3) 0.45859(14) 0.0297(7) Uani 1 1 d . . . C16 C 0.18998(15) -0.0119(3) 0.40535(14) 0.0335(7) Uani 1 1 d . . . C17 C 0.13516(19) -0.1813(3) 0.41313(17) 0.0484(9) Uani 1 1 d . . . C18 C 0.17837(17) -0.1572(3) 0.46178(15) 0.0401(8) Uani 1 1 d . . . H18 H 0.1874 -0.2005 0.4946 0.048 Uiso 1 1 calc R . . C19 C 0.0922(2) -0.2720(4) 0.4025(2) 0.0642(12) Uani 1 1 d . . . H19A H 0.0670 -0.2667 0.3636 0.096 Uiso 1 1 calc R . . H19B H 0.0644 -0.2744 0.4324 0.096 Uiso 1 1 calc R . . H19C H 0.1175 -0.3331 0.4044 0.096 Uiso 1 1 calc R . . C20 C 0.20957(18) 0.0867(3) 0.38273(16) 0.0417(8) Uani 1 1 d . . . H20A H 0.1870 0.0981 0.3432 0.063 Uiso 1 1 calc R . . H20B H 0.2548 0.0860 0.3814 0.063 Uiso 1 1 calc R . . H20C H 0.1997 0.1405 0.4088 0.063 Uiso 1 1 calc R . . C21 C 0.24296(14) 0.0791(3) 0.53516(13) 0.0279(6) Uani 1 1 d . . . C22 C 0.18684(15) 0.1428(3) 0.51288(13) 0.0329(7) Uani 1 1 d . . . C23 C 0.19049(18) 0.2444(3) 0.50046(15) 0.0417(8) Uani 1 1 d . . . C24 C 0.07745(18) 0.1776(4) 0.48297(16) 0.0492(10) Uani 1 1 d . . . C25 C 0.12186(16) 0.1054(3) 0.50254(14) 0.0395(8) Uani 1 1 d . . . H25 H 0.1113 0.0377 0.5087 0.047 Uiso 1 1 calc R . . C26 C 0.00611(19) 0.1650(4) 0.4680(2) 0.0650(13) Uani 1 1 d . . . H26A H -0.0130 0.2294 0.4553 0.098 Uiso 1 1 calc R . . H26B H -0.0109 0.1415 0.5027 0.098 Uiso 1 1 calc R . . H26C H -0.0033 0.1159 0.4364 0.098 Uiso 1 1 calc R . . C27 C 0.2473(2) 0.3101(3) 0.5003(2) 0.0539(10) Uani 1 1 d . . . H27A H 0.2339 0.3786 0.4897 0.081 Uiso 1 1 calc R . . H27B H 0.2728 0.2843 0.4718 0.081 Uiso 1 1 calc R . . H27C H 0.2722 0.3101 0.5395 0.081 Uiso 1 1 calc R . . C28 C 0.28525(14) 0.1133(3) 0.58413(13) 0.0291(6) Uani 1 1 d . . . H28 H 0.2788 0.1774 0.5999 0.035 Uiso 1 1 calc R . . C29 C 0.44690(16) 0.3096(3) 0.74288(15) 0.0394(8) Uani 1 1 d . . . H29 H 0.4167 0.3552 0.7241 0.047 Uiso 1 1 calc R . . C30 C 0.49868(17) 0.3466(3) 0.78164(16) 0.0445(9) Uani 1 1 d . . . H30 H 0.5040 0.4166 0.7877 0.053 Uiso 1 1 calc R . . C31 C 0.54264(17) 0.2780(3) 0.81145(15) 0.0445(9) Uani 1 1 d . . . H31 H 0.5768 0.3022 0.8385 0.053 Uiso 1 1 calc R . . C32 C 0.53601(17) 0.1749(3) 0.80123(15) 0.0414(8) Uani 1 1 d . . . H32 H 0.5657 0.1302 0.8217 0.050 Uiso 1 1 calc R . . C33 C 0.68571(15) 0.1858(3) 0.16777(15) 0.0324(7) Uani 1 1 d . . . H33A H 0.7252 0.2244 0.1762 0.039 Uiso 1 1 calc R . . H33B H 0.6743 0.1831 0.1246 0.039 Uiso 1 1 calc R . . C34 C 0.63395(17) 0.2443(3) 0.19302(18) 0.0412(8) Uani 1 1 d . . . H34A H 0.5942 0.2061 0.1869 0.049 Uiso 1 1 calc R . . H34B H 0.6462 0.2548 0.2356 0.049 Uiso 1 1 calc R . . C35 C 0.6252(2) 0.3463(3) 0.16121(19) 0.0509(10) Uani 1 1 d . . . H35A H 0.6656 0.3826 0.1676 0.061 Uiso 1 1 calc R . . H35B H 0.6145 0.3338 0.1186 0.061 Uiso 1 1 calc R . . C36 C 0.5748(2) 0.4136(3) 0.1805(2) 0.0635(12) Uani 1 1 d . . . H36A H 0.5726 0.4763 0.1582 0.095 Uiso 1 1 calc R . . H36B H 0.5853 0.4283 0.2224 0.095 Uiso 1 1 calc R . . H36C H 0.5342 0.3796 0.1732 0.095 Uiso 1 1 calc R . . C37 C 0.64004(15) 0.0096(3) 0.17352(14) 0.0322(7) Uani 1 1 d . . . H37A H 0.6036 0.0422 0.1873 0.039 Uiso 1 1 calc R . . H37B H 0.6473 -0.0549 0.1946 0.039 Uiso 1 1 calc R . . C38 C 0.62320(17) -0.0124(3) 0.10663(15) 0.0384(8) Uani 1 1 d . . . H38A H 0.6256 0.0505 0.0844 0.046 Uiso 1 1 calc R . . H38B H 0.6541 -0.0599 0.0945 0.046 Uiso 1 1 calc R . . C39 C 0.55610(18) -0.0577(3) 0.09164(17) 0.0426(8) Uani 1 1 d . . . H39A H 0.5512 -0.0865 0.0517 0.051 Uiso 1 1 calc R . . H39B H 0.5513 -0.1127 0.1194 0.051 Uiso 1 1 calc R . . C40 C 0.5039(2) 0.0203(3) 0.0946(2) 0.0540(10) Uani 1 1 d . . . H40A H 0.4628 -0.0119 0.0847 0.081 Uiso 1 1 calc R . . H40B H 0.5078 0.0744 0.0667 0.081 Uiso 1 1 calc R . . H40C H 0.5077 0.0479 0.1344 0.081 Uiso 1 1 calc R . . C41 C 0.75479(15) 0.0399(3) 0.16114(14) 0.0319(7) Uani 1 1 d . . . H41A H 0.7426 0.0423 0.1181 0.038 Uiso 1 1 calc R . . H41B H 0.7902 0.0869 0.1713 0.038 Uiso 1 1 calc R . . C42 C 0.77796(17) -0.0673(3) 0.17838(16) 0.0397(8) Uani 1 1 d . . . H42A H 0.7420 -0.1142 0.1727 0.048 Uiso 1 1 calc R . . H42B H 0.7962 -0.0686 0.2203 0.048 Uiso 1 1 calc R . . C43 C 0.82840(19) -0.1016(3) 0.14024(17) 0.0476(9) Uani 1 1 d . . . H43A H 0.8623 -0.0510 0.1436 0.057 Uiso 1 1 calc R . . H43B H 0.8471 -0.1654 0.1561 0.057 Uiso 1 1 calc R . . C44 C 0.8025(2) -0.1163(3) 0.07505(18) 0.0541(10) Uani 1 1 d . . . H44A H 0.8365 -0.1374 0.0538 0.081 Uiso 1 1 calc R . . H44B H 0.7847 -0.0531 0.0586 0.081 Uiso 1 1 calc R . . H44C H 0.7697 -0.1678 0.0712 0.081 Uiso 1 1 calc R . . C45 C 0.71515(15) 0.0762(3) 0.25838(13) 0.0312(7) Uani 1 1 d . . . H45A H 0.6796 0.1052 0.2754 0.037 Uiso 1 1 calc R . . H45B H 0.7201 0.0058 0.2717 0.037 Uiso 1 1 calc R . . C46 C 0.77550(17) 0.1345(3) 0.28237(15) 0.0406(8) Uani 1 1 d . . . H46A H 0.8117 0.1039 0.2671 0.049 Uiso 1 1 calc R . . H46B H 0.7715 0.2045 0.2682 0.049 Uiso 1 1 calc R . . C47 C 0.78787(17) 0.1342(3) 0.34954(15) 0.0399(8) Uani 1 1 d . . . H47A H 0.7893 0.0642 0.3638 0.048 Uiso 1 1 calc R . . H47B H 0.7529 0.1685 0.3648 0.048 Uiso 1 1 calc R . . C48 C 0.85048(18) 0.1873(4) 0.37339(17) 0.0483(10) Uani 1 1 d . . . H48A H 0.8568 0.1856 0.4163 0.072 Uiso 1 1 calc R . . H48B H 0.8489 0.2570 0.3600 0.072 Uiso 1 1 calc R . . H48C H 0.8853 0.1528 0.3589 0.072 Uiso 1 1 calc R . . C49 C 0.0482(2) 0.2596(4) 0.13062(17) 0.0578(12) Uani 1 1 d . D . H49A H 0.0509 0.2110 0.1633 0.069 Uiso 1 1 calc R . . H49B H 0.0202 0.3146 0.1394 0.069 Uiso 1 1 calc R . . C50 C 0.01781(19) 0.2067(3) 0.07344(17) 0.0481(10) Uani 1 1 d . . . H50A H 0.0437 0.1485 0.0654 0.058 Uiso 1 1 calc R . . H50B H 0.0160 0.2536 0.0400 0.058 Uiso 1 1 calc R . . C51 C -0.04993(19) 0.1710(4) 0.0799(2) 0.0554(11) Uani 1 1 d . . . H51A H -0.0486 0.1326 0.1168 0.067 Uiso 1 1 calc R . . H51B H -0.0771 0.2301 0.0823 0.067 Uiso 1 1 calc R . . C52 C -0.0783(2) 0.1049(3) 0.0280(2) 0.0536(10) Uani 1 1 d . . . H52A H -0.1205 0.0837 0.0336 0.080 Uiso 1 1 calc R . . H52B H -0.0518 0.0457 0.0259 0.080 Uiso 1 1 calc R . . H52C H -0.0805 0.1431 -0.0085 0.080 Uiso 1 1 calc R . . C53 C 0.15766(19) 0.2292(3) 0.10211(16) 0.0439(9) Uani 1 1 d . D . H53A H 0.1988 0.2617 0.1012 0.053 Uiso 1 1 calc R . . H53B H 0.1390 0.2160 0.0610 0.053 Uiso 1 1 calc R . . C54 C 0.1692(3) 0.1260(4) 0.13455(19) 0.0633(12) Uani 1 1 d . . . H54A H 0.1965 0.1364 0.1725 0.076 Uiso 1 1 calc R . . H54B H 0.1287 0.0988 0.1428 0.076 Uiso 1 1 calc R . . C55 C 0.2006(3) 0.0490(4) 0.0975(2) 0.0639(13) Uani 1 1 d . . . H55A H 0.1997 -0.0177 0.1160 0.077 Uiso 1 1 calc R . . H55B H 0.1755 0.0447 0.0580 0.077 Uiso 1 1 calc R . . C56 C 0.2685(3) 0.0742(4) 0.0906(3) 0.0816(16) Uani 1 1 d . . . H56A H 0.2849 0.0227 0.0666 0.122 Uiso 1 1 calc R . . H56B H 0.2942 0.0765 0.1293 0.122 Uiso 1 1 calc R . . H56C H 0.2699 0.1395 0.0714 0.122 Uiso 1 1 calc R . . C57 C 0.1435(2) 0.3295(4) 0.19284(18) 0.0674(14) Uani 1 1 d . B . H57A H 0.1131 0.3717 0.2101 0.081 Uiso 1 1 calc R . . H57B H 0.1487 0.2665 0.2156 0.081 Uiso 1 1 calc R . . C58 C 0.2075(2) 0.3847(5) 0.2002(2) 0.0734(15) Uani 1 1 d . B . H58A H 0.2362 0.3486 0.1776 0.088 Uiso 1 1 calc R . . H58B H 0.2012 0.4529 0.1837 0.088 Uiso 1 1 calc R . . C59 C 0.2386(3) 0.3926(5) 0.2647(2) 0.0788(16) Uani 1 1 d D . . H59A H 0.2726 0.4429 0.2678 0.095 Uiso 1 1 calc R A 1 H59B H 0.2072 0.4158 0.2890 0.095 Uiso 1 1 calc R A 1 C60 C 0.2659(5) 0.2913(7) 0.2886(4) 0.135(3) Uiso 1 1 d D B 1 H60A H 0.2873 0.3001 0.3287 0.203 Uiso 0.25 1 calc PR B 1 H60B H 0.2959 0.2668 0.2637 0.203 Uiso 0.25 1 calc PR B 1 H60C H 0.2318 0.2426 0.2883 0.203 Uiso 0.25 1 calc PR B 1 C61 C 0.1096(2) 0.3981(3) 0.08852(18) 0.0509(10) Uani 1 1 d . D . H61A H 0.0938 0.3767 0.0480 0.061 Uiso 1 1 calc R . . H61B H 0.1522 0.4257 0.0885 0.061 Uiso 1 1 calc R . . C62 C 0.0666(3) 0.4838(5) 0.1054(4) 0.104(2) Uani 1 1 d D . . H62A H 0.0256 0.4810 0.0797 0.125 Uiso 1 1 calc R C 1 H62B H 0.0590 0.4744 0.1464 0.125 Uiso 1 1 calc R C 1 C63A C 0.0966(6) 0.5860(12) 0.0994(11) 0.092(6) Uani 0.40 1 d PU D 1 C64A C 0.079(2) 0.5971(19) 0.0281(15) 0.18(2) Uani 0.40 1 d PU D 1 C63 C 0.0606(5) 0.5678(8) 0.0504(6) 0.084(3) Uani 0.60 1 d PDU D 2 H63A H 0.0629 0.5336 0.0127 0.101 Uiso 0.60 1 calc PR D 2 H63B H 0.0201 0.6038 0.0474 0.101 Uiso 0.60 1 calc PR D 2 C64 C 0.1136(6) 0.6390(13) 0.0641(14) 0.174(12) Uani 0.60 1 d PDU D 2 H64A H 0.1117 0.6891 0.0328 0.261 Uiso 0.60 1 calc PR D 2 H64B H 0.1533 0.6025 0.0670 0.261 Uiso 0.60 1 calc PR D 2 H64C H 0.1107 0.6725 0.1014 0.261 Uiso 0.60 1 calc PR D 2 N1 N 0.38372(11) 0.0813(2) 0.66026(10) 0.0257(5) Uani 1 1 d . . . N2 N 0.39817(11) -0.0997(2) 0.61814(10) 0.0256(5) Uani 1 1 d . . . N3 N 0.69879(12) 0.0775(2) 0.19040(11) 0.0287(6) Uani 1 1 d . . . N4 N 0.11500(16) 0.3038(3) 0.12868(13) 0.0493(8) Uani 1 1 d . . . Ni1 Ni 0.436346(18) -0.03079(3) 0.686693(16) 0.02820(14) Uani 1 1 d . . . O1 O 0.48252(11) 0.03549(19) 0.75157(10) 0.0384(6) Uani 1 1 d . . . O2 O 0.33773(11) 0.2368(2) 0.67599(12) 0.0507(7) Uani 1 1 d . . . O3 O 0.40606(11) -0.20887(18) 0.54002(9) 0.0331(5) Uani 1 1 d . . . O4 O 0.48034(12) -0.14407(19) 0.72029(10) 0.0413(6) Uani 1 1 d . . . O5 O 0.39299(16) 0.0593(3) 0.23098(16) 0.0721(9) Uani 1 1 d . . . S1 S 0.13328(4) -0.08505(9) 0.36058(4) 0.0456(3) Uani 1 1 d . . . S2 S 0.11304(5) 0.29226(8) 0.47653(4) 0.0515(3) 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 0.0285(15) 0.055(2) 0.0199(14) -0.0078(14) 0.0049(12) -0.0066(15) C2 0.0263(15) 0.053(2) 0.0226(14) -0.0133(14) 0.0086(12) -0.0063(14) C3 0.0226(14) 0.050(2) 0.0282(15) -0.0123(15) 0.0071(12) -0.0035(14) C4 0.0190(13) 0.0372(17) 0.0180(13) -0.0024(12) 0.0020(10) -0.0047(12) C5 0.0192(12) 0.0301(16) 0.0201(13) 0.0008(11) 0.0041(10) -0.0004(11) C6 0.0205(13) 0.0311(16) 0.0234(14) 0.0018(12) 0.0005(11) -0.0047(12) C7 0.0260(14) 0.0360(17) 0.0281(15) 0.0065(13) 0.0002(12) -0.0031(13) C8 0.0340(16) 0.0378(19) 0.0287(16) 0.0072(14) 0.0023(13) -0.0021(14) C9 0.048(2) 0.053(2) 0.0347(18) 0.0129(17) -0.0099(16) 0.0039(18) C10 0.059(2) 0.049(2) 0.050(2) 0.0116(19) -0.0118(19) 0.016(2) C11 0.065(3) 0.046(2) 0.055(2) -0.0004(19) -0.011(2) 0.020(2) C12 0.0430(19) 0.0376(19) 0.0388(19) -0.0011(15) -0.0033(15) 0.0065(16) C13 0.0253(14) 0.0304(16) 0.0203(13) -0.0017(12) 0.0041(11) -0.0004(12) C14 0.0203(13) 0.0363(17) 0.0193(13) -0.0025(12) 0.0016(10) -0.0028(12) C15 0.0261(15) 0.0382(17) 0.0242(15) -0.0055(13) 0.0022(12) 0.0043(13) C16 0.0258(15) 0.049(2) 0.0247(15) -0.0049(14) -0.0015(12) 0.0046(14) C17 0.044(2) 0.059(2) 0.041(2) -0.0120(18) 0.0008(16) -0.0122(18) C18 0.0397(18) 0.049(2) 0.0307(17) -0.0088(15) 0.0013(14) -0.0026(16) C19 0.064(3) 0.066(3) 0.060(3) -0.014(2) -0.001(2) -0.023(2) C20 0.0427(19) 0.051(2) 0.0311(17) -0.0005(16) 0.0038(14) 0.0039(17) C21 0.0236(14) 0.0371(17) 0.0226(14) -0.0021(13) 0.0023(11) -0.0001(13) C22 0.0318(16) 0.0435(19) 0.0226(14) -0.0045(13) 0.0012(12) 0.0075(14) C23 0.0460(19) 0.044(2) 0.0326(17) -0.0077(15) -0.0040(14) 0.0121(17) C24 0.0348(18) 0.077(3) 0.0335(18) -0.0081(19) -0.0034(14) 0.0145(19) C25 0.0299(16) 0.058(2) 0.0282(16) -0.0034(16) -0.0018(13) 0.0114(16) C26 0.037(2) 0.099(4) 0.055(3) -0.006(3) -0.0054(18) 0.022(2) C27 0.069(3) 0.036(2) 0.054(2) -0.0005(18) -0.002(2) -0.0023(19) C28 0.0270(14) 0.0328(16) 0.0276(15) -0.0062(13) 0.0044(12) 0.0000(13) C29 0.0304(16) 0.055(2) 0.0333(17) -0.0153(16) 0.0067(13) -0.0024(16) C30 0.0383(18) 0.054(2) 0.043(2) -0.0228(18) 0.0126(15) -0.0138(17) C31 0.0343(17) 0.069(3) 0.0289(17) -0.0171(17) 0.0004(14) -0.0116(18) C32 0.0357(17) 0.059(2) 0.0284(16) -0.0041(16) -0.0005(13) -0.0087(17) C33 0.0318(16) 0.0322(17) 0.0334(16) 0.0040(14) 0.0053(13) -0.0016(14) C34 0.0378(18) 0.0373(19) 0.050(2) -0.0005(16) 0.0129(16) 0.0025(15) C35 0.056(2) 0.043(2) 0.056(2) 0.0084(18) 0.0152(19) 0.0132(19) C36 0.062(3) 0.044(2) 0.087(3) 0.001(2) 0.020(2) 0.016(2) C37 0.0298(15) 0.0349(17) 0.0318(16) 0.0018(14) 0.0043(13) -0.0046(13) C38 0.0423(19) 0.0390(19) 0.0330(17) -0.0003(15) 0.0021(14) -0.0049(16) C39 0.0427(19) 0.043(2) 0.0386(19) -0.0013(16) -0.0039(15) -0.0063(16) C40 0.044(2) 0.056(3) 0.059(3) 0.002(2) -0.0051(18) -0.0025(19) C41 0.0300(15) 0.0388(18) 0.0286(16) 0.0007(14) 0.0099(12) -0.0007(14) C42 0.0391(18) 0.044(2) 0.0379(18) 0.0070(16) 0.0110(15) 0.0068(16) C43 0.045(2) 0.052(2) 0.049(2) 0.0038(18) 0.0158(17) 0.0134(18) C44 0.067(3) 0.050(2) 0.050(2) -0.0048(19) 0.023(2) 0.014(2) C45 0.0303(15) 0.0382(18) 0.0262(15) 0.0006(13) 0.0079(12) -0.0053(14) C46 0.0396(18) 0.052(2) 0.0308(17) -0.0018(16) 0.0070(14) -0.0132(16) C47 0.0384(18) 0.050(2) 0.0312(17) 0.0011(15) 0.0059(14) -0.0094(16) C48 0.0385(19) 0.072(3) 0.0342(18) -0.0083(18) 0.0039(15) -0.0079(19) C49 0.059(2) 0.082(3) 0.038(2) -0.010(2) 0.0256(18) -0.032(2) C50 0.048(2) 0.058(2) 0.042(2) -0.0059(18) 0.0193(17) -0.0164(19) C51 0.043(2) 0.066(3) 0.060(3) -0.010(2) 0.0175(18) -0.019(2) C52 0.043(2) 0.058(3) 0.060(3) -0.001(2) 0.0070(18) -0.0088(19) C53 0.047(2) 0.054(2) 0.0306(17) 0.0014(16) 0.0085(15) -0.0093(18) C54 0.084(3) 0.062(3) 0.041(2) 0.011(2) -0.003(2) -0.019(3) C55 0.083(3) 0.047(2) 0.056(3) 0.008(2) -0.010(2) -0.005(2) C56 0.089(4) 0.056(3) 0.096(4) -0.004(3) -0.001(3) -0.003(3) C57 0.081(3) 0.094(4) 0.031(2) -0.018(2) 0.020(2) -0.037(3) C58 0.074(3) 0.099(4) 0.050(3) -0.020(3) 0.019(2) -0.043(3) C59 0.085(4) 0.092(4) 0.058(3) -0.016(3) 0.006(3) -0.031(3) C61 0.057(2) 0.052(2) 0.051(2) -0.0133(19) 0.0317(19) -0.0127(19) C62 0.114(5) 0.076(4) 0.145(6) -0.010(4) 0.097(5) 0.017(4) C63A 0.031(6) 0.053(8) 0.19(2) -0.035(10) 0.023(9) 0.011(6) C64A 0.31(4) 0.077(14) 0.22(3) 0.085(17) 0.24(3) 0.12(2) C63 0.077(7) 0.076(7) 0.110(9) 0.003(7) 0.051(7) 0.034(6) C64 0.058(7) 0.102(14) 0.37(4) 0.059(17) 0.063(12) 0.026(7) N1 0.0208(11) 0.0351(14) 0.0208(12) -0.0065(10) 0.0021(9) 0.0006(10) N2 0.0217(11) 0.0363(14) 0.0185(11) -0.0002(10) 0.0024(9) -0.0007(10) N3 0.0284(13) 0.0316(14) 0.0274(13) 0.0016(11) 0.0083(10) -0.0022(11) N4 0.0571(19) 0.066(2) 0.0288(15) -0.0107(15) 0.0178(14) -0.0263(17) Ni1 0.0243(2) 0.0413(3) 0.0182(2) -0.00048(16) 0.00059(14) -0.00286(16) O1 0.0375(13) 0.0490(15) 0.0252(11) -0.0062(10) -0.0070(9) -0.0035(11) O2 0.0299(12) 0.0608(17) 0.0574(16) -0.0339(14) -0.0070(11) 0.0134(12) O3 0.0354(12) 0.0386(13) 0.0241(11) -0.0043(9) 0.0001(9) 0.0078(10) O4 0.0502(14) 0.0434(14) 0.0262(11) 0.0052(10) -0.0080(10) 0.0061(12) O5 0.0545(18) 0.085(2) 0.073(2) 0.0139(19) -0.0021(16) -0.0014(17) S1 0.0378(5) 0.0668(7) 0.0290(4) -0.0085(4) -0.0064(3) -0.0083(4) S2 0.0586(6) 0.0476(6) 0.0429(5) -0.0067(4) -0.0103(4) 0.0251(5) _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 1.319(4) . ? C1 C2 1.411(5) . ? C1 C32 1.420(4) . ? C2 C29 1.404(5) . ? C2 C3 1.504(4) . ? C3 O2 1.244(4) . ? C3 N1 1.357(4) . ? C4 C28 1.404(4) . ? C4 C5 1.414(4) . ? C4 N1 1.423(4) . ? C5 C13 1.401(4) . ? C5 N2 1.416(4) . ? C6 O3 1.246(4) . ? C6 N2 1.356(4) . ? C6 C7 1.494(4) . ? C7 C12 1.401(5) . ? C7 C8 1.410(4) . ? C8 O4 1.304(4) . ? C8 C9 1.426(5) . ? C9 C10 1.360(6) . ? C9 H9 0.9300 . ? C10 C11 1.398(6) . ? C10 H10 0.9300 . ? C11 C12 1.374(5) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.396(4) . ? C13 H13 0.9300 . ? C14 C21 1.411(4) . ? C14 C15 1.496(4) . ? C15 C16 1.363(5) . ? C15 C18 1.437(5) . ? C16 C20 1.470(5) . ? C16 S1 1.738(3) . ? C17 C18 1.359(5) . ? C17 C19 1.492(6) . ? C17 S1 1.728(4) . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C28 1.391(4) . ? C21 C22 1.476(4) . ? C22 C23 1.364(5) . ? C22 C25 1.444(5) . ? C23 C27 1.477(6) . ? C23 S2 1.762(4) . ? C24 C25 1.359(5) . ? C24 C26 1.505(5) . ? C24 S2 1.694(5) . ? C25 H25 0.9300 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28 0.9300 . ? C29 C30 1.385(5) . ? C29 H29 0.9300 . ? C30 C31 1.393(6) . ? C30 H30 0.9300 . ? C31 C32 1.372(6) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.513(5) . ? C33 N3 1.519(4) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C35 1.514(5) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C36 1.494(6) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 N3 1.529(4) . ? C37 C38 1.529(5) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.528(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.511(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.518(5) . ? C41 N3 1.519(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.532(5) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.507(6) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 C46 1.516(4) . ? C45 N3 1.525(4) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.502(5) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? C47 C48 1.521(5) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 C50 1.523(5) . ? C49 N4 1.531(5) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C50 C51 1.533(5) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 C52 1.510(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 N4 1.511(5) . ? C53 C54 1.539(6) . ? C53 H53A 0.9700 . ? C53 H53B 0.9700 . ? C54 C55 1.523(7) . ? C54 H54A 0.9700 . ? C54 H54B 0.9700 . ? C55 C56 1.502(8) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.521(6) . ? C57 N4 1.524(5) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 C59 1.512(7) . ? C58 H58A 0.9700 . ? C58 H58B 0.9700 . ? C59 C60 1.513(9) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 N4 1.526(5) . ? C61 C62 1.527(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63A 1.495(18) . ? C62 C63 1.650(12) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63A C64A 1.61(4) . ? C63 C64 1.455(15) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? N1 Ni1 1.885(3) . ? N2 Ni1 1.871(2) . ? Ni1 O4 1.852(2) . ? Ni1 O1 1.854(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 124.3(3) . . ? O1 C1 C32 117.6(3) . . ? C2 C1 C32 118.1(3) . . ? C29 C2 C1 119.3(3) . . ? C29 C2 C3 116.6(3) . . ? C1 C2 C3 124.1(3) . . ? O2 C3 N1 124.7(3) . . ? O2 C3 C2 117.6(3) . . ? N1 C3 C2 117.7(3) . . ? C28 C4 C5 118.7(3) . . ? C28 C4 N1 127.3(3) . . ? C5 C4 N1 114.0(3) . . ? C13 C5 C4 118.9(3) . . ? C13 C5 N2 126.2(3) . . ? C4 C5 N2 114.8(2) . . ? O3 C6 N2 123.8(3) . . ? O3 C6 C7 117.9(3) . . ? N2 C6 C7 118.3(3) . . ? C12 C7 C8 119.0(3) . . ? C12 C7 C6 116.8(3) . . ? C8 C7 C6 124.1(3) . . ? O4 C8 C7 124.9(3) . . ? O4 C8 C9 118.0(3) . . ? C7 C8 C9 117.1(3) . . ? C10 C9 C8 122.7(3) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C9 C10 C11 119.6(4) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 119.2(4) . . ? C12 C11 H11 120.4 . . ? C10 C11 H11 120.4 . . ? C11 C12 C7 122.3(3) . . ? C11 C12 H12 118.8 . . ? C7 C12 H12 118.8 . . ? C14 C13 C5 121.9(3) . . ? C14 C13 H13 119.0 . . ? C5 C13 H13 119.0 . . ? C13 C14 C21 119.2(3) . . ? C13 C14 C15 119.0(3) . . ? C21 C14 C15 121.8(3) . . ? C16 C15 C18 112.0(3) . . ? C16 C15 C14 126.3(3) . . ? C18 C15 C14 121.6(3) . . ? C15 C16 C20 130.4(3) . . ? C15 C16 S1 110.5(3) . . ? C20 C16 S1 119.1(2) . . ? C18 C17 C19 129.5(4) . . ? C18 C17 S1 109.4(3) . . ? C19 C17 S1 121.1(3) . . ? C17 C18 C15 114.8(4) . . ? C17 C18 H18 122.6 . . ? C15 C18 H18 122.6 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C28 C21 C14 119.0(3) . . ? C28 C21 C22 118.7(3) . . ? C14 C21 C22 122.2(3) . . ? C23 C22 C25 112.2(3) . . ? C23 C22 C21 123.6(3) . . ? C25 C22 C21 124.1(3) . . ? C22 C23 C27 129.7(3) . . ? C22 C23 S2 109.4(3) . . ? C27 C23 S2 120.7(3) . . ? C25 C24 C26 128.2(4) . . ? C25 C24 S2 110.5(3) . . ? C26 C24 S2 121.4(3) . . ? C24 C25 C22 114.3(4) . . ? C24 C25 H25 122.8 . . ? C22 C25 H25 122.8 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C21 C28 C4 122.2(3) . . ? C21 C28 H28 118.9 . . ? C4 C28 H28 118.9 . . ? C30 C29 C2 121.4(4) . . ? C30 C29 H29 119.3 . . ? C2 C29 H29 119.3 . . ? C29 C30 C31 119.3(4) . . ? C29 C30 H30 120.4 . . ? C31 C30 H30 120.4 . . ? C32 C31 C30 120.5(3) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C31 C32 C1 121.3(4) . . ? C31 C32 H32 119.4 . . ? C1 C32 H32 119.4 . . ? C34 C33 N3 116.8(3) . . ? C34 C33 H33A 108.1 . . ? N3 C33 H33A 108.1 . . ? C34 C33 H33B 108.1 . . ? N3 C33 H33B 108.1 . . ? H33A C33 H33B 107.3 . . ? C35 C34 C33 108.2(3) . . ? C35 C34 H34A 110.1 . . ? C33 C34 H34A 110.1 . . ? C35 C34 H34B 110.1 . . ? C33 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? C36 C35 C34 115.1(4) . . ? C36 C35 H35A 108.5 . . ? C34 C35 H35A 108.5 . . ? C36 C35 H35B 108.5 . . ? C34 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 C38 114.8(3) . . ? N3 C37 H37A 108.6 . . ? C38 C37 H37A 108.6 . . ? N3 C37 H37B 108.6 . . ? C38 C37 H37B 108.6 . . ? H37A C37 H37B 107.5 . . ? C39 C38 C37 111.5(3) . . ? C39 C38 H38A 109.3 . . ? C37 C38 H38A 109.3 . . ? C39 C38 H38B 109.3 . . ? C37 C38 H38B 109.3 . . ? H38A C38 H38B 108.0 . . ? C40 C39 C38 112.9(3) . . ? C40 C39 H39A 109.0 . . ? C38 C39 H39A 109.0 . . ? C40 C39 H39B 109.0 . . ? C38 C39 H39B 109.0 . . ? H39A C39 H39B 107.8 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 N3 115.5(3) . . ? C42 C41 H41A 108.4 . . ? N3 C41 H41A 108.4 . . ? C42 C41 H41B 108.4 . . ? N3 C41 H41B 108.4 . . ? H41A C41 H41B 107.5 . . ? C41 C42 C43 110.6(3) . . ? C41 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C44 C43 C42 113.8(3) . . ? C44 C43 H43A 108.8 . . ? C42 C43 H43A 108.8 . . ? C44 C43 H43B 108.8 . . ? C42 C43 H43B 108.8 . . ? H43A C43 H43B 107.7 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N3 114.2(3) . . ? C46 C45 H45A 108.7 . . ? N3 C45 H45A 108.7 . . ? C46 C45 H45B 108.7 . . ? N3 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C47 C46 C45 111.9(3) . . ? C47 C46 H46A 109.2 . . ? C45 C46 H46A 109.2 . . ? C47 C46 H46B 109.2 . . ? C45 C46 H46B 109.2 . . ? H46A C46 H46B 107.9 . . ? C46 C47 C48 111.8(3) . . ? C46 C47 H47A 109.3 . . ? C48 C47 H47A 109.3 . . ? C46 C47 H47B 109.3 . . ? C48 C47 H47B 109.3 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N4 115.1(3) . . ? C50 C49 H49A 108.5 . . ? N4 C49 H49A 108.5 . . ? C50 C49 H49B 108.5 . . ? N4 C49 H49B 108.5 . . ? H49A C49 H49B 107.5 . . ? C49 C50 C51 110.0(3) . . ? C49 C50 H50A 109.7 . . ? C51 C50 H50A 109.7 . . ? C49 C50 H50B 109.7 . . ? C51 C50 H50B 109.7 . . ? H50A C50 H50B 108.2 . . ? C52 C51 C50 111.7(3) . . ? C52 C51 H51A 109.3 . . ? C50 C51 H51A 109.3 . . ? C52 C51 H51B 109.3 . . ? C50 C51 H51B 109.3 . . ? H51A C51 H51B 107.9 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N4 C53 C54 116.1(3) . . ? N4 C53 H53A 108.3 . . ? C54 C53 H53A 108.3 . . ? N4 C53 H53B 108.3 . . ? C54 C53 H53B 108.3 . . ? H53A C53 H53B 107.4 . . ? C55 C54 C53 111.7(4) . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54B 109.3 . . ? C53 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 114.3(4) . . ? C56 C55 H55A 108.7 . . ? C54 C55 H55A 108.7 . . ? C56 C55 H55B 108.7 . . ? C54 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N4 115.5(3) . . ? C58 C57 H57A 108.4 . . ? N4 C57 H57A 108.4 . . ? C58 C57 H57B 108.4 . . ? N4 C57 H57B 108.4 . . ? H57A C57 H57B 107.5 . . ? C59 C58 C57 113.1(4) . . ? C59 C58 H58A 109.0 . . ? C57 C58 H58A 109.0 . . ? C59 C58 H58B 109.0 . . ? C57 C58 H58B 109.0 . . ? H58A C58 H58B 107.8 . . ? C60 C59 C58 111.9(6) . . ? C60 C59 H59A 109.2 . . ? C58 C59 H59A 109.2 . . ? C60 C59 H59B 109.2 . . ? C58 C59 H59B 109.2 . . ? H59A C59 H59B 107.9 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N4 C61 C62 116.1(4) . . ? N4 C61 H61A 108.3 . . ? C62 C61 H61A 108.3 . . ? N4 C61 H61B 108.3 . . ? C62 C61 H61B 108.3 . . ? H61A C61 H61B 107.4 . . ? C63A C62 C61 111.0(6) . . ? C63A C62 C63 47.4(9) . . ? C61 C62 C63 106.4(5) . . ? C63A C62 H62A 109.4 . . ? C61 C62 H62A 109.4 . . ? C63 C62 H62A 67.0 . . ? C63A C62 H62B 109.4 . . ? C61 C62 H62B 109.4 . . ? C63 C62 H62B 143.0 . . ? H62A C62 H62B 108.0 . . ? C62 C63A C64A 97.5(18) . . ? C64 C63 C62 107.2(15) . . ? C64 C63 H63A 110.3 . . ? C62 C63 H63A 110.3 . . ? C64 C63 H63B 110.3 . . ? C62 C63 H63B 110.3 . . ? H63A C63 H63B 108.5 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C3 N1 C4 121.0(3) . . ? C3 N1 Ni1 127.3(2) . . ? C4 N1 Ni1 111.3(2) . . ? C6 N2 C5 120.7(2) . . ? C6 N2 Ni1 126.22(19) . . ? C5 N2 Ni1 111.8(2) . . ? C41 N3 C33 105.7(2) . . ? C41 N3 C45 111.0(2) . . ? C33 N3 C45 110.7(2) . . ? C41 N3 C37 111.0(2) . . ? C33 N3 C37 110.9(2) . . ? C45 N3 C37 107.5(2) . . ? C53 N4 C61 106.4(3) . . ? C53 N4 C57 110.2(4) . . ? C61 N4 C57 111.8(3) . . ? C53 N4 C49 111.9(3) . . ? C61 N4 C49 109.5(3) . . ? C57 N4 C49 107.1(3) . . ? O4 Ni1 O1 82.87(11) . . ? O4 Ni1 N2 94.77(11) . . ? O1 Ni1 N2 173.81(11) . . ? O4 Ni1 N1 172.04(11) . . ? O1 Ni1 N1 95.98(11) . . ? N2 Ni1 N1 87.14(11) . . ? C1 O1 Ni1 125.5(2) . . ? C8 O4 Ni1 126.1(2) . . ? C17 S1 C16 93.24(17) . . ? C24 S2 C23 93.59(19) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.159 _refine_diff_density_min -0.720 _refine_diff_density_rms 0.085 data_mk1101 _database_code_depnum_ccdc_archive 'CCDC 850435' #TrackingRef '17768_web_deposit_cif_file_2_FrankW.Heinemann_1360922652.CCDC850435_36.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 N2 O4 S2, C H Cl3' _chemical_formula_sum 'C33 H29 Cl3 N2 O4 S2' _chemical_formula_weight 688.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.992(2) _cell_length_b 11.907(3) _cell_length_c 14.865(3) _cell_angle_alpha 74.563(4) _cell_angle_beta 75.616(4) _cell_angle_gamma 67.825(4) _cell_volume 1556.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4954 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.91 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.471 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.667 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2009' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'ImuS micro-focus tube' _diffrn_radiation_monochromator 'Quazar focussing montel optics' _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24101 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6808 _reflns_number_gt 4936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. DFIX and SADI restraints were indroduced for the refinement of the disordered CHCl3 molecule. ; _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^)+(0.0390P)^2^+1.5307P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6808 _refine_ls_number_parameters 431 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1025 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.72280(8) 0.35956(6) 0.53927(5) 0.02414(15) Uani 1 1 d . . . S2 S 0.24921(7) 0.11347(5) 0.55443(4) 0.02084(15) Uani 1 1 d . . . O1 O 0.75320(17) 0.09616(14) 0.99635(12) 0.0189(4) Uani 1 1 d . . . O2 O 0.8551(2) 0.08389(15) 1.14169(13) 0.0281(4) Uani 1 1 d . . . H2A H 0.8167 0.1182 1.0928 0.042 Uiso 1 1 calc R . . O3 O 0.78988(17) -0.31329(14) 0.95119(12) 0.0206(4) Uani 1 1 d . . . O4 O 0.86855(19) -0.53387(15) 1.04154(14) 0.0275(4) Uani 1 1 d . . . H4 H 0.8790 -0.4668 1.0104 0.041 Uiso 1 1 calc R . . N1 N 0.7573(2) -0.07938(17) 0.96233(14) 0.0176(4) Uani 1 1 d . . . H1A H 0.7917 -0.1606 0.9768 0.021 Uiso 1 1 calc R . . N2 N 0.5532(2) -0.19345(16) 0.95722(14) 0.0169(4) Uani 1 1 d . . . H2B H 0.4629 -0.1862 0.9862 0.020 Uiso 1 1 calc R . . C1 C 0.5866(2) 0.1223(2) 0.75281(16) 0.0158(5) Uani 1 1 d . . . C2 C 0.6705(2) 0.0765(2) 0.82524(17) 0.0173(5) Uani 1 1 d . . . H2C H 0.7325 0.1187 0.8286 0.021 Uiso 1 1 calc R . . C3 C 0.6660(2) -0.0285(2) 0.89221(16) 0.0170(5) Uani 1 1 d . . . C4 C 0.5734(2) -0.08985(19) 0.88815(16) 0.0153(5) Uani 1 1 d . . . C5 C 0.4882(2) -0.0433(2) 0.81731(16) 0.0156(5) Uani 1 1 d . . . H5A H 0.4239 -0.0844 0.8157 0.019 Uiso 1 1 calc R . . C6 C 0.4927(2) 0.0609(2) 0.74838(16) 0.0157(5) Uani 1 1 d . . . C7 C 0.7120(3) 0.2175(2) 0.60066(17) 0.0196(5) Uani 1 1 d . . . C8 C 0.6106(3) 0.2301(2) 0.68082(17) 0.0166(5) Uani 1 1 d . . . C9 C 0.5419(3) 0.3560(2) 0.69238(18) 0.0199(5) Uani 1 1 d . . . H9A H 0.4692 0.3804 0.7450 0.024 Uiso 1 1 calc R . . C10 C 0.5901(3) 0.4371(2) 0.62144(18) 0.0207(5) Uani 1 1 d . . . C11 C 0.8085(3) 0.1019(2) 0.5650(2) 0.0323(7) Uani 1 1 d . . . H11A H 0.7835 0.0311 0.6066 0.049 Uiso 1 1 calc R . . H11B H 0.9112 0.0901 0.5643 0.049 Uiso 1 1 calc R . . H11C H 0.7939 0.1087 0.5007 0.049 Uiso 1 1 calc R . . C12 C 0.5469(3) 0.5744(2) 0.6094(2) 0.0284(6) Uani 1 1 d . . . H12A H 0.4474 0.6070 0.6436 0.043 Uiso 1 1 calc R . . H12B H 0.5498 0.6118 0.5420 0.043 Uiso 1 1 calc R . . H12C H 0.6153 0.5943 0.6347 0.043 Uiso 1 1 calc R . . C13 C 0.3740(3) 0.0288(2) 0.62983(17) 0.0181(5) Uani 1 1 d . . . C14 C 0.3981(2) 0.1042(2) 0.67516(16) 0.0154(5) Uani 1 1 d . . . C15 C 0.3124(3) 0.2311(2) 0.64752(17) 0.0177(5) Uani 1 1 d . . . H15A H 0.3158 0.2958 0.6720 0.021 Uiso 1 1 calc R . . C16 C 0.2263(3) 0.2511(2) 0.58359(17) 0.0181(5) Uani 1 1 d . . . C17 C 0.4373(3) -0.1086(2) 0.63622(19) 0.0247(6) Uani 1 1 d . . . H17A H 0.5319 -0.1400 0.6582 0.037 Uiso 1 1 calc R . . H17B H 0.4514 -0.1278 0.5737 0.037 Uiso 1 1 calc R . . H17C H 0.3700 -0.1477 0.6810 0.037 Uiso 1 1 calc R . . C18 C 0.1200(3) 0.3692(2) 0.54240(19) 0.0239(6) Uani 1 1 d . . . H18A H 0.1205 0.4369 0.5678 0.036 Uiso 1 1 calc R . . H18B H 0.0216 0.3628 0.5588 0.036 Uiso 1 1 calc R . . H18C H 0.1481 0.3854 0.4734 0.036 Uiso 1 1 calc R . . C19 C 0.7974(2) -0.0192(2) 1.00931(17) 0.0175(5) Uani 1 1 d . . . C20 C 0.8924(2) -0.0961(2) 1.08078(17) 0.0180(5) Uani 1 1 d . . . C21 C 0.9113(3) -0.0395(2) 1.14589(18) 0.0201(5) Uani 1 1 d . . . C22 C 0.9896(3) -0.1109(2) 1.21848(18) 0.0248(6) Uani 1 1 d . . . H22A H 0.9993 -0.0726 1.2639 0.030 Uiso 1 1 calc R . . C23 C 1.0533(3) -0.2364(2) 1.2251(2) 0.0295(6) Uani 1 1 d . . . H23A H 1.1067 -0.2846 1.2750 0.035 Uiso 1 1 calc R . . C24 C 1.0396(3) -0.2926(2) 1.1591(2) 0.0298(6) Uani 1 1 d . . . H24A H 1.0855 -0.3792 1.1630 0.036 Uiso 1 1 calc R . . C25 C 0.9602(3) -0.2236(2) 1.08811(19) 0.0250(6) Uani 1 1 d . . . H25A H 0.9511 -0.2631 1.0433 0.030 Uiso 1 1 calc R . . C26 C 0.6571(3) -0.3007(2) 0.98264(16) 0.0171(5) Uani 1 1 d . . . C27 C 0.6139(3) -0.4037(2) 1.04546(17) 0.0177(5) Uani 1 1 d . . . C28 C 0.7246(3) -0.5178(2) 1.07032(18) 0.0213(5) Uani 1 1 d . . . C29 C 0.6869(3) -0.6190(2) 1.12585(19) 0.0249(6) Uani 1 1 d . . . H29A H 0.7614 -0.6951 1.1429 0.030 Uiso 1 1 calc R . . C30 C 0.5428(3) -0.6089(2) 1.15580(19) 0.0259(6) Uani 1 1 d . . . H30A H 0.5178 -0.6788 1.1927 0.031 Uiso 1 1 calc R . . C31 C 0.4324(3) -0.4978(2) 1.13309(19) 0.0259(6) Uani 1 1 d . . . H31A H 0.3326 -0.4915 1.1551 0.031 Uiso 1 1 calc R . . C32 C 0.4680(3) -0.3970(2) 1.07872(18) 0.0218(5) Uani 1 1 d . . . H32A H 0.3920 -0.3212 1.0634 0.026 Uiso 1 1 calc R . . C100 C 0.0152(3) 0.3283(2) 0.24647(19) 0.0310(6) Uani 1 1 d D . . H10A H 0.0299 0.3519 0.1758 0.037 Uiso 1 1 calc R A 1 Cl11 Cl 0.1716(6) 0.3321(4) 0.2774(5) 0.0354(14) Uani 0.39(2) 1 d PD B 1 Cl12 Cl -0.1394(6) 0.4467(7) 0.2847(6) 0.0468(16) Uani 0.39(2) 1 d PD B 1 Cl13 Cl -0.0037(9) 0.1875(4) 0.2705(11) 0.064(2) Uani 0.39(2) 1 d PD B 1 Cl21 Cl 0.1720(4) 0.3052(10) 0.2908(6) 0.0893(16) Uani 0.61(2) 1 d PD B 2 Cl22 Cl -0.1257(6) 0.4577(4) 0.2763(4) 0.0518(12) Uani 0.61(2) 1 d PD B 2 Cl23 Cl -0.0444(10) 0.2002(5) 0.3045(5) 0.0705(13) Uani 0.61(2) 1 d PD B 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 S1 0.0343(4) 0.0235(3) 0.0170(3) 0.0015(3) -0.0017(3) -0.0174(3) S2 0.0242(3) 0.0172(3) 0.0226(3) -0.0013(2) -0.0105(3) -0.0060(2) O1 0.0158(8) 0.0168(8) 0.0218(9) -0.0004(7) -0.0038(7) -0.0048(7) O2 0.0311(10) 0.0232(9) 0.0322(11) -0.0062(8) -0.0127(9) -0.0063(8) O3 0.0148(8) 0.0182(8) 0.0228(9) -0.0021(7) -0.0007(7) -0.0017(7) O4 0.0198(9) 0.0164(8) 0.0386(12) -0.0004(8) -0.0066(8) 0.0000(7) N1 0.0169(10) 0.0160(9) 0.0179(11) 0.0040(8) -0.0067(8) -0.0058(8) N2 0.0147(10) 0.0129(9) 0.0184(11) 0.0024(8) -0.0024(8) -0.0034(8) C1 0.0150(11) 0.0132(10) 0.0150(12) 0.0010(9) -0.0013(9) -0.0035(9) C2 0.0147(11) 0.0162(11) 0.0198(13) -0.0004(10) -0.0016(10) -0.0068(9) C3 0.0136(11) 0.0183(11) 0.0164(12) -0.0015(10) -0.0038(9) -0.0028(9) C4 0.0152(11) 0.0117(10) 0.0152(12) 0.0007(9) -0.0003(9) -0.0041(9) C5 0.0144(11) 0.0132(10) 0.0181(12) -0.0004(9) -0.0025(9) -0.0053(9) C6 0.0138(11) 0.0142(10) 0.0181(12) -0.0024(9) -0.0032(9) -0.0036(9) C7 0.0249(13) 0.0191(12) 0.0171(13) 0.0011(10) -0.0047(10) -0.0124(10) C8 0.0175(11) 0.0155(11) 0.0178(12) 0.0036(9) -0.0074(10) -0.0084(9) C9 0.0209(12) 0.0166(11) 0.0214(13) 0.0021(10) -0.0061(10) -0.0077(10) C10 0.0241(13) 0.0180(11) 0.0224(13) 0.0000(10) -0.0080(10) -0.0096(10) C11 0.0420(17) 0.0248(14) 0.0283(16) -0.0082(12) 0.0048(13) -0.0137(13) C12 0.0347(15) 0.0179(12) 0.0335(16) 0.0013(11) -0.0099(12) -0.0113(11) C13 0.0194(12) 0.0147(11) 0.0182(13) 0.0022(9) -0.0051(10) -0.0057(9) C14 0.0148(11) 0.0147(11) 0.0142(12) 0.0035(9) -0.0022(9) -0.0064(9) C15 0.0194(12) 0.0135(11) 0.0204(13) 0.0014(9) -0.0051(10) -0.0076(9) C16 0.0194(12) 0.0141(11) 0.0195(13) 0.0012(10) -0.0049(10) -0.0059(9) C17 0.0305(14) 0.0160(12) 0.0278(15) -0.0026(10) -0.0094(11) -0.0062(10) C18 0.0241(13) 0.0173(12) 0.0277(15) 0.0027(11) -0.0109(11) -0.0047(10) C19 0.0114(11) 0.0185(11) 0.0187(13) -0.0016(10) -0.0005(9) -0.0033(9) C20 0.0139(11) 0.0205(12) 0.0178(13) 0.0015(10) -0.0031(9) -0.0071(9) C21 0.0135(11) 0.0213(12) 0.0228(14) -0.0019(10) 0.0004(10) -0.0065(10) C22 0.0197(12) 0.0365(15) 0.0204(14) -0.0054(12) -0.0018(10) -0.0131(11) C23 0.0206(13) 0.0334(14) 0.0301(16) 0.0101(12) -0.0106(11) -0.0109(12) C24 0.0245(14) 0.0214(13) 0.0408(18) 0.0041(12) -0.0126(12) -0.0070(11) C25 0.0216(13) 0.0228(12) 0.0321(15) -0.0033(11) -0.0091(11) -0.0074(10) C26 0.0170(11) 0.0169(11) 0.0164(12) -0.0045(9) -0.0035(9) -0.0033(9) C27 0.0212(12) 0.0144(11) 0.0166(12) 0.0002(9) -0.0056(10) -0.0054(9) C28 0.0212(12) 0.0194(12) 0.0230(13) -0.0041(10) -0.0068(10) -0.0044(10) C29 0.0298(14) 0.0138(11) 0.0301(15) 0.0003(10) -0.0114(12) -0.0051(10) C30 0.0346(15) 0.0191(12) 0.0259(15) 0.0021(11) -0.0085(12) -0.0130(11) C31 0.0243(13) 0.0246(13) 0.0279(15) -0.0016(11) -0.0029(11) -0.0106(11) C32 0.0225(13) 0.0161(11) 0.0238(14) -0.0003(10) -0.0059(10) -0.0043(10) C100 0.0266(14) 0.0384(16) 0.0255(15) -0.0087(13) -0.0035(12) -0.0068(12) Cl11 0.0310(18) 0.043(3) 0.040(2) -0.0057(14) -0.0136(13) -0.0180(11) Cl12 0.0227(19) 0.077(4) 0.046(3) -0.046(3) 0.0067(17) -0.0074(19) Cl13 0.076(3) 0.0296(14) 0.096(5) -0.017(2) -0.034(3) -0.0128(15) Cl21 0.0370(16) 0.162(4) 0.072(3) -0.048(3) -0.0185(14) -0.013(2) Cl22 0.067(3) 0.0282(13) 0.053(2) -0.0112(12) -0.0223(18) 0.0023(13) Cl23 0.125(3) 0.0301(14) 0.063(2) 0.0030(11) -0.036(2) -0.0281(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C7 1.724(2) . ? S1 C10 1.725(3) . ? S2 C13 1.724(2) . ? S2 C16 1.724(2) . ? O1 C19 1.250(3) . ? O2 C21 1.350(3) . ? O2 H2A 0.8400 . ? O3 C26 1.257(3) . ? O4 C28 1.348(3) . ? O4 H4 0.8400 . ? N1 C19 1.336(3) . ? N1 C3 1.415(3) . ? N1 H1A 0.8800 . ? N2 C26 1.337(3) . ? N2 C4 1.424(3) . ? N2 H2B 0.8800 . ? C1 C2 1.397(3) . ? C1 C6 1.412(3) . ? C1 C8 1.492(3) . ? C2 C3 1.383(3) . ? C2 H2C 0.9500 . ? C3 C4 1.399(3) . ? C4 C5 1.385(3) . ? C5 C6 1.391(3) . ? C5 H5A 0.9500 . ? C6 C14 1.479(3) . ? C7 C8 1.360(3) . ? C7 C11 1.496(3) . ? C8 C9 1.431(3) . ? C9 C10 1.354(3) . ? C9 H9A 0.9500 . ? C10 C12 1.497(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.373(3) . ? C13 C17 1.501(3) . ? C14 C15 1.433(3) . ? C15 C16 1.353(3) . ? C15 H15A 0.9500 . ? C16 C18 1.489(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.482(3) . ? C20 C25 1.395(3) . ? C20 C21 1.400(3) . ? C21 C22 1.389(3) . ? C22 C23 1.372(4) . ? C22 H22A 0.9500 . ? C23 C24 1.383(4) . ? C23 H23A 0.9500 . ? C24 C25 1.372(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C27 1.468(3) . ? C27 C32 1.397(3) . ? C27 C28 1.416(3) . ? C28 C29 1.391(4) . ? C29 C30 1.366(4) . ? C29 H29A 0.9500 . ? C30 C31 1.388(3) . ? C30 H30A 0.9500 . ? C31 C32 1.372(4) . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? C100 Cl13 1.692(5) . ? C100 Cl22 1.723(4) . ? C100 Cl12 1.745(5) . ? C100 Cl21 1.748(4) . ? C100 Cl11 1.754(4) . ? C100 Cl23 1.777(4) . ? C100 H10A 1.0000 . ? 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 C7 S1 C10 92.98(12) . . ? C13 S2 C16 92.90(11) . . ? C21 O2 H2A 109.5 . . ? C28 O4 H4 109.5 . . ? C19 N1 C3 127.9(2) . . ? C19 N1 H1A 116.0 . . ? C3 N1 H1A 116.0 . . ? C26 N2 C4 126.8(2) . . ? C26 N2 H2B 116.6 . . ? C4 N2 H2B 116.6 . . ? C2 C1 C6 119.2(2) . . ? C2 C1 C8 116.5(2) . . ? C6 C1 C8 124.2(2) . . ? C3 C2 C1 122.0(2) . . ? C3 C2 H2C 119.0 . . ? C1 C2 H2C 119.0 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 N1 122.1(2) . . ? C4 C3 N1 118.7(2) . . ? C5 C4 C3 119.0(2) . . ? C5 C4 N2 117.3(2) . . ? C3 C4 N2 123.5(2) . . ? C4 C5 C6 122.8(2) . . ? C4 C5 H5A 118.6 . . ? C6 C5 H5A 118.6 . . ? C5 C6 C1 117.9(2) . . ? C5 C6 C14 119.3(2) . . ? C1 C6 C14 122.8(2) . . ? C8 C7 C11 128.7(2) . . ? C8 C7 S1 110.50(17) . . ? C11 C7 S1 120.74(19) . . ? C7 C8 C9 112.6(2) . . ? C7 C8 C1 122.8(2) . . ? C9 C8 C1 124.3(2) . . ? C10 C9 C8 113.8(2) . . ? C10 C9 H9A 123.1 . . ? C8 C9 H9A 123.1 . . ? C9 C10 C12 129.4(2) . . ? C9 C10 S1 110.09(18) . . ? C12 C10 S1 120.5(2) . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C17 130.8(2) . . ? C14 C13 S2 110.91(16) . . ? C17 C13 S2 118.30(17) . . ? C13 C14 C15 111.6(2) . . ? C13 C14 C6 124.9(2) . . ? C15 C14 C6 123.3(2) . . ? C16 C15 C14 114.4(2) . . ? C16 C15 H15A 122.8 . . ? C14 C15 H15A 122.8 . . ? C15 C16 C18 128.9(2) . . ? C15 C16 S2 110.14(17) . . ? C18 C16 S2 120.91(17) . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O1 C19 N1 122.0(2) . . ? O1 C19 C20 121.4(2) . . ? N1 C19 C20 116.6(2) . . ? C25 C20 C21 118.4(2) . . ? C25 C20 C19 122.8(2) . . ? C21 C20 C19 118.7(2) . . ? O2 C21 C22 117.6(2) . . ? O2 C21 C20 122.5(2) . . ? C22 C21 C20 119.9(2) . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C22 C23 C24 119.9(2) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C25 C24 C23 120.2(2) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C20 120.9(2) . . ? C24 C25 H25A 119.5 . . ? C20 C25 H25A 119.5 . . ? O3 C26 N2 120.1(2) . . ? O3 C26 C27 120.7(2) . . ? N2 C26 C27 119.2(2) . . ? C32 C27 C28 118.0(2) . . ? C32 C27 C26 123.2(2) . . ? C28 C27 C26 118.8(2) . . ? O4 C28 C29 117.3(2) . . ? O4 C28 C27 122.5(2) . . ? C29 C28 C27 120.2(2) . . ? C30 C29 C28 120.0(2) . . ? C30 C29 H29A 120.0 . . ? C28 C29 H29A 120.0 . . ? C29 C30 C31 120.9(2) . . ? C29 C30 H30A 119.6 . . ? C31 C30 H30A 119.6 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31A 120.1 . . ? C30 C31 H31A 120.1 . . ? C31 C32 C27 121.2(2) . . ? C31 C32 H32A 119.4 . . ? C27 C32 H32A 119.4 . . ? Cl13 C100 Cl22 122.7(3) . . ? Cl13 C100 Cl12 115.6(4) . . ? Cl13 C100 Cl21 105.4(5) . . ? Cl22 C100 Cl21 111.4(3) . . ? Cl12 C100 Cl21 114.5(4) . . ? Cl13 C100 Cl11 115.6(3) . . ? Cl22 C100 Cl11 106.1(3) . . ? Cl12 C100 Cl11 110.3(3) . . ? Cl22 C100 Cl23 106.3(3) . . ? Cl12 C100 Cl23 99.1(4) . . ? Cl21 C100 Cl23 106.4(4) . . ? Cl11 C100 Cl23 117.2(3) . . ? Cl13 C100 H10A 104.6 . . ? Cl22 C100 H10A 100.6 . . ? Cl12 C100 H10A 104.6 . . ? Cl21 C100 H10A 111.8 . . ? Cl11 C100 H10A 104.6 . . ? Cl23 C100 H10A 120.1 . . ? 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 C6 C1 C2 C3 0.9(3) . . . . ? C8 C1 C2 C3 -175.2(2) . . . . ? C1 C2 C3 C4 -0.9(3) . . . . ? C1 C2 C3 N1 176.2(2) . . . . ? C19 N1 C3 C2 37.8(4) . . . . ? C19 N1 C3 C4 -145.1(2) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? N1 C3 C4 C5 -177.4(2) . . . . ? C2 C3 C4 N2 -175.6(2) . . . . ? N1 C3 C4 N2 7.3(3) . . . . ? C26 N2 C4 C5 126.8(2) . . . . ? C26 N2 C4 C3 -57.8(3) . . . . ? C3 C4 C5 C6 1.3(3) . . . . ? N2 C4 C5 C6 176.9(2) . . . . ? C4 C5 C6 C1 -1.3(3) . . . . ? C4 C5 C6 C14 179.9(2) . . . . ? C2 C1 C6 C5 0.1(3) . . . . ? C8 C1 C6 C5 175.9(2) . . . . ? C2 C1 C6 C14 178.9(2) . . . . ? C8 C1 C6 C14 -5.3(3) . . . . ? C10 S1 C7 C8 -0.07(19) . . . . ? C10 S1 C7 C11 -179.0(2) . . . . ? C11 C7 C8 C9 178.6(2) . . . . ? S1 C7 C8 C9 -0.2(3) . . . . ? C11 C7 C8 C1 4.5(4) . . . . ? S1 C7 C8 C1 -174.28(17) . . . . ? C2 C1 C8 C7 89.8(3) . . . . ? C6 C1 C8 C7 -86.1(3) . . . . ? C2 C1 C8 C9 -83.5(3) . . . . ? C6 C1 C8 C9 100.6(3) . . . . ? C7 C8 C9 C10 0.5(3) . . . . ? C1 C8 C9 C10 174.5(2) . . . . ? C8 C9 C10 C12 -178.9(2) . . . . ? C8 C9 C10 S1 -0.5(3) . . . . ? C7 S1 C10 C9 0.36(19) . . . . ? C7 S1 C10 C12 178.8(2) . . . . ? C16 S2 C13 C14 -0.6(2) . . . . ? C16 S2 C13 C17 179.5(2) . . . . ? C17 C13 C14 C15 -179.7(3) . . . . ? S2 C13 C14 C15 0.4(3) . . . . ? C17 C13 C14 C6 -3.5(4) . . . . ? S2 C13 C14 C6 176.55(19) . . . . ? C5 C6 C14 C13 -41.6(3) . . . . ? C1 C6 C14 C13 139.7(2) . . . . ? C5 C6 C14 C15 134.2(2) . . . . ? C1 C6 C14 C15 -44.6(3) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C6 C14 C15 C16 -176.2(2) . . . . ? C14 C15 C16 C18 177.5(2) . . . . ? C14 C15 C16 S2 -0.5(3) . . . . ? C13 S2 C16 C15 0.6(2) . . . . ? C13 S2 C16 C18 -177.5(2) . . . . ? C3 N1 C19 O1 1.4(4) . . . . ? C3 N1 C19 C20 178.9(2) . . . . ? O1 C19 C20 C25 -170.8(2) . . . . ? N1 C19 C20 C25 11.6(4) . . . . ? O1 C19 C20 C21 11.4(4) . . . . ? N1 C19 C20 C21 -166.1(2) . . . . ? C25 C20 C21 O2 177.1(2) . . . . ? C19 C20 C21 O2 -5.1(4) . . . . ? C25 C20 C21 C22 -3.2(4) . . . . ? C19 C20 C21 C22 174.6(2) . . . . ? O2 C21 C22 C23 -178.0(2) . . . . ? C20 C21 C22 C23 2.3(4) . . . . ? C21 C22 C23 C24 0.0(4) . . . . ? C22 C23 C24 C25 -1.3(4) . . . . ? C23 C24 C25 C20 0.3(4) . . . . ? C21 C20 C25 C24 2.0(4) . . . . ? C19 C20 C25 C24 -175.8(2) . . . . ? C4 N2 C26 O3 7.0(3) . . . . ? C4 N2 C26 C27 -171.5(2) . . . . ? O3 C26 C27 C32 -176.7(2) . . . . ? N2 C26 C27 C32 1.7(3) . . . . ? O3 C26 C27 C28 0.2(3) . . . . ? N2 C26 C27 C28 178.6(2) . . . . ? C32 C27 C28 O4 179.8(2) . . . . ? C26 C27 C28 O4 2.7(3) . . . . ? C32 C27 C28 C29 0.3(3) . . . . ? C26 C27 C28 C29 -176.8(2) . . . . ? O4 C28 C29 C30 -178.9(2) . . . . ? C27 C28 C29 C30 0.6(4) . . . . ? C28 C29 C30 C31 -1.2(4) . . . . ? C29 C30 C31 C32 0.9(4) . . . . ? C30 C31 C32 C27 0.0(4) . . . . ? C28 C27 C32 C31 -0.6(3) . . . . ? C26 C27 C32 C31 176.3(2) . . . . ? 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 O2 H2A O1 0.84 1.82 2.557(2) 146.0 . O4 H4 O3 0.84 1.79 2.532(2) 145.8 . O4 H4 O4 0.84 2.45 2.921(4) 116.3 2_747 N1 H1A O3 0.88 1.96 2.725(3) 144.3 . N2 H2B O1 0.88 2.00 2.809(3) 152.1 2_657 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.446 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.064 _iucr_refine_instruction_details ; TITL MK1101 in P-1, KOEHLER/KHUSNIYAROV, MAK66org CELL 0.71073 9.9920 11.9075 14.8653 74.563 75.616 67.825 ZERR 2.00 0.0024 0.0028 0.0033 0.004 0.004 0.004 LATT 1 SFAC C H N O S CL UNIT 66 58 4 8 4 6 TEMP -173.000 ACTA SIZE 0.26 0.20 0.08 SHEL 8.0 0.78 L.S. 16 FMAP 2 PLAN 20 BOND .5 $H EQIV $1 -x+2, -y-1, -z+2 EQIV $2 -x+1, -y, -z+2 DFIX 1.750 0.007 C100 CL11 C100 CL12 C100 CL13 DFIX 1.750 0.007 C100 CL21 C100 CL22 C100 CL23 DFIX 2.890 0.007 CL11 CL12 CL21 CL22 SADI C100 CL11 C100 CL13 SADI C100 CL21 C100 CL23 SADI CL11 CL12 CL11 CL13 CL11 CL12 CL12 CL13 SADI CL21 CL22 CL21 CL23 CL21 CL22 CL22 CL23 HTAB O2 O1 HTAB O4 O3 HTAB O4 O4_$1 HTAB N1 O3 HTAB N2 O1_$2 HTAB CONF WPDB -1 LIST 4 WGHT 0.039000 1.530700 FVAR 0.14795 0.39433 S1 5 0.722802 0.359555 0.539270 11.00000 0.03426 0.02350 = 0.01697 0.00145 -0.00167 -0.01742 S2 5 0.249206 0.113475 0.554429 11.00000 0.02418 0.01720 = 0.02261 -0.00132 -0.01053 -0.00603 O1 4 0.753203 0.096159 0.996351 11.00000 0.01576 0.01682 = 0.02182 -0.00037 -0.00380 -0.00476 O2 4 0.855107 0.083886 1.141692 11.00000 0.03109 0.02322 = 0.03221 -0.00621 -0.01265 -0.00628 AFIX 147 H2A 2 0.816661 0.118219 1.092768 11.00000 -1.50000 AFIX 0 O3 4 0.789880 -0.313285 0.951192 11.00000 0.01483 0.01815 = 0.02277 -0.00210 -0.00071 -0.00172 O4 4 0.868546 -0.533865 1.041541 11.00000 0.01983 0.01638 = 0.03863 -0.00035 -0.00661 -0.00001 AFIX 147 H4 2 0.879018 -0.466760 1.010441 11.00000 -1.50000 AFIX 0 N1 3 0.757256 -0.079377 0.962333 11.00000 0.01685 0.01598 = 0.01789 0.00398 -0.00671 -0.00581 AFIX 43 H1A 2 0.791732 -0.160575 0.976758 11.00000 -1.20000 AFIX 0 N2 3 0.553176 -0.193453 0.957224 11.00000 0.01473 0.01292 = 0.01840 0.00240 -0.00245 -0.00341 AFIX 43 H2B 2 0.462910 -0.186172 0.986203 11.00000 -1.20000 AFIX 0 C1 1 0.586563 0.122331 0.752807 11.00000 0.01502 0.01324 = 0.01498 0.00097 -0.00126 -0.00350 C2 1 0.670486 0.076503 0.825235 11.00000 0.01470 0.01623 = 0.01975 -0.00045 -0.00158 -0.00678 AFIX 43 H2C 2 0.732479 0.118698 0.828614 11.00000 -1.20000 AFIX 0 C3 1 0.666030 -0.028508 0.892208 11.00000 0.01358 0.01834 = 0.01635 -0.00147 -0.00380 -0.00283 C4 1 0.573357 -0.089848 0.888155 11.00000 0.01519 0.01167 = 0.01525 0.00072 -0.00026 -0.00411 C5 1 0.488163 -0.043315 0.817309 11.00000 0.01440 0.01318 = 0.01805 -0.00036 -0.00253 -0.00531 AFIX 43 H5A 2 0.423871 -0.084356 0.815748 11.00000 -1.20000 AFIX 0 C6 1 0.492710 0.060886 0.748383 11.00000 0.01381 0.01418 = 0.01808 -0.00236 -0.00320 -0.00358 C7 1 0.712038 0.217498 0.600658 11.00000 0.02492 0.01910 = 0.01709 0.00105 -0.00465 -0.01238 C8 1 0.610618 0.230135 0.680818 11.00000 0.01749 0.01554 = 0.01776 0.00360 -0.00737 -0.00844 C9 1 0.541902 0.355979 0.692382 11.00000 0.02087 0.01662 = 0.02139 0.00212 -0.00607 -0.00768 AFIX 43 H9A 2 0.469189 0.380351 0.744964 11.00000 -1.20000 AFIX 0 C10 1 0.590113 0.437097 0.621443 11.00000 0.02414 0.01801 = 0.02235 -0.00005 -0.00798 -0.00958 C11 1 0.808481 0.101885 0.564974 11.00000 0.04200 0.02481 = 0.02830 -0.00819 0.00481 -0.01366 AFIX 137 H11A 2 0.783545 0.031058 0.606594 11.00000 -1.50000 H11B 2 0.911209 0.090141 0.564276 11.00000 -1.50000 H11C 2 0.793861 0.108728 0.500678 11.00000 -1.50000 AFIX 0 C12 1 0.546905 0.574402 0.609401 11.00000 0.03467 0.01793 = 0.03352 0.00126 -0.00995 -0.01125 AFIX 137 H12A 2 0.447410 0.607028 0.643618 11.00000 -1.50000 H12B 2 0.549766 0.611795 0.542016 11.00000 -1.50000 H12C 2 0.615254 0.594263 0.634686 11.00000 -1.50000 AFIX 0 C13 1 0.373983 0.028819 0.629829 11.00000 0.01936 0.01472 = 0.01820 0.00220 -0.00514 -0.00571 C14 1 0.398104 0.104224 0.675165 11.00000 0.01476 0.01471 = 0.01419 0.00348 -0.00222 -0.00635 C15 1 0.312410 0.231119 0.647518 11.00000 0.01940 0.01350 = 0.02036 0.00143 -0.00512 -0.00762 AFIX 43 H15A 2 0.315766 0.295826 0.672024 11.00000 -1.20000 AFIX 0 C16 1 0.226294 0.251121 0.583593 11.00000 0.01936 0.01409 = 0.01953 0.00115 -0.00491 -0.00587 C17 1 0.437332 -0.108601 0.636222 11.00000 0.03047 0.01595 = 0.02784 -0.00259 -0.00942 -0.00623 AFIX 137 H17A 2 0.531884 -0.140014 0.658174 11.00000 -1.50000 H17B 2 0.451442 -0.127845 0.573689 11.00000 -1.50000 H17C 2 0.370035 -0.147675 0.680979 11.00000 -1.50000 AFIX 0 C18 1 0.120025 0.369159 0.542398 11.00000 0.02405 0.01733 = 0.02772 0.00272 -0.01092 -0.00473 AFIX 137 H18A 2 0.120475 0.436930 0.567844 11.00000 -1.50000 H18B 2 0.021551 0.362817 0.558828 11.00000 -1.50000 H18C 2 0.148095 0.385433 0.473404 11.00000 -1.50000 AFIX 0 C19 1 0.797428 -0.019158 1.009312 11.00000 0.01137 0.01851 = 0.01867 -0.00157 -0.00051 -0.00329 C20 1 0.892443 -0.096132 1.080776 11.00000 0.01387 0.02053 = 0.01780 0.00147 -0.00314 -0.00706 C21 1 0.911253 -0.039476 1.145890 11.00000 0.01347 0.02132 = 0.02285 -0.00192 0.00038 -0.00645 C22 1 0.989649 -0.110898 1.218485 11.00000 0.01972 0.03655 = 0.02044 -0.00542 -0.00177 -0.01307 AFIX 43 H22A 2 0.999250 -0.072558 1.263891 11.00000 -1.20000 AFIX 0 C23 1 1.053306 -0.236374 1.225101 11.00000 0.02056 0.03338 = 0.03005 0.01010 -0.01061 -0.01088 AFIX 43 H23A 2 1.106716 -0.284627 1.274954 11.00000 -1.20000 AFIX 0 C24 1 1.039649 -0.292556 1.159116 11.00000 0.02455 0.02141 = 0.04075 0.00411 -0.01258 -0.00702 AFIX 43 H24A 2 1.085453 -0.379211 1.162978 11.00000 -1.20000 AFIX 0 C25 1 0.960172 -0.223550 1.088107 11.00000 0.02157 0.02277 = 0.03209 -0.00327 -0.00912 -0.00737 AFIX 43 H25A 2 0.951143 -0.263107 1.043303 11.00000 -1.20000 AFIX 0 C26 1 0.657084 -0.300656 0.982643 11.00000 0.01701 0.01692 = 0.01641 -0.00454 -0.00351 -0.00331 C27 1 0.613907 -0.403738 1.045464 11.00000 0.02117 0.01442 = 0.01662 0.00019 -0.00558 -0.00542 C28 1 0.724612 -0.517763 1.070315 11.00000 0.02123 0.01939 = 0.02302 -0.00409 -0.00680 -0.00439 C29 1 0.686900 -0.618991 1.125848 11.00000 0.02984 0.01383 = 0.03009 0.00026 -0.01142 -0.00511 AFIX 43 H29A 2 0.761372 -0.695149 1.142935 11.00000 -1.20000 AFIX 0 C30 1 0.542788 -0.608872 1.155803 11.00000 0.03461 0.01905 = 0.02587 0.00206 -0.00851 -0.01301 AFIX 43 H30A 2 0.517761 -0.678807 1.192671 11.00000 -1.20000 AFIX 0 C31 1 0.432430 -0.497775 1.133095 11.00000 0.02434 0.02461 = 0.02791 -0.00162 -0.00292 -0.01060 AFIX 43 H31A 2 0.332596 -0.491531 1.155116 11.00000 -1.20000 AFIX 0 C32 1 0.467993 -0.396968 1.078725 11.00000 0.02245 0.01607 = 0.02381 -0.00030 -0.00594 -0.00425 AFIX 43 H32A 2 0.391959 -0.321170 1.063423 11.00000 -1.20000 AFIX 0 C100 1 0.015237 0.328323 0.246467 11.00000 0.02661 0.03838 = 0.02546 -0.00870 -0.00348 -0.00676 AFIX 13 H10A 2 0.029873 0.351870 0.175849 11.00000 -1.20000 AFIX 0 PART 1 CL11 6 0.171568 0.332112 0.277446 21.00000 0.03101 0.04340 = 0.03982 -0.00573 -0.01361 -0.01804 CL12 6 -0.139436 0.446729 0.284719 21.00000 0.02270 0.07739 = 0.04565 -0.04561 0.00672 -0.00735 CL13 6 -0.003745 0.187487 0.270495 21.00000 0.07593 0.02960 = 0.09653 -0.01744 -0.03441 -0.01284 PART 2 CL21 6 0.171986 0.305220 0.290797 -21.00000 0.03699 0.16150 = 0.07226 -0.04829 -0.01855 -0.01261 CL22 6 -0.125665 0.457732 0.276260 -21.00000 0.06653 0.02822 = 0.05341 -0.01119 -0.02226 0.00230 CL23 6 -0.044421 0.200198 0.304513 -21.00000 0.12469 0.03010 = 0.06302 0.00296 -0.03596 -0.02810 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM MK1101 in P-1, KOEHLER/KHUSNIYAROV, MAK66org REM R1 = 0.0460 for 4936 Fo > 4sig(Fo) and 0.0739 for all 6808 data REM 431 parameters refined using 16 restraints END ; data_aw1101 _database_code_depnum_ccdc_archive 'CCDC 850436' #TrackingRef '17768_web_deposit_cif_file_2_FrankW.Heinemann_1360922652.CCDC850435_36.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 N2 Ni O6 S2, 2(C16 H36 N), 2(H2 O)' _chemical_formula_sum 'C54 H92 N4 Ni O8 S2' _chemical_formula_weight 1048.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall -P2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.6821(2) _cell_length_b 29.3828(4) _cell_length_c 15.8815(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.8330(10) _cell_angle_gamma 90.00 _cell_volume 5601.18(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9982 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 24.85 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.475 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2008' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 83.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72307 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.10 _reflns_number_total 11761 _reflns_number_gt 8378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some apparent short intermolecular H...H and O...O distances are due to the heavily disordered cations and water molecules. Both tetrabutyl ammonium cations were disordered. Distance restraints as well as SIMU restraints were applied in the refinement of the disordered cations. The compound crystallized with a total of two water molecules that were distributed over four sites. No hydrogen atoms were included for these water locations and SIMU as well as ISOR restraints were applied. ; _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^)+(0.0610P)^2^+5.0891P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11761 _refine_ls_number_parameters 817 _refine_ls_number_restraints 387 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0518 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1250 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.31450(3) 1.130379(11) 0.36789(2) 0.03845(11) Uani 1 1 d . . . S1 S 0.08562(8) 0.86576(3) 0.13957(6) 0.0578(2) Uani 1 1 d . . . S2 S 0.40412(8) 0.93153(3) -0.03101(5) 0.0568(2) Uani 1 1 d . . . N1 N 0.24339(17) 1.07572(7) 0.35085(14) 0.0367(5) Uani 1 1 d . . . N2 N 0.39157(17) 1.10841(7) 0.29778(15) 0.0371(5) Uani 1 1 d . . . O1 O 0.22451(16) 1.14535(7) 0.43832(13) 0.0472(5) Uani 1 1 d . . . O2 O 0.0938(2) 1.11402(9) 0.48618(16) 0.0673(7) Uani 1 1 d . . . O3 O 0.11472(15) 1.03376(7) 0.39462(13) 0.0453(5) Uani 1 1 d . . . O4 O 0.39997(17) 1.18370(6) 0.37825(13) 0.0468(5) Uani 1 1 d . . . O5 O 0.5355(2) 1.21171(7) 0.33244(16) 0.0609(6) Uani 1 1 d . . . O6 O 0.53390(18) 1.12768(7) 0.24309(16) 0.0530(5) Uani 1 1 d . . . C1 C 0.1596(2) 1.11264(11) 0.4438(2) 0.0485(7) Uani 1 1 d . . . C2 C 0.1691(2) 1.06860(10) 0.39256(18) 0.0395(6) Uani 1 1 d . . . C3 C 0.4716(2) 1.18120(9) 0.3360(2) 0.0459(7) Uani 1 1 d . . . C4 C 0.4704(2) 1.13525(9) 0.28566(19) 0.0420(6) Uani 1 1 d . . . C5 C 0.2758(2) 1.04590(9) 0.29470(17) 0.0355(6) Uani 1 1 d . . . C6 C 0.3593(2) 1.06443(8) 0.26344(17) 0.0355(6) Uani 1 1 d . . . C7 C 0.3959(2) 1.03974(9) 0.20366(17) 0.0376(6) Uani 1 1 d . . . H7 H 0.4520 1.0521 0.1827 0.045 Uiso 1 1 calc R . . C8 C 0.3508(2) 0.99667(9) 0.17371(18) 0.0387(6) Uani 1 1 d . . . C9 C 0.2706(2) 0.97796(9) 0.20740(18) 0.0385(6) Uani 1 1 d . . . C10 C 0.2347(2) 1.00283(9) 0.26832(18) 0.0379(6) Uani 1 1 d . . . H10 H 0.1815 0.9899 0.2918 0.045 Uiso 1 1 calc R . . C11 C 0.2232(2) 0.93169(9) 0.18428(18) 0.0415(6) Uani 1 1 d . . . C12 C 0.1117(3) 0.92355(10) 0.1545(2) 0.0493(7) Uani 1 1 d . . . C13 C 0.2259(3) 0.85240(10) 0.1749(2) 0.0521(8) Uani 1 1 d . . . C14 C 0.2872(3) 0.89084(10) 0.19497(19) 0.0462(7) Uani 1 1 d . . . H14 H 0.3663 0.8907 0.2146 0.055 Uiso 1 1 calc R . . C15 C 0.0173(3) 0.95706(11) 0.1302(3) 0.0637(9) Uani 1 1 d . . . H15A H -0.0004 0.9656 0.1837 0.096 Uiso 1 1 calc R . . H15B H -0.0483 0.9432 0.0870 0.096 Uiso 1 1 calc R . . H15C H 0.0391 0.9842 0.1040 0.096 Uiso 1 1 calc R . . C16 C 0.2627(4) 0.80348(11) 0.1826(3) 0.0709(11) Uani 1 1 d . . . H16A H 0.3385 0.8016 0.1795 0.106 Uiso 1 1 calc R . . H16B H 0.2121 0.7859 0.1338 0.106 Uiso 1 1 calc R . . H16C H 0.2616 0.7911 0.2396 0.106 Uiso 1 1 calc R . . C17 C 0.3905(2) 0.97296(9) 0.10706(18) 0.0420(6) Uani 1 1 d . . . C18 C 0.3246(3) 0.95616(11) 0.0270(2) 0.0516(7) Uani 1 1 d . . . C19 C 0.5274(3) 0.94393(10) 0.05083(19) 0.0488(7) Uani 1 1 d . . . C20 C 0.5063(2) 0.96603(9) 0.11875(19) 0.0440(7) Uani 1 1 d . . . H20 H 0.5639 0.9761 0.1701 0.053 Uiso 1 1 calc R . . C21 C 0.2003(3) 0.95843(15) -0.0149(2) 0.0727(11) Uani 1 1 d . . . H21A H 0.1677 0.9288 -0.0093 0.109 Uiso 1 1 calc R . . H21B H 0.1818 0.9663 -0.0779 0.109 Uiso 1 1 calc R . . H21C H 0.1702 0.9817 0.0153 0.109 Uiso 1 1 calc R . . C22 C 0.6380(3) 0.93039(12) 0.0438(2) 0.0623(9) Uani 1 1 d . . . H22A H 0.6972 0.9472 0.0880 0.094 Uiso 1 1 calc R . . H22B H 0.6399 0.9375 -0.0160 0.094 Uiso 1 1 calc R . . H22C H 0.6491 0.8976 0.0547 0.094 Uiso 1 1 calc R . . N3 N 0.22551(17) 0.96422(8) 0.61895(16) 0.0414(5) Uani 1 1 d . . . C23 C 0.1419(2) 1.00255(10) 0.6115(2) 0.0459(7) Uani 1 1 d . . . H23A H 0.1323 1.0193 0.5554 0.055 Uiso 1 1 calc R . . H23B H 0.0690 0.9889 0.6073 0.055 Uiso 1 1 calc R . . C24 C 0.1727(2) 1.03647(10) 0.6876(2) 0.0510(7) Uani 1 1 d . . . H24A H 0.2420 1.0526 0.6897 0.061 Uiso 1 1 calc R . . H24B H 0.1858 1.0203 0.7448 0.061 Uiso 1 1 calc R . . C25 C 0.0776(2) 1.07064(11) 0.6735(2) 0.0545(8) Uani 1 1 d . . . H25A H 0.0538 1.0814 0.6111 0.065 Uiso 1 1 calc R . . H25B H 0.0132 1.0552 0.6835 0.065 Uiso 1 1 calc R . . C26 C 0.1107(3) 1.11134(11) 0.7353(3) 0.0655(10) Uani 1 1 d . . . H26A H 0.0460 1.1312 0.7266 0.098 Uiso 1 1 calc R . . H26B H 0.1700 1.1283 0.7221 0.098 Uiso 1 1 calc R . . H26C H 0.1375 1.1008 0.7971 0.098 Uiso 1 1 calc R . . C27 C 0.2337(2) 0.93355(10) 0.69778(19) 0.0449(7) Uani 1 1 d . B . H27A H 0.2882 0.9091 0.6998 0.054 Uiso 1 1 calc R . . H27B H 0.2631 0.9517 0.7530 0.054 Uiso 1 1 calc R . . C28 C 0.1259(3) 0.91186(11) 0.6970(2) 0.0599(9) Uani 1 1 d D . . H28A H 0.0692 0.9357 0.6925 0.072 Uiso 1 1 calc R A 1 H28B H 0.0981 0.8916 0.6446 0.072 Uiso 1 1 calc R A 1 C29 C 0.1437(10) 0.8853(4) 0.7794(6) 0.065(3) Uani 0.417(7) 1 d PDU B 1 H29A H 0.1619 0.9056 0.8319 0.078 Uiso 0.417(7) 1 calc PR B 1 H29B H 0.2052 0.8632 0.7877 0.078 Uiso 0.417(7) 1 calc PR B 1 C30 C 0.0348(9) 0.8609(4) 0.7667(8) 0.101(4) Uani 0.417(7) 1 d PDU B 1 H30A H 0.0405 0.8427 0.8198 0.151 Uiso 0.417(7) 1 calc PR B 1 H30B H 0.0185 0.8408 0.7148 0.151 Uiso 0.417(7) 1 calc PR B 1 H30C H -0.0252 0.8833 0.7573 0.151 Uiso 0.417(7) 1 calc PR B 1 C29A C 0.1437(7) 0.8691(2) 0.7575(5) 0.0549(19) Uani 0.583(7) 1 d PDU B 2 H29C H 0.1977 0.8765 0.8165 0.066 Uiso 0.583(7) 1 calc PR B 2 H29D H 0.0722 0.8610 0.7662 0.066 Uiso 0.583(7) 1 calc PR B 2 C30A C 0.1872(5) 0.82738(18) 0.7187(4) 0.0622(18) Uani 0.583(7) 1 d PDU B 2 H30D H 0.1369 0.8210 0.6586 0.093 Uiso 0.583(7) 1 calc PR B 2 H30E H 0.1904 0.8008 0.7567 0.093 Uiso 0.583(7) 1 calc PR B 2 H30F H 0.2620 0.8339 0.7162 0.093 Uiso 0.583(7) 1 calc PR B 2 C31 C 0.1844(2) 0.93836(10) 0.53139(19) 0.0426(6) Uani 1 1 d . . . H31A H 0.1067 0.9286 0.5219 0.051 Uiso 1 1 calc R . . H31B H 0.1832 0.9595 0.4826 0.051 Uiso 1 1 calc R . . C32 C 0.2524(3) 0.89681(11) 0.5246(2) 0.0502(7) Uani 1 1 d . . . H32A H 0.3307 0.9059 0.5346 0.060 Uiso 1 1 calc R . . H32B H 0.2515 0.8745 0.5711 0.060 Uiso 1 1 calc R . . C33 C 0.2050(3) 0.87506(11) 0.4336(2) 0.0566(8) Uani 1 1 d . . . H33A H 0.2090 0.8971 0.3875 0.068 Uiso 1 1 calc R . . H33B H 0.1255 0.8676 0.4226 0.068 Uiso 1 1 calc R . . C34 C 0.2676(4) 0.83209(13) 0.4259(3) 0.0769(11) Uani 1 1 d . . . H34A H 0.2333 0.8185 0.3670 0.115 Uiso 1 1 calc R . . H34B H 0.2646 0.8104 0.4719 0.115 Uiso 1 1 calc R . . H34C H 0.3455 0.8397 0.4337 0.115 Uiso 1 1 calc R . . C35 C 0.3414(2) 0.98278(10) 0.6352(2) 0.0473(7) Uani 1 1 d . C . H35A H 0.3665 0.9969 0.6950 0.057 Uiso 1 1 calc R . . H35B H 0.3916 0.9568 0.6365 0.057 Uiso 1 1 calc R . . C36 C 0.3561(2) 1.01690(11) 0.5702(2) 0.0545(8) Uani 1 1 d D . . H36A H 0.2992 1.0411 0.5603 0.065 Uiso 0.865(2) 1 calc PR C 1 H36B H 0.3478 1.0020 0.5125 0.065 Uiso 0.865(2) 1 calc PR C 1 H36C H 0.3276 1.0460 0.5857 0.065 Uiso 0.135(2) 1 calc PR C 2 H36D H 0.3035 1.0078 0.5117 0.065 Uiso 0.135(2) 1 calc PR C 2 C37 C 0.4738(2) 1.03740(13) 0.6093(2) 0.0463(8) Uani 0.865(2) 1 d PDU C 1 H37A H 0.4804 1.0525 0.6665 0.056 Uiso 0.865(2) 1 calc PR C 1 H37B H 0.5296 1.0126 0.6215 0.056 Uiso 0.865(2) 1 calc PR C 1 C38 C 0.4992(3) 1.07166(14) 0.5470(3) 0.0525(10) Uani 0.865(2) 1 d PDU C 1 H38A H 0.5758 1.0827 0.5731 0.079 Uiso 0.865(2) 1 calc PR C 1 H38B H 0.4474 1.0974 0.5381 0.079 Uiso 0.865(2) 1 calc PR C 1 H38C H 0.4906 1.0571 0.4897 0.079 Uiso 0.865(2) 1 calc PR C 1 C37A C 0.4662(12) 1.0288(6) 0.5532(16) 0.046(4) Uani 0.135(2) 1 d PDU C 2 H37C H 0.4558 1.0295 0.4887 0.055 Uiso 0.135(2) 1 calc PR C 2 H37D H 0.5254 1.0067 0.5825 0.055 Uiso 0.135(2) 1 calc PR C 2 C38A C 0.4951(19) 1.0768(7) 0.595(2) 0.073(6) Uani 0.135(2) 1 d PDU C 2 H38D H 0.5719 1.0845 0.5993 0.109 Uiso 0.135(2) 1 calc PR C 2 H38E H 0.4875 1.0770 0.6543 0.109 Uiso 0.135(2) 1 calc PR C 2 H38F H 0.4441 1.0992 0.5572 0.109 Uiso 0.135(2) 1 calc PR C 2 N4 N 0.6689(3) 0.77227(8) 0.95107(17) 0.0590(7) Uani 1 1 d D . . C39 C 0.5593(4) 0.79653(12) 0.9167(2) 0.0588(10) Uani 0.865(2) 1 d PDU C 1 H39A H 0.5344 0.7958 0.8509 0.071 Uiso 0.865(2) 1 calc PR C 1 H39B H 0.5709 0.8288 0.9352 0.071 Uiso 0.865(2) 1 calc PR C 1 C40 C 0.4674(4) 0.77746(17) 0.9472(3) 0.0770(14) Uani 0.865(2) 1 d PDU C 1 H40A H 0.4407 0.7487 0.9148 0.092 Uiso 0.865(2) 1 calc PR C 1 H40B H 0.4986 0.7700 1.0113 0.092 Uiso 0.865(2) 1 calc PR C 1 C41 C 0.3742(5) 0.80719(17) 0.9345(4) 0.0996(16) Uani 0.865(2) 1 d PDU C 1 H41A H 0.3492 0.8163 0.8711 0.120 Uiso 0.865(2) 1 calc PR C 1 H41B H 0.4029 0.8350 0.9694 0.120 Uiso 0.865(2) 1 calc PR C 1 C42 C 0.2739(6) 0.7936(3) 0.9554(7) 0.101(2) Uani 0.865(2) 1 d PDU C 1 H42A H 0.2312 0.8207 0.9599 0.151 Uiso 0.865(2) 1 calc PR C 1 H42B H 0.2958 0.7771 1.0121 0.151 Uiso 0.865(2) 1 calc PR C 1 H42C H 0.2279 0.7738 0.9081 0.151 Uiso 0.865(2) 1 calc PR C 1 C39A C 0.5781(16) 0.7729(9) 0.9963(16) 0.075(4) Uani 0.135(2) 1 d PDU C 2 H39C H 0.5638 0.7406 1.0065 0.090 Uiso 0.135(2) 1 calc PR C 2 H39D H 0.6141 0.7863 1.0560 0.090 Uiso 0.135(2) 1 calc PR C 2 C40A C 0.465(2) 0.7949(12) 0.962(2) 0.074(3) Uani 0.135(2) 1 d PDU C 2 H40C H 0.4786 0.8274 0.9525 0.088 Uiso 0.135(2) 1 calc PR C 2 H40D H 0.4286 0.7819 0.9019 0.088 Uiso 0.135(2) 1 calc PR C 2 C41A C 0.380(2) 0.7946(11) 1.005(2) 0.084(4) Uani 0.135(2) 1 d PDU C 2 H41C H 0.4077 0.8142 1.0588 0.100 Uiso 0.135(2) 1 calc PR C 2 H41D H 0.3765 0.7632 1.0269 0.100 Uiso 0.135(2) 1 calc PR C 2 C42A C 0.266(3) 0.8089(16) 0.957(4) 0.080(7) Uani 0.135(2) 1 d PDU C 2 H42D H 0.2227 0.8104 0.9986 0.119 Uiso 0.135(2) 1 calc PR C 2 H42E H 0.2308 0.7868 0.9102 0.119 Uiso 0.135(2) 1 calc PR C 2 H42F H 0.2665 0.8389 0.9307 0.119 Uiso 0.135(2) 1 calc PR C 2 C43 C 0.6572(4) 0.72250(11) 0.9247(2) 0.0531(9) Uani 0.865(2) 1 d PDU C 1 H43A H 0.6012 0.7086 0.9481 0.064 Uiso 0.865(2) 1 calc PR C 1 H43B H 0.7293 0.7073 0.9545 0.064 Uiso 0.865(2) 1 calc PR C 1 C44 C 0.6237(3) 0.71233(11) 0.8257(2) 0.0521(9) Uani 0.865(2) 1 d PDU C 1 H44A H 0.5564 0.7301 0.7936 0.062 Uiso 0.865(2) 1 calc PR C 1 H44B H 0.6845 0.7215 0.8028 0.062 Uiso 0.865(2) 1 calc PR C 1 C45 C 0.6001(4) 0.66194(12) 0.8094(3) 0.0520(9) Uani 0.865(2) 1 d PDU C 1 H45A H 0.5349 0.6534 0.8275 0.062 Uiso 0.865(2) 1 calc PR C 1 H45B H 0.6650 0.6441 0.8457 0.062 Uiso 0.865(2) 1 calc PR C 1 C46 C 0.5762(4) 0.65107(17) 0.7099(3) 0.0665(13) Uani 0.865(2) 1 d PDU C 1 H46A H 0.5555 0.6189 0.6990 0.100 Uiso 0.865(2) 1 calc PR C 1 H46B H 0.6430 0.6571 0.6936 0.100 Uiso 0.865(2) 1 calc PR C 1 H46C H 0.5149 0.6702 0.6740 0.100 Uiso 0.865(2) 1 calc PR C 1 C43A C 0.612(2) 0.7441(6) 0.8713(10) 0.057(3) Uani 0.135(2) 1 d PDU C 2 H43C H 0.6651 0.7396 0.8376 0.068 Uiso 0.135(2) 1 calc PR C 2 H43D H 0.5482 0.7615 0.8328 0.068 Uiso 0.135(2) 1 calc PR C 2 C44A C 0.571(2) 0.6983(7) 0.8881(13) 0.058(3) Uani 0.135(2) 1 d PDU C 2 H44C H 0.6352 0.6795 0.9231 0.070 Uiso 0.135(2) 1 calc PR C 2 H44D H 0.5201 0.7019 0.9232 0.070 Uiso 0.135(2) 1 calc PR C 2 C45A C 0.512(2) 0.6750(8) 0.8024(15) 0.065(4) Uani 0.135(2) 1 d PDU C 2 H45C H 0.4534 0.6954 0.7652 0.078 Uiso 0.135(2) 1 calc PR C 2 H45D H 0.4757 0.6472 0.8148 0.078 Uiso 0.135(2) 1 calc PR C 2 C46A C 0.590(3) 0.6621(13) 0.751(2) 0.076(6) Uani 0.135(2) 1 d PDU C 2 H46D H 0.5858 0.6293 0.7398 0.114 Uiso 0.135(2) 1 calc PR C 2 H46E H 0.6670 0.6702 0.7862 0.114 Uiso 0.135(2) 1 calc PR C 2 H46F H 0.5690 0.6785 0.6944 0.114 Uiso 0.135(2) 1 calc PR C 2 C47 C 0.7497(4) 0.79398(12) 0.9062(2) 0.0590(10) Uani 0.865(2) 1 d PDU C 1 H47A H 0.8184 0.7754 0.9229 0.071 Uiso 0.865(2) 1 calc PR C 1 H47B H 0.7146 0.7911 0.8410 0.071 Uiso 0.865(2) 1 calc PR C 1 C48 C 0.7829(4) 0.84194(16) 0.9258(3) 0.0671(12) Uani 0.865(2) 1 d PDU C 1 H48A H 0.8155 0.8459 0.9910 0.081 Uiso 0.865(2) 1 calc PR C 1 H48B H 0.7157 0.8614 0.9050 0.081 Uiso 0.865(2) 1 calc PR C 1 C49 C 0.8662(5) 0.85751(16) 0.8821(3) 0.0787(15) Uani 0.865(2) 1 d PDU C 1 H49A H 0.9319 0.8372 0.9025 0.094 Uiso 0.865(2) 1 calc PR C 1 H49B H 0.8325 0.8530 0.8172 0.094 Uiso 0.865(2) 1 calc PR C 1 C50 C 0.9061(5) 0.90474(17) 0.8973(3) 0.0837(17) Uani 0.865(2) 1 d PDU C 1 H50A H 0.9486 0.9121 0.8573 0.125 Uiso 0.865(2) 1 calc PR C 1 H50B H 0.9540 0.9083 0.9592 0.125 Uiso 0.865(2) 1 calc PR C 1 H50C H 0.8423 0.9254 0.8855 0.125 Uiso 0.865(2) 1 calc PR C 1 C47A C 0.682(2) 0.8230(4) 0.9465(16) 0.064(4) Uani 0.135(2) 1 d PDU C 2 H47C H 0.6359 0.8333 0.8864 0.077 Uiso 0.135(2) 1 calc PR C 2 H47D H 0.6502 0.8372 0.9897 0.077 Uiso 0.135(2) 1 calc PR C 2 C48A C 0.793(2) 0.8398(11) 0.9637(19) 0.069(4) Uani 0.135(2) 1 d PDU C 2 H48C H 0.8416 0.8128 0.9722 0.082 Uiso 0.135(2) 1 calc PR C 2 H48D H 0.8130 0.8556 1.0218 0.082 Uiso 0.135(2) 1 calc PR C 2 C49A C 0.823(3) 0.8697(8) 0.9036(17) 0.068(4) Uani 0.135(2) 1 d PDU C 2 H49C H 0.7555 0.8759 0.8526 0.081 Uiso 0.135(2) 1 calc PR C 2 H49D H 0.8757 0.8530 0.8802 0.081 Uiso 0.135(2) 1 calc PR C 2 C50A C 0.876(3) 0.9150(8) 0.938(2) 0.062(6) Uani 0.135(2) 1 d PDU C 2 H50D H 0.9499 0.9167 0.9308 0.092 Uiso 0.135(2) 1 calc PR C 2 H50E H 0.8835 0.9180 1.0010 0.092 Uiso 0.135(2) 1 calc PR C 2 H50F H 0.8290 0.9396 0.9042 0.092 Uiso 0.135(2) 1 calc PR C 2 C51 C 0.7155(4) 0.77583(12) 1.0505(2) 0.0555(10) Uani 0.865(2) 1 d PU C 1 H51A H 0.7071 0.8078 1.0667 0.067 Uiso 0.865(2) 1 calc PR C 1 H51B H 0.6681 0.7571 1.0756 0.067 Uiso 0.865(2) 1 calc PR C 1 C51A C 0.7382(16) 0.7417(5) 1.0238(11) 0.064(5) Uani 0.135(2) 1 d PDU C 2 H51C H 0.6878 0.7271 1.0521 0.097 Uiso 0.135(2) 1 calc PR C 2 H51D H 0.7690 0.7173 0.9957 0.097 Uiso 0.135(2) 1 calc PR C 2 C52 C 0.8329(3) 0.76245(12) 1.0960(2) 0.0662(10) Uani 1 1 d D . . H52A H 0.8829 0.7849 1.0817 0.079 Uiso 0.865(2) 1 calc PR C 1 H52B H 0.8468 0.7324 1.0733 0.079 Uiso 0.865(2) 1 calc PR C 1 H52C H 0.8284 0.7954 1.0825 0.079 Uiso 0.135(2) 1 calc PR C 2 H52D H 0.9008 0.7515 1.0845 0.079 Uiso 0.135(2) 1 calc PR C 2 C53 C 0.8602(4) 0.75977(14) 1.1950(2) 0.0762(11) Uani 1 1 d . C . H53A H 0.8357 0.7885 1.2155 0.091 Uiso 1 1 calc R . . H53B H 0.8153 0.7349 1.2083 0.091 Uiso 1 1 calc R . . C54 C 0.9766(4) 0.75212(17) 1.2476(3) 0.0943(14) Uani 1 1 d . . . H54A H 0.9842 0.7524 1.3110 0.142 Uiso 1 1 calc R C . H54B H 1.0228 0.7763 1.2352 0.142 Uiso 1 1 calc R . . H54C H 1.0008 0.7226 1.2320 0.142 Uiso 1 1 calc R . . O7 O -0.0046(12) 0.8019(4) 0.4831(9) 0.126(3) Uani 0.397(7) 1 d PU D 1 O8 O 0.2725(7) 0.8059(2) 0.6854(6) 0.159(3) Uani 0.603(7) 1 d PU E 1 O9 O -0.0821(5) 0.80080(16) 0.4320(4) 0.1042(16) Uani 0.751(7) 1 d PU F 2 O10 O 0.0869(14) 0.8016(6) 0.5701(12) 0.128(3) Uani 0.249(6) 1 d PU G 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 Ni1 0.04107(19) 0.03424(19) 0.0359(2) -0.00276(15) 0.00670(14) -0.00359(14) S1 0.0716(5) 0.0392(4) 0.0605(5) -0.0069(4) 0.0183(4) -0.0130(4) S2 0.0865(6) 0.0454(4) 0.0408(4) -0.0048(3) 0.0239(4) -0.0077(4) N1 0.0350(11) 0.0362(12) 0.0352(12) -0.0030(10) 0.0063(9) -0.0018(9) N2 0.0384(11) 0.0316(11) 0.0374(12) 0.0037(9) 0.0070(9) 0.0006(9) O1 0.0526(11) 0.0437(11) 0.0449(12) -0.0126(9) 0.0152(9) -0.0083(9) O2 0.0714(15) 0.0742(16) 0.0679(16) -0.0348(13) 0.0387(13) -0.0257(12) O3 0.0365(10) 0.0472(11) 0.0507(12) -0.0094(9) 0.0120(9) -0.0098(8) O4 0.0562(12) 0.0350(10) 0.0453(12) -0.0029(9) 0.0109(9) -0.0063(9) O5 0.0735(15) 0.0368(11) 0.0727(16) 0.0081(11) 0.0240(12) -0.0128(10) O6 0.0567(12) 0.0365(11) 0.0750(15) 0.0123(10) 0.0339(11) 0.0044(9) C1 0.0469(16) 0.0542(18) 0.0431(17) -0.0131(14) 0.0126(13) -0.0085(14) C2 0.0336(13) 0.0445(15) 0.0357(15) -0.0054(12) 0.0047(11) -0.0021(11) C3 0.0510(16) 0.0363(15) 0.0447(17) 0.0087(13) 0.0075(13) -0.0018(13) C4 0.0437(15) 0.0322(14) 0.0444(16) 0.0134(12) 0.0061(12) 0.0024(11) C5 0.0340(13) 0.0339(13) 0.0325(14) 0.0018(11) 0.0021(10) 0.0030(10) C6 0.0346(13) 0.0306(13) 0.0355(14) 0.0051(11) 0.0032(10) 0.0024(10) C7 0.0378(13) 0.0361(14) 0.0358(15) 0.0057(12) 0.0075(11) 0.0041(11) C8 0.0427(14) 0.0347(14) 0.0341(15) 0.0041(11) 0.0058(11) 0.0065(11) C9 0.0421(14) 0.0316(13) 0.0359(15) 0.0020(11) 0.0045(11) 0.0035(11) C10 0.0363(13) 0.0345(14) 0.0382(15) 0.0037(12) 0.0055(11) 0.0010(10) C11 0.0517(16) 0.0338(14) 0.0368(15) 0.0003(12) 0.0111(12) 0.0011(12) C12 0.0564(18) 0.0367(15) 0.0491(18) -0.0003(13) 0.0092(14) -0.0049(13) C13 0.078(2) 0.0350(15) 0.0496(19) -0.0024(14) 0.0293(16) 0.0014(15) C14 0.0601(18) 0.0386(15) 0.0420(17) 0.0027(13) 0.0193(14) 0.0047(13) C15 0.0488(18) 0.0472(18) 0.082(2) 0.0018(17) 0.0023(16) -0.0057(14) C16 0.111(3) 0.0365(17) 0.083(3) -0.0009(17) 0.056(2) 0.0052(18) C17 0.0573(17) 0.0309(14) 0.0358(15) 0.0060(12) 0.0119(13) 0.0046(12) C18 0.0640(19) 0.0464(17) 0.0431(17) -0.0023(14) 0.0153(14) -0.0069(14) C19 0.075(2) 0.0350(15) 0.0389(16) 0.0102(13) 0.0215(15) 0.0126(14) C20 0.0551(17) 0.0365(15) 0.0379(16) 0.0074(12) 0.0115(13) 0.0112(12) C21 0.066(2) 0.099(3) 0.043(2) -0.0029(19) 0.0047(16) -0.017(2) C22 0.088(2) 0.060(2) 0.0476(19) 0.0125(16) 0.0342(18) 0.0306(18) N3 0.0289(10) 0.0422(13) 0.0494(14) -0.0063(11) 0.0074(10) 0.0023(9) C23 0.0286(13) 0.0427(16) 0.0612(19) -0.0056(14) 0.0073(12) 0.0033(11) C24 0.0375(15) 0.0462(17) 0.065(2) -0.0107(15) 0.0099(14) 0.0002(12) C25 0.0437(16) 0.0478(17) 0.071(2) -0.0078(16) 0.0170(15) 0.0043(13) C26 0.0557(19) 0.0461(18) 0.098(3) -0.0140(18) 0.0291(19) 0.0026(15) C27 0.0415(15) 0.0468(16) 0.0437(16) -0.0047(13) 0.0097(12) 0.0052(12) C28 0.0472(17) 0.0526(19) 0.081(2) 0.0068(17) 0.0213(16) 0.0044(14) C29 0.063(4) 0.102(7) 0.034(5) -0.021(5) 0.021(4) -0.003(6) C30 0.088(7) 0.114(8) 0.098(7) 0.046(6) 0.026(6) -0.018(6) C29A 0.065(3) 0.074(5) 0.033(4) -0.008(3) 0.025(3) -0.016(4) C30A 0.083(4) 0.044(3) 0.072(4) -0.006(3) 0.041(3) -0.009(3) C31 0.0333(13) 0.0477(16) 0.0434(16) -0.0043(13) 0.0077(11) 0.0011(11) C32 0.0505(17) 0.0532(18) 0.0458(17) -0.0021(14) 0.0139(13) 0.0111(14) C33 0.063(2) 0.057(2) 0.0472(19) -0.0059(15) 0.0142(15) 0.0096(15) C34 0.104(3) 0.067(2) 0.060(2) -0.0071(19) 0.027(2) 0.024(2) C35 0.0272(13) 0.0495(17) 0.0595(19) -0.0011(14) 0.0061(12) 0.0015(11) C36 0.0298(14) 0.0605(19) 0.068(2) 0.0049(16) 0.0083(13) 0.0026(13) C37 0.0292(15) 0.063(2) 0.041(2) -0.0013(18) 0.0037(14) 0.0008(14) C38 0.0387(18) 0.067(2) 0.046(2) -0.003(2) 0.0066(17) -0.0055(16) C37A 0.027(6) 0.057(7) 0.049(8) 0.005(7) 0.008(7) 0.002(6) C38A 0.056(10) 0.075(10) 0.064(11) -0.023(11) -0.015(10) 0.021(9) N4 0.092(2) 0.0289(12) 0.0452(15) -0.0017(11) 0.0065(14) -0.0020(13) C39 0.095(3) 0.0302(17) 0.044(2) 0.0010(15) 0.0119(19) 0.0034(17) C40 0.102(3) 0.067(3) 0.052(3) 0.013(2) 0.011(2) 0.006(3) C41 0.120(4) 0.060(3) 0.117(4) 0.023(3) 0.037(3) 0.020(3) C42 0.133(5) 0.096(6) 0.074(4) 0.011(5) 0.035(3) 0.022(4) C39A 0.104(6) 0.047(6) 0.058(6) 0.017(6) 0.005(6) 0.003(6) C40A 0.103(5) 0.047(5) 0.067(5) 0.017(5) 0.022(5) 0.009(5) C41A 0.111(7) 0.059(7) 0.083(7) 0.021(7) 0.033(7) 0.012(7) C42A 0.118(11) 0.054(12) 0.078(11) 0.030(11) 0.046(10) 0.007(10) C43 0.087(3) 0.0286(16) 0.043(2) -0.0040(15) 0.0199(18) -0.0046(16) C44 0.076(2) 0.0390(18) 0.0426(19) -0.0044(15) 0.0213(17) -0.0093(16) C45 0.072(2) 0.0419(19) 0.051(2) -0.0145(18) 0.0318(19) -0.0154(17) C46 0.072(3) 0.075(3) 0.063(3) -0.039(2) 0.037(2) -0.031(2) C43A 0.081(6) 0.037(6) 0.048(6) 0.003(5) 0.017(6) -0.011(6) C44A 0.079(6) 0.041(5) 0.051(5) -0.001(5) 0.016(5) -0.009(5) C45A 0.081(7) 0.054(7) 0.059(7) -0.004(6) 0.020(7) -0.014(7) C46A 0.072(10) 0.079(11) 0.077(12) -0.030(11) 0.024(11) -0.019(10) C47 0.098(3) 0.0419(19) 0.0345(19) 0.0007(15) 0.0173(18) -0.0083(18) C48 0.103(3) 0.055(2) 0.027(2) 0.015(2) -0.002(2) -0.007(2) C49 0.094(3) 0.057(3) 0.058(3) 0.015(2) -0.013(2) -0.013(2) C50 0.094(4) 0.067(3) 0.058(3) 0.018(2) -0.019(3) -0.020(3) C47A 0.100(6) 0.043(6) 0.037(6) 0.009(6) 0.004(6) -0.012(6) C48A 0.103(6) 0.046(5) 0.041(6) 0.014(6) 0.000(6) -0.007(5) C49A 0.094(6) 0.053(6) 0.041(6) 0.023(6) -0.001(6) -0.010(6) C50A 0.079(12) 0.055(11) 0.053(12) 0.000(10) 0.024(10) -0.001(10) C51 0.093(3) 0.0347(18) 0.0345(19) -0.0019(15) 0.0140(18) 0.0013(18) C51A 0.097(9) 0.041(8) 0.050(8) 0.003(8) 0.016(8) 0.015(8) C52 0.096(3) 0.0419(18) 0.055(2) 0.0088(16) 0.0155(19) -0.0031(17) C53 0.103(3) 0.067(2) 0.050(2) 0.0014(18) 0.014(2) -0.007(2) C54 0.097(3) 0.102(4) 0.078(3) 0.024(3) 0.020(2) 0.033(3) O7 0.138(5) 0.112(4) 0.135(5) -0.006(4) 0.053(4) -0.004(4) O8 0.198(6) 0.100(5) 0.239(7) 0.000(4) 0.155(6) -0.004(4) O9 0.120(3) 0.088(3) 0.119(4) -0.020(3) 0.058(3) -0.013(3) O10 0.133(5) 0.119(5) 0.135(5) -0.001(4) 0.048(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.819(2) . ? Ni1 N2 1.821(2) . ? Ni1 O4 1.8819(19) . ? Ni1 O1 1.890(2) . ? S1 C13 1.729(4) . ? S1 C12 1.732(3) . ? S2 C19 1.719(3) . ? S2 C18 1.729(3) . ? N1 C2 1.331(3) . ? N1 C5 1.403(3) . ? N2 C4 1.335(3) . ? N2 C6 1.411(3) . ? O1 C1 1.287(4) . ? O2 C1 1.230(4) . ? O3 C2 1.241(3) . ? O4 C3 1.294(4) . ? O5 C3 1.222(3) . ? O6 C4 1.228(4) . ? C1 C2 1.554(4) . ? C3 C4 1.566(4) . ? C5 C10 1.381(4) . ? C5 C6 1.415(4) . ? C6 C7 1.388(4) . ? C7 C8 1.407(4) . ? C7 H7 0.9500 . ? C8 C9 1.406(4) . ? C8 C17 1.484(4) . ? C9 C10 1.400(4) . ? C9 C11 1.484(4) . ? C10 H10 0.9500 . ? C11 C12 1.360(4) . ? C11 C14 1.428(4) . ? C12 C15 1.500(4) . ? C13 C14 1.350(4) . ? C13 C16 1.504(4) . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.368(4) . ? C17 C20 1.434(4) . ? C18 C21 1.502(5) . ? C19 C20 1.358(4) . ? C19 C22 1.496(4) . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? N3 C35 1.509(3) . ? N3 C27 1.519(4) . ? N3 C31 1.521(4) . ? N3 C23 1.525(3) . ? C23 C24 1.516(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.529(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.518(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.504(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.478(9) . ? C28 C29A 1.553(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.510(9) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C29A C30A 1.551(7) . ? C29A H29C 0.9900 . ? C29A H29D 0.9900 . ? C30A H30D 0.9800 . ? C30A H30E 0.9800 . ? C30A H30F 0.9800 . ? C31 C32 1.519(4) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.516(4) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.518(5) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.494(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.542(4) . ? C36 C37A 1.545(10) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 H36C 0.9900 . ? C36 H36D 0.9900 . ? C37 C38 1.516(5) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C37A C38A 1.549(10) . ? C37A H37C 0.9900 . ? C37A H37D 0.9900 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? N4 C43A 1.489(10) . ? N4 C39 1.499(5) . ? N4 C51 1.500(4) . ? N4 C51A 1.502(10) . ? N4 C47A 1.504(10) . ? N4 C43 1.515(4) . ? N4 C39A 1.542(9) . ? N4 C47 1.561(5) . ? C39 C40 1.508(7) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.431(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.469(10) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C39A C40A 1.510(19) . ? C39A H39C 0.9900 . ? C39A H39D 0.9900 . ? C40A C41A 1.45(2) . ? C40A H40C 0.9900 . ? C40A H40D 0.9900 . ? C41A C42A 1.47(2) . ? C41A H41C 0.9900 . ? C41A H41D 0.9900 . ? C42A H42D 0.9800 . ? C42A H42E 0.9800 . ? C42A H42F 0.9800 . ? C43 C44 1.520(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.516(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.543(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C43A C44A 1.496(17) . ? C43A H43C 0.9900 . ? C43A H43D 0.9900 . ? C44A C45A 1.492(18) . ? C44A H44C 0.9900 . ? C44A H44D 0.9900 . ? C45A C46A 1.521(19) . ? C45A H45C 0.9900 . ? C45A H45D 0.9900 . ? C46A H46D 0.9800 . ? C46A H46E 0.9800 . ? C46A H46F 0.9800 . ? C47 C48 1.475(6) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.510(7) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.470(6) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C47A C48A 1.432(19) . ? C47A H47C 0.9900 . ? C47A H47D 0.9900 . ? C48A C49A 1.441(19) . ? C48A H48C 0.9900 . ? C48A H48D 0.9900 . ? C49A C50A 1.508(9) . ? C49A H49C 0.9900 . ? C49A H49D 0.9900 . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? C51 C52 1.483(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C51A C52 1.496(10) . ? C51A H51C 0.9900 . ? C51A H51D 0.9900 . ? C52 C53 1.499(5) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C52 H52C 0.9900 . ? C52 H52D 0.9900 . ? C53 C54 1.460(6) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 N2 86.22(10) . . ? N1 Ni1 O4 172.76(10) . . ? N2 Ni1 O4 86.61(9) . . ? N1 Ni1 O1 85.90(9) . . ? N2 Ni1 O1 172.12(9) . . ? O4 Ni1 O1 101.27(9) . . ? C13 S1 C12 92.72(15) . . ? C19 S2 C18 93.03(15) . . ? C2 N1 C5 128.2(2) . . ? C2 N1 Ni1 117.45(18) . . ? C5 N1 Ni1 114.39(17) . . ? C4 N2 C6 128.5(2) . . ? C4 N2 Ni1 116.96(19) . . ? C6 N2 Ni1 114.53(17) . . ? C1 O1 Ni1 112.82(18) . . ? C3 O4 Ni1 112.85(18) . . ? O2 C1 O1 125.0(3) . . ? O2 C1 C2 119.7(3) . . ? O1 C1 C2 115.3(3) . . ? O3 C2 N1 129.2(3) . . ? O3 C2 C1 122.4(2) . . ? N1 C2 C1 108.5(2) . . ? O5 C3 O4 124.7(3) . . ? O5 C3 C4 120.4(3) . . ? O4 C3 C4 114.9(2) . . ? O6 C4 N2 128.8(3) . . ? O6 C4 C3 122.5(2) . . ? N2 C4 C3 108.7(3) . . ? C10 C5 N1 127.3(2) . . ? C10 C5 C6 119.9(2) . . ? N1 C5 C6 112.9(2) . . ? C7 C6 N2 128.6(2) . . ? C7 C6 C5 119.5(2) . . ? N2 C6 C5 111.9(2) . . ? C6 C7 C8 120.8(3) . . ? C6 C7 H7 119.6 . . ? C8 C7 H7 119.6 . . ? C9 C8 C7 119.2(2) . . ? C9 C8 C17 122.8(2) . . ? C7 C8 C17 118.0(2) . . ? C10 C9 C8 119.7(2) . . ? C10 C9 C11 117.0(2) . . ? C8 C9 C11 123.3(2) . . ? C5 C10 C9 120.9(3) . . ? C5 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C14 112.4(3) . . ? C12 C11 C9 122.7(3) . . ? C14 C11 C9 124.8(3) . . ? C11 C12 C15 128.9(3) . . ? C11 C12 S1 110.5(2) . . ? C15 C12 S1 120.5(2) . . ? C14 C13 C16 129.9(3) . . ? C14 C13 S1 109.9(2) . . ? C16 C13 S1 120.2(3) . . ? C13 C14 C11 114.4(3) . . ? C13 C14 H14 122.8 . . ? C11 C14 H14 122.8 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C20 111.2(3) . . ? C18 C17 C8 125.9(3) . . ? C20 C17 C8 122.9(3) . . ? C17 C18 C21 129.4(3) . . ? C17 C18 S2 111.1(2) . . ? C21 C18 S2 119.5(2) . . ? C20 C19 C22 128.1(3) . . ? C20 C19 S2 109.7(2) . . ? C22 C19 S2 122.2(2) . . ? C19 C20 C17 114.9(3) . . ? C19 C20 H20 122.5 . . ? C17 C20 H20 122.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C35 N3 C27 105.7(2) . . ? C35 N3 C31 111.4(2) . . ? C27 N3 C31 111.7(2) . . ? C35 N3 C23 111.1(2) . . ? C27 N3 C23 111.3(2) . . ? C31 N3 C23 105.9(2) . . ? C24 C23 N3 115.5(2) . . ? C24 C23 H23A 108.4 . . ? N3 C23 H23A 108.4 . . ? C24 C23 H23B 108.4 . . ? N3 C23 H23B 108.4 . . ? H23A C23 H23B 107.5 . . ? C23 C24 C25 109.1(2) . . ? C23 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? C23 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C26 C25 C24 112.4(3) . . ? C26 C25 H25A 109.1 . . ? C24 C25 H25A 109.1 . . ? C26 C25 H25B 109.1 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 N3 115.1(2) . . ? C28 C27 H27A 108.5 . . ? N3 C27 H27A 108.5 . . ? C28 C27 H27B 108.5 . . ? N3 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? C29 C28 C27 109.8(5) . . ? C27 C28 C29A 112.8(4) . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? C29A C28 H28A 125.1 . . ? C29 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? C29A C28 H28B 88.6 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 105.1(7) . . ? C28 C29 H29A 110.7 . . ? C30 C29 H29A 110.7 . . ? C28 C29 H29B 110.7 . . ? C30 C29 H29B 110.7 . . ? H29A C29 H29B 108.8 . . ? C30A C29A C28 113.2(5) . . ? C30A C29A H29C 108.9 . . ? C28 C29A H29C 108.9 . . ? C30A C29A H29D 108.9 . . ? C28 C29A H29D 108.9 . . ? H29C C29A H29D 107.8 . . ? C29A C30A H30D 109.5 . . ? C29A C30A H30E 109.5 . . ? H30D C30A H30E 109.5 . . ? C29A C30A H30F 109.5 . . ? H30D C30A H30F 109.5 . . ? H30E C30A H30F 109.5 . . ? C32 C31 N3 115.5(2) . . ? C32 C31 H31A 108.4 . . ? N3 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? N3 C31 H31B 108.4 . . ? H31A C31 H31B 107.5 . . ? C33 C32 C31 110.3(2) . . ? C33 C32 H32A 109.6 . . ? C31 C32 H32A 109.6 . . ? C33 C32 H32B 109.6 . . ? C31 C32 H32B 109.6 . . ? H32A C32 H32B 108.1 . . ? C32 C33 C34 111.8(3) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 107.9 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 N3 117.2(2) . . ? C36 C35 H35A 108.0 . . ? N3 C35 H35A 108.0 . . ? C36 C35 H35B 108.0 . . ? N3 C35 H35B 108.0 . . ? H35A C35 H35B 107.3 . . ? C35 C36 C37 107.7(3) . . ? C35 C36 C37A 126.5(9) . . ? C35 C36 H36A 110.2 . . ? C37 C36 H36A 110.2 . . ? C37A C36 H36A 117.6 . . ? C35 C36 H36B 110.2 . . ? C37 C36 H36B 110.2 . . ? C37A C36 H36B 76.7 . . ? H36A C36 H36B 108.5 . . ? C35 C36 H36C 105.7 . . ? C37 C36 H36C 86.9 . . ? C37A C36 H36C 105.7 . . ? H36B C36 H36C 132.3 . . ? C35 C36 H36D 105.7 . . ? C37 C36 H36D 139.0 . . ? C37A C36 H36D 105.7 . . ? H36A C36 H36D 79.0 . . ? H36C C36 H36D 106.1 . . ? C38 C37 C36 112.2(3) . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37B 109.2 . . ? C36 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C36 C37A C38A 103.5(12) . . ? C36 C37A H37C 111.1 . . ? C38A C37A H37C 111.1 . . ? C36 C37A H37D 111.1 . . ? C38A C37A H37D 111.1 . . ? H37C C37A H37D 109.0 . . ? C37A C38A H38D 109.5 . . ? C37A C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C37A C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C43A N4 C39 79.7(11) . . ? C43A N4 C51 148.4(8) . . ? C39 N4 C51 110.8(3) . . ? C43A N4 C51A 108.8(11) . . ? C39 N4 C51A 143.9(11) . . ? C51 N4 C51A 45.4(8) . . ? C43A N4 C47A 122.7(12) . . ? C39 N4 C47A 67.2(9) . . ? C51 N4 C47A 88.3(9) . . ? C51A N4 C47A 125.8(10) . . ? C39 N4 C43 111.2(3) . . ? C51 N4 C43 109.2(2) . . ? C51A N4 C43 67.5(6) . . ? C47A N4 C43 161.1(10) . . ? C43A N4 C39A 100.2(15) . . ? C39 N4 C39A 54.6(9) . . ? C51 N4 C39A 67.0(10) . . ? C51A N4 C39A 89.3(14) . . ? C47A N4 C39A 96.8(14) . . ? C43 N4 C39A 96.9(11) . . ? C43A N4 C47 92.6(9) . . ? C39 N4 C47 107.9(3) . . ? C51 N4 C47 111.0(3) . . ? C51A N4 C47 106.7(10) . . ? C47A N4 C47 58.4(10) . . ? C43 N4 C47 106.7(3) . . ? C39A N4 C47 155.1(10) . . ? N4 C39 C40 115.3(3) . . ? N4 C39 H39A 108.4 . . ? C40 C39 H39A 108.4 . . ? N4 C39 H39B 108.4 . . ? C40 C39 H39B 108.4 . . ? H39A C39 H39B 107.5 . . ? C41 C40 C39 114.6(4) . . ? C41 C40 H40A 108.6 . . ? C39 C40 H40A 108.6 . . ? C41 C40 H40B 108.6 . . ? C39 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C40 C41 C42 122.5(5) . . ? C40 C41 H41A 106.7 . . ? C42 C41 H41A 106.7 . . ? C40 C41 H41B 106.7 . . ? C42 C41 H41B 106.7 . . ? H41A C41 H41B 106.6 . . ? C40A C39A N4 127.1(19) . . ? C40A C39A H39C 105.5 . . ? N4 C39A H39C 105.5 . . ? C40A C39A H39D 105.5 . . ? N4 C39A H39D 105.5 . . ? H39C C39A H39D 106.1 . . ? C41A C40A C39A 126(2) . . ? C41A C40A H40C 105.8 . . ? C39A C40A H40C 105.8 . . ? C41A C40A H40D 105.8 . . ? C39A C40A H40D 105.8 . . ? H40C C40A H40D 106.2 . . ? C40A C41A C42A 121(3) . . ? C40A C41A H41C 107.2 . . ? C42A C41A H41C 107.2 . . ? C40A C41A H41D 107.2 . . ? C42A C41A H41D 107.2 . . ? H41C C41A H41D 106.8 . . ? C41A C42A H42D 109.5 . . ? C41A C42A H42E 109.5 . . ? H42D C42A H42E 109.5 . . ? C41A C42A H42F 109.5 . . ? H42D C42A H42F 109.5 . . ? H42E C42A H42F 109.5 . . ? N4 C43 C44 116.4(3) . . ? N4 C43 H43A 108.2 . . ? C44 C43 H43A 108.2 . . ? N4 C43 H43B 108.2 . . ? C44 C43 H43B 108.2 . . ? H43A C43 H43B 107.3 . . ? C45 C44 C43 110.0(3) . . ? C45 C44 H44A 109.7 . . ? C43 C44 H44A 109.7 . . ? C45 C44 H44B 109.7 . . ? C43 C44 H44B 109.7 . . ? H44A C44 H44B 108.2 . . ? C44 C45 C46 109.8(3) . . ? C44 C45 H45A 109.7 . . ? C46 C45 H45A 109.7 . . ? C44 C45 H45B 109.7 . . ? C46 C45 H45B 109.7 . . ? H45A C45 H45B 108.2 . . ? N4 C43A C44A 116.6(14) . . ? N4 C43A H43C 108.1 . . ? C44A C43A H43C 108.1 . . ? N4 C43A H43D 108.1 . . ? C44A C43A H43D 108.1 . . ? H43C C43A H43D 107.3 . . ? C45A C44A C43A 110.6(15) . . ? C45A C44A H44C 109.5 . . ? C43A C44A H44C 109.5 . . ? C45A C44A H44D 109.5 . . ? C43A C44A H44D 109.5 . . ? H44C C44A H44D 108.1 . . ? C44A C45A C46A 112(2) . . ? C44A C45A H45C 109.1 . . ? C46A C45A H45C 109.1 . . ? C44A C45A H45D 109.1 . . ? C46A C45A H45D 109.1 . . ? H45C C45A H45D 107.9 . . ? C45A C46A H46D 109.5 . . ? C45A C46A H46E 109.5 . . ? H46D C46A H46E 109.5 . . ? C45A C46A H46F 109.5 . . ? H46D C46A H46F 109.5 . . ? H46E C46A H46F 109.5 . . ? C48 C47 N4 118.6(3) . . ? C48 C47 H47A 107.7 . . ? N4 C47 H47A 107.7 . . ? C48 C47 H47B 107.7 . . ? N4 C47 H47B 107.7 . . ? H47A C47 H47B 107.1 . . ? C47 C48 C49 112.8(4) . . ? C47 C48 H48A 109.0 . . ? C49 C48 H48A 109.0 . . ? C47 C48 H48B 109.0 . . ? C49 C48 H48B 109.0 . . ? H48A C48 H48B 107.8 . . ? C50 C49 C48 117.8(5) . . ? C50 C49 H49A 107.9 . . ? C48 C49 H49A 107.9 . . ? C50 C49 H49B 107.9 . . ? C48 C49 H49B 107.9 . . ? H49A C49 H49B 107.2 . . ? C48A C47A N4 116.5(19) . . ? C48A C47A H47C 108.2 . . ? N4 C47A H47C 108.2 . . ? C48A C47A H47D 108.2 . . ? N4 C47A H47D 108.2 . . ? H47C C47A H47D 107.3 . . ? C47A C48A C49A 123(2) . . ? C47A C48A H48C 106.6 . . ? C49A C48A H48C 106.6 . . ? C47A C48A H48D 106.6 . . ? C49A C48A H48D 106.6 . . ? H48C C48A H48D 106.5 . . ? C48A C49A C50A 119(2) . . ? C48A C49A H49C 107.6 . . ? C50A C49A H49C 107.6 . . ? C48A C49A H49D 107.6 . . ? C50A C49A H49D 107.6 . . ? H49C C49A H49D 107.0 . . ? C49A C50A H50D 109.5 . . ? C49A C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? C49A C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C52 C51 N4 119.2(3) . . ? C52 C51 H51A 107.5 . . ? N4 C51 H51A 107.5 . . ? C52 C51 H51B 107.5 . . ? N4 C51 H51B 107.5 . . ? H51A C51 H51B 107.0 . . ? C52 C51A N4 118.2(9) . . ? C52 C51A H51C 107.8 . . ? N4 C51A H51C 107.8 . . ? C52 C51A H51D 107.8 . . ? N4 C51A H51D 107.8 . . ? H51C C51A H51D 107.1 . . ? C51 C52 C51A 45.8(8) . . ? C51 C52 C53 112.4(3) . . ? C51A C52 C53 129.7(10) . . ? C51 C52 H52A 109.1 . . ? C51A C52 H52A 120.6 . . ? C53 C52 H52A 109.1 . . ? C51 C52 H52B 109.1 . . ? C51A C52 H52B 63.4 . . ? C53 C52 H52B 109.1 . . ? H52A C52 H52B 107.9 . . ? C51 C52 H52C 69.9 . . ? C51A C52 H52C 104.9 . . ? C53 C52 H52C 104.9 . . ? H52A C52 H52C 45.2 . . ? H52B C52 H52C 142.9 . . ? C51 C52 H52D 142.4 . . ? C51A C52 H52D 104.9 . . ? C53 C52 H52D 104.9 . . ? H52A C52 H52D 61.1 . . ? H52B C52 H52D 51.2 . . ? H52C C52 H52D 105.8 . . ? C54 C53 C52 117.2(4) . . ? C54 C53 H53A 108.0 . . ? C52 C53 H53A 108.0 . . ? C54 C53 H53B 108.0 . . ? C52 C53 H53B 108.0 . . ? H53A C53 H53B 107.2 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 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 N2 Ni1 N1 C2 177.6(2) . . . . ? O1 Ni1 N1 C2 -2.31(19) . . . . ? N2 Ni1 N1 C5 -1.85(18) . . . . ? O1 Ni1 N1 C5 178.22(18) . . . . ? N1 Ni1 N2 C4 -177.3(2) . . . . ? O4 Ni1 N2 C4 1.72(19) . . . . ? N1 Ni1 N2 C6 2.49(17) . . . . ? O4 Ni1 N2 C6 -178.52(18) . . . . ? N1 Ni1 O1 C1 1.1(2) . . . . ? O4 Ni1 O1 C1 -177.9(2) . . . . ? N2 Ni1 O4 C3 -1.20(19) . . . . ? O1 Ni1 O4 C3 178.59(19) . . . . ? Ni1 O1 C1 O2 179.5(3) . . . . ? Ni1 O1 C1 C2 0.2(3) . . . . ? C5 N1 C2 O3 3.1(5) . . . . ? Ni1 N1 C2 O3 -176.3(2) . . . . ? C5 N1 C2 C1 -177.9(2) . . . . ? Ni1 N1 C2 C1 2.8(3) . . . . ? O2 C1 C2 O3 -2.1(4) . . . . ? O1 C1 C2 O3 177.2(3) . . . . ? O2 C1 C2 N1 178.8(3) . . . . ? O1 C1 C2 N1 -1.9(3) . . . . ? Ni1 O4 C3 O5 179.3(2) . . . . ? Ni1 O4 C3 C4 0.5(3) . . . . ? C6 N2 C4 O6 -1.2(5) . . . . ? Ni1 N2 C4 O6 178.5(2) . . . . ? C6 N2 C4 C3 178.6(2) . . . . ? Ni1 N2 C4 C3 -1.7(3) . . . . ? O5 C3 C4 O6 1.6(4) . . . . ? O4 C3 C4 O6 -179.5(3) . . . . ? O5 C3 C4 N2 -178.1(3) . . . . ? O4 C3 C4 N2 0.7(3) . . . . ? C2 N1 C5 C10 2.1(4) . . . . ? Ni1 N1 C5 C10 -178.5(2) . . . . ? C2 N1 C5 C6 -178.6(2) . . . . ? Ni1 N1 C5 C6 0.8(3) . . . . ? C4 N2 C6 C7 -5.2(4) . . . . ? Ni1 N2 C6 C7 175.1(2) . . . . ? C4 N2 C6 C5 177.1(2) . . . . ? Ni1 N2 C6 C5 -2.6(3) . . . . ? C10 C5 C6 C7 2.6(4) . . . . ? N1 C5 C6 C7 -176.8(2) . . . . ? C10 C5 C6 N2 -179.5(2) . . . . ? N1 C5 C6 N2 1.1(3) . . . . ? N2 C6 C7 C8 -177.4(2) . . . . ? C5 C6 C7 C8 0.1(4) . . . . ? C6 C7 C8 C9 -2.2(4) . . . . ? C6 C7 C8 C17 177.6(2) . . . . ? C7 C8 C9 C10 1.6(4) . . . . ? C17 C8 C9 C10 -178.2(2) . . . . ? C7 C8 C9 C11 -176.2(2) . . . . ? C17 C8 C9 C11 4.1(4) . . . . ? N1 C5 C10 C9 176.1(2) . . . . ? C6 C5 C10 C9 -3.2(4) . . . . ? C8 C9 C10 C5 1.1(4) . . . . ? C11 C9 C10 C5 179.0(2) . . . . ? C10 C9 C11 C12 53.6(4) . . . . ? C8 C9 C11 C12 -128.7(3) . . . . ? C10 C9 C11 C14 -122.8(3) . . . . ? C8 C9 C11 C14 55.0(4) . . . . ? C14 C11 C12 C15 -176.3(3) . . . . ? C9 C11 C12 C15 6.9(5) . . . . ? C14 C11 C12 S1 -0.1(3) . . . . ? C9 C11 C12 S1 -176.8(2) . . . . ? C13 S1 C12 C11 0.7(3) . . . . ? C13 S1 C12 C15 177.3(3) . . . . ? C12 S1 C13 C14 -1.1(2) . . . . ? C12 S1 C13 C16 176.7(3) . . . . ? C16 C13 C14 C11 -176.3(3) . . . . ? S1 C13 C14 C11 1.3(3) . . . . ? C12 C11 C14 C13 -0.8(4) . . . . ? C9 C11 C14 C13 175.9(3) . . . . ? C9 C8 C17 C18 53.5(4) . . . . ? C7 C8 C17 C18 -126.2(3) . . . . ? C9 C8 C17 C20 -128.4(3) . . . . ? C7 C8 C17 C20 51.9(4) . . . . ? C20 C17 C18 C21 -176.0(3) . . . . ? C8 C17 C18 C21 2.3(5) . . . . ? C20 C17 C18 S2 1.1(3) . . . . ? C8 C17 C18 S2 179.4(2) . . . . ? C19 S2 C18 C17 -0.6(2) . . . . ? C19 S2 C18 C21 176.8(3) . . . . ? C18 S2 C19 C20 -0.1(2) . . . . ? C18 S2 C19 C22 178.9(3) . . . . ? C22 C19 C20 C17 -178.1(3) . . . . ? S2 C19 C20 C17 0.8(3) . . . . ? C18 C17 C20 C19 -1.3(4) . . . . ? C8 C17 C20 C19 -179.6(2) . . . . ? C35 N3 C23 C24 -52.3(3) . . . . ? C27 N3 C23 C24 65.1(3) . . . . ? C31 N3 C23 C24 -173.4(3) . . . . ? N3 C23 C24 C25 -176.3(3) . . . . ? C23 C24 C25 C26 -168.0(3) . . . . ? C35 N3 C27 C28 178.6(3) . . . . ? C31 N3 C27 C28 -60.2(3) . . . . ? C23 N3 C27 C28 57.9(3) . . . . ? N3 C27 C28 C29 -176.6(5) . . . . ? N3 C27 C28 C29A 159.7(4) . . . . ? C27 C28 C29 C30 -173.6(8) . . . . ? C29A C28 C29 C30 -71.6(17) . . . . ? C29 C28 C29A C30A -159(2) . . . . ? C27 C28 C29A C30A -72.6(7) . . . . ? C35 N3 C31 C32 61.7(3) . . . . ? C27 N3 C31 C32 -56.1(3) . . . . ? C23 N3 C31 C32 -177.4(2) . . . . ? N3 C31 C32 C33 -178.3(3) . . . . ? C31 C32 C33 C34 -177.3(3) . . . . ? C27 N3 C35 C36 -175.9(3) . . . . ? C31 N3 C35 C36 62.7(3) . . . . ? C23 N3 C35 C36 -55.1(3) . . . . ? N3 C35 C36 C37 169.5(3) . . . . ? N3 C35 C36 C37A -158.4(10) . . . . ? C35 C36 C37 C38 178.2(3) . . . . ? C37A C36 C37 C38 48.2(14) . . . . ? C35 C36 C37A C38A -108.0(16) . . . . ? C37 C36 C37A C38A -42.9(14) . . . . ? C43A N4 C39 C40 85.8(9) . . . . ? C51 N4 C39 C40 -63.2(4) . . . . ? C51A N4 C39 C40 -22.1(10) . . . . ? C47A N4 C39 C40 -142.0(11) . . . . ? C43 N4 C39 C40 58.4(4) . . . . ? C39A N4 C39 C40 -24.8(14) . . . . ? C47 N4 C39 C40 175.2(3) . . . . ? N4 C39 C40 C41 164.0(4) . . . . ? C39 C40 C41 C42 176.4(6) . . . . ? C43A N4 C39A C40A -66(3) . . . . ? C39 N4 C39A C40A 3(2) . . . . ? C51 N4 C39A C40A 144(3) . . . . ? C51A N4 C39A C40A -175(3) . . . . ? C47A N4 C39A C40A 59(3) . . . . ? C43 N4 C39A C40A -108(3) . . . . ? C47 N4 C39A C40A 54(5) . . . . ? N4 C39A C40A C41A 179(3) . . . . ? C39A C40A C41A C42A -167(4) . . . . ? C43A N4 C43 C44 21.3(16) . . . . ? C39 N4 C43 C44 64.4(4) . . . . ? C51 N4 C43 C44 -173.1(3) . . . . ? C51A N4 C43 C44 -154.7(12) . . . . ? C47A N4 C43 C44 -17(3) . . . . ? C39A N4 C43 C44 118.9(10) . . . . ? C47 N4 C43 C44 -53.1(4) . . . . ? N4 C43 C44 C45 -172.2(3) . . . . ? C43 C44 C45 C46 -175.1(4) . . . . ? C39 N4 C43A C44A -106(2) . . . . ? C51 N4 C43A C44A 7(4) . . . . ? C51A N4 C43A C44A 38(3) . . . . ? C47A N4 C43A C44A -160(2) . . . . ? C43 N4 C43A C44A 34.0(15) . . . . ? C39A N4 C43A C44A -55(2) . . . . ? C47 N4 C43A C44A 147(2) . . . . ? N4 C43A C44A C45A 177(2) . . . . ? C43A C44A C45A C46A 68(3) . . . . ? C43A N4 C47 C48 144.7(11) . . . . ? C39 N4 C47 C48 64.7(4) . . . . ? C51 N4 C47 C48 -56.8(4) . . . . ? C51A N4 C47 C48 -104.8(8) . . . . ? C47A N4 C47 C48 17.3(11) . . . . ? C43 N4 C47 C48 -175.7(3) . . . . ? C39A N4 C47 C48 23(3) . . . . ? N4 C47 C48 C49 176.6(3) . . . . ? C47 C48 C49 C50 -179.7(4) . . . . ? C43A N4 C47A C48A -112(2) . . . . ? C39 N4 C47A C48A -172(2) . . . . ? C51 N4 C47A C48A 74(2) . . . . ? C51A N4 C47A C48A 47(3) . . . . ? C43 N4 C47A C48A -83(4) . . . . ? C39A N4 C47A C48A 141(2) . . . . ? C47 N4 C47A C48A -41.7(18) . . . . ? N4 C47A C48A C49A 127(3) . . . . ? C47A C48A C49A C50A 123(3) . . . . ? C43A N4 C51 C52 88(2) . . . . ? C39 N4 C51 C52 -167.7(3) . . . . ? C51A N4 C51 C52 45.3(12) . . . . ? C47A N4 C51 C52 -102.9(10) . . . . ? C43 N4 C51 C52 69.5(4) . . . . ? C39A N4 C51 C52 159.0(11) . . . . ? C47 N4 C51 C52 -47.8(4) . . . . ? C43A N4 C51A C52 157.8(19) . . . . ? C39 N4 C51A C52 -103.9(17) . . . . ? C51 N4 C51A C52 -44.2(12) . . . . ? C47A N4 C51A C52 -4(3) . . . . ? C43 N4 C51A C52 161(2) . . . . ? C39A N4 C51A C52 -102(2) . . . . ? C47 N4 C51A C52 59(2) . . . . ? N4 C51 C52 C51A -45.2(12) . . . . ? N4 C51 C52 C53 -169.4(3) . . . . ? N4 C51A C52 C51 44.5(12) . . . . ? N4 C51A C52 C53 127.8(14) . . . . ? C51 C52 C53 C54 -173.0(4) . . . . ? C51A C52 C53 C54 136.6(11) . . . . ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.640 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.055 _iucr_refine_instructions_details ; TITL AW1101 in P2(1)/c, WITT/KHUSNIYAROV, aw_NiL1 CELL 0.71073 12.6821 29.3828 15.8815 90.000 108.833 90.000 ZERR 4.00 0.0002 0.0004 0.0002 0.000 0.001 0.000 LATT 1 SYMM -x, y+1/2, -z+1/2 SFAC C H N O S Ni UNIT 216 368 16 32 8 4 L.S. 16 SADI N4 C39 N4 C39A SIMU 0.01 0.02 C29 > C30A SIMU 0.01 0.02 C37 > C38A SIMU 0.01 0.02 C39 > C42A SIMU 0.01 0.02 C43 > C46A SIMU 0.01 0.02 C47 > C50A SIMU 0.01 0.02 C51 C51A ISOR 0.005 0.01 O7 > O9 ISOR 0.003 0.006 O10 SIMU 0.005 0.01 O7 > O10 DFIX 1.54 0.01 C37 C38 C37A C38A C36 C37 C36 C37A C28 C29 C28 C29A DFIX 1.54 0.01 C29 C30 C29A C30A C52 C51A C49A C50A DFIX 1.52 0.01 N4 C39A N4 C43A N4 C47A N4 C51A ACTA 50 SADI C36 C38 C36 C38A TEMP -173.000 SIZE 0.53 0.26 0.22 BOND .5 $h CONF WPDB -1 LIST 4 FMAP 2 PLAN 20 SUMP 1.0 0.001 1.0 4 1.0 5 SUMP 1.0 0.001 1.0 6 1.0 7 WGHT 0.061000 5.089100 FVAR 0.07361 0.42056 0.86553 0.75079 0.24938 0.39684 0.60222 FVAR 0.52453 NI1 6 0.314497 1.130379 0.367892 11.00000 0.04106 0.03422 = 0.03592 -0.00276 0.00669 -0.00359 S1 5 0.085631 0.865758 0.139569 11.00000 0.07157 0.03919 = 0.06043 -0.00690 0.01833 -0.01302 S2 5 0.404119 0.931530 -0.031009 11.00000 0.08649 0.04542 = 0.04075 -0.00475 0.02391 -0.00768 N1 3 0.243394 1.075711 0.350851 11.00000 0.03500 0.03617 = 0.03527 -0.00299 0.00634 -0.00181 N2 3 0.391566 1.108406 0.297786 11.00000 0.03846 0.03164 = 0.03740 0.00366 0.00699 0.00055 O1 4 0.224509 1.145347 0.438316 11.00000 0.05263 0.04360 = 0.04497 -0.01260 0.01531 -0.00838 O2 4 0.093828 1.114020 0.486170 11.00000 0.07127 0.07428 = 0.06793 -0.03478 0.03865 -0.02567 O3 4 0.114720 1.033750 0.394622 11.00000 0.03649 0.04722 = 0.05070 -0.00936 0.01195 -0.00985 O4 4 0.399959 1.183698 0.378244 11.00000 0.05614 0.03497 = 0.04531 -0.00300 0.01086 -0.00633 O5 4 0.535482 1.211718 0.332433 11.00000 0.07360 0.03669 = 0.07289 0.00802 0.02413 -0.01280 O6 4 0.533902 1.127679 0.243090 11.00000 0.05673 0.03654 = 0.07497 0.01224 0.03392 0.00438 C1 1 0.159592 1.112638 0.443778 11.00000 0.04684 0.05436 = 0.04304 -0.01310 0.01253 -0.00857 C2 1 0.169126 1.068606 0.392562 11.00000 0.03362 0.04444 = 0.03565 -0.00536 0.00470 -0.00213 C3 1 0.471574 1.181192 0.335961 11.00000 0.05100 0.03630 = 0.04470 0.00861 0.00750 -0.00181 C4 1 0.470376 1.135265 0.285658 11.00000 0.04358 0.03213 = 0.04439 0.01339 0.00606 0.00233 C5 1 0.275829 1.045906 0.294688 11.00000 0.03395 0.03397 = 0.03249 0.00180 0.00216 0.00299 C6 1 0.359299 1.064430 0.263437 11.00000 0.03466 0.03058 = 0.03557 0.00505 0.00321 0.00236 C7 1 0.395862 1.039743 0.203663 11.00000 0.03780 0.03620 = 0.03582 0.00561 0.00761 0.00414 AFIX 43 H7 2 0.452009 1.052096 0.182711 11.00000 -1.20000 AFIX 0 C8 1 0.350862 0.996676 0.173713 11.00000 0.04264 0.03478 = 0.03406 0.00407 0.00571 0.00642 C9 1 0.270597 0.977960 0.207414 11.00000 0.04224 0.03158 = 0.03582 0.00200 0.00452 0.00348 C10 1 0.234738 1.002833 0.268323 11.00000 0.03624 0.03448 = 0.03813 0.00367 0.00547 0.00106 AFIX 43 H10 2 0.181460 0.989918 0.291814 11.00000 -1.20000 AFIX 0 C11 1 0.223193 0.931681 0.184279 11.00000 0.05168 0.03379 = 0.03692 0.00035 0.01109 0.00112 C12 1 0.111664 0.923555 0.154460 11.00000 0.05638 0.03659 = 0.04909 -0.00027 0.00915 -0.00489 C13 1 0.225902 0.852395 0.174921 11.00000 0.07773 0.03493 = 0.04970 -0.00242 0.02924 0.00146 C14 1 0.287179 0.890847 0.194975 11.00000 0.06014 0.03859 = 0.04221 0.00280 0.01942 0.00465 AFIX 43 H14 2 0.366318 0.890744 0.214580 11.00000 -1.20000 AFIX 0 C15 1 0.017330 0.957053 0.130201 11.00000 0.04880 0.04720 = 0.08170 0.00170 0.00238 -0.00568 AFIX 137 H15A 2 -0.000367 0.965653 0.183740 11.00000 -1.50000 H15B 2 -0.048296 0.943171 0.087053 11.00000 -1.50000 H15C 2 0.039033 0.984215 0.103963 11.00000 -1.50000 AFIX 0 C16 1 0.262736 0.803475 0.182611 11.00000 0.11131 0.03634 = 0.08311 -0.00085 0.05624 0.00518 AFIX 137 H16A 2 0.338417 0.801598 0.179232 11.00000 -1.50000 H16B 2 0.211907 0.785838 0.133910 11.00000 -1.50000 H16C 2 0.261882 0.791116 0.239702 11.00000 -1.50000 AFIX 0 C17 1 0.390470 0.972960 0.107061 11.00000 0.05717 0.03080 = 0.03583 0.00605 0.01187 0.00467 C18 1 0.324607 0.956163 0.027042 11.00000 0.06405 0.04633 = 0.04302 -0.00239 0.01527 -0.00687 C19 1 0.527370 0.943935 0.050824 11.00000 0.07472 0.03497 = 0.03890 0.01018 0.02152 0.01255 C20 1 0.506284 0.966031 0.118755 11.00000 0.05516 0.03649 = 0.03786 0.00745 0.01153 0.01114 AFIX 43 H20 2 0.563866 0.976135 0.170132 11.00000 -1.20000 AFIX 0 C21 1 0.200263 0.958439 -0.014878 11.00000 0.06647 0.09898 = 0.04336 -0.00287 0.00467 -0.01720 AFIX 137 H21A 2 0.167680 0.928804 -0.009310 11.00000 -1.50000 H21B 2 0.181836 0.966301 -0.077956 11.00000 -1.50000 H21C 2 0.170155 0.981697 0.015286 11.00000 -1.50000 AFIX 0 C22 1 0.637990 0.930392 0.043786 11.00000 0.08824 0.05995 = 0.04754 0.01246 0.03415 0.03060 AFIX 137 H22A 2 0.697257 0.947184 0.087980 11.00000 -1.50000 H22B 2 0.639951 0.937481 -0.015988 11.00000 -1.50000 H22C 2 0.649192 0.897645 0.054757 11.00000 -1.50000 AFIX 0 N3 3 0.225513 0.964223 0.618958 11.00000 0.02888 0.04210 = 0.04951 -0.00626 0.00735 0.00239 C23 1 0.141889 1.002551 0.611548 11.00000 0.02862 0.04287 = 0.06114 -0.00563 0.00726 0.00337 AFIX 23 H23A 2 0.132335 1.019267 0.555444 11.00000 -1.20000 H23B 2 0.069024 0.988863 0.607316 11.00000 -1.20000 AFIX 0 C24 1 0.172669 1.036464 0.687561 11.00000 0.03754 0.04607 = 0.06490 -0.01075 0.00998 0.00012 AFIX 23 H24A 2 0.241989 1.052618 0.689689 11.00000 -1.20000 H24B 2 0.185796 1.020333 0.744766 11.00000 -1.20000 AFIX 0 C25 1 0.077568 1.070637 0.673452 11.00000 0.04362 0.04796 = 0.07072 -0.00778 0.01688 0.00436 AFIX 23 H25A 2 0.053794 1.081402 0.611054 11.00000 -1.20000 H25B 2 0.013243 1.055199 0.683451 11.00000 -1.20000 AFIX 0 C26 1 0.110710 1.111326 0.735311 11.00000 0.05575 0.04614 = 0.09777 -0.01407 0.02918 0.00253 AFIX 137 H26A 2 0.045936 1.131154 0.726694 11.00000 -1.50000 H26B 2 0.169948 1.128318 0.722035 11.00000 -1.50000 H26C 2 0.137642 1.100773 0.797137 11.00000 -1.50000 AFIX 0 C27 1 0.233680 0.933555 0.697780 11.00000 0.04138 0.04703 = 0.04357 -0.00479 0.00965 0.00526 AFIX 23 H27A 2 0.288258 0.909150 0.699783 11.00000 -1.20000 H27B 2 0.263128 0.951660 0.753000 11.00000 -1.20000 AFIX 0 C28 1 0.125884 0.911858 0.696960 11.00000 0.04721 0.05258 = 0.08053 0.00669 0.02130 0.00445 AFIX 23 H28A 2 0.069267 0.935712 0.692712 11.00000 -1.20000 H28B 2 0.098012 0.891686 0.644506 11.00000 -1.20000 AFIX 0 PART 1 C29 1 0.143861 0.885129 0.779327 21.00000 0.06357 0.10297 = 0.03420 -0.02067 0.02049 -0.00368 AFIX 23 H29A 2 0.162517 0.905369 0.831936 21.00000 -1.20000 H29B 2 0.205107 0.862954 0.787367 21.00000 -1.20000 AFIX 0 C30 1 0.034781 0.860922 0.766702 21.00000 0.08852 0.11489 = 0.09789 0.04599 0.02538 -0.01791 AFIX 137 H30A 2 0.040475 0.842656 0.819621 21.00000 -1.50000 H30B 2 0.017998 0.840994 0.714549 21.00000 -1.50000 H30C 2 -0.024914 0.883409 0.757746 21.00000 -1.50000 AFIX 0 PART 2 C29A 1 0.143580 0.869079 0.757331 -21.00000 0.06447 0.07464 = 0.03250 -0.00759 0.02447 -0.01679 AFIX 23 H29C 2 0.197401 0.876522 0.816389 -21.00000 -1.20000 H29D 2 0.071995 0.860963 0.765956 -21.00000 -1.20000 AFIX 0 C30A 1 0.187172 0.827373 0.718779 -21.00000 0.08111 0.04385 = 0.07236 -0.00640 0.04185 -0.00906 AFIX 137 H30D 2 0.139000 0.821931 0.657567 -21.00000 -1.50000 H30E 2 0.186709 0.800494 0.755193 -21.00000 -1.50000 H30F 2 0.263376 0.833314 0.719194 -21.00000 -1.50000 AFIX 0 PART 0 C31 1 0.184399 0.938364 0.531391 11.00000 0.03322 0.04782 = 0.04331 -0.00428 0.00755 0.00110 AFIX 23 H31A 2 0.106708 0.928575 0.521852 11.00000 -1.20000 H31B 2 0.183209 0.959545 0.482614 11.00000 -1.20000 AFIX 0 C32 1 0.252391 0.896811 0.524597 11.00000 0.05047 0.05320 = 0.04580 -0.00210 0.01390 0.01114 AFIX 23 H32A 2 0.330678 0.905876 0.534598 11.00000 -1.20000 H32B 2 0.251466 0.874515 0.571090 11.00000 -1.20000 AFIX 0 C33 1 0.204944 0.875054 0.433604 11.00000 0.06310 0.05684 = 0.04719 -0.00592 0.01410 0.00960 AFIX 23 H33A 2 0.208989 0.897051 0.387527 11.00000 -1.20000 H33B 2 0.125529 0.867543 0.422634 11.00000 -1.20000 AFIX 0 C34 1 0.267635 0.832087 0.425902 11.00000 0.10381 0.06701 = 0.06010 -0.00713 0.02657 0.02422 AFIX 137 H34A 2 0.233224 0.818445 0.367088 11.00000 -1.50000 H34B 2 0.264700 0.810406 0.471984 11.00000 -1.50000 H34C 2 0.345460 0.839666 0.433660 11.00000 -1.50000 AFIX 0 C35 1 0.341357 0.982767 0.635179 11.00000 0.02719 0.04951 = 0.05942 -0.00112 0.00611 0.00145 AFIX 23 H35A 2 0.366521 0.996844 0.695013 11.00000 -1.20000 H35B 2 0.391549 0.956783 0.636464 11.00000 -1.20000 AFIX 0 C36 1 0.356104 1.016910 0.570195 11.00000 0.02981 0.06035 = 0.06789 0.00484 0.00823 0.00251 PART 1 AFIX 23 H36A 2 0.299175 1.041149 0.560357 31.00000 -1.20000 H36B 2 0.347809 1.002067 0.512447 31.00000 -1.20000 PART 2 AFIX 23 H36C 2 0.327534 1.045999 0.585703 -31.00000 -1.20000 H36D 2 0.303571 1.007783 0.511660 -31.00000 -1.20000 AFIX 0 PART 1 C37 1 0.473841 1.037397 0.609315 31.00000 0.02912 0.06319 = 0.04119 -0.00135 0.00372 0.00089 AFIX 23 H37A 2 0.480423 1.052487 0.666525 31.00000 -1.20000 H37B 2 0.529555 1.012581 0.621502 31.00000 -1.20000 AFIX 0 C38 1 0.499178 1.071658 0.547051 31.00000 0.03856 0.06707 = 0.04648 -0.00263 0.00661 -0.00550 AFIX 137 H38A 2 0.575809 1.082649 0.573114 31.00000 -1.50000 H38B 2 0.447461 1.097357 0.538100 31.00000 -1.50000 H38C 2 0.490637 1.057107 0.489700 31.00000 -1.50000 AFIX 0 PART 2 C37A 1 0.466212 1.028886 0.553286 -31.00000 0.02730 0.05743 = 0.04937 0.00513 0.00765 0.00227 AFIX 23 H37C 2 0.455886 1.029544 0.488790 -31.00000 -1.20000 H37D 2 0.525413 1.006685 0.582576 -31.00000 -1.20000 AFIX 0 C38A 1 0.495109 1.076813 0.595038 -31.00000 0.05568 0.07464 = 0.06330 -0.02294 -0.01466 0.02108 AFIX 137 H38D 2 0.571809 1.084574 0.599279 -31.00000 -1.50000 H38E 2 0.487860 1.076921 0.654633 -31.00000 -1.50000 H38F 2 0.443938 1.099260 0.557613 -31.00000 -1.50000 AFIX 0 PART 0 N4 3 0.668861 0.772269 0.951073 11.00000 0.09176 0.02890 = 0.04508 -0.00172 0.00639 -0.00194 PART 1 C39 1 0.559286 0.796527 0.916689 31.00000 0.09510 0.03032 = 0.04364 0.00102 0.01189 0.00344 AFIX 23 H39A 2 0.534414 0.795796 0.850858 31.00000 -1.20000 H39B 2 0.570868 0.828815 0.935186 31.00000 -1.20000 AFIX 0 C40 1 0.467384 0.777481 0.947267 31.00000 0.10157 0.06723 = 0.05192 0.01267 0.01079 0.00639 AFIX 23 H40A 2 0.440715 0.748743 0.914843 31.00000 -1.20000 H40B 2 0.498617 0.770015 1.011335 31.00000 -1.20000 AFIX 0 C41 1 0.374165 0.807187 0.934519 31.00000 0.12010 0.06052 = 0.11663 0.02331 0.03638 0.02014 AFIX 23 H41A 2 0.349204 0.816302 0.871114 31.00000 -1.20000 H41B 2 0.402894 0.835040 0.969475 31.00000 -1.20000 AFIX 0 C42 1 0.273902 0.793561 0.955395 31.00000 0.13273 0.09616 = 0.07383 0.01055 0.03442 0.02222 AFIX 137 H42A 2 0.231484 0.820738 0.960327 31.00000 -1.50000 H42B 2 0.295724 0.776924 1.011894 31.00000 -1.50000 H42C 2 0.227630 0.773934 0.907884 31.00000 -1.50000 AFIX 0 PART 2 SAME C39 > C42 C39A 1 0.578056 0.772950 0.996264 -31.00000 0.10395 0.04704 = 0.05807 0.01729 0.00497 0.00255 AFIX 23 H39C 2 0.563776 0.740627 1.006481 -31.00000 -1.20000 H39D 2 0.614012 0.786344 1.055864 -31.00000 -1.20000 AFIX 0 C40A 1 0.464673 0.794973 0.961744 -31.00000 0.10313 0.04708 = 0.06666 0.01681 0.02177 0.00910 AFIX 23 H40C 2 0.478571 0.827442 0.952408 -31.00000 -1.20000 H40D 2 0.428650 0.781907 0.901860 -31.00000 -1.20000 AFIX 0 C41A 1 0.380300 0.794627 1.005282 -31.00000 0.11061 0.05905 = 0.08243 0.02048 0.03298 0.01173 AFIX 23 H41C 2 0.407798 0.814164 1.058711 -31.00000 -1.20000 H41D 2 0.376553 0.763211 1.026666 -31.00000 -1.20000 AFIX 0 C42A 1 0.265464 0.808907 0.957292 -31.00000 0.11837 0.05405 = 0.07739 0.02971 0.04596 0.00682 AFIX 137 H42D 2 0.223066 0.810759 0.998985 -31.00000 -1.50000 H42E 2 0.230398 0.786666 0.910673 -31.00000 -1.50000 H42F 2 0.266378 0.838816 0.930225 -31.00000 -1.50000 AFIX 0 PART 1 C43 1 0.657194 0.722500 0.924693 31.00000 0.08732 0.02861 = 0.04271 -0.00398 0.01991 -0.00453 AFIX 23 H43A 2 0.601111 0.708617 0.948044 31.00000 -1.20000 H43B 2 0.729223 0.707251 0.954499 31.00000 -1.20000 AFIX 0 C44 1 0.623749 0.712326 0.825747 31.00000 0.07612 0.03906 = 0.04254 -0.00441 0.02120 -0.00933 AFIX 23 H44A 2 0.556456 0.730085 0.793579 31.00000 -1.20000 H44B 2 0.684559 0.721445 0.802837 31.00000 -1.20000 AFIX 0 C45 1 0.600072 0.661933 0.809445 31.00000 0.07167 0.04193 = 0.05114 -0.01452 0.03180 -0.01541 AFIX 23 H45A 2 0.534968 0.653348 0.827482 31.00000 -1.20000 H45B 2 0.665056 0.644055 0.845680 31.00000 -1.20000 AFIX 0 C46 1 0.576155 0.651074 0.709914 31.00000 0.07233 0.07527 = 0.06310 -0.03949 0.03713 -0.03136 AFIX 137 H46A 2 0.555593 0.618939 0.699002 31.00000 -1.50000 H46B 2 0.642954 0.657195 0.693508 31.00000 -1.50000 H46C 2 0.514734 0.670193 0.674043 31.00000 -1.50000 AFIX 0 PART 2 SAME C43 > C46 C43A 1 0.612447 0.744055 0.871304 -31.00000 0.08116 0.03722 = 0.04789 0.00311 0.01661 -0.01125 AFIX 23 H43C 2 0.665037 0.739606 0.837551 -31.00000 -1.20000 H43D 2 0.548158 0.761500 0.832749 -31.00000 -1.20000 AFIX 0 C44A 1 0.571485 0.698319 0.888097 -31.00000 0.07859 0.04080 = 0.05074 -0.00135 0.01659 -0.00945 AFIX 23 H44C 2 0.635339 0.679447 0.922933 -31.00000 -1.20000 H44D 2 0.520321 0.701891 0.923352 -31.00000 -1.20000 AFIX 0 C45A 1 0.512056 0.675054 0.802365 -31.00000 0.08115 0.05365 = 0.05874 -0.00361 0.01983 -0.01409 AFIX 23 H45C 2 0.453197 0.695447 0.765206 -31.00000 -1.20000 H45D 2 0.475530 0.647232 0.814723 -31.00000 -1.20000 AFIX 0 C46A 1 0.590317 0.662145 0.751038 -31.00000 0.07254 0.07819 = 0.07663 -0.03018 0.02389 -0.01883 AFIX 137 H46D 2 0.585983 0.629277 0.739959 -31.00000 -1.50000 H46E 2 0.666833 0.670399 0.785936 -31.00000 -1.50000 H46F 2 0.568536 0.678445 0.694166 -31.00000 -1.50000 AFIX 0 PART 1 C47 1 0.749656 0.793979 0.906189 31.00000 0.09755 0.04202 = 0.03434 0.00070 0.01709 -0.00827 AFIX 23 H47A 2 0.818457 0.775404 0.922962 31.00000 -1.20000 H47B 2 0.714591 0.791095 0.840980 31.00000 -1.20000 AFIX 0 C48 1 0.782832 0.841932 0.925739 31.00000 0.10270 0.05486 = 0.02718 0.01528 -0.00217 -0.00713 AFIX 23 H48A 2 0.815468 0.845858 0.990939 31.00000 -1.20000 H48B 2 0.715700 0.861415 0.904941 31.00000 -1.20000 AFIX 0 C49 1 0.866224 0.857499 0.882147 31.00000 0.09421 0.05661 = 0.05810 0.01471 -0.01316 -0.01306 AFIX 23 H49A 2 0.931888 0.837199 0.902578 31.00000 -1.20000 H49B 2 0.832532 0.852988 0.817178 31.00000 -1.20000 AFIX 0 C50 1 0.906101 0.904760 0.897294 31.00000 0.09432 0.06704 = 0.05782 0.01760 -0.01956 -0.02044 AFIX 137 H50A 2 0.948476 0.912103 0.857252 31.00000 -1.50000 H50B 2 0.954151 0.908282 0.959142 31.00000 -1.50000 H50C 2 0.842245 0.925385 0.885580 31.00000 -1.50000 AFIX 0 PART 2 SAME C47 > C50 C47A 1 0.681563 0.823012 0.946475 -31.00000 0.09980 0.04264 = 0.03696 0.00935 0.00382 -0.01171 AFIX 23 H47C 2 0.635731 0.833354 0.886496 -31.00000 -1.20000 H47D 2 0.650512 0.837249 0.989866 -31.00000 -1.20000 AFIX 0 C48A 1 0.792630 0.839707 0.963451 -31.00000 0.10249 0.04613 = 0.04039 0.01405 0.00060 -0.00745 AFIX 23 H48C 2 0.841430 0.812658 0.971433 -31.00000 -1.20000 H48D 2 0.813559 0.855330 1.021763 -31.00000 -1.20000 AFIX 0 C49A 1 0.823413 0.869772 0.903554 -31.00000 0.09376 0.05299 = 0.04053 0.02281 -0.00107 -0.00961 AFIX 23 H49C 2 0.755479 0.875941 0.852585 -31.00000 -1.20000 H49D 2 0.875596 0.853047 0.879953 -31.00000 -1.20000 AFIX 0 C50A 1 0.876141 0.914981 0.938002 -31.00000 0.07926 0.05508 = 0.05251 0.00064 0.02352 -0.00124 AFIX 137 H50D 2 0.949638 0.916890 0.930309 -31.00000 -1.50000 H50E 2 0.884294 0.917771 1.001285 -31.00000 -1.50000 H50F 2 0.828750 0.939657 0.904796 -31.00000 -1.50000 AFIX 0 PART 1 C51 1 0.715583 0.775836 1.050501 31.00000 0.09239 0.03484 = 0.03463 -0.00189 0.01417 0.00134 AFIX 23 H51A 2 0.707141 0.807844 1.066718 31.00000 -1.20000 H51B 2 0.668138 0.757100 1.075666 31.00000 -1.20000 AFIX 0 PART 2 C51A 1 0.738179 0.741677 1.023737 -31.00000 0.09649 0.04149 = 0.05011 0.00324 0.01626 0.01496 AFIX 23 H51C 2 0.687820 0.727000 1.051985 -31.00000 -1.50000 H51D 2 0.768975 0.717243 0.995614 -31.00000 -1.50000 AFIX 0 PART 0 C52 1 0.832927 0.762454 1.096012 11.00000 0.09562 0.04193 = 0.05441 0.00881 0.01536 -0.00314 PART 1 AFIX 23 H52A 2 0.882884 0.784880 1.081709 31.00000 -1.20000 H52B 2 0.846849 0.732441 1.073298 31.00000 -1.20000 PART 2 AFIX 23 H52C 2 0.828373 0.795427 1.082486 -31.00000 -1.20000 H52D 2 0.900827 0.751477 1.084535 -31.00000 -1.20000 AFIX 0 PART 0 C53 1 0.860163 0.759781 1.195005 11.00000 0.10270 0.06767 = 0.05047 0.00128 0.01395 -0.00702 AFIX 23 H53A 2 0.835740 0.788528 1.215478 11.00000 -1.20000 H53B 2 0.815258 0.734930 1.208330 11.00000 -1.20000 AFIX 0 C54 1 0.976572 0.752128 1.247622 11.00000 0.09658 0.10261 = 0.07786 0.02365 0.01977 0.03354 AFIX 137 H54A 2 0.984140 0.752177 1.311014 11.00000 -1.50000 H54B 2 1.022724 0.776399 1.235547 11.00000 -1.50000 H54C 2 1.000985 0.722670 1.231621 11.00000 -1.50000 AFIX 0 PART 1 O7 4 -0.004794 0.801862 0.482923 61.00000 0.13964 0.11086 = 0.13622 -0.00650 0.05461 -0.00493 O8 4 0.273301 0.806015 0.686081 71.00000 0.17433 0.12485 = 0.19960 0.00043 0.11761 -0.00415 PART 2 O9 4 -0.082148 0.800787 0.431956 41.00000 0.12018 0.08822 = 0.11933 -0.02020 0.05812 -0.01335 O10 4 0.087173 0.801630 0.570380 51.00000 0.13622 0.11497 = 0.13756 -0.00164 0.05194 -0.00665 PART 0 PART 2 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM AW1101 in P2(1)/c, WITT/KHUSNIYAROV, aw_NiL1 REM R1 = 0.0524 for 8378 Fo > 4sig(Fo) and 0.0818 for all 11761 data REM 817 parameters refined using 387 restraints END ; #===END OF ALL DATA