# Electronic Supplementary Material for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Liya Wang' _publ_contact_author_email WLYA@LYNU.EDU.CN _publ_section_title ; Dicarboxylate anion-dependent assembly of Ni(II) coordination polymers with 4,4'-dipyridyl sulfide ; loop_ _publ_author_name 'Liya Wang.' 'Stuart Batten' 'Jiang-Liang Hu.' 'Lu-Fang Ma.' 'Jian-ge Wang.' ; Yao-Yu Wang ; data_a _database_code_depnum_ccdc_archive 'CCDC 701845' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H38 N4 Ni2 O15 S2' _chemical_formula_weight 948.24 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2688(10) _cell_length_b 11.1859(10) _cell_length_c 18.4444(17) _cell_angle_alpha 80.2550(10) _cell_angle_beta 83.1220(10) _cell_angle_gamma 89.7290(10) _cell_volume 2072.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6504 _cell_measurement_theta_min 0.00 _cell_measurement_theta_max 0.00 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 980 _exptl_absorpt_coefficient_mu 1.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6199 _exptl_absorpt_correction_T_max 0.8417 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15524 _diffrn_reflns_av_R_equivalents 0.0191 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7684 _reflns_number_gt 6395 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0499P)^2^+1.8609P] 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 7684 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.1036 _refine_ls_wR_factor_gt 0.0969 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.49722(3) 0.44443(3) 0.286042(18) 0.02795(10) Uani 1 1 d . . . Ni2 Ni 0.52187(3) 0.94796(3) -0.162951(17) 0.02786(10) Uani 1 1 d . . . S1 S 0.00603(8) 1.29304(8) -0.10288(7) 0.0610(3) Uani 1 1 d . . . S2 S -0.04082(8) 0.67910(9) 0.44066(5) 0.0550(2) Uani 1 1 d . . . O6 O 0.67788(19) 0.84737(18) -0.20536(11) 0.0400(5) Uani 1 1 d . . . H11W H 0.6573 0.7745 -0.2037 0.060 Uiso 1 1 d R . . H12W H 0.6905 0.8823 -0.2495 0.060 Uiso 1 1 d R . . O7 O 0.66056(19) 0.34960(18) 0.24669(10) 0.0365(4) Uani 1 1 d . . . H13W H 0.6434 0.3048 0.2163 0.055 Uiso 1 1 d R . . H14W H 0.6735 0.3039 0.2860 0.055 Uiso 1 1 d R . . O8 O 0.45179(19) 0.30803(18) 0.37062(11) 0.0407(5) Uani 1 1 d . . . O9 O 0.6500(2) 0.2351(2) 0.38887(11) 0.0443(5) Uani 1 1 d . . . O10 O 0.6766(2) 0.0056(2) 0.65979(11) 0.0536(6) Uani 1 1 d . . . O11 O 0.4927(2) 0.0216(2) 0.73416(10) 0.0457(5) Uani 1 1 d . . . O12 O 0.50060(19) 0.56087(17) 0.18272(10) 0.0358(4) Uani 1 1 d . . . O13 O 0.38400(19) 0.39182(16) 0.20646(10) 0.0334(4) Uani 1 1 d . . . O14 O 0.50921(19) 0.83220(17) -0.05950(10) 0.0363(5) Uani 1 1 d . . . O15 O 0.39426(18) 0.78927(16) -0.14474(9) 0.0322(4) Uani 1 1 d . . . N1 N -0.3729(2) 0.5350(2) 0.33535(12) 0.0324(5) Uani 1 1 d . . . N2 N 0.3306(2) 0.5281(2) 0.33069(12) 0.0321(5) Uani 1 1 d . . . N3 N -0.3401(2) 1.0671(2) -0.14134(12) 0.0321(5) Uani 1 1 d . . . N4 N 0.3575(2) 1.0476(2) -0.13233(12) 0.0306(5) Uani 1 1 d . . . C1 C 0.5301(3) 0.2423(2) 0.40822(15) 0.0325(6) Uani 1 1 d . . . C2 C 0.4681(3) 0.1738(2) 0.48115(14) 0.0295(6) Uani 1 1 d . . . C3 C 0.3327(3) 0.1555(3) 0.49274(15) 0.0352(6) Uani 1 1 d . . . H3 H 0.2823 0.1840 0.4549 0.042 Uiso 1 1 calc R . . C4 C 0.2727(3) 0.0955(3) 0.55968(16) 0.0398(7) Uani 1 1 d . . . H4 H 0.1828 0.0800 0.5663 0.048 Uiso 1 1 calc R . . C5 C 0.3468(3) 0.0583(3) 0.61724(15) 0.0373(6) Uani 1 1 d . . . H5 H 0.3056 0.0219 0.6633 0.045 Uiso 1 1 calc R . . C6 C 0.4818(3) 0.0749(2) 0.60685(14) 0.0308(6) Uani 1 1 d . . . C7 C 0.5428(3) 0.1301(2) 0.53785(14) 0.0294(6) Uani 1 1 d . . . H7A H 0.6337 0.1378 0.5296 0.035 Uiso 1 1 calc R . . C8 C 0.5588(3) 0.0303(2) 0.67101(15) 0.0345(6) Uani 1 1 d . . . C9 C 0.3284(3) 0.6354(3) 0.35319(16) 0.0364(6) Uani 1 1 d . . . H9 H 0.4066 0.6795 0.3473 0.044 Uiso 1 1 calc R . . C10 C 0.2165(3) 0.6845(3) 0.38464(18) 0.0409(7) Uani 1 1 d . . . H10 H 0.2195 0.7603 0.3989 0.049 Uiso 1 1 calc R . . C11 C 0.0992(3) 0.6190(3) 0.39477(17) 0.0386(7) Uani 1 1 d . . . C12 C 0.1004(3) 0.5069(3) 0.37243(17) 0.0416(7) Uani 1 1 d . . . H12 H 0.0239 0.4603 0.3787 0.050 Uiso 1 1 calc R . . C13 C 0.2161(3) 0.4656(3) 0.34089(17) 0.0387(7) Uani 1 1 d . . . H13 H 0.2154 0.3904 0.3258 0.046 Uiso 1 1 calc R . . C14 C -0.2698(3) 0.5934(3) 0.29314(17) 0.0438(7) Uani 1 1 d . . . H14 H -0.2677 0.6042 0.2419 0.053 Uiso 1 1 calc R . . C15 C -0.1668(3) 0.6382(3) 0.32231(19) 0.0492(8) Uani 1 1 d . . . H15 H -0.0968 0.6784 0.2912 0.059 Uiso 1 1 calc R . . C16 C -0.1684(3) 0.6230(3) 0.39807(17) 0.0389(7) Uani 1 1 d . . . C17 C -0.2762(3) 0.5657(3) 0.44210(16) 0.0415(7) Uani 1 1 d . . . H17 H -0.2818 0.5560 0.4935 0.050 Uiso 1 1 calc R . . C18 C -0.3750(3) 0.5235(3) 0.40861(16) 0.0390(7) Uani 1 1 d . . . H18 H -0.4471 0.4849 0.4386 0.047 Uiso 1 1 calc R . . C19 C 0.4216(3) 0.4896(2) 0.16336(14) 0.0281(6) Uani 1 1 d . . . C20 C 0.3675(3) 0.5225(2) 0.09089(14) 0.0269(5) Uani 1 1 d . . . C21 C 0.2616(3) 0.4591(3) 0.07496(16) 0.0353(6) Uani 1 1 d . . . H21 H 0.2257 0.3928 0.1087 0.042 Uiso 1 1 calc R . . C22 C 0.2093(3) 0.4946(3) 0.00877(16) 0.0390(7) Uani 1 1 d . . . H22 H 0.1375 0.4527 -0.0014 0.047 Uiso 1 1 calc R . . C23 C 0.2638(3) 0.5921(3) -0.04211(15) 0.0356(6) Uani 1 1 d . . . H23 H 0.2292 0.6148 -0.0867 0.043 Uiso 1 1 calc R . . C24 C 0.3700(3) 0.6565(2) -0.02681(14) 0.0270(5) Uani 1 1 d . . . C25 C 0.4209(2) 0.6212(2) 0.03995(14) 0.0274(5) Uani 1 1 d . . . H25 H 0.4915 0.6640 0.0507 0.033 Uiso 1 1 calc R . . C26 C 0.4279(3) 0.7645(2) -0.07981(14) 0.0292(6) Uani 1 1 d . . . C27 C 0.3563(3) 1.1371(3) -0.09323(17) 0.0415(7) Uani 1 1 d . . . H27 H 0.4316 1.1512 -0.0723 0.050 Uiso 1 1 calc R . . C28 C 0.2511(3) 1.2097(3) -0.0819(2) 0.0484(8) Uani 1 1 d . . . H28 H 0.2554 1.2706 -0.0537 0.058 Uiso 1 1 calc R . . C29 C 0.1379(3) 1.1916(3) -0.11302(17) 0.0371(6) Uani 1 1 d . . . C30 C 0.1374(3) 1.0987(3) -0.15377(19) 0.0477(8) Uani 1 1 d . . . H30 H 0.0634 1.0829 -0.1754 0.057 Uiso 1 1 calc R . . C31 C 0.2475(3) 1.0304(3) -0.16185(18) 0.0449(8) Uani 1 1 d . . . H31 H 0.2458 0.9683 -0.1895 0.054 Uiso 1 1 calc R . . C32 C -0.3109(3) 1.1760(3) -0.18110(19) 0.0489(8) Uani 1 1 d . . . H32 H -0.3634 1.2064 -0.2175 0.059 Uiso 1 1 calc R . . C33 C -0.2065(3) 1.2466(3) -0.1713(2) 0.0507(8) Uani 1 1 d . . . H33 H -0.1885 1.3217 -0.2013 0.061 Uiso 1 1 calc R . . C34 C -0.1300(3) 1.2049(3) -0.11681(18) 0.0410(7) Uani 1 1 d . . . C35 C -0.1635(4) 1.0951(4) -0.0731(2) 0.0665(11) Uani 1 1 d . . . H35 H -0.1167 1.0657 -0.0338 0.080 Uiso 1 1 calc R . . C36 C -0.2664(4) 1.0290(3) -0.0877(2) 0.0586(10) Uani 1 1 d . . . H36 H -0.2857 0.9534 -0.0585 0.070 Uiso 1 1 calc R . . O1 O 0.9202(4) -0.0008(6) 0.5725(3) 0.182(3) Uani 1 1 d . . . H2W H 0.9565 -0.0533 0.5498 0.273 Uiso 1 1 d R . . H1W H 0.8493 -0.0291 0.5963 0.273 Uiso 1 1 d R . . O2 O 0.9581(8) 0.0490(9) 0.7137(4) 0.277(4) Uani 1 1 d . . . H3W H 0.9417 0.0373 0.6716 0.416 Uiso 1 1 d R . . H4W H 0.9606 -0.0196 0.7411 0.416 Uiso 1 1 d R . . O3 O 0.9627(11) -0.1610(10) 0.8268(11) 0.513(12) Uani 1 1 d . . . H6W H 1.0133 -0.1880 0.7945 0.770 Uiso 1 1 d R . . H5W H 0.8834 -0.1581 0.8178 0.770 Uiso 1 1 d R . . O4 O 1.0943(5) -0.2215(6) 0.5836(5) 0.247(4) Uani 1 1 d . . . H8W H 1.1749 -0.2291 0.5850 0.370 Uiso 1 1 d R . . H7W H 1.0606 -0.2460 0.5487 0.370 Uiso 1 1 d R . . O5 O 1.0377(8) -0.3409(13) 0.7679(7) 0.420(9) Uani 1 1 d . . . H10W H 1.0281 -0.3718 0.7293 0.630 Uiso 1 1 d R . . H9W H 1.1210 -0.3438 0.7637 0.630 Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.03056(19) 0.03070(19) 0.02225(18) -0.00034(13) -0.00766(13) -0.00166(14) Ni2 0.03115(19) 0.02956(19) 0.02218(18) -0.00039(13) -0.00603(13) -0.00145(14) S1 0.0324(4) 0.0464(5) 0.1142(8) -0.0379(5) -0.0154(5) 0.0028(4) S2 0.0301(4) 0.0789(6) 0.0688(6) -0.0455(5) -0.0109(4) 0.0009(4) O6 0.0409(11) 0.0333(10) 0.0443(12) -0.0042(9) -0.0021(9) 0.0007(9) O7 0.0417(11) 0.0413(11) 0.0279(10) -0.0067(8) -0.0090(8) 0.0025(9) O8 0.0390(11) 0.0424(12) 0.0352(11) 0.0123(9) -0.0087(9) -0.0003(9) O9 0.0407(12) 0.0534(13) 0.0335(11) 0.0071(9) -0.0031(9) 0.0082(10) O10 0.0440(13) 0.0799(17) 0.0327(12) 0.0031(11) -0.0058(10) 0.0139(12) O11 0.0498(13) 0.0613(14) 0.0228(10) 0.0020(9) -0.0057(9) 0.0108(11) O12 0.0440(11) 0.0345(10) 0.0288(10) 0.0012(8) -0.0132(8) -0.0088(9) O13 0.0450(11) 0.0275(10) 0.0268(10) 0.0020(8) -0.0097(8) -0.0037(8) O14 0.0448(11) 0.0364(11) 0.0270(10) 0.0023(8) -0.0121(8) -0.0107(9) O15 0.0426(11) 0.0322(10) 0.0221(9) -0.0023(8) -0.0084(8) -0.0022(8) N1 0.0286(12) 0.0397(13) 0.0304(12) -0.0084(10) -0.0059(9) -0.0007(10) N2 0.0307(12) 0.0333(12) 0.0323(12) -0.0023(10) -0.0078(9) -0.0008(9) N3 0.0294(12) 0.0342(12) 0.0319(12) -0.0029(10) -0.0047(9) -0.0003(10) N4 0.0303(12) 0.0348(12) 0.0272(12) -0.0055(9) -0.0056(9) -0.0018(9) C1 0.0407(16) 0.0301(14) 0.0275(14) -0.0034(11) -0.0098(12) 0.0006(12) C2 0.0387(15) 0.0246(13) 0.0263(13) -0.0048(10) -0.0079(11) 0.0020(11) C3 0.0395(16) 0.0354(15) 0.0317(15) -0.0026(12) -0.0121(12) 0.0043(12) C4 0.0319(15) 0.0479(17) 0.0381(16) -0.0033(13) -0.0039(12) -0.0007(13) C5 0.0403(16) 0.0407(16) 0.0274(14) 0.0005(12) 0.0011(12) -0.0009(13) C6 0.0397(15) 0.0271(13) 0.0257(13) -0.0034(11) -0.0059(11) 0.0029(11) C7 0.0321(14) 0.0281(13) 0.0278(14) -0.0031(11) -0.0059(11) 0.0011(11) C8 0.0466(17) 0.0303(14) 0.0260(14) -0.0012(11) -0.0076(12) -0.0003(12) C9 0.0306(15) 0.0345(15) 0.0444(17) -0.0038(13) -0.0099(12) -0.0039(12) C10 0.0348(15) 0.0385(16) 0.0538(19) -0.0155(14) -0.0124(14) 0.0014(13) C11 0.0311(15) 0.0473(17) 0.0411(16) -0.0135(13) -0.0103(12) -0.0003(13) C12 0.0296(15) 0.0453(17) 0.0523(19) -0.0142(14) -0.0061(13) -0.0082(13) C13 0.0361(16) 0.0373(16) 0.0454(17) -0.0115(13) -0.0094(13) -0.0043(12) C14 0.0402(17) 0.057(2) 0.0335(16) -0.0044(14) -0.0059(13) -0.0092(14) C15 0.0352(17) 0.062(2) 0.0491(19) -0.0082(16) -0.0016(14) -0.0147(15) C16 0.0271(14) 0.0475(17) 0.0478(18) -0.0215(14) -0.0079(12) 0.0027(12) C17 0.0413(17) 0.0555(19) 0.0317(15) -0.0169(14) -0.0070(13) -0.0003(14) C18 0.0351(15) 0.0521(18) 0.0311(15) -0.0121(13) -0.0019(12) -0.0080(13) C19 0.0322(14) 0.0274(13) 0.0245(13) -0.0024(11) -0.0062(11) 0.0025(11) C20 0.0322(14) 0.0258(13) 0.0231(13) -0.0033(10) -0.0060(10) 0.0018(10) C21 0.0387(15) 0.0321(14) 0.0336(15) 0.0004(12) -0.0055(12) -0.0078(12) C22 0.0401(16) 0.0404(16) 0.0377(16) -0.0027(13) -0.0150(13) -0.0123(13) C23 0.0392(16) 0.0406(16) 0.0290(14) -0.0038(12) -0.0144(12) -0.0005(13) C24 0.0322(14) 0.0258(13) 0.0238(13) -0.0057(10) -0.0042(10) 0.0017(10) C25 0.0287(13) 0.0289(13) 0.0257(13) -0.0056(10) -0.0064(10) -0.0006(10) C26 0.0334(14) 0.0299(14) 0.0245(13) -0.0037(11) -0.0060(11) 0.0011(11) C27 0.0323(15) 0.0496(18) 0.0487(18) -0.0214(15) -0.0109(13) -0.0032(13) C28 0.0344(16) 0.0519(19) 0.068(2) -0.0357(17) -0.0089(15) 0.0001(14) C29 0.0297(14) 0.0359(15) 0.0464(17) -0.0094(13) -0.0035(12) -0.0019(12) C30 0.0352(16) 0.0528(19) 0.064(2) -0.0244(17) -0.0194(15) 0.0041(14) C31 0.0418(17) 0.0461(18) 0.055(2) -0.0247(15) -0.0172(15) 0.0022(14) C32 0.0479(19) 0.0448(18) 0.052(2) 0.0070(15) -0.0187(15) -0.0079(15) C33 0.0454(18) 0.0385(17) 0.066(2) 0.0025(15) -0.0126(16) -0.0101(14) C34 0.0290(15) 0.0392(16) 0.059(2) -0.0197(15) -0.0044(14) 0.0021(12) C35 0.063(2) 0.073(3) 0.063(2) 0.012(2) -0.037(2) -0.018(2) C36 0.059(2) 0.057(2) 0.056(2) 0.0181(17) -0.0281(17) -0.0217(17) O1 0.095(3) 0.284(7) 0.187(5) -0.118(5) 0.016(3) -0.062(4) O2 0.303(10) 0.365(12) 0.185(7) -0.090(8) -0.049(6) -0.069(9) O3 0.252(11) 0.295(13) 1.07(4) -0.28(2) -0.175(17) -0.048(9) O4 0.106(4) 0.226(6) 0.470(12) -0.158(7) -0.144(6) 0.021(4) O5 0.145(6) 0.58(2) 0.59(2) -0.302(18) 0.037(9) -0.096(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O8 2.0015(19) . ? Ni1 N1 2.061(2) 1_655 ? Ni1 N2 2.096(2) . ? Ni1 O7 2.1018(19) . ? Ni1 O12 2.1152(18) . ? Ni1 O13 2.1355(18) . ? Ni1 C19 2.451(3) . ? Ni2 O11 1.9935(19) 1_564 ? Ni2 N3 2.067(2) 1_655 ? Ni2 N4 2.092(2) . ? Ni2 O6 2.104(2) . ? Ni2 O14 2.1072(18) . ? Ni2 O15 2.1669(18) . ? Ni2 C26 2.468(3) . ? S1 C29 1.775(3) . ? S1 C34 1.782(3) . ? S2 C11 1.769(3) . ? S2 C16 1.774(3) . ? O6 H11W 0.8376 . ? O6 H12W 0.8358 . ? O7 H13W 0.8464 . ? O7 H14W 0.8370 . ? O8 C1 1.274(3) . ? O9 C1 1.246(3) . ? O10 C8 1.240(4) . ? O11 C8 1.265(3) . ? O11 Ni2 1.9935(19) 1_546 ? O12 C19 1.262(3) . ? O13 C19 1.270(3) . ? O14 C26 1.260(3) . ? O15 C26 1.271(3) . ? N1 C18 1.333(4) . ? N1 C14 1.338(4) . ? N1 Ni1 2.061(2) 1_455 ? N2 C9 1.334(4) . ? N2 C13 1.348(4) . ? N3 C32 1.327(4) . ? N3 C36 1.330(4) . ? N3 Ni2 2.067(2) 1_455 ? N4 C27 1.328(4) . ? N4 C31 1.339(4) . ? C1 C2 1.501(4) . ? C2 C3 1.392(4) . ? C2 C7 1.392(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.386(4) . ? C4 H4 0.9300 . ? C5 C6 1.386(4) . ? C5 H5 0.9300 . ? C6 C7 1.392(4) . ? C6 C8 1.515(4) . ? C7 H7A 0.9300 . ? C9 C10 1.378(4) . ? C9 H9 0.9300 . ? C10 C11 1.390(4) . ? C10 H10 0.9300 . ? C11 C12 1.383(4) . ? C12 C13 1.372(4) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.375(4) . ? C14 H14 0.9300 . ? C15 C16 1.377(4) . ? C15 H15 0.9300 . ? C16 C17 1.383(4) . ? C17 C18 1.373(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.497(3) . ? C20 C21 1.387(4) . ? C20 C25 1.390(4) . ? C21 C22 1.388(4) . ? C21 H21 0.9300 . ? C22 C23 1.385(4) . ? C22 H22 0.9300 . ? C23 C24 1.392(4) . ? C23 H23 0.9300 . ? C24 C25 1.390(3) . ? C24 C26 1.496(4) . ? C25 H25 0.9300 . ? C27 C28 1.365(4) . ? C27 H27 0.9300 . ? C28 C29 1.387(4) . ? C28 H28 0.9300 . ? C29 C30 1.382(4) . ? C30 C31 1.369(4) . ? C30 H30 0.9300 . ? C31 H31 0.9300 . ? C32 C33 1.382(4) . ? C32 H32 0.9300 . ? C33 C34 1.368(4) . ? C33 H33 0.9300 . ? C34 C35 1.370(5) . ? C35 C36 1.371(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? O1 H2W 0.8380 . ? O1 H1W 0.8378 . ? O2 H3W 0.8437 . ? O2 H4W 0.8463 . ? O3 H6W 0.8376 . ? O3 H5W 0.8498 . ? O4 H8W 0.8345 . ? O4 H7W 0.8500 . ? O5 H10W 0.8583 . ? O5 H9W 0.8504 . ? 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 O8 Ni1 N1 97.39(9) . 1_655 ? O8 Ni1 N2 85.44(9) . . ? N1 Ni1 N2 94.73(9) 1_655 . ? O8 Ni1 O7 90.61(8) . . ? N1 Ni1 O7 86.26(8) 1_655 . ? N2 Ni1 O7 176.02(8) . . ? O8 Ni1 O12 162.19(8) . . ? N1 Ni1 O12 100.39(8) 1_655 . ? N2 Ni1 O12 91.89(8) . . ? O7 Ni1 O12 91.72(8) . . ? O8 Ni1 O13 100.12(8) . . ? N1 Ni1 O13 162.37(8) 1_655 . ? N2 Ni1 O13 88.71(8) . . ? O7 Ni1 O13 91.50(7) . . ? O12 Ni1 O13 62.17(7) . . ? O8 Ni1 C19 131.25(9) . . ? N1 Ni1 C19 131.37(9) 1_655 . ? N2 Ni1 C19 89.66(9) . . ? O7 Ni1 C19 92.58(8) . . ? O12 Ni1 C19 30.99(8) . . ? O13 Ni1 C19 31.19(8) . . ? O11 Ni2 N3 101.02(9) 1_564 1_655 ? O11 Ni2 N4 84.12(8) 1_564 . ? N3 Ni2 N4 96.20(9) 1_655 . ? O11 Ni2 O6 89.96(8) 1_564 . ? N3 Ni2 O6 87.98(8) 1_655 . ? N4 Ni2 O6 173.31(8) . . ? O11 Ni2 O14 162.42(9) 1_564 . ? N3 Ni2 O14 96.56(8) 1_655 . ? N4 Ni2 O14 93.84(8) . . ? O6 Ni2 O14 90.86(8) . . ? O11 Ni2 O15 100.77(8) 1_564 . ? N3 Ni2 O15 158.13(8) 1_655 . ? N4 Ni2 O15 87.89(8) . . ? O6 Ni2 O15 90.17(7) . . ? O14 Ni2 O15 61.67(7) . . ? O11 Ni2 C26 131.74(9) 1_564 . ? N3 Ni2 C26 127.24(9) 1_655 . ? N4 Ni2 C26 90.70(9) . . ? O6 Ni2 C26 90.92(8) . . ? O14 Ni2 C26 30.69(8) . . ? O15 Ni2 C26 30.98(7) . . ? C29 S1 C34 101.92(14) . . ? C11 S2 C16 101.39(13) . . ? Ni2 O6 H11W 112.6 . . ? Ni2 O6 H12W 101.2 . . ? H11W O6 H12W 109.8 . . ? Ni1 O7 H13W 113.3 . . ? Ni1 O7 H14W 99.9 . . ? H13W O7 H14W 107.3 . . ? C1 O8 Ni1 127.79(18) . . ? C8 O11 Ni2 135.03(19) . 1_546 ? C19 O12 Ni1 89.37(15) . . ? C19 O13 Ni1 88.26(15) . . ? C26 O14 Ni2 90.69(15) . . ? C26 O15 Ni2 87.70(15) . . ? C18 N1 C14 117.4(2) . . ? C18 N1 Ni1 122.95(19) . 1_455 ? C14 N1 Ni1 118.90(19) . 1_455 ? C9 N2 C13 116.8(2) . . ? C9 N2 Ni1 125.94(19) . . ? C13 N2 Ni1 117.17(19) . . ? C32 N3 C36 116.5(3) . . ? C32 N3 Ni2 125.0(2) . 1_455 ? C36 N3 Ni2 118.2(2) . 1_455 ? C27 N4 C31 116.4(2) . . ? C27 N4 Ni2 125.67(19) . . ? C31 N4 Ni2 117.44(19) . . ? O9 C1 O8 124.5(3) . . ? O9 C1 C2 120.7(2) . . ? O8 C1 C2 114.8(2) . . ? C3 C2 C7 119.3(2) . . ? C3 C2 C1 119.3(2) . . ? C7 C2 C1 121.4(2) . . ? C4 C3 C2 120.6(3) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 120.6(3) . . ? C6 C5 H5 119.7 . . ? C4 C5 H5 119.7 . . ? C5 C6 C7 119.3(2) . . ? C5 C6 C8 118.6(2) . . ? C7 C6 C8 122.0(2) . . ? C2 C7 C6 120.2(3) . . ? C2 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? O10 C8 O11 125.0(3) . . ? O10 C8 C6 120.7(2) . . ? O11 C8 C6 114.3(3) . . ? N2 C9 C10 123.6(3) . . ? N2 C9 H9 118.2 . . ? C10 C9 H9 118.2 . . ? C9 C10 C11 118.9(3) . . ? C9 C10 H10 120.5 . . ? C11 C10 H10 120.5 . . ? C12 C11 C10 118.1(3) . . ? C12 C11 S2 123.6(2) . . ? C10 C11 S2 118.2(2) . . ? C13 C12 C11 119.1(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? N2 C13 C12 123.5(3) . . ? N2 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? N1 C14 C15 122.8(3) . . ? N1 C14 H14 118.6 . . ? C15 C14 H14 118.6 . . ? C14 C15 C16 119.3(3) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 118.2(3) . . ? C15 C16 S2 122.5(2) . . ? C17 C16 S2 119.2(2) . . ? C18 C17 C16 118.8(3) . . ? C18 C17 H17 120.6 . . ? C16 C17 H17 120.6 . . ? N1 C18 C17 123.4(3) . . ? N1 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? O12 C19 O13 120.1(2) . . ? O12 C19 C20 120.1(2) . . ? O13 C19 C20 119.7(2) . . ? O12 C19 Ni1 59.63(13) . . ? O13 C19 Ni1 60.55(13) . . ? C20 C19 Ni1 175.79(19) . . ? C21 C20 C25 119.5(2) . . ? C21 C20 C19 121.1(2) . . ? C25 C20 C19 119.4(2) . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C23 C22 C21 120.2(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C24 120.3(2) . . ? C22 C23 H23 119.9 . . ? C24 C23 H23 119.9 . . ? C25 C24 C23 119.2(2) . . ? C25 C24 C26 119.5(2) . . ? C23 C24 C26 121.3(2) . . ? C24 C25 C20 120.8(2) . . ? C24 C25 H25 119.6 . . ? C20 C25 H25 119.6 . . ? O14 C26 O15 119.9(2) . . ? O14 C26 C24 119.6(2) . . ? O15 C26 C24 120.4(2) . . ? O14 C26 Ni2 58.62(13) . . ? O15 C26 Ni2 61.32(13) . . ? C24 C26 Ni2 177.56(19) . . ? N4 C27 C28 123.9(3) . . ? N4 C27 H27 118.1 . . ? C28 C27 H27 118.1 . . ? C27 C28 C29 119.4(3) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C30 C29 C28 117.5(3) . . ? C30 C29 S1 123.7(2) . . ? C28 C29 S1 118.7(2) . . ? C31 C30 C29 119.0(3) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? N4 C31 C30 123.9(3) . . ? N4 C31 H31 118.0 . . ? C30 C31 H31 118.0 . . ? N3 C32 C33 123.4(3) . . ? N3 C32 H32 118.3 . . ? C33 C32 H32 118.3 . . ? C34 C33 C32 119.2(3) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 117.7(3) . . ? C33 C34 S1 120.4(2) . . ? C35 C34 S1 121.8(3) . . ? C34 C35 C36 119.5(3) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? N3 C36 C35 123.5(3) . . ? N3 C36 H36 118.3 . . ? C35 C36 H36 118.3 . . ? H2W O1 H1W 109.3 . . ? H3W O2 H4W 107.8 . . ? H6W O3 H5W 113.2 . . ? H8W O4 H7W 118.4 . . ? H10W O5 H9W 96.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 O8 C1 -48.3(2) 1_655 . . . ? N2 Ni1 O8 C1 -142.5(2) . . . . ? O7 Ni1 O8 C1 38.0(2) . . . . ? O12 Ni1 O8 C1 135.5(3) . . . . ? O13 Ni1 O8 C1 129.6(2) . . . . ? C19 Ni1 O8 C1 131.9(2) . . . . ? O8 Ni1 O12 C19 -5.3(4) . . . . ? N1 Ni1 O12 C19 178.65(16) 1_655 . . . ? N2 Ni1 O12 C19 -86.19(16) . . . . ? O7 Ni1 O12 C19 92.13(16) . . . . ? O13 Ni1 O12 C19 1.35(15) . . . . ? O8 Ni1 O13 C19 176.61(15) . . . . ? N1 Ni1 O13 C19 -10.1(3) 1_655 . . . ? N2 Ni1 O13 C19 91.48(16) . . . . ? O7 Ni1 O13 C19 -92.50(15) . . . . ? O12 Ni1 O13 C19 -1.34(15) . . . . ? O11 Ni2 O14 C26 2.3(4) 1_564 . . . ? N3 Ni2 O14 C26 -178.41(16) 1_655 . . . ? N4 Ni2 O14 C26 84.89(17) . . . . ? O6 Ni2 O14 C26 -90.35(16) . . . . ? O15 Ni2 O14 C26 -0.62(15) . . . . ? O11 Ni2 O15 C26 -178.50(15) 1_564 . . . ? N3 Ni2 O15 C26 6.5(3) 1_655 . . . ? N4 Ni2 O15 C26 -94.89(16) . . . . ? O6 Ni2 O15 C26 91.51(15) . . . . ? O14 Ni2 O15 C26 0.62(15) . . . . ? O8 Ni1 N2 C9 121.3(2) . . . . ? N1 Ni1 N2 C9 24.2(2) 1_655 . . . ? O7 Ni1 N2 C9 128.5(11) . . . . ? O12 Ni1 N2 C9 -76.4(2) . . . . ? O13 Ni1 N2 C9 -138.5(2) . . . . ? C19 Ni1 N2 C9 -107.3(2) . . . . ? O8 Ni1 N2 C13 -55.4(2) . . . . ? N1 Ni1 N2 C13 -152.5(2) 1_655 . . . ? O7 Ni1 N2 C13 -48.2(12) . . . . ? O12 Ni1 N2 C13 106.9(2) . . . . ? O13 Ni1 N2 C13 44.8(2) . . . . ? C19 Ni1 N2 C13 76.0(2) . . . . ? O11 Ni2 N4 C27 -116.2(2) 1_564 . . . ? N3 Ni2 N4 C27 -15.7(2) 1_655 . . . ? O6 Ni2 N4 C27 -144.1(6) . . . . ? O14 Ni2 N4 C27 81.3(2) . . . . ? O15 Ni2 N4 C27 142.8(2) . . . . ? C26 Ni2 N4 C27 111.9(2) . . . . ? O11 Ni2 N4 C31 55.2(2) 1_564 . . . ? N3 Ni2 N4 C31 155.7(2) 1_655 . . . ? O6 Ni2 N4 C31 27.3(8) . . . . ? O14 Ni2 N4 C31 -107.2(2) . . . . ? O15 Ni2 N4 C31 -45.8(2) . . . . ? C26 Ni2 N4 C31 -76.7(2) . . . . ? Ni1 O8 C1 O9 -15.8(4) . . . . ? Ni1 O8 C1 C2 162.45(18) . . . . ? O9 C1 C2 C3 -162.2(3) . . . . ? O8 C1 C2 C3 19.4(4) . . . . ? O9 C1 C2 C7 19.0(4) . . . . ? O8 C1 C2 C7 -159.4(2) . . . . ? C7 C2 C3 C4 0.4(4) . . . . ? C1 C2 C3 C4 -178.5(3) . . . . ? C2 C3 C4 C5 3.2(4) . . . . ? C3 C4 C5 C6 -3.6(5) . . . . ? C4 C5 C6 C7 0.3(4) . . . . ? C4 C5 C6 C8 -178.7(3) . . . . ? C3 C2 C7 C6 -3.7(4) . . . . ? C1 C2 C7 C6 175.1(2) . . . . ? C5 C6 C7 C2 3.4(4) . . . . ? C8 C6 C7 C2 -177.7(2) . . . . ? Ni2 O11 C8 O10 -11.4(5) 1_546 . . . ? Ni2 O11 C8 C6 168.7(2) 1_546 . . . ? C5 C6 C8 O10 156.0(3) . . . . ? C7 C6 C8 O10 -23.0(4) . . . . ? C5 C6 C8 O11 -24.2(4) . . . . ? C7 C6 C8 O11 156.9(3) . . . . ? C13 N2 C9 C10 -0.9(4) . . . . ? Ni1 N2 C9 C10 -177.6(2) . . . . ? N2 C9 C10 C11 0.9(5) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? C9 C10 C11 S2 176.0(2) . . . . ? C16 S2 C11 C12 -34.9(3) . . . . ? C16 S2 C11 C10 149.2(3) . . . . ? C10 C11 C12 C13 -0.5(5) . . . . ? S2 C11 C12 C13 -176.4(2) . . . . ? C9 N2 C13 C12 0.2(4) . . . . ? Ni1 N2 C13 C12 177.2(2) . . . . ? C11 C12 C13 N2 0.5(5) . . . . ? C18 N1 C14 C15 1.6(5) . . . . ? Ni1 N1 C14 C15 -168.5(3) 1_455 . . . ? N1 C14 C15 C16 0.0(5) . . . . ? C14 C15 C16 C17 -1.8(5) . . . . ? C14 C15 C16 S2 -179.3(3) . . . . ? C11 S2 C16 C15 -51.9(3) . . . . ? C11 S2 C16 C17 130.6(3) . . . . ? C15 C16 C17 C18 1.8(5) . . . . ? S2 C16 C17 C18 179.5(2) . . . . ? C14 N1 C18 C17 -1.6(5) . . . . ? Ni1 N1 C18 C17 168.2(2) 1_455 . . . ? C16 C17 C18 N1 -0.2(5) . . . . ? Ni1 O12 C19 O13 -2.3(3) . . . . ? Ni1 O12 C19 C20 175.1(2) . . . . ? Ni1 O13 C19 O12 2.3(2) . . . . ? Ni1 O13 C19 C20 -175.2(2) . . . . ? O8 Ni1 C19 O12 177.87(14) . . . . ? N1 Ni1 C19 O12 -1.8(2) 1_655 . . . ? N2 Ni1 C19 O12 94.24(16) . . . . ? O7 Ni1 C19 O12 -89.06(16) . . . . ? O13 Ni1 C19 O12 -177.7(2) . . . . ? O8 Ni1 C19 O13 -4.4(2) . . . . ? N1 Ni1 C19 O13 175.93(14) 1_655 . . . ? N2 Ni1 C19 O13 -88.07(16) . . . . ? O7 Ni1 C19 O13 88.64(15) . . . . ? O12 Ni1 C19 O13 177.7(2) . . . . ? O8 Ni1 C19 C20 90(3) . . . . ? N1 Ni1 C19 C20 -89(3) 1_655 . . . ? N2 Ni1 C19 C20 7(3) . . . . ? O7 Ni1 C19 C20 -177(3) . . . . ? O12 Ni1 C19 C20 -87(3) . . . . ? O13 Ni1 C19 C20 95(3) . . . . ? O12 C19 C20 C21 -166.8(3) . . . . ? O13 C19 C20 C21 10.7(4) . . . . ? Ni1 C19 C20 C21 -82(3) . . . . ? O12 C19 C20 C25 10.7(4) . . . . ? O13 C19 C20 C25 -171.9(2) . . . . ? Ni1 C19 C20 C25 96(3) . . . . ? C25 C20 C21 C22 -0.3(4) . . . . ? C19 C20 C21 C22 177.1(3) . . . . ? C20 C21 C22 C23 1.0(5) . . . . ? C21 C22 C23 C24 -1.0(5) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C22 C23 C24 C26 -178.1(3) . . . . ? C23 C24 C25 C20 0.4(4) . . . . ? C26 C24 C25 C20 178.8(2) . . . . ? C21 C20 C25 C24 -0.4(4) . . . . ? C19 C20 C25 C24 -177.9(2) . . . . ? Ni2 O14 C26 O15 1.1(3) . . . . ? Ni2 O14 C26 C24 -178.0(2) . . . . ? Ni2 O15 C26 O14 -1.1(3) . . . . ? Ni2 O15 C26 C24 178.0(2) . . . . ? C25 C24 C26 O14 -9.8(4) . . . . ? C23 C24 C26 O14 168.5(3) . . . . ? C25 C24 C26 O15 171.1(2) . . . . ? C23 C24 C26 O15 -10.6(4) . . . . ? C25 C24 C26 Ni2 -54(5) . . . . ? C23 C24 C26 Ni2 124(4) . . . . ? O11 Ni2 C26 O14 -179.09(15) 1_564 . . . ? N3 Ni2 C26 O14 2.0(2) 1_655 . . . ? N4 Ni2 C26 O14 -96.35(16) . . . . ? O6 Ni2 C26 O14 90.14(16) . . . . ? O15 Ni2 C26 O14 178.9(3) . . . . ? O11 Ni2 C26 O15 2.0(2) 1_564 . . . ? N3 Ni2 C26 O15 -176.95(14) 1_655 . . . ? N4 Ni2 C26 O15 84.72(15) . . . . ? O6 Ni2 C26 O15 -88.79(15) . . . . ? O14 Ni2 C26 O15 -178.9(3) . . . . ? O11 Ni2 C26 C24 -134(4) 1_564 . . . ? N3 Ni2 C26 C24 47(4) 1_655 . . . ? N4 Ni2 C26 C24 -51(4) . . . . ? O6 Ni2 C26 C24 135(4) . . . . ? O14 Ni2 C26 C24 45(4) . . . . ? O15 Ni2 C26 C24 -136(5) . . . . ? C31 N4 C27 C28 0.3(5) . . . . ? Ni2 N4 C27 C28 171.7(3) . . . . ? N4 C27 C28 C29 -0.6(5) . . . . ? C27 C28 C29 C30 0.7(5) . . . . ? C27 C28 C29 S1 -175.9(3) . . . . ? C34 S1 C29 C30 25.4(3) . . . . ? C34 S1 C29 C28 -158.2(3) . . . . ? C28 C29 C30 C31 -0.4(5) . . . . ? S1 C29 C30 C31 176.0(3) . . . . ? C27 N4 C31 C30 0.0(5) . . . . ? Ni2 N4 C31 C30 -172.2(3) . . . . ? C29 C30 C31 N4 0.1(5) . . . . ? C36 N3 C32 C33 2.9(5) . . . . ? Ni2 N3 C32 C33 -171.1(3) 1_455 . . . ? N3 C32 C33 C34 -1.6(6) . . . . ? C32 C33 C34 C35 -1.7(5) . . . . ? C32 C33 C34 S1 179.6(3) . . . . ? C29 S1 C34 C33 -122.9(3) . . . . ? C29 S1 C34 C35 58.4(3) . . . . ? C33 C34 C35 C36 3.4(6) . . . . ? S1 C34 C35 C36 -177.8(3) . . . . ? C32 N3 C36 C35 -1.0(6) . . . . ? Ni2 N3 C36 C35 173.4(3) 1_455 . . . ? C34 C35 C36 N3 -2.2(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H12W O10 0.84 2.00 2.800(3) 159.9 1_564 O7 H13W O15 0.85 1.90 2.742(3) 177.4 2_665 O7 H14W O9 0.84 1.91 2.707(3) 158.4 . O1 H2W O4 0.84 2.39 3.034(9) 134.0 . O1 H2W O1 0.84 2.43 2.961(10) 121.8 2_756 O1 H1W O10 0.84 2.08 2.816(5) 146.6 . O2 H3W O1 0.84 1.98 2.824(8) 173.9 . O2 H4W O3 0.85 2.04 2.870(17) 166.4 . O3 H6W O5 0.84 1.87 2.519(17) 133.9 . O3 H5W O6 0.85 2.20 3.051(11) 179.4 1_546 O4 H8W O9 0.83 1.91 2.732(5) 166.2 2_756 O4 H7W S2 0.85 2.61 3.463(6) 179.4 1_645 O5 H9W O7 0.85 2.23 3.081(9) 179.4 2_756 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.644 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.063 # Attachment '2.cif' data_b _database_code_depnum_ccdc_archive 'CCDC 701846' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H26 N6 Ni2 O14 S2' _chemical_formula_weight 948.17 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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 14.3584(14) _cell_length_b 8.2781(8) _cell_length_c 15.8981(15) _cell_angle_alpha 90.00 _cell_angle_beta 93.7350(10) _cell_angle_gamma 90.00 _cell_volume 1885.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 6302 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 28.02 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 1.189 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5941 _exptl_absorpt_correction_T_max 0.6383 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13517 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3504 _reflns_number_gt 3157 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.7500P] 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 3504 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0303 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0942 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 0.735 _refine_ls_restrained_S_all 0.735 _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 0.7500 0.72217(4) 1.2500 0.02295(12) Uani 1 2 d S . . Ni2 Ni 0.7500 0.24878(4) 0.7500 0.02719(13) Uani 1 2 d S . . S1 S 1.04475(5) 0.73099(7) 0.97408(4) 0.04790(18) Uani 1 1 d . . . O1 O 0.63149(9) 0.65651(17) 1.17995(8) 0.0337(3) Uani 1 1 d . . . O2 O 0.76140(9) 0.53202(17) 1.15171(9) 0.0383(3) Uani 1 1 d . . . O3 O 0.69000(11) 0.25382(17) 0.86195(9) 0.0399(4) Uani 1 1 d . . . O4 O 0.56350(9) 0.09528(16) 0.84502(8) 0.0342(3) Uani 1 1 d . . . O5 O 0.32576(9) 0.1641(2) 1.06030(9) 0.0501(4) Uani 1 1 d . . . O6 O 0.37542(10) 0.24900(17) 1.18355(9) 0.0385(4) Uani 1 1 d . . . O7 O 0.84237(12) 0.06311(18) 0.79484(9) 0.0468(4) Uani 1 1 d . . . H1W H 0.8805 0.0478 0.7582 0.070 Uiso 1 1 d R . . H2W H 0.8132 -0.0204 0.8046 0.070 Uiso 1 1 d R . . N1 N 0.84667(10) 0.41882(19) 0.80565(10) 0.0292(3) Uani 1 1 d . . . N2 N 1.18709(10) 1.10664(18) 0.81880(9) 0.0293(3) Uani 1 1 d . . . N3 N 0.38595(11) 0.2247(2) 1.10898(10) 0.0297(4) Uani 1 1 d . . . C1 C 0.67424(13) 0.5439(2) 1.14365(11) 0.0280(4) Uani 1 1 d . . . C2 C 0.61593(12) 0.4239(2) 1.09303(11) 0.0268(4) Uani 1 1 d . . . C3 C 0.53048(12) 0.3798(2) 1.12156(11) 0.0282(4) Uani 1 1 d . . . H3 H 0.5105 0.4227 1.1714 0.034 Uiso 1 1 calc R . . C4 C 0.47536(13) 0.2713(2) 1.07506(12) 0.0257(4) Uani 1 1 d . . . C5 C 0.49997(13) 0.2092(2) 0.99862(11) 0.0250(4) Uani 1 1 d . . . H5A H 0.4601 0.1404 0.9672 0.030 Uiso 1 1 calc R . . C6 C 0.58652(13) 0.25339(19) 0.97035(11) 0.0254(4) Uani 1 1 d . . . C7 C 0.64470(12) 0.3573(2) 1.01858(11) 0.0273(4) Uani 1 1 d . . . H7A H 0.7034 0.3825 1.0008 0.033 Uiso 1 1 calc R . . C8 C 0.61482(12) 0.1934(2) 0.88524(10) 0.0266(4) Uani 1 1 d . . . C9 C 0.81561(13) 0.5344(2) 0.85511(13) 0.0370(5) Uani 1 1 d . . . H9 H 0.7514 0.5478 0.8567 0.044 Uiso 1 1 calc R . . C10 C 0.87354(14) 0.6359(3) 0.90437(14) 0.0400(5) Uani 1 1 d . . . H10 H 0.8486 0.7149 0.9379 0.048 Uiso 1 1 calc R . . C11 C 0.96925(14) 0.6169(2) 0.90250(12) 0.0352(4) Uani 1 1 d . . . C12 C 1.00312(13) 0.4999(3) 0.85020(12) 0.0362(4) Uani 1 1 d . . . H12 H 1.0670 0.4856 0.8469 0.043 Uiso 1 1 calc R . . C13 C 0.94021(13) 0.4046(2) 0.80309(12) 0.0329(4) Uani 1 1 d . . . H13 H 0.9634 0.3267 0.7678 0.040 Uiso 1 1 calc R . . C14 C 1.21414(14) 1.0736(3) 0.89897(12) 0.0379(5) Uani 1 1 d . . . H14 H 1.2635 1.1325 0.9244 0.046 Uiso 1 1 calc R . . C15 C 1.17277(15) 0.9567(3) 0.94614(12) 0.0394(5) Uani 1 1 d . . . H15 H 1.1941 0.9370 1.0017 0.047 Uiso 1 1 calc R . . C16 C 1.09872(13) 0.8692(2) 0.90865(12) 0.0310(4) Uani 1 1 d . . . C17 C 1.07071(14) 0.9006(2) 0.82504(12) 0.0373(5) Uani 1 1 d . . . H17 H 1.0223 0.8423 0.7977 0.045 Uiso 1 1 calc R . . C18 C 1.11622(13) 1.0201(2) 0.78331(12) 0.0355(4) Uani 1 1 d . . . H18 H 1.0966 1.0416 0.7275 0.043 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0241(2) 0.02250(19) 0.0222(2) 0.000 0.00093(13) 0.000 Ni2 0.0321(2) 0.0287(2) 0.0217(2) 0.000 0.00872(15) 0.000 S1 0.0594(4) 0.0534(4) 0.0303(3) 0.0107(2) -0.0016(3) -0.0282(3) O1 0.0333(7) 0.0328(7) 0.0347(7) -0.0116(6) -0.0013(5) 0.0001(6) O2 0.0279(7) 0.0424(8) 0.0449(8) -0.0145(7) 0.0047(6) -0.0037(6) O3 0.0461(9) 0.0490(9) 0.0265(8) -0.0108(6) 0.0159(6) -0.0173(6) O4 0.0400(7) 0.0360(7) 0.0272(7) -0.0082(6) 0.0061(5) -0.0077(6) O5 0.0279(7) 0.0796(12) 0.0421(9) -0.0091(8) -0.0028(6) -0.0103(8) O6 0.0371(8) 0.0471(9) 0.0329(9) -0.0076(6) 0.0147(7) -0.0011(6) O7 0.0652(10) 0.0409(8) 0.0356(8) 0.0101(7) 0.0143(7) 0.0137(8) N1 0.0278(8) 0.0309(8) 0.0295(8) 0.0040(6) 0.0055(6) -0.0007(6) N2 0.0321(8) 0.0294(8) 0.0260(8) 0.0038(6) -0.0017(6) -0.0037(6) N3 0.0235(8) 0.0365(9) 0.0293(9) -0.0021(6) 0.0039(7) 0.0012(6) C1 0.0333(10) 0.0277(9) 0.0233(9) -0.0032(7) 0.0044(7) -0.0023(7) C2 0.0292(9) 0.0266(9) 0.0246(9) -0.0024(7) 0.0012(7) 0.0000(7) C3 0.0309(9) 0.0321(10) 0.0221(9) -0.0056(7) 0.0049(7) 0.0028(7) C4 0.0241(9) 0.0289(9) 0.0245(10) 0.0009(7) 0.0046(7) 0.0017(7) C5 0.0282(9) 0.0262(9) 0.0204(8) -0.0011(7) 0.0006(7) -0.0012(7) C6 0.0316(10) 0.0241(9) 0.0211(9) -0.0008(6) 0.0048(7) 0.0006(7) C7 0.0286(9) 0.0287(9) 0.0253(9) -0.0002(7) 0.0058(7) -0.0025(7) C8 0.0336(10) 0.0255(9) 0.0210(9) -0.0009(7) 0.0054(7) -0.0021(7) C9 0.0272(10) 0.0337(11) 0.0504(12) -0.0026(9) 0.0061(8) 0.0017(8) C10 0.0405(11) 0.0307(10) 0.0497(12) -0.0040(9) 0.0102(9) 0.0001(9) C11 0.0389(10) 0.0348(10) 0.0322(10) 0.0102(8) 0.0040(8) -0.0114(8) C12 0.0287(10) 0.0482(12) 0.0327(10) 0.0085(9) 0.0082(8) -0.0028(8) C13 0.0307(10) 0.0412(11) 0.0278(9) 0.0033(8) 0.0093(7) 0.0004(8) C14 0.0420(11) 0.0417(11) 0.0288(10) 0.0039(8) -0.0071(8) -0.0163(9) C15 0.0467(11) 0.0459(12) 0.0242(9) 0.0089(8) -0.0075(8) -0.0147(9) C16 0.0344(10) 0.0285(10) 0.0300(9) 0.0057(8) 0.0016(7) -0.0053(8) C17 0.0370(10) 0.0384(11) 0.0348(10) 0.0058(8) -0.0107(8) -0.0117(9) C18 0.0391(11) 0.0388(11) 0.0272(9) 0.0076(8) -0.0097(8) -0.0100(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N2 2.0369(15) 3_777 ? Ni1 N2 2.0369(15) 4_576 ? Ni1 O1 2.0456(13) 2_657 ? Ni1 O1 2.0456(13) . ? Ni1 O2 2.2315(13) 2_657 ? Ni1 O2 2.2315(13) . ? Ni1 C1 2.4453(18) . ? Ni1 C1 2.4453(18) 2_657 ? Ni2 O3 2.0276(14) . ? Ni2 O3 2.0277(14) 2_656 ? Ni2 O7 2.1229(15) . ? Ni2 O7 2.1229(15) 2_656 ? Ni2 N1 2.1286(16) . ? Ni2 N1 2.1286(16) 2_656 ? S1 C16 1.7600(19) . ? S1 C11 1.789(2) . ? O1 C1 1.274(2) . ? O2 C1 1.254(2) . ? O3 C8 1.267(2) . ? O4 C8 1.245(2) . ? O5 N3 1.229(2) . ? O6 N3 1.222(2) . ? O7 H1W 0.8351 . ? O7 H2W 0.8283 . ? N1 C9 1.334(3) . ? N1 C13 1.351(2) . ? N2 C14 1.336(2) . ? N2 C18 1.339(2) . ? N2 Ni1 2.0369(15) 3_777 ? N3 C4 1.476(2) . ? C1 C2 1.499(2) . ? C2 C3 1.385(3) . ? C2 C7 1.393(2) . ? C3 C4 1.380(3) . ? C3 H3 0.9300 . ? C4 C5 1.386(3) . ? C5 C6 1.397(3) . ? C5 H5A 0.9300 . ? C6 C7 1.394(3) . ? C6 C8 1.521(2) . ? C7 H7A 0.9300 . ? C9 C10 1.388(3) . ? C9 H9 0.9300 . ? C10 C11 1.385(3) . ? C10 H10 0.9300 . ? C11 C12 1.386(3) . ? C12 C13 1.382(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.382(3) . ? C14 H14 0.9300 . ? C15 C16 1.388(3) . ? C15 H15 0.9300 . ? C16 C17 1.388(3) . ? C17 C18 1.379(3) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? 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 N2 Ni1 N2 91.83(9) 3_777 4_576 ? N2 Ni1 O1 95.45(6) 3_777 2_657 ? N2 Ni1 O1 105.95(6) 4_576 2_657 ? N2 Ni1 O1 105.95(6) 3_777 . ? N2 Ni1 O1 95.45(6) 4_576 . ? O1 Ni1 O1 149.18(8) 2_657 . ? N2 Ni1 O2 157.23(5) 3_777 2_657 ? N2 Ni1 O2 93.41(6) 4_576 2_657 ? O1 Ni1 O2 61.82(5) 2_657 2_657 ? O1 Ni1 O2 95.59(5) . 2_657 ? N2 Ni1 O2 93.41(6) 3_777 . ? N2 Ni1 O2 157.23(5) 4_576 . ? O1 Ni1 O2 95.59(5) 2_657 . ? O1 Ni1 O2 61.81(5) . . ? O2 Ni1 O2 90.28(8) 2_657 . ? N2 Ni1 C1 103.97(6) 3_777 . ? N2 Ni1 C1 126.74(6) 4_576 . ? O1 Ni1 C1 122.21(6) 2_657 . ? O1 Ni1 C1 31.39(6) . . ? O2 Ni1 C1 90.51(6) 2_657 . ? O2 Ni1 C1 30.66(5) . . ? N2 Ni1 C1 126.74(6) 3_777 2_657 ? N2 Ni1 C1 103.97(6) 4_576 2_657 ? O1 Ni1 C1 31.39(6) 2_657 2_657 ? O1 Ni1 C1 122.21(6) . 2_657 ? O2 Ni1 C1 30.66(5) 2_657 2_657 ? O2 Ni1 C1 90.52(6) . 2_657 ? C1 Ni1 C1 105.78(9) . 2_657 ? O3 Ni2 O3 177.64(8) . 2_656 ? O3 Ni2 O7 90.69(6) . . ? O3 Ni2 O7 91.02(6) 2_656 . ? O3 Ni2 O7 91.02(6) . 2_656 ? O3 Ni2 O7 90.68(6) 2_656 2_656 ? O7 Ni2 O7 87.22(9) . 2_656 ? O3 Ni2 N1 85.66(6) . . ? O3 Ni2 N1 92.78(6) 2_656 . ? O7 Ni2 N1 87.88(7) . . ? O7 Ni2 N1 174.05(6) 2_656 . ? O3 Ni2 N1 92.77(6) . 2_656 ? O3 Ni2 N1 85.66(6) 2_656 2_656 ? O7 Ni2 N1 174.05(6) . 2_656 ? O7 Ni2 N1 87.88(7) 2_656 2_656 ? N1 Ni2 N1 97.20(8) . 2_656 ? C16 S1 C11 103.83(9) . . ? C1 O1 Ni1 91.87(11) . . ? C1 O2 Ni1 84.13(10) . . ? C8 O3 Ni2 131.86(12) . . ? Ni2 O7 H1W 107.4 . . ? Ni2 O7 H2W 110.8 . . ? H1W O7 H2W 111.5 . . ? C9 N1 C13 116.83(17) . . ? C9 N1 Ni2 119.05(12) . . ? C13 N1 Ni2 123.52(13) . . ? C14 N2 C18 117.25(16) . . ? C14 N2 Ni1 122.89(12) . 3_777 ? C18 N2 Ni1 119.85(12) . 3_777 ? O6 N3 O5 123.51(16) . . ? O6 N3 C4 118.50(16) . . ? O5 N3 C4 117.99(16) . . ? O2 C1 O1 121.22(16) . . ? O2 C1 C2 121.44(16) . . ? O1 C1 C2 117.32(16) . . ? O2 C1 Ni1 65.20(10) . . ? O1 C1 Ni1 56.73(9) . . ? C2 C1 Ni1 168.15(13) . . ? C3 C2 C7 119.48(16) . . ? C3 C2 C1 118.34(15) . . ? C7 C2 C1 122.17(16) . . ? C4 C3 C2 119.07(16) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 122.75(17) . . ? C3 C4 N3 117.17(16) . . ? C5 C4 N3 120.06(16) . . ? C4 C5 C6 117.89(17) . . ? C4 C5 H5A 121.1 . . ? C6 C5 H5A 121.1 . . ? C7 C6 C5 119.89(16) . . ? C7 C6 C8 120.37(16) . . ? C5 C6 C8 119.69(16) . . ? C2 C7 C6 120.77(16) . . ? C2 C7 H7A 119.6 . . ? C6 C7 H7A 119.6 . . ? O4 C8 O3 126.48(16) . . ? O4 C8 C6 119.10(16) . . ? O3 C8 C6 114.40(15) . . ? N1 C9 C10 123.77(18) . . ? N1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C11 C10 C9 118.58(19) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 118.64(18) . . ? C10 C11 S1 119.17(17) . . ? C12 C11 S1 121.94(16) . . ? C13 C12 C11 118.80(18) . . ? C13 C12 H12 120.6 . . ? C11 C12 H12 120.6 . . ? N1 C13 C12 123.34(18) . . ? N1 C13 H13 118.3 . . ? C12 C13 H13 118.3 . . ? N2 C14 C15 123.54(17) . . ? N2 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? C14 C15 C16 118.45(17) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? C17 C16 C15 118.66(17) . . ? C17 C16 S1 125.21(15) . . ? C15 C16 S1 116.08(14) . . ? C18 C17 C16 118.57(17) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? N2 C18 C17 123.52(17) . . ? N2 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ni1 O1 C1 90.78(12) 3_777 . . . ? N2 Ni1 O1 C1 -175.74(11) 4_576 . . . ? O1 Ni1 O1 C1 -41.43(10) 2_657 . . . ? O2 Ni1 O1 C1 -81.77(11) 2_657 . . . ? O2 Ni1 O1 C1 5.54(10) . . . . ? C1 Ni1 O1 C1 -65.46(15) 2_657 . . . ? N2 Ni1 O2 C1 -111.94(11) 3_777 . . . ? N2 Ni1 O2 C1 -9.0(2) 4_576 . . . ? O1 Ni1 O2 C1 152.23(11) 2_657 . . . ? O1 Ni1 O2 C1 -5.66(10) . . . . ? O2 Ni1 O2 C1 90.53(11) 2_657 . . . ? C1 Ni1 O2 C1 121.20(11) 2_657 . . . ? O3 Ni2 O3 C8 123.24(18) 2_656 . . . ? O7 Ni2 O3 C8 -100.34(19) . . . . ? O7 Ni2 O3 C8 -13.10(19) 2_656 . . . ? N1 Ni2 O3 C8 171.84(19) . . . . ? N1 Ni2 O3 C8 74.82(19) 2_656 . . . ? O3 Ni2 N1 C9 -39.45(15) . . . . ? O3 Ni2 N1 C9 138.78(15) 2_656 . . . ? O7 Ni2 N1 C9 -130.30(15) . . . . ? O7 Ni2 N1 C9 -95.7(5) 2_656 . . . ? N1 Ni2 N1 C9 52.80(13) 2_656 . . . ? O3 Ni2 N1 C13 131.41(15) . . . . ? O3 Ni2 N1 C13 -50.36(14) 2_656 . . . ? O7 Ni2 N1 C13 40.56(14) . . . . ? O7 Ni2 N1 C13 75.2(6) 2_656 . . . ? N1 Ni2 N1 C13 -136.33(16) 2_656 . . . ? Ni1 O2 C1 O1 9.39(17) . . . . ? Ni1 O2 C1 C2 -168.86(16) . . . . ? Ni1 O1 C1 O2 -10.21(18) . . . . ? Ni1 O1 C1 C2 168.11(14) . . . . ? N2 Ni1 C1 O2 72.58(12) 3_777 . . . ? N2 Ni1 C1 O2 175.68(10) 4_576 . . . ? O1 Ni1 C1 O2 -33.23(13) 2_657 . . . ? O1 Ni1 C1 O2 170.39(17) . . . . ? O2 Ni1 C1 O2 -89.68(12) 2_657 . . . ? C1 Ni1 C1 O2 -62.73(10) 2_657 . . . ? N2 Ni1 C1 O1 -97.81(11) 3_777 . . . ? N2 Ni1 C1 O1 5.29(13) 4_576 . . . ? O1 Ni1 C1 O1 156.38(9) 2_657 . . . ? O2 Ni1 C1 O1 99.93(11) 2_657 . . . ? O2 Ni1 C1 O1 -170.39(17) . . . . ? C1 Ni1 C1 O1 126.88(12) 2_657 . . . ? N2 Ni1 C1 C2 -160.8(6) 3_777 . . . ? N2 Ni1 C1 C2 -57.7(7) 4_576 . . . ? O1 Ni1 C1 C2 93.4(6) 2_657 . . . ? O1 Ni1 C1 C2 -63.0(6) . . . . ? O2 Ni1 C1 C2 36.9(6) 2_657 . . . ? O2 Ni1 C1 C2 126.6(7) . . . . ? C1 Ni1 C1 C2 63.9(6) 2_657 . . . ? O2 C1 C2 C3 142.81(19) . . . . ? O1 C1 C2 C3 -35.5(2) . . . . ? Ni1 C1 C2 C3 21.5(7) . . . . ? O2 C1 C2 C7 -37.7(3) . . . . ? O1 C1 C2 C7 143.98(18) . . . . ? Ni1 C1 C2 C7 -159.0(6) . . . . ? C7 C2 C3 C4 -0.4(3) . . . . ? C1 C2 C3 C4 179.06(16) . . . . ? C2 C3 C4 C5 -2.9(3) . . . . ? C2 C3 C4 N3 178.50(17) . . . . ? O6 N3 C4 C3 -18.3(2) . . . . ? O5 N3 C4 C3 161.29(18) . . . . ? O6 N3 C4 C5 163.06(17) . . . . ? O5 N3 C4 C5 -17.4(3) . . . . ? C3 C4 C5 C6 3.2(3) . . . . ? N3 C4 C5 C6 -178.21(16) . . . . ? C4 C5 C6 C7 -0.3(3) . . . . ? C4 C5 C6 C8 -177.64(16) . . . . ? C3 C2 C7 C6 3.3(3) . . . . ? C1 C2 C7 C6 -176.17(16) . . . . ? C5 C6 C7 C2 -2.9(3) . . . . ? C8 C6 C7 C2 174.41(17) . . . . ? Ni2 O3 C8 O4 9.9(3) . . . . ? Ni2 O3 C8 C6 -168.71(12) . . . . ? C7 C6 C8 O4 176.98(17) . . . . ? C5 C6 C8 O4 -5.7(3) . . . . ? C7 C6 C8 O3 -4.3(3) . . . . ? C5 C6 C8 O3 173.06(17) . . . . ? C13 N1 C9 C10 -1.5(3) . . . . ? Ni2 N1 C9 C10 169.95(17) . . . . ? N1 C9 C10 C11 0.0(3) . . . . ? C9 C10 C11 C12 1.3(3) . . . . ? C9 C10 C11 S1 -173.13(16) . . . . ? C16 S1 C11 C10 -110.60(17) . . . . ? C16 S1 C11 C12 75.13(18) . . . . ? C10 C11 C12 C13 -1.1(3) . . . . ? S1 C11 C12 C13 173.17(15) . . . . ? C9 N1 C13 C12 1.7(3) . . . . ? Ni2 N1 C13 C12 -169.32(15) . . . . ? C11 C12 C13 N1 -0.4(3) . . . . ? C18 N2 C14 C15 -0.3(3) . . . . ? Ni1 N2 C14 C15 -179.30(17) 3_777 . . . ? N2 C14 C15 C16 -0.4(3) . . . . ? C14 C15 C16 C17 1.3(3) . . . . ? C14 C15 C16 S1 -176.28(17) . . . . ? C11 S1 C16 C17 12.7(2) . . . . ? C11 S1 C16 C15 -169.88(17) . . . . ? C15 C16 C17 C18 -1.5(3) . . . . ? S1 C16 C17 C18 175.84(17) . . . . ? C14 N2 C18 C17 0.0(3) . . . . ? Ni1 N2 C18 C17 179.11(16) 3_777 . . . ? C16 C17 C18 N2 0.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H1W O4 0.84 1.91 2.690(2) 153.9 2_656 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.287 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.061 # Attachment '3.cif' data_c _database_code_depnum_ccdc_archive 'CCDC 701847' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H22 N4 Ni O6 S2' _chemical_formula_weight 633.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.117(4) _cell_length_b 19.692(8) _cell_length_c 15.346(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.672(4) _cell_angle_gamma 90.00 _cell_volume 2929(2) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 5219 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6845 _exptl_absorpt_correction_T_max 0.8333 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22057 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 5446 _reflns_number_gt 4829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+1.9066P] 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 5446 _refine_ls_number_parameters 371 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.48207(3) 0.009444(11) 0.241134(16) 0.02702(8) Uani 1 1 d . . . S1 S -0.09779(7) 0.13922(4) -0.03665(6) 0.0747(2) Uani 1 1 d . . . S2 S 1.08067(6) -0.12910(3) 0.47083(4) 0.04575(15) Uani 1 1 d . . . O1 O 0.50565(15) 0.09585(6) 0.32011(8) 0.0321(3) Uani 1 1 d . . . O2 O 0.52248(18) 0.17635(7) 0.22176(9) 0.0433(4) Uani 1 1 d . . . O3 O 0.53384(15) 0.41863(6) 0.32399(9) 0.0327(3) Uani 1 1 d . . . O4 O 0.4553(3) 0.44128(8) 0.44140(13) 0.0806(7) Uani 1 1 d . . . O5 O 0.4994(2) 0.21643(7) 0.60388(9) 0.0519(4) Uani 1 1 d . . . H5 H 0.5062 0.2492 0.6378 0.078 Uiso 1 1 calc R . . O6 O 0.59601(16) 0.05360(7) 0.16301(9) 0.0399(3) Uani 1 1 d . . . H1W H 0.5798 0.0944 0.1581 0.060 Uiso 1 1 d R . . H2W H 0.5779 0.0352 0.1119 0.060 Uiso 1 1 d R . . N1 N 0.29511(18) 0.04758(8) 0.15143(11) 0.0363(4) Uani 1 1 d . . . N2 N 0.0238(3) 0.31275(18) -0.1931(2) 0.1038(10) Uani 1 1 d U . . N3 N 0.66983(17) -0.02862(8) 0.32591(11) 0.0315(4) Uani 1 1 d . . . N4 N 1.36162(16) -0.03466(8) 0.31866(10) 0.0295(3) Uani 1 1 d . . . C1 C 0.50535(19) 0.20990(9) 0.36763(12) 0.0254(4) Uani 1 1 d . . . C2 C 0.50064(19) 0.27858(9) 0.34621(12) 0.0269(4) Uani 1 1 d . . . H2 H 0.5025 0.2923 0.2886 0.032 Uiso 1 1 calc R . . C3 C 0.4931(2) 0.32671(9) 0.41059(12) 0.0284(4) Uani 1 1 d . . . C4 C 0.4889(2) 0.30627(9) 0.49622(12) 0.0332(4) Uani 1 1 d . . . H4 H 0.4798 0.3385 0.5384 0.040 Uiso 1 1 calc R . . C5 C 0.4982(2) 0.23818(9) 0.51929(12) 0.0325(4) Uani 1 1 d . . . C6 C 0.5048(2) 0.18991(9) 0.45467(12) 0.0303(4) Uani 1 1 d . . . H6A H 0.5088 0.1440 0.4695 0.036 Uiso 1 1 calc R . . C7 C 0.51164(19) 0.15709(9) 0.29734(12) 0.0271(4) Uani 1 1 d . . . C8 C 0.4915(2) 0.40158(9) 0.39035(13) 0.0370(5) Uani 1 1 d . . . C9 C 0.2093(3) 0.08615(12) 0.18201(16) 0.0507(6) Uani 1 1 d . . . H9 H 0.2308 0.0939 0.2443 0.061 Uiso 1 1 calc R . . C10 C 0.0910(3) 0.11504(14) 0.12674(18) 0.0577(7) Uani 1 1 d . . . H10 H 0.0344 0.1415 0.1513 0.069 Uiso 1 1 calc R . . C11 C 0.0582(2) 0.10399(13) 0.03470(17) 0.0516(6) Uani 1 1 d . . . C12 C 0.1439(3) 0.06304(14) 0.00214(16) 0.0552(6) Uani 1 1 d . . . H12 H 0.1230 0.0536 -0.0597 0.066 Uiso 1 1 calc R . . C13 C 0.2611(2) 0.03618(11) 0.06223(14) 0.0438(5) Uani 1 1 d . . . H13 H 0.3187 0.0090 0.0394 0.053 Uiso 1 1 calc R . . C14 C 0.1203(4) 0.2748(2) -0.1363(3) 0.1086(13) Uani 1 1 d U . . H14 H 0.2122 0.2854 -0.1300 0.130 Uiso 1 1 calc R . . C15 C 0.0940(3) 0.22168(18) -0.0869(2) 0.0785(9) Uani 1 1 d U . . H15 H 0.1660 0.1974 -0.0481 0.094 Uiso 1 1 calc R . . C16 C -0.0407(2) 0.20467(13) -0.09552(15) 0.0488(6) Uani 1 1 d U . . C17 C -0.1422(3) 0.24337(13) -0.15365(17) 0.0538(6) Uani 1 1 d U . . H17 H -0.2349 0.2340 -0.1611 0.065 Uiso 1 1 calc R . . C18 C -0.1050(3) 0.29538(17) -0.2000(2) 0.0742(8) Uani 1 1 d U . . H18 H -0.1750 0.3205 -0.2392 0.089 Uiso 1 1 calc R . . C19 C 0.7893(2) 0.00361(10) 0.33441(15) 0.0385(5) Uani 1 1 d . . . H19 H 0.7861 0.0470 0.3101 0.046 Uiso 1 1 calc R . . C20 C 0.9162(2) -0.02368(11) 0.37692(16) 0.0416(5) Uani 1 1 d . . . H20 H 0.9963 0.0009 0.3809 0.050 Uiso 1 1 calc R . . C21 C 0.9236(2) -0.08812(10) 0.41373(14) 0.0361(5) Uani 1 1 d . . . C22 C 0.8005(2) -0.12136(11) 0.40756(16) 0.0419(5) Uani 1 1 d . . . H22 H 0.8009 -0.1642 0.4332 0.050 Uiso 1 1 calc R . . C23 C 0.6780(2) -0.09055(10) 0.36327(15) 0.0375(5) Uani 1 1 d . . . H23 H 0.5964 -0.1138 0.3590 0.045 Uiso 1 1 calc R . . C24 C 1.2763(3) -0.08545(13) 0.28435(17) 0.0557(7) Uani 1 1 d . . . H24 H 1.2744 -0.1020 0.2272 0.067 Uiso 1 1 calc R . . C25 C 1.1904(3) -0.11504(13) 0.32852(17) 0.0568(7) Uani 1 1 d . . . H25 H 1.1324 -0.1505 0.3016 0.068 Uiso 1 1 calc R . . C26 C 1.1915(2) -0.09163(10) 0.41240(14) 0.0350(4) Uani 1 1 d . . . C27 C 1.2809(3) -0.04011(12) 0.44939(14) 0.0469(6) Uani 1 1 d . . . H27 H 1.2866 -0.0237 0.5072 0.056 Uiso 1 1 calc R . . C28 C 1.3620(2) -0.01283(11) 0.40007(14) 0.0397(5) Uani 1 1 d . . . H28 H 1.4204 0.0230 0.4255 0.048 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.04108(15) 0.01639(12) 0.02726(13) -0.00124(9) 0.01569(10) 0.00096(9) S1 0.0412(4) 0.0902(6) 0.0814(5) 0.0305(4) -0.0006(3) -0.0041(3) S2 0.0405(3) 0.0506(3) 0.0505(3) 0.0222(3) 0.0201(3) 0.0046(2) O1 0.0548(9) 0.0159(6) 0.0287(7) -0.0018(5) 0.0167(6) -0.0006(6) O2 0.0865(12) 0.0209(7) 0.0296(7) 0.0001(5) 0.0282(8) 0.0029(7) O3 0.0539(9) 0.0193(6) 0.0312(7) 0.0040(5) 0.0222(6) 0.0006(6) O4 0.185(2) 0.0197(8) 0.0736(12) -0.0012(8) 0.0949(15) 0.0043(10) O5 0.1125(14) 0.0236(7) 0.0266(7) -0.0003(6) 0.0311(8) -0.0098(8) O6 0.0647(10) 0.0240(7) 0.0377(8) 0.0004(6) 0.0256(7) -0.0022(6) N1 0.0487(10) 0.0282(9) 0.0329(9) -0.0006(7) 0.0131(8) 0.0023(7) N2 0.0820(19) 0.123(3) 0.104(2) 0.0577(19) 0.0239(17) 0.0042(18) N3 0.0403(9) 0.0226(8) 0.0352(9) 0.0004(6) 0.0164(7) -0.0005(7) N4 0.0349(9) 0.0259(8) 0.0295(8) -0.0019(6) 0.0124(7) -0.0004(7) C1 0.0332(10) 0.0191(8) 0.0253(9) -0.0017(7) 0.0103(7) -0.0008(7) C2 0.0409(10) 0.0202(9) 0.0237(9) 0.0004(7) 0.0158(8) -0.0016(7) C3 0.0433(11) 0.0182(9) 0.0275(9) -0.0011(7) 0.0161(8) -0.0034(8) C4 0.0580(13) 0.0203(9) 0.0264(9) -0.0051(7) 0.0201(9) -0.0060(8) C5 0.0536(12) 0.0232(9) 0.0234(9) 0.0004(7) 0.0154(9) -0.0063(8) C6 0.0467(11) 0.0167(8) 0.0285(10) 0.0014(7) 0.0124(8) -0.0018(8) C7 0.0379(10) 0.0200(9) 0.0247(9) -0.0006(7) 0.0111(8) 0.0013(7) C8 0.0683(14) 0.0186(9) 0.0321(10) -0.0021(8) 0.0273(10) -0.0035(9) C9 0.0578(15) 0.0501(14) 0.0417(13) -0.0077(10) 0.0102(11) 0.0140(11) C10 0.0556(15) 0.0567(15) 0.0577(15) -0.0066(12) 0.0116(12) 0.0162(12) C11 0.0444(13) 0.0512(14) 0.0538(14) 0.0089(11) 0.0056(11) -0.0015(11) C12 0.0615(16) 0.0665(16) 0.0335(12) 0.0011(11) 0.0073(11) -0.0047(13) C13 0.0569(14) 0.0405(12) 0.0365(12) 0.0007(9) 0.0171(10) 0.0005(10) C14 0.0608(19) 0.144(3) 0.119(3) 0.063(3) 0.0234(19) -0.006(2) C15 0.0468(15) 0.102(2) 0.081(2) 0.0374(18) 0.0094(14) 0.0037(15) C16 0.0420(12) 0.0589(15) 0.0411(12) -0.0030(11) 0.0050(10) 0.0032(11) C17 0.0467(13) 0.0579(15) 0.0519(14) -0.0060(11) 0.0064(11) 0.0098(11) C18 0.0710(18) 0.079(2) 0.0659(18) 0.0154(15) 0.0088(15) 0.0188(16) C19 0.0445(12) 0.0258(10) 0.0487(12) 0.0060(9) 0.0190(10) -0.0034(9) C20 0.0383(12) 0.0358(11) 0.0544(13) 0.0082(10) 0.0191(10) -0.0066(9) C21 0.0396(11) 0.0354(11) 0.0384(11) 0.0055(8) 0.0190(9) 0.0017(9) C22 0.0459(12) 0.0294(11) 0.0546(13) 0.0143(9) 0.0210(11) 0.0001(9) C23 0.0393(11) 0.0289(10) 0.0479(12) 0.0077(9) 0.0180(10) -0.0033(8) C24 0.0722(17) 0.0585(15) 0.0489(14) -0.0267(12) 0.0372(13) -0.0315(13) C25 0.0645(16) 0.0572(15) 0.0587(15) -0.0228(12) 0.0338(13) -0.0312(13) C26 0.0335(10) 0.0353(11) 0.0382(11) 0.0091(8) 0.0138(9) 0.0036(8) C27 0.0623(15) 0.0535(14) 0.0296(11) -0.0069(10) 0.0210(10) -0.0136(11) C28 0.0512(13) 0.0405(12) 0.0292(10) -0.0073(9) 0.0142(9) -0.0149(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 O3 2.0325(14) 2_645 ? Ni1 O1 2.0627(13) . ? Ni1 O6 2.0773(14) . ? Ni1 N3 2.1083(18) . ? Ni1 N4 2.1181(16) 1_455 ? Ni1 N1 2.1313(18) . ? S1 C16 1.764(3) . ? S1 C11 1.783(2) . ? S2 C21 1.773(2) . ? S2 C26 1.784(2) . ? O1 C7 1.262(2) . ? O2 C7 1.255(2) . ? O3 C8 1.258(2) . ? O3 Ni1 2.0325(14) 2_655 ? O4 C8 1.234(2) . ? O5 C5 1.364(2) . ? O5 H5 0.8200 . ? O6 H1W 0.8200 . ? O6 H2W 0.8361 . ? N1 C13 1.331(3) . ? N1 C9 1.336(3) . ? N2 C18 1.321(4) . ? N2 C14 1.336(4) . ? N3 C19 1.338(3) . ? N3 C23 1.340(2) . ? N4 C28 1.320(2) . ? N4 C24 1.328(3) . ? N4 Ni1 2.1181(16) 1_655 ? C1 C2 1.389(3) . ? C1 C6 1.394(3) . ? C1 C7 1.513(2) . ? C2 C3 1.387(2) . ? C2 H2 0.9300 . ? C3 C4 1.387(3) . ? C3 C8 1.506(3) . ? C4 C5 1.383(3) . ? C4 H4 0.9300 . ? C5 C6 1.389(3) . ? C6 H6A 0.9300 . ? C9 C10 1.376(3) . ? C9 H9 0.9300 . ? C10 C11 1.372(4) . ? C10 H10 0.9300 . ? C11 C12 1.378(4) . ? C12 C13 1.382(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.361(4) . ? C14 H14 0.9300 . ? C15 C16 1.373(4) . ? C15 H15 0.9300 . ? C16 C17 1.380(3) . ? C17 C18 1.360(4) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.372(3) . ? C19 H19 0.9300 . ? C20 C21 1.382(3) . ? C20 H20 0.9300 . ? C21 C22 1.386(3) . ? C22 C23 1.372(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.375(3) . ? C24 H24 0.9300 . ? C25 C26 1.364(3) . ? C25 H25 0.9300 . ? C26 C27 1.369(3) . ? C27 C28 1.376(3) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? 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 O3 Ni1 O1 173.84(5) 2_645 . ? O3 Ni1 O6 93.63(6) 2_645 . ? O1 Ni1 O6 90.23(6) . . ? O3 Ni1 N3 85.46(6) 2_645 . ? O1 Ni1 N3 89.93(6) . . ? O6 Ni1 N3 87.36(7) . . ? O3 Ni1 N4 86.46(6) 2_645 1_455 ? O1 Ni1 N4 89.80(6) . 1_455 ? O6 Ni1 N4 178.66(6) . 1_455 ? N3 Ni1 N4 93.98(7) . 1_455 ? O3 Ni1 N1 93.56(6) 2_645 . ? O1 Ni1 N1 91.17(6) . . ? O6 Ni1 N1 90.94(7) . . ? N3 Ni1 N1 177.98(6) . . ? N4 Ni1 N1 87.72(7) 1_455 . ? C16 S1 C11 103.68(12) . . ? C21 S2 C26 99.61(10) . . ? C7 O1 Ni1 129.22(12) . . ? C8 O3 Ni1 129.44(12) . 2_655 ? C5 O5 H5 109.5 . . ? Ni1 O6 H1W 109.5 . . ? Ni1 O6 H2W 110.6 . . ? H1W O6 H2W 110.8 . . ? C13 N1 C9 117.1(2) . . ? C13 N1 Ni1 121.61(15) . . ? C9 N1 Ni1 121.28(15) . . ? C18 N2 C14 115.3(3) . . ? C19 N3 C23 116.55(18) . . ? C19 N3 Ni1 121.36(13) . . ? C23 N3 Ni1 121.44(14) . . ? C28 N4 C24 116.47(17) . . ? C28 N4 Ni1 123.50(13) . 1_655 ? C24 N4 Ni1 119.98(14) . 1_655 ? C2 C1 C6 119.49(16) . . ? C2 C1 C7 120.40(15) . . ? C6 C1 C7 120.11(16) . . ? C3 C2 C1 120.12(16) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C4 C3 C2 119.97(16) . . ? C4 C3 C8 118.56(16) . . ? C2 C3 C8 121.45(16) . . ? C5 C4 C3 120.38(16) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? O5 C5 C4 121.97(16) . . ? O5 C5 C6 118.40(16) . . ? C4 C5 C6 119.63(17) . . ? C5 C6 C1 120.33(17) . . ? C5 C6 H6A 119.8 . . ? C1 C6 H6A 119.8 . . ? O2 C7 O1 124.67(16) . . ? O2 C7 C1 118.95(15) . . ? O1 C7 C1 116.38(15) . . ? O4 C8 O3 125.21(18) . . ? O4 C8 C3 118.48(17) . . ? O3 C8 C3 116.22(16) . . ? N1 C9 C10 123.8(2) . . ? N1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C11 C10 C9 118.6(2) . . ? C11 C10 H10 120.7 . . ? C9 C10 H10 120.7 . . ? C10 C11 C12 118.3(2) . . ? C10 C11 S1 118.7(2) . . ? C12 C11 S1 122.9(2) . . ? C11 C12 C13 119.4(2) . . ? C11 C12 H12 120.3 . . ? C13 C12 H12 120.3 . . ? N1 C13 C12 122.7(2) . . ? N1 C13 H13 118.6 . . ? C12 C13 H13 118.6 . . ? N2 C14 C15 124.7(3) . . ? N2 C14 H14 117.6 . . ? C15 C14 H14 117.6 . . ? C14 C15 C16 118.8(3) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C15 C16 C17 117.5(3) . . ? C15 C16 S1 126.2(2) . . ? C17 C16 S1 116.26(19) . . ? C18 C17 C16 119.2(3) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? N2 C18 C17 124.6(3) . . ? N2 C18 H18 117.7 . . ? C17 C18 H18 117.7 . . ? N3 C19 C20 123.83(19) . . ? N3 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? C19 C20 C21 119.16(19) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C20 C21 C22 117.61(19) . . ? C20 C21 S2 123.73(16) . . ? C22 C21 S2 118.63(16) . . ? C23 C22 C21 119.42(19) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? N3 C23 C22 123.40(19) . . ? N3 C23 H23 118.3 . . ? C22 C23 H23 118.3 . . ? N4 C24 C25 123.7(2) . . ? N4 C24 H24 118.2 . . ? C25 C24 H24 118.2 . . ? C26 C25 C24 119.1(2) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 117.86(19) . . ? C25 C26 S2 119.89(17) . . ? C27 C26 S2 122.24(16) . . ? C26 C27 C28 119.25(19) . . ? C26 C27 H27 120.4 . . ? C28 C27 H27 120.4 . . ? N4 C28 C27 123.59(19) . . ? N4 C28 H28 118.2 . . ? C27 C28 H28 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Ni1 O1 C7 163.0(5) 2_645 . . . ? O6 Ni1 O1 C7 34.16(17) . . . . ? N3 Ni1 O1 C7 121.52(17) . . . . ? N4 Ni1 O1 C7 -144.50(17) 1_455 . . . ? N1 Ni1 O1 C7 -56.78(17) . . . . ? O3 Ni1 N1 C13 -40.41(17) 2_645 . . . ? O1 Ni1 N1 C13 143.53(16) . . . . ? O6 Ni1 N1 C13 53.28(17) . . . . ? N3 Ni1 N1 C13 20.5(18) . . . . ? N4 Ni1 N1 C13 -126.72(17) 1_455 . . . ? O3 Ni1 N1 C9 142.10(17) 2_645 . . . ? O1 Ni1 N1 C9 -33.96(18) . . . . ? O6 Ni1 N1 C9 -124.21(18) . . . . ? N3 Ni1 N1 C9 -157.0(17) . . . . ? N4 Ni1 N1 C9 55.79(18) 1_455 . . . ? O3 Ni1 N3 C19 121.79(16) 2_645 . . . ? O1 Ni1 N3 C19 -62.30(16) . . . . ? O6 Ni1 N3 C19 27.93(16) . . . . ? N4 Ni1 N3 C19 -152.09(16) 1_455 . . . ? N1 Ni1 N3 C19 60.8(18) . . . . ? O3 Ni1 N3 C23 -48.58(15) 2_645 . . . ? O1 Ni1 N3 C23 127.33(15) . . . . ? O6 Ni1 N3 C23 -142.44(15) . . . . ? N4 Ni1 N3 C23 37.54(15) 1_455 . . . ? N1 Ni1 N3 C23 -109.6(17) . . . . ? C6 C1 C2 C3 -1.1(3) . . . . ? C7 C1 C2 C3 179.20(17) . . . . ? C1 C2 C3 C4 -0.7(3) . . . . ? C1 C2 C3 C8 178.44(18) . . . . ? C2 C3 C4 C5 2.8(3) . . . . ? C8 C3 C4 C5 -176.3(2) . . . . ? C3 C4 C5 O5 177.6(2) . . . . ? C3 C4 C5 C6 -3.2(3) . . . . ? O5 C5 C6 C1 -179.33(19) . . . . ? C4 C5 C6 C1 1.5(3) . . . . ? C2 C1 C6 C5 0.6(3) . . . . ? C7 C1 C6 C5 -179.62(18) . . . . ? Ni1 O1 C7 O2 -10.1(3) . . . . ? Ni1 O1 C7 C1 170.05(12) . . . . ? C2 C1 C7 O2 5.0(3) . . . . ? C6 C1 C7 O2 -174.71(19) . . . . ? C2 C1 C7 O1 -175.08(17) . . . . ? C6 C1 C7 O1 5.2(3) . . . . ? Ni1 O3 C8 O4 -15.7(4) 2_655 . . . ? Ni1 O3 C8 C3 167.70(13) 2_655 . . . ? C4 C3 C8 O4 -16.3(3) . . . . ? C2 C3 C8 O4 164.6(2) . . . . ? C4 C3 C8 O3 160.6(2) . . . . ? C2 C3 C8 O3 -18.5(3) . . . . ? C13 N1 C9 C10 -1.1(4) . . . . ? Ni1 N1 C9 C10 176.5(2) . . . . ? N1 C9 C10 C11 -0.1(4) . . . . ? C9 C10 C11 C12 1.5(4) . . . . ? C9 C10 C11 S1 178.1(2) . . . . ? C16 S1 C11 C10 109.2(2) . . . . ? C16 S1 C11 C12 -74.4(2) . . . . ? C10 C11 C12 C13 -1.8(4) . . . . ? S1 C11 C12 C13 -178.22(19) . . . . ? C9 N1 C13 C12 0.8(3) . . . . ? Ni1 N1 C13 C12 -176.81(18) . . . . ? C11 C12 C13 N1 0.7(4) . . . . ? C18 N2 C14 C15 -0.4(7) . . . . ? N2 C14 C15 C16 0.5(7) . . . . ? C14 C15 C16 C17 -0.6(5) . . . . ? C14 C15 C16 S1 -178.6(3) . . . . ? C11 S1 C16 C15 1.0(3) . . . . ? C11 S1 C16 C17 -177.07(19) . . . . ? C15 C16 C17 C18 0.7(4) . . . . ? S1 C16 C17 C18 178.9(2) . . . . ? C14 N2 C18 C17 0.4(6) . . . . ? C16 C17 C18 N2 -0.6(5) . . . . ? C23 N3 C19 C20 1.3(3) . . . . ? Ni1 N3 C19 C20 -169.54(17) . . . . ? N3 C19 C20 C21 -0.1(3) . . . . ? C19 C20 C21 C22 -1.6(3) . . . . ? C19 C20 C21 S2 -179.70(17) . . . . ? C26 S2 C21 C20 -30.1(2) . . . . ? C26 S2 C21 C22 151.86(18) . . . . ? C20 C21 C22 C23 2.1(3) . . . . ? S2 C21 C22 C23 -179.71(17) . . . . ? C19 N3 C23 C22 -0.7(3) . . . . ? Ni1 N3 C23 C22 170.07(17) . . . . ? C21 C22 C23 N3 -1.0(3) . . . . ? C28 N4 C24 C25 0.4(4) . . . . ? Ni1 N4 C24 C25 -177.2(2) 1_655 . . . ? N4 C24 C25 C26 0.0(4) . . . . ? C24 C25 C26 C27 -1.2(4) . . . . ? C24 C25 C26 S2 179.8(2) . . . . ? C21 S2 C26 C25 -79.3(2) . . . . ? C21 S2 C26 C27 101.8(2) . . . . ? C25 C26 C27 C28 2.0(4) . . . . ? S2 C26 C27 C28 -179.05(18) . . . . ? C24 N4 C28 C27 0.5(3) . . . . ? Ni1 N4 C28 C27 178.01(18) 1_655 . . . ? C26 C27 C28 N4 -1.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O6 H2W O4 0.84 2.59 3.290(3) 141.4 4_565 O6 H2W O4 0.84 2.01 2.693(2) 138.3 2_645 O6 H1W O2 0.82 2.05 2.756(2) 143.4 . O5 H5 O2 0.82 1.93 2.746(2) 177.5 4_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.564 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.044 # Attachment '4.cif' data_e _database_code_depnum_ccdc_archive 'CCDC 701848' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H42N4 Ni2O9 S2' _chemical_formula_weight 952.36 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 Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 15.3099(10) _cell_length_b 27.9468(18) _cell_length_c 15.7112(10) _cell_angle_alpha 90.00 _cell_angle_beta 114.8620(10) _cell_angle_gamma 90.00 _cell_volume 6099.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 291(2) _cell_measurement_reflns_used 9065 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 25.92 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.037 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7380 _exptl_absorpt_correction_T_max 0.8078 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 291(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22314 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 25.50 _reflns_number_total 10908 _reflns_number_gt 10042 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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.The carbon atoms of tert-butyl groups have departed into two parts and their site occupation was refined by programme. The restraints are needed to restrict the large Ueq of tert-butyl groups. ; _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^)+(0.1061P)^2^+2.3998P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.003(14) _refine_ls_number_reflns 10908 _refine_ls_number_parameters 570 _refine_ls_number_restraints 237 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1506 _refine_ls_wR_factor_gt 0.1458 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.088 _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 C10 C 0.5395(16) 0.0090(8) 0.2055(14) 0.129(5) Uani 0.562(11) 1 d PDU A 1 H10A H 0.6053 -0.0009 0.2259 0.193 Uiso 0.562(11) 1 calc PR A 1 H10B H 0.5362 0.0433 0.2050 0.193 Uiso 0.562(11) 1 calc PR A 1 H10C H 0.5020 -0.0030 0.1435 0.193 Uiso 0.562(11) 1 calc PR A 1 C11 C 0.545(2) 0.0179(8) 0.3637(12) 0.179(6) Uani 0.562(11) 1 d PDU A 1 H11A H 0.6095 0.0065 0.4000 0.268 Uiso 0.562(11) 1 calc PR A 1 H11B H 0.5076 0.0140 0.3989 0.268 Uiso 0.562(11) 1 calc PR A 1 H11C H 0.5475 0.0511 0.3494 0.268 Uiso 0.562(11) 1 calc PR A 1 C12 C 0.535(2) -0.0620(5) 0.2953(17) 0.148(5) Uani 0.562(11) 1 d PDU A 1 H12A H 0.6036 -0.0623 0.3288 0.223 Uiso 0.562(11) 1 calc PR A 1 H12B H 0.5163 -0.0799 0.2382 0.223 Uiso 0.562(11) 1 calc PR A 1 H12C H 0.5065 -0.0763 0.3334 0.223 Uiso 0.562(11) 1 calc PR A 1 C10' C 0.544(2) 0.0376(7) 0.2697(19) 0.129(5) Uani 0.438(11) 1 d PDU A 2 H10D H 0.6070 0.0397 0.3210 0.193 Uiso 0.438(11) 1 calc PR A 2 H10E H 0.5041 0.0627 0.2748 0.193 Uiso 0.438(11) 1 calc PR A 2 H10F H 0.5504 0.0408 0.2115 0.193 Uiso 0.438(11) 1 calc PR A 2 C11' C 0.548(3) -0.0336(10) 0.3687(13) 0.179(6) Uani 0.438(11) 1 d PDU A 2 H11D H 0.5618 -0.0665 0.3622 0.268 Uiso 0.438(11) 1 calc PR A 2 H11E H 0.5051 -0.0318 0.3994 0.268 Uiso 0.438(11) 1 calc PR A 2 H11F H 0.6063 -0.0169 0.4055 0.268 Uiso 0.438(11) 1 calc PR A 2 C12' C 0.500(3) -0.0439(9) 0.1958(17) 0.148(5) Uani 0.438(11) 1 d PDU A 2 H12D H 0.5613 -0.0595 0.2168 0.223 Uiso 0.438(11) 1 calc PR A 2 H12E H 0.4885 -0.0256 0.1404 0.223 Uiso 0.438(11) 1 calc PR A 2 H12F H 0.4502 -0.0674 0.1819 0.223 Uiso 0.438(11) 1 calc PR A 2 C22 C -0.3487(8) 0.2690(4) -0.0686(5) 0.106(3) Uani 0.923(10) 1 d PDU B 1 H22A H -0.3263 0.3002 -0.0757 0.158 Uiso 0.923(10) 1 calc PR B 1 H22B H -0.2946 0.2482 -0.0378 0.158 Uiso 0.923(10) 1 calc PR B 1 H22C H -0.3850 0.2714 -0.0317 0.158 Uiso 0.923(10) 1 calc PR B 1 C23 C -0.4415(7) 0.1958(3) -0.1542(7) 0.109(3) Uani 0.923(10) 1 d PDU B 1 H23A H -0.4714 0.1955 -0.1114 0.163 Uiso 0.923(10) 1 calc PR B 1 H23B H -0.3846 0.1764 -0.1297 0.163 Uiso 0.923(10) 1 calc PR B 1 H23C H -0.4856 0.1834 -0.2138 0.163 Uiso 0.923(10) 1 calc PR B 1 C24 C -0.5044(6) 0.2787(4) -0.2146(7) 0.108(3) Uani 0.923(10) 1 d PDU B 1 H24A H -0.5394 0.2793 -0.1762 0.161 Uiso 0.923(10) 1 calc PR B 1 H24B H -0.5442 0.2652 -0.2746 0.161 Uiso 0.923(10) 1 calc PR B 1 H24C H -0.4866 0.3107 -0.2228 0.161 Uiso 0.923(10) 1 calc PR B 1 C22' C -0.3620(12) 0.2179(4) -0.0774(6) 0.106(3) Uani 0.077(10) 1 d PDU B 2 H22D H -0.2937 0.2199 -0.0576 0.158 Uiso 0.077(10) 1 calc PR B 2 H22E H -0.3822 0.1851 -0.0905 0.158 Uiso 0.077(10) 1 calc PR B 2 H22F H -0.3781 0.2297 -0.0284 0.158 Uiso 0.077(10) 1 calc PR B 2 C23' C -0.5145(6) 0.2272(4) -0.2190(13) 0.109(3) Uani 0.077(10) 1 d PDU B 2 H23D H -0.5560 0.2506 -0.2616 0.163 Uiso 0.077(10) 1 calc PR B 2 H23E H -0.5396 0.2183 -0.1746 0.163 Uiso 0.077(10) 1 calc PR B 2 H23F H -0.5112 0.1995 -0.2536 0.163 Uiso 0.077(10) 1 calc PR B 2 C24' C -0.4232(10) 0.2988(5) -0.1360(9) 0.108(3) Uani 0.077(10) 1 d PDU B 2 H24D H -0.4640 0.2985 -0.1033 0.161 Uiso 0.077(10) 1 calc PR B 2 H24E H -0.4510 0.3192 -0.1900 0.161 Uiso 0.077(10) 1 calc PR B 2 H24F H -0.3607 0.3107 -0.0950 0.161 Uiso 0.077(10) 1 calc PR B 2 Ni1 Ni -0.00008(4) 0.118199(18) -0.05227(4) 0.02424(14) Uani 1 1 d . . . Ni2 Ni 0.21592(3) 0.140853(18) -0.07066(3) 0.02415(14) Uani 1 1 d . . . S1 S 0.68448(9) 0.18504(5) 0.13051(10) 0.0451(3) Uani 1 1 d U . . S2 S -0.23921(14) 0.07197(8) 0.20661(15) 0.0788(7) Uani 1 1 d U . . O1 O 0.0988(2) 0.07122(13) 0.0347(2) 0.0382(8) Uani 1 1 d . . . O2 O 0.2368(3) 0.08753(13) 0.0237(3) 0.0428(8) Uani 1 1 d . . . O3 O 0.1035(3) -0.05758(16) 0.2638(3) 0.0581(12) Uani 1 1 d . . . O4 O 0.2454(2) -0.09261(12) 0.3452(2) 0.0372(8) Uani 1 1 d . . . O5 O -0.1114(2) 0.16299(13) -0.1362(2) 0.0392(8) Uani 1 1 d . . . O6 O -0.0684(3) 0.18801(16) -0.2478(3) 0.0532(10) Uani 1 1 d . . . O7 O -0.2944(2) 0.30844(12) -0.4817(2) 0.0356(7) Uani 1 1 d . . . O8 O -0.4303(3) 0.32599(14) -0.4688(3) 0.0444(9) Uani 1 1 d . . . O9 O 0.0677(2) 0.12709(11) -0.1431(2) 0.0277(6) Uani 1 1 d . . . H9A H 0.0375 0.1534 -0.1856 0.042 Uiso 1 1 d R . . H9B H 0.0586 0.0983 -0.1804 0.042 Uiso 1 1 d R . . N1 N -0.0752(3) 0.10911(14) 0.0326(3) 0.0309(8) Uani 1 1 d . . . N2 N -0.0758(3) -0.05875(14) 0.3682(3) 0.0344(9) Uani 1 1 d . . . N3 N 0.3637(3) 0.15414(14) -0.0067(2) 0.0290(8) Uani 1 1 d . . . N4 N 0.7020(3) 0.30503(14) 0.3326(3) 0.0334(8) Uani 1 1 d . . . C1 C 0.1873(3) 0.06593(16) 0.0576(3) 0.0309(10) Uani 1 1 d . . . C2 C 0.2381(4) 0.02982(18) 0.1334(4) 0.0393(11) Uani 1 1 d . . . C3 C 0.1911(3) 0.00233(17) 0.1730(3) 0.0327(10) Uani 1 1 d . . . H3 H 0.1251 0.0060 0.1535 0.039 Uiso 1 1 calc R . . C4 C 0.2413(4) -0.03128(19) 0.2425(4) 0.0416(12) Uani 1 1 d . . . C5 C 0.3408(5) -0.0352(3) 0.2695(6) 0.082(3) Uani 1 1 d . . . H5 H 0.3747 -0.0576 0.3154 0.098 Uiso 1 1 calc R . . C6 C 0.3898(5) -0.0089(4) 0.2335(7) 0.097(3) Uani 1 1 d U A . C7 C 0.3376(4) 0.0251(3) 0.1651(6) 0.084(3) Uani 1 1 d . . . H7 H 0.3700 0.0448 0.1404 0.101 Uiso 1 1 calc R . . C8 C 0.1926(4) -0.06304(18) 0.2874(3) 0.0368(11) Uani 1 1 d . . . C9 C 0.4998(7) -0.0107(4) 0.2724(8) 0.118(3) Uani 1 1 d DU . . C13 C -0.1228(3) 0.18763(17) -0.2068(3) 0.0338(10) Uani 1 1 d . . . C14 C -0.2131(4) 0.21826(19) -0.2445(4) 0.0406(11) Uani 1 1 d . . . C15 C -0.2383(3) 0.24633(18) -0.3256(3) 0.0339(10) Uani 1 1 d . . . H15 H -0.1991 0.2467 -0.3576 0.041 Uiso 1 1 calc R . . C16 C -0.3209(4) 0.27307(19) -0.3573(4) 0.0380(11) Uani 1 1 d . . . C17 C -0.3792(5) 0.2731(3) -0.3086(5) 0.0615(18) Uani 1 1 d . . . H17 H -0.4352 0.2913 -0.3306 0.074 Uiso 1 1 calc R . . C18 C -0.3543(5) 0.2471(3) -0.2303(5) 0.074(2) Uani 1 1 d D B . C19 C -0.2708(5) 0.2199(3) -0.1967(5) 0.0647(19) Uani 1 1 d . . . H19 H -0.2534 0.2026 -0.1415 0.078 Uiso 1 1 calc R . . C20 C -0.3512(3) 0.30472(16) -0.4434(3) 0.0284(9) Uani 1 1 d . . . C21 C -0.4138(5) 0.2483(2) -0.1669(5) 0.093(3) Uani 1 1 d D . . C25 C -0.1713(4) 0.10771(19) -0.0065(4) 0.0400(11) Uani 1 1 d . . . H25 H -0.2042 0.1156 -0.0696 0.048 Uiso 1 1 calc R . . C26 C -0.2238(4) 0.09493(19) 0.0435(4) 0.0395(11) Uani 1 1 d . . . H26 H -0.2906 0.0931 0.0143 0.047 Uiso 1 1 calc R . . C27 C -0.1740(4) 0.0850(2) 0.1382(4) 0.0458(13) Uani 1 1 d . . . C28 C -0.0765(5) 0.0885(3) 0.1782(4) 0.0571(16) Uani 1 1 d . . . H28 H -0.0418 0.0828 0.2420 0.069 Uiso 1 1 calc R . . C29 C -0.0295(4) 0.1004(2) 0.1234(3) 0.0423(11) Uani 1 1 d . . . H29 H 0.0373 0.1025 0.1515 0.051 Uiso 1 1 calc R . . C30 C -0.1744(4) 0.0204(2) 0.2682(4) 0.0506(14) Uani 1 1 d . . . C31 C -0.1676(5) -0.0206(3) 0.2242(4) 0.0615(17) Uani 1 1 d . . . H31 H -0.1964 -0.0223 0.1591 0.074 Uiso 1 1 calc R . . C32 C -0.1187(4) -0.0590(2) 0.2753(4) 0.0485(13) Uani 1 1 d . . . H32 H -0.1152 -0.0866 0.2438 0.058 Uiso 1 1 calc R . . C33 C -0.0825(4) -0.01857(18) 0.4121(4) 0.0484(13) Uani 1 1 d . . . H33 H -0.0528 -0.0179 0.4773 0.058 Uiso 1 1 calc R . . C34 C -0.1314(5) 0.0217(2) 0.3652(5) 0.0617(17) Uani 1 1 d . . . H34 H -0.1353 0.0489 0.3977 0.074 Uiso 1 1 calc R . . C35 C 0.3958(3) 0.19829(17) 0.0165(3) 0.0357(10) Uani 1 1 d . . . H35 H 0.3509 0.2228 0.0030 0.043 Uiso 1 1 calc R . . C36 C 0.4920(4) 0.20996(19) 0.0595(4) 0.0383(11) Uani 1 1 d . . . H36 H 0.5113 0.2416 0.0742 0.046 Uiso 1 1 calc R . . C37 C 0.5594(4) 0.17367(18) 0.0805(3) 0.0340(10) Uani 1 1 d . . . C38 C 0.5269(4) 0.12704(17) 0.0558(3) 0.0360(10) Uani 1 1 d . . . H38 H 0.5701 0.1018 0.0680 0.043 Uiso 1 1 calc R . . C39 C 0.4277(4) 0.11907(17) 0.0123(4) 0.0356(10) Uani 1 1 d . . . H39 H 0.4056 0.0879 -0.0040 0.043 Uiso 1 1 calc R . . C40 C 0.6904(3) 0.23220(18) 0.2093(3) 0.0367(11) Uani 1 1 d . . . C41 C 0.7439(4) 0.2710(2) 0.2145(4) 0.0484(13) Uani 1 1 d . . . H41 H 0.7779 0.2735 0.1776 0.058 Uiso 1 1 calc R . . C42 C 0.7478(4) 0.3076(2) 0.2760(4) 0.0432(12) Uani 1 1 d . . . H42 H 0.7834 0.3349 0.2781 0.052 Uiso 1 1 calc R . . C43 C 0.6504(4) 0.26552(19) 0.3270(4) 0.0428(12) Uani 1 1 d . . . H43 H 0.6175 0.2634 0.3650 0.051 Uiso 1 1 calc R . . C44 C 0.6436(4) 0.2278(2) 0.2678(4) 0.0464(13) Uani 1 1 d . . . H44 H 0.6088 0.2004 0.2671 0.056 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 C10 0.107(6) 0.141(7) 0.142(7) 0.025(5) 0.056(5) -0.013(5) C11 0.162(7) 0.180(8) 0.189(8) 0.009(6) 0.069(5) 0.002(6) C12 0.130(7) 0.157(7) 0.161(7) 0.016(6) 0.064(5) 0.008(6) C10' 0.107(6) 0.141(7) 0.142(7) 0.025(5) 0.056(5) -0.013(5) C11' 0.162(7) 0.180(8) 0.189(8) 0.009(6) 0.069(5) 0.002(6) C12' 0.130(7) 0.157(7) 0.161(7) 0.016(6) 0.064(5) 0.008(6) C22 0.120(6) 0.112(5) 0.097(5) 0.001(4) 0.058(4) 0.011(5) C23 0.107(5) 0.132(6) 0.109(5) 0.014(4) 0.067(4) -0.016(4) C24 0.099(5) 0.134(6) 0.117(5) 0.023(4) 0.072(4) 0.018(4) C22' 0.120(6) 0.112(5) 0.097(5) 0.001(4) 0.058(4) 0.011(5) C23' 0.107(5) 0.132(6) 0.109(5) 0.014(4) 0.067(4) -0.016(4) C24' 0.099(5) 0.134(6) 0.117(5) 0.023(4) 0.072(4) 0.018(4) Ni1 0.0230(3) 0.0256(3) 0.0228(2) 0.0007(2) 0.00828(19) -0.0001(2) Ni2 0.0254(3) 0.0240(3) 0.0234(2) -0.0002(2) 0.0107(2) -0.0004(2) S1 0.0279(6) 0.0464(7) 0.0583(8) -0.0237(6) 0.0155(6) -0.0007(5) S2 0.0743(11) 0.0928(13) 0.1045(14) 0.0689(11) 0.0721(11) 0.0572(10) O1 0.0252(17) 0.045(2) 0.0432(19) 0.0176(15) 0.0135(15) 0.0072(14) O2 0.0342(18) 0.047(2) 0.047(2) 0.0219(16) 0.0168(16) 0.0028(16) O3 0.031(2) 0.070(3) 0.075(3) 0.045(2) 0.0239(19) 0.0105(18) O4 0.0327(17) 0.0332(18) 0.0443(19) 0.0141(15) 0.0149(15) 0.0027(14) O5 0.0373(19) 0.044(2) 0.0392(19) 0.0165(15) 0.0185(15) 0.0117(15) O6 0.040(2) 0.073(3) 0.056(2) 0.032(2) 0.0304(18) 0.0240(19) O7 0.0388(18) 0.0422(19) 0.0328(17) 0.0124(14) 0.0219(15) 0.0103(15) O8 0.0395(19) 0.051(2) 0.050(2) 0.0229(17) 0.0259(16) 0.0184(17) O9 0.0278(16) 0.0292(15) 0.0255(16) 0.0010(12) 0.0106(13) 0.0005(13) N1 0.028(2) 0.034(2) 0.031(2) 0.0000(16) 0.0126(17) -0.0004(16) N2 0.035(2) 0.031(2) 0.041(2) 0.0061(16) 0.0192(18) 0.0022(17) N3 0.032(2) 0.0293(19) 0.0271(18) -0.0037(15) 0.0133(16) -0.0023(16) N4 0.031(2) 0.035(2) 0.034(2) -0.0047(16) 0.0141(17) -0.0048(16) C1 0.030(2) 0.029(2) 0.030(2) 0.0045(18) 0.0095(19) 0.0012(18) C2 0.034(3) 0.038(3) 0.042(3) 0.016(2) 0.012(2) 0.003(2) C3 0.027(2) 0.033(2) 0.040(2) 0.0086(19) 0.015(2) 0.0045(19) C4 0.032(2) 0.041(3) 0.049(3) 0.018(2) 0.015(2) 0.002(2) C5 0.036(3) 0.100(6) 0.104(6) 0.077(5) 0.024(3) 0.014(3) C6 0.050(3) 0.115(5) 0.125(5) 0.081(4) 0.035(4) 0.013(4) C7 0.037(3) 0.092(5) 0.129(7) 0.076(5) 0.040(4) 0.016(3) C8 0.037(3) 0.035(2) 0.040(3) 0.007(2) 0.017(2) -0.003(2) C9 0.065(4) 0.131(6) 0.145(6) 0.081(5) 0.029(4) 0.009(4) C13 0.032(2) 0.036(2) 0.034(2) 0.0070(19) 0.013(2) 0.0082(19) C14 0.036(3) 0.045(3) 0.045(3) 0.020(2) 0.021(2) 0.012(2) C15 0.029(2) 0.040(3) 0.036(2) 0.015(2) 0.0165(19) 0.0092(19) C16 0.036(3) 0.044(3) 0.041(3) 0.016(2) 0.022(2) 0.006(2) C17 0.049(3) 0.082(5) 0.069(4) 0.040(4) 0.041(3) 0.033(3) C18 0.064(4) 0.091(5) 0.084(5) 0.050(4) 0.049(4) 0.033(4) C19 0.067(4) 0.078(5) 0.065(4) 0.048(4) 0.044(3) 0.030(3) C20 0.029(2) 0.028(2) 0.028(2) 0.0046(17) 0.0117(18) -0.0002(18) C21 0.101(6) 0.105(6) 0.114(7) 0.054(5) 0.086(6) 0.041(5) C25 0.038(3) 0.044(3) 0.036(3) 0.003(2) 0.014(2) 0.009(2) C26 0.032(2) 0.049(3) 0.046(3) 0.011(2) 0.024(2) 0.011(2) C27 0.049(3) 0.050(3) 0.056(3) 0.023(3) 0.039(3) 0.020(3) C28 0.052(3) 0.081(4) 0.044(3) 0.025(3) 0.027(3) 0.029(3) C29 0.035(3) 0.061(3) 0.031(2) 0.005(2) 0.014(2) 0.005(2) C30 0.046(3) 0.054(3) 0.065(4) 0.032(3) 0.037(3) 0.027(3) C31 0.059(4) 0.079(5) 0.044(3) 0.022(3) 0.020(3) 0.023(3) C32 0.055(3) 0.055(3) 0.034(3) 0.007(2) 0.018(2) 0.015(3) C33 0.061(3) 0.032(3) 0.050(3) 0.003(2) 0.022(3) 0.011(2) C34 0.078(4) 0.050(3) 0.070(4) 0.019(3) 0.044(4) 0.028(3) C35 0.031(2) 0.029(2) 0.048(3) -0.005(2) 0.017(2) 0.0045(18) C36 0.033(2) 0.035(3) 0.046(3) -0.009(2) 0.015(2) -0.001(2) C37 0.035(2) 0.039(3) 0.031(2) -0.0044(19) 0.016(2) 0.001(2) C38 0.034(3) 0.029(2) 0.042(3) -0.0038(19) 0.012(2) 0.0043(19) C39 0.032(2) 0.029(2) 0.043(3) -0.0040(19) 0.014(2) -0.0014(19) C40 0.025(2) 0.039(3) 0.041(3) -0.013(2) 0.009(2) -0.0002(19) C41 0.045(3) 0.057(3) 0.057(3) -0.020(3) 0.035(3) -0.015(3) C42 0.047(3) 0.048(3) 0.046(3) -0.013(2) 0.030(2) -0.018(2) C43 0.049(3) 0.043(3) 0.044(3) -0.010(2) 0.027(2) -0.014(2) C44 0.050(3) 0.043(3) 0.052(3) -0.014(2) 0.028(3) -0.016(2) _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 C10 C9 1.521(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C9 1.530(10) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C9 1.520(10) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C10' C9 1.522(10) . ? C10' H10D 0.9600 . ? C10' H10E 0.9600 . ? C10' H10F 0.9600 . ? C11' C9 1.517(10) . ? C11' H11D 0.9600 . ? C11' H11E 0.9600 . ? C11' H11F 0.9600 . ? C12' C9 1.519(10) . ? C12' H12D 0.9600 . ? C12' H12E 0.9600 . ? C12' H12F 0.9600 . ? C22 C21 1.555(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C21 1.563(7) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C21 1.527(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C22' C21 1.547(9) . ? C22' H22D 0.9600 . ? C22' H22E 0.9600 . ? C22' H22F 0.9600 . ? C23' C21 1.527(9) . ? C23' H23D 0.9600 . ? C23' H23E 0.9600 . ? C23' H23F 0.9600 . ? C24' C21 1.519(9) . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? Ni1 O8 2.029(3) 4 ? Ni1 O1 2.035(3) . ? Ni1 O5 2.078(3) . ? Ni1 O9 2.103(3) . ? Ni1 N2 2.109(4) 2_554 ? Ni1 N1 2.110(4) . ? Ni2 O2 2.030(3) . ? Ni2 O7 2.043(3) 4 ? Ni2 O4 2.066(3) 2_554 ? Ni2 N3 2.087(4) . ? Ni2 N4 2.091(4) 4_454 ? Ni2 O9 2.102(3) . ? S1 C37 1.766(5) . ? S1 C40 1.784(5) . ? S2 C27 1.785(5) . ? S2 C30 1.787(5) . ? O1 C1 1.256(6) . ? O2 C1 1.250(6) . ? O3 C8 1.264(6) . ? O4 C8 1.243(6) . ? O4 Ni2 2.066(3) 2 ? O5 C13 1.254(6) . ? O6 C13 1.249(6) . ? O7 C20 1.251(5) . ? O7 Ni2 2.043(3) 4_454 ? O8 C20 1.254(6) . ? O8 Ni1 2.029(3) 4_454 ? O9 H9A 0.9700 . ? O9 H9B 0.9700 . ? N1 C29 1.321(6) . ? N1 C25 1.336(7) . ? N2 C32 1.324(7) . ? N2 C33 1.345(7) . ? N2 Ni1 2.109(4) 2 ? N3 C35 1.321(6) . ? N3 C39 1.328(6) . ? N4 C43 1.340(7) . ? N4 C42 1.346(7) . ? N4 Ni2 2.091(4) 4 ? C1 C2 1.503(6) . ? C2 C3 1.368(7) . ? C2 C7 1.396(8) . ? C3 C4 1.400(7) . ? C3 H3 0.9300 . ? C4 C5 1.403(8) . ? C4 C8 1.511(7) . ? C5 C6 1.335(9) . ? C5 H5 0.9300 . ? C6 C7 1.405(9) . ? C6 C9 1.532(11) . ? C7 H7 0.9300 . ? C13 C14 1.519(7) . ? C14 C19 1.379(8) . ? C14 C15 1.406(6) . ? C15 C16 1.369(7) . ? C15 H15 0.9300 . ? C16 C17 1.398(7) . ? C16 C20 1.517(6) . ? C17 C18 1.341(8) . ? C17 H17 0.9300 . ? C18 C19 1.387(9) . ? C18 C21 1.608(9) . ? C19 H19 0.9300 . ? C25 C26 1.388(7) . ? C25 H25 0.9300 . ? C26 C27 1.384(8) . ? C26 H26 0.9300 . ? C27 C28 1.359(9) . ? C28 C29 1.374(8) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.364(10) . ? C30 C34 1.383(9) . ? C31 C32 1.360(9) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.381(8) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.377(7) . ? C35 H35 0.9300 . ? C36 C37 1.384(7) . ? C36 H36 0.9300 . ? C37 C38 1.391(7) . ? C38 C39 1.396(7) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.341(7) . ? C40 C44 1.389(8) . ? C41 C42 1.389(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.380(7) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? 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 C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C10' H10D 109.5 . . ? C9 C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9 C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C9 C11' H11D 109.5 . . ? C9 C11' H11E 109.5 . . ? H11D C11' H11E 109.5 . . ? C9 C11' H11F 109.5 . . ? H11D C11' H11F 109.5 . . ? H11E C11' H11F 109.5 . . ? C9 C12' H12D 109.5 . . ? C9 C12' H12E 109.5 . . ? H12D C12' H12E 109.5 . . ? C9 C12' H12F 109.5 . . ? H12D C12' H12F 109.5 . . ? H12E C12' H12F 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 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C22' H22D 109.5 . . ? C21 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C21 C23' H23D 109.5 . . ? C21 C23' H23E 109.5 . . ? H23D C23' H23E 109.5 . . ? C21 C23' H23F 109.5 . . ? H23D C23' H23F 109.5 . . ? H23E C23' H23F 109.5 . . ? C21 C24' H24D 109.5 . . ? C21 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C21 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? O8 Ni1 O1 91.21(16) 4 . ? O8 Ni1 O5 90.90(16) 4 . ? O1 Ni1 O5 173.90(14) . . ? O8 Ni1 O9 94.09(13) 4 . ? O1 Ni1 O9 95.25(13) . . ? O5 Ni1 O9 90.31(13) . . ? O8 Ni1 N2 176.05(16) 4 2_554 ? O1 Ni1 N2 87.58(16) . 2_554 ? O5 Ni1 N2 89.94(15) . 2_554 ? O9 Ni1 N2 89.77(14) . 2_554 ? O8 Ni1 N1 87.90(15) 4 . ? O1 Ni1 N1 86.99(14) . . ? O5 Ni1 N1 87.37(14) . . ? O9 Ni1 N1 176.96(15) . . ? N2 Ni1 N1 88.28(16) 2_554 . ? O2 Ni2 O7 92.48(16) . 4 ? O2 Ni2 O4 88.76(15) . 2_554 ? O7 Ni2 O4 172.25(13) 4 2_554 ? O2 Ni2 N3 88.46(14) . . ? O7 Ni2 N3 85.85(14) 4 . ? O4 Ni2 N3 86.54(14) 2_554 . ? O2 Ni2 N4 176.82(16) . 4_454 ? O7 Ni2 N4 88.98(14) 4 4_454 ? O4 Ni2 N4 89.41(16) 2_554 4_454 ? N3 Ni2 N4 88.83(15) . 4_454 ? O2 Ni2 O9 93.65(13) . . ? O7 Ni2 O9 96.94(13) 4 . ? O4 Ni2 O9 90.62(13) 2_554 . ? N3 Ni2 O9 176.42(13) . . ? N4 Ni2 O9 88.98(14) 4_454 . ? C37 S1 C40 99.8(2) . . ? C27 S2 C30 99.6(2) . . ? C1 O1 Ni1 132.6(3) . . ? C1 O2 Ni2 136.8(3) . . ? C8 O4 Ni2 130.6(3) . 2 ? C13 O5 Ni1 131.6(3) . . ? C20 O7 Ni2 131.0(3) . 4_454 ? C20 O8 Ni1 138.2(3) . 4_454 ? Ni1 O9 Ni2 112.50(14) . . ? Ni1 O9 H9A 109.1 . . ? Ni2 O9 H9A 109.2 . . ? Ni1 O9 H9B 109.0 . . ? Ni2 O9 H9B 109.1 . . ? H9A O9 H9B 107.9 . . ? C29 N1 C25 118.2(4) . . ? C29 N1 Ni1 121.5(3) . . ? C25 N1 Ni1 120.0(3) . . ? C32 N2 C33 117.4(5) . . ? C32 N2 Ni1 122.9(4) . 2 ? C33 N2 Ni1 119.7(3) . 2 ? C35 N3 C39 118.3(4) . . ? C35 N3 Ni2 120.1(3) . . ? C39 N3 Ni2 121.7(3) . . ? C43 N4 C42 117.2(4) . . ? C43 N4 Ni2 121.4(3) . 4 ? C42 N4 Ni2 121.3(3) . 4 ? O2 C1 O1 126.5(4) . . ? O2 C1 C2 117.2(4) . . ? O1 C1 C2 116.2(4) . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 122.8(4) . . ? C7 C2 C1 118.0(5) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C5 C4 C3 117.3(5) . . ? C5 C4 C8 119.9(5) . . ? C3 C4 C8 122.8(4) . . ? C6 C5 C4 124.2(6) . . ? C6 C5 H5 117.9 . . ? C4 C5 H5 117.9 . . ? C5 C6 C7 117.1(6) . . ? C5 C6 C9 122.2(6) . . ? C7 C6 C9 120.3(6) . . ? C2 C7 C6 121.5(6) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? O4 C8 O3 125.8(4) . . ? O4 C8 C4 115.8(4) . . ? O3 C8 C4 118.4(4) . . ? C11' C9 C10 132.5(19) . . ? C11' C9 C6 113.7(17) . . ? C10 C9 C6 113.8(11) . . ? C11' C9 C10' 111.5(10) . . ? C10 C9 C10' 49.0(11) . . ? C6 C9 C10' 113.0(13) . . ? C11' C9 C12 52.6(12) . . ? C10 C9 C12 107.6(9) . . ? C6 C9 C12 110.1(13) . . ? C10' C9 C12 136.5(16) . . ? C11' C9 C12' 111.9(10) . . ? C10 C9 C12' 62.6(11) . . ? C6 C9 C12' 94.1(15) . . ? C10' C9 C12' 111.6(10) . . ? C12 C9 C12' 59.6(11) . . ? C11' C9 C11 56.4(11) . . ? C10 C9 C11 107.5(9) . . ? C6 C9 C11 110.4(15) . . ? C10' C9 C11 61.9(11) . . ? C12 C9 C11 107.2(9) . . ? C12' C9 C11 155.4(19) . . ? O6 C13 O5 125.9(4) . . ? O6 C13 C14 119.3(4) . . ? O5 C13 C14 114.8(4) . . ? C19 C14 C15 118.8(5) . . ? C19 C14 C13 119.5(4) . . ? C15 C14 C13 121.7(4) . . ? C16 C15 C14 119.5(4) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 C20 122.1(4) . . ? C17 C16 C20 117.4(4) . . ? C18 C17 C16 120.1(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 C21 122.7(5) . . ? C19 C18 C21 116.7(5) . . ? C14 C19 C18 120.7(5) . . ? C14 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? O7 C20 O8 125.5(4) . . ? O7 C20 C16 117.6(4) . . ? O8 C20 C16 116.9(4) . . ? C24' C21 C23' 108.7(8) . . ? C24' C21 C24 56.8(3) . . ? C23' C21 C24 56.5(3) . . ? C24' C21 C22' 107.5(8) . . ? C23' C21 C22' 106.9(7) . . ? C24 C21 C22' 139.8(9) . . ? C24' C21 C22 56.3(3) . . ? C23' C21 C22 139.2(9) . . ? C24 C21 C22 110.6(5) . . ? C22' C21 C22 55.4(3) . . ? C24' C21 C23 139.8(10) . . ? C23' C21 C23 55.9(3) . . ? C24 C21 C23 110.2(5) . . ? C22' C21 C23 55.3(3) . . ? C22 C21 C23 108.5(5) . . ? C24' C21 C18 111.9(8) . . ? C23' C21 C18 111.5(8) . . ? C24 C21 C18 110.0(5) . . ? C22' C21 C18 110.1(7) . . ? C22 C21 C18 109.2(5) . . ? C23 C21 C18 108.2(5) . . ? N1 C25 C26 122.4(5) . . ? N1 C25 H25 118.8 . . ? C26 C25 H25 118.8 . . ? C27 C26 C25 118.1(5) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C28 C27 C26 119.0(5) . . ? C28 C27 S2 121.4(4) . . ? C26 C27 S2 119.5(4) . . ? C27 C28 C29 119.4(5) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? N1 C29 C28 122.8(5) . . ? N1 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C31 C30 C34 118.6(5) . . ? C31 C30 S2 123.1(5) . . ? C34 C30 S2 118.3(5) . . ? C30 C31 C32 120.2(6) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? N2 C32 C31 122.8(6) . . ? N2 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? N2 C33 C34 123.2(5) . . ? N2 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? C33 C34 C30 117.8(6) . . ? C33 C34 H34 121.1 . . ? C30 C34 H34 121.1 . . ? N3 C35 C36 123.6(4) . . ? N3 C35 H35 118.2 . . ? C36 C35 H35 118.2 . . ? C35 C36 C37 118.7(5) . . ? C35 C36 H36 120.7 . . ? C37 C36 H36 120.7 . . ? C36 C37 C38 118.4(5) . . ? C36 C37 S1 122.3(4) . . ? C38 C37 S1 119.1(4) . . ? C37 C38 C39 118.3(5) . . ? C37 C38 H38 120.8 . . ? C39 C38 H38 120.8 . . ? N3 C39 C38 122.7(4) . . ? N3 C39 H39 118.7 . . ? C38 C39 H39 118.7 . . ? C41 C40 C44 120.2(5) . . ? C41 C40 S1 119.5(4) . . ? C44 C40 S1 120.3(4) . . ? C40 C41 C42 119.0(5) . . ? C40 C41 H41 120.5 . . ? C42 C41 H41 120.5 . . ? N4 C42 C41 122.5(5) . . ? N4 C42 H42 118.7 . . ? C41 C42 H42 118.7 . . ? N4 C43 C44 123.3(5) . . ? N4 C43 H43 118.4 . . ? C44 C43 H43 118.4 . . ? C43 C44 C40 117.7(5) . . ? C43 C44 H44 121.1 . . ? C40 C44 H44 121.1 . . ? 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 O8 Ni1 O1 C1 -64.1(5) 4 . . . ? O5 Ni1 O1 C1 -174.3(13) . . . . ? O9 Ni1 O1 C1 30.1(5) . . . . ? N2 Ni1 O1 C1 119.6(5) 2_554 . . . ? N1 Ni1 O1 C1 -152.0(5) . . . . ? O7 Ni2 O2 C1 70.9(5) 4 . . . ? O4 Ni2 O2 C1 -116.7(5) 2_554 . . . ? N3 Ni2 O2 C1 156.7(5) . . . . ? N4 Ni2 O2 C1 -172(3) 4_454 . . . ? O9 Ni2 O2 C1 -26.2(5) . . . . ? O8 Ni1 O5 C13 88.4(5) 4 . . . ? O1 Ni1 O5 C13 -161.4(13) . . . . ? O9 Ni1 O5 C13 -5.7(5) . . . . ? N2 Ni1 O5 C13 -95.5(5) 2_554 . . . ? N1 Ni1 O5 C13 176.2(5) . . . . ? O8 Ni1 O9 Ni2 43.06(18) 4 . . . ? O1 Ni1 O9 Ni2 -48.54(17) . . . . ? O5 Ni1 O9 Ni2 133.98(17) . . . . ? N2 Ni1 O9 Ni2 -136.09(17) 2_554 . . . ? N1 Ni1 O9 Ni2 174(26) . . . . ? O2 Ni2 O9 Ni1 46.43(18) . . . . ? O7 Ni2 O9 Ni1 -46.52(17) 4 . . . ? O4 Ni2 O9 Ni1 135.23(16) 2_554 . . . ? N3 Ni2 O9 Ni1 173(2) . . . . ? N4 Ni2 O9 Ni1 -135.37(17) 4_454 . . . ? O8 Ni1 N1 C29 -59.4(4) 4 . . . ? O1 Ni1 N1 C29 31.9(4) . . . . ? O5 Ni1 N1 C29 -150.4(4) . . . . ? O9 Ni1 N1 C29 170(3) . . . . ? N2 Ni1 N1 C29 119.6(4) 2_554 . . . ? O8 Ni1 N1 C25 126.7(4) 4 . . . ? O1 Ni1 N1 C25 -141.9(4) . . . . ? O5 Ni1 N1 C25 35.7(4) . . . . ? O9 Ni1 N1 C25 -4(3) . . . . ? N2 Ni1 N1 C25 -54.3(4) 2_554 . . . ? O2 Ni2 N3 C35 -131.3(4) . . . . ? O7 Ni2 N3 C35 -38.7(4) 4 . . . ? O4 Ni2 N3 C35 139.8(4) 2_554 . . . ? N4 Ni2 N3 C35 50.3(4) 4_454 . . . ? O9 Ni2 N3 C35 102(2) . . . . ? O2 Ni2 N3 C39 48.2(4) . . . . ? O7 Ni2 N3 C39 140.8(4) 4 . . . ? O4 Ni2 N3 C39 -40.6(4) 2_554 . . . ? N4 Ni2 N3 C39 -130.1(4) 4_454 . . . ? O9 Ni2 N3 C39 -78(2) . . . . ? Ni2 O2 C1 O1 4.4(9) . . . . ? Ni2 O2 C1 C2 -175.7(4) . . . . ? Ni1 O1 C1 O2 -6.8(8) . . . . ? Ni1 O1 C1 C2 173.4(3) . . . . ? O2 C1 C2 C3 -176.9(5) . . . . ? O1 C1 C2 C3 2.9(7) . . . . ? O2 C1 C2 C7 4.1(8) . . . . ? O1 C1 C2 C7 -176.0(6) . . . . ? C7 C2 C3 C4 -1.9(9) . . . . ? C1 C2 C3 C4 179.2(5) . . . . ? C2 C3 C4 C5 0.2(9) . . . . ? C2 C3 C4 C8 -179.0(5) . . . . ? C3 C4 C5 C6 0.4(14) . . . . ? C8 C4 C5 C6 179.6(10) . . . . ? C4 C5 C6 C7 0.8(18) . . . . ? C4 C5 C6 C9 173.3(10) . . . . ? C3 C2 C7 C6 3.1(13) . . . . ? C1 C2 C7 C6 -177.9(9) . . . . ? C5 C6 C7 C2 -2.5(17) . . . . ? C9 C6 C7 C2 -175.2(10) . . . . ? Ni2 O4 C8 O3 -3.6(8) 2 . . . ? Ni2 O4 C8 C4 176.5(3) 2 . . . ? C5 C4 C8 O4 -2.2(9) . . . . ? C3 C4 C8 O4 177.0(5) . . . . ? C5 C4 C8 O3 177.8(7) . . . . ? C3 C4 C8 O3 -3.0(8) . . . . ? C5 C6 C9 C11' -15.7(18) . . . . ? C7 C6 C9 C11' 156.6(15) . . . . ? C5 C6 C9 C10 162.1(13) . . . . ? C7 C6 C9 C10 -25.6(16) . . . . ? C5 C6 C9 C10' -144.2(15) . . . . ? C7 C6 C9 C10' 28.2(17) . . . . ? C5 C6 C9 C12 41.2(17) . . . . ? C7 C6 C9 C12 -146.5(12) . . . . ? C5 C6 C9 C12' 100.3(15) . . . . ? C7 C6 C9 C12' -87.4(15) . . . . ? C5 C6 C9 C11 -76.9(16) . . . . ? C7 C6 C9 C11 95.4(13) . . . . ? Ni1 O5 C13 O6 5.2(8) . . . . ? Ni1 O5 C13 C14 -176.3(3) . . . . ? O6 C13 C14 C19 -176.7(6) . . . . ? O5 C13 C14 C19 4.7(8) . . . . ? O6 C13 C14 C15 1.4(8) . . . . ? O5 C13 C14 C15 -177.2(5) . . . . ? C19 C14 C15 C16 -2.4(9) . . . . ? C13 C14 C15 C16 179.5(5) . . . . ? C14 C15 C16 C17 1.0(9) . . . . ? C14 C15 C16 C20 179.0(5) . . . . ? C15 C16 C17 C18 0.2(11) . . . . ? C20 C16 C17 C18 -177.9(7) . . . . ? C16 C17 C18 C19 0.1(13) . . . . ? C16 C17 C18 C21 175.6(6) . . . . ? C15 C14 C19 C18 2.7(11) . . . . ? C13 C14 C19 C18 -179.2(7) . . . . ? C17 C18 C19 C14 -1.6(13) . . . . ? C21 C18 C19 C14 -177.4(6) . . . . ? Ni2 O7 C20 O8 18.1(7) 4_454 . . . ? Ni2 O7 C20 C16 -159.9(3) 4_454 . . . ? Ni1 O8 C20 O7 -15.1(8) 4_454 . . . ? Ni1 O8 C20 C16 162.9(4) 4_454 . . . ? C15 C16 C20 O7 -5.0(7) . . . . ? C17 C16 C20 O7 173.1(5) . . . . ? C15 C16 C20 O8 176.8(5) . . . . ? C17 C16 C20 O8 -5.1(8) . . . . ? C17 C18 C21 C24' -55.5(9) . . . . ? C19 C18 C21 C24' 120.1(8) . . . . ? C17 C18 C21 C23' 66.4(9) . . . . ? C19 C18 C21 C23' -117.9(8) . . . . ? C17 C18 C21 C24 5.6(10) . . . . ? C19 C18 C21 C24 -178.7(7) . . . . ? C17 C18 C21 C22' -175.1(8) . . . . ? C19 C18 C21 C22' 0.6(9) . . . . ? C17 C18 C21 C22 -116.0(8) . . . . ? C19 C18 C21 C22 59.7(8) . . . . ? C17 C18 C21 C23 126.1(8) . . . . ? C19 C18 C21 C23 -58.2(8) . . . . ? C29 N1 C25 C26 -3.7(8) . . . . ? Ni1 N1 C25 C26 170.4(4) . . . . ? N1 C25 C26 C27 2.3(8) . . . . ? C25 C26 C27 C28 0.5(9) . . . . ? C25 C26 C27 S2 176.2(4) . . . . ? C30 S2 C27 C28 -50.9(6) . . . . ? C30 S2 C27 C26 133.5(5) . . . . ? C26 C27 C28 C29 -1.8(9) . . . . ? S2 C27 C28 C29 -177.4(5) . . . . ? C25 N1 C29 C28 2.3(8) . . . . ? Ni1 N1 C29 C28 -171.7(5) . . . . ? C27 C28 C29 N1 0.4(10) . . . . ? C27 S2 C30 C31 -60.4(6) . . . . ? C27 S2 C30 C34 121.3(5) . . . . ? C34 C30 C31 C32 -0.4(10) . . . . ? S2 C30 C31 C32 -178.7(5) . . . . ? C33 N2 C32 C31 0.5(9) . . . . ? Ni1 N2 C32 C31 179.9(5) 2 . . . ? C30 C31 C32 N2 -0.3(10) . . . . ? C32 N2 C33 C34 -0.1(9) . . . . ? Ni1 N2 C33 C34 -179.4(5) 2 . . . ? N2 C33 C34 C30 -0.6(10) . . . . ? C31 C30 C34 C33 0.9(9) . . . . ? S2 C30 C34 C33 179.2(5) . . . . ? C39 N3 C35 C36 -0.1(7) . . . . ? Ni2 N3 C35 C36 179.4(4) . . . . ? N3 C35 C36 C37 -0.5(8) . . . . ? C35 C36 C37 C38 1.0(7) . . . . ? C35 C36 C37 S1 176.9(4) . . . . ? C40 S1 C37 C36 38.5(5) . . . . ? C40 S1 C37 C38 -145.6(4) . . . . ? C36 C37 C38 C39 -1.0(7) . . . . ? S1 C37 C38 C39 -177.0(4) . . . . ? C35 N3 C39 C38 0.2(7) . . . . ? Ni2 N3 C39 C38 -179.4(4) . . . . ? C37 C38 C39 N3 0.4(8) . . . . ? C37 S1 C40 C41 -135.2(5) . . . . ? C37 S1 C40 C44 47.7(5) . . . . ? C44 C40 C41 C42 -3.0(9) . . . . ? S1 C40 C41 C42 179.9(5) . . . . ? C43 N4 C42 C41 -0.8(8) . . . . ? Ni2 N4 C42 C41 176.6(5) 4 . . . ? C40 C41 C42 N4 1.9(9) . . . . ? C42 N4 C43 C44 1.0(8) . . . . ? Ni2 N4 C43 C44 -176.4(4) 4 . . . ? N4 C43 C44 C40 -2.1(9) . . . . ? C41 C40 C44 C43 3.1(8) . . . . ? S1 C40 C44 C43 -179.8(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O6 0.97 1.78 2.658(5) 148.1 . O9 H9B O3 0.97 1.74 2.624(5) 149.1 2_554 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.985 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.098