# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ;New Supramolecular Isomers with 2D 44 Square-Grid and 3D 65?8 CdSO4 Frameworks in One-Pot Synthesis; Reversible Solvent Uptake and Intriguing Luminescence Properties ; _publ_contact_author_name 'Prof. Pi-Tai Chou' _publ_contact_author_email CHOP@NTU.EDU.TW loop_ _publ_author_name 'Pi-Tai Chou.' 'Mei-Lin Ho.' 'Wei-Ting Huang.' 'Mei-Ju Ko.' ; Gene-Hsiang Lee ; 'Wei-Zeng Lin.' 'Chun-Wei Lin.' 'Chun-Wei Shih.' 'Chih-Chieh Wang.' # Attachment 'compound1.cif' data_ic11717 _database_code_depnum_ccdc_archive 'CCDC 666607' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 N10 Ni O4 S2' _chemical_formula_weight 751.57 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' 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' O O 0.0106 0.0060 '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 22.5500(4) _cell_length_b 18.8168(3) _cell_length_c 8.7610(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.6734(9) _cell_angle_gamma 90.00 _cell_volume 3713.41(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.50 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.614 _exptl_absorpt_correction_T_max 0.736 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20076 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8492 _reflns_number_gt 5908 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _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^)+(0.0879P)^2^+14.6214P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8492 _refine_ls_number_parameters 449 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0690 _refine_ls_wR_factor_ref 0.2275 _refine_ls_wR_factor_gt 0.2063 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.075 _refine_ls_shift/su_max 0.021 _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 0.25021(2) 0.45665(3) 0.00789(5) 0.02004(16) Uani 1 1 d . . . S1 S 0.13970(8) 0.42054(10) -0.46499(18) 0.0647(5) Uani 1 1 d . . . S2 S 0.36029(6) 0.41677(7) 0.48506(14) 0.0418(3) Uani 1 1 d . . . N1 N 0.19198(15) 0.53690(17) 0.0778(4) 0.0232(7) Uani 1 1 d . . . N2 N 0.04669(17) 0.6923(2) 0.3415(5) 0.0354(9) Uani 1 1 d . . . N3 N 0.00593(17) 0.7449(2) 0.3723(5) 0.0343(9) Uani 1 1 d . . . N4 N -0.18468(15) 0.87979(18) 0.4340(4) 0.0248(7) Uani 1 1 d . . . N5 N 0.31024(14) 0.53700(17) -0.0539(4) 0.0212(7) Uani 1 1 d . . . N6 N 0.46128(17) 0.6881(2) -0.3068(4) 0.0334(9) Uani 1 1 d . . . N7 N 0.49960(17) 0.7426(2) -0.3393(4) 0.0320(8) Uani 1 1 d . . . N8 N 0.68605(14) 0.87935(18) -0.4412(4) 0.0240(7) Uani 1 1 d . . . N9 N 0.21232(15) 0.45529(19) -0.2099(4) 0.0269(7) Uani 1 1 d . . . N10 N 0.28837(16) 0.44886(19) 0.2247(4) 0.0268(8) Uani 1 1 d . . . C1 C 0.1718(2) 0.5871(2) -0.0193(5) 0.0302(9) Uani 1 1 d . . . H1A H 0.1852 0.5870 -0.1205 0.036 Uiso 1 1 calc R . . C2 C 0.1323(2) 0.6390(2) 0.0213(5) 0.0345(10) Uani 1 1 d . . . H2A H 0.1194 0.6742 -0.0506 0.041 Uiso 1 1 calc R . . C3 C 0.11166(18) 0.6394(2) 0.1674(5) 0.0252(8) Uani 1 1 d . . . C4 C 0.13268(19) 0.5877(2) 0.2695(5) 0.0292(9) Uani 1 1 d . . . H4A H 0.1199 0.5867 0.3712 0.035 Uiso 1 1 calc R . . C5 C 0.17259(19) 0.5377(2) 0.2206(5) 0.0281(9) Uani 1 1 d . . . H5A H 0.1869 0.5025 0.2908 0.034 Uiso 1 1 calc R . . C6 C 0.06799(19) 0.6933(2) 0.2107(5) 0.0306(9) Uani 1 1 d . . . H6A H 0.0557 0.7290 0.1395 0.037 Uiso 1 1 calc R . . C7 C -0.0485(2) 0.7311(2) 0.3383(5) 0.0324(10) Uani 1 1 d . . . H7A H -0.0593 0.6871 0.2920 0.039 Uiso 1 1 calc R . . C8 C -0.12819(18) 0.8903(2) 0.4855(5) 0.0254(8) Uani 1 1 d . . . H8A H -0.1194 0.9316 0.5449 0.030 Uiso 1 1 calc R . . C9 C -0.08247(18) 0.8444(2) 0.4564(5) 0.0273(9) Uani 1 1 d . . . H9A H -0.0432 0.8544 0.4943 0.033 Uiso 1 1 calc R . . C10 C -0.09447(19) 0.7834(2) 0.3709(5) 0.0300(9) Uani 1 1 d . . . C11 C -0.1528(2) 0.7725(3) 0.3168(7) 0.0460(13) Uani 1 1 d . . . H11A H -0.1631 0.7314 0.2584 0.055 Uiso 1 1 calc R . . C12 C -0.1957(2) 0.8225(3) 0.3494(6) 0.0418(12) Uani 1 1 d . . . H12A H -0.2350 0.8153 0.3089 0.050 Uiso 1 1 calc R . . C13 C 0.33017(18) 0.5865(2) 0.0443(5) 0.0245(8) Uani 1 1 d . . . H13A H 0.3158 0.5865 0.1446 0.029 Uiso 1 1 calc R . . C14 C 0.37100(19) 0.6380(2) 0.0065(5) 0.0265(9) Uani 1 1 d . . . H14A H 0.3842 0.6724 0.0797 0.032 Uiso 1 1 calc R . . C15 C 0.39228(17) 0.6386(2) -0.1396(4) 0.0218(8) Uani 1 1 d . . . C16 C 0.37075(18) 0.5872(2) -0.2432(5) 0.0253(8) Uani 1 1 d . . . H16A H 0.3839 0.5863 -0.3447 0.030 Uiso 1 1 calc R . . C17 C 0.33038(18) 0.5379(2) -0.1968(5) 0.0255(8) Uani 1 1 d . . . H17A H 0.3161 0.5031 -0.2679 0.031 Uiso 1 1 calc R . . C18 C 0.43543(18) 0.6931(2) -0.1819(5) 0.0262(9) Uani 1 1 d . . . H18A H 0.4439 0.7320 -0.1155 0.031 Uiso 1 1 calc R . . C19 C 0.55451(19) 0.7287(2) -0.3238(5) 0.0308(9) Uani 1 1 d . . . H19A H 0.5670 0.6834 -0.2862 0.037 Uiso 1 1 calc R . . C20 C 0.6996(2) 0.8225(3) -0.3570(6) 0.0401(12) Uani 1 1 d . . . H20A H 0.7398 0.8160 -0.3224 0.048 Uiso 1 1 calc R . . C21 C 0.6583(2) 0.7720(3) -0.3169(7) 0.0427(13) Uani 1 1 d . . . H21A H 0.6703 0.7314 -0.2587 0.051 Uiso 1 1 calc R . . C22 C 0.59914(18) 0.7816(2) -0.3632(5) 0.0274(9) Uani 1 1 d . . . C23 C 0.58484(18) 0.8422(2) -0.4485(5) 0.0271(9) Uani 1 1 d . . . H23A H 0.5448 0.8515 -0.4804 0.033 Uiso 1 1 calc R . . C24 C 0.62883(17) 0.8884(2) -0.4860(5) 0.0258(9) Uani 1 1 d . . . H24A H 0.6183 0.9288 -0.5467 0.031 Uiso 1 1 calc R . . C25 C 0.1835(2) 0.4407(2) -0.3173(5) 0.0307(10) Uani 1 1 d . . . C26 C 0.31761(19) 0.4352(2) 0.3339(5) 0.0260(9) Uani 1 1 d . . . O1 O 0.3377(2) 0.6892(2) 0.3792(4) 0.0534(10) Uani 1 1 d D . . H1 H 0.323(3) 0.699(4) 0.471(4) 0.080 Uiso 1 1 d D . . H1' H 0.364(2) 0.653(3) 0.386(8) 0.080 Uiso 1 1 d D . . O2 O 0.41139(16) 0.5715(2) 0.3726(4) 0.0450(9) Uani 1 1 d . . . H2 H 0.4035 0.5322 0.4120 0.068 Uiso 1 1 calc R . . C27 C 0.4733(2) 0.5751(3) 0.3471(7) 0.0486(13) Uani 1 1 d . . . H27A H 0.4961 0.5674 0.4450 0.058 Uiso 1 1 calc R . . H27B H 0.4831 0.6232 0.3096 0.058 Uiso 1 1 calc R . . C28 C 0.4917(3) 0.5204(3) 0.2323(7) 0.0569(16) Uani 1 1 d . . . H28A H 0.5343 0.5253 0.2162 0.085 Uiso 1 1 calc R . . H28B H 0.4692 0.5278 0.1352 0.085 Uiso 1 1 calc R . . H28C H 0.4837 0.4727 0.2709 0.085 Uiso 1 1 calc R . . O3 O 0.28597(18) 0.7622(2) 0.1417(4) 0.0533(10) Uani 1 1 d . . . H3 H 0.3040 0.7354 0.2049 0.080 Uiso 1 1 calc R . . C29 C 0.2353(3) 0.7896(4) 0.2065(6) 0.0523(14) Uani 1 1 d . . . H29A H 0.2469 0.8179 0.2984 0.063 Uiso 1 1 calc R . . H29B H 0.2095 0.7502 0.2380 0.063 Uiso 1 1 calc R . . C30 C 0.2022(3) 0.8357(4) 0.0916(8) 0.075(2) Uani 1 1 d . . . H30A H 0.1659 0.8536 0.1356 0.112 Uiso 1 1 calc R . . H30B H 0.1917 0.8077 -0.0001 0.112 Uiso 1 1 calc R . . H30C H 0.2273 0.8758 0.0642 0.112 Uiso 1 1 calc R . . O4 O 0.0298(6) 1.0329(6) 0.2948(13) 0.184(4) Uiso 1 1 d . . . H4 H 0.0400 1.0585 0.2220 0.276 Uiso 1 1 calc R . . C31 C -0.0041(4) 0.9836(4) 0.2439(14) 0.108(3) Uani 1 1 d D . . H31A H -0.0308 1.0037 0.1620 0.129 Uiso 1 1 calc R . . H31B H -0.0292 0.9680 0.3274 0.129 Uiso 1 1 calc R . . C32 C 0.0252(4) 0.9211(5) 0.1831(10) 0.098(3) Uani 1 1 d D . . H32A H 0.0648 0.9343 0.1515 0.146 Uiso 1 1 calc R . . H32B H 0.0017 0.9028 0.0949 0.146 Uiso 1 1 calc R . . H32C H 0.0287 0.8844 0.2623 0.146 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 0.0128(2) 0.0187(3) 0.0292(3) -0.0001(2) 0.00651(18) 0.00002(19) S1 0.0671(11) 0.0810(12) 0.0439(8) 0.0144(8) -0.0206(7) -0.0301(9) S2 0.0443(7) 0.0464(7) 0.0339(6) -0.0008(5) -0.0067(5) 0.0054(6) N1 0.0183(16) 0.0210(17) 0.0309(17) 0.0009(14) 0.0079(13) 0.0009(13) N2 0.028(2) 0.034(2) 0.045(2) -0.0027(18) 0.0099(17) 0.0113(16) N3 0.0236(19) 0.035(2) 0.045(2) -0.0042(17) 0.0083(16) 0.0122(16) N4 0.0168(16) 0.0228(17) 0.0351(18) -0.0040(14) 0.0040(14) 0.0028(13) N5 0.0166(16) 0.0186(16) 0.0287(17) 0.0001(13) 0.0059(13) -0.0015(12) N6 0.028(2) 0.034(2) 0.039(2) 0.0009(17) 0.0108(16) -0.0130(16) N7 0.0246(19) 0.031(2) 0.041(2) 0.0033(16) 0.0100(16) -0.0089(15) N8 0.0143(16) 0.0220(17) 0.0360(19) 0.0042(14) 0.0057(13) -0.0015(13) N9 0.0204(17) 0.0295(19) 0.0312(18) -0.0006(15) 0.0056(14) -0.0005(14) N10 0.0203(17) 0.0277(18) 0.0331(19) 0.0015(15) 0.0086(14) 0.0007(14) C1 0.032(2) 0.026(2) 0.034(2) 0.0053(17) 0.0097(18) 0.0065(18) C2 0.035(3) 0.032(2) 0.037(2) 0.0072(19) 0.0082(19) 0.010(2) C3 0.0178(19) 0.025(2) 0.033(2) -0.0029(17) 0.0027(16) 0.0038(16) C4 0.026(2) 0.032(2) 0.030(2) -0.0036(18) 0.0069(17) 0.0047(18) C5 0.026(2) 0.028(2) 0.030(2) 0.0028(17) 0.0086(17) 0.0052(17) C6 0.025(2) 0.029(2) 0.037(2) -0.0038(18) 0.0012(18) 0.0085(18) C7 0.027(2) 0.029(2) 0.041(2) -0.0062(19) 0.0060(19) 0.0079(18) C8 0.019(2) 0.022(2) 0.036(2) -0.0063(17) 0.0047(16) 0.0011(16) C9 0.0150(19) 0.031(2) 0.036(2) -0.0046(18) 0.0044(16) 0.0045(16) C10 0.021(2) 0.029(2) 0.040(2) -0.0036(19) 0.0048(17) 0.0067(17) C11 0.026(2) 0.036(3) 0.075(4) -0.023(3) -0.005(2) 0.006(2) C12 0.020(2) 0.037(3) 0.067(3) -0.021(2) -0.007(2) 0.0028(19) C13 0.025(2) 0.023(2) 0.0257(19) -0.0012(16) 0.0067(16) -0.0025(16) C14 0.025(2) 0.023(2) 0.031(2) -0.0036(16) 0.0055(16) -0.0042(16) C15 0.0165(19) 0.0209(19) 0.028(2) 0.0015(15) 0.0051(15) -0.0018(15) C16 0.021(2) 0.027(2) 0.028(2) -0.0006(16) 0.0054(16) -0.0031(16) C17 0.020(2) 0.026(2) 0.031(2) -0.0029(17) 0.0075(16) -0.0035(16) C18 0.020(2) 0.024(2) 0.035(2) 0.0013(17) 0.0024(16) -0.0043(16) C19 0.026(2) 0.026(2) 0.040(2) 0.0054(19) 0.0041(18) -0.0062(18) C20 0.017(2) 0.032(2) 0.071(3) 0.018(2) -0.004(2) 0.0001(18) C21 0.023(2) 0.032(3) 0.072(4) 0.022(2) -0.004(2) -0.0023(19) C22 0.020(2) 0.026(2) 0.036(2) 0.0045(17) 0.0050(17) -0.0027(16) C23 0.0142(19) 0.031(2) 0.036(2) 0.0052(18) 0.0024(16) -0.0049(16) C24 0.0158(19) 0.026(2) 0.035(2) 0.0066(17) 0.0044(16) -0.0022(16) C25 0.030(2) 0.027(2) 0.035(2) 0.0069(18) 0.0062(19) -0.0025(18) C26 0.024(2) 0.024(2) 0.031(2) -0.0019(17) 0.0067(17) -0.0013(16) O1 0.062(3) 0.056(3) 0.043(2) 0.0046(19) 0.0109(19) 0.021(2) O2 0.040(2) 0.046(2) 0.049(2) -0.0013(17) 0.0070(16) 0.0033(17) C27 0.035(3) 0.050(3) 0.061(3) 0.013(3) 0.006(2) 0.001(2) C28 0.054(4) 0.053(3) 0.066(4) 0.006(3) 0.021(3) 0.008(3) O3 0.058(3) 0.059(3) 0.045(2) 0.0100(18) 0.0153(19) 0.017(2) C29 0.042(3) 0.071(4) 0.044(3) -0.003(3) 0.003(2) 0.011(3) C30 0.077(5) 0.090(5) 0.056(4) -0.011(4) -0.017(3) 0.043(4) C31 0.078(6) 0.066(5) 0.183(11) 0.000(6) 0.049(6) -0.011(5) C32 0.093(6) 0.120(8) 0.082(6) 0.033(5) 0.030(5) 0.040(6) _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 N10 2.053(4) . ? Ni1 N9 2.054(4) . ? Ni1 N1 2.111(3) . ? Ni1 N5 2.116(3) . ? Ni1 N8 2.145(3) 2_644 ? Ni1 N4 2.146(3) 2_545 ? S1 C25 1.636(5) . ? S2 C26 1.637(5) . ? N1 C1 1.337(5) . ? N1 C5 1.344(5) . ? N2 C6 1.264(6) . ? N2 N3 1.385(5) . ? N3 C7 1.277(6) . ? N4 C12 1.325(6) . ? N4 C8 1.346(5) . ? N4 Ni1 2.146(3) 2 ? N5 C13 1.331(5) . ? N5 C17 1.352(5) . ? N6 C18 1.267(6) . ? N6 N7 1.380(5) . ? N7 C19 1.267(6) . ? N8 C20 1.327(6) . ? N8 C24 1.342(5) . ? N8 Ni1 2.145(3) 2_654 ? N9 C25 1.151(6) . ? N10 C26 1.165(6) . ? C1 C2 1.379(6) . ? C2 C3 1.383(6) . ? C3 C4 1.390(6) . ? C3 C6 1.475(6) . ? C4 C5 1.384(6) . ? C7 C10 1.466(6) . ? C8 C9 1.378(5) . ? C9 C10 1.390(6) . ? C10 C11 1.393(6) . ? C11 C12 1.389(6) . ? C13 C14 1.388(6) . ? C14 C15 1.387(6) . ? C15 C16 1.398(6) . ? C15 C18 1.473(5) . ? C16 C17 1.374(5) . ? C19 C22 1.469(6) . ? C20 C21 1.387(6) . ? C21 C22 1.388(6) . ? C22 C23 1.393(6) . ? C23 C24 1.370(5) . ? O2 C27 1.427(6) . ? C27 C28 1.510(8) . ? O3 C29 1.398(6) . ? C29 C30 1.502(8) . ? O4 C31 1.269(12) . ? C31 C32 1.461(8) . ? 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 N10 Ni1 N9 175.19(15) . . ? N10 Ni1 N1 91.27(14) . . ? N9 Ni1 N1 92.36(14) . . ? N10 Ni1 N5 92.41(13) . . ? N9 Ni1 N5 90.85(13) . . ? N1 Ni1 N5 88.69(13) . . ? N10 Ni1 N8 86.93(14) . 2_644 ? N9 Ni1 N8 89.62(14) . 2_644 ? N1 Ni1 N8 176.41(13) . 2_644 ? N5 Ni1 N8 88.29(12) . 2_644 ? N10 Ni1 N4 89.77(14) . 2_545 ? N9 Ni1 N4 87.18(14) . 2_545 ? N1 Ni1 N4 88.20(13) . 2_545 ? N5 Ni1 N4 176.24(13) . 2_545 ? N8 Ni1 N4 94.89(13) 2_644 2_545 ? C1 N1 C5 118.0(4) . . ? C1 N1 Ni1 121.2(3) . . ? C5 N1 Ni1 120.8(3) . . ? C6 N2 N3 116.7(4) . . ? C7 N3 N2 116.8(4) . . ? C12 N4 C8 117.2(4) . . ? C12 N4 Ni1 124.6(3) . 2 ? C8 N4 Ni1 118.2(3) . 2 ? C13 N5 C17 118.2(3) . . ? C13 N5 Ni1 122.3(3) . . ? C17 N5 Ni1 119.5(3) . . ? C18 N6 N7 116.2(4) . . ? C19 N7 N6 116.2(4) . . ? C20 N8 C24 117.3(4) . . ? C20 N8 Ni1 123.9(3) . 2_654 ? C24 N8 Ni1 118.8(3) . 2_654 ? C25 N9 Ni1 163.0(3) . . ? C26 N10 Ni1 166.4(3) . . ? N1 C1 C2 122.7(4) . . ? C1 C2 C3 119.5(4) . . ? C2 C3 C4 118.2(4) . . ? C2 C3 C6 120.0(4) . . ? C4 C3 C6 121.8(4) . . ? C5 C4 C3 119.0(4) . . ? N1 C5 C4 122.7(4) . . ? N2 C6 C3 120.7(4) . . ? N3 C7 C10 120.0(4) . . ? N4 C8 C9 123.4(4) . . ? C8 C9 C10 119.3(4) . . ? C9 C10 C11 117.5(4) . . ? C9 C10 C7 122.5(4) . . ? C11 C10 C7 119.9(4) . . ? C12 C11 C10 119.0(4) . . ? N4 C12 C11 123.5(4) . . ? N5 C13 C14 122.8(4) . . ? C15 C14 C13 119.2(4) . . ? C14 C15 C16 118.0(4) . . ? C14 C15 C18 119.9(4) . . ? C16 C15 C18 122.1(4) . . ? C17 C16 C15 119.3(4) . . ? N5 C17 C16 122.6(4) . . ? N6 C18 C15 120.2(4) . . ? N7 C19 C22 120.7(4) . . ? N8 C20 C21 123.5(4) . . ? C20 C21 C22 119.0(4) . . ? C21 C22 C23 117.3(4) . . ? C21 C22 C19 120.2(4) . . ? C23 C22 C19 122.5(4) . . ? C24 C23 C22 119.7(4) . . ? N8 C24 C23 123.1(4) . . ? N9 C25 S1 177.2(4) . . ? N10 C26 S2 178.4(4) . . ? O2 C27 C28 111.9(5) . . ? O3 C29 C30 109.3(5) . . ? O4 C31 C32 116.1(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.433 _refine_diff_density_min -0.929 _refine_diff_density_rms 0.108 # Attachment 'compound2.cif' data_ic12192 _database_code_depnum_ccdc_archive 'CCDC 666608' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H28 N10 Ni O2 S2' _chemical_formula_weight 659.43 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 13.8640(5) _cell_length_b 13.8737(5) _cell_length_c 21.1162(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.5310(10) _cell_angle_gamma 90.00 _cell_volume 3964.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 6279 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.84 _exptl_crystal_description block _exptl_crystal_colour light-yellow _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1368 _exptl_absorpt_coefficient_mu 0.629 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5720 _exptl_absorpt_correction_T_max 0.7870 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31705 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0374 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6985 _reflns_number_gt 5429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _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^)+(0.1716P)^2^+12.1493P] 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 6985 _refine_ls_number_parameters 386 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1140 _refine_ls_R_factor_gt 0.0952 _refine_ls_wR_factor_ref 0.3045 _refine_ls_wR_factor_gt 0.2827 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.023 _refine_ls_shift/su_mean 0.001 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 0.28957(5) 0.21753(5) 0.75773(3) 0.0360(3) Uani 1 1 d . . . S1 S 0.3565(4) -0.1053(4) 0.6959(3) 0.0932(15) Uiso 0.50 1 d P A 1 S2 S 0.2450(5) 0.5569(5) 0.7873(3) 0.1050(17) Uiso 0.50 1 d P B 1 S1' S 0.3769(5) -0.0782(5) 0.6724(3) 0.0975(16) Uiso 0.50 1 d P A 2 S2' S 0.1904(10) 0.5390(9) 0.7494(7) 0.101(3) Uiso 0.25 1 d P B 2 S2" S 0.1811(12) 0.5295(11) 0.7861(8) 0.121(4) Uiso 0.25 1 d P B 3 N1 N 0.4317(3) 0.2171(3) 0.8187(2) 0.0389(11) Uani 1 1 d . . . N2 N 0.7294(5) 0.2398(6) 1.0026(4) 0.079(2) Uani 1 1 d . . . N3 N 0.8261(5) 0.2259(5) 1.0379(4) 0.080(2) Uani 1 1 d . . . N4 N 1.1465(4) 0.2847(4) 1.1960(3) 0.0480(12) Uani 1 1 d . . . N5 N 0.2309(4) 0.1576(4) 0.8345(2) 0.0536(14) Uani 1 1 d . . . N6 N 0.0177(5) 0.0260(5) 0.9773(3) 0.0741(19) Uani 1 1 d . . . N7 N 0.3474(4) 0.2757(3) 0.6809(2) 0.0414(11) Uani 1 1 d . . . N8 N 0.4901(5) 0.4850(4) 0.5299(3) 0.0618(15) Uani 1 1 d . . . N9 N 0.3129(4) 0.0821(4) 0.7274(2) 0.0474(12) Uani 1 1 d . A . N10 N 0.2637(4) 0.3538(4) 0.7864(3) 0.0520(13) Uani 1 1 d . B . C1 C 0.5068(4) 0.1710(5) 0.8031(3) 0.0470(14) Uani 1 1 d . . . H1A H 0.4967 0.1408 0.7623 0.056 Uiso 1 1 calc R . . C2 C 0.5989(4) 0.1650(5) 0.8435(3) 0.0520(15) Uani 1 1 d . . . H2A H 0.6500 0.1314 0.8303 0.062 Uiso 1 1 calc R . . C3 C 0.6153(5) 0.2087(5) 0.9034(3) 0.0549(17) Uani 1 1 d . . . C4 C 0.5380(5) 0.2582(5) 0.9206(3) 0.0537(16) Uani 1 1 d . . . H4A H 0.5466 0.2891 0.9610 0.064 Uiso 1 1 calc R . . C5 C 0.4486(4) 0.2612(5) 0.8772(3) 0.0462(14) Uani 1 1 d . . . H5A H 0.3965 0.2956 0.8887 0.055 Uiso 1 1 calc R . . C6 C 0.7135(5) 0.2027(6) 0.9473(4) 0.066(2) Uani 1 1 d . . . H6A H 0.7650 0.1706 0.9335 0.080 Uiso 1 1 calc R . . C7 C 0.8576(6) 0.2919(6) 1.0750(4) 0.074(2) Uani 1 1 d . . . H7A H 0.8168 0.3452 1.0776 0.088 Uiso 1 1 calc R . . C8 C 1.1088(5) 0.2084(5) 1.1599(3) 0.0591(19) Uani 1 1 d . . . H8A H 1.1475 0.1523 1.1625 0.071 Uiso 1 1 calc R . . C9 C 1.0180(6) 0.2079(5) 1.1199(4) 0.069(2) Uani 1 1 d . . . H9A H 0.9954 0.1528 1.0952 0.082 Uiso 1 1 calc R . . C10 C 0.9581(5) 0.2895(5) 1.1156(4) 0.0637(19) Uani 1 1 d . . . C11 C 0.9964(5) 0.3666(6) 1.1536(4) 0.079(3) Uani 1 1 d . . . H11A H 0.9583 0.4227 1.1530 0.094 Uiso 1 1 calc R . . C12 C 1.0896(5) 0.3628(5) 1.1922(4) 0.066(2) Uani 1 1 d . . . H12A H 1.1142 0.4173 1.2170 0.079 Uiso 1 1 calc R . . C13 C 0.1548(6) 0.1943(8) 0.8515(4) 0.084(3) Uani 1 1 d . . . H13A H 0.1289 0.2532 0.8334 0.101 Uiso 1 1 calc R . . C14 C 0.1083(6) 0.1459(7) 0.8985(5) 0.085(3) Uani 1 1 d . . . H14A H 0.0522 0.1716 0.9107 0.102 Uiso 1 1 calc R . . C15 C 0.1495(6) 0.0630(5) 0.9234(4) 0.0654(19) Uani 1 1 d . . . C16 C 0.2290(6) 0.0256(6) 0.9084(4) 0.072(2) Uani 1 1 d . . . H16A H 0.2588 -0.0307 0.9283 0.086 Uiso 1 1 calc R . . C17 C 0.2656(6) 0.0740(6) 0.8620(3) 0.0643(19) Uani 1 1 d . . . H17A H 0.3196 0.0461 0.8484 0.077 Uiso 1 1 calc R . . C18 C 0.1031(7) 0.0102(7) 0.9724(4) 0.078(2) Uani 1 1 d . . . H18A H 0.1407 -0.0358 0.9998 0.094 Uiso 1 1 calc R . . C19 C 0.3227(5) 0.2393(5) 0.6215(3) 0.0536(16) Uani 1 1 d . . . H19A H 0.2837 0.1834 0.6145 0.064 Uiso 1 1 calc R . . C20 C 0.3527(6) 0.2811(5) 0.5693(3) 0.0583(18) Uani 1 1 d . . . H20A H 0.3334 0.2542 0.5276 0.070 Uiso 1 1 calc R . . C21 C 0.4108(5) 0.3624(4) 0.5790(3) 0.0477(14) Uani 1 1 d . . . C22 C 0.4383(5) 0.3990(5) 0.6415(3) 0.0487(14) Uani 1 1 d . . . H22A H 0.4789 0.4538 0.6501 0.058 Uiso 1 1 calc R . . C23 C 0.4053(4) 0.3540(4) 0.6900(3) 0.0447(13) Uani 1 1 d . . . H23A H 0.4241 0.3792 0.7322 0.054 Uiso 1 1 calc R . . C24 C 0.4413(5) 0.4083(5) 0.5235(3) 0.0532(16) Uani 1 1 d . . . H24A H 0.4238 0.3793 0.4823 0.064 Uiso 1 1 calc R . . C25 C 0.3334(5) 0.0108(6) 0.7103(4) 0.0626(18) Uani 1 1 d . . . C26 C 0.2449(7) 0.4340(7) 0.7846(4) 0.085(3) Uani 1 1 d . . . O1 O 0.1683(15) 0.5408(15) 0.6310(10) 0.156(7) Uiso 0.50 1 d P . . H1 H 0.1912 0.5909 0.6573 0.234 Uiso 0.50 1 d PR . . H1' H 0.2224 0.5023 0.6417 0.234 Uiso 0.50 1 d PR . . O2 O -0.117(3) 0.296(2) 0.7839(17) 0.250(15) Uiso 0.50 1 d P . . H2 H -0.0777 0.3283 0.7701 0.374 Uiso 0.50 1 d PR . . H2' H -0.1244 0.3161 0.8174 0.374 Uiso 0.50 1 d PR . . O3 O 0.4008(18) 0.477(2) 0.9815(14) 0.202(10) Uiso 0.50 1 d PD . . H3 H 0.3750 0.4130 0.9883 0.303 Uiso 0.50 1 d PR . . C27 C 0.4392(19) 0.522(2) 0.9329(11) 0.148(10) Uiso 0.50 1 d PD . . H27A H 0.4057 0.5844 0.9220 0.178 Uiso 0.50 1 calc PR . . H27B H 0.4253 0.4822 0.8938 0.178 Uiso 0.50 1 calc PR . . C28 C 0.5471(19) 0.539(3) 0.9523(17) 0.170(13) Uiso 0.50 1 d PD . . H28A H 0.5700 0.5718 0.9182 0.255 Uiso 0.50 1 d PR . . H28B H 0.5610 0.5783 0.9908 0.255 Uiso 0.50 1 d PR . . H28C H 0.5802 0.4784 0.9610 0.255 Uiso 0.50 1 d PR . . O4 O 0.253(3) 0.444(3) 0.982(2) 0.32(2) Uiso 0.50 1 d PD . . H4 H 0.2830 0.4825 1.0091 0.487 Uiso 0.50 1 d PR . . C29 C 0.155(2) 0.441(3) 0.9876(18) 0.180(14) Uiso 0.50 1 d PD . . H29A H 0.1400 0.3758 1.0008 0.217 Uiso 0.50 1 calc PR . . H29B H 0.1116 0.4543 0.9454 0.217 Uiso 0.50 1 calc PR . . C30 C 0.135(3) 0.512(3) 1.036(2) 0.210(17) Uiso 0.50 1 d PD . . H30A H 0.0845 0.5576 1.0162 0.315 Uiso 0.50 1 d PR . . H30B H 0.1961 0.5471 1.0536 0.315 Uiso 0.50 1 d PR . . H30C H 0.1141 0.4791 1.0715 0.315 Uiso 0.50 1 d PR . . 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 0.0283(4) 0.0476(5) 0.0317(4) 0.0113(3) 0.0055(3) -0.0062(3) N1 0.032(2) 0.047(3) 0.036(2) 0.0117(19) 0.0045(19) -0.0057(19) N2 0.049(3) 0.092(5) 0.079(5) -0.005(4) -0.025(3) 0.003(3) N3 0.049(3) 0.084(5) 0.087(5) -0.011(4) -0.030(3) 0.010(3) N4 0.035(3) 0.056(3) 0.049(3) -0.017(2) 0.000(2) 0.006(2) N5 0.038(3) 0.080(4) 0.043(3) 0.018(3) 0.011(2) -0.015(3) N6 0.083(4) 0.081(4) 0.076(4) 0.013(3) 0.054(4) -0.010(3) N7 0.042(3) 0.049(3) 0.035(2) 0.007(2) 0.011(2) -0.010(2) N8 0.090(4) 0.063(4) 0.043(3) 0.010(3) 0.038(3) -0.014(3) N9 0.047(3) 0.048(3) 0.047(3) 0.003(2) 0.007(2) -0.009(2) N10 0.045(3) 0.063(4) 0.049(3) 0.004(3) 0.011(2) 0.003(3) C1 0.037(3) 0.057(4) 0.045(3) 0.003(3) 0.006(2) -0.004(3) C2 0.036(3) 0.054(4) 0.062(4) 0.002(3) 0.002(3) 0.004(3) C3 0.038(3) 0.059(4) 0.059(4) 0.010(3) -0.008(3) -0.004(3) C4 0.047(4) 0.067(4) 0.042(3) 0.004(3) -0.003(3) -0.008(3) C5 0.040(3) 0.058(4) 0.040(3) 0.005(3) 0.004(2) -0.005(3) C6 0.044(4) 0.067(5) 0.076(5) 0.004(4) -0.012(3) -0.001(3) C7 0.047(4) 0.079(5) 0.080(5) -0.006(4) -0.016(4) 0.008(4) C8 0.041(3) 0.063(4) 0.064(4) -0.029(3) -0.007(3) 0.015(3) C9 0.057(4) 0.064(5) 0.072(5) -0.026(4) -0.016(4) 0.007(3) C10 0.042(4) 0.073(5) 0.066(4) -0.013(4) -0.010(3) 0.004(3) C11 0.050(4) 0.067(5) 0.104(6) -0.023(4) -0.015(4) 0.019(4) C12 0.045(3) 0.061(4) 0.080(5) -0.023(4) -0.011(3) 0.015(3) C13 0.065(5) 0.116(7) 0.084(6) 0.036(5) 0.045(4) 0.010(5) C14 0.065(5) 0.089(6) 0.111(7) 0.005(5) 0.044(5) 0.017(4) C15 0.064(4) 0.056(4) 0.074(5) 0.015(4) 0.011(4) -0.007(3) C16 0.069(5) 0.084(5) 0.067(5) 0.025(4) 0.025(4) 0.005(4) C17 0.077(5) 0.068(5) 0.050(4) 0.021(3) 0.017(3) -0.017(4) C18 0.089(6) 0.082(6) 0.071(5) 0.015(4) 0.032(4) -0.008(5) C19 0.066(4) 0.056(4) 0.039(3) 0.002(3) 0.012(3) -0.021(3) C20 0.079(5) 0.061(4) 0.037(3) 0.001(3) 0.018(3) -0.020(3) C21 0.059(4) 0.048(3) 0.041(3) 0.007(3) 0.023(3) -0.002(3) C22 0.058(4) 0.050(3) 0.042(3) 0.002(3) 0.020(3) -0.015(3) C23 0.047(3) 0.053(3) 0.035(3) 0.002(2) 0.013(2) -0.015(3) C24 0.073(4) 0.055(4) 0.039(3) 0.006(3) 0.027(3) -0.006(3) C25 0.050(4) 0.072(5) 0.060(4) -0.002(4) -0.001(3) 0.001(4) C26 0.100(7) 0.083(6) 0.081(6) 0.006(5) 0.040(5) 0.032(5) _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 N9 2.033(6) . ? Ni1 N10 2.040(6) . ? Ni1 N1 2.107(4) . ? Ni1 N7 2.118(4) . ? Ni1 N4 2.123(5) 4_465 ? Ni1 N5 2.133(5) . ? S1 C25 1.682(11) . ? S2 C26 1.706(12) . ? S1' C25 1.654(10) . ? S2' C26 1.733(16) . ? S2" C26 1.597(18) . ? N1 C1 1.325(8) . ? N1 C5 1.351(8) . ? N2 C6 1.251(11) . ? N2 N3 1.398(8) . ? N3 C7 1.223(10) . ? N4 C12 1.333(8) . ? N4 C8 1.343(8) . ? N4 Ni1 2.123(5) 4_666 ? N5 C13 1.292(10) . ? N5 C17 1.339(9) . ? N6 C18 1.230(10) . ? N6 N6 1.372(11) 3_557 ? N7 C19 1.328(8) . ? N7 C23 1.339(7) . ? N8 C24 1.252(9) . ? N8 N8 1.413(9) 3_666 ? N9 C25 1.112(9) . ? N10 C26 1.141(10) . ? C1 C2 1.375(8) . ? C2 C3 1.377(10) . ? C3 C4 1.386(10) . ? C3 C6 1.473(9) . ? C4 C5 1.373(9) . ? C7 C10 1.469(9) . ? C8 C9 1.356(9) . ? C9 C10 1.395(10) . ? C10 C11 1.371(10) . ? C11 C12 1.372(9) . ? C13 C14 1.458(12) . ? C14 C15 1.340(12) . ? C15 C16 1.316(11) . ? C15 C18 1.521(11) . ? C16 C17 1.373(10) . ? C19 C20 1.386(9) . ? C20 C21 1.375(9) . ? C21 C22 1.387(9) . ? C21 C24 1.475(8) . ? C22 C23 1.361(8) . ? O3 C27 1.402(10) . ? O3 C28 1.45(3) 3_667 ? C27 C28 1.481(10) . ? C28 O3 1.45(3) 3_667 ? O4 C29 1.394(10) . ? C29 C30 1.500(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N9 Ni1 N10 178.7(2) . . ? N9 Ni1 N1 89.93(19) . . ? N10 Ni1 N1 91.3(2) . . ? N9 Ni1 N7 89.9(2) . . ? N10 Ni1 N7 89.7(2) . . ? N1 Ni1 N7 90.58(18) . . ? N9 Ni1 N4 89.1(2) . 4_465 ? N10 Ni1 N4 89.7(2) . 4_465 ? N1 Ni1 N4 179.0(2) . 4_465 ? N7 Ni1 N4 89.66(19) . 4_465 ? N9 Ni1 N5 89.5(2) . . ? N10 Ni1 N5 90.9(2) . . ? N1 Ni1 N5 89.69(18) . . ? N7 Ni1 N5 179.4(2) . . ? N4 Ni1 N5 90.06(19) 4_465 . ? C1 N1 C5 117.2(5) . . ? C1 N1 Ni1 122.0(4) . . ? C5 N1 Ni1 120.7(4) . . ? C6 N2 N3 113.3(7) . . ? C7 N3 N2 114.0(7) . . ? C12 N4 C8 117.0(5) . . ? C12 N4 Ni1 120.7(4) . 4_666 ? C8 N4 Ni1 122.3(4) . 4_666 ? C13 N5 C17 117.3(6) . . ? C13 N5 Ni1 121.8(5) . . ? C17 N5 Ni1 120.5(5) . . ? C18 N6 N6 117.5(9) . 3_557 ? C19 N7 C23 117.8(5) . . ? C19 N7 Ni1 121.1(4) . . ? C23 N7 Ni1 121.0(4) . . ? C24 N8 N8 111.0(7) . 3_666 ? C25 N9 Ni1 173.9(6) . . ? C26 N10 Ni1 161.3(6) . . ? N1 C1 C2 123.2(6) . . ? C1 C2 C3 119.4(6) . . ? C2 C3 C4 118.3(6) . . ? C2 C3 C6 120.0(7) . . ? C4 C3 C6 121.7(7) . . ? C5 C4 C3 118.6(6) . . ? N1 C5 C4 123.3(6) . . ? N2 C6 C3 121.1(8) . . ? N3 C7 C10 121.3(7) . . ? N4 C8 C9 123.5(6) . . ? C8 C9 C10 119.7(6) . . ? C11 C10 C9 116.4(6) . . ? C11 C10 C7 121.4(7) . . ? C9 C10 C7 122.1(7) . . ? C10 C11 C12 120.9(7) . . ? N4 C12 C11 122.4(6) . . ? N5 C13 C14 121.1(8) . . ? C15 C14 C13 116.6(7) . . ? C16 C15 C14 123.6(8) . . ? C16 C15 C18 118.3(7) . . ? C14 C15 C18 118.2(8) . . ? C15 C16 C17 115.9(8) . . ? N5 C17 C16 125.4(8) . . ? N6 C18 C15 122.0(8) . . ? N7 C19 C20 122.2(6) . . ? C21 C20 C19 119.4(6) . . ? C20 C21 C22 118.2(5) . . ? C20 C21 C24 119.6(6) . . ? C22 C21 C24 122.1(6) . . ? C23 C22 C21 118.7(6) . . ? N7 C23 C22 123.6(5) . . ? N8 C24 C21 121.4(6) . . ? N9 C25 S1' 165.4(8) . . ? N9 C25 S1 169.4(8) . . ? S1' C25 S1 25.2(3) . . ? N10 C26 S2" 158.6(11) . . ? N10 C26 S2 167.1(10) . . ? S2" C26 S2 33.6(6) . . ? N10 C26 S2' 155.3(10) . . ? S2" C26 S2' 28.3(6) . . ? S2 C26 S2' 34.0(5) . . ? C27 O3 C28 126(2) . 3_667 ? O3 C27 C28 112.9(11) . . ? O3 C28 C27 120(2) 3_667 . ? O4 C29 C30 111.6(11) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.292 _refine_diff_density_min -0.944 _refine_diff_density_rms 0.157