# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address R.Sekiya ; Department of Life Sciences, Graduate School of Arts and Sciences, The University of Tokyo 3-8-1 Komaba, Meguro-ku, Tokyo 153-8902, Japan ; S.Nishikiori ; Department of Basic Sciences, Graduate School of Arts and Sciences, The University of Tokyo 3-8-1 Komaba, Meguro-ku, Tokyo 153-8902, Japan ; _publ_contact_author 'Sekiya, Ryo' _publ_contact_author_address ; Department of Life Sciences, Graduate School of Arts and Sciences, The University of Tokyo 3-8-1 Komaba, Meguro-ku, Tokyo 153-8902, Japan ; _publ_contact_author_email csekiya@mail.ecc.u-tokyo.ac.jp _publ_contact_author_fax +81-3-5454-6601 _publ_contact_author_phone +81-3-5454-6601 _publ_contact_author_name 'Sekiya, Ryo' data_dibenzanthracene _database_code_depnum_ccdc_archive 'CCDC 759628' #TrackingRef '- Revised_dibenzanthracene.cif' _audit_creation_date 2009-11-11T14:03:33-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H22 N4 Ni O4 S2, 0.5(C22 H14)' _chemical_formula_sum 'C41 H29 N4 Ni O4 S2' _chemical_formula_weight 764.53 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.9753(4) _cell_length_b 10.7633(6) _cell_length_c 29.7359(11) _cell_angle_alpha 86.267(2) _cell_angle_beta 46.207(2) _cell_angle_gamma 72.569(2) _cell_volume 1720.05(14) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_theta_min 0.97 _cell_measurement_theta_max 27.48 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.476 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 790 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_absorpt_correction_T_min 0.8093 _exptl_absorpt_correction_T_max 0.8976 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 153(2) _diffrn_radiation_probe X-ray _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0260 _diffrn_reflns_av_unetI/netI 0.0348 _diffrn_reflns_number 14211 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.97 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.977 _diffrn_measured_fraction_theta_max 0.977 _reflns_number_total 7712 _reflns_number_gt 5952 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection RAPID-AUTO _computing_cell_refinement RAPID-AUTO _computing_data_reduction RAPID-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0999P)^2^+0.2859P] 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_number_reflns 7712 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0634 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1246 _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 _refine_diff_density_max 0.556 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.125 0.123 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.339 1.112 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C36 C 0.5701(7) 0.5496(4) 0.3514(2) 0.0659(12) Uani 1 1 d . . . H36 H 0.7224 0.5654 0.3231 0.079 Uiso 1 1 calc R . . C37 C 0.4612(7) 0.5404(4) 0.4111(2) 0.0623(11) Uani 1 1 d . . . H37 H 0.539 0.5483 0.4239 0.075 Uiso 1 1 calc R . . C28 C 0.2284(7) 0.5187(3) 0.4558(2) 0.0576(10) Uani 1 1 d . . . C29 C 0.1131(7) 0.5065(3) 0.4363(2) 0.0566(10) Uani 1 1 d . . . C27 C 0.1147(7) 0.5115(3) 0.5179(2) 0.0580(10) Uani 1 1 d . . . H27 H 0.1966 0.5191 0.5295 0.07 Uiso 1 1 calc R . . C30 C 0.2366(7) 0.5137(3) 0.3708(2) 0.0564(10) Uani 1 1 d . . . C31 C 0.1413(9) 0.4984(4) 0.3464(2) 0.0663(12) Uani 1 1 d . . . H31 H -0.0107 0.4826 0.3734 0.08 Uiso 1 1 calc R . . C32 C 0.2629(9) 0.5059(4) 0.2846(2) 0.0692(12) Uani 1 1 d . . . H32 H 0.1936 0.4951 0.2696 0.083 Uiso 1 1 calc R . . C33 C 0.4841(9) 0.5289(4) 0.2438(2) 0.0725(13) Uani 1 1 d . . . H33 H 0.567 0.5338 0.2011 0.087 Uiso 1 1 calc R . . C34 C 0.5825(8) 0.5446(4) 0.2660(2) 0.0700(13) Uani 1 1 d . . . H34 H 0.7338 0.5613 0.2383 0.084 Uiso 1 1 calc R . . C35 C 0.4632(7) 0.5364(3) 0.3292(2) 0.0601(11) Uani 1 1 d . . . C1 C 0.2917(4) 0.9385(2) -0.05243(11) 0.0205(5) Uani 1 1 d . . . C2 C -0.2912(4) 0.5588(2) 0.05127(11) 0.0192(5) Uani 1 1 d . . . C11 C 0.1666(5) 0.7511(3) 0.04740(12) 0.0296(6) Uani 1 1 d . . . H11 H 0.3247 0.727 0.0046 0.035 Uiso 1 1 calc R . . C12 C 0.1544(5) 0.7690(3) 0.09544(12) 0.0301(6) Uani 1 1 d . A . H12 H 0.301 0.7591 0.085 0.036 Uiso 1 1 calc R . . C13 C -0.0725(5) 0.8014(3) 0.15911(12) 0.0246(5) Uani 1 1 d . . . C14 C -0.2746(6) 0.8154(4) 0.16921(14) 0.0485(9) Uani 1 1 d . A . H14 H -0.4345 0.8377 0.2115 0.058 Uiso 1 1 calc R . . C15 C -0.2482(6) 0.7974(4) 0.11882(14) 0.0449(9) Uani 1 1 d . . . H15 H -0.3923 0.808 0.1279 0.054 Uiso 1 1 calc R A . C20 C 0.1036(6) 0.8372(3) 0.86667(14) 0.0322(6) Uani 1 1 d . . . H20 H 0.1782 0.8878 0.8687 0.039 Uiso 1 1 calc R . . C19 C 0.1076(6) 0.8459(3) 0.81980(14) 0.0331(6) Uani 1 1 d . A . H19 H 0.1859 0.9005 0.7902 0.04 Uiso 1 1 calc R . . C18 C -0.0020(5) 0.7755(2) 0.81531(11) 0.0231(5) Uani 1 1 d . . . C17 C -0.1128(5) 0.6974(3) 0.86074(12) 0.0244(5) Uani 1 1 d . A . H17 H -0.1927 0.6478 0.8605 0.029 Uiso 1 1 calc R . . C16 C -0.1060(5) 0.6926(2) 0.90594(12) 0.0230(5) Uani 1 1 d . . . H16 H -0.1807 0.6378 0.9359 0.028 Uiso 1 1 calc R A . N1 N 0.2172(4) 0.8686(2) -0.05736(10) 0.0221(4) Uani 1 1 d . A . N2 N -0.2205(4) 0.6430(2) 0.02563(10) 0.0229(4) Uani 1 1 d . A . N11 N -0.0297(4) 0.7657(2) 0.05763(10) 0.0239(4) Uani 1 1 d . A . N21 N 0.0002(4) 0.7609(2) 0.91005(10) 0.0214(4) Uani 1 1 d . . . S1 S 0.39295(12) 1.03609(6) -0.04284(3) 0.02512(15) Uani 1 1 d . . . S2 S -0.39229(12) 0.44009(6) 0.08799(3) 0.02484(15) Uani 1 1 d . . . Ni1 Ni -0.00870(6) 0.75935(3) -0.017695(14) 0.01905(11) Uani 1 1 d . . . C60A C -0.0756(15) 0.8266(8) 0.2092(4) 0.023(2) Uiso 0.506(4) 1 d P A 1 C61A C 0.1060(10) 0.8563(6) 0.1969(3) 0.0293(12) Uiso 0.506(4) 1 d P A 1 H61A H 0.2397 0.8654 0.1551 0.035 Uiso 0.506(4) 1 calc PR A 1 C62A C 0.1007(11) 0.8735(6) 0.2432(3) 0.0339(13) Uiso 0.506(4) 1 d P A 1 H62A H 0.2276 0.8977 0.2328 0.041 Uiso 0.506(4) 1 calc PR A 1 C63A C -0.0792(12) 0.8572(6) 0.3035(3) 0.0276(13) Uiso 0.506(4) 1 d P A 1 C64A C -0.2746(13) 0.8353(6) 0.3187(3) 0.0306(13) Uiso 0.506(4) 1 d P A 1 H64A H -0.4104 0.8314 0.3614 0.037 Uiso 0.506(4) 1 calc PR A 1 C65A C -0.2770(13) 0.8188(7) 0.2729(3) 0.0330(14) Uiso 0.506(4) 1 d P A 1 H65A H -0.4117 0.8026 0.2842 0.04 Uiso 0.506(4) 1 calc PR A 1 C66A C -0.0605(11) 0.8646(5) 0.3485(3) 0.0288(12) Uiso 0.506(4) 1 d P A 1 H66A H 0.0833 0.8788 0.3324 0.035 Uiso 0.506(4) 1 calc PR A 1 C67A C -0.2155(10) 0.8542(5) 0.4085(2) 0.0276(12) Uiso 0.506(4) 1 d P A 1 H67A H -0.3694 0.847 0.4288 0.033 Uiso 0.506(4) 1 calc PR A 1 C68A C -0.1483(15) 0.8541(5) 0.4440(4) 0.0235(12) Uiso 0.506(4) 1 d P A 1 C69A C -0.0786(12) 0.8146(5) 0.6357(3) 0.0280(12) Uiso 0.506(4) 1 d P A 1 H69A H -0.2315 0.8133 0.6526 0.034 Uiso 0.506(4) 1 calc PR A 1 C70A C 0.0827(10) 0.8254(5) 0.5750(2) 0.0289(12) Uiso 0.506(4) 1 d P A 1 H70A H 0.2414 0.8252 0.5544 0.035 Uiso 0.506(4) 1 calc PR A 1 C71A C 0.0093(15) 0.8376(6) 0.5406(4) 0.0292(13) Uiso 0.506(4) 1 d P A 1 C72A C -0.0516(14) 0.8046(6) 0.6801(3) 0.0249(14) Uiso 0.506(4) 1 d P A 1 C73A C -0.2384(14) 0.7872(7) 0.7403(4) 0.0311(19) Uiso 0.506(4) 1 d P A 1 H73A H -0.3828 0.7841 0.7525 0.037 Uiso 0.506(4) 1 calc PR A 1 C74A C -0.2195(15) 0.7744(8) 0.7829(4) 0.024(2) Uiso 0.506(4) 1 d P A 1 H74A H -0.3491 0.7584 0.8233 0.029 Uiso 0.506(4) 1 calc PR A 1 C75A C -0.0234(17) 0.7834(9) 0.7701(4) 0.024(3) Uiso 0.506(4) 1 d P A 1 C76A C 0.194(2) 0.7886(11) 0.7040(5) 0.035(3) Uiso 0.506(4) 1 d P A 1 H76A H 0.3468 0.7803 0.6902 0.042 Uiso 0.506(4) 1 calc PR A 1 C77A C 0.1596(15) 0.8071(7) 0.6625(3) 0.0314(18) Uiso 0.506(4) 1 d P A 1 H77A H 0.2864 0.8215 0.6213 0.038 Uiso 0.506(4) 1 calc PR A 1 O61A O 0.0459(11) 0.8629(4) 0.4211(2) 0.0290(10) Uiso 0.506(4) 1 d P A 1 O62A O -0.3184(9) 0.8439(5) 0.5026(2) 0.0392(12) Uiso 0.506(4) 1 d P A 1 H6A H -0.2726 0.8447 0.5209 0.059 Uiso 0.506(4) 1 calc PR A 1 O71A O -0.1939(11) 0.8394(4) 0.5654(2) 0.0320(10) Uiso 0.506(4) 1 d P A 1 O72A O 0.1836(9) 0.8465(4) 0.4813(2) 0.0359(11) Uiso 0.506(4) 1 d P A 1 H7A H 0.1338 0.8534 0.4637 0.054 Uiso 0.506(4) 1 calc PR A 1 C60B C -0.1072(15) 0.8154(8) 0.2137(4) 0.020(2) Uiso 0.494(4) 1 d P A 2 C61B C 0.1045(10) 0.7800(6) 0.2032(3) 0.0274(12) Uiso 0.494(4) 1 d P A 2 H61B H 0.2653 0.7461 0.1611 0.033 Uiso 0.494(4) 1 calc PR A 2 C62B C 0.0812(11) 0.7941(6) 0.2533(3) 0.0315(13) Uiso 0.494(4) 1 d P A 2 H62B H 0.225 0.7702 0.2456 0.038 Uiso 0.494(4) 1 calc PR A 2 C63B C -0.1590(12) 0.8444(5) 0.3164(3) 0.0222(12) Uiso 0.494(4) 1 d P A 2 C64B C -0.3617(12) 0.8782(6) 0.3258(3) 0.0274(12) Uiso 0.494(4) 1 d P A 2 H64B H -0.523 0.9115 0.3679 0.033 Uiso 0.494(4) 1 calc PR A 2 C65B C -0.3370(11) 0.8650(6) 0.2757(3) 0.0260(12) Uiso 0.494(4) 1 d P A 2 H65B H -0.4821 0.8907 0.2839 0.031 Uiso 0.494(4) 1 calc PR A 2 C66B C -0.1959(11) 0.8583(5) 0.3720(3) 0.0271(12) Uiso 0.494(4) 1 d P A 2 H66B H -0.361 0.8807 0.4129 0.033 Uiso 0.494(4) 1 calc PR A 2 C67B C -0.0185(11) 0.8423(6) 0.3702(3) 0.0322(13) Uiso 0.494(4) 1 d P A 2 H67B H 0.1458 0.822 0.3292 0.039 Uiso 0.494(4) 1 calc PR A 2 C68B C -0.0524(17) 0.8529(6) 0.4248(3) 0.0297(14) Uiso 0.494(4) 1 d P A 2 C69B C 0.0372(12) 0.8245(6) 0.6144(3) 0.0282(12) Uiso 0.494(4) 1 d P A 2 H69B H 0.1907 0.8243 0.5742 0.034 Uiso 0.494(4) 1 calc PR A 2 C70B C -0.1421(12) 0.8384(6) 0.6181(3) 0.0358(14) Uiso 0.494(4) 1 d P A 2 H70B H -0.2977 0.84 0.6581 0.043 Uiso 0.494(4) 1 calc PR A 2 C71B C -0.1174(17) 0.8517(7) 0.5638(3) 0.0338(15) Uiso 0.494(4) 1 d P A 2 C72B C 0.0242(14) 0.8091(6) 0.6662(3) 0.0242(14) Uiso 0.494(4) 1 d P A 2 C73B C -0.1874(16) 0.8002(8) 0.7272(4) 0.033(2) Uiso 0.494(4) 1 d P A 2 H73B H -0.3259 0.8008 0.7354 0.04 Uiso 0.494(4) 1 calc PR A 2 C74B C -0.1959(18) 0.7905(9) 0.7756(5) 0.034(3) Uiso 0.494(4) 1 d P A 2 H74B H -0.3403 0.7865 0.8169 0.04 Uiso 0.494(4) 1 calc PR A 2 C75B C 0.0117(17) 0.7868(9) 0.7625(4) 0.021(3) Uiso 0.494(4) 1 d P A 2 C76B C 0.198(2) 0.8065(11) 0.7059(5) 0.033(3) Uiso 0.494(4) 1 d P A 2 H76B H 0.324 0.82 0.6999 0.039 Uiso 0.494(4) 1 calc PR A 2 C77B C 0.2229(15) 0.8090(7) 0.6560(3) 0.0308(18) Uiso 0.494(4) 1 d P A 2 H77B H 0.3722 0.8106 0.615 0.037 Uiso 0.494(4) 1 calc PR A 2 O61B O -0.2747(12) 0.8685(5) 0.4803(3) 0.0473(13) Uiso 0.494(4) 1 d P A 2 H6C H -0.2773 0.8735 0.5088 0.071 Uiso 0.494(4) 1 calc PR A 2 O62B O 0.1222(10) 0.8454(5) 0.4170(2) 0.0356(13) Uiso 0.494(4) 1 d P A 2 O71B O 0.0962(11) 0.8468(5) 0.5107(3) 0.0414(12) Uiso 0.494(4) 1 d P A 2 H7B H 0.0942 0.8549 0.4827 0.062 Uiso 0.494(4) 1 calc PR A 2 O72B O -0.2975(11) 0.8648(5) 0.5729(2) 0.0438(13) Uiso 0.494(4) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C36 0.039(2) 0.041(2) 0.089(3) -0.004(2) -0.037(2) -0.0058(17) C37 0.047(2) 0.041(2) 0.092(3) 0.008(2) -0.048(2) -0.0115(17) C28 0.048(2) 0.0246(16) 0.092(3) 0.0074(17) -0.048(2) -0.0078(15) C29 0.051(2) 0.0212(15) 0.092(3) 0.0079(16) -0.051(2) -0.0071(15) C27 0.053(2) 0.0293(17) 0.096(3) 0.0112(18) -0.055(2) -0.0120(16) C30 0.051(2) 0.0231(15) 0.083(3) 0.0047(16) -0.045(2) -0.0062(15) C31 0.068(3) 0.0362(19) 0.102(3) 0.014(2) -0.062(3) -0.0200(19) C32 0.079(3) 0.037(2) 0.091(3) 0.006(2) -0.061(3) -0.016(2) C33 0.069(3) 0.044(2) 0.079(3) -0.008(2) -0.046(3) -0.010(2) C34 0.052(2) 0.038(2) 0.072(3) -0.0126(19) -0.030(2) -0.0061(18) C35 0.044(2) 0.0278(17) 0.081(3) -0.0085(17) -0.037(2) -0.0009(15) C1 0.0249(12) 0.0170(11) 0.0262(12) 0.0045(9) -0.0205(10) -0.0067(9) C2 0.0214(11) 0.0175(11) 0.0246(11) 0.0014(9) -0.0187(10) -0.0046(9) C11 0.0255(13) 0.0353(15) 0.0253(12) 0.0001(11) -0.0199(11) -0.0006(11) C12 0.0255(13) 0.0430(16) 0.0258(12) 0.0026(11) -0.0211(11) -0.0062(12) C13 0.0289(13) 0.0257(12) 0.0273(12) 0.0091(10) -0.0228(11) -0.0102(11) C14 0.0310(15) 0.100(3) 0.0278(14) 0.0260(17) -0.0217(13) -0.0365(18) C15 0.0356(16) 0.093(3) 0.0341(15) 0.0305(16) -0.0300(14) -0.0393(18) C20 0.0503(17) 0.0366(15) 0.0484(16) 0.0253(13) -0.0442(15) -0.0311(14) C19 0.0451(16) 0.0385(15) 0.0426(15) 0.0253(13) -0.0373(14) -0.0274(14) C18 0.0237(12) 0.0244(12) 0.0248(12) 0.0041(9) -0.0187(10) -0.0074(10) C17 0.0278(13) 0.0276(13) 0.0271(12) 0.0043(10) -0.0215(11) -0.0129(11) C16 0.0270(12) 0.0228(12) 0.0278(12) 0.0068(10) -0.0215(11) -0.0117(10) N1 0.0261(10) 0.0206(10) 0.0280(10) 0.0040(8) -0.0218(9) -0.0088(9) N2 0.0255(10) 0.0215(10) 0.0303(11) 0.0064(8) -0.0225(9) -0.0092(9) N11 0.0319(11) 0.0248(11) 0.0295(10) 0.0111(9) -0.0255(10) -0.0149(9) N21 0.0275(11) 0.0203(10) 0.0287(10) 0.0068(8) -0.0237(9) -0.0100(9) S1 0.0268(3) 0.0202(3) 0.0379(3) 0.0027(2) -0.0256(3) -0.0094(3) S2 0.0262(3) 0.0189(3) 0.0285(3) 0.0079(2) -0.0182(3) -0.0109(2) Ni1 0.02664(18) 0.01725(17) 0.02624(18) 0.00774(12) -0.02235(15) -0.01085(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C36 C37 1.346(6) . ? C36 C35 1.430(6) . ? C36 H36 0.95 . ? C37 C28 1.439(6) . ? C37 H37 0.95 . ? C28 C27 1.395(6) . ? C28 C29 1.421(6) . ? C29 C27 1.394(6) 2_566 ? C29 C30 1.462(6) . ? C27 C29 1.394(6) 2_566 ? C27 H27 0.95 . ? C30 C31 1.408(6) . ? C30 C35 1.410(6) . ? C31 C32 1.374(6) . ? C31 H31 0.95 . ? C32 C33 1.380(7) . ? C32 H32 0.95 . ? C33 C34 1.376(7) . ? C33 H33 0.95 . ? C34 C35 1.413(6) . ? C34 H34 0.95 . ? C1 N1 1.159(3) . ? C1 S1 1.644(3) . ? C2 N2 1.158(3) . ? C2 S2 1.640(2) . ? C11 N11 1.330(3) . ? C11 C12 1.385(4) . ? C11 H11 0.95 . ? C12 C13 1.395(4) . ? C12 H12 0.95 . ? C13 C14 1.379(4) . ? C13 C60B 1.454(8) . ? C13 C60A 1.513(9) . ? C14 C15 1.380(4) . ? C14 H14 0.95 . ? C15 N11 1.341(4) . ? C15 H15 0.95 . ? C20 N21 1.346(3) . ? C20 C19 1.370(4) . ? C20 H20 0.95 . ? C19 C18 1.389(4) . ? C19 H19 0.95 . ? C18 C17 1.399(4) . ? C18 C75A 1.463(10) . ? C18 C75B 1.497(10) . ? C17 C16 1.379(3) . ? C17 H17 0.95 . ? C16 N21 1.342(3) . ? C16 H16 0.95 . ? N1 Ni1 2.042(2) . ? N2 Ni1 2.032(2) . ? N11 Ni1 2.131(2) . ? N21 Ni1 2.099(2) 1_556 ? S1 Ni1 2.5135(7) 2_575 ? S2 Ni1 2.5345(7) 2_565 ? Ni1 N21 2.099(2) 1_554 ? Ni1 S1 2.5135(7) 2_575 ? Ni1 S2 2.5345(7) 2_565 ? C60A C61A 1.365(10) . ? C60A C65A 1.422(10) . ? C61A C62A 1.371(8) . ? C61A H61A 0.95 . ? C62A C63A 1.361(8) . ? C62A H62A 0.95 . ? C63A C64A 1.384(9) . ? C63A C66A 1.457(8) . ? C64A C65A 1.401(9) . ? C64A H64A 0.95 . ? C65A H65A 0.95 . ? C66A C67A 1.313(8) . ? C66A H66A 0.95 . ? C67A C68A 1.477(8) . ? C67A H67A 0.95 . ? C68A O61A 1.222(8) . ? C68A O62A 1.298(9) . ? C69A C70A 1.332(8) . ? C69A C72A 1.469(8) . ? C69A H69A 0.95 . ? C70A C71A 1.474(8) . ? C70A H70A 0.95 . ? C71A O71A 1.225(9) . ? C71A O72A 1.310(8) . ? C72A C73A 1.375(10) . ? C72A C77A 1.384(10) . ? C73A C74A 1.369(11) . ? C73A H73A 0.95 . ? C74A C75A 1.365(13) . ? C74A H74A 0.95 . ? C75A C76A 1.484(14) . ? C76A C77A 1.431(14) . ? C76A H76A 0.95 . ? C77A H77A 0.95 . ? O62A H6A 0.84 . ? O72A H7A 0.84 . ? C60B C65B 1.381(10) . ? C60B C61B 1.413(10) . ? C61B C62B 1.380(8) . ? C61B H61B 0.95 . ? C62B C63B 1.421(8) . ? C62B H62B 0.95 . ? C63B C64B 1.362(9) . ? C63B C66B 1.477(8) . ? C64B C65B 1.375(8) . ? C64B H64B 0.95 . ? C65B H65B 0.95 . ? C66B C67B 1.334(9) . ? C66B H66B 0.95 . ? C67B C68B 1.458(9) . ? C67B H67B 0.95 . ? C68B O62B 1.220(10) . ? C68B O61B 1.305(9) . ? C69B C70B 1.318(9) . ? C69B C72B 1.471(8) . ? C69B H69B 0.95 . ? C70B C71B 1.486(9) . ? C70B H70B 0.95 . ? C71B O72B 1.227(10) . ? C71B O71B 1.278(9) . ? C72B C77B 1.391(10) . ? C72B C73B 1.409(10) . ? C73B C74B 1.390(13) . ? C73B H73B 0.95 . ? C74B C75B 1.401(14) . ? C74B H74B 0.95 . ? C75B C76B 1.329(15) . ? C76B C77B 1.353(13) . ? C76B H76B 0.95 . ? C77B H77B 0.95 . ? O61B H6C 0.84 . ? O71B H7B 0.84 . ? 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 C37 C36 C35 121.9(4) . . ? C37 C36 H36 119 . . ? C35 C36 H36 119 . . ? C36 C37 C28 120.9(4) . . ? C36 C37 H37 119.6 . . ? C28 C37 H37 119.6 . . ? C27 C28 C29 120.1(4) . . ? C27 C28 C37 120.5(4) . . ? C29 C28 C37 119.4(4) . . ? C27 C29 C28 116.6(4) 2_566 . ? C27 C29 C30 124.3(4) 2_566 . ? C28 C29 C30 119.1(4) . . ? C29 C27 C28 123.3(4) 2_566 . ? C29 C27 H27 118.4 2_566 . ? C28 C27 H27 118.4 . . ? C31 C30 C35 117.4(4) . . ? C31 C30 C29 123.3(4) . . ? C35 C30 C29 119.2(4) . . ? C32 C31 C30 121.6(4) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C33 121.2(5) . . ? C31 C32 H32 119.4 . . ? C33 C32 H32 119.4 . . ? C34 C33 C32 118.9(5) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C33 C34 C35 121.4(5) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 119.3 . . ? C30 C35 C34 119.5(4) . . ? C30 C35 C36 119.5(4) . . ? C34 C35 C36 121.0(4) . . ? N1 C1 S1 177.8(2) . . ? N2 C2 S2 179.7(2) . . ? N11 C11 C12 123.9(2) . . ? N11 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C13 120.3(3) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 115.4(2) . . ? C14 C13 C60B 119.1(4) . . ? C12 C13 C60B 125.4(4) . . ? C14 C13 C60A 126.8(4) . . ? C12 C13 C60A 117.7(4) . . ? C60B C13 C60A 9.7(5) . . ? C13 C14 C15 121.0(3) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? N11 C15 C14 123.5(3) . . ? N11 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N21 C20 C19 123.8(2) . . ? N21 C20 H20 118.1 . . ? C19 C20 H20 118.1 . . ? C20 C19 C18 120.4(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C18 C17 116.1(2) . . ? C19 C18 C75A 125.4(4) . . ? C17 C18 C75A 118.4(4) . . ? C19 C18 C75B 118.2(4) . . ? C17 C18 C75B 125.7(4) . . ? C75A C18 C75B 8.4(6) . . ? C16 C17 C18 119.9(2) . . ? C16 C17 H17 120 . . ? C18 C17 H17 120 . . ? N21 C16 C17 123.7(2) . . ? N21 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C1 N1 Ni1 149.99(19) . . ? C2 N2 Ni1 159.75(19) . . ? C11 N11 C15 115.9(2) . . ? C11 N11 Ni1 122.51(17) . . ? C15 N11 Ni1 121.27(18) . . ? C16 N21 C20 116.0(2) . . ? C16 N21 Ni1 122.80(17) . 1_556 ? C20 N21 Ni1 121.07(17) . 1_556 ? C1 S1 Ni1 96.73(9) . 2_575 ? C2 S2 Ni1 100.81(9) . 2_565 ? N2 Ni1 N1 174.31(8) . . ? N2 Ni1 N21 92.59(8) . 1_554 ? N1 Ni1 N21 92.49(8) . 1_554 ? N2 Ni1 N11 87.80(8) . . ? N1 Ni1 N11 87.23(8) . . ? N21 Ni1 N11 177.60(8) 1_554 . ? N2 Ni1 S1 90.29(6) . 2_575 ? N1 Ni1 S1 92.58(6) . 2_575 ? N21 Ni1 S1 86.49(6) 1_554 2_575 ? N11 Ni1 S1 91.14(6) . 2_575 ? N2 Ni1 S2 92.61(6) . 2_565 ? N1 Ni1 S2 84.92(6) . 2_565 ? N21 Ni1 S2 89.01(6) 1_554 2_565 ? N11 Ni1 S2 93.34(6) . 2_565 ? S1 Ni1 S2 174.75(2) 2_575 2_565 ? C61A C60A C65A 117.3(7) . . ? C61A C60A C13 123.7(6) . . ? C65A C60A C13 119.0(7) . . ? C60A C61A C62A 121.8(6) . . ? C60A C61A H61A 119.1 . . ? C62A C61A H61A 119.1 . . ? C63A C62A C61A 122.6(6) . . ? C63A C62A H62A 118.7 . . ? C61A C62A H62A 118.7 . . ? C62A C63A C64A 117.1(5) . . ? C62A C63A C66A 119.6(6) . . ? C64A C63A C66A 123.3(6) . . ? C63A C64A C65A 121.6(5) . . ? C63A C64A H64A 119.2 . . ? C65A C64A H64A 119.2 . . ? C64A C65A C60A 119.3(6) . . ? C64A C65A H65A 120.4 . . ? C60A C65A H65A 120.4 . . ? C67A C66A C63A 128.8(6) . . ? C67A C66A H66A 115.6 . . ? C63A C66A H66A 115.6 . . ? C66A C67A C68A 119.4(6) . . ? C66A C67A H67A 120.3 . . ? C68A C67A H67A 120.3 . . ? O61A C68A O62A 123.0(5) . . ? O61A C68A C67A 124.1(7) . . ? O62A C68A C67A 112.9(6) . . ? C70A C69A C72A 128.7(6) . . ? C70A C69A H69A 115.7 . . ? C72A C69A H69A 115.7 . . ? C69A C70A C71A 118.5(6) . . ? C69A C70A H70A 120.8 . . ? C71A C70A H70A 120.8 . . ? O71A C71A O72A 124.2(6) . . ? O71A C71A C70A 123.1(7) . . ? O72A C71A C70A 112.8(6) . . ? C73A C72A C77A 118.9(6) . . ? C73A C72A C69A 118.8(6) . . ? C77A C72A C69A 122.2(6) . . ? C74A C73A C72A 121.1(7) . . ? C74A C73A H73A 119.5 . . ? C72A C73A H73A 119.5 . . ? C75A C74A C73A 123.2(8) . . ? C75A C74A H74A 118.4 . . ? C73A C74A H74A 118.4 . . ? C74A C75A C18 124.7(8) . . ? C74A C75A C76A 117.9(9) . . ? C18 C75A C76A 117.2(8) . . ? C77A C76A C75A 115.6(10) . . ? C77A C76A H76A 122.2 . . ? C75A C76A H76A 122.2 . . ? C72A C77A C76A 122.5(7) . . ? C72A C77A H77A 118.7 . . ? C76A C77A H77A 118.7 . . ? C68A O62A H6A 109.5 . . ? C71A O72A H7A 109.5 . . ? C65B C60B C61B 117.4(7) . . ? C65B C60B C13 123.7(7) . . ? C61B C60B C13 118.8(6) . . ? C62B C61B C60B 121.0(6) . . ? C62B C61B H61B 119.5 . . ? C60B C61B H61B 119.5 . . ? C61B C62B C63B 119.6(6) . . ? C61B C62B H62B 120.2 . . ? C63B C62B H62B 120.2 . . ? C64B C63B C62B 118.8(5) . . ? C64B C63B C66B 119.0(5) . . ? C62B C63B C66B 122.1(6) . . ? C63B C64B C65B 121.2(6) . . ? C63B C64B H64B 119.4 . . ? C65B C64B H64B 119.4 . . ? C64B C65B C60B 121.9(6) . . ? C64B C65B H65B 119 . . ? C60B C65B H65B 119 . . ? C67B C66B C63B 126.0(6) . . ? C67B C66B H66B 117 . . ? C63B C66B H66B 117 . . ? C66B C67B C68B 126.3(6) . . ? C66B C67B H67B 116.8 . . ? C68B C67B H67B 116.8 . . ? O62B C68B O61B 124.0(6) . . ? O62B C68B C67B 120.1(7) . . ? O61B C68B C67B 115.9(8) . . ? C70B C69B C72B 126.8(6) . . ? C70B C69B H69B 116.6 . . ? C72B C69B H69B 116.6 . . ? C69B C70B C71B 124.5(7) . . ? C69B C70B H70B 117.8 . . ? C71B C70B H70B 117.8 . . ? O72B C71B O71B 125.6(6) . . ? O72B C71B C70B 118.8(7) . . ? O71B C71B C70B 115.6(8) . . ? C77B C72B C73B 118.1(6) . . ? C77B C72B C69B 119.3(6) . . ? C73B C72B C69B 122.5(7) . . ? C74B C73B C72B 120.8(8) . . ? C74B C73B H73B 119.6 . . ? C72B C73B H73B 119.6 . . ? C73B C74B C75B 119.0(8) . . ? C73B C74B H74B 120.5 . . ? C75B C74B H74B 120.5 . . ? C76B C75B C74B 117.6(9) . . ? C76B C75B C18 124.1(9) . . ? C74B C75B C18 117.9(8) . . ? C75B C76B C77B 125.5(11) . . ? C75B C76B H76B 117.3 . . ? C77B C76B H76B 117.3 . . ? C76B C77B C72B 118.2(8) . . ? C76B C77B H77B 120.9 . . ? C72B C77B H77B 120.9 . . ? C68B O61B H6C 109.5 . . ? C71B O71B H7B 109.5 . . ? #===END #===END # Attachment '5396_web_deposit_cif_file_1_RyoSekiya_1305266004.cif' data_bromobenzoicacid _database_code_depnum_ccdc_archive 'CCDC 759629' #TrackingRef '5396_web_deposit_cif_file_1_RyoSekiya_1305266004.cif' _audit_creation_date 2009-11-11T14:07:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H22 N4 Ni O4 S2, C7 H5 Br O2' _chemical_formula_sum 'C37 H27 Br N4 Ni O6 S2' _chemical_formula_weight 826.37 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.89220(10) _cell_length_b 10.7080(2) _cell_length_c 29.7550(7) _cell_angle_alpha 91.0610(10) _cell_angle_beta 46.772(2) _cell_angle_gamma 74.8750(10) _cell_volume 1697.79(6) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_theta_min 0.98 _cell_measurement_theta_max 27.48 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.926 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.9098 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 153(2) _diffrn_radiation_probe X-ray _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_unetI/netI 0.0664 _diffrn_reflns_number 14793 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 0.98 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.96 _diffrn_measured_fraction_theta_max 0.96 _reflns_number_total 7479 _reflns_number_gt 5129 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection RAPID-AUTO _computing_cell_refinement RAPID-AUTO _computing_data_reduction RAPID-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0817P)^2^+1.1060P] 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_number_reflns 7479 _refine_ls_number_parameters 451 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.087 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1488 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.953 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.125 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2930(7) 0.9301(4) -0.05098(18) 0.0190(8) Uani 1 1 d . . . C2 C -0.2933(7) 0.5647(4) 0.05175(18) 0.0176(8) Uani 1 1 d . . . C11 C -0.2696(9) 0.8419(6) 0.1190(2) 0.0379(13) Uani 1 1 d . . . H11 H -0.4171 0.8726 0.1281 0.046 Uiso 1 1 calc R . . C12 C -0.2948(9) 0.8663(6) 0.1695(2) 0.0376(12) Uani 1 1 d . . . H12 H -0.4551 0.9157 0.2115 0.045 Uiso 1 1 calc R . . C13 C -0.0844(8) 0.8181(4) 0.1585(2) 0.0225(9) Uani 1 1 d . . . C14 C 0.1401(9) 0.7548(6) 0.0960(2) 0.0446(14) Uani 1 1 d . . . H14 H 0.2904 0.7216 0.0856 0.053 Uiso 1 1 calc R . . C15 C 0.1517(9) 0.7383(6) 0.0476(2) 0.0383(13) Uani 1 1 d . . . H15 H 0.3122 0.6967 0.0046 0.046 Uiso 1 1 calc R . . C16 C -0.1002(8) 0.8390(4) 0.2111(2) 0.0229(9) Uani 1 1 d . A . C17 C -0.3223(9) 0.8651(5) 0.2752(2) 0.0296(10) Uani 1 1 d . . . H17 H -0.4721 0.8764 0.2865 0.035 Uiso 1 1 calc R . . C18 C -0.3276(10) 0.8748(5) 0.3230(2) 0.0322(11) Uani 1 1 d . A . H18 H -0.4797 0.8904 0.3664 0.039 Uiso 1 1 calc R . . C19 C -0.1096(10) 0.8617(5) 0.3071(2) 0.0319(11) Uani 1 1 d . . . C20 C 0.1068(11) 0.8413(6) 0.2435(3) 0.0429(13) Uani 1 1 d . A . H20 H 0.255 0.8353 0.232 0.052 Uiso 1 1 calc R . . C21 C 0.1122(10) 0.8295(6) 0.1964(2) 0.0407(13) Uani 1 1 d . . . H21 H 0.2642 0.8147 0.153 0.049 Uiso 1 1 calc R A . C31 C 0.0885(8) 0.8298(4) 0.8680(2) 0.0213(8) Uani 1 1 d . . . H31 H 0.1588 0.8832 0.8721 0.026 Uiso 1 1 calc R . . C32 C 0.0873(8) 0.8376(4) 0.8220(2) 0.0218(9) Uani 1 1 d . . . H32 H 0.1585 0.8939 0.795 0.026 Uiso 1 1 calc R . . C33 C -0.0177(7) 0.7634(4) 0.81519(18) 0.0186(8) Uani 1 1 d . . . C34 C -0.1153(8) 0.6813(4) 0.85635(19) 0.0208(8) Uani 1 1 d . . . H34 H -0.189 0.628 0.8538 0.025 Uiso 1 1 calc R . . C35 C -0.1036(8) 0.6785(4) 0.90077(19) 0.0216(9) Uani 1 1 d . . . H35 H -0.1701 0.6218 0.928 0.026 Uiso 1 1 calc R . . C36 C -0.0299(8) 0.7719(4) 0.76770(19) 0.0209(8) Uani 1 1 d . A . C37 C 0.1484(9) 0.8024(5) 0.7110(2) 0.0290(10) Uani 1 1 d . . . H37 H 0.2799 0.8181 0.7025 0.035 Uiso 1 1 calc R . . C38 C 0.1357(10) 0.8102(5) 0.6666(2) 0.0327(11) Uani 1 1 d . A . H38 H 0.2595 0.8305 0.6281 0.039 Uiso 1 1 calc R . . C39 C -0.0560(10) 0.7888(5) 0.6782(2) 0.0341(11) Uani 1 1 d . . . C40 C -0.2316(9) 0.7574(5) 0.7344(2) 0.0329(11) Uani 1 1 d . A . H40 H -0.3625 0.7413 0.7428 0.039 Uiso 1 1 calc R . . C41 C -0.2198(8) 0.7492(5) 0.7786(2) 0.0276(10) Uani 1 1 d . . . H41 H -0.3428 0.7278 0.8168 0.033 Uiso 1 1 calc R A . C100 C 0.5390(9) 0.4631(5) 0.6989(2) 0.0323(11) Uani 1 1 d . . . C101 C 0.7264(9) 0.4904(5) 0.6428(2) 0.0364(11) Uani 1 1 d . . . H101 H 0.8567 0.5048 0.6354 0.044 Uiso 1 1 calc R . . C102 C 0.7182(9) 0.4962(5) 0.5977(2) 0.0334(11) Uani 1 1 d . . . H102 H 0.8433 0.5156 0.559 0.04 Uiso 1 1 calc R . . C103 C 0.5278(9) 0.4738(5) 0.6089(2) 0.0305(10) Uani 1 1 d . . . C104 C 0.3459(9) 0.4441(5) 0.6648(2) 0.0315(10) Uani 1 1 d . . . H104 H 0.2175 0.4274 0.6721 0.038 Uiso 1 1 calc R . . C105 C 0.3524(10) 0.4388(5) 0.7101(2) 0.0328(11) Uani 1 1 d . . . H105 H 0.2284 0.4186 0.7486 0.039 Uiso 1 1 calc R . . C106 C 0.5184(9) 0.4826(5) 0.5607(2) 0.0315(10) Uani 1 1 d . . . N1 N 0.2204(6) 0.8592(3) -0.05822(15) 0.0184(7) Uani 1 1 d . . . N2 N -0.2287(6) 0.6427(3) 0.02263(16) 0.0198(7) Uani 1 1 d . . . N11 N -0.0475(7) 0.7771(4) 0.05758(16) 0.0217(7) Uani 1 1 d . . . N21 N -0.0038(6) 0.7513(3) 0.90731(15) 0.0172(7) Uani 1 1 d . . . O101 O 0.6803(7) 0.5150(4) 0.51112(17) 0.0413(9) Uani 1 1 d . . . O102 O 0.3442(6) 0.4579(4) 0.57216(16) 0.0392(9) Uani 1 1 d . . . H10A H 0.3571 0.4659 0.542 0.059 Uiso 1 1 calc R . . S1 S 0.3957(2) 1.02954(11) -0.03983(5) 0.0251(2) Uani 1 1 d . . . S2 S -0.38532(19) 0.45465(11) 0.09268(5) 0.0218(2) Uani 1 1 d . . . Br1 Br 0.54241(11) 0.45973(6) 0.76218(2) 0.04157(16) Uani 1 1 d . . . Ni1 Ni -0.01623(9) 0.75763(5) -0.01971(2) 0.01580(13) Uani 1 1 d . . . C22A C -0.0787(11) 0.8633(5) 0.3507(3) 0.0249(13) Uiso 0.812(8) 1 d PU A 1 H22A H 0.0678 0.8746 0.335 0.03 Uiso 0.812(8) 1 calc PR A 1 C23A C -0.2351(11) 0.8507(6) 0.4095(3) 0.0280(14) Uiso 0.812(8) 1 d PU A 1 H23A H -0.3869 0.8437 0.4271 0.034 Uiso 0.812(8) 1 calc PR A 1 C24A C -0.1848(16) 0.8468(6) 0.4491(4) 0.0276(15) Uiso 0.812(8) 1 d PU A 1 C42A C -0.0975(12) 0.7956(6) 0.6366(3) 0.0267(13) Uiso 0.812(8) 1 d PU A 1 H42A H -0.2432 0.7836 0.6521 0.032 Uiso 0.812(8) 1 calc PR A 1 C43A C 0.0550(11) 0.8173(6) 0.5787(3) 0.0274(14) Uiso 0.812(8) 1 d PU A 1 H43A H 0.2025 0.8285 0.5621 0.033 Uiso 0.812(8) 1 calc PR A 1 C44A C 0.0022(16) 0.8246(6) 0.5393(4) 0.0270(14) Uiso 0.812(8) 1 d PU A 1 O11A O -0.3307(10) 0.8242(6) 0.5014(3) 0.0410(14) Uiso 0.812(8) 1 d PU A 1 O12A O 0.0147(12) 0.8625(5) 0.4251(2) 0.0326(12) Uiso 0.812(8) 1 d PU A 1 H12A H 0.0259 0.8585 0.4512 0.049 Uiso 0.812(8) 1 calc PR A 1 O31A O -0.2024(12) 0.8130(5) 0.5647(2) 0.0373(12) Uiso 0.812(8) 1 d PU A 1 H31A H -0.2163 0.8184 0.5391 0.056 Uiso 0.812(8) 1 calc PR A 1 O32A O 0.1522(11) 0.8447(6) 0.4858(3) 0.0390(17) Uiso 0.812(8) 1 d PU A 1 C22B C -0.215(4) 0.867(2) 0.3740(10) 0.014(5) Uiso 0.188(8) 1 d PU A 2 H22B H -0.3801 0.873 0.4106 0.017 Uiso 0.188(8) 1 calc PR A 2 C23B C -0.043(5) 0.863(2) 0.3740(12) 0.027(6) Uiso 0.188(8) 1 d PU A 2 H23B H 0.1124 0.8672 0.3369 0.032 Uiso 0.188(8) 1 calc PR A 2 C24B C -0.097(5) 0.8513(17) 0.4334(10) 0.002(4) Uiso 0.188(8) 1 d PU A 2 C42B C 0.011(4) 0.807(2) 0.6179(11) 0.017(5) Uiso 0.188(8) 1 d PU A 2 H42B H 0.163 0.8169 0.5823 0.02 Uiso 0.188(8) 1 calc PR A 2 C43B C -0.157(5) 0.807(3) 0.6193(14) 0.039(7) Uiso 0.188(8) 1 d PU A 2 H43B H -0.3086 0.798 0.6554 0.046 Uiso 0.188(8) 1 calc PR A 2 C44B C -0.093(5) 0.8247(19) 0.5582(11) 0.009(4) Uiso 0.188(8) 1 d PU A 2 O11B O 0.103(4) 0.8565(19) 0.4183(9) 0.030(5) Uiso 0.188(8) 1 d PU A 2 O12B O -0.317(4) 0.866(3) 0.4937(12) 0.040(6) Uiso 0.188(8) 1 d PU A 2 H12B H -0.2952 0.8558 0.5175 0.06 Uiso 0.188(8) 1 calc PR A 2 O31B O 0.108(5) 0.828(3) 0.5001(15) 0.039(7) Uiso 0.188(8) 1 d PU A 2 H31B H 0.0765 0.8384 0.4782 0.058 Uiso 0.188(8) 1 calc PR A 2 O32B O -0.299(5) 0.826(2) 0.5734(10) 0.034(5) Uiso 0.188(8) 1 d PU A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0191(19) 0.020(2) 0.0160(19) 0.0040(16) -0.0126(17) -0.0052(16) C2 0.0143(18) 0.019(2) 0.0188(19) 0.0017(16) -0.0127(17) -0.0031(16) C11 0.026(2) 0.071(4) 0.025(2) 0.015(2) -0.020(2) -0.022(3) C12 0.024(2) 0.069(4) 0.023(2) 0.014(2) -0.017(2) -0.020(2) C13 0.031(2) 0.025(2) 0.022(2) 0.0098(18) -0.022(2) -0.0124(19) C14 0.027(2) 0.070(4) 0.027(3) -0.005(2) -0.023(2) 0.004(3) C15 0.026(2) 0.053(3) 0.020(2) -0.006(2) -0.017(2) 0.007(2) C16 0.029(2) 0.025(2) 0.021(2) 0.0076(17) -0.021(2) -0.0084(18) C17 0.032(2) 0.043(3) 0.021(2) 0.011(2) -0.020(2) -0.020(2) C18 0.048(3) 0.029(3) 0.019(2) 0.0114(19) -0.023(2) -0.016(2) C19 0.049(3) 0.029(3) 0.030(2) 0.010(2) -0.034(2) -0.012(2) C20 0.047(3) 0.057(4) 0.040(3) 0.009(3) -0.038(3) -0.015(3) C21 0.037(3) 0.064(4) 0.029(3) 0.012(3) -0.026(2) -0.020(3) C31 0.027(2) 0.022(2) 0.024(2) 0.0102(17) -0.0209(19) -0.0110(18) C32 0.028(2) 0.023(2) 0.022(2) 0.0111(17) -0.0198(19) -0.0119(18) C33 0.0161(18) 0.023(2) 0.0134(18) 0.0005(16) -0.0110(17) -0.0017(16) C34 0.026(2) 0.026(2) 0.020(2) 0.0087(17) -0.0190(19) -0.0139(18) C35 0.026(2) 0.023(2) 0.0168(19) 0.0062(17) -0.0150(18) -0.0111(18) C36 0.025(2) 0.020(2) 0.019(2) 0.0032(16) -0.0170(19) -0.0044(17) C37 0.038(3) 0.033(3) 0.023(2) 0.0118(19) -0.024(2) -0.015(2) C38 0.047(3) 0.028(3) 0.024(2) 0.0104(19) -0.027(2) -0.011(2) C39 0.049(3) 0.025(3) 0.034(3) 0.003(2) -0.035(3) -0.003(2) C40 0.036(3) 0.043(3) 0.026(2) 0.004(2) -0.025(2) -0.010(2) C41 0.026(2) 0.037(3) 0.021(2) 0.0055(19) -0.018(2) -0.010(2) C100 0.040(3) 0.028(3) 0.024(2) 0.0024(19) -0.023(2) -0.004(2) C101 0.031(3) 0.041(3) 0.031(3) 0.003(2) -0.021(2) -0.009(2) C102 0.031(2) 0.038(3) 0.027(2) 0.008(2) -0.020(2) -0.012(2) C103 0.033(2) 0.027(2) 0.026(2) 0.0034(19) -0.021(2) -0.007(2) C104 0.034(2) 0.026(2) 0.025(2) 0.0007(19) -0.019(2) -0.009(2) C105 0.040(3) 0.025(2) 0.023(2) 0.0041(19) -0.019(2) -0.010(2) C106 0.033(3) 0.028(3) 0.029(2) 0.001(2) -0.022(2) -0.005(2) N1 0.0202(17) 0.0184(18) 0.0160(16) 0.0053(13) -0.0129(15) -0.0067(14) N2 0.0191(16) 0.0195(18) 0.0220(18) 0.0062(15) -0.0155(16) -0.0058(14) N11 0.0250(18) 0.030(2) 0.0197(17) 0.0106(15) -0.0178(16) -0.0146(16) N21 0.0212(16) 0.0181(17) 0.0165(16) 0.0039(13) -0.0152(15) -0.0065(14) O101 0.041(2) 0.059(3) 0.0307(19) 0.0175(18) -0.0262(18) -0.0232(19) O102 0.038(2) 0.053(2) 0.0324(19) 0.0108(17) -0.0269(17) -0.0177(18) S1 0.0226(5) 0.0226(6) 0.0319(6) 0.0008(4) -0.0206(5) -0.0075(4) S2 0.0224(5) 0.0200(5) 0.0189(5) 0.0086(4) -0.0130(4) -0.0087(4) Br1 0.0521(3) 0.0373(3) 0.0330(3) 0.0047(2) -0.0331(3) -0.0050(2) Ni1 0.0197(3) 0.0178(3) 0.0158(3) 0.0063(2) -0.0142(2) -0.0087(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.158(5) . ? C1 S1 1.645(4) . ? C2 N2 1.163(5) . ? C2 S2 1.640(4) . ? C11 N11 1.351(6) . ? C11 C12 1.384(6) . ? C11 H11 0.95 . ? C12 C13 1.391(6) . ? C12 H12 0.95 . ? C13 C14 1.369(7) . ? C13 C16 1.491(5) . ? C14 C15 1.384(6) . ? C14 H14 0.95 . ? C15 N11 1.321(6) . ? C15 H15 0.95 . ? C16 C21 1.383(7) . ? C16 C17 1.390(6) . ? C17 C18 1.394(6) . ? C17 H17 0.95 . ? C18 C19 1.400(7) . ? C18 H18 0.95 . ? C19 C20 1.382(7) . ? C19 C22A 1.478(7) . ? C19 C22B 1.54(2) . ? C20 C21 1.374(6) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C31 N21 1.339(5) . ? C31 C32 1.378(5) . ? C31 H31 0.95 . ? C32 C33 1.389(6) . ? C32 H32 0.95 . ? C33 C34 1.402(6) . ? C33 C36 1.483(5) . ? C34 C35 1.387(5) . ? C34 H34 0.95 . ? C35 N21 1.339(5) . ? C35 H35 0.95 . ? C36 C41 1.392(6) . ? C36 C37 1.394(6) . ? C37 C38 1.393(6) . ? C37 H37 0.95 . ? C38 C39 1.391(7) . ? C38 H38 0.95 . ? C39 C40 1.386(7) . ? C39 C42A 1.479(7) . ? C39 C42B 1.52(2) . ? C40 C41 1.382(6) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? C100 C105 1.371(7) . ? C100 C101 1.387(7) . ? C100 Br1 1.901(4) . ? C101 C102 1.390(7) . ? C101 H101 0.95 . ? C102 C103 1.390(7) . ? C102 H102 0.95 . ? C103 C104 1.384(7) . ? C103 C106 1.489(6) . ? C104 C105 1.385(7) . ? C104 H104 0.95 . ? C105 H105 0.95 . ? C106 O101 1.263(6) . ? C106 O102 1.275(6) . ? N1 Ni1 2.039(3) . ? N2 Ni1 2.038(3) . ? N11 Ni1 2.138(3) . ? N21 Ni1 2.104(3) 1_556 ? O102 H10A 0.84 . ? S1 Ni1 2.5143(12) 2_575 ? S2 Ni1 2.5607(12) 2_565 ? Ni1 N21 2.104(3) 1_554 ? Ni1 S1 2.5143(12) 2_575 ? Ni1 S2 2.5607(12) 2_565 ? C22A C23A 1.319(8) . ? C22A H22A 0.95 . ? C23A C24A 1.476(8) . ? C23A H23A 0.95 . ? C24A O11A 1.230(10) . ? C24A O12A 1.273(8) . ? C42A C43A 1.339(8) . ? C42A H42A 0.95 . ? C43A C44A 1.485(8) . ? C43A H43A 0.95 . ? C44A O32A 1.244(10) . ? C44A O31A 1.278(8) . ? O12A H12A 0.84 . ? O31A H31A 0.84 . ? C22B C23B 1.34(3) . ? C22B H22B 0.95 . ? C23B C24B 1.52(3) . ? C23B H23B 0.95 . ? C24B O11B 1.33(3) . ? C24B O12B 1.36(3) . ? C42B C43B 1.30(4) . ? C42B H42B 0.95 . ? C43B C44B 1.55(3) . ? C43B H43B 0.95 . ? C44B O31B 1.33(3) . ? C44B O32B 1.35(3) . ? O12B H12B 0.84 . ? O31B H31B 0.84 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 S1 179.1(4) . . ? N2 C2 S2 179.6(4) . . ? N11 C11 C12 123.8(4) . . ? N11 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C13 119.7(5) . . ? C11 C12 H12 120.1 . . ? C13 C12 H12 120.1 . . ? C14 C13 C12 115.9(4) . . ? C14 C13 C16 121.8(4) . . ? C12 C13 C16 122.2(4) . . ? C13 C14 C15 121.0(4) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? N11 C15 C14 123.8(4) . . ? N11 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? C21 C16 C17 118.4(4) . . ? C21 C16 C13 119.7(4) . . ? C17 C16 C13 121.9(4) . . ? C16 C17 C18 120.7(4) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 118.2(4) . . ? C20 C19 C22A 114.4(5) . . ? C18 C19 C22A 127.5(5) . . ? C20 C19 C22B 143.6(9) . . ? C18 C19 C22B 98.0(9) . . ? C22A C19 C22B 29.5(7) . . ? C21 C20 C19 121.4(5) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C16 121.1(5) . . ? C20 C21 H21 119.4 . . ? C16 C21 H21 119.4 . . ? N21 C31 C32 123.7(4) . . ? N21 C31 H31 118.1 . . ? C32 C31 H31 118.1 . . ? C31 C32 C33 120.2(4) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C32 C33 C34 116.3(3) . . ? C32 C33 C36 122.0(4) . . ? C34 C33 C36 121.7(4) . . ? C35 C34 C33 119.7(4) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? N21 C35 C34 123.5(4) . . ? N21 C35 H35 118.2 . . ? C34 C35 H35 118.2 . . ? C41 C36 C37 118.2(4) . . ? C41 C36 C33 120.8(4) . . ? C37 C36 C33 121.0(4) . . ? C38 C37 C36 120.6(4) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 120.8(4) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C40 C39 C38 118.2(4) . . ? C40 C39 C42A 114.5(5) . . ? C38 C39 C42A 127.3(5) . . ? C40 C39 C42B 140.7(10) . . ? C38 C39 C42B 101.0(10) . . ? C42A C39 C42B 26.2(8) . . ? C41 C40 C39 121.3(5) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C40 C41 C36 120.8(4) . . ? C40 C41 H41 119.6 . . ? C36 C41 H41 119.6 . . ? C105 C100 C101 122.1(4) . . ? C105 C100 Br1 119.3(4) . . ? C101 C100 Br1 118.6(4) . . ? C100 C101 C102 118.1(5) . . ? C100 C101 H101 121 . . ? C102 C101 H101 121 . . ? C103 C102 C101 120.3(4) . . ? C103 C102 H102 119.8 . . ? C101 C102 H102 119.8 . . ? C104 C103 C102 120.3(4) . . ? C104 C103 C106 119.8(4) . . ? C102 C103 C106 119.9(4) . . ? C103 C104 C105 119.6(5) . . ? C103 C104 H104 120.2 . . ? C105 C104 H104 120.2 . . ? C100 C105 C104 119.5(4) . . ? C100 C105 H105 120.2 . . ? C104 C105 H105 120.2 . . ? O101 C106 O102 123.4(4) . . ? O101 C106 C103 118.9(4) . . ? O102 C106 C103 117.7(4) . . ? C1 N1 Ni1 148.7(3) . . ? C2 N2 Ni1 152.8(3) . . ? C15 N11 C11 115.6(4) . . ? C15 N11 Ni1 122.0(3) . . ? C11 N11 Ni1 122.1(3) . . ? C35 N21 C31 116.6(3) . . ? C35 N21 Ni1 122.6(3) . 1_556 ? C31 N21 Ni1 120.5(3) . 1_556 ? C106 O102 H10A 109.5 . . ? C1 S1 Ni1 96.84(15) . 2_575 ? C2 S2 Ni1 102.61(14) . 2_565 ? N2 Ni1 N1 171.75(13) . . ? N2 Ni1 N21 93.85(13) . 1_554 ? N1 Ni1 N21 92.93(13) . 1_554 ? N2 Ni1 N11 86.89(13) . . ? N1 Ni1 N11 86.65(13) . . ? N21 Ni1 N11 176.23(14) 1_554 . ? N2 Ni1 S1 92.44(10) . 2_575 ? N1 Ni1 S1 92.85(10) . 2_575 ? N21 Ni1 S1 84.77(10) 1_554 2_575 ? N11 Ni1 S1 91.50(10) . 2_575 ? N2 Ni1 S2 90.48(10) . 2_565 ? N1 Ni1 S2 84.97(10) . 2_565 ? N21 Ni1 S2 88.80(10) 1_554 2_565 ? N11 Ni1 S2 94.89(10) . 2_565 ? S1 Ni1 S2 173.11(4) 2_575 2_565 ? C23A C22A C19 126.1(6) . . ? C23A C22A H22A 116.9 . . ? C19 C22A H22A 116.9 . . ? C22A C23A C24A 122.9(6) . . ? C22A C23A H23A 118.6 . . ? C24A C23A H23A 118.6 . . ? O11A C24A O12A 124.2(6) . . ? O11A C24A C23A 118.8(7) . . ? O12A C24A C23A 117.0(7) . . ? C43A C42A C39 124.8(6) . . ? C43A C42A H42A 117.6 . . ? C39 C42A H42A 117.6 . . ? C42A C43A C44A 122.5(6) . . ? C42A C43A H43A 118.8 . . ? C44A C43A H43A 118.8 . . ? O32A C44A O31A 124.6(6) . . ? O32A C44A C43A 119.2(6) . . ? O31A C44A C43A 116.2(7) . . ? C24A O12A H12A 109.5 . . ? C44A O31A H31A 109.5 . . ? C23B C22B C19 111.4(18) . . ? C23B C22B H22B 124.3 . . ? C19 C22B H22B 124.3 . . ? C22B C23B C24B 120(2) . . ? C22B C23B H23B 119.9 . . ? C24B C23B H23B 119.9 . . ? O11B C24B O12B 124.6(19) . . ? O11B C24B C23B 104.5(19) . . ? O12B C24B C23B 129(2) . . ? C43B C42B C39 114(2) . . ? C43B C42B H42B 123 . . ? C39 C42B H42B 123 . . ? C42B C43B C44B 115(3) . . ? C42B C43B H43B 122.3 . . ? C44B C43B H43B 122.3 . . ? O31B C44B O32B 122(2) . . ? O31B C44B C43B 135(3) . . ? O32B C44B C43B 103(2) . . ? C24B O12B H12B 109.5 . . ? C44B O31B H31B 109.5 . . ? #===END # Attachment '5397_web_deposit_cif_file_2_RyoSekiya_1305266004.cif' data_dibromobiphenyl _database_code_depnum_ccdc_archive 'CCDC 759630' #TrackingRef '5397_web_deposit_cif_file_2_RyoSekiya_1305266004.cif' _audit_creation_date 2009-11-11T14:08:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H22 N4 Ni O4 S2, C12 H8 Br2' _chemical_formula_sum 'C42 H30 Br2 N4 Ni O4 S2' _chemical_formula_weight 937.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.268(2) _cell_length_b 11.0835(7) _cell_length_c 28.807(4) _cell_angle_alpha 87.171(12) _cell_angle_beta 35.532(7) _cell_angle_gamma 84.060(10) _cell_volume 1891.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_theta_min 1.22 _cell_measurement_theta_max 29.96 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 2.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_absorpt_correction_T_min 0.5312 _exptl_absorpt_correction_T_max 0.8733 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 153(2) _diffrn_radiation_probe X-ray _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_unetI/netI 0.0497 _diffrn_reflns_number 21211 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 29.96 _diffrn_reflns_theta_full 29.96 _diffrn_measured_fraction_theta_full 0.969 _diffrn_measured_fraction_theta_max 0.969 _reflns_number_total 10659 _reflns_number_gt 7627 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection RAPID-AUTO _computing_cell_refinement RAPID-AUTO _computing_data_reduction RAPID-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0631P)^2^+1.7699P] 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_number_reflns 10659 _refine_ls_number_parameters 499 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.124 _refine_ls_wR_factor_gt 0.1048 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.041 _refine_diff_density_min -1.046 _refine_diff_density_rms 0.142 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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' 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 Br2 Br -1.14584(7) 0.58130(4) 0.66126(2) 0.03980(11) Uani 1 1 d . . . Ni2 Ni 0 0.5 0 0.01307(11) Uani 1 2 d S . . Ni1 Ni 0 0 0 0.01270(11) Uani 1 2 d S . . Br1 Br 0.35651(6) 0.22562(4) 0.04360(2) 0.03378(10) Uani 1 1 d . . . S1 S -0.36464(12) 0.40330(7) 0.12141(4) 0.02012(15) Uani 1 1 d . . . S2 S 0.35363(12) 0.09533(6) -0.08355(4) 0.01810(15) Uani 1 1 d . . . C41 C 0.2089(5) 0.2900(3) 0.70790(17) 0.0182(6) Uani 1 1 d . . . H41 H 0.3468 0.2867 0.6846 0.022 Uiso 1 1 calc R . . C33 C 0.0046(5) 0.3621(3) 0.83836(17) 0.0156(5) Uani 1 1 d . . . C1 C -0.2683(5) 0.2618(3) 0.08195(17) 0.0152(5) Uani 1 1 d . . . N21 N 0.0051(4) 0.4373(2) 0.93069(14) 0.0149(4) Uani 1 1 d . . . N2 N 0.1901(4) 0.3427(2) -0.03367(15) 0.0169(5) Uani 1 1 d . . . O31 O 0.0836(4) 0.1741(3) 0.53142(14) 0.0303(5) Uani 1 1 d . . . H231 H 0.082 0.1576 0.5038 0.045 Uiso 1 1 calc R . . O12 O -0.2459(4) 0.1406(2) 0.52814(14) 0.0292(5) Uani 1 1 d . . . H212 H -0.2451 0.1523 0.5565 0.044 Uiso 1 1 calc R . . N11 N -0.0715(4) -0.0175(2) 0.09214(15) 0.0172(5) Uani 1 1 d . . . C36 C 0.0075(5) 0.3255(3) 0.78842(17) 0.0154(5) Uani 1 1 d . . . O11 O 0.1278(4) 0.1251(3) 0.43087(15) 0.0334(6) Uani 1 1 d . . . N1 N -0.1990(4) 0.1635(2) 0.05408(15) 0.0169(5) Uani 1 1 d . . . C2 C 0.2563(5) 0.2403(3) -0.05357(17) 0.0151(5) Uani 1 1 d . . . C19 C -0.1610(5) 0.0735(3) 0.36027(18) 0.0193(6) Uani 1 1 d . . . C23 C -0.0084(6) 0.1023(3) 0.39511(19) 0.0241(6) Uani 1 1 d . . . H23 H 0.1414 0.0908 0.3403 0.029 Uiso 1 1 calc R . . C40 C 0.2121(5) 0.2591(3) 0.66083(18) 0.0210(6) Uani 1 1 d . . . H40 H 0.3521 0.235 0.6059 0.025 Uiso 1 1 calc R . . C43 C -0.1520(5) 0.2242(3) 0.66333(19) 0.0233(6) Uani 1 1 d . . . H43 H -0.301 0.2408 0.718 0.028 Uiso 1 1 calc R . . C42 C 0.0224(5) 0.2295(3) 0.64147(18) 0.0188(6) Uani 1 1 d . . . H42 H 0.1685 0.2093 0.5867 0.023 Uiso 1 1 calc R . . C38 C -0.1914(5) 0.2986(3) 0.77439(18) 0.0210(6) Uani 1 1 d . . . H38 H -0.3294 0.3022 0.7977 0.025 Uiso 1 1 calc R . . C12 C 0.0724(5) -0.0541(3) 0.12791(18) 0.0193(6) Uani 1 1 d . . . H12 H 0.1929 -0.0877 0.1128 0.023 Uiso 1 1 calc R . . C44 C -0.1192(5) 0.1934(3) 0.60496(19) 0.0219(6) Uani 1 1 d . . . C11 C 0.0927(5) -0.0621(3) 0.07447(18) 0.0197(6) Uani 1 1 d . . . H11 H 0.2288 -0.1008 0.023 0.024 Uiso 1 1 calc R . . C13 C -0.1221(5) 0.0026(3) 0.20331(17) 0.0166(5) Uani 1 1 d . . . C15 C -0.2655(5) 0.0309(3) 0.16649(18) 0.0203(6) Uani 1 1 d . . . H15 H -0.3864 0.0587 0.1809 0.024 Uiso 1 1 calc R . . C16 C -0.1398(5) 0.0253(3) 0.25881(17) 0.0175(6) Uani 1 1 d . . . C22 C -0.1795(5) 0.0980(3) 0.41501(19) 0.0213(6) Uani 1 1 d . . . H22 H -0.3275 0.1121 0.4701 0.026 Uiso 1 1 calc R . . O32 O -0.2888(4) 0.1895(3) 0.62868(15) 0.0347(6) Uani 1 1 d . . . C17 C 0.0569(5) 0.0225(3) 0.22893(18) 0.0208(6) Uani 1 1 d . . . H17 H 0.2001 0.0042 0.1735 0.025 Uiso 1 1 calc R . . C37 C -0.1935(5) 0.3285(3) 0.82092(17) 0.0192(6) Uani 1 1 d . . . H37 H -0.3336 0.3517 0.876 0.023 Uiso 1 1 calc R . . C14 C -0.2992(5) 0.0428(3) 0.22353(18) 0.0207(6) Uani 1 1 d . . . H14 H -0.4402 0.0776 0.2756 0.025 Uiso 1 1 calc R . . C39 C 0.0118(5) 0.2631(3) 0.69317(17) 0.0170(5) Uani 1 1 d . . . C24 C -0.0429(5) 0.1242(3) 0.45460(19) 0.0236(6) Uani 1 1 d . . . C31 C -0.1760(5) 0.4633(3) 0.95492(18) 0.0198(6) Uani 1 1 d . . . H31 H -0.3064 0.5082 1.0046 0.024 Uiso 1 1 calc R . . C18 C 0.0450(5) 0.0460(3) 0.27888(19) 0.0228(6) Uani 1 1 d . . . H18 H 0.1801 0.0433 0.2573 0.027 Uiso 1 1 calc R . . C100 C 0.0975(6) 0.2958(3) 0.1497(2) 0.0258(7) Uani 1 1 d . . . C32 C -0.1816(5) 0.4281(3) 0.91118(18) 0.0183(6) Uani 1 1 d . . . H32 H -0.3136 0.4492 0.9311 0.022 Uiso 1 1 calc R . . C105 C -0.1065(6) 0.3152(3) 0.1850(2) 0.0284(7) Uani 1 1 d . . . H105 H -0.1158 0.2955 0.1561 0.034 Uiso 1 1 calc R . . C20 C -0.3575(5) 0.0759(3) 0.39042(19) 0.0232(6) Uani 1 1 d . . . H20 H -0.5003 0.0937 0.446 0.028 Uiso 1 1 calc R . . C21 C -0.3470(5) 0.0524(3) 0.34027(18) 0.0219(6) Uani 1 1 d . . . H21 H -0.4822 0.055 0.3619 0.026 Uiso 1 1 calc R . . C106 C -0.4902(6) 0.4420(3) 0.3913(2) 0.0275(7) Uani 1 1 d . . . C35 C 0.1846(5) 0.3728(3) 0.86040(18) 0.0211(6) Uani 1 1 d . . . H35 H 0.3149 0.3537 0.8416 0.025 Uiso 1 1 calc R . . C108 C -0.7070(6) 0.4558(3) 0.5250(2) 0.0332(8) Uani 1 1 d . . . H108 H -0.722 0.4348 0.5615 0.04 Uiso 1 1 calc R . . C34 C 0.1919(5) 0.3323(3) 0.81358(18) 0.0222(6) Uani 1 1 d . . . H34 H 0.3223 0.2848 0.7651 0.027 Uiso 1 1 calc R . . C102 C -0.0754(6) 0.3749(3) 0.2683(2) 0.0294(7) Uani 1 1 d . . . H102 H -0.064 0.3957 0.2965 0.035 Uiso 1 1 calc R . . C101 C 0.1157(6) 0.3269(3) 0.1902(2) 0.0297(7) Uani 1 1 d . . . H101 H 0.2574 0.3155 0.1646 0.036 Uiso 1 1 calc R . . C103 C -0.2856(6) 0.3933(3) 0.3068(2) 0.0257(7) Uani 1 1 d . . . C111 C -0.6622(6) 0.5184(3) 0.4186(2) 0.0305(7) Uani 1 1 d . . . H111 H -0.6467 0.5411 0.3822 0.037 Uiso 1 1 calc R . . C109 C -0.8763(6) 0.5299(4) 0.5506(2) 0.0323(8) Uani 1 1 d . . . C104 C -0.2963(6) 0.3640(3) 0.2632(2) 0.0277(7) Uani 1 1 d . . . H104 H -0.4364 0.3777 0.2878 0.033 Uiso 1 1 calc R . . C107 C -0.5155(6) 0.4126(3) 0.4456(2) 0.0307(7) Uani 1 1 d . . . H107 H -0.3991 0.3619 0.4279 0.037 Uiso 1 1 calc R . . C110 C -0.8564(6) 0.5620(3) 0.4985(2) 0.0324(8) Uani 1 1 d . . . H110 H -0.9731 0.6132 0.5166 0.039 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 Br2 0.0343(2) 0.0417(2) 0.0332(2) -0.00304(16) -0.02525(18) -0.00306(16) Ni2 0.0152(2) 0.0117(2) 0.0153(2) -0.00274(18) -0.0131(2) 0.00131(18) Ni1 0.0149(2) 0.0117(2) 0.0144(2) -0.00176(17) -0.0126(2) 0.00078(18) Br1 0.03052(19) 0.0347(2) 0.03024(18) 0.00051(14) -0.02371(17) -0.00040(14) S1 0.0178(3) 0.0146(3) 0.0182(3) -0.0040(3) -0.0127(3) 0.0010(3) S2 0.0151(3) 0.0135(3) 0.0217(3) -0.0031(3) -0.0142(3) 0.0015(2) C41 0.0160(13) 0.0249(15) 0.0169(13) -0.0016(11) -0.0142(12) 0.0005(11) C33 0.0180(13) 0.0153(13) 0.0167(13) -0.0001(10) -0.0148(12) -0.0018(10) C1 0.0141(12) 0.0166(13) 0.0151(12) 0.0020(10) -0.0119(11) -0.0028(10) N21 0.0153(11) 0.0154(11) 0.0148(11) -0.0009(9) -0.0125(10) -0.0008(9) N2 0.0173(11) 0.0156(12) 0.0196(12) -0.0015(9) -0.0155(11) 0.0005(9) O31 0.0256(12) 0.0501(16) 0.0202(11) -0.0065(10) -0.0199(11) 0.0033(11) O12 0.0256(12) 0.0470(15) 0.0204(11) -0.0048(10) -0.0198(11) -0.0010(11) N11 0.0198(12) 0.0176(12) 0.0180(12) -0.0003(9) -0.0162(11) -0.0009(9) C36 0.0188(13) 0.0155(13) 0.0170(13) -0.0012(10) -0.0156(12) -0.0014(10) O11 0.0251(12) 0.0570(18) 0.0266(12) -0.0081(11) -0.0230(11) 0.0037(11) N1 0.0170(11) 0.0169(12) 0.0175(11) -0.0003(9) -0.0141(10) -0.0020(9) C2 0.0145(12) 0.0177(13) 0.0167(13) -0.0007(10) -0.0134(12) -0.0010(10) C19 0.0216(14) 0.0229(15) 0.0191(14) -0.0020(11) -0.0180(13) 0.0018(11) C23 0.0259(16) 0.0325(18) 0.0195(14) -0.0013(12) -0.0197(14) -0.0011(13) C40 0.0181(14) 0.0303(16) 0.0162(13) -0.0030(12) -0.0144(13) 0.0008(12) C43 0.0204(14) 0.0352(18) 0.0164(14) -0.0055(12) -0.0155(13) 0.0018(12) C42 0.0195(14) 0.0218(15) 0.0165(13) -0.0005(11) -0.0148(12) -0.0019(11) C38 0.0188(14) 0.0284(16) 0.0192(14) -0.0005(12) -0.0161(13) -0.0026(12) C12 0.0244(15) 0.0203(14) 0.0223(14) -0.0020(11) -0.0211(14) 0.0024(11) C44 0.0224(15) 0.0279(16) 0.0215(14) -0.0041(12) -0.0193(13) 0.0018(12) C11 0.0193(14) 0.0205(14) 0.0200(14) -0.0030(11) -0.0164(13) 0.0025(11) C13 0.0177(13) 0.0198(14) 0.0152(13) 0.0001(10) -0.0139(12) -0.0019(11) C15 0.0183(14) 0.0267(16) 0.0199(14) -0.0006(12) -0.0165(13) 0.0000(11) C16 0.0203(14) 0.0194(14) 0.0195(14) -0.0007(11) -0.0177(13) 0.0002(11) C22 0.0250(15) 0.0246(15) 0.0209(14) -0.0037(12) -0.0201(14) 0.0016(12) O32 0.0240(12) 0.0611(18) 0.0256(12) -0.0135(12) -0.0219(11) 0.0069(11) C17 0.0166(13) 0.0286(16) 0.0169(14) -0.0018(11) -0.0137(12) 0.0017(11) C37 0.0141(13) 0.0300(16) 0.0124(12) -0.0034(11) -0.0105(12) -0.0005(11) C14 0.0165(13) 0.0297(16) 0.0166(13) -0.0024(11) -0.0137(12) 0.0001(12) C39 0.0186(13) 0.0188(14) 0.0167(13) -0.0004(10) -0.0149(12) -0.0019(11) C24 0.0258(15) 0.0290(17) 0.0223(15) -0.0036(12) -0.0210(14) 0.0016(13) C31 0.0184(14) 0.0223(15) 0.0200(14) -0.0070(11) -0.0160(13) 0.0037(11) C18 0.0199(14) 0.0333(17) 0.0211(15) -0.0011(12) -0.0180(13) 0.0001(12) C100 0.0296(17) 0.0218(16) 0.0295(17) 0.0071(13) -0.0247(15) -0.0065(13) C32 0.0170(13) 0.0213(14) 0.0206(14) -0.0020(11) -0.0161(12) -0.0003(11) C105 0.0300(17) 0.0307(18) 0.0302(17) 0.0085(14) -0.0254(16) -0.0102(14) C20 0.0192(14) 0.0332(17) 0.0179(14) -0.0032(12) -0.0152(13) 0.0001(12) C21 0.0175(14) 0.0305(17) 0.0191(14) -0.0038(12) -0.0153(13) 0.0007(12) C106 0.0267(16) 0.0240(16) 0.0326(18) 0.0050(13) -0.0241(16) -0.0076(13) C35 0.0176(13) 0.0277(16) 0.0208(14) -0.0090(12) -0.0164(13) 0.0054(12) C108 0.0358(19) 0.0310(19) 0.0344(19) 0.0076(15) -0.0286(18) -0.0101(15) C34 0.0201(14) 0.0304(17) 0.0194(14) -0.0072(12) -0.0169(13) 0.0039(12) C102 0.0316(18) 0.0314(18) 0.0343(18) 0.0062(14) -0.0286(17) -0.0073(14) C101 0.0263(17) 0.0312(18) 0.0339(18) 0.0061(14) -0.0250(16) -0.0054(14) C103 0.0284(16) 0.0191(15) 0.0312(17) 0.0060(13) -0.0244(15) -0.0069(12) C111 0.0316(18) 0.0294(18) 0.0322(18) 0.0045(14) -0.0263(17) -0.0053(14) C109 0.0277(17) 0.035(2) 0.0290(17) 0.0014(14) -0.0216(16) -0.0077(15) C104 0.0257(16) 0.0295(18) 0.0338(18) 0.0049(14) -0.0254(16) -0.0050(13) C107 0.0300(18) 0.0304(18) 0.0305(18) 0.0068(14) -0.0243(16) -0.0074(14) C110 0.0297(18) 0.0301(19) 0.0366(19) 0.0006(15) -0.0268(17) -0.0028(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Br2 C109 1.908(4) . ? Ni2 N2 2.042(2) 2_565 ? Ni2 N2 2.042(2) . ? Ni2 N21 2.105(2) 1_554 ? Ni2 N21 2.105(2) 2_566 ? Ni2 S1 2.5587(10) 2_565 ? Ni2 S1 2.5587(10) . ? Ni1 N1 2.053(2) 2 ? Ni1 N1 2.053(2) . ? Ni1 N11 2.105(2) 2 ? Ni1 N11 2.105(2) . ? Ni1 S2 2.5325(10) . ? Ni1 S2 2.5325(10) 2 ? Br1 C100 1.897(4) . ? S1 C1 1.659(3) . ? S2 C2 1.651(3) . ? C41 C36 1.388(4) . ? C41 C40 1.389(4) . ? C41 H41 0.95 . ? C33 C32 1.388(4) . ? C33 C34 1.406(4) . ? C33 C36 1.490(4) . ? C1 N1 1.156(4) . ? N21 C35 1.343(4) . ? N21 C31 1.351(4) . ? N21 Ni2 2.105(2) 1_556 ? N2 C2 1.162(4) . ? O31 C44 1.282(4) . ? O31 H231 0.84 . ? O12 C24 1.280(4) . ? O12 H212 0.84 . ? N11 C15 1.338(4) . ? N11 C11 1.342(4) . ? C36 C37 1.408(4) . ? O11 C24 1.263(4) . ? C19 C18 1.389(4) . ? C19 C20 1.402(4) . ? C19 C22 1.463(4) . ? C23 C22 1.339(4) . ? C23 C24 1.468(4) . ? C23 H23 0.95 . ? C40 C39 1.403(4) . ? C40 H40 0.95 . ? C43 C42 1.338(4) . ? C43 C44 1.473(4) . ? C43 H43 0.95 . ? C42 C39 1.467(4) . ? C42 H42 0.95 . ? C38 C37 1.379(4) . ? C38 C39 1.399(4) . ? C38 H38 0.95 . ? C12 C11 1.382(4) . ? C12 C13 1.384(4) . ? C12 H12 0.95 . ? C44 O32 1.256(4) . ? C11 H11 0.95 . ? C13 C14 1.407(4) . ? C13 C16 1.486(4) . ? C15 C14 1.387(4) . ? C15 H15 0.95 . ? C16 C21 1.391(4) . ? C16 C17 1.408(4) . ? C22 H22 0.95 . ? C17 C18 1.377(4) . ? C17 H17 0.95 . ? C37 H37 0.95 . ? C14 H14 0.95 . ? C31 C32 1.384(4) . ? C31 H31 0.95 . ? C18 H18 0.95 . ? C100 C101 1.386(5) . ? C100 C105 1.389(5) . ? C32 H32 0.95 . ? C105 C104 1.386(5) . ? C105 H105 0.95 . ? C20 C21 1.394(4) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C106 C107 1.388(5) . ? C106 C111 1.396(5) . ? C106 C103 1.483(5) . ? C35 C34 1.383(4) . ? C35 H35 0.95 . ? C108 C109 1.386(5) . ? C108 C107 1.386(5) . ? C108 H108 0.95 . ? C34 H34 0.95 . ? C102 C101 1.383(5) . ? C102 C103 1.402(5) . ? C102 H102 0.95 . ? C101 H101 0.95 . ? C103 C104 1.402(5) . ? C111 C110 1.396(5) . ? C111 H111 0.95 . ? C109 C110 1.371(5) . ? C104 H104 0.95 . ? C107 H107 0.95 . ? C110 H110 0.95 . ? 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 Ni2 N2 180 2_565 . ? N2 Ni2 N21 91.23(10) 2_565 1_554 ? N2 Ni2 N21 88.77(10) . 1_554 ? N2 Ni2 N21 88.77(10) 2_565 2_566 ? N2 Ni2 N21 91.23(10) . 2_566 ? N21 Ni2 N21 180.00(7) 1_554 2_566 ? N2 Ni2 S1 91.23(7) 2_565 2_565 ? N2 Ni2 S1 88.77(7) . 2_565 ? N21 Ni2 S1 90.50(7) 1_554 2_565 ? N21 Ni2 S1 89.50(7) 2_566 2_565 ? N2 Ni2 S1 88.77(7) 2_565 . ? N2 Ni2 S1 91.23(7) . . ? N21 Ni2 S1 89.50(7) 1_554 . ? N21 Ni2 S1 90.50(7) 2_566 . ? S1 Ni2 S1 180.00(3) 2_565 . ? N1 Ni1 N1 180.00(14) 2 . ? N1 Ni1 N11 89.14(10) 2 2 ? N1 Ni1 N11 90.86(10) . 2 ? N1 Ni1 N11 90.86(10) 2 . ? N1 Ni1 N11 89.14(10) . . ? N11 Ni1 N11 180.00(13) 2 . ? N1 Ni1 S2 86.40(7) 2 . ? N1 Ni1 S2 93.60(7) . . ? N11 Ni1 S2 90.32(7) 2 . ? N11 Ni1 S2 89.68(7) . . ? N1 Ni1 S2 93.60(7) 2 2 ? N1 Ni1 S2 86.40(7) . 2 ? N11 Ni1 S2 89.68(7) 2 2 ? N11 Ni1 S2 90.32(7) . 2 ? S2 Ni1 S2 180.00(4) . 2 ? C1 S1 Ni2 97.68(10) . . ? C2 S2 Ni1 101.71(10) . . ? C36 C41 C40 121.1(3) . . ? C36 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C32 C33 C34 116.5(3) . . ? C32 C33 C36 122.0(3) . . ? C34 C33 C36 121.5(3) . . ? N1 C1 S1 179.3(2) . . ? C35 N21 C31 116.0(2) . . ? C35 N21 Ni2 123.46(19) . 1_556 ? C31 N21 Ni2 120.49(19) . 1_556 ? C2 N2 Ni2 155.9(2) . . ? C44 O31 H231 109.5 . . ? C24 O12 H212 109.5 . . ? C15 N11 C11 117.2(3) . . ? C15 N11 Ni1 122.4(2) . . ? C11 N11 Ni1 119.6(2) . . ? C41 C36 C37 117.8(3) . . ? C41 C36 C33 121.1(2) . . ? C37 C36 C33 121.1(3) . . ? C1 N1 Ni1 160.3(2) . . ? N2 C2 S2 178.9(3) . . ? C18 C19 C20 118.0(3) . . ? C18 C19 C22 122.6(3) . . ? C20 C19 C22 119.4(3) . . ? C22 C23 C24 122.7(3) . . ? C22 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C41 C40 C39 121.0(3) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C42 C43 C44 121.7(3) . . ? C42 C43 H43 119.1 . . ? C44 C43 H43 119.1 . . ? C43 C42 C39 126.8(3) . . ? C43 C42 H42 116.6 . . ? C39 C42 H42 116.6 . . ? C37 C38 C39 120.7(3) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C11 C12 C13 120.5(3) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? O32 C44 O31 123.1(3) . . ? O32 C44 C43 119.2(3) . . ? O31 C44 C43 117.7(3) . . ? N11 C11 C12 122.9(3) . . ? N11 C11 H11 118.6 . . ? C12 C11 H11 118.6 . . ? C12 C13 C14 116.6(3) . . ? C12 C13 C16 121.9(3) . . ? C14 C13 C16 121.5(3) . . ? N11 C15 C14 123.5(3) . . ? N11 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C21 C16 C17 118.2(3) . . ? C21 C16 C13 121.8(3) . . ? C17 C16 C13 119.9(3) . . ? C23 C22 C19 126.4(3) . . ? C23 C22 H22 116.8 . . ? C19 C22 H22 116.8 . . ? C18 C17 C16 121.0(3) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C38 C37 C36 121.4(3) . . ? C38 C37 H37 119.3 . . ? C36 C37 H37 119.3 . . ? C15 C14 C13 119.2(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C38 C39 C40 118.0(3) . . ? C38 C39 C42 122.7(3) . . ? C40 C39 C42 119.3(3) . . ? O11 C24 O12 123.5(3) . . ? O11 C24 C23 118.6(3) . . ? O12 C24 C23 117.8(3) . . ? N21 C31 C32 123.5(3) . . ? N21 C31 H31 118.3 . . ? C32 C31 H31 118.3 . . ? C17 C18 C19 121.3(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C101 C100 C105 121.4(3) . . ? C101 C100 Br1 119.5(3) . . ? C105 C100 Br1 119.1(3) . . ? C31 C32 C33 120.4(3) . . ? C31 C32 H32 119.8 . . ? C33 C32 H32 119.8 . . ? C104 C105 C100 118.8(3) . . ? C104 C105 H105 120.6 . . ? C100 C105 H105 120.6 . . ? C21 C20 C19 121.1(3) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C16 C21 C20 120.4(3) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C107 C106 C111 118.0(3) . . ? C107 C106 C103 120.5(3) . . ? C111 C106 C103 121.4(3) . . ? N21 C35 C34 124.2(3) . . ? N21 C35 H35 117.9 . . ? C34 C35 H35 117.9 . . ? C109 C108 C107 119.2(4) . . ? C109 C108 H108 120.4 . . ? C107 C108 H108 120.4 . . ? C35 C34 C33 119.4(3) . . ? C35 C34 H34 120.3 . . ? C33 C34 H34 120.3 . . ? C101 C102 C103 121.2(3) . . ? C101 C102 H102 119.4 . . ? C103 C102 H102 119.4 . . ? C102 C101 C100 119.1(3) . . ? C102 C101 H101 120.5 . . ? C100 C101 H101 120.5 . . ? C104 C103 C102 118.1(3) . . ? C104 C103 C106 121.2(3) . . ? C102 C103 C106 120.7(3) . . ? C106 C111 C110 121.2(4) . . ? C106 C111 H111 119.4 . . ? C110 C111 H111 119.4 . . ? C110 C109 C108 121.2(3) . . ? C110 C109 Br2 120.1(3) . . ? C108 C109 Br2 118.7(3) . . ? C105 C104 C103 121.3(3) . . ? C105 C104 H104 119.3 . . ? C103 C104 H104 119.3 . . ? C108 C107 C106 121.3(4) . . ? C108 C107 H107 119.3 . . ? C106 C107 H107 119.3 . . ? C109 C110 C111 119.0(3) . . ? C109 C110 H110 120.5 . . ? C111 C110 H110 120.5 . . ? #===END # Attachment '5398_web_deposit_cif_file_3_RyoSekiya_1305266004.cif' data_guestfree _database_code_depnum_ccdc_archive 'CCDC 759631' #TrackingRef '5398_web_deposit_cif_file_3_RyoSekiya_1305266004.cif' _audit_creation_date 2009-11-11T13:00:26-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H22 N4 Ni O4 S2' _chemical_formula_sum 'C30 H22 N4 Ni O4 S2' _chemical_formula_weight 625.35 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0241(18) _cell_length_b 11.139(2) _cell_length_c 29.368(5) _cell_angle_alpha 73.49(2) _cell_angle_beta 32.633(9) _cell_angle_gamma 62.65(3) _cell_volume 1381.1(5) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 29.97 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_absorpt_correction_T_min 0.7682 _exptl_absorpt_correction_T_max 0.9156 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 153(2) _diffrn_radiation_probe X-ray _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'RIGAKU RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_unetI/netI 0.0363 _diffrn_reflns_number 16580 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 29.97 _diffrn_reflns_theta_full 29.97 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 7952 _reflns_number_gt 5342 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection RAPID-AUTO _computing_cell_refinement RAPID-AUTO _computing_data_reduction RAPID-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 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^)+(0.0560P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7952 _refine_ls_number_parameters 373 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0656 _refine_ls_R_factor_gt 0.0382 _refine_ls_wR_factor_ref 0.1006 _refine_ls_wR_factor_gt 0.0918 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.396 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.073 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C2 C 0.3419(4) 0.17691(17) -0.06623(11) 0.0166(3) Uani 1 1 d . . . C1 C -0.3609(4) 0.32006(17) 0.07757(11) 0.0167(3) Uani 1 1 d . . . C11 C -0.3350(4) 0.0443(2) 0.17248(12) 0.0273(4) Uani 1 1 d . . . H11 H -0.4953 0.1117 0.1895 0.033 Uiso 1 1 calc R . . C12 C -0.3781(4) 0.0361(2) 0.23075(12) 0.0266(4) Uani 1 1 d . . . H12 H -0.5637 0.0973 0.2859 0.032 Uiso 1 1 calc R . . C13 C -0.1494(4) -0.06192(18) 0.20873(11) 0.0184(3) Uani 1 1 d . . . C14 C 0.1101(4) -0.15020(18) 0.12768(11) 0.0201(3) Uani 1 1 d . . . H14 H 0.2699 -0.2215 0.1101 0.024 Uiso 1 1 calc R . . C15 C 0.1374(4) -0.13507(18) 0.07277(11) 0.0203(3) Uani 1 1 d . . . H15 H 0.3183 -0.1966 0.0178 0.024 Uiso 1 1 calc R . . C16 C -0.1667(4) -0.06761(18) 0.26420(11) 0.0180(3) Uani 1 1 d . . . C17 C -0.3355(4) 0.05103(19) 0.32084(11) 0.0210(4) Uani 1 1 d . . . H17 H -0.4671 0.1335 0.3309 0.025 Uiso 1 1 calc R . . C18 C -0.3139(4) 0.05019(19) 0.36253(11) 0.0212(4) Uani 1 1 d . . . H18 H -0.4293 0.1319 0.4003 0.025 Uiso 1 1 calc R . . C19 C -0.1231(4) -0.07053(19) 0.34911(11) 0.0196(3) Uani 1 1 d . . . C20 C 0.0294(4) -0.19084(19) 0.29715(11) 0.0209(4) Uani 1 1 d . . . H20 H 0.1509 -0.275 0.29 0.025 Uiso 1 1 calc R . . C21 C 0.0064(4) -0.18948(18) 0.25593(11) 0.0202(3) Uani 1 1 d . . . H21 H 0.1103 -0.2729 0.2215 0.024 Uiso 1 1 calc R . . C22 C -0.0690(4) -0.07594(19) 0.38498(11) 0.0222(4) Uani 1 1 d . . . H22 H 0.0522 -0.1642 0.3758 0.027 Uiso 1 1 calc R . . C23 C -0.1742(4) 0.0316(2) 0.42935(11) 0.0224(4) Uani 1 1 d . . . H23 H -0.3055 0.1204 0.4424 0.027 Uiso 1 1 calc R . . C24 C -0.0928(4) 0.0165(2) 0.45851(12) 0.0225(4) Uani 1 1 d . . . C31 C -0.1140(4) 0.58996(19) 0.11867(12) 0.0236(4) Uani 1 1 d . . . H31 H -0.0929 0.6682 0.0929 0.028 Uiso 1 1 calc R . . C32 C -0.1568(4) 0.58389(19) 0.17659(12) 0.0239(4) Uani 1 1 d . . . H32 H -0.166 0.6576 0.19 0.029 Uiso 1 1 calc R . . C33 C -0.1867(4) 0.47103(19) 0.21565(11) 0.0209(4) Uani 1 1 d . . . C34 C -0.1775(5) 0.3688(2) 0.19390(13) 0.0288(4) Uani 1 1 d . . . H34 H -0.2008 0.2901 0.2193 0.035 Uiso 1 1 calc R . . C35 C -0.1345(5) 0.3822(2) 0.13521(13) 0.0282(4) Uani 1 1 d . . . H35 H -0.1284 0.311 0.1214 0.034 Uiso 1 1 calc R . . C36 C -0.2093(4) 0.46007(19) 0.27262(11) 0.0193(3) Uani 1 1 d . . . C37 C -0.3377(4) 0.57985(19) 0.31974(12) 0.0233(4) Uani 1 1 d . . . H37 H -0.4395 0.6674 0.3223 0.028 Uiso 1 1 calc R . . C38 C -0.3188(4) 0.57278(19) 0.36263(12) 0.0228(4) Uani 1 1 d . . . H38 H -0.4067 0.6554 0.3939 0.027 Uiso 1 1 calc R . . C39 C -0.1716(4) 0.44541(19) 0.36041(11) 0.0203(4) Uani 1 1 d . . . C40 C -0.0661(4) 0.3259(2) 0.31920(11) 0.0224(4) Uani 1 1 d . . . H40 H 0.019 0.238 0.3211 0.027 Uiso 1 1 calc R . . C41 C -0.0824(4) 0.33221(19) 0.27558(11) 0.0219(4) Uani 1 1 d . . . H41 H -0.007 0.2493 0.2477 0.026 Uiso 1 1 calc R . . C42 C -0.1114(4) 0.4339(2) 0.39500(12) 0.0238(4) Uani 1 1 d . . . H42 H -0.0331 0.3437 0.3973 0.029 Uiso 1 1 calc R . . C43 C -0.1565(4) 0.5388(2) 0.42364(12) 0.0256(4) Uani 1 1 d . . . H43 H -0.2417 0.6301 0.4239 0.031 Uiso 1 1 calc R . . C44 C -0.0806(4) 0.5196(2) 0.45473(12) 0.0255(4) Uani 1 1 d . . . N2 N 0.2424(3) 0.29177(15) -0.04171(10) 0.0192(3) Uani 1 1 d . . . N1 N -0.2653(3) 0.20415(15) 0.05547(9) 0.0187(3) Uani 1 1 d . . . N11 N -0.0795(3) -0.03755(15) 0.09314(9) 0.0193(3) Uani 1 1 d . . . N21 N -0.1009(4) 0.49029(15) 0.09693(10) 0.0207(3) Uani 1 1 d . . . O11 O -0.1791(3) 0.12289(14) 0.49355(10) 0.0326(3) Uani 1 1 d . . . O12 O 0.0679(3) -0.10642(14) 0.44537(10) 0.0328(3) Uani 1 1 d . . . H212 H 0.1004 -0.1025 0.4645 0.049 Uiso 1 1 calc R . . O31 O -0.1511(4) 0.62545(15) 0.48595(10) 0.0366(4) Uani 1 1 d . . . O32 O 0.0549(3) 0.39551(15) 0.44817(10) 0.0342(3) Uani 1 1 d . . . H232 H 0.0863 0.3974 0.4679 0.051 Uiso 1 1 calc R . . S2 S 0.48119(10) 0.01442(4) -0.10131(3) 0.02160(10) Uani 1 1 d . . . S1 S -0.48650(10) 0.48403(4) 0.10613(3) 0.02462(11) Uani 1 1 d . . . Ni1 Ni 0 0 0 0.01384(8) Uani 1 2 d S . . Ni2 Ni 0 0.5 0 0.01535(8) Uani 1 2 d S . . 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 C2 0.0181(8) 0.0163(8) 0.0197(8) 0.0049(6) -0.0163(7) -0.0082(7) C1 0.0183(8) 0.0177(8) 0.0179(8) 0.0035(6) -0.0156(7) -0.0077(7) C11 0.0200(8) 0.0331(10) 0.0205(9) -0.0019(8) -0.0176(8) -0.0008(8) C12 0.0201(8) 0.0307(10) 0.0186(8) -0.0029(8) -0.0162(8) -0.0014(8) C13 0.0226(8) 0.0203(8) 0.0188(8) 0.0057(7) -0.0182(7) -0.0101(7) C14 0.0227(8) 0.0183(8) 0.0235(8) 0.0020(7) -0.0205(8) -0.0057(7) C15 0.0218(8) 0.0193(8) 0.0219(8) 0.0009(7) -0.0190(8) -0.0055(7) C16 0.0214(8) 0.0207(8) 0.0195(8) 0.0055(7) -0.0180(7) -0.0102(7) C17 0.0224(8) 0.0206(9) 0.0205(8) 0.0025(7) -0.0186(8) -0.0063(7) C18 0.0244(9) 0.0203(9) 0.0206(8) 0.0020(7) -0.0192(8) -0.0079(7) C19 0.0232(8) 0.0221(9) 0.0208(8) 0.0052(7) -0.0194(8) -0.0103(7) C20 0.0237(9) 0.0199(8) 0.0218(8) 0.0038(7) -0.0199(8) -0.0072(7) C21 0.0261(9) 0.0183(8) 0.0217(8) 0.0034(7) -0.0210(8) -0.0083(7) C22 0.0243(9) 0.0255(9) 0.0219(8) 0.0048(7) -0.0203(8) -0.0098(8) C23 0.0254(9) 0.0268(9) 0.0229(9) 0.0053(8) -0.0215(8) -0.0107(8) C24 0.0257(9) 0.0265(9) 0.0226(8) 0.0041(8) -0.0210(8) -0.0113(8) C31 0.0368(10) 0.0219(9) 0.0296(9) 0.0105(8) -0.0299(9) -0.0170(8) C32 0.0368(10) 0.0222(9) 0.0284(9) 0.0082(8) -0.0290(9) -0.0160(8) C33 0.0253(9) 0.0228(9) 0.0209(8) 0.0050(7) -0.0201(8) -0.0110(8) C34 0.0509(12) 0.0256(10) 0.0365(10) 0.0172(9) -0.0397(11) -0.0248(10) C35 0.0498(12) 0.0255(10) 0.0361(11) 0.0153(9) -0.0389(11) -0.0241(10) C36 0.0224(8) 0.0229(9) 0.0195(8) 0.0054(7) -0.0185(8) -0.0102(7) C37 0.0275(9) 0.0210(9) 0.0253(9) 0.0029(7) -0.0236(9) -0.0063(8) C38 0.0269(9) 0.0204(9) 0.0237(9) 0.0000(7) -0.0221(8) -0.0057(8) C39 0.0199(8) 0.0246(9) 0.0170(8) 0.0028(7) -0.0159(7) -0.0075(7) C40 0.0246(9) 0.0226(9) 0.0213(8) 0.0047(7) -0.0199(8) -0.0084(8) C41 0.0265(9) 0.0210(9) 0.0213(8) 0.0049(7) -0.0206(8) -0.0101(8) C42 0.0241(9) 0.0283(10) 0.0218(9) 0.0023(8) -0.0202(8) -0.0079(8) C43 0.0324(10) 0.0294(10) 0.0292(10) 0.0084(8) -0.0282(9) -0.0136(9) C44 0.0282(9) 0.0307(10) 0.0258(9) 0.0060(8) -0.0236(9) -0.0131(9) N2 0.0219(7) 0.0172(7) 0.0238(7) 0.0037(6) -0.0197(7) -0.0085(6) N1 0.0197(7) 0.0172(7) 0.0209(7) 0.0035(6) -0.0170(6) -0.0082(6) N11 0.0202(7) 0.0210(7) 0.0188(7) 0.0028(6) -0.0172(6) -0.0063(6) N21 0.0305(8) 0.0185(7) 0.0247(7) 0.0068(6) -0.0246(7) -0.0124(7) O11 0.0461(9) 0.0264(7) 0.0460(9) 0.0019(7) -0.0424(8) -0.0098(7) O12 0.0406(8) 0.0276(7) 0.0433(8) -0.0034(7) -0.0389(8) -0.0026(7) O31 0.0505(9) 0.0317(8) 0.0518(10) 0.0038(7) -0.0473(9) -0.0120(7) O32 0.0437(9) 0.0305(8) 0.0446(9) 0.0018(7) -0.0411(8) -0.0069(7) S2 0.0192(2) 0.0134(2) 0.0251(2) 0.00009(17) -0.0170(2) -0.00578(17) S1 0.0209(2) 0.0136(2) 0.0295(2) -0.00188(18) -0.0191(2) -0.00509(18) Ni1 0.01798(15) 0.01076(14) 0.01665(14) 0.00246(11) -0.01510(14) -0.00572(12) Ni2 0.02185(16) 0.01224(15) 0.01946(15) 0.00388(12) -0.01831(14) -0.00783(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 C2 N2 1.158(2) . ? C2 S2 1.6450(19) . ? C1 N1 1.158(2) . ? C1 S1 1.6407(19) . ? C11 N11 1.343(2) . ? C11 C12 1.382(3) . ? C11 H11 0.95 . ? C12 C13 1.397(3) . ? C12 H12 0.95 . ? C13 C14 1.394(3) . ? C13 C16 1.485(2) . ? C14 C15 1.380(2) . ? C14 H14 0.95 . ? C15 N11 1.346(2) . ? C15 H15 0.95 . ? C16 C21 1.393(3) . ? C16 C17 1.402(3) . ? C17 C18 1.389(2) . ? C17 H17 0.95 . ? C18 C19 1.400(3) . ? C18 H18 0.95 . ? C19 C20 1.396(3) . ? C19 C22 1.467(2) . ? C20 C21 1.385(2) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C23 1.339(2) . ? C22 H22 0.95 . ? C23 C24 1.471(2) . ? C23 H23 0.95 . ? C24 O11 1.251(2) . ? C24 O12 1.289(2) . ? C31 N21 1.345(2) . ? C31 C32 1.378(2) . ? C31 H31 0.95 . ? C32 C33 1.393(3) . ? C32 H32 0.95 . ? C33 C34 1.396(2) . ? C33 C36 1.479(2) . ? C34 C35 1.387(3) . ? C34 H34 0.95 . ? C35 N21 1.341(2) . ? C35 H35 0.95 . ? C36 C41 1.395(3) . ? C36 C37 1.402(3) . ? C37 C38 1.384(3) . ? C37 H37 0.95 . ? C38 C39 1.399(3) . ? C38 H38 0.95 . ? C39 C40 1.398(3) . ? C39 C42 1.461(2) . ? C40 C41 1.387(2) . ? C40 H40 0.95 . ? C41 H41 0.95 . ? C42 C43 1.335(3) . ? C42 H42 0.95 . ? C43 C44 1.468(3) . ? C43 H43 0.95 . ? C44 O31 1.256(2) . ? C44 O32 1.282(2) . ? N2 Ni2 2.0261(19) . ? N1 Ni1 2.023(2) . ? N11 Ni1 2.1192(15) . ? N21 Ni2 2.1201(15) . ? O12 H212 0.84 . ? O32 H232 0.84 . ? S2 Ni1 2.5185(9) . ? S1 Ni2 2.5250(9) . ? Ni1 N1 2.023(2) 2 ? Ni1 N11 2.1192(15) 2 ? Ni1 S2 2.5185(9) 2 ? Ni2 N2 2.0261(19) 2_565 ? Ni2 N21 2.1201(15) 2_565 ? Ni2 S1 2.5250(9) 2_565 ? 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 C2 S2 179.17(16) . . ? N1 C1 S1 178.3(2) . . ? N11 C11 C12 123.78(17) . . ? N11 C11 H11 118.1 . . ? C12 C11 H11 118.1 . . ? C11 C12 C13 120.16(17) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 115.75(16) . . ? C14 C13 C16 120.97(16) . . ? C12 C13 C16 123.15(17) . . ? C15 C14 C13 120.70(17) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? N11 C15 C14 123.33(17) . . ? N11 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C21 C16 C17 117.85(16) . . ? C21 C16 C13 120.47(16) . . ? C17 C16 C13 121.46(16) . . ? C18 C17 C16 121.21(17) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 120.33(17) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 118.28(17) . . ? C20 C19 C22 118.42(17) . . ? C18 C19 C22 123.27(17) . . ? C21 C20 C19 121.04(17) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C16 121.01(17) . . ? C20 C21 H21 119.5 . . ? C16 C21 H21 119.5 . . ? C23 C22 C19 126.25(18) . . ? C23 C22 H22 116.9 . . ? C19 C22 H22 116.9 . . ? C22 C23 C24 122.08(18) . . ? C22 C23 H23 119 . . ? C24 C23 H23 119 . . ? O11 C24 O12 123.50(17) . . ? O11 C24 C23 118.74(18) . . ? O12 C24 C23 117.75(16) . . ? N21 C31 C32 123.03(17) . . ? N21 C31 H31 118.5 . . ? C32 C31 H31 118.5 . . ? C31 C32 C33 120.79(17) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? C32 C33 C34 115.97(16) . . ? C32 C33 C36 120.52(16) . . ? C34 C33 C36 123.43(17) . . ? C35 C34 C33 119.99(17) . . ? C35 C34 H34 120 . . ? C33 C34 H34 120 . . ? N21 C35 C34 123.46(17) . . ? N21 C35 H35 118.3 . . ? C34 C35 H35 118.3 . . ? C41 C36 C37 118.20(16) . . ? C41 C36 C33 121.33(17) . . ? C37 C36 C33 120.25(17) . . ? C38 C37 C36 121.14(17) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C37 C38 C39 120.75(17) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C40 C39 C38 117.62(17) . . ? C40 C39 C42 119.60(17) . . ? C38 C39 C42 122.69(17) . . ? C41 C40 C39 121.76(17) . . ? C41 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? C40 C41 C36 120.17(17) . . ? C40 C41 H41 119.9 . . ? C36 C41 H41 119.9 . . ? C43 C42 C39 125.83(19) . . ? C43 C42 H42 117.1 . . ? C39 C42 H42 117.1 . . ? C42 C43 C44 123.12(19) . . ? C42 C43 H43 118.4 . . ? C44 C43 H43 118.4 . . ? O31 C44 O32 123.78(18) . . ? O31 C44 C43 118.22(18) . . ? O32 C44 C43 118.00(17) . . ? C2 N2 Ni2 162.61(14) . . ? C1 N1 Ni1 164.91(14) . . ? C11 N11 C15 116.20(16) . . ? C11 N11 Ni1 121.85(12) . . ? C15 N11 Ni1 121.54(12) . . ? C35 N21 C31 116.74(16) . . ? C35 N21 Ni2 122.51(12) . . ? C31 N21 Ni2 120.61(12) . . ? C24 O12 H212 109.5 . . ? C44 O32 H232 109.5 . . ? C2 S2 Ni1 100.00(8) . . ? C1 S1 Ni2 101.52(9) . . ? N1 Ni1 N1 180.0(3) . 2 ? N1 Ni1 N11 89.89(7) . . ? N1 Ni1 N11 90.11(7) 2 . ? N1 Ni1 N11 90.11(7) . 2 ? N1 Ni1 N11 89.89(7) 2 2 ? N11 Ni1 N11 180.00(5) . 2 ? N1 Ni1 S2 94.62(7) . . ? N1 Ni1 S2 85.38(7) 2 . ? N11 Ni1 S2 89.25(5) . . ? N11 Ni1 S2 90.75(5) 2 . ? N1 Ni1 S2 85.38(7) . 2 ? N1 Ni1 S2 94.62(7) 2 2 ? N11 Ni1 S2 90.75(5) . 2 ? N11 Ni1 S2 89.25(5) 2 2 ? S2 Ni1 S2 180.00(4) . 2 ? N2 Ni2 N2 180.00(18) 2_565 . ? N2 Ni2 N21 89.70(7) 2_565 . ? N2 Ni2 N21 90.30(7) . . ? N2 Ni2 N21 90.30(7) 2_565 2_565 ? N2 Ni2 N21 89.70(7) . 2_565 ? N21 Ni2 N21 180.00(4) . 2_565 ? N2 Ni2 S1 92.59(7) 2_565 2_565 ? N2 Ni2 S1 87.41(7) . 2_565 ? N21 Ni2 S1 90.29(5) . 2_565 ? N21 Ni2 S1 89.71(5) 2_565 2_565 ? N2 Ni2 S1 87.41(7) 2_565 . ? N2 Ni2 S1 92.59(7) . . ? N21 Ni2 S1 89.71(5) . . ? N21 Ni2 S1 90.29(5) 2_565 . ? S1 Ni2 S1 180.00(2) 2_565 . ? #===END