# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Seiji Ogo' _publ_contact_author_email OGO-TCM@MBOX.NC.KYUSHU-U.AC.JP _publ_section_title ; Critical aspects of [NiFe]hydrogenase ligand composition ; loop_ _publ_author_name 'Seiji Ogo' 'Koji Ichikawa' 'Takahiro Matsumoto' # Attachment 'CIF_NiFe' data__Ni(C13H28N2S2)Fe(CH3CN)(T _database_code_depnum_ccdc_archive 'CCDC 707320' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C33 H56 B2 F8 Fe N10 Ni S2 ' _chemical_formula_moiety ? _chemical_formula_weight 945.15 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 30.102(5) _cell_length_b 10.651(2) _cell_length_c 26.668(4) _cell_angle_alpha 90 _cell_angle_beta 97.138(2) _cell_angle_gamma 90 _cell_volume 8483(2) _cell_formula_units_Z 8 _cell_measurement_reflns_used 12710 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.2 #------------------------------------------------------------------------------ _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.140 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936.00 _exptl_absorpt_coefficient_mu 0.958 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Jacobson, 1998)' _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 0.935 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Saturn CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.57 _diffrn_reflns_number 33913 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9930 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9930 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 9665 _reflns_number_gt 5392 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0624 _refine_ls_wR_factor_ref 0.1574 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9665 _refine_ls_number_parameters 514 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0006 _refine_diff_density_max 1.18 _refine_diff_density_min -0.94 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; B B 0.001 0.001 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; F F 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Fe Fe 0.346 0.844 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ni(1) Ni 0.31534(2) 0.32179(5) 0.15307(2) 0.0257(2) Uani 1.00 1 d . . . Fe(1) Fe 0.40059(2) 0.20760(6) 0.09441(2) 0.0231(2) Uani 1.00 1 d . . . S(1) S 0.38068(4) 0.3927(1) 0.14243(5) 0.0348(3) Uani 1.00 1 d . . . S(2) S 0.31727(3) 0.2252(1) 0.08185(4) 0.0241(3) Uani 1.00 1 d . . . F(1) F 0.2783(2) 0.6855(6) -0.1364(2) 0.187(3) Uani 1.00 1 d . . . F(2) F 0.3092(2) 0.8607(4) -0.1567(2) 0.107(2) Uani 1.00 1 d . . . F(3) F 0.3429(2) 0.7473(7) -0.0996(3) 0.180(3) Uani 1.00 1 d . . . F(4) F 0.2822(2) 0.8350(5) -0.0829(2) 0.136(2) Uani 1.00 1 d . . . F(5) F 0.3869(1) 0.2303(3) -0.1912(1) 0.0515(10) Uani 1.00 1 d . . . F(6) F 0.4265(1) 0.4036(3) -0.1646(1) 0.063(1) Uani 1.00 1 d . . . F(7) F 0.4176(1) 0.2502(3) -0.1098(1) 0.061(1) Uani 1.00 1 d . . . F(8) F 0.35940(10) 0.3712(4) -0.1415(1) 0.072(1) Uani 1.00 1 d . . . N(1) N 0.3972(1) 0.3395(4) 0.0283(1) 0.0267(10) Uani 1.00 1 d . . . N(2) N 0.3204(1) 0.4251(4) 0.2157(2) 0.040(1) Uani 1.00 1 d . . . N(3) N 0.2550(1) 0.2508(4) 0.1537(1) 0.030(1) Uani 1.00 1 d . . . N(4) N 0.4145(1) 0.0592(3) 0.0439(1) 0.0243(9) Uani 1.00 1 d . . . N(5) N 0.4529(1) -0.0098(3) 0.0574(1) 0.0228(9) Uani 1.00 1 d . . . N(6) N 0.4729(1) 0.2360(4) 0.1006(1) 0.0254(10) Uani 1.00 1 d . . . N(7) N 0.4985(1) 0.1306(4) 0.1119(1) 0.0251(10) Uani 1.00 1 d . . . N(8) N 0.4162(1) 0.0602(4) 0.1534(1) 0.028(1) Uani 1.00 1 d . . . N(9) N 0.4515(1) -0.0167(4) 0.1464(1) 0.0251(10) Uani 1.00 1 d . . . N(10) N 0.4019(2) -0.2774(5) 0.0851(2) 0.056(2) Uani 1.00 1 d . . . C(1) C 0.3959(1) 0.4148(4) -0.0020(2) 0.028(1) Uani 1.00 1 d . . . C(2) C 0.3958(2) 0.5139(5) -0.0400(2) 0.042(2) Uani 1.00 1 d . . . C(3) C 0.4042(2) 0.4327(7) 0.2076(2) 0.067(2) Uani 1.00 1 d . . . C(4) C 0.3668(2) 0.4149(6) 0.2411(2) 0.050(2) Uani 1.00 1 d . . . C(5) C 0.3090(2) 0.5570(6) 0.1992(2) 0.063(2) Uani 1.00 1 d . . . C(6) C 0.2910(2) 0.3875(5) 0.2547(2) 0.040(1) Uani 1.00 1 d . . . C(7) C 0.2433(2) 0.3643(5) 0.2351(2) 0.045(2) Uani 1.00 1 d . . . C(8) C 0.2378(1) 0.2442(5) 0.2039(2) 0.035(1) Uani 1.00 1 d . . . C(9) C 0.2239(2) 0.3331(6) 0.1202(2) 0.044(2) Uani 1.00 1 d . . . C(10) C 0.2543(1) 0.1191(5) 0.1338(2) 0.031(1) Uani 1.00 1 d . . . C(11) C 0.2760(1) 0.0979(5) 0.0857(2) 0.032(1) Uani 1.00 1 d . . . C(12) C 0.4428(2) 0.3447(10) 0.2268(2) 0.094(3) Uani 1.00 1 d . . . C(13) C 0.4214(3) 0.5683(9) 0.2079(3) 0.124(4) Uani 1.00 1 d . . . C(14) C 0.2414(2) 0.0999(6) 0.0382(2) 0.049(2) Uani 1.00 1 d . . . C(15) C 0.3002(2) -0.0283(5) 0.0888(2) 0.041(2) Uani 1.00 1 d . . . C(16) C 0.3564(1) 0.0686(5) -0.0299(2) 0.031(1) Uani 1.00 1 d . . . C(17) C 0.3971(1) 0.0122(4) -0.0004(2) 0.025(1) Uani 1.00 1 d . . . C(18) C 0.4231(1) -0.0877(4) -0.0146(2) 0.027(1) Uani 1.00 1 d . . . C(19) C 0.4583(1) -0.1011(4) 0.0228(2) 0.026(1) Uani 1.00 1 d . . . C(20) C 0.4960(2) -0.1913(5) 0.0279(2) 0.034(1) Uani 1.00 1 d . . . C(21) C 0.4876(2) 0.4642(5) 0.0975(2) 0.037(1) Uani 1.00 1 d . . . C(22) C 0.5020(1) 0.3315(5) 0.1089(2) 0.029(1) Uani 1.00 1 d . . . C(23) C 0.5452(1) 0.2871(5) 0.1258(2) 0.030(1) Uani 1.00 1 d . . . C(24) C 0.5424(1) 0.1594(5) 0.1285(2) 0.029(1) Uani 1.00 1 d . . . C(25) C 0.5762(1) 0.0625(5) 0.1454(2) 0.036(1) Uani 1.00 1 d . . . C(26) C 0.3607(2) 0.0634(5) 0.2153(2) 0.040(1) Uani 1.00 1 d . . . C(27) C 0.4002(1) 0.0104(5) 0.1940(2) 0.030(1) Uani 1.00 1 d . . . C(28) C 0.4250(2) -0.0949(5) 0.2116(2) 0.032(1) Uani 1.00 1 d . . . C(29) C 0.4578(1) -0.1107(4) 0.1808(2) 0.026(1) Uani 1.00 1 d . . . C(30) C 0.4940(2) -0.2061(5) 0.1795(2) 0.033(1) Uani 1.00 1 d . . . C(31) C 0.3669(2) -0.3090(5) 0.0711(2) 0.045(2) Uani 1.00 1 d . . . C(32) C 0.3219(2) -0.3523(6) 0.0516(3) 0.067(2) Uani 1.00 1 d . . . C(33) C 0.4781(1) 0.0078(4) 0.1065(2) 0.025(1) Uani 1.00 1 d . . . B(1) B 0.3027(3) 0.7768(7) -0.1186(3) 0.053(2) Uani 1.00 1 d . . . B(2) B 0.3980(2) 0.3122(5) -0.1519(2) 0.031(1) Uani 1.00 1 d . . . H(1) H 0.4230 0.5106 -0.0554 0.0528 Uiso 1.00 1 calc . . . H(2) H 0.3712 0.5042 -0.0656 0.0528 Uiso 1.00 1 calc . . . H(3) H 0.3941 0.5946 -0.0247 0.0528 Uiso 1.00 1 calc . . . H(4) H 0.3700 0.3337 0.2568 0.0607 Uiso 1.00 1 calc . . . H(5) H 0.3706 0.4769 0.2674 0.0607 Uiso 1.00 1 calc . . . H(6) H 0.3263 0.5825 0.1735 0.0780 Uiso 1.00 1 calc . . . H(7) H 0.2774 0.5590 0.1839 0.0780 Uiso 1.00 1 calc . . . H(8) H 0.3122 0.6132 0.2261 0.0780 Uiso 1.00 1 calc . . . H(9) H 0.3033 0.3099 0.2704 0.0484 Uiso 1.00 1 calc . . . H(10) H 0.2928 0.4496 0.2803 0.0484 Uiso 1.00 1 calc . . . H(11) H 0.2325 0.4322 0.2147 0.0485 Uiso 1.00 1 calc . . . H(12) H 0.2262 0.3571 0.2631 0.0485 Uiso 1.00 1 calc . . . H(13) H 0.2534 0.1769 0.2232 0.0420 Uiso 1.00 1 calc . . . H(14) H 0.2067 0.2219 0.1987 0.0420 Uiso 1.00 1 calc . . . H(15) H 0.2307 0.3249 0.0855 0.0506 Uiso 1.00 1 calc . . . H(16) H 0.2250 0.4153 0.1298 0.0506 Uiso 1.00 1 calc . . . H(17) H 0.1933 0.3010 0.1194 0.0506 Uiso 1.00 1 calc . . . H(18) H 0.2226 0.0946 0.1264 0.0383 Uiso 1.00 1 calc . . . H(19) H 0.2675 0.0648 0.1595 0.0383 Uiso 1.00 1 calc . . . H(20) H 0.4324 0.2572 0.2245 0.0993 Uiso 1.00 1 calc . . . H(21) H 0.4667 0.3503 0.2063 0.0993 Uiso 1.00 1 calc . . . H(22) H 0.4539 0.3604 0.2608 0.0993 Uiso 1.00 1 calc . . . H(23) H 0.4426 0.5829 0.1850 0.1296 Uiso 1.00 1 calc . . . H(24) H 0.4305 0.6017 0.2394 0.1296 Uiso 1.00 1 calc . . . H(25) H 0.3947 0.6249 0.1933 0.1296 Uiso 1.00 1 calc . . . H(26) H 0.2193 0.0361 0.0385 0.0574 Uiso 1.00 1 calc . . . H(27) H 0.2553 0.0917 0.0081 0.0574 Uiso 1.00 1 calc . . . H(28) H 0.2257 0.1804 0.0360 0.0574 Uiso 1.00 1 calc . . . H(29) H 0.2792 -0.0963 0.0922 0.0479 Uiso 1.00 1 calc . . . H(30) H 0.3137 -0.0438 0.0588 0.0479 Uiso 1.00 1 calc . . . H(31) H 0.3225 -0.0312 0.1172 0.0479 Uiso 1.00 1 calc . . . H(32) H 0.3316 0.0667 -0.0107 0.0370 Uiso 1.00 1 calc . . . H(33) H 0.3620 0.1539 -0.0382 0.0370 Uiso 1.00 1 calc . . . H(34) H 0.3482 0.0233 -0.0607 0.0370 Uiso 1.00 1 calc . . . H(35) H 0.4166 -0.1393 -0.0457 0.0336 Uiso 1.00 1 calc . . . H(36) H 0.4938 -0.2482 -0.0002 0.0440 Uiso 1.00 1 calc . . . H(37) H 0.5243 -0.1492 0.0296 0.0440 Uiso 1.00 1 calc . . . H(38) H 0.4964 -0.2411 0.0582 0.0440 Uiso 1.00 1 calc . . . H(39) H 0.4642 0.4880 0.1171 0.0440 Uiso 1.00 1 calc . . . H(40) H 0.4761 0.4739 0.0625 0.0440 Uiso 1.00 1 calc . . . H(41) H 0.5119 0.5213 0.1051 0.0440 Uiso 1.00 1 calc . . . H(42) H 0.5721 0.3374 0.1414 0.0402 Uiso 1.00 1 calc . . . H(43) H 0.6050 0.0988 0.1551 0.0443 Uiso 1.00 1 calc . . . H(44) H 0.5792 0.0039 0.1181 0.0443 Uiso 1.00 1 calc . . . H(45) H 0.5677 0.0154 0.1730 0.0443 Uiso 1.00 1 calc . . . H(46) H 0.3669 0.1505 0.2255 0.0489 Uiso 1.00 1 calc . . . H(47) H 0.3351 0.0650 0.1903 0.0489 Uiso 1.00 1 calc . . . H(48) H 0.3541 0.0185 0.2438 0.0489 Uiso 1.00 1 calc . . . H(49) H 0.4202 -0.1461 0.2407 0.0369 Uiso 1.00 1 calc . . . H(50) H 0.4936 -0.2669 0.2062 0.0405 Uiso 1.00 1 calc . . . H(51) H 0.4896 -0.2527 0.1479 0.0405 Uiso 1.00 1 calc . . . H(52) H 0.5228 -0.1690 0.1823 0.0405 Uiso 1.00 1 calc . . . H(53) H 0.5015 -0.0549 0.1095 0.0402 Uiso 1.00 1 calc . . . H(54) H 0.3219 -0.4380 0.0399 0.0743 Uiso 1.00 1 calc . . . H(55) H 0.3017 -0.3485 0.0770 0.0743 Uiso 1.00 1 calc . . . H(56) H 0.3087 -0.3019 0.0235 0.0743 Uiso 1.00 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni(1) 0.0303(3) 0.0246(3) 0.0241(3) 0.0014(2) 0.0109(2) 0.0009(2) Fe(1) 0.0232(3) 0.0289(3) 0.0180(3) 0.0003(3) 0.0056(2) 0.0025(3) S(1) 0.0409(7) 0.0368(7) 0.0296(6) -0.0152(6) 0.0162(5) -0.0092(6) S(2) 0.0228(5) 0.0279(6) 0.0220(5) 0.0016(4) 0.0050(4) 0.0020(5) F(1) 0.273(7) 0.203(6) 0.114(4) -0.195(6) 0.135(5) -0.106(4) F(2) 0.097(3) 0.080(3) 0.148(5) -0.015(3) 0.029(3) 0.032(3) F(3) 0.107(4) 0.210(7) 0.224(8) 0.073(4) 0.020(4) 0.120(6) F(4) 0.128(4) 0.129(4) 0.170(6) -0.051(3) 0.092(4) -0.079(4) F(5) 0.059(2) 0.056(2) 0.040(2) 0.003(2) 0.007(2) -0.021(2) F(6) 0.050(2) 0.066(2) 0.071(3) -0.020(2) -0.002(2) 0.027(2) F(7) 0.085(2) 0.060(2) 0.036(2) 0.017(2) 0.001(2) 0.016(2) F(8) 0.035(2) 0.088(3) 0.093(3) 0.012(2) 0.009(2) -0.052(2) N(1) 0.031(2) 0.026(2) 0.023(2) -0.000(2) 0.005(2) 0.003(2) N(2) 0.059(3) 0.031(2) 0.034(2) -0.004(2) 0.022(2) -0.005(2) N(3) 0.026(2) 0.041(2) 0.026(2) 0.010(2) 0.008(2) 0.008(2) N(4) 0.025(2) 0.031(2) 0.018(2) 0.005(2) 0.006(1) 0.004(2) N(5) 0.024(2) 0.028(2) 0.017(2) 0.005(1) 0.001(1) 0.003(2) N(6) 0.023(2) 0.032(2) 0.021(2) -0.001(2) 0.006(1) 0.002(2) N(7) 0.025(2) 0.030(2) 0.020(2) 0.002(2) 0.002(1) 0.002(2) N(8) 0.027(2) 0.037(2) 0.019(2) 0.005(2) 0.006(1) 0.012(2) N(9) 0.025(2) 0.033(2) 0.018(2) 0.007(2) 0.004(1) 0.007(2) N(10) 0.059(3) 0.054(3) 0.053(3) -0.010(3) 0.007(3) 0.008(3) C(1) 0.029(2) 0.029(3) 0.027(2) 0.000(2) 0.006(2) -0.003(2) C(2) 0.057(3) 0.035(3) 0.036(3) -0.001(3) 0.011(2) 0.005(2) C(3) 0.064(4) 0.115(6) 0.027(3) -0.060(4) 0.023(3) -0.028(3) C(4) 0.056(3) 0.064(4) 0.034(3) -0.029(3) 0.020(3) -0.019(3) C(5) 0.110(5) 0.034(3) 0.055(4) 0.007(3) 0.045(4) -0.004(3) C(6) 0.052(3) 0.038(3) 0.035(3) 0.000(2) 0.022(2) -0.003(2) C(7) 0.054(3) 0.048(3) 0.037(3) 0.016(3) 0.027(3) 0.008(3) C(8) 0.026(2) 0.051(3) 0.028(3) 0.007(2) 0.010(2) 0.009(2) C(9) 0.027(2) 0.069(4) 0.038(3) 0.020(2) 0.007(2) 0.017(3) C(10) 0.027(2) 0.035(3) 0.031(3) 0.003(2) 0.003(2) 0.003(2) C(11) 0.033(2) 0.037(3) 0.026(2) -0.009(2) 0.004(2) -0.002(2) C(12) 0.033(3) 0.22(1) 0.026(3) -0.032(5) 0.003(2) -0.019(5) C(13) 0.172(8) 0.148(8) 0.067(5) -0.130(7) 0.074(6) -0.069(5) C(14) 0.045(3) 0.071(4) 0.030(3) -0.020(3) 0.003(2) -0.003(3) C(15) 0.055(3) 0.028(3) 0.043(3) -0.014(2) 0.018(3) -0.008(2) C(16) 0.032(2) 0.041(3) 0.018(2) 0.006(2) -0.003(2) -0.002(2) C(17) 0.025(2) 0.032(2) 0.019(2) 0.000(2) 0.004(2) 0.005(2) C(18) 0.033(2) 0.033(3) 0.015(2) 0.002(2) 0.005(2) -0.001(2) C(19) 0.034(2) 0.025(2) 0.021(2) 0.005(2) 0.012(2) 0.001(2) C(20) 0.036(3) 0.040(3) 0.029(3) 0.013(2) 0.009(2) 0.006(2) C(21) 0.034(3) 0.033(3) 0.047(3) -0.008(2) 0.010(2) -0.000(2) C(22) 0.031(2) 0.037(3) 0.021(2) -0.007(2) 0.011(2) 0.000(2) C(23) 0.030(2) 0.042(3) 0.017(2) -0.005(2) 0.005(2) 0.000(2) C(24) 0.022(2) 0.052(3) 0.012(2) -0.000(2) -0.000(2) 0.001(2) C(25) 0.025(2) 0.053(3) 0.028(3) -0.000(2) -0.002(2) 0.012(2) C(26) 0.037(3) 0.054(3) 0.033(3) 0.014(2) 0.015(2) 0.016(3) C(27) 0.026(2) 0.044(3) 0.022(2) 0.006(2) 0.007(2) 0.010(2) C(28) 0.034(2) 0.039(3) 0.023(2) 0.004(2) 0.006(2) 0.010(2) C(29) 0.026(2) 0.033(3) 0.020(2) 0.000(2) 0.002(2) 0.006(2) C(30) 0.033(2) 0.036(3) 0.029(3) 0.007(2) 0.001(2) 0.005(2) C(31) 0.058(4) 0.034(3) 0.044(3) -0.006(3) 0.010(3) -0.007(3) C(32) 0.061(4) 0.052(4) 0.084(5) 0.002(3) -0.001(4) -0.018(4) C(33) 0.023(2) 0.034(3) 0.020(2) 0.004(2) 0.004(2) 0.004(2) B(1) 0.060(4) 0.040(4) 0.065(5) -0.014(3) 0.028(4) -0.015(4) B(2) 0.032(3) 0.031(3) 0.030(3) 0.001(2) 0.003(2) 0.000(2) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 2.0' _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni(1) S(1) 2.158(1) . . yes Ni(1) S(2) 2.167(1) . . yes Ni(1) N(2) 1.990(4) . . yes Ni(1) N(3) 1.968(4) . . yes Fe(1) S(1) 2.465(1) . . yes Fe(1) S(2) 2.496(1) . . yes Fe(1) N(1) 2.247(4) . . yes Fe(1) N(4) 2.151(4) . . yes Fe(1) N(6) 2.184(4) . . yes Fe(1) N(8) 2.232(4) . . yes S(1) C(3) 1.844(6) . . yes S(2) C(11) 1.850(5) . . yes F(1) B(1) 1.274(8) . . yes F(2) B(1) 1.385(9) . . yes F(3) B(1) 1.293(9) . . yes F(4) B(1) 1.347(8) . . yes F(5) B(2) 1.374(6) . . yes F(6) B(2) 1.368(6) . . yes F(7) B(2) 1.370(6) . . yes F(8) B(2) 1.378(6) . . yes N(1) C(1) 1.135(6) . . yes N(2) C(4) 1.480(7) . . yes N(2) C(5) 1.500(7) . . yes N(2) C(6) 1.499(6) . . yes N(3) C(8) 1.497(6) . . yes N(3) C(9) 1.496(6) . . yes N(3) C(10) 1.498(6) . . yes N(4) N(5) 1.381(4) . . yes N(4) C(17) 1.329(5) . . yes N(5) C(19) 1.364(5) . . yes N(5) C(33) 1.440(5) . . yes N(6) N(7) 1.373(5) . . yes N(6) C(22) 1.343(6) . . yes N(7) C(24) 1.375(5) . . yes N(7) C(33) 1.444(6) . . yes N(8) N(9) 1.372(5) . . yes N(8) C(27) 1.346(5) . . yes N(9) C(29) 1.356(5) . . yes N(9) C(33) 1.436(5) . . yes N(10) C(31) 1.126(7) . . yes C(1) C(2) 1.463(7) . . yes C(3) C(4) 1.535(7) . . yes C(3) C(12) 1.53(1) . . yes C(3) C(13) 1.534(10) . . yes C(6) C(7) 1.488(7) . . yes C(7) C(8) 1.523(7) . . yes C(10) C(11) 1.527(6) . . yes C(11) C(14) 1.538(7) . . yes C(11) C(15) 1.525(7) . . yes C(16) C(17) 1.499(6) . . yes C(17) C(18) 1.400(6) . . yes C(18) C(19) 1.371(6) . . yes C(19) C(20) 1.479(6) . . yes C(21) C(22) 1.498(7) . . yes C(22) C(23) 1.405(6) . . yes C(23) C(24) 1.366(7) . . yes C(24) C(25) 1.480(6) . . yes C(26) C(27) 1.492(6) . . yes C(27) C(28) 1.395(6) . . yes C(28) C(29) 1.372(6) . . yes C(29) C(30) 1.491(6) . . yes C(31) C(32) 1.463(8) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ni(1) S(2) 85.81(5) . . . yes S(1) Ni(1) N(2) 86.6(1) . . . yes S(1) Ni(1) N(3) 172.7(1) . . . yes S(2) Ni(1) N(2) 172.1(1) . . . yes S(2) Ni(1) N(3) 87.1(1) . . . yes N(2) Ni(1) N(3) 100.3(2) . . . yes S(1) Fe(1) S(2) 72.82(4) . . . yes S(1) Fe(1) N(1) 85.3(1) . . . yes S(1) Fe(1) N(4) 172.6(1) . . . yes S(1) Fe(1) N(6) 98.9(1) . . . yes S(1) Fe(1) N(8) 103.9(1) . . . yes S(2) Fe(1) N(1) 84.29(9) . . . yes S(2) Fe(1) N(4) 103.96(10) . . . yes S(2) Fe(1) N(6) 167.3(1) . . . yes S(2) Fe(1) N(8) 105.51(9) . . . yes N(1) Fe(1) N(4) 87.8(1) . . . yes N(1) Fe(1) N(6) 85.5(1) . . . yes N(1) Fe(1) N(8) 168.1(1) . . . yes N(4) Fe(1) N(6) 83.1(1) . . . yes N(4) Fe(1) N(8) 83.4(1) . . . yes N(6) Fe(1) N(8) 85.6(1) . . . yes Ni(1) S(1) Fe(1) 94.16(5) . . . yes Ni(1) S(1) C(3) 101.9(2) . . . yes Fe(1) S(1) C(3) 125.8(3) . . . yes Ni(1) S(2) Fe(1) 93.09(4) . . . yes Ni(1) S(2) C(11) 102.0(2) . . . yes Fe(1) S(2) C(11) 127.4(2) . . . yes Fe(1) N(1) C(1) 173.7(4) . . . yes Ni(1) N(2) C(4) 108.2(3) . . . yes Ni(1) N(2) C(5) 106.3(3) . . . yes Ni(1) N(2) C(6) 116.4(3) . . . yes C(4) N(2) C(5) 111.8(5) . . . yes C(4) N(2) C(6) 105.5(4) . . . yes C(5) N(2) C(6) 108.7(4) . . . yes Ni(1) N(3) C(8) 116.6(3) . . . yes Ni(1) N(3) C(9) 106.3(3) . . . yes Ni(1) N(3) C(10) 109.3(3) . . . yes C(8) N(3) C(9) 107.5(3) . . . yes C(8) N(3) C(10) 106.3(4) . . . yes C(9) N(3) C(10) 110.9(4) . . . yes Fe(1) N(4) N(5) 116.7(3) . . . yes Fe(1) N(4) C(17) 138.5(3) . . . yes N(5) N(4) C(17) 104.8(3) . . . yes N(4) N(5) C(19) 111.7(3) . . . yes N(4) N(5) C(33) 119.8(3) . . . yes C(19) N(5) C(33) 127.9(4) . . . yes Fe(1) N(6) N(7) 115.5(3) . . . yes Fe(1) N(6) C(22) 137.8(3) . . . yes N(7) N(6) C(22) 104.3(3) . . . yes N(6) N(7) C(24) 112.3(4) . . . yes N(6) N(7) C(33) 119.9(3) . . . yes C(24) N(7) C(33) 127.8(4) . . . yes Fe(1) N(8) N(9) 115.0(3) . . . yes Fe(1) N(8) C(27) 141.2(3) . . . yes N(9) N(8) C(27) 103.6(3) . . . yes N(8) N(9) C(29) 113.3(3) . . . yes N(8) N(9) C(33) 120.4(3) . . . yes C(29) N(9) C(33) 126.3(4) . . . yes N(1) C(1) C(2) 177.9(5) . . . yes S(1) C(3) C(4) 107.3(4) . . . yes S(1) C(3) C(12) 111.1(5) . . . yes S(1) C(3) C(13) 108.2(5) . . . yes C(4) C(3) C(12) 108.2(6) . . . yes C(4) C(3) C(13) 112.7(6) . . . yes C(12) C(3) C(13) 109.4(6) . . . yes N(2) C(4) C(3) 116.4(5) . . . yes N(2) C(6) C(7) 115.3(4) . . . yes C(6) C(7) C(8) 111.5(4) . . . yes N(3) C(8) C(7) 115.0(4) . . . yes N(3) C(10) C(11) 116.5(4) . . . yes S(2) C(11) C(10) 107.4(3) . . . yes S(2) C(11) C(14) 109.6(4) . . . yes S(2) C(11) C(15) 109.3(3) . . . yes C(10) C(11) C(14) 111.8(4) . . . yes C(10) C(11) C(15) 109.7(4) . . . yes C(14) C(11) C(15) 109.0(4) . . . yes N(4) C(17) C(16) 121.4(4) . . . yes N(4) C(17) C(18) 110.9(4) . . . yes C(16) C(17) C(18) 127.6(4) . . . yes C(17) C(18) C(19) 106.8(4) . . . yes N(5) C(19) C(18) 105.8(4) . . . yes N(5) C(19) C(20) 123.7(4) . . . yes C(18) C(19) C(20) 130.5(4) . . . yes N(6) C(22) C(21) 121.0(4) . . . yes N(6) C(22) C(23) 110.9(4) . . . yes C(21) C(22) C(23) 128.0(4) . . . yes C(22) C(23) C(24) 106.9(4) . . . yes N(7) C(24) C(23) 105.6(4) . . . yes N(7) C(24) C(25) 122.7(4) . . . yes C(23) C(24) C(25) 131.6(4) . . . yes N(8) C(27) C(26) 122.6(4) . . . yes N(8) C(27) C(28) 110.9(4) . . . yes C(26) C(27) C(28) 126.5(4) . . . yes C(27) C(28) C(29) 107.1(4) . . . yes N(9) C(29) C(28) 105.2(4) . . . yes N(9) C(29) C(30) 121.9(4) . . . yes C(28) C(29) C(30) 132.9(4) . . . yes N(10) C(31) C(32) 178.2(7) . . . yes N(5) C(33) N(7) 112.2(4) . . . yes N(5) C(33) N(9) 111.8(3) . . . yes N(7) C(33) N(9) 111.1(4) . . . yes F(1) B(1) F(2) 110.3(7) . . . yes F(1) B(1) F(3) 115.4(8) . . . yes F(1) B(1) F(4) 108.8(6) . . . yes F(2) B(1) F(3) 103.5(6) . . . yes F(2) B(1) F(4) 109.8(6) . . . yes F(3) B(1) F(4) 108.9(7) . . . yes F(5) B(2) F(6) 111.3(5) . . . yes F(5) B(2) F(7) 111.0(4) . . . yes F(5) B(2) F(8) 108.2(4) . . . yes F(6) B(2) F(7) 108.9(4) . . . yes F(6) B(2) F(8) 107.2(4) . . . yes F(7) B(2) F(8) 110.2(5) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ni(1) S(1) Fe(1) S(2) 26.65(4) . . . . yes Ni(1) S(1) Fe(1) N(1) 112.1(1) . . . . yes Ni(1) S(1) Fe(1) N(4) 91.8(8) . . . . yes Ni(1) S(1) Fe(1) N(6) -163.2(1) . . . . yes Ni(1) S(1) Fe(1) N(8) -75.6(1) . . . . yes Ni(1) S(1) C(3) C(4) -6.6(5) . . . . yes Ni(1) S(1) C(3) C(12) 111.5(4) . . . . yes Ni(1) S(1) C(3) C(13) -128.4(5) . . . . yes Ni(1) S(2) Fe(1) S(1) -26.50(4) . . . . yes Ni(1) S(2) Fe(1) N(1) -113.3(1) . . . . yes Ni(1) S(2) Fe(1) N(4) 160.4(1) . . . . yes Ni(1) S(2) Fe(1) N(6) -76.9(5) . . . . yes Ni(1) S(2) Fe(1) N(8) 73.6(1) . . . . yes Ni(1) S(2) C(11) C(10) 5.5(3) . . . . yes Ni(1) S(2) C(11) C(14) 127.2(3) . . . . yes Ni(1) S(2) C(11) C(15) -113.4(3) . . . . yes Ni(1) N(2) C(4) C(3) 47.5(6) . . . . yes Ni(1) N(2) C(6) C(7) -47.6(5) . . . . yes Ni(1) N(3) C(8) C(7) 47.7(5) . . . . yes Ni(1) N(3) C(10) C(11) -45.7(4) . . . . yes Fe(1) S(1) Ni(1) S(2) -29.66(5) . . . . yes Fe(1) S(1) Ni(1) N(2) 152.6(1) . . . . yes Fe(1) S(1) Ni(1) N(3) -43.9(9) . . . . yes Fe(1) S(1) C(3) C(4) -110.7(5) . . . . yes Fe(1) S(1) C(3) C(12) 7.3(5) . . . . yes Fe(1) S(1) C(3) C(13) 127.5(5) . . . . yes Fe(1) S(2) Ni(1) S(1) 29.22(5) . . . . yes Fe(1) S(2) Ni(1) N(2) 46.2(10) . . . . yes Fe(1) S(2) Ni(1) N(3) -152.6(1) . . . . yes Fe(1) S(2) C(11) C(10) 108.9(3) . . . . yes Fe(1) S(2) C(11) C(14) -129.4(3) . . . . yes Fe(1) S(2) C(11) C(15) -10.0(4) . . . . yes Fe(1) N(1) C(1) C(2) 51(15) . . . . yes Fe(1) N(4) N(5) C(19) 179.9(3) . . . . yes Fe(1) N(4) N(5) C(33) 8.4(5) . . . . yes Fe(1) N(4) C(17) C(16) 1.5(7) . . . . yes Fe(1) N(4) C(17) C(18) 178.8(3) . . . . yes Fe(1) N(6) N(7) C(24) -163.6(3) . . . . yes Fe(1) N(6) N(7) C(33) 15.4(5) . . . . yes Fe(1) N(6) C(22) C(21) -23.7(7) . . . . yes Fe(1) N(6) C(22) C(23) 159.6(3) . . . . yes Fe(1) N(8) N(9) C(29) -175.4(3) . . . . yes Fe(1) N(8) N(9) C(33) 6.0(5) . . . . yes Fe(1) N(8) C(27) C(26) -6.2(8) . . . . yes Fe(1) N(8) C(27) C(28) 172.9(4) . . . . yes S(1) Ni(1) S(2) C(11) 158.5(2) . . . . yes S(1) Ni(1) N(2) C(4) -40.6(3) . . . . yes S(1) Ni(1) N(2) C(5) 79.7(3) . . . . yes S(1) Ni(1) N(2) C(6) -159.1(4) . . . . yes S(1) Ni(1) N(3) C(8) 173.4(8) . . . . yes S(1) Ni(1) N(3) C(9) -66(1) . . . . yes S(1) Ni(1) N(3) C(10) 52(1) . . . . yes S(1) Fe(1) S(2) C(11) -134.1(2) . . . . yes S(1) Fe(1) N(1) C(1) 19(3) . . . . yes S(1) Fe(1) N(4) N(5) 145.1(6) . . . . yes S(1) Fe(1) N(4) C(17) -31(1) . . . . yes S(1) Fe(1) N(6) N(7) 135.8(3) . . . . yes S(1) Fe(1) N(6) C(22) -23.1(5) . . . . yes S(1) Fe(1) N(8) N(9) -141.6(3) . . . . yes S(1) Fe(1) N(8) C(27) 46.0(5) . . . . yes S(1) C(3) C(4) N(2) -24.7(7) . . . . yes S(2) Ni(1) S(1) C(3) -157.6(3) . . . . yes S(2) Ni(1) N(2) C(4) -57(1) . . . . yes S(2) Ni(1) N(2) C(5) 62(1) . . . . yes S(2) Ni(1) N(2) C(6) -176.1(8) . . . . yes S(2) Ni(1) N(3) C(8) 159.1(3) . . . . yes S(2) Ni(1) N(3) C(9) -81.1(3) . . . . yes S(2) Ni(1) N(3) C(10) 38.6(3) . . . . yes S(2) Fe(1) S(1) C(3) 134.6(2) . . . . yes S(2) Fe(1) N(1) C(1) 92(3) . . . . yes S(2) Fe(1) N(4) N(5) -151.6(3) . . . . yes S(2) Fe(1) N(4) C(17) 31.6(5) . . . . yes S(2) Fe(1) N(6) N(7) -176.0(3) . . . . yes S(2) Fe(1) N(6) C(22) 25.0(8) . . . . yes S(2) Fe(1) N(8) N(9) 142.8(3) . . . . yes S(2) Fe(1) N(8) C(27) -29.7(5) . . . . yes S(2) C(11) C(10) N(3) 23.9(5) . . . . yes N(1) Fe(1) S(1) C(3) -139.9(2) . . . . yes N(1) Fe(1) S(2) C(11) 139.0(2) . . . . yes N(1) Fe(1) N(4) N(5) 124.8(3) . . . . yes N(1) Fe(1) N(4) C(17) -52.0(4) . . . . yes N(1) Fe(1) N(6) N(7) -139.7(3) . . . . yes N(1) Fe(1) N(6) C(22) 61.4(4) . . . . yes N(1) Fe(1) N(8) N(9) -2.0(8) . . . . yes N(1) Fe(1) N(8) C(27) -174.5(6) . . . . yes N(2) Ni(1) S(1) C(3) 24.7(3) . . . . yes N(2) Ni(1) S(2) C(11) 175.5(10) . . . . yes N(2) Ni(1) N(3) C(8) -23.5(4) . . . . yes N(2) Ni(1) N(3) C(9) 96.3(3) . . . . yes N(2) Ni(1) N(3) C(10) -144.0(3) . . . . yes N(2) C(4) C(3) C(12) -144.6(5) . . . . yes N(2) C(4) C(3) C(13) 94.3(7) . . . . yes N(2) C(6) C(7) C(8) 70.8(6) . . . . yes N(3) Ni(1) S(1) C(3) -171.9(10) . . . . yes N(3) Ni(1) S(2) C(11) -23.3(2) . . . . yes N(3) Ni(1) N(2) C(4) 141.5(3) . . . . yes N(3) Ni(1) N(2) C(5) -98.2(4) . . . . yes N(3) Ni(1) N(2) C(6) 23.0(4) . . . . yes N(3) C(8) C(7) C(6) -71.0(5) . . . . yes N(3) C(10) C(11) C(14) -96.3(5) . . . . yes N(3) C(10) C(11) C(15) 142.6(4) . . . . yes N(4) Fe(1) S(1) C(3) -160.2(8) . . . . yes N(4) Fe(1) S(2) C(11) 52.8(2) . . . . yes N(4) Fe(1) N(1) C(1) -162(3) . . . . yes N(4) Fe(1) N(6) N(7) -51.4(3) . . . . yes N(4) Fe(1) N(6) C(22) 149.7(5) . . . . yes N(4) Fe(1) N(8) N(9) 40.1(3) . . . . yes N(4) Fe(1) N(8) C(27) -132.4(5) . . . . yes N(4) N(5) C(19) C(18) 1.9(5) . . . . yes N(4) N(5) C(19) C(20) -178.6(4) . . . . yes N(4) N(5) C(33) N(7) -67.1(5) . . . . yes N(4) N(5) C(33) N(9) 58.5(5) . . . . yes N(4) C(17) C(18) C(19) -0.7(5) . . . . yes N(5) N(4) Fe(1) N(6) 39.1(3) . . . . yes N(5) N(4) Fe(1) N(8) -47.2(3) . . . . yes N(5) N(4) C(17) C(16) -175.5(4) . . . . yes N(5) N(4) C(17) C(18) 1.7(5) . . . . yes N(5) C(19) C(18) C(17) -0.7(5) . . . . yes N(5) C(33) N(7) N(6) 51.6(5) . . . . yes N(5) C(33) N(7) C(24) -129.6(4) . . . . yes N(5) C(33) N(9) N(8) -66.9(5) . . . . yes N(5) C(33) N(9) C(29) 114.7(5) . . . . yes N(6) Fe(1) S(1) C(3) -55.3(2) . . . . yes N(6) Fe(1) S(2) C(11) 175.5(5) . . . . yes N(6) Fe(1) N(1) C(1) -79(3) . . . . yes N(6) Fe(1) N(4) C(17) -137.7(5) . . . . yes N(6) Fe(1) N(8) N(9) -43.5(3) . . . . yes N(6) Fe(1) N(8) C(27) 144.0(5) . . . . yes N(6) N(7) C(24) C(23) -2.3(5) . . . . yes N(6) N(7) C(24) C(25) 176.9(4) . . . . yes N(6) N(7) C(33) N(9) -74.3(5) . . . . yes N(6) C(22) C(23) C(24) -0.5(5) . . . . yes N(7) N(6) Fe(1) N(8) 32.5(3) . . . . yes N(7) N(6) C(22) C(21) 175.9(4) . . . . yes N(7) N(6) C(22) C(23) -0.9(5) . . . . yes N(7) C(24) C(23) C(22) 1.7(5) . . . . yes N(7) C(33) N(5) C(19) 122.9(4) . . . . yes N(7) C(33) N(9) N(8) 59.3(5) . . . . yes N(7) C(33) N(9) C(29) -119.1(4) . . . . yes N(8) Fe(1) S(1) C(3) 32.3(2) . . . . yes N(8) Fe(1) S(2) C(11) -34.1(2) . . . . yes N(8) Fe(1) N(1) C(1) -120(3) . . . . yes N(8) Fe(1) N(4) C(17) 136.0(5) . . . . yes N(8) Fe(1) N(6) C(22) -126.5(5) . . . . yes N(8) N(9) C(29) C(28) 0.4(5) . . . . yes N(8) N(9) C(29) C(30) 179.0(4) . . . . yes N(8) C(27) C(28) C(29) 0.4(6) . . . . yes N(9) N(8) C(27) C(26) -179.2(4) . . . . yes N(9) N(8) C(27) C(28) -0.1(5) . . . . yes N(9) C(29) C(28) C(27) -0.5(5) . . . . yes N(9) C(33) N(5) C(19) -111.5(5) . . . . yes N(9) C(33) N(7) C(24) 104.5(5) . . . . yes C(3) C(4) N(2) C(5) -69.3(6) . . . . yes C(3) C(4) N(2) C(6) 172.7(5) . . . . yes C(4) N(2) C(6) C(7) -167.6(5) . . . . yes C(5) N(2) C(6) C(7) 72.3(6) . . . . yes C(7) C(8) N(3) C(9) -71.4(5) . . . . yes C(7) C(8) N(3) C(10) 169.8(4) . . . . yes C(8) N(3) C(10) C(11) -172.4(4) . . . . yes C(9) N(3) C(10) C(11) 71.1(5) . . . . yes C(16) C(17) C(18) C(19) 176.4(4) . . . . yes C(17) N(4) N(5) C(19) -2.3(5) . . . . yes C(17) N(4) N(5) C(33) -173.8(4) . . . . yes C(17) C(18) C(19) C(20) 179.8(5) . . . . yes C(18) C(19) N(5) C(33) 172.6(4) . . . . yes C(20) C(19) N(5) C(33) -7.9(7) . . . . yes C(21) C(22) C(23) C(24) -176.9(5) . . . . yes C(22) N(6) N(7) C(24) 2.0(5) . . . . yes C(22) N(6) N(7) C(33) -179.0(4) . . . . yes C(22) C(23) C(24) C(25) -177.5(5) . . . . yes C(23) C(24) N(7) C(33) 178.8(4) . . . . yes C(25) C(24) N(7) C(33) -2.0(7) . . . . yes C(26) C(27) C(28) C(29) 179.4(5) . . . . yes C(27) N(8) N(9) C(29) -0.2(5) . . . . yes C(27) N(8) N(9) C(33) -178.8(4) . . . . yes C(27) C(28) C(29) C(30) -178.8(5) . . . . yes C(28) C(29) N(9) C(33) 178.9(4) . . . . yes C(30) C(29) N(9) C(33) -2.5(7) . . . . yes C(30) C(29) N(9) C(33) -2.5(7) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag F(1) C(6) 3.077(7) . 4_564 ? F(1) C(15) 3.277(6) . 7_555 ? F(1) C(10) 3.392(7) . 7_555 ? F(1) C(7) 3.499(8) . 4_564 ? F(2) C(25) 3.522(6) . 3_665 ? F(2) C(6) 3.543(8) . 4_564 ? F(2) C(9) 3.580(8) . 7_565 ? F(3) C(2) 3.257(7) . . ? F(3) C(25) 3.500(8) . 3_665 ? F(3) C(23) 3.542(7) . 3_665 ? F(3) C(18) 3.562(9) . 1_565 ? F(4) C(32) 3.347(8) . 7_555 ? F(4) C(16) 3.519(7) . 1_565 ? F(5) C(28) 3.295(5) . 4_554 ? F(5) C(25) 3.482(6) . 3_655 ? F(5) C(30) 3.571(6) . 3_655 ? F(6) C(30) 3.248(6) . 3_655 ? F(6) C(21) 3.275(6) . 3_665 ? F(6) C(13) 3.399(8) . 4_564 ? F(6) C(4) 3.488(6) . 4_564 ? F(6) C(23) 3.525(6) . 3_665 ? F(7) C(20) 3.243(6) . 3_655 ? F(7) C(30) 3.461(6) . 3_655 ? F(7) C(25) 3.474(7) . 3_655 ? F(7) C(2) 3.479(7) . . ? F(7) C(1) 3.500(6) . . ? F(7) C(16) 3.559(6) . . ? F(8) C(2) 3.178(6) . . ? F(8) C(8) 3.411(6) . 7_555 ? F(8) C(9) 3.420(7) . 7_555 ? F(8) C(10) 3.454(5) . 7_555 ? N(5) N(10) 3.362(6) . . ? N(9) N(10) 3.464(6) . . ? N(10) C(19) 3.140(7) . . ? N(10) C(29) 3.381(7) . . ? N(10) C(18) 3.461(7) . . ? N(10) C(20) 3.500(7) . . ? N(10) C(30) 3.586(7) . . ? C(9) C(16) 3.359(6) . 7_555 ? C(12) C(12) 3.51(1) . 2_655 ? C(13) C(30) 3.395(8) . 1_565 ? C(13) C(28) 3.59(1) . 1_565 ? C(18) C(24) 3.415(6) . 3_655 ? C(18) C(25) 3.500(6) . 3_655 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ # Attachment 'CIF_NiRu' data__NiRu2 _database_code_depnum_ccdc_archive 'CCDC 707321' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C25 H44 N6 Ni O6 Ru S2' _chemical_formula_moiety ? _chemical_formula_weight 748.55 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _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 10.163(1) _cell_length_b 10.299(1) _cell_length_c 16.887(3) _cell_angle_alpha 72.521(4) _cell_angle_beta 87.063(6) _cell_angle_gamma 67.188(5) _cell_volume 1549.7(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4980 _cell_measurement_theta_min 3.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.2 #------------------------------------------------------------------------------ _exptl_crystal_description Prism _exptl_crystal_colour Red _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.604 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 776.00 _exptl_absorpt_coefficient_mu 1.278 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(Higashi, 1999)' _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.942 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Saturn CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 28.57 _diffrn_reflns_number 12658 _diffrn_reflns_av_R_equivalents 0.025 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9637 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9637 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 19 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement was carried out using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6824 _reflns_number_gt 5442 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0655 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 6824 _refine_ls_number_parameters 370 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.02800(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0013 _refine_diff_density_max 0.82 _refine_diff_density_min -0.59 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? 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 for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; O O 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; Ru Ru -1.259 0.836 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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 Ru(1) Ru 0.98553(2) -0.11004(2) 0.74193(1) 0.01219(5) Uani 1.00 1 d . . . Ni(1) Ni 0.68997(3) 0.13560(3) 0.76106(2) 0.01240(7) Uani 1.00 1 d . . . S(1) S 0.85835(6) -0.02926(7) 0.85381(4) 0.0147(1) Uani 1.00 1 d . . . S(2) S 0.73393(6) -0.05365(7) 0.71688(4) 0.0147(1) Uani 1.00 1 d . . . O(1) O 1.2369(2) 0.0823(3) 0.9287(1) 0.0370(6) Uani 1.00 1 d . . . O(2) O 1.1571(2) 0.1968(2) 0.7993(1) 0.0285(5) Uani 1.00 1 d . . . O(3) O 1.2617(2) 0.2880(2) 0.8635(1) 0.0342(6) Uani 1.00 1 d . . . O(4) O 0.7045(2) -0.1765(3) 0.4906(1) 0.0358(6) Uani 1.00 1 d . . . O(5) O 0.7258(2) -0.4051(3) 0.5258(1) 0.0413(6) Uani 1.00 1 d . . . O(6) O 0.6017(3) -0.2615(3) 0.5971(2) 0.0645(10) Uani 1.00 1 d . . . N(1) N 0.9702(2) 0.1005(2) 0.6781(1) 0.0149(5) Uani 1.00 1 d . . . N(2) N 0.6820(2) 0.2848(2) 0.8138(1) 0.0150(5) Uani 1.00 1 d . . . N(3) N 0.5504(2) 0.2591(2) 0.6644(1) 0.0158(5) Uani 1.00 1 d . . . N(4) N 0.3451(3) 0.4128(4) 1.0746(2) 0.0497(9) Uani 1.00 1 d . . . N(5) N 1.2185(2) 0.1895(3) 0.8639(1) 0.0219(6) Uani 1.00 1 d . . . N(6) N 0.6794(2) -0.2815(3) 0.5391(1) 0.0286(7) Uani 1.00 1 d . . . C(1) C 0.9920(2) 0.2040(3) 0.6468(1) 0.0153(6) Uani 1.00 1 d . . . C(2) C 1.0232(3) 0.3348(3) 0.6099(2) 0.0213(6) Uani 1.00 1 d . . . C(3) C 0.9080(3) 0.0912(3) 0.8950(1) 0.0178(6) Uani 1.00 1 d . . . C(4) C 0.8328(3) 0.2505(3) 0.8427(2) 0.0187(6) Uani 1.00 1 d . . . C(5) C 0.5952(3) 0.2694(3) 0.8873(2) 0.0228(7) Uani 1.00 1 d . . . C(6) C 0.6236(3) 0.4428(3) 0.7602(2) 0.0218(7) Uani 1.00 1 d . . . C(7) C 0.4864(3) 0.4876(3) 0.7093(2) 0.0240(7) Uani 1.00 1 d . . . C(8) C 0.5132(3) 0.4215(3) 0.6378(2) 0.0215(6) Uani 1.00 1 d . . . C(9) C 0.4154(3) 0.2332(3) 0.6837(2) 0.0220(7) Uani 1.00 1 d . . . C(10) C 0.6140(3) 0.2070(3) 0.5921(1) 0.0180(6) Uani 1.00 1 d . . . C(11) C 0.6527(3) 0.0430(3) 0.6103(1) 0.0196(6) Uani 1.00 1 d . . . C(12) C 1.1688(2) -0.2000(3) 0.6700(1) 0.0166(6) Uani 1.00 1 d . . . C(13) C 1.0785(3) -0.2765(3) 0.6733(1) 0.0165(6) Uani 1.00 1 d . . . C(14) C 1.0360(3) -0.3434(3) 0.7526(2) 0.0164(6) Uani 1.00 1 d . . . C(15) C 1.0897(3) -0.3385(3) 0.8270(1) 0.0167(6) Uani 1.00 1 d . . . C(16) C 1.1827(2) -0.2617(3) 0.8234(1) 0.0168(6) Uani 1.00 1 d . . . C(17) C 1.2246(2) -0.1942(3) 0.7454(2) 0.0165(6) Uani 1.00 1 d . . . C(18) C 1.2094(3) -0.1228(3) 0.5872(2) 0.0262(7) Uani 1.00 1 d . . . C(19) C 1.0291(3) -0.2916(3) 0.5945(2) 0.0276(7) Uani 1.00 1 d . . . C(20) C 0.9347(3) -0.4197(3) 0.7574(2) 0.0261(7) Uani 1.00 1 d . . . C(21) C 1.0509(3) -0.4146(3) 0.9101(2) 0.0248(7) Uani 1.00 1 d . . . C(22) C 1.2357(3) -0.2515(3) 0.9022(2) 0.0261(7) Uani 1.00 1 d . . . C(23) C 1.3250(3) -0.1167(3) 0.7406(2) 0.0258(7) Uani 1.00 1 d . . . C(24) C 0.3821(3) 0.2965(4) 1.0703(2) 0.0293(8) Uani 1.00 1 d . . . C(25) C 0.4284(3) 0.1479(4) 1.0650(2) 0.0292(8) Uani 1.00 1 d . . . H(1) H 1.0645 0.3546 0.6519 0.0255 Uiso 1.00 1 calc . . . H(2) H 1.0882 0.3186 0.5682 0.0255 Uiso 1.00 1 calc . . . H(3) H 0.9369 0.4169 0.5859 0.0255 Uiso 1.00 1 calc . . . H(4) H 1.0086 0.0639 0.8944 0.0213 Uiso 1.00 1 calc . . . H(5) H 0.8812 0.0806 0.9506 0.0213 Uiso 1.00 1 calc . . . H(6) H 0.8850 0.2693 0.7952 0.0225 Uiso 1.00 1 calc . . . H(7) H 0.8304 0.3127 0.8748 0.0225 Uiso 1.00 1 calc . . . H(8) H 0.6312 0.1690 0.9214 0.0275 Uiso 1.00 1 calc . . . H(9) H 0.6009 0.3302 0.9185 0.0275 Uiso 1.00 1 calc . . . H(10) H 0.4982 0.2987 0.8690 0.0275 Uiso 1.00 1 calc . . . H(11) H 0.6934 0.4577 0.7231 0.0262 Uiso 1.00 1 calc . . . H(12) H 0.6057 0.5041 0.7950 0.0262 Uiso 1.00 1 calc . . . H(13) H 0.4224 0.4541 0.7443 0.0292 Uiso 1.00 1 calc . . . H(14) H 0.4445 0.5923 0.6873 0.0292 Uiso 1.00 1 calc . . . H(15) H 0.5902 0.4401 0.6092 0.0261 Uiso 1.00 1 calc . . . H(16) H 0.4293 0.4689 0.6010 0.0261 Uiso 1.00 1 calc . . . H(17) H 0.4370 0.1300 0.7005 0.0264 Uiso 1.00 1 calc . . . H(18) H 0.3733 0.2723 0.7274 0.0264 Uiso 1.00 1 calc . . . H(19) H 0.3505 0.2809 0.6356 0.0264 Uiso 1.00 1 calc . . . H(20) H 0.5464 0.2592 0.5451 0.0216 Uiso 1.00 1 calc . . . H(21) H 0.6979 0.2267 0.5801 0.0216 Uiso 1.00 1 calc . . . H(22) H 0.5686 0.0263 0.6046 0.0235 Uiso 1.00 1 calc . . . H(23) H 0.7185 0.0076 0.5724 0.0235 Uiso 1.00 1 calc . . . H(24) H 1.2998 -0.1849 0.5753 0.0314 Uiso 1.00 1 calc . . . H(25) H 1.2147 -0.0335 0.5901 0.0314 Uiso 1.00 1 calc . . . H(26) H 1.1391 -0.0991 0.5448 0.0314 Uiso 1.00 1 calc . . . H(27) H 1.0260 -0.3863 0.6059 0.0329 Uiso 1.00 1 calc . . . H(28) H 1.0938 -0.2799 0.5530 0.0329 Uiso 1.00 1 calc . . . H(29) H 0.9361 -0.2173 0.5753 0.0329 Uiso 1.00 1 calc . . . H(30) H 0.9856 -0.5161 0.7529 0.0314 Uiso 1.00 1 calc . . . H(31) H 0.8619 -0.3644 0.7132 0.0314 Uiso 1.00 1 calc . . . H(32) H 0.8921 -0.4267 0.8091 0.0314 Uiso 1.00 1 calc . . . H(33) H 1.1352 -0.4740 0.9461 0.0296 Uiso 1.00 1 calc . . . H(34) H 1.0048 -0.4753 0.9029 0.0296 Uiso 1.00 1 calc . . . H(35) H 0.9880 -0.3426 0.9338 0.0296 Uiso 1.00 1 calc . . . H(36) H 1.3135 -0.3411 0.9289 0.0311 Uiso 1.00 1 calc . . . H(37) H 1.2664 -0.1717 0.8889 0.0311 Uiso 1.00 1 calc . . . H(38) H 1.1604 -0.2347 0.9384 0.0311 Uiso 1.00 1 calc . . . H(39) H 1.3928 -0.1413 0.7011 0.0308 Uiso 1.00 1 calc . . . H(40) H 1.3736 -0.1473 0.7937 0.0308 Uiso 1.00 1 calc . . . H(41) H 1.2720 -0.0128 0.7240 0.0308 Uiso 1.00 1 calc . . . H(42) H 0.5278 0.0963 1.0815 0.0348 Uiso 1.00 1 calc . . . H(43) H 0.4118 0.1519 1.0093 0.0348 Uiso 1.00 1 calc . . . H(44) H 0.3763 0.0979 1.1007 0.0348 Uiso 1.00 1 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ru(1) 0.01378(10) 0.01096(10) 0.01165(9) -0.00490(7) 0.00156(7) -0.00319(7) Ni(1) 0.0124(1) 0.0138(2) 0.0117(1) -0.0053(1) 0.0012(1) -0.0047(1) S(1) 0.0149(3) 0.0161(3) 0.0125(3) -0.0053(2) 0.0017(2) -0.0048(2) S(2) 0.0154(3) 0.0157(3) 0.0151(3) -0.0074(2) 0.0017(2) -0.0059(2) O(1) 0.037(1) 0.039(1) 0.030(1) -0.018(1) -0.0071(9) 0.0014(10) O(2) 0.0246(10) 0.042(1) 0.0250(10) -0.0162(9) 0.0008(8) -0.0136(9) O(3) 0.036(1) 0.037(1) 0.046(1) -0.025(1) 0.0112(10) -0.023(1) O(4) 0.043(1) 0.035(1) 0.039(1) -0.024(1) 0.0108(10) -0.014(1) O(5) 0.031(1) 0.026(1) 0.056(1) -0.0060(10) -0.000(1) -0.005(1) O(6) 0.098(2) 0.072(2) 0.045(2) -0.052(2) 0.040(1) -0.028(1) N(1) 0.0143(10) 0.013(1) 0.0171(10) -0.0043(8) 0.0022(8) -0.0060(8) N(2) 0.0133(10) 0.016(1) 0.0169(10) -0.0053(8) 0.0033(8) -0.0076(8) N(3) 0.0147(10) 0.017(1) 0.0150(9) -0.0049(8) 0.0004(8) -0.0051(8) N(4) 0.057(2) 0.042(2) 0.044(2) -0.007(2) -0.015(1) -0.017(1) N(5) 0.015(1) 0.025(1) 0.027(1) -0.0071(9) 0.0045(9) -0.0118(10) N(6) 0.026(1) 0.034(1) 0.025(1) -0.015(1) -0.0043(10) -0.005(1) C(1) 0.013(1) 0.015(1) 0.017(1) -0.0043(9) 0.0014(9) -0.0044(10) C(2) 0.026(1) 0.016(1) 0.022(1) -0.011(1) 0.002(1) -0.003(1) C(3) 0.017(1) 0.022(1) 0.016(1) -0.007(1) -0.0008(9) -0.010(1) C(4) 0.018(1) 0.022(1) 0.021(1) -0.010(1) 0.0025(10) -0.010(1) C(5) 0.023(1) 0.028(2) 0.021(1) -0.010(1) 0.009(1) -0.014(1) C(6) 0.024(1) 0.016(1) 0.025(1) -0.006(1) 0.000(1) -0.008(1) C(7) 0.024(1) 0.016(1) 0.027(1) -0.002(1) -0.001(1) -0.007(1) C(8) 0.020(1) 0.019(1) 0.020(1) -0.005(1) -0.0040(10) -0.002(1) C(9) 0.014(1) 0.032(2) 0.024(1) -0.012(1) 0.0032(10) -0.011(1) C(10) 0.018(1) 0.021(1) 0.014(1) -0.006(1) 0.0015(9) -0.0058(10) C(11) 0.023(1) 0.023(1) 0.015(1) -0.009(1) 0.0009(10) -0.009(1) C(12) 0.015(1) 0.012(1) 0.017(1) -0.0004(9) 0.0051(9) -0.0038(10) C(13) 0.018(1) 0.011(1) 0.018(1) -0.0002(9) -0.0013(9) -0.0078(10) C(14) 0.017(1) 0.009(1) 0.021(1) -0.0031(9) 0.0015(9) -0.0053(10) C(15) 0.018(1) 0.010(1) 0.016(1) -0.0021(9) 0.0020(9) -0.0000(9) C(16) 0.016(1) 0.014(1) 0.015(1) -0.0000(10) -0.0051(9) -0.0037(9) C(17) 0.012(1) 0.012(1) 0.022(1) -0.0027(9) 0.0025(9) -0.0037(10) C(18) 0.025(1) 0.024(1) 0.023(1) -0.007(1) 0.008(1) -0.004(1) C(19) 0.042(2) 0.024(1) 0.020(1) -0.013(1) -0.001(1) -0.009(1) C(20) 0.029(1) 0.018(1) 0.037(2) -0.013(1) 0.002(1) -0.011(1) C(21) 0.030(1) 0.020(1) 0.020(1) -0.009(1) 0.003(1) -0.000(1) C(22) 0.025(1) 0.030(2) 0.020(1) -0.007(1) -0.006(1) -0.007(1) C(23) 0.019(1) 0.026(2) 0.039(2) -0.013(1) 0.006(1) -0.013(1) C(24) 0.023(1) 0.042(2) 0.024(1) -0.011(1) -0.001(1) -0.012(1) C(25) 0.031(2) 0.041(2) 0.024(1) -0.023(1) 0.007(1) -0.011(1) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 2.0' _computing_publication_material 'teXsan Ver. 2.0' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ru(1) S(1) 2.4069(6) . . yes Ru(1) S(2) 2.4220(7) . . yes Ru(1) N(1) 2.059(2) . . yes Ru(1) C(12) 2.215(2) . . yes Ru(1) C(13) 2.236(2) . . yes Ru(1) C(14) 2.206(2) . . yes Ru(1) C(15) 2.217(2) . . yes Ru(1) C(16) 2.216(2) . . yes Ru(1) C(17) 2.238(2) . . yes Ni(1) S(1) 2.1653(6) . . yes Ni(1) S(2) 2.1723(7) . . yes Ni(1) N(2) 1.970(2) . . yes Ni(1) N(3) 1.971(2) . . yes S(1) C(3) 1.821(3) . . yes S(2) C(11) 1.830(2) . . yes O(1) N(5) 1.259(3) . . yes O(2) N(5) 1.253(3) . . yes O(3) N(5) 1.250(3) . . yes O(4) N(6) 1.251(3) . . yes O(5) N(6) 1.260(3) . . yes O(6) N(6) 1.242(3) . . yes N(1) C(1) 1.139(3) . . yes N(2) C(4) 1.505(3) . . yes N(2) C(5) 1.490(3) . . yes N(2) C(6) 1.497(3) . . yes N(3) C(8) 1.489(3) . . yes N(3) C(9) 1.498(3) . . yes N(3) C(10) 1.497(3) . . yes N(4) C(24) 1.131(4) . . yes C(1) C(2) 1.452(3) . . yes C(3) C(4) 1.511(4) . . yes C(6) C(7) 1.511(4) . . yes C(7) C(8) 1.520(4) . . yes C(10) C(11) 1.512(4) . . yes C(12) C(13) 1.413(4) . . yes C(12) C(17) 1.446(3) . . yes C(12) C(18) 1.512(3) . . yes C(13) C(14) 1.438(3) . . yes C(13) C(19) 1.516(3) . . yes C(14) C(15) 1.418(3) . . yes C(14) C(20) 1.505(4) . . yes C(15) C(16) 1.437(4) . . yes C(15) C(21) 1.504(3) . . yes C(16) C(17) 1.422(3) . . yes C(16) C(22) 1.508(3) . . yes C(17) C(23) 1.505(3) . . yes C(24) C(25) 1.446(4) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S(1) Ru(1) S(2) 71.21(2) . . . yes S(1) Ru(1) N(1) 91.75(6) . . . yes S(1) Ru(1) C(12) 158.94(6) . . . yes S(1) Ru(1) C(13) 152.33(7) . . . yes S(1) Ru(1) C(14) 114.89(7) . . . yes S(1) Ru(1) C(15) 90.63(6) . . . yes S(1) Ru(1) C(16) 93.24(7) . . . yes S(1) Ru(1) C(17) 121.05(6) . . . yes S(2) Ru(1) N(1) 94.48(5) . . . yes S(2) Ru(1) C(12) 129.66(6) . . . yes S(2) Ru(1) C(13) 99.15(6) . . . yes S(2) Ru(1) C(14) 89.82(6) . . . yes S(2) Ru(1) C(15) 109.27(7) . . . yes S(2) Ru(1) C(16) 145.01(7) . . . yes S(2) Ru(1) C(17) 166.67(7) . . . yes N(1) Ru(1) C(12) 89.41(8) . . . yes N(1) Ru(1) C(13) 115.22(9) . . . yes N(1) Ru(1) C(14) 152.90(8) . . . yes N(1) Ru(1) C(15) 155.58(8) . . . yes N(1) Ru(1) C(16) 117.75(9) . . . yes N(1) Ru(1) C(17) 90.52(8) . . . yes C(12) Ru(1) C(13) 37.01(9) . . . yes C(12) Ru(1) C(14) 67.67(9) . . . yes C(12) Ru(1) C(15) 79.95(9) . . . yes C(12) Ru(1) C(16) 67.80(9) . . . yes C(12) Ru(1) C(17) 37.90(9) . . . yes C(13) Ru(1) C(14) 37.77(9) . . . yes C(13) Ru(1) C(15) 67.59(9) . . . yes C(13) Ru(1) C(16) 80.04(9) . . . yes C(13) Ru(1) C(17) 67.57(9) . . . yes C(14) Ru(1) C(15) 37.40(9) . . . yes C(14) Ru(1) C(16) 68.02(9) . . . yes C(14) Ru(1) C(17) 80.23(9) . . . yes C(15) Ru(1) C(16) 37.83(9) . . . yes C(15) Ru(1) C(17) 67.62(9) . . . yes C(16) Ru(1) C(17) 37.23(9) . . . yes S(1) Ni(1) S(2) 80.80(2) . . . yes S(1) Ni(1) N(2) 89.19(6) . . . yes S(1) Ni(1) N(3) 169.17(6) . . . yes S(2) Ni(1) N(2) 169.76(6) . . . yes S(2) Ni(1) N(3) 88.87(6) . . . yes N(2) Ni(1) N(3) 101.00(8) . . . yes Ru(1) S(1) Ni(1) 87.50(2) . . . yes Ru(1) S(1) C(3) 118.88(8) . . . yes Ni(1) S(1) C(3) 99.75(8) . . . yes Ru(1) S(2) Ni(1) 86.96(2) . . . yes Ru(1) S(2) C(11) 118.15(8) . . . yes Ni(1) S(2) C(11) 99.40(9) . . . yes Ru(1) N(1) C(1) 165.5(2) . . . yes Ni(1) N(2) C(4) 107.4(1) . . . yes Ni(1) N(2) C(5) 107.8(2) . . . yes Ni(1) N(2) C(6) 116.8(1) . . . yes C(4) N(2) C(5) 109.4(2) . . . yes C(4) N(2) C(6) 106.2(2) . . . yes C(5) N(2) C(6) 109.0(2) . . . yes Ni(1) N(3) C(8) 117.7(1) . . . yes Ni(1) N(3) C(9) 107.6(2) . . . yes Ni(1) N(3) C(10) 106.5(1) . . . yes C(8) N(3) C(9) 108.2(2) . . . yes C(8) N(3) C(10) 106.3(2) . . . yes C(9) N(3) C(10) 110.3(2) . . . yes O(1) N(5) O(2) 119.6(2) . . . yes O(1) N(5) O(3) 120.6(2) . . . yes O(2) N(5) O(3) 119.8(2) . . . yes O(4) N(6) O(5) 119.7(3) . . . yes O(4) N(6) O(6) 120.0(3) . . . yes O(5) N(6) O(6) 120.1(3) . . . yes N(1) C(1) C(2) 177.7(2) . . . yes S(1) C(3) C(4) 110.2(2) . . . yes N(2) C(4) C(3) 112.1(2) . . . yes N(2) C(6) C(7) 113.9(2) . . . yes C(6) C(7) C(8) 111.6(2) . . . yes N(3) C(8) C(7) 114.0(2) . . . yes N(3) C(10) C(11) 111.6(2) . . . yes S(2) C(11) C(10) 109.3(2) . . . yes Ru(1) C(12) C(13) 72.3(1) . . . yes Ru(1) C(12) C(17) 71.9(1) . . . yes Ru(1) C(12) C(18) 128.7(2) . . . yes C(13) C(12) C(17) 121.0(2) . . . yes C(13) C(12) C(18) 120.4(2) . . . yes C(17) C(12) C(18) 118.6(2) . . . yes Ru(1) C(13) C(12) 70.7(1) . . . yes Ru(1) C(13) C(14) 70.0(1) . . . yes Ru(1) C(13) C(19) 133.1(2) . . . yes C(12) C(13) C(14) 119.4(2) . . . yes C(12) C(13) C(19) 120.6(2) . . . yes C(14) C(13) C(19) 120.0(2) . . . yes Ru(1) C(14) C(13) 72.3(1) . . . yes Ru(1) C(14) C(15) 71.7(1) . . . yes Ru(1) C(14) C(20) 128.5(2) . . . yes C(13) C(14) C(15) 120.3(2) . . . yes C(13) C(14) C(20) 120.4(2) . . . yes C(15) C(14) C(20) 119.3(2) . . . yes Ru(1) C(15) C(14) 70.9(1) . . . yes Ru(1) C(15) C(16) 71.1(1) . . . yes Ru(1) C(15) C(21) 131.3(2) . . . yes C(14) C(15) C(16) 120.1(2) . . . yes C(14) C(15) C(21) 120.3(2) . . . yes C(16) C(15) C(21) 119.6(2) . . . yes Ru(1) C(16) C(15) 71.1(1) . . . yes Ru(1) C(16) C(17) 72.2(1) . . . yes Ru(1) C(16) C(22) 128.8(2) . . . yes C(15) C(16) C(17) 120.2(2) . . . yes C(15) C(16) C(22) 120.2(2) . . . yes C(17) C(16) C(22) 119.6(2) . . . yes Ru(1) C(17) C(12) 70.2(1) . . . yes Ru(1) C(17) C(16) 70.5(1) . . . yes Ru(1) C(17) C(23) 131.2(2) . . . yes C(12) C(17) C(16) 119.0(2) . . . yes C(12) C(17) C(23) 120.1(2) . . . yes C(16) C(17) C(23) 120.9(2) . . . yes N(4) C(24) C(25) 179.6(3) . . . yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Ru(1) S(1) Ni(1) S(2) 43.76(2) . . . . yes Ru(1) S(1) Ni(1) N(2) -134.09(6) . . . . yes Ru(1) S(1) Ni(1) N(3) 26.2(3) . . . . yes Ru(1) S(1) C(3) C(4) 84.2(2) . . . . yes Ru(1) S(2) Ni(1) S(1) -43.44(2) . . . . yes Ru(1) S(2) Ni(1) N(2) -31.3(3) . . . . yes Ru(1) S(2) Ni(1) N(3) 133.31(6) . . . . yes Ru(1) S(2) C(11) C(10) -81.8(2) . . . . yes Ru(1) N(1) C(1) C(2) -47(7) . . . . yes Ru(1) C(12) C(13) C(14) -52.1(2) . . . . yes Ru(1) C(12) C(13) C(19) 129.3(2) . . . . yes Ru(1) C(12) C(17) C(16) 52.8(2) . . . . yes Ru(1) C(12) C(17) C(23) -126.9(2) . . . . yes Ru(1) C(13) C(12) C(17) 55.2(2) . . . . yes Ru(1) C(13) C(12) C(18) -125.1(2) . . . . yes Ru(1) C(13) C(14) C(15) -55.4(2) . . . . yes Ru(1) C(13) C(14) C(20) 124.8(2) . . . . yes Ru(1) C(14) C(13) C(12) 52.4(2) . . . . yes Ru(1) C(14) C(13) C(19) -129.0(2) . . . . yes Ru(1) C(14) C(15) C(16) -53.3(2) . . . . yes Ru(1) C(14) C(15) C(21) 127.3(2) . . . . yes Ru(1) C(15) C(14) C(13) 55.6(2) . . . . yes Ru(1) C(15) C(14) C(20) -124.5(2) . . . . yes Ru(1) C(15) C(16) C(17) -55.1(2) . . . . yes Ru(1) C(15) C(16) C(22) 124.5(2) . . . . yes Ru(1) C(16) C(15) C(14) 53.2(2) . . . . yes Ru(1) C(16) C(15) C(21) -127.4(2) . . . . yes Ru(1) C(16) C(17) C(12) -52.6(2) . . . . yes Ru(1) C(16) C(17) C(23) 127.1(2) . . . . yes Ru(1) C(17) C(12) C(13) -55.4(2) . . . . yes Ru(1) C(17) C(12) C(18) 124.9(2) . . . . yes Ru(1) C(17) C(16) C(15) 54.5(2) . . . . yes Ru(1) C(17) C(16) C(22) -125.1(2) . . . . yes Ni(1) S(1) Ru(1) S(2) -40.31(2) . . . . yes Ni(1) S(1) Ru(1) N(1) 53.83(6) . . . . yes Ni(1) S(1) Ru(1) C(12) 146.7(2) . . . . yes Ni(1) S(1) Ru(1) C(13) -113.6(1) . . . . yes Ni(1) S(1) Ru(1) C(14) -121.01(7) . . . . yes Ni(1) S(1) Ru(1) C(15) -150.48(7) . . . . yes Ni(1) S(1) Ru(1) C(16) 171.76(7) . . . . yes Ni(1) S(1) Ru(1) C(17) 145.49(8) . . . . yes Ni(1) S(1) C(3) C(4) -8.3(2) . . . . yes Ni(1) S(2) Ru(1) S(1) 40.17(2) . . . . yes Ni(1) S(2) Ru(1) N(1) -50.15(6) . . . . yes Ni(1) S(2) Ru(1) C(12) -143.10(8) . . . . yes Ni(1) S(2) Ru(1) C(13) -166.60(7) . . . . yes Ni(1) S(2) Ru(1) C(14) 156.64(7) . . . . yes Ni(1) S(2) Ru(1) C(15) 124.05(7) . . . . yes Ni(1) S(2) Ru(1) C(16) 107.7(1) . . . . yes Ni(1) S(2) Ru(1) C(17) -161.9(3) . . . . yes Ni(1) S(2) C(11) C(10) 9.8(2) . . . . yes Ni(1) N(2) C(4) C(3) -51.9(2) . . . . yes Ni(1) N(2) C(6) C(7) 46.6(3) . . . . yes Ni(1) N(3) C(8) C(7) -44.5(3) . . . . yes Ni(1) N(3) C(10) C(11) 55.4(2) . . . . yes S(1) Ru(1) S(2) C(11) 139.2(1) . . . . yes S(1) Ru(1) N(1) C(1) 111.4(8) . . . . yes S(1) Ru(1) C(12) C(13) 130.5(2) . . . . yes S(1) Ru(1) C(12) C(17) -1.7(3) . . . . yes S(1) Ru(1) C(12) C(18) -114.3(2) . . . . yes S(1) Ru(1) C(13) C(12) -144.0(1) . . . . yes S(1) Ru(1) C(13) C(14) -11.0(2) . . . . yes S(1) Ru(1) C(13) C(19) 101.8(3) . . . . yes S(1) Ru(1) C(14) C(13) 174.4(1) . . . . yes S(1) Ru(1) C(14) C(15) -54.1(1) . . . . yes S(1) Ru(1) C(14) C(20) 59.2(2) . . . . yes S(1) Ru(1) C(15) C(14) 132.7(1) . . . . yes S(1) Ru(1) C(15) C(16) -94.5(1) . . . . yes S(1) Ru(1) C(15) C(21) 18.8(2) . . . . yes S(1) Ru(1) C(16) C(15) 86.9(1) . . . . yes S(1) Ru(1) C(16) C(17) -141.2(1) . . . . yes S(1) Ru(1) C(16) C(22) -27.2(2) . . . . yes S(1) Ru(1) C(17) C(12) 179.3(1) . . . . yes S(1) Ru(1) C(17) C(16) 46.9(2) . . . . yes S(1) Ru(1) C(17) C(23) -67.6(2) . . . . yes S(1) Ni(1) S(2) C(11) -161.49(9) . . . . yes S(1) Ni(1) N(2) C(4) 37.1(1) . . . . yes S(1) Ni(1) N(2) C(5) -80.7(1) . . . . yes S(1) Ni(1) N(2) C(6) 156.2(2) . . . . yes S(1) Ni(1) N(3) C(8) -140.6(3) . . . . yes S(1) Ni(1) N(3) C(9) 96.8(4) . . . . yes S(1) Ni(1) N(3) C(10) -21.5(4) . . . . yes S(1) C(3) C(4) N(2) 38.2(2) . . . . yes S(2) Ru(1) S(1) C(3) -140.06(10) . . . . yes S(2) Ru(1) N(1) C(1) -177.3(8) . . . . yes S(2) Ru(1) C(12) C(13) -40.8(2) . . . . yes S(2) Ru(1) C(12) C(17) -173.1(1) . . . . yes S(2) Ru(1) C(12) C(18) 74.3(2) . . . . yes S(2) Ru(1) C(13) C(12) 149.3(1) . . . . yes S(2) Ru(1) C(13) C(14) -77.7(1) . . . . yes S(2) Ru(1) C(13) C(19) 35.1(3) . . . . yes S(2) Ru(1) C(14) C(13) 105.3(1) . . . . yes S(2) Ru(1) C(14) C(15) -123.2(1) . . . . yes S(2) Ru(1) C(14) C(20) -9.9(2) . . . . yes S(2) Ru(1) C(15) C(14) 62.4(1) . . . . yes S(2) Ru(1) C(15) C(16) -164.8(1) . . . . yes S(2) Ru(1) C(15) C(21) -51.5(2) . . . . yes S(2) Ru(1) C(16) C(15) 25.7(2) . . . . yes S(2) Ru(1) C(16) C(17) 157.6(1) . . . . yes S(2) Ru(1) C(16) C(22) -88.4(3) . . . . yes S(2) Ru(1) C(17) C(12) 23.8(4) . . . . yes S(2) Ru(1) C(17) C(16) -108.6(3) . . . . yes S(2) Ru(1) C(17) C(23) 136.9(2) . . . . yes S(2) Ni(1) S(1) C(3) 162.64(8) . . . . yes S(2) Ni(1) N(2) C(4) 25.1(4) . . . . yes S(2) Ni(1) N(2) C(5) -92.7(4) . . . . yes S(2) Ni(1) N(2) C(6) 144.2(3) . . . . yes S(2) Ni(1) N(3) C(8) -158.0(2) . . . . yes S(2) Ni(1) N(3) C(9) 79.5(2) . . . . yes S(2) Ni(1) N(3) C(10) -38.8(1) . . . . yes S(2) C(11) C(10) N(3) -41.5(2) . . . . yes N(1) Ru(1) S(1) C(3) -45.9(1) . . . . yes N(1) Ru(1) S(2) C(11) 48.9(1) . . . . yes N(1) Ru(1) C(12) C(13) -136.2(1) . . . . yes N(1) Ru(1) C(12) C(17) 91.6(1) . . . . yes N(1) Ru(1) C(12) C(18) -21.0(2) . . . . yes N(1) Ru(1) C(13) C(12) 49.9(2) . . . . yes N(1) Ru(1) C(13) C(14) -177.1(1) . . . . yes N(1) Ru(1) C(13) C(19) -64.3(3) . . . . yes N(1) Ru(1) C(14) C(13) 5.8(2) . . . . yes N(1) Ru(1) C(14) C(15) 137.3(2) . . . . yes N(1) Ru(1) C(14) C(20) -109.4(3) . . . . yes N(1) Ru(1) C(15) C(14) -131.6(2) . . . . yes N(1) Ru(1) C(15) C(16) 1.2(3) . . . . yes N(1) Ru(1) C(15) C(21) 114.4(3) . . . . yes N(1) Ru(1) C(16) C(15) -179.5(1) . . . . yes N(1) Ru(1) C(16) C(17) -47.5(2) . . . . yes N(1) Ru(1) C(16) C(22) 66.5(3) . . . . yes N(1) Ru(1) C(17) C(12) -88.4(1) . . . . yes N(1) Ru(1) C(17) C(16) 139.3(1) . . . . yes N(1) Ru(1) C(17) C(23) 24.7(2) . . . . yes N(2) Ni(1) S(1) C(3) -15.2(1) . . . . yes N(2) Ni(1) S(2) C(11) -149.3(4) . . . . yes N(2) Ni(1) N(3) C(8) 19.3(2) . . . . yes N(2) Ni(1) N(3) C(9) -103.2(2) . . . . yes N(2) Ni(1) N(3) C(10) 138.4(2) . . . . yes N(2) C(6) C(7) C(8) -72.9(3) . . . . yes N(3) Ni(1) S(1) C(3) 145.1(3) . . . . yes N(3) Ni(1) S(2) C(11) 15.3(1) . . . . yes N(3) Ni(1) N(2) C(4) -139.2(1) . . . . yes N(3) Ni(1) N(2) C(5) 103.0(2) . . . . yes N(3) Ni(1) N(2) C(6) -20.1(2) . . . . yes N(3) C(8) C(7) C(6) 71.6(3) . . . . yes C(1) N(1) Ru(1) C(12) -47.6(8) . . . . yes C(1) N(1) Ru(1) C(13) -75.0(8) . . . . yes C(1) N(1) Ru(1) C(14) -78.9(8) . . . . yes C(1) N(1) Ru(1) C(15) 16.0(9) . . . . yes C(1) N(1) Ru(1) C(16) 16.8(8) . . . . yes C(1) N(1) Ru(1) C(17) -9.7(8) . . . . yes C(3) S(1) Ru(1) C(12) 47.0(2) . . . . yes C(3) S(1) Ru(1) C(13) 146.6(2) . . . . yes C(3) S(1) Ru(1) C(14) 139.2(1) . . . . yes C(3) S(1) Ru(1) C(15) 109.8(1) . . . . yes C(3) S(1) Ru(1) C(16) 72.0(1) . . . . yes C(3) S(1) Ru(1) C(17) 45.7(1) . . . . yes C(3) C(4) N(2) C(5) 64.9(3) . . . . yes C(3) C(4) N(2) C(6) -177.6(2) . . . . yes C(4) N(2) C(6) C(7) 166.4(2) . . . . yes C(5) N(2) C(6) C(7) -75.8(3) . . . . yes C(7) C(8) N(3) C(9) 77.7(2) . . . . yes C(7) C(8) N(3) C(10) -163.7(2) . . . . yes C(8) N(3) C(10) C(11) -178.3(2) . . . . yes C(9) N(3) C(10) C(11) -61.1(3) . . . . yes C(11) S(2) Ru(1) C(12) -44.1(1) . . . . yes C(11) S(2) Ru(1) C(13) -67.6(1) . . . . yes C(11) S(2) Ru(1) C(14) -104.3(1) . . . . yes C(11) S(2) Ru(1) C(15) -136.9(1) . . . . yes C(11) S(2) Ru(1) C(16) -153.2(1) . . . . yes C(11) S(2) Ru(1) C(17) -62.8(3) . . . . yes C(12) Ru(1) C(13) C(14) 133.0(2) . . . . yes C(12) Ru(1) C(13) C(19) -114.2(3) . . . . yes C(12) Ru(1) C(14) C(13) -28.4(1) . . . . yes C(12) Ru(1) C(14) C(15) 103.1(2) . . . . yes C(12) Ru(1) C(14) C(20) -143.6(2) . . . . yes C(12) Ru(1) C(15) C(14) -66.2(1) . . . . yes C(12) Ru(1) C(15) C(16) 66.6(1) . . . . yes C(12) Ru(1) C(15) C(21) 179.8(2) . . . . yes C(12) Ru(1) C(16) C(15) -102.6(2) . . . . yes C(12) Ru(1) C(16) C(17) 29.4(1) . . . . yes C(12) Ru(1) C(16) C(22) 143.4(3) . . . . yes C(12) Ru(1) C(17) C(16) -132.4(2) . . . . yes C(12) Ru(1) C(17) C(23) 113.1(3) . . . . yes C(12) C(13) Ru(1) C(14) -133.0(2) . . . . yes C(12) C(13) Ru(1) C(15) -103.5(2) . . . . yes C(12) C(13) Ru(1) C(16) -66.2(1) . . . . yes C(12) C(13) Ru(1) C(17) -29.5(1) . . . . yes C(12) C(13) C(14) C(15) -2.9(3) . . . . yes C(12) C(13) C(14) C(20) 177.2(2) . . . . yes C(12) C(17) Ru(1) C(13) 28.8(1) . . . . yes C(12) C(17) Ru(1) C(14) 66.0(1) . . . . yes C(12) C(17) Ru(1) C(15) 102.8(2) . . . . yes C(12) C(17) Ru(1) C(16) 132.4(2) . . . . yes C(12) C(17) C(16) C(15) 1.9(3) . . . . yes C(12) C(17) C(16) C(22) -177.7(2) . . . . yes C(13) Ru(1) C(12) C(17) -132.2(2) . . . . yes C(13) Ru(1) C(12) C(18) 115.2(3) . . . . yes C(13) Ru(1) C(14) C(15) 131.5(2) . . . . yes C(13) Ru(1) C(14) C(20) -115.2(3) . . . . yes C(13) Ru(1) C(15) C(14) -29.7(1) . . . . yes C(13) Ru(1) C(15) C(16) 103.1(2) . . . . yes C(13) Ru(1) C(15) C(21) -143.7(3) . . . . yes C(13) Ru(1) C(16) C(15) -66.1(1) . . . . yes C(13) Ru(1) C(16) C(17) 65.8(1) . . . . yes C(13) Ru(1) C(16) C(22) 179.9(3) . . . . yes C(13) Ru(1) C(17) C(16) -103.5(2) . . . . yes C(13) Ru(1) C(17) C(23) 141.9(3) . . . . yes C(13) C(12) Ru(1) C(14) 29.0(1) . . . . yes C(13) C(12) Ru(1) C(15) 65.9(1) . . . . yes C(13) C(12) Ru(1) C(16) 103.4(2) . . . . yes C(13) C(12) Ru(1) C(17) 132.2(2) . . . . yes C(13) C(12) C(17) C(16) -2.6(3) . . . . yes C(13) C(12) C(17) C(23) 177.8(2) . . . . yes C(13) C(14) Ru(1) C(15) -131.5(2) . . . . yes C(13) C(14) Ru(1) C(16) -102.5(1) . . . . yes C(13) C(14) Ru(1) C(17) -65.8(1) . . . . yes C(13) C(14) C(15) C(16) 2.3(3) . . . . yes C(13) C(14) C(15) C(21) -177.1(2) . . . . yes C(14) Ru(1) C(12) C(17) -103.2(2) . . . . yes C(14) Ru(1) C(12) C(18) 144.1(3) . . . . yes C(14) Ru(1) C(13) C(19) 112.8(3) . . . . yes C(14) Ru(1) C(15) C(16) 132.8(2) . . . . yes C(14) Ru(1) C(15) C(21) -113.9(3) . . . . yes C(14) Ru(1) C(16) C(15) -28.7(1) . . . . yes C(14) Ru(1) C(16) C(17) 103.2(2) . . . . yes C(14) Ru(1) C(16) C(22) -142.8(3) . . . . yes C(14) Ru(1) C(17) C(16) -66.3(1) . . . . yes C(14) Ru(1) C(17) C(23) 179.1(3) . . . . yes C(14) C(13) Ru(1) C(15) 29.5(1) . . . . yes C(14) C(13) Ru(1) C(16) 66.8(1) . . . . yes C(14) C(13) Ru(1) C(17) 103.5(1) . . . . yes C(14) C(13) C(12) C(17) 3.1(3) . . . . yes C(14) C(13) C(12) C(18) -177.2(2) . . . . yes C(14) C(15) Ru(1) C(16) -132.8(2) . . . . yes C(14) C(15) Ru(1) C(17) -103.7(2) . . . . yes C(14) C(15) C(16) C(17) -1.8(3) . . . . yes C(14) C(15) C(16) C(22) 177.8(2) . . . . yes C(15) Ru(1) C(12) C(17) -66.3(1) . . . . yes C(15) Ru(1) C(12) C(18) -178.9(2) . . . . yes C(15) Ru(1) C(13) C(19) 142.3(3) . . . . yes C(15) Ru(1) C(14) C(20) 113.3(3) . . . . yes C(15) Ru(1) C(16) C(17) 132.0(2) . . . . yes C(15) Ru(1) C(16) C(22) -114.0(3) . . . . yes C(15) Ru(1) C(17) C(16) -29.6(1) . . . . yes C(15) Ru(1) C(17) C(23) -144.1(3) . . . . yes C(15) C(14) Ru(1) C(16) 29.0(1) . . . . yes C(15) C(14) Ru(1) C(17) 65.7(1) . . . . yes C(15) C(14) C(13) C(19) 175.7(2) . . . . yes C(15) C(16) Ru(1) C(17) -132.0(2) . . . . yes C(15) C(16) C(17) C(23) -178.4(2) . . . . yes C(16) Ru(1) C(12) C(17) -28.9(1) . . . . yes C(16) Ru(1) C(12) C(18) -141.5(3) . . . . yes C(16) Ru(1) C(13) C(19) 179.6(3) . . . . yes C(16) Ru(1) C(14) C(20) 142.3(2) . . . . yes C(16) Ru(1) C(15) C(21) 113.2(3) . . . . yes C(16) Ru(1) C(17) C(23) -114.5(3) . . . . yes C(16) C(15) Ru(1) C(17) 29.1(1) . . . . yes C(16) C(15) C(14) C(20) -177.9(2) . . . . yes C(16) C(17) C(12) C(18) 177.7(2) . . . . yes C(17) Ru(1) C(12) C(18) -112.6(3) . . . . yes C(17) Ru(1) C(13) C(19) -143.7(3) . . . . yes C(17) Ru(1) C(14) C(20) 179.0(2) . . . . yes C(17) Ru(1) C(15) C(21) 142.4(3) . . . . yes C(17) Ru(1) C(16) C(22) 114.0(3) . . . . yes C(17) C(12) C(13) C(19) -175.5(2) . . . . yes C(17) C(16) C(15) C(21) 177.6(2) . . . . yes C(18) C(12) C(13) C(19) 4.2(3) . . . . yes C(18) C(12) C(17) C(23) -2.0(3) . . . . yes C(19) C(13) C(14) C(20) -4.2(3) . . . . yes C(20) C(14) C(15) C(21) 2.7(3) . . . . yes C(21) C(15) C(16) C(22) -2.8(3) . . . . yes C(22) C(16) C(17) C(23) 2.0(3) . . . . yes C(22) C(16) C(17) C(23) 2.0(3) . . . . yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) C(25) 3.291(4) . 2_757 ? O(1) C(3) 3.382(3) . . ? O(1) C(25) 3.458(3) . 1_655 ? O(1) C(3) 3.553(3) . 2_757 ? O(2) C(1) 3.112(3) . . ? O(2) C(4) 3.207(3) . . ? O(2) C(2) 3.211(3) . . ? O(2) C(9) 3.262(3) . 1_655 ? O(2) C(3) 3.296(3) . . ? O(2) C(23) 3.434(4) . . ? O(2) N(1) 3.444(3) . . ? O(2) C(20) 3.575(4) . 1_565 ? O(3) C(21) 3.283(4) . 1_565 ? O(3) C(5) 3.358(3) . 1_655 ? O(3) C(15) 3.421(3) . 1_565 ? O(3) C(9) 3.440(3) . 1_655 ? O(3) C(25) 3.505(4) . 1_655 ? O(3) C(14) 3.549(3) . 1_565 ? O(3) C(20) 3.596(4) . 1_565 ? O(4) C(2) 3.299(4) . 2_756 ? O(4) C(11) 3.345(3) . . ? O(4) C(18) 3.396(4) . 2_756 ? O(4) C(19) 3.417(4) . . ? O(4) C(9) 3.527(3) . 2_656 ? O(5) C(2) 3.194(3) . 1_545 ? O(5) C(8) 3.462(4) . 1_545 ? O(5) C(2) 3.481(4) . 2_756 ? O(5) C(9) 3.534(3) . 2_656 ? O(5) C(10) 3.585(3) . 2_656 ? O(6) C(7) 3.289(4) . 1_545 ? O(6) C(6) 3.377(4) . 1_545 ? O(6) C(11) 3.442(4) . . ? O(6) C(8) 3.579(4) . 1_545 ? N(5) C(9) 3.567(3) . 1_655 ? N(6) C(10) 3.503(3) . 2_656 ? C(5) C(25) 3.509(4) . . ? C(7) C(12) 3.478(4) . 1_465 ? C(7) C(17) 3.531(4) . 1_465 ? C(11) C(18) 3.541(4) . 2_756 ? C(21) C(21) 3.356(5) . 2_747 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------