# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_A_TEXRAY.INF_file_is_not_p _database_code_depnum_ccdc_archive 'CCDC 645114' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H6 I2 N Ni2 S20 ' _chemical_formula_moiety '2(C6 Ni S10), C6 H6 I2 N ' _chemical_formula_weight 1248.66 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' _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 14.3470(7) _cell_length_b 6.4710(3) _cell_length_c 76.540(3) _cell_angle_alpha 90 _cell_angle_beta 92.998(4) _cell_angle_gamma 90 _cell_volume 7096.2(6) _cell_formula_units_Z 8 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature 297.0 #------------------------------------------------------------------------------ _exptl_crystal_description 'hexagonal plate' _exptl_crystal_colour black _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.050 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.337 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4824.00 _exptl_absorpt_coefficient_mu 3.999 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.896 _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_process_details DIP320 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type DIP320 _diffrn_measurement_method \w _diffrn_reflns_number 8552 _diffrn_reflns_av_R_equivalents 0.062 _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 28.30 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -101 _diffrn_reflns_limit_l_max 101 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_max 0.89 _diffrn_measured_fraction_theta_full 0.97 #------------------------------------------------------------------------------ # 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 8552 _reflns_number_gt 6205 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0635 _refine_ls_wR_factor_ref 0.1857 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 8552 _refine_ls_number_parameters 388 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0050 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 2.11 _refine_diff_density_min -1.07 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 I(1) I 0.48889(3) 0.30055(8) 0.66507(1) 0.0501(2) Uani 1.00 1 d . . . I(2) I 0.34586(4) 1.05377(9) 0.62238(1) 0.0679(2) Uani 1.00 1 d . . . Ni(1) Ni 0.35560(6) 0.1928(1) 0.51122(1) 0.0388(2) Uani 1.00 1 d . . . Ni(2) Ni 0.32830(6) 0.1797(1) 0.72633(1) 0.0348(2) Uani 1.00 1 d . . . S(1) S 0.3101(1) 0.0203(3) 0.53363(2) 0.0482(4) Uani 1.00 1 d . . . S(2) S 0.3633(2) 0.4815(3) 0.52545(2) 0.0500(4) Uani 1.00 1 d . . . S(3) S 0.3568(2) -0.0948(3) 0.49672(2) 0.0524(5) Uani 1.00 1 d . . . S(4) S 0.4020(2) 0.3686(3) 0.48933(2) 0.0520(5) Uani 1.00 1 d . . . S(5) S 0.2746(2) 0.1629(3) 0.57058(2) 0.0515(4) Uani 1.00 1 d . . . S(6) S 0.3253(2) 0.5836(3) 0.56301(2) 0.0560(5) Uani 1.00 1 d . . . S(7) S 0.4136(2) -0.1890(3) 0.45999(2) 0.0517(4) Uani 1.00 1 d . . . S(8) S 0.4549(2) 0.2407(3) 0.45331(2) 0.0510(4) Uani 1.00 1 d . . . S(9) S 0.2653(2) 0.4837(3) 0.59854(2) 0.0598(5) Uani 1.00 1 d . . . S(10) S 0.4785(2) -0.0673(4) 0.42519(2) 0.0610(5) Uani 1.00 1 d . . . S(11) S 0.3491(1) -0.1147(2) 0.73930(2) 0.0413(4) Uani 1.00 1 d . . . S(12) S 0.3753(1) 0.3503(2) 0.74953(2) 0.0425(4) Uani 1.00 1 d . . . S(13) S 0.2752(1) 0.0065(2) 0.70378(2) 0.0404(3) Uani 1.00 1 d . . . S(14) S 0.3128(1) 0.4739(2) 0.71301(2) 0.0418(4) Uani 1.00 1 d . . . S(15) S 0.4260(1) -0.2251(3) 0.77563(2) 0.0431(4) Uani 1.00 1 d . . . S(16) S 0.4457(1) 0.2058(3) 0.78549(2) 0.0427(4) Uani 1.00 1 d . . . S(17) S 0.2121(1) 0.1465(3) 0.66727(2) 0.0426(4) Uani 1.00 1 d . . . S(18) S 0.2447(1) 0.5762(2) 0.67573(2) 0.0426(4) Uani 1.00 1 d . . . S(19) S 0.5036(1) -0.1204(3) 0.81110(2) 0.0503(4) Uani 1.00 1 d . . . S(20) S 0.1837(2) 0.4592(3) 0.63914(2) 0.0529(4) Uani 1.00 1 d . . . N(1) N 0.5389(4) 0.5640(9) 0.61540(7) 0.047(1) Uani 1.00 1 d . . . C(1) C 0.3068(5) 0.211(1) 0.54919(8) 0.040(1) Uani 1.00 1 d . . . C(2) C 0.3297(5) 0.409(1) 0.54561(8) 0.042(1) Uani 1.00 1 d . . . C(3) C 0.3964(5) -0.019(1) 0.47717(8) 0.040(1) Uani 1.00 1 d . . . C(4) C 0.4169(5) 0.185(1) 0.47402(7) 0.040(1) Uani 1.00 1 d . . . C(5) C 0.2871(5) 0.413(1) 0.57820(8) 0.044(1) Uani 1.00 1 d . . . C(6) C 0.4492(5) -0.007(1) 0.44517(8) 0.042(1) Uani 1.00 1 d . . . C(7) C 0.3916(4) -0.0469(9) 0.75957(7) 0.033(1) Uani 1.00 1 d . . . C(8) C 0.4016(4) 0.1608(9) 0.76408(8) 0.036(1) Uani 1.00 1 d . . . C(9) C 0.2530(4) 0.1972(9) 0.68867(7) 0.035(1) Uani 1.00 1 d . . . C(10) C 0.2688(5) 0.4024(10) 0.69272(8) 0.038(1) Uani 1.00 1 d . . . C(11) C 0.4585(5) -0.0491(10) 0.79173(8) 0.039(1) Uani 1.00 1 d . . . C(12) C 0.2113(5) 0.398(1) 0.65962(8) 0.040(1) Uani 1.00 1 d . . . C(13) C 0.5430(5) 0.451(1) 0.63026(9) 0.048(2) Uani 1.00 1 d . . . C(14) C 0.4873(5) 0.506(1) 0.64377(8) 0.045(1) Uani 1.00 1 d . . . C(15) C 0.4317(5) 0.679(1) 0.64239(9) 0.048(2) Uani 1.00 1 d . . . C(16) C 0.4292(5) 0.793(1) 0.62681(9) 0.046(2) Uani 1.00 1 d . . . C(17) C 0.4828(6) 0.734(1) 0.61345(9) 0.050(2) Uani 1.00 1 d . . . C(18) C 0.5932(7) 0.506(2) 0.6005(1) 0.069(2) Uani 1.00 1 d . . . H(1) H 0.5847 0.3355 0.6316 0.0574 Uiso 1.00 1 calc . . . H(2) H 0.3959 0.7229 0.6521 0.0585 Uiso 1.00 1 calc . . . H(3) H 0.4807 0.8096 0.6027 0.0610 Uiso 1.00 1 calc . . . H(4) H 0.6306 0.3850 0.6034 0.0828 Uiso 1.00 1 calc . . . H(5) H 0.5533 0.4740 0.5906 0.0828 Uiso 1.00 1 calc . . . H(6) H 0.6345 0.6145 0.5976 0.0828 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 I(1) 0.0570(3) 0.0458(3) 0.0473(3) -0.0003(2) 0.0003(2) 0.0130(2) I(2) 0.0828(4) 0.0385(3) 0.0796(4) 0.0145(3) -0.0230(3) -0.0021(2) Ni(1) 0.0559(5) 0.0283(4) 0.0331(4) -0.0011(3) 0.0087(3) 0.0008(3) Ni(2) 0.0458(5) 0.0246(4) 0.0339(4) 0.0017(3) 0.0001(3) -0.0019(3) S(1) 0.076(1) 0.0314(8) 0.0388(8) -0.0068(8) 0.0162(8) -0.0004(6) S(2) 0.085(1) 0.0309(8) 0.0355(8) -0.0075(8) 0.0143(8) 0.0012(6) S(3) 0.087(1) 0.0293(8) 0.0426(8) -0.0090(8) 0.0212(9) 0.0003(7) S(4) 0.092(1) 0.0264(8) 0.0385(8) -0.0049(8) 0.0182(9) 0.0000(6) S(5) 0.079(1) 0.0402(9) 0.0369(8) -0.0063(8) 0.0183(8) 0.0019(7) S(6) 0.098(1) 0.0346(9) 0.0372(8) -0.0011(9) 0.0143(9) -0.0019(7) S(7) 0.083(1) 0.0316(9) 0.0417(8) -0.0044(8) 0.0166(9) -0.0051(7) S(8) 0.084(1) 0.0343(9) 0.0365(8) -0.0043(8) 0.0156(8) 0.0017(6) S(9) 0.097(2) 0.049(1) 0.0353(8) 0.010(1) 0.0150(9) -0.0035(7) S(10) 0.090(1) 0.056(1) 0.0378(8) -0.002(1) 0.0149(9) -0.0076(8) S(11) 0.0606(10) 0.0255(7) 0.0374(7) -0.0069(7) -0.0027(7) -0.0015(6) S(12) 0.062(1) 0.0238(7) 0.0409(8) 0.0054(7) -0.0056(7) -0.0039(6) S(13) 0.0599(10) 0.0247(7) 0.0362(7) -0.0023(7) -0.0023(7) 0.0009(6) S(14) 0.0615(10) 0.0240(7) 0.0389(8) 0.0016(7) -0.0055(7) -0.0042(6) S(15) 0.065(1) 0.0262(7) 0.0374(7) -0.0051(7) -0.0008(7) 0.0013(6) S(16) 0.061(1) 0.0266(8) 0.0392(8) -0.0006(7) -0.0040(7) -0.0046(6) S(17) 0.061(1) 0.0304(8) 0.0354(7) -0.0029(7) -0.0032(7) -0.0022(6) S(18) 0.063(1) 0.0259(7) 0.0383(7) 0.0043(7) -0.0011(7) 0.0005(6) S(19) 0.070(1) 0.0437(10) 0.0361(8) 0.0012(8) -0.0042(8) 0.0026(7) S(20) 0.077(1) 0.044(1) 0.0363(8) 0.0089(9) -0.0016(8) 0.0026(7) N(1) 0.059(3) 0.037(3) 0.045(3) -0.001(3) 0.002(3) -0.002(2) C(1) 0.052(4) 0.036(3) 0.033(3) 0.000(3) 0.011(3) 0.001(2) C(2) 0.061(4) 0.032(3) 0.034(3) -0.003(3) 0.010(3) 0.000(2) C(3) 0.053(4) 0.031(3) 0.037(3) 0.001(3) 0.008(3) -0.002(2) C(4) 0.058(4) 0.034(3) 0.029(3) -0.002(3) 0.009(3) 0.000(2) C(5) 0.055(4) 0.044(4) 0.033(3) 0.006(3) 0.008(3) 0.000(3) C(6) 0.059(4) 0.033(3) 0.033(3) 0.003(3) 0.010(3) 0.001(2) C(7) 0.039(3) 0.028(3) 0.032(3) -0.003(2) 0.000(2) -0.002(2) C(8) 0.042(3) 0.028(3) 0.039(3) 0.000(2) 0.006(2) -0.006(2) C(9) 0.046(3) 0.026(3) 0.032(3) 0.001(2) -0.003(2) 0.000(2) C(10) 0.052(4) 0.025(3) 0.036(3) 0.003(2) 0.004(3) -0.002(2) C(11) 0.051(4) 0.030(3) 0.034(3) -0.007(3) 0.004(3) -0.001(2) C(12) 0.046(3) 0.030(3) 0.044(3) -0.001(3) 0.009(3) -0.006(3) C(13) 0.055(4) 0.035(4) 0.053(4) -0.003(3) 0.001(3) 0.003(3) C(14) 0.057(4) 0.036(3) 0.041(3) -0.001(3) -0.002(3) 0.008(3) C(15) 0.053(4) 0.046(4) 0.045(4) 0.001(3) 0.006(3) 0.003(3) C(16) 0.056(4) 0.032(3) 0.049(4) 0.004(3) -0.007(3) 0.005(3) C(17) 0.065(5) 0.038(4) 0.048(4) -0.004(3) -0.002(3) 0.006(3) C(18) 0.089(6) 0.073(6) 0.045(4) -0.013(5) 0.011(4) -0.002(4) #------------------------------------------------------------------------------ _computing_data_collection . _computing_cell_refinement . _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR97 _computing_structure_refinement SHELXL97 _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 I(1) C(14) 2.105(7) . . yes I(2) C(16) 2.088(7) . . yes Ni(1) S(1) 2.176(2) . . yes Ni(1) S(2) 2.163(2) . . yes Ni(1) S(3) 2.167(2) . . yes Ni(1) S(4) 2.159(2) . . yes Ni(2) S(11) 2.162(2) . . yes Ni(2) S(12) 2.168(2) . . yes Ni(2) S(13) 2.163(2) . . yes Ni(2) S(14) 2.166(2) . . yes S(1) C(1) 1.716(7) . . yes S(2) C(2) 1.706(7) . . yes S(3) C(3) 1.699(7) . . yes S(4) C(4) 1.691(6) . . yes S(5) C(1) 1.752(7) . . yes S(5) C(5) 1.727(7) . . yes S(6) C(2) 1.749(7) . . yes S(6) C(5) 1.714(7) . . yes S(7) C(3) 1.741(7) . . yes S(7) C(6) 1.729(7) . . yes S(8) C(4) 1.741(6) . . yes S(8) C(6) 1.723(7) . . yes S(9) C(5) 1.668(7) . . yes S(10) C(6) 1.653(7) . . yes S(11) C(7) 1.696(6) . . yes S(12) C(8) 1.686(6) . . yes S(13) C(9) 1.710(6) . . yes S(14) C(10) 1.710(6) . . yes S(15) C(7) 1.738(6) . . yes S(15) C(11) 1.724(6) . . yes S(16) C(8) 1.750(6) . . yes S(16) C(11) 1.725(7) . . yes S(17) C(9) 1.742(6) . . yes S(17) C(12) 1.730(7) . . yes S(18) C(10) 1.740(6) . . yes S(18) C(12) 1.737(6) . . yes S(19) C(11) 1.652(6) . . yes S(20) C(12) 1.645(6) . . yes N(1) C(13) 1.350(9) . . yes N(1) C(17) 1.365(10) . . yes N(1) C(18) 1.46(1) . . yes C(1) C(2) 1.359(9) . . yes C(3) C(4) 1.378(9) . . yes C(7) C(8) 1.393(8) . . yes C(9) C(10) 1.380(9) . . yes C(13) C(14) 1.386(10) . . yes C(14) C(15) 1.38(1) . . yes C(15) C(16) 1.398(10) . . yes C(16) C(17) 1.37(1) . . 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) 93.19(7) . . . yes S(1) Ni(1) S(3) 88.52(7) . . . yes S(1) Ni(1) S(4) 178.85(8) . . . yes S(2) Ni(1) S(3) 176.53(9) . . . yes S(2) Ni(1) S(4) 85.75(7) . . . yes S(3) Ni(1) S(4) 92.51(7) . . . yes S(11) Ni(2) S(12) 92.46(6) . . . yes S(11) Ni(2) S(13) 86.81(6) . . . yes S(11) Ni(2) S(14) 177.85(8) . . . yes S(12) Ni(2) S(13) 177.22(8) . . . yes S(12) Ni(2) S(14) 87.59(6) . . . yes S(13) Ni(2) S(14) 93.23(7) . . . yes Ni(1) S(1) C(1) 101.5(2) . . . yes Ni(1) S(2) C(2) 102.1(2) . . . yes Ni(1) S(3) C(3) 102.5(2) . . . yes Ni(1) S(4) C(4) 102.9(2) . . . yes C(1) S(5) C(5) 97.0(3) . . . yes C(2) S(6) C(5) 97.3(3) . . . yes C(3) S(7) C(6) 97.2(3) . . . yes C(4) S(8) C(6) 97.2(3) . . . yes Ni(2) S(11) C(7) 103.1(2) . . . yes Ni(2) S(12) C(8) 102.7(2) . . . yes Ni(2) S(13) C(9) 102.2(2) . . . yes Ni(2) S(14) C(10) 102.4(2) . . . yes C(7) S(15) C(11) 97.1(3) . . . yes C(8) S(16) C(11) 97.4(3) . . . yes C(9) S(17) C(12) 97.9(3) . . . yes C(10) S(18) C(12) 98.0(3) . . . yes C(13) N(1) C(17) 121.7(6) . . . yes C(13) N(1) C(18) 121.0(7) . . . yes C(17) N(1) C(18) 117.2(6) . . . yes S(1) C(1) S(5) 122.7(4) . . . yes S(1) C(1) C(2) 121.6(5) . . . yes S(5) C(1) C(2) 115.7(5) . . . yes S(2) C(2) S(6) 122.4(4) . . . yes S(2) C(2) C(1) 121.6(5) . . . yes S(6) C(2) C(1) 116.0(5) . . . yes S(3) C(3) S(7) 123.5(4) . . . yes S(3) C(3) C(4) 120.9(5) . . . yes S(7) C(3) C(4) 115.6(5) . . . yes S(4) C(4) S(8) 122.8(4) . . . yes S(4) C(4) C(3) 121.2(5) . . . yes S(8) C(4) C(3) 116.0(5) . . . yes S(5) C(5) S(6) 113.9(4) . . . yes S(5) C(5) S(9) 123.4(4) . . . yes S(6) C(5) S(9) 122.6(4) . . . yes S(7) C(6) S(8) 114.0(4) . . . yes S(7) C(6) S(10) 123.1(4) . . . yes S(8) C(6) S(10) 122.9(4) . . . yes S(11) C(7) S(15) 123.4(3) . . . yes S(11) C(7) C(8) 120.3(4) . . . yes S(15) C(7) C(8) 116.3(4) . . . yes S(12) C(8) S(16) 123.7(4) . . . yes S(12) C(8) C(7) 121.4(5) . . . yes S(16) C(8) C(7) 114.8(4) . . . yes S(13) C(9) S(17) 122.8(3) . . . yes S(13) C(9) C(10) 121.3(4) . . . yes S(17) C(9) C(10) 115.8(4) . . . yes S(14) C(10) S(18) 123.6(4) . . . yes S(14) C(10) C(9) 120.9(5) . . . yes S(18) C(10) C(9) 115.5(4) . . . yes S(15) C(11) S(16) 114.4(3) . . . yes S(15) C(11) S(19) 122.4(4) . . . yes S(16) C(11) S(19) 123.1(4) . . . yes S(17) C(12) S(18) 112.8(3) . . . yes S(17) C(12) S(20) 123.1(4) . . . yes S(18) C(12) S(20) 124.1(4) . . . yes N(1) C(13) C(14) 119.2(6) . . . yes I(1) C(14) C(13) 115.6(5) . . . yes I(1) C(14) C(15) 123.9(5) . . . yes C(13) C(14) C(15) 120.5(6) . . . yes C(14) C(15) C(16) 118.7(7) . . . yes I(2) C(16) C(15) 123.5(5) . . . yes I(2) C(16) C(17) 116.4(5) . . . yes C(15) C(16) C(17) 120.1(7) . . . yes N(1) C(17) C(16) 119.7(6) . . . 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 I(1) C(14) C(13) N(1) 173.6(5) . . . . yes I(1) C(14) C(15) C(16) -173.2(5) . . . . yes I(2) C(16) C(15) C(14) 178.3(5) . . . . yes I(2) C(16) C(17) N(1) -179.9(5) . . . . yes Ni(1) S(1) C(1) S(5) -179.7(4) . . . . yes Ni(1) S(1) C(1) C(2) 0.0(6) . . . . yes Ni(1) S(2) C(2) S(6) 178.6(4) . . . . yes Ni(1) S(2) C(2) C(1) 0.2(6) . . . . yes Ni(1) S(3) C(3) S(7) 179.1(4) . . . . yes Ni(1) S(3) C(3) C(4) -1.0(6) . . . . yes Ni(1) S(4) C(4) S(8) -179.8(4) . . . . yes Ni(1) S(4) C(4) C(3) 2.3(6) . . . . yes Ni(2) S(11) C(7) S(15) -177.3(3) . . . . yes Ni(2) S(11) C(7) C(8) 2.1(5) . . . . yes Ni(2) S(12) C(8) S(16) 179.0(3) . . . . yes Ni(2) S(12) C(8) C(7) 0.7(6) . . . . yes Ni(2) S(13) C(9) S(17) 177.6(3) . . . . yes Ni(2) S(13) C(9) C(10) -0.9(6) . . . . yes Ni(2) S(14) C(10) S(18) -178.1(4) . . . . yes Ni(2) S(14) C(10) C(9) -0.3(6) . . . . yes S(1) Ni(1) S(2) C(2) -0.1(3) . . . . yes S(1) Ni(1) S(3) C(3) -177.6(2) . . . . yes S(1) C(1) S(5) C(5) -180.0(4) . . . . yes S(1) C(1) C(2) S(2) -0.1(9) . . . . yes S(1) C(1) C(2) S(6) -178.7(4) . . . . yes S(2) Ni(1) S(1) C(1) 0.1(2) . . . . yes S(2) Ni(1) S(4) C(4) 174.7(3) . . . . yes S(2) C(2) S(6) C(5) 179.6(5) . . . . yes S(2) C(2) C(1) S(5) 179.6(4) . . . . yes S(3) Ni(1) S(1) C(1) 177.0(2) . . . . yes S(3) Ni(1) S(4) C(4) -2.3(3) . . . . yes S(3) C(3) S(7) C(6) 178.4(5) . . . . yes S(3) C(3) C(4) S(4) -1.0(9) . . . . yes S(3) C(3) C(4) S(8) -179.0(4) . . . . yes S(4) Ni(1) S(2) C(2) -179.7(3) . . . . yes S(4) Ni(1) S(3) C(3) 1.9(3) . . . . yes S(4) C(4) S(8) C(6) -177.9(5) . . . . yes S(4) C(4) C(3) S(7) 179.0(4) . . . . yes S(5) C(1) C(2) S(6) 1.1(7) . . . . yes S(5) C(5) S(6) C(2) 2.0(5) . . . . yes S(6) C(5) S(5) C(1) -1.5(5) . . . . yes S(7) C(3) C(4) S(8) 1.0(7) . . . . yes S(7) C(6) S(8) C(4) -1.2(5) . . . . yes S(8) C(6) S(7) C(3) 1.6(5) . . . . yes S(9) C(5) S(5) C(1) 179.1(5) . . . . yes S(9) C(5) S(6) C(2) -178.6(5) . . . . yes S(10) C(6) S(7) C(3) 179.7(5) . . . . yes S(10) C(6) S(8) C(4) -179.2(5) . . . . yes S(11) Ni(2) S(12) C(8) 0.5(2) . . . . yes S(11) Ni(2) S(13) C(9) -177.3(2) . . . . yes S(11) C(7) S(15) C(11) -179.6(4) . . . . yes S(11) C(7) C(8) S(12) -1.9(8) . . . . yes S(11) C(7) C(8) S(16) 179.6(3) . . . . yes S(12) Ni(2) S(11) C(7) -1.3(2) . . . . yes S(12) Ni(2) S(14) C(10) -177.5(2) . . . . yes S(12) C(8) S(16) C(11) -178.0(4) . . . . yes S(12) C(8) C(7) S(15) 177.4(3) . . . . yes S(13) Ni(2) S(11) C(7) -178.6(2) . . . . yes S(13) Ni(2) S(14) C(10) -0.2(2) . . . . yes S(13) C(9) S(17) C(12) -177.3(4) . . . . yes S(13) C(9) C(10) S(14) 0.9(8) . . . . yes S(13) C(9) C(10) S(18) 178.8(4) . . . . yes S(14) Ni(2) S(13) C(9) 0.5(2) . . . . yes S(14) C(10) S(18) C(12) 176.3(4) . . . . yes S(14) C(10) C(9) S(17) -177.7(4) . . . . yes S(15) C(7) C(8) S(16) -1.0(7) . . . . yes S(15) C(11) S(16) C(8) 0.3(4) . . . . yes S(16) C(11) S(15) C(7) -0.8(4) . . . . yes S(17) C(9) C(10) S(18) 0.2(7) . . . . yes S(17) C(12) S(18) C(10) 2.3(4) . . . . yes S(18) C(12) S(17) C(9) -2.2(4) . . . . yes S(19) C(11) S(15) C(7) -177.6(4) . . . . yes S(19) C(11) S(16) C(8) 177.1(4) . . . . yes S(20) C(12) S(17) C(9) 176.6(4) . . . . yes S(20) C(12) S(18) C(10) -176.5(5) . . . . yes N(1) C(13) C(14) C(15) -2(1) . . . . yes N(1) C(17) C(16) C(15) 0(1) . . . . yes C(1) C(2) S(6) C(5) -1.9(6) . . . . yes C(2) C(1) S(5) C(5) 0.2(6) . . . . yes C(3) C(4) S(8) C(6) 0.1(6) . . . . yes C(4) C(3) S(7) C(6) -1.6(6) . . . . yes C(7) C(8) S(16) C(11) 0.4(5) . . . . yes C(8) C(7) S(15) C(11) 1.1(5) . . . . yes C(9) C(10) S(18) C(12) -1.5(6) . . . . yes C(10) C(9) S(17) C(12) 1.3(6) . . . . yes C(13) N(1) C(17) C(16) 0(1) . . . . yes C(13) C(14) C(15) C(16) 2(1) . . . . yes C(14) C(13) N(1) C(17) 1(1) . . . . yes C(14) C(13) N(1) C(18) -177.2(7) . . . . yes C(14) C(15) C(16) C(17) -1(1) . . . . yes C(16) C(17) N(1) C(18) 178.7(7) . . . . yes C(16) C(17) N(1) C(18) 178.7(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 I(1) S(19) 3.277(2) . 2_656 ? I(2) S(9) 3.491(2) . 1_565 ? Ni(1) Ni(1) 3.484(2) . 7_556 ? Ni(2) S(16) 3.416(2) . 2_656 ? S(1) S(4) 3.508(3) . 7_556 ? S(2) S(8) 3.498(3) . 3_666 ? S(2) S(3) 3.513(2) . 1_565 ? S(2) S(3) 3.583(3) . 7_556 ? S(3) S(4) 3.583(3) . 1_545 ? S(5) S(10) 3.593(3) . 3_656 ? S(10) C(18) 3.58(1) . 3_656 ? S(11) S(14) 3.361(2) . 1_545 ? S(11) S(12) 3.381(3) . 6_546 ? S(11) S(15) 3.552(3) . 2_656 ? S(11) S(12) 3.565(2) . 1_545 ? S(12) S(15) 3.453(2) . 1_565 ? S(12) S(12) 3.577(4) . 2_656 ? S(13) S(19) 3.525(3) . 2_656 ? S(13) S(18) 3.530(2) . 1_545 ? S(13) S(14) 3.554(2) . 1_545 ? C(7) C(7) 3.51(1) . 2_656 ? C(10) C(11) 3.543(9) . 6_556 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data__2 _database_code_depnum_ccdc_archive 'CCDC 910061' #TrackingRef '16103_web_deposit_cif_file_0_HiroshiM.Yamamoto_1355276590.1.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H6 Br2 N Ni2 S20 ' _chemical_formula_moiety 'C6 H6 Br2 N, 2(C6 Ni S10)' _chemical_formula_weight 1154.66 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 7.632(5) _cell_length_b 11.716(7) _cell_length_c 20.19(1) _cell_angle_alpha 98.87(1) _cell_angle_beta 93.400(8) _cell_angle_gamma 101.19(1) _cell_volume 1742.4(18) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4675 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 295.0 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Black _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.070 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.201 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1134.00 _exptl_absorpt_coefficient_mu 4.600 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.9453 _exptl_absorpt_correction_T_min 0.5862 _exptl_absorpt_process_details 'Rigaku/MSC CrysatalClear' #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 14223 _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 #------------------------------------------------------------------------------ # 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 7856 _reflns_number_gt 5632 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1805 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7856 _refine_ls_number_parameters 452 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0460 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 1.00 _refine_diff_density_min -0.79 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 Br(1) Br 0.7404(6) -0.0269(4) 0.4869(2) 0.0553(6) Uani 0.60 2 d P . 1 Br(2) Br 0.9674(2) 0.4367(2) 0.6302(1) 0.0746(8) Uani 0.60 2 d P . 1 Br(3) Br 0.754(1) -0.0138(6) 0.5002(4) 0.090(2) Uani 0.40 2 d P . 2 Br(4) Br 0.9157(6) 0.4885(3) 0.5845(3) 0.116(2) Uani 0.40 2 d P . 2 Ni(1) Ni 0.89498(8) 0.12459(5) 1.02358(3) 0.0313(2) Uani 1.00 1 d . . . Ni(2) Ni 0.55983(9) 0.35424(6) 0.89674(3) 0.0341(2) Uani 1.00 1 d . . . S(1) S 0.9929(2) 0.2254(1) 0.94704(7) 0.0389(3) Uani 1.00 1 d . . . S(2) S 0.7029(2) -0.0019(1) 0.95216(7) 0.0393(3) Uani 1.00 1 d . . . S(3) S 1.0889(2) 0.2503(1) 1.09468(7) 0.0379(3) Uani 1.00 1 d . . . S(4) S 0.7860(2) 0.0298(1) 1.10053(7) 0.0375(3) Uani 1.00 1 d . . . S(5) S 0.8800(2) 0.1931(1) 0.79821(7) 0.0430(3) Uani 1.00 1 d . . . S(6) S 0.6144(2) -0.0179(1) 0.80282(7) 0.0431(3) Uani 1.00 1 d . . . S(7) S 1.1590(2) 0.2761(1) 1.24646(7) 0.0428(3) Uani 1.00 1 d . . . S(8) S 0.8799(2) 0.0728(1) 1.25154(7) 0.0464(3) Uani 1.00 1 d . . . S(9) S 0.6580(3) 0.0688(2) 0.67259(8) 0.0690(5) Uani 1.00 1 d . . . S(10) S 1.0788(3) 0.2079(2) 1.37960(8) 0.0667(5) Uani 1.00 1 d . . . S(11) S 0.6572(2) 0.4560(1) 0.82106(7) 0.0420(3) Uani 1.00 1 d . . . S(12) S 0.3609(2) 0.2296(1) 0.82633(7) 0.0413(3) Uani 1.00 1 d . . . S(13) S 0.7503(2) 0.4818(1) 0.96784(7) 0.0437(3) Uani 1.00 1 d . . . S(14) S 0.4676(2) 0.2528(1) 0.97271(7) 0.0420(3) Uani 1.00 1 d . . . S(15) S 0.5375(2) 0.4254(1) 0.67255(8) 0.0484(4) Uani 1.00 1 d . . . S(16) S 0.2642(2) 0.2211(1) 0.67718(8) 0.0504(4) Uani 1.00 1 d . . . S(17) S 0.8348(2) 0.5020(1) 1.11758(8) 0.0483(4) Uani 1.00 1 d . . . S(18) S 0.5691(2) 0.2898(1) 1.12206(8) 0.0475(3) Uani 1.00 1 d . . . S(19) S 0.3104(3) 0.3115(2) 0.54673(8) 0.0553(4) Uani 1.00 1 d . . . S(20) S 0.7837(3) 0.4179(2) 1.24749(9) 0.0772(6) Uani 1.00 1 d . . . N(1) N 0.665(2) 0.296(1) 0.4520(7) 0.048(3) Uani 0.60 2 d P . 1 N(2) N 0.647(3) 0.260(2) 0.424(1) 0.055(6) Uani 0.40 2 d P . 2 C(1) C 0.8626(7) 0.1501(4) 0.8766(3) 0.032(1) Uani 1.00 1 d . . . C(2) C 0.7367(7) 0.0494(4) 0.8794(3) 0.034(1) Uani 1.00 1 d . . . C(3) C 1.0436(7) 0.2037(5) 1.1693(3) 0.035(1) Uani 1.00 1 d . . . C(4) C 0.9123(7) 0.1075(5) 1.1717(3) 0.035(1) Uani 1.00 1 d . . . C(5) C 0.7166(8) 0.0799(5) 0.7541(3) 0.042(1) Uani 1.00 1 d . . . C(6) C 1.0413(8) 0.1868(5) 1.2966(3) 0.044(1) Uani 1.00 1 d . . . C(7) C 0.5224(8) 0.3825(5) 0.7507(3) 0.038(1) Uani 1.00 1 d . . . C(8) C 0.3913(7) 0.2838(5) 0.7532(3) 0.038(1) Uani 1.00 1 d . . . C(9) C 0.7154(7) 0.4328(4) 1.0414(3) 0.036(1) Uani 1.00 1 d . . . C(10) C 0.5901(8) 0.3310(5) 1.0438(3) 0.039(1) Uani 1.00 1 d . . . C(11) C 0.3676(8) 0.3181(5) 0.6285(3) 0.044(1) Uani 1.00 1 d . . . C(12) C 0.7324(8) 0.4048(5) 1.1662(3) 0.046(1) Uani 1.00 1 d . . . C(13) C 0.6614(9) 0.1695(7) 0.4420(4) 0.059(2) Uani 1.00 1 d . . . C(14) C 0.7499(8) 0.1382(5) 0.4939(3) 0.044(1) Uani 1.00 1 d . . . C(15) C 0.849(3) 0.214(2) 0.5528(9) 0.043(4) Uani 0.60 2 d P . 1 C(16) C 0.848(2) 0.329(2) 0.552(1) 0.058(6) Uani 0.60 2 d P . 1 C(17) C 0.751(3) 0.370(2) 0.506(1) 0.054(5) Uani 0.60 2 d P . 1 C(18) C 0.570(2) 0.341(2) 0.3972(8) 0.069(4) Uani 0.60 2 d P . 1 C(19) C 0.820(4) 0.229(4) 0.537(1) 0.046(7) Uani 0.40 2 d P . 2 C(20) C 0.803(4) 0.346(2) 0.526(2) 0.08(2) Uani 0.40 2 d P . 2 C(21) C 0.725(5) 0.363(3) 0.467(2) 0.08(1) Uani 0.40 2 d P . 2 C(22) C 0.560(4) 0.277(3) 0.360(1) 0.095(8) Uani 0.40 2 d P . 2 H(1) H 0.6031 0.1153 0.4035 0.0719 Uiso 0.60 2 calc P . 1 H(2) H 0.9100 0.1866 0.5883 0.0510 Uiso 0.60 2 calc P . 1 H(3) H 0.7451 0.4518 0.5107 0.0647 Uiso 0.60 2 calc P . 1 H(4) H 0.6513 0.3952 0.3785 0.0837 Uiso 0.60 2 calc P . 1 H(5) H 0.5144 0.2758 0.3630 0.0837 Uiso 0.60 2 calc P . 1 H(6) H 0.4783 0.3779 0.4156 0.0837 Uiso 0.60 2 calc P . 1 H(7) H 0.5940 0.1025 0.4123 0.0719 Uiso 0.40 2 calc P . 2 H(8) H 0.8839 0.2178 0.5764 0.0528 Uiso 0.40 2 calc P . 2 H(9) H 0.7248 0.4382 0.4561 0.0886 Uiso 0.40 2 calc P . 2 H(10) H 0.4718 0.3216 0.3687 0.1171 Uiso 0.40 2 calc P . 2 H(11) H 0.6508 0.3191 0.3364 0.1171 Uiso 0.40 2 calc P . 2 H(12) H 0.5108 0.2028 0.3337 0.1171 Uiso 0.40 2 calc P . 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Br(1) 0.052(1) 0.0470(10) 0.0614(9) 0.0022(8) 0.0070(8) 0.0031(8) Br(2) 0.0466(7) 0.074(1) 0.084(1) 0.0041(6) -0.0004(6) -0.0326(10) Br(3) 0.093(4) 0.074(3) 0.132(5) 0.042(3) 0.049(3) 0.058(3) Br(4) 0.101(3) 0.089(2) 0.118(3) -0.042(2) 0.060(3) -0.045(2) Ni(1) 0.0317(3) 0.0304(3) 0.0292(3) 0.0013(3) 0.0032(2) 0.0030(3) Ni(2) 0.0343(4) 0.0293(3) 0.0377(4) 0.0035(3) 0.0039(3) 0.0067(3) S(1) 0.0398(7) 0.0368(7) 0.0341(7) -0.0054(6) 0.0016(5) 0.0052(5) S(2) 0.0419(7) 0.0364(7) 0.0336(7) -0.0062(6) 0.0019(5) 0.0054(5) S(3) 0.0392(7) 0.0355(7) 0.0332(6) -0.0060(5) 0.0019(5) 0.0055(5) S(4) 0.0389(7) 0.0330(6) 0.0354(7) -0.0042(5) 0.0022(5) 0.0054(5) S(5) 0.0479(8) 0.0433(8) 0.0353(7) 0.0011(6) 0.0052(6) 0.0088(6) S(6) 0.0457(8) 0.0404(7) 0.0367(7) -0.0014(6) -0.0039(6) 0.0021(6) S(7) 0.0454(8) 0.0441(8) 0.0324(7) -0.0015(6) -0.0021(6) 0.0024(6) S(8) 0.0517(8) 0.0488(8) 0.0350(7) -0.0033(7) 0.0032(6) 0.0133(6) S(9) 0.084(1) 0.082(1) 0.0319(8) -0.003(1) -0.0061(8) 0.0097(8) S(10) 0.068(1) 0.096(1) 0.0305(8) 0.004(1) 0.0022(7) 0.0094(8) S(11) 0.0437(8) 0.0366(7) 0.0413(7) -0.0039(6) 0.0030(6) 0.0086(6) S(12) 0.0437(8) 0.0375(7) 0.0387(7) -0.0034(6) 0.0008(6) 0.0103(6) S(13) 0.0479(8) 0.0357(7) 0.0411(7) -0.0066(6) 0.0042(6) 0.0061(6) S(14) 0.0429(8) 0.0355(7) 0.0435(8) -0.0041(6) 0.0004(6) 0.0108(6) S(15) 0.0561(9) 0.0474(8) 0.0393(8) -0.0010(7) 0.0089(6) 0.0130(6) S(16) 0.0560(9) 0.0485(8) 0.0395(8) -0.0061(7) -0.0036(6) 0.0100(6) S(17) 0.0507(9) 0.0469(8) 0.0410(8) 0.0035(7) 0.0001(6) -0.0020(6) S(18) 0.0563(9) 0.0468(8) 0.0413(8) 0.0083(7) 0.0082(6) 0.0146(6) S(19) 0.069(1) 0.0589(10) 0.0372(8) 0.0095(8) 0.0041(7) 0.0101(7) S(20) 0.092(2) 0.109(2) 0.0371(9) 0.043(1) 0.0019(9) 0.0072(10) N(1) 0.046(6) 0.046(9) 0.056(9) 0.007(7) 0.012(7) 0.024(8) N(2) 0.05(1) 0.06(1) 0.06(1) 0.016(10) 0.03(1) 0.011(10) C(1) 0.032(2) 0.036(3) 0.032(2) 0.013(2) 0.006(2) 0.005(2) C(2) 0.036(3) 0.033(3) 0.034(3) 0.009(2) 0.002(2) 0.003(2) C(3) 0.040(3) 0.034(3) 0.031(3) 0.009(2) -0.001(2) 0.002(2) C(4) 0.038(3) 0.036(3) 0.032(2) 0.008(2) 0.005(2) 0.006(2) C(5) 0.042(3) 0.048(3) 0.036(3) 0.010(3) 0.002(2) 0.006(2) C(6) 0.044(3) 0.047(3) 0.038(3) 0.006(3) 0.004(2) 0.008(2) C(7) 0.046(3) 0.033(3) 0.037(3) 0.006(2) 0.010(2) 0.008(2) C(8) 0.040(3) 0.036(3) 0.036(3) 0.003(2) 0.003(2) 0.006(2) C(9) 0.041(3) 0.031(3) 0.037(3) 0.008(2) 0.004(2) 0.003(2) C(10) 0.043(3) 0.035(3) 0.043(3) 0.015(2) 0.011(2) 0.009(2) C(11) 0.051(3) 0.044(3) 0.038(3) 0.011(3) 0.011(2) 0.009(2) C(12) 0.053(3) 0.043(3) 0.046(3) 0.023(3) 0.008(3) 0.005(2) C(13) 0.047(4) 0.072(5) 0.059(4) -0.001(3) 0.009(3) 0.025(4) C(14) 0.038(3) 0.050(3) 0.040(3) 0.003(3) 0.008(2) 0.006(3) C(15) 0.030(9) 0.072(10) 0.024(9) 0.008(6) -0.009(6) 0.005(7) C(16) 0.022(7) 0.08(1) 0.065(9) 0.003(7) 0.010(6) -0.015(9) C(17) 0.06(1) 0.041(10) 0.07(1) 0.018(7) 0.029(10) 0.024(9) C(18) 0.069(8) 0.09(1) 0.057(8) 0.021(8) 0.018(7) 0.037(8) C(19) 0.03(1) 0.09(2) 0.02(1) 0.013(10) -0.015(8) 0.01(1) C(20) 0.04(2) 0.02(1) 0.17(5) -0.01(1) 0.03(2) 0.00(2) C(21) 0.08(2) 0.06(2) 0.12(3) 0.04(2) 0.09(2) 0.06(2) C(22) 0.12(2) 0.12(2) 0.07(2) 0.05(2) 0.02(2) 0.05(2) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR97 _computing_structure_refinement SHELXL97 _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 Br(1) Br(3) 0.291(8) . . yes Br(1) C(14) 1.905(8) . . yes Br(2) Br(4) 1.264(6) . . yes Br(2) C(16) 1.91(2) . . yes Br(3) C(14) 1.81(1) . . yes Br(4) C(16) 1.84(3) . . yes Br(4) C(17) 2.11(2) . . yes Br(4) C(20) 1.90(3) . . yes Ni(1) S(1) 2.168(2) . . yes Ni(1) S(2) 2.161(1) . . yes Ni(1) S(3) 2.161(1) . . yes Ni(1) S(4) 2.160(2) . . yes Ni(2) S(11) 2.159(2) . . yes Ni(2) S(12) 2.168(1) . . yes Ni(2) S(13) 2.158(1) . . yes Ni(2) S(14) 2.151(2) . . yes S(1) C(1) 1.701(5) . . yes S(2) C(2) 1.686(6) . . yes S(3) C(3) 1.712(6) . . yes S(4) C(4) 1.707(5) . . yes S(5) C(1) 1.738(6) . . yes S(5) C(5) 1.722(5) . . yes S(6) C(2) 1.746(5) . . yes S(6) C(5) 1.725(6) . . yes S(7) C(3) 1.750(5) . . yes S(7) C(6) 1.731(6) . . yes S(8) C(4) 1.742(6) . . yes S(8) C(6) 1.727(5) . . yes S(9) C(5) 1.659(6) . . yes S(10) C(6) 1.655(6) . . yes S(11) C(7) 1.709(5) . . yes S(12) C(8) 1.706(6) . . yes S(13) C(9) 1.690(6) . . yes S(14) C(10) 1.696(5) . . yes S(15) C(7) 1.732(6) . . yes S(15) C(11) 1.714(5) . . yes S(16) C(8) 1.742(5) . . yes S(16) C(11) 1.722(6) . . yes S(17) C(9) 1.737(5) . . yes S(17) C(12) 1.721(7) . . yes S(18) C(10) 1.729(6) . . yes S(18) C(12) 1.734(6) . . yes S(19) C(11) 1.669(6) . . yes S(20) C(12) 1.641(6) . . yes N(1) N(2) 0.65(2) . . yes N(1) C(13) 1.46(2) . . yes N(1) C(17) 1.33(2) . . yes N(1) C(18) 1.51(2) . . yes N(1) C(20) 1.73(4) . . yes N(1) C(21) 0.82(4) . . yes N(2) C(13) 1.20(3) . . yes N(2) C(18) 1.37(3) . . yes N(2) C(21) 1.38(4) . . yes N(2) C(22) 1.48(4) . . yes C(1) C(2) 1.380(7) . . yes C(3) C(4) 1.364(7) . . yes C(7) C(8) 1.384(7) . . yes C(9) C(10) 1.385(7) . . yes C(13) C(14) 1.35(1) . . yes C(14) C(15) 1.45(2) . . yes C(14) C(19) 1.27(4) . . yes C(15) C(16) 1.35(4) . . yes C(15) C(19) 0.46(5) . . yes C(15) C(20) 1.80(4) . . yes C(16) C(17) 1.37(3) . . yes C(16) C(19) 1.14(5) . . yes C(16) C(20) 0.69(5) . . yes C(17) C(20) 0.69(5) . . yes C(17) C(21) 0.78(5) . . yes C(18) C(21) 1.73(4) . . yes C(18) C(22) 0.97(3) . . yes C(19) C(20) 1.45(6) . . yes C(20) C(21) 1.37(6) . . 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 Br(3) Br(1) C(14) 66(1) . . . yes Br(4) Br(2) C(16) 67.2(9) . . . yes Br(1) Br(3) C(14) 104(2) . . . yes Br(2) Br(4) C(16) 73.5(7) . . . yes Br(2) Br(4) C(17) 112.4(7) . . . yes Br(2) Br(4) C(20) 94(1) . . . yes S(1) Ni(1) S(2) 92.79(6) . . . yes S(1) Ni(1) S(3) 87.10(6) . . . yes S(1) Ni(1) S(4) 176.81(7) . . . yes S(2) Ni(1) S(3) 179.49(7) . . . yes S(2) Ni(1) S(4) 87.03(6) . . . yes S(3) Ni(1) S(4) 93.11(6) . . . yes S(11) Ni(2) S(12) 93.60(6) . . . yes S(11) Ni(2) S(13) 86.62(6) . . . yes S(11) Ni(2) S(14) 179.00(7) . . . yes S(12) Ni(2) S(13) 177.91(7) . . . yes S(12) Ni(2) S(14) 87.06(6) . . . yes S(13) Ni(2) S(14) 92.75(6) . . . yes Ni(1) S(1) C(1) 102.3(2) . . . yes Ni(1) S(2) C(2) 102.5(2) . . . yes Ni(1) S(3) C(3) 102.1(2) . . . yes Ni(1) S(4) C(4) 102.3(2) . . . yes C(1) S(5) C(5) 97.0(3) . . . yes C(2) S(6) C(5) 97.4(2) . . . yes C(3) S(7) C(6) 97.1(3) . . . yes C(4) S(8) C(6) 97.7(3) . . . yes Ni(2) S(11) C(7) 102.0(2) . . . yes Ni(2) S(12) C(8) 101.9(2) . . . yes Ni(2) S(13) C(9) 102.7(2) . . . yes Ni(2) S(14) C(10) 102.9(2) . . . yes C(7) S(15) C(11) 98.2(3) . . . yes C(8) S(16) C(11) 97.8(3) . . . yes C(9) S(17) C(12) 97.0(3) . . . yes C(10) S(18) C(12) 96.6(3) . . . yes N(2) N(1) C(13) 54(2) . . . yes N(2) N(1) C(17) 163(3) . . . yes N(2) N(1) C(18) 65(2) . . . yes N(2) N(1) C(20) 148(3) . . . yes N(2) N(1) C(21) 138(4) . . . yes C(13) N(1) C(17) 122(1) . . . yes C(13) N(1) C(18) 117(1) . . . yes C(13) N(1) C(20) 101(1) . . . yes C(13) N(1) C(21) 145(3) . . . yes C(17) N(1) C(18) 120(1) . . . yes C(18) N(1) C(20) 140(1) . . . yes C(18) N(1) C(21) 91(3) . . . yes C(20) N(1) C(21) 50(3) . . . yes N(1) N(2) C(13) 100(3) . . . yes N(1) N(2) C(18) 89(3) . . . yes N(1) N(2) C(22) 128(3) . . . yes C(13) N(2) C(18) 160(2) . . . yes C(13) N(2) C(21) 116(2) . . . yes C(13) N(2) C(22) 128(2) . . . yes C(18) N(2) C(21) 78(2) . . . yes C(21) N(2) C(22) 114(2) . . . yes S(1) C(1) S(5) 122.9(3) . . . yes S(1) C(1) C(2) 120.6(4) . . . yes S(5) C(1) C(2) 116.4(4) . . . yes S(2) C(2) S(6) 123.2(3) . . . yes S(2) C(2) C(1) 121.7(4) . . . yes S(6) C(2) C(1) 115.0(4) . . . yes S(3) C(3) S(7) 122.6(3) . . . yes S(3) C(3) C(4) 121.2(4) . . . yes S(7) C(3) C(4) 116.2(4) . . . yes S(4) C(4) S(8) 123.0(3) . . . yes S(4) C(4) C(3) 121.3(4) . . . yes S(8) C(4) C(3) 115.6(4) . . . yes S(5) C(5) S(6) 114.1(3) . . . yes S(5) C(5) S(9) 122.8(4) . . . yes S(6) C(5) S(9) 123.0(3) . . . yes S(7) C(6) S(8) 113.4(3) . . . yes S(7) C(6) S(10) 123.6(3) . . . yes S(8) C(6) S(10) 123.0(4) . . . yes S(11) C(7) S(15) 123.2(3) . . . yes S(11) C(7) C(8) 121.3(4) . . . yes S(15) C(7) C(8) 115.5(4) . . . yes S(12) C(8) S(16) 123.7(3) . . . yes S(12) C(8) C(7) 121.1(4) . . . yes S(16) C(8) C(7) 115.2(4) . . . yes S(13) C(9) S(17) 123.3(3) . . . yes S(13) C(9) C(10) 121.0(4) . . . yes S(17) C(9) C(10) 115.7(4) . . . yes S(14) C(10) S(18) 123.1(3) . . . yes S(14) C(10) C(9) 120.6(4) . . . yes S(18) C(10) C(9) 116.3(4) . . . yes S(15) C(11) S(16) 113.3(3) . . . yes S(15) C(11) S(19) 122.2(4) . . . yes S(16) C(11) S(19) 124.5(3) . . . yes S(17) C(12) S(18) 114.4(3) . . . yes S(17) C(12) S(20) 123.5(3) . . . yes S(18) C(12) S(20) 122.1(4) . . . yes N(1) C(13) C(14) 112.2(8) . . . yes N(2) C(13) C(14) 136(1) . . . yes Br(1) C(14) C(13) 114.8(5) . . . yes Br(1) C(14) C(15) 117(1) . . . yes Br(1) C(14) C(19) 135(1) . . . yes Br(3) C(14) C(13) 123.1(5) . . . yes Br(3) C(14) C(15) 108(1) . . . yes Br(3) C(14) C(19) 126(1) . . . yes C(13) C(14) C(15) 127(1) . . . yes C(13) C(14) C(19) 110(2) . . . yes C(14) C(15) C(16) 112(1) . . . yes C(14) C(15) C(19) 58(5) . . . yes C(14) C(15) C(20) 93(1) . . . yes C(16) C(15) C(19) 53(5) . . . yes Br(2) C(16) C(15) 115(1) . . . yes Br(2) C(16) C(17) 119(1) . . . yes Br(2) C(16) C(19) 134(2) . . . yes Br(2) C(16) C(20) 123(3) . . . yes Br(4) C(16) C(15) 154(1) . . . yes Br(4) C(16) C(17) 80(1) . . . yes Br(4) C(16) C(19) 172(2) . . . yes Br(4) C(16) C(20) 84(3) . . . yes C(15) C(16) C(17) 124(1) . . . yes C(15) C(16) C(20) 121(3) . . . yes C(17) C(16) C(19) 106(2) . . . yes C(19) C(16) C(20) 102(3) . . . yes Br(4) C(17) N(1) 173(1) . . . yes Br(4) C(17) C(16) 59(1) . . . yes Br(4) C(17) C(20) 63(2) . . . yes Br(4) C(17) C(21) 140(3) . . . yes N(1) C(17) C(16) 119(2) . . . yes N(1) C(17) C(20) 115(3) . . . yes C(16) C(17) C(21) 142(3) . . . yes C(20) C(17) C(21) 136(5) . . . yes N(1) C(18) C(22) 101(2) . . . yes N(2) C(18) C(21) 50(1) . . . yes N(2) C(18) C(22) 76(2) . . . yes C(21) C(18) C(22) 123(2) . . . yes C(14) C(19) C(15) 103(7) . . . yes C(14) C(19) C(16) 148(3) . . . yes C(14) C(19) C(20) 121(2) . . . yes C(15) C(19) C(16) 107(5) . . . yes C(15) C(19) C(20) 134(6) . . . yes Br(4) C(20) N(1) 141(2) . . . yes Br(4) C(20) C(15) 114(2) . . . yes Br(4) C(20) C(16) 74(3) . . . yes Br(4) C(20) C(17) 97(2) . . . yes Br(4) C(20) C(19) 124(2) . . . yes Br(4) C(20) C(21) 114(2) . . . yes N(1) C(20) C(15) 104(1) . . . yes N(1) C(20) C(16) 144(3) . . . yes N(1) C(20) C(19) 94(2) . . . yes C(15) C(20) C(17) 147(3) . . . yes C(15) C(20) C(21) 130(2) . . . yes C(16) C(20) C(17) 168(7) . . . yes C(16) C(20) C(19) 50(3) . . . yes C(16) C(20) C(21) 168(5) . . . yes C(17) C(20) C(19) 137(3) . . . yes C(19) C(20) C(21) 120(3) . . . yes N(1) C(21) C(17) 111(5) . . . yes N(1) C(21) C(18) 60(2) . . . yes N(1) C(21) C(20) 101(4) . . . yes N(2) C(21) C(17) 127(4) . . . yes N(2) C(21) C(18) 50(1) . . . yes N(2) C(21) C(20) 114(3) . . . yes C(17) C(21) C(18) 152(4) . . . yes C(18) C(21) C(20) 159(2) . . . yes N(2) C(22) C(18) 64(2) . . . 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 Br(1) Br(3) C(14) C(13) 13(2) . . . . yes Br(1) Br(3) C(14) C(15) -168(2) . . . . yes Br(1) Br(3) C(14) C(19) -169(2) . . . . yes Br(1) C(14) C(13) N(1) 176.9(8) . . . . yes Br(1) C(14) C(13) N(2) -171(1) . . . . yes Br(1) C(14) C(15) C(16) 179(1) . . . . yes Br(1) C(14) C(15) C(19) -178(5) . . . . yes Br(1) C(14) C(15) C(20) 179(1) . . . . yes Br(1) C(14) C(19) C(15) 2(6) . . . . yes Br(1) C(14) C(19) C(16) 177(4) . . . . yes Br(1) C(14) C(19) C(20) 179(2) . . . . yes Br(2) Br(4) C(16) C(15) -13(3) . . . . yes Br(2) Br(4) C(16) C(17) 167(1) . . . . yes Br(2) Br(4) C(16) C(20) 171(3) . . . . yes Br(2) Br(4) C(17) C(16) -13(1) . . . . yes Br(2) Br(4) C(17) C(20) -17(4) . . . . yes Br(2) Br(4) C(17) C(21) -150(5) . . . . yes Br(2) Br(4) C(20) N(1) 171(3) . . . . yes Br(2) Br(4) C(20) C(15) -9(2) . . . . yes Br(2) Br(4) C(20) C(16) -7(3) . . . . yes Br(2) Br(4) C(20) C(17) 163(4) . . . . yes Br(2) Br(4) C(20) C(19) -9(3) . . . . yes Br(2) Br(4) C(20) C(21) -179(2) . . . . yes Br(2) C(16) Br(4) C(17) -167(1) . . . . yes Br(2) C(16) Br(4) C(20) -171(3) . . . . yes Br(2) C(16) C(15) C(14) 177(1) . . . . yes Br(2) C(16) C(15) C(19) 175(5) . . . . yes Br(2) C(16) C(15) C(20) 176(5) . . . . yes Br(2) C(16) C(17) Br(4) 9.0(10) . . . . yes Br(2) C(16) C(17) N(1) -178(1) . . . . yes Br(2) C(16) C(17) C(20) 138(14) . . . . yes Br(2) C(16) C(17) C(21) 144(5) . . . . yes Br(2) C(16) C(19) C(14) 178(4) . . . . yes Br(2) C(16) C(19) C(15) -6(7) . . . . yes Br(2) C(16) C(19) C(20) 175(5) . . . . yes Br(2) C(16) C(20) Br(4) 6(2) . . . . yes Br(2) C(16) C(20) N(1) -173(4) . . . . yes Br(2) C(16) C(20) C(15) -176(5) . . . . yes Br(2) C(16) C(20) C(17) -45(4) . . . . yes Br(2) C(16) C(20) C(19) -176(4) . . . . yes Br(2) C(16) C(20) C(21) 145(19) . . . . yes Br(3) Br(1) C(14) C(13) -167(2) . . . . yes Br(3) Br(1) C(14) C(15) 12(2) . . . . yes Br(3) Br(1) C(14) C(19) 11(3) . . . . yes Br(3) C(14) C(13) N(1) 174.7(8) . . . . yes Br(3) C(14) C(13) N(2) -174(1) . . . . yes Br(3) C(14) C(15) C(16) -178(1) . . . . yes Br(3) C(14) C(15) C(19) -176(5) . . . . yes Br(3) C(14) C(15) C(20) -178(1) . . . . yes Br(3) C(14) C(19) C(15) 4(6) . . . . yes Br(3) C(14) C(19) C(16) -180.0 . . . . yes Br(3) C(14) C(19) C(20) -178(2) . . . . yes Br(4) Br(2) C(16) C(15) 173(1) . . . . yes Br(4) Br(2) C(16) C(17) -14(1) . . . . yes Br(4) Br(2) C(16) C(19) 175(3) . . . . yes Br(4) Br(2) C(16) C(20) -9(4) . . . . yes Br(4) C(16) C(15) C(14) -173(2) . . . . yes Br(4) C(16) C(15) C(19) -175(6) . . . . yes Br(4) C(16) C(15) C(20) -173(7) . . . . yes Br(4) C(16) C(17) N(1) 172(1) . . . . yes Br(4) C(16) C(17) C(20) 129(13) . . . . yes Br(4) C(16) C(17) C(21) 135(5) . . . . yes Br(4) C(16) C(20) C(15) 177(3) . . . . yes Br(4) C(16) C(20) C(17) -51(5) . . . . yes Br(4) C(16) C(20) C(19) 177(2) . . . . yes Br(4) C(16) C(20) C(21) 140(14) . . . . yes Br(4) C(17) C(16) C(15) -179(2) . . . . yes Br(4) C(17) C(16) C(19) -178(2) . . . . yes Br(4) C(17) C(16) C(20) -129(13) . . . . yes Br(4) C(17) C(20) N(1) -172(1) . . . . yes Br(4) C(17) C(20) C(15) 168(10) . . . . yes Br(4) C(17) C(20) C(16) 49(5) . . . . yes Br(4) C(17) C(20) C(19) 171(8) . . . . yes Br(4) C(17) C(20) C(21) -137(5) . . . . yes Br(4) C(17) C(21) N(1) 170(2) . . . . yes Br(4) C(17) C(21) N(2) 161(2) . . . . yes Br(4) C(17) C(21) C(18) -123(6) . . . . yes Br(4) C(17) C(21) C(20) 105(8) . . . . yes Br(4) C(20) N(1) C(13) 174(3) . . . . yes Br(4) C(20) N(1) C(17) -11(3) . . . . yes Br(4) C(20) N(1) C(18) 0(5) . . . . yes Br(4) C(20) N(1) C(21) 17(4) . . . . yes Br(4) C(20) C(15) C(14) -176(1) . . . . yes Br(4) C(20) C(15) C(16) 2(3) . . . . yes Br(4) C(20) C(15) C(19) -179(8) . . . . yes Br(4) C(20) C(16) C(15) -177(3) . . . . yes Br(4) C(20) C(16) C(17) 51(5) . . . . yes Br(4) C(20) C(16) C(19) -177(2) . . . . yes Br(4) C(20) C(17) N(1) 172(1) . . . . yes Br(4) C(20) C(17) C(16) -49(5) . . . . yes Br(4) C(20) C(17) C(21) 137(5) . . . . yes Br(4) C(20) C(19) C(14) -175(2) . . . . yes Br(4) C(20) C(19) C(15) 0(9) . . . . yes Br(4) C(20) C(19) C(16) 2(2) . . . . yes Br(4) C(20) C(21) N(1) -168(3) . . . . yes Br(4) C(20) C(21) N(2) 178(2) . . . . yes Br(4) C(20) C(21) C(17) -47(6) . . . . yes Br(4) C(20) C(21) C(18) -141(8) . . . . yes Ni(1) S(1) C(1) S(5) 179.1(3) . . . . yes Ni(1) S(1) C(1) C(2) -1.5(5) . . . . yes Ni(1) S(2) C(2) S(6) -179.1(3) . . . . yes Ni(1) S(2) C(2) C(1) -0.4(5) . . . . yes Ni(1) S(3) C(3) S(7) -178.6(3) . . . . yes Ni(1) S(3) C(3) C(4) 0.6(5) . . . . yes Ni(1) S(4) C(4) S(8) 178.4(3) . . . . yes Ni(1) S(4) C(4) C(3) 0.0(5) . . . . yes Ni(2) S(11) C(7) S(15) 179.5(3) . . . . yes Ni(2) S(11) C(7) C(8) 0.0(6) . . . . yes Ni(2) S(12) C(8) S(16) -178.7(3) . . . . yes Ni(2) S(12) C(8) C(7) 1.5(5) . . . . yes Ni(2) S(13) C(9) S(17) 179.6(3) . . . . yes Ni(2) S(13) C(9) C(10) 1.3(5) . . . . yes Ni(2) S(14) C(10) S(18) 179.4(3) . . . . yes Ni(2) S(14) C(10) C(9) -1.1(5) . . . . yes S(1) Ni(1) S(2) C(2) -0.4(2) . . . . yes S(1) Ni(1) S(3) C(3) 176.4(2) . . . . yes S(1) C(1) S(5) C(5) 179.4(4) . . . . yes S(1) C(1) C(2) S(2) 1.3(7) . . . . yes S(1) C(1) C(2) S(6) -179.8(3) . . . . yes S(2) Ni(1) S(1) C(1) 0.9(2) . . . . yes S(2) Ni(1) S(4) C(4) 179.8(2) . . . . yes S(2) C(2) S(6) C(5) 179.3(4) . . . . yes S(2) C(2) C(1) S(5) -179.2(3) . . . . yes S(3) Ni(1) S(1) C(1) -179.6(2) . . . . yes S(3) Ni(1) S(4) C(4) 0.3(2) . . . . yes S(3) C(3) S(7) C(6) 178.1(4) . . . . yes S(3) C(3) C(4) S(4) -0.5(7) . . . . yes S(3) C(3) C(4) S(8) -178.9(3) . . . . yes S(4) Ni(1) S(2) C(2) 176.4(2) . . . . yes S(4) Ni(1) S(3) C(3) -0.5(2) . . . . yes S(4) C(4) S(8) C(6) -177.7(4) . . . . yes S(4) C(4) C(3) S(7) 178.8(3) . . . . yes S(5) C(1) C(2) S(6) -0.3(6) . . . . yes S(5) C(5) S(6) C(2) -0.5(4) . . . . yes S(6) C(5) S(5) C(1) 0.4(4) . . . . yes S(7) C(3) C(4) S(8) 0.3(6) . . . . yes S(7) C(6) S(8) C(4) -1.5(4) . . . . yes S(8) C(6) S(7) C(3) 1.6(4) . . . . yes S(9) C(5) S(5) C(1) 178.4(4) . . . . yes S(9) C(5) S(6) C(2) -178.5(4) . . . . yes S(10) C(6) S(7) C(3) -178.4(4) . . . . yes S(10) C(6) S(8) C(4) 178.5(4) . . . . yes S(11) Ni(2) S(12) C(8) -1.2(2) . . . . yes S(11) Ni(2) S(13) C(9) 179.3(2) . . . . yes S(11) C(7) S(15) C(11) -179.1(4) . . . . yes S(11) C(7) C(8) S(12) -1.0(8) . . . . yes S(11) C(7) C(8) S(16) 179.1(3) . . . . yes S(12) Ni(2) S(11) C(7) 0.8(2) . . . . yes S(12) C(8) S(16) C(11) -179.6(4) . . . . yes S(12) C(8) C(7) S(15) 179.4(3) . . . . yes S(13) Ni(2) S(11) C(7) -177.2(2) . . . . yes S(13) Ni(2) S(14) C(10) 1.4(2) . . . . yes S(13) C(9) S(17) C(12) -179.0(4) . . . . yes S(13) C(9) C(10) S(14) -0.1(8) . . . . yes S(13) C(9) C(10) S(18) 179.4(3) . . . . yes S(14) Ni(2) S(12) C(8) 179.6(2) . . . . yes S(14) Ni(2) S(13) C(9) -1.5(2) . . . . yes S(14) C(10) S(18) C(12) 178.7(4) . . . . yes S(14) C(10) C(9) S(17) -178.5(3) . . . . yes S(15) C(7) C(8) S(16) -0.5(7) . . . . yes S(15) C(11) S(16) C(8) 0.1(4) . . . . yes S(16) C(11) S(15) C(7) -0.3(4) . . . . yes S(17) C(9) C(10) S(18) 1.0(7) . . . . yes S(17) C(12) S(18) C(10) 0.3(4) . . . . yes S(18) C(12) S(17) C(9) 0.1(4) . . . . yes S(19) C(11) S(15) C(7) 179.2(4) . . . . yes S(19) C(11) S(16) C(8) -179.4(5) . . . . yes S(20) C(12) S(17) C(9) 179.8(5) . . . . yes S(20) C(12) S(18) C(10) -179.4(5) . . . . yes N(1) N(2) C(13) C(14) -24(4) . . . . yes N(1) N(2) C(18) C(21) 20(2) . . . . yes N(1) N(2) C(18) C(22) 177(3) . . . . yes N(1) N(2) C(21) C(17) 28(6) . . . . yes N(1) N(2) C(21) C(18) -116(7) . . . . yes N(1) N(2) C(21) C(20) 46(6) . . . . yes N(1) N(2) C(22) C(18) -2(4) . . . . yes N(1) C(13) N(2) C(18) -117(7) . . . . yes N(1) C(13) N(2) C(21) 17(2) . . . . yes N(1) C(13) N(2) C(22) -164(5) . . . . yes N(1) C(13) C(14) C(15) -3(1) . . . . yes N(1) C(13) C(14) C(19) -2(1) . . . . yes N(1) C(17) C(16) C(15) -7(3) . . . . yes N(1) C(17) C(16) C(19) -6(3) . . . . yes N(1) C(17) C(16) C(20) 43(4) . . . . yes N(1) C(17) C(20) C(15) -19(10) . . . . yes N(1) C(17) C(20) C(16) -139(14) . . . . yes N(1) C(17) C(20) C(19) -15(8) . . . . yes N(1) C(17) C(20) C(21) 35(4) . . . . yes N(1) C(17) C(21) N(2) -9(2) . . . . yes N(1) C(17) C(21) C(18) 65(7) . . . . yes N(1) C(17) C(21) C(20) -64(8) . . . . yes N(1) C(18) N(2) C(13) 119(7) . . . . yes N(1) C(18) N(2) C(21) -20(2) . . . . yes N(1) C(18) N(2) C(22) -177(3) . . . . yes N(1) C(18) C(21) N(2) 18(2) . . . . yes N(1) C(18) C(21) C(17) -78(8) . . . . yes N(1) C(18) C(21) C(20) -30(7) . . . . yes N(1) C(18) C(22) N(2) 0(1) . . . . yes N(1) C(20) Br(4) C(16) 179(6) . . . . yes N(1) C(20) Br(4) C(17) 8(2) . . . . yes N(1) C(20) C(15) C(14) 2(2) . . . . yes N(1) C(20) C(15) C(16) -178(5) . . . . yes N(1) C(20) C(15) C(19) 0(8) . . . . yes N(1) C(20) C(16) C(15) 3(9) . . . . yes N(1) C(20) C(16) C(17) -128(13) . . . . yes N(1) C(20) C(16) C(19) 2(8) . . . . yes N(1) C(20) C(17) C(16) 139(14) . . . . yes N(1) C(20) C(17) C(21) -35(4) . . . . yes N(1) C(20) C(19) C(14) 3(3) . . . . yes N(1) C(20) C(19) C(15) 179(7) . . . . yes N(1) C(20) C(19) C(16) -178(4) . . . . yes N(1) C(20) C(21) N(2) -13(1) . . . . yes N(1) C(20) C(21) C(17) 120(8) . . . . yes N(1) C(20) C(21) C(18) 26(6) . . . . yes N(1) C(21) N(2) C(13) -49(6) . . . . yes N(1) C(21) N(2) C(18) 116(7) . . . . yes N(1) C(21) N(2) C(22) 132(7) . . . . yes N(1) C(21) C(17) C(16) 63(7) . . . . yes N(1) C(21) C(17) C(20) 64(8) . . . . yes N(1) C(21) C(18) N(2) -18(2) . . . . yes N(1) C(21) C(18) C(22) -45(4) . . . . yes N(1) C(21) C(20) C(15) 23(5) . . . . yes N(1) C(21) C(20) C(16) 55(6) . . . . yes N(1) C(21) C(20) C(17) -120(8) . . . . yes N(1) C(21) C(20) C(19) 21(5) . . . . yes N(2) N(1) C(13) C(14) 162(3) . . . . yes N(2) N(1) C(17) C(16) -70(12) . . . . yes N(2) N(1) C(17) C(20) -66(13) . . . . yes N(2) N(1) C(17) C(21) 70(13) . . . . yes N(2) N(1) C(18) C(21) -144(4) . . . . yes N(2) N(1) C(18) C(22) -2(3) . . . . yes N(2) N(1) C(20) C(15) -40(6) . . . . yes N(2) N(1) C(20) C(16) -42(11) . . . . yes N(2) N(1) C(20) C(17) 150(6) . . . . yes N(2) N(1) C(20) C(19) -40(6) . . . . yes N(2) N(1) C(20) C(21) 120(7) . . . . yes N(2) N(1) C(21) C(17) -156(5) . . . . yes N(2) N(1) C(21) C(18) 52(5) . . . . yes N(2) N(1) C(21) C(20) -137(5) . . . . yes N(2) C(13) N(1) C(17) -160(3) . . . . yes N(2) C(13) N(1) C(18) 17(2) . . . . yes N(2) C(13) N(1) C(20) -157(3) . . . . yes N(2) C(13) N(1) C(21) -125(7) . . . . yes N(2) C(13) C(14) C(15) 7(2) . . . . yes N(2) C(13) C(14) C(19) 8(2) . . . . yes N(2) C(18) N(1) C(13) -15(2) . . . . yes N(2) C(18) N(1) C(17) 162(3) . . . . yes N(2) C(18) N(1) C(20) 157(4) . . . . yes N(2) C(18) N(1) C(21) 144(4) . . . . yes N(2) C(18) C(21) C(17) -97(9) . . . . yes N(2) C(18) C(21) C(20) -49(8) . . . . yes N(2) C(21) N(1) C(13) 95(8) . . . . yes N(2) C(21) N(1) C(17) 156(5) . . . . yes N(2) C(21) N(1) C(18) -52(5) . . . . yes N(2) C(21) N(1) C(20) 137(5) . . . . yes N(2) C(21) C(17) C(16) 54(8) . . . . yes N(2) C(21) C(17) C(20) 55(8) . . . . yes N(2) C(21) C(18) C(22) -26(3) . . . . yes N(2) C(21) C(20) C(15) 10(5) . . . . yes N(2) C(21) C(20) C(16) 41(4) . . . . yes N(2) C(21) C(20) C(17) -133(7) . . . . yes N(2) C(21) C(20) C(19) 8(5) . . . . yes N(2) C(22) C(18) C(21) 21(2) . . . . yes C(1) C(2) S(6) C(5) 0.5(5) . . . . yes C(2) C(1) S(5) C(5) -0.1(5) . . . . yes C(3) C(4) S(8) C(6) 0.7(5) . . . . yes C(4) C(3) S(7) C(6) -1.2(5) . . . . yes C(7) C(8) S(16) C(11) 0.2(5) . . . . yes C(8) C(7) S(15) C(11) 0.5(5) . . . . yes C(9) C(10) S(18) C(12) -0.8(5) . . . . yes C(10) C(9) S(17) C(12) -0.6(5) . . . . yes C(13) N(1) N(2) C(18) 162(2) . . . . yes C(13) N(1) N(2) C(21) -136(5) . . . . yes C(13) N(1) N(2) C(22) 164(5) . . . . yes C(13) N(1) C(17) C(16) 3(2) . . . . yes C(13) N(1) C(17) C(20) 7(5) . . . . yes C(13) N(1) C(17) C(21) 144(5) . . . . yes C(13) N(1) C(18) C(21) -160(3) . . . . yes C(13) N(1) C(18) C(22) -17(2) . . . . yes C(13) N(1) C(20) C(15) -4(2) . . . . yes C(13) N(1) C(20) C(16) -6(8) . . . . yes C(13) N(1) C(20) C(17) -173(4) . . . . yes C(13) N(1) C(20) C(19) -4(2) . . . . yes C(13) N(1) C(20) C(21) 157(4) . . . . yes C(13) N(1) C(21) C(17) -61(8) . . . . yes C(13) N(1) C(21) C(18) 147(5) . . . . yes C(13) N(1) C(21) C(20) -42(7) . . . . yes C(13) N(2) N(1) C(17) 84(11) . . . . yes C(13) N(2) N(1) C(18) -162(2) . . . . yes C(13) N(2) N(1) C(20) 45(6) . . . . yes C(13) N(2) N(1) C(21) 136(5) . . . . yes C(13) N(2) C(18) C(21) 139(6) . . . . yes C(13) N(2) C(18) C(22) -62(6) . . . . yes C(13) N(2) C(21) C(17) -20(6) . . . . yes C(13) N(2) C(21) C(18) -165(2) . . . . yes C(13) N(2) C(21) C(20) -2(4) . . . . yes C(13) N(2) C(22) C(18) 157(3) . . . . yes C(13) C(14) C(15) C(16) 0(2) . . . . yes C(13) C(14) C(15) C(19) 2(5) . . . . yes C(13) C(14) C(15) C(20) 0(1) . . . . yes C(13) C(14) C(19) C(15) -178(4) . . . . yes C(13) C(14) C(19) C(16) -2(6) . . . . yes C(13) C(14) C(19) C(20) -1(3) . . . . yes C(14) C(13) N(1) C(17) 1(2) . . . . yes C(14) C(13) N(1) C(18) -179(1) . . . . yes C(14) C(13) N(1) C(20) 4(1) . . . . yes C(14) C(13) N(1) C(21) 36(6) . . . . yes C(14) C(13) N(2) C(18) -141(4) . . . . yes C(14) C(13) N(2) C(21) -6(3) . . . . yes C(14) C(13) N(2) C(22) 171(1) . . . . yes C(14) C(15) C(16) C(17) 5(2) . . . . yes C(14) C(15) C(16) C(19) 2(5) . . . . yes C(14) C(15) C(16) C(20) 0(4) . . . . yes C(14) C(15) C(19) C(16) -177(5) . . . . yes C(14) C(15) C(19) C(20) -176(9) . . . . yes C(14) C(15) C(20) C(16) -179(4) . . . . yes C(14) C(15) C(20) C(17) 16(9) . . . . yes C(14) C(15) C(20) C(19) 2(7) . . . . yes C(14) C(15) C(20) C(21) -8(3) . . . . yes C(14) C(19) C(15) C(16) 177(5) . . . . yes C(14) C(19) C(15) C(20) 176(9) . . . . yes C(14) C(19) C(16) C(15) -175(10) . . . . yes C(14) C(19) C(16) C(17) 7(6) . . . . yes C(14) C(19) C(16) C(20) 3(7) . . . . yes C(14) C(19) C(20) C(15) -176(10) . . . . yes C(14) C(19) C(20) C(16) -178(4) . . . . yes C(14) C(19) C(20) C(17) 14(9) . . . . yes C(14) C(19) C(20) C(21) -6(5) . . . . yes C(15) C(14) C(19) C(16) 175(10) . . . . yes C(15) C(14) C(19) C(20) 177(7) . . . . yes C(15) C(16) Br(4) C(17) 179(4) . . . . yes C(15) C(16) Br(4) C(20) 174(6) . . . . yes C(15) C(16) C(17) C(20) -52(5) . . . . yes C(15) C(16) C(17) C(21) -44(6) . . . . yes C(15) C(16) C(19) C(20) -178(6) . . . . yes C(15) C(16) C(20) C(17) 131(13) . . . . yes C(15) C(16) C(20) C(19) 0(2) . . . . yes C(15) C(16) C(20) C(21) -38(4) . . . . yes C(15) C(19) C(16) C(17) -177(5) . . . . yes C(15) C(19) C(16) C(20) 178(6) . . . . yes C(15) C(19) C(20) C(16) -1(8) . . . . yes C(15) C(19) C(20) C(17) -169(9) . . . . yes C(15) C(19) C(20) C(21) 169(7) . . . . yes C(15) C(20) Br(4) C(16) -1(2) . . . . yes C(15) C(20) Br(4) C(17) -173(5) . . . . yes C(15) C(20) N(1) C(17) 169(5) . . . . yes C(15) C(20) N(1) C(18) -177(1) . . . . yes C(15) C(20) N(1) C(21) -161(4) . . . . yes C(15) C(20) C(16) C(17) -131(13) . . . . yes C(15) C(20) C(16) C(19) 0(2) . . . . yes C(15) C(20) C(17) C(16) 117(12) . . . . yes C(15) C(20) C(17) C(21) -54(12) . . . . yes C(15) C(20) C(19) C(16) 1(8) . . . . yes C(15) C(20) C(21) C(17) 144(7) . . . . yes C(15) C(20) C(21) C(18) 50(11) . . . . yes C(16) Br(2) Br(4) C(17) 8.6(9) . . . . yes C(16) Br(2) Br(4) C(20) 2(1) . . . . yes C(16) Br(4) C(17) C(20) -4(4) . . . . yes C(16) Br(4) C(17) C(21) -137(6) . . . . yes C(16) Br(4) C(20) C(17) 171(7) . . . . yes C(16) Br(4) C(20) C(19) -2(2) . . . . yes C(16) Br(4) C(20) C(21) -171(5) . . . . yes C(16) C(15) C(14) C(19) -2(5) . . . . yes C(16) C(15) C(19) C(20) 0(4) . . . . yes C(16) C(15) C(20) C(17) -164(12) . . . . yes C(16) C(15) C(20) C(19) -177(10) . . . . yes C(16) C(15) C(20) C(21) 170(7) . . . . yes C(16) C(17) Br(4) C(20) 4(4) . . . . yes C(16) C(17) N(1) C(18) -175(1) . . . . yes C(16) C(17) N(1) C(20) -4(3) . . . . yes C(16) C(17) N(1) C(21) -141(6) . . . . yes C(16) C(17) C(20) C(19) 121(12) . . . . yes C(16) C(17) C(20) C(21) 175(18) . . . . yes C(16) C(17) C(21) C(18) 129(7) . . . . yes C(16) C(17) C(21) C(20) 0(3) . . . . yes C(16) C(19) C(15) C(20) 0(4) . . . . yes C(16) C(19) C(20) C(17) -167(10) . . . . yes C(16) C(19) C(20) C(21) 171(6) . . . . yes C(16) C(20) Br(4) C(17) -171(7) . . . . yes C(16) C(20) N(1) C(17) 167(11) . . . . yes C(16) C(20) N(1) C(18) 179(6) . . . . yes C(16) C(20) N(1) C(21) -163(9) . . . . yes C(16) C(20) C(15) C(19) 177(10) . . . . yes C(16) C(20) C(17) C(21) -175(18) . . . . yes C(16) C(20) C(21) C(17) 174(18) . . . . yes C(16) C(20) C(21) C(18) 79(8) . . . . yes C(17) Br(4) C(16) C(20) 4(3) . . . . yes C(17) Br(4) C(20) C(19) -173(6) . . . . yes C(17) Br(4) C(20) C(21) 16(3) . . . . yes C(17) N(1) N(2) C(18) -112(11) . . . . yes C(17) N(1) N(2) C(21) -51(10) . . . . yes C(17) N(1) N(2) C(22) -110(11) . . . . yes C(17) N(1) C(18) C(21) 17(3) . . . . yes C(17) N(1) C(18) C(22) 160(2) . . . . yes C(17) N(1) C(20) C(19) 169(5) . . . . yes C(17) N(1) C(20) C(21) -29(5) . . . . yes C(17) N(1) C(21) C(18) -151(4) . . . . yes C(17) N(1) C(21) C(20) 18(3) . . . . yes C(17) C(16) Br(4) C(20) -4(3) . . . . yes C(17) C(16) C(15) C(19) 3(6) . . . . yes C(17) C(16) C(15) C(20) 5(3) . . . . yes C(17) C(16) C(19) C(20) 4(3) . . . . yes C(17) C(16) C(20) C(19) -131(13) . . . . yes C(17) C(16) C(20) C(21) -169(17) . . . . yes C(17) C(20) N(1) C(18) 12(5) . . . . yes C(17) C(20) N(1) C(21) 29(5) . . . . yes C(17) C(20) C(15) C(19) 13(11) . . . . yes C(17) C(20) C(16) C(19) 131(13) . . . . yes C(17) C(20) C(21) C(18) -94(11) . . . . yes C(17) C(21) N(1) C(18) 151(4) . . . . yes C(17) C(21) N(1) C(20) -18(3) . . . . yes C(17) C(21) N(2) C(18) 144(5) . . . . yes C(17) C(21) N(2) C(22) 160(5) . . . . yes C(17) C(21) C(18) C(22) -124(8) . . . . yes C(17) C(21) C(20) C(19) 142(7) . . . . yes C(18) N(1) N(2) C(21) 61(6) . . . . yes C(18) N(1) N(2) C(22) 1(2) . . . . yes C(18) N(1) C(17) C(20) -170(4) . . . . yes C(18) N(1) C(17) C(21) -33(5) . . . . yes C(18) N(1) C(20) C(19) -178(2) . . . . yes C(18) N(1) C(20) C(21) -16(4) . . . . yes C(18) N(1) C(21) C(20) 169(2) . . . . yes C(18) N(2) N(1) C(20) -151(4) . . . . yes C(18) N(2) N(1) C(21) -61(6) . . . . yes C(18) N(2) C(21) C(20) 163(3) . . . . yes C(18) C(21) N(1) C(20) -169(2) . . . . yes C(18) C(21) N(2) C(22) 15(2) . . . . yes C(18) C(21) C(17) C(20) 130(8) . . . . yes C(18) C(21) C(20) C(19) 48(11) . . . . yes C(18) C(22) N(2) C(21) -24(3) . . . . yes C(19) C(14) C(15) C(20) -1(5) . . . . yes C(19) C(15) C(16) C(20) -1(7) . . . . yes C(19) C(15) C(20) C(21) -11(8) . . . . yes C(19) C(16) C(15) C(20) 1(7) . . . . yes C(19) C(16) C(17) C(20) -51(5) . . . . yes C(19) C(16) C(17) C(21) -42(6) . . . . yes C(19) C(16) C(20) C(21) -38(4) . . . . yes C(19) C(20) N(1) C(21) -161(4) . . . . yes C(19) C(20) C(17) C(21) -50(10) . . . . yes C(20) Br(4) C(17) C(21) -132(7) . . . . yes C(20) N(1) N(2) C(21) -90(8) . . . . yes C(20) N(1) N(2) C(22) -150(4) . . . . yes C(20) N(1) C(17) C(21) 136(7) . . . . yes C(20) N(1) C(18) C(21) 12(3) . . . . yes C(20) N(1) C(18) C(22) 155(3) . . . . yes C(20) C(16) C(17) C(21) 6(1) . . . . yes C(20) C(17) N(1) C(21) -136(7) . . . . yes C(20) C(21) N(2) C(22) 178(3) . . . . yes C(20) C(21) C(18) C(22) -75(10) . . . . yes C(21) N(1) N(2) C(22) -59(8) . . . . yes C(21) N(1) C(18) C(22) 142(3) . . . . yes C(21) N(2) C(18) C(22) 157(2) . . . . yes C(21) C(18) N(2) C(22) -157(2) . . . . yes C(21) C(18) N(2) C(22) -157(2) . . . . 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 Br(1) S(19) 3.240(5) . 2_656 ? Br(2) S(20) 3.081(3) . 2_767 ? Br(2) C(11) 3.593(7) . 1_655 ? Br(3) S(19) 3.401(7) . 2_656 ? Br(4) C(21) 3.27(4) . 2_766 ? Br(4) S(10) 3.510(4) . 2_767 ? Br(4) C(17) 3.51(2) . 2_766 ? S(1) S(14) 3.574(3) . 1_655 ? S(2) S(14) 3.572(2) . 2_657 ? S(3) S(13) 3.585(2) . 2_767 ? S(4) S(14) 3.543(2) . 2_657 ? S(4) S(12) 3.596(2) . 2_657 ? S(10) C(13) 3.469(8) . 1_556 ? S(10) C(14) 3.573(6) . 1_556 ? S(15) C(18) 3.47(2) . 2_666 ? S(19) C(15) 3.50(2) . 1_455 ? S(19) C(16) 3.58(2) . 1_455 ? S(20) C(22) 3.36(3) . 1_556 ? data_2 _database_code_depnum_ccdc_archive 'CCDC 910062' #TrackingRef '16104_web_deposit_cif_file_1_HiroshiM.Yamamoto_1355276590.2.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C24 H6 I2 N Ni3 S30 ' _chemical_formula_moiety 'C6 H6 I2 N, 3(C6 Ni S10)' _chemical_formula_weight 1700.03 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c ' _symmetry_space_group_name_Hall '-C 2yc' _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 35.368(7) _cell_length_b 11.088(2) _cell_length_c 13.129(3) _cell_angle_alpha 90 _cell_angle_beta 103.317(3) _cell_angle_gamma 90 _cell_volume 5010.2(18) _cell_formula_units_Z 4 _cell_measurement_reflns_used 6270 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 295.0 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Black _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.254 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3308.00 _exptl_absorpt_coefficient_mu 3.627 _exptl_absorpt_correction_type Numerical _exptl_absorpt_correction_T_max 0.8541 _exptl_absorpt_correction_T_min 0.5685 _exptl_absorpt_process_details 'Rigaku/MSC CrysatalClear' #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku/MSC Mercury CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.71 _diffrn_reflns_number 20627 _diffrn_reflns_av_R_equivalents 0.031 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 27.48 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 #------------------------------------------------------------------------------ # 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 5731 _reflns_number_gt 3981 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.1034 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5731 _refine_ls_number_parameters 287 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max -0.0010 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.82 _refine_diff_density_min -1.01 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 I(1) I 0.94414(3) 1.0218(2) 0.52580(9) 0.1162(6) Uani 0.50 2 d P . 1 I(2) I 0.95125(3) 0.94715(8) 0.54333(8) 0.0577(2) Uani 0.50 2 d P . 2 Ni(1) Ni 0.7500 0.7500 0.0000 0.0351(2) Uani 1.00 2 d S . . Ni(2) Ni 0.79376(2) 0.41628(5) 0.07556(4) 0.0392(1) Uani 1.00 1 d . . . S(1) S 0.76542(3) 0.7882(1) 0.16546(7) 0.0398(2) Uani 1.00 1 d . . . S(2) S 0.80911(3) 0.7049(1) -0.00639(8) 0.0426(3) Uani 1.00 1 d . . . S(3) S 0.84273(3) 0.7780(1) 0.32159(8) 0.0418(2) Uani 1.00 1 d . . . S(4) S 0.88278(3) 0.6986(1) 0.16534(9) 0.0458(3) Uani 1.00 1 d . . . S(5) S 0.92710(4) 0.7229(1) 0.3864(1) 0.0604(3) Uani 1.00 1 d . . . S(6) S 0.81512(3) 0.4414(1) 0.24144(8) 0.0455(3) Uani 1.00 1 d . . . S(7) S 0.85051(3) 0.3723(1) 0.05244(9) 0.0474(3) Uani 1.00 1 d . . . S(8) S 0.73731(3) 0.4647(1) 0.09776(8) 0.0456(3) Uani 1.00 1 d . . . S(9) S 0.77130(3) 0.3773(1) -0.08790(8) 0.0445(3) Uani 1.00 1 d . . . S(10) S 0.89514(4) 0.4014(1) 0.3819(1) 0.0580(3) Uani 1.00 1 d . . . S(11) S 0.92833(3) 0.3485(1) 0.2041(1) 0.0569(3) Uani 1.00 1 d . . . S(12) S 0.65852(3) 0.4723(1) -0.05060(9) 0.0474(3) Uani 1.00 1 d . . . S(13) S 0.69002(4) 0.3878(1) -0.22419(9) 0.0497(3) Uani 1.00 1 d . . . S(14) S 0.97953(4) 0.3491(2) 0.4176(1) 0.0940(6) Uani 1.00 1 d . . . S(15) S 0.60645(4) 0.4456(1) -0.2631(1) 0.0641(4) Uani 1.00 1 d . . . N(1) N 1.0000 1.2530(6) 0.7500 0.071(2) Uani 1.00 2 d S . . C(1) C 0.8141(1) 0.7608(3) 0.1956(3) 0.0356(8) Uani 1.00 1 d . . . C(2) C 0.8332(1) 0.7246(4) 0.1215(3) 0.0355(9) Uani 1.00 1 d . . . C(3) C 0.8866(1) 0.7338(4) 0.2961(3) 0.0429(10) Uani 1.00 1 d . . . C(4) C 0.8631(1) 0.4050(4) 0.2597(3) 0.0415(9) Uani 1.00 1 d . . . C(5) C 0.8785(1) 0.3771(4) 0.1758(3) 0.0412(9) Uani 1.00 1 d . . . C(6) C 0.7081(1) 0.4445(4) -0.0222(3) 0.0378(9) Uani 1.00 1 d . . . C(7) C 0.7232(1) 0.4049(4) -0.1049(3) 0.0393(9) Uani 1.00 1 d . . . C(8) C 0.9364(1) 0.3656(4) 0.3391(4) 0.058(1) Uani 1.00 1 d . . . C(9) C 0.6492(1) 0.4357(4) -0.1830(4) 0.046(1) Uani 1.00 1 d . . . C(10) C 0.9801(2) 1.1912(7) 0.6660(4) 0.072(2) Uani 1.00 1 d . . . C(11) C 0.9800(1) 1.0677(6) 0.6660(4) 0.058(1) Uani 1.00 1 d . . . C(12) C 1.0000 1.0083(7) 0.7500 0.059(2) Uani 1.00 2 d S . . C(13) C 0.9910(3) 1.3867(8) 0.7210(10) 0.063(3) Uani 0.50 2 d P . . H(1) H 0.9658 1.2353 0.6056 0.0878 Uiso 1.00 1 calc . . . H(2) H 1.0000 0.9210 0.7500 0.0848 Uiso 1.00 2 calc S . . H(3) H 1.0146 1.4301 0.7195 0.0820 Uiso 0.50 2 calc P . . H(4) H 0.9801 1.4259 0.7743 0.0820 Uiso 0.50 2 calc P . . H(5) H 0.9733 1.3956 0.6562 0.0820 Uiso 0.50 2 calc P . . 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 I(1) 0.0681(7) 0.229(2) 0.0513(6) -0.0659(10) 0.0127(5) -0.0489(9) I(2) 0.0496(4) 0.0695(6) 0.0545(5) -0.0130(4) 0.0131(3) -0.0109(4) Ni(1) 0.0371(4) 0.0400(4) 0.0271(4) 0.0019(3) 0.0051(3) -0.0028(3) Ni(2) 0.0401(3) 0.0413(3) 0.0392(3) -0.0010(2) 0.0156(2) -0.0033(2) S(1) 0.0392(5) 0.0515(7) 0.0285(5) 0.0054(5) 0.0069(4) -0.0031(4) S(2) 0.0397(6) 0.0569(7) 0.0306(5) 0.0034(5) 0.0068(4) -0.0079(5) S(3) 0.0413(6) 0.0530(7) 0.0291(5) -0.0049(5) 0.0044(4) -0.0018(4) S(4) 0.0355(6) 0.0590(7) 0.0421(6) 0.0013(5) 0.0069(5) -0.0065(5) S(5) 0.0410(6) 0.0789(9) 0.0530(7) -0.0041(6) -0.0063(5) -0.0059(6) S(6) 0.0454(6) 0.0547(7) 0.0398(6) 0.0033(5) 0.0167(5) -0.0034(5) S(7) 0.0431(6) 0.0577(7) 0.0450(6) -0.0028(5) 0.0177(5) -0.0104(5) S(8) 0.0454(6) 0.0559(7) 0.0390(6) 0.0053(5) 0.0169(5) -0.0029(5) S(9) 0.0459(6) 0.0514(7) 0.0405(6) -0.0012(5) 0.0186(5) -0.0045(5) S(10) 0.0531(7) 0.0716(9) 0.0474(7) -0.0017(6) 0.0077(6) 0.0028(6) S(11) 0.0420(6) 0.0654(8) 0.0660(8) 0.0002(6) 0.0181(6) 0.0026(6) S(12) 0.0432(6) 0.0535(7) 0.0474(6) 0.0042(5) 0.0143(5) 0.0056(5) S(13) 0.0542(7) 0.0568(7) 0.0393(6) -0.0070(6) 0.0132(5) 0.0004(5) S(14) 0.0495(9) 0.141(2) 0.085(1) -0.0026(9) 0.0014(8) 0.044(1) S(15) 0.0537(8) 0.0748(9) 0.0578(8) -0.0062(7) 0.0005(6) 0.0148(7) N(1) 0.078(5) 0.056(4) 0.099(6) 0.0000 0.061(5) 0.0000 C(1) 0.040(2) 0.035(2) 0.029(2) -0.002(2) 0.002(2) 0.005(2) C(2) 0.033(2) 0.038(2) 0.034(2) -0.001(2) 0.004(2) 0.004(2) C(3) 0.048(2) 0.037(2) 0.042(2) -0.005(2) 0.006(2) 0.002(2) C(4) 0.046(2) 0.036(2) 0.041(2) -0.003(2) 0.007(2) 0.000(2) C(5) 0.037(2) 0.037(2) 0.052(3) -0.003(2) 0.016(2) -0.002(2) C(6) 0.039(2) 0.034(2) 0.042(2) -0.001(2) 0.013(2) 0.007(2) C(7) 0.045(2) 0.032(2) 0.042(2) -0.008(2) 0.012(2) 0.005(2) C(8) 0.051(3) 0.057(3) 0.067(3) -0.004(2) 0.013(3) 0.018(3) C(9) 0.054(3) 0.037(2) 0.047(3) -0.007(2) 0.010(2) 0.009(2) C(10) 0.049(3) 0.117(6) 0.055(3) 0.024(3) 0.023(3) 0.039(3) C(11) 0.037(3) 0.096(4) 0.042(3) -0.009(3) 0.009(2) -0.004(3) C(12) 0.051(4) 0.064(5) 0.062(5) 0.0000 0.013(4) 0.0000 C(13) 0.060(10) 0.044(5) 0.09(1) -0.004(5) 0.020(6) -0.013(5) #------------------------------------------------------------------------------ _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR97 _computing_structure_refinement SHELXL97 _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 I(1) I(2) 0.881(2) . . yes I(1) C(11) 2.044(4) . . yes I(2) C(11) 2.158(5) . . yes Ni(1) S(1) 2.1564(9) . . yes Ni(1) S(1) 2.1564(9) . 7_665 yes Ni(1) S(2) 2.170(1) . . yes Ni(1) S(2) 2.170(1) . 7_665 yes Ni(2) S(6) 2.152(1) . . yes Ni(2) S(7) 2.154(1) . . yes Ni(2) S(8) 2.151(1) . . yes Ni(2) S(9) 2.154(1) . . yes S(1) C(1) 1.704(4) . . yes S(2) C(2) 1.712(4) . . yes S(3) C(1) 1.739(4) . . yes S(3) C(3) 1.732(5) . . yes S(4) C(2) 1.741(4) . . yes S(4) C(3) 1.735(4) . . yes S(5) C(3) 1.640(4) . . yes S(6) C(4) 1.706(4) . . yes S(7) C(5) 1.694(4) . . yes S(8) C(6) 1.687(4) . . yes S(9) C(7) 1.691(4) . . yes S(10) C(4) 1.739(4) . . yes S(10) C(8) 1.726(6) . . yes S(11) C(5) 1.745(4) . . yes S(11) C(8) 1.739(6) . . yes S(12) C(6) 1.736(4) . . yes S(12) C(9) 1.741(5) . . yes S(13) C(7) 1.738(4) . . yes S(13) C(9) 1.737(5) . . yes S(14) C(8) 1.643(5) . . yes S(15) C(9) 1.635(4) . . yes N(1) C(10) 1.351(6) . . yes N(1) C(10) 1.351(6) . 2_756 yes N(1) C(13) 1.55(1) . . yes N(1) C(13) 1.55(1) . 2_756 yes C(1) C(2) 1.364(6) . . yes C(4) C(5) 1.372(7) . . yes C(6) C(7) 1.387(6) . . yes C(10) C(11) 1.369(10) . . yes C(11) C(12) 1.339(6) . . yes C(13) C(13) 0.87(2) . 2_756 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 I(2) I(1) C(11) 85.3(2) . . . yes I(1) I(2) C(11) 70.7(2) . . . yes S(1) Ni(1) S(1) 180.0 . . 7_665 yes S(1) Ni(1) S(2) 93.55(4) . . . yes S(1) Ni(1) S(2) 86.45(4) . . 7_665 yes S(1) Ni(1) S(2) 86.45(4) 7_665 . . yes S(1) Ni(1) S(2) 93.55(4) 7_665 . 7_665 yes S(2) Ni(1) S(2) 180.0 . . 7_665 yes S(6) Ni(2) S(7) 92.90(5) . . . yes S(6) Ni(2) S(8) 87.20(5) . . . yes S(6) Ni(2) S(9) 175.64(5) . . . yes S(7) Ni(2) S(8) 178.59(5) . . . yes S(7) Ni(2) S(9) 87.48(5) . . . yes S(8) Ni(2) S(9) 92.54(5) . . . yes Ni(1) S(1) C(1) 101.9(1) . . . yes Ni(1) S(2) C(2) 101.4(1) . . . yes C(1) S(3) C(3) 97.8(2) . . . yes C(2) S(4) C(3) 97.6(2) . . . yes Ni(2) S(6) C(4) 102.6(2) . . . yes Ni(2) S(7) C(5) 102.5(2) . . . yes Ni(2) S(8) C(6) 103.1(2) . . . yes Ni(2) S(9) C(7) 103.0(2) . . . yes C(4) S(10) C(8) 97.2(2) . . . yes C(5) S(11) C(8) 96.8(2) . . . yes C(6) S(12) C(9) 97.0(2) . . . yes C(7) S(13) C(9) 97.1(2) . . . yes C(10) N(1) C(10) 119.1(7) . . 2_756 yes C(10) N(1) C(13) 104.2(5) . . . yes C(10) N(1) C(13) 136.6(6) . . 2_756 yes C(10) N(1) C(13) 136.6(6) 2_756 . . yes C(10) N(1) C(13) 104.2(5) 2_756 . 2_756 yes S(1) C(1) S(3) 122.5(2) . . . yes S(1) C(1) C(2) 121.6(3) . . . yes S(3) C(1) C(2) 115.9(3) . . . yes S(2) C(2) S(4) 122.6(3) . . . yes S(2) C(2) C(1) 121.5(3) . . . yes S(4) C(2) C(1) 116.0(3) . . . yes S(3) C(3) S(4) 112.7(2) . . . yes S(3) C(3) S(5) 123.6(3) . . . yes S(4) C(3) S(5) 123.7(3) . . . yes S(6) C(4) S(10) 123.5(3) . . . yes S(6) C(4) C(5) 120.4(3) . . . yes S(10) C(4) C(5) 116.1(3) . . . yes S(7) C(5) S(11) 122.5(3) . . . yes S(7) C(5) C(4) 121.5(3) . . . yes S(11) C(5) C(4) 116.0(3) . . . yes S(8) C(6) S(12) 123.2(3) . . . yes S(8) C(6) C(7) 120.7(3) . . . yes S(12) C(6) C(7) 116.1(3) . . . yes S(9) C(7) S(13) 123.3(3) . . . yes S(9) C(7) C(6) 120.7(3) . . . yes S(13) C(7) C(6) 115.9(3) . . . yes S(10) C(8) S(11) 113.9(3) . . . yes S(10) C(8) S(14) 123.6(3) . . . yes S(11) C(8) S(14) 122.5(3) . . . yes S(12) C(9) S(13) 113.7(2) . . . yes S(12) C(9) S(15) 124.1(3) . . . yes S(13) C(9) S(15) 122.1(3) . . . yes N(1) C(10) C(11) 120.5(5) . . . yes I(1) C(11) C(10) 104.5(3) . . . yes I(1) C(11) C(12) 136.1(5) . . . yes I(2) C(11) C(10) 128.3(3) . . . yes I(2) C(11) C(12) 112.3(4) . . . yes C(10) C(11) C(12) 119.4(5) . . . yes C(11) C(12) C(11) 121.1(7) . . 2_756 yes N(1) C(13) C(13) 73.6(4) . . 2_756 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 I(1) I(2) C(11) C(10) -6.9(5) . . . . yes I(1) I(2) C(11) C(12) 173.7(4) . . . . yes I(1) C(11) C(10) N(1) 177.6(4) . . . . yes I(1) C(11) C(12) C(11) -176.8(6) . . . 2_756 yes I(2) I(1) C(11) C(10) 174.4(4) . . . . yes I(2) I(1) C(11) C(12) -8.4(5) . . . . yes I(2) C(11) C(10) N(1) -179.6(3) . . . . yes I(2) C(11) C(12) C(11) 179.6(4) . . . 2_756 yes Ni(1) S(1) C(1) S(3) 179.7(2) . . . . yes Ni(1) S(1) C(1) C(2) 0.2(4) . . . . yes Ni(1) S(1) C(1) S(3) -179.7(2) . 7_665 7_665 7_665 yes Ni(1) S(1) C(1) C(2) -0.2(4) . 7_665 7_665 7_665 yes Ni(1) S(2) C(2) S(4) 179.0(2) . . . . yes Ni(1) S(2) C(2) C(1) -0.4(4) . . . . yes Ni(1) S(2) C(2) S(4) -179.0(2) . 7_665 7_665 7_665 yes Ni(1) S(2) C(2) C(1) 0.4(4) . 7_665 7_665 7_665 yes Ni(2) S(6) C(4) S(10) -176.7(2) . . . . yes Ni(2) S(6) C(4) C(5) 3.8(4) . . . . yes Ni(2) S(7) C(5) S(11) -179.9(2) . . . . yes Ni(2) S(7) C(5) C(4) -0.3(4) . . . . yes Ni(2) S(8) C(6) S(12) -179.3(2) . . . . yes Ni(2) S(8) C(6) C(7) 0.1(4) . . . . yes Ni(2) S(9) C(7) S(13) -179.9(2) . . . . yes Ni(2) S(9) C(7) C(6) 0.8(4) . . . . yes S(1) Ni(1) S(2) C(2) 0.4(1) . . . . yes S(1) Ni(1) S(2) C(2) 179.6(1) . . 7_665 7_665 yes S(1) C(1) S(3) C(3) 178.8(3) . . . . yes S(1) C(1) C(2) S(2) 0.2(5) . . . . yes S(1) C(1) C(2) S(4) -179.2(2) . . . . yes S(2) Ni(1) S(1) C(1) -0.3(1) . . . . yes S(2) Ni(1) S(1) C(1) -179.7(1) . . 7_665 7_665 yes S(2) C(2) S(4) C(3) -179.5(3) . . . . yes S(2) C(2) C(1) S(3) -179.4(2) . . . . yes S(3) C(1) C(2) S(4) 1.2(4) . . . . yes S(3) C(3) S(4) C(2) -1.0(3) . . . . yes S(4) C(3) S(3) C(1) 1.5(3) . . . . yes S(5) C(3) S(3) C(1) -177.0(3) . . . . yes S(5) C(3) S(4) C(2) 177.5(3) . . . . yes S(6) Ni(2) S(7) C(5) 2.1(2) . . . . yes S(6) Ni(2) S(8) C(6) -175.3(2) . . . . yes S(6) C(4) S(10) C(8) -177.7(3) . . . . yes S(6) C(4) C(5) S(7) -2.5(5) . . . . yes S(6) C(4) C(5) S(11) 177.1(2) . . . . yes S(7) Ni(2) S(6) C(4) -3.1(2) . . . . yes S(7) Ni(2) S(9) C(7) -179.2(1) . . . . yes S(7) C(5) S(11) C(8) -178.7(3) . . . . yes S(7) C(5) C(4) S(10) 177.9(2) . . . . yes S(8) Ni(2) S(6) C(4) 178.4(2) . . . . yes S(8) Ni(2) S(9) C(7) -0.6(2) . . . . yes S(8) C(6) S(12) C(9) 178.9(3) . . . . yes S(8) C(6) C(7) S(9) -0.7(5) . . . . yes S(8) C(6) C(7) S(13) -180.0(2) . . . . yes S(9) Ni(2) S(7) C(5) -173.6(2) . . . . yes S(9) Ni(2) S(8) C(6) 0.3(2) . . . . yes S(9) C(7) S(13) C(9) -177.9(3) . . . . yes S(9) C(7) C(6) S(12) 178.8(2) . . . . yes S(10) C(4) C(5) S(11) -2.5(5) . . . . yes S(10) C(8) S(11) C(5) -0.4(3) . . . . yes S(11) C(8) S(10) C(4) -0.7(3) . . . . yes S(12) C(6) C(7) S(13) -0.6(4) . . . . yes S(12) C(9) S(13) C(7) -1.7(3) . . . . yes S(13) C(9) S(12) C(6) 1.4(3) . . . . yes S(14) C(8) S(10) C(4) 179.2(3) . . . . yes S(14) C(8) S(11) C(5) 179.7(3) . . . . yes S(15) C(9) S(12) C(6) -178.1(3) . . . . yes S(15) C(9) S(13) C(7) 177.9(3) . . . . yes N(1) C(10) C(11) C(12) -0.2(8) . . . . yes N(1) C(10) C(11) C(12) -0.2(8) . 2_756 2_756 . yes C(1) C(2) S(4) C(3) -0.1(4) . . . . yes C(2) C(1) S(3) C(3) -1.6(3) . . . . yes C(4) C(5) S(11) C(8) 1.7(4) . . . . yes C(5) C(4) S(10) C(8) 1.9(4) . . . . yes C(6) C(7) S(13) C(9) 1.4(4) . . . . yes C(7) C(6) S(12) C(9) -0.5(4) . . . . yes C(10) N(1) C(10) C(11) 0.1(4) . . 2_756 2_756 yes C(10) N(1) C(13) C(13) -171(1) . . . 2_756 yes C(10) N(1) C(13) C(13) 11(2) . . 2_756 . yes C(10) C(11) C(12) C(11) 0.1(4) . . . 2_756 yes C(11) C(10) N(1) C(13) -177.3(7) . . . . yes C(11) C(10) N(1) C(13) 176.4(8) . . . 2_756 yes C(11) C(10) N(1) C(13) 176.4(8) . . . 2_756 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 I(1) S(15) 3.519(2) . 7_665 ? I(2) S(5) 3.217(2) . . ? Ni(1) S(8) 3.481(1) . . ? Ni(1) S(8) 3.481(1) . 7_665 ? Ni(2) S(2) 3.459(1) . . ? S(1) C(7) 3.539(4) . 7_665 ? S(3) S(7) 3.414(2) . 4_565 ? S(3) S(9) 3.485(2) . 4_565 ? S(4) C(5) 3.572(4) . . ? S(5) N(1) 3.471(2) . 3_776 ? S(6) C(1) 3.592(4) . . ? S(8) S(13) 3.569(2) . 4_565 ? S(12) C(2) 3.518(4) . 7_665 ? S(15) C(3) 3.596(4) . 7_665 ? data_KCE286_smp3_ip1234 _database_code_depnum_ccdc_archive 'CCDC 910623' #TrackingRef '16107_web_deposit_cif_file_4_HiroshiM.Yamamoto_1355276590.5.cif' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C18 H6 Br I N Ni2 S20 ' _chemical_formula_moiety ? _chemical_formula_weight 1201.66 _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 14.218(4) _cell_length_b 6.436(1) _cell_length_c 76.15(2) _cell_angle_alpha 90 _cell_angle_beta 93.836(9) _cell_angle_gamma 90 _cell_volume 6952.7 _cell_formula_units_Z 8 _cell_measurement_reflns_used 8636 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 296.2 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Black _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.297 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4680.00 _exptl_absorpt_coefficient_mu 4.348 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_ambient_temperature 296.2 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type ? _diffrn_reflns_number 13033 _diffrn_reflns_av_R_equivalents 0.071 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -98 _diffrn_reflns_limit_l_max 98 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.99 #------------------------------------------------------------------------------ # 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 7838 _reflns_number_gt 5884 _reflns_threshold_expression >2.0sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1734 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7838 _refine_ls_number_parameters 389 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.0030 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0000 _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_diff_density_max 0.70 _refine_diff_density_min -1.42 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 6.1.1.4) ; H H 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Br Br -0.290 2.459 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #------------------------------------------------------------------------------ # 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 I(1) I 0.35052(5) -0.5322(1) 0.62313(1) 0.0853(3) Uani 0.33 3 d P . . I(2) I 0.48902(3) 0.21055(8) 0.66400(1) 0.0609(2) Uani 0.67 1 d P . . Br(1) Br 0.48902(3) 0.21055(8) 0.66400(1) 0.0609(2) Uani 0.33 3 d P . . Br(2) Br 0.35052(5) -0.5322(1) 0.62313(1) 0.0853(3) Uani 0.67 1 d P . . Ni(1) Ni 0.32949(5) 0.3330(1) 0.72708(1) 0.0411(2) Uani 1.00 1 d . . . Ni(2) Ni 0.35688(6) 0.3135(1) 0.51108(1) 0.0477(2) Uani 1.00 1 d . . . S(1) S 0.3138(1) 0.0378(2) 0.71364(2) 0.0476(3) Uani 1.00 1 d . . . S(2) S 0.2765(1) 0.5071(2) 0.70426(2) 0.0464(3) Uani 1.00 1 d . . . S(3) S 0.3759(1) 0.1621(2) 0.75048(2) 0.0489(3) Uani 1.00 1 d . . . S(4) S 0.3506(1) 0.6283(2) 0.74010(2) 0.0473(3) Uani 1.00 1 d . . . S(5) S 0.2467(1) -0.0646(2) 0.67605(2) 0.0484(3) Uani 1.00 1 d . . . S(6) S 0.2148(1) 0.3662(2) 0.66740(2) 0.0493(3) Uani 1.00 1 d . . . S(7) S 0.4462(1) 0.3068(2) 0.78671(2) 0.0487(3) Uani 1.00 1 d . . . S(8) S 0.4275(1) 0.7388(2) 0.77667(2) 0.0487(3) Uani 1.00 1 d . . . S(9) S 0.1870(1) 0.0523(3) 0.63911(2) 0.0589(4) Uani 1.00 1 d . . . S(10) S 0.5046(1) 0.6341(3) 0.81257(2) 0.0577(4) Uani 1.00 1 d . . . S(11) S 0.4020(2) 0.1363(2) 0.48917(2) 0.0642(5) Uani 1.00 1 d . . . S(12) S 0.3560(1) 0.6005(2) 0.49641(2) 0.0622(4) Uani 1.00 1 d . . . S(13) S 0.3669(1) 0.0251(2) 0.52553(2) 0.0606(4) Uani 1.00 1 d . . . S(14) S 0.3124(1) 0.4864(2) 0.53350(2) 0.0586(4) Uani 1.00 1 d . . . S(15) S 0.4511(1) 0.2630(3) 0.45296(2) 0.0625(4) Uani 1.00 1 d . . . S(16) S 0.4085(1) 0.6935(2) 0.45950(2) 0.0617(4) Uani 1.00 1 d . . . S(17) S 0.3319(2) -0.0750(3) 0.56323(2) 0.0660(5) Uani 1.00 1 d . . . S(18) S 0.2808(1) 0.3457(3) 0.57064(2) 0.0620(4) Uani 1.00 1 d . . . S(19) S 0.4700(2) 0.5705(3) 0.42452(2) 0.0707(5) Uani 1.00 1 d . . . S(20) S 0.2763(2) 0.0278(3) 0.59891(2) 0.0686(5) Uani 1.00 1 d . . . N(1) N 0.5419(4) -0.0666(9) 0.61551(6) 0.058(1) Uani 1.00 1 d . . . C(1) C 0.2713(4) 0.1105(8) 0.69296(6) 0.043(1) Uani 1.00 1 d . . . C(2) C 0.2547(4) 0.3155(8) 0.68903(6) 0.043(1) Uani 1.00 1 d . . . C(3) C 0.4020(4) 0.3530(8) 0.76522(6) 0.041(1) Uani 1.00 1 d . . . C(4) C 0.3928(4) 0.5601(8) 0.76045(6) 0.041(1) Uani 1.00 1 d . . . C(5) C 0.2149(4) 0.1135(9) 0.65998(6) 0.048(1) Uani 1.00 1 d . . . C(6) C 0.4596(4) 0.5629(9) 0.79298(6) 0.045(1) Uani 1.00 1 d . . . C(7) C 0.4146(4) 0.3194(9) 0.47375(6) 0.051(1) Uani 1.00 1 d . . . C(8) C 0.3938(4) 0.5268(9) 0.47695(7) 0.051(1) Uani 1.00 1 d . . . C(9) C 0.3350(5) 0.0992(9) 0.54584(6) 0.052(1) Uani 1.00 1 d . . . C(10) C 0.3099(4) 0.2980(9) 0.54906(7) 0.050(1) Uani 1.00 1 d . . . C(11) C 0.4433(4) 0.5118(10) 0.44459(7) 0.052(1) Uani 1.00 1 d . . . C(12) C 0.2952(5) 0.097(1) 0.57863(7) 0.054(1) Uani 1.00 1 d . . . C(13) C 0.5444(5) 0.0532(9) 0.63017(8) 0.056(1) Uani 1.00 1 d . . . C(14) C 0.4883(4) 0.0032(9) 0.64353(7) 0.053(1) Uani 1.00 1 d . . . C(15) C 0.4308(4) -0.1667(9) 0.64229(7) 0.053(1) Uani 1.00 1 d . . . C(16) C 0.4296(5) -0.2844(10) 0.62701(8) 0.057(1) Uani 1.00 1 d . . . C(17) C 0.4845(5) -0.234(1) 0.61380(7) 0.062(2) Uani 1.00 1 d . . . C(18) C 0.6014(6) -0.017(1) 0.6011(1) 0.086(2) Uani 1.00 1 d . . . H(1) H 0.5854 0.1729 0.6312 0.0684 Uiso 1.00 1 calc . . . H(2) H 0.3920 -0.2042 0.6518 0.0635 Uiso 1.00 1 calc . . . H(3) H 0.4812 -0.3160 0.6032 0.0729 Uiso 1.00 1 calc . . . H(4) H 0.6436 -0.1299 0.5990 0.1045 Uiso 1.00 1 calc . . . H(5) H 0.5642 0.0097 0.5905 0.1045 Uiso 1.00 1 calc . . . H(6) H 0.6394 0.1038 0.6039 0.1045 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 I(1) 0.0939(5) 0.0601(4) 0.0975(5) -0.0136(3) -0.0258(4) 0.0054(3) I(2) 0.0622(3) 0.0703(3) 0.0499(3) 0.0023(2) 0.0004(2) -0.0118(2) Br(1) 0.0622(3) 0.0703(3) 0.0499(3) 0.0023(2) 0.0004(2) -0.0118(2) Br(2) 0.0939(5) 0.0601(4) 0.0975(5) -0.0136(3) -0.0258(4) 0.0054(3) Ni(1) 0.0482(4) 0.0394(4) 0.0354(3) -0.0015(3) 0.0012(3) 0.0021(2) Ni(2) 0.0638(5) 0.0449(4) 0.0355(3) 0.0040(3) 0.0100(3) -0.0004(3) S(1) 0.0660(9) 0.0374(7) 0.0384(6) -0.0029(6) -0.0046(6) 0.0037(5) S(2) 0.0606(8) 0.0374(6) 0.0406(6) 0.0012(6) -0.0012(6) 0.0006(5) S(3) 0.0660(9) 0.0389(7) 0.0406(6) -0.0054(6) -0.0047(6) 0.0026(5) S(4) 0.0658(9) 0.0373(7) 0.0383(6) 0.0059(6) 0.0002(6) 0.0029(5) S(5) 0.0651(9) 0.0410(7) 0.0387(6) -0.0014(6) 0.0011(6) 0.0005(5) S(6) 0.0650(9) 0.0453(7) 0.0372(6) 0.0051(7) 0.0004(6) 0.0037(5) S(7) 0.0622(9) 0.0429(7) 0.0401(6) -0.0009(6) -0.0041(6) 0.0039(5) S(8) 0.0649(9) 0.0394(7) 0.0413(6) 0.0047(6) 0.0004(6) -0.0018(5) S(9) 0.079(1) 0.0600(9) 0.0371(6) -0.0025(8) -0.0004(6) -0.0028(6) S(10) 0.072(1) 0.0585(9) 0.0414(6) -0.0011(8) -0.0039(6) -0.0044(6) S(11) 0.107(1) 0.0451(8) 0.0428(7) 0.0098(8) 0.0223(8) 0.0001(5) S(12) 0.098(1) 0.0458(8) 0.0455(7) 0.0114(8) 0.0247(8) 0.0010(6) S(13) 0.098(1) 0.0474(8) 0.0384(6) 0.0102(8) 0.0166(7) -0.0002(5) S(14) 0.088(1) 0.0482(8) 0.0421(6) 0.0099(8) 0.0197(7) 0.0008(5) S(15) 0.097(1) 0.0517(8) 0.0410(7) 0.0083(8) 0.0186(7) -0.0009(6) S(16) 0.093(1) 0.0482(8) 0.0462(7) 0.0073(8) 0.0192(8) 0.0054(6) S(17) 0.108(1) 0.0504(8) 0.0414(7) 0.0075(9) 0.0159(8) 0.0034(6) S(18) 0.088(1) 0.0590(9) 0.0410(6) 0.0121(8) 0.0202(7) 0.0012(6) S(19) 0.100(1) 0.073(1) 0.0402(7) 0.0025(10) 0.0161(8) 0.0066(7) S(20) 0.098(1) 0.071(1) 0.0377(6) 0.0018(10) 0.0123(7) 0.0065(6) N(1) 0.065(3) 0.062(3) 0.048(2) 0.015(3) 0.006(2) 0.004(2) C(1) 0.047(3) 0.046(3) 0.035(2) -0.002(2) 0.004(2) 0.003(2) C(2) 0.044(3) 0.044(3) 0.040(2) 0.004(2) 0.004(2) 0.003(2) C(3) 0.038(3) 0.046(3) 0.040(2) -0.002(2) 0.003(2) 0.003(2) C(4) 0.044(3) 0.041(3) 0.037(2) 0.001(2) 0.004(2) -0.001(2) C(5) 0.052(3) 0.052(3) 0.040(2) 0.000(3) 0.008(2) 0.000(2) C(6) 0.045(3) 0.050(3) 0.041(2) 0.006(2) 0.006(2) 0.000(2) C(7) 0.064(4) 0.052(3) 0.036(2) 0.003(3) 0.006(2) -0.002(2) C(8) 0.062(4) 0.048(3) 0.043(2) 0.006(3) 0.012(2) 0.000(2) C(9) 0.066(4) 0.053(3) 0.038(2) 0.000(3) 0.007(2) -0.001(2) C(10) 0.057(3) 0.053(3) 0.042(2) 0.007(3) 0.010(2) -0.003(2) C(11) 0.061(4) 0.056(3) 0.040(2) -0.003(3) 0.002(2) 0.005(2) C(12) 0.061(4) 0.062(3) 0.040(2) -0.004(3) 0.005(2) 0.003(2) C(13) 0.062(4) 0.045(3) 0.062(3) 0.003(3) 0.008(3) -0.001(2) C(14) 0.059(3) 0.051(3) 0.050(3) 0.011(3) 0.001(3) -0.008(2) C(15) 0.061(4) 0.047(3) 0.049(3) -0.004(3) 0.000(3) -0.005(2) C(16) 0.063(4) 0.055(3) 0.053(3) 0.003(3) -0.007(3) -0.003(2) C(17) 0.078(4) 0.059(4) 0.046(3) 0.013(3) -0.002(3) -0.011(3) C(18) 0.091(6) 0.105(6) 0.066(4) 0.015(5) 0.030(4) 0.014(4) #------------------------------------------------------------------------------ _computing_data_collection . _computing_cell_refinement . _computing_data_reduction 'teXsan Ver. 2.0' _computing_structure_solution SIR97 _computing_structure_refinement SHELXL97 _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 I(1) C(16) 1.963(7) . . yes I(2) C(14) 2.052(6) . . yes Br(1) C(14) 2.052(6) . . yes Br(2) C(16) 1.963(7) . . yes Ni(1) S(1) 2.162(2) . . yes Ni(1) S(2) 2.161(2) . . yes Ni(1) S(3) 2.159(2) . . yes Ni(1) S(4) 2.155(2) . . yes Ni(2) S(11) 2.154(2) . . yes Ni(2) S(12) 2.158(2) . . yes Ni(2) S(13) 2.158(2) . . yes Ni(2) S(14) 2.168(2) . . yes S(1) C(1) 1.714(5) . . yes S(2) C(2) 1.707(5) . . yes S(3) C(3) 1.689(5) . . yes S(4) C(4) 1.682(5) . . yes S(5) C(1) 1.729(5) . . yes S(5) C(5) 1.716(5) . . yes S(6) C(2) 1.737(5) . . yes S(6) C(5) 1.722(6) . . yes S(7) C(3) 1.739(5) . . yes S(7) C(6) 1.723(6) . . yes S(8) C(4) 1.735(5) . . yes S(8) C(6) 1.720(5) . . yes S(9) C(5) 1.660(5) . . yes S(10) C(6) 1.648(5) . . yes S(11) C(7) 1.682(6) . . yes S(12) C(8) 1.678(6) . . yes S(13) C(9) 1.708(5) . . yes S(14) C(10) 1.697(6) . . yes S(15) C(7) 1.737(5) . . yes S(15) C(11) 1.724(6) . . yes S(16) C(8) 1.732(6) . . yes S(16) C(11) 1.725(6) . . yes S(17) C(9) 1.738(5) . . yes S(17) C(12) 1.719(6) . . yes S(18) C(10) 1.749(6) . . yes S(18) C(12) 1.720(7) . . yes S(19) C(11) 1.643(6) . . yes S(20) C(12) 1.646(6) . . yes N(1) C(13) 1.355(8) . . yes N(1) C(17) 1.351(9) . . yes N(1) C(18) 1.468(10) . . yes C(1) C(2) 1.370(7) . . yes C(3) C(4) 1.385(7) . . yes C(7) C(8) 1.392(8) . . yes C(9) C(10) 1.355(8) . . yes C(13) C(14) 1.372(9) . . yes C(14) C(15) 1.365(8) . . yes C(15) C(16) 1.388(8) . . yes C(16) C(17) 1.354(9) . . 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) 93.18(6) . . . yes S(1) Ni(1) S(3) 87.66(6) . . . yes S(1) Ni(1) S(4) 177.74(7) . . . yes S(2) Ni(1) S(3) 177.11(7) . . . yes S(2) Ni(1) S(4) 86.74(6) . . . yes S(3) Ni(1) S(4) 92.52(6) . . . yes S(11) Ni(2) S(12) 92.51(7) . . . yes S(11) Ni(2) S(13) 85.81(6) . . . yes S(11) Ni(2) S(14) 178.78(7) . . . yes S(12) Ni(2) S(13) 176.48(9) . . . yes S(12) Ni(2) S(14) 88.65(6) . . . yes S(13) Ni(2) S(14) 93.02(7) . . . yes Ni(1) S(1) C(1) 102.4(2) . . . yes Ni(1) S(2) C(2) 102.1(2) . . . yes Ni(1) S(3) C(3) 102.7(2) . . . yes Ni(1) S(4) C(4) 102.9(2) . . . yes C(1) S(5) C(5) 97.2(3) . . . yes C(2) S(6) C(5) 97.3(2) . . . yes C(3) S(7) C(6) 97.1(2) . . . yes C(4) S(8) C(6) 97.3(2) . . . yes Ni(2) S(11) C(7) 102.8(2) . . . yes Ni(2) S(12) C(8) 103.0(2) . . . yes Ni(2) S(13) C(9) 102.1(2) . . . yes Ni(2) S(14) C(10) 101.8(2) . . . yes C(7) S(15) C(11) 97.3(3) . . . yes C(8) S(16) C(11) 98.0(3) . . . yes C(9) S(17) C(12) 97.4(3) . . . yes C(10) S(18) C(12) 98.0(3) . . . yes C(13) N(1) C(17) 121.0(5) . . . yes C(13) N(1) C(18) 120.7(6) . . . yes C(17) N(1) C(18) 118.4(5) . . . yes S(1) C(1) S(5) 123.2(3) . . . yes S(1) C(1) C(2) 120.6(4) . . . yes S(5) C(1) C(2) 116.2(4) . . . yes S(2) C(2) S(6) 122.8(3) . . . yes S(2) C(2) C(1) 121.8(4) . . . yes S(6) C(2) C(1) 115.4(4) . . . yes S(3) C(3) S(7) 123.4(3) . . . yes S(3) C(3) C(4) 120.9(4) . . . yes S(7) C(3) C(4) 115.7(4) . . . yes S(4) C(4) S(8) 123.3(3) . . . yes S(4) C(4) C(3) 120.9(4) . . . yes S(8) C(4) C(3) 115.7(3) . . . yes S(5) C(5) S(6) 113.8(3) . . . yes S(5) C(5) S(9) 124.0(4) . . . yes S(6) C(5) S(9) 122.2(3) . . . yes S(7) C(6) S(8) 114.2(3) . . . yes S(7) C(6) S(10) 123.1(3) . . . yes S(8) C(6) S(10) 122.6(3) . . . yes S(11) C(7) S(15) 122.8(3) . . . yes S(11) C(7) C(8) 121.0(4) . . . yes S(15) C(7) C(8) 116.1(4) . . . yes S(12) C(8) S(16) 124.4(3) . . . yes S(12) C(8) C(7) 120.7(4) . . . yes S(16) C(8) C(7) 114.9(4) . . . yes S(13) C(9) S(17) 122.1(4) . . . yes S(13) C(9) C(10) 121.1(4) . . . yes S(17) C(9) C(10) 116.8(4) . . . yes S(14) C(10) S(18) 123.2(3) . . . yes S(14) C(10) C(9) 122.0(4) . . . yes S(18) C(10) C(9) 114.7(4) . . . yes S(15) C(11) S(16) 113.6(3) . . . yes S(15) C(11) S(19) 123.0(4) . . . yes S(16) C(11) S(19) 123.4(4) . . . yes S(17) C(12) S(18) 113.1(3) . . . yes S(17) C(12) S(20) 122.8(4) . . . yes S(18) C(12) S(20) 124.1(4) . . . yes N(1) C(13) C(14) 119.5(6) . . . yes I(2) C(14) C(13) 115.9(4) . . . yes I(2) C(14) C(15) 123.1(4) . . . yes C(13) C(14) C(15) 120.8(5) . . . yes C(14) C(15) C(16) 117.9(6) . . . yes I(1) C(16) C(15) 123.0(5) . . . yes I(1) C(16) C(17) 115.9(5) . . . yes C(15) C(16) C(17) 121.1(6) . . . yes N(1) C(17) C(16) 119.6(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 I(1) C(16) C(15) C(14) -179.8(5) . . . . yes I(1) C(16) C(17) N(1) -179.3(5) . . . . yes I(2) C(14) C(13) N(1) -174.6(4) . . . . yes I(2) C(14) C(15) C(16) 173.6(4) . . . . yes Br(1) C(14) C(13) N(1) -174.6(4) . . . . yes Br(1) C(14) C(15) C(16) 173.6(4) . . . . yes Br(2) C(16) C(15) C(14) -179.8(5) . . . . yes Br(2) C(16) C(17) N(1) -179.3(5) . . . . yes Ni(1) S(1) C(1) S(5) 178.9(3) . . . . yes Ni(1) S(1) C(1) C(2) -1.2(5) . . . . yes Ni(1) S(2) C(2) S(6) -177.2(3) . . . . yes Ni(1) S(2) C(2) C(1) 0.2(5) . . . . yes Ni(1) S(3) C(3) S(7) -178.6(3) . . . . yes Ni(1) S(3) C(3) C(4) -1.3(5) . . . . yes Ni(1) S(4) C(4) S(8) 177.3(3) . . . . yes Ni(1) S(4) C(4) C(3) -2.6(5) . . . . yes Ni(2) S(11) C(7) S(15) 179.7(3) . . . . yes Ni(2) S(11) C(7) C(8) -1.9(6) . . . . yes Ni(2) S(12) C(8) S(16) -179.6(3) . . . . yes Ni(2) S(12) C(8) C(7) 1.3(5) . . . . yes Ni(2) S(13) C(9) S(17) -179.3(3) . . . . yes Ni(2) S(13) C(9) C(10) 1.4(6) . . . . yes Ni(2) S(14) C(10) S(18) 178.6(3) . . . . yes Ni(2) S(14) C(10) C(9) 1.8(6) . . . . yes S(1) Ni(1) S(2) C(2) -0.7(2) . . . . yes S(1) Ni(1) S(3) C(3) 177.5(2) . . . . yes S(1) Ni(1) S(4) C(4) -93(1) . . . . yes S(1) C(1) S(5) C(5) -177.0(4) . . . . yes S(1) C(1) C(2) S(2) 0.7(7) . . . . yes S(1) C(1) C(2) S(6) 178.3(3) . . . . yes S(2) Ni(1) S(1) C(1) 1.0(2) . . . . yes S(2) Ni(1) S(3) C(3) -75(1) . . . . yes S(2) Ni(1) S(4) C(4) 178.6(2) . . . . yes S(2) C(2) S(6) C(5) 177.1(4) . . . . yes S(2) C(2) C(1) S(5) -179.4(3) . . . . yes S(3) Ni(1) S(1) C(1) 178.3(2) . . . . yes S(3) Ni(1) S(2) C(2) -107(1) . . . . yes S(3) Ni(1) S(4) C(4) 1.4(2) . . . . yes S(3) C(3) S(7) C(6) 177.4(4) . . . . yes S(3) C(3) C(4) S(4) 2.8(7) . . . . yes S(3) C(3) C(4) S(8) -177.1(3) . . . . yes S(4) Ni(1) S(1) C(1) -86(1) . . . . yes S(4) Ni(1) S(2) C(2) 177.0(2) . . . . yes S(4) Ni(1) S(3) C(3) -0.2(2) . . . . yes S(4) C(4) S(8) C(6) 179.5(4) . . . . yes S(4) C(4) C(3) S(7) -179.7(3) . . . . yes S(5) C(1) C(2) S(6) -1.8(6) . . . . yes S(5) C(5) S(6) C(2) 2.5(4) . . . . yes S(6) C(5) S(5) C(1) -3.3(4) . . . . yes S(7) C(3) C(4) S(8) 0.4(6) . . . . yes S(7) C(6) S(8) C(4) 0.7(4) . . . . yes S(8) C(6) S(7) C(3) -0.5(4) . . . . yes S(9) C(5) S(5) C(1) 176.4(4) . . . . yes S(9) C(5) S(6) C(2) -177.2(4) . . . . yes S(10) C(6) S(7) C(3) -177.5(4) . . . . yes S(10) C(6) S(8) C(4) 177.7(4) . . . . yes S(11) Ni(2) S(12) C(8) -1.9(2) . . . . yes S(11) Ni(2) S(13) C(9) 179.5(2) . . . . yes S(11) Ni(2) S(14) C(10) -15(4) . . . . yes S(11) C(7) S(15) C(11) 177.8(4) . . . . yes S(11) C(7) C(8) S(12) 0.4(8) . . . . yes S(11) C(7) C(8) S(16) -178.8(3) . . . . yes S(12) Ni(2) S(11) C(7) 2.1(2) . . . . yes S(12) Ni(2) S(13) C(9) 118(1) . . . . yes S(12) Ni(2) S(14) C(10) -177.6(2) . . . . yes S(12) C(8) S(16) C(11) -178.0(4) . . . . yes S(12) C(8) C(7) S(15) 178.9(3) . . . . yes S(13) Ni(2) S(11) C(7) -174.9(2) . . . . yes S(13) Ni(2) S(12) C(8) 59(1) . . . . yes S(13) Ni(2) S(14) C(10) -0.7(2) . . . . yes S(13) C(9) S(17) C(12) -179.7(4) . . . . yes S(13) C(9) C(10) S(14) -2.3(8) . . . . yes S(13) C(9) C(10) S(18) -179.3(3) . . . . yes S(14) Ni(2) S(11) C(7) -159(3) . . . . yes S(14) Ni(2) S(12) C(8) 177.7(2) . . . . yes S(14) Ni(2) S(13) C(9) -0.2(2) . . . . yes S(14) C(10) S(18) C(12) -178.6(4) . . . . yes S(14) C(10) C(9) S(17) 178.3(3) . . . . yes S(15) C(7) C(8) S(16) -0.3(6) . . . . yes S(15) C(11) S(16) C(8) -1.6(4) . . . . yes S(16) C(11) S(15) C(7) 1.5(4) . . . . yes S(17) C(9) C(10) S(18) 1.3(7) . . . . yes S(17) C(12) S(18) C(10) 1.4(4) . . . . yes S(18) C(12) S(17) C(9) -0.8(4) . . . . yes S(19) C(11) S(15) C(7) 179.5(4) . . . . yes S(19) C(11) S(16) C(8) -179.6(4) . . . . yes S(20) C(12) S(17) C(9) 179.3(4) . . . . yes S(20) C(12) S(18) C(10) -178.7(4) . . . . yes N(1) C(13) C(14) C(15) 0.6(9) . . . . yes N(1) C(17) C(16) C(15) 0.3(10) . . . . yes C(1) C(2) S(6) C(5) -0.4(5) . . . . yes C(2) C(1) S(5) C(5) 3.1(5) . . . . yes C(3) C(4) S(8) C(6) -0.6(5) . . . . yes C(4) C(3) S(7) C(6) 0.1(5) . . . . yes C(7) C(8) S(16) C(11) 1.1(5) . . . . yes C(8) C(7) S(15) C(11) -0.7(5) . . . . yes C(9) C(10) S(18) C(12) -1.6(5) . . . . yes C(10) C(9) S(17) C(12) -0.3(6) . . . . yes C(13) N(1) C(17) C(16) -0.9(9) . . . . yes C(13) C(14) C(15) C(16) -1.1(9) . . . . yes C(14) C(13) N(1) C(17) 0.5(9) . . . . yes C(14) C(13) N(1) C(18) -179.7(6) . . . . yes C(14) C(15) C(16) C(17) 0.7(9) . . . . yes C(16) C(17) N(1) C(18) 179.3(6) . . . . yes C(16) C(17) N(1) C(18) 179.3(6) . . . . 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 I(1) S(20) 3.503(2) . 1_545 ? I(2) S(10) 3.256(2) . 2_656 ? Br(1) S(10) 3.256(2) . 2_656 ? Br(2) S(20) 3.503(2) . 1_545 ? Ni(1) S(7) 3.429(2) . 2_656 ? Ni(2) Ni(2) 3.474(2) . 7_556 ? S(1) S(4) 3.338(2) . 1_545 ? S(1) S(2) 3.523(2) . 1_545 ? S(2) S(5) 3.503(2) . 1_565 ? S(2) S(10) 3.540(2) . 2_656 ? S(3) S(4) 3.353(2) . 6_546 ? S(3) S(8) 3.427(2) . 1_545 ? S(3) S(3) 3.535(3) . 2_656 ? S(3) S(4) 3.538(2) . 1_545 ? S(4) S(8) 3.554(2) . 2_656 ? S(11) S(14) 3.492(3) . 7_556 ? S(11) S(12) 3.560(2) . 1_545 ? S(11) S(11) 3.598(4) . 3_656 ? S(12) S(13) 3.516(2) . 1_565 ? S(12) S(13) 3.575(3) . 7_556 ? S(13) S(15) 3.501(3) . 3_656 ? S(18) S(19) 3.578(3) . 3_666 ? S(19) C(18) 3.581(9) . 3_666 ? C(1) C(6) 3.534(8) . 6_546 ? C(4) C(4) 3.53(1) . 2_656 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------ data___276 _database_code_depnum_ccdc_archive 'CCDC 915357' #TrackingRef '16106_web_deposit_cif_file_3_HiroshiM.Yamamoto_1355276590.4.cif' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C18 H6 I2 N Ni2 S20 ' _chemical_formula_moiety 'C18 H6 I2 N Ni2 S20 ' _chemical_formula_weight 1248.66 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 7.427(2) _cell_length_b 11.680(3) _cell_length_c 21.199(7) _cell_angle_alpha 81.935(10) _cell_angle_beta 96.406(11) _cell_angle_gamma 99.938(11) _cell_volume 1786.2(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4244 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 295 #------------------------------------------------------------------------------ _exptl_crystal_description Platelet _exptl_crystal_colour Black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_diffrn 2.322 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1206.00 _exptl_absorpt_coefficient_mu 3.972 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details MERCURY _exptl_absorpt_correction_T_min 0.316 _exptl_absorpt_correction_T_max 0.452 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 295 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71070 _diffrn_measurement_device_type MERCURY _diffrn_reflns_number 13804 _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.95 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.95 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 27 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using reflections with F^2^ > 2.0 sigma(F^2^). 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 7510 _reflns_number_gt 5313 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.1679 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5369 _refine_ls_number_parameters 388 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0038Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.60 _refine_diff_density_min -1.17 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Ni Ni 0.339 1.112 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; I I -0.474 1.812 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL 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 I(1) I 0.73317(9) -0.00180(5) 0.94560(3) 0.05296(19) Uani 1.00 1 d . . . I(2) I 0.68649(9) 0.51438(5) 0.92485(3) 0.04828(18) Uani 1.00 1 d . . . N(I1) Ni 0.12633(13) 0.35488(8) 0.58947(5) 0.0310(2) Uani 1.00 1 d . . . N(I2) Ni 0.38285(13) 0.12798(8) 0.48129(4) 0.0298(2) Uani 1.00 1 d . . . S(1) S 0.2768(2) 0.45809(18) 0.66075(10) 0.0367(5) Uani 1.00 1 d . . . S(2) S -0.0247(2) 0.23294(18) 0.65904(10) 0.0381(5) Uani 1.00 1 d . . . S(3) S 0.2733(2) 0.48245(18) 0.52245(10) 0.0376(5) Uani 1.00 1 d . . . S(4) S -0.0125(2) 0.25337(18) 0.51553(10) 0.0370(5) Uani 1.00 1 d . . . S(5) S 0.2818(3) 0.4240(2) 0.80412(11) 0.0482(6) Uani 1.00 1 d . . . S(6) S -0.0107(3) 0.2258(2) 0.80357(11) 0.0479(6) Uani 1.00 1 d . . . S(7) S 0.2626(3) 0.5090(2) 0.37930(10) 0.0397(5) Uani 1.00 1 d . . . S(8) S -0.0023(3) 0.29544(19) 0.37167(11) 0.0411(5) Uani 1.00 1 d . . . S(9) S 0.1613(4) 0.3058(3) 0.92780(13) 0.0773(9) Uani 1.00 1 d . . . S(10) S 0.1371(4) 0.4344(2) 0.25248(12) 0.0580(7) Uani 1.00 1 d . . . S(11) S 0.5286(2) 0.22899(18) 0.55511(10) 0.0356(5) Uani 1.00 1 d . . . S(12) S 0.2308(2) 0.00408(18) 0.55002(10) 0.0376(5) Uani 1.00 1 d . . . S(13) S 0.5374(2) 0.25371(18) 0.41511(10) 0.0368(5) Uani 1.00 1 d . . . S(14) S 0.2295(2) 0.03301(17) 0.40597(10) 0.0340(5) Uani 1.00 1 d . . . S(15) S 0.5136(3) 0.19647(19) 0.69829(10) 0.0388(5) Uani 1.00 1 d . . . S(16) S 0.2400(3) -0.01253(19) 0.69402(11) 0.0419(5) Uani 1.00 1 d . . . S(17) S 0.5227(2) 0.28138(18) 0.27046(10) 0.0372(5) Uani 1.00 1 d . . . S(18) S 0.2408(2) 0.07961(18) 0.26154(10) 0.0379(5) Uani 1.00 1 d . . . S(19) S 0.3727(4) 0.0748(2) 0.81923(12) 0.0605(7) Uani 1.00 1 d . . . S(20) S 0.3681(3) 0.2227(2) 0.14148(10) 0.0451(6) Uani 1.00 1 d . . . N(1) N 0.8103(9) 0.2512(6) 1.0793(3) 0.045(2) Uani 1.00 1 d . . . C(1) C 0.1972(10) 0.3851(6) 0.7290(3) 0.0323(19) Uani 1.00 1 d . . . C(2) C 0.0611(10) 0.2883(6) 0.7280(3) 0.034(2) Uani 1.00 1 d . . . C(3) C 0.1912(10) 0.4352(6) 0.4512(3) 0.034(2) Uani 1.00 1 d . . . C(4) C 0.0641(10) 0.3331(7) 0.4483(3) 0.034(2) Uani 1.00 1 d . . . C(5) C 0.1423(13) 0.3166(8) 0.8496(4) 0.049(2) Uani 1.00 1 d . . . C(6) C 0.1321(11) 0.4132(7) 0.3300(4) 0.039(2) Uani 1.00 1 d . . . C(7) C 0.4436(10) 0.1547(7) 0.6224(3) 0.035(2) Uani 1.00 1 d . . . C(8) C 0.3149(10) 0.0551(7) 0.6197(4) 0.035(2) Uani 1.00 1 d . . . C(9) C 0.4528(10) 0.2083(6) 0.3428(3) 0.034(2) Uani 1.00 1 d . . . C(10) C 0.3172(10) 0.1118(6) 0.3391(3) 0.0299(19) Uani 1.00 1 d . . . C(11) C 0.3745(11) 0.0849(7) 0.7411(4) 0.040(2) Uani 1.00 1 d . . . C(12) C 0.3771(11) 0.1949(6) 0.2213(3) 0.034(2) Uani 1.00 1 d . . . C(13) C 0.7975(12) 0.1533(7) 1.0525(4) 0.040(2) Uani 1.00 1 d . . . C(14) C 0.7470(12) 0.1520(7) 0.9882(4) 0.042(2) Uani 1.00 1 d . . . C(15) C 0.7062(13) 0.2509(7) 0.9502(4) 0.046(2) Uani 1.00 1 d . . . C(16) C 0.7235(11) 0.3539(7) 0.9787(4) 0.039(2) Uani 1.00 1 d . . . C(17) C 0.7717(11) 0.3518(7) 1.0438(4) 0.041(2) Uani 1.00 1 d . . . C(18) C 0.8648(14) 0.2505(10) 1.1486(4) 0.059(3) Uani 1.00 1 d . . . H(1) H 0.8217 0.0817 1.0785 0.047 Uiso 1.00 1 c R . . H(2) H 0.6665 0.2516 0.9053 0.055 Uiso 1.00 1 c R . . H(3) H 0.7833 0.4218 1.0643 0.050 Uiso 1.00 1 c R . . H(4) H 0.9413 0.3235 1.1561 0.070 Uiso 1.00 1 c R . . H(5) H 0.7576 0.2437 1.1712 0.070 Uiso 1.00 1 c R . . H(6) H 0.9288 0.1883 1.1645 0.070 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 I(1) 0.0573(4) 0.0417(3) 0.0598(4) 0.0056(2) 0.0017(3) -0.0115(2) I(2) 0.0594(4) 0.0426(3) 0.0401(3) 0.0047(2) 0.0008(2) -0.0026(2) N(I1) 0.0308(5) 0.0315(5) 0.0300(5) 0.0019(4) 0.0002(3) -0.0069(3) N(I2) 0.0297(5) 0.0313(5) 0.0268(5) 0.0006(4) 0.0010(3) -0.0045(3) S(1) 0.0395(10) 0.0356(10) 0.0313(10) -0.0059(8) 0.0040(7) -0.0059(7) S(2) 0.0389(10) 0.0371(10) 0.0352(11) -0.0036(8) 0.0012(8) -0.0069(8) S(3) 0.0400(10) 0.0367(10) 0.0325(10) -0.0069(8) 0.0018(8) -0.0087(8) S(4) 0.0359(10) 0.0353(10) 0.0379(11) -0.0017(8) 0.0013(8) -0.0092(8) S(5) 0.0520(13) 0.0540(13) 0.0330(11) -0.0084(11) 0.0027(9) -0.0078(9) S(6) 0.0478(12) 0.0533(13) 0.0379(12) -0.0058(10) 0.0091(9) -0.0023(10) S(7) 0.0411(11) 0.0436(11) 0.0336(11) 0.0029(9) 0.0050(8) -0.0055(8) S(8) 0.0448(11) 0.0411(11) 0.0373(11) 0.0035(9) -0.0036(8) -0.0147(8) S(9) 0.0744(19) 0.113(2) 0.0337(13) -0.0153(18) 0.0104(12) -0.0060(14) S(10) 0.0729(17) 0.0764(17) 0.0299(11) 0.0227(14) 0.0021(10) -0.0127(11) S(11) 0.0379(10) 0.0367(10) 0.0288(10) -0.0039(8) 0.0030(7) -0.0043(7) S(12) 0.0390(10) 0.0355(10) 0.0343(11) -0.0061(8) 0.0050(8) -0.0046(8) S(13) 0.0412(10) 0.0372(10) 0.0284(10) -0.0057(8) 0.0032(8) -0.0065(7) S(14) 0.0364(10) 0.0325(9) 0.0302(10) -0.0038(8) 0.0047(7) -0.0043(7) S(15) 0.0440(11) 0.0407(11) 0.0297(10) 0.0020(9) 0.0013(8) -0.0054(8) S(16) 0.0489(12) 0.0383(11) 0.0356(11) 0.0007(9) 0.0103(9) 0.0024(8) S(17) 0.0443(11) 0.0340(10) 0.0306(10) -0.0021(8) 0.0052(8) -0.0039(7) S(18) 0.0426(11) 0.0380(10) 0.0303(10) -0.0030(9) 0.0019(8) -0.0076(8) S(19) 0.0806(19) 0.0680(16) 0.0299(12) 0.0109(14) 0.0073(11) 0.0047(10) S(20) 0.0640(14) 0.0415(11) 0.0303(10) 0.0098(10) 0.0026(9) -0.0060(8) N(1) 0.041(3) 0.056(4) 0.036(4) 0.004(3) 0.003(3) -0.006(3) C(1) 0.034(3) 0.038(4) 0.026(3) 0.005(3) 0.001(2) -0.011(3) C(2) 0.036(4) 0.034(4) 0.031(4) 0.004(3) 0.004(3) -0.002(3) C(3) 0.037(4) 0.035(4) 0.029(4) 0.009(3) -0.001(3) -0.004(3) C(4) 0.035(4) 0.041(4) 0.028(3) 0.008(3) -0.004(3) -0.011(3) C(5) 0.048(5) 0.054(5) 0.043(5) 0.001(4) 0.007(4) -0.004(4) C(6) 0.039(4) 0.047(4) 0.036(4) 0.017(3) -0.005(3) -0.013(3) C(7) 0.036(4) 0.046(4) 0.025(3) 0.008(3) 0.000(3) -0.008(3) C(8) 0.032(3) 0.039(4) 0.035(4) 0.014(3) 0.003(3) 0.002(3) C(9) 0.037(4) 0.035(4) 0.034(4) 0.003(3) 0.013(3) -0.009(3) C(10) 0.029(3) 0.033(3) 0.030(3) 0.009(3) -0.001(2) -0.008(2) C(11) 0.034(4) 0.045(4) 0.039(4) 0.011(3) 0.001(3) -0.001(3) C(12) 0.042(4) 0.031(3) 0.031(4) 0.008(3) 0.007(3) -0.005(3) C(13) 0.044(4) 0.030(4) 0.045(5) -0.000(3) 0.013(3) 0.001(3) C(14) 0.045(4) 0.032(4) 0.049(5) 0.003(3) 0.006(3) -0.013(3) C(15) 0.058(5) 0.048(5) 0.030(4) 0.003(4) 0.006(3) -0.006(3) C(16) 0.041(4) 0.040(4) 0.038(4) 0.010(3) 0.009(3) -0.003(3) C(17) 0.044(4) 0.040(4) 0.039(4) 0.009(3) 0.005(3) -0.006(3) C(18) 0.055(5) 0.079(7) 0.037(5) 0.004(5) -0.007(4) -0.005(4) #============================================================================== _computing_data_collection CRYSTALCLEAR _computing_cell_refinement CRYSTALCLEAR _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.8' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 I(1) C(14) 2.103(9) yes . . I(2) C(16) 2.097(8) yes . . N(I1) S(1) 2.157(2) yes . . N(I1) S(2) 2.166(2) yes . . N(I1) S(3) 2.150(2) yes . . N(I1) S(4) 2.160(2) yes . . N(I2) S(11) 2.171(2) yes . . N(I2) S(12) 2.169(2) yes . . N(I2) S(13) 2.155(2) yes . . N(I2) S(14) 2.175(2) yes . . S(1) C(1) 1.686(7) yes . . S(2) C(2) 1.695(8) yes . . S(3) C(3) 1.694(8) yes . . S(4) C(4) 1.688(7) yes . . S(5) C(1) 1.737(7) yes . . S(5) C(5) 1.735(9) yes . . S(6) C(2) 1.765(8) yes . . S(6) C(5) 1.730(9) yes . . S(7) C(3) 1.733(7) yes . . S(7) C(6) 1.736(8) yes . . S(8) C(4) 1.739(8) yes . . S(8) C(6) 1.746(8) yes . . S(9) C(5) 1.638(10) yes . . S(10) C(6) 1.631(9) yes . . S(11) C(7) 1.688(8) yes . . S(12) C(8) 1.686(8) yes . . S(13) C(9) 1.709(8) yes . . S(14) C(10) 1.707(7) yes . . S(15) C(7) 1.744(8) yes . . S(15) C(11) 1.733(8) yes . . S(16) C(8) 1.764(8) yes . . S(16) C(11) 1.731(8) yes . . S(17) C(9) 1.734(8) yes . . S(17) C(12) 1.715(7) yes . . S(18) C(10) 1.749(7) yes . . S(18) C(12) 1.721(7) yes . . S(19) C(11) 1.644(9) yes . . S(20) C(12) 1.675(8) yes . . N(1) C(13) 1.332(12) yes . . N(1) C(17) 1.360(11) yes . . N(1) C(18) 1.480(12) yes . . C(1) C(2) 1.381(10) yes . . C(3) C(4) 1.391(10) yes . . C(7) C(8) 1.375(10) yes . . C(9) C(10) 1.381(10) yes . . C(13) C(14) 1.374(12) yes . . C(14) C(15) 1.372(12) yes . . C(15) C(16) 1.400(13) yes . . C(16) C(17) 1.386(12) yes . . C(13) H(1) 0.968 no . . C(15) H(2) 0.963 no . . C(17) H(3) 0.966 no . . C(18) H(4) 0.962 no . . C(18) H(5) 0.960 no . . C(18) H(6) 0.938 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S(1) N(I1) S(2) 93.45(8) yes . . . S(1) N(I1) S(3) 84.76(8) yes . . . S(1) N(I1) S(4) 177.19(9) yes . . . S(2) N(I1) S(3) 177.35(10) yes . . . S(2) N(I1) S(4) 88.87(8) yes . . . S(3) N(I1) S(4) 92.97(8) yes . . . S(11) N(I2) S(12) 92.49(8) yes . . . S(11) N(I2) S(13) 85.95(8) yes . . . S(11) N(I2) S(14) 177.42(9) yes . . . S(12) N(I2) S(13) 178.43(9) yes . . . S(12) N(I2) S(14) 88.23(8) yes . . . S(13) N(I2) S(14) 93.33(8) yes . . . N(I1) S(1) C(1) 102.2(2) yes . . . N(I1) S(2) C(2) 101.3(2) yes . . . N(I1) S(3) C(3) 102.7(2) yes . . . N(I1) S(4) C(4) 102.5(2) yes . . . C(1) S(5) C(5) 98.1(4) yes . . . C(2) S(6) C(5) 97.9(4) yes . . . C(3) S(7) C(6) 97.1(3) yes . . . C(4) S(8) C(6) 97.6(3) yes . . . N(I2) S(11) C(7) 102.6(2) yes . . . N(I2) S(12) C(8) 102.0(2) yes . . . N(I2) S(13) C(9) 102.6(2) yes . . . N(I2) S(14) C(10) 101.8(2) yes . . . C(7) S(15) C(11) 97.5(3) yes . . . C(8) S(16) C(11) 97.3(3) yes . . . C(9) S(17) C(12) 97.6(3) yes . . . C(10) S(18) C(12) 97.3(3) yes . . . C(13) N(1) C(17) 120.7(7) yes . . . C(13) N(1) C(18) 119.8(7) yes . . . C(17) N(1) C(18) 119.5(8) yes . . . S(1) C(1) S(5) 122.9(4) yes . . . S(1) C(1) C(2) 121.0(6) yes . . . S(5) C(1) C(2) 116.1(5) yes . . . S(2) C(2) S(6) 123.2(4) yes . . . S(2) C(2) C(1) 121.9(6) yes . . . S(6) C(2) C(1) 114.8(5) yes . . . S(3) C(3) S(7) 122.2(4) yes . . . S(3) C(3) C(4) 120.8(6) yes . . . S(7) C(3) C(4) 117.0(6) yes . . . S(4) C(4) S(8) 124.1(4) yes . . . S(4) C(4) C(3) 120.9(6) yes . . . S(8) C(4) C(3) 114.9(5) yes . . . S(5) C(5) S(6) 113.0(5) yes . . . S(5) C(5) S(9) 121.5(5) yes . . . S(6) C(5) S(9) 125.5(5) yes . . . S(7) C(6) S(8) 113.4(4) yes . . . S(7) C(6) S(10) 122.0(4) yes . . . S(8) C(6) S(10) 124.6(5) yes . . . S(11) C(7) S(15) 123.1(4) yes . . . S(11) C(7) C(8) 120.6(6) yes . . . S(15) C(7) C(8) 116.3(6) yes . . . S(12) C(8) S(16) 122.6(4) yes . . . S(12) C(8) C(7) 122.2(6) yes . . . S(16) C(8) C(7) 115.2(6) yes . . . S(13) C(9) S(17) 123.2(4) yes . . . S(13) C(9) C(10) 120.8(6) yes . . . S(17) C(9) C(10) 116.0(6) yes . . . S(14) C(10) S(18) 123.3(4) yes . . . S(14) C(10) C(9) 121.6(6) yes . . . S(18) C(10) C(9) 115.1(5) yes . . . S(15) C(11) S(16) 113.7(5) yes . . . S(15) C(11) S(19) 122.3(5) yes . . . S(16) C(11) S(19) 124.1(4) yes . . . S(17) C(12) S(18) 114.0(4) yes . . . S(17) C(12) S(20) 122.3(4) yes . . . S(18) C(12) S(20) 123.6(4) yes . . . N(1) C(13) C(14) 120.8(7) yes . . . I(1) C(14) C(13) 120.6(6) yes . . . I(1) C(14) C(15) 118.4(6) yes . . . C(13) C(14) C(15) 120.9(8) yes . . . C(14) C(15) C(16) 117.8(8) yes . . . I(2) C(16) C(15) 121.8(6) yes . . . I(2) C(16) C(17) 118.4(6) yes . . . C(15) C(16) C(17) 119.8(7) yes . . . N(1) C(17) C(16) 119.9(8) yes . . . N(1) C(13) H(1) 119.8 no . . . C(14) C(13) H(1) 119.4 no . . . C(14) C(15) H(2) 122.6 no . . . C(16) C(15) H(2) 119.6 no . . . N(1) C(17) H(3) 119.1 no . . . C(16) C(17) H(3) 120.9 no . . . N(1) C(18) H(4) 109.4 no . . . N(1) C(18) H(5) 109.6 no . . . N(1) C(18) H(6) 111.1 no . . . H(4) C(18) H(5) 107.6 no . . . H(4) C(18) H(6) 109.4 no . . . H(5) C(18) H(6) 109.6 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(1) N(I1) S(2) C(2) 0.0(2) ? . . . . S(2) N(I1) S(1) C(1) 1.3(3) ? . . . . S(1) N(I1) S(3) C(3) -179.2(3) ? . . . . S(3) N(I1) S(1) C(1) 179.3(3) ? . . . . S(1) N(I1) S(4) C(4) -38.5(19) ? . . . . S(4) N(I1) S(1) C(1) -144.4(18) ? . . . . S(2) N(I1) S(3) C(3) -131.7(19) ? . . . . S(3) N(I1) S(2) C(2) -47(2) ? . . . . S(2) N(I1) S(4) C(4) 175.7(3) ? . . . . S(4) N(I1) S(2) C(2) 178.5(3) ? . . . . S(3) N(I1) S(4) C(4) -2.4(3) ? . . . . S(4) N(I1) S(3) C(3) 2.4(3) ? . . . . S(11) N(I2) S(12) C(8) -1.1(3) ? . . . . S(12) N(I2) S(11) C(7) 0.4(3) ? . . . . S(11) N(I2) S(13) C(9) -177.4(3) ? . . . . S(13) N(I2) S(11) C(7) -179.7(3) ? . . . . S(11) N(I2) S(14) C(10) 73(2) ? . . . . S(14) N(I2) S(11) C(7) 106.5(19) ? . . . . S(12) N(I2) S(13) C(9) -176(3) ? . . . . S(13) N(I2) S(12) C(8) -3(3) ? . . . . S(12) N(I2) S(14) C(10) 179.5(2) ? . . . . S(14) N(I2) S(12) C(8) -178.6(3) ? . . . . S(13) N(I2) S(14) C(10) -0.4(3) ? . . . . S(14) N(I2) S(13) C(9) 0.2(2) ? . . . . N(I1) S(1) C(1) S(5) 175.9(4) ? . . . . N(I1) S(1) C(1) C(2) -2.9(7) ? . . . . N(I1) S(2) C(2) S(6) 179.7(4) ? . . . . N(I1) S(2) C(2) C(1) -1.9(7) ? . . . . N(I1) S(3) C(3) S(7) 179.0(4) ? . . . . N(I1) S(3) C(3) C(4) -2.0(7) ? . . . . N(I1) S(4) C(4) S(8) -179.5(4) ? . . . . N(I1) S(4) C(4) C(3) 1.8(7) ? . . . . C(1) S(5) C(5) S(6) -0.8(6) ? . . . . C(1) S(5) C(5) S(9) 178.7(7) ? . . . . C(5) S(5) C(1) S(1) 179.7(5) ? . . . . C(5) S(5) C(1) C(2) -1.5(8) ? . . . . C(2) S(6) C(5) S(5) 2.1(6) ? . . . . C(2) S(6) C(5) S(9) -177.3(7) ? . . . . C(5) S(6) C(2) S(2) 175.3(6) ? . . . . C(5) S(6) C(2) C(1) -3.2(7) ? . . . . C(3) S(7) C(6) S(8) 0.3(5) ? . . . . C(3) S(7) C(6) S(10) 179.9(4) ? . . . . C(6) S(7) C(3) S(3) 178.7(5) ? . . . . C(6) S(7) C(3) C(4) -0.4(7) ? . . . . C(4) S(8) C(6) S(7) -0.1(4) ? . . . . C(4) S(8) C(6) S(10) -179.7(5) ? . . . . C(6) S(8) C(4) S(4) -178.9(6) ? . . . . C(6) S(8) C(4) C(3) -0.1(5) ? . . . . N(I2) S(11) C(7) S(15) 179.6(4) ? . . . . N(I2) S(11) C(7) C(8) 0.7(8) ? . . . . N(I2) S(12) C(8) S(16) -180.0(4) ? . . . . N(I2) S(12) C(8) C(7) 1.9(8) ? . . . . N(I2) S(13) C(9) S(17) 177.7(4) ? . . . . N(I2) S(13) C(9) C(10) 0.2(5) ? . . . . N(I2) S(14) C(10) S(18) -178.0(4) ? . . . . N(I2) S(14) C(10) C(9) 0.6(7) ? . . . . C(7) S(15) C(11) S(16) 0.7(6) ? . . . . C(7) S(15) C(11) S(19) -179.1(6) ? . . . . C(11) S(15) C(7) S(11) -180.0(5) ? . . . . C(11) S(15) C(7) C(8) -1.0(8) ? . . . . C(8) S(16) C(11) S(15) -0.4(6) ? . . . . C(8) S(16) C(11) S(19) 179.4(6) ? . . . . C(11) S(16) C(8) S(12) -178.6(5) ? . . . . C(11) S(16) C(8) C(7) -0.3(6) ? . . . . C(9) S(17) C(12) S(18) -1.8(5) ? . . . . C(9) S(17) C(12) S(20) 177.3(6) ? . . . . C(12) S(17) C(9) S(13) -176.8(5) ? . . . . C(12) S(17) C(9) C(10) 0.8(7) ? . . . . C(10) S(18) C(12) S(17) 2.0(5) ? . . . . C(10) S(18) C(12) S(20) -177.1(5) ? . . . . C(12) S(18) C(10) S(14) 177.2(5) ? . . . . C(12) S(18) C(10) C(9) -1.5(7) ? . . . . C(13) N(1) C(17) C(16) -1.8(12) ? . . . . C(17) N(1) C(13) C(14) 0.7(11) ? . . . . C(18) N(1) C(13) C(14) 180.0(7) ? . . . . C(18) N(1) C(17) C(16) 178.9(8) ? . . . . S(1) C(1) C(2) S(2) 3.5(11) ? . . . . S(1) C(1) C(2) S(6) -178.0(4) ? . . . . S(5) C(1) C(2) S(2) -175.4(4) ? . . . . S(5) C(1) C(2) S(6) 3.2(9) ? . . . . S(3) C(3) C(4) S(4) 0.1(8) ? . . . . S(3) C(3) C(4) S(8) -178.7(4) ? . . . . S(7) C(3) C(4) S(4) 179.2(4) ? . . . . S(7) C(3) C(4) S(8) 0.3(7) ? . . . . S(11) C(7) C(8) S(12) -1.8(11) ? . . . . S(11) C(7) C(8) S(16) 179.9(3) ? . . . . S(15) C(7) C(8) S(12) 179.1(5) ? . . . . S(15) C(7) C(8) S(16) 0.9(9) ? . . . . S(13) C(9) C(10) S(14) -0.6(10) ? . . . . S(13) C(9) C(10) S(18) 178.1(4) ? . . . . S(17) C(9) C(10) S(14) -178.2(4) ? . . . . S(17) C(9) C(10) S(18) 0.5(9) ? . . . . N(1) C(13) C(14) I(1) 178.5(6) ? . . . . N(1) C(13) C(14) C(15) -0.8(13) ? . . . . I(1) C(14) C(15) C(16) -177.4(6) ? . . . . C(13) C(14) C(15) C(16) 2.0(13) ? . . . . C(14) C(15) C(16) I(2) 174.9(6) ? . . . . C(14) C(15) C(16) C(17) -3.1(13) ? . . . . I(2) C(16) C(17) N(1) -175.1(6) ? . . . . C(15) C(16) C(17) N(1) 3.0(12) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 I(1) S(20) 3.315(2) ? . 2_656 I(2) S(20) 3.265(2) ? . 2_666 N(I1) C(7) 3.547(8) ? . . N(I2) C(4) 3.599(8) ? . . S(1) S(7) 3.560(3) ? . 2_666 S(1) S(17) 3.578(2) ? . 2_666 S(2) S(15) 3.559(3) ? . 1_455 S(3) S(3) 3.541(3) ? . 2_666 S(3) S(13) 3.530(2) ? . 2_666 S(4) S(11) 3.555(3) ? . 1_455 S(4) S(12) 3.548(2) ? . 2_556 S(6) S(19) 3.562(4) ? . . S(7) S(1) 3.560(3) ? . 2_666 S(7) S(11) 3.574(3) ? . 2_666 S(8) S(13) 3.574(3) ? . 1_455 S(9) C(14) 3.558(9) ? . 1_455 S(9) C(15) 3.403(10) ? . 1_455 S(10) S(17) 3.587(3) ? . . S(10) C(18) 3.519(11) ? . 1_454 S(11) S(4) 3.555(3) ? . 1_655 S(11) S(7) 3.574(3) ? . 2_666 S(12) S(4) 3.548(2) ? . 2_556 S(12) S(14) 3.582(3) ? . 2_556 S(13) S(3) 3.530(2) ? . 2_666 S(13) S(8) 3.574(3) ? . 1_655 S(14) S(12) 3.582(3) ? . 2_556 S(15) S(2) 3.559(3) ? . 1_655 S(17) S(1) 3.578(2) ? . 2_666 S(17) S(10) 3.587(3) ? . . S(19) S(6) 3.562(4) ? . . S(20) I(1) 3.315(2) ? . 2_656 S(20) I(2) 3.265(2) ? . 2_666 C(2) C(11) 3.566(12) ? . . C(4) N(I2) 3.599(8) ? . . C(7) N(I1) 3.547(8) ? . . C(8) C(10) 3.586(11) ? . 2_656 C(10) C(8) 3.586(11) ? . 2_656 C(11) C(2) 3.566(12) ? . . C(14) S(9) 3.558(9) ? . 1_655 C(15) S(9) 3.403(10) ? . 1_655 C(18) S(10) 3.519(11) ? . 1_656 I(2) H(4) 3.538 ? . 2_767 S(6) H(2) 3.476 ? . 1_455 S(9) H(3) 3.163 ? . 2_667 S(10) H(4) 2.720 ? . 1_454 S(17) H(5) 3.002 ? . 1_554 S(18) H(6) 3.230 ? . 1_454 S(19) H(1) 2.966 ? . 2_657 S(19) H(2) 3.312 ? . . S(19) H(6) 3.475 ? . 2_657 S(20) H(5) 2.866 ? . 1_554 S(20) H(6) 3.300 ? . 1_454 C(12) H(5) 3.064 ? . 1_554 C(12) H(6) 3.404 ? . 1_454 H(1) S(19) 2.966 ? . 2_657 H(2) S(6) 3.476 ? . 1_655 H(2) S(19) 3.312 ? . . H(3) S(9) 3.163 ? . 2_667 H(4) I(2) 3.538 ? . 2_767 H(4) S(10) 2.720 ? . 1_656 H(5) S(17) 3.002 ? . 1_556 H(5) S(20) 2.866 ? . 1_556 H(5) C(12) 3.064 ? . 1_556 H(6) S(18) 3.230 ? . 1_656 H(6) S(19) 3.475 ? . 2_657 H(6) S(20) 3.300 ? . 1_656 H(6) C(12) 3.404 ? . 1_656