Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Bigoli, Francesco' 'Chen, Chin-Ti' 'Deplano, Paola' 'Mercuri, Maria Laura' 'Pellinghelli, Maria Angela' 'Pilia, Luca' 'Pintus, Gloria' 'Serpe, Angela' 'Trogu, Emanuele F.' 'Wu, Wei-Ching' _publ_contact_author_name 'Dr Paola Deplano' _publ_contact_author_address ; Dipartimento di Chimica Inorganica ed Analytica Universita diCagliari Cittadella di Monserrato Monserrato Cagliari I-9042 ITALY ; _publ_contact_author_email 'DEPLANO@VAXCA1.UNICA.IT' _publ_section_title ; [Ni(R2pipdt)2](BF4)2(R2pipdt==1,4-disubstituted-piperazine-3,2-dithione) as useful precursors of mixed-ligand dithiolenes of interest for non-linear optics ; data_1 _database_code_CSD 167946 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Ni(C6H10N2S2)2](BF4)2 _chemical_formula_sum 'C12 H20 B2 F8 N4 Ni S4' _chemical_formula_weight 580.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Fddd' (no. 70) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/4, -y+1/4, z' 'x, -y+1/4, -z+1/4' '-x+1/4, y, -z+1/4' 'x, y+1/2, z+1/2' '-x+1/4, -y+3/4, z+1/2' 'x, -y+3/4, -z+3/4' '-x+1/4, y+1/2, -z+3/4' 'x+1/2, y, z+1/2' '-x+3/4, -y+1/4, z+1/2' 'x+1/2, -y+1/4, -z+3/4' '-x+3/4, y, -z+3/4' 'x+1/2, y+1/2, z' '-x+3/4, -y+3/4, z' 'x+1/2, -y+3/4, -z+1/4' '-x+3/4, y+1/2, -z+1/4' '-x, -y, -z' 'x-1/4, y-1/4, -z' '-x, y-1/4, z-1/4' 'x-1/4, -y, z-1/4' '-x, -y+1/2, -z+1/2' 'x-1/4, y+1/4, -z+1/2' '-x, y+1/4, z+1/4' 'x-1/4, -y+1/2, z+1/4' '-x+1/2, -y, -z+1/2' 'x+1/4, y-1/4, -z+1/2' '-x+1/2, y-1/4, z+1/4' 'x+1/4, -y, z+1/4' '-x+1/2, -y+1/2, -z' 'x+1/4, y+1/4, -z' '-x+1/2, y+1/4, z-1/4' 'x+1/4, -y+1/2, z-1/4' _cell_length_a 16.646(6) _cell_length_b 18.189(6) _cell_length_c 14.887(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4507(3) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 9 _cell_measurement_theta_max 17 _exptl_crystal_description 'irregular octahedron' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.712 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2352 _exptl_absorpt_coefficient_mu 1.305 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 994 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 25.07 _reflns_number_total 994 _reflns_number_gt 326 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens AED local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ZORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.1580P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00013(11) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 994 _refine_ls_number_parameters 68 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1554 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2316 _refine_ls_wR_factor_gt 0.2019 _refine_ls_goodness_of_fit_ref 0.766 _refine_ls_restrained_S_all 0.766 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.1250 0.1250 0.1250 0.0635(9) Uani 1 4 d S . . S S 0.03497(13) 0.21039(12) 0.12147(18) 0.0704(9) Uani 1 1 d . . . N N -0.1214(5) 0.2017(4) 0.1314(5) 0.0662(18) Uani 1 1 d . . . C1 C -0.0537(4) 0.1656(5) 0.1265(6) 0.058(2) Uani 1 1 d . . . C2 C -0.1984(5) 0.1610(5) 0.1442(9) 0.098(4) Uani 1 1 d . . . H2A H -0.2092 0.1570 0.2080 0.53(2) Uiso 1 1 calc R . . H2B H -0.2416 0.1893 0.1175 0.53(2) Uiso 1 1 calc R . . C3 C -0.1257(5) 0.2818(5) 0.1320(7) 0.077(3) Uani 1 1 d . . . H3A H -0.1748 0.2971 0.1602 0.16(3) Uiso 1 1 calc R . . H3B H -0.1244 0.2998 0.0714 0.16(3) Uiso 1 1 calc R . . H3C H -0.0809 0.3013 0.1647 0.16(3) Uiso 1 1 calc R . . B B 0.1250 0.8153(9) 0.1250 0.072(4) Uiso 1 2 d S . . F1 F 0.0729(5) 0.8543(5) 0.0760(6) 0.155(3) Uiso 1 1 d . . . F2A F 0.1833(10) 0.7999(9) 0.0612(9) 0.127(7) Uiso 0.53(2) 1 d P . . F2B F 0.1406(10) 0.7508(11) 0.0754(10) 0.129(8) Uiso 0.47(2) 1 d 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0571(15) 0.0612(14) 0.0721(16) 0.000 0.000 0.000 S 0.0581(15) 0.0606(14) 0.0925(19) 0.0056(14) -0.0065(14) -0.0008(9) N 0.065(4) 0.060(4) 0.073(4) 0.005(4) 0.001(7) 0.007(4) C1 0.042(5) 0.090(5) 0.042(4) 0.007(6) -0.002(5) -0.001(4) C2 0.051(6) 0.070(5) 0.173(13) 0.010(8) 0.021(7) 0.004(5) C3 0.070(5) 0.075(6) 0.087(6) -0.007(5) -0.004(8) 0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S 2.159(2) . ? Ni S 2.159(2) 4 ? Ni S 2.159(2) 2 ? Ni S 2.159(2) 3 ? S C1 1.688(7) . ? N C1 1.306(9) . ? N C3 1.460(10) . ? N C2 1.491(11) . ? C1 C1 1.477(17) 3 ? C2 C2 1.43(2) 3 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? B F1 1.337(11) 4 ? B F1 1.337(11) . ? B F2A 1.386(15) 4 ? B F2A 1.386(15) . ? B F2B 1.41(2) 4 ? B F2B 1.41(2) . ? F2A F2B 1.161(18) . ? F2B F2B 1.57(3) 4 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S Ni S 87.98(12) . 4 ? S Ni S 177.21(14) . 2 ? S Ni S 92.09(12) 4 2 ? S Ni S 92.08(12) . 3 ? S Ni S 177.21(14) 4 3 ? S Ni S 87.98(12) 2 3 ? C1 S Ni 105.0(3) . . ? C1 N C3 123.0(8) . . ? C1 N C2 120.0(7) . . ? C3 N C2 116.8(8) . . ? N C1 C1 120.3(5) . 3 ? N C1 S 120.9(7) . . ? C1 C1 S 118.8(3) 3 . ? C2 C2 N 113.8(7) 3 . ? C2 C2 H2A 108.8 3 . ? N C2 H2A 108.8 . . ? C2 C2 H2B 108.8 3 . ? N C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? N C3 H3A 109.5 . . ? N C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? F1 B F1 115.9(14) 4 . ? F1 B F2A 100.8(7) 4 4 ? F1 B F2A 91.5(8) . 4 ? F1 B F2A 91.5(8) 4 . ? F1 B F2A 100.8(7) . . ? F2A B F2A 156.8(18) 4 . ? F1 B F2B 106.0(8) 4 4 ? F1 B F2B 127.4(9) . 4 ? F2A B F2B 49.1(7) 4 4 ? F2A B F2B 108.7(15) . 4 ? F1 B F2B 127.4(9) 4 . ? F1 B F2B 106.0(8) . . ? F2A B F2B 108.7(15) 4 . ? F2A B F2B 49.1(7) . . ? F2B B F2B 67.5(16) 4 . ? F2B F2A B 66.5(12) . . ? F2A F2B B 64.4(12) . . ? F2A F2B F2B 112.0(13) . 4 ? B F2B F2B 56.3(8) . 4 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.824 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.116 #==END #==BEGIN data_d18a [Ni(C6H10N2S2)(C4N2S2)] _database_code_CSD 167947 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Ni(C6H10N2S2)(C4N2S2)] _chemical_formula_sum 'C10 H10 N4 Ni S4' _chemical_formula_weight 373.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/C' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 15.381(4) _cell_length_b 13.623(4) _cell_length_c 7.464(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.16(2) _cell_angle_gamma 90.00 _cell_volume 1502.2(12) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 18 _exptl_crystal_description 'prism' _exptl_crystal_colour 'blue' _exptl_crystal_size_max 27 _exptl_crystal_size_mid 19 _exptl_crystal_size_min 13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.837 _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens AED diffractometer' _diffrn_measurement_method '\q/2\q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'none' _diffrn_reflns_number 1431 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_sigmaI/netI 0.1705 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 25.08 _reflns_number_total 1330 _reflns_number_gt 384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens AED local upgrade' _computing_cell_refinement 'local programs' _computing_data_reduction 'local programs' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w==1/[\s^2^(Fo^2^)+(0.0694P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(4) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1330 _refine_ls_number_parameters 91 _refine_ls_number_restraints 00 _refine_ls_R_factor_all 0.1493 _refine_ls_R_factor_gt 0.0452 _refine_ls_wR_factor_ref 0.1215 _refine_ls_wR_factor_gt 0.1020 _refine_ls_goodness_of_fit_ref 0.665 _refine_ls_restrained_S_all 0.665 _refine_ls_shift/su_max 00.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.0000 0.16844(9) 0.2500 0.0625(5) Uani 1 d S . . S1 S 0.10373(12) 0.05783(13) 0.2781(3) 0.0693(7) Uani 1 d . . . S2 S 0.10492(12) 0.27736(13) 0.3072(3) 0.0754(7) Uani 1 d . . . N1 N 0.0911(4) -0.1333(5) 0.2746(8) 0.0684(19) Uani 1 d . . . N2 N 0.1381(5) 0.5478(4) 0.3172(11) 0.111(3) Uani 1 d . . . C1 C 0.0479(4) -0.0509(5) 0.2623(10) 0.0600(19) Uani 1 d . . . C2 C 0.0493(5) -0.2287(5) 0.2822(12) 0.088(3) Uani 1 d . . . H2A H 0.0678 -0.2521 0.4100 0.12(2) Uiso 1 calc R . . H2B H 0.0721 -0.2747 0.2070 0.12(2) Uiso 1 calc R . . C3 C 0.1899(5) -0.1402(5) 0.3029(11) 0.093(3) Uani 1 d . . . H3A H 0.2096 -0.0869 0.2396 0.16(2) Uiso 1 calc R . . H3B H 0.2040 -0.2014 0.2537 0.16(2) Uiso 1 calc R . . H3C H 0.2204 -0.1368 0.4338 0.16(2) Uiso 1 calc R . . C4 C 0.0445(5) 0.3865(4) 0.2757(12) 0.072(3) Uani 1 d . . . C5 C 0.0963(5) 0.4770(5) 0.2963(11) 0.079(3) Uani 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0641(8) 0.0472(8) 0.0783(10) 0.000 0.0235(7) 0.000 S1 0.0584(11) 0.0484(11) 0.1024(18) -0.0002(10) 0.0242(11) 0.0014(9) S2 0.0695(14) 0.0486(12) 0.1065(19) 0.0011(11) 0.0219(13) -0.0021(10) N1 0.072(5) 0.060(4) 0.071(4) 0.002(3) 0.016(4) 0.018(3) N2 0.096(5) 0.063(4) 0.165(8) -0.012(5) 0.019(5) -0.028(4) C1 0.083(5) 0.052(4) 0.046(4) 0.000(4) 0.020(5) -0.003(4) C2 0.112(7) 0.048(5) 0.112(8) 0.008(6) 0.045(6) 0.017(5) C3 0.071(5) 0.088(6) 0.118(7) 0.004(5) 0.023(5) 0.030(4) C4 0.139(9) 0.025(3) 0.065(6) -0.003(4) 0.048(8) -0.006(4) C5 0.080(6) 0.042(5) 0.110(7) 0.010(5) 0.017(5) 0.014(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni S2 2.146(2) 6_556 ? Ni S2 2.146(2) . ? Ni S1 2.162(2) 6_556 ? Ni S1 2.162(2) . ? S1 C1 1.700(6) . ? S2 C4 1.735(6) . ? N1 C1 1.295(7) . ? N1 C2 1.457(8) . ? N1 C3 1.479(8) . ? N2 C5 1.146(8) . ? C1 C1 1.433(13) 6_556 ? C2 C2 1.458(13) 6_556 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C4 1.316(14) 6_556 ? C4 C5 1.452(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Ni S2 92.51(12) 6_556 . ? S2 Ni S1 88.21(7) 6_556 6_556 ? S2 Ni S1 174.33(8) . 6_556 ? S2 Ni S1 174.33(8) 6_556 . ? S2 Ni S1 88.21(7) . . ? S1 Ni S1 91.63(11) 6_556 . ? C1 S1 Ni 104.8(2) . . ? C4 S2 Ni 102.8(2) . . ? C1 N1 C2 123.6(6) . . ? C1 N1 C3 123.5(6) . . ? C2 N1 C3 112.6(5) . . ? N1 C1 C1 119.8(4) . 6_556 ? N1 C1 S1 120.8(6) . . ? C1 C1 S1 119.4(2) 6_556 . ? N1 C2 C2 114.6(4) . 6_556 ? N1 C2 H2A 108.6 . . ? C2 C2 H2A 108.6 6_556 . ? N1 C2 H2B 108.6 . . ? C2 C2 H2B 108.6 6_556 . ? H2A C2 H2B 107.6 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C4 C4 C5 121.8(4) 6_556 . ? C4 C4 S2 121.0(2) 6_556 . ? C5 C4 S2 117.1(5) . . ? N2 C5 C4 178.3(9) . . ? _diffrn_measured_fraction_theta_max 0.498 _diffrn_reflns_theta_full 25.08 _diffrn_measured_fraction_theta_full 0.498 _refine_diff_density_max 0.623 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.084 #==END