data_rhrichpnlike _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ni3.75 Rh0.38 S4' _chemical_formula_weight 386.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source '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' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, z' '-y, -x, z' 'y, -x, -z' '-y, x, -z' 'x, z, y' '-x, z, -y' '-x, -z, y' 'x, -z, -y' 'z, y, x' 'z, -y, -x' '-z, y, -x' '-z, -y, x' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x+1/2, y+1/2' 'z, -x+1/2, -y+1/2' '-z, -x+1/2, y+1/2' '-z, x+1/2, -y+1/2' 'y, z+1/2, x+1/2' '-y, z+1/2, -x+1/2' 'y, -z+1/2, -x+1/2' '-y, -z+1/2, x+1/2' 'y, x+1/2, z+1/2' '-y, -x+1/2, z+1/2' 'y, -x+1/2, -z+1/2' '-y, x+1/2, -z+1/2' 'x, z+1/2, y+1/2' '-x, z+1/2, -y+1/2' '-x, -z+1/2, y+1/2' 'x, -z+1/2, -y+1/2' 'z, y+1/2, x+1/2' 'z, -y+1/2, -x+1/2' '-z, y+1/2, -x+1/2' '-z, -y+1/2, x+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+1/2, y, -z+1/2' 'x+1/2, -y, -z+1/2' 'z+1/2, x, y+1/2' 'z+1/2, -x, -y+1/2' '-z+1/2, -x, y+1/2' '-z+1/2, x, -y+1/2' 'y+1/2, z, x+1/2' '-y+1/2, z, -x+1/2' 'y+1/2, -z, -x+1/2' '-y+1/2, -z, x+1/2' 'y+1/2, x, z+1/2' '-y+1/2, -x, z+1/2' 'y+1/2, -x, -z+1/2' '-y+1/2, x, -z+1/2' 'x+1/2, z, y+1/2' '-x+1/2, z, -y+1/2' '-x+1/2, -z, y+1/2' 'x+1/2, -z, -y+1/2' 'z+1/2, y, x+1/2' 'z+1/2, -y, -x+1/2' '-z+1/2, y, -x+1/2' '-z+1/2, -y, x+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' 'z+1/2, x+1/2, y' 'z+1/2, -x+1/2, -y' '-z+1/2, -x+1/2, y' '-z+1/2, x+1/2, -y' 'y+1/2, z+1/2, x' '-y+1/2, z+1/2, -x' 'y+1/2, -z+1/2, -x' '-y+1/2, -z+1/2, x' 'y+1/2, x+1/2, z' '-y+1/2, -x+1/2, z' 'y+1/2, -x+1/2, -z' '-y+1/2, x+1/2, -z' 'x+1/2, z+1/2, y' '-x+1/2, z+1/2, -y' '-x+1/2, -z+1/2, y' 'x+1/2, -z+1/2, -y' 'z+1/2, y+1/2, x' 'z+1/2, -y+1/2, -x' '-z+1/2, y+1/2, -x' '-z+1/2, -y+1/2, x' _cell_length_a 10.066(5) _cell_length_b 10.066(5) _cell_length_c 10.066(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1019.9(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 5.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1487 _exptl_absorpt_coefficient_mu 16.285 _exptl_absorpt_correction_type ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2962 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0079 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 29.95 _reflns_number_total 186 _reflns_number_gt 186 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0148P)^2^+0.6851P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.49(4) _refine_ls_number_reflns 186 _refine_ls_number_parameters 17 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0104 _refine_ls_R_factor_gt 0.0104 _refine_ls_wR_factor_ref 0.0229 _refine_ls_wR_factor_gt 0.0229 _refine_ls_goodness_of_fit_ref 1.206 _refine_ls_restrained_S_all 1.206 _refine_ls_shift/su_max 0.000 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.5000 0.0000 0.0000 0.00947(15) Uani 0.616(9) 24 d SP . . Ni3 Ni 0.5000 0.0000 0.0000 0.00947(15) Uani 0.384(9) 24 d SP . . Ni1 Ni 0.62693(9) 0.37307(9) 0.12693(9) 0.0128(6) Uani 1 6 d S . . Ni2 Ni 0.62562(9) 0.62562(9) 0.12562(9) 0.0097(6) Uani 0.935(6) 6 d SP . . S3 S 0.7500 0.7500 0.2500 0.0175(18) Uani 1 24 d S . . S1 S 0.5000 0.23944(5) 0.0000 0.01075(15) Uani 1 4 d S . . S2 S 0.7500 0.2500 0.2500 0.0081(12) Uani 1 24 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.00947(15) 0.00947(15) 0.00947(15) 0.000 0.000 0.000 Ni3 0.00947(15) 0.00947(15) 0.00947(15) 0.000 0.000 0.000 Ni1 0.0128(6) 0.0128(6) 0.0128(6) 0.0012(3) -0.0012(3) 0.0012(3) Ni2 0.0097(6) 0.0097(6) 0.0097(6) 0.0016(3) 0.0016(3) 0.0016(3) S3 0.0175(18) 0.0175(18) 0.0175(18) 0.000 0.000 0.000 S1 0.01121(18) 0.0098(2) 0.01121(18) 0.000 -0.0006(10) 0.000 S2 0.0081(12) 0.0081(12) 0.0081(12) 0.000 0.000 0.000 _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 Rh1 S1 2.4102(13) 58 ? Rh1 S1 2.4102(13) 57_554 ? Rh1 S1 2.4102(13) 2_655 ? Rh1 S1 2.4102(13) 77_545 ? Rh1 S1 2.4102(13) 78 ? Rh1 S1 2.4102(13) . ? Ni1 S2 2.1457(19) . ? Ni1 S1 2.2526(13) . ? Ni1 S1 2.2526(13) 34_655 ? Ni1 S1 2.2526(13) 54_565 ? Ni1 Ni2 2.5423(13) . ? Ni1 Ni2 2.5423(13) 4_565 ? Ni1 Ni2 2.5423(13) 2_665 ? Ni2 S3 2.1685(18) . ? Ni2 S1 2.2456(12) 34_655 ? Ni2 S1 2.2456(12) 54_565 ? Ni2 S1 2.2456(12) 2_665 ? Ni2 Ni1 2.5423(13) 2_665 ? Ni2 Ni1 2.5423(13) 4_565 ? S3 Ni2 2.1684(18) 28_565 ? S3 Ni2 2.1684(18) 51_655 ? S3 Ni2 2.1684(18) 74_665 ? S1 Ni2 2.2456(12) 4_565 ? S1 Ni2 2.2456(12) 2_665 ? S1 Ni1 2.2526(13) 3_655 ? S2 Ni1 2.1457(19) 51_655 ? S2 Ni1 2.1457(19) 28 ? S2 Ni1 2.1457(19) 74_655 ? 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 S1 Rh1 S1 180.0 58 57_554 ? S1 Rh1 S1 90.0 58 2_655 ? S1 Rh1 S1 90.0 57_554 2_655 ? S1 Rh1 S1 90.0 58 77_545 ? S1 Rh1 S1 90.0 57_554 77_545 ? S1 Rh1 S1 90.0 2_655 77_545 ? S1 Rh1 S1 90.0 58 78 ? S1 Rh1 S1 90.0 57_554 78 ? S1 Rh1 S1 90.0 2_655 78 ? S1 Rh1 S1 180.0 77_545 78 ? S1 Rh1 S1 90.0 58 . ? S1 Rh1 S1 90.0 57_554 . ? S1 Rh1 S1 180.0 2_655 . ? S1 Rh1 S1 90.0 77_545 . ? S1 Rh1 S1 90.0 78 . ? S2 Ni1 S1 108.07(4) . . ? S2 Ni1 S1 108.07(4) . 34_655 ? S1 Ni1 S1 110.83(3) . 34_655 ? S2 Ni1 S1 108.07(4) . 54_565 ? S1 Ni1 S1 110.83(3) . 54_565 ? S1 Ni1 S1 110.83(3) 34_655 54_565 ? S2 Ni1 Ni2 125.68(6) . . ? S1 Ni1 Ni2 126.24(9) . . ? S1 Ni1 Ni2 55.456(18) 34_655 . ? S1 Ni1 Ni2 55.456(18) 54_565 . ? S2 Ni1 Ni2 125.68(6) . 4_565 ? S1 Ni1 Ni2 55.456(18) . 4_565 ? S1 Ni1 Ni2 55.456(18) 34_655 4_565 ? S1 Ni1 Ni2 126.24(9) 54_565 4_565 ? Ni2 Ni1 Ni2 89.40(8) . 4_565 ? S2 Ni1 Ni2 125.68(6) . 2_665 ? S1 Ni1 Ni2 55.456(18) . 2_665 ? S1 Ni1 Ni2 126.24(9) 34_655 2_665 ? S1 Ni1 Ni2 55.456(18) 54_565 2_665 ? Ni2 Ni1 Ni2 89.40(8) . 2_665 ? Ni2 Ni1 Ni2 89.41(8) 4_565 2_665 ? S3 Ni2 S1 107.52(4) . 34_655 ? S3 Ni2 S1 107.52(4) . 54_565 ? S1 Ni2 S1 111.35(4) 34_655 54_565 ? S3 Ni2 S1 107.52(4) . 2_665 ? S1 Ni2 S1 111.35(4) 34_655 2_665 ? S1 Ni2 S1 111.35(4) 54_565 2_665 ? S3 Ni2 Ni1 124.84(6) . 2_665 ? S1 Ni2 Ni1 127.64(10) 34_655 2_665 ? S1 Ni2 Ni1 55.716(19) 54_565 2_665 ? S1 Ni2 Ni1 55.716(19) 2_665 2_665 ? S3 Ni2 Ni1 124.84(6) . 4_565 ? S1 Ni2 Ni1 55.716(19) 34_655 4_565 ? S1 Ni2 Ni1 127.64(10) 54_565 4_565 ? S1 Ni2 Ni1 55.716(19) 2_665 4_565 ? Ni1 Ni2 Ni1 90.59(8) 2_665 4_565 ? S3 Ni2 Ni1 124.84(6) . . ? S1 Ni2 Ni1 55.716(19) 34_655 . ? S1 Ni2 Ni1 55.716(19) 54_565 . ? S1 Ni2 Ni1 127.64(10) 2_665 . ? Ni1 Ni2 Ni1 90.59(8) 2_665 . ? Ni1 Ni2 Ni1 90.59(8) 4_565 . ? Ni2 S3 Ni2 109.5 28_565 51_655 ? Ni2 S3 Ni2 109.471(1) 28_565 74_665 ? Ni2 S3 Ni2 109.471(1) 51_655 74_665 ? Ni2 S3 Ni2 109.5 28_565 . ? Ni2 S3 Ni2 109.5 51_655 . ? Ni2 S3 Ni2 109.5 74_665 . ? Ni2 S1 Ni2 105.57(8) 4_565 2_665 ? Ni2 S1 Ni1 68.829(12) 4_565 3_655 ? Ni2 S1 Ni1 68.829(12) 2_665 3_655 ? Ni2 S1 Ni1 68.829(12) 4_565 . ? Ni2 S1 Ni1 68.829(12) 2_665 . ? Ni1 S1 Ni1 106.67(7) 3_655 . ? Ni2 S1 Rh1 127.22(4) 4_565 . ? Ni2 S1 Rh1 127.22(4) 2_665 . ? Ni1 S1 Rh1 126.66(4) 3_655 . ? Ni1 S1 Rh1 126.66(4) . . ? Ni1 S2 Ni1 109.5 . 51_655 ? Ni1 S2 Ni1 109.5 . 28 ? Ni1 S2 Ni1 109.5 51_655 28 ? Ni1 S2 Ni1 109.5 . 74_655 ? Ni1 S2 Ni1 109.5 51_655 74_655 ? Ni1 S2 Ni1 109.5 28 74_655 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 29.95 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.361 _refine_diff_density_min -0.971 _refine_diff_density_rms 0.237