data_torry _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'Ni10 Rh5 S16' _chemical_formula_weight 1614.61 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+1/3, y+2/3, z+2/3' 'x+2/3, y+1/3, z+1/3' '-y, x-y, z' '-x+y, -x, z' '-y, -x, z' 'x, x-y, z' '-x+y, y, z' '-y+1/3, x-y+2/3, z+2/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+1/3, -x+2/3, z+2/3' '-x+y+2/3, -x+1/3, z+1/3' '-y+1/3, -x+2/3, z+2/3' '-y+2/3, -x+1/3, z+1/3' 'x+1/3, x-y+2/3, z+2/3' 'x+2/3, x-y+1/3, z+1/3' '-x+y+1/3, y+2/3, z+2/3' '-x+y+2/3, y+1/3, z+1/3' '-x, -y, -z' '-x-1/3, -y-2/3, -z-2/3' '-x-2/3, -y-1/3, -z-1/3' 'y, -x+y, -z' 'x-y, x, -z' 'y, x, -z' '-x, -x+y, -z' 'x-y, -y, -z' 'y-1/3, -x+y-2/3, -z-2/3' 'y-2/3, -x+y-1/3, -z-1/3' 'x-y-1/3, x-2/3, -z-2/3' 'x-y-2/3, x-1/3, -z-1/3' 'y-1/3, x-2/3, -z-2/3' 'y-2/3, x-1/3, -z-1/3' '-x-1/3, -x+y-2/3, -z-2/3' '-x-2/3, -x+y-1/3, -z-1/3' 'x-y-1/3, -y-2/3, -z-2/3' 'x-y-2/3, -y-1/3, -z-1/3' _cell_length_a 7.0600(10) _cell_length_b 7.0600(10) _cell_length_c 34.271(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1479.3(4) _cell_formula_units_Z 3 _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 5.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2283 _exptl_absorpt_coefficient_mu 15.040 _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 5720 _diffrn_reflns_av_R_equivalents 0.0126 _diffrn_reflns_av_sigmaI/netI 0.0065 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 30.08 _reflns_number_total 598 _reflns_number_gt 589 _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^)+(0.0072P)^2^+23.9614P] 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 0.000127(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 598 _refine_ls_number_parameters 40 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0165 _refine_ls_R_factor_gt 0.0162 _refine_ls_wR_factor_ref 0.0438 _refine_ls_wR_factor_gt 0.0437 _refine_ls_goodness_of_fit_ref 1.411 _refine_ls_restrained_S_all 1.411 _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_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 0.00609(11) Uani 1 4 d S . . Rh2 Rh 0.0000 0.0000 0.248907(15) 0.00618(13) Uani 1 6 d S . . Ni1 Ni 0.0000 0.0000 -0.05577(3) 0.01041(19) Uani 1 6 d S . . Ni2 Ni 0.0000 0.0000 0.56721(3) 0.00897(19) Uani 1 6 d S . . Ni3 Ni 0.50231(5) 0.49769(5) 0.188526(15) 0.00880(18) Uani 0.958(3) 2 d SP . . S5 S 0.3333 0.6667 0.1667 0.00880(18) Uani 0.042(3) 12 d SP . . S1 S 0.0000 0.0000 0.87776(5) 0.0110(3) Uani 1 6 d S . . S2 S 0.16060(8) 0.83940(8) 0.21053(3) 0.00825(19) Uani 1 2 d S . . S3 S 0.84988(8) 0.69976(17) 0.29399(3) 0.00741(18) Uani 1 2 d S . . S4 S 0.0000 0.0000 0.63177(5) 0.0076(3) Uani 1 6 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 0.00613(15) 0.0056(2) 0.00638(18) -0.00017(14) -0.00008(7) 0.00280(10) Rh2 0.00628(16) 0.00628(16) 0.0060(2) 0.000 0.000 0.00314(8) Ni1 0.0095(3) 0.0095(3) 0.0123(4) 0.000 0.000 0.00473(14) Ni2 0.0091(3) 0.0091(3) 0.0086(4) 0.000 0.000 0.00456(14) Ni3 0.0085(2) 0.0085(2) 0.0086(3) -0.00016(10) 0.00016(10) 0.0037(2) S5 0.0085(2) 0.0085(2) 0.0086(3) -0.00016(10) 0.00016(10) 0.0037(2) S1 0.0107(5) 0.0107(5) 0.0115(7) 0.000 0.000 0.0054(2) S2 0.0084(3) 0.0084(3) 0.0088(4) -0.00040(16) 0.00040(16) 0.0048(4) S3 0.0074(3) 0.0071(4) 0.0077(4) -0.0004(3) -0.00018(16) 0.0035(2) S4 0.0081(5) 0.0081(5) 0.0065(7) 0.000 0.000 0.0040(2) _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 S4 2.3631(9) 21_656 ? Rh1 S4 2.3631(9) 3_554 ? Rh1 S3 2.3664(7) 29_656 ? Rh1 S3 2.3664(7) 11_554 ? Rh1 S3 2.3664(7) 9_644 ? Rh1 S3 2.3664(7) 27_566 ? Rh2 S2 2.3635(10) 5_455 ? Rh2 S2 2.3635(11) 4_665 ? Rh2 S2 2.3635(10) 1_545 ? Rh2 S3 2.3994(11) 4_655 ? Rh2 S3 2.3994(11) 1_445 ? Rh2 S3 2.3994(11) 5_565 ? Ni1 S1 2.278(2) 1_554 ? Ni1 S3 2.3101(11) 2_444 ? Ni1 S3 2.3101(11) 9_544 ? Ni1 S3 2.3101(11) 11_554 ? Ni2 S4 2.2124(19) . ? Ni2 S2 2.2587(11) 10 ? Ni2 S2 2.2587(11) 12_455 ? Ni2 S2 2.2587(11) 3_445 ? Ni2 S5 2.3034(10) 3_445 ? Ni2 Ni3 2.5856(8) 12_455 ? Ni2 Ni3 2.5856(8) 3_445 ? Ni2 Ni3 2.5856(8) 10 ? Ni3 S1 2.1534(9) 3_554 ? Ni3 S5 2.1979(6) . ? Ni3 S2 2.2216(7) 5_565 ? Ni3 S2 2.2216(7) 4_665 ? Ni3 S2 2.2529(11) 20_676 ? Ni3 Ni3 2.5524(8) 27_566 ? Ni3 Ni3 2.5524(8) 29_666 ? Ni3 Ni2 2.5856(8) 2_554 ? S5 Ni3 2.1978(6) 4_665 ? S5 Ni3 2.1978(6) 5_565 ? S5 Ni3 2.1979(6) 20_676 ? S5 Ni3 2.1979(6) 27_566 ? S5 Ni3 2.1979(6) 29_666 ? S5 Ni2 2.3034(10) 21_666 ? S5 Ni2 2.3034(10) 2_554 ? S1 Ni3 2.1535(9) 9_545 ? S1 Ni3 2.1535(9) 11 ? S1 Ni3 2.1535(9) 2_445 ? S1 Ni1 2.278(2) 1_556 ? S2 Ni3 2.2216(7) 5_565 ? S2 Ni3 2.2216(7) 4_665 ? S2 Ni3 2.2530(11) 20_676 ? S2 Ni2 2.2588(11) 2_554 ? S2 Rh2 2.3636(10) 1_565 ? S3 Ni1 2.3101(11) 3 ? S3 Rh1 2.3665(7) 29_666 ? S3 Rh1 2.3665(7) 27_676 ? S3 Rh2 2.3994(11) 1_665 ? S4 Rh1 2.3630(9) 11 ? S4 Rh1 2.3631(9) 9_545 ? S4 Rh1 2.3631(9) 2_445 ? 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 S4 Rh1 S4 180.00(7) 21_656 3_554 ? S4 Rh1 S3 96.89(3) 21_656 29_656 ? S4 Rh1 S3 83.11(3) 3_554 29_656 ? S4 Rh1 S3 83.11(3) 21_656 11_554 ? S4 Rh1 S3 96.89(3) 3_554 11_554 ? S3 Rh1 S3 180.00(4) 29_656 11_554 ? S4 Rh1 S3 83.11(3) 21_656 9_644 ? S4 Rh1 S3 96.89(3) 3_554 9_644 ? S3 Rh1 S3 95.58(5) 29_656 9_644 ? S3 Rh1 S3 84.42(5) 11_554 9_644 ? S4 Rh1 S3 96.89(3) 21_656 27_566 ? S4 Rh1 S3 83.11(3) 3_554 27_566 ? S3 Rh1 S3 84.42(5) 29_656 27_566 ? S3 Rh1 S3 95.58(5) 11_554 27_566 ? S3 Rh1 S3 180.00(6) 9_644 27_566 ? S2 Rh2 S2 92.04(4) 5_455 4_665 ? S2 Rh2 S2 92.04(4) 5_455 1_545 ? S2 Rh2 S2 92.04(4) 4_665 1_545 ? S2 Rh2 S3 173.72(4) 5_455 4_655 ? S2 Rh2 S3 92.32(3) 4_665 4_655 ? S2 Rh2 S3 92.32(3) 1_545 4_655 ? S2 Rh2 S3 92.32(3) 5_455 1_445 ? S2 Rh2 S3 173.72(4) 4_665 1_445 ? S2 Rh2 S3 92.32(3) 1_545 1_445 ? S3 Rh2 S3 82.99(4) 4_655 1_445 ? S2 Rh2 S3 92.32(3) 5_455 5_565 ? S2 Rh2 S3 92.32(3) 4_665 5_565 ? S2 Rh2 S3 173.72(4) 1_545 5_565 ? S3 Rh2 S3 82.99(4) 4_655 5_565 ? S3 Rh2 S3 82.99(4) 1_445 5_565 ? S1 Ni1 S3 104.11(3) 1_554 2_444 ? S1 Ni1 S3 104.11(3) 1_554 9_544 ? S3 Ni1 S3 114.26(3) 2_444 9_544 ? S1 Ni1 S3 104.11(3) 1_554 11_554 ? S3 Ni1 S3 114.26(3) 2_444 11_554 ? S3 Ni1 S3 114.26(3) 9_544 11_554 ? S4 Ni2 S2 110.74(3) . 10 ? S4 Ni2 S2 110.74(3) . 12_455 ? S2 Ni2 S2 108.17(3) 10 12_455 ? S4 Ni2 S2 110.74(3) . 3_445 ? S2 Ni2 S2 108.17(3) 10 3_445 ? S2 Ni2 S2 108.17(3) 12_455 3_445 ? S4 Ni2 S5 180.0 . 3_445 ? S2 Ni2 S5 69.26(3) 10 3_445 ? S2 Ni2 S5 69.26(3) 12_455 3_445 ? S2 Ni2 S5 69.26(3) 3_445 3_445 ? S4 Ni2 Ni3 126.95(2) . 12_455 ? S2 Ni2 Ni3 54.085(17) 10 12_455 ? S2 Ni2 Ni3 122.31(5) 12_455 12_455 ? S2 Ni2 Ni3 54.085(17) 3_445 12_455 ? S5 Ni2 Ni3 53.05(2) 3_445 12_455 ? S4 Ni2 Ni3 126.95(2) . 3_445 ? S2 Ni2 Ni3 54.085(17) 10 3_445 ? S2 Ni2 Ni3 54.086(17) 12_455 3_445 ? S2 Ni2 Ni3 122.31(5) 3_445 3_445 ? S5 Ni2 Ni3 53.05(2) 3_445 3_445 ? Ni3 Ni2 Ni3 87.59(3) 12_455 3_445 ? S4 Ni2 Ni3 126.95(2) . 10 ? S2 Ni2 Ni3 122.31(5) 10 10 ? S2 Ni2 Ni3 54.085(17) 12_455 10 ? S2 Ni2 Ni3 54.085(17) 3_445 10 ? S5 Ni2 Ni3 53.05(2) 3_445 10 ? Ni3 Ni2 Ni3 87.59(3) 12_455 10 ? Ni3 Ni2 Ni3 87.59(3) 3_445 10 ? S1 Ni3 S5 178.88(5) 3_554 . ? S1 Ni3 S2 107.60(3) 3_554 5_565 ? S5 Ni3 S2 71.84(3) . 5_565 ? S1 Ni3 S2 107.60(3) 3_554 4_665 ? S5 Ni3 S2 71.84(3) . 4_665 ? S2 Ni3 S2 110.86(5) 5_565 4_665 ? S1 Ni3 S2 109.87(6) 3_554 20_676 ? S5 Ni3 S2 71.24(3) . 20_676 ? S2 Ni3 S2 110.41(3) 5_565 20_676 ? S2 Ni3 S2 110.41(3) 4_665 20_676 ? S1 Ni3 Ni3 126.06(2) 3_554 27_566 ? S5 Ni3 Ni3 54.505(7) . 27_566 ? S2 Ni3 Ni3 126.34(2) 5_565 27_566 ? S2 Ni3 Ni3 55.80(3) 4_665 27_566 ? S2 Ni3 Ni3 54.64(2) 20_676 27_566 ? S1 Ni3 Ni3 126.06(2) 3_554 29_666 ? S5 Ni3 Ni3 54.505(7) . 29_666 ? S2 Ni3 Ni3 55.80(3) 5_565 29_666 ? S2 Ni3 Ni3 126.34(2) 4_665 29_666 ? S2 Ni3 Ni3 54.64(2) 20_676 29_666 ? Ni3 Ni3 Ni3 89.03(3) 27_566 29_666 ? S1 Ni3 Ni2 122.00(6) 3_554 2_554 ? S5 Ni3 Ni2 56.88(2) . 2_554 ? S2 Ni3 Ni2 55.43(3) 5_565 2_554 ? S2 Ni3 Ni2 55.43(3) 4_665 2_554 ? S2 Ni3 Ni2 128.12(4) 20_676 2_554 ? Ni3 Ni3 Ni2 91.69(2) 27_566 2_554 ? Ni3 Ni3 Ni2 91.69(2) 29_666 2_554 ? Ni3 S5 Ni3 109.012(15) 4_665 5_565 ? Ni3 S5 Ni3 109.012(15) 4_665 . ? Ni3 S5 Ni3 109.012(15) 5_565 . ? Ni3 S5 Ni3 70.989(15) 4_665 20_676 ? Ni3 S5 Ni3 70.989(15) 5_565 20_676 ? Ni3 S5 Ni3 180.0 . 20_676 ? Ni3 S5 Ni3 180.0 4_665 27_566 ? Ni3 S5 Ni3 70.990(15) 5_565 27_566 ? Ni3 S5 Ni3 70.991(15) . 27_566 ? Ni3 S5 Ni3 109.008(15) 20_676 27_566 ? Ni3 S5 Ni3 70.990(15) 4_665 29_666 ? Ni3 S5 Ni3 180.0 5_565 29_666 ? Ni3 S5 Ni3 70.991(15) . 29_666 ? Ni3 S5 Ni3 109.008(15) 20_676 29_666 ? Ni3 S5 Ni3 109.008(15) 27_566 29_666 ? Ni3 S5 Ni2 109.926(15) 4_665 21_666 ? Ni3 S5 Ni2 109.926(15) 5_565 21_666 ? Ni3 S5 Ni2 109.928(15) . 21_666 ? Ni3 S5 Ni2 70.071(15) 20_676 21_666 ? Ni3 S5 Ni2 70.069(15) 27_566 21_666 ? Ni3 S5 Ni2 70.069(15) 29_666 21_666 ? Ni3 S5 Ni2 70.075(15) 4_665 2_554 ? Ni3 S5 Ni2 70.075(15) 5_565 2_554 ? Ni3 S5 Ni2 70.070(15) . 2_554 ? Ni3 S5 Ni2 109.931(15) 20_676 2_554 ? Ni3 S5 Ni2 109.930(14) 27_566 2_554 ? Ni3 S5 Ni2 109.930(15) 29_666 2_554 ? Ni2 S5 Ni2 180.0 21_666 2_554 ? Ni3 S1 Ni3 107.85(5) 9_545 11 ? Ni3 S1 Ni3 107.85(5) 9_545 2_445 ? Ni3 S1 Ni3 107.85(5) 11 2_445 ? Ni3 S1 Ni1 111.05(5) 9_545 1_556 ? Ni3 S1 Ni1 111.05(5) 11 1_556 ? Ni3 S1 Ni1 111.05(5) 2_445 1_556 ? Ni3 S2 Ni3 107.31(5) 5_565 4_665 ? Ni3 S2 Ni3 69.55(3) 5_565 20_676 ? Ni3 S2 Ni3 69.55(3) 4_665 20_676 ? Ni3 S2 Ni2 70.49(3) 5_565 2_554 ? Ni3 S2 Ni2 70.49(3) 4_665 2_554 ? Ni3 S2 Ni2 109.58(5) 20_676 2_554 ? Ni3 S2 Rh2 126.34(3) 5_565 1_565 ? Ni3 S2 Rh2 126.34(3) 4_665 1_565 ? Ni3 S2 Rh2 124.98(5) 20_676 1_565 ? Ni2 S2 Rh2 125.44(5) 2_554 1_565 ? Ni1 S3 Rh1 118.27(3) 3 29_666 ? Ni1 S3 Rh1 118.27(3) 3 27_676 ? Rh1 S3 Rh1 96.46(4) 29_666 27_676 ? Ni1 S3 Rh2 125.80(5) 3 1_665 ? Rh1 S3 Rh2 95.90(3) 29_666 1_665 ? Rh1 S3 Rh2 95.90(3) 27_676 1_665 ? Ni2 S4 Rh1 120.41(4) . 11 ? Ni2 S4 Rh1 120.41(4) . 9_545 ? Rh1 S4 Rh1 96.65(5) 11 9_545 ? Ni2 S4 Rh1 120.41(4) . 2_445 ? Rh1 S4 Rh1 96.65(5) 11 2_445 ? Rh1 S4 Rh1 96.65(5) 9_545 2_445 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.264 _refine_diff_density_min -1.289 _refine_diff_density_rms 0.142