Chemistry of Transition-Metal Clusters with Mixed Sb/S Ligands: Evidence for a Terminal SbS Double Bond in Cp*3Rh3Sb2S5 (Cp* = C5Me5)
Andreas Lange; Marek M. Kubicki; Joachim Wachter; Manfred Zabel; Inorganic Chemistry 44 (2005) 7328–7332; doi:10.1021/ic050493e

data_4309730
_publ_section_title
;
Chemistry of Transition-Metal Clusters with Mixed Sb/S Ligands: Evidence
for a Terminal SbS Double Bond in Cp*3Rh3Sb2S5 (Cp* = C5Me5)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7328
_journal_page_last               7332
_journal_paper_doi               10.1021/ic050493e
_journal_volume                  44
_journal_year                    2005
_chemical_compound_source        'see text'
_chemical_formula_moiety
'2(C40 H60 Rh4 S4.61), 2(C40 H60 Rh4 S5), 2(C7 H8)'
_chemical_formula_sum            'C174 H256 Rh16 S19.22'
_chemical_formula_weight         4610.74
_chemical_name_systematic        ' ?'
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      11
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 100.017(8)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   11.3831(7)
_cell_length_b                   17.0652(14)
_cell_length_c                   24.2939(16)
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.83
_cell_measurement_theta_min      1.82
_cell_volume                     4647.3(6)
_computing_cell_refinement       'STOE (1998)'
_computing_data_collection       'STOE (1998)'
_computing_data_reduction        'STOE (1998)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1993)'
_diffrn_ambient_temperature      173(1)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'STOE-IPDS diffractometer'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0497
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            32582
_diffrn_reflns_reduction_process ' ?'
_diffrn_reflns_theta_full        25.83
_diffrn_reflns_theta_max         25.83
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.640
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.6443
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
'analytical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_crystal_colour            'brown to black'
_exptl_crystal_density_diffrn    1.648
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_refine_diff_density_max         1.705
_refine_diff_density_min         -1.004
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.924
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         9054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.924
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0615P)^2^]         where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1054
_reflns_number_gt                6215
_reflns_number_total             9054
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic050493esi20050404_071730.cif
_cod_data_source_block           d140
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               4309730