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_4309731
_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         '(C30 H45 Rh3 S5 Sb2), (C4 H8 O)'
_chemical_formula_structural     '(C30 H45 Rh3 S5 Sb2), (C4 H8 O)'
_chemical_formula_sum            'C34 H53 O Rh3 S5 Sb2'
_chemical_formula_weight         1190.37
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 95.435(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0804(5)
_cell_length_b                   18.5111(10)
_cell_length_c                   21.9383(11)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.82
_cell_measurement_theta_min      1.86
_cell_volume                     4075.3(4)
_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 1.00
_diffrn_measured_fraction_theta_max 1.00
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0460
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39686
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.780
_exptl_absorpt_correction_T_max  0.7535
_exptl_absorpt_correction_T_min  0.3535
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
'numerical from crystal shape (X-SHAPE, X-RED. STOE, 1996)'
_exptl_crystal_colour            'brown to black'
_exptl_crystal_density_diffrn    1.940
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       platelike
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.892
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         7835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0390
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0325P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0594
_refine_ls_wR_factor_ref         0.0615
_reflns_number_gt                6227
_reflns_number_total             7835
_reflns_threshold_expression     I>4\\s(I)
_cod_data_source_file            ic050493esi20050404_071757.cif
_cod_data_source_block           b061
_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/c'
_cod_original_formula_sum        'C34 H53 O1 Rh3 S5 Sb2'
_cod_database_code               4309731