Chemistry of a Metallathiaborane Cluster. 5.†Reaction of [8,8-(η2-dppm)-8-(η1-dppm)-nido-8,7-RhSB9H10] and Its Derivatives with Organotransition-Metal Reagents
Volkov, Oleg; Rath, Nigam P.; Barton, Lawrence; Organometallics 21 (2002) 5505–; doi:10.1021/om020480y

data_4077046
_publ_section_title
;
 Chemistry of a Metallathiaborane Cluster. 5.&#x2020;Reaction of
 [8,8-(\h2-dppm)-8-(\h1-dppm)-nido-8,7-RhSB9H10] and Its Derivatives with
 Organotransition-Metal Reagents
;
_journal_issue                   25
_journal_name_full               Organometallics
_journal_page_first              5505
_journal_paper_doi               10.1021/om020480y
_journal_volume                  21
_journal_year                    2002
_chemical_formula_sum            'C45.5 H49 B9 Cl6 P3 Rh S'
_chemical_formula_weight         1133.72
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.631(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.4160(4)
_cell_length_b                   20.7474(5)
_cell_length_c                   16.8186(4)
_cell_measurement_reflns_used    9758
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.8
_cell_measurement_theta_min      2.4
_cell_volume                     5164.6(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker-SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'Bruker-SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'Bruker-SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'Bruker-SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.12
_diffrn_reflns_av_sigmaI/netI    0.0679
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            101621
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.808
_exptl_absorpt_correction_T_max  0.8953
_exptl_absorpt_correction_T_min  0.7936
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2300
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.343
_refine_diff_density_min         -1.393
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         10519
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1059
_refine_ls_R_factor_gt           0.0704
_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^)+(0.0801P)^2^+21.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1903
_reflns_number_gt                7485
_reflns_number_total             10519
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om020480y.cif
_cod_data_source_block           Compd8
_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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'no' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P2~1~/c
_cod_original_formula_sum        'C45.50 H49 B9 Cl6 P3 Rh S'
_cod_database_code               4077046