Chemistry of 11-vertex rhodathiaboranes: reactions with monodentate phosphines.
Calvo, Beatriz; Kess, Martin; Macías, Ramón; Cunchillos, Carmen; Lahoz, Fernando J.; Kennedy, John D.; Oro, Luis A.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 6555–6564; doi:10.1039/c1dt10355e

data_7015933
_publ_section_title
;
 Chemistry of 11-vertex rhodathiaboranes: reactions with monodentate
 phosphines.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6555
_journal_page_last               6564
_journal_paper_doi               10.1039/c1dt10355e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C39 H49 B9 P3 Rh S, 0.5 (C6 H14)'
_chemical_formula_sum            'C42 H56 B9 P3 Rh S'
_chemical_formula_weight         886.04
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.9350(10)
_cell_angle_beta                 82.6070(10)
_cell_angle_gamma                65.0700(10)
_cell_formula_units_Z            2
_cell_length_a                   11.4960(10)
_cell_length_b                   12.6030(10)
_cell_length_c                   17.1240(10)
_cell_measurement_reflns_used    43398
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.304
_cell_measurement_theta_min      1.892
_cell_volume                     2181.4(3)
_computing_cell_refinement       'HKL2000 (Z. Otwinowski & W. Minor, 1997)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'HKL2000 (Z. Otwinowski & W. Minor, 1997)'
_computing_molecular_graphics    'XP program, SHELXTL v6.10,Bruker2000'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_detector_type            'ADSC Q210r CCD (binned mode)'
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.749
_diffrn_measurement_details      '1 degree, 1 sec, detector distance 63.50 mm'
_diffrn_measurement_device_type  'Single axis HUBER diffractometer'
_diffrn_measurement_method       phi-scans
_diffrn_radiation_monochromator  'Si 111 double crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.73780
_diffrn_reflns_av_R_equivalents  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0308
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            43398
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         33.30
_diffrn_reflns_theta_min         1.89
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF CRG BM16'
_exptl_absorpt_coefficient_mu    0.577
_exptl_absorpt_correction_T_max  0.9886
_exptl_absorpt_correction_T_min  0.9446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
R.H. Blessing, Acta Cryst. (1995) A51, 33-38
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.279
_refine_diff_density_min         -1.886
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.0382(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     576
_refine_ls_number_reflns         11291
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0423
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0688P)^2^+1.7632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1091
_refine_ls_wR_factor_ref         0.1105
_reflns_number_gt                10602
_reflns_number_total             11291
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10355e.txt
_cod_data_source_block           compound_9
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7015933