Phosphine-Boranes as Bidentate Ligands: Formation of [8,8-η2-{η2-(BH3).dppm}-nido-8,7-RhSB9H10] and [9,9-η2-{η2-(BH3).dppm}-nido-9,7,8-RhC2B8H11] from [8,8-(η2-dppm)-8-(η1-dppm)-nido-8,7-RhSB9H10] and [9,9-(η2-dppm)-9-(η1-dppm)-nido-9,7,8-RhC2B8H11], Respectively
Oleg Volkov; Ramón Macías; Nigam P. Rath; Lawrence Barton; Inorganic Chemistry 41 (2002) 5837–5843; doi:10.1021/ic0258375

data_4318794
_publ_section_title
;
 Phosphine-Boranes as Bidentate Ligands: Formation of
 [8,8-\h2-{\h2-(BH3).dppm}-nido-8,7-RhSB9H10] and
 [9,9-\h2-{\h2-(BH3).dppm}-nido-9,7,8-RhC2B8H11] from
 [8,8-(\h2-dppm)-8-(\h1-dppm)-nido-8,7-RhSB9H10] and
 [9,9-(\h2-dppm)-9-(\h1-dppm)-nido-9,7,8-RhC2B8H11], Respectively
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5837
_journal_page_last               5843
_journal_paper_doi               10.1021/ic0258375
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C25 H35 B10 P2 Rh S'
_chemical_formula_weight         640.54
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 94.898(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2721(1)
_cell_length_b                   11.5727(1)
_cell_length_c                   19.9181(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     3048.13(5)
_computing_cell_refinement       'Siemens SMART'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL (Sheldrick, 1993)'
_computing_publication_material  'Siemens SHELXTL (Sheldrick, 1993)'
_computing_structure_refinement  'Siemens SHELXTL(Sheldrick, 1993)'
_computing_structure_solution    'Siemens SHELXTL(Sheldrick, 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens CCD'
_diffrn_measurement_method       '\w 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  0.07
_diffrn_reflns_av_sigmaI/netI    0.0390
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            61274
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0
_diffrn_standards_number         'CCD data, see expt'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.83
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.688
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_obs   1.067
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         6943
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_obs          0.0303
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.5274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0661
_refine_ls_wR_factor_obs         0.0597
_reflns_number_observed          5641
_reflns_number_total             6964
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0258375_s1_1.cif
_cod_data_source_block           Compd3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.5274P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+1.5274P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4318794