[(iPr3P)6Rh6H12]2+: A High-Hydride Content Octahedron that Bridges the Gap between Late and Early Transition Metal Clusters
Michael J. Ingleson; Mary F. Mahon; Paul R. Raithby; Andrew S. Weller; Journal of the American Chemical Society 126 (2004) 4784–4785; doi:10.1021/ja049402n

data_4112469
_publ_section_title
;
 [(iPr3P)6Rh6H12]2+: A High-Hydride Content Octahedron that Bridges the
 Gap between Late and Early Transition Metal Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4784
_journal_page_last               4785
_journal_paper_doi               10.1021/ja049402n
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C82.5 H206 B22 P6 Rh6'
_chemical_formula_weight         2239.57
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.30
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.50300(10)
_cell_length_b                   25.48900(10)
_cell_length_c                   21.82500(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      12
_cell_volume                     11641.23(9)
_computing_data_reduction
'Denzo and Scalepack (otwinowski & Minor, 1997'
_computing_molecular_graphics    'ORTEX (P.McArdle, 1995)'
_computing_publication_material  'SHELXL-97/2 (Sheldrick,1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       KappaCCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            205546
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Nearly_black
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       Block
_exptl_crystal_F_000             4684
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.629
_refine_diff_density_min         -2.201
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         33956
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0480
_refine_ls_shift/su_max          1.169
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0406P)^2^+23.9538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                23910
_reflns_number_total             33956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja049402nsi20040203_034043.cif
_cod_data_source_block           c:\x-ray\k03asw23\maxus\k03asw23
_cod_original_cell_volume        11641.32(9)
_cod_original_formula_sum        'C82.50 H206 B22 P6 Rh6'
_cod_database_code               4112469