High Hydride Count Rhodium Octahedra, [Rh6(PR3)6H12][BArF4]2: Synthesis, Structures, and Reversible Hydrogen Uptake under Mild Conditions
Simon K. Brayshaw; Michael J. Ingleson; Jennifer C. Green; J. Scott McIndoe; Paul R. Raithby; Gabriele Kociok-Köhn; Andrew S. Weller; Journal of the American Chemical Society 128 (2006) 6247–6263; doi:10.1021/ja0604663

data_4110593
_publ_contact_author_address
;Department of Chemistry
University of Bath
Bath, BA2 7AY
United Kingdom
;
_publ_contact_author_email       a.s.weller@bath.ac.uk
_publ_contact_author_fax         '44 1225 82 6231'
_publ_contact_author_name        'Andrew S.Weller'
_publ_contact_author_phone       '44 1225 38 3394'
_publ_section_title
;
 High Hydride Count Rhodium Octahedra, [Rh6(PR3)6H12][BArF4]2: Synthesis,
 Structures, and Reversible Hydrogen Uptake under Mild Conditions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6247
_journal_page_last               6263
_journal_paper_doi               10.1021/ja0604663
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C50 H47 B F25 P2 Rh'
_chemical_formula_weight         1298.54
_chemical_name_common            'Compound 5'
_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                 109.9230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.8930(2)
_cell_length_b                   16.8620(2)
_cell_length_c                   20.1470(2)
_cell_measurement_temperature    150(2)
_cell_volume                     5395.41(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0428
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            68282
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.78
_exptl_absorpt_coefficient_mu    0.497
_exptl_absorpt_correction_T_max  0.8858
_exptl_absorpt_correction_T_min  0.7891
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_F_000             2608
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.680
_refine_diff_density_min         -0.691
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     793
_refine_ls_number_reflns         12293
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0549
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0427P)^2^+3.5859P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0904
_reflns_number_gt                9482
_reflns_number_total             12293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0604663si20060201_035932_4.cif
_cod_data_source_block           h05asw8
_cod_original_cell_volume        5395.40(11)
_cod_database_code               4110593