Sequential Reduction of High Hydride Count Octahedral Rhodium Clusters [Rh6(PR3)6H12][BArF4]2: Redox-Switchable Hydrogen Storage
Simon K. Brayshaw; Andrew Harrison; J. Scott McIndoe; Frank Marken; Paul R. Raithby; John E. Warren; Andrew S. Weller; Journal of the American Chemical Society 129 (2007) 1793–1804; doi:10.1021/ja066940m

data_4109068
_publ_section_title
;
 Sequential Reduction of High Hydride Count Octahedral Rhodium Clusters
 [Rh6(PR3)6H12][BArF4]2: Redox-Switchable Hydrogen Storage
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1793
_journal_page_last               1804
_journal_paper_doi               10.1021/ja066940m
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C54 H138 P6 Rh6'
_chemical_formula_weight         1590.92
_chemical_name_common            iPr-[H12]
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           'rhombohedral (hexagonal axes)'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   13.4673(5)
_cell_length_b                   13.4673(5)
_cell_length_c                   33.922(2)
_cell_measurement_reflns_used    11064
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.80
_cell_measurement_theta_min      3.60
_cell_volume                     5328.1(4)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'Bruker APEX II SMART control software'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX II'
_diffrn_measurement_method       'omega scans, narrow slicing'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Station 9.8, SRS'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.84600
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            11064
_diffrn_reflns_theta_full        29.80
_diffrn_reflns_theta_max         29.80
_diffrn_reflns_theta_min         3.60
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   Semi-empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2001)'
_exptl_crystal_colour            'Dark red'
_exptl_crystal_density_diffrn    1.487
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2466
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     114
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0185
_refine_ls_R_factor_gt           0.0179
_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^)+(0.0238P)^2^+7.9421P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0454
_refine_ls_wR_factor_ref         0.0459
_reflns_number_gt                1936
_reflns_number_total             2004
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066940msi20060927_050208_2.cif
_cod_data_source_block           bath169
_cod_original_cell_volume        5328.1(5)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4109068