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_4109067
_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_moiety         'C108 H210 P6 Rh6, C32 H12 B F24, 5.5(C7 H8)'
_chemical_formula_sum            'C178.5 H265.5 B F24 P6 Rh6'
_chemical_formula_weight         3681.50
_chemical_name_common            Cy-[H12]+
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/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                 90.13
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.34200(10)
_cell_length_b                   24.4480(2)
_cell_length_c                   35.3600(3)
_cell_measurement_reflns_used    188199
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.508
_cell_measurement_theta_min      2.91
_cell_volume                     17585.2(2)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'Collect, Nonius program suite version 1.9 (1997)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
'ORTEP3 for Windows - L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material  'SHELX97-2, G. M. Sheldrick'
_computing_structure_refinement
;
 SHELX97-2 Program for Crystal Structure Analysis. G. M. Sheldrick,
 Institut f. Anorg. Chemie der Universit\"at, Tammanstrasse 4, 
 D-3400 G\"ottingen, Germany, 1998.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119.
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '770 1.0 degree images with \f and \w scans'
_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  0.0595
_diffrn_reflns_av_sigmaI/netI    0.0603
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            188785
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         3.53
_exptl_absorpt_coefficient_mu    0.679
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_description       slab
_exptl_crystal_F_000             7670
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.903
_refine_diff_density_min         -1.414
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2222
_refine_ls_number_reflns         43989
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0363P)^2^+18.2124P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.1065
_reflns_number_gt                24422
_reflns_number_total             43989
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja066940msi20060927_050208_1.cif
_cod_data_source_block           h06asw5
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_original_formula_sum        'C178.50 H265.50 B F24 P6 Rh6'
_cod_database_code               4109067