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_4110591
_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_moiety
'[(C108 H201 P6 Rh6)+2(B11 C12 H34)-(C H2 Cl2)]'
_chemical_formula_sum            'C133 H271 B22 Cl2 P6 Rh6'
_chemical_formula_weight         2982.50
_chemical_name_common            'Compound 2b[CB11Me11H]2'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.6720(2)
_cell_length_b                   28.0280(3)
_cell_length_c                   31.0780(5)
_cell_measurement_reflns_used    78163
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.1
_cell_measurement_theta_min      2.91
_cell_volume                     15393.3(3)
_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 0.923
_diffrn_measured_fraction_theta_max 0.923
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '244 1.5 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  0.0614
_diffrn_reflns_av_sigmaI/netI    0.1022
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            64581
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         3.55
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.769
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       prism
_exptl_crystal_F_000             6292
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.136
_refine_diff_density_min         -1.106
_refine_diff_density_rms         0.114
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.45(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1535
_refine_ls_number_reflns         27469
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0940
_refine_ls_R_factor_gt           0.0561
_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^)+(0.0523P)^2^+11.5426P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1105
_refine_ls_wR_factor_ref         0.1216
_reflns_number_gt                19757
_reflns_number_total             27469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0604663si20060201_035932_2.cif
_cod_data_source_block           h03asw13
_cod_database_code               4110591