Amine-Borane σ-Complexes of Rhodium. Relevance to the Catalytic Dehydrogenation of Amine-Boranes
Thomas M. Douglas; Adrian B. Chaplin; Andrew S. Weller; Journal of the American Chemical Society 130 (2008) 14432–14433; doi:10.1021/ja806582n

data_4108616
_publ_section_title
;
 Amine-Borane \s-Complexes of Rhodium. Relevance to the Catalytic
 Dehydrogenation of Amine-Boranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14432
_journal_page_last               14433
_journal_paper_doi               10.1021/ja806582n
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C27 H66 B N P2 Rh, C32 H12 B F24 '
_chemical_formula_sum            'C59 H78 B2 F24 N P2 Rh'
_chemical_formula_weight         1443.69
_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                 93.4556(0)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.97140(10)
_cell_length_b                   20.0178(2)
_cell_length_c                   26.8437(2)
_cell_measurement_reflns_used    15765
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     6957.53(10)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2004 (Burla et al., 2005)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_sigmaI/netI    0.0278
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            23229
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.672
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         12157
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0655
_refine_ls_R_factor_gt           0.0542
_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^)+(0.0708P)^2^+15.0829P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1387
_refine_ls_wR_factor_ref         0.1484
_reflns_number_gt                10212
_reflns_number_total             12157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806582n_si_001_1.cif
_cod_data_source_block           2-Me
_cod_database_code               4108616