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_4108618
_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         'C28 H70 B2 N2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C60 H82 B3 F24 N2 P2 Rh'
_chemical_formula_weight         1484.56
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/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                 91.5253(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.2225(2)
_cell_length_b                   50.9939(7)
_cell_length_c                   19.5840(3)
_cell_measurement_reflns_used    27645
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      5.12
_cell_volume                     14198.5(4)
_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 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.075
_diffrn_reflns_av_sigmaI/netI    0.0775
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       60
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            22815
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         5.12
_exptl_absorpt_coefficient_mu    0.386
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.648
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             6096
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.373
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1997
_refine_ls_number_reflns         22815
_refine_ls_number_restraints     470
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.1179
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0143P)^2^+53.8819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1284
_refine_ls_wR_factor_ref         0.1528
_reflns_number_gt                15661
_reflns_number_total             22815
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja806582n_si_001_3.cif
_cod_data_source_block           5
_cod_database_code               4108618