Monomeric and Oligomeric Amine-Borane σ-Complexes of Rhodium. Intermediates in the Catalytic Dehydrogenation of Amine-Boranes
Thomas M. Douglas; Adrian B. Chaplin; Andrew S. Weller; Xinzheng Yang; Michael B. Hall; Journal of the American Chemical Society 131 (2009) 15440–15456; doi:10.1021/ja906070r

data_4105187
_publ_section_title
;
 Monomeric and Oligomeric Amine-Borane \s-Complexes of Rhodium.
 Intermediates in the Catalytic Dehydrogenation of Amine-Boranes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15440
_journal_page_last               15456
_journal_paper_doi               10.1021/ja906070r
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C28 H72 B2 N2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C60 H84 B3 F24 N2 P2 Rh'
_chemical_formula_weight         1486.57
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n 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            8
_cell_length_a                   50.6131(4)
_cell_length_b                   19.6787(2)
_cell_length_c                   14.39940(10)
_cell_measurement_reflns_used    10102
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     14341.8(2)
_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 0.884
_diffrn_measured_fraction_theta_max 0.883
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0413
_diffrn_reflns_limit_h_max       57
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19425
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    0.382
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.569
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             6112
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.989
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881; 7742 Friedel pairs'
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2004
_refine_ls_number_reflns         19425
_refine_ls_number_restraints     1564
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0718
_refine_ls_R_factor_gt           0.0563
_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^)+(0.0790P)^2^+21.1475P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                16731
_reflns_number_total             19425
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906070r_si_003.cif
_cod_data_source_block           10
_cod_database_code               4105187