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_4105186
_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         'C30 H58 F2 P2 Rh, C32 H12 B F24'
_chemical_formula_sum            'C62 H70 B F26 P2 Rh'
_chemical_formula_weight         1484.84
_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                 113.7594(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.7964(2)
_cell_length_b                   13.1712(2)
_cell_length_c                   25.5387(3)
_cell_measurement_reflns_used    15227
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      5.097
_cell_volume                     6710.37(15)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            25291
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         5.10
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Denzo/Scalepack (Otwinowski & Minor 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       block
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.089
_refine_diff_density_min         -0.958
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1207
_refine_ls_number_reflns         13607
_refine_ls_number_restraints     1596
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0906
_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^)+(0.1605P)^2^+20.5330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2499
_refine_ls_wR_factor_ref         0.2825
_reflns_number_gt                9106
_reflns_number_total             13607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja906070r_si_002.cif
_cod_data_source_block           2
_cod_original_cell_volume        6710.37(14)
_cod_database_code               4105186