Stereochemical Nonrigidity of a Chiral Rhodium Boryl Hydride Complex: A σ-Borane Complex as Transition State for Isomerization
Marius V. Câmpian; Eric Clot; Odile Eisenstein; Ulrike Helmstedt; Naseralla Jasim; Robin N. Perutz; Adrian C. Whitwood; David Williamson; Journal of the American Chemical Society 130 (2008) 4375–4385; doi:10.1021/ja077357o

data_4107614
_publ_contact_author_address
;Department of Chemistry,
University of York,
Heslington,
York YO10 5DD
UK
;
_publ_contact_author_email       rnp1@york.ac.uk
_publ_contact_author_fax         '+44 1904 432516'
_publ_contact_author_name        'Prof Robin N Perutz'
_publ_contact_author_phone       '+44 1904 432549'
_publ_section_title
;
 Stereochemical Nonrigidity of a Chiral Rhodium Boryl Hydride Complex: A
 \s-Borane Complex as Transition State for Isomerization
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4375
_journal_page_last               4385
_journal_paper_doi               10.1021/ja077357o
_journal_volume                  130
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C17 H22 Br2 P Rh'
_chemical_formula_sum            'C17 H22 Br2 P Rh'
_chemical_formula_weight         520.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   9.817(4)
_cell_length_b                   12.992(5)
_cell_length_c                   14.271(5)
_cell_measurement_reflns_used    8057
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      30.01
_cell_measurement_theta_min      2.52
_cell_volume                     1820.2(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25782
_diffrn_reflns_theta_full        30.10
_diffrn_reflns_theta_max         30.10
_diffrn_reflns_theta_min         2.12
_exptl_absorpt_coefficient_mu    5.409
_exptl_absorpt_correction_T_max  0.620
_exptl_absorpt_correction_T_min  0.407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2.03; (Sheldrick)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_description       plate
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.434
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.047(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         5289
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0243
_refine_ls_R_factor_gt           0.0225
_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^)+(0.0263P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0511
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                5011
_reflns_number_total             5289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077357o-file004.cif
_cod_data_source_block           rnp0607m
_cod_original_cell_volume        1820.0(12)
_cod_database_code               4107614