Thermodynamic Studies and Hydride Transfer Reactions from a Rhodium Complex to BX3 Compounds
Michael T. Mock; Robert G. Potter; Donald M. Camaioni; Jun Li; William G. Dougherty; W. Scott Kassel; Brendan Twamley; Daniel L. DuBois; Journal of the American Chemical Society 131 (2009) 14454–14465; doi:10.1021/ja905287q

data_4105108
_publ_section_title
;
 Thermodynamic Studies and Hydride Transfer Reactions from a Rhodium
 Complex to BX3 Compounds
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14454
_journal_page_last               14465
_journal_paper_doi               10.1021/ja905287q
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C18 H15 B S3'
_chemical_formula_weight         338.29
_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                 94.553(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.8212(8)
_cell_length_b                   24.359(3)
_cell_length_c                   11.9665(16)
_cell_measurement_reflns_used    4380
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      32.89
_cell_measurement_theta_min      3.52
_cell_volume                     1691.5(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0756
_diffrn_reflns_av_sigmaI/netI    0.1020
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19016
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         33.18
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9851
_exptl_absorpt_correction_T_min  0.9049
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.328
_exptl_crystal_description       needle
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         6406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.1187
_refine_ls_R_factor_gt           0.0478
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0796
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3605
_reflns_number_total             6406
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905287q_si_005.cif
_cod_data_source_block           pnl033
_cod_database_code               4105108