Direct Observation of Reductive Elimination of MeX (X = Cl, Br, I) from RhIII Complexes: Mechanistic Insight and the Importance of Sterics
Moran Feller; Yael Diskin-Posner; Gregory Leitus; Linda J. W. Shimon; David Milstein; Journal of the American Chemical Society 135 (2013) 11040–11047; doi:10.1021/ja401852c

data_4120185
_publ_section_title
;
 Direct Observation of Reductive Elimination of MeX (X = Cl, Br, I) from
 RhIII Complexes: Mechanistic Insight and the Importance of Sterics
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11040
_journal_page_last               11047
_journal_paper_doi               10.1021/ja401852c
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C20 H38 Cl N P2 Rh, B F4'
_chemical_formula_sum            'C20 H38 B Cl F4 N P2 Rh'
_chemical_formula_weight         579.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 106.398(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.7456(3)
_cell_length_b                   29.8765(10)
_cell_length_c                   11.2637(4)
_cell_measurement_reflns_used    114573
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.8515
_cell_measurement_theta_min      2.326
_cell_volume                     2500.52(16)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package Bruker'
_computing_data_reduction        HKL
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II KappaCCD'
_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  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            114366
_diffrn_reflns_theta_full        34.91
_diffrn_reflns_theta_max         34.91
_diffrn_reflns_theta_min         2.33
_exptl_absorpt_coefficient_mu    0.956
_exptl_absorpt_correction_T_max  0.9105
_exptl_absorpt_correction_T_min  0.7625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SHELXTL'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       prism
_exptl_crystal_F_000             1192
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.403
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.084
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 10700 Friedel pairs'
_refine_ls_abs_structure_Flack   0.039(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         21805
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0339P)^2^+0.8777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0640
_refine_ls_wR_factor_ref         0.0650
_reflns_number_gt                20649
_reflns_number_total             21805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401852c_si_002_7.cif
_cod_data_source_block           m933
_cod_original_sg_symbol_Hall     P2yb
_cod_database_code               4120185