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_4120183
_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 I N P2 Rh, B F4'
_chemical_formula_sum            'C20 H38 B F4 I N P2 Rh'
_chemical_formula_weight         671.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.5844(10)
_cell_angle_beta                 87.4471(12)
_cell_angle_gamma                74.2329(11)
_cell_formula_units_Z            4
_cell_length_a                   7.8269(2)
_cell_length_b                   11.2717(3)
_cell_length_c                   30.4115(8)
_cell_measurement_reflns_used    59103
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.55
_cell_volume                     2578.21(12)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package Bruker-Nonius'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_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  0.065
_diffrn_reflns_av_sigmaI/netI    0.0488
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11165
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    2.021
_exptl_absorpt_correction_T_max  0.8715
_exptl_absorpt_correction_T_min  0.6320
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            'Orange Red'
_exptl_crystal_density_diffrn    1.729
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.848
_refine_diff_density_min         -1.534
_refine_diff_density_rms         0.214
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.329
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9424
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.329
_refine_ls_R_factor_all          0.0772
_refine_ls_R_factor_gt           0.0670
_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^)+(0.0000P)^2^+43.7603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1440
_reflns_number_gt                8523
_reflns_number_total             9424
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401852c_si_002_5.cif
_cod_data_source_block           m789a
_cod_original_sg_symbol_Hall     -P1
_cod_database_code               4120183