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_4120182
_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         'C33 H55 I N2 P2 Rh, C H2 Cl2, B F4'
_chemical_formula_sum            'C34 H57 B Cl2 F4 I N2 P2 Rh'
_chemical_formula_weight         943.28
_chemical_name_systematic
; 
 ? 
;
_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                 91.4252(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3722(2)
_cell_length_b                   21.6932(3)
_cell_length_c                   13.9191(3)
_cell_measurement_reflns_used    9332
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.70
_cell_measurement_theta_min      2.55
_cell_volume                     4036.48(12)
_computing_cell_refinement       HKL
_computing_data_collection       'Collect package (Bruker Nonius)'
_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      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Nonius 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  0.0610
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10363
_diffrn_reflns_theta_full        28.70
_diffrn_reflns_theta_max         28.70
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.444
_exptl_absorpt_correction_T_max  0.8691
_exptl_absorpt_correction_T_min  0.5958
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       plate
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.702
_refine_diff_density_min         -0.794
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         10363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+3.7971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0869
_refine_ls_wR_factor_ref         0.0952
_reflns_number_gt                7666
_reflns_number_total             10363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401852c_si_002_4.cif
_cod_data_source_block           m902a
_cod_original_sg_symbol_Hall     -P2yn
_cod_database_code               4120182