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_4120187
_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 I2 N P2 Rh'
_chemical_formula_sum            'C20 H38 I2 N P2 Rh'
_chemical_formula_weight         711.16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 113.6717(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.1006(3)
_cell_length_b                   11.7405(3)
_cell_length_c                   16.5928(3)
_cell_measurement_reflns_used    6544
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      1.00
_cell_volume                     2515.78(10)
_computing_cell_refinement       HKL
_computing_data_collection       'collect package Nonius'
_computing_data_reduction        HKL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altmore et al, 1994)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega and phi 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  0.1600
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            44019
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    3.266
_exptl_absorpt_correction_T_max  0.852
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
gaussian integration (Coppens, 1970)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.878
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.864
_refine_diff_density_min         -2.432
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         5535
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0919P)^2^+4.7777P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1411
_refine_ls_wR_factor_ref         0.1544
_reflns_number_gt                4371
_reflns_number_total             5535
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja401852c_si_002_9.cif
_cod_data_source_block           m1396
_cod_original_sg_symbol_Hall     -P2ybc
_cod_database_code               4120187