A Mechanistic Investigation of Oxidative Addition of Methyl Iodide to [Tp*Rh(CO)(L)]
Valérie Chauby; Jean-Claude Daran; Carole Serra-Le Berre; François Malbosc; Philippe Kalck; Oscar Delgado Gonzalez; Claire E. Haslam; Anthony Haynes; Inorganic Chemistry 41 (2002) 3280–3290; doi:10.1021/ic0255959

data_4318123
_publ_contact_author
;
Daran Jean-Claude
Laboratoire de Chimie de Coordination, CNRS UPR-8241
205, route de Narbonne
31077 Toulouse cedex
;
_publ_contact_author_email       ' daran@lcc-toulouse.fr '
_publ_contact_author_fax         ' (33) 05 61 55 30 03 '
_publ_contact_author_phone       ' (33) 05 61 33 31 74 '
_publ_section_title
;
 A Mechanistic Investigation of Oxidative Addition of Methyl Iodide to
 [Tp*Rh(CO)(L)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3280
_journal_page_last               3290
_journal_paper_doi               10.1021/ic0255959
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        ' synthesis as described'
_chemical_formula_moiety         ' C20 H34 Rh I P B N6 O '
_chemical_formula_sum            'C20 H34 B I N6 O P Rh'
_chemical_formula_weight         646.13
_chemical_name_systematic
;
  [(\h3-tris(3,5-dimethylpyrazolyl)borato)iodo(acetyl)
 (trimethylphosphine)rhodium(III)] 
;
_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
_cell_angle_alpha                93.18(2)
_cell_angle_beta                 97.25(2)
_cell_angle_gamma                93.92(2)
_cell_formula_units_Z            4
_cell_length_a                   11.556(3)
_cell_length_b                   14.144(3)
_cell_length_c                   15.684(3)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    293
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      1.8
_cell_volume                     2531.7(10)
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0528
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19955
_diffrn_reflns_theta_max         24.23
_diffrn_reflns_theta_min         1.78
_diffrn_standards_decay_%        0.00
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    1.95
_exptl_absorpt_correction_T_max  1.203
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.69
_exptl_crystal_description       box
_exptl_crystal_F_000             1280.37
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.06
_refine_diff_density_min         -3.21
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_obs   1.0677
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         5671
_refine_ls_R_factor_obs          0.0638
_refine_ls_shift/esd_max         0.144463
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.0630
_reflns_number_observed          5170
_reflns_number_total             7466
_reflns_observed_criterion       >3\s(I)
_cod_data_source_file            ic0255959_s1_1.cif
_cod_data_source_block           3a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2531.6(10)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        ' C20 H34 Rh I P B N6 O '
_cod_database_code               4318123