CO-Induced Methyl Migration in a Rhodium Thiophosphoryl Pincer Complex and Its Comparison with Phosphine-Based Complexes: The Divergent Effects of S and P Donor Ligands
Montag, Michael; Efremenko, Irena; Leitus, Gregory; Ben-David, Yehoshoa; Martin, Jan M. L.; Milstein, David; Organometallics 32 (2013) 7163–; doi:10.1021/om4008696

data_4081990
_publ_section_title
;
 CO-Induced Methyl Migration in a Rhodium Thiophosphoryl Pincer Complex
 and Its Comparison with Phosphine-Based Complexes: The Divergent Effects
 of S and P Donor Ligands
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              7163
_journal_paper_doi               10.1021/om4008696
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C38 H68 I2 P4 Rh2 S4'
_chemical_formula_sum            'C38 H68 I2 P4 Rh2 S4'
_chemical_formula_weight         1236.66
_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                 96.54(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.701(2)
_cell_length_b                   16.033(3)
_cell_length_c                   12.540(3)
_cell_measurement_reflns_used    27839
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.0
_cell_volume                     2337.2(8)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0321
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5327
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.6487
_exptl_absorpt_correction_T_min  0.3838
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Bruker SHELXTL'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.177
_refine_diff_density_min         -1.110
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5327
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0405
_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^)+(0.0637P)^2^+4.5601P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1018
_refine_ls_wR_factor_ref         0.1094
_reflns_number_gt                4248
_reflns_number_total             5327
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4008696_si_002.cif
_cod_data_source_block           Complex_8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4081990