Exclusive C‒C Oxidative Addition in a Rhodium Thiophosphoryl Pincer Complex and Computational Evidence for an η3-C‒C‒H Agostic Intermediate
Montag, Michael; Efremenko, Irena; Diskin-Posner, Yael; Ben-David, Yehoshoa; Martin, Jan M. L.; Milstein, David; Organometallics 31 (2012) 505–; doi:10.1021/om201205y

data_4068201
_publ_section_title
;
 Exclusive C--C Oxidative Addition in a Rhodium Thiophosphoryl Pincer
 Complex and Computational Evidence for an \h3-C--C--H Agostic
 Intermediate
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              505
_journal_paper_doi               10.1021/om201205y
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C25 H46 O2 P2 Rh S2, B F4'
_chemical_formula_sum            'C25 H46 B F4 O2 P2 Rh S2'
_chemical_formula_weight         694.40
_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                 101.268(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.8444(6)
_cell_length_b                   21.2018(14)
_cell_length_c                   17.7823(12)
_cell_measurement_reflns_used    38485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.597
_cell_measurement_theta_min      2.5255
_cell_volume                     3270.2(4)
_computing_cell_refinement       APEX2
_computing_data_collection       APEX2
_computing_data_reduction        APEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker kappaAPEXII 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  0.0362
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37814
_diffrn_reflns_theta_full        30.63
_diffrn_reflns_theta_max         30.63
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.791
_exptl_absorpt_correction_T_max  0.9394
_exptl_absorpt_correction_T_min  0.9110
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SHELXL-97 (Sheldrick, 1997)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.493
_refine_diff_density_min         -0.951
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         10079
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0389
_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^)+(0.0422P)^2^+2.9547P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0972
_reflns_number_gt                8013
_reflns_number_total             10079
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201205y_si_002.cif
_cod_data_source_block           m920a
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     -P2ybc
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               4068201