Exploring Oxidation of Half-Sandwich Rhodium Complexes: Oxygen Atom Insertion into the Rhodium‒Carbon Bond of κ2-Coordinated 2-Phenylpyridine
Turlington, Christopher R.; Morris, James; White, Peter S.; Brennessel, William W.; Jones, William D.; Brookhart, Maurice; Templeton, Joseph L.; Organometallics 33 (2014) 4442–; doi:10.1021/om500660n

data_4084320
_publ_section_title
;
 Exploring Oxidation of Half-Sandwich Rhodium Complexes: Oxygen Atom
 Insertion into the Rhodium--Carbon Bond of \k2-Coordinated
 2-Phenylpyridine
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4442
_journal_paper_doi               10.1021/om500660n
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C42 H46 N2 O2 Rh2, 2(C F3 O3 S)'
_chemical_formula_sum            'C44 H46 F6 N2 O8 Rh2 S2'
_chemical_formula_weight         1114.77
_chemical_name_common            jonjcm27
_chemical_name_systematic
; 
 {[Cp*Rh(O-PhPy)]2}2+ [CF3SO3]2-
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.647(4)
_cell_angle_beta                 115.317(4)
_cell_angle_gamma                91.827(4)
_cell_formula_units_Z            1
_cell_length_a                   9.925(3)
_cell_length_b                   10.598(3)
_cell_length_c                   11.517(3)
_cell_measurement_reflns_used    2476
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      22.38
_cell_measurement_theta_min      2.27
_cell_volume                     1093.3(5)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2010)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100.0(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD Platform'
_diffrn_measurement_method       'area detector, \w scans per \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  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0870
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14736
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.92
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.9637
_exptl_absorpt_correction_T_min  0.8502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.693
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             564
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.334
_refine_diff_density_min         -1.131
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3865
_refine_ls_number_restraints     82
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1053
_refine_ls_R_factor_gt           0.0683
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1708
_refine_ls_wR_factor_ref         0.2002
_reflns_number_gt                2650
_reflns_number_total             3865
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500660n_si_002.cif
_cod_data_source_block           3-OTf
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084320