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_4084319
_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
'C31 H36 I N O4 Rh S, C H2 Cl2, C32 H12 B F24'
_chemical_formula_sum            'C64 H50 B Cl2 F24 I N O4 Rh S'
_chemical_formula_weight         1696.63
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_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     iterative
_audit_creation_date             2014-01-24
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.4368(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.5769(4)
_cell_length_b                   25.1329(8)
_cell_length_c                   19.3985(5)
_cell_measurement_reflns_used    9639
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.17
_cell_measurement_theta_min      3.04
_cell_volume                     6967.8(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2013)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0539
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55603
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.167
_diffrn_reflns_theta_min         3.042
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.441
_exptl_absorpt_correction_T_max  0.7570
_exptl_absorpt_correction_T_min  0.2738
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0735 before and 0.0538 after correction.
The Ratio of minimum to maximum transmission is 0.3617.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       plate
_exptl_crystal_F_000             3368
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.169
_exptl_crystal_size_min          0.068
_refine_diff_density_max         1.389
_refine_diff_density_min         -1.493
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         12977
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+12.1186P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10241
_reflns_number_total             12977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om500660n_si_002.cif
_cod_data_source_block           Compound2
_cod_database_code               4084319
_shelxl_version_number           2013-2
_shelx_estimated_absorpt_t_max   0.632
_shelx_estimated_absorpt_t_min   0.175
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 F21A, F19A, F20A, F19, F21, F20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F22A, F23A, F24A, C63, F23, F24, F22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
3. Others
 Fixed Sof: F19(0.5) F19A(0.5) F20(0.5) F20A(0.5) F21(0.5) F21A(0.5) F22(0.5)
 F22A(0.5) F23(0.5) F23A(0.5) F24(0.5) F24A(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C12(H12), C13(H13), C14(H14), C15(H15),
 C18(H18), C19(H19), C20(H20), C21(H21), C33(H33), C35(H35), C37(H37), C41(H41),
  C43(H43), C45(H45), C49(H49), C51(H51), C53(H53), C57(H57), C59(H59), C61(H61)
4.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C)
;
_shelx_res_checksum              65662
_shelx_hkl_checksum              23341