Probing the Oxidation Chemistry of Half-Sandwich Iridium Complexes with Oxygen Atom Transfer Reagents
Christopher R. Turlington; Daniel P. Harrison; Peter S. White; Maurice Brookhart; Joseph L. Templeton; Inorganic Chemistry 52 (2013) 11351–11360; doi:10.1021/ic4016405

data_4336249
_publ_contact_author_name
;
;
_publ_section_title
;
 Probing the Oxidation Chemistry of Half-Sandwich Iridium Complexes with
 Oxygen Atom Transfer Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11351
_journal_page_last               11360
_journal_paper_doi               10.1021/ic4016405
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C21 H25 Ir N O, C F3 O3 S'
_chemical_formula_sum            'C22 H25 F3 Ir N O4 S'
_chemical_formula_weight         648.69
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-12
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 107.4690(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.1914(4)
_cell_length_b                   12.4570(3)
_cell_length_c                   11.5310(3)
_cell_measurement_reflns_used    9386
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.33
_cell_measurement_theta_min      2.86
_cell_volume                     2218.49(10)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            20785
_diffrn_reflns_theta_full        69.72
_diffrn_reflns_theta_max         69.72
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.026
_exptl_absorpt_correction_T_max  0.3706
_exptl_absorpt_correction_T_min  0.1687
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
R(int) was 0.0731 before and 0.0449 after correction.
The Ratio of minimum to maximum transmission is 0.4552.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.942
_exptl_crystal_F_000             1264
_exptl_crystal_recrystallization_method
;
crystallized by layering pentanes over a concentrated solution in methylene 
chloride at room temperature
;
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.239
_exptl_crystal_size_min          0.157
_refine_diff_density_max         2.127
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4103
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0358
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0407P)^2^+5.2380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0787
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                3621
_reflns_number_total             4103
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic4016405_si_002.cif
_cod_data_source_block           crt211try2
_cod_database_code               4336249
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C21(H21), C22(H22), C23(H23), C24(H24), C26(H26), C27(H27), C30(H30)
2.b Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C25(H25A,H25B,H25C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C)
;