Oxygen atom transfer to a half-sandwich iridium complex: clean oxidation yielding a molecular product.
Turlington, Christopher R.; White, Peter S.; Brookhart, Maurice; Templeton, Joseph L.; Journal of the American Chemical Society 136 (2014) 3981–3994; doi:10.1021/ja413023f

data_4121406
_publ_section_title
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 Oxygen atom transfer to a half-sandwich iridium complex: clean oxidation
 yielding a molecular product.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3981
_journal_page_last               3994
_journal_paper_doi               10.1021/ja413023f
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'C30 H27 Cl F6 Ir N2 O, C32 H12 B F24'
_chemical_formula_sum            'C62 H39 B Cl F30 Ir N2 O'
_chemical_formula_weight         1636.41
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_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     iterative
_audit_creation_date             2013-04-01
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Mar 21 2013 11:17:50, GUI svn.r4446)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.1810(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1858(3)
_cell_length_b                   20.1500(5)
_cell_length_c                   24.1403(6)
_cell_measurement_reflns_used    9923
_cell_measurement_temperature    100
_cell_measurement_theta_max      70.09
_cell_measurement_theta_min      3.72
_cell_volume                     6312.9(3)
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_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
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.0407
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            64683
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         1.86
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.694
_exptl_absorpt_correction_T_max  0.6256
_exptl_absorpt_correction_T_min  0.3732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0580 before and 0.0483 after correction.
The Ratio of minimum to maximum transmission is 0.5965.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_description       block
_exptl_crystal_F_000             3208
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.080
_refine_diff_density_min         -0.509
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     999
_refine_ls_number_reflns         11930
_refine_ls_number_restraints     240
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+9.4980P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0695
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10714
_reflns_number_total             11930
_reflns_threshold_expression     'I > 2\s(I)'
_cod_duplicate_entry             4121405
_cod_data_source_file            ja413023f_si_002.cif
_cod_data_source_block           x1303020
_cod_database_code               4121406
_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, All O(H) groups
2. Uiso/Uaniso restraints and constraints
C46 \\sim F16 \\sim F16A \\sim F17 \\sim F17A \\sim F18 \\sim F18A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
C53 \\sim F19A \\sim F19 \\sim F20 \\sim F20A \\sim F21 \\sim F21A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
F26 \\sim F26A \\sim F27 \\sim F27A \\sim F25 \\sim F25A \\sim C61: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
C62 \\sim F28 \\sim F28A \\sim F30 \\sim F30A \\sim F29 \\sim F29A: within 1.7A with sigma of 0.005 and sigma for terminal atoms of 0.005
3. Others
 Sof(F16)=1-Sof(F16A)=Sof(F17)=1-Sof(F16A)=Sof(F18)=1-Sof(F16A)
 Sof(F28)=1-Sof(F28A)=Sof(F29)=1-Sof(F28A)=Sof(F30)=1-Sof(F28A)
 Fixed Sof: F19(0.5) F19A(0.5) F20(0.5) F20A(0.5) F21(0.5) F21A(0.5) F25(0.5)
 F25A(0.5) F26(0.5) F26A(0.5) F27(0.5) F27A(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C14(H14),
 C16(H16), C18(H18), C32(H32), C34(H34), C36(H36), C40(H40), C42(H42), C44(H44),
  C48(H48), C50(H50), C52(H52), C56(H56), C58(H58), C60(H60)
4.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C30(H30A,H30B,H30C)
4.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_hkl_checksum              72484
_shelx_res_checksum              91863
_shelxl_version_number           2013-2