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_4121404
_publ_section_title
;
 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
'C32 H12 B F24, 0.5(C42 H46 Ir2 N2 O2), C H2 Cl2'
_chemical_formula_sum            'C54 H37 B Cl2 F24 Ir N O'
_chemical_formula_weight         1445.76
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-18
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                106.1770(10)
_cell_angle_beta                 110.3230(10)
_cell_angle_gamma                98.0160(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8140(2)
_cell_length_b                   13.7210(2)
_cell_length_c                   18.1145(3)
_cell_measurement_reflns_used    9945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.12
_cell_measurement_theta_min      3.61
_cell_volume                     2767.98(8)
_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
;
XL, 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      100.15
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0210
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39637
_diffrn_reflns_theta_full        70.11
_diffrn_reflns_theta_max         70.11
_diffrn_reflns_theta_min         2.78
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.664
_exptl_absorpt_correction_T_max  0.5418
_exptl_absorpt_correction_T_min  0.2030
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0502 before and 0.0298 after correction.
The Ratio of minimum to maximum transmission is 0.3747.
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    1.735
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.261
_exptl_crystal_size_min          0.168
_refine_diff_density_max         1.286
_refine_diff_density_min         -0.955
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     789
_refine_ls_number_reflns         10164
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0287P)^2^+4.7985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0598
_reflns_number_gt                10003
_reflns_number_total             10164
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja413023f_si_002.cif
_cod_data_source_block           x1301004
_cod_original_cell_volume        2767.97(7)
_cod_database_code               4121404
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H10 of C10, H9 of C9, H8 of C8, H5 of C5, H4 of C4, H3 of C3, H2 of C2, H43
  of C43, H35 of C35, H31 of C31, H41 of C41, H33 of C33, H39 of C39, H25 of
  C25, H27 of C27, H23 of C23, {H54A,H54B} of C54, H47 of C47, H49 of C49, H51
  of C51, H11 of C11
 At 1.5 times of:
  {H21A,H21B,H21C} of C21, {H20A,H20B,H20C} of C20, {H19A,H19B,H19C} of C19,
  {H17A,H17B,H17C} of C17, {H18A,H18B,H18C} of C18
2. Uiso/Uaniso restraints and constraints
C53 ~ F22 ~ F23 ~ F24 ~ F25 ~ F26 ~ F27: within 1.7A with sigma of 0.002 and sigma for terminal atoms of 0.005
3. Others
 Fixed Sof: F22(0.5) F23(0.5) F24(0.5) F25(0.5) F26(0.5) F27(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B)
4.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C23(H23),
 C25(H25), C27(H27), C31(H31), C33(H33), C35(H35), C39(H39), C41(H41), C43(H43),
  C47(H47), C49(H49), C51(H51)
4.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C)
;