Oxyfunctionalization with Cp*IrIII(NHC)(Me)L Complexes
Lehman, Matthew C.; Boyle, Paul D.; Sommer, Roger D.; Ison, Elon A.; Organometallics 33 (2014) 5081–; doi:10.1021/om5007352

data_4084732
_publ_section_title
;
 Oxyfunctionalization with Cp*IrIII(NHC)(Me)L Complexes
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5081
_journal_paper_doi               10.1021/om5007352
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C21.5 H29 Cl2 F3 Ir N3 O3 S'
_chemical_formula_weight         729.64
_chemical_name_common            'ML 1405'
_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     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                75.660(2)
_cell_angle_beta                 87.416(2)
_cell_angle_gamma                87.231(2)
_cell_formula_units_Z            2
_cell_length_a                   8.6215(3)
_cell_length_b                   12.0541(4)
_cell_length_c                   12.7969(4)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      35.8014
_cell_measurement_theta_min      2.3665
_cell_volume                     1286.22(7)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection       'Bruker Instrument Service v2012.12.0.3'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS Inc., 2009)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0363
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            40354
_diffrn_reflns_theta_full        36.56
_diffrn_reflns_theta_max         36.56
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    5.530
_exptl_absorpt_correction_T_max  0.70
_exptl_absorpt_correction_T_min  0.47
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.318
_refine_diff_density_min         -1.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         12586
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0240
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[\s^2^(Fo^2^)+(0.0268P)^2^]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0510
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                11507
_reflns_number_total             12586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5007352_si_001.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C21.50 H29 Cl2 F3 Ir N3 O3 S'
_cod_database_code               4084732
_shelx_res_checksum              7008
_shelx_hkl_checksum              92686