Direct transformation of 2-acetylpyridine oxime esters into α-oxygenated imines in an Ir( <scp>iii</scp> ) complex
Takahashi, Hiroyuki; Kodama, Shintaro; Ishii, Youichi; Dalton Transactions 46 (2017) 12032–12035; doi:10.1039/C7DT02528A

data_1546823
_publ_section_title
;
 Direct transformation of 2-acetylpyridine oxime esters into \a-oxygenated
 imines in an Ir( <scp>iii</scp> ) complex
;
_journal_issue                   36
_journal_name_full               'Dalton Transactions'
_journal_page_first              12032
_journal_page_last               12035
_journal_paper_doi               10.1039/C7DT02528A
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C19 H29 Cl2 Ir N2 O2'
_chemical_formula_sum            'C19 H29 Cl2 Ir N2 O2'
_chemical_formula_weight         580.58
_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_update_record
;
2017-07-12 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.3973(15)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   11.7603(11)
_cell_length_b                   12.1239(12)
_cell_length_c                   15.2286(15)
_cell_measurement_reflns_used    8138
_cell_measurement_temperature    93
_cell_measurement_theta_max      31.17
_cell_measurement_theta_min      3.36
_cell_volume                     2170.7(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.2.4'
_computing_publication_material  'CrystalStructure 4.2.4 (Rigaku, 2016)'
_computing_structure_refinement  'SHELXL Version 2016/6 (Sheldrick, 2008)'
_computing_structure_solution    'SIR2011 (Burla, et al., 2012)'
_diffrn_ambient_temperature      93
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0330
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17299
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.492
_diffrn_reflns_theta_min         3.361
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.429
_exptl_absorpt_correction_T_max  0.564
_exptl_absorpt_correction_T_min  0.362
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Rigaku, 1999)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.776
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136.00
_exptl_crystal_size_max          0.186
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.089
_refine_diff_density_max         0.76
_refine_diff_density_min         -2.15
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     347
_refine_ls_number_reflns         4889
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0253
_refine_ls_shift/su_max          0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0622
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4076
_reflns_number_total             4889
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            c7dt02528a2.cif
_cod_data_source_block           Compound_4Cl
_cod_database_code               1546823
_shelx_res_checksum              61087