Revisiting the iridacycle-catalyzed hydrosilylation of enolizable imines
Pèrez-Miqueo, Jorge; San Nacianceno, Virginia; Urquiola, F. Borja; Freixa, Zoraida; Catalysis Science & Technology 8 (2018) 6316–; doi:10.1039/C8CY01236A

data_1549858
_publ_section_title
;
 Revisiting the iridacycle-catalyzed hydrosilylation of enolizable imines
;
_journal_issue                   24
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6316
_journal_paper_doi               10.1039/C8CY01236A
_journal_volume                  8
_journal_year                    2018
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C23 H26 Ir1 N1 O3'
_chemical_formula_sum            'C23 H26 Ir N O3'
_chemical_formula_weight         556.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      61
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-04-26T14:43:17-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-06-15 deposited with the CCDC.
2018-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.13031(15)
_cell_length_b                   14.54437(12)
_cell_length_c                   17.33703(17)
_cell_measurement_reflns_used    20060
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.375
_cell_measurement_theta_min      4.789
_cell_measurement_wavelength     1.54184
_cell_volume                     4067.36(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2012
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     29.00  96.00   1.00    2.00    --   40.83-125.00-180.00   67
  2  \w     33.00  92.00   1.00    2.00    --   40.83  77.00  90.00   59
  3  \w      6.00  48.00   1.00    2.00    --   40.83-132.00  63.00   42
  4  \w    105.00 147.00   1.00    8.00    --  113.00  30.00  60.00   42
  5  \w     36.00  66.00   1.00    8.00    --  113.00 -30.00  30.00   30
  6  \w     38.00  63.00   1.00    8.00    --  113.00 -45.00 120.00   25
  7  \w    117.00 154.00   1.00    8.00    --  113.00 137.00 -49.00   37
  8  \w     47.00  73.00   1.00    8.00    --  113.00 -45.00   0.00   26
  9  \w    133.00 158.00   1.00    8.00    --  113.00  61.00-120.00   25
 10  \w     41.00  74.00   1.00    8.00    --  113.00 -45.00 -30.00   33
 11  \w     79.00 155.00   1.00    8.00    --  113.00  77.00 150.00   76
 12  \w     35.00  65.00   1.00    8.00    --  113.00 -30.00  60.00   30
 13  \w     35.00  65.00   1.00    8.00    --  113.00 -30.00  90.00   30
 14  \w   -111.00 -12.00   1.00    2.00    --  -40.83 -77.00-120.00   99
 15  \w     79.00 117.00   1.00    2.00    --   40.83  37.00 120.00   38
 16  \w    -33.00  74.00   1.00    2.00    --   40.83 -77.00 -30.00  107
 17  \w     27.00  54.00   1.00    2.00    --   40.83  37.00 120.00   27
 18  \w    -68.00 -40.00   1.00    8.00    --  -83.00  30.00 150.00   28
 19  \w    -57.00  -5.00   1.00    8.00    --  -83.00  30.00-120.00   52
 20  \w     63.00 109.00   1.00    8.00    --  113.00 -94.00   0.00   46
 21  \w     35.00  69.00   1.00    8.00    --  113.00 -30.00-120.00   34
 22  \w     55.00 112.00   1.00    8.00    --  113.00-111.00 -90.00   57
 23  \w     33.00  96.00   1.00    8.00    --  113.00 -15.00-120.00   63
 24  \w     35.00  69.00   1.00    8.00    --  113.00 -30.00-180.00   34
 25  \w     87.00 114.00   1.00    8.00    --  113.00  30.00 150.00   27
 26  \w     35.00  68.00   1.00    8.00    --  113.00 -30.00-150.00   33
 27  \w     56.00  83.00   1.00    8.00    --  113.00 -94.00  60.00   27
 28  \w     43.00 102.00   1.00    8.00    --  113.00 -94.00 150.00   59
 29  \w     86.00 112.00   1.00    8.00    --  113.00-111.00 -30.00   26
 30  \w     59.00 108.00   1.00    8.00    --  113.00-111.00-120.00   49
 31  \w     35.00  69.00   1.00    8.00    --  113.00 -30.00 150.00   34
 32  \w     53.00 116.00   1.00    8.00    --  113.00-111.00 120.00   63
 33  \w    111.00 149.00   1.00    8.00    --  113.00 -15.00-120.00   38
 34  \w     49.00 137.00   1.00    8.00    --  113.00 -61.00-120.00   88
;
_diffrn_measurement_device       'four-circle\k-geometry diffractometer'
_diffrn_measurement_device_type  'Agilent SuperNova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0149789
_diffrn_orient_matrix_UB_12      0.066876
_diffrn_orient_matrix_UB_13      -0.0675372
_diffrn_orient_matrix_UB_21      0.094303
_diffrn_orient_matrix_UB_22      0.0086692
_diffrn_orient_matrix_UB_23      -0.0121277
_diffrn_orient_matrix_UB_31      -0.0022692
_diffrn_orient_matrix_UB_32      -0.0816203
_diffrn_orient_matrix_UB_33      -0.0565145
_diffrn_radiation_monochromator  'Multilayer optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            33175
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         69.999
_diffrn_reflns_theta_min         4.824
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_current           0.8
_diffrn_source_power             0.04
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    12.917
_exptl_absorpt_correction_T_max  0.648
_exptl_absorpt_correction_T_min  0.267
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.758
_refine_diff_density_min         -0.64
_refine_diff_density_rms         0.08
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         3856
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0263P)^2^+3.2166P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0437
_refine_ls_wR_factor_ref         0.045
_reflns_number_gt                3570
_reflns_number_total             3856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cy01236a2.cif
_cod_data_source_block           compound6
_cod_depositor_comments          'Adding full bibliography for 1549858.cif.'
_cod_original_cell_volume        4067.35(6)
_cod_database_code               1549858