Highly Active Cp*Ir Catalyst at Low Temperatures Bearing an N-Heterocyclic Carbene Ligand and a Chelated Primary Benzylamine in Transfer Hydrogenation
Sabater, Sara; Baya, Miguel; Mata, Jose A.; Organometallics 33 (2014) 6830–; doi:10.1021/om500888d

data_4084856
_publ_section_title
;
 Highly Active Cp*Ir Catalyst at Low Temperatures Bearing an
 N-Heterocyclic Carbene Ligand and a Chelated Primary Benzylamine in
 Transfer Hydrogenation
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6830
_journal_paper_doi               10.1021/om500888d
_journal_volume                  33
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C27 H35 Ir N3, F6 P, C H2 Cl2'
_chemical_formula_sum            'C28 H37 Cl2 F6 Ir N3 P'
_chemical_formula_weight         823.68
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-03-25
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9558(3)
_cell_length_b                   15.5372(3)
_cell_length_c                   18.1992(5)
_cell_measurement_reflns_used    10361
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      28.9590
_cell_measurement_theta_min      3.5640
_cell_volume                     3380.68(14)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200.00(10)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.8674
_diffrn_measurement_details
;
  1 omega  -14.00   29.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000 -180.0000 43

  2 omega   16.00   64.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   37.0000   30.0000 48

  3 omega  -51.00  -26.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -37.0000   30.0000 25

  4 omega    8.00   67.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   77.0000  -90.0000 59

  5 omega -100.00  -75.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000  -30.0000 25

  6 omega   35.00  102.00   1.0000    7.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  178.0000  -60.0000 67
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0542389000
_diffrn_orient_matrix_UB_12      0.0114811000
_diffrn_orient_matrix_UB_13      -0.0124118000
_diffrn_orient_matrix_UB_21      -0.0108613000
_diffrn_orient_matrix_UB_22      0.0202385000
_diffrn_orient_matrix_UB_23      0.0341962000
_diffrn_orient_matrix_UB_31      0.0214656000
_diffrn_orient_matrix_UB_32      0.0392723000
_diffrn_orient_matrix_UB_33      -0.0139796000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0405
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22883
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.81
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.210
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.768
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.140
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.006(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         7775
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0498P)^2^+13.5917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1170
_reflns_number_gt                6531
_reflns_number_total             7775
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500888d_si_003.cif
_cod_data_source_block           Compound_5_str1472
_cod_depositor_comments
'Adding full bibliography for 4084855--4084857.cif.'
_cod_original_cell_volume        3380.66(15)
_cod_database_code               4084856
_chemical_oxdiff_formula         'C29 H34 N3 Ir'
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32