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_4084857
_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         'C33 H47 Ir N3, F6 P'
_chemical_formula_sum            'C33 H47 F6 Ir N3 P'
_chemical_formula_weight         822.91
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 91.3639(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.2778(2)
_cell_length_b                   9.17011(16)
_cell_length_c                   16.3880(3)
_cell_measurement_reflns_used    21555
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      29.2970
_cell_measurement_theta_min      3.0780
_cell_volume                     1694.34(5)
_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(14)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9219
_diffrn_measurement_details
;
  1 omega  -11.00   27.40   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000 -120.0000 48

  2 omega  -17.00    8.60   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000  -60.0000 32

  3 omega  -78.00   10.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -77.0000   90.0000 110

  4 omega  -34.60   63.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253   57.0000    0.0000 122

  5 omega  -99.00  -59.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000    0.0000 50

  6 omega  -17.00    9.40   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -99.0000    0.0000 33

  7 omega   35.00   62.20   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  178.0000   90.0000 34

  8 omega   62.00   88.40   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  178.0000   90.0000 33

  9 omega   58.00   97.20   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191 -178.0000    0.0000 49

 10 omega  -85.00    5.40   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.1253  -57.0000   30.0000 113

 11 omega   35.00  100.60   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  178.0000   30.0000 82

 12 omega   18.00   90.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191 -155.0000  128.2495 90

 13 omega  -14.00   86.80   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191   37.0000  -60.0000 126

 14 omega  -66.00   46.00   0.8000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       12.2191  -77.0000 -180.0000 140
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0066379000
_diffrn_orient_matrix_UB_12      -0.0206036000
_diffrn_orient_matrix_UB_13      -0.0415913000
_diffrn_orient_matrix_UB_21      -0.0581719000
_diffrn_orient_matrix_UB_22      -0.0252788000
_diffrn_orient_matrix_UB_23      0.0074131000
_diffrn_orient_matrix_UB_31      -0.0229740000
_diffrn_orient_matrix_UB_32      0.0701282000
_diffrn_orient_matrix_UB_33      -0.0095352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0303
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38409
_diffrn_reflns_theta_full        29.35
_diffrn_reflns_theta_max         29.35
_diffrn_reflns_theta_min         3.04
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    4.047
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84852
_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    1.613
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.1888
_exptl_crystal_size_mid          0.1282
_exptl_crystal_size_min          0.0851
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.747
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.024(4)
_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     475
_refine_ls_number_reflns         8581
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0195
_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^)+(0.0104P)^2^+0.7910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0376
_reflns_number_gt                7870
_reflns_number_total             8581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500888d_si_003.cif
_cod_data_source_block           Compound_6_str1456
_cod_depositor_comments
'Adding full bibliography for 4084855--4084857.cif.'
_cod_database_code               4084857
_chemical_oxdiff_formula         'C33 H46 N3 Ir'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32