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_4084855
_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_formula_moiety         'C33 H47 Ir N3, F6 P'
_chemical_formula_sum            'C33 H47 F6 Ir N3 P'
_chemical_formula_weight         822.91
_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
_audit_creation_date             2013-07-25
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2013.07.19 svn.r0, GUI svn.r4539)
;
_cell_angle_alpha                101.7413(16)
_cell_angle_beta                 102.1693(14)
_cell_angle_gamma                101.9854(16)
_cell_formula_units_Z            2
_cell_length_a                   8.71445(14)
_cell_length_b                   11.7851(2)
_cell_length_c                   17.6537(3)
_cell_measurement_reflns_used    32305
_cell_measurement_temperature    199(3)
_cell_measurement_theta_max      29.4720
_cell_measurement_theta_min      2.9960
_cell_volume                     1674.70(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELX, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      199(3)
_diffrn_detector_area_resol_mean 10.4051
_diffrn_measured_fraction_theta_full 0.9987
_diffrn_measured_fraction_theta_max 0.8567
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0008546000
_diffrn_orient_matrix_UB_12      0.0583481000
_diffrn_orient_matrix_UB_13      -0.0044471000
_diffrn_orient_matrix_UB_21      0.0395517000
_diffrn_orient_matrix_UB_22      0.0246120000
_diffrn_orient_matrix_UB_23      0.0413881000
_diffrn_orient_matrix_UB_31      0.0766527000
_diffrn_orient_matrix_UB_32      0.0067141000
_diffrn_orient_matrix_UB_33      -0.0087565000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0536
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            74491
_diffrn_reflns_theta_full        30.11
_diffrn_reflns_theta_max         30.11
_diffrn_reflns_theta_min         2.86
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.4759
_exptl_crystal_size_mid          0.2029
_exptl_crystal_size_min          0.0637
_refine_diff_density_max         2.486
_refine_diff_density_min         -1.862
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     405
_refine_ls_number_reflns         8920
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0332
_refine_ls_shift/su_max          0.044
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+4.2443P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0849
_refine_ls_wR_factor_ref         0.0885
_reflns_number_gt                8239
_reflns_number_total             8920
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500888d_si_003.cif
_cod_data_source_block           Compound_4_str1533
_cod_depositor_comments
'Adding full bibliography for 4084855--4084857.cif.'
_cod_original_cell_volume        1674.71(5)
_cod_database_code               4084855
_chemical_oxdiff_formula         'C33 H47 N3 P F6 Ir'
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 N2(H2A,H2B), C24(H24A,H24B), C20(H20A,H20B), C25(H25A,H25B), C26(H26A,H26B),
 C22(H22A,H22B), C21(H21A,H21B)
2.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C13(H13), C8(H8), C7(H7), C11(H11), C18(H18), C10(H10), C17(H17)
2.d Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C37(H37A,H37B,H37C), C35(H35A,H35B,H35C), C29(H29A,H29B,
 H29C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C), C4(H4A,H4B,H4C), C27(H27A,
 H27B,H27C)
;