Base-Free Transfer Hydrogenation of Ketones Using Cp*Ir(pyridinesulfonamide)Cl Precatalysts
Ruff, Andrew; Kirby, Christopher; Chan, Benny C.; O'Connor, Abby R.; Organometallics 35 (2016) 327–335; doi:10.1021/acs.organomet.5b00864

data_4086408
_publ_section_title
;
 Base-Free Transfer Hydrogenation of Ketones Using
 Cp*Ir(pyridinesulfonamide)Cl Precatalysts
;
_journal_name_full               Organometallics
_journal_page_first              327
_journal_page_last               335
_journal_paper_doi               10.1021/acs.organomet.5b00864
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C25 H31 Cl3 Ir N3 O4 S'
_chemical_formula_weight         768.14
_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
_audit_creation_method           'APEX2 v2013.6-2'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4255(6)
_cell_length_b                   13.2575(10)
_cell_length_c                   25.0656(19)
_cell_measurement_reflns_used    193
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.2387
_cell_measurement_theta_min      4.7494
_cell_volume                     2799.9(4)
_computing_cell_refinement       'APEX2 v2013.6-2 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service v2013.10.0.0'
_computing_data_reduction        'SAINT V8.32B (Bruker AXS Inc., 2013)'
_computing_molecular_graphics
'Crystalmaker v.8.7.2 (CrystalMaker Software Ltd)'
_computing_publication_material  'APEX2 v2013.6-2 (Bruker AXS)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       '\w and \f'
_diffrn_radiation_monochromator  Graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0665
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33911
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.84
_diffrn_reflns_theta_min         1.63
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.166
_exptl_absorpt_correction_T_max  0.90473
_exptl_absorpt_correction_T_min  0.50780
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_density_diffrn    1.822
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.567
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.435
_refine_diff_density_min         -1.278
_refine_ls_abs_structure_details 'Refined as an inversion twin.'
_refine_ls_abs_structure_Flack   -0.003(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         6902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0360
_refine_ls_R_factor_gt           0.0304
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0505
_refine_ls_wR_factor_ref         0.0522
_reflns_number_gt                6307
_reflns_number_total             6902
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00864_si_002.cif
_cod_data_source_block           9
_cod_database_code               4086408
_shelx_res_checksum              34258
_shelx_hkl_checksum              39885