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_4086405
_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            'C13 H13 N3 O4 S'
_chemical_formula_weight         307.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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            8
_cell_length_a                   7.2086(6)
_cell_length_b                   14.8189(11)
_cell_length_c                   24.7866(19)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    100.(2)
_cell_measurement_theta_max      28.5838
_cell_measurement_theta_min      4.5406
_cell_volume                     2647.8(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 0.960
_diffrn_measured_fraction_theta_max 0.960
_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  0.0700
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            29941
_diffrn_reflns_theta_full        28.90
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         1.64
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6965
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.214
_exptl_crystal_size_mid          0.204
_exptl_crystal_size_min          0.132
_refine_diff_density_max         0.494
_refine_diff_density_min         -0.640
_refine_ls_extinction_method     none1.cif
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+2.4643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1158
_reflns_number_gt                2455
_reflns_number_total             3352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om5b00864_si_002.cif
_cod_data_source_block           1
_cod_database_code               4086405
_shelx_res_checksum              76966
_shelx_hkl_checksum              49337