Iridium Catalysts for Acceptorless Dehydrogenation of Alcohols to Carboxylic Acids: Scope and Mechanism.
Cherepakhin, Valeriy; Williams, Travis J.; ACS catalysis 8 (2018) 3754–3763; doi:10.1021/acscatal.8b00105

data_4515606
_publ_section_title
;
 Iridium Catalysts for Acceptorless Dehydrogenation of Alcohols to
 Carboxylic Acids: Scope and Mechanism.
;
_journal_issue                   5
_journal_name_full               'ACS catalysis'
_journal_page_first              3754
_journal_page_last               3763
_journal_paper_doi               10.1021/acscatal.8b00105
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C22 H37 Ir N P'
_chemical_formula_weight         538.69
_chemical_name_common            VAL1
_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'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5276(13)
_cell_length_b                   10.7464(14)
_cell_length_c                   18.567(2)
_cell_measurement_reflns_used    9753
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      30.5292
_cell_measurement_theta_min      2.1910
_cell_volume                     2100.6(4)
_computing_cell_refinement       'APEX3 v2016.5-0 (Bruker AXS, 2016)'
_computing_data_collection
'Bruker Instrument Service v2012.12.0.3 (Bruker AXS, 2012)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS, 2013)'
_computing_molecular_graphics    'shelXle (C.B. Huebschle, rev 807)'
_computing_publication_material  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_structure_refinement  'SHELXTL XL 2014/7 (Bruker AXS, 2014)'
_computing_structure_solution    'SHELXTL XT 2014/5 (Bruker AXS, 2014)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'omega- and phi-scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_type           'MoK\a '
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0432
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            43910
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus tube'
_exptl_absorpt_coefficient_mu    6.437
_exptl_absorpt_correction_T_max  0.34
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.213
_refine_diff_density_max         2.336
_refine_diff_density_min         -0.666
_refine_ls_abs_structure_details
;

Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.487(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         4809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0145
_refine_ls_R_factor_gt           0.0143
_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^)+(0.0162P)^2^+1.1237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0354
_reflns_number_gt                4770
_reflns_number_total             4809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00105_si_002.cif
_cod_data_source_block           VAL1
_cod_original_cell_volume        2100.6(5)
_cod_database_code               4515606
_shelx_res_checksum              12456
_shelx_hkl_checksum              13597