Iridium and Ruthenium Complexes of N-Heterocyclic Carbene- and Pyridinol-Derived Chelates as Catalysts for Aqueous Carbon Dioxide Hydrogenation and Formic Acid Dehydrogenation: The Role of the Alkali Metal
Siek, Sopheavy; Burks, Dalton B.; Gerlach, Deidra L.; Liang, Guangchao; Tesh, Jamie M.; Thompson, Courtney R.; Qu, Fengrui; Shankwitz, Jennifer E.; Vasquez, Robert M.; Chambers, Nicole; Szulczewski, Gregory J.; Grotjahn, Douglas B.; Webster, Charles Edwin; Papish, Elizabeth T.; Organometallics 36 (2017) 1091–; doi:10.1021/acs.organomet.6b00806

data_4087088
_publ_section_title
;
 Iridium and Ruthenium Complexes of N-Heterocyclic Carbene- and
 Pyridinol-Derived Chelates as Catalysts for Aqueous Carbon Dioxide
 Hydrogenation and Formic Acid Dehydrogenation: The Role of the Alkali
 Metal
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1091
_journal_paper_doi               10.1021/acs.organomet.6b00806
_journal_volume                  36
_journal_year                    2017
_chemical_formula_moiety         'C22 H27 Cl Ir N2 O2, C F3 O3 S'
_chemical_formula_sum            'C23 H27 Cl F3 Ir N2 O5 S'
_chemical_formula_weight         728.17
_chemical_name_common            '5Ir [Cp(star)IrCl(66dmbp)]OTf'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.661(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3686(3)
_cell_length_b                   15.6037(6)
_cell_length_c                   23.0349(8)
_cell_measurement_reflns_used    9701
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      34.6598
_cell_measurement_theta_min      2.7962
_cell_volume                     2618.29(17)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2013.10-0 (Bruker, 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Mercury CSD 3.5.1 (2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0299
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            63478
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.765
_diffrn_reflns_theta_min         1.582
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.339
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.3750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5 (Bruker AXS Inc., 2014)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.390
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.452
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     332
_refine_ls_number_reflns         11265
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0284
_refine_ls_R_factor_gt           0.0226
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+1.6838P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0486
_refine_ls_wR_factor_ref         0.0501
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9891
_reflns_number_total             11265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00806_si_003.cif
_cod_data_source_block           complex5Ir_DLG15_0m_a
_cod_depositor_comments
'Adding full bibliography for 4087084--4087091.cif.'
_cod_database_code               4087088
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.230
_shelx_estimated_absorpt_t_max   0.740
_shelx_res_checksum              10808
_shelx_hkl_checksum              7561