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_4087086
_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         'C20 H26 Cl Ir N3 O, C1 F3 O3 S'
_chemical_formula_sum            'C21 H26 Cl F3 Ir N3 O4 S'
_chemical_formula_weight         701.16
_chemical_name_common            '3 [Cp(star)IrCl(NHC(Me)-py(OMe))]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                 97.709(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.3609(3)
_cell_length_b                   15.3328(6)
_cell_length_c                   22.3550(9)
_cell_measurement_reflns_used    9484
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      35.0104
_cell_measurement_theta_min      2.6568
_cell_volume                     2500.25(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 0.996
_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  0.0363
_diffrn_reflns_av_unetI/netI     0.0285
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            63707
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.073
_diffrn_reflns_theta_min         1.615
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.585
_exptl_absorpt_correction_T_max  0.2877
_exptl_absorpt_correction_T_min  0.1843
_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    1.863
_exptl_crystal_description       plate
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.410
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.190
_refine_diff_density_max         2.716
_refine_diff_density_min         -5.131
_refine_diff_density_rms         0.148
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.280
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         11027
_refine_ls_number_restraints     249
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0464
_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^)+10.9119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0870
_refine_ls_wR_factor_ref         0.0894
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9310
_reflns_number_total             11027
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00806_si_003.cif
_cod_data_source_block           complex3_SS13b_0m_a
_cod_depositor_comments
'Adding full bibliography for 4087084--4087091.cif.'
_cod_database_code               4087086
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.208
_shelx_estimated_absorpt_t_max   0.417
_exptl_absorpt_special_details
;
Additional spherical absorption correction applied with mu*r =  0.9500
;
_shelx_res_checksum              96168
_shelx_hkl_checksum              9945