The Trans Effect in Electrocatalytic CO<sub>2</sub> Reduction: Mechanistic Studies of Asymmetric Ruthenium Pyridyl-Carbene Catalysts.
Gonell, Sergio; Massey, Marsha D.; Moseley, Ian P.; Schauer, Cynthia K.; Muckerman, James T.; Miller, Alexander J. M.; Journal of the American Chemical Society 141 (2019) 6658–6671; doi:10.1021/jacs.9b01735

data_4128255
_publ_section_title
;
 The Trans Effect in Electrocatalytic CO<sub>2</sub> Reduction:
 Mechanistic Studies of Asymmetric Ruthenium Pyridyl-Carbene Catalysts.
;
_journal_issue                   16
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6658
_journal_page_last               6671
_journal_paper_doi               10.1021/jacs.9b01735
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety         'C29 H19 N6 O Ru, 2(C F3 O3 S), C5.08 O3'
_chemical_formula_sum            'C36.08 H19 F6 N6 O10 Ru S2'
_chemical_formula_weight         975.75
_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
_audit_creation_date             2018-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_cell_angle_alpha                90
_cell_angle_beta                 114.047(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0654(11)
_cell_length_b                   18.8075(13)
_cell_length_c                   15.5986(11)
_cell_measurement_reflns_used    9985
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      70.229
_cell_measurement_theta_min      3.441
_cell_volume                     3768.3(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            37088
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.339
_diffrn_reflns_theta_min         3.441
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.282
_exptl_absorpt_correction_T_max  0.7881
_exptl_absorpt_correction_T_min  0.5901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0756 before and 0.0667 after correction. The Ratio of minimum to maximum transmission is 0.7488. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             1950
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.481
_refine_diff_density_min         -1.485
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         7097
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.082
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0610P)^2^+8.7900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6061
_reflns_number_total             7097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01735_si_002.cif
_cod_data_source_block           x1610002
_cod_database_code               4128255
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.634
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F7)
3. Others
 Sof(C32)=1-FVAR(1)
 Sof(C31)=FVAR(1)
 Sof(F9)=1-FVAR(2)
 Sof(F5)=FVAR(2)
 Sof(F7)=1-FVAR(3)
 Sof(F6)=FVAR(3)
 Sof(F8)=1-FVAR(4)
 Sof(F4)=FVAR(4)
 Fixed Sof: C34(0.75) C36(0.33333)
4.a Aromatic/amide H refined with riding coordinates:
 C15(H15), C8(H8), C21(H21), C23(H23), C18(H18), C16(H16), C27(H27), C22(H22),
 C7(H7), C6(H6), C14(H14), C12(H12), C28(H28), C11(H11), C17(H17), C29(H29),
 C26(H26), C13(H13), C5(H5)
;
_olex2_submission_special_instructions 'No special instructions were received'