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_4128254
_publ_section_title
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 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 H22 N6 O Ru, 2(F6 P), C3 H6 O'
_chemical_formula_sum            'C32 H28 F12 N6 O2 P2 Ru'
_chemical_formula_weight         919.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 109.7350(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6370(6)
_cell_length_b                   17.2240(7)
_cell_length_c                   16.2229(7)
_cell_measurement_reflns_used    9492
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.227
_cell_measurement_theta_min      3.675
_cell_volume                     3586.7(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.987
_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  0.0756
_diffrn_reflns_av_unetI/netI     0.0539
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            28681
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.427
_diffrn_reflns_theta_min         3.675
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.328
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.5126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0954 before and 0.0566 after correction. The Ratio of minimum to maximum transmission is 0.6802. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.078
_refine_diff_density_max         1.044
_refine_diff_density_min         -1.136
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         7003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+8.1300P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5983
_reflns_number_total             7003
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01735_si_002.cif
_cod_data_source_block           x1710002
_cod_database_code               4128254
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.681
_shelx_estimated_absorpt_t_min   0.459
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(F9) = Uanis(F10)
3. Others
 Sof(F12)=1-FVAR(1)
 Sof(F11)=FVAR(1)
 Sof(F18)=1-FVAR(2)
 Sof(F17)=FVAR(2)
 Sof(F16)=1-FVAR(3)
 Sof(F15)=FVAR(3)
 Sof(F14)=1-FVAR(4)
 Sof(F13)=FVAR(4)
 Sof(F9)=1-FVAR(5)
 Sof(F10)=FVAR(5)
 Sof(F7)=1-FVAR(6)
 Sof(F8)=FVAR(6)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C26(H26), C16(H16), C18(H18), C22(H22), C8(H8), C15(H15), C7(H7),
 C29(H29), C21(H21), C14(H14), C11(H11), C27(H27), C6(H6), C23(H23), C28(H28),
 C17(H17), C13(H13), C12(H12)
4.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C32(H32A,H32B,H32C), C30(H30A,H30B,H30C)
;
_olex2_submission_special_instructions 'No special instructions were received'