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_4128253
_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         'C30 H25 N7 Ru, 2(F6 P), 2(C3 H6 O)'
_chemical_formula_sum            'C36 H37 F12 N7 O2 P2 Ru'
_chemical_formula_weight         990.73
_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             2019-02-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 92.385(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8554(3)
_cell_length_b                   8.8160(3)
_cell_length_c                   50.7233(17)
_cell_measurement_reflns_used    4794
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.130
_cell_measurement_theta_min      3.489
_cell_volume                     3956.5(2)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0632
_diffrn_reflns_av_unetI/netI     0.0454
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -62
_diffrn_reflns_number            36686
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.272
_diffrn_reflns_theta_min         1.743
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.885
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0698 before and 0.0637 after correction. The Ratio of minimum to maximum transmission is 0.9141. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear reddish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_description       block
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.093
_exptl_crystal_size_mid          0.088
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     547
_refine_ls_number_reflns         7768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0340P)^2^+2.5925P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0790
_refine_ls_wR_factor_ref         0.0832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6555
_reflns_number_total             7768
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01735_si_002.cif
_cod_data_source_block           x1708001
_cod_database_code               4128253
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.705
_shelx_estimated_absorpt_t_min   0.659
_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.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C20(H20), C15(H15), C7(H7), C17(H17), C28(H28), C14(H14), C16(H16),
 C27(H27), C4(H4), C6(H6), C12(H12), C22(H22), C26(H26), C11(H11), C25(H25),
 C21(H21), C13(H13), C5(H5)
2.b Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C2(H2A,H2B,H2C), C33(H33A,H33B,H33C), C31(H31A,H31B,
 H31C), C36(H36A,H36B,H36C), C34(H34A,H34B,H34C)
;
_olex2_submission_special_instructions 'No special instructions were received'