CO<sub>2</sub> Reduction Catalysts on Gold Electrode Surfaces Influenced by Large Electric Fields.
Clark, Melissa L.; Ge, Aimin; Videla, Pablo E.; Rudshteyn, Benjamin; Miller, Christopher J.; Song, Jia; Batista, Victor S.; Lian, Tianquan; Kubiak, Clifford P.; Journal of the American Chemical Society 140 (2018) 17643–17655; doi:10.1021/jacs.8b09852

data_4133401
_publ_section_title
;
 CO<sub>2</sub> Reduction Catalysts on Gold Electrode Surfaces Influenced
 by Large Electric Fields.
;
_journal_issue                   50
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17643
_journal_page_last               17655
_journal_paper_doi               10.1021/jacs.8b09852
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C14 H10 Cl N2 O3 Re S'
_chemical_formula_sum            'C14 H10 Cl N2 O3 Re S'
_chemical_formula_weight         507.96
_chemical_name_systematic        Re(4-methylthio-2,2'-bipyridine)(CO)3Cl
_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_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.859(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5295(6)
_cell_length_b                   12.7123(8)
_cell_length_c                   11.9526(8)
_cell_measurement_reflns_used    4769
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.35
_cell_volume                     1580.82(17)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9742
_diffrn_reflns_theta_full        25.3591
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.35
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.000
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6118
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1093 before and 0.0917 after correction.
The Ratio of minimum to maximum transmission is 0.8210.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.1342
_exptl_crystal_description       cubic
_exptl_crystal_F_000             960.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.5408
_refine_diff_density_min         -1.7422
_refine_diff_density_rms         0.3355
_refine_ls_d_res_high            0.8297
_refine_ls_d_res_low             8.6524
_refine_ls_goodness_of_fit_ref   1.0015
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2894
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0015
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0550P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1066
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              8
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              -8
_reflns_number_gt                2559
_reflns_number_total             2894
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b09852_si_002.cif
_cod_data_source_block           Kubiak_151012_MLC_0m
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4133401
_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:
 C4(H6), C7(H3), C6(H2), C5(H1), C13(H10), C10(H8), C12(H11)
2.b Idealised Me refined as rotating group:
 C14(H16a,H16b,H16c)
;
_olex2_submission_special_instructions 'No special instructions were received'