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_4133400
_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 Br Mn N2 O3 S'
_chemical_formula_sum            'C14 H10 Br Mn N2 O3 S'
_chemical_formula_weight         421.15
_chemical_name_systematic        Mn(4-mercaptomethyl-2,2'-bipyridine)(CO)3Br
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     direct
_audit_creation_date             2016-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-05-02 # Formatted by publCIF

;
_cell_angle_alpha                92.589(7)
_cell_angle_beta                 97.506(7)
_cell_angle_gamma                93.047(7)
_cell_formula_units_Z            2
_cell_length_a                   6.6811(15)
_cell_length_b                   8.3367(18)
_cell_length_c                   13.932(3)
_cell_measurement_reflns_used    2033
_cell_measurement_temperature    100
_cell_measurement_theta_max      24.27
_cell_measurement_theta_min      2.79
_cell_volume                     767.2(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 v2013.6-2 (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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9961
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0950
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10791
_diffrn_reflns_theta_full        25.0000
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         1.48
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.612
_exptl_absorpt_correction_T_max  0.0916
_exptl_absorpt_correction_T_min  0.0617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0568 after correction.
The Ratio of minimum to maximum transmission is 0.6736.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear orangish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.8230
_exptl_crystal_description       needle
_exptl_crystal_F_000             416.5493
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.3135
_refine_diff_density_min         -1.1900
_refine_diff_density_rms         0.2819
_refine_ls_d_res_high            0.8297
_refine_ls_d_res_low             13.7933
_refine_ls_goodness_of_fit_ref   1.0647
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2796
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0647
_refine_ls_R_factor_all          0.1085
_refine_ls_R_factor_gt           0.0619
_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^)+(0.0514P)^2^+2.0373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -8
_reflns_limit_k_max              9
_reflns_limit_k_min              -10
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                1850
_reflns_number_total             2796
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            ja8b09852_si_003.cif
_cod_data_source_block           p-1_a
_cod_database_code               4133400
_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:
 C13(H13), C12(H12), C7(H7), C10(H10), C4(H4), C5(H5), C6(H6)
2.b Idealised Me refined as rotating group:
 C14(H14a,H14b,H14c)
;
_olex2_submission_original_sample_id 160311
_olex2_submission_special_instructions 'No special instructions were received'