Electrocatalytic Hydrogen Evolution with a Cobalt Complex Bearing Pendant Proton Relays: Acid Strength and Applied Potential Govern Mechanism and Stability.
Queyriaux, Nicolas; Sun, Dongyue; Fize, Jennifer; Pecaut, Jacques; Field, Martin J.; Chavarot-Kerlidou, Murielle; Artero, Vincent; Journal of the American Chemical Society  (2019) –; doi:10.1021/jacs.9b10407

data_4133810
_publ_section_title
;
 Electrocatalytic Hydrogen Evolution with a Cobalt Complex Bearing Pendant
 Proton Relays: Acid Strength and Applied Potential Govern Mechanism and
 Stability.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.9b10407
_journal_year                    2019
_chemical_formula_sum            'C21 H20 Cl2 Co N6 O'
_chemical_formula_weight         502.26
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                86.398(8)
_cell_angle_beta                 89.550(8)
_cell_angle_gamma                83.366(8)
_cell_formula_units_Z            2
_cell_length_a                   8.4314(9)
_cell_length_b                   10.6619(9)
_cell_length_c                   11.7732(12)
_cell_measurement_reflns_used    3232
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.9140
_cell_measurement_theta_min      3.2710
_cell_volume                     1049.19(18)
_computing_cell_refinement
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171. 36.28, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_data_collection
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171.36.28, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_data_reduction
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171. 36.28, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_molecular_graphics
;
Mercury 3.1 New software for searching the Cambridge Structural Database 
and visualizing crystal structures (I.J. Bruno, J.C. Cole, P.R. Edgington, 
M. Kessler, C.F. Macrae, P. McCabe, J. Pearson, R. Taylor, 
Acta Cryst., 2002, B58, 389-397)
;
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement
;
OLEX2: a complete structure solution, refinement and analysis program 
(O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34).
;
_computing_structure_solution
;
SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   -4.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   77.0000  -90.0000 100

  2 omega  -25.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000  150.0000 92

  3 omega  -25.00   67.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000   30.0000 92

  4 omega -100.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801    0.0000  120.0000 146

  5 omega    4.00   68.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   57.0000   90.0000 64

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12731
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.500
_diffrn_reflns_theta_min         3.273
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.100
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96559
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent dark brown'
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_description       block
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.525
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     360
_refine_ls_number_reflns         6357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0239P)^2^+0.3626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0758
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5095
_reflns_number_total             6357
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10407_si_002.cif
_cod_data_source_block           nq258
_cod_database_code               4133810
_shelx_estimated_absorpt_t_min   0.667
_shelx_estimated_absorpt_t_max   0.734
_shelxl_version_number           2013-4
_shelx_res_checksum              24145
_shelx_hkl_checksum              67560