A Matrix of Heterobimetallic Complexes for Interrogation of Hydrogen Evolution Reaction Electrocatalysts
Ghosh, Pokhraj; Ding, Shengda; Chupik, Rachel B.; Quiroz, Manuel; Hsieh, Chung-Hung; Bhuvanesh, Nattamai; Hall, Michael B.; Darensbourg, Marcetta Y.; Chem. Sci.  (2017) –; doi:10.1039/C7SC03378H

data_1547671
_publ_section_title
;
 A Matrix of Heterobimetallic Complexes for Interrogation of Hydrogen
 Evolution Reaction Electrocatalysts
;
_journal_name_full               'Chem. Sci.'
_journal_paper_doi               10.1039/C7SC03378H
_journal_year                    2017
_chemical_formula_sum            'C10.5 H21 Cl Fe N4 Ni O2 S2'
_chemical_formula_weight         449.44
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc142wkn
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-01-24 deposited with the CCDC.
2017-10-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.062(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.318(8)
_cell_length_b                   11.116(7)
_cell_length_c                   24.241(15)
_cell_measurement_reflns_used    5268
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.47
_cell_volume                     3319(4)
_computing_cell_refinement       'APEXII (Bruker, 2012a)'
_computing_data_collection       'APEXII (Bruker, 2012a)'
_computing_data_reduction        'SAINT (Bruker, 2012b)'
_computing_molecular_graphics    'shelXLe (H\"ubschle 2011)'
_computing_publication_material  'Ciftab (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS (Sheldrick 2008)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            20288
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.638
_diffrn_reflns_theta_min         2.468
_exptl_absorpt_coefficient_mu    2.429
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6617
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2009/1 (Bruker,2009) was employed for absorption correction.
wR2(int) was   0.0718 before and   0.0550 after correction.
The ratio of minimum to maximum transmission factors was   0.8871.
Additional spherical absorption correction applied with mu*r =  0.2000.
The \l/2 correction factor of 0.0015 was applied.
;
_exptl_crystal_colour            'dark brown       '
_exptl_crystal_density_diffrn    1.799
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.733
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4376
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0314
_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^)+(0.0296P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0708
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3564
_reflns_number_total             4376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc03378h2.cif
_cod_data_source_block           feni
_cod_original_formula_sum        'C10.50 H21 Cl Fe N4 Ni O2 S2'
_cod_database_code               1547671
_shelx_estimated_absorpt_t_min   0.443
_shelx_estimated_absorpt_t_max   0.888
_shelxl_version_number           2013-4
_shelx_res_checksum              14678