Electrocatalytic Reduction of Protons to Hydrogen by a Copper Complex of the Pentadentate Ligand Dmphen-DPA in Nonaqueous Electrolyte
Gao, Yingchun; Zhao, Yingguo; Song, Xiao-Wei; Huang, Rong-Yi; Meng, Yan; Wang, Junwei; Wang, Wenjing; Chen, Chengneng; New Journal of Chemistry 43 (2019) 18134–18140; doi:10.1039/C9NJ04275J

data_7058899
_publ_section_title
;
 Electrocatalytic Reduction of Protons to Hydrogen by a Copper Complex of
 the Pentadentate Ligand Dmphen-DPA in Nonaqueous Electrolyte
;
_journal_issue                   46
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18134
_journal_page_last               18140
_journal_paper_doi               10.1039/C9NJ04275J
_journal_volume                  43
_journal_year                    2019
_chemical_formula_moiety         C26H23CuN5,2(ClO4)
_chemical_formula_sum            'C26 H23 Cl2 Cu N5 O8'
_chemical_formula_weight         667.93
_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   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-10-07 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.699(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7945(19)
_cell_length_b                   14.576(2)
_cell_length_c                   15.784(2)
_cell_measurement_reflns_used    5973
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.66
_cell_volume                     2715.6(7)
_computing_cell_refinement       'Siemens SMART & SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens XPREP'
_computing_molecular_graphics
'SHELXL-2016/6 crystallographic software package'
_computing_publication_material
'SHELXL-2016/6 crystallographic software package'
_computing_structure_refinement
'SHELXL-2016/6 crystallographic software package'
_computing_structure_solution
'SHELXL-2016/6 crystallographic software package'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  BrukerAXS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20485
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.526
_diffrn_reflns_theta_min         2.660
_exptl_absorpt_coefficient_mu    1.062
_exptl_absorpt_correction_T_max  .8990
_exptl_absorpt_correction_T_min  .8090
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_description       Block
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          .20
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .10
_refine_diff_density_max         0.341
_refine_diff_density_min         -0.247
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         6202
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0445P)^2^+1.0957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4473
_reflns_number_total             6202
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04275j2.cif
_cod_data_source_block           S
_cod_database_code               7058899
_shelx_shelxl_version_number     2016/6
_refine_ls_r_factor_ref          0.0594
_shelx_res_checksum              31339