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_7058900
_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         C26H23ZnN5,2(ClO4)
_chemical_formula_sum            'C26 H23 Cl2 N5 O8 Zn'
_chemical_formula_weight         669.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_Hall           '-P 2ab 2ac'
_space_group_name_H-M_alt        'P c c n'
_symmetry_space_group_name_Hall  '-P 2ab 2ac'
_symmetry_space_group_name_H-M   'P c c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-10-12 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   26.3912(6)
_cell_length_b                   14.1307(3)
_cell_length_c                   14.7958(3)
_cell_measurement_reflns_used    9916
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      1.63
_cell_volume                     5517.7(2)
_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 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  BrukerAXS
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0313
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39104
_diffrn_reflns_point_group_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.635
_exptl_absorpt_coefficient_mu    1.144
_exptl_absorpt_correction_T_max  .795
_exptl_absorpt_correction_T_min  .760
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.612
_exptl_crystal_description       Block
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          .30
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .20
_refine_diff_density_max         1.370
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         4673
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_gt           0.0559
_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^)+(0.0799P)^2^+15.9685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1541
_refine_ls_wR_factor_ref         0.1698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3599
_reflns_number_total             4673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9nj04275j2.cif
_cod_data_source_block           Szn
_cod_database_code               7058900
_shelx_shelxl_version_number     2016/6
_refine_ls_r_factor_ref          0.0762
_shelx_res_checksum              42891