Electrocatalytic hydrogen production activity with a copper(ii)-dipyridylamine complex in acidic water
Diyali, Nilankar; Chettri, Meena; Saha, Subhajit; Saha, Ankita; Kundu, Subhankar; Mondal, Debasish; Dhak, Debasis; Biswas, Bhaskar; CrystEngComm 25 (2023) 6837–6844; doi:10.1039/D3CE00996C

data_7247745
_publ_section_title
;
 Electrocatalytic hydrogen production activity with a
 copper(ii)-dipyridylamine complex in acidic water
;
_journal_issue                   48
_journal_name_full               CrystEngComm
_journal_page_first              6837
_journal_page_last               6844
_journal_paper_doi               10.1039/D3CE00996C
_journal_volume                  25
_journal_year                    2023
_chemical_formula_moiety         'C20 H18 Cu N9, Cl, 4(H2 O)'
_chemical_formula_sum            'C20 H26 Cl Cu N9 O4'
_chemical_formula_weight         555.486
_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_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2023-10-04 deposited with the CCDC.	2023-11-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.071(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0295(4)
_cell_length_b                   27.8164(16)
_cell_length_c                   12.8722(7)
_cell_measurement_reflns_used    3422
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      30.0830
_cell_measurement_theta_min      3.1910
_cell_volume                     2485.5(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.35c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      250.00(10)
_diffrn_measured_fraction_theta_full 0.9993
_diffrn_measured_fraction_theta_max 0.8830
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -68.00 -41.00   1.00   23.00    --   29.89  54.00-180.00   27
  2  \w    -67.00 117.00   1.00   23.00    --   29.89  54.00  60.00  184
;
_diffrn_measurement_device       'two-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Mini (ROW)'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0207
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.9993
_diffrn_reflns_Laue_measured_fraction_max 0.8830
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13179
_diffrn_reflns_point_group_measured_fraction_full 0.9993
_diffrn_reflns_point_group_measured_fraction_max 0.8830
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         32.76
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    1.032
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.35c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1150.771
_exptl_crystal_size_max          0.032
_exptl_crystal_size_mid          0.026
_exptl_crystal_size_min          0.023
_refine_diff_density_max         1.6626
_refine_diff_density_min         -1.5850
_refine_diff_density_rms         0.1215
_refine_ls_d_res_high            0.6567
_refine_ls_d_res_low             7.4910
_refine_ls_goodness_of_fit_ref   1.0320
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    52
_refine_ls_number_parameters     232
_refine_ls_number_reflns         8127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0320
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0576
_refine_ls_shift/su_max          -0.0006
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.2685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1378
_refine_ls_wR_factor_ref         0.1577
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              9
_reflns_limit_h_min              -10
_reflns_limit_k_max              39
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                6096
_reflns_number_total             8127
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3ce00996c2.cif
_cod_data_source_block           me-03-violet
_cod_depositor_comments          'Adding full bibliography for 7247745.cif.'
_cod_database_code               7247745
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C7) = Uanis(C6)
Uanis(N1) = Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5)
Uanis(C6) = Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(N3)
Uanis(N4) = Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15)
Uanis(N6) = Uanis(C16) = Uanis(C17) = Uanis(C18) = Uanis(C19) = Uanis(C20)
3.a Free rotating group:
 O1(H1a,H1b), O2(H2b,H2c), O3(H3a,H3b), O4(H4a,H4b)
3.b Aromatic/amide H refined with riding coordinates:
 N2(H2), N5(H5), C1(H1), C2(H2a), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9),
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
  C20(H20)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;