Harnessing the hydrogen evolution reaction (HER) through the electrical mobility of an embossed Ag(I)-molecular cage and a Cu(II)-coordination polymer.
Debnath, Ananya; Diyali, Sangharaj; Das, Mainak; Panda, Subhra Jyoti; Mondal, Debasish; Dhak, Debasis; Purohit, Chandra Shekhar; Ray, Partha Pratim; Biswas, Bhaskar; Dalton transactions (Cambridge, England : 2003) 52 (2023) 8850–8856; doi:10.1039/d3dt01073b

data_7713379
_publ_section_title
;
 Harnessing the hydrogen evolution reaction (HER) through the electrical
 mobility of an embossed Ag(I)-molecular cage and a Cu(II)-coordination
 polymer.
;
_journal_issue                   26
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8850
_journal_page_last               8856
_journal_paper_doi               10.1039/d3dt01073b
_journal_volume                  52
_journal_year                    2023
_chemical_formula_moiety         'C3.5 H5.5 Cu N2 O1.5 S'
_chemical_formula_sum            'C3.5 H5.5 Cu N2 O1.5 S'
_chemical_formula_weight         195.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-23
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-12-25 deposited with the CCDC.	2023-06-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.109(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   11.4097(8)
_cell_length_b                   10.5099(6)
_cell_length_c                   12.2374(10)
_cell_measurement_reflns_used    4198
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      31.1500
_cell_measurement_theta_min      3.7280
_cell_volume                     1306.2(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.9977
_diffrn_measured_fraction_theta_max 0.8490
_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     -9.00  47.00   0.50    1.00    --    7.48-106.00  -5.00  112
  2  \w    -55.00  17.00   0.50    1.00    --    7.48 -57.00 -60.00  144
  3  \w    -10.00  41.00   0.50    1.00    --    7.48 -99.00  30.00  102
  4  \w    -14.00  31.00   0.50    1.00    --    7.48 -99.00-150.00   90
  5  \w     -8.00  18.00   0.50    1.00    --   -8.10  77.00-180.00   52
  6  \w    -71.00  -7.00   0.50    1.00    --   -8.10 -37.00   0.00  128
  7  \w    -30.00  19.00   0.50    1.00    --   -8.10  77.00 150.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0564605000
_diffrn_orient_matrix_UB_12      0.0309046000
_diffrn_orient_matrix_UB_13      0.0454663000
_diffrn_orient_matrix_UB_21      0.0042843000
_diffrn_orient_matrix_UB_22      -0.0466244000
_diffrn_orient_matrix_UB_23      0.0434720000
_diffrn_orient_matrix_UB_31      0.0408411000
_diffrn_orient_matrix_UB_32      -0.0377866000
_diffrn_orient_matrix_UB_33      -0.0167693000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            7320
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.811
_diffrn_reflns_theta_min         3.741
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.579
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.985
_exptl_crystal_description       block
_exptl_crystal_F_000             780
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.716
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     97
_refine_ls_number_reflns         1883
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0495
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+3.2587P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0930
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1509
_reflns_number_total             1883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01073b2.cif
_cod_data_source_block           csp-cual1
_cod_original_cell_volume        1306.23(19)
_cod_original_formula_sum        'C3.50 H5.50 Cu N2 O1.50 S'
_cod_database_code               7713379
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C32 H28 Cu8 N12 O16 S8 '
_chemical_oxdiff_usercomment     'BLUE BLOCKS'
_shelx_estimated_absorpt_t_max   0.468
_shelx_estimated_absorpt_t_min   0.434
_diffrn_oxdiff_digest_frames
;
013baf0d454a2e831260ba99f6b91ed9050003512e0
;
_diffrn_oxdiff_digest_hkl
;
01b51f8da1d8cff7d1c1eec2a379ea3ecdf7db
;
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(N1) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
3. Others
 Fixed Sof: C2(0.5) H5A(0.5) H5B(0.5) H5C(0.5)
4.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
4.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C)
;
_shelx_res_checksum              32262
_shelx_hkl_checksum              93446
_olex2_exptl_crystal_mounting_method 'Mounted on the loop'
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.412
_oxdiff_exptl_absorpt_empirical_full_min 0.725