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_7713378
_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
'C38 H44 Ag2 N4 O6, 2(N O3), 0.5(C6), [+ solvents]'
_chemical_formula_sum            'C41 H44 Ag2 N6 O12'
_chemical_formula_weight         1028.56
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_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                72.7500(10)
_cell_angle_beta                 87.4870(10)
_cell_angle_gamma                74.1000(10)
_cell_formula_units_Z            1
_cell_length_a                   7.72690(10)
_cell_length_b                   12.04360(10)
_cell_length_c                   13.6225(2)
_cell_measurement_reflns_used    50129
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      37.8790
_cell_measurement_theta_min      3.5440
_cell_volume                     1163.40(3)
_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 0.9991
_diffrn_measured_fraction_theta_max 0.9422
_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      6.00  88.00   0.50    3.00    --   24.78  72.00  -6.00  164
  2  \w    -39.00  44.00   0.50    3.00    --   24.78 -72.00-136.00  166
  3  \w    -45.00  38.00   0.50    3.00    --  -25.72  72.00  -6.00  166
  4  \w    -89.00  -6.00   0.50    3.00    --  -25.72 -72.00-136.00  166
  5  \w      7.00  88.00   0.50    3.00    --   24.78  68.00 100.93  162
  6  \w    -42.00  28.00   0.50    3.00    --   24.78 -37.00  30.00  140
  7  \w    -42.00  28.00   0.50    3.00    --   24.78 -37.00-120.00  140
  8  \w     19.00  94.00   0.50    3.00    --   24.78  19.00-150.00  150
  9  \w     37.00  93.00   0.50    3.00    --   24.78-178.00-150.00  112
 10  \w     22.00  91.00   0.50    3.00    --   24.78  37.00 -90.00  138
 11  \w    -45.00  31.00   0.50    3.00    --   24.78 -19.00 -90.00  152
 12  \w     37.00  93.00   0.50    3.00    --   24.78-178.00 -90.00  112
 13  \w     22.00  91.00   0.50    3.00    --   24.78  37.00 -30.00  138
 14  \w    -88.00 -14.00   0.50    3.00    --  -25.72 -57.00 -60.00  148
 15  \w    -14.00  13.00   0.50    3.00    --  -25.72-104.00 -16.22   54
 16  \w    -92.00 -22.00   0.50    3.00    --  -25.72 -37.00 -30.00  140
 17  \w    -80.00 -30.00   0.50    3.00    --  -25.72 131.00 113.97  100
 18  \w    -81.00 -30.00   0.50    3.00    --  -25.72 132.00 -38.15  102
 19  \w    -88.00 -14.00   0.50    3.00    --  -25.72 -57.00  90.00  148
 20  \w    -23.00   6.00   0.50    3.00    --  -25.72 -92.00 166.44   58
 21  \w    -16.00  10.00   0.50    3.00    --  -25.72 -98.00 140.47   52
 22  \w    -94.00 -43.00   0.50    3.00    --  -25.72 154.00  54.76  102
 23  \w    -18.00   9.00   0.50    3.00    --  -25.72 -96.00  -0.41   54
 24  \w    -79.00 -30.00   0.50    3.00    --  -25.72 128.00-161.52   98
 25  \w    -32.00   2.00   0.50    3.00    --  -25.72 -85.00 122.34   68
 26  \w    -90.00 -38.00   0.50    3.00    --  -25.72 146.00-144.65  104
 27  \w    -93.00 -39.00   0.50    3.00    --  -25.72 149.00   5.70  108
 28  \w    -42.00  -3.00   0.50    3.00    --  -25.72 -76.00  40.63   78
 29  \w      6.00  76.00   0.50    3.00    --   24.78-125.00  -7.94  140
 30  \w     22.00  91.00   0.50    3.00    --   24.78  37.00-120.00  138
 31  \w    -45.00  31.00   0.50    3.00    --   24.78 -19.00  90.00  152
 32  \w     37.00  93.00   0.50    3.00    --   24.78-178.00   0.00  112
 33  \w    -16.00  10.00   0.50    3.00    --  -25.72 -98.00 126.37   52
 34  \w    -82.00 -33.00   0.50    3.00    --  -25.72 133.00  47.63   98
 35  \w    -93.00 -39.00   0.50    3.00    --  -25.72 149.00 148.50  108
 36  \w    -42.00  -2.00   0.50    3.00    --  -25.72 -77.00 -29.04   80
 37  \w    -49.00  10.00   0.50    3.00    --  -25.72  77.00  60.00  118
 38  \w    -79.00 -30.00   0.50    3.00    --  -25.72 128.00 -63.89   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      -0.0930706000
_diffrn_orient_matrix_UB_12      0.0247626000
_diffrn_orient_matrix_UB_13      -0.0139566000
_diffrn_orient_matrix_UB_21      -0.0200257000
_diffrn_orient_matrix_UB_22      -0.0460595000
_diffrn_orient_matrix_UB_23      0.0413581000
_diffrn_orient_matrix_UB_31      -0.0078955000
_diffrn_orient_matrix_UB_32      0.0370918000
_diffrn_orient_matrix_UB_33      0.0327439000
_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  0.0679
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            99131
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.571
_diffrn_reflns_theta_min         3.460
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83829
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             522
_exptl_crystal_preparation       'As per the reaction scheme'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.682
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.145
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         12597
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0982P)^2^+0.4521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9871
_reflns_number_total             12597
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt01073b2.cif
_cod_data_source_block           csp-ag-al1
_cod_database_code               7713378
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C38 H44 Ag2 N6 O12 '
_chemical_oxdiff_usercomment     'COLOURLESS BLOCKS'
_shelx_estimated_absorpt_t_max   0.840
_shelx_estimated_absorpt_t_min   0.773
_diffrn_oxdiff_digest_frames
;
01fe77740dd27b4dadac037b187f041413000259f95
;
_diffrn_oxdiff_digest_hkl
;
018e87d808bb49f4c6188e84f9a77d3a53a337
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.95
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Others
 Sof(O6)=1-FVAR(1)
 Sof(O6A)=FVAR(1)
 Fixed Sof: C22(0.5) C21(0.5) C20(0.5)
3.a Ternary CH refined with riding coordinates:
 C10(H10)
3.b Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C9(H9A,H9B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C8(H8), C14(H14), C6(H6), C3(H3), C15(H15), C4(H4), C17(H17),
 C12(H12), C16(H16)
3.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C1(H1A,H1B,H1C)
3.e Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56222
_shelx_hkl_checksum              30701
_shelx_fab_checksum              74775
_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 1.698
_oxdiff_exptl_absorpt_empirical_full_min 0.513