#------------------------------------------------------------------------------
#$Date: 2023-07-05 02:04:24 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284791 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/33/7713379.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7713379
loop_
_publ_author_name
'Debnath, Ananya'
'Diyali, Sangharaj'
'Das, Mainak'
'Panda, Subhra Jyoti'
'Mondal, Debasish'
'Dhak, Debasis'
'Purohit, Chandra Shekhar'
'Ray, Partha Pratim'
'Biswas, Bhaskar'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -9.00  47.00   0.50    1.00    --    7.48-106.00  -5.00  112
  2  ω    -55.00  17.00   0.50    1.00    --    7.48 -57.00 -60.00  144
  3  ω    -10.00  41.00   0.50    1.00    --    7.48 -99.00  30.00  102
  4  ω    -14.00  31.00   0.50    1.00    --    7.48 -99.00-150.00   90
  5  ω     -8.00  18.00   0.50    1.00    --   -8.10  77.00-180.00   52
  6  ω    -71.00  -7.00   0.50    1.00    --   -8.10 -37.00   0.00  128
  7  ω    -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       'ω 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/[σ²(Fo²)+(0.0407P)²+3.2587P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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)
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.58015(3) 0.52620(3) 0.40742(4) 0.03013(14) Uani 1 1 d . . . . .
S1 S 0.12309(7) 0.47865(10) 0.20026(8) 0.0447(2) Uani 1 1 d . . . . .
O1 O 0.63983(18) 0.3507(2) 0.4600(2) 0.0408(6) Uani 1 1 d . . . . .
O2 O 0.750000 0.5994(3) 0.500000 0.0272(6) Uani 1 2 d S T P . .
N1 N 0.9835(3) 0.7068(3) 0.6118(4) 0.0556(9) Uani 1 1 d . U . . .
H1A H 1.032385 0.725347 0.692770 0.067 Uiso 1 1 calc R U . . .
H1B H 1.035192 0.717316 0.573651 0.067 Uiso 1 1 calc R U . . .
N2 N 0.3972(2) 0.4665(2) 0.3242(3) 0.0339(6) Uani 1 1 d . . . . .
C1 C 0.2839(3) 0.4719(3) 0.2735(3) 0.0309(6) Uani 1 1 d . . . . .
C2 C 0.7544(6) 0.7320(5) 0.5341(5) 0.0262(12) Uani 0.5 1 d . . P . .
H2 H 0.761(7) 0.743(7) 0.612(6) 0.14(3) Uiso 1 1 d . . . . .
C3 C 0.8729(3) 0.7899(3) 0.5589(4) 0.0499(10) Uani 1 1 d . U . . .
H3 H 0.893(4) 0.866(4) 0.567(3) 0.038(10) Uiso 1 1 d . . . . .
C4 C 0.750000 0.2963(4) 0.500000 0.0283(8) Uani 1 2 d S T P . .
C5 C 0.750000 0.1540(4) 0.500000 0.0331(9) Uani 1 2 d S T P . .
H5A H 0.726338 0.122889 0.562850 0.050 Uiso 0.5 1 calc R U P A -1
H5B H 0.837905 0.122889 0.517903 0.050 Uiso 0.5 1 calc R U P A -1
H5C H 0.685757 0.122889 0.419246 0.050 Uiso 0.5 1 calc R U P A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cu1 S1 95.85(8) . 6_665 ?
O1 Cu1 N1 167.50(14) . 2_656 ?
O2 Cu1 S1 89.74(2) . 6_665 ?
O2 Cu1 O1 94.43(9) . . ?
O2 Cu1 N1 84.46(11) . 2_656 ?
O2 Cu1 N2 172.28(10) . . ?
N1 Cu1 S1 96.60(11) 2_656 6_665 ?
N2 Cu1 S1 96.20(9) . 6_665 ?
N2 Cu1 O1 89.87(9) . . ?
N2 Cu1 N1 89.95(11) . 2_656 ?
C1 S1 Cu1 96.80(12) . 6_565 ?
C4 O1 Cu1 133.4(2) . . ?
Cu1 O2 Cu1 132.37(15) . 2_656 ?
C2 O2 Cu1 116.9(2) . . ?
C2 O2 Cu1 116.9(2) 2_656 2_656 ?
C2 O2 Cu1 108.9(2) 2_656 . ?
C2 O2 Cu1 108.9(2) . 2_656 ?
C2 O2 C2 31.8(4) . 2_656 ?
Cu1 N1 H1A 109.8 2_656 . ?
Cu1 N1 H1B 109.8 2_656 . ?
H1A N1 H1B 108.3 . . ?
C3 N1 Cu1 109.2(2) . 2_656 ?
C3 N1 H1A 109.8 . . ?
C3 N1 H1B 109.8 . . ?
C1 N2 Cu1 158.5(3) . . ?
N2 C1 S1 179.3(3) . . ?
O2 C2 H2 113(5) . . ?
O2 C2 C3 106.0(4) . 2_656 ?
C2 C2 O2 74.1(2) 2_656 . ?
C2 C2 H2 172(5) 2_656 . ?
C2 C2 C3 82.8(8) 2_656 . ?
C2 C2 C3 65.7(7) 2_656 2_656 ?
C3 C2 O2 112.9(4) . . ?
C3 C2 H2 96(5) . . ?
C3 C2 H2 109(5) 2_656 . ?
C3 C2 C3 119.8(5) . 2_656 ?
N1 C3 C2 116.4(3) . 2_656 ?
N1 C3 H3 113(3) . . ?
C2 C3 N1 113.8(4) . . ?
C2 C3 C2 31.5(4) . 2_656 ?
C2 C3 H3 130(3) . . ?
C2 C3 H3 127(3) 2_656 . ?
O1 C4 O1 126.0(4) 2_656 . ?
O1 C4 C5 117.0(2) . . ?
O1 C4 C5 116.98(19) 2_656 . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 S1 2.7932(10) 6_665 ?
Cu1 O1 1.970(2) . ?
Cu1 O2 1.9052(12) . ?
Cu1 N1 2.007(3) 2_656 ?
Cu1 N2 1.962(2) . ?
S1 C1 1.636(3) . ?
O1 C4 1.259(3) . ?
O2 C2 1.449(6) . ?
O2 C2 1.449(6) 2_656 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C3 1.425(4) . ?
N2 C1 1.153(4) . ?
C2 C2 0.794(10) 2_656 ?
C2 H2 0.93(7) . ?
C2 C3 1.384(6) . ?
C2 C3 1.507(6) 2_656 ?
C3 H3 0.82(4) . ?
C4 C5 1.496(6) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cu1 O1 C4 O1 15.28(17) . . . 2_656 ?
Cu1 O1 C4 C5 -164.72(17) . . . . ?
Cu1 O2 C2 C2 -82.7(8) . . . 2_656 ?
Cu1 O2 C2 C2 110.7(8) 2_656 . . 2_656 ?
Cu1 O2 C2 C3 -157.5(3) . . . . ?
Cu1 O2 C2 C3 168.9(3) 2_656 . . 2_656 ?
Cu1 O2 C2 C3 35.9(4) 2_656 . . . ?
Cu1 O2 C2 C3 -24.5(4) . . . 2_656 ?
Cu1 N1 C3 C2 -21.1(5) 2_656 . . 2_656 ?
Cu1 N1 C3 C2 13.7(5) 2_656 . . . ?
O2 C2 C3 N1 -32.8(6) . . . . ?
O2 C2 C3 C2 69.3(4) . . . 2_656 ?
C2 O2 C2 C3 58.2(7) 2_656 . . 2_656 ?
C2 O2 C2 C3 -74.8(8) 2_656 . . . ?
C2 C2 C3 N1 -102.1(5) 2_656 . . . ?
C3 C2 C3 N1 -158.7(5) 2_656 . . . ?
C3 C2 C3 C2 -56.6(5) 2_656 . . 2_656 ?
