#------------------------------------------------------------------------------
#$Date: 2024-12-06 21:00:06 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296581 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/70/7717068.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_7717068
loop_
_publ_author_name
'Dubskikh, Vadim A.'
'Lysova, Anna A.'
'Kovalenko, Konstantin A.'
'Samsonenko, Denis G.'
'Dybtsev, Danil N.'
'Fedin, Vladimir P.'
_publ_section_title
;
 Metal-organic frameworks with a sulfur-rich heterocycle: synthesis, gas
 adsorption properties, and metal exchange.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              16654
_journal_page_last               16660
_journal_paper_doi               10.1039/d4dt02209b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_sum            'C34 H49 Cu N5 O14 S4 Zn'
_chemical_formula_weight         1008.93
_space_group_crystal_system      tetragonal
_space_group_IT_number           123
_space_group_name_Hall           '-P 4 2'
_space_group_name_H-M_alt        'P 4/m m m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-08 deposited with the CCDC.	2024-09-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   12.5936(7)
_cell_length_b                   12.5936(7)
_cell_length_c                   9.6955(14)
_cell_measurement_reflns_used    1235
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      24.60
_cell_measurement_theta_min      2.33
_cell_volume                     1537.7(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'ShelXle (Hübschle, 2011)'
_computing_publication_material  'CIFTAB (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT-2018 (Sheldrick, 2015)'
_diffrn_ambient_temperature      290(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.877
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     -7.00  21.00   0.25   72.50    --  -10.11 -99.00 -60.00  112
  2  ω    -74.00  -4.00   0.25   72.50    --  -10.11 -38.00-180.00  280
;
_diffrn_measurement_device       'κ-geometry four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0453
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.877
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            4079
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.877
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.041
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.920
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_description       block
_exptl_crystal_F_000             523
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.130
_refine_diff_density_max         1.827
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1099
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0462
_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)+(0.0748P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1133
_refine_ls_wR_factor_ref         0.1172
_reflns_Friedel_coverage         0.000
_reflns_number_gt                871
_reflns_number_total             1099
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02209b2.cif
_cod_data_source_block           fin146Cu_sq
_cod_depositor_comments
'Adding full bibliography for 7717067--7717068.cif.'
_cod_database_code               7717068
_shelx_shelxl_version_number     2019/3
_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_min   0.859
_shelx_estimated_absorpt_t_max   0.890
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x, y, -z'
'x, -y, -z'
'y, x, -z'
'-y, -x, -z'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x, -y, z'
'-x, y, z'
'-y, -x, z'
'y, x, z'
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
Zn1 Zn 0.500000 0.500000 0.65267(6) 0.0307(3) Uani 0.5 8 d DS T P A .
Cu1 Cu 0.500000 0.500000 0.65267(6) 0.0307(3) Uani 0.5 8 d S T P A .
N1 N 0.500000 0.500000 0.8649(4) 0.0338(10) Uani 1 8 d DS TU P . .
C1D C 0.457(3) 0.6008(16) 0.9209(14) 0.037(5) Uani 0.0625 1 d D U P A -1
H1DA H 0.384639 0.610590 0.887795 0.044 Uiso 0.0625 1 calc R U P A -1
H1DB H 0.499114 0.659802 0.887828 0.044 Uiso 0.0625 1 calc R U P A -1
C2D C 0.457(3) 0.6008(16) 1.0787(14) 0.038(6) Uani 0.0625 1 d D U P A -1
H2D1 H 0.499043 0.659831 1.111840 0.046 Uiso 0.0625 1 calc R U P A -1
H2D2 H 0.384596 0.610581 1.111808 0.046 Uiso 0.0625 1 calc R U P A -1
C3D C 0.435(3) 0.412(2) 0.9210(14) 0.037(4) Uani 0.0625 1 d D U P A -1
H3DA H 0.462703 0.344677 0.887968 0.045 Uiso 0.0625 1 calc R U P A -1
H3DB H 0.362478 0.418702 0.887770 0.045 Uiso 0.0625 1 calc R U P A -1
C4D C 0.435(3) 0.412(2) 1.0788(14) 0.039(6) Uani 0.0625 1 d D U P A -1
H4D1 H 0.362267 0.418919 1.111779 0.047 Uiso 0.0625 1 calc R U P A -1
H4D2 H 0.462320 0.344661 1.111977 0.047 Uiso 0.0625 1 calc R U P A -1
C5D C 0.6093(11) 0.487(4) 0.9208(14) 0.036(4) Uani 0.0625 1 d D U P A -1
H5DA H 0.653529 0.545116 0.887716 0.043 Uiso 0.0625 1 calc R U P A -1
H5DB H 0.639348 0.421304 0.887559 0.043 Uiso 0.0625 1 calc R U P A -1
C6D C 0.6091(10) 0.487(4) 1.0786(14) 0.037(5) Uani 0.0625 1 d D U P A -1
H6D1 H 0.639144 0.421108 1.111600 0.044 Uiso 0.0625 1 calc R U P A -1
H6D2 H 0.653549 0.544857 1.111757 0.044 Uiso 0.0625 1 calc R U P A -1
O1 O 0.34226(18) 0.500000 0.6152(2) 0.0618(7) Uani 1 2 d S TU P . .
C1 C 0.2981(3) 0.500000 0.500000 0.0492(10) Uani 1 4 d S TU P A .
C2 C 0.1805(3) 0.500000 0.500000 0.0560(12) Uani 1 4 d DS TU P . .
C3 C 0.1110(7) 0.500000 0.3874(9) 0.067(3) Uani 0.5 2 d DS TU P A .
H3 H 0.133355 0.500000 0.295928 0.080 Uiso 0.5 2 calc R U P . .
C4 C 0.000000 0.500000 0.4289(5) 0.0664(14) Uani 1 4 d DS TU P . .
S1 S 0.1144(2) 0.500000 0.6551(3) 0.0763(9) Uani 0.5 2 d S TU P A .
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'
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N1 Cu1 Zn1 180.0 . 9_666 ?
O1 Cu1 Zn1 79.64(7) . 9_666 ?
O1 Cu1 Zn1 79.64(7) 2_665 9_666 ?
O1 Cu1 Zn1 79.64(7) 3_655 9_666 ?
O1 Cu1 Zn1 79.64(7) 4_565 9_666 ?
O1 Cu1 N1 100.36(7) . . ?
O1 Cu1 N1 100.36(7) 2_665 . ?
O1 Cu1 N1 100.36(7) 3_655 . ?
O1 Cu1 N1 100.36(7) 4_565 . ?
O1 Cu1 O1 88.15(2) 3_655 . ?
O1 Cu1 O1 88.15(2) 3_655 2_665 ?
O1 Cu1 O1 88.15(2) 4_565 . ?
O1 Cu1 O1 88.15(2) 4_565 2_665 ?
O1 Cu1 O1 159.28(13) 2_665 . ?
O1 Cu1 O1 159.28(13) 3_655 4_565 ?
C1D N1 Cu1 111.5(6) . . ?
C1D N1 C5D 107.3(7) . . ?
C3D N1 Cu1 111.5(6) . . ?
C3D N1 C1D 107.6(7) . . ?
C3D N1 C5D 107.4(7) . . ?
C5D N1 Cu1 111.4(6) . . ?
N1 C1D H1DA 109.3 . . ?
N1 C1D H1DB 109.3 . . ?
N1 C1D C2D 111.5(12) . . ?
H1DA C1D H1DB 108.0 . . ?
C2D C1D H1DA 109.3 . . ?
C2D C1D H1DB 109.3 . . ?
N1 C2D C1D 111.6(11) 5_657 . ?
N1 C2D H2D1 109.3 5_657 . ?
N1 C2D H2D2 109.3 5_657 . ?
C1D C2D H2D1 109.3 . . ?
C1D C2D H2D2 109.3 . . ?
H2D1 C2D H2D2 108.0 . . ?
N1 C3D H3DA 109.3 . . ?
N1 C3D H3DB 109.3 . . ?
N1 C3D C4D 111.5(11) . . ?
H3DA C3D H3DB 108.0 . . ?
C4D C3D H3DA 109.3 . . ?
C4D C3D H3DB 109.3 . . ?
N1 C4D C3D 111.5(11) 5_657 . ?
N1 C4D H4D1 109.3 5_657 . ?
N1 C4D H4D2 109.3 5_657 . ?
C3D C4D H4D1 109.3 . . ?
C3D C4D H4D2 109.3 . . ?
H4D1 C4D H4D2 108.0 . . ?
N1 C5D H5DA 109.4 . . ?
N1 C5D H5DB 109.4 . . ?
N1 C5D C6D 111.3(11) . . ?
H5DA C5D H5DB 108.0 . . ?
C6D C5D H5DA 109.4 . . ?
C6D C5D H5DB 109.4 . . ?
N1 C6D C5D 111.7(11) 5_657 . ?
N1 C6D H6D1 109.3 5_657 . ?
N1 C6D H6D2 109.3 5_657 . ?
C5D C6D H6D1 109.3 . . ?
C5D C6D H6D2 109.3 . . ?
H6D1 C6D H6D2 107.9 . . ?
C1 O1 Cu1 126.8(2) . . ?
O1 C1 O1 127.1(4) . 10_556 ?
O1 C1 C2 116.5(2) . . ?
O1 C1 C2 116.5(2) 10_556 . ?
C1 C2 S1 118.98(15) . . ?
C1 C2 S1 118.98(15) . 6_566 ?
C3 C2 C1 128.7(4) . . ?
C3 C2 C1 128.7(4) 6_566 . ?
C3 C2 C3 102.6(8) . 6_566 ?
C3 C2 S1 9.7(4) . 6_566 ?
C3 C2 S1 9.7(4) 6_566 . ?
C3 C2 S1 112.3(4) . . ?
C3 C2 S1 112.3(4) 6_566 6_566 ?
S1 C2 S1 122.0(3) 6_566 . ?
C2 C3 H3 123.7 . . ?
C2 C3 C4 112.6(6) . . ?
C4 C3 H3 123.7 . . ?
C3 C4 C3 147.8(8) . 2_565 ?
C3 C4 S1 13.4(4) . 6_566 ?
C3 C4 S1 13.4(4) 2_565 9_566 ?
C3 C4 S1 134.4(4) . 9_566 ?
C3 C4 S1 134.4(4) 2_565 6_566 ?
C4 C4 C3 106.1(4) 9_566 . ?
C4 C4 C3 106.1(4) 9_566 2_565 ?
C4 C4 S1 119.48(17) 9_566 6_566 ?
C4 C4 S1 119.48(17) 9_566 9_566 ?
S1 C4 S1 121.0(3) 9_566 6_566 ?
C2 S1 H3 124.3(12) . 10_556 ?
C4 S1 C2 89.5(2) 9_566 . ?
C4 S1 H3 146.2(11) 9_566 10_556 ?
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 N1 2.057(4) . ?
Cu1 O1 2.019(2) . ?
Cu1 O1 2.019(2) 2_665 ?
Cu1 O1 2.019(2) 3_655 ?
Cu1 O1 2.019(2) 4_565 ?
N1 C1D 1.485(10) . ?
N1 C3D 1.484(9) . ?
N1 C5D 1.487(9) . ?
C1D H1DA 0.9700 . ?
C1D H1DB 0.9700 . ?
C1D C2D 1.5301(11) . ?
C2D H2D1 0.9700 . ?
C2D H2D2 0.9700 . ?
C3D H3DA 0.9700 . ?
C3D H3DB 0.9700 . ?
C3D C4D 1.5302(11) . ?
C4D H4D1 0.9700 . ?
C4D H4D2 0.9700 . ?
C5D H5DA 0.9700 . ?
C5D H5DB 0.9700 . ?
C5D C6D 1.5302(11) . ?
C6D H6D1 0.9700 . ?
C6D H6D2 0.9700 . ?
O1 C1 1.248(3) . ?
C1 C2 1.481(5) . ?
C2 C3 1.400(8) . ?
C2 C3 1.400(8) 6_566 ?
C2 S1 1.719(3) . ?
C2 S1 1.719(3) 6_566 ?
C3 H3 0.9300 . ?
C3 C4 1.455(9) . ?
C4 C4 1.378(9) 9_566 ?
C4 S1 1.655(4) 6_566 ?
C4 S1 1.655(4) 9_566 ?
