#------------------------------------------------------------------------------
#$Date: 2024-12-06 21:00:06 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296581 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/70/7717067.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_7717067
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            'C30 H38 N4 O12 S4 Zn2'
_chemical_formula_weight         905.62
_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-2018/3
_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                   12.588(4)
_cell_length_b                   12.588(4)
_cell_length_c                   9.604(3)
_cell_measurement_reflns_used    6611
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0
_cell_measurement_theta_min      3.2
_cell_volume                     1521.8(8)
_computing_cell_refinement       'XDS (Kabsch, 2010)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        'XDS (Kabsch, 2010)'
_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      100(2)
_diffrn_detector_area_resol_mean 12.4
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Rayonix SX-165 CCD'
_diffrn_measurement_method       'φ scan'
_diffrn_radiation_monochromator  'Double Crystal Monochromator'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.745
_diffrn_reflns_av_R_equivalents  0.0352
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7785
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        26.551
_diffrn_reflns_theta_max         30.997
_diffrn_reflns_theta_min         3.271
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.094
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XDS (Kabsch, 2010)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_description       plate
_exptl_crystal_F_000             466
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1244
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.269
_refine_ls_R_factor_all          0.0513
_refine_ls_R_factor_gt           0.0489
_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)+(0.0791P)²+0.7520P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1360
_refine_ls_wR_factor_ref         0.1373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1153
_reflns_number_total             1244
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02209b2.cif
_cod_data_source_block           fin146_sq
_cod_depositor_comments
'Adding full bibliography for 7717067--7717068.cif.'
_cod_original_cell_volume        1521.8(11)
_cod_database_code               7717067
_shelx_shelxl_version_number     2018/3
_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   0.898
_shelx_estimated_absorpt_t_max   0.947
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 0.65382(5) 0.0285(2) Uani 1 8 d DS T P A .
N1 N 0.500000 0.500000 0.8657(4) 0.0300(8) Uani 1 8 d DS TU P . .
C1D C 0.459(2) 0.6030(12) 0.9204(14) 0.030(4) Uani 0.0625 1 d D U P A -1
H1DA H 0.385901 0.614784 0.885929 0.036 Uiso 0.0625 1 calc R U P A -1
H1DB H 0.504226 0.661794 0.885881 0.036 Uiso 0.0625 1 calc R U P A -1
C2D C 0.459(2) 0.6030(12) 1.0797(14) 0.030(5) Uani 0.0625 1 d D U P A -1
H2D1 H 0.504307 0.661780 1.114104 0.036 Uiso 0.0625 1 calc R U P A -1
H2D2 H 0.385957 0.614834 1.114152 0.036 Uiso 0.0625 1 calc R U P A -1
C3D C 0.432(2) 0.4129(17) 0.9205(14) 0.032(4) Uani 0.0625 1 d D U P A -1
H3DA H 0.458661 0.343740 0.886218 0.038 Uiso 0.0625 1 calc R U P A -1
H3DB H 0.358345 0.422118 0.885976 0.038 Uiso 0.0625 1 calc R U P A -1
C4D C 0.432(2) 0.4129(17) 1.0799(14) 0.033(5) Uani 0.0625 1 d D U P A -1
H4D1 H 0.358121 0.422427 1.114175 0.039 Uiso 0.0625 1 calc R U P A -1
H4D2 H 0.458247 0.343765 1.114416 0.039 Uiso 0.0625 1 calc R U P A -1
C5D C 0.6100(11) 0.484(3) 0.9202(14) 0.030(4) Uani 0.0625 1 d D U P A -1
H5DA H 0.656497 0.542164 0.885828 0.037 Uiso 0.0625 1 calc R U P A -1
H5DB H 0.638682 0.416081 0.885563 0.037 Uiso 0.0625 1 calc R U P A -1
C6D C 0.6099(10) 0.484(3) 1.0795(14) 0.031(5) Uani 0.0625 1 d D U P A -1
H6D1 H 0.638389 0.415741 1.113818 0.037 Uiso 0.0625 1 calc R U P A -1
H6D2 H 0.656570 0.541750 1.114084 0.037 Uiso 0.0625 1 calc R U P A -1
O1 O 0.34235(18) 0.500000 0.6150(2) 0.0663(8) Uani 1 2 d S TU P . .
C1 C 0.2985(3) 0.500000 0.500000 0.0420(8) Uani 1 4 d S TU P A .
C2 C 0.1805(3) 0.500000 0.500000 0.0488(9) Uani 1 4 d DS TU P . .
C3 C 0.1120(6) 0.500000 0.3869(7) 0.0603(17) Uani 0.5 2 d DS TU P A .
H3 H 0.135115 0.500000 0.292796 0.072 Uiso 0.5 2 calc R U P . .
C4 C 0.000000 0.500000 0.4285(4) 0.0555(11) Uani 1 4 d DS TU P . .
S1 S 0.11378(18) 0.500000 0.65589(19) 0.0729(8) 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 0.0039 0.0019 'Calculated with ShelXle (H\"ubschle, 2011)'
H H 0.0000 0.0000 'Calculated with ShelXle (H\"ubschle, 2011)'
N N 0.0075 0.0038 'Calculated with ShelXle (H\"ubschle, 2011)'
O O 0.0128 0.0069 'Calculated with ShelXle (H\"ubschle, 2011)'
S S 0.1364 0.1381 'Calculated with ShelXle (H\"ubschle, 2011)'
Zn Zn 0.2618 1.5600 'Calculated with ShelXle (H\"ubschle, 2011)'
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 Zn1 Zn1 180.0 . 9_666 ?
O1 Zn1 Zn1 79.36(7) . 9_666 ?
O1 Zn1 Zn1 79.36(7) 2_665 9_666 ?
O1 Zn1 Zn1 79.36(7) 3_655 9_666 ?
O1 Zn1 Zn1 79.36(7) 4_565 9_666 ?
O1 Zn1 N1 100.64(7) . . ?
O1 Zn1 N1 100.64(7) 2_665 . ?
O1 Zn1 N1 100.64(7) 3_655 . ?
O1 Zn1 N1 100.64(7) 4_565 . ?
O1 Zn1 O1 88.05(2) 3_655 2_665 ?
O1 Zn1 O1 88.05(2) 4_565 . ?
O1 Zn1 O1 88.05(3) 3_655 . ?
O1 Zn1 O1 88.05(3) 4_565 2_665 ?
O1 Zn1 O1 158.72(13) 2_665 . ?
O1 Zn1 O1 158.72(13) 3_655 4_565 ?
C1D N1 Zn1 110.6(6) . . ?
C1D N1 C5D 108.1(7) . . ?
C3D N1 Zn1 110.7(6) . . ?
C3D N1 C1D 108.5(7) . . ?
C3D N1 C5D 108.3(7) . . ?
C5D N1 Zn1 110.5(6) . . ?
N1 C1D H1DA 109.5 . . ?
N1 C1D H1DB 109.5 . . ?
N1 C1D C2D 110.6(11) . . ?
H1DA C1D H1DB 108.1 . . ?
C2D C1D H1DA 109.5 . . ?
C2D C1D H1DB 109.5 . . ?
N1 C2D C1D 110.6(11) 5_657 . ?
N1 C2D H2D1 109.5 5_657 . ?
N1 C2D H2D2 109.5 5_657 . ?
C1D C2D H2D1 109.5 . . ?
C1D C2D H2D2 109.5 . . ?
H2D1 C2D H2D2 108.1 . . ?
N1 C3D H3DA 109.5 . . ?
N1 C3D H3DB 109.5 . . ?
N1 C3D C4D 110.8(11) . . ?
H3DA C3D H3DB 108.1 . . ?
C4D C3D H3DA 109.5 . . ?
C4D C3D H3DB 109.5 . . ?
N1 C4D C3D 110.5(11) 5_657 . ?
N1 C4D H4D1 109.5 5_657 . ?
N1 C4D H4D2 109.5 5_657 . ?
C3D C4D H4D1 109.5 . . ?
C3D C4D H4D2 109.5 . . ?
H4D1 C4D H4D2 108.1 . . ?
N1 C5D H5DA 109.6 . . ?
N1 C5D H5DB 109.6 . . ?
N1 C5D C6D 110.5(11) . . ?
H5DA C5D H5DB 108.1 . . ?
C6D C5D H5DA 109.6 . . ?
C6D C5D H5DB 109.6 . . ?
N1 C6D C5D 110.7(11) 5_657 . ?
N1 C6D H6D1 109.5 5_657 . ?
N1 C6D H6D2 109.5 5_657 . ?
C5D C6D H6D1 109.5 . . ?
C5D C6D H6D2 109.5 . . ?
H6D1 C6D H6D2 108.1 . . ?
C1 O1 Zn1 127.2(2) . . ?
O1 C1 O1 126.9(4) . 10_556 ?
O1 C1 C2 116.56(18) . . ?
O1 C1 C2 116.56(18) 10_556 . ?
C1 C2 S1 119.29(14) . . ?
C1 C2 S1 119.29(14) . 6_566 ?
C3 C2 C1 128.5(3) . . ?
C3 C2 C1 128.5(3) 6_566 . ?
C3 C2 C3 103.1(7) . 6_566 ?
C3 C2 S1 9.2(3) . 6_566 ?
C3 C2 S1 9.2(3) 6_566 . ?
C3 C2 S1 112.2(4) . . ?
C3 C2 S1 112.2(4) 6_566 6_566 ?
S1 C2 S1 121.4(3) 6_566 . ?
C2 C3 H3 123.7 . . ?
C2 C3 C4 112.6(5) . . ?
C4 C3 H3 123.7 . . ?
C3 C4 C3 148.4(6) . 2_565 ?
C3 C4 S1 13.7(3) . 6_566 ?
C3 C4 S1 13.7(3) 2_565 9_566 ?
C3 C4 S1 134.7(4) . 9_566 ?
C3 C4 S1 134.7(4) 2_565 6_566 ?
C4 C4 C3 105.8(3) 9_566 . ?
C4 C4 C3 105.8(3) 9_566 2_565 ?
C4 C4 S1 119.51(13) 9_566 6_566 ?
C4 C4 S1 119.51(13) 9_566 9_566 ?
S1 C4 S1 121.0(3) 9_566 6_566 ?
C2 S1 H3 122.1(9) . 10_556 ?
C4 S1 C2 89.78(19) 9_566 . ?
C4 S1 H3 148.1(9) 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
Zn1 Zn1 2.9545(13) 9_666 ?
Zn1 N1 2.035(4) . ?
Zn1 O1 2.019(2) . ?
Zn1 O1 2.019(2) 2_665 ?
Zn1 O1 2.019(2) 3_655 ?
Zn1 O1 2.019(2) 4_565 ?
N1 C1D 1.491(9) . ?
N1 C3D 1.488(9) . ?
N1 C5D 1.493(9) . ?
C1D H1DA 0.9900 . ?
C1D H1DB 0.9900 . ?
C1D C2D 1.5302(12) . ?
C2D H2D1 0.9900 . ?
C2D H2D2 0.9900 . ?
C3D H3DA 0.9900 . ?
C3D H3DB 0.9900 . ?
C3D C4D 1.5302(11) . ?
C4D H4D1 0.9900 . ?
C4D H4D2 0.9900 . ?
C5D H5DA 0.9900 . ?
C5D H5DB 0.9900 . ?
C5D C6D 1.5302(12) . ?
C6D H6D1 0.9900 . ?
C6D H6D2 0.9900 . ?
O1 C1 1.235(3) . ?
C1 C2 1.485(5) . ?
C2 C3 1.387(7) . ?
C2 C3 1.387(7) 6_566 ?
C2 S1 1.717(3) . ?
C2 S1 1.717(3) 6_566 ?
C3 H3 0.9500 . ?
C3 C4 1.465(7) . ?
C4 C4 1.373(8) 9_566 ?
C4 S1 1.646(3) 6_566 ?
C4 S1 1.646(3) 9_566 ?
