#------------------------------------------------------------------------------
#$Date: 2024-07-05 20:46:46 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293222 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/32/7063225.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_7063225
loop_
_publ_author_name
'Zhang, Kuo'
'Pang, Jing-Jing'
'Lian, Xin'
'Song, Zi-Han'
'Yuan, Yue-Chao'
'Huang, Hongliang'
'Yao, Zhao-Quan'
'Xu, Jian'
_publ_section_title
;
 A pacs-type metal--organic framework with high adsorption capacity for
 inverse C2H6/C2H4 separation
;
_journal_issue                   23
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10577
_journal_page_last               10583
_journal_paper_doi               10.1039/D4NJ00605D
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C66 H39 N6 O13 Zn3'
_chemical_formula_sum            'C66 H39 N6 O13 Zn3'
_chemical_formula_weight         1320.14
_chemical_name_common            Zn-adc-tpt
_chemical_name_systematic        Zn-adc-tpt
_space_group_crystal_system      trigonal
_space_group_IT_number           163
_space_group_name_Hall           '-P 3 2c'
_space_group_name_H-M_alt        'P -3 1 c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2j5l4g
_audit_creation_date             2024-01-20
_audit_creation_method
;
Olex2 1.5-alpha
(compiled 2023.11.24 svn.r209d9fb2 for OlexSys, GUI svn.r6869)
;
_audit_update_record
;
2024-01-29 deposited with the CCDC.	2024-05-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   16.7370(2)
_cell_length_b                   16.7370(2)
_cell_length_c                   15.8689(3)
_cell_measurement_reflns_used    3772
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      74.6100
_cell_measurement_theta_min      4.1050
_cell_volume                     3849.75(10)
_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 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -30.00  -5.00   0.50    6.43    --    0.00 -22.00  59.00   50
  2  ω     80.00 187.00   0.50   25.73    --  101.30  19.00 -45.00  214
  3  ω     12.00 103.00   0.50   25.73    --  101.30 -43.00  41.00  182
  4  ω    -31.00  13.00   0.50    6.43    --    0.00  82.00-180.00   88
  5  ω    -33.00  37.00   0.50    6.43    --    0.00  82.00  30.00  140
  6  ω    115.00 141.00   0.50   25.73    --  101.30  82.00  90.00   52
  7  ω    163.00 191.00   0.50   25.73    --  101.30  82.00  90.00   56
  8  ω    136.00 177.00   0.50   25.73    --  101.30  82.00 150.00   82
  9  ω     82.00 123.00   0.50   25.73    --  101.30  82.00 150.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0269374000
_diffrn_orient_matrix_UB_12      -0.0091718000
_diffrn_orient_matrix_UB_13      -0.0938358000
_diffrn_orient_matrix_UB_21      0.0509858000
_diffrn_orient_matrix_UB_22      -0.0537463000
_diffrn_orient_matrix_UB_23      -0.0161908000
_diffrn_orient_matrix_UB_31      -0.0892877000
_diffrn_orient_matrix_UB_32      -0.0911648000
_diffrn_orient_matrix_UB_33      0.0191951000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            12862
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.855
_diffrn_reflns_theta_min         4.131
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49791
_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            yellow
_exptl_crystal_density_diffrn    1.139
_exptl_crystal_description       prism
_exptl_crystal_F_000             1342
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.519
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2633
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0815P)²+2.6535P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1373
_refine_ls_wR_factor_ref         0.1410
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2271
_reflns_number_total             2633
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4nj00605d2.cif
_cod_data_source_block           TPT-EN
_cod_depositor_comments
'Adding full bibliography for 7063225--7063226.cif.'
_cod_original_cell_volume        3849.75(12)
_cod_database_code               7063225
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Zn'
_chemical_oxdiff_usercomment     'C H O N Zn'
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N6(H6), C10(H10), C12(H12), C2(H2), C11(H11), C9(H9), C3(H3)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 2.361
_oxdiff_exptl_absorpt_empirical_full_min 0.569
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, 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
Zn16 Zn 0.26447(2) 0.73553(2) 0.250000 0.01950(18) Uani 1 2 d S T P . .
O7 O 0.18283(13) 0.66124(12) 0.35734(11) 0.0252(4) Uani 1 1 d . . . . .
O18 O 0.15755(12) 0.51865(12) 0.33151(12) 0.0258(4) Uani 1 1 d . . . . .
O20 O 0.333333 0.666667 0.250000 0.0442(15) Uani 1 6 d S T P . .
N15 N 0.19120(10) 0.80880(10) 0.250000 0.0243(7) Uani 1 2 d S T P . .
C4 C 0.14273(17) 0.57601(18) 0.36921(16) 0.0223(5) Uani 1 1 d . . . . .
C22 C 0.06835(18) 0.53706(17) 0.43643(16) 0.0232(5) Uani 1 1 d . . . . .
C24 C 0.09103(18) 0.51960(18) 0.51684(17) 0.0242(5) Uani 1 1 d . . . . .
C13 C -0.02128(18) 0.51856(18) 0.41899(17) 0.0257(6) Uani 1 1 d . . . . .
N6 N -0.04706(12) 0.9059(2) 0.250000 0.0580(14) Uani 1 2 d S T P . .
H6 H -0.077421 0.845159 0.250000 0.070 Uiso 1 2 calc R U P . .
C10 C 0.1826(2) 0.5394(2) 0.53757(19) 0.0330(7) Uani 1 1 d . . . . .
H10 H 0.229185 0.563631 0.495507 0.040 Uiso 1 1 calc R U . . .
C12 C 0.0470(2) 0.4653(2) 0.66224(19) 0.0347(7) Uani 1 1 d . . . . .
H12 H 0.001570 0.439543 0.705299 0.042 Uiso 1 1 calc R U . . .
C2 C 0.2035(2) 0.5242(3) 0.6160(2) 0.0446(8) Uani 1 1 d . . . . .
H2 H 0.264978 0.539246 0.628733 0.054 Uiso 1 1 calc R U . . .
C11 C 0.1346(2) 0.4858(3) 0.6795(2) 0.0474(9) Uani 1 1 d . . . . .
H11 H 0.149903 0.474588 0.734202 0.057 Uiso 1 1 calc R U . . .
C19 C 0.09584(14) 0.90416(14) 0.250000 0.0464(13) Uani 1 2 d S T P . .
C9 C 0.2345(2) 0.8992(2) 0.2586(3) 0.0448(9) Uani 1 1 d . . . . .
H9 H 0.299561 0.931053 0.266191 0.054 Uiso 1 1 calc R U . . .
C3 C 0.1897(2) 0.9500(2) 0.2572(3) 0.0557(11) Uani 1 1 d . . . . .
H3 H 0.223687 1.015363 0.261145 0.067 Uiso 1 1 calc R U . . .
C17 C 0.04459(16) 0.95541(16) 0.250000 0.0537(15) Uani 1 2 d S T P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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
O7 Zn16 O7 174.31(10) . 4_665 ?
O18 Zn16 O7 90.04(7) 3_565 . ?
O18 Zn16 O7 89.56(7) 3_565 4_665 ?
O18 Zn16 O7 90.04(7) 6_565 4_665 ?
O18 Zn16 O7 89.56(7) 6_565 . ?
O18 Zn16 O18 172.02(10) 6_565 3_565 ?
O20 Zn16 O7 92.84(5) . . ?
O20 Zn16 O7 92.84(5) . 4_665 ?
O20 Zn16 O18 93.99(5) . 3_565 ?
O20 Zn16 O18 93.99(5) . 6_565 ?
O20 Zn16 N15 180.0 . . ?
N15 Zn16 O7 87.16(5) . . ?
N15 Zn16 O7 87.16(5) . 4_665 ?
N15 Zn16 O18 86.01(5) . 3_565 ?
N15 Zn16 O18 86.01(5) . 6_565 ?
C4 O7 Zn16 127.08(16) . . ?
C4 O18 Zn16 134.55(17) . 2_665 ?
Zn16 O20 Zn16 120.0 . 2_665 ?
Zn16 O20 Zn16 120.0 2_665 3_565 ?
Zn16 O20 Zn16 120.0 . 3_565 ?
C9 N15 Zn16 121.16(17) . . ?
C9 N15 Zn16 121.16(17) 4_665 . ?
C9 N15 C9 117.7(3) . 4_665 ?
O7 C4 O18 127.0(2) . . ?
O7 C4 C22 117.0(2) . . ?
O18 C4 C22 116.1(2) . . ?
C24 C22 C4 118.7(2) . . ?
C13 C22 C4 121.0(2) . . ?
C13 C22 C24 120.4(2) . . ?
C22 C24 C13 119.5(2) . 7_566 ?
C22 C24 C10 122.0(2) . . ?
C10 C24 C13 118.5(2) . 7_566 ?
C22 C13 C24 120.1(3) . 7_566 ?
C22 C13 C12 121.9(3) . 7_566 ?
C12 C13 C24 118.0(3) 7_566 7_566 ?
C17 N6 H6 122.7 . . ?
C17 N6 H6 122.7 3_465 . ?
C17 N6 C17 114.6(4) . 3_465 ?
C24 C10 H10 119.5 . . ?
C2 C10 C24 121.1(3) . . ?
C2 C10 H10 119.5 . . ?
C13 C12 H12 119.2 7_566 . ?
C11 C12 C13 121.6(3) . 7_566 ?
C11 C12 H12 119.2 . . ?
C10 C2 H2 119.7 . . ?
C10 C2 C11 120.6(3) . . ?
C11 C2 H2 119.7 . . ?
C12 C11 C2 120.1(3) . . ?
C12 C11 H11 119.9 . . ?
C2 C11 H11 119.9 . . ?
C3 C19 C3 118.6(4) . 4_665 ?
C3 C19 C17 120.7(2) 4_665 . ?
C3 C19 C17 120.7(2) . . ?
N15 C9 H9 118.5 . . ?
N15 C9 C3 123.1(3) . . ?
C3 C9 H9 118.5 . . ?
C19 C3 C9 118.7(3) . . ?
C19 C3 H3 120.6 . . ?
C9 C3 H3 120.6 . . ?
N6 C17 N6 125.4(4) . 2_675 ?
N6 C17 C19 117.3(2) 2_675 . ?
N6 C17 C19 117.3(2) . . ?
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
Zn16 O7 2.1484(17) 4_665 ?
Zn16 O7 2.1484(17) . ?
Zn16 O18 2.1441(18) 6_565 ?
Zn16 O18 2.1441(18) 3_565 ?
Zn16 O20 1.9963(4) . ?
Zn16 N15 2.124(3) . ?
O7 C4 1.250(3) . ?
O18 C4 1.257(3) . ?
N15 C9 1.318(3) . ?
N15 C9 1.318(3) 4_665 ?
C4 C22 1.517(3) . ?
C22 C24 1.403(4) . ?
C22 C13 1.399(4) . ?
C24 C13 1.436(4) 7_566 ?
C24 C10 1.434(4) . ?
C13 C12 1.427(4) 7_566 ?
N6 H6 0.8800 . ?
N6 C17 1.330(3) . ?
N6 C17 1.330(3) 3_465 ?
C10 H10 0.9500 . ?
C10 C2 1.351(5) . ?
C12 H12 0.9500 . ?
C12 C11 1.357(5) . ?
C2 H2 0.9500 . ?
C2 C11 1.421(5) . ?
C11 H11 0.9500 . ?
C19 C3 1.366(4) 4_665 ?
C19 C3 1.366(4) . ?
C19 C17 1.486(6) . ?
C9 H9 0.9500 . ?
C9 C3 1.387(4) . ?
C3 H3 0.9500 . ?
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
Zn16 O7 C4 O18 17.0(4) . . . . ?
Zn16 O7 C4 C22 -163.20(17) . . . . ?
Zn16 O18 C4 O7 13.0(4) 2_665 . . . ?
Zn16 O18 C4 C22 -166.75(17) 2_665 . . . ?
Zn16 N15 C9 C3 178.6(3) . . . . ?
O7 C4 C22 C24 -98.1(3) . . . . ?
O7 C4 C22 C13 82.0(3) . . . . ?
O18 C4 C22 C24 81.7(3) . . . . ?
O18 C4 C22 C13 -98.2(3) . . . . ?
N15 C9 C3 C19 2.8(6) . . . . ?
C4 C22 C24 C13 -179.1(2) . . . 7_566 ?
C4 C22 C24 C10 1.4(4) . . . . ?
C4 C22 C13 C24 179.1(2) . . . 7_566 ?
C4 C22 C13 C12 0.4(4) . . . 7_566 ?
C22 C24 C10 C2 178.4(3) . . . . ?
C24 C22 C13 C24 -0.8(4) . . . 7_566 ?
C24 C22 C13 C12 -179.4(3) . . . 7_566 ?
C24 C10 C2 C11 1.6(6) . . . . ?
C13 C22 C24 C13 0.8(4) . . . 7_566 ?
C13 C22 C24 C10 -178.7(3) . . . . ?
C13 C24 C10 C2 -1.1(5) 7_566 . . . ?
C13 C12 C11 C2 -0.2(6) 7_566 . . . ?
C10 C2 C11 C12 -0.9(6) . . . . ?
C9 N15 C9 C3 -1.4(3) 4_665 . . . ?
C3 C19 C3 C9 -1.3(3) 4_665 . . . ?
C3 C19 C17 N6 -174.4(2) . . . . ?
C3 C19 C17 N6 5.6(2) . . . 2_675 ?
C3 C19 C17 N6 5.6(2) 4_665 . . . ?
C3 C19 C17 N6 -174.4(2) 4_665 . . 2_675 ?
C17 N6 C17 N6 0.0 3_465 . . 2_675 ?
C17 N6 C17 C19 180.0 3_465 . . . ?
C17 C19 C3 C9 178.7(3) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.066 1539.2 403.5 ?
2 0.333 0.667 0.750 13.4 0.0 ?
3 0.667 0.333 0.250 13.4 0.0 ?
