#------------------------------------------------------------------------------
#$Date: 2024-10-06 10:56:06 +0300 (Sun, 06 Oct 2024) $
#$Revision: 295246 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/69/7716939.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_7716939
loop_
_publ_author_name
'Gupta, Gajendra'
'Paul, Anup'
'Gupta, Ajay'
'Lee, Junseong'
'Lee, Chang Yeon'
_publ_section_title
;
 Removal of organic dyes from aqueous solution using a novel pyrene
 appended Zn(ii)-based metal--organic framework and its photocatalytic
 properties
;
_journal_issue                   37
_journal_name_full               'Dalton Transactions'
_journal_page_first              15732
_journal_page_last               15741
_journal_paper_doi               10.1039/D4DT01869A
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C52 H32 F6 N4 Si Zn, 4(C H Cl3)'
_chemical_formula_sum            'C56 H36 Cl12 F6 N4 Si Zn'
_chemical_formula_weight         1397.75
_space_group_crystal_system      tetragonal
_space_group_IT_number           142
_space_group_name_Hall           '-I 4bd 2c'
_space_group_name_H-M_alt        'I 41/a c d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-11-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6429)
;
_audit_update_record
;
2024-06-03 deposited with the CCDC.	2024-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.0983(6)
_cell_length_b                   28.0983(6)
_cell_length_c                   14.9330(3)
_cell_measurement_reflns_used    7490
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.512
_cell_measurement_theta_min      2.895
_cell_volume                     11789.8(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-1997  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3365
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            77527
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.731
_diffrn_reflns_theta_min         2.118
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.042
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5185
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/2 (Bruker,2014/2) was used for absorption correction.
wR2(int) was 0.1014 before and 0.0639 after correction.
The Ratio of minimum to maximum transmission is 0.6958.
The λ/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_description       block
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         2815
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.2037
_refine_ls_R_factor_gt           0.0785
_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)+(0.1214P)²+62.6277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2041
_refine_ls_wR_factor_ref         0.2773
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1088
_reflns_number_total             2815
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01869a2.cif
_cod_data_source_block           lcy03-5_pl
_cod_depositor_comments          'Adding full bibliography for 7716939.cif.'
_cod_original_cell_volume        11789.8(6)
_cod_original_sg_symbol_H-M      'I 41/a c d'
_cod_database_code               7716939
_shelxl_version_number           2014-3
_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_max   0.903
_shelx_estimated_absorpt_t_min   0.903
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Ternary CH refined with riding coordinates:
 C17(H17)
3.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C15(H15), C1(H1), C5(H5), C12(H12), C7(H7), C8(H8), C16(H16)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
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 0.0000 0.2500 0.1250 0.0225(5) Uani 1 4 d S T P . .
Si1 Si 0.0000 0.2500 -0.1250 0.0247(9) Uani 1 4 d S T P . .
F1 F 0.0000 0.2500 -0.0121(4) 0.0347(14) Uani 1 2 d S T P . .
F2 F 0.05894(15) 0.24354(18) -0.1244(5) 0.0438(13) Uani 1 1 d . . . . .
N1 N 0.0544(2) 0.1956(2) 0.1250 0.028(2) Uani 1 2 d S T P . .
N2 N -0.0537(2) 0.1963(2) 0.1250 0.026(2) Uani 1 2 d S T P . .
C14 C 0.3757(3) -0.1257(3) 0.1250 0.029(3) Uani 1 2 d S T P . .
C4 C 0.1619(3) 0.0881(3) 0.1250 0.026(3) Uani 1 2 d S T P . .
C2 C 0.0873(4) 0.1244(4) 0.0624(7) 0.039(3) Uani 1 1 d . . . . .
H2 H 0.0852 0.0994 0.0198 0.047 Uiso 1 1 calc R U . . .
C13 C 0.3385(3) -0.0885(3) 0.1250 0.034(3) Uani 1 2 d S T P . .
C15 C -0.0895(3) 0.1975(3) 0.0664(7) 0.031(2) Uani 1 1 d . . . . .
H15 H -0.0905 0.2227 0.0239 0.038 Uiso 1 1 calc R U . . .
C3 C 0.1245(3) 0.1255(3) 0.1250 0.035(3) Uani 1 2 d S T P . .
C1 C 0.0539(3) 0.1602(3) 0.0640(7) 0.031(2) Uani 1 1 d . . . . .
H1 H 0.0293 0.1600 0.0202 0.037 Uiso 1 1 calc R U . . .
C6 C 0.2450(3) 0.0666(3) 0.1310(8) 0.030(2) Uani 1 1 d . . . . .
C9 C 0.3171(3) -0.0054(3) 0.1314(8) 0.030(2) Uani 1 1 d . . . . .
C5 C 0.2093(3) 0.1014(3) 0.1336(7) 0.031(2) Uani 1 1 d . . . . .
H5 H 0.2175 0.1339 0.1412 0.038 Uiso 1 1 calc R U . . .
C12 C 0.3513(3) -0.0410(3) 0.1306(8) 0.031(2) Uani 1 1 d . . . . .
H12 H 0.3840 -0.0327 0.1340 0.038 Uiso 1 1 calc R U . . .
C10 C 0.2686(3) -0.0186(3) 0.1250 0.027(3) Uani 1 2 d S T P . .
C11 C 0.2325(3) 0.0175(3) 0.1250 0.029(3) Uani 1 2 d S T P . .
C7 C 0.2948(3) 0.0786(3) 0.1366(8) 0.040(3) Uani 1 1 d . . . . .
H7 H 0.3038 0.1111 0.1405 0.048 Uiso 1 1 calc R U . . .
C8 C 0.3292(3) 0.0447(3) 0.1362(8) 0.038(2) Uani 1 1 d . U . . .
H8 H 0.3617 0.0539 0.1393 0.046 Uiso 1 1 calc R U . . .
C16 C -0.1246(3) 0.1643(3) 0.0649(7) 0.032(2) Uani 1 1 d . . . . .
H16 H -0.1498 0.1671 0.0227 0.038 Uiso 1 1 calc R U . . .
Cl3 Cl -0.03647(11) 0.04269(12) 0.3728(3) 0.0832(11) Uani 1 1 d . . . . .
Cl1 Cl 0.04379(12) 0.07413(14) 0.4739(2) 0.0831(12) Uani 1 1 d . . . . .
C17 C 0.0118(3) 0.0826(4) 0.3750(9) 0.054(3) Uani 1 1 d . . . . .
H17 H -0.0005 0.1160 0.3731 0.065 Uiso 1 1 calc R U . . .
Cl2 Cl 0.04763(13) 0.07239(15) 0.2811(3) 0.0912(13) Uani 1 1 d . . . . .
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Si Si 0.0817 0.0704 '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
F1 Zn1 F1 180.0 14_444 . ?
F1 Zn1 N1 90.0 14_444 . ?
F1 Zn1 N1 90.0 . . ?
F1 Zn1 N1 90.0 . 11_454 ?
F1 Zn1 N1 90.0 14_444 11_454 ?
F1 Zn1 N2 90.0 14_444 11_454 ?
F1 Zn1 N2 90.0 . 11_454 ?
F1 Zn1 N2 90.0 14_444 . ?
F1 Zn1 N2 90.0 . . ?
N1 Zn1 N1 180.0(2) 11_454 . ?
N2 Zn1 N1 90.0 . 11_454 ?
N2 Zn1 N1 90.0 . . ?
N2 Zn1 N1 89.999(1) 11_454 . ?
N2 Zn1 N1 90.001(1) 11_454 11_454 ?
N2 Zn1 N2 180.0 11_454 . ?
F1 Si1 F1 180.0 . 18_565 ?
F2 Si1 F1 90.3(3) 28 . ?
F2 Si1 F1 90.3(3) . 18_565 ?
F2 Si1 F1 89.7(3) 11_454 . ?
F2 Si1 F1 90.3(3) 11_454 18_565 ?
F2 Si1 F1 89.7(3) . . ?
F2 Si1 F1 90.3(3) 18_565 . ?
F2 Si1 F1 89.7(3) 18_565 18_565 ?
F2 Si1 F1 89.7(3) 28 18_565 ?
F2 Si1 F2 90.002(4) 18_565 11_454 ?
F2 Si1 F2 90.004(4) 18_565 . ?
F2 Si1 F2 90.000(4) 28 . ?
F2 Si1 F2 179.4(6) 28 18_565 ?
F2 Si1 F2 90.002(4) 28 11_454 ?
F2 Si1 F2 179.4(6) 11_454 . ?
Si1 F1 Zn1 180.0 . . ?
C1 N1 Zn1 120.8(5) 8 . ?
C1 N1 Zn1 120.8(5) . . ?
C1 N1 C1 118.3(10) 8 . ?
C15 N2 Zn1 121.0(5) 14_444 . ?
C15 N2 Zn1 121.0(5) . . ?
C15 N2 C15 117.9(10) 14_444 . ?
C16 C14 C13 122.7(5) 26 . ?
C16 C14 C13 122.7(5) 23_655 . ?
C16 C14 C16 114.6(11) 23_655 26 ?
C5 C4 C3 119.2(5) . . ?
C5 C4 C3 119.2(5) 8 . ?
C5 C4 C5 121.5(10) . 8 ?
C3 C2 H2 120.6 . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C3 118.8(10) . . ?
C12 C13 C14 119.8(5) . . ?
C12 C13 C14 119.8(5) 8 . ?
C12 C13 C12 120.3(10) 8 . ?
N2 C15 H15 118.6 . . ?
N2 C15 C16 122.7(9) . . ?
C16 C15 H15 118.6 . . ?
C2 C3 C4 120.8(6) 8 . ?
C2 C3 C4 120.8(6) . . ?
C2 C3 C2 118.4(12) . 8 ?
N1 C1 C2 122.8(9) . . ?
N1 C1 H1 118.6 . . ?
C2 C1 H1 118.6 . . ?
C5 C6 C11 120.0(8) . . ?
C5 C6 C7 122.0(8) . . ?
C11 C6 C7 118.0(8) . . ?
C12 C9 C10 118.5(7) . . ?
C12 C9 C8 122.5(8) . . ?
C10 C9 C8 119.0(8) . . ?
C4 C5 C6 119.8(8) . . ?
C4 C5 H5 120.1 . . ?
C6 C5 H5 120.1 . . ?
C13 C12 C9 121.1(8) . . ?
C13 C12 H12 119.5 . . ?
C9 C12 H12 119.5 . . ?
C9 C10 C9 120.6(10) 8 . ?
C9 C10 C11 119.7(5) 8 . ?
C9 C10 C11 119.7(5) . . ?
C6 C11 C6 118.8(10) . 8 ?
C6 C11 C10 120.6(5) . . ?
C6 C11 C10 120.6(5) 8 . ?
C6 C7 H7 119.1 . . ?
C8 C7 C6 121.8(9) . . ?
C8 C7 H7 119.1 . . ?
C9 C8 H8 119.5 . . ?
C7 C8 C9 120.9(9) . . ?
C7 C8 H8 119.5 . . ?
C14 C16 H16 119.5 20_556 . ?
C15 C16 C14 121.0(9) . 20_556 ?
C15 C16 H16 119.5 . . ?
Cl3 C17 H17 109.3 . . ?
Cl1 C17 Cl3 109.0(7) . . ?
Cl1 C17 H17 109.3 . . ?
Cl1 C17 Cl2 111.1(6) . . ?
Cl2 C17 Cl3 108.9(7) . . ?
Cl2 C17 H17 109.3 . . ?
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 F1 2.048(6) 14_444 ?
Zn1 F1 2.048(6) . ?
Zn1 N1 2.163(9) 11_454 ?
Zn1 N1 2.163(9) . ?
Zn1 N2 2.133(8) 11_454 ?
Zn1 N2 2.134(8) . ?
Si1 F1 1.685(6) . ?
Si1 F1 1.685(6) 18_565 ?
Si1 F2 1.666(4) . ?
Si1 F2 1.666(4) 28 ?
Si1 F2 1.666(4) 18_565 ?
Si1 F2 1.666(4) 11_454 ?
N1 C1 1.348(10) 8 ?
N1 C1 1.348(10) . ?
N2 C15 1.335(10) 14_444 ?
N2 C15 1.335(10) . ?
C14 C13 1.479(15) . ?
C14 C16 1.407(10) 23_655 ?
C14 C16 1.407(10) 26 ?
C4 C3 1.484(14) . ?
C4 C5 1.389(9) 8 ?
C4 C5 1.389(9) . ?
C2 H2 0.9500 . ?
C2 C3 1.403(11) . ?
C2 C1 1.377(13) . ?
C13 C12 1.384(9) 8 ?
C13 C12 1.384(9) . ?
C15 H15 0.9500 . ?
C15 C16 1.358(12) . ?
C3 C2 1.403(11) 8 ?
C1 H1 0.9500 . ?
C6 C5 1.401(11) . ?
C6 C11 1.425(9) . ?
C6 C7 1.442(11) . ?
C9 C12 1.389(11) . ?
C9 C10 1.416(9) . ?
C9 C8 1.449(11) . ?
C5 H5 0.9500 . ?
C12 H12 0.9500 . ?
C10 C9 1.416(9) 8 ?
C10 C11 1.435(13) . ?
C11 C6 1.425(9) 8 ?
C7 H7 0.9500 . ?
C7 C8 1.358(10) . ?
C8 H8 0.9500 . ?
C16 C14 1.407(10) 20_556 ?
C16 H16 0.9500 . ?
Cl3 C17 1.760(9) . ?
Cl1 C17 1.745(13) . ?
C17 H17 1.0000 . ?
C17 Cl2 1.750(12) . ?
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
Zn1 N1 C1 C2 -178.9(7) . . . . ?
Zn1 N2 C15 C16 -179.3(7) . . . . ?
N2 C15 C16 C14 -1.5(14) . . . 20_556 ?
C14 C13 C12 C9 -179.6(9) . . . . ?
C15 N2 C15 C16 0.7(7) 14_444 . . . ?
C3 C4 C5 C6 -178.1(8) . . . . ?
C3 C2 C1 N1 -2.2(14) . . . . ?
C1 N1 C1 C2 1.1(7) 8 . . . ?
C1 C2 C3 C4 -179.0(7) . . . . ?
C1 C2 C3 C2 1.1(7) . . . 8 ?
C6 C7 C8 C9 -1(2) . . . . ?
C9 C10 C11 C6 0.2(10) 8 . . 8 ?
C9 C10 C11 C6 0.2(10) . . . . ?
C9 C10 C11 C6 -179.8(10) . . . 8 ?
C9 C10 C11 C6 -179.8(10) 8 . . . ?
C5 C4 C3 C2 135.3(7) . . . . ?
C5 C4 C3 C2 -44.7(7) 8 . . . ?
C5 C4 C3 C2 135.3(7) 8 . . 8 ?
C5 C4 C3 C2 -44.7(7) . . . 8 ?
C5 C4 C5 C6 1.9(8) 8 . . . ?
C5 C6 C11 C6 1.9(8) . . . 8 ?
C5 C6 C11 C10 -178.1(8) . . . . ?
C5 C6 C7 C8 178.4(12) . . . . ?
C12 C13 C12 C9 0.4(9) 8 . . . ?
C12 C9 C10 C9 0.4(9) . . . 8 ?
C12 C9 C10 C11 -179.6(9) . . . . ?
C12 C9 C8 C7 179.8(13) . . . . ?
C10 C9 C12 C13 -0.8(17) . . . . ?
C10 C9 C8 C7 1.3(19) . . . . ?
C11 C6 C5 C4 -3.7(16) . . . . ?
C11 C6 C7 C8 -0.1(19) . . . . ?
C7 C6 C5 C4 177.8(9) . . . . ?
C7 C6 C11 C6 -179.6(13) . . . 8 ?
C7 C6 C11 C10 0.4(13) . . . . ?
C8 C9 C12 C13 -179.4(10) . . . . ?
C8 C9 C10 C9 179.0(13) . . . 8 ?
C8 C9 C10 C11 -1.0(13) . . . . ?
C16 C14 C13 C12 -134.7(7) 23_655 . . . ?
C16 C14 C13 C12 -134.7(7) 26 . . 8 ?
C16 C14 C13 C12 45.3(7) 23_655 . . 8 ?
C16 C14 C13 C12 45.3(7) 26 . . . ?
