#------------------------------------------------------------------------------
#$Date: 2025-03-04 21:59:09 +0200 (Tue, 04 Mar 2025) $
#$Revision: 298234 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/73/7717347.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_7717347
loop_
_publ_author_name
'Xie, Hui-Hui'
'Yu, Hao'
'Xu, Xiuling'
'Tang, Si-Fu'
_publ_section_title
;
 Rational fabrication of an anionic zinc carboxylate framework as a
 fluorescent probe for 2,6-pyridinedicarboxylic acid.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              159
_journal_page_last               165
_journal_paper_doi               10.1039/d4dt02529f
_journal_volume                  54
_journal_year                    2024
_chemical_formula_sum            'C56 H48 N4 O24 Zn5'
_chemical_formula_weight         1487.83
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2024-08-14 deposited with the CCDC.	2024-10-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.473(3)
_cell_length_b                   25.935(3)
_cell_length_c                   10.4545(19)
_cell_measurement_reflns_used    22293
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.441
_cell_measurement_theta_min      2.305
_cell_volume                     5822.1(15)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0768
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            32268
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.441
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    2.118
_exptl_absorpt_correction_T_max  0.9000
_exptl_absorpt_correction_T_min  0.673
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       block
_exptl_crystal_F_000             3016
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.215
_refine_diff_density_min         -1.009
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         3070
_refine_ls_number_restraints     47
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0858
_refine_ls_R_factor_gt           0.0659
_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)+(0.0854P)²+74.8320P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1683
_refine_ls_wR_factor_ref         0.1861
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2384
_reflns_number_total             3070
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt02529f2.cif
_cod_data_source_block           2
_cod_depositor_comments          'Adding full bibliography for 7717347.cif.'
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_original_sg_symbol_H-M      'C m c a'
_cod_database_code               7717347
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y+1/2, z+1/2'
'x, -y, -z'
'-x, y+1/2, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z'
'-x+1/2, y+1, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z-1/2'
'-x, y, z'
'x, -y-1/2, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y, -z-1/2'
'-x+1/2, y+1/2, z'
'x+1/2, -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
Zn1 Zn 0.07512(3) 0.45163(2) 1.26054(7) 0.0310(2) Uani 1 1 d . . . . .
Zn2 Zn 0.0000 0.0000 1.5000 0.0281(3) Uani 1 4 d S T P . .
N2 N 0.2255(4) 0.5000 1.5000 0.057(2) Uani 1 2 d S T P . .
H0A H 0.1991 0.5205 1.5540 0.068 Uiso 0.5 1 d R U P . .
O1 O 0.1306(2) 0.39608(19) 1.2091(5) 0.0507(12) Uani 1 1 d . . . . .
O2 O 0.1970(4) 0.4249(3) 1.3446(8) 0.108(2) Uani 1 1 d . U . . .
O3 O 0.0998(2) 0.02320(15) 1.2286(4) 0.0410(10) Uani 1 1 d . . . . .
O4 O 0.0666(3) 0.0466(2) 1.4183(6) 0.0768(17) Uani 1 1 d . U . . .
O5 O 0.0000 0.44680(19) 1.1529(6) 0.0298(12) Uani 1 2 d S T P . .
H5A H -0.0071 0.4153 1.1357 0.045 Uiso 0.5 1 d R U P . .
O6 O 0.0515(2) 0.4341(2) 1.4376(5) 0.0542(12) Uani 1 1 d . . . . .
C1 C 0.1803(3) 0.3933(2) 1.2691(7) 0.0399(15) Uani 1 1 d . . . . .
C2 C 0.2175(3) 0.3450(2) 1.2550(5) 0.0275(11) Uani 1 1 d . . . . .
C3 C 0.1866(3) 0.2980(2) 1.2633(6) 0.0311(12) Uani 1 1 d . . . . .
H3A H 0.1436 0.2980 1.2732 0.037 Uiso 1 1 calc R U . . .
C4 C 0.2175(3) 0.2512(2) 1.2574(5) 0.0295(11) Uani 1 1 d . . . . .
C5 C 0.1824(3) 0.2018(2) 1.2696(6) 0.0331(13) Uani 1 1 d . . . . .
C6 C 0.1719(3) 0.1701(2) 1.1640(6) 0.0393(14) Uani 1 1 d . . . . .
H6A H 0.1855 0.1804 1.0835 0.047 Uiso 1 1 calc R U . . .
C7 C 0.1413(3) 0.1234(2) 1.1782(6) 0.0392(14) Uani 1 1 d . . . . .
H7A H 0.1349 0.1022 1.1075 0.047 Uiso 1 1 calc R U . . .
C8 C 0.1202(3) 0.1082(2) 1.2973(6) 0.0369(14) Uani 1 1 d . . . . .
C9 C 0.1282(4) 0.1406(2) 1.4012(7) 0.0491(18) Uani 1 1 d . . . . .
H9A H 0.1129 0.1311 1.4809 0.059 Uiso 1 1 calc R U . . .
C10 C 0.1591(3) 0.1872(2) 1.3869(7) 0.0464(16) Uani 1 1 d . . . . .
H10A H 0.1641 0.2089 1.4571 0.056 Uiso 1 1 calc R U . . .
C11 C 0.0924(3) 0.0559(2) 1.3171(7) 0.0403(14) Uani 1 1 d . . . . .
C15 C 0.0000 0.4296(4) 1.4885(10) 0.049(2) Uani 1 2 d S T P . .
H15A H 0.0000 0.4220 1.5754 0.059 Uiso 1 2 calc R U P . .
C16 C 0.2639(5) 0.4663(4) 1.5789(10) 0.078(3) Uiso 1 1 d . . . . .
H16A H 0.2376 0.4445 1.6298 0.117 Uiso 1 1 calc R U . . .
H16B H 0.2897 0.4454 1.5248 0.117 Uiso 1 1 calc R U . . .
H16C H 0.2897 0.4868 1.6339 0.117 Uiso 1 1 calc R U . . .
O7 O 0.0000 0.3392(5) 1.1290(13) 0.116(4) Uani 1 2 d S TU P . .
N1 N 0.0000 0.2497(12) 1.077(3) 0.248(13) Uani 1 2 d DS TU P . .
C14 C 0.0000 0.3056(11) 1.053(4) 0.231(17) Uani 1 2 d DS TU P . .
H14A H 0.0000 0.3157 0.9675 0.277 Uiso 1 2 calc R U P . .
C13 C 0.0000 0.2369(15) 1.212(3) 0.250(18) Uani 1 2 d DS TU P . .
H13A H 0.0000 0.2670 1.2656 0.375 Uiso 1 2 d R U P . .
H13B H -0.0365 0.2167 1.2297 0.375 Uiso 0.5 1 d R U P . .
C12 C 0.0000 0.2199(16) 0.957(4) 0.39(4) Uani 1 2 d DS TU P . .
H12A H 0.0000 0.1856 0.9911 0.587 Uiso 1 2 d R U P . .
H12B H -0.0365 0.2249 0.9055 0.587 Uiso 0.5 1 d R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
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
O3 Zn1 O1 124.0(2) 10_568 . ?
O3 Zn1 O5 108.6(2) 10_568 . ?
O1 Zn1 O5 107.2(2) . . ?
O3 Zn1 O6 103.7(2) 10_568 . ?
O1 Zn1 O6 104.2(2) . . ?
O5 Zn1 O6 108.1(2) . . ?
O4 Zn2 O4 92.0(4) 9_558 11 ?
O4 Zn2 O4 88.0(4) 9_558 3_558 ?
O4 Zn2 O4 180.0 11 3_558 ?
O4 Zn2 O4 180.0(3) 9_558 . ?
O4 Zn2 O4 88.0(4) 11 . ?
O4 Zn2 O4 92.0(4) 3_558 . ?
O4 Zn2 O5 86.0(2) 9_558 10_558 ?
O4 Zn2 O5 94.0(2) 11 10_558 ?
O4 Zn2 O5 86.0(2) 3_558 10_558 ?
O4 Zn2 O5 94.0(2) . 10_558 ?
O4 Zn2 O5 94.0(2) 9_558 2 ?
O4 Zn2 O5 86.0(2) 11 2 ?
O4 Zn2 O5 94.0(2) 3_558 2 ?
O4 Zn2 O5 86.0(2) . 2 ?
O5 Zn2 O5 180.0 10_558 2 ?
C16 N2 C16 111.1(10) . 3_568 ?
C16 N2 H0A 109.4 . . ?
C16 N2 H0A 109.5 3_568 . ?
C1 O1 Zn1 115.5(4) . . ?
C11 O3 Zn1 124.5(4) . 10_558 ?
C11 O4 Zn2 142.3(5) . . ?
Zn1 O5 Zn1 109.9(3) 11 . ?
Zn1 O5 Zn2 112.99(16) 11 2_554 ?
Zn1 O5 Zn2 112.99(16) . 2_554 ?
Zn1 O5 H5A 92.1 11 . ?
Zn1 O5 H5A 109.2 . . ?
Zn2 O5 H5A 117.9 2_554 . ?
C15 O6 Zn1 131.0(6) . . ?
O2 C1 O1 123.7(7) . . ?
O2 C1 C2 118.8(7) . . ?
O1 C1 C2 117.2(5) . . ?
C3 C2 C2 118.7(3) . 8_547 ?
C3 C2 C1 118.4(5) . . ?
C2 C2 C1 122.7(3) 8_547 . ?
C4 C3 C2 122.5(5) . . ?
C4 C3 H3A 118.8 . . ?
C2 C3 H3A 118.8 . . ?
C3 C4 C4 118.8(3) . 8_547 ?
C3 C4 C5 120.5(5) . . ?
C4 C4 C5 120.7(3) 8_547 . ?
C10 C5 C6 119.0(5) . . ?
C10 C5 C4 119.6(5) . . ?
C6 C5 C4 121.4(5) . . ?
C7 C6 C5 120.5(6) . . ?
C7 C6 H6A 119.8 . . ?
C5 C6 H6A 119.8 . . ?
C8 C7 C6 120.0(6) . . ?
C8 C7 H7A 120.0 . . ?
C6 C7 H7A 120.0 . . ?
C7 C8 C9 119.6(5) . . ?
C7 C8 C11 120.8(6) . . ?
C9 C8 C11 119.5(6) . . ?
C8 C9 C10 120.3(6) . . ?
C8 C9 H9A 119.8 . . ?
C10 C9 H9A 119.8 . . ?
C5 C10 C9 120.5(6) . . ?
C5 C10 H10A 119.7 . . ?
C9 C10 H10A 119.7 . . ?
O4 C11 O3 124.1(6) . . ?
O4 C11 C8 118.7(6) . . ?
O3 C11 C8 117.2(6) . . ?
O6 C15 O6 127.7(10) 11 . ?
O6 C15 H15A 116.2 11 . ?
O6 C15 H15A 116.2 . . ?
N2 C16 H16A 109.5 . . ?
N2 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N2 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C13 N1 C12 135(3) . . ?
C13 N1 C14 113.0(18) . . ?
C12 N1 C14 111.9(19) . . ?
O7 C14 N1 128(3) . . ?
O7 C14 H14A 116.1 . . ?
N1 C14 H14A 116.1 . . ?
N1 C13 H13A 112.3 . . ?
N1 C13 H13B 108.1 . . ?
H13A C13 H13B 109.5 . . ?
N1 C12 H12A 99.9 . . ?
N1 C12 H12B 114.0 . . ?
H12A C12 H12B 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
Zn1 O3 1.933(4) 10_568 ?
Zn1 O1 1.946(5) . ?
Zn1 O5 1.971(3) . ?
Zn1 O6 1.973(5) . ?
Zn2 O4 2.059(6) 9_558 ?
Zn2 O4 2.059(6) 11 ?
Zn2 O4 2.059(6) 3_558 ?
Zn2 O4 2.059(6) . ?
Zn2 O5 2.112(5) 10_558 ?
Zn2 O5 2.112(5) 2 ?
N2 C16 1.457(11) . ?
N2 C16 1.457(11) 3_568 ?
N2 H0A 0.9600 . ?
O1 C1 1.240(7) . ?
O2 C1 1.193(10) . ?
O3 C11 1.265(8) . ?
O3 Zn1 1.933(4) 10_558 ?
O4 C11 1.218(9) . ?
O5 Zn1 1.971(3) 11 ?
O5 Zn2 2.112(5) 2_554 ?
O5 H5A 0.8500 . ?
O6 C15 1.233(7) . ?
C1 C2 1.493(8) . ?
C2 C3 1.391(7) . ?
C2 C2 1.401(11) 8_547 ?
C3 C4 1.384(7) . ?
C3 H3A 0.9300 . ?
C4 C4 1.404(11) 8_547 ?
C4 C5 1.493(7) . ?
C5 C10 1.377(9) . ?
C5 C6 1.394(9) . ?
C6 C7 1.388(8) . ?
C6 H6A 0.9300 . ?
C7 C8 1.382(9) . ?
C7 H7A 0.9300 . ?
C8 C9 1.384(9) . ?
C8 C11 1.497(8) . ?
C9 C10 1.387(9) . ?
C9 H9A 0.9300 . ?
C10 H10A 0.9300 . ?
C15 O6 1.233(7) 11 ?
C15 H15A 0.9300 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
O7 C14 1.18(3) . ?
N1 C13 1.455(18) . ?
N1 C12 1.470(19) . ?
N1 C14 1.472(18) . ?
C14 H14A 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C12 H12A 0.9601 . ?
C12 H12B 0.9599 . ?
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 O1 C1 O2 -7.3(11) . . . . ?
Zn1 O1 C1 C2 166.2(4) . . . . ?
O2 C1 C2 C3 128.0(8) . . . . ?
O1 C1 C2 C3 -45.8(9) . . . . ?
O2 C1 C2 C2 -46.2(11) . . . 8_547 ?
O1 C1 C2 C2 140.0(8) . . . 8_547 ?
C2 C2 C3 C4 -2.4(10) 8_547 . . . ?
C1 C2 C3 C4 -176.9(6) . . . . ?
C2 C3 C4 C4 0.1(10) . . . 8_547 ?
C2 C3 C4 C5 178.7(5) . . . . ?
C3 C4 C5 C10 -72.5(8) . . . . ?
C4 C4 C5 C10 106.1(8) 8_547 . . . ?
C3 C4 C5 C6 106.6(7) . . . . ?
C4 C4 C5 C6 -74.8(9) 8_547 . . . ?
C10 C5 C6 C7 -3.4(10) . . . . ?
C4 C5 C6 C7 177.5(6) . . . . ?
C5 C6 C7 C8 0.9(10) . . . . ?
C6 C7 C8 C9 1.9(10) . . . . ?
C6 C7 C8 C11 -174.3(6) . . . . ?
C7 C8 C9 C10 -2.2(11) . . . . ?
C11 C8 C9 C10 174.0(7) . . . . ?
C6 C5 C10 C9 3.1(11) . . . . ?
C4 C5 C10 C9 -177.8(7) . . . . ?
C8 C9 C10 C5 -0.4(12) . . . . ?
Zn2 O4 C11 O3 -27.9(14) . . . . ?
Zn2 O4 C11 C8 155.4(7) . . . . ?
Zn1 O3 C11 O4 -2.9(10) 10_558 . . . ?
Zn1 O3 C11 C8 173.8(4) 10_558 . . . ?
C7 C8 C11 O4 -169.9(7) . . . . ?
C9 C8 C11 O4 14.0(10) . . . . ?
C7 C8 C11 O3 13.1(9) . . . . ?
C9 C8 C11 O3 -163.0(7) . . . . ?
Zn1 O6 C15 O6 2.0(17) . . . 11 ?
C13 N1 C14 O7 0.000(12) . . . . ?
C12 N1 C14 O7 180.000(11) . . . . ?
