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#$Date: 2022-09-25 02:52:24 +0300 (Sun, 25 Sep 2022) $
#$Revision: 278151 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/76/1567689.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_1567689
loop_
_publ_author_name
'Xu, Heng'
'Zhang, Le-Xi'
'Xing, Yue'
'Yin, Yanyan'
'Tang, Bo'
'Bie, Lijian'
_publ_section_title
;
 Self-assembled mononuclear complexes: open metal sites and inverse
 dimension-dependent catalytic activity for Knoevenagel condensation and
 CO2 cycloaddition
;
_journal_name_full               Nanoscale
_journal_paper_doi               10.1039/D2NR04103K
_journal_year                    2022
_chemical_formula_sum            'C17 H18 N2 O7 S Zn'
_chemical_formula_weight         459.76
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2021-12-26 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.0233(3)
_cell_length_b                   14.6001(2)
_cell_length_c                   16.6104(3)
_cell_measurement_reflns_used    9087
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      78.9350
_cell_measurement_theta_min      4.1650
_cell_volume                     3885.87(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa dual home/near'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_sigmaI/netI    0.0624
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            16468
_diffrn_reflns_theta_full        79.16
_diffrn_reflns_theta_max         79.16
_diffrn_reflns_theta_min         4.89
_exptl_absorpt_coefficient_mu    3.145
_exptl_absorpt_correction_T_max  0.5720
_exptl_absorpt_correction_T_min  0.3660
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.572
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1888
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.387
_refine_diff_density_min         -2.073
_refine_diff_density_rms         0.217
_refine_ls_extinction_coef       0.0252(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.099
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         4135
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.1053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1918P)²+7.4136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2829
_refine_ls_wR_factor_ref         0.2904
_reflns_number_gt                3735
_reflns_number_total             4135
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2nr04103k3.cif
_cod_data_source_block           Zn-TMA-2,2-bpy
_cod_original_cell_volume        3885.86(11)
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1567689
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.00649(4) 0.20294(4) 0.15341(4) 0.0311(4) Uani 1 1 d . . .
S1 S 0.16755(17) 0.33047(19) -0.03982(15) 0.0872(7) Uani 1 1 d U . .
O2 O -0.0328(2) 0.3266(2) 0.1947(2) 0.0389(8) Uani 1 1 d . . .
O4 O 0.1112(2) 0.2180(2) 0.2183(2) 0.0417(9) Uani 1 1 d . . .
O5 O -0.0630(2) 0.1185(2) 0.2170(3) 0.0506(10) Uani 1 1 d . . .
H5A H -0.0484 0.0635 0.2077 0.076 Uiso 1 1 d R . .
H5B H -0.1131 0.1215 0.2003 0.076 Uiso 1 1 d R . .
O3 O 0.2116(3) 0.3021(3) 0.2701(3) 0.0574(12) Uani 1 1 d . . .
C6 C 0.0160(3) 0.3920(3) 0.2094(3) 0.0313(9) Uani 1 1 d . . .
N7 N 0.0682(2) 0.1110(3) 0.0741(2) 0.0361(9) Uani 1 1 d . . .
C2 C 0.1222(3) 0.3780(3) 0.1008(3) 0.0375(10) Uani 1 1 d . . .
C7 C 0.1467(3) 0.2942(3) 0.2302(3) 0.0336(10) Uani 1 1 d . . .
O1 O -0.0093(2) 0.4659(3) 0.2369(3) 0.0537(11) Uani 1 1 d . . .
C13 C -0.0219(4) 0.1829(4) -0.0218(3) 0.0425(11) Uani 1 1 d . . .
C5 C 0.1095(3) 0.3806(3) 0.1908(3) 0.0322(9) Uani 1 1 d . . .
H5 H 0.1391 0.4341 0.2121 0.039 Uiso 1 1 calc R . .
N13 N -0.0505(3) 0.2303(3) 0.0417(3) 0.0425(10) Uani 1 1 d . . .
C8 C 0.1287(3) 0.0536(4) 0.0959(3) 0.0441(12) Uani 1 1 d . . .
H8 H 0.1424 0.0490 0.1501 0.053 Uiso 1 1 calc R . .
C4 C 0.1108(5) 0.4248(6) -0.0406(5) 0.0757(14) Uani 1 1 d DU . .
H4 H 0.0947 0.4589 -0.0852 0.091 Uiso 1 1 calc R . .
C17 C -0.1116(5) 0.2923(4) 0.0307(5) 0.0616(18) Uani 1 1 d . . .
H17 H -0.1323 0.3237 0.0751 0.074 Uiso 1 1 calc R . .
C12 C 0.0467(3) 0.1171(3) -0.0042(3) 0.0387(11) Uani 1 1 d . . .
C14 C -0.0533(5) 0.1953(5) -0.0980(4) 0.0650(18) Uani 1 1 d . . .
H14 H -0.0331 0.1611 -0.1410 0.078 Uiso 1 1 calc R . .
C11 C 0.0864(5) 0.0659(5) -0.0621(4) 0.0601(16) Uani 1 1 d . . .
H11 H 0.0710 0.0707 -0.1159 0.072 Uiso 1 1 calc R . .
C16 C -0.1444(5) 0.3107(5) -0.0439(6) 0.071(2) Uani 1 1 d . . .
H16 H -0.1847 0.3559 -0.0505 0.085 Uiso 1 1 calc R . .
C1 C 0.1651(4) 0.3130(4) 0.0600(5) 0.0566(12) Uani 1 1 d U . .
H1 H 0.1908 0.2634 0.0849 0.068 Uiso 1 1 calc R . .
C9 C 0.1720(4) 0.0003(4) 0.0407(4) 0.0572(16) Uani 1 1 d . . .
H9 H 0.2146 -0.0386 0.0576 0.069 Uiso 1 1 calc R . .
C10 C 0.1509(5) 0.0060(5) -0.0385(5) 0.0657(18) Uani 1 1 d . . .
H10 H 0.1788 -0.0293 -0.0766 0.079 Uiso 1 1 calc R . .
C15 C -0.1161(5) 0.2603(7) -0.1094(5) 0.082(3) Uani 1 1 d . . .
H15 H -0.1387 0.2698 -0.1603 0.099 Uiso 1 1 calc R . .
C3 C 0.0906(5) 0.4441(5) 0.0470(4) 0.0664(18) Uani 1 1 d D . .
H3 H 0.0600 0.4949 0.0636 0.080 Uiso 1 1 calc R . .
O6 O 0.2234(3) 0.6211(2) 0.2761(5) 0.094(2) Uani 1 1 d G . .
H6A H 0.2615 0.5811 0.2812 0.142 Uiso 1 1 d G . .
H6B H 0.2495 0.6714 0.2706 0.142 Uiso 1 1 d G . .
O7 O 0.1917(3) 0.9605(2) 0.2827(5) 0.0843(19) Uani 1 1 d G . .
H7A H 0.2057 0.9392 0.2371 0.127 Uiso 1 1 d G . .
H7B H 0.1441 0.9369 0.2919 0.127 Uiso 1 1 d G . .
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'
S S 0.3331 0.5567 '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
O5 Zn1 O4 104.68(17) . . ?
O5 Zn1 O2 101.52(15) . . ?
O4 Zn1 O2 88.89(14) . . ?
O5 Zn1 N13 110.24(18) . . ?
O4 Zn1 N13 144.61(17) . . ?
O2 Zn1 N13 89.67(16) . . ?
O5 Zn1 N7 101.56(17) . . ?
O4 Zn1 N7 90.76(15) . . ?
O2 Zn1 N7 156.22(16) . . ?
N13 Zn1 N7 77.03(17) . . ?
C4 S1 C1 97.0(4) . . ?
C6 O2 Zn1 123.2(3) . . ?
C7 O4 Zn1 123.8(3) . . ?
O1 C6 O2 121.9(4) . . ?
O1 C6 C5 119.1(4) . . ?
O2 C6 C5 118.9(4) . . ?
C8 N7 C12 119.3(4) . . ?
C8 N7 Zn1 124.6(3) . . ?
C12 N7 Zn1 115.9(3) . . ?
C1 C2 C3 110.2(6) . . ?
C1 C2 C5 125.6(5) . . ?
C3 C2 C5 124.3(5) . . ?
O3 C7 O4 122.9(4) . . ?
O3 C7 C5 118.4(4) . . ?
O4 C7 C5 118.6(4) . . ?
N13 C13 C14 122.0(6) . . ?
N13 C13 C12 115.5(4) . . ?
C14 C13 C12 122.5(6) . . ?
C2 C5 C6 109.4(4) . . ?
C2 C5 C7 110.4(4) . . ?
C6 C5 C7 112.4(4) . . ?
C13 N13 C17 119.3(5) . . ?
C13 N13 Zn1 116.5(4) . . ?
C17 N13 Zn1 124.2(5) . . ?
N7 C8 C9 122.6(5) . . ?
C3 C4 S1 105.4(6) . . ?
N13 C17 C16 122.2(7) . . ?
N7 C12 C11 121.4(5) . . ?
N7 C12 C13 114.9(4) . . ?
C11 C12 C13 123.7(5) . . ?
C13 C14 C15 118.6(7) . . ?
C12 C11 C10 118.8(6) . . ?
C17 C16 C15 118.6(7) . . ?
C2 C1 S1 113.6(5) . . ?
C10 C9 C8 118.6(6) . . ?
C9 C10 C11 119.3(6) . . ?
C16 C15 C14 119.3(7) . . ?
C2 C3 C4 113.8(6) . . ?
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 O5 1.968(4) . ?
Zn1 O4 2.006(4) . ?
Zn1 O2 2.031(3) . ?
Zn1 N13 2.107(4) . ?
Zn1 N7 2.124(4) . ?
S1 C4 1.650(9) . ?
S1 C1 1.678(8) . ?
O2 C6 1.259(5) . ?
O4 C7 1.266(6) . ?
O3 C7 1.238(6) . ?
C6 O1 1.239(6) . ?
C6 C5 1.540(6) . ?
N7 C8 1.332(6) . ?
N7 C12 1.348(6) . ?
C2 C1 1.354(8) . ?
C2 C3 1.410(8) . ?
C2 C5 1.509(7) . ?
C7 C5 1.541(6) . ?
C13 N13 1.343(8) . ?
C13 C14 1.373(8) . ?
C13 C12 1.488(8) . ?
N13 C17 1.344(7) . ?
C8 C9 1.388(8) . ?
C4 C3 1.516(10) . ?
C17 C16 1.372(11) . ?
C12 C11 1.376(8) . ?
C14 C15 1.396(11) . ?
C11 C10 1.410(10) . ?
C16 C15 1.390(14) . ?
C9 C10 1.360(11) . ?
