#------------------------------------------------------------------------------
#$Date: 2023-04-06 09:45:37 +0300 (Thu, 06 Apr 2023) $
#$Revision: 282451 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/70/8107042.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_8107042
loop_
_publ_author_name
'Ma, Fa-Xue'
'Zhao, Dan'
'Yang, Rui-Juan'
'Huang, Min'
_publ_section_title
;
 Crystal structure of
 poly-[tetraaquabis(μ8-benzene-1,2,4,5-tetracarboxylato-1κ3 O 4:O 6:O
 8:2κ4 O 2:O 2:O 5:O 5:3κ4 O 1:O 3:O 5:O
 7)(di-μ3-hydroxido)-pentazinc(II)] decahydrate, C20H34O32Zn5
;
_journal_issue                   3
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              897
_journal_page_last               899
_journal_paper_doi               10.1515/ncrs-2015-0310
_journal_volume                  231
_journal_year                    2016
_chemical_formula_sum            'C20 H34 O32 Zn5'
_chemical_formula_weight         1113.32
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_cell_angle_alpha                90
_cell_angle_beta                 113.2070(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4196(2)
_cell_length_b                   16.7276(4)
_cell_length_c                   15.4905(3)
_cell_measurement_reflns_used    257
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      21.69
_cell_measurement_theta_min      4.27
_cell_volume                     1767.00(7)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'SMART APEX II (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2014)'
_computing_publication_material  'SHELXTL (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 83.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker smart APEX II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            21372
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.323
_diffrn_reflns_theta_min         1.878
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.463
_exptl_absorpt_correction_T_max  0.791
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.092
_exptl_crystal_description       prism
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.064
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.0016(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         4391
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0503
_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)+(0.0744P)²+2.9609P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3084
_reflns_number_total             4391
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2015-0310_suppl.cif
_cod_data_source_block           a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               8107042
_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   0.544
_shelx_estimated_absorpt_t_max   0.846
_exptl_absorpt_special_details   .
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
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'
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 0.46318(8) 0.98302(3) 0.18370(4) 0.02065(17) Uani 1 1 d . . . . .
Zn2 Zn 0.0000 1.0000 0.0000 0.0216(2) Uani 1 2 d S . P . .
Zn3 Zn 0.28995(9) 0.87559(4) -0.02236(4) 0.02724(19) Uani 1 1 d . . . . .
C1 C 0.0663(8) 0.8401(3) 0.0948(4) 0.0325(13) Uani 1 1 d . . . . .
C2 C 0.0082(7) 0.7776(3) 0.1480(4) 0.0265(11) Uani 1 1 d . . . . .
C3 C 0.1326(7) 0.7131(3) 0.1842(4) 0.0265(11) Uani 1 1 d . . . . .
H3 H 0.2428 0.7079 0.1702 0.032 Uiso 1 1 calc R U . . .
C7 C -0.1623(7) 0.7835(3) 0.1652(4) 0.0267(11) Uani 1 1 d . . . . .
C4 C 0.0976(7) 0.6561(3) 0.2411(4) 0.0253(11) Uani 1 1 d . . . . .
C5 C -0.0734(7) 0.6614(3) 0.2583(4) 0.0236(11) Uani 1 1 d . . . . .
C6 C -0.2024(7) 0.7242(3) 0.2182(4) 0.0279(11) Uani 1 1 d . . . . .
H14 H -0.3191 0.7267 0.2271 0.033 Uiso 1 1 calc R U . . .
C8 C -0.3127(7) 0.8483(3) 0.1282(4) 0.0272(11) Uani 1 1 d . . . . .
C9 C -0.1303(7) 0.6014(3) 0.3149(4) 0.0236(11) Uani 1 1 d . . . . .
C10 C 0.2509(7) 0.5928(3) 0.2801(4) 0.0253(11) Uani 1 1 d . . . . .
O1 O 0.1938(7) 0.8190(3) 0.0645(4) 0.0564(14) Uani 1 1 d . . . . .
O2 O -0.0149(6) 0.9063(2) 0.0841(3) 0.0339(9) Uani 1 1 d . . . . .
O3 O -0.4210(6) 0.8467(3) 0.0421(3) 0.0402(10) Uani 1 1 d . . . . .
O4 O -0.3256(6) 0.8961(2) 0.1871(3) 0.0387(10) Uani 1 1 d . . . . .
O5 O -0.0074(5) 0.5846(2) 0.3950(3) 0.0337(9) Uani 1 1 d . . . . .
O6 O -0.2995(6) 0.5739(3) 0.2790(3) 0.0464(12) Uani 1 1 d . . . . .
O7 O 0.3439(6) 0.5850(2) 0.3668(3) 0.0362(10) Uani 1 1 d . . . . .
O8 O 0.2934(6) 0.5508(2) 0.2239(3) 0.0352(9) Uani 1 1 d . . . . .
O9 O 0.2991(5) 0.9844(2) 0.0439(3) 0.0261(8) Uani 1 1 d . . . . .
H9 H 0.3401 1.0302 0.0227 0.031 Uiso 1 1 d R U . . .
O10 O 0.3953(7) 0.9106(3) 0.2738(4) 0.0629(14) Uani 1 1 d . . . . .
O11 O 0.2718(10) 0.7472(4) -0.0722(5) 0.093(2) Uani 1 1 d . . . . .
H11A H 0.1736 0.7291 -0.1255 0.111 Uiso 1 1 d R U . . .
H11B H 0.2460 0.7267 -0.0242 0.111 Uiso 1 1 d R U . . .
O12 O 0.604(2) 0.7686(9) 0.3791(11) 0.227(6) Uani 1 1 d . . . . .
O13 O 0.049(3) 1.1547(10) 0.5577(13) 0.261(7) Uani 1 1 d . U . . .
O14 O -0.5592(16) 0.6019(6) 0.0671(6) 0.159(4) Uani 1 1 d . . . . .
H14A H -0.5063 0.5529 0.0871 0.191 Uiso 1 1 d R U . . .
H14B H -0.5204 0.6366 0.1171 0.191 Uiso 1 1 d R U . . .
O15 O 0.0793(10) 0.9304(5) 0.3214(5) 0.105(3) Uani 1 1 d . . . . .
H15A H -0.0511 0.9308 0.2825 0.126 Uiso 1 1 d R U . . .
H15B H 0.0997 0.9446 0.3820 0.126 Uiso 1 1 d R U . . .
H10B H 0.2697 0.9116 0.2678 0.126 Uiso 1 1 d R U . . .
H10A H 0.4757 0.8695 0.3068 0.126 Uiso 1 1 d R U . . .
H12B H 0.5980 0.8018 0.4268 0.147 Uiso 1 1 d R U . . .
H12A H 0.6839 0.7260 0.4043 0.168 Uiso 1 1 d R U . . .
H16A H 0.1746 1.0897 0.4800 0.168 Uiso 1 1 d R U . . .
H16B H 0.2197 1.0444 0.4140 0.168 Uiso 1 1 d R U . . .
H13B H -0.0755 1.1368 0.5322 0.168 Uiso 1 1 d R U . . .
H13A H 0.0916 1.2008 0.5973 0.168 Uiso 1 1 d R U . . .
O16 O 0.231(3) 1.0418(11) 0.4729(11) 0.250(7) Uani 1 1 d . U . . .
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'
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'
H H 0.0000 0.0000 '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
O9 Zn1 O10 121.87(19) . .
O9 Zn1 O4 99.26(15) . 1_655
O10 Zn1 O4 87.46(19) . 1_655
O9 Zn1 O8 134.82(15) . 2_655
O10 Zn1 O8 103.12(19) . 2_655
O4 Zn1 O8 85.75(16) 1_655 2_655
O9 Zn1 O6 96.54(15) . 2
O10 Zn1 O6 85.4(2) . 2
O4 Zn1 O6 164.14(16) 1_655 2
O8 Zn1 O6 82.13(16) 2_655 2
O9 Zn2 O9 180.0 3_575 .
O9 Zn2 O2 90.78(15) 3_575 3_575
O9 Zn2 O2 89.22(15) . 3_575
O9 Zn2 O2 89.22(15) 3_575 .
O9 Zn2 O2 90.78(15) . .
O2 Zn2 O2 180.0 3_575 .
O9 Zn2 O5 97.53(14) 3_575 4_575
O9 Zn2 O5 82.47(14) . 4_575
O2 Zn2 O5 90.78(16) 3_575 4_575
O2 Zn2 O5 89.22(16) . 4_575
O9 Zn2 O5 82.47(14) 3_575 2
O9 Zn2 O5 97.53(14) . 2
O2 Zn2 O5 89.22(16) 3_575 2
O2 Zn2 O5 90.78(16) . 2
O5 Zn2 O5 180.00(15) 4_575 2
O9 Zn2 Zn3 138.49(10) 3_575 .
O9 Zn2 Zn3 41.50(10) . .
O2 Zn2 Zn3 103.05(11) 3_575 .
O2 Zn2 Zn3 76.95(11) . .
O5 Zn2 Zn3 44.31(10) 4_575 .
O5 Zn2 Zn3 135.69(10) 2 .
O9 Zn2 Zn3 41.51(10) 3_575 3_575
O9 Zn2 Zn3 138.49(10) . 3_575
O2 Zn2 Zn3 76.95(11) 3_575 3_575
O2 Zn2 Zn3 103.05(11) . 3_575
O5 Zn2 Zn3 135.69(10) 4_575 3_575
O5 Zn2 Zn3 44.31(10) 2 3_575
Zn3 Zn2 Zn3 180.0 . 3_575
O1 Zn3 O7 166.4(2) . 4_575
O1 Zn3 O3 98.29(19) . 1_655
O7 Zn3 O3 88.36(17) 4_575 1_655
O1 Zn3 O9 91.88(18) . .
O7 Zn3 O9 98.95(16) 4_575 .
O3 Zn3 O9 98.21(16) 1_655 .
O1 Zn3 O5 89.60(18) . 4_575
O7 Zn3 O5 83.94(16) 4_575 4_575
O3 Zn3 O5 172.12(17) 1_655 4_575
O9 Zn3 O5 81.40(14) . 4_575
O1 Zn3 O11 78.0(2) . .
O7 Zn3 O11 91.4(2) 4_575 .
O3 Zn3 O11 81.5(2) 1_655 .
O9 Zn3 O11 169.6(2) . .
O5 Zn3 O11 100.3(2) 4_575 .
O1 Zn3 Zn2 78.18(12) . .
O7 Zn3 Zn2 104.70(12) 4_575 .
O3 Zn3 Zn2 138.24(12) 1_655 .
O9 Zn3 Zn2 41.22(10) . .
O5 Zn3 Zn2 43.46(9) 4_575 .
O11 Zn3 Zn2 136.12(19) . .
O2 C1 O1 126.6(5) . .
O2 C1 C2 117.9(5) . .
O1 C1 C2 115.5(5) . .
C3 C2 C7 119.1(5) . .
C3 C2 C1 118.5(5) . .
C7 C2 C1 122.4(5) . .
C2 C3 C4 122.0(5) . .
C2 C3 H3 119.0 . .
C4 C3 H3 119.0 . .
C6 C7 C2 118.9(5) . .
C6 C7 C8 116.1(4) . .
C2 C7 C8 125.0(5) . .
C3 C4 C5 119.2(5) . .
C3 C4 C10 116.1(4) . .
C5 C4 C10 124.8(4) . .
C6 C5 C4 118.5(5) . .
C6 C5 C9 117.7(4) . .
C4 C5 C9 123.7(4) . .
C7 C6 C5 122.2(5) . .
C7 C6 H14 118.9 . .
C5 C6 H14 118.9 . .
O4 C8 O3 126.1(5) . .
O4 C8 C7 116.5(5) . .
O3 C8 C7 117.2(5) . .
O6 C9 O5 125.0(5) . .
O6 C9 C5 117.0(4) . .
O5 C9 C5 118.0(4) . .
O8 C10 O7 120.3(5) . .
O8 C10 C4 118.4(5) . .
O7 C10 C4 121.1(5) . .
C1 O1 Zn3 129.7(4) . .
C1 O2 Zn2 128.1(4) . .
C8 O3 Zn3 128.7(4) . 1_455
C8 O4 Zn1 133.7(4) . 1_455
C9 O5 Zn2 134.0(3) . 2_545
C9 O5 Zn3 133.7(3) . 4_576
Zn2 O5 Zn3 92.23(14) 2_545 4_576
C9 O6 Zn1 135.6(4) . 2_545
C10 O7 Zn3 131.9(3) . 4_576
C10 O8 Zn1 102.2(3) . 2_645
Zn1 O9 Zn2 118.00(18) . .
Zn1 O9 Zn3 114.08(16) . .
Zn2 O9 Zn3 97.28(15) . .
Zn1 O9 H9 104.1 . .
Zn2 O9 H9 103.7 . .
Zn3 O9 H9 119.9 . .
Zn1 O10 H10B 116.2 . .
Zn1 O10 H10A 122.6 . .
H10B O10 H10A 119.2 . .
Zn3 O11 H11A 122.8 . .
Zn3 O11 H11B 94.7 . .
H11A O11 H11B 105.4 . .
H12B O12 H12A 110.4 . .
H13B O13 H13A 124.4 . .
H14A O14 H14B 109.3 . .
H15A O15 H15B 112.0 . .
H16A O16 H16B 102.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O9 2.023(4) .
Zn1 O10 2.054(5) .
Zn1 O4 2.123(4) 1_655
Zn1 O8 2.135(4) 2_655
Zn1 O6 2.162(4) 2
Zn2 O9 2.065(4) 3_575
Zn2 O9 2.065(4) .
Zn2 O2 2.068(4) 3_575
Zn2 O2 2.068(4) .
Zn2 O5 2.140(4) 4_575
Zn2 O5 2.140(4) 2
Zn2 Zn3 3.1091(6) .
Zn2 Zn3 3.1091(6) 3_575
Zn3 O1 1.993(4) .
Zn3 O7 2.021(4) 4_575
Zn3 O3 2.035(4) 1_655
Zn3 O9 2.077(4) .
Zn3 O5 2.173(4) 4_575
Zn3 O11 2.268(7) .
C1 O2 1.240(7) .
C1 O1 1.261(7) .
C1 C2 1.495(7) .
C2 C3 1.387(7) .
C2 C7 1.395(7) .
C3 C4 1.390(7) .
C3 H3 0.9300 .
C7 C6 1.392(7) .
C7 C8 1.499(7) .
C4 C5 1.399(7) .
C4 C10 1.495(7) .
C5 C6 1.393(7) .
C5 C9 1.497(7) .
C6 H14 0.9300 .
C8 O4 1.244(7) .
C8 O3 1.257(7) .
C9 O6 1.244(6) .
C9 O5 1.249(6) .
C10 O8 1.251(6) .
C10 O7 1.252(6) .
O3 Zn3 2.035(4) 1_455
O4 Zn1 2.123(4) 1_455
O5 Zn2 2.140(4) 2_545
O5 Zn3 2.173(4) 4_576
O6 Zn1 2.162(4) 2_545
O7 Zn3 2.021(4) 4_576
O8 Zn1 2.135(4) 2_645
O9 H9 0.9313 .
O10 H10B 0.9001 .
O10 H10A 0.9211 .
O11 H11A 0.9106 .
O11 H11B 0.9051 .
O12 H12B 0.9405 .
O12 H12A 0.9114 .
O13 H13B 0.9029 .
O13 H13A 0.9585 .
O14 H14A 0.9083 .
O14 H14B 0.9195 .
O15 H15A 0.9162 .
O15 H15B 0.9211 .
O16 H16A 0.9301 .
O16 H16B 0.8838 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9 O3 0.93 2.47 3.397(6) 175.4 3_575
O9 H9 O7 0.93 2.47 2.980(5) 114.5 2_655
O11 H11B O1 0.91 2.20 2.689(9) 113.2 .
O11 H11B O13 0.91 2.37 2.924(19) 119.3 2_545
O11 H11B O14 0.91 2.61 3.163(12) 119.7 1_655
O14 H14B O6 0.92 2.61 3.118(9) 115.2 .
O15 H15A O4 0.92 2.07 2.959(8) 162.3 .
O15 H15B O16 0.92 2.12 2.857(17) 136.3 .
O10 H10B O15 0.90 1.93 2.742(8) 149.9 .
O10 H10A O12 0.92 2.04 2.951(16) 168.7 .
O16 H16A O13 0.93 2.09 2.92(2) 147.0 .
O16 H16B O15 0.88 2.37 2.857(17) 115.1 .
O13 H13B O14 0.90 2.60 3.49(2) 169.5 2_455
O13 H13A O12 0.96 2.20 2.69(2) 110.4 3_676
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{dd67b5c3-b5d2-41f7-967c-2ed71d078d04} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{dd67b5c3-b5d2-41f7-967c-2ed71d078d04} '_publcif_info_datablock.publ_exptl'
{dd67b5c3-b5d2-41f7-967c-2ed71d078d04} '_geom_hbond_atom_site_label_D'
