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#$Date: 2016-03-26 19:31:59 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180438 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/07/7210783.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_7210783
loop_
_publ_author_name
'Xing, Feifei'
'Jia, Juan'
'Liu, Licong'
'Zhong, Lina'
'Shao, Min'
'Bai, Yue-ling'
'Zhao, Yongmei'
'Zhu, Shourong'
'He, Xiang'
'Li, Mingxing'
_publ_section_title
;
 Synthesis, structure and adsorption of coordination polymers constructed
 from 3,3′,5,5′-azobenzenetetracarboxylic acid and Zn ions
;
_journal_issue                   24
_journal_name_full               CrystEngComm
_journal_page_first              4970
_journal_paper_doi               10.1039/c3ce40174j
_journal_volume                  15
_journal_year                    2013
_chemical_formula_sum            'C42 H30 N8 O20 Zn3'
_chemical_formula_weight         1162.85
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                110.091(2)
_cell_angle_beta                 99.943(2)
_cell_angle_gamma                95.800(2)
_cell_formula_units_Z            1
_cell_length_a                   9.5593(13)
_cell_length_b                   10.2131(14)
_cell_length_c                   11.9424(16)
_cell_measurement_temperature    296(2)
_cell_volume                     1062.2(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_sigmaI/netI    0.1493
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6715
_diffrn_reflns_theta_full        27.53
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    1.778
_exptl_absorpt_correction_T_max  0.7763
_exptl_absorpt_correction_T_min  0.7175
_exptl_crystal_density_diffrn    1.818
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             588
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.076
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4712
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.1288
_refine_ls_R_factor_gt           0.0664
_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)+(0.0722P)²+0.0100P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1432
_refine_ls_wR_factor_ref         0.1712
_reflns_number_gt                2330
_reflns_number_total             4712
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ce40174j.txt
_cod_data_source_block           1
_cod_original_cell_volume        1062.2(2)
_cod_database_code               7210783
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Zn1 Zn 1.0000 0.0000 0.5000 0.0301(3) Uani 1 2 d S
Zn2 Zn 0.03414(8) 0.29728(8) 0.73249(7) 0.0308(2) Uani 1 1 d .
C1 C 0.7638(7) 0.1740(7) 0.5650(6) 0.0314(15) Uani 1 1 d .
C2 C 0.6068(7) 0.1694(6) 0.5188(6) 0.0277(14) Uani 1 1 d .
C3 C 0.5169(7) 0.2210(6) 0.5976(6) 0.0282(14) Uani 1 1 d .
H3 H 0.5555 0.2645 0.6812 0.034 Uiso 1 1 calc R
C4 C 0.3715(7) 0.2086(7) 0.5532(6) 0.0281(14) Uani 1 1 d .
C5 C 0.3154(7) 0.1487(8) 0.4278(6) 0.0410(18) Uani 1 1 d .
H5 H 0.2184 0.1443 0.3960 0.049 Uiso 1 1 calc R
C6 C 0.4055(8) 0.0961(9) 0.3515(6) 0.052(2) Uani 1 1 d .
C7 C 0.5491(8) 0.1023(8) 0.3939(6) 0.0451(19) Uani 1 1 d .
H7 H 0.6069 0.0626 0.3405 0.054 Uiso 1 1 calc R
C8 C 0.2743(7) 0.2554(7) 0.6405(6) 0.0301(15) Uani 1 1 d .
C9 C 0.2048(10) -0.0662(9) 0.0352(7) 0.065(3) Uani 1 1 d U
C10 C 0.1730(8) -0.2112(8) -0.0189(7) 0.046(2) Uani 1 1 d .
H10 H 0.1945 -0.2674 0.0265 0.055 Uiso 1 1 calc R
C11 C 0.1091(7) -0.2715(7) -0.1409(6) 0.0343(16) Uani 1 1 d .
C12 C 0.0770(7) -0.1854(7) -0.2066(6) 0.0328(16) Uani 1 1 d .
H12 H 0.0375 -0.2263 -0.2902 0.039 Uiso 1 1 calc R
C13 C 0.1029(7) -0.0400(7) -0.1493(6) 0.0324(16) Uani 1 1 d .
C14 C 0.1665(9) 0.0205(7) -0.0274(6) 0.049(2) Uani 1 1 d .
H14 H 0.1835 0.1183 0.0126 0.059 Uiso 1 1 calc R
C15 C 0.0761(7) -0.4317(7) -0.2060(7) 0.0386(17) Uani 1 1 d .
C16 C 0.0573(7) 0.0494(7) -0.2225(6) 0.0324(16) Uani 1 1 d .
C17 C 0.2717(10) 0.4273(9) 0.0728(9) 0.064(3) Uani 1 1 d .
H17 H 0.1903 0.4567 0.0409 0.076 Uiso 1 1 calc R
C18 C 0.2985(9) 0.4440(8) 0.1900(7) 0.055(2) Uani 1 1 d .
H18 H 0.2368 0.4842 0.2393 0.066 Uiso 1 1 calc R
C19 C 0.4214(9) 0.4002(8) 0.2383(8) 0.054(2) Uani 1 1 d .
C20 C 0.5092(10) 0.3399(10) 0.1617(10) 0.072(3) Uani 1 1 d .
H20 H 0.5914 0.3098 0.1912 0.086 Uiso 1 1 calc R
C21 C 0.4730(11) 0.3250(10) 0.0407(9) 0.073(3) Uani 1 1 d .
H21 H 0.5303 0.2831 -0.0123 0.088 Uiso 1 1 calc R
N3 N 0.3566(9) 0.3702(8) -0.0006(7) 0.076(2) Uani 1 1 d .
H3A H 0.3360 0.3623 -0.0759 0.091 Uiso 1 1 calc R
N4 N 0.4543(9) 0.4221(8) 0.3581(7) 0.081(2) Uani 1 1 d .
H4A H 0.5315 0.3984 0.3885 0.097 Uiso 1 1 calc R
H4B H 0.3981 0.4599 0.4043 0.097 Uiso 1 1 calc R
O1 O 0.8258(5) 0.0939(5) 0.4930(4) 0.0401(12) Uani 1 1 d .
O2 O 0.8231(5) 0.2594(5) 0.6720(4) 0.0412(12) Uani 1 1 d .
O3 O 0.1366(4) 0.2157(4) 0.5982(4) 0.0317(11) Uani 1 1 d .
O4 O 0.3267(5) 0.3293(5) 0.7487(4) 0.0498(14) Uani 1 1 d .
O5 O 0.0812(5) -0.5050(4) -0.1421(4) 0.0364(11) Uani 1 1 d .
O6 O 0.0425(6) -0.4834(5) -0.3209(4) 0.0511(14) Uani 1 1 d .
O7 O 0.0033(5) -0.0112(5) -0.3322(4) 0.0344(11) Uani 1 1 d .
O8 O 0.0790(5) 0.1825(5) -0.1646(4) 0.0382(12) Uani 1 1 d .
O1W O 0.2233(5) 0.5252(5) 0.5028(4) 0.094(2) Uani 1 1 d .
H1WA H 0.1851 0.5500 0.5645 0.113 Uiso 1 1 d R
H1WB H 0.1426 0.4957 0.4517 0.113 Uiso 1 1 d R
N2 N 0.3579(5) 0.0030(5) 0.2170(4) 0.091(3) Uani 1 1 d RU
N1 N 0.2443(5) 0.0272(5) 0.1774(4) 0.090(3) Uani 1 1 d RU
O9 O 0.4261(8) -0.0922(7) 0.1670(6) 0.089(2) Uiso 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'
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
O1 Zn1 O1 180.000(1) 2_756 .
O1 Zn1 O7 96.14(18) 2_756 2_655
O1 Zn1 O7 83.86(18) . 2_655
O1 Zn1 O7 83.86(18) 2_756 1_656
O1 Zn1 O7 96.14(18) . 1_656
O7 Zn1 O7 180.0(2) 2_655 1_656
O1 Zn1 O3 91.50(17) 2_756 1_655
O1 Zn1 O3 88.50(17) . 1_655
O7 Zn1 O3 92.74(16) 2_655 1_655
O7 Zn1 O3 87.26(16) 1_656 1_655
O1 Zn1 O3 88.50(17) 2_756 2_656
O1 Zn1 O3 91.50(17) . 2_656
O7 Zn1 O3 87.26(16) 2_655 2_656
O7 Zn1 O3 92.74(16) 1_656 2_656
O3 Zn1 O3 180.00(15) 1_655 2_656
O2 Zn2 O8 107.3(2) 1_455 1_556
O2 Zn2 O5 105.58(18) 1_455 1_566
O8 Zn2 O5 101.87(18) 1_556 1_566
O2 Zn2 O3 112.05(18) 1_455 .
O8 Zn2 O3 101.62(18) 1_556 .
O5 Zn2 O3 126.53(19) 1_566 .
O2 Zn2 C15 98.4(2) 1_455 1_566
O8 Zn2 C15 129.3(2) 1_556 1_566
O5 Zn2 C15 28.0(2) 1_566 1_566
O3 Zn2 C15 108.2(2) . 1_566
O1 C1 O2 125.3(6) . .
O1 C1 C2 116.6(6) . .
O2 C1 C2 118.1(6) . .
C3 C2 C7 119.8(6) . .
C3 C2 C1 121.9(6) . .
C7 C2 C1 118.2(6) . .
C4 C3 C2 120.7(6) . .
C4 C3 H3 119.6 . .
C2 C3 H3 119.6 . .
C3 C4 C5 119.4(6) . .
C3 C4 C8 119.9(6) . .
C5 C4 C8 120.7(6) . .
C6 C5 C4 119.0(6) . .
C6 C5 H5 120.5 . .
C4 C5 H5 120.5 . .
C7 C6 C5 122.6(7) . .
C7 C6 N2 110.9(6) . .
C5 C6 N2 125.6(6) . .
C6 C7 C2 118.4(6) . .
C6 C7 H7 120.8 . .
C2 C7 H7 120.8 . .
O4 C8 O3 122.2(6) . .
O4 C8 C4 119.9(6) . .
O3 C8 C4 118.0(6) . .
C10 C9 C14 122.2(7) . .
C10 C9 N1 127.5(7) . .
C14 C9 N1 108.0(6) . .
C11 C10 C9 118.8(7) . .
C11 C10 H10 120.6 . .
C9 C10 H10 120.6 . .
C10 C11 C12 119.6(6) . .
C10 C11 C15 120.8(6) . .
C12 C11 C15 119.6(6) . .
C13 C12 C11 120.8(6) . .
C13 C12 H12 119.6 . .
C11 C12 H12 119.6 . .
C14 C13 C12 119.7(6) . .
C14 C13 C16 121.2(6) . .
C12 C13 C16 119.0(6) . .
C13 C14 C9 118.8(7) . .
C13 C14 H14 120.6 . .
C9 C14 H14 120.6 . .
O5 C15 O6 123.1(7) . .
O5 C15 C11 117.7(6) . .
O6 C15 C11 119.1(7) . .
O5 C15 Zn2 49.5(3) . 1_544
O6 C15 Zn2 73.6(4) . 1_544
C11 C15 Zn2 167.2(5) . 1_544
O7 C16 O8 125.3(7) . .
O7 C16 C13 118.1(6) . .
O8 C16 C13 116.6(6) . .
N3 C17 C18 122.5(9) . .
N3 C17 H17 118.7 . .
C18 C17 H17 118.7 . .
C17 C18 C19 118.8(9) . .
C17 C18 H18 120.6 . .
C19 C18 H18 120.6 . .
N4 C19 C20 121.5(9) . .
N4 C19 C18 119.8(8) . .
C20 C19 C18 118.7(8) . .
C19 C20 C21 118.9(9) . .
C19 C20 H20 120.6 . .
C21 C20 H20 120.6 . .
N3 C21 C20 120.3(9) . .
N3 C21 H21 119.8 . .
C20 C21 H21 119.8 . .
C17 N3 C21 120.8(9) . .
C17 N3 H3A 119.6 . .
C21 N3 H3A 119.6 . .
C19 N4 H4A 120.0 . .
C19 N4 H4B 120.0 . .
H4A N4 H4B 120.0 . .
C1 O1 Zn1 138.6(4) . .
C1 O2 Zn2 121.5(4) . 1_655
C8 O3 Zn2 109.3(4) . .
C8 O3 Zn1 131.7(4) . 1_455
Zn2 O3 Zn1 100.66(18) . 1_455
C15 O5 Zn2 102.5(4) . 1_544
C16 O7 Zn1 143.5(5) . 1_454
C16 O8 Zn2 115.2(4) . 1_554
H1WA O1W H1WB 93.7 . .
N1 N2 O9 129.4(4) . .
N1 N2 C6 108.3(4) . .
O9 N2 C6 121.8(6) . .
N2 N1 C9 106.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zn1 O1 2.007(4) 2_756
Zn1 O1 2.007(4) .
Zn1 O7 2.041(4) 2_655
Zn1 O7 2.041(4) 1_656
Zn1 O3 2.247(4) 1_655
Zn1 O3 2.247(4) 2_656
Zn2 O2 1.972(4) 1_455
Zn2 O8 1.994(5) 1_556
Zn2 O5 2.008(4) 1_566
Zn2 O3 2.004(4) .
Zn2 C15 2.577(7) 1_566
C1 O1 1.245(7) .
C1 O2 1.264(7) .
C1 C2 1.496(9) .
C2 C3 1.390(8) .
C2 C7 1.392(9) .
C3 C4 1.376(8) .
C3 H3 0.9300 .
C4 C5 1.390(9) .
C4 C8 1.503(9) .
C5 C6 1.374(9) .
C5 H5 0.9300 .
C6 C7 1.366(9) .
C6 N2 1.518(8) .
C7 H7 0.9300 .
C8 O4 1.233(7) .
C8 O3 1.294(7) .
C9 C10 1.373(10) .
C9 C14 1.379(10) .
C9 N1 1.590(9) .
C10 C11 1.370(9) .
C10 H10 0.9300 .
C11 C12 1.388(9) .
C11 C15 1.523(9) .
C12 C13 1.380(8) .
C12 H12 0.9300 .
C13 C14 1.368(9) .
C13 C16 1.511(9) .
C14 H14 0.9300 .
C15 O5 1.238(8) .
C15 O6 1.258(8) .
C15 Zn2 2.577(7) 1_544
C16 O7 1.229(7) .
C16 O8 1.272(7) .
C17 N3 1.325(11) .
C17 C18 1.326(11) .
C17 H17 0.9300 .
C18 C19 1.402(10) .
C18 H18 0.9300 .
C19 N4 1.344(10) .
C19 C20 1.379(11) .
C20 C21 1.376(13) .
C20 H20 0.9300 .
C21 N3 1.329(11) .
C21 H21 0.9300 .
N3 H3A 0.8600 .
N4 H4A 0.8600 .
N4 H4B 0.8600 .
O2 Zn2 1.972(4) 1_655
O3 Zn1 2.247(4) 1_455
O5 Zn2 2.008(4) 1_544
O7 Zn1 2.041(4) 1_454
O8 Zn2 1.994(5) 1_554
O1W H1WA 0.8499 .
O1W H1WB 0.8501 .
N2 N1 1.1921 .
N2 O9 1.261(7) .
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
N3 H3A O4 0.86 1.99 2.835(9) 168.2 1_554
O1W H1WB O6 0.85 2.11 2.931(7) 162.4 2
O1W H1WA O6 0.85 2.17 2.963(7) 154.5 1_566
N4 H4B O1W 0.86 2.23 3.084(9) 170.0 .
N4 H4A O1W 0.86 2.38 3.136(9) 146.6 2_666
