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#$Date: 2016-03-22 23:50:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179080 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/42/4304241.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_4304241
loop_
_publ_author_name
'Jing Wang'
'Zhuojia Lin'
'Yong-Cong Ou'
'Nai-Liang Yang'
'Yue-Hua Zhang'
'Ming-Liang Tong'
_publ_section_title
;
Hydrothermal Synthesis, Structures, and Photoluminescent Properties of
Benzenepentacarboxylate Bridged Networks Incorporating Zinc(II)-Hydroxide
Clusters or Zinc(II)-Carboxylate Layers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              190
_journal_page_last               199
_journal_paper_doi               10.1021/ic701721t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_sum            'C35 H22 N4 O12 Zn2'
_chemical_formula_weight         821.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.863(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.065(2)
_cell_length_b                   7.9324(9)
_cell_length_c                   19.605(2)
_cell_measurement_temperature    293(2)
_cell_volume                     3109.2(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0529
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5246
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.622
_exptl_absorpt_correction_T_max  0.7270
_exptl_absorpt_correction_T_min  0.6249
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedral
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.769
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         2951
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0619
_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)+(0.0809P)²+23.8968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1568
_refine_ls_wR_factor_ref         0.1658
_reflns_number_gt                2427
_reflns_number_total             2951
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701721t-file003.cif
_cod_data_source_block           compound3
_cod_original_cell_volume        3109.3(6)
_cod_database_code               4304241
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.09225(3) 0.88190(8) 0.07898(3) 0.0241(2) Uani 1 1 d D . .
O1W O 0.0185(2) 0.7910(5) 0.0106(2) 0.0372(10) Uani 1 1 d D . .
H1WA H 0.012(3) 0.829(6) -0.0289(15) 0.05(2) Uiso 1 1 d D . .
H1WB H 0.008(3) 0.687(3) 0.012(2) 0.05(2) Uiso 1 1 d D . .
O1 O 0.0680(3) 0.6981(6) 0.1454(2) 0.0516(13) Uani 1 1 d . . .
O2 O 0.0277(2) 0.4908(5) 0.07704(19) 0.0359(10) Uani 1 1 d . . .
O3 O 0.1270(2) 0.2219(6) 0.1449(2) 0.0388(10) Uani 1 1 d . . .
O4 O 0.03776(19) 0.0677(5) 0.1144(2) 0.0351(10) Uani 1 1 d . . .
O5 O -0.0561(3) -0.0670(9) 0.2418(4) 0.100(3) Uani 1 1 d D . .
H5O H -0.0596 -0.1357 0.2745 0.121 Uiso 0.50 1 d PRD . .
N2 N 0.1910(2) 0.8599(6) 0.1254(2) 0.0331(11) Uani 1 1 d . . .
N1 N 0.1493(2) 0.9726(6) -0.0003(2) 0.0299(11) Uani 1 1 d . . .
C1 C 0.1284(3) 1.0276(9) -0.0624(3) 0.0421(16) Uani 1 1 d . . .
H1 H 0.0828 1.0269 -0.0757 0.051 Uiso 1 1 calc R . .
C2 C 0.1724(4) 1.0864(11) -0.1085(3) 0.055(2) Uani 1 1 d . . .
H2 H 0.1560 1.1232 -0.1517 0.066 Uiso 1 1 calc R . .
C3 C 0.2385(4) 1.0897(10) -0.0904(4) 0.0524(19) Uani 1 1 d . . .
H3 H 0.2679 1.1292 -0.1210 0.063 Uiso 1 1 calc R . .
C4 C 0.2628(3) 1.0337(9) -0.0257(3) 0.0403(15) Uani 1 1 d . . .
C5 C 0.2160(3) 0.9747(7) 0.0185(3) 0.0297(12) Uani 1 1 d . . .
C6 C 0.2382(3) 0.9138(7) 0.0855(3) 0.0337(13) Uani 1 1 d . . .
C7 C 0.3067(3) 0.9133(9) 0.1069(4) 0.0462(16) Uani 1 1 d . . .
C8 C 0.3253(4) 0.8529(12) 0.1730(5) 0.069(2) Uani 1 1 d . . .
H8 H 0.3702 0.8479 0.1890 0.082 Uiso 1 1 calc R . .
C9 C 0.2776(4) 0.8019(13) 0.2133(4) 0.069(3) Uani 1 1 d . . .
H9 H 0.2894 0.7659 0.2579 0.083 Uiso 1 1 calc R . .
C10 C 0.2102(4) 0.8037(10) 0.1873(3) 0.0495(17) Uani 1 1 d . . .
H10 H 0.1780 0.7639 0.2147 0.059 Uiso 1 1 calc R . .
C11 C 0.3326(3) 1.0318(11) -0.0021(4) 0.057(2) Uani 1 1 d . . .
H11 H 0.3638 1.0719 -0.0306 0.068 Uiso 1 1 calc R . .
C12 C 0.3536(3) 0.9732(11) 0.0602(5) 0.061(2) Uani 1 1 d . . .
H12 H 0.3991 0.9710 0.0737 0.073 Uiso 1 1 calc R . .
C13 C 0.0000 0.5411(9) 0.2500 0.0270(16) Uani 1 2 d S . .
H13 H 0.0000 0.6583 0.2500 0.032 Uiso 1 2 calc SR . .
C14 C 0.0253(3) 0.4566(7) 0.1959(3) 0.0243(11) Uani 1 1 d . . .
C15 C 0.0287(2) 0.2807(6) 0.1981(2) 0.0223(11) Uani 1 1 d . . .
C16 C 0.0000 0.1928(9) 0.2500 0.0233(15) Uani 1 2 d S . .
C17 C 0.0427(3) 0.5535(7) 0.1339(3) 0.0278(12) Uani 1 1 d . . .
C18 C 0.0686(2) 0.1854(7) 0.1484(3) 0.0233(11) Uani 1 1 d . . .
C19 C 0.0000 0.0124(14) 0.2500 0.061(3) Uani 1 2 d S . .
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
O4 Zn1 O1 98.0(2) 1_565 . ?
O4 Zn1 O1W 95.81(17) 1_565 . ?
O1 Zn1 O1W 88.18(17) . . ?
O4 Zn1 N2 115.58(17) 1_565 . ?
O1 Zn1 N2 86.09(19) . . ?
O1W Zn1 N2 148.56(19) . . ?
O4 Zn1 N1 110.41(18) 1_565 . ?
O1 Zn1 N1 151.4(2) . . ?
O1W Zn1 N1 92.53(18) . . ?
N2 Zn1 N1 78.50(18) . . ?
Zn1 O1W H1WA 122(3) . . ?
Zn1 O1W H1WB 119(3) . . ?
H1WA O1W H1WB 111(3) . . ?
C17 O1 Zn1 130.3(4) . . ?
C18 O4 Zn1 117.8(3) . 1_545 ?
C19 O5 H5O 110.2 . . ?
C10 N2 C6 118.4(5) . . ?
C10 N2 Zn1 127.8(5) . . ?
C6 N2 Zn1 113.8(4) . . ?
C1 N1 C5 118.1(5) . . ?
C1 N1 Zn1 129.3(4) . . ?
C5 N1 Zn1 112.6(4) . . ?
N1 C1 C2 122.4(6) . . ?
N1 C1 H1 118.8 . . ?
C2 C1 H1 118.8 . . ?
C3 C2 C1 120.0(6) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C2 C3 C4 119.7(6) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C4 C5 117.7(6) . . ?
C3 C4 C11 123.6(6) . . ?
C5 C4 C11 118.7(6) . . ?
N1 C5 C4 122.0(5) . . ?
N1 C5 C6 117.9(5) . . ?
C4 C5 C6 120.2(5) . . ?
N2 C6 C7 123.0(6) . . ?
N2 C6 C5 117.3(5) . . ?
C7 C6 C5 119.6(6) . . ?
C6 C7 C8 117.0(7) . . ?
C6 C7 C12 118.9(6) . . ?
C8 C7 C12 124.1(7) . . ?
C9 C8 C7 119.8(7) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.4(7) . . ?
C8 C9 H9 120.3 . . ?
C10 C9 H9 120.3 . . ?
N2 C10 C9 122.3(7) . . ?
N2 C10 H10 118.8 . . ?
C9 C10 H10 118.8 . . ?
C12 C11 C4 121.3(6) . . ?
C12 C11 H11 119.4 . . ?
C4 C11 H11 119.4 . . ?
C11 C12 C7 121.2(6) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C14 C13 C14 122.2(7) . 2 ?
C14 C13 H13 118.9 . . ?
C14 C13 H13 118.9 2 . ?
C13 C14 C15 118.6(5) . . ?
C13 C14 C17 119.7(5) . . ?
C15 C14 C17 121.4(5) . . ?
C14 C15 C16 119.9(5) . . ?
C14 C15 C18 120.4(5) . . ?
C16 C15 C18 119.5(5) . . ?
C15 C16 C15 120.1(7) . 2 ?
C15 C16 C19 119.9(3) . . ?
C15 C16 C19 119.9(3) 2 . ?
O2 C17 O1 126.1(5) . . ?
O2 C17 C14 117.9(5) . . ?
O1 C17 C14 115.9(5) . . ?
O3 C18 O4 124.9(5) . . ?
O3 C18 C15 118.8(5) . . ?
O4 C18 C15 116.2(4) . . ?
O5 C19 O5 121.5(11) . 2 ?
O5 C19 C16 119.3(5) . . ?
O5 C19 C16 119.3(5) 2 . ?
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 O4 1.995(4) 1_565 ?
Zn1 O1 2.040(4) . ?
Zn1 O1W 2.043(4) . ?
Zn1 N2 2.117(5) . ?
Zn1 N1 2.132(4) . ?
O1W H1WA 0.831(19) . ?
O1W H1WB 0.852(19) . ?
O1 C17 1.267(7) . ?
O2 C17 1.234(7) . ?
O3 C18 1.214(6) . ?
O4 C18 1.275(6) . ?
O4 Zn1 1.995(4) 1_545 ?
O5 C19 1.289(8) . ?
O5 H5O 0.8498 . ?
N2 C10 1.320(8) . ?
N2 C6 1.347(8) . ?
N1 C1 1.327(7) . ?
N1 C5 1.358(7) . ?
C1 C2 1.395(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.343(10) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(10) . ?
C3 H3 0.9300 . ?
C4 C5 1.410(8) . ?
C4 C11 1.437(9) . ?
C5 C6 1.436(8) . ?
C6 C7 1.402(8) . ?
C7 C8 1.402(11) . ?
C7 C12 1.447(10) . ?
C8 C9 1.354(12) . ?
C8 H8 0.9300 . ?
C9 C10 1.404(10) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.341(11) . ?
C11 H11 0.9300 . ?
C12 H12 0.9300 . ?
C13 C14 1.387(6) . ?
C13 C14 1.387(6) 2 ?
C13 H13 0.9300 . ?
C14 C15 1.397(7) . ?
C14 C17 1.504(7) . ?
C15 C16 1.397(6) . ?
C15 C18 1.515(7) . ?
C16 C15 1.397(6) 2 ?
C16 C19 1.431(14) . ?
C19 O5 1.289(8) 2 ?
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
O1W H1WA O4 0.831(19) 2.05(3) 2.840(6) 160(6) 5_565
O1W H1WB O2 0.852(19) 2.03(3) 2.714(6) 137(3) .
O5 H5O O1 0.85 2.07 2.918(9) 179.7 2_545
C3 H3 O3 0.93 2.50 3.340(8) 150.8 7_565
C11 H11 O2 0.93 2.48 3.279(8) 144.0 7_565
C12 H12 O2 0.93 2.58 3.484(8) 164.3 3
C13 H13 O5 0.93 2.45 3.306(10) 152.7 1_565
C13 H13 O5 0.93 2.45 3.306(10) 152.7 2_565
