#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/60/2236030.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2236030
loop_
_publ_author_name
'Zhang, Kou-Lin'
'Qiu, Ting-Ting'
'Ng, Seik Weng'
_publ_section_title
;
 Poly[[bis(μ-3-amino-5-carboxybenzoato-κ²N:O¹)diaquazinc]
 dihydrate]
;
_journal_coeditor_code           XU5588
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1088
_journal_paper_doi               10.1107/S1600536812031789
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Zn (C8 H6 N O4)2 (H2 O)2], 2H2 O'
_chemical_formula_moiety         'C16 H16 N2 O10 Zn, 2H2 O'
_chemical_formula_sum            'C16 H20 N2 O12 Zn'
_chemical_formula_weight         497.71
_chemical_name_systematic
;
Poly[[bis(μ-3-amino-5-carboxybenzoato-
κ²N:O¹)diaquazinc] dihydrate]
;
_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                 113.2860(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.2209(10)
_cell_length_b                   11.2252(8)
_cell_length_c                   12.7139(9)
_cell_measurement_reflns_used    4815
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.15
_cell_measurement_theta_min      2.39
_cell_volume                     1864.2(2)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'OLEX (Dolomanov et al., 2003) and X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'ω scans'
_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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0163
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8005
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.392
_exptl_absorpt_correction_T_max  0.7878
_exptl_absorpt_correction_T_min  0.6802
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.773
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.373
_refine_diff_density_min         -0.371
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     144
_refine_ls_number_reflns         2130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0385
_refine_ls_R_factor_gt           0.0337
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0506P)²+3.2779P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.0979
_reflns_number_gt                1843
_reflns_number_total             2130
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            xu5588.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2236030
_cod_database_fobs_code          2236030
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_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Zn Zn1 0.2500 0.2500 0.0000 0.02950(14) Uani d S 1 2
O O1 0.20751(15) 0.32463(16) 0.12770(14) 0.0412(4) Uani d . 1 1
O O2 0.1529(2) 0.1571(2) 0.1754(2) 0.0655(7) Uani d . 1 1
O O3 0.09628(17) 0.14472(16) 0.53610(16) 0.0436(4) Uani d . 1 1
H H1 0.0885 0.1154 0.5929 0.065 Uiso calc R 1 1
O O4 0.07472(15) 0.31377(16) 0.61500(15) 0.0408(4) Uani d . 1 1
O O1W 0.35790(16) 0.38916(19) 0.03707(18) 0.0531(5) Uani d . 1 1
H H2 0.3743 0.3994 -0.0189 0.080 Uiso calc R 1 1
H H3 0.4102 0.3714 0.0953 0.080 Uiso calc PR 0.50 1
H H3' 0.3322 0.4522 0.0496 0.080 Uiso calc PR 0.50 1
O O2W 0.0898(2) -0.04635(18) 0.22475(18) 0.0594(6) Uani d . 1 1
H H4 0.1052 0.0229 0.2118 0.089 Uiso d R 1 1
H H5 0.0334 -0.0439 0.2320 0.089 Uiso d PR 0.50 1
H H5' 0.1397 -0.0755 0.2797 0.089 Uiso d PR 0.50 1
N N1 0.12864(15) 0.64309(17) 0.36983(16) 0.0312(4) Uani d . 1 1
H H6 0.0705 0.6633 0.3742 0.037 Uiso calc R 1 1
H H7 0.1250 0.6675 0.3025 0.037 Uiso calc R 1 1
C C1 0.1718(2) 0.2655(2) 0.1878(2) 0.0349(5) Uani d . 1 1
C C2 0.15207(17) 0.3304(2) 0.28176(18) 0.0291(4) Uani d . 1 1
C C3 0.15228(17) 0.4538(2) 0.28397(18) 0.0294(5) Uani d . 1 1
H H3A 0.1667 0.4963 0.2293 0.035 Uiso calc R 1 1
C C4 0.13087(16) 0.5152(2) 0.36787(17) 0.0274(4) Uani d . 1 1
C C5 0.11166(17) 0.4506(2) 0.45058(18) 0.0295(5) Uani d . 1 1
H H5A 0.0982 0.4904 0.5073 0.035 Uiso calc R 1 1
C C6 0.11247(17) 0.3261(2) 0.44894(17) 0.0277(4) Uani d . 1 1
C C7 0.13167(19) 0.2662(2) 0.3638(2) 0.0302(5) Uani d . 1 1
H H7A 0.1309 0.1834 0.3618 0.036 Uiso calc R 1 1
C C8 0.09264(19) 0.2626(2) 0.54063(19) 0.0309(5) Uani d . 1 1
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1W Zn1 O1W . 7 180.00(9)
O1W Zn1 O1 . . 86.47(8)
O1W Zn1 O1 7 . 93.53(8)
O1W Zn1 O1 . 7 93.53(8)
O1W Zn1 O1 7 7 86.47(8)
O1 Zn1 O1 . 7 180.00(8)
O1W Zn1 N1 . 6_565 92.80(8)
O1W Zn1 N1 7 6_565 87.20(8)
O1 Zn1 N1 . 6_565 89.10(7)
O1 Zn1 N1 7 6_565 90.90(7)
O1W Zn1 N1 . 4_545 87.20(8)
O1W Zn1 N1 7 4_545 92.80(8)
O1 Zn1 N1 . 4_545 90.90(7)
O1 Zn1 N1 7 4_545 89.10(7)
N1 Zn1 N1 6_565 4_545 180.00(18)
C1 O1 Zn1 . . 124.19(16)
C8 O3 H1 . . 109.5
Zn1 O1W H2 . . 109.5
Zn1 O1W H3 . . 109.5
H2 O1W H3 . . 109.5
Zn1 O1W H3' . . 109.5
H2 O1W H3' . . 109.5
H3 O1W H3' . . 109.5
H4 O2W H5 . . 108.9
H4 O2W H5' . . 108.8
H5 O2W H5' . . 116.7
C4 N1 Zn1 . 4 122.60(14)
C4 N1 H6 . . 106.7
Zn1 N1 H6 4 . 106.7
C4 N1 H7 . . 106.7
Zn1 N1 H7 4 . 106.7
H6 N1 H7 . . 106.6
O2 C1 O1 . . 123.9(2)
O2 C1 C2 . . 118.2(2)
O1 C1 C2 . . 117.9(2)
C7 C2 C3 . . 120.2(2)
C7 C2 C1 . . 120.1(2)
C3 C2 C1 . . 119.8(2)
C2 C3 C4 . . 120.5(2)
C2 C3 H3A . . 119.7
C4 C3 H3A . . 119.7
C5 C4 C3 . . 119.1(2)
C5 C4 N1 . . 119.72(19)
C3 C4 N1 . . 121.18(19)
C4 C5 C6 . . 120.31(19)
C4 C5 H5A . . 119.8
C6 C5 H5A . . 119.8
C7 C6 C5 . . 120.1(2)
C7 C6 C8 . . 122.4(2)
C5 C6 C8 . . 117.58(19)
C2 C7 C6 . . 119.8(2)
C2 C7 H7A . . 120.1
C6 C7 H7A . . 120.1
O4 C8 O3 . . 121.9(2)
O4 C8 C6 . . 123.1(2)
O3 C8 C6 . . 114.96(19)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Zn1 O1W . 2.108(2)
Zn1 O1W 7 2.108(2)
Zn1 O1 . 2.1163(16)
Zn1 O1 7 2.1163(16)
Zn1 N1 6_565 2.214(2)
Zn1 N1 4_545 2.214(2)
O1 C1 . 1.261(3)
O2 C1 . 1.243(3)
O3 C8 . 1.326(3)
O3 H1 . 0.8400
O4 C8 . 1.217(3)
O1W H2 . 0.8400
O1W H3 . 0.8400
O1W H3' . 0.8400
O2W H4 . 0.8408
O2W H5 . 0.8425
O2W H5' . 0.8407
N1 C4 . 1.436(3)
N1 Zn1 4 2.214(2)
N1 H6 . 0.8800
N1 H7 . 0.8800
C1 C2 . 1.517(3)
C2 C7 . 1.390(3)
C2 C3 . 1.386(3)
C3 C4 . 1.401(3)
C3 H3A . 0.9300
C4 C5 . 1.390(3)
C5 C6 . 1.398(3)
C5 H5A . 0.9300
C6 C7 . 1.390(3)
C6 C8 . 1.486(3)
C7 H7A . 0.9300
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H1 O2W 6_556 0.84 1.84 2.675(3) 172.3
O1W H2 O2 7 0.84 1.97 2.695(3) 143.1
O2W H4 O2 . 0.84 1.79 2.619(3) 169.9
O2W H5 O2W 2 0.84 2.03 2.869(5) 170.9
O2W H5' O1 4_545 0.84 2.31 3.106(3) 157.9
O2W H5' O1W 4_545 0.84 2.35 2.910(3) 124.5
N1 H6 O4 5_566 0.88 2.14 3.013(3) 171.9
N1 H7 O4 6_565 0.88 2.21 3.059(2) 161.3
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_site_symmetry_1
_geom_torsion
O1W Zn1 O1 C1 . -150.9(2)
O1W Zn1 O1 C1 7 29.1(2)
N1 Zn1 O1 C1 6_565 116.2(2)
N1 Zn1 O1 C1 4_545 -63.8(2)
Zn1 O1 C1 O2 . -3.4(4)
Zn1 O1 C1 C2 . 175.68(15)
O2 C1 C2 C7 . 11.5(4)
O1 C1 C2 C7 . -167.7(2)
O2 C1 C2 C3 . -167.1(3)
O1 C1 C2 C3 . 13.8(3)
C7 C2 C3 C4 . -0.7(3)
C1 C2 C3 C4 . 177.9(2)
C2 C3 C4 C5 . 1.4(3)
C2 C3 C4 N1 . -178.7(2)
Zn1 N1 C4 C5 4 72.4(2)
Zn1 N1 C4 C3 4 -107.5(2)
C3 C4 C5 C6 . -0.8(3)
N1 C4 C5 C6 . 179.3(2)
C4 C5 C6 C7 . -0.6(3)
C4 C5 C6 C8 . 179.3(2)
C3 C2 C7 C6 . -0.7(3)
C1 C2 C7 C6 . -179.2(2)
C5 C6 C7 C2 . 1.3(3)
C8 C6 C7 C2 . -178.5(2)
C7 C6 C8 O4 . -179.2(2)
C5 C6 C8 O4 . 1.0(3)
C7 C6 C8 O3 . 1.0(3)
C5 C6 C8 O3 . -178.8(2)
