#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/75/2217565.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_2217565
loop_
_publ_author_name
'Tan, Yu-Hui'
'Li, Qing-Song'
'Luo, Xian-Ping'
'Xie, Xiao-Bing'
_publ_section_title
catena-Poly[[tetraaquazinc(II)]-μ-2,2'-dihydroxy-5,5'-diazenediyldibenzoato]
_journal_coeditor_code           IS2258
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m276
_journal_page_last               m277
_journal_paper_doi               10.1107/S1600536807064860
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '[Zn (C14 H8 N2 O6) (H2 O)4]'
_chemical_formula_moiety         'C14 H16 N2 O10 Zn'
_chemical_formula_sum            'C14 H16 N2 O10 Zn'
_chemical_formula_weight         437.66
_chemical_name_systematic
;
catena-Poly[[tetraaquazinc(II)]-
μ-2,2'-dihydroxy-5,5'-diazenediyldibenzoato]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 107.019(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.510(2)
_cell_length_b                   11.255(3)
_cell_length_c                   16.214(4)
_cell_measurement_reflns_used    935
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.99
_cell_measurement_theta_min      1.81
_cell_volume                     1659.5(7)
_computing_cell_refinement       'SAINT (Bruker, 2000)'
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2000)'
_computing_publication_material  'SHELXTL (Bruker, 2000)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and 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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0564
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10784
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        0.03
_diffrn_standards_interval_count 150
_diffrn_standards_interval_time  10
_diffrn_standards_number         2807
_exptl_absorpt_coefficient_mu    1.542
_exptl_absorpt_correction_T_max  0.8611
_exptl_absorpt_correction_T_min  0.6992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2000)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.752
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.696
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3278
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max_lt       0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0307P)²+1.3308P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0956
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                3036
_reflns_number_total             3278
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            is2258.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2217565
_cod_database_fobs_code          2217565
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Zn Zn1 0.71408(5) 0.64023(4) 0.21196(3) 0.03166(13) Uani d . 1
O O6 0.9487(4) 0.4284(3) 0.2011(2) 0.0620(11) Uani d . 1
O O5 0.7705(4) 0.5388(3) 0.1179(2) 0.0434(8) Uani d . 1
O O4 0.6849(4) 0.5057(3) -0.0439(2) 0.0511(9) Uani d . 1
H H4A 0.6873 0.5359 0.0025 0.077 Uiso calc R 1
O O3 1.5187(4) -0.2597(3) -0.0536(2) 0.0570(10) Uani d . 1
H H3A 1.5603 -0.2816 -0.0042 0.085 Uiso calc R 1
O O2 1.5791(3) -0.2637(2) 0.10891(19) 0.0375(7) Uani d . 1
O O1 1.4725(4) -0.1395(3) 0.17841(18) 0.0508(8) Uani d . 1
O O4W 0.5362(4) 0.5313(3) 0.2060(3) 0.0535(9) Uani d . 1
O O3W 0.8865(4) 0.7510(3) 0.2132(3) 0.0501(8) Uani d . 1
O O2W 0.6659(4) 0.7520(3) 0.3064(2) 0.0493(9) Uani d . 1
O O1W 0.8398(4) 0.5403(3) 0.3147(2) 0.0431(8) Uani d . 1
N N2 1.0930(4) 0.1421(3) 0.0030(2) 0.0343(7) Uani d . 1
N N1 1.1233(4) 0.1052(3) -0.0637(2) 0.0334(8) Uani d . 1
C C14 0.8672(5) 0.4557(4) 0.1291(3) 0.0402(11) Uani d . 1
C C13 0.8783(5) 0.3916(3) 0.0511(3) 0.0335(9) Uani d . 1
C C12 0.7874(5) 0.4192(4) -0.0312(3) 0.0343(9) Uani d . 1
C C11 0.7972(5) 0.3553(4) -0.1026(3) 0.0414(10) Uani d . 1
H H11A 0.7367 0.3751 -0.1571 0.050 Uiso calc R 1
C C10 0.8949(5) 0.2633(4) -0.0935(3) 0.0372(9) Uani d . 1
H H10A 0.8989 0.2196 -0.1414 0.045 Uiso calc R 1
C C9 0.9877(5) 0.2357(3) -0.0127(3) 0.0316(9) Uani d . 1
C C8 0.9781(5) 0.2998(4) 0.0582(3) 0.0370(10) Uani d . 1
H H8A 1.0406 0.2807 0.1123 0.044 Uiso calc R 1
C C7 1.2236(4) 0.0099(3) -0.0537(3) 0.0322(9) Uani d . 1
C C6 1.2416(5) -0.0349(4) -0.1298(3) 0.0396(10) Uani d . 1
H H6A 1.1871 -0.0025 -0.1822 0.048 Uiso calc R 1
C C5 1.3378(6) -0.1259(4) -0.1296(3) 0.0473(12) Uani d . 1
H H5A 1.3469 -0.1558 -0.1812 0.057 Uiso calc R 1
C C4 1.4210(5) -0.1727(4) -0.0517(3) 0.0372(10) Uani d . 1
C C3 1.4032(4) -0.1293(4) 0.0259(2) 0.0301(8) Uani d . 1
C C2 1.3051(5) -0.0383(3) 0.0244(3) 0.0316(9) Uani d . 1
H H2A 1.2936 -0.0093 0.0758 0.038 Uiso calc R 1
C C1 1.4901(5) -0.1794(4) 0.1108(3) 0.0321(9) Uani d . 1
H H1WA 0.872(6) 0.496(5) 0.283(4) 0.062(18) Uiso d . 1
H H3WA 0.872(7) 0.779(5) 0.170(4) 0.05(2) Uiso d . 1
H H4WA 0.507(9) 0.504(6) 0.159(5) 0.09(3) Uiso d . 1
H H2WA 0.597(7) 0.802(5) 0.260(4) 0.073(19) Uiso d . 1
H H3WB 0.921(7) 0.796(6) 0.250(5) 0.07(2) Uiso d . 1
H H4WB 0.545(7) 0.488(5) 0.253(4) 0.066(19) Uiso d . 1
H H1WB 0.895(8) 0.580(6) 0.359(4) 0.08(2) Uiso d . 1
H H2WB 0.619(8) 0.703(6) 0.330(5) 0.09(3) Uiso d . 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
_geom_angle_publ_flag
O3W Zn1 O4W . . 177.75(16) yes
O3W Zn1 O1W . . 92.90(16) yes
O4W Zn1 O1W . . 89.28(15) yes
O3W Zn1 O2 . 1_465 89.72(15) yes
O4W Zn1 O2 . 1_465 88.10(14) yes
O1W Zn1 O2 . 1_465 177.36(13) yes
O3W Zn1 O5 . . 87.93(16) yes
O4W Zn1 O5 . . 91.35(16) yes
O1W Zn1 O5 . . 94.52(13) yes
O2 Zn1 O5 1_465 . 85.89(11) yes
O3W Zn1 O2W . . 88.49(17) yes
O4W Zn1 O2W . . 92.21(18) yes
O1W Zn1 O2W . . 86.44(15) yes
O2 Zn1 O2W 1_465 . 93.32(13) yes
O5 Zn1 O2W . . 176.33(15) yes
C14 O5 Zn1 . . 128.2(3) ?
C12 O4 H4A . . 109.5 ?
C4 O3 H3A . . 109.5 ?
C1 O2 Zn1 . 1_645 128.5(3) ?
Zn1 O4W H4WA . . 109(6) ?
Zn1 O4W H4WB . . 114(4) ?
H4WA O4W H4WB . . 122(6) ?
Zn1 O3W H3WA . . 109(5) ?
Zn1 O3W H3WB . . 125(5) ?
H3WA O3W H3WB . . 111(7) ?
Zn1 O2W H2WA . . 91(3) ?
Zn1 O2W H2WB . . 101(5) ?
H2WA O2W H2WB . . 112(5) ?
Zn1 O1W H1WA . . 93(4) ?
Zn1 O1W H1WB . . 117(4) ?
H1WA O1W H1WB . . 125(6) ?
N1 N2 C9 . . 114.4(3) ?
N2 N1 C7 . . 117.7(3) ?
O6 C14 O5 . . 122.6(4) ?
O6 C14 C13 . . 120.1(4) ?
O5 C14 C13 . . 117.3(4) ?
C8 C13 C12 . . 117.6(4) ?
C8 C13 C14 . . 120.6(4) ?
C12 C13 C14 . . 121.8(4) ?
O4 C12 C11 . . 117.9(4) ?
O4 C12 C13 . . 121.6(4) ?
C11 C12 C13 . . 120.5(4) ?
C10 C11 C12 . . 120.7(4) ?
C10 C11 H11A . . 119.7 ?
C12 C11 H11A . . 119.7 ?
C11 C10 C9 . . 119.8(4) ?
C11 C10 H10A . . 120.1 ?
C9 C10 H10A . . 120.1 ?
C8 C9 C10 . . 119.4(4) ?
C8 C9 N2 . . 116.8(4) ?
C10 C9 N2 . . 123.8(4) ?
C9 C8 C13 . . 122.0(4) ?
C9 C8 H8A . . 119.0 ?
C13 C8 H8A . . 119.0 ?
C2 C7 C6 . . 119.2(4) ?
C2 C7 N1 . . 125.4(4) ?
C6 C7 N1 . . 115.4(3) ?
C5 C6 C7 . . 121.6(4) ?
C5 C6 H6A . . 119.2 ?
C7 C6 H6A . . 119.2 ?
C6 C5 C4 . . 119.3(4) ?
C6 C5 H5A . . 120.3 ?
C4 C5 H5A . . 120.3 ?
O3 C4 C5 . . 117.9(4) ?
O3 C4 C3 . . 122.2(4) ?
C5 C4 C3 . . 119.9(4) ?
C2 C3 C4 . . 120.0(3) ?
C2 C3 C1 . . 119.0(4) ?
C4 C3 C1 . . 121.0(4) ?
C3 C2 C7 . . 120.0(4) ?
C3 C2 H2A . . 120.0 ?
C7 C2 H2A . . 120.0 ?
O1 C1 O2 . . 123.5(4) ?
O1 C1 C3 . . 119.8(4) ?
O2 C1 C3 . . 116.7(4) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 O3W . 2.055(4) yes
Zn1 O4W . 2.069(4) yes
Zn1 O1W . 2.075(3) yes
Zn1 O2 1_465 2.086(3) yes
Zn1 O5 . 2.097(3) yes
Zn1 O2W . 2.132(3) yes
O6 C14 . 1.236(6) ?
O5 C14 . 1.286(5) ?
O4 C12 . 1.350(5) ?
O4 H4A . 0.8200 ?
O3 C4 . 1.356(5) ?
O3 H3A . 0.8200 ?
O2 C1 . 1.278(5) ?
O2 Zn1 1_645 2.086(3) ?
O1 C1 . 1.240(5) ?
O4W H4WA . 0.80(8) ?
O4W H4WB . 0.88(7) ?
O3W H3WA . 0.74(6) ?
O3W H3WB . 0.78(7) ?
O2W H2WA . 1.02(7) ?
O2W H2WB . 0.87(7) ?
O1W H1WA . 0.83(6) ?
O1W H1WB . 0.88(7) ?
N2 N1 . 1.267(5) ?
N2 C9 . 1.425(5) ?
N1 C7 . 1.413(5) ?
C14 C13 . 1.487(6) ?
C13 C8 . 1.385(6) ?
C13 C12 . 1.396(6) ?
C12 C11 . 1.389(6) ?
C11 C10 . 1.370(6) ?
C11 H11A . 0.9300 ?
C10 C9 . 1.383(6) ?
C10 H10A . 0.9300 ?
C9 C8 . 1.383(6) ?
C8 H8A . 0.9300 ?
C7 C2 . 1.387(6) ?
C7 C6 . 1.389(6) ?
C6 C5 . 1.372(6) ?
C6 H6A . 0.9300 ?
C5 C4 . 1.382(6) ?
C5 H5A . 0.9300 ?
C4 C3 . 1.406(6) ?
C3 C2 . 1.381(5) ?
C3 C1 . 1.493(5) ?
C2 H2A . 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
O1W H1WA O6 . 0.84(6) 1.86(6) 2.677(5) 168(6)
O1W H1WB N2 2_755 0.88(7) 2.32(6) 3.058(5) 143(6)
O2W H2WA O1 1_465 1.01(6) 1.63(6) 2.636(5) 170(6)
O2W H2WB O3 4_466 0.87(7) 2.44(8) 2.997(5) 123(6)
O3W H3WA N1 3_765 0.74(6) 2.17(6) 2.893(5) 164(5)
O3W H3WB O6 2_755 0.78(8) 1.95(7) 2.664(5) 152(7)
O4W H4WA O4 3_665 0.79(7) 2.20(8) 2.875(6) 144(8)
O4W H4WB O1 2_755 0.89(6) 1.85(6) 2.703(5) 160(6)
O3 H3A O2 . 0.82 1.80 2.528(4) 147
O4 H4A O5 . 0.82 1.81 2.537(4) 148
C2 H2A O1W 2_745 0.93 2.53 3.405(6) 157
