#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/97/2229764.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_2229764
loop_
_publ_author_name
'Şerb, Mihaela-Diana'
'Wang, Yutian'
'Dumitru, Florina'
'Englert, Ulli'
_publ_section_title
;
 Triaquabis[4-(methoxycarbonyl)benzoato-κO¹]zinc dihydrate
;
_journal_coeditor_code           NC2223
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m475
_journal_page_last               m476
_journal_paper_doi               10.1107/S1600536811010269
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zn (C9 H7 O4)2 (H2 O)3], 2H2 O'
_chemical_formula_moiety         'C18 H20 O11 Zn, 2(H2 O)'
_chemical_formula_sum            'C18 H24 O13 Zn'
_chemical_formula_weight         513.74
_chemical_name_systematic
;
Triaquabis[4-(methoxycarbonyl)benzoato-κO¹]zinc(II) 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
_cell_angle_alpha                90.00
_cell_angle_beta                 91.551(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7157(15)
_cell_length_b                   5.9719(7)
_cell_length_c                   25.874(3)
_cell_measurement_reflns_used    2818
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.58
_cell_measurement_theta_min      2.97
_cell_volume                     2118.5(4)
_computing_cell_refinement       'SAINT-Plus (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus (Bruker, 1999)'
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_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  0.0448
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            12212
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.228
_exptl_absorpt_correction_T_max  0.9759
_exptl_absorpt_correction_T_min  0.7249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2004)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.611
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.02
_refine_diff_density_max         .434
_refine_diff_density_min         -.300
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2435
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0320
_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)+(0.0415P)²+1.9928P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                2269
_reflns_number_total             2435
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            nc2223.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2229764
_cod_database_fobs_code          2229764
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_disorder_assembly
_atom_site_disorder_group
Zn Zn1 0.5000 0.22322(5) 0.2500 0.01550(11) Uani d S 1 . .
O O1 0.43857(11) -0.1990(2) 0.16962(5) 0.0234(3) Uani d . 1 . .
O O2 0.50650(10) 0.1406(2) 0.17621(5) 0.0206(3) Uani d . 1 . .
O O3 0.30981(11) 0.0349(3) -0.08830(5) 0.0282(3) Uani d . 1 . .
O O4 0.36264(11) 0.3853(2) -0.07513(5) 0.0256(3) Uani d . 1 . .
O O5 0.5000 0.5587(3) 0.2500 0.0363(6) Uani d S 1 . .
H H50 0.4839 0.6475 0.2239 0.053(9) Uiso d R 1 . .
O O6 0.65137(10) 0.1991(3) 0.25858(6) 0.0263(3) Uani d . 1 . .
H H60 0.6780 0.3069 0.2724 0.041(8) Uiso d R 1 . .
H H61 0.6851 0.1665 0.2313 0.048(8) Uiso d R 1 . .
C C1 0.45986(13) -0.0115(3) 0.15193(7) 0.0166(4) Uani d . 1 . .
C C2 0.42900(12) 0.0408(3) 0.09683(6) 0.0153(4) Uani d . 1 . .
C C3 0.38816(15) -0.1255(3) 0.06540(7) 0.0207(4) Uani d . 1 . .
H H3 0.3786 -0.2715 0.0789 0.025 Uiso calc R 1 . .
C C4 0.36134(14) -0.0791(3) 0.01444(7) 0.0207(4) Uani d . 1 . .
H H4 0.3347 -0.1940 -0.0071 0.025 Uiso calc R 1 . .
C C5 0.44032(15) 0.2554(3) 0.07716(8) 0.0209(4) Uani d . 1 . .
H H5 0.4676 0.3701 0.0985 0.025 Uiso calc R 1 . .
C C6 0.41201(15) 0.3030(3) 0.02661(8) 0.0218(4) Uani d . 1 . .
H H6 0.4189 0.4506 0.0135 0.026 Uiso calc R 1 . .
C C7 0.37346(13) 0.1352(3) -0.00510(7) 0.0158(4) Uani d . 1 . .
C C8 0.34468(13) 0.1775(3) -0.06031(7) 0.0178(4) Uani d . 1 . .
O O10 0.77354(10) 0.0523(3) 0.18399(5) 0.0229(3) Uani d . 1 . .
H H100 0.8165 0.1421 0.1773 0.060(10) Uiso d R 1 . .
H H101 0.7457 0.0254 0.1559 0.051(8) Uiso d R 1 . .
C C10 0.33801(16) 0.4409(4) -0.12870(8) 0.0288(5) Uani d . 1 . .
H H10A 0.3762 0.3468 -0.1517 0.043 Uiso calc R 1 . .
H H10B 0.3529 0.5989 -0.1350 0.043 Uiso calc R 1 . .
H H10C 0.2683 0.4142 -0.1355 0.043 Uiso calc R 1 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn .2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O2 Zn1 O2 . 2_655 151.08(9) ?
O2 Zn1 O5 . . 104.46(4) ?
O2 Zn1 O5 2_655 . 104.46(4) ?
O2 Zn1 O6 . . 90.85(5) ?
O2 Zn1 O6 2_655 . 87.18(6) ?
O5 Zn1 O6 . . 93.97(4) ?
O2 Zn1 O6 . 2_655 87.17(6) ?
O2 Zn1 O6 2_655 2_655 90.85(5) ?
O5 Zn1 O6 . 2_655 93.97(4) ?
O6 Zn1 O6 . 2_655 172.07(9) ?
C1 O2 Zn1 . . 128.49(12) ?
C8 O4 C10 . . 116.67(16) ?
Zn1 O5 H50 . . 127.0 ?
Zn1 O6 H60 . . 115.1 ?
Zn1 O6 H61 . . 118.4 ?
H60 O6 H61 . . 106.7 ?
O1 C1 O2 . . 125.53(16) ?
O1 C1 C2 . . 118.06(16) ?
O2 C1 C2 . . 116.41(16) ?
C5 C2 C3 . . 119.45(16) ?
C5 C2 C1 . . 120.40(16) ?
C3 C2 C1 . . 120.15(17) ?
C4 C3 C2 . . 120.33(18) ?
C4 C3 H3 . . 119.8 ?
C2 C3 H3 . . 119.8 ?
C3 C4 C7 . . 119.94(17) ?
C3 C4 H4 . . 120.0 ?
C7 C4 H4 . . 120.0 ?
C6 C5 C2 . . 120.29(17) ?
C6 C5 H5 . . 119.9 ?
C2 C5 H5 . . 119.9 ?
C5 C6 C7 . . 120.15(18) ?
C5 C6 H6 . . 119.9 ?
C7 C6 H6 . . 119.9 ?
C4 C7 C6 . . 119.81(17) ?
C4 C7 C8 . . 118.24(17) ?
C6 C7 C8 . . 121.95(17) ?
O3 C8 O4 . . 124.12(17) ?
O3 C8 C7 . . 122.99(18) ?
O4 C8 C7 . . 112.89(16) ?
H100 O10 H101 . . 105.0 ?
O4 C10 H10A . . 109.5 ?
O4 C10 H10B . . 109.5 ?
H10A C10 H10B . . 109.5 ?
O4 C10 H10C . . 109.5 ?
H10A C10 H10C . . 109.5 ?
H10B C10 H10C . . 109.5 ?
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 O2 . 1.9763(12) yes
Zn1 O2 2_655 1.9765(12) yes
Zn1 O5 . 2.003(2) yes
Zn1 O6 . 2.0869(14) yes
Zn1 O6 2_655 2.0870(14) yes
O1 C1 . 1.247(2) ?
O2 C1 . 1.268(2) ?
O3 C8 . 1.208(2) ?
O4 C8 . 1.324(2) ?
O4 C10 . 1.456(2) ?
O5 H50 . 0.88 ?
O6 H60 . 0.82 ?
O6 H61 . 0.88 ?
C1 C2 . 1.509(2) ?
C2 C5 . 1.389(3) ?
C2 C3 . 1.392(3) ?
C3 C4 . 1.387(2) ?
C3 H3 . 0.95 ?
C4 C7 . 1.388(3) ?
C4 H4 . 0.95 ?
C5 C6 . 1.384(3) ?
C5 H5 . 0.95 ?
C6 C7 . 1.390(3) ?
C6 H6 . 0.95 ?
C7 C8 . 1.493(2) ?
O10 H100 . 0.82 ?
O10 H101 . 0.83 ?
C10 H10A . 0.98 ?
C10 H10B . 0.98 ?
C10 H10C . 0.98 ?
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
O5 H50 O1 1_565 0.88 1.78 2.6522(16) 172
O6 H60 O10 4_655 0.82 1.96 2.763(2) 170
O6 H61 O10 . 0.88 1.87 2.734(2) 166
O10 H100 O1 3_555 0.82 1.94 2.741(2) 166
O10 H101 O3 5_655 0.83 1.92 2.7486(19) 176
