#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/08/2230812.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_2230812
loop_
_publ_author_name
'Nie, Jing-Jing'
'Xu, Xun'
'Xu, Duan-Jun'
_publ_section_title
;
 Aquabis(4-chloro-2-hydroxybenzoato-κO)(1,10-phenanthroline-κ²N,N')zinc(II)
;
_journal_coeditor_code           NG5174
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m855
_journal_page_last               m856
_journal_paper_doi               10.1107/S1600536811020435
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Zn (C7 H4 Cl O3)2 (C12 H8 N2) (H2 O)]'
_chemical_formula_moiety         'C26 H18 Cl2 N2 O7 Zn'
_chemical_formula_sum            'C26 H18 Cl2 N2 O7 Zn'
_chemical_formula_weight         606.69
_chemical_name_systematic
;
Aquabis(4-chloro-2-hydroxybenzoato-κO)(1,10-phenanthroline-
κ²N,N')zinc(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                100.534(7)
_cell_angle_beta                 94.360(8)
_cell_angle_gamma                111.315(5)
_cell_formula_units_Z            2
_cell_length_a                   8.2611(12)
_cell_length_b                   11.0124(16)
_cell_length_c                   14.654(2)
_cell_measurement_reflns_used    4275
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      1.4
_cell_volume                     1206.2(3)
_computing_cell_refinement       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      294(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_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  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0290
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13131
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    1.292
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(ABSCOR; Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.643
_refine_diff_density_min         -0.285
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0343
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0614P)²+0.2083P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0959
_refine_ls_wR_factor_ref         0.1010
_reflns_number_gt                3695
_reflns_number_total             4275
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ng5174.cif
_cod_data_source_block           I
_cod_original_cell_volume        1206.1(3)
_cod_database_code               2230812
_cod_database_fobs_code          2230812
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn Zn 0.82980(4) 0.50277(3) 0.61362(2) 0.03699(12) Uani d . 1 1 . .
Cl Cl1 0.11084(11) 0.33056(8) 1.01904(6) 0.0632(2) Uani d . 1 1 . .
Cl Cl2 0.18339(13) 0.01494(10) 0.08427(6) 0.0760(3) Uani d . 1 1 . .
N N1 1.0170(3) 0.6673(2) 0.71593(15) 0.0386(5) Uani d . 1 1 . .
N N2 0.8102(3) 0.6686(2) 0.56568(14) 0.0345(5) Uani d . 1 1 . .
O O1 0.6382(2) 0.44332(18) 0.69227(12) 0.0418(4) Uani d . 1 1 . .
O O2 0.7884(3) 0.3686(2) 0.78612(13) 0.0474(5) Uani d . 1 1 . .
O O3 0.6810(3) 0.3089(2) 0.93748(14) 0.0553(5) Uani d . 1 1 . .
H H3A 0.7437 0.3201 0.8855 0.083 Uiso d R 1 1 . .
O O4 0.7237(3) 0.39070(18) 0.48131(13) 0.0505(5) Uani d . 1 1 . .
O O5 0.7478(3) 0.1972(2) 0.48595(15) 0.0586(6) Uani d . 1 1 . .
O O6 0.5411(4) -0.0177(2) 0.36472(17) 0.0726(7) Uani d . 1 1 . .
H H6A 0.6098 0.0407 0.4219 0.109 Uiso d R 1 1 . .
O O7 0.9615(3) 0.3763(2) 0.63633(14) 0.0550(5) Uani d . 1 1 . .
H H7A 0.9124 0.3467 0.6815 0.082 Uiso d R 1 1 . .
H H7B 0.8986 0.3023 0.5846 0.082 Uiso d R 1 1 . .
C C1 1.1169(4) 0.6657(3) 0.7912(2) 0.0468(7) Uani d . 1 1 . .
H H1 1.1155 0.5836 0.7996 0.056 Uiso calc R 1 1 . .
C C2 1.2232(4) 0.7806(3) 0.8579(2) 0.0513(8) Uani d . 1 1 . .
H H2 1.2903 0.7748 0.9096 0.062 Uiso calc R 1 1 . .
C C3 1.2277(4) 0.9020(3) 0.8463(2) 0.0484(7) Uani d . 1 1 . .
H H3 1.2990 0.9797 0.8901 0.058 Uiso calc R 1 1 . .
C C4 1.1245(3) 0.9098(3) 0.76815(18) 0.0398(6) Uani d . 1 1 . .
C C5 1.1198(4) 1.0317(3) 0.7507(2) 0.0472(7) Uani d . 1 1 . .
H H5 1.1891 1.1122 0.7923 0.057 Uiso calc R 1 1 . .
C C6 1.0167(4) 1.0327(3) 0.6750(2) 0.0469(7) Uani d . 1 1 . .
H H6 1.0161 1.1137 0.6653 0.056 Uiso calc R 1 1 . .
C C7 0.9084(3) 0.9110(3) 0.60930(18) 0.0376(6) Uani d . 1 1 . .
C C8 0.7985(4) 0.9050(3) 0.5286(2) 0.0440(7) Uani d . 1 1 . .
H H8 0.7930 0.9831 0.5157 0.053 Uiso calc R 1 1 . .
C C9 0.7007(4) 0.7849(3) 0.46974(19) 0.0438(7) Uani d . 1 1 . .
H H9 0.6292 0.7805 0.4160 0.053 Uiso calc R 1 1 . .
C C10 0.7084(4) 0.6680(3) 0.49066(18) 0.0398(6) Uani d . 1 1 . .
H H10 0.6394 0.5863 0.4503 0.048 Uiso calc R 1 1 . .
C C11 0.9101(3) 0.7889(2) 0.62411(17) 0.0321(5) Uani d . 1 1 . .
C C12 1.0201(3) 0.7880(2) 0.70504(17) 0.0335(6) Uani d . 1 1 . .
C C13 0.6586(4) 0.3973(2) 0.76426(18) 0.0369(6) Uani d . 1 1 . .
C C14 0.5204(3) 0.3775(2) 0.82579(17) 0.0339(6) Uani d . 1 1 . .
C C15 0.5405(4) 0.3348(3) 0.90948(18) 0.0380(6) Uani d . 1 1 . .
C C16 0.4128(4) 0.3204(3) 0.96834(19) 0.0435(7) Uani d . 1 1 . .
H H16 0.4265 0.2934 1.0240 0.052 Uiso calc R 1 1 . .
C C17 0.2668(4) 0.3462(3) 0.9437(2) 0.0434(7) Uani d . 1 1 . .
C C18 0.2414(4) 0.3856(3) 0.8610(2) 0.0471(7) Uani d . 1 1 . .
H H18 0.1410 0.4014 0.8448 0.056 Uiso calc R 1 1 . .
C C19 0.3681(4) 0.4009(3) 0.8035(2) 0.0424(6) Uani d . 1 1 . .
H H19 0.3521 0.4276 0.7480 0.051 Uiso calc R 1 1 . .
C C20 0.6860(4) 0.2680(3) 0.44804(19) 0.0404(6) Uani d . 1 1 . .
C C21 0.5611(4) 0.2044(3) 0.35760(18) 0.0398(6) Uani d . 1 1 . .
C C22 0.4962(4) 0.0653(3) 0.3208(2) 0.0469(7) Uani d . 1 1 . .
C C23 0.3784(4) 0.0078(3) 0.2366(2) 0.0529(8) Uani d . 1 1 . .
H H23 0.3348 -0.0841 0.2125 0.063 Uiso calc R 1 1 . .
C C24 0.3277(4) 0.0890(3) 0.1900(2) 0.0494(7) Uani d . 1 1 . .
C C25 0.3862(4) 0.2253(3) 0.2244(2) 0.0488(7) Uani d . 1 1 . .
H H25 0.3482 0.2781 0.1925 0.059 Uiso calc R 1 1 . .
C C26 0.5025(4) 0.2811(3) 0.30724(18) 0.0435(7) Uani d . 1 1 . .
H H26 0.5438 0.3732 0.3306 0.052 Uiso calc R 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'
Cl Cl 0.1484 0.1585 '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
O1 Zn O4 . . 105.38(8) ?
O1 Zn O7 . . 99.35(8) ?
O4 Zn O7 . . 90.95(8) ?
O1 Zn N2 . . 107.32(8) ?
O4 Zn N2 . . 87.64(8) ?
O7 Zn N2 . . 152.69(9) ?
O1 Zn N1 . . 98.75(8) ?
O4 Zn N1 . . 154.83(9) ?
O7 Zn N1 . . 92.12(9) ?
N2 Zn N1 . . 78.33(8) ?
C1 N1 C12 . . 117.5(2) ?
C1 N1 Zn . . 128.83(19) ?
C12 N1 Zn . . 113.36(16) ?
C10 N2 C11 . . 117.9(2) ?
C10 N2 Zn . . 128.55(17) ?
C11 N2 Zn . . 113.47(16) ?
C13 O1 Zn . . 122.31(18) ?
C15 O3 H3A . . 101.5 ?
C20 O4 Zn . . 130.02(18) ?
C22 O6 H6A . . 102.5 ?
Zn O7 H7A . . 99.6 ?
Zn O7 H7B . . 98.8 ?
H7A O7 H7B . . 100.6 ?
N1 C1 C2 . . 123.3(3) ?
N1 C1 H1 . . 118.3 ?
C2 C1 H1 . . 118.3 ?
C3 C2 C1 . . 119.1(3) ?
C3 C2 H2 . . 120.4 ?
C1 C2 H2 . . 120.4 ?
C2 C3 C4 . . 120.1(3) ?
C2 C3 H3 . . 120.0 ?
C4 C3 H3 . . 120.0 ?
C12 C4 C3 . . 116.7(3) ?
C12 C4 C5 . . 119.4(2) ?
C3 C4 C5 . . 124.0(3) ?
C6 C5 C4 . . 121.3(3) ?
C6 C5 H5 . . 119.4 ?
C4 C5 H5 . . 119.4 ?
C5 C6 C7 . . 121.0(3) ?
C5 C6 H6 . . 119.5 ?
C7 C6 H6 . . 119.5 ?
C11 C7 C8 . . 116.8(2) ?
C11 C7 C6 . . 119.3(2) ?
C8 C7 C6 . . 123.9(2) ?
C9 C8 C7 . . 119.9(3) ?
C9 C8 H8 . . 120.0 ?
C7 C8 H8 . . 120.0 ?
C8 C9 C10 . . 119.4(3) ?
C8 C9 H9 . . 120.3 ?
C10 C9 H9 . . 120.3 ?
N2 C10 C9 . . 122.8(2) ?
N2 C10 H10 . . 118.6 ?
C9 C10 H10 . . 118.6 ?
N2 C11 C7 . . 123.1(2) ?
N2 C11 C12 . . 117.3(2) ?
C7 C11 C12 . . 119.6(2) ?
N1 C12 C4 . . 123.3(2) ?
N1 C12 C11 . . 117.3(2) ?
C4 C12 C11 . . 119.4(2) ?
O2 C13 O1 . . 123.9(3) ?
O2 C13 C14 . . 118.5(2) ?
O1 C13 C14 . . 117.6(2) ?
C19 C14 C15 . . 117.9(2) ?
C19 C14 C13 . . 121.7(2) ?
C15 C14 C13 . . 120.3(2) ?
O3 C15 C16 . . 117.1(2) ?
O3 C15 C14 . . 122.9(2) ?
C16 C15 C14 . . 120.0(3) ?
C17 C16 C15 . . 119.7(3) ?
C17 C16 H16 . . 120.1 ?
C15 C16 H16 . . 120.1 ?
C16 C17 C18 . . 121.7(3) ?
C16 C17 Cl1 . . 119.1(2) ?
C18 C17 Cl1 . . 119.2(2) ?
C19 C18 C17 . . 118.5(3) ?
C19 C18 H18 . . 120.8 ?
C17 C18 H18 . . 120.8 ?
C18 C19 C14 . . 122.2(3) ?
C18 C19 H19 . . 118.9 ?
C14 C19 H19 . . 118.9 ?
O5 C20 O4 . . 123.9(3) ?
O5 C20 C21 . . 118.7(2) ?
O4 C20 C21 . . 117.4(2) ?
C26 C21 C22 . . 117.6(3) ?
C26 C21 C20 . . 121.1(2) ?
C22 C21 C20 . . 121.3(3) ?
O6 C22 C23 . . 117.3(3) ?
O6 C22 C21 . . 122.3(3) ?
C23 C22 C21 . . 120.4(3) ?
C24 C23 C22 . . 119.1(3) ?
C24 C23 H23 . . 120.4 ?
C22 C23 H23 . . 120.4 ?
C23 C24 C25 . . 122.3(3) ?
C23 C24 Cl2 . . 118.2(2) ?
C25 C24 Cl2 . . 119.5(3) ?
C26 C25 C24 . . 118.1(3) ?
C26 C25 H25 . . 120.9 ?
C24 C25 H25 . . 120.9 ?
C25 C26 C21 . . 122.4(3) ?
C25 C26 H26 . . 118.8 ?
C21 C26 H26 . . 118.8 ?
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
Zn O1 . 2.0155(18) y
Zn O4 . 2.0325(19) y
Zn O7 . 2.109(2) y
Zn N1 . 2.130(2) y
Zn N2 . 2.126(2) y
Cl1 C17 . 1.741(3) ?
Cl2 C24 . 1.743(3) ?
N1 C1 . 1.333(3) ?
N1 C12 . 1.360(3) ?
N2 C10 . 1.330(3) ?
N2 C11 . 1.361(3) ?
O1 C13 . 1.276(3) ?
O2 C13 . 1.259(3) ?
O3 C15 . 1.344(3) ?
O3 H3A . 0.9554 ?
O4 C20 . 1.261(3) ?
O5 C20 . 1.258(3) ?
O6 C22 . 1.347(4) ?
O6 H6A . 0.9509 ?
O7 H7A . 0.8559 ?
O7 H7B . 0.9565 ?
C1 C2 . 1.391(4) ?
C1 H1 . 0.9300 ?
C2 C3 . 1.366(4) ?
C2 H2 . 0.9300 ?
C3 C4 . 1.410(4) ?
C3 H3 . 0.9300 ?
C4 C12 . 1.408(4) ?
C4 C5 . 1.426(4) ?
C5 C6 . 1.351(4) ?
C5 H5 . 0.9300 ?
C6 C7 . 1.432(4) ?
C6 H6 . 0.9300 ?
C7 C11 . 1.405(4) ?
C7 C8 . 1.412(4) ?
C8 C9 . 1.358(4) ?
C8 H8 . 0.9300 ?
C9 C10 . 1.399(4) ?
C9 H9 . 0.9300 ?
C10 H10 . 0.9300 ?
C11 C12 . 1.442(3) ?
C13 C14 . 1.487(4) ?
C14 C19 . 1.400(4) ?
C14 C15 . 1.410(4) ?
C15 C16 . 1.396(4) ?
C16 C17 . 1.373(4) ?
C16 H16 . 0.9300 ?
C17 C18 . 1.387(4) ?
C18 C19 . 1.376(4) ?
C18 H18 . 0.9300 ?
C19 H19 . 0.9300 ?
C20 C21 . 1.496(4) ?
C21 C26 . 1.401(4) ?
C21 C22 . 1.407(4) ?
C22 C23 . 1.397(4) ?
C23 C24 . 1.376(5) ?
C23 H23 . 0.9300 ?
C24 C25 . 1.378(4) ?
C25 C26 . 1.377(4) ?
C25 H25 . 0.9300 ?
C26 H26 . 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 H3A O2 . 0.95 1.66 2.559(3) 155
O6 H6A O5 . 0.95 1.72 2.595(3) 151
O7 H7A O2 . 0.86 1.93 2.707(3) 150
O7 H7B O5 . 0.96 1.75 2.674(3) 163
