#------------------------------------------------------------------------------
#$Date: 2016-02-20 22:30:07 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176789 $
#$URL: svn://www.crystallography.net/cod/cif/2/22/52/2225285.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_2225285
loop_
_publ_author_name
'Xiao, Jun-Xia'
'Wu, Xian-Ge'
'Qin, Liang'
_publ_section_title
;catena-Poly[[[aqua[(2-hydroxyphenyl)acetato-κ²O,O']lead(II)]-μ₃-[(2-hydroxyphenyl)acetato-κ⁴O:O,O':O']]
 monohydrate]
;
_journal_coeditor_code           HY2276
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m273
_journal_page_last               m274
_journal_paper_doi               10.1107/S1600536810004162
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[Pb (C8 H7 O3)2 (H2 O)], H2 O'
_chemical_formula_moiety         'C16 H16 O7 Pb, H2 O'
_chemical_formula_sum            'C16 H18 O8 Pb'
_chemical_formula_weight         545.50
_chemical_name_systematic
;
catena-Poly[[[aqua[(2-hydroxyphenyl)acetato-
κ²O,O']lead(II)]-μ₃-[(2-hydroxyphenyl)acetato-
κ⁴O:O,O':O']] monohydrate]
;
_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                109.72(3)
_cell_angle_beta                 90.10(3)
_cell_angle_gamma                102.92(3)
_cell_formula_units_Z            2
_cell_length_a                   7.4610(15)
_cell_length_b                   10.721(2)
_cell_length_c                   11.701(2)
_cell_measurement_reflns_used    2895
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.35
_cell_volume                     855.7(3)
_computing_cell_refinement       'CrystalStructure (Rigaku/MSC, 2002)'
_computing_data_collection       'CrystalStructure (Rigaku/MSC, 2002)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku/MSC Mercury 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  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0699
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6821
_diffrn_reflns_theta_full        25.20
_diffrn_reflns_theta_max         25.20
_diffrn_reflns_theta_min         3.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.900
_exptl_absorpt_correction_T_max  0.126
_exptl_absorpt_correction_T_min  0.075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(REQAB; Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.117
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.22
_refine_diff_density_max         2.769
_refine_diff_density_min         -1.582
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         3076
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0431P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0840
_reflns_number_gt                2951
_reflns_number_total             3076
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            hy2276.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 'Triclinic' changed to 'triclinic'
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_database_code               2225285
_cod_database_fobs_code          2225285
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_disorder_assembly
_atom_site_disorder_group
Pb Pb1 0.76187(2) 0.029805(17) 0.601979(13) 0.02638(11) Uani d . 1 . .
O O1 0.6798(6) 0.2761(5) 0.6889(4) 0.0433(10) Uani d . 1 . .
O O2 0.9615(6) 0.2666(4) 0.6423(4) 0.0439(10) Uani d . 1 . .
O O6 0.7995(6) -0.2407(5) 0.1437(5) 0.0487(11) Uani d . 1 . .
H H6 0.8311 -0.3082 0.1465 0.073 Uiso calc R 1 . .
O O5 1.1923(6) 0.5007(4) 0.8890(3) 0.0413(9) Uani d . 1 . .
H H5 1.2721 0.5388 0.9460 0.062 Uiso calc R 1 . .
C C1 0.8449(8) 0.3338(6) 0.6845(5) 0.0320(12) Uani d . 1 . .
C C2 0.9012(8) 0.4889(6) 0.7318(6) 0.0435(14) Uani d . 1 . .
H H2A 0.8219 0.5223 0.6892 0.052 Uiso calc R 1 . .
H H2B 0.8802 0.5217 0.8175 0.052 Uiso calc R 1 . .
C C3 1.0981(8) 0.5484(5) 0.7178(5) 0.0392(13) Uani d . 1 . .
C C4 1.1459(10) 0.6010(6) 0.6257(6) 0.0471(15) Uani d . 1 . .
H H4 1.0530 0.6059 0.5753 0.056 Uiso calc R 1 . .
C C5 1.3273(10) 0.6461(7) 0.6070(6) 0.0512(17) Uani d . 1 . .
H H5A 1.3558 0.6801 0.5442 0.061 Uiso calc R 1 . .
C C6 1.4641(10) 0.6410(7) 0.6797(6) 0.0531(17) Uani d . 1 . .
H H6A 1.5865 0.6687 0.6652 0.064 Uiso calc R 1 . .
C C7 1.4221(9) 0.5938(6) 0.7770(6) 0.0443(14) Uani d . 1 . .
H H7 1.5162 0.5935 0.8289 0.053 Uiso calc R 1 . .
C C8 1.2403(8) 0.5481(5) 0.7949(5) 0.0340(12) Uani d . 1 . .
C C9 0.7658(7) 0.0291(5) 0.3582(5) 0.0269(11) Uani d . 1 . .
C C10 0.7743(8) 0.0257(7) 0.2278(5) 0.0324(12) Uani d . 1 . .
H H10A 0.6655 -0.0388 0.1794 0.039 Uiso calc R 1 . .
H H10B 0.7718 0.1151 0.2260 0.039 Uiso calc R 1 . .
C C11 0.9411(7) -0.0131(6) 0.1715(4) 0.0296(12) Uani d . 1 . .
C C12 0.9491(7) -0.1495(6) 0.1294(4) 0.0300(12) Uani d . 1 . .
C C13 1.1053(8) -0.1886(7) 0.0786(5) 0.0407(14) Uani d . 1 . .
H H13 1.1097 -0.2799 0.0523 0.049 Uiso calc R 1 . .
C C14 1.2530(9) -0.0917(8) 0.0675(6) 0.0448(16) Uani d . 1 . .
H H14 1.3572 -0.1176 0.0332 0.054 Uiso calc R 1 . .
C C15 1.2474(9) 0.0435(7) 0.1069(5) 0.0478(18) Uani d . 1 . .
H H15 1.3478 0.1088 0.0996 0.057 Uiso calc R 1 . .
C C16 1.0910(9) 0.0828(6) 0.1580(5) 0.0390(14) Uani d . 1 . .
H H16 1.0871 0.1741 0.1833 0.047 Uiso calc R 1 . .
O O3 0.9083(5) 0.0283(4) 0.4142(3) 0.0339(9) Uani d . 1 . .
O O4 0.6204(5) 0.0363(4) 0.4101(3) 0.0366(9) Uani d . 1 . .
O O1W 0.6888(6) -0.2332(5) 0.4561(4) 0.0531(12) Uani d D 1 . .
H H2W 0.7696 -0.2339 0.4061 0.080 Uiso d RD 1 . .
H H1W 0.5860 -0.2720 0.4161 0.080 Uiso d RD 1 . .
O O2W 0.4261(6) 0.6318(6) 0.0817(4) 0.0617(14) Uani d D 1 . .
H H3W 0.3977 0.6548 0.1537 0.093 Uiso d RD 1 . .
H H4W 0.5291 0.6783 0.0746 0.093 Uiso d RD 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 '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
O3 Pb1 O4 . . 51.86(12) ?
O3 Pb1 O2 . . 72.89(14) ?
O4 Pb1 O2 . . 89.65(15) ?
O3 Pb1 O3 . 2_756 64.41(14) ?
O4 Pb1 O3 . 2_756 115.37(11) ?
O2 Pb1 O3 . 2_756 80.89(13) ?
O3 Pb1 O1W . . 74.25(14) ?
O4 Pb1 O1W . . 77.54(15) ?
O2 Pb1 O1W . . 145.72(13) ?
O3 Pb1 O1W 2_756 . 76.41(14) ?
O3 Pb1 O1 . . 104.29(14) ?
O4 Pb1 O1 . . 80.18(14) ?
O2 Pb1 O1 . . 49.36(13) ?
O3 Pb1 O1 2_756 . 128.80(13) ?
O1 Pb1 O4 . 2_656 76.94(13) ?
O2 Pb1 O4 . 2_656 125.05(14) ?
O3 Pb1 O4 . 2_656 117.78(12) ?
O3 Pb1 O4 2_756 2_656 154.01(12) ?
O4 Pb1 O4 . 2_656 67.94(11) ?
O1W Pb1 O4 . 2_656 79.49(13) ?
O1W Pb1 O1 . . 152.25(15) ?
C1 O1 Pb1 . . 90.2(4) ?
C1 O2 Pb1 . . 98.8(3) ?
C12 O6 H6 . . 109.5 ?
C8 O5 H5 . . 109.5 ?
O2 C1 O1 . . 121.5(5) ?
O2 C1 C2 . . 120.0(5) ?
O1 C1 C2 . . 118.5(5) ?
C3 C2 C1 . . 114.7(5) ?
C3 C2 H2A . . 108.6 ?
C1 C2 H2A . . 108.6 ?
C3 C2 H2B . . 108.6 ?
C1 C2 H2B . . 108.6 ?
H2A C2 H2B . . 107.6 ?
C4 C3 C8 . . 117.8(6) ?
C4 C3 C2 . . 121.6(6) ?
C8 C3 C2 . . 120.6(6) ?
C5 C4 C3 . . 121.5(7) ?
C5 C4 H4 . . 119.2 ?
C3 C4 H4 . . 119.2 ?
C6 C5 C4 . . 120.1(6) ?
C6 C5 H5A . . 119.9 ?
C4 C5 H5A . . 119.9 ?
C5 C6 C7 . . 120.2(6) ?
C5 C6 H6A . . 119.9 ?
C7 C6 H6A . . 119.9 ?
C8 C7 C6 . . 119.5(6) ?
C8 C7 H7 . . 120.2 ?
C6 C7 H7 . . 120.2 ?
O5 C8 C7 . . 121.6(6) ?
O5 C8 C3 . . 117.7(5) ?
C7 C8 C3 . . 120.7(6) ?
O3 C9 O4 . . 120.4(5) ?
O3 C9 C10 . . 118.9(4) ?
O4 C9 C10 . . 120.6(5) ?
C11 C10 C9 . . 113.5(4) ?
C11 C10 H10A . . 108.9 ?
C9 C10 H10A . . 108.9 ?
C11 C10 H10B . . 108.9 ?
C9 C10 H10B . . 108.9 ?
H10A C10 H10B . . 107.7 ?
C12 C11 C16 . . 118.2(5) ?
C12 C11 C10 . . 119.8(5) ?
C16 C11 C10 . . 122.1(5) ?
O6 C12 C11 . . 116.6(5) ?
O6 C12 C13 . . 122.3(5) ?
C11 C12 C13 . . 121.1(5) ?
C14 C13 C12 . . 119.7(6) ?
C14 C13 H13 . . 120.1 ?
C12 C13 H13 . . 120.1 ?
C15 C14 C13 . . 120.3(6) ?
C15 C14 H14 . . 119.9 ?
C13 C14 H14 . . 119.9 ?
C14 C15 C16 . . 120.0(6) ?
C14 C15 H15 . . 120.0 ?
C16 C15 H15 . . 120.0 ?
C11 C16 C15 . . 120.7(6) ?
C11 C16 H16 . . 119.6 ?
C15 C16 H16 . . 119.6 ?
C9 O3 Pb1 . . 95.1(3) ?
C9 O3 Pb1 . 2_756 146.8(3) ?
Pb1 O3 Pb1 . 2_756 115.59(14) ?
C9 O4 Pb1 . . 92.5(3) ?
H2W O1W H1W . . 107.6 ?
H3W O2W H4W . . 112.2 ?
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
Pb1 O1 . 2.701(5) y
Pb1 O2 . 2.527(4) y
Pb1 O3 . 2.453(3) y
Pb1 O3 2_756 2.662(4) y
Pb1 O4 . 2.508(4) y
Pb1 O4 2_656 2.772(4) y
Pb1 O1W . 2.687(4) y
O1 C1 . 1.259(7) ?
O2 C1 . 1.249(7) ?
O6 C12 . 1.362(7) ?
O6 H6 . 0.8200 ?
O5 C8 . 1.377(7) ?
O5 H5 . 0.8200 ?
C1 C2 . 1.521(8) ?
C2 C3 . 1.499(8) ?
C2 H2A . 0.9700 ?
C2 H2B . 0.9700 ?
C3 C4 . 1.389(9) ?
C3 C8 . 1.393(8) ?
C4 C5 . 1.376(10) ?
C4 H4 . 0.9300 ?
C5 C6 . 1.349(10) ?
C5 H5A . 0.9300 ?
C6 C7 . 1.403(9) ?
C6 H6A . 0.9300 ?
C7 C8 . 1.377(8) ?
C7 H7 . 0.9300 ?
C9 O3 . 1.251(6) ?
C9 O4 . 1.249(6) ?
C9 C10 . 1.515(7) ?
C10 C11 . 1.485(7) ?
C10 H10A . 0.9700 ?
C10 H10B . 0.9700 ?
C11 C12 . 1.392(8) ?
C11 C16 . 1.388(8) ?
C12 C13 . 1.393(8) ?
C13 C14 . 1.375(9) ?
C13 H13 . 0.9300 ?
C14 C15 . 1.375(9) ?
C14 H14 . 0.9300 ?
C15 C16 . 1.396(9) ?
C15 H15 . 0.9300 ?
C16 H16 . 0.9300 ?
O1W H2W . 0.8401 ?
O1W H1W . 0.8400 ?
O2W H3W . 0.8365 ?
O2W H4W . 0.8383 ?
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
_geom_hbond_publ_flag
O5 H5 O2W 1_656 0.82 1.80 2.618(6) 173 y
O6 H6 O5 2_756 0.82 1.93 2.698(6) 156 y
O1W H1W O1 2_656 0.84 2.31 3.089(6) 154 y
O1W H2W O2 2_756 0.84 2.16 2.900(6) 147 y
O2W H3W O1 2_666 0.84 1.88 2.715(6) 172 y
O2W H4W O6 1_565 0.84 2.05 2.788(7) 146 y
