#------------------------------------------------------------------------------
#$Date: 2016-03-23 02:33:33 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179251 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/71/4317108.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4317108
loop_
_publ_author_name
'Catherine M. Mauck'
'Titus W. P. van den Heuvel'
'Michaela M. Hull'
'Matthias Zeller'
'Catherine M. Oertel'
_publ_contact_author
; Dr Catherine M. Oertel
Department of Chemistry and Biochemistry
Oberlin College 
Oberlin, OH  44074, USA 
;
_publ_contact_author_email       catherine.oertel@oberlin.edu
_publ_contact_author_fax         '440 775 6682'
_publ_contact_author_phone       '440 775 8989'
_publ_section_title
;
 Synthesis and Structures of Pb3O2(CH3COO)2.0.5H2O and Pb2O(HCOO)2: Two
 Corrosion Products Revisited
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10736
_journal_page_last               10743
_journal_paper_doi               10.1021/ic101904j
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C2 H2 O5 Pb2'
_chemical_formula_weight         520.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           66
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2 2c'
_symmetry_space_group_name_H-M   'C c c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3955(15)
_cell_length_b                   10.8276(17)
_cell_length_c                   5.8133(9)
_cell_measurement_reflns_used    3095
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.4985
_cell_measurement_theta_min      2.8705
_cell_volume                     591.39(16)
_computing_cell_refinement       'SAINT+ 6.45 (Bruker, 2003)'
_computing_data_collection       'SMART 5.630 (Bruker, 1997-2002)'
_computing_data_reduction        'SAINT+ 6.45'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_structure_solution    'SHELXTL 6.14 (Bruker, 2000-2003)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_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  0.0334
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2265
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    56.806
_exptl_absorpt_correction_T_max  0.321
_exptl_absorpt_correction_T_min  0.056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS in SAINT+ (Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.845
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.910
_refine_diff_density_min         -4.119
_refine_diff_density_rms         0.717
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.289
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     37
_refine_ls_number_reflns         409
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.265
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_gt           0.0340
_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)+(0.0558P)²+50.7940P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1030
_reflns_number_gt                407
_reflns_number_total             409
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic101904j_si_001_3.cif
_cod_data_source_block           basic_lead_formate_(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4317108
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 1.13583(6) 0.38183(5) 0.0000 0.0039(3) Uani 1 2 d S . .
O1 O 1.0000 0.5000 0.2500 0.016(4) Uani 1 4 d S . .
C1 C 0.876(2) 0.134(2) 0.047(5) 0.009(4) Uani 0.50 1 d PU . -1
H1B H 0.9069 0.1118 -0.1025 0.011 Uiso 0.50 1 calc PR . -1
O2 O 0.9204(16) 0.2365(14) 0.125(3) 0.009(3) Uani 0.50 1 d PU . -1
O3 O 0.7973(16) 0.0608(14) 0.146(3) 0.010(3) Uani 0.50 1 d PU . -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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Pb1 O1 77.614(19) 9_765 . ?
O1 Pb1 O3 96.5(4) 9_765 5 ?
O1 Pb1 O3 72.9(4) . 5 ?
O1 Pb1 O3 72.9(4) 9_765 14 ?
O1 Pb1 O3 96.5(4) . 14 ?
O3 Pb1 O3 38.0(8) 5 14 ?
O1 Pb1 O3 132.6(3) 9_765 8 ?
O1 Pb1 O3 72.3(4) . 8 ?
O3 Pb1 O3 40.0(7) 5 8 ?
O3 Pb1 O3 75.1(4) 14 8 ?
O1 Pb1 O3 72.3(4) 9_765 15 ?
O1 Pb1 O3 132.6(3) . 15 ?
O3 Pb1 O3 75.1(4) 5 15 ?
O3 Pb1 O3 40.0(7) 14 15 ?
O3 Pb1 O3 103.0(7) 8 15 ?
O1 Pb1 O2 74.8(4) 9_765 10 ?
O1 Pb1 O2 94.5(4) . 10 ?
O3 Pb1 O2 166.2(5) 5 10 ?
O3 Pb1 O2 142.5(6) 14 10 ?
O3 Pb1 O2 142.2(5) 8 10 ?
O3 Pb1 O2 111.3(5) 15 10 ?
O1 Pb1 O2 94.5(4) 9_765 . ?
O1 Pb1 O2 74.8(4) . . ?
O3 Pb1 O2 142.5(6) 5 . ?
O3 Pb1 O2 166.2(5) 14 . ?
O3 Pb1 O2 111.3(5) 8 . ?
O3 Pb1 O2 142.2(5) 15 . ?
O2 Pb1 O2 31.6(8) 10 . ?
O1 Pb1 O2 73.3(3) 9_765 12_755 ?
O1 Pb1 O2 135.2(3) . 12_755 ?
O3 Pb1 O2 143.0(5) 5 12_755 ?
O3 Pb1 O2 106.3(5) 14 12_755 ?
O3 Pb1 O2 150.4(5) 8 12_755 ?
O3 Pb1 O2 67.9(5) 15 12_755 ?
O2 Pb1 O2 45.4(7) 10 12_755 ?
O2 Pb1 O2 74.4(4) . 12_755 ?
O1 Pb1 O2 135.2(3) 9_765 3_755 ?
O1 Pb1 O2 73.3(3) . 3_755 ?
O3 Pb1 O2 106.3(5) 5 3_755 ?
O3 Pb1 O2 143.0(5) 14 3_755 ?
O3 Pb1 O2 67.9(5) 8 3_755 ?
O3 Pb1 O2 150.4(5) 15 3_755 ?
O2 Pb1 O2 74.4(4) 10 3_755 ?
O2 Pb1 O2 45.4(7) . 3_755 ?
O2 Pb1 O2 105.4(7) 12_755 3_755 ?
O1 Pb1 Pb1 140.505(11) 9_765 13_755 ?
O1 Pb1 Pb1 140.505(11) . 13_755 ?
O3 Pb1 Pb1 104.2(3) 5 13_755 ?
O3 Pb1 Pb1 104.2(3) 14 13_755 ?
O3 Pb1 Pb1 80.9(3) 8 13_755 ?
O3 Pb1 Pb1 80.9(3) 15 13_755 ?
O2 Pb1 Pb1 89.1(3) 10 13_755 ?
O2 Pb1 Pb1 89.1(3) . 13_755 ?
O2 Pb1 Pb1 69.9(3) 12_755 13_755 ?
O2 Pb1 Pb1 69.9(3) 3_755 13_755 ?
O1 Pb1 Pb1 38.807(10) 9_765 9_765 ?
O1 Pb1 Pb1 38.807(10) . 9_765 ?
O3 Pb1 Pb1 83.4(3) 5 9_765 ?
O3 Pb1 Pb1 83.4(3) 14 9_765 ?
O3 Pb1 Pb1 103.9(3) 8 9_765 ?
O3 Pb1 Pb1 103.9(3) 15 9_765 ?
O2 Pb1 Pb1 83.2(3) 10 9_765 ?
O2 Pb1 Pb1 83.2(3) . 9_765 ?
O2 Pb1 Pb1 105.7(3) 12_755 9_765 ?
O2 Pb1 Pb1 105.7(3) 3_755 9_765 ?
Pb1 Pb1 Pb1 172.00(4) 13_755 9_765 ?
Pb1 O1 Pb1 102.387(19) . 9_765 ?
Pb1 O1 Pb1 113.03(3) . 3_755 ?
Pb1 O1 Pb1 113.22(3) 9_765 3_755 ?
Pb1 O1 Pb1 113.22(3) . 11_566 ?
Pb1 O1 Pb1 113.03(3) 9_765 11_566 ?
Pb1 O1 Pb1 102.388(19) 3_755 11_566 ?
O3 C1 O2 127(3) . . ?
O3 C1 H1B 116.6 . . ?
O2 C1 H1B 116.6 . . ?
C1 O2 Pb1 132.1(16) . . ?
C1 O2 Pb1 136.2(16) . 3_755 ?
Pb1 O2 Pb1 91.4(5) . 3_755 ?
C1 O3 Pb1 133.0(18) . 5_445 ?
C1 O3 Pb1 124.0(15) . 15_456 ?
Pb1 O3 Pb1 95.4(5) 5_445 15_456 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pb1 O1 2.3190(4) 9_765 ?
Pb1 O1 2.3190(4) . ?
Pb1 O3 2.603(16) 5 ?
Pb1 O3 2.603(16) 14 ?
Pb1 O3 2.632(17) 8 ?
Pb1 O3 2.632(17) 15 ?
Pb1 O2 2.664(15) 10 ?
Pb1 O2 2.664(15) . ?
Pb1 O2 2.741(17) 12_755 ?
Pb1 O2 2.741(17) 3_755 ?
O1 Pb1 2.3190(5) 9_765 ?
O1 Pb1 2.3190(5) 3_755 ?
O1 Pb1 2.3191(5) 11_566 ?
C1 O3 1.23(3) . ?
C1 O2 1.27(3) . ?
C1 H1B 0.9500 . ?
O2 Pb1 2.741(17) 3_755 ?
O3 Pb1 2.603(16) 5_445 ?
O3 Pb1 2.632(17) 15_456 ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Pb1 O1 Pb1 0.0 9_765 . . 9_765 ?
O3 Pb1 O1 Pb1 100.9(4) 5 . . 9_765 ?
O3 Pb1 O1 Pb1 70.8(4) 14 . . 9_765 ?
O3 Pb1 O1 Pb1 142.9(4) 8 . . 9_765 ?
O3 Pb1 O1 Pb1 51.3(5) 15 . . 9_765 ?
O2 Pb1 O1 Pb1 -73.3(4) 10 . . 9_765 ?
O2 Pb1 O1 Pb1 -98.2(4) . . . 9_765 ?
O2 Pb1 O1 Pb1 -50.3(5) 12_755 . . 9_765 ?
O2 Pb1 O1 Pb1 -145.5(3) 3_755 . . 9_765 ?
Pb1 Pb1 O1 Pb1 -167.36(6) 13_755 . . 9_765 ?
O1 Pb1 O1 Pb1 122.142(18) 9_765 . . 3_755 ?
O3 Pb1 O1 Pb1 -136.9(4) 5 . . 3_755 ?
O3 Pb1 O1 Pb1 -167.0(4) 14 . . 3_755 ?
O3 Pb1 O1 Pb1 -94.9(4) 8 . . 3_755 ?
O3 Pb1 O1 Pb1 173.5(5) 15 . . 3_755 ?
O2 Pb1 O1 Pb1 48.8(4) 10 . . 3_755 ?
O2 Pb1 O1 Pb1 23.9(4) . . . 3_755 ?
O2 Pb1 O1 Pb1 71.9(5) 12_755 . . 3_755 ?
O2 Pb1 O1 Pb1 -23.4(3) 3_755 . . 3_755 ?
Pb1 Pb1 O1 Pb1 -45.22(4) 13_755 . . 3_755 ?
Pb1 Pb1 O1 Pb1 122.142(18) 9_765 . . 3_755 ?
O1 Pb1 O1 Pb1 -122.008(18) 9_765 . . 11_566 ?
O3 Pb1 O1 Pb1 -21.1(4) 5 . . 11_566 ?
O3 Pb1 O1 Pb1 -51.2(4) 14 . . 11_566 ?
O3 Pb1 O1 Pb1 20.9(4) 8 . . 11_566 ?
O3 Pb1 O1 Pb1 -70.7(5) 15 . . 11_566 ?
O2 Pb1 O1 Pb1 164.7(4) 10 . . 11_566 ?
O2 Pb1 O1 Pb1 139.8(4) . . . 11_566 ?
O2 Pb1 O1 Pb1 -172.3(5) 12_755 . . 11_566 ?
O2 Pb1 O1 Pb1 92.5(3) 3_755 . . 11_566 ?
Pb1 Pb1 O1 Pb1 70.63(4) 13_755 . . 11_566 ?
Pb1 Pb1 O1 Pb1 -122.008(18) 9_765 . . 11_566 ?
O3 C1 O2 Pb1 162.3(16) . . . . ?
O3 C1 O2 Pb1 -9(4) . . . 3_755 ?
O1 Pb1 O2 C1 92(2) 9_765 . . . ?
O1 Pb1 O2 C1 168(2) . . . . ?
O3 Pb1 O2 C1 -161.1(18) 5 . . . ?
O3 Pb1 O2 C1 116(3) 14 . . . ?
O3 Pb1 O2 C1 -129(2) 8 . . . ?
O3 Pb1 O2 C1 25(2) 15 . . . ?
O2 Pb1 O2 C1 41(2) 10 . . . ?
O2 Pb1 O2 C1 21(2) 12_755 . . . ?
O2 Pb1 O2 C1 -111(2) 3_755 . . . ?
Pb1 Pb1 O2 C1 -49(2) 13_755 . . . ?
Pb1 Pb1 O2 C1 129(2) 9_765 . . . ?
O1 Pb1 O2 Pb1 -94.2(4) 9_765 . . 3_755 ?
O1 Pb1 O2 Pb1 -18.4(3) . . . 3_755 ?
O3 Pb1 O2 Pb1 12.7(10) 5 . . 3_755 ?
O3 Pb1 O2 Pb1 -70(2) 14 . . 3_755 ?
O3 Pb1 O2 Pb1 45.2(6) 8 . . 3_755 ?
O3 Pb1 O2 Pb1 -161.0(6) 15 . . 3_755 ?
O2 Pb1 O2 Pb1 -145.1(3) 10 . . 3_755 ?
O2 Pb1 O2 Pb1 -165.5(5) 12_755 . . 3_755 ?
O2 Pb1 O2 Pb1 63.0(7) 3_755 . . 3_755 ?
Pb1 Pb1 O2 Pb1 125.1(4) 13_755 . . 3_755 ?
Pb1 Pb1 O2 Pb1 -57.0(3) 9_765 . . 3_755 ?
O2 C1 O3 Pb1 160.0(16) . . . 5_445 ?
O2 C1 O3 Pb1 18(3) . . . 15_456 ?
