Synthesis and Structures of Pb3O2(CH3COO)2.0.5H2O and Pb2O(HCOO)2: Two Corrosion Products Revisited
Catherine M. Mauck; Titus W. P. van den Heuvel; Michaela M. Hull; Matthias Zeller; Catherine M. Oertel; Inorganic Chemistry 49 (2010) 10736–10743; doi:10.1021/ic101904j

data_4317108
_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       '\w 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/[\s^2^(Fo^2^)+(0.0558P)^2^+50.7940P] where P=(Fo^2^+2Fc^2^)/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>2\s(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