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_4317106
_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_moiety         'C8 H12 O12 Pb6, H2 O'
_chemical_formula_sum            'C8 H14 O13 Pb6'
_chemical_formula_weight         1561.39
_chemical_name_systematic
; 
 ? 
;
_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                112.322(2)
_cell_angle_beta                 101.107(2)
_cell_angle_gamma                90.740(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2427(9)
_cell_length_b                   11.5314(15)
_cell_length_c                   13.5236(18)
_cell_measurement_reflns_used    3284
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.98
_cell_measurement_theta_min      3.14
_cell_volume                     1020.6(2)
_computing_cell_refinement       'Bruker SAINT v7.60A'
_computing_data_collection       'Bruker APEX2 v2009.11.0'
_computing_data_reduction        'Bruker SAINT v7.60A'
_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; Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'omega/phi scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77490
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_sigmaI/netI    0.0663
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23403
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         34.26
_diffrn_reflns_theta_min         3.14
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    60.984
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.4157
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    5.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.007
_refine_diff_density_max         2.006
_refine_diff_density_min         -1.858
_refine_diff_density_rms         0.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         6214
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0138P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0783
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                4178
_reflns_number_total             6214
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101904j_si_001_1.cif
_cod_data_source_block           basic_lead_acetate_(1a)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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               4317106