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_4317107
_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         1561.33
_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                113.354(3)
_cell_angle_beta                 100.108(3)
_cell_angle_gamma                90.270(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2637(16)
_cell_length_b                   11.548(3)
_cell_length_c                   13.778(3)
_cell_measurement_reflns_used    2338
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      31.20
_cell_measurement_theta_min      2.86
_cell_volume                     1041.0(4)
_computing_cell_refinement       'Apex2 v2009.7-0'
_computing_data_collection       'Apex2 v2009.7-0 (Bruker, 2009)'
_computing_data_reduction        'Apex2 v2009.7-0'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.911
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0375
_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       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23479
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         31.34
_diffrn_reflns_theta_min         1.64
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    48.396
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.2641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2  v2009.7-0 (Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    4.981
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.184
_refine_diff_density_min         -1.840
_refine_diff_density_rms         0.461
_refine_ls_extinction_coef       0.00070(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         6230
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0586
_refine_ls_R_factor_gt           0.0354
_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^)+(0.0468P)^2^+0.0302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0949
_refine_ls_wR_factor_ref         0.1213
_reflns_number_gt                4343
_reflns_number_total             6230
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101904j_si_001_2.cif
_cod_data_source_block           basic_lead_acetate_(1b)
_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_original_cell_volume        1041.1(4)
_cod_database_code               4317107