#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/01/2010135.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_2010135
loop_
_publ_author_name
'Markus Schürmann'
'Friedo Huber'
_publ_section_title
;
 A redetermination of lead(IV) acetate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1710
_journal_page_last               1713
_journal_paper_doi               10.1107/S0108270194006438
_journal_volume                  50
_journal_year                    1994
_chemical_formula_structural     '[Pb(OAc)~4~]'
_chemical_formula_sum            'C8 H12 O8 Pb'
_chemical_formula_weight         443.36
_chemical_melting_point          .448E-305
_chemical_name_systematic
;
 Lead(IV) acetate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 103.71(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.781(3)
_cell_length_b                   26.726(9)
_cell_length_c                   12.781(8)
_cell_measurement_reflns_used    35
_cell_measurement_temperature    170.0(10)
_cell_measurement_theta_max      15.3
_cell_measurement_theta_min      7.7
_cell_volume                     2582(2)
_diffrn_ambient_temperature      170.0(10)
_diffrn_measurement_device       'Nicolet R3m/V'
_diffrn_measurement_method       ω/2θ
_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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4955
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_count 300
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    13.093
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.234
_exptl_absorpt_correction_type   'empirical, \y-scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.281
_exptl_crystal_description       block
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.20
_refine_diff_density_max         '2.374 (near Pb(2), 0.879(11) \%A)'
_refine_diff_density_min         -4.594
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.940
_refine_ls_goodness_of_fit_obs   1.077
_refine_ls_hydrogen_treatment    'only H atoms U refined'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     308
_refine_ls_number_reflns         4422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_restrained_S_obs      1.077
_refine_ls_R_factor_all          0.0893
_refine_ls_R_factor_obs          0.0585
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.1115P)^2^+0.0000P] where
 P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1786
_refine_ls_wR_factor_obs         0.1542
_reflns_number_observed          2948
_reflns_number_total             4436
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ab1189.cif
_cod_data_source_block           361
_cod_original_cell_volume        2582.(2)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C8 H12 O8 Pb1'
_cod_database_code               2010135
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_group
_atom_site_type_symbol
Pb(1) 0.23273(8) 0.11053(3) -0.61391(5) 0.0351(2) Uani d . 1 . Pb
O(1) 0.1223(14) 0.0531(4) -0.5154(9) 0.038(3) Uani d . 1 . O
O(2) 0.4026(16) 0.0662(5) -0.4787(9) 0.042(3) Uani d . 1 . O
C(1) 0.272(2) 0.0422(6) -0.4613(13) 0.031(4) Uani d . 1 . C
C(2) 0.300(2) 0.0028(7) -0.3745(12) 0.043(5) Uani d . 1 . C
H(2A) 0.427(2) -0.0004(7) -0.3413(12) 0.13(2) Uiso calc R 1 . H
H(2B) 0.254(2) -0.0294(7) -0.4061(12) 0.13(2) Uiso calc R 1 . H
H(2C) 0.237(2) 0.0125(7) -0.3196(12) 0.13(2) Uiso calc R 1 . H
O(3) 0.3185(16) 0.0522(5) -0.7223(10) 0.048(3) Uani d . 1 . O
O(4) 0.0459(17) 0.0739(5) -0.7566(11) 0.053(4) Uani d . 1 . O
C(3) 0.162(3) 0.0477(7) -0.7781(13) 0.039(4) Uani d . 1 . C
C(4) 0.125(3) 0.0131(8) -0.8762(14) 0.061(6) Uani d . 1 . C
H(4A) 0.234(3) -0.0046(8) -0.8796(14) 0.13(2) Uiso calc R 1 . H
H(4B) 0.084(3) 0.0330(8) -0.9418(14) 0.13(2) Uiso calc R 1 . H
H(4C) 0.034(3) -0.0112(8) -0.8700(14) 0.13(2) Uiso calc R 1 . H
O(5) -0.0159(17) 0.1538(5) -0.6140(13) 0.066(4) Uani d . 1 . O
O(6) 0.2220(18) 0.1719(5) -0.4881(11) 0.057(4) Uani d . 1 . O
C(5) 0.053(3) 0.1805(8) -0.5325(16) 0.056(6) Uani d . 1 . C
C(6) -0.044(3) 0.2183(8) -0.4894(16) 0.063(6) Uani d . 1 . C
H(6A) 0.035(3) 0.2342(8) -0.4269(16) 0.13(2) Uiso calc R 1 . H
H(6B) -0.144(3) 0.2028(8) -0.4673(16) 0.13(2) Uiso calc R 1 . H
H(6C) -0.088(3) 0.2436(8) -0.5446(16) 0.13(2) Uiso calc R 1 . H
O(7) 0.2743(18) 0.1693(5) -0.7361(10) 0.047(3) Uani d . 1 . O
O(8) 0.5019(17) 0.1432(5) -0.6086(12) 0.056(4) Uani d . 1 . O
C(7) 0.444(3) 0.1717(7) -0.6940(15) 0.045(5) Uani d . 1 . C
C(8) 0.553(3) 0.2059(9) -0.7404(16) 0.069(7) Uani d . 1 . C
H(8A 0.677(3) 0.2033(9) -0.7001(16) 0.13(2) Uiso calc R 1 . H
H(8B) 0.511(3) 0.2403(9) -0.7365(16) 0.13(2) Uiso calc R 1 . H
H(8C) 0.544(3) 0.1969(9) -0.8159(16) 0.13(2) Uiso calc R 1 . H
Pb(2) 0.23579(8) 0.13205(2) -0.13405(5) 0.0332(2) Uani d . 1 . Pb(
O(9) -0.0033(15) 0.1473(4) -0.2759(10) 0.043(3) Uani d . 1 . O
O(10) 0.0858(16) 0.0711(4) -0.2382(10) 0.046(3) Uani d . 1 . O
C(9) -0.024(2) 0.1002(7) -0.2919(14) 0.040(4) Uani d . 1 . C
C(10) -0.177(2) 0.0799(8) -0.3823(16) 0.057(6) Uani d . 1 . C
H(10A) -0.251(2) 0.1079(8) -0.4165(16) 0.13(2) Uiso calc R 1 . H
H(10B) -0.249(2) 0.0566(8) -0.3515(16) 0.13(2) Uiso calc R 1 . H
H(10C) -0.128(2) 0.0625(8) -0.4362(16) 0.13(2) Uiso calc R 1 . H
O(11) 0.0352(16) 0.1174(5) -0.0329(10) 0.045(3) Uani d . 1 . O
O(12) 0.1138(16) 0.1955(5) -0.0573(11) 0.050(3) Uani d . 1 . O
C(11) 0.022(2) 0.1645(7) -0.0137(16) 0.045(5) Uani d . 1 . C
C(12) -0.098(3) 0.1853(8) 0.0567(19) 0.063(6) Uani d . 1 . C
H(12A) -0.087(3) 0.2218(8) 0.0605(19) 0.13(2) Uiso calc R 1 . H
H(12B) -0.061(3) 0.1712(8) 0.1294(19) 0.13(2) Uiso calc R 1 . H
H(12C) -0.221(3) 0.1760(8) 0.0249(19) 0.13(2) Uiso calc R 1 . H
O(13) 0.3593(15) 0.1981(4) -0.1964(10) 0.042(3) Uani d . 1 . O
O(14) 0.4424(17) 0.1235(5) -0.2333(9) 0.046(3) Uani d . 1 . O
C(13) 0.457(2) 0.1708(7) -0.2422(14) 0.035(4) Uani d . 1 . C
C(14) 0.585(3) 0.1948(8) -0.3001(16) 0.062(6) Uani d . 1 . C
H(14A) 0.575(3) 0.2313(8) -0.2973(16) 0.13(2) Uiso calc R 1 . H
H(14B) 0.557(3) 0.1838(8) -0.3754(16) 0.13(2) Uiso calc R 1 . H
H(14C) 0.706(3) 0.1848(8) -0.2651(16) 0.13(2) Uiso calc R 1 . H
O(15) 0.3739(16) 0.0639(5) -0.0464(10) 0.047(3) Uani d . 1 . O
O(16) 0.4673(16) 0.1371(5) 0.0141(10) 0.041(3) Uani d . 1 . O
C(15) 0.481(2) 0.0903(6) 0.0242(16) 0.040(4) Uani d . 1 . C
C(16) 0.612(3) 0.0655(9) 0.1100(17) 0.069(7) Uani d . 1 . C
H(16A) 0.599(3) 0.0291(9) 0.1020(17) 0.13(2) Uiso calc R 1 . H
H(16B) 0.593(3) 0.0756(9) 0.1802(17) 0.13(2) Uiso calc R 1 . H
H(16C) 0.731(3) 0.0751(9) 0.1051(17) 0.13(2) Uiso calc R 1 . H
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_publ_flag
O(1) Pb(1) O(2) 56.7(4) yes
O(3) Pb(1) O(4) 56.1(4) yes
O(5) Pb(1) O(6) 57.6(5) yes
O(7) Pb(1) O(8) 58.3(5) yes
O(1) Pb(1) O(7) 166.1(4) yes
O(3) Pb(1) O(6) 165.5(5) yes
C(1) Pb(1) C(3) 96.5(5) yes
C(1) Pb(1) C(5) 100.1(5) yes
C(1) Pb(1) C(7) 136.8(6) yes
C(3) Pb(1) C(5) 136.0(7) yes
C(3) Pb(1) C(7) 96.6(5) yes
C(5) Pb(1) C(7) 98.4(7) yes
C(1) C(2) Pb(1) 178.3(12) yes
C(3) C(4) Pb(1) 177.2(13) yes
C(5) C(6) Pb(1) 179.6(14) yes
C(7) C(8) Pb(1) 177.8(16) yes
O(9) Pb(2) O(10) 56.9(4) yes
O(11) Pb(2) O(12) 58.2(4) yes
O(13) Pb(2) O(14) 57.6(4) yes
O(15) Pb(2) O(16) 56.7(4) yes
O(9) Pb(2) O(16) 166.2(4) yes
O(11) Pb(2) O(14) 164.3(5) yes
C(9) Pb(2) C(11) 94.4(5) yes
C(9) Pb(2) C(13) 101.6(5) yes
C(9) Pb(2) C(15) 136.4(6) yes
C(11) Pb(2) C(13) 138.0(6) yes
C(11) Pb(2) C(15) 97.5(6) yes
C(13) Pb(2) C(15) 97.0(5) yes
C(9) C(10) Pb(2) 178.1(14) yes
C(11) C(12) Pb(2) 177.7(14) yes
C(13) C(14) Pb(2) 177.4(14) yes
C(15) C(16) Pb(2) 177.7(14) yes
O(13) Pb(2) O(16) 85.9(4) ?
O(2) Pb(1) O(5) 128.3(5) ?
O(2) Pb(1) O(8) 79.0(5) ?
O(5) Pb(1) O(8) 126.3(6) ?
O(2) Pb(1) O(4) 122.6(5) ?
O(5) Pb(1) O(4) 80.5(5) ?
O(8) Pb(1) O(4) 127.2(5) ?
O(5) Pb(1) O(1) 84.8(5) ?
O(8) Pb(1) O(1) 135.5(4) ?
O(4) Pb(1) O(1) 84.2(5) ?
O(2) Pb(1) O(3) 84.5(4) ?
O(5) Pb(1) O(3) 136.3(5) ?
O(8) Pb(1) O(3) 83.1(5) ?
O(1) Pb(1) O(3) 94.5(5) ?
O(2) Pb(1) O(7) 137.1(5) ?
O(5) Pb(1) O(7) 84.7(6) ?
O(4) Pb(1) O(7) 85.1(5) ?
O(3) Pb(1) O(7) 86.9(5) ?
O(2) Pb(1) O(6) 87.2(5) ?
O(8) Pb(1) O(6) 83.7(5) ?
O(4) Pb(1) O(6) 138.1(5) ?
O(1) Pb(1) O(6) 90.7(5) ?
O(7) Pb(1) O(6) 91.3(5) ?
O(2) Pb(1) C(5) 109.5(5) ?
O(5) Pb(1) C(5) 28.1(6) ?
O(8) Pb(1) C(5) 106.5(6) ?
O(4) Pb(1) C(5) 108.6(6) ?
O(1) Pb(1) C(5) 87.4(5) ?
O(3) Pb(1) C(5) 164.1(6) ?
O(7) Pb(1) C(5) 87.6(6) ?
O(6) Pb(1) C(5) 29.5(6) ?
C(1) O(1) Pb(1) 92.3(10) ?
C(1) O(2) Pb(1) 93.0(10) ?
O(1) C(1) O(2) 118.0(16) ?
O(1) C(1) C(2) 121.8(16) ?
O(2) C(1) C(2) 120.2(15) ?
O(1) C(1) Pb(1) 59.7(9) ?
O(2) C(1) Pb(1) 58.4(8) ?
C(3) O(3) Pb(1) 91.5(11) ?
C(3) O(4) Pb(1) 93.5(11) ?
O(4) C(3) O(3) 118.8(16) ?
O(4) C(3) C(4) 121.7(18) ?
O(3) C(3) C(4) 119.2(18) ?
O(4) C(3) Pb(1) 58.9(9) ?
O(3) C(3) Pb(1) 59.9(9) ?
C(5) O(5) Pb(1) 95.4(13) ?
C(5) O(6) Pb(1) 91.3(11) ?
O(5) C(5) O(6) 115.7(17) ?
O(5) C(5) C(6) 123.(2) ?
O(6) C(5) C(6) 120.9(19) ?
O(5) C(5) Pb(1) 56.5(9) ?
O(6) C(5) Pb(1) 59.2(9) ?
C(7) O(7) Pb(1) 92.5(11) ?
C(7) O(8) Pb(1) 93.8(11) ?
O(7) C(7) O(8) 115.3(17) ?
O(7) C(7) C(8) 119.3(18) ?
O(8) C(7) C(8) 125.3(19) ?
O(7) C(7) Pb(1) 58.5(9) ?
O(8) C(7) Pb(1) 56.9(9) ?
O(13) Pb(2) O(10) 124.5(5) ?
O(13) Pb(2) O(15) 127.9(4) ?
O(10) Pb(2) O(15) 80.2(4) ?
O(13) Pb(2) O(12) 79.9(4) ?
O(10) Pb(2) O(12) 125.7(5) ?
O(15) Pb(2) O(12) 125.6(5) ?
O(10) Pb(2) O(14) 86.2(5) ?
O(15) Pb(2) O(14) 83.1(5) ?
O(12) Pb(2) O(14) 137.3(4) ?
O(13) Pb(2) O(11) 138.0(4) ?
O(10) Pb(2) O(11) 83.2(5) ?
O(15) Pb(2) O(11) 83.7(5) ?
O(10) Pb(2) O(16) 136.8(4) ?
O(12) Pb(2) O(16) 85.8(5) ?
O(14) Pb(2) O(16) 86.9(4) ?
O(11) Pb(2) O(16) 92.9(4) ?
O(13) Pb(2) O(9) 85.2(4) ?
O(15) Pb(2) O(9) 136.8(4) ?
O(12) Pb(2) O(9) 82.3(5) ?
O(14) Pb(2) O(9) 97.1(4) ?
O(11) Pb(2) O(9) 86.7(4) ?
C(9) O(9) Pb(2) 90.0(10) ?
C(9) O(10) Pb(2) 93.8(11) ?
O(10) C(9) O(9) 119.1(17) ?
O(10) C(9) C(10) 120.2(17) ?
O(9) C(9) C(10) 120.6(17) ?
O(10) C(9) Pb(2) 58.3(10) ?
O(9) C(9) Pb(2) 61.0(9) ?
C(11) O(11) Pb(2) 92.0(10) ?
C(11) O(12) Pb(2) 92.2(11) ?
O(11) C(11) O(12) 117.6(17) ?
O(11) C(11) C(12) 123.1(17) ?
O(12) C(11) C(12) 119.2(18) ?
O(11) C(11) Pb(2) 59.0(9) ?
O(12) C(11) Pb(2) 58.6(9) ?
C(13) O(13) Pb(2) 93.8(10) ?
C(13) O(14) Pb(2) 92.3(10) ?
O(14) C(13) O(13) 116.3(16) ?
O(14) C(13) C(14) 123.1(17) ?
O(13) C(13) C(14) 120.6(17) ?
O(14) C(13) Pb(2) 59.0(9) ?
O(13) C(13) Pb(2) 57.3(9) ?
C(15) O(15) Pb(2) 93.4(10) ?
C(15) O(16) Pb(2) 93.3(10) ?
O(16) C(15) O(15) 116.5(15) ?
O(16) C(15) C(16) 123.6(17) ?
O(15) C(15) C(16) 119.8(17) ?
O(16) C(15) Pb(2) 58.6(8) ?
O(15) C(15) Pb(2) 57.9(9) ?
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
Pb(1) O(1) . 2.278(11) yes
Pb(1) O(2) . 2.249(11) yes
Pb(1) O(3) . 2.287(13) yes
Pb(1) O(4) . 2.268(13) yes
Pb(1) O(5) . 2.253(11) yes
Pb(1) O(6) . 2.312(13) yes
Pb(1) O(7) . 2.292(12) yes
Pb(1) O(8) . 2.255(13) yes
Pb(1) C(1) . 2.64(2) yes
Pb(1) C(5) . 2.69(2) yes
Pb(1) C(3) . 2.64(2) yes
Pb(1) C(7) . 2.69(2) yes
Pb(2) O(9) . 2.305(11) yes
Pb(2) O(10) . 2.248(12) yes
Pb(2) O(11) . 2.284(12) yes
Pb(2) O(12) . 2.275(13) yes
Pb(2) O(13) . 2.244(12) yes
Pb(2) O(14) . 2.283(12) yes
Pb(2) O(15) . 2.271(12) yes
Pb(2) O(16) . 2.288(12) yes
Pb(2) C(9) . 2.64(2) yes
Pb(2) C(11) . 2.66(2) yes
Pb(2) C(13) . 2.66(2) yes
Pb(2) C(15) . 2.68(2) yes
O(1) C(1) . 1.24(2) ?
O(2) C(1) . 1.26(2) ?
C(1) C(2) . 1.51(2) ?
O(3) C(3) . 1.26(2) ?
O(4) C(3) . 1.22(2) ?
C(3) C(4) . 1.53(2) ?
O(5) C(5) . 1.27(2) ?
O(6) C(5) . 1.33(3) ?
C(5) C(6) . 1.44(3) ?
O(7) C(7) . 1.30(2) ?
O(8) C(7) . 1.32(2) ?
C(7) C(8) . 1.47(3) ?
O(9) C(9) . 1.28(2) ?
O(10) C(9) . 1.24(2) ?
C(9) C(10) . 1.55(2) ?
O(11) C(11) . 1.29(2) ?
O(12) C(11) . 1.30(2) ?
C(11) C(12) . 1.54(2) ?
O(13) C(13) . 1.29(2) ?
O(14) C(13) . 1.28(2) ?
C(13) C(14) . 1.52(2) ?
O(15) C(15) . 1.29(2) ?
O(16) C(15) . 1.26(2) ?
C(15) C(16) . 1.46(3) ?
