#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:40:25 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179256 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/76/4317667.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_4317667
loop_
_publ_author_name
'Philip M. Almond'
'Thomas E. Albrecht-Schmitt'
_publ_contact_author
;
Prof. Thomas E. Albrecht-Schmitt
179 Chemistry Building
Department of Chemistry
Auburn University, AL
36849
;
_publ_contact_author_email       ' albreth@auburn.edu '
_publ_contact_author_fax         ' 334 844 6959 '
_publ_contact_author_phone       ' 334 844 6948 '
_publ_section_title
;
 Hydrothermal Syntheses, Structures, and Properties of the New Uranyl
 Selenites Ag2(UO2)(SeO3)2, M[(UO2)(HSeO3)(SeO3)] (M = K, Rb, Cs, Tl), and
 Pb(UO2)(SeO3)2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1177
_journal_page_last               1183
_journal_paper_doi               10.1021/ic0110732
_journal_volume                  41
_journal_year                    2002
_chemical_compound_source        'original synthesis'
_chemical_formula_structural     Pb(UO2)(SeO3)2
_chemical_formula_sum            'O8 Pb Se2 U'
_chemical_formula_weight         731.14
_chemical_name_systematic
;
   ?
;
_space_group_IT_number           26
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2'
_symmetry_space_group_name_H-M   'P m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.9911(7)
_cell_length_b                   5.7814(3)
_cell_length_c                   11.2525(6)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      1.70
_cell_volume                     780.08(7)
_computing_cell_refinement       'SMART, SAINT'
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-93 (Sheldrick, 1993)'
_computing_publication_material  'SHELXCIF-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Bruker APEX'
_diffrn_measurement_method       '0.3 wide w/ exposures'
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0420
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7421
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.70
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count na
_diffrn_standards_interval_time  na
_diffrn_standards_number         na
_exptl_absorpt_coefficient_mu    51.625
_exptl_absorpt_correction_T_max  '0.646955 ratio min/max'
_exptl_absorpt_correction_T_min  '0.646955 ratio min/max'
_exptl_absorpt_correction_type   'multiscan (SADABS)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    6.225
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    calcd
_exptl_crystal_description       prism
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.448
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.593
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.255
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.025(10)
_refine_ls_extinction_coef       0.00400(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.800
_refine_ls_goodness_of_fit_obs   0.801
_refine_ls_hydrogen_treatment    na
_refine_ls_matrix_type           full
_refine_ls_number_parameters     120
_refine_ls_number_reflns         2015
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.800
_refine_ls_restrained_S_obs      0.801
_refine_ls_R_factor_all          0.0196
_refine_ls_R_factor_obs          0.0193
_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
   [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
     [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l]
   where P = 1.00000Fo^2^ + 0.00000Fc^2^
;
_refine_ls_wR_factor_all         0.0514
_refine_ls_wR_factor_obs         0.0512
_reflns_number_observed          1992
_reflns_number_total             2015
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic0110732_6.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'nm' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               4317667
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y, z+1/2'
'-x, y, z'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
U1 U 0.25133(2) -0.00309(5) -0.27474(4) 0.00939(8) Uani 1 d . .
Pb1 Pb 0.0000 0.04743(7) -0.02335(4) 0.01439(10) Uani 1 d S .
Pb2 Pb 0.5000 -0.51038(6) -0.22437(4) 0.01186(10) Uani 1 d S .
Se1 Se 0.23407(6) -0.37615(13) -0.05023(7) 0.0125(2) Uani 1 d . .
Se2 Se 0.0000 0.4017(2) -0.28408(9) 0.0105(2) Uani 1 d S .
Se3 Se 0.5000 -0.8620(2) 0.03151(10) 0.0118(2) Uani 1 d S .
O1 O 0.2805(5) -0.2574(9) 0.0777(5) 0.0163(10) Uani 1 d . .
O2 O 0.3338(4) -0.3116(9) -0.1523(5) 0.0169(11) Uani 1 d . .
O3 O 0.1485(4) -0.1660(10) -0.1085(5) 0.0183(11) Uani 1 d . .
O4 O 0.1087(4) 0.2513(10) -0.2245(5) 0.0226(12) Uani 1 d . .
O5 O 0.0000 -0.3204(14) 0.0732(7) 0.019(2) Uani 1 d S .
O6 O 0.3945(8) -0.8366(14) 0.1305(8) 0.062(3) Uani 1 d . .
O7 O 0.5000 -0.5929(12) -0.0227(8) 0.027(2) Uani 1 d S .
O8 O 0.1581(5) -0.1725(11) -0.3640(5) 0.0253(13) Uani 1 d . .
O9 O 0.3414(4) 0.1717(9) -0.1842(5) 0.0193(11) Uani 1 d . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'
U U -9.6767 9.6646 '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
O8 U1 O9 178.4(3) . . ?
O8 U1 O6 89.1(4) . 3_544 ?
O9 U1 O6 92.4(4) . 3_544 ?
O8 U1 O1 92.8(2) . 3_554 ?
O9 U1 O1 87.1(2) . 3_554 ?
O6 U1 O1 78.9(2) 3_544 3_554 ?
O8 U1 O4 91.3(2) . . ?
O9 U1 O4 87.1(2) . . ?
O6 U1 O4 161.5(2) 3_544 . ?
O1 U1 O4 82.6(2) 3_554 . ?
O8 U1 O3 84.4(2) . . ?
O9 U1 O3 95.0(2) . . ?
O6 U1 O3 126.8(2) 3_544 . ?
O1 U1 O3 154.0(2) 3_554 . ?
O4 U1 O3 71.6(2) . . ?
O8 U1 O2 99.7(2) . . ?
O9 U1 O2 81.3(2) . . ?
O6 U1 O2 69.9(2) 3_544 . ?
O1 U1 O2 146.0(2) 3_554 . ?
O4 U1 O2 128.2(2) . . ?
O3 U1 O2 59.5(2) . . ?
O8 U1 Se1 91.9(2) . . ?
O9 U1 Se1 88.4(2) . . ?
O6 U1 Se1 98.2(2) 3_544 . ?
O1 U1 Se1 174.43(14) 3_554 . ?
O4 U1 Se1 100.35(14) . . ?
O3 U1 Se1 29.91(12) . . ?
O2 U1 Se1 29.60(12) . . ?
O3 Pb1 O3 97.5(3) 4 . ?
O3 Pb1 O5 73.8(2) 4 . ?
O3 Pb1 O5 73.8(2) . . ?
O3 Pb1 O8 158.9(2) 4 3 ?
O3 Pb1 O8 83.2(2) . 3 ?
O5 Pb1 O8 86.4(2) . 3 ?
O3 Pb1 O8 83.2(2) 4 2 ?
O3 Pb1 O8 158.9(2) . 2 ?
O5 Pb1 O8 86.4(2) . 2 ?
O8 Pb1 O8 88.9(3) 3 2 ?
O7 Pb2 O2 76.8(2) . 4_655 ?
O7 Pb2 O2 76.8(2) . . ?
O2 Pb2 O2 109.6(3) 4_655 . ?
O7 Pb2 O9 72.2(2) . 1_545 ?
O2 Pb2 O9 147.8(2) 4_655 1_545 ?
O2 Pb2 O9 71.8(2) . 1_545 ?
O7 Pb2 O9 72.2(2) . 4_645 ?
O2 Pb2 O9 71.8(2) 4_655 4_645 ?
O2 Pb2 O9 147.8(2) . 4_645 ?
O9 Pb2 O9 90.3(2) 1_545 4_645 ?
O1 Se1 O2 104.8(3) . . ?
O1 Se1 O3 103.6(3) . . ?
O2 Se1 O3 90.4(2) . . ?
O1 Se1 U1 111.3(2) . . ?
O2 Se1 U1 45.7(2) . . ?
O3 Se1 U1 44.8(2) . . ?
O5 Se2 O4 103.5(3) 2_554 . ?
O5 Se2 O4 103.5(3) 2_554 4 ?
O4 Se2 O4 99.8(4) . 4 ?
O7 Se3 O6 99.2(4) . 4_655 ?
O7 Se3 O6 99.2(4) . . ?
O6 Se3 O6 96.8(8) 4_655 . ?
Se1 O1 U1 147.4(3) . 3 ?
Se1 O2 Pb2 134.1(3) . . ?
Se1 O2 U1 104.7(2) . . ?
Pb2 O2 U1 118.9(2) . . ?
Se1 O3 Pb1 131.5(3) . . ?
Se1 O3 U1 105.3(2) . . ?
Pb1 O3 U1 119.4(2) . . ?
Se2 O4 U1 142.1(3) . . ?
Se2 O5 Pb1 133.4(4) 2 . ?
Se3 O6 U1 149.0(4) . 3_545 ?
Se3 O7 Pb2 123.3(4) . . ?
U1 O8 Pb1 131.4(3) . 2_554 ?
U1 O9 Pb2 135.8(3) . 1_565 ?
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
U1 O8 1.794(6) . ?
U1 O9 1.796(5) . ?
U1 O6 2.224(6) 3_544 ?
U1 O1 2.269(5) 3_554 ?
U1 O4 2.326(5) . ?
U1 O3 2.431(5) . ?
U1 O2 2.461(5) . ?
U1 Se1 3.3282(9) . ?
Pb1 O3 2.368(5) 4 ?
Pb1 O3 2.368(5) . ?
Pb1 O5 2.388(8) . ?
Pb1 O8 2.708(6) 3 ?
Pb1 O8 2.708(6) 2 ?
Pb2 O7 2.319(10) . ?
Pb2 O2 2.439(5) 4_655 ?
Pb2 O2 2.439(5) . ?
Pb2 O9 2.683(5) 1_545 ?
Pb2 O9 2.683(5) 4_645 ?
Se1 O1 1.689(5) . ?
Se1 O2 1.700(5) . ?
Se1 O3 1.721(5) . ?
Se2 O5 1.673(8) 2_554 ?
Se2 O4 1.704(5) . ?
Se2 O4 1.704(5) 4 ?
Se3 O7 1.671(8) . ?
Se3 O6 1.691(7) 4_655 ?
Se3 O6 1.691(7) . ?
O1 U1 2.269(5) 3 ?
O5 Se2 1.673(8) 2 ?
O6 U1 2.224(6) 3_545 ?
O8 Pb1 2.708(6) 2_554 ?
O9 Pb2 2.683(5) 1_565 ?
