#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324613.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_4324613
loop_
_publ_author_name
'Jessica M. Morrison'
'Laura J. Moore-Shay'
'Peter C. Burns'
_publ_section_title
;
 U(VI) Uranyl Cation-Cation Interactions in Framework Germanates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2272
_journal_page_last               2277
_journal_paper_doi               10.1021/ic1019444
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'Ba2+, (UO2)2+, (UO6)6-, (GeO4)4-'
_chemical_formula_sum            'Ba Ge2 O38 U11'
_chemical_formula_weight         3508.85
_chemical_name_systematic        'Barium uranyl germanate'
_space_group_IT_number           163
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2c'
_symmetry_space_group_name_H-M   'P -3 1 c'
_atom_sites_solution_hydrogens   notdet
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   10.2012(5)
_cell_length_b                   10.2012(5)
_cell_length_c                   17.1570(12)
_cell_measurement_reflns_used    4168
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.59
_cell_volume                     1546.23(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'CrystalMaker v.8.2.3'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω 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  0.0740
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17102
_diffrn_reflns_theta_full        27.58
_diffrn_reflns_theta_max         27.58
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    60.657
_exptl_absorpt_correction_T_max  0.7513
_exptl_absorpt_correction_T_min  0.1083
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    7.537
_exptl_crystal_description       platy
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.038
_exptl_crystal_size_min          0.005
_refine_diff_density_max         2.065
_refine_diff_density_min         -3.585
_refine_diff_density_rms         0.508
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1197
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0403P)²+11.7302P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0750
_refine_ls_wR_factor_ref         0.0772
_reflns_number_gt                1075
_reflns_number_total             1197
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1019444_si_002_2.cif
_cod_data_source_block           final_ba
_cod_database_code               4324613
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.6667 0.3333 0.39723(4) 0.00483(17) Uani 1 3 d S
U2 U 1.02001(4) 0.35908(4) 0.44017(2) 0.00736(14) Uani 1 1 d .
U3 U 0.86198(3) 0.13802(3) 0.2500 0.00771(16) Uani 1 2 d S
Ba1 Ba 1.3333 0.6667 0.2500 0.0226(4) Uani 1 6 d S
Ge1 Ge 1.0000 0.0000 0.39850(15) 0.0176(5) Uani 1 3 d S
O1 O 0.8442(8) -0.1743(8) 0.3720(4) 0.0108(15) Uani 1 1 d .
O2 O 1.1405(8) 0.4948(8) 0.3693(5) 0.0135(16) Uani 1 1 d .
O3 O 0.8165(8) 0.2877(8) 0.3419(4) 0.0110(15) Uani 1 1 d .
O4 O 0.5956(8) 0.1378(7) 0.4659(4) 0.0085(14) Uani 1 1 d .
O5 O 0.9023(8) 0.2254(8) 0.5169(4) 0.0091(15) Uiso 1 1 d .
O6 O 1.0000 0.0000 0.5000 0.016(4) Uani 1 6 d S
O7 O 0.6924(9) -0.0226(9) 0.2817(5) 0.0149(17) Uani 1 1 d .
O8 O 1.0000 0.0000 0.2500 0.020(5) Uani 1 6 d S
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'
Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
O3 U1 O3 100.1(3) 3_665 2_655
O3 U1 O3 100.1(3) 3_665 .
O3 U1 O3 100.1(3) 2_655 .
O3 U1 O4 78.8(3) 3_665 .
O3 U1 O4 170.6(3) 2_655 .
O3 U1 O4 89.2(3) . .
O3 U1 O4 170.6(3) 3_665 2_655
O3 U1 O4 89.2(3) 2_655 2_655
O3 U1 O4 78.8(3) . 2_655
O4 U1 O4 91.8(3) . 2_655
O3 U1 O4 89.2(3) 3_665 3_665
O3 U1 O4 78.8(3) 2_655 3_665
O3 U1 O4 170.6(3) . 3_665
O4 U1 O4 91.8(3) . 3_665
O4 U1 O4 91.8(3) 2_655 3_665
O3 U1 U2 42.8(2) 3_665 3_665
O3 U1 U2 136.6(2) 2_655 3_665
O3 U1 U2 107.2(2) . 3_665
O4 U1 U2 38.88(19) . 3_665
O4 U1 U2 128.36(19) 2_655 3_665
O4 U1 U2 79.08(19) 3_665 3_665
O3 U1 U2 107.2(2) 3_665 2_655
O3 U1 U2 42.8(2) 2_655 2_655
O3 U1 U2 136.6(2) . 2_655
O4 U1 U2 128.36(19) . 2_655
O4 U1 U2 79.08(19) 2_655 2_655
O4 U1 U2 38.88(19) 3_665 2_655
U2 U1 U2 115.829(8) 3_665 2_655
O3 U1 U2 136.6(2) 3_665 .
O3 U1 U2 107.2(2) 2_655 .
O3 U1 U2 42.8(2) . .
O4 U1 U2 79.08(19) . .
O4 U1 U2 38.88(19) 2_655 .
O4 U1 U2 128.36(19) 3_665 .
U2 U1 U2 115.829(8) 3_665 .
U2 U1 U2 115.830(8) 2_655 .
O2 U2 O5 177.2(3) . .
O2 U2 O1 95.5(3) . 3_765
O5 U2 O1 86.6(3) . 3_765
O2 U2 O4 88.2(3) . 8_666
O5 U2 O4 89.0(3) . 8_666
O1 U2 O4 153.8(3) 3_765 8_666
O2 U2 O4 98.6(3) . 2_655
O5 U2 O4 81.3(3) . 2_655
O1 U2 O4 131.4(3) 3_765 2_655
O4 U2 O4 73.1(3) 8_666 2_655
O2 U2 O5 90.7(3) . 8_666
O5 U2 O5 87.9(3) . 8_666
O1 U2 O5 77.4(3) 3_765 8_666
O4 U2 O5 76.6(2) 8_666 8_666
O4 U2 O5 147.9(2) 2_655 8_666
O2 U2 O3 85.2(3) . .
O5 U2 O3 97.3(3) . .
O1 U2 O3 68.9(2) 3_765 .
O4 U2 O3 137.3(2) 8_666 .
O4 U2 O3 66.3(2) 2_655 .
O5 U2 O3 145.5(2) 8_666 .
O2 U2 U1 101.2(2) . .
O5 U2 U1 80.3(2) . .
O1 U2 U1 96.97(19) 3_765 .
O4 U2 U1 107.69(17) 8_666 .
O4 U2 U1 34.63(17) 2_655 .
O5 U2 U1 167.32(16) 8_666 .
O3 U2 U1 33.95(16) . .
O2 U2 U2 94.3(2) . 7_766
O5 U2 U2 84.0(2) . 7_766
O1 U2 U2 165.68(19) 3_765 7_766
O4 U2 U2 36.82(17) 8_666 7_766
O4 U2 U2 36.27(17) 2_655 7_766
O5 U2 U2 112.82(17) 8_666 7_766
O3 U2 U2 101.69(16) . 7_766
U1 U2 U2 70.880(13) . 7_766
O2 U2 U3 78.5(2) . .
O5 U2 U3 104.2(2) . .
O1 U2 U3 35.18(19) 3_765 .
O4 U2 U3 165.86(18) 8_666 .
O4 U2 U3 103.75(17) 2_655 .
O5 U2 U3 108.17(17) 8_666 .
O3 U2 U3 37.43(16) . .
U1 U2 U3 70.596(13) . .
U2 U2 U3 138.456(17) 7_766 .
O7 U3 O7 174.9(6) 4_665 .
O7 U3 O1 91.5(3) 4_665 6_545
O7 U3 O1 90.4(3) . 6_545
O7 U3 O1 90.4(3) 4_665 3_765
O7 U3 O1 91.5(3) . 3_765
O1 U3 O1 135.7(3) 6_545 3_765
O7 U3 O3 87.6(3) 4_665 .
O7 U3 O3 88.7(3) . .
O1 U3 O3 156.2(2) 6_545 .
O1 U3 O3 68.2(2) 3_765 .
O7 U3 O3 88.7(3) 4_665 4_665
O7 U3 O3 87.6(3) . 4_665
O1 U3 O3 68.2(2) 6_545 4_665
O1 U3 O3 156.2(2) 3_765 4_665
O3 U3 O3 88.0(3) . 4_665
O7 U3 O8 92.6(3) 4_665 .
O7 U3 O8 92.6(3) . .
O1 U3 O8 67.84(17) 6_545 .
O1 U3 O8 67.84(17) 3_765 .
O3 U3 O8 136.00(17) . .
O3 U3 O8 136.00(17) 4_665 .
O7 U3 U2 102.2(3) 4_665 4_665
O7 U3 U2 77.0(3) . 4_665
O1 U3 U2 32.75(17) 6_545 4_665
O1 U3 U2 161.91(17) 3_765 4_665
O3 U3 U2 124.59(17) . 4_665
O3 U3 U2 39.05(17) 4_665 4_665
O8 U3 U2 98.352(9) . 4_665
O7 U3 U2 77.0(3) 4_665 .
O7 U3 U2 102.2(3) . .
O1 U3 U2 161.91(17) 6_545 .
O1 U3 U2 32.75(17) 3_765 .
O3 U3 U2 39.05(17) . .
O3 U3 U2 124.59(17) 4_665 .
O8 U3 U2 98.351(9) . .
U2 U3 U2 163.297(18) 4_665 .
O2 Ba1 O2 113.6(3) 6 3_775
O2 Ba1 O2 71.5(2) 6 4_775
O2 Ba1 O2 104.2(3) 3_775 4_775
O2 Ba1 O2 71.5(2) 6 5_755
O2 Ba1 O2 172.3(3) 3_775 5_755
O2 Ba1 O2 71.5(2) 4_775 5_755
O2 Ba1 O2 172.3(3) 6 2_755
O2 Ba1 O2 71.5(2) 3_775 2_755
O2 Ba1 O2 113.6(3) 4_775 2_755
O2 Ba1 O2 104.2(3) 5_755 2_755
O2 Ba1 O2 104.2(3) 6 .
O2 Ba1 O2 71.5(2) 3_775 .
O2 Ba1 O2 172.3(3) 4_775 .
O2 Ba1 O2 113.6(3) 5_755 .
O2 Ba1 O2 71.5(2) 2_755 .
O6 Ge1 O1 105.0(3) . 2_645
O6 Ge1 O1 105.0(3) . 3_765
O1 Ge1 O1 113.5(2) 2_645 3_765
O6 Ge1 O1 105.0(3) . .
O1 Ge1 O1 113.5(2) 2_645 .
O1 Ge1 O1 113.5(2) 3_765 .
Ge1 O1 U2 131.0(4) . 2_645
Ge1 O1 U3 116.2(4) . 2_645
U2 O1 U3 112.1(3) 2_645 2_645
U2 O2 Ba1 170.5(4) . .
U1 O3 U3 149.0(4) . .
U1 O3 U2 103.2(3) . .
U3 O3 U2 103.5(3) . .
U1 O4 U2 146.5(3) . 9_546
U1 O4 U2 106.5(3) . 3_665
U2 O4 U2 106.9(3) 9_546 3_665
U2 O5 U2 149.8(4) . 9_546
Ge1 O6 Ge1 180.0 7_756 .
U3 O8 U3 120.0 3_765 2_645
U3 O8 U3 120.0 3_765 .
U3 O8 U3 120.0 2_645 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O3 2.041(7) 3_665
U1 O3 2.041(7) 2_655
U1 O3 2.041(7) .
U1 O4 2.109(7) .
U1 O4 2.109(7) 2_655
U1 O4 2.109(7) 3_665
U2 O2 1.790(8) .
U2 O5 1.843(8) .
U2 O1 2.238(7) 3_765
U2 O4 2.299(7) 8_666
U2 O4 2.329(7) 2_655
U2 O5 2.416(7) 8_666
U2 O3 2.484(7) .
U3 O7 1.771(7) 4_665
U3 O7 1.771(7) .
U3 O1 2.383(8) 6_545
U3 O1 2.383(8) 3_765
U3 O3 2.396(7) .
U3 O3 2.396(7) 4_665
U3 O8 2.4387(5) .
Ba1 O2 2.773(8) 6
Ba1 O2 2.773(8) 3_775
Ba1 O2 2.773(8) 4_775
Ba1 O2 2.773(8) 5_755
Ba1 O2 2.773(8) 2_755
Ba1 O2 2.773(8) .
Ge1 O6 1.741(3) .
Ge1 O1 1.752(7) 2_645
Ge1 O1 1.752(7) 3_765
Ge1 O1 1.752(7) .
O1 U2 2.238(7) 2_645
O1 U3 2.383(8) 2_645
O4 U2 2.299(7) 9_546
O4 U2 2.329(7) 3_665
O5 U2 2.416(7) 9_546
O6 Ge1 1.741(3) 7_756
O8 U3 2.4387(5) 3_765
O8 U3 2.4387(5) 2_645
