#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324612.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_4324612
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         '(NH4)+, (UO2)2+, (UO6)6-, (GeO4)'
_chemical_formula_sum            'Ge2 H N O38 U11'
_chemical_formula_weight         3385.52
_chemical_name_systematic        'Ammonium uranyl germanate hydroxide'
_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                   10.2525(5)
_cell_length_b                   10.2525(5)
_cell_length_c                   17.3972(13)
_cell_measurement_reflns_used    4006
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      2.29
_cell_volume                     1583.69(16)
_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  0.0843
_diffrn_reflns_av_sigmaI/netI    0.0441
_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            17559
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.29
_exptl_absorpt_coefficient_mu    58.006
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.2980
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    7.100
_exptl_crystal_description       platy
_exptl_crystal_F_000             2774
_exptl_crystal_size_max          0.029
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.005
_refine_diff_density_max         3.207
_refine_diff_density_min         -2.570
_refine_diff_density_rms         0.624
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     83
_refine_ls_number_reflns         1237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.199
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0349
_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)+(0.0466P)²+31.2260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.0977
_reflns_number_gt                1137
_reflns_number_total             1237
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1019444_si_002_1.cif
_cod_data_source_block           final_amm
_cod_database_code               4324612
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 0.59956(5) 0.0050(2) Uani 1 3 d S
U2 U 0.01874(5) 0.35713(5) 0.55909(3) 0.00653(17) Uani 1 1 d .
U3 U 0.85534(3) 0.14466(3) 0.7500 0.0095(2) Uani 1 2 d S
Ge1 Ge 0.0000 0.0000 0.0997(3) 0.0093(8) Uani 0.558(6) 3 d SP
Ge2 Ge 0.0000 0.0000 0.1419(4) 0.0093(8) Uani 0.442(6) 3 d SP
N1 N 0.3333 0.6667 0.7500 0.039(10) Uani 1 6 d S
O1 O 0.8465(10) 0.8247(11) 0.6300(6) 0.016(2) Uani 1 1 d .
O2 O 0.1377(11) 0.4902(11) 0.6276(6) 0.016(2) Uani 1 1 d .
O3 O 0.8166(10) 0.2892(10) 0.6565(5) 0.0120(18) Uani 1 1 d .
O4 O 0.5951(9) 0.1377(9) 0.5339(5) 0.0096(17) Uani 1 1 d .
O5 O 0.9029(10) 0.2213(10) 0.4854(6) 0.0122(19) Uani 1 1 d .
O6 O 0.0000 0.0000 0.0000 0.042(8) Uani 1 6 d S
O7 O 0.6920(11) -0.0171(11) 0.7197(7) 0.020(2) Uani 1 1 d .
O8 O 0.0000 0.0000 0.7500 0.013(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'
N N 0.0061 0.0033 '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 98.8(3) . 3_665
O3 U1 O3 98.8(3) . 2_655
O3 U1 O3 98.8(3) 3_665 2_655
O3 U1 O4 89.7(4) . .
O3 U1 O4 78.6(4) 3_665 .
O3 U1 O4 171.4(3) 2_655 .
O3 U1 O4 78.6(4) . 2_655
O3 U1 O4 171.4(3) 3_665 2_655
O3 U1 O4 89.7(4) 2_655 2_655
O4 U1 O4 93.1(3) . 2_655
O3 U1 O4 171.4(4) . 3_665
O3 U1 O4 89.7(4) 3_665 3_665
O3 U1 O4 78.6(4) 2_655 3_665
O4 U1 O4 93.1(3) . 3_665
O4 U1 O4 93.1(3) 2_655 3_665
O3 U1 U2 43.0(3) . 1_655
O3 U1 U2 135.5(3) 3_665 1_655
O3 U1 U2 107.6(3) 2_655 1_655
O4 U1 U2 79.4(2) . 1_655
O4 U1 U2 38.9(2) 2_655 1_655
O4 U1 U2 129.7(2) 3_665 1_655
O3 U1 U2 107.6(3) . 3
O3 U1 U2 43.0(3) 3_665 3
O3 U1 U2 135.5(3) 2_655 3
O4 U1 U2 38.9(2) . 3
O4 U1 U2 129.7(2) 2_655 3
O4 U1 U2 79.4(2) 3_665 3
U2 U1 U2 116.197(9) 1_655 3
O3 U1 U2 135.5(3) . 2_665
O3 U1 U2 107.6(3) 3_665 2_665
O3 U1 U2 43.0(3) 2_655 2_665
O4 U1 U2 129.7(2) . 2_665
O4 U1 U2 79.4(2) 2_655 2_665
O4 U1 U2 38.9(2) 3_665 2_665
U2 U1 U2 116.197(9) 1_655 2_665
U2 U1 U2 116.197(9) 3 2_665
O2 U2 O5 177.4(4) . 1_455
O2 U2 O1 94.7(4) . 3_565
O5 U2 O1 86.0(4) 1_455 3_565
O2 U2 O4 87.7(4) . 8_566
O5 U2 O4 90.6(4) 1_455 8_566
O1 U2 O4 155.2(3) 3_565 8_566
O2 U2 O4 98.5(4) . 2
O5 U2 O4 82.9(3) 1_455 2
O1 U2 O4 130.8(3) 3_565 2
O4 U2 O4 72.8(3) 8_566 2
O2 U2 O5 91.4(4) . 8_566
O5 U2 O5 86.3(4) 1_455 8_566
O1 U2 O5 78.6(3) 3_565 8_566
O4 U2 O5 76.7(3) 8_566 8_566
O4 U2 O5 147.4(3) 2 8_566
O2 U2 O3 85.0(4) . 1_455
O5 U2 O3 97.6(4) 1_455 1_455
O1 U2 O3 68.3(3) 3_565 1_455
O4 U2 O3 136.5(3) 8_566 1_455
O4 U2 O3 66.0(3) 2 1_455
O5 U2 O3 146.2(3) 8_566 1_455
O2 U2 U1 101.8(3) . 1_455
O5 U2 U1 80.6(3) 1_455 1_455
O1 U2 U1 96.7(2) 3_565 1_455
O4 U2 U1 107.0(2) 8_566 1_455
O4 U2 U1 34.3(2) 2 1_455
O5 U2 U1 166.3(2) 8_566 1_455
O3 U2 U1 34.3(2) 1_455 1_455
O2 U2 U2 93.9(3) . 7_566
O5 U2 U2 85.9(3) 1_455 7_566
O1 U2 U2 165.8(2) 3_565 7_566
O4 U2 U2 36.6(2) 8_566 7_566
O4 U2 U2 36.3(2) 2 7_566
O5 U2 U2 112.5(2) 8_566 7_566
O3 U2 U2 101.2(2) 1_455 7_566
U1 U2 U2 70.497(15) 1_455 7_566
O2 U2 U3 78.0(3) . 1_455
O5 U2 U3 103.9(3) 1_455 1_455
O1 U2 U3 35.8(2) 3_565 1_455
O4 U2 U3 164.1(2) 8_566 1_455
O4 U2 U3 102.1(2) 2 1_455
O5 U2 U3 110.3(2) 8_566 1_455
O3 U2 U3 36.1(2) 1_455 1_455
U1 U2 U3 69.690(16) 1_455 1_455
U2 U2 U3 136.57(2) 7_566 1_455
O7 U3 O7 179.1(7) . 4_666
O7 U3 O3 89.1(4) . 4_666
O7 U3 O3 90.3(5) 4_666 4_666
O7 U3 O3 90.3(5) . .
O7 U3 O3 89.1(4) 4_666 .
O3 U3 O3 93.0(4) 4_666 .
O7 U3 O1 89.9(5) . 6_556
O7 U3 O1 90.5(4) 4_666 6_556
O3 U3 O1 68.3(3) 4_666 6_556
O3 U3 O1 161.2(3) . 6_556
O7 U3 O1 90.5(4) . 3_665
O7 U3 O1 89.9(5) 4_666 3_665
O3 U3 O1 161.2(3) 4_666 3_665
O3 U3 O1 68.3(3) . 3_665
O1 U3 O1 130.5(5) 6_556 3_665
O7 U3 O8 90.5(4) . 1_655
O7 U3 O8 90.5(4) 4_666 1_655
O3 U3 O8 133.5(2) 4_666 1_655
O3 U3 O8 133.5(2) . 1_655
O1 U3 O8 65.2(2) 6_556 1_655
O1 U3 O8 65.2(2) 3_665 1_655
O7 U3 Ge2 80.1(4) . 10_656
O7 U3 Ge2 100.7(4) 4_666 10_656
O3 U3 Ge2 164.1(2) 4_666 10_656
O3 U3 Ge2 98.6(2) . 10_656
O1 U3 Ge2 99.9(3) 6_556 10_656
O1 U3 Ge2 32.0(2) 3_665 10_656
O8 U3 Ge2 36.21(10) 1_655 10_656
O7 U3 Ge2 100.7(4) . 7_656
O7 U3 Ge2 80.1(4) 4_666 7_656
O3 U3 Ge2 98.6(2) 4_666 7_656
O3 U3 Ge2 164.1(2) . 7_656
O1 U3 Ge2 32.0(2) 6_556 7_656
O1 U3 Ge2 99.9(3) 3_665 7_656
O8 U3 Ge2 36.21(10) 1_655 7_656
Ge2 U3 Ge2 72.4(2) 10_656 7_656
O7 U3 U2 102.4(4) . 1_655
O7 U3 U2 77.5(4) 4_666 1_655
O3 U3 U2 128.9(2) 4_666 1_655
O3 U3 U2 38.4(2) . 1_655
O1 U3 U2 158.3(2) 6_556 1_655
O1 U3 U2 33.4(2) 3_665 1_655
O8 U3 U2 96.472(11) 1_655 1_655
Ge2 U3 U2 65.37(9) 10_656 1_655
Ge2 U3 U2 126.77(8) 7_656 1_655
O7 U3 U2 77.5(4) . 4_656
O7 U3 U2 102.4(4) 4_666 4_656
O3 U3 U2 38.4(2) 4_666 4_656
O3 U3 U2 128.9(2) . 4_656
O1 U3 U2 33.4(2) 6_556 4_656
O1 U3 U2 158.3(2) 3_665 4_656
O8 U3 U2 96.472(11) 1_655 4_656
Ge2 U3 U2 126.77(8) 10_656 4_656
Ge2 U3 U2 65.37(9) 7_656 4_656
U2 U3 U2 167.06(2) 1_655 4_656
Ge2 Ge1 O6 180.000(1) . .
Ge2 Ge1 O1 72.8(4) . 12_655
O6 Ge1 O1 107.2(4) . 12_655
Ge2 Ge1 O1 72.8(4) . 10_445
O6 Ge1 O1 107.2(4) . 10_445
O1 Ge1 O1 111.6(3) 12_655 10_445
Ge2 Ge1 O1 72.8(4) . 11_565
O6 Ge1 O1 107.2(4) . 11_565
O1 Ge1 O1 111.6(3) 12_655 11_565
O1 Ge1 O1 111.6(3) 10_445 11_565
Ge1 Ge2 O1 83.0(4) . 12_655
Ge1 Ge2 O1 83.0(4) . 10_445
O1 Ge2 O1 118.55(17) 12_655 10_445
Ge1 Ge2 O1 83.0(4) . 11_565
O1 Ge2 O1 118.55(17) 12_655 11_565
O1 Ge2 O1 118.55(17) 10_445 11_565
Ge1 Ge2 O8 180.0 . 7_556
O1 Ge2 O8 97.0(4) 12_655 7_556
O1 Ge2 O8 97.0(4) 10_445 7_556
O1 Ge2 O8 97.0(4) 11_565 7_556
Ge1 Ge2 U3 126.21(10) . 7_656
O1 Ge2 U3 48.5(3) 12_655 7_656
O1 Ge2 U3 99.4(4) 10_445 7_656
O1 Ge2 U3 135.6(4) 11_565 7_656
O8 Ge2 U3 53.79(10) 7_556 7_656
Ge1 Ge2 U3 126.21(10) . 8_566
O1 Ge2 U3 99.4(4) 12_655 8_566
O1 Ge2 U3 135.6(4) 10_445 8_566
O1 Ge2 U3 48.5(3) 11_565 8_566
O8 Ge2 U3 53.79(10) 7_556 8_566
U3 Ge2 U3 88.66(15) 7_656 8_566
Ge1 Ge2 U3 126.21(10) . 9_446
O1 Ge2 U3 135.6(4) 12_655 9_446
O1 Ge2 U3 48.5(3) 10_445 9_446
O1 Ge2 U3 99.4(4) 11_565 9_446
O8 Ge2 U3 53.79(10) 7_556 9_446
U3 Ge2 U3 88.66(15) 7_656 9_446
U3 Ge2 U3 88.66(15) 8_566 9_446
Ge2 O1 U2 149.5(6) 10_666 2_665
Ge1 O1 U2 127.3(5) 10_666 2_665
Ge2 O1 U3 99.6(5) 10_666 2_655
Ge1 O1 U3 121.1(5) 10_666 2_655
U2 O1 U3 110.8(4) 2_665 2_655
U1 O3 U3 147.8(5) . .
U1 O3 U2 102.7(4) . 1_655
U3 O3 U2 105.4(3) . 1_655
U1 O4 U2 145.8(4) . 9_656
U1 O4 U2 106.8(3) . 3
U2 O4 U2 107.2(3) 9_656 3
U2 O5 U2 150.6(5) 1_655 9_656
Ge1 O6 Ge1 180.0 . 7
Ge2 O8 Ge2 180.000(3) 10_556 7_556
Ge2 O8 U3 90.0 10_556 1_455
Ge2 O8 U3 90.0 7_556 1_455
Ge2 O8 U3 90.000(1) 10_556 3_665
Ge2 O8 U3 90.000(1) 7_556 3_665
U3 O8 U3 120.001(1) 1_455 3_665
Ge2 O8 U3 90.000(1) 10_556 2_545
Ge2 O8 U3 90.000(1) 7_556 2_545
U3 O8 U3 120.0 1_455 2_545
U3 O8 U3 120.0 3_665 2_545
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O3 2.060(9) .
U1 O3 2.060(9) 3_665
U1 O3 2.060(9) 2_655
U1 O4 2.096(8) .
U1 O4 2.096(8) 2_655
U1 O4 2.096(8) 3_665
U2 O2 1.763(10) .
U2 O5 1.828(10) 1_455
U2 O1 2.277(9) 3_565
U2 O4 2.324(8) 8_566
U2 O4 2.339(8) 2
U2 O5 2.428(9) 8_566
U2 O3 2.492(9) 1_455
U3 O7 1.748(10) .
U3 O7 1.748(10) 4_666
U3 O3 2.364(9) 4_666
U3 O3 2.364(9) .
U3 O1 2.417(10) 6_556
U3 O1 2.417(10) 3_665
U3 O8 2.5689(6) 1_655
U3 Ge2 3.184(4) 10_656
U3 Ge2 3.184(4) 7_656
Ge1 Ge2 0.734(6) .
Ge1 O6 1.735(5) .
Ge1 O1 1.777(9) 12_655
Ge1 O1 1.777(9) 10_445
Ge1 O1 1.777(9) 11_565
Ge2 O1 1.709(9) 12_655
Ge2 O1 1.710(9) 10_445
Ge2 O1 1.710(9) 11_565
Ge2 O8 1.881(7) 7_556
Ge2 U3 3.184(4) 7_656
Ge2 U3 3.184(4) 8_566
Ge2 U3 3.184(4) 9_446
O1 Ge2 1.710(9) 10_666
O1 Ge1 1.777(9) 10_666
O1 U2 2.277(9) 2_665
O1 U3 2.417(10) 2_655
O3 U2 2.492(9) 1_655
O4 U2 2.324(8) 9_656
O4 U2 2.339(8) 3
O5 U2 1.828(9) 1_655
O5 U2 2.428(9) 9_656
O6 Ge1 1.735(5) 7
O8 Ge2 1.881(7) 10_556
O8 Ge2 1.881(7) 7_556
O8 U3 2.5689(6) 1_455
O8 U3 2.5689(6) 3_665
O8 U3 2.5689(6) 2_545
