#------------------------------------------------------------------------------
#$Date: 2016-03-24 03:05:36 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179612 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/76/4507692.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_4507692
loop_
_publ_author_name
'Villa, Eric M.'
'Alekseev, Evgeny V.'
'Depmeier, Wulf'
'Albrecht-Schmitt, Thomas E.'
_publ_section_title
;
 Syntheses, Structures, and Comparisons of Thallium Uranium Phosphites,
 Mixed Phosphate-Phosphites, and Phosphate
;
_journal_issue                   4
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              1721
_journal_paper_doi               10.1021/cg400046a
_journal_volume                  13
_journal_year                    2013
_chemical_formula_moiety         Tl2[(UO2)2(HPO3)3]*H2O
_chemical_formula_sum            'H3 O14 P3 Tl2 U2'
_chemical_formula_weight         1204.73
_chemical_melting_point          ?
_chemical_name_common            'Thallium Uranyl Phosphite'
_chemical_name_systematic
; 
 ? 
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.9070(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1774(2)
_cell_length_b                   11.4215(2)
_cell_length_c                   12.1390(2)
_cell_measurement_reflns_used    4475
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.65
_cell_measurement_theta_min      2.15
_cell_volume                     1466.08(4)
_computing_cell_refinement       'smart saint'
_computing_data_collection       smart
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 0
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'BRUKER apex II'
_diffrn_measurement_method       '0.5 wide w/ exposures'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_source         'Imus microfocused'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22369
_diffrn_reflns_theta_full        30.65
_diffrn_reflns_theta_max         30.65
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    44.332
_exptl_absorpt_correction_T_max  0.412
_exptl_absorpt_correction_T_min  0.306
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SHELTXPREP
_exptl_crystal_colour            Light-Yellow
_exptl_crystal_density_diffrn    5.458
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Column
_exptl_crystal_F_000             2024
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.020
_refine_diff_density_max         3.297
_refine_diff_density_min         -3.388
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0684
_refine_ls_R_factor_gt           0.0358
_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)+(0.0329P)²+5.9906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0883
_reflns_number_gt                2960
_reflns_number_total             4475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg400046a_si_002.cif
_cod_data_source_block           Tl_U(VI)_PO3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'N/A' was changed to '?' - the value
is undefined or not given.

'_symmetry_cell_setting' value
'Monoclinic' changed to 'monoclinic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'N/A' 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_original_sg_symbol_H-M      P21/n
_cod_database_code               4507692
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_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 0.24429(3) 0.37938(3) 0.23760(3) 0.02053(9) Uani 1 1 d .
U2 U 0.70305(3) 0.63032(3) 0.29194(3) 0.02538(10) Uani 1 1 d .
Tl1A Tl 0.1275(3) 0.6197(2) 0.4661(4) 0.0434(8) Uani 0.80 1 d P
Tl1B Tl 0.1328(9) 0.6159(8) 0.4498(13) 0.0247(10) Uani 0.20 1 d P
Tl2A Tl 0.3594(6) 0.6380(7) 0.0417(7) 0.0399(8) Uani 0.50 1 d P
Tl2B Tl 0.3624(5) 0.6230(7) 0.0423(7) 0.0472(12) Uani 0.50 1 d P
P1 P 0.07224(19) 0.12716(17) 0.1175(2) 0.0189(4) Uani 1 1 d .
H1 H -0.021(9) 0.116(7) 0.032(9) 0.023 Uiso 1 1 d .
P2 P 0.9245(2) 0.4327(2) 0.2278(3) 0.0389(8) Uani 1 1 d .
H2 H 0.877(10) 0.440(10) 0.102(10) 0.047 Uiso 1 1 d .
P3 P 0.5666(2) 0.3301(3) 0.2540(3) 0.0433(9) Uani 1 1 d .
H3 H 0.612(11) 0.326(10) 0.380(11) 0.052 Uiso 1 1 d .
O1 O 0.0111(5) 0.1342(5) 0.2112(6) 0.0232(13) Uani 1 1 d .
O2 O 0.1434(7) 0.2388(5) 0.1096(7) 0.0333(17) Uani 1 1 d .
O3 O 0.1602(7) 0.0236(6) 0.1316(7) 0.0357(18) Uani 1 1 d .
O4 O 0.8776(7) 0.5074(6) 0.3083(9) 0.051(3) Uani 1 1 d .
O5 O 0.6168(6) 0.2495(6) 0.1835(7) 0.038(2) Uani 1 1 d .
O6 O 0.2894(7) 0.2725(6) 0.3481(7) 0.0372(18) Uani 1 1 d .
O7 O 0.7551(7) 0.6204(7) 0.4462(7) 0.0434(19) Uani 1 1 d .
O8A O 0.653(2) 0.602(2) 0.141(2) 0.072(9) Uani 0.50 1 d P
O8B O 0.656(2) 0.6738(19) 0.1379(19) 0.043(5) Uani 0.50 1 d P
O9 O 0.4263(6) 0.3475(6) 0.1970(8) 0.041(2) Uani 1 1 d .
O10 O 1.0648(6) 0.4152(6) 0.2816(7) 0.041(2) Uani 1 1 d .
O11 O 0.2001(7) 0.4844(6) 0.1230(7) 0.041(2) Uani 1 1 d .
O12A O 0.8489(8) 0.3294(7) 0.1752(10) 0.037(2) Uani 0.80 1 d P
O12B O 0.881(3) 0.301(3) 0.287(3) 0.026(8) Uani 0.20 1 d P
O13A O 0.6438(11) 0.4290(9) 0.3150(13) 0.045(3) Uani 0.65 1 d P
O13B O 0.610(2) 0.4589(15) 0.204(3) 0.049(7) Uani 0.35 1 d P
O1W O 0.9782(7) 0.6290(6) 0.0856(6) 0.0372(18) Uani 1 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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Tl Tl -2.8358 9.6688 '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
O6 U1 O11 178.2(4) . .
O6 U1 O2 89.3(3) . .
O11 U1 O2 89.5(3) . .
O6 U1 O9 89.9(3) . .
O11 U1 O9 88.8(3) . .
O2 U1 O9 91.1(3) . .
O6 U1 O10 90.1(3) . 1_455
O11 U1 O10 91.1(3) . 1_455
O2 U1 O10 90.4(3) . 1_455
O9 U1 O10 178.5(2) . 1_455
O6 U1 O3 90.9(3) . 2
O11 U1 O3 90.4(3) . 2
O2 U1 O3 177.9(3) . 2
O9 U1 O3 91.0(3) . 2
O10 U1 O3 87.5(3) 1_455 2
O8A U2 O7 165.8(10) . .
O8A U2 O8B 26.3(9) . .
O7 U2 O8B 167.9(7) . .
O8A U2 O12B 76.4(14) . 2_655
O7 U2 O12B 117.2(10) . 2_655
O8B U2 O12B 52.2(12) . 2_655
O8A U2 O13B 54.5(12) . .
O7 U2 O13B 112.3(8) . .
O8B U2 O13B 79.6(10) . .
O12B U2 O13B 118.3(11) 2_655 .
O8A U2 O4 87.4(9) . .
O7 U2 O4 83.9(3) . .
O8B U2 O4 101.8(8) . .
O12B U2 O4 140.8(8) 2_655 .
O13B U2 O4 76.8(6) . .
O8A U2 O5 102.0(8) . 2_655
O7 U2 O5 85.9(3) . 2_655
O8B U2 O5 85.8(7) . 2_655
O12B U2 O5 77.1(8) 2_655 2_655
O13B U2 O5 141.5(6) . 2_655
O4 U2 O5 71.7(2) . 2_655
O8A U2 O1 90.4(9) . 2
O7 U2 O1 90.1(3) . 2
O8B U2 O1 91.2(7) . 2
O12B U2 O1 72.3(8) 2_655 2
O13B U2 O1 73.1(6) . 2
O4 U2 O1 144.3(2) . 2
O5 U2 O1 143.2(2) 2_655 2
O8A U2 O12A 109.4(10) . 2_655
O7 U2 O12A 84.3(4) . 2_655
O8B U2 O12A 84.7(7) . 2_655
O12B U2 O12A 32.9(10) 2_655 2_655
O13B U2 O12A 141.1(6) . 2_655
O4 U2 O12A 141.6(3) . 2_655
O5 U2 O12A 71.2(3) 2_655 2_655
O1 U2 O12A 72.0(2) 2 2_655
O8A U2 O13A 86.5(9) . .
O7 U2 O13A 80.0(4) . .
O8B U2 O13A 111.9(7) . .
O12B U2 O13A 141.1(9) 2_655 .
O13B U2 O13A 32.3(7) . .
O4 U2 O13A 71.1(3) . .
O5 U2 O13A 141.3(3) 2_655 .
O1 U2 O13A 73.1(3) 2 .
O12A U2 O13A 141.5(4) 2_655 .
O1 P1 O3 113.2(4) . .
O1 P1 O2 112.1(4) . .
O3 P1 O2 109.2(4) . .
O12A P2 O10 116.9(5) . .
O12A P2 O4 117.5(5) . .
O10 P2 O4 109.0(5) . .
O12A P2 O12B 46.5(11) . .
O10 P2 O12B 95.3(11) . .
O4 P2 O12B 91.1(11) . .
O13A P3 O5 119.8(6) . .
O13A P3 O9 119.0(6) . .
O5 P3 O9 110.3(4) . .
O13A P3 O13B 48.3(9) . .
O5 P3 O13B 97.1(9) . .
O9 P3 O13B 95.4(8) . .
P1 O1 U2 133.3(4) . 2_545
P1 O2 U1 134.8(5) . .
P1 O3 U1 141.1(5) . 2_545
P2 O4 U2 137.0(6) . .
P3 O5 U2 138.4(5) . 2_645
O8B O8A U2 82(3) . .
O8A O8B U2 72(3) . .
P3 O9 U1 142.4(5) . .
P2 O10 U1 142.8(5) . 1_655
O12B O12A P2 80.0(13) . .
O12B O12A U2 66.4(12) . 2_645
P2 O12A U2 145.1(7) . 2_645
O12A O12B P2 53.5(13) . .
O12A O12B U2 80.7(15) . 2_645
P2 O12B U2 133(2) . 2_645
O13B O13A P3 75.9(10) . .
O13B O13A U2 68.8(9) . .
P3 O13A U2 143.8(9) . .
O13A O13B P3 55.8(11) . .
O13A O13B U2 78.9(11) . .
P3 O13B U2 134.1(17) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 O6 1.762(8) .
U1 O11 1.782(7) .
U1 O2 2.265(7) .
U1 O9 2.273(7) .
U1 O10 2.274(7) 1_455
U1 O3 2.297(7) 2
U2 O8A 1.77(3) .
U2 O7 1.775(8) .
U2 O8B 1.84(2) .
U2 O12B 2.24(3) 2_655
U2 O13B 2.312(18) .
U2 O4 2.359(7) .
U2 O5 2.367(7) 2_655
U2 O1 2.382(6) 2
U2 O12A 2.411(8) 2_655
U2 O13A 2.434(11) .
P1 O1 1.507(7) .
P1 O3 1.512(6) .
P1 O2 1.522(6) .
P2 O12A 1.472(8) .
P2 O10 1.504(7) .
P2 O4 1.513(8) .
P2 O12B 1.80(3) .
P3 O13A 1.468(10) .
P3 O5 1.487(8) .
P3 O9 1.508(7) .
P3 O13B 1.72(2) .
O1 U2 2.382(6) 2_545
O3 U1 2.297(7) 2_545
O5 U2 2.367(7) 2_645
O8A O8B 0.82(3) .
O10 U1 2.274(7) 1_655
O12A O12B 1.33(4) .
O12A U2 2.411(8) 2_645
O12B U2 2.24(3) 2_645
O13A O13B 1.32(3) .
