#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:43:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179455 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/52/4335253.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_4335253
loop_
_publ_author_name
'Yu-Chih Chang'
'Wen-Jung Chang'
'Sophie Boudin'
'Kwang-Hwa Lii'
_publ_section_title
;
 High-Temperature, High-Pressure Hydrothermal Synthesis and
 Characterization of a Salt-Inclusion Mixed-Valence Uranium(V,VI)
 Silicate: [Na9F2][(UVO2)(UVIO2)2(Si2O7)2]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7230
_journal_page_last               7235
_journal_paper_doi               10.1021/ic400854j
_journal_volume                  52
_journal_year                    2013
_chemical_formula_structural     Na9F2(UO2)(UO2)2(Si2O7)2
_chemical_formula_sum            'F2 Na9 O20 Si4 U3'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                90.41(1)
_cell_angle_beta                 94.96(1)
_cell_angle_gamma                90.01(2)
_cell_formula_units_Z            1
_cell_length_a                   5.842(1)
_cell_length_b                   7.411(2)
_cell_length_c                   11.902(1)
_cell_volume                     513.35(17)
_computing_structure_refinement  'Fullprof Suite 1.00 (Feb 2007)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'X'Pert Pro Panalytical Philips'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_source_type              'x-ray tube'
_exptl_crystal_density_diffrn    4.50
_pd_calc_method                  'Rietveld refinement'
_pd_char_colour                  green
_pd_meas_2theta_range_inc        0.013132
_pd_meas_2theta_range_max        90.049461
_pd_meas_2theta_range_min        5.124620
_pd_meas_number_of_points        6464
_pd_meas_scan_method             step
_pd_proc_2theta_range_inc        0.013132
_pd_proc_2theta_range_max        90.04946
_pd_proc_2theta_range_min        5.124620
_pd_proc_ls_pref_orient_corr
;
Preferred orientation (March Model) defined as follows :
Ph = [(G1 cos (alpha,h))^2 +((sin (alpha,h))^2 /G1)]^1.5
Ph : preferred orientation correction for the h reflection
alpha,h : acute angle between the scattering vector and the normal to the
crystallites
G1 preferred orientation coefficient ; G1 = 0.4782(2)
h = 001
;
_pd_proc_ls_profile_function
;
Profile function : Pseudo-Voigt function, pV(x) defined as follows :
pV(x) = Eta L(x) + (1-Eta)G(x)
with 
x = 2thetai * 2thetah; thetai, thetah: theta angle of the ith measured
 step and of the h reflection.
L(x), G(x) : Lorentzian and gaussian function
Eta = Lorentzian ratio
and with
FWHM = U tan^2(theta) + V tan(theta) + W    for L(x) and G(x)
Eta = 0.914(3)
U = 2.23(1)
V = -1.016(5)
W = 0.1267(6)

Asymmetry correction applied up to 2theta=28\% as follows :
A(x)= 1 + ((P1.F1(x)+P2.F2(x))/tanh(thetah))
with
x = 2thetai *  2thetah; 
thetai,thetah: theta angle of the ith measured step and of the h reflection.
F1(x)=2x.exp(-x^2) and F2(x)=2(2x^2-3).F1(x)
P1 = 0.02380(4)
P2 = 0.01435(1)
;
_pd_proc_ls_prof_R_factor        0.1210
_pd_proc_ls_prof_wR_expected     0.0550
_pd_proc_ls_prof_wR_factor       0.1640
_pd_proc_number_of_points        6464
_pd_spec_mount_mode              reflection
_pd_spec_shape                   flat_sheet
_refine_diff_density_max         2.77
_refine_diff_density_min         -1.20
_refine_ls_goodness_of_fit_all   0.0871
_refine_ls_number_constraints    0
_refine_ls_number_parameters     86
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0322
_refine_ls_R_I_factor            0.0703
_refine_ls_shift/su_max          0.83
_refine_ls_weighting_scheme      sigma
_reflns_limit_h_max              5
_reflns_limit_h_min              -5
_reflns_limit_k_max              6
_reflns_limit_k_min              -6
_reflns_limit_l_max              10
_reflns_limit_l_min              0
_reflns_number_observed          886
_cod_data_source_file            ic400854j_si_003.cif
_cod_data_source_block           F2Na9O20Si4U3
_cod_original_cell_volume        513.4(2)
_cod_database_code               4335253
_cod_database_fobs_code          4335253
#BEGIN Tags that were not found in dictionaries:
_pd_calib_2theta_offset'         0.0004(37)
_reflns_d_spacing_max            11.856631
_reflns_d_spacing_min            1.089737
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Na1 NA 1 c 0. 0.5 0. 1. 1.
Na2 NA 2 i 0.28680 0.00010 -0.28190 1. 1.
Na3 NA 2 i 0.50010 0.25750 -0.00010 1. 1.
Na4 NA 2 i 0.99990 0.76920 0.50010 1. 1.
Na5 NA 2 i 0.50030 0.22690 0.50000 1. 1.
F F 2 i 0.25760 -0.00030 -0.46990 1. 1.
U1 U 1 a 0. 0. 0. 1. 1.
U2 U 2 i 0.71423 0.50006 0.28481 1. 1.
Si1 SI 2 i 0.20360 0.21460 0.23507 1. 1.
Si2 SI 2 i 0.20370 -0.21440 0.23504 1. 1.
O1 O 2 i 0.17320 0.23980 0.10050 1. 1.
O2 O 2 i 0.98910 0.29220 0.29750 1. 1.
O3 O 2 i 0.44940 0.28580 0.29090 1. 1.
O4 O 2 i 0.20230 0.00010 0.25960 1. 1.
O5 O 2 i 0.98900 0.70890 0.29740 1. 1.
O6 O 2 i 0.17290 -0.24060 0.10080 1. 1.
O7 O 2 i 0.44910 0.71510 0.29070 1. 1.
O8 O 2 i 0.25830 -0.00030 -0.08520 1. 1.
O9 O 2 i 0.73750 0.50010 0.44010 1. 1.
O10 O 2 i 0.68790 0.50010 0.12900 1. 1.
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
NA +1 9
U +5.66 3
Si +4 4
O -2 20
F -1 2
loop_
_pd_meas_point_id
_pd_meas_2theta_scan
_pd_proc_intensity_bkg_fix
1 6.2664 181(3)
2 8.0258 244(6)
3 9.2207 206(5)
4 11.0457 163(6)
5 11.6103 221(6)
6 13.2647 171(6)
7 13.7899 206(7)
8 15.7331 199(7)
9 16.6260 163(7)
10 17.2562 188(6)
11 20.0004 156(6)
12 20.8801 159(7)
13 21.6154 204(7)
14 23.4011 195(5)
15 25.8958 194(5)
16 27.0906 196(7)
17 27.7340 199(6)
18 29.5459 179(7)
19 29.5984 166(13)
20 31.4891 190(7)
21 32.2638 184(7)
22 33.6162 197(8)
23 34.0495 191(7)
24 35.4019 185(9)
25 36.2422 197(7)
26 37.5027 182(6)
27 39.2884 168(6)
28 41.1003 196(7)
29 41.5205 188(8)
30 42.7284 185(7)
31 44.1990 191(7)
32 44.8424 201(7)
33 45.8928 189(7)
34 46.6543 180(8)
35 48.0461 178(8)
36 48.7551 167(7)
37 50.5014 181(7)
38 50.9347 190(7)
39 52.8910 154(8)
40 52.9567 129(9)
41 55.0050 148(6)
42 56.9876 203(7)
43 57.3421 173(8)
44 58.3925 170(8)
45 59.3247 142(7)
46 61.3074 158(7)
47 61.4912 172(8)
48 63.3163 156(7)
49 63.7758 127(7)
50 66.2049 150(7)
51 67.0846 138(7)
52 68.3976 181(7)
53 69.2116 190(8)
54 70.0126 167(7)
55 71.2074 123(7)
56 72.8486 45(7)
57 73.6233 137(9)
58 74.3061 177(7)
59 75.7898 119(7)
60 77.2866 119(7)
61 78.3632 149(8)
62 78.9016 157(8)
63 79.7550 154(7)
64 80.7529 42(6)
65 83.6678 110(6)
66 84.0485 127(8)
67 85.4928 83(8)
68 85.9261 -369(8)
69 87.8956 32(8)
70 88.5127 79(8)
71 89.6157 140(8)
