#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:54:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179459 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/56/4335679.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_4335679
loop_
_publ_author_name
'Jeongho Yeon'
'Mark D. Smith'
'Athena S. Sefat'
'T. Thao Tran'
'P. Shiv Halasyamani'
'Hans-Conrad zur Loye'
_publ_contact_author_name
;
;
_publ_section_title
;
 U3F12(H2O), a Noncentrosymmetric Uranium(IV) Fluoride Prepared via a
 Convenient In Situ Route That Creates U4+ under Mild Hydrothermal
 Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8303
_journal_page_last               8305
_journal_paper_doi               10.1021/ic401412t
_journal_volume                  52
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_formula_moiety         'F12 H2 O U3'
_chemical_formula_sum            'F12 H2 O U3'
_chemical_formula_weight         960.11
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_symmetry_space_group_name_Hall  'C -2y'
_symmetry_space_group_name_H-M   'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-09
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 128.787(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1594(11)
_cell_length_b                   11.8457(11)
_cell_length_c                   8.5409(8)
_cell_measurement_reflns_used    5774
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.59
_cell_measurement_theta_min      2.75
_cell_volume                     958.92(16)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            17471
_diffrn_reflns_theta_full        38.59
_diffrn_reflns_theta_max         38.59
_diffrn_reflns_theta_min         2.75
_diffrn_source                   'sealed tube'
_diffrn_source_current           39.0
_diffrn_source_power             1.833
_diffrn_source_target            Mo
_diffrn_source_voltage           47.0
_exptl_absorpt_coefficient_mu    50.704
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.281997
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1452 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.2820.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    6.650
_exptl_crystal_description       needle
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         4.361
_refine_diff_density_min         -3.155
_refine_diff_density_rms         0.542
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(4)
_refine_ls_extinction_coef       0.00016(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         4686
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0308
_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)+(0.0325P)²+2.1921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0675
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                4563
_reflns_number_total             4686
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401412t_si_001.cif
_cod_data_source_block           jy1156ds
_cod_original_cell_volume        958.92(15)
_cod_database_code               4335679
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 'x, -y, z'
3 'x+1/2, y+1/2, z'
4 'x+1/2, -y+1/2, 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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
U1 U 0.51816(3) 0.31196(2) 0.07317(4) 0.00579(6) Uani 1 1 d .
U2 U 0.65045(2) 0.32832(2) 0.67996(3) 0.00559(6) Uani 1 1 d .
U3 U 0.91301(4) 0.5000 0.55887(6) 0.00630(7) Uani 1 2 d S
U4 U 0.28322(4) 0.5000 0.23328(6) 0.00572(7) Uani 1 2 d S
F1 F 0.5397(6) 0.1538(5) 0.6065(9) 0.0121(10) Uani 1 1 d .
F2 F 0.5894(7) 0.3043(4) 0.8845(10) 0.0107(9) Uani 1 1 d .
F3 F 0.5900(7) 0.2676(4) 0.3851(9) 0.0095(8) Uani 1 1 d .
F4 F 0.6354(6) 0.1439(4) 0.1560(9) 0.0099(9) Uani 1 1 d .
F5 F 0.7365(5) 0.3840(5) 0.3034(8) 0.0104(9) Uani 1 1 d .
F6 F 0.8080(6) 0.1777(5) 0.7586(9) 0.0083(10) Uani 1 1 d .
F7 F 0.8356(6) 0.3882(5) 0.6868(9) 0.0114(10) Uani 1 1 d .
F8 F 0.8618(6) 0.3282(5) 1.0118(9) 0.0096(10) Uani 1 1 d .
F9 F 0.3618(6) 0.3859(5) 0.1133(8) 0.0118(10) Uani 1 1 d .
F10 F 0.4188(5) 0.3675(5) 0.4831(8) 0.0098(9) Uani 1 1 d .
F11 F 0.5000(8) 0.5000 0.0000(11) 0.0119(13) Uani 1 2 d S
F12 F 0.5780(9) 0.5000 0.4659(12) 0.0117(13) Uani 1 2 d S
F13 F 0.6777(8) 0.5000 0.8238(11) 0.0117(14) Uani 1 2 d S
F14 F 0.1047(9) 0.5000 -0.1101(15) 0.0115(14) Uani 1 2 d S
O1 O 0.9297(11) 0.5000 0.2877(16) 0.0116(17) Uani 1 2 d SD
H1 H 0.903(15) 0.4452(9) 0.208(15) 0.03(3) Uiso 1 1 d D
O2 O 0.2375(12) 0.5000 0.4813(16) 0.0107(17) Uani 1 2 d SD
H2 H 0.214(15) 0.4450(9) 0.52(2) 0.03(3) Uiso 1 1 d D
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
H H 0.0000 0.0000 '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
F2 U1 U2 96.53(17) 1_554 4_454
F2 U1 F3 141.7(2) 1_554 .
F2 U1 F4 75.1(2) 1_554 .
F2 U1 F5 82.5(2) 1_554 .
F2 U1 F6 78.9(2) 1_554 4_454
F2 U1 F8 115.8(2) 1_554 4_454
F2 U1 F9 147.3(2) 1_554 .
F2 U1 F11 81.9(2) 1_554 .
F3 U1 U2 107.49(15) . 4_454
F3 U1 F4 74.4(2) . .
F3 U1 F8 76.1(2) . 4_454
F3 U1 F9 70.3(2) . .
F3 U1 F11 116.3(2) . .
F4 U1 U2 92.96(14) . 4_454
F4 U1 F8 73.2(2) . 4_454
F4 U1 F9 134.2(2) . .
F5 U1 U2 176.89(14) . 4_454
F5 U1 F3 71.91(19) . .
F5 U1 F4 83.9(2) . .
F5 U1 F6 147.9(2) . 4_454
F5 U1 F8 144.6(2) . 4_454
F5 U1 F9 110.86(19) . .
F5 U1 F11 74.3(2) . .
F6 U1 U2 34.04(14) 4_454 4_454
F6 U1 F3 135.8(2) 4_454 .
F6 U1 F4 115.7(2) 4_454 .
F6 U1 F8 67.45(19) 4_454 4_454
F6 U1 F9 74.6(2) 4_454 .
F6 U1 F11 77.3(2) 4_454 .
F8 U1 U2 33.57(15) 4_454 4_454
F9 U1 U2 71.50(14) . 4_454
F9 U1 F8 70.8(2) . 4_454
F11 U1 U2 108.50(19) . 4_454
F11 U1 F4 150.1(2) . .
F11 U1 F8 135.2(2) . 4_454
F11 U1 F9 73.9(2) . .
U1 U2 U2 115.213(6) 4_556 2_565
F1 U2 U1 90.63(15) . 4_556
F1 U2 U2 152.61(15) . 2_565
F1 U2 F6 68.8(2) . .
F1 U2 F8 109.6(2) . .
F1 U2 F12 130.3(2) . .
F2 U2 U1 91.99(16) . 4_556
F2 U2 U2 97.08(12) . 2_565
F2 U2 F1 71.8(2) . .
F2 U2 F6 106.1(2) . .
F2 U2 F7 141.7(2) . .
F2 U2 F8 73.3(2) . .
F2 U2 F12 121.5(2) . .
F3 U2 U1 102.81(15) . 4_556
F3 U2 U2 108.61(13) . 2_565
F3 U2 F1 71.7(2) . .
F3 U2 F2 140.6(2) . .
F3 U2 F6 73.6(2) . .
F3 U2 F7 76.0(2) . .
F3 U2 F8 133.9(2) . .
F3 U2 F12 73.92(19) . .
F3 U2 F13 136.0(2) . .
F6 U2 U1 32.21(15) . 4_556
F6 U2 U2 138.38(15) . 2_565
F6 U2 F12 131.9(2) . .
F7 U2 U1 62.55(14) . 4_556
F7 U2 U2 72.24(14) . 2_565
F7 U2 F1 131.7(2) . .
F7 U2 F6 68.1(2) . .
F7 U2 F8 70.1(2) . .
F7 U2 F12 70.2(2) . .
F8 U2 U1 33.19(14) . 4_556
F8 U2 U2 90.02(14) . 2_565
F8 U2 F6 65.2(2) . .
F8 U2 F12 120.1(2) . .
F10 U2 U1 162.99(13) . 4_556
F10 U2 U2 78.06(14) . 2_565
F10 U2 F1 74.9(2) . .
F10 U2 F2 75.2(2) . .
F10 U2 F3 81.4(2) . .
F10 U2 F6 140.8(2) . .
F10 U2 F7 134.11(19) . .
F10 U2 F8 144.6(2) . .
F10 U2 F12 65.3(2) . .
F10 U2 F13 84.9(2) . .
F12 U2 U1 131.72(19) . 4_556
F12 U2 U2 35.49(14) . 2_565
F13 U2 U1 102.34(18) . 4_556
F13 U2 U2 27.38(17) . 2_565
F13 U2 F1 142.9(3) . .
F13 U2 F2 73.1(2) . .
F13 U2 F6 133.8(2) . .
F13 U2 F7 84.4(2) . .
F13 U2 F8 70.8(2) . .
F13 U2 F12 62.4(2) . .
F1 U3 F1 108.0(3) 3 4
F1 U3 F5 140.7(2) 4 2_565
F1 U3 F5 79.4(2) 3 2_565
F1 U3 F5 79.4(2) 4 .
F1 U3 F5 140.7(2) 3 .
F1 U3 F7 146.1(2) 3 .
F1 U3 F7 83.3(2) 4 .
F1 U3 F7 83.3(2) 3 2_565
F1 U3 F7 146.1(2) 4 2_565
F1 U3 F14 73.9(2) 3 1_656
F1 U3 F14 73.9(2) 4 1_656
F1 U3 O1 73.6(2) 4 .
F1 U3 O1 73.6(2) 3 .
F5 U3 F5 72.6(3) . 2_565
F5 U3 O1 71.7(2) . .
F5 U3 O1 71.7(2) 2_565 .
F7 U3 F5 71.82(19) 2_565 2_565
F7 U3 F5 71.8(2) . .
F7 U3 F5 112.39(19) . 2_565
F7 U3 F5 112.39(19) 2_565 .
F7 U3 F7 71.6(3) . 2_565
F7 U3 F14 79.2(2) 2_565 1_656
F7 U3 F14 79.2(2) . 1_656
F7 U3 O1 139.70(19) 2_565 .
F7 U3 O1 139.70(19) . .
F14 U3 F5 142.43(15) 1_656 .
F14 U3 F5 142.43(15) 1_656 2_565
F14 U3 O1 123.3(3) 1_656 .
F4 U4 F4 98.2(3) 3_455 4_455
F4 U4 F10 74.54(19) 3_455 2_565
F4 U4 F10 139.6(2) 4_455 2_565
F4 U4 F10 139.6(2) 3_455 .
F4 U4 F10 74.54(19) 4_455 .
F4 U4 F12 129.62(15) 4_455 .
F4 U4 F12 129.62(15) 3_455 .
F4 U4 F14 71.7(2) 3_455 .
F4 U4 F14 71.7(2) 4_455 .
F4 U4 O2 71.9(2) 3_455 .
F4 U4 O2 71.9(2) 4_455 .
F9 U4 F4 84.3(2) . 4_455
F9 U4 F4 144.3(2) . 3_455
F9 U4 F4 144.3(2) 2_565 4_455
F9 U4 F4 84.3(2) 2_565 3_455
F9 U4 F9 74.2(3) 2_565 .
F9 U4 F10 124.81(19) . 2_565
F9 U4 F10 75.55(19) 2_565 2_565
F9 U4 F10 75.55(19) . .
F9 U4 F10 124.81(19) 2_565 .
F9 U4 F12 66.54(18) 2_565 .
F9 U4 F12 66.54(18) . .
F9 U4 F14 75.5(2) . .
F9 U4 F14 75.5(2) 2_565 .
F9 U4 O2 140.49(17) . .
F9 U4 O2 140.49(17) 2_565 .
F10 U4 F10 85.7(3) 2_565 .
F10 U4 F12 59.31(16) . .
F10 U4 F12 59.31(16) 2_565 .
F10 U4 F14 137.11(14) . .
F10 U4 F14 137.11(14) 2_565 .
F10 U4 O2 68.1(2) 2_565 .
F10 U4 O2 68.1(2) . .
F14 U4 F12 131.8(3) . .
F14 U4 O2 122.9(3) . .
O2 U4 F12 105.3(3) . .
U3 F1 U2 168.9(3) 3_445 .
U1 F2 U2 170.2(3) 1_556 .
U2 F3 U1 148.0(2) . .
U4 F4 U1 167.5(3) 3_545 .
U1 F5 U3 158.8(3) . .
U1 F6 U2 113.7(2) 4_556 .
U3 F7 U2 148.8(3) . .
U1 F8 U2 113.2(2) 4_556 .
U4 F9 U1 157.7(3) . .
U2 F10 U4 131.9(2) . .
U1 F11 U1 153.9(4) . 2_565
U2 F12 U2 109.0(3) 2_565 .
U2 F12 U4 103.1(2) . .
U2 F12 U4 103.1(2) 2_565 .
U2 F13 U2 125.2(3) 2_565 .
U3 F14 U4 174.1(4) 1_454 .
U3 O1 H1 123(7) . .
U4 O2 H2 128(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 F2 2.259(7) 1_554
U1 F3 2.285(6) .
U1 F4 2.287(5) .
U1 F5 2.259(5) .
U1 F6 2.272(6) 4_454
U1 F8 2.324(6) 4_454
U1 F9 2.306(5) .
U1 F11 2.2864(18) .
U2 F1 2.329(6) .
U2 F2 2.304(7) .
U2 F3 2.254(6) .
U2 F6 2.386(6) .
U2 F7 2.326(5) .
U2 F8 2.348(6) .
U2 F10 2.246(5) .
U2 F12 2.498(4) .
U2 F13 2.290(4) .
U3 F1 2.252(6) 4
U3 F1 2.252(6) 3
U3 F5 2.321(5) .
U3 F5 2.321(5) 2_565
U3 F7 2.264(5) .
U3 F7 2.264(5) 2_565
U3 F14 2.273(10) 1_656
U3 O1 2.448(11) .
U4 F4 2.255(5) 4_455
U4 F4 2.255(5) 3_455
U4 F9 2.239(5) 2_565
U4 F9 2.239(5) .
U4 F10 2.308(5) .
U4 F10 2.308(5) 2_565
U4 F12 2.806(9) .
U4 F14 2.311(10) .
U4 O2 2.504(9) .
F1 U3 2.252(6) 3_445
F2 U1 2.259(7) 1_556
F4 U4 2.255(5) 3_545
F6 U1 2.272(6) 4_556
F8 U1 2.324(6) 4_556
F11 U1 2.2865(18) 2_565
F12 U2 2.498(4) 2_565
F13 U2 2.290(4) 2_565
F14 U3 2.273(10) 1_454
O1 H1 0.84(6) .
O2 H2 0.84(6) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 F8 0.84(6) 1.98(7) 2.817(9) 170(12) 1_554
O2 H2 F6 0.84(6) 2.17(10) 2.869(8) 140(13) 4_455
