#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:10:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179526 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/23/4342341.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_4342341
loop_
_publ_author_name
'Yeon, Jeongho'
'Smith, Mark D.'
'Morrison, Gregory'
'Zur Loye, Hans-Conrad'
_publ_section_title
;
 Trivalent Cation-Controlled Phase Space of New U(IV) Fluorides, Na3MU6F30
 (M = Al(3+), Ga(3+), Ti(3+), V(3+), Cr(3+), Fe(3+)): Mild Hydrothermal
 Synthesis Including an in Situ Reduction Step, Structures, Optical, and
 Magnetic Properties.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2058
_journal_page_last               2066
_journal_paper_doi               10.1021/ic503034t
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'F30 Na3 Ti U6'
_chemical_formula_sum            'F30 Na3 Ti U6'
_chemical_formula_weight         2115.05
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           165
_space_group_name_Hall           '-P 3 2"c'
_space_group_name_H-M_alt        'P -3 c 1'
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.8556(3)
_cell_length_b                   9.8556(3)
_cell_length_c                   12.9667(8)
_cell_measurement_reflns_used    7993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.058
_cell_measurement_theta_min      2.386
_cell_volume                     1090.75(8)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.631 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0530
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            24356
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.057
_diffrn_reflns_theta_min         2.386
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    45.025
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.2075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    6.440
_exptl_crystal_description       'round plate'
_exptl_crystal_F_000             1754
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.040
_refine_diff_density_max         3.060
_refine_diff_density_min         -2.377
_refine_diff_density_rms         0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         1616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0302
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0299P)²+12.9070P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0703
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                1519
_reflns_number_total             1616
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic503034t_si_002.cif
_cod_data_source_block           Na3TiU6F30
_cod_depositor_comments
'Adding full bibliography for 4342339--4342344.cif.'
_cod_original_cell_volume        1090.75(9)
_cod_database_code               4342341
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.052
_shelx_estimated_absorpt_t_max   0.266
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
U1 U 0.39988(2) 0.32422(2) 0.39808(2) 0.00777(7) Uani 1 1 d . . .
Ti1 Ti 0.0000 0.0000 0.2500 0.0222(6) Uani 1 6 d S T P
Na1 Na 0.3333 0.6667 0.3381(3) 0.0103(7) Uani 1 3 d S T P
Na2 Na 0.0000 0.0000 0.5000 0.038(2) Uani 1 6 d S T P
F1 F 0.3047(4) 0.4360(4) 0.2835(3) 0.0120(6) Uani 1 1 d . . .
F2 F 0.1904(4) 0.3081(4) 0.4818(3) 0.0117(6) Uani 1 1 d . . .
F3 F 0.5333(4) 0.4138(4) 0.5518(3) 0.0119(6) Uani 1 1 d . . .
F4 F 0.1814(5) 0.1007(5) 0.3364(3) 0.0181(8) Uani 1 1 d . . .
F5 F 0.5115(4) 0.1706(4) 0.3630(3) 0.0118(6) 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
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 '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
F2 U1 F5 143.30(13) . 3_665
F2 U1 F3 86.43(13) . .
F5 U1 F3 71.30(12) 3_665 .
F2 U1 F1 76.63(12) . .
F5 U1 F1 96.37(13) 3_665 .
F3 U1 F1 131.53(12) . .
F2 U1 F5 139.57(13) . .
F5 U1 F5 72.30(18) 3_665 .
F3 U1 F5 93.09(13) . .
F1 U1 F5 128.59(12) . .
F2 U1 F4 73.65(14) . .
F5 U1 F4 141.44(13) 3_665 .
F3 U1 F4 137.90(13) . .
F1 U1 F4 79.96(14) . .
F5 U1 F4 80.23(14) . .
F2 U1 F2 71.33(14) . 8_556
F5 U1 F2 123.68(13) 3_665 8_556
F3 U1 F2 70.04(12) . 8_556
F1 U1 F2 139.95(13) . 8_556
F5 U1 F2 70.61(12) . 8_556
F4 U1 F2 68.54(13) . 8_556
F2 U1 F1 129.05(12) . 4
F5 U1 F1 72.76(12) 3_665 4
F3 U1 F1 142.97(13) . 4
F1 U1 F1 61.31(15) . 4
F5 U1 F1 67.52(12) . 4
F4 U1 F1 71.97(13) . 4
F2 U1 F1 125.92(12) 8_556 4
F2 U1 F3 72.40(13) . 7_666
F5 U1 F3 71.66(13) 3_665 7_666
F3 U1 F3 63.85(14) . 7_666
F1 U1 F3 67.75(12) . 7_666
F5 U1 F3 141.90(13) . 7_666
F4 U1 F3 137.38(14) . 7_666
F2 U1 F3 121.89(12) 8_556 7_666
F1 U1 F3 112.18(12) 4 7_666
F2 U1 Na1 66.89(10) . .
F5 U1 Na1 87.62(9) 3_665 .
F3 U1 Na1 98.88(10) . .
F1 U1 Na1 32.73(10) . .
F5 U1 Na1 151.96(10) . .
F4 U1 Na1 106.29(11) . .
F2 U1 Na1 137.37(10) 8_556 .
F1 U1 Na1 88.23(11) 4 .
F3 U1 Na1 35.54(9) 7_666 .
F2 U1 Na2 42.33(9) . .
F5 U1 Na2 166.44(9) 3_665 .
F3 U1 Na2 99.89(9) . .
F1 U1 Na2 97.17(9) . .
F5 U1 Na2 98.52(9) . .
F4 U1 Na2 41.71(10) . .
F2 U1 Na2 42.78(9) 8_556 .
F1 U1 Na2 113.57(9) 4 .
F3 U1 Na2 114.39(9) 7_666 .
Na1 U1 Na2 104.209(19) . .
F2 U1 U1 77.41(9) . 7_666
F5 U1 U1 68.03(9) 3_665 7_666
F3 U1 U1 32.73(9) . 7_666
F1 U1 U1 98.84(9) . 7_666
F5 U1 U1 120.33(9) . 7_666
F4 U1 U1 150.52(10) . 7_666
F2 U1 U1 96.99(8) 8_556 7_666
F1 U1 U1 133.40(9) 4 7_666
F3 U1 U1 31.13(8) 7_666 7_666
Na1 U1 U1 66.35(5) . 7_666
Na2 U1 U1 110.344(7) . 7_666
F4 Ti1 F4 174.1(3) . 6
F4 Ti1 F4 95.1(3) . 5
F4 Ti1 F4 89.20(17) 6 5
F4 Ti1 F4 89.20(17) . 2
F4 Ti1 F4 86.8(2) 6 2
F4 Ti1 F4 174.1(3) 5 2
F4 Ti1 F4 86.8(2) . 4
F4 Ti1 F4 89.20(17) 6 4
F4 Ti1 F4 89.20(17) 5 4
F4 Ti1 F4 95.1(3) 2 4
F4 Ti1 F4 89.20(17) . 3
F4 Ti1 F4 95.1(3) 6 3
F4 Ti1 F4 86.8(2) 5 3
F4 Ti1 F4 89.20(17) 2 3
F4 Ti1 F4 174.1(3) 4 3
F4 Ti1 Na2 54.17(12) . .
F4 Ti1 Na2 125.83(12) 6 .
F4 Ti1 Na2 125.83(12) 5 .
F4 Ti1 Na2 54.17(12) 2 .
F4 Ti1 Na2 125.83(12) 4 .
F4 Ti1 Na2 54.17(12) 3 .
F4 Ti1 Na2 125.83(12) . 4
F4 Ti1 Na2 54.17(12) 6 4
F4 Ti1 Na2 54.17(12) 5 4
F4 Ti1 Na2 125.83(12) 2 4
F4 Ti1 Na2 54.17(12) 4 4
F4 Ti1 Na2 125.83(12) 3 4
Na2 Ti1 Na2 180.0 . 4
F1 Na1 F1 110.67(12) 3_565 2_665
F1 Na1 F1 110.67(12) 3_565 .
F1 Na1 F1 110.67(12) 2_665 .
F1 Na1 F3 90.09(13) 3_565 8_566
F1 Na1 F3 69.98(13) 2_665 8_566
F1 Na1 F3 156.33(19) . 8_566
F1 Na1 F3 69.98(13) 3_565 9_556
F1 Na1 F3 156.33(19) 2_665 9_556
F1 Na1 F3 90.09(13) . 9_556
F3 Na1 F3 86.43(17) 8_566 9_556
F1 Na1 F3 156.33(19) 3_565 7_666
F1 Na1 F3 90.09(13) 2_665 7_666
F1 Na1 F3 69.98(13) . 7_666
F3 Na1 F3 86.43(17) 8_566 7_666
F3 Na1 F3 86.43(17) 9_556 7_666
F1 Na1 U1 136.41(10) 3_565 .
F1 Na1 U1 107.47(9) 2_665 .
F1 Na1 U1 33.55(9) . .
F3 Na1 U1 122.81(15) 8_566 .
F3 Na1 U1 83.32(10) 9_556 .
F3 Na1 U1 36.97(9) 7_666 .
F1 Na1 U1 107.46(9) 3_565 2_665
F1 Na1 U1 33.55(9) 2_665 2_665
F1 Na1 U1 136.41(10) . 2_665
F3 Na1 U1 36.97(9) 8_566 2_665
F3 Na1 U1 122.81(15) 9_556 2_665
F3 Na1 U1 83.32(10) 7_666 2_665
U1 Na1 U1 115.98(4) . 2_665
F1 Na1 U1 33.55(9) 3_565 3_565
F1 Na1 U1 136.41(10) 2_665 3_565
F1 Na1 U1 107.47(9) . 3_565
F3 Na1 U1 83.32(10) 8_566 3_565
F3 Na1 U1 36.97(9) 9_556 3_565
F3 Na1 U1 122.81(15) 7_666 3_565
U1 Na1 U1 115.98(4) . 3_565
U1 Na1 U1 115.98(4) 2_665 3_565
F1 Na1 U1 31.82(10) 3_565 5_565
F1 Na1 U1 96.35(14) 2_665 5_565
F1 Na1 U1 91.23(13) . 5_565
F3 Na1 U1 112.37(10) 8_566 5_565
F3 Na1 U1 94.37(10) 9_556 5_565
F3 Na1 U1 161.20(12) 7_666 5_565
U1 Na1 U1 124.41(6) . 5_565
U1 Na1 U1 111.52(5) 2_665 5_565
U1 Na1 U1 62.24(2) 3_565 5_565
F1 Na1 U1 91.23(13) 3_565 6_665
F1 Na1 U1 31.82(10) 2_665 6_665
F1 Na1 U1 96.35(14) . 6_665
F3 Na1 U1 94.37(10) 8_566 6_665
F3 Na1 U1 161.20(12) 9_556 6_665
F3 Na1 U1 112.37(10) 7_666 6_665
U1 Na1 U1 111.51(5) . 6_665
U1 Na1 U1 62.24(2) 2_665 6_665
U1 Na1 U1 124.41(6) 3_565 6_665
U1 Na1 U1 67.93(6) 5_565 6_665
F1 Na1 U1 96.35(14) 3_565 4
F1 Na1 U1 91.23(13) 2_665 4
F1 Na1 U1 31.81(10) . 4
F3 Na1 U1 161.20(12) 8_566 4
F3 Na1 U1 112.37(10) 9_556 4
F3 Na1 U1 94.37(10) 7_666 4
U1 Na1 U1 62.23(2) . 4
U1 Na1 U1 124.41(6) 2_665 4
U1 Na1 U1 111.52(5) 3_565 4
U1 Na1 U1 67.93(6) 5_565 4
U1 Na1 U1 67.93(6) 6_665 4
F4 Na2 F4 180.0 9_556 3
F4 Na2 F4 61.49(14) 9_556 8_556
F4 Na2 F4 118.51(14) 3 8_556
F4 Na2 F4 118.51(14) 9_556 2
F4 Na2 F4 61.49(14) 3 2
F4 Na2 F4 180.00(10) 8_556 2
F4 Na2 F4 61.49(14) 9_556 7_556
F4 Na2 F4 118.51(14) 3 7_556
F4 Na2 F4 61.49(14) 8_556 7_556
F4 Na2 F4 118.51(14) 2 7_556
F4 Na2 F4 118.51(14) 9_556 .
F4 Na2 F4 61.49(14) 3 .
F4 Na2 F4 118.51(14) 8_556 .
F4 Na2 F4 61.49(14) 2 .
F4 Na2 F4 180.00(10) 7_556 .
F4 Na2 F2 74.99(12) 9_556 8_556
F4 Na2 F2 105.01(12) 3 8_556
F4 Na2 F2 62.60(12) 8_556 8_556
F4 Na2 F2 117.40(12) 2 8_556
F4 Na2 F2 120.33(11) 7_556 8_556
F4 Na2 F2 59.67(11) . 8_556
F4 Na2 F2 105.01(12) 9_556 2
F4 Na2 F2 74.99(12) 3 2
F4 Na2 F2 117.40(12) 8_556 2
F4 Na2 F2 62.60(12) 2 2
F4 Na2 F2 59.67(11) 7_556 2
F4 Na2 F2 120.33(11) . 2
F2 Na2 F2 180.0 8_556 2
F4 Na2 F2 120.33(11) 9_556 7_556
F4 Na2 F2 59.67(11) 3 7_556
F4 Na2 F2 74.99(12) 8_556 7_556
F4 Na2 F2 105.01(12) 2 7_556
F4 Na2 F2 62.60(12) 7_556 7_556
F4 Na2 F2 117.40(12) . 7_556
F2 Na2 F2 119.23(2) 8_556 7_556
F2 Na2 F2 60.77(2) 2 7_556
F4 Na2 F2 59.67(11) 9_556 .
F4 Na2 F2 120.33(11) 3 .
F4 Na2 F2 105.01(12) 8_556 .
F4 Na2 F2 74.99(12) 2 .
F4 Na2 F2 117.40(12) 7_556 .
F4 Na2 F2 62.60(12) . .
F2 Na2 F2 60.77(2) 8_556 .
F2 Na2 F2 119.23(2) 2 .
F2 Na2 F2 180.0 7_556 .
F4 Na2 F2 62.60(12) 9_556 9_556
F4 Na2 F2 117.40(12) 3 9_556
F4 Na2 F2 120.33(11) 8_556 9_556
F4 Na2 F2 59.67(11) 2 9_556
F4 Na2 F2 74.99(12) 7_556 9_556
F4 Na2 F2 105.01(12) . 9_556
F2 Na2 F2 119.23(2) 8_556 9_556
F2 Na2 F2 60.77(2) 2 9_556
F2 Na2 F2 119.23(2) 7_556 9_556
F2 Na2 F2 60.77(2) . 9_556
F4 Na2 F2 117.40(12) 9_556 3
F4 Na2 F2 62.60(12) 3 3
F4 Na2 F2 59.67(11) 8_556 3
F4 Na2 F2 120.33(11) 2 3
F4 Na2 F2 105.01(12) 7_556 3
F4 Na2 F2 74.99(12) . 3
F2 Na2 F2 60.77(2) 8_556 3
F2 Na2 F2 119.23(2) 2 3
F2 Na2 F2 60.77(2) 7_556 3
F2 Na2 F2 119.23(2) . 3
F2 Na2 F2 180.0 9_556 3
Na1 F1 U1 113.72(17) . .
Na1 F1 U1 118.47(18) . 4
U1 F1 U1 118.53(15) . 4
U1 F2 U1 152.30(17) . 9_556
U1 F2 Na2 102.72(13) . .
U1 F2 Na2 100.33(12) 9_556 .
U1 F3 Na1 135.17(18) . 7_666
U1 F3 U1 116.15(14) . 7_666
Na1 F3 U1 107.49(15) 7_666 7_666
Ti1 F4 U1 151.3(2) . .
Ti1 F4 Na2 89.65(15) . .
U1 F4 Na2 102.31(15) . .
U1 F5 U1 153.27(17) 2_655 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 F2 2.266(3) .
U1 F5 2.285(3) 3_665
U1 F3 2.307(3) .
U1 F1 2.310(3) .
U1 F5 2.318(3) .
U1 F4 2.321(4) .
U1 F2 2.355(3) 8_556
U1 F1 2.404(3) 4
U1 F3 2.413(4) 7_666
U1 Na1 3.8262(9) .
U1 Na2 3.8595(2) .
U1 U1 4.0060(4) 7_666
Ti1 F4 1.914(4) .
Ti1 F4 1.914(4) 6
Ti1 F4 1.914(4) 5
Ti1 F4 1.914(4) 2
Ti1 F4 1.914(4) 4
Ti1 F4 1.914(4) 3
Ti1 Na2 3.2417(2) .
Ti1 Na2 3.2417(2) 4
Na1 F1 2.260(4) 3_565
Na1 F1 2.260(4) 2_665
Na1 F1 2.260(4) .
Na1 F3 2.332(4) 8_566
Na1 F3 2.332(4) 9_556
Na1 F3 2.332(4) 7_666
Na1 U1 3.8262(8) 2_665
Na1 U1 3.8262(8) 3_565
Na1 U1 4.008(3) 5_565
Na1 U1 4.008(3) 6_665
Na1 U1 4.008(3) 4
Na2 F4 2.628(4) 9_556
Na2 F4 2.628(4) 3
Na2 F4 2.628(4) 8_556
Na2 F4 2.628(4) 2
Na2 F4 2.628(4) 7_556
Na2 F4 2.628(4) .
Na2 F2 2.664(4) 8_556
Na2 F2 2.664(4) 2
Na2 F2 2.664(4) 7_556
Na2 F2 2.664(4) .
Na2 F2 2.664(4) 9_556
Na2 F2 2.664(4) 3
F1 U1 2.404(3) 4
F2 U1 2.355(3) 9_556
F3 Na1 2.332(4) 7_666
F3 U1 2.413(4) 7_666
F5 U1 2.285(3) 2_655
