#------------------------------------------------------------------------------
#$Date: 2016-03-24 00:10:55 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179526 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/23/4342340.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_4342340
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 Ga Na3 U6'
_chemical_formula_sum            'F30 Ga Na3 U6'
_chemical_formula_weight         2136.87
_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'
_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                   9.84880(10)
_cell_length_b                   9.84880(10)
_cell_length_c                   12.9757(3)
_cell_measurement_reflns_used    5998
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.2634
_cell_measurement_theta_min      2.3879
_cell_volume                     1090.00(3)
_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-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0119
_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       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13727
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         2.39
_exptl_absorpt_coefficient_mu    45.925
_exptl_absorpt_correction_T_max  0.1203
_exptl_absorpt_correction_T_min  0.0727
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    6.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'trigonal dipyramid'
_exptl_crystal_F_000             1772
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.560
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.269
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.192
_refine_ls_matrix_type           full
_refine_ls_number_parameters     62
_refine_ls_number_reflns         913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.192
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0203
_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)+(0.0265P)²+9.8294P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0518
_refine_ls_wR_factor_ref         0.0523
_reflns_number_gt                889
_reflns_number_total             913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic503034t_si_002.cif
_cod_data_source_block           Na3GaU6F30
_cod_depositor_comments
'Adding full bibliography for 4342339--4342344.cif.'
_cod_database_code               4342340
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 0.67681(2) 0.60039(2) 0.102255(16) 0.00960(10) Uani 1 1 d .
Ga1 Ga 1.0000 1.0000 0.2500 0.0103(3) Uani 1 6 d S
Na1 Na 0.3333 0.6667 0.1646(4) 0.0188(9) Uani 1 3 d S
Na2 Na 1.0000 1.0000 0.0000 0.043(2) Uani 1 6 d S
F1 F 0.5665(5) 0.6978(5) 0.2154(3) 0.0208(8) Uani 1 1 d .
F2 F 0.6927(4) 0.8078(4) 0.0173(3) 0.0161(7) Uani 1 1 d .
F3 F 0.5872(4) 0.4677(4) -0.0518(3) 0.0160(7) Uani 1 1 d .
F4 F 0.9182(5) 1.0967(5) 0.1642(3) 0.0186(8) Uani 1 1 d .
F5 F 0.8296(5) 0.4879(5) 0.1385(3) 0.0205(8) 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'
Ga Ga 0.2307 1.6083 '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 143.11(14) . 2_655
F2 U1 F1 76.56(14) . .
F5 U1 F1 96.53(15) 2_655 .
F2 U1 F3 85.59(14) . .
F5 U1 F3 71.91(14) 2_655 .
F1 U1 F3 131.41(13) . .
F2 U1 F5 139.78(14) . .
F5 U1 F5 72.2(2) 2_655 .
F1 U1 F5 128.61(14) . .
F3 U1 F5 93.51(14) . .
F2 U1 F4 73.96(14) . 2_765
F5 U1 F4 141.32(14) 2_655 2_765
F1 U1 F4 79.79(14) . 2_765
F3 U1 F4 137.63(14) . 2_765
F5 U1 F4 80.28(14) . 2_765
F2 U1 F2 71.12(14) . 9_655
F5 U1 F2 124.12(14) 2_655 9_655
F1 U1 F2 139.34(14) . 9_655
F3 U1 F2 70.21(13) . 9_655
F5 U1 F2 70.83(14) . 9_655
F4 U1 F2 68.17(13) 2_765 9_655
F2 U1 F1 129.22(13) . 4
F5 U1 F1 72.89(14) 2_655 4
F1 U1 F1 61.53(17) . 4
F3 U1 F1 143.70(13) . 4
F5 U1 F1 67.30(14) . 4
F4 U1 F1 71.65(14) 2_765 4
F2 U1 F1 125.45(14) 9_655 4
F2 U1 F3 72.45(13) . 7_665
F5 U1 F3 71.44(14) 2_655 7_665
F1 U1 F3 67.89(13) . 7_665
F3 U1 F3 63.67(15) . 7_665
F5 U1 F3 141.59(14) . 7_665
F4 U1 F3 137.61(13) 2_765 7_665
F2 U1 F3 122.20(12) 9_655 7_665
F1 U1 F3 112.35(13) 4 7_665
F2 U1 Na1 67.48(10) . .
F5 U1 Na1 87.22(11) 2_655 .
F1 U1 Na1 32.31(11) . .
F3 U1 Na1 99.12(11) . .
F5 U1 Na1 151.16(12) . .
F4 U1 Na1 106.24(11) 2_765 .
F2 U1 Na1 137.93(11) 9_655 .
F1 U1 Na1 87.75(12) 4 .
F3 U1 Na1 35.97(10) 7_665 .
F2 U1 Na2 42.23(10) . .
F5 U1 Na2 166.86(11) 2_655 .
F1 U1 Na2 96.59(11) . .
F3 U1 Na2 99.59(9) . .
F5 U1 Na2 98.96(10) . .
F4 U1 Na2 41.72(9) 2_765 .
F2 U1 Na2 42.75(9) 9_655 .
F1 U1 Na2 113.25(10) 4 .
F3 U1 Na2 114.39(9) 7_665 .
Na1 U1 Na2 104.30(2) . .
F2 U1 Na1 159.65(10) . 4
F5 U1 Na1 48.42(11) 2_655 4
F1 U1 Na1 85.96(11) . 4
F3 U1 Na1 114.11(10) . 4
F5 U1 Na1 48.53(10) . 4
F4 U1 Na1 92.94(10) 2_765 4
F2 U1 Na1 119.00(10) 9_655 4
F1 U1 Na1 30.47(10) 4 4
F3 U1 Na1 110.67(9) 7_665 4
Na1 U1 Na1 102.67(3) . 4
Na2 U1 Na1 132.225(17) . 4
F4 Ga1 F4 175.6(3) 2_765 6_765
F4 Ga1 F4 94.5(2) 2_765 4
F4 Ga1 F4 88.73(17) 6_765 4
F4 Ga1 F4 88.3(2) 2_765 5_675
F4 Ga1 F4 88.73(17) 6_765 5_675
F4 Ga1 F4 88.73(17) 4 5_675
F4 Ga1 F4 88.73(17) 2_765 .
F4 Ga1 F4 88.3(2) 6_765 .
F4 Ga1 F4 175.6(3) 4 .
F4 Ga1 F4 94.5(2) 5_675 .
F4 Ga1 F4 88.73(17) 2_765 3_675
F4 Ga1 F4 94.5(3) 6_765 3_675
F4 Ga1 F4 88.3(2) 4 3_675
F4 Ga1 F4 175.6(3) 5_675 3_675
F4 Ga1 F4 88.73(17) . 3_675
F4 Ga1 Na2 126.16(12) 2_765 4
F4 Ga1 Na2 53.84(12) 6_765 4
F4 Ga1 Na2 53.84(12) 4 4
F4 Ga1 Na2 53.84(12) 5_675 4
F4 Ga1 Na2 126.16(12) . 4
F4 Ga1 Na2 126.16(12) 3_675 4
F4 Ga1 Na2 53.84(12) 2_765 .
F4 Ga1 Na2 126.16(12) 6_765 .
F4 Ga1 Na2 126.16(12) 4 .
F4 Ga1 Na2 126.16(12) 5_675 .
F4 Ga1 Na2 53.84(12) . .
F4 Ga1 Na2 53.84(12) 3_675 .
Na2 Ga1 Na2 180.0 4 .
F1 Na1 F1 111.85(14) 2_665 3_565
F1 Na1 F1 111.85(14) 2_665 .
F1 Na1 F1 111.85(14) 3_565 .
F1 Na1 F3 88.93(15) 2_665 9
F1 Na1 F3 69.90(14) 3_565 9
F1 Na1 F3 155.1(2) . 9
F1 Na1 F3 69.90(14) 2_665 8_565
F1 Na1 F3 155.1(2) 3_565 8_565
F1 Na1 F3 88.93(15) . 8_565
F3 Na1 F3 85.44(19) 9 8_565
F1 Na1 F3 155.1(2) 2_665 7_665
F1 Na1 F3 88.93(15) 3_565 7_665
F1 Na1 F3 69.90(14) . 7_665
F3 Na1 F3 85.44(19) 9 7_665
F3 Na1 F3 85.44(19) 8_565 7_665
F1 Na1 F5 62.34(16) 2_665 4
F1 Na1 F5 104.4(2) 3_565 4
F1 Na1 F5 57.88(15) . 4
F3 Na1 F5 147.01(15) 9 4
F3 Na1 F5 98.22(13) 8_565 4
F3 Na1 F5 127.47(13) 7_665 4
F1 Na1 F5 57.88(15) 2_665 6_665
F1 Na1 F5 62.34(16) 3_565 6_665
F1 Na1 F5 104.4(2) . 6_665
F3 Na1 F5 98.22(13) 9 6_665
F3 Na1 F5 127.47(13) 8_565 6_665
F3 Na1 F5 147.01(15) 7_665 6_665
F5 Na1 F5 53.79(16) 4 6_665
F1 Na1 F5 104.4(2) 2_665 5_565
F1 Na1 F5 57.88(15) 3_565 5_565
F1 Na1 F5 62.34(16) . 5_565
F3 Na1 F5 127.47(13) 9 5_565
F3 Na1 F5 147.01(15) 8_565 5_565
F3 Na1 F5 98.22(13) 7_665 5_565
F5 Na1 F5 53.79(16) 4 5_565
F5 Na1 F5 53.79(16) 6_665 5_565
F1 Na1 U1 106.97(11) 2_665 3_565
F1 Na1 U1 33.03(11) 3_565 3_565
F1 Na1 U1 136.98(11) . 3_565
F3 Na1 U1 37.27(9) 9 3_565
F3 Na1 U1 122.04(17) 8_565 3_565
F3 Na1 U1 82.65(11) 7_665 3_565
F5 Na1 U1 132.89(14) 4 3_565
F5 Na1 U1 80.97(8) 6_665 3_565
F5 Na1 U1 90.90(8) 5_565 3_565
F1 Na1 U1 33.03(11) 2_665 2_665
F1 Na1 U1 136.98(11) 3_565 2_665
F1 Na1 U1 106.97(11) . 2_665
F3 Na1 U1 82.65(11) 9 2_665
F3 Na1 U1 37.27(9) 8_565 2_665
F3 Na1 U1 122.04(17) 7_665 2_665
F5 Na1 U1 80.97(8) 4 2_665
F5 Na1 U1 90.90(8) 6_665 2_665
F5 Na1 U1 132.89(14) 5_565 2_665
U1 Na1 U1 115.68(5) 3_565 2_665
F1 Na1 U1 136.98(11) 2_665 .
F1 Na1 U1 106.97(11) 3_565 .
F1 Na1 U1 33.03(11) . .
F3 Na1 U1 122.04(17) 9 .
F3 Na1 U1 82.65(11) 8_565 .
F3 Na1 U1 37.27(9) 7_665 .
F5 Na1 U1 90.90(8) 4 .
F5 Na1 U1 132.89(14) 6_665 .
F5 Na1 U1 80.97(8) 5_565 .
U1 Na1 U1 115.68(5) 3_565 .
U1 Na1 U1 115.68(5) 2_665 .
F4 Na2 F4 180.0(2) 3_675 9_655
F4 Na2 F4 60.51(13) 3_675 2_765
F4 Na2 F4 119.49(13) 9_655 2_765
F4 Na2 F4 60.51(13) 3_675 .
F4 Na2 F4 119.49(13) 9_655 .
F4 Na2 F4 60.51(13) 2_765 .
F4 Na2 F4 119.49(13) 3_675 7_775
F4 Na2 F4 60.51(13) 9_655 7_775
F4 Na2 F4 119.49(13) 2_765 7_775
F4 Na2 F4 180.0 . 7_775
F4 Na2 F4 119.49(13) 3_675 8_565
F4 Na2 F4 60.51(13) 9_655 8_565
F4 Na2 F4 180.0 2_765 8_565
F4 Na2 F4 119.49(13) . 8_565
F4 Na2 F4 60.51(13) 7_775 8_565
F4 Na2 F2 104.93(12) 3_675 9_655
F4 Na2 F2 75.07(12) 9_655 9_655
F4 Na2 F2 59.97(11) 2_765 9_655
F4 Na2 F2 116.67(12) . 9_655
F4 Na2 F2 63.33(12) 7_775 9_655
F4 Na2 F2 120.03(11) 8_565 9_655
F4 Na2 F2 120.03(11) 3_675 .
F4 Na2 F2 59.97(11) 9_655 .
F4 Na2 F2 63.33(12) 2_765 .
F4 Na2 F2 75.07(12) . .
F4 Na2 F2 104.93(12) 7_775 .
F4 Na2 F2 116.67(12) 8_565 .
F2 Na2 F2 60.71(2) 9_655 .
F4 Na2 F2 59.97(11) 3_675 7_775
F4 Na2 F2 120.03(11) 9_655 7_775
F4 Na2 F2 116.67(12) 2_765 7_775
F4 Na2 F2 104.93(12) . 7_775
F4 Na2 F2 75.07(12) 7_775 7_775
F4 Na2 F2 63.33(12) 8_565 7_775
F2 Na2 F2 119.29(2) 9_655 7_775
F2 Na2 F2 180.00(15) . 7_775
F4 Na2 F2 75.07(12) 3_675 3_675
F4 Na2 F2 104.93(12) 9_655 3_675
F4 Na2 F2 120.03(11) 2_765 3_675
F4 Na2 F2 63.33(12) . 3_675
F4 Na2 F2 116.67(12) 7_775 3_675
F4 Na2 F2 59.97(11) 8_565 3_675
F2 Na2 F2 180.000(1) 9_655 3_675
F2 Na2 F2 119.29(2) . 3_675
F2 Na2 F2 60.71(2) 7_775 3_675
F4 Na2 F2 63.33(12) 3_675 2_765
F4 Na2 F2 116.67(12) 9_655 2_765
F4 Na2 F2 75.07(12) 2_765 2_765
F4 Na2 F2 120.03(11) . 2_765
F4 Na2 F2 59.97(11) 7_775 2_765
F4 Na2 F2 104.93(12) 8_565 2_765
F2 Na2 F2 60.71(2) 9_655 2_765
F2 Na2 F2 119.29(2) . 2_765
F2 Na2 F2 60.71(2) 7_775 2_765
F2 Na2 F2 119.29(2) 3_675 2_765
F4 Na2 F2 116.67(12) 3_675 8_565
F4 Na2 F2 63.33(12) 9_655 8_565
F4 Na2 F2 104.93(12) 2_765 8_565
F4 Na2 F2 59.97(11) . 8_565
F4 Na2 F2 120.03(11) 7_775 8_565
F4 Na2 F2 75.07(12) 8_565 8_565
F2 Na2 F2 119.29(2) 9_655 8_565
F2 Na2 F2 60.71(2) . 8_565
F2 Na2 F2 119.29(2) 7_775 8_565
F2 Na2 F2 60.71(2) 3_675 8_565
F2 Na2 F2 180.000(1) 2_765 8_565
Na1 F1 U1 114.65(19) . .
Na1 F1 U1 116.7(2) . 4
U1 F1 U1 118.37(17) . 4
U1 F2 U1 152.78(19) . 8_565
U1 F2 Na2 102.98(13) . .
U1 F2 Na2 100.20(13) 8_565 .
U1 F3 Na1 135.71(18) . 7_665
U1 F3 U1 116.33(15) . 7_665
Na1 F3 U1 106.76(15) 7_665 7_665
Ga1 F4 U1 150.3(2) . 3_675
Ga1 F4 Na2 90.58(14) . .
U1 F4 Na2 101.67(14) 3_675 .
U1 F5 U1 152.6(2) 3_665 .
U1 F5 Na1 96.82(13) 3_665 4
U1 F5 Na1 96.03(13) . 4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 F2 2.257(4) .
U1 F5 2.283(4) 2_655
U1 F1 2.302(4) .
U1 F3 2.309(4) .
U1 F5 2.319(4) .
U1 F4 2.347(4) 2_765
U1 F2 2.360(3) 9_655
U1 F1 2.413(4) 4
U1 F3 2.428(4) 7_665
Ga1 F4 1.887(4) 2_765
Ga1 F4 1.887(4) 6_765
Ga1 F4 1.887(4) 4
Ga1 F4 1.887(4) 5_675
Ga1 F4 1.887(4) .
Ga1 F4 1.887(4) 3_675
Na1 F1 2.257(4) 2_665
Na1 F1 2.257(4) 3_565
Na1 F1 2.257(4) .
Na1 F3 2.355(5) 9
Na1 F3 2.355(5) 8_565
Na1 F3 2.355(5) 7_665
Na1 F5 2.996(6) 4
Na1 F5 2.996(6) 6_665
Na1 F5 2.996(6) 5_565
Na2 F4 2.619(4) 3_675
Na2 F4 2.619(4) 9_655
Na2 F4 2.619(4) 2_765
Na2 F4 2.619(4) .
Na2 F4 2.619(4) 7_775
Na2 F4 2.619(4) 8_565
Na2 F2 2.658(4) 9_655
Na2 F2 2.658(4) .
Na2 F2 2.658(4) 7_775
Na2 F2 2.658(4) 3_675
Na2 F2 2.658(4) 2_765
Na2 F2 2.658(4) 8_565
F1 U1 2.413(4) 4
F2 U1 2.360(3) 8_565
F3 Na1 2.355(5) 7_665
F3 U1 2.428(4) 7_665
F4 U1 2.347(4) 3_675
F5 U1 2.283(4) 3_665
F5 Na1 2.996(6) 4
