#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:41:30 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179488 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/85/4338516.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_4338516
loop_
_publ_author_name
'Yeon, Jeongho'
'Smith, Mark D.'
'Tapp, Joshua'
'Möller, Angela'
'Zur Loye, Hans-Conrad'
_publ_section_title
;
 Mild Hydrothermal Crystal Growth, Structure, and Magnetic Properties of
 Ternary U(IV) Containing Fluorides: LiUF5, KU2F9, K7U6F31, RbUF5, RbU2F9,
 and RbU3F13.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6289
_journal_page_last               6298
_journal_paper_doi               10.1021/ic5008507
_journal_volume                  53
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'F13 Rb U3'
_chemical_formula_sum            'F13 Rb U3'
_chemical_formula_weight         1046.56
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_symmetry_space_group_name_Hall  'P 2c -2'
_symmetry_space_group_name_H-M   'P m c 21'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-18
_audit_creation_method
;
  Olex2 1.1
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9943(6)
_cell_length_b                   7.3217(5)
_cell_length_c                   8.4677(6)
_cell_measurement_reflns_used    5209
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.301
_cell_measurement_theta_min      2.548
_cell_volume                     495.63(6)
_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  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            14717
_diffrn_reflns_theta_full        36.40
_diffrn_reflns_theta_max         36.40
_diffrn_reflns_theta_min         2.41
_diffrn_source                   'sealed tube'
_diffrn_source_current           37.0
_diffrn_source_power             1.739
_diffrn_source_target            Mo
_diffrn_source_voltage           47.0
_exptl_absorpt_coefficient_mu    53.939
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.179815
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1715 before and 0.0479 after correction.
The Ratio of minimum to maximum transmission is 0.1798.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    7.013
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular block'
_exptl_crystal_F_000             860
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.05
_refine_diff_density_max         4.853
_refine_diff_density_min         -6.134
_refine_diff_density_rms         0.555
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.30(2)
_refine_ls_extinction_coef       0.0058(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         2490
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0417
_refine_ls_R_factor_gt           0.0400
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0754P)²+1.8560P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                2386
_reflns_number_total             2490
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5008507_si_002.cif
_cod_data_source_block           RbU3F13
_cod_depositor_comments
'Adding full bibliography for 4338511--4338516.cif.'
_cod_database_code               4338516
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 '-x, y, z'
4 '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 0.25281(4) 0.10441(3) 0.12730(7) 0.00555(9) Uani 1 1 d .
U2 U 0.0000 0.39081(5) 0.46370(7) 0.00531(10) Uani 1 2 d S
Rb1 Rb 0.5000 0.60578(17) 0.26538(18) 0.0124(3) Uani 1 2 d S
F1 F 0.1723(8) 0.1948(7) 0.5966(6) 0.0098(10) Uani 1 1 d .
F2 F 0.1958(9) 0.3898(7) 0.0052(8) 0.0106(11) Uani 1 1 d .
F3 F 0.2581(6) 0.3224(8) 0.3176(8) 0.0101(11) Uani 1 1 d .
F4 F 0.3018(7) -0.0486(8) 0.3665(6) 0.0083(9) Uani 1 1 d .
F5 F 0.5000 -0.0608(13) 0.1146(10) 0.0111(15) Uani 1 2 d S
F6 F 0.5000 0.2725(11) 0.0896(10) 0.0097(14) Uani 1 2 d S
F7 F 0.0000 0.0979(11) 0.0000(11) 0.0101(16) Uani 1 2 d S
F8 F 0.0000 0.1380(11) 0.2833(9) 0.0060(13) Uani 1 2 d S
F9 F 0.0000 0.5307(11) 0.2275(11) 0.0109(16) Uani 1 2 d S
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'
Rb Rb -0.9393 2.9676 '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
U1 U1 U1 180.0 3_655 3
U1 U1 U2 119.743(7) 3_655 .
U1 U1 U2 60.256(7) 3 .
F1 U1 U1 106.27(16) 4_554 3_655
F1 U1 U1 73.73(16) 4_554 3
F1 U1 U2 115.51(15) 4_554 .
F1 U1 F2 137.4(2) 4_554 .
F1 U1 F4 71.9(2) 4_554 .
F1 U1 F5 74.7(3) 4_554 .
F1 U1 F6 136.0(2) 4_554 .
F1 U1 F8 85.7(2) 4_554 .
F2 U1 U1 101.05(17) . 3_655
F2 U1 U1 78.95(17) . 3
F2 U1 U2 75.90(16) . .
F2 U1 F8 89.3(3) . .
F3 U1 U1 91.06(13) . 3
F3 U1 U1 88.94(13) . 3_655
F3 U1 U2 31.82(13) . .
F3 U1 F1 139.1(2) . 4_554
F3 U1 F2 72.2(2) . .
F3 U1 F4 144.2(2) . 4_554
F3 U1 F4 73.7(2) . .
F3 U1 F5 112.6(2) . .
F3 U1 F6 73.3(2) . .
F3 U1 F7 111.4(2) . .
F3 U1 F8 63.7(2) . .
F4 U1 U1 99.90(14) 4_554 3
F4 U1 U1 99.61(14) . 3
F4 U1 U1 80.10(14) 4_554 3_655
F4 U1 U1 80.39(14) . 3_655
F4 U1 U2 74.05(14) . .
F4 U1 U2 148.74(15) 4_554 .
F4 U1 F1 76.6(2) 4_554 4_554
F4 U1 F2 145.8(2) . .
F4 U1 F2 76.6(2) 4_554 .
F4 U1 F4 136.18(13) 4_554 .
F4 U1 F5 73.4(3) 4_554 .
F4 U1 F6 103.1(2) . .
F4 U1 F6 79.5(3) 4_554 .
F4 U1 F7 72.1(3) 4_554 .
F4 U1 F8 133.5(2) 4_554 .
F4 U1 F8 73.6(2) . .
F5 U1 U1 31.6(2) . 3_655
F5 U1 U1 148.4(2) . 3
F5 U1 U2 136.4(2) . .
F5 U1 F2 127.0(3) . .
F5 U1 F4 69.4(3) . .
F5 U1 F6 63.3(3) . .
F5 U1 F8 142.0(3) . .
F6 U1 U1 32.76(17) . 3_655
F6 U1 U1 147.24(17) . 3
F6 U1 U2 104.0(2) . .
F6 U1 F2 69.0(2) . .
F6 U1 F8 136.2(3) . .
F7 U1 U1 151.9(2) . 3_655
F7 U1 U1 28.1(2) . 3
F7 U1 U2 84.4(2) . .
F7 U1 F1 71.3(2) . 4_554
F7 U1 F2 69.2(3) . .
F7 U1 F4 122.9(2) . .
F7 U1 F5 136.0(3) . .
F7 U1 F6 133.5(3) . .
F7 U1 F8 61.5(3) . .
F8 U1 U1 146.39(16) . 3_655
F8 U1 U1 33.61(16) . 3
F8 U1 U2 32.24(18) . .
U1 U2 U1 59.487(14) 3 .
U1 U2 Rb1 110.55(2) . 1_455
U1 U2 Rb1 59.413(18) 3 1_455
F1 U2 U1 108.67(14) 3 .
F1 U2 U1 73.87(14) . .
F1 U2 U1 108.67(14) . 3
F1 U2 U1 73.87(14) 3 3
F1 U2 Rb1 156.32(15) . 1_455
F1 U2 Rb1 82.61(16) 3 1_455
F1 U2 F1 74.1(3) . 3
F1 U2 F3 128.74(19) 3 .
F1 U2 F3 67.3(2) . .
F1 U2 F3 67.3(2) 3 3
F1 U2 F3 128.74(19) . 3
F1 U2 F8 80.2(2) 3 .
F1 U2 F8 80.2(2) . .
F1 U2 F9 71.3(2) . 2_565
F1 U2 F9 71.3(2) 3 2_565
F2 U2 U1 144.54(18) 2_565 .
F2 U2 U1 97.49(17) 4_565 .
F2 U2 U1 97.49(17) 2_565 3
F2 U2 U1 144.54(18) 4_565 3
F2 U2 Rb1 114.36(16) 4_565 1_455
F2 U2 Rb1 38.50(17) 2_565 1_455
F2 U2 F1 141.6(2) 4_565 3
F2 U2 F1 87.3(2) 2_565 3
F2 U2 F1 141.6(2) 2_565 .
F2 U2 F1 87.3(2) 4_565 .
F2 U2 F2 87.2(3) 4_565 2_565
F2 U2 F3 69.1(2) 4_565 .
F2 U2 F3 69.1(2) 2_565 3
F2 U2 F3 143.2(2) 2_565 .
F2 U2 F3 143.2(2) 4_565 3
F2 U2 F8 130.11(19) 4_565 .
F2 U2 F8 130.11(19) 2_565 .
F2 U2 F9 71.0(2) 4_565 2_565
F2 U2 F9 71.0(2) 2_565 2_565
F3 U2 U1 29.13(13) . .
F3 U2 U1 29.13(13) 3 3
F3 U2 U1 87.68(14) . 3
F3 U2 U1 87.68(14) 3 .
F3 U2 Rb1 32.72(13) 3 1_455
F3 U2 Rb1 127.88(16) . 1_455
F3 U2 F3 114.2(3) 3 .
F8 U2 U1 32.64(7) . 3
F8 U2 U1 32.64(7) . .
F8 U2 Rb1 91.80(10) . 1_455
F8 U2 F3 61.46(15) . 3
F8 U2 F3 61.46(15) . .
F9 U2 U1 143.65(12) 2_565 3
F9 U2 U1 67.19(18) . .
F9 U2 U1 143.65(12) 2_565 .
F9 U2 U1 67.19(18) . 3
F9 U2 Rb1 105.52(10) 2_565 1_455
F9 U2 Rb1 61.34(4) . 1_455
F9 U2 F1 136.44(18) . .
F9 U2 F1 136.44(19) . 3
F9 U2 F2 79.4(2) . 2_565
F9 U2 F2 79.4(2) . 4_565
F9 U2 F3 122.57(15) 2_565 3
F9 U2 F3 69.21(18) . 3
F9 U2 F3 122.57(15) 2_565 .
F9 U2 F3 69.20(18) . .
F9 U2 F8 77.6(3) . .
F9 U2 F8 144.0(3) 2_565 .
F9 U2 F9 138.45(5) . 2_565
F1 Rb1 U1 73.86(10) 2_664 2_665
F1 Rb1 U1 117.44(10) 4_564 2_665
F1 Rb1 F1 104.1(2) 2_664 4_564
F2 Rb1 U1 33.87(10) 2_665 2_665
F2 Rb1 U1 83.61(12) 4_565 2_665
F2 Rb1 F1 151.21(14) 2_665 4_564
F2 Rb1 F1 151.21(14) 4_565 2_664
F2 Rb1 F1 70.49(16) 2_665 2_664
F2 Rb1 F1 70.49(16) 4_565 4_564
F2 Rb1 F2 100.3(3) 2_665 4_565
F3 Rb1 U1 124.55(15) . 2_665
F3 Rb1 U1 86.33(13) 3_655 2_665
F3 Rb1 F1 81.53(15) 3_655 2_664
F3 Rb1 F1 156.23(16) . 2_664
F3 Rb1 F1 81.53(15) . 4_564
F3 Rb1 F1 156.23(16) 3_655 4_564
F3 Rb1 F2 115.19(18) 3_655 4_565
F3 Rb1 F2 52.53(16) . 4_565
F3 Rb1 F2 115.19(18) . 2_665
F3 Rb1 F2 52.53(16) 3_655 2_665
F3 Rb1 F3 84.7(2) . 3_655
F3 Rb1 F4 152.88(18) . 3_665
F3 Rb1 F4 101.70(15) 3_655 3_665
F3 Rb1 F4 152.88(18) 3_655 1_565
F3 Rb1 F4 101.70(15) . 1_565
F3 Rb1 F6 94.39(19) 3_655 2_665
F3 Rb1 F6 94.39(19) . 2_665
F4 Rb1 U1 68.22(11) 1_565 2_665
F4 Rb1 U1 31.91(10) 3_665 2_665
F4 Rb1 F1 50.07(14) 3_665 2_664
F4 Rb1 F1 99.36(15) 3_665 4_564
F4 Rb1 F1 99.36(15) 1_565 2_664
F4 Rb1 F1 50.07(14) 1_565 4_564
F4 Rb1 F2 101.91(15) 3_665 4_565
F4 Rb1 F2 54.79(14) 1_565 4_565
F4 Rb1 F2 101.91(15) 1_565 2_665
F4 Rb1 F2 54.79(14) 3_665 2_665
F4 Rb1 F4 61.3(2) 3_665 1_565
F5 Rb1 U1 83.75(17) 1_565 2_665
F5 Rb1 F1 53.93(11) 1_565 2_664
F5 Rb1 F1 53.93(11) 1_565 4_564
F5 Rb1 F2 106.74(15) 1_565 2_665
F5 Rb1 F2 106.74(15) 1_565 4_565
F5 Rb1 F3 135.39(14) 1_565 .
F5 Rb1 F3 135.39(14) 1_565 3_655
F5 Rb1 F4 53.54(18) 1_565 3_665
F5 Rb1 F4 53.54(18) 1_565 1_565
F5 Rb1 F6 121.0(3) 1_565 .
F5 Rb1 F6 99.6(3) 1_565 2_665
F6 Rb1 U1 32.20(8) 2_665 2_665
F6 Rb1 U1 143.86(11) . 2_665
F6 Rb1 F1 105.87(14) 2_665 4_564
F6 Rb1 F1 98.70(14) . 4_564
F6 Rb1 F1 98.70(14) . 2_664
F6 Rb1 F1 105.87(14) 2_665 2_664
F6 Rb1 F2 52.20(13) 2_665 4_565
F6 Rb1 F2 110.03(14) . 4_565
F6 Rb1 F2 52.20(13) 2_665 2_665
F6 Rb1 F2 110.03(14) . 2_665
F6 Rb1 F3 57.53(16) . .
F6 Rb1 F3 57.53(16) . 3_655
F6 Rb1 F4 147.05(12) . 1_565
F6 Rb1 F4 59.09(17) 2_665 3_665
F6 Rb1 F4 59.09(17) 2_665 1_565
F6 Rb1 F4 147.05(12) . 3_665
F6 Rb1 F6 139.4(2) . 2_665
U1 F1 Rb1 98.6(2) 4 2_665
U2 F1 U1 145.4(3) . 4
U2 F1 Rb1 114.3(2) . 2_665
U1 F2 Rb1 98.1(2) . 2_664
U2 F2 U1 145.3(3) 2_564 .
U2 F2 Rb1 115.0(2) 2_564 2_664
U1 F3 U2 119.1(2) . .
U1 F3 Rb1 114.3(2) . .
U2 F3 Rb1 119.7(2) . .
U1 F4 U1 153.2(3) 4 .
U1 F4 Rb1 102.0(2) 4 1_545
U1 F4 Rb1 103.67(19) . 1_545
U1 F5 U1 116.9(4) . 3_655
U1 F5 Rb1 116.1(2) . 1_545
U1 F5 Rb1 116.1(2) 3_655 1_545
U1 F6 U1 114.5(3) . 3_655
U1 F6 Rb1 112.1(2) 3_655 .
U1 F6 Rb1 112.1(2) . .
U1 F6 Rb1 106.9(2) 3_655 2_664
U1 F6 Rb1 106.9(2) . 2_664
Rb1 F6 Rb1 103.4(3) . 2_664
U1 F7 U1 123.8(4) 3 .
U1 F8 U1 112.8(3) 3 .
U2 F8 U1 115.1(2) . 3
U2 F8 U1 115.1(2) . .
U2 F9 U2 167.3(4) . 2_564
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
U1 F1 2.298(6) 4_554
U1 F2 2.375(5) .
U1 F3 2.268(6) .
U1 F4 2.347(6) .
U1 F4 2.280(6) 4_554
U1 F5 2.319(5) .
U1 F6 2.350(4) .
U1 F7 2.291(5) .
U1 F8 2.427(4) .
U2 F1 2.285(6) .
U2 F1 2.285(6) 3
U2 F2 2.271(6) 2_565
U2 F2 2.271(6) 4_565
U2 F3 2.457(6) 3
U2 F3 2.457(6) .
U2 F8 2.400(8) .
U2 F9 2.307(9) 2_565
U2 F9 2.247(9) .
Rb1 F1 3.322(6) 4_564
Rb1 F1 3.322(6) 2_664
Rb1 F2 3.168(7) 4_565
Rb1 F2 3.168(7) 2_665
Rb1 F3 2.871(5) 3_655
Rb1 F3 2.871(5) .
Rb1 F4 3.106(6) 3_665
Rb1 F4 3.106(6) 1_565
Rb1 F5 2.755(9) 1_565
Rb1 F6 2.887(9) 2_665
Rb1 F6 2.858(9) .
F1 U1 2.298(6) 4
F1 Rb1 3.322(6) 2_665
F2 U2 2.271(6) 2_564
F2 Rb1 3.168(7) 2_664
F4 U1 2.280(6) 4
F4 Rb1 3.106(6) 1_545
F5 U1 2.319(5) 3_655
F5 Rb1 2.755(9) 1_545
F6 U1 2.350(4) 3_655
F6 Rb1 2.887(9) 2_664
F7 U1 2.291(5) 3
F8 U1 2.427(4) 3
F9 U2 2.307(9) 2_564
