Mild Hydrothermal Crystal Growth, Structure, and Magnetic Properties of Ternary U(IV) Containing Fluorides: LiUF5, KU2F9, K7U6F31, RbUF5, RbU2F9, and RbU3F13.
Yeon, Jeongho; Smith, Mark D.; Tapp, Joshua; Möller, Angela; Zur Loye, Hans-Conrad; Inorganic chemistry 53 (2014) 6289–6298; doi:10.1021/ic5008507

data_4338513
_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_formula_moiety         'F31 K7 U6'
_chemical_formula_sum            'F31 K7 U6'
_chemical_formula_weight         2290.88
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-01-24
_audit_creation_method
;
  Olex2 1.2
  (compiled Dec  5 2012 16:17:34, GUI svn.r4385)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   15.1426(8)
_cell_length_b                   15.1426(8)
_cell_length_c                   10.3856(10)
_cell_measurement_reflns_used    3229
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      30.10
_cell_measurement_theta_min      2.50
_cell_volume                     2062.4(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_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      295(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0556
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            16928
_diffrn_reflns_theta_full        33.13
_diffrn_reflns_theta_max         33.13
_diffrn_reflns_theta_min         2.50
_diffrn_source                   'fine-focus 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    36.475
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.441793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1699 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.4418.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    5.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2892
_exptl_crystal_preparation       'Fragment cleaved from aggregation'
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.633
_refine_diff_density_min         -1.717
_refine_diff_density_rms         0.485
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_matrix_type           full
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1756
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0395
_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/[\s^2^(Fo^2^)+(0.0609P)^2^+12.5659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1008
_refine_ls_wR_factor_ref         0.1055
_reflns_number_gt                1516
_reflns_number_total             1756
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5008507_si_002.cif
_cod_data_source_block           K7U6F31
_cod_depositor_comments
'Adding full bibliography for 4338511--4338516.cif.'
_cod_database_code               4338513