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_4338515
_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         'F9 Rb U2'
_chemical_formula_sum            'F9 Rb U2'
_chemical_formula_weight         732.53
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-10-18
_audit_creation_method
;
  Olex2 1.2
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7330(8)
_cell_length_b                   11.6754(10)
_cell_length_c                   7.0304(6)
_cell_measurement_reflns_used    6730
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.23
_cell_measurement_theta_min      3.38
_cell_volume                     716.83(11)
_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    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0511
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            21276
_diffrn_reflns_theta_full        36.30
_diffrn_reflns_theta_max         36.30
_diffrn_reflns_theta_min         3.38
_diffrn_source                   'sealed tube'
_diffrn_source_current           38.0
_diffrn_source_power             1.786
_diffrn_source_target            Mo
_diffrn_source_voltage           47.0
_exptl_absorpt_coefficient_mu    51.986
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.331202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0997 before and 0.0473 after correction.
The Ratio of minimum to maximum transmission is 0.3312.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    6.788
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blade
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.940
_refine_diff_density_min         -3.697
_refine_diff_density_rms         0.488
_refine_ls_extinction_coef       0.00218(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.146
_refine_ls_matrix_type           full
_refine_ls_number_parameters     59
_refine_ls_number_reflns         1804
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0301
_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/[\s^2^(Fo^2^)+(0.0358P)^2^+6.7368P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0725
_refine_ls_wR_factor_ref         0.0743
_reflns_number_gt                1629
_reflns_number_total             1804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5008507_si_002.cif
_cod_data_source_block           RbU2F9
_cod_depositor_comments
'Adding full bibliography for 4338511--4338516.cif.'
_cod_database_code               4338515