Application of a Mild Hydrothermal Approach Containing an in Situ Reduction Step to the Growth of Single Crystals of the Quaternary U(IV)-Containing Fluorides Na4MU6F30 (M = Mn(2+), Co(2+), Ni(2+), Cu(2+), and Zn(2+)) Crystal Growth, Structures, and Magnetic Properties.
Yeon, Jeongho; Smith, Mark D.; Tapp, Joshua; Möller, Angela; Zur Loye, Hans-Conrad; Journal of the American Chemical Society 136 (2014) 3955–3963; doi:10.1021/ja412725r

data_4121445
_publ_section_title
;
 Application of a Mild Hydrothermal Approach Containing an in Situ
 Reduction Step to the Growth of Single Crystals of the Quaternary
 U(IV)-Containing Fluorides Na4MU6F30 (M = Mn(2+), Co(2+), Ni(2+), Cu(2+),
 and Zn(2+)) Crystal Growth, Structures, and Magnetic Properties.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3955
_journal_page_last               3963
_journal_paper_doi               10.1021/ja412725r
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         'F30 Mn Na4 U6'
_chemical_formula_sum            'F30 Mn Na4 U6'
_chemical_formula_weight         2145.08
_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     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-05
_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            2
_cell_length_a                   9.9172(8)
_cell_length_b                   9.9172(8)
_cell_length_c                   13.033(2)
_cell_measurement_reflns_used    3737
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.01
_cell_measurement_theta_min      2.37
_cell_volume                     1110.1(2)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100(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  0.0687
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_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            26070
_diffrn_reflns_theta_full        34.32
_diffrn_reflns_theta_max         34.32
_diffrn_reflns_theta_min         2.37
_diffrn_source                   'fine-focus 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    44.471
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.387124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.1204 before and 0.0540 after correction.
The Ratio of minimum to maximum transmission is 0.3871.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    6.418
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal drum'
_exptl_crystal_F_000             1782
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         5.265
_refine_diff_density_min         -3.802
_refine_diff_density_rms         0.705
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.187
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1563
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.187
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0650P)^2^+3.8910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1119
_reflns_number_gt                1388
_reflns_number_total             1563
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja412725r_si_002.cif
_cod_data_source_block           Na4MnU6F30
_cod_database_code               4121445