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_4121449
_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 Na4 U6 Zn'
_chemical_formula_sum            'F30 Na4 U6 Zn'
_chemical_formula_weight         2155.51
_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'
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   9.8783(7)
_cell_length_b                   9.8783(7)
_cell_length_c                   13.0455(18)
_cell_measurement_reflns_used    2254
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.742
_cell_measurement_theta_min      3.123
_cell_volume                     1102.44(19)
_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    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_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  0.0815
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            22793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.986
_diffrn_reflns_theta_min         2.381
_exptl_absorpt_coefficient_mu    45.294
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    6.493
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1792
_exptl_crystal_size_max          0.040
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         5.633
_refine_diff_density_min         -3.399
_refine_diff_density_rms         0.507
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         1625
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0361
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+11.5343P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0719
_refine_ls_wR_factor_ref         0.0757
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1382
_reflns_number_total             1625
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja412725r_si_002.cif
_cod_data_source_block           Na4ZnU6F30
_cod_original_cell_volume        1102.4(2)
_cod_database_code               4121449
_shelx_estimated_absorpt_t_min   0.265
_shelx_estimated_absorpt_t_max   0.464