Trivalent Cation-Controlled Phase Space of New U(IV) Fluorides, Na3MU6F30 (M = Al(3+), Ga(3+), Ti(3+), V(3+), Cr(3+), Fe(3+)): Mild Hydrothermal Synthesis Including an in Situ Reduction Step, Structures, Optical, and Magnetic Properties.
Yeon, Jeongho; Smith, Mark D.; Morrison, Gregory; Zur Loye, Hans-Conrad; Inorganic chemistry 54 (2015) 2058–2066; doi:10.1021/ic503034t

data_4342344
_publ_section_title
;
 Trivalent Cation-Controlled Phase Space of New U(IV) Fluorides, Na3MU6F30
 (M = Al(3+), Ga(3+), Ti(3+), V(3+), Cr(3+), Fe(3+)): Mild Hydrothermal
 Synthesis Including an in Situ Reduction Step, Structures, Optical, and
 Magnetic Properties.
;
_journal_issue                   4
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2058
_journal_page_last               2066
_journal_paper_doi               10.1021/ic503034t
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'F30 Fe Na3 U6'
_chemical_formula_sum            'F30 Fe Na3 U6'
_chemical_formula_weight         2123.00
_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                   9.8351(3)
_cell_length_b                   9.8351(3)
_cell_length_c                   12.9869(10)
_cell_measurement_reflns_used    3962
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.882
_cell_measurement_theta_min      2.391
_cell_volume                     1087.91(10)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.631 (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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0697
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24085
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.461
_diffrn_reflns_theta_min         2.391
_exptl_absorpt_coefficient_mu    45.442
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.3205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    6.481
_exptl_crystal_description       'trigonal dipyramid'
_exptl_crystal_F_000             1762
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         4.218
_refine_diff_density_min         -2.621
_refine_diff_density_rms         0.504
_refine_ls_extinction_coef       0.00044(7)
_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   1.131
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     63
_refine_ls_number_reflns         1787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0339
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+6.4376P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0708
_refine_ls_wR_factor_ref         0.0733
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1581
_reflns_number_total             1787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic503034t_si_002.cif
_cod_data_source_block           Na3FeU6F30
_cod_depositor_comments
'Adding full bibliography for 4342339--4342344.cif.'
_cod_original_cell_volume        1087.91(11)
_cod_database_code               4342344
_shelx_estimated_absorpt_t_min   0.092
_shelx_estimated_absorpt_t_max   0.171