Application of a mild hydrothermal method to the synthesis of mixed transition-metal(ii)/uranium(iv) fluorides
Felder, Justin; Yeon, Jeongho; Smith, Mark; zur Loye, Hans-Conrad; Inorganic Chemistry Frontiers 4 (2017) 368–; doi:10.1039/C6QI00491A

data_4349611
_publ_section_title
;
 Application of a mild hydrothermal method to the synthesis of mixed
 transition-metal(ii)/uranium(iv) fluorides
;
_journal_issue                   2
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              368
_journal_paper_doi               10.1039/C6QI00491A
_journal_volume                  4
_journal_year                    2017
_chemical_formula_moiety         '2(F5 U), H12 Ni O6, 2(H2 O)'
_chemical_formula_sum            'F10 H16 Ni O8 U2'
_chemical_formula_weight         868.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-11-07 deposited with the CCDC.
2016-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.532(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.9605(7)
_cell_length_b                   7.0441(4)
_cell_length_c                   8.8514(6)
_cell_measurement_reflns_used    9001
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.014
_cell_measurement_theta_min      3.441
_cell_volume                     681.25(7)
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_molecular_graphics    various
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_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         37.782
_diffrn_reflns_theta_min         3.441
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    25.234
_exptl_absorpt_correction_T_max  0.1158
_exptl_absorpt_correction_T_min  0.0376
_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    4.236
_exptl_crystal_description       plate
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_exptl_crystal_size_mid          0.060
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_refine_diff_density_min         -1.005
_refine_diff_density_rms         0.183
_refine_ls_extinction_coef       0.00492(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         3655
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0175
_refine_ls_R_factor_gt           0.0150
_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^)+(0.0042P)^2^+0.7012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0272
_refine_ls_wR_factor_ref         0.0276
_reflns_number_gt                3456
_reflns_number_total             3655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6qi00491a2.cif
_cod_data_source_block           jbf1186d
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349611
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.237
_shelx_estimated_absorpt_t_max   0.432
_shelx_res_checksum              71968
_shelx_hkl_checksum              52385