Synthesis and crystal structure of triethylammonium hexabromidouranate(IV) dichloromethane monosolvate
Deubner, Holger Lars; Koester, Marcel; von Haenisch, Carsten; Kraus, Florian; Acta Crystallographica Section E 76 (2020) 1587–1590; doi:10.1107/S205698902001169X

data_2243578
_publ_section_title
;
 Synthesis and crystal structure of triethylammonium
 hexabromidouranate(IV) dichloromethane monosolvate
;
_journal_coeditor_code           ZL2792
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1587
_journal_page_last               1590
_journal_paper_doi               10.1107/S205698902001169X
_journal_volume                  76
_journal_year                    2020
_chemical_formula_iupac          '(C6 H16 N)2 [U Br6], C H2 Cl2'
_chemical_formula_moiety         '2(C6 H16 N +), Br6 U 2-, C H2 Cl2'
_chemical_formula_sum            'C13 H34 Br6 Cl2 N2 U'
_chemical_formula_weight         1006.81
_chemical_name_systematic
;
Triethylammonium hexabromidouranate(IV) dichloromethane monosolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.0550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7318(4)
_cell_length_b                   17.4541(4)
_cell_length_c                   15.0082(4)
_cell_measurement_reflns_used    72381
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      53.6
_cell_measurement_theta_min      5.1
_cell_volume                     2809.44(14)
_computing_cell_refinement
;
X-Area (Stoe & Cie, 2018)
;
_computing_data_collection
;
X-Area (Stoe & Cie, 2018)
;
_computing_data_reduction
;
X-Area (Stoe & Cie, 2018)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2019)
;
_computing_structure_refinement
;
<i>SHELXL2018/3</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2018/3</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            35494
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.791
_diffrn_reflns_theta_min         2.574
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    14.503
_exptl_absorpt_correction_T_max  0.5269
_exptl_absorpt_correction_T_min  0.0492
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
(X-Red32; Stoe & Cie, 2009)
;
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    2.380
_exptl_crystal_description       plate
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.518
_refine_diff_density_min         -1.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         5945
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0302
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0252P)^2^+6.7371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0594
_reflns_number_gt                5307
_reflns_number_total             5945
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2792sup1.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2243578
_shelx_hkl_checksum              25661
_shelx_res_checksum              9312