Tetra-<i>n</i>-butylammonium di-μ-hydroxo-bis[dinitratodioxouranate(VI)]
Andreas Fischer; Giuseppe Palladino; Acta Crystallographica Section E 61 (2005) m1542–m1544; doi:10.1107/S1600536805021045

data_2206453
_publ_section_title
;
 Tetra-<i>n</i>-butylammonium
 di-\m-hydroxo-bis[dinitratodioxouranate(VI)]
;
_journal_coeditor_code           HK6022
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1542
_journal_page_last               m1544
_journal_paper_doi               10.1107/S1600536805021045
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C16 H36 N)2 [U2 (N O3)4 (O H)2 O4]'
_chemical_formula_moiety         '2C16 H36 N + , H2 N4 O18 U2 2-'
_chemical_formula_sum            'C32 H74 N6 O18 U2'
_chemical_formula_weight         1307.02
_chemical_name_systematic
;
Tetra-n-butylammonium di-\m-hydroxo-bis[dinitratodioxouranium(VI)]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 94.239(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8335(13)
_cell_length_b                   13.217(2)
_cell_length_c                   14.148(3)
_cell_measurement_reflns_used    58
_cell_measurement_temperature    299
_cell_measurement_theta_max      18.4
_cell_measurement_theta_min      4.6
_cell_volume                     2393.2(7)
_computing_cell_refinement       'DIRAX/LSQ (Duisenberg, 1992)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EVALCCD (Duisenberg <i>et al.</i>, 2003)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001)'
_computing_publication_material  'MAXUS (Mackay <i>et al.</i>, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Bruker Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_av_sigmaI/netI    0.043
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25561
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         4.5
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.82
_exptl_absorpt_correction_T_max  0.498
_exptl_absorpt_correction_T_min  0.390
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(HABITUS; Herrendorf & B\"arnighausen, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.062
_refine_diff_density_min         -0.812
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.27
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         5427
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.27
_refine_ls_R_factor_all          0.094
_refine_ls_R_factor_gt           0.052
_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^)+(0.005P)^2^+11.1326P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.084
_refine_ls_wR_factor_ref         0.101
_reflns_number_gt                3712
_reflns_number_total             5427
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hk6022.cif
_cod_data_source_block           I
_cod_original_cell_volume        2393.1(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206453
_cod_database_fobs_code          2206453