Tetrakis(tetramethylammonium) tricarbonatodioxidouranate octahydrate
Reed, Wendy A.; Oliver, Allen G.; Rao, Linfeng; Acta Crystallographica Section C 67 (2011) m301–m303; doi:10.1107/S0108270111032641

data_2018211
_publ_section_title
;
 Tetrakis(tetramethylammonium) tricarbonatodioxidouranate octahydrate
;
_journal_coeditor_code           BG3140
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m301
_journal_page_last               m303
_journal_paper_doi               10.1107/S0108270111032641
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(C4 H12 N4) [U O2 (C O3)3], 8H2 O'
_chemical_formula_moiety         '4(C4 H12 N +), C3 O11 U 4-, 8(H2 O)'
_chemical_formula_sum            'C19 H64 N4 O19 U'
_chemical_formula_weight         890.77
_chemical_name_systematic
;
Tetrakis(tetramethylammonium) tricarbonatodioxidouranate octahydrate
;
_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_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.343(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.5377(18)
_cell_length_b                   12.358(2)
_cell_length_c                   28.533(5)
_cell_measurement_reflns_used    7411
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.98
_cell_measurement_theta_min      4.78
_cell_volume                     3666.4(11)
_computing_cell_refinement       'APEX2 (Bruker, 2008)'
_computing_data_collection       'APEX2  (Bruker, 2008)'
_computing_data_reduction        'APEX2 or SAINT? (Bruker, 2008)'
_computing_molecular_graphics
;
XP (Sheldrick, 2008); POV-ray  (Cason, 2003); DIAMOND
(Brandenburg, 2009)
;
_computing_publication_material
;
XCIF (Sheldrick, 2008); enCIFer (Allen <i>et al.</i>, 2004);
publCIF (Westrip, 2010)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Platinum 200'
_diffrn_measurement_method       'combination of /w and /f-scans'
_diffrn_radiation_monochromator  'Channel-cut Si-<111> crystal'
_diffrn_radiation_source
'ALS at Lawrence Berkeley National Laboratory, Beamline 11.3.1'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7750
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0346
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            26534
_diffrn_reflns_theta_full        28.97
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         1.58
_exptl_absorpt_coefficient_mu    2.462
_exptl_absorpt_correction_T_max  0.8868
_exptl_absorpt_correction_T_min  0.8465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2008)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.697
_refine_diff_density_min         -0.792
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         7499
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+2.5078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                6587
_reflns_number_total             7499
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bg3140.cif
_cod_data_source_block           I
_cod_original_cell_volume        3666.5(11)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2018211
_cod_database_fobs_code          2018211