Redetermination of di-μ-hydroxido-bis[diaquachloridodioxidouranium(VI)] from single-crystal synchrotron data
Huys, Diederik; Van Deun, Rik; Pattison, Phil; Van Meervelt, Luc; Van Hecke, Kristof; Acta Crystallographica Section E 66 (2010) i11–; doi:10.1107/S1600536810002394

data_2224865
_publ_section_title
;
 Redetermination of
 di-\m-hydroxido-bis[diaquachloridodioxidouranium(VI)] from
 single-crystal synchrotron data
;
_journal_coeditor_code           BT5153
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i11
_journal_paper_doi               10.1107/S1600536810002394
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '[U2 Cl2 O4 (O H)2 (H2 O)4]'
_chemical_formula_moiety         'H10 Cl2 O10 U2'
_chemical_formula_sum            'Cl2 H10 O10 U2'
_chemical_formula_weight         717.04
_chemical_name_systematic
;
Di-\m-hydroxido-bis[diaquachloridodioxidouranium(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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.47(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.712(2)
_cell_length_b                   6.1212(12)
_cell_length_c                   17.662(4)
_cell_measurement_reflns_used    4751
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.2
_cell_measurement_theta_min      2.3
_cell_volume                     1152.8(4)
_computing_cell_refinement       'CrysAlis Pro (Oxford Diffraction, 2006)'
_computing_data_collection       '<i>MAR345 Program Manual</i> (Mar, 2000)'
_computing_data_reduction        'CrysAlis Pro (Oxford Diffraction, 2006)'
_computing_molecular_graphics    'PLUTON (Spek, 2009)'
_computing_publication_material  'PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'ESRF, SNBL, BM01A'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  'double crystal'
_diffrn_radiation_source         'bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.77000
_diffrn_reflns_av_R_equivalents  0.067
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13020
_diffrn_reflns_theta_full        26.44
_diffrn_reflns_theta_max         26.44
_diffrn_reflns_theta_min         2.32
_exptl_absorpt_coefficient_mu    63.627
_exptl_absorpt_correction_T_max  0.0564
_exptl_absorpt_correction_T_min  0.0075
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'(SCALE3 in ABSPACK; Oxford Diffraction, 2006)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.370
_refine_diff_density_min         -1.671
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         1846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0885P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1238
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                1620
_reflns_number_total             1846
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5153.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'H10 Cl2 O10 U2'
_cod_database_code               2224865
_cod_database_fobs_code          2224865