Expanding the Crystal Chemistry of Uranyl Peroxides: Synthesis and Structures of Di- and Triperoxodioxouranium(VI) Complexes
Karrie-Ann Kubatko; Tori Z. Forbes; Amanda L. Klingensmith; Peter C. Burns; Inorganic Chemistry 46 (2007) 3657–3662; doi:10.1021/ic070118h

data_4308128
_publ_section_title
;
Expanding the Crystal Chemistry of Uranyl Peroxides: Synthesis and
Structures of Di- and Triperoxodioxouranium(VI) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3657
_journal_page_last               3662
_journal_paper_doi               10.1021/ic070118h
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'H24 Na4 O20 U'
_chemical_formula_sum            'H24 Na4 O20 U'
_chemical_formula_weight         647.17
_chemical_name_common            'sodium uranyl triperoxo hydrate'
_chemical_name_systematic
; 
sodium uranyl triperoxo hydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.917(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.7883(6)
_cell_length_b                   16.0005(15)
_cell_length_c                   16.5624(16)
_cell_measurement_reflns_used    13509
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.05
_cell_measurement_theta_min      2.06
_cell_volume                     1797.9(3)
_computing_cell_refinement       'SAINT+ NT (Bruker, 2000)'
_computing_data_collection       'SMART NT (Bruker, 2001)'
_computing_data_reduction        'SAINT+ NT (Bruker, 2000)'
_computing_molecular_graphics    'ATOMS (Dowty, 2000)'
_computing_publication_material
;
SHELXTL NT (Bruker, 1998) and WINGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32522
_diffrn_reflns_theta_full        32.88
_diffrn_reflns_theta_max         32.88
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    9.217
_exptl_absorpt_correction_T_max  0.1617
_exptl_absorpt_correction_T_min  0.0670
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via \y-scan (SHELXTL NT; Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.491
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       euhedral
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          .05
_exptl_crystal_size_min          .01
_refine_diff_density_max         2.023
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.213
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         6690
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0281
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0282P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                5570
_reflns_number_total             6690
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070118hsi20070123_024423.cif
_cod_data_source_block           final
_cod_database_code               4308128