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_4308127
_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         'H16 O21 K6 U2'
_chemical_formula_sum            'H16 K6 O21 U2'
_chemical_formula_weight         1062.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           54
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2a 2ac'
_symmetry_space_group_name_H-M   'P c c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.078(8)
_cell_length_b                   6.669(4)
_cell_length_c                   23.526(13)
_cell_measurement_temperature    293(2)
_cell_volume                     2366(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.1867
_diffrn_reflns_av_sigmaI/netI    0.1410
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            30033
_diffrn_reflns_theta_full        34.19
_diffrn_reflns_theta_max         34.19
_diffrn_reflns_theta_min         2.20
_exptl_absorpt_coefficient_mu    14.811
_exptl_absorpt_correction_T_max  0.31
_exptl_absorpt_correction_T_min  0.11
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'via \y-scan (SHELXTL-NT; Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         8.486
_refine_diff_density_min         -3.862
_refine_diff_density_rms         0.506
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.852
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         4841
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.852
_refine_ls_R_factor_all          0.1975
_refine_ls_R_factor_gt           0.0589
_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^)+(0.0697P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1733
_reflns_number_gt                1484
_reflns_number_total             4841
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070118hsi20070123_024411.cif
_cod_data_source_block           final
_cod_original_formula_sum        'H16 O21 K6 U2'
_cod_database_code               4308127