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_4308126
_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_sum            'Ca2 H18 O17 U'
_chemical_formula_weight         608.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_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                   9.576(3)
_cell_length_b                   12.172(3)
_cell_length_c                   12.314(2)
_cell_measurement_temperature    293(2)
_cell_volume                     1435.3(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.896
_diffrn_measured_fraction_theta_max 0.896
_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  0.1456
_diffrn_reflns_av_sigmaI/netI    0.3698
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            7894
_diffrn_reflns_theta_full        34.53
_diffrn_reflns_theta_max         34.53
_diffrn_reflns_theta_min         2.71
_exptl_absorpt_coefficient_mu    12.107
_exptl_absorpt_correction_T_max  0.55
_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    2.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       acicular
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.173
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.460
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.460
_refine_ls_R_factor_all          0.1670
_refine_ls_R_factor_gt           0.0397
_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^)+(0.0314P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0959
_reflns_number_gt                836
_reflns_number_total             2738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070118hsi20070123_024356.cif
_cod_data_source_block
;
;
_cod_original_cell_volume        1435.4(6)
_cod_original_formula_sum        'H18 O17 Ca2 U'
_cod_database_code               4308126