Expanding the Crystal Chemistry of Actinyl Peroxides: μ-η2:η1 Peroxide Coordination in Trimers of U6+ Polyhedra
Daniel K. Unruh; Alicia Burtner; Peter C. Burns; Inorganic Chemistry 48 (2009) 2346–2348; doi:10.1021/ic8024217

data_4301748
_publ_section_title
;
Expanding the Crystal Chemistry of Actinyl Peroxides: \m-\h2:\h1 Peroxide
Coordination in Trimers of U6+ Polyhedra
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2346
_journal_page_last               2348
_journal_paper_doi               10.1021/ic8024217
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'O22 U3, 4(H12 Mg O6), 2(H2 O), 2(K)'
_chemical_formula_sum            'H52 K2 Mg4 O48 U3'
_chemical_formula_weight         1709.95
_chemical_name_systematic        'Potassium Magnesium Uranyl Peroxide Trimer'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.064(5)
_cell_angle_beta                 93.359(4)
_cell_angle_gamma                94.770(3)
_cell_formula_units_Z            1
_cell_length_a                   6.5554(18)
_cell_length_b                   8.2865(18)
_cell_length_c                   18.146(5)
_cell_measurement_temperature    100(2)
_cell_volume                     976.3(4)
_computing_cell_refinement       'SMART-NT v5.0'
_computing_data_collection       'SMART-NT v5.0'
_computing_data_reduction        'SMART-NT v5.0'
_computing_molecular_graphics    'CrystalMaker v 1.3.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      382(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker PLATFORM with a SMART CCD detector'
_diffrn_measurement_method       \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  0.0504
_diffrn_reflns_av_sigmaI/netI    0.0655
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            17278
_diffrn_reflns_theta_full        31.37
_diffrn_reflns_theta_max         31.37
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    12.829
_exptl_absorpt_correction_T_max  0.3602
_exptl_absorpt_correction_T_min  0.3327
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.908
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             798
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.870
_refine_diff_density_min         -1.927
_refine_diff_density_rms         0.281
_refine_ls_extinction_coef       SHELXL
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     335
_refine_ls_number_reflns         6385
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0350
_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^)+(0.0239P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0722
_reflns_number_gt                5171
_reflns_number_total             6385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8024217_si_002.cif
_cod_data_source_block           pcb
_cod_database_code               4301748