Structurally Characterized Ternary U-O-N Compound, UN4O12: UO2(NO3)2.N2O4 or NO+UO2(NO3)3-?
Margaret-Jane Crawford; Peter Mayer; Inorganic Chemistry 44 (2005) 8481–8485; doi:10.1021/ic050409v

data_4309927
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus D)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       mjc@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77492
_publ_contact_author_name        'Margret-Jane Crawford'
_publ_contact_author_phone       +49-89-2180-77503
_publ_section_title
;
Structurally Characterized Ternary U-O-N Compound, UN4O12:
UO2(NO3)2.N2O4 or NO+UO2(NO3)3-?
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8481
_journal_page_last               8485
_journal_paper_doi               10.1021/ic050409v
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'U O2, 3(N O3), N O'
_chemical_formula_sum            'N4 O12 U'
_chemical_formula_weight         486.049
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'Mayer, P.'
_audit_block_code                UO2_NO_NO3_in191_klapoetke
_audit_creation_date             27-Apr-04
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             02-Mar-05
_cell_angle_alpha                90.00
_cell_angle_beta                 115.452(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.3992(4)
_cell_length_b                   9.9781(4)
_cell_length_c                   7.6455(2)
_cell_measurement_reflns_used    7909
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      3.134
_cell_volume                     922.98(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_orient_matrix_type       'by Nonius Collect from scalepack cell'
_diffrn_orient_matrix_UB_11      -0.0251828
_diffrn_orient_matrix_UB_12      -0.0031015
_diffrn_orient_matrix_UB_13      -0.1434783
_diffrn_orient_matrix_UB_21      -0.0787184
_diffrn_orient_matrix_UB_22      -0.0001352
_diffrn_orient_matrix_UB_23      -0.0194132
_diffrn_orient_matrix_UB_31      -0.0008859
_diffrn_orient_matrix_UB_32      0.1001714
_diffrn_orient_matrix_UB_33      -0.0044686
_diffrn_radiation_collimation    0.35
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7898
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.37
_diffrn_source_current           90.00
_diffrn_source_power             4.050
_diffrn_source_type              'FR 591 generator'
_diffrn_source_voltage           45.00
_exptl_absorpt_coefficient_mu    17.668
_exptl_absorpt_correction_T_max  0.5661
_exptl_absorpt_correction_T_min  0.3057
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
Crystal faces optimized with XShape, rev. 1.02, STOE (Darmstadt, Germany)
Absorption correction with XRed, rev 1.09, STOE (Darmstadt, Germany)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.49786(19)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.933
_refine_diff_density_min         -2.822
_refine_diff_density_rms         0.207
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1049
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0228
_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^)+(0.0283P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0515
_reflns_number_gt                1006
_reflns_number_total             1049
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050409vsi20050703_034251.cif
_cod_data_source_block           in191
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4309927