Nitrate and Perchlorate Complexes of Uranium(IV)
Margaret-Jane Crawford; Arkady Ellern; Konstantin Karaghiosoff; Peter Mayer; Inorganic Chemistry 48 (2009) 10877–10879; doi:10.1021/ic901386y

data_4303682
_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        'M.-J. Crawford'
_publ_contact_author_phone       +49-89-2180-77491
_publ_section_title
;
Nitrate and Perchlorate Complexes of Uranium(IV)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10877
_journal_page_last               10879
_journal_paper_doi               10.1021/ic901386y
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'U 6(N O3), 2(N C12 H28)'
_chemical_formula_sum            'C24 H56 N8 O18 U'
_chemical_formula_weight         982.773
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_author_name               'P. Mayer'
_audit_block_code                U_NO3_nPr4N_dx074_klapoetke
_audit_creation_date
;
'Tue Sep 09 15:31:57 2008'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             10-Sep-08
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6269(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.6953(2)
_cell_length_b                   15.8043(2)
_cell_length_c                   16.8333(3)
_cell_measurement_reflns_used    9165
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.2494
_cell_measurement_theta_min      3.7804
_cell_volume                     3909.28(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
;
_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 15.9809
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   -1.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       32.0000   79.0000    0.0000    0.0000    0.0000 104

  2 omega   -1.00  103.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       32.0000   79.0000  120.0000    0.0000    0.0000 104

  3 omega  -65.00   39.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -32.0000   80.0000  250.0000    0.0000    0.0000 104

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       omega-scans
_diffrn_orient_matrix_UB_11      -0.0233751354
_diffrn_orient_matrix_UB_12      0.0391318250
_diffrn_orient_matrix_UB_13      -0.0031954166
_diffrn_orient_matrix_UB_21      -0.0326329195
_diffrn_orient_matrix_UB_22      -0.0190067736
_diffrn_orient_matrix_UB_23      -0.0256998042
_diffrn_orient_matrix_UB_31      -0.0268621840
_diffrn_orient_matrix_UB_32      -0.0109601102
_diffrn_orient_matrix_UB_33      0.0332477470
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0486
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20116
_diffrn_reflns_theta_full        26.34
_diffrn_reflns_theta_max         26.34
_diffrn_reflns_theta_min         3.79
_diffrn_source_current           45_mA
_diffrn_source_power             2.48_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    4.231
_exptl_absorpt_correction_T_max  0.5706
_exptl_absorpt_correction_T_min  0.4357
_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    1.66983(4)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.358
_refine_diff_density_min         -2.159
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     468
_refine_ls_number_reflns         7882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.0554
_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^)+(0.0278P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0661
_reflns_number_gt                5554
_reflns_number_total             7882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901386y_si_001_2.cif
_cod_data_source_block           dx074
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4303682