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_4303681
_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(P C24 H20), 4(C2 H3 N)'
_chemical_formula_sum            'C56 H52 N10 O18 P2 U'
_chemical_formula_weight         1453.045
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_author_name               'P. Mayer'
_audit_block_code                U_NO3_PPh4_CH3CN_dx066_klapoetke
_audit_creation_date
;
'Tue Sep 09 15:20:26 2008'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             01-Jul-09
_cell_angle_alpha                65.904(4)
_cell_angle_beta                 85.548(3)
_cell_angle_gamma                77.243(3)
_cell_formula_units_Z            1
_cell_length_a                   10.6347(4)
_cell_length_b                   11.8326(5)
_cell_length_c                   13.3839(6)
_cell_measurement_reflns_used    12305
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.2490
_cell_measurement_theta_min      3.8150
_cell_volume                     1499.32(12)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -61.00   -7.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682   75.0000    0.0000    0.0000    0.0000 54

  2 omega  -61.00   -7.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682   75.0000  240.0000    0.0000    0.0000 54

  3 phi     88.00  150.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -29.1682    0.0000     -        0.0000    0.0000 62

  4 omega   -8.00   42.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682   45.0000    0.0000    0.0000    0.0000 50

  5 omega  -50.00    3.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682  -75.0000  240.0000    0.0000    0.0000 53

  6 phi     -2.00   62.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
 -40.0000  -29.1682    0.0000     -        0.0000    0.0000 64

  7 omega -101.00  -48.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682  -75.0000  240.0000    0.0000    0.0000 53

  8 omega  -56.00   -4.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -29.1682   45.0000  120.0000    0.0000    0.0000 52

  9 omega   50.00  102.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244   45.0000  120.0000    0.0000    0.0000 52

 10 omega   22.00   50.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244   45.0000    0.0000    0.0000    0.0000 28

 11 phi   -143.00 -104.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
  40.0000   29.3244    0.0000     -        0.0000    0.0000 39

 12 omega   19.00   61.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244  -75.0000    0.0000    0.0000    0.0000 42

 13 omega    7.00   53.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244  -75.0000  120.0000    0.0000    0.0000 46

 14 omega    2.00   30.00   1.0000   12.7000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       29.3244   75.0000  120.0000    0.0000    0.0000 28

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_orient_matrix_UB_11      -0.0469472489
_diffrn_orient_matrix_UB_12      0.0256141425
_diffrn_orient_matrix_UB_13      -0.0426924569
_diffrn_orient_matrix_UB_21      -0.0496899923
_diffrn_orient_matrix_UB_22      -0.0050601732
_diffrn_orient_matrix_UB_23      0.0391346266
_diffrn_orient_matrix_UB_31      -0.0001195598
_diffrn_orient_matrix_UB_32      0.0618337214
_diffrn_orient_matrix_UB_33      -0.0045192911
_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  0.0413
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            16990
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         3.82
_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    2.840
_exptl_absorpt_correction_T_max  0.7703
_exptl_absorpt_correction_T_min  0.4664
_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    1.60931(12)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.987
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6111
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0262
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0258P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0520
_refine_ls_wR_factor_ref         0.0528
_reflns_number_gt                5941
_reflns_number_total             6111
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901386y_si_001_1.cif
_cod_data_source_block           dx066
_cod_original_cell_volume        1499.32(11)
_cod_database_code               4303681