Synthesis, Structure, and Bonding of Stable Complexes of Pentavalent Uranyl
Grégory Nocton; Pawel Horeglad; Valentina Vetere; Jacques Pécaut; Lionel Dubois; Pascale Maldivi; Norman M. Edelstein; Marinella Mazzanti; Journal of the American Chemical Society 132 (2010) 495–508; doi:10.1021/ja9037164

data_4101774
_publ_contact_author
;
      Dr Marinella Mazzanti
      LCIB (UMR-E 3 CEA-UJF)
      DRFMC, CEA Grenoble
      17, rue des Martyrs
      38054 Grenoble cedex 9
;
_publ_section_title
;
 Synthesis, Structure, and Bonding of Stable Complexes of Pentavalent
 Uranyl
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              495
_journal_page_last               508
_journal_paper_doi               10.1021/ja9037164
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C65 H99 K N3 O10 U'
_chemical_formula_weight         1359.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.0642(19)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.4372(6)
_cell_length_b                   20.4126(4)
_cell_length_c                   20.8384(3)
_cell_measurement_reflns_used    13937
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0167
_cell_measurement_theta_min      2.9967
_cell_volume                     13297.5(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
  1 omega   -2.00   39.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       17.1550 -126.0000  220.0000    0.0000    0.0000 82

  2 omega   -8.00   41.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       17.1550  -45.0000   30.0000    0.0000    0.0000 98

  3 omega  -42.00    7.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175   45.0000   60.0000    0.0000    0.0000 98

  4 omega  -22.00   24.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175 -104.0000  138.0000    0.0000    0.0000 92

  5 omega  -42.00    6.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175   45.0000  150.0000    0.0000    0.0000 96

  6 omega    4.00   54.00   0.5000   60.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175    0.0000   90.0000    0.0000    0.0000 100

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0599
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            34513
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.559
_exptl_absorpt_correction_T_max  0.8827
_exptl_absorpt_correction_T_min  0.7839
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)
(compiled Jan 10 2008,16:37:18)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5608
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.440
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.919
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         13293
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.919
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0320
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0695
_refine_ls_wR_factor_ref         0.0727
_reflns_number_gt                8573
_reflns_number_total             13293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9037164_si_001_1.cif
_cod_data_source_block           compound4
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4101774