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_4101776
_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            'C52 H78 K N2 O8 U'
_chemical_formula_weight         1136.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 112.9413(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.46080(19)
_cell_length_b                   21.55872(18)
_cell_length_c                   15.06929(15)
_cell_measurement_reflns_used    30930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.9165
_cell_measurement_theta_min      3.0330
_cell_volume                     5223.90(10)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_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 0.975
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details
;
  1 omega   -6.00   81.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550   64.0000   64.0000 87

  2 omega  -26.00   43.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550  -37.0000  330.0000 69

  3 omega  -47.00   47.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550  -77.0000  210.0000 94

  4 omega   -9.00   59.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550   37.0000  210.0000 68

  5 omega  -53.00   24.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550  -77.0000   90.0000 77

  6 omega  -13.00   87.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550   77.0000  270.0000 100

  7 omega   34.00   70.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550  179.0000   30.0000 36

  8 omega  -50.00   40.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -       17.1550  -64.0000  115.0000 90

;
_diffrn_measurement_device_type  'Goniometer KM4/Xcalibur,detector: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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            65088
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.98
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    3.239
_exptl_absorpt_correction_T_max  0.8050
_exptl_absorpt_correction_T_min  0.4056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             2316
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.172
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         12734
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0257
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0551
_reflns_number_gt                9162
_reflns_number_total             12734
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9037164_si_001_3.cif
_cod_data_source_block           complex8
_cod_original_cell_volume        5223.89(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4101776