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_4101775
_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            'C79 H109 Co N7 O4 U'
_chemical_formula_weight         1517.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                82.170(10)
_cell_angle_beta                 84.019(14)
_cell_angle_gamma                69.999(12)
_cell_formula_units_Z            2
_cell_length_a                   11.850(2)
_cell_length_b                   13.9279(12)
_cell_length_c                   26.375(5)
_cell_measurement_reflns_used    3312
_cell_measurement_temperature    150.0(2)
_cell_measurement_theta_max      28.8872
_cell_measurement_theta_min      3.0562
_cell_volume                     4044.6(11)
_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      150.0(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.718
_diffrn_measured_fraction_theta_max 0.718
_diffrn_measurement_details
;
  1 omega  -92.00    8.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175    0.0000   90.0000    0.0000    0.0000 100

  2 omega  -42.00    6.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175   45.0000  150.0000    0.0000    0.0000 48

  3 omega  -49.00    2.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175   77.0000  120.0000    0.0000    0.0000 51

  4 omega  -49.00    2.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175   77.0000  300.0000    0.0000    0.0000 51

  5 omega    5.00   54.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -18.7175    0.0000  270.0000    0.0000    0.0000 49

;
_diffrn_measurement_device_type  '\k-geometry diffractometer'
_diffrn_measurement_method       omega-scan
_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  0.0660
_diffrn_reflns_av_sigmaI/netI    0.2207
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22765
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    2.253
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.897
_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            orange
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             1566
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         4.799
_refine_diff_density_min         -1.412
_refine_diff_density_rms         0.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.955
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         15475
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.955
_refine_ls_R_factor_all          0.1599
_refine_ls_R_factor_gt           0.0918
_refine_ls_shift/su_max          0.077
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1011P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1974
_refine_ls_wR_factor_ref         0.2301
_reflns_number_gt                7651
_reflns_number_total             15475
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja9037164_si_001_2.cif
_cod_data_source_block           6
_cod_original_cell_volume        4044.7(11)
_cod_database_code               4101775