Oxo-Functionalization and Reduction of the Uranyl Ion through Lanthanide-Element Bond Homolysis: Synthetic, Structural, and Bonding Analysis of a Series of Singly Reduced Uranyl-Rare Earth 5f1-4fn Complexes
Polly L. Arnold; Emmalina Hollis; Gary S. Nichol; Jason B. Love; Jean-Christophe Griveau; Roberto Caciuffo; Nicola Magnani; Laurent Maron; Ludovic Castro; Ahmed Yahia; Samuel O. Odoh; Georg Schreckenbach; Journal of the American Chemical Society 135 (2013) 3841–3854; doi:10.1021/ja308993g

data_4119441
_publ_section_title
;
 Oxo-Functionalization and Reduction of the Uranyl Ion through
 Lanthanide-Element Bond Homolysis: Synthetic, Structural, and Bonding
 Analysis of a Series of Singly Reduced Uranyl-Rare Earth 5f1-4fn
 Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3841
_journal_page_last               3854
_journal_paper_doi               10.1021/ja308993g
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C109 H105 Ce2 N21 O4 U2'
_chemical_formula_sum            'C109 H105 Ce2 N21 O4 U2'
_chemical_formula_weight         2529.44
_chemical_name_systematic
;
 ?
;
_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                 108.585(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5830(4)
_cell_length_b                   27.5120(5)
_cell_length_c                   23.2171(6)
_cell_measurement_reflns_used    19604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1552
_cell_measurement_theta_min      2.8644
_cell_volume                     10040.0(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_molecular_graphics    'ORTEP (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Xcalibur, Eos'
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.1340
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67855
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    4.170
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.673
_exptl_crystal_description       plate
_exptl_crystal_F_000             4952
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.041
_refine_diff_density_max         4.763
_refine_diff_density_min         -1.086
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1236
_refine_ls_number_reflns         22268
_refine_ls_number_restraints     148
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1004
_refine_ls_R_factor_gt           0.0527
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0598P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1224
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                13242
_reflns_number_total             22268
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja308993g_si_004.cif
_cod_data_source_block           p10089
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4119441