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_4119447
_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 Er2 N21 O4 U2'
_chemical_formula_sum            'C109 H105 Er2 N21 O4 U2'
_chemical_formula_weight         2583.72
_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                 108.055(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.3807(3)
_cell_length_b                   27.5419(4)
_cell_length_c                   23.0385(4)
_cell_measurement_reflns_used    21586
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.1789
_cell_measurement_theta_min      2.9716
_cell_volume                     9882.1(3)
_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
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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 0.978
_diffrn_measured_fraction_theta_max 0.978
_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  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            65338
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    5.014
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       plate
_exptl_crystal_F_000             5032
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.031
_refine_diff_density_max         1.770
_refine_diff_density_min         -1.890
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1314
_refine_ls_number_reflns         22196
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0647
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0203P)^2^+22.2297P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                16914
_reflns_number_total             22196
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja308993g_si_010.cif
_cod_data_source_block           p10093
_cod_database_code               4119447