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_4119443
_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         'C116 H143 N16 O12 Sm2 U2'
_chemical_formula_sum            'C116 H143 N16 O12 Sm2 U2'
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                96.358(3)
_cell_angle_beta                 97.314(3)
_cell_angle_gamma                102.638(4)
_cell_formula_units_Z            2
_cell_length_a                   15.1951(6)
_cell_length_b                   16.2840(8)
_cell_length_c                   26.5859(8)
_cell_measurement_reflns_used    8632
_cell_measurement_temperature    170(2)
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_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'ORTEP (Farrugia, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      170(2)
_diffrn_detector_area_resol_mean 16.1042
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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
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_diffrn_reflns_av_R_equivalents  0.0976
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_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            56565
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.83
_diffrn_standards_number         56565
_exptl_absorpt_coefficient_mu    3.540
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_description       block
_exptl_crystal_F_000             2710
_exptl_crystal_size_max          0.181
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.043
_platon_squeeze_details
;
;
_refine_diff_density_max         1.969
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.899
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1349
_refine_ls_number_reflns         18046
_refine_ls_number_restraints     604
_refine_ls_restrained_S_all      0.894
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                8606
_reflns_number_total             18046
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja308993g_si_006.cif
_cod_data_source_block           p11187
_cod_original_cell_volume        6301.1(4)
_cod_database_code               4119443