Actinide Redox-Active Ligand Complexes: Reversible Intramolecular Electron-Transfer in U(dpp-BIAN)2/U(dpp-BIAN)2(THF)
Eric J. Schelter; Ruilian Wu; Brian L. Scott; Joe D. Thompson; Thibault Cantat; Kevin D. John; Enrique R. Batista; David E. Morris; Jaqueline L. Kiplinger; Inorganic Chemistry 49 (2010) 924–933; doi:10.1021/ic901636f

data_4314643
_publ_contact_author_address
;Los Alamos National Laboratory
Los Alamos, NM
87545
U.S.A.
;
_publ_contact_author_email       kiplinger@lanl.gov
_publ_contact_author_fax         505-667-9905
_publ_contact_author_name        'Jaqueline L. Kiplinger'
_publ_contact_author_phone       505-665-9553
_publ_section_title
;
 Actinide Redox-Active Ligand Complexes: Reversible Intramolecular
 Electron-Transfer in U(dpp-BIAN)2/U(dpp-BIAN)2(THF)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              924
_journal_page_last               933
_journal_paper_doi               10.1021/ic901636f
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C76 H88 N4 O Th'
_chemical_formula_weight         1305.58
_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                108.072(2)
_cell_angle_beta                 101.114(2)
_cell_angle_gamma                101.312(2)
_cell_formula_units_Z            4
_cell_length_a                   17.1974(19)
_cell_length_b                   18.163(2)
_cell_length_c                   24.980(3)
_cell_measurement_temperature    120(1)
_cell_volume                     6999.3(14)
_computing_cell_refinement       'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_data_collection       'APEX II, v. 1.08 (Bruker AXS, 2003)'
_computing_data_reduction        'SAINT+, v. 7.06 (Bruker AXS, 2001)'
_computing_molecular_graphics    'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_publication_material  'SHELXTL, v. 6.10, (Bruker AXS, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(1)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 with APEXII CCD'
_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  0.0889
_diffrn_reflns_av_sigmaI/netI    0.1283
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            68068
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.182
_exptl_absorpt_correction_T_max  0.9178
_exptl_absorpt_correction_T_min  0.6694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.03 (Sheldrick, 2001)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             2980
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_platon_squeeze_details
;
5 thf solvent molecules and 2 solvent hexane molecules, all disordered, were
treated using SQUEEZE platon.  A.L. Spek, 2003, J. Appl. Cryst. 36, 7-13.
;
_refine_diff_density_max         2.825
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.158
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1509
_refine_ls_number_reflns         25322
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0568
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1351
_reflns_number_gt                16152
_reflns_number_total             25322
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901636f_si_001_3.cif
_cod_data_source_block           apx701s
_cod_original_cell_volume        6999.4(13)
_cod_original_formula_sum        'C76 H88 N4 O1 Th1'
_cod_database_code               4314643