Multielectron Redox Reactions Involving C-C Coupling and Cleavage in Uranium Schiff Base Complexes
Clément Camp; Victor Mougel; Pawel Horeglad; Jacques Pécaut; Marinella Mazzanti; Journal of the American Chemical Society 132 (2010) 17374–17377; doi:10.1021/ja1089364

data_4103686
_publ_section_title
;
 Multielectron Redox Reactions Involving C-C Coupling and Cleavage in
 Uranium Schiff Base Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17374
_journal_page_last               17377
_journal_paper_doi               10.1021/ja1089364
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C87.27 H99.27 N8.65 Na2 O16 U'
_chemical_formula_weight         1809.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 116.62(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.019(3)
_cell_length_b                   45.018(9)
_cell_length_c                   14.960(3)
_cell_measurement_reflns_used    4599
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.8687
_cell_measurement_theta_min      3.2640
_cell_volume                     8441(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_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega   63.00  103.50   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -       28.0166  179.0000   30.0000 54

  2 omega -124.00  -34.00   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.4229  179.0000   60.0000 120

  3 omega   30.00   55.50   0.7500   80.0000
omega____ theta____ kappa____ phi______ frames
    -      -29.4229   37.0000 -150.0000 34

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1463
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       56
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            17185
_diffrn_reflns_theta_full        26.30
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.28
_exptl_absorpt_coefficient_mu    2.004
_exptl_absorpt_correction_T_max  0.9591
_exptl_absorpt_correction_T_min  0.4559
_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            black
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3702
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.283
_refine_diff_density_min         -2.309
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1045
_refine_ls_number_reflns         17185
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0581
_refine_ls_shift/su_max          0.086
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                9506
_reflns_number_total             17185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1089364_si_003.cif
_cod_data_source_block           cc_global
_cod_original_cell_volume        8440(3)
_cod_database_code               4103686