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_4103685
_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            'C40 H28 N4 O4 U'
_chemical_formula_weight         866.69
_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                 104.828(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0533(4)
_cell_length_b                   16.1590(5)
_cell_length_c                   18.3135(6)
_cell_measurement_reflns_used    4736
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3732
_cell_measurement_theta_min      3.4054
_cell_volume                     3162.05(19)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   15.00   41.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489   77.0000   30.0000 26

  2 omega   48.00   98.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489  179.0000  150.0000 50

  3 omega   36.00   87.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489  179.0000 -150.0000 51

  4 omega   35.00   91.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.2489  179.0000  -90.0000 56

  5 omega  -89.00   -1.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9676  -37.0000  -90.0000 88

  6 omega -103.00  -34.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9676  179.0000  150.0000 69

  7 omega  -96.00   -5.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -26.9676  -37.0000    0.0000 91

;
_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  0.0654
_diffrn_reflns_av_sigmaI/netI    0.1209
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            28635
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.41
_exptl_absorpt_coefficient_mu    5.185
_exptl_absorpt_correction_T_max  0.8040
_exptl_absorpt_correction_T_min  0.5043
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.821
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'monoclinic prism'
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.254
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         7842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.784
_refine_ls_R_factor_all          0.0845
_refine_ls_R_factor_gt           0.0464
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.0958
_reflns_number_gt                4535
_reflns_number_total             7842
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1089364_si_002.cif
_cod_data_source_block           bi113
_cod_original_cell_volume        3162.04(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4103685