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_4103684
_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            'C140 H116 N20 O8 U4'
_chemical_formula_weight         3158.65
_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                103.1296(14)
_cell_angle_beta                 99.9454(15)
_cell_angle_gamma                91.5909(14)
_cell_formula_units_Z            1
_cell_length_a                   11.6556(2)
_cell_length_b                   12.0214(2)
_cell_length_c                   22.0847(4)
_cell_measurement_reflns_used    23343
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.6398
_cell_measurement_theta_min      2.9908
_cell_volume                     2961.01(9)
_computing_cell_refinement
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega  -39.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577  -77.0000   60.0000 99

  2 omega   35.00   88.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577  179.0000    0.0000 53

  3 omega  -31.00   -1.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577  132.0000   99.0000 30

  4 omega  -32.00   56.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577  -37.0000   90.0000 88

  5 omega    3.00   92.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577 -131.0000  -93.0000 89

  6 omega   -5.00   85.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577 -123.0000    6.0000 90

  7 omega -101.00   -3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  -77.0000    0.0000 98

  8 omega  -74.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  -37.0000   60.0000 68

  9 omega  -95.00   -6.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  -37.0000    0.0000 89

 10 omega  -91.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  179.0000  -90.0000 59

 11 omega -100.00   -2.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  -77.0000  -90.0000 98

 12 omega -101.00  -11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  -58.0000  168.0000 90

 13 omega    9.00  100.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577   52.0000  175.0000 91

 14 omega    1.00  101.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       30.6577   77.0000  -90.0000 100

 15 omega -109.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  179.0000   90.0000 77

 16 omega -102.00  -11.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.2202  -52.0000   30.0000 91

;
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: 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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            94669
_diffrn_reflns_theta_full        30.45
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    5.523
_exptl_absorpt_correction_T_max  0.7697
_exptl_absorpt_correction_T_min  0.4913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.771
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.912
_refine_diff_density_min         -0.633
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.853
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     945
_refine_ls_number_reflns         18076
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.853
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0642P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1083
_reflns_number_gt                11429
_reflns_number_total             18076
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1089364_si_001.cif
_cod_data_source_block           ph192
_cod_original_cell_volume        2960.99(9)
_cod_database_code               4103684