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_4103687
_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            'C34 H38 F6 N2 O11 S2 U'
_chemical_formula_weight         1066.81
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 99.689(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.2090(13)
_cell_length_b                   17.2523(14)
_cell_length_c                   15.0510(10)
_cell_measurement_reflns_used    7918
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      42.9032
_cell_measurement_theta_min      3.4461
_cell_volume                     3892.9(5)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -50.00  -17.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.5857  -55.0000  168.0000 33

  2 omega  -73.00   24.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.5857  -37.0000 -150.0000 97

  3 omega   20.00   95.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  -90.0000 75

  4 omega   20.00   87.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000 -150.0000 67

  5 omega   43.00   84.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000   30.0000 41

  6 omega   20.00   90.00   1.0000  100.0000
omega____ theta____ kappa____ phi______ frames
    -       50.0000   77.0000  120.0000 70

;
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.1078
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26300
_diffrn_reflns_theta_full        28.20
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.45
_exptl_absorpt_coefficient_mu    4.365
_exptl_absorpt_correction_T_max  0.8016
_exptl_absorpt_correction_T_min  0.2995
_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            yellow
_exptl_crystal_density_diffrn    1.820
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2088
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.05
_refine_diff_density_max         7.726
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     506
_refine_ls_number_reflns         9767
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.936
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0791
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1866
_refine_ls_wR_factor_ref         0.2069
_reflns_number_gt                5682
_reflns_number_total             9767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1089364_si_004.cif
_cod_data_source_block           cc88_2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4103687