Diamine Bis(phenolate) as Supporting Ligands in Organoactinide(IV) Chemistry. Synthesis, Structural Characterization, and Reactivity of Stable Dialkyl Derivatives
Mora, Elsa; Maria, Leonor; Biswas, Biplab; Camp, Clément; Santos, Isabel C.; Pécaut, Jacques; Cruz, Adelaide; Carretas, José M.; Marçalo, Joaquim; Mazzanti, Marinella; Organometallics 32 (2013) 1409–; doi:10.1021/om3010806

data_4080317
_publ_section_title
;
 Diamine Bis(phenolate) as Supporting Ligands in Organoactinide(IV)
 Chemistry. Synthesis, Structural Characterization, and Reactivity of
 Stable Dialkyl Derivatives
;
_journal_issue                   5
_journal_name_full               Organometallics
_journal_page_first              1409
_journal_paper_doi               10.1021/om3010806
_journal_volume                  32
_journal_year                    2013
_chemical_formula_sum            'C70.5 H111.75 N5.25 O4 U'
_chemical_formula_weight         1334.93
_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                85.198(2)
_cell_angle_beta                 78.323(2)
_cell_angle_gamma                60.699(3)
_cell_formula_units_Z            4
_cell_length_a                   15.1010(4)
_cell_length_b                   15.3382(5)
_cell_length_c                   36.8413(6)
_cell_measurement_reflns_used    26755
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.7185
_cell_measurement_theta_min      3.3262
_cell_volume                     7286.3(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
  1 omega  -66.00    7.50   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7031   37.0000  -60.0000 98

  2 omega  -26.00   22.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7031  -77.0000  120.0000 65

  3 omega   18.00   84.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.7031   37.0000  -60.0000 88

  4 omega   73.00  100.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5792  125.0000  -30.0000 36

  5 omega   73.00  109.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5792  125.0000  -60.0000 48

  6 omega   -6.00  102.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5792   77.0000 -120.0000 144

  7 omega   80.00  117.50   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5792  125.0000   60.0000 50

  8 omega   89.00  119.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5792  147.0000  107.0000 41

  9 omega  -28.00    8.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9855  -77.0000 -120.0000 48

 10 omega -123.00  -27.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9855  -37.0000  -30.0000 128

 11 omega -121.00  -72.25   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9855  -77.0000 -120.0000 65

 12 omega  -62.00   47.50   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9855   77.0000   90.0000 146

 13 omega -109.00   -9.25   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9855  125.0000   90.0000 133

 14 omega  -22.00    5.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -37.9855  -37.0000  -30.0000 36

;
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.1291
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            78136
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.34
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.9106
_exptl_absorpt_correction_T_min  0.3558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2782
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.04
_refine_diff_density_max         8.976
_refine_diff_density_min         -1.782
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1522
_refine_ls_number_reflns         35669
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      0.909
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0836P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1459
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                20929
_reflns_number_total             35669
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010806_si_002.cif
_cod_data_source_block           Comp-2.CH3CN
_cod_original_formula_sum        'C70.50 H111.75 N5.25 O4 U'
_cod_database_code               4080317