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_4080320
_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            'C24 H33 I2 N3 O2 U'
_chemical_formula_weight         887.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           96
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.52423(14)
_cell_length_b                   8.52423(14)
_cell_length_c                   38.5227(12)
_cell_measurement_reflns_used    7805
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      36.8979
_cell_measurement_theta_min      3.3646
_cell_volume                     2799.16(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
  1 omega  -97.00  -67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.2186  179.0000 -150.0000 30

  2 omega  -73.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.2186  179.0000 -180.0000 41

  3 omega   74.00  109.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0099  125.0000    0.0000 35

  4 omega   77.00  126.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0099  125.0000   60.0000 49

  5 omega   79.00  138.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0099   86.0000  107.0000 59

  6 omega   50.00   93.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0099  -45.0000   30.0000 43

  7 omega  -34.00   -3.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       48.0099  -45.0000   30.0000 31

  8 omega  -46.00   88.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -0.2186   77.0000   90.0000 134

  9 omega  -47.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       -1.1877   77.0000   30.0000 134

 10 omega -131.00  -97.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -49.4161  -45.0000   30.0000 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  0.0432
_diffrn_reflns_av_sigmaI/netI    0.0696
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -55
_diffrn_reflns_number            16414
_diffrn_reflns_theta_full        30.50
_diffrn_reflns_theta_max         30.50
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    8.028
_exptl_absorpt_correction_T_max  0.4587
_exptl_absorpt_correction_T_min  0.2596
_exptl_absorpt_correction_type   analytical
_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)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bloc
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.288
_refine_diff_density_min         -1.735
_refine_diff_density_rms         0.168
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         4223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0845
_reflns_number_gt                2986
_reflns_number_total             4223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om3010806_si_002.cif
_cod_data_source_block           Comp-4
_cod_original_cell_volume        2799.15(11)
_cod_database_code               4080320