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_4080324
_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_moiety         'C42 H76 N2 O2 Si2 Th'
_chemical_formula_sum            'C42 H76 N2 O2 Si2 Th'
_chemical_formula_weight         929.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 92.1110(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.0165(4)
_cell_length_b                   10.3489(2)
_cell_length_c                   21.9123(5)
_cell_measurement_reflns_used    6771
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.86
_cell_measurement_theta_min      2.81
_cell_volume                     4536.03(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    ORTEP3(Farrugia,1997)
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \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  0.0422
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            16160
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.87
_exptl_absorpt_coefficient_mu    3.373
_exptl_absorpt_correction_T_max  0.8232
_exptl_absorpt_correction_T_min  0.6876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs; Sheldrick 2004'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.496
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0306
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0227P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0489
_refine_ls_wR_factor_ref         0.0501
_reflns_number_gt                3917
_reflns_number_total             4316
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3010806_si_002.cif
_cod_data_source_block           Comp-9
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4080324