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_4080319
_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         'C44 H62 I2 N4 O2 U, 2(C7 H8)'
_chemical_formula_sum            'C58 H78 I2 N4 O2 U'
_chemical_formula_weight         1355.07
_chemical_name_systematic
;
 ?
;
_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                 91.005(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.1592(9)
_cell_length_b                   31.130(3)
_cell_length_c                   18.5587(17)
_cell_measurement_reflns_used    5097
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.83
_cell_measurement_theta_min      2.62
_cell_volume                     5868.4(9)
_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, 2008)'
_computing_structure_solution    'SIR97 (Altomare, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_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  0.0743
_diffrn_reflns_av_sigmaI/netI    0.1343
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            27270
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    3.859
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_correction_T_min  0.5124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'sadabs; Sheldrick 2004'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.534
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.494
_refine_diff_density_min         -2.303
_refine_diff_density_rms         0.220
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         10070
_refine_ls_number_restraints     128
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.1411
_refine_ls_R_factor_gt           0.0719
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0587P)^2^+1.4363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1413
_refine_ls_wR_factor_ref         0.1571
_reflns_number_gt                6059
_reflns_number_total             10070
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om3010806_si_002.cif
_cod_data_source_block           comp-3
_cod_original_cell_volume        5868.4(10)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4080319