Complexes of Triamidoamines with the Early Actinides. Synthetic Routes to Monomeric Compounds of Tetravalent Uranium and Thorium Containing Halide and Amide Ligands
Paul Roussel; Nathaniel W. Alcock; Rita Boaretto; Andrew J. Kingsley; Ian J. Munslow; Christopher J. Sanders; Peter Scott; Inorganic Chemistry 38 (1999) 3651–3656; doi:10.1021/ic990563f

data_4322191
_publ_section_title
;
 Complexes of Triamidoamines with the Early Actinides. Synthetic Routes to
 Monomeric Compounds of Tetravalent Uranium and Thorium Containing Halide
 and Amide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3651
_journal_page_last               3656
_journal_paper_doi               10.1021/ic990563f
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C24 H57 Cl N4 Si3 U'
_chemical_formula_weight         759.49
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 116.69
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.7553(10)
_cell_length_b                   15.1678(10)
_cell_length_c                   22.7921(10)
_cell_measurement_reflns_used    42988
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     7028.5(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_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  0.0771
_diffrn_reflns_av_sigmaI/netI    0.0581
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            42973
_diffrn_reflns_theta_full        28.61
_diffrn_reflns_theta_max         28.61
_diffrn_reflns_theta_min         1.00
_exptl_absorpt_coefficient_mu    4.815
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            Pale_orange
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3040
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.692
_refine_diff_density_min         -3.620
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.255(7)
_refine_ls_extinction_coef       0.00013(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1251
_refine_ls_number_reflns         24510
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.242
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.195
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1574
_refine_ls_wR_factor_ref         0.1718
_reflns_number_gt                21578
_reflns_number_total             24510
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990563f_1.cif
_cod_data_source_block           unclm
_cod_original_cell_volume        7028.3(6)
_cod_database_code               4322191