Synthesis and reactivity of uranium(IV) amide complexes supported by a triamidotriazacyclononane ligand.
Antunes, Maria Augusta; Dias, Marta; Monteiro, Bernardo; Domingos, Angela; Santos, Isabel C.; Marques, Noémia; Dalton transactions (Cambridge, England : 2003)  (2006) 3368–3374; doi:10.1039/b603000a

data_7007298
_publ_section_title
;
 Synthesis and reactivity of uranium(IV) amide complexes supported by a
 triamidotriazacyclononane ligand.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3368
_journal_page_last               3374
_journal_paper_doi               10.1039/b603000a
_journal_year                    2006
_chemical_formula_moiety         'C48 H60 N6 O P Si3 U, 2(C7 H8)'
_chemical_formula_sum            'C62 H76 N6 O P Si3 U'
_chemical_formula_weight         1274.56
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.2797(4)
_cell_length_b                   17.8483(6)
_cell_length_c                   27.1851(8)
_cell_measurement_temperature    110(2)
_cell_volume                     5958.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       'phi and omega 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  0.0590
_diffrn_reflns_av_sigmaI/netI    0.1257
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            70126
_diffrn_reflns_theta_full        34.41
_diffrn_reflns_theta_max         34.41
_diffrn_reflns_theta_min         1.82
_exptl_absorpt_coefficient_mu    2.857
_exptl_absorpt_correction_T_max  0.6905
_exptl_absorpt_correction_T_min  0.5018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2588
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.249
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.156
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.012(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.892
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         24465
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.892
_refine_ls_R_factor_all          0.0809
_refine_ls_R_factor_gt           0.0481
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0681
_reflns_number_gt                18480
_reflns_number_total             24465
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b603000a.txt
_cod_data_source_block           UtacnOPPh3
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7007298