A trigonal Bipyramidal Uranyl Amido Complex: Synthesis and Structural Characterization of [Na(THF)~2~][UO~2~(N(SiMe~3~)~2~)~3~]
Carol J. Burns; David L. Clark; Robert J. Donohoe; Paul B. Duval; Brian L. Scott; C. Drew Tait; Inorganic Chemistry 39 (2000) 5464–5468; doi:10.1021/ic0003168

data_4321589
_publ_section_title
;
 A trigonal Bipyramidal Uranyl Amido Complex: Synthesis and Structural
 Characterization of [Na(THF)~2~][UO~2~(N(SiMe~3~)~2~)~3~]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5464
_journal_page_last               5468
_journal_paper_doi               10.1021/ic0003168
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C26 H70 N3 Na O4 Si6 U'
_chemical_formula_weight         918.41
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 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                   22.945(1)
_cell_length_b                   15.2830(7)
_cell_length_c                   12.6787(6)
_cell_measurement_temperature    203(2)
_cell_volume                     4446.0(4)
_computing_cell_refinement       'XSCANS 2.10b (Siemens, 1994)'
_computing_data_collection       'XSCANS 2.10b (Siemens, 1994)'
_computing_data_reduction        'XSCANS 2.10b (Siemens, 1994)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device_type  'Bruker P4/CCD'
_diffrn_measurement_method       '\w and \f 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  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            20628
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.60
_diffrn_standards_decay_%        '< 2'
_exptl_absorpt_coefficient_mu    3.851
_exptl_absorpt_correction_T_max  0.86
_exptl_absorpt_correction_T_min  0.73
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.372
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1864
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.467
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.000(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.939
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.939
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0140P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0524
_refine_ls_wR_factor_ref         0.0573
_reflns_number_gt                5790
_reflns_number_total             7514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0003168.cif
_cod_data_source_block           ccd172a
_cod_database_code               4321589