Synthesis of a Nitrido-Substituted Analogue of the Uranyl Ion, [N=U=O]+
Skye Fortier; Guang Wu; Trevor W. Hayton; Journal of the American Chemical Society 132 (2010) 6888–6889; doi:10.1021/ja101567h

data_4102430
_publ_contact_author_email       hayton@chem.ucsb.edu
_publ_contact_author_name        'Trevor W. Hayton'
_publ_section_title
;
 Synthesis of a Nitrido-Substituted Analogue of the Uranyl Ion, [N=U=O]+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6888
_journal_page_last               6889
_journal_paper_doi               10.1021/ja101567h
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C30 H89 N6 Si10 U2'
_chemical_formula_weight         1291.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.970(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1880(16)
_cell_length_b                   25.359(3)
_cell_length_c                   18.120(2)
_cell_measurement_temperature    150(2)
_cell_volume                     5559.1(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0636
_diffrn_reflns_av_sigmaI/netI    0.0627
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            44879
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.39
_exptl_absorpt_coefficient_mu    6.060
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.4587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark_orange
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2540
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.346
_refine_diff_density_min         -2.866
_refine_diff_density_rms         0.240
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         11167
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0791P)^2^+4.4341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1314
_reflns_number_gt                8636
_reflns_number_total             11167
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja101567h_si_001_2.cif
_cod_data_source_block           Complex_2
_cod_original_cell_volume        5559.0(12)
_cod_database_code               4102430