Uranium-Nitrogen Multiple Bonding: Isostructural Anionic, Neutral, and Cationic Uranium Nitride Complexes Featuring a Linear U=N=U Core
Alexander R. Fox; Polly L. Arnold; Christopher C. Cummins; Journal of the American Chemical Society 132 (2010) 3250–3251; doi:10.1021/ja910364u

data_4102058
_publ_contact_author_address
;77 Massachusetts Avenue
Room 6-435
Cambridge, MA 02139 USA
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_publ_contact_author_email       ccummins@mit.edu
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Uranium-Nitrogen Multiple Bonding: Isostructural Anionic, Neutral, and
 Cationic Uranium Nitride Complexes Featuring a Linear U=N=U Core
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3250
_journal_page_last               3251
_journal_paper_doi               10.1021/ja910364u
_journal_volume                  132
_journal_year                    2010
_chemical_formula_sum            'C108 H128 B F24 N7 O U2'
_chemical_formula_weight         2483.04
_chemical_name_systematic
'[(u-N)(U(N[t-Bu][3,5-Me2C6H3])3)2][B(3,5-(CF3)2C6H3)4]'
_chemical_properties_physical
'air-sensitive, moisture-sensitive, oxygen-sensitive, paramagnetic'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.253(4)
_cell_angle_beta                 94.050(4)
_cell_angle_gamma                91.825(4)
_cell_formula_units_Z            2
_cell_length_a                   14.138(3)
_cell_length_b                   14.224(3)
_cell_length_c                   27.716(6)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.12
_cell_measurement_theta_min      2.31
_cell_volume                     5382(2)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_data_collection       'APEX2 3.0 (Bruker-AXS, 2008)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_sigmaI/netI    0.0792
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            103322
_diffrn_reflns_theta_full        27.88
_diffrn_reflns_theta_max         27.88
_diffrn_reflns_theta_min         0.76
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.097
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.2381
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2476
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.340
_refine_diff_density_min         -1.213
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1377
_refine_ls_number_reflns         25673
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0311P)^2^+3.4137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0754
_refine_ls_wR_factor_ref         0.0880
_reflns_number_gt                17681
_reflns_number_total             25673
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja910364u_si_001_1.cif
_cod_data_source_block           08055
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
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_cod_database_code               4102058