Uranium-Nitrogen Multiple Bonding: The Case of a Four-Coordinate Uranium(VI) Nitridoborate Complex
Alexander R. Fox; Christopher C. Cummins; Journal of the American Chemical Society 131 (2009) 5716–5717; doi:10.1021/ja8095812

data_4104239
_publ_contact_author_address
;77 Massachusetts Avenue
Room 6-435
Cambridge, MA 02139
USA
;
_publ_contact_author_name        'Christopher C. Cummins'
_publ_section_title
;
 Uranium-Nitrogen Multiple Bonding: The Case of a Four-Coordinate
 Uranium(VI) Nitridoborate Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5716
_journal_page_last               5717
_journal_paper_doi               10.1021/ja8095812
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C56 H59 B F15 N4 O0.5 U'
_chemical_formula_weight         1329.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                102.6840(10)
_cell_angle_beta                 90.3810(10)
_cell_angle_gamma                106.7380(10)
_cell_formula_units_Z            2
_cell_length_a                   12.8381(6)
_cell_length_b                   14.0439(7)
_cell_length_c                   17.3667(8)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      22.9
_cell_measurement_theta_min      2.2
_cell_volume                     2917.1(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      193(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX CCD'
_diffrn_measurement_method       'omega and phi 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  0.0672
_diffrn_reflns_av_sigmaI/netI    0.0750
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            63873
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    2.870
_exptl_absorpt_correction_T_max  0.8029
_exptl_absorpt_correction_T_min  0.5459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             1318
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.412
_refine_diff_density_min         -1.165
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         16304
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0420
_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^)+(0.0535P)^2^+0.7818P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                12162
_reflns_number_total             16304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8095812_si_002_1.cif
_cod_data_source_block           07166
_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 
;
_cod_original_formula_sum        'C56 H59 B F15 N4 O0.50 U'
_cod_database_code               4104239