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_4104240
_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            'C72 H95 B F15 N5 O0.5 U'
_chemical_formula_weight         1572.37
_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                83.463(2)
_cell_angle_beta                 78.237(2)
_cell_angle_gamma                88.230(3)
_cell_formula_units_Z            2
_cell_length_a                   12.1153(16)
_cell_length_b                   13.9807(18)
_cell_length_c                   23.246(3)
_cell_measurement_reflns_used    9914
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.07
_cell_measurement_theta_min      2.22
_cell_volume                     3829.5(9)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0776
_diffrn_reflns_av_sigmaI/netI    0.0783
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            78994
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.77
_exptl_absorpt_coefficient_mu    2.198
_exptl_absorpt_correction_T_max  0.8981
_exptl_absorpt_correction_T_min  0.7632
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1596
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.836
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     920
_refine_ls_number_reflns         18938
_refine_ls_number_restraints     166
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0420P)^2^+0.4933P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                15007
_reflns_number_total             18938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8095812_si_002_2.cif
_cod_data_source_block           07159'
_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_cell_volume        3829.6(9)
_cod_original_formula_sum        'C72 H95 B F15 N5 O0.50 U'
_cod_database_code               4104240