Tuning Uranium-Nitrogen Multiple Bond Formation with Ancillary Siloxide Ligands
Clément Camp; Jacques Pécaut; Marinella Mazzanti; Journal of the American Chemical Society 135 (2013) 12101–12111; doi:10.1021/ja405815b

data_4120287
_publ_section_title
;
 Tuning Uranium-Nitrogen Multiple Bond Formation with Ancillary Siloxide
 Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12101
_journal_page_last               12111
_journal_paper_doi               10.1021/ja405815b
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C86 H178 K2 N2 O24 Si6 U2'
_chemical_formula_weight         2347.10
_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                90.824(3)
_cell_angle_beta                 106.789(3)
_cell_angle_gamma                115.962(3)
_cell_formula_units_Z            1
_cell_length_a                   13.3139(4)
_cell_length_b                   13.6374(4)
_cell_length_c                   18.3661(7)
_cell_measurement_reflns_used    16094
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.5881
_cell_measurement_theta_min      3.3617
_cell_volume                     2831.68(19)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
  1 omega   53.00   91.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7176 -138.0000  -14.0000 38

  2 omega  -47.00   52.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7176  -37.0000 -120.0000 99

  3 omega  -93.00   -5.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  138.0000   47.0000 88

  4 omega  -98.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -77.0000 -120.0000 101

  5 omega  -98.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -77.0000   30.0000 101

  6 omega -101.00  -34.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364 -179.0000   90.0000 67

  7 omega  -98.00    3.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -77.0000  150.0000 101

  8 omega -100.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -37.0000  -90.0000 98

  9 omega  -68.00   45.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364   19.0000   90.0000 113

 10 omega    0.00   98.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7176   37.0000    0.0000 98

 11 omega   34.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       25.7176  179.0000  120.0000 68

 12 omega  -96.00  -49.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -57.0000  120.0000 47

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w 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  0.0842
_diffrn_reflns_av_sigmaI/netI    0.0810
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            67850
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    3.054
_exptl_absorpt_correction_T_max  0.7664
_exptl_absorpt_correction_T_min  0.2603
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_description       plate
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.09
_refine_diff_density_max         11.179
_refine_diff_density_min         -3.932
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         17272
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0977
_refine_ls_R_factor_gt           0.0739
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+37.2578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1679
_reflns_number_gt                13943
_reflns_number_total             17272
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_10.cif
_cod_data_source_block           9
_cod_original_cell_volume        2831.69(17)
_cod_database_code               4120287