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_4120282
_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            'C71.5 H150.5 K N O22 Si4 U'
_chemical_formula_weight         1765.92
_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                94.358(4)
_cell_angle_beta                 91.810(4)
_cell_angle_gamma                118.909(5)
_cell_formula_units_Z            2
_cell_length_a                   14.4543(8)
_cell_length_b                   14.5344(8)
_cell_length_c                   25.4464(12)
_cell_measurement_reflns_used    3690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.0035
_cell_measurement_theta_min      3.2585
_cell_volume                     4651.9(5)
_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      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
  1 omega  -39.00   50.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613   57.0000  120.0000 89

  2 omega  -25.00   23.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613  -99.0000 -120.0000 48

  3 omega  -42.00   52.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613   37.0000 -120.0000 94

  4 omega  -87.00    3.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613  -57.0000  -30.0000 90

  5 omega  -95.00  -32.00   1.0000   98.0000
omega____ theta____ kappa____ phi______ frames
    -      -18.5613  179.0000 -120.0000 63

;
_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  0.0979
_diffrn_reflns_av_sigmaI/netI    0.2167
_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       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            35721
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.27
_exptl_absorpt_coefficient_mu    1.902
_exptl_absorpt_correction_T_max  0.9487
_exptl_absorpt_correction_T_min  0.8195
_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            'translucent light bronze'
_exptl_crystal_density_diffrn    1.261
_exptl_crystal_description       plate
_exptl_crystal_F_000             1859
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     978
_refine_ls_number_reflns         18800
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.1476
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0259P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1100
_refine_ls_wR_factor_ref         0.1325
_reflns_number_gt                11498
_reflns_number_total             18800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_05.cif
_cod_data_source_block           5-Ad
_cod_original_cell_volume        4651.9(4)
_cod_original_formula_sum        'C71.50 H150.50 K N O22 Si4 U'
_cod_database_code               4120282