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_4120284
_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            'C68 H139 K N4 O18 Si5 U'
_chemical_formula_weight         1718.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.479(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.7947(3)
_cell_length_b                   26.1912(7)
_cell_length_c                   25.0278(5)
_cell_measurement_reflns_used    16500
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3960
_cell_measurement_theta_min      3.3741
_cell_volume                     9025.9(4)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega  -20.00   60.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000  -90.0000 80

  2 omega   29.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   57.0000   60.0000 65

  3 omega    6.00   39.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -57.0000   30.0000 33

  4 omega  -75.00  -49.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801 -179.0000 -150.0000 26

  5 omega  -97.00    3.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000 -120.0000 100

  6 omega  -89.00  -41.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  134.0000   66.0000 48

  7 omega  -90.00    9.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -19.0000   60.0000 99

  8 omega    0.00   58.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   37.0000    0.0000 58

;
_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  0.0564
_diffrn_reflns_av_sigmaI/netI    0.0558
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            95622
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.38
_exptl_absorpt_coefficient_mu    1.969
_exptl_absorpt_correction_T_max  0.8023
_exptl_absorpt_correction_T_min  0.3217
_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 blue'
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3600
_exptl_crystal_size_max          0.75
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.395
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     932
_refine_ls_number_reflns         22368
_refine_ls_number_restraints     226
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0355P)^2^+22.2811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0941
_refine_ls_wR_factor_ref         0.1074
_reflns_number_gt                16407
_reflns_number_total             22368
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_07.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4120284