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_4120278
_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            'C48 H108 O16 Si4 U'
_chemical_formula_weight         1291.73
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
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_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                 96.462(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.1332(9)
_cell_length_b                   13.5042(6)
_cell_length_c                   20.4034(9)
_cell_measurement_reflns_used    4982
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4594
_cell_measurement_theta_min      3.3915
_cell_volume                     6607.2(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_computing_data_reduction
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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 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
  1 omega   -4.00   96.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   77.0000  -60.0000 100

  2 omega  -87.00   26.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801    0.0000  -30.0000 113

  3 omega  -71.00  -23.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   19.0000   60.0000 48

  4 omega   -6.00   22.00   1.0000    2.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   19.0000  -90.0000 28

;
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0670
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            20116
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.40
_exptl_absorpt_coefficient_mu    2.584
_exptl_absorpt_correction_T_max  0.5795
_exptl_absorpt_correction_T_min  0.2890
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             2688
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.53
_exptl_crystal_size_min          0.24
_refine_diff_density_max         2.798
_refine_diff_density_min         -1.553
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         8461
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0459
_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^)+(0.0436P)^2^+7.5926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1070
_reflns_number_gt                7113
_reflns_number_total             8461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_01.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'C 2/m '
_cod_database_code               4120278