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_4120279
_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            'C58 H118 N2 O16 Si4 U'
_chemical_formula_weight         1449.93
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 118.606(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.5649(8)
_cell_length_b                   13.2630(3)
_cell_length_c                   25.9619(8)
_cell_measurement_reflns_used    18552
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4232
_cell_measurement_theta_min      3.3107
_cell_volume                     7426.0(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
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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_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   34.00   99.25   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  179.0000    0.0000 87

  2 omega   24.00   68.25   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614 -103.0000    6.0000 59

  3 omega  -71.00   -3.50   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  103.0000  173.0000 90

  4 omega  -49.00   40.25   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   57.0000  120.0000 119

  5 omega  -63.00   39.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   19.0000   60.0000 136

  6 omega  -97.00  -67.75   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  120.0000 39

  7 omega  -97.00    2.00   0.7500   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000    0.0000 132

;
_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  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33275
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    2.308
_exptl_absorpt_correction_T_max  0.8123
_exptl_absorpt_correction_T_min  0.5918
_exptl_absorpt_correction_type   multi-scan
_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)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light green'
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3024
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7590
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0234
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0281P)^2^+4.2675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0529
_refine_ls_wR_factor_ref         0.0542
_reflns_number_gt                7026
_reflns_number_total             7590
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_02.cif
_cod_data_source_block           3-py
_cod_original_cell_volume        7426.0(4)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4120279