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_4120285
_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            'C67 H140 K N3 O22 Si4 U'
_chemical_formula_weight         1729.31
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 98.009(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0305(5)
_cell_length_b                   24.7215(7)
_cell_length_c                   26.3108(9)
_cell_measurement_reflns_used    11495
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.3738
_cell_measurement_theta_min      3.4840
_cell_volume                     9037.0(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  -47.00   53.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8739    0.0000  150.0000 100

  2 omega    2.00   66.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8739  -99.0000  -60.0000 64

  3 omega  -45.00    4.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -84.0000  134.0000 49

  4 omega -100.00  -48.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -19.0000 -150.0000 52

  5 omega    5.00   94.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000  -30.0000 89

  6 omega -103.00  -34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239 -179.0000   30.0000 69

  7 omega  -19.00   50.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   19.0000 -150.0000 69

;
_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  0.0454
_diffrn_reflns_av_sigmaI/netI    0.0719
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            44869
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         3.51
_exptl_absorpt_coefficient_mu    1.957
_exptl_absorpt_correction_T_max  0.4915
_exptl_absorpt_correction_T_min  0.2805
_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            'light green'
_exptl_crystal_density_diffrn    1.271
_exptl_crystal_description       Bloc
_exptl_crystal_F_000             3624
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.62
_exptl_crystal_size_min          0.42
_refine_diff_density_max         2.530
_refine_diff_density_min         -1.285
_refine_diff_density_rms         0.095
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.003(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         21805
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0750
_refine_ls_R_factor_gt           0.0580
_refine_ls_shift/su_max          0.052
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+9.5553P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1200
_refine_ls_wR_factor_ref         0.1287
_reflns_number_gt                18236
_reflns_number_total             21805
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_08.cif
_cod_data_source_block           7
_cod_database_code               4120285