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_4120281
_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            'C88 H168 N4 O16 Si4 U2'
_chemical_formula_weight         2126.68
_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                 97.154(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5600(7)
_cell_length_b                   28.0501(11)
_cell_length_c                   25.1711(11)
_cell_measurement_reflns_used    3794
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.4328
_cell_measurement_theta_min      3.2559
_cell_volume                     10900.6(8)
_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_molecular_graphics
;
Mercury 3.1 New software for searching the Cambridge Structural Database 
and visualizing crystal structures (I.J. Bruno, J.C. Cole, P.R. Edgington, 
M. Kessler, C.F. Macrae, P. McCabe, J. Pearson, R. Taylor, 
Acta Cryst., 2002, B58, 389-397)
;
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement
;
OLEX2: a complete structure solution, refinement and analysis program 
(O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and 
H. Puschmann. J. Appl. Cryst. 2009, 42, 339-34).
;
_computing_structure_solution
;
SUPERFLIP program (Palatinus, L. & Chapuis, G. J. Appl. Cryst., 2007,
 40, 786-790)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 15.9653
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -27.00   75.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051    0.0000 -180.0000 102

  2 omega   -5.00   93.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   77.0000  150.0000 98

  3 omega  -57.00   -5.00   1.0000  150.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   77.0000   90.0000 52

;
_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  0.1588
_diffrn_reflns_av_sigmaI/netI    0.2922
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            49524
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    3.066
_exptl_absorpt_correction_T_max  0.9384
_exptl_absorpt_correction_T_min  0.7532
_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 dark brown'
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       plate
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.150
_refine_diff_density_min         -2.063
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1063
_refine_ls_number_reflns         22210
_refine_ls_number_restraints     78
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1939
_refine_ls_R_factor_gt           0.0822
_refine_ls_shift/su_max          0.030
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0509P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.2252
_reflns_number_gt                10507
_reflns_number_total             22210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja405815b_si_002_04.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4120281