CO2 conversion to isocyanate via multiple N-Si bond cleavage at a bulky uranium(III) complex
Clement Camp; Lucile Chatelain; Christos E. Kefalidis; Jacques Pecaut; Laurent Maron; Marinella Mazzanti; Chem.Commun. 51 (2015) 15454–; doi:10.1039/C5cc06707C

data_7117930
_publ_section_title
;
 CO2 conversion to isocyanate via multiple N-Si bond cleavage at a bulky
 uranium(III) complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              15454
_journal_paper_doi               10.1039/C5cc06707C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C32 H78 K N5 O8 Si6 U'
_chemical_formula_weight         1106.66
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-08-05 deposited with the CCDC.
2015-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.687(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.5823(2)
_cell_length_b                   17.9907(5)
_cell_length_c                   14.1292(3)
_cell_measurement_reflns_used    15568
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.3680
_cell_measurement_theta_min      3.6300
_cell_volume                     2735.76(11)
_computing_cell_refinement
;
Agilent Technologies, (2014), CrysAlisPro Software system, 
version 1.171. 37.35, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_data_collection
;
Agilent Technologies, (2014), CrysAlisPro Software system, 
version 1.171.37.35, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_data_reduction
;
Agilent Technologies, (2014), CrysAlisPro Software system, 
version 1.171. 37.35, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_molecular_graphics
;
Mercury 3.5 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
;
SHELXL-2013 
(Sheldrick, Acta Cryst. A64, 112-122)
;
_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 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega    8.00   81.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614 -124.0000   30.0000 73

  2 omega  -49.00   42.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   57.0000  -90.0000 91

  3 omega  -27.00   36.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801   57.0000   60.0000 63

  4 omega  -97.00    3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000  -90.0000 100

  5 omega  -84.00  -21.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  124.0000  110.0000 63

  6 omega  -71.00    3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000  150.0000 74

  7 omega  -84.00   28.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801    0.0000 -120.0000 112

  8 omega  -78.00    3.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -77.0000   30.0000 81

  9 omega  -96.00   10.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -19.0000   90.0000 106

 10 omega    0.00   74.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614   37.0000 -150.0000 74

 11 omega -103.00  -34.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801 -179.0000   30.0000 69

 12 omega  -96.00   -6.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801  -57.0000   60.0000 90

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            67035
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.521
_exptl_absorpt_coefficient_mu    3.216
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76424
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent colourless'
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.371
_exptl_crystal_size_min          0.246
_refine_diff_density_max         1.274
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     466
_refine_ls_number_reflns         8579
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.9876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0673
_refine_ls_wR_factor_ref         0.0718
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                7176
_reflns_number_total             8579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc06707c2.cif
_cod_data_source_block           cc720_2
_cod_original_cell_volume        2735.75(11)
_cod_database_code               7117930
_shelx_estimated_absorpt_t_min   0.307
_shelx_estimated_absorpt_t_max   0.505
_shelxl_version_number           2013-4
_shelx_res_checksum              67244
_shelx_hkl_checksum              93001