Synthesis and reactivity of a terminal uranium(iv) sulfide supported by siloxide ligands
Andrez, Julie; Pécaut, Jacques; Scopelliti, Rosario; Kefalidis, Christos E.; Maron, Laurent; Rosenzweig, Michael W.; Meyer, Karsten; Mazzanti, Marinella; Chem. Sci. 7 (2016) 5846–; doi:10.1039/C6SC00675B

data_1543287
_publ_section_title
;
 Synthesis and reactivity of a terminal uranium(iv) sulfide supported by
 siloxide ligands
;
_journal_issue                   9
_journal_name_full               'Chem. Sci.'
_journal_page_first              5846
_journal_paper_doi               10.1039/C6SC00675B
_journal_volume                  7
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_sum            'C90 H198 K4 N2 O30 S3 Si6 U2'
_chemical_formula_weight         2685.67
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_symmetry_space_group_name_Hall  'P 2 2ab'
_symmetry_space_group_name_H-M   'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-01-18 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   27.6846(8)
_cell_length_b                   17.5786(4)
_cell_length_c                   14.8975(4)
_cell_measurement_reflns_used    5160
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.7800
_cell_measurement_theta_min      3.1050
_cell_volume                     7250.0(3)
_computing_cell_refinement
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171. 37.31, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_data_collection
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171.37.31, Agilent Technologies UK Ltd, Oxford, UK
;
_computing_data_reduction
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171. 37.31, Agilent Technologies UK Ltd, Oxford, UK
;
_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  'SHELXL-2013 (Sheldrick, 2013)'
_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 0.994
_diffrn_measurement_details
;
  1 omega   35.00   66.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051  178.0000   30.0000 31

  2 omega   10.00   72.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000   90.0000 62

  3 omega   15.00   63.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   37.0000 -150.0000 48

  4 omega   15.00   68.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -       25.4051   57.0000  150.0000 53

  5 omega  -76.00  -46.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000  -90.0000 30

  6 omega -104.00  -77.00   1.0000   60.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  178.0000   30.0000 27

;
_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  0.0851
_diffrn_reflns_av_unetI/netI     0.1635
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43886
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.060
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.495
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92914
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent brown'
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.231
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.063
_refine_diff_density_max         1.995
_refine_diff_density_min         -1.027
_refine_diff_density_rms         0.159
_refine_ls_abs_structure_details
; 
 Flack x determined using 4357 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.213(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     905
_refine_ls_number_reflns         21867
_refine_ls_number_restraints     317
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.1361
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0579P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                13869
_reflns_number_total             21867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00675b2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 1543284--1543292.cif.'
_cod_database_code               1543287
_shelx_estimated_absorpt_t_min   0.596
_shelx_estimated_absorpt_t_max   0.859
_shelxl_version_number           2013-4
_shelx_res_checksum              47928