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_1543284
_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_formula_sum            'C51.5 H112 K2 O16 S Si4 U'
_chemical_formula_weight         1448.05
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_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                76.530(4)
_cell_angle_beta                 74.270(4)
_cell_angle_gamma                65.093(4)
_cell_formula_units_Z            2
_cell_length_a                   13.2622(7)
_cell_length_b                   15.3715(6)
_cell_length_c                   20.3762(10)
_cell_measurement_reflns_used    8308
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.2760
_cell_measurement_theta_min      3.2490
_cell_volume                     3592.7(3)
_computing_cell_refinement
;
Agilent Technologies, (2013), CrysAlisPro Software system, 
version 1.171. 36.28, 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. 36.28, 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 0.997
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega   -4.00   96.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       25.8739   77.0000 -180.0000 100

  2 omega  -98.00    3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -77.0000 -120.0000 101

  3 omega  -98.00    3.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364  -77.0000  -30.0000 101

  4 omega  -57.00   43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364   77.0000   90.0000 100

  5 omega  -53.00   39.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.4364   37.0000  -60.0000 92

;
_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  0.0499
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            43383
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.231
_exptl_absorpt_coefficient_mu    2.525
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82891
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent intense green'
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1502
_exptl_crystal_size_max          0.800
_exptl_crystal_size_mid          0.700
_exptl_crystal_size_min          0.600
_refine_diff_density_max         2.712
_refine_diff_density_min         -2.218
_refine_diff_density_rms         0.131
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1017
_refine_ls_number_reflns         21655
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0637
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0233P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0785
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17658
_reflns_number_total             21655
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00675b2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 1543284--1543292.cif.'
_cod_original_cell_volume        3592.8(3)
_cod_original_formula_sum        'C51.50 H112 K2 O16 S Si4 U'
_cod_database_code               1543284
_shelx_estimated_absorpt_t_min   0.237
_shelx_estimated_absorpt_t_max   0.313
_shelxl_version_number           2013-4
_shelx_res_checksum              85169