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_1543292
_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_moiety         'C72 H162 K2 O24 S4.37 Si6 U2, C7 H8'
_chemical_formula_sum            'C79 H170 K2 O24 S4.36 Si6 U2'
_chemical_formula_weight         2366.88
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-27
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_audit_update_record
;
2016-01-18 deposited with the CCDC.
2016-04-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.218(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.1455(8)
_cell_length_b                   18.0590(13)
_cell_length_c                   22.1126(12)
_cell_measurement_reflns_used    5408
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.7250
_cell_measurement_theta_min      3.5450
_cell_volume                     5644.5(6)
_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 1.171.36.28, 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
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_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 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega  -47.00   70.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -19.0000  120.0000 117

  2 omega -103.00  -35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801 -178.0000  -60.0000 68

  3 omega -103.00  -35.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.2801 -178.0000   30.0000 68
;
_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  0.0446
_diffrn_reflns_av_unetI/netI     0.0784
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            34303
_diffrn_reflns_point_group_measured_fraction_full 0.998
_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         3.095
_exptl_absorpt_coefficient_mu    3.142
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.490
_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            'dark red'
_exptl_crystal_density_diffrn    1.393
_exptl_crystal_description       block
_exptl_crystal_F_000             2424
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.180
_refine_diff_density_max         1.400
_refine_diff_density_min         -1.013
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         17040
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0475
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0341P)^2^+5.6078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1055
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11962
_reflns_number_total             17040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00675b2.cif
_cod_data_source_block           ojc130
_cod_depositor_comments
'Adding full bibliography for 1543284--1543292.cif.'
_cod_database_code               1543292
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.602
_shelx_estimated_absorpt_t_min   0.532
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C62-C67 = C66-C67
 2.5 with sigma of 0.02
 C61-C67
 1.52 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C61) \\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64)
\\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq:
with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C6) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C26)
\\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(C22) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(S1B)=Sof(S2B)=Sof(S3B)=1-FVAR(1)
 Sof(S1)=Sof(S2)=FVAR(1)
 Fixed Sof: C61(0.5) C62(0.5) H62(0.5) C63(0.5) H63(0.5) C64(0.5) H64(0.5)
 C65(0.5) H65(0.5) C66(0.5) H66(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5)
5.a Rotating group:
 C52(C61,C62), C62(C63), C63(C64), C64(C65), C65(C66)
5.b Aromatic/amide H refined with riding coordinates:
 C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H1B,H3A,H3B), C4(H4A,H4B,H4C), C6(H6A,H6B,H6C), C7(H7A,
 H7B,H7C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C42(H1A,H42A,H42B), C43(H43A,
 H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C),
 C48(H48A,H48B,H48C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C), C67(H67A,H67B,H67C)
;