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_1543289
_publ_section_title
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 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         'C48 H109 O16 S Si4 U, C12 H24 K O6, C7 H8'
_chemical_formula_sum            'C67 H141 K O22 S Si4 U'
_chemical_formula_weight         1720.34
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-09-15
_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                 95.317(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.8962(5)
_cell_length_b                   24.5807(16)
_cell_length_c                   26.1417(14)
_cell_measurement_reflns_used    3068
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.3580
_cell_measurement_theta_min      3.6010
_cell_volume                     8891.0(8)
_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
;
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 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -25.00   67.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -99.0000  150.0000 92

  2 omega   38.00  102.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  178.0000   90.0000 64

  3 omega  -62.00   39.00   1.0000  120.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239   19.0000  -60.0000 101
;
_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  0.0559
_diffrn_reflns_av_unetI/netI     0.0918
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20499
_diffrn_reflns_point_group_measured_fraction_full 0.633
_diffrn_reflns_point_group_measured_fraction_max 0.629
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.204
_exptl_absorpt_coefficient_mu    2.011
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89043
_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 pale blue'
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_description       'long plate'
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.890
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.027
_refine_diff_density_max         1.676
_refine_diff_density_min         -1.648
_refine_diff_density_rms         0.108
_refine_ls_abs_structure_details
;
 Flack x determined using 1497 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons and Flack (2004), Acta Cryst. A60, s61). 
;
_refine_ls_abs_structure_Flack   0.007(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1094
_refine_ls_number_reflns         11450
_refine_ls_number_restraints     615
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0941
_refine_ls_R_factor_gt           0.0674
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0575P)^2^+31.3252P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1322
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.262
_reflns_Friedel_fraction_full    0.271
_reflns_Friedel_fraction_max     0.262
_reflns_number_gt                8892
_reflns_number_total             11450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00675b2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 1543284--1543292.cif.'
_cod_database_code               1543289
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.948
_shelx_estimated_absorpt_t_min   0.268
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All S(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C82B-C83B = C84B-C85B = C86-C87 = C86B-C87B = O83B-C86B
 2.4 with sigma of 0.02
 O83B-C85B
 1.4 with sigma of 0.01
 C85B-C86B
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C83 \\sim O84B \\sim O82 \\sim O86 \\sim O83B \\sim O83 \\sim O82B \\sim O86B
\\sim O84 \\sim O81 \\sim O85 \\sim O85B \\sim O81B \\sim C85B \\sim C87B \\sim
C86B \\sim C82 \\sim C91 \\sim C90 \\sim C84B \\sim C84 \\sim C85 \\sim C82B
\\sim C83B \\sim C90B \\sim C91B \\sim C87 \\sim C86 \\sim C92 \\sim C81 \\sim
C88 \\sim C89 \\sim C88B \\sim C81B \\sim C92B: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
C22 \\sim C22B \\sim O22 \\sim O22B \\sim O23 \\sim O23B \\sim C28B \\sim C28
\\sim C26 \\sim C26B: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C28B) \\sim Ueq, Uanis(C103) \\sim Ueq, Uanis(C104)
\\sim Ueq, Uanis(C105) \\sim Ueq, Uanis(C22) \\sim Ueq, Uanis(C42) \\sim Ueq,
Uanis(C22B) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C50) \\sim Ueq, Uanis(C52)
\\sim Ueq, Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
4. Others
 Sof(H90C)=Sof(H90D)=Sof(O81B)=Sof(O82B)=Sof(O83B)=Sof(O84B)=Sof(O85B)=
 Sof(O86B)=Sof(C81B)=Sof(H81C)=Sof(H81D)=Sof(C82B)=Sof(H82C)=Sof(H82D)=
 Sof(C83B)=Sof(H1A)=Sof(H83C)=Sof(C84B)=Sof(H84C)=Sof(H84D)=Sof(C85B)=Sof(H85C)=
 Sof(H85D)=Sof(C86B)=Sof(H86C)=Sof(H86D)=Sof(C87B)=Sof(H87C)=Sof(H87D)=
 Sof(C88B)=Sof(H88C)=Sof(H88D)=Sof(C90B)=Sof(H90E)=Sof(H90F)=Sof(C91B)=
 Sof(H91C)=Sof(H91D)=Sof(C92B)=Sof(H92C)=Sof(H92D)=1-FVAR(1)
 Sof(O81)=Sof(O82)=Sof(O83)=Sof(O84)=Sof(O85)=Sof(O86)=Sof(C81)=Sof(H81A)=
 Sof(H81B)=Sof(C82)=Sof(H82A)=Sof(H82B)=Sof(C83)=Sof(H83A)=Sof(H83B)=Sof(C84)=
 Sof(H84A)=Sof(H84B)=Sof(C85)=Sof(H85A)=Sof(H85B)=Sof(C86)=Sof(H86A)=Sof(H86B)=
 Sof(C87)=Sof(H87A)=Sof(H87B)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(C89)=Sof(H89A)=
 Sof(H89B)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)=Sof(C92)=Sof(H92A)=
 Sof(H92B)=FVAR(1)
 Sof(O22B)=Sof(O23B)=Sof(C22B)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C26B)=
 Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=1-FVAR(2)
 Sof(O22)=Sof(O23)=Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C26)=Sof(H26A)=
 Sof(H26B)=Sof(H26C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,
 H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B), C89(H89A,H89B),
 C90(H90A,H90B), C90(H90C,H90D), C91(H91A,H91B), C92(H92A,H92B), C81B(H81C,
 H81D), C82B(H82C,H82D), C83B(H1A,H83C), C84B(H84C,H84D), C85B(H85C,H85D),
 C86B(H86C,H86D), C87B(H87C,H87D), C88B(H88C,H88D), C90B(H90E,H90F), C91B(H91C,
 H91D), C92B(H92C,H92D)
5.b Aromatic/amide H refined with riding coordinates:
 C102(H102), C103(H103), C104(H104), C105(H105), C106(H106)
5.c Fitted hexagon refined as free rotating group:
 C101(C102,C103,C104,C105,C106)
5.d Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), 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), C22B(H22D,H22E,H22F),
 C26B(H26D,H26E,H26F), C28B(H28D,H28E,H28F), C42(H42A,H42B,H42C), 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),
 C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,H70B,H70C), C71(H71A,
 H71B,H71C), C72(H72A,H72B,H72C), C107(H10D,H10E,H10F)
5.e Idealised tetrahedral OH refined as rotating group:
 S1(H1)
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