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_1543291
_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         'C48 H108 K2 O16 S2 Si4 U, C7 H8'
_chemical_formula_sum            'C55 H116 K2 O16 S2 Si4 U'
_chemical_formula_weight         1526.18
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-26
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.2882(5)
_cell_length_b                   19.3780(5)
_cell_length_c                   40.5378(9)
_cell_measurement_reflns_used    13392
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.2600
_cell_measurement_theta_min      3.6210
_cell_volume                     15151.7(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
;
_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 0.999
_diffrn_measurement_details
;
  1 omega  -44.00   47.50   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5614  -37.0000  -30.0000 122

  2 omega  -96.00   -6.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -57.0000  120.0000 120

  3 omega  -97.00  -31.00   0.7500   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1239  -77.0000  -30.0000 88
;
_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  0.0718
_diffrn_reflns_av_unetI/netI     0.0759
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            89393
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         3.324
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78570
_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 pale yellow'
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.171
_exptl_crystal_size_min          0.018
_refine_diff_density_max         2.555
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         23090
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.1090
_refine_ls_R_factor_gt           0.0550
_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^)+(0.0293P)^2^+37.6122P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14501
_reflns_number_total             23090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6sc00675b2.cif
_cod_data_source_block           ojc115
_cod_depositor_comments
'Adding full bibliography for 1543284--1543292.cif.'
_cod_database_code               1543291
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.958
_shelx_estimated_absorpt_t_min   0.542
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2A(0.153) H2B(0.153) H2C(0.153) H3A(0.148) H3B(0.148) H3C(0.148)
 H4A(0.104) H4B(0.104) H4C(0.104) H6A(0.1) H6B(0.1) H6C(0.1) H7A(0.088)
 H7B(0.088) H7C(0.088) H8A(0.073) H8B(0.073) H8C(0.073) H10A(0.121) H10B(0.121)
 H10C(0.121) H11A(0.095) H11B(0.095) H11C(0.095) H12A(0.082) H12B(0.082)
 H12C(0.082) H22A(0.133) H22B(0.133) H22C(0.133) H23A(0.137) H23B(0.137)
 H23C(0.137) H24A(0.135) H24B(0.135) H24C(0.135) H26A(0.115) H26B(0.115)
 H26C(0.115) H27A(0.072) H27B(0.072) H27C(0.072) H27D(0.072) H27E(0.072)
 H27F(0.072) H28A(0.109) H28B(0.109) H28C(0.109) H30D(0.119) H30E(0.119)
 H30F(0.119) H31D(0.146) H31E(0.146) H31F(0.146) H32A(0.153) H32B(0.153)
 H32C(0.153) H30A(0.13) H30B(0.13) H30C(0.13) H31A(0.142) H31B(0.142)
 H31C(0.142) H42A(0.157) H42B(0.157) H42C(0.157) H43A(0.138) H43B(0.138)
 H43C(0.138) H44A(0.145) H44B(0.145) H44C(0.145) H46A(0.079) H46B(0.079)
 H46C(0.079) H47A(0.077) H47B(0.077) H47C(0.077) H48A(0.08) H48B(0.08)
 H48C(0.08) H50A(0.115) H50B(0.115) H50C(0.115) H51A(0.1) H51B(0.1) H51C(0.1)
 H52A(0.146) H52B(0.146) H52C(0.146) H62A(0.077) H62B(0.077) H62C(0.077)
 H63A(0.071) H63B(0.071) H63C(0.071) H64A(0.063) H64B(0.063) H64C(0.063)
 H66A(0.079) H66B(0.079) H66C(0.079) H67A(0.145) H67B(0.145) H67C(0.145)
 H68A(0.125) H68B(0.125) H68C(0.125) H70A(0.084) H70B(0.084) H70C(0.084)
 H71A(0.078) H71B(0.078) H71C(0.078) H72A(0.082) H72B(0.082) H72C(0.082)
 H82(0.137) H83(0.144) H84(0.159) H85(0.162) H86(0.143) H87A(0.206) H87B(0.206)
 H87C(0.206) H82B(0.16) H83B(0.153) H84B(0.138) H85B(0.14) H86B(0.142)
 H87D(0.24) H87E(0.24) H87F(0.24)
 Fixed X: H2A(0.561) H2B(0.6131) H2C(0.6417) H3A(0.6942) H3B(0.6969)
 H3C(0.7265) H4A(0.6204) H4B(0.5687) H4C(0.6505) H6A(0.7046) H6B(0.6376)
 H6C(0.6655) H7A(0.6215) H7B(0.6948) H7C(0.6585) H8A(0.522) H8B(0.5166)
 H8C(0.5548) H10A(0.4611) H10B(0.4336) H10C(0.3796) H11A(0.381) H11B(0.3729)
 H11C(0.3244) H12A(0.4034) H12B(0.444) H12C(0.3627) H22A(0.5273) H22B(0.5583)
 H22C(0.5927) H23A(0.668) H23B(0.7128) H23C(0.7038) H24A(0.668) H24B(0.5933)
 H24C(0.6569) H26A(0.6922) H26B(0.6367) H26C(0.7176) H27A(0.6716) H27B(0.7082)
 H27C(0.6272) H27D(0.6402) H27E(0.7202) H27F(0.6649) H28A(0.7959) H28B(0.7664)
 H28C(0.77) H30D(0.4833) H30E(0.4848) H30F(0.4358) H31D(0.6473) H31E(0.6002)
 H31F(0.6177) H32A(0.5065) H32B(0.5251) H32C(0.4562) H30A(0.5699) H30B(0.5223)
 H30C(0.4888) H31A(0.6523) H31B(0.6289) H31C(0.622) H42A(0.3861) H42B(0.307)
 H42C(0.345) H43A(0.4594) H43B(0.476) H43C(0.4371) H44A(0.2791) H44B(0.3393)
 H44C(0.3135) H46A(0.4293) H46B(0.401) H46C(0.414) H47A(0.2803) H47B(0.2304)
 H47C(0.2921) H48A(0.2731) H48B(0.3525) H48C(0.333) H50A(0.2428) H50B(0.2612)
 H50C(0.1835) H51A(0.2357) H51B(0.1843) H51C(0.1553) H52A(0.1389) H52B(0.1685)
 H52C(0.1133) H62A(0.3023) H62B(0.2633) H62C(0.3282) H63A(0.4558) H63B(0.4206)
 H63C(0.4506) H64A(0.3195) H64B(0.3961) H64C(0.3845) H66A(0.3372) H66B(0.2692)
 H66C(0.2722) H67A(0.1648) H67B(0.1605) H67C(0.1606) H68A(0.2661) H68B(0.3327)
 H68C(0.2633) H70A(0.1735) H70B(0.1992) H70C(0.1181) H71A(0.1009) H71B(0.1091)
 H71C(0.0576) H72A(0.19) H72B(0.1502) H72C(0.1077) H82(0.4925) H83(0.4988)
 H84(0.4368) H85(0.3939) H86(0.3869) H87A(0.4209) H87B(0.4229) H87C(0.4937)
 H82B(0.368) H83B(0.3342) H84B(0.384) H85B(0.4684) H86B(0.4927) H87D(0.5219)
 H87E(0.4757) H87F(0.4522)
 Fixed Y: H2A(0.2613) H2B(0.3252) H2C(0.2509) H3A(0.3326) H3B(0.2722)
 H3C(0.2591) H4A(0.17) H4B(0.1655) H4C(0.1574) H6A(0.2996) H6B(0.3441)
 H6C(0.2862) H7A(0.1445) H7B(0.183) H7C(0.1582) H8A(0.2831) H8B(0.2042)
 H8C(0.2235) H10A(0.1142) H10B(0.0905) H10C(0.1079) H11A(0.1745) H11B(0.2536)
 H11C(0.196) H12A(0.2886) H12B(0.235) H12C(0.2254) H22A(0.5982) H22B(0.6585)
 H22C(0.6419) H23A(0.6422) H23B(0.5741) H23C(0.6308) H24A(0.4824) H24B(0.4886)
 H24C(0.5331) H26A(0.5704) H26B(0.509) H26C(0.4923) H27A(0.4435) H27B(0.4104)
 H27C(0.4283) H27D(0.428) H27E(0.417) H27F(0.4308) H28A(0.507) H28B(0.5283)
 H28C(0.5843) H30D(0.6416) H30E(0.7221) H30F(0.6946) H31D(0.7212) H31E(0.7479)
 H31F(0.6675) H32A(0.7971) H32B(0.7616) H32C(0.7396) H30A(0.6626) H30B(0.7301)
 H30C(0.6574) H31A(0.6986) H31B(0.7308) H31C(0.7755) H42A(0.3042) H42B(0.3291)
 H42C(0.3198) H43A(0.4597) H43B(0.382) H43C(0.3968) H44A(0.4511) H44B(0.5009)
 H44C(0.4378) H46A(0.5723) H46B(0.5846) H46C(0.649) H47A(0.6266) H47B(0.6349)
 H47C(0.6887) H48A(0.6066) H48B(0.5854) H48C(0.6629) H50A(0.286) H50B(0.3356)
 H50C(0.3086) H51A(0.4557) H51B(0.4872) H51C(0.4354) H52A(0.411) H52B(0.3342)
 H52C(0.3518) H62A(0.2919) H62B(0.2533) H62C(0.2175) H63A(0.3371) H63B(0.3297)
 H63C(0.263) H64A(0.2466) H64B(0.2766) H64C(0.2077) H66A(0.5622) H66B(0.5339)
 H66C(0.6121) H67A(0.509) H67B(0.5228) H67C(0.5863) H68A(0.5737) H68B(0.5926)
 H68C(0.6371) H70A(0.2504) H70B(0.2429) H70C(0.2423) H71A(0.4187) H71B(0.3549)
 H71C(0.3494) H72A(0.3434) H72B(0.4116) H72C(0.3422) H82(-0.0598) H83(-0.0659)
 H84(0.0236) H85(0.1171) H86(0.1179) H87A(0.0705) H87B(-0.0121) H87C(0.0309)
 H82B(0.076) H83B(0.1397) H84B(0.1167) H85B(0.0284) H86B(-0.0412) H87D(0.0059)
 H87E(-0.0626) H87F(0.0051)
 Fixed Z: H2A(0.7335) H2B(0.7307) H2C(0.7412) H3A(0.6843) H3B(0.6574)
 H3C(0.6938) H4A(0.6634) H4B(0.6942) H4C(0.6997) H6A(0.5747) H6B(0.5654)
 H6C(0.5405) H7A(0.5956) H7B(0.5943) H7C(0.5608) H8A(0.5619) H8B(0.5733)
 H8C(0.5394) H10A(0.6776) H10B(0.6421) H10C(0.6709) H11A(0.6051) H11B(0.6157)
 H11C(0.6321) H12A(0.6735) H12B(0.6965) H12C(0.69) H22A(0.7395) H22B(0.7168)
 H22C(0.7519) H23A(0.688) H23B(0.6947) H23C(0.7232) H24A(0.7289) H24B(0.7458)
 H24C(0.7597) H26A(0.5737) H26B(0.5731) H26C(0.5695) H27A(0.6545) H27B(0.6228)
 H27C(0.6219) H27D(0.6293) H27E(0.6203) H27F(0.5916) H28A(0.6166) H28B(0.6521)
 H28C(0.6231) H30D(0.597) H30E(0.5882) H30F(0.6172) H31D(0.6261) H31E(0.5962)
 H31F(0.5996) H32A(0.6374) H32B(0.672) H32C(0.6527) H30A(0.5897) H30B(0.5878)
 H30C(0.5976) H31A(0.6271) H31B(0.6618) H31C(0.6287) H42A(0.7435) H42B(0.7421)
 H42C(0.777) H43A(0.7693) H43B(0.7584) H43C(0.7926) H44A(0.7553) H44B(0.7684)
 H44C(0.7907) H46A(0.6913) H46B(0.7279) H46C(0.704) H47A(0.7361) H47B(0.7048)
 H47C(0.7107) H48A(0.6491) H48B(0.6439) H48C(0.6538) H50A(0.6635) H50B(0.6332)
 H50C(0.6382) H51A(0.635) H51B(0.6621) H51C(0.6346) H52A(0.7057) H52B(0.7092)
 H52C(0.681) H62A(0.4673) H62B(0.4968) H62C(0.4792) H63A(0.5089) H63B(0.4733)
 H63C(0.4917) H64A(0.5526) H64B(0.5575) H64C(0.5365) H66A(0.5752) H66B(0.5934)
 H66C(0.5808) H67A(0.563) H67B(0.5241) H67C(0.5493) H68A(0.4951) H68B(0.5168)
 H68C(0.5204) H70A(0.5789) H70B(0.5415) H70C(0.5498) H71A(0.5714) H71B(0.5962)
 H71C(0.5653) H72A(0.5031) H72B(0.5147) H72C(0.5078) H82(0.4062) H83(0.4593)
 H84(0.49) H85(0.4631) H86(0.4048) H87A(0.3537) H87B(0.3538) H87C(0.3539)
 H82B(0.4654) H83B(0.4192) H84B(0.3676) H85B(0.3625) H86B(0.4082) H87D(0.4702)
 H87E(0.472) H87F(0.4917)
;