Reactivity of a Lewis base supported uranium terminal imido metallocene towards small molecules
Li, Tongyu; Wang, Dongwei; Heng, Yi; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02165C

data_7713804
_publ_section_title
;
 Reactivity of a Lewis base supported uranium terminal imido metallocene
 towards small molecules
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02165C
_journal_year                    2023
_chemical_formula_moiety         'C41 H68 S2 Si6 U, C3 H7'
_chemical_formula_sum            'C44 H75 S2 Si6 U'
_chemical_formula_weight         1074.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                76.998(2)
_cell_angle_beta                 81.201(3)
_cell_angle_gamma                80.413(4)
_cell_formula_units_Z            2
_cell_length_a                   10.8797(5)
_cell_length_b                   10.9007(4)
_cell_length_c                   22.5081(5)
_cell_measurement_reflns_used    15056
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7060
_cell_measurement_theta_min      4.1420
_cell_volume                     2546.02(16)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    107.00 149.00   0.50    0.06    --  104.75  45.00 -30.00   84
  2  \w     83.00 120.00   0.50    0.06    --  104.75  91.00 -78.00   74
  3  \w     92.00 164.00   0.50    0.06    --  104.75  30.00-120.00  144
  4  \w     97.00 154.00   0.50    0.06    --  104.75  45.00-180.00  114
  5  \w    -68.00 -32.00   0.50    0.06    -- -102.00  61.00 -60.00   72
  6  \w    -40.00  -9.00   0.50    0.05    --  -46.63  37.00 -90.00   62
  7  \w    -36.00  17.00   0.50    0.05    --  -46.63  37.00-150.00  106
  8  \w    -20.00  19.00   0.50    0.05    --  -46.63  19.00-180.00   78
  9  \w    -64.00 -29.00   0.50    0.06    -- -102.00  61.00 -30.00   70
 10  \w    -68.00 -39.00   0.50    0.06    -- -102.00  61.00 120.00   58
 11  \w    -60.00 -30.00   0.50    0.06    -- -102.00 125.00  30.00   60
 12  \w   -117.00 -77.00   0.50    0.06    -- -102.00 125.00  30.00   80
 13  \w   -110.00 -29.00   0.50    0.06    -- -102.00 125.00 -30.00  162
 14  \w   -104.00 -79.00   0.50    0.06    -- -102.00  91.00 -78.00   50
 15  \w    -90.00 -51.00   0.50    0.06    -- -102.00 125.00 -60.00   78
 16  \w   -117.00 -50.00   0.50    0.06    -- -102.00 125.00-180.00  134
 17  \w    -56.00  18.00   0.50    0.05    --  -46.63  91.00 -78.00  148
 18  \w     54.00  79.00   0.50    0.06    --  104.75 -77.00 150.00   50
 19  \w     33.00  72.00   0.50    0.06    --  104.75 -61.00 150.00   78
 20  \w     34.00  72.00   0.50    0.06    --  104.75 -61.00  90.00   76
 21  \w     83.00 108.00   0.50    0.06    --  104.75 -77.00 -60.00   50
 22  \w     51.00  76.00   0.50    0.06    --  104.75 -77.00 -60.00   50
 23  \w     35.00  73.00   0.50    0.06    --  104.75 -61.00-120.00   76
 24  \w    -22.00   6.00   0.50    0.05    --   46.63 -19.00 -90.00   56
 25  \w    -27.00  27.00   0.50    0.05    --   46.63 -19.00   0.00  108
 26  \w     37.00 115.00   0.50    0.06    --  104.75-125.00 150.00  156
 27  \w     35.00  78.00   0.50    0.06    --  104.75 -91.00 167.00   86
 28  \w     35.00  96.00   0.50    0.06    --  104.75 -94.00  60.00  122
 29  \w     46.00 108.00   0.50    0.06    --  104.75 -94.00-180.00  124
 30  \w     47.00  72.00   0.50    0.06    --  104.75-125.00 -60.00   50
 31  \w     77.00 113.00   0.50    0.06    --  104.75-125.00 -60.00   72
 32  \w     -8.00  68.00   0.50    0.05    --   46.63 -91.00 167.00  152
 33  \w   -165.00-117.00   0.50    0.06    -- -102.00 -45.00  60.00   96
 34  \w   -133.00 -91.00   0.50    0.06    -- -102.00 -15.00 120.00   84
 35  \w   -173.00-138.00   0.50    0.06    -- -102.00 -15.00 120.00   70
 36  \w   -174.00-132.00   0.50    0.06    -- -102.00 -45.00 -60.00   84
 37  \w   -112.00 -71.00   0.50    0.05    --  -46.63-125.00 -60.00   82
 38  \w   -106.00 -76.00   0.50    0.05    --  -46.63-125.00 -90.00   60
 39  \w   -173.00 -71.00   0.50    0.06    -- -102.00-125.00-120.00  204
 40  \w   -170.00-135.00   0.50    0.06    -- -102.00 -94.00 -90.00   70
 41  \w   -124.00 -82.00   0.50    0.06    -- -102.00 -94.00 -90.00   84
 42  \w   -174.00 -77.00   0.50    0.06    -- -102.00 -91.00 167.00  194
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0953732000
_diffrn_orient_matrix_UB_12      0.0553349000
_diffrn_orient_matrix_UB_13      -0.0464680000
_diffrn_orient_matrix_UB_21      0.1028273000
_diffrn_orient_matrix_UB_22      0.0642365000
_diffrn_orient_matrix_UB_23      -0.0453328000
_diffrn_orient_matrix_UB_31      0.0354078000
_diffrn_orient_matrix_UB_32      -0.1193985000
_diffrn_orient_matrix_UB_33      -0.0281588000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1308
_diffrn_reflns_av_unetI/netI     0.1153
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30768
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.211
_diffrn_reflns_theta_min         4.061
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.293
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             1094
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.526
_refine_diff_density_min         -5.668
_refine_diff_density_rms         0.356
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         10092
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.205
_refine_ls_R_factor_all          0.0928
_refine_ls_R_factor_gt           0.0719
_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^)+(0.1583P)^2^+4.1820P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1905
_refine_ls_wR_factor_ref         0.2610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8175
_reflns_number_total             10092
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound8
_cod_original_cell_volume        2546.02(17)
_cod_database_code               7713804
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1U1S1Si1
_shelx_estimated_absorpt_t_max   0.282
_shelx_estimated_absorpt_t_min   0.211
_diffrn_oxdiff_digest_frames
;
0131814575d3a4ad11ab681184393beec4039085585
;
_diffrn_oxdiff_digest_hkl
;
0144e2f08e0520b9371ab3951844aba80c9b94
;
_reflns_odcompleteness_completeness 99.22
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq, Uanis(C19) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C26) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 C43(H43A,H43B), C44(H44A,H44B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,
 H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C42(H42A,H42B,H42C)
;
_shelx_res_checksum              81858
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 3.910
_oxdiff_exptl_absorpt_empirical_full_min 0.554