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_7713807
_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 H70 N S Si6 U'
_chemical_formula_sum            'C41 H70 N S Si6 U'
_chemical_formula_weight         1015.61
_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             2021-03-31
_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                79.0060(10)
_cell_angle_beta                 86.4970(10)
_cell_angle_gamma                88.8810(10)
_cell_formula_units_Z            4
_cell_length_a                   11.2283(2)
_cell_length_b                   19.4707(3)
_cell_length_c                   22.7290(3)
_cell_measurement_reflns_used    37199
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1970
_cell_measurement_theta_min      3.8050
_cell_volume                     4868.61(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.958
_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     82.00 122.00   0.50    0.20    --  104.75  77.00  30.00   80
  2  \w    120.00 146.00   0.50    0.20    --  104.75  45.00  90.00   52
  3  \w     92.00 167.00   0.50    0.20    --  104.75  45.00 150.00  150
  4  \w    129.00 178.00   0.50    0.20    --  104.75  77.00  30.00   98
  5  \w    115.00 169.00   0.50    0.20    --  104.75  45.00 -90.00  108
  6  \w    113.00 178.00   0.50    0.20    --  104.75  15.00-150.00  130
  7  \w    -39.00  25.00   0.50    0.08    --  -46.95  37.00  60.00  128
  8  \w    -60.00  23.00   0.50    0.08    --  -46.95  57.00 120.00  166
  9  \w    -69.00 -44.00   0.50    0.20    -- -102.00  61.00   0.00   50
 10  \w    -68.00 -32.00   0.50    0.20    -- -102.00  61.00 120.00   72
 11  \w   -108.00 -75.00   0.50    0.20    -- -102.00 103.00 171.00   66
 12  \w    -48.00   5.00   0.50    0.08    --  -46.95 103.00 171.00  106
 13  \w    -72.00 -31.00   0.50    0.20    -- -102.00 125.00 -90.00   82
 14  \w   -117.00 -87.00   0.50    0.20    -- -102.00 125.00 -90.00   60
 15  \w   -169.00 -92.00   0.50    0.20    -- -102.00 -30.00  90.00  154
 16  \w   -164.00 -85.00   0.50    0.20    -- -102.00 -61.00 150.00  158
 17  \w   -118.00 -32.00   0.50    0.08    --  -46.95 -57.00 -90.00  172
 18  \w   -174.00 -97.00   0.50    0.20    -- -102.00 -45.00   0.00  154
 19  \w   -175.00 -82.00   0.50    0.20    -- -102.00-103.00  69.00  186
 20  \w   -113.00 -72.00   0.50    0.08    --  -46.95-125.00-120.00   82
 21  \w   -118.00 -71.00   0.50    0.08    --  -46.95-125.00-150.00   94
 22  \w     32.00  68.00   0.50    0.20    --  104.75 -61.00-180.00   72
 23  \w     73.00  99.00   0.50    0.20    --  104.75 -77.00-180.00   52
 24  \w     33.00  60.00   0.50    0.20    --  104.75 -61.00-150.00   54
 25  \w     41.00  72.00   0.50    0.20    --  104.75 -61.00 -90.00   62
 26  \w     37.00  65.00   0.50    0.20    --  104.75 -61.00 -60.00   56
 27  \w     76.00 102.00   0.50    0.20    --  104.75 -77.00  60.00   52
 28  \w    113.00 156.00   0.50    0.20    --  104.75 103.00 171.00   86
 29  \w     34.00  70.00   0.50    0.20    --  104.75 -61.00  60.00   72
 30  \w     33.00  75.00   0.50    0.20    --  104.75 -77.00  60.00   84
 31  \w    -20.00   5.00   0.50    0.08    --   46.95 -19.00-180.00   50
 32  \w     37.00  67.00   0.50    0.20    --  104.75 -94.00 -60.00   60
 33  \w     41.00 112.00   0.50    0.20    --  104.75-125.00  30.00  142
 34  \w     34.00 117.00   0.50    0.20    --  104.75-125.00 -60.00  166
 35  \w     53.00  78.00   0.50    0.08    --   46.95-125.00-180.00   50
 36  \w     64.00 106.00   0.50    0.20    --  104.75-125.00-180.00   84
 37  \w     80.00 107.00   0.50    0.20    --  104.75-125.00-150.00   54
 38  \w     47.00  73.00   0.50    0.20    --  104.75-125.00-150.00   52
 39  \w     62.00  88.00   0.50    0.20    --  104.75 -94.00-150.00   52
 40  \w     70.00  95.00   0.50    0.20    --  104.75 -94.00 -60.00   50
 41  \w     43.00 114.00   0.50    0.20    --  104.75-125.00  60.00  142
 42  \w     57.00 108.00   0.50    0.20    --  104.75-103.00  69.00  102
 43  \w     20.00  79.00   0.50    0.08    --   46.95-103.00  69.00  118
 44  \w     33.00  59.00   0.50    0.20    --  104.75 -94.00-150.00   52
;
_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      0.0536114000
_diffrn_orient_matrix_UB_12      0.0526391000
_diffrn_orient_matrix_UB_13      0.0335663000
_diffrn_orient_matrix_UB_21      -0.0015294000
_diffrn_orient_matrix_UB_22      0.0568174000
_diffrn_orient_matrix_UB_23      -0.0573111000
_diffrn_orient_matrix_UB_31      -0.1265701000
_diffrn_orient_matrix_UB_32      0.0223133000
_diffrn_orient_matrix_UB_33      0.0193016000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66554
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.077
_diffrn_reflns_theta_min         3.321
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.395
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.57032
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
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    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.011
_refine_diff_density_min         -3.436
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     939
_refine_ls_number_reflns         19740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0597
_refine_ls_R_factor_gt           0.0532
_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^)+(0.0891P)^2^+19.7205P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1530
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16916
_reflns_number_total             19740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound15
_cod_database_code               7713807
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1Si1S1U1
_shelx_estimated_absorpt_t_max   0.280
_shelx_estimated_absorpt_t_min   0.280
_diffrn_oxdiff_digest_frames
;
01ffc10b6eaad83767764482fbbdcd6bfd04112e2d4
;
_diffrn_oxdiff_digest_hkl
;
015af1643a406121ba57251824d83b4fb01612
;
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C30(H30), C31(H31), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C46(H46), C58(H58),
  C60(H60), C71(H71), C72(H72), C74(H74), C75(H75), C78(H78), C79(H79),
 C80(H80), C81(H81), C82(H82)
2.b 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), C35(H35A,H35B,H35C),
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C55(H55A,H55B,H55C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C),
 C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,
 H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C76(H76A,
 H76B,H76C)
;
_shelx_res_checksum              31958
_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 1.764
_oxdiff_exptl_absorpt_empirical_full_min 0.634