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_7713803
_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         'C51 H75 N Si6 U'
_chemical_formula_sum            'C51 H75 N Si6 U'
_chemical_formula_weight         1108.69
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-06-02
_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                81.1320(10)
_cell_angle_beta                 80.211(2)
_cell_angle_gamma                61.361(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9779(3)
_cell_length_b                   12.2577(2)
_cell_length_c                   21.5594(3)
_cell_measurement_reflns_used    25474
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      76.1380
_cell_measurement_theta_min      4.1150
_cell_volume                     2727.99(10)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.954
_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    -26.00  39.00   0.50    0.05    --   46.95 -37.00 -30.00  130
  2  \w     23.00  59.00   0.50    0.05    --   46.95-121.00  90.00   72
  3  \w     75.00 113.00   0.50    0.05    --  104.75-121.00  90.00   76
  4  \w     63.00  89.00   0.50    0.05    --  104.75 -77.00  90.00   52
  5  \w     41.00  68.00   0.50    0.05    --  104.75-121.00  90.00   54
  6  \w     35.00 116.00   0.50    0.05    --  104.75-125.00 150.00  162
  7  \w     32.00  73.00   0.50    0.05    --  104.75 -61.00  60.00   82
  8  \w     32.00  72.00   0.50    0.05    --  104.75 -61.00  90.00   80
  9  \w     46.00  72.00   0.50    0.05    --  104.75 -77.00 -30.00   52
 10  \w     65.00 107.00   0.50    0.05    --  104.75 -77.00 -90.00   84
 11  \w     83.00 121.00   0.50    0.05    --  104.75-151.00 -69.00   76
 12  \w     68.00  94.00   0.50    0.05    --   46.95-151.00 -69.00   52
 13  \w     32.00 105.00   0.50    0.05    --  104.75 -94.00-150.00  146
 14  \w     32.00  95.00   0.50    0.05    --  104.75 -77.00-120.00  126
 15  \w     33.00  72.00   0.50    0.05    --  104.75 -61.00 -60.00   78
 16  \w     94.00 176.00   0.50    0.05    --  104.75  45.00-150.00  164
 17  \w    131.00 170.00   0.50    0.05    --  104.75 125.00 -90.00   78
 18  \w     90.00 115.00   0.50    0.05    --  104.75 151.00 -26.00   50
 19  \w     85.00 114.00   0.50    0.05    --  104.75 125.00 -90.00   58
 20  \w     58.00  84.00   0.50    0.05    --   46.95 151.00 -26.00   52
 21  \w    141.00 166.00   0.50    0.05    --  104.75 125.00 120.00   50
 22  \w     92.00 127.00   0.50    0.05    --  104.75 121.00 172.00   70
 23  \w     87.00 122.00   0.50    0.05    --  104.75 125.00 120.00   70
 24  \w     82.00 178.00   0.50    0.05    --  104.75  77.00 150.00  192
 25  \w    -14.00  28.00   0.50    0.05    --   46.95 -19.00-180.00   84
 26  \w    -27.00  27.00   0.50    0.05    --   46.95 -19.00 -90.00  108
 27  \w    -24.00  29.00   0.50    0.05    --  -46.95  19.00-180.00  106
 28  \w    -60.00 -33.00   0.50    0.05    -- -102.00 151.00 -26.00   54
 29  \w    -56.00 -31.00   0.50    0.05    -- -102.00 125.00 -60.00   50
 30  \w    -64.00 -32.00   0.50    0.05    -- -102.00  61.00  30.00   64
 31  \w    -69.00 -32.00   0.50    0.05    -- -102.00  61.00  90.00   74
 32  \w    -60.00 -35.00   0.50    0.05    -- -102.00  61.00 150.00   50
 33  \w    -78.00 -15.00   0.50    0.05    --  -46.95 121.00 172.00  126
 34  \w   -103.00 -32.00   0.50    0.05    -- -102.00 121.00 172.00  142
 35  \w   -101.00 -65.00   0.50    0.05    --  -46.95 151.00 -26.00   72
 36  \w    -97.00 -59.00   0.50    0.05    --  -46.95-151.00 -69.00   76
 37  \w   -107.00 -81.00   0.50    0.05    --  -46.95-125.00-180.00   52
 38  \w   -136.00-111.00   0.50    0.05    -- -102.00-151.00 -69.00   50
 39  \w   -115.00 -86.00   0.50    0.05    -- -102.00 -61.00 -60.00   58
 40  \w   -139.00 -92.00   0.50    0.05    -- -102.00 -45.00-180.00   94
 41  \w   -155.00-130.00   0.50    0.05    -- -102.00 -61.00 -60.00   50
 42  \w   -171.00 -88.00   0.50    0.05    -- -102.00 -15.00 -90.00  166
 43  \w    -64.00 -38.00   0.50    0.05    -- -102.00  61.00 -60.00   52
 44  \w    -61.00 -32.00   0.50    0.05    -- -102.00  61.00 -90.00   58
 45  \w   -117.00 -86.00   0.50    0.05    -- -102.00 125.00 -60.00   62
 46  \w   -134.00 -90.00   0.50    0.05    -- -102.00 151.00 -26.00   88
 47  \w   -173.00 -91.00   0.50    0.05    -- -102.00 -45.00 150.00  164
 48  \w   -116.00 -91.00   0.50    0.05    -- -102.00-121.00  90.00   50
 49  \w   -115.00 -90.00   0.50    0.05    --  -46.95-125.00 150.00   50
;
_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      0.0656844000
_diffrn_orient_matrix_UB_12      0.0239289000
_diffrn_orient_matrix_UB_13      0.0481097000
_diffrn_orient_matrix_UB_21      0.0646993000
_diffrn_orient_matrix_UB_22      0.0553283000
_diffrn_orient_matrix_UB_23      -0.0540964000
_diffrn_orient_matrix_UB_31      -0.1150762000
_diffrn_orient_matrix_UB_32      0.1304554000
_diffrn_orient_matrix_UB_33      0.0073824000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0475
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            38415
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.723
_diffrn_reflns_theta_min         4.124
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.870
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.24948
_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    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         3.190
_refine_diff_density_min         -2.605
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10976
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0713P)^2^+2.7390P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1095
_refine_ls_wR_factor_ref         0.1107
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10533
_reflns_number_total             10976
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound5
_cod_database_code               7713803
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1Si1U1
_shelx_estimated_absorpt_t_max   0.319
_shelx_estimated_absorpt_t_min   0.243
_diffrn_oxdiff_digest_frames
;
013c26a1194e62e5d2068510736c1619da04106d179
;
_diffrn_oxdiff_digest_hkl
;
01e1044aa7c10ad6d42c4c0e5e578a5b77b97b
;
_reflns_odcompleteness_completeness 99.97
_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.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C30(H30), C31(H31), C33(H33), C34(H34),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C47(H47), C48(H48), C49(H49),
  C50(H50), C51(H51)
2.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), 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)
;
_shelx_res_checksum              10189
_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 3.038
_oxdiff_exptl_absorpt_empirical_full_min 0.618