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_7713805
_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         'C56 H82 N2 O2 Si6 U, C3 H3'
_chemical_formula_sum            'C59 H85 N2 O2 Si6 U'
_chemical_formula_weight         1260.85
_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             2022-12-14
_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                95.9330(10)
_cell_angle_beta                 99.850(2)
_cell_angle_gamma                110.413(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5856(2)
_cell_length_b                   12.8140(3)
_cell_length_c                   22.9235(3)
_cell_measurement_reflns_used    22220
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2470
_cell_measurement_theta_min      3.7540
_cell_volume                     3093.08(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.961
_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     34.00 117.00   0.50    0.05    --   46.91  60.00 115.00  166
  2  \w    110.00 162.00   0.50    0.06    --  104.75  60.00 115.00  104
  3  \w    140.00 166.00   0.50    0.06    --  104.75  45.00  30.00   52
  4  \w     98.00 124.00   0.50    0.06    --  104.75  45.00  30.00   52
  5  \w    108.00 136.00   0.50    0.06    --  104.75  30.00 -60.00   56
  6  \w    152.00 177.00   0.50    0.06    --  104.75  45.00-180.00   50
  7  \w     93.00 177.00   0.50    0.06    --  104.75  30.00-180.00  168
  8  \w     97.00 123.00   0.50    0.06    --  104.75  45.00-180.00   52
  9  \w     -8.00  25.00   0.50    0.05    --  -46.91  37.00  90.00   66
 10  \w    -34.00  24.00   0.50    0.05    --  -46.91  60.00 115.00  116
 11  \w    -67.00 -31.00   0.50    0.06    -- -102.00  61.00 150.00   72
 12  \w    -68.00 -31.00   0.50    0.06    -- -102.00  60.00 115.00   74
 13  \w    -57.00 -31.00   0.50    0.06    -- -102.00  61.00-120.00   52
 14  \w    -68.00 -33.00   0.50    0.06    -- -102.00  77.00-150.00   70
 15  \w   -100.00 -71.00   0.50    0.06    -- -102.00  77.00-150.00   58
 16  \w    -26.00  13.00   0.50    0.05    --   46.91 -19.00-180.00   78
 17  \w    -24.00  59.00   0.50    0.05    --   46.91 -60.00 -24.00  166
 18  \w     78.00 174.00   0.50    0.06    --  104.75 125.00  30.00  192
 19  \w     34.00  60.00   0.50    0.06    --  104.75 -60.00 -24.00   52
 20  \w     34.00  73.00   0.50    0.06    --  104.75 -61.00 -90.00   78
 21  \w     39.00  65.00   0.50    0.06    --  104.75 -77.00  30.00   52
 22  \w     34.00  73.00   0.50    0.06    --  104.75 -61.00 150.00   78
 23  \w     35.00 107.00   0.50    0.06    --  104.75 -94.00 150.00  144
 24  \w     50.00 116.00   0.50    0.06    --  104.75-125.00 150.00  132
 25  \w     45.00  87.00   0.50    0.05    --   46.91-125.00 120.00   84
 26  \w     18.00  95.00   0.50    0.05    --   46.91-125.00  30.00  154
 27  \w     32.00 117.00   0.50    0.06    --  104.75-125.00  30.00  170
 28  \w     43.00 100.00   0.50    0.06    --  104.75 -94.00  60.00  114
 29  \w     55.00  89.00   0.50    0.06    --  104.75 -94.00  90.00   68
 30  \w     87.00 117.00   0.50    0.06    --  104.75-125.00 -30.00   60
 31  \w     60.00  86.00   0.50    0.06    --  104.75-125.00 -30.00   52
 32  \w     39.00  66.00   0.50    0.06    --  104.75 -94.00 -90.00   54
 33  \w     81.00 116.00   0.50    0.06    --  104.75-125.00-150.00   70
 34  \w     83.00 109.00   0.50    0.06    --  104.75 -94.00 -90.00   52
 35  \w     56.00 104.00   0.50    0.06    --  104.75 -94.00   0.00   96
 36  \w   -117.00 -31.00   0.50    0.05    --  -46.91 -60.00 -24.00  172
 37  \w   -173.00 -86.00   0.50    0.06    -- -102.00 -60.00 -24.00  174
 38  \w   -172.00-106.00   0.50    0.06    -- -102.00 -45.00  30.00  132
 39  \w   -111.00 -78.00   0.50    0.05    --  -46.91-125.00  90.00   66
 40  \w   -142.00 -71.00   0.50    0.06    -- -102.00-125.00 120.00  142
 41  \w   -174.00-148.00   0.50    0.06    -- -102.00-125.00 120.00   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      0.0525005000
_diffrn_orient_matrix_UB_12      -0.0765627000
_diffrn_orient_matrix_UB_13      -0.0343604000
_diffrn_orient_matrix_UB_21      0.0577687000
_diffrn_orient_matrix_UB_22      0.0950108000
_diffrn_orient_matrix_UB_23      -0.0346256000
_diffrn_orient_matrix_UB_31      0.1228112000
_diffrn_orient_matrix_UB_32      0.0457877000
_diffrn_orient_matrix_UB_33      0.0492214000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0783
_diffrn_reflns_av_unetI/netI     0.0775
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            41774
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.593
_diffrn_reflns_theta_min         3.739
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.802
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89311
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       block
_exptl_crystal_F_000             1290
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.815
_refine_diff_density_min         -1.778
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       0.00025(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         12507
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0488
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0285P)^2^+3.6671P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0994
_refine_ls_wR_factor_ref         0.1025
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11092
_reflns_number_total             12507
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound10
_cod_database_code               7713805
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1O1Si1U1
_diffrn_oxdiff_digest_frames
;
01dd778abaf5bd42801f97b8799f1138b1038924a85
;
_diffrn_oxdiff_digest_hkl
;
01965427d414c5f7b9fc523298728eba0edf14
;
_reflns_odcompleteness_completeness 99.93
_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), C31(H31), C32(H32), C33(H33), C34(H34),
 C35(H35), C37(H37), C38(H38), C40(H40), C41(H41), C45(H45), C46(H46), C47(H47),
  C48(H48), C49(H49), C51(H51), C52(H52), C54(H54), C55(H55), C57(H57),
 C58(H58), C59(H59)
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), C42(H42A,H42B,H42C),
 C56(H56A,H56B,H56C)
;
_shelx_res_checksum              80422
_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 1.261
_oxdiff_exptl_absorpt_empirical_full_min 0.847