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_7713810
_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 H79 N3 Si6 U'
_chemical_formula_sum            'C51 H79 N3 Si6 U'
_chemical_formula_weight         1140.74
_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
_audit_creation_date             2021-04-21
_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                69.8910(8)
_cell_angle_beta                 73.7899(9)
_cell_angle_gamma                85.9991(8)
_cell_formula_units_Z            4
_cell_length_a                   15.71148(17)
_cell_length_b                   17.09461(16)
_cell_length_c                   23.34218(17)
_cell_measurement_reflns_used    48735
_cell_measurement_temperature    100.03(18)
_cell_measurement_theta_max      76.1270
_cell_measurement_theta_min      3.6770
_cell_volume                     5650.67(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  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.03(18)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_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     36.00 177.00   0.50    0.05    --  104.75   0.00 150.00  282
  2  \w     39.00 177.00   0.50    0.05    --  104.75   0.00   0.00  276
  3  \w    114.00 164.00   0.50    0.05    --  104.75  45.00-180.00  100
  4  \w     27.00  95.00   0.50    0.05    --   46.95-127.00   1.00  136
  5  \w     42.00 116.00   0.50    0.05    --  104.75-125.00  60.00  148
  6  \w     41.00 119.00   0.50    0.05    --  104.75-127.00   1.00  156
  7  \w     30.00 101.00   0.50    0.05    --   46.95-143.00-168.00  142
  8  \w     69.00 130.00   0.50    0.05    --  104.75-143.00-168.00  122
  9  \w     32.00  87.00   0.50    0.05    --  104.75 -94.00-180.00  110
 10  \w     35.00 107.00   0.50    0.05    --  104.75 -77.00-150.00  144
 11  \w     32.00  72.00   0.50    0.05    --  104.75 -61.00 -60.00   80
 12  \w     37.00  71.00   0.50    0.05    --  104.75 -61.00 -30.00   68
 13  \w    -26.00  28.00   0.50    0.05    --   46.95 -19.00-120.00  108
 14  \w     37.00  69.00   0.50    0.05    --  104.75 -61.00   0.00   64
 15  \w     37.00  67.00   0.50    0.05    --  104.75 -61.00  30.00   60
 16  \w     32.00 104.00   0.50    0.05    --  104.75 -77.00 150.00  144
 17  \w    102.00 127.00   0.50    0.05    --  104.75 127.00  77.00   50
 18  \w     67.00  92.00   0.50    0.05    --   46.95 143.00-113.00   50
 19  \w     96.00 121.00   0.50    0.05    --  104.75 143.00-113.00   50
 20  \w    -87.00 -62.00   0.50    0.05    --  -46.95 143.00-113.00   50
 21  \w   -117.00 -42.00   0.50    0.05    -- -102.00 125.00-120.00  150
 22  \w   -113.00 -57.00   0.50    0.05    -- -102.00 143.00-113.00  112
 23  \w    -76.00 -41.00   0.50    0.05    --  -46.95 127.00  77.00   70
 24  \w   -108.00 -44.00   0.50    0.05    -- -102.00 127.00  77.00  128
 25  \w    -93.00 -48.00   0.50    0.05    -- -102.00  77.00 120.00   90
 26  \w    -83.00 -58.00   0.50    0.05    -- -102.00  77.00  90.00   50
 27  \w    -89.00 -64.00   0.50    0.05    -- -102.00  77.00  30.00   50
 28  \w    -68.00 -32.00   0.50    0.05    -- -102.00  61.00 -60.00   72
 29  \w    -61.00 -35.00   0.50    0.05    -- -102.00  61.00 -90.00   52
 30  \w   -103.00 -64.00   0.50    0.05    -- -102.00  77.00-120.00   78
 31  \w    -62.00 -37.00   0.50    0.05    -- -102.00  61.00-150.00   50
 32  \w    -68.00 -40.00   0.50    0.05    -- -102.00  61.00-120.00   56
 33  \w    -23.00  29.00   0.50    0.05    --  -46.95  19.00  90.00  104
 34  \w   -119.00 -24.00   0.50    0.05    --  -46.95 -77.00 -30.00  190
 35  \w   -118.00 -70.00   0.50    0.05    --  -46.95-127.00   1.00   96
 36  \w   -138.00 -89.00   0.50    0.05    -- -102.00 -30.00  60.00   98
 37  \w   -109.00 -71.00   0.50    0.05    --  -46.95-125.00  90.00   76
 38  \w   -168.00 -93.00   0.50    0.05    -- -102.00 -30.00-150.00  150
 39  \w   -104.00 -79.00   0.50    0.05    --  -46.95-125.00 -90.00   50
 40  \w   -113.00 -75.00   0.50    0.05    --  -46.95-125.00-120.00   76
 41  \w   -113.00 -88.00   0.50    0.05    --  -46.95-143.00-168.00   50
 42  \w   -141.00-116.00   0.50    0.05    -- -102.00-143.00-168.00   50
 43  \w   -147.00-122.00   0.50    0.05    -- -102.00-127.00   1.00   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      -0.0344709000
_diffrn_orient_matrix_UB_12      0.0542009000
_diffrn_orient_matrix_UB_13      -0.0563822000
_diffrn_orient_matrix_UB_21      0.0810680000
_diffrn_orient_matrix_UB_22      -0.0220122000
_diffrn_orient_matrix_UB_23      -0.0462303000
_diffrn_orient_matrix_UB_31      -0.0517259000
_diffrn_orient_matrix_UB_32      -0.0761299000
_diffrn_orient_matrix_UB_33      0.0044162000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0513
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            82922
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.490
_diffrn_reflns_theta_min         3.713
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.555
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.12493
_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    1.341
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.326
_refine_diff_density_min         -3.081
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1142
_refine_ls_number_reflns         22813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1101
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20863
_reflns_number_total             22813
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound11
_cod_original_cell_volume        5650.68(10)
_cod_database_code               7713810
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1Si1U1
_shelx_estimated_absorpt_t_max   0.448
_shelx_estimated_absorpt_t_min   0.251
_diffrn_oxdiff_digest_frames
;
01cbedc7463cf4b17eb3396207bf4f1f6e04288f18d
;
_diffrn_oxdiff_digest_hkl
;
0127673c50453cdbe3ba5a5be09efdf465c65d
;
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H102,H2,H5A} of C102, All C(H,H) groups
 At 1.5 times of:
  {H14A,H14B,H14C} of C14, {H27A,H27B,H27C} of C27, {H60A,H60B,H60C} of C60,
  {H7A,H7B,H7C} of C7, {H59A,H59B,H59C} of C59, {H20A,H20B,H20C} of C20, {H22A,
  H22B,H22C} of C22, {H77A,H77B,H77C} of C77, {H10A,H10B,H10C} of C10, {H8A,H8B,
  H8C} of C8, {H79A,H79B,H79C} of C79, {H71A,H71B,H71C} of C71, {H35A,H35B,
  H35C} of C35, {H6A,H6B,H6C} of C6, {H78A,H78B,H78C} of C78, {H57A,H57B,H57C}
  of C57, {H63A,H63B,H63C} of C63, {H74A,H74B,H74C} of C74, {H65A,H65B,H65C} of
  C65, {H73A,H73B,H73C} of C73, {H64A,H64B,H64C} of C64, {H23A,H23B,H23C} of
  C23, {H26A,H26B,H26C} of C26, {H28A,H28B,H28C} of C28, {H21A,H21B,H21C} of
  C21, {H12A,H12B,H12C} of C12, {H72A,H72B,H72C} of C72, {H11A,H11B,H11C} of
  C11, {H76A,H76B,H76C} of C76, {H61A,H61B,H61C} of C61, {H24A,H24B,H24C} of
  C24, {H25A,H25B,H25C} of C25, {H86A,H86B,H86C} of C86, {H9A,H9B,H9C} of C9,
  {H62A,H62B,H62C} of C62, {H13A,H13B,H13C} of C13, {H58A,H58B,H58C} of C58,
  {H75A,H75B,H75C} of C75
2.a Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C88(H88A,H88B)
2.b Me refined with riding coordinates:
 C74(H74A,H74B,H74C)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C30(H30), C31(H31), C33(H33), C34(H34),
 C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C45(H45), C47(H47), C48(H48),
  C49(H49), C50(H50), C51(H51), C54(H54), C56(H56), C68(H68), C70(H70),
 C81(H81), C82(H82), C84(H84), C85(H85), C90(H90), C91(H91), C92(H92), C93(H93),
  C94(H94), C96(H96), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102)
2.d 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),
 C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,
 H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,
 H64B,H64C), C65(H65A,H65B,H65C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C),
 C73(H73A,H73B,H73C), C75(H75A,H75B,H75C), C76(H76A,H76B,H76C), C77(H77A,H77B,
 H77C), C78(H78A,H78B,H78C), C79(H79A,H79B,H79C), C86(H86A,H86B,H86C)
;
_shelx_res_checksum              85203
_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 5.531
_oxdiff_exptl_absorpt_empirical_full_min 0.523