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_7713811
_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         'C49 H80 N4 S Si6 U, C6 H14'
_chemical_formula_sum            'C55 H94 N4 S Si6 U'
_chemical_formula_weight         1249.97
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-03-09
_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                96.102(2)
_cell_angle_beta                 90.987(2)
_cell_angle_gamma                111.065(2)
_cell_formula_units_Z            2
_cell_length_a                   12.1303(3)
_cell_length_b                   12.8239(3)
_cell_length_c                   21.7214(4)
_cell_measurement_reflns_used    22819
_cell_measurement_temperature    99.8(4)
_cell_measurement_theta_max      76.0620
_cell_measurement_theta_min      3.6940
_cell_volume                     3129.66(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)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.8(4)
_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 0.955
_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     82.00 143.00   0.50    0.11    --  104.75  77.00-180.00  122
  2  \w    146.00 172.00   0.50    0.11    --  104.75  77.00-180.00   52
  3  \w    110.00 142.00   0.50    0.11    --  104.75  45.00-180.00   64
  4  \w    119.00 178.00   0.50    0.11    --  104.75  30.00 -60.00  118
  5  \w     27.00 115.00   0.50    0.08    --   46.95  77.00 -90.00  176
  6  \w    -23.00  21.00   0.50    0.08    --  -46.95  19.00 -30.00   88
  7  \w    -66.00 -39.00   0.50    0.11    -- -102.00  61.00 -90.00   54
  8  \w   -100.00 -29.00   0.50    0.11    -- -102.00  77.00 -30.00  142
  9  \w    -98.00 -29.00   0.50    0.11    -- -102.00  77.00 150.00  138
 10  \w     32.00 106.00   0.50    0.08    --   46.95-154.00  57.00  148
 11  \w     76.00 114.00   0.50    0.11    --  104.75-125.00  90.00   76
 12  \w     87.00 137.00   0.50    0.11    --  104.75-154.00  57.00  100
 13  \w     25.00  87.00   0.50    0.08    --   46.95-120.00-145.00  124
 14  \w     33.00  65.00   0.50    0.11    --  104.75-120.00-145.00   64
 15  \w     69.00 111.00   0.50    0.11    --  104.75-120.00-145.00   84
 16  \w     34.00 107.00   0.50    0.11    --  104.75 -77.00   0.00  146
 17  \w     33.00  68.00   0.50    0.11    --  104.75 -61.00  60.00   70
 18  \w     32.00  73.00   0.50    0.11    --  104.75 -61.00   0.00   82
 19  \w     32.00  71.00   0.50    0.11    --  104.75 -61.00 -30.00   78
 20  \w     34.00  63.00   0.50    0.11    --  104.75 -61.00-120.00   58
 21  \w     33.00  64.00   0.50    0.11    --  104.75 -61.00-150.00   62
 22  \w    -16.00  28.00   0.50    0.08    --   46.95 -19.00 -60.00   88
 23  \w     80.00 119.00   0.50    0.11    --  104.75 120.00 -61.00   78
 24  \w     85.00 168.00   0.50    0.11    --  104.75 125.00 -30.00  166
 25  \w    143.00 178.00   0.50    0.11    --  104.75 125.00   0.00   70
 26  \w     79.00 121.00   0.50    0.11    --  104.75 125.00   0.00   84
 27  \w     83.00 112.00   0.50    0.11    --  104.75 154.00  96.00   58
 28  \w     64.00  90.00   0.50    0.08    --   46.95 154.00  96.00   52
 29  \w   -104.00 -79.00   0.50    0.08    --  -46.95 154.00  96.00   50
 30  \w   -130.00 -31.00   0.50    0.11    -- -102.00 154.00  96.00  198
 31  \w   -101.00 -30.00   0.50    0.11    -- -102.00 125.00  90.00  142
 32  \w    -74.00 -49.00   0.50    0.08    --  -46.95 120.00 -61.00   50
 33  \w   -109.00 -32.00   0.50    0.11    -- -102.00 120.00 -61.00  154
 34  \w   -167.00 -92.00   0.50    0.11    -- -102.00 -30.00 -90.00  150
 35  \w   -112.00 -74.00   0.50    0.08    --  -46.95-125.00 -90.00   76
 36  \w   -117.00 -79.00   0.50    0.08    --  -46.95-125.00 -30.00   76
 37  \w   -114.00 -51.00   0.50    0.08    --  -46.95-154.00  57.00  126
 38  \w   -166.00-100.00   0.50    0.11    -- -102.00 -45.00 120.00  132
 39  \w   -147.00 -93.00   0.50    0.11    -- -102.00 -45.00  60.00  108
 40  \w   -173.00-148.00   0.50    0.11    -- -102.00 -94.00 -30.00   50
 41  \w   -135.00-110.00   0.50    0.11    -- -102.00-120.00-145.00   50
 42  \w   -128.00 -98.00   0.50    0.11    -- -102.00 -94.00 -30.00   60
 43  \w   -110.00 -85.00   0.50    0.11    -- -102.00-154.00  57.00   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      -0.1164130000
_diffrn_orient_matrix_UB_12      0.0160960000
_diffrn_orient_matrix_UB_13      0.0163087000
_diffrn_orient_matrix_UB_21      0.0279591000
_diffrn_orient_matrix_UB_22      -0.0033144000
_diffrn_orient_matrix_UB_23      0.0690566000
_diffrn_orient_matrix_UB_31      0.0652319000
_diffrn_orient_matrix_UB_32      0.1286353000
_diffrn_orient_matrix_UB_33      0.0084249000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            43435
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.955
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.426
_diffrn_reflns_theta_min         3.721
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.978
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68825
_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    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.934
_refine_diff_density_min         -2.024
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         12555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0488
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+7.3873P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1244
_refine_ls_wR_factor_ref         0.1281
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11473
_reflns_number_total             12555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound6
_cod_database_code               7713811
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1S1Si1U1
_shelx_estimated_absorpt_t_max   0.467
_shelx_estimated_absorpt_t_min   0.267
_diffrn_oxdiff_digest_frames
;
015887dea9c0aad4a4316e709e761633e804114182b
;
_diffrn_oxdiff_digest_hkl
;
01d43488149d50cee6f1319636089f3f2941bc
;
_reflns_odcompleteness_completeness 99.88
_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:
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B)
2.b Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
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),
 C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46),
  C47(H47)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), 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), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C55(H55A,H55B,H55C)
;
_shelx_res_checksum              85246
_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 1.499
_oxdiff_exptl_absorpt_empirical_full_min 0.718