Intrinsic reactivity of [η<sup>5</sup>-1,3-(Me<sub>3</sub>Si)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>U(η<sup>4</sup>-C<sub>4</sub>Ph<sub>2</sub>) in small molecule activation.
Wang, Shichun; Heng, Yi; Li, Tongyu; Wang, Dongwei; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Dalton transactions (Cambridge, England : 2003) 51 (2022) 11072–11085; doi:10.1039/d2dt01730j

data_7710609
_publ_section_title
;
 Intrinsic reactivity of
 [\h<sup>5</sup>-1,3-(Me<sub>3</sub>Si)<sub>2</sub>C<sub>5</sub>H<sub>3</sub>]<sub>2</sub>U(\h<sup>4</sup>-C<sub>4</sub>Ph<sub>2</sub>)
 in small molecule activation.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11072
_journal_page_last               11085
_journal_paper_doi               10.1039/d2dt01730j
_journal_volume                  51
_journal_year                    2022
_chemical_formula_moiety         'C60 H84 O2 Si6 U, C6 H6'
_chemical_formula_sum            'C66 H90 O2 Si6 U'
_chemical_formula_weight         1321.94
_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             2021-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-05-12 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.262(3)
_cell_angle_beta                 102.482(3)
_cell_angle_gamma                90.682(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5700(5)
_cell_length_b                   12.2058(5)
_cell_length_c                   23.5380(6)
_cell_measurement_reflns_used    15357
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0210
_cell_measurement_theta_min      3.8010
_cell_volume                     3245.2(2)
_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      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 0.952
_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    -15.00  29.00   0.50    0.64    --  -46.70  19.00   0.00   88
  2  \w    -24.00  16.00   0.50    0.64    --  -46.70  19.00-120.00   80
  3  \w    -37.00  25.00   0.50    0.64    --  -46.70  37.00  30.00  124
  4  \w    -54.00 -29.00   0.50    1.00    -- -102.00  84.00  83.00   50
  5  \w    -71.00 -36.00   0.50    1.00    -- -102.00 125.00  30.00   70
  6  \w    -73.00  26.00   0.50    0.64    --  -46.70  84.00  83.00  198
  7  \w    -12.00  53.00   0.50    0.64    --   46.70 -84.00 -36.00  130
  8  \w     32.00 107.00   0.50    1.00    --  104.75 -94.00  60.00  150
  9  \w     84.00 117.00   0.50    1.00    --  104.75-125.00 150.00   66
 10  \w     50.00 117.00   0.50    1.00    --  104.75-125.00  60.00  134
 11  \w     80.00 117.00   0.50    1.00    --  104.75-125.00 -30.00   74
 12  \w     53.00 121.00   0.50    1.00    --  104.75-134.00   3.15  136
 13  \w     46.00 105.00   0.50    1.00    --  104.75 -94.00 150.00  118
 14  \w     91.00 177.00   0.50    1.00    --  104.75  15.00  30.00  172
 15  \w    130.00 177.00   0.50    1.00    --  104.75  61.00-150.00   94
 16  \w     96.00 135.00   0.50    1.00    --  104.75  45.00-150.00   78
 17  \w     91.00 126.00   0.50    1.00    --  104.75  61.00-150.00   70
 18  \w     77.00 131.00   0.50    1.00    --  104.75 125.00 -90.00  108
 19  \w     81.00 177.00   0.50    1.00    --  104.75  84.00  83.00  192
 20  \w     33.00  71.00   0.50    1.00    --  104.75 -61.00-150.00   76
 21  \w     39.00  69.00   0.50    1.00    --  104.75 -61.00-180.00   60
 22  \w     33.00  73.00   0.50    1.00    --  104.75 -61.00-120.00   80
 23  \w     36.00  61.00   0.50    1.00    --  104.75 -84.00 -36.00   50
 24  \w    -22.00  24.00   0.50    0.64    --   46.70 -19.00  30.00   92
 25  \w   -105.00 -80.00   0.50    0.64    --  -46.70-125.00-180.00   50
 26  \w   -133.00 -86.00   0.50    1.00    -- -102.00-125.00-120.00   94
 27  \w   -134.00 -94.00   0.50    1.00    -- -102.00 -84.00 -36.00   80
 28  \w   -124.00 -99.00   0.50    1.00    -- -102.00 -45.00   0.00   50
 29  \w   -105.00 -72.00   0.50    0.64    --  -46.70-125.00 -60.00   66
 30  \w   -117.00 -71.00   0.50    0.64    --  -46.70-125.00 120.00   92
 31  \w   -174.00-132.00   0.50    1.00    -- -102.00 -45.00   0.00   84
 32  \w   -174.00 -82.00   0.50    1.00    -- -102.00 -94.00  60.00  184
 33  \w   -173.00-136.00   0.50    1.00    -- -102.00-125.00-120.00   74
 34  \w   -173.00-116.00   0.50    1.00    -- -102.00 -61.00 120.00  114
 35  \w    -68.00 -30.00   0.50    1.00    -- -102.00  61.00 150.00   76
 36  \w    -68.00 -42.00   0.50    1.00    -- -102.00  61.00  90.00   52
 37  \w   -108.00 -82.00   0.50    1.00    -- -102.00  84.00  83.00   52
 38  \w   -104.00 -32.00   0.50    1.00    -- -102.00 125.00-120.00  144
 39  \w    -69.00 -43.00   0.50    1.00    -- -102.00  61.00-120.00   52
 40  \w    -68.00 -30.00   0.50    1.00    -- -102.00  61.00-180.00   76
 41  \w    -99.00 -50.00   0.50    1.00    -- -102.00  77.00-180.00   98
 42  \w   -114.00 -42.00   0.50    1.00    -- -102.00 125.00-150.00  144
;
_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      0.1008507000
_diffrn_orient_matrix_UB_12      -0.0120837000
_diffrn_orient_matrix_UB_13      0.0541962000
_diffrn_orient_matrix_UB_21      -0.0732105000
_diffrn_orient_matrix_UB_22      -0.0878206000
_diffrn_orient_matrix_UB_23      0.0239229000
_diffrn_orient_matrix_UB_31      0.0554459000
_diffrn_orient_matrix_UB_32      -0.0898233000
_diffrn_orient_matrix_UB_33      -0.0313908000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0772
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            42946
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.726
_diffrn_reflns_theta_min         3.622
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.408
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50773
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       block
_exptl_crystal_F_000             1356
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         4.460
_refine_diff_density_min         -3.995
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         13023
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0662
_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^)+(0.0826P)^2^+33.4302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1694
_refine_ls_wR_factor_ref         0.1748
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11630
_reflns_number_total             13023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound15
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710609
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1Si1U1
_shelx_estimated_absorpt_t_max   0.365
_shelx_estimated_absorpt_t_min   0.365
_diffrn_oxdiff_digest_frames
;
0153a38fe326066dce3863553c5ec7d0b304072cfb1
;
_diffrn_oxdiff_digest_hkl
;
015978413dd32880f8e37466bcabc2e6b50319
;
_reflns_odcompleteness_completeness 99.76
_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. Uiso/Uaniso restraints and constraints
Uanis(O2) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C32(H32), C33(H33), C34(H34), C35(H35),
 C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C56(H56), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66)
3.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), C30(H30A,H30B,H30C),
 C54(H54A,H54B,H54C)
;
_shelx_res_checksum              4731
_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 1.797
_oxdiff_exptl_absorpt_empirical_full_min 0.379