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_7710615
_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         'C64 H72 S2 Si4 U, 2(C6 H6)'
_chemical_formula_sum            'C76 H84 S2 Si4 U'
_chemical_formula_weight         1411.94
_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
_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
;
2022-05-12 deposited with the CCDC.	2022-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                86.336(2)
_cell_angle_beta                 88.711(2)
_cell_angle_gamma                78.197(2)
_cell_formula_units_Z            2
_cell_length_a                   12.5008(3)
_cell_length_b                   14.1759(3)
_cell_length_c                   19.8061(4)
_cell_measurement_reflns_used    24037
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.2380
_cell_measurement_theta_min      4.1710
_cell_volume                     3428.45(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 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 0.998
_diffrn_measured_fraction_theta_max 0.958
_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     93.00 172.00   0.50    0.80    --  104.75  45.00 -90.00  158
  2  \w    104.00 170.00   0.50    0.80    --  104.75  30.00 -30.00  132
  3  \w    151.00 176.00   0.50    0.80    --  104.75  15.00 120.00   50
  4  \w     93.00 142.00   0.50    0.80    --  104.75  15.00 120.00   98
  5  \w     78.00 108.00   0.50    0.80    --  104.75 -94.00 -30.00   60
  6  \w     44.00  70.00   0.50    0.30    --   46.95-142.00 -67.00   52
  7  \w     32.00 120.00   0.50    0.80    --  104.75-142.00 -67.00  176
  8  \w     32.00 116.00   0.50    0.80    --  104.75-125.00 -60.00  168
  9  \w     43.00  68.00   0.50    0.30    --   46.95-128.00 103.00   50
 10  \w     60.00 101.00   0.50    0.80    --  104.75 -94.00 -60.00   82
 11  \w     39.00  66.00   0.50    0.80    --  104.75 -94.00 -30.00   54
 12  \w     50.00 116.00   0.50    0.80    --  104.75-128.00 103.00  132
 13  \w     56.00 104.00   0.50    0.80    --  104.75 -94.00 150.00   96
 14  \w     74.00 107.00   0.50    0.80    --  104.75 -94.00  90.00   66
 15  \w     60.00 105.00   0.50    0.80    --  104.75 -77.00  60.00   90
 16  \w    -26.00  27.00   0.50    0.30    --   46.95 -19.00 -90.00  106
 17  \w     35.00  61.00   0.50    0.80    --  104.75 -61.00 -30.00   52
 18  \w     32.00  72.00   0.50    0.80    --  104.75 -61.00 120.00   80
 19  \w     37.00  72.00   0.50    0.80    --  104.75 -61.00 150.00   70
 20  \w     83.00 108.00   0.50    0.30    --   46.95 142.00 -11.00   50
 21  \w     96.00 121.00   0.50    0.80    --  104.75 142.00 -11.00   50
 22  \w     82.00 127.00   0.50    0.80    --  104.75 128.00 178.00   90
 23  \w    -95.00 -44.00   0.50    0.30    --  -46.95 128.00 178.00  102
 24  \w   -116.00 -29.00   0.50    0.80    -- -102.00 128.00 178.00  174
 25  \w    -98.00 -62.00   0.50    0.30    --  -46.95 142.00 -11.00   72
 26  \w   -129.00 -29.00   0.50    0.80    -- -102.00 142.00 -11.00  200
 27  \w    -69.00 -33.00   0.50    0.80    -- -102.00  61.00   0.00   72
 28  \w    -68.00 -32.00   0.50    0.80    -- -102.00  61.00 120.00   72
 29  \w    -67.00 -30.00   0.50    0.80    -- -102.00  61.00 150.00   74
 30  \w    -65.00 -40.00   0.50    0.80    -- -102.00  61.00  30.00   50
 31  \w    -65.00 -29.00   0.50    0.80    -- -102.00  61.00 -30.00   72
 32  \w    -69.00 -44.00   0.50    0.80    -- -102.00  61.00-150.00   50
 33  \w    -24.00  28.00   0.50    0.30    --  -46.95  19.00-180.00  104
 34  \w    -23.00  26.00   0.50    0.30    --  -46.95  19.00 -90.00   98
 35  \w   -119.00 -25.00   0.50    0.30    --  -46.95 -77.00 120.00  188
 36  \w   -173.00 -79.00   0.50    0.80    -- -102.00 -77.00 -60.00  188
 37  \w   -138.00-100.00   0.50    0.80    -- -102.00 -45.00 120.00   76
 38  \w   -157.00 -89.00   0.50    0.80    -- -102.00 -15.00 150.00  136
 39  \w   -126.00 -82.00   0.50    0.80    -- -102.00 -94.00  60.00   88
 40  \w   -103.00 -77.00   0.50    0.80    -- -102.00-128.00 103.00   52
 41  \w   -173.00-148.00   0.50    0.80    -- -102.00 -94.00  60.00   50
 42  \w   -175.00 -86.00   0.50    0.80    -- -102.00 -94.00-120.00  178
 43  \w   -119.00 -67.00   0.50    0.30    --  -46.95-142.00 -67.00  104
 44  \w    -98.00 -73.00   0.50    0.30    --  -46.95-125.00-120.00   50
 45  \w    -98.00 -71.00   0.50    0.30    --  -46.95-128.00 103.00   54
 46  \w   -112.00 -78.00   0.50    0.30    --  -46.95-125.00 120.00   68
;
_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      -0.0710997000
_diffrn_orient_matrix_UB_12      -0.0261071000
_diffrn_orient_matrix_UB_13      0.0600758000
_diffrn_orient_matrix_UB_21      -0.0789011000
_diffrn_orient_matrix_UB_22      -0.0294786000
_diffrn_orient_matrix_UB_23      -0.0495035000
_diffrn_orient_matrix_UB_31      0.0676123000
_diffrn_orient_matrix_UB_32      -0.1040227000
_diffrn_orient_matrix_UB_33      0.0040051000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.958
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            49912
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.544
_diffrn_reflns_theta_min         3.612
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.208
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60566
_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    1.368
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.056
_refine_diff_density_min         -2.631
_refine_diff_density_rms         0.138
_refine_ls_extinction_coef       0.00031(4)
_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   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     761
_refine_ls_number_reflns         13809
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0460
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0538P)^2^+6.1357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1098
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12595
_reflns_number_total             13809
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound18
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710615
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1S1Si1U1
_shelx_estimated_absorpt_t_max   0.684
_shelx_estimated_absorpt_t_min   0.494
_diffrn_oxdiff_digest_frames
;
0133186649660b3e296f2acd04afd58218043344257
;
_diffrn_oxdiff_digest_hkl
;
010281737d31b612f03ca3b2acfb7bd1c819a3
;
_reflns_odcompleteness_completeness 99.89
_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 Ternary CH refined with riding coordinates:
 C25(H25), C43(H43), C44(H44)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C42(H42), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51),
 C53(H53), C54(H54), C55(H55), C56(H56), C57(H57), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C67(H67), C68(H68), C69(H69), C70(H70),
 C71(H71), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C77(H77)
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), C11(H11A,H11B,H11C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              37898
_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 1.637
_oxdiff_exptl_absorpt_empirical_full_min 0.660