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_7710608
_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         'C51 H73 N S Si6 U, C3 H3'
_chemical_formula_sum            'C54 H76 N S Si6 U'
_chemical_formula_weight         1177.78
_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             2021-05-05
_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                87.659(2)
_cell_angle_beta                 80.068(2)
_cell_angle_gamma                64.874(3)
_cell_formula_units_Z            2
_cell_length_a                   11.6893(3)
_cell_length_b                   12.0620(4)
_cell_length_c                   23.1044(3)
_cell_measurement_reflns_used    23475
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.0190
_cell_measurement_theta_min      3.8490
_cell_volume                     2903.27(15)
_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 0.957
_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     33.00 118.00   0.50    0.06    --   46.95  58.00   5.00  170
  2  \w    148.00 176.00   0.50    0.10    --  104.75 125.00-120.00   56
  3  \w     90.00 141.00   0.50    0.10    --  104.75 125.00-120.00  102
  4  \w    104.00 177.00   0.50    0.10    --  104.75  58.00   5.00  146
  5  \w     92.00 177.00   0.50    0.10    --  104.75  45.00 -60.00  170
  6  \w     49.00 107.00   0.50    0.10    --  104.75 -94.00   0.00  116
  7  \w     47.00  95.00   0.50    0.06    --   46.95-125.00 -90.00   96
  8  \w     22.00  91.00   0.50    0.06    --   46.95-125.00-150.00  138
  9  \w     37.00  62.00   0.50    0.10    --  104.75-125.00 -60.00   50
 10  \w     76.00 115.00   0.50    0.10    --  104.75-125.00 -60.00   78
 11  \w     82.00 108.00   0.50    0.10    --  104.75-125.00-120.00   52
 12  \w     58.00 108.00   0.50    0.10    --  104.75 -94.00-180.00  100
 13  \w     45.00 105.00   0.50    0.10    --  104.75 -94.00 -60.00  120
 14  \w     35.00  63.00   0.50    0.10    --  104.75-125.00   0.00   56
 15  \w     92.00 117.00   0.50    0.10    --  104.75-125.00   0.00   50
 16  \w     60.00 116.00   0.50    0.10    --  104.75-125.00 120.00  112
 17  \w     51.00  95.00   0.50    0.10    --  104.75 -94.00 150.00   88
 18  \w     36.00  73.00   0.50    0.10    --  104.75 -61.00 120.00   74
 19  \w     38.00  66.00   0.50    0.10    --  104.75 -61.00 150.00   56
 20  \w     39.00  72.00   0.50    0.10    --  104.75 -61.00  30.00   66
 21  \w     38.00  72.00   0.50    0.10    --  104.75 -61.00   0.00   68
 22  \w    -27.00   6.00   0.50    0.06    --   46.95 -19.00  60.00   66
 23  \w     40.00  72.00   0.50    0.10    --  104.75 -61.00-150.00   64
 24  \w     34.00  69.00   0.50    0.10    --  104.75 -58.00-135.00   70
 25  \w    -24.00  61.00   0.50    0.06    --   46.95 -58.00-135.00  170
 26  \w    -22.00  22.00   0.50    0.06    --  -46.95  19.00   0.00   88
 27  \w    -31.00  25.00   0.50    0.06    --  -46.95  58.00   5.00  112
 28  \w    -69.00 -44.00   0.50    0.10    -- -102.00  61.00 120.00   50
 29  \w    -63.00 -37.00   0.50    0.10    -- -102.00  61.00  60.00   52
 30  \w    -63.00 -29.00   0.50    0.10    -- -102.00  58.00   5.00   68
 31  \w    -84.00 -34.00   0.50    0.10    -- -102.00  77.00 -30.00  100
 32  \w    -56.00 -31.00   0.50    0.10    -- -102.00  61.00 -60.00   50
 33  \w    -67.00 -31.00   0.50    0.10    -- -102.00 125.00  30.00   72
 34  \w   -111.00 -85.00   0.50    0.10    -- -102.00 125.00  30.00   52
 35  \w   -166.00-105.00   0.50    0.10    -- -102.00 -15.00  90.00  122
 36  \w   -164.00 -99.00   0.50    0.10    -- -102.00 -15.00  60.00  130
 37  \w   -173.00 -89.00   0.50    0.10    -- -102.00 -61.00-150.00  168
 38  \w   -170.00 -92.00   0.50    0.10    -- -102.00 -58.00-135.00  156
 39  \w   -115.00 -56.00   0.50    0.06    --  -46.95 -58.00-135.00  118
 40  \w   -161.00 -71.00   0.50    0.10    -- -102.00-125.00   0.00  180
;
_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      0.1105103000
_diffrn_orient_matrix_UB_12      0.0382747000
_diffrn_orient_matrix_UB_13      -0.0194763000
_diffrn_orient_matrix_UB_21      -0.0697617000
_diffrn_orient_matrix_UB_22      0.1131587000
_diffrn_orient_matrix_UB_23      0.0423325000
_diffrn_orient_matrix_UB_31      0.0689371000
_diffrn_orient_matrix_UB_32      -0.0752108000
_diffrn_orient_matrix_UB_33      0.0491632000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_av_unetI/netI     0.0705
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.957
_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       28
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            38484
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.746
_diffrn_reflns_theta_min         3.887
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82718
_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    1.347
_exptl_crystal_description       block
_exptl_crystal_F_000             1198
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.802
_refine_diff_density_min         -2.549
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         11710
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0722P)^2^+6.8750P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1333
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10791
_reflns_number_total             11710
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_original_cell_volume        2903.27(14)
_cod_database_code               7710608
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1S1Si1U1
_shelx_estimated_absorpt_t_max   0.446
_shelx_estimated_absorpt_t_min   0.446
_diffrn_oxdiff_digest_frames
;
019665a3cc283ef828e0a38f0c96b8798f0010404d2
;
_diffrn_oxdiff_digest_hkl
;
01b72db7eda17920009b450bcf936c4bd4cbae
;
_reflns_odcompleteness_completeness 99.91
_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. Restrained distances
 C54-C53 = C53-C52
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C54) \\sim Ueq, Uanis(C53) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C47(H47), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54)
4.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)
;
_shelx_res_checksum              93271
_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 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.645