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_7710611
_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         'C45 H57 N S Si4 U'
_chemical_formula_sum            'C45 H57 N S Si4 U'
_chemical_formula_weight         994.36
_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             2022-05-11
_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                85.2590(10)
_cell_angle_beta                 87.9470(10)
_cell_angle_gamma                74.7230(10)
_cell_formula_units_Z            2
_cell_length_a                   11.8426(2)
_cell_length_b                   13.5469(2)
_cell_length_c                   14.92600(10)
_cell_measurement_reflns_used    20595
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.7040
_cell_measurement_theta_min      3.3410
_cell_volume                     2301.82(6)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_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      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.959
_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    -23.00   3.00   0.50    0.07    --   47.70 -68.00 -13.00   52
  2  \w     13.00  61.00   0.50    0.07    --   47.70 -68.00 -13.00   96
  3  \w     22.00  92.00   0.50    0.07    --   47.70-125.00   0.00  140
  4  \w     40.00  99.00   0.50    0.30    --  104.75-125.00 -30.00  118
  5  \w     83.00 115.00   0.50    0.30    --  104.75-125.00  30.00   64
  6  \w     76.00 109.00   0.50    0.30    --  104.75 -94.00  90.00   66
  7  \w     56.00 109.00   0.50    0.30    --  104.75 -94.00   0.00  106
  8  \w     36.00 118.00   0.50    0.30    --  104.75 -15.00 150.00  164
  9  \w     88.00 178.00   0.50    0.30    --  104.75  61.00 150.00  180
 10  \w    109.00 167.00   0.50    0.30    --  104.75  68.00 119.00  116
 11  \w     55.00 111.00   0.50    0.07    --   47.70  68.00 119.00  112
 12  \w     37.00 116.00   0.50    0.30    --  104.75 -45.00   0.00  158
 13  \w     35.00  74.00   0.50    0.30    --  104.75-125.00  30.00   78
 14  \w     32.00 122.00   0.50    0.30    --  104.75 -68.00 -13.00  180
 15  \w     51.00  77.00   0.50    0.30    --  104.75 -94.00-180.00   52
 16  \w    -65.00  16.00   0.50    0.07    --  -47.70  68.00 119.00  162
 17  \w    -58.00 -33.00   0.50    0.30    -- -102.00  68.00 119.00   50
 18  \w    -78.00 -29.00   0.50    0.30    -- -102.00 125.00 150.00   98
 19  \w    -94.00 -13.00   0.50    0.07    --  -47.70 125.00 120.00  162
 20  \w   -117.00 -86.00   0.50    0.30    -- -102.00 125.00 150.00   62
 21  \w   -114.00 -82.00   0.50    0.30    -- -102.00  45.00 -30.00   64
 22  \w   -131.00 -97.00   0.50    0.30    -- -102.00 -30.00  60.00   68
 23  \w   -117.00 -92.00   0.50    0.30    -- -102.00 -68.00 -13.00   50
 24  \w   -115.00 -41.00   0.50    0.07    --  -47.70 -68.00 -13.00  148
 25  \w   -106.00 -71.00   0.50    0.07    --  -47.70-125.00 120.00   70
 26  \w   -164.00 -88.00   0.50    0.30    -- -102.00 -77.00 -30.00  152
 27  \w   -174.00-141.00   0.50    0.30    -- -102.00 -30.00  60.00   66
 28  \w   -118.00 -45.00   0.50    0.30    -- -102.00  61.00-120.00  146
 29  \w   -111.00 -31.00   0.50    0.30    -- -102.00 125.00-150.00  160
;
_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      -0.1063598000
_diffrn_orient_matrix_UB_12      -0.0159592000
_diffrn_orient_matrix_UB_13      -0.0476976000
_diffrn_orient_matrix_UB_21      0.0829034000
_diffrn_orient_matrix_UB_22      -0.0686748000
_diffrn_orient_matrix_UB_23      -0.0650994000
_diffrn_orient_matrix_UB_31      0.0018432000
_diffrn_orient_matrix_UB_32      -0.0949043000
_diffrn_orient_matrix_UB_33      0.0649281000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0400
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            26302
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.648
_diffrn_reflns_theta_min         2.971
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       block
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.307
_refine_diff_density_min         -2.747
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         9180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0287
_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^)+(0.0409P)^2^+4.9393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8803
_reflns_number_total             9180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710611
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1S1U1
_shelx_estimated_absorpt_t_max   0.391
_shelx_estimated_absorpt_t_min   0.391
_diffrn_oxdiff_digest_frames
;
017cc3d03cdaf5c1d07aa620ded92aa975000707c12
;
_diffrn_oxdiff_digest_hkl
;
01bb1c1527a9db9152e51886efc280c383678e
;
_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 Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C29(H29), C30(H30),
 C31(H31), C32(H32), C33(H33), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39),
  C41(H41), C42(H42), C43(H43), C44(H44), C45(H45)
2.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), 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              46390
_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 1.896
_oxdiff_exptl_absorpt_empirical_full_min 0.573