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_7710617
_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         'C56 H68 O2 Si4 U, 1.5(C6 H6)'
_chemical_formula_sum            'C65 H77 O2 Si4 U'
_chemical_formula_weight         1240.65
_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                79.5620(10)
_cell_angle_beta                 75.3780(10)
_cell_angle_gamma                81.0250(10)
_cell_formula_units_Z            2
_cell_length_a                   12.0572(2)
_cell_length_b                   13.04160(10)
_cell_length_c                   19.9628(2)
_cell_measurement_reflns_used    29608
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.7360
_cell_measurement_theta_min      2.3270
_cell_volume                     2967.00(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      100.00(10)
_diffrn_detector                 'CCD plate'
_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    -53.00  24.00   0.50    0.05    --  -47.70  40.00 -34.00  154
  2  \w    -59.00 -31.00   0.50    0.05    -- -102.00  40.00 -34.00   56
  3  \w    -65.00 -39.00   0.50    0.05    -- -102.00 125.00  90.00   52
  4  \w   -101.00 -27.00   0.50    0.05    -- -102.00  30.00 150.00  148
  5  \w    -62.00 -36.00   0.50    0.05    --  -47.70 -40.00 171.00   52
  6  \w     51.00  97.00   0.50    0.05    --   47.70  40.00 -34.00   92
  7  \w    111.00 172.00   0.50    0.05    --  104.75  40.00 -34.00  122
  8  \w    153.00 178.00   0.50    0.05    --  104.75  30.00  60.00   50
  9  \w     94.00 126.00   0.50    0.05    --  104.75  30.00  60.00   64
 10  \w     47.00 116.00   0.50    0.05    --  104.75 -40.00 171.00  138
 11  \w     65.00  95.00   0.50    0.05    --  104.75 -94.00  60.00   60
 12  \w     33.00  82.00   0.50    0.05    --  104.75 -94.00   0.00   98
 13  \w     35.00 108.00   0.50    0.05    --  104.75 -94.00  30.00  146
 14  \w     36.00 107.00   0.50    0.05    --  104.75 -94.00 150.00  142
 15  \w     16.00  94.00   0.50    0.05    --   47.70-125.00  60.00  156
 16  \w    -18.00  42.00   0.50    0.05    --   47.70 -40.00 171.00  120
 17  \w    -24.00  60.00   0.50    0.05    --   47.70 -57.00 -60.00  168
 18  \w     48.00  95.00   0.50    0.05    --  104.75 -94.00-180.00   94
 19  \w     32.00 119.00   0.50    0.05    --  104.75 -61.00-180.00  174
 20  \w    -70.00  25.00   0.50    0.05    --  -47.70  77.00-180.00  190
 21  \w    -65.00 -31.00   0.50    0.05    -- -102.00 125.00 -60.00   68
 22  \w    -95.00 -30.00   0.50    0.05    -- -102.00  45.00-180.00  130
 23  \w   -116.00 -29.00   0.50    0.05    -- -102.00 125.00-120.00  174
 24  \w   -115.00 -89.00   0.50    0.05    -- -102.00 125.00 -60.00   52
 25  \w   -103.00 -78.00   0.50    0.05    -- -102.00 125.00  90.00   50
 26  \w   -174.00 -88.00   0.50    0.05    -- -102.00 -15.00  30.00  172
 27  \w   -116.00 -91.00   0.50    0.05    --  -47.70-125.00 120.00   50
 28  \w   -174.00 -91.00   0.50    0.05    -- -102.00 -40.00 171.00  166
 29  \w   -174.00-142.00   0.50    0.05    -- -102.00 -45.00 150.00   64
;
_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      -0.0637784000
_diffrn_orient_matrix_UB_12      0.1083083000
_diffrn_orient_matrix_UB_13      0.0149330000
_diffrn_orient_matrix_UB_21      -0.1099875000
_diffrn_orient_matrix_UB_22      -0.0514303000
_diffrn_orient_matrix_UB_23      0.0383347000
_diffrn_orient_matrix_UB_31      0.0388471000
_diffrn_orient_matrix_UB_32      -0.0157528000
_diffrn_orient_matrix_UB_33      0.0693639000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_unetI/netI     0.0379
_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       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            34843
_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         75.985
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.789
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55207
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       block
_exptl_crystal_F_000             1262
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.205
_refine_diff_density_min         -2.230
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     661
_refine_ls_number_reflns         11867
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0463
_refine_ls_R_factor_gt           0.0392
_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^)+31.3911P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0917
_refine_ls_wR_factor_ref         0.0966
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11473
_reflns_number_total             11867
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound14
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710617
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1U1Si1
_shelx_estimated_absorpt_t_max   0.474
_shelx_estimated_absorpt_t_min   0.474
_diffrn_oxdiff_digest_frames
;
01c41347f01f64db34f2844e9933c01f2e032026579
;
_diffrn_oxdiff_digest_hkl
;
017f163961902176f5147e07691ed78ab3d439
;
_reflns_odcompleteness_completeness 99.90
_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:
 C24(H24A,H24B), C25(H25A,H25B), C55(H55A,H55B), C56(H56A,H56B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C27(H27), C28(H28),
 C29(H29), C30(H30), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52),
 C53(H53), C57(H57), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C63(H63),
  C64(H64), C65(H65)
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              10325
_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 1.372
_oxdiff_exptl_absorpt_empirical_full_min 0.742