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_7710610
_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         'C54 H68 O2 Si4 U'
_chemical_formula_sum            'C54 H68 O2 Si4 U'
_chemical_formula_weight         1099.47
_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                76.927(2)
_cell_angle_beta                 89.400(2)
_cell_angle_gamma                68.021(2)
_cell_formula_units_Z            2
_cell_length_a                   11.8507(2)
_cell_length_b                   12.1083(2)
_cell_length_c                   19.7897(3)
_cell_measurement_reflns_used    19874
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      75.6020
_cell_measurement_theta_min      4.0000
_cell_volume                     2556.36(8)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.962
_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    -66.00 -23.00   0.50    0.19    --  -47.70 104.00-112.00   86
  2  \w      2.00  61.00   0.50    0.19    --   47.70-104.00 146.00  118
  3  \w   -174.00-142.00   0.50    0.50    -- -102.00-104.00 146.00   64
  4  \w   -132.00 -84.00   0.50    0.50    -- -102.00-104.00 146.00   96
  5  \w   -109.00 -84.00   0.50    0.50    -- -102.00 104.00-112.00   50
  6  \w     34.00 107.00   0.50    0.50    --  104.75-104.00 146.00  146
  7  \w    -60.00  26.00   0.50    0.19    --  -47.70  37.00-150.00  172
  8  \w   -118.00 -33.00   0.50    0.19    --  -47.70 -57.00-120.00  170
  9  \w   -116.00 -71.00   0.50    0.19    --  -47.70-125.00-180.00   90
 10  \w   -119.00 -93.00   0.50    0.19    --  -47.70-125.00 -60.00   52
 11  \w     15.00  85.00   0.50    0.19    --   47.70-125.00  30.00  140
 12  \w     -1.00  28.00   0.50    0.19    --   47.70 -37.00   0.00   58
 13  \w     31.00  56.00   0.50    0.19    --   47.70 -37.00   0.00   50
 14  \w   -117.00 -86.00   0.50    0.50    -- -102.00 125.00 -60.00   62
 15  \w   -116.00 -86.00   0.50    0.50    -- -102.00 -61.00-150.00   60
 16  \w   -140.00 -90.00   0.50    0.50    -- -102.00 -45.00 120.00  100
 17  \w   -163.00 -99.00   0.50    0.50    -- -102.00 -45.00-180.00  128
 18  \w   -168.00-143.00   0.50    0.50    -- -102.00 -45.00 120.00   50
 19  \w   -165.00-136.00   0.50    0.50    -- -102.00 -61.00-150.00   58
 20  \w   -117.00 -29.00   0.50    0.50    -- -102.00  61.00 -30.00  176
 21  \w    -65.00 -29.00   0.50    0.50    -- -102.00  15.00 120.00   72
 22  \w   -112.00 -30.00   0.50    0.50    -- -102.00  61.00  90.00  164
 23  \w     79.00 115.00   0.50    0.50    --  104.75-125.00   0.00   72
 24  \w     94.00 175.00   0.50    0.50    --  104.75  45.00   0.00  162
 25  \w     56.00  82.00   0.50    0.50    --  104.75 -94.00  60.00   52
 26  \w     33.00  69.00   0.50    0.50    --  104.75-125.00   0.00   72
 27  \w     34.00 116.00   0.50    0.50    --  104.75 -45.00 -60.00  164
 28  \w     32.00  95.00   0.50    0.50    --  104.75 -94.00 -90.00  126
 29  \w     54.00 103.00   0.50    0.50    --  104.75 -94.00-180.00   98
 30  \w     84.00 170.00   0.50    0.50    --  104.75  77.00-150.00  172
 31  \w     79.00 111.00   0.50    0.50    --  104.75-125.00 150.00   64
 32  \w     38.00  63.00   0.50    0.50    --  104.75-125.00 150.00   50
 33  \w     32.00 101.00   0.50    0.50    --  104.75 -61.00 120.00  138
 34  \w     98.00 134.00   0.50    0.50    --  104.75 104.00-112.00   72
;
_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      -0.0296939000
_diffrn_orient_matrix_UB_12      0.0157444000
_diffrn_orient_matrix_UB_13      0.0740557000
_diffrn_orient_matrix_UB_21      0.0158247000
_diffrn_orient_matrix_UB_22      -0.1356356000
_diffrn_orient_matrix_UB_23      0.0231997000
_diffrn_orient_matrix_UB_31      0.1365769000
_diffrn_orient_matrix_UB_32      -0.0364304000
_diffrn_orient_matrix_UB_33      0.0201948000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30586
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.663
_diffrn_reflns_theta_min         2.300
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.123
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65430
_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    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         6.915
_refine_diff_density_min         -4.600
_refine_diff_density_rms         0.312
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         10212
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0605
_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^)+(0.1265P)^2^+6.8691P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1604
_refine_ls_wR_factor_ref         0.1664
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9639
_reflns_number_total             10212
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound12
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_original_cell_volume        2556.37(8)
_cod_database_code               7710610
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1O1U1
_shelx_estimated_absorpt_t_max   0.431
_shelx_estimated_absorpt_t_min   0.237
_diffrn_oxdiff_digest_frames
;
01669fbc010726c7e427c1e94009ba197603404f579
;
_diffrn_oxdiff_digest_hkl
;
014daf3b8cafbe8600d55a44ba91b2a98ac86f
;
_reflns_odcompleteness_completeness 99.79
_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:
 C23(H23), C28(H28)
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),
 C33(H33), C34(H34), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C49(H49), C50(H50), C52(H52), C53(H53)
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), C35(H35A,H35B,H35C), C54(H54A,H54B,H54C)
;
_shelx_res_checksum              37300
_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 2.812
_oxdiff_exptl_absorpt_empirical_full_min 0.451