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_7710614
_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 H62 N2 Si4 U, C6 H6'
_chemical_formula_sum            'C51 H68 N2 Si4 U'
_chemical_formula_weight         1059.46
_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
_atom_sites_solution_primary     dual
_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                93.068(2)
_cell_angle_beta                 92.354(2)
_cell_angle_gamma                108.278(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1296(3)
_cell_length_b                   11.5631(3)
_cell_length_c                   20.5536(2)
_cell_measurement_reflns_used    25698
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      76.1950
_cell_measurement_theta_min      4.0020
_cell_volume                     2503.37(10)
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.956
_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    104.00 130.00   0.50    0.08    --  104.75  30.00 150.00   52
  2  \w    144.00 178.00   0.50    0.08    --  104.75  30.00 150.00   68
  3  \w     70.00  95.00   0.50    0.05    --   46.95 134.00-140.00   50
  4  \w     90.00 116.00   0.50    0.05    --   46.95 135.00  38.00   52
  5  \w    -24.00  29.00   0.50    0.05    --  -46.95  19.00  30.00  106
  6  \w    -69.00 -30.00   0.50    0.08    -- -102.00  61.00  90.00   78
  7  \w    -60.00 -34.00   0.50    0.08    -- -102.00  61.00  60.00   52
  8  \w   -103.00 -64.00   0.50    0.08    -- -102.00  77.00   0.00   78
  9  \w    -66.00 -41.00   0.50    0.08    -- -102.00  61.00-180.00   50
 10  \w    -23.00  28.00   0.50    0.05    --  -46.95  19.00 -90.00  102
 11  \w    114.00 139.00   0.50    0.08    --  104.75 135.00  38.00   50
 12  \w    144.00 173.00   0.50    0.08    --  104.75 125.00 -30.00   58
 13  \w     92.00 178.00   0.50    0.08    --  104.75 125.00   0.00  172
 14  \w     87.00 124.00   0.50    0.08    --  104.75 125.00 -30.00   74
 15  \w     80.00 177.00   0.50    0.08    --  104.75 125.00  90.00  194
 16  \w     76.00 160.00   0.50    0.08    --  104.75 125.00-120.00  168
 17  \w     81.00 133.00   0.50    0.08    --  104.75 134.00-140.00  104
 18  \w    -24.00  21.00   0.50    0.05    --   46.95 -19.00 -30.00   90
 19  \w     38.00  66.00   0.50    0.08    --  104.75 -61.00-180.00   56
 20  \w     70.00 105.00   0.50    0.08    --  104.75 -77.00 -60.00   70
 21  \w     33.00  61.00   0.50    0.08    --  104.75 -77.00 -60.00   56
 22  \w     32.00  73.00   0.50    0.08    --  104.75 -61.00 -30.00   82
 23  \w     44.00  72.00   0.50    0.08    --  104.75 -61.00 150.00   56
 24  \w     78.00 109.00   0.50    0.08    --  104.75 -94.00   0.00   62
 25  \w     85.00 122.00   0.50    0.08    --  104.75-135.00 -26.00   74
 26  \w     58.00  83.00   0.50    0.05    --   46.95-135.00 -26.00   50
 27  \w     50.00 104.00   0.50    0.08    --  104.75 -94.00  90.00  108
 28  \w     90.00 124.00   0.50    0.08    --  104.75-134.00 152.00   68
 29  \w     38.00 106.00   0.50    0.08    --  104.75 -94.00 150.00  136
 30  \w     38.00 100.00   0.50    0.05    --   46.95-134.00 152.00  124
 31  \w    -82.00 -56.00   0.50    0.05    --  -46.95 135.00  38.00   52
 32  \w   -123.00 -87.00   0.50    0.08    -- -102.00 134.00-140.00   72
 33  \w    -80.00 -47.00   0.50    0.08    -- -102.00 134.00-140.00   66
 34  \w    -82.00 -57.00   0.50    0.05    --  -46.95 134.00-140.00   50
 35  \w   -123.00 -30.00   0.50    0.08    -- -102.00 135.00  38.00  186
 36  \w   -169.00-104.00   0.50    0.08    -- -102.00 -15.00 -90.00  130
 37  \w   -168.00-142.00   0.50    0.08    -- -102.00 -61.00-180.00   52
 38  \w   -124.00 -86.00   0.50    0.08    -- -102.00 -61.00-180.00   76
 39  \w   -118.00 -24.00   0.50    0.05    --  -46.95 -77.00 -30.00  188
 40  \w   -172.00 -89.00   0.50    0.08    -- -102.00 -45.00  30.00  166
 41  \w   -117.00 -79.00   0.50    0.05    --  -46.95-125.00   0.00   76
 42  \w   -119.00 -67.00   0.50    0.05    --  -46.95-135.00 -26.00  104
 43  \w   -174.00-149.00   0.50    0.08    -- -102.00 -94.00 -90.00   50
 44  \w   -139.00 -97.00   0.50    0.08    -- -102.00 -94.00 -90.00   84
 45  \w   -144.00-119.00   0.50    0.08    -- -102.00-135.00 -26.00   50
 46  \w    -94.00 -66.00   0.50    0.05    --  -46.95-134.00 152.00   56
 47  \w   -145.00-120.00   0.50    0.08    -- -102.00-134.00 152.00   50
;
_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      -0.0049900000
_diffrn_orient_matrix_UB_12      0.0013064000
_diffrn_orient_matrix_UB_13      0.0748203000
_diffrn_orient_matrix_UB_21      0.1412502000
_diffrn_orient_matrix_UB_22      0.0767738000
_diffrn_orient_matrix_UB_23      0.0075296000
_diffrn_orient_matrix_UB_31      -0.0367880000
_diffrn_orient_matrix_UB_32      0.1178472000
_diffrn_orient_matrix_UB_33      0.0005454000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0606
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            34664
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.584
_diffrn_reflns_theta_min         4.036
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    10.295
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73446
_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    1.406
_exptl_crystal_description       block
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.849
_refine_diff_density_min         -2.120
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     537
_refine_ls_number_reflns         10052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0376P)^2^+12.7437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1021
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9412
_reflns_number_total             10052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound11
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710614
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1Si1U1
_shelx_estimated_absorpt_t_max   0.426
_shelx_estimated_absorpt_t_min   0.426
_diffrn_oxdiff_digest_frames
;
011a884470229bde7ce3f3bd455b4573f0000599111
;
_diffrn_oxdiff_digest_hkl
;
01365495b950ed6e092db1ad0c70b9696ce685
;
_reflns_odcompleteness_completeness 99.87
_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:
 C29(H29)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C40(H40), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48), C49(H49),
 C50(H50), C51(H51)
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), C44(H44A,H44B,H44C), C45(H45A,H45B,H45C)
;
_shelx_res_checksum              1470
_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 1.337
_oxdiff_exptl_absorpt_empirical_full_min 0.650