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_7710613
_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         'C58 H78 N2 Si6 U'
_chemical_formula_sum            'C58 H78 N2 Si6 U'
_chemical_formula_weight         1209.79
_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                97.3550(10)
_cell_angle_beta                 98.3800(10)
_cell_angle_gamma                106.9790(10)
_cell_formula_units_Z            2
_cell_length_a                   11.6769(2)
_cell_length_b                   12.1414(2)
_cell_length_c                   22.3112(2)
_cell_measurement_reflns_used    31029
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.6840
_cell_measurement_theta_min      3.8530
_cell_volume                     2943.94(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      100.00(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 0.960
_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    -57.00  25.00   0.50    0.05    --  -47.70  57.00 -90.00  164
  2  \w    -56.00  17.00   0.50    0.05    --  -47.70  90.00 -60.00  146
  3  \w     29.00  59.00   0.50    0.05    --   47.70 -37.00 -30.00   60
  4  \w     36.00  75.00   0.50    0.05    --  104.75 -94.00  60.00   78
  5  \w     65.00 108.00   0.50    0.05    --  104.75 -94.00 120.00   86
  6  \w     92.00 118.00   0.50    0.05    --  104.75 -77.00   0.00   52
  7  \w     71.00 109.00   0.50    0.05    --  104.75 -94.00 -30.00   76
  8  \w     42.00  67.00   0.50    0.05    --  104.75 -94.00 -30.00   50
  9  \w     32.00  90.00   0.50    0.05    --  104.75-125.00  30.00  116
 10  \w     32.00  59.00   0.50    0.05    --  104.75 -94.00 120.00   54
 11  \w    -21.00   5.00   0.50    0.05    --   47.70 -37.00 -30.00   52
 12  \w    -16.00  59.00   0.50    0.05    --   47.70 -19.00  60.00  150
 13  \w    112.00 153.00   0.50    0.05    --  104.75  90.00 -60.00   82
 14  \w    102.00 178.00   0.50    0.05    --  104.75  15.00-120.00  152
 15  \w     52.00 123.00   0.50    0.05    --  104.75 -90.00-174.00  142
 16  \w     37.00 116.00   0.50    0.05    --  104.75 -15.00-180.00  158
 17  \w     33.00 128.00   0.50    0.05    --  104.75 -77.00-180.00  190
 18  \w     20.00  74.00   0.50    0.05    --   47.70 -90.00-174.00  108
 19  \w    -23.00   5.00   0.50    0.05    --   47.70 -90.00-174.00   56
 20  \w   -117.00 -80.00   0.50    0.05    --  -47.70-125.00  60.00   74
 21  \w   -119.00 -73.00   0.50    0.05    --  -47.70-125.00 -90.00   92
 22  \w   -118.00 -93.00   0.50    0.05    --  -47.70-125.00-120.00   50
 23  \w   -175.00 -77.00   0.50    0.05    -- -102.00 -90.00-174.00  196
 24  \w   -115.00 -28.00   0.50    0.05    -- -102.00  30.00 -60.00  174
 25  \w    -73.00 -46.00   0.50    0.05    -- -102.00 125.00 -30.00   54
 26  \w   -120.00 -95.00   0.50    0.05    -- -102.00  90.00 -60.00   50
 27  \w   -117.00 -79.00   0.50    0.05    -- -102.00 125.00 -30.00   76
 28  \w   -116.00 -34.00   0.50    0.05    -- -102.00 125.00  60.00  164
 29  \w   -115.00 -30.00   0.50    0.05    -- -102.00  45.00 150.00  170
 30  \w   -170.00 -95.00   0.50    0.05    -- -102.00 -30.00 120.00  150
 31  \w   -166.00 -90.00   0.50    0.05    -- -102.00 -45.00  30.00  152
;
_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      -0.1103455000
_diffrn_orient_matrix_UB_12      -0.0534099000
_diffrn_orient_matrix_UB_13      0.0292810000
_diffrn_orient_matrix_UB_21      0.0869812000
_diffrn_orient_matrix_UB_22      -0.0056751000
_diffrn_orient_matrix_UB_23      0.0576463000
_diffrn_orient_matrix_UB_31      0.0048855000
_diffrn_orient_matrix_UB_32      0.1237234000
_diffrn_orient_matrix_UB_33      0.0292293000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            34975
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.861
_diffrn_reflns_theta_min         3.870
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44876
_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            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         6.507
_refine_diff_density_min         -3.350
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     610
_refine_ls_number_reflns         11780
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0732
_refine_ls_R_factor_gt           0.0635
_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^)+(0.0827P)^2^+109.5690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1826
_refine_ls_wR_factor_ref         0.1912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11293
_reflns_number_total             11780
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound17
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_original_cell_volume        2943.93(8)
_cod_database_code               7710613
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1Si1U1
_shelx_estimated_absorpt_t_max   0.261
_shelx_estimated_absorpt_t_min   0.261
_diffrn_oxdiff_digest_frames
;
019fde2b74fe3b1279744c77f9bb28b098033741916
;
_diffrn_oxdiff_digest_hkl
;
01b0994c2a70cc2781d2fb96b3fd7c229d5435
;
_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. Rigid bond restraints
 C15, Si4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C15 \\sim Si4: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C16) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C4) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(C1) = Uanis(C2)
Uanis(C15) = Uanis(C25)
4.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C36(H36), C37(H37), C38(H38), C39(H39),
 C40(H40), C42(H42), C43(H43), C44(H44), C45(H45), C46(H46), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
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              35867
_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 2.197
_oxdiff_exptl_absorpt_empirical_full_min 0.657