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_7710607
_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         'C51 H74 N2 Si4 U'
_chemical_formula_sum            'C51 H74 N2 Si4 U'
_chemical_formula_weight         1065.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 91.0730(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5053(3)
_cell_length_b                   11.6123(2)
_cell_length_c                   20.7096(3)
_cell_measurement_reflns_used    19932
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.6180
_cell_measurement_theta_min      4.3040
_cell_volume                     5170.82(14)
_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 0.998
_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    -25.00  60.00   0.50    0.14    --   47.70 -37.00 -60.00  170
  2  \w     61.00  87.00   0.50    0.55    --  104.75 -88.00  62.00   52
  3  \w     94.00 177.00   0.50    0.55    --  104.75  45.00  90.00  166
  4  \w    117.00 178.00   0.50    0.55    --  104.75  30.00 120.00  122
  5  \w     97.00 178.00   0.50    0.55    --  104.75  30.00 150.00  162
  6  \w     83.00 178.00   0.50    0.55    --  104.75  88.00 178.00  190
  7  \w    -21.00  14.00   0.50    0.14    --  -47.70  88.00 178.00   70
  8  \w    -21.00  75.00   0.50    0.14    --   47.70 -88.00  62.00  192
  9  \w    -75.00 -28.00   0.50    0.14    --  -47.70  88.00 178.00   94
 10  \w   -100.00 -48.00   0.50    0.55    -- -102.00  45.00  60.00  104
 11  \w   -115.00 -78.00   0.50    0.55    -- -102.00  45.00 -30.00   74
 12  \w   -113.00 -29.00   0.50    0.55    -- -102.00  61.00-180.00  168
 13  \w   -119.00 -93.00   0.50    0.14    --  -47.70-125.00  60.00   52
 14  \w   -175.00-132.00   0.50    0.55    -- -102.00 -88.00  62.00   86
 15  \w   -108.00 -71.00   0.50    0.14    --  -47.70-125.00-150.00   74
 16  \w   -115.00 -57.00   0.50    0.55    -- -102.00  88.00 178.00  116
;
_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      -0.0265123000
_diffrn_orient_matrix_UB_12      -0.0610074000
_diffrn_orient_matrix_UB_13      -0.0604888000
_diffrn_orient_matrix_UB_21      0.0196823000
_diffrn_orient_matrix_UB_22      0.1028844000
_diffrn_orient_matrix_UB_23      -0.0419166000
_diffrn_orient_matrix_UB_31      0.0636029000
_diffrn_orient_matrix_UB_32      -0.0575095000
_diffrn_orient_matrix_UB_33      -0.0106383000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33150
_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         75.918
_diffrn_reflns_theta_min         4.112
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.968
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63705
_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    1.369
_exptl_crystal_description       block
_exptl_crystal_F_000             2168
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.268
_refine_diff_density_min         -1.263
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         10343
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+5.2539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0728
_refine_ls_wR_factor_ref         0.0745
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9502
_reflns_number_total             10343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound10
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710607
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1U1Si1
_shelx_estimated_absorpt_t_max   0.503
_shelx_estimated_absorpt_t_min   0.436
_diffrn_oxdiff_digest_frames
;
0128faa555f9391e24d1279570f7486ada018929907
;
_diffrn_oxdiff_digest_hkl
;
01c5d0bb6f4295e5973bc9aa264b93db4fcba5
;
_reflns_odcompleteness_completeness 99.94
_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 Ternary CH refined with riding coordinates:
 C26(H26), C32(H32)
2.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,
 H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C37(H37A,H37B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C13(H13), C15(H15), C16(H16), C41(H41), C42(H42),
 C43(H43), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C51(H51)
2.d 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              60335
_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 1.377
_oxdiff_exptl_absorpt_empirical_full_min 0.771