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_7710616
_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         'C57 H78 O Si6 U'
_chemical_formula_sum            'C57 H78 O Si6 U'
_chemical_formula_weight         1185.76
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-05
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3718(2)
_cell_length_b                   15.3179(3)
_cell_length_c                   28.4830(5)
_cell_measurement_reflns_used    15982
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      75.7930
_cell_measurement_theta_min      3.6150
_cell_volume                     5834.11(18)
_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 0.968
_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     88.00 127.00   0.50    0.30    --  104.75 110.00-125.00   78
  2  \w    112.00 173.00   0.50    0.30    --  104.75  99.00 -25.00  122
  3  \w    -25.00  36.00   0.50    0.16    --   46.95 -29.00 -14.00  122
  4  \w    -16.00  28.00   0.50    0.16    --   46.95 -19.00-150.00   88
  5  \w     -3.00  23.00   0.50    0.16    --  -46.95  19.00-120.00   52
  6  \w    -67.00 -29.00   0.50    0.30    -- -102.00  61.00-180.00   76
  7  \w   -114.00 -89.00   0.50    0.16    --  -46.95-125.00 120.00   50
  8  \w   -153.00 -96.00   0.50    0.30    -- -102.00 -29.00 -14.00  114
  9  \w   -109.00 -83.00   0.50    0.16    --  -46.95-125.00-180.00   52
 10  \w     40.00  65.00   0.50    0.30    --  104.75 -94.00-180.00   50
 11  \w     74.00 107.00   0.50    0.30    --  104.75 -94.00-180.00   66
 12  \w     45.00  72.00   0.50    0.30    --  104.75 -61.00-150.00   54
 13  \w     37.00  72.00   0.50    0.30    --  104.75 -61.00-120.00   70
 14  \w     34.00  73.00   0.50    0.30    --  104.75 -61.00  30.00   78
 15  \w     34.00  60.00   0.50    0.30    --  104.75 -61.00  60.00   52
 16  \w     39.00  64.00   0.50    0.30    --  104.75 -61.00 120.00   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      -0.0181788000
_diffrn_orient_matrix_UB_12      -0.0188985000
_diffrn_orient_matrix_UB_13      -0.0524296000
_diffrn_orient_matrix_UB_21      -0.0400950000
_diffrn_orient_matrix_UB_22      0.0935449000
_diffrn_orient_matrix_UB_23      -0.0067541000
_diffrn_orient_matrix_UB_31      0.1063916000
_diffrn_orient_matrix_UB_32      0.0320373000
_diffrn_orient_matrix_UB_33      -0.0113524000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0591
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            23646
_diffrn_reflns_point_group_measured_fraction_full 0.940
_diffrn_reflns_point_group_measured_fraction_max 0.888
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.496
_diffrn_reflns_theta_min         3.103
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.276
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87589
_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    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             2416
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.411
_refine_diff_density_min         -2.196
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details
;
 Flack x determined using 3514 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.026(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         10877
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0454P)^2^+7.6087P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1022
_reflns_Friedel_coverage         0.665
_reflns_Friedel_fraction_full    0.869
_reflns_Friedel_fraction_max     0.790
_reflns_number_gt                9736
_reflns_number_total             10877
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt01730j2.cif
_cod_data_source_block           compound16
_cod_depositor_comments
'Adding full bibliography for 7710605--7710617.cif.'
_cod_database_code               7710616
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1Si1O1U1
_shelx_estimated_absorpt_t_max   0.457
_shelx_estimated_absorpt_t_min   0.457
_diffrn_oxdiff_digest_frames
;
01ca02c132823419043351892edf55385b000584e33
;
_diffrn_oxdiff_digest_hkl
;
01046d0ccf86513a5a154e4764655fef83b85e
;
_reflns_odcompleteness_completeness 99.71
_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. Uiso/Uaniso restraints and constraints
Uanis(C34) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C35(H35), C36(H36), C37(H37), C38(H38),
 C39(H39), C41(H41), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48), C49(H49),
  C50(H50), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57), C58(H58)
3.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              22188
_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 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.802