Reactivity of a Lewis base supported uranium terminal imido metallocene towards small molecules
Li, Tongyu; Wang, Dongwei; Heng, Yi; Hou, Guohua; Zi, Guofu; Walter, Marc D.; Dalton Transactions  (2023) –; doi:10.1039/D3DT02165C

data_7713809
_publ_section_title
;
 Reactivity of a Lewis base supported uranium terminal imido metallocene
 towards small molecules
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02165C
_journal_year                    2023
_chemical_formula_moiety         'C35 H65 I N Si6 U'
_chemical_formula_sum            'C35 H65 I N Si6 U'
_chemical_formula_weight         1033.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-12-14
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-29 deposited with the CCDC.	2023-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.701(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2421(3)
_cell_length_b                   17.3258(3)
_cell_length_c                   24.2585(6)
_cell_measurement_reflns_used    6718
_cell_measurement_temperature    99.97(19)
_cell_measurement_theta_max      27.3260
_cell_measurement_theta_min      3.4770
_cell_volume                     4609.41(19)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.97(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6254
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.866
_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     28.00  72.25   0.75    1.62    --   12.53   0.00 120.00   59
  2  \w    -52.00 -16.00   0.75    1.62    --   12.53   0.00 120.00   48
  3  \w    -42.00  -6.00   0.75    3.00    --  -11.04 -77.00 -90.00   48
  4  \w     -7.00  84.50   0.75    3.00    --   12.53  57.00 150.00  122
  5  \w     29.00  58.25   0.75    3.00    --   12.53-165.00 -26.00   39
  6  \w     74.00 100.25   0.75    3.00    --   12.53 178.00  30.00   35
  7  \w    -15.00  12.00   0.75    3.00    --  -11.04 -99.00-180.00   36
  8  \w      3.00  37.50   0.75    3.00    --   12.53  57.00  60.00   46
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0082542000
_diffrn_orient_matrix_UB_12      0.0118954000
_diffrn_orient_matrix_UB_13      0.0285655000
_diffrn_orient_matrix_UB_21      -0.0511581000
_diffrn_orient_matrix_UB_22      0.0248355000
_diffrn_orient_matrix_UB_23      -0.0075367000
_diffrn_orient_matrix_UB_31      -0.0386863000
_diffrn_orient_matrix_UB_32      -0.0303013000
_diffrn_orient_matrix_UB_33      0.0050498000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0944
_diffrn_reflns_av_unetI/netI     0.1271
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.866
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            39104
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.866
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.867
_diffrn_reflns_theta_min         3.229
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.370
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65974
_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    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.853
_refine_diff_density_min         -1.105
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         11494
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1098
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0127P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7220
_reflns_number_total             11494
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02165c2.cif
_cod_data_source_block           compound14
_cod_original_cell_volume        4609.43(19)
_cod_database_code               7713809
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C1H1N1U1I1Si1
_shelx_estimated_absorpt_t_max   0.560
_shelx_estimated_absorpt_t_min   0.475
_diffrn_oxdiff_digest_frames
;
0137c7d91497a6d38afb4fb688c36d17e500459ffa9
;
_diffrn_oxdiff_digest_hkl
;
015d841b27f02e89dc3a8e8b6e897e0cc9df7b
;
_reflns_odcompleteness_completeness 99.74
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(C7) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C35)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C29) \\sim Ueq, Uanis(N1) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C7)
\\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C31) = Uanis(C29)
Uanis(C32) = Uanis(C31) = Uanis(C33) = Uanis(C30) = Uanis(C34) = Uanis(C29)
Uanis(C29) = Uanis(C30) = Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C17(H17), C19(H19), C30(H30), C31(H31), C33(H33), C34(H34)
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), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              10091
_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 1.598
_oxdiff_exptl_absorpt_empirical_full_min 0.798