Quantitative U=O bond activation in uranyl complexes via silyl radical transfer
Valerio, Leyla R.; Hakey, Brett; Brennessel, William W.; Matson, Ellen; Chemical Communications  (2022) –; doi:10.1039/D2CC04424B

data_7130611
_publ_section_title
;
 Quantitative U=O bond activation in uranyl complexes via silyl radical
 transfer
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D2CC04424B
_journal_year                    2022
_chemical_formula_moiety         'C56 H65 N5 O2 Si2 U, C4 H10 O'
_chemical_formula_sum            'C60 H75 N5 O3 Si2 U'
_chemical_formula_weight         1208.46
_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
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-05-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-07-26 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.1300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.21430(10)
_cell_length_b                   22.69980(10)
_cell_length_c                   19.21290(10)
_cell_measurement_reflns_used    63438
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      79.9400
_cell_measurement_theta_min      3.8710
_cell_volume                     5730.19(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015b)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2015a)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_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    -79.00 -19.00   0.50    0.73    --  -91.75  92.00 144.00  120
  2  \w    -77.00  26.00   0.50    0.18    --  -47.17  92.00 144.00  206
  3  \w    -16.00  28.00   0.50    0.18    --  -47.17  19.00 -60.00   88
  4  \w    -16.00  28.00   0.50    0.18    --  -47.17  19.00 -90.00   88
  5  \w    -16.00  28.00   0.50    0.18    --  -47.17  19.00-120.00   88
  6  \w     32.00 120.00   0.50    0.18    --   47.17  57.00-120.00  176
  7  \w     25.00 120.00   0.50    0.18    --   47.17  77.00 -90.00  190
  8  \w     32.00 120.00   0.50    0.18    --   47.17  57.00   0.00  176
  9  \w     25.00 120.00   0.50    0.18    --   47.17  77.00  30.00  190
 10  \w     25.00 120.00   0.50    0.18    --   47.17  77.00 150.00  190
 11  \w     32.00 120.00   0.50    0.18    --   47.17  57.00 120.00  176
 12  \w    101.00 178.00   0.50    0.73    --  113.25  45.00  30.00  154
 13  \w    101.00 178.00   0.50    0.73    --  113.25  30.00  90.00  154
 14  \w    101.00 178.00   0.50    0.73    --  113.25  30.00 -30.00  154
 15  \w    101.00 178.00   0.50    0.73    --  113.25  30.00 -60.00  154
 16  \w    101.00 178.00   0.50    0.73    --  113.25  30.00-180.00  154
 17  \w    101.00 178.00   0.50    0.73    --  113.25  45.00-150.00  154
 18  \w    100.00 178.00   0.50    0.73    --  113.25  15.00 -90.00  156
 19  \w    101.00 178.00   0.50    0.73    --  113.25  30.00 120.00  154
 20  \w    102.00 178.00   0.50    0.73    --  113.25  92.00 144.00  152
 21  \w     42.00 136.00   0.50    0.73    --  113.25 -77.00 150.00  188
 22  \w     42.00 136.00   0.50    0.73    --  113.25 -77.00  30.00  188
 23  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00 -30.00   74
 24  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00 -60.00   74
 25  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00 -90.00   74
 26  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00-120.00   74
 27  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00-180.00   74
 28  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00  30.00   74
 29  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00  60.00   74
 30  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00  90.00   74
 31  \w     42.00  79.00   0.50    0.73    --  113.25 -61.00 150.00   74
 32  \w    -19.00  77.00   0.50    0.18    --   47.17 -92.00  31.00  192
 33  \w     42.00 105.00   0.50    0.73    --  113.25 -92.00  31.00  126
 34  \w     42.00 106.00   0.50    0.73    --  113.25 -94.00-180.00  128
 35  \w     42.00 106.00   0.50    0.73    --  113.25 -94.00-120.00  128
 36  \w     42.00 106.00   0.50    0.73    --  113.25 -94.00  90.00  128
 37  \w   -119.00 -73.00   0.50    0.18    --  -47.17-125.00 120.00   92
 38  \w   -163.00 -80.00   0.50    0.73    --  -91.75 -92.00  31.00  166
 39  \w   -119.00 -73.00   0.50    0.18    --  -47.17-125.00-180.00   92
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0551539000
_diffrn_orient_matrix_UB_12      -0.0022503000
_diffrn_orient_matrix_UB_13      0.0747707000
_diffrn_orient_matrix_UB_21      0.0399736000
_diffrn_orient_matrix_UB_22      -0.0620810000
_diffrn_orient_matrix_UB_23      -0.0143736000
_diffrn_orient_matrix_UB_31      0.0954293000
_diffrn_orient_matrix_UB_32      0.0273621000
_diffrn_orient_matrix_UB_33      -0.0265680000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0565
_diffrn_reflns_av_unetI/netI     0.0280
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            97688
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        74.504
_diffrn_reflns_theta_max         80.443
_diffrn_reflns_theta_min         3.874
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.737
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
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    1.401
_exptl_crystal_description       plate
_exptl_crystal_F_000             2456
_exptl_crystal_size_max          0.226
_exptl_crystal_size_mid          0.125
_exptl_crystal_size_min          0.017
_refine_diff_density_max         1.707
_refine_diff_density_min         -1.873
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         12409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+6.0906P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0763
_refine_ls_wR_factor_ref         0.0776
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11542
_reflns_number_total             12409
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cc04424b2.cif
_cod_data_source_block           matlrv04
_cod_database_code               7130611
_shelx_shelxl_version_number     2019/2
_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 Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C59(H59A,H59B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C6(H6), C7(H7), C8(H8), C12(H12), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C28(H28),
  C30(H30), C37(H37), C39(H39), C44(H44), C45(H45), C47(H47), C48(H48)
2.c Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C34(H34A,H34B,H34C), C41(H41A,H41B,
 H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C49(H49A,H49B,H49C), C50(H50A,
 H50B,H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C54(H54A,H54B,H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,
 H57C), C60(H60A,H60B,H60C)
;
_shelx_res_checksum              82552
_shelx_hkl_checksum              19670
_olex2_submission_original_sample_id matlrv04
_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 1.635
_oxdiff_exptl_absorpt_empirical_full_min 0.701