Uranyl oxo silylation promoted by silsesquioxane coordination.
Assefa, Mikiyas K.; Wu, Guang; Hayton, Trevor W.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c00990

data_4134823
_publ_section_title
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 Uranyl oxo silylation promoted by silsesquioxane coordination.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c00990
_journal_year                    2020
_chemical_formula_moiety         'C84 H80 O24 Si14 U'
_chemical_formula_sum            'C84 H154 O24 Si14 U'
_chemical_formula_weight         2179.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           64
_space_group_name_Hall           '-C 2ac 2'
_space_group_name_H-M_alt        'C m c e'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-07
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9919(14)
_cell_length_b                   25.2308(18)
_cell_length_c                   21.8579(16)
_cell_measurement_reflns_used    5914
_cell_measurement_temperature    110.04
_cell_measurement_theta_max      25.134
_cell_measurement_theta_min      2.464
_cell_volume                     10473.9(13)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL n/a (Sheldrick, 2008)'
_diffrn_ambient_temperature      110.04
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            24395
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.170
_diffrn_reflns_theta_min         1.614
_exptl_absorpt_coefficient_mu    1.775
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.7012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       Plate
_exptl_crystal_F_000             4552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.954
_refine_diff_density_min         -1.456
_refine_diff_density_rms         0.172
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         5986
_refine_ls_number_restraints     207
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0949
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0855P)^2^+225.8738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1784
_refine_ls_wR_factor_ref         0.1936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4542
_reflns_number_total             5986
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00990_si_002.cif
_cod_data_source_block           complex_3
_cod_original_sg_symbol_Hall     '-C 2bc 2'
_cod_database_code               4134823
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C13-C16A \\sim C14A-C17A \\sim C15A-C18A \\sim C16A-C13 \\sim C17A-C14A \\sim
C18A-C15A
 with sigma of 0.01
 C13-C15A \\sim C14A-C16A \\sim C15A-C17A \\sim C16A-C18A \\sim C17A-C13 \\sim
C18A-C14A
 with sigma of 0.01
 C13-C14A \\sim C14A-C15A \\sim C15A-C16A \\sim C16A-C17A \\sim C17A-C18A \\sim
C18A-C13
 with sigma of 0.01
 C13-C16 \\sim C14-C17 \\sim C15-C18 \\sim C16-C13 \\sim C17-C14 \\sim C18-C15
 with sigma of 0.01
 C13-C15 \\sim C14-C16 \\sim C15-C17 \\sim C16-C18 \\sim C17-C13 \\sim C18-C14
 with sigma of 0.01
 C13-C14 \\sim C14-C15 \\sim C15-C16 \\sim C16-C17 \\sim C17-C18 \\sim C18-C13
 with sigma of 0.01
 C7-C10 \\sim C8-C11 \\sim C9-C12 \\sim C10-C7 \\sim C11-C8 \\sim C12-C9
 with sigma of 0.01
 C7-C9 \\sim C8-C10 \\sim C9-C11 \\sim C10-C12 \\sim C11-C7 \\sim C12-C8
 with sigma of 0.01
 C7-C8 \\sim C8-C9 \\sim C9-C10 \\sim C10-C11 \\sim C11-C12 \\sim C12-C7
 with sigma of 0.01
 C7-C10A \\sim C8A-C11A \\sim C9A-C12A \\sim C10-C7 \\sim C11A-C8A \\sim
C12A-C9A
 with sigma of 0.01
 C7-C9A \\sim C8A-C10A \\sim C9A-C11A \\sim C10A-C12A \\sim C11A-C7 \\sim
C12A-C8A
 with sigma of 0.01
 C7-C8A \\sim C8A-C9A \\sim C9A-C10A \\sim C10A-C11A \\sim C11A-C12A \\sim
C12A-C7
 with sigma of 0.01
 C1-C2 \\sim C2-C3 \\sim C3-C4 \\sim C4-C5 \\sim C5-C6 \\sim C6-C1
 with sigma of 0.01
 C1-C3 \\sim C2-C4 \\sim C3-C5 \\sim C4-C6 \\sim C5-C1 \\sim C6-C2
 with sigma of 0.01
 C1-C4 \\sim C2-C5 \\sim C3-C6 \\sim C4-C1 \\sim C5-C2 \\sim C6-C3
 with sigma of 0.01
 C19-C20 \\sim C20-C21 \\sim C21-C22 \\sim C22-C23 \\sim C23-C24 \\sim C24-C19
 with sigma of 0.01
 C19-C21 \\sim C20-C22 \\sim C21-C23 \\sim C22-C24 \\sim C23-C19 \\sim C24-C20
 with sigma of 0.01
 C19-C22 \\sim C20-C23 \\sim C21-C24 \\sim C22-C19 \\sim C23-C20 \\sim C24-C21
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6)
Uanis(C14) = Uanis(C18) = Uanis(C14A) = Uanis(C18A)
Uanis(Si2) = Uanis(Si3) = Uanis(Si5)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12) =
Uanis(C8A) = Uanis(C9A) = Uanis(C10A) = Uanis(C11A) = Uanis(C12A)
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30)
4. Others
 Fixed Sof: C8(0.5) H8A(0.5) H8B(0.5) C9(0.5) H9A(0.5) H9B(0.5) C10(0.5)
 H10A(0.5) H10B(0.5) C11(0.5) H11A(0.5) H11B(0.5) C12(0.5) H12A(0.5) H12B(0.5)
 C8A(0.5) H8AA(0.5) H8AB(0.5) C9A(0.5) H9AA(0.5) H9AB(0.5) C10A(0.5) H10C(0.5)
 H10D(0.5) C11A(0.5) H11C(0.5) H11D(0.5) C12A(0.5) H12C(0.5) H12D(0.5) C14(0.5)
 H14A(0.5) H14B(0.5) C15(0.5) H15A(0.5) H15B(0.5) C16(0.5) H16A(0.5) H16B(0.5)
 C17(0.5) H17A(0.5) H17B(0.5) C18(0.5) H18A(0.5) H18B(0.5) C14A(0.5) H14C(0.5)
 H14D(0.5) C15A(0.5) H15C(0.5) H15D(0.5) C16A(0.5) H16C(0.5) H16D(0.5)
 C17A(0.5) H17C(0.5) H17D(0.5) C18A(0.5) H18C(0.5) H18D(0.5) C2(0.5) C3(0.5)
 C5(0.5) C6(0.5) C20(0.5) C21(0.5) C22(0.5) C23(0.5) C24(0.5) C26(0.5) C27(0.5)
 C28(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B),
 C8A(H8AA,H8AB), C9A(H9AA,H9AB), C10A(H10C,H10D), C11A(H11C,H11D), C12A(H12C,
 H12D), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B),
 C18(H18A,H18B), C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,
 H17D), C18A(H18C,H18D)
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_shelx_res_checksum              3448
_shelx_hkl_checksum              28755
_olex2_submission_special_instructions 'No special instructions were received'