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_4134825
_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         'C0.5 Cl, C92 H155 Li O26 Si14 U'
_chemical_formula_sum            'C92.5 H171 Cl Li O26 Si14 U'
_chemical_formula_weight         2372.96
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2019.09.11 svn.r3662 for OlexSys, GUI svn.r5938)
;
_cell_angle_alpha                78.946(4)
_cell_angle_beta                 77.534(3)
_cell_angle_gamma                64.451(3)
_cell_formula_units_Z            2
_cell_length_a                   14.417(4)
_cell_length_b                   15.026(4)
_cell_length_c                   30.501(9)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    110.0
_cell_measurement_theta_max      25.498
_cell_measurement_theta_min      2.3295
_cell_volume                     5784(3)
_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      110.0
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.942
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0898
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.942
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            43951
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.942
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.578
_diffrn_reflns_theta_min         0.688
_exptl_absorpt_coefficient_mu    1.637
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6237
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.362
_exptl_crystal_description       Plate
_exptl_crystal_F_000             2484
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.905
_refine_diff_density_min         -2.726
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1022
_refine_ls_number_reflns         22790
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0826
_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^)+(0.1140P)^2^+81.8972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2139
_refine_ls_wR_factor_ref         0.2433
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16378
_reflns_number_total             22790
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00990_si_002.cif
_cod_data_source_block           complex_5
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_formula_sum        'C92.50 H171 Cl Li O26 Si14 U'
_cod_database_code               4134825
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 C93-Cl1
 1.75 with sigma of 0.01
 Cl1-Cl2_$1
 3.1 with sigma of 0.01
 Cl1-Cl2_$1 \\sim Cl1-Cl2B_$1
 with sigma of 0.01
 C93-Cl1 \\sim C93-Cl2_$1 \\sim C93-Cl2B_$1
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48)
Uanis(C85) = Uanis(C86) = Uanis(O25) = Uanis(C87) = Uanis(C88)
Uanis(C89) = Uanis(C90) = Uanis(C91) = Uanis(C92)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12)
Uanis(C7) = Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) =
Uanis(C36)
Uanis(C67) = Uanis(C68) = Uanis(C69) = Uanis(C70) = Uanis(C70A) = Uanis(C71) =
Uanis(C71A) = Uanis(C72) = Uanis(C72A)
Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C58A) = Uanis(C59) =
Uanis(C59A) = Uanis(C60) = Uanis(C60A)
Uanis(C61) = Uanis(C62) = Uanis(C63) = Uanis(C64) = Uanis(C64A) = Uanis(C65) =
Uanis(C65A) = Uanis(C66) = Uanis(C66A)
4. Others
 Fixed Sof: Cl2(0.25) C93(0.5) Cl2B(0.25) C58(0.5) H58A(0.5) H58B(0.5)
 C59(0.5) H59A(0.5) H59B(0.5) C60(0.5) H60A(0.5) H60B(0.5) C58A(0.5) H58C(0.5)
 H58D(0.5) C59A(0.5) H59C(0.5) H59D(0.5) C60A(0.5) H60C(0.5) H60D(0.5) C64(0.5)
 H64A(0.5) H64B(0.5) C65(0.5) H65A(0.5) H65B(0.5) C66(0.5) H66A(0.5) H66B(0.5)
 C64A(0.5) H64C(0.5) H64D(0.5) C65A(0.5) H65C(0.5) H65D(0.5) C66A(0.5)
 H66C(0.5) H66D(0.5) C70(0.5) H70A(0.5) H70B(0.5) C71(0.5) H71A(0.5) H71B(0.5)
 C72(0.5) H72A(0.5) H72B(0.5) C70A(0.5) H70C(0.5) H70D(0.5) C71A(0.5) H71C(0.5)
 H71D(0.5) C72A(0.5) H72C(0.5) H72D(0.5) Cl1(0.5)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C31(H31), C37(H37), C43(H43),
 C49(H49), C73(H73), C79(H79)
5.b Secondary CH2 refined with riding coordinates:
 C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C58A(H58C,H58D), C59A(H59C,
 H59D), C60A(H60C,H60D), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B),
 C64A(H64C,H64D), C65A(H65C,H65D), C66A(H66C,H66D), C70(H70A,H70B), C71(H71A,
 H71B), C72(H72A,H72B), C70A(H70C,H70D), C71A(H71C,H71D), C72A(H72C,H72D),
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C8(H8A,H8B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B),
 C15(H15A,H15B), C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B),
  C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C26(H26A,
 H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
 C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B),
  C54(H54A,H54B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,
 H77B), C78(H78A,H78B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B),
 C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B),
  C88(H88A,H88B), C89(H89A,H89B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B)
;
_smtbx_masks_void_probe_radius   0.2
_smtbx_masks_void_truncation_radius 0.2
_shelx_res_checksum              2497
_shelx_hkl_checksum              75169
_shelx_fab_checksum              8411
_olex2_submission_special_instructions 'No special instructions were received'