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_4134822
_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         'C92 H169 N2 O31 Si14 U3, 3(C2 N), C4 O'
_chemical_formula_sum            'C102 H189 N5 O32 Si14 U3'
_chemical_formula_weight         3104.92
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 92.053(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.266(4)
_cell_length_b                   31.423(6)
_cell_length_c                   24.877(5)
_cell_measurement_reflns_used    319
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.2
_cell_measurement_theta_min      1.095
_cell_volume                     15051(5)
_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      100.19
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.1068
_diffrn_reflns_av_unetI/netI     0.1743
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            55747
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.654
_diffrn_reflns_theta_max         24.654
_diffrn_reflns_theta_min         1.058
_exptl_absorpt_coefficient_mu    3.393
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.5104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       Rod
_exptl_crystal_F_000             6256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         3.010
_refine_diff_density_min         -2.911
_refine_diff_density_rms         0.227
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     867
_refine_ls_number_reflns         25090
_refine_ls_number_restraints     263
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.1831
_refine_ls_R_factor_gt           0.0943
_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^)+(0.1252P)^2^+245.4089P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2271
_refine_ls_wR_factor_ref         0.2844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12484
_reflns_number_total             25090
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00990_si_002.cif
_cod_data_source_block           complex_2
_cod_database_code               4134822
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
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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. Restrained distances
 C95-C96
 1.5 with sigma of 0.01
 O32-C96
 1.4 with sigma of 0.01
 C95-O32
 2.4 with sigma of 0.01
 C96-C97
 2.4 with sigma of 0.01
 C31-C33 \\sim C19-C21 \\sim C32-C34 \\sim C20-C22 \\sim C33-C35 \\sim C21-C23
 with sigma of 0.01
 C34-C36 \\sim C22-C24 \\sim C35-C31 \\sim C23-C19 \\sim C36-C32 \\sim C24-C20
 with sigma of 0.01
 C31-C32 \\sim C19-C20 \\sim C32-C33 \\sim C20-C21 \\sim C33-C34 \\sim C21-C22
 with sigma of 0.01
 C34-C35 \\sim C22-C23 \\sim C35-C36 \\sim C23-C24 \\sim C36-C31 \\sim C24-C19
 with sigma of 0.01
 C31-C33 \\sim C32-C34 \\sim C33-C35 \\sim C34-C36 \\sim C35-C31 \\sim C36-C32
 with sigma of 0.01
 C31-C32 \\sim C32-C33 \\sim C33-C34 \\sim C34-C35 \\sim C35-C36 \\sim C36-C31
 with sigma of 0.01
 C61-C63 \\sim C62-C64 \\sim C63-C65 \\sim C64-C66 \\sim C65-C61 \\sim C66-C62
 with sigma of 0.01
 C61-C62 \\sim C62-C63 \\sim C63-C64 \\sim C64-C65 \\sim C65-C66 \\sim C66-C61
 with sigma of 0.01
 C79-C80 \\sim C80-C81 \\sim C81-C82 \\sim C82-C83 \\sim C83-C84 \\sim C84-C79
 with sigma of 0.01
 C79-C81 \\sim C80-C82 \\sim C81-C83 \\sim C82-C84 \\sim C83-C79 \\sim C84-C80
 with sigma of 0.01
 C25-C26 \\sim C26-C27 \\sim C27-C28 \\sim C28-C29 \\sim C29-C30 \\sim C30-C25
 with sigma of 0.01
 C25-C27 \\sim C26-C28 \\sim C27-C29 \\sim C28-C30 \\sim C29-C25 \\sim C30-C26
 with sigma of 0.01
 C25-C28 \\sim C26-C29 \\sim C27-C30
 with sigma of 0.01
 C85-N1 \\sim C99-N2 \\sim C101-N3 \\sim C87-N5 \\sim C103-N4
 with sigma of 0.01
 C86-N1 \\sim C100-N2 \\sim C102-N3 \\sim C88-N5 \\sim C104-N4
 with sigma of 0.01
 C85-C86 \\sim C99-C100 \\sim C101-C102 \\sim C87-C88 \\sim C103-C104
 with sigma of 0.01
 C96-O32 \\sim C97-O32
 with sigma of 0.01
 C95-C96 \\sim C97-C98
 with sigma of 0.01
 C95-O32 \\sim C98-O32
 with sigma of 0.01
 C95-C97 \\sim C96-C98
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C31) = Uanis(C61)
Uanis(C73) = Uanis(C74) = Uanis(C75) = Uanis(C76) = Uanis(C77) = Uanis(C78)
Uanis(C49) = Uanis(C50) = Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54) =
Uanis(C79)
Uanis(C43) = Uanis(C44) = Uanis(C45) = Uanis(C46) = Uanis(C47) = Uanis(C48)
Uanis(C103) = Uanis(C104)
Uanis(C85) = Uanis(C86)
Uanis(Si13) = Uanis(Si12)
Uanis(C91) = Uanis(C92) = Uanis(C93) = Uanis(C94) = Uanis(C2)
Uanis(O21) = Uanis(O31) = Uanis(O32)
Uanis(O3) = Uanis(O4)
Uanis(C79) = Uanis(C80) = Uanis(C81) = Uanis(C82) = Uanis(C83) = Uanis(C84)
Uanis(O7) = Uanis(O8) = Uanis(O13) = Uanis(O30) = Uanis(O20) = Uanis(O14) =
Uanis(O9) = Uanis(O23)
Uiso(C95) = Uiso(C96) = Uiso(C97) = Uiso(C98)
Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18)
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24)
Uanis(C31) = Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36)
Uanis(C61) = Uanis(C62) = Uanis(C63) = Uanis(C64) = Uanis(C65) = Uanis(C66)
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30)
Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60)
Uanis(C1) = Uanis(C2) = Uanis(C3) = Uanis(C4) = Uanis(C5) = Uanis(C6)
Uanis(C7) = Uanis(C8) = Uanis(C9) = Uanis(C10) = Uanis(C11) = Uanis(C12)
4.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), C60(H60), C61(H61), C67(H67), C73(H73)
4.b Secondary CH2 refined with riding coordinates:
 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), C55(H55A,H55B), C56(H56A,H56B), C57(H57A,H57B), C58(H58A,
 H58B), C59(H59A,H59B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B),
 C65(H65A,H65B), C66(H66A,H66B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,H70B),
  C71(H71A,H71B), C72(H72A,H72B), 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), C92(H92A,H92B), C93(H93A,H93B)
4.c Idealised Me refined as rotating group:
 C85(H85A,H85B,H85C), C91(H91A,H91B,H91C), C94(H94A,H94B,H94C), C103(H10C,H10D,
 H10E)
;
_smtbx_masks_void_probe_radius   0.2
_smtbx_masks_void_truncation_radius 0.2
_shelx_res_checksum              1521
_shelx_hkl_checksum              28126
_shelx_fab_checksum              19177
_olex2_submission_special_instructions 'No special instructions were received'