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_4134821
_publ_section_title
;
 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         'C51 H102 O15 Si10 U, C2.5 H6'
_chemical_formula_sum            'C53.5 H110 O15 Si10 U'
_chemical_formula_weight         1512.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/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                 106.277(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   25.785(3)
_cell_length_b                   13.9805(17)
_cell_length_c                   20.860(3)
_cell_measurement_reflns_used    970
_cell_measurement_temperature    99.97
_cell_measurement_theta_max      30.315
_cell_measurement_theta_min      1.845
_cell_volume                     7218.4(16)
_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      99.97
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'Bruker Apex II'
_diffrn_measurement_method       'Omega Scan'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0770
_diffrn_reflns_av_unetI/netI     0.1221
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33272
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.286
_diffrn_reflns_theta_min         1.457
_exptl_absorpt_coefficient_mu    2.470
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       Plate
_exptl_crystal_F_000             3132
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.066
_refine_diff_density_min         -2.405
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         15835
_refine_ls_number_restraints     551
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1386
_refine_ls_R_factor_gt           0.0785
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0658P)^2^+63.5823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9674
_reflns_number_total             15835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00990_si_002.cif
_cod_data_source_block           complex_1
_cod_original_cell_volume        7218.2(16)
_cod_original_formula_sum        'C53.50 H110 O15 Si10 U'
_cod_database_code               4134821
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C58-C59 \\sim C59-C60
 with sigma of 0.02
 C58-C60 \\sim C59-C59_$1
 with sigma of 0.01
 C49-C51A \\sim C50A-C52A \\sim C51A-C53A \\sim C52A-C54A \\sim C53A-C49A \\sim
C54A-C50A
 with sigma of 0.01
 C49-C50A \\sim C50A-C51A \\sim C51A-C52A \\sim C52A-C53A \\sim C53A-C54A \\sim
C54A-C49A
 with sigma of 0.01
 C49-C51A \\sim C49-C51 \\sim C50-C52 \\sim C51-C53 \\sim C52-C54 \\sim C53-C49
\\sim C54-C50
 with sigma of 0.01
 C49-C50A \\sim C49-C50 \\sim C50-C51 \\sim C51-C52 \\sim C52-C53 \\sim C53-C54
\\sim C54-C49
 with sigma of 0.01
 C13-C14 \\sim C13A-C14A \\sim C14A-C15A \\sim C15A-C16A \\sim C16A-C17A \\sim
C17A-C18A \\sim C18A-C13A
 with sigma of 0.01
 C13-C15 \\sim C13A-C15A \\sim C14A-C16A \\sim C15A-C17A \\sim C16A-C18A \\sim
C17A-C13A \\sim C18A-C14A
 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
 C13-C15 \\sim C14-C16 \\sim C15-C17 \\sim C16-C18 \\sim C17-C13 \\sim C18-C14
 with sigma of 0.01
 C40A-C41A \\sim C40-C41 \\sim C41-C42 \\sim C42-C43 \\sim C43-C44 \\sim
C44-C45 \\sim C45-C40
 with sigma of 0.01
 C40A-C42A \\sim C40-C42 \\sim C41-C43 \\sim C42-C44 \\sim C43-C45 \\sim
C44-C40 \\sim C45-C41
 with sigma of 0.01
 C40A-C41A \\sim C41A-C42A \\sim C42A-C43A \\sim C43A-C44A \\sim C44A-C45A
\\sim C45A-C40A
 with sigma of 0.01
 C40A-C42A \\sim C41A-C43A \\sim C42A-C44A \\sim C43A-C45A \\sim C44A-C40A
\\sim C45A-C41A
 with sigma of 0.01
 C49-C52 \\sim C50-C53 \\sim C51-C54 \\sim C49-C52A \\sim C50A-C53A \\sim
C51A-C54A
 with sigma of 0.01
 C49-C52 \\sim C13-C16 \\sim C14-C17 \\sim C15-C18 \\sim C13A-C16A \\sim
C14A-C17A \\sim C15A-C18A
 with sigma of 0.01
 C49-C52 \\sim C40-C43 \\sim C41-C44 \\sim C42-C45 \\sim C40A-C43A \\sim
C41A-C44A \\sim C42A-C45A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uiso(C58) = Uiso(C59) = Uiso(C60)
Uanis(C40) = Uanis(C41) = Uanis(C42) = Uanis(C43) = Uanis(C44) = Uanis(C45) =
Uanis(C40A) = Uanis(C41A) = Uanis(C42A) = Uanis(C43A) = Uanis(C44A) =
Uanis(C45A)
Uanis(C49) = Uanis(C50) = Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54) =
Uanis(C49A) = Uanis(C50A) = Uanis(C51A) = Uanis(C52A) = Uanis(C53A) =
Uanis(C54A)
Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18) =
Uanis(C13A) = Uanis(C14A) = Uanis(C15A) = Uanis(C16A) = Uanis(C17A) =
Uanis(C18A)
4. Others
 Fixed Sof: C13(0.5) H13(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) C13A(0.5) H13A(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) C40(0.5) H40(0.5) C41(0.5)
 H41A(0.5) H41B(0.5) C42(0.5) H42A(0.5) H42B(0.5) C43(0.5) H43A(0.5) H43B(0.5)
 C44(0.5) H44A(0.5) H44B(0.5) C45(0.5) H45A(0.5) H45B(0.5) C40A(0.5) H40A(0.5)
 C41A(0.5) H41C(0.5) H41D(0.5) C42A(0.5) H42C(0.5) H42D(0.5) C43A(0.5)
 H43C(0.5) H43D(0.5) C44A(0.5) H44C(0.5) H44D(0.5) C45A(0.5) H45C(0.5)
 H45D(0.5) C49(0.5) H49(0.5) C50(0.5) H50A(0.5) H50B(0.5) C51(0.5) H51A(0.5)
 H51B(0.5) C54(0.5) H54A(0.5) H54B(0.5) C53(0.5) C52(0.5) C49A(0.5) H49A(0.5)
 C54A(0.5) H54C(0.5) H54D(0.5) C53A(0.5) H53A(0.5) H53B(0.5) C52A(0.5)
 H52A(0.5) H52B(0.5) C51A(0.5) H51C(0.5) H51D(0.5) C50A(0.5) H50C(0.5)
 H50D(0.5) H60A(0.5) H60B(0.5)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C13A(H13A), C40(H40), C40A(H40A), C49(H49), C49A(H49A), C1(H1),
 C7(H7), C19(H19), C34(H34)
5.b Secondary CH2 refined with riding coordinates:
 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), C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,
 H44B), C45(H45A,H45B), C41A(H41C,H41D), C42A(H42C,H42D), C43A(H43C,H43D),
 C44A(H44C,H44D), C45A(H45C,H45D), C50(H50A,H50B), C51(H51A,H51B), C54(H54A,
 H54B), C54A(H54C,H54D), C53A(H53A,H53B), C52A(H52A,H52B), C51A(H51C,H51D),
 C50A(H50C,H50D), 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),
  C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
 C39(H39A,H39B), C59(H59A,H59B), C60(H60A,H60B)
5.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,
 H32B,H32C), C33(H33A,H33B,H33C), C58(H58A,H58B,H58C)
;
_smtbx_masks_void_probe_radius   0.2
_smtbx_masks_void_truncation_radius 0.2
_shelx_res_checksum              97180
_shelx_hkl_checksum              6842
_shelx_fab_checksum              38195
_olex2_submission_special_instructions 'No special instructions were received'