Structure and small molecule activation reactivity of a metallasilsesquioxane of divalent ytterbium.
Willauer, Aurélien R; Dabrowska, Anna M.; Scopelliti, Rosario; Mazzanti, Marinella; Chemical communications (Cambridge, England) 56 (2020) 8936–8939; doi:10.1039/d0cc04197a

data_7126814
_publ_section_title
;
 Structure and small molecule activation reactivity of a
 metallasilsesquioxane of divalent ytterbium.
;
_journal_issue                   63
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              8936
_journal_page_last               8939
_journal_paper_doi               10.1039/d0cc04197a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety         '2(C49 H94 O13 Si8 Yb)'
_chemical_formula_sum            'C98 H188 O26 Si16 Yb2'
_chemical_formula_weight         2577.99
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-05-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_audit_update_record
;
2020-06-02 deposited with the CCDC.	2020-07-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.570(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.788(3)
_cell_length_b                   30.084(5)
_cell_length_c                   25.587(3)
_cell_measurement_reflns_used    163
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      3
_cell_measurement_theta_min      22
_cell_volume                     12922(3)
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1478
_diffrn_reflns_av_unetI/netI     0.1419
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            110312
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        23.999
_diffrn_reflns_theta_max         23.999
_diffrn_reflns_theta_min         1.045
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_T_max  0.6868
_exptl_absorpt_correction_T_min  0.5356
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1136 before and 0.0972 after correction.
The Ratio of minimum to maximum transmission is 0.7798.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5392
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.228
_exptl_crystal_size_min          0.216
_refine_diff_density_max         1.657
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.230
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1340
_refine_ls_number_reflns         19944
_refine_ls_number_restraints     1687
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1960
_refine_ls_R_factor_gt           0.1206
_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^)+(0.0001P)^2^+754.2104P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2536
_refine_ls_wR_factor_ref         0.2935
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11826
_reflns_number_total             19944
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04197a2.cif
_cod_data_source_block           ad40
_cod_depositor_comments
'Adding full bibliography for 7126813--7126814.cif.'
_cod_database_code               7126814
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.717
_shelx_estimated_absorpt_t_min   0.637
_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
 C94-C89 \\sim C89-C90 \\sim C91-C90 \\sim C91-C92 \\sim C92-C93 \\sim C94-C93
\\sim C95-C100 \\sim C100-
 C99 \\sim C99-C98 \\sim C98-C97 \\sim C97-C96 \\sim C95-C96
 with sigma of 0.02
 Si16-C89 \\sim Si16-C95
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C89 \\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim
C97 \\sim C98 \\sim C99 \\sim C100: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O26 \\sim C101 \\sim C102 \\sim C103 \\sim C104: within 2A with sigma of 0.02
and sigma for terminal atoms of 0.04 within 2A
C25 \\sim C30 \\sim C29 \\sim C28 \\sim C27 \\sim C26: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
O13 \\sim C49 \\sim C48 \\sim C47 \\sim C46: within 2A with sigma of 0.02 and
sigma for terminal atoms of 0.04 within 2A
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C95)=Sof(H95)=Sof(C96)=Sof(H96A)=Sof(H96B)=Sof(C97)=Sof(H97A)=Sof(H97B)=
 Sof(C98)=Sof(H98A)=Sof(H98B)=Sof(C99)=Sof(H99A)=Sof(H99B)=Sof(C100)=Sof(H10A)=
 Sof(H10B)=1-FVAR(1)
 Sof(C89)=Sof(H89)=Sof(C90)=Sof(H90A)=Sof(H90B)=Sof(C91)=Sof(H91A)=Sof(H91B)=
 Sof(C92)=Sof(H92A)=Sof(H92B)=Sof(C93)=Sof(H93A)=Sof(H93B)=Sof(C94)=Sof(H94A)=
 Sof(H94B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C7(H7), C13(H13), C19(H19), C25(H25), C34(H34), C40(H40), C50(H50),
 C56(H56), C62(H62), C68(H68), C74(H74), C83(H83), C89(H89), C95(H95)
6.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(H10K,H10L), 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),
 C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B), C39(H39A,H39B),
  C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,
 H45B), C46(H46A,H46B), C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B),
 C51(H51A,H51B), C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
  C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B), C61(H61A,
 H61B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B),
 C67(H67A,H67B), C69(H69A,H69B), C70(H70A,H70B), C71(H71A,H71B), C72(H72A,H72B),
  C73(H73A,H73B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A,H77B), C78(H78A,
 H78B), C79(H79A,H79B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B),
 C87(H87A,H87B), C88(H88A,H88B), C90(H90A,H90B), C91(H91A,H91B), C92(H92A,H92B),
  C93(H93A,H93B), C94(H94A,H94B), C96(H96A,H96B), C97(H97A,H97B), C98(H98A,
 H98B), C99(H99A,H99B), C100(H10A,H10B), C101(H10C,H10D), C102(H10E,H10F),
 C103(H10G,H10H), C104(H10I,H10J)
6.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C80(H80A,H80B,
 H80C), C81(H81A,H81B,H81C), C82(H82A,H82B,H82C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              26616
_shelx_hkl_checksum              42671
_shelx_fab_checksum              51959
_olex2_submission_special_instructions 'No special instructions were received'