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_7126813
_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         'C118 H214 N2 O28 Si16 Yb2'
_chemical_formula_sum            'C118 H214 N2 O28 Si16 Yb2'
_chemical_formula_weight         2904.42
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-05-28
_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                113.031(9)
_cell_angle_beta                 90.664(14)
_cell_angle_gamma                100.204(10)
_cell_formula_units_Z            2
_cell_length_a                   16.342(2)
_cell_length_b                   23.291(3)
_cell_length_c                   24.187(4)
_cell_measurement_reflns_used    364
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      3
_cell_measurement_theta_min      22
_cell_volume                     8305(2)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'EvalCCD (Duisenberg & Schreurs, 1990-2000)'
_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 0.984
_diffrn_measured_fraction_theta_max 0.969
_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  0.0738
_diffrn_reflns_av_unetI/netI     0.0924
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            107079
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.271
_exptl_absorpt_coefficient_mu    1.291
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1020 before and 0.0858 after correction.
The Ratio of minimum to maximum transmission is 0.6691.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3048
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.573
_refine_diff_density_rms         0.157
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1556
_refine_ls_number_reflns         36962
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1028
_refine_ls_R_factor_gt           0.0643
_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^)+(0.0642P)^2^+51.6927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25240
_reflns_number_total             36962
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc04197a2.cif
_cod_data_source_block           ad61
_cod_depositor_comments
'Adding full bibliography for 7126813--7126814.cif.'
_cod_database_code               7126813
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.820
_shelx_estimated_absorpt_t_min   0.747
_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
 C44-C43 \\sim C44-C45 \\sim C45-C46 \\sim C46-C47 \\sim C47-C48 \\sim C48-C43
\\sim C42-C37 \\sim C41-C42
 \\sim C40-C41 \\sim C39-C40 \\sim C38-C39 \\sim C38-C37
 with sigma of 0.02
 Si5-C37 \\sim Si5-C43
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim
C45 \\sim C46 \\sim C47 \\sim C48: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4. Others
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=
 Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=1-FVAR(1)
 Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(C42)=Sof(H42A)=
 Sof(H42B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C13(H13), C19(H19), C25(H25), C31(H31), C37(H37), C43(H43), C52(H52),
 C58(H58), C72(H72), C78(H78), C84(H84), C90(H90), C96(H96), C105(H105),
 C111(H111)
5.b Secondary CH2 refined with riding coordinates:
 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), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,
 H55B), C56(H56A,H56B), C57(H57A,H57B), C59(H59A,H59B), C60(H60A,H60B),
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B), C64(H64A,H64B), C65(H65A,H65B),
  C66(H66A,H66B), C67(H67A,H67B), C68(H68A,H68B), C69(H69A,H69B), C70(H70A,
 H70B), C71(H71A,H71B), C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B),
 C76(H76A,H76B), C77(H77A,H77B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B),
  C82(H82A,H82B), C83(H83A,H83B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,
 H87B), C88(H88A,H88B), C89(H89A,H89B), C91(H91A,H91B), C92(H92A,H92B),
 C93(H93A,H93B), C94(H94A,H94B), C95(H95A,H95B), C97(H97A,H97B), C98(H98A,H98B),
  C99(H99A,H99B), C100(H10A,H10B), C101(H10C,H10D), C106(H10N,H10O), C107(H10P,
 H10Q), C108(H10R,H10S), C109(H10T,H10U), C110(H11A,H11B), C112(H11C,H11D),
 C113(H11E,H11F), C114(H11G,H11H), C115(H11I,H11J), C116(H11K,H11L), C117(H11M,
 H11N), C118(H11O,H11P), C119(H11Q,H11R), C120(H12A,H12B), C121(H12C,H12D),
 C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
5.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C102(H10E,H10F,
 H10G), C103(H10H,H10I,H10J), C104(H10K,H10L,H10M)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              85125
_shelx_hkl_checksum              68222
_shelx_fab_checksum              59369
_olex2_submission_special_instructions 'No special instructions were received'