Isolation of R6Si6 Dianion, a Bridged Tricyclic Isomer of Dianionic Hexasilabenzene.
Li, Yang; Li, Jianfeng; Zhang, Jianying; Song, Haibin; Cui, Chunming; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b12163

data_4127047
_publ_section_title
;
 Isolation of R6Si6 Dianion, a Bridged Tricyclic Isomer of Dianionic
 Hexasilabenzene.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b12163
_journal_year                    2018
_chemical_formula_moiety         'C16 H32 K O7, C70 H98 K O7 Si6, 2(C4 H8 O)'
_chemical_formula_sum            'C94 H148 K2 O16 Si6'
_chemical_formula_weight         1780.86
_chemical_name_systematic
;
 ? 
;
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-07-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.190(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.036(5)
_cell_length_b                   19.079(3)
_cell_length_c                   23.557(3)
_cell_measurement_reflns_used    4828
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.0
_cell_volume                     9836(3)
_computing_cell_refinement
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_collection
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_data_reduction
'CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      113
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Rigaku Xtalab P200'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.1151
_diffrn_reflns_av_unetI/netI     0.1052
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            55935
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.230
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB(Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3848
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.968
_refine_diff_density_min         -0.458
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1274
_refine_ls_number_reflns         17172
_refine_ls_number_restraints     548
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.0819
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1040P)^2^+17.2620P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1914
_refine_ls_wR_factor_ref         0.2430
_reflns_number_gt                9529
_reflns_number_total             17172
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7b12163_si_005.cif
_cod_data_source_block           shelx_trans
_cod_database_code               4127047
_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
 O14-C29 = O14-C32 = O14A-C29A = O14A-C32A
 1.45 with sigma of 0.01
 C29-C30 = C30-C31 = C31-C32
 1.54 with sigma of 0.01
 C29A-C30A = C30A-C31A = C31A-C32A
 1.54 with sigma of 0.01
 C29-C31 = C30-C32 = C29A-C31A = C30A-C32A
 2.52 with sigma of 0.01
 O14-C30 = O14-C31 = O14A-C30A = O14A-C31A
 2.45 with sigma of 0.01
 C29-C32 = C29A-C32A
 2.4 with sigma of 0.01
 O7-C14 = O7-C15 = C13A-C15A = C13A-C16A
 2.45 with sigma of 0.01
 C13-C15 = C14-C16 = C14A-C16A
 2.52 with sigma of 0.01
 C13-C16
 2.4 with sigma of 0.01
 C13-C14 = C14-C15 = C15-C16 = C14A-C15A = C15A-C16A
 1.54 with sigma of 0.01
 O7-C13 = O7-C16 = C13A-C14A
 1.45 with sigma of 0.01
 C1A-C2A = C3A-C4A = C5A-C6A = C7A-C8A = C9A-C10A = C11A-C12A
 1.54 with sigma of 0.01
 O5A-C8A = O5A-C9A = O6A-C10A = O6A-C11A = O1A-C12A
 1.45 with sigma of 0.01
 O1A-C1A = O2A-C2A = O2A-C3A = O3A-C4A = O3A-C5A = O4A-C6A = O4A-C7A
 1.45 with sigma of 0.01
 C1-C12 = C2-C3 = C4-C5 = C6-C7 = C8-C9 = C10-C11
 2.4 with sigma of 0.01
 C1-C2 = C3-C4 = C5-C6 = C7-C8 = C9-C10 = C11-C12
 1.54 with sigma of 0.01
 O5-C8 = O5-C9 = O6-C10 = O6-C11 = O1-C12
 1.45 with sigma of 0.01
 O1-C1 = O2-C2 = O2-C3 = O3-C4 = O3-C5 = O4-C6 = O4-C7
 1.45 with sigma of 0.01
 O17-C37 = O17-C40 = O17A-C37A = O17A-C40A
 1.45 with sigma of 0.01
 C37-C38 = C38-C39 = C39-C40
 1.54 with sigma of 0.01
 C37A-C38A = C38A-C39A = C39A-C40A
 1.54 with sigma of 0.01
 C37-C39 = C38-C40 = C37A-C39A = C38A-C40A
 2.52 with sigma of 0.01
 O17-C38 = O17-C39 = O17A-C38A = O17A-C39A
 2.45 with sigma of 0.01
 C37-C40 = C37A-C40A
 2.42 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim
Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C2)
\\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C9) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C12) \\sim Ueq, Uanis(O7)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq,
Uanis(C16) \\sim Ueq, Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O3A)
\\sim Ueq, Uanis(O4A) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O6A) \\sim Ueq,
Uanis(C1A) \\sim Ueq, Uanis(C2A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C4A)
\\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A) \\sim Ueq,
Uanis(C8A) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C11A)
\\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(O7A) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(O7) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O14) \\sim Ueq, Uanis(C29) \\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C31)
\\sim Ueq, Uanis(C32) \\sim Ueq, Uanis(O14A) \\sim Ueq, Uanis(C29A) \\sim Ueq,
Uanis(C30A) \\sim Ueq, Uanis(C31A) \\sim Ueq, Uanis(C32A) \\sim Ueq, Uanis(O17)
\\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq,
Uanis(C40) \\sim Ueq, Uanis(O17A) \\sim Ueq, Uanis(C37A) \\sim Ueq, Uanis(C38A)
\\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(C8) = Uanis(C8A)
Uanis(C9) = Uanis(C9A)
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C7) = Uanis(C7A)
Uanis(O5) = Uanis(O5A)
Uanis(O3) = Uanis(O3A)
Uanis(C15) = Uanis(C16A)
Uanis(C4) = Uanis(C4A)
Uanis(C6) = Uanis(C6A)
Uanis(O6) = Uanis(O6A)
Uanis(O4) = Uanis(O4A)
Uanis(O17) = Uanis(O17A)
Uanis(C37) = Uanis(C37A)
Uanis(C38) = Uanis(C38A)
Uanis(C39) = Uanis(C39A)
Uanis(C40) = Uanis(C40A)
Uanis(C31) = Uanis(C31A)
4. Others
 Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C1A)=Sof(H1AA)=
 Sof(H1AB)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=
 Sof(H4AA)=Sof(H4AB)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=Sof(H11C)=Sof(H11D)=
 Sof(C12A)=Sof(H12C)=Sof(H12D)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(C1)=Sof(H1A)=Sof(H1B)=
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=
 Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(C9)=Sof(H9A)=
 Sof(H9B)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(C12)=Sof(H12A)=Sof(H12B)=FVAR(1)
 Sof(O7A)=Sof(C13A)=Sof(H13C)=Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=
 Sof(C15A)=Sof(H15C)=Sof(H15D)=Sof(C16A)=Sof(H16C)=Sof(H16D)=1-FVAR(2)
 Sof(O7)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(C15)=
 Sof(H15A)=Sof(H15B)=Sof(C16)=Sof(H16A)=Sof(H16B)=FVAR(2)
 Sof(O14A)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30C)=Sof(H30D)=
 Sof(C31A)=Sof(H31C)=Sof(H31D)=Sof(C32A)=Sof(H32C)=Sof(H32D)=1-FVAR(3)
 Sof(O14)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(C32)=Sof(H32A)=Sof(H32B)=FVAR(3)
 Sof(O17A)=Sof(C37A)=Sof(H37C)=Sof(H37D)=Sof(C38A)=Sof(H38C)=Sof(H38D)=
 Sof(C39A)=Sof(H39C)=Sof(H39D)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(4)
 Sof(O17)=Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=
 Sof(H39A)=Sof(H39B)=Sof(C40)=Sof(H40A)=Sof(H40B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C10(H10A,H10B), C5(H5A,
 H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C1A(H1AA,H1AB), C2A(H2AA,H2AB), C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,
 H5AB), C6A(H6AA,H6AB), C7A(H7AA,H7AB), C8A(H8AA,H8AB), C9A(H9AA,H9AB),
 C10A(H10C,H10D), C11A(H11C,H11D), C12A(H12C,H12D), C13A(H13C,H13D), C14A(H14C,
 H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17(H17A,H17B), C18(H18A,H18B),
 C19(H19A,H19B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B),
  C24(H24A,H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C28(H28A,
 H28B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C29A(H29C,
 H29D), C30A(H30C,H30D), C31A(H31C,H31D), C32A(H32C,H32D), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C37A(H37C,H37D), C38A(H38C,
 H38D), C39A(H39C,H39D), C40A(H40C,H40D)
5.b Aromatic/amide H refined with riding coordinates:
 C43(H43), C45(H45), C52(H52), C54(H54), C61(H61), C63(H63), C70(H70),
 C72(H72), C79(H79), C81(H81), C88(H88), C90(H90)
5.c Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C56(H56A,H56B,
 H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C65(H65A,H65B,H65C), C66(H66A,
 H66B,H66C), C67(H67A,H67B,H67C), C74(H74A,H74B,H74C), C75(H75A,H75B,H75C),
 C76(H76A,H76B,H76C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C), C85(H85A,H85B,
 H85C), C92(H92A,H92B,H92C), C93(H93A,H93B,H93C), C94(H94A,H94B,H94C)
;
_olex2_submission_special_instructions 'No special instructions were received'