Silole Allylic Anions Instead of Silanides
Pöcheim, Alexander; Albers, Lena; Müller, Thomas; Baumgartner, Judith; Marschner, Christoph; Dalton Transactions  (2021) –; doi:10.1039/D1DT02363B

data_7708729
_publ_section_title
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 Silole Allylic Anions Instead of Silanides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02363B
_journal_year                    2021
_chemical_formula_moiety         'C12 H24 K O6, C46 H88 K O6 Si9'
_chemical_formula_sum            'C58 H112 K2 O12 Si9'
_chemical_formula_weight         1332.48
_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     dual
_audit_creation_date             2021-10-24
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2021-10-25 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                88.349(6)
_cell_angle_beta                 84.449(6)
_cell_angle_gamma                61.697(5)
_cell_formula_units_Z            2
_cell_length_a                   11.090(4)
_cell_length_b                   11.339(5)
_cell_length_c                   34.641(14)
_cell_measurement_reflns_used    987
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.18
_cell_measurement_theta_min      3.15
_cell_volume                     3817(3)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0479
_diffrn_reflns_av_unetI/netI     0.0724
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            26562
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.181
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_min  0.568359
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0908 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.5684.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.274
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     911
_refine_ls_number_reflns         13238
_refine_ls_number_restraints     75
_refine_ls_restrained_S_all      1.270
_refine_ls_R_factor_all          0.1520
_refine_ls_R_factor_gt           0.1444
_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^)+(0.0477P)^2^+53.3778P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3073
_refine_ls_wR_factor_ref         0.3114
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12365
_reflns_number_total             13238
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02363b2.cif
_cod_data_source_block           sad1_K2[3a]_1281j
_cod_original_cell_volume        3816(3)
_cod_database_code               7708729
_shelx_shelxl_version_number     2018/3
_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
 O12-C48 = O11-C47 = O16-C58 = O15-C57 = O16-C68 = O17-C67
 1.44 with sigma of 0.001
 C48-C47 = C58-C57 = C68-C67
 1.5 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(C50) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65) \\sim Ueq, Uanis(C69)
\\sim Ueq, Uanis(C62) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C54) \\sim Ueq, Uanis(O18)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
4. Others
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=Sof(O17)=Sof(O18)=Sof(C62)=Sof(H62A)=
 Sof(H62B)=Sof(C58)=Sof(H58A)=Sof(H58B)=Sof(C59)=Sof(H59A)=Sof(H59B)=Sof(C57)=
 Sof(H57A)=Sof(H57B)=Sof(C60)=Sof(H60A)=Sof(H60B)=Sof(C61)=Sof(H61A)=Sof(H61B)=
 Sof(C65)=Sof(H65A)=Sof(H65B)=Sof(C63)=Sof(H63A)=Sof(H63B)=Sof(C66)=Sof(H66A)=
 Sof(H66B)=Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(C64)=
 Sof(H64A)=Sof(H64B)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C48)=Sof(H48A)=
 Sof(H48B)=Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(C50)=Sof(H50A)=Sof(H50B)=Sof(C52)=
 Sof(H52A)=Sof(H52B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=
 Sof(H56B)=Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(C69)=
 Sof(H69A)=Sof(H69B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C47(H47A,H47B), C50(H50A,H50B), C52(H52A,H52B), C51(H51A,
 H51B), C54(H54A,H54B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B),
 C49(H49A,H49B), C70(H70A,H70B), C69(H69A,H69B), C62(H62A,H62B), C58(H58A,H58B),
  C59(H59A,H59B), C57(H57A,H57B), C60(H60A,H60B), C61(H61A,H61B), C65(H65A,
 H65B), C63(H63A,H63B), C66(H66A,H66B), C68(H68A,H68B), C67(H67A,H67B),
 C64(H64A,H64B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
  C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12)
5.c Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), 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), C46(H46A,H46B,H46C)
;
_shelx_res_checksum              60986
_shelx_hkl_checksum              24181
_olex2_submission_special_instructions 'No special instructions were received'