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

data_7708732
_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         'C74 H146 K2 Si20'
_chemical_formula_sum            'C74 H146 K2 Si20'
_chemical_formula_weight         1675.90
_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
_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                110.608(3)
_cell_angle_beta                 93.224(3)
_cell_angle_gamma                101.578(3)
_cell_formula_units_Z            2
_cell_length_a                   16.821(3)
_cell_length_b                   17.503(3)
_cell_length_c                   18.760(3)
_cell_measurement_reflns_used    974
_cell_measurement_temperature    496(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.34
_cell_volume                     5015.9(15)
_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      496.30
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.0657
_diffrn_reflns_av_unetI/netI     0.1109
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            36177
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.248
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.369
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.702544
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0727 before and 0.0458 after correction.
The Ratio of minimum to maximum transmission is 0.7025.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blocks
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.926
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     907
_refine_ls_number_reflns         17515
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1644
_refine_ls_R_factor_gt           0.1429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0032P)^2^+110.3815P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2678
_refine_ls_wR_factor_ref         0.2805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14766
_reflns_number_total             17515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02363b2.cif
_cod_data_source_block           sad1_K[4a]_1303j
_cod_original_cell_volume        5016.0(13)
_cod_database_code               7708732
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.954
_shelx_estimated_absorpt_t_min   0.904
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Ternary CH refined with riding coordinates:
 C17(H17), C4(H4)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C7(H7), C11(H11), C8(H8), C20(H20), C12(H12), C32(H32), C33(H33),
 C34(H34), C30(H30), C21(H21), C35(H35), C41(H41), C42(H42), C43(H43), C45(H45),
  C48(H48), C50(H50)
3.c Idealised Me refined as rotating group:
 C16(H16A,H16B,H16C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C28(H28A,
 H28B,H28C), C31(H31A,H31B,H31C), C29(H29A,H29B,H29C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C44(H44A,H44B,
 H44C), C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C51(H51A,
 H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,H54B,H54C),
 C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,
 H58C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,
 H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C),
 C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,
 H69C), C70(H70A,H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C74(H74A,H74B,H74C)
;
_shelx_res_checksum              12520
_shelx_hkl_checksum              27538
_olex2_submission_special_instructions 'No special instructions were received'