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

data_7708731
_publ_section_title
;
 Silole Allylic Anions Instead of Silanides
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02363B
_journal_year                    2021
_chemical_formula_moiety         'C37 H73 Si10, C20 H40 Br Mg O5, C4 H8 O'
_chemical_formula_sum            'C61 H119 Br Mg O6 Si10'
_chemical_formula_weight         1333.67
_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                101.384(4)
_cell_angle_beta                 98.071(4)
_cell_angle_gamma                119.395(4)
_cell_formula_units_Z            2
_cell_length_a                   16.567(3)
_cell_length_b                   16.634(3)
_cell_length_c                   17.495(3)
_cell_measurement_reflns_used    1022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.83
_cell_measurement_theta_min      2.50
_cell_volume                     3955.8(12)
_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      150.00
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.987
_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  0.0731
_diffrn_reflns_av_unetI/netI     0.1387
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.987
_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       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29478
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_min         1.422
_diffrn_source_current           5.0
_diffrn_source_power             0.1
_diffrn_source_voltage           20.0
_exptl_absorpt_coefficient_mu    0.720
_exptl_absorpt_correction_T_max  0.9315
_exptl_absorpt_correction_T_min  0.700900
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0574 before and 0.0411 after correction.
The Ratio of minimum to maximum transmission is 0.7009.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.760
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     752
_refine_ls_number_reflns         14514
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.996
_refine_ls_R_factor_all          0.1422
_refine_ls_R_factor_gt           0.0836
_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^)+(0.0836P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1692
_refine_ls_wR_factor_ref         0.1899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8407
_reflns_number_total             14514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02363b2.cif
_cod_data_source_block           sadp-1_BrMg[4a]_1354j
_cod_original_cell_volume        3955.8(13)
_cod_database_code               7708731
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.932
_shelx_estimated_absorpt_t_min   0.858
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C25 \\sim C25A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
C24 \\sim C24A: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 2A
3. Others
 Sof(H26C)=Sof(H26D)=Sof(H27C)=Sof(H27D)=Sof(C25A)=Sof(H25C)=Sof(H25D)=
 Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(H26A)=Sof(H26B)=Sof(H27A)=Sof(H27B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C3(H3)
4.b Secondary CH2 refined with riding coordinates:
 C26(H26A,H26B), C26(H26C,H26D), C27(H27A,H27B), C27(H27C,H27D), C42(H42A,
 H42B), C43(H43A,H43B), C44(H44A,H44B), C45(H45A,H45B), C46(H46A,H46B),
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B),
  C52(H52A,H52B), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,
 H56B), C57(H57A,H57B), C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B),
 C65(H65A,H65B), C24(H24A,H24B), C25(H25A,H25B), C25A(H25C,H25D), C24A(H24C,
 H24D)
4.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C28(H28), C31(H31), C32(H32),
 C33(H33)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), 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), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C),
 C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              3079
_shelx_hkl_checksum              38268
_shelx_fab_checksum              58631
_olex2_submission_special_instructions 'No special instructions were received'