Synthesis of a dilithiobutadiene bearing extremely bulky silyl substituents and its reactivity toward functionalized silanes.
Münster, Katharina; Kudo, Shunsuke; Kuwabara, Takuya; Shimamura, Eriko; Furukawa, Shunsuke; Yoshida, Yusuke; Ishida, Shintaro; Iwamoto, Takeaki; Tanifuji, Kazuki; Ohki, Yasuhiro; Minoura, Mao; Saito, Masaichi; Dalton transactions (Cambridge, England : 2003) 54 (2025) 4030–4038; doi:10.1039/d4dt03537b

data_7717959
_publ_section_title
;
 Synthesis of a dilithiobutadiene bearing extremely bulky silyl
 substituents and its reactivity toward functionalized silanes.
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4030
_journal_page_last               4038
_journal_paper_doi               10.1039/d4dt03537b
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C34 H52 Br2 Si3'
_chemical_formula_sum            'C34 H52 Br2 Si3'
_chemical_formula_weight         704.84
_chemical_name_systematic        KM040-6
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'I 2y'
_space_group_name_H-M_alt        'I 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-11-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.01.12 svn.r2f8d729c for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-15 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.683(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.3003(8)
_cell_length_b                   8.7240(2)
_cell_length_c                   34.4836(11)
_cell_measurement_reflns_used    7458
_cell_measurement_temperature    123.15
_cell_measurement_theta_max      27.6590
_cell_measurement_theta_min      2.3030
_cell_volume                     7210.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.130a (Rigaku OD, 2024)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      123.15
_diffrn_detector                 'Rigaku HyPix-6000HE'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'Hybrid photon counting detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'AFC11L: Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku HyPix-6000HE'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 30/50/150um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0436
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            24321
_diffrn_reflns_point_group_measured_fraction_full 0.920
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         2.289
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.130a (Rigaku Oxford Diffraction, 2024)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.847
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details
;
 Flack x determined using 4552 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.089(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     727
_refine_ls_number_reflns         13377
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0444P)^2^+0.7852P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0792
_reflns_Friedel_coverage         0.703
_reflns_Friedel_fraction_full    0.829
_reflns_Friedel_fraction_max     0.806
_reflns_number_gt                12144
_reflns_number_total             13377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03537b2.cif
_cod_data_source_block           exp_2_autored
_cod_depositor_comments
'Adding full bibliography for 7717959--7717961.cif.'
_cod_database_code               7717959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.833
_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.a Ternary CH refined with riding coordinates:
 C42(H42), C45(H45), C39(H39), C32(H32), C8(H8), C63(H63), C66(H66), C60(H60),
 C11(H11), C5(H5), C29(H29), C26(H26)
2.b Aromatic/amide H refined with riding coordinates:
 C49(H49), C55(H55), C53(H53), C15(H15), C19(H19), C59(H59), C18(H18),
 C16(H16), C52(H52), C25(H25), C17(H17), C56(H56), C50(H50), C58(H58), C57(H57),
  C51(H51), C21(H21), C24(H24), C22(H22), C23(H23)
2.c Idealised Me refined as rotating group:
 C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C34(H34A,H34B,H34C), C10(H10A,H10B,
 H10C), C9(H9A,H9B,H9C), C61(H61A,H61B,H61C), C6(H6A,H6B,H6C), C41(H41A,H41B,
 H41C), C13(H13A,H13B,H13C), C62(H62A,H62B,H62C), C40(H40A,H40B,H40C), C7(H7A,
 H7B,H7C), C12(H12A,H12B,H12C), C67(H67A,H67B,H67C), C47(H47A,H47B,H47C),
 C31(H31A,H31B,H31C), C46(H46A,H46B,H46C), C30(H30A,H30B,H30C), C27(H27A,H27B,
 H27C), C28(H28A,H28B,H28C), C65(H65A,H65B,H65C), C68(H68A,H68B,H68C), C33(H33A,
 H33B,H33C), C64(H64A,H64B,H64C)
;
_olex2_exptl_crystal_mounting_method 'Loop 150 ?5m'
_olex2_submission_special_instructions 'No special instructions were received'