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_7717960
_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_sum            'C42 H68 Li2 O2 Si3'
_chemical_formula_weight         703.11
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-11-15 deposited with the CCDC.	2025-02-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.074(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.4817(14)
_cell_length_b                   12.5178(12)
_cell_length_c                   12.8080(11)
_cell_measurement_reflns_used    1532
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.4256
_cell_measurement_theta_min      2.5571
_cell_volume                     2190.1(4)
_computing_cell_refinement       'Bruker SAINT (Bruker 2016)'
_computing_data_collection       'Bruker APEX5 (Bruker 2022)'
_computing_data_reduction        'Bruker SAINT and XPREP (Bruker 2016)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'XCIF-2014/2 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2015)'
_computing_structure_solution    'XT, VERSION 2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'PHOTON III 7'
_diffrn_detector_area_resol_mean 7.3910
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  'Triumph monochromator'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13155
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.111
_diffrn_reflns_theta_max         25.111
_diffrn_reflns_theta_min         2.207
_exptl_absorpt_coefficient_mu    0.138
_exptl_absorpt_correction_T_max  0.959
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker 2016'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.066
_exptl_crystal_description       cube
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details
;
 Refined as a perfect inversion twin.
;
_refine_ls_abs_structure_Flack   0.5
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0566P)^2^+0.5484P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1035
_refine_ls_wR_factor_ref         0.1082
_reflns_Friedel_coverage         0.905
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                3413
_reflns_number_total             3908
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03537b2.cif
_cod_data_source_block           masa1604_a
_cod_depositor_comments
'Adding full bibliography for 7717959--7717961.cif.'
_cod_original_sg_symbol_H-M      'C 2'
_cod_database_code               7717960
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.986
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              11381