Facile synthesis and bridgehead-functionalization of bicyclo[3.3.3]pentasiloxanes
Yokouchi, Yuki; Ishida, Shintaro; Onodera, Tsunenobu; Oikawa, Hidetoshi; Iwamoto, Takeaki; Chemical Communications  (2018) –; doi:10.1039/C7CC08790J

data_7120989
_publ_section_title
;
 Facile synthesis and bridgehead-functionalization of
 bicyclo[3.3.3]pentasiloxanes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C7CC08790J
_journal_year                    2018
_chemical_formula_moiety         'C18 H42 O4 Si3.50'
_chemical_formula_sum            'C18 H42 O4 Si3.5'
_chemical_formula_weight         420.83
_chemical_name_systematic
1,5-bis(t-butyldimethylsiloxy)hexaisobutylbicyclo[3.3.3]pentasiloxane
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-27 deposited with the CCDC.
2017-12-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.8890(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0349(5)
_cell_length_b                   13.7423(3)
_cell_length_c                   21.0422(5)
_cell_measurement_reflns_used    8203
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.22
_cell_volume                     5343.4(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Bruker Helios multilayer confocal mirror'
_diffrn_radiation_source         'Bruker TXS fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32950
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.417
_diffrn_reflns_theta_min         1.847
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.046
_exptl_crystal_description       block
_exptl_crystal_F_000             1848
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: EtOH'
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.453
_refine_diff_density_min         -0.390
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         4920
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0703
_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^)+(0.1075P)^2^+7.2071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1945
_refine_ls_wR_factor_ref         0.2335
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3476
_reflns_number_total             4920
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08790j2.cif
_cod_data_source_block           yy39c_a
_cod_original_formula_sum        'C18 H42 O4 Si3.50'
_cod_database_code               7120989
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.938
_shelx_res_checksum              87183