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_7120988
_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         'C36 H84 O8 Si7'
_chemical_formula_sum            'C36 H84 O8 Si7'
_chemical_formula_weight         841.66
_chemical_melting_point          393.5(5)
_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                 104.5550(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.2557(12)
_cell_length_b                   13.4289(9)
_cell_length_c                   21.0576(13)
_cell_measurement_reflns_used    9806
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.28
_cell_volume                     4996.7(6)
_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      100(2)
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0205
_diffrn_reflns_av_unetI/netI     0.0119
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            36402
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         1.905
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6704
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS Sheldrick 1996'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.119
_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         0.514
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0297
_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^)+(0.0309P)^2^+6.2335P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5235
_reflns_number_total             5751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc08790j2.cif
_cod_data_source_block           yy39b_a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '393-394' was changed to '393.5(5)' -
the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               7120988
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.934
_shelx_estimated_absorpt_t_max   0.934
_shelx_res_checksum              62190