Ring Contraction of 1,2,4,5,7,8-Hexaoxa-3-silonanes by Selective Reduction of COOSi Fragments. Synthesis of New Silicon-Containing Rings, 1,3,5,6-Tetraoxa-2-silepanes
Alexander O. Terent'ev; Maxim M. Platonov; Anna I. Tursina; Vladimir V. Chernyshev; Gennady I. Nikishin; Journal of Organic Chemistry 74 (2009) 1917–1922; doi:10.1021/jo8023957

data_4024361
_publ_contact_author             V.V.Chernyshev
_publ_contact_author_address
;
      Department of Chemistry 
      Moscow State University
      119991 Moscow
      Russia
;
_publ_contact_author_email       vladimir@struct.chem.msu.ru
_publ_contact_author_fax         '+ 7-095-9390898'
_publ_contact_author_name        'Dr. Vladimir V. Chernyshev'
_publ_contact_author_phone       '+ 7-095-9393654'
_publ_section_title
;
Ring Contraction of 1,2,4,5,7,8-Hexaoxa-3-silonanes by Selective Reduction
of COOSi Fragments. Synthesis of New Silicon-Containing Rings,
1,3,5,6-Tetraoxa-2-silepanes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1917
_journal_page_last               1922
_journal_paper_doi               10.1021/jo8023957
_journal_volume                  74
_journal_year                    2009
_chemical_formula_moiety         'C26 H50 O4 Si'
_chemical_formula_sum            'C26 H50 O4 Si'
_chemical_formula_weight         454.75
_chemical_name_systematic
; 
28,28-dimethyl-13,14,27,29-tetraoxa-28-siladispiro[11.2.11.3]nonacosane
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           manual
_cell_angle_alpha                91.07(2)
_cell_angle_beta                 96.37(4)
_cell_angle_gamma                88.63(2)
_cell_formula_units_Z            4
_cell_length_a                   17.659(7)
_cell_length_b                   18.624(8)
_cell_length_c                   8.505(3)
_cell_measurement_reflns_used    2875
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      37.49
_cell_measurement_theta_min      2.35
_cell_volume                     2778.7(19)
_computing_cell_refinement       'MRIA (Zlokazov & Chernyshev, 1992)'
_computing_data_collection       'Huber local program (Huber, 2002)'
_computing_data_reduction        'Huber local program'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  '  MRIA, SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  MRIA
_computing_structure_solution    MRIA
_diffrn_ambient_temperature      294(2)
_diffrn_detector_type            'Imaging Plate'
_diffrn_measurement_device       'Guinier camera G670'
_diffrn_radiation_monochromator  'Curved Germanium (111)'
_diffrn_radiation_source         'line-focus sealed tube'
_diffrn_radiation_type           CuK\a~1~
_diffrn_radiation_wavelength     1.54059
_diffrn_source                   'Fine focus X-ray tube'
_diffrn_source_target            Cu
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.087
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1008
_pd_char_colour                  colourless
_pd_char_particle_morphology     'no specific habit'
_pd_instr_location
;
Dept. of Chemistry, Moscow State University, 119991 Moscow, Russia
;
_pd_meas_2theta_range_inc        0.01
_pd_meas_2theta_range_max        75.00
_pd_meas_2theta_range_min        3.00
_pd_meas_number_of_points        7201
_pd_meas_scan_method             cont
_pd_proc_2theta_range_inc        0.01
_pd_proc_2theta_range_max        75.00
_pd_proc_2theta_range_min        3.00
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr     none
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_prof_R_factor        0.0228
_pd_proc_ls_prof_wR_expected     0.0139
_pd_proc_ls_prof_wR_factor       0.0305
_pd_proc_wavelength              1.54059
_pd_spec_mounting
; 
?
;
_pd_spec_mount_mode              transmission
_pd_spec_shape                   flat_sheet
_pd_spec_size_axial              15
_pd_spec_size_equat              1
_pd_spec_size_thick              1
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.39
_refine_diff_density_rms         0.25
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   2.194
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_constraints    0
_refine_ls_number_parameters     281
_refine_ls_number_restraints     380
_refine_ls_R_I_factor            0.0435
_refine_ls_shift/su_max          .004
_refine_ls_shift/su_mean         .001
_refine_ls_structure_factor_coef Inet
_refine_ls_weighting_scheme      sigma
_cod_data_source_file            jo8023957_si_002_2.cif
_cod_data_source_block           ioh26tr
_cod_depositor_comments
;
 Correcting the z coordinate of the 'C14B' atom by changing it from '0.9261(62'
 to '0.9261(62)'.

 Antanas Vaitkus,
 2018-07-18
;
_cod_database_code               4024361