Reduction of Organosilicon Peroxides: Ring Contraction and Cyclodimerization
Arzumanyan, Ashot V.; Terent’ev, Alexander O.; Novikov, Roman A.; Lakhtin, Valentin G.; Grigoriev, Michail S.; Nikishin, Gennady I.; Organometallics 35 (2016) 1667–; doi:10.1021/acs.organomet.6b00129

data_4088487
_publ_section_title
;
 Reduction of Organosilicon Peroxides: Ring Contraction and
 Cyclodimerization
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1667
_journal_paper_doi               10.1021/acs.organomet.6b00129
_journal_volume                  35
_journal_year                    2016
_chemical_formula_sum            'C28 H56 O4 Si2'
_chemical_formula_weight         512.90
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 100.108(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9229(3)
_cell_length_b                   14.9018(4)
_cell_length_c                   17.4042(5)
_cell_measurement_reflns_used    1733
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.78
_cell_measurement_theta_min      6.14
_cell_volume                     3044.25(14)
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_unetI/netI     0.0665
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            30382
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         4.085
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.145
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         8832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0825
_refine_ls_R_factor_gt           0.0455
_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^)+(0.0482P)^2^+0.3670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0985
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                5968
_reflns_number_total             8832
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00129_si_002.cif
_cod_data_source_block           911
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4088487
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.971
_shelxl_version_number           2014-3
_shelx_res_checksum              47677
_shelx_hkl_checksum              37183