Synthesis of a Stable Four-Membered Si2O2Ring and a Dimer with Two Four-Membered Si2O2Rings Bridged by Two Oxygen Atoms, with Five-Coordinate Silicon Atoms in Both Ring Systems
Sen, Sakya S.; Tavčar, Gašper; Roesky, Herbert W.; Kratzert, Daniel; Hey, Jakob; Stalke, Dietmar; Organometallics 29 (2010) 2343–; doi:10.1021/om100164u

data_4065859
_publ_section_title
;
 Synthesis of a Stable Four-Membered Si2O2Ring and a Dimer with Two
 Four-Membered Si2O2Rings Bridged by Two Oxygen Atoms, with
 Five-Coordinate Silicon Atoms in Both Ring Systems
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2343
_journal_paper_doi               10.1021/om100164u
_journal_volume                  29
_journal_year                    2010
_chemical_formula_moiety         'C56 H68 N4 O2 Si2, 2(C7 H8)'
_chemical_formula_sum            'C70 H84 N4 O2 Si2'
_chemical_formula_weight         1069.59
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 100.954(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.4840(17)
_cell_length_b                   11.4379(16)
_cell_length_c                   21.383(3)
_cell_measurement_reflns_used    6136
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.4415
_cell_measurement_theta_min      2.4335
_cell_volume                     2997.7(7)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2008.11'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'XSHELL in SHELXTL-97'
_computing_publication_material  'XSHELL in SHELXTL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Helios mirror optics'
_diffrn_radiation_source         'Bruker TXS-Mo rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_sigmaI/netI    0.0339
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            60807
_diffrn_reflns_theta_full        27.10
_diffrn_reflns_theta_max         27.10
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.108
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.9840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.185
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.322
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         6607
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+1.5213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0999
_reflns_number_gt                5220
_reflns_number_total             6607
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100164u_si_001.cif
_cod_data_source_block           p21n
_cod_original_cell_volume        2997.6(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4065859