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_4065858
_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         'C60 H92 N8 O6 Si4, 0.5(C7 H8), 0.5(C7 H8)'
_chemical_formula_sum            'C67 H100 N8 O6 Si4'
_chemical_formula_weight         1225.91
_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                 101.979(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7264(16)
_cell_length_b                   28.415(4)
_cell_length_c                   23.012(3)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.3415
_cell_measurement_theta_min      2.3055
_cell_volume                     6861.1(17)
_computing_cell_refinement       'SAINT V7.66A'
_computing_data_collection       'APEX2 v2009.11-0'
_computing_data_reduction        'SAINT V7.46A'
_computing_molecular_graphics
'XP in SHELXTL Version 2008/4 and XShell in SHELXTL Version 2008/4'
_computing_publication_material
'XP in SHELXTL Version 2008/4 and XShell in SHELXTL Version 2008/4'
_computing_structure_refinement  'SHELXL in SHELXTL 2008/4'
_computing_structure_solution    'SHELXS in SHELXTL 2008/4'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Smart Apex II with D8-Goniometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'INCOATEC Quazar mirror optics'
_diffrn_radiation_source         'INCOATEC Mo Microsource'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1051
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            162534
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.15
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_T_max  0.9916
_exptl_absorpt_correction_T_min  0.9156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/2
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.261
_refine_diff_density_min         -0.337
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         14016
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0338P)^2^+4.9702P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0940
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                10744
_reflns_number_total             14016
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om100164u_si_001.cif
_cod_data_source_block           p21n80
_cod_original_cell_volume        6861.2(18)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4065858