Synthesis of Multiply Substituted Alkylidene Silacyclohexadiene Derivatives via Palladium-Catalyzed Insertion of Alkynes into Alkylidene Silacyclobutenes
Junhui Liu; Xiaohua Sun; Mikihiro Miyazaki; Lantao Liu; Congyang Wang; Zhenfeng Xi; Journal of Organic Chemistry 72 (2007) 3137–3140; doi:10.1021/jo062583m

data_4022830
_publ_section_title
;
 Synthesis of Multiply Substituted Alkylidene
 Silacyclohexadiene Derivatives via Palladium-Catalyzed
 Insertion of Alkynes into Alkylidene Silacyclobutenes
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              3137
_journal_page_last               3140
_journal_paper_doi               10.1021/jo062583m
_journal_volume                  72
_journal_year                    2007
_chemical_formula_sum            'C24 H24 O4 Si'
_chemical_formula_weight         404.52
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens
;
                                  hydrogen atoms are generated by HFIX
                                  instructions
;
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.39(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2495(18)
_cell_length_b                   8.9167(18)
_cell_length_c                   26.294(5)
_cell_measurement_reflns_used    11134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.02
_cell_measurement_theta_min      2.41
_cell_volume                     2168.6(7)
_computing_cell_refinement
;
                                   Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   MSC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381 USA.
;
_computing_data_collection
;
                                   Molecular Structure Corporation (1994)
                                   MSC/AFC Diffractometer Control Software
                                   SC, 3200 Research Forest Drive, The
                                   Woodlands, TX 77381, USA.
;
_computing_data_reduction
;
                                   Sheldrick, G. M. (1998) SHELXS98, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.
;
_computing_molecular_graphics
;
                                   Interactive Molecular Graphics XP, Virsion
                                   4.2 for MSDOS (1990), Siemens Analytical
                                   X-ray Instruments Inc., Madison, Wisconsin,
                                   USA.
;
_computing_publication_material
;
                                   Sheldrick, G. M. (1998) SHELXL98, Program
                                   for the refinement of Crystal Structure,
                                   University of Gottingen, Germany.
;
_computing_structure_refinement
;
                                   Sheldrick, G. M. (1998) SHELXL98, Program
                                   for the Refinement of Crystal Structure,
                                   University of Gottingen, Germany.
;
_computing_structure_solution
;
                                   Sheldrick, G. M. (1998) SHELXS98, Program
                                   for the Solution of Crystal Structure,
                                   University of Gottingen, Germany.
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Rigaku RAXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0562
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            11134
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.41
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.976
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
                                  HIGASHI, T. (1995). Abscor-Empirical
                                  Absorption
                                  Correction based on Fourier Series
                                  Approximation.Rigaku Corporation,Tokyo,
                                  Japan.
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.043
_refine_ls_extinction_coef       0.0066(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment
;
                                  hydrogen coordinates ride on the coordinates
                                  of the previous atom, the isotropic U values
                                  are 1.2 OR 1.5 time over the U values of the
                                  previous atom.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         3768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1093
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                2468
_reflns_number_total             3768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo062583msi20061216_064051.cif
_cod_data_source_block           a
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Empirical' changed to
'empirical' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022830