Silver-Catalyzed [2 + 2] Cycloadditions of Siloxy Alkynes
Randy F. Sweis; Michael P. Schramm; Sergey A. Kozmin; Journal of the American Chemical Society 126 (2004) 7442–7443; doi:10.1021/ja048251l

data_4112685
_publ_contact_author_address
;
Department of Chemistry
The University of Chicago
5735 S. Ellis Ave
Chicago, IL 60637
USA
;
_publ_contact_author_email       skozmin@uchicago.edu
_publ_contact_author_name        'Sergey A. Kozmin'
_publ_section_title
;
 Silver-Catalyzed [2 + 2] Cycloadditions of Siloxy Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7442
_journal_page_last               7443
_journal_paper_doi               10.1021/ja048251l
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C28 H40 N2 O4 S Si'
_chemical_formula_weight         528.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.092(5)
_cell_angle_beta                 81.484(6)
_cell_angle_gamma                69.293(5)
_cell_formula_units_Z            2
_cell_length_a                   7.857(3)
_cell_length_b                   10.517(4)
_cell_length_c                   18.996(6)
_cell_measurement_temperature    373(2)
_cell_volume                     1443.2(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0303
_diffrn_reflns_av_sigmaI/netI    0.0262
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14069
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.188
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.70
_exptl_absorpt_correction_type   empirical
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5106
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0800P)^2^+1.3635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1469
_reflns_number_gt                4868
_reflns_number_total             5106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048251l.cif
_cod_data_source_block           mike17s
_cod_database_code               4112685