Proton-Catalyzed Oxo-Alkene Coupling: 2-Platinaoxetane Formation
Nandita M. Weliange; Endre Szuromi; Paul R. Sharp; Journal of the American Chemical Society 131 (2009) 8736–8737; doi:10.1021/ja902180k

data_4104599
_publ_section_title
;
 Proton-Catalyzed Oxo-Alkene Coupling: 2-Platinaoxetane Formation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8736
_journal_page_last               8737
_journal_paper_doi               10.1021/ja902180k
_journal_volume                  131
_journal_year                    2009
_chemical_formula_sum            'C36 H52 F12 O16 Pt4 S4'
_chemical_formula_weight         1877.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 133.29
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.560(3)
_cell_length_b                   10.5832(10)
_cell_length_c                   21.554(2)
_cell_measurement_reflns_used    6390
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.08
_cell_measurement_theta_min      2.60
_cell_volume                     4908.1(8)
_computing_cell_refinement       'SMART (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics
;
   L. J. Barbour, X-Seed - Graphical Interface to
   SHELX-97 and POV-Ray, 1999
   ORTEP (Johnson, 1976), ORTEP 3 for Windows (L. J. Farrugia, 1997)
;
_computing_structure_refinement
;
   SHELXL-97 (Sheldrick, 1997), L. J. Barbour, X-Seed - Graphical Interface to
   SHELX-97 and POV-Ray, 1999
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0508
_diffrn_reflns_av_sigmaI/netI    0.0571
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            16923
_diffrn_reflns_theta_full        27.19
_diffrn_reflns_theta_max         27.19
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    11.648
_exptl_absorpt_correction_T_max  0.3888
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
   Data were corrected for decay and absorption using the program SADABS
   based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995).
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.541
_exptl_crystal_description       block
_exptl_crystal_F_000             3520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         3.746
_refine_diff_density_min         -3.474
_refine_diff_density_rms         0.332
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         5412
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0663
_refine_ls_shift/su_max          0.049
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+463.1043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1617
_reflns_number_gt                4180
_reflns_number_total             5412
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja902180k_si_002.cif
_cod_data_source_block           '[Pt(COD)(m-OH)]4(OTf)4_(5-OTf,n=4)'
_cod_original_cell_volume        4907.9(8)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               4104599