Reversible Alkene Extrusion from Platinaoxetanes
Endre Szuromi; Jianguo Wu; Paul R. Sharp; Journal of the American Chemical Society 128 (2006) 12088–12089; doi:10.1021/ja065207s

data_4110888
_publ_contact_author_address
;
 Department of Chemistry
 University of Missouri
 Columbia, MO  65211
;
_publ_contact_author_email       SharpP@missouri.edu
_publ_contact_author_fax         573-882-2754
_publ_contact_author_name        ' Paul R. Sharp'
_publ_contact_author_phone       573-882-7715
_publ_section_title
;
 Reversible Alkene Extrusion from Platinaoxetanes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12088
_journal_page_last               12089
_journal_paper_doi               10.1021/ja065207s
_journal_volume                  128
_journal_year                    2006
_chemical_formula_moiety         'C23 H26 B F3 O5 Pt'
_chemical_formula_sum            'C23 H26 B F3 O5 Pt'
_chemical_formula_weight         645.34
_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                107.7030(10)
_cell_angle_beta                 108.9250(10)
_cell_angle_gamma                103.7460(10)
_cell_formula_units_Z            2
_cell_length_a                   9.3406(6)
_cell_length_b                   11.7311(7)
_cell_length_c                   12.2403(8)
_cell_measurement_reflns_used    4696
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      54.112
_cell_measurement_theta_min      4.814
_cell_volume                     1121.37(12)
_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_publication_material  'CIFTAB (Sheldrick, 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 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w 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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0524
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8024
_diffrn_reflns_theta_full        27.15
_diffrn_reflns_theta_max         27.15
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    6.315
_exptl_absorpt_correction_T_max  0.3649
_exptl_absorpt_correction_T_min  0.3013
_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    1.911
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.637
_refine_diff_density_min         -2.210
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0627P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0963
_refine_ls_wR_factor_ref         0.1008
_reflns_number_gt                4255
_reflns_number_total             4799
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja065207ssi20060720_112527_1.cif
_cod_data_source_block           BF3_platinaoxetane_NB2_(9)
_cod_database_code               4110888