Synthesis, Structure, and Thermolysis of a Pentacoordinate 1,2-Oxastibetane
Yosuke Uchiyama; Naokazu Kano; Takayuki Kawashima; Journal of the American Chemical Society 125 (2003) 13346–13347; doi:10.1021/ja037586k

data_4114326
_publ_contact_author_address
;
Department of Chemistry, Graduate School of Science,
The University of Tokyo,
7-3-1 Hongo, Bunkyo-ku, Tokyo, 113-0033, Japan
;
_publ_contact_author_email       takayuki@chem.s.u-tokyo.ac.jp
_publ_contact_author_fax         +81-5800-6899
_publ_contact_author_name        'Takayuki Kawashima'
_publ_contact_author_phone       +81-5800-6899
_publ_section_title
;
 Synthesis, Structure, and Thermolysis of a Pentacoordinate
 1,2-Oxastibetane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13346
_journal_page_last               13347
_journal_paper_doi               10.1021/ja037586k
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C34 H28 F9 O2 Sb'
_chemical_formula_sum            'C34 H28 F9 O2 Sb'
_chemical_formula_weight         761.31
_chemical_melting_point          462(1)
_chemical_name_common            1,2-oxastibetane
_chemical_name_systematic
;
3,4'-Diphenyl-3,4'-bis(trifluoromethyl)-1-[4-(t-butyl)phenyl]spiro
[2,1-benzoxastibole-1(3H),2'\l^5^-[1,2-oxastibetane]
;
_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                97.523(6)
_cell_angle_beta                 90.015(13)
_cell_angle_gamma                118.133(7)
_cell_formula_units_Z            4
_cell_length_a                   9.733(2)
_cell_length_b                   10.284(5)
_cell_length_c                   36.391(7)
_cell_measurement_reflns_used    7382
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.02
_cell_volume                     3176.5(18)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        YadokariXG
_computing_molecular_graphics    'ORTEP-III ver.1.0.3'
_computing_publication_material  YadokariXG
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_av_sigmaI/netI    0.0673
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            25836
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_diffrn_standards_number         10504
_exptl_absorpt_coefficient_mu    0.952
_exptl_absorpt_correction_T_max  0.9540
_exptl_absorpt_correction_T_min  0.8704
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.592
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.543
_refine_diff_density_min         -1.488
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.382
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     835
_refine_ls_number_reflns         10995
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.382
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0988
_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^)+(0.0000P)^2^+48.0262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1917
_refine_ls_wR_factor_ref         0.1964
_reflns_number_gt                10009
_reflns_number_total             10995
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja037586ksi20030729_013858.cif
_cod_data_source_block           oxastibetane
_cod_original_cell_volume        3176.6(17)
_cod_database_code               4114326