Synthesis and thermolysis of novel spiroselenuranes bearing two oxaselenetane rings: double oxirane formation reactions from 1,5-dioxa-4λ4-selenaspiro[3.3]heptanes
Ohno, Fumihiko; Kawashima, Takayuki; Okazaki, Renji; Chemical Communications  (2001) 463–; doi:10.1039/b009789f

data_7114923
_publ_section_title
;
 Synthesis and thermolysis of novel spiroselenuranes bearing two
 oxaselenetane rings: double oxirane formation reactions from
 1,5-dioxa-4\l4-selenaspiro[3.3]heptanes
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_page_first              463
_journal_paper_doi               10.1039/b009789f
_journal_year                    2001
_chemical_formula_sum            'C20 H12 F12 O2 Se'
_chemical_formula_weight         591.26
_chemical_name_common
;
1,5-dioxa-4lambda4-selenaspiro[3.3]heptane
;
_chemical_name_systematic
; 
3,7-diphenyl-2,2,6,6-tetrakis(trifluoromethyl)-
1,5-dioxa-4lambda4-selenaspiro[3.3]heptane
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 106.209(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            6
_cell_length_a                   9.621(2)
_cell_length_b                   22.144(3)
_cell_length_c                   16.221(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     3318.5(9)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan for Windows (MSC, 1997)'
_computing_molecular_graphics    'Yadokari-X (Wakita, 2000)'
_computing_publication_material  'Yadokari-X (Wakita, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0753
_diffrn_reflns_av_sigmaI/netI    0.1623
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            8040
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        2.07
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.814
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1740
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.939
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.2105
_refine_ls_R_factor_gt           0.0809
_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^)+(0.0970P)^2^+0.4452P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1757
_refine_ls_wR_factor_ref         0.2193
_reflns_number_gt                3407
_reflns_number_total             7600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b009789f.txt
_cod_data_source_block           se44
_cod_original_cell_volume        3318.3(9)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7114923