Synthesis, Crystal Structure, and Thermolysis of the First Tetracoordinate 1λ4,2-Selenazetidines: Aziridine Formation Reaction from a Four-Membered Heterocycle Bearing Highly Coordinate Selenium
Kano, Naokazu; Daicho, Yuya; Nakanishi, Nobuhito; Kawashima, Takayuki; Organic Letters 3 (2001) 691–; doi:10.1021/ol007015m

data_1507507
_publ_section_title
;
 Synthesis, Crystal Structure, and Thermolysis of the First
 Tetracoordinate 1\l4,2-Selenazetidines:&#x2009; Aziridine Formation
 Reaction from a Four-Membered Heterocycle Bearing Highly Coordinate
 Selenium
;
_journal_issue                   5
_journal_name_full               'Organic Letters'
_journal_page_first              691
_journal_paper_doi               10.1021/ol007015m
_journal_volume                  3
_journal_year                    2001
_chemical_formula_moiety         'C25 H15 F12 N O Se '
_chemical_formula_sum            'C25 H15 F12 N O Se'
_chemical_formula_weight         652.34
_chemical_name_systematic
;
trans-4'-phenyl-3,3,3',3'-tetrakis(trifluoromethyl)-3H-
spiro[[2,1]benzoxaselenole-1\l4,1'-[1,2]-selenazetidine]
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.446(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.7010(2)
_cell_length_b                   15.3350(5)
_cell_length_c                   16.8410(5)
_cell_measurement_reflns_used    18492
_cell_measurement_temperature    150.2
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.036
_cell_volume                     2455.52(12)
_computing_cell_refinement       DENZO
_computing_data_collection       Xpress
_computing_data_reduction        DENZO
_computing_publication_material  'teXsan Ver. 1.10'
_computing_structure_refinement  'teXsan Ver. 1.10'
_computing_structure_solution    SIR92
_diffrn_detector_area_resol_mean 0.010000
_diffrn_measured_fraction_theta_full 0.9371
_diffrn_measured_fraction_theta_max 0.9371
_diffrn_measurement_device_type  'Mac Science DIP2030 Image Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
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_diffrn_reflns_theta_full        25.61
_diffrn_reflns_theta_max         25.61
_exptl_absorpt_coefficient_mu    1.642
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.764
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.500
_exptl_crystal_size_min          0.300
_refine_diff_density_max         0.39
_refine_diff_density_min         -1.22
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4340
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.0011
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.05000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]'
_refine_ls_weighting_scheme      calc
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_reflns_number_total             4340
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ol007015m_s1.cif
_cod_data_source_block           sencc2
_cod_original_cell_volume        2455.5(1)
_cod_original_formula_sum        'C25 H15 F12 N O Se '
_cod_database_code               1507507