Studies on the formal [3 + 2] cycloaddition of aziridines with alkenes for the synthesis of 1-azaspiroalkanes.
Martinand-Lurin, Elodie; Gruber, Raymond; Retailleau, Pascal; Fleurat-Lessard, Paul; Dauban, Philippe; The Journal of organic chemistry 80 (2015) 1414–1426; doi:10.1021/jo502333j

data_4030467
_publ_section_title
;
 Studies on the formal [3 + 2] cycloaddition of aziridines with alkenes
 for the synthesis of 1-azaspiroalkanes.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1414
_journal_page_last               1426
_journal_paper_doi               10.1021/jo502333j
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C18 H24 Cl3 N O4 S'
_chemical_formula_sum            'C18 H24 Cl3 N O4 S'
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
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_cell_angle_gamma                105.04(4)
_cell_formula_units_Z            2
_cell_length_a                   6.0360(10)
_cell_length_b                   10.487(3)
_cell_length_c                   17.295(4)
_cell_measurement_reflns_used    6257
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_cell_measurement_theta_min      0.407
_cell_volume                     1055.4(5)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997); COLLECT (Nonius B.V., 1999)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
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'SHELXL97 (Sheldrick, 2008); CRYSTALBUILDER (Welter, 2006)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Nonius kappa-CCD diffractometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
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_diffrn_radiation_wavelength     0.71070
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_diffrn_reflns_limit_h_max       7
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_diffrn_reflns_limit_k_min       -12
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20120
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_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         2.38
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius Kappa CCD'
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_exptl_absorpt_correction_type   multi-scan
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.437
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tab
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_exptl_crystal_size_max          0.36
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_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.636
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_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4259
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0629
_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^)+(0.0745P)^2^+1.0748P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
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_reflns_number_gt                3073
_reflns_number_total             4265
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502333j_si_011.cif
_cod_data_source_block           compound_4b
_cod_depositor_comments
'Adding full bibliography for 4030461--4030470.cif.'
_cod_original_cell_volume        1055.4(4)
_cod_database_code               4030467