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_4030463
_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         'C17 H22 Cl3 N O3 S'
_chemical_formula_sum            'C17 H22 Cl3 N O3 S'
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_atom_sites_solution_secondary   difmap
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_cell_angle_beta                 91.751(3)
_cell_angle_gamma                102.466(3)
_cell_formula_units_Z            2
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_cell_length_b                   10.244(3)
_cell_length_c                   16.192(4)
_cell_measurement_reflns_used    2524
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.350
_cell_measurement_theta_min      0.407
_cell_volume                     971.2(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)'
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'SHELXL97 (Sheldrick, 2008); CRYSTALBUILDER (Welter, 2006)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
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_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Nonius kappa-CCD diffractometer'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
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_diffrn_reflns_Laue_measured_fraction_full 0.886
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7902
_diffrn_reflns_point_group_measured_fraction_full 0.886
_diffrn_reflns_point_group_measured_fraction_max 0.944
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_diffrn_reflns_theta_max         24.711
_diffrn_reflns_theta_min         3.337
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Nonius Kappa CCD'
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_exptl_absorpt_correction_T_max  0.96
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             444
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.07
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_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         3117
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+0.9759P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1362
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2481
_reflns_number_total             3117
_reflns_threshold_expression     'I > 2\s(I)'
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_cod_data_source_block           compound_4a
_cod_depositor_comments
'Adding full bibliography for 4030461--4030470.cif.'
_cod_database_code               4030463
_shelx_estimated_absorpt_t_min   0.943
_shelx_estimated_absorpt_t_max   0.943
_shelxl_version_number           2012-9
_shelx_res_checksum              36442
_shelx_hkl_checksum              8489