Dynamic kinetic asymmetric [3 + 2] annulation reactions of aminocyclopropanes.
de Nanteuil, Florian; Serrano, Eloisa; Perrotta, Daniele; Waser, Jerome; Journal of the American Chemical Society 136 (2014) 6239–6242; doi:10.1021/ja5024578

data_4121720
_publ_section_title
;
 Dynamic kinetic asymmetric [3 + 2] annulation reactions of
 aminocyclopropanes.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6239
_journal_page_last               6242
_journal_paper_doi               10.1021/ja5024578
_journal_volume                  136
_journal_year                    2014
_chemical_formula_sum            'C16.5 H27 Cl3 Cu1.5 N3 O15'
_chemical_formula_weight         709.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.497(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.4821(9)
_cell_length_b                   9.4938(7)
_cell_length_c                   14.3422(19)
_cell_measurement_temperature    293(2)
_cell_volume                     1255.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.721
_diffrn_measured_fraction_theta_max 0.721
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_sigmaI/netI    0.0213
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2371
_diffrn_reflns_theta_full        67.95
_diffrn_reflns_theta_max         67.95
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    5.338
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             723
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.093
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         2289
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.386
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1109P)^2^+0.0997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1271
_reflns_number_gt                2203
_reflns_number_total             2289
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja5024578_si_001.cif
_cod_data_source_block           ouf
_cod_depositor_comments
'Adding full bibliography for 4121719--4121720.cif.'
_cod_original_formula_sum        'C16.50 H27 Cl3 Cu1.50 N3 O15'
_cod_database_code               4121720