Lewis acid mediated (3 + 2) cycloadditions of donor-acceptor cyclopropanes with heterocumulenes.
Goldberg, Alexander F. G.; O'Connor, Nicholas R; Craig, 2nd, Robert A; Stoltz, Brian M.; Organic letters 14 (2012) 5314–5317; doi:10.1021/ol302494n

data_1508697
_publ_section_title
;
 Lewis acid mediated (3 + 2) cycloadditions of donor-acceptor
 cyclopropanes with heterocumulenes.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5314
_journal_page_last               5317
_journal_paper_doi               10.1021/ol302494n
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C20 H25 N O4 S'
_chemical_formula_sum            'C20 H25 N O4 S'
_chemical_formula_weight         375.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-08-21
_audit_creation_method
; 
  Olex2 1.1 
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906) 
;
_cell_angle_alpha                90
_cell_angle_beta                 92.145(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5982(10)
_cell_length_b                   16.1620(12)
_cell_length_c                   8.2014(6)
_cell_measurement_reflns_used    5787
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.600
_cell_measurement_theta_min      2.521
_cell_volume                     1933.7(2)
_computing_cell_refinement       'SAINT V8.18C (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 2012.2-0 (Bruker-AXS, 2007)'
_computing_data_reduction        'SAINT V8.18C (Bruker-AXS, 2007)'
_computing_molecular_graphics    'DIAMOND 3 (Crystal Impact, 1999)'
_computing_publication_material  'SHELXTL (Bruker-AXS, 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       'narrow \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0676
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            15085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         37.42
_diffrn_reflns_theta_min         1.40
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'TWINABS v2008/4 (Bruker-AXS, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         15085
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1034
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0645P)^2^+0.3700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1221
_refine_ls_wR_factor_ref         0.1431
_reflns_number_gt                10418
_reflns_number_total             15085
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol302494n_si_003.cif
_cod_data_source_block           rac13
_cod_database_code               1508697