A Stereoselective Intramolecular Cyclopropanation via a De Novo Class of Push-Pull Carbenes Derived from DMDO-Epoxidations of Chiral Ynamides.
Li, Hongyan; Antoline, Jennifer E.; Yang, Jin-Haek; Al-Rashid, Ziyad F; Hsung, Richard P.; New journal of chemistry = Nouveau journal de chimie 34 (2010) 1309–1316; doi:10.1039/c0nj00063a

data_7053469
_publ_section_title
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 A Stereoselective Intramolecular Cyclopropanation via a De Novo Class of
 Push-Pull Carbenes Derived from DMDO-Epoxidations of Chiral Ynamides.
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_journal_issue                   7
_journal_name_full
'New journal of chemistry = Nouveau journal de chimie'
_journal_page_first              1309
_journal_page_last               1316
_journal_paper_doi               10.1039/c0nj00063a
_journal_volume                  34
_journal_year                    2010
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C21 H19 N O3'
_chemical_formula_sum            'C21 H19 N O3'
_chemical_formula_weight         333.37
_chemical_name_common            CMC0772a
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_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                 102.432(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.959(2)
_cell_length_b                   6.0746(12)
_cell_length_c                   12.943(3)
_cell_measurement_reflns_used    3390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      13.21
_cell_measurement_theta_min      2.21
_cell_volume                     841.4(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.903
_diffrn_measured_fraction_theta_max 0.903
_diffrn_measurement_device_type  'Bruker-AXS APEX-II'
_diffrn_measurement_method       'Phi-scans fixed Chi'
_diffrn_radiation_monochromator  Double-diamond
_diffrn_radiation_source         'APS 15-ID-B'
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0517
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14159
_diffrn_reflns_theta_full        14.96
_diffrn_reflns_theta_max         14.96
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.009
_exptl_absorpt_correction_T_max  0.9999
_exptl_absorpt_correction_T_min  0.9993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             352
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.167
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.045
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         1715
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0428P)^2^+0.2619P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0834
_refine_ls_wR_factor_ref         0.0926
_reflns_number_gt                1401
_reflns_number_total             1715
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0nj00063a.txt
_cod_data_source_block           cmc0772a
_cod_depositor_comments
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The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Multi-scan'
changed to 'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7053469