Highly regioselective [3 + 2] annulation of azomethine imines with 1-alkynyl Fischer carbene complexes to functionalized N,N-bicyclic pyrazolidin-3-ones.
Luo, Ning; Zheng, Zhaoyan; Yu, Zhengkun; Organic letters 13 (2011) 3384–3387; doi:10.1021/ol201139w

data_1502245
_publ_section_title
;
 Highly regioselective [3 + 2] annulation of azomethine imines with
 1-alkynyl Fischer carbene complexes to functionalized N,N-bicyclic
 pyrazolidin-3-ones.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3384
_journal_page_last               3387
_journal_paper_doi               10.1021/ol201139w
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C32 H24 N2 O7 W'
_chemical_formula_weight         732.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                77.3790(10)
_cell_angle_beta                 77.5530(10)
_cell_angle_gamma                84.9940(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0314(8)
_cell_length_b                   10.7337(9)
_cell_length_c                   14.5403(12)
_cell_measurement_reflns_used    4232
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      49.932
_cell_measurement_theta_min      4.581
_cell_volume                     1490.5(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8786
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    3.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73678
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatci
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.333
_exptl_crystal_size_min          0.213
_refine_diff_density_max         1.903
_refine_diff_density_min         -1.293
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         6304
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0944
_reflns_number_gt                5379
_reflns_number_total             6304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201139w_si_002.cif
_cod_data_source_block           complex_3b_(cd26385)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1502245