Tandem reaction of propargyl alcohol and N-sulfonylhydrazone: synthesis of dihydropyrazole and its utility in the preparation of 3,3-diarylacrylonitrile.
Zhu, Yuanxun; Wen, Shan; Yin, Guangwei; Hong, Deng; Lu, Ping; Wang, Yanguang; Organic letters 13 (2011) 3553–3555; doi:10.1021/ol201203g

data_1502258
_publ_section_title
;
 Tandem reaction of propargyl alcohol and N-sulfonylhydrazone: synthesis
 of dihydropyrazole and its utility in the preparation of
 3,3-diarylacrylonitrile.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3553
_journal_page_last               3555
_journal_paper_doi               10.1021/ol201203g
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C28 H22 N2 O2 S'
_chemical_formula_sum            'C28 H22 N2 O2 S'
_chemical_formula_weight         450.54
_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                88.426(3)
_cell_angle_beta                 87.150(3)
_cell_angle_gamma                68.296(4)
_cell_formula_units_Z            4
_cell_length_a                   10.7469(4)
_cell_length_b                   12.9651(5)
_cell_length_c                   17.9436(8)
_cell_measurement_reflns_used    7512
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.6354
_cell_measurement_theta_min      2.8408
_cell_volume                     2319.94(17)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2010)'
_computing_data_collection       'CrysAlis PRO'
_computing_data_reduction        'CrysAlis PRO'
_computing_molecular_graphics    'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 10.3592
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w 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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            18089
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         2.85
_exptl_absorpt_coefficient_mu    0.168
_exptl_absorpt_correction_T_max  0.9391
_exptl_absorpt_correction_T_min  0.9239
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis PRO (Oxford Diffraction, 2010) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.43
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     595
_refine_ls_number_reflns         8474
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0466P)^2^+0.4954P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0986
_refine_ls_wR_factor_ref         0.1093
_reflns_number_gt                6365
_reflns_number_total             8474
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol201203g_si_002.cif
_cod_data_source_block           110221_zyx2044
_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_database_code               1502258