Silver triflate and N-heterocyclic carbene co-catalyzed reaction of N'-(2-alkynylbenzylidene)hydrazide, methanol with alpha,beta-unsaturated aldehyde.
Chen, Zhiyuan; Yu, Xingxin; Wu, Jie; Chemical communications (Cambridge, England) 46 (2010) 6356–6358; doi:10.1039/c0cc01207f

data_7113015
_publ_section_title
;
 Silver triflate and N-heterocyclic carbene co-catalyzed reaction of
 N'-(2-alkynylbenzylidene)hydrazide, methanol with alpha,beta-unsaturated
 aldehyde.
;
_journal_issue                   34
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6356
_journal_page_last               6358
_journal_paper_doi               10.1039/c0cc01207f
_journal_volume                  46
_journal_year                    2010
_chemical_formula_sum            'C34 H33 Br Cl N2 O4.5 S'
_chemical_formula_weight         689.04
_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                109.666(2)
_cell_angle_beta                 107.568(2)
_cell_angle_gamma                105.852(2)
_cell_formula_units_Z            2
_cell_length_a                   12.3918(15)
_cell_length_b                   12.6265(16)
_cell_length_c                   12.6305(15)
_cell_measurement_reflns_used    2252
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      45.706
_cell_measurement_theta_min      5.420
_cell_volume                     1612.2(3)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0796
_diffrn_reflns_av_sigmaI/netI    0.0910
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8502
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.465
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6578
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             710
_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.381
_exptl_crystal_size_min          0.207
_refine_diff_density_max         2.071
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     386
_refine_ls_number_reflns         5903
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0755
_refine_ls_shift/su_max          0.132
_refine_ls_shift/su_mean         0.026
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1488P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2185
_refine_ls_wR_factor_ref         0.2363
_reflns_number_gt                3489
_reflns_number_total             5903
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0cc01207f.txt
_cod_data_source_block           cd20199
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C34 H33 Br Cl N2 O4.50 S'
_cod_database_code               7113015