Unprecedented Synthesis of 3-Alkenyl-3-ethoxy-2-iminoketones via 1,3-Dipolar Cycloadditions of Nitrones with Alkynyl Fischer Carbene Complexes
Flores-Conde, María Inés; Vázquez, Miguel Angel; Reyes, Leonor; Tamariz, Joaquín; Delgado, Francisco; Organometallics 32 (2013) 4244–; doi:10.1021/om400420c

data_4081208
_publ_section_title
;
 Unprecedented Synthesis of 3-Alkenyl-3-ethoxy-2-iminoketones via
 1,3-Dipolar Cycloadditions of Nitrones with Alkynyl Fischer Carbene
 Complexes
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4244
_journal_paper_doi               10.1021/om400420c
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C25 H22 N4 O7'
_chemical_formula_sum            'C25 H22 N4 O7'
_chemical_formula_weight         490.47
_chemical_melting_point          428.5(5)
_chemical_name_systematic
;
(2Z,3Z)-3-ethoxy-2-[2-(2,4-dinitrophenyl)hidrazono]-4-(4-methoxyphenyl)-1-phenylbut-3-en-1-one 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.767(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8392(2)
_cell_length_b                   17.8601(4)
_cell_length_c                   13.5960(3)
_cell_measurement_reflns_used    6997
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      32.4372
_cell_measurement_theta_min      2.6885
_cell_volume                     2377.12(9)
_computing_cell_refinement
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_data_collection
;
        CrysAlis CCD, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_data_reduction
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.871
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S'
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0269
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            15662
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         32.46
_diffrn_reflns_theta_min         2.70
_diffrn_standards_decay_%        <2%
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_T_max  0.9848
_exptl_absorpt_correction_T_min  0.9789
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        CrysAlis RED, Oxford Diffraction Ltd.,
        Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET)
        (compiled Jun 10 2008,16:49:55)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.948
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         7468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.0958
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0883P)^2^+1.0776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1642
_refine_ls_wR_factor_ref         0.1796
_reflns_number_gt                4856
_reflns_number_total             7468
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om400420c_si_003.cif
_cod_data_source_block           0038-fdr
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '428-429K' was changed to '428.5(5)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_database_code               4081208