Reaction of Fischer alkynylcarbene complexes with 1-azadiene derivatives: unexpected formation of 3,4-dihydropyridines
José Barluenga; Miguel Tomás; Alfredo Ballesteros; Javier Santamaría; Raúl Corzo-Suárez; Santiago García-Granda; New J. Chem. 25 (2001) 8–10; doi:10.1039/b005648k

data_7051026
_publ_section_title
;
 Reaction of Fischer alkynylcarbene complexes with 1-azadiene
 derivatives: unexpected formation of 3,4-dihydropyridines
;
_journal_issue                   1
_journal_name_full               'New J. Chem.'
_journal_page_first              8
_journal_page_last               10
_journal_paper_doi               10.1039/b005648k
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         'C26 H30 N2 O'
_chemical_formula_sum            'C26 H30 N2 O'
_chemical_formula_weight         386.52
_chemical_name_systematic
;
4-phenil-4-(N-ciclohexyl)imidoyl-6-(4-methylphenyl)-
2-methoxi-3,4-dihydropyridin
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2b'
_symmetry_space_group_name_H-M   'P b c 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   6.632(2)
_cell_length_b                   19.859(2)
_cell_length_c                   34.049(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     4484.4(15)
_computing_cell_refinement       'CRYSDA (Beurkens et al., 1992)'
_computing_data_collection
;
CAD-4 Diffractometer Control Software (Enraf-Nonius, 1994)
;
_computing_data_reduction        'REFLEX (Garc\'ia-Granda et al., 1998)'
_computing_molecular_graphics    'Xtal_GX (Hall & Boulay, 1995)'
_computing_publication_material
;
 SHELXL-97 (Sheldrick, 1997). All calculations made at the University of
 Oviedo on the Scientific Computer Center and X-Ray group DEC/AXP-computers
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Nonius CAD-4 diffractometer'
_diffrn_measurement_method       \w-2\Q
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1501
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4015
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        3.39
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.069
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.202
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.029
_refine_ls_goodness_of_fit_ref   1.306
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     592
_refine_ls_number_reflns         4003
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.217
_refine_ls_restrained_S_obs      1.305
_refine_ls_R_factor_all          0.2450
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          -0.017
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1145P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.2829
_reflns_number_gt                1368
_reflns_number_total             4015
_reflns_threshold_expression     I2\s(I)
_cod_data_source_file            b005648k.txt
_cod_data_source_block           njcx_r
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        4484.1(15)
_cod_original_sg_symbol_H-M      p_b_c_21
_cod_database_code               7051026