Chichibabin-Type Condensation of Cyclic Ketones with 3-R-1,2,4-triazin-5(4H)-ones
Ilya N. Egorov; Tatyana A. Tseitler; Igor S. Kovalev; Pavel A. Slepukhin; Vladimir L. Rusinov; Oleg N. Chupakhin; Journal of Organic Chemistry 77 (2012) 6007–6013; doi:10.1021/jo300697v

data_4027298
_publ_contact_author_address
;620002, Russian Federation, Ekaterinburg, Mira St. 19
Ural Federal University, Dept. of Organic Chemistry
;
_publ_contact_author_email       i.n.egorov@gmail.com
_publ_contact_author_fax         +7(343)3740458
_publ_contact_author_name        'Ilya N. Egorov'
_publ_contact_author_phone       +7(343)3754501
_publ_section_title
;
 Chichibabin-Type Condensation of Cyclic Ketones with
 3-R-1,2,4-triazin-5(4H)-ones
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6007
_journal_page_last               6013
_journal_paper_doi               10.1021/jo300697v
_journal_volume                  77
_journal_year                    2012
_chemical_formula_moiety         'C21 H25 N3 O2'
_chemical_formula_sum            'C21 H25 N3 O2'
_chemical_formula_weight         351.44
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
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_symmetry_space_group_name_Hall  '-P 2ybc'
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_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90.00
_cell_angle_beta                 96.562(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.543(2)
_cell_length_b                   6.2491(6)
_cell_length_c                   17.155(2)
_cell_measurement_reflns_used    1491
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.29
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_cell_volume                     1868.3(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.9 (release 23-03-2006 CrysAlis171 .NET)
(compiled Mar 23 2006,23:39:28)
;
_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Xcalibur S CCD'
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_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  0.0395
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_diffrn_reflns_limit_h_max       23
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_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11287
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.78
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
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_exptl_absorpt_coefficient_mu    0.082
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prism
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_refine_diff_density_max         0.223
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4486
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1518
_refine_ls_R_factor_gt           0.0453
_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^)+(0.0230P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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