Ethyl 6-amino-2-(chloromethyl)-5-cyano-4-<i>o</i>-tolyl-4<i>H</i>-pyran-3-carboxylate
S. Athimoolam; N. Savitha Devi; S. Asath Bahadur; R. Sayee Kannan; S. Perumal; Acta Crystallographica Section E 63 (2007) o4680–o4681; doi:10.1107/S160053680705581X

data_2216781
_publ_section_title
;Ethyl
 6-amino-2-(chloromethyl)-5-cyano-4-<i>o</i>-tolyl-4<i>H</i>-pyran-3-carboxylate
;
_journal_coeditor_code           SJ2408
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4680
_journal_page_last               o4681
_journal_paper_doi               10.1107/S160053680705581X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C17 H17 Cl N2 O3'
_chemical_formula_moiety         'C17 H17 Cl N2 O3'
_chemical_formula_sum            'C17 H17 Cl N2 O3'
_chemical_formula_weight         332.78
_chemical_name_systematic
;
Ethyl 6-amino-2-(chloromethyl)-5-cyano-4-o-tolyl-4H-pyran-3-carboxylate
;
_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           SHELXTL/PC
_cell_angle_alpha                109.030(11)
_cell_angle_beta                 100.769(15)
_cell_angle_gamma                103.813(16)
_cell_formula_units_Z            2
_cell_length_a                   8.5734(5)
_cell_length_b                   9.7735(7)
_cell_length_c                   11.0781(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.27
_cell_measurement_theta_min      9.65
_cell_volume                     815.96(17)
_computing_cell_refinement       'CAD4 Express (Enraf--Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf--Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics
;
ORTEP-3  (Farrugia, 1997) and PLATON (Spek, 2003)
;
_computing_publication_material  'SHELXTL/PC (Bruker, 2000)'
_computing_structure_refinement  'SHELXTL/PC (Bruker, 2000)'
_computing_structure_solution    'SHELXTL/PC (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf--Nonius MACH3'
_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  0.0113
_diffrn_reflns_av_sigmaI/netI    0.0255
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3482
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.03
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.250
_exptl_absorpt_correction_T_max  0.9654
_exptl_absorpt_correction_T_min  0.9479
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.304
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         2858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0411
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.4918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1037
_refine_ls_wR_factor_ref         0.1311
_reflns_number_gt                1993
_reflns_number_total             2858
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2408.cif
_cod_data_source_block           I
_cod_database_code               2216781
_cod_database_fobs_code          2216781