Dimethyl 2-[(<i>E</i>)-(hydroxyimino)methyl]-6-methyl-4-(2-thienyl)-1,4-dihydropyridine-3,5-dicarboxylate
Švorc, Ľubomír; Vrábel, Viktor; Kožíšek, Jozef; Marchalín, Štefan; Šafář Peter; Acta Crystallographica Section E 63 (2007) o2240–o2242; doi:10.1107/S1600536807014122

data_2213254
_publ_section_title
;Dimethyl
 2-[(<i>E</i>)-(hydroxyimino)methyl]-6-methyl-4-(2-thienyl)-1,4-dihydropyridine-3,5-dicarboxylate
;
_journal_coeditor_code           CS2032
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2240
_journal_page_last               o2242
_journal_paper_doi               10.1107/S1600536807014122
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C15 H16 N2 O5 S'
_chemical_formula_moiety         'C15 H16 N2 O5 S'
_chemical_formula_sum            'C15 H16 N2 O5 S'
_chemical_formula_weight         336.36
_chemical_name_systematic
;
Dimethyl 2-[(E)-(hydroxyimino)methyl]-6-methyl-4-(2-thienyl)-
1,4-dihydropyridine-3,5-dicarboxylate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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            4
_cell_length_a                   8.3272(2)
_cell_length_b                   10.0252(2)
_cell_length_c                   19.1730(4)
_cell_measurement_reflns_used    14100
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.92
_cell_measurement_theta_min      3.18
_cell_volume                     1600.60(6)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED
;
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2002)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295
_diffrn_detector_area_resol_mean 10.4340
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Oxford Diffraction Gemini R CCD'
_diffrn_measurement_method
;
Rotation method data acquisition using \w and \f
;
_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  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0445
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            31461
_diffrn_reflns_theta_full        29.01
_diffrn_reflns_theta_max         29.01
_diffrn_reflns_theta_min         3.24
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.229
_exptl_absorpt_correction_T_max  0.93404
_exptl_absorpt_correction_T_min  0.92903
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(Clark & Reid, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.215
_refine_diff_density_min         -0.166
_refine_ls_abs_structure_details 'Flack (1983), 1539 Friedel pairs????'
_refine_ls_abs_structure_Flack   0.03(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0571
_refine_ls_R_factor_gt           0.0344
_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^)+(0.0499P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0795
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                2676
_reflns_number_total             3981
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            cs2032.cif
_cod_data_source_block           I
_cod_database_code               2213254
_cod_database_fobs_code          2213254