5-Ethoxycarbonyl-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic anhydride ethyl acetate solvate
Sun, Feng-Xia; Yu, Yi-Feng; Guo, Xing-Na; Guo, Jun-Yong; Acta Crystallographica Section E 62 (2006) o83–o84; doi:10.1107/S1600536805039772

data_2207943
_publ_section_title
;5-Ethoxycarbonyl-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3-carboxylic
 anhydride ethyl acetate solvate
;
_journal_coeditor_code           XU6072
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o83
_journal_page_last               o84
_journal_paper_doi               10.1107/S1600536805039772
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C34 H34 N4 O11, C4 H8 O2'
_chemical_formula_moiety         'C34 H34 N4 O11, C4 H8 O2'
_chemical_formula_sum            'C38 H42 N4 O13'
_chemical_formula_weight         762.76
_chemical_melting_point          .45E-305
_chemical_name_common
;
5-Ethoxycarbonyl-2,6-dimethyl-4-
(m-nitrophenyl)-1,4-dihydro-pyridine-3-carboxylic acid anhydride
ethyl acetate solvate
;
_chemical_name_systematic
;
5-Ethoxycarbonyl-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydro-pyridine-
3-carboxylic anhydride ethyl acetate solvate
;
_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           SHELXL-97
_cell_angle_alpha                99.59(3)
_cell_angle_beta                 106.29(3)
_cell_angle_gamma                105.69(3)
_cell_formula_units_Z            2
_cell_length_a                   10.896(2)
_cell_length_b                   12.017(2)
_cell_length_c                   16.162(3)
_cell_measurement_reflns_used    15558
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      3.2
_cell_volume                     1887.1(9)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       'PROCESS-AUTO (Rigaku, 1998)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2002)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2002)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.038
_diffrn_reflns_av_sigmaI/netI    0.068
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15558
_diffrn_reflns_theta_full        25.5
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.102
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.57
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     504
_refine_ls_number_reflns         6953
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.102
_refine_ls_R_factor_gt           0.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1184P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.187
_refine_ls_wR_factor_ref         0.206
_reflns_number_gt                4362
_reflns_number_total             6953
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            xu6072.cif
_cod_data_source_block           I
_cod_database_code               2207943
_cod_database_fobs_code          2207943