Methyl 5-[<i>N</i>,<i>N</i>-bis(methoxycarbonylmethyl)amino]-4-cyano-2-methoxycarbonyl-3-thiopheneethanoate
Wang, Qiang; Li, Zhong-Shu; Sun, Bai-Wang; Acta Crystallographica Section E 64 (2008) o1927–; doi:10.1107/S1600536808028699

data_2219699
_publ_section_title
;Methyl
 5-[<i>N</i>,<i>N</i>-bis(methoxycarbonylmethyl)amino]-4-cyano-2-methoxycarbonyl-3-thiopheneethanoate
;
_journal_coeditor_code           SG2258
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1927
_journal_paper_doi               10.1107/S1600536808028699
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C16 H18 N2 O8 S'
_chemical_formula_moiety         'C16 H18 N2 O8 S'
_chemical_formula_sum            'C16 H18 N2 O8 S'
_chemical_formula_weight         398.38
_chemical_name_systematic
;
methyl
5-[<i>N</i>,<i>N</i>-bis(methoxycarbonylmethyl)amino]-4-cyano-2-
methoxycarbonyl-3-thiophene-ethanoate
;
_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           SHELXL97
_cell_angle_alpha                98.05(3)
_cell_angle_beta                 96.71(3)
_cell_angle_gamma                95.81(3)
_cell_formula_units_Z            2
_cell_length_a                   9.7164(19)
_cell_length_b                   9.790(2)
_cell_length_c                   10.170(2)
_cell_measurement_reflns_used    6733
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      3.31
_cell_volume                     944.5(3)
_computing_cell_refinement       'CrystalClear (Rigaku, 2005)'
_computing_data_collection       'CrystalClear (Rigaku, 2005)'
_computing_data_reduction        'CrystalClear (Rigaku, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick,2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku SCXmini'
_diffrn_measurement_method       '\w scans'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0334
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9976
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.14
_exptl_absorpt_coefficient_mu    0.217
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2005)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.401
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.2500
_exptl_crystal_size_mid          0.2000
_exptl_crystal_size_min          0.1800
_refine_diff_density_max         0.331
_refine_diff_density_min         -0.383
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         4313
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0620P)^2^+0.4110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                3561
_reflns_number_total             4313
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sg2258.cif
_cod_data_source_block           I
_cod_database_code               2219699
_cod_database_fobs_code          2219699