2-Amino-7-methyl-4-(3,4-methylenedioxyphenyl)-5-oxopyrano[3,2-<i>c</i>]pyran-3-carbonitrile <i>N,N</i>-dimethylformamide solvate
Daqing Shi; Lihui Niu; Xiangshan Wang; Qiya Zhuang; Yong Zhang; Acta Crystallographica Section E 60 (2004) o2371–o2373; doi:10.1107/S1600536804029289

data_2204763
_publ_section_title
;2-Amino-7-methyl-4-(3,4-methylenedioxyphenyl)-5-oxopyrano[3,2-<i>c</i>]pyran-3-carbonitrile
 <i>N,N</i>-dimethylformamide solvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2371
_journal_page_last               o2373
_journal_paper_doi               10.1107/S1600536804029289
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C17 H12 N2 O5, C3 H7 N O'
_chemical_formula_moiety         'C17 H12 N2 O5, C3 H7 N O'
_chemical_formula_sum            'C20 H19 N3 O6'
_chemical_formula_weight         397.38
_chemical_melting_point          502.0(10)
_chemical_name_systematic
;
2-Amino-7-methyl-4-(3,4-methylenedioxyphenyl)-5-oxopyrano[3,2-c]pyran-3-
carbonitrile N,N-dimethylformamide 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
_cell_angle_alpha                107.117(5)
_cell_angle_beta                 93.142(3)
_cell_angle_gamma                104.813(5)
_cell_formula_units_Z            2
_cell_length_a                   6.7513(18)
_cell_length_b                   11.010(3)
_cell_length_c                   13.740(4)
_cell_measurement_reflns_used    3676
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     934.2(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2003)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0167
_diffrn_reflns_av_sigmaI/netI    0.0240
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9243
_diffrn_reflns_theta_full        25.33
_diffrn_reflns_theta_max         25.33
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.106
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.924
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.181
_refine_diff_density_min         -0.200
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0446
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0516P)^2^+0.295P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0974
_refine_ls_wR_factor_ref         0.1018
_reflns_number_gt                3042
_reflns_number_total             3391
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6426.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '501-503' was changed to '502.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '501-503' was changed to '502.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        934.2(5)
_cod_database_code               2204763
_cod_database_fobs_code          2204763