Methyl 2-amino-4-(4-chlorophenyl)-4<i>H</i>-pyrano[3,2-<i>c</i>]coumarin-3-carboxylate <i>N</i>,<i>N</i>-dimethylformamide solvate
Daqing Shi; Nan Wu; Qiya Zhuang; Yong Zhang; Acta Crystallographica Section E 61 (2005) o87–o89; doi:10.1107/S1600536804032040

data_2204948
_publ_section_title
;Methyl
 2-amino-4-(4-chlorophenyl)-4<i>H</i>-pyrano[3,2-<i>c</i>]coumarin-3-carboxylate
 <i>N</i>,<i>N</i>-dimethylformamide solvate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o87
_journal_page_last               o89
_journal_paper_doi               10.1107/S1600536804032040
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C20 H14 Cl N O5, C3 H7 N O'
_chemical_formula_moiety         'C20 H14 Cl N O5, C3 H7 N O'
_chemical_formula_sum            'C23 H21 Cl N2 O6'
_chemical_formula_weight         456.87
_chemical_melting_point          490.0(10)
_chemical_name_common
;
Methyl 2-amino-4-(4-chlorophenyl)-4H-pyrano[3,2-c]coumarin-3-carboxylate
N,N-dimethylformamide solvate
;
_chemical_name_systematic
;
methyl
2-amino-4-(4-chlorophenyl)-5-oxo-4H,5H-pyrano[3,2-c]chromene-3-carboxylate
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                62.186(5)
_cell_angle_beta                 89.802(8)
_cell_angle_gamma                74.080(6)
_cell_formula_units_Z            2
_cell_length_a                   7.5757(5)
_cell_length_b                   12.7812(4)
_cell_length_c                   12.9142(8)
_cell_measurement_reflns_used    3920
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.3
_cell_measurement_theta_min      3.1
_cell_volume                     1052.09(12)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Corporation, 2000)'
_computing_data_reduction        'CrystalStructure (Rigaku/MSC, 2003)'
_computing_molecular_graphics    'program (reference)?'
_computing_publication_material  'program (reference)?'
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0163
_diffrn_reflns_av_sigmaI/netI    0.0260
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10329
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.226
_exptl_absorpt_correction_T_max  0.9190
_exptl_absorpt_correction_T_min  0.8596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.69
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.257
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     301
_refine_ls_number_reflns         3814
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0561P)^2^+0.3138P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1020
_reflns_number_gt                3463
_reflns_number_total             3814
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ob6453.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '489-491' was changed to '490.0(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 '489-491' was changed to '490.0(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_sg_symbol_Hall     '-p 1'
_cod_database_code               2204948
_cod_database_fobs_code          2204948