(<i>E</i>)-3-{[(Dimethoxythiophosphoryl)methylhydrazono]methyl}-4<i>H</i>-1-benzopyran-4-one, a new chromone derivative substituted with phosphorohydrazide at position 3
Rybarczyk-Pirek, Agnieszka J.; Nawrot-Modranka, Jolanta; Acta Crystallographica Section E 60 (2004) o988–o990; doi:10.1107/S1600536804010943

data_2203738
_publ_section_title
;(<i>E</i>)-3-{[(Dimethoxythiophosphoryl)methylhydrazono]methyl}-4<i>H</i>-1-benzopyran-4-one,
 a new chromone derivative substituted with phosphorohydrazide at position 3
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o988
_journal_page_last               o990
_journal_paper_doi               10.1107/S1600536804010943
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C13 H15 N2 O4 P S'
_chemical_formula_moiety         'C13 H15 N2 O4 P S'
_chemical_formula_sum            'C13 H15 N2 O4 P S'
_chemical_formula_weight         326.30
_chemical_name_systematic
(E)-3-{[(Dimethoxythiophosphoryl)methylhydrazono]methyl}-4H-1-benzopyran-4-one
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.146(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.5760(9)
_cell_length_b                   14.9072(9)
_cell_length_c                   12.0912(5)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.62
_cell_measurement_theta_min      20.10
_cell_volume                     1544.7(2)
_computing_cell_refinement       'MSC/AFC Software Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1989)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'PLATON (Spek, 1998)'
_computing_publication_material
;
SHELXL97,  PARST97 (Nardelli, 1996) and WinGX (Farrugia, 1999)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_sigmaI/netI    0.1522
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2930
_diffrn_reflns_theta_full        68.50
_diffrn_reflns_theta_max         68.50
_diffrn_reflns_theta_min         4.71
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.001
_exptl_absorpt_correction_T_max  0.7254
_exptl_absorpt_correction_T_min  0.5297
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.619
_refine_diff_density_min         -0.248
_refine_ls_extinction_coef       0.0009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.1403
_refine_ls_R_factor_gt           0.0471
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w = [exp{4.20(sin\q/\l)^2^}]/[\s^2^(Fo^2^)+(0.0533P)^2^]
where P = 0.33Fo^2^ + 0.67Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1112
_refine_ls_wR_factor_ref         0.1273
_reflns_number_gt                1105
_reflns_number_total             2751
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv6309.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2203738
_cod_database_fobs_code          2203738