3-[α-(2-Hydroxyethylamino)benzylidene]-2-methoxy-2,3-dihydro-1,2λ^5^-benzoxaphosphinine-2,4-dione
Małecka, Magdalena; Budzisz, Elżbieta; Acta Crystallographica Section E 62 (2006) o4560–o4562; doi:10.1107/S1600536806037469

data_2210613
_publ_section_title
3-[\a-(2-Hydroxyethylamino)benzylidene]-2-methoxy-2,3-dihydro-1,2\l^5^-benzoxaphosphinine-2,4-dione
_journal_coeditor_code           GD2014
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4560
_journal_page_last               o4562
_journal_paper_doi               10.1107/S1600536806037469
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C18 H18 N O5 P'
_chemical_formula_moiety         'C18 H18 N O5 P'
_chemical_formula_sum            'C18 H18 N O5 P'
_chemical_formula_weight         359.30
_chemical_name_systematic
;
3-[\a-(2-Hydroxyethylamino)benzylidene]-2-methoxy-2,3-dihydro-
1,2\l^5^-benzoxaphosphinine-2,4-dione
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 114.513(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.178(3)
_cell_length_b                   9.8913(6)
_cell_length_c                   19.1983(19)
_cell_measurement_reflns_used    4841
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      25.95
_cell_measurement_theta_min      2.35
_cell_volume                     3313.6(7)
_computing_cell_refinement       'Win-Cell in IPDS-II Software'
_computing_data_collection
'Win-Xpose in IPDS-II Software (Stoe & Cie,  2000)'
_computing_data_reduction        'Win-Integrate in IPDS-II Software'
_computing_molecular_graphics
;
PLATON (Spek, 2003)
;
_computing_publication_material  'PARST97 (Nardelli, 1996)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193(2)
_diffrn_detector_area_resol_mean 150
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Stoe IPDS-II'
_diffrn_measurement_method       \f
_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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0427
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16527
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(XPREP; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.475
_refine_diff_density_min         -0.421
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3166
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.945
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0380
_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^)+(0.0716P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0966
_refine_ls_wR_factor_ref         0.1025
_reflns_number_gt                2339
_reflns_number_total             3166
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gd2014.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               2210613
_cod_database_fobs_code          2210613