5-Ethyl-6-oxo-4-thioxo-1,3,2-oxazaphospholidino[3,2-<i>a</i>][1,3,2]benzodiazaphosphorine
Sheng-Lou Deng; Ru-Yu Chen; Xue-Bing Leng; Lin-Hong Weng; Acta Crystallographica Section E 59 (2003) o285–o287; doi:10.1107/S1600536803002290

data_2202223
_publ_section_title
5-Ethyl-6-oxo-4-thioxo-1,3,2-oxazaphospholidino[3,2-<i>a</i>][1,3,2]benzodiazaphosphorine
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o285
_journal_page_last               o287
_journal_paper_doi               10.1107/S1600536803002290
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          'C11 H13 N2 O2 P S'
_chemical_formula_moiety         'C11 H13 N2 O2 P S'
_chemical_formula_sum            'C11 H13 N2 O2 P S'
_chemical_formula_weight         268.26
_chemical_melting_point          384
_chemical_name_systematic
;
5-Ethyl-6-oxo-4-thioxo-1,3,2-
oxazaphospholidino[3,2-a][1,3,2]benzodiazaphosphorine
;
_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           SHELXL-97
_cell_angle_alpha                61.633(2)
_cell_angle_beta                 78.828(2)
_cell_angle_gamma                83.139(2)
_cell_formula_units_Z            2
_cell_length_a                   6.9347(7)
_cell_length_b                   9.9827(10)
_cell_length_c                   10.4868(11)
_cell_measurement_reflns_used    231
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      22.80
_cell_measurement_theta_min      2.80
_cell_volume                     626.38(11)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1997)'
_computing_data_reduction        'SHELXTL (Bruker, 1997)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-7 (Sheldrick, 1997)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_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  0.0166
_diffrn_reflns_av_sigmaI/netI    0.0193
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2621
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.377
_exptl_absorpt_correction_T_max  0.927
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.441
_refine_diff_density_min         -0.286
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2208
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0414
_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^)+(0.0718P)^2^+0.2182P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1127
_refine_ls_wR_factor_ref         0.1184
_reflns_number_gt                1940
_reflns_number_total             2208
_reflns_threshold_expression     I>2\s(1)
_cod_data_source_file            ww6058.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2202223
_cod_database_fobs_code          2202223