Methyl 12-Acetyl-9-methyl-11-thioxo-8-oxa-10,12-diazatricyclo[7.3.1.0^2,7^]trideca-2,4,6-triene-13-carboxylate
Kettmann, Viktor; Svetlík, Ján; Acta Crystallographica Section C 53 (1997) 1493–1495; doi:10.1107/S010827019700557X

data_2006619
_publ_contact_author
;
      Dr Viktor Kettmann
      Faculty of Pharmacy
      Comenius University
      Odbojarov 10
      Bratislava
      Slovak Republic    83232
;
_publ_section_title
;Methyl
 12-Acetyl-9-methyl-11-thioxo-8-oxa-10,12-diazatricyclo[7.3.1.0^2,7^]trideca-2,4,6-triene-13-carboxylate
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1493
_journal_page_last               1495
_journal_paper_doi               10.1107/S010827019700557X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C15 H16 N2 O4 S '
_chemical_formula_sum            'C15 H16 N2 O4 S'
_chemical_formula_weight         320.36
_chemical_melting_point          482
_chemical_name_systematic
;
 Methyl 9-Methyl-11-thioxo-8-oxa-12-acetyl-10,12-diazatricyclo[7.3.1.0^2,7^]
 trideca-2,4,6-triene-13-carboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                68.45(3)
_cell_angle_beta                 71.46(3)
_cell_angle_gamma                81.52(3)
_cell_formula_units_Z            2
_cell_length_a                   8.962(3)
_cell_length_b                   9.651(4)
_cell_length_c                   10.009(4)
_cell_measurement_reflns_used    15
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      18
_cell_measurement_theta_min      8
_cell_volume                     762.9(5)
_computing_cell_refinement       'Syntex P2~1~ diffractometer software'
_computing_data_collection       'Syntex P2~1~ diffractometer software'
_computing_data_reduction        'XP21 (Pavel\<c\'ik, 1987)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL-93
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Syntex P2~1~ diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.031
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2893
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  100
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.395
_exptl_crystal_density_meas      1.400(10)
_exptl_crystal_density_method    'flotation in bromoform--hexane'
_exptl_crystal_description       prism
_exptl_crystal_F_000             336
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.623
_refine_diff_density_min         -0.472
_refine_ls_extinction_coef       0.002(5)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.041
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         2715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0713
_refine_ls_R_factor_obs          .0505
_refine_ls_shift/esd_max         0.028
_refine_ls_shift/esd_mean        0.007
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.4132P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1453
_refine_ls_wR_factor_obs         .1133
_reflns_number_observed          2008
_reflns_number_total             2715
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            sk1098.cif
_cod_data_source_block           default
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.4132P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0905P)^2^+0.4132P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               2006619