2-(Bromophenylimino)-10-oxo-9-oxa-1-thia-3,4-diazaspiro[4.15]eicosa-3-ene
Li, Jian-Jun; Jin, Shu-Hui; Liang, Xiao-Mei; Yuan, De-Kai; Wang, Dao-Quan; Acta Crystallographica Section E 63 (2007) o1940–o1941; doi:10.1107/S1600536807012330

data_2212842
_publ_section_title
;
 2-(Bromophenylimino)-10-oxo-9-oxa-1-thia-3,4-diazaspiro[4.15]eicosa-3-ene
;
_journal_coeditor_code           CV2212
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1940
_journal_page_last               o1941
_journal_paper_doi               10.1107/S1600536807012330
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C22 H30 Br N3 O2 S'
_chemical_formula_moiety         'C22 H30 Br N3 O2 S'
_chemical_formula_sum            'C22 H30 Br N3 O2 S'
_chemical_formula_weight         480.46
_chemical_melting_point          364.0(10)
_chemical_name_systematic
;
2-(Bromophenylimino)-10-oxo-9-oxa-1-thia-3,4-diazaspiro[4.15]-3-eicosa-3-ene
;
_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                79.297(4)
_cell_angle_beta                 87.928(4)
_cell_angle_gamma                79.413(4)
_cell_formula_units_Z            2
_cell_length_a                   9.6152(18)
_cell_length_b                   10.527(2)
_cell_length_c                   12.013(2)
_cell_measurement_reflns_used    1127
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      19.38
_cell_measurement_theta_min      2.66
_cell_volume                     1174.5(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 1998)'
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      292(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Bruker SMART 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  0.0221
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5899
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.73
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.861
_exptl_absorpt_correction_T_max  0.8358
_exptl_absorpt_correction_T_min  0.7072
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.552
_refine_diff_density_min         -0.242
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4285
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0598
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0698P)^2^+0.1277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1306
_refine_ls_wR_factor_ref         0.1589
_reflns_number_gt                2578
_reflns_number_total             4285
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            cv2212.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '363--365' was changed to '364.0(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 '363--365' was changed to '364.0(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_cell_volume        1174.4(4)
_cod_database_code               2212842
_cod_database_fobs_code          2212842