9,10,11,12-Tetrachloro-12b-hydroxy-12c-phenyl-1,2,3,3a,5,6,12b,12c-octahydro-8<i>H</i>-cyclopenta[6,7][1,4]oxazepino[5,4-<i>a</i>]isoindol-8-one
Hoong-Kun Fun; Yong-Miao Shen; Jian-Hua Xu; Suchada Chantrapromma; Acta Crystallographica Section E 63 (2007) o495–o497; doi:10.1107/S160053680605567X

data_2212373
_publ_section_title
9,10,11,12-Tetrachloro-12b-hydroxy-12c-phenyl-1,2,3,3a,5,6,12b,12c-octahydro-8<i>H</i>-cyclopenta[6,7][1,4]oxazepino[5,4-<i>a</i>]isoindol-8-one
_journal_coeditor_code           SJ2205
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o495
_journal_page_last               o497
_journal_paper_doi               10.1107/S160053680605567X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C21 H17 Cl4 N O3'
_chemical_formula_moiety         'C21 H17 Cl4 N O3'
_chemical_formula_sum            'C21 H17 Cl4 N O3'
_chemical_formula_weight         473.16
_chemical_melting_point          539.0(10)
_chemical_name_systematic
9,10,11,12-Tetrachloro-12b-hydroxy-12c-phenyl-1,2,3,3a,5,6,12b,12c-octahydro-8H-cyclopenta[6,7][1,4]oxazepino[5,4-a]isoindol-8-one
_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                75.391(2)
_cell_angle_beta                 88.559(2)
_cell_angle_gamma                88.083(2)
_cell_formula_units_Z            4
_cell_length_a                   9.0183(4)
_cell_length_b                   12.5563(5)
_cell_length_c                   18.3224(7)
_cell_measurement_reflns_used    8288
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      1.15
_cell_volume                     2006.26(14)
_computing_cell_refinement       APEX2
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material
;
SHELXTL and PLATON (Spek, 2003)
;
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      297(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type
;
Bruker SMART APEX2 CCD area-detector
;
_diffrn_measurement_method       \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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0337
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29592
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.15
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.8666
_exptl_absorpt_correction_T_min  0.7121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.566
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.438
_refine_diff_density_min         -0.684
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         9537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.147
_refine_ls_R_factor_all          0.0778
_refine_ls_R_factor_gt           0.0697
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0783P)^2^+15.8392P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2138
_refine_ls_wR_factor_ref         0.2227
_reflns_number_gt                8288
_reflns_number_total             9537
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sj2205.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '538-540' was changed to '539.0(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 '538-540' was changed to '539.0(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_database_code               2212373
_cod_database_fobs_code          2212373