6-Chloro-2-(4-chlorophenoxy)-2-thioxo-4-trichloromethyl-4<i>H</i>-1,3,2-benzodioxaphosphorine
Krishnaiah, M.; Radha Krishna, J.; Jagadeesh Kumar, N.; Devandranath Reddy, C.; Rao, S. N.; Acta Crystallographica Section E 63 (2007) o731–o732; doi:10.1107/S160053680700092X

data_2212340
_publ_section_title
6-Chloro-2-(4-chlorophenoxy)-2-thioxo-4-trichloromethyl-4<i>H</i>-1,3,2-benzodioxaphosphorine
_journal_coeditor_code           RZ2105
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o731
_journal_page_last               o732
_journal_paper_doi               10.1107/S160053680700092X
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          'C14 H8 Cl5 O3 P S'
_chemical_formula_moiety         'C14 H8 Cl5 O3 P S'
_chemical_formula_sum            'C14 H8 Cl5 O3 P S'
_chemical_formula_weight         464.48
_chemical_name_systematic
;
6-Chloro-2-(4-chlorophenoxy)-2-thioxo-4-trichloromethyl-4H-1,3,2-
benzodioxaphosphorine
;
_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                100.694(10)
_cell_angle_beta                 101.516(8)
_cell_angle_gamma                112.166(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4022(9)
_cell_length_b                   10.6065(10)
_cell_length_c                   10.6577(9)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      2.04
_cell_volume                     923.75(18)
_computing_cell_refinement       'SAINT (Bruker 2002)'
_computing_data_collection       'SMART (Bruker 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ZORTEPII (Zsolnai, 1997)'
_computing_publication_material
;
enCIFer (Allen <i>et al.</i>,  2004) and PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
;
Siemens SMART 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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3412
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.04
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.995
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_meas      1.67
_exptl_crystal_density_method    'KI flotation'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     249
_refine_ls_number_reflns         3192
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0386P)^2^+0.3459P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0975
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                1981
_reflns_number_total             3192
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            rz2105.cif
_cod_data_source_block           I
_cod_database_code               2212340
_cod_database_fobs_code          2212340