#------------------------------------------------------------------------------ #$Date: 2008-02-08 10:23:56 +0000 (Fri, 08 Feb 2008) $ #$Revision: 101 $ #$URL: svn://www.crystallography.net/cod/cif/2/2203586.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2203586 loop_ _publ_author_name 'Ying Peng' 'Su-Yuan Xie' 'Shun-Liu Deng' 'Rong-Bin Huang' 'Lan-Sun Zheng' _publ_section_title ; 1,2,3,5,6,7,8,9-Octachlorocyclopenta[def]phenanthren-4-one ; _journal_issue 5 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first o899 _journal_page_last o900 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac 'C15 Cl8 O' _chemical_formula_moiety 'C15 Cl8 O' _chemical_formula_sum 'C15 Cl8 O' _chemical_formula_weight 479.75 _chemical_name_systematic ; 1,2,3,5,6,7,8,9-Octachloro-cyclopenta[def]phenanthren-4-one ; _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_formula_units_Z 8 _cell_length_a 22.979(5) _cell_length_b 8.7180(17) _cell_length_c 15.697(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 15.0 _cell_measurement_theta_min 8.0 _cell_volume 3144.6(11) _computing_cell_refinement 'CAD-4 Software' _computing_data_collection 'CAD-4 Software (Enraf--Nonius, 1988)' _computing_data_reduction 'XCAD4 (Harms, 1997)' _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 298(2) _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Enraf--Nonius CAD-4 diffractometer' _diffrn_measurement_method '\w scan' _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 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 1588 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 1.77 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 60 _diffrn_standards_number 3 _exptl_absorpt_coefficient_mu 1.432 _exptl_absorpt_correction_T_max 0.7826 _exptl_absorpt_correction_T_min 0.6572 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details '(\y scan; North et al., 1968)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.027 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.301 _refine_diff_density_min -0.290 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_matrix_type full _refine_ls_number_parameters 112 _refine_ls_number_reflns 1588 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.042 _refine_ls_R_factor_all 0.0849 _refine_ls_R_factor_gt 0.0498 _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^)+(0.0421P)^2^+1.1559P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0975 _refine_ls_wR_factor_ref 0.1099 _reflns_number_gt 1078 _reflns_number_total 1588 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cv6304.cif loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' '-x, y+1/2, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1, z+1/2' '-x+1/2, y+1, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' 'x, -y-1/2, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y, -z-1/2' 'x+1/2, -y, z-1/2' '-x+1/2, y+1/2, z' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol Cl1 0.43537(5) 0.11507(13) 0.40342(7) 0.0550(3) Uani d . 1 Cl Cl2 0.36045(5) 0.61323(15) 0.75240(9) 0.0697(4) Uani d . 1 Cl Cl3 0.27914(5) 0.42763(17) 0.63532(9) 0.0743(4) Uani d . 1 Cl Cl4 0.32524(5) 0.21792(16) 0.49757(9) 0.0744(5) Uani d . 1 Cl C1 0.46970(16) 0.2195(4) 0.4813(2) 0.0404(10) Uani d . 1 C C2 0.38952(18) 0.5000(5) 0.6740(2) 0.0459(10) Uani d . 1 C C3 0.35317(17) 0.4146(5) 0.6191(3) 0.0468(11) Uani d . 1 C C4 0.37460(18) 0.3197(4) 0.5559(3) 0.0435(10) Uani d . 1 C C5 0.43605(17) 0.3064(4) 0.5427(2) 0.0395(9) Uani d . 1 C C6 0.46890(17) 0.3929(4) 0.5985(2) 0.0376(9) Uani d . 1 C C7 0.44829(17) 0.4884(5) 0.6634(2) 0.0412(9) Uani d . 1 C C8 0.5000 0.5560(7) 0.7077(4) 0.0462(15) Uani d S 1 C O1 0.5000 0.6456(5) 0.7663(3) 0.0623(12) Uani d S 1 O loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.0599(7) 0.0569(7) 0.0481(6) -0.0067(6) -0.0075(5) -0.0114(6) Cl2 0.0654(8) 0.0785(8) 0.0653(7) 0.0143(7) 0.0153(6) -0.0192(7) Cl3 0.0405(6) 0.0975(10) 0.0849(9) 0.0068(7) 0.0074(6) -0.0121(8) Cl4 0.0440(6) 0.0892(10) 0.0899(9) -0.0090(7) -0.0077(7) -0.0285(8) C1 0.050(2) 0.037(2) 0.034(2) -0.0036(19) -0.0049(17) -0.0022(18) C2 0.053(2) 0.046(2) 0.039(2) 0.008(2) 0.008(2) 0.002(2) C3 0.037(2) 0.049(3) 0.054(3) 0.001(2) 0.0002(19) 0.005(2) C4 0.042(2) 0.041(2) 0.047(2) 0.0007(19) -0.0031(19) 0.004(2) C5 0.045(2) 0.034(2) 0.040(2) -0.0043(19) -0.0002(19) 0.0049(19) C6 0.043(2) 0.033(2) 0.036(2) 0.0022(19) 0.0007(18) 0.0048(17) C7 0.048(2) 0.038(2) 0.038(2) 0.001(2) 0.0022(19) 0.0012(19) C8 0.064(4) 0.044(3) 0.031(3) 0.000 0.000 -0.002(3) O1 0.068(3) 0.063(3) 0.056(3) 0.000 0.000 -0.019(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C1 . 1.717(4) y Cl2 C2 . 1.713(4) y Cl3 C3 . 1.724(4) y Cl4 C4 . 1.706(4) y C1 C1 12_655 1.392(8) y C1 C5 . 1.450(5) y C2 C7 . 1.365(5) y C2 C3 . 1.413(6) y C3 C4 . 1.382(6) y C4 C5 . 1.432(5) y C5 C6 . 1.379(5) y C6 C7 . 1.398(5) y C6 C6 12_655 1.429(8) y C7 C8 . 1.498(5) y C8 O1 . 1.206(7) y C8 C7 12_655 1.498(5) y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C1 C1 C5 12_655 . 122.2(2) y C1 C1 Cl1 12_655 . 117.36(13) y C5 C1 Cl1 . . 120.4(3) y C7 C2 C3 . . 118.1(4) y C7 C2 Cl2 . . 121.1(3) y C3 C2 Cl2 . . 120.8(3) y C4 C3 C2 . . 122.9(4) y C4 C3 Cl3 . . 119.8(3) y C2 C3 Cl3 . . 117.3(3) y C3 C4 C5 . . 120.2(4) y C3 C4 Cl4 . . 117.3(3) y C5 C4 Cl4 . . 122.4(3) y C6 C5 C4 . . 113.8(4) y C6 C5 C1 . . 114.5(3) y C4 C5 C1 . . 131.6(4) y C5 C6 C7 . . 127.0(4) y C5 C6 C6 . 12_655 123.2(2) y C7 C6 C6 . 12_655 109.8(2) y C2 C7 C6 . . 118.0(4) y C2 C7 C8 . . 134.3(4) y C6 C7 C8 . . 107.7(4) y O1 C8 C7 . . 127.5(2) y O1 C8 C7 . 12_655 127.5(2) y C7 C8 C7 . 12_655 105.0(5) y