# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 188/221 data_global _publ_requested_journal ' J. Chem. Soc., Perkin Trans. 2' _publ_section_title ; Selenium and Tellurium Overcrowded Homomerous Bistricyclic Aromatic Enes ; _publ_contact_author_name ' Israel Agranat' _publ_contact_author_address ; Department of Organic Chemistry The Hebrew University of Jerusalem Jerusalem 91904, ISRAEL ; _publ_contact_author_fax ' 972-2-6511907 ' _publ_contact_author_email ' isria@vms.huji.ac.il ' loop_ _publ_author_name ; A. Levy, P. U. Biedermann, S. Cohen and I. Agranat ; _publ_author_address ;Department of Organic Chemistry The Hebrew University of Jerusalem Jerusalem 91904, ISRAEL ; #----------------------------------------------------------------------- data_7 #----------------------------------------------------------------------- _audit_creation_date 'Mon Oct 25 13:57:44 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'Philips Diffractometer Control' _computing_cell_refinement 'Philips Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 18.215(3) _cell_length_b 5.947(1) _cell_length_c 18.071(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1957.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 13.0 _cell_measurement_theta_max 15.0 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P c a 21 ' _symmetry_Int_Tables_number 29 _symmetry_space_group_name_Hall ? 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' #----------------------------------------------------------------------- _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 486.33 _chemical_formula_moiety 'C 26 H 16 Se 2' _chemical_compound_source ? _exptl_crystal_F_000 960.00 _exptl_absorpt_coefficient_mu 3.787 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.457 _exptl_absorpt_correction_T_min 0.821 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'Philips PW1100/20' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 3 4 2 10 4 1 5 11 _diffrn_reflns_number 2624 _reflns_number_total 2624 _reflns_number_observed 1885 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.03870 _diffrn_orient_matrix_UB_12 -0.01330 _diffrn_orient_matrix_UB_13 -0.00284 _diffrn_orient_matrix_UB_21 0.00293 _diffrn_orient_matrix_UB_22 -0.00308 _diffrn_orient_matrix_UB_23 -0.03920 _diffrn_orient_matrix_UB_31 0.00429 _diffrn_orient_matrix_UB_32 -0.11872 _diffrn_orient_matrix_UB_33 0.00131 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 104 0.003 0.002 'International Tables' H 0 64 0.000 0.000 'International Tables' Se 0 8 -0.093 2.226 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Se(10) 0.30986(4) 0.2810(1) 0.600 0.038 Uij ? ? Se(10') 0.39508(4) 1.1759(1) 0.35041(7) 0.038 Uij ? ? C(1) 0.4486(4) 0.836(1) 0.5872(4) 0.035 Uij ? ? C(1') 0.4991(4) 0.609(1) 0.4327(4) 0.034 Uij ? ? C(2) 0.4940(4) 0.800(1) 0.6492(5) 0.043 Uij ? ? C(2') 0.5717(4) 0.639(1) 0.4104(5) 0.039 Uij ? ? C(3) 0.4881(4) 0.609(2) 0.6908(5) 0.047 Uij ? ? C(3') 0.5925(4) 0.829(1) 0.3719(4) 0.040 Uij ? ? C(4) 0.4349(4) 0.454(1) 0.6749(4) 0.037 Uij ? ? C(4') 0.5406(4) 0.991(1) 0.3538(5) 0.036 Uij ? ? C(4a) 0.3874(3) 0.488(1) 0.6154(4) 0.029 Uij ? ? C(4a') 0.4677(3) 0.962(1) 0.3737(4) 0.031 Uij ? ? C(5) 0.1680(4) 0.497(1) 0.5929(5) 0.038 Uij ? ? C(5') 0.2744(4) 0.984(1) 0.2656(4) 0.039 Uij ? ? C(6) 0.1193(4) 0.664(1) 0.5741(5) 0.047 Uij ? ? C(6') 0.2216(4) 0.823(1) 0.2505(5) 0.044 Uij ? ? C(7) 0.1416(4) 0.849(1) 0.5329(5) 0.043 Uij ? ? C(7') 0.2159(4) 0.634(1) 0.2954(5) 0.043 Uij ? ? C(8) 0.2143(3) 0.860(1) 0.5100(4) 0.034 Uij ? ? C(8') 0.2625(3) 0.606(1) 0.3552(5) 0.034 Uij ? ? C(8a) 0.2651(3) 0.691(1) 0.5267(4) 0.025 Uij ? ? C(8a') 0.3157(3) 0.770(1) 0.3724(4) 0.027 Uij ? ? C(9) 0.3438(3) 0.7078(10) 0.5058(4) 0.025 Uij ? ? C(9') 0.3665(3) 0.7444(9) 0.4365(4) 0.025 Uij ? ? C(9a) 0.3951(3) 0.678(1) 0.5707(4) 0.026 Uij ? ? C(9a') 0.4463(3) 0.769(1) 0.4149(4) 0.026 Uij ? ? C(10a) 0.2405(4) 0.510(1) 0.5698(4) 0.031 Uij ? ? C(10a') 0.3212(3) 0.955(1) 0.3261(4) 0.032 Uij ? ? H(1) 0.455 0.966 0.557 0.041 Uij ? ? H(1') 0.486 0.479 0.460 0.041 Uij ? ? H(2) 0.529 0.910 0.662 0.052 Uij ? ? H(2') 0.607 0.527 0.422 0.047 Uij ? ? H(3) 0.521 0.584 0.731 0.057 Uij ? ? H(3') 0.642 0.849 0.358 0.048 Uij ? ? H(4) 0.430 0.322 0.705 0.044 Uij ? ? H(4') 0.555 1.122 0.328 0.044 Uij ? ? H(5) 0.152 0.373 0.622 0.046 Uij ? ? H(5') 0.279 1.113 0.235 0.046 Uij ? ? H(6) 0.070 0.652 0.589 0.057 Uij ? ? H(6') 0.189 0.842 0.210 0.053 Uij ? ? H(7) 0.108 0.966 0.521 0.051 Uij ? ? H(7') 0.180 0.523 0.285 0.052 Uij ? ? H(8) 0.230 0.987 0.482 0.040 Uij ? ? H(8') 0.258 0.475 0.385 0.041 Uij ? ? 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 Se(10) 0.0403(3) 0.0376(3) 0.0353(4) -0.0034(3) 0.0003(4) 0.0099(4) Se(10') 0.0341(3) 0.0355(3) 0.0454(5) -0.0041(3) 0.0009(4) 0.0112(4) C(1) 0.034(3) 0.041(3) 0.028(4) -0.007(3) 0.005(3) -0.003(3) C(1') 0.035(3) 0.047(4) 0.020(4) 0.000(3) 0.000(3) 0.003(3) C(2) 0.026(3) 0.062(5) 0.042(5) -0.006(3) -0.003(3) -0.019(4) C(2') 0.028(3) 0.052(4) 0.036(5) 0.004(3) 0.003(3) -0.002(4) C(3) 0.044(4) 0.078(6) 0.020(4) 0.016(4) -0.004(3) -0.008(4) C(3') 0.024(3) 0.062(5) 0.033(5) -0.005(3) 0.009(3) 0.002(4) C(4) 0.037(4) 0.055(4) 0.019(4) 0.015(3) 0.000(3) 0.003(3) C(4') 0.031(3) 0.047(3) 0.031(4) -0.016(3) 0.002(4) 0.003(4) C(4a) 0.028(3) 0.047(4) 0.013(4) 0.003(2) 0.004(3) -0.003(3) C(4a') 0.029(3) 0.044(4) 0.019(4) -0.004(3) 0.003(3) 0.002(3) C(5) 0.034(3) 0.049(4) 0.031(5) -0.011(3) 0.009(4) 0.014(4) C(5') 0.047(4) 0.052(4) 0.017(4) 0.007(3) 0.001(3) 0.012(3) C(6) 0.027(4) 0.074(6) 0.041(5) 0.003(3) 0.004(3) 0.006(4) C(6') 0.034(4) 0.066(5) 0.033(4) -0.004(4) -0.014(3) 0.001(4) C(7) 0.033(4) 0.062(5) 0.033(4) 0.008(3) 0.000(3) 0.007(4) C(7') 0.039(4) 0.057(5) 0.033(5) -0.005(3) -0.009(4) 0.003(4) C(8) 0.031(3) 0.043(4) 0.026(4) -0.003(3) 0.003(3) 0.002(3) C(8') 0.029(3) 0.040(3) 0.034(4) -0.003(2) -0.001(4) 0.003(4) C(8a) 0.022(3) 0.036(3) 0.018(3) -0.004(2) 0.000(2) -0.002(3) C(8a') 0.023(3) 0.040(4) 0.017(4) -0.003(3) 0.003(2) -0.001(3) C(9) 0.023(3) 0.032(3) 0.021(3) -0.003(2) -0.001(3) 0.001(3) C(9') 0.032(3) 0.023(3) 0.022(3) 0.000(3) -0.002(3) 0.004(3) C(9a) 0.022(3) 0.032(3) 0.023(4) 0.009(2) 0.001(3) -0.001(3) C(9a') 0.022(3) 0.039(3) 0.016(3) 0.001(2) 0.000(3) 0.000(3) C(10a) 0.025(3) 0.045(4) 0.024(4) -0.005(3) 0.003(3) 0.005(3) C(10a') 0.036(3) 0.035(3) 0.024(4) -0.002(3) 0.001(3) 0.004(3) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment calculated _refine_ls_extinction_method none _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1885 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0350 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0430 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.500 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.41 _refine_diff_density_max -0.49 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se(10) C(4a) 1.893(6) ? ? yes Se(10) C(10a) 1.936(7) ? ? yes Se(10' C(4a') 1.884(7) ? ? yes Se(10' C(10a' 1.933(6) ? ? yes C(1) C(2) 1.41(1) ? ? yes C(1) C(9a) 1.385(9) ? ? yes C(1') C(2') 1.393(9) ? ? yes C(1') C(9a') 1.391(9) ? ? yes C(2) C(3) 1.37(1) ? ? yes C(2') C(3') 1.38(1) ? ? yes C(3) C(4) 1.37(1) ? ? yes C(3') C(4') 1.387(10) ? ? yes C(4) C(4a) 1.395(9) ? ? yes C(4') C(4a') 1.385(8) ? ? yes C(4a) C(9a) 1.396(10) ? ? yes C(4a') C(9a') 1.421(9) ? ? yes C(5) C(6) 1.37(1) ? ? yes C(5) C(10a) 1.388(9) ? ? yes C(5') C(6') 1.381(10) ? ? yes C(5') C(10a' 1.396(10) ? ? yes C(6) C(7) 1.39(1) ? ? yes C(6') C(7') 1.39(1) ? ? yes C(7) C(8) 1.389(9) ? ? yes C(7') C(8') 1.38(1) ? ? yes C(8) C(8a) 1.400(9) ? ? yes C(8') C(8a') 1.408(8) ? ? yes C(8a) C(9) 1.486(8) ? ? yes C(8a) C(10a) 1.401(9) ? ? yes C(8a') C(9') 1.490(9) ? ? yes C(8a') C(10a' 1.386(9) ? ? yes C(9) C(9') 1.338(9) ? ? yes C(9) C(9a) 1.510(9) ? ? yes C(9') C(9a') 1.512(8) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(4a) Se(10) C(10a) 94.1(3) ? ? ? yes C(4a') Se(10' C(10a' 94.6(3) ? ? ? yes C(2) C(1) C(9a) 118.8(6) ? ? ? yes C(2') C(1') C(9a') 120.2(7) ? ? ? yes C(1) C(2) C(3) 121.1(7) ? ? ? yes C(1') C(2') C(3') 120.6(7) ? ? ? yes C(2) C(3) C(4) 120.1(7) ? ? ? yes C(2') C(3') C(4') 119.9(6) ? ? ? yes C(3) C(4) C(4a) 120.1(7) ? ? ? yes C(3') C(4') C(4a') 120.4(7) ? ? ? yes Se(10) C(4a) C(4) 118.8(5) ? ? ? yes Se(10) C(4a) C(9a) 121.1(5) ? ? ? yes C(4) C(4a) C(9a) 120.1(6) ? ? ? yes Se(10' C(4a') C(4') 122.1(5) ? ? ? yes Se(10' C(4a') C(9a') 118.0(5) ? ? ? yes C(4') C(4a') C(9a') 119.9(6) ? ? ? yes C(6) C(5) C(10a) 120.1(6) ? ? ? yes C(6') C(5') C(10a' 119.6(7) ? ? ? yes C(5) C(6) C(7) 121.1(7) ? ? ? yes C(5') C(6') C(7') 119.7(7) ? ? ? yes C(6) C(7) C(8) 118.3(7) ? ? ? yes C(6') C(7') C(8') 120.3(7) ? ? ? yes C(7) C(8) C(8a) 122.2(6) ? ? ? yes C(7') C(8') C(8a') 120.9(7) ? ? ? yes C(8) C(8a) C(9) 122.2(6) ? ? ? yes C(8) C(8a) C(10a) 117.4(6) ? ? ? yes C(9) C(8a) C(10a) 120.1(5) ? ? ? yes C(8') C(8a') C(9') 122.0(6) ? ? ? yes C(8') C(8a') C(10a' 117.6(6) ? ? ? yes C(9') C(8a') C(10a' 120.4(6) ? ? ? yes C(8a) C(9) C(9') 123.2(6) ? ? ? yes C(8a) C(9) C(9a) 113.1(6) ? ? ? yes C(9') C(9) C(9a) 123.7(5) ? ? ? yes C(8a') C(9') C(9) 123.5(6) ? ? ? yes C(8a') C(9') C(9a') 112.7(5) ? ? ? yes C(9) C(9') C(9a') 123.7(6) ? ? ? yes C(1) C(9a) C(4a) 119.7(7) ? ? ? yes C(1) C(9a) C(9) 121.5(6) ? ? ? yes C(4a) C(9a) C(9) 118.8(6) ? ? ? yes C(1') C(9a') C(4a') 118.9(6) ? ? ? yes C(1') C(9a') C(9') 122.5(6) ? ? ? yes C(4a') C(9a') C(9') 118.6(5) ? ? ? yes Se(10) C(10a) C(5) 119.9(5) ? ? ? yes Se(10) C(10a) C(8a) 119.2(5) ? ? ? yes C(5) C(10a) C(8a) 120.9(6) ? ? ? yes Se(10' C(10a' C(5') 121.3(5) ? ? ? yes Se(10' C(10a' C(8a') 116.9(5) ? ? ? yes C(5') C(10a' C(8a') 121.8(6) ? ? ? yes #----------------------------------------------------------------------- #===END data_8 #----------------------------------------------------------------------- _audit_creation_date 'Mon Oct 25 16:05:45 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'Philips Diffractometer Control' _computing_cell_refinement 'Philips Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 8.967(1) _cell_length_b 15.968(3) _cell_length_c 7.526(1) _cell_angle_alpha 97.20(1) _cell_angle_beta 102.59(1) _cell_angle_gamma 84.91(1) _cell_volume 1041.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 12.0 _cell_measurement_theta_max 15.0 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.861 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 583.61 _chemical_formula_moiety 'C 26 H 16 Te 2' _chemical_compound_source ? _exptl_crystal_F_000 552.00 _exptl_absorpt_coefficient_mu 2.810 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.263 _exptl_absorpt_correction_T_min 0.655 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'Philips PW1100/20' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -6 2 2 0 -10 1 -1 0 5 _diffrn_reflns_number 3660 _reflns_number_total 3660 _reflns_number_observed 3050 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 25.00 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.08130 _diffrn_orient_matrix_UB_12 0.00104 _diffrn_orient_matrix_UB_13 -0.01940 _diffrn_orient_matrix_UB_21 0.00347 _diffrn_orient_matrix_UB_22 -0.04355 _diffrn_orient_matrix_UB_23 0.01269 _diffrn_orient_matrix_UB_31 0.00039 _diffrn_orient_matrix_UB_32 0.01110 _diffrn_orient_matrix_UB_33 0.09454 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 52 0.003 0.002 'International Tables' H 0 32 0.000 0.000 'International Tables' Te 0 4 -0.531 1.675 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Te(10) 0.81123(4) 0.13573(2) 0.25102(6) 0.059 Uij ? ? Te(10") 0.85284(4) 0.37145(2) 0.68011(6) 0.060 Uij ? ? C(1) 0.3828(6) 0.0463(3) 0.3083(7) 0.045 Uij ? ? C(1") 0.6841(6) 0.6336(3) 0.6360(7) 0.047 Uij ? ? C(2) 0.3458(6) 0.0973(4) 0.4591(7) 0.051 Uij ? ? C(2") 0.8129(8) 0.6781(4) 0.6863(8) 0.061 Uij ? ? C(3) 0.4387(8) 0.1608(4) 0.5453(8) 0.061 Uij ? ? C(3") 0.9548(8) 0.6364(4) 0.7337(9) 0.069 Uij ? ? C(4) 0.5675(7) 0.1728(3) 0.4878(7) 0.056 Uij ? ? C(4") 0.9665(7) 0.5499(5) 0.7306(9) 0.067 Uij ? ? C(4a) 0.6079(6) 0.1208(3) 0.3386(7) 0.044 Uij ? ? C(4a") 0.8380(6) 0.5046(3) 0.6816(7) 0.046 Uij ? ? C(5) 0.9793(6) -0.0397(4) 0.2178(8) 0.062 Uij ? ? C(5") 0.6286(7) 0.3281(3) 0.9086(7) 0.056 Uij ? ? C(6) 0.9946(7) -0.1256(5) 0.1810(9) 0.073 Uij ? ? C(6") 0.4978(9) 0.3366(4) 0.9734(8) 0.066 Uij ? ? C(7) 0.8657(8) -0.1718(4) 0.1116(8) 0.063 Uij ? ? C(7") 0.3818(8) 0.3976(4) 0.9149(8) 0.063 Uij ? ? C(8) 0.7221(7) -0.1275(4) 0.0772(7) 0.052 Uij ? ? C(8") 0.4015(6) 0.4492(4) 0.7885(7) 0.049 Uij ? ? C(8a) 0.7051(5) -0.0408(3) 0.1110(6) 0.039 Uij ? ? C(8a") 0.5337(5) 0.4409(3) 0.7168(6) 0.040 Uij ? ? C(9) 0.5509(5) 0.0041(3) 0.0802(6) 0.038 Uij ? ? C(9") 0.5521(5) 0.4969(3) 0.5796(6) 0.039 Uij ? ? C(9a) 0.5115(5) 0.0581(3) 0.2442(6) 0.040 Uij ? ? C(9a") 0.6935(6) 0.5446(3) 0.6297(6) 0.039 Uij ? ? C(10a) 0.8359(6) 0.0031(4) 0.1861(7) 0.050 Uij ? ? C(10a") 0.6490(6) 0.3809(3) 0.7827(7) 0.049 Uij ? ? H(1) 0.318 0.003 0.249 0.054 Uij ? ? H(1") 0.587 0.663 0.605 0.057 Uij ? ? H(2) 0.257 0.088 0.502 0.061 Uij ? ? H(2") 0.805 0.738 0.689 0.073 Uij ? ? H(3) 0.412 0.197 0.646 0.073 Uij ? ? H(3") 1.044 0.667 0.768 0.083 Uij ? ? H(4) 0.631 0.217 0.549 0.067 Uij ? ? H(4") 1.064 0.521 0.763 0.080 Uij ? ? H(5) 1.068 -0.009 0.266 0.075 Uij ? ? H(5") 0.706 0.286 0.949 0.068 Uij ? ? H(6) 1.094 -0.154 0.203 0.087 Uij ? ? H(6") 0.485 0.301 1.060 0.079 Uij ? ? H(7) 0.875 -0.232 0.088 0.076 Uij ? ? H(7") 0.291 0.404 0.961 0.076 Uij ? ? H(8) 0.634 -0.158 0.029 0.063 Uij ? ? H(8") 0.323 0.491 0.750 0.059 Uij ? ? 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 Te(10) 0.0556(3) 0.0564(3) 0.0671(3) -0.0190(2) 0.0119(2) 0.0063(2) Te(10") 0.0518(3) 0.0544(3) 0.0743(3) 0.0103(2) 0.0145(2) 0.0111(2) C(1) 0.047(3) 0.048(3) 0.041(3) -0.001(2) 0.010(2) 0.007(2) C(1") 0.056(3) 0.047(3) 0.036(3) -0.004(2) 0.004(2) -0.001(2) C(2) 0.056(3) 0.060(3) 0.036(3) -0.001(2) 0.010(2) 0.008(2) C(2") 0.079(4) 0.052(3) 0.052(3) -0.023(3) 0.009(3) 0.007(3) C(3) 0.075(4) 0.062(4) 0.041(3) 0.007(3) 0.016(3) -0.005(3) C(3") 0.065(4) 0.072(4) 0.070(4) -0.034(3) 0.007(3) 0.000(3) C(4) 0.073(4) 0.048(3) 0.044(3) -0.014(3) 0.013(3) -0.008(2) C(4") 0.043(3) 0.094(5) 0.060(4) -0.010(3) 0.006(3) 0.005(3) C(4a) 0.052(3) 0.044(3) 0.037(3) -0.007(2) 0.008(2) 0.005(2) C(4a") 0.042(3) 0.050(3) 0.046(3) 0.001(2) 0.010(2) 0.002(2) C(5) 0.035(3) 0.089(5) 0.059(4) 0.004(3) 0.005(2) 0.006(3) C(5") 0.076(4) 0.050(3) 0.040(3) -0.006(3) 0.002(3) 0.007(2) C(6) 0.057(4) 0.086(5) 0.068(4) 0.030(3) 0.009(3) 0.016(3) C(6") 0.101(5) 0.060(4) 0.039(3) -0.026(3) 0.010(3) 0.008(3) C(7) 0.068(4) 0.066(4) 0.050(3) 0.020(3) 0.013(3) 0.005(3) C(7") 0.077(4) 0.077(4) 0.042(3) -0.029(3) 0.020(3) -0.003(3) C(8) 0.055(3) 0.059(3) 0.038(3) -0.002(2) 0.004(2) 0.003(2) C(8") 0.047(3) 0.065(3) 0.035(3) -0.013(2) 0.007(2) 0.001(2) C(8a) 0.038(2) 0.052(3) 0.028(2) -0.006(2) 0.007(2) 0.001(2) C(8a") 0.040(2) 0.044(3) 0.035(2) -0.007(2) 0.003(2) 0.006(2) C(9) 0.038(2) 0.038(2) 0.039(2) -0.007(2) 0.009(2) 0.002(2) C(9") 0.039(2) 0.044(3) 0.036(2) 0.001(2) 0.008(2) 0.006(2) C(9a) 0.044(3) 0.042(2) 0.031(2) 0.002(2) 0.004(2) 0.007(2) C(9a") 0.046(3) 0.042(3) 0.032(2) -0.005(2) 0.010(2) 0.004(2) C(10a) 0.042(3) 0.064(3) 0.044(3) -0.002(2) 0.007(2) 0.012(2) C(10a") 0.060(3) 0.043(3) 0.040(3) -0.004(2) 0.004(2) 0.006(2) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment calculated _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 14.07300 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3050 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0300 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0510 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.910 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.60 _refine_diff_density_max -0.43 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Te(10) C(4a) 2.111(5) ? ? yes Te(10) C(10a) 2.116(6) ? ? yes Te(10" C(4a") 2.118(5) ? ? yes Te(10" C(10a" 2.121(6) ? ? yes C(1) C(2) 1.394(7) ? ? yes C(1) C(9a) 1.380(7) ? ? yes C(1") C(2") 1.367(8) ? ? yes C(1") C(9a") 1.412(7) ? ? yes C(2) C(3) 1.376(8) ? ? yes C(2") C(3") 1.378(10) ? ? yes C(3) C(4) 1.355(8) ? ? yes C(3") C(4") 1.373(9) ? ? yes C(4) C(4a) 1.405(7) ? ? yes C(4") C(4a") 1.372(8) ? ? yes C(4a) C(9a) 1.401(7) ? ? yes C(4a") C(9a") 1.390(7) ? ? yes C(5) C(6) 1.365(9) ? ? yes C(5) C(10a) 1.389(7) ? ? yes C(5") C(6") 1.356(9) ? ? yes C(5") C(10a" 1.393(7) ? ? yes C(6) C(7) 1.394(10) ? ? yes C(6") C(7") 1.397(10) ? ? yes C(7) C(8) 1.401(8) ? ? yes C(7") C(8") 1.382(8) ? ? yes C(8) C(8a) 1.377(7) ? ? yes C(8") C(8a") 1.395(7) ? ? yes C(8a) C(9) 1.485(6) ? ? yes C(8a) C(10a) 1.395(7) ? ? yes C(8a") C(9") 1.492(6) ? ? yes C(8a") C(10a" 1.397(7) ? ? yes C(9) C(9) 1.345(9) 1_555 2_655 yes C(9) C(9a) 1.503(7) ? ? yes C(9") C(9") 1.358(9) 1_555 2_666 yes C(9") C(9a") 1.490(7) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(4a) Te(10) C(10a) 89.3(2) ? ? ? yes C(4a") Te(10" C(10a" 89.4(2) ? ? ? yes C(2) C(1) C(9a) 121.3(5) ? ? ? yes C(2") C(1") C(9a") 121.0(5) ? ? ? yes C(1) C(2) C(3) 119.5(5) ? ? ? yes C(1") C(2") C(3") 120.2(5) ? ? ? yes C(2) C(3) C(4) 120.6(5) ? ? ? yes C(2") C(3") C(4") 119.8(5) ? ? ? yes C(3) C(4) C(4a) 120.5(5) ? ? ? yes C(3") C(4") C(4a") 120.5(6) ? ? ? yes Te(10) C(4a) C(4) 121.3(4) ? ? ? yes Te(10) C(4a) C(9a) 118.9(4) ? ? ? yes C(4) C(4a) C(9a) 119.8(5) ? ? ? yes Te(10" C(4a") C(4") 121.2(4) ? ? ? yes Te(10" C(4a") C(9a") 117.7(4) ? ? ? yes C(4") C(4a") C(9a") 121.1(5) ? ? ? yes C(6) C(5) C(10a) 120.8(6) ? ? ? yes C(6") C(5") C(10a" 120.0(6) ? ? ? yes C(5) C(6) C(7) 120.3(5) ? ? ? yes C(5") C(6") C(7") 120.7(5) ? ? ? yes C(6) C(7) C(8) 118.2(6) ? ? ? yes C(6") C(7") C(8") 119.1(6) ? ? ? yes C(7) C(8) C(8a) 122.2(5) ? ? ? yes C(7") C(8") C(8a") 121.3(5) ? ? ? yes C(8) C(8a) C(9) 121.0(4) ? ? ? yes C(8) C(8a) C(10a) 118.1(5) ? ? ? yes C(9) C(8a) C(10a) 120.8(4) ? ? ? yes C(8") C(8a") C(9") 120.5(4) ? ? ? yes C(8") C(8a") C(10a" 117.8(5) ? ? ? yes C(9") C(8a") C(10a" 121.7(4) ? ? ? yes C(8a) C(9) C(9) 123.4(5) 1_555 1_555 2_655 yes C(8a) C(9) C(9a) 115.5(4) ? ? ? yes C(9) C(9) C(9a) 121.0(5) 2_655 1_555 1_555 yes C(8a") C(9") C(9") 122.2(6) 1_555 1_555 2_666 yes C(8a") C(9") C(9a") 115.1(4) ? ? ? yes C(9") C(9") C(9a") 122.7(5) 2_666 1_555 1_555 yes C(1) C(9a) C(4a) 118.3(5) ? ? ? yes C(1) C(9a) C(9) 121.5(4) ? ? ? yes C(4a) C(9a) C(9) 120.2(4) ? ? ? yes C(1") C(9a") C(4a") 117.3(5) ? ? ? yes C(1") C(9a") C(9") 120.6(4) ? ? ? yes C(4a") C(9a") C(9") 122.0(4) ? ? ? yes Te(10) C(10a) C(5) 120.9(4) ? ? ? yes Te(10) C(10a) C(8a) 118.7(4) ? ? ? yes C(5) C(10a) C(8a) 120.4(5) ? ? ? yes Te(10" C(10a" C(5") 121.5(4) ? ? ? yes Te(10" C(10a" C(8a") 117.7(4) ? ? ? yes C(5") C(10a" C(8a") 120.8(5) ? ? ? yes #----------------------------------------------------------------------- #===END data_9 #----------------------------------------------------------------------- _audit_creation_date 'Mon Oct 25 16:39:37 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'CAD4 Diffractometer Control' _computing_cell_refinement 'CAD4 Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 8.767(5) _cell_length_b 6.241(3) _cell_length_c 18.042(8) _cell_angle_alpha 90 _cell_angle_beta 95.71(4) _cell_angle_gamma 90 _cell_volume 982.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 23.0 _cell_measurement_theta_max 31.0 #----------------------------------------------------------------------- _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y,1/2-z' ' -x, -y, -z' ' +x,1/2-y,1/2+z' #----------------------------------------------------------------------- _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.651 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 244.17 _chemical_formula_moiety 'C 26 H 18 Se 2' _chemical_compound_source ? _exptl_crystal_F_000 484.00 _exptl_absorpt_coefficient_mu 4.750 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.376 _exptl_absorpt_correction_T_min 0.760 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% -1.08 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 2 3 -1 -3 3 0 1 -9 _diffrn_reflns_number 2055 _reflns_number_total 2055 _reflns_number_observed 1614 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 69.90 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.11429 _diffrn_orient_matrix_UB_12 -0.00637 _diffrn_orient_matrix_UB_13 -0.00910 _diffrn_orient_matrix_UB_21 -0.00326 _diffrn_orient_matrix_UB_22 -0.09339 _diffrn_orient_matrix_UB_23 0.04485 _diffrn_orient_matrix_UB_31 -0.00813 _diffrn_orient_matrix_UB_32 0.13004 _diffrn_orient_matrix_UB_33 0.03175 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 52 0.018 0.009 'International Tables' H 0 36 0.000 0.000 'International Tables' Se 0 4 -0.794 1.137 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Se(10) 0.25532(5) 0.88936(7) 0.44931(3) 0.061 Uij ? ? C(1) 0.4122(5) 0.3427(8) 0.3505(2) 0.058 Uij ? ? C(2) 0.3716(6) 0.3793(9) 0.2757(3) 0.066 Uij ? ? C(3) 0.3009(6) 0.5655(10) 0.2524(3) 0.069 Uij ? ? C(4) 0.2675(6) 0.7172(9) 0.3037(2) 0.065 Uij ? ? C(4a) 0.3076(5) 0.6819(7) 0.3790(2) 0.051 Uij ? ? C(5) 0.0937(5) 0.7284(9) 0.5666(2) 0.062 Uij ? ? C(6) 0.0549(6) 0.5819(9) 0.6186(3) 0.068 Uij ? ? C(7) 0.1351(6) 0.3905(9) 0.6266(3) 0.064 Uij ? ? C(8) 0.2538(5) 0.3513(8) 0.5833(3) 0.058 Uij ? ? C(8a) 0.2951(4) 0.4964(7) 0.5317(2) 0.050 Uij ? ? C(9) 0.4249(4) 0.4508(8) 0.4853(2) 0.055 Uij ? ? C(9a) 0.3814(4) 0.4941(7) 0.4032(2) 0.048 Uij ? ? C(10a) 0.2116(5) 0.6856(8) 0.5232(2) 0.052 Uij ? ? H(1) 0.462(5) 0.218(7) 0.373(2) 0.041(10) Uij ? ? H(2) 0.409(7) 0.277(10) 0.244(3) 0.08(2) Uij ? ? H(3) 0.279(7) 0.607(7) 0.190(3) 0.08(2) Uij ? ? H(4) 0.219(6) 0.871(7) 0.288(3) 0.06(1) Uij ? ? H(5) 0.032(5) 0.869(6) 0.560(2) 0.05(1) Uij ? ? H(6) -0.025(7) 0.617(7) 0.652(3) 0.07(2) Uij ? ? H(7) 0.090(6) 0.294(9) 0.658(3) 0.06(1) Uij ? ? H(8) 0.317(6) 0.219(8) 0.591(3) 0.06(1) Uij ? ? H(9) 0.456(6) 0.270(8) 0.490(3) 0.07(1) Uij ? ? 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 Se(10) 0.0621(4) 0.0590(4) 0.0617(4) 0.0022(2) 0.0065(2) 0.0000(2) C(1) 0.052(2) 0.073(3) 0.048(2) 0.002(2) 0.000(2) -0.001(2) C(2) 0.062(3) 0.092(4) 0.043(2) -0.004(2) 0.004(2) -0.012(2) C(3) 0.064(3) 0.099(3) 0.042(2) -0.002(3) -0.001(2) 0.006(2) C(4) 0.061(3) 0.081(3) 0.051(3) -0.006(2) 0.001(2) 0.012(2) C(4a) 0.044(2) 0.064(2) 0.043(2) -0.004(2) 0.001(2) 0.002(2) C(5) 0.047(2) 0.085(3) 0.053(2) 0.005(2) 0.002(2) -0.008(2) C(6) 0.052(2) 0.096(4) 0.055(3) -0.005(2) 0.009(2) -0.010(2) C(7) 0.055(3) 0.089(4) 0.050(3) -0.005(2) 0.008(2) 0.004(2) C(8) 0.050(2) 0.078(3) 0.045(2) 0.000(2) 0.001(2) 0.003(2) C(8a) 0.041(2) 0.067(2) 0.041(2) -0.001(2) -0.003(1) -0.002(2) C(9) 0.042(2) 0.084(3) 0.038(2) 0.004(2) 0.001(2) 0.002(2) C(9a) 0.037(2) 0.067(2) 0.040(2) -0.001(2) 0.000(1) 0.002(2) C(10a) 0.046(2) 0.067(2) 0.044(2) -0.004(2) 0.001(2) -0.004(2) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 7.80593 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1614 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0510 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0740 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.590 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.56 _refine_diff_density_max -0.74 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se(10) C(4a) 1.900(4) ? ? yes Se(10) C(10a) 1.909(4) ? ? yes C(1) C(2) 1.380(6) ? ? yes C(1) C(9a) 1.386(6) ? ? yes C(2) C(3) 1.363(7) ? ? yes C(3) C(4) 1.375(8) ? ? yes C(4) C(4a) 1.386(6) ? ? yes C(4a) C(9a) 1.388(6) ? ? yes C(5) C(6) 1.377(7) ? ? yes C(5) C(10a) 1.383(6) ? ? yes C(6) C(7) 1.387(8) ? ? yes C(7) C(8) 1.383(7) ? ? yes C(8) C(8a) 1.373(7) ? ? yes C(8a) C(9) 1.506(6) ? ? yes C(8a) C(10a) 1.389(6) ? ? yes C(9) C(9) 1.501(8) 1_555 3_666 yes C(9) C(9a) 1.516(5) ? ? yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(4a) Se(10) C(10a) 95.2(2) ? ? ? yes C(2) C(1) C(9a) 120.6(5) ? ? ? yes C(1) C(2) C(3) 120.4(5) ? ? ? yes C(2) C(3) C(4) 120.1(4) ? ? ? yes C(3) C(4) C(4a) 120.0(5) ? ? ? yes Se(10) C(4a) C(4) 119.4(4) ? ? ? yes Se(10) C(4a) C(9a) 120.1(3) ? ? ? yes C(4) C(4a) C(9a) 120.5(4) ? ? ? yes C(6) C(5) C(10a) 120.4(5) ? ? ? yes C(5) C(6) C(7) 119.0(5) ? ? ? yes C(6) C(7) C(8) 119.7(5) ? ? ? yes C(7) C(8) C(8a) 122.0(5) ? ? ? yes C(8) C(8a) C(9) 121.2(4) ? ? ? yes C(8) C(8a) C(10a) 117.6(4) ? ? ? yes C(9) C(8a) C(10a) 121.2(4) ? ? ? yes C(8a) C(9) C(9) 114.2(5) 1_555 1_555 3_666 yes C(8a) C(9) C(9a) 112.2(3) ? ? ? yes C(9) C(9) C(9a) 113.6(5) 3_666 1_555 1_555 yes C(1) C(9a) C(4a) 118.4(4) ? ? ? yes C(1) C(9a) C(9) 120.1(4) ? ? ? yes C(4a) C(9a) C(9) 121.5(4) ? ? ? yes Se(10) C(10a) C(5) 118.7(4) ? ? ? yes Se(10) C(10a) C(8a) 120.2(3) ? ? ? yes C(5) C(10a) C(8a) 121.2(4) ? ? ? yes #----------------------------------------------------------------------- #===END data_20 #----------------------------------------------------------------------- _audit_creation_date 'Thu Jul 15 14:13:10 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'CAD4 Diffractometer Control' _computing_cell_refinement 'CAD4 Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #----------------------------------------------------------------------- _cell_length_a 11.535(5) _cell_length_b 14.111(4) _cell_length_c 6.9294(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1127.9(4) _cell_formula_units_Z 8 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 25.0 _cell_measurement_theta_max 30.0 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C m c 21 ' _symmetry_Int_Tables_number 36 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2+x,1/2+y, +z' ' -x, +y, +z' '1/2-x,1/2+y, +z' ' -x, -y,1/2+z' '1/2-x,1/2-y,1/2+z' ' +x, -y,1/2+z' '1/2+x,1/2-y,1/2+z' #----------------------------------------------------------------------- _exptl_crystal_description 'unknown' _exptl_crystal_colour 'unknown' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 257.19 _chemical_formula_moiety 'C 14 H 10 Se' _chemical_compound_source ? _exptl_crystal_F_000 512.00 _exptl_absorpt_coefficient_mu 4.169 _exptl_absorpt_correction_type refdelf _exptl_absorpt_process_details Walker&Stuart_DIFABS _exptl_absorpt_correction_T_max 1.567 _exptl_absorpt_correction_T_min 0.663 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 293.2 _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector scintillation _diffrn_measurement_device 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% -2.92 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 -7 1 _diffrn_reflns_number 1042 _reflns_number_total 732 _reflns_number_observed 590 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 0.056 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.0 _diffrn_reflns_theta_max 69.93 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.01343 _diffrn_orient_matrix_UB_12 -0.06644 _diffrn_orient_matrix_UB_13 0.04491 _diffrn_orient_matrix_UB_21 -0.08527 _diffrn_orient_matrix_UB_22 0.00832 _diffrn_orient_matrix_UB_23 -0.01986 _diffrn_orient_matrix_UB_31 0.00799 _diffrn_orient_matrix_UB_32 -0.02320 _diffrn_orient_matrix_UB_33 -0.13569 #----------------------------------------------------------------------- loop_ _atom_type_symbol _atom_type_oxidation_number _atom_type_number_in_cell _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C 0 56 0.018 0.009 'International Tables' H 0 40 0.000 0.000 'International Tables' Se 0 4 -0.794 1.137 'International Tables' #----------------------------------------------------------------------- loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag _atom_site_calc_attached_atom Se(10) 0.000 0.76303(5) 0.600 0.064 Uij ? ? C(1) -0.2055(5) 0.5674(4) 0.309(1) 0.060 Uij ? ? C(2) -0.3106(5) 0.5767(5) 0.406(2) 0.073 Uij ? ? C(3) -0.3219(4) 0.6373(5) 0.549(1) 0.074 Uij ? ? C(4) -0.2284(5) 0.6907(4) 0.619(1) 0.061 Uij ? ? C(4a) -0.1225(4) 0.6837(3) 0.515(1) 0.051 Uij ? ? C(9) 0.000 0.6191(5) 0.251(2) 0.053 Uij ? ? C(9') 0.000 0.5994(8) 0.058(2) 0.076 Uij ? ? C(9a) -0.1100(4) 0.6228(3) 0.3624(9) 0.047 Uij ? ? H(1) -0.199 0.523 0.206 0.072 Uij ? ? H(2) -0.375 0.539 0.369 0.087 Uij ? ? H(3) -0.396 0.645 0.606 0.089 Uij ? ? H(4) -0.236 0.729 0.731 0.074 Uij ? ? H(9') -0.071 0.597 -0.011 0.091 Uij ? ? 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 Se(10) 0.0606(5) 0.0634(6) 0.0671(7) 0.000 0.000 -0.0186(7) C(1) 0.049(2) 0.062(3) 0.071(5) 0.000(2) -0.013(3) -0.001(3) C(2) 0.051(3) 0.075(3) 0.092(6) -0.007(3) -0.018(4) 0.012(4) C(3) 0.041(2) 0.087(4) 0.094(8) 0.011(2) 0.010(3) 0.014(4) C(4) 0.056(2) 0.073(3) 0.056(5) 0.020(2) 0.000(3) -0.006(4) C(4a) 0.046(2) 0.054(2) 0.052(3) 0.005(2) -0.008(3) -0.007(2) C(9) 0.056(4) 0.044(3) 0.059(6) 0.000 0.000 -0.015(4) C(9') 0.066(5) 0.092(6) 0.069(10) 0.000 0.000 0.033(6) C(9a) 0.050(2) 0.050(2) 0.042(3) 0.004(2) -0.008(2) 0.000(2) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment calculated _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 6.02567 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 590 _refine_ls_number_parameters 73 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0450 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0540 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.750 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.71 _refine_diff_density_max -1.00 #----------------------------------------------------------------------- _geom_special_details ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se(10) C(4a) 1.896(5) ? ? yes Se(10) C(4a) 1.896(5) 1 3 yes C(1) C(2) 1.39(1) ? ? yes C(1) C(9a) 1.400(7) ? ? yes C(2) C(3) 1.31(1) ? ? yes C(3) C(4) 1.403(10) ? ? yes C(4) C(4a) 1.423(9) ? ? yes C(4a) C(9a) 1.371(9) ? ? yes C(9) C(9') 1.37(2) ? ? yes C(9) C(9a) 1.485(7) ? ? yes C(9) C(9a) 1.485(7) 1 3 yes #----------------------------------------------------------------------- loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(4a) Se(10) C(4a) 96.3(3) 1 1 3 yes C(2) C(1) C(9a) 120.2(6) ? ? ? yes C(1) C(2) C(3) 120.8(6) ? ? ? yes C(2) C(3) C(4) 122.3(6) ? ? ? yes C(3) C(4) C(4a) 116.5(8) ? ? ? yes Se(10) C(4a) C(4) 116.2(5) ? ? ? yes Se(10) C(4a) C(9a) 122.1(4) ? ? ? yes C(4) C(4a) C(9a) 121.7(5) ? ? ? yes C(9') C(9) C(9a) 121.0(4) ? ? ? yes C(9') C(9) C(9a) 121.0(4) 1 1 3 yes C(9a) C(9) C(9a) 117.4(8) 1 1 3 yes C(1) C(9a) C(4a) 118.1(5) ? ? ? yes C(1) C(9a) C(9) 121.1(5) ? ? ? yes C(4a) C(9a) C(9) 120.8(5) ? ? ? yes #----------------------------------------------------------------------- #===END