# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 188/192 data_[D75]_R.S._P21/c #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 28 09:13:31 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 9.6580 _cell_length_b 15.3750 _cell_length_c 9.9750 _cell_angle_alpha 90 _cell_angle_beta 103 _cell_angle_gamma 90 _cell_volume 1438.5699 _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 24 _cell_measurement_theta_min 11.0 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _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 1.133 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 245.34 _chemical_formula_moiety '1/2(C31H28*C6H6)' _chemical_compound_source 'Rachel Suissa' _exptl_crystal_F_000 524.00 _exptl_absorpt_coefficient_mu 0.064 #------------------------------------------------------------------------------ _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 'CAD4' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% -0.36 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -4 9 2 -5 4 2 1 1 6 _diffrn_reflns_number 2782 _reflns_number_total 2782 _reflns_number_observed 1826 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 1.83 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 24.96 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.02518 _diffrn_orient_matrix_UB_12 -0.05673 _diffrn_orient_matrix_UB_13 -0.04889 _diffrn_orient_matrix_UB_21 -0.01721 _diffrn_orient_matrix_UB_22 0.03066 _diffrn_orient_matrix_UB_23 -0.09102 _diffrn_orient_matrix_UB_31 0.10223 _diffrn_orient_matrix_UB_32 -0.00881 _diffrn_orient_matrix_UB_33 -0.00164 #------------------------------------------------------------------------------ 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 76 0.003 0.002 'International Tables' H 0 68 0.000 0.000 '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 C(1) 0.7597(2) 0.55678(10) 0.4594(2) 0.0467 Uij ? ? C(2) 0.8841(2) 0.6039(1) 0.4743(2) 0.0560 Uij ? ? C(3) 0.8992(2) 0.6818(1) 0.5427(2) 0.0610 Uij ? ? C(4) 0.7898(2) 0.7143(1) 0.5952(2) 0.0549 Uij ? ? C(4a) 0.6622(1) 0.66888(10) 0.5804(1) 0.0422 Uij ? ? C(5) 0.2929(2) 0.7467(1) 0.4745(2) 0.0523 Uij ? ? C(6) 0.1792(2) 0.7298(1) 0.3646(2) 0.0589 Uij ? ? C(7) 0.1714(2) 0.6525(1) 0.2941(2) 0.0544 Uij ? ? C(8) 0.2760(2) 0.59094(10) 0.3359(2) 0.0453 Uij ? ? C(8a) 0.3898(1) 0.60638(9) 0.4477(1) 0.0382 Uij ? ? C(9) 0.5088(1) 0.54293(8) 0.4915(1) 0.0370 Uij ? ? C(9a) 0.6487(1) 0.58820(9) 0.5135(1) 0.0382 Uij ? ? C(10) 0.5349(2) 0.7029(1) 0.6318(2) 0.0474 Uij ? ? C(10a) 0.4018(1) 0.68640(9) 0.5161(1) 0.0410 Uij ? ? C(11) 0.5514(2) 0.7989(1) 0.6715(2) 0.0706 Uij ? ? C(12) 0.5232(2) 0.6510(1) 0.7614(2) 0.0669 Uij ? ? C(13) 0.9328(4) 0.5638(2) -0.0850(4) 0.1164 Uij ? ? C(14) 0.9429(4) 0.4682(2) 0.1028(3) 0.1183 Uij ? ? C(15) 0.8748(3) 0.5328(2) 0.0163(4) 0.1182 Uij ? ? H(1) 0.7497 0.5025 0.4123 0.0560 Uij ? ? H(2) 0.9590 0.5823 0.4366 0.0669 Uij ? ? H(3) 0.9856 0.7136 0.5543 0.0735 Uij ? ? H(4) 0.8018 0.7685 0.6422 0.0655 Uij ? ? H(5) 0.2967 0.8004 0.5227 0.0623 Uij ? ? H(6) 0.1058 0.7719 0.3375 0.0704 Uij ? ? H(7) 0.0940 0.6418 0.2167 0.0653 Uij ? ? H(8) 0.2702 0.5373 0.2874 0.0541 Uij ? ? H(15) 0.8855 0.6086 -0.1442 0.1375 Uij ? ? H(16) 0.9035 0.4462 0.1740 0.1410 Uij ? ? H(17) 0.7872 0.5555 0.0277 0.1409 Uij ? ? H(111) 0.6351 0.8066 0.7430 0.0831 Uij ? ? H(112) 0.5589 0.8323 0.5932 0.0831 Uij ? ? H(113) 0.4707 0.8176 0.7025 0.0831 Uij ? ? H(121) 0.4434 0.6712 0.7928 0.0790 Uij ? ? H(122) 0.5113 0.5910 0.7390 0.0790 Uij ? ? H(123) 0.6076 0.6589 0.8321 0.0790 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 C(1) 0.0417(9) 0.0466(9) 0.0548(10) 0.0027(7) 0.0172(7) 0.0041(8) C(2) 0.0393(9) 0.062(1) 0.072(1) 0.0028(8) 0.0233(8) 0.0096(9) C(3) 0.0393(9) 0.067(1) 0.077(1) -0.0117(9) 0.0135(9) 0.0039(10) C(4) 0.0481(10) 0.054(1) 0.059(1) -0.0092(8) 0.0069(8) -0.0057(8) C(4a) 0.0373(8) 0.0489(9) 0.0388(8) -0.0013(7) 0.0062(6) 0.0002(7) C(5) 0.0476(10) 0.0508(10) 0.062(1) 0.0062(8) 0.0211(8) 0.0005(8) C(6) 0.0394(9) 0.062(1) 0.075(1) 0.0124(8) 0.0131(9) 0.0153(10) C(7) 0.0371(9) 0.062(1) 0.059(1) -0.0011(8) 0.0020(7) 0.0121(9) C(8) 0.0385(8) 0.0491(9) 0.0469(9) -0.0032(7) 0.0075(7) 0.0030(7) C(8a) 0.0328(8) 0.0441(9) 0.0397(8) 0.0001(7) 0.0123(6) 0.0041(7) C(9) 0.0336(7) 0.0444(8) 0.0341(8) 0.0008(7) 0.0103(6) -0.0015(7) C(9a) 0.0331(8) 0.0444(9) 0.0369(8) 0.0008(7) 0.0078(6) 0.0040(7) C(10) 0.0473(9) 0.0528(10) 0.0432(9) 0.0011(8) 0.0127(7) -0.0084(7) C(10a) 0.0384(8) 0.0459(9) 0.0418(9) 0.0019(7) 0.0157(7) 0.0008(7) C(11) 0.066(1) 0.071(1) 0.073(1) 0.0006(10) 0.0136(10) -0.029(1) C(12) 0.063(1) 0.096(1) 0.0434(10) 0.007(1) 0.0168(8) -0.0048(9) C(13) 0.122(3) 0.068(2) 0.121(2) -0.010(2) -0.047(2) 0.013(2) C(14) 0.141(3) 0.087(2) 0.109(2) -0.023(2) -0.005(2) -0.004(2) C(15) 0.102(2) 0.075(2) 0.157(3) -0.003(2) -0.011(2) -0.013(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 80.81068 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1826 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0340 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0360 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.410 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.12 _refine_diff_density_max -0.11 #------------------------------------------------------------------------------ _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 C(1) C(2) 1.380(2) ? ? yes C(1) C(9a) 1.396(2) ? ? yes C(2) C(3) 1.369(2) ? ? yes C(3) C(4) 1.380(2) ? ? yes C(4) C(4a) 1.393(2) ? ? yes C(4a) C(9a) 1.400(2) ? ? yes C(4a) C(10) 1.533(2) ? ? yes C(5) C(6) 1.379(2) ? ? yes C(5) C(10a) 1.390(2) ? ? yes C(6) C(7) 1.375(2) ? ? yes C(7) C(8) 1.374(2) ? ? yes C(8) C(8a) 1.387(2) ? ? yes C(8a) C(9) 1.491(2) ? ? yes C(8a) C(10a) 1.398(2) ? ? yes C(9) C(9) 1.347(3) ? ? yes C(9) C(9a) 1.489(2) ? ? yes C(10) C(10a) 1.530(2) ? ? yes C(10) C(11) 1.527(2) ? ? yes C(10) C(12) 1.546(2) ? ? yes C(13) C(14) 1.347(4) ? ? yes C(13) C(15) 1.354(4) ? ? yes C(14) C(15) 1.376(4) ? ? 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(2) C(1) C(9a) 120.4(1) ? ? ? yes C(1) C(2) C(3) 120.0(1) ? ? ? yes C(2) C(3) C(4) 120.4(1) ? ? ? yes C(3) C(4) C(4a) 121.1(1) ? ? ? yes C(4) C(4a) C(9a) 118.3(1) ? ? ? yes C(4) C(4a) C(10) 123.6(1) ? ? ? yes C(9a) C(4a) C(10) 118.1(1) ? ? ? yes C(6) C(5) C(10a) 120.9(1) ? ? ? yes C(5) C(6) C(7) 120.4(1) ? ? ? yes C(6) C(7) C(8) 119.6(1) ? ? ? yes C(7) C(8) C(8a) 120.7(1) ? ? ? yes C(8) C(8a) C(9) 122.1(1) ? ? ? yes C(8) C(8a) C(10a) 120.0(1) ? ? ? yes C(9) C(8a) C(10a) 117.7(1) ? ? ? yes C(8a) C(9) C(9) 124.5(2) ? ? ? yes C(8a) C(9) C(9a) 110.2(1) ? ? ? yes C(9) C(9) C(9a) 125.2(2) ? ? ? yes C(1) C(9a) C(4a) 119.8(1) ? ? ? yes C(1) C(9a) C(9) 122.4(1) ? ? ? yes C(4a) C(9a) C(9) 117.6(1) ? ? ? yes C(4a) C(10) C(10a) 106.7(1) ? ? ? yes C(4a) C(10) C(11) 112.0(1) ? ? ? yes C(4a) C(10) C(12) 109.1(1) ? ? ? yes C(10a) C(10) C(11) 111.9(1) ? ? ? yes C(10a) C(10) C(12) 109.3(1) ? ? ? yes C(11) C(10) C(12) 107.8(1) ? ? ? yes C(5) C(10a) C(8a) 118.2(1) ? ? ? yes C(5) C(10a) C(10) 123.7(1) ? ? ? yes C(8a) C(10a) C(10) 118.1(1) ? ? ? yes C(14) C(13) C(15) 120.7(3) ? ? ? yes C(13) C(14) C(15) 119.3(3) ? ? ? yes C(13) C(15) C(14) 120.1(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J.Chem.Soc.Perkin 2' _publ_contact_author ; Israel Agranat, Department of Organic Chemistry, The Hebrew University of Jerusalem, Jerusalem 91904 ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+972-2-6585221' _publ_contact_author_fax '+972-2-6511907' _publ_contact_author_email 'isria@vms.huji.ac.il' _publ_section_title ; The Stereochemistry of Overcrowded Homomerous Bistricyclic Aromatic Enes with Alkylidene Bridges ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; #===END data_[E87]_R.S._P21/n #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 28 09:01:28 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Philips 1100 Diffractometer Control' _computing_cell_refinement 'Philips 1100 Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'SHELXS86' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 12.1390 _cell_length_b 8.2600 _cell_length_c 11.8160 _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1184.6000 _cell_formula_units_Z 4 _cell_measurement_temperature 293.2 _cell_measurement_reflns_used 18 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -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 1.162 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 207.29 _chemical_formula_moiety '1/2(C32H30)' _chemical_compound_source 'Rachel Suissa' _exptl_crystal_F_000 444.00 _exptl_absorpt_coefficient_mu 0.061 #------------------------------------------------------------------------------ _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 'UNKNOWN' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 75 _diffrn_standards_decay_% 0.00 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 6 1 2 -1 4 3 0 0 6 _diffrn_reflns_number 2606 _reflns_number_total 2606 _reflns_number_observed 1553 _reflns_observed_criterion 2.00 _diffrn_reflns_av_R_equivalents 2.25 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00000 _diffrn_orient_matrix_UB_12 0.00000 _diffrn_orient_matrix_UB_13 0.00000 _diffrn_orient_matrix_UB_21 0.00000 _diffrn_orient_matrix_UB_22 0.00000 _diffrn_orient_matrix_UB_23 0.00000 _diffrn_orient_matrix_UB_31 0.00000 _diffrn_orient_matrix_UB_32 0.00000 _diffrn_orient_matrix_UB_33 0.00000 #------------------------------------------------------------------------------ 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 64 0.003 0.002 'International Tables' H 0 60 0.000 0.000 '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 C(1) 0.5075(2) 0.5037(3) 0.2599(2) 0.0468 Uij ? ? C(2) 0.4938(3) 0.5794(4) 0.1573(2) 0.0621 Uij ? ? C(3) 0.4084(3) 0.6870(5) 0.1424(2) 0.0723 Uij ? ? C(4) 0.3366(3) 0.7146(4) 0.2290(3) 0.0638 Uij ? ? C(4a) 0.3474(2) 0.6377(3) 0.3342(2) 0.0413 Uij ? ? C(5) 0.1740(2) 0.5020(4) 0.5834(2) 0.0538 Uij ? ? C(6) 0.1681(2) 0.3704(4) 0.6543(2) 0.0616 Uij ? ? C(7) 0.2514(3) 0.2581(4) 0.6559(2) 0.0597 Uij ? ? C(8) 0.3424(2) 0.2832(3) 0.5908(2) 0.0479 Uij ? ? C(8a) 0.3518(2) 0.4180(3) 0.5214(2) 0.0363 Uij ? ? C(9) 0.4579(2) 0.4509(3) 0.4612(2) 0.0361 Uij ? ? C(9a) 0.4366(2) 0.5319(3) 0.3495(2) 0.0357 Uij ? ? C(10) 0.2645(2) 0.6680(3) 0.4287(2) 0.0449 Uij ? ? C(10a) 0.2642(2) 0.5270(3) 0.5124(2) 0.0387 Uij ? ? C(11) 0.2936(2) 0.8274(4) 0.4900(3) 0.0682 Uij ? ? C(12) 0.1479(2) 0.6853(4) 0.3755(3) 0.0715 Uij ? ? H(1) 0.5665 0.4295 0.2702 0.0559 Uij ? ? H(2) 0.5433 0.5579 0.0975 0.0745 Uij ? ? H(3) 0.3989 0.7420 0.0723 0.0868 Uij ? ? H(4) 0.2776 0.7882 0.2169 0.0769 Uij ? ? H(5) 0.1151 0.5780 0.5821 0.0652 Uij ? ? H(6) 0.1066 0.3572 0.7020 0.0740 Uij ? ? H(7) 0.2460 0.1642 0.7016 0.0722 Uij ? ? H(8) 0.4006 0.2061 0.5933 0.0576 Uij ? ? H(9) 0.4905 0.3490 0.4458 0.0434 Uij ? ? H(111) 0.3657 0.8199 0.5222 0.0829 Uij ? ? H(112) 0.2910 0.9144 0.4374 0.0829 Uij ? ? H(113) 0.2422 0.8465 0.5482 0.0829 Uij ? ? H(121) 0.0965 0.7063 0.4335 0.0857 Uij ? ? H(122) 0.1473 0.7726 0.3231 0.0857 Uij ? ? H(123) 0.1285 0.5880 0.3375 0.0857 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 C(1) 0.043(1) 0.055(2) 0.043(1) -0.008(1) 0.006(1) -0.009(1) C(2) 0.064(2) 0.084(2) 0.039(2) -0.029(2) 0.008(1) -0.005(2) C(3) 0.078(2) 0.096(3) 0.043(2) -0.023(2) -0.007(2) 0.026(2) C(4) 0.062(2) 0.069(2) 0.060(2) 0.003(2) -0.008(2) 0.023(2) C(4a) 0.040(1) 0.041(2) 0.043(1) -0.002(1) -0.005(1) 0.007(1) C(5) 0.036(2) 0.068(2) 0.058(2) 0.002(1) 0.007(1) -0.005(2) C(6) 0.049(2) 0.087(2) 0.049(2) -0.020(2) 0.012(1) 0.002(2) C(7) 0.051(2) 0.074(2) 0.054(2) -0.022(2) -0.003(1) 0.017(2) C(8) 0.041(2) 0.050(2) 0.053(2) -0.005(1) -0.007(1) 0.011(1) C(8a) 0.032(1) 0.039(1) 0.038(1) -0.002(1) -0.0032(10) 0.002(1) C(9) 0.031(1) 0.035(1) 0.042(1) 0.003(1) 0.002(1) 0.001(1) C(9a) 0.034(1) 0.040(1) 0.033(1) -0.004(1) 0.0009(10) -0.001(1) C(10) 0.037(1) 0.043(2) 0.054(2) 0.010(1) -0.001(1) 0.001(1) C(10a) 0.036(1) 0.046(2) 0.034(1) -0.003(1) 0.002(1) -0.005(1) C(11) 0.072(2) 0.047(2) 0.086(2) 0.012(2) 0.008(2) -0.003(2) C(12) 0.046(2) 0.088(2) 0.080(2) 0.020(2) -0.005(2) 0.016(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 20.42225 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1553 _refine_ls_number_parameters 146 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0540 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0650 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.750 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.20 _refine_diff_density_max -0.22 #------------------------------------------------------------------------------ _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 C(1) C(2) 1.372(4) ? ? yes C(1) C(9a) 1.394(3) ? ? yes C(2) C(3) 1.374(4) ? ? yes C(3) C(4) 1.374(4) ? ? yes C(4) C(4a) 1.400(4) ? ? yes C(4a) C(9a) 1.401(3) ? ? yes C(4a) C(10) 1.536(3) ? ? yes C(5) C(6) 1.375(4) ? ? yes C(5) C(10a) 1.405(3) ? ? yes C(6) C(7) 1.372(4) ? ? yes C(7) C(8) 1.372(4) ? ? yes C(8) C(8a) 1.389(3) ? ? yes C(8a) C(9) 1.506(3) ? ? yes C(8a) C(10a) 1.397(3) ? ? yes C(9) C(9) 1.585(4) ? ? yes C(9) C(9a) 1.499(3) ? ? yes C(10) C(10a) 1.528(3) ? ? yes C(10) C(11) 1.541(4) ? ? yes C(10) C(12) 1.546(4) ? ? 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(2) C(1) C(9a) 121.8(3) ? ? ? yes C(1) C(2) C(3) 119.2(3) ? ? ? yes C(2) C(3) C(4) 119.9(3) ? ? ? yes C(3) C(4) C(4a) 122.4(3) ? ? ? yes C(4) C(4a) C(9a) 117.2(2) ? ? ? yes C(4) C(4a) C(10) 121.3(2) ? ? ? yes C(9a) C(4a) C(10) 121.5(2) ? ? ? yes C(6) C(5) C(10a) 121.9(3) ? ? ? yes C(5) C(6) C(7) 119.8(2) ? ? ? yes C(6) C(7) C(8) 119.3(3) ? ? ? yes C(7) C(8) C(8a) 121.9(3) ? ? ? yes C(8) C(8a) C(9) 120.2(2) ? ? ? yes C(8) C(8a) C(10a) 119.4(2) ? ? ? yes C(9) C(8a) C(10a) 120.3(2) ? ? ? yes C(8a) C(9) C(9) 111.6(2) ? ? ? yes C(8a) C(9) C(9a) 111.2(2) ? ? ? yes C(9) C(9) C(9a) 112.4(2) ? ? ? yes C(1) C(9a) C(4a) 119.5(2) ? ? ? yes C(1) C(9a) C(9) 119.6(2) ? ? ? yes C(4a) C(9a) C(9) 120.9(2) ? ? ? yes C(4a) C(10) C(10a) 110.8(2) ? ? ? yes C(4a) C(10) C(11) 109.5(2) ? ? ? yes C(4a) C(10) C(12) 109.0(2) ? ? ? yes C(10a) C(10) C(11) 110.5(2) ? ? ? yes C(10a) C(10) C(12) 108.7(2) ? ? ? yes C(11) C(10) C(12) 108.2(2) ? ? ? yes C(5) C(10a) C(8a) 117.4(2) ? ? ? yes C(5) C(10a) C(10) 120.6(2) ? ? ? yes C(8a) C(10a) C(10) 122.0(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J.Chem.Soc.Perkin 2' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+972-2-6585221' _publ_contact_author_fax '+972-2-6511907' _publ_contact_author_email 'isria@vms.huji.ac.il' _publ_section_title ; The Stereochemistry of Overcrowded Homomerous Bistricyclic Aromatic Enes with Alkylidene Bridges ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER REFERENCES ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ;