# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 207/319 data_[L95]_Mehta_P21/c #------------------------------------------------------------------------------ _audit_creation_date 'Thu Feb 4 14:23:49 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 'SHELXS' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' #------------------------------------------------------------------------------ _cell_length_a 3.838(1) _cell_length_b 13.823(2) _cell_length_c 14.166(3) _cell_angle_alpha 90 _cell_angle_beta 93.76(1) _cell_angle_gamma 90 _cell_volume 749.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0.0 _cell_measurement_theta_max 0.0 #------------------------------------------------------------------------------ _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 'needles' _exptl_crystal_colour 'reddish-orange' _exptl_crystal_size_max 0.000 _exptl_crystal_size_mid 0.000 _exptl_crystal_size_min 0.000 _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 332.36 _chemical_formula_moiety 'C24 H12 O2' _chemical_compound_source ? _exptl_crystal_F_000 344.00 _exptl_absorpt_coefficient_mu 0.697 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 293 _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 'CAD4' _diffrn_measurement_method 'omega/twotheta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_% -1.03 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 1 4 1 7 1 1 3 7 _diffrn_reflns_number 1466 _reflns_number_total 1466 _reflns_number_observed 1194 _reflns_observed_criterion 3.00 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 69.78 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 0.00256 _diffrn_orient_matrix_UB_12 -0.07185 _diffrn_orient_matrix_UB_13 -0.00812 _diffrn_orient_matrix_UB_21 -0.00550 _diffrn_orient_matrix_UB_22 0.00836 _diffrn_orient_matrix_UB_23 -0.07020 _diffrn_orient_matrix_UB_31 0.26107 _diffrn_orient_matrix_UB_32 0.00095 _diffrn_orient_matrix_UB_33 0.00324 #------------------------------------------------------------------------------ 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 48 0.018 0.009 'International Tables' H 0 24 0.000 0.000 'International Tables' O 0 4 0.049 0.032 '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 O 0.7479(4) 0.35736(8) 0.39563(9) 0.0722 Uij ? ? C(1) 0.4865(3) 0.4545(1) 0.51849(9) 0.0365 Uij ? ? C(2) 0.6000(4) 0.3629(1) 0.4688(1) 0.0428 Uij ? ? C(2A) 0.5145(4) 0.2805(1) 0.5273(1) 0.0418 Uij ? ? C(3) 0.5544(5) 0.1824(1) 0.5151(1) 0.0521 Uij ? ? C(4) 0.4578(5) 0.1211(1) 0.5879(1) 0.0595 Uij ? ? C(5) 0.3280(5) 0.1563(1) 0.6695(1) 0.0549 Uij ? ? C(5A) 0.2833(4) 0.2570(1) 0.6825(1) 0.0448 Uij ? ? C(6) 0.1534(4) 0.3021(1) 0.7624(1) 0.0512 Uij ? ? C(7) 0.1290(4) 0.4009(1) 0.7634(1) 0.0521 Uij ? ? C(8) 0.2261(4) 0.4605(1) 0.6882(1) 0.0450 Uij ? ? C(8A) 0.3531(3) 0.4199(1) 0.60903(9) 0.0372 Uij ? ? C(8B) 0.3779(3) 0.3167(1) 0.6090(1) 0.0388 Uij ? ? H(3) 0.650(5) 0.159(1) 0.458(1) 0.072(6) U11 ? ? H(4) 0.488(5) 0.052(2) 0.578(1) 0.074(6) U11 ? ? H(5) 0.266(5) 0.109(1) 0.720(1) 0.076(6) U11 ? ? H(6) 0.079(5) 0.263(1) 0.815(1) 0.061(5) U11 ? ? H(7) 0.038(5) 0.432(1) 0.821(1) 0.062(5) U11 ? ? H(8) 0.190(5) 0.536(1) 0.691(1) 0.082(7) U11 ? ? 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 O 0.108(1) 0.0491(7) 0.0596(7) 0.0133(6) 0.0363(7) 0.0014(5) C(1) 0.0314(7) 0.0418(8) 0.0363(7) -0.0006(5) -0.0006(5) 0.0002(5) C(2) 0.0439(8) 0.0426(8) 0.0420(7) 0.0030(6) 0.0018(6) -0.0004(5) C(2A) 0.0386(8) 0.0421(8) 0.0447(8) 0.0017(6) -0.0032(6) 0.0009(6) C(3) 0.057(1) 0.0423(8) 0.057(1) 0.0035(7) -0.0004(7) -0.0009(7) C(4) 0.067(1) 0.0406(8) 0.071(1) 0.0007(7) -0.0029(9) 0.0065(7) C(5) 0.054(1) 0.0476(9) 0.063(1) -0.0041(7) -0.0041(8) 0.0133(7) C(5A) 0.0360(8) 0.0491(8) 0.0493(8) -0.0041(6) -0.0053(6) 0.0095(6) C(6) 0.0439(9) 0.062(1) 0.0477(8) -0.0053(7) 0.0023(6) 0.0131(7) C(7) 0.050(1) 0.062(1) 0.0444(8) -0.0014(7) 0.0096(7) 0.0051(7) C(8) 0.0406(9) 0.0512(8) 0.0435(8) -0.0007(6) 0.0063(6) 0.0023(6) C(8A) 0.0300(7) 0.0432(8) 0.0384(7) -0.0017(5) -0.0017(5) 0.0025(5) C(8B) 0.0315(7) 0.0436(8) 0.0414(7) -0.0012(5) -0.0054(5) 0.0040(5) #------------------------------------------------------------------------------ _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 30.03605 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1194 _refine_ls_number_parameters 143 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.043 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.063 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 3.099 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.17 _refine_diff_density_max -0.23 #------------------------------------------------------------------------------ _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 O C(2) 1.217(2) ? ? yes C(1) C(1) 1.368(3) ? ? yes C(1) C(2) 1.526(2) ? ? yes C(1) C(8A) 1.491(2) ? ? yes C(2) C(2A) 1.459(2) ? ? yes C(2A) C(3) 1.376(2) ? ? yes C(2A) C(8B) 1.394(2) ? ? yes C(3) C(4) 1.404(3) ? ? yes C(4) C(5) 1.376(3) ? ? yes C(5) C(5A) 1.417(2) ? ? yes C(5A) C(6) 1.412(2) ? ? yes C(5A) C(8B) 1.394(2) ? ? yes C(6) C(7) 1.369(3) ? ? yes C(7) C(8) 1.415(2) ? ? yes C(8) C(8A) 1.373(2) ? ? yes C(8A) C(8B) 1.429(2) ? ? 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(1) C(1) C(2) 123.7(2) ? ? ? yes C(1) C(1) C(8A) 131.6(2) ? ? ? yes C(2) C(1) C(8A) 104.7(1) ? ? ? yes O C(2) C(1) 127.5(1) ? ? ? yes O C(2) C(2A) 124.7(1) ? ? ? yes C(1) C(2) C(2A) 107.7(1) ? ? ? yes C(2) C(2A) C(3) 131.8(1) ? ? ? yes C(2) C(2A) C(8B) 107.6(1) ? ? ? yes C(3) C(2A) C(8B) 120.6(1) ? ? ? yes C(2A) C(3) C(4) 117.8(2) ? ? ? yes C(3) C(4) C(5) 122.0(2) ? ? ? yes C(4) C(5) C(5A) 120.7(2) ? ? ? yes C(5) C(5A) C(6) 126.2(1) ? ? ? yes C(5) C(5A) C(8B) 116.4(2) ? ? ? yes C(6) C(5A) C(8B) 117.4(1) ? ? ? yes C(5A) C(6) C(7) 118.5(1) ? ? ? yes C(6) C(7) C(8) 123.4(2) ? ? ? yes C(7) C(8) C(8A) 120.1(2) ? ? ? yes C(1) C(8A) C(8) 137.1(1) ? ? ? yes C(1) C(8A) C(8B) 107.1(1) ? ? ? yes C(8) C(8A) C(8B) 115.8(1) ? ? ? yes C(2A) C(8B) C(5A) 122.5(1) ? ? ? yes C(2A) C(8B) C(8A) 112.8(1) ? ? ? yes C(5A) C(8B) C(8A) 124.7(1) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal ' Chem. Comm. Perkin Trans. 2 ' _publ_contact_author ; Goverdhad Mehta School of Chemistry, University of Hyderabad, Hyderabad 500 046, India ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' 91-80-3092850 ' _publ_contact_author_fax ' 91-40-3010367 ' _publ_contact_author_email ' gm@orgchem.iisc.ernet.in ' loop_ _publ_author_name _publ_author_address ' P.V.V.S.Sarma ' ; School of Chemistry, University of Hyderabad, Hyderabad 500 046, India ; ' R.Uma ' ; School of Chemistry, University of Hyderabad, Hyderabad 500 046, India ; ' Sergey Pogodin ' ; Department of Organic Chemistry, The Hebrew University of Jerusalem, Jerusalem 91904, Israel ; ' Shmuel Cohen ' ; Department of Organic Chemistry, The Hebrew University of Jerusalem, Jerusalem 91904, Israel ; ' Israel Agranat ' ; Department of Organic Chemistry, The Hebrew University of Jerusalem, Jerusalem 91904, Israel ; _publ_section_title ; bis-2,2'-Acenaphthylidene-1-one: Molecular Structure and Reactions ; _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 ;