#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/2/2000649.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_2000649 _journal_name_full 'Acta Cryst.' _journal_year 1992 _journal_volume C48 _journal_page_first 1730 _journal_page_last 1733 _publ_section_title ; Structure and Conformation of cis,anti,cis- 4b,4c,8b,9,10,10a-Hexahydro-4b-hydroxy- benzo[3,4]cyclobuta[1,2-a]biphenylene- 4-carbaldehyde ; loop_ _publ_author_name 'Sandra Ianelli' 'Mario Nardelli*' 'Daniele Belletti' "Brigitte Jamart-Gr\'egoire" 'M. Abdellah Zouaoui' 'Paul Caub\`ere' _chemical_name_systematic ; cis,anti,cis-4b,5,6,6a,10b,10c-hexahydro-4b-hydroxybenzo[3,4]cyclobuta- [1,2a]biphenylene-4-carboxaldehyde ; _chemical_formula_moiety ' C19 H16 O2 ' _chemical_formula_sum ' C19 H16 O2 ' _chemical_formula_structural ? _chemical_formula_analytical ' C19 H16 O2 ' _chemical_formula_weight 276.33 _chemical_melting_point ? _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M ' P 21/c ' _symmetry_space_group_name_Hall ? _cell_length_a 13.737(2) _cell_length_b 6.9879(5) _cell_length_c 15.124(5) _cell_angle_alpha 90.00000 _cell_angle_beta 94.370(10) _cell_angle_gamma 90.00000 _cell_volume 1447.6(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 30 _cell_measurement_theta_min 21 _cell_measurement_theta_max 40 _cell_measurement_temperature 293(2) _exptl_crystal_description ; Thick prisms ; _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.36 _exptl_crystal_density_diffrn 1.2679 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 584.0 _exptl_absorpt_coefficient_mu .6066 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_type ' Cu K\a~1~' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_source 'standard copper anode' _diffrn_radiation_monochromator 'Ni filter' _diffrn_measurement_device 'Siemens-AED diffractometer' _diffrn_measurement_method 'Peak profile: \q--2\q' _diffrn_reflns_number 2268 _diffrn_reflns_av_R_equivalents 0.0268 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 70 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_reduction_process ; Standard. Lp correction. ; _diffrn_standards_number 1 _diffrn_standards_interval_count 50 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -5 2 8 _reflns_observed_criterion 'I>2\s(I)' _refine_ls_structure_factor_coef 'F' _refine_ls_matrix_type 'full' _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0453 _refine_ls_wR_factor_obs 0.0468 _refine_ls_goodness_of_fit_obs 0.7321 _refine_ls_number_reflns 2183 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme 'unit ' _refine_ls_shift/esd_max 0.03 _refine_ls_shift/esd_mean ? _refine_diff_density_max 0.08 _refine_diff_density_min -0.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source O Oxygen .047 .032 'IT.4 Tab.2.2A 2.3.1' C Carbon .017 .009 'IT.4 Tab.2.2A 2.3.1' H Hydrogen .000 .000 'IT.4 Tab.2.2C ' 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 _atom_site_type_symbol O1 .49500(10) -.1726(3) .10670(10) .0672(8) Uani . . O O2 .39000(10) -.0078(3) .39600(10) .0487(6) Uani . . O C1 .4539(2) -.1166(4) .1698(2) .0499(9) Uani . . C C2 .3992(2) .0623(4) .17140(10) .0411(8) Uani . . C C3 .3964(2) .1952(4) .1016(2) .0515(9) Uani . . C C4 .3416(2) .3616(5) .1038(2) .0600(11) Uani . . C C5 .2878(2) .4071(4) .1760(2) .0590(10) Uani . . C C6 .2936(2) .2790(4) .2455(2) .0458(8) Uani . . C C7 .3448(2) .1103(4) .24220(10) .0391(8) Uani . . C C8 .3140(2) .0366(4) .33100(10) .0383(8) Uani . . C C9 .2611(2) .2402(4) .3388(2) .0479(8) Uani . . C C10 .1516(2) .2407(5) .3496(2) .0633(12) Uani . . C C11 .0987(2) .1012(5) .2857(2) .0652(12) Uani . . C C12 .1334(2) -.1035(5) .3005(2) .0509(9) Uani . . C C13 .2476(2) -.1375(4) .3248(2) .0409(8) Uani . . C C14 .2179(2) -.2190(4) .4121(2) .0412(8) Uani . . C C15 .1195(2) -.1884(4) .3917(2) .0478(9) Uani . . C C16 .0502(2) -.2357(5) .4496(2) .0608(11) Uani . . C C17 .0863(2) -.3198(5) .5292(2) .0634(11) Uani . . C C18 .1850(2) -.3548(5) .5483(2) .0592(11) Uani . . C C19 .2542(2) -.3047(4) .4898(2) .0504(8) Uani . . C H2O .432(2) .067(5) .397(2) .079(12) Uiso . O2 H H1 .4532(16) -.204(4) .2273(15) .044(7) Uiso . C1 H H3 .4311(19) .159(4) .0494(18) .062(8) Uiso . C3 H H4 .338(2) .448(4) .0528(18) .066(9) Uiso . C4 H H5 .240(2) .517(5) .1716(19) .078(10) Uiso . C5 H H9 .2978(19) .327(4) .3901(18) .064(8) Uiso . C9 H H101 .122(2) .378(5) .333(2) .084(10) Uiso . C10 H H102 .144(2) .214(4) .4119(19) .063(9) Uiso . C10 H H111 .105(2) .141(4) .2223(19) .068(9) Uiso . C11 H H112 .020(2) .101(4) .2897(18) .075(9) Uiso . C11 H H12 .1030(19) -.192(4) .2462(17) .060(8) Uiso . C12 H H13 .2788(17) -.238(4) .2863(15) .045(7) Uiso . C13 H H16 -.026(2) -.210(5) .430(2) .084(10) Uiso . C16 H H17 .042(2) -.358(5) .577(2) .081(10) Uiso . C17 H H18 .2053(19) -.421(4) .6038(18) .065(9) Uiso . C18 H H19 .3236(19) -.334(4) .5002(16) .055(8) Uiso . C19 H