#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003518.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_2003518 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1137 _journal_page_last 1139 _publ_section_title ; cis- and trans-Spiro[(4',4'-dimethyl-2',6'-dioxacyclohexane)-1',3- (4-methylenebicyclo[3.3.0]octane)]-2,2-dicarboxylate ; _chemical_formula_moiety 'C18 H26 O6' _chemical_formula_sum 'C18 H26 O6' _chemical_formula_structural 'C18 H26 O6' _chemical_formula_weight 338.39 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _symmetry_space_group_name_H-M 'P -1' _cell_length_a 8.960(4) _cell_length_b 11.507(6) _cell_length_c 8.889(7) _cell_angle_alpha 97.29(5) _cell_angle_beta 97.71(5) _cell_angle_gamma 105.58(3) _cell_volume 862.0(9) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.304 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.615 _cell_measurement_theta_max 15.020 _exptl_absorpt_coefficient_mu 0.097 _cell_measurement_temperature 296(2) _exptl_crystal_description 'prismatic' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.06 _exptl_crystal_colour 'colourless' _chemical_compound_source ? _diffrn_measurement_device 'AFC5R' _diffrn_measurement_method 'omega scans with profile analysis' _exptl_absorpt_correction_type '\y scan' _exptl_absorpt_correction_T_min 0.883 _exptl_absorpt_correction_T_max 1.000 _diffrn_reflns_number 3964 _reflns_number_total 3964 _reflns_number_observed 2101 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.038 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -3.23 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.061 _refine_ls_wR_factor_obs 0.154 _refine_ls_wR_factor_all 0.198 _refine_ls_goodness_of_fit_obs 1.109 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_number_reflns 3963 _refine_ls_number_parameters 231 _refine_ls_hydrogen_treatment ? _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0919P)^2^+0.2615P] wh _refine_ls_shift/esd_max 0.001 _refine_diff_density_max 0.30 _refine_diff_density_min -0.34 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag 'C' 'C' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0033 0.001 'H' 'H' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0000 0.000 'O' 'O' 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 0.0106 0.006 ;MSC/AFC Diffractometer Control Software (Molecular Structure Corporation, 1992) ; loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv O1 1 0.6669(3) 0.4951(2) 0.1061(3) 0.057 O2 1 0.5262(3) 0.4363(2) 0.2856(3) 0.055 O3 1 0.7536(3) 0.2432(2) -0.0580(3) 0.068 O4 1 0.9163(2) 0.3771(2) 0.1388(2) 0.045 O5 1 0.7827(2) 0.1732(2) 0.2917(2) 0.042 O6 1 0.7928(2) 0.3620(2) 0.4329(2) 0.037 C1 1 0.6501(3) 0.2964(2) 0.1699(3) 0.038 C2 1 0.6973(3) 0.2582(2) 0.3297(3) 0.037 C3 1 0.5398(4) 0.1896(3) 0.3734(4) 0.045 C4A 0.753(10) 0.4098(4) 0.1769(4) 0.2417(5) 0.038 H4A 0.753(10) 0.3698(4) 0.2479(4) 0.2586(5) 0.046 C4B 0.247(10) 0.4572(15) 0.1096(11) 0.2223(7) 0.048 H4B 0.247(10) 0.4974(15) 0.0385(11) 0.2067(7) 0.058 C5 1 0.2736(4) 0.0675(3) 0.1757(4) 0.063 H5A 0.753(10) 0.1861(4) 0.0662(3) 0.2297(4) 0.075 H5B 0.753(10) 0.3025(4) -0.0074(3) 0.1813(4) 0.075 H5C 0.247(10) 0.2320(4) -0.0175(3) 0.1864(4) 0.075 H5D 0.247(10) 0.2282(4) 0.1169(3) 0.2422(4) 0.075 C6 1 0.2308(4) 0.0827(3) 0.0063(4) 0.063 H6A 1 0.1333(4) 0.1046(3) -0.0093(4) 0.075 H6B 1 0.2177(4) 0.0068(3) -0.0626(4) 0.075 C7 1 0.3685(4) 0.1859(3) -0.0257(4) 0.055 H7A 1 0.3942(4) 0.1657(3) -0.1264(4) 0.066 H7B 1 0.3442(4) 0.2634(3) -0.0183(4) 0.066 C8 1 0.5005(4) 0.1892(3) 0.1022(4) 0.050 H8A 0.753(10) 0.5325(4) 0.1148(3) 0.0795(4) 0.060 H8B 0.247(10) 0.5501(4) 0.1368(3) 0.0434(4) 0.060 C9 1 0.5112(4) 0.1606(3) 0.5072(4) 0.059 H9A 0.753(10) 0.4079(4) 0.1313(3) 0.5222(4) 0.071 H9B 0.753(10) 0.5942(4) 0.1695(3) 0.5868(4) 0.071 H9C 0.247(10) 0.4367(4) 0.0876(3) 0.5111(4) 0.071 H9D 0.247(10) 0.5653(4) 0.2132(3) 0.5979(4) 0.071 C10 1 0.6175(3) 0.4207(3) 0.1824(3) 0.039 C11 1 0.4818(4) 0.5487(3) 0.2971(4) 0.062 H11A 1 0.4151(25) 0.5497(11) 0.3729(22) 0.093 H11B 1 0.4263(27) 0.5536(12) 0.1990(9) 0.093 H11C 1 0.5746(5) 0.6174(4) 0.3270(29) 0.093 C12 1 0.7770(4) 0.3009(3) 0.0693(3) 0.041 C13 1 1.0449(4) 0.3786(4) 0.0571(4) 0.065 H13A 1 1.1367(10) 0.4424(17) 0.1100(18) 0.098 H13B 1 1.0171(13) 0.3932(25) -0.0455(11) 0.098 H13C 1 1.0666(21) 0.3011(9) 0.0521(28) 0.098 C14 1 0.8612(4) 0.1399(3) 0.4243(4) 0.046 H14A 1 0.9179(4) 0.0832(3) 0.3907(4) 0.056 H14B 1 0.7835(4) 0.0986(3) 0.4809(4) 0.056 C15 1 0.9756(3) 0.2512(3) 0.5299(3) 0.041 C16 1 0.8828(4) 0.3406(3) 0.5680(3) 0.043 H16A 1 0.8120(4) 0.3086(3) 0.6362(3) 0.052 H16B 1 0.9552(4) 0.4178(3) 0.6222(3) 0.052 C17 1 1.0413(4) 0.2121(3) 0.6768(4) 0.057 H17A 1 1.1130(22) 0.2824(5) 0.7444(12) 0.086 H17B 1 1.0957(24) 0.1531(17) 0.6508(5) 0.086 H17C 1 0.9563(5) 0.1764(20) 0.7274(15) 0.086 C18 1 1.1112(4) 0.3102(3) 0.4502(4) 0.056 H18A 1 1.1796(16) 0.3824(13) 0.5169(12) 0.083 H18B 1 1.0695(4) 0.3319(21) 0.3561(15) 0.083 H18C 1 1.1694(18) 0.2531(9) 0.4276(26) 0.083 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 O1 0.0599(14) 0.0214(11) 0.0285(12) 0.0538(13) 0.0341(12) 0.070(2) O2 0.0581(13) 0.0309(12) 0.0246(11) 0.0703(15) 0.0238(11) 0.0521(13) O3 0.078(2) 0.0096(13) 0.0202(12) 0.074(2) -0.0085(12) 0.0436(14) O4 0.0385(11) 0.0100(10) 0.0157(9) 0.0548(12) 0.0132(10) 0.0423(12) O5 0.0482(11) 0.0121(9) 0.0056(9) 0.0361(10) 0.0050(9) 0.0401(11) O6 0.0434(10) 0.0094(8) 0.0038(8) 0.0311(9) 0.0070(8) 0.0361(10) C1 0.0378(15) 0.0035(12) 0.0085(12) 0.0384(15) 0.0100(12) 0.0334(14) C2 0.0370(14) 0.0087(11) 0.0092(12) 0.0346(14) 0.0094(11) 0.0383(15) C3 0.045(2) 0.0040(13) 0.0114(14) 0.0366(15) 0.0150(13) 0.051(2) C4A 0.037(2) 0.008(2) 0.013(2) 0.026(2) 0.005(2) 0.052(2) C4B 0.052(8) 0.007(6) 0.023(6) 0.043(8) 0.023(6) 0.054(8) C5 0.046(2) 0.003(2) 0.016(2) 0.062(2) 0.007(2) 0.073(2) C6 0.047(2) 0.005(2) -0.007(2) 0.053(2) -0.005(2) 0.074(3) C7 0.049(2) 0.008(2) -0.005(2) 0.054(2) 0.001(2) 0.052(2) C8 0.047(2) 0.0002(14) 0.0008(14) 0.048(2) 0.0133(14) 0.046(2) C9 0.056(2) 0.006(2) 0.025(2) 0.060(2) 0.019(2) 0.061(2) C10 0.0308(14) 0.0083(12) 0.0035(12) 0.046(2) 0.0087(13) 0.037(2) C11 0.064(2) 0.044(2) 0.010(2) 0.074(2) 0.009(2) 0.061(2) C12 0.052(2) 0.0149(13) 0.0125(13) 0.0360(15) 0.0092(12) 0.039(2) C13 0.057(2) 0.029(2) 0.036(2) 0.091(3) 0.028(2) 0.064(2) C14 0.056(2) 0.0181(14) 0.0052(14) 0.039(2) 0.0093(13) 0.045(2) C15 0.045(2) 0.0162(13) 0.0044(13) 0.040(2) 0.0084(12) 0.039(2) C16 0.048(2) 0.0093(13) 0.0020(13) 0.042(2) 0.0065(12) 0.036(2) C17 0.068(2) 0.023(2) 0.001(2) 0.054(2) 0.016(2) 0.051(2) C18 0.049(2) 0.016(2) 0.012(2) 0.066(2) 0.015(2) 0.053(2)