#------------------------------------------------------------------------------ #$Date: 2008-01-26 17:25:03 +0000 (Sat, 26 Jan 2008) $ #$Revision: 20 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003578.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_2003578 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1131 _journal_page_last 1133 _publ_section_title ; Vanillin-I ; _chemical_formula_sum 'C8 H8 O3' _chemical_formula_weight 152.14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _symmetry_space_group_name_H-M 'P 21' _cell_length_a 14.049(1) _cell_length_b 7.8740(8) _cell_length_c 15.017(1) _cell_angle_alpha 90.00 _cell_angle_beta 115.45(1) _cell_angle_gamma 90.00 _cell_volume 1499.9(2) _cell_formula_units_Z 8 _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_meas No _exptl_crystal_density_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 15 _exptl_absorpt_coefficient_mu 0.104 _cell_measurement_temperature 293(2) _exptl_crystal_description Needles _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_colour Colourless _chemical_compound_source ; Single crystals of vanillin were grown by gel technique. Details are published elsewhere (Sureshkumar, Sivakumar & Natarajan, 1994). ; _diffrn_measurement_device 'Enraf Nonius CAD-4 diffractometer' _diffrn_measurement_method '\w/2\q scans' _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _diffrn_reflns_number 2970 _reflns_number_total 2848 _reflns_number_observed 2139 _reflns_observed_criterion >2sigma(I) _diffrn_reflns_av_R_equivalents 0.0090 _diffrn_reflns_theta_max 24.96 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2 _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_obs 0.0250 _refine_ls_wR_factor_obs 0.0603 _refine_ls_wR_factor_all 0.0658 _refine_ls_goodness_of_fit_obs 1.066 _refine_ls_goodness_of_fit_all 0.970 _refine_ls_number_reflns 2848 _refine_ls_number_parameters 526 _refine_ls_hydrogen_treatment refall _refine_ls_weighting_scheme ;calc w = 1/[\s^2^(F~o~^2^)+(0.0421P)^2^+0.0000P] where P = (F~o~^2^+2F~c~^2^)/3 ; _refine_ls_shift/esd_max -0.001 _refine_diff_density_max 0.093 _refine_diff_density_min -0.085 _refine_ls_extinction_method 'F~c~^*^ = kF~c~[1 + 0.001\xF~c~^2^\l^3^/sin(2\ _refine_ls_extinction_coef 0.0110(10) 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 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881 _refine_ls_abs_structure_Flack 0.01(81) 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 C1A 1 -0.5353(2) -0.1403(3) -0.1898(2) 0.0522(6) C2A 1 -0.6376(2) -0.1900(3) -0.2551(2) 0.0474(5) C3A 1 -0.6984(2) -0.2800(3) -0.2202(1) 0.0431(5) C4A 1 -0.6580(2) -0.3225(3) -0.1203(1) 0.0485(5) C5A 1 -0.5578(2) -0.2711(4) -0.0560(2) 0.0605(7) C6A 1 -0.4971(2) -0.1802(3) -0.0912(2) 0.0607(6) C7A 1 -0.4684(2) -0.0463(4) -0.2247(2) 0.0649(7) C8A 1 -0.8469(2) -0.2927(4) -0.3769(2) 0.0606(7) O1A 1 -0.4922(1) -0.0024(2) -0.3085(2) 0.0756(5) O2A 1 -0.7993(1) -0.3332(2) -0.27468(9) 0.0555(4) O3A 1 -0.7148(1) -0.4128(3) -0.0834(1) 0.0654(5) C1B 1 -0.0811(2) 0.3711(3) -0.2820(2) 0.0516(6) C2B 1 -0.1194(2) 0.3109(3) -0.2159(2) 0.0496(6) C3B 1 -0.2175(2) 0.2403(3) -0.2499(2) 0.0486(5) C4B 1 -0.2801(2) 0.2283(3) -0.3520(2) 0.0573(6) C5B 1 -0.2421(2) 0.2893(4) -0.4167(2) 0.0699(8) C6B 1 -0.1427(2) 0.3592(4) -0.3816(2) 0.0638(7) C7B 1 0.0241(2) 0.4459(4) -0.2465(2) 0.0614(6) C8B 1 -0.2067(3) 0.1908(5) -0.0895(2) 0.0745(8) O1B 1 0.0852(1) 0.4656(3) -0.1616(1) 0.0752(5) O2B 1 -0.2640(1) 0.1771(3) -0.1943(1) 0.0664(5) O3B 1 -0.3772(1) 0.1597(3) -0.3889(1) 0.0823(6) C1C 1 -0.0993(2) -0.1683(3) -0.2131(2) 0.0520(6) C2C 1 -0.1988(2) -0.2257(3) -0.2797(2) 0.0477(5) C3C 1 -0.2641(2) -0.3041(3) -0.2464(1) 0.0458(5) C4C 1 -0.2314(2) -0.3264(3) -0.1445(1) 0.0501(5) C5C 1 -0.1339(2) -0.2682(4) -0.0792(2) 0.0657(7) C6C 1 -0.0686(2) -0.1896(4) -0.1131(2) 0.0669(7) C7C 1 -0.0283(2) -0.0853(4) -0.2471(2) 0.0644(7) C8C 1 -0.4045(2) -0.3334(6) -0.4071(2) 0.0758(9) O1C 1 -0.0445(1) -0.0610(3) -0.3317(1) 0.0710(5) O2C 1 -0.3620(1) -0.3656(2) -0.3034(1) 0.0617(5) O3C 1 -0.2928(1) -0.4023(3) -0.1081(1) 0.0687(5) C1D 1 0.3563(2) 0.3354(3) -0.3111(2) 0.0515(5) C2D 1 0.3226(2) 0.2615(3) -0.2450(2) 0.0462(5) C3D 1 0.2240(2) 0.1904(3) -0.2789(1) 0.0419(5) C4D 1 0.1566(2) 0.1947(3) -0.3800(2) 0.0465(5) C5D 1 0.1899(2) 0.2683(3) -0.4455(2) 0.0561(6) C6D 1 0.2894(2) 0.3377(4) -0.4108(2) 0.0599(6) C7D 1 0.4609(2) 0.4114(4) -0.2760(2) 0.0637(7) C8D 1 0.2466(2) 0.1089(4) -0.1180(2) 0.0598(6) O1D 1 0.5264(1) 0.4147(3) -0.1917(1) 0.0725(5) O2D 1 0.1828(1) 0.1121(2) -0.22245(9) 0.0541(4) O3D 1 0.0588(1) 0.1277(3) -0.4165(1) 0.0624(5) H2A 1 -0.665(2) -0.159(3) -0.327(2) 0.052(6) H5A 1 -0.538(2) -0.295(4) 0.011(2) 0.073(8) H6A 1 -0.425(2) -0.144(4) -0.047(2) 0.079(8) H7A 1 -0.395(2) -0.016(4) -0.170(2) 0.077(8) H81A 1 -0.916(2) -0.344(4) -0.399(2) 0.084(9) H82A 1 -0.808(2) -0.347(4) -0.411(2) 0.068(7) H83A 1 -0.850(2) -0.173(4) -0.389(2) 0.075(9) H3A 1 -0.779(2) -0.424(4) -0.125(2) 0.069(8) H2B 1 -0.074(2) 0.314(3) -0.148(2) 0.055(6) H5B 1 -0.290(2) 0.281(4) -0.486(2) 0.083(8) H6B 1 -0.118(2) 0.401(4) -0.428(2) 0.072(7) H7B 1 0.044(2) 0.478(4) -0.303(2) 0.078(8) H81B 1 -0.195(2) 0.320(5) -0.071(2) 0.088(9) H82B 1 -0.134(3) 0.136(5) -0.06(3) 0.12(1) H83B 1 -0.246(3) 0.140(5) -0.061(3) 0.118(11) H3B 1 -0.390(2) 0.118(4) -0.340(2) 0.10(1) H2C 1 -0.221(2) -0.216(3) -0.353(2) 0.059(6) H5C 1 -0.113(2) -0.294(4) -0.011(2) 0.10(1) H6C 1 -0.000(2) -0.145(4) -0.070(2) 0.089(9) H7C 1 0.038(2) -0.038(4) -0.195(2) 0.081(8) H81C 1 -0.361(2) -0.385(4) -0.437(2) 0.087(9) H82C 1 -0.407(2) -0.212(5) -0.422(2) 0.09(1) H83C 1 -0.471(2) -0.383(4) -0.434(2) 0.086(9) H3C 1 -0.350(2) -0.450(4) -0.152(2) 0.09(1) H2D 1 0.370(2) 0.261(3) -0.179(2) 0.053(6) H5D 1 0.143(2) 0.273(3) -0.513(2) 0.061(7) H6D 1 0.312(2) 0.394(3) -0.458(2) 0.072(8) H7D 1 0.474(2) 0.459(4) -0.334(2) 0.088(9) H81D 1 0.320(2) 0.058(4) -0.102(2) 0.074(7) H82D 1 0.254(2) 0.225(4) -0.095(2) 0.074(9) H83D 1 0.205(2) 0.038(4) -0.091(2) 0.075(8) H3D 1 0.050(2) 0.076(4) -0.372(2) 0.068(8) 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 C1A 0.0408(11) -0.0031(10) 0.0247(11) 0.0484(13) -0.0013(11) 0.0686(15) C2A 0.0445(12) -0.0009(11) 0.0194(10) 0.0497(13) 0.0000(11) 0.0475(13) C3A 0.0369(10) -0.0034(9) 0.0150(9) 0.0456(13) -0.0026(9) 0.0442(11) C4A 0.0452(10) -0.0020(11) 0.0193(9) 0.0550(14) 0.0005(11) 0.0452(11) C5A 0.0497(13) -0.0071(12) 0.0095(11) 0.073(2) 0.0049(12) 0.0466(13) C6A 0.0392(12) -0.0059(12) 0.0067(11) 0.064(2) -0.0006(13) 0.0631(15) C7A 0.0488(14) -0.0060(13) 0.0303(14) 0.060(2) 0.0015(15) 0.087(2) C8A 0.0531(14) -0.0088(14) 0.0133(11) 0.073(2) 0.0025(13) 0.0474(14) O1A 0.0650(11) -0.0120(10) 0.0442(10) 0.0818(14) 0.0049(11) 0.0913(14) O2A 0.0408(7) -0.0136(8) 0.0102(6) 0.0751(11) 0.0039(8) 0.0425(8) O3A 0.0515(9) -0.0161(10) 0.0165(8) 0.0943(14) 0.0056(9) 0.0458(9) C1B 0.0501(12) -0.0034(11) 0.0310(11) 0.0506(14) -0.0014(11) 0.0616(14) C2B 0.0436(11) -0.0020(11) 0.0194(10) 0.0563(15) -0.0026(12) 0.0484(13) C3B 0.0475(11) -0.0045(11) 0.0239(10) 0.0560(14) -0.0013(11) 0.0463(12) C4B 0.0497(12) -0.0143(12) 0.0198(10) 0.072(2) -0.0035(12) 0.0490(12) C5B 0.069(2) -0.019(2) 0.0235(12) 0.094(2) -0.0008(14) 0.0456(13) C6B 0.066(2) -0.0130(14) 0.0365(13) 0.078(2) 0.0003(13) 0.0577(15) C7B 0.0578(14) -0.0072(13) 0.0362(14) 0.060(2) 0.0004(14) 0.075(2) C8B 0.075(2) -0.021(2) 0.0288(13) 0.102(3) 0.001(2) 0.0490(14) O1B 0.0519(9) -0.0155(10) 0.0277(9) 0.0941(14) -0.0024(11) 0.0793(13) O2B 0.0565(9) -0.0232(10) 0.0258(7) 0.0983(14) -0.0020(9) 0.0479(9) O3B 0.0598(10) -0.0366(11) 0.0152(8) 0.125(2) 0.0004(11) 0.0524(10) C1C 0.0426(11) -0.0071(11) 0.0192(10) 0.0588(15) -0.0012(11) 0.0531(13) C2C 0.0425(11) -0.0010(11) 0.0162(9) 0.0555(14) -0.0012(11) 0.0429(12) C3C 0.0377(10) -0.0021(10) 0.0129(9) 0.0509(13) -0.0007(10) 0.0441(11) C4C 0.0456(11) -0.0025(11) 0.0175(10) 0.0575(14) 0.0028(11) 0.0450(12) C5C 0.0547(13) -0.0150(14) 0.0119(11) 0.089(2) 0.0056(13) 0.0434(13) C6C 0.0454(13) -0.0191(14) 0.0066(11) 0.089(2) 0.0017(14) 0.0516(14) C7C 0.0497(13) -0.0182(14) 0.0215(12) 0.078(2) -0.0069(14) 0.063(2) C8C 0.055(2) -0.025(2) 0.0074(12) 0.111(3) 0.002(2) 0.0459(14) O1C 0.0641(10) -0.0252(10) 0.0333(9) 0.0908(13) -0.0109(10) 0.0641(11) O2C 0.0434(8) -0.0168(9) 0.0093(6) 0.0875(13) 0.0051(8) 0.0442(8) O3C 0.0563(9) -0.0220(10) 0.0207(8) 0.0976(14) 0.0044(9) 0.0498(9) C1D 0.0473(12) -0.0026(11) 0.0251(10) 0.0514(14) -0.0030(11) 0.0585(13) C2D 0.0413(11) 0.0002(10) 0.0140(10) 0.0487(12) -0.0010(10) 0.0440(12) C3D 0.0413(10) 0.0013(10) 0.0183(9) 0.0451(12) 0.0014(10) 0.0401(11) C4D 0.0423(11) -0.0009(11) 0.0137(9) 0.0506(13) -0.0016(10) 0.0421(11) C5D 0.0568(13) -0.0057(13) 0.0157(11) 0.066(2) 0.0044(12) 0.0397(12) C6D 0.0659(14) -0.0086(13) 0.0314(12) 0.066(2) 0.0018(12) 0.0536(14) C7D 0.0554(14) -0.0105(14) 0.0332(14) 0.068(2) -0.0052(14) 0.073(2) C8D 0.0561(14) -0.0093(15) 0.0127(10) 0.079(2) 0.0021(13) 0.0370(12) O1D 0.0482(9) -0.0131(10) 0.0232(9) 0.0870(14) -0.0028(11) 0.0780(13) O2D 0.0453(7) -0.0110(8) 0.0142(6) 0.0750(11) 0.0022(8) 0.0381(7) O3D 0.0467(8) -0.0144(9) 0.0098(7) 0.0867(13) 0.0068(9) 0.0436(8)