# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/440 data_Sherr2_Royals/4th_yr #----------------------------------------------------------------------- _audit_creation_date 'Wed Mar 16 03:46:34 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? _publ_requested_journal 'JCS Perkin' _publ_contact_author ; Alan Kennedy Dept of P & A Chemistry University of Strathclyde 295 Cathedral St Glasgow G1 1XL ; _publ_contact_author_phone ' 0141 548 2016 ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email 'a.r.kennedy@strath.ac.uk ' #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution SAPI91 _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _cell_length_a 6.667(2) _cell_length_b 7.607(3) _cell_length_c 10.567(4) _cell_angle_alpha 73.34(3) _cell_angle_beta 86.35(3) _cell_angle_gamma 75.58(3) _cell_volume 497.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 123 _cell_measurement_reflns_used 23 _cell_measurement_theta_min 21.5 _cell_measurement_theta_max 26.2 #----------------------------------------------------------------------- _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x, -y, -z' #----------------------------------------------------------------------- _exptl_crystal_description 'chip' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.400 _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_meas 0.000 _chemical_formula_weight 206.20 _chemical_formula_analytical ? _chemical_formula_sum 'C11 H10 O4 ' _chemical_formula_moiety 'C11 H10 O4 ' _chemical_formula_structural ? _chemical_compound_source ? _exptl_crystal_F_000 216.00 _exptl_absorpt_coefficient_mu 0.105 _exptl_absorpt_correction_type none #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 123 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'Rigaku AFC7S' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 2.75 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2371 _reflns_number_total 2179 _reflns_number_observed 1840 _reflns_observed_criterion 1.50 _diffrn_reflns_av_R_equivalents 0.0097 _diffrn_reflns_av_sigmaI/netI ? _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min ? _diffrn_reflns_theta_max 26.99 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_UB_11 -0.07652 _diffrn_orient_matrix_UB_12 -0.07872 _diffrn_orient_matrix_UB_13 0.06857 _diffrn_orient_matrix_UB_21 -0.09432 _diffrn_orient_matrix_UB_22 0.00022 _diffrn_orient_matrix_UB_23 -0.06996 _diffrn_orient_matrix_UB_31 0.09610 _diffrn_orient_matrix_UB_32 -0.11745 _diffrn_orient_matrix_UB_33 -0.01276 #----------------------------------------------------------------------- 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 22 0.003 0.002 'International Tables' H 0 20 0.000 0.000 'International Tables' O 0 8 0.011 0.006 '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(1) -0.1501(1) -0.3429(1) -0.58757(9) 0.0267 Uij ? ? O(2) -0.1417(1) -0.3192(1) -0.34197(9) 0.0255 Uij ? ? O(3) -0.1668(1) -0.0868(1) -0.18525(8) 0.0285 Uij ? ? O(4) -0.4677(2) -0.1731(2) -0.13511(9) 0.0390 Uij ? ? C(1) -0.2108(2) -0.1696(2) -0.6236(1) 0.0212 Uij ? ? C(2) -0.2403(2) -0.0506(2) -0.5344(1) 0.0193 Uij ? ? C(3) -0.3003(2) 0.1467(2) -0.5868(1) 0.0208 Uij ? ? C(4) -0.3224(2) 0.2635(2) -0.5057(1) 0.0242 Uij ? ? C(5) -0.2855(2) 0.1842(2) -0.3708(1) 0.0248 Uij ? ? C(6) -0.2267(2) -0.0099(2) -0.3182(1) 0.0226 Uij ? ? C(7) -0.2029(2) -0.1313(2) -0.3985(1) 0.0202 Uij ? ? C(8) -0.2970(2) -0.1783(2) -0.1024(1) 0.0272 Uij ? ? C(9) -0.2020(2) -0.2813(2) 0.0305(1) 0.0300 Uij ? ? C(10) -0.0054(3) -0.2776(2) 0.0585(2) 0.0399 Uij ? ? C(11) -0.3302(3) -0.3845(3) 0.1227(1) 0.0443 Uij ? ? H(1) -0.121(3) -0.373(3) -0.409(2) 0.062(6) Uij ? ? H(2) -0.237(2) -0.104(2) -0.714(2) 0.025(3) Uij ? ? H(3) -0.323(2) 0.197(2) -0.679(2) 0.028(4) Uij ? ? H(4) -0.358(2) 0.400(2) -0.543(1) 0.032(4) Uij ? ? H(5) -0.299(2) 0.266(2) -0.313(2) 0.036(4) Uij ? ? H(6) 0.085(4) -0.232(3) -0.012(2) 0.079(7) Uij ? ? H(7) 0.048(3) -0.351(2) 0.144(2) 0.047(5) Uij ? ? H(8) -0.269(3) -0.444(2) 0.207(2) 0.051(5) Uij ? ? H(9) -0.381(4) -0.469(4) 0.096(3) 0.090(8) Uij ? ? H(10) -0.470(5) -0.311(4) 0.128(3) 0.115(10) 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 O(1) 0.0288(5) 0.0209(5) 0.0313(5) -0.0040(3) -0.0039(4) -0.0095(4) O(2) 0.0313(5) 0.0199(4) 0.0218(5) -0.0040(4) -0.0031(4) -0.0013(3) O(3) 0.0289(5) 0.0382(5) 0.0200(4) -0.0096(4) -0.0034(3) -0.0084(4) O(4) 0.0339(6) 0.0557(7) 0.0248(5) -0.0164(5) -0.0025(4) -0.0020(5) C(1) 0.0193(6) 0.0226(6) 0.0213(6) -0.0052(4) -0.0015(4) -0.0052(5) C(2) 0.0161(5) 0.0199(6) 0.0219(6) -0.0053(4) 0.0007(4) -0.0053(4) C(3) 0.0177(5) 0.0208(6) 0.0218(6) -0.0052(4) 0.0013(4) -0.0024(5) C(4) 0.0205(6) 0.0189(6) 0.0328(7) -0.0050(5) 0.0044(5) -0.0072(5) C(5) 0.0204(6) 0.0279(6) 0.0307(7) -0.0073(5) 0.0039(5) -0.0148(5) C(6) 0.0199(6) 0.0292(6) 0.0196(6) -0.0074(5) 0.0000(4) -0.0069(5) C(7) 0.0163(5) 0.0202(6) 0.0228(6) -0.0050(4) -0.0002(4) -0.0035(4) C(8) 0.0319(7) 0.0289(6) 0.0211(6) -0.0051(5) -0.0006(5) -0.0092(5) C(9) 0.0417(8) 0.0274(6) 0.0212(6) -0.0047(6) -0.0037(5) -0.0095(5) C(10) 0.0451(9) 0.0424(8) 0.0276(7) -0.0070(7) -0.0109(6) -0.0034(6) C(11) 0.063(1) 0.0511(10) 0.0209(7) -0.0238(9) -0.0004(7) -0.0044(7) _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 '0.86(15) x 10^-5^' _refine_ls_number_reflns 1840 _refine_ls_number_parameters 177 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_obs 0.0333 _refine_ls_wR_factor_all 0.0517 _refine_ls_wR_factor_obs 0.0501 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.908 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min -0.18 _refine_diff_density_max 0.25 #----------------------------------------------------------------------- _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(1) C(1) 1.230(1) ? ? yes O(2) C(7) 1.348(1) ? ? yes O(2) H(1) 0.90(2) ? ? no O(3) C(6) 1.400(1) ? ? yes O(3) C(8) 1.363(2) ? ? yes O(4) C(8) 1.199(2) ? ? yes C(1) C(2) 1.457(2) ? ? yes C(1) H(2) 0.95(2) ? ? no C(2) C(3) 1.404(2) ? ? yes C(2) C(7) 1.402(2) ? ? yes C(3) C(4) 1.378(2) ? ? yes C(3) H(3) 0.95(2) ? ? no C(4) C(5) 1.391(2) ? ? yes C(4) H(4) 0.97(2) ? ? no C(5) C(6) 1.383(2) ? ? yes C(5) H(5) 0.97(2) ? ? no C(6) C(7) 1.400(2) ? ? yes C(8) C(9) 1.491(2) ? ? yes C(9) C(10) 1.371(2) ? ? yes C(9) C(11) 1.444(2) ? ? yes C(10) H(6) 0.97(2) ? ? no C(10) H(7) 0.95(2) ? ? no C(11) H(8) 0.94(2) ? ? no C(11) H(9) 0.92(3) ? ? no C(11) H(10) 0.97(3) ? ? no #----------------------------------------------------------------------- #===END