# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1244 data_1 #----------------------------------------------------------------------- _audit_creation_date 'Sat Feb 6 07:46:31 1999' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #----------------------------------------------------------------------- _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution SHELXS86 _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #----------------------------------------------------------------------- _cell_length_a 13.690(4) _cell_length_b 25.900(3) _cell_length_c 5.179(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1836(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 15 _cell_measurement_theta_min 13.49 _cell_measurement_theta_max 21.41 #----------------------------------------------------------------------- _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_Int_Tables_number 19 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x, -y,1/2+z' '1/2+x,1/2-y, -z' ' -x,1/2+y,1/2-z' #----------------------------------------------------------------------- _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid ? _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.173 _exptl_crystal_density_measured ? _exptl_crystal_F000 704.00 _exptl_absorpt_coefficient_mu_cm 0.841 #----------------------------------------------------------------------- _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source 'X-ray tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector ? _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_decay_\% 0.35 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2487 _diffrn_reflns_av_R_equivalents 0.00 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 17 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 21 _diffrn_reflns_l_min 0 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 27.4795 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.05128 _diffrn_orient_matrix_12 -0.02746 _diffrn_orient_matrix_13 0.00710 _diffrn_orient_matrix_21 -0.05125 _diffrn_orient_matrix_22 0.02701 _diffrn_orient_matrix_23 0.02624 _diffrn_orient_matrix_31 -0.00894 _diffrn_orient_matrix_32 0.00269 _diffrn_orient_matrix_33 -0.19118 #----------------------------------------------------------------------- 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 72 0.003 0.002 'International Tables' H 0 112 0.000 0.000 'International Tables' O 0 20 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 O1 1.2766(3) 0.2699(2) 0.342(1) 0.0766 Uij ? ? O2 0.9678(2) 0.2039(1) 0.1105(8) 0.0446 Uij ? ? O3 1.2091(3) 0.1532(1) 0.2856(7) 0.0527 Uij ? ? O4 1.3443(3) 0.1353(2) 0.065(1) 0.0923 Uij ? ? O5 0.9212(3) 0.1487(2) -0.3642(8) 0.0592 Uij ? ? C1 1.0284(4) 0.2382(2) 0.228(1) 0.0462 Uij ? ? C2 0.9736(4) 0.2816(2) 0.347(1) 0.0560 Uij ? ? C3 1.0383(6) 0.3228(3) 0.430(2) 0.1497 Uij ? ? C4 1.1385(5) 0.3124(3) 0.513(2) 0.0803 Uij ? ? C5 1.1870(4) 0.2712(2) 0.356(1) 0.0568 Uij ? ? C6 1.1273(4) 0.2327(2) 0.227(1) 0.0442 Uij ? ? C7 1.1766(4) 0.1900(2) 0.087(1) 0.0469 Uij ? ? C8 1.1070(4) 0.1632(2) -0.095(1) 0.0516 Uij ? ? C9 1.0106(4) 0.1541(2) 0.043(1) 0.0431 Uij ? ? C10 1.2933(4) 0.1282(3) 0.247(1) 0.0563 Uij ? ? C11 1.3127(5) 0.0911(2) 0.461(1) 0.0726 Uij ? ? C12 0.9358(4) 0.1252(2) -0.117(1) 0.0466 Uij ? ? C13 0.8400(4) 0.1163(2) 0.023(1) 0.0500 Uij ? ? C14 0.7743(4) 0.0771(2) -0.108(1) 0.0538 Uij ? ? C15 0.6787(4) 0.0683(2) 0.027(1) 0.0574 Uij ? ? C16 0.6101(4) 0.0309(2) -0.109(1) 0.0634 Uij ? ? C17 0.5135(5) 0.0249(2) 0.025(2) 0.0802 Uij ? ? C18 0.4479(5) -0.0155(3) -0.104(2) 0.1049 Uij ? ? H1 0.9708 0.2743 0.5379 0.0899 Uij ? ? H2 0.9113 0.2869 0.2276 0.0899 Uij ? ? H3 1.0063 0.3388 0.5753 0.0899 Uij ? ? H4 1.0415 0.3467 0.2934 0.1772 Uij ? ? H5 1.1229 0.2965 0.6795 0.0899 Uij ? ? H6 1.1709 0.3456 0.5040 0.0899 Uij ? ? H7 1.2367 0.2049 -0.0064 0.0899 Uij ? ? H8 1.1330 0.1264 -0.1534 0.0899 Uij ? ? H9 1.0889 0.1867 -0.2644 0.0899 Uij ? ? H10 1.0160 0.1349 0.2162 0.0899 Uij ? ? H11 1.3744 0.0747 0.4267 0.0888 Uij ? ? H12 1.2631 0.0665 0.4653 0.0888 Uij ? ? H13 1.3170 0.1094 0.6177 0.1273 Uij ? ? H14 0.9653 0.0874 -0.1644 0.0899 Uij ? ? H15 0.8510 0.1039 0.1956 0.0899 Uij ? ? H16 0.8034 0.1504 0.0073 0.0899 Uij ? ? H17 0.8110 0.0426 -0.1231 0.0899 Uij ? ? H18 0.7676 0.0899 -0.2989 0.0899 Uij ? ? H19 0.6890 0.0585 0.2160 0.0899 Uij ? ? H20 0.6461 0.1021 0.0593 0.0899 Uij ? ? H21 0.6429 -0.0036 -0.1138 0.0899 Uij ? ? H22 0.6129 0.0382 -0.2942 0.1772 Uij ? ? H23 0.5252 0.0089 0.2135 0.0899 Uij ? ? H24 0.4842 0.0571 0.0724 0.0899 Uij ? ? H25 0.4792 -0.0475 -0.1046 0.1772 Uij ? ? H26 0.3884 -0.0179 -0.0031 0.1273 Uij ? ? H27 0.4319 -0.0045 -0.2715 0.1273 Uij ? ? H28 0.8793 0.1712 -0.3306 0.1772 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 O1 0.041(2) 0.086(3) 0.103(4) -0.008(2) -0.010(3) 0.002(3) O2 0.035(2) 0.043(2) 0.057(3) 0.000(2) 0.001(2) -0.005(2) O3 0.042(2) 0.066(2) 0.050(2) 0.011(2) 0.004(2) 0.011(2) O4 0.067(3) 0.119(4) 0.090(4) 0.041(3) 0.035(3) 0.022(4) O5 0.058(3) 0.077(3) 0.042(2) 0.006(2) -0.003(2) -0.001(2) C1 0.046(3) 0.042(3) 0.050(4) -0.002(3) 0.002(4) 0.009(3) C2 0.052(3) 0.049(3) 0.068(5) 0.005(3) 0.000(4) -0.013(4) C3 0.072(5) 0.124(7) 0.25(1) 0.018(5) -0.021(8) -0.124(9) C4 0.069(5) 0.068(4) 0.104(6) -0.011(4) -0.008(5) -0.021(5) C5 0.052(4) 0.059(4) 0.059(4) -0.004(4) -0.004(4) 0.015(4) C6 0.037(3) 0.047(3) 0.049(4) -0.005(3) 0.002(3) 0.009(3) C7 0.035(3) 0.059(4) 0.047(4) 0.001(3) 0.005(3) 0.004(4) C8 0.044(3) 0.066(4) 0.044(4) 0.007(3) 0.010(4) -0.006(4) C9 0.043(3) 0.051(3) 0.036(3) 0.002(3) 0.005(3) -0.008(3) C10 0.039(3) 0.071(4) 0.059(4) 0.005(4) 0.005(4) -0.007(4) C11 0.062(4) 0.072(4) 0.084(6) 0.021(4) -0.003(4) 0.013(4) C12 0.046(4) 0.053(3) 0.041(4) 0.006(3) 0.007(3) -0.003(3) C13 0.055(4) 0.052(4) 0.043(4) -0.006(3) -0.004(3) -0.001(3) C14 0.050(3) 0.061(4) 0.050(4) -0.006(3) 0.004(4) -0.007(4) C15 0.058(4) 0.054(4) 0.059(4) -0.002(3) -0.001(4) -0.009(4) C16 0.048(4) 0.064(4) 0.078(5) -0.005(3) 0.006(4) -0.021(4) C17 0.055(4) 0.062(4) 0.124(7) -0.004(4) 0.000(5) -0.010(5) C18 0.075(5) 0.088(5) 0.151(8) -0.029(4) -0.019(7) 0.005(7) #----------------------------------------------------------------------- _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 20.02295 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1140 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0570 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0570 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.600 _refine_ls_shift/esd_max 0.0000 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.21450 _refine_diff_density_max -0.22280 #----------------------------------------------------------------------- _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(5) 1.228(6) ? ? yes O(2) C(1) 1.358(6) ? ? yes O(2) C(9) 1.460(6) ? ? yes O(3) C(7) 1.473(6) ? ? yes O(3) C(10) 1.336(7) ? ? yes O(4) C(10) 1.189(7) ? ? yes O(5) C(12) 1.431(7) ? ? yes C(1) C(2) 1.486(8) ? ? yes C(1) C(6) 1.362(7) ? ? yes C(2) C(3) 1.453(9) ? ? yes C(3) C(4) 1.463(10) ? ? yes C(4) C(5) 1.498(9) ? ? yes C(5) C(6) 1.452(8) ? ? yes C(6) C(7) 1.486(7) ? ? yes C(7) C(8) 1.508(8) ? ? yes C(8) C(9) 1.520(7) ? ? yes C(9) C(12) 1.515(7) ? ? yes C(10) C(11) 1.488(9) ? ? yes C(12) C(13) 1.518(8) ? ? yes C(13) C(14) 1.516(7) ? ? yes C(14) C(15) 1.501(8) ? ? yes C(15) C(16) 1.520(8) ? ? yes C(16) C(17) 1.501(9) ? ? yes C(17) C(18) 1.533(9) ? ? 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) O(2) C(9) 116.0(4) ? ? ? yes C(7) O(3) C(10) 118.0(5) ? ? ? yes O(2) C(1) C(2) 111.9(5) ? ? ? yes O(2) C(1) C(6) 122.5(6) ? ? ? yes C(2) C(1) C(6) 125.6(6) ? ? ? yes C(1) C(2) C(3) 111.8(5) ? ? ? yes C(2) C(3) C(4) 121.5(7) ? ? ? yes C(3) C(4) C(5) 112.8(7) ? ? ? yes O(1) C(5) C(4) 119.6(6) ? ? ? yes O(1) C(5) C(6) 121.1(6) ? ? ? yes C(4) C(5) C(6) 119.3(5) ? ? ? yes C(1) C(6) C(5) 119.1(6) ? ? ? yes C(1) C(6) C(7) 122.1(6) ? ? ? yes C(5) C(6) C(7) 118.7(5) ? ? ? yes O(3) C(7) C(6) 106.1(5) ? ? ? yes O(3) C(7) C(8) 109.2(4) ? ? ? yes C(6) C(7) C(8) 111.1(4) ? ? ? yes C(7) C(8) C(9) 109.1(5) ? ? ? yes O(2) C(9) C(8) 108.9(4) ? ? ? yes O(2) C(9) C(12) 107.2(4) ? ? ? yes C(8) C(9) C(12) 113.8(4) ? ? ? yes O(3) C(10) O(4) 123.4(7) ? ? ? yes O(3) C(10) C(11) 110.9(6) ? ? ? yes O(4) C(10) C(11) 125.7(6) ? ? ? yes O(5) C(12) C(9) 112.1(5) ? ? ? yes O(5) C(12) C(13) 111.8(5) ? ? ? yes C(9) C(12) C(13) 113.4(5) ? ? ? yes C(12) C(13) C(14) 113.6(5) ? ? ? yes C(13) C(14) C(15) 114.2(5) ? ? ? yes C(14) C(15) C(16) 114.9(5) ? ? ? yes C(15) C(16) C(17) 113.4(6) ? ? ? yes C(16) C(17) C(18) 112.7(6) ? ? ? yes #----------------------------------------------------------------------- _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_contact_author ; ENTER NAME ENTER ADDRESS ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_email ' ENTER EMAIL ADDRESS ' loop_ _publ_author_name _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_title ; ENTER SECTION TITLE ; _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 ;