# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 207/336 data_master #------------------------------------------------------------------------------ _audit_creation_date 'Tue Jun 23 11:43:42 1998' _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 9.405(3) _cell_length_b 9.677(4) _cell_length_c 8.158(4) _cell_angle_alpha 107.91(4) _cell_angle_beta 100.72(3) _cell_angle_gamma 106.76(3) _cell_volume 645.0(5) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 21 _cell_measurement_theta_min 18.43 _cell_measurement_theta_max 24.69 #------------------------------------------------------------------------------ _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 '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 1.335 _exptl_crystal_density_measured ? _exptl_crystal_F000 276.00 _exptl_absorpt_coefficient_mu_cm 0.930 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.957 #------------------------------------------------------------------------------ _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_\% -0.61 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l ? ? ? ? ? ? ? ? ? _diffrn_reflns_number 2433 _diffrn_reflns_av_R_equivalents 3.40 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 11 _diffrn_reflns_k_min -3 _diffrn_reflns_k_max 3 _diffrn_reflns_l_min -8 _diffrn_reflns_l_max 0 _diffrn_theta_min ? _diffrn_theta_max 24.9969 _diffrn_reflns_reduction_process ? _diffrn_orient_matrix_11 -0.10014 _diffrn_orient_matrix_12 0.00356 _diffrn_orient_matrix_13 0.02230 _diffrn_orient_matrix_21 0.05666 _diffrn_orient_matrix_22 0.10867 _diffrn_orient_matrix_23 0.09277 _diffrn_orient_matrix_31 -0.01799 _diffrn_orient_matrix_32 0.04286 _diffrn_orient_matrix_33 -0.09566 #------------------------------------------------------------------------------ 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 30 0.003 0.002 'International Tables' H 0 34 0.000 0.000 'International Tables' O 0 6 0.011 0.006 'International Tables' N 0 2 0.006 0.003 '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 -0.2082(3) 0.3932(3) 0.2848(3) 0.0466 Uij ? ? O2 -0.3413(3) 0.4031(2) -0.2988(3) 0.0391 Uij ? ? O3 -0.3525(3) 0.2141(3) -0.5535(3) 0.0570 Uij ? ? N -0.2583(3) 0.6004(3) 0.2515(3) 0.0349 Uij ? ? C1 -0.2954(3) 0.6802(3) 0.1434(4) 0.0315 Uij ? ? C2 -0.2982(4) 0.8306(4) 0.2170(4) 0.0404 Uij ? ? C3 -0.3370(4) 0.9042(4) 0.1062(5) 0.0442 Uij ? ? C4 -0.3757(4) 0.8329(4) -0.0792(4) 0.0406 Uij ? ? C5 -0.3713(4) 0.6860(4) -0.1541(4) 0.0360 Uij ? ? C6 -0.3292(3) 0.6092(3) -0.0444(4) 0.0287 Uij ? ? C7 -0.3120(4) 0.4610(3) -0.1167(4) 0.0289 Uij ? ? C8 -0.2663(3) 0.3896(3) -0.0087(4) 0.0307 Uij ? ? C9 -0.2423(4) 0.4581(4) 0.1815(4) 0.0342 Uij ? ? C10 -0.2476(4) 0.2343(4) -0.0849(4) 0.0359 Uij ? ? C11 -0.3211(4) 0.1615(4) -0.2883(4) 0.0402 Uij ? ? C12 -0.2815(4) 0.2803(4) -0.3717(4) 0.0390 Uij ? ? C13 -0.2394(4) 0.6664(4) 0.4472(4) 0.0450 Uij ? ? C14 -0.0756(5) 0.7801(5) 0.5576(5) 0.0699 Uij ? ? C15 -0.0763(4) 0.2525(4) -0.0303(5) 0.0549 Uij ? ? H1 -0.2765 0.8783 0.3412 0.0625 Uij ? ? H2 -0.3353 0.9998 0.1597 0.0625 Uij ? ? H3 -0.4135 0.8804 -0.1637 0.0625 Uij ? ? H4 -0.3963 0.6375 -0.2804 0.0625 Uij ? ? H5 -0.3048 0.1702 -0.0277 0.0625 Uij ? ? H6 -0.2821 0.0755 -0.3411 0.0625 Uij ? ? H7 -0.4298 0.1172 -0.3193 0.0625 Uij ? ? H8 -0.1617 0.3410 -0.3593 0.0625 Uij ? ? H9 -0.2718 0.5759 0.4874 0.0625 Uij ? ? H10 -0.3168 0.7186 0.4638 0.0625 Uij ? ? H11 -0.0455 0.8543 0.4959 0.0625 Uij ? ? H12 -0.0768 0.8175 0.6878 0.0625 Uij ? ? H13 -0.0133 0.7223 0.5567 0.0625 Uij ? ? H14 -0.0248 0.3065 0.1150 0.0625 Uij ? ? H15 -0.0708 0.1549 -0.0650 0.0625 Uij ? ? H16 -0.0203 0.3086 -0.1009 0.0625 Uij ? ? H17 -0.3075 0.2778 -0.6148 0.0625 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 0.063(2) 0.049(1) 0.040(1) 0.028(1) 0.017(1) 0.026(1) O2 0.058(2) 0.035(1) 0.029(1) 0.024(1) 0.015(1) 0.011(1) O3 0.089(2) 0.038(1) 0.037(2) 0.016(1) 0.022(1) 0.010(1) N 0.041(2) 0.037(2) 0.029(2) 0.016(1) 0.012(1) 0.012(1) C1 0.028(2) 0.033(2) 0.032(2) 0.010(2) 0.008(2) 0.012(2) C2 0.049(2) 0.037(2) 0.032(2) 0.017(2) 0.013(2) 0.008(2) C3 0.056(2) 0.031(2) 0.047(2) 0.020(2) 0.018(2) 0.012(2) C4 0.051(2) 0.034(2) 0.044(2) 0.023(2) 0.015(2) 0.017(2) C5 0.042(2) 0.033(2) 0.033(2) 0.015(2) 0.010(2) 0.013(2) C6 0.030(2) 0.027(2) 0.030(2) 0.010(1) 0.011(2) 0.011(1) C7 0.029(2) 0.027(2) 0.029(2) 0.008(1) 0.012(1) 0.009(1) C8 0.032(2) 0.027(2) 0.035(2) 0.010(1) 0.013(2) 0.014(2) C9 0.035(2) 0.036(2) 0.035(2) 0.012(2) 0.011(2) 0.018(2) C10 0.044(2) 0.029(2) 0.042(2) 0.016(2) 0.018(2) 0.016(2) C11 0.048(2) 0.028(2) 0.043(2) 0.014(2) 0.016(2) 0.011(2) C12 0.058(2) 0.029(2) 0.030(2) 0.017(2) 0.018(2) 0.007(2) C13 0.063(3) 0.051(2) 0.024(2) 0.026(2) 0.017(2) 0.013(2) C14 0.077(3) 0.082(3) 0.035(2) 0.030(3) 0.001(2) 0.011(2) C15 0.055(3) 0.054(2) 0.063(3) 0.032(2) 0.015(2) 0.023(2) #------------------------------------------------------------------------------ _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 5.98420 _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 1242 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_R_factor_all ? _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_obs 0.0500 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_obs 1.500 _refine_ls_shift/esd_max 0.0020 _refine_ls_shift/esd_mean ? _refine_diff_density_min 0.23830 _refine_diff_density_max -0.17810 #------------------------------------------------------------------------------ _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(9) 1.244(4) ? ? yes O(2) C(7) 1.358(4) ? ? yes O(2) C(12) 1.469(4) ? ? yes O(3) C(12) 1.362(4) ? ? yes N C(1) 1.398(4) ? ? yes N C(9) 1.383(4) ? ? yes N C(13) 1.480(4) ? ? yes C(1) C(2) 1.403(4) ? ? yes C(1) C(6) 1.402(4) ? ? yes C(2) C(3) 1.371(4) ? ? yes C(3) C(4) 1.380(5) ? ? yes C(4) C(5) 1.380(4) ? ? yes C(5) C(6) 1.398(4) ? ? yes C(6) C(7) 1.442(4) ? ? yes C(7) C(8) 1.358(4) ? ? yes C(8) C(9) 1.432(4) ? ? yes C(8) C(10) 1.515(4) ? ? yes C(10) C(11) 1.517(4) ? ? yes C(10) C(15) 1.531(5) ? ? yes C(11) C(12) 1.501(4) ? ? yes C(13) C(14) 1.514(5) ? ? 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(7) O(2) C(12) 115.9(2) ? ? ? yes C(1) N C(9) 122.3(3) ? ? ? yes C(1) N C(13) 119.7(3) ? ? ? yes C(9) N C(13) 117.9(3) ? ? ? yes N C(1) C(2) 122.1(3) ? ? ? yes N C(1) C(6) 119.3(3) ? ? ? yes C(2) C(1) C(6) 118.6(3) ? ? ? yes C(1) C(2) C(3) 120.3(3) ? ? ? yes C(2) C(3) C(4) 121.4(3) ? ? ? yes C(3) C(4) C(5) 119.2(3) ? ? ? yes C(4) C(5) C(6) 120.8(3) ? ? ? yes C(1) C(6) C(5) 119.7(3) ? ? ? yes C(1) C(6) C(7) 118.0(3) ? ? ? yes C(5) C(6) C(7) 122.3(3) ? ? ? yes O(2) C(7) C(6) 114.3(3) ? ? ? yes O(2) C(7) C(8) 123.8(3) ? ? ? yes C(6) C(7) C(8) 121.9(3) ? ? ? yes C(7) C(8) C(9) 119.6(3) ? ? ? yes C(7) C(8) C(10) 121.8(3) ? ? ? yes C(9) C(8) C(10) 118.5(3) ? ? ? yes O(1) C(9) N 119.3(3) ? ? ? yes O(1) C(9) C(8) 122.0(3) ? ? ? yes N C(9) C(8) 118.7(3) ? ? ? yes C(8) C(10) C(11) 109.7(3) ? ? ? yes C(8) C(10) C(15) 111.2(3) ? ? ? yes C(11) C(10) C(15) 112.1(3) ? ? ? yes C(10) C(11) C(12) 111.5(3) ? ? ? yes O(2) C(12) O(3) 106.4(3) ? ? ? yes O(2) C(12) C(11) 109.5(3) ? ? ? yes O(3) C(12) C(11) 110.7(3) ? ? ? yes N C(13) C(14) 112.9(3) ? ? ? 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 ;