# Copyright The Royal Society of Chemistry, 1998 data_Benzylcyanide_adduct,[2d] #------------------------------------------------------------------------------ _audit_creation_date 'Fri Dec 26 15:04:37 1997' _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 ? _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 11.027(3) _cell_length_b 14.571(3) _cell_length_c 11.562(3) _cell_angle_alpha 90 _cell_angle_beta 93.47(2) _cell_angle_gamma 90 _cell_volume 1854.3(8) _cell_formula_units_Z 2.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22.65 _cell_measurement_theta_max 29.51 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' ' -x,1/2+y, -z' #------------------------------------------------------------------------------ _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange-redplate' _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_measured 'not determined' _exptl_crystal_F000 860.00 _exptl_absorpt_coefficient_mu_cm 5.868 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.939 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source '12 kW rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_\% 2.55 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 3 0 0 1 2 2 1 -1 _diffrn_reflns_number 4653 _diffrn_reflns_av_R_equivalents 2.55 _diffrn_reflns_av_sigmaI/Inet ? _diffrn_reflns_h_min 0 _diffrn_reflns_h_max 14 _diffrn_reflns_k_min 0 _diffrn_reflns_k_max 17 _diffrn_reflns_l_min -6 _diffrn_reflns_l_max 14 _diffrn_theta_min ? _diffrn_theta_max 27.5001 _diffrn_reflns_reduction_process ; Of those 4653 reflections which were collected 4435 were unique (Rint = 0.025). The intensities of three representative reflections were measured after every 150 reflections. No decay correction was applied. The linear absorption coefficient, m, for Mo-Ka radiation is 5.9 cm-1. An empirical absorption correction based on azimuthal scans of several reflections was applied which reulted in transmission factors ranging from 0.94 to 1.00. The data were corrected for Lorentz and polarization effects. ; _diffrn_orient_matrix_11 0.07172 _diffrn_orient_matrix_12 0.01542 _diffrn_orient_matrix_13 0.05355 _diffrn_orient_matrix_21 0.05180 _diffrn_orient_matrix_22 0.00524 _diffrn_orient_matrix_23 -0.06776 _diffrn_orient_matrix_31 -0.02066 _diffrn_orient_matrix_32 0.06667 _diffrn_orient_matrix_33 -0.00706 #------------------------------------------------------------------------------ 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 Fe 0 2 0.346 0.844 'International Tables' P 0 4 0.102 0.094 'International Tables' F 0 24 0.017 0.010 'International Tables' C 0 60 0.003 0.002 'International Tables' N 0 12 0.006 0.003 'International Tables' H 0 72 0.000 0.000 'International Tables' O 0 2 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 Fe1 0.21263(9) 0.0065 0.21106(10) 0.0458 Uij 1 0 P1 0.3510(2) 0.4185(2) 0.9207(3) 0.0670 Uij 1 0 P2 0.8456(3) 0.1804(3) 0.4585(3) 0.0856 Uij 1 0 F1 0.4827(7) 0.4431(8) 0.9224(9) 0.2048 Uij 1 0 F2 0.2176(7) 0.3909(8) 0.9163(8) 0.1717 Uij 1 0 F3 0.382(1) 0.3502(7) 1.0147(9) 0.2017 Uij 1 0 F4 0.317(1) 0.4873(8) 0.8241(9) 0.2233 Uij 1 0 F5 0.3718(9) 0.3451(8) 0.8269(10) 0.2031 Uij 1 0 F6 0.3296(8) 0.4926(6) 1.0091(7) 0.1657 Uij 1 0 F7 0.962(1) 0.215(1) 0.431(1) 0.2787 Uij 1 0 F8 0.734(1) 0.133(2) 0.472(1) 0.3335 Uij 1 0 F9 0.912(2) 0.0931(9) 0.463(1) 0.2943 Uij 1 0 F10 0.800(2) 0.272(1) 0.469(1) 0.3757 Uij 1 0 F11 0.864(1) 0.1806(9) 0.5869(7) 0.2365 Uij 1 0 F12 0.819(1) 0.185(1) 0.3268(8) 0.2283 Uij 1 0 O1 0.277(1) 0.3261(9) 0.344(1) 0.1918 Uij 1 0 N1 0.2463(6) -0.1025(5) 0.1116(6) 0.0501 Uij 1 0 N2 0.3339(7) -0.0543(5) 0.3128(6) 0.0543 Uij 1 0 N3 0.3384(6) 0.0893(5) 0.1672(6) 0.0485 Uij 1 0 N4 0.1202(6) 0.0700(5) 0.0798(6) 0.0510 Uij 1 0 N5 0.1873(6) 0.0921(5) 0.3354(6) 0.0550 Uij 1 0 N6 0.0717(6) -0.0611(5) 0.2634(6) 0.0549 Uij 1 0 C1 0.2098(9) -0.1181(7) -0.0027(9) 0.0645 Uij 1 0 C2 0.229(1) -0.2016(8) -0.0549(9) 0.0803 Uij 1 0 C3 0.284(1) -0.2706(8) 0.007(1) 0.0876 Uij 1 0 C4 0.3196(10) -0.2567(7) 0.121(1) 0.0768 Uij 1 0 C5 0.3009(8) -0.1717(7) 0.1700(9) 0.0600 Uij 1 0 C6 0.3383(9) -0.1536(7) 0.294(1) 0.0749 Uij 1 0 C7 0.4145(8) -0.0107(7) 0.3743(7) 0.0604 Uij 1 0 C8 0.4031(8) 0.0930(7) 0.3671(7) 0.0579 Uij 1 0 C9 0.4137(7) 0.1247(6) 0.2419(8) 0.0565 Uij 1 0 C10 0.3267(8) 0.1156(7) 0.0462(7) 0.0576 Uij 1 0 C11 0.1926(8) 0.1116(6) 0.0067(8) 0.0523 Uij 1 0 C12 0.1478(10) 0.1509(8) -0.0957(8) 0.0727 Uij 1 0 C13 0.027(1) 0.1410(8) -0.1279(10) 0.0905 Uij 1 0 C14 -0.0467(9) 0.0938(8) -0.0511(10) 0.0747 Uij 1 0 C15 0.0019(9) 0.0607(7) 0.0494(9) 0.0661 Uij 1 0 C16 0.5193(9) -0.0510(8) 0.4410(8) 0.0829 Uij 1 0 C17 0.5070(9) 0.1966(8) 0.2201(10) 0.0850 Uij 1 0 C18 0.2757(9) 0.1206(7) 0.4039(8) 0.0637 Uij 1 0 C19 0.2643(9) 0.1644(8) 0.5169(9) 0.0753 Uij 1 0 C20 0.3082(9) 0.0972(8) 0.6123(8) 0.0688 Uij 1 0 C21 0.411(1) 0.1159(8) 0.6811(10) 0.0863 Uij 1 0 C22 0.450(1) 0.050(1) 0.763(1) 0.1039 Uij 1 0 C23 0.396(1) -0.0316(10) 0.771(1) 0.1007 Uij 1 0 C24 0.295(1) -0.0514(10) 0.6997(10) 0.1116 Uij 1 0 C25 0.2538(10) 0.015(1) 0.6229(9) 0.0876 Uij 1 0 C26 -0.0063(8) -0.0929(7) 0.3043(7) 0.0611 Uij 1 0 C27 -0.1086(9) -0.1321(9) 0.3567(10) 0.0899 Uij 1 0 C28 0.119(2) 0.322(1) 0.200(1) 0.1575 Uij 1 0 C29 0.204(2) 0.367(1) 0.288(1) 0.1286 Uij 1 0 C30 0.178(3) 0.458(2) 0.301(2) 0.3676 Uij 1 0 H1 0.1704 -0.0698 -0.0490 0.0734 Uij 0 0 H2 0.2015 -0.2094 -0.1373 0.0896 Uij 0 0 H3 0.2957 -0.3277 -0.0359 0.1060 Uij 0 0 H4 0.3585 -0.3076 0.1663 0.0970 Uij 0 0 H5 0.2853 -0.1858 0.3467 0.0892 Uij 0 0 H6 0.4197 -0.1782 0.3153 0.0892 Uij 0 0 H7 0.4642 0.1243 0.4191 0.0674 Uij 0 0 H8 0.3736 0.0748 0.0001 0.0679 Uij 0 0 H9 0.3584 0.1765 0.0362 0.0679 Uij 0 0 H10 0.2022 0.1846 -0.1439 0.0890 Uij 0 0 H11 -0.0095 0.1658 -0.2023 0.1003 Uij 0 0 H12 -0.1320 0.0836 -0.0746 0.0863 Uij 0 0 H13 -0.0495 0.0309 0.1047 0.0816 Uij 0 0 H14 0.4914 -0.0947 0.4993 0.1030 Uij 0 0 H15 0.5700 -0.0866 0.3929 0.1030 Uij 0 0 H16 0.5669 -0.0066 0.4813 0.1030 Uij 0 0 H17 0.4669 0.2512 0.1895 0.1003 Uij 0 0 H18 0.5613 0.1757 0.1654 0.1003 Uij 0 0 H19 0.5516 0.2130 0.2902 0.1003 Uij 0 0 H20 0.1056 0.1144 0.3452 0.0653 Uij 0 0 H21 0.1801 0.1816 0.5263 0.0877 Uij 0 0 H22 0.3105 0.2206 0.5209 0.0877 Uij 0 0 H23 0.4553 0.1746 0.6733 0.1024 Uij 0 0 H24 0.5277 0.0629 0.8115 0.1200 Uij 0 0 H25 0.4266 -0.0745 0.8310 0.1123 Uij 0 0 H26 0.2548 -0.1136 0.7015 0.1347 Uij 0 0 H27 0.1802 0.0007 0.5713 0.1071 Uij 0 0 H28 -0.1558 -0.1725 0.3055 0.1003 Uij 0 0 H29 -0.0813 -0.1704 0.4237 0.1003 Uij 0 0 H30 -0.1611 -0.0870 0.3849 0.1003 Uij 0 0 H31 0.0589 0.2772 0.2361 0.2026 Uij 0 0 H32 0.1499 0.2890 0.1399 0.2026 Uij 0 0 H33 0.0548 0.3650 0.1599 0.2026 Uij 0 0 H34 0.2690 0.4921 0.2749 0.2655 Uij 0 0 H35 0.1298 0.4937 0.2460 0.2655 Uij 0 0 H36 0.1803 0.4827 0.3734 0.2655 Uij 0 0 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 Fe1 0.0426(6) 0.0465(6) 0.0486(6) 0.0008(7) 0.0057(4) 0.0042(7) P1 0.059(2) 0.063(2) 0.079(2) -0.001(1) 0.004(1) 0.003(2) P2 0.078(2) 0.087(2) 0.090(2) 0.007(2) -0.005(2) -0.008(2) F1 0.089(6) 0.24(1) 0.29(1) -0.066(7) 0.041(7) -0.05(1) F2 0.082(5) 0.26(1) 0.173(9) -0.026(7) 0.006(5) -0.018(9) F3 0.29(1) 0.120(8) 0.183(10) 0.020(8) -0.079(9) 0.070(7) F4 0.33(1) 0.17(1) 0.159(9) -0.06(1) -0.077(9) 0.060(9) F5 0.149(8) 0.24(1) 0.22(1) 0.036(8) -0.003(7) -0.13(1) F6 0.204(8) 0.127(7) 0.160(7) 0.070(7) -0.035(6) -0.067(7) F7 0.128(9) 0.38(2) 0.32(2) -0.03(1) 0.01(1) 0.02(2) F8 0.16(1) 0.53(3) 0.30(2) -0.22(2) -0.04(1) 0.13(2) F9 0.45(3) 0.12(1) 0.33(2) 0.12(1) 0.15(2) 0.02(1) F10 0.65(3) 0.23(1) 0.27(2) 0.29(2) 0.25(2) 0.12(1) F11 0.39(2) 0.22(1) 0.089(6) 0.10(1) -0.043(9) -0.023(8) F12 0.26(1) 0.31(2) 0.106(7) -0.06(1) -0.034(8) 0.025(9) O1 0.20(1) 0.15(1) 0.23(1) 0.00(1) -0.03(1) 0.07(1) N1 0.048(4) 0.043(4) 0.061(5) 0.001(3) 0.017(4) 0.000(4) N2 0.057(5) 0.052(5) 0.055(5) 0.009(4) 0.011(4) 0.012(4) N3 0.039(4) 0.052(4) 0.054(4) -0.006(3) 0.004(3) 0.005(4) N4 0.053(4) 0.048(5) 0.053(4) 0.006(3) 0.004(3) 0.000(4) N5 0.052(4) 0.053(5) 0.060(5) 0.004(4) 0.008(4) 0.007(4) N6 0.044(4) 0.059(5) 0.062(5) -0.006(4) 0.004(4) 0.008(4) C1 0.069(7) 0.061(7) 0.065(7) 0.002(5) 0.020(6) -0.002(5) C2 0.104(9) 0.069(8) 0.072(7) -0.021(7) 0.037(6) -0.015(6) C3 0.089(8) 0.047(6) 0.13(1) -0.010(6) 0.049(8) -0.008(7) C4 0.088(8) 0.042(6) 0.101(9) 0.007(6) 0.021(7) 0.000(6) C5 0.050(5) 0.055(6) 0.075(7) 0.002(5) 0.010(5) 0.009(5) C6 0.067(6) 0.060(7) 0.097(8) 0.002(5) 0.006(6) 0.022(6) C7 0.053(5) 0.080(9) 0.048(5) 0.019(6) 0.000(4) 0.005(5) C8 0.052(5) 0.078(7) 0.043(5) -0.013(5) -0.004(4) 0.003(5) C9 0.050(5) 0.048(5) 0.072(6) -0.006(4) 0.010(5) 0.012(5) C10 0.055(5) 0.069(6) 0.049(5) -0.007(5) 0.007(4) 0.015(5) C11 0.060(6) 0.043(5) 0.053(6) 0.005(5) -0.002(5) 0.008(4) C12 0.088(7) 0.074(7) 0.055(6) -0.007(6) -0.009(5) 0.014(5) C13 0.092(8) 0.078(8) 0.096(9) 0.015(7) -0.036(7) 0.022(7) C14 0.056(6) 0.075(7) 0.090(8) 0.004(6) -0.011(5) 0.017(7) C15 0.063(6) 0.063(6) 0.071(7) 0.016(5) -0.005(5) -0.006(5) C16 0.071(6) 0.104(9) 0.072(7) 0.018(6) -0.017(5) 0.015(6) C17 0.056(6) 0.090(9) 0.109(9) -0.019(6) -0.001(6) 0.004(7) C18 0.074(6) 0.067(7) 0.051(6) 0.001(5) 0.007(5) 0.008(5) C19 0.084(7) 0.074(7) 0.069(7) -0.008(6) 0.009(6) -0.018(6) C20 0.078(7) 0.084(8) 0.046(6) -0.008(6) 0.014(5) -0.018(6) C21 0.103(9) 0.079(8) 0.075(7) -0.014(7) -0.015(6) 0.004(7) C22 0.103(9) 0.14(1) 0.062(8) -0.026(9) -0.018(7) 0.013(8) C23 0.13(1) 0.084(9) 0.088(10) -0.011(8) 0.044(9) 0.021(7) C24 0.15(1) 0.13(1) 0.056(7) -0.07(1) -0.003(8) 0.015(8) C25 0.100(8) 0.100(9) 0.063(6) -0.010(10) 0.006(5) 0.007(9) C26 0.058(6) 0.072(7) 0.052(5) -0.011(5) -0.005(4) 0.010(5) C27 0.064(7) 0.109(10) 0.096(9) -0.033(7) 0.005(6) 0.026(8) C28 0.18(2) 0.18(2) 0.11(1) -0.04(1) -0.03(1) 0.03(1) C29 0.14(1) 0.13(2) 0.11(1) 0.02(1) -0.01(1) 0.05(1) C30 0.71(7) 0.14(2) 0.24(3) 0.18(3) -0.06(4) -0.05(2) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_hydrogen_treatment 'calculated position' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details ; For nonhydrogen atoms. the selected enantiomer has R and Rw of 0.0766 and 0.0780 while the opposite enantiomer has fose of 0.0775 and 0.00789, respectively. ; _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2956 _refine_ls_number_parameters 468 _refine_ls_number_restraints 0 _refine_ls_number_constraints none _refine_ls_R_factor_all none _refine_ls_R_factor_obs 0.0640 _refine_ls_wR_factor_all none _refine_ls_wR_factor_obs 0.0550 _refine_ls_goodness_of_fit_all none _refine_ls_goodness_of_fit_obs 2.040 _refine_ls_shift/esd_max 0.0910 _refine_ls_shift/esd_mean none _refine_diff_density_min 0.38640 _refine_diff_density_max -0.30620 #------------------------------------------------------------------------------ _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 Fe(1) N(1) 2.009(7) ? ? yes Fe(1) N(2) 1.940(7) ? ? yes Fe(1) N(3) 1.929(7) ? ? yes Fe(1) N(4) 2.003(7) ? ? yes Fe(1) N(5) 1.936(7) ? ? yes Fe(1) N(6) 1.966(7) ? ? yes P(1) F(1) 1.495(7) ? ? yes P(1) F(2) 1.522(8) ? ? yes P(1) F(3) 1.498(8) ? ? yes P(1) F(4) 1.530(9) ? ? yes P(1) F(5) 1.550(9) ? ? yes P(1) F(6) 1.515(8) ? ? yes P(2) F(7) 1.43(1) ? ? yes P(2) F(8) 1.430(10) ? ? yes P(2) F(9) 1.47(1) ? ? yes P(2) F(10) 1.43(1) ? ? yes P(2) F(11) 1.486(9) ? ? yes P(2) F(12) 1.534(9) ? ? yes O(1) C(29) 1.17(2) ? ? yes N(1) C(1) 1.38(1) ? ? yes N(1) C(5) 1.34(1) ? ? yes N(2) C(6) 1.46(1) ? ? yes N(2) C(7) 1.27(1) ? ? yes N(3) C(9) 1.271(10) ? ? yes N(3) C(10) 1.45(1) ? ? yes N(4) C(11) 1.34(1) ? ? yes N(4) C(15) 1.34(1) ? ? yes N(5) C(18) 1.29(1) ? ? yes N(6) C(26) 1.108(10) ? ? yes C(1) C(2) 1.38(1) ? ? yes C(2) C(3) 1.35(2) ? ? yes C(3) C(4) 1.37(1) ? ? yes C(4) C(5) 1.38(1) ? ? yes C(5) C(6) 1.49(1) ? ? yes C(7) C(8) 1.52(1) ? ? yes C(7) C(16) 1.47(1) ? ? yes C(8) C(9) 1.53(1) ? ? yes C(8) C(18) 1.55(1) ? ? yes C(9) C(17) 1.50(1) ? ? yes C(10) C(11) 1.52(1) ? ? yes C(11) C(12) 1.38(1) ? ? yes C(12) C(13) 1.37(1) ? ? yes C(13) C(14) 1.42(1) ? ? yes C(14) C(15) 1.34(1) ? ? yes C(18) C(19) 1.47(1) ? ? yes C(19) C(20) 1.53(1) ? ? yes C(20) C(21) 1.37(1) ? ? yes C(20) C(25) 1.35(2) ? ? yes C(21) C(22) 1.40(2) ? ? yes C(22) C(23) 1.34(2) ? ? yes C(23) C(24) 1.38(2) ? ? yes C(24) C(25) 1.37(2) ? ? yes C(26) C(27) 1.43(1) ? ? yes C(28) C(29) 1.50(2) ? ? yes C(29) C(30) 1.37(2) ? ? 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 N(1) Fe(1) N(2) 80.9(3) ? ? ? yes N(1) Fe(1) N(3) 100.6(3) ? ? ? yes N(1) Fe(1) N(4) 92.0(3) ? ? ? yes N(1) Fe(1) N(5) 167.0(3) ? ? ? yes N(1) Fe(1) N(6) 87.5(3) ? ? ? yes N(2) Fe(1) N(3) 88.0(3) ? ? ? yes N(2) Fe(1) N(4) 166.1(3) ? ? ? yes N(2) Fe(1) N(5) 88.2(3) ? ? ? yes N(2) Fe(1) N(6) 96.5(3) ? ? ? yes N(3) Fe(1) N(4) 81.5(3) ? ? ? yes N(3) Fe(1) N(5) 86.0(3) ? ? ? yes N(3) Fe(1) N(6) 171.3(3) ? ? ? yes N(4) Fe(1) N(5) 100.1(3) ? ? ? yes N(4) Fe(1) N(6) 95.1(3) ? ? ? yes N(5) Fe(1) N(6) 86.7(3) ? ? ? yes F(1) P(1) F(2) 178.1(6) ? ? ? yes F(1) P(1) F(3) 88.5(6) ? ? ? yes F(1) P(1) F(4) 92.8(7) ? ? ? yes F(1) P(1) F(5) 89.4(5) ? ? ? yes F(1) P(1) F(6) 90.6(6) ? ? ? yes F(2) P(1) F(3) 91.4(6) ? ? ? yes F(2) P(1) F(4) 87.3(6) ? ? ? yes F(2) P(1) F(5) 88.8(6) ? ? ? yes F(2) P(1) F(6) 91.2(5) ? ? ? yes F(3) P(1) F(4) 178.7(7) ? ? ? yes F(3) P(1) F(5) 90.7(7) ? ? ? yes F(3) P(1) F(6) 91.2(6) ? ? ? yes F(4) P(1) F(5) 89.0(6) ? ? ? yes F(4) P(1) F(6) 89.1(6) ? ? ? yes F(5) P(1) F(6) 178.1(7) ? ? ? yes F(7) P(2) F(8) 170(1) ? ? ? yes F(7) P(2) F(9) 82.1(9) ? ? ? yes F(7) P(2) F(10) 90(1) ? ? ? yes F(7) P(2) F(11) 98.9(9) ? ? ? yes F(7) P(2) F(12) 83.2(7) ? ? ? yes F(8) P(2) F(9) 90(1) ? ? ? yes F(8) P(2) F(10) 97(1) ? ? ? yes F(8) P(2) F(11) 87.4(8) ? ? ? yes F(8) P(2) F(12) 91.0(7) ? ? ? yes F(9) P(2) F(10) 168(1) ? ? ? yes F(9) P(2) F(11) 86.1(8) ? ? ? yes F(9) P(2) F(12) 97.7(9) ? ? ? yes F(10) P(2) F(11) 86.7(8) ? ? ? yes F(10) P(2) F(12) 89.8(9) ? ? ? yes F(11) P(2) F(12) 176.0(8) ? ? ? yes Fe(1) N(1) C(1) 128.8(6) ? ? ? yes Fe(1) N(1) C(5) 113.6(6) ? ? ? yes C(1) N(1) C(5) 117.2(8) ? ? ? yes Fe(1) N(2) C(6) 112.9(7) ? ? ? yes Fe(1) N(2) C(7) 122.9(6) ? ? ? yes C(6) N(2) C(7) 123.1(9) ? ? ? yes Fe(1) N(3) C(9) 121.7(6) ? ? ? yes Fe(1) N(3) C(10) 113.3(5) ? ? ? yes C(9) N(3) C(10) 124.4(7) ? ? ? yes Fe(1) N(4) C(11) 113.0(6) ? ? ? yes Fe(1) N(4) C(15) 126.6(6) ? ? ? yes C(11) N(4) C(15) 119.2(8) ? ? ? yes Fe(1) N(5) C(18) 121.8(6) ? ? ? yes Fe(1) N(6) C(26) 171.7(8) ? ? ? yes N(1) C(1) C(2) 121.4(10) ? ? ? yes C(1) C(2) C(3) 119(1) ? ? ? yes C(2) C(3) C(4) 119(1) ? ? ? yes C(3) C(4) C(5) 119(1) ? ? ? yes N(1) C(5) C(4) 122.8(9) ? ? ? yes N(1) C(5) C(6) 116.3(9) ? ? ? yes C(4) C(5) C(6) 120.9(10) ? ? ? yes N(2) C(6) C(5) 107.9(8) ? ? ? yes N(2) C(7) C(8) 114.4(8) ? ? ? yes N(2) C(7) C(16) 126.4(10) ? ? ? yes C(8) C(7) C(16) 119.0(9) ? ? ? yes C(7) C(8) C(9) 109.9(8) ? ? ? yes C(7) C(8) C(18) 108.5(8) ? ? ? yes C(9) C(8) C(18) 107.7(7) ? ? ? yes N(3) C(9) C(8) 115.8(7) ? ? ? yes N(3) C(9) C(17) 126.6(9) ? ? ? yes C(8) C(9) C(17) 117.5(8) ? ? ? yes N(3) C(10) C(11) 107.9(7) ? ? ? yes N(4) C(11) C(10) 115.6(8) ? ? ? yes N(4) C(11) C(12) 122.2(9) ? ? ? yes C(10) C(11) C(12) 122.2(9) ? ? ? yes C(11) C(12) C(13) 118.8(10) ? ? ? yes C(12) C(13) C(14) 117.8(10) ? ? ? yes C(13) C(14) C(15) 120.3(9) ? ? ? yes N(4) C(15) C(14) 121.6(9) ? ? ? yes N(5) C(18) C(8) 114.4(8) ? ? ? yes N(5) C(18) C(19) 125.9(9) ? ? ? yes C(8) C(18) C(19) 119.1(9) ? ? ? yes C(18) C(19) C(20) 108.9(9) ? ? ? yes C(19) C(20) C(21) 120(1) ? ? ? yes C(19) C(20) C(25) 120.8(10) ? ? ? yes C(21) C(20) C(25) 118(1) ? ? ? yes C(20) C(21) C(22) 117(1) ? ? ? yes C(21) C(22) C(23) 122(1) ? ? ? yes C(22) C(23) C(24) 119(1) ? ? ? yes C(23) C(24) C(25) 117(1) ? ? ? yes C(20) C(25) C(24) 123(1) ? ? ? yes N(6) C(26) C(27) 178(1) ? ? ? yes O(1) C(29) C(28) 122(2) ? ? ? yes O(1) C(29) C(30) 125(2) ? ? ? yes C(28) C(29) C(30) 111(2) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc Dalton Trans.' _publ_contact_author ; ENTER NAME Masafumi Goto ENTER ADDRESS Faculty of Pharmaceutical Sciences, Kumamoto University, Oe-honmachi 5-1, Kumamoto 862, Japan ; _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? _publ_contact_author_phone +81-96-371-4310 _publ_contact_author_fax +81-96-371-4314 _publ_contact_author_email gotomphi@gpo.kumamoto-u.ac.jp loop_ _publ_author_name _publ_author_address 'FIRST AUTHORS NAME Masafumi Goto' ; FIRST AUTHORS ADDRESS Faculty of Pharmaceutical Sciences, Kumamoto University, Oe-honmachi 5-1, Kumamoto 862, Japan ; # = END data_Benzonitrile_adduct,[2e] #------------------------------------------------------------------------------ _audit_creation_date 'Tue Nov 11 13:16:05 1997' _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 ? _computing_structure_refinement 'teXsan: LS (MSC)' _computing_publication_material 'teXsan: FINISH (MSC)' #------------------------------------------------------------------------------ _cell_length_a 13.027(4) _cell_length_b 15.798(3) _cell_length_c 15.667(2) _cell_angle_alpha 90 _cell_angle_beta 94.91(2) _cell_angle_gamma 90 _cell_volume 3212(1) _cell_formula_units_Z 4.00 _cell_measurement_temperature 20.0 _cell_measurement_reflns_used 20 _cell_measurement_theta_min 20.08 _cell_measurement_theta_max 26.13 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz ' +x, +y, +z' '1/2-x,1/2+y,1/2-z' ' -x, -y, -z' '1/2+x,1/2-y,1/2+z' #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.480 _exptl_crystal_F000 1528.00 _exptl_absorpt_coefficient_mu_cm 6.971 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_descript psi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.950 #------------------------------------------------------------------------------ _diffrn_special_details none _diffrn_ambient_temperature 20.0 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoKalpha _diffrn_radiation_source '12 kW rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device 'AFC7R' _diffrn_measurement_method 'omega/2-theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.47 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 1 3 1 0 3 0 -2 3 _diffrn_reflns_number 7981 _diffrn_reflns_av_R_equivalents 3.36 _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 -20 _diffrn_reflns_l_max 20 _diffrn_theta_min ? _diffrn_theta_max 27.4980 _diffrn_reflns_reduction_process ; Of these 7981 reflections which were collected, 7656 were unique (Rint = 0.034). The intensities of three representative reflection were measured after every 150 reflections. No decay correction was applied. The linear absorption coefficient, m, for Mo-Ka radiation is 7.0 cm-1. An empirical absorption correction based on azimuthal scans of several reflections was applied which resulted in transmission factors ranging from 0.95 to 1.00. The data were corrected fo Lorentz and polarization effects. ; _diffrn_orient_matrix_11 -0.02490 _diffrn_orient_matrix_12 -0.03510 _diffrn_orient_matrix_13 0.04718 _diffrn_orient_matrix_21 0.06109 _diffrn_orient_matrix_22 -0.03805 _diffrn_orient_matrix_23 -0.00207 _diffrn_orient_matrix_31 0.03981 _diffrn_orient_matrix_32 0.03643 _diffrn_orient_matrix_33 0.04329 #------------------------------------------------------------------------------ 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 Fe 0 4 0.346 0.844 'International Tables' C 0 120 0.003 0.002 'International Tables' H 0 128 0.000 0.000 'International Tables' N 0 24 0.006 0.003 'International Tables' O 0 34 0.011 0.006 'International Tables' Cl 0 8 0.148 0.159 '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 Fe1 0.15472(6) 0.25893(5) 0.16657(5) 0.0339 Uij 1 0 Cl1 0.8698(2) 0.3255(1) 0.9321(1) 0.0700 Uij 1 0 Cl2 0.2007(1) 0.0174(1) -0.1927(1) 0.0621 Uij 1 0 O1 0.7877(8) 0.3592(6) 0.8810(6) 0.1360 Uij 1 0 O2 0.8525(8) 0.2385(4) 0.9453(5) 0.1048 Uij 1 0 O3 0.949(1) 0.3328(9) 0.877(2) 0.2482 Uij 1 0 O4 0.903(1) 0.3672(6) 0.9995(7) 0.2189 Uij 1 0 O5 0.1676(8) 0.0442(7) -0.1157(5) 0.1237 Uij 1 0 O6 0.1189(5) -0.0295(5) -0.2395(5) 0.1008 Uij 1 0 O7 0.2872(6) -0.0358(5) -0.1805(6) 0.1165 Uij 1 0 O8 0.2251(6) 0.0915(4) -0.2404(5) 0.0919 Uij 1 0 O9 0.057(2) -0.049(3) 0.422(2) 0.2336 Uij 1 0 N1 0.1858(4) 0.2852(3) 0.0452(3) 0.0441 Uij 1 0 N2 0.1082(4) 0.3740(3) 0.1587(3) 0.0392 Uij 1 0 N3 0.0154(4) 0.2228(3) 0.1412(3) 0.0371 Uij 1 0 N4 0.1792(4) 0.1353(3) 0.1557(3) 0.0379 Uij 1 0 N5 0.1251(4) 0.2600(3) 0.2854(3) 0.0381 Uij 1 0 N6 0.2977(5) 0.2881(3) 0.2010(4) 0.0479 Uij 1 0 C1 0.2055(6) 0.2316(4) -0.0185(4) 0.0519 Uij 1 0 C2 0.2306(8) 0.2593(6) -0.0977(5) 0.0702 Uij 1 0 C3 0.2400(8) 0.3447(6) -0.1114(5) 0.0701 Uij 1 0 C4 0.2197(7) 0.4015(5) -0.0470(5) 0.0602 Uij 1 0 C5 0.1905(5) 0.3692(4) 0.0298(4) 0.0441 Uij 1 0 C6 0.1638(6) 0.4249(4) 0.0989(5) 0.0530 Uij 1 0 C7 0.0245(5) 0.3976(4) 0.1871(4) 0.0411 Uij 1 0 C8 -0.0299(5) 0.3307(4) 0.2357(4) 0.0401 Uij 1 0 C9 -0.0592(5) 0.2565(4) 0.1758(4) 0.0385 Uij 1 0 C10 0.0060(5) 0.1450(4) 0.0919(4) 0.0459 Uij 1 0 C11 0.0992(5) 0.0927(4) 0.1170(4) 0.0384 Uij 1 0 C12 0.1035(6) 0.0075(4) 0.1008(4) 0.0533 Uij 1 0 C13 0.1953(8) -0.0358(5) 0.1227(5) 0.0645 Uij 1 0 C14 0.2751(7) 0.0065(5) 0.1618(5) 0.0619 Uij 1 0 C15 0.2670(6) 0.0918(4) 0.1792(4) 0.0474 Uij 1 0 C16 -0.0289(6) 0.4821(5) 0.1750(5) 0.0661 Uij 1 0 C17 -0.1709(5) 0.2331(4) 0.1641(4) 0.0479 Uij 1 0 C18 0.0460(5) 0.2979(4) 0.3098(4) 0.0413 Uij 1 0 C19 0.0273(5) 0.3183(5) 0.3982(4) 0.0453 Uij 1 0 C20 0.0864(8) 0.278(1) 0.4661(6) 0.1300 Uij 1 0 C21 0.0742(9) 0.303(1) 0.5490(6) 0.1598 Uij 1 0 C22 0.0033(8) 0.3638(9) 0.5681(6) 0.0965 Uij 1 0 C23 -0.0566(8) 0.4013(7) 0.5024(6) 0.0856 Uij 1 0 C24 -0.0418(7) 0.3783(6) 0.4200(5) 0.0689 Uij 1 0 C25 0.3799(6) 0.3053(5) 0.2253(5) 0.0541 Uij 1 0 C26 0.4849(7) 0.3304(10) 0.2540(8) 0.1080 Uij 1 0 C27 0.077(3) 0.043(3) 0.452(3) 0.2336 Uij 1 0 C28 0.033(3) 0.054(3) 0.540(3) 0.2336 Uij 1 0 C29 -0.014(3) -0.031(3) 0.564(2) 0.2336 Uij 1 0 C30 0.000(3) -0.095(2) 0.491(3) 0.2336 Uij 1 0 H1 0.1990 0.1721 -0.0086 0.0615 Uiso 0 0 H2 0.2432 0.2194 -0.1415 0.0851 Uiso 0 0 H3 0.2615 0.3660 -0.1644 0.0847 Uiso 0 0 H4 0.2255 0.4610 -0.0555 0.0710 Uiso 0 0 H5 0.1214 0.4703 0.0753 0.0626 Uiso 0 0 H6 0.2251 0.4490 0.1269 0.0626 Uiso 0 0 H7 -0.0901 0.3539 0.2573 0.0493 Uiso 0 0 H8 -0.0549 0.1149 0.1034 0.0573 Uiso 0 0 H9 0.0022 0.1573 0.0317 0.0573 Uiso 0 0 H10 0.0437 -0.0218 0.0751 0.0671 Uiso 0 0 H11 0.1999 -0.0948 0.1110 0.0777 Uiso 0 0 H12 0.3398 -0.0219 0.1762 0.0729 Uiso 0 0 H13 0.3237 0.1211 0.2091 0.0572 Uiso 0 0 H14 0.0157 0.5253 0.1999 0.0815 Uiso 0 0 H15 -0.0433 0.4933 0.1158 0.0815 Uiso 0 0 H16 -0.0906 0.4816 0.2026 0.0815 Uiso 0 0 H17 -0.2096 0.2687 0.1982 0.0580 Uiso 0 0 H18 -0.1957 0.2386 0.1057 0.0580 Uiso 0 0 H19 -0.1797 0.1755 0.1815 0.0580 Uiso 0 0 H20 0.1699 0.2307 0.3270 0.0453 Uiso 0 0 H21 0.1401 0.2408 0.4558 0.1565 Uiso 0 0 H22 0.1146 0.2750 0.5938 0.1798 Uiso 0 0 H23 -0.0052 0.3761 0.6273 0.1160 Uiso 0 0 H24 -0.1055 0.4450 0.5134 0.0992 Uiso 0 0 H25 -0.0847 0.4047 0.3739 0.0825 Uiso 0 0 H26 0.5240 0.2797 0.2731 0.1314 Uiso 0 0 H27 0.5177 0.3564 0.2109 0.1314 Uiso 0 0 H28 0.4843 0.3664 0.3031 0.1314 Uiso 0 0 H29 0.160(3) 0.056(4) 0.458(4) 0.2336 Uiso 0 0 H30 0.038(4) 0.087(3) 0.405(3) 0.2336 Uiso 0 0 H31 -0.027(4) 0.103(3) 0.535(4) 0.2336 Uiso 0 0 H32 0.095(4) 0.072(4) 0.588(3) 0.2336 Uiso 0 0 H33 -0.097(3) -0.023(4) 0.572(3) 0.2336 Uiso 0 0 H34 0.025(4) -0.055(4) 0.624(2) 0.2336 Uiso 0 0 H35 -0.075(3) -0.118(3) 0.464(4) 0.2336 Uiso 0 0 H36 0.047(4) -0.149(2) 0.517(4) 0.2336 Uiso 0 0 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 Fe1 0.0382(5) 0.0286(4) 0.0350(4) -0.0005(3) 0.0038(3) -0.0009(3) Cl1 0.074(1) 0.0464(10) 0.084(1) -0.0161(9) -0.026(1) 0.0123(9) Cl2 0.054(1) 0.052(1) 0.082(1) -0.0067(8) 0.0113(9) 0.0027(9) O1 0.176(9) 0.086(6) 0.129(7) -0.008(6) -0.084(6) 0.013(5) O2 0.161(8) 0.040(3) 0.108(5) -0.018(4) -0.022(5) 0.011(3) O3 0.130(9) 0.16(1) 0.47(3) -0.062(9) 0.13(1) -0.04(2) O4 0.41(2) 0.079(6) 0.132(8) -0.040(9) -0.17(1) 0.002(5) O5 0.153(8) 0.136(8) 0.090(5) -0.040(6) 0.057(5) -0.028(5) O6 0.082(5) 0.087(5) 0.128(6) -0.030(4) -0.024(4) 0.001(4) O7 0.069(4) 0.091(5) 0.188(8) 0.016(4) 0.002(5) 0.036(6) O8 0.089(5) 0.067(4) 0.121(5) -0.012(3) 0.021(4) 0.025(4) N1 0.053(3) 0.036(3) 0.043(3) -0.001(2) 0.004(2) -0.001(2) N2 0.039(3) 0.035(2) 0.043(3) -0.005(2) 0.000(2) -0.001(2) N3 0.037(2) 0.034(3) 0.039(2) -0.005(2) -0.004(2) -0.004(2) N4 0.050(3) 0.032(2) 0.032(2) 0.003(2) 0.004(2) 0.003(2) N5 0.032(2) 0.047(3) 0.034(2) -0.002(2) -0.002(2) 0.000(2) N6 0.054(3) 0.042(3) 0.048(3) -0.007(3) 0.008(3) -0.007(2) C1 0.074(5) 0.040(3) 0.043(3) 0.000(3) 0.014(3) 0.001(3) C2 0.098(7) 0.063(5) 0.054(4) 0.005(5) 0.029(4) -0.006(4) C3 0.098(6) 0.061(5) 0.054(4) -0.001(5) 0.028(4) 0.012(4) C4 0.083(6) 0.050(4) 0.049(4) 0.004(4) 0.011(4) 0.013(3) C5 0.042(3) 0.039(3) 0.052(4) -0.003(3) 0.006(3) 0.001(3) C6 0.070(5) 0.038(3) 0.052(4) 0.000(3) 0.010(3) 0.001(3) C7 0.053(4) 0.031(3) 0.038(3) -0.001(3) 0.000(3) -0.009(2) C8 0.036(3) 0.047(3) 0.037(3) 0.012(3) 0.007(2) -0.007(2) C9 0.036(3) 0.039(3) 0.039(3) -0.001(2) -0.004(2) 0.003(2) C10 0.051(4) 0.031(3) 0.055(4) -0.003(3) -0.002(3) -0.003(3) C11 0.051(4) 0.033(3) 0.031(3) -0.001(2) 0.003(2) 0.003(2) C12 0.068(5) 0.035(3) 0.056(4) 0.000(3) -0.001(3) -0.001(3) C13 0.109(7) 0.036(3) 0.050(4) 0.006(4) 0.012(4) -0.011(3) C14 0.080(5) 0.042(4) 0.064(5) 0.024(4) 0.005(4) 0.006(3) C15 0.058(4) 0.039(3) 0.046(3) 0.001(3) 0.001(3) -0.002(3) C16 0.066(5) 0.049(4) 0.082(6) 0.016(4) 0.001(4) 0.004(4) C17 0.042(3) 0.053(4) 0.049(3) -0.004(3) 0.007(3) -0.004(3) C18 0.041(3) 0.046(3) 0.038(3) 0.002(3) 0.005(2) 0.004(2) C19 0.040(3) 0.063(4) 0.033(3) -0.001(3) 0.001(3) -0.005(3) C20 0.064(6) 0.27(2) 0.054(5) 0.083(9) 0.009(4) 0.014(7) C21 0.073(7) 0.36(3) 0.045(5) 0.08(1) 0.001(5) 0.005(9) C22 0.064(5) 0.18(1) 0.050(5) -0.014(6) 0.014(4) -0.038(6) C23 0.080(6) 0.107(8) 0.073(6) 0.002(5) 0.028(5) -0.039(5) C24 0.083(6) 0.069(5) 0.057(4) 0.012(4) 0.017(4) -0.011(4) C25 0.047(4) 0.054(4) 0.060(4) -0.011(3) 0.001(3) -0.010(3) C26 0.040(5) 0.16(1) 0.126(9) -0.022(6) -0.003(5) -0.032(8) #------------------------------------------------------------------------------ _refine_special_details ? _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_hydrogen_treatment 'calculated position' _refine_ls_extinction_method Zachariasen_type_2_Gaussian_isotropic _refine_ls_extinction_coef 0.00000 _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack none _refine_ls_number_reflns 3773 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_number_constraints 'rigid group method was applied for thf' _refine_ls_R_factor_obs 0.0640 _refine_ls_wR_factor_obs 0.1180 _refine_ls_goodness_of_fit_obs 0.110 _refine_ls_shift/esd_max 0.0430 _refine_diff_density_min 0.87140 _refine_diff_density_max -0.59740 #------------------------------------------------------------------------------ _geom_special_details none 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 Fe(1) N(1) 2.021(5) ? ? yes Fe(1) N(2) 1.917(5) ? ? yes Fe(1) N(3) 1.912(5) ? ? yes Fe(1) N(4) 1.989(5) ? ? yes Fe(1) N(5) 1.934(5) ? ? yes Fe(1) N(6) 1.950(6) ? ? yes Cl(1) O(1) 1.39(1) ? ? yes Cl(1) O(2) 1.411(7) ? ? yes Cl(1) O(3) 1.40(2) ? ? yes Cl(1) O(4) 1.29(1) ? ? yes Cl(2) O(5) 1.381(9) ? ? yes Cl(2) O(6) 1.446(7) ? ? yes Cl(2) O(7) 1.406(8) ? ? yes Cl(2) O(8) 1.439(8) ? ? yes N(1) C(1) 1.350(9) ? ? yes N(1) C(5) 1.350(8) ? ? yes N(2) C(6) 1.472(9) ? ? yes N(2) C(7) 1.268(9) ? ? yes N(3) C(9) 1.270(8) ? ? yes N(3) C(10) 1.451(8) ? ? yes N(4) C(11) 1.342(8) ? ? yes N(4) C(15) 1.357(9) ? ? yes N(5) C(18) 1.279(8) ? ? yes N(6) C(25) 1.138(9) ? ? yes C(1) C(2) 1.38(1) ? ? yes C(2) C(3) 1.37(1) ? ? yes C(3) C(4) 1.39(1) ? ? yes C(4) C(5) 1.39(1) ? ? yes C(5) C(6) 1.461(10) ? ? yes C(7) C(8) 1.514(9) ? ? yes C(7) C(16) 1.51(1) ? ? yes C(8) C(9) 1.529(8) ? ? yes C(8) C(18) 1.548(8) ? ? yes C(9) C(17) 1.497(9) ? ? yes C(10) C(11) 1.493(9) ? ? yes C(11) C(12) 1.371(9) ? ? yes C(12) C(13) 1.40(1) ? ? yes C(13) C(14) 1.34(1) ? ? yes C(14) C(15) 1.382(10) ? ? yes C(18) C(19) 1.462(9) ? ? yes C(19) C(20) 1.41(1) ? ? yes C(19) C(24) 1.37(1) ? ? yes C(20) C(21) 1.38(2) ? ? yes C(21) C(22) 1.38(2) ? ? yes C(22) C(23) 1.37(1) ? ? yes C(23) C(24) 1.37(1) ? ? yes C(25) C(26) 1.46(1) ? ? yes O(9) C(27) 1.54(6) ? ? yes O(9) C(28) 1.35(5) ? ? yes O(9) C(29) 1.40(6) ? ? yes O(9) C(30) 1.54(5) ? ? yes C(27) C(28) 1.54(6) ? ? yes C(27) C(29) 0.85(5) ? ? yes C(27) C(30) 1.62(6) ? ? yes C(28) C(29) 1.54(6) ? ? yes C(28) C(29) 1.66(5) ? ? yes C(28) C(30) 0.90(5) ? ? yes C(29) C(30) 1.54(6) ? ? 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 N(1) Fe(1) N(2) 80.4(2) ? ? ? yes N(1) Fe(1) N(3) 97.4(2) ? ? ? yes N(1) Fe(1) N(4) 94.3(2) ? ? ? yes N(1) Fe(1) N(5) 167.6(2) ? ? ? yes N(1) Fe(1) N(6) 87.0(2) ? ? ? yes N(2) Fe(1) N(3) 88.9(2) ? ? ? yes N(2) Fe(1) N(4) 168.0(2) ? ? ? yes N(2) Fe(1) N(5) 88.0(2) ? ? ? yes N(2) Fe(1) N(6) 94.8(2) ? ? ? yes N(3) Fe(1) N(4) 81.1(2) ? ? ? yes N(3) Fe(1) N(5) 86.5(2) ? ? ? yes N(3) Fe(1) N(6) 174.7(2) ? ? ? yes N(4) Fe(1) N(5) 97.9(2) ? ? ? yes N(4) Fe(1) N(6) 95.7(2) ? ? ? yes N(5) Fe(1) N(6) 89.7(2) ? ? ? yes O(1) Cl(1) O(2) 109.5(6) ? ? ? yes O(1) Cl(1) O(3) 100.8(9) ? ? ? yes O(1) Cl(1) O(4) 117.7(8) ? ? ? yes O(2) Cl(1) O(3) 107.8(7) ? ? ? yes O(2) Cl(1) O(4) 115.2(6) ? ? ? yes O(3) Cl(1) O(4) 104(1) ? ? ? yes O(5) Cl(2) O(6) 109.2(5) ? ? ? yes O(5) Cl(2) O(7) 111.8(6) ? ? ? yes O(5) Cl(2) O(8) 107.6(5) ? ? ? yes O(6) Cl(2) O(7) 108.0(5) ? ? ? yes O(6) Cl(2) O(8) 109.9(4) ? ? ? yes O(7) Cl(2) O(8) 110.3(5) ? ? ? yes Fe(1) N(1) C(1) 129.3(4) ? ? ? yes Fe(1) N(1) C(5) 112.7(4) ? ? ? yes C(1) N(1) C(5) 118.0(6) ? ? ? yes Fe(1) N(2) C(6) 112.9(4) ? ? ? yes Fe(1) N(2) C(7) 122.2(4) ? ? ? yes C(6) N(2) C(7) 123.2(5) ? ? ? yes Fe(1) N(3) C(9) 122.2(4) ? ? ? yes Fe(1) N(3) C(10) 113.5(4) ? ? ? yes C(9) N(3) C(10) 123.3(5) ? ? ? yes Fe(1) N(4) C(11) 114.0(4) ? ? ? yes Fe(1) N(4) C(15) 127.7(4) ? ? ? yes C(11) N(4) C(15) 118.2(5) ? ? ? yes Fe(1) N(5) C(18) 121.6(4) ? ? ? yes Fe(1) N(6) C(25) 176.6(6) ? ? ? yes N(1) C(1) C(2) 122.7(7) ? ? ? yes C(1) C(2) C(3) 118.9(8) ? ? ? yes C(2) C(3) C(4) 119.6(8) ? ? ? yes C(3) C(4) C(5) 118.3(7) ? ? ? yes N(1) C(5) C(4) 122.4(6) ? ? ? yes N(1) C(5) C(6) 116.2(6) ? ? ? yes C(4) C(5) C(6) 121.4(6) ? ? ? yes N(2) C(6) C(5) 107.7(5) ? ? ? yes N(2) C(7) C(8) 115.1(5) ? ? ? yes N(2) C(7) C(16) 128.1(6) ? ? ? yes C(8) C(7) C(16) 116.7(6) ? ? ? yes C(7) C(8) C(9) 109.3(5) ? ? ? yes C(7) C(8) C(18) 108.4(5) ? ? ? yes C(9) C(8) C(18) 108.3(5) ? ? ? yes N(3) C(9) C(8) 115.0(5) ? ? ? yes N(3) C(9) C(17) 128.0(6) ? ? ? yes C(8) C(9) C(17) 117.0(5) ? ? ? yes N(3) C(10) C(11) 107.4(5) ? ? ? yes N(4) C(11) C(10) 115.1(5) ? ? ? yes N(4) C(11) C(12) 122.3(6) ? ? ? yes C(10) C(11) C(12) 122.6(6) ? ? ? yes C(11) C(12) C(13) 118.8(7) ? ? ? yes C(12) C(13) C(14) 119.0(7) ? ? ? yes C(13) C(14) C(15) 120.5(8) ? ? ? yes N(4) C(15) C(14) 121.1(6) ? ? ? yes N(5) C(18) C(8) 114.3(5) ? ? ? yes N(5) C(18) C(19) 126.2(5) ? ? ? yes C(8) C(18) C(19) 119.3(5) ? ? ? yes C(18) C(19) C(20) 119.4(7) ? ? ? yes C(18) C(19) C(24) 123.7(6) ? ? ? yes C(20) C(19) C(24) 116.8(8) ? ? ? yes C(19) C(20) C(21) 118(1) ? ? ? yes C(20) C(21) C(22) 122(1) ? ? ? yes C(21) C(22) C(23) 119.0(9) ? ? ? yes C(22) C(23) C(24) 118.4(10) ? ? ? yes C(19) C(24) C(23) 124.5(8) ? ? ? yes N(6) C(25) C(26) 177.6(9) ? ? ? yes C(27) O(9) C(28) 92(3) ? ? ? yes C(27) O(9) C(29) 33(2) ? ? ? yes C(27) O(9) C(30) 108(2) ? ? ? yes C(28) O(9) C(29) 67(2) ? ? ? yes C(28) O(9) C(30) 35(2) ? ? ? yes C(29) O(9) C(30) 95(2) ? ? ? yes O(9) C(27) C(28) 108(3) ? ? ? yes O(9) C(27) C(29) 64(4) ? ? ? yes O(9) C(27) C(30) 123(2) ? ? ? yes C(28) C(27) C(29) 82(4) ? ? ? yes C(28) C(27) C(30) 32(2) ? ? ? yes C(29) C(27) C(30) 69(3) ? ? ? yes O(9) C(28) C(27) 141(3) ? ? ? yes O(9) C(28) C(29) 57(2) ? ? ? yes O(9) C(28) C(29) 111(3) ? ? ? yes O(9) C(28) C(30) 83(4) ? ? ? yes C(27) C(28) C(29) 107(3) ? ? ? yes C(27) C(28) C(29) 30(2) ? ? ? yes C(27) C(28) C(30) 78(4) ? ? ? yes C(29) C(28) C(29) 91(2) ? ? ? yes C(29) C(28) C(30) 125(4) ? ? ? yes C(29) C(28) C(30) 66(3) ? ? ? yes O(9) C(29) C(27) 82(4) ? ? ? yes O(9) C(29) C(28) 54(2) ? ? ? yes O(9) C(29) C(28) 108(2) ? ? ? yes O(9) C(29) C(30) 140(3) ? ? ? yes C(27) C(29) C(28) 120(4) ? ? ? yes C(27) C(29) C(28) 66(3) ? ? ? yes C(27) C(29) C(30) 79(4) ? ? ? yes C(28) C(29) C(28) 88(2) ? ? ? yes C(28) C(29) C(30) 107(3) ? ? ? yes C(28) C(29) C(30) 32(2) ? ? ? yes O(9) C(30) C(27) 120(2) ? ? ? yes O(9) C(30) C(28) 60(3) ? ? ? yes O(9) C(30) C(29) 107(2) ? ? ? yes C(27) C(30) C(28) 68(3) ? ? ? yes C(27) C(30) C(29) 31(2) ? ? ? yes C(28) C(30) C(29) 81(3) ? ? ? yes #------------------------------------------------------------------------------ _publ_requested_journal 'J. Chem. Soc. Dalton Trans.' _publ_contact_author ; ENTER NAME Masafumi Goto ENTER ADDRESS Faculty of Pharmaceutical Sciences, Kumamoto University, Oe-honmachi 5-1, Kumamoto 862, Japan ; _publ_contact_author_phone +81-96-371-4310 _publ_contact_author_fax +81-96-371-4314 _publ_contact_author_email gotomphi@gpo.kumamoto-u.ac.jp loop_ _publ_author_name _publ_author_address 'FIRST AUTHORS NAME Masafumi Goto' ; FIRST AUTHORS ADDRESS Faculty of Pharmaceutical Sciences, Kumamoto University, Oe-honmachi 5-1, Kumamoto 862, Japan ;