# 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
;