# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rao02 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; rao02 ; # start Validation Reply Form _vrf_PLAT021_rao02 ; PROBLEM: Ratio Unique / Expected Reflections too High ... 6.811 RESPONSE: Twinned data set. Reflections are for 2 components. ; _vrf_PLAT341_rao02 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0154 Ang. RESPONSE: Twinned data set is limiting bond precision. ; _vrf_PLAT415_rao02 ; PROBLEM: Short Inter D-H..H-X H2B .. H5Y .. 2.00 Ang. RESPONSE: Hydrogen from partial water occupancy placed, not refined. ; # end Validation Reply Form _chemical_name_common FeA _chemical_melting_point ? _chemical_formula_moiety 'C5 H8 Cl2 Fe N3 O2, 0.3(H2 O)' _chemical_formula_sum 'C5 H8.62 Cl2 Fe N3 O2.25' _chemical_formula_weight 273.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _diffrn_refln_scan_width 0.5 _diffrn_refln_scan_rate 10 _space_group.centring_type primitive _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.3249(5) _cell_length_b 9.4984(4) _cell_length_c 22.7056(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2011.07(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4623 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 25.30 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.807 _exptl_crystal_F_000 1101 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 2.005 _shelx_estimated_absorpt_T_min 0.856 _shelx_estimated_absorpt_T_max 0.961 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details TWINABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'microfocus sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 26858 _diffrn_reflns_av_unetI/netI 0.0889 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.794 _diffrn_reflns_theta_max 25.358 _diffrn_reflns_theta_full 25.000 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 14493 _reflns_number_gt 12384 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.733 _reflns_Friedel_fraction_max 0.995 _reflns_Friedel_fraction_full 0.997 _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refined as a 2-component twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0359P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1205 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.028(16) _chemical_absolute_configuration ad _refine_ls_number_reflns 14493 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0971 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3050(11) 0.4941(11) -0.0342(4) 0.013(2) Uani 1 1 d . . . . . C2 C 0.2756(13) 0.6408(12) -0.0145(4) 0.023(3) Uani 1 1 d . . . . . H2A H 0.1780 0.6467 0.0026 0.027 Uiso 1 1 calc R U . . . H2B H 0.2807 0.7058 -0.0485 0.027 Uiso 1 1 calc R U . . . C3 C 0.3857(15) 0.6822(12) 0.0313(5) 0.040(3) Uani 1 1 d . . . . . H3A H 0.4791 0.6969 0.0115 0.048 Uiso 1 1 calc R U . . . H3B H 0.3567 0.7730 0.0491 0.048 Uiso 1 1 calc R U . . . C4 C 0.4048(12) 0.5750(11) 0.0797(4) 0.017(3) Uani 1 1 d . . . . . H4A H 0.4928 0.5968 0.1023 0.021 Uiso 1 1 calc R U . . . H4B H 0.3222 0.5795 0.1070 0.021 Uiso 1 1 calc R U . . . C5 C 0.4158(11) 0.4314(11) 0.0545(4) 0.011(2) Uani 1 1 d . . . . . C6 C 0.6881(11) 0.4466(12) 0.3369(4) 0.012(3) Uani 1 1 d . . . . . C7 C 0.8392(11) 0.4786(14) 0.3524(4) 0.019(3) Uani 1 1 d . . . . . H7A H 0.8755 0.4070 0.3803 0.023 Uiso 1 1 calc R U . . . H7B H 0.8445 0.5718 0.3718 0.023 Uiso 1 1 calc R U . . . C8 C 0.9298(14) 0.4792(15) 0.2984(5) 0.036(4) Uani 1 1 d . . . . . H8A H 1.0319 0.4815 0.3103 0.043 Uiso 1 1 calc R U . . . H8B H 0.9099 0.5663 0.2759 0.043 Uiso 1 1 calc R U . . . C9 C 0.9061(10) 0.3518(13) 0.2576(4) 0.022(3) Uani 1 1 d . . . . . H9A H 0.9547 0.3675 0.2194 0.026 Uiso 1 1 calc R U . . . H9B H 0.9465 0.2658 0.2758 0.026 Uiso 1 1 calc R U . . . C10 C 0.7491(11) 0.3346(12) 0.2482(4) 0.012(2) Uani 1 1 d . . . . . N1 N 0.2622(9) 0.4422(9) -0.0840(4) 0.013(2) Uani 1 1 d . . . . . H1 H 0.2171 0.4951 -0.1098 0.016 Uiso 1 1 calc R U . . . N2 N 0.3764(9) 0.4010(9) -0.0014(3) 0.009(2) Uani 1 1 d . . . . . N3 N 0.4635(9) 0.3221(9) 0.0826(3) 0.013(2) Uani 1 1 d . . . . . H3 H 0.4935 0.3290 0.1193 0.015 Uiso 1 1 calc R U . . . N4 N 0.5765(9) 0.4891(9) 0.3666(3) 0.012(2) Uani 1 1 d . . . . . H4 H 0.5868 0.5400 0.3987 0.015 Uiso 1 1 calc R U . . . N5 N 0.6499(9) 0.3691(9) 0.2890(3) 0.011(2) Uani 1 1 d . . . . . N6 N 0.6921(9) 0.2844(10) 0.2007(3) 0.013(2) Uani 1 1 d . . . . . H6 H 0.7463 0.2551 0.1714 0.016 Uiso 1 1 calc R U . . . O1 O 0.2889(8) 0.3031(8) -0.0954(3) 0.0137(17) Uani 1 1 d . . . . . O2 O 0.4659(7) 0.1962(8) 0.0538(3) 0.0141(17) Uani 1 1 d . . . . . O3 O 0.4421(8) 0.4525(8) 0.3466(3) 0.0159(17) Uani 1 1 d . . . . . O4 O 0.5456(8) 0.2778(8) 0.1969(3) 0.0156(18) Uani 1 1 d . . . . . O5 O 0.0270(15) 0.1858(16) 0.3778(5) 0.042(6) Uani 0.61(2) 1 d . . P . . H5X H -0.0037 0.1015 0.3776 0.050 Uiso 0.61(2) 1 d R U P . . H5Y H 0.1144 0.1894 0.3882 0.050 Uiso 0.61(2) 1 d R U P . . Cl1 Cl 0.5823(3) 0.1400(3) -0.08355(11) 0.0250(7) Uani 1 1 d . . . . . Cl2 Cl 0.2519(3) 0.0150(3) -0.01888(12) 0.0224(7) Uani 1 1 d . . . . . Cl3 Cl 0.3300(3) 0.1518(3) 0.30242(11) 0.0233(7) Uani 1 1 d . . . . . Cl4 Cl 0.2779(3) 0.4735(3) 0.22339(12) 0.0207(7) Uani 1 1 d . . . . . Fe1 Fe 0.39331(17) 0.20206(16) -0.03009(6) 0.0116(4) Uani 1 1 d . . . . . Fe2 Fe 0.44118(16) 0.34464(17) 0.26959(6) 0.0129(4) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.012(6) 0.017(7) 0.010(5) 0.002(5) -0.002(5) -0.002(5) C2 0.030(7) 0.013(6) 0.026(6) -0.003(5) -0.005(5) 0.005(6) C3 0.064(10) 0.020(7) 0.036(7) -0.002(6) -0.019(7) 0.004(8) C4 0.020(7) 0.011(6) 0.020(6) -0.009(5) -0.003(5) -0.004(6) C5 0.006(6) 0.011(6) 0.017(6) 0.000(4) 0.002(5) -0.003(5) C6 0.014(6) 0.015(7) 0.007(5) 0.000(4) 0.003(5) 0.004(5) C7 0.012(6) 0.024(8) 0.022(6) -0.004(5) -0.005(5) 0.004(6) C8 0.026(8) 0.050(10) 0.031(7) -0.013(6) 0.005(6) -0.007(8) C9 0.009(6) 0.032(7) 0.026(6) -0.007(5) 0.004(5) 0.001(6) C10 0.014(6) 0.009(6) 0.014(6) 0.001(4) 0.003(4) 0.000(5) N1 0.015(5) 0.008(5) 0.017(5) 0.003(4) -0.004(4) -0.001(4) N2 0.009(5) 0.010(5) 0.007(4) 0.004(3) -0.002(4) -0.001(4) N3 0.018(5) 0.015(6) 0.005(4) -0.003(4) -0.003(4) -0.004(4) N4 0.018(6) 0.010(5) 0.009(4) -0.003(4) -0.002(4) -0.003(4) N5 0.016(5) 0.007(5) 0.012(4) -0.001(4) 0.002(4) -0.003(4) N6 0.016(5) 0.012(5) 0.010(5) 0.001(4) 0.007(4) 0.004(5) O1 0.019(4) 0.008(4) 0.014(4) -0.003(3) -0.005(3) 0.001(4) O2 0.019(4) 0.011(4) 0.012(4) 0.001(3) -0.001(3) 0.000(4) O3 0.012(4) 0.018(5) 0.017(4) -0.007(3) 0.000(3) -0.002(4) O4 0.014(4) 0.021(5) 0.011(4) -0.002(3) 0.001(3) -0.001(4) O5 0.048(11) 0.033(11) 0.044(10) 0.007(8) -0.008(7) 0.010(9) Cl1 0.0203(16) 0.0336(19) 0.0211(15) -0.0027(13) 0.0030(12) 0.0084(15) Cl2 0.0237(16) 0.0136(16) 0.0298(16) 0.0040(12) -0.0056(12) -0.0048(13) Cl3 0.0295(18) 0.0196(18) 0.0208(14) -0.0006(13) 0.0017(13) -0.0076(15) Cl4 0.0184(15) 0.0241(17) 0.0195(14) 0.0015(13) -0.0011(13) 0.0033(13) Fe1 0.0135(9) 0.0110(9) 0.0103(8) 0.0007(7) -0.0023(7) 0.0013(7) Fe2 0.0146(9) 0.0135(9) 0.0105(8) -0.0023(7) 0.0012(7) 0.0001(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.296(12) . ? C1 N2 1.334(12) . ? C1 C2 1.489(15) . ? C2 C3 1.513(15) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(14) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.483(14) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.298(13) . ? C5 N2 1.354(11) . ? C6 N4 1.304(12) . ? C6 N5 1.360(12) . ? C6 C7 1.484(14) . ? C7 C8 1.489(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.540(15) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.488(13) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N6 1.294(11) . ? C10 N5 1.349(11) . ? N1 O1 1.369(11) . ? N1 H1 0.8800 . ? N2 Fe1 2.005(8) . ? N3 O2 1.364(10) . ? N3 H3 0.8800 . ? N4 O3 1.377(10) . ? N4 H4 0.8800 . ? N5 Fe2 2.009(8) . ? N6 O4 1.371(10) . ? N6 H6 0.8800 . ? O1 Fe1 2.017(7) . ? O2 Fe1 2.021(6) . ? O3 Fe2 2.026(6) . ? O4 Fe2 2.018(6) . ? O5 H5X 0.8501 . ? O5 H5Y 0.8494 . ? Cl1 Fe1 2.220(3) . ? Cl2 Fe1 2.227(3) . ? Cl3 Fe2 2.233(3) . ? Cl4 Fe2 2.217(3) . ? 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_3 _geom_angle_publ_flag N1 C1 N2 112.8(9) . . ? N1 C1 C2 124.2(10) . . ? N2 C1 C2 123.0(9) . . ? C1 C2 C3 109.0(9) . . ? C1 C2 H2A 109.9 . . ? C3 C2 H2A 109.9 . . ? C1 C2 H2B 109.9 . . ? C3 C2 H2B 109.9 . . ? H2A C2 H2B 108.3 . . ? C4 C3 C2 113.9(10) . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3B 108.8 . . ? C2 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 110.4(8) . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 N2 112.6(9) . . ? N3 C5 C4 124.7(9) . . ? N2 C5 C4 122.7(10) . . ? N4 C6 N5 111.8(9) . . ? N4 C6 C7 124.9(9) . . ? N5 C6 C7 123.3(9) . . ? C6 C7 C8 110.1(9) . . ? C6 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? C6 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? C7 C8 C9 114.3(10) . . ? C7 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? C7 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 108.3(9) . . ? C10 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? C10 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N6 C10 N5 112.4(9) . . ? N6 C10 C9 124.3(9) . . ? N5 C10 C9 123.3(9) . . ? C1 N1 O1 118.5(8) . . ? C1 N1 H1 120.8 . . ? O1 N1 H1 120.8 . . ? C1 N2 C5 121.1(9) . . ? C1 N2 Fe1 118.9(6) . . ? C5 N2 Fe1 119.0(7) . . ? C5 N3 O2 118.1(8) . . ? C5 N3 H3 121.0 . . ? O2 N3 H3 121.0 . . ? C6 N4 O3 118.5(8) . . ? C6 N4 H4 120.7 . . ? O3 N4 H4 120.7 . . ? C10 N5 C6 120.0(9) . . ? C10 N5 Fe2 119.0(6) . . ? C6 N5 Fe2 119.4(7) . . ? C10 N6 O4 118.5(8) . . ? C10 N6 H6 120.7 . . ? O4 N6 H6 120.7 . . ? N1 O1 Fe1 114.0(5) . . ? N3 O2 Fe1 115.1(6) . . ? N4 O3 Fe2 114.6(5) . . ? N6 O4 Fe2 114.6(5) . . ? H5X O5 H5Y 111.2 . . ? N2 Fe1 O1 75.7(3) . . ? N2 Fe1 O2 75.3(3) . . ? O1 Fe1 O2 150.1(3) . . ? N2 Fe1 Cl1 119.3(3) . . ? O1 Fe1 Cl1 96.2(2) . . ? O2 Fe1 Cl1 104.0(2) . . ? N2 Fe1 Cl2 131.9(3) . . ? O1 Fe1 Cl2 100.2(2) . . ? O2 Fe1 Cl2 93.9(2) . . ? Cl1 Fe1 Cl2 108.72(13) . . ? N5 Fe2 O4 75.4(3) . . ? N5 Fe2 O3 75.4(3) . . ? O4 Fe2 O3 149.6(3) . . ? N5 Fe2 Cl4 134.9(3) . . ? O4 Fe2 Cl4 96.8(2) . . ? O3 Fe2 Cl4 97.6(2) . . ? N5 Fe2 Cl3 118.1(3) . . ? O4 Fe2 Cl3 103.8(2) . . ? O3 Fe2 Cl3 97.4(2) . . ? Cl4 Fe2 Cl3 106.97(12) . . ? _refine_diff_density_max 0.744 _refine_diff_density_min -0.431 _refine_diff_density_rms 0.088 _shelxl_version_number 2013-4 _shelx_res_file ; TITL twin4 in P2(1)2(1)2(1) CELL 0.71073 9.3249 9.4984 22.7056 90.000 90.000 90.000 ZERR 8.00 0.0005 0.0004 0.0008 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL FE UNIT 40 69 24 18 16 8 MERG 0 FMAP 2 PLAN 25 SIZE 0.020 0.060 0.080 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.035900 BASF 0.52654 FVAR 0.55220 0.60832 C1 1 0.304974 0.494118 -0.034190 11.00000 0.01186 0.01679 = 0.01045 0.00242 -0.00242 -0.00167 C2 1 0.275564 0.640782 -0.014458 11.00000 0.02970 0.01294 = 0.02591 -0.00328 -0.00532 0.00506 AFIX 23 H2A 2 0.178034 0.646725 0.002588 11.00000 -1.20000 H2B 2 0.280730 0.705821 -0.048463 11.00000 -1.20000 AFIX 0 C3 1 0.385710 0.682230 0.031310 11.00000 0.06357 0.02000 = 0.03582 -0.00175 -0.01912 0.00378 AFIX 23 H3A 2 0.479106 0.696929 0.011509 11.00000 -1.20000 H3B 2 0.356694 0.772971 0.049147 11.00000 -1.20000 AFIX 0 C4 1 0.404842 0.575009 0.079715 11.00000 0.02001 0.01141 = 0.02048 -0.00871 -0.00326 -0.00403 AFIX 23 H4A 2 0.492838 0.596767 0.102347 11.00000 -1.20000 H4B 2 0.322208 0.579492 0.107026 11.00000 -1.20000 AFIX 0 C5 1 0.415827 0.431408 0.054501 11.00000 0.00575 0.01084 = 0.01681 0.00017 0.00169 -0.00292 C6 1 0.688069 0.446615 0.336856 11.00000 0.01387 0.01508 = 0.00739 0.00028 0.00321 0.00425 C7 1 0.839216 0.478633 0.352352 11.00000 0.01231 0.02377 = 0.02193 -0.00387 -0.00491 0.00401 AFIX 23 H7A 2 0.875529 0.407005 0.380296 11.00000 -1.20000 H7B 2 0.844481 0.571783 0.371793 11.00000 -1.20000 AFIX 0 C8 1 0.929809 0.479169 0.298372 11.00000 0.02640 0.04953 = 0.03069 -0.01268 0.00515 -0.00693 AFIX 23 H8A 2 1.031896 0.481498 0.310305 11.00000 -1.20000 H8B 2 0.909896 0.566349 0.275918 11.00000 -1.20000 AFIX 0 C9 1 0.906077 0.351809 0.257577 11.00000 0.00862 0.03180 = 0.02551 -0.00722 0.00411 0.00140 AFIX 23 H9A 2 0.954744 0.367511 0.219387 11.00000 -1.20000 H9B 2 0.946457 0.265788 0.275775 11.00000 -1.20000 AFIX 0 C10 1 0.749072 0.334553 0.248237 11.00000 0.01422 0.00902 = 0.01382 0.00086 0.00265 -0.00030 N1 3 0.262236 0.442195 -0.083970 11.00000 0.01520 0.00756 = 0.01706 0.00328 -0.00367 -0.00140 AFIX 43 H1 2 0.217111 0.495126 -0.109823 11.00000 -1.20000 AFIX 0 N2 3 0.376403 0.400988 -0.001443 11.00000 0.00889 0.01026 = 0.00704 0.00351 -0.00211 -0.00103 N3 3 0.463548 0.322082 0.082632 11.00000 0.01849 0.01470 = 0.00468 -0.00305 -0.00322 -0.00430 AFIX 43 H3 2 0.493511 0.328970 0.119271 11.00000 -1.20000 AFIX 0 N4 3 0.576480 0.489105 0.366557 11.00000 0.01794 0.01023 = 0.00857 -0.00309 -0.00192 -0.00313 AFIX 43 H4 2 0.586797 0.540041 0.398653 11.00000 -1.20000 AFIX 0 N5 3 0.649900 0.369082 0.289013 11.00000 0.01552 0.00735 = 0.01163 -0.00141 0.00173 -0.00265 N6 3 0.692146 0.284399 0.200710 11.00000 0.01630 0.01213 = 0.01048 0.00078 0.00682 0.00432 AFIX 43 H6 2 0.746323 0.255131 0.171433 11.00000 -1.20000 AFIX 0 O1 4 0.288894 0.303096 -0.095422 11.00000 0.01876 0.00834 = 0.01403 -0.00344 -0.00484 0.00136 O2 4 0.465902 0.196221 0.053752 11.00000 0.01916 0.01117 = 0.01190 0.00114 -0.00113 -0.00003 O3 4 0.442112 0.452478 0.346570 11.00000 0.01237 0.01827 = 0.01713 -0.00702 -0.00027 -0.00199 O4 4 0.545561 0.277839 0.196948 11.00000 0.01431 0.02121 = 0.01132 -0.00211 0.00100 -0.00069 O5 4 0.026969 0.185829 0.377819 21.00000 0.04788 0.03271 = 0.04413 0.00739 -0.00775 0.00953 AFIX 3 H5X 2 -0.003676 0.101544 0.377640 21.00000 -1.20000 H5Y 2 0.114398 0.189445 0.388214 21.00000 -1.20000 AFIX 0 CL1 5 0.582331 0.140019 -0.083549 11.00000 0.02029 0.03363 = 0.02110 -0.00266 0.00301 0.00838 CL2 5 0.251857 0.014997 -0.018882 11.00000 0.02372 0.01361 = 0.02983 0.00402 -0.00556 -0.00483 CL3 5 0.330004 0.151754 0.302420 11.00000 0.02952 0.01960 = 0.02083 -0.00057 0.00174 -0.00764 CL4 5 0.277909 0.473456 0.223391 11.00000 0.01840 0.02412 = 0.01949 0.00154 -0.00111 0.00333 FE1 6 0.393308 0.202056 -0.030087 11.00000 0.01348 0.01103 = 0.01028 0.00070 -0.00230 0.00128 FE2 6 0.441183 0.344636 0.269594 11.00000 0.01464 0.01355 = 0.01050 -0.00234 0.00119 0.00009 HKLF 5 REM twin4 in P2(1)2(1)2(1) REM R1 = 0.0479 for 12384 Fo > 4sig(Fo) and 0.0605 for all 14493 data REM 246 parameters refined using 0 restraints END WGHT 0.0359 0.0000 REM Highest difference peak 0.744, deepest hole -0.431, 1-sigma level 0.088 Q1 1 0.2745 0.6617 0.0466 11.00000 0.05 0.74 Q2 1 0.9441 0.3689 0.3182 11.00000 0.05 0.55 Q3 1 0.5799 0.0348 -0.0290 11.00000 0.05 0.34 Q4 1 0.3039 0.0711 0.0364 11.00000 0.05 0.33 Q5 1 0.7155 0.4413 0.2279 11.00000 0.05 0.31 Q6 1 0.1862 0.6511 0.1308 11.00000 0.05 0.31 Q7 1 -0.0841 0.2208 0.3992 11.00000 0.05 0.30 Q8 1 0.9417 0.5022 0.2411 11.00000 0.05 0.30 Q9 1 0.9173 0.2448 0.2855 11.00000 0.05 0.30 Q10 1 0.2397 0.8019 -0.0690 11.00000 0.05 0.30 Q11 1 0.3560 0.2844 -0.0706 11.00000 0.05 0.29 Q12 1 0.2691 0.4575 -0.0998 11.00000 0.05 0.29 Q13 1 0.3814 0.8738 0.0774 11.00000 0.05 0.29 Q14 1 0.6902 0.3310 0.1139 11.00000 0.05 0.29 Q15 1 0.9159 0.5167 0.3949 11.00000 0.05 0.29 Q16 1 0.9963 0.5753 0.2057 11.00000 0.05 0.28 Q17 1 0.4426 0.6275 0.1664 11.00000 0.05 0.28 Q18 1 0.2786 0.3538 0.3162 11.00000 0.05 0.28 Q19 1 0.1050 0.5817 0.0589 11.00000 0.05 0.28 Q20 1 0.7371 0.2784 0.2384 11.00000 0.05 0.27 Q21 1 0.2782 0.2057 0.0432 11.00000 0.05 0.27 Q22 1 0.1803 -0.0856 0.0366 11.00000 0.05 0.27 Q23 1 0.4636 0.2533 0.0683 11.00000 0.05 0.27 Q24 1 0.4506 0.3514 -0.0590 11.00000 0.05 0.27 Q25 1 0.1831 0.0406 0.0248 11.00000 0.05 0.26 ; _shelx_res_checksum 82338 _shelx_hkl_file ; 1 0 0 2.89370 5.51935 -1 -1 0 0 2.89370 5.51935 2 -1 0 0 11.1339 6.82099 -1 1 0 0 11.1339 6.82099 2 -1 0 0 -5.2703 5.66143 -1 1 0 0 -5.2703 5.66143 2 -2 0 0 19.6133 12.7785 -1 2 0 0 19.6133 12.7785 2 -2 0 0 32.7735 13.1934 -1 2 0 0 32.7735 13.1934 2 -2 0 0 48.1785 14.8951 -1 2 0 0 48.1785 14.8951 2 -3 0 0 -12.021 12.8125 -1 3 0 0 -12.021 12.8125 2 -3 0 0 23.1312 16.2764 -1 3 0 0 23.1312 16.2764 2 -3 0 0 14.4414 15.4077 -1 3 0 0 14.4414 15.4077 2 -4 0 0 27.2810 16.9242 -1 4 0 0 27.2810 16.9242 2 -4 0 0 -12.835 15.2387 -1 4 0 0 -12.835 15.2387 2 -4 0 0 -1.5577 17.5033 -1 4 0 0 -1.5577 17.5033 2 -5 0 0 2.38921 19.9844 -1 5 0 0 2.38921 19.9844 2 -5 0 0 19.0254 20.5441 -1 5 0 0 19.0254 20.5441 2 -5 0 0 -26.018 18.0416 -1 5 0 0 -26.018 18.0416 2 -6 0 0 7577.87 240.963 -1 6 0 0 7577.87 240.963 2 -6 0 0 8144.29 237.929 -1 6 0 0 8144.29 237.929 2 -6 0 0 7845.66 249.496 -1 6 0 0 7845.66 249.496 2 -7 0 0 -8.6301 23.2509 -1 7 0 0 -8.6301 23.2509 2 -7 0 0 -11.589 22.0346 -1 7 0 0 -11.589 22.0346 2 -7 0 0 -2.6983 22.1964 -1 7 0 0 -2.6983 22.1964 2 -8 0 0 599.491 55.7808 -1 8 0 0 599.491 55.7808 2 -8 0 0 513.189 51.9869 -1 8 0 0 513.189 51.9869 2 -9 0 0 -6.8104 30.3657 -1 9 0 0 -6.8104 30.3657 2 -10 0 0 46.8734 34.5439 -1 10 0 0 46.8734 34.5439 2 -11 0 0 4.09305 37.4724 -1 11 0 0 4.09305 37.4724 2 0 -1 0 6.15956 6.52391 -1 0 -1 0 6.15956 6.52391 2 0 1 0 7.06028 8.95406 -1 0 1 0 7.06028 8.95406 2 1 -1 0 36.5920 9.31956 -1 -1 -1 0 36.5920 9.31956 2 -1 -1 0 47.6062 11.0295 -1 1 -1 0 47.6062 11.0295 2 -1 1 0 53.2001 9.66137 -1 1 1 0 53.2001 9.66137 2 -1 1 0 32.7000 12.7649 -1 1 1 0 32.7000 12.7649 2 -1 1 0 36.1740 12.0097 -1 1 1 0 36.1740 12.0097 2 1 1 0 63.5000 12.4497 -1 -1 1 0 63.5000 12.4497 2 -2 -1 0 5114.07 145.803 -1 2 -1 0 5114.07 145.803 2 -2 -1 0 5475.34 142.828 -1 2 -1 0 5475.34 142.828 2 2 -1 0 5011.63 135.196 -1 -2 -1 0 5011.63 135.196 2 -2 1 0 5583.36 147.011 -1 2 1 0 5583.36 147.011 2 2 1 0 5362.78 147.500 -1 -2 1 0 5362.78 147.500 2 -2 1 0 5208.28 148.391 -1 2 1 0 5208.28 148.391 2 2 1 0 4927.03 144.247 -1 -2 1 0 4927.03 144.247 2 -2 1 0 4928.41 146.564 -1 2 1 0 4928.41 146.564 2 -2 1 0 5310.28 155.857 -1 2 1 0 5310.28 155.857 2 -3 -1 0 454.163 29.1364 -1 3 -1 0 454.163 29.1364 2 -3 -1 0 441.786 31.0641 -1 3 -1 0 441.786 31.0641 2 -3 1 0 437.779 27.8220 -1 3 1 0 437.779 27.8220 2 -3 1 0 375.867 32.4024 -1 3 1 0 375.867 32.4024 2 -3 1 0 408.919 31.9352 -1 3 1 0 408.919 31.9352 2 3 1 0 348.310 28.3666 -1 -3 1 0 348.310 28.3666 2 -4 -1 0 1221.81 54.5924 -1 4 -1 0 1221.81 54.5924 2 -4 -1 0 1176.21 56.5987 -1 4 -1 0 1176.21 56.5987 2 -4 1 0 1131.50 60.1491 -1 4 1 0 1131.50 60.1491 2 4 1 0 1140.25 55.2401 -1 -4 1 0 1140.25 55.2401 2 -4 1 0 1147.90 57.8345 -1 4 1 0 1147.90 57.8345 2 -5 -1 0 2131.01 83.4460 -1 5 -1 0 2131.01 83.4460 2 -5 -1 0 2067.71 86.1091 -1 5 -1 0 2067.71 86.1091 2 -5 1 0 2006.56 84.0938 -1 5 1 0 2006.56 84.0938 2 -5 1 0 2101.56 87.6934 -1 5 1 0 2101.56 87.6934 2 -5 1 0 1900.01 88.4586 -1 5 1 0 1900.01 88.4586 2 -6 -1 0 28.7980 24.1671 -1 6 -1 0 28.7980 24.1671 2 -6 -1 0 30.5841 25.8569 -1 6 -1 0 30.5841 25.8569 2 -6 1 0 6.01688 27.5928 -1 6 1 0 6.01688 27.5928 2 -6 1 0 21.8451 28.6917 -1 6 1 0 21.8451 28.6917 2 -6 1 0 50.7183 25.8975 -1 6 1 0 50.7183 25.8975 2 -7 -1 0 36.5105 27.9854 -1 7 -1 0 36.5105 27.9854 2 -7 -1 0 22.3725 26.3658 -1 7 -1 0 22.3725 26.3658 2 -7 1 0 43.3969 33.5848 -1 7 1 0 43.3969 33.5848 2 -7 1 0 72.7935 32.4053 -1 7 1 0 72.7935 32.4053 2 -7 1 0 31.8087 32.8657 -1 7 1 0 31.8087 32.8657 2 -8 -1 0 3.55487 29.6494 -1 8 -1 0 3.55487 29.6494 2 -8 1 0 24.8841 35.5533 -1 8 1 0 24.8841 35.5533 2 -8 1 0 23.3409 36.6234 -1 8 1 0 23.3409 36.6234 2 -9 -1 0 260.617 45.9071 -1 9 -1 0 260.617 45.9071 2 -9 1 0 297.052 53.6528 -1 9 1 0 297.052 53.6528 2 -10 -1 0 -13.608 35.3362 -1 10 -1 0 -13.608 35.3362 2 -11 -1 0 93.4006 46.3912 -1 11 -1 0 93.4006 46.3912 2 0 -2 0 50.2375 16.1733 -1 0 -2 0 50.2375 16.1733 2 0 -2 0 25.3518 13.4206 -1 0 -2 0 25.3518 13.4206 2 0 2 0 32.3331 18.4719 -1 0 2 0 32.3331 18.4719 2 -1 -2 0 18.3444 11.7814 -1 1 -2 0 18.3444 11.7814 2 -1 2 0 19.0967 13.4916 -1 1 2 0 19.0967 13.4916 2 1 2 0 30.0665 17.1361 -1 -1 2 0 30.0665 17.1361 2 -1 2 0 59.9182 19.5267 -1 1 2 0 59.9182 19.5267 2 -2 -2 0 7156.72 188.239 -1 2 -2 0 7156.72 188.239 2 -2 -2 0 6741.54 191.500 -1 2 -2 0 6741.54 191.500 2 2 2 0 6929.04 193.909 -1 -2 2 0 6929.04 193.909 2 -2 2 0 7095.04 197.730 -1 2 2 0 7095.04 197.730 2 -3 -2 0 1112.46 52.8227 -1 3 -2 0 1112.46 52.8227 2 -3 -2 0 1180.46 50.6892 -1 3 -2 0 1180.46 50.6892 2 -3 2 0 1284.14 53.8384 -1 3 2 0 1284.14 53.8384 2 -3 2 0 1241.88 58.2146 -1 3 2 0 1241.88 58.2146 2 3 2 0 1163.43 53.7405 -1 -3 2 0 1163.43 53.7405 2 -4 -2 0 1697.40 66.3418 -1 4 -2 0 1697.40 66.3418 2 -4 -2 0 1597.61 68.9605 -1 4 -2 0 1597.61 68.9605 2 -4 2 0 1308.52 64.9244 -1 4 2 0 1308.52 64.9244 2 4 2 0 1634.50 69.4196 -1 -4 2 0 1634.50 69.4196 2 -5 -2 0 1248.33 61.3485 -1 5 -2 0 1248.33 61.3485 2 -5 -2 0 1266.35 66.0472 -1 5 -2 0 1266.35 66.0472 2 5 2 0 1140.30 62.7528 -1 -5 2 0 1140.30 62.7528 2 -6 -2 0 192.488 33.5828 -1 6 -2 0 192.488 33.5828 2 -6 -2 0 163.962 34.9665 -1 6 -2 0 163.962 34.9665 2 6 2 0 106.041 22.6260 2 -7 -2 0 308.444 43.1602 -1 7 -2 0 308.444 43.1602 2 7 2 0 137.505 26.2024 2 -8 -2 0 50.3119 34.2031 -1 8 -2 0 50.3119 34.2031 2 8 2 0 39.6081 22.5649 2 -9 -2 0 445.119 58.0833 -1 9 -2 0 445.119 58.0833 2 -9 2 0 216.740 41.5085 -1 9 2 0 216.740 41.5085 2 9 2 1 216.740 41.5085 2 -10 -2 0 199.567 50.3147 -1 10 -2 0 199.567 50.3147 2 -11 -2 0 1085.07 93.6204 -1 11 -2 0 1085.07 93.6204 2 0 -3 0 382.791 27.8343 -1 0 -3 -1 382.791 27.8343 2 0 3 0 3.38569 6.77008 2 1 -3 0 105.605 19.4863 2 -1 3 0 746.913 37.9747 -1 1 3 1 746.913 37.9747 2 2 -3 0 11.6698 10.3079 2 -2 3 0 252.405 24.1927 -1 2 3 1 252.405 24.1927 2 -3 -3 0 273.250 20.5286 2 3 -3 0 231.936 18.2707 2 3 -3 0 213.795 24.0597 2 -3 3 0 225.438 25.2699 -1 3 3 1 225.438 25.2699 2 -3 3 0 232.525 28.9779 -1 3 3 1 232.525 28.9779 2 4 -3 0 12.7862 11.7821 2 4 -3 0 9.14153 9.06934 2 -4 -3 0 14.2413 9.78006 2 4 -3 0 2680.64 83.5345 -1 -4 -3 -1 2680.64 83.5345 2 -4 3 0 2176.94 92.3268 -1 4 3 1 2176.94 92.3268 2 5 -3 0 2209.32 75.1588 -1 -5 -3 -1 2209.32 75.1588 2 -5 3 0 2184.35 104.439 -1 5 3 1 2184.35 104.439 2 -5 3 0 1884.99 88.3933 -1 5 3 1 1884.99 88.3933 2 6 -3 0 333.938 29.0909 -1 -6 -3 -1 333.938 29.0909 2 -6 3 0 270.703 35.6330 -1 6 3 1 270.703 35.6330 2 -6 3 0 346.590 53.4642 -1 6 3 1 346.590 53.4642 2 -7 3 0 62.8222 41.8395 -1 7 3 1 62.8222 41.8395 2 -7 3 0 40.7122 25.5734 -1 7 3 1 40.7122 25.5734 2 -8 3 0 67.0015 43.1973 -1 8 3 1 67.0015 43.1973 2 -8 3 0 61.5933 43.1330 -1 8 3 1 61.5933 43.1330 2 -8 3 0 96.4130 32.2871 -1 8 3 1 96.4130 32.2871 2 -9 3 0 154.146 49.1223 -1 9 3 1 154.146 49.1223 2 -9 3 0 87.2505 51.1032 -1 9 3 1 87.2505 51.1032 2 -9 3 0 126.878 37.7389 -1 9 3 1 126.878 37.7389 2 -9 3 0 93.2864 47.6372 -1 9 3 1 93.2864 47.6372 2 -10 3 0 105.700 53.5631 -1 10 3 1 105.700 53.5631 2 -10 3 0 36.5150 50.3421 -1 10 3 1 36.5150 50.3421 2 0 -4 0 91.8065 21.5212 -1 0 -4 -1 91.8065 21.5212 2 0 4 0 105.325 25.5627 -1 0 4 1 105.325 25.5627 2 0 4 0 100.022 23.2022 -1 0 4 1 100.022 23.2022 2 -1 -4 0 862.892 46.6992 -1 1 -4 -1 862.892 46.6992 2 -1 -4 0 869.360 44.1768 -1 1 -4 -1 869.360 44.1768 2 -1 4 0 774.179 45.0509 -1 1 4 1 774.179 45.0509 2 -1 4 0 914.710 50.0962 -1 1 4 1 914.710 50.0962 2 -1 4 0 901.825 47.7723 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21.9216 2 9 1 -10 14.1267 22.6976 2 8 -1 -10 598.880 52.9906 2 8 1 -10 646.760 55.6939 2 7 -1 -10 97.0390 24.3522 2 7 1 -10 126.512 28.8367 2 6 -1 -10 78.7237 22.4595 2 6 1 -10 44.9398 19.2109 2 5 -1 -10 527.972 36.3325 2 5 1 -10 532.381 40.9677 2 4 -1 -10 2004.28 70.6698 2 4 -1 -10 1917.30 58.8796 2 4 1 -10 1841.18 75.6624 2 4 1 -10 2027.11 81.0447 2 3 -1 -10 40.7876 10.3432 2 3 -1 -10 42.1296 10.3710 2 -3 -1 10 26.3680 10.5686 2 3 1 -10 56.5762 11.6297 2 -3 1 10 41.0750 10.7241 2 -3 1 10 45.4336 11.6210 2 3 1 -10 55.9303 15.5733 2 3 1 -10 49.0287 14.9678 2 -2 -1 10 2457.20 81.1411 2 2 1 -10 2447.99 76.6870 2 2 1 -10 2407.03 75.3220 2 -2 1 10 2506.72 87.3927 2 2 1 -10 2478.96 89.5851 2 -1 -1 10 1248.81 55.0538 2 -1 -1 10 1328.27 49.1216 2 -1 1 10 1284.93 59.1338 2 1 1 -10 1246.87 56.5121 2 1 1 -10 1303.12 45.0032 2 0 -1 -10 4.92674 4.24647 2 0 -1 -10 5.99133 5.22248 2 0 -1 10 -6.0444 5.89661 2 0 -1 10 12.8773 10.7018 2 0 1 10 2.51481 8.32891 2 0 1 10 2.67178 5.09456 2 0 1 10 0.35322 9.39608 2 0 1 10 5.40745 5.81134 2 0 1 -10 1.60836 8.76372 2 1 -1 10 1288.53 52.2497 2 -1 -1 -10 1290.26 47.8527 2 1 -1 10 1467.10 58.5358 2 -1 -1 -10 1299.23 48.5704 2 1 1 10 1302.95 66.3174 2 1 1 10 1302.57 42.1756 2 -1 1 -10 1343.73 57.2252 2 1 1 10 1252.33 56.4325 2 1 1 10 1282.40 48.9644 2 1 1 10 1239.89 47.6275 2 2 -1 10 2388.51 88.7044 2 2 -1 10 2330.83 85.0213 2 -2 -1 -10 2461.36 83.1871 2 2 -1 10 2305.89 91.8429 2 2 1 10 2536.85 93.0393 2 2 1 10 2430.85 76.5195 2 2 1 10 2417.19 83.7959 2 2 1 10 2428.30 82.5657 2 2 1 10 2516.44 82.7705 2 2 1 10 2254.85 100.014 2 -2 1 -10 2404.30 88.6185 2 -3 -1 -10 55.9145 16.0042 2 3 -1 10 48.7809 16.9994 2 3 -1 10 33.6691 14.6815 2 3 -1 10 58.0294 16.3460 2 3 1 10 33.5713 15.9222 2 3 1 10 59.5986 14.9238 2 3 1 10 59.5615 15.8295 2 3 1 10 51.7106 15.0742 2 -3 1 -10 37.1077 14.5257 2 3 1 10 47.1927 12.8549 2 4 -1 10 1816.12 79.8847 2 -4 -1 -10 1983.82 81.9468 2 4 -1 10 1801.17 84.4696 2 4 -1 10 1789.95 82.4509 2 4 1 10 1914.44 86.0485 2 4 1 10 1957.50 80.4718 2 4 1 10 1958.37 81.5355 2 4 1 10 1996.52 77.7395 2 -4 1 -10 1852.26 83.0501 2 4 1 10 1970.04 82.0395 2 5 -1 10 498.976 44.2828 2 5 -1 10 539.406 44.7893 2 5 -1 10 522.946 45.4021 2 -5 -1 -10 594.469 43.9103 2 5 1 10 582.906 45.4073 2 5 1 10 505.897 41.9190 2 5 1 10 565.257 43.1952 2 -5 1 -10 487.923 42.5416 2 6 -1 10 17.4573 16.3495 2 6 -1 10 49.5472 20.5454 2 6 -1 10 51.6141 22.6882 2 6 1 10 59.0942 36.3060 -1 -6 1 -10 59.0942 36.3060 2 -7 -1 -10 160.276 51.4625 -1 7 -1 10 160.276 51.4625 2 7 1 10 217.121 49.8352 -1 -7 1 -10 217.121 49.8352 2 -8 -1 -10 1299.28 94.9955 -1 8 -1 10 1299.28 94.9955 2 -8 -1 -10 1324.76 91.1977 -1 8 -1 10 1324.76 91.1977 2 8 1 10 770.240 65.1155 2 8 1 10 753.860 64.9907 2 -9 -1 -10 28.2914 50.5359 -1 9 -1 10 28.2914 50.5359 2 -9 -1 -10 12.1403 60.1593 -1 9 -1 10 12.1403 60.1593 2 -9 1 -10 75.2971 52.4967 -1 9 1 10 75.2971 52.4967 2 -10 -1 -10 34.3030 55.9912 -1 10 -1 10 34.3030 55.9912 2 -10 1 -10 -10.996 56.8207 -1 10 1 10 -10.996 56.8207 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477.606 37.8516 2 4 -4 10 430.078 39.9841 2 4 -4 10 441.479 43.6851 2 -4 -4 -10 482.505 42.9047 2 4 -4 10 323.462 40.8779 2 4 4 10 407.484 50.5338 2 4 4 10 424.675 37.6460 2 -4 4 -10 349.380 39.5596 2 4 4 10 441.776 37.2581 2 5 -4 10 626.007 52.5913 2 -5 -4 -10 535.828 46.7821 2 5 -4 10 582.763 54.2545 2 5 -4 10 455.866 43.7141 2 5 4 10 517.382 45.2590 2 -5 4 -10 628.722 53.1481 2 5 4 10 581.809 45.3345 2 5 4 10 621.764 47.6176 2 5 4 10 557.399 59.6033 2 6 -4 10 873.661 66.2443 2 6 -4 10 856.568 68.6998 2 6 -4 10 874.450 61.8462 2 -6 -4 -10 870.117 61.1030 2 -6 -4 -10 1189.37 92.2986 -1 6 -4 9 1189.37 92.2986 2 -7 -4 -10 205.387 35.4628 2 7 -4 10 157.500 41.4682 2 7 -4 10 217.675 42.8497 2 7 -4 10 157.692 33.3577 2 -7 -4 -10 231.731 64.3638 -1 7 -4 9 231.731 64.3638 2 -7 4 -10 79.7495 28.3681 2 7 4 10 91.8559 30.0629 2 7 4 10 124.293 32.7814 2 7 4 10 113.053 33.0428 2 -8 -4 -10 48.6137 50.6571 -1 8 -4 9 48.6137 50.6571 2 -8 -4 -10 28.3706 60.6998 -1 8 -4 9 28.3706 60.6998 2 8 4 10 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190.602 27.4310 2 -5 1 -11 207.659 29.2071 2 5 1 11 160.797 29.1779 2 5 1 11 151.902 27.0239 2 6 -1 11 210.950 31.7439 2 6 -1 11 232.024 38.2703 2 6 -1 11 202.810 35.0901 2 6 1 11 152.422 30.7596 2 6 1 11 197.675 31.5873 2 -6 1 -11 176.394 29.9873 2 7 -1 11 114.061 30.8985 2 7 -1 11 114.252 33.7359 2 7 1 11 277.327 53.9631 -1 -7 1 -11 277.327 53.9631 2 -8 -1 -11 833.218 74.9695 -1 8 -1 11 833.218 74.9695 2 -8 -1 -11 789.411 79.7103 -1 8 -1 11 789.411 79.7103 2 8 1 11 474.994 52.3825 2 8 1 11 457.644 54.5093 2 -9 -1 -11 374.314 65.1153 -1 9 -1 11 374.314 65.1153 2 9 1 11 144.525 39.4192 2 9 1 11 129.062 40.1124 2 9 1 11 156.291 38.8755 2 -10 -1 -11 294.740 68.0737 -1 10 -1 11 294.740 68.0737 2 10 1 11 120.559 41.6775 2 10 -2 -11 -1.5955 25.4685 2 10 2 -11 8.72869 23.6365 2 9 -2 -11 188.185 38.7069 2 9 2 -11 228.774 43.7216 2 9 2 -11 149.519 38.1828 2 8 -2 -11 265.842 37.8708 2 8 2 -11 304.242 42.5465 2 8 2 -11 250.575 41.9829 2 7 -2 -11 64.9538 21.7382 2 7 2 -11 83.3272 27.6956 2 7 2 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134.292 21.5213 2 -3 6 11 140.968 37.5072 2 3 6 -11 115.922 38.8081 2 3 6 -11 199.552 31.7266 2 3 6 -11 118.533 28.7047 2 2 -6 -11 46.6021 12.8186 2 -2 -6 11 28.6065 20.7770 2 2 6 -11 35.1066 24.4300 2 2 6 -11 37.7106 21.7189 2 -2 6 11 -1.4650 17.9888 2 1 -6 -11 45.7376 13.6799 2 -1 -6 11 67.1392 24.7374 2 1 -6 -11 71.2328 20.8160 2 1 6 -11 51.7277 23.6205 2 1 6 -11 15.0922 23.2155 2 -1 6 11 60.0684 25.5278 2 0 -6 -11 1036.72 49.4782 2 0 -6 -11 1049.98 60.8214 2 0 -6 11 1015.92 72.9937 2 0 -6 11 1023.09 65.7132 2 0 6 -11 932.986 71.9465 2 0 6 11 1025.95 73.8885 2 1 -6 11 62.1797 23.9780 2 1 -6 11 66.9782 29.0173 2 -1 -6 -11 34.4037 16.6065 2 1 6 11 14.9619 22.6204 2 1 6 11 44.7814 16.4824 2 -1 6 -11 60.6962 28.4554 2 2 -6 11 50.8806 29.5381 2 2 -6 11 27.1798 19.0645 2 -2 -6 -11 14.0871 16.5007 2 -2 6 -11 9.49356 22.0459 2 2 6 11 32.1955 16.1958 2 2 6 11 64.1809 28.8172 2 -3 -6 -11 172.222 32.4369 2 3 -6 11 173.811 37.9163 2 3 -6 11 116.340 36.5168 2 3 6 11 145.267 24.9164 2 3 6 11 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38.3861 2 6 -7 -11 67.6460 22.7360 2 6 7 -11 21.6391 31.8011 2 6 7 -11 24.5685 26.8963 2 5 -7 -11 72.5034 21.0648 2 5 7 -11 24.0018 32.4853 2 5 7 -11 27.7840 21.8281 2 4 -7 -11 48.3042 17.6105 2 -4 7 11 48.2141 28.9011 2 4 7 -11 24.7768 31.3494 2 4 7 -11 36.5779 25.4919 2 4 7 -11 58.1614 25.7255 2 -3 -7 11 179.602 41.2829 2 3 -7 -11 199.229 27.1890 2 3 7 -11 175.994 34.4519 2 -3 7 11 215.249 45.2880 2 3 7 -11 210.042 48.0816 2 3 7 -11 232.171 36.5064 2 -2 -7 11 554.462 53.3628 2 2 -7 -11 441.635 34.0728 2 2 7 -11 449.122 47.2477 2 -2 7 11 376.328 50.8251 2 2 7 -11 491.889 59.0598 2 -1 -7 11 42.5863 23.2444 2 1 -7 -11 10.1274 11.6788 2 -1 7 11 1.12121 20.8401 2 1 7 -11 37.5952 28.8211 2 1 7 -11 -0.8343 16.6503 2 0 -7 -11 7.51406 14.2594 2 0 -7 11 3.13001 22.8619 2 0 -7 -11 3.25251 12.3439 2 0 -7 11 14.6171 21.1598 2 0 7 -11 -0.5339 22.4688 2 0 7 11 8.00906 22.6070 2 -1 -7 -11 3.79789 15.6856 2 1 -7 11 2.61464 18.5184 2 1 -7 11 1.83563 25.2240 2 -1 -7 -11 10.4252 15.8840 2 1 7 11 19.4934 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354.169 19.2130 2 0 2 12 329.729 36.8246 2 0 2 12 313.645 26.4409 2 1 -2 12 177.505 23.1671 2 -1 -2 -12 196.998 18.6242 2 1 -2 12 110.066 23.1843 2 -1 2 -12 195.245 26.6567 2 1 2 12 198.849 16.7742 2 1 2 12 134.439 30.8680 2 1 2 12 167.510 17.7851 2 1 2 12 188.685 23.3232 2 2 -2 12 891.471 53.0854 2 2 -2 12 861.477 49.3049 2 2 -2 12 841.077 52.3063 2 -2 2 -12 868.751 51.8256 2 2 2 12 860.917 60.9410 2 2 2 12 896.276 43.5858 2 2 2 12 866.384 50.9906 2 2 2 12 901.471 40.0510 2 2 2 12 904.522 44.3927 2 3 -2 12 959.599 56.8581 2 3 -2 12 856.429 54.1735 2 3 -2 12 798.082 51.3064 2 3 2 12 859.670 53.0607 2 3 2 12 872.351 43.7660 2 3 2 12 786.594 60.5883 2 -3 2 -12 780.155 51.7078 2 3 2 12 819.061 47.1169 2 3 2 12 924.767 47.4774 2 4 -2 12 576.748 47.6216 2 4 -2 12 612.098 47.0513 2 4 -2 12 644.570 48.4665 2 4 2 12 543.705 54.0843 2 4 2 12 559.788 39.3822 2 -4 2 -12 603.706 47.0342 2 4 2 12 605.799 42.2821 2 4 2 12 631.848 44.4245 2 5 -2 12 424.654 43.2409 2 5 -2 12 271.525 38.7708 2 5 -2 12 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1379.14 61.6481 2 2 -3 12 727.879 47.3138 2 2 -3 12 677.013 49.8811 2 -2 -3 -12 588.277 46.3314 2 -2 3 -12 737.649 51.6417 2 2 3 12 831.828 62.1954 2 2 3 12 775.550 39.8939 2 2 3 12 762.734 39.8637 2 2 3 12 752.386 40.0904 2 3 -3 12 209.316 29.2102 2 3 -3 12 209.067 31.4618 2 3 -3 12 198.765 31.0099 2 3 3 12 179.234 37.2205 2 -3 3 -12 215.238 30.4826 2 3 3 12 200.775 23.6408 2 3 3 12 218.086 25.8231 2 3 3 12 209.594 24.8617 2 4 -3 12 289.969 37.7288 2 4 -3 12 307.602 39.3948 2 4 -3 12 228.617 31.9295 2 -4 3 -12 359.276 39.0437 2 4 3 12 311.825 31.6422 2 4 3 12 337.761 46.8201 2 4 3 12 304.452 32.9730 2 4 3 12 331.381 32.7841 2 5 -3 12 152.647 28.7627 2 5 -3 12 184.515 36.6008 2 5 -3 12 221.922 37.1857 2 5 3 12 145.702 38.7876 2 5 3 12 153.907 26.4419 2 5 3 12 152.319 29.3862 2 5 3 12 197.733 31.5550 2 -5 3 -12 184.773 32.0888 2 6 -3 12 280.155 42.6588 2 6 -3 12 238.221 36.3471 2 6 -3 12 254.209 40.8527 2 6 3 12 218.774 36.1843 2 6 3 12 257.564 34.8675 2 6 3 12 212.587 45.7996 2 -6 3 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44.9551 2 4 -5 14 13.2983 18.2921 2 -4 -5 -14 -7.1041 16.9169 2 4 -5 14 2.11048 23.6137 2 4 -5 14 46.3258 23.6077 2 4 5 14 27.3418 19.0119 2 4 5 14 29.6206 28.8636 2 4 5 14 66.0002 21.9813 2 -4 5 -14 26.8322 23.5970 2 5 -5 14 202.056 41.9783 2 -5 -5 -14 132.739 35.2076 2 5 -5 14 146.885 40.6771 2 5 -5 14 115.926 30.8606 2 5 5 14 149.728 30.6295 2 5 5 14 142.064 29.0437 2 -5 5 -14 122.609 35.0680 2 5 5 14 151.788 46.7506 2 6 -5 14 228.039 39.5853 2 -6 -5 -14 201.146 40.9912 2 6 -5 14 148.090 42.7895 2 6 5 14 159.525 33.5407 2 6 5 14 167.376 49.0360 2 6 5 14 176.827 34.6234 2 -6 5 -14 224.284 42.7376 2 7 -5 14 388.312 56.9628 2 -7 -5 -14 276.455 46.6255 2 7 -5 14 290.142 45.9824 2 7 5 14 268.191 41.2052 2 -7 5 -14 338.282 50.9863 2 7 5 14 325.400 58.9022 2 7 5 14 283.930 45.0776 2 -8 -5 -14 313.148 50.5994 2 8 -5 14 209.595 51.9918 2 8 5 14 256.082 59.5904 2 -8 5 -14 269.146 48.7317 2 8 5 14 234.357 45.2910 2 7 6 -14 64.1696 40.1730 2 6 6 -14 80.4168 39.4798 2 5 6 -14 448.874 61.4282 2 4 6 -14 84.6167 34.1423 2 3 6 -14 60.7217 31.5437 2 -3 6 14 32.6734 23.6608 2 2 -6 -14 535.157 45.5497 2 -2 6 14 715.232 63.5653 2 2 6 -14 719.996 67.5387 2 1 -6 -14 204.109 31.6547 2 -1 6 14 171.177 44.1344 2 1 6 -14 201.601 33.2754 2 1 6 -14 157.205 38.6960 2 ; _database_code_depnum_ccdc_archive 'CCDC 947989' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rao03 _audit_creation_method SHELXL-97 _chemical_name_systematic ; rao03 ; _chemical_name_common Fe-A-2 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H31 Fe N6 O12' _chemical_formula_weight 483.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.102(4) _cell_length_b 11.929(3) _cell_length_c 12.857(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.976(3) _cell_angle_gamma 90.00 _cell_volume 2161.5(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 25.41 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9138 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details SADABS _diffrn_refln_scan_width 0.5 _diffrn_refln_scan_rate 10 _space_group.centring_type primitive _space_group.IT_number 14 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-I CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 47520 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.0108 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.44 _diffrn_reflns_theta_max 25.42 _reflns_number_total 3972 _reflns_number_gt 3739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution SIR-97 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+1.7492P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3972 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0265 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0653 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.10478(10) 0.15525(12) 0.49845(11) 0.0120(3) Uani 1 1 d . . . C2 C 1.19385(11) 0.15714(13) 0.43824(12) 0.0164(3) Uani 1 1 d . . . H2A H 1.1859 0.1090 0.3758 0.020 Uiso 1 1 calc R . . H2B H 1.2472 0.1271 0.4819 0.020 Uiso 1 1 calc R . . C3 C 1.21630(11) 0.27810(13) 0.40494(13) 0.0179(3) Uani 1 1 d . . . H3A H 1.2389 0.3214 0.4666 0.021 Uiso 1 1 calc R . . H3B H 1.2678 0.2769 0.3546 0.021 Uiso 1 1 calc R . . C4 C 1.12920(11) 0.33611(13) 0.35524(12) 0.0171(3) Uani 1 1 d . . . H4A H 1.1429 0.4167 0.3448 0.021 Uiso 1 1 calc R . . H4B H 1.1137 0.3023 0.2864 0.021 Uiso 1 1 calc R . . C5 C 1.04696(10) 0.32337(12) 0.42431(11) 0.0130(3) Uani 1 1 d . . . C6 C 0.76417(11) 0.22205(12) 0.70919(11) 0.0121(3) Uani 1 1 d . . . C7 C 0.66854(11) 0.20739(13) 0.75445(12) 0.0164(3) Uani 1 1 d . . . H7A H 0.6284 0.2737 0.7385 0.020 Uiso 1 1 calc R . . H7B H 0.6752 0.1996 0.8310 0.020 Uiso 1 1 calc R . . C8 C 0.62232(11) 0.10189(14) 0.70715(12) 0.0176(3) Uani 1 1 d . . . H8A H 0.6586 0.0348 0.7303 0.021 Uiso 1 1 calc R . . H8B H 0.5568 0.0946 0.7315 0.021 Uiso 1 1 calc R . . C9 C 0.62033(10) 0.10878(14) 0.58821(12) 0.0165(3) Uani 1 1 d . . . H9A H 0.5966 0.0372 0.5583 0.020 Uiso 1 1 calc R . . H9B H 0.5767 0.1694 0.5645 0.020 Uiso 1 1 calc R . . C10 C 0.71837(10) 0.13182(12) 0.55087(11) 0.0116(3) Uani 1 1 d . . . N1 N 1.08259(8) 0.07550(10) 0.56188(9) 0.0121(3) Uani 1 1 d . . . H1 H 1.1219 0.0197 0.5754 0.015 Uiso 1 1 calc R . . N2 N 1.03808(9) 0.23541(11) 0.48878(10) 0.0126(3) Uani 1 1 d . . . N3 N 0.97642(9) 0.39281(11) 0.42719(10) 0.0139(3) Uani 1 1 d . . . H3 H 0.9747 0.4532 0.3878 0.017 Uiso 1 1 calc R . . N4 N 0.83524(9) 0.26970(11) 0.75878(10) 0.0133(3) Uani 1 1 d . . . H4 H 0.8295 0.2962 0.8221 0.016 Uiso 1 1 calc R . . N5 N 0.78380(9) 0.18656(11) 0.61371(9) 0.0123(3) Uani 1 1 d . . . N6 N 0.74447(8) 0.10020(10) 0.46027(9) 0.0123(3) Uani 1 1 d . . . O1 O 0.99621(7) 0.08074(9) 0.60708(8) 0.0137(2) Uani 1 1 d . . . O2 O 0.90470(7) 0.37004(9) 0.49279(8) 0.0167(2) Uani 1 1 d . . . O3 O 0.91937(7) 0.27724(9) 0.70892(8) 0.0153(2) Uani 1 1 d . . . O4 O 0.84092(7) 0.13054(9) 0.44393(7) 0.0120(2) Uani 1 1 d . . . O5 O 1.04074(7) 0.44775(9) 0.72810(8) 0.0155(2) Uani 1 1 d . . . H5X H 1.0318 0.4830 0.7769 0.019 Uiso 1 1 d R . . H5Y H 1.0011 0.4011 0.7245 0.019 Uiso 1 1 d R . . O6 O 0.78464(9) 0.64262(12) 0.33468(10) 0.0335(3) Uani 1 1 d . . . H6X H 0.8332 0.6266 0.3099 0.040 Uiso 1 1 d R . . H6Y H 0.7664 0.5901 0.3644 0.040 Uiso 1 1 d R . . O7 O 0.73240(8) 0.46014(11) 0.44511(10) 0.0292(3) Uani 1 1 d . . . H7X H 0.7005 0.4617 0.4932 0.035 Uiso 1 1 d R . . H7Y H 0.7805 0.4270 0.4597 0.035 Uiso 1 1 d R . . O8 O 0.60214(8) 0.47939(10) 0.60076(9) 0.0224(3) Uani 1 1 d . . . H8X H 0.6094 0.4822 0.6615 0.027 Uiso 1 1 d R . . H8Y H 0.5697 0.4395 0.5836 0.027 Uiso 1 1 d R . . O9 O 0.46973(8) 0.33186(10) 0.50404(9) 0.0227(3) Uani 1 1 d . . . H9X H 0.4452 0.3041 0.5413 0.027 Uiso 1 1 d R . . H9Y H 0.4463 0.3803 0.4721 0.027 Uiso 1 1 d R . . O10 O 0.46556(8) 0.33572(10) 0.84809(9) 0.0260(3) Uani 1 1 d . . . H10X H 0.5053 0.3789 0.8425 0.031 Uiso 1 1 d R . . H10Y H 0.4736 0.2999 0.8824 0.031 Uiso 1 1 d R . . O11 O 0.61566(8) 0.00168(9) 0.31641(8) 0.0196(2) Uani 1 1 d . . . H11X H 0.6573 0.0288 0.3544 0.023 Uiso 1 1 d R . . H11Y H 0.6170 -0.0550 0.3233 0.023 Uiso 1 1 d R . . O12 O 1.37860(8) 0.26392(10) 0.17170(9) 0.0215(3) Uani 1 1 d . . . H12X H 1.3302 0.2374 0.1741 0.026 Uiso 1 1 d R . . H12Y H 1.4057 0.2370 0.2188 0.026 Uiso 1 1 d R . . Fe1 Fe 0.914118(14) 0.214890(17) 0.562189(15) 0.01021(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0120(7) 0.0138(7) 0.0101(7) -0.0031(6) -0.0013(5) -0.0012(6) C2 0.0142(7) 0.0192(8) 0.0160(7) 0.0004(6) 0.0031(6) 0.0011(6) C3 0.0141(8) 0.0215(8) 0.0183(8) 0.0010(6) 0.0048(6) -0.0027(6) C4 0.0188(8) 0.0175(8) 0.0154(7) 0.0023(6) 0.0061(6) -0.0017(6) C5 0.0157(7) 0.0118(7) 0.0115(7) -0.0013(6) 0.0001(6) -0.0035(6) C6 0.0141(7) 0.0113(7) 0.0109(7) 0.0005(5) 0.0016(6) 0.0006(5) C7 0.0141(7) 0.0209(8) 0.0145(7) -0.0034(6) 0.0049(6) -0.0016(6) C8 0.0135(7) 0.0225(8) 0.0169(8) -0.0011(6) 0.0045(6) -0.0047(6) C9 0.0121(7) 0.0207(8) 0.0165(8) -0.0017(6) -0.0001(6) -0.0022(6) C10 0.0124(7) 0.0100(7) 0.0123(7) 0.0014(6) -0.0014(5) 0.0004(5) N1 0.0102(6) 0.0135(6) 0.0126(6) -0.0005(5) 0.0004(5) 0.0017(5) N2 0.0131(6) 0.0126(6) 0.0123(6) -0.0001(5) 0.0019(5) -0.0014(5) N3 0.0158(6) 0.0120(6) 0.0141(6) 0.0024(5) 0.0044(5) -0.0016(5) N4 0.0137(6) 0.0172(6) 0.0092(6) -0.0025(5) 0.0037(5) -0.0015(5) N5 0.0122(6) 0.0140(6) 0.0107(6) -0.0014(5) 0.0007(5) -0.0013(5) N6 0.0107(6) 0.0136(6) 0.0127(6) 0.0013(5) -0.0008(5) -0.0010(5) O1 0.0115(5) 0.0155(5) 0.0142(5) 0.0022(4) 0.0035(4) 0.0003(4) O2 0.0158(5) 0.0152(5) 0.0197(5) 0.0034(4) 0.0089(4) 0.0013(4) O3 0.0123(5) 0.0215(6) 0.0123(5) -0.0047(4) 0.0039(4) -0.0044(4) O4 0.0111(5) 0.0150(5) 0.0098(5) 0.0003(4) 0.0015(4) -0.0006(4) O5 0.0185(5) 0.0135(5) 0.0147(5) -0.0031(4) 0.0040(4) -0.0034(4) O6 0.0279(7) 0.0393(8) 0.0341(7) 0.0120(6) 0.0125(6) 0.0121(6) O7 0.0199(6) 0.0405(8) 0.0275(7) 0.0048(6) 0.0049(5) 0.0092(5) O8 0.0247(6) 0.0249(6) 0.0175(6) 0.0005(5) -0.0011(5) -0.0024(5) O9 0.0277(6) 0.0206(6) 0.0198(6) 0.0054(5) 0.0015(5) 0.0018(5) O10 0.0251(6) 0.0244(6) 0.0286(7) 0.0059(5) 0.0012(5) -0.0032(5) O11 0.0201(6) 0.0172(6) 0.0209(6) -0.0020(5) -0.0069(4) -0.0021(4) O12 0.0210(6) 0.0219(6) 0.0215(6) 0.0012(5) -0.0015(5) -0.0012(5) Fe1 0.01061(12) 0.01113(12) 0.00898(12) -0.00033(7) 0.00158(8) -0.00124(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.298(2) . ? C1 N2 1.344(2) . ? C1 C2 1.498(2) . ? C2 C3 1.541(2) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.530(2) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.493(2) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.296(2) . ? C5 N2 1.346(2) . ? C6 N4 1.300(2) . ? C6 N5 1.336(2) . ? C6 C7 1.497(2) . ? C7 C8 1.533(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.531(2) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.504(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N6 1.290(2) . ? C10 N5 1.3707(19) . ? N1 O1 1.3690(16) . ? N1 H1 0.8800 . ? N2 Fe1 2.0298(13) . ? N3 O2 1.3664(16) . ? N3 H3 0.8800 . ? N4 O3 1.3707(16) . ? N4 H4 0.8800 . ? N5 Fe1 2.0035(13) . ? N6 O4 1.4299(15) . ? O1 Fe1 2.0465(11) . ? O2 Fe1 2.0569(12) . ? O3 Fe1 2.0268(11) . ? O4 Fe1 2.0692(11) . ? O5 H5X 0.7691 . ? O5 H5Y 0.7886 . ? O6 H6X 0.7883 . ? O6 H6Y 0.7816 . ? O7 H7X 0.7768 . ? O7 H7Y 0.8013 . ? O8 H8X 0.7853 . ? O8 H8Y 0.6913 . ? O9 H9X 0.6862 . ? O9 H9Y 0.7760 . ? O10 H10X 0.7665 . ? O10 H10Y 0.6217 . ? O11 H11X 0.8173 . ? O11 H11Y 0.6825 . ? O12 H12X 0.7542 . ? O12 H12Y 0.7745 . ? 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_3 _geom_angle_publ_flag N1 C1 N2 113.35(13) . . ? N1 C1 C2 124.06(13) . . ? N2 C1 C2 122.55(13) . . ? C1 C2 C3 109.97(13) . . ? C1 C2 H2A 109.7 . . ? C3 C2 H2A 109.7 . . ? C1 C2 H2B 109.7 . . ? C3 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C4 C3 C2 111.71(13) . . ? C4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 109.53(13) . . ? C5 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? C5 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N3 C5 N2 113.14(13) . . ? N3 C5 C4 124.39(14) . . ? N2 C5 C4 122.45(13) . . ? N4 C6 N5 114.11(13) . . ? N4 C6 C7 123.36(13) . . ? N5 C6 C7 122.54(13) . . ? C6 C7 C8 108.54(12) . . ? C6 C7 H7A 110.0 . . ? C8 C7 H7A 110.0 . . ? C6 C7 H7B 110.0 . . ? C8 C7 H7B 110.0 . . ? H7A C7 H7B 108.4 . . ? C9 C8 C7 110.19(13) . . ? C9 C8 H8A 109.6 . . ? C7 C8 H8A 109.6 . . ? C9 C8 H8B 109.6 . . ? C7 C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 110.07(12) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? N6 C10 N5 117.66(13) . . ? N6 C10 C9 121.91(13) . . ? N5 C10 C9 120.42(13) . . ? C1 N1 O1 118.06(12) . . ? C1 N1 H1 121.0 . . ? O1 N1 H1 121.0 . . ? C1 N2 C5 122.14(13) . . ? C1 N2 Fe1 118.84(10) . . ? C5 N2 Fe1 118.71(10) . . ? C5 N3 O2 118.41(12) . . ? C5 N3 H3 120.8 . . ? O2 N3 H3 120.8 . . ? C6 N4 O3 117.67(12) . . ? C6 N4 H4 121.2 . . ? O3 N4 H4 121.2 . . ? C6 N5 C10 122.39(13) . . ? C6 N5 Fe1 118.14(10) . . ? C10 N5 Fe1 119.47(10) . . ? C10 N6 O4 111.17(11) . . ? N1 O1 Fe1 114.77(8) . . ? N3 O2 Fe1 114.12(8) . . ? N4 O3 Fe1 114.00(8) . . ? N6 O4 Fe1 117.91(8) . . ? H5X O5 H5Y 107.3 . . ? H6X O6 H6Y 107.9 . . ? H7X O7 H7Y 109.5 . . ? H8X O8 H8Y 114.2 . . ? H9X O9 H9Y 120.9 . . ? H10X O10 H10Y 114.3 . . ? H11X O11 H11Y 107.4 . . ? H12X O12 H12Y 102.5 . . ? N5 Fe1 O3 76.03(5) . . ? N5 Fe1 N2 171.31(5) . . ? O3 Fe1 N2 112.59(5) . . ? N5 Fe1 O1 106.93(5) . . ? O3 Fe1 O1 91.28(4) . . ? N2 Fe1 O1 74.79(5) . . ? N5 Fe1 O2 104.41(5) . . ? O3 Fe1 O2 94.20(5) . . ? N2 Fe1 O2 74.55(5) . . ? O1 Fe1 O2 148.58(4) . . ? N5 Fe1 O4 73.79(5) . . ? O3 Fe1 O4 149.73(4) . . ? N2 Fe1 O4 97.63(5) . . ? O1 Fe1 O4 95.16(4) . . ? O2 Fe1 O4 95.49(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.420 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.052 _iucr_refine_instructions_details ; TITL rao03_0ma in P2(1)/c CELL 0.71073 14.1017 11.9292 12.8569 90.000 91.976 90.000 ZERR 4.00 0.0035 0.0030 0.0032 0.000 0.003 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O FE UNIT 40 124 24 48 4 MERG 2 FMAP 2 PLAN 25 SIZE 0.04 0.10 0.12 ACTA 50.00 BOND $H LIST 4 WPDB -2 L.S. 8 TEMP -173.00 WGHT 0.032200 1.749200 FVAR 0.13080 C1 1 1.104781 0.155251 0.498451 11.00000 0.01203 0.01377 = 0.01014 -0.00311 -0.00128 -0.00118 C2 1 1.193854 0.157144 0.438242 11.00000 0.01420 0.01924 = 0.01602 0.00043 0.00313 0.00114 AFIX 23 H2A 2 1.185906 0.109002 0.375828 11.00000 -1.20000 H2B 2 1.247233 0.127127 0.481851 11.00000 -1.20000 AFIX 0 C3 1 1.216297 0.278097 0.404944 11.00000 0.01409 0.02148 = 0.01834 0.00102 0.00481 -0.00272 AFIX 23 H3A 2 1.238926 0.321437 0.466601 11.00000 -1.20000 H3B 2 1.267822 0.276855 0.354568 11.00000 -1.20000 AFIX 0 C4 1 1.129200 0.336111 0.355236 11.00000 0.01878 0.01748 = 0.01541 0.00234 0.00608 -0.00173 AFIX 23 H4A 2 1.142871 0.416658 0.344827 11.00000 -1.20000 H4B 2 1.113704 0.302285 0.286417 11.00000 -1.20000 AFIX 0 C5 1 1.046959 0.323373 0.424308 11.00000 0.01573 0.01179 = 0.01145 -0.00127 0.00010 -0.00347 C6 1 0.764168 0.222052 0.709185 11.00000 0.01412 0.01125 = 0.01087 0.00049 0.00157 0.00059 C7 1 0.668544 0.207386 0.754452 11.00000 0.01408 0.02089 = 0.01449 -0.00339 0.00492 -0.00157 AFIX 23 H7A 2 0.628436 0.273716 0.738489 11.00000 -1.20000 H7B 2 0.675194 0.199602 0.831018 11.00000 -1.20000 AFIX 0 C8 1 0.622324 0.101893 0.707154 11.00000 0.01353 0.02251 = 0.01694 -0.00105 0.00448 -0.00467 AFIX 23 H8A 2 0.658588 0.034821 0.730346 11.00000 -1.20000 H8B 2 0.556782 0.094553 0.731528 11.00000 -1.20000 AFIX 0 C9 1 0.620329 0.108778 0.588212 11.00000 0.01209 0.02075 = 0.01653 -0.00168 -0.00006 -0.00222 AFIX 23 H9A 2 0.596552 0.037223 0.558294 11.00000 -1.20000 H9B 2 0.576736 0.169368 0.564534 11.00000 -1.20000 AFIX 0 C10 1 0.718371 0.131819 0.550873 11.00000 0.01236 0.01000 = 0.01235 0.00144 -0.00143 0.00042 N1 3 1.082586 0.075496 0.561876 11.00000 0.01023 0.01351 = 0.01260 -0.00051 0.00039 0.00170 AFIX 43 H1 2 1.121918 0.019693 0.575410 11.00000 -1.20000 AFIX 0 N2 3 1.038078 0.235409 0.488784 11.00000 0.01308 0.01261 = 0.01225 -0.00009 0.00194 -0.00141 N3 3 0.976415 0.392815 0.427186 11.00000 0.01580 0.01197 = 0.01409 0.00236 0.00437 -0.00162 AFIX 43 H3 2 0.974747 0.453185 0.387830 11.00000 -1.20000 AFIX 0 N4 3 0.835241 0.269701 0.758780 11.00000 0.01367 0.01720 = 0.00919 -0.00253 0.00368 -0.00148 AFIX 43 H4 2 0.829540 0.296187 0.822140 11.00000 -1.20000 AFIX 0 N5 3 0.783797 0.186564 0.613706 11.00000 0.01222 0.01395 = 0.01066 -0.00143 0.00068 -0.00134 N6 3 0.744470 0.100196 0.460274 11.00000 0.01065 0.01356 = 0.01271 0.00134 -0.00084 -0.00104 O1 4 0.996212 0.080743 0.607084 11.00000 0.01149 0.01555 = 0.01423 0.00217 0.00352 0.00027 O2 4 0.904697 0.370040 0.492793 11.00000 0.01579 0.01519 = 0.01974 0.00343 0.00887 0.00126 O3 4 0.919365 0.277238 0.708922 11.00000 0.01230 0.02148 = 0.01232 -0.00471 0.00391 -0.00444 O4 4 0.840918 0.130540 0.443932 11.00000 0.01114 0.01504 = 0.00983 0.00028 0.00150 -0.00063 O5 4 1.040738 0.447754 0.728095 11.00000 0.01854 0.01354 = 0.01472 -0.00313 0.00402 -0.00335 AFIX 3 H5X 2 1.031760 0.483012 0.776865 11.00000 -1.20000 H5Y 2 1.001128 0.401120 0.724522 11.00000 -1.20000 AFIX 0 O6 4 0.784644 0.642617 0.334683 11.00000 0.02787 0.03934 = 0.03414 0.01197 0.01246 0.01205 AFIX 3 H6X 2 0.833172 0.626610 0.309889 11.00000 -1.20000 H6Y 2 0.766445 0.590102 0.364390 11.00000 -1.20000 AFIX 0 O7 4 0.732400 0.460137 0.445114 11.00000 0.01992 0.04048 = 0.02752 0.00476 0.00487 0.00921 AFIX 3 H7X 2 0.700502 0.461692 0.493164 11.00000 -1.20000 H7Y 2 0.780460 0.426983 0.459705 11.00000 -1.20000 AFIX 0 O8 4 0.602143 0.479389 0.600757 11.00000 0.02472 0.02494 = 0.01753 0.00047 -0.00109 -0.00240 AFIX 3 H8X 2 0.609449 0.482160 0.661534 11.00000 -1.20000 H8Y 2 0.569711 0.439461 0.583565 11.00000 -1.20000 AFIX 0 O9 4 0.469731 0.331858 0.504038 11.00000 0.02767 0.02061 = 0.01980 0.00536 0.00145 0.00177 AFIX 3 H9X 2 0.445186 0.304110 0.541343 11.00000 -1.20000 H9Y 2 0.446344 0.380314 0.472092 11.00000 -1.20000 AFIX 0 O10 4 0.465560 0.335720 0.848092 11.00000 0.02505 0.02437 = 0.02857 0.00590 0.00115 -0.00317 AFIX 3 H10X 2 0.505317 0.378896 0.842511 11.00000 -1.20000 H10Y 2 0.473649 0.299889 0.882372 11.00000 -1.20000 AFIX 0 O11 4 0.615663 0.001675 0.316414 11.00000 0.02009 0.01718 = 0.02089 -0.00197 -0.00692 -0.00208 AFIX 3 H11X 2 0.657309 0.028831 0.354351 11.00000 -1.20000 H11Y 2 0.617030 -0.055041 0.323288 11.00000 -1.20000 AFIX 0 O12 4 1.378600 0.263921 0.171702 11.00000 0.02103 0.02186 = 0.02147 0.00123 -0.00154 -0.00120 AFIX 3 H12X 2 1.330168 0.237414 0.174118 11.00000 -1.20000 H12Y 2 1.405682 0.236969 0.218790 11.00000 -1.20000 AFIX 0 FE1 5 0.914118 0.214890 0.562189 11.00000 0.01061 0.01113 = 0.00898 -0.00033 0.00158 -0.00124 HKLF 4 REM rao03_0ma in P2(1)/c REM R1 = 0.0247 for 3739 Fo > 4sig(Fo) and 0.0265 for all 3972 data REM 262 parameters refined using 0 restraints END WGHT 0.0322 1.7492 REM Highest difference peak 0.420, deepest hole -0.440, 1-sigma level 0.052 Q1 1 0.8366 0.2031 0.5957 11.00000 0.05 0.42 Q2 1 0.9915 0.2243 0.5095 11.00000 0.05 0.37 Q3 1 0.7164 0.2141 0.7310 11.00000 0.05 0.36 Q4 1 0.6706 0.1195 0.5667 11.00000 0.05 0.31 Q5 1 1.1432 0.1514 0.4668 11.00000 0.05 0.29 Q6 1 1.0440 0.2688 0.4555 11.00000 0.05 0.28 Q7 1 0.7465 0.1658 0.5830 11.00000 0.05 0.28 Q8 1 1.2024 0.2172 0.4186 11.00000 0.05 0.28 Q9 1 0.6223 0.1052 0.6491 11.00000 0.05 0.27 Q10 1 0.4458 0.3118 0.7853 11.00000 0.05 0.27 Q11 1 0.5241 0.3790 0.5464 11.00000 0.05 0.27 Q12 1 0.4668 0.2642 0.4473 11.00000 0.05 0.26 Q13 1 0.9184 0.2320 0.6625 11.00000 0.05 0.26 Q14 1 0.7801 0.1903 0.6561 11.00000 0.05 0.26 Q15 1 0.7211 0.1403 0.4976 11.00000 0.05 0.26 Q16 1 0.6476 0.1556 0.7288 11.00000 0.05 0.25 Q17 1 0.5798 0.5465 0.5670 11.00000 0.05 0.25 Q18 1 1.0385 0.0822 0.5830 11.00000 0.05 0.24 Q19 1 1.0973 0.0040 0.5466 11.00000 0.05 0.24 Q20 1 0.7910 0.1177 0.4521 11.00000 0.05 0.23 Q21 1 1.0625 0.1918 0.4805 11.00000 0.05 0.23 Q22 1 0.9394 0.3765 0.4654 11.00000 0.05 0.22 Q23 1 1.3834 0.3394 0.1614 11.00000 0.05 0.22 Q24 1 0.9755 0.1297 0.5972 11.00000 0.05 0.22 Q25 1 0.7412 0.0914 0.5136 11.00000 0.05 0.21 ; _database_code_depnum_ccdc_archive 'CCDC 947990'