Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Buchanan, Robert' 'Cheruzel, Lionel E.' 'Mashuta, Mark S.' 'Wang, Jianping' _publ_contact_author_name 'Prof Robert Buchanan' _publ_contact_author_address ; Chemistry University of Louisville Department of Chemistry Louisville Kentucky 40292 UNITED STATES OF AMERICA ; _publ_contact_author_phone '502-852-6580' _publ_contact_author_fax '502-852-8149' _publ_contact_author_email 'bob.buchanan@louisville.edu' _publ_section_title ; Structure and properties of an Fe(III) complex containing a novel amide functionalized polyimidazole ligand. ; _publ_requested_journal 'test' _publ_requested_category FO _publ_requested_coeditor_name 'Professor Carol P. Brock' _publ_contact_letter ; April 17, 2002 Please consider this CIF submission for publication in J. Chem. Soc. Chem. Comm. . All authors have seen and approved this submission. The CIF has passed the Chester CHECKCIF routines and gives a satisfactory PRINTCIF file. The space group Cmca appears incorrectly as Cm~ca~ in the PRINTCIF and generates a 128_Alert C error which I am unable to correct. Your technical assistance here is greatly appreciated. When you reply by e-mail with your reference number I will send a signed Copyright Transfer Form. The Structure Factor Listing (in CIF format) and all artwork (diagrams, figures) as encapsulated PostScript files will be transferred to Chester by ftp as instructed in Notes for Authors. Best regards, Robert M. Buchanan ; _publ_section_exptl_refinement ; All non-H atoms were refined anisotropically. All hydrogen atoms were calculated except for the amide hydrogen atom H8n which was located by difference maps and refined. All other hydrogen atoms were allowed to ride on the attached atom. ; _publ_section_acknowledgements ; We thank the Kentucky Research Challenge Trust Fund for the purchase of CCD X-ray equipment and upgrade of our X-ray facility. ; data_1 _database_code_CSD 186290 _audit_creation_method SHELXL-97 _chemical_name_systematic ; dichloro tris((1-methylimidazol-2-yl)methyl)amine iron(III) perchlorate hemiacetonitrile ; _chemical_name_common '[(tmima)FeCl~2~]ClO~4~ ^.^ 0.5CH~3~CN' _chemical_melting_point ? _chemical_formula_moiety 'C15 H21 Cl2 Fe N7, Cl O4, 0.5(C2 N)' _chemical_formula_sum 'C16 H21 Cl3 Fe N7.5 O4' _chemical_formula_weight 544.60 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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.0262(10) _cell_length_b 9.8000(10) _cell_length_c 22.5631(10) _cell_angle_alpha 90.00 _cell_angle_beta 113.951(10) _cell_angle_gamma 90.00 _cell_volume 4653.1(6) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4351 _cell_measurement_theta_min 2.13 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 1.54 _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'picnometry' _exptl_crystal_F_000 2228 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.697 _exptl_absorpt_correction_T_max 0.721 _exptl_absorpt_process_details empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CAD4' _diffrn_measurement_method '\w/\2o scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 4180 _diffrn_reflns_av_R_equivalents 0.0091 _diffrn_reflns_av_sigmaI/netI 0.0190 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4067 _reflns_number_gt 3327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf Nonius CAD4 diffractometer control' _computing_cell_refinement 25 _computing_data_reduction 'Enraf Nonius CAD4 diffractometer control' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.12 (Bruker, 2001)' _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^)+(0.0966P)^2^+14.4655P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00070(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4067 _refine_ls_number_parameters 281 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1702 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.050 _refine_ls_shift/su_mean 0.026 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 Fe1 Fe 0.17588(3) 1.13856(6) 0.64198(3) 0.0392(2) Uani 1 1 d . . . Cl1 Cl 0.15420(8) 1.36067(12) 0.64177(6) 0.0643(4) Uani 1 1 d . . . Cl2 Cl 0.17864(6) 1.07842(11) 0.74302(5) 0.0549(3) Uani 1 1 d . . . N1 N 0.20483(16) 0.9163(3) 0.62107(16) 0.0404(8) Uani 1 1 d . . . N2 N 0.09093(17) 1.0320(4) 0.60112(17) 0.0481(9) Uani 1 1 d . . . N3 N 0.0347(2) 0.8434(5) 0.5814(2) 0.0621(11) Uani 1 1 d . . . N4 N 0.27450(17) 1.1349(4) 0.68137(17) 0.0447(8) Uani 1 1 d . . . N5 N 0.36609(18) 1.0299(4) 0.72637(18) 0.0530(10) Uani 1 1 d . . . N6 N 0.17580(16) 1.1545(3) 0.54896(16) 0.0414(8) Uani 1 1 d . . . N7 N 0.19006(18) 1.0766(4) 0.46519(17) 0.0478(9) Uani 1 1 d . . . C1 C 0.1541(2) 0.8210(5) 0.6198(2) 0.0512(11) Uani 1 1 d . . . H1A H 0.1499 0.7465 0.5900 0.061 Uiso 1 1 calc R . . H1B H 0.1648 0.7830 0.6627 0.061 Uiso 1 1 calc R . . C2 C 0.0931(2) 0.8978(5) 0.5985(2) 0.0497(11) Uani 1 1 d . . . C3 C 0.0279(2) 1.0659(6) 0.5849(3) 0.0635(13) Uani 1 1 d . . . H3 H 0.0120 1.1538 0.5828 0.076 Uiso 1 1 calc R . . C4 C -0.0061(3) 0.9505(7) 0.5728(3) 0.0699(15) Uani 1 1 d . . . H4 H -0.0498 0.9443 0.5608 0.084 Uiso 1 1 calc R . . C5 C 0.0185(3) 0.6995(7) 0.5736(3) 0.0876(19) Uani 1 1 d . . . H5A H 0.0561 0.6461 0.5960 0.131 Uiso 1 1 calc R . . H5B H 0.0009 0.6765 0.5284 0.131 Uiso 1 1 calc R . . H5C H -0.0121 0.6806 0.5914 0.131 Uiso 1 1 calc R . . C6 C 0.2666(2) 0.8857(4) 0.6764(2) 0.0485(10) Uani 1 1 d . . . H6A H 0.2593 0.8516 0.7131 0.058 Uiso 1 1 calc R . . H6B H 0.2898 0.8171 0.6638 0.058 Uiso 1 1 calc R . . C7 C 0.3031(2) 1.0153(5) 0.69358(19) 0.0443(10) Uani 1 1 d . . . C8 C 0.3219(3) 1.2313(5) 0.7080(2) 0.0559(12) Uani 1 1 d . . . H8 H 0.3161 1.3253 0.7073 0.067 Uiso 1 1 calc R . . C9 C 0.3779(3) 1.1656(6) 0.7352(2) 0.0632(14) Uani 1 1 d . . . H9 H 0.4176 1.2061 0.7562 0.076 Uiso 1 1 calc R . . C10 C 0.4131(2) 0.9190(7) 0.7481(3) 0.0727(16) Uani 1 1 d . . . H10A H 0.3941 0.8395 0.7577 0.109 Uiso 1 1 calc R . . H10B H 0.4489 0.9472 0.7864 0.109 Uiso 1 1 calc R . . H10C H 0.4271 0.8979 0.7145 0.109 Uiso 1 1 calc R . . C11 C 0.2128(3) 0.9167(5) 0.5594(2) 0.0550(12) Uani 1 1 d . . . H11A H 0.2571 0.9003 0.5683 0.066 Uiso 1 1 calc R . . H11B H 0.1880 0.8431 0.5322 0.066 Uiso 1 1 calc R . . C12 C 0.19272(19) 1.0471(4) 0.52436(19) 0.0409(9) Uani 1 1 d . . . C13 C 0.1609(2) 1.2572(4) 0.5033(2) 0.0457(10) Uani 1 1 d . . . H13 H 0.1471 1.3444 0.5074 0.055 Uiso 1 1 calc R . . C14 C 0.1699(2) 1.2092(5) 0.4517(2) 0.0533(11) Uani 1 1 d . . . H14 H 0.1637 1.2570 0.4139 0.064 Uiso 1 1 calc R . . C15 C 0.2079(3) 0.9859(6) 0.4235(2) 0.0681(15) Uani 1 1 d . . . H15A H 0.1966 1.0279 0.3819 0.102 Uiso 1 1 calc R . . H15B H 0.1858 0.9007 0.4183 0.102 Uiso 1 1 calc R . . H15C H 0.2529 0.9700 0.4432 0.102 Uiso 1 1 calc R . . Cl3 Cl 0.40189(6) 0.87608(13) 0.57188(6) 0.0571(3) Uani 1 1 d . . . O1A O 0.3848(7) 0.7662(14) 0.5991(7) 0.140(5) Uiso 0.50 1 d PD . . O2A O 0.3958(5) 1.0031(11) 0.6038(5) 0.099(3) Uiso 0.50 1 d PD . . O3A O 0.3566(7) 0.8893(13) 0.5052(6) 0.135(5) Uiso 0.50 1 d PD . . O4A O 0.4629(8) 0.888(2) 0.5766(10) 0.205(9) Uiso 0.50 1 d PD . . O1B O 0.4000(9) 0.731(2) 0.5763(9) 0.170(7) Uiso 0.50 1 d P . . O2B O 0.3575(7) 0.9530(15) 0.5838(6) 0.132(4) Uiso 0.50 1 d P . . O3B O 0.3948(5) 0.8990(10) 0.5071(5) 0.090(3) Uiso 0.50 1 d P . . O4B O 0.4650(6) 0.8970(14) 0.6146(7) 0.123(4) Uiso 0.50 1 d P . . N30A N 0.4877(7) 0.3558(15) 0.7183(7) 0.117(5) Uiso 0.50 1 d P . . C30A C 0.4926(7) 0.4692(13) 0.7322(6) 0.080(4) Uiso 0.50 1 d P . . C31A C 0.5000 0.6086(16) 0.7500 0.132(5) Uiso 1 2 d S . . 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 Fe1 0.0511(4) 0.0327(3) 0.0352(3) 0.0000(2) 0.0189(3) 0.0038(2) Cl1 0.1026(10) 0.0392(6) 0.0608(7) 0.0057(5) 0.0432(7) 0.0191(6) Cl2 0.0863(8) 0.0422(6) 0.0424(6) 0.0007(5) 0.0324(6) -0.0004(5) N1 0.0484(19) 0.0346(18) 0.0354(17) -0.0002(14) 0.0142(15) 0.0006(15) N2 0.048(2) 0.053(2) 0.045(2) -0.0016(17) 0.0204(17) 0.0013(17) N3 0.058(2) 0.073(3) 0.055(2) -0.006(2) 0.023(2) -0.018(2) N4 0.052(2) 0.043(2) 0.0391(18) -0.0011(15) 0.0184(16) -0.0024(16) N5 0.047(2) 0.068(3) 0.046(2) 0.0022(19) 0.0210(17) -0.0016(19) N6 0.0485(19) 0.0402(19) 0.0365(17) 0.0034(14) 0.0183(15) 0.0017(15) N7 0.057(2) 0.051(2) 0.0411(19) -0.0017(16) 0.0256(17) -0.0063(18) C1 0.061(3) 0.037(2) 0.057(3) -0.005(2) 0.024(2) -0.005(2) C2 0.054(3) 0.054(3) 0.040(2) -0.005(2) 0.018(2) -0.010(2) C3 0.050(3) 0.080(4) 0.063(3) 0.000(3) 0.025(2) 0.004(3) C4 0.048(3) 0.093(4) 0.070(3) -0.005(3) 0.025(3) -0.004(3) C5 0.085(4) 0.081(4) 0.097(5) -0.019(4) 0.037(4) -0.037(4) C6 0.056(3) 0.037(2) 0.048(2) 0.0029(18) 0.015(2) 0.0090(19) C7 0.047(2) 0.048(2) 0.037(2) 0.0004(18) 0.0163(18) 0.0039(19) C8 0.076(3) 0.052(3) 0.045(2) -0.009(2) 0.029(2) -0.020(2) C9 0.055(3) 0.084(4) 0.050(3) -0.003(3) 0.021(2) -0.020(3) C10 0.043(3) 0.104(5) 0.072(3) 0.012(3) 0.025(2) 0.020(3) C11 0.081(3) 0.044(2) 0.048(2) 0.001(2) 0.034(2) 0.014(2) C12 0.045(2) 0.042(2) 0.038(2) -0.0034(17) 0.0186(18) -0.0047(18) C13 0.053(2) 0.039(2) 0.044(2) 0.0066(18) 0.0188(19) 0.0011(19) C14 0.070(3) 0.049(3) 0.043(2) 0.010(2) 0.025(2) -0.003(2) C15 0.100(4) 0.066(3) 0.055(3) -0.008(3) 0.049(3) -0.002(3) Cl3 0.0547(7) 0.0583(7) 0.0595(7) 0.0010(5) 0.0243(6) 0.0006(5) _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 Fe1 N1 2.380(3) . yes Fe1 N2 2.074(4) . yes Fe1 N4 2.076(4) . yes Fe1 N6 2.104(3) . yes Fe1 Cl1 2.233(1) . yes Fe1 Cl2 2.331(1) . yes N1 C1 1.488(6) . no N1 C6 1.492(5) . no N1 C11 1.475(6) . no N2 C2 1.319(6) . no N2 C3 1.385(6) . no N3 C2 1.348(6) . no N3 C4 1.370(7) . no N3 C5 1.451(8) . no N4 C7 1.318(6) . no N4 C8 1.383(6) . no N5 C7 1.342(6) . no N5 C9 1.356(7) . no N5 C10 1.471(7) . no N6 C12 1.320(5) . no N6 C13 1.381(5) . no N7 C12 1.343(5) . no N7 C14 1.372(6) . no N7 C15 1.467(6) . no C1 C2 1.490(7) . no C1 H1A 0.9700 . no C1 H1B 0.9700 . no C3 C4 1.340(8) . no C3 H3 0.9300 . no C4 H4 0.9300 . no C5 H5A 0.9600 . no C5 H5B 0.9600 . no C5 H5C 0.9600 . no C6 C7 1.485(6) . no C6 H6A 0.9700 . no C6 H6B 0.9700 . no C8 C9 1.346(8) . no C8 H8 0.9300 . no C9 H9 0.9300 . no C10 H10A 0.9600 . no C10 H10B 0.9600 . no C10 H10C 0.9600 . no C11 C12 1.475(6) . no C11 H11A 0.9700 . no C11 H11B 0.9700 . no C13 C14 1.349(6) . no C13 H13 0.9300 . no C14 H14 0.9300 . no C15 H15A 0.9600 . no C15 H15B 0.9600 . no C15 H15C 0.9600 . no Cl3 O1A 1.375(14) . no Cl3 O2A 1.473(10) . no Cl3 O3A 1.447(13) . no Cl3 O4A 1.370(17) . no Cl3 O1B 1.43(2) . no Cl3 O2B 1.382(14) . no Cl3 O3B 1.421(10) . no Cl3 O4B 1.394(13) . no N30A C30A 1.148(17) . no C30A C31A 1.415(17) . no 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 Fe1 N2 74.97(14) . . yes N1 Fe1 N4 73.93(13) . . yes N1 Fe1 N6 75.93(12) . . yes N2 Fe1 N4 148.41(15) . . yes N2 Fe1 N6 88.57(14) . . yes N4 Fe1 N6 89.20(14) . . yes N1 Fe1 Cl1 166.40(9) . . yes N1 Fe1 Cl2 93.66(9) . . yes N2 Fe1 Cl1 108.68(12) . . yes N2 Fe1 Cl2 87.35(11) . . yes N4 Fe1 Cl1 102.86(11) . . yes N4 Fe1 Cl2 89.21(10) . . yes N6 Fe1 Cl1 90.92(10) . . yes N6 Fe1 Cl2 169.50(10) . . yes Cl1 Fe1 Cl2 99.55(5) . . yes C11 N1 C6 110.3(4) . . no C11 N1 C1 112.4(4) . . no C6 N1 C1 111.3(3) . . no C11 N1 Fe1 109.7(2) . . no C6 N1 Fe1 105.5(2) . . no C1 N1 Fe1 107.3(3) . . no C2 N2 C3 106.4(4) . . no C2 N2 Fe1 118.4(3) . . no C3 N2 Fe1 134.0(4) . . no C2 N3 C4 106.6(5) . . no C2 N3 C5 126.6(5) . . no C4 N3 C5 126.8(5) . . no C7 N4 C8 106.1(4) . . no C7 N4 Fe1 118.1(3) . . no C8 N4 Fe1 135.0(3) . . no C7 N5 C9 107.1(4) . . no C7 N5 C10 126.1(4) . . no C9 N5 C10 126.8(5) . . no C12 N6 C13 107.1(3) . . no C12 N6 Fe1 118.7(3) . . no C13 N6 Fe1 134.3(3) . . no C12 N7 C14 107.4(4) . . no C12 N7 C15 126.5(4) . . no C14 N7 C15 126.0(4) . . no C2 C1 N1 108.6(4) . . no C2 C1 H1A 110.0 . . no N1 C1 H1A 110.0 . . no C2 C1 H1B 110.0 . . no N1 C1 H1B 110.0 . . no H1A C1 H1B 108.3 . . no N2 C2 N3 110.8(5) . . no N2 C2 C1 122.5(4) . . no N3 C2 C1 126.3(5) . . no C4 C3 N2 108.4(5) . . no C4 C3 H3 125.8 . . no N2 C3 H3 125.8 . . no C3 C4 N3 107.8(5) . . no C3 C4 H4 126.1 . . no N3 C4 H4 126.1 . . no N3 C5 H5A 109.5 . . no N3 C5 H5B 109.5 . . no H5A C5 H5B 109.5 . . no N3 C5 H5C 109.5 . . no H5A C5 H5C 109.5 . . no H5B C5 H5C 109.5 . . no C7 C6 N1 107.0(3) . . no C7 C6 H6A 110.3 . . no N1 C6 H6A 110.3 . . no C7 C6 H6B 110.3 . . no N1 C6 H6B 110.3 . . no H6A C6 H6B 108.6 . . no N4 C7 N5 110.9(4) . . no N4 C7 C6 121.6(4) . . no N5 C7 C6 127.3(4) . . no C9 C8 N4 108.2(5) . . no C9 C8 H8 125.9 . . no N4 C8 H8 125.9 . . no C8 C9 N5 107.7(4) . . no C8 C9 H9 126.2 . . no N5 C9 H9 126.2 . . no N5 C10 H10A 109.5 . . no N5 C10 H10B 109.5 . . no H10A C10 H10B 109.5 . . no N5 C10 H10C 109.5 . . no H10A C10 H10C 109.5 . . no H10B C10 H10C 109.5 . . no C12 C11 N1 112.1(4) . . no C12 C11 H11A 109.2 . . no N1 C11 H11A 109.2 . . no C12 C11 H11B 109.2 . . no N1 C11 H11B 109.2 . . no H11A C11 H11B 107.9 . . no N6 C12 N7 110.2(4) . . no N6 C12 C11 123.1(4) . . no N7 C12 C11 126.7(4) . . no C14 C13 N6 108.2(4) . . no C14 C13 H13 125.9 . . no N6 C13 H13 125.9 . . no C13 C14 N7 107.2(4) . . no C13 C14 H14 126.4 . . no N7 C14 H14 126.4 . . no N7 C15 H15A 109.5 . . no N7 C15 H15B 109.5 . . no H15A C15 H15B 109.5 . . no N7 C15 H15C 109.5 . . no H15A C15 H15C 109.5 . . no H15B C15 H15C 109.5 . . no O1A Cl3 O2A 110.1(7) . . no O1A Cl3 O3A 108.5(7) . . no O1A Cl3 O4A 120.4(9) . . no O2A Cl3 O3A 105.1(6) . . no O2A Cl3 O4A 100.6(10) . . no O3A Cl3 O4A 110.9(9) . . no O1B Cl3 O2B 118.9(10) . . no O1B Cl3 O3B 103.6(9) . . no O1B Cl3 O4B 98.7(9) . . no O2B Cl3 O3B 109.2(7) . . no O2B Cl3 O4B 115.6(8) . . no O3B Cl3 O4B 109.8(8) . . no N30A C30A C31A 178.8(18) . . no _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.040 _refine_diff_density_min -0.722 _refine_diff_density_rms 0.088 #===END data_2 _database_code_CSD 186291 _audit_creation_method SHELXL-97 _audit_update_record ; April_17_2002 text and data added by Mark S. Mashuta ; _chemical_name_systematic ; di[bis((1-methylimidazol-2-yl)methyl)((4-tertbutylamido-1-methylimidazol- 2-yl)methyl)amine dichloroiron(III)][u-oxo-bis(trichloroferrate(III))] ; _chemical_name_common '[(^Am^tmima) FeCl~2~]~2~[Fe~2~OCl~6~]' _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 Cl2 Fe N8 O, 0.5(Cl6 Fe2 O)' _chemical_formula_sum 'C20 H30 Cl5 Fe2 N8 O1.5' _chemical_formula_weight 695.47 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' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'P2(1)/c ' _symmetry_space_group_name_Hall '-P 2ybc ' 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 11.2811(12) _cell_length_b 17.749(2) _cell_length_c 14.7148(16) _cell_angle_alpha 90.00 _cell_angle_beta 104.619(2) _cell_angle_gamma 90.00 _cell_volume 2850.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6672 _cell_measurement_theta_min 2.19 _cell_measurement_theta_max 27.78 _exptl_crystal_description 'small block' _exptl_crystal_colour orange _exptl_crystal_size_min 0.063 _exptl_crystal_size_mid 0.134 _exptl_crystal_size_max 0.147 _exptl_crystal_density_meas 1.610 _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_method 'picnometry' _exptl_crystal_F_000 1420 _exptl_absorpt_coefficient_mu 1.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.909 _exptl_absorpt_process_details ; Sheldrick, G. M.; SADABS (1996). ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% 0.1 _diffrn_reflns_number 24973 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0596 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.31 _reflns_number_total 6672 _reflns_number_gt 5240 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.624 (Bruker, 1994)' _computing_cell_refinement 'SAINT 6.2 (Bruker, 1994)' _computing_data_reduction 'SAINT 6.2 (Bruker, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker, 2001)' _computing_publication_material 'SHELXTL 6.12 (Bruker, 2001)' _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^)+(0.0171P)^2^+1.9126P] 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 mixed _refine_ls_number_reflns 6672 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.054 _refine_ls_R_factor_gt 0.036 _refine_ls_wR_factor_ref 0.084 _refine_ls_wR_factor_gt 0.078 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.05 _refine_ls_shift/su_mean 0.032 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 Fe1 Fe 0.33106(3) 0.171973(17) 0.58585(2) 0.01361(9) Uani 1 1 d . . . Cl1 Cl 0.48779(5) 0.09576(3) 0.65403(4) 0.02060(14) Uani 1 1 d . . . Cl2 Cl 0.31796(5) 0.24399(3) 0.71383(4) 0.01955(13) Uani 1 1 d . . . O1 O 0.11496(16) -0.11150(9) 0.65380(13) 0.0239(4) Uani 1 1 d . . . N1 N 0.16809(17) 0.23810(10) 0.49159(13) 0.0149(4) Uani 1 1 d . . . N2 N 0.17400(17) 0.11172(10) 0.59763(13) 0.0156(4) Uani 1 1 d . . . N3 N -0.02377(17) 0.10727(11) 0.58260(13) 0.0166(4) Uani 1 1 d . . . N4 N 0.41310(18) 0.25796(11) 0.52806(14) 0.0167(4) Uani 1 1 d . . . N5 N 0.39972(19) 0.35928(11) 0.44109(14) 0.0211(4) Uani 1 1 d . . . N6 N 0.29750(17) 0.11391(10) 0.45693(13) 0.0152(4) Uani 1 1 d . . . N7 N 0.18443(17) 0.09011(11) 0.31493(13) 0.0158(4) Uani 1 1 d . . . N8 N 0.2388(2) -0.01174(11) 0.65387(15) 0.0191(4) Uani 1 1 d . . . H8N H 0.317(3) 0.0042(18) 0.664(2) 0.046(9) Uiso 1 1 d . . . C1 C 0.0644(2) 0.22838(13) 0.53538(17) 0.0171(5) Uani 1 1 d . . . H1A H -0.0143 0.2374 0.4884 0.021 Uiso 1 1 calc R . . H1B H 0.0712 0.2647 0.5875 0.021 Uiso 1 1 calc R . . C2 C 0.0692(2) 0.14960(13) 0.57157(16) 0.0149(5) Uani 1 1 d . . . C3 C 0.1455(2) 0.04123(13) 0.62489(16) 0.0162(5) Uani 1 1 d . . . C4 C 0.0231(2) 0.03737(13) 0.61599(17) 0.0188(5) Uani 1 1 d . . . H4 H -0.0215 -0.0046 0.6298 0.023 Uiso 1 1 calc R . . C5 C -0.1514(2) 0.13014(14) 0.56737(18) 0.0222(5) Uani 1 1 d . . . H5A H -0.1695 0.1397 0.6281 0.033 Uiso 1 1 calc R . . H5B H -0.2048 0.0899 0.5344 0.033 Uiso 1 1 calc R . . H5C H -0.1656 0.1762 0.5294 0.033 Uiso 1 1 calc R . . C6 C 0.2113(2) 0.31737(12) 0.49332(17) 0.0182(5) Uani 1 1 d . . . H6A H 0.1603 0.3462 0.4400 0.022 Uiso 1 1 calc R . . H6B H 0.2074 0.3424 0.5526 0.022 Uiso 1 1 calc R . . C7 C 0.3399(2) 0.31271(13) 0.48575(16) 0.0172(5) Uani 1 1 d . . . C8 C 0.5259(2) 0.27071(14) 0.51008(17) 0.0216(5) Uani 1 1 d . . . H8 H 0.5971 0.2406 0.5319 0.026 Uiso 1 1 calc R . . C9 C 0.5179(2) 0.33305(15) 0.45636(18) 0.0252(6) Uani 1 1 d . . . H9 H 0.5818 0.3547 0.4334 0.030 Uiso 1 1 calc R . . C10 C 0.3505(3) 0.42405(14) 0.3829(2) 0.0307(6) Uani 1 1 d . . . H10A H 0.2652 0.4141 0.3494 0.046 Uiso 1 1 calc R . . H10B H 0.3991 0.4330 0.3374 0.046 Uiso 1 1 calc R . . H10C H 0.3539 0.4686 0.4228 0.046 Uiso 1 1 calc R . . C11 C 0.1373(2) 0.20893(13) 0.39295(16) 0.0166(5) Uani 1 1 d . . . H11A H 0.0481 0.1993 0.3716 0.020 Uiso 1 1 calc R . . H11B H 0.1590 0.2471 0.3509 0.020 Uiso 1 1 calc R . . C12 C 0.2058(2) 0.13795(13) 0.38807(16) 0.0152(5) Uani 1 1 d . . . C13 C 0.3363(2) 0.04729(13) 0.42628(17) 0.0173(5) Uani 1 1 d . . . H13 H 0.4010 0.0167 0.4612 0.021 Uiso 1 1 calc R . . C14 C 0.2677(2) 0.03202(13) 0.33838(17) 0.0187(5) Uani 1 1 d . . . H14 H 0.2755 -0.0102 0.3006 0.022 Uiso 1 1 calc R . . C15 C 0.0915(2) 0.09823(14) 0.22601(16) 0.0186(5) Uani 1 1 d . . . H15A H 0.0283 0.1336 0.2341 0.028 Uiso 1 1 calc R . . H15B H 0.0541 0.0491 0.2065 0.028 Uiso 1 1 calc R . . H15C H 0.1300 0.1174 0.1779 0.028 Uiso 1 1 calc R . . C16 C 0.2193(2) -0.08671(13) 0.66777(16) 0.0188(5) Uani 1 1 d . . . C17 C 0.3345(2) -0.13430(13) 0.70240(17) 0.0209(5) Uani 1 1 d . . . C18 C 0.4202(3) -0.12579(16) 0.6374(2) 0.0312(6) Uani 1 1 d . . . H18A H 0.3770 -0.1407 0.5735 0.047 Uiso 1 1 calc R . . H18B H 0.4921 -0.1581 0.6597 0.047 Uiso 1 1 calc R . . H18C H 0.4465 -0.0732 0.6374 0.047 Uiso 1 1 calc R . . C19 C 0.4048(3) -0.10672(16) 0.79950(18) 0.0297(6) Uani 1 1 d . . . H19A H 0.4373 -0.0562 0.7941 0.045 Uiso 1 1 calc R . . H19B H 0.4726 -0.1413 0.8255 0.045 Uiso 1 1 calc R . . H19C H 0.3495 -0.1050 0.8412 0.045 Uiso 1 1 calc R . . C20 C 0.2971(3) -0.21650(15) 0.7072(3) 0.0416(8) Uani 1 1 d . . . H20A H 0.2430 -0.2211 0.7496 0.062 Uiso 1 1 calc R . . H20B H 0.3704 -0.2474 0.7308 0.062 Uiso 1 1 calc R . . H20C H 0.2539 -0.2338 0.6443 0.062 Uiso 1 1 calc R . . Fe2 Fe 0.87674(3) 0.439664(19) 0.44933(2) 0.01651(10) Uani 1 1 d . . . Cl3 Cl 0.84151(5) 0.35616(4) 0.55223(4) 0.02350(14) Uani 1 1 d . . . Cl4 Cl 0.92391(6) 0.37939(4) 0.32989(4) 0.02673(15) Uani 1 1 d . . . Cl5 Cl 0.70391(5) 0.50458(3) 0.39784(4) 0.02242(14) Uani 1 1 d . . . O2 O 1.0000 0.5000 0.5000 0.0254(6) Uani 1 2 d S . . 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 Fe1 0.01204(17) 0.01293(17) 0.01531(18) -0.00097(13) 0.00244(13) -0.00091(13) Cl1 0.0152(3) 0.0203(3) 0.0237(3) -0.0003(2) 0.0000(2) 0.0030(2) Cl2 0.0209(3) 0.0197(3) 0.0178(3) -0.0037(2) 0.0044(2) -0.0008(2) O1 0.0182(9) 0.0200(9) 0.0335(10) 0.0031(8) 0.0067(8) -0.0030(7) N1 0.0158(10) 0.0118(9) 0.0173(10) -0.0010(8) 0.0048(8) -0.0013(8) N2 0.0151(10) 0.0150(10) 0.0167(10) 0.0011(8) 0.0040(8) 0.0000(8) N3 0.0127(10) 0.0190(10) 0.0184(10) 0.0019(8) 0.0046(8) 0.0005(8) N4 0.0145(10) 0.0174(10) 0.0184(10) -0.0023(8) 0.0047(8) -0.0040(8) N5 0.0261(12) 0.0189(10) 0.0194(11) -0.0007(8) 0.0078(9) -0.0058(9) N6 0.0138(10) 0.0161(10) 0.0156(10) -0.0010(8) 0.0035(8) 0.0003(8) N7 0.0157(10) 0.0176(10) 0.0139(10) -0.0008(8) 0.0035(8) -0.0004(8) N8 0.0145(11) 0.0174(10) 0.0243(11) 0.0024(9) 0.0027(9) -0.0013(8) C1 0.0142(12) 0.0168(11) 0.0218(12) 0.0022(10) 0.0071(10) 0.0022(9) C2 0.0154(12) 0.0152(11) 0.0141(11) 0.0002(9) 0.0034(9) -0.0005(9) C3 0.0168(12) 0.0158(11) 0.0162(12) 0.0006(9) 0.0043(9) -0.0004(9) C4 0.0211(13) 0.0166(12) 0.0204(13) 0.0028(10) 0.0081(10) -0.0006(10) C5 0.0138(12) 0.0263(13) 0.0261(14) 0.0062(11) 0.0043(10) 0.0025(10) C6 0.0229(13) 0.0115(11) 0.0204(13) -0.0003(9) 0.0060(10) -0.0018(10) C7 0.0213(13) 0.0138(11) 0.0163(12) -0.0033(9) 0.0046(10) -0.0058(10) C8 0.0152(12) 0.0267(13) 0.0229(13) -0.0043(11) 0.0050(10) -0.0048(10) C9 0.0232(14) 0.0301(14) 0.0253(14) -0.0044(11) 0.0116(11) -0.0097(11) C10 0.0436(18) 0.0206(13) 0.0320(16) 0.0077(12) 0.0169(13) -0.0033(12) C11 0.0162(12) 0.0151(11) 0.0172(12) -0.0001(9) 0.0017(9) -0.0002(9) C12 0.0135(12) 0.0156(11) 0.0167(12) -0.0008(9) 0.0043(9) -0.0028(9) C13 0.0139(12) 0.0179(12) 0.0206(13) -0.0016(10) 0.0053(10) 0.0014(9) C14 0.0181(12) 0.0173(12) 0.0213(13) -0.0021(10) 0.0059(10) 0.0019(10) C15 0.0191(13) 0.0235(13) 0.0115(11) 0.0001(10) 0.0006(9) 0.0024(10) C16 0.0213(13) 0.0190(12) 0.0170(12) 0.0002(10) 0.0065(10) 0.0000(10) C17 0.0207(13) 0.0174(12) 0.0231(13) 0.0006(10) 0.0025(10) 0.0016(10) C18 0.0248(15) 0.0389(16) 0.0306(15) 0.0062(13) 0.0085(12) 0.0131(13) C19 0.0299(15) 0.0310(15) 0.0242(14) 0.0035(12) -0.0002(12) 0.0112(12) C20 0.0295(17) 0.0163(13) 0.074(2) 0.0067(14) 0.0047(16) 0.0006(12) Fe2 0.01378(18) 0.01707(18) 0.01749(18) -0.00014(14) 0.00171(14) -0.00212(13) Cl3 0.0193(3) 0.0262(3) 0.0250(3) 0.0081(3) 0.0057(2) 0.0024(2) Cl4 0.0287(4) 0.0285(3) 0.0229(3) -0.0026(3) 0.0063(3) 0.0048(3) Cl5 0.0199(3) 0.0211(3) 0.0255(3) 0.0031(2) 0.0043(2) 0.0038(2) O2 0.0207(13) 0.0278(14) 0.0254(14) -0.0031(11) 0.0018(11) -0.0091(11) _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 Fe1 N4 2.0751(19) . yes Fe1 N6 2.1075(19) . yes Fe1 N2 2.1138(19) . yes Fe1 Cl1 2.2511(7) . yes Fe1 Cl2 2.3114(7) . yes Fe1 N1 2.3225(19) . yes O1 C16 1.224(3) . no N1 C1 1.481(3) . no N1 C6 1.487(3) . no N1 C11 1.497(3) . no N2 C2 1.330(3) . no N2 C3 1.377(3) . no N3 C2 1.333(3) . no N3 C4 1.389(3) . no N3 C5 1.458(3) . no N4 C7 1.324(3) . no N4 C8 1.382(3) . no N5 C7 1.339(3) . no N5 C9 1.377(3) . no N5 C10 1.457(3) . no N6 C12 1.323(3) . no N6 C13 1.376(3) . no N7 C12 1.344(3) . no N7 C14 1.379(3) . no N7 C15 1.462(3) . no N8 C16 1.373(3) . no N8 C3 1.396(3) . no N8 H8N 0.90(3) . yes C1 C2 1.492(3) . no C1 H1A 0.9900 . no C1 H1B 0.9900 . no C3 C4 1.355(3) . no C4 H4 0.9500 . no C5 H5A 0.9800 . no C5 H5B 0.9800 . no C5 H5C 0.9800 . no C6 C7 1.486(3) . no C6 H6A 0.9900 . no C6 H6B 0.9900 . no C8 C9 1.350(4) . no C8 H8 0.9500 . no C9 H9 0.9500 . no C10 H10A 0.9800 . no C10 H10B 0.9800 . no C10 H10C 0.9800 . no C11 C12 1.489(3) . no C11 H11A 0.9900 . no C11 H11B 0.9900 . no C13 C14 1.356(3) . no C13 H13 0.9500 . no C14 H14 0.9500 . no C15 H15A 0.9800 . no C15 H15B 0.9800 . no C15 H15C 0.9800 . no C16 C17 1.526(3) . no C17 C20 1.525(4) . no C17 C19 1.529(3) . no C17 C18 1.530(4) . no C18 H18A 0.9800 . no C18 H18B 0.9800 . no C18 H18C 0.9800 . no C19 H19A 0.9800 . no C19 H19B 0.9800 . no C19 H19C 0.9800 . no C20 H20A 0.9800 . no C20 H20B 0.9800 . no C20 H20C 0.9800 . no Fe2 O2 1.7643(4) . no Fe2 Cl3 2.2251(7) . no Fe2 Cl5 2.2265(7) . no Fe2 Cl4 2.2334(7) . no O2 Fe2 1.7643(4) 3_766 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_3 _geom_angle_publ_flag N4 Fe1 N6 89.32(8) . . yes N4 Fe1 N2 151.10(8) . . yes N6 Fe1 N2 82.10(7) . . yes N4 Fe1 Cl1 104.08(6) . . yes N6 Fe1 Cl1 92.85(6) . . yes N2 Fe1 Cl1 103.88(6) . . yes N4 Fe1 Cl2 93.10(6) . . yes N6 Fe1 Cl2 165.90(6) . . yes N2 Fe1 Cl2 89.18(5) . . yes Cl1 Fe1 Cl2 100.01(3) . . yes N4 Fe1 N1 75.60(7) . . yes N6 Fe1 N1 76.96(7) . . yes N2 Fe1 N1 75.59(7) . . yes Cl1 Fe1 N1 169.79(5) . . yes Cl2 Fe1 N1 90.19(5) . . yes C1 N1 C6 113.22(18) . . no C1 N1 C11 111.46(18) . . no C6 N1 C11 109.79(18) . . no C1 N1 Fe1 105.93(13) . . no C6 N1 Fe1 105.14(14) . . no C11 N1 Fe1 111.06(13) . . no C2 N2 C3 106.71(19) . . no C2 N2 Fe1 115.05(15) . . no C3 N2 Fe1 138.25(16) . . no C2 N3 C4 107.78(19) . . no C2 N3 C5 127.0(2) . . no C4 N3 C5 125.2(2) . . no C7 N4 C8 106.5(2) . . no C7 N4 Fe1 116.28(16) . . no C8 N4 Fe1 136.57(17) . . no C7 N5 C9 107.4(2) . . no C7 N5 C10 127.6(2) . . no C9 N5 C10 124.9(2) . . no C12 N6 C13 106.15(19) . . no C12 N6 Fe1 117.37(15) . . no C13 N6 Fe1 135.70(16) . . no C12 N7 C14 107.40(19) . . no C12 N7 C15 126.7(2) . . no C14 N7 C15 125.92(19) . . no C16 N8 C3 124.2(2) . . no C16 N8 H8N 118(2) . . no C3 N8 H8N 118(2) . . no N1 C1 C2 107.62(18) . . no N1 C1 H1A 110.2 . . no C2 C1 H1A 110.2 . . no N1 C1 H1B 110.2 . . no C2 C1 H1B 110.2 . . no H1A C1 H1B 108.5 . . no N2 C2 N3 110.5(2) . . no N2 C2 C1 121.8(2) . . no N3 C2 C1 127.8(2) . . no C4 C3 N2 109.0(2) . . no C4 C3 N8 131.9(2) . . no N2 C3 N8 119.2(2) . . no C3 C4 N3 106.1(2) . . no C3 C4 H4 127.0 . . no N3 C4 H4 127.0 . . no N3 C5 H5A 109.5 . . no N3 C5 H5B 109.5 . . no H5A C5 H5B 109.5 . . no N3 C5 H5C 109.5 . . no H5A C5 H5C 109.5 . . no H5B C5 H5C 109.5 . . no C7 C6 N1 105.56(18) . . no C7 C6 H6A 110.6 . . no N1 C6 H6A 110.6 . . no C7 C6 H6B 110.6 . . no N1 C6 H6B 110.6 . . no H6A C6 H6B 108.8 . . no N4 C7 N5 110.6(2) . . no N4 C7 C6 120.7(2) . . no N5 C7 C6 128.7(2) . . no C9 C8 N4 108.5(2) . . no C9 C8 H8 125.7 . . no N4 C8 H8 125.7 . . no C8 C9 N5 106.9(2) . . no C8 C9 H9 126.5 . . no N5 C9 H9 126.5 . . no N5 C10 H10A 109.5 . . no N5 C10 H10B 109.5 . . no H10A C10 H10B 109.5 . . no N5 C10 H10C 109.5 . . no H10A C10 H10C 109.5 . . no H10B C10 H10C 109.5 . . no C12 C11 N1 110.06(18) . . no C12 C11 H11A 109.6 . . no N1 C11 H11A 109.6 . . no C12 C11 H11B 109.6 . . no N1 C11 H11B 109.6 . . no H11A C11 H11B 108.2 . . no N6 C12 N7 110.9(2) . . no N6 C12 C11 123.4(2) . . no N7 C12 C11 125.7(2) . . no C14 C13 N6 109.4(2) . . no C14 C13 H13 125.3 . . no N6 C13 H13 125.3 . . no C13 C14 N7 106.1(2) . . no C13 C14 H14 126.9 . . no N7 C14 H14 126.9 . . no N7 C15 H15A 109.5 . . no N7 C15 H15B 109.5 . . no H15A C15 H15B 109.5 . . no N7 C15 H15C 109.5 . . no H15A C15 H15C 109.5 . . no H15B C15 H15C 109.5 . . no O1 C16 N8 120.5(2) . . no O1 C16 C17 124.0(2) . . no N8 C16 C17 115.5(2) . . no C20 C17 C16 108.8(2) . . no C20 C17 C19 110.3(2) . . no C16 C17 C19 109.4(2) . . no C20 C17 C18 110.4(2) . . no C16 C17 C18 110.9(2) . . no C19 C17 C18 107.0(2) . . no C17 C18 H18A 109.5 . . no C17 C18 H18B 109.5 . . no H18A C18 H18B 109.5 . . no C17 C18 H18C 109.5 . . no H18A C18 H18C 109.5 . . no H18B C18 H18C 109.5 . . no C17 C19 H19A 109.5 . . no C17 C19 H19B 109.5 . . no H19A C19 H19B 109.5 . . no C17 C19 H19C 109.5 . . no H19A C19 H19C 109.5 . . no H19B C19 H19C 109.5 . . no C17 C20 H20A 109.5 . . no C17 C20 H20B 109.5 . . no H20A C20 H20B 109.5 . . no C17 C20 H20C 109.5 . . no H20A C20 H20C 109.5 . . no H20B C20 H20C 109.5 . . no O2 Fe2 Cl3 111.95(2) . . no O2 Fe2 Cl5 111.03(2) . . no Cl3 Fe2 Cl5 106.54(3) . . no O2 Fe2 Cl4 107.72(2) . . no Cl3 Fe2 Cl4 109.60(3) . . no Cl5 Fe2 Cl4 110.01(3) . . no Fe2 O2 Fe2 180.000(17) . 3_766 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N8 H8N Cl1 0.90(3) 2.55(3) 3.395(2) 155(3) . _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 0.457 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.085 #===END