# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Mostafa, Golam' _publ_contact_author_email mostafa@phys.jdvu.ac.in _publ_section_title ; A Supramolecular Spin Crossover Fe(III) Complex and its Cr(III) Isomer: Stabilization of Water-Chloride Cluster within Supramolecular Host ; loop_ _publ_author_name R.Saha S.Biswas I.Steele K.Dey G.Mostafa # Attachment '- complex1.cif' data_sb41 _database_code_depnum_ccdc_archive 'CCDC 778259' #TrackingRef '- complex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Cr N8 O4 S2, 3(H2 O), Cl' _chemical_formula_sum 'C18 H36 Cl Cr N8 O7 S2' _chemical_formula_weight 628.14 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' Cr Cr 0.3209 0.6236 '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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 15.379(4) _cell_length_b 22.955(5) _cell_length_c 7.9671(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.769(4) _cell_angle_gamma 90.00 _cell_volume 2786.7(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6748 _cell_measurement_theta_min 1.34 _cell_measurement_theta_max 28.32 _exptl_crystal_description Rhombohedral _exptl_crystal_colour Pink _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.708 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 0.930 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32562 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6748 _reflns_number_gt 4610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.0319P)^2^+0.0000P] 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 nonref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6748 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0739 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0834 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.001 _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 0.33409(16) 0.41237(11) 0.1148(3) 0.0209(6) Uani 1 1 d . . . C2 C 0.38591(18) 0.38733(11) -0.0131(3) 0.0315(7) Uani 1 1 d . . . H2A H 0.4219 0.4180 -0.0547 0.047 Uiso 1 1 calc R . . H2B H 0.3458 0.3713 -0.1080 0.047 Uiso 1 1 calc R . . H2C H 0.4240 0.3562 0.0393 0.047 Uiso 1 1 calc R . . C3 C 0.27293(16) 0.37639(11) 0.1971(3) 0.0206(6) Uani 1 1 d . . . C4 C 0.26381(17) 0.31234(10) 0.1701(3) 0.0263(6) Uani 1 1 d . . . H4A H 0.2696 0.2925 0.2800 0.039 Uiso 1 1 calc R . . H4B H 0.3097 0.2986 0.1056 0.039 Uiso 1 1 calc R . . H4C H 0.2061 0.3038 0.1068 0.039 Uiso 1 1 calc R . . C5 C 0.12895(16) 0.40796(10) 0.4798(3) 0.0200(5) Uani 1 1 d . . . C6 C 0.06339(18) 0.31800(10) 0.5731(3) 0.0267(6) Uani 1 1 d . . . H6A H 0.0888 0.3007 0.4767 0.032 Uiso 1 1 calc R . . H6B H 0.0007 0.3068 0.5625 0.032 Uiso 1 1 calc R . . C7 C 0.11088(19) 0.29522(11) 0.7368(3) 0.0314(7) Uani 1 1 d . . . H7A H 0.1034 0.2524 0.7410 0.038 Uiso 1 1 calc R . . H7B H 0.1744 0.3035 0.7419 0.038 Uiso 1 1 calc R . . C8 C 0.08832(18) 0.38266(11) 0.8752(3) 0.0273(6) Uani 1 1 d . . . H8A H 0.1512 0.3928 0.8812 0.033 Uiso 1 1 calc R . . H8B H 0.0661 0.3999 0.9750 0.033 Uiso 1 1 calc R . . C9 C 0.03832(17) 0.40809(11) 0.7150(3) 0.0236(6) Uani 1 1 d . . . H9A H -0.0252 0.4000 0.7110 0.028 Uiso 1 1 calc R . . H9B H 0.0468 0.4508 0.7132 0.028 Uiso 1 1 calc R . . C10 C 0.35984(17) 0.55670(11) 0.5588(3) 0.0224(6) Uani 1 1 d . . . C11 C 0.42512(19) 0.57397(12) 0.7060(3) 0.0333(7) Uani 1 1 d . . . H11A H 0.4463 0.5391 0.7699 0.050 Uiso 1 1 calc R . . H11B H 0.3973 0.6003 0.7797 0.050 Uiso 1 1 calc R . . H11C H 0.4746 0.5939 0.6652 0.050 Uiso 1 1 calc R . . C12 C 0.30756(16) 0.60027(10) 0.4535(3) 0.0210(6) Uani 1 1 d . . . C13 C 0.32033(18) 0.66408(10) 0.4818(3) 0.0287(6) Uani 1 1 d . . . H13A H 0.3178 0.6839 0.3723 0.043 Uiso 1 1 calc R . . H13B H 0.3777 0.6711 0.5487 0.043 Uiso 1 1 calc R . . H13C H 0.2739 0.6792 0.5429 0.043 Uiso 1 1 calc R . . C14 C 0.15620(16) 0.59025(10) 0.0947(3) 0.0201(5) Uani 1 1 d . . . C15 C 0.11567(18) 0.68794(11) -0.0169(3) 0.0292(6) Uani 1 1 d . . . H15A H 0.1432 0.7007 0.0967 0.035 Uiso 1 1 calc R . . H15B H 0.0566 0.7058 -0.0396 0.035 Uiso 1 1 calc R . . C16 C 0.17056(19) 0.70741(12) -0.1481(3) 0.0339(7) Uani 1 1 d . . . H16A H 0.1731 0.7505 -0.1490 0.041 Uiso 1 1 calc R . . H16B H 0.2311 0.6926 -0.1182 0.041 Uiso 1 1 calc R . . C17 C 0.12968(18) 0.62517(11) -0.3152(3) 0.0288(6) Uani 1 1 d . . . H17A H 0.1890 0.6082 -0.2865 0.035 Uiso 1 1 calc R . . H17B H 0.1057 0.6118 -0.4303 0.035 Uiso 1 1 calc R . . C18 C 0.07137(17) 0.60399(11) -0.1898(3) 0.0239(6) Uani 1 1 d . . . H18A H 0.0112 0.6194 -0.2202 0.029 Uiso 1 1 calc R . . H18B H 0.0685 0.5609 -0.1914 0.029 Uiso 1 1 calc R . . Cr1 Cr 0.24530(3) 0.491739(17) 0.31229(5) 0.01921(11) Uani 1 1 d . . . N1 N 0.33703(13) 0.46656(9) 0.1593(3) 0.0227(5) Uani 1 1 d . . . N2 N 0.22680(13) 0.40528(8) 0.2961(2) 0.0187(5) Uani 1 1 d . . . N3 N 0.16930(13) 0.37423(8) 0.3787(2) 0.0203(5) Uani 1 1 d . . . N4 N 0.07121(13) 0.38145(8) 0.5687(3) 0.0221(5) Uani 1 1 d . . . N5 N 0.34426(14) 0.50331(9) 0.5104(3) 0.0238(5) Uani 1 1 d . . . N6 N 0.25222(13) 0.57886(8) 0.3303(2) 0.0196(5) Uani 1 1 d . . . N7 N 0.20471(13) 0.61733(8) 0.2222(3) 0.0212(5) Uani 1 1 d . . . N8 N 0.10790(14) 0.62431(9) -0.0211(3) 0.0237(5) Uani 1 1 d . . . O1 O 0.39276(12) 0.50045(8) 0.0785(2) 0.0317(5) Uani 1 1 d . . . H1 H 0.3993 0.5330 0.1266 0.048 Uiso 1 1 calc R . . O2 O 0.07918(12) 0.32093(8) 0.8796(2) 0.0320(5) Uani 1 1 d . . . O3 O 0.39351(13) 0.46249(8) 0.6095(2) 0.0371(5) Uani 1 1 d . . . H3 H 0.3829 0.4291 0.5685 0.056 Uiso 1 1 calc R . . O4 O 0.13576(12) 0.68694(7) -0.3139(2) 0.0317(5) Uani 1 1 d . . . O5 O 0.50103(15) 0.73137(10) 0.7339(3) 0.0391(5) Uani 1 1 d . . . O6 O 0.57227(15) 0.39641(9) 0.8013(3) 0.0340(5) Uani 1 1 d . . . O7 O 0.40024(14) 0.69702(9) 0.9876(3) 0.0432(6) Uani 1 1 d . . . S1 S 0.14703(4) 0.51476(3) 0.07130(8) 0.02402(16) Uani 1 1 d . . . S2 S 0.14242(4) 0.48315(3) 0.50112(8) 0.02442(16) Uani 1 1 d . . . Cl1 Cl 0.58762(5) 0.83544(3) 0.95439(9) 0.03630(19) Uani 1 1 d . . . H4W H 0.438(3) 0.708(2) 0.891(6) 0.14(2) Uiso 1 1 d . . . H5W H 0.5901(19) 0.3624(14) 0.890(4) 0.056(10) Uiso 1 1 d . . . H3W H 0.427(3) 0.7207(18) 1.086(5) 0.113(17) Uiso 1 1 d . . . H6W H 0.527(2) 0.3892(15) 0.749(4) 0.066(14) Uiso 1 1 d . . . H1W H 0.533(2) 0.7598(15) 0.785(4) 0.063(12) Uiso 1 1 d . . . H2W H 0.537(3) 0.7097(18) 0.659(5) 0.113(16) Uiso 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 0.0211(14) 0.0234(14) 0.0177(13) 0.0006(11) 0.0007(11) 0.0024(11) C2 0.0365(17) 0.0277(15) 0.0328(17) -0.0016(13) 0.0142(14) 0.0024(13) C3 0.0214(14) 0.0208(13) 0.0182(13) 0.0007(11) -0.0025(11) 0.0033(10) C4 0.0285(15) 0.0209(14) 0.0292(15) -0.0036(12) 0.0030(12) 0.0008(11) C5 0.0226(14) 0.0180(13) 0.0180(13) 0.0012(10) -0.0024(11) 0.0016(10) C6 0.0352(16) 0.0186(13) 0.0276(15) -0.0049(11) 0.0090(13) -0.0057(12) C7 0.0378(17) 0.0217(14) 0.0354(17) 0.0009(13) 0.0074(14) 0.0011(12) C8 0.0322(16) 0.0269(15) 0.0228(15) -0.0019(12) 0.0031(12) -0.0006(12) C9 0.0256(15) 0.0225(14) 0.0236(15) -0.0044(11) 0.0070(12) -0.0025(11) C10 0.0225(14) 0.0229(14) 0.0207(14) 0.0004(11) -0.0006(11) 0.0002(11) C11 0.0389(18) 0.0281(15) 0.0290(16) 0.0015(12) -0.0095(13) -0.0009(13) C12 0.0226(14) 0.0200(13) 0.0205(14) 0.0010(11) 0.0032(11) -0.0001(11) C13 0.0368(17) 0.0200(14) 0.0277(16) -0.0014(12) -0.0017(13) -0.0024(12) C14 0.0205(14) 0.0207(13) 0.0197(14) 0.0002(11) 0.0057(11) 0.0016(11) C15 0.0402(17) 0.0192(14) 0.0253(15) 0.0003(12) -0.0063(13) 0.0061(12) C16 0.0426(18) 0.0231(15) 0.0338(17) -0.0001(13) -0.0034(14) -0.0032(13) C17 0.0359(17) 0.0270(15) 0.0230(15) -0.0006(12) 0.0021(13) 0.0015(12) C18 0.0286(15) 0.0214(13) 0.0199(14) -0.0022(11) -0.0027(12) 0.0005(11) Cr1 0.0223(2) 0.0158(2) 0.0193(2) 0.00094(17) 0.00206(17) 0.00005(17) N1 0.0231(12) 0.0241(12) 0.0213(12) 0.0044(9) 0.0041(10) -0.0022(9) N2 0.0202(11) 0.0185(11) 0.0169(11) 0.0025(9) 0.0007(9) 0.0011(9) N3 0.0246(12) 0.0181(11) 0.0184(11) 0.0001(9) 0.0033(9) -0.0013(9) N4 0.0283(13) 0.0162(11) 0.0228(12) -0.0015(9) 0.0070(10) -0.0023(9) N5 0.0272(12) 0.0216(11) 0.0213(12) 0.0041(9) -0.0008(10) 0.0031(9) N6 0.0230(12) 0.0178(11) 0.0179(11) 0.0011(9) 0.0020(9) 0.0007(9) N7 0.0236(12) 0.0178(11) 0.0211(12) 0.0023(9) -0.0007(9) 0.0011(9) N8 0.0317(13) 0.0191(11) 0.0189(12) -0.0014(9) -0.0016(10) 0.0018(9) O1 0.0377(12) 0.0259(11) 0.0341(11) 0.0003(9) 0.0137(9) -0.0062(9) O2 0.0456(12) 0.0241(10) 0.0260(11) 0.0031(8) 0.0035(9) -0.0008(9) O3 0.0497(13) 0.0230(10) 0.0326(12) 0.0013(9) -0.0155(10) 0.0073(10) O4 0.0456(13) 0.0237(10) 0.0240(11) 0.0027(8) -0.0016(9) -0.0046(9) O5 0.0448(14) 0.0353(13) 0.0358(13) -0.0055(10) 0.0004(11) -0.0057(11) O6 0.0319(13) 0.0342(12) 0.0356(13) 0.0004(10) 0.0036(10) -0.0048(10) O7 0.0419(14) 0.0369(13) 0.0489(15) -0.0026(11) -0.0009(12) 0.0013(10) S1 0.0289(4) 0.0170(3) 0.0244(4) -0.0003(3) -0.0028(3) -0.0006(3) S2 0.0316(4) 0.0153(3) 0.0279(4) -0.0011(3) 0.0098(3) 0.0000(3) Cl1 0.0462(5) 0.0267(4) 0.0327(4) 0.0022(3) -0.0065(3) -0.0067(3) _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 1.293(3) . ? C1 C3 1.471(3) . ? C1 C2 1.491(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 N2 1.311(3) . ? C3 C4 1.490(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 N3 1.330(3) . ? C5 N4 1.353(3) . ? C5 S2 1.744(2) . ? C6 N4 1.462(3) . ? C6 C7 1.501(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.425(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.425(3) . ? C8 C9 1.515(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N4 1.465(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N5 1.297(3) . ? C10 C12 1.472(3) . ? C10 C11 1.491(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 N6 1.305(3) . ? C12 C13 1.491(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 N7 1.331(3) . ? C14 N8 1.352(3) . ? C14 S1 1.746(2) . ? C15 N8 1.465(3) . ? C15 C16 1.498(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O4 1.436(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O4 1.421(3) . ? C17 C18 1.510(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N8 1.461(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? Cr1 N2 2.007(2) . ? Cr1 N6 2.007(2) . ? Cr1 N5 2.056(2) . ? Cr1 N1 2.068(2) . ? Cr1 S2 2.3343(8) . ? Cr1 S1 2.3378(8) . ? N1 O1 1.380(2) . ? N2 N3 1.371(3) . ? N5 O3 1.383(2) . ? N6 N7 1.373(3) . ? O1 H1 0.8400 . ? O3 H3 0.8400 . ? O5 H1W 0.88(3) . ? O5 H2W 1.00(4) . ? O6 H5W 1.06(3) . ? O6 H6W 0.79(3) . ? O7 H4W 1.05(5) . ? O7 H3W 1.00(5) . ? 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 C3 114.8(2) . . ? N1 C1 C2 123.8(2) . . ? C3 C1 C2 121.4(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C1 114.5(2) . . ? N2 C3 C4 122.6(2) . . ? C1 C3 C4 122.9(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 N4 116.7(2) . . ? N3 C5 S2 125.16(19) . . ? N4 C5 S2 118.16(18) . . ? N4 C6 C7 109.6(2) . . ? N4 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? N4 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? O2 C7 C6 111.8(2) . . ? O2 C7 H7A 109.3 . . ? C6 C7 H7A 109.3 . . ? O2 C7 H7B 109.3 . . ? C6 C7 H7B 109.3 . . ? H7A C7 H7B 107.9 . . ? O2 C8 C9 111.3(2) . . ? O2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? O2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N4 C9 C8 108.6(2) . . ? N4 C9 H9A 110.0 . . ? C8 C9 H9A 110.0 . . ? N4 C9 H9B 110.0 . . ? C8 C9 H9B 110.0 . . ? H9A C9 H9B 108.4 . . ? N5 C10 C12 114.1(2) . . ? N5 C10 C11 124.2(2) . . ? C12 C10 C11 121.7(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N6 C12 C10 115.0(2) . . ? N6 C12 C13 122.9(2) . . ? C10 C12 C13 122.1(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N7 C14 N8 116.8(2) . . ? N7 C14 S1 125.01(19) . . ? N8 C14 S1 118.17(19) . . ? N8 C15 C16 109.5(2) . . ? N8 C15 H15A 109.8 . . ? C16 C15 H15A 109.8 . . ? N8 C15 H15B 109.8 . . ? C16 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? O4 C16 C15 111.7(2) . . ? O4 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? O4 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 107.9 . . ? O4 C17 C18 111.1(2) . . ? O4 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O4 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N8 C18 C17 108.5(2) . . ? N8 C18 H18A 110.0 . . ? C17 C18 H18A 110.0 . . ? N8 C18 H18B 110.0 . . ? C17 C18 H18B 110.0 . . ? H18A C18 H18B 108.4 . . ? N2 Cr1 N6 174.82(8) . . ? N2 Cr1 N5 105.12(8) . . ? N6 Cr1 N5 77.86(8) . . ? N2 Cr1 N1 77.75(8) . . ? N6 Cr1 N1 106.68(8) . . ? N5 Cr1 N1 89.74(9) . . ? N2 Cr1 S2 81.67(6) . . ? N6 Cr1 S2 94.13(6) . . ? N5 Cr1 S2 90.69(6) . . ? N1 Cr1 S2 158.79(6) . . ? N2 Cr1 S1 95.77(6) . . ? N6 Cr1 S1 81.70(6) . . ? N5 Cr1 S1 158.50(6) . . ? N1 Cr1 S1 89.76(6) . . ? S2 Cr1 S1 97.42(3) . . ? C1 N1 O1 114.6(2) . . ? C1 N1 Cr1 115.42(16) . . ? O1 N1 Cr1 129.33(15) . . ? C3 N2 N3 117.6(2) . . ? C3 N2 Cr1 117.10(16) . . ? N3 N2 Cr1 125.34(15) . . ? C5 N3 N2 111.8(2) . . ? C5 N4 C6 121.5(2) . . ? C5 N4 C9 123.4(2) . . ? C6 N4 C9 111.01(19) . . ? C10 N5 O3 113.9(2) . . ? C10 N5 Cr1 115.97(17) . . ? O3 N5 Cr1 129.92(15) . . ? C12 N6 N7 117.9(2) . . ? C12 N6 Cr1 116.87(16) . . ? N7 N6 Cr1 125.27(16) . . ? C14 N7 N6 112.0(2) . . ? C14 N8 C18 123.4(2) . . ? C14 N8 C15 121.7(2) . . ? C18 N8 C15 111.06(19) . . ? N1 O1 H1 109.5 . . ? C7 O2 C8 110.28(19) . . ? N5 O3 H3 109.5 . . ? C17 O4 C16 110.44(19) . . ? H1W O5 H2W 108(3) . . ? H5W O6 H6W 109(3) . . ? H4W O7 H3W 104(3) . . ? C14 S1 Cr1 95.90(9) . . ? C5 S2 Cr1 95.90(9) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.486 _refine_diff_density_min -0.343 _refine_diff_density_rms 0.074 # Attachment '- complex2.cif' data_sb42x _database_code_depnum_ccdc_archive 'CCDC 778260' #TrackingRef '- complex2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H30 Fe N8 O4 S2, 3(H2 O), Cl' _chemical_formula_sum 'C18 H36 Cl Fe N8 O7 S2' _chemical_formula_weight 631.97 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' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 15.370(4) _cell_length_b 22.703(5) _cell_length_c 7.9312(19) _cell_angle_alpha 90.00 _cell_angle_beta 97.217(4) _cell_angle_gamma 90.00 _cell_volume 2745.6(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6672 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 28.32 _exptl_crystal_description Rhombohedral _exptl_crystal_colour Brown _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.529 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1324 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.795 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32330 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6672 _reflns_number_gt 5049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for windows (Farrugia, 1997)' _computing_publication_material 'Platon99 (Spek, 1999)' _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^)+(0.0438P)^2^+0.0000P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6672 _refine_ls_number_parameters 358 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0435 _refine_ls_wR_factor_ref 0.0985 _refine_ls_wR_factor_gt 0.0929 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.005 _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 C5 C 0.15167(15) 0.41176(10) 0.6102(3) 0.0165(5) Uani 1 1 d . . . C6 C 0.06520(16) 0.39985(11) 0.3276(3) 0.0205(5) Uani 1 1 d . . . H6A H 0.0648 0.4434 0.3252 0.025 Uiso 1 1 calc R . . H6B H 0.0045 0.3858 0.2944 0.025 Uiso 1 1 calc R . . C7 C 0.12441(17) 0.37659(11) 0.2053(3) 0.0229(6) Uani 1 1 d . . . H7A H 0.1028 0.3901 0.0888 0.027 Uiso 1 1 calc R . . H7B H 0.1843 0.3924 0.2359 0.027 Uiso 1 1 calc R . . C8 C 0.15853(18) 0.29304(11) 0.3760(3) 0.0269(6) Uani 1 1 d . . . H8A H 0.2194 0.3069 0.4083 0.032 Uiso 1 1 calc R . . H8B H 0.1591 0.2494 0.3759 0.032 Uiso 1 1 calc R . . C9 C 0.10174(17) 0.31462(10) 0.5040(3) 0.0225(6) Uani 1 1 d . . . H9A H 0.0421 0.2979 0.4783 0.027 Uiso 1 1 calc R . . H9B H 0.1264 0.3015 0.6192 0.027 Uiso 1 1 calc R . . C3 C 0.30491(15) 0.40031(10) 0.9623(3) 0.0179(5) Uani 1 1 d . . . C4 C 0.31040(17) 0.33647(11) 1.0026(3) 0.0256(6) Uani 1 1 d . . . H4A H 0.2584 0.3245 1.0538 0.038 Uiso 1 1 calc R . . H4B H 0.3631 0.3288 1.0827 0.038 Uiso 1 1 calc R . . H4C H 0.3134 0.3140 0.8980 0.038 Uiso 1 1 calc R . . C1 C 0.36137(15) 0.44459(11) 1.0515(3) 0.0182(5) Uani 1 1 d . . . C2 C 0.43165(17) 0.42981(11) 1.1930(3) 0.0253(6) Uani 1 1 d . . . H2A H 0.4776 0.4069 1.1482 0.038 Uiso 1 1 calc R . . H2B H 0.4065 0.4066 1.2792 0.038 Uiso 1 1 calc R . . H2C H 0.4569 0.4662 1.2443 0.038 Uiso 1 1 calc R . . C14 C 0.13480(15) 0.59063(10) 0.9620(3) 0.0167(5) Uani 1 1 d . . . C15 C 0.04514(16) 0.59377(11) 1.1991(3) 0.0193(5) Uani 1 1 d . . . H15A H 0.0521 0.5504 1.2003 0.023 Uiso 1 1 calc R . . H15B H -0.0176 0.6030 1.2020 0.023 Uiso 1 1 calc R . . C16 C 0.09987(17) 0.62043(11) 1.3526(3) 0.0235(6) Uani 1 1 d . . . H16A H 0.0799 0.6048 1.4578 0.028 Uiso 1 1 calc R . . H16B H 0.1621 0.6091 1.3524 0.028 Uiso 1 1 calc R . . C17 C 0.12124(18) 0.70670(11) 1.2007(3) 0.0263(6) Uani 1 1 d . . . H17A H 0.1838 0.6969 1.1986 0.032 Uiso 1 1 calc R . . H17B H 0.1157 0.7501 1.2021 0.032 Uiso 1 1 calc R . . C18 C 0.06798(17) 0.68261(10) 1.0434(3) 0.0215(5) Uani 1 1 d . . . H18A H 0.0059 0.6947 1.0405 0.026 Uiso 1 1 calc R . . H18B H 0.0904 0.6985 0.9408 0.026 Uiso 1 1 calc R . . C12 C 0.28324(15) 0.61604(10) 0.6806(3) 0.0167(5) Uani 1 1 d . . . C13 C 0.27558(16) 0.68031(10) 0.6420(3) 0.0219(6) Uani 1 1 d . . . H13A H 0.2185 0.6883 0.5762 0.033 Uiso 1 1 calc R . . H13B H 0.3224 0.6921 0.5759 0.033 Uiso 1 1 calc R . . H13C H 0.2808 0.7026 0.7485 0.033 Uiso 1 1 calc R . . C10 C 0.34391(15) 0.57681(11) 0.6103(3) 0.0182(5) Uani 1 1 d . . . C11 C 0.40248(17) 0.59724(11) 0.4862(3) 0.0248(6) Uani 1 1 d . . . H11A H 0.4413 0.5650 0.4613 0.037 Uiso 1 1 calc R . . H11B H 0.4379 0.6305 0.5345 0.037 Uiso 1 1 calc R . . H11C H 0.3669 0.6097 0.3810 0.037 Uiso 1 1 calc R . . Fe1 Fe 0.24930(2) 0.506189(14) 0.81050(4) 0.01497(10) Uani 1 1 d . . . N4 N 0.09729(13) 0.37913(9) 0.4988(2) 0.0188(4) Uani 1 1 d . . . N3 N 0.19770(12) 0.38435(8) 0.7383(2) 0.0169(4) Uani 1 1 d . . . N2 N 0.25100(12) 0.42254(8) 0.8376(2) 0.0156(4) Uani 1 1 d . . . N1 N 0.34496(13) 0.49755(9) 0.9958(2) 0.0181(4) Uani 1 1 d . . . N8 N 0.07422(13) 0.61817(8) 1.0445(2) 0.0182(4) Uani 1 1 d . . . N7 N 0.17465(12) 0.62226(9) 0.8546(2) 0.0172(4) Uani 1 1 d . . . N6 N 0.23514(12) 0.58927(8) 0.7827(2) 0.0157(4) Uani 1 1 d . . . N5 N 0.33970(13) 0.52301(9) 0.6633(2) 0.0181(4) Uani 1 1 d . . . O2 O 0.12717(12) 0.31391(7) 0.2088(2) 0.0264(4) Uani 1 1 d . . . O1 O 0.40104(12) 0.53982(8) 1.0724(2) 0.0284(4) Uani 1 1 d . . . H2 H 0.3834 0.5734 1.0389 0.043 Uiso 1 1 calc R . . O4 O 0.09251(12) 0.68289(8) 1.3509(2) 0.0257(4) Uani 1 1 d . . . O3 O 0.39557(12) 0.48439(8) 0.5964(2) 0.0257(4) Uani 1 1 d . . . H4 H 0.3991 0.4531 0.6533 0.038 Uiso 1 1 calc R . . O1W O 0.42651(13) 0.38124(9) 0.7196(3) 0.0357(5) Uani 1 1 d . . . O2W O 0.40302(15) 0.20192(10) -0.0282(3) 0.0496(6) Uani 1 1 d . . . O3W O 0.49267(14) 0.72691(10) 0.7841(3) 0.0446(6) Uani 1 1 d . . . S2 S 0.15442(4) 0.48813(3) 0.58042(8) 0.01902(14) Uani 1 1 d . . . S1 S 0.15395(4) 0.51558(3) 0.99769(8) 0.01895(14) Uani 1 1 d . . . Cl1 Cl 0.39556(5) 0.67008(3) 0.06402(9) 0.03721(19) Uani 1 1 d . . . H1W1 H 0.478(2) 0.3698(14) 0.771(4) 0.045 Uiso 1 1 d . . . H2W1 H 0.3982(18) 0.3595(10) 0.6349(4) 0.045 Uiso 1 1 d . . . H1W2 H 0.4347(14) 0.2251(10) 0.0593(3) 0.045 Uiso 1 1 d . . . H2W2 H 0.4388(19) 0.2094(13) -0.1217(4) 0.045 Uiso 1 1 d . . . H1W3 H 0.4589(16) 0.7616(13) 0.7259(3) 0.045 Uiso 1 1 d . . . H2W3 H 0.4526(16) 0.7095(11) 0.8705(4) 0.045 Uiso 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 C5 0.0158(12) 0.0171(12) 0.0174(12) -0.0004(10) 0.0056(10) 0.0000(9) C6 0.0239(13) 0.0175(13) 0.0185(12) 0.0010(10) -0.0040(10) -0.0005(10) C7 0.0277(14) 0.0203(14) 0.0202(13) 0.0008(11) 0.0014(11) -0.0025(11) C8 0.0330(15) 0.0191(14) 0.0270(15) -0.0001(11) -0.0022(12) 0.0027(11) C9 0.0282(14) 0.0177(13) 0.0201(13) 0.0009(10) -0.0023(11) -0.0044(11) C3 0.0177(12) 0.0200(13) 0.0161(12) -0.0008(10) 0.0031(10) 0.0005(10) C4 0.0283(14) 0.0208(14) 0.0258(14) 0.0019(11) -0.0038(11) -0.0002(11) C1 0.0175(12) 0.0208(13) 0.0162(12) 0.0008(10) 0.0015(10) 0.0016(10) C2 0.0243(14) 0.0251(14) 0.0245(14) -0.0013(11) -0.0046(11) -0.0014(11) C14 0.0171(12) 0.0153(12) 0.0161(12) -0.0018(10) -0.0036(10) -0.0013(9) C15 0.0207(13) 0.0187(13) 0.0193(13) 0.0016(10) 0.0056(10) 0.0009(10) C16 0.0269(14) 0.0231(14) 0.0204(13) 0.0016(11) 0.0023(11) 0.0036(11) C17 0.0311(15) 0.0204(14) 0.0283(15) -0.0001(11) 0.0073(12) -0.0011(11) C18 0.0275(14) 0.0170(13) 0.0210(13) 0.0023(10) 0.0065(11) 0.0054(11) C12 0.0172(12) 0.0183(13) 0.0140(12) -0.0001(10) -0.0004(9) -0.0021(10) C13 0.0249(14) 0.0201(14) 0.0208(13) 0.0021(11) 0.0029(11) -0.0024(11) C10 0.0170(12) 0.0222(13) 0.0147(12) -0.0006(10) -0.0004(9) -0.0027(10) C11 0.0265(14) 0.0267(15) 0.0223(14) 0.0018(11) 0.0071(11) -0.0001(11) Fe1 0.01601(18) 0.01440(18) 0.01436(17) -0.00087(14) 0.00134(13) 0.00009(14) N4 0.0224(11) 0.0148(11) 0.0181(10) -0.0014(8) -0.0017(9) -0.0028(8) N3 0.0182(10) 0.0150(10) 0.0167(10) -0.0008(8) -0.0008(8) -0.0015(8) N2 0.0157(10) 0.0174(10) 0.0142(10) -0.0013(8) 0.0032(8) -0.0002(8) N1 0.0180(10) 0.0191(11) 0.0170(10) -0.0046(9) 0.0016(8) -0.0027(8) N8 0.0220(11) 0.0154(11) 0.0178(10) 0.0001(8) 0.0054(9) 0.0024(8) N7 0.0172(10) 0.0174(11) 0.0174(10) -0.0009(8) 0.0031(8) 0.0009(8) N6 0.0158(10) 0.0163(10) 0.0144(10) -0.0016(8) -0.0010(8) -0.0005(8) N5 0.0172(10) 0.0205(11) 0.0165(10) -0.0030(9) 0.0024(8) 0.0018(8) O2 0.0375(11) 0.0193(10) 0.0216(10) -0.0018(8) 0.0008(8) 0.0016(8) O1 0.0293(11) 0.0211(10) 0.0314(11) -0.0030(8) -0.0099(8) -0.0054(8) O4 0.0340(11) 0.0228(10) 0.0200(9) -0.0034(8) 0.0025(8) 0.0011(8) O3 0.0283(10) 0.0229(10) 0.0278(10) 0.0004(8) 0.0117(8) 0.0063(8) O1W 0.0304(11) 0.0365(12) 0.0414(13) 0.0033(10) 0.0090(10) 0.0053(10) O2W 0.0476(14) 0.0435(14) 0.0552(15) -0.0050(12) -0.0040(12) 0.0000(11) O3W 0.0446(14) 0.0475(14) 0.0408(13) 0.0087(11) 0.0015(11) 0.0069(11) S2 0.0217(3) 0.0148(3) 0.0193(3) 0.0003(2) -0.0025(2) -0.0001(2) S1 0.0224(3) 0.0145(3) 0.0211(3) 0.0012(2) 0.0072(3) 0.0014(2) Cl1 0.0536(5) 0.0240(4) 0.0302(4) 0.0005(3) -0.0099(3) -0.0021(3) _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 C5 N3 1.319(3) . ? C5 N4 1.358(3) . ? C5 S2 1.751(2) . ? C6 N4 1.462(3) . ? C6 C7 1.507(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O2 1.424(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O2 1.433(3) . ? C8 C9 1.502(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N4 1.467(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C3 N2 1.309(3) . ? C3 C1 1.453(3) . ? C3 C4 1.484(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C1 N1 1.295(3) . ? C1 C2 1.495(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C14 N7 1.322(3) . ? C14 N8 1.356(3) . ? C14 S1 1.746(2) . ? C15 N8 1.465(3) . ? C15 C16 1.517(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O4 1.422(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O4 1.427(3) . ? C17 C18 1.507(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N8 1.466(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C12 N6 1.313(3) . ? C12 C10 1.451(3) . ? C12 C13 1.492(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C10 N5 1.296(3) . ? C10 C11 1.489(3) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? Fe1 N6 1.908(2) . ? Fe1 N2 1.911(2) . ? Fe1 N1 1.954(2) . ? Fe1 N5 1.961(2) . ? Fe1 S1 2.2236(8) . ? Fe1 S2 2.2262(8) . ? N3 N2 1.372(3) . ? N1 O1 1.379(2) . ? N7 N6 1.372(3) . ? N5 O3 1.379(2) . ? O1 H2 0.8400 . ? O3 H4 0.8400 . ? O1W H2W1 0.900(16) . ? O1W H1W1 0.88(3) . ? O2W H1W2 0.954(16) . ? O2W H2W2 0.99(2) . ? O3W H1W3 1.02(3) . ? O3W H2W3 1.054(19) . ? 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 N3 C5 N4 118.1(2) . . ? N3 C5 S2 123.47(18) . . ? N4 C5 S2 118.40(17) . . ? N4 C6 C7 108.9(2) . . ? N4 C6 H6A 109.9 . . ? C7 C6 H6A 109.9 . . ? N4 C6 H6B 109.9 . . ? C7 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? O2 C7 C6 110.9(2) . . ? O2 C7 H7A 109.5 . . ? C6 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? O2 C8 C9 111.2(2) . . ? O2 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? O2 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N4 C9 C8 109.6(2) . . ? N4 C9 H9A 109.8 . . ? C8 C9 H9A 109.7 . . ? N4 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N2 C3 C1 112.6(2) . . ? N2 C3 C4 123.5(2) . . ? C1 C3 C4 123.8(2) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C1 C3 113.4(2) . . ? N1 C1 C2 123.8(2) . . ? C3 C1 C2 122.8(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N7 C14 N8 117.5(2) . . ? N7 C14 S1 123.52(18) . . ? N8 C14 S1 118.92(18) . . ? N8 C15 C16 108.9(2) . . ? N8 C15 H15A 109.9 . . ? C16 C15 H15A 109.9 . . ? N8 C15 H15B 109.9 . . ? C16 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? O4 C16 C15 110.8(2) . . ? O4 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? O4 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? O4 C17 C18 111.2(2) . . ? O4 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O4 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108.0 . . ? N8 C18 C17 109.2(2) . . ? N8 C18 H18A 109.8 . . ? C17 C18 H18A 109.8 . . ? N8 C18 H18B 109.8 . . ? C17 C18 H18B 109.8 . . ? H18A C18 H18B 108.3 . . ? N6 C12 C10 113.1(2) . . ? N6 C12 C13 122.9(2) . . ? C10 C12 C13 124.0(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C10 C12 113.2(2) . . ? N5 C10 C11 124.5(2) . . ? C12 C10 C11 122.3(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N6 Fe1 N2 174.25(8) . . ? N6 Fe1 N1 104.49(8) . . ? N2 Fe1 N1 79.47(8) . . ? N6 Fe1 N5 79.51(8) . . ? N2 Fe1 N5 105.06(8) . . ? N1 Fe1 N5 86.84(8) . . ? N6 Fe1 S1 84.67(6) . . ? N2 Fe1 S1 91.20(6) . . ? N1 Fe1 S1 90.23(6) . . ? N5 Fe1 S1 162.63(6) . . ? N6 Fe1 S2 91.94(6) . . ? N2 Fe1 S2 84.70(6) . . ? N1 Fe1 S2 162.12(6) . . ? N5 Fe1 S2 89.32(6) . . ? S1 Fe1 S2 98.40(3) . . ? C5 N4 C6 122.5(2) . . ? C5 N4 C9 120.2(2) . . ? C6 N4 C9 110.90(18) . . ? C5 N3 N2 111.60(19) . . ? C3 N2 N3 117.8(2) . . ? C3 N2 Fe1 117.81(16) . . ? N3 N2 Fe1 124.39(15) . . ? C1 N1 O1 114.33(19) . . ? C1 N1 Fe1 116.47(16) . . ? O1 N1 Fe1 129.13(15) . . ? C14 N8 C15 122.0(2) . . ? C14 N8 C18 120.4(2) . . ? C15 N8 C18 110.84(18) . . ? C14 N7 N6 111.36(19) . . ? C12 N6 N7 117.9(2) . . ? C12 N6 Fe1 117.65(16) . . ? N7 N6 Fe1 124.39(15) . . ? C10 N5 O3 114.5(2) . . ? C10 N5 Fe1 116.40(16) . . ? O3 N5 Fe1 128.84(15) . . ? C7 O2 C8 110.77(18) . . ? N1 O1 H2 109.5 . . ? C16 O4 C17 110.68(18) . . ? N5 O3 H4 109.5 . . ? H2W1 O1W H1W1 120(3) . . ? H1W2 O2W H2W2 99.6(18) . . ? H1W3 O3W H2W3 106(2) . . ? C5 S2 Fe1 95.52(8) . . ? C14 S1 Fe1 95.57(8) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.620 _refine_diff_density_min -0.565 _refine_diff_density_rms 0.085