Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Greg Brewer' _publ_contact_author_address ; Department of Chemistry Catholic University 620 Michigan Avenue 201 Maloney Hall Washington DC 20064 UNITED STATES OF AMERICA ; _publ_contact_author_email BREWER@CUA.EDU _publ_section_title ; Supramolecular assemblies prepared from an iron(II) tripodal complex containing 2-imidazolecarboxaldehyde. A molecular scaffolding for the self assembly of icosahedral complexes of potassium, rubidium, cesium and ammonium cations. ; loop_ _publ_author_name 'Greg Brewer' 'R. Butcher' 'Carol Viragh' 'Genevieve White' data_gw69am _database_code_depnum_ccdc_archive 'CCDC 628770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl3 Fe K N10 O12' _chemical_formula_weight 773.77 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' K K 0.2009 0.2494 '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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.389(2) _cell_length_b 13.389(2) _cell_length_c 9.174(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1424.4(6) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9900 _cell_measurement_theta_min 2.81 _cell_measurement_theta_max 29.54 _exptl_crystal_description hexagonal_plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.804 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 788 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6471 _exptl_absorpt_correction_T_max 0.7744 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16177 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0134 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 29.80 _reflns_number_total 2718 _reflns_number_gt 2548 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0372P)^2^+0.5009P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2718 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0689 _refine_ls_wR_factor_gt 0.0672 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _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 Fe Fe 0.6667 0.3333 0.13773(3) 0.01592(8) Uani 1 3 d S . . K1 K 1.0000 0.0000 0.0000 0.02754(13) Uani 1 6 d S . . K2 K 1.0000 0.0000 -0.5000 0.02347(12) Uani 1 6 d S . . Cl Cl 0.84481(2) -0.23069(2) -0.25597(3) 0.02539(8) Uani 1 1 d . . . O1 O 0.89598(9) -0.23770(9) -0.38958(11) 0.0350(2) Uani 1 1 d . . . O2 O 0.91026(11) -0.23629(10) -0.13617(11) 0.0425(3) Uani 1 1 d . . . O3 O 0.84971(9) -0.12072(8) -0.25009(12) 0.0338(2) Uani 1 1 d . . . O4 O 0.72801(9) -0.32124(9) -0.24754(14) 0.0446(3) Uani 1 1 d . . . N N 0.6667 0.3333 -0.2274(2) 0.0330(4) Uani 1 3 d S . . N1 N 0.53240(9) 0.31838(9) 0.03209(10) 0.02266(19) Uani 1 1 d . . . N2 N 0.54526(8) 0.21362(8) 0.25563(10) 0.02042(18) Uani 1 1 d . . . N3 N 0.36133(10) 0.11308(10) 0.30555(13) 0.0350(3) Uani 1 1 d . . . H3B H 0.2881 0.0859 0.3000 0.042 Uiso 1 1 calc R . . C1 C 0.56377(13) 0.34035(14) -0.23357(14) 0.0355(3) Uani 1 1 d . . . H1A H 0.4994 0.2642 -0.2545 0.043 Uiso 1 1 calc R . . H1B H 0.5703 0.3903 -0.3140 0.043 Uiso 1 1 calc R . . C2 C 0.53648(12) 0.38542(13) -0.09520(13) 0.0308(3) Uani 1 1 d . . . H2A H 0.5950 0.4655 -0.0806 0.037 Uiso 1 1 calc R . . H2B H 0.4627 0.3818 -0.1064 0.037 Uiso 1 1 calc R . . C3 C 0.43419(10) 0.25064(12) 0.09011(14) 0.0279(2) Uani 1 1 d . . . H3A H 0.3651 0.2414 0.0544 0.033 Uiso 1 1 calc R . . C4 C 0.44126(10) 0.19066(11) 0.21509(13) 0.0252(2) Uani 1 1 d . . . C5 C 0.41661(13) 0.08519(13) 0.40711(16) 0.0371(3) Uani 1 1 d . . . H5A H 0.3829 0.0333 0.4836 0.045 Uiso 1 1 calc R . . C6 C 0.53087(11) 0.14770(11) 0.37565(14) 0.0285(2) Uani 1 1 d . . . H6A H 0.5896 0.1458 0.4274 0.034 Uiso 1 1 calc R . . 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 Fe 0.01660(9) 0.01660(9) 0.01457(12) 0.000 0.000 0.00830(5) K1 0.03069(19) 0.03069(19) 0.0212(3) 0.000 0.000 0.01535(10) K2 0.02525(17) 0.02525(17) 0.0199(3) 0.000 0.000 0.01262(9) Cl 0.02600(14) 0.02210(13) 0.02679(14) 0.00223(9) 0.00245(10) 0.01107(11) O1 0.0352(5) 0.0398(5) 0.0301(5) -0.0022(4) 0.0050(4) 0.0188(4) O2 0.0537(6) 0.0429(6) 0.0332(5) 0.0115(4) -0.0039(5) 0.0260(5) O3 0.0340(5) 0.0257(4) 0.0446(5) -0.0003(4) -0.0015(4) 0.0172(4) O4 0.0303(5) 0.0294(5) 0.0593(7) -0.0043(5) 0.0119(5) 0.0039(4) N 0.0371(6) 0.0371(6) 0.0247(9) 0.000 0.000 0.0186(3) N1 0.0247(5) 0.0277(5) 0.0180(4) -0.0014(3) -0.0033(3) 0.0149(4) N2 0.0203(4) 0.0205(4) 0.0187(4) 0.0000(3) 0.0009(3) 0.0088(4) N3 0.0207(5) 0.0361(6) 0.0388(6) 0.0040(5) 0.0082(4) 0.0071(4) C1 0.0419(7) 0.0482(8) 0.0185(5) 0.0008(5) -0.0062(5) 0.0241(7) C2 0.0357(6) 0.0405(7) 0.0230(5) 0.0036(5) -0.0045(5) 0.0241(6) C3 0.0216(5) 0.0375(6) 0.0253(5) -0.0042(5) -0.0045(4) 0.0154(5) C4 0.0188(5) 0.0271(5) 0.0254(5) -0.0021(4) 0.0013(4) 0.0083(4) C5 0.0364(7) 0.0341(7) 0.0354(7) 0.0118(5) 0.0145(5) 0.0135(6) C6 0.0319(6) 0.0287(6) 0.0248(5) 0.0069(4) 0.0057(4) 0.0150(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 Fe N2 1.9432(10) 2_655 ? Fe N2 1.9432(10) . ? Fe N2 1.9432(10) 3_665 ? Fe N1 1.9624(10) . ? Fe N1 1.9624(10) 2_655 ? Fe N1 1.9624(10) 3_665 ? K1 O3 2.9451(12) 4_755 ? K1 O3 2.9451(12) 2_645 ? K1 O3 2.9451(12) 6_545 ? K1 O3 2.9451(12) 3_765 ? K1 O3 2.9451(12) 5_665 ? K1 O3 2.9451(12) . ? K1 O2 3.0351(13) 2_645 ? K1 O2 3.0351(13) 6_545 ? K1 O2 3.0351(13) 4_755 ? K1 O2 3.0351(13) 3_765 ? K1 O2 3.0351(13) 5_665 ? K1 O2 3.0351(13) . ? K2 O1 2.9432(11) 2_645 ? K2 O1 2.9432(11) 6_544 ? K2 O1 2.9432(11) 4_754 ? K2 O1 2.9432(11) 3_765 ? K2 O1 2.9432(11) 5_664 ? K2 O1 2.9432(11) . ? K2 O3 2.9438(12) 2_645 ? K2 O3 2.9438(12) 4_754 ? K2 O3 2.9438(12) 6_544 ? K2 O3 2.9438(12) 3_765 ? K2 O3 2.9438(12) 5_664 ? K2 O3 2.9438(12) . ? Cl O4 1.4232(11) . ? Cl O1 1.4301(10) . ? Cl O2 1.4309(11) . ? Cl O3 1.4417(10) . ? N C1 1.4281(15) 3_665 ? N C1 1.4281(15) 2_655 ? N C1 1.4281(15) . ? N1 C3 1.2816(16) . ? N1 C2 1.4572(15) . ? N2 C4 1.3206(15) . ? N2 C6 1.3633(15) . ? N3 C4 1.3422(16) . ? N3 C5 1.353(2) . ? N3 H3B 0.8600 . ? C1 C2 1.5263(19) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.4299(18) . ? C3 H3A 0.9300 . ? C5 C6 1.3580(19) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? 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 N2 Fe N2 92.02(4) 2_655 . ? N2 Fe N2 92.02(4) 2_655 3_665 ? N2 Fe N2 92.02(4) . 3_665 ? N2 Fe N1 173.02(4) 2_655 . ? N2 Fe N1 81.08(4) . . ? N2 Fe N1 89.27(4) 3_665 . ? N2 Fe N1 81.08(4) 2_655 2_655 ? N2 Fe N1 89.26(4) . 2_655 ? N2 Fe N1 173.02(4) 3_665 2_655 ? N1 Fe N1 97.71(4) . 2_655 ? N2 Fe N1 89.27(4) 2_655 3_665 ? N2 Fe N1 173.02(4) . 3_665 ? N2 Fe N1 81.08(4) 3_665 3_665 ? N1 Fe N1 97.71(4) . 3_665 ? N1 Fe N1 97.71(4) 2_655 3_665 ? O3 K1 O3 114.23(4) 4_755 2_645 ? O3 K1 O3 65.77(4) 4_755 6_545 ? O3 K1 O3 114.23(4) 2_645 6_545 ? O3 K1 O3 114.23(4) 4_755 3_765 ? O3 K1 O3 65.77(4) 2_645 3_765 ? O3 K1 O3 180.0 6_545 3_765 ? O3 K1 O3 65.77(4) 4_755 5_665 ? O3 K1 O3 180.0 2_645 5_665 ? O3 K1 O3 65.77(4) 6_545 5_665 ? O3 K1 O3 114.23(4) 3_765 5_665 ? O3 K1 O3 180.0 4_755 . ? O3 K1 O3 65.77(4) 2_645 . ? O3 K1 O3 114.23(4) 6_545 . ? O3 K1 O3 65.77(4) 3_765 . ? O3 K1 O3 114.23(4) 5_665 . ? O3 K1 O2 76.15(3) 4_755 2_645 ? O3 K1 O2 45.70(3) 2_645 2_645 ? O3 K1 O2 120.20(3) 6_545 2_645 ? O3 K1 O2 59.80(3) 3_765 2_645 ? O3 K1 O2 134.30(3) 5_665 2_645 ? O3 K1 O2 103.86(3) . 2_645 ? O3 K1 O2 59.80(3) 4_755 6_545 ? O3 K1 O2 76.15(3) 2_645 6_545 ? O3 K1 O2 45.70(3) 6_545 6_545 ? O3 K1 O2 134.30(3) 3_765 6_545 ? O3 K1 O2 103.86(3) 5_665 6_545 ? O3 K1 O2 120.20(3) . 6_545 ? O2 K1 O2 75.77(2) 2_645 6_545 ? O3 K1 O2 45.69(3) 4_755 4_755 ? O3 K1 O2 120.19(3) 2_645 4_755 ? O3 K1 O2 103.85(3) 6_545 4_755 ? O3 K1 O2 76.15(3) 3_765 4_755 ? O3 K1 O2 59.81(3) 5_665 4_755 ? O3 K1 O2 134.30(3) . 4_755 ? O2 K1 O2 75.76(2) 2_645 4_755 ? O2 K1 O2 104.23(2) 6_545 4_755 ? O3 K1 O2 120.20(3) 4_755 3_765 ? O3 K1 O2 103.86(3) 2_645 3_765 ? O3 K1 O2 134.30(3) 6_545 3_765 ? O3 K1 O2 45.70(3) 3_765 3_765 ? O3 K1 O2 76.14(3) 5_665 3_765 ? O3 K1 O2 59.80(3) . 3_765 ? O2 K1 O2 104.24(2) 2_645 3_765 ? O2 K1 O2 180.0 6_545 3_765 ? O2 K1 O2 75.77(2) 4_755 3_765 ? O3 K1 O2 103.86(3) 4_755 5_665 ? O3 K1 O2 134.30(3) 2_645 5_665 ? O3 K1 O2 59.80(3) 6_545 5_665 ? O3 K1 O2 120.19(3) 3_765 5_665 ? O3 K1 O2 45.70(3) 5_665 5_665 ? O3 K1 O2 76.14(3) . 5_665 ? O2 K1 O2 180.0 2_645 5_665 ? O2 K1 O2 104.23(2) 6_545 5_665 ? O2 K1 O2 104.24(2) 4_755 5_665 ? O2 K1 O2 75.76(2) 3_765 5_665 ? O3 K1 O2 134.30(3) 4_755 . ? O3 K1 O2 59.80(3) 2_645 . ? O3 K1 O2 76.15(3) 6_545 . ? O3 K1 O2 103.85(3) 3_765 . ? O3 K1 O2 120.19(3) 5_665 . ? O3 K1 O2 45.70(3) . . ? O2 K1 O2 104.24(2) 2_645 . ? O2 K1 O2 75.77(2) 6_545 . ? O2 K1 O2 180.0 4_755 . ? O2 K1 O2 104.23(2) 3_765 . ? O2 K1 O2 75.76(2) 5_665 . ? O1 K2 O1 71.20(2) 2_645 6_544 ? O1 K2 O1 71.20(2) 2_645 4_754 ? O1 K2 O1 108.80(2) 6_544 4_754 ? O1 K2 O1 108.80(2) 2_645 3_765 ? O1 K2 O1 180.0 6_544 3_765 ? O1 K2 O1 71.20(2) 4_754 3_765 ? O1 K2 O1 180.0 2_645 5_664 ? O1 K2 O1 108.80(2) 6_544 5_664 ? O1 K2 O1 108.80(2) 4_754 5_664 ? O1 K2 O1 71.20(2) 3_765 5_664 ? O1 K2 O1 108.80(2) 2_645 . ? O1 K2 O1 71.20(2) 6_544 . ? O1 K2 O1 180.0 4_754 . ? O1 K2 O1 108.80(2) 3_765 . ? O1 K2 O1 71.20(2) 5_664 . ? O1 K2 O3 46.70(3) 2_645 2_645 ? O1 K2 O3 72.53(3) 6_544 2_645 ? O1 K2 O3 114.75(3) 4_754 2_645 ? O1 K2 O3 107.48(3) 3_765 2_645 ? O1 K2 O3 133.30(3) 5_664 2_645 ? O1 K2 O3 65.25(3) . 2_645 ? O1 K2 O3 72.53(3) 2_645 4_754 ? O1 K2 O3 65.25(3) 6_544 4_754 ? O1 K2 O3 46.70(3) 4_754 4_754 ? O1 K2 O3 114.75(3) 3_765 4_754 ? O1 K2 O3 107.48(3) 5_664 4_754 ? O1 K2 O3 133.30(3) . 4_754 ? O3 K2 O3 114.20(4) 2_645 4_754 ? O1 K2 O3 114.75(3) 2_645 6_544 ? O1 K2 O3 46.70(3) 6_544 6_544 ? O1 K2 O3 107.48(3) 4_754 6_544 ? O1 K2 O3 133.30(3) 3_765 6_544 ? O1 K2 O3 65.25(3) 5_664 6_544 ? O1 K2 O3 72.52(3) . 6_544 ? O3 K2 O3 114.20(4) 2_645 6_544 ? O3 K2 O3 65.80(4) 4_754 6_544 ? O1 K2 O3 65.25(3) 2_645 3_765 ? O1 K2 O3 133.30(3) 6_544 3_765 ? O1 K2 O3 72.52(3) 4_754 3_765 ? O1 K2 O3 46.70(3) 3_765 3_765 ? O1 K2 O3 114.75(3) 5_664 3_765 ? O1 K2 O3 107.48(3) . 3_765 ? O3 K2 O3 65.80(4) 2_645 3_765 ? O3 K2 O3 114.20(4) 4_754 3_765 ? O3 K2 O3 179.999(1) 6_544 3_765 ? O1 K2 O3 133.30(3) 2_645 5_664 ? O1 K2 O3 107.48(3) 6_544 5_664 ? O1 K2 O3 65.25(3) 4_754 5_664 ? O1 K2 O3 72.52(3) 3_765 5_664 ? O1 K2 O3 46.70(3) 5_664 5_664 ? O1 K2 O3 114.75(3) . 5_664 ? O3 K2 O3 180.00(4) 2_645 5_664 ? O3 K2 O3 65.80(4) 4_754 5_664 ? O3 K2 O3 65.80(4) 6_544 5_664 ? O3 K2 O3 114.20(4) 3_765 5_664 ? O1 K2 O3 107.48(3) 2_645 . ? O1 K2 O3 114.75(3) 6_544 . ? O1 K2 O3 133.30(3) 4_754 . ? O1 K2 O3 65.25(3) 3_765 . ? O1 K2 O3 72.52(3) 5_664 . ? O1 K2 O3 46.70(3) . . ? O3 K2 O3 65.80(4) 2_645 . ? O3 K2 O3 180.0 4_754 . ? O3 K2 O3 114.20(4) 6_544 . ? O3 K2 O3 65.80(4) 3_765 . ? O3 K2 O3 114.20(4) 5_664 . ? O4 Cl O1 110.43(7) . . ? O4 Cl O2 110.76(7) . . ? O1 Cl O2 109.20(7) . . ? O4 Cl O3 109.72(6) . . ? O1 Cl O3 108.69(6) . . ? O2 Cl O3 107.97(7) . . ? O4 Cl K2 134.06(6) . . ? O1 Cl K2 54.68(4) . . ? O2 Cl K2 115.16(5) . . ? O3 Cl K2 54.80(4) . . ? O4 Cl K1 127.78(5) . . ? O1 Cl K1 121.71(5) . . ? O2 Cl K1 55.80(5) . . ? O3 Cl K1 52.21(4) . . ? K2 Cl K1 80.11(2) . . ? Cl O1 K2 101.96(5) . . ? Cl O2 K1 101.25(6) . . ? Cl O3 K2 101.61(5) . . ? Cl O3 K1 105.03(5) . . ? K2 O3 K1 102.33(4) . . ? C1 N C1 119.845(13) 3_665 2_655 ? C1 N C1 119.843(13) 3_665 . ? C1 N C1 119.842(13) 2_655 . ? C3 N1 C2 118.55(10) . . ? C3 N1 Fe 115.50(8) . . ? C2 N1 Fe 125.64(8) . . ? C4 N2 C6 106.59(10) . . ? C4 N2 Fe 112.64(8) . . ? C6 N2 Fe 140.61(9) . . ? C4 N3 C5 107.75(11) . . ? C4 N3 H3B 126.1 . . ? C5 N3 H3B 126.1 . . ? N C1 C2 114.99(12) . . ? N C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C1 111.44(11) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 113.45(10) . . ? N1 C3 H3A 123.3 . . ? C4 C3 H3A 123.3 . . ? N2 C4 N3 110.24(11) . . ? N2 C4 C3 116.96(10) . . ? N3 C4 C3 132.80(12) . . ? N3 C5 C6 106.66(12) . . ? N3 C5 H5A 126.7 . . ? C6 C5 H5A 126.7 . . ? C5 C6 N2 108.76(12) . . ? C5 C6 H6A 125.6 . . ? N2 C6 H6A 125.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 K2 Cl O4 177.84(7) 2_645 . . . ? O1 K2 Cl O4 -111.24(7) 6_544 . . . ? O1 K2 Cl O4 95.18(9) 4_754 . . . ? O1 K2 Cl O4 68.76(7) 3_765 . . . ? O1 K2 Cl O4 -2.16(7) 5_664 . . . ? O1 K2 Cl O4 -84.82(9) . . . . ? O3 K2 Cl O4 -179.86(7) 2_645 . . . ? O3 K2 Cl O4 -96.19(8) 4_754 . . . ? O3 K2 Cl O4 -64.51(7) 6_544 . . . ? O3 K2 Cl O4 115.49(7) 3_765 . . . ? O3 K2 Cl O4 0.14(7) 5_664 . . . ? O3 K2 Cl O4 83.81(8) . . . . ? O1 K2 Cl O1 -97.34(3) 2_645 . . . ? O1 K2 Cl O1 -26.42(5) 6_544 . . . ? O1 K2 Cl O1 180.0 4_754 . . . ? O1 K2 Cl O1 153.58(5) 3_765 . . . ? O1 K2 Cl O1 82.66(3) 5_664 . . . ? O3 K2 Cl O1 -95.05(6) 2_645 . . . ? O3 K2 Cl O1 -11.37(8) 4_754 . . . ? O3 K2 Cl O1 20.31(6) 6_544 . . . ? O3 K2 Cl O1 -159.69(6) 3_765 . . . ? O3 K2 Cl O1 84.95(6) 5_664 . . . ? O3 K2 Cl O1 168.62(8) . . . . ? O1 K2 Cl O2 -0.89(6) 2_645 . . . ? O1 K2 Cl O2 70.04(6) 6_544 . . . ? O1 K2 Cl O2 -83.54(8) 4_754 . . . ? O1 K2 Cl O2 -109.96(6) 3_765 . . . ? O1 K2 Cl O2 179.11(6) 5_664 . . . ? O1 K2 Cl O2 96.46(8) . . . . ? O3 K2 Cl O2 1.41(6) 2_645 . . . ? O3 K2 Cl O2 85.08(8) 4_754 . . . ? O3 K2 Cl O2 116.76(6) 6_544 . . . ? O3 K2 Cl O2 -63.24(6) 3_765 . . . ? O3 K2 Cl O2 -178.59(6) 5_664 . . . ? O3 K2 Cl O2 -94.92(8) . . . . ? O1 K2 Cl O3 94.03(6) 2_645 . . . ? O1 K2 Cl O3 164.96(5) 6_544 . . . ? O1 K2 Cl O3 11.37(8) 4_754 . . . ? O1 K2 Cl O3 -15.04(5) 3_765 . . . ? O1 K2 Cl O3 -85.97(6) 5_664 . . . ? O1 K2 Cl O3 -168.62(8) . . . . ? O3 K2 Cl O3 96.33(7) 2_645 . . . ? O3 K2 Cl O3 180.0 4_754 . . . ? O3 K2 Cl O3 -148.32(5) 6_544 . . . ? O3 K2 Cl O3 31.68(5) 3_765 . . . ? O3 K2 Cl O3 -83.67(7) 5_664 . . . ? O1 K2 Cl K1 43.69(2) 2_645 . . . ? O1 K2 Cl K1 114.61(2) 6_544 . . . ? O1 K2 Cl K1 -38.97(5) 4_754 . . . ? O1 K2 Cl K1 -65.39(2) 3_765 . . . ? O1 K2 Cl K1 -136.31(2) 5_664 . . . ? O1 K2 Cl K1 141.03(5) . . . . ? O3 K2 Cl K1 45.98(2) 2_645 . . . ? O3 K2 Cl K1 129.66(5) 4_754 . . . ? O3 K2 Cl K1 161.336(19) 6_544 . . . ? O3 K2 Cl K1 -18.665(19) 3_765 . . . ? O3 K2 Cl K1 -134.02(2) 5_664 . . . ? O3 K2 Cl K1 -50.35(5) . . . . ? O3 K1 Cl O4 93.47(9) 4_755 . . . ? O3 K1 Cl O4 174.20(7) 2_645 . . . ? O3 K1 Cl O4 59.41(7) 6_545 . . . ? O3 K1 Cl O4 -120.59(7) 3_765 . . . ? O3 K1 Cl O4 -5.80(7) 5_665 . . . ? O3 K1 Cl O4 -86.52(9) . . . . ? O2 K1 Cl O4 -177.30(7) 2_645 . . . ? O2 K1 Cl O4 105.40(7) 6_545 . . . ? O2 K1 Cl O4 -89.11(9) 4_755 . . . ? O2 K1 Cl O4 -74.60(7) 3_765 . . . ? O2 K1 Cl O4 2.69(7) 5_665 . . . ? O2 K1 Cl O4 90.89(9) . . . . ? O3 K1 Cl O1 -90.14(8) 4_755 . . . ? O3 K1 Cl O1 -9.42(6) 2_645 . . . ? O3 K1 Cl O1 -124.21(6) 6_545 . . . ? O3 K1 Cl O1 55.80(6) 3_765 . . . ? O3 K1 Cl O1 170.58(6) 5_665 . . . ? O3 K1 Cl O1 89.86(8) . . . . ? O2 K1 Cl O1 -0.92(6) 2_645 . . . ? O2 K1 Cl O1 -78.22(6) 6_545 . . . ? O2 K1 Cl O1 87.28(8) 4_755 . . . ? O2 K1 Cl O1 101.78(6) 3_765 . . . ? O2 K1 Cl O1 179.08(6) 5_665 . . . ? O2 K1 Cl O1 -92.72(8) . . . . ? O3 K1 Cl O2 2.58(8) 4_755 . . . ? O3 K1 Cl O2 83.30(6) 2_645 . . . ? O3 K1 Cl O2 -31.48(6) 6_545 . . . ? O3 K1 Cl O2 148.52(6) 3_765 . . . ? O3 K1 Cl O2 -96.70(6) 5_665 . . . ? O3 K1 Cl O2 -177.42(8) . . . . ? O2 K1 Cl O2 91.80(4) 2_645 . . . ? O2 K1 Cl O2 14.50(6) 6_545 . . . ? O2 K1 Cl O2 180.0 4_755 . . . ? O2 K1 Cl O2 -165.50(6) 3_765 . . . ? O2 K1 Cl O2 -88.20(4) 5_665 . . . ? O3 K1 Cl O3 180.0 4_755 . . . ? O3 K1 Cl O3 -99.28(8) 2_645 . . . ? O3 K1 Cl O3 145.93(5) 6_545 . . . ? O3 K1 Cl O3 -34.07(5) 3_765 . . . ? O3 K1 Cl O3 80.72(8) 5_665 . . . ? O2 K1 Cl O3 -90.78(6) 2_645 . . . ? O2 K1 Cl O3 -168.08(6) 6_545 . . . ? O2 K1 Cl O3 -2.59(8) 4_755 . . . ? O2 K1 Cl O3 11.92(6) 3_765 . . . ? O2 K1 Cl O3 89.22(6) 5_665 . . . ? O2 K1 Cl O3 177.42(8) . . . . ? O3 K1 Cl K2 -127.24(5) 4_755 . . . ? O3 K1 Cl K2 -46.52(2) 2_645 . . . ? O3 K1 Cl K2 -161.306(19) 6_545 . . . ? O3 K1 Cl K2 18.695(19) 3_765 . . . ? O3 K1 Cl K2 133.48(2) 5_665 . . . ? O3 K1 Cl K2 52.76(5) . . . . ? O2 K1 Cl K2 -38.02(3) 2_645 . . . ? O2 K1 Cl K2 -115.32(2) 6_545 . . . ? O2 K1 Cl K2 50.18(6) 4_755 . . . ? O2 K1 Cl K2 64.68(2) 3_765 . . . ? O2 K1 Cl K2 141.98(3) 5_665 . . . ? O2 K1 Cl K2 -129.82(6) . . . . ? O4 Cl O1 K2 130.21(6) . . . . ? O2 Cl O1 K2 -107.76(6) . . . . ? O3 Cl O1 K2 9.80(6) . . . . ? K1 Cl O1 K2 -46.74(5) . . . . ? O1 K2 O1 Cl 90.38(4) 2_645 . . . ? O1 K2 O1 Cl 151.98(6) 6_544 . . . ? O1 K2 O1 Cl -31(37) 4_754 . . . ? O1 K2 O1 Cl -28.02(6) 3_765 . . . ? O1 K2 O1 Cl -89.62(4) 5_664 . . . ? O3 K2 O1 Cl 73.07(5) 2_645 . . . ? O3 K2 O1 Cl 173.78(4) 4_754 . . . ? O3 K2 O1 Cl -158.73(6) 6_544 . . . ? O3 K2 O1 Cl 21.27(6) 3_765 . . . ? O3 K2 O1 Cl -106.93(5) 5_664 . . . ? O3 K2 O1 Cl -6.23(4) . . . . ? O4 Cl O2 K1 -122.31(6) . . . . ? O1 Cl O2 K1 115.87(6) . . . . ? O3 Cl O2 K1 -2.15(7) . . . . ? K2 Cl O2 K1 56.71(5) . . . . ? O3 K1 O2 Cl -178.61(4) 4_755 . . . ? O3 K1 O2 Cl -83.12(6) 2_645 . . . ? O3 K1 O2 Cl 147.64(6) 6_545 . . . ? O3 K1 O2 Cl -32.36(6) 3_765 . . . ? O3 K1 O2 Cl 96.88(6) 5_665 . . . ? O3 K1 O2 Cl 1.40(4) . . . . ? O2 K1 O2 Cl -94.21(4) 2_645 . . . ? O2 K1 O2 Cl -165.18(6) 6_545 . . . ? O2 K1 O2 Cl -117(3) 4_755 . . . ? O2 K1 O2 Cl 14.83(6) 3_765 . . . ? O2 K1 O2 Cl 85.79(4) 5_665 . . . ? O4 Cl O3 K2 -130.63(6) . . . . ? O1 Cl O3 K2 -9.78(6) . . . . ? O2 Cl O3 K2 108.56(6) . . . . ? K1 Cl O3 K2 106.31(5) . . . . ? O4 Cl O3 K1 123.06(6) . . . . ? O1 Cl O3 K1 -116.09(6) . . . . ? O2 Cl O3 K1 2.25(7) . . . . ? K2 Cl O3 K1 -106.31(5) . . . . ? O1 K2 O3 Cl -93.48(5) 2_645 . . . ? O1 K2 O3 Cl -16.60(6) 6_544 . . . ? O1 K2 O3 Cl -173.83(4) 4_754 . . . ? O1 K2 O3 Cl 163.40(6) 3_765 . . . ? O1 K2 O3 Cl 86.52(5) 5_664 . . . ? O1 K2 O3 Cl 6.17(4) . . . . ? O3 K2 O3 Cl -71.87(6) 2_645 . . . ? O3 K2 O3 Cl 114.33(9) 4_754 . . . ? O3 K2 O3 Cl 35.04(5) 6_544 . . . ? O3 K2 O3 Cl -144.96(5) 3_765 . . . ? O3 K2 O3 Cl 108.13(6) 5_664 . . . ? O1 K2 O3 K1 14.93(4) 2_645 . . . ? O1 K2 O3 K1 91.82(3) 6_544 . . . ? O1 K2 O3 K1 -65.42(4) 4_754 . . . ? O1 K2 O3 K1 -88.18(3) 3_765 . . . ? O1 K2 O3 K1 -165.07(4) 5_664 . . . ? O1 K2 O3 K1 114.58(4) . . . . ? O3 K2 O3 K1 36.549(9) 2_645 . . . ? O3 K2 O3 K1 -137.26(5) 4_754 . . . ? O3 K2 O3 K1 143.451(9) 6_544 . . . ? O3 K2 O3 K1 -36.550(9) 3_765 . . . ? O3 K2 O3 K1 -143.451(9) 5_664 . . . ? O3 K1 O3 Cl -113(4) 4_755 . . . ? O3 K1 O3 Cl 69.24(7) 2_645 . . . ? O3 K1 O3 Cl -37.68(5) 6_545 . . . ? O3 K1 O3 Cl 142.32(5) 3_765 . . . ? O3 K1 O3 Cl -110.76(7) 5_665 . . . ? O2 K1 O3 Cl 95.09(6) 2_645 . . . ? O2 K1 O3 Cl 13.69(7) 6_545 . . . ? O2 K1 O3 Cl 178.59(4) 4_755 . . . ? O2 K1 O3 Cl -166.31(7) 3_765 . . . ? O2 K1 O3 Cl -84.91(6) 5_665 . . . ? O2 K1 O3 Cl -1.41(4) . . . . ? O3 K1 O3 K2 141(4) 4_755 . . . ? O3 K1 O3 K2 -36.541(9) 2_645 . . . ? O3 K1 O3 K2 -143.459(9) 6_545 . . . ? O3 K1 O3 K2 36.542(9) 3_765 . . . ? O3 K1 O3 K2 143.459(9) 5_665 . . . ? O2 K1 O3 K2 -10.69(4) 2_645 . . . ? O2 K1 O3 K2 -92.09(3) 6_545 . . . ? O2 K1 O3 K2 72.81(5) 4_755 . . . ? O2 K1 O3 K2 87.91(3) 3_765 . . . ? O2 K1 O3 K2 169.31(4) 5_665 . . . ? O2 K1 O3 K2 -107.18(5) . . . . ? N2 Fe N1 C3 14.2(4) 2_655 . . . ? N2 Fe N1 C3 5.66(9) . . . . ? N2 Fe N1 C3 -86.50(10) 3_665 . . . ? N1 Fe N1 C3 93.69(11) 2_655 . . . ? N1 Fe N1 C3 -167.40(9) 3_665 . . . ? N2 Fe N1 C2 -172.4(3) 2_655 . . . ? N2 Fe N1 C2 179.13(10) . . . . ? N2 Fe N1 C2 86.97(10) 3_665 . . . ? N1 Fe N1 C2 -92.84(8) 2_655 . . . ? N1 Fe N1 C2 6.08(10) 3_665 . . . ? N2 Fe N2 C4 176.35(8) 2_655 . . . ? N2 Fe N2 C4 84.26(10) 3_665 . . . ? N1 Fe N2 C4 -4.68(8) . . . . ? N1 Fe N2 C4 -102.60(9) 2_655 . . . ? N1 Fe N2 C4 75.9(3) 3_665 . . . ? N2 Fe N2 C6 1.77(13) 2_655 . . . ? N2 Fe N2 C6 -90.32(11) 3_665 . . . ? N1 Fe N2 C6 -179.26(13) . . . . ? N1 Fe N2 C6 82.82(13) 2_655 . . . ? N1 Fe N2 C6 -98.7(3) 3_665 . . . ? C1 N C1 C2 -73.5(2) 3_665 . . . ? C1 N C1 C2 114.40(18) 2_655 . . . ? C3 N1 C2 C1 -108.15(14) . . . . ? Fe N1 C2 C1 78.55(13) . . . . ? N C1 C2 N1 -54.78(16) . . . . ? C2 N1 C3 C4 -179.27(11) . . . . ? Fe N1 C3 C4 -5.30(14) . . . . ? C6 N2 C4 N3 0.39(14) . . . . ? Fe N2 C4 N3 -176.02(8) . . . . ? C6 N2 C4 C3 179.76(11) . . . . ? Fe N2 C4 C3 3.34(14) . . . . ? C5 N3 C4 N2 -0.31(16) . . . . ? C5 N3 C4 C3 -179.54(14) . . . . ? N1 C3 C4 N2 1.28(17) . . . . ? N1 C3 C4 N3 -179.53(13) . . . . ? C4 N3 C5 C6 0.10(16) . . . . ? N3 C5 C6 N2 0.14(16) . . . . ? C4 N2 C6 C5 -0.33(14) . . . . ? Fe N2 C6 C5 174.46(10) . . . . ? 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 N3 H3B O3 0.86 2.17 2.9229(16) 146.7 4_655 N3 H3B O1 0.86 2.48 3.0781(16) 127.1 6_445 N3 H3B O2 0.86 2.63 3.2016(18) 124.8 6_445 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.338 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.049 #===END data_gw72bm _database_code_depnum_ccdc_archive 'CCDC 630381' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl3 Fe N10 O12 Rb' _chemical_formula_weight 820.14 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' 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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.4744(8) _cell_length_b 13.4744(8) _cell_length_c 9.3487(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1469.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8229 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 30.44 _exptl_crystal_description chunk _exptl_crystal_colour translucent _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.853 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 2.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3445 _exptl_absorpt_correction_T_max 0.5008 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16933 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0174 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 30.83 _reflns_number_total 2919 _reflns_number_gt 2567 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0286P)^2^+0.6681P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2919 _refine_ls_number_parameters 141 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0292 _refine_ls_R_factor_gt 0.0233 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0571 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _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 Fe Fe 0.3333 0.6667 0.35743(3) 0.01480(7) Uani 1 3 d S . . Rb1 Rb 1.0000 1.0000 0.0000 0.02216(8) Uani 1 6 d S . . Rb2 Rb 1.0000 1.0000 0.5000 0.02488(8) Uani 1 6 d S . . Cl Cl 0.83852(3) 1.07455(3) 0.24369(4) 0.02440(8) Uani 1 1 d . . . O1 O 0.84357(10) 0.96950(9) 0.24920(12) 0.0296(2) Uani 1 1 d . . . O2 O 0.88853(11) 1.13301(10) 0.11176(12) 0.0330(2) Uani 1 1 d . . . O3 O 0.90488(12) 1.14644(11) 0.36081(13) 0.0409(3) Uani 1 1 d . . . O4 O 0.72184(11) 1.04814(12) 0.25344(16) 0.0459(3) Uani 1 1 d . . . N N 0.3333 0.6667 0.7186(2) 0.0299(5) Uani 1 3 d S . . N1 N 0.46877(10) 0.78363(10) 0.46217(12) 0.0209(2) Uani 1 1 d . . . N2 N 0.45336(9) 0.66585(10) 0.24078(12) 0.0190(2) Uani 1 1 d . . . N3 N 0.63701(12) 0.74511(14) 0.19246(17) 0.0344(3) Uani 1 1 d . . . H3N H 0.701(2) 0.786(2) 0.198(3) 0.045(6) Uiso 1 1 d . . . C1 C 0.43744(15) 0.77565(15) 0.72442(16) 0.0319(3) Uani 1 1 d . . . H1A H 0.5018 0.7623 0.7459 0.038 Uiso 1 1 calc R . . H1B H 0.4316 0.8205 0.8046 0.038 Uiso 1 1 calc R . . C2 C 0.46607(14) 0.84761(13) 0.58737(15) 0.0284(3) Uani 1 1 d . . . H2A H 0.4079 0.8710 0.5724 0.034 Uiso 1 1 calc R . . H2B H 0.5416 0.9179 0.5984 0.034 Uiso 1 1 calc R . . C3 C 0.56667(12) 0.81163(13) 0.40565(16) 0.0261(3) Uani 1 1 d . . . H3A H 0.6375 0.8709 0.4422 0.031 Uiso 1 1 calc R . . C4 C 0.55807(12) 0.74436(13) 0.28196(15) 0.0240(3) Uani 1 1 d . . . C5 C 0.46633(13) 0.61433(13) 0.12125(16) 0.0271(3) Uani 1 1 d . . . H5A H 0.4060 0.5543 0.0683 0.033 Uiso 1 1 calc R . . C6 C 0.58090(15) 0.66390(16) 0.09094(19) 0.0359(4) Uani 1 1 d . . . H6A H 0.6145 0.6451 0.0139 0.043 Uiso 1 1 calc R . . 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 Fe 0.01492(9) 0.01492(9) 0.01457(14) 0.000 0.000 0.00746(5) Rb1 0.02411(10) 0.02411(10) 0.01825(14) 0.000 0.000 0.01206(5) Rb2 0.02831(11) 0.02831(11) 0.01803(15) 0.000 0.000 0.01415(6) Cl 0.02524(16) 0.02522(16) 0.02585(17) 0.00044(12) 0.00212(12) 0.01495(13) O1 0.0327(6) 0.0236(5) 0.0353(6) -0.0003(4) -0.0012(4) 0.0162(5) O2 0.0365(6) 0.0333(6) 0.0293(6) 0.0071(5) 0.0057(5) 0.0175(5) O3 0.0554(8) 0.0410(7) 0.0320(6) -0.0145(5) -0.0057(6) 0.0284(6) O4 0.0295(6) 0.0519(8) 0.0648(9) 0.0186(7) 0.0133(6) 0.0267(6) N 0.0333(7) 0.0333(7) 0.0232(10) 0.000 0.000 0.0166(4) N1 0.0227(5) 0.0201(5) 0.0173(5) -0.0010(4) -0.0028(4) 0.0087(4) N2 0.0184(5) 0.0207(5) 0.0192(5) 0.0012(4) 0.0013(4) 0.0107(4) N3 0.0198(6) 0.0409(8) 0.0392(8) 0.0039(6) 0.0089(6) 0.0126(6) C1 0.0358(8) 0.0369(8) 0.0191(7) -0.0061(6) -0.0056(6) 0.0152(7) C2 0.0323(8) 0.0246(7) 0.0224(7) -0.0076(5) -0.0049(6) 0.0097(6) C3 0.0189(6) 0.0266(7) 0.0246(7) 0.0006(5) -0.0036(5) 0.0053(5) C4 0.0175(6) 0.0279(7) 0.0249(6) 0.0045(5) 0.0024(5) 0.0102(5) C5 0.0296(7) 0.0275(7) 0.0249(7) -0.0015(6) 0.0065(6) 0.0147(6) C6 0.0353(9) 0.0402(9) 0.0353(9) 0.0015(7) 0.0153(7) 0.0211(8) _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 Fe N2 1.9552(11) 3_565 ? Fe N2 1.9553(11) 2_665 ? Fe N2 1.9552(11) . ? Fe N1 1.9741(12) 2_665 ? Fe N1 1.9740(12) . ? Fe N1 1.9740(12) 3_565 ? Rb1 O1 3.0287(12) 6_655 ? Rb1 O1 3.0287(12) 2_765 ? Rb1 O1 3.0287(12) . ? Rb1 O1 3.0287(12) 4_775 ? Rb1 O1 3.0288(12) 5_565 ? Rb1 O1 3.0288(12) 3_675 ? Rb1 O2 3.0416(12) 6_655 ? Rb1 O2 3.0417(12) 3_675 ? Rb1 O2 3.0417(12) 2_765 ? Rb1 O2 3.0417(12) . ? Rb1 O2 3.0417(12) 4_775 ? Rb1 O2 3.0418(12) 5_565 ? Rb2 O1 3.0402(12) . ? Rb2 O1 3.0402(12) 6_656 ? Rb2 O1 3.0402(11) 2_765 ? Rb2 O1 3.0402(12) 4_776 ? Rb2 O1 3.0403(11) 5_566 ? Rb2 O1 3.0403(12) 3_675 ? Rb2 O3 3.1238(14) 2_765 ? Rb2 O3 3.1238(14) 6_656 ? Rb2 O3 3.1238(14) . ? Rb2 O3 3.1238(14) 4_776 ? Rb2 O3 3.1239(14) 3_675 ? Rb2 O3 3.1239(14) 5_566 ? Cl O4 1.4307(12) . ? Cl O2 1.4370(12) . ? Cl O3 1.4389(13) . ? Cl O1 1.4517(11) . ? N C1 1.4378(17) 2_665 ? N C1 1.4378(17) . ? N C1 1.4378(17) 3_565 ? N1 C3 1.2900(19) . ? N1 C2 1.4649(18) . ? N2 C4 1.3287(18) . ? N2 C5 1.3720(18) . ? N3 C4 1.3493(19) . ? N3 C6 1.357(2) . ? N3 H3N 0.76(2) . ? C1 C2 1.535(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.438(2) . ? C3 H3A 0.9500 . ? C5 C6 1.371(2) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? 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 N2 Fe N2 91.92(5) 3_565 2_665 ? N2 Fe N2 91.91(5) 3_565 . ? N2 Fe N2 91.91(5) 2_665 . ? N2 Fe N1 89.65(5) 3_565 2_665 ? N2 Fe N1 81.03(5) 2_665 2_665 ? N2 Fe N1 172.82(5) . 2_665 ? N2 Fe N1 172.82(5) 3_565 . ? N2 Fe N1 89.64(5) 2_665 . ? N2 Fe N1 81.03(5) . . ? N1 Fe N1 97.52(5) 2_665 . ? N2 Fe N1 81.03(5) 3_565 3_565 ? N2 Fe N1 172.83(5) 2_665 3_565 ? N2 Fe N1 89.64(5) . 3_565 ? N1 Fe N1 97.52(5) 2_665 3_565 ? N1 Fe N1 97.52(5) . 3_565 ? O1 Rb1 O1 112.80(3) 6_655 2_765 ? O1 Rb1 O1 112.80(4) 6_655 . ? O1 Rb1 O1 67.20(3) 2_765 . ? O1 Rb1 O1 67.20(3) 6_655 4_775 ? O1 Rb1 O1 112.80(3) 2_765 4_775 ? O1 Rb1 O1 180.0 . 4_775 ? O1 Rb1 O1 67.20(3) 6_655 5_565 ? O1 Rb1 O1 179.999(1) 2_765 5_565 ? O1 Rb1 O1 112.80(3) . 5_565 ? O1 Rb1 O1 67.20(3) 4_775 5_565 ? O1 Rb1 O1 180.0 6_655 3_675 ? O1 Rb1 O1 67.20(3) 2_765 3_675 ? O1 Rb1 O1 67.20(3) . 3_675 ? O1 Rb1 O1 112.80(3) 4_775 3_675 ? O1 Rb1 O1 112.80(3) 5_565 3_675 ? O1 Rb1 O2 45.61(3) 6_655 6_655 ? O1 Rb1 O2 113.86(3) 2_765 6_655 ? O1 Rb1 O2 71.87(3) . 6_655 ? O1 Rb1 O2 108.13(3) 4_775 6_655 ? O1 Rb1 O2 66.15(3) 5_565 6_655 ? O1 Rb1 O2 134.39(3) 3_675 6_655 ? O1 Rb1 O2 134.39(3) 6_655 3_675 ? O1 Rb1 O2 66.15(3) 2_765 3_675 ? O1 Rb1 O2 108.13(3) . 3_675 ? O1 Rb1 O2 71.87(3) 4_775 3_675 ? O1 Rb1 O2 113.85(3) 5_565 3_675 ? O1 Rb1 O2 45.61(3) 3_675 3_675 ? O2 Rb1 O2 180.0 6_655 3_675 ? O1 Rb1 O2 71.87(3) 6_655 2_765 ? O1 Rb1 O2 45.62(3) 2_765 2_765 ? O1 Rb1 O2 66.15(3) . 2_765 ? O1 Rb1 O2 113.86(3) 4_775 2_765 ? O1 Rb1 O2 134.39(3) 5_565 2_765 ? O1 Rb1 O2 108.13(3) 3_675 2_765 ? O2 Rb1 O2 71.16(2) 6_655 2_765 ? O2 Rb1 O2 108.85(2) 3_675 2_765 ? O1 Rb1 O2 113.85(3) 6_655 . ? O1 Rb1 O2 108.13(3) 2_765 . ? O1 Rb1 O2 45.62(3) . . ? O1 Rb1 O2 134.38(3) 4_775 . ? O1 Rb1 O2 71.87(3) 5_565 . ? O1 Rb1 O2 66.15(3) 3_675 . ? O2 Rb1 O2 71.16(2) 6_655 . ? O2 Rb1 O2 108.84(2) 3_675 . ? O2 Rb1 O2 108.84(2) 2_765 . ? O1 Rb1 O2 66.15(3) 6_655 4_775 ? O1 Rb1 O2 71.87(3) 2_765 4_775 ? O1 Rb1 O2 134.38(3) . 4_775 ? O1 Rb1 O2 45.62(3) 4_775 4_775 ? O1 Rb1 O2 108.13(3) 5_565 4_775 ? O1 Rb1 O2 113.85(3) 3_675 4_775 ? O2 Rb1 O2 108.84(2) 6_655 4_775 ? O2 Rb1 O2 71.16(2) 3_675 4_775 ? O2 Rb1 O2 71.16(2) 2_765 4_775 ? O2 Rb1 O2 180.0 . 4_775 ? O1 Rb1 O2 108.13(3) 6_655 5_565 ? O1 Rb1 O2 134.38(3) 2_765 5_565 ? O1 Rb1 O2 113.85(3) . 5_565 ? O1 Rb1 O2 66.14(3) 4_775 5_565 ? O1 Rb1 O2 45.61(3) 5_565 5_565 ? O1 Rb1 O2 71.87(3) 3_675 5_565 ? O2 Rb1 O2 108.84(2) 6_655 5_565 ? O2 Rb1 O2 71.15(2) 3_675 5_565 ? O2 Rb1 O2 180.00(5) 2_765 5_565 ? O2 Rb1 O2 71.15(2) . 5_565 ? O2 Rb1 O2 108.84(2) 4_775 5_565 ? O1 Rb2 O1 113.09(4) . 6_656 ? O1 Rb2 O1 66.91(4) . 2_765 ? O1 Rb2 O1 113.09(4) 6_656 2_765 ? O1 Rb2 O1 180.0 . 4_776 ? O1 Rb2 O1 66.91(4) 6_656 4_776 ? O1 Rb2 O1 113.09(4) 2_765 4_776 ? O1 Rb2 O1 113.09(4) . 5_566 ? O1 Rb2 O1 66.91(4) 6_656 5_566 ? O1 Rb2 O1 180.0 2_765 5_566 ? O1 Rb2 O1 66.91(3) 4_776 5_566 ? O1 Rb2 O1 66.91(4) . 3_675 ? O1 Rb2 O1 180.0 6_656 3_675 ? O1 Rb2 O1 66.91(3) 2_765 3_675 ? O1 Rb2 O1 113.09(4) 4_776 3_675 ? O1 Rb2 O1 113.09(4) 5_566 3_675 ? O1 Rb2 O3 60.25(3) . 2_765 ? O1 Rb2 O3 75.88(3) 6_656 2_765 ? O1 Rb2 O3 44.64(3) 2_765 2_765 ? O1 Rb2 O3 119.75(3) 4_776 2_765 ? O1 Rb2 O3 135.36(3) 5_566 2_765 ? O1 Rb2 O3 104.12(3) 3_675 2_765 ? O1 Rb2 O3 75.88(3) . 6_656 ? O1 Rb2 O3 44.64(3) 6_656 6_656 ? O1 Rb2 O3 119.75(3) 2_765 6_656 ? O1 Rb2 O3 104.12(3) 4_776 6_656 ? O1 Rb2 O3 60.25(3) 5_566 6_656 ? O1 Rb2 O3 135.36(3) 3_675 6_656 ? O3 Rb2 O3 76.13(3) 2_765 6_656 ? O1 Rb2 O3 44.64(3) . . ? O1 Rb2 O3 119.75(3) 6_656 . ? O1 Rb2 O3 104.12(3) 2_765 . ? O1 Rb2 O3 135.36(3) 4_776 . ? O1 Rb2 O3 75.88(3) 5_566 . ? O1 Rb2 O3 60.25(3) 3_675 . ? O3 Rb2 O3 103.87(3) 2_765 . ? O3 Rb2 O3 76.13(3) 6_656 . ? O1 Rb2 O3 135.36(3) . 4_776 ? O1 Rb2 O3 60.25(3) 6_656 4_776 ? O1 Rb2 O3 75.88(3) 2_765 4_776 ? O1 Rb2 O3 44.64(3) 4_776 4_776 ? O1 Rb2 O3 104.12(3) 5_566 4_776 ? O1 Rb2 O3 119.75(3) 3_675 4_776 ? O3 Rb2 O3 76.13(3) 2_765 4_776 ? O3 Rb2 O3 103.87(3) 6_656 4_776 ? O3 Rb2 O3 180.0 . 4_776 ? O1 Rb2 O3 104.12(3) . 3_675 ? O1 Rb2 O3 135.36(3) 6_656 3_675 ? O1 Rb2 O3 60.25(3) 2_765 3_675 ? O1 Rb2 O3 75.88(3) 4_776 3_675 ? O1 Rb2 O3 119.74(3) 5_566 3_675 ? O1 Rb2 O3 44.64(3) 3_675 3_675 ? O3 Rb2 O3 103.87(3) 2_765 3_675 ? O3 Rb2 O3 180.0 6_656 3_675 ? O3 Rb2 O3 103.87(3) . 3_675 ? O3 Rb2 O3 76.13(3) 4_776 3_675 ? O1 Rb2 O3 119.75(3) . 5_566 ? O1 Rb2 O3 104.12(3) 6_656 5_566 ? O1 Rb2 O3 135.36(3) 2_765 5_566 ? O1 Rb2 O3 60.25(3) 4_776 5_566 ? O1 Rb2 O3 44.64(3) 5_566 5_566 ? O1 Rb2 O3 75.88(3) 3_675 5_566 ? O3 Rb2 O3 180.0 2_765 5_566 ? O3 Rb2 O3 103.87(3) 6_656 5_566 ? O3 Rb2 O3 76.13(3) . 5_566 ? O3 Rb2 O3 103.87(3) 4_776 5_566 ? O3 Rb2 O3 76.13(3) 3_675 5_566 ? O4 Cl O2 110.30(8) . . ? O4 Cl O3 110.77(9) . . ? O2 Cl O3 108.71(8) . . ? O4 Cl O1 109.67(8) . . ? O2 Cl O1 109.10(7) . . ? O3 Cl O1 108.24(7) . . ? O4 Cl Rb1 135.14(7) . . ? O2 Cl Rb1 55.26(5) . . ? O3 Cl Rb1 114.08(6) . . ? O1 Cl Rb1 54.86(5) . . ? O4 Cl Rb2 127.86(6) . . ? O2 Cl Rb2 121.79(5) . . ? O3 Cl Rb2 55.78(5) . . ? O1 Cl Rb2 52.50(5) . . ? Rb1 Cl Rb2 79.370(10) . . ? Cl O1 Rb1 102.07(6) . . ? Cl O1 Rb2 105.24(6) . . ? Rb1 O1 Rb2 100.75(3) . . ? Cl O2 Rb1 101.90(6) . . ? Cl O3 Rb2 101.83(6) . . ? C1 N C1 119.856(15) 2_665 . ? C1 N C1 119.860(15) 2_665 3_565 ? C1 N C1 119.856(15) . 3_565 ? C3 N1 C2 118.54(12) . . ? C3 N1 Fe 115.61(10) . . ? C2 N1 Fe 125.53(10) . . ? C4 N2 C5 106.60(12) . . ? C4 N2 Fe 112.70(9) . . ? C5 N2 Fe 140.54(10) . . ? C4 N3 C6 107.95(14) . . ? C4 N3 H3N 124.0(18) . . ? C6 N3 H3N 128.0(18) . . ? N C1 C2 114.97(14) . . ? N C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C1 111.56(13) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 113.38(13) . . ? N1 C3 H3A 123.3 . . ? C4 C3 H3A 123.3 . . ? N2 C4 N3 110.22(14) . . ? N2 C4 C3 116.98(12) . . ? N3 C4 C3 132.78(14) . . ? C6 C5 N2 108.61(14) . . ? C6 C5 H5A 125.7 . . ? N2 C5 H5A 125.7 . . ? N3 C6 C5 106.62(14) . . ? N3 C6 H6A 126.7 . . ? C5 C6 H6A 126.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Rb1 Cl O4 -0.59(8) 6_655 . . . ? O1 Rb1 Cl O4 -114.68(8) 2_765 . . . ? O1 Rb1 Cl O4 -82.88(10) . . . . ? O1 Rb1 Cl O4 97.12(10) 4_775 . . . ? O1 Rb1 Cl O4 65.32(8) 5_565 . . . ? O1 Rb1 Cl O4 179.41(8) 3_675 . . . ? O2 Rb1 Cl O4 1.64(8) 6_655 . . . ? O2 Rb1 Cl O4 -178.36(8) 3_675 . . . ? O2 Rb1 Cl O4 -69.06(8) 2_765 . . . ? O2 Rb1 Cl O4 84.35(10) . . . . ? O2 Rb1 Cl O4 -95.65(10) 4_775 . . . ? O2 Rb1 Cl O4 110.94(8) 5_565 . . . ? O1 Rb1 Cl O2 -84.94(7) 6_655 . . . ? O1 Rb1 Cl O2 160.97(7) 2_765 . . . ? O1 Rb1 Cl O2 -167.23(9) . . . . ? O1 Rb1 Cl O2 12.78(9) 4_775 . . . ? O1 Rb1 Cl O2 -19.03(7) 5_565 . . . ? O1 Rb1 Cl O2 95.06(7) 3_675 . . . ? O2 Rb1 Cl O2 -82.71(4) 6_655 . . . ? O2 Rb1 Cl O2 97.29(4) 3_675 . . . ? O2 Rb1 Cl O2 -153.41(6) 2_765 . . . ? O2 Rb1 Cl O2 180.0 4_775 . . . ? O2 Rb1 Cl O2 26.59(6) 5_565 . . . ? O1 Rb1 Cl O3 178.30(7) 6_655 . . . ? O1 Rb1 Cl O3 64.21(7) 2_765 . . . ? O1 Rb1 Cl O3 96.01(8) . . . . ? O1 Rb1 Cl O3 -83.99(8) 4_775 . . . ? O1 Rb1 Cl O3 -115.79(7) 5_565 . . . ? O1 Rb1 Cl O3 -1.70(7) 3_675 . . . ? O2 Rb1 Cl O3 -179.47(7) 6_655 . . . ? O2 Rb1 Cl O3 0.53(7) 3_675 . . . ? O2 Rb1 Cl O3 109.83(7) 2_765 . . . ? O2 Rb1 Cl O3 -96.76(9) . . . . ? O2 Rb1 Cl O3 83.24(9) 4_775 . . . ? O2 Rb1 Cl O3 -70.17(7) 5_565 . . . ? O1 Rb1 Cl O1 82.29(8) 6_655 . . . ? O1 Rb1 Cl O1 -31.80(6) 2_765 . . . ? O1 Rb1 Cl O1 180.0 4_775 . . . ? O1 Rb1 Cl O1 148.20(6) 5_565 . . . ? O1 Rb1 Cl O1 -97.71(8) 3_675 . . . ? O2 Rb1 Cl O1 84.52(6) 6_655 . . . ? O2 Rb1 Cl O1 -95.48(6) 3_675 . . . ? O2 Rb1 Cl O1 13.82(6) 2_765 . . . ? O2 Rb1 Cl O1 167.23(9) . . . . ? O2 Rb1 Cl O1 -12.77(9) 4_775 . . . ? O2 Rb1 Cl O1 -166.18(6) 5_565 . . . ? O1 Rb1 Cl Rb2 133.58(2) 6_655 . . . ? O1 Rb1 Cl Rb2 19.49(2) 2_765 . . . ? O1 Rb1 Cl Rb2 51.29(6) . . . . ? O1 Rb1 Cl Rb2 -128.71(6) 4_775 . . . ? O1 Rb1 Cl Rb2 -160.51(2) 5_565 . . . ? O1 Rb1 Cl Rb2 -46.42(2) 3_675 . . . ? O2 Rb1 Cl Rb2 135.81(3) 6_655 . . . ? O2 Rb1 Cl Rb2 -44.19(3) 3_675 . . . ? O2 Rb1 Cl Rb2 65.11(2) 2_765 . . . ? O2 Rb1 Cl Rb2 -141.49(6) . . . . ? O2 Rb1 Cl Rb2 38.51(6) 4_775 . . . ? O2 Rb1 Cl Rb2 -114.89(2) 5_565 . . . ? O1 Rb2 Cl O4 86.60(10) . . . . ? O1 Rb2 Cl O4 6.95(9) 6_656 . . . ? O1 Rb2 Cl O4 120.69(9) 2_765 . . . ? O1 Rb2 Cl O4 -93.40(10) 4_776 . . . ? O1 Rb2 Cl O4 -59.31(9) 5_566 . . . ? O1 Rb2 Cl O4 -173.05(9) 3_675 . . . ? O3 Rb2 Cl O4 75.85(9) 2_765 . . . ? O3 Rb2 Cl O4 -1.80(9) 6_656 . . . ? O3 Rb2 Cl O4 -90.84(11) . . . . ? O3 Rb2 Cl O4 89.16(11) 4_776 . . . ? O3 Rb2 Cl O4 178.20(9) 3_675 . . . ? O3 Rb2 Cl O4 -104.15(9) 5_566 . . . ? O1 Rb2 Cl O2 -90.55(8) . . . . ? O1 Rb2 Cl O2 -170.20(6) 6_656 . . . ? O1 Rb2 Cl O2 -56.46(6) 2_765 . . . ? O1 Rb2 Cl O2 89.45(8) 4_776 . . . ? O1 Rb2 Cl O2 123.54(6) 5_566 . . . ? O1 Rb2 Cl O2 9.80(6) 3_675 . . . ? O3 Rb2 Cl O2 -101.30(6) 2_765 . . . ? O3 Rb2 Cl O2 -178.96(7) 6_656 . . . ? O3 Rb2 Cl O2 92.01(9) . . . . ? O3 Rb2 Cl O2 -87.99(9) 4_776 . . . ? O3 Rb2 Cl O2 1.05(7) 3_675 . . . ? O3 Rb2 Cl O2 78.70(6) 5_566 . . . ? O1 Rb2 Cl O3 177.44(9) . . . . ? O1 Rb2 Cl O3 97.79(7) 6_656 . . . ? O1 Rb2 Cl O3 -148.47(7) 2_765 . . . ? O1 Rb2 Cl O3 -2.56(9) 4_776 . . . ? O1 Rb2 Cl O3 31.53(7) 5_566 . . . ? O1 Rb2 Cl O3 -82.21(7) 3_675 . . . ? O3 Rb2 Cl O3 166.69(7) 2_765 . . . ? O3 Rb2 Cl O3 89.04(4) 6_656 . . . ? O3 Rb2 Cl O3 180.0 4_776 . . . ? O3 Rb2 Cl O3 -90.96(4) 3_675 . . . ? O3 Rb2 Cl O3 -13.31(7) 5_566 . . . ? O1 Rb2 Cl O1 -79.65(8) 6_656 . . . ? O1 Rb2 Cl O1 34.09(6) 2_765 . . . ? O1 Rb2 Cl O1 180.0 4_776 . . . ? O1 Rb2 Cl O1 -145.91(6) 5_566 . . . ? O1 Rb2 Cl O1 100.35(8) 3_675 . . . ? O3 Rb2 Cl O1 -10.75(6) 2_765 . . . ? O3 Rb2 Cl O1 -88.40(7) 6_656 . . . ? O3 Rb2 Cl O1 -177.44(9) . . . . ? O3 Rb2 Cl O1 2.56(9) 4_776 . . . ? O3 Rb2 Cl O1 91.60(7) 3_675 . . . ? O3 Rb2 Cl O1 169.25(6) 5_566 . . . ? O1 Rb2 Cl Rb1 -53.54(6) . . . . ? O1 Rb2 Cl Rb1 -133.19(2) 6_656 . . . ? O1 Rb2 Cl Rb1 -19.45(2) 2_765 . . . ? O1 Rb2 Cl Rb1 126.46(6) 4_776 . . . ? O1 Rb2 Cl Rb1 160.55(2) 5_566 . . . ? O1 Rb2 Cl Rb1 46.81(2) 3_675 . . . ? O3 Rb2 Cl Rb1 -64.29(2) 2_765 . . . ? O3 Rb2 Cl Rb1 -141.94(3) 6_656 . . . ? O3 Rb2 Cl Rb1 129.02(7) . . . . ? O3 Rb2 Cl Rb1 -50.98(7) 4_776 . . . ? O3 Rb2 Cl Rb1 38.06(3) 3_675 . . . ? O3 Rb2 Cl Rb1 115.71(2) 5_566 . . . ? O4 Cl O1 Rb1 131.99(7) . . . . ? O2 Cl O1 Rb1 11.08(7) . . . . ? O3 Cl O1 Rb1 -107.06(7) . . . . ? Rb2 Cl O1 Rb1 -104.83(5) . . . . ? O4 Cl O1 Rb2 -123.19(7) . . . . ? O2 Cl O1 Rb2 115.91(6) . . . . ? O3 Cl O1 Rb2 -2.23(8) . . . . ? Rb1 Cl O1 Rb2 104.83(5) . . . . ? O1 Rb1 O1 Cl -108.58(7) 6_655 . . . ? O1 Rb1 O1 Cl 145.21(6) 2_765 . . . ? O1 Rb1 O1 Cl 83(3) 4_775 . . . ? O1 Rb1 O1 Cl -34.79(6) 5_565 . . . ? O1 Rb1 O1 Cl 71.42(7) 3_675 . . . ? O2 Rb1 O1 Cl -87.98(6) 6_655 . . . ? O2 Rb1 O1 Cl 92.02(6) 3_675 . . . ? O2 Rb1 O1 Cl -164.86(7) 2_765 . . . ? O2 Rb1 O1 Cl -6.90(5) . . . . ? O2 Rb1 O1 Cl 173.10(5) 4_775 . . . ? O2 Rb1 O1 Cl 15.14(7) 5_565 . . . ? O1 Rb1 O1 Rb2 143.109(9) 6_655 . . . ? O1 Rb1 O1 Rb2 36.891(9) 2_765 . . . ? O1 Rb1 O1 Rb2 -25(3) 4_775 . . . ? O1 Rb1 O1 Rb2 -143.108(9) 5_565 . . . ? O1 Rb1 O1 Rb2 -36.892(9) 3_675 . . . ? O2 Rb1 O1 Rb2 163.71(4) 6_655 . . . ? O2 Rb1 O1 Rb2 -16.29(4) 3_675 . . . ? O2 Rb1 O1 Rb2 86.82(3) 2_765 . . . ? O2 Rb1 O1 Rb2 -115.21(5) . . . . ? O2 Rb1 O1 Rb2 64.79(5) 4_775 . . . ? O2 Rb1 O1 Rb2 -93.18(3) 5_565 . . . ? O1 Rb2 O1 Cl 111.02(7) 6_656 . . . ? O1 Rb2 O1 Cl -142.62(6) 2_765 . . . ? O1 Rb2 O1 Cl -54(100) 4_776 . . . ? O1 Rb2 O1 Cl 37.38(6) 5_566 . . . ? O1 Rb2 O1 Cl -68.98(7) 3_675 . . . ? O3 Rb2 O1 Cl 167.72(7) 2_765 . . . ? O3 Rb2 O1 Cl 85.82(6) 6_656 . . . ? O3 Rb2 O1 Cl 1.39(5) . . . . ? O3 Rb2 O1 Cl -178.61(5) 4_776 . . . ? O3 Rb2 O1 Cl -94.18(6) 3_675 . . . ? O3 Rb2 O1 Cl -12.28(7) 5_566 . . . ? O1 Rb2 O1 Rb1 -143.181(9) 6_656 . . . ? O1 Rb2 O1 Rb1 -36.819(9) 2_765 . . . ? O1 Rb2 O1 Rb1 52(20) 4_776 . . . ? O1 Rb2 O1 Rb1 143.179(9) 5_566 . . . ? O1 Rb2 O1 Rb1 36.820(9) 3_675 . . . ? O3 Rb2 O1 Rb1 -86.48(4) 2_765 . . . ? O3 Rb2 O1 Rb1 -168.38(4) 6_656 . . . ? O3 Rb2 O1 Rb1 107.19(5) . . . . ? O3 Rb2 O1 Rb1 -72.81(5) 4_776 . . . ? O3 Rb2 O1 Rb1 11.62(4) 3_675 . . . ? O3 Rb2 O1 Rb1 93.52(4) 5_566 . . . ? O4 Cl O2 Rb1 -131.55(7) . . . . ? O3 Cl O2 Rb1 106.81(7) . . . . ? O1 Cl O2 Rb1 -11.03(7) . . . . ? Rb2 Cl O2 Rb1 46.06(6) . . . . ? O1 Rb1 O2 Cl 106.18(6) 6_655 . . . ? O1 Rb1 O2 Cl -20.03(7) 2_765 . . . ? O1 Rb1 O2 Cl 6.96(5) . . . . ? O1 Rb1 O2 Cl -173.03(5) 4_775 . . . ? O1 Rb1 O2 Cl 159.97(7) 5_565 . . . ? O1 Rb1 O2 Cl -73.82(6) 3_675 . . . ? O2 Rb1 O2 Cl 89.72(4) 6_655 . . . ? O2 Rb1 O2 Cl -90.28(4) 3_675 . . . ? O2 Rb1 O2 Cl 28.22(7) 2_765 . . . ? O2 Rb1 O2 Cl -140(6) 4_775 . . . ? O2 Rb1 O2 Cl -151.78(7) 5_565 . . . ? O4 Cl O3 Rb2 122.41(7) . . . . ? O2 Cl O3 Rb2 -116.25(6) . . . . ? O1 Cl O3 Rb2 2.14(8) . . . . ? Rb1 Cl O3 Rb2 -56.76(6) . . . . ? O1 Rb2 O3 Cl -1.38(5) . . . . ? O1 Rb2 O3 Cl -95.05(7) 6_656 . . . ? O1 Rb2 O3 Cl 32.50(7) 2_765 . . . ? O1 Rb2 O3 Cl 178.62(5) 4_776 . . . ? O1 Rb2 O3 Cl -147.50(7) 5_566 . . . ? O1 Rb2 O3 Cl 84.95(7) 3_675 . . . ? O3 Rb2 O3 Cl -13.58(7) 2_765 . . . ? O3 Rb2 O3 Cl -85.21(4) 6_656 . . . ? O3 Rb2 O3 Cl 138(4) 4_776 . . . ? O3 Rb2 O3 Cl 94.80(4) 3_675 . . . ? O3 Rb2 O3 Cl 166.42(7) 5_566 . . . ? N2 Fe N1 C3 15.7(4) 3_565 . . . ? N2 Fe N1 C3 -86.92(11) 2_665 . . . ? N2 Fe N1 C3 5.07(11) . . . . ? N1 Fe N1 C3 -167.82(11) 2_665 . . . ? N1 Fe N1 C3 93.51(13) 3_565 . . . ? N2 Fe N1 C2 -170.9(3) 3_565 . . . ? N2 Fe N1 C2 86.52(12) 2_665 . . . ? N2 Fe N1 C2 178.51(12) . . . . ? N1 Fe N1 C2 5.62(12) 2_665 . . . ? N1 Fe N1 C2 -93.05(9) 3_565 . . . ? N2 Fe N2 C4 177.25(10) 3_565 . . . ? N2 Fe N2 C4 85.27(12) 2_665 . . . ? N1 Fe N2 C4 74.8(4) 2_665 . . . ? N1 Fe N2 C4 -4.06(10) . . . . ? N1 Fe N2 C4 -101.73(10) 3_565 . . . ? N2 Fe N2 C5 2.68(16) 3_565 . . . ? N2 Fe N2 C5 -89.30(13) 2_665 . . . ? N1 Fe N2 C5 -99.8(4) 2_665 . . . ? N1 Fe N2 C5 -178.63(16) . . . . ? N1 Fe N2 C5 83.70(16) 3_565 . . . ? C1 N C1 C2 -73.6(2) 2_665 . . . ? C1 N C1 C2 113.9(2) 3_565 . . . ? C3 N1 C2 C1 -107.69(16) . . . . ? Fe N1 C2 C1 79.04(15) . . . . ? N C1 C2 N1 -54.64(18) . . . . ? C2 N1 C3 C4 -178.80(12) . . . . ? Fe N1 C3 C4 -4.88(16) . . . . ? C5 N2 C4 N3 0.39(17) . . . . ? Fe N2 C4 N3 -176.01(10) . . . . ? C5 N2 C4 C3 179.17(13) . . . . ? Fe N2 C4 C3 2.76(16) . . . . ? C6 N3 C4 N2 -0.30(19) . . . . ? C6 N3 C4 C3 -178.81(16) . . . . ? N1 C3 C4 N2 1.38(19) . . . . ? N1 C3 C4 N3 179.81(16) . . . . ? C4 N2 C5 C6 -0.34(17) . . . . ? Fe N2 C5 C6 174.44(12) . . . . ? C4 N3 C6 C5 0.08(19) . . . . ? N2 C5 C6 N3 0.16(19) . . . . ? 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 N3 H3N O1 0.76(2) 2.29(2) 2.959(2) 147(2) . N3 H3N O2 0.76(2) 2.61(2) 3.1236(19) 127(2) 2_765 C3 H3A O3 0.95 2.35 3.1267(19) 138.9 6_656 _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.356 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.055 #===END data_f29rb _database_code_depnum_ccdc_archive 'CCDC 631972' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl2 Mn N10 O8' _chemical_formula_weight 634.31 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) 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' _cell_length_a 9.7997(9) _cell_length_b 16.6091(16) _cell_length_c 16.0430(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2611.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6461 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 28.78 _exptl_crystal_description needle _exptl_crystal_colour clear _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.774 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6538 _exptl_absorpt_correction_T_max 0.9550 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21315 _diffrn_reflns_av_R_equivalents 0.0415 _diffrn_reflns_av_sigmaI/netI 0.0451 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 29.51 _reflns_number_total 5817 _reflns_number_gt 5101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0303P)^2^+0.3789P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.015(14) _refine_ls_number_reflns 5817 _refine_ls_number_parameters 390 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0737 _refine_ls_wR_factor_gt 0.0702 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.031 _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 Mn Mn 0.44493(3) 0.445649(17) 0.44733(5) 0.02416(8) Uani 1 1 d . . . Cl1 Cl 0.49344(6) 0.23220(3) 0.80359(5) 0.02644(11) Uani 1 1 d . . . Cl2 Cl 0.99780(7) 0.39135(4) 0.11646(4) 0.04161(16) Uani 1 1 d D . . O11 O 0.5426(2) 0.19047(11) 0.87580(13) 0.0438(5) Uani 1 1 d . . . O12 O 0.5480(2) 0.19520(11) 0.72977(13) 0.0368(4) Uani 1 1 d . . . O13 O 0.53702(18) 0.31552(9) 0.80577(14) 0.0348(4) Uani 1 1 d . . . O14 O 0.3476(2) 0.22858(12) 0.79995(16) 0.0480(5) Uani 1 1 d . . . O21A O 0.8598(2) 0.3673(3) 0.1221(3) 0.0638(18) Uani 0.607(9) 1 d PD A 1 O22A O 1.0830(4) 0.32649(19) 0.1400(4) 0.089(3) Uani 0.607(9) 1 d PD A 1 O23A O 1.0212(4) 0.4574(2) 0.1700(3) 0.0476(14) Uani 0.607(9) 1 d PD A 1 O24A O 1.0276(6) 0.4138(4) 0.03341(15) 0.131(4) Uani 0.607(9) 1 d PD A 1 O21B O 1.0623(8) 0.3761(4) 0.0393(3) 0.076(4) Uani 0.393(9) 1 d PD A 2 O22B O 1.0330(13) 0.3303(4) 0.1739(4) 0.164(8) Uani 0.393(9) 1 d PD A 2 O23B O 0.8546(2) 0.3920(7) 0.1051(6) 0.144(7) Uani 0.393(9) 1 d PD A 2 O24B O 1.0406(9) 0.4668(3) 0.1475(4) 0.113(6) Uani 0.393(9) 1 d PD A 2 N N 0.1897(2) 0.37710(11) 0.40984(15) 0.0316(5) Uani 1 1 d . . . N1A N 0.3504(2) 0.37822(11) 0.55573(14) 0.0300(5) Uani 1 1 d . . . N2A N 0.6212(2) 0.39234(11) 0.52526(15) 0.0276(4) Uani 1 1 d . . . N3A N 0.6794(2) 0.35042(12) 0.65067(16) 0.0357(5) Uani 1 1 d . . . H3AA H 0.6722 0.3312 0.7016 0.043 Uiso 1 1 calc R . . N1B N 0.2861(2) 0.53685(11) 0.41149(14) 0.0290(4) Uani 1 1 d . . . N2B N 0.4945(2) 0.56023(11) 0.52098(14) 0.0295(4) Uani 1 1 d . . . N3B N 0.4737(3) 0.69191(12) 0.51712(16) 0.0394(6) Uani 1 1 d . . . H3BA H 0.4402 0.7400 0.5064 0.047 Uiso 1 1 calc R . . N1C N 0.4500(2) 0.35603(11) 0.33852(15) 0.0296(4) Uani 1 1 d . . . N2C N 0.6063(2) 0.48978(11) 0.35604(15) 0.0286(4) Uani 1 1 d . . . N3C N 0.7277(2) 0.46382(13) 0.24396(16) 0.0390(5) Uani 1 1 d . . . H3CA H 0.7566 0.4397 0.1984 0.047 Uiso 1 1 calc R . . C1A C 0.1528(3) 0.32782(16) 0.48214(19) 0.0385(6) Uani 1 1 d . . . H1AA H 0.1935 0.2736 0.4761 0.046 Uiso 1 1 calc R . . H1AB H 0.0524 0.3216 0.4844 0.046 Uiso 1 1 calc R . . C2A C 0.2026(3) 0.36573(16) 0.5624(2) 0.0388(7) Uani 1 1 d . . . H2AA H 0.1560 0.4179 0.5717 0.047 Uiso 1 1 calc R . . H2AB H 0.1820 0.3299 0.6102 0.047 Uiso 1 1 calc R . . C3A C 0.4298(3) 0.35306(15) 0.61228(18) 0.0327(6) Uani 1 1 d . . . H3AB H 0.3964 0.3286 0.6617 0.039 Uiso 1 1 calc R . . C4A C 0.5760(3) 0.36384(14) 0.59722(17) 0.0279(5) Uani 1 1 d . . . C5A C 0.7589(3) 0.39790(14) 0.53408(19) 0.0342(6) Uani 1 1 d . . . H5AA H 0.8197 0.4170 0.4924 0.041 Uiso 1 1 calc R . . C6A C 0.7971(3) 0.37201(15) 0.6114(2) 0.0390(6) Uani 1 1 d . . . H6AA H 0.8871 0.3696 0.6333 0.047 Uiso 1 1 calc R . . C1B C 0.0948(3) 0.44530(15) 0.3981(2) 0.0376(6) Uani 1 1 d . . . H1BA H 0.0561 0.4613 0.4527 0.045 Uiso 1 1 calc R . . H1BB H 0.0186 0.4284 0.3616 0.045 Uiso 1 1 calc R . . C2B C 0.1684(3) 0.51718(15) 0.35901(19) 0.0366(6) Uani 1 1 d . . . H2BA H 0.1991 0.5035 0.3019 0.044 Uiso 1 1 calc R . . H2BB H 0.1060 0.5639 0.3556 0.044 Uiso 1 1 calc R . . C3B C 0.3027(3) 0.60802(12) 0.43908(18) 0.0318(5) Uani 1 1 d . . . H3BB H 0.2413 0.6503 0.4256 0.038 Uiso 1 1 calc R . . C4B C 0.4204(3) 0.62123(13) 0.49212(17) 0.0302(6) Uani 1 1 d . . . C5B C 0.6001(3) 0.59388(15) 0.56416(19) 0.0364(6) Uani 1 1 d . . . H5BA H 0.6708 0.5650 0.5915 0.044 Uiso 1 1 calc R . . C6B C 0.5880(3) 0.67595(16) 0.56174(19) 0.0421(7) Uani 1 1 d . . . H6BA H 0.6478 0.7141 0.5864 0.051 Uiso 1 1 calc R . . C1C C 0.2071(3) 0.32953(15) 0.33339(19) 0.0390(7) Uani 1 1 d . . . H1CA H 0.1940 0.3648 0.2843 0.047 Uiso 1 1 calc R . . H1CB H 0.1368 0.2867 0.3314 0.047 Uiso 1 1 calc R . . C2C C 0.3488(3) 0.29119(14) 0.3295(2) 0.0384(6) Uani 1 1 d . . . H2CA H 0.3596 0.2514 0.3750 0.046 Uiso 1 1 calc R . . H2CB H 0.3615 0.2632 0.2756 0.046 Uiso 1 1 calc R . . C3C C 0.5352(3) 0.36994(15) 0.28103(17) 0.0307(6) Uani 1 1 d . . . H3CB H 0.5415 0.3367 0.2330 0.037 Uiso 1 1 calc R . . C4C C 0.6234(3) 0.43977(13) 0.29256(16) 0.0295(5) Uani 1 1 d . . . C5C C 0.7054(3) 0.54757(14) 0.34716(18) 0.0348(6) Uani 1 1 d . . . H5CA H 0.7193 0.5917 0.3839 0.042 Uiso 1 1 calc R . . C6C C 0.7803(3) 0.53221(15) 0.27806(19) 0.0389(6) Uani 1 1 d . . . H6CA H 0.8548 0.5630 0.2575 0.047 Uiso 1 1 calc R . . 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 Mn 0.02309(17) 0.02281(13) 0.02659(17) 0.00483(14) 0.00159(17) 0.00107(12) Cl1 0.0266(3) 0.0255(2) 0.0272(3) 0.0018(2) 0.0005(2) -0.0013(2) Cl2 0.0380(4) 0.0510(4) 0.0358(4) -0.0131(3) 0.0018(3) 0.0020(3) O11 0.0646(15) 0.0340(9) 0.0327(11) 0.0050(8) -0.0087(10) 0.0038(9) O12 0.0419(12) 0.0347(9) 0.0338(11) -0.0069(8) 0.0033(8) 0.0027(8) O13 0.0410(11) 0.0234(7) 0.0399(10) -0.0013(7) 0.0021(9) -0.0044(6) O14 0.0245(10) 0.0565(11) 0.0630(15) 0.0049(10) 0.0070(11) -0.0064(8) O21A 0.041(3) 0.052(2) 0.098(5) -0.047(2) 0.018(3) -0.0142(17) O22A 0.076(4) 0.062(3) 0.130(7) -0.037(3) -0.052(4) 0.021(2) O23A 0.041(2) 0.044(2) 0.058(3) -0.0182(19) 0.020(2) -0.0130(17) O24A 0.076(4) 0.281(11) 0.035(3) 0.002(4) 0.013(3) 0.024(6) O21B 0.093(7) 0.054(4) 0.081(6) -0.045(4) 0.057(5) -0.019(4) O22B 0.36(2) 0.077(7) 0.057(7) 0.024(5) -0.105(10) -0.030(9) O23B 0.036(6) 0.304(19) 0.092(8) -0.101(10) -0.022(5) 0.040(7) O24B 0.175(11) 0.070(5) 0.093(8) -0.044(5) 0.091(8) -0.082(6) N 0.0242(12) 0.0283(9) 0.0424(13) 0.0083(8) -0.0036(10) -0.0021(8) N1A 0.0235(11) 0.0333(10) 0.0331(12) 0.0100(8) 0.0011(9) 0.0002(8) N2A 0.0224(11) 0.0284(9) 0.0319(11) 0.0061(8) 0.0023(9) 0.0021(8) N3A 0.0321(13) 0.0383(10) 0.0369(13) 0.0124(9) -0.0074(10) -0.0042(9) N1B 0.0252(12) 0.0281(9) 0.0338(11) 0.0085(8) 0.0000(9) -0.0003(8) N2B 0.0318(12) 0.0264(9) 0.0303(12) 0.0004(8) -0.0011(9) 0.0032(8) N3B 0.0508(16) 0.0264(10) 0.0411(14) -0.0016(9) -0.0065(11) 0.0032(9) N1C 0.0274(12) 0.0260(9) 0.0354(12) 0.0014(8) -0.0017(10) -0.0018(8) N2C 0.0259(12) 0.0279(9) 0.0320(12) 0.0026(8) 0.0041(9) -0.0021(8) N3C 0.0368(14) 0.0436(12) 0.0365(13) 0.0016(9) 0.0152(11) -0.0008(10) C1A 0.0227(13) 0.0391(13) 0.0536(18) 0.0187(12) 0.0006(12) -0.0050(10) C2A 0.0213(14) 0.0500(15) 0.0449(17) 0.0196(13) 0.0064(12) 0.0008(11) C3A 0.0270(15) 0.0384(13) 0.0327(15) 0.0149(11) 0.0039(11) 0.0009(10) C4A 0.0242(14) 0.0287(11) 0.0306(14) 0.0083(9) -0.0030(10) -0.0004(9) C5A 0.0230(14) 0.0354(12) 0.0440(16) 0.0109(11) 0.0014(12) -0.0039(10) C6A 0.0238(14) 0.0425(14) 0.0508(18) 0.0128(12) -0.0076(13) -0.0029(10) C1B 0.0240(15) 0.0383(13) 0.0507(18) 0.0101(12) -0.0092(12) 0.0021(10) C2B 0.0331(16) 0.0324(12) 0.0443(17) 0.0128(11) -0.0083(13) 0.0024(10) C3B 0.0345(14) 0.0295(10) 0.0313(14) 0.0063(10) 0.0026(12) 0.0082(9) C4B 0.0389(16) 0.0262(11) 0.0255(13) 0.0018(9) 0.0055(11) 0.0031(9) C5B 0.0377(16) 0.0355(12) 0.0361(15) -0.0016(11) -0.0045(12) 0.0019(11) C6B 0.0509(19) 0.0375(13) 0.0380(16) -0.0068(11) -0.0072(14) -0.0041(12) C1C 0.0354(16) 0.0367(13) 0.0449(17) 0.0021(11) -0.0119(13) -0.0106(11) C2C 0.0384(17) 0.0278(11) 0.0491(18) -0.0032(10) -0.0017(13) -0.0062(10) C3C 0.0332(15) 0.0294(11) 0.0294(15) -0.0028(9) -0.0010(11) 0.0061(9) C4C 0.0280(13) 0.0316(11) 0.0291(14) 0.0049(9) 0.0037(11) 0.0037(9) C5C 0.0314(15) 0.0293(11) 0.0436(17) 0.0063(10) 0.0042(12) -0.0034(10) C6C 0.0343(16) 0.0387(13) 0.0437(17) 0.0079(11) 0.0066(13) -0.0042(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 Mn N1B 2.247(2) . ? Mn N1A 2.267(2) . ? Mn N2C 2.277(2) . ? Mn N2B 2.292(2) . ? Mn N1C 2.295(2) . ? Mn N2A 2.309(2) . ? Cl1 O14 1.432(2) . ? Cl1 O11 1.433(2) . ? Cl1 O12 1.437(2) . ? Cl1 O13 1.4486(16) . ? Cl2 O23A 1.4126(17) . ? Cl2 O24B 1.4127(18) . ? Cl2 O21B 1.4134(18) . ? Cl2 O21A 1.4135(18) . ? Cl2 O22B 1.4136(18) . ? Cl2 O24A 1.4141(18) . ? Cl2 O22A 1.4146(18) . ? Cl2 O23B 1.4148(18) . ? N C1A 1.465(3) . ? N C1C 1.469(4) . ? N C1B 1.478(3) . ? N1A C3A 1.266(3) . ? N1A C2A 1.467(3) . ? N2A C4A 1.324(3) . ? N2A C5A 1.360(3) . ? N3A C4A 1.346(3) . ? N3A C6A 1.362(4) . ? N1B C3B 1.273(3) . ? N1B C2B 1.465(4) . ? N2B C4B 1.329(3) . ? N2B C5B 1.366(4) . ? N3B C4B 1.346(3) . ? N3B C6B 1.355(4) . ? N1C C3C 1.266(3) . ? N1C C2C 1.471(3) . ? N2C C4C 1.325(3) . ? N2C C5C 1.372(3) . ? N3C C4C 1.346(3) . ? N3C C6C 1.362(3) . ? C1A C2A 1.514(4) . ? C3A C4A 1.464(4) . ? C5A C6A 1.365(4) . ? C1B C2B 1.529(4) . ? C3B C4B 1.450(4) . ? C5B C6B 1.369(4) . ? C1C C2C 1.529(4) . ? C3C C4C 1.458(3) . ? C5C C6C 1.354(4) . ? 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 N1B Mn N1A 104.27(8) . . ? N1B Mn N2C 95.71(8) . . ? N1A Mn N2C 159.48(8) . . ? N1B Mn N2B 73.66(8) . . ? N1A Mn N2B 95.81(8) . . ? N2C Mn N2B 85.25(8) . . ? N1B Mn N1C 104.93(8) . . ? N1A Mn N1C 105.78(7) . . ? N2C Mn N1C 72.82(7) . . ? N2B Mn N1C 157.86(8) . . ? N1B Mn N2A 156.26(8) . . ? N1A Mn N2A 72.58(7) . . ? N2C Mn N2A 87.26(8) . . ? N2B Mn N2A 83.16(7) . . ? N1C Mn N2A 98.46(7) . . ? O14 Cl1 O11 110.36(14) . . ? O14 Cl1 O12 108.64(13) . . ? O11 Cl1 O12 109.53(11) . . ? O14 Cl1 O13 109.59(11) . . ? O11 Cl1 O13 110.09(12) . . ? O12 Cl1 O13 108.59(11) . . ? O23A Cl2 O24B 17.8(4) . . ? O23A Cl2 O21B 126.8(4) . . ? O24B Cl2 O21B 109.59(9) . . ? O23A Cl2 O21A 109.66(8) . . ? O24B Cl2 O21A 120.8(4) . . ? O21B Cl2 O21A 115.7(4) . . ? O23A Cl2 O22B 97.0(4) . . ? O24B Cl2 O22B 109.54(9) . . ? O21B Cl2 O22B 109.48(9) . . ? O21A Cl2 O22B 89.4(6) . . ? O23A Cl2 O24A 109.53(9) . . ? O24B Cl2 O24A 92.1(4) . . ? O21B Cl2 O24A 29.5(3) . . ? O21A Cl2 O24A 109.45(9) . . ? O22B Cl2 O24A 138.9(4) . . ? O23A Cl2 O22A 109.46(8) . . ? O24B Cl2 O22A 114.0(5) . . ? O21B Cl2 O22A 80.4(4) . . ? O21A Cl2 O22A 109.40(9) . . ? O22B Cl2 O22A 30.1(4) . . ? O24A Cl2 O22A 109.33(9) . . ? O23A Cl2 O23B 103.5(5) . . ? O24B Cl2 O23B 109.48(9) . . ? O21B Cl2 O23B 109.36(9) . . ? O21A Cl2 O23B 20.2(6) . . ? O22B Cl2 O23B 109.37(9) . . ? O24A Cl2 O23B 94.7(5) . . ? O22A Cl2 O23B 128.7(6) . . ? C1A N C1C 112.9(2) . . ? C1A N C1B 112.0(2) . . ? C1C N C1B 112.3(2) . . ? C3A N1A C2A 120.5(2) . . ? C3A N1A Mn 117.50(17) . . ? C2A N1A Mn 121.97(16) . . ? C4A N2A C5A 105.4(2) . . ? C4A N2A Mn 111.06(16) . . ? C5A N2A Mn 140.58(17) . . ? C4A N3A C6A 107.4(2) . . ? C3B N1B C2B 120.5(2) . . ? C3B N1B Mn 116.65(18) . . ? C2B N1B Mn 122.84(15) . . ? C4B N2B C5B 106.2(2) . . ? C4B N2B Mn 109.73(17) . . ? C5B N2B Mn 139.63(17) . . ? C4B N3B C6B 107.9(2) . . ? C3C N1C C2C 120.5(2) . . ? C3C N1C Mn 116.75(17) . . ? C2C N1C Mn 122.35(17) . . ? C4C N2C C5C 105.6(2) . . ? C4C N2C Mn 112.35(15) . . ? C5C N2C Mn 141.56(18) . . ? C4C N3C C6C 107.6(2) . . ? N C1A C2A 111.2(2) . . ? N1A C2A C1A 108.3(2) . . ? N1A C3A C4A 116.3(2) . . ? N2A C4A N3A 111.3(2) . . ? N2A C4A C3A 121.0(2) . . ? N3A C4A C3A 127.7(2) . . ? N2A C5A C6A 110.2(2) . . ? N3A C6A C5A 105.7(2) . . ? N C1B C2B 110.7(2) . . ? N1B C2B C1B 108.0(2) . . ? N1B C3B C4B 116.5(2) . . ? N2B C4B N3B 110.4(2) . . ? N2B C4B C3B 121.6(2) . . ? N3B C4B C3B 128.0(2) . . ? N2B C5B C6B 109.1(2) . . ? N3B C6B C5B 106.4(2) . . ? N C1C C2C 111.3(2) . . ? N1C C2C C1C 107.65(19) . . ? N1C C3C C4C 116.4(2) . . ? N2C C4C N3C 110.8(2) . . ? N2C C4C C3C 121.4(2) . . ? N3C C4C C3C 127.8(2) . . ? C6C C5C N2C 109.7(2) . . ? C5C C6C N3C 106.3(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1B Mn N1A C3A -146.6(2) . . . . ? N2C Mn N1A C3A 19.9(3) . . . . ? N2B Mn N1A C3A -72.0(2) . . . . ? N1C Mn N1A C3A 103.0(2) . . . . ? N2A Mn N1A C3A 8.91(19) . . . . ? N1B Mn N1A C2A 31.6(2) . . . . ? N2C Mn N1A C2A -161.9(2) . . . . ? N2B Mn N1A C2A 106.2(2) . . . . ? N1C Mn N1A C2A -78.8(2) . . . . ? N2A Mn N1A C2A -172.9(2) . . . . ? N1B Mn N2A C4A 75.1(2) . . . . ? N1A Mn N2A C4A -10.73(16) . . . . ? N2C Mn N2A C4A 173.12(17) . . . . ? N2B Mn N2A C4A 87.58(17) . . . . ? N1C Mn N2A C4A -114.70(17) . . . . ? N1B Mn N2A C5A -81.2(4) . . . . ? N1A Mn N2A C5A -167.1(3) . . . . ? N2C Mn N2A C5A 16.7(3) . . . . ? N2B Mn N2A C5A -68.8(3) . . . . ? N1C Mn N2A C5A 88.9(3) . . . . ? N1A Mn N1B C3B 98.9(2) . . . . ? N2C Mn N1B C3B -76.4(2) . . . . ? N2B Mn N1B C3B 6.92(19) . . . . ? N1C Mn N1B C3B -150.12(19) . . . . ? N2A Mn N1B C3B 19.8(3) . . . . ? N1A Mn N1B C2B -81.2(2) . . . . ? N2C Mn N1B C2B 103.5(2) . . . . ? N2B Mn N1B C2B -173.2(2) . . . . ? N1C Mn N1B C2B 29.8(2) . . . . ? N2A Mn N1B C2B -160.3(2) . . . . ? N1B Mn N2B C4B -11.18(17) . . . . ? N1A Mn N2B C4B -114.38(18) . . . . ? N2C Mn N2B C4B 86.20(18) . . . . ? N1C Mn N2B C4B 78.4(3) . . . . ? N2A Mn N2B C4B 174.00(18) . . . . ? N1B Mn N2B C5B -162.7(3) . . . . ? N1A Mn N2B C5B 94.1(3) . . . . ? N2C Mn N2B C5B -65.4(3) . . . . ? N1C Mn N2B C5B -73.2(4) . . . . ? N2A Mn N2B C5B 22.4(3) . . . . ? N1B Mn N1C C3C 92.12(19) . . . . ? N1A Mn N1C C3C -157.98(18) . . . . ? N2C Mn N1C C3C 0.66(18) . . . . ? N2B Mn N1C C3C 8.8(3) . . . . ? N2A Mn N1C C3C -83.79(19) . . . . ? N1B Mn N1C C2C -80.41(19) . . . . ? N1A Mn N1C C2C 29.5(2) . . . . ? N2C Mn N1C C2C -171.9(2) . . . . ? N2B Mn N1C C2C -163.7(2) . . . . ? N2A Mn N1C C2C 103.68(19) . . . . ? N1B Mn N2C C4C -107.42(17) . . . . ? N1A Mn N2C C4C 85.7(3) . . . . ? N2B Mn N2C C4C 179.55(17) . . . . ? N1C Mn N2C C4C -3.54(16) . . . . ? N2A Mn N2C C4C 96.19(17) . . . . ? N1B Mn N2C C5C 82.0(3) . . . . ? N1A Mn N2C C5C -84.9(3) . . . . ? N2B Mn N2C C5C 9.0(3) . . . . ? N1C Mn N2C C5C -174.1(3) . . . . ? N2A Mn N2C C5C -74.4(3) . . . . ? C1C N C1A C2A 151.6(2) . . . . ? C1B N C1A C2A -80.5(3) . . . . ? C3A N1A C2A C1A -128.6(3) . . . . ? Mn N1A C2A C1A 53.2(3) . . . . ? N C1A C2A N1A -56.0(3) . . . . ? C2A N1A C3A C4A 176.2(2) . . . . ? Mn N1A C3A C4A -5.6(3) . . . . ? C5A N2A C4A N3A -0.6(3) . . . . ? Mn N2A C4A N3A -165.34(16) . . . . ? C5A N2A C4A C3A 177.3(2) . . . . ? Mn N2A C4A C3A 12.6(3) . . . . ? C6A N3A C4A N2A 0.5(3) . . . . ? C6A N3A C4A C3A -177.2(3) . . . . ? N1A C3A C4A N2A -5.3(4) . . . . ? N1A C3A C4A N3A 172.2(2) . . . . ? C4A N2A C5A C6A 0.5(3) . . . . ? Mn N2A C5A C6A 157.7(2) . . . . ? C4A N3A C6A C5A -0.2(3) . . . . ? N2A C5A C6A N3A -0.2(3) . . . . ? C1A N C1B C2B 149.2(2) . . . . ? C1C N C1B C2B -82.6(3) . . . . ? C3B N1B C2B C1B -126.4(3) . . . . ? Mn N1B C2B C1B 53.7(3) . . . . ? N C1B C2B N1B -55.2(3) . . . . ? C2B N1B C3B C4B 178.6(2) . . . . ? Mn N1B C3B C4B -1.5(3) . . . . ? C5B N2B C4B N3B -1.4(3) . . . . ? Mn N2B C4B N3B -162.68(18) . . . . ? C5B N2B C4B C3B 176.7(2) . . . . ? Mn N2B C4B C3B 15.4(3) . . . . ? C6B N3B C4B N2B 1.7(3) . . . . ? C6B N3B C4B C3B -176.3(3) . . . . ? N1B C3B C4B N2B -10.2(4) . . . . ? N1B C3B C4B N3B 167.5(3) . . . . ? C4B N2B C5B C6B 0.7(3) . . . . ? Mn N2B C5B C6B 152.8(2) . . . . ? C4B N3B C6B C5B -1.2(3) . . . . ? N2B C5B C6B N3B 0.3(3) . . . . ? C1A N C1C C2C -82.1(3) . . . . ? C1B N C1C C2C 150.2(2) . . . . ? C3C N1C C2C C1C -119.1(3) . . . . ? Mn N1C C2C C1C 53.2(3) . . . . ? N C1C C2C N1C -55.1(3) . . . . ? C2C N1C C3C C4C 174.8(2) . . . . ? Mn N1C C3C C4C 2.2(3) . . . . ? C5C N2C C4C N3C -0.5(3) . . . . ? Mn N2C C4C N3C -174.43(17) . . . . ? C5C N2C C4C C3C -179.8(2) . . . . ? Mn N2C C4C C3C 6.2(3) . . . . ? C6C N3C C4C N2C 0.3(3) . . . . ? C6C N3C C4C C3C 179.6(2) . . . . ? N1C C3C C4C N2C -5.9(4) . . . . ? N1C C3C C4C N3C 174.9(2) . . . . ? C4C N2C C5C C6C 0.5(3) . . . . ? Mn N2C C5C C6C 171.5(2) . . . . ? N2C C5C C6C N3C -0.4(3) . . . . ? C4C N3C C6C C5C 0.1(3) . . . . ? 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 N3A H3AA O13 0.88 2.15 2.911(3) 144.6 . N3A H3AA O14 0.88 2.54 3.190(3) 131.8 3 N3A H3AA O12 0.88 2.61 3.149(3) 120.8 . N3B H3BA O21B 0.88 2.32 3.100(7) 147.5 4_655 N3B H3BA O11 0.88 2.40 2.997(3) 125.6 2_664 N3B H3BA O22A 0.88 2.59 3.032(5) 112.0 4_655 N3C H3CA O23B 0.88 1.95 2.817(8) 169.2 . N3C H3CA O21A 0.88 1.99 2.841(4) 161.5 . N3C H3CA O23A 0.88 2.65 3.113(5) 114.1 . C3B H3BB O14 0.95 2.55 3.341(3) 140.6 4_554 _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.259 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.049 #===END #===END data_ctbe48nh4m _database_code_depnum_ccdc_archive 'CCDC 635041' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Cl3 Fe N11 O12' _chemical_formula_weight 752.71 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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.5873(4) _cell_length_b 13.5873(4) _cell_length_c 9.3764(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1499.11(11) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 30.58 _exptl_crystal_description hexagonal _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.848 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7067 _exptl_absorpt_correction_T_max 0.9200 _exptl_absorpt_process_details Sadabs _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17231 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0093 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 30.64 _reflns_number_total 2929 _reflns_number_gt 2696 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0592P)^2^+0.4344P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2929 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Fe Fe 1.3333 0.6667 1.13841(3) 0.02756(10) Uani 1 3 d S . . Cl Cl 0.92608(3) 0.16307(3) 1.25572(4) 0.04692(12) Uani 1 1 d . . . O1 O 0.95312(17) 0.27832(14) 1.2474(2) 0.0892(6) Uani 1 1 d . . . O2 O 0.86689(14) 0.11242(14) 1.38543(17) 0.0690(4) Uani 1 1 d . . . O3 O 0.85484(16) 0.09534(18) 1.13967(18) 0.0819(5) Uani 1 1 d . . . O4 O 1.02903(11) 0.15640(12) 1.25098(16) 0.0586(3) Uani 1 1 d . . . N1A N 1.0000 0.0000 1.0000 0.0467(7) Uani 1 6 d S . . N2A N 1.0000 0.0000 1.5000 0.0430(6) Uani 1 6 d S . . N N 1.3333 0.6667 0.7792(3) 0.0533(6) Uani 1 3 d S . . N1 N 1.21600(10) 0.53289(10) 1.03395(12) 0.0373(2) Uani 1 1 d . . . N2 N 1.33254(10) 0.54618(10) 1.25446(12) 0.0350(2) Uani 1 1 d . . . N3 N 1.25334(16) 0.36415(13) 1.30107(19) 0.0608(4) Uani 1 1 d . . . H3B H 1.2092 0.2918 1.2944 0.073 Uiso 1 1 calc R . . C1 C 1.22465(17) 0.56441(18) 0.77249(17) 0.0567(4) Uani 1 1 d . . . H1A H 1.2367 0.5014 0.7509 0.068 Uiso 1 1 calc R . . H1B H 1.1817 0.5712 0.6943 0.068 Uiso 1 1 calc R . . C2 C 1.15313(14) 0.53614(16) 0.90873(17) 0.0502(4) Uani 1 1 d . . . H2A H 1.1307 0.5929 0.9233 0.060 Uiso 1 1 calc R . . H2B H 1.0846 0.4629 0.8976 0.060 Uiso 1 1 calc R . . C3 C 1.18766(14) 0.43560(13) 1.09010(17) 0.0462(3) Uani 1 1 d . . . H3A H 1.1298 0.3671 1.0543 0.055 Uiso 1 1 calc R . . C4 C 1.25404(14) 0.44309(12) 1.21317(17) 0.0427(3) Uani 1 1 d . . . C5 C 1.38350(15) 0.53230(15) 1.37261(18) 0.0491(4) Uani 1 1 d . . . H5A H 1.4420 0.5904 1.4247 0.059 Uiso 1 1 calc R . . C6 C 1.3339(2) 0.41844(18) 1.4012(2) 0.0643(5) Uani 1 1 d . . . H6A H 1.3522 0.3851 1.4754 0.077 Uiso 1 1 calc R . . 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 Fe 0.02760(12) 0.02760(12) 0.02748(16) 0.000 0.000 0.01380(6) Cl 0.0475(2) 0.0504(2) 0.0490(2) 0.00361(15) 0.00089(14) 0.02908(17) O1 0.0934(12) 0.0575(9) 0.1303(17) 0.0282(10) 0.0399(12) 0.0480(9) O2 0.0692(9) 0.0733(9) 0.0638(8) 0.0126(7) 0.0179(7) 0.0353(8) O3 0.0810(11) 0.1100(14) 0.0668(9) -0.0119(9) -0.0290(8) 0.0567(10) O4 0.0457(6) 0.0613(8) 0.0733(9) -0.0023(6) -0.0020(6) 0.0300(6) N1A 0.0524(11) 0.0524(11) 0.0354(14) 0.000 0.000 0.0262(5) N2A 0.0468(10) 0.0468(10) 0.0353(14) 0.000 0.000 0.0234(5) N 0.0585(9) 0.0585(9) 0.0427(12) 0.000 0.000 0.0293(4) N1 0.0360(5) 0.0378(6) 0.0325(5) -0.0046(4) -0.0016(4) 0.0143(5) N2 0.0379(5) 0.0335(5) 0.0351(5) 0.0035(4) 0.0023(4) 0.0189(4) N3 0.0743(10) 0.0358(7) 0.0668(10) 0.0155(6) 0.0077(8) 0.0235(7) C1 0.0644(11) 0.0657(11) 0.0337(7) -0.0098(7) -0.0101(7) 0.0276(9) C2 0.0433(8) 0.0565(9) 0.0409(7) -0.0086(6) -0.0118(6) 0.0176(7) C3 0.0472(8) 0.0332(6) 0.0441(7) -0.0060(5) 0.0012(6) 0.0094(6) C4 0.0502(8) 0.0311(6) 0.0437(7) 0.0039(5) 0.0069(6) 0.0180(6) C5 0.0514(9) 0.0522(9) 0.0455(8) 0.0117(6) -0.0020(6) 0.0272(7) C6 0.0737(12) 0.0601(11) 0.0641(11) 0.0263(9) 0.0038(9) 0.0371(10) _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 Fe N2 1.9611(11) 3_775 ? Fe N2 1.9612(11) . ? Fe N2 1.9612(11) 2_755 ? Fe N1 1.9766(12) 2_755 ? Fe N1 1.9766(12) 3_775 ? Fe N1 1.9766(12) . ? Cl O1 1.4206(16) . ? Cl O2 1.4305(15) . ? Cl O3 1.4412(17) . ? Cl O4 1.4469(13) . ? N C1 1.436(2) 3_775 ? N C1 1.436(2) . ? N C1 1.437(2) 2_755 ? N1 C3 1.290(2) . ? N1 C2 1.466(2) . ? N2 C4 1.3249(19) . ? N2 C5 1.3686(19) . ? N3 C6 1.348(3) . ? N3 C4 1.349(2) . ? N3 H3B 0.8600 . ? C1 C2 1.533(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.437(2) . ? C3 H3A 0.9300 . ? C5 C6 1.370(3) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? 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 N2 Fe N2 92.19(5) 3_775 . ? N2 Fe N2 92.20(5) 3_775 2_755 ? N2 Fe N2 92.19(5) . 2_755 ? N2 Fe N1 172.97(5) 3_775 2_755 ? N2 Fe N1 89.44(5) . 2_755 ? N2 Fe N1 80.91(5) 2_755 2_755 ? N2 Fe N1 80.91(5) 3_775 3_775 ? N2 Fe N1 172.98(5) . 3_775 ? N2 Fe N1 89.44(5) 2_755 3_775 ? N1 Fe N1 97.57(5) 2_755 3_775 ? N2 Fe N1 89.44(5) 3_775 . ? N2 Fe N1 80.91(5) . . ? N2 Fe N1 172.97(5) 2_755 . ? N1 Fe N1 97.57(5) 2_755 . ? N1 Fe N1 97.57(5) 3_775 . ? O1 Cl O2 110.49(11) . . ? O1 Cl O3 112.55(13) . . ? O2 Cl O3 107.35(12) . . ? O1 Cl O4 110.01(10) . . ? O2 Cl O4 108.94(9) . . ? O3 Cl O4 107.37(10) . . ? C1 N C1 119.812(19) 3_775 . ? C1 N C1 119.81(2) 3_775 2_755 ? C1 N C1 119.808(19) . 2_755 ? C3 N1 C2 118.55(13) . . ? C3 N1 Fe 115.49(10) . . ? C2 N1 Fe 125.70(11) . . ? C4 N2 C5 106.62(13) . . ? C4 N2 Fe 112.70(10) . . ? C5 N2 Fe 140.55(11) . . ? C6 N3 C4 108.03(15) . . ? C6 N3 H3B 126.0 . . ? C4 N3 H3B 126.0 . . ? N C1 C2 114.97(16) . . ? N C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C1 111.66(14) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N1 C3 C4 113.58(13) . . ? N1 C3 H3A 123.2 . . ? C4 C3 H3A 123.2 . . ? N2 C4 N3 110.12(15) . . ? N2 C4 C3 117.04(13) . . ? N3 C4 C3 132.84(15) . . ? N2 C5 C6 108.48(17) . . ? N2 C5 H5A 125.8 . . ? C6 C5 H5A 125.8 . . ? N3 C6 C5 106.74(16) . . ? N3 C6 H6A 126.6 . . ? C5 C6 H6A 126.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe N1 C3 -87.46(12) 3_775 . . . ? N2 Fe N1 C3 4.85(12) . . . . ? N2 Fe N1 C3 16.1(5) 2_755 . . . ? N1 Fe N1 C3 93.06(14) 2_755 . . . ? N1 Fe N1 C3 -168.21(12) 3_775 . . . ? N2 Fe N1 C2 86.66(13) 3_775 . . . ? N2 Fe N1 C2 178.97(13) . . . . ? N2 Fe N1 C2 -169.8(4) 2_755 . . . ? N1 Fe N1 C2 -92.82(10) 2_755 . . . ? N1 Fe N1 C2 5.90(13) 3_775 . . . ? N2 Fe N2 C4 85.13(13) 3_775 . . . ? N2 Fe N2 C4 177.41(10) 2_755 . . . ? N1 Fe N2 C4 -101.71(11) 2_755 . . . ? N1 Fe N2 C4 74.1(4) 3_775 . . . ? N1 Fe N2 C4 -3.95(10) . . . . ? N2 Fe N2 C5 -90.01(15) 3_775 . . . ? N2 Fe N2 C5 2.27(17) 2_755 . . . ? N1 Fe N2 C5 83.15(17) 2_755 . . . ? N1 Fe N2 C5 -101.1(4) 3_775 . . . ? N1 Fe N2 C5 -179.09(18) . . . . ? C1 N C1 C2 -74.5(3) 3_775 . . . ? C1 N C1 C2 114.2(2) 2_755 . . . ? C3 N1 C2 C1 -107.64(18) . . . . ? Fe N1 C2 C1 78.41(18) . . . . ? N C1 C2 N1 -54.1(2) . . . . ? C2 N1 C3 C4 -179.20(14) . . . . ? Fe N1 C3 C4 -4.64(18) . . . . ? C5 N2 C4 N3 0.02(19) . . . . ? Fe N2 C4 N3 -176.76(12) . . . . ? C5 N2 C4 C3 179.53(14) . . . . ? Fe N2 C4 C3 2.75(18) . . . . ? C6 N3 C4 N2 -0.1(2) . . . . ? C6 N3 C4 C3 -179.51(19) . . . . ? N1 C3 C4 N2 1.2(2) . . . . ? N1 C3 C4 N3 -179.40(18) . . . . ? C4 N2 C5 C6 0.1(2) . . . . ? Fe N2 C5 C6 175.40(14) . . . . ? C4 N3 C6 C5 0.1(2) . . . . ? N2 C5 C6 N3 -0.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.513 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.054 #===END data_gregcs _database_code_depnum_ccdc_archive 'CCDC 635168' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H24 Cl3 Cs Fe N10 O12' _chemical_formula_weight 867.58 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' Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.5022(13) _cell_length_b 13.5022(13) _cell_length_c 9.5419(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1506.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 30.75 _exptl_crystal_description hexagonal _exptl_crystal_colour translucent _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.913 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 2.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4823 _exptl_absorpt_correction_T_max 0.7925 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16336 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0219 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 30.75 _reflns_number_total 2978 _reflns_number_gt 2573 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0434P)^2^+3.4127P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2978 _refine_ls_number_parameters 137 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.1015 _refine_ls_wR_factor_gt 0.0989 _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_restrained_S_all 1.128 _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 Cs1 Cs -1.0000 0.0000 0.0000 0.03144(12) Uani 1 6 d S . . Cs2 Cs -1.0000 0.0000 -0.5000 0.02637(11) Uani 1 6 d S . . Fe Fe -0.6667 -0.3333 -0.35285(6) 0.01525(13) Uani 1 3 d S . . Cl Cl -0.75540(6) 0.07276(6) -0.24243(8) 0.02728(15) Uani 1 1 d . . . O1 O -0.86574(19) -0.03172(19) -0.2477(2) 0.0310(5) Uani 1 1 d . . . O2 O -0.7461(2) 0.1313(2) -0.1132(3) 0.0385(5) Uani 1 1 d . . . O3 O -0.7503(2) 0.1458(2) -0.3557(3) 0.0462(7) Uani 1 1 d . . . O4 O -0.6661(2) 0.0457(3) -0.2526(4) 0.0559(9) Uani 1 1 d . . . N N -0.6667 -0.3333 -0.7077(5) 0.0283(9) Uani 1 3 d S . . N1 N -0.6886(2) -0.21880(19) -0.4563(2) 0.0203(4) Uani 1 1 d . . . N2 N -0.78877(19) -0.33710(19) -0.2384(2) 0.0198(4) Uani 1 1 d . . . N3 N -0.8984(3) -0.2631(3) -0.1934(3) 0.0348(6) Uani 1 1 d . . . H3B H -0.9306 -0.2205 -0.2010 0.042 Uiso 1 1 calc R . . C1 C -0.6636(3) -0.2250(3) -0.7135(3) 0.0306(6) Uani 1 1 d . . . H1A H -0.7414 -0.2395 -0.7355 0.037 Uiso 1 1 calc R . . H1B H -0.6128 -0.1794 -0.7914 0.037 Uiso 1 1 calc R . . C2 C -0.6225(3) -0.1538(3) -0.5791(3) 0.0271(6) Uani 1 1 d . . . H2A H -0.5407 -0.1286 -0.5640 0.033 Uiso 1 1 calc R . . H2B H -0.6295 -0.0846 -0.5899 0.033 Uiso 1 1 calc R . . C3 C -0.7610(3) -0.1942(3) -0.4022(3) 0.0263(6) Uani 1 1 d . . . H3A H -0.7753 -0.1371 -0.4390 0.032 Uiso 1 1 calc R . . C4 C -0.8182(2) -0.2614(3) -0.2807(3) 0.0242(5) Uani 1 1 d . . . C5 C -0.9202(3) -0.3422(3) -0.0925(4) 0.0371(7) Uani 1 1 d . . . H5A H -0.9723 -0.3615 -0.0167 0.044 Uiso 1 1 calc R . . C6 C -0.8526(3) -0.3890(3) -0.1210(3) 0.0283(6) Uani 1 1 d . . . H6A H -0.8503 -0.4475 -0.0683 0.034 Uiso 1 1 calc R . . 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 Cs1 0.03430(16) 0.03430(16) 0.0257(2) 0.000 0.000 0.01715(8) Cs2 0.03026(15) 0.03026(15) 0.01860(18) 0.000 0.000 0.01513(8) Fe 0.01458(17) 0.01458(17) 0.0166(3) 0.000 0.000 0.00729(9) Cl 0.0222(3) 0.0272(3) 0.0299(3) -0.0010(3) -0.0001(2) 0.0104(3) O1 0.0267(10) 0.0230(10) 0.0365(12) -0.0003(9) -0.0026(9) 0.0073(8) O2 0.0376(13) 0.0362(13) 0.0351(12) -0.0086(10) -0.0029(10) 0.0135(10) O3 0.0428(14) 0.0416(14) 0.0368(13) 0.0153(11) 0.0062(11) 0.0081(12) O4 0.0319(13) 0.0575(18) 0.087(2) -0.0286(17) -0.0115(14) 0.0289(13) N 0.0283(13) 0.0283(13) 0.028(2) 0.000 0.000 0.0141(6) N1 0.0244(10) 0.0194(10) 0.0184(10) 0.0004(8) -0.0021(8) 0.0117(9) N2 0.0184(10) 0.0205(10) 0.0208(10) -0.0006(8) 0.0013(8) 0.0099(8) N3 0.0363(14) 0.0407(15) 0.0398(15) -0.0019(12) 0.0088(12) 0.0285(13) C1 0.0406(17) 0.0342(15) 0.0200(12) 0.0053(11) -0.0005(11) 0.0209(14) C2 0.0335(15) 0.0228(13) 0.0238(12) 0.0052(10) 0.0006(11) 0.0131(11) C3 0.0358(15) 0.0276(13) 0.0243(13) -0.0002(10) -0.0031(11) 0.0225(12) C4 0.0254(12) 0.0288(13) 0.0252(12) -0.0035(10) -0.0002(10) 0.0186(11) C5 0.0363(17) 0.0398(17) 0.0368(16) -0.0008(14) 0.0152(14) 0.0203(15) C6 0.0293(14) 0.0273(14) 0.0265(13) 0.0010(11) 0.0082(11) 0.0126(12) _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 Cs1 O1 3.135(2) . ? Cs1 O1 3.135(2) 2_465 ? Cs1 O1 3.135(2) 3_345 ? Cs1 O1 3.136(2) 6_565 ? Cs1 O1 3.135(2) 4_355 ? Cs1 O1 3.136(2) 5_445 ? Cs1 O2 3.160(3) 2_465 ? Cs1 O2 3.160(3) 6_565 ? Cs1 O2 3.160(3) 3_345 ? Cs1 O2 3.160(3) 4_355 ? Cs1 O2 3.160(3) . ? Cs1 O2 3.160(3) 5_445 ? Cs2 O1 3.169(2) 4_354 ? Cs2 O1 3.169(2) . ? Cs2 O1 3.169(2) 6_564 ? Cs2 O1 3.169(2) 5_444 ? Cs2 O1 3.169(2) 2_465 ? Cs2 O1 3.169(2) 3_345 ? Cs2 O3 3.241(3) 6_564 ? Cs2 O3 3.241(3) 4_354 ? Cs2 O3 3.241(3) 2_465 ? Cs2 O3 3.241(3) . ? Cs2 O3 3.241(3) 3_345 ? Cs2 O3 3.241(3) 5_444 ? Fe N2 1.957(2) 3_445 ? Fe N2 1.957(2) 2_455 ? Fe N2 1.957(2) . ? Fe N1 1.978(2) . ? Fe N1 1.978(2) 2_455 ? Fe N1 1.978(2) 3_445 ? Cl O4 1.427(3) . ? Cl O2 1.436(3) . ? Cl O3 1.441(3) . ? Cl O1 1.453(2) . ? N C1 1.444(3) 2_455 ? N C1 1.444(3) 3_445 ? N C1 1.444(3) . ? N1 C3 1.288(4) . ? N1 C2 1.469(4) . ? N2 C4 1.332(3) . ? N2 C6 1.373(4) . ? N3 C5 1.356(5) . ? N3 C4 1.356(4) . ? N3 H3B 0.8800 . ? C1 C2 1.531(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.436(4) . ? C3 H3A 0.9500 . ? C5 C6 1.374(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? 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 O1 Cs1 O1 69.38(7) . 2_465 ? O1 Cs1 O1 69.38(7) . 3_345 ? O1 Cs1 O1 69.38(7) 2_465 3_345 ? O1 Cs1 O1 110.62(7) . 6_565 ? O1 Cs1 O1 110.62(7) 2_465 6_565 ? O1 Cs1 O1 180.0 3_345 6_565 ? O1 Cs1 O1 180.0 . 4_355 ? O1 Cs1 O1 110.62(7) 2_465 4_355 ? O1 Cs1 O1 110.62(7) 3_345 4_355 ? O1 Cs1 O1 69.38(7) 6_565 4_355 ? O1 Cs1 O1 110.62(7) . 5_445 ? O1 Cs1 O1 180.0 2_465 5_445 ? O1 Cs1 O1 110.62(7) 3_345 5_445 ? O1 Cs1 O1 69.38(7) 6_565 5_445 ? O1 Cs1 O1 69.38(7) 4_355 5_445 ? O1 Cs1 O2 109.15(6) . 2_465 ? O1 Cs1 O2 43.93(6) 2_465 2_465 ? O1 Cs1 O2 67.62(6) 3_345 2_465 ? O1 Cs1 O2 112.38(6) 6_565 2_465 ? O1 Cs1 O2 70.85(6) 4_355 2_465 ? O1 Cs1 O2 136.07(6) 5_445 2_465 ? O1 Cs1 O2 112.38(6) . 6_565 ? O1 Cs1 O2 70.85(6) 2_465 6_565 ? O1 Cs1 O2 136.07(6) 3_345 6_565 ? O1 Cs1 O2 43.93(6) 6_565 6_565 ? O1 Cs1 O2 67.62(6) 4_355 6_565 ? O1 Cs1 O2 109.15(6) 5_445 6_565 ? O2 Cs1 O2 71.05(5) 2_465 6_565 ? O1 Cs1 O2 67.62(6) . 3_345 ? O1 Cs1 O2 109.15(6) 2_465 3_345 ? O1 Cs1 O2 43.93(6) 3_345 3_345 ? O1 Cs1 O2 136.07(6) 6_565 3_345 ? O1 Cs1 O2 112.38(6) 4_355 3_345 ? O1 Cs1 O2 70.85(6) 5_445 3_345 ? O2 Cs1 O2 108.95(5) 2_465 3_345 ? O2 Cs1 O2 180.0 6_565 3_345 ? O1 Cs1 O2 136.07(6) . 4_355 ? O1 Cs1 O2 112.38(6) 2_465 4_355 ? O1 Cs1 O2 70.85(6) 3_345 4_355 ? O1 Cs1 O2 109.15(6) 6_565 4_355 ? O1 Cs1 O2 43.93(6) 4_355 4_355 ? O1 Cs1 O2 67.62(6) 5_445 4_355 ? O2 Cs1 O2 71.05(5) 2_465 4_355 ? O2 Cs1 O2 108.95(5) 6_565 4_355 ? O2 Cs1 O2 71.05(5) 3_345 4_355 ? O1 Cs1 O2 43.93(6) . . ? O1 Cs1 O2 67.62(6) 2_465 . ? O1 Cs1 O2 109.15(6) 3_345 . ? O1 Cs1 O2 70.85(6) 6_565 . ? O1 Cs1 O2 136.07(6) 4_355 . ? O1 Cs1 O2 112.38(6) 5_445 . ? O2 Cs1 O2 108.95(5) 2_465 . ? O2 Cs1 O2 71.05(5) 6_565 . ? O2 Cs1 O2 108.95(5) 3_345 . ? O2 Cs1 O2 180.00(8) 4_355 . ? O1 Cs1 O2 70.85(6) . 5_445 ? O1 Cs1 O2 136.07(6) 2_465 5_445 ? O1 Cs1 O2 112.38(6) 3_345 5_445 ? O1 Cs1 O2 67.62(6) 6_565 5_445 ? O1 Cs1 O2 109.15(6) 4_355 5_445 ? O1 Cs1 O2 43.93(6) 5_445 5_445 ? O2 Cs1 O2 180.00(7) 2_465 5_445 ? O2 Cs1 O2 108.95(5) 6_565 5_445 ? O2 Cs1 O2 71.05(5) 3_345 5_445 ? O2 Cs1 O2 108.95(5) 4_355 5_445 ? O2 Cs1 O2 71.05(5) . 5_445 ? O1 Cs2 O1 180.0 4_354 . ? O1 Cs2 O1 68.54(7) 4_354 6_564 ? O1 Cs2 O1 111.46(7) . 6_564 ? O1 Cs2 O1 68.54(7) 4_354 5_444 ? O1 Cs2 O1 111.46(7) . 5_444 ? O1 Cs2 O1 68.54(7) 6_564 5_444 ? O1 Cs2 O1 111.46(7) 4_354 2_465 ? O1 Cs2 O1 68.54(7) . 2_465 ? O1 Cs2 O1 111.46(7) 6_564 2_465 ? O1 Cs2 O1 180.0 5_444 2_465 ? O1 Cs2 O1 111.46(7) 4_354 3_345 ? O1 Cs2 O1 68.54(7) . 3_345 ? O1 Cs2 O1 180.00(5) 6_564 3_345 ? O1 Cs2 O1 111.46(7) 5_444 3_345 ? O1 Cs2 O1 68.54(7) 2_465 3_345 ? O1 Cs2 O3 61.04(7) 4_354 6_564 ? O1 Cs2 O3 118.96(7) . 6_564 ? O1 Cs2 O3 42.91(6) 6_564 6_564 ? O1 Cs2 O3 104.36(6) 5_444 6_564 ? O1 Cs2 O3 75.64(6) 2_465 6_564 ? O1 Cs2 O3 137.09(6) 3_345 6_564 ? O1 Cs2 O3 42.91(6) 4_354 4_354 ? O1 Cs2 O3 137.09(6) . 4_354 ? O1 Cs2 O3 104.36(6) 6_564 4_354 ? O1 Cs2 O3 61.04(7) 5_444 4_354 ? O1 Cs2 O3 118.96(7) 2_465 4_354 ? O1 Cs2 O3 75.64(6) 3_345 4_354 ? O3 Cs2 O3 103.24(6) 6_564 4_354 ? O1 Cs2 O3 75.64(6) 4_354 2_465 ? O1 Cs2 O3 104.36(6) . 2_465 ? O1 Cs2 O3 118.96(7) 6_564 2_465 ? O1 Cs2 O3 137.09(6) 5_444 2_465 ? O1 Cs2 O3 42.91(6) 2_465 2_465 ? O1 Cs2 O3 61.04(7) 3_345 2_465 ? O3 Cs2 O3 76.76(6) 6_564 2_465 ? O3 Cs2 O3 76.76(6) 4_354 2_465 ? O1 Cs2 O3 137.09(6) 4_354 . ? O1 Cs2 O3 42.91(6) . . ? O1 Cs2 O3 75.64(6) 6_564 . ? O1 Cs2 O3 118.96(7) 5_444 . ? O1 Cs2 O3 61.04(7) 2_465 . ? O1 Cs2 O3 104.36(6) 3_345 . ? O3 Cs2 O3 76.76(6) 6_564 . ? O3 Cs2 O3 180.0 4_354 . ? O3 Cs2 O3 103.24(6) 2_465 . ? O1 Cs2 O3 118.96(7) 4_354 3_345 ? O1 Cs2 O3 61.04(7) . 3_345 ? O1 Cs2 O3 137.09(6) 6_564 3_345 ? O1 Cs2 O3 75.64(6) 5_444 3_345 ? O1 Cs2 O3 104.36(6) 2_465 3_345 ? O1 Cs2 O3 42.91(6) 3_345 3_345 ? O3 Cs2 O3 180.0 6_564 3_345 ? O3 Cs2 O3 76.76(6) 4_354 3_345 ? O3 Cs2 O3 103.24(6) 2_465 3_345 ? O3 Cs2 O3 103.24(6) . 3_345 ? O1 Cs2 O3 104.36(6) 4_354 5_444 ? O1 Cs2 O3 75.64(6) . 5_444 ? O1 Cs2 O3 61.04(7) 6_564 5_444 ? O1 Cs2 O3 42.91(6) 5_444 5_444 ? O1 Cs2 O3 137.09(6) 2_465 5_444 ? O1 Cs2 O3 118.96(7) 3_345 5_444 ? O3 Cs2 O3 103.24(6) 6_564 5_444 ? O3 Cs2 O3 103.24(6) 4_354 5_444 ? O3 Cs2 O3 180.0 2_465 5_444 ? O3 Cs2 O3 76.76(6) . 5_444 ? O3 Cs2 O3 76.76(6) 3_345 5_444 ? N2 Fe N2 91.89(9) 3_445 2_455 ? N2 Fe N2 91.89(9) 3_445 . ? N2 Fe N2 91.89(9) 2_455 . ? N2 Fe N1 89.90(9) 3_445 . ? N2 Fe N1 172.80(10) 2_455 . ? N2 Fe N1 81.08(9) . . ? N2 Fe N1 172.80(10) 3_445 2_455 ? N2 Fe N1 81.08(9) 2_455 2_455 ? N2 Fe N1 89.90(9) . 2_455 ? N1 Fe N1 97.26(9) . 2_455 ? N2 Fe N1 81.08(9) 3_445 3_445 ? N2 Fe N1 89.90(9) 2_455 3_445 ? N2 Fe N1 172.80(10) . 3_445 ? N1 Fe N1 97.26(9) . 3_445 ? N1 Fe N1 97.26(9) 2_455 3_445 ? O4 Cl O2 110.26(18) . . ? O4 Cl O3 111.5(2) . . ? O2 Cl O3 107.81(18) . . ? O4 Cl O1 109.67(17) . . ? O2 Cl O1 109.23(15) . . ? O3 Cl O1 108.27(15) . . ? O4 Cl Cs1 136.30(17) . . ? O2 Cl Cs1 55.68(11) . . ? O3 Cl Cs1 112.16(13) . . ? O1 Cl Cs1 54.82(10) . . ? O4 Cl Cs2 128.42(13) . . ? O2 Cl Cs2 121.29(11) . . ? O3 Cl Cs2 55.55(12) . . ? O1 Cl Cs2 52.75(10) . . ? Cs1 Cl Cs2 78.140(16) . . ? Cl O1 Cs1 102.92(11) . . ? Cl O1 Cs2 105.85(11) . . ? Cs1 O1 Cs2 98.36(7) . . ? Cl O2 Cs1 102.28(12) . . ? Cl O3 Cs2 102.93(13) . . ? C1 N C1 119.85(3) 2_455 3_445 ? C1 N C1 119.85(3) 2_455 . ? C1 N C1 119.85(3) 3_445 . ? C3 N1 C2 118.6(2) . . ? C3 N1 Fe 115.56(19) . . ? C2 N1 Fe 125.53(19) . . ? C4 N2 C6 106.7(2) . . ? C4 N2 Fe 112.49(18) . . ? C6 N2 Fe 140.7(2) . . ? C5 N3 C4 107.9(3) . . ? C5 N3 H3B 126.1 . . ? C4 N3 H3B 126.1 . . ? N C1 C2 114.9(3) . . ? N C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C1 111.8(2) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N1 C3 C4 113.5(2) . . ? N1 C3 H3A 123.2 . . ? C4 C3 H3A 123.2 . . ? N2 C4 N3 110.1(3) . . ? N2 C4 C3 117.1(2) . . ? N3 C4 C3 132.8(3) . . ? N3 C5 C6 106.8(3) . . ? N3 C5 H5A 126.6 . . ? C6 C5 H5A 126.6 . . ? N2 C6 C5 108.6(3) . . ? N2 C6 H6A 125.7 . . ? C5 C6 H6A 125.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cs1 Cl O4 -81.9(2) . . . . ? O1 Cs1 Cl O4 178.63(19) 2_465 . . . ? O1 Cs1 Cl O4 -113.50(19) 3_345 . . . ? O1 Cs1 Cl O4 66.50(19) 6_565 . . . ? O1 Cs1 Cl O4 98.1(2) 4_355 . . . ? O1 Cs1 Cl O4 -1.37(19) 5_445 . . . ? O2 Cs1 Cl O4 -179.29(19) 2_465 . . . ? O2 Cs1 Cl O4 110.42(19) 6_565 . . . ? O2 Cs1 Cl O4 -69.58(19) 3_345 . . . ? O2 Cs1 Cl O4 -96.2(2) 4_355 . . . ? O2 Cs1 Cl O4 83.8(2) . . . . ? O2 Cs1 Cl O4 0.71(19) 5_445 . . . ? O1 Cs1 Cl O2 -165.69(19) . . . . ? O1 Cs1 Cl O2 94.80(15) 2_465 . . . ? O1 Cs1 Cl O2 162.67(15) 3_345 . . . ? O1 Cs1 Cl O2 -17.33(15) 6_565 . . . ? O1 Cs1 Cl O2 14.31(19) 4_355 . . . ? O1 Cs1 Cl O2 -85.20(15) 5_445 . . . ? O2 Cs1 Cl O2 96.89(9) 2_465 . . . ? O2 Cs1 Cl O2 26.59(14) 6_565 . . . ? O2 Cs1 Cl O2 -153.41(14) 3_345 . . . ? O2 Cs1 Cl O2 180.0 4_355 . . . ? O2 Cs1 Cl O2 -83.11(9) 5_445 . . . ? O1 Cs1 Cl O3 97.30(18) . . . . ? O1 Cs1 Cl O3 -2.21(14) 2_465 . . . ? O1 Cs1 Cl O3 65.66(14) 3_345 . . . ? O1 Cs1 Cl O3 -114.34(14) 6_565 . . . ? O1 Cs1 Cl O3 -82.70(18) 4_355 . . . ? O1 Cs1 Cl O3 177.79(14) 5_445 . . . ? O2 Cs1 Cl O3 -0.12(14) 2_465 . . . ? O2 Cs1 Cl O3 -70.41(14) 6_565 . . . ? O2 Cs1 Cl O3 109.59(14) 3_345 . . . ? O2 Cs1 Cl O3 82.99(19) 4_355 . . . ? O2 Cs1 Cl O3 -97.01(19) . . . . ? O2 Cs1 Cl O3 179.88(14) 5_445 . . . ? O1 Cs1 Cl O1 -99.51(16) 2_465 . . . ? O1 Cs1 Cl O1 -31.64(12) 3_345 . . . ? O1 Cs1 Cl O1 148.36(12) 6_565 . . . ? O1 Cs1 Cl O1 180.0 4_355 . . . ? O1 Cs1 Cl O1 80.49(16) 5_445 . . . ? O2 Cs1 Cl O1 -97.42(13) 2_465 . . . ? O2 Cs1 Cl O1 -167.71(12) 6_565 . . . ? O2 Cs1 Cl O1 12.29(12) 3_345 . . . ? O2 Cs1 Cl O1 -14.31(19) 4_355 . . . ? O2 Cs1 Cl O1 165.69(19) . . . . ? O2 Cs1 Cl O1 82.58(13) 5_445 . . . ? O1 Cs1 Cl Cs2 52.50(12) . . . . ? O1 Cs1 Cl Cs2 -47.01(5) 2_465 . . . ? O1 Cs1 Cl Cs2 20.86(4) 3_345 . . . ? O1 Cs1 Cl Cs2 -159.14(4) 6_565 . . . ? O1 Cs1 Cl Cs2 -127.50(12) 4_355 . . . ? O1 Cs1 Cl Cs2 132.99(5) 5_445 . . . ? O2 Cs1 Cl Cs2 -44.92(5) 2_465 . . . ? O2 Cs1 Cl Cs2 -115.21(5) 6_565 . . . ? O2 Cs1 Cl Cs2 64.79(5) 3_345 . . . ? O2 Cs1 Cl Cs2 38.19(14) 4_355 . . . ? O2 Cs1 Cl Cs2 -141.81(14) . . . . ? O2 Cs1 Cl Cs2 135.08(5) 5_445 . . . ? O1 Cs2 Cl O4 -93.6(2) 4_354 . . . ? O1 Cs2 Cl O4 86.4(2) . . . . ? O1 Cs2 Cl O4 -59.7(2) 6_564 . . . ? O1 Cs2 Cl O4 8.0(2) 5_444 . . . ? O1 Cs2 Cl O4 -172.0(2) 2_465 . . . ? O1 Cs2 Cl O4 120.3(2) 3_345 . . . ? O3 Cs2 Cl O4 -102.7(2) 6_564 . . . ? O3 Cs2 Cl O4 88.6(3) 4_354 . . . ? O3 Cs2 Cl O4 179.0(2) 2_465 . . . ? O3 Cs2 Cl O4 -91.4(3) . . . . ? O3 Cs2 Cl O4 77.3(2) 3_345 . . . ? O3 Cs2 Cl O4 -1.0(2) 5_444 . . . ? O1 Cs2 Cl O2 88.74(18) 4_354 . . . ? O1 Cs2 Cl O2 -91.26(18) . . . . ? O1 Cs2 Cl O2 122.63(14) 6_564 . . . ? O1 Cs2 Cl O2 -169.58(14) 5_444 . . . ? O1 Cs2 Cl O2 10.42(14) 2_465 . . . ? O1 Cs2 Cl O2 -57.37(14) 3_345 . . . ? O3 Cs2 Cl O2 79.66(14) 6_564 . . . ? O3 Cs2 Cl O2 -89.0(2) 4_354 . . . ? O3 Cs2 Cl O2 1.38(15) 2_465 . . . ? O3 Cs2 Cl O2 91.0(2) . . . . ? O3 Cs2 Cl O2 -100.34(14) 3_345 . . . ? O3 Cs2 Cl O2 -178.62(15) 5_444 . . . ? O1 Cs2 Cl O3 -2.2(2) 4_354 . . . ? O1 Cs2 Cl O3 177.8(2) . . . . ? O1 Cs2 Cl O3 31.64(16) 6_564 . . . ? O1 Cs2 Cl O3 99.44(17) 5_444 . . . ? O1 Cs2 Cl O3 -80.57(17) 2_465 . . . ? O1 Cs2 Cl O3 -148.36(16) 3_345 . . . ? O3 Cs2 Cl O3 -11.33(16) 6_564 . . . ? O3 Cs2 Cl O3 180.0 4_354 . . . ? O3 Cs2 Cl O3 -89.61(10) 2_465 . . . ? O3 Cs2 Cl O3 168.67(16) 3_345 . . . ? O3 Cs2 Cl O3 90.39(10) 5_444 . . . ? O1 Cs2 Cl O1 180.0 4_354 . . . ? O1 Cs2 Cl O1 -146.11(12) 6_564 . . . ? O1 Cs2 Cl O1 -78.32(17) 5_444 . . . ? O1 Cs2 Cl O1 101.68(17) 2_465 . . . ? O1 Cs2 Cl O1 33.89(12) 3_345 . . . ? O3 Cs2 Cl O1 170.91(13) 6_564 . . . ? O3 Cs2 Cl O1 2.2(2) 4_354 . . . ? O3 Cs2 Cl O1 92.64(14) 2_465 . . . ? O3 Cs2 Cl O1 -177.8(2) . . . . ? O3 Cs2 Cl O1 -9.09(13) 3_345 . . . ? O3 Cs2 Cl O1 -87.36(14) 5_444 . . . ? O1 Cs2 Cl Cs1 125.44(12) 4_354 . . . ? O1 Cs2 Cl Cs1 -54.56(12) . . . . ? O1 Cs2 Cl Cs1 159.33(4) 6_564 . . . ? O1 Cs2 Cl Cs1 -132.88(5) 5_444 . . . ? O1 Cs2 Cl Cs1 47.12(5) 2_465 . . . ? O1 Cs2 Cl Cs1 -20.67(4) 3_345 . . . ? O3 Cs2 Cl Cs1 116.35(5) 6_564 . . . ? O3 Cs2 Cl Cs1 -52.31(16) 4_354 . . . ? O3 Cs2 Cl Cs1 38.08(6) 2_465 . . . ? O3 Cs2 Cl Cs1 127.69(16) . . . . ? O3 Cs2 Cl Cs1 -63.65(5) 3_345 . . . ? O3 Cs2 Cl Cs1 -141.92(6) 5_444 . . . ? O4 Cl O1 Cs1 133.42(17) . . . . ? O2 Cl O1 Cs1 12.48(16) . . . . ? O3 Cl O1 Cs1 -104.67(16) . . . . ? Cs2 Cl O1 Cs1 -102.72(11) . . . . ? O4 Cl O1 Cs2 -123.86(18) . . . . ? O2 Cl O1 Cs2 115.20(14) . . . . ? O3 Cl O1 Cs2 -1.95(18) . . . . ? Cs1 Cl O1 Cs2 102.72(11) . . . . ? O1 Cs1 O1 Cl 71.03(15) 2_465 . . . ? O1 Cs1 O1 Cl 145.93(12) 3_345 . . . ? O1 Cs1 O1 Cl -34.07(12) 6_565 . . . ? O1 Cs1 O1 Cl -167(23) 4_355 . . . ? O1 Cs1 O1 Cl -108.97(15) 5_445 . . . ? O2 Cs1 O1 Cl 90.08(12) 2_465 . . . ? O2 Cs1 O1 Cl 13.31(13) 6_565 . . . ? O2 Cs1 O1 Cl -166.69(13) 3_345 . . . ? O2 Cs1 O1 Cl 172.32(10) 4_355 . . . ? O2 Cs1 O1 Cl -7.68(10) . . . . ? O2 Cs1 O1 Cl -89.92(12) 5_445 . . . ? O1 Cs1 O1 Cs2 -37.452(18) 2_465 . . . ? O1 Cs1 O1 Cs2 37.452(18) 3_345 . . . ? O1 Cs1 O1 Cs2 -142.548(18) 6_565 . . . ? O1 Cs1 O1 Cs2 84(23) 4_355 . . . ? O1 Cs1 O1 Cs2 142.548(18) 5_445 . . . ? O2 Cs1 O1 Cs2 -18.40(8) 2_465 . . . ? O2 Cs1 O1 Cs2 -95.18(7) 6_565 . . . ? O2 Cs1 O1 Cs2 84.83(7) 3_345 . . . ? O2 Cs1 O1 Cs2 63.84(11) 4_355 . . . ? O2 Cs1 O1 Cs2 -116.16(11) . . . . ? O2 Cs1 O1 Cs2 161.60(8) 5_445 . . . ? O1 Cs2 O1 Cl -158(7) 4_354 . . . ? O1 Cs2 O1 Cl 36.70(12) 6_564 . . . ? O1 Cs2 O1 Cl 111.17(15) 5_444 . . . ? O1 Cs2 O1 Cl -68.83(15) 2_465 . . . ? O1 Cs2 O1 Cl -143.30(12) 3_345 . . . ? O3 Cs2 O1 Cl -10.30(15) 6_564 . . . ? O3 Cs2 O1 Cl -178.79(11) 4_354 . . . ? O3 Cs2 O1 Cl -92.91(13) 2_465 . . . ? O3 Cs2 O1 Cl 1.21(11) . . . . ? O3 Cs2 O1 Cl 169.70(15) 3_345 . . . ? O3 Cs2 O1 Cl 87.09(13) 5_444 . . . ? O1 Cs2 O1 Cs1 -52(7) 4_354 . . . ? O1 Cs2 O1 Cs1 142.767(18) 6_564 . . . ? O1 Cs2 O1 Cs1 -142.768(18) 5_444 . . . ? O1 Cs2 O1 Cs1 37.232(18) 2_465 . . . ? O1 Cs2 O1 Cs1 -37.233(18) 3_345 . . . ? O3 Cs2 O1 Cs1 95.76(7) 6_564 . . . ? O3 Cs2 O1 Cs1 -72.73(11) 4_354 . . . ? O3 Cs2 O1 Cs1 13.15(8) 2_465 . . . ? O3 Cs2 O1 Cs1 107.27(11) . . . . ? O3 Cs2 O1 Cs1 -84.24(7) 3_345 . . . ? O3 Cs2 O1 Cs1 -166.85(8) 5_444 . . . ? O4 Cl O2 Cs1 -132.93(18) . . . . ? O3 Cl O2 Cs1 105.09(15) . . . . ? O1 Cl O2 Cs1 -12.35(16) . . . . ? Cs2 Cl O2 Cs1 45.08(14) . . . . ? O1 Cs1 O2 Cl 7.75(10) . . . . ? O1 Cs1 O2 Cl -75.27(13) 2_465 . . . ? O1 Cs1 O2 Cl -18.37(15) 3_345 . . . ? O1 Cs1 O2 Cl 161.63(15) 6_565 . . . ? O1 Cs1 O2 Cl -172.25(10) 4_355 . . . ? O1 Cs1 O2 Cl 104.73(13) 5_445 . . . ? O2 Cs1 O2 Cl -90.50(9) 2_465 . . . ? O2 Cs1 O2 Cl -151.75(15) 6_565 . . . ? O2 Cs1 O2 Cl 28.25(15) 3_345 . . . ? O2 Cs1 O2 Cl -122(11) 4_355 . . . ? O2 Cs1 O2 Cl 89.50(9) 5_445 . . . ? O4 Cl O3 Cs2 122.64(15) . . . . ? O2 Cl O3 Cs2 -116.17(14) . . . . ? O1 Cl O3 Cs2 1.88(17) . . . . ? Cs1 Cl O3 Cs2 -56.74(13) . . . . ? O1 Cs2 O3 Cl 178.80(11) 4_354 . . . ? O1 Cs2 O3 Cl -1.20(11) . . . . ? O1 Cs2 O3 Cl -147.30(17) 6_564 . . . ? O1 Cs2 O3 Cl -92.28(15) 5_444 . . . ? O1 Cs2 O3 Cl 87.72(15) 2_465 . . . ? O1 Cs2 O3 Cl 32.70(17) 3_345 . . . ? O3 Cs2 O3 Cl 168.46(17) 6_564 . . . ? O3 Cs2 O3 Cl -43(7) 4_354 . . . ? O3 Cs2 O3 Cl 95.75(10) 2_465 . . . ? O3 Cs2 O3 Cl -11.54(17) 3_345 . . . ? O3 Cs2 O3 Cl -84.25(10) 5_444 . . . ? N2 Fe N1 C3 -87.8(2) 3_445 . . . ? N2 Fe N1 C3 16.7(9) 2_455 . . . ? N2 Fe N1 C3 4.2(2) . . . . ? N1 Fe N1 C3 92.9(3) 2_455 . . . ? N1 Fe N1 C3 -168.8(2) 3_445 . . . ? N2 Fe N1 C2 86.2(2) 3_445 . . . ? N2 Fe N1 C2 -169.4(7) 2_455 . . . ? N2 Fe N1 C2 178.1(2) . . . . ? N1 Fe N1 C2 -93.12(17) 2_455 . . . ? N1 Fe N1 C2 5.2(2) 3_445 . . . ? N2 Fe N2 C4 86.3(2) 3_445 . . . ? N2 Fe N2 C4 178.3(2) 2_455 . . . ? N1 Fe N2 C4 -3.3(2) . . . . ? N1 Fe N2 C4 -100.6(2) 2_455 . . . ? N1 Fe N2 C4 74.0(8) 3_445 . . . ? N2 Fe N2 C6 -89.0(3) 3_445 . . . ? N2 Fe N2 C6 3.0(3) 2_455 . . . ? N1 Fe N2 C6 -178.6(3) . . . . ? N1 Fe N2 C6 84.1(3) 2_455 . . . ? N1 Fe N2 C6 -101.3(8) 3_445 . . . ? C1 N C1 C2 113.4(4) 2_455 . . . ? C1 N C1 C2 -74.3(5) 3_445 . . . ? C3 N1 C2 C1 -106.9(3) . . . . ? Fe N1 C2 C1 79.4(3) . . . . ? N C1 C2 N1 -54.1(4) . . . . ? C2 N1 C3 C4 -178.5(2) . . . . ? Fe N1 C3 C4 -4.0(3) . . . . ? C6 N2 C4 N3 0.3(3) . . . . ? Fe N2 C4 N3 -176.6(2) . . . . ? C6 N2 C4 C3 179.1(3) . . . . ? Fe N2 C4 C3 2.2(3) . . . . ? C5 N3 C4 N2 0.2(4) . . . . ? C5 N3 C4 C3 -178.4(3) . . . . ? N1 C3 C4 N2 1.2(4) . . . . ? N1 C3 C4 N3 179.7(3) . . . . ? C4 N3 C5 C6 -0.5(4) . . . . ? C4 N2 C6 C5 -0.6(4) . . . . ? Fe N2 C6 C5 174.9(3) . . . . ? N3 C5 C6 N2 0.7(4) . . . . ? 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 N3 H3B O1 0.88 2.29 2.974(4) 134.9 . N3 H3B O2 0.88 2.54 3.185(4) 130.5 3_345 N3 H3B O3 0.88 2.62 3.260(4) 130.0 3_345 C3 H3A O3 0.95 2.38 3.153(4) 138.6 5_444 _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.804 _refine_diff_density_min -2.476 _refine_diff_density_rms 0.109 #===END data_ctbe48nh4ltm _database_code_depnum_ccdc_archive 'CCDC 635260' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H28 Cl3 Fe N11 O12' _chemical_formula_weight 752.71 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 Trigonal _symmetry_space_group_name_H-M P-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' _cell_length_a 13.4838(4) _cell_length_b 13.4838(4) _cell_length_c 9.3520(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 1472.51(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8718 _cell_measurement_theta_min 2.79 _cell_measurement_theta_max 30.56 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 772 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.860 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details Sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16951 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0143 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 30.68 _reflns_number_total 2884 _reflns_number_gt 2642 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0406P)^2^+0.4838P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2884 _refine_ls_number_parameters 145 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Fe Fe 0.6667 0.3333 0.14241(3) 0.01605(8) Uani 1 3 d S . . Cl Cl 1.07463(3) 0.23610(2) 0.25628(3) 0.02667(9) Uani 1 1 d . . . O1 O 0.96967(8) 0.12609(8) 0.25007(11) 0.0336(2) Uani 1 1 d . . . O2 O 1.13238(9) 0.24429(9) 0.38878(11) 0.0372(2) Uani 1 1 d . . . O3 O 1.04823(11) 0.32630(10) 0.24634(15) 0.0493(3) Uani 1 1 d . . . O4 O 1.14706(10) 0.24117(10) 0.13991(12) 0.0450(3) Uani 1 1 d . . . N N 0.6667 0.3333 -0.2190(2) 0.0308(4) Uani 1 3 d S . . N1 N 0.78372(8) 0.31509(9) 0.03758(10) 0.02219(19) Uani 1 1 d . . . N2 N 0.66584(8) 0.21237(8) 0.25911(10) 0.02076(19) Uani 1 1 d . . . N3 N 0.74547(11) 0.10821(11) 0.30738(14) 0.0359(3) Uani 1 1 d . . . H3B H 0.7906 0.0787 0.3011 0.043 Uiso 1 1 calc R . . N1A N 1.0000 0.0000 0.0000 0.0276(5) Uani 1 6 d S . . H1A1 H 0.960(6) 0.007(8) 0.047(4) 0.11(2) Uiso 0.67 1 d P . . N2A N 1.0000 0.0000 0.5000 0.0248(5) Uani 1 6 d S . . H2A1 H 0.970(9) 0.029(9) 0.461(5) 0.13(3) Uiso 0.67 1 d P . . C1 C 0.77569(13) 0.33844(14) -0.22499(14) 0.0337(3) Uani 1 1 d . . . H1A H 0.8204 0.3893 -0.3050 0.040 Uiso 1 1 calc R . . H1B H 0.7625 0.2609 -0.2468 0.040 Uiso 1 1 calc R . . C2 C 0.84772(11) 0.38155(12) -0.08795(13) 0.0299(3) Uani 1 1 d . . . H2A H 0.9178 0.3760 -0.0991 0.036 Uiso 1 1 calc R . . H2B H 0.8715 0.4631 -0.0730 0.036 Uiso 1 1 calc R . . C3 C 0.81172(11) 0.24500(12) 0.09406(14) 0.0277(2) Uani 1 1 d . . . H3A H 0.8708 0.2333 0.0574 0.033 Uiso 1 1 calc R . . C4 C 0.74452(11) 0.18643(11) 0.21806(13) 0.0253(2) Uani 1 1 d . . . C5 C 0.61451(11) 0.14817(11) 0.37856(14) 0.0291(3) Uani 1 1 d . . . H5A H 0.5546 0.1487 0.4314 0.035 Uiso 1 1 calc R . . C6 C 0.66381(14) 0.08316(13) 0.40911(17) 0.0377(3) Uani 1 1 d . . . H6A H 0.6448 0.0308 0.4862 0.045 Uiso 1 1 calc R . . 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 Fe 0.01624(9) 0.01624(9) 0.01566(13) 0.000 0.000 0.00812(5) Cl 0.02725(15) 0.02287(14) 0.02825(15) 0.00194(10) -0.00036(10) 0.01129(11) O1 0.0258(4) 0.0269(5) 0.0413(6) -0.0010(4) 0.0011(4) 0.0081(4) O2 0.0379(5) 0.0398(6) 0.0330(5) -0.0019(4) -0.0082(4) 0.0188(5) O3 0.0555(7) 0.0318(5) 0.0686(8) -0.0070(5) -0.0212(6) 0.0278(5) O4 0.0450(6) 0.0442(6) 0.0359(6) 0.0100(5) 0.0160(5) 0.0149(5) N 0.0339(6) 0.0339(6) 0.0244(9) 0.000 0.000 0.0170(3) N1 0.0213(4) 0.0267(5) 0.0189(4) -0.0018(4) 0.0011(3) 0.0122(4) N2 0.0224(4) 0.0200(4) 0.0202(4) 0.0007(3) -0.0013(3) 0.0108(4) N3 0.0439(7) 0.0370(6) 0.0394(6) 0.0053(5) -0.0037(5) 0.0298(6) N1A 0.0311(8) 0.0311(8) 0.0207(12) 0.000 0.000 0.0155(4) N2A 0.0266(8) 0.0266(8) 0.0212(11) 0.000 0.000 0.0133(4) C1 0.0382(7) 0.0449(8) 0.0200(5) 0.0004(5) 0.0059(5) 0.0223(6) C2 0.0266(6) 0.0391(7) 0.0238(6) 0.0027(5) 0.0076(5) 0.0162(5) C3 0.0283(6) 0.0370(7) 0.0258(6) -0.0042(5) -0.0007(5) 0.0224(5) C4 0.0296(6) 0.0262(5) 0.0263(6) -0.0014(4) -0.0039(4) 0.0184(5) C5 0.0302(6) 0.0293(6) 0.0262(6) 0.0077(5) 0.0013(5) 0.0137(5) C6 0.0420(8) 0.0356(7) 0.0370(7) 0.0132(6) -0.0024(6) 0.0204(6) _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 Fe N2 1.9578(10) 2_655 ? Fe N2 1.9579(10) . ? Fe N2 1.9579(10) 3_665 ? Fe N1 1.9751(10) . ? Fe N1 1.9751(10) 2_655 ? Fe N1 1.9751(10) 3_665 ? Cl O3 1.4308(11) . ? Cl O2 1.4381(10) . ? Cl O4 1.4409(11) . ? Cl O1 1.4516(10) . ? N C1 1.4379(15) . ? N C1 1.4380(15) 3_665 ? N C1 1.4380(15) 2_655 ? N1 C3 1.2929(16) . ? N1 C2 1.4672(15) . ? N2 C4 1.3290(15) . ? N2 C5 1.3701(16) . ? N3 C4 1.3505(16) . ? N3 C6 1.364(2) . ? N3 H3B 0.8800 . ? N1A H1A1 0.74(4) . ? N2A H2A1 0.78(4) . ? C1 C2 1.5360(19) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.4402(18) . ? C3 H3A 0.9500 . ? C5 C6 1.3692(19) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? 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 N2 Fe N2 91.95(4) 2_655 . ? N2 Fe N2 91.95(4) 2_655 3_665 ? N2 Fe N2 91.95(4) . 3_665 ? N2 Fe N1 89.59(4) 2_655 . ? N2 Fe N1 81.08(4) . . ? N2 Fe N1 172.91(4) 3_665 . ? N2 Fe N1 81.08(4) 2_655 2_655 ? N2 Fe N1 172.91(4) . 2_655 ? N2 Fe N1 89.58(4) 3_665 2_655 ? N1 Fe N1 97.49(4) . 2_655 ? N2 Fe N1 172.91(4) 2_655 3_665 ? N2 Fe N1 89.59(4) . 3_665 ? N2 Fe N1 81.08(4) 3_665 3_665 ? N1 Fe N1 97.49(4) . 3_665 ? N1 Fe N1 97.49(4) 2_655 3_665 ? O3 Cl O2 110.24(7) . . ? O3 Cl O4 111.19(8) . . ? O2 Cl O4 108.60(7) . . ? O3 Cl O1 109.64(7) . . ? O2 Cl O1 109.07(6) . . ? O4 Cl O1 108.04(7) . . ? C1 N C1 119.849(13) . 3_665 ? C1 N C1 119.848(13) . 2_655 ? C1 N C1 119.844(13) 3_665 2_655 ? C3 N1 C2 118.41(11) . . ? C3 N1 Fe 115.59(8) . . ? C2 N1 Fe 125.71(8) . . ? C4 N2 C5 106.66(10) . . ? C4 N2 Fe 112.67(8) . . ? C5 N2 Fe 140.49(9) . . ? C4 N3 C6 107.65(11) . . ? C4 N3 H3B 126.2 . . ? C6 N3 H3B 126.2 . . ? N C1 C2 115.04(12) . . ? N C1 H1A 108.5 . . ? C2 C1 H1A 108.5 . . ? N C1 H1B 108.5 . . ? C2 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? N1 C2 C1 111.65(11) . . ? N1 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N1 C3 C4 113.34(11) . . ? N1 C3 H3A 123.3 . . ? C4 C3 H3A 123.3 . . ? N2 C4 N3 110.33(12) . . ? N2 C4 C3 117.03(11) . . ? N3 C4 C3 132.63(12) . . ? C6 C5 N2 108.72(12) . . ? C6 C5 H5A 125.6 . . ? N2 C5 H5A 125.6 . . ? N3 C6 C5 106.63(12) . . ? N3 C6 H6A 126.7 . . ? C5 C6 H6A 126.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Fe N1 C3 87.03(10) 2_655 . . . ? N2 Fe N1 C3 -5.01(9) . . . . ? N2 Fe N1 C3 -15.5(4) 3_665 . . . ? N1 Fe N1 C3 167.98(9) 2_655 . . . ? N1 Fe N1 C3 -93.40(11) 3_665 . . . ? N2 Fe N1 C2 -86.65(10) 2_655 . . . ? N2 Fe N1 C2 -178.69(10) . . . . ? N2 Fe N1 C2 170.8(3) 3_665 . . . ? N1 Fe N1 C2 -5.70(10) 2_655 . . . ? N1 Fe N1 C2 92.92(8) 3_665 . . . ? N2 Fe N2 C4 -85.10(10) 2_655 . . . ? N2 Fe N2 C4 -177.12(8) 3_665 . . . ? N1 Fe N2 C4 4.17(8) . . . . ? N1 Fe N2 C4 -74.7(4) 2_655 . . . ? N1 Fe N2 C4 101.82(9) 3_665 . . . ? N2 Fe N2 C5 89.17(11) 2_655 . . . ? N2 Fe N2 C5 -2.84(14) 3_665 . . . ? N1 Fe N2 C5 178.45(14) . . . . ? N1 Fe N2 C5 99.5(4) 2_655 . . . ? N1 Fe N2 C5 -83.90(14) 3_665 . . . ? C1 N C1 C2 -113.84(18) 3_665 . . . ? C1 N C1 C2 74.0(2) 2_655 . . . ? C3 N1 C2 C1 107.76(13) . . . . ? Fe N1 C2 C1 -78.72(13) . . . . ? N C1 C2 N1 54.26(16) . . . . ? C2 N1 C3 C4 178.84(11) . . . . ? Fe N1 C3 C4 4.67(14) . . . . ? C5 N2 C4 N3 -0.20(14) . . . . ? Fe N2 C4 N3 176.00(9) . . . . ? C5 N2 C4 C3 -179.21(11) . . . . ? Fe N2 C4 C3 -3.01(14) . . . . ? C6 N3 C4 N2 0.19(16) . . . . ? C6 N3 C4 C3 178.99(14) . . . . ? N1 C3 C4 N2 -1.07(17) . . . . ? N1 C3 C4 N3 -179.81(14) . . . . ? C4 N2 C5 C6 0.14(15) . . . . ? Fe N2 C5 C6 -174.35(11) . . . . ? C4 N3 C6 C5 -0.09(17) . . . . ? N2 C5 C6 N3 -0.03(17) . . . . ? 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 N3 H3B O1 0.88 2.22 2.9589(16) 141.6 . N3 H3B O2 0.88 2.51 3.1333(16) 128.6 2_645 N3 H3B O4 0.88 2.62 3.2278(18) 126.6 2_645 N1A H1A1 O1 0.74(4) 2.45(6) 3.0369(10) 138(7) . N1A H1A1 O4 0.74(4) 2.50(6) 3.1258(12) 143(9) 2_645 N2A H2A1 O1 0.78(4) 2.37(6) 3.0359(11) 144(7) . N2A H2A1 O2 0.78(4) 2.58(4) 3.0395(11) 119(4) 6_546 _diffrn_measured_fraction_theta_max 0.944 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.375 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.050