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 'Michael Carney' _publ_contact_author_address ; Chemistry University of Wisconsin-Eau Claire 105 Garfield Avenue Eau Claire Wisconsin 54702 UNITED STATES OF AMERICA ; _publ_contact_author_email CARNEYMJ@UWEC.EDU _publ_section_title ; Alternatives to Pyridinediimine Ligands: Syntheses and Structures of Metal Complexes Supported by Donor-Modified ?-Diimine Ligands ; loop_ _publ_author_name 'Michael Carney' 'Deidra L. Gerlach' 'Jason Halfen' 'Benjamin M. Schmiege' 'Brooke L. Small' data_1 _database_code_depnum_ccdc_archive 'CCDC 636867' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040017 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H15 N O S' _chemical_formula_weight 365.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 14.488(2) _cell_length_b 15.586(2) _cell_length_c 16.1046(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3636.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.15 _cell_measurement_theta_max 13.65 _exptl_crystal_description block _exptl_crystal_colour amber _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 6255 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3195 _reflns_number_gt 1887 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3195 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 0.990 _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 S1 S 0.93043(5) 0.82412(5) 0.43955(4) 0.0538(2) Uani 1 1 d . . . N1 N 0.92885(15) 0.62819(14) 0.45092(12) 0.0481(6) Uani 1 1 d . . . O1 O 0.75688(13) 0.54250(13) 0.42202(10) 0.0629(6) Uani 1 1 d . . . C1 C 0.95724(18) 0.59049(17) 0.30054(15) 0.0427(7) Uani 1 1 d . . . C2 C 1.04093(19) 0.61797(19) 0.27110(16) 0.0550(8) Uani 1 1 d . . . H2A H 1.0835 0.6434 0.3066 0.066 Uiso 1 1 calc R . . C3 C 1.0615(2) 0.6071(2) 0.18618(18) 0.0654(9) Uani 1 1 d . . . H3A H 1.1185 0.6255 0.1665 0.079 Uiso 1 1 calc R . . C4 C 1.0013(2) 0.57084(19) 0.13223(17) 0.0607(9) Uani 1 1 d . . . H4A H 1.0180 0.5645 0.0768 0.073 Uiso 1 1 calc R . . C5 C 0.9137(2) 0.54261(17) 0.15883(16) 0.0500(7) Uani 1 1 d . . . C6 C 0.8427(2) 0.5066(2) 0.11032(17) 0.0632(9) Uani 1 1 d . . . H6A H 0.8512 0.5002 0.0534 0.076 Uiso 1 1 calc R . . C7 C 0.7619(2) 0.48096(19) 0.14551(17) 0.0656(9) Uani 1 1 d . . . H7A H 0.7169 0.4565 0.1118 0.079 Uiso 1 1 calc R . . C8 C 0.7439(2) 0.49001(18) 0.23104(17) 0.0598(8) Uani 1 1 d . . . H8A H 0.6884 0.4714 0.2538 0.072 Uiso 1 1 calc R . . C9 C 0.81075(19) 0.52710(17) 0.27983(15) 0.0462(7) Uani 1 1 d . . . C10 C 0.89454(18) 0.55227(16) 0.24399(15) 0.0437(6) Uani 1 1 d . . . C11 C 0.90937(17) 0.59399(17) 0.38135(15) 0.0411(6) Uani 1 1 d . . . C12 C 0.81426(19) 0.55126(17) 0.36822(16) 0.0470(7) Uani 1 1 d . . . C13 C 1.01666(18) 0.66697(19) 0.46243(14) 0.0431(7) Uani 1 1 d . . . C14 C 1.02605(18) 0.75560(19) 0.45978(15) 0.0447(7) Uani 1 1 d . . . C15 C 1.1119(2) 0.79129(19) 0.47622(16) 0.0519(7) Uani 1 1 d . . . H15A H 1.1189 0.8506 0.4741 0.062 Uiso 1 1 calc R . . C16 C 1.1867(2) 0.7409(2) 0.49555(16) 0.0571(8) Uani 1 1 d . . . H16A H 1.2437 0.7661 0.5064 0.069 Uiso 1 1 calc R . . C17 C 1.1770(2) 0.6534(2) 0.49872(16) 0.0583(8) Uani 1 1 d . . . H17A H 1.2274 0.6191 0.5120 0.070 Uiso 1 1 calc R . . C18 C 1.0925(2) 0.61627(19) 0.48219(15) 0.0541(8) Uani 1 1 d . . . H18A H 1.0863 0.5569 0.4843 0.065 Uiso 1 1 calc R . . C19 C 0.9150(2) 0.81093(17) 0.33042(15) 0.0481(7) Uani 1 1 d . . . C20 C 0.9837(2) 0.8347(2) 0.27595(17) 0.0642(9) Uani 1 1 d . . . H20A H 1.0388 0.8574 0.2958 0.077 Uiso 1 1 calc R . . C21 C 0.9699(3) 0.8246(2) 0.19100(18) 0.0794(11) Uani 1 1 d . . . H21A H 1.0164 0.8399 0.1541 0.095 Uiso 1 1 calc R . . C22 C 0.8892(3) 0.7925(2) 0.1615(2) 0.0822(11) Uani 1 1 d . . . H22A H 0.8808 0.7859 0.1046 0.099 Uiso 1 1 calc R . . C23 C 0.8200(2) 0.7696(2) 0.2154(2) 0.0739(10) Uani 1 1 d . . . H23A H 0.7647 0.7477 0.1951 0.089 Uiso 1 1 calc R . . C24 C 0.8330(2) 0.77947(19) 0.30049(17) 0.0594(8) Uani 1 1 d . . . H24A H 0.7860 0.7647 0.3372 0.071 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 S1 0.0570(5) 0.0653(5) 0.0392(4) -0.0046(4) -0.0006(3) 0.0105(4) N1 0.0496(14) 0.0579(15) 0.0367(12) 0.0001(11) 0.0000(11) -0.0053(12) O1 0.0535(12) 0.0838(16) 0.0514(11) 0.0077(11) 0.0084(11) -0.0097(12) C1 0.0445(16) 0.0458(16) 0.0379(15) 0.0021(13) 0.0015(13) 0.0045(14) C2 0.0483(18) 0.068(2) 0.0486(17) 0.0029(15) 0.0040(14) 0.0008(16) C3 0.056(2) 0.087(3) 0.0533(19) 0.0076(18) 0.0143(16) 0.0045(19) C4 0.078(2) 0.065(2) 0.0391(17) 0.0039(16) 0.0133(17) 0.0155(19) C5 0.070(2) 0.0419(16) 0.0381(15) -0.0012(13) -0.0009(14) 0.0104(16) C6 0.094(3) 0.051(2) 0.0438(17) -0.0057(15) -0.0079(18) 0.0078(19) C7 0.086(3) 0.053(2) 0.057(2) -0.0099(16) -0.0253(18) -0.0031(19) C8 0.0655(19) 0.0520(19) 0.0620(19) -0.0010(16) -0.0083(17) -0.0071(17) C9 0.0528(17) 0.0438(17) 0.0420(15) 0.0005(13) -0.0035(14) 0.0004(15) C10 0.0533(17) 0.0397(15) 0.0381(14) -0.0009(13) -0.0020(13) 0.0065(14) C11 0.0447(16) 0.0430(16) 0.0355(14) 0.0037(13) 0.0002(12) 0.0021(13) C12 0.0459(17) 0.0479(17) 0.0472(16) 0.0078(14) 0.0020(14) -0.0009(15) C13 0.0423(17) 0.060(2) 0.0273(13) -0.0013(13) 0.0007(11) 0.0000(16) C14 0.0446(17) 0.0589(19) 0.0305(14) 0.0001(13) -0.0006(12) -0.0007(15) C15 0.0546(19) 0.0556(19) 0.0454(16) -0.0010(15) 0.0029(14) -0.0028(17) C16 0.0461(18) 0.074(2) 0.0516(17) -0.0028(15) -0.0026(14) -0.0082(18) C17 0.0506(19) 0.068(2) 0.0561(18) 0.0007(16) -0.0082(15) 0.0113(17) C18 0.060(2) 0.054(2) 0.0485(17) 0.0004(15) -0.0035(14) 0.0015(17) C19 0.0569(19) 0.0481(18) 0.0394(14) 0.0008(13) -0.0026(14) 0.0081(15) C20 0.073(2) 0.068(2) 0.0510(18) 0.0036(16) 0.0038(16) -0.0036(18) C21 0.099(3) 0.095(3) 0.0444(19) 0.0076(19) 0.0148(19) 0.011(2) C22 0.113(3) 0.087(3) 0.047(2) -0.0037(19) -0.011(2) 0.024(3) C23 0.086(3) 0.075(2) 0.060(2) -0.0039(18) -0.024(2) 0.011(2) C24 0.060(2) 0.066(2) 0.0522(18) 0.0002(16) -0.0043(15) 0.0057(17) _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 S1 C14 1.779(3) . ? S1 C19 1.784(3) . ? N1 C11 1.272(3) . ? N1 C13 1.421(3) . ? O1 C12 1.209(3) . ? C1 C2 1.371(3) . ? C1 C10 1.418(3) . ? C1 C11 1.476(3) . ? C2 C3 1.410(4) . ? C3 C4 1.355(4) . ? C4 C5 1.410(4) . ? C5 C10 1.408(3) . ? C5 C6 1.409(4) . ? C6 C7 1.360(4) . ? C7 C8 1.409(4) . ? C8 C9 1.374(3) . ? C9 C10 1.400(3) . ? C9 C12 1.473(3) . ? C11 C12 1.545(4) . ? C13 C14 1.389(4) . ? C13 C18 1.391(4) . ? C14 C15 1.388(3) . ? C15 C16 1.374(4) . ? C16 C17 1.373(4) . ? C17 C18 1.380(4) . ? C19 C24 1.373(4) . ? C19 C20 1.378(4) . ? C20 C21 1.392(4) . ? C21 C22 1.357(5) . ? C22 C23 1.373(4) . ? C23 C24 1.392(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 C14 S1 C19 102.07(12) . . ? C11 N1 C13 119.5(2) . . ? C2 C1 C10 118.4(2) . . ? C2 C1 C11 135.2(3) . . ? C10 C1 C11 106.3(2) . . ? C1 C2 C3 119.0(3) . . ? C4 C3 C2 122.4(3) . . ? C3 C4 C5 121.0(3) . . ? C10 C5 C6 116.0(3) . . ? C10 C5 C4 116.1(3) . . ? C6 C5 C4 127.8(3) . . ? C7 C6 C5 121.0(3) . . ? C6 C7 C8 122.5(3) . . ? C9 C8 C7 118.1(3) . . ? C8 C9 C10 119.5(2) . . ? C8 C9 C12 133.2(3) . . ? C10 C9 C12 107.3(2) . . ? C9 C10 C5 122.9(2) . . ? C9 C10 C1 114.1(2) . . ? C5 C10 C1 123.0(3) . . ? N1 C11 C1 133.5(2) . . ? N1 C11 C12 119.9(2) . . ? C1 C11 C12 106.4(2) . . ? O1 C12 C9 129.8(3) . . ? O1 C12 C11 124.3(2) . . ? C9 C12 C11 105.9(2) . . ? C14 C13 C18 119.7(3) . . ? C14 C13 N1 120.5(2) . . ? C18 C13 N1 119.7(3) . . ? C15 C14 C13 118.7(3) . . ? C15 C14 S1 119.5(2) . . ? C13 C14 S1 121.8(2) . . ? C16 C15 C14 121.4(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 120.0(3) . . ? C17 C18 C13 120.5(3) . . ? C24 C19 C20 119.9(3) . . ? C24 C19 S1 119.7(2) . . ? C20 C19 S1 120.4(2) . . ? C19 C20 C21 119.4(3) . . ? C22 C21 C20 120.7(3) . . ? C21 C22 C23 120.3(3) . . ? C22 C23 C24 119.6(3) . . ? C19 C24 C23 120.1(3) . . ? 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 C10 C1 C2 C3 -0.1(4) . . . . ? C11 C1 C2 C3 -176.4(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C2 C3 C4 C5 0.6(5) . . . . ? C3 C4 C5 C10 -1.7(4) . . . . ? C3 C4 C5 C6 177.7(3) . . . . ? C10 C5 C6 C7 -1.7(4) . . . . ? C4 C5 C6 C7 178.9(3) . . . . ? C5 C6 C7 C8 1.1(5) . . . . ? C6 C7 C8 C9 0.7(5) . . . . ? C7 C8 C9 C10 -1.7(4) . . . . ? C7 C8 C9 C12 175.8(3) . . . . ? C8 C9 C10 C5 1.0(4) . . . . ? C12 C9 C10 C5 -177.1(2) . . . . ? C8 C9 C10 C1 179.3(2) . . . . ? C12 C9 C10 C1 1.3(3) . . . . ? C6 C5 C10 C9 0.7(4) . . . . ? C4 C5 C10 C9 -179.8(2) . . . . ? C6 C5 C10 C1 -177.5(3) . . . . ? C4 C5 C10 C1 2.0(4) . . . . ? C2 C1 C10 C9 -179.4(2) . . . . ? C11 C1 C10 C9 -2.2(3) . . . . ? C2 C1 C10 C5 -1.1(4) . . . . ? C11 C1 C10 C5 176.1(2) . . . . ? C13 N1 C11 C1 -6.3(4) . . . . ? C13 N1 C11 C12 179.7(2) . . . . ? C2 C1 C11 N1 4.1(5) . . . . ? C10 C1 C11 N1 -172.5(3) . . . . ? C2 C1 C11 C12 178.7(3) . . . . ? C10 C1 C11 C12 2.1(3) . . . . ? C8 C9 C12 O1 1.5(5) . . . . ? C10 C9 C12 O1 179.2(3) . . . . ? C8 C9 C12 C11 -177.5(3) . . . . ? C10 C9 C12 C11 0.2(3) . . . . ? N1 C11 C12 O1 -5.0(4) . . . . ? C1 C11 C12 O1 179.5(3) . . . . ? N1 C11 C12 C9 174.0(2) . . . . ? C1 C11 C12 C9 -1.4(3) . . . . ? C11 N1 C13 C14 102.5(3) . . . . ? C11 N1 C13 C18 -82.0(3) . . . . ? C18 C13 C14 C15 0.7(4) . . . . ? N1 C13 C14 C15 176.2(2) . . . . ? C18 C13 C14 S1 -177.08(18) . . . . ? N1 C13 C14 S1 -1.6(3) . . . . ? C19 S1 C14 C15 106.6(2) . . . . ? C19 S1 C14 C13 -75.6(2) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? S1 C14 C15 C16 177.3(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C18 0.3(4) . . . . ? C16 C17 C18 C13 -0.1(4) . . . . ? C14 C13 C18 C17 -0.4(4) . . . . ? N1 C13 C18 C17 -175.9(2) . . . . ? C14 S1 C19 C24 119.7(2) . . . . ? C14 S1 C19 C20 -62.4(3) . . . . ? C24 C19 C20 C21 -1.6(5) . . . . ? S1 C19 C20 C21 -179.5(2) . . . . ? C19 C20 C21 C22 0.8(5) . . . . ? C20 C21 C22 C23 0.1(6) . . . . ? C21 C22 C23 C24 -0.1(5) . . . . ? C20 C19 C24 C23 1.6(5) . . . . ? S1 C19 C24 C23 179.5(2) . . . . ? C22 C23 C24 C19 -0.7(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.153 _refine_diff_density_min -0.174 _refine_diff_density_rms 0.039 #===END data_(3a)FeCl _database_code_depnum_ccdc_archive 'CCDC 636868' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040023 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H33 Cl2 Fe N3' _chemical_formula_weight 538.32 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' 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.336(2) _cell_length_b 12.5150(8) _cell_length_c 23.120(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2701.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.56 _cell_measurement_theta_max 14.50 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue-green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1128 _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7463 _exptl_absorpt_correction_T_max 0.8728 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6489 _diffrn_reflns_av_R_equivalents 0.0269 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 27.05 _reflns_number_total 5874 _reflns_number_gt 4548 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0374P)^2^+0.4380P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 5874 _refine_ls_number_parameters 313 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0674 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.0941 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _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 Fe1 Fe 0.67544(5) 0.98765(3) 0.233431(19) 0.03550(12) Uani 1 1 d . . . Cl1 Cl 0.88969(11) 0.90562(8) 0.20952(5) 0.0613(3) Uani 1 1 d . . . Cl2 Cl 0.52019(10) 0.85293(7) 0.25567(4) 0.0573(3) Uani 1 1 d . . . N1 N 0.7473(3) 1.1480(2) 0.22060(11) 0.0357(6) Uani 1 1 d . . . N2 N 0.7234(3) 1.0480(2) 0.32047(12) 0.0434(7) Uani 1 1 d . . . N3 N 0.5649(3) 1.04015(19) 0.15623(10) 0.0339(6) Uani 1 1 d . . . C1 C 0.5669(4) 1.2003(3) 0.08804(14) 0.0401(8) Uani 1 1 d . . . C2 C 0.4763(5) 1.1913(3) 0.04196(16) 0.0559(11) Uani 1 1 d . . . H2A H 0.4201 1.1306 0.0370 0.067 Uiso 1 1 calc R . . C3 C 0.4700(6) 1.2762(4) 0.00208(18) 0.0726(14) Uani 1 1 d . . . H3A H 0.4090 1.2704 -0.0296 0.087 Uiso 1 1 calc R . . C4 C 0.5504(5) 1.3671(3) 0.00820(16) 0.0618(12) Uani 1 1 d . . . H4A H 0.5419 1.4217 -0.0189 0.074 Uiso 1 1 calc R . . C5 C 0.6464(4) 1.3790(3) 0.05514(14) 0.0445(9) Uani 1 1 d . . . C6 C 0.7379(4) 1.4663(3) 0.06692(17) 0.0539(10) Uani 1 1 d . . . H6A H 0.7401 1.5242 0.0417 0.065 Uiso 1 1 calc R . . C7 C 0.8225(5) 1.4665(3) 0.11449(16) 0.0537(9) Uani 1 1 d . . . H7A H 0.8808 1.5254 0.1213 0.064 Uiso 1 1 calc R . . C8 C 0.8255(4) 1.3807(2) 0.15426(15) 0.0443(8) Uani 1 1 d . . . H8A H 0.8853 1.3825 0.1864 0.053 Uiso 1 1 calc R . . C9 C 0.7380(3) 1.2948(2) 0.14421(14) 0.0327(7) Uani 1 1 d . . . C10 C 0.6498(4) 1.2942(2) 0.09446(13) 0.0356(8) Uani 1 1 d . . . C11 C 0.7104(3) 1.1923(2) 0.17358(14) 0.0321(7) Uani 1 1 d . . . C12 C 0.6059(4) 1.1333(2) 0.13741(13) 0.0349(7) Uani 1 1 d . . . C13 C 0.8264(4) 1.2008(2) 0.26583(15) 0.0446(7) Uani 1 1 d . . . H13A H 0.7729 1.2617 0.2803 0.053 Uiso 1 1 calc R . . H13B H 0.9177 1.2260 0.2512 0.053 Uiso 1 1 calc R . . C14 C 0.8496(4) 1.1193(3) 0.31405(15) 0.0505(9) Uani 1 1 d . . . H14A H 0.9337 1.0767 0.3054 0.061 Uiso 1 1 calc R . . H14B H 0.8666 1.1565 0.3502 0.061 Uiso 1 1 calc R . . C15 C 0.5972(5) 1.1052(3) 0.34260(17) 0.0624(11) Uani 1 1 d . . . H15A H 0.6176 1.1328 0.3805 0.094 Uiso 1 1 calc R . . H15B H 0.5174 1.0569 0.3448 0.094 Uiso 1 1 calc R . . H15C H 0.5741 1.1631 0.3171 0.094 Uiso 1 1 calc R . . C16 C 0.7601(5) 0.9593(3) 0.36013(17) 0.0660(12) Uani 1 1 d . . . H16A H 0.7810 0.9876 0.3978 0.099 Uiso 1 1 calc R . . H16B H 0.8425 0.9221 0.3456 0.099 Uiso 1 1 calc R . . H16C H 0.6807 0.9108 0.3627 0.099 Uiso 1 1 calc R . . C17 C 0.4527(4) 0.9844(3) 0.12641(12) 0.0367(7) Uani 1 1 d . . . C18 C 0.4905(4) 0.9007(3) 0.08930(14) 0.0442(9) Uani 1 1 d . . . C19 C 0.3795(6) 0.8441(3) 0.06387(16) 0.0563(11) Uani 1 1 d . . . H19A H 0.4011 0.7895 0.0380 0.068 Uiso 1 1 calc R . . C20 C 0.2390(5) 0.8663(3) 0.07580(17) 0.0599(12) Uani 1 1 d . . . H20A H 0.1668 0.8255 0.0591 0.072 Uiso 1 1 calc R . . C21 C 0.2047(4) 0.9487(3) 0.11254(16) 0.0516(10) Uani 1 1 d . . . H21A H 0.1089 0.9627 0.1206 0.062 Uiso 1 1 calc R . . C22 C 0.3095(4) 1.0115(3) 0.13785(13) 0.0405(7) Uani 1 1 d . . . C23 C 0.2702(4) 1.1061(3) 0.17647(16) 0.0460(9) Uani 1 1 d . . . H23A H 0.3530 1.1541 0.1778 0.055 Uiso 1 1 calc R . . C24 C 0.1427(6) 1.1701(3) 0.1540(2) 0.0772(14) Uani 1 1 d . . . H24A H 0.1228 1.2280 0.1800 0.116 Uiso 1 1 calc R . . H24B H 0.0603 1.1244 0.1514 0.116 Uiso 1 1 calc R . . H24C H 0.1648 1.1982 0.1164 0.116 Uiso 1 1 calc R . . C25 C 0.2388(5) 1.0707(3) 0.23755(18) 0.0686(12) Uani 1 1 d . . . H25A H 0.2242 1.1323 0.2616 0.103 Uiso 1 1 calc R . . H25B H 0.3183 1.0300 0.2521 0.103 Uiso 1 1 calc R . . H25C H 0.1541 1.0272 0.2379 0.103 Uiso 1 1 calc R . . C26 C 0.6469(5) 0.8769(3) 0.07666(17) 0.0579(11) Uani 1 1 d . . . H26A H 0.7046 0.9183 0.1041 0.069 Uiso 1 1 calc R . . C27 C 0.6884(7) 0.9131(4) 0.0157(2) 0.110(2) Uani 1 1 d . . . H27A H 0.6721 0.9885 0.0120 0.166 Uiso 1 1 calc R . . H27B H 0.6312 0.8755 -0.0122 0.166 Uiso 1 1 calc R . . H27C H 0.7878 0.8978 0.0091 0.166 Uiso 1 1 calc R . . C28 C 0.6847(6) 0.7586(3) 0.0852(2) 0.0798(14) Uani 1 1 d . . . H28A H 0.6663 0.7384 0.1245 0.120 Uiso 1 1 calc R . . H28B H 0.7842 0.7476 0.0765 0.120 Uiso 1 1 calc R . . H28C H 0.6273 0.7156 0.0597 0.120 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 Fe1 0.0385(2) 0.0295(2) 0.0385(2) 0.0007(2) 0.0004(2) -0.0014(2) Cl1 0.0468(5) 0.0552(6) 0.0817(7) -0.0034(5) 0.0097(5) 0.0123(5) Cl2 0.0560(6) 0.0479(5) 0.0679(6) 0.0142(4) 0.0039(5) -0.0138(4) N1 0.0375(15) 0.0327(13) 0.0369(16) -0.0014(12) -0.0013(12) -0.0008(12) N2 0.0514(18) 0.0397(15) 0.0390(15) -0.0020(12) -0.0003(14) 0.0004(13) N3 0.0385(15) 0.0301(14) 0.0330(14) -0.0036(11) 0.0046(12) -0.0046(12) C1 0.051(2) 0.0354(17) 0.0343(17) 0.0021(14) -0.0002(16) -0.0086(16) C2 0.069(3) 0.052(2) 0.047(2) 0.0079(18) -0.014(2) -0.020(2) C3 0.096(4) 0.076(3) 0.045(2) 0.019(2) -0.022(2) -0.032(3) C4 0.087(3) 0.052(2) 0.046(2) 0.0181(19) -0.009(2) -0.014(2) C5 0.058(3) 0.0344(17) 0.0407(19) 0.0046(14) 0.0028(17) -0.0050(17) C6 0.069(3) 0.0311(19) 0.062(2) 0.0141(17) 0.005(2) -0.0039(19) C7 0.064(2) 0.0331(18) 0.064(2) 0.0034(16) -0.005(2) -0.012(2) C8 0.045(2) 0.0373(17) 0.050(2) -0.0026(15) -0.0016(18) -0.0060(18) C9 0.0358(18) 0.0239(15) 0.0386(17) -0.0022(13) 0.0068(14) 0.0011(13) C10 0.041(2) 0.0306(15) 0.0350(17) 0.0009(13) 0.0065(15) -0.0015(15) C11 0.0312(18) 0.0286(15) 0.0366(17) -0.0011(13) 0.0062(13) -0.0020(13) C12 0.0396(18) 0.0303(16) 0.0348(17) -0.0045(13) 0.0070(14) -0.0041(15) C13 0.0449(18) 0.0409(16) 0.0479(18) -0.0010(16) -0.010(2) -0.0063(17) C14 0.055(2) 0.051(2) 0.045(2) -0.0025(16) -0.0152(18) -0.0021(19) C15 0.064(3) 0.064(3) 0.060(3) -0.018(2) 0.015(2) 0.008(2) C16 0.095(3) 0.058(3) 0.045(2) 0.0122(18) -0.015(2) -0.001(2) C17 0.051(2) 0.0291(16) 0.0295(15) 0.0031(14) -0.0026(14) -0.0101(16) C18 0.070(3) 0.0317(17) 0.0307(17) -0.0002(14) 0.0062(17) -0.0072(18) C19 0.096(3) 0.0316(19) 0.041(2) -0.0040(16) -0.008(2) -0.015(2) C20 0.078(3) 0.047(2) 0.055(2) 0.001(2) -0.025(2) -0.025(2) C21 0.053(3) 0.045(2) 0.056(2) 0.0069(17) -0.0094(19) -0.0111(19) C22 0.048(2) 0.0343(16) 0.0391(16) 0.0004(14) -0.0044(15) -0.0083(18) C23 0.042(2) 0.0423(19) 0.054(2) -0.0067(17) -0.0014(17) -0.0070(17) C24 0.098(4) 0.055(3) 0.078(3) 0.007(2) -0.004(3) 0.018(3) C25 0.081(3) 0.072(3) 0.053(2) -0.007(2) 0.004(2) 0.015(2) C26 0.079(3) 0.040(2) 0.055(2) -0.0137(17) 0.019(2) -0.003(2) C27 0.155(6) 0.079(3) 0.098(4) 0.010(3) 0.072(4) 0.004(4) C28 0.094(4) 0.056(3) 0.090(3) 0.002(2) 0.019(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.137(3) . ? Fe1 N3 2.164(3) . ? Fe1 N2 2.195(3) . ? Fe1 Cl2 2.2821(10) . ? Fe1 Cl1 2.3153(11) . ? N1 C11 1.268(4) . ? N1 C13 1.441(4) . ? N2 C15 1.470(4) . ? N2 C16 1.480(4) . ? N2 C14 1.486(4) . ? N3 C12 1.302(4) . ? N3 C17 1.435(4) . ? C1 C2 1.365(5) . ? C1 C10 1.415(4) . ? C1 C12 1.462(5) . ? C2 C3 1.408(5) . ? C3 C4 1.371(6) . ? C4 C5 1.415(5) . ? C5 C10 1.398(4) . ? C5 C6 1.413(5) . ? C6 C7 1.354(5) . ? C7 C8 1.414(5) . ? C8 C9 1.370(4) . ? C9 C10 1.414(5) . ? C9 C11 1.473(4) . ? C11 C12 1.482(4) . ? C13 C14 1.527(4) . ? C17 C18 1.400(4) . ? C17 C22 1.404(5) . ? C18 C19 1.386(5) . ? C18 C26 1.518(6) . ? C19 C20 1.369(6) . ? C20 C21 1.375(5) . ? C21 C22 1.384(5) . ? C22 C23 1.528(5) . ? C23 C25 1.509(5) . ? C23 C24 1.526(5) . ? C26 C27 1.529(6) . ? C26 C28 1.536(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N3 75.53(9) . . ? N1 Fe1 N2 74.95(10) . . ? N3 Fe1 N2 138.49(10) . . ? N1 Fe1 Cl2 157.62(8) . . ? N3 Fe1 Cl2 96.15(7) . . ? N2 Fe1 Cl2 100.20(8) . . ? N1 Fe1 Cl1 96.43(8) . . ? N3 Fe1 Cl1 110.48(7) . . ? N2 Fe1 Cl1 101.26(8) . . ? Cl2 Fe1 Cl1 105.96(4) . . ? C11 N1 C13 124.1(3) . . ? C11 N1 Fe1 116.4(2) . . ? C13 N1 Fe1 119.42(19) . . ? C15 N2 C16 109.6(3) . . ? C15 N2 C14 112.2(3) . . ? C16 N2 C14 109.2(3) . . ? C15 N2 Fe1 108.9(2) . . ? C16 N2 Fe1 110.9(2) . . ? C14 N2 Fe1 106.1(2) . . ? C12 N3 C17 119.3(3) . . ? C12 N3 Fe1 114.0(2) . . ? C17 N3 Fe1 126.65(19) . . ? C2 C1 C10 119.3(3) . . ? C2 C1 C12 135.8(3) . . ? C10 C1 C12 105.0(3) . . ? C1 C2 C3 118.4(4) . . ? C4 C3 C2 122.4(4) . . ? C3 C4 C5 120.9(3) . . ? C10 C5 C6 116.6(3) . . ? C10 C5 C4 115.7(3) . . ? C6 C5 C4 127.7(3) . . ? C7 C6 C5 120.7(3) . . ? C6 C7 C8 122.6(3) . . ? C9 C8 C7 118.3(3) . . ? C8 C9 C10 119.3(3) . . ? C8 C9 C11 135.1(3) . . ? C10 C9 C11 105.6(3) . . ? C5 C10 C9 122.6(3) . . ? C5 C10 C1 123.4(3) . . ? C9 C10 C1 114.0(3) . . ? N1 C11 C9 136.8(3) . . ? N1 C11 C12 116.4(3) . . ? C9 C11 C12 106.8(3) . . ? N3 C12 C1 134.5(3) . . ? N3 C12 C11 116.8(3) . . ? C1 C12 C11 108.6(3) . . ? N1 C13 C14 107.2(2) . . ? N2 C14 C13 111.2(3) . . ? C18 C17 C22 122.4(3) . . ? C18 C17 N3 118.3(3) . . ? C22 C17 N3 119.2(3) . . ? C19 C18 C17 117.0(4) . . ? C19 C18 C26 122.5(3) . . ? C17 C18 C26 120.5(3) . . ? C20 C19 C18 121.8(4) . . ? C19 C20 C21 120.0(4) . . ? C20 C21 C22 121.5(4) . . ? C21 C22 C17 117.2(3) . . ? C21 C22 C23 121.1(3) . . ? C17 C22 C23 121.7(3) . . ? C25 C23 C24 108.8(3) . . ? C25 C23 C22 111.5(3) . . ? C24 C23 C22 113.3(3) . . ? C18 C26 C27 111.3(4) . . ? C18 C26 C28 112.7(4) . . ? C27 C26 C28 110.2(4) . . ? 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 N3 Fe1 N1 C11 -8.2(2) . . . . ? N2 Fe1 N1 C11 -158.7(3) . . . . ? Cl2 Fe1 N1 C11 -78.6(3) . . . . ? Cl1 Fe1 N1 C11 101.3(2) . . . . ? N3 Fe1 N1 C13 168.5(3) . . . . ? N2 Fe1 N1 C13 18.0(2) . . . . ? Cl2 Fe1 N1 C13 98.1(3) . . . . ? Cl1 Fe1 N1 C13 -82.0(2) . . . . ? N1 Fe1 N2 C15 85.4(2) . . . . ? N3 Fe1 N2 C15 39.4(3) . . . . ? Cl2 Fe1 N2 C15 -72.2(2) . . . . ? Cl1 Fe1 N2 C15 179.1(2) . . . . ? N1 Fe1 N2 C16 -153.9(3) . . . . ? N3 Fe1 N2 C16 160.0(2) . . . . ? Cl2 Fe1 N2 C16 48.5(3) . . . . ? Cl1 Fe1 N2 C16 -60.2(3) . . . . ? N1 Fe1 N2 C14 -35.5(2) . . . . ? N3 Fe1 N2 C14 -81.5(2) . . . . ? Cl2 Fe1 N2 C14 166.90(19) . . . . ? Cl1 Fe1 N2 C14 58.2(2) . . . . ? N1 Fe1 N3 C12 6.9(2) . . . . ? N2 Fe1 N3 C12 52.7(3) . . . . ? Cl2 Fe1 N3 C12 165.7(2) . . . . ? Cl1 Fe1 N3 C12 -84.7(2) . . . . ? N1 Fe1 N3 C17 -171.5(3) . . . . ? N2 Fe1 N3 C17 -125.6(2) . . . . ? Cl2 Fe1 N3 C17 -12.6(2) . . . . ? Cl1 Fe1 N3 C17 97.0(2) . . . . ? C10 C1 C2 C3 0.6(6) . . . . ? C12 C1 C2 C3 -179.4(4) . . . . ? C1 C2 C3 C4 -0.5(7) . . . . ? C2 C3 C4 C5 1.0(7) . . . . ? C3 C4 C5 C10 -1.5(6) . . . . ? C3 C4 C5 C6 178.8(4) . . . . ? C10 C5 C6 C7 -0.7(6) . . . . ? C4 C5 C6 C7 178.9(4) . . . . ? C5 C6 C7 C8 0.6(6) . . . . ? C6 C7 C8 C9 -0.7(6) . . . . ? C7 C8 C9 C10 0.8(5) . . . . ? C7 C8 C9 C11 179.4(3) . . . . ? C6 C5 C10 C9 0.9(5) . . . . ? C4 C5 C10 C9 -178.8(3) . . . . ? C6 C5 C10 C1 -178.6(3) . . . . ? C4 C5 C10 C1 1.7(5) . . . . ? C8 C9 C10 C5 -1.0(5) . . . . ? C11 C9 C10 C5 -179.9(3) . . . . ? C8 C9 C10 C1 178.6(3) . . . . ? C11 C9 C10 C1 -0.4(4) . . . . ? C2 C1 C10 C5 -1.3(5) . . . . ? C12 C1 C10 C5 178.7(3) . . . . ? C2 C1 C10 C9 179.2(3) . . . . ? C12 C1 C10 C9 -0.8(4) . . . . ? C13 N1 C11 C9 7.6(6) . . . . ? Fe1 N1 C11 C9 -175.9(3) . . . . ? C13 N1 C11 C12 -168.3(3) . . . . ? Fe1 N1 C11 C12 8.3(4) . . . . ? C8 C9 C11 N1 6.6(7) . . . . ? C10 C9 C11 N1 -174.7(4) . . . . ? C8 C9 C11 C12 -177.3(4) . . . . ? C10 C9 C11 C12 1.4(3) . . . . ? C17 N3 C12 C1 -2.8(5) . . . . ? Fe1 N3 C12 C1 178.8(3) . . . . ? C17 N3 C12 C11 173.4(3) . . . . ? Fe1 N3 C12 C11 -5.1(3) . . . . ? C2 C1 C12 N3 -1.9(7) . . . . ? C10 C1 C12 N3 178.0(4) . . . . ? C2 C1 C12 C11 -178.3(4) . . . . ? C10 C1 C12 C11 1.7(4) . . . . ? N1 C11 C12 N3 -2.0(4) . . . . ? C9 C11 C12 N3 -179.0(3) . . . . ? N1 C11 C12 C1 175.1(3) . . . . ? C9 C11 C12 C1 -1.9(3) . . . . ? C11 N1 C13 C14 -179.4(3) . . . . ? Fe1 N1 C13 C14 4.1(4) . . . . ? C15 N2 C14 C13 -68.1(4) . . . . ? C16 N2 C14 C13 170.2(3) . . . . ? Fe1 N2 C14 C13 50.6(3) . . . . ? N1 C13 C14 N2 -36.4(4) . . . . ? C12 N3 C17 C18 102.0(4) . . . . ? Fe1 N3 C17 C18 -79.8(3) . . . . ? C12 N3 C17 C22 -81.6(4) . . . . ? Fe1 N3 C17 C22 96.6(3) . . . . ? C22 C17 C18 C19 -0.2(5) . . . . ? N3 C17 C18 C19 176.1(3) . . . . ? C22 C17 C18 C26 177.9(3) . . . . ? N3 C17 C18 C26 -5.8(5) . . . . ? C17 C18 C19 C20 -2.1(5) . . . . ? C26 C18 C19 C20 179.8(4) . . . . ? C18 C19 C20 C21 2.0(6) . . . . ? C19 C20 C21 C22 0.5(6) . . . . ? C20 C21 C22 C17 -2.7(5) . . . . ? C20 C21 C22 C23 177.2(3) . . . . ? C18 C17 C22 C21 2.5(5) . . . . ? N3 C17 C22 C21 -173.8(3) . . . . ? C18 C17 C22 C23 -177.4(3) . . . . ? N3 C17 C22 C23 6.3(5) . . . . ? C21 C22 C23 C25 83.0(4) . . . . ? C17 C22 C23 C25 -97.1(4) . . . . ? C21 C22 C23 C24 -40.1(5) . . . . ? C17 C22 C23 C24 139.8(3) . . . . ? C19 C18 C26 C27 71.8(5) . . . . ? C17 C18 C26 C27 -106.1(4) . . . . ? C19 C18 C26 C28 -52.5(5) . . . . ? C17 C18 C26 C28 129.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.05 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.251 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.047 #===END data_(2c)FeCl2_0.5MeCN _database_code_depnum_ccdc_archive 'CCDC 636869' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040026 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H24.50 Cl2 Fe N3.50' _chemical_formula_weight 536.76 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' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.348(2) _cell_length_b 15.047(3) _cell_length_c 16.062(3) _cell_angle_alpha 85.13(5) _cell_angle_beta 77.33(4) _cell_angle_gamma 76.89(6) _cell_volume 2604.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.12 _cell_measurement_theta_max 14.66 _exptl_crystal_description Prism _exptl_crystal_colour Blue-green _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.369 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.807 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 9637 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 24.99 _reflns_number_total 9134 _reflns_number_gt 6314 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0711P)^2^+2.7599P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9134 _refine_ls_number_parameters 623 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1584 _refine_ls_wR_factor_gt 0.1322 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 Fe1 Fe 0.63467(6) 0.71559(4) 0.36298(3) 0.04957(18) Uani 1 1 d . . . Cl1 Cl 0.60405(12) 0.57906(9) 0.32186(7) 0.0652(3) Uani 1 1 d . . . Cl2 Cl 0.59280(12) 0.83366(10) 0.26624(8) 0.0788(4) Uani 1 1 d . . . N1 N 0.7186(3) 0.6653(2) 0.46950(18) 0.0433(8) Uani 1 1 d . . . N2 N 0.8390(3) 0.7123(3) 0.3132(2) 0.0538(9) Uani 1 1 d . . . N3 N 0.4638(3) 0.7603(3) 0.4602(2) 0.0549(9) Uani 1 1 d . . . C1 C 0.9297(4) 0.6258(3) 0.5104(2) 0.0446(9) Uani 1 1 d . . . C2 C 0.9273(4) 0.5976(3) 0.5942(3) 0.0533(11) Uani 1 1 d . . . H2A H 0.8530 0.5956 0.6320 0.064 Uiso 1 1 calc R . . C3 C 1.0422(5) 0.5714(3) 0.6215(3) 0.0644(13) Uani 1 1 d . . . H3A H 1.0414 0.5518 0.6781 0.077 Uiso 1 1 calc R . . C4 C 1.1535(5) 0.5739(3) 0.5682(3) 0.0623(12) Uani 1 1 d . . . H4A H 1.2261 0.5553 0.5888 0.075 Uiso 1 1 calc R . . C5 C 1.1587(4) 0.6044(3) 0.4823(3) 0.0543(11) Uani 1 1 d . . . C6 C 1.2655(4) 0.6106(3) 0.4198(3) 0.0639(12) Uani 1 1 d . . . H6A H 1.3427 0.5946 0.4343 0.077 Uiso 1 1 calc R . . C7 C 1.2563(4) 0.6401(3) 0.3379(3) 0.0652(13) Uani 1 1 d . . . H7A H 1.3282 0.6435 0.2979 0.078 Uiso 1 1 calc R . . C8 C 1.1426(4) 0.6653(3) 0.3122(3) 0.0609(12) Uani 1 1 d . . . H8A H 1.1394 0.6845 0.2560 0.073 Uiso 1 1 calc R . . C9 C 1.0356(4) 0.6611(3) 0.3713(2) 0.0453(9) Uani 1 1 d . . . C10 C 1.0448(4) 0.6297(3) 0.4558(3) 0.0447(9) Uani 1 1 d . . . C11 C 0.8368(4) 0.6559(3) 0.4573(2) 0.0416(9) Uani 1 1 d . . . C12 C 0.9034(4) 0.6804(3) 0.3699(2) 0.0476(10) Uani 1 1 d . . . C13 C 0.6519(4) 0.6399(3) 0.5537(2) 0.0486(10) Uani 1 1 d . . . H13A H 0.6439 0.6872 0.5933 0.058 Uiso 1 1 calc R . . H13B H 0.6989 0.5836 0.5748 0.058 Uiso 1 1 calc R . . C14 C 0.5244(4) 0.6269(3) 0.5503(3) 0.0516(10) Uani 1 1 d . . . H14A H 0.5322 0.5858 0.5050 0.062 Uiso 1 1 calc R . . H14B H 0.4902 0.5983 0.6037 0.062 Uiso 1 1 calc R . . C15 C 0.4370(4) 0.7139(3) 0.5351(3) 0.0518(10) Uani 1 1 d . . . C16 C 0.3325(5) 0.7471(4) 0.5956(3) 0.0693(14) Uani 1 1 d . . . H16A H 0.3154 0.7150 0.6473 0.083 Uiso 1 1 calc R . . C17 C 0.2540(5) 0.8272(4) 0.5795(4) 0.0811(16) Uani 1 1 d . . . H17A H 0.1837 0.8497 0.6203 0.097 Uiso 1 1 calc R . . C18 C 0.2795(5) 0.8740(4) 0.5034(4) 0.0788(15) Uani 1 1 d . . . H18A H 0.2267 0.9279 0.4906 0.095 Uiso 1 1 calc R . . C19 C 0.3863(5) 0.8384(4) 0.4462(3) 0.0706(14) Uani 1 1 d . . . H19A H 0.4054 0.8708 0.3949 0.085 Uiso 1 1 calc R . . C20 C 0.8959(4) 0.7424(4) 0.2299(3) 0.0602(12) Uani 1 1 d . . . C21 C 0.9263(4) 0.6828(4) 0.1629(3) 0.0692(14) Uani 1 1 d . . . C22 C 0.9704(5) 0.7174(5) 0.0815(3) 0.0902(19) Uani 1 1 d . . . H22A H 0.9906 0.6796 0.0352 0.108 Uiso 1 1 calc R . . C23 C 0.9845(5) 0.8051(6) 0.0683(4) 0.103(2) Uani 1 1 d . . . H23A H 1.0135 0.8266 0.0133 0.123 Uiso 1 1 calc R . . C24 C 0.9564(5) 0.8623(5) 0.1353(4) 0.0911(19) Uani 1 1 d . . . H24A H 0.9667 0.9222 0.1254 0.109 Uiso 1 1 calc R . . C25 C 0.9124(5) 0.8314(4) 0.2185(3) 0.0716(14) Uani 1 1 d . . . C26 C 0.9133(6) 0.5864(4) 0.1766(3) 0.0889(18) Uani 1 1 d . . . H26A H 0.8837 0.5742 0.2363 0.133 Uiso 1 1 calc R . . H26B H 0.9921 0.5466 0.1576 0.133 Uiso 1 1 calc R . . H26C H 0.8554 0.5762 0.1448 0.133 Uiso 1 1 calc R . . C27 C 0.8814(6) 0.8944(4) 0.2911(4) 0.0965(19) Uani 1 1 d . . . H27A H 0.8546 0.8622 0.3435 0.145 Uiso 1 1 calc R . . H27B H 0.8163 0.9451 0.2819 0.145 Uiso 1 1 calc R . . H27C H 0.9532 0.9164 0.2943 0.145 Uiso 1 1 calc R . . Fe2 Fe 0.62779(6) 0.70498(4) -0.12975(4) 0.05368(19) Uani 1 1 d . . . Cl3 Cl 0.82216(14) 0.61166(10) -0.14317(11) 0.0975(5) Uani 1 1 d . . . Cl4 Cl 0.53833(18) 0.66127(11) -0.23228(8) 0.0996(6) Uani 1 1 d . . . N4 N 0.6414(3) 0.7948(2) -0.0361(2) 0.0496(8) Uani 1 1 d . . . N5 N 0.6588(3) 0.8325(2) -0.2043(2) 0.0520(9) Uani 1 1 d . . . N6 N 0.5074(3) 0.6509(2) -0.0201(2) 0.0505(9) Uani 1 1 d . . . C30 C 0.6752(4) 0.9544(3) -0.0263(3) 0.0511(10) Uani 1 1 d . . . C31 C 0.6811(5) 0.9762(4) 0.0546(3) 0.0660(13) Uani 1 1 d . . . H31A H 0.6684 0.9357 0.1011 0.079 Uiso 1 1 calc R . . C32 C 0.7068(5) 1.0614(4) 0.0641(3) 0.0790(16) Uani 1 1 d . . . H32A H 0.7133 1.0759 0.1179 0.095 Uiso 1 1 calc R . . C33 C 0.7227(5) 1.1235(4) -0.0014(4) 0.0776(15) Uani 1 1 d . . . H33A H 0.7373 1.1796 0.0088 0.093 Uiso 1 1 calc R . . C34 C 0.7174(4) 1.1042(3) -0.0848(3) 0.0615(12) Uani 1 1 d . . . C35 C 0.7326(5) 1.1603(3) -0.1590(4) 0.0730(14) Uani 1 1 d . . . H35A H 0.7455 1.2187 -0.1556 0.088 Uiso 1 1 calc R . . C36 C 0.7288(5) 1.1304(3) -0.2366(4) 0.0786(16) Uani 1 1 d . . . H36A H 0.7405 1.1690 -0.2847 0.094 Uiso 1 1 calc R . . C37 C 0.7080(5) 1.0435(3) -0.2460(3) 0.0658(13) Uani 1 1 d . . . H37A H 0.7065 1.0244 -0.2992 0.079 Uiso 1 1 calc R . . C38 C 0.6901(4) 0.9877(3) -0.1744(3) 0.0513(10) Uani 1 1 d . . . C39 C 0.6937(4) 1.0189(3) -0.0947(3) 0.0513(10) Uani 1 1 d . . . C40 C 0.6575(4) 0.8737(3) -0.0636(3) 0.0485(10) Uani 1 1 d . . . C41 C 0.6665(4) 0.8949(3) -0.1575(3) 0.0473(10) Uani 1 1 d . . . C42 C 0.6395(5) 0.7694(3) 0.0548(3) 0.0572(11) Uani 1 1 d . . . H42A H 0.5639 0.8029 0.0894 0.069 Uiso 1 1 calc R . . H42B H 0.7088 0.7859 0.0712 0.069 Uiso 1 1 calc R . . C43 C 0.6469(5) 0.6681(3) 0.0715(3) 0.0620(12) Uani 1 1 d . . . H43A H 0.7201 0.6352 0.0341 0.074 Uiso 1 1 calc R . . H43B H 0.6563 0.6525 0.1298 0.074 Uiso 1 1 calc R . . C44 C 0.5362(4) 0.6366(3) 0.0580(3) 0.0518(10) Uani 1 1 d . . . C45 C 0.4663(5) 0.5933(3) 0.1238(3) 0.0648(13) Uani 1 1 d . . . H45A H 0.4888 0.5822 0.1767 0.078 Uiso 1 1 calc R . . C46 C 0.3634(5) 0.5666(3) 0.1109(3) 0.0697(14) Uani 1 1 d . . . H46A H 0.3157 0.5378 0.1548 0.084 Uiso 1 1 calc R . . C47 C 0.3328(5) 0.5832(3) 0.0327(3) 0.0694(14) Uani 1 1 d . . . H47A H 0.2631 0.5667 0.0227 0.083 Uiso 1 1 calc R . . C48 C 0.4064(5) 0.6247(3) -0.0311(3) 0.0616(12) Uani 1 1 d . . . H48A H 0.3853 0.6350 -0.0844 0.074 Uiso 1 1 calc R . . C49 C 0.6763(5) 0.8509(3) -0.2957(3) 0.0568(12) Uani 1 1 d . . . C50 C 0.7947(5) 0.8339(3) -0.3438(3) 0.0713(15) Uani 1 1 d . . . C51 C 0.8090(8) 0.8519(4) -0.4329(4) 0.096(2) Uani 1 1 d . . . H51A H 0.8876 0.8423 -0.4677 0.115 Uiso 1 1 calc R . . C52 C 0.7059(9) 0.8838(4) -0.4681(4) 0.107(3) Uani 1 1 d . . . H52A H 0.7161 0.8942 -0.5269 0.128 Uiso 1 1 calc R . . C53 C 0.5907(8) 0.9003(4) -0.4193(4) 0.092(2) Uani 1 1 d . . . H53A H 0.5231 0.9226 -0.4447 0.110 Uiso 1 1 calc R . . C54 C 0.5722(6) 0.8844(3) -0.3320(3) 0.0682(14) Uani 1 1 d . . . C55 C 0.9041(6) 0.8028(4) -0.3033(4) 0.098(2) Uani 1 1 d . . . H55A H 0.8766 0.7940 -0.2428 0.147 Uiso 1 1 calc R . . H55B H 0.9536 0.8480 -0.3140 0.147 Uiso 1 1 calc R . . H55C H 0.9524 0.7462 -0.3269 0.147 Uiso 1 1 calc R . . C56 C 0.4450(6) 0.9061(4) -0.2788(4) 0.0885(17) Uani 1 1 d . . . H56A H 0.3868 0.9280 -0.3150 0.133 Uiso 1 1 calc R . . H56B H 0.4399 0.9523 -0.2396 0.133 Uiso 1 1 calc R . . H56C H 0.4264 0.8521 -0.2474 0.133 Uiso 1 1 calc R . . N1S N 0.8553(13) 0.1864(10) 0.1744(7) 0.221(6) Uani 1 1 d . . . C1S C 0.8483(10) 0.2672(12) 0.1745(6) 0.160(5) Uani 1 1 d . . . C2S C 0.8361(15) 0.3628(10) 0.1780(7) 0.257(9) Uani 1 1 d . . . H1SA H 0.7524 0.3903 0.2035 0.385 Uiso 1 1 calc R . . H2SA H 0.8568 0.3883 0.1212 0.385 Uiso 1 1 calc R . . H3SA H 0.8908 0.3746 0.2115 0.385 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 Fe1 0.0498(4) 0.0660(4) 0.0317(3) 0.0072(3) -0.0095(3) -0.0121(3) Cl1 0.0725(8) 0.0785(8) 0.0503(6) -0.0033(6) -0.0164(6) -0.0235(6) Cl2 0.0691(8) 0.0924(9) 0.0590(7) 0.0312(7) -0.0081(6) -0.0025(7) N1 0.048(2) 0.052(2) 0.0301(16) 0.0059(14) -0.0066(14) -0.0155(16) N2 0.055(2) 0.072(2) 0.0306(17) 0.0125(16) -0.0052(16) -0.0144(19) N3 0.054(2) 0.068(2) 0.0425(19) 0.0025(17) -0.0080(17) -0.0147(19) C1 0.055(3) 0.045(2) 0.038(2) 0.0023(17) -0.0179(18) -0.0128(19) C2 0.064(3) 0.059(3) 0.042(2) 0.0066(19) -0.022(2) -0.017(2) C3 0.091(4) 0.066(3) 0.048(3) 0.013(2) -0.041(3) -0.021(3) C4 0.074(3) 0.058(3) 0.063(3) 0.003(2) -0.038(3) -0.010(2) C5 0.057(3) 0.050(2) 0.062(3) 0.002(2) -0.029(2) -0.010(2) C6 0.053(3) 0.065(3) 0.079(3) -0.002(3) -0.024(3) -0.011(2) C7 0.039(3) 0.081(3) 0.077(3) 0.002(3) -0.011(2) -0.018(2) C8 0.053(3) 0.071(3) 0.055(3) 0.010(2) -0.008(2) -0.016(2) C9 0.035(2) 0.055(2) 0.045(2) 0.0061(18) -0.0117(17) -0.0096(18) C10 0.047(2) 0.043(2) 0.046(2) 0.0016(17) -0.0180(19) -0.0066(18) C11 0.048(3) 0.045(2) 0.0326(19) 0.0055(16) -0.0096(17) -0.0141(18) C12 0.064(3) 0.049(2) 0.0292(19) 0.0081(17) -0.0080(19) -0.014(2) C13 0.058(3) 0.060(3) 0.0279(19) 0.0077(17) -0.0065(18) -0.017(2) C14 0.057(3) 0.063(3) 0.036(2) 0.0039(19) -0.0035(19) -0.023(2) C15 0.052(3) 0.067(3) 0.040(2) -0.001(2) -0.0072(19) -0.024(2) C16 0.067(3) 0.084(4) 0.053(3) -0.004(3) 0.006(2) -0.025(3) C17 0.056(3) 0.098(4) 0.078(4) -0.020(3) 0.009(3) -0.010(3) C18 0.060(3) 0.085(4) 0.078(4) -0.005(3) -0.006(3) 0.004(3) C19 0.069(3) 0.077(3) 0.059(3) 0.006(3) -0.014(3) -0.006(3) C20 0.044(3) 0.088(4) 0.042(2) 0.022(2) -0.0081(19) -0.010(2) C21 0.050(3) 0.099(4) 0.043(3) 0.013(3) -0.005(2) 0.007(3) C22 0.070(4) 0.139(6) 0.043(3) 0.012(3) 0.002(2) -0.001(4) C23 0.069(4) 0.173(7) 0.049(3) 0.046(4) 0.000(3) -0.021(4) C24 0.077(4) 0.123(5) 0.072(4) 0.045(4) -0.012(3) -0.038(4) C25 0.062(3) 0.094(4) 0.057(3) 0.024(3) -0.011(2) -0.023(3) C26 0.082(4) 0.112(5) 0.054(3) -0.003(3) -0.005(3) 0.009(3) C27 0.117(5) 0.089(4) 0.091(4) 0.019(4) -0.021(4) -0.046(4) Fe2 0.0743(5) 0.0513(4) 0.0366(3) 0.0005(3) -0.0042(3) -0.0235(3) Cl3 0.0788(10) 0.0697(9) 0.1205(13) 0.0020(8) 0.0191(9) -0.0078(7) Cl4 0.1758(17) 0.1132(12) 0.0400(6) 0.0106(7) -0.0291(8) -0.0908(12) N4 0.059(2) 0.053(2) 0.0375(18) 0.0012(15) -0.0105(16) -0.0158(17) N5 0.068(2) 0.053(2) 0.0368(18) 0.0034(16) -0.0087(16) -0.0205(18) N6 0.060(2) 0.054(2) 0.0375(18) 0.0027(15) -0.0063(16) -0.0169(18) C30 0.049(3) 0.057(3) 0.050(2) -0.005(2) -0.0103(19) -0.015(2) C31 0.076(3) 0.082(3) 0.046(3) -0.011(2) -0.008(2) -0.029(3) C32 0.099(4) 0.087(4) 0.060(3) -0.022(3) -0.007(3) -0.040(3) C33 0.085(4) 0.069(3) 0.086(4) -0.027(3) -0.011(3) -0.031(3) C34 0.060(3) 0.050(3) 0.077(3) -0.011(2) -0.011(2) -0.017(2) C35 0.085(4) 0.047(3) 0.094(4) 0.002(3) -0.025(3) -0.024(3) C36 0.103(4) 0.056(3) 0.088(4) 0.020(3) -0.036(3) -0.032(3) C37 0.089(4) 0.055(3) 0.061(3) 0.013(2) -0.027(3) -0.026(3) C38 0.056(3) 0.048(2) 0.052(2) 0.0020(19) -0.017(2) -0.011(2) C39 0.047(2) 0.052(2) 0.056(3) -0.005(2) -0.010(2) -0.013(2) C40 0.052(3) 0.053(3) 0.042(2) 0.0002(19) -0.0090(19) -0.015(2) C41 0.056(3) 0.046(2) 0.042(2) -0.0001(18) -0.0112(19) -0.014(2) C42 0.070(3) 0.070(3) 0.039(2) 0.003(2) -0.017(2) -0.028(2) C43 0.072(3) 0.072(3) 0.045(2) 0.016(2) -0.022(2) -0.017(3) C44 0.067(3) 0.047(2) 0.039(2) 0.0059(18) -0.009(2) -0.011(2) C45 0.096(4) 0.056(3) 0.040(2) 0.004(2) -0.007(2) -0.021(3) C46 0.089(4) 0.060(3) 0.054(3) -0.002(2) 0.011(3) -0.030(3) C47 0.073(3) 0.069(3) 0.069(3) -0.009(3) 0.001(3) -0.034(3) C48 0.071(3) 0.069(3) 0.049(3) -0.001(2) -0.013(2) -0.025(3) C49 0.084(3) 0.050(3) 0.038(2) -0.0039(19) -0.006(2) -0.023(2) C50 0.087(4) 0.054(3) 0.067(3) -0.004(2) 0.010(3) -0.029(3) C51 0.136(6) 0.069(4) 0.064(4) -0.008(3) 0.033(4) -0.036(4) C52 0.194(9) 0.077(4) 0.046(3) 0.003(3) -0.004(5) -0.042(5) C53 0.160(7) 0.071(4) 0.052(3) 0.005(3) -0.033(4) -0.033(4) C54 0.113(5) 0.054(3) 0.045(3) -0.001(2) -0.024(3) -0.027(3) C55 0.078(4) 0.090(4) 0.117(5) -0.014(4) 0.018(4) -0.033(3) C56 0.099(5) 0.085(4) 0.085(4) -0.003(3) -0.031(4) -0.016(3) N1S 0.265(13) 0.287(15) 0.153(8) -0.073(10) -0.016(7) -0.149(12) C1S 0.142(8) 0.278(17) 0.087(6) -0.039(9) -0.024(5) -0.089(11) C2S 0.45(3) 0.264(16) 0.170(11) 0.051(10) -0.162(13) -0.248(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.139(3) . ? Fe1 N3 2.215(4) . ? Fe1 N2 2.271(4) . ? Fe1 Cl2 2.2952(17) . ? Fe1 Cl1 2.3308(16) . ? N1 C11 1.289(5) . ? N1 C13 1.465(5) . ? N2 C12 1.286(5) . ? N2 C20 1.436(5) . ? N3 C19 1.333(6) . ? N3 C15 1.349(5) . ? C1 C2 1.372(5) . ? C1 C10 1.416(6) . ? C1 C11 1.468(5) . ? C2 C3 1.428(6) . ? C3 C4 1.368(7) . ? C4 C5 1.410(6) . ? C5 C6 1.409(7) . ? C5 C10 1.410(6) . ? C6 C7 1.371(7) . ? C7 C8 1.402(6) . ? C8 C9 1.377(6) . ? C9 C10 1.417(5) . ? C9 C12 1.466(6) . ? C11 C12 1.500(5) . ? C13 C14 1.516(6) . ? C14 C15 1.490(6) . ? C15 C16 1.382(6) . ? C16 C17 1.368(8) . ? C17 C18 1.366(8) . ? C18 C19 1.379(7) . ? C20 C25 1.385(7) . ? C20 C21 1.393(7) . ? C21 C22 1.395(7) . ? C21 C26 1.485(8) . ? C22 C23 1.358(10) . ? C23 C24 1.373(10) . ? C24 C25 1.400(7) . ? C25 C27 1.496(8) . ? Fe2 N4 2.158(3) . ? Fe2 N6 2.199(3) . ? Fe2 N5 2.229(3) . ? Fe2 Cl3 2.307(2) . ? Fe2 Cl4 2.3228(16) . ? N4 C40 1.269(5) . ? N4 C42 1.475(5) . ? N5 C41 1.281(5) . ? N5 C49 1.449(5) . ? N6 C48 1.344(6) . ? N6 C44 1.352(5) . ? C30 C31 1.385(6) . ? C30 C39 1.416(6) . ? C30 C40 1.471(6) . ? C31 C32 1.406(7) . ? C32 C33 1.356(7) . ? C33 C34 1.411(7) . ? C34 C39 1.399(6) . ? C34 C35 1.403(7) . ? C35 C36 1.374(7) . ? C36 C37 1.406(7) . ? C37 C38 1.370(6) . ? C38 C39 1.412(6) . ? C38 C41 1.473(6) . ? C40 C41 1.500(5) . ? C42 C43 1.511(6) . ? C43 C44 1.501(6) . ? C44 C45 1.387(6) . ? C45 C46 1.378(7) . ? C46 C47 1.364(7) . ? C47 C48 1.374(6) . ? C49 C50 1.375(7) . ? C49 C54 1.404(7) . ? C50 C51 1.414(8) . ? C50 C55 1.491(8) . ? C51 C52 1.382(10) . ? C52 C53 1.349(10) . ? C53 C54 1.380(7) . ? C54 C56 1.488(8) . ? N1S C1S 1.200(17) . ? C1S C2S 1.419(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N3 85.27(13) . . ? N1 Fe1 N2 75.51(12) . . ? N3 Fe1 N2 149.14(14) . . ? N1 Fe1 Cl2 147.37(10) . . ? N3 Fe1 Cl2 95.85(12) . . ? N2 Fe1 Cl2 88.12(11) . . ? N1 Fe1 Cl1 99.41(10) . . ? N3 Fe1 Cl1 101.59(12) . . ? N2 Fe1 Cl1 105.16(12) . . ? Cl2 Fe1 Cl1 112.16(6) . . ? C11 N1 C13 118.4(3) . . ? C11 N1 Fe1 116.8(2) . . ? C13 N1 Fe1 124.8(3) . . ? C12 N2 C20 121.1(4) . . ? C12 N2 Fe1 112.0(3) . . ? C20 N2 Fe1 126.9(3) . . ? C19 N3 C15 118.1(4) . . ? C19 N3 Fe1 119.0(3) . . ? C15 N3 Fe1 122.8(3) . . ? C2 C1 C10 118.9(4) . . ? C2 C1 C11 135.5(4) . . ? C10 C1 C11 105.7(3) . . ? C1 C2 C3 118.1(4) . . ? C4 C3 C2 122.9(4) . . ? C3 C4 C5 120.4(4) . . ? C6 C5 C10 116.6(4) . . ? C6 C5 C4 127.0(4) . . ? C10 C5 C4 116.3(4) . . ? C7 C6 C5 120.5(4) . . ? C6 C7 C8 122.4(4) . . ? C9 C8 C7 119.1(4) . . ? C8 C9 C10 118.6(4) . . ? C8 C9 C12 135.5(4) . . ? C10 C9 C12 105.9(3) . . ? C5 C10 C1 123.5(4) . . ? C5 C10 C9 122.7(4) . . ? C1 C10 C9 113.8(3) . . ? N1 C11 C1 135.2(3) . . ? N1 C11 C12 117.4(3) . . ? C1 C11 C12 107.4(3) . . ? N2 C12 C9 134.6(4) . . ? N2 C12 C11 118.2(4) . . ? C9 C12 C11 107.2(3) . . ? N1 C13 C14 111.5(3) . . ? C15 C14 C13 113.3(4) . . ? N3 C15 C16 120.7(5) . . ? N3 C15 C14 117.7(4) . . ? C16 C15 C14 121.6(4) . . ? C17 C16 C15 120.1(5) . . ? C18 C17 C16 119.7(5) . . ? C17 C18 C19 117.6(5) . . ? N3 C19 C18 123.8(5) . . ? C25 C20 C21 122.5(4) . . ? C25 C20 N2 118.4(5) . . ? C21 C20 N2 119.0(5) . . ? C20 C21 C22 117.2(6) . . ? C20 C21 C26 121.9(4) . . ? C22 C21 C26 120.8(5) . . ? C23 C22 C21 121.4(6) . . ? C22 C23 C24 120.7(5) . . ? C23 C24 C25 120.6(6) . . ? C20 C25 C24 117.6(6) . . ? C20 C25 C27 122.2(4) . . ? C24 C25 C27 120.1(6) . . ? N4 Fe2 N6 82.76(13) . . ? N4 Fe2 N5 75.46(13) . . ? N6 Fe2 N5 143.57(14) . . ? N4 Fe2 Cl3 98.54(12) . . ? N6 Fe2 Cl3 107.21(11) . . ? N5 Fe2 Cl3 104.66(12) . . ? N4 Fe2 Cl4 154.42(11) . . ? N6 Fe2 Cl4 95.28(10) . . ? N5 Fe2 Cl4 92.27(10) . . ? Cl3 Fe2 Cl4 106.33(8) . . ? C40 N4 C42 118.9(3) . . ? C40 N4 Fe2 116.2(3) . . ? C42 N4 Fe2 124.8(3) . . ? C41 N5 C49 118.0(3) . . ? C41 N5 Fe2 112.9(3) . . ? C49 N5 Fe2 129.0(3) . . ? C48 N6 C44 117.9(4) . . ? C48 N6 Fe2 119.9(3) . . ? C44 N6 Fe2 122.0(3) . . ? C31 C30 C39 118.8(4) . . ? C31 C30 C40 135.0(4) . . ? C39 C30 C40 106.1(4) . . ? C30 C31 C32 117.9(5) . . ? C33 C32 C31 123.0(5) . . ? C32 C33 C34 121.0(5) . . ? C39 C34 C35 115.9(4) . . ? C39 C34 C33 116.1(5) . . ? C35 C34 C33 128.0(5) . . ? C36 C35 C34 121.0(4) . . ? C35 C36 C37 122.3(5) . . ? C38 C37 C36 118.1(5) . . ? C37 C38 C39 119.4(4) . . ? C37 C38 C41 134.7(4) . . ? C39 C38 C41 106.0(4) . . ? C34 C39 C38 123.2(4) . . ? C34 C39 C30 123.1(4) . . ? C38 C39 C30 113.7(4) . . ? N4 C40 C30 135.7(4) . . ? N4 C40 C41 117.2(4) . . ? C30 C40 C41 107.0(3) . . ? N5 C41 C38 134.5(4) . . ? N5 C41 C40 118.2(4) . . ? C38 C41 C40 107.3(3) . . ? N4 C42 C43 111.1(4) . . ? C44 C43 C42 114.0(4) . . ? N6 C44 C45 121.1(4) . . ? N6 C44 C43 118.3(4) . . ? C45 C44 C43 120.7(4) . . ? C46 C45 C44 119.9(4) . . ? C47 C46 C45 118.8(4) . . ? C46 C47 C48 119.1(5) . . ? N6 C48 C47 123.1(4) . . ? C50 C49 C54 122.4(4) . . ? C50 C49 N5 118.5(5) . . ? C54 C49 N5 119.0(4) . . ? C49 C50 C51 117.3(6) . . ? C49 C50 C55 121.4(5) . . ? C51 C50 C55 121.2(6) . . ? C52 C51 C50 119.8(6) . . ? C53 C52 C51 121.7(6) . . ? C52 C53 C54 120.6(7) . . ? C53 C54 C49 118.2(6) . . ? C53 C54 C56 119.9(6) . . ? C49 C54 C56 121.8(4) . . ? N1S C1S C2S 177.5(14) . . ? 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 N3 Fe1 N1 C11 -156.4(3) . . . . ? N2 Fe1 N1 C11 -0.8(3) . . . . ? Cl2 Fe1 N1 C11 -63.0(4) . . . . ? Cl1 Fe1 N1 C11 102.6(3) . . . . ? N3 Fe1 N1 C13 24.6(3) . . . . ? N2 Fe1 N1 C13 -179.8(3) . . . . ? Cl2 Fe1 N1 C13 118.1(3) . . . . ? Cl1 Fe1 N1 C13 -76.4(3) . . . . ? N1 Fe1 N2 C12 2.0(3) . . . . ? N3 Fe1 N2 C12 55.3(4) . . . . ? Cl2 Fe1 N2 C12 153.5(3) . . . . ? Cl1 Fe1 N2 C12 -94.0(3) . . . . ? N1 Fe1 N2 C20 -177.0(4) . . . . ? N3 Fe1 N2 C20 -123.7(4) . . . . ? Cl2 Fe1 N2 C20 -25.5(4) . . . . ? Cl1 Fe1 N2 C20 87.0(4) . . . . ? N1 Fe1 N3 C19 144.0(4) . . . . ? N2 Fe1 N3 C19 92.9(4) . . . . ? Cl2 Fe1 N3 C19 -3.3(4) . . . . ? Cl1 Fe1 N3 C19 -117.4(4) . . . . ? N1 Fe1 N3 C15 -33.0(3) . . . . ? N2 Fe1 N3 C15 -84.1(4) . . . . ? Cl2 Fe1 N3 C15 179.8(3) . . . . ? Cl1 Fe1 N3 C15 65.7(3) . . . . ? C10 C1 C2 C3 -1.5(6) . . . . ? C11 C1 C2 C3 178.7(4) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? C2 C3 C4 C5 0.9(7) . . . . ? C3 C4 C5 C6 -179.8(5) . . . . ? C3 C4 C5 C10 -1.1(7) . . . . ? C10 C5 C6 C7 0.0(7) . . . . ? C4 C5 C6 C7 178.7(5) . . . . ? C5 C6 C7 C8 0.1(8) . . . . ? C6 C7 C8 C9 0.6(8) . . . . ? C7 C8 C9 C10 -1.2(7) . . . . ? C7 C8 C9 C12 -179.6(5) . . . . ? C6 C5 C10 C1 178.9(4) . . . . ? C4 C5 C10 C1 0.1(6) . . . . ? C6 C5 C10 C9 -0.8(6) . . . . ? C4 C5 C10 C9 -179.6(4) . . . . ? C2 C1 C10 C5 1.3(6) . . . . ? C11 C1 C10 C5 -178.8(4) . . . . ? C2 C1 C10 C9 -179.0(4) . . . . ? C11 C1 C10 C9 0.9(5) . . . . ? C8 C9 C10 C5 1.4(6) . . . . ? C12 C9 C10 C5 -179.8(4) . . . . ? C8 C9 C10 C1 -178.3(4) . . . . ? C12 C9 C10 C1 0.5(5) . . . . ? C13 N1 C11 C1 -1.8(7) . . . . ? Fe1 N1 C11 C1 179.2(4) . . . . ? C13 N1 C11 C12 178.6(3) . . . . ? Fe1 N1 C11 C12 -0.4(5) . . . . ? C2 C1 C11 N1 -1.6(8) . . . . ? C10 C1 C11 N1 178.5(4) . . . . ? C2 C1 C11 C12 178.0(5) . . . . ? C10 C1 C11 C12 -1.8(4) . . . . ? C20 N2 C12 C9 -3.1(8) . . . . ? Fe1 N2 C12 C9 177.8(4) . . . . ? C20 N2 C12 C11 176.1(4) . . . . ? Fe1 N2 C12 C11 -2.9(5) . . . . ? C8 C9 C12 N2 -3.8(9) . . . . ? C10 C9 C12 N2 177.7(5) . . . . ? C8 C9 C12 C11 176.9(5) . . . . ? C10 C9 C12 C11 -1.6(4) . . . . ? N1 C11 C12 N2 2.4(6) . . . . ? C1 C11 C12 N2 -177.3(4) . . . . ? N1 C11 C12 C9 -178.1(4) . . . . ? C1 C11 C12 C9 2.2(4) . . . . ? C11 N1 C13 C14 -162.4(4) . . . . ? Fe1 N1 C13 C14 16.5(5) . . . . ? N1 C13 C14 C15 -70.2(5) . . . . ? C19 N3 C15 C16 -0.5(7) . . . . ? Fe1 N3 C15 C16 176.5(3) . . . . ? C19 N3 C15 C14 -179.7(4) . . . . ? Fe1 N3 C15 C14 -2.7(5) . . . . ? C13 C14 C15 N3 63.8(5) . . . . ? C13 C14 C15 C16 -115.5(5) . . . . ? N3 C15 C16 C17 0.9(7) . . . . ? C14 C15 C16 C17 -179.9(5) . . . . ? C15 C16 C17 C18 0.1(9) . . . . ? C16 C17 C18 C19 -1.3(9) . . . . ? C15 N3 C19 C18 -0.8(8) . . . . ? Fe1 N3 C19 C18 -178.0(4) . . . . ? C17 C18 C19 N3 1.8(9) . . . . ? C12 N2 C20 C25 -86.3(6) . . . . ? Fe1 N2 C20 C25 92.6(5) . . . . ? C12 N2 C20 C21 97.1(5) . . . . ? Fe1 N2 C20 C21 -84.0(5) . . . . ? C25 C20 C21 C22 -2.5(7) . . . . ? N2 C20 C21 C22 174.0(4) . . . . ? C25 C20 C21 C26 177.3(5) . . . . ? N2 C20 C21 C26 -6.2(7) . . . . ? C20 C21 C22 C23 0.8(8) . . . . ? C26 C21 C22 C23 -179.0(6) . . . . ? C21 C22 C23 C24 0.5(9) . . . . ? C22 C23 C24 C25 -0.1(9) . . . . ? C21 C20 C25 C24 2.8(7) . . . . ? N2 C20 C25 C24 -173.7(4) . . . . ? C21 C20 C25 C27 -179.0(5) . . . . ? N2 C20 C25 C27 4.5(7) . . . . ? C23 C24 C25 C20 -1.5(8) . . . . ? C23 C24 C25 C27 -179.7(6) . . . . ? N6 Fe2 N4 C40 -149.5(3) . . . . ? N5 Fe2 N4 C40 1.1(3) . . . . ? Cl3 Fe2 N4 C40 104.1(3) . . . . ? Cl4 Fe2 N4 C40 -62.4(4) . . . . ? N6 Fe2 N4 C42 33.7(3) . . . . ? N5 Fe2 N4 C42 -175.8(4) . . . . ? Cl3 Fe2 N4 C42 -72.7(3) . . . . ? Cl4 Fe2 N4 C42 120.8(3) . . . . ? N4 Fe2 N5 C41 -1.4(3) . . . . ? N6 Fe2 N5 C41 53.8(4) . . . . ? Cl3 Fe2 N5 C41 -96.6(3) . . . . ? Cl4 Fe2 N5 C41 155.9(3) . . . . ? N4 Fe2 N5 C49 175.5(4) . . . . ? N6 Fe2 N5 C49 -129.3(4) . . . . ? Cl3 Fe2 N5 C49 80.3(4) . . . . ? Cl4 Fe2 N5 C49 -27.3(4) . . . . ? N4 Fe2 N6 C48 142.5(4) . . . . ? N5 Fe2 N6 C48 89.2(4) . . . . ? Cl3 Fe2 N6 C48 -120.8(3) . . . . ? Cl4 Fe2 N6 C48 -11.8(3) . . . . ? N4 Fe2 N6 C44 -42.5(3) . . . . ? N5 Fe2 N6 C44 -95.7(4) . . . . ? Cl3 Fe2 N6 C44 54.3(3) . . . . ? Cl4 Fe2 N6 C44 163.2(3) . . . . ? C39 C30 C31 C32 -0.8(7) . . . . ? C40 C30 C31 C32 176.4(5) . . . . ? C30 C31 C32 C33 1.8(9) . . . . ? C31 C32 C33 C34 -1.8(9) . . . . ? C32 C33 C34 C39 0.7(8) . . . . ? C32 C33 C34 C35 -179.5(6) . . . . ? C39 C34 C35 C36 -2.4(8) . . . . ? C33 C34 C35 C36 177.8(5) . . . . ? C34 C35 C36 C37 0.9(9) . . . . ? C35 C36 C37 C38 0.5(9) . . . . ? C36 C37 C38 C39 -0.3(7) . . . . ? C36 C37 C38 C41 -179.9(5) . . . . ? C35 C34 C39 C38 2.7(7) . . . . ? C33 C34 C39 C38 -177.5(4) . . . . ? C35 C34 C39 C30 -179.6(4) . . . . ? C33 C34 C39 C30 0.2(7) . . . . ? C37 C38 C39 C34 -1.4(7) . . . . ? C41 C38 C39 C34 178.3(4) . . . . ? C37 C38 C39 C30 -179.3(4) . . . . ? C41 C38 C39 C30 0.4(5) . . . . ? C31 C30 C39 C34 -0.2(7) . . . . ? C40 C30 C39 C34 -178.1(4) . . . . ? C31 C30 C39 C38 177.7(4) . . . . ? C40 C30 C39 C38 -0.2(5) . . . . ? C42 N4 C40 C30 -0.8(8) . . . . ? Fe2 N4 C40 C30 -177.8(4) . . . . ? C42 N4 C40 C41 176.4(4) . . . . ? Fe2 N4 C40 C41 -0.6(5) . . . . ? C31 C30 C40 N4 -0.2(9) . . . . ? C39 C30 C40 N4 177.3(5) . . . . ? C31 C30 C40 C41 -177.5(5) . . . . ? C39 C30 C40 C41 -0.1(5) . . . . ? C49 N5 C41 C38 0.2(8) . . . . ? Fe2 N5 C41 C38 177.4(4) . . . . ? C49 N5 C41 C40 -175.7(4) . . . . ? Fe2 N5 C41 C40 1.6(5) . . . . ? C37 C38 C41 N5 3.1(9) . . . . ? C39 C38 C41 N5 -176.6(5) . . . . ? C37 C38 C41 C40 179.3(5) . . . . ? C39 C38 C41 C40 -0.4(5) . . . . ? N4 C40 C41 N5 -0.7(6) . . . . ? C30 C40 C41 N5 177.2(4) . . . . ? N4 C40 C41 C38 -177.6(4) . . . . ? C30 C40 C41 C38 0.3(5) . . . . ? C40 N4 C42 C43 -167.9(4) . . . . ? Fe2 N4 C42 C43 8.9(5) . . . . ? N4 C42 C43 C44 -65.9(5) . . . . ? C48 N6 C44 C45 2.3(6) . . . . ? Fe2 N6 C44 C45 -172.8(3) . . . . ? C48 N6 C44 C43 -178.4(4) . . . . ? Fe2 N6 C44 C43 6.5(5) . . . . ? C42 C43 C44 N6 59.2(6) . . . . ? C42 C43 C44 C45 -121.4(5) . . . . ? N6 C44 C45 C46 -2.1(7) . . . . ? C43 C44 C45 C46 178.6(4) . . . . ? C44 C45 C46 C47 0.4(7) . . . . ? C45 C46 C47 C48 1.0(8) . . . . ? C44 N6 C48 C47 -0.9(7) . . . . ? Fe2 N6 C48 C47 174.3(4) . . . . ? C46 C47 C48 N6 -0.7(8) . . . . ? C41 N5 C49 C50 85.8(5) . . . . ? Fe2 N5 C49 C50 -91.0(5) . . . . ? C41 N5 C49 C54 -95.0(5) . . . . ? Fe2 N5 C49 C54 88.3(5) . . . . ? C54 C49 C50 C51 0.3(7) . . . . ? N5 C49 C50 C51 179.5(4) . . . . ? C54 C49 C50 C55 177.0(5) . . . . ? N5 C49 C50 C55 -3.8(7) . . . . ? C49 C50 C51 C52 -1.0(8) . . . . ? C55 C50 C51 C52 -177.7(5) . . . . ? C50 C51 C52 C53 1.4(10) . . . . ? C51 C52 C53 C54 -1.0(10) . . . . ? C52 C53 C54 C49 0.2(8) . . . . ? C52 C53 C54 C56 177.8(5) . . . . ? C50 C49 C54 C53 0.1(7) . . . . ? N5 C49 C54 C53 -179.1(4) . . . . ? C50 C49 C54 C56 -177.4(5) . . . . ? N5 C49 C54 C56 3.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.645 _refine_diff_density_min -0.597 _refine_diff_density_rms 0.066 #===END data_(2d)FeCl2 _database_code_depnum_ccdc_archive 'CCDC 636870' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040031 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H27 Cl2 Fe N3 O' _chemical_formula_weight 524.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3090(10) _cell_length_b 14.355(3) _cell_length_c 14.553(2) _cell_angle_alpha 89.42(2) _cell_angle_beta 77.510(10) _cell_angle_gamma 77.480(10) _cell_volume 2449.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.73 _cell_measurement_theta_max 15.78 _exptl_crystal_description Rod _exptl_crystal_colour Red-brown _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.692 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 8980 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.1080 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.95 _reflns_number_total 8545 _reflns_number_gt 5260 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0790P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8545 _refine_ls_number_parameters 599 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1247 _refine_ls_R_factor_gt 0.0680 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1460 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 Fe1 Fe 0.72129(7) 0.68790(6) 0.13970(6) 0.0218(2) Uani 1 1 d . . . Cl1 Cl 0.54563(13) 0.70355(11) 0.24270(10) 0.0316(4) Uani 1 1 d . . . Cl2 Cl 0.87920(13) 0.60651(11) 0.18452(11) 0.0314(4) Uani 1 1 d . . . N1 N 0.6823(4) 0.7717(3) 0.0269(3) 0.0232(11) Uani 1 1 d . . . N2 N 0.7479(4) 0.8339(3) 0.1749(3) 0.0242(11) Uani 1 1 d . . . N3 N 0.6815(4) 0.5776(3) 0.0396(3) 0.0247(11) Uani 1 1 d . . . O1 O 0.7922(4) 0.3801(3) 0.0561(3) 0.0370(11) Uani 1 1 d . . . C1 C 0.6536(5) 0.9432(4) -0.0256(4) 0.0223(13) Uani 1 1 d . . . C2 C 0.6129(5) 0.9578(4) -0.1075(4) 0.0268(14) Uani 1 1 d . . . H2A H 0.5980 0.9063 -0.1395 0.032 Uiso 1 1 calc R . . C3 C 0.5944(5) 1.0497(4) -0.1420(4) 0.0293(14) Uani 1 1 d . . . H3A H 0.5644 1.0604 -0.1971 0.035 Uiso 1 1 calc R . . C4 C 0.6182(5) 1.1252(4) -0.0986(4) 0.0301(15) Uani 1 1 d . . . H4A H 0.6053 1.1866 -0.1245 0.036 Uiso 1 1 calc R . . C5 C 0.6620(5) 1.1126(4) -0.0152(4) 0.0279(14) Uani 1 1 d . . . C6 C 0.6932(6) 1.1818(5) 0.0365(5) 0.0389(17) Uani 1 1 d . . . H6A H 0.6852 1.2454 0.0157 0.047 Uiso 1 1 calc R . . C7 C 0.7348(6) 1.1590(5) 0.1165(5) 0.0381(16) Uani 1 1 d . . . H7A H 0.7555 1.2070 0.1494 0.046 Uiso 1 1 calc R . . C8 C 0.7474(5) 1.0656(4) 0.1504(4) 0.0316(15) Uani 1 1 d . . . H8A H 0.7753 1.0512 0.2060 0.038 Uiso 1 1 calc R . . C9 C 0.7193(5) 0.9967(4) 0.1028(4) 0.0230(13) Uani 1 1 d . . . C10 C 0.6767(5) 1.0207(4) 0.0198(4) 0.0218(13) Uani 1 1 d . . . C11 C 0.6823(5) 0.8600(4) 0.0321(4) 0.0211(12) Uani 1 1 d . . . C12 C 0.7210(5) 0.8942(4) 0.1143(4) 0.0201(12) Uani 1 1 d . . . C13 C 0.6457(6) 0.7277(4) -0.0475(4) 0.0312(15) Uani 1 1 d . . . H13A H 0.7107 0.7077 -0.1019 0.037 Uiso 1 1 calc R . . H13B H 0.5851 0.7740 -0.0691 0.037 Uiso 1 1 calc R . . C14 C 0.6009(5) 0.6416(4) -0.0087(5) 0.0318(15) Uani 1 1 d . . . H14A H 0.5270 0.6636 0.0365 0.038 Uiso 1 1 calc R . . H14B H 0.5873 0.6052 -0.0609 0.038 Uiso 1 1 calc R . . C15 C 0.7815(5) 0.5246(4) -0.0322(4) 0.0298(14) Uani 1 1 d . . . H15A H 0.7536 0.4969 -0.0823 0.036 Uiso 1 1 calc R . . H15B H 0.8277 0.5699 -0.0616 0.036 Uiso 1 1 calc R . . C16 C 0.8550(6) 0.4465(4) 0.0095(4) 0.0312(15) Uani 1 1 d . . . H16A H 0.9181 0.4122 -0.0410 0.037 Uiso 1 1 calc R . . H16B H 0.8890 0.4747 0.0552 0.037 Uiso 1 1 calc R . . C17 C 0.7015(6) 0.4317(4) 0.1298(4) 0.0350(16) Uani 1 1 d . . . H17A H 0.7344 0.4620 0.1748 0.042 Uiso 1 1 calc R . . H17B H 0.6585 0.3866 0.1646 0.042 Uiso 1 1 calc R . . C18 C 0.6224(5) 0.5067(4) 0.0892(4) 0.0318(15) Uani 1 1 d . . . H18A H 0.5890 0.4760 0.0448 0.038 Uiso 1 1 calc R . . H18B H 0.5592 0.5394 0.1405 0.038 Uiso 1 1 calc R . . C19 C 0.7935(5) 0.8631(4) 0.2519(4) 0.0263(14) Uani 1 1 d . . . C20 C 0.7205(6) 0.8954(4) 0.3378(4) 0.0295(14) Uani 1 1 d . . . C21 C 0.7691(6) 0.9182(5) 0.4110(4) 0.0373(17) Uani 1 1 d . . . H21A H 0.7217 0.9392 0.4710 0.045 Uiso 1 1 calc R . . C22 C 0.8842(6) 0.9104(5) 0.3963(4) 0.0362(16) Uani 1 1 d . . . H22A H 0.9159 0.9273 0.4461 0.043 Uiso 1 1 calc R . . C23 C 0.9550(6) 0.8784(4) 0.3103(4) 0.0336(15) Uani 1 1 d . . . H23A H 1.0349 0.8731 0.3019 0.040 Uiso 1 1 calc R . . C24 C 0.9117(5) 0.8539(4) 0.2356(4) 0.0271(14) Uani 1 1 d . . . C25 C 0.9893(6) 0.8215(5) 0.1411(4) 0.0346(16) Uani 1 1 d . . . H25A H 0.9741 0.7620 0.1198 0.052 Uiso 1 1 calc R . . H25B H 1.0690 0.8106 0.1468 0.052 Uiso 1 1 calc R . . H25C H 0.9754 0.8708 0.0954 0.052 Uiso 1 1 calc R . . C26 C 0.5927(6) 0.9099(5) 0.3520(5) 0.0413(17) Uani 1 1 d . . . H26A H 0.5741 0.8535 0.3271 0.062 Uiso 1 1 calc R . . H26B H 0.5634 0.9662 0.3187 0.062 Uiso 1 1 calc R . . H26C H 0.5577 0.9193 0.4194 0.062 Uiso 1 1 calc R . . Fe2 Fe 0.72605(8) 0.70665(6) -0.36694(6) 0.0269(2) Uani 1 1 d . . . Cl3 Cl 0.59403(16) 0.84524(13) -0.33143(14) 0.0492(5) Uani 1 1 d . . . Cl4 Cl 0.75737(17) 0.59274(12) -0.25986(11) 0.0436(5) Uani 1 1 d . . . N4 N 0.8499(4) 0.6707(4) -0.4920(3) 0.0264(11) Uani 1 1 d . . . N5 N 0.8871(4) 0.7680(3) -0.3466(3) 0.0274(12) Uani 1 1 d . . . N6 N 0.6289(4) 0.6324(4) -0.4572(3) 0.0284(12) Uani 1 1 d . . . O2 O 0.4403(4) 0.5595(3) -0.3523(3) 0.0434(12) Uani 1 1 d . . . C27 C 1.0473(5) 0.6826(4) -0.5779(4) 0.0284(14) Uani 1 1 d . . . C28 C 1.0803(5) 0.6406(4) -0.6672(4) 0.0316(15) Uani 1 1 d . . . H28A H 1.0340 0.6050 -0.6896 0.038 Uiso 1 1 calc R . . C29 C 1.1846(5) 0.6518(5) -0.7246(4) 0.0347(15) Uani 1 1 d . . . H29A H 1.2072 0.6230 -0.7862 0.042 Uiso 1 1 calc R . . C30 C 1.2544(6) 0.7019(5) -0.6957(5) 0.0375(16) Uani 1 1 d . . . H30A H 1.3232 0.7085 -0.7371 0.045 Uiso 1 1 calc R . . C31 C 1.2233(5) 0.7443(4) -0.6030(4) 0.0313(15) Uani 1 1 d . . . C32 C 1.2869(5) 0.7977(4) -0.5627(4) 0.0320(15) Uani 1 1 d . . . H32A H 1.3586 0.8061 -0.5977 0.038 Uiso 1 1 calc R . . C33 C 1.2444(6) 0.8377(4) -0.4723(5) 0.0380(17) Uani 1 1 d . . . H33A H 1.2876 0.8738 -0.4465 0.046 Uiso 1 1 calc R . . C34 C 1.1384(5) 0.8263(4) -0.4170(4) 0.0326(15) Uani 1 1 d . . . H34A H 1.1105 0.8547 -0.3553 0.039 Uiso 1 1 calc R . . C35 C 1.0776(5) 0.7739(4) -0.4542(4) 0.0270(14) Uani 1 1 d . . . C36 C 1.1201(5) 0.7338(4) -0.5468(4) 0.0251(13) Uani 1 1 d . . . C37 C 0.9449(5) 0.6945(4) -0.5026(4) 0.0266(14) Uani 1 1 d . . . C38 C 0.9644(5) 0.7505(4) -0.4216(4) 0.0227(13) Uani 1 1 d . . . C39 C 0.8203(5) 0.6183(5) -0.5656(4) 0.0392(17) Uani 1 1 d . . . H39A H 0.8449 0.5486 -0.5587 0.047 Uiso 1 1 calc R . . H39B H 0.8593 0.6346 -0.6285 0.047 Uiso 1 1 calc R . . C40 C 0.6919(6) 0.6457(5) -0.5555(4) 0.0368(17) Uani 1 1 d . . . H40A H 0.6697 0.7133 -0.5716 0.044 Uiso 1 1 calc R . . H40B H 0.6697 0.6060 -0.6005 0.044 Uiso 1 1 calc R . . C41 C 0.6361(6) 0.5293(5) -0.4413(4) 0.0358(16) Uani 1 1 d . . . H41A H 0.7148 0.4984 -0.4368 0.043 Uiso 1 1 calc R . . H41B H 0.6189 0.4991 -0.4958 0.043 Uiso 1 1 calc R . . C42 C 0.5540(6) 0.5131(5) -0.3526(5) 0.0407(17) Uani 1 1 d . . . H42A H 0.5586 0.4437 -0.3464 0.049 Uiso 1 1 calc R . . H42B H 0.5766 0.5369 -0.2976 0.049 Uiso 1 1 calc R . . C43 C 0.4338(6) 0.6585(5) -0.3605(5) 0.0402(17) Uani 1 1 d . . . H43A H 0.4580 0.6833 -0.3068 0.048 Uiso 1 1 calc R . . H43B H 0.3538 0.6917 -0.3582 0.048 Uiso 1 1 calc R . . C44 C 0.5086(5) 0.6792(5) -0.4515(5) 0.0360(16) Uani 1 1 d . . . H44A H 0.4827 0.6563 -0.5052 0.043 Uiso 1 1 calc R . . H44B H 0.5014 0.7491 -0.4559 0.043 Uiso 1 1 calc R . . C45 C 0.9100(5) 0.8159(4) -0.2685(4) 0.0279(14) Uani 1 1 d . . . C46 C 0.9674(5) 0.7608(5) -0.2062(4) 0.0338(15) Uani 1 1 d . . . C47 C 0.9853(6) 0.8073(5) -0.1290(4) 0.0393(17) Uani 1 1 d . . . H47A H 1.0212 0.7711 -0.0845 0.047 Uiso 1 1 calc R . . C48 C 0.9519(6) 0.9047(5) -0.1165(4) 0.0368(17) Uani 1 1 d . . . H48A H 0.9661 0.9358 -0.0644 0.044 Uiso 1 1 calc R . . C49 C 0.8970(5) 0.9578(5) -0.1806(4) 0.0345(15) Uani 1 1 d . . . H49A H 0.8720 1.0251 -0.1704 0.041 Uiso 1 1 calc R . . C50 C 0.8781(5) 0.9148(5) -0.2590(4) 0.0290(14) Uani 1 1 d . . . C51 C 1.0128(6) 0.6546(5) -0.2232(5) 0.0449(19) Uani 1 1 d . . . H51A H 0.9510 0.6244 -0.2309 0.067 Uiso 1 1 calc R . . H51B H 1.0432 0.6279 -0.1693 0.067 Uiso 1 1 calc R . . H51C H 1.0736 0.6426 -0.2803 0.067 Uiso 1 1 calc R . . C52 C 0.8238(6) 0.9734(4) -0.3300(4) 0.0343(16) Uani 1 1 d . . . H52A H 0.7965 1.0399 -0.3063 0.051 Uiso 1 1 calc R . . H52B H 0.7594 0.9482 -0.3404 0.051 Uiso 1 1 calc R . . H52C H 0.8801 0.9704 -0.3895 0.051 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 Fe1 0.0243(5) 0.0257(5) 0.0177(4) 0.0047(3) -0.0085(4) -0.0067(4) Cl1 0.0286(8) 0.0384(9) 0.0269(8) 0.0020(7) -0.0018(7) -0.0097(7) Cl2 0.0310(9) 0.0352(9) 0.0306(8) 0.0019(7) -0.0163(7) -0.0034(7) N1 0.026(3) 0.031(3) 0.016(2) 0.000(2) -0.013(2) -0.007(2) N2 0.034(3) 0.024(3) 0.017(2) 0.005(2) -0.011(2) -0.008(2) N3 0.026(3) 0.026(3) 0.026(3) 0.007(2) -0.013(2) -0.008(2) O1 0.047(3) 0.025(2) 0.038(3) 0.002(2) -0.011(2) -0.004(2) C1 0.021(3) 0.028(3) 0.018(3) 0.004(2) -0.005(2) -0.004(2) C2 0.027(3) 0.038(4) 0.015(3) 0.007(3) 0.000(3) -0.011(3) C3 0.026(3) 0.043(4) 0.018(3) 0.013(3) -0.006(3) -0.005(3) C4 0.024(3) 0.034(4) 0.029(3) 0.012(3) -0.004(3) -0.002(3) C5 0.027(3) 0.024(3) 0.031(3) 0.006(3) -0.004(3) -0.007(3) C6 0.039(4) 0.026(4) 0.051(4) 0.008(3) -0.008(3) -0.007(3) C7 0.044(4) 0.030(4) 0.042(4) -0.005(3) -0.014(3) -0.008(3) C8 0.038(4) 0.025(3) 0.037(4) 0.001(3) -0.018(3) -0.007(3) C9 0.023(3) 0.025(3) 0.020(3) 0.004(2) -0.004(3) -0.004(3) C10 0.019(3) 0.024(3) 0.021(3) 0.002(2) -0.003(2) -0.004(2) C11 0.019(3) 0.031(3) 0.014(3) 0.002(2) -0.006(2) -0.006(3) C12 0.019(3) 0.022(3) 0.017(3) 0.001(2) -0.003(2) 0.000(2) C13 0.044(4) 0.026(3) 0.028(3) 0.000(3) -0.021(3) -0.005(3) C14 0.031(4) 0.029(3) 0.039(4) -0.002(3) -0.019(3) -0.003(3) C15 0.041(4) 0.031(3) 0.016(3) -0.003(3) -0.006(3) -0.008(3) C16 0.043(4) 0.027(3) 0.020(3) -0.001(3) -0.006(3) -0.001(3) C17 0.051(4) 0.027(3) 0.027(3) 0.007(3) -0.003(3) -0.015(3) C18 0.034(4) 0.027(3) 0.035(4) 0.000(3) -0.006(3) -0.008(3) C19 0.043(4) 0.023(3) 0.019(3) 0.004(2) -0.011(3) -0.016(3) C20 0.041(4) 0.021(3) 0.026(3) 0.004(3) -0.011(3) -0.004(3) C21 0.064(5) 0.035(4) 0.017(3) 0.002(3) -0.013(3) -0.017(3) C22 0.051(5) 0.038(4) 0.028(4) 0.002(3) -0.025(3) -0.012(3) C23 0.040(4) 0.036(4) 0.032(4) 0.008(3) -0.019(3) -0.015(3) C24 0.040(4) 0.026(3) 0.022(3) 0.012(3) -0.016(3) -0.014(3) C25 0.036(4) 0.045(4) 0.027(3) 0.000(3) -0.005(3) -0.017(3) C26 0.051(5) 0.041(4) 0.030(4) -0.010(3) -0.007(3) -0.007(4) Fe2 0.0318(5) 0.0325(5) 0.0174(4) 0.0043(4) -0.0068(4) -0.0079(4) Cl3 0.0416(11) 0.0393(10) 0.0660(13) -0.0103(9) -0.0178(9) -0.0004(8) Cl4 0.0705(13) 0.0444(10) 0.0286(9) 0.0138(7) -0.0278(9) -0.0235(9) N4 0.027(3) 0.039(3) 0.018(3) 0.002(2) -0.009(2) -0.013(2) N5 0.027(3) 0.033(3) 0.023(3) 0.005(2) -0.010(2) -0.005(2) N6 0.025(3) 0.045(3) 0.020(3) 0.003(2) -0.008(2) -0.014(2) O2 0.034(3) 0.059(3) 0.042(3) 0.009(2) -0.008(2) -0.022(2) C27 0.030(4) 0.030(3) 0.025(3) 0.003(3) -0.011(3) 0.000(3) C28 0.030(4) 0.032(4) 0.032(4) -0.005(3) -0.010(3) -0.003(3) C29 0.027(4) 0.047(4) 0.026(3) -0.003(3) -0.002(3) -0.005(3) C30 0.027(4) 0.045(4) 0.033(4) 0.008(3) 0.003(3) -0.003(3) C31 0.030(4) 0.032(4) 0.034(4) 0.006(3) -0.012(3) -0.005(3) C32 0.025(3) 0.036(4) 0.034(4) 0.005(3) -0.005(3) -0.005(3) C33 0.033(4) 0.031(4) 0.057(5) 0.003(3) -0.021(4) -0.011(3) C34 0.026(4) 0.040(4) 0.032(4) 0.001(3) -0.007(3) -0.005(3) C35 0.030(4) 0.029(3) 0.026(3) 0.005(3) -0.012(3) -0.009(3) C36 0.027(3) 0.027(3) 0.024(3) 0.001(3) -0.011(3) -0.007(3) C37 0.031(4) 0.026(3) 0.024(3) -0.001(3) -0.007(3) -0.006(3) C38 0.024(3) 0.024(3) 0.022(3) 0.008(2) -0.011(3) -0.004(3) C39 0.034(4) 0.067(5) 0.021(3) -0.006(3) -0.001(3) -0.025(4) C40 0.042(4) 0.060(5) 0.016(3) 0.009(3) -0.008(3) -0.026(4) C41 0.040(4) 0.038(4) 0.035(4) 0.005(3) -0.013(3) -0.016(3) C42 0.044(4) 0.045(4) 0.041(4) 0.015(3) -0.016(3) -0.020(4) C43 0.032(4) 0.053(5) 0.032(4) 0.010(3) -0.002(3) -0.007(3) C44 0.027(4) 0.049(4) 0.036(4) 0.010(3) -0.014(3) -0.012(3) C45 0.027(3) 0.036(4) 0.022(3) -0.001(3) -0.003(3) -0.011(3) C46 0.032(4) 0.042(4) 0.031(4) 0.014(3) -0.014(3) -0.011(3) C47 0.045(4) 0.060(5) 0.021(3) 0.010(3) -0.016(3) -0.020(4) C48 0.039(4) 0.060(5) 0.019(3) 0.001(3) -0.010(3) -0.026(4) C49 0.027(4) 0.046(4) 0.028(4) -0.009(3) -0.001(3) -0.008(3) C50 0.027(3) 0.043(4) 0.016(3) 0.004(3) 0.000(3) -0.013(3) C51 0.054(5) 0.046(4) 0.041(4) 0.021(3) -0.029(4) -0.005(4) C52 0.043(4) 0.034(4) 0.031(4) 0.006(3) -0.015(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.102(4) . ? Fe1 Cl2 2.2620(17) . ? Fe1 N2 2.270(5) . ? Fe1 Cl1 2.3166(17) . ? Fe1 N3 2.358(5) . ? N1 C11 1.272(7) . ? N1 C13 1.457(7) . ? N2 C12 1.275(7) . ? N2 C19 1.460(7) . ? N3 C18 1.473(7) . ? N3 C14 1.488(7) . ? N3 C15 1.496(7) . ? O1 C16 1.430(7) . ? O1 C17 1.444(7) . ? C1 C2 1.386(8) . ? C1 C10 1.411(8) . ? C1 C11 1.476(7) . ? C2 C3 1.397(8) . ? C3 C4 1.376(9) . ? C4 C5 1.425(8) . ? C5 C10 1.398(8) . ? C5 C6 1.417(9) . ? C6 C7 1.379(9) . ? C7 C8 1.412(8) . ? C8 C9 1.358(8) . ? C9 C10 1.429(7) . ? C9 C12 1.475(7) . ? C11 C12 1.502(7) . ? C13 C14 1.515(8) . ? C15 C16 1.493(8) . ? C17 C18 1.496(8) . ? C19 C20 1.389(8) . ? C19 C24 1.399(8) . ? C20 C21 1.402(8) . ? C20 C26 1.510(9) . ? C21 C22 1.366(9) . ? C22 C23 1.381(9) . ? C23 C24 1.388(8) . ? C24 C25 1.508(8) . ? Fe2 N4 2.093(5) . ? Fe2 Cl3 2.263(2) . ? Fe2 Cl4 2.2773(18) . ? Fe2 N6 2.356(5) . ? Fe2 N5 2.410(5) . ? N4 C37 1.266(7) . ? N4 C39 1.466(7) . ? N5 C38 1.269(7) . ? N5 C45 1.443(7) . ? N6 C44 1.473(8) . ? N6 C41 1.482(8) . ? N6 C40 1.505(7) . ? O2 C43 1.412(8) . ? O2 C42 1.413(8) . ? C27 C28 1.378(8) . ? C27 C36 1.420(8) . ? C27 C37 1.459(8) . ? C28 C29 1.412(8) . ? C29 C30 1.365(9) . ? C30 C31 1.425(9) . ? C31 C36 1.392(8) . ? C31 C32 1.418(9) . ? C32 C33 1.387(9) . ? C33 C34 1.419(9) . ? C34 C35 1.359(8) . ? C35 C36 1.415(8) . ? C35 C38 1.482(8) . ? C37 C38 1.522(8) . ? C39 C40 1.518(9) . ? C41 C42 1.508(9) . ? C43 C44 1.507(8) . ? C45 C50 1.389(8) . ? C45 C46 1.402(8) . ? C46 C47 1.393(9) . ? C46 C51 1.508(9) . ? C47 C48 1.372(9) . ? C48 C49 1.393(9) . ? C49 C50 1.389(8) . ? C50 C52 1.503(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 Cl2 137.57(14) . . ? N1 Fe1 N2 75.56(17) . . ? Cl2 Fe1 N2 94.56(13) . . ? N1 Fe1 Cl1 103.21(14) . . ? Cl2 Fe1 Cl1 118.94(6) . . ? N2 Fe1 Cl1 95.84(13) . . ? N1 Fe1 N3 77.25(17) . . ? Cl2 Fe1 N3 103.79(12) . . ? N2 Fe1 N3 152.68(16) . . ? Cl1 Fe1 N3 92.81(13) . . ? C11 N1 C13 123.7(5) . . ? C11 N1 Fe1 117.7(4) . . ? C13 N1 Fe1 118.3(4) . . ? C12 N2 C19 119.5(5) . . ? C12 N2 Fe1 111.3(4) . . ? C19 N2 Fe1 129.1(3) . . ? C18 N3 C14 108.0(5) . . ? C18 N3 C15 107.6(5) . . ? C14 N3 C15 109.6(4) . . ? C18 N3 Fe1 114.3(4) . . ? C14 N3 Fe1 101.2(3) . . ? C15 N3 Fe1 115.8(3) . . ? C16 O1 C17 108.1(4) . . ? C2 C1 C10 119.4(5) . . ? C2 C1 C11 135.1(5) . . ? C10 C1 C11 105.5(5) . . ? C1 C2 C3 118.8(6) . . ? C4 C3 C2 121.9(6) . . ? C3 C4 C5 120.9(5) . . ? C10 C5 C6 115.8(5) . . ? C10 C5 C4 116.3(5) . . ? C6 C5 C4 127.9(6) . . ? C7 C6 C5 121.4(6) . . ? C6 C7 C8 121.2(6) . . ? C9 C8 C7 119.5(6) . . ? C8 C9 C10 119.0(5) . . ? C8 C9 C12 135.6(5) . . ? C10 C9 C12 105.3(5) . . ? C5 C10 C1 122.6(5) . . ? C5 C10 C9 123.0(5) . . ? C1 C10 C9 114.3(5) . . ? N1 C11 C1 135.4(5) . . ? N1 C11 C12 117.0(5) . . ? C1 C11 C12 107.6(5) . . ? N2 C12 C9 134.6(5) . . ? N2 C12 C11 118.2(5) . . ? C9 C12 C11 107.2(4) . . ? N1 C13 C14 108.4(5) . . ? N3 C14 C13 112.2(5) . . ? C16 C15 N3 112.3(5) . . ? O1 C16 C15 112.0(5) . . ? O1 C17 C18 110.5(5) . . ? N3 C18 C17 111.7(5) . . ? C20 C19 C24 122.9(6) . . ? C20 C19 N2 119.9(6) . . ? C24 C19 N2 117.2(5) . . ? C19 C20 C21 117.7(6) . . ? C19 C20 C26 121.9(6) . . ? C21 C20 C26 120.3(6) . . ? C22 C21 C20 120.3(6) . . ? C21 C22 C23 121.0(6) . . ? C22 C23 C24 121.2(6) . . ? C23 C24 C19 116.9(6) . . ? C23 C24 C25 120.8(6) . . ? C19 C24 C25 122.2(5) . . ? N4 Fe2 Cl3 126.75(15) . . ? N4 Fe2 Cl4 109.67(15) . . ? Cl3 Fe2 Cl4 123.09(8) . . ? N4 Fe2 N6 78.74(17) . . ? Cl3 Fe2 N6 97.56(14) . . ? Cl4 Fe2 N6 100.05(13) . . ? N4 Fe2 N5 73.92(17) . . ? Cl3 Fe2 N5 96.77(13) . . ? Cl4 Fe2 N5 91.49(12) . . ? N6 Fe2 N5 152.54(17) . . ? C37 N4 C39 122.5(5) . . ? C37 N4 Fe2 120.7(4) . . ? C39 N4 Fe2 116.8(4) . . ? C38 N5 C45 118.1(5) . . ? C38 N5 Fe2 109.0(4) . . ? C45 N5 Fe2 132.9(4) . . ? C44 N6 C41 108.5(5) . . ? C44 N6 C40 106.3(5) . . ? C41 N6 C40 109.8(5) . . ? C44 N6 Fe2 115.7(4) . . ? C41 N6 Fe2 114.8(4) . . ? C40 N6 Fe2 101.1(3) . . ? C43 O2 C42 109.0(5) . . ? C28 C27 C36 118.8(6) . . ? C28 C27 C37 134.8(6) . . ? C36 C27 C37 106.2(5) . . ? C27 C28 C29 118.4(6) . . ? C30 C29 C28 123.1(6) . . ? C29 C30 C31 119.5(6) . . ? C36 C31 C32 116.6(6) . . ? C36 C31 C30 117.2(6) . . ? C32 C31 C30 126.1(6) . . ? C33 C32 C31 119.9(6) . . ? C32 C33 C34 122.1(6) . . ? C35 C34 C33 118.5(6) . . ? C34 C35 C36 119.6(6) . . ? C34 C35 C38 134.3(6) . . ? C36 C35 C38 106.0(5) . . ? C31 C36 C35 123.2(5) . . ? C31 C36 C27 122.9(6) . . ? C35 C36 C27 113.9(5) . . ? N4 C37 C27 135.2(6) . . ? N4 C37 C38 117.4(5) . . ? C27 C37 C38 107.4(5) . . ? N5 C38 C35 134.7(5) . . ? N5 C38 C37 118.9(5) . . ? C35 C38 C37 106.4(5) . . ? N4 C39 C40 108.3(5) . . ? N6 C40 C39 111.8(5) . . ? N6 C41 C42 111.7(5) . . ? O2 C42 C41 112.3(5) . . ? O2 C43 C44 111.1(6) . . ? N6 C44 C43 111.2(5) . . ? C50 C45 C46 122.1(6) . . ? C50 C45 N5 119.2(5) . . ? C46 C45 N5 118.6(5) . . ? C47 C46 C45 118.2(6) . . ? C47 C46 C51 120.3(6) . . ? C45 C46 C51 121.5(6) . . ? C48 C47 C46 120.9(6) . . ? C47 C48 C49 119.7(6) . . ? C50 C49 C48 121.6(6) . . ? C49 C50 C45 117.4(6) . . ? C49 C50 C52 121.0(6) . . ? C45 C50 C52 121.5(5) . . ? 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 Cl2 Fe1 N1 C11 -85.8(5) . . . . ? N2 Fe1 N1 C11 -5.0(4) . . . . ? Cl1 Fe1 N1 C11 87.7(4) . . . . ? N3 Fe1 N1 C11 177.6(5) . . . . ? Cl2 Fe1 N1 C13 100.4(4) . . . . ? N2 Fe1 N1 C13 -178.8(5) . . . . ? Cl1 Fe1 N1 C13 -86.1(4) . . . . ? N3 Fe1 N1 C13 3.8(4) . . . . ? N1 Fe1 N2 C12 3.6(4) . . . . ? Cl2 Fe1 N2 C12 141.7(4) . . . . ? Cl1 Fe1 N2 C12 -98.6(4) . . . . ? N3 Fe1 N2 C12 9.2(6) . . . . ? N1 Fe1 N2 C19 -173.9(5) . . . . ? Cl2 Fe1 N2 C19 -35.8(5) . . . . ? Cl1 Fe1 N2 C19 84.0(5) . . . . ? N3 Fe1 N2 C19 -168.3(4) . . . . ? N1 Fe1 N3 C18 -143.7(4) . . . . ? Cl2 Fe1 N3 C18 79.9(4) . . . . ? N2 Fe1 N3 C18 -149.3(4) . . . . ? Cl1 Fe1 N3 C18 -40.8(4) . . . . ? N1 Fe1 N3 C14 -27.9(4) . . . . ? Cl2 Fe1 N3 C14 -164.2(3) . . . . ? N2 Fe1 N3 C14 -33.5(6) . . . . ? Cl1 Fe1 N3 C14 75.0(3) . . . . ? N1 Fe1 N3 C15 90.4(4) . . . . ? Cl2 Fe1 N3 C15 -45.9(4) . . . . ? N2 Fe1 N3 C15 84.9(5) . . . . ? Cl1 Fe1 N3 C15 -166.6(3) . . . . ? C10 C1 C2 C3 -1.0(8) . . . . ? C11 C1 C2 C3 179.4(6) . . . . ? C1 C2 C3 C4 1.8(9) . . . . ? C2 C3 C4 C5 -0.7(9) . . . . ? C3 C4 C5 C10 -1.1(9) . . . . ? C3 C4 C5 C6 178.4(6) . . . . ? C10 C5 C6 C7 -0.3(9) . . . . ? C4 C5 C6 C7 -179.9(6) . . . . ? C5 C6 C7 C8 -0.4(10) . . . . ? C6 C7 C8 C9 0.8(10) . . . . ? C7 C8 C9 C10 -0.5(9) . . . . ? C7 C8 C9 C12 179.4(6) . . . . ? C6 C5 C10 C1 -177.6(6) . . . . ? C4 C5 C10 C1 2.0(8) . . . . ? C6 C5 C10 C9 0.7(9) . . . . ? C4 C5 C10 C9 -179.7(5) . . . . ? C2 C1 C10 C5 -1.0(9) . . . . ? C11 C1 C10 C5 178.8(5) . . . . ? C2 C1 C10 C9 -179.4(5) . . . . ? C11 C1 C10 C9 0.4(7) . . . . ? C8 C9 C10 C5 -0.3(9) . . . . ? C12 C9 C10 C5 179.9(5) . . . . ? C8 C9 C10 C1 178.2(5) . . . . ? C12 C9 C10 C1 -1.7(7) . . . . ? C13 N1 C11 C1 -1.8(10) . . . . ? Fe1 N1 C11 C1 -175.2(5) . . . . ? C13 N1 C11 C12 179.1(5) . . . . ? Fe1 N1 C11 C12 5.6(7) . . . . ? C2 C1 C11 N1 1.6(12) . . . . ? C10 C1 C11 N1 -178.1(6) . . . . ? C2 C1 C11 C12 -179.2(6) . . . . ? C10 C1 C11 C12 1.1(6) . . . . ? C19 N2 C12 C9 -3.5(10) . . . . ? Fe1 N2 C12 C9 178.8(5) . . . . ? C19 N2 C12 C11 175.7(5) . . . . ? Fe1 N2 C12 C11 -2.1(6) . . . . ? C8 C9 C12 N2 1.6(12) . . . . ? C10 C9 C12 N2 -178.5(6) . . . . ? C8 C9 C12 C11 -177.5(7) . . . . ? C10 C9 C12 C11 2.3(6) . . . . ? N1 C11 C12 N2 -2.1(8) . . . . ? C1 C11 C12 N2 178.5(5) . . . . ? N1 C11 C12 C9 177.2(5) . . . . ? C1 C11 C12 C9 -2.2(6) . . . . ? C11 N1 C13 C14 -151.9(5) . . . . ? Fe1 N1 C13 C14 21.5(6) . . . . ? C18 N3 C14 C13 169.9(5) . . . . ? C15 N3 C14 C13 -73.2(6) . . . . ? Fe1 N3 C14 C13 49.5(5) . . . . ? N1 C13 C14 N3 -49.9(7) . . . . ? C18 N3 C15 C16 -52.4(6) . . . . ? C14 N3 C15 C16 -169.6(5) . . . . ? Fe1 N3 C15 C16 76.8(5) . . . . ? C17 O1 C16 C15 -59.4(6) . . . . ? N3 C15 C16 O1 56.8(7) . . . . ? C16 O1 C17 C18 61.2(6) . . . . ? C14 N3 C18 C17 172.8(5) . . . . ? C15 N3 C18 C17 54.6(6) . . . . ? Fe1 N3 C18 C17 -75.4(6) . . . . ? O1 C17 C18 N3 -61.2(7) . . . . ? C12 N2 C19 C20 93.6(7) . . . . ? Fe1 N2 C19 C20 -89.2(6) . . . . ? C12 N2 C19 C24 -88.5(7) . . . . ? Fe1 N2 C19 C24 88.7(6) . . . . ? C24 C19 C20 C21 -0.9(9) . . . . ? N2 C19 C20 C21 176.9(5) . . . . ? C24 C19 C20 C26 176.6(6) . . . . ? N2 C19 C20 C26 -5.6(8) . . . . ? C19 C20 C21 C22 1.4(9) . . . . ? C26 C20 C21 C22 -176.1(6) . . . . ? C20 C21 C22 C23 -1.3(10) . . . . ? C21 C22 C23 C24 0.6(10) . . . . ? C22 C23 C24 C19 0.0(9) . . . . ? C22 C23 C24 C25 178.4(6) . . . . ? C20 C19 C24 C23 0.2(9) . . . . ? N2 C19 C24 C23 -177.6(5) . . . . ? C20 C19 C24 C25 -178.2(5) . . . . ? N2 C19 C24 C25 4.0(8) . . . . ? Cl3 Fe2 N4 C37 85.9(5) . . . . ? Cl4 Fe2 N4 C37 -86.3(5) . . . . ? N6 Fe2 N4 C37 176.9(5) . . . . ? N5 Fe2 N4 C37 -0.6(4) . . . . ? Cl3 Fe2 N4 C39 -93.5(5) . . . . ? Cl4 Fe2 N4 C39 94.3(4) . . . . ? N6 Fe2 N4 C39 -2.5(4) . . . . ? N5 Fe2 N4 C39 -180.0(5) . . . . ? N4 Fe2 N5 C38 1.7(4) . . . . ? Cl3 Fe2 N5 C38 -124.7(4) . . . . ? Cl4 Fe2 N5 C38 111.8(4) . . . . ? N6 Fe2 N5 C38 -3.6(6) . . . . ? N4 Fe2 N5 C45 -176.7(5) . . . . ? Cl3 Fe2 N5 C45 56.9(5) . . . . ? Cl4 Fe2 N5 C45 -66.6(5) . . . . ? N6 Fe2 N5 C45 178.0(5) . . . . ? N4 Fe2 N6 C44 -138.2(4) . . . . ? Cl3 Fe2 N6 C44 -12.1(4) . . . . ? Cl4 Fe2 N6 C44 113.6(4) . . . . ? N5 Fe2 N6 C44 -133.0(4) . . . . ? N4 Fe2 N6 C41 94.3(4) . . . . ? Cl3 Fe2 N6 C41 -139.6(4) . . . . ? Cl4 Fe2 N6 C41 -14.0(4) . . . . ? N5 Fe2 N6 C41 99.5(5) . . . . ? N4 Fe2 N6 C40 -23.8(4) . . . . ? Cl3 Fe2 N6 C40 102.3(4) . . . . ? Cl4 Fe2 N6 C40 -132.1(4) . . . . ? N5 Fe2 N6 C40 -18.6(6) . . . . ? C36 C27 C28 C29 -1.1(9) . . . . ? C37 C27 C28 C29 173.7(6) . . . . ? C27 C28 C29 C30 0.2(10) . . . . ? C28 C29 C30 C31 1.1(10) . . . . ? C29 C30 C31 C36 -1.4(9) . . . . ? C29 C30 C31 C32 179.5(6) . . . . ? C36 C31 C32 C33 -1.2(9) . . . . ? C30 C31 C32 C33 177.9(6) . . . . ? C31 C32 C33 C34 0.7(9) . . . . ? C32 C33 C34 C35 0.4(9) . . . . ? C33 C34 C35 C36 -1.0(9) . . . . ? C33 C34 C35 C38 -176.4(6) . . . . ? C32 C31 C36 C35 0.6(9) . . . . ? C30 C31 C36 C35 -178.5(6) . . . . ? C32 C31 C36 C27 179.7(6) . . . . ? C30 C31 C36 C27 0.6(9) . . . . ? C34 C35 C36 C31 0.5(9) . . . . ? C38 C35 C36 C31 177.1(5) . . . . ? C34 C35 C36 C27 -178.7(5) . . . . ? C38 C35 C36 C27 -2.1(7) . . . . ? C28 C27 C36 C31 0.7(9) . . . . ? C37 C27 C36 C31 -175.4(5) . . . . ? C28 C27 C36 C35 179.9(5) . . . . ? C37 C27 C36 C35 3.8(7) . . . . ? C39 N4 C37 C27 -0.1(11) . . . . ? Fe2 N4 C37 C27 -179.4(5) . . . . ? C39 N4 C37 C38 178.8(5) . . . . ? Fe2 N4 C37 C38 -0.5(7) . . . . ? C28 C27 C37 N4 0.1(12) . . . . ? C36 C27 C37 N4 175.3(7) . . . . ? C28 C27 C37 C38 -179.0(6) . . . . ? C36 C27 C37 C38 -3.7(6) . . . . ? C45 N5 C38 C35 -5.3(9) . . . . ? Fe2 N5 C38 C35 176.0(5) . . . . ? C45 N5 C38 C37 176.2(5) . . . . ? Fe2 N5 C38 C37 -2.5(6) . . . . ? C34 C35 C38 N5 -3.2(12) . . . . ? C36 C35 C38 N5 -179.1(6) . . . . ? C34 C35 C38 C37 175.5(7) . . . . ? C36 C35 C38 C37 -0.4(6) . . . . ? N4 C37 C38 N5 2.3(8) . . . . ? C27 C37 C38 N5 -178.5(5) . . . . ? N4 C37 C38 C35 -176.6(5) . . . . ? C27 C37 C38 C35 2.6(6) . . . . ? C37 N4 C39 C40 -150.5(6) . . . . ? Fe2 N4 C39 C40 28.9(7) . . . . ? C44 N6 C40 C39 168.7(5) . . . . ? C41 N6 C40 C39 -74.2(6) . . . . ? Fe2 N6 C40 C39 47.5(6) . . . . ? N4 C39 C40 N6 -53.2(7) . . . . ? C44 N6 C41 C42 -51.7(7) . . . . ? C40 N6 C41 C42 -167.6(5) . . . . ? Fe2 N6 C41 C42 79.3(6) . . . . ? C43 O2 C42 C41 -59.3(7) . . . . ? N6 C41 C42 O2 55.9(7) . . . . ? C42 O2 C43 C44 61.0(7) . . . . ? C41 N6 C44 C43 53.8(7) . . . . ? C40 N6 C44 C43 171.8(5) . . . . ? Fe2 N6 C44 C43 -76.9(6) . . . . ? O2 C43 C44 N6 -60.0(7) . . . . ? C38 N5 C45 C50 92.4(7) . . . . ? Fe2 N5 C45 C50 -89.3(6) . . . . ? C38 N5 C45 C46 -85.5(7) . . . . ? Fe2 N5 C45 C46 92.7(6) . . . . ? C50 C45 C46 C47 4.5(9) . . . . ? N5 C45 C46 C47 -177.6(5) . . . . ? C50 C45 C46 C51 -173.3(6) . . . . ? N5 C45 C46 C51 4.6(9) . . . . ? C45 C46 C47 C48 -2.6(10) . . . . ? C51 C46 C47 C48 175.2(6) . . . . ? C46 C47 C48 C49 1.4(10) . . . . ? C47 C48 C49 C50 -1.9(10) . . . . ? C48 C49 C50 C45 3.6(9) . . . . ? C48 C49 C50 C52 -177.1(6) . . . . ? C46 C45 C50 C49 -4.9(9) . . . . ? N5 C45 C50 C49 177.2(5) . . . . ? C46 C45 C50 C52 175.8(6) . . . . ? N5 C45 C50 C52 -2.1(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.95 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.693 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.097 #===END data_(2a)MnCl2 _database_code_depnum_ccdc_archive 'CCDC 636871' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 050003 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H25 Cl2 Mn N3' _chemical_formula_weight 481.31 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' 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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.107(2) _cell_length_b 16.5813(7) _cell_length_c 14.8160(1) _cell_angle_alpha 90.00 _cell_angle_beta 102.740(1) _cell_angle_gamma 90.00 _cell_volume 4578.4(6) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12.75 _cell_measurement_theta_max 22.61 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.397 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.826 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.9514 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 5125 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0223 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.97 _reflns_number_total 4975 _reflns_number_gt 4244 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0426P)^2^+2.6298P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4975 _refine_ls_number_parameters 275 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0312 _refine_ls_wR_factor_ref 0.0803 _refine_ls_wR_factor_gt 0.0762 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Mn1 Mn 0.174004(13) 0.012773(16) 0.299092(16) 0.02393(8) Uani 1 1 d . . . Cl1 Cl 0.18697(3) -0.11574(3) 0.23800(3) 0.03976(12) Uani 1 1 d . . . Cl2 Cl 0.09485(2) 0.09586(3) 0.19503(3) 0.03019(11) Uani 1 1 d . . . N1 N 0.21549(7) 0.08056(9) 0.42905(10) 0.0269(3) Uani 1 1 d . . . N2 N 0.28928(7) 0.06632(9) 0.29263(9) 0.0262(3) Uani 1 1 d . . . N3 N 0.11303(7) -0.03360(9) 0.40718(9) 0.0248(3) Uani 1 1 d . . . C1 C 0.31982(9) 0.16517(10) 0.51405(11) 0.0262(3) Uani 1 1 d . . . C2 C 0.31225(10) 0.19139(11) 0.59981(12) 0.0312(4) Uani 1 1 d . . . H2A H 0.2716 0.1788 0.6218 0.037 Uiso 1 1 calc R . . C3 C 0.36851(11) 0.23816(11) 0.65320(13) 0.0369(4) Uani 1 1 d . . . H3A H 0.3639 0.2564 0.7110 0.044 Uiso 1 1 calc R . . C4 C 0.42925(11) 0.25768(11) 0.62370(13) 0.0371(4) Uani 1 1 d . . . H4A H 0.4646 0.2888 0.6612 0.045 Uiso 1 1 calc R . . C5 C 0.43889(10) 0.23083(11) 0.53595(13) 0.0317(4) Uani 1 1 d . . . C6 C 0.49778(11) 0.24653(12) 0.49536(14) 0.0380(4) Uani 1 1 d . . . H6A H 0.5364 0.2765 0.5276 0.046 Uiso 1 1 calc R . . C7 C 0.49850(10) 0.21776(12) 0.40828(15) 0.0389(5) Uani 1 1 d . . . H7A H 0.5376 0.2298 0.3827 0.047 Uiso 1 1 calc R . . C8 C 0.44192(10) 0.17056(12) 0.35631(14) 0.0341(4) Uani 1 1 d . . . H8A H 0.4440 0.1510 0.2981 0.041 Uiso 1 1 calc R . . C9 C 0.38401(9) 0.15451(10) 0.39403(12) 0.0269(3) Uani 1 1 d . . . C10 C 0.38265(9) 0.18516(10) 0.48304(12) 0.0269(3) Uani 1 1 d . . . C11 C 0.27555(9) 0.11666(10) 0.43991(11) 0.0248(3) Uani 1 1 d . . . C12 C 0.31629(9) 0.10930(10) 0.36363(12) 0.0253(3) Uani 1 1 d . . . C13 C 0.17469(10) 0.07925(12) 0.50182(12) 0.0305(4) Uani 1 1 d . . . H13A H 0.1661 0.1339 0.5200 0.037 Uiso 1 1 calc R . . H13B H 0.2017 0.0510 0.5557 0.037 Uiso 1 1 calc R . . C14 C 0.10361(9) 0.03666(11) 0.46509(12) 0.0293(4) Uani 1 1 d . . . H14A H 0.0839 0.0187 0.5166 0.035 Uiso 1 1 calc R . . H14B H 0.0699 0.0742 0.4286 0.035 Uiso 1 1 calc R . . C15 C 0.15707(10) -0.09645(12) 0.46385(13) 0.0338(4) Uani 1 1 d . . . H15A H 0.1351 -0.1118 0.5136 0.051 Uiso 1 1 calc R . . H15B H 0.2043 -0.0756 0.4887 0.051 Uiso 1 1 calc R . . H15C H 0.1604 -0.1427 0.4260 0.051 Uiso 1 1 calc R . . C16 C 0.04203(10) -0.06795(12) 0.36622(13) 0.0344(4) Uani 1 1 d . . . H16A H 0.0204 -0.0877 0.4146 0.052 Uiso 1 1 calc R . . H16B H 0.0474 -0.1116 0.3257 0.052 Uiso 1 1 calc R . . H16C H 0.0120 -0.0270 0.3317 0.052 Uiso 1 1 calc R . . C17 C 0.32918(9) 0.05489(11) 0.22193(11) 0.0287(4) Uani 1 1 d . . . C18 C 0.37542(10) -0.01151(12) 0.22937(13) 0.0327(4) Uani 1 1 d . . . C19 C 0.41222(11) -0.02292(13) 0.15894(14) 0.0400(5) Uani 1 1 d . . . H19A H 0.4438 -0.0661 0.1624 0.048 Uiso 1 1 calc R . . C20 C 0.40266(12) 0.02867(15) 0.08432(14) 0.0452(5) Uani 1 1 d . . . H20A H 0.4274 0.0198 0.0377 0.054 Uiso 1 1 calc R . . C21 C 0.35651(11) 0.09350(14) 0.07851(14) 0.0421(5) Uani 1 1 d . . . H21A H 0.3502 0.1276 0.0275 0.051 Uiso 1 1 calc R . . C22 C 0.31914(10) 0.10892(12) 0.14786(12) 0.0327(4) Uani 1 1 d . . . C23 C 0.38578(11) -0.06743(14) 0.31088(14) 0.0423(5) Uani 1 1 d . . . H23A H 0.3400 -0.0870 0.3178 0.063 Uiso 1 1 calc R . . H23B H 0.4088 -0.0390 0.3659 0.063 Uiso 1 1 calc R . . H23C H 0.4152 -0.1121 0.3011 0.063 Uiso 1 1 calc R . . C24 C 0.27215(12) 0.18215(12) 0.14532(14) 0.0403(5) Uani 1 1 d . . . H24A H 0.2271 0.1665 0.1587 0.060 Uiso 1 1 calc R . . H24B H 0.2639 0.2062 0.0850 0.060 Uiso 1 1 calc R . . H24C H 0.2955 0.2204 0.1907 0.060 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 Mn1 0.02521(14) 0.02799(14) 0.01831(13) -0.00143(10) 0.00418(10) -0.00268(10) Cl1 0.0580(3) 0.0303(2) 0.0360(2) -0.00330(19) 0.0211(2) 0.0004(2) Cl2 0.0311(2) 0.0317(2) 0.0252(2) -0.00027(16) 0.00070(16) -0.00043(17) N1 0.0258(7) 0.0327(8) 0.0221(7) -0.0039(6) 0.0049(6) -0.0011(6) N2 0.0266(7) 0.0313(8) 0.0210(7) -0.0030(6) 0.0058(5) -0.0032(6) N3 0.0242(7) 0.0288(7) 0.0211(7) 0.0035(6) 0.0044(5) 0.0017(6) C1 0.0303(9) 0.0224(8) 0.0243(8) -0.0010(6) 0.0022(7) 0.0012(7) C2 0.0398(10) 0.0271(9) 0.0255(8) -0.0032(7) 0.0044(7) -0.0010(8) C3 0.0554(12) 0.0271(9) 0.0241(9) -0.0050(7) 0.0002(8) -0.0026(9) C4 0.0465(11) 0.0269(9) 0.0311(9) -0.0022(7) -0.0061(8) -0.0069(8) C5 0.0352(9) 0.0229(8) 0.0322(9) 0.0005(7) -0.0029(7) -0.0038(7) C6 0.0334(10) 0.0303(10) 0.0454(11) -0.0008(8) -0.0018(8) -0.0092(8) C7 0.0303(10) 0.0338(10) 0.0524(12) -0.0003(9) 0.0086(9) -0.0075(8) C8 0.0320(9) 0.0326(10) 0.0381(10) -0.0039(8) 0.0088(8) -0.0038(8) C9 0.0265(8) 0.0242(8) 0.0287(8) -0.0024(7) 0.0034(7) -0.0009(7) C10 0.0293(9) 0.0218(8) 0.0270(8) 0.0004(7) 0.0009(7) 0.0009(7) C11 0.0276(8) 0.0252(8) 0.0202(8) -0.0006(6) 0.0024(6) 0.0024(7) C12 0.0253(8) 0.0254(8) 0.0248(8) -0.0005(7) 0.0045(7) 0.0003(7) C13 0.0316(9) 0.0397(10) 0.0212(8) -0.0063(7) 0.0076(7) -0.0010(8) C14 0.0265(9) 0.0360(10) 0.0274(8) 0.0013(7) 0.0103(7) 0.0024(7) C15 0.0355(10) 0.0365(10) 0.0288(9) 0.0100(8) 0.0061(8) 0.0076(8) C16 0.0282(9) 0.0366(10) 0.0372(10) 0.0021(8) 0.0047(8) -0.0022(8) C17 0.0265(8) 0.0358(10) 0.0244(8) -0.0087(7) 0.0071(7) -0.0105(7) C18 0.0284(9) 0.0398(10) 0.0301(9) -0.0094(8) 0.0068(7) -0.0072(8) C19 0.0317(10) 0.0504(12) 0.0397(11) -0.0159(9) 0.0116(8) -0.0064(9) C20 0.0406(11) 0.0666(15) 0.0335(10) -0.0147(10) 0.0189(9) -0.0159(10) C21 0.0440(11) 0.0556(13) 0.0283(10) -0.0027(9) 0.0115(8) -0.0204(10) C22 0.0331(9) 0.0376(10) 0.0265(9) -0.0063(7) 0.0047(7) -0.0149(8) C23 0.0396(11) 0.0474(12) 0.0397(11) -0.0023(9) 0.0084(9) 0.0082(9) C24 0.0511(12) 0.0343(10) 0.0335(10) 0.0004(8) 0.0052(9) -0.0108(9) _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 Mn1 N1 2.2194(14) . ? Mn1 N3 2.3100(14) . ? Mn1 Cl1 2.3495(5) . ? Mn1 Cl2 2.3524(5) . ? Mn1 N2 2.3962(14) . ? N1 C11 1.273(2) . ? N1 C13 1.463(2) . ? N2 C12 1.281(2) . ? N2 C17 1.437(2) . ? N3 C16 1.473(2) . ? N3 C15 1.479(2) . ? N3 C14 1.481(2) . ? C1 C2 1.380(2) . ? C1 C10 1.416(2) . ? C1 C11 1.469(2) . ? C2 C3 1.417(3) . ? C3 C4 1.366(3) . ? C4 C5 1.424(3) . ? C5 C10 1.404(2) . ? C5 C6 1.412(3) . ? C6 C7 1.378(3) . ? C7 C8 1.417(3) . ? C8 C9 1.371(3) . ? C9 C10 1.419(2) . ? C9 C12 1.477(2) . ? C11 C12 1.512(2) . ? C13 C14 1.521(2) . ? C17 C22 1.397(3) . ? C17 C18 1.401(3) . ? C18 C19 1.394(3) . ? C18 C23 1.501(3) . ? C19 C20 1.378(3) . ? C20 C21 1.381(3) . ? C21 C22 1.398(3) . ? C22 C24 1.506(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Mn1 N3 72.86(5) . . ? N1 Mn1 Cl1 138.22(4) . . ? N3 Mn1 Cl1 94.44(4) . . ? N1 Mn1 Cl2 109.09(4) . . ? N3 Mn1 Cl2 107.44(4) . . ? Cl1 Mn1 Cl2 112.70(2) . . ? N1 Mn1 N2 72.03(5) . . ? N3 Mn1 N2 139.43(5) . . ? Cl1 Mn1 N2 98.32(4) . . ? Cl2 Mn1 N2 102.74(4) . . ? C11 N1 C13 121.73(14) . . ? C11 N1 Mn1 119.17(11) . . ? C13 N1 Mn1 119.03(11) . . ? C12 N2 C17 119.30(14) . . ? C12 N2 Mn1 112.37(11) . . ? C17 N2 Mn1 128.32(10) . . ? C16 N3 C15 108.56(14) . . ? C16 N3 C14 108.92(14) . . ? C15 N3 C14 110.61(14) . . ? C16 N3 Mn1 113.74(11) . . ? C15 N3 Mn1 108.50(10) . . ? C14 N3 Mn1 106.50(10) . . ? C2 C1 C10 119.56(16) . . ? C2 C1 C11 134.48(17) . . ? C10 C1 C11 105.95(14) . . ? C1 C2 C3 117.76(18) . . ? C4 C3 C2 122.99(18) . . ? C3 C4 C5 120.53(17) . . ? C10 C5 C6 116.44(17) . . ? C10 C5 C4 116.19(17) . . ? C6 C5 C4 127.35(17) . . ? C7 C6 C5 120.54(17) . . ? C6 C7 C8 122.41(18) . . ? C9 C8 C7 118.25(18) . . ? C8 C9 C10 119.41(16) . . ? C8 C9 C12 134.87(16) . . ? C10 C9 C12 105.72(15) . . ? C5 C10 C1 122.97(16) . . ? C5 C10 C9 122.92(17) . . ? C1 C10 C9 114.10(15) . . ? N1 C11 C1 134.93(16) . . ? N1 C11 C12 117.78(15) . . ? C1 C11 C12 107.26(14) . . ? N2 C12 C9 134.41(16) . . ? N2 C12 C11 118.56(15) . . ? C9 C12 C11 106.97(14) . . ? N1 C13 C14 108.78(14) . . ? N3 C14 C13 111.07(14) . . ? C22 C17 C18 122.74(16) . . ? C22 C17 N2 119.01(17) . . ? C18 C17 N2 118.23(16) . . ? C19 C18 C17 117.48(18) . . ? C19 C18 C23 121.32(19) . . ? C17 C18 C23 121.19(16) . . ? C20 C19 C18 121.1(2) . . ? C19 C20 C21 120.22(19) . . ? C20 C21 C22 121.3(2) . . ? C17 C22 C21 117.15(19) . . ? C17 C22 C24 120.97(17) . . ? C21 C22 C24 121.84(18) . . ? 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 N3 Mn1 N1 C11 161.47(15) . . . . ? Cl1 Mn1 N1 C11 84.39(14) . . . . ? Cl2 Mn1 N1 C11 -95.52(13) . . . . ? N2 Mn1 N1 C11 2.13(13) . . . . ? N3 Mn1 N1 C13 -15.58(12) . . . . ? Cl1 Mn1 N1 C13 -92.67(13) . . . . ? Cl2 Mn1 N1 C13 87.43(13) . . . . ? N2 Mn1 N1 C13 -174.93(14) . . . . ? N1 Mn1 N2 C12 -2.56(12) . . . . ? N3 Mn1 N2 C12 -33.79(16) . . . . ? Cl1 Mn1 N2 C12 -140.71(12) . . . . ? Cl2 Mn1 N2 C12 103.65(12) . . . . ? N1 Mn1 N2 C17 176.59(16) . . . . ? N3 Mn1 N2 C17 145.36(13) . . . . ? Cl1 Mn1 N2 C17 38.44(15) . . . . ? Cl2 Mn1 N2 C17 -77.21(15) . . . . ? N1 Mn1 N3 C16 154.89(13) . . . . ? Cl1 Mn1 N3 C16 -65.76(12) . . . . ? Cl2 Mn1 N3 C16 49.71(12) . . . . ? N2 Mn1 N3 C16 -174.04(11) . . . . ? N1 Mn1 N3 C15 -84.19(12) . . . . ? Cl1 Mn1 N3 C15 55.17(11) . . . . ? Cl2 Mn1 N3 C15 170.63(10) . . . . ? N2 Mn1 N3 C15 -53.12(14) . . . . ? N1 Mn1 N3 C14 34.91(10) . . . . ? Cl1 Mn1 N3 C14 174.26(10) . . . . ? Cl2 Mn1 N3 C14 -70.27(10) . . . . ? N2 Mn1 N3 C14 65.97(13) . . . . ? C10 C1 C2 C3 0.4(3) . . . . ? C11 C1 C2 C3 179.64(18) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? C2 C3 C4 C5 -0.3(3) . . . . ? C3 C4 C5 C10 0.8(3) . . . . ? C3 C4 C5 C6 179.23(19) . . . . ? C10 C5 C6 C7 0.0(3) . . . . ? C4 C5 C6 C7 -178.38(19) . . . . ? C5 C6 C7 C8 -1.1(3) . . . . ? C6 C7 C8 C9 1.2(3) . . . . ? C7 C8 C9 C10 -0.2(3) . . . . ? C7 C8 C9 C12 180.00(19) . . . . ? C6 C5 C10 C1 -179.41(17) . . . . ? C4 C5 C10 C1 -0.8(3) . . . . ? C6 C5 C10 C9 1.0(3) . . . . ? C4 C5 C10 C9 179.60(16) . . . . ? C2 C1 C10 C5 0.2(3) . . . . ? C11 C1 C10 C5 -179.22(16) . . . . ? C2 C1 C10 C9 179.84(16) . . . . ? C11 C1 C10 C9 0.4(2) . . . . ? C8 C9 C10 C5 -1.0(3) . . . . ? C12 C9 C10 C5 178.92(16) . . . . ? C8 C9 C10 C1 179.44(16) . . . . ? C12 C9 C10 C1 -0.7(2) . . . . ? C13 N1 C11 C1 -2.1(3) . . . . ? Mn1 N1 C11 C1 -179.07(15) . . . . ? C13 N1 C11 C12 175.46(15) . . . . ? Mn1 N1 C11 C12 -1.5(2) . . . . ? C2 C1 C11 N1 -1.5(4) . . . . ? C10 C1 C11 N1 177.8(2) . . . . ? C2 C1 C11 C12 -179.27(19) . . . . ? C10 C1 C11 C12 0.09(18) . . . . ? C17 N2 C12 C9 0.3(3) . . . . ? Mn1 N2 C12 C9 179.56(16) . . . . ? C17 N2 C12 C11 -176.46(15) . . . . ? Mn1 N2 C12 C11 2.77(19) . . . . ? C8 C9 C12 N2 3.5(4) . . . . ? C10 C9 C12 N2 -176.36(19) . . . . ? C8 C9 C12 C11 -179.5(2) . . . . ? C10 C9 C12 C11 0.69(18) . . . . ? N1 C11 C12 N2 -1.1(2) . . . . ? C1 C11 C12 N2 177.11(15) . . . . ? N1 C11 C12 C9 -178.68(15) . . . . ? C1 C11 C12 C9 -0.49(18) . . . . ? C11 N1 C13 C14 176.09(16) . . . . ? Mn1 N1 C13 C14 -6.94(19) . . . . ? C16 N3 C14 C13 -174.66(14) . . . . ? C15 N3 C14 C13 66.11(18) . . . . ? Mn1 N3 C14 C13 -51.61(15) . . . . ? N1 C13 C14 N3 39.3(2) . . . . ? C12 N2 C17 C22 -90.9(2) . . . . ? Mn1 N2 C17 C22 90.02(18) . . . . ? C12 N2 C17 C18 90.6(2) . . . . ? Mn1 N2 C17 C18 -88.48(18) . . . . ? C22 C17 C18 C19 -0.1(3) . . . . ? N2 C17 C18 C19 178.31(16) . . . . ? C22 C17 C18 C23 178.91(17) . . . . ? N2 C17 C18 C23 -2.6(2) . . . . ? C17 C18 C19 C20 -0.8(3) . . . . ? C23 C18 C19 C20 -179.87(19) . . . . ? C18 C19 C20 C21 0.6(3) . . . . ? C19 C20 C21 C22 0.6(3) . . . . ? C18 C17 C22 C21 1.3(3) . . . . ? N2 C17 C22 C21 -177.16(15) . . . . ? C18 C17 C22 C24 -176.48(17) . . . . ? N2 C17 C22 C24 5.1(2) . . . . ? C20 C21 C22 C17 -1.5(3) . . . . ? C20 C21 C22 C24 176.22(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.248 _refine_diff_density_min -0.284 _refine_diff_density_rms 0.050 #===END data_(3g)FeCl2 _database_code_depnum_ccdc_archive 'CCDC 636872' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040028 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H43 Cl2 Fe N4 P' _chemical_formula_weight 761.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 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 10.690(2) _cell_length_b 30.399(6) _cell_length_c 11.998(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3898.9(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.07 _cell_measurement_theta_max 14.50 _exptl_crystal_description rod _exptl_crystal_colour green _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.600 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.839 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7128 _diffrn_reflns_av_R_equivalents 0.0719 _diffrn_reflns_av_sigmaI/netI 0.0917 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3609 _reflns_number_gt 2575 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0387P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _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 -0.04(3) _refine_ls_number_reflns 3609 _refine_ls_number_parameters 453 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0855 _refine_ls_R_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.1044 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 Fe1 Fe 1.40031(8) -0.05529(3) 1.31086(9) 0.0209(2) Uani 1 1 d . . . P1 P 1.30197(16) 0.01713(6) 1.26657(16) 0.0239(4) Uani 1 1 d . . . N1 N 1.3804(5) -0.05344(19) 1.1300(5) 0.0210(14) Uani 1 1 d . . . N2 N 1.3640(5) -0.12307(18) 1.2654(5) 0.0224(13) Uani 1 1 d . . . Cl1 Cl 1.33621(18) -0.06480(6) 1.49110(15) 0.0311(5) Uani 1 1 d . . . Cl2 Cl 1.60851(15) -0.03499(5) 1.30022(18) 0.0315(4) Uani 1 1 d . . . C1 C 1.3544(6) -0.1078(2) 0.9699(6) 0.0224(16) Uani 1 1 d . . . C2 C 1.3508(7) -0.0893(2) 0.8672(6) 0.0299(18) Uani 1 1 d . . . H2A H 1.3555 -0.0589 0.8591 0.036 Uiso 1 1 calc R . . C3 C 1.3396(7) -0.1167(3) 0.7728(6) 0.0352(19) Uani 1 1 d . . . H3A H 1.3349 -0.1039 0.7025 0.042 Uiso 1 1 calc R . . C4 C 1.3356(7) -0.1618(3) 0.7824(6) 0.038(2) Uani 1 1 d . . . H4A H 1.3308 -0.1791 0.7186 0.046 Uiso 1 1 calc R . . C5 C 1.3385(7) -0.1818(2) 0.8882(6) 0.0303(19) Uani 1 1 d . . . C6 C 1.3372(8) -0.2280(3) 0.9096(7) 0.039(2) Uani 1 1 d . . . H6A H 1.3305 -0.2478 0.8509 0.047 Uiso 1 1 calc R . . C7 C 1.3459(8) -0.2429(2) 1.0170(7) 0.040(2) Uani 1 1 d . . . H7A H 1.3467 -0.2731 1.0295 0.048 Uiso 1 1 calc R . . C8 C 1.3538(7) -0.2144(2) 1.1097(7) 0.031(2) Uani 1 1 d . . . H8A H 1.3587 -0.2254 1.1819 0.037 Uiso 1 1 calc R . . C9 C 1.3539(6) -0.1699(2) 1.0895(6) 0.0233(17) Uani 1 1 d . . . C10 C 1.3482(6) -0.1542(2) 0.9791(6) 0.0204(15) Uani 1 1 d . . . C11 C 1.3679(6) -0.0917(2) 1.0823(6) 0.0195(16) Uani 1 1 d . . . C12 C 1.3625(6) -0.1302(2) 1.1604(6) 0.0208(16) Uani 1 1 d . . . C13 C 1.3781(6) -0.0136(2) 1.0630(6) 0.0247(16) Uani 1 1 d . . . H13A H 1.3019 -0.0130 1.0192 0.030 Uiso 1 1 calc R . . H13B H 1.4485 -0.0139 1.0119 0.030 Uiso 1 1 calc R . . C14 C 1.3847(7) 0.0275(2) 1.1356(6) 0.0284(18) Uani 1 1 d . . . H14A H 1.3466 0.0521 1.0970 0.034 Uiso 1 1 calc R . . H14B H 1.4714 0.0348 1.1508 0.034 Uiso 1 1 calc R . . C15 C 1.3182(6) 0.0671(2) 1.3502(6) 0.0264(17) Uani 1 1 d . . . C16 C 1.3141(6) 0.0628(2) 1.4648(6) 0.0301(18) Uani 1 1 d . . . H16A H 1.3064 0.0351 1.4966 0.036 Uiso 1 1 calc R . . C17 C 1.3212(7) 0.0992(3) 1.5318(7) 0.037(2) Uani 1 1 d . . . H17A H 1.3193 0.0959 1.6088 0.044 Uiso 1 1 calc R . . C18 C 1.3310(8) 0.1405(3) 1.4858(8) 0.039(2) Uani 1 1 d . . . H18A H 1.3348 0.1652 1.5316 0.047 Uiso 1 1 calc R . . C19 C 1.3353(7) 0.1453(3) 1.3729(8) 0.040(2) Uani 1 1 d . . . H19A H 1.3430 0.1732 1.3419 0.048 Uiso 1 1 calc R . . C20 C 1.3282(6) 0.1089(2) 1.3044(8) 0.0384(18) Uani 1 1 d . . . H20A H 1.3301 0.1124 1.2274 0.046 Uiso 1 1 calc R . . C21 C 1.1353(5) 0.0162(2) 1.2304(6) 0.0237(16) Uani 1 1 d . . . C22 C 1.0825(8) 0.0455(3) 1.1588(8) 0.051(2) Uani 1 1 d . . . H22A H 1.1317 0.0669 1.1249 0.061 Uiso 1 1 calc R . . C23 C 0.9526(8) 0.0435(3) 1.1357(8) 0.050(3) Uani 1 1 d . . . H23A H 0.9172 0.0628 1.0844 0.061 Uiso 1 1 calc R . . C24 C 0.8794(7) 0.0133(3) 1.1888(7) 0.043(2) Uani 1 1 d . . . H24A H 0.7934 0.0129 1.1771 0.052 Uiso 1 1 calc R . . C25 C 0.9332(7) -0.0162(3) 1.2589(9) 0.061(3) Uani 1 1 d . . . H25A H 0.8841 -0.0378 1.2922 0.073 Uiso 1 1 calc R . . C26 C 1.0619(7) -0.0146(3) 1.2817(8) 0.051(3) Uani 1 1 d . . . H26A H 1.0972 -0.0345 1.3315 0.062 Uiso 1 1 calc R . . C27 C 1.3489(7) -0.1588(2) 1.3421(5) 0.0247(17) Uani 1 1 d . . . C28 C 1.2311(7) -0.1764(2) 1.3629(6) 0.0340(19) Uani 1 1 d . . . C29 C 1.2225(7) -0.2091(2) 1.4436(7) 0.038(2) Uani 1 1 d . . . H29A H 1.1445 -0.2212 1.4595 0.046 Uiso 1 1 calc R . . C30 C 1.3244(9) -0.2240(3) 1.4999(7) 0.042(2) Uani 1 1 d . . . H30A H 1.3154 -0.2461 1.5527 0.050 Uiso 1 1 calc R . . C31 C 1.4409(8) -0.2065(2) 1.4794(7) 0.0362(19) Uani 1 1 d . . . H31A H 1.5098 -0.2171 1.5184 0.043 Uiso 1 1 calc R . . C32 C 1.4569(7) -0.1733(2) 1.4013(6) 0.0259(17) Uani 1 1 d . . . C33 C 1.1141(7) -0.1598(2) 1.3046(9) 0.0403(18) Uani 1 1 d . . . H33A H 1.1399 -0.1391 1.2462 0.048 Uiso 1 1 calc R . . C34 C 1.0305(9) -0.1345(3) 1.3882(9) 0.067(3) Uani 1 1 d . . . H34A H 1.0777 -0.1110 1.4214 0.101 Uiso 1 1 calc R . . H34B H 1.0023 -0.1543 1.4453 0.101 Uiso 1 1 calc R . . H34C H 0.9595 -0.1225 1.3497 0.101 Uiso 1 1 calc R . . C35 C 1.0385(8) -0.1963(3) 1.2500(9) 0.062(3) Uani 1 1 d . . . H35A H 1.0901 -0.2116 1.1972 0.094 Uiso 1 1 calc R . . H35B H 0.9677 -0.1839 1.2124 0.094 Uiso 1 1 calc R . . H35C H 1.0103 -0.2166 1.3061 0.094 Uiso 1 1 calc R . . C36 C 1.5837(7) -0.1528(2) 1.3789(7) 0.0341(19) Uani 1 1 d . . . H36A H 1.5695 -0.1235 1.3472 0.041 Uiso 1 1 calc R . . C37 C 1.6606(9) -0.1470(3) 1.4855(9) 0.064(3) Uani 1 1 d . . . H37A H 1.6137 -0.1300 1.5384 0.096 Uiso 1 1 calc R . . H37B H 1.7373 -0.1320 1.4683 0.096 Uiso 1 1 calc R . . H37C H 1.6792 -0.1753 1.5166 0.096 Uiso 1 1 calc R . . C38 C 1.6551(7) -0.1796(3) 1.2932(7) 0.054(2) Uani 1 1 d . . . H38A H 1.6059 -0.1823 1.2266 0.080 Uiso 1 1 calc R . . H38B H 1.6718 -0.2084 1.3227 0.080 Uiso 1 1 calc R . . H38C H 1.7327 -0.1653 1.2761 0.080 Uiso 1 1 calc R . . C1S C 1.4908(14) -0.3233(5) 1.7242(16) 0.140(6) Uani 1 1 d . . . H1SA H 1.5018 -0.3348 1.7981 0.209 Uiso 1 1 calc R . . H1SB H 1.5240 -0.3437 1.6709 0.209 Uiso 1 1 calc R . . H1SC H 1.4033 -0.3189 1.7101 0.209 Uiso 1 1 calc R . . C2S C 1.5561(12) -0.2816(5) 1.7144(11) 0.075(4) Uani 1 1 d . . . N1S N 1.6039(10) -0.2487(4) 1.7104(9) 0.084(3) Uani 1 1 d . . . C3S C 1.5290(11) -0.4358(4) 1.9869(14) 0.105(5) Uani 1 1 d . . . H3SA H 1.5529 -0.4470 2.0586 0.157 Uiso 1 1 calc R . . H3SB H 1.5895 -0.4446 1.9322 0.157 Uiso 1 1 calc R . . H3SC H 1.4483 -0.4472 1.9670 0.157 Uiso 1 1 calc R . . C4S C 1.5232(11) -0.3877(5) 1.9915(12) 0.088(4) Uani 1 1 d . . . N2S N 1.5180(12) -0.3502(4) 1.9923(14) 0.133(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0171(4) 0.0230(4) 0.0227(5) 0.0004(6) 0.0002(5) -0.0019(4) P1 0.0193(9) 0.0266(10) 0.0259(10) 0.0021(8) 0.0005(8) 0.0002(8) N1 0.012(3) 0.025(3) 0.026(3) 0.006(3) 0.003(2) 0.002(3) N2 0.013(3) 0.030(3) 0.024(3) 0.006(3) -0.001(2) -0.009(2) Cl1 0.0323(10) 0.0390(11) 0.0220(10) -0.0004(9) 0.0032(9) -0.0009(10) Cl2 0.0197(8) 0.0373(9) 0.0374(11) -0.0053(11) 0.0025(10) -0.0063(8) C1 0.014(3) 0.038(4) 0.016(4) -0.001(3) -0.003(3) -0.001(3) C2 0.026(4) 0.031(4) 0.033(5) -0.001(4) 0.003(4) -0.001(4) C3 0.032(4) 0.050(5) 0.024(4) 0.006(4) 0.003(4) -0.003(4) C4 0.035(4) 0.060(5) 0.020(5) -0.013(4) 0.001(4) -0.008(4) C5 0.031(5) 0.036(5) 0.024(4) -0.008(4) 0.005(4) -0.005(4) C6 0.037(5) 0.041(5) 0.039(5) -0.018(4) 0.000(4) -0.009(4) C7 0.047(5) 0.032(5) 0.040(5) -0.008(4) -0.005(4) -0.003(4) C8 0.031(5) 0.031(5) 0.031(4) 0.004(4) -0.006(4) 0.007(4) C9 0.017(4) 0.020(4) 0.033(4) 0.000(3) 0.007(3) 0.001(3) C10 0.013(3) 0.023(4) 0.026(4) -0.002(3) 0.002(3) -0.003(3) C11 0.004(3) 0.028(4) 0.027(4) 0.001(3) 0.000(3) 0.003(3) C12 0.007(3) 0.027(4) 0.028(4) 0.000(3) -0.001(3) -0.003(3) C13 0.021(4) 0.027(4) 0.026(4) 0.003(3) -0.003(3) -0.006(3) C14 0.028(4) 0.031(4) 0.026(4) 0.003(3) -0.003(4) -0.002(3) C15 0.019(4) 0.027(4) 0.034(5) 0.001(3) 0.000(3) 0.003(3) C16 0.029(4) 0.033(4) 0.029(5) 0.004(4) -0.004(4) 0.004(3) C17 0.027(5) 0.055(6) 0.028(4) -0.012(4) 0.000(4) 0.002(4) C18 0.035(5) 0.036(5) 0.047(5) -0.014(4) -0.007(4) 0.013(4) C19 0.032(5) 0.028(4) 0.059(6) -0.002(4) -0.009(5) 0.005(4) C20 0.038(4) 0.039(4) 0.038(5) 0.000(5) -0.008(5) 0.001(3) C21 0.014(3) 0.031(4) 0.026(4) 0.006(3) -0.004(3) -0.003(3) C22 0.031(5) 0.059(6) 0.062(6) 0.030(5) -0.013(4) -0.015(4) C23 0.026(4) 0.073(7) 0.052(6) 0.020(5) -0.004(4) 0.003(5) C24 0.023(4) 0.054(5) 0.052(6) 0.008(4) -0.003(4) 0.000(4) C25 0.023(4) 0.063(6) 0.097(8) 0.033(6) 0.001(5) -0.016(4) C26 0.029(4) 0.053(5) 0.072(7) 0.032(5) -0.002(5) -0.001(4) C27 0.033(4) 0.023(4) 0.019(4) 0.001(3) -0.001(3) 0.002(3) C28 0.035(5) 0.036(4) 0.031(4) 0.010(4) 0.002(4) -0.006(4) C29 0.034(5) 0.044(5) 0.037(5) 0.009(4) 0.012(4) -0.010(4) C30 0.065(7) 0.030(5) 0.031(5) 0.014(4) 0.004(5) -0.004(5) C31 0.041(5) 0.030(4) 0.038(5) 0.004(4) -0.001(4) 0.005(4) C32 0.032(4) 0.020(4) 0.026(4) -0.002(3) -0.005(3) -0.001(3) C33 0.028(4) 0.043(4) 0.050(5) 0.011(5) -0.003(5) -0.013(4) C34 0.042(6) 0.063(7) 0.097(9) -0.017(6) 0.005(6) -0.004(5) C35 0.037(5) 0.074(7) 0.075(7) -0.010(6) -0.013(5) -0.009(5) C36 0.030(5) 0.027(4) 0.045(5) 0.002(4) -0.007(4) 0.003(4) C37 0.046(6) 0.077(7) 0.068(7) -0.018(6) -0.018(6) -0.011(6) C38 0.042(5) 0.081(6) 0.038(6) -0.001(5) 0.011(5) -0.015(4) C1S 0.111(13) 0.119(13) 0.19(2) -0.002(14) -0.002(13) -0.006(10) C2S 0.074(9) 0.095(10) 0.056(7) 0.011(8) 0.012(7) 0.036(8) N1S 0.098(8) 0.100(7) 0.054(6) -0.001(7) -0.004(6) 0.036(7) C3S 0.048(7) 0.106(11) 0.161(15) 0.030(11) -0.028(9) 0.000(8) C4S 0.061(8) 0.105(11) 0.096(10) -0.028(11) 0.002(7) 0.002(8) N2S 0.103(10) 0.121(11) 0.176(14) -0.044(12) 0.000(10) 0.011(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.166(6) . ? Fe1 N1 2.181(6) . ? Fe1 Cl1 2.287(2) . ? Fe1 Cl2 2.3131(18) . ? Fe1 P1 2.497(2) . ? P1 C15 1.829(7) . ? P1 C14 1.830(7) . ? P1 C21 1.834(6) . ? N1 C11 1.304(9) . ? N1 C13 1.453(9) . ? N2 C12 1.278(9) . ? N2 C27 1.432(8) . ? C1 C2 1.355(10) . ? C1 C10 1.414(9) . ? C1 C11 1.441(9) . ? C2 C3 1.410(10) . ? C3 C4 1.377(11) . ? C4 C5 1.409(11) . ? C5 C10 1.381(9) . ? C5 C6 1.426(10) . ? C6 C7 1.369(11) . ? C7 C8 1.410(10) . ? C8 C9 1.376(10) . ? C9 C10 1.410(10) . ? C9 C12 1.479(10) . ? C11 C12 1.499(10) . ? C13 C14 1.525(9) . ? C15 C16 1.382(10) . ? C15 C20 1.388(9) . ? C16 C17 1.368(10) . ? C17 C18 1.377(11) . ? C18 C19 1.363(12) . ? C19 C20 1.379(11) . ? C21 C22 1.361(10) . ? C21 C26 1.369(10) . ? C22 C23 1.417(12) . ? C23 C24 1.365(11) . ? C24 C25 1.357(11) . ? C25 C26 1.404(10) . ? C27 C28 1.390(10) . ? C27 C32 1.425(10) . ? C28 C29 1.392(10) . ? C28 C33 1.520(10) . ? C29 C30 1.360(11) . ? C30 C31 1.376(12) . ? C31 C32 1.389(10) . ? C32 C36 1.516(10) . ? C33 C35 1.522(11) . ? C33 C34 1.547(12) . ? C36 C38 1.519(11) . ? C36 C37 1.530(12) . ? C1S C2S 1.451(16) . ? C2S N1S 1.125(14) . ? C3S C4S 1.464(16) . ? C4S N2S 1.140(15) . ? 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 Fe1 N1 75.9(2) . . ? N2 Fe1 Cl1 93.68(16) . . ? N1 Fe1 Cl1 156.17(16) . . ? N2 Fe1 Cl2 114.34(15) . . ? N1 Fe1 Cl2 91.85(16) . . ? Cl1 Fe1 Cl2 111.98(8) . . ? N2 Fe1 P1 135.20(16) . . ? N1 Fe1 P1 74.01(16) . . ? Cl1 Fe1 P1 100.76(7) . . ? Cl2 Fe1 P1 99.10(7) . . ? C15 P1 C14 106.4(3) . . ? C15 P1 C21 103.6(3) . . ? C14 P1 C21 105.6(3) . . ? C15 P1 Fe1 125.2(2) . . ? C14 P1 Fe1 97.5(2) . . ? C21 P1 Fe1 116.5(2) . . ? C11 N1 C13 119.9(6) . . ? C11 N1 Fe1 115.1(5) . . ? C13 N1 Fe1 125.0(4) . . ? C12 N2 C27 120.3(6) . . ? C12 N2 Fe1 114.3(5) . . ? C27 N2 Fe1 125.4(4) . . ? C2 C1 C10 118.9(7) . . ? C2 C1 C11 135.4(7) . . ? C10 C1 C11 105.7(6) . . ? C1 C2 C3 119.2(7) . . ? C4 C3 C2 121.5(7) . . ? C3 C4 C5 120.4(7) . . ? C10 C5 C4 116.7(7) . . ? C10 C5 C6 117.2(7) . . ? C4 C5 C6 126.0(7) . . ? C7 C6 C5 119.6(7) . . ? C6 C7 C8 122.9(7) . . ? C9 C8 C7 117.7(7) . . ? C8 C9 C10 119.9(7) . . ? C8 C9 C12 134.6(7) . . ? C10 C9 C12 105.5(6) . . ? C5 C10 C9 122.6(6) . . ? C5 C10 C1 123.2(7) . . ? C9 C10 C1 114.1(6) . . ? N1 C11 C1 136.4(7) . . ? N1 C11 C12 115.1(6) . . ? C1 C11 C12 108.5(6) . . ? N2 C12 C9 134.9(7) . . ? N2 C12 C11 118.9(6) . . ? C9 C12 C11 106.2(6) . . ? N1 C13 C14 111.4(6) . . ? C13 C14 P1 109.1(5) . . ? C16 C15 C20 118.9(7) . . ? C16 C15 P1 117.6(5) . . ? C20 C15 P1 123.4(6) . . ? C17 C16 C15 120.4(7) . . ? C16 C17 C18 120.4(8) . . ? C19 C18 C17 119.8(8) . . ? C18 C19 C20 120.4(8) . . ? C19 C20 C15 120.1(9) . . ? C22 C21 C26 119.6(6) . . ? C22 C21 P1 122.9(5) . . ? C26 C21 P1 117.4(5) . . ? C21 C22 C23 120.1(7) . . ? C24 C23 C22 120.0(8) . . ? C25 C24 C23 119.4(8) . . ? C24 C25 C26 120.9(8) . . ? C21 C26 C25 119.9(8) . . ? C28 C27 C32 121.7(6) . . ? C28 C27 N2 120.6(6) . . ? C32 C27 N2 117.6(6) . . ? C27 C28 C29 117.4(7) . . ? C27 C28 C33 122.4(6) . . ? C29 C28 C33 120.2(7) . . ? C30 C29 C28 122.0(7) . . ? C29 C30 C31 120.6(7) . . ? C30 C31 C32 120.9(8) . . ? C31 C32 C27 117.5(7) . . ? C31 C32 C36 121.9(7) . . ? C27 C32 C36 120.6(6) . . ? C28 C33 C35 113.1(6) . . ? C28 C33 C34 110.0(8) . . ? C35 C33 C34 109.6(7) . . ? C32 C36 C38 110.4(6) . . ? C32 C36 C37 112.3(7) . . ? C38 C36 C37 110.9(7) . . ? N1S C2S C1S 177.1(15) . . ? N2S C4S C3S 178.3(18) . . ? 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 Fe1 P1 C15 158.7(3) . . . . ? N1 Fe1 P1 C15 -151.7(3) . . . . ? Cl1 Fe1 P1 C15 52.2(3) . . . . ? Cl2 Fe1 P1 C15 -62.4(3) . . . . ? N2 Fe1 P1 C14 -85.1(3) . . . . ? N1 Fe1 P1 C14 -35.6(3) . . . . ? Cl1 Fe1 P1 C14 168.4(2) . . . . ? Cl2 Fe1 P1 C14 53.8(2) . . . . ? N2 Fe1 P1 C21 26.5(4) . . . . ? N1 Fe1 P1 C21 76.1(3) . . . . ? Cl1 Fe1 P1 C21 -80.0(3) . . . . ? Cl2 Fe1 P1 C21 165.4(3) . . . . ? N2 Fe1 N1 C11 -5.4(4) . . . . ? Cl1 Fe1 N1 C11 -71.5(6) . . . . ? Cl2 Fe1 N1 C11 109.3(4) . . . . ? P1 Fe1 N1 C11 -151.8(5) . . . . ? N2 Fe1 N1 C13 173.5(5) . . . . ? Cl1 Fe1 N1 C13 107.4(6) . . . . ? Cl2 Fe1 N1 C13 -71.8(5) . . . . ? P1 Fe1 N1 C13 27.1(5) . . . . ? N1 Fe1 N2 C12 7.2(5) . . . . ? Cl1 Fe1 N2 C12 165.4(5) . . . . ? Cl2 Fe1 N2 C12 -78.4(5) . . . . ? P1 Fe1 N2 C12 56.2(6) . . . . ? N1 Fe1 N2 C27 -176.1(6) . . . . ? Cl1 Fe1 N2 C27 -17.8(5) . . . . ? Cl2 Fe1 N2 C27 98.3(5) . . . . ? P1 Fe1 N2 C27 -127.1(5) . . . . ? C10 C1 C2 C3 0.6(11) . . . . ? C11 C1 C2 C3 178.1(7) . . . . ? C1 C2 C3 C4 -1.7(11) . . . . ? C2 C3 C4 C5 2.0(12) . . . . ? C3 C4 C5 C10 -1.3(12) . . . . ? C3 C4 C5 C6 -178.8(7) . . . . ? C10 C5 C6 C7 -0.2(13) . . . . ? C4 C5 C6 C7 177.2(8) . . . . ? C5 C6 C7 C8 1.3(14) . . . . ? C6 C7 C8 C9 -0.7(13) . . . . ? C7 C8 C9 C10 -1.0(11) . . . . ? C7 C8 C9 C12 -178.8(8) . . . . ? C4 C5 C10 C9 -179.1(7) . . . . ? C6 C5 C10 C9 -1.4(11) . . . . ? C4 C5 C10 C1 0.3(11) . . . . ? C6 C5 C10 C1 178.0(7) . . . . ? C8 C9 C10 C5 2.1(11) . . . . ? C12 C9 C10 C5 -179.5(7) . . . . ? C8 C9 C10 C1 -177.4(7) . . . . ? C12 C9 C10 C1 1.0(8) . . . . ? C2 C1 C10 C5 0.0(11) . . . . ? C11 C1 C10 C5 -178.2(7) . . . . ? C2 C1 C10 C9 179.5(6) . . . . ? C11 C1 C10 C9 1.3(8) . . . . ? C13 N1 C11 C1 2.3(11) . . . . ? Fe1 N1 C11 C1 -178.7(6) . . . . ? C13 N1 C11 C12 -175.9(5) . . . . ? Fe1 N1 C11 C12 3.1(7) . . . . ? C2 C1 C11 N1 0.9(14) . . . . ? C10 C1 C11 N1 178.7(7) . . . . ? C2 C1 C11 C12 179.2(8) . . . . ? C10 C1 C11 C12 -3.0(7) . . . . ? C27 N2 C12 C9 -3.6(12) . . . . ? Fe1 N2 C12 C9 173.3(6) . . . . ? C27 N2 C12 C11 175.0(6) . . . . ? Fe1 N2 C12 C11 -8.1(8) . . . . ? C8 C9 C12 N2 -6.0(15) . . . . ? C10 C9 C12 N2 175.9(8) . . . . ? C8 C9 C12 C11 175.3(8) . . . . ? C10 C9 C12 C11 -2.8(7) . . . . ? N1 C11 C12 N2 3.4(9) . . . . ? C1 C11 C12 N2 -175.3(6) . . . . ? N1 C11 C12 C9 -177.6(5) . . . . ? C1 C11 C12 C9 3.7(7) . . . . ? C11 N1 C13 C14 175.9(6) . . . . ? Fe1 N1 C13 C14 -3.0(7) . . . . ? N1 C13 C14 P1 -33.9(7) . . . . ? C15 P1 C14 C13 178.3(5) . . . . ? C21 P1 C14 C13 -72.1(5) . . . . ? Fe1 P1 C14 C13 48.2(5) . . . . ? C14 P1 C15 C16 -152.7(6) . . . . ? C21 P1 C15 C16 96.3(6) . . . . ? Fe1 P1 C15 C16 -40.7(6) . . . . ? C14 P1 C15 C20 30.6(7) . . . . ? C21 P1 C15 C20 -80.5(6) . . . . ? Fe1 P1 C15 C20 142.5(5) . . . . ? C20 C15 C16 C17 -0.7(11) . . . . ? P1 C15 C16 C17 -177.7(6) . . . . ? C15 C16 C17 C18 0.8(12) . . . . ? C16 C17 C18 C19 -0.8(13) . . . . ? C17 C18 C19 C20 0.8(13) . . . . ? C18 C19 C20 C15 -0.8(12) . . . . ? C16 C15 C20 C19 0.8(10) . . . . ? P1 C15 C20 C19 177.5(6) . . . . ? C15 P1 C21 C22 69.5(8) . . . . ? C14 P1 C21 C22 -42.1(8) . . . . ? Fe1 P1 C21 C22 -149.0(6) . . . . ? C15 P1 C21 C26 -108.2(7) . . . . ? C14 P1 C21 C26 140.2(6) . . . . ? Fe1 P1 C21 C26 33.3(7) . . . . ? C26 C21 C22 C23 -1.3(14) . . . . ? P1 C21 C22 C23 -178.9(7) . . . . ? C21 C22 C23 C24 2.6(15) . . . . ? C22 C23 C24 C25 -3.6(15) . . . . ? C23 C24 C25 C26 3.3(15) . . . . ? C22 C21 C26 C25 0.9(14) . . . . ? P1 C21 C26 C25 178.7(8) . . . . ? C24 C25 C26 C21 -1.9(16) . . . . ? C12 N2 C27 C28 -77.8(9) . . . . ? Fe1 N2 C27 C28 105.6(7) . . . . ? C12 N2 C27 C32 106.3(8) . . . . ? Fe1 N2 C27 C32 -70.2(7) . . . . ? C32 C27 C28 C29 -0.4(11) . . . . ? N2 C27 C28 C29 -176.0(6) . . . . ? C32 C27 C28 C33 177.0(7) . . . . ? N2 C27 C28 C33 1.3(11) . . . . ? C27 C28 C29 C30 -0.7(12) . . . . ? C33 C28 C29 C30 -178.1(8) . . . . ? C28 C29 C30 C31 0.8(13) . . . . ? C29 C30 C31 C32 0.2(13) . . . . ? C30 C31 C32 C27 -1.2(11) . . . . ? C30 C31 C32 C36 178.7(7) . . . . ? C28 C27 C32 C31 1.3(11) . . . . ? N2 C27 C32 C31 177.1(6) . . . . ? C28 C27 C32 C36 -178.6(7) . . . . ? N2 C27 C32 C36 -2.8(10) . . . . ? C27 C28 C33 C35 127.6(8) . . . . ? C29 C28 C33 C35 -55.1(11) . . . . ? C27 C28 C33 C34 -109.5(9) . . . . ? C29 C28 C33 C34 67.8(9) . . . . ? C31 C32 C36 C38 85.9(9) . . . . ? C27 C32 C36 C38 -94.2(8) . . . . ? C31 C32 C36 C37 -38.4(10) . . . . ? C27 C32 C36 C37 141.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.592 _refine_diff_density_min -0.452 _refine_diff_density_rms 0.074 #===END data_(1a)FeCl2 _database_code_depnum_ccdc_archive 'CCDC 636873' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040029 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H25 Cl2 Fe N3 S' _chemical_formula_weight 562.32 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 38.587(6) _cell_length_b 38.587(6) _cell_length_c 10.062(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 12975(4) _cell_formula_units_Z 18 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8.92 _cell_measurement_theta_max 14.52 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.295 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5220 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.7400 _exptl_absorpt_correction_T_max 0.9242 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 5914 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.1355 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 41 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.98 _reflns_number_total 5649 _reflns_number_gt 2587 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1154P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5649 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1886 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2550 _refine_ls_wR_factor_gt 0.2008 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _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 Fe1 Fe 0.37826(3) 0.10654(3) 0.05451(11) 0.0453(3) Uani 1 1 d . . . Cl1 Cl 0.42594(7) 0.12123(7) 0.2118(2) 0.0650(6) Uani 1 1 d . . . Cl2 Cl 0.38015(6) 0.06715(6) -0.11352(19) 0.0556(6) Uani 1 1 d . . . S1 S 0.45436(8) 0.24727(8) 0.0882(3) 0.0800(8) Uani 1 1 d . . . N1 N 0.33292(18) 0.11787(18) -0.0045(6) 0.0452(15) Uani 1 1 d . . . N2 N 0.41015(19) 0.16471(18) -0.0504(6) 0.0478(16) Uani 1 1 d . . . N3 N 0.32466(19) 0.06177(17) 0.1649(6) 0.0458(15) Uani 1 1 d . . . C1 C 0.3210(3) 0.1670(2) -0.1377(8) 0.050(2) Uani 1 1 d . . . C2 C 0.2825(3) 0.1586(3) -0.1430(9) 0.060(2) Uani 1 1 d . . . H2A H 0.2627 0.1366 -0.0976 0.072 Uiso 1 1 calc R . . C3 C 0.2727(4) 0.1827(3) -0.2158(10) 0.081(3) Uani 1 1 d . . . H3A H 0.2461 0.1764 -0.2200 0.097 Uiso 1 1 calc R . . C4 C 0.3011(4) 0.2156(3) -0.2820(9) 0.071(3) Uani 1 1 d . . . H4A H 0.2934 0.2313 -0.3301 0.085 Uiso 1 1 calc R . . C5 C 0.3410(3) 0.2261(3) -0.2789(7) 0.060(2) Uani 1 1 d . . . C6 C 0.3744(4) 0.2595(3) -0.3366(9) 0.076(3) Uani 1 1 d . . . H6A H 0.3700 0.2770 -0.3881 0.092 Uiso 1 1 calc R . . C7 C 0.4129(4) 0.2673(3) -0.3199(9) 0.077(3) Uani 1 1 d . . . H7A H 0.4338 0.2900 -0.3585 0.093 Uiso 1 1 calc R . . C8 C 0.4217(3) 0.2412(3) -0.2445(8) 0.062(2) Uani 1 1 d . . . H8A H 0.4477 0.2460 -0.2360 0.075 Uiso 1 1 calc R . . C9 C 0.3898(3) 0.2085(2) -0.1846(7) 0.055(2) Uani 1 1 d . . . C10 C 0.3507(3) 0.2015(2) -0.2023(7) 0.049(2) Uani 1 1 d . . . C11 C 0.3431(2) 0.1494(2) -0.0735(7) 0.0421(18) Uani 1 1 d . . . C12 C 0.3858(2) 0.1753(2) -0.1000(7) 0.0440(18) Uani 1 1 d . . . C13 C 0.2917(2) 0.0891(2) 0.0276(8) 0.052(2) Uani 1 1 d . . . H13A H 0.2750 0.0832 -0.0507 0.062 Uiso 1 1 calc R . . H13B H 0.2818 0.0998 0.0955 0.062 Uiso 1 1 calc R . . C14 C 0.2904(2) 0.0515(2) 0.0775(8) 0.050(2) Uani 1 1 d . . . H14A H 0.2657 0.0354 0.1259 0.060 Uiso 1 1 calc R . . H14B H 0.2909 0.0360 0.0026 0.060 Uiso 1 1 calc R . . C15 C 0.3268(3) 0.0252(2) 0.1912(8) 0.065(2) Uani 1 1 d . . . H15A H 0.3033 0.0063 0.2390 0.097 Uiso 1 1 calc R . . H15B H 0.3501 0.0319 0.2433 0.097 Uiso 1 1 calc R . . H15C H 0.3282 0.0136 0.1085 0.097 Uiso 1 1 calc R . . C16 C 0.3199(3) 0.0779(3) 0.2923(8) 0.073(3) Uani 1 1 d . . . H16A H 0.2965 0.0578 0.3371 0.110 Uiso 1 1 calc R . . H16B H 0.3172 0.1009 0.2758 0.110 Uiso 1 1 calc R . . H16C H 0.3430 0.0854 0.3469 0.110 Uiso 1 1 calc R . . C17 C 0.4518(2) 0.1872(2) -0.0686(8) 0.051(2) Uani 1 1 d . . . C18 C 0.4759(3) 0.2239(3) -0.0076(9) 0.064(2) Uani 1 1 d . . . C19 C 0.5171(3) 0.2439(3) -0.0239(11) 0.082(3) Uani 1 1 d . . . H19A H 0.5335 0.2684 0.0166 0.098 Uiso 1 1 calc R . . C20 C 0.5333(3) 0.2253(4) -0.1049(11) 0.087(3) Uani 1 1 d . . . H20A H 0.5608 0.2381 -0.1174 0.105 Uiso 1 1 calc R . . C21 C 0.5100(3) 0.1898(3) -0.1641(10) 0.082(3) Uani 1 1 d . . . H21A H 0.5214 0.1785 -0.2173 0.098 Uiso 1 1 calc R . . C22 C 0.4696(3) 0.1705(3) -0.1457(9) 0.064(2) Uani 1 1 d . . . H22A H 0.4537 0.1457 -0.1855 0.076 Uiso 1 1 calc R . . C23 C 0.4783(3) 0.2547(3) 0.2483(9) 0.067(3) Uani 1 1 d . . . C24 C 0.4872(3) 0.2271(3) 0.3025(12) 0.091(3) Uani 1 1 d . . . H24A H 0.4829 0.2048 0.2542 0.110 Uiso 1 1 calc R . . C25 C 0.5025(4) 0.2334(4) 0.4291(14) 0.114(4) Uani 1 1 d . . . H25A H 0.5094 0.2154 0.4649 0.137 Uiso 1 1 calc R . . C26 C 0.5077(4) 0.2647(4) 0.5022(14) 0.119(5) Uani 1 1 d . . . H26A H 0.5171 0.2678 0.5891 0.143 Uiso 1 1 calc R . . C27 C 0.4991(4) 0.2920(4) 0.4474(14) 0.108(4) Uani 1 1 d . . . H27A H 0.5036 0.3142 0.4970 0.129 Uiso 1 1 calc R . . C28 C 0.4838(3) 0.2873(3) 0.3204(11) 0.077(3) Uani 1 1 d . . . H28A H 0.4775 0.3057 0.2847 0.092 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 Fe1 0.0492(7) 0.0450(7) 0.0465(7) 0.0027(5) -0.0036(5) 0.0271(6) Cl1 0.0598(14) 0.0663(14) 0.0649(14) 0.0006(11) -0.0186(11) 0.0285(12) Cl2 0.0690(14) 0.0597(13) 0.0474(12) -0.0033(10) -0.0025(10) 0.0392(11) S1 0.0741(17) 0.0766(18) 0.097(2) -0.0247(15) -0.0087(15) 0.0435(15) N1 0.051(4) 0.042(4) 0.044(4) 0.004(3) 0.000(3) 0.025(3) N2 0.047(4) 0.047(4) 0.051(4) 0.003(3) -0.003(3) 0.025(3) N3 0.059(4) 0.038(3) 0.039(3) -0.006(3) -0.011(3) 0.023(3) C1 0.070(6) 0.050(5) 0.045(5) -0.008(4) -0.009(4) 0.041(5) C2 0.075(6) 0.059(6) 0.063(6) -0.013(4) -0.019(5) 0.047(5) C3 0.105(9) 0.093(8) 0.074(7) -0.022(6) -0.031(7) 0.072(8) C4 0.111(9) 0.089(8) 0.047(5) -0.019(5) -0.025(6) 0.076(7) C5 0.112(8) 0.049(5) 0.031(4) -0.009(4) -0.013(5) 0.051(6) C6 0.148(11) 0.053(6) 0.048(5) -0.011(5) -0.015(6) 0.065(7) C7 0.124(10) 0.040(5) 0.058(6) 0.008(4) 0.000(6) 0.034(6) C8 0.086(7) 0.055(5) 0.044(5) -0.002(4) 0.000(5) 0.033(5) C9 0.089(7) 0.038(5) 0.039(5) 0.003(4) 0.005(4) 0.034(5) C10 0.076(6) 0.048(5) 0.035(4) -0.018(4) -0.017(4) 0.040(5) C11 0.057(5) 0.039(4) 0.033(4) -0.005(3) -0.007(4) 0.026(4) C12 0.065(5) 0.037(4) 0.037(4) 0.006(3) 0.007(4) 0.031(4) C13 0.053(5) 0.065(6) 0.048(5) 0.000(4) -0.001(4) 0.038(5) C14 0.046(5) 0.041(4) 0.062(5) -0.001(4) -0.013(4) 0.021(4) C15 0.076(6) 0.052(5) 0.062(6) 0.016(4) -0.004(5) 0.028(5) C16 0.082(7) 0.088(7) 0.039(5) -0.014(5) -0.008(5) 0.035(6) C17 0.058(5) 0.045(5) 0.052(5) 0.004(4) 0.002(4) 0.026(4) C18 0.060(6) 0.062(6) 0.077(6) -0.002(5) 0.007(5) 0.035(5) C19 0.061(6) 0.074(7) 0.105(8) 0.004(6) 0.010(6) 0.029(6) C20 0.054(6) 0.092(8) 0.114(9) 0.008(7) 0.023(6) 0.036(6) C21 0.083(8) 0.091(8) 0.081(7) 0.006(6) 0.023(6) 0.051(7) C22 0.070(7) 0.053(5) 0.072(6) 0.004(5) 0.003(5) 0.033(5) C23 0.055(6) 0.062(6) 0.076(6) -0.021(5) -0.005(5) 0.023(5) C24 0.115(9) 0.074(7) 0.109(10) -0.025(7) -0.014(8) 0.065(7) C25 0.153(12) 0.087(9) 0.117(11) -0.020(8) -0.041(10) 0.071(9) C26 0.148(13) 0.113(11) 0.102(10) -0.031(9) -0.032(9) 0.070(10) C27 0.111(10) 0.086(9) 0.107(10) -0.036(8) -0.013(8) 0.035(8) C28 0.076(7) 0.056(6) 0.091(8) -0.018(5) -0.004(6) 0.027(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N1 2.090(6) . ? Fe1 N2 2.215(6) . ? Fe1 N3 2.219(6) . ? Fe1 Cl1 2.273(2) . ? Fe1 Cl2 2.299(2) . ? S1 C18 1.784(9) . ? S1 C23 1.807(10) . ? N1 C11 1.281(9) . ? N1 C13 1.449(9) . ? N2 C12 1.298(9) . ? N2 C17 1.406(10) . ? N3 C14 1.469(9) . ? N3 C16 1.475(10) . ? N3 C15 1.477(9) . ? C1 C2 1.355(11) . ? C1 C10 1.408(11) . ? C1 C11 1.476(10) . ? C2 C3 1.376(12) . ? C3 C4 1.365(14) . ? C4 C5 1.382(13) . ? C5 C10 1.411(11) . ? C5 C6 1.413(14) . ? C6 C7 1.374(14) . ? C7 C8 1.429(12) . ? C8 C9 1.383(11) . ? C9 C10 1.406(11) . ? C9 C12 1.481(10) . ? C11 C12 1.462(10) . ? C13 C14 1.509(10) . ? C17 C18 1.389(11) . ? C17 C22 1.391(11) . ? C18 C19 1.386(12) . ? C19 C20 1.418(13) . ? C20 C21 1.344(14) . ? C21 C22 1.363(12) . ? C23 C28 1.376(12) . ? C23 C24 1.383(13) . ? C24 C25 1.373(15) . ? C25 C26 1.341(15) . ? C26 C27 1.369(16) . ? C27 C28 1.381(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 75.6(2) . . ? N1 Fe1 N3 75.7(2) . . ? N2 Fe1 N3 149.0(2) . . ? N1 Fe1 Cl1 143.45(18) . . ? N2 Fe1 Cl1 96.26(17) . . ? N3 Fe1 Cl1 99.72(17) . . ? N1 Fe1 Cl2 103.65(17) . . ? N2 Fe1 Cl2 97.71(17) . . ? N3 Fe1 Cl2 100.30(16) . . ? Cl1 Fe1 Cl2 112.80(9) . . ? C18 S1 C23 103.4(4) . . ? C11 N1 C13 123.1(6) . . ? C11 N1 Fe1 117.5(5) . . ? C13 N1 Fe1 119.2(5) . . ? C12 N2 C17 122.7(6) . . ? C12 N2 Fe1 112.3(5) . . ? C17 N2 Fe1 124.9(5) . . ? C14 N3 C16 110.4(6) . . ? C14 N3 C15 108.8(6) . . ? C16 N3 C15 108.9(6) . . ? C14 N3 Fe1 105.9(4) . . ? C16 N3 Fe1 111.8(5) . . ? C15 N3 Fe1 111.0(5) . . ? C2 C1 C10 118.8(8) . . ? C2 C1 C11 136.4(8) . . ? C10 C1 C11 104.7(7) . . ? C1 C2 C3 119.9(10) . . ? C4 C3 C2 121.6(10) . . ? C3 C4 C5 121.3(9) . . ? C4 C5 C10 116.5(9) . . ? C4 C5 C6 129.2(9) . . ? C10 C5 C6 114.3(9) . . ? C7 C6 C5 122.8(9) . . ? C6 C7 C8 121.5(10) . . ? C9 C8 C7 117.3(9) . . ? C8 C9 C10 120.0(8) . . ? C8 C9 C12 134.4(9) . . ? C10 C9 C12 105.6(7) . . ? C9 C10 C1 114.2(7) . . ? C9 C10 C5 124.1(9) . . ? C1 C10 C5 121.7(8) . . ? N1 C11 C12 116.9(7) . . ? N1 C11 C1 134.5(8) . . ? C12 C11 C1 108.6(6) . . ? N2 C12 C11 117.5(6) . . ? N2 C12 C9 135.6(8) . . ? C11 C12 C9 106.9(7) . . ? N1 C13 C14 107.9(6) . . ? N3 C14 C13 110.3(6) . . ? C18 C17 C22 119.0(8) . . ? C18 C17 N2 123.4(7) . . ? C22 C17 N2 117.6(7) . . ? C19 C18 C17 120.8(8) . . ? C19 C18 S1 118.6(7) . . ? C17 C18 S1 120.6(7) . . ? C18 C19 C20 117.3(10) . . ? C21 C20 C19 122.0(10) . . ? C20 C21 C22 119.8(10) . . ? C21 C22 C17 121.1(9) . . ? C28 C23 C24 120.8(10) . . ? C28 C23 S1 116.6(8) . . ? C24 C23 S1 122.3(7) . . ? C25 C24 C23 118.8(10) . . ? C26 C25 C24 121.7(12) . . ? C25 C26 C27 119.1(13) . . ? C26 C27 C28 121.7(12) . . ? C23 C28 C27 117.9(11) . . ? 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 Fe1 N1 C11 2.9(5) . . . . ? N3 Fe1 N1 C11 171.0(6) . . . . ? Cl1 Fe1 N1 C11 83.9(6) . . . . ? Cl2 Fe1 N1 C11 -91.7(5) . . . . ? N2 Fe1 N1 C13 179.7(6) . . . . ? N3 Fe1 N1 C13 -12.3(5) . . . . ? Cl1 Fe1 N1 C13 -99.4(6) . . . . ? Cl2 Fe1 N1 C13 85.1(5) . . . . ? N1 Fe1 N2 C12 -3.3(5) . . . . ? N3 Fe1 N2 C12 -26.2(8) . . . . ? Cl1 Fe1 N2 C12 -147.0(5) . . . . ? Cl2 Fe1 N2 C12 98.9(5) . . . . ? N1 Fe1 N2 C17 179.7(6) . . . . ? N3 Fe1 N2 C17 156.8(6) . . . . ? Cl1 Fe1 N2 C17 36.0(6) . . . . ? Cl2 Fe1 N2 C17 -78.1(6) . . . . ? N1 Fe1 N3 C14 33.0(4) . . . . ? N2 Fe1 N3 C14 55.9(6) . . . . ? Cl1 Fe1 N3 C14 175.9(4) . . . . ? Cl2 Fe1 N3 C14 -68.6(4) . . . . ? N1 Fe1 N3 C16 -87.3(5) . . . . ? N2 Fe1 N3 C16 -64.4(7) . . . . ? Cl1 Fe1 N3 C16 55.6(5) . . . . ? Cl2 Fe1 N3 C16 171.1(5) . . . . ? N1 Fe1 N3 C15 150.9(5) . . . . ? N2 Fe1 N3 C15 173.8(5) . . . . ? Cl1 Fe1 N3 C15 -66.2(5) . . . . ? Cl2 Fe1 N3 C15 49.3(5) . . . . ? C10 C1 C2 C3 3.0(12) . . . . ? C11 C1 C2 C3 179.8(9) . . . . ? C1 C2 C3 C4 -1.1(14) . . . . ? C2 C3 C4 C5 0.1(14) . . . . ? C3 C4 C5 C10 -1.1(12) . . . . ? C3 C4 C5 C6 -177.5(9) . . . . ? C4 C5 C6 C7 176.7(9) . . . . ? C10 C5 C6 C7 0.2(12) . . . . ? C5 C6 C7 C8 1.4(14) . . . . ? C6 C7 C8 C9 -2.4(13) . . . . ? C7 C8 C9 C10 1.7(11) . . . . ? C7 C8 C9 C12 -179.7(8) . . . . ? C8 C9 C10 C1 179.1(7) . . . . ? C12 C9 C10 C1 0.1(9) . . . . ? C8 C9 C10 C5 -0.1(12) . . . . ? C12 C9 C10 C5 -179.1(7) . . . . ? C2 C1 C10 C9 176.7(7) . . . . ? C11 C1 C10 C9 -1.0(9) . . . . ? C2 C1 C10 C5 -4.0(11) . . . . ? C11 C1 C10 C5 178.2(6) . . . . ? C4 C5 C10 C9 -177.8(7) . . . . ? C6 C5 C10 C9 -0.9(11) . . . . ? C4 C5 C10 C1 3.0(11) . . . . ? C6 C5 C10 C1 180.0(7) . . . . ? C13 N1 C11 C12 -178.8(6) . . . . ? Fe1 N1 C11 C12 -2.2(8) . . . . ? C13 N1 C11 C1 0.4(13) . . . . ? Fe1 N1 C11 C1 177.0(7) . . . . ? C2 C1 C11 N1 5.1(16) . . . . ? C10 C1 C11 N1 -177.8(8) . . . . ? C2 C1 C11 C12 -175.6(9) . . . . ? C10 C1 C11 C12 1.5(8) . . . . ? C17 N2 C12 C11 -179.7(7) . . . . ? Fe1 N2 C12 C11 3.3(8) . . . . ? C17 N2 C12 C9 1.9(13) . . . . ? Fe1 N2 C12 C9 -175.1(7) . . . . ? N1 C11 C12 N2 -0.9(10) . . . . ? C1 C11 C12 N2 179.7(6) . . . . ? N1 C11 C12 C9 177.9(6) . . . . ? C1 C11 C12 C9 -1.5(8) . . . . ? C8 C9 C12 N2 0.6(16) . . . . ? C10 C9 C12 N2 179.4(8) . . . . ? C8 C9 C12 C11 -177.9(8) . . . . ? C10 C9 C12 C11 0.9(8) . . . . ? C11 N1 C13 C14 165.5(7) . . . . ? Fe1 N1 C13 C14 -11.0(8) . . . . ? C16 N3 C14 C13 71.1(8) . . . . ? C15 N3 C14 C13 -169.4(7) . . . . ? Fe1 N3 C14 C13 -50.0(7) . . . . ? N1 C13 C14 N3 40.9(8) . . . . ? C12 N2 C17 C18 71.3(11) . . . . ? Fe1 N2 C17 C18 -112.1(8) . . . . ? C12 N2 C17 C22 -112.5(9) . . . . ? Fe1 N2 C17 C22 64.2(9) . . . . ? C22 C17 C18 C19 0.5(14) . . . . ? N2 C17 C18 C19 176.7(8) . . . . ? C22 C17 C18 S1 178.1(6) . . . . ? N2 C17 C18 S1 -5.7(12) . . . . ? C23 S1 C18 C19 -58.5(9) . . . . ? C23 S1 C18 C17 123.8(8) . . . . ? C17 C18 C19 C20 0.1(15) . . . . ? S1 C18 C19 C20 -177.6(8) . . . . ? C18 C19 C20 C21 0.0(17) . . . . ? C19 C20 C21 C22 -0.6(17) . . . . ? C20 C21 C22 C17 1.2(15) . . . . ? C18 C17 C22 C21 -1.2(13) . . . . ? N2 C17 C22 C21 -177.6(8) . . . . ? C18 S1 C23 C28 149.1(8) . . . . ? C18 S1 C23 C24 -37.0(10) . . . . ? C28 C23 C24 C25 -1.2(17) . . . . ? S1 C23 C24 C25 -174.9(10) . . . . ? C23 C24 C25 C26 2(2) . . . . ? C24 C25 C26 C27 -3(2) . . . . ? C25 C26 C27 C28 2(2) . . . . ? C24 C23 C28 C27 0.9(16) . . . . ? S1 C23 C28 C27 174.9(8) . . . . ? C26 C27 C28 C23 -1.4(19) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.696 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.092 #===END data_(2i)FeCl2(MeCN).1.5MeCN _database_code_depnum_ccdc_archive 'CCDC 636874' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040039 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H30.50 Cl3 Fe N4.50 S' _chemical_formula_weight 684.38 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.463(1) _cell_length_b 25.473(2) _cell_length_c 12.291(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.59(2) _cell_angle_gamma 90.00 _cell_volume 3268.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.10 _cell_measurement_theta_max 17.72 _exptl_crystal_description prism _exptl_crystal_colour amber _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1412 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7488 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.1085 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 26.97 _reflns_number_total 7106 _reflns_number_gt 4077 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0723P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7106 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1349 _refine_ls_R_factor_gt 0.0661 _refine_ls_wR_factor_ref 0.1673 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.004 _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 Fe1 Fe 0.84551(6) 0.09726(3) 0.26901(6) 0.02259(18) Uani 1 1 d . . . S1 S 0.68167(13) 0.29599(5) 0.39903(11) 0.0296(3) Uani 1 1 d . . . Cl1 Cl 0.71076(12) 0.10106(5) 0.10948(11) 0.0366(3) Uani 1 1 d . . . Cl2 Cl 0.80996(14) 0.10420(5) 0.45122(10) 0.0395(3) Uani 1 1 d . . . Cl3 Cl 0.16223(13) 0.19082(6) 0.49810(11) 0.0383(3) Uani 1 1 d . . . N1 N 0.8834(3) 0.18160(14) 0.2572(3) 0.0190(8) Uani 1 1 d . . . N2 N 1.0444(3) 0.09908(15) 0.2384(3) 0.0205(8) Uani 1 1 d . . . N3 N 0.8459(4) 0.01138(17) 0.2739(3) 0.0325(10) Uani 1 1 d . . . C1 C 1.0744(5) 0.23940(18) 0.2226(4) 0.0225(10) Uani 1 1 d . . . C2 C 1.0495(5) 0.29252(18) 0.2227(4) 0.0266(11) Uani 1 1 d . . . H2A H 0.9680 0.3053 0.2382 0.032 Uiso 1 1 calc R . . C3 C 1.1471(5) 0.3273(2) 0.1994(4) 0.0328(12) Uani 1 1 d . . . H3A H 1.1298 0.3638 0.1988 0.039 Uiso 1 1 calc R . . C4 C 1.2667(5) 0.3105(2) 0.1775(4) 0.0333(12) Uani 1 1 d . . . H4A H 1.3305 0.3353 0.1629 0.040 Uiso 1 1 calc R . . C5 C 1.2942(5) 0.25658(19) 0.1768(4) 0.0256(11) Uani 1 1 d . . . C6 C 1.4133(5) 0.2323(2) 0.1543(4) 0.0278(11) Uani 1 1 d . . . H6A H 1.4837 0.2538 0.1396 0.033 Uiso 1 1 calc R . . C7 C 1.4267(5) 0.1792(2) 0.1537(4) 0.0322(12) Uani 1 1 d . . . H7A H 1.5059 0.1646 0.1368 0.039 Uiso 1 1 calc R . . C8 C 1.3264(4) 0.1451(2) 0.1774(4) 0.0255(11) Uani 1 1 d . . . H8A H 1.3379 0.1081 0.1771 0.031 Uiso 1 1 calc R . . C9 C 1.2116(4) 0.16676(18) 0.2011(4) 0.0218(10) Uani 1 1 d . . . C10 C 1.1974(4) 0.22185(18) 0.1996(4) 0.0211(10) Uani 1 1 d . . . C11 C 0.9986(4) 0.19168(17) 0.2395(3) 0.0186(9) Uani 1 1 d . . . C12 C 1.0879(4) 0.14509(18) 0.2274(3) 0.0195(10) Uani 1 1 d . . . C13 C 0.7880(4) 0.22346(18) 0.2662(4) 0.0224(10) Uani 1 1 d . . . H13A H 0.7005 0.2092 0.2479 0.027 Uiso 1 1 calc R . . H13B H 0.8020 0.2519 0.2138 0.027 Uiso 1 1 calc R . . C14 C 0.7997(4) 0.24551(18) 0.3821(4) 0.0232(10) Uani 1 1 d . . . H14A H 0.8868 0.2603 0.3993 0.028 Uiso 1 1 calc R . . H14B H 0.7886 0.2167 0.4342 0.028 Uiso 1 1 calc R . . C15 C 0.5409(5) 0.26187(19) 0.4269(4) 0.0247(11) Uani 1 1 d . . . C16 C 0.5276(5) 0.20835(19) 0.4342(4) 0.0286(11) Uani 1 1 d . . . H16A H 0.5985 0.1863 0.4237 0.034 Uiso 1 1 calc R . . C17 C 0.4118(5) 0.1861(2) 0.4569(4) 0.0309(12) Uani 1 1 d . . . H17A H 0.4032 0.1491 0.4616 0.037 Uiso 1 1 calc R . . C18 C 0.3088(5) 0.21889(19) 0.4725(4) 0.0256(11) Uani 1 1 d . . . C19 C 0.3200(5) 0.2724(2) 0.4671(4) 0.0291(11) Uani 1 1 d . . . H19A H 0.2493 0.2944 0.4785 0.035 Uiso 1 1 calc R . . C20 C 0.4358(5) 0.29357(19) 0.4448(4) 0.0271(11) Uani 1 1 d . . . H20A H 0.4445 0.3306 0.4416 0.032 Uiso 1 1 calc R . . C21 C 1.1195(4) 0.05299(17) 0.2190(4) 0.0188(10) Uani 1 1 d . . . C22 C 1.1328(4) 0.03864(18) 0.1107(4) 0.0241(11) Uani 1 1 d . . . C23 C 1.1956(5) -0.0085(2) 0.0946(4) 0.0297(12) Uani 1 1 d . . . H23A H 1.2086 -0.0189 0.0223 0.036 Uiso 1 1 calc R . . C24 C 1.2393(5) -0.0404(2) 0.1803(5) 0.0366(13) Uani 1 1 d . . . H24A H 1.2798 -0.0728 0.1669 0.044 Uiso 1 1 calc R . . C25 C 1.2239(5) -0.0250(2) 0.2866(4) 0.0316(12) Uani 1 1 d . . . H25A H 1.2550 -0.0469 0.3458 0.038 Uiso 1 1 calc R . . C26 C 1.1638(5) 0.0219(2) 0.3074(4) 0.0267(11) Uani 1 1 d . . . C27 C 1.0821(5) 0.0716(2) 0.0153(4) 0.0327(12) Uani 1 1 d . . . H27A H 1.1020 0.0547 -0.0525 0.049 Uiso 1 1 calc R . . H27B H 1.1224 0.1063 0.0210 0.049 Uiso 1 1 calc R . . H27C H 0.9889 0.0753 0.0150 0.049 Uiso 1 1 calc R . . C28 C 1.1473(5) 0.0387(2) 0.4225(4) 0.0367(13) Uani 1 1 d . . . H28A H 1.1854 0.0123 0.4737 0.055 Uiso 1 1 calc R . . H28B H 1.0557 0.0423 0.4313 0.055 Uiso 1 1 calc R . . H28C H 1.1903 0.0725 0.4373 0.055 Uiso 1 1 calc R . . C29 C 0.8666(6) -0.0318(2) 0.2867(4) 0.0349(13) Uani 1 1 d . . . C30 C 0.8961(8) -0.0865(2) 0.3049(5) 0.060(2) Uani 1 1 d . . . H30A H 0.9247 -0.1018 0.2384 0.090 Uiso 1 1 calc R . . H30B H 0.8192 -0.1049 0.3240 0.090 Uiso 1 1 calc R . . H30C H 0.9644 -0.0899 0.3648 0.090 Uiso 1 1 calc R . . C1S C 0.5264(9) 0.0327(4) 0.3364(10) 0.116(4) Uani 1 1 d . . . H1SA H 0.5782 0.0552 0.3879 0.174 Uiso 1 1 calc R . . H2SA H 0.4351 0.0399 0.3409 0.174 Uiso 1 1 calc R . . H3SA H 0.5480 0.0398 0.2621 0.174 Uiso 1 1 calc R . . C2S C 0.5537(9) -0.0234(5) 0.3640(10) 0.115(4) Uani 1 1 d . . . N1S N 0.5718(9) -0.0679(5) 0.3768(13) 0.210(8) Uani 1 1 d . . . C3S C 1.4624(17) 0.0264(6) -0.0464(15) 0.090(6) Uani 0.50 1 d P . . H3SB H 1.5039 0.0322 0.0274 0.135 Uiso 0.50 1 calc PR . . H3SC H 1.5218 0.0079 -0.0900 0.135 Uiso 0.50 1 calc PR . . H3SD H 1.3849 0.0052 -0.0425 0.135 Uiso 0.50 1 calc PR . . C4S C 1.4290(17) 0.0748(8) -0.0953(17) 0.083(5) Uani 0.50 1 d P . . N2S N 1.4033(18) 0.1124(11) -0.142(2) 0.179(12) Uani 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0233(4) 0.0179(3) 0.0283(4) -0.0011(3) 0.0116(3) -0.0017(3) S1 0.0330(7) 0.0220(6) 0.0359(7) -0.0037(5) 0.0146(6) 0.0047(5) Cl1 0.0345(7) 0.0332(7) 0.0411(7) -0.0109(6) -0.0016(6) 0.0053(6) Cl2 0.0616(9) 0.0282(7) 0.0327(7) 0.0035(6) 0.0249(6) 0.0060(7) Cl3 0.0333(7) 0.0429(8) 0.0406(8) -0.0001(6) 0.0124(6) -0.0033(6) N1 0.019(2) 0.018(2) 0.021(2) -0.0036(15) 0.0084(16) 0.0005(16) N2 0.0217(19) 0.0165(19) 0.0248(19) -0.0010(17) 0.0094(16) 0.0013(17) N3 0.038(3) 0.025(2) 0.037(3) 0.001(2) 0.019(2) -0.003(2) C1 0.027(3) 0.021(2) 0.020(2) 0.0000(19) 0.005(2) -0.002(2) C2 0.037(3) 0.017(2) 0.027(3) -0.0006(19) 0.008(2) 0.002(2) C3 0.047(3) 0.021(3) 0.031(3) 0.003(2) 0.005(3) -0.007(2) C4 0.037(3) 0.031(3) 0.032(3) 0.004(2) 0.003(2) -0.018(3) C5 0.029(3) 0.028(3) 0.020(2) 0.000(2) 0.003(2) -0.011(2) C6 0.021(3) 0.040(3) 0.023(3) 0.000(2) 0.005(2) -0.011(2) C7 0.019(3) 0.043(3) 0.035(3) -0.001(2) 0.008(2) -0.007(2) C8 0.023(3) 0.027(3) 0.027(3) 0.002(2) 0.003(2) 0.001(2) C9 0.021(2) 0.021(2) 0.024(2) -0.0015(19) 0.006(2) -0.001(2) C10 0.025(2) 0.021(2) 0.017(2) 0.0037(18) 0.0030(19) -0.003(2) C11 0.025(2) 0.017(2) 0.014(2) -0.0021(18) 0.0008(18) 0.0027(19) C12 0.020(2) 0.024(3) 0.015(2) -0.0040(18) 0.0062(18) -0.004(2) C13 0.022(2) 0.020(2) 0.027(3) 0.0021(19) 0.006(2) 0.006(2) C14 0.024(2) 0.021(2) 0.026(2) -0.003(2) 0.007(2) 0.006(2) C15 0.028(3) 0.025(3) 0.021(2) -0.003(2) 0.004(2) 0.000(2) C16 0.030(3) 0.026(3) 0.031(3) 0.000(2) 0.009(2) 0.008(2) C17 0.043(3) 0.026(3) 0.025(3) -0.001(2) 0.007(2) 0.003(2) C18 0.029(3) 0.027(3) 0.021(2) -0.001(2) 0.005(2) -0.001(2) C19 0.026(3) 0.031(3) 0.030(3) -0.007(2) 0.004(2) 0.005(2) C20 0.030(3) 0.023(3) 0.029(3) -0.003(2) 0.006(2) 0.005(2) C21 0.016(2) 0.014(2) 0.027(2) -0.0013(19) 0.0097(19) 0.0010(18) C22 0.022(2) 0.023(2) 0.028(3) -0.003(2) 0.008(2) -0.007(2) C23 0.030(3) 0.027(3) 0.035(3) -0.005(2) 0.018(2) -0.001(2) C24 0.043(3) 0.019(3) 0.049(3) -0.005(2) 0.016(3) 0.009(2) C25 0.031(3) 0.021(3) 0.043(3) 0.006(2) 0.008(2) 0.004(2) C26 0.027(3) 0.026(3) 0.027(3) 0.003(2) 0.007(2) -0.004(2) C27 0.044(3) 0.029(3) 0.025(3) 0.001(2) 0.006(2) -0.001(2) C28 0.045(3) 0.037(3) 0.029(3) 0.011(2) 0.008(2) 0.006(3) C29 0.051(4) 0.027(3) 0.030(3) 0.002(2) 0.015(3) -0.007(3) C30 0.109(6) 0.027(3) 0.046(4) 0.004(3) 0.014(4) 0.005(4) C1S 0.069(6) 0.106(9) 0.173(11) 0.039(8) 0.010(7) -0.023(6) C2S 0.055(6) 0.127(10) 0.155(10) 0.050(9) -0.020(6) -0.035(6) N1S 0.076(6) 0.136(9) 0.40(2) 0.151(12) -0.047(9) -0.044(7) C3S 0.087(13) 0.065(11) 0.122(15) -0.015(11) 0.032(11) -0.049(10) C4S 0.059(11) 0.087(14) 0.108(15) 0.004(12) 0.023(10) 0.003(10) N2S 0.070(13) 0.23(3) 0.24(3) 0.11(2) 0.040(15) 0.022(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.151(4) . ? Fe1 N3 2.190(4) . ? Fe1 N1 2.194(4) . ? Fe1 Cl1 2.3058(15) . ? Fe1 Cl2 2.3161(14) . ? S1 C15 1.773(5) . ? S1 C14 1.810(4) . ? Cl3 C18 1.748(5) . ? N1 C11 1.272(6) . ? N1 C13 1.473(5) . ? N2 C12 1.270(6) . ? N2 C21 1.446(5) . ? N3 C29 1.129(6) . ? C1 C2 1.379(6) . ? C1 C10 1.417(6) . ? C1 C11 1.478(6) . ? C2 C3 1.402(7) . ? C3 C4 1.373(7) . ? C4 C5 1.405(7) . ? C5 C10 1.394(6) . ? C5 C6 1.441(7) . ? C6 C7 1.362(7) . ? C7 C8 1.415(7) . ? C8 C9 1.379(6) . ? C9 C10 1.412(6) . ? C9 C12 1.472(6) . ? C11 C12 1.527(6) . ? C13 C14 1.527(6) . ? C15 C16 1.375(7) . ? C15 C20 1.399(7) . ? C16 C17 1.390(7) . ? C17 C18 1.392(7) . ? C18 C19 1.370(7) . ? C19 C20 1.379(7) . ? C21 C26 1.389(6) . ? C21 C22 1.403(6) . ? C22 C23 1.393(7) . ? C22 C27 1.499(7) . ? C23 C24 1.374(7) . ? C24 C25 1.391(7) . ? C25 C26 1.385(7) . ? C26 C28 1.507(7) . ? C29 C30 1.442(7) . ? C1S C2S 1.492(14) . ? C2S N1S 1.158(15) . ? C3S C4S 1.40(2) . ? C3S C3S 1.89(4) 3_855 ? C4S N2S 1.14(2) . ? 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 Fe1 N3 91.56(15) . . ? N2 Fe1 N1 77.48(14) . . ? N3 Fe1 N1 169.03(15) . . ? N2 Fe1 Cl1 111.82(11) . . ? N3 Fe1 Cl1 93.71(13) . . ? N1 Fe1 Cl1 90.10(11) . . ? N2 Fe1 Cl2 114.67(11) . . ? N3 Fe1 Cl2 92.87(12) . . ? N1 Fe1 Cl2 92.08(10) . . ? Cl1 Fe1 Cl2 132.79(6) . . ? C15 S1 C14 105.2(2) . . ? C11 N1 C13 121.8(4) . . ? C11 N1 Fe1 112.9(3) . . ? C13 N1 Fe1 125.3(3) . . ? C12 N2 C21 121.8(4) . . ? C12 N2 Fe1 113.7(3) . . ? C21 N2 Fe1 124.2(3) . . ? C29 N3 Fe1 167.8(5) . . ? C2 C1 C10 119.0(4) . . ? C2 C1 C11 134.8(5) . . ? C10 C1 C11 106.2(4) . . ? C1 C2 C3 118.6(5) . . ? C4 C3 C2 122.6(5) . . ? C3 C4 C5 119.8(5) . . ? C10 C5 C4 117.8(5) . . ? C10 C5 C6 115.1(4) . . ? C4 C5 C6 127.1(5) . . ? C7 C6 C5 121.3(5) . . ? C6 C7 C8 122.1(5) . . ? C9 C8 C7 118.4(5) . . ? C8 C9 C10 119.2(4) . . ? C8 C9 C12 134.3(4) . . ? C10 C9 C12 106.4(4) . . ? C5 C10 C9 123.8(5) . . ? C5 C10 C1 122.1(4) . . ? C9 C10 C1 114.1(4) . . ? N1 C11 C1 136.1(4) . . ? N1 C11 C12 117.3(4) . . ? C1 C11 C12 106.5(4) . . ? N2 C12 C9 134.6(4) . . ? N2 C12 C11 118.6(4) . . ? C9 C12 C11 106.8(4) . . ? N1 C13 C14 110.1(4) . . ? C13 C14 S1 112.1(3) . . ? C16 C15 C20 118.5(5) . . ? C16 C15 S1 126.2(4) . . ? C20 C15 S1 115.3(4) . . ? C15 C16 C17 120.9(5) . . ? C16 C17 C18 119.0(5) . . ? C19 C18 C17 121.3(5) . . ? C19 C18 Cl3 119.8(4) . . ? C17 C18 Cl3 119.0(4) . . ? C18 C19 C20 118.7(5) . . ? C19 C20 C15 121.6(5) . . ? C26 C21 C22 122.6(4) . . ? C26 C21 N2 118.7(4) . . ? C22 C21 N2 118.3(4) . . ? C23 C22 C21 116.9(4) . . ? C23 C22 C27 120.5(4) . . ? C21 C22 C27 122.6(4) . . ? C24 C23 C22 121.8(5) . . ? C23 C24 C25 119.6(5) . . ? C26 C25 C24 120.9(5) . . ? C25 C26 C21 118.1(4) . . ? C25 C26 C28 121.0(5) . . ? C21 C26 C28 120.9(4) . . ? N3 C29 C30 178.5(7) . . ? N1S C2S C1S 174.5(15) . . ? C4S C3S C3S 163.6(19) . 3_855 ? N2S C4S C3S 175(3) . . ? 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 Fe1 N1 C11 -0.4(3) . . . . ? N3 Fe1 N1 C11 -2.3(10) . . . . ? Cl1 Fe1 N1 C11 -112.7(3) . . . . ? Cl2 Fe1 N1 C11 114.4(3) . . . . ? N2 Fe1 N1 C13 178.5(3) . . . . ? N3 Fe1 N1 C13 176.6(7) . . . . ? Cl1 Fe1 N1 C13 66.2(3) . . . . ? Cl2 Fe1 N1 C13 -66.7(3) . . . . ? N3 Fe1 N2 C12 179.0(3) . . . . ? N1 Fe1 N2 C12 -0.6(3) . . . . ? Cl1 Fe1 N2 C12 84.4(3) . . . . ? Cl2 Fe1 N2 C12 -87.1(3) . . . . ? N3 Fe1 N2 C21 6.0(3) . . . . ? N1 Fe1 N2 C21 -173.7(4) . . . . ? Cl1 Fe1 N2 C21 -88.7(3) . . . . ? Cl2 Fe1 N2 C21 99.8(3) . . . . ? N2 Fe1 N3 C29 42(2) . . . . ? N1 Fe1 N3 C29 44(2) . . . . ? Cl1 Fe1 N3 C29 154(2) . . . . ? Cl2 Fe1 N3 C29 -73(2) . . . . ? C10 C1 C2 C3 0.3(7) . . . . ? C11 C1 C2 C3 -178.0(5) . . . . ? C1 C2 C3 C4 -0.6(8) . . . . ? C2 C3 C4 C5 0.7(8) . . . . ? C3 C4 C5 C10 -0.5(7) . . . . ? C3 C4 C5 C6 179.2(5) . . . . ? C10 C5 C6 C7 1.3(7) . . . . ? C4 C5 C6 C7 -178.4(5) . . . . ? C5 C6 C7 C8 -1.5(8) . . . . ? C6 C7 C8 C9 0.4(8) . . . . ? C7 C8 C9 C10 0.7(7) . . . . ? C7 C8 C9 C12 178.9(5) . . . . ? C4 C5 C10 C9 179.6(4) . . . . ? C6 C5 C10 C9 -0.1(7) . . . . ? C4 C5 C10 C1 0.2(7) . . . . ? C6 C5 C10 C1 -179.5(4) . . . . ? C8 C9 C10 C5 -0.9(7) . . . . ? C12 C9 C10 C5 -179.5(4) . . . . ? C8 C9 C10 C1 178.5(4) . . . . ? C12 C9 C10 C1 -0.1(6) . . . . ? C2 C1 C10 C5 -0.1(7) . . . . ? C11 C1 C10 C5 178.6(4) . . . . ? C2 C1 C10 C9 -179.6(4) . . . . ? C11 C1 C10 C9 -0.9(5) . . . . ? C13 N1 C11 C1 -0.4(8) . . . . ? Fe1 N1 C11 C1 178.5(4) . . . . ? C13 N1 C11 C12 -177.7(4) . . . . ? Fe1 N1 C11 C12 1.2(5) . . . . ? C2 C1 C11 N1 2.3(9) . . . . ? C10 C1 C11 N1 -176.2(5) . . . . ? C2 C1 C11 C12 179.8(5) . . . . ? C10 C1 C11 C12 1.4(5) . . . . ? C21 N2 C12 C9 -3.3(8) . . . . ? Fe1 N2 C12 C9 -176.6(4) . . . . ? C21 N2 C12 C11 174.7(4) . . . . ? Fe1 N2 C12 C11 1.4(5) . . . . ? C8 C9 C12 N2 0.8(10) . . . . ? C10 C9 C12 N2 179.1(5) . . . . ? C8 C9 C12 C11 -177.4(5) . . . . ? C10 C9 C12 C11 0.9(5) . . . . ? N1 C11 C12 N2 -1.8(6) . . . . ? C1 C11 C12 N2 -179.9(4) . . . . ? N1 C11 C12 C9 176.7(4) . . . . ? C1 C11 C12 C9 -1.4(5) . . . . ? C11 N1 C13 C14 -83.8(5) . . . . ? Fe1 N1 C13 C14 97.4(4) . . . . ? N1 C13 C14 S1 -178.4(3) . . . . ? C15 S1 C14 C13 84.1(4) . . . . ? C14 S1 C15 C16 0.4(5) . . . . ? C14 S1 C15 C20 179.1(4) . . . . ? C20 C15 C16 C17 1.2(7) . . . . ? S1 C15 C16 C17 179.8(4) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C16 C17 C18 C19 -0.7(8) . . . . ? C16 C17 C18 Cl3 178.7(4) . . . . ? C17 C18 C19 C20 0.6(8) . . . . ? Cl3 C18 C19 C20 -178.8(4) . . . . ? C18 C19 C20 C15 0.5(8) . . . . ? C16 C15 C20 C19 -1.4(7) . . . . ? S1 C15 C20 C19 179.8(4) . . . . ? C12 N2 C21 C26 110.6(5) . . . . ? Fe1 N2 C21 C26 -76.9(5) . . . . ? C12 N2 C21 C22 -76.0(6) . . . . ? Fe1 N2 C21 C22 96.5(4) . . . . ? C26 C21 C22 C23 -1.2(7) . . . . ? N2 C21 C22 C23 -174.3(4) . . . . ? C26 C21 C22 C27 178.5(5) . . . . ? N2 C21 C22 C27 5.4(6) . . . . ? C21 C22 C23 C24 1.9(7) . . . . ? C27 C22 C23 C24 -177.8(5) . . . . ? C22 C23 C24 C25 -1.7(8) . . . . ? C23 C24 C25 C26 0.7(8) . . . . ? C24 C25 C26 C21 0.0(8) . . . . ? C24 C25 C26 C28 -179.8(5) . . . . ? C22 C21 C26 C25 0.3(7) . . . . ? N2 C21 C26 C25 173.4(4) . . . . ? C22 C21 C26 C28 -179.9(4) . . . . ? N2 C21 C26 C28 -6.8(7) . . . . ? Fe1 N3 C29 C30 6(26) . . . . ? C3S C3S C4S N2S 131(26) 3_855 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.97 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.458 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.098 #===END data_[(2i)FeCl2]2_CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 636875' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 040041 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H25 Cl5 Fe N2 S' _chemical_formula_weight 666.67 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.095(1) _cell_length_b 13.842(1) _cell_length_c 20.837(3) _cell_angle_alpha 92.33(2) _cell_angle_beta 92.33(1) _cell_angle_gamma 92.78(2) _cell_volume 2903.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10.52 _cell_measurement_theta_max 14.80 _exptl_crystal_description rod _exptl_crystal_colour amber _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 1.075 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.7815 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'Omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 12053 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.97 _reflns_number_total 11373 _reflns_number_gt 6848 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0813P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11373 _refine_ls_number_parameters 689 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1265 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1733 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Fe1 Fe 1.08824(8) -0.05154(6) 0.06563(4) 0.01899(19) Uani 1 1 d . . . Cl1 Cl 1.17571(14) -0.19809(10) 0.05385(7) 0.0284(3) Uani 1 1 d . . . Cl2 Cl 0.86613(13) -0.00626(10) 0.04283(6) 0.0235(3) Uani 1 1 d . . . N1 N 1.0318(4) -0.0562(3) 0.1662(2) 0.0194(10) Uani 1 1 d . . . N2 N 1.2053(4) 0.0675(3) 0.1093(2) 0.0199(10) Uani 1 1 d . . . S1 S 0.80159(17) -0.30331(11) 0.18687(9) 0.0364(4) Uani 1 1 d . . . Cl5 Cl 0.29819(16) -0.10466(12) 0.28364(9) 0.0406(4) Uani 1 1 d . . . C1 C 1.0666(5) 0.0568(4) 0.2653(3) 0.0214(12) Uani 1 1 d . . . C2 C 0.9935(6) 0.0304(5) 0.3169(3) 0.0281(14) Uani 1 1 d . . . H2A H 0.9364 -0.0264 0.3142 0.034 Uiso 1 1 calc R . . C3 C 1.0054(6) 0.0896(5) 0.3741(3) 0.0347(16) Uani 1 1 d . . . H3A H 0.9556 0.0712 0.4097 0.042 Uiso 1 1 calc R . . C4 C 1.0848(6) 0.1714(5) 0.3800(3) 0.0300(14) Uani 1 1 d . . . H4A H 1.0880 0.2101 0.4188 0.036 Uiso 1 1 calc R . . C5 C 1.1631(6) 0.1995(4) 0.3284(3) 0.0261(13) Uani 1 1 d . . . C6 C 1.2495(7) 0.2819(5) 0.3268(3) 0.0370(16) Uani 1 1 d . . . H6A H 1.2603 0.3246 0.3637 0.044 Uiso 1 1 calc R . . C7 C 1.3188(7) 0.3023(5) 0.2733(3) 0.0404(17) Uani 1 1 d . . . H7A H 1.3766 0.3587 0.2740 0.049 Uiso 1 1 calc R . . C8 C 1.3061(6) 0.2413(4) 0.2169(3) 0.0306(14) Uani 1 1 d . . . H8A H 1.3551 0.2559 0.1803 0.037 Uiso 1 1 calc R . . C9 C 1.2218(5) 0.1608(4) 0.2164(3) 0.0210(12) Uani 1 1 d . . . C10 C 1.1507(5) 0.1405(4) 0.2718(2) 0.0217(12) Uani 1 1 d . . . C11 C 1.0789(5) 0.0178(4) 0.1989(3) 0.0194(12) Uani 1 1 d . . . C12 C 1.1773(5) 0.0856(4) 0.1686(3) 0.0203(12) Uani 1 1 d . . . C13 C 0.9419(6) -0.1264(4) 0.1961(3) 0.0250(13) Uani 1 1 d . . . H13A H 0.8662 -0.0924 0.2134 0.030 Uiso 1 1 calc R . . H13B H 0.9898 -0.1551 0.2325 0.030 Uiso 1 1 calc R . . C14 C 0.8896(6) -0.2067(4) 0.1487(3) 0.0317(15) Uani 1 1 d . . . H14A H 0.9649 -0.2332 0.1260 0.038 Uiso 1 1 calc R . . H14B H 0.8294 -0.1793 0.1162 0.038 Uiso 1 1 calc R . . C15 C 0.6600(6) -0.2453(4) 0.2131(3) 0.0267(13) Uani 1 1 d . . . C16 C 0.6557(6) -0.2099(4) 0.2770(3) 0.0281(14) Uani 1 1 d . . . H16A H 0.7300 -0.2152 0.3059 0.034 Uiso 1 1 calc R . . C17 C 0.5438(6) -0.1675(4) 0.2977(3) 0.0253(13) Uani 1 1 d . . . H17A H 0.5411 -0.1425 0.3407 0.030 Uiso 1 1 calc R . . C18 C 0.4370(6) -0.1615(4) 0.2565(3) 0.0260(13) Uani 1 1 d . . . C19 C 0.4360(6) -0.1982(4) 0.1942(3) 0.0319(15) Uani 1 1 d . . . H19A H 0.3593 -0.1950 0.1666 0.038 Uiso 1 1 calc R . . C20 C 0.5486(6) -0.2398(4) 0.1724(3) 0.0317(15) Uani 1 1 d . . . H20A H 0.5496 -0.2648 0.1293 0.038 Uiso 1 1 calc R . . C21 C 1.3056(5) 0.1263(4) 0.0792(2) 0.0185(11) Uani 1 1 d . . . C22 C 1.4312(6) 0.0894(4) 0.0757(3) 0.0229(12) Uani 1 1 d . . . C23 C 1.5273(6) 0.1420(4) 0.0444(3) 0.0266(13) Uani 1 1 d . . . H23A H 1.6141 0.1189 0.0420 0.032 Uiso 1 1 calc R . . C24 C 1.4982(6) 0.2273(5) 0.0167(3) 0.0303(14) Uani 1 1 d . . . H24A H 1.5648 0.2626 -0.0048 0.036 Uiso 1 1 calc R . . C25 C 1.3737(6) 0.2618(4) 0.0200(3) 0.0288(14) Uani 1 1 d . . . H25A H 1.3553 0.3210 0.0008 0.035 Uiso 1 1 calc R . . C26 C 1.2726(6) 0.2114(4) 0.0512(3) 0.0247(13) Uani 1 1 d . . . C27 C 1.4612(6) -0.0060(4) 0.1035(3) 0.0311(14) Uani 1 1 d . . . H27A H 1.4471 -0.0028 0.1498 0.047 Uiso 1 1 calc R . . H27B H 1.5538 -0.0199 0.0963 0.047 Uiso 1 1 calc R . . H27C H 1.4024 -0.0573 0.0826 0.047 Uiso 1 1 calc R . . C28 C 1.1369(6) 0.2493(5) 0.0542(3) 0.0322(15) Uani 1 1 d . . . H28A H 1.0705 0.1972 0.0416 0.048 Uiso 1 1 calc R . . H28B H 1.1287 0.3023 0.0248 0.048 Uiso 1 1 calc R . . H28C H 1.1223 0.2731 0.0982 0.048 Uiso 1 1 calc R . . Fe2 Fe 0.90813(8) 0.50113(6) 0.42523(4) 0.01939(19) Uani 1 1 d . . . Cl3 Cl 0.80590(15) 0.63180(11) 0.39161(7) 0.0324(4) Uani 1 1 d . . . Cl4 Cl 1.12676(13) 0.46558(11) 0.45620(6) 0.0251(3) Uani 1 1 d . . . N3 N 0.9405(4) 0.4379(3) 0.3277(2) 0.0175(10) Uani 1 1 d . . . N4 N 0.7860(4) 0.3720(3) 0.4223(2) 0.0197(10) Uani 1 1 d . . . S2 S 1.13822(17) 0.63870(11) 0.22466(8) 0.0346(4) Uani 1 1 d . . . Cl6 Cl 1.66624(18) 0.42709(16) 0.19463(10) 0.0554(5) Uani 1 1 d . . . C31 C 0.8599(5) 0.2844(4) 0.2636(2) 0.0190(12) Uani 1 1 d . . . C32 C 0.9092(6) 0.2754(4) 0.2036(3) 0.0232(12) Uani 1 1 d . . . H32A H 0.9743 0.3209 0.1897 0.028 Uiso 1 1 calc R . . C33 C 0.8608(6) 0.1967(4) 0.1630(3) 0.0264(13) Uani 1 1 d . . . H33A H 0.8931 0.1911 0.1209 0.032 Uiso 1 1 calc R . . C34 C 0.7705(6) 0.1286(4) 0.1811(3) 0.0284(14) Uani 1 1 d . . . H34A H 0.7428 0.0759 0.1521 0.034 Uiso 1 1 calc R . . C35 C 0.7169(6) 0.1355(4) 0.2431(3) 0.0263(13) Uani 1 1 d . . . C36 C 0.6230(7) 0.0705(5) 0.2690(3) 0.0375(16) Uani 1 1 d . . . H36A H 0.5907 0.0142 0.2445 0.045 Uiso 1 1 calc R . . C37 C 0.5779(7) 0.0886(5) 0.3298(3) 0.0405(17) Uani 1 1 d . . . H37A H 0.5115 0.0459 0.3456 0.049 Uiso 1 1 calc R . . C38 C 0.6276(7) 0.1688(4) 0.3693(3) 0.0361(16) Uani 1 1 d . . . H38A H 0.5976 0.1787 0.4116 0.043 Uiso 1 1 calc R . . C39 C 0.7192(6) 0.2314(4) 0.3453(3) 0.0216(12) Uani 1 1 d . . . C40 C 0.7656(5) 0.2142(4) 0.2828(3) 0.0213(12) Uani 1 1 d . . . C41 C 0.8782(5) 0.3570(4) 0.3183(2) 0.0179(11) Uani 1 1 d . . . C42 C 0.7909(5) 0.3203(4) 0.3700(3) 0.0209(12) Uani 1 1 d . . . C43 C 1.0166(5) 0.4792(4) 0.2759(3) 0.0209(12) Uani 1 1 d . . . H43A H 0.9595 0.4782 0.2361 0.025 Uiso 1 1 calc R . . H43B H 1.0928 0.4388 0.2674 0.025 Uiso 1 1 calc R . . C44 C 1.0669(6) 0.5812(4) 0.2927(3) 0.0321(15) Uani 1 1 d . . . H44A H 1.1349 0.5809 0.3282 0.038 Uiso 1 1 calc R . . H44B H 0.9927 0.6191 0.3078 0.038 Uiso 1 1 calc R . . C45 C 1.2875(6) 0.5774(4) 0.2176(3) 0.0250(13) Uani 1 1 d . . . C46 C 1.3862(6) 0.5862(4) 0.2655(3) 0.0308(14) Uani 1 1 d . . . H46A H 1.3722 0.6229 0.3039 0.037 Uiso 1 1 calc R . . C47 C 1.5051(6) 0.5425(5) 0.2585(3) 0.0325(15) Uani 1 1 d . . . H47A H 1.5735 0.5494 0.2913 0.039 Uiso 1 1 calc R . . C48 C 1.5219(6) 0.4884(5) 0.2023(3) 0.0317(15) Uani 1 1 d . . . C49 C 1.4261(6) 0.4806(5) 0.1536(3) 0.0385(16) Uani 1 1 d . . . H49A H 1.4409 0.4453 0.1147 0.046 Uiso 1 1 calc R . . C50 C 1.3081(6) 0.5244(5) 0.1617(3) 0.0319(15) Uani 1 1 d . . . H50A H 1.2404 0.5181 0.1286 0.038 Uiso 1 1 calc R . . C51 C 0.6926(5) 0.3434(4) 0.4696(2) 0.0209(12) Uani 1 1 d . . . C52 C 0.5637(5) 0.3749(4) 0.4615(3) 0.0204(12) Uani 1 1 d . . . C53 C 0.4744(6) 0.3517(4) 0.5086(3) 0.0268(13) Uani 1 1 d . . . H53A H 0.3857 0.3716 0.5049 0.032 Uiso 1 1 calc R . . C54 C 0.5143(6) 0.2995(4) 0.5610(3) 0.0277(14) Uani 1 1 d . . . H54A H 0.4527 0.2843 0.5928 0.033 Uiso 1 1 calc R . . C55 C 0.6402(6) 0.2700(4) 0.5672(3) 0.0261(13) Uani 1 1 d . . . H55A H 0.6652 0.2344 0.6034 0.031 Uiso 1 1 calc R . . C56 C 0.7342(6) 0.2910(4) 0.5214(3) 0.0226(12) Uani 1 1 d . . . C57 C 0.5234(6) 0.4328(4) 0.4055(3) 0.0286(14) Uani 1 1 d . . . H57A H 0.5831 0.4905 0.4040 0.043 Uiso 1 1 calc R . . H57B H 0.4321 0.4523 0.4101 0.043 Uiso 1 1 calc R . . H57C H 0.5284 0.3933 0.3656 0.043 Uiso 1 1 calc R . . C58 C 0.8723(6) 0.2570(5) 0.5271(3) 0.0335(15) Uani 1 1 d . . . H58A H 0.9357 0.3103 0.5184 0.050 Uiso 1 1 calc R . . H58B H 0.8819 0.2031 0.4960 0.050 Uiso 1 1 calc R . . H58C H 0.8900 0.2355 0.5707 0.050 Uiso 1 1 calc R . . Cl1S Cl 0.6764(3) 1.0194(2) 0.54036(16) 0.1101(12) Uani 1 1 d . . . Cl2S Cl 0.7933(3) 0.8919(2) 0.44972(13) 0.0995(10) Uani 1 1 d . . . C1S C 0.6700(10) 0.9068(6) 0.5040(5) 0.078(3) Uani 1 1 d . . . H1SA H 0.5824 0.8945 0.4813 0.093 Uiso 1 1 calc R . . H1SB H 0.6784 0.8582 0.5374 0.093 Uiso 1 1 calc R . . Cl3S Cl 0.94467(19) 0.48886(15) 0.08732(9) 0.0521(5) Uani 1 1 d . . . Cl4S Cl 0.6914(2) 0.47507(15) 0.01505(10) 0.0568(5) Uani 1 1 d . . . C2S C 0.8292(8) 0.4125(5) 0.0414(4) 0.0481(19) Uani 1 1 d . . . H2SA H 0.8728 0.3848 0.0037 0.058 Uiso 1 1 calc R . . H2SB H 0.7989 0.3583 0.0677 0.058 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 Fe1 0.0222(4) 0.0206(4) 0.0139(4) -0.0055(3) 0.0053(3) -0.0010(3) Cl1 0.0278(8) 0.0255(8) 0.0320(8) -0.0054(6) 0.0070(6) 0.0026(6) Cl2 0.0233(7) 0.0320(8) 0.0155(7) -0.0021(6) 0.0067(5) 0.0017(6) N1 0.022(2) 0.021(2) 0.014(2) -0.0029(19) 0.0033(19) -0.001(2) N2 0.024(2) 0.023(2) 0.013(2) -0.0024(19) 0.0017(19) -0.002(2) S1 0.0384(9) 0.0237(8) 0.0482(10) 0.0009(7) 0.0207(8) -0.0027(7) Cl5 0.0306(9) 0.0396(10) 0.0525(11) 0.0015(8) 0.0036(8) 0.0105(7) C1 0.020(3) 0.032(3) 0.012(3) -0.002(2) 0.002(2) 0.002(2) C2 0.025(3) 0.039(4) 0.020(3) -0.002(3) 0.006(2) -0.002(3) C3 0.035(4) 0.054(4) 0.015(3) -0.010(3) 0.011(3) -0.002(3) C4 0.034(4) 0.038(4) 0.017(3) -0.012(3) 0.003(3) 0.002(3) C5 0.029(3) 0.028(3) 0.021(3) -0.005(2) -0.001(2) 0.001(3) C6 0.052(4) 0.038(4) 0.019(3) -0.009(3) -0.002(3) 0.001(3) C7 0.057(5) 0.036(4) 0.026(4) -0.010(3) -0.003(3) -0.014(3) C8 0.042(4) 0.030(3) 0.018(3) -0.004(3) 0.002(3) -0.005(3) C9 0.024(3) 0.026(3) 0.013(3) -0.001(2) -0.001(2) -0.001(2) C10 0.024(3) 0.029(3) 0.011(3) -0.002(2) 0.000(2) 0.002(2) C11 0.021(3) 0.022(3) 0.015(3) 0.001(2) 0.004(2) 0.002(2) C12 0.021(3) 0.023(3) 0.017(3) -0.001(2) 0.004(2) 0.001(2) C13 0.028(3) 0.024(3) 0.023(3) -0.002(2) 0.010(3) -0.006(3) C14 0.038(4) 0.027(3) 0.029(3) -0.007(3) 0.012(3) -0.011(3) C15 0.031(3) 0.021(3) 0.028(3) 0.001(2) 0.011(3) -0.008(3) C16 0.027(3) 0.030(3) 0.027(3) 0.007(3) -0.001(3) -0.005(3) C17 0.027(3) 0.024(3) 0.024(3) -0.003(2) 0.005(3) -0.001(2) C18 0.028(3) 0.024(3) 0.027(3) 0.008(3) 0.005(3) -0.003(3) C19 0.032(4) 0.029(3) 0.034(4) 0.013(3) -0.007(3) -0.006(3) C20 0.038(4) 0.032(4) 0.024(3) 0.004(3) 0.004(3) -0.010(3) C21 0.019(3) 0.023(3) 0.013(3) -0.005(2) 0.001(2) -0.003(2) C22 0.030(3) 0.026(3) 0.013(3) -0.004(2) 0.003(2) 0.001(3) C23 0.018(3) 0.037(4) 0.025(3) -0.001(3) 0.006(2) -0.001(3) C24 0.034(4) 0.037(4) 0.020(3) -0.003(3) 0.012(3) -0.005(3) C25 0.040(4) 0.022(3) 0.024(3) 0.005(3) 0.007(3) -0.005(3) C26 0.029(3) 0.028(3) 0.016(3) -0.004(2) 0.003(2) -0.002(3) C27 0.024(3) 0.032(4) 0.038(4) 0.005(3) 0.003(3) 0.003(3) C28 0.035(4) 0.032(4) 0.031(4) 0.001(3) 0.011(3) 0.004(3) Fe2 0.0206(4) 0.0232(4) 0.0140(4) -0.0043(3) 0.0040(3) -0.0013(3) Cl3 0.0301(8) 0.0366(9) 0.0327(8) 0.0070(7) 0.0120(7) 0.0103(7) Cl4 0.0226(7) 0.0373(8) 0.0152(7) -0.0084(6) 0.0041(5) 0.0035(6) N3 0.018(2) 0.022(2) 0.012(2) 0.0006(18) 0.0043(18) -0.0018(19) N4 0.019(2) 0.026(3) 0.014(2) -0.0009(19) 0.0053(18) -0.004(2) S2 0.0360(9) 0.0287(9) 0.0417(10) 0.0094(7) 0.0219(8) 0.0041(7) Cl6 0.0368(10) 0.0714(14) 0.0616(13) 0.0158(10) 0.0094(9) 0.0229(9) C31 0.023(3) 0.022(3) 0.013(3) -0.003(2) 0.002(2) 0.003(2) C32 0.030(3) 0.024(3) 0.017(3) -0.003(2) 0.006(2) 0.002(2) C33 0.027(3) 0.037(4) 0.015(3) -0.007(3) 0.006(2) 0.005(3) C34 0.036(4) 0.028(3) 0.020(3) -0.010(3) 0.002(3) -0.004(3) C35 0.038(4) 0.023(3) 0.017(3) -0.006(2) 0.002(3) 0.000(3) C36 0.055(4) 0.027(3) 0.029(4) -0.009(3) 0.009(3) -0.015(3) C37 0.054(4) 0.035(4) 0.031(4) -0.007(3) 0.016(3) -0.020(3) C38 0.052(4) 0.031(4) 0.024(3) -0.007(3) 0.012(3) -0.015(3) C39 0.030(3) 0.017(3) 0.017(3) -0.005(2) 0.006(2) -0.001(2) C40 0.025(3) 0.023(3) 0.016(3) 0.001(2) -0.001(2) 0.003(2) C41 0.015(3) 0.028(3) 0.011(3) -0.003(2) 0.002(2) 0.002(2) C42 0.023(3) 0.025(3) 0.016(3) 0.001(2) 0.008(2) 0.001(2) C43 0.023(3) 0.026(3) 0.015(3) 0.000(2) 0.011(2) -0.001(2) C44 0.034(4) 0.033(4) 0.030(3) -0.005(3) 0.022(3) 0.001(3) C45 0.025(3) 0.027(3) 0.023(3) 0.000(2) 0.012(2) -0.005(2) C46 0.044(4) 0.025(3) 0.022(3) -0.001(3) 0.001(3) -0.004(3) C47 0.033(4) 0.038(4) 0.026(3) 0.008(3) -0.003(3) -0.011(3) C48 0.028(3) 0.038(4) 0.031(4) 0.012(3) 0.006(3) 0.005(3) C49 0.036(4) 0.056(5) 0.024(3) -0.006(3) 0.007(3) 0.007(3) C50 0.029(3) 0.048(4) 0.018(3) -0.004(3) 0.002(3) -0.001(3) C51 0.025(3) 0.026(3) 0.010(3) -0.010(2) 0.009(2) -0.007(2) C52 0.025(3) 0.020(3) 0.015(3) -0.007(2) 0.006(2) -0.008(2) C53 0.025(3) 0.024(3) 0.030(3) -0.007(3) 0.005(3) 0.000(2) C54 0.034(4) 0.025(3) 0.025(3) -0.002(3) 0.015(3) -0.001(3) C55 0.034(3) 0.030(3) 0.016(3) 0.002(2) 0.006(2) 0.003(3) C56 0.027(3) 0.021(3) 0.019(3) -0.006(2) 0.006(2) -0.002(2) C57 0.023(3) 0.036(4) 0.025(3) -0.003(3) 0.000(3) 0.001(3) C58 0.033(4) 0.048(4) 0.020(3) 0.006(3) 0.003(3) 0.000(3) Cl1S 0.088(2) 0.108(2) 0.127(3) -0.072(2) 0.0113(18) -0.0100(17) Cl2S 0.123(2) 0.104(2) 0.0698(17) -0.0310(16) 0.0237(17) -0.0037(18) C1S 0.079(7) 0.056(6) 0.096(8) -0.007(5) 0.005(6) -0.009(5) Cl3S 0.0515(11) 0.0628(13) 0.0409(11) -0.0128(9) 0.0069(9) -0.0014(9) Cl4S 0.0691(14) 0.0506(12) 0.0502(12) 0.0061(9) -0.0097(10) 0.0036(10) C2S 0.066(5) 0.028(4) 0.049(5) -0.011(3) 0.004(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 2.131(4) . ? Fe1 N1 2.196(4) . ? Fe1 Cl1 2.2596(16) . ? Fe1 Cl2 2.3917(16) . ? Fe1 Cl2 2.4810(16) 2_755 ? Cl2 Fe1 2.4809(15) 2_755 ? N1 C11 1.269(7) . ? N1 C13 1.472(7) . ? N2 C12 1.296(7) . ? N2 C21 1.447(7) . ? S1 C15 1.768(6) . ? S1 C14 1.800(6) . ? Cl5 C18 1.743(6) . ? C1 C2 1.382(8) . ? C1 C10 1.401(8) . ? C1 C11 1.476(7) . ? C2 C3 1.416(8) . ? C3 C4 1.353(9) . ? C4 C5 1.415(8) . ? C5 C6 1.405(9) . ? C5 C10 1.405(8) . ? C6 C7 1.372(9) . ? C7 C8 1.416(8) . ? C8 C9 1.369(8) . ? C9 C10 1.414(7) . ? C9 C12 1.453(8) . ? C11 C12 1.508(7) . ? C13 C14 1.516(8) . ? C15 C20 1.389(9) . ? C15 C16 1.402(8) . ? C16 C17 1.375(8) . ? C17 C18 1.357(8) . ? C18 C19 1.375(9) . ? C19 C20 1.384(9) . ? C21 C26 1.384(8) . ? C21 C22 1.393(8) . ? C22 C23 1.386(8) . ? C22 C27 1.502(8) . ? C23 C24 1.374(8) . ? C24 C25 1.369(9) . ? C25 C26 1.405(8) . ? C26 C28 1.493(8) . ? Fe2 N4 2.119(4) . ? Fe2 N3 2.223(4) . ? Fe2 Cl3 2.2477(17) . ? Fe2 Cl4 2.3548(16) . ? Fe2 Cl4 2.5367(15) 2_766 ? Cl4 Fe2 2.5368(15) 2_766 ? N3 C41 1.261(7) . ? N3 C43 1.469(6) . ? N4 C42 1.284(7) . ? N4 C51 1.445(6) . ? S2 C45 1.773(6) . ? S2 C44 1.811(6) . ? Cl6 C48 1.732(6) . ? C31 C32 1.368(7) . ? C31 C40 1.408(8) . ? C31 C41 1.489(7) . ? C32 C33 1.406(8) . ? C33 C34 1.355(8) . ? C34 C35 1.423(8) . ? C35 C40 1.398(8) . ? C35 C36 1.413(8) . ? C36 C37 1.381(9) . ? C37 C38 1.413(8) . ? C38 C39 1.361(8) . ? C39 C40 1.418(7) . ? C39 C42 1.460(8) . ? C41 C42 1.507(7) . ? C43 C44 1.499(8) . ? C45 C46 1.379(8) . ? C45 C50 1.380(8) . ? C46 C47 1.380(9) . ? C47 C48 1.385(9) . ? C48 C49 1.370(9) . ? C49 C50 1.376(9) . ? C51 C56 1.387(8) . ? C51 C52 1.398(8) . ? C52 C53 1.397(8) . ? C52 C57 1.497(8) . ? C53 C54 1.389(8) . ? C54 C55 1.356(8) . ? C55 C56 1.402(8) . ? C56 C58 1.495(8) . ? Cl1S C1S 1.702(9) . ? Cl2S C1S 1.730(10) . ? Cl3S C2S 1.761(7) . ? Cl4S C2S 1.755(8) . ? 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 Fe1 N1 78.18(16) . . ? N2 Fe1 Cl1 119.98(13) . . ? N1 Fe1 Cl1 99.85(13) . . ? N2 Fe1 Cl2 110.58(13) . . ? N1 Fe1 Cl2 85.88(12) . . ? Cl1 Fe1 Cl2 129.26(6) . . ? N2 Fe1 Cl2 90.68(12) . 2_755 ? N1 Fe1 Cl2 162.31(12) . 2_755 ? Cl1 Fe1 Cl2 97.62(6) . 2_755 ? Cl2 Fe1 Cl2 85.25(5) . 2_755 ? Fe1 Cl2 Fe1 94.75(5) . 2_755 ? C11 N1 C13 119.5(4) . . ? C11 N1 Fe1 111.3(4) . . ? C13 N1 Fe1 128.9(3) . . ? C12 N2 C21 120.5(4) . . ? C12 N2 Fe1 112.8(4) . . ? C21 N2 Fe1 126.7(3) . . ? C15 S1 C14 101.6(3) . . ? C2 C1 C10 118.7(5) . . ? C2 C1 C11 135.1(5) . . ? C10 C1 C11 106.2(5) . . ? C1 C2 C3 118.6(6) . . ? C4 C3 C2 122.7(6) . . ? C3 C4 C5 120.1(5) . . ? C6 C5 C10 115.9(5) . . ? C6 C5 C4 127.1(5) . . ? C10 C5 C4 117.0(5) . . ? C7 C6 C5 121.7(6) . . ? C6 C7 C8 121.5(6) . . ? C9 C8 C7 118.6(6) . . ? C8 C9 C10 119.5(5) . . ? C8 C9 C12 135.0(5) . . ? C10 C9 C12 105.5(5) . . ? C1 C10 C5 122.9(5) . . ? C1 C10 C9 114.3(5) . . ? C5 C10 C9 122.8(5) . . ? N1 C11 C1 135.5(5) . . ? N1 C11 C12 118.6(5) . . ? C1 C11 C12 105.8(4) . . ? N2 C12 C9 133.7(5) . . ? N2 C12 C11 118.2(5) . . ? C9 C12 C11 108.2(4) . . ? N1 C13 C14 112.0(5) . . ? C13 C14 S1 112.6(4) . . ? C20 C15 C16 119.1(6) . . ? C20 C15 S1 120.7(5) . . ? C16 C15 S1 120.1(5) . . ? C17 C16 C15 119.8(6) . . ? C18 C17 C16 119.9(6) . . ? C17 C18 C19 121.8(6) . . ? C17 C18 Cl5 118.8(5) . . ? C19 C18 Cl5 119.3(5) . . ? C18 C19 C20 118.9(6) . . ? C19 C20 C15 120.3(6) . . ? C26 C21 C22 122.7(5) . . ? C26 C21 N2 120.2(5) . . ? C22 C21 N2 116.9(5) . . ? C23 C22 C21 118.1(5) . . ? C23 C22 C27 120.6(5) . . ? C21 C22 C27 121.2(5) . . ? C24 C23 C22 120.6(6) . . ? C25 C24 C23 120.4(6) . . ? C24 C25 C26 121.4(6) . . ? C21 C26 C25 116.8(5) . . ? C21 C26 C28 122.2(5) . . ? C25 C26 C28 121.0(5) . . ? N4 Fe2 N3 77.61(16) . . ? N4 Fe2 Cl3 114.62(13) . . ? N3 Fe2 Cl3 96.00(12) . . ? N4 Fe2 Cl4 109.12(13) . . ? N3 Fe2 Cl4 88.92(12) . . ? Cl3 Fe2 Cl4 136.03(7) . . ? N4 Fe2 Cl4 92.54(12) . 2_766 ? N3 Fe2 Cl4 167.17(12) . 2_766 ? Cl3 Fe2 Cl4 95.59(6) . 2_766 ? Cl4 Fe2 Cl4 86.57(5) . 2_766 ? Fe2 Cl4 Fe2 93.43(5) . 2_766 ? C41 N3 C43 119.8(4) . . ? C41 N3 Fe2 111.2(3) . . ? C43 N3 Fe2 129.0(3) . . ? C42 N4 C51 119.1(5) . . ? C42 N4 Fe2 114.1(4) . . ? C51 N4 Fe2 126.5(3) . . ? C45 S2 C44 101.4(3) . . ? C32 C31 C40 119.2(5) . . ? C32 C31 C41 135.0(5) . . ? C40 C31 C41 105.8(4) . . ? C31 C32 C33 118.1(5) . . ? C34 C33 C32 123.3(5) . . ? C33 C34 C35 120.3(5) . . ? C40 C35 C36 117.1(5) . . ? C40 C35 C34 115.8(5) . . ? C36 C35 C34 127.1(5) . . ? C37 C36 C35 120.2(6) . . ? C36 C37 C38 122.0(6) . . ? C39 C38 C37 118.5(6) . . ? C38 C39 C40 120.0(5) . . ? C38 C39 C42 134.7(5) . . ? C40 C39 C42 105.3(5) . . ? C35 C40 C31 123.4(5) . . ? C35 C40 C39 122.0(5) . . ? C31 C40 C39 114.5(5) . . ? N3 C41 C31 135.2(5) . . ? N3 C41 C42 118.8(5) . . ? C31 C41 C42 105.8(4) . . ? N4 C42 C39 133.1(5) . . ? N4 C42 C41 118.2(5) . . ? C39 C42 C41 108.5(4) . . ? N3 C43 C44 111.8(4) . . ? C43 C44 S2 111.9(4) . . ? C46 C45 C50 119.4(6) . . ? C46 C45 S2 121.2(5) . . ? C50 C45 S2 119.3(5) . . ? C45 C46 C47 121.1(6) . . ? C46 C47 C48 118.1(6) . . ? C49 C48 C47 121.7(6) . . ? C49 C48 Cl6 119.5(5) . . ? C47 C48 Cl6 118.8(5) . . ? C48 C49 C50 119.2(6) . . ? C49 C50 C45 120.5(6) . . ? C56 C51 C52 123.3(5) . . ? C56 C51 N4 119.9(5) . . ? C52 C51 N4 116.7(5) . . ? C53 C52 C51 117.2(5) . . ? C53 C52 C57 121.2(5) . . ? C51 C52 C57 121.6(5) . . ? C54 C53 C52 120.4(6) . . ? C55 C54 C53 120.8(5) . . ? C54 C55 C56 121.4(5) . . ? C51 C56 C55 116.9(5) . . ? C51 C56 C58 121.3(5) . . ? C55 C56 C58 121.8(5) . . ? Cl1S C1S Cl2S 112.9(5) . . ? Cl4S C2S Cl3S 111.6(4) . . ? 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 Fe1 Cl2 Fe1 88.94(13) . . . 2_755 ? N1 Fe1 Cl2 Fe1 164.67(12) . . . 2_755 ? Cl1 Fe1 Cl2 Fe1 -95.97(8) . . . 2_755 ? Cl2 Fe1 Cl2 Fe1 0.0 2_755 . . 2_755 ? N2 Fe1 N1 C11 8.5(4) . . . . ? Cl1 Fe1 N1 C11 127.3(4) . . . . ? Cl2 Fe1 N1 C11 -103.5(4) . . . . ? Cl2 Fe1 N1 C11 -43.4(7) 2_755 . . . ? N2 Fe1 N1 C13 -177.1(5) . . . . ? Cl1 Fe1 N1 C13 -58.3(5) . . . . ? Cl2 Fe1 N1 C13 70.8(4) . . . . ? Cl2 Fe1 N1 C13 130.9(4) 2_755 . . . ? N1 Fe1 N2 C12 -7.1(4) . . . . ? Cl1 Fe1 N2 C12 -101.7(4) . . . . ? Cl2 Fe1 N2 C12 73.9(4) . . . . ? Cl2 Fe1 N2 C12 159.1(4) 2_755 . . . ? N1 Fe1 N2 C21 173.8(5) . . . . ? Cl1 Fe1 N2 C21 79.2(4) . . . . ? Cl2 Fe1 N2 C21 -105.2(4) . . . . ? Cl2 Fe1 N2 C21 -20.0(4) 2_755 . . . ? C10 C1 C2 C3 0.8(9) . . . . ? C11 C1 C2 C3 -177.9(6) . . . . ? C1 C2 C3 C4 0.4(10) . . . . ? C2 C3 C4 C5 -1.7(10) . . . . ? C3 C4 C5 C6 179.7(6) . . . . ? C3 C4 C5 C10 1.8(9) . . . . ? C10 C5 C6 C7 -0.9(10) . . . . ? C4 C5 C6 C7 -178.9(7) . . . . ? C5 C6 C7 C8 0.2(11) . . . . ? C6 C7 C8 C9 0.5(10) . . . . ? C7 C8 C9 C10 -0.3(9) . . . . ? C7 C8 C9 C12 176.1(6) . . . . ? C2 C1 C10 C5 -0.7(9) . . . . ? C11 C1 C10 C5 178.3(5) . . . . ? C2 C1 C10 C9 179.5(5) . . . . ? C11 C1 C10 C9 -1.5(7) . . . . ? C6 C5 C10 C1 -178.7(6) . . . . ? C4 C5 C10 C1 -0.6(9) . . . . ? C6 C5 C10 C9 1.1(9) . . . . ? C4 C5 C10 C9 179.2(5) . . . . ? C8 C9 C10 C1 179.4(5) . . . . ? C12 C9 C10 C1 2.0(7) . . . . ? C8 C9 C10 C5 -0.4(9) . . . . ? C12 C9 C10 C5 -177.8(5) . . . . ? C13 N1 C11 C1 -0.4(10) . . . . ? Fe1 N1 C11 C1 174.5(5) . . . . ? C13 N1 C11 C12 176.4(5) . . . . ? Fe1 N1 C11 C12 -8.7(6) . . . . ? C2 C1 C11 N1 -3.8(12) . . . . ? C10 C1 C11 N1 177.4(6) . . . . ? C2 C1 C11 C12 179.1(6) . . . . ? C10 C1 C11 C12 0.3(6) . . . . ? C21 N2 C12 C9 3.8(9) . . . . ? Fe1 N2 C12 C9 -175.4(5) . . . . ? C21 N2 C12 C11 -175.8(5) . . . . ? Fe1 N2 C12 C11 5.0(6) . . . . ? C8 C9 C12 N2 2.0(12) . . . . ? C10 C9 C12 N2 178.8(6) . . . . ? C8 C9 C12 C11 -178.4(6) . . . . ? C10 C9 C12 C11 -1.6(6) . . . . ? N1 C11 C12 N2 2.8(8) . . . . ? C1 C11 C12 N2 -179.5(5) . . . . ? N1 C11 C12 C9 -176.8(5) . . . . ? C1 C11 C12 C9 0.8(6) . . . . ? C11 N1 C13 C14 176.7(5) . . . . ? Fe1 N1 C13 C14 2.8(7) . . . . ? N1 C13 C14 S1 170.6(4) . . . . ? C15 S1 C14 C13 67.4(5) . . . . ? C14 S1 C15 C20 86.0(5) . . . . ? C14 S1 C15 C16 -98.4(5) . . . . ? C20 C15 C16 C17 -2.3(8) . . . . ? S1 C15 C16 C17 -178.0(4) . . . . ? C15 C16 C17 C18 1.1(9) . . . . ? C16 C17 C18 C19 1.0(9) . . . . ? C16 C17 C18 Cl5 -178.4(4) . . . . ? C17 C18 C19 C20 -1.9(9) . . . . ? Cl5 C18 C19 C20 177.5(4) . . . . ? C18 C19 C20 C15 0.7(9) . . . . ? C16 C15 C20 C19 1.4(9) . . . . ? S1 C15 C20 C19 177.1(4) . . . . ? C12 N2 C21 C26 -85.6(7) . . . . ? Fe1 N2 C21 C26 93.5(6) . . . . ? C12 N2 C21 C22 99.2(6) . . . . ? Fe1 N2 C21 C22 -81.7(6) . . . . ? C26 C21 C22 C23 1.9(8) . . . . ? N2 C21 C22 C23 176.9(5) . . . . ? C26 C21 C22 C27 -176.6(5) . . . . ? N2 C21 C22 C27 -1.5(8) . . . . ? C21 C22 C23 C24 -1.1(8) . . . . ? C27 C22 C23 C24 177.4(5) . . . . ? C22 C23 C24 C25 0.3(9) . . . . ? C23 C24 C25 C26 -0.3(9) . . . . ? C22 C21 C26 C25 -1.8(8) . . . . ? N2 C21 C26 C25 -176.7(5) . . . . ? C22 C21 C26 C28 178.8(5) . . . . ? N2 C21 C26 C28 3.9(8) . . . . ? C24 C25 C26 C21 1.0(8) . . . . ? C24 C25 C26 C28 -179.6(6) . . . . ? N4 Fe2 Cl4 Fe2 -91.50(13) . . . 2_766 ? N3 Fe2 Cl4 Fe2 -167.99(12) . . . 2_766 ? Cl3 Fe2 Cl4 Fe2 94.49(9) . . . 2_766 ? Cl4 Fe2 Cl4 Fe2 0.0 2_766 . . 2_766 ? N4 Fe2 N3 C41 -2.6(4) . . . . ? Cl3 Fe2 N3 C41 -116.6(4) . . . . ? Cl4 Fe2 N3 C41 107.2(4) . . . . ? Cl4 Fe2 N3 C41 37.9(8) 2_766 . . . ? N4 Fe2 N3 C43 174.6(5) . . . . ? Cl3 Fe2 N3 C43 60.7(4) . . . . ? Cl4 Fe2 N3 C43 -75.5(4) . . . . ? Cl4 Fe2 N3 C43 -144.8(5) 2_766 . . . ? N3 Fe2 N4 C42 1.8(4) . . . . ? Cl3 Fe2 N4 C42 92.8(4) . . . . ? Cl4 Fe2 N4 C42 -82.6(4) . . . . ? Cl4 Fe2 N4 C42 -169.9(4) 2_766 . . . ? N3 Fe2 N4 C51 -172.1(5) . . . . ? Cl3 Fe2 N4 C51 -81.1(4) . . . . ? Cl4 Fe2 N4 C51 103.5(4) . . . . ? Cl4 Fe2 N4 C51 16.2(4) 2_766 . . . ? C40 C31 C32 C33 1.4(8) . . . . ? C41 C31 C32 C33 -176.2(6) . . . . ? C31 C32 C33 C34 -1.6(9) . . . . ? C32 C33 C34 C35 1.7(9) . . . . ? C33 C34 C35 C40 -1.4(9) . . . . ? C33 C34 C35 C36 -179.7(6) . . . . ? C40 C35 C36 C37 3.3(10) . . . . ? C34 C35 C36 C37 -178.4(7) . . . . ? C35 C36 C37 C38 -3.1(11) . . . . ? C36 C37 C38 C39 2.3(11) . . . . ? C37 C38 C39 C40 -1.8(10) . . . . ? C37 C38 C39 C42 179.3(7) . . . . ? C36 C35 C40 C31 179.7(6) . . . . ? C34 C35 C40 C31 1.2(9) . . . . ? C36 C35 C40 C39 -2.9(9) . . . . ? C34 C35 C40 C39 178.6(5) . . . . ? C32 C31 C40 C35 -1.2(9) . . . . ? C41 C31 C40 C35 177.0(5) . . . . ? C32 C31 C40 C39 -178.8(5) . . . . ? C41 C31 C40 C39 -0.6(6) . . . . ? C38 C39 C40 C35 2.2(9) . . . . ? C42 C39 C40 C35 -178.6(5) . . . . ? C38 C39 C40 C31 179.8(6) . . . . ? C42 C39 C40 C31 -1.0(7) . . . . ? C43 N3 C41 C31 0.7(9) . . . . ? Fe2 N3 C41 C31 178.2(5) . . . . ? C43 N3 C41 C42 -174.5(5) . . . . ? Fe2 N3 C41 C42 3.0(6) . . . . ? C32 C31 C41 N3 4.0(12) . . . . ? C40 C31 C41 N3 -173.8(6) . . . . ? C32 C31 C41 C42 179.7(6) . . . . ? C40 C31 C41 C42 1.9(6) . . . . ? C51 N4 C42 C39 -0.8(10) . . . . ? Fe2 N4 C42 C39 -175.2(5) . . . . ? C51 N4 C42 C41 173.5(5) . . . . ? Fe2 N4 C42 C41 -0.9(6) . . . . ? C38 C39 C42 N4 -4.1(12) . . . . ? C40 C39 C42 N4 176.8(6) . . . . ? C38 C39 C42 C41 -178.8(7) . . . . ? C40 C39 C42 C41 2.1(6) . . . . ? N3 C41 C42 N4 -1.6(8) . . . . ? C31 C41 C42 N4 -178.1(5) . . . . ? N3 C41 C42 C39 174.0(5) . . . . ? C31 C41 C42 C39 -2.5(6) . . . . ? C41 N3 C43 C44 171.6(5) . . . . ? Fe2 N3 C43 C44 -5.4(7) . . . . ? N3 C43 C44 S2 -171.1(4) . . . . ? C45 S2 C44 C43 -71.7(5) . . . . ? C44 S2 C45 C46 -64.7(5) . . . . ? C44 S2 C45 C50 118.9(5) . . . . ? C50 C45 C46 C47 -0.2(9) . . . . ? S2 C45 C46 C47 -176.6(5) . . . . ? C45 C46 C47 C48 -0.9(9) . . . . ? C46 C47 C48 C49 2.3(9) . . . . ? C46 C47 C48 Cl6 -176.2(5) . . . . ? C47 C48 C49 C50 -2.6(10) . . . . ? Cl6 C48 C49 C50 175.9(5) . . . . ? C48 C49 C50 C45 1.4(10) . . . . ? C46 C45 C50 C49 0.0(9) . . . . ? S2 C45 C50 C49 176.4(5) . . . . ? C42 N4 C51 C56 97.3(6) . . . . ? Fe2 N4 C51 C56 -89.1(6) . . . . ? C42 N4 C51 C52 -85.5(6) . . . . ? Fe2 N4 C51 C52 88.1(5) . . . . ? C56 C51 C52 C53 0.1(8) . . . . ? N4 C51 C52 C53 -177.0(5) . . . . ? C56 C51 C52 C57 179.0(5) . . . . ? N4 C51 C52 C57 1.9(7) . . . . ? C51 C52 C53 C54 0.2(8) . . . . ? C57 C52 C53 C54 -178.8(5) . . . . ? C52 C53 C54 C55 -0.2(9) . . . . ? C53 C54 C55 C56 0.1(9) . . . . ? C52 C51 C56 C55 -0.2(8) . . . . ? N4 C51 C56 C55 176.8(5) . . . . ? C52 C51 C56 C58 178.6(5) . . . . ? N4 C51 C56 C58 -4.4(8) . . . . ? C54 C55 C56 C51 0.1(8) . . . . ? C54 C55 C56 C58 -178.7(6) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.057 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.112 #===END data_(3j)FeCl2_0.5THF _database_code_depnum_ccdc_archive 'CCDC 636876' _chemical_name_common 050019 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 Cl2 Fe N2 O0.50 S' _chemical_formula_weight 667.51 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.8801(13) _cell_length_b 17.027(2) _cell_length_c 16.671(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.91(2) _cell_angle_gamma 90.00 _cell_volume 3367.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.92 _cell_measurement_theta_max 20.90 _exptl_crystal_description block _exptl_crystal_colour 'dark amber' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8197 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'North et al. Acta Cryst. 1968, A24, 351' _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 'Bruker-Nonius MACH3S' _diffrn_measurement_method 'omega 2-theta scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 90 _diffrn_standards_decay_% ? _diffrn_reflns_number 6026 _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 24.71 _reflns_number_total 5731 _reflns_number_gt 4239 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0501P)^2^+1.1797P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5731 _refine_ls_number_parameters 412 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.1068 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.004 _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 Fe1 Fe 0.29987(4) 0.21299(3) 0.28810(3) 0.02640(13) Uani 1 1 d . . . S1 S 0.19965(7) 0.32969(5) 0.36922(5) 0.0297(2) Uani 1 1 d . . . Cl1 Cl 0.20361(8) 0.24163(6) 0.17089(5) 0.0447(2) Uani 1 1 d . . . Cl2 Cl 0.48197(7) 0.25994(5) 0.30403(5) 0.0391(2) Uani 1 1 d . . . N1 N 0.3117(2) 0.08687(15) 0.27443(14) 0.0255(6) Uani 1 1 d . . . N2 N 0.3032(2) 0.17340(15) 0.40976(14) 0.0234(6) Uani 1 1 d . . . C1 C 0.3563(2) -0.02897(18) 0.36683(18) 0.0248(7) Uani 1 1 d . . . C2 C 0.3768(3) -0.09783(18) 0.3271(2) 0.0311(7) Uani 1 1 d . . . H2A H 0.3740 -0.0997 0.2701 0.037 Uiso 1 1 calc R . . C3 C 0.4022(3) -0.16542(19) 0.3729(2) 0.0368(8) Uani 1 1 d . . . H3A H 0.4177 -0.2129 0.3456 0.044 Uiso 1 1 calc R . . C4 C 0.4056(3) -0.16584(19) 0.4556(2) 0.0335(8) Uani 1 1 d . . . H4A H 0.4219 -0.2131 0.4841 0.040 Uiso 1 1 calc R . . C5 C 0.3850(2) -0.09582(19) 0.49800(19) 0.0292(7) Uani 1 1 d . . . C6 C 0.3852(3) -0.0859(2) 0.5829(2) 0.0346(8) Uani 1 1 d . . . H6A H 0.4008 -0.1295 0.6173 0.042 Uiso 1 1 calc R . . C7 C 0.3630(3) -0.0142(2) 0.61524(19) 0.0352(8) Uani 1 1 d . . . H7A H 0.3628 -0.0098 0.6720 0.042 Uiso 1 1 calc R . . C8 C 0.3405(3) 0.0535(2) 0.56863(18) 0.0303(7) Uani 1 1 d . . . H8A H 0.3249 0.1025 0.5931 0.036 Uiso 1 1 calc R . . C9 C 0.3419(2) 0.04631(18) 0.48588(18) 0.0244(7) Uani 1 1 d . . . C10 C 0.3620(2) -0.02859(18) 0.45234(18) 0.0252(7) Uani 1 1 d . . . C11 C 0.3315(2) 0.05197(18) 0.34253(17) 0.0237(7) Uani 1 1 d . . . C12 C 0.3243(2) 0.10010(18) 0.41757(17) 0.0220(6) Uani 1 1 d . . . C13 C 0.2912(3) 0.22264(17) 0.48055(17) 0.0261(7) Uani 1 1 d . . . H13A H 0.3547 0.2124 0.5200 0.031 Uiso 1 1 calc R . . H13B H 0.2203 0.2091 0.5060 0.031 Uiso 1 1 calc R . . C14 C 0.2899(3) 0.30922(18) 0.45782(19) 0.0294(7) Uani 1 1 d . . . H14A H 0.3677 0.3262 0.4479 0.035 Uiso 1 1 calc R . . H14B H 0.2636 0.3403 0.5034 0.035 Uiso 1 1 calc R . . C15 C 0.0652(2) 0.29359(19) 0.39573(18) 0.0290(7) Uani 1 1 d . . . C16 C -0.0080(3) 0.2670(2) 0.33337(19) 0.0344(8) Uani 1 1 d . . . H16A H 0.0169 0.2646 0.2801 0.041 Uiso 1 1 calc R . . C17 C -0.1168(3) 0.2441(2) 0.3488(2) 0.0390(9) Uani 1 1 d . . . C18 C -0.1494(3) 0.2449(2) 0.4278(2) 0.0378(8) Uani 1 1 d . . . H18A H -0.2231 0.2280 0.4391 0.045 Uiso 1 1 calc R . . C19 C -0.0769(3) 0.2698(2) 0.49007(19) 0.0342(8) Uani 1 1 d . . . C20 C 0.0304(3) 0.2956(2) 0.47383(18) 0.0320(8) Uani 1 1 d . . . H20A H 0.0799 0.3145 0.5161 0.038 Uiso 1 1 calc R . . C21 C -0.1988(3) 0.2188(3) 0.2817(2) 0.0625(13) Uani 1 1 d . . . H21A H -0.1777 0.2429 0.2313 0.094 Uiso 1 1 calc R . . H21B H -0.2750 0.2356 0.2938 0.094 Uiso 1 1 calc R . . H21C H -0.1970 0.1615 0.2765 0.094 Uiso 1 1 calc R . . C22 C -0.1145(3) 0.2686(3) 0.5757(2) 0.0490(10) Uani 1 1 d . . . H22A H -0.1685 0.2257 0.5818 0.074 Uiso 1 1 calc R . . H22B H -0.1504 0.3187 0.5878 0.074 Uiso 1 1 calc R . . H22C H -0.0489 0.2604 0.6128 0.074 Uiso 1 1 calc R . . C23 C 0.2985(3) 0.03953(19) 0.20190(18) 0.0301(7) Uani 1 1 d . . . C24 C 0.3903(3) 0.02699(19) 0.15412(18) 0.0345(8) Uani 1 1 d . . . C25 C 0.3709(4) -0.0178(2) 0.0853(2) 0.0561(12) Uani 1 1 d . . . H25A H 0.4315 -0.0277 0.0516 0.067 Uiso 1 1 calc R . . C26 C 0.2663(4) -0.0485(3) 0.0644(2) 0.0720(15) Uani 1 1 d . . . H26A H 0.2555 -0.0789 0.0169 0.086 Uiso 1 1 calc R . . C27 C 0.1774(4) -0.0352(3) 0.1121(3) 0.0637(13) Uani 1 1 d . . . H27A H 0.1056 -0.0567 0.0973 0.076 Uiso 1 1 calc R . . C28 C 0.1908(3) 0.0093(2) 0.1817(2) 0.0431(9) Uani 1 1 d . . . C29 C 0.0910(3) 0.0236(2) 0.2332(3) 0.0584(12) Uani 1 1 d . . . H29A H 0.1136 0.0630 0.2755 0.070 Uiso 1 1 calc R . . C30 C -0.0090(5) 0.0551(4) 0.1849(5) 0.126(3) Uani 1 1 d . . . H30A H 0.0124 0.1034 0.1575 0.190 Uiso 1 1 calc R . . H30B H -0.0699 0.0666 0.2206 0.190 Uiso 1 1 calc R . . H30C H -0.0348 0.0160 0.1449 0.190 Uiso 1 1 calc R . . C31 C 0.0554(4) -0.0511(3) 0.2743(3) 0.0807(15) Uani 1 1 d . . . H31A H 0.1183 -0.0710 0.3087 0.121 Uiso 1 1 calc R . . H31B H 0.0337 -0.0906 0.2336 0.121 Uiso 1 1 calc R . . H31C H -0.0089 -0.0400 0.3070 0.121 Uiso 1 1 calc R . . C32 C 0.5061(3) 0.06037(19) 0.17303(19) 0.0346(8) Uani 1 1 d . . . H32A H 0.5092 0.0789 0.2300 0.041 Uiso 1 1 calc R . . C33 C 0.5999(3) -0.0002(2) 0.1649(2) 0.0491(10) Uani 1 1 d . . . H33A H 0.5843 -0.0464 0.1975 0.074 Uiso 1 1 calc R . . H33B H 0.6722 0.0229 0.1834 0.074 Uiso 1 1 calc R . . H33C H 0.6033 -0.0157 0.1084 0.074 Uiso 1 1 calc R . . C34 C 0.5261(3) 0.1312(2) 0.1196(2) 0.0437(9) Uani 1 1 d . . . H34A H 0.4679 0.1709 0.1277 0.066 Uiso 1 1 calc R . . H34B H 0.5225 0.1147 0.0632 0.066 Uiso 1 1 calc R . . H34C H 0.6005 0.1536 0.1336 0.066 Uiso 1 1 calc R . . O1S O 0.1046(4) 0.0216(3) 0.4431(3) 0.0496(14) Uani 0.50 1 d P . . C1S C 0.0313(12) 0.0815(8) 0.4677(10) 0.081(4) Uani 0.50 1 d P . . H1SA H 0.0113 0.1170 0.4221 0.097 Uiso 0.50 1 calc PR . . H1SB H 0.0685 0.1129 0.5114 0.097 Uiso 0.50 1 calc PR . . C2S C 0.087(2) -0.0419(19) 0.4958(17) 0.065(7) Uani 0.50 1 d P . . H2SA H 0.1242 -0.0319 0.5493 0.078 Uiso 0.50 1 calc PR . . H2SB H 0.1172 -0.0913 0.4740 0.078 Uiso 0.50 1 calc PR . . C4S C -0.0413(11) -0.0468(7) 0.5012(8) 0.060(3) Uani 0.50 1 d P . . H4SA H -0.0633 -0.0693 0.5529 0.072 Uiso 0.50 1 calc PR . . H4SB H -0.0777 -0.0766 0.4560 0.072 Uiso 0.50 1 calc PR . . C3S C -0.067(3) 0.0451(16) 0.495(2) 0.090(9) Uani 0.50 1 d P . . H3SA H -0.1320 0.0549 0.4567 0.108 Uiso 0.50 1 calc PR . . H3SB H -0.0850 0.0662 0.5481 0.108 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0349(3) 0.0260(2) 0.0185(2) 0.00268(19) 0.00320(18) 0.0003(2) S1 0.0304(4) 0.0309(5) 0.0284(4) 0.0044(3) 0.0066(3) 0.0011(3) Cl1 0.0547(6) 0.0582(6) 0.0208(4) 0.0090(4) -0.0009(4) 0.0081(5) Cl2 0.0330(4) 0.0428(5) 0.0423(5) 0.0043(4) 0.0108(4) -0.0045(4) N1 0.0304(14) 0.0253(14) 0.0212(14) -0.0014(11) 0.0061(11) -0.0011(11) N2 0.0243(13) 0.0261(14) 0.0203(13) -0.0022(11) 0.0049(10) 0.0017(11) C1 0.0237(16) 0.0263(17) 0.0248(16) -0.0003(13) 0.0060(13) 0.0014(13) C2 0.0357(19) 0.0282(18) 0.0298(18) -0.0025(15) 0.0056(14) -0.0005(15) C3 0.041(2) 0.0253(19) 0.045(2) 0.0001(16) 0.0073(16) -0.0009(15) C4 0.0297(17) 0.0266(19) 0.045(2) 0.0109(16) 0.0059(15) 0.0044(14) C5 0.0209(16) 0.0335(19) 0.0335(18) 0.0116(15) 0.0050(13) 0.0002(14) C6 0.0284(18) 0.041(2) 0.0346(19) 0.0171(16) -0.0001(14) -0.0007(15) C7 0.0303(18) 0.054(2) 0.0214(17) 0.0093(16) 0.0049(14) 0.0006(16) C8 0.0256(17) 0.043(2) 0.0224(16) 0.0025(15) 0.0051(13) 0.0008(15) C9 0.0225(16) 0.0282(17) 0.0227(16) 0.0027(13) 0.0047(12) 0.0012(13) C10 0.0198(15) 0.0304(18) 0.0257(16) 0.0031(14) 0.0043(12) -0.0013(13) C11 0.0239(16) 0.0254(16) 0.0224(16) -0.0001(13) 0.0082(12) -0.0020(13) C12 0.0230(15) 0.0248(17) 0.0186(15) 0.0017(13) 0.0052(12) -0.0012(13) C13 0.0295(16) 0.0313(18) 0.0177(15) -0.0044(13) 0.0024(12) -0.0006(14) C14 0.0304(17) 0.0301(18) 0.0278(17) -0.0056(14) 0.0025(14) -0.0013(14) C15 0.0228(16) 0.0355(19) 0.0291(17) 0.0070(15) 0.0045(13) 0.0067(14) C16 0.0328(18) 0.049(2) 0.0214(17) 0.0059(15) 0.0048(14) 0.0063(16) C17 0.0295(18) 0.061(2) 0.0264(18) -0.0002(17) 0.0023(14) 0.0014(17) C18 0.0319(18) 0.052(2) 0.0296(19) 0.0045(17) 0.0067(15) -0.0034(17) C19 0.0305(18) 0.046(2) 0.0274(18) 0.0007(15) 0.0087(14) 0.0053(15) C20 0.0316(18) 0.043(2) 0.0218(16) 0.0007(15) 0.0014(13) 0.0057(16) C21 0.034(2) 0.124(4) 0.030(2) -0.009(2) 0.0012(16) -0.012(2) C22 0.045(2) 0.077(3) 0.0265(19) -0.0061(19) 0.0131(16) -0.012(2) C23 0.044(2) 0.0264(17) 0.0200(16) -0.0001(13) 0.0005(14) -0.0033(15) C24 0.054(2) 0.0304(19) 0.0198(16) -0.0020(14) 0.0078(15) -0.0058(16) C25 0.077(3) 0.060(3) 0.034(2) -0.021(2) 0.024(2) -0.026(2) C26 0.094(4) 0.085(3) 0.038(2) -0.031(2) 0.013(2) -0.041(3) C27 0.066(3) 0.072(3) 0.053(3) -0.020(2) -0.002(2) -0.030(2) C28 0.046(2) 0.042(2) 0.041(2) -0.0077(17) 0.0023(17) -0.0100(18) C29 0.041(2) 0.054(3) 0.081(3) -0.027(2) 0.006(2) -0.011(2) C30 0.064(4) 0.121(5) 0.195(8) 0.065(5) 0.017(4) 0.020(4) C31 0.069(3) 0.103(4) 0.073(3) 0.003(3) 0.029(3) -0.003(3) C32 0.050(2) 0.0335(19) 0.0214(17) -0.0063(14) 0.0098(15) -0.0019(16) C33 0.062(3) 0.048(2) 0.039(2) -0.0017(18) 0.0135(19) 0.014(2) C34 0.052(2) 0.034(2) 0.046(2) -0.0030(17) 0.0119(18) -0.0053(17) O1S 0.029(3) 0.052(3) 0.069(4) 0.011(3) 0.015(3) 0.002(2) C1S 0.056(7) 0.066(9) 0.125(13) 0.009(7) 0.043(8) 0.007(7) C2S 0.029(8) 0.064(11) 0.100(12) 0.027(9) -0.010(10) -0.025(7) C4S 0.048(7) 0.066(9) 0.067(8) 0.003(6) 0.016(5) -0.016(6) C3S 0.059(15) 0.046(11) 0.168(18) 0.046(10) 0.050(10) 0.020(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 Fe1 N2 2.136(2) . ? Fe1 N1 2.165(3) . ? Fe1 Cl1 2.2665(10) . ? Fe1 Cl2 2.3089(10) . ? Fe1 S1 2.7126(10) . ? S1 C15 1.787(3) . ? S1 C14 1.814(3) . ? N1 C11 1.292(4) . ? N1 C23 1.455(4) . ? N2 C12 1.278(4) . ? N2 C13 1.460(4) . ? C1 C2 1.374(4) . ? C1 C10 1.424(4) . ? C1 C11 1.462(4) . ? C2 C3 1.405(5) . ? C3 C4 1.378(5) . ? C4 C5 1.414(5) . ? C5 C10 1.394(4) . ? C5 C6 1.426(5) . ? C6 C7 1.366(5) . ? C7 C8 1.409(5) . ? C8 C9 1.386(4) . ? C9 C10 1.418(4) . ? C9 C12 1.468(4) . ? C11 C12 1.502(4) . ? C13 C14 1.522(4) . ? C15 C20 1.386(4) . ? C15 C16 1.397(4) . ? C16 C17 1.387(5) . ? C17 C18 1.391(5) . ? C17 C21 1.508(5) . ? C18 C19 1.381(5) . ? C19 C20 1.388(4) . ? C19 C22 1.517(4) . ? C23 C24 1.400(5) . ? C23 C28 1.403(5) . ? C24 C25 1.388(5) . ? C24 C32 1.507(5) . ? C25 C26 1.376(6) . ? C26 C27 1.372(6) . ? C27 C28 1.387(5) . ? C28 C29 1.519(5) . ? C29 C30 1.501(7) . ? C29 C31 1.514(6) . ? C32 C34 1.525(5) . ? C32 C33 1.528(5) . ? O1S C4S 1.297(13) 3_556 ? O1S C1S 1.415(14) . ? O1S C2S 1.42(3) . ? O1S C3S 1.61(3) 3_556 ? C1S C3S 1.42(3) . ? C2S C4S 1.53(3) . ? C4S C3S 1.60(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N1 77.81(9) . . ? N2 Fe1 Cl1 150.56(7) . . ? N1 Fe1 Cl1 98.92(7) . . ? N2 Fe1 Cl2 91.60(7) . . ? N1 Fe1 Cl2 106.88(7) . . ? Cl1 Fe1 Cl2 116.96(4) . . ? N2 Fe1 S1 75.24(7) . . ? N1 Fe1 S1 144.24(7) . . ? Cl1 Fe1 S1 93.28(3) . . ? Cl2 Fe1 S1 96.97(3) . . ? C15 S1 C14 103.37(15) . . ? C15 S1 Fe1 106.96(11) . . ? C14 S1 Fe1 90.51(10) . . ? C11 N1 C23 118.8(3) . . ? C11 N1 Fe1 111.9(2) . . ? C23 N1 Fe1 129.22(19) . . ? C12 N2 C13 120.3(3) . . ? C12 N2 Fe1 113.51(19) . . ? C13 N2 Fe1 126.04(19) . . ? C2 C1 C10 119.1(3) . . ? C2 C1 C11 135.1(3) . . ? C10 C1 C11 105.8(3) . . ? C1 C2 C3 118.4(3) . . ? C4 C3 C2 122.8(3) . . ? C3 C4 C5 120.0(3) . . ? C10 C5 C4 117.0(3) . . ? C10 C5 C6 115.8(3) . . ? C4 C5 C6 127.2(3) . . ? C7 C6 C5 120.4(3) . . ? C6 C7 C8 123.3(3) . . ? C9 C8 C7 117.7(3) . . ? C8 C9 C10 118.9(3) . . ? C8 C9 C12 135.1(3) . . ? C10 C9 C12 106.0(3) . . ? C5 C10 C9 123.7(3) . . ? C5 C10 C1 122.8(3) . . ? C9 C10 C1 113.5(3) . . ? N1 C11 C1 134.6(3) . . ? N1 C11 C12 117.7(3) . . ? C1 C11 C12 107.6(2) . . ? N2 C12 C9 135.0(3) . . ? N2 C12 C11 117.9(3) . . ? C9 C12 C11 107.1(3) . . ? N2 C13 C14 110.8(2) . . ? C13 C14 S1 112.8(2) . . ? C20 C15 C16 120.2(3) . . ? C20 C15 S1 122.5(3) . . ? C16 C15 S1 117.2(2) . . ? C17 C16 C15 120.3(3) . . ? C16 C17 C18 118.7(3) . . ? C16 C17 C21 121.1(3) . . ? C18 C17 C21 120.3(3) . . ? C19 C18 C17 121.5(3) . . ? C18 C19 C20 119.6(3) . . ? C18 C19 C22 120.1(3) . . ? C20 C19 C22 120.3(3) . . ? C15 C20 C19 119.7(3) . . ? C24 C23 C28 122.3(3) . . ? C24 C23 N1 120.2(3) . . ? C28 C23 N1 117.4(3) . . ? C25 C24 C23 116.9(3) . . ? C25 C24 C32 119.5(3) . . ? C23 C24 C32 123.6(3) . . ? C26 C25 C24 121.9(4) . . ? C27 C26 C25 120.2(4) . . ? C26 C27 C28 121.0(4) . . ? C27 C28 C23 117.7(3) . . ? C27 C28 C29 120.0(3) . . ? C23 C28 C29 122.3(3) . . ? C30 C29 C31 108.2(4) . . ? C30 C29 C28 111.9(4) . . ? C31 C29 C28 111.4(4) . . ? C24 C32 C34 110.1(3) . . ? C24 C32 C33 112.9(3) . . ? C34 C32 C33 110.2(3) . . ? C4S O1S C1S 33.6(6) 3_556 . ? C4S O1S C2S 72.5(16) 3_556 . ? C1S O1S C2S 105.0(16) . . ? C4S O1S C3S 65.5(14) 3_556 3_556 ? C1S O1S C3S 97.3(14) . 3_556 ? C2S O1S C3S 8(2) . 3_556 ? O1S C1S C3S 107.9(15) . . ? O1S C2S C4S 104.8(18) . . ? C2S C4S C3S 97.5(18) . . ? C1S C3S C4S 107(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 N2 Fe1 S1 C15 -71.39(13) . . . . ? N1 Fe1 S1 C15 -29.10(17) . . . . ? Cl1 Fe1 S1 C15 81.11(11) . . . . ? Cl2 Fe1 S1 C15 -161.21(11) . . . . ? N2 Fe1 S1 C14 32.76(12) . . . . ? N1 Fe1 S1 C14 75.05(16) . . . . ? Cl1 Fe1 S1 C14 -174.74(11) . . . . ? Cl2 Fe1 S1 C14 -57.06(11) . . . . ? N2 Fe1 N1 C11 -9.5(2) . . . . ? Cl1 Fe1 N1 C11 -159.77(19) . . . . ? Cl2 Fe1 N1 C11 78.4(2) . . . . ? S1 Fe1 N1 C11 -51.3(3) . . . . ? N2 Fe1 N1 C23 169.2(3) . . . . ? Cl1 Fe1 N1 C23 19.0(3) . . . . ? Cl2 Fe1 N1 C23 -102.8(2) . . . . ? S1 Fe1 N1 C23 127.5(2) . . . . ? N1 Fe1 N2 C12 8.3(2) . . . . ? Cl1 Fe1 N2 C12 94.9(2) . . . . ? Cl2 Fe1 N2 C12 -98.6(2) . . . . ? S1 Fe1 N2 C12 164.6(2) . . . . ? N1 Fe1 N2 C13 -175.9(2) . . . . ? Cl1 Fe1 N2 C13 -89.3(3) . . . . ? Cl2 Fe1 N2 C13 77.2(2) . . . . ? S1 Fe1 N2 C13 -19.6(2) . . . . ? C10 C1 C2 C3 0.3(5) . . . . ? C11 C1 C2 C3 177.6(3) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C2 C3 C4 C5 -1.1(5) . . . . ? C3 C4 C5 C10 -0.2(5) . . . . ? C3 C4 C5 C6 -180.0(3) . . . . ? C10 C5 C6 C7 0.5(4) . . . . ? C4 C5 C6 C7 -179.7(3) . . . . ? C5 C6 C7 C8 -0.9(5) . . . . ? C6 C7 C8 C9 -0.4(5) . . . . ? C7 C8 C9 C10 2.0(4) . . . . ? C7 C8 C9 C12 -179.6(3) . . . . ? C4 C5 C10 C9 -178.6(3) . . . . ? C6 C5 C10 C9 1.2(4) . . . . ? C4 C5 C10 C1 1.6(4) . . . . ? C6 C5 C10 C1 -178.6(3) . . . . ? C8 C9 C10 C5 -2.5(5) . . . . ? C12 C9 C10 C5 178.7(3) . . . . ? C8 C9 C10 C1 177.3(3) . . . . ? C12 C9 C10 C1 -1.5(3) . . . . ? C2 C1 C10 C5 -1.6(5) . . . . ? C11 C1 C10 C5 -179.7(3) . . . . ? C2 C1 C10 C9 178.5(3) . . . . ? C11 C1 C10 C9 0.5(3) . . . . ? C23 N1 C11 C1 7.3(5) . . . . ? Fe1 N1 C11 C1 -173.8(3) . . . . ? C23 N1 C11 C12 -169.3(3) . . . . ? Fe1 N1 C11 C12 9.6(3) . . . . ? C2 C1 C11 N1 6.3(6) . . . . ? C10 C1 C11 N1 -176.2(3) . . . . ? C2 C1 C11 C12 -176.9(3) . . . . ? C10 C1 C11 C12 0.7(3) . . . . ? C13 N2 C12 C9 -0.2(5) . . . . ? Fe1 N2 C12 C9 175.9(3) . . . . ? C13 N2 C12 C11 177.8(2) . . . . ? Fe1 N2 C12 C11 -6.1(3) . . . . ? C8 C9 C12 N2 1.4(6) . . . . ? C10 C9 C12 N2 180.0(3) . . . . ? C8 C9 C12 C11 -176.7(3) . . . . ? C10 C9 C12 C11 1.8(3) . . . . ? N1 C11 C12 N2 -2.6(4) . . . . ? C1 C11 C12 N2 179.9(3) . . . . ? N1 C11 C12 C9 175.9(3) . . . . ? C1 C11 C12 C9 -1.6(3) . . . . ? C12 N2 C13 C14 168.7(3) . . . . ? Fe1 N2 C13 C14 -6.9(3) . . . . ? N2 C13 C14 S1 45.2(3) . . . . ? C15 S1 C14 C13 57.2(2) . . . . ? Fe1 S1 C14 C13 -50.4(2) . . . . ? C14 S1 C15 C20 32.6(3) . . . . ? Fe1 S1 C15 C20 127.3(3) . . . . ? C14 S1 C15 C16 -151.2(3) . . . . ? Fe1 S1 C15 C16 -56.5(3) . . . . ? C20 C15 C16 C17 1.5(5) . . . . ? S1 C15 C16 C17 -174.9(3) . . . . ? C15 C16 C17 C18 -2.8(5) . . . . ? C15 C16 C17 C21 177.1(4) . . . . ? C16 C17 C18 C19 1.6(6) . . . . ? C21 C17 C18 C19 -178.2(4) . . . . ? C17 C18 C19 C20 0.8(6) . . . . ? C17 C18 C19 C22 -178.8(4) . . . . ? C16 C15 C20 C19 1.0(5) . . . . ? S1 C15 C20 C19 177.2(3) . . . . ? C18 C19 C20 C15 -2.2(5) . . . . ? C22 C19 C20 C15 177.5(3) . . . . ? C11 N1 C23 C24 -95.6(4) . . . . ? Fe1 N1 C23 C24 85.7(3) . . . . ? C11 N1 C23 C28 85.8(4) . . . . ? Fe1 N1 C23 C28 -92.9(3) . . . . ? C28 C23 C24 C25 -0.6(5) . . . . ? N1 C23 C24 C25 -179.1(3) . . . . ? C28 C23 C24 C32 178.4(3) . . . . ? N1 C23 C24 C32 -0.1(5) . . . . ? C23 C24 C25 C26 0.3(6) . . . . ? C32 C24 C25 C26 -178.8(4) . . . . ? C24 C25 C26 C27 -0.1(7) . . . . ? C25 C26 C27 C28 0.2(8) . . . . ? C26 C27 C28 C23 -0.6(7) . . . . ? C26 C27 C28 C29 179.6(4) . . . . ? C24 C23 C28 C27 0.8(6) . . . . ? N1 C23 C28 C27 179.3(3) . . . . ? C24 C23 C28 C29 -179.4(3) . . . . ? N1 C23 C28 C29 -0.9(5) . . . . ? C27 C28 C29 C30 -52.0(6) . . . . ? C23 C28 C29 C30 128.2(5) . . . . ? C27 C28 C29 C31 69.2(5) . . . . ? C23 C28 C29 C31 -110.6(4) . . . . ? C25 C24 C32 C34 76.4(4) . . . . ? C23 C24 C32 C34 -102.6(4) . . . . ? C25 C24 C32 C33 -47.2(4) . . . . ? C23 C24 C32 C33 133.8(3) . . . . ? C4S O1S C1S C3S -48.9(18) 3_556 . . . ? C2S O1S C1S C3S -33.9(16) . . . . ? C3S O1S C1S C3S -31(2) 3_556 . . . ? C4S O1S C2S C4S 52.5(18) 3_556 . . . ? C1S O1S C2S C4S 43.9(18) . . . . ? C3S O1S C2S C4S 21(12) 3_556 . . . ? O1S C2S C4S C3S -35(3) . . . . ? O1S C1S C3S C4S 10(2) . . . . ? C2S C4S C3S C1S 15(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.373 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.059 #===END