Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Holland, Patrick' 'Lachicotte, Rene J.' 'Smith, Jeremy M.' _publ_contact_author_name 'Dr Patrick Holland' _publ_contact_author_address ; Chemistry Department University of Rochester Rochester 14627 UNITED STATES OF AMERICA ; _publ_contact_author_email 'HOLLAND@CHEM.ROCHESTER.EDU' _publ_section_title ; Tuning Metal Coordination Number by Ancillary Ligand Steric Effects: Synthesis of a Three-Coordinate Iron(II) Complex ; data_js01b _database_code_CSD 167176 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point '310 (dec)' _chemical_formula_moiety ? _chemical_formula_sum 'C37 H57 Cl2 Fe Li N2 O2' _chemical_formula_weight 695.54 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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 ? _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 23.1015(12) _cell_length_b 9.3748(5) _cell_length_c 35.9530(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7786.4(7) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8196 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.64 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 0.556 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.826 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 SMART CCD _diffrn_measurement_method SMART CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32164 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 23.24 _reflns_number_total 10201 _reflns_number_gt 9540 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SIR-92 _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^)+(0.0376P)^2^+5.8206P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.038(17) _refine_ls_number_reflns 10201 _refine_ls_number_parameters 811 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.0983 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.143 _refine_ls_restrained_S_all 1.143 _refine_ls_shift/su_max 0.160 _refine_ls_shift/su_mean 0.016 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 0.28692(2) 0.01759(6) 0.387606(18) 0.02756(15) Uani 1 1 d . . . Cl11 Cl 0.31805(6) 0.24722(12) 0.37371(5) 0.0460(4) Uani 1 1 d . . . Cl21 Cl 0.22080(6) 0.00111(13) 0.33857(4) 0.0441(3) Uani 1 1 d . . . O11 O 0.26371(16) 0.2907(4) 0.28119(12) 0.0540(11) Uani 1 1 d . . . O21 O 0.18704(14) 0.3931(3) 0.34693(10) 0.0435(9) Uani 1 1 d . . . N11 N 0.35139(14) -0.1233(3) 0.39451(10) 0.0251(8) Uani 1 1 d . . . N21 N 0.25004(15) -0.0309(4) 0.43700(10) 0.0275(9) Uani 1 1 d . . . Li11 Li 0.2414(4) 0.2461(8) 0.3304(3) 0.040(3) Uani 1 1 d . . . C1S C 0.2275(3) 0.3180(8) 0.24970(19) 0.073(2) Uani 1 1 d . . . H1SA H 0.1974 0.3891 0.2560 0.088 Uiso 1 1 calc R . . H1SB H 0.2083 0.2291 0.2414 0.088 Uiso 1 1 calc R . . C2S C 0.2656(3) 0.3727(9) 0.22072(19) 0.084(2) Uani 1 1 d . . . H2SA H 0.2655 0.4783 0.2206 0.101 Uiso 1 1 calc R . . H2SB H 0.2532 0.3382 0.1960 0.101 Uiso 1 1 calc R . . C3S C 0.3254(3) 0.3160(9) 0.2303(2) 0.077(2) Uani 1 1 d . . . H3SA H 0.3393 0.2489 0.2110 0.092 Uiso 1 1 calc R . . H3SB H 0.3536 0.3949 0.2328 0.092 Uiso 1 1 calc R . . C4S C 0.3170(2) 0.2416(6) 0.2665(2) 0.0496(18) Uani 1 1 d . . . H4SA H 0.3158 0.1370 0.2627 0.059 Uiso 1 1 calc R . . H4SB H 0.3492 0.2643 0.2837 0.059 Uiso 1 1 calc R . . C5S C 0.1982(4) 0.5378(6) 0.3372(2) 0.080(2) Uani 1 1 d . . . H5SA H 0.1690 0.5719 0.3192 0.096 Uiso 1 1 calc R . . H5SB H 0.2370 0.5466 0.3257 0.096 Uiso 1 1 calc R . . C6S C 0.1955(6) 0.6205(8) 0.3707(3) 0.164(5) Uani 1 1 d . . . H6SA H 0.2348 0.6522 0.3777 0.197 Uiso 1 1 calc R . . H6SB H 0.1713 0.7063 0.3665 0.197 Uiso 1 1 calc R . . C7S C 0.1714(3) 0.5373(7) 0.39964(19) 0.080(2) Uani 1 1 d . . . H7SA H 0.1325 0.5733 0.4065 0.096 Uiso 1 1 calc R . . H7SB H 0.1965 0.5400 0.4219 0.096 Uiso 1 1 calc R . . C8S C 0.1674(2) 0.3890(5) 0.38473(17) 0.0481(13) Uani 1 1 d . . . H8SA H 0.1919 0.3238 0.3996 0.058 Uiso 1 1 calc R . . H8SB H 0.1269 0.3546 0.3858 0.058 Uiso 1 1 calc R . . C11 C 0.3951(2) -0.3461(5) 0.41797(15) 0.0409(13) Uani 1 1 d . . . H11A H 0.4220 -0.3270 0.3975 0.061 Uiso 1 1 calc R . . H11B H 0.3770 -0.4395 0.4143 0.061 Uiso 1 1 calc R . . H11C H 0.4163 -0.3456 0.4416 0.061 Uiso 1 1 calc R . . C12 C 0.40219(18) -0.1103(4) 0.37116(14) 0.0299(11) Uani 1 1 d . . . C13 C 0.21068(19) 0.0733(5) 0.45203(12) 0.0288(10) Uani 1 1 d . . . C21 C 0.3487(2) -0.2316(4) 0.41875(15) 0.0268(13) Uani 1 1 d . . . C22 C 0.4484(2) -0.0229(5) 0.38334(16) 0.0400(12) Uani 1 1 d . . . C23 C 0.2350(2) 0.1948(5) 0.47033(14) 0.0316(11) Uani 1 1 d . . . C31 C 0.3058(2) -0.2429(4) 0.44661(16) 0.0280(13) Uani 1 1 d . . . H31A H 0.3068 -0.3283 0.4608 0.034 Uiso 1 1 calc R . . C32 C 0.4983(2) -0.0165(7) 0.36175(18) 0.0593(17) Uani 1 1 d . . . H32A H 0.5298 0.0410 0.3697 0.071 Uiso 1 1 calc R . . C52 C 0.4566(2) -0.1724(6) 0.31637(17) 0.0508(14) Uani 1 1 d . . . H32B H 0.4594 -0.2203 0.2932 0.061 Uiso 1 1 calc R . . C33 C 0.1973(3) 0.2988(6) 0.48386(15) 0.0462(14) Uani 1 1 d . . . H34A H 0.2124 0.3795 0.4965 0.055 Uiso 1 1 calc R . . C41 C 0.26272(19) -0.1478(4) 0.45620(13) 0.0280(10) Uani 1 1 d . . . C42 C 0.5027(3) -0.0922(7) 0.32913(19) 0.0680(19) Uani 1 1 d . . . H42A H 0.5377 -0.0893 0.3152 0.082 Uiso 1 1 calc R . . C43 C 0.1385(3) 0.2858(6) 0.47906(17) 0.0471(15) Uani 1 1 d . . . H44A H 0.1134 0.3582 0.4882 0.056 Uiso 1 1 calc R . . C51 C 0.2297(2) -0.1842(5) 0.49126(14) 0.0410(13) Uani 1 1 d . . . H51A H 0.2001 -0.1112 0.4958 0.062 Uiso 1 1 calc R . . H51B H 0.2565 -0.1876 0.5124 0.062 Uiso 1 1 calc R . . H51C H 0.2110 -0.2774 0.4883 0.062 Uiso 1 1 calc R . . C53 C 0.1159(2) 0.1700(6) 0.46138(15) 0.0421(13) Uani 1 1 d . . . H54A H 0.0751 0.1635 0.4583 0.051 Uiso 1 1 calc R . . C62 C 0.4063(2) -0.1835(5) 0.33707(14) 0.0358(11) Uani 1 1 d . . . C63 C 0.1505(2) 0.0618(5) 0.44786(13) 0.0328(11) Uani 1 1 d . . . C72 C 0.4442(2) 0.0612(6) 0.41963(16) 0.0472(14) Uani 1 1 d . . . H72A H 0.4028 0.0615 0.4276 0.057 Uiso 1 1 calc R . . C73 C 0.3001(2) 0.2044(6) 0.47603(16) 0.0407(13) Uani 1 1 d . . . H74A H 0.3193 0.1493 0.4557 0.049 Uiso 1 1 calc R . . C82 C 0.4802(3) -0.0082(7) 0.4508(2) 0.078(2) Uani 1 1 d . . . H82A H 0.4765 0.0484 0.4736 0.117 Uiso 1 1 calc R . . H82B H 0.5210 -0.0121 0.4433 0.117 Uiso 1 1 calc R . . H82C H 0.4660 -0.1052 0.4554 0.117 Uiso 1 1 calc R . . C83 C 0.3174(3) 0.1366(7) 0.51320(18) 0.0625(17) Uani 1 1 d . . . H83A H 0.3029 0.0384 0.5142 0.094 Uiso 1 1 calc R . . H83B H 0.3006 0.1918 0.5337 0.094 Uiso 1 1 calc R . . H83C H 0.3596 0.1361 0.5155 0.094 Uiso 1 1 calc R . . C92 C 0.4631(3) 0.2161(6) 0.4142(2) 0.0646(19) Uani 1 1 d . . . H92A H 0.4401 0.2596 0.3943 0.097 Uiso 1 1 calc R . . H92B H 0.5042 0.2190 0.4075 0.097 Uiso 1 1 calc R . . H92C H 0.4571 0.2691 0.4374 0.097 Uiso 1 1 calc R . . C93 C 0.3229(2) 0.3573(6) 0.47470(18) 0.0561(16) Uani 1 1 d . . . H93A H 0.3119 0.4014 0.4510 0.084 Uiso 1 1 calc R . . H93B H 0.3652 0.3565 0.4770 0.084 Uiso 1 1 calc R . . H93C H 0.3063 0.4122 0.4953 0.084 Uiso 1 1 calc R . . C102 C 0.3569(3) -0.2722(5) 0.32281(19) 0.0388(13) Uani 1 1 d . . . H10A H 0.3257 -0.2723 0.3421 0.047 Uiso 1 1 calc R . . C103 C 0.12181(19) -0.0657(5) 0.42935(15) 0.0413(13) Uani 1 1 d . . . H10B H 0.1529 -0.1344 0.4221 0.050 Uiso 1 1 calc R . . C112 C 0.3314(3) -0.2113(7) 0.28677(18) 0.0649(17) Uani 1 1 d . . . H11D H 0.3198 -0.1120 0.2908 0.097 Uiso 1 1 calc R . . H11E H 0.2975 -0.2676 0.2795 0.097 Uiso 1 1 calc R . . H11F H 0.3606 -0.2155 0.2670 0.097 Uiso 1 1 calc R . . C113 C 0.0887(2) -0.0238(7) 0.39413(18) 0.0609(17) Uani 1 1 d . . . H11G H 0.1149 0.0248 0.3769 0.091 Uiso 1 1 calc R . . H11H H 0.0568 0.0403 0.4007 0.091 Uiso 1 1 calc R . . H11I H 0.0731 -0.1097 0.3823 0.091 Uiso 1 1 calc R . . C122 C 0.3745(3) -0.4274(6) 0.31544(18) 0.0597(16) Uani 1 1 d . . . H12A H 0.3909 -0.4687 0.3381 0.090 Uiso 1 1 calc R . . H12B H 0.4034 -0.4304 0.2955 0.090 Uiso 1 1 calc R . . H12C H 0.3403 -0.4824 0.3080 0.090 Uiso 1 1 calc R . . C123 C 0.0809(3) -0.1421(7) 0.4562(2) 0.076(2) Uani 1 1 d . . . H12D H 0.0629 -0.2234 0.4436 0.114 Uiso 1 1 calc R . . H12E H 0.0507 -0.0757 0.4645 0.114 Uiso 1 1 calc R . . H12F H 0.1028 -0.1762 0.4778 0.114 Uiso 1 1 calc R . . Fe2 Fe 0.03961(2) 0.03237(6) 0.147239(18) 0.02852(15) Uani 1 1 d . . . Cl12 Cl -0.02718(6) 0.01627(14) 0.19592(4) 0.0476(3) Uani 1 1 d . . . Cl22 Cl 0.07436(7) 0.25848(13) 0.16255(5) 0.0506(5) Uani 1 1 d . . . O12 O -0.05729(15) 0.4006(4) 0.18973(10) 0.0498(9) Uani 1 1 d . . . O22 O 0.01706(17) 0.2840(5) 0.25648(12) 0.0543(11) Uani 1 1 d . . . N12 N 0.00308(15) -0.0189(4) 0.09797(10) 0.0289(9) Uani 1 1 d . . . N22 N 0.10376(14) -0.1103(4) 0.14158(11) 0.0285(9) Uani 1 1 d . . . Li12 Li -0.0033(5) 0.2571(10) 0.2051(4) 0.058(3) Uani 1 1 d . . . C9S C -0.0759(3) 0.4010(6) 0.15130(17) 0.0576(15) Uani 1 1 d . . . H9SA H -0.1160 0.3646 0.1492 0.069 Uiso 1 1 calc R . . H9SB H -0.0502 0.3400 0.1360 0.069 Uiso 1 1 calc R . . C10S C -0.0728(4) 0.5514(8) 0.1385(2) 0.089(2) Uani 1 1 d . . . H10C H -0.0404 0.5647 0.1208 0.107 Uiso 1 1 calc R . . H10D H -0.1094 0.5801 0.1262 0.107 Uiso 1 1 calc R . . C11S C -0.0637(7) 0.6310(8) 0.1711(3) 0.204(7) Uani 1 1 d . . . H11J H -0.0981 0.6912 0.1758 0.244 Uiso 1 1 calc R . . H11Q H -0.0302 0.6951 0.1673 0.244 Uiso 1 1 calc R . . C12S C -0.0533(4) 0.5437(7) 0.2026(2) 0.093(3) Uani 1 1 d . . . H12G H -0.0144 0.5628 0.2130 0.111 Uiso 1 1 calc R . . H12N H -0.0826 0.5621 0.2222 0.111 Uiso 1 1 calc R . . C13S C 0.0751(3) 0.2589(8) 0.2689(3) 0.091(3) Uani 1 1 d . . . H13A H 0.0970 0.3496 0.2695 0.109 Uiso 1 1 calc R . . H13B H 0.0950 0.1925 0.2517 0.109 Uiso 1 1 calc R . . C14S C 0.0716(3) 0.1949(9) 0.3074(2) 0.085(2) Uani 1 1 d . . . H14A H 0.1016 0.1208 0.3109 0.102 Uiso 1 1 calc R . . H14B H 0.0764 0.2692 0.3267 0.102 Uiso 1 1 calc R . . C14 C -0.0164(2) -0.1737(6) 0.04358(15) 0.0468(14) Uani 1 1 d . . . H14C H -0.0456 -0.1005 0.0384 0.070 Uiso 1 1 calc R . . H14D H -0.0355 -0.2665 0.0464 0.070 Uiso 1 1 calc R . . H14E H 0.0112 -0.1783 0.0229 0.070 Uiso 1 1 calc R . . C15S C 0.0130(3) 0.1320(9) 0.3089(2) 0.084(2) Uani 1 1 d . . . H15A H -0.0021 0.1310 0.3347 0.101 Uiso 1 1 calc R . . H15B H 0.0128 0.0335 0.2990 0.101 Uiso 1 1 calc R . . C15 C -0.03594(19) 0.0856(5) 0.08254(12) 0.0296(10) Uani 1 1 d . . . C16S C -0.0218(3) 0.2315(8) 0.2845(2) 0.068(2) Uani 1 1 d . . . H16A H -0.0545 0.1798 0.2728 0.082 Uiso 1 1 calc R . . H16B H -0.0376 0.3115 0.2993 0.082 Uiso 1 1 calc R . . C16 C 0.15457(18) -0.0922(5) 0.16383(13) 0.0300(11) Uani 1 1 d . . . C24 C 0.01564(19) -0.1362(5) 0.07948(14) 0.0315(11) Uani 1 1 d . . . C25 C -0.0120(2) 0.2039(5) 0.06482(14) 0.0362(12) Uani 1 1 d . . . C26 C 0.2008(2) -0.0140(5) 0.14906(17) 0.0444(13) Uani 1 1 d . . . C34 C 0.0600(3) -0.2332(5) 0.09094(18) 0.0355(14) Uani 1 1 d . . . H34B H 0.0605 -0.3214 0.0779 0.043 Uiso 1 1 calc R . . C35 C -0.0484(2) 0.3098(6) 0.05165(15) 0.0451(13) Uani 1 1 d . . . H35A H -0.0321 0.3906 0.0396 0.054 Uiso 1 1 calc R . . C36 C 0.2514(2) -0.0035(7) 0.17019(19) 0.0649(19) Uani 1 1 d . . . H36A H 0.2838 0.0464 0.1604 0.078 Uiso 1 1 calc R . . C44 C 0.1019(2) -0.2188(5) 0.11784(15) 0.0299(12) Uani 1 1 d . . . C45 C -0.1079(3) 0.3008(6) 0.05555(17) 0.0490(15) Uani 1 1 d . . . H45A H -0.1322 0.3749 0.0466 0.059 Uiso 1 1 calc R . . C46 C 0.2549(3) -0.0643(7) 0.2050(2) 0.073(2) Uani 1 1 d . . . H46A H 0.2899 -0.0582 0.2188 0.087 Uiso 1 1 calc R . . C54 C 0.1475(2) -0.3360(5) 0.11871(16) 0.0456(14) Uani 1 1 d . . . H54B H 0.1756 -0.3159 0.1384 0.068 Uiso 1 1 calc R . . H54C H 0.1674 -0.3398 0.0947 0.068 Uiso 1 1 calc R . . H54D H 0.1287 -0.4280 0.1236 0.068 Uiso 1 1 calc R . . C55 C -0.1312(2) 0.1821(6) 0.07271(15) 0.0450(14) Uani 1 1 d . . . H55A H -0.1721 0.1747 0.0748 0.054 Uiso 1 1 calc R . . C56 C 0.2085(2) -0.1330(6) 0.21955(17) 0.0603(17) Uani 1 1 d . . . H56A H 0.2109 -0.1693 0.2442 0.072 Uiso 1 1 calc R . . C65 C -0.0966(2) 0.0718(5) 0.08715(14) 0.0363(12) Uani 1 1 d . . . C66 C 0.1573(2) -0.1521(5) 0.19956(15) 0.0409(13) Uani 1 1 d . . . C75 C 0.0532(2) 0.2191(6) 0.05881(17) 0.0380(13) Uani 1 1 d . . . H75A H 0.0722 0.1668 0.0797 0.046 Uiso 1 1 calc R . . C76 C 0.1984(2) 0.0570(6) 0.11111(16) 0.0453(13) Uani 1 1 d . . . H76A H 0.1578 0.0489 0.1018 0.054 Uiso 1 1 calc R . . C85 C 0.0725(3) 0.1463(7) 0.02350(18) 0.0635(18) Uani 1 1 d . . . H85A H 0.1143 0.1582 0.0205 0.095 Uiso 1 1 calc R . . H85B H 0.0524 0.1890 0.0022 0.095 Uiso 1 1 calc R . . H85C H 0.0631 0.0445 0.0249 0.095 Uiso 1 1 calc R . . C86 C 0.2374(3) -0.0152(7) 0.0831(2) 0.075(2) Uani 1 1 d . . . H86A H 0.2345 0.0341 0.0591 0.113 Uiso 1 1 calc R . . H86B H 0.2255 -0.1149 0.0801 0.113 Uiso 1 1 calc R . . H86C H 0.2775 -0.0117 0.0919 0.113 Uiso 1 1 calc R . . C95 C 0.0749(3) 0.3723(6) 0.06086(19) 0.0592(16) Uani 1 1 d . . . H95A H 0.1169 0.3739 0.0567 0.089 Uiso 1 1 calc R . . H95B H 0.0662 0.4119 0.0855 0.089 Uiso 1 1 calc R . . H95C H 0.0557 0.4296 0.0417 0.089 Uiso 1 1 calc R . . C96 C 0.2134(3) 0.2152(6) 0.11300(19) 0.0573(17) Uani 1 1 d . . . H96A H 0.2113 0.2566 0.0880 0.086 Uiso 1 1 calc R . . H96B H 0.2527 0.2267 0.1228 0.086 Uiso 1 1 calc R . . H96C H 0.1859 0.2640 0.1294 0.086 Uiso 1 1 calc R . . C105 C -0.1242(2) -0.0555(6) 0.10521(16) 0.0452(13) Uani 1 1 d . . . H10E H -0.0928 -0.1228 0.1127 0.054 Uiso 1 1 calc R . . C106 C 0.1066(3) -0.2314(6) 0.2177(2) 0.0570(19) Uani 1 1 d . . . H10F H 0.0735 -0.2297 0.1998 0.068 Uiso 1 1 calc R . . C115 C -0.1582(2) -0.0128(6) 0.14060(18) 0.0610(17) Uani 1 1 d . . . H11K H -0.1324 0.0383 0.1577 0.091 Uiso 1 1 calc R . . H11L H -0.1730 -0.0988 0.1528 0.091 Uiso 1 1 calc R . . H11M H -0.1906 0.0492 0.1337 0.091 Uiso 1 1 calc R . . C116 C 0.0868(4) -0.1596(9) 0.2529(2) 0.103(3) Uani 1 1 d . . . H11N H 0.0772 -0.0598 0.2477 0.154 Uiso 1 1 calc R . . H11O H 0.1179 -0.1634 0.2715 0.154 Uiso 1 1 calc R . . H11P H 0.0525 -0.2087 0.2626 0.154 Uiso 1 1 calc R . . C125 C -0.1652(3) -0.1351(8) 0.0788(2) 0.078(2) Uani 1 1 d . . . H12H H -0.1442 -0.1629 0.0563 0.117 Uiso 1 1 calc R . . H12I H -0.1976 -0.0727 0.0721 0.117 Uiso 1 1 calc R . . H12J H -0.1801 -0.2206 0.0913 0.117 Uiso 1 1 calc R . . C126 C 0.1224(3) -0.3880(7) 0.2246(2) 0.087(2) Uani 1 1 d . . . H12K H 0.0895 -0.4370 0.2362 0.131 Uiso 1 1 calc R . . H12L H 0.1560 -0.3930 0.2412 0.131 Uiso 1 1 calc R . . H12M H 0.1318 -0.4340 0.2009 0.131 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 0.0287(3) 0.0255(3) 0.0285(4) 0.0078(3) 0.0015(3) 0.0023(3) Cl11 0.0478(9) 0.0382(8) 0.0520(11) 0.0187(6) -0.0104(7) -0.0104(5) Cl21 0.0475(8) 0.0417(7) 0.0430(8) 0.0071(6) -0.0147(6) -0.0025(6) O11 0.040(2) 0.073(3) 0.049(3) 0.020(2) 0.011(2) 0.010(2) O21 0.050(2) 0.0360(19) 0.044(2) 0.0110(16) 0.0051(17) 0.0049(16) N11 0.0218(18) 0.0252(19) 0.028(2) -0.0025(16) 0.0019(16) 0.0008(15) N21 0.0252(19) 0.029(2) 0.029(2) 0.0022(17) 0.0012(16) 0.0008(16) Li11 0.051(6) 0.046(5) 0.024(6) 0.012(3) -0.002(5) 0.006(4) C1S 0.050(4) 0.108(6) 0.062(5) 0.031(4) -0.004(3) 0.026(4) C2S 0.066(4) 0.137(7) 0.050(4) 0.033(4) 0.014(3) 0.011(4) C3S 0.050(4) 0.119(6) 0.061(5) 0.008(4) 0.023(3) 0.006(4) C4S 0.043(4) 0.060(4) 0.046(4) -0.001(3) -0.006(3) 0.011(3) C5S 0.130(6) 0.045(4) 0.065(5) 0.023(3) 0.028(5) 0.009(4) C6S 0.346(16) 0.062(5) 0.086(7) -0.026(5) 0.078(9) -0.080(8) C7S 0.116(6) 0.065(4) 0.059(5) -0.004(3) 0.012(4) -0.013(4) C8S 0.048(3) 0.047(3) 0.050(4) 0.010(3) 0.008(3) 0.000(2) C11 0.042(3) 0.039(3) 0.041(3) 0.007(2) 0.002(2) 0.009(2) C12 0.024(2) 0.023(2) 0.043(3) 0.002(2) 0.002(2) 0.0036(18) C13 0.036(3) 0.028(2) 0.022(3) 0.0087(19) 0.003(2) 0.004(2) C21 0.032(3) 0.015(2) 0.033(3) -0.001(2) -0.009(2) 0.0080(19) C22 0.030(2) 0.042(3) 0.048(3) -0.004(3) 0.002(3) 0.001(2) C23 0.030(3) 0.036(3) 0.028(3) 0.004(2) 0.007(2) 0.007(2) C31 0.029(3) 0.026(3) 0.029(3) 0.0096(19) 0.009(3) 0.0001(19) C32 0.036(3) 0.065(4) 0.077(5) -0.013(3) 0.016(3) -0.018(3) C52 0.046(3) 0.052(3) 0.054(4) -0.013(3) 0.017(3) -0.007(3) C33 0.072(4) 0.032(3) 0.034(3) -0.001(2) 0.007(3) 0.008(3) C41 0.034(3) 0.027(2) 0.023(3) 0.004(2) -0.001(2) -0.005(2) C42 0.056(4) 0.075(4) 0.073(5) -0.010(4) 0.038(3) -0.007(3) C43 0.052(4) 0.054(4) 0.036(4) -0.001(3) 0.005(3) 0.029(3) C51 0.052(3) 0.039(3) 0.032(3) 0.009(2) 0.010(2) 0.002(2) C53 0.033(3) 0.054(3) 0.040(3) 0.009(3) 0.006(2) 0.008(3) C62 0.037(3) 0.033(3) 0.038(3) 0.004(2) 0.010(2) 0.004(2) C63 0.034(3) 0.033(3) 0.031(3) 0.010(2) 0.008(2) 0.009(2) C72 0.032(3) 0.053(3) 0.056(4) -0.006(3) 0.000(3) -0.007(2) C73 0.050(3) 0.036(3) 0.037(4) -0.012(3) 0.000(3) -0.003(3) C82 0.110(6) 0.066(4) 0.058(5) 0.003(3) -0.011(4) 0.003(4) C83 0.060(4) 0.068(4) 0.059(4) 0.008(3) -0.022(3) -0.004(3) C92 0.062(4) 0.048(3) 0.084(5) -0.019(3) -0.011(3) -0.013(3) C93 0.051(3) 0.056(4) 0.062(4) -0.004(3) 0.000(3) -0.009(3) C102 0.040(3) 0.043(3) 0.033(3) -0.002(2) 0.003(3) 0.001(2) C103 0.026(3) 0.046(3) 0.053(4) 0.005(3) 0.000(2) -0.001(2) C112 0.066(4) 0.080(4) 0.049(4) 0.004(3) -0.013(3) 0.010(3) C113 0.049(3) 0.075(4) 0.059(4) -0.003(3) -0.004(3) 0.007(3) C122 0.072(4) 0.044(3) 0.063(4) -0.004(3) 0.002(3) 0.002(3) C123 0.060(4) 0.088(5) 0.080(5) 0.023(4) 0.000(4) -0.018(4) Fe2 0.0284(3) 0.0280(3) 0.0291(4) -0.0053(3) -0.0003(3) 0.0030(3) Cl12 0.0494(8) 0.0428(7) 0.0506(9) -0.0036(7) 0.0162(7) -0.0031(6) Cl22 0.0525(9) 0.0368(8) 0.0626(12) -0.0175(6) 0.0170(8) -0.0125(5) O12 0.061(2) 0.045(2) 0.044(2) -0.0067(18) 0.0013(19) 0.0077(18) O22 0.038(2) 0.079(3) 0.046(3) 0.000(2) -0.005(2) 0.001(2) N12 0.0266(19) 0.029(2) 0.031(2) -0.0038(17) -0.0011(17) 0.0009(17) N22 0.0281(19) 0.0283(19) 0.029(2) -0.0025(18) -0.0013(17) 0.0037(16) Li12 0.059(7) 0.052(6) 0.063(9) 0.003(5) 0.001(6) 0.019(4) C9S 0.064(4) 0.055(3) 0.055(4) 0.005(3) -0.003(3) 0.012(3) C10S 0.113(6) 0.075(5) 0.080(6) 0.022(4) -0.001(5) -0.012(4) C11S 0.43(2) 0.035(4) 0.145(10) 0.013(5) -0.119(12) -0.040(8) C12S 0.123(6) 0.055(4) 0.100(7) -0.039(4) -0.032(5) 0.027(4) C13S 0.035(4) 0.097(6) 0.141(9) 0.037(5) -0.033(5) -0.020(3) C14S 0.092(6) 0.087(5) 0.075(6) -0.007(4) -0.029(4) 0.004(4) C14 0.046(3) 0.049(3) 0.045(4) -0.014(3) -0.010(3) 0.003(3) C15S 0.089(5) 0.110(6) 0.053(5) 0.015(4) 0.003(4) -0.006(5) C15 0.032(3) 0.032(3) 0.025(3) -0.005(2) -0.007(2) 0.007(2) C16S 0.038(3) 0.112(6) 0.055(4) -0.039(4) -0.004(3) -0.008(3) C16 0.030(2) 0.026(2) 0.033(3) -0.003(2) -0.005(2) 0.0055(19) C24 0.031(2) 0.029(3) 0.034(3) -0.005(2) -0.006(2) -0.001(2) C25 0.050(3) 0.033(3) 0.025(3) -0.004(2) -0.001(2) 0.008(3) C26 0.036(2) 0.047(3) 0.051(4) -0.008(3) -0.010(3) -0.004(2) C34 0.044(3) 0.025(3) 0.038(4) -0.012(2) 0.002(3) -0.005(2) C35 0.051(4) 0.050(3) 0.035(3) 0.003(3) -0.005(3) 0.005(3) C36 0.046(3) 0.079(4) 0.071(5) 0.016(4) -0.015(3) -0.016(3) C44 0.029(3) 0.025(2) 0.036(4) -0.001(2) -0.008(2) -0.004(2) C45 0.056(4) 0.047(3) 0.044(4) 0.003(3) -0.007(3) 0.018(3) C46 0.050(4) 0.091(5) 0.078(5) 0.014(4) -0.029(4) -0.022(3) C54 0.044(3) 0.040(3) 0.052(4) -0.010(3) -0.008(3) 0.013(2) C55 0.033(3) 0.070(4) 0.031(3) -0.010(3) -0.006(2) 0.018(3) C56 0.063(4) 0.073(4) 0.044(4) 0.013(3) -0.023(3) 0.003(3) C65 0.037(3) 0.042(3) 0.029(3) -0.014(2) -0.003(2) 0.001(2) C66 0.041(3) 0.035(3) 0.047(3) 0.000(2) -0.001(3) 0.005(2) C75 0.032(3) 0.040(3) 0.042(4) 0.004(3) 0.003(3) 0.004(2) C76 0.031(3) 0.057(3) 0.048(4) 0.010(3) 0.001(3) -0.012(2) C85 0.060(4) 0.069(4) 0.062(5) -0.008(3) 0.024(3) -0.008(3) C86 0.096(5) 0.074(4) 0.057(5) -0.009(3) 0.012(4) -0.007(4) C95 0.069(4) 0.044(3) 0.065(4) 0.010(3) -0.003(3) -0.013(3) C96 0.058(4) 0.059(4) 0.055(4) -0.002(3) 0.015(3) -0.003(3) C105 0.036(3) 0.052(3) 0.048(4) -0.006(3) -0.002(3) 0.003(2) C106 0.048(3) 0.066(4) 0.057(5) 0.030(3) -0.012(4) 0.008(3) C115 0.048(3) 0.073(4) 0.061(4) 0.004(3) 0.015(3) 0.000(3) C116 0.113(6) 0.112(7) 0.083(6) 0.025(5) 0.043(5) 0.025(5) C125 0.048(4) 0.085(5) 0.101(6) -0.020(4) 0.004(4) -0.025(3) C126 0.100(5) 0.060(4) 0.102(6) 0.027(4) 0.006(4) -0.002(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 N11 2.006(3) . ? Fe1 N21 2.021(4) . ? Fe1 Cl11 2.3240(13) . ? Fe1 Cl21 2.3378(14) . ? Fe1 Li11 3.150(9) . ? Cl11 Li11 2.357(11) . ? Cl21 Li11 2.363(8) . ? O11 C4S 1.417(7) . ? O11 C1S 1.431(7) . ? O11 Li11 1.890(11) . ? O21 C5S 1.425(6) . ? O21 C8S 1.433(6) . ? O21 Li11 1.957(10) . ? N11 C21 1.339(6) . ? N11 C12 1.448(5) . ? N21 C41 1.328(5) . ? N21 C13 1.440(5) . ? C1S C2S 1.457(9) . ? C2S C3S 1.520(9) . ? C3S C4S 1.489(9) . ? C5S C6S 1.433(10) . ? C6S C7S 1.416(10) . ? C7S C8S 1.492(8) . ? C11 C21 1.517(6) . ? C12 C62 1.408(7) . ? C12 C22 1.415(6) . ? C13 C63 1.401(6) . ? C13 C23 1.430(7) . ? C21 C31 1.412(8) . ? C22 C32 1.391(7) . ? C22 C72 1.528(8) . ? C23 C33 1.395(7) . ? C23 C73 1.521(7) . ? C31 C41 1.380(7) . ? C32 C42 1.374(8) . ? C52 C42 1.382(8) . ? C52 C62 1.384(7) . ? C33 C43 1.375(8) . ? C41 C51 1.513(6) . ? C43 C53 1.363(8) . ? C53 C63 1.381(7) . ? C62 C102 1.501(7) . ? C63 C103 1.520(7) . ? C72 C92 1.529(8) . ? C72 C82 1.540(9) . ? C73 C93 1.528(7) . ? C73 C83 1.533(8) . ? C102 C112 1.534(9) . ? C102 C122 1.533(7) . ? C103 C113 1.531(8) . ? C103 C123 1.531(8) . ? Fe2 N22 2.006(3) . ? Fe2 N12 2.020(4) . ? Fe2 Cl22 2.3325(14) . ? Fe2 Cl12 2.3383(15) . ? Fe2 Li12 3.123(12) . ? Cl12 Li12 2.348(10) . ? Cl22 Li12 2.358(13) . ? O12 C12S 1.423(7) . ? O12 C9S 1.447(7) . ? O12 Li12 1.917(11) . ? O22 C13S 1.431(7) . ? O22 C16S 1.435(8) . ? O22 Li12 1.921(15) . ? N12 C24 1.317(6) . ? N12 C15 1.443(5) . ? N22 C44 1.329(6) . ? N22 C16 1.431(5) . ? C9S C10S 1.484(8) . ? C10S C11S 1.403(12) . ? C11S C12S 1.419(12) . ? C13S C14S 1.512(12) . ? C14S C15S 1.476(10) . ? C14 C24 1.529(7) . ? C15S C16S 1.514(9) . ? C15 C25 1.393(7) . ? C15 C65 1.416(7) . ? C16 C26 1.401(7) . ? C16 C66 1.404(7) . ? C24 C34 1.430(7) . ? C25 C35 1.383(7) . ? C25 C75 1.529(7) . ? C26 C36 1.397(7) . ? C26 C76 1.519(8) . ? C34 C44 1.376(8) . ? C35 C45 1.383(8) . ? C36 C46 1.377(9) . ? C44 C54 1.521(7) . ? C45 C55 1.382(8) . ? C46 C56 1.357(8) . ? C55 C65 1.408(7) . ? C56 C66 1.395(7) . ? C65 C105 1.501(7) . ? C66 C106 1.532(8) . ? C75 C85 1.509(8) . ? C75 C95 1.523(7) . ? C76 C86 1.512(8) . ? C76 C96 1.525(7) . ? C105 C125 1.534(8) . ? C105 C115 1.547(8) . ? C106 C116 1.505(11) . ? C106 C126 1.533(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 N11 Fe1 N21 93.21(14) . . ? N11 Fe1 Cl11 114.00(10) . . ? N21 Fe1 Cl11 121.84(12) . . ? N11 Fe1 Cl21 122.34(11) . . ? N21 Fe1 Cl21 111.86(11) . . ? Cl11 Fe1 Cl21 95.81(6) . . ? N11 Fe1 Li11 140.9(2) . . ? N21 Fe1 Li11 125.9(2) . . ? Cl11 Fe1 Li11 48.17(19) . . ? Cl21 Fe1 Li11 48.28(18) . . ? Fe1 Cl11 Li11 84.6(2) . . ? Fe1 Cl21 Li11 84.1(3) . . ? C4S O11 C1S 105.7(5) . . ? C4S O11 Li11 120.9(5) . . ? C1S O11 Li11 128.4(5) . . ? C5S O21 C8S 108.4(4) . . ? C5S O21 Li11 118.7(5) . . ? C8S O21 Li11 118.2(4) . . ? C21 N11 C12 118.6(4) . . ? C21 N11 Fe1 123.0(3) . . ? C12 N11 Fe1 118.3(3) . . ? C41 N21 C13 120.3(4) . . ? C41 N21 Fe1 123.3(3) . . ? C13 N21 Fe1 116.3(3) . . ? O11 Li11 O21 107.6(4) . . ? O11 Li11 Cl21 112.7(5) . . ? O21 Li11 Cl21 121.1(5) . . ? O11 Li11 Cl11 114.4(5) . . ? O21 Li11 Cl11 106.2(5) . . ? Cl21 Li11 Cl11 94.2(3) . . ? O11 Li11 Fe1 132.1(4) . . ? O21 Li11 Fe1 119.7(5) . . ? Cl21 Li11 Fe1 47.59(16) . . ? Cl11 Li11 Fe1 47.27(16) . . ? O11 C1S C2S 106.0(5) . . ? C1S C2S C3S 105.3(5) . . ? C4S C3S C2S 104.1(5) . . ? O11 C4S C3S 106.6(5) . . ? O21 C5S C6S 107.6(6) . . ? C7S C6S C5S 109.7(6) . . ? C6S C7S C8S 105.9(6) . . ? O21 C8S C7S 107.2(4) . . ? C62 C12 C22 120.1(4) . . ? C62 C12 N11 121.2(4) . . ? C22 C12 N11 118.7(4) . . ? C63 C13 C23 120.0(4) . . ? C63 C13 N21 122.2(4) . . ? C23 C13 N21 117.7(4) . . ? N11 C21 C31 123.4(4) . . ? N11 C21 C11 119.4(5) . . ? C31 C21 C11 117.1(4) . . ? C32 C22 C12 118.5(5) . . ? C32 C22 C72 120.4(5) . . ? C12 C22 C72 121.1(4) . . ? C33 C23 C13 118.1(5) . . ? C33 C23 C73 121.9(5) . . ? C13 C23 C73 119.9(4) . . ? C41 C31 C21 129.4(4) . . ? C42 C32 C22 121.0(5) . . ? C42 C52 C62 120.7(5) . . ? C43 C33 C23 120.8(5) . . ? N21 C41 C31 124.2(4) . . ? N21 C41 C51 120.5(4) . . ? C31 C41 C51 115.3(4) . . ? C32 C42 C52 120.4(5) . . ? C53 C43 C33 120.5(5) . . ? C43 C53 C63 121.8(5) . . ? C52 C62 C12 119.2(5) . . ? C52 C62 C102 119.7(5) . . ? C12 C62 C102 121.1(4) . . ? C53 C63 C13 118.7(5) . . ? C53 C63 C103 118.6(4) . . ? C13 C63 C103 122.7(4) . . ? C92 C72 C22 111.3(5) . . ? C92 C72 C82 109.9(5) . . ? C22 C72 C82 111.7(5) . . ? C23 C73 C93 113.1(5) . . ? C23 C73 C83 110.5(5) . . ? C93 C73 C83 109.1(5) . . ? C62 C102 C112 112.0(5) . . ? C62 C102 C122 112.6(5) . . ? C112 C102 C122 108.0(5) . . ? C113 C103 C63 112.3(4) . . ? C113 C103 C123 109.5(4) . . ? C63 C103 C123 111.2(5) . . ? N22 Fe2 N12 93.50(15) . . ? N22 Fe2 Cl22 112.05(11) . . ? N12 Fe2 Cl22 124.55(12) . . ? N22 Fe2 Cl12 121.35(12) . . ? N12 Fe2 Cl12 111.42(11) . . ? Cl22 Fe2 Cl12 96.27(6) . . ? N22 Fe2 Li12 138.7(3) . . ? N12 Fe2 Li12 127.8(2) . . ? Cl22 Fe2 Li12 48.6(2) . . ? Cl12 Fe2 Li12 48.3(2) . . ? Fe2 Cl12 Li12 83.6(3) . . ? Fe2 Cl22 Li12 83.5(3) . . ? C12S O12 C9S 109.1(5) . . ? C12S O12 Li12 121.7(5) . . ? C9S O12 Li12 118.1(5) . . ? C13S O22 C16S 108.1(6) . . ? C13S O22 Li12 120.4(6) . . ? C16S O22 Li12 118.4(5) . . ? C24 N12 C15 120.7(4) . . ? C24 N12 Fe2 123.3(3) . . ? C15 N12 Fe2 115.9(3) . . ? C44 N22 C16 118.4(4) . . ? C44 N22 Fe2 123.5(3) . . ? C16 N22 Fe2 118.1(3) . . ? O12 Li12 O22 110.2(6) . . ? O12 Li12 Cl12 118.7(6) . . ? O22 Li12 Cl12 108.6(5) . . ? O12 Li12 Cl22 107.7(6) . . ? O22 Li12 Cl22 115.9(6) . . ? Cl12 Li12 Cl22 95.3(4) . . ? O12 Li12 Fe2 119.2(6) . . ? O22 Li12 Fe2 130.6(5) . . ? Cl12 Li12 Fe2 48.1(2) . . ? Cl22 Li12 Fe2 47.9(2) . . ? O12 C9S C10S 106.5(5) . . ? C11S C10S C9S 104.7(6) . . ? C10S C11S C12S 112.7(6) . . ? O12 C12S C11S 105.8(6) . . ? O22 C13S C14S 107.5(7) . . ? C15S C14S C13S 104.0(6) . . ? C14S C15S C16S 102.6(6) . . ? C25 C15 C65 121.2(4) . . ? C25 C15 N12 118.0(4) . . ? C65 C15 N12 120.7(4) . . ? O22 C16S C15S 106.6(5) . . ? C26 C16 C66 121.5(4) . . ? C26 C16 N22 118.4(4) . . ? C66 C16 N22 120.1(4) . . ? N12 C24 C34 122.9(4) . . ? N12 C24 C14 120.8(4) . . ? C34 C24 C14 116.3(4) . . ? C35 C25 C15 119.1(5) . . ? C35 C25 C75 118.9(5) . . ? C15 C25 C75 122.0(4) . . ? C16 C26 C36 118.0(5) . . ? C16 C26 C76 122.8(4) . . ? C36 C26 C76 119.2(5) . . ? C44 C34 C24 130.2(5) . . ? C45 C35 C25 121.6(5) . . ? C46 C36 C26 120.9(6) . . ? N22 C44 C34 123.3(4) . . ? N22 C44 C54 121.2(4) . . ? C34 C44 C54 115.5(4) . . ? C55 C45 C35 118.8(5) . . ? C56 C46 C36 120.1(5) . . ? C45 C55 C65 122.3(5) . . ? C46 C56 C66 122.2(6) . . ? C55 C65 C15 116.9(5) . . ? C55 C65 C105 120.1(4) . . ? C15 C65 C105 123.0(4) . . ? C56 C66 C16 117.2(5) . . ? C56 C66 C106 119.3(5) . . ? C16 C66 C106 123.4(5) . . ? C85 C75 C95 111.7(5) . . ? C85 C75 C25 111.6(5) . . ? C95 C75 C25 114.0(5) . . ? C86 C76 C96 109.3(5) . . ? C86 C76 C26 112.4(5) . . ? C96 C76 C26 112.2(5) . . ? C65 C105 C125 112.5(5) . . ? C65 C105 C115 111.5(4) . . ? C125 C105 C115 108.7(4) . . ? C116 C106 C66 111.9(6) . . ? C116 C106 C126 111.4(6) . . ? C66 C106 C126 110.6(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.312 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.046 data_rene _database_code_CSD 167177 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H57 Cl2 Fe Li N2 O2' _chemical_formula_weight 695.54 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' 'Li' 'Li' -0.0003 0.0001 '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 ? _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 16.7761(8) _cell_length_b 19.0238(9) _cell_length_c 36.8905(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11773.4(10) _cell_formula_units_Z 12 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 8196 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.177 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4464 _exptl_absorpt_coefficient_mu 0.552 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.893 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 53706 _diffrn_reflns_av_R_equivalents 0.0520 _diffrn_reflns_av_sigmaI/netI 0.0713 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 23.28 _reflns_number_total 16937 _reflns_number_gt 11681 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP32 _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^)+(0.0424P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.461(13) _refine_ls_number_reflns 16937 _refine_ls_number_parameters 1217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0910 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 0.942 _refine_ls_restrained_S_all 0.942 _refine_ls_shift/su_max 0.136 _refine_ls_shift/su_mean 0.005 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 0.47377(4) 0.86424(3) 0.193169(15) 0.03675(16) Uani 1 1 d . . . Cl11 Cl 0.47643(8) 0.75343(6) 0.21934(3) 0.0578(3) Uani 1 1 d . . . Cl21 Cl 0.61154(6) 0.88048(7) 0.19107(4) 0.0633(4) Uani 1 1 d . . . O1 O 0.6754(2) 0.7649(2) 0.25865(10) 0.0884(12) Uani 1 1 d . . . O2 O 0.6596(2) 0.70338(19) 0.17920(10) 0.0768(11) Uani 1 1 d . . . N11 N 0.41368(19) 0.94017(17) 0.21879(9) 0.0336(8) Uani 1 1 d . . . N21 N 0.40804(18) 0.87299(17) 0.14806(8) 0.0334(8) Uani 1 1 d . . . Li1 Li 0.6159(5) 0.7643(5) 0.2140(2) 0.065(2) Uani 1 1 d . . . Fe2 Fe 0.03747(3) 0.63322(3) 0.144590(16) 0.03885(16) Uani 1 1 d . . . Cl3 Cl -0.10028(6) 0.63040(7) 0.15037(4) 0.0672(4) Uani 1 1 d . . . Cl4 Cl 0.04375(7) 0.74227(6) 0.11651(3) 0.0588(3) Uani 1 1 d . . . O3S O -0.1410(2) 0.7082(2) 0.06614(11) 0.0847(12) Uani 1 1 d . . . O4S O -0.1463(3) 0.8090(2) 0.13472(15) 0.1087(15) Uani 1 1 d . . . N12 N 0.08822(19) 0.55180(17) 0.11934(9) 0.0368(9) Uani 1 1 d . . . N22 N 0.10307(18) 0.62107(18) 0.18946(9) 0.0377(9) Uani 1 1 d . . . Li2 Li -0.0970(5) 0.7308(5) 0.1126(3) 0.073(3) Uani 1 1 d . . . Fe3 Fe 0.02975(4) 0.12614(3) 0.020319(15) 0.03820(15) Uani 1 1 d . . . Cl13 Cl -0.08481(7) 0.06520(6) 0.03662(4) 0.0578(3) Uani 1 1 d . . . Cl23 Cl -0.01141(8) 0.23516(6) 0.04185(3) 0.0653(4) Uani 1 1 d . . . O5S O -0.1571(3) 0.1705(2) 0.10590(10) 0.0934(14) Uani 1 1 d . . . O6S O -0.2202(3) 0.1942(2) 0.02424(12) 0.0888(12) Uani 1 1 d . . . N13 N 0.1281(2) 0.07918(17) 0.03899(9) 0.0387(9) Uani 1 1 d . . . N23 N 0.06928(19) 0.12740(17) -0.03122(8) 0.0360(8) Uani 1 1 d . . . Li3 Li -0.1283(5) 0.1757(5) 0.0563(2) 0.069(3) Uani 1 1 d . . . C17S C -0.1370(8) 0.1151(5) 0.1284(2) 0.267(8) Uani 1 1 d . . . H17A H -0.0782 0.1113 0.1295 0.320 Uiso 1 1 calc R . . H17E H -0.1577 0.0709 0.1178 0.320 Uiso 1 1 calc R . . C18S C -0.1666(5) 0.1220(4) 0.16354(18) 0.114(2) Uani 1 1 d . . . H18A H -0.1229 0.1205 0.1816 0.137 Uiso 1 1 calc R . . H18B H -0.2054 0.0843 0.1691 0.137 Uiso 1 1 calc R . . C19S C -0.2056(5) 0.1914(4) 0.16330(18) 0.115(3) Uani 1 1 d . . . H19A H -0.1874 0.2203 0.1840 0.138 Uiso 1 1 calc R . . H19B H -0.2643 0.1865 0.1645 0.138 Uiso 1 1 calc R . . C20S C -0.1806(5) 0.2234(3) 0.12807(19) 0.110(2) Uani 1 1 d . . . H20A H -0.2256 0.2494 0.1171 0.132 Uiso 1 1 calc R . . H20B H -0.1360 0.2567 0.1320 0.132 Uiso 1 1 calc R . . C21S C -0.2788(4) 0.1396(5) 0.0189(2) 0.123(3) Uani 1 1 d . . . H21A H -0.2553 0.0928 0.0240 0.147 Uiso 1 1 calc R . . H21B H -0.3250 0.1467 0.0352 0.147 Uiso 1 1 calc R . . C22S C -0.3030(7) 0.1446(6) -0.0186(3) 0.191(5) Uani 1 1 d . . . H22A H -0.2894 0.1003 -0.0313 0.229 Uiso 1 1 calc R . . H22B H -0.3615 0.1509 -0.0198 0.229 Uiso 1 1 calc R . . C23S C -0.2681(6) 0.1970(6) -0.0347(3) 0.183(5) Uani 1 1 d . . . H23A H -0.3074 0.2344 -0.0401 0.219 Uiso 1 1 calc R . . H23B H -0.2442 0.1811 -0.0579 0.219 Uiso 1 1 calc R . . C24S C -0.2054(5) 0.2245(4) -0.0104(2) 0.132(3) Uani 1 1 d . . . H24A H -0.1520 0.2109 -0.0194 0.158 Uiso 1 1 calc R . . H24B H -0.2082 0.2764 -0.0091 0.158 Uiso 1 1 calc R . . C17 C 0.2719(2) 0.0505(3) 0.03931(13) 0.0605(14) Uani 1 1 d . . . H17B H 0.2605 0.0382 0.0646 0.091 Uiso 1 1 calc R . . H17C H 0.3122 0.0877 0.0386 0.091 Uiso 1 1 calc R . . H17D H 0.2919 0.0089 0.0265 0.091 Uiso 1 1 calc R . . C18 C 0.1202(2) 0.0470(2) 0.07424(12) 0.0395(11) Uani 1 1 d . . . C19 C 0.0103(2) 0.1358(2) -0.05909(11) 0.0394(11) Uani 1 1 d . . . C27 C 0.1965(3) 0.0759(2) 0.02124(12) 0.0432(11) Uani 1 1 d . . . C28 C 0.0881(3) -0.0215(2) 0.07656(12) 0.0433(11) Uani 1 1 d . . . C29 C -0.0342(3) 0.0764(2) -0.06921(11) 0.0421(11) Uani 1 1 d . . . C37 C 0.2034(2) 0.0966(2) -0.01545(12) 0.0463(12) Uani 1 1 d . . . H37A H 0.2564 0.0979 -0.0245 0.056 Uiso 1 1 calc R . . C38 C 0.0737(3) -0.0505(3) 0.11004(13) 0.0533(13) Uani 1 1 d . . . H38A H 0.0543 -0.0973 0.1118 0.064 Uiso 1 1 calc R . . C39 C -0.0911(3) 0.0844(3) -0.09601(13) 0.0576(14) Uani 1 1 d . . . H39A H -0.1215 0.0448 -0.1034 0.069 Uiso 1 1 calc R . . C47 C 0.1454(3) 0.1150(2) -0.04016(11) 0.0416(11) Uani 1 1 d . . . C48 C 0.0875(3) -0.0122(3) 0.14098(15) 0.0628(14) Uani 1 1 d . . . H48A H 0.0753 -0.0319 0.1640 0.075 Uiso 1 1 calc R . . C49 C -0.1047(3) 0.1481(3) -0.11218(13) 0.0700(16) Uani 1 1 d . . . H49A H -0.1439 0.1518 -0.1307 0.084 Uiso 1 1 calc R . . C57 C 0.1700(3) 0.1211(3) -0.07944(12) 0.0677(15) Uani 1 1 d . . . H57A H 0.1239 0.1349 -0.0941 0.102 Uiso 1 1 calc R . . H57B H 0.1902 0.0756 -0.0879 0.102 Uiso 1 1 calc R . . H57C H 0.2120 0.1566 -0.0818 0.102 Uiso 1 1 calc R . . C58 C 0.1190(3) 0.0550(3) 0.13896(12) 0.0514(13) Uani 1 1 d . . . H58A H 0.1288 0.0807 0.1606 0.062 Uiso 1 1 calc R . . C59 C -0.0625(3) 0.2065(3) -0.10192(13) 0.0622(15) Uani 1 1 d . . . H59A H -0.0726 0.2504 -0.1133 0.075 Uiso 1 1 calc R . . C68 C 0.1364(3) 0.0852(2) 0.10557(12) 0.0446(12) Uani 1 1 d . . . C69 C -0.0042(3) 0.2020(2) -0.07462(12) 0.0479(13) Uani 1 1 d . . . C78 C 0.0747(3) -0.0657(2) 0.04246(13) 0.0558(13) Uani 1 1 d . . . H78A H 0.0695 -0.0324 0.0216 0.067 Uiso 1 1 calc R . . C79 C -0.0211(3) 0.0044(2) -0.05183(12) 0.0479(12) Uani 1 1 d . . . H79A H 0.0025 0.0128 -0.0273 0.057 Uiso 1 1 calc R . . C88 C -0.0012(3) -0.1094(2) 0.04376(14) 0.0711(16) Uani 1 1 d . . . H88A H -0.0061 -0.1366 0.0213 0.107 Uiso 1 1 calc R . . H88B H -0.0473 -0.0782 0.0463 0.107 Uiso 1 1 calc R . . H88C H 0.0011 -0.1415 0.0645 0.107 Uiso 1 1 calc R . . C89 C -0.0980(3) -0.0371(2) -0.04622(13) 0.0633(14) Uani 1 1 d . . . H89A H -0.0857 -0.0825 -0.0350 0.095 Uiso 1 1 calc R . . H89B H -0.1239 -0.0449 -0.0697 0.095 Uiso 1 1 calc R . . H89C H -0.1339 -0.0105 -0.0304 0.095 Uiso 1 1 calc R . . C98 C 0.1451(3) -0.1137(3) 0.03434(16) 0.0875(19) Uani 1 1 d . . . H98A H 0.1339 -0.1413 0.0125 0.131 Uiso 1 1 calc R . . H98B H 0.1537 -0.1456 0.0549 0.131 Uiso 1 1 calc R . . H98C H 0.1931 -0.0853 0.0305 0.131 Uiso 1 1 calc R . . C99 C 0.0392(3) -0.0387(3) -0.07333(14) 0.0752(16) Uani 1 1 d . . . H99A H 0.0882 -0.0114 -0.0765 0.113 Uiso 1 1 calc R . . H99B H 0.0169 -0.0504 -0.0971 0.113 Uiso 1 1 calc R . . H99C H 0.0513 -0.0822 -0.0602 0.113 Uiso 1 1 calc R . . C108 C 0.1734(3) 0.1579(3) 0.10539(14) 0.0636(15) Uani 1 1 d . . . H10G H 0.1813 0.1718 0.0795 0.076 Uiso 1 1 calc R . . C109 C 0.0407(3) 0.2669(2) -0.06480(12) 0.0608(14) Uani 1 1 d . . . H10H H 0.0830 0.2535 -0.0470 0.073 Uiso 1 1 calc R . . C118 C 0.2550(3) 0.1591(3) 0.12377(15) 0.0875(19) Uani 1 1 d . . . H11R H 0.2767 0.2069 0.1230 0.131 Uiso 1 1 calc R . . H11S H 0.2911 0.1270 0.1111 0.131 Uiso 1 1 calc R . . H11T H 0.2494 0.1441 0.1491 0.131 Uiso 1 1 calc R . . C119 C -0.0115(3) 0.3219(2) -0.04724(13) 0.0794(17) Uani 1 1 d . . . H11U H -0.0379 0.3017 -0.0260 0.119 Uiso 1 1 calc R . . H11V H -0.0519 0.3378 -0.0646 0.119 Uiso 1 1 calc R . . H11W H 0.0213 0.3620 -0.0398 0.119 Uiso 1 1 calc R . . C128 C 0.1187(4) 0.2127(3) 0.12283(14) 0.0842(19) Uani 1 1 d . . . H12O H 0.0665 0.2118 0.1109 0.126 Uiso 1 1 calc R . . H12P H 0.1424 0.2595 0.1201 0.126 Uiso 1 1 calc R . . H12Q H 0.1122 0.2020 0.1486 0.126 Uiso 1 1 calc R . . C129 C 0.0821(3) 0.2994(3) -0.09827(13) 0.0758(17) Uani 1 1 d . . . H12R H 0.1161 0.2640 -0.1098 0.114 Uiso 1 1 calc R . . H12S H 0.1148 0.3394 -0.0906 0.114 Uiso 1 1 calc R . . H12T H 0.0417 0.3154 -0.1156 0.114 Uiso 1 1 calc R . . C9S C -0.1402(4) 0.6379(4) 0.0527(2) 0.128(3) Uani 1 1 d . . . H9SA H -0.1838 0.6100 0.0637 0.154 Uiso 1 1 calc R . . H9SB H -0.0888 0.6148 0.0583 0.154 Uiso 1 1 calc R . . C10S C -0.1515(6) 0.6440(6) 0.0132(2) 0.208(6) Uani 1 1 d . . . H10C H -0.1005 0.6362 0.0003 0.250 Uiso 1 1 calc R . . H10D H -0.1909 0.6091 0.0046 0.250 Uiso 1 1 calc R . . C11S C -0.1803(6) 0.7150(6) 0.0071(2) 0.184(5) Uani 1 1 d . . . H11J H -0.1472 0.7386 -0.0115 0.221 Uiso 1 1 calc R . . H11K H -0.2361 0.7138 -0.0017 0.221 Uiso 1 1 calc R . . C12S C -0.1758(6) 0.7526(4) 0.0405(2) 0.171(4) Uani 1 1 d . . . H12G H -0.1431 0.7956 0.0375 0.206 Uiso 1 1 calc R . . H12N H -0.2298 0.7667 0.0486 0.206 Uiso 1 1 calc R . . C13S C -0.1705(6) 0.8704(5) 0.1223(3) 0.203(5) Uani 1 1 d . . . H13A H -0.2260 0.8663 0.1134 0.243 Uiso 1 1 calc R . . H13B H -0.1364 0.8848 0.1017 0.243 Uiso 1 1 calc R . . C14S C -0.1662(9) 0.9241(5) 0.1513(5) 0.240(9) Uani 1 1 d . . . H14A H -0.1232 0.9584 0.1465 0.288 Uiso 1 1 calc R . . H14B H -0.2175 0.9495 0.1537 0.288 Uiso 1 1 calc R . . C15S C -0.1496(8) 0.8837(7) 0.1828(4) 0.254(9) Uani 1 1 d . . . H15A H -0.1015 0.9020 0.1952 0.304 Uiso 1 1 calc R . . H15B H -0.1950 0.8861 0.1999 0.304 Uiso 1 1 calc R . . C16S C -0.1379(8) 0.8182(6) 0.1723(3) 0.224(6) Uani 1 1 d . . . H16A H -0.1764 0.7873 0.1849 0.269 Uiso 1 1 calc R . . H16B H -0.0836 0.8035 0.1796 0.269 Uiso 1 1 calc R . . C14 C 0.1938(3) 0.4644(2) 0.10748(12) 0.0579(14) Uani 1 1 d . . . H14C H 0.1620 0.4571 0.0855 0.087 Uiso 1 1 calc R . . H14D H 0.1965 0.4205 0.1213 0.087 Uiso 1 1 calc R . . H14E H 0.2478 0.4790 0.1007 0.087 Uiso 1 1 calc R . . C15 C 0.0488(2) 0.5242(2) 0.08807(13) 0.0432(12) Uani 1 1 d . . . C16 C 0.0740(2) 0.6565(2) 0.22118(11) 0.0377(11) Uani 1 1 d . . . C24 C 0.1554(3) 0.5213(2) 0.13058(13) 0.0429(12) Uani 1 1 d . . . C25 C 0.0690(3) 0.5481(3) 0.05311(13) 0.0526(13) Uani 1 1 d . . . C26 C 0.0990(3) 0.7248(3) 0.22958(12) 0.0470(12) Uani 1 1 d . . . C34 C 0.1931(2) 0.5386(2) 0.16289(12) 0.0407(12) Uani 1 1 d . . . H34A H 0.2438 0.5173 0.1662 0.049 Uiso 1 1 calc R . . C35 C 0.0283(3) 0.5189(3) 0.02376(14) 0.0700(15) Uani 1 1 d . . . H35A H 0.0412 0.5345 0.0000 0.084 Uiso 1 1 calc R . . C36 C 0.0642(3) 0.7579(3) 0.25924(15) 0.0744(17) Uani 1 1 d . . . H36A H 0.0802 0.8043 0.2654 0.089 Uiso 1 1 calc R . . C44 C 0.1690(2) 0.5821(2) 0.19115(13) 0.0433(12) Uani 1 1 d . . . C45 C -0.0286(4) 0.4691(3) 0.02774(17) 0.0849(18) Uani 1 1 d . . . H45A H -0.0539 0.4493 0.0071 0.102 Uiso 1 1 calc R . . C46 C 0.0067(3) 0.7245(4) 0.27982(16) 0.0806(19) Uani 1 1 d . . . H46A H -0.0158 0.7477 0.3002 0.097 Uiso 1 1 calc R . . C54 C 0.2201(3) 0.5826(3) 0.22508(12) 0.0553(14) Uani 1 1 d . . . H54A H 0.1970 0.6151 0.2428 0.083 Uiso 1 1 calc R . . H54B H 0.2742 0.5980 0.2189 0.083 Uiso 1 1 calc R . . H54C H 0.2220 0.5352 0.2354 0.083 Uiso 1 1 calc R . . C55 C -0.0495(3) 0.4475(3) 0.06213(18) 0.0779(18) Uani 1 1 d . . . H55A H -0.0903 0.4133 0.0648 0.094 Uiso 1 1 calc R . . C56 C -0.0177(3) 0.6586(3) 0.27107(15) 0.0779(18) Uani 1 1 d . . . H56A H -0.0574 0.6364 0.2854 0.093 Uiso 1 1 calc R . . C65 C -0.0129(3) 0.4741(2) 0.09303(15) 0.0552(13) Uani 1 1 d . . . C66 C 0.0142(3) 0.6230(3) 0.24169(12) 0.0511(12) Uani 1 1 d . . . C75 C 0.1318(3) 0.6029(3) 0.04613(13) 0.0612(15) Uani 1 1 d . . . H75A H 0.1579 0.6145 0.0698 0.073 Uiso 1 1 calc R . . C76 C 0.1611(3) 0.7640(2) 0.20824(13) 0.0517(13) Uani 1 1 d . . . H76A H 0.1766 0.7337 0.1872 0.062 Uiso 1 1 calc R . . C85 C 0.0960(4) 0.6708(3) 0.03075(14) 0.0868(19) Uani 1 1 d . . . H85A H 0.0549 0.6885 0.0473 0.130 Uiso 1 1 calc R . . H85B H 0.0722 0.6613 0.0070 0.130 Uiso 1 1 calc R . . H85C H 0.1381 0.7062 0.0281 0.130 Uiso 1 1 calc R . . C86 C 0.1293(3) 0.8336(3) 0.19287(14) 0.0723(16) Uani 1 1 d . . . H86A H 0.0810 0.8246 0.1786 0.108 Uiso 1 1 calc R . . H86B H 0.1699 0.8550 0.1773 0.108 Uiso 1 1 calc R . . H86C H 0.1167 0.8657 0.2129 0.108 Uiso 1 1 calc R . . C95 C 0.1957(3) 0.5766(3) 0.02047(15) 0.0887(19) Uani 1 1 d . . . H95A H 0.2187 0.5331 0.0301 0.133 Uiso 1 1 calc R . . H95B H 0.2375 0.6122 0.0181 0.133 Uiso 1 1 calc R . . H95C H 0.1720 0.5674 -0.0034 0.133 Uiso 1 1 calc R . . C96 C 0.2372(3) 0.7784(3) 0.23064(14) 0.0770(17) Uani 1 1 d . . . H96A H 0.2578 0.7340 0.2403 0.116 Uiso 1 1 calc R . . H96B H 0.2244 0.8101 0.2507 0.116 Uiso 1 1 calc R . . H96C H 0.2775 0.8002 0.2151 0.116 Uiso 1 1 calc R . . C105 C -0.0342(3) 0.4482(2) 0.13026(15) 0.0676(15) Uani 1 1 d . . . H10E H -0.0165 0.4849 0.1479 0.081 Uiso 1 1 calc R . . C106 C -0.0118(3) 0.5486(3) 0.23271(14) 0.0656(16) Uani 1 1 d . . . H10F H -0.0003 0.5407 0.2064 0.079 Uiso 1 1 calc R . . C115 C 0.0081(3) 0.3802(3) 0.14019(18) 0.103(2) Uani 1 1 d . . . H11L H 0.0657 0.3862 0.1371 0.155 Uiso 1 1 calc R . . H11M H -0.0107 0.3423 0.1244 0.155 Uiso 1 1 calc R . . H11N H -0.0034 0.3684 0.1655 0.155 Uiso 1 1 calc R . . C116 C -0.1010(3) 0.5354(3) 0.23843(15) 0.088(2) Uani 1 1 d . . . H11O H -0.1136 0.4866 0.2322 0.132 Uiso 1 1 calc R . . H11P H -0.1318 0.5672 0.2229 0.132 Uiso 1 1 calc R . . H11Q H -0.1147 0.5439 0.2639 0.132 Uiso 1 1 calc R . . C125 C -0.1251(3) 0.4387(3) 0.13526(18) 0.097(2) Uani 1 1 d . . . H12H H -0.1525 0.4825 0.1289 0.146 Uiso 1 1 calc R . . H12I H -0.1365 0.4267 0.1606 0.146 Uiso 1 1 calc R . . H12J H -0.1440 0.4008 0.1194 0.146 Uiso 1 1 calc R . . C126 C 0.0356(3) 0.4940(3) 0.25416(16) 0.096(2) Uani 1 1 d . . . H12K H 0.0928 0.5017 0.2503 0.144 Uiso 1 1 calc R . . H12L H 0.0212 0.4468 0.2459 0.144 Uiso 1 1 calc R . . H12M H 0.0234 0.4987 0.2800 0.144 Uiso 1 1 calc R . . C1S C 0.6535(5) 0.8165(5) 0.2842(2) 0.134(3) Uani 1 1 d . . . H1SA H 0.6350 0.7944 0.3070 0.161 Uiso 1 1 calc R . . H1SB H 0.6104 0.8467 0.2745 0.161 Uiso 1 1 calc R . . C2S C 0.7269(6) 0.8580(5) 0.2905(3) 0.161(4) Uani 1 1 d . . . H2SA H 0.7302 0.8980 0.2734 0.193 Uiso 1 1 calc R . . H2SB H 0.7283 0.8764 0.3156 0.193 Uiso 1 1 calc R . . C3S C 0.7906(6) 0.8094(6) 0.2845(3) 0.202(6) Uani 1 1 d . . . H3SA H 0.8136 0.7938 0.3079 0.242 Uiso 1 1 calc R . . H3SB H 0.8333 0.8315 0.2699 0.242 Uiso 1 1 calc R . . C4S C 0.7556(4) 0.7489(4) 0.2648(2) 0.136(3) Uani 1 1 d . . . H4SA H 0.7836 0.7416 0.2414 0.163 Uiso 1 1 calc R . . H4SB H 0.7603 0.7055 0.2794 0.163 Uiso 1 1 calc R . . C5S C 0.6421(5) 0.7149(4) 0.14216(16) 0.122(3) Uani 1 1 d . . . H5SA H 0.5837 0.7180 0.1387 0.147 Uiso 1 1 calc R . . H5SB H 0.6662 0.7597 0.1341 0.147 Uiso 1 1 calc R . . C6S C 0.6733(4) 0.6585(3) 0.12151(17) 0.098(2) Uani 1 1 d . . . H6SA H 0.7269 0.6701 0.1120 0.118 Uiso 1 1 calc R . . H6SB H 0.6378 0.6472 0.1009 0.118 Uiso 1 1 calc R . . C7S C 0.6774(4) 0.5987(3) 0.14728(19) 0.098(2) Uani 1 1 d . . . H7SA H 0.7273 0.5718 0.1438 0.118 Uiso 1 1 calc R . . H7SB H 0.6316 0.5666 0.1437 0.118 Uiso 1 1 calc R . . C8S C 0.6750(4) 0.6306(3) 0.18442(16) 0.0889(19) Uani 1 1 d . . . H8SA H 0.6323 0.6088 0.1991 0.107 Uiso 1 1 calc R . . H8SB H 0.7265 0.6238 0.1970 0.107 Uiso 1 1 calc R . . C11 C 0.2985(3) 1.0182(2) 0.23079(13) 0.0574(14) Uani 1 1 d . . . H11A H 0.3278 1.0263 0.2534 0.086 Uiso 1 1 calc R . . H11B H 0.2458 0.9988 0.2363 0.086 Uiso 1 1 calc R . . H11C H 0.2924 1.0627 0.2178 0.086 Uiso 1 1 calc R . . C12 C 0.4525(2) 0.9668(2) 0.25072(11) 0.0340(10) Uani 1 1 d . . . C13 C 0.4404(2) 0.8375(2) 0.11709(11) 0.0363(11) Uani 1 1 d . . . C21 C 0.3443(3) 0.9666(2) 0.20736(12) 0.0371(11) Uani 1 1 d . . . C22 C 0.5061(2) 1.0230(2) 0.24657(11) 0.0386(11) Uani 1 1 d . . . C23 C 0.5024(2) 0.8703(2) 0.09796(11) 0.0418(12) Uani 1 1 d . . . C31 C 0.3101(2) 0.9497(2) 0.17384(12) 0.0392(11) Uani 1 1 d . . . H31A H 0.2592 0.9697 0.1695 0.047 Uiso 1 1 calc R . . C32 C 0.5455(3) 1.0481(2) 0.27701(13) 0.0531(13) Uani 1 1 d . . . H32A H 0.5802 1.0874 0.2749 0.064 Uiso 1 1 calc R . . C33 C 0.5382(3) 0.8339(2) 0.07005(12) 0.0530(13) Uani 1 1 d . . . H33A H 0.5807 0.8552 0.0570 0.064 Uiso 1 1 calc R . . C41 C 0.3395(2) 0.9081(2) 0.14620(12) 0.0352(11) Uani 1 1 d . . . C42 C 0.5349(3) 1.0167(3) 0.31037(13) 0.0577(13) Uani 1 1 d . . . H42A H 0.5639 1.0330 0.3308 0.069 Uiso 1 1 calc R . . C43 C 0.5132(3) 0.7670(3) 0.06071(12) 0.0595(14) Uani 1 1 d . . . H43A H 0.5391 0.7423 0.0417 0.071 Uiso 1 1 calc R . . C51 C 0.2882(3) 0.9044(2) 0.11228(11) 0.0520(13) Uani 1 1 d . . . H51A H 0.3139 0.8740 0.0943 0.078 Uiso 1 1 calc R . . H51B H 0.2818 0.9517 0.1022 0.078 Uiso 1 1 calc R . . H51C H 0.2357 0.8852 0.1185 0.078 Uiso 1 1 calc R . . C52 C 0.4821(3) 0.9616(2) 0.31397(12) 0.0509(12) Uani 1 1 d . . . H52A H 0.4743 0.9410 0.3372 0.061 Uiso 1 1 calc R . . C53 C 0.4516(3) 0.7366(2) 0.07883(12) 0.0490(13) Uani 1 1 d . . . H53A H 0.4344 0.6911 0.0717 0.059 Uiso 1 1 calc R . . C62 C 0.4400(2) 0.9355(2) 0.28447(11) 0.0391(11) Uani 1 1 d . . . C63 C 0.4129(2) 0.7695(2) 0.10739(11) 0.0341(10) Uani 1 1 d . . . C72 C 0.5216(3) 1.0567(2) 0.20908(12) 0.0509(12) Uani 1 1 d . . . H72A H 0.5074 1.0210 0.1902 0.061 Uiso 1 1 calc R . . C73 C 0.5269(3) 0.9451(2) 0.10726(12) 0.0536(13) Uani 1 1 d . . . H73A H 0.5210 0.9507 0.1341 0.064 Uiso 1 1 calc R . . C82 C 0.6087(3) 1.0765(3) 0.20347(14) 0.0784(18) Uani 1 1 d . . . H82A H 0.6153 1.0976 0.1794 0.118 Uiso 1 1 calc R . . H82B H 0.6419 1.0343 0.2053 0.118 Uiso 1 1 calc R . . H82C H 0.6248 1.1104 0.2221 0.118 Uiso 1 1 calc R . . C83 C 0.6132(3) 0.9615(3) 0.09795(15) 0.090(2) Uani 1 1 d . . . H83A H 0.6481 0.9268 0.1095 0.135 Uiso 1 1 calc R . . H83B H 0.6268 1.0086 0.1067 0.135 Uiso 1 1 calc R . . H83C H 0.6204 0.9596 0.0716 0.135 Uiso 1 1 calc R . . C92 C 0.4679(3) 1.1215(3) 0.20303(13) 0.0754(15) Uani 1 1 d . . . H92A H 0.4788 1.1416 0.1791 0.113 Uiso 1 1 calc R . . H92B H 0.4790 1.1567 0.2217 0.113 Uiso 1 1 calc R . . H92C H 0.4118 1.1074 0.2044 0.113 Uiso 1 1 calc R . . C93 C 0.4716(4) 0.9989(2) 0.08937(14) 0.0777(17) Uani 1 1 d . . . H93A H 0.4161 0.9878 0.0954 0.116 Uiso 1 1 calc R . . H93B H 0.4787 0.9973 0.0630 0.116 Uiso 1 1 calc R . . H93C H 0.4846 1.0461 0.0983 0.116 Uiso 1 1 calc R . . C102 C 0.3821(2) 0.8760(2) 0.29010(12) 0.0458(12) Uani 1 1 d . . . H10A H 0.3631 0.8604 0.2657 0.055 Uiso 1 1 calc R . . C103 C 0.3464(2) 0.7323(2) 0.12713(12) 0.0432(12) Uani 1 1 d . . . H10B H 0.3259 0.7645 0.1464 0.052 Uiso 1 1 calc R . . C112 C 0.3089(3) 0.8994(3) 0.31195(13) 0.0675(16) Uani 1 1 d . . . H11D H 0.2842 0.9400 0.3001 0.101 Uiso 1 1 calc R . . H11E H 0.3254 0.9123 0.3365 0.101 Uiso 1 1 calc R . . H11F H 0.2704 0.8607 0.3132 0.101 Uiso 1 1 calc R . . C113 C 0.3753(3) 0.6650(2) 0.14535(13) 0.0550(13) Uani 1 1 d . . . H11G H 0.4198 0.6759 0.1616 0.083 Uiso 1 1 calc R . . H11H H 0.3932 0.6316 0.1268 0.083 Uiso 1 1 calc R . . H11I H 0.3317 0.6441 0.1593 0.083 Uiso 1 1 calc R . . C122 C 0.4203(3) 0.8123(3) 0.30884(13) 0.0674(15) Uani 1 1 d . . . H12A H 0.4670 0.7970 0.2950 0.101 Uiso 1 1 calc R . . H12B H 0.3815 0.7738 0.3101 0.101 Uiso 1 1 calc R . . H12C H 0.4368 0.8254 0.3334 0.101 Uiso 1 1 calc R . . C123 C 0.2764(3) 0.7142(3) 0.10152(14) 0.0672(15) Uani 1 1 d . . . H12D H 0.2572 0.7572 0.0898 0.101 Uiso 1 1 calc R . . H12E H 0.2330 0.6930 0.1155 0.101 Uiso 1 1 calc R . . H12F H 0.2945 0.6809 0.0830 0.101 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 0.0386(3) 0.0393(4) 0.0324(3) -0.0026(3) -0.0055(3) 0.0084(3) Cl11 0.0705(8) 0.0448(7) 0.0581(8) 0.0080(6) -0.0128(8) 0.0075(7) Cl21 0.0395(6) 0.0682(9) 0.0823(10) 0.0038(8) -0.0002(7) 0.0074(7) O1 0.075(3) 0.129(4) 0.062(3) -0.008(3) -0.018(2) 0.010(3) O2 0.106(3) 0.076(3) 0.048(2) 0.007(2) 0.003(2) 0.042(2) N11 0.035(2) 0.036(2) 0.029(2) -0.0047(18) 0.0006(18) -0.0024(18) N21 0.042(2) 0.032(2) 0.026(2) -0.0027(18) -0.0014(18) 0.0030(18) Li1 0.079(6) 0.065(6) 0.051(5) -0.002(5) -0.012(5) 0.025(5) Fe2 0.0364(3) 0.0392(4) 0.0409(4) 0.0038(3) -0.0062(3) 0.0031(3) Cl3 0.0368(7) 0.0741(9) 0.0907(10) 0.0233(9) -0.0014(7) 0.0059(7) Cl4 0.0656(8) 0.0479(7) 0.0628(8) 0.0158(6) -0.0076(7) -0.0002(7) O3S 0.090(3) 0.091(3) 0.073(3) 0.002(3) -0.032(2) 0.011(2) O4S 0.115(3) 0.089(3) 0.122(4) -0.013(3) 0.007(3) 0.049(3) N12 0.034(2) 0.037(2) 0.039(2) 0.0046(19) -0.0060(19) 0.0041(18) N22 0.0316(19) 0.045(2) 0.036(2) 0.007(2) 0.0033(18) -0.0039(19) Li2 0.075(6) 0.072(6) 0.072(6) 0.008(5) -0.016(5) 0.019(5) Fe3 0.0411(3) 0.0387(4) 0.0348(3) 0.0008(3) 0.0026(3) 0.0054(4) Cl13 0.0462(7) 0.0536(8) 0.0736(9) -0.0088(7) 0.0181(7) 0.0020(6) Cl23 0.0935(10) 0.0417(7) 0.0607(8) -0.0065(6) 0.0054(8) 0.0098(7) O5S 0.155(4) 0.072(3) 0.053(3) 0.008(2) 0.036(3) 0.033(3) O6S 0.089(3) 0.101(3) 0.076(3) -0.004(3) -0.003(3) 0.028(3) N13 0.041(2) 0.040(2) 0.035(2) 0.0022(19) -0.004(2) -0.0027(18) N23 0.040(2) 0.040(2) 0.029(2) 0.0038(18) -0.0035(18) -0.0024(18) Li3 0.078(6) 0.065(6) 0.065(6) 0.002(5) 0.011(5) 0.025(5) C17S 0.53(2) 0.173(9) 0.099(7) 0.078(7) 0.156(10) 0.193(12) C18S 0.149(6) 0.116(6) 0.076(5) 0.013(5) 0.023(5) 0.023(6) C19S 0.136(6) 0.136(7) 0.074(5) -0.010(5) 0.021(5) 0.032(6) C20S 0.157(7) 0.075(5) 0.098(6) -0.002(4) 0.020(5) 0.018(5) C21S 0.077(4) 0.180(8) 0.111(7) 0.038(7) 0.004(5) 0.004(6) C22S 0.282(14) 0.184(11) 0.107(8) 0.005(8) -0.073(9) -0.024(10) C23S 0.179(10) 0.249(13) 0.121(8) 0.097(9) -0.021(8) -0.030(9) C24S 0.155(7) 0.099(6) 0.141(8) 0.056(6) -0.036(7) -0.001(5) C17 0.045(3) 0.081(4) 0.056(3) 0.010(3) 0.000(3) 0.005(3) C18 0.035(2) 0.046(3) 0.037(3) 0.007(2) 0.001(2) 0.011(2) C19 0.044(3) 0.042(3) 0.032(2) 0.001(2) 0.004(2) 0.000(2) C27 0.038(3) 0.053(3) 0.039(3) 0.005(2) -0.002(3) -0.006(2) C28 0.043(3) 0.040(3) 0.047(3) 0.006(3) -0.009(2) -0.001(2) C29 0.036(3) 0.053(3) 0.038(3) -0.003(2) 0.008(3) 0.003(3) C37 0.025(2) 0.071(3) 0.042(3) 0.004(3) 0.008(2) -0.001(2) C38 0.063(3) 0.047(3) 0.050(3) 0.017(3) -0.007(3) 0.001(3) C39 0.055(3) 0.072(4) 0.046(3) 0.001(3) -0.003(3) -0.007(3) C47 0.042(3) 0.050(3) 0.033(3) 0.004(2) 0.005(2) -0.003(2) C48 0.069(3) 0.072(4) 0.048(3) 0.025(3) 0.009(3) 0.017(3) C49 0.065(4) 0.101(5) 0.044(3) 0.019(3) -0.015(3) 0.009(3) C57 0.051(3) 0.100(4) 0.051(3) 0.010(3) 0.015(3) 0.008(3) C58 0.060(3) 0.065(4) 0.029(3) 0.003(3) -0.002(3) 0.019(3) C59 0.073(4) 0.062(4) 0.051(3) 0.015(3) -0.009(3) 0.005(3) C68 0.054(3) 0.047(3) 0.033(3) 0.002(3) 0.000(3) 0.007(2) C69 0.054(3) 0.052(3) 0.038(3) 0.008(3) -0.002(3) 0.003(2) C78 0.065(3) 0.047(3) 0.055(3) 0.012(3) -0.009(3) 0.000(3) C79 0.053(3) 0.045(3) 0.046(3) -0.002(2) -0.001(3) -0.004(3) C88 0.083(4) 0.048(3) 0.083(4) 0.009(3) -0.022(3) -0.012(3) C89 0.068(3) 0.057(3) 0.064(4) -0.007(3) 0.005(3) -0.011(3) C98 0.075(4) 0.094(4) 0.093(5) -0.037(4) -0.017(4) 0.009(4) C99 0.065(3) 0.067(3) 0.094(4) -0.015(3) 0.013(4) 0.017(3) C108 0.088(4) 0.058(4) 0.045(3) -0.010(3) 0.002(3) 0.002(3) C109 0.093(4) 0.049(3) 0.041(3) 0.011(3) -0.007(3) -0.007(3) C118 0.086(4) 0.090(5) 0.087(4) -0.008(4) -0.013(4) -0.030(3) C119 0.123(5) 0.049(3) 0.066(4) 0.008(3) 0.011(4) 0.007(3) C128 0.129(5) 0.064(4) 0.059(4) -0.012(3) -0.007(4) 0.015(4) C129 0.100(4) 0.063(4) 0.064(4) 0.008(3) -0.002(4) -0.016(3) C9S 0.114(6) 0.150(8) 0.119(7) -0.051(6) -0.030(5) 0.054(6) C10S 0.251(12) 0.250(13) 0.125(8) -0.089(9) -0.130(8) 0.131(10) C11S 0.194(10) 0.272(15) 0.086(7) 0.029(9) -0.036(7) -0.038(10) C12S 0.255(11) 0.143(8) 0.116(7) 0.061(7) -0.112(8) -0.061(7) C13S 0.250(11) 0.101(7) 0.257(14) 0.028(9) 0.073(10) 0.078(9) C14S 0.213(13) 0.068(7) 0.44(3) 0.003(11) 0.080(15) 0.013(7) C15S 0.204(11) 0.184(13) 0.37(2) -0.211(16) -0.020(14) -0.004(12) C16S 0.330(16) 0.221(13) 0.121(9) -0.074(9) 0.011(10) 0.120(11) C14 0.056(3) 0.065(3) 0.053(3) 0.005(3) -0.005(3) 0.019(3) C15 0.037(3) 0.045(3) 0.047(3) -0.006(2) -0.010(3) 0.011(2) C16 0.029(2) 0.052(3) 0.032(3) 0.004(2) -0.001(2) -0.002(2) C24 0.036(3) 0.044(3) 0.049(3) 0.005(2) 0.005(3) -0.003(2) C25 0.051(3) 0.061(3) 0.046(3) -0.013(3) -0.015(3) 0.007(3) C26 0.047(3) 0.054(3) 0.040(3) -0.003(3) -0.004(3) 0.002(3) C34 0.027(2) 0.052(3) 0.042(3) 0.004(3) -0.008(2) 0.008(2) C35 0.065(3) 0.094(4) 0.051(3) -0.012(3) -0.019(3) -0.001(4) C36 0.083(4) 0.068(4) 0.072(4) -0.016(4) 0.009(4) -0.010(3) C44 0.035(3) 0.048(3) 0.046(3) 0.015(3) -0.005(3) -0.002(2) C45 0.080(4) 0.099(5) 0.075(5) -0.038(4) -0.011(4) -0.004(4) C46 0.072(4) 0.103(5) 0.067(4) -0.031(4) 0.023(3) -0.006(4) C54 0.047(3) 0.074(4) 0.045(3) 0.007(3) -0.016(3) 0.005(3) C55 0.051(3) 0.070(4) 0.113(5) -0.037(4) -0.007(4) -0.014(3) C56 0.070(4) 0.104(5) 0.059(4) -0.001(4) 0.022(3) -0.025(4) C65 0.044(3) 0.045(3) 0.076(4) -0.012(3) -0.001(3) -0.004(3) C66 0.050(3) 0.057(3) 0.046(3) 0.004(3) 0.002(3) -0.011(3) C75 0.064(3) 0.084(4) 0.036(3) 0.003(3) -0.007(3) -0.013(3) C76 0.057(3) 0.055(3) 0.043(3) -0.001(3) -0.001(3) -0.010(3) C85 0.132(5) 0.073(4) 0.055(4) 0.004(3) -0.020(4) 0.011(4) C86 0.086(4) 0.058(4) 0.073(4) 0.007(3) -0.013(3) -0.013(3) C95 0.079(4) 0.112(5) 0.074(4) 0.008(4) 0.003(4) 0.002(4) C96 0.062(3) 0.094(5) 0.075(4) 0.004(4) -0.006(3) -0.022(3) C105 0.059(3) 0.046(3) 0.098(5) -0.009(3) 0.005(4) -0.018(3) C106 0.058(3) 0.079(4) 0.060(4) 0.018(3) 0.014(3) -0.011(3) C115 0.086(4) 0.077(4) 0.146(6) 0.036(4) 0.011(4) 0.006(3) C116 0.070(4) 0.112(5) 0.083(4) 0.016(4) 0.003(4) -0.035(4) C125 0.062(4) 0.085(4) 0.144(6) -0.010(4) 0.017(4) -0.029(3) C126 0.082(4) 0.080(4) 0.125(5) 0.030(4) 0.002(5) -0.015(4) C1S 0.118(7) 0.206(9) 0.079(6) -0.030(6) -0.007(5) 0.001(7) C2S 0.191(10) 0.154(10) 0.137(8) -0.040(7) 0.028(8) -0.061(8) C3S 0.147(9) 0.208(13) 0.250(14) 0.002(10) -0.109(10) -0.065(9) C4S 0.092(5) 0.164(8) 0.152(8) 0.019(7) -0.051(6) 0.028(6) C5S 0.198(8) 0.117(6) 0.052(4) 0.007(4) 0.013(5) 0.047(6) C6S 0.126(6) 0.094(5) 0.076(5) -0.019(4) -0.020(4) 0.005(4) C7S 0.111(5) 0.071(5) 0.113(6) -0.014(5) -0.015(5) -0.003(4) C8S 0.108(5) 0.074(4) 0.084(5) 0.026(4) 0.002(4) 0.017(4) C11 0.050(3) 0.063(3) 0.059(3) -0.028(3) -0.003(3) 0.013(3) C12 0.035(3) 0.037(3) 0.030(3) -0.009(2) -0.004(2) 0.007(2) C13 0.045(3) 0.040(3) 0.024(2) 0.001(2) -0.003(2) 0.011(2) C21 0.037(3) 0.040(3) 0.034(3) -0.005(2) 0.005(2) 0.003(2) C22 0.039(3) 0.040(3) 0.037(3) -0.005(2) 0.000(2) -0.004(2) C23 0.052(3) 0.045(3) 0.028(2) 0.011(2) 0.001(2) -0.002(2) C31 0.037(3) 0.042(3) 0.039(3) 0.000(2) -0.005(2) 0.002(2) C32 0.053(3) 0.052(3) 0.055(3) -0.011(3) -0.002(3) -0.020(3) C33 0.065(3) 0.058(3) 0.036(3) 0.006(3) 0.013(3) -0.009(3) C41 0.040(3) 0.037(3) 0.029(3) 0.000(2) -0.011(2) 0.000(2) C42 0.062(3) 0.066(3) 0.046(3) -0.019(3) -0.008(3) -0.011(3) C43 0.085(4) 0.050(3) 0.043(3) -0.004(3) 0.014(3) 0.009(3) C51 0.058(3) 0.061(3) 0.038(3) 0.000(3) -0.013(3) 0.010(2) C52 0.055(3) 0.060(3) 0.037(3) -0.006(2) -0.005(3) -0.008(3) C53 0.069(4) 0.040(3) 0.037(3) -0.005(2) 0.000(3) -0.002(3) C62 0.045(3) 0.043(3) 0.030(3) -0.008(2) -0.002(2) -0.002(2) C63 0.044(3) 0.036(3) 0.022(2) 0.003(2) -0.001(2) 0.002(2) C72 0.062(3) 0.045(3) 0.046(3) 0.000(2) 0.006(3) -0.011(3) C73 0.072(3) 0.039(3) 0.050(3) 0.003(2) 0.012(3) -0.015(3) C82 0.072(4) 0.097(5) 0.067(4) 0.014(4) 0.014(3) -0.024(3) C83 0.089(4) 0.095(5) 0.086(5) -0.014(4) 0.019(4) -0.041(4) C92 0.098(4) 0.063(3) 0.066(3) 0.015(3) -0.009(4) 0.009(4) C93 0.120(5) 0.036(3) 0.076(4) 0.018(3) 0.003(4) -0.009(4) C102 0.047(3) 0.050(3) 0.041(3) -0.003(3) 0.003(2) -0.010(3) C103 0.049(3) 0.040(3) 0.041(3) -0.010(2) 0.001(2) 0.000(2) C112 0.070(3) 0.080(4) 0.053(4) -0.008(3) 0.016(3) -0.015(3) C113 0.070(3) 0.046(3) 0.049(3) -0.003(3) 0.003(3) -0.013(3) C122 0.084(4) 0.060(3) 0.059(4) 0.006(3) 0.000(3) -0.015(3) C123 0.065(3) 0.064(4) 0.072(4) -0.007(3) -0.021(3) -0.007(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 N11 1.999(3) . ? Fe1 N21 2.003(3) . ? Fe1 Cl11 2.3190(13) . ? Fe1 Cl21 2.3331(13) . ? Fe1 Li1 3.145(8) . ? Cl11 Li1 2.356(9) . ? Cl21 Li1 2.369(9) . ? O1 C4S 1.398(7) . ? O1 C1S 1.408(8) . ? O1 Li1 1.925(9) . ? O2 C5S 1.414(6) . ? O2 C8S 1.421(6) . ? O2 Li1 1.878(9) . ? N11 C21 1.337(5) . ? N11 C12 1.439(5) . ? N21 C41 1.331(5) . ? N21 C13 1.434(5) . ? Fe2 N12 1.998(3) . ? Fe2 N22 2.001(3) . ? Fe2 Cl3 2.3214(12) . ? Fe2 Cl4 2.3210(13) . ? Fe2 Li2 3.151(8) . ? Cl3 Li2 2.365(9) . ? Cl4 Li2 2.376(9) . ? O3S C12S 1.395(7) . ? O3S C9S 1.426(7) . ? O3S Li2 1.915(10) . ? O4S C13S 1.318(9) . ? O4S C16S 1.405(9) . ? O4S Li2 1.887(10) . ? N12 C24 1.333(5) . ? N12 C15 1.430(5) . ? N22 C44 1.333(5) . ? N22 C16 1.436(5) . ? Fe3 N13 1.998(3) . ? Fe3 N23 2.014(3) . ? Fe3 Cl13 2.3237(13) . ? Fe3 Cl23 2.3258(13) . ? Fe3 Li3 3.112(8) . ? Cl13 Li3 2.341(8) . ? Cl23 Li3 2.326(10) . ? O5S C20S 1.355(6) . ? O5S C17S 1.384(8) . ? O5S Li3 1.895(9) . ? O6S C24S 1.425(8) . ? O6S C21S 1.444(7) . ? O6S Li3 1.975(10) . ? N13 C27 1.323(5) . ? N13 C18 1.443(5) . ? N23 C47 1.339(5) . ? N23 C19 1.435(5) . ? C17S C18S 1.394(8) . ? C18S C19S 1.473(8) . ? C19S C20S 1.496(8) . ? C21S C22S 1.444(10) . ? C22S C23S 1.301(10) . ? C23S C24S 1.477(10) . ? C17 C27 1.509(6) . ? C18 C68 1.391(6) . ? C18 C28 1.413(5) . ? C19 C69 1.404(6) . ? C19 C29 1.406(6) . ? C27 C37 1.414(6) . ? C28 C38 1.374(6) . ? C28 C78 1.529(6) . ? C29 C39 1.383(6) . ? C29 C79 1.528(6) . ? C37 C47 1.379(6) . ? C38 C48 1.374(6) . ? C39 C49 1.369(6) . ? C47 C57 1.511(6) . ? C48 C58 1.384(6) . ? C49 C59 1.371(6) . ? C58 C68 1.390(6) . ? C59 C69 1.406(6) . ? C68 C108 1.516(6) . ? C69 C109 1.490(6) . ? C78 C88 1.522(6) . ? C78 C98 1.523(6) . ? C79 C99 1.525(6) . ? C79 C89 1.527(6) . ? C108 C118 1.527(6) . ? C108 C128 1.531(6) . ? C109 C119 1.512(6) . ? C109 C129 1.546(6) . ? C9S C10S 1.473(10) . ? C10S C11S 1.453(11) . ? C11S C12S 1.429(11) . ? C13S C14S 1.482(16) . ? C14S C15S 1.422(18) . ? C15S C16S 1.320(12) . ? C14 C24 1.521(6) . ? C15 C25 1.409(6) . ? C15 C65 1.418(6) . ? C16 C26 1.399(6) . ? C16 C66 1.410(6) . ? C24 C34 1.389(6) . ? C25 C35 1.395(6) . ? C25 C75 1.505(6) . ? C26 C36 1.391(6) . ? C26 C76 1.503(6) . ? C34 C44 1.390(6) . ? C35 C45 1.353(7) . ? C36 C46 1.383(7) . ? C44 C54 1.517(6) . ? C45 C55 1.379(7) . ? C46 C56 1.357(7) . ? C55 C65 1.390(7) . ? C56 C66 1.385(6) . ? C65 C105 1.502(7) . ? C66 C106 1.517(7) . ? C75 C95 1.515(7) . ? C75 C85 1.534(6) . ? C76 C86 1.537(6) . ? C76 C96 1.545(6) . ? C105 C115 1.520(7) . ? C105 C125 1.547(6) . ? C106 C126 1.529(7) . ? C106 C116 1.532(7) . ? C1S C2S 1.481(10) . ? C2S C3S 1.430(11) . ? C3S C4S 1.484(10) . ? C5S C6S 1.416(7) . ? C6S C7S 1.484(8) . ? C7S C8S 1.499(8) . ? C11 C21 1.516(5) . ? C12 C62 1.397(5) . ? C12 C22 1.405(5) . ? C13 C23 1.402(5) . ? C13 C63 1.419(5) . ? C21 C31 1.400(6) . ? C22 C32 1.388(6) . ? C22 C72 1.546(6) . ? C23 C33 1.378(6) . ? C23 C73 1.521(6) . ? C31 C41 1.382(5) . ? C32 C42 1.380(6) . ? C33 C43 1.384(6) . ? C41 C51 1.520(5) . ? C42 C52 1.379(6) . ? C43 C53 1.360(6) . ? C52 C62 1.389(5) . ? C53 C63 1.387(5) . ? C62 C102 1.505(6) . ? C63 C103 1.510(5) . ? C72 C82 1.523(6) . ? C72 C92 1.544(6) . ? C73 C83 1.521(6) . ? C73 C93 1.530(6) . ? C102 C112 1.535(6) . ? C102 C122 1.535(6) . ? C103 C113 1.526(6) . ? C103 C123 1.546(6) . ? 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 N11 Fe1 N21 93.16(13) . . ? N11 Fe1 Cl11 118.02(10) . . ? N21 Fe1 Cl11 115.59(10) . . ? N11 Fe1 Cl21 114.81(10) . . ? N21 Fe1 Cl21 120.44(10) . . ? Cl11 Fe1 Cl21 96.61(5) . . ? N11 Fe1 Li1 134.71(18) . . ? N21 Fe1 Li1 132.12(18) . . ? Cl11 Fe1 Li1 48.23(18) . . ? Cl21 Fe1 Li1 48.50(18) . . ? Fe1 Cl11 Li1 84.6(2) . . ? Fe1 Cl21 Li1 84.0(2) . . ? C4S O1 C1S 107.1(5) . . ? C4S O1 Li1 129.5(5) . . ? C1S O1 Li1 116.2(5) . . ? C5S O2 C8S 108.6(4) . . ? C5S O2 Li1 119.0(4) . . ? C8S O2 Li1 125.4(4) . . ? C21 N11 C12 121.3(3) . . ? C21 N11 Fe1 124.2(3) . . ? C12 N11 Fe1 114.4(2) . . ? C41 N21 C13 121.5(3) . . ? C41 N21 Fe1 124.0(3) . . ? C13 N21 Fe1 114.5(2) . . ? O2 Li1 O1 112.7(4) . . ? O2 Li1 Cl11 113.0(4) . . ? O1 Li1 Cl11 116.4(4) . . ? O2 Li1 Cl21 110.1(4) . . ? O1 Li1 Cl21 108.4(4) . . ? Cl11 Li1 Cl21 94.6(3) . . ? O2 Li1 Fe1 120.1(4) . . ? O1 Li1 Fe1 126.7(4) . . ? Cl11 Li1 Fe1 47.22(15) . . ? Cl21 Li1 Fe1 47.53(15) . . ? N12 Fe2 N22 93.54(14) . . ? N12 Fe2 Cl3 116.69(11) . . ? N22 Fe2 Cl3 117.95(10) . . ? N12 Fe2 Cl4 117.75(10) . . ? N22 Fe2 Cl4 116.58(10) . . ? Cl3 Fe2 Cl4 96.14(5) . . ? N12 Fe2 Li2 126.0(2) . . ? N22 Fe2 Li2 140.5(2) . . ? Cl3 Fe2 Li2 48.35(18) . . ? Cl4 Fe2 Li2 48.61(17) . . ? Fe2 Cl3 Li2 84.5(2) . . ? Fe2 Cl4 Li2 84.3(2) . . ? C12S O3S C9S 109.7(5) . . ? C12S O3S Li2 129.1(5) . . ? C9S O3S Li2 121.2(5) . . ? C13S O4S C16S 105.4(7) . . ? C13S O4S Li2 133.0(7) . . ? C16S O4S Li2 118.7(6) . . ? C24 N12 C15 118.8(4) . . ? C24 N12 Fe2 123.5(3) . . ? C15 N12 Fe2 117.6(2) . . ? C44 N22 C16 120.3(4) . . ? C44 N22 Fe2 124.0(3) . . ? C16 N22 Fe2 115.6(2) . . ? O4S Li2 O3S 113.3(5) . . ? O4S Li2 Cl3 111.8(5) . . ? O3S Li2 Cl3 109.7(4) . . ? O4S Li2 Cl4 109.7(5) . . ? O3S Li2 Cl4 117.3(5) . . ? Cl3 Li2 Cl4 93.5(3) . . ? O4S Li2 Fe2 128.0(4) . . ? O3S Li2 Fe2 118.6(4) . . ? Cl3 Li2 Fe2 47.16(15) . . ? Cl4 Li2 Fe2 47.13(15) . . ? N13 Fe3 N23 93.38(14) . . ? N13 Fe3 Cl13 111.75(10) . . ? N23 Fe3 Cl13 121.51(10) . . ? N13 Fe3 Cl23 121.73(11) . . ? N23 Fe3 Cl23 114.19(10) . . ? Cl13 Fe3 Cl23 96.36(5) . . ? N13 Fe3 Li3 133.77(19) . . ? N23 Fe3 Li3 132.83(19) . . ? Cl13 Fe3 Li3 48.38(17) . . ? Cl23 Fe3 Li3 48.02(18) . . ? Fe3 Cl13 Li3 83.7(2) . . ? Fe3 Cl23 Li3 84.0(2) . . ? C20S O5S C17S 105.9(5) . . ? C20S O5S Li3 128.2(5) . . ? C17S O5S Li3 123.9(5) . . ? C24S O6S C21S 106.7(5) . . ? C24S O6S Li3 118.3(5) . . ? C21S O6S Li3 118.9(5) . . ? C27 N13 C18 120.4(4) . . ? C27 N13 Fe3 124.5(3) . . ? C18 N13 Fe3 115.1(3) . . ? C47 N23 C19 120.0(3) . . ? C47 N23 Fe3 123.0(3) . . ? C19 N23 Fe3 116.8(2) . . ? O5S Li3 O6S 112.9(5) . . ? O5S Li3 Cl23 117.5(5) . . ? O6S Li3 Cl23 115.7(4) . . ? O5S Li3 Cl13 109.4(4) . . ? O6S Li3 Cl13 102.6(4) . . ? Cl23 Li3 Cl13 95.9(3) . . ? O5S Li3 Fe3 127.8(4) . . ? O6S Li3 Fe3 117.6(4) . . ? Cl23 Li3 Fe3 48.00(16) . . ? Cl13 Li3 Fe3 47.91(15) . . ? O5S C17S C18S 113.5(7) . . ? C17S C18S C19S 103.7(6) . . ? C18S C19S C20S 104.2(6) . . ? O5S C20S C19S 107.6(5) . . ? C22S C21S O6S 105.9(7) . . ? C23S C22S C21S 111.3(10) . . ? C22S C23S C24S 108.3(8) . . ? O6S C24S C23S 106.1(6) . . ? C68 C18 C28 120.3(4) . . ? C68 C18 N13 120.6(4) . . ? C28 C18 N13 118.7(4) . . ? C69 C19 C29 121.4(4) . . ? C69 C19 N23 120.8(4) . . ? C29 C19 N23 117.8(4) . . ? N13 C27 C37 122.1(4) . . ? N13 C27 C17 121.5(4) . . ? C37 C27 C17 116.3(4) . . ? C38 C28 C18 119.5(4) . . ? C38 C28 C78 119.5(4) . . ? C18 C28 C78 120.9(4) . . ? C39 C29 C19 117.9(4) . . ? C39 C29 C79 119.9(4) . . ? C19 C29 C79 122.2(4) . . ? C47 C37 C27 130.2(4) . . ? C28 C38 C48 120.2(5) . . ? C49 C39 C29 121.7(5) . . ? N23 C47 C37 123.7(4) . . ? N23 C47 C57 118.9(4) . . ? C37 C47 C57 117.4(4) . . ? C38 C48 C58 120.6(5) . . ? C39 C49 C59 120.7(5) . . ? C48 C58 C68 120.6(5) . . ? C49 C59 C69 120.5(5) . . ? C18 C68 C58 118.7(4) . . ? C18 C68 C108 123.5(4) . . ? C58 C68 C108 117.8(4) . . ? C19 C69 C59 117.8(4) . . ? C19 C69 C109 123.7(4) . . ? C59 C69 C109 118.4(4) . . ? C88 C78 C98 109.1(4) . . ? C88 C78 C28 113.4(4) . . ? C98 C78 C28 112.2(4) . . ? C99 C79 C89 110.7(4) . . ? C99 C79 C29 111.1(4) . . ? C89 C79 C29 113.5(4) . . ? C68 C108 C118 112.2(4) . . ? C68 C108 C128 112.0(4) . . ? C118 C108 C128 109.9(4) . . ? C69 C109 C119 112.6(4) . . ? C69 C109 C129 111.4(4) . . ? C119 C109 C129 109.0(4) . . ? O3S C9S C10S 105.6(7) . . ? C11S C10S C9S 105.7(8) . . ? C12S C11S C10S 108.2(8) . . ? O3S C12S C11S 107.7(8) . . ? O4S C13S C14S 110.1(10) . . ? C15S C14S C13S 103.2(9) . . ? C16S C15S C14S 107.4(13) . . ? C15S C16S O4S 113.1(11) . . ? C25 C15 C65 120.7(4) . . ? C25 C15 N12 120.5(4) . . ? C65 C15 N12 118.7(4) . . ? C26 C16 C66 121.0(4) . . ? C26 C16 N22 120.9(4) . . ? C66 C16 N22 117.8(4) . . ? N12 C24 C34 123.2(4) . . ? N12 C24 C14 119.6(4) . . ? C34 C24 C14 117.2(4) . . ? C35 C25 C15 117.6(5) . . ? C35 C25 C75 119.1(5) . . ? C15 C25 C75 123.3(4) . . ? C36 C26 C16 117.9(5) . . ? C36 C26 C76 118.5(5) . . ? C16 C26 C76 123.5(4) . . ? C24 C34 C44 130.7(4) . . ? C45 C35 C25 122.7(5) . . ? C46 C36 C26 121.1(5) . . ? N22 C44 C34 122.5(4) . . ? N22 C44 C54 120.2(4) . . ? C34 C44 C54 117.3(4) . . ? C35 C45 C55 119.2(6) . . ? C56 C46 C36 120.3(5) . . ? C45 C55 C65 122.3(5) . . ? C46 C56 C66 121.4(5) . . ? C55 C65 C15 117.4(5) . . ? C55 C65 C105 121.7(5) . . ? C15 C65 C105 120.8(5) . . ? C56 C66 C16 118.2(5) . . ? C56 C66 C106 121.1(5) . . ? C16 C66 C106 120.6(4) . . ? C25 C75 C95 111.9(4) . . ? C25 C75 C85 111.9(4) . . ? C95 C75 C85 108.9(4) . . ? C26 C76 C86 112.4(4) . . ? C26 C76 C96 112.3(4) . . ? C86 C76 C96 109.3(4) . . ? C65 C105 C115 112.9(5) . . ? C65 C105 C125 112.4(5) . . ? C115 C105 C125 109.4(4) . . ? C66 C106 C126 111.8(4) . . ? C66 C106 C116 113.8(5) . . ? C126 C106 C116 109.0(4) . . ? O1 C1S C2S 105.1(7) . . ? C3S C2S C1S 104.6(8) . . ? C2S C3S C4S 106.3(8) . . ? O1 C4S C3S 107.0(7) . . ? C6S C5S O2 109.0(5) . . ? C5S C6S C7S 104.7(6) . . ? C6S C7S C8S 105.9(5) . . ? O2 C8S C7S 106.0(5) . . ? C62 C12 C22 121.3(4) . . ? C62 C12 N11 120.7(4) . . ? C22 C12 N11 117.9(4) . . ? C23 C13 C63 121.3(4) . . ? C23 C13 N21 118.2(4) . . ? C63 C13 N21 120.4(4) . . ? N11 C21 C31 123.2(4) . . ? N11 C21 C11 120.3(4) . . ? C31 C21 C11 116.4(4) . . ? C32 C22 C12 118.6(4) . . ? C32 C22 C72 120.1(4) . . ? C12 C22 C72 121.4(4) . . ? C33 C23 C13 118.5(4) . . ? C33 C23 C73 121.3(4) . . ? C13 C23 C73 120.2(4) . . ? C41 C31 C21 129.6(4) . . ? C42 C32 C22 120.7(4) . . ? C23 C33 C43 121.0(5) . . ? N21 C41 C31 123.9(4) . . ? N21 C41 C51 120.6(4) . . ? C31 C41 C51 115.5(4) . . ? C32 C42 C52 119.9(4) . . ? C53 C43 C33 119.9(5) . . ? C42 C52 C62 121.5(4) . . ? C43 C53 C63 122.4(4) . . ? C52 C62 C12 117.9(4) . . ? C52 C62 C102 119.3(4) . . ? C12 C62 C102 122.8(4) . . ? C53 C63 C13 116.8(4) . . ? C53 C63 C103 120.0(4) . . ? C13 C63 C103 123.1(4) . . ? C82 C72 C92 110.0(4) . . ? C82 C72 C22 112.7(4) . . ? C92 C72 C22 111.2(4) . . ? C23 C73 C83 113.5(4) . . ? C23 C73 C93 111.4(4) . . ? C83 C73 C93 110.0(4) . . ? C62 C102 C112 111.7(4) . . ? C62 C102 C122 112.7(4) . . ? C112 C102 C122 109.0(4) . . ? C63 C103 C113 111.7(3) . . ? C63 C103 C123 111.8(4) . . ? C113 C103 C123 108.9(4) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.251 _refine_diff_density_min -0.211 _refine_diff_density_rms 0.040 data_sad _database_code_CSD 167178 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H60 Cl2 Fe Li N2 O2' _chemical_formula_weight 698.56 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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)/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 12.0855(12) _cell_length_b 21.241(2) _cell_length_c 15.8835(15) _cell_angle_alpha 90.00 _cell_angle_beta 99.674(2) _cell_angle_gamma 90.00 _cell_volume 4019.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5231 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description glob _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas na _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.735 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23267 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9265 _reflns_number_gt 5231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^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 9265 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0589 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1245 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 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 0.76171(3) 0.238025(19) 0.99014(3) 0.03381(13) Uani 1 1 d . . . Cl11 Cl 0.61968(6) 0.25766(4) 1.07056(5) 0.0471(2) Uani 1 1 d . . . Cl21 Cl 0.64667(7) 0.24483(4) 0.85763(5) 0.0572(2) Uani 1 1 d . . . N11 N 0.85321(18) 0.15904(10) 1.01028(14) 0.0322(5) Uani 1 1 d . . . N21 N 0.89624(18) 0.29403(10) 1.02081(15) 0.0337(5) Uani 1 1 d . . . Li11 Li 0.5077(4) 0.2816(2) 0.9362(3) 0.0462(13) Uani 1 1 d . . . C11 C 1.0157(3) 0.09441(14) 1.0736(2) 0.0498(8) Uani 1 1 d . . . H11A H 0.9648 0.0602 1.0510 0.075 Uiso 1 1 calc R . . H11B H 1.0371 0.0896 1.1355 0.075 Uiso 1 1 calc R . . H11C H 1.0831 0.0929 1.0468 0.075 Uiso 1 1 calc R . . C21 C 0.9573(2) 0.15693(13) 1.05401(18) 0.0351(7) Uani 1 1 d . . . C31 C 1.0186(2) 0.21043(14) 1.08215(18) 0.0376(7) Uani 1 1 d . . . H31 H 1.0870 0.2029 1.1199 0.045 Uiso 1 1 calc R . . C41 C 0.9943(2) 0.27387(14) 1.06294(19) 0.0381(7) Uani 1 1 d . . . C51 C 1.0892(3) 0.31943(15) 1.0929(2) 0.0580(10) Uani 1 1 d . . . H51A H 1.0645 0.3624 1.0772 0.087 Uiso 1 1 calc R . . H51B H 1.1538 0.3089 1.0657 0.087 Uiso 1 1 calc R . . H51C H 1.1106 0.3165 1.1551 0.087 Uiso 1 1 calc R . . C12 C 0.8862(2) 0.35902(13) 0.9932(2) 0.0388(7) Uani 1 1 d . . . C22 C 0.8954(2) 0.37245(14) 0.9081(2) 0.0446(8) Uani 1 1 d . . . C32 C 0.8841(3) 0.43494(16) 0.8812(2) 0.0533(9) Uani 1 1 d . . . H32 H 0.8911 0.4448 0.8240 0.064 Uiso 1 1 calc R . . C42 C 0.8633(3) 0.48217(16) 0.9343(2) 0.0581(10) Uani 1 1 d . . . H42 H 0.8569 0.5244 0.9142 0.070 Uiso 1 1 calc R . . C52 C 0.8515(3) 0.46862(15) 1.0173(2) 0.0509(9) Uani 1 1 d . . . H52 H 0.8361 0.5017 1.0538 0.061 Uiso 1 1 calc R . . C62 C 0.8619(2) 0.40689(14) 1.0486(2) 0.0417(7) Uani 1 1 d . . . C72 C 0.9223(3) 0.32149(16) 0.8470(2) 0.0570(9) Uani 1 1 d . . . H72 H 0.8966 0.2805 0.8680 0.068 Uiso 1 1 calc R . . C82 C 1.0485(4) 0.3162(2) 0.8486(3) 0.1003(16) Uani 1 1 d . . . H82A H 1.0867 0.3105 0.9076 0.150 Uiso 1 1 calc R . . H82B H 1.0760 0.3547 0.8250 0.150 Uiso 1 1 calc R . . H82C H 1.0640 0.2800 0.8142 0.150 Uiso 1 1 calc R . . C92 C 0.8609(4) 0.33028(19) 0.7558(2) 0.0782(12) Uani 1 1 d . . . H92A H 0.7800 0.3331 0.7558 0.117 Uiso 1 1 calc R . . H92B H 0.8764 0.2943 0.7209 0.117 Uiso 1 1 calc R . . H92C H 0.8869 0.3691 0.7320 0.117 Uiso 1 1 calc R . . C102 C 0.8467(3) 0.39467(14) 1.1398(2) 0.0473(8) Uani 1 1 d . . . H102 H 0.8595 0.3488 1.1515 0.057 Uiso 1 1 calc R . . C112 C 0.9329(3) 0.43181(17) 1.2050(2) 0.0674(11) Uani 1 1 d . . . H11D H 1.0092 0.4216 1.1961 0.101 Uiso 1 1 calc R . . H11E H 0.9241 0.4201 1.2632 0.101 Uiso 1 1 calc R . . H11F H 0.9197 0.4771 1.1968 0.101 Uiso 1 1 calc R . . C122 C 0.7270(3) 0.41036(16) 1.1530(2) 0.0621(10) Uani 1 1 d . . . H12A H 0.6732 0.3867 1.1119 0.093 Uiso 1 1 calc R . . H12B H 0.7135 0.4556 1.1445 0.093 Uiso 1 1 calc R . . H12C H 0.7179 0.3988 1.2112 0.093 Uiso 1 1 calc R . . C103 C 0.7110(3) 0.08215(15) 1.1023(2) 0.0484(8) Uani 1 1 d . . . H103 H 0.7453 0.1243 1.1177 0.058 Uiso 1 1 calc R . . C13 C 0.8021(2) 0.10240(13) 0.97121(18) 0.0366(7) Uani 1 1 d . . . C23 C 0.8210(3) 0.08681(14) 0.8886(2) 0.0445(8) Uani 1 1 d . . . C33 C 0.7670(3) 0.03345(17) 0.8499(2) 0.0607(10) Uani 1 1 d . . . H33 H 0.7787 0.0218 0.7943 0.073 Uiso 1 1 calc R . . C43 C 0.6974(3) -0.00264(18) 0.8904(3) 0.0705(11) Uani 1 1 d . . . H43 H 0.6612 -0.0386 0.8627 0.085 Uiso 1 1 calc R . . C53 C 0.6804(3) 0.01361(16) 0.9716(2) 0.0595(10) Uani 1 1 d . . . H53 H 0.6327 -0.0118 0.9994 0.071 Uiso 1 1 calc R . . C63 C 0.7313(3) 0.06607(14) 1.0136(2) 0.0424(7) Uani 1 1 d . . . C73 C 0.8961(3) 0.12506(16) 0.8414(2) 0.0556(9) Uani 1 1 d . . . H73 H 0.9163 0.1645 0.8748 0.067 Uiso 1 1 calc R . . C83 C 1.0054(3) 0.0902(2) 0.8355(3) 0.0802(13) Uani 1 1 d . . . H83A H 1.0422 0.0779 0.8929 0.120 Uiso 1 1 calc R . . H83B H 1.0553 0.1179 0.8097 0.120 Uiso 1 1 calc R . . H83C H 0.9887 0.0525 0.8001 0.120 Uiso 1 1 calc R . . C93 C 0.8408(4) 0.1440(2) 0.7526(2) 0.0869(14) Uani 1 1 d . . . H93A H 0.7717 0.1674 0.7558 0.130 Uiso 1 1 calc R . . H93B H 0.8227 0.1062 0.7176 0.130 Uiso 1 1 calc R . . H93C H 0.8921 0.1707 0.7268 0.130 Uiso 1 1 calc R . . C113 C 0.7657(4) 0.0350(2) 1.1684(3) 0.0861(13) Uani 1 1 d . . . H11G H 0.8463 0.0325 1.1666 0.129 Uiso 1 1 calc R . . H11H H 0.7315 -0.0065 1.1559 0.129 Uiso 1 1 calc R . . H11I H 0.7547 0.0486 1.2254 0.129 Uiso 1 1 calc R . . C123 C 0.5870(3) 0.08613(18) 1.1081(3) 0.0739(12) Uani 1 1 d . . . H12D H 0.5500 0.1159 1.0653 0.111 Uiso 1 1 calc R . . H12E H 0.5783 0.1005 1.1652 0.111 Uiso 1 1 calc R . . H12F H 0.5526 0.0445 1.0974 0.111 Uiso 1 1 calc R . . O21 O 0.49143(18) 0.37246(10) 0.92962(14) 0.0535(6) Uani 1 1 d . . . C2S C 0.3324(4) 0.22947(19) 0.8061(3) 0.0821(14) Uani 1 1 d . . . H2SA H 0.2528 0.2162 0.7938 0.099 Uiso 1 1 calc R . . H2SB H 0.3781 0.1961 0.7850 0.099 Uiso 1 1 calc R . . C7S C 0.5818(3) 0.40973(18) 0.9099(3) 0.0717(11) Uani 1 1 d . . . H7SA H 0.6483 0.3824 0.9105 0.086 Uiso 1 1 calc R . . H7SB H 0.6014 0.4419 0.9550 0.086 Uiso 1 1 calc R . . C1S C 0.3458(3) 0.2882(2) 0.7610(2) 0.0741(12) Uani 1 1 d . . . H1SA H 0.3210 0.2821 0.6995 0.111 Uiso 1 1 calc R . . H1SB H 0.4250 0.3007 0.7715 0.111 Uiso 1 1 calc R . . H1SC H 0.3005 0.3213 0.7816 0.111 Uiso 1 1 calc R . . C8S C 0.5569(4) 0.4411(3) 0.8277(3) 0.122(2) Uani 1 1 d . . . H8SA H 0.6219 0.4661 0.8184 0.183 Uiso 1 1 calc R . . H8SB H 0.4919 0.4688 0.8268 0.183 Uiso 1 1 calc R . . H8SC H 0.5401 0.4095 0.7823 0.183 Uiso 1 1 calc R . . C3S C 0.3447(5) 0.1779(3) 0.9380(3) 0.1181(19) Uani 1 1 d . . . H3SA H 0.2858 0.1539 0.9004 0.142 Uiso 1 1 calc R . . H3SB H 0.4139 0.1521 0.9469 0.142 Uiso 1 1 calc R . . C6S C 0.4082(5) 0.4076(2) 0.9599(4) 0.132(2) Uani 1 1 d . . . H6SA H 0.3899 0.4490 0.9392 0.158 Uiso 1 1 calc R . . C4S C 0.3118(6) 0.1876(3) 1.0137(4) 0.161(3) Uani 1 1 d . . . H4SA H 0.2985 0.1470 1.0395 0.242 Uiso 1 1 calc R . . H4SB H 0.2424 0.2124 1.0052 0.242 Uiso 1 1 calc R . . H4SC H 0.3706 0.2105 1.0516 0.242 Uiso 1 1 calc R . . C5S C 0.3562(5) 0.3821(3) 1.0173(4) 0.152(3) Uani 1 1 d . . . H5SA H 0.2994 0.4113 1.0314 0.228 Uiso 1 1 calc R . . H5SB H 0.4105 0.3728 1.0689 0.228 Uiso 1 1 calc R . . H5SC H 0.3198 0.3430 0.9946 0.228 Uiso 1 1 calc R . . O11 O 0.36602(19) 0.23645(10) 0.89569(15) 0.0537(6) 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 0.0278(2) 0.0334(2) 0.0388(2) 0.0018(2) 0.00146(17) 0.00194(18) Cl11 0.0378(4) 0.0609(5) 0.0427(4) 0.0015(4) 0.0073(3) 0.0050(4) Cl21 0.0447(5) 0.0854(7) 0.0390(4) -0.0049(4) -0.0006(4) 0.0179(4) N11 0.0293(13) 0.0325(13) 0.0342(13) 0.0007(10) 0.0039(10) 0.0007(10) N21 0.0304(13) 0.0325(13) 0.0378(14) 0.0026(11) 0.0046(11) 0.0008(10) Li11 0.040(3) 0.044(3) 0.052(3) 0.005(2) 0.003(2) 0.004(2) C11 0.0420(19) 0.0463(19) 0.057(2) 0.0046(16) -0.0031(16) 0.0114(15) C21 0.0349(17) 0.0387(17) 0.0323(16) 0.0055(13) 0.0072(13) 0.0036(13) C31 0.0283(16) 0.0442(18) 0.0380(17) 0.0014(14) -0.0011(13) 0.0014(13) C41 0.0306(16) 0.0451(19) 0.0383(17) -0.0015(14) 0.0051(13) -0.0052(13) C51 0.0374(19) 0.054(2) 0.080(3) -0.0041(19) 0.0002(18) -0.0083(16) C12 0.0283(16) 0.0345(17) 0.053(2) 0.0057(15) 0.0062(14) -0.0062(13) C22 0.0371(18) 0.0430(19) 0.054(2) 0.0104(16) 0.0089(15) -0.0031(14) C32 0.053(2) 0.048(2) 0.061(2) 0.0157(18) 0.0129(18) -0.0114(16) C42 0.057(2) 0.0360(19) 0.081(3) 0.0172(19) 0.011(2) -0.0067(16) C52 0.046(2) 0.0357(18) 0.071(2) -0.0014(17) 0.0110(17) -0.0076(15) C62 0.0327(17) 0.0383(17) 0.053(2) 0.0030(15) 0.0051(15) -0.0040(14) C72 0.072(2) 0.055(2) 0.048(2) 0.0106(17) 0.0205(19) 0.0000(19) C82 0.083(3) 0.128(4) 0.098(4) 0.000(3) 0.042(3) 0.026(3) C92 0.105(3) 0.080(3) 0.052(2) 0.007(2) 0.019(2) 0.002(3) C102 0.051(2) 0.0364(17) 0.056(2) -0.0041(16) 0.0126(16) -0.0042(15) C112 0.073(3) 0.069(2) 0.060(2) -0.012(2) 0.009(2) -0.009(2) C122 0.067(2) 0.051(2) 0.073(3) -0.0065(19) 0.026(2) -0.0025(18) C103 0.051(2) 0.0466(19) 0.050(2) 0.0015(16) 0.0138(16) -0.0115(16) C13 0.0366(17) 0.0321(16) 0.0387(17) -0.0029(13) -0.0006(13) 0.0050(13) C23 0.0469(19) 0.0398(18) 0.0459(19) -0.0045(15) 0.0051(15) 0.0073(15) C33 0.063(2) 0.062(2) 0.058(2) -0.0218(19) 0.0127(19) 0.004(2) C43 0.070(3) 0.059(2) 0.082(3) -0.028(2) 0.009(2) -0.014(2) C53 0.054(2) 0.049(2) 0.076(3) -0.0078(19) 0.0126(19) -0.0147(17) C63 0.0385(17) 0.0359(17) 0.0512(19) -0.0033(15) 0.0025(14) -0.0016(14) C73 0.073(2) 0.052(2) 0.046(2) -0.0099(17) 0.0205(18) 0.0031(18) C83 0.062(3) 0.107(3) 0.077(3) 0.012(3) 0.027(2) 0.006(2) C93 0.096(3) 0.109(4) 0.060(3) 0.021(2) 0.026(2) 0.034(3) C113 0.078(3) 0.115(4) 0.065(3) 0.025(3) 0.011(2) 0.017(3) C123 0.058(2) 0.084(3) 0.083(3) -0.004(2) 0.021(2) 0.005(2) O21 0.0533(14) 0.0482(13) 0.0623(15) 0.0081(11) 0.0194(12) 0.0090(11) C2S 0.095(3) 0.069(3) 0.069(3) -0.005(2) -0.025(2) -0.010(2) C7S 0.062(3) 0.060(2) 0.088(3) 0.010(2) -0.003(2) -0.005(2) C1S 0.068(3) 0.100(3) 0.049(2) 0.011(2) -0.006(2) -0.002(2) C8S 0.082(3) 0.168(5) 0.111(4) 0.076(4) 0.005(3) -0.038(3) C3S 0.142(5) 0.122(5) 0.088(4) 0.025(3) 0.012(4) -0.030(4) C6S 0.156(5) 0.086(3) 0.185(6) 0.046(4) 0.122(5) 0.071(4) C4S 0.182(7) 0.168(7) 0.160(6) 0.078(5) 0.103(5) 0.045(5) C5S 0.170(6) 0.143(5) 0.177(6) 0.074(5) 0.130(5) 0.090(5) O11 0.0559(14) 0.0519(13) 0.0533(15) 0.0071(12) 0.0094(11) -0.0085(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N11 2.005(2) . ? Fe1 N21 2.007(2) . ? Fe1 Cl21 2.3238(9) . ? Fe1 Cl11 2.3428(9) . ? Fe1 Li11 3.182(5) . ? Cl11 Li11 2.382(5) . ? Cl21 Li11 2.386(6) . ? N11 C21 1.332(3) . ? N11 C13 1.444(3) . ? N21 C41 1.330(3) . ? N21 C12 1.447(3) . ? Li11 O21 1.941(5) . ? Li11 O11 1.974(6) . ? C11 C21 1.511(4) . ? C21 C31 1.389(4) . ? C31 C41 1.402(4) . ? C41 C51 1.515(4) . ? C12 C22 1.404(4) . ? C12 C62 1.408(4) . ? C22 C32 1.394(4) . ? C22 C72 1.525(4) . ? C32 C42 1.361(5) . ? C42 C52 1.380(5) . ? C52 C62 1.401(4) . ? C62 C102 1.512(4) . ? C72 C92 1.525(5) . ? C72 C82 1.526(5) . ? C102 C122 1.533(4) . ? C102 C112 1.555(4) . ? C103 C63 1.508(4) . ? C103 C113 1.520(5) . ? C103 C123 1.520(5) . ? C13 C63 1.406(4) . ? C13 C23 1.409(4) . ? C23 C33 1.397(4) . ? C23 C73 1.508(5) . ? C33 C43 1.375(5) . ? C43 C53 1.384(5) . ? C53 C63 1.388(4) . ? C73 C93 1.511(5) . ? C73 C83 1.532(5) . ? O21 C6S 1.401(5) . ? O21 C7S 1.426(4) . ? C2S O11 1.421(4) . ? C2S C1S 1.462(5) . ? C7S C8S 1.452(5) . ? C3S C4S 1.344(7) . ? C3S O11 1.457(5) . ? C6S C5S 1.309(6) . ? 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 N11 Fe1 N21 93.13(9) . . ? N11 Fe1 Cl21 115.24(7) . . ? N21 Fe1 Cl21 121.32(7) . . ? N11 Fe1 Cl11 119.79(7) . . ? N21 Fe1 Cl11 113.57(7) . . ? Cl21 Fe1 Cl11 95.80(3) . . ? N11 Fe1 Li11 140.11(12) . . ? N21 Fe1 Li11 126.75(12) . . ? Cl21 Fe1 Li11 48.31(10) . . ? Cl11 Fe1 Li11 48.17(10) . . ? Fe1 Cl11 Li11 84.69(13) . . ? Fe1 Cl21 Li11 85.01(13) . . ? C21 N11 C13 119.6(2) . . ? C21 N11 Fe1 123.97(19) . . ? C13 N11 Fe1 116.35(17) . . ? C41 N21 C12 118.8(2) . . ? C41 N21 Fe1 123.24(19) . . ? C12 N21 Fe1 117.95(17) . . ? O21 Li11 O11 113.0(3) . . ? O21 Li11 Cl11 107.3(2) . . ? O11 Li11 Cl11 121.3(3) . . ? O21 Li11 Cl21 111.8(3) . . ? O11 Li11 Cl21 108.6(2) . . ? Cl11 Li11 Cl21 93.16(18) . . ? O21 Li11 Fe1 112.8(2) . . ? O11 Li11 Fe1 133.7(2) . . ? Cl11 Li11 Fe1 47.14(9) . . ? Cl21 Li11 Fe1 46.68(9) . . ? N11 C21 C31 123.1(3) . . ? N11 C21 C11 120.3(3) . . ? C31 C21 C11 116.6(3) . . ? C21 C31 C41 129.4(3) . . ? N21 C41 C31 123.7(3) . . ? N21 C41 C51 121.1(3) . . ? C31 C41 C51 115.2(3) . . ? C22 C12 C62 120.9(3) . . ? C22 C12 N21 118.0(3) . . ? C62 C12 N21 121.0(3) . . ? C32 C22 C12 118.0(3) . . ? C32 C22 C72 120.1(3) . . ? C12 C22 C72 121.9(3) . . ? C42 C32 C22 122.1(3) . . ? C32 C42 C52 119.8(3) . . ? C42 C52 C62 121.2(3) . . ? C52 C62 C12 118.0(3) . . ? C52 C62 C102 118.9(3) . . ? C12 C62 C102 123.1(3) . . ? C92 C72 C22 113.4(3) . . ? C92 C72 C82 110.5(3) . . ? C22 C72 C82 111.2(3) . . ? C62 C102 C122 111.3(3) . . ? C62 C102 C112 112.0(3) . . ? C122 C102 C112 109.9(3) . . ? C63 C103 C113 112.1(3) . . ? C63 C103 C123 112.7(3) . . ? C113 C103 C123 108.3(3) . . ? C63 C13 C23 121.6(3) . . ? C63 C13 N11 120.2(3) . . ? C23 C13 N11 118.1(3) . . ? C33 C23 C13 117.6(3) . . ? C33 C23 C73 119.6(3) . . ? C13 C23 C73 122.8(3) . . ? C43 C33 C23 121.6(3) . . ? C33 C43 C53 119.7(3) . . ? C43 C53 C63 121.7(3) . . ? C53 C63 C13 117.8(3) . . ? C53 C63 C103 120.2(3) . . ? C13 C63 C103 122.0(3) . . ? C23 C73 C93 113.5(3) . . ? C23 C73 C83 111.6(3) . . ? C93 C73 C83 108.8(3) . . ? C6S O21 C7S 113.6(3) . . ? C6S O21 Li11 125.7(3) . . ? C7S O21 Li11 119.3(3) . . ? O11 C2S C1S 111.4(3) . . ? O21 C7S C8S 113.7(3) . . ? C4S C3S O11 112.5(5) . . ? C5S C6S O21 118.3(4) . . ? C2S O11 C3S 109.3(3) . . ? C2S O11 Li11 117.6(3) . . ? C3S O11 Li11 118.4(3) . . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.470 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.053 data_js05a _database_code_CSD 167179 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 302-304 _chemical_formula_moiety ? _chemical_formula_sum 'C41 H65 Cl2 Fe Mg0.50 N2 O3' _chemical_formula_weight 772.86 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' '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' 'Mg' 'Mg' 0.0486 0.0363 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _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 12.6469(8) _cell_length_b 13.0103(8) _cell_length_c 26.4143(17) _cell_angle_alpha 90.00 _cell_angle_beta 102.8530(10) _cell_angle_gamma 90.00 _cell_volume 4237.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4610 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.211 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1660 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.290 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(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 SMART CCD _diffrn_measurement_method SMART CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18679 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 23.25 _reflns_number_total 6069 _reflns_number_gt 4610 _reflns_threshold_expression >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SAINT _computing_data_reduction SAINT _computing_structure_solution SIR-92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP32 _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^)+(0.0770P)^2^+3.4468P] 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 6069 _refine_ls_number_parameters 443 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1454 _refine_ls_wR_factor_gt 0.1361 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.061 _refine_ls_shift/su_mean 0.002 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 0.25557(4) 0.17801(4) 0.87874(2) 0.03215(18) Uani 1 1 d . . . Cl1 Cl 0.38553(8) 0.04929(7) 0.91259(4) 0.0364(3) Uani 1 1 d . . . Cl2 Cl 0.22713(11) 0.26623(9) 0.94855(4) 0.0571(3) Uani 1 1 d . . . O1 O 0.4207(2) 0.10175(19) 1.03972(10) 0.0335(6) Uani 1 1 d . . . O2 O 0.6121(2) 0.11940(19) 0.99346(9) 0.0324(6) Uani 1 1 d . . . N11 N 0.1262(2) 0.1146(2) 0.83042(12) 0.0287(7) Uani 1 1 d . . . N21 N 0.2903(2) 0.2651(2) 0.82167(11) 0.0268(7) Uani 1 1 d . . . Mg1 Mg 0.5000 0.0000 1.0000 0.0271(4) Uani 1 2 d S . . C1S C 0.3211(5) 0.0808(4) 1.0548(3) 0.0737(18) Uani 1 1 d . . . H1SA H 0.3243 0.0135 1.0726 0.088 Uiso 1 1 calc R . . H1SB H 0.2595 0.0803 1.0242 0.088 Uiso 1 1 calc R . . C2S C 0.3096(7) 0.1668(5) 1.0911(4) 0.144(4) Uani 1 1 d . . . H2SA H 0.2343 0.1932 1.0828 0.173 Uiso 1 1 calc R . . H2SB H 0.3260 0.1416 1.1274 0.173 Uiso 1 1 calc R . . C3S C 0.3812(5) 0.2451(5) 1.0857(3) 0.096(2) Uani 1 1 d . . . H3SA H 0.4173 0.2728 1.1201 0.115 Uiso 1 1 calc R . . H3SB H 0.3422 0.3017 1.0644 0.115 Uiso 1 1 calc R . . C4S C 0.4595(4) 0.1997(5) 1.0605(3) 0.095(2) Uani 1 1 d . . . H4SA H 0.4713 0.2451 1.0322 0.114 Uiso 1 1 calc R . . H4SB H 0.5296 0.1912 1.0858 0.114 Uiso 1 1 calc R . . C5S C 0.7217(3) 0.1349(3) 1.02393(18) 0.0482(11) Uani 1 1 d . . . H5SA H 0.7747 0.0981 1.0081 0.058 Uiso 1 1 calc R . . H5SB H 0.7283 0.1093 1.0598 0.058 Uiso 1 1 calc R . . C6S C 0.7411(4) 0.2473(4) 1.0241(2) 0.0621(14) Uani 1 1 d . . . H6SA H 0.7219 0.2798 1.0547 0.075 Uiso 1 1 calc R . . H6SB H 0.8183 0.2620 1.0248 0.075 Uiso 1 1 calc R . . C7S C 0.6713(4) 0.2860(4) 0.9759(2) 0.0646(15) Uani 1 1 d . . . H7SA H 0.7149 0.3016 0.9500 0.077 Uiso 1 1 calc R . . H7SB H 0.6338 0.3496 0.9828 0.077 Uiso 1 1 calc R . . C8S C 0.5896(4) 0.2025(3) 0.95575(19) 0.0599(14) Uani 1 1 d . . . H8SA H 0.5148 0.2285 0.9525 0.072 Uiso 1 1 calc R . . H8SB H 0.5975 0.1784 0.9213 0.072 Uiso 1 1 calc R . . C11 C -0.0331(3) 0.1159(4) 0.75648(18) 0.0518(12) Uani 1 1 d . . . H11A H -0.0540 0.0568 0.7751 0.078 Uiso 1 1 calc R . . H11B H -0.0261 0.0944 0.7218 0.078 Uiso 1 1 calc R . . H11C H -0.0887 0.1694 0.7532 0.078 Uiso 1 1 calc R . . C12 C 0.0869(3) 0.0192(3) 0.84752(15) 0.0335(9) Uani 1 1 d . . . C13 C 0.3996(3) 0.3034(3) 0.82853(14) 0.0286(9) Uani 1 1 d . . . C21 C 0.0747(3) 0.1580(3) 0.78644(15) 0.0338(9) Uani 1 1 d . . . C22 C 0.0130(3) 0.0211(3) 0.88003(16) 0.0405(10) Uani 1 1 d . . . C23 C 0.4301(3) 0.3960(3) 0.85553(15) 0.0337(9) Uani 1 1 d . . . C31 C 0.1157(3) 0.2438(3) 0.76454(15) 0.0365(10) Uani 1 1 d . . . H31A H 0.0670 0.2749 0.7361 0.044 Uiso 1 1 calc R . . C32 C -0.0179(4) -0.0733(4) 0.89738(18) 0.0515(12) Uani 1 1 d . . . H32A H -0.0680 -0.0744 0.9193 0.062 Uiso 1 1 calc R . . C33 C 0.5374(4) 0.4285(3) 0.86142(17) 0.0453(11) Uani 1 1 d . . . H33A H 0.5599 0.4908 0.8794 0.054 Uiso 1 1 calc R . . C41 C 0.2173(3) 0.2896(3) 0.77868(15) 0.0313(9) Uani 1 1 d . . . C42 C 0.0219(4) -0.1636(4) 0.88365(19) 0.0544(13) Uani 1 1 d . . . H42A H -0.0010 -0.2267 0.8958 0.065 Uiso 1 1 calc R . . C43 C 0.6115(3) 0.3724(4) 0.84169(18) 0.0476(11) Uani 1 1 d . . . H43A H 0.6837 0.3967 0.8456 0.057 Uiso 1 1 calc R . . C51 C 0.2413(3) 0.3715(3) 0.74252(17) 0.0446(11) Uani 1 1 d . . . H51A H 0.3144 0.3987 0.7559 0.067 Uiso 1 1 calc R . . H51B H 0.1883 0.4272 0.7401 0.067 Uiso 1 1 calc R . . H51C H 0.2368 0.3419 0.7080 0.067 Uiso 1 1 calc R . . C52 C 0.0950(4) -0.1642(3) 0.85224(17) 0.0464(11) Uani 1 1 d . . . H52A H 0.1222 -0.2280 0.8431 0.056 Uiso 1 1 calc R . . C53 C 0.5808(3) 0.2817(4) 0.81643(16) 0.0435(11) Uani 1 1 d . . . H53A H 0.6325 0.2436 0.8030 0.052 Uiso 1 1 calc R . . C62 C 0.1299(3) -0.0738(3) 0.83356(15) 0.0363(10) Uani 1 1 d . . . C63 C 0.4757(3) 0.2441(3) 0.80999(14) 0.0326(9) Uani 1 1 d . . . C72 C -0.0343(3) 0.1201(4) 0.89616(18) 0.0510(12) Uani 1 1 d . . . H72A H 0.0031 0.1788 0.8830 0.061 Uiso 1 1 calc R . . C73 C 0.3511(4) 0.4601(3) 0.87791(17) 0.0428(11) Uani 1 1 d . . . H73A H 0.2809 0.4219 0.8726 0.051 Uiso 1 1 calc R . . C82 C -0.0148(4) 0.1306(4) 0.95508(19) 0.0645(14) Uani 1 1 d . . . H82A H 0.0630 0.1247 0.9704 0.097 Uiso 1 1 calc R . . H82B H -0.0539 0.0760 0.9688 0.097 Uiso 1 1 calc R . . H82C H -0.0410 0.1977 0.9638 0.097 Uiso 1 1 calc R . . C83 C 0.3935(4) 0.4766(4) 0.9364(2) 0.0623(14) Uani 1 1 d . . . H83A H 0.4076 0.4098 0.9537 0.093 Uiso 1 1 calc R . . H83B H 0.3390 0.5140 0.9504 0.093 Uiso 1 1 calc R . . H83C H 0.4608 0.5166 0.9424 0.093 Uiso 1 1 calc R . . C92 C -0.1560(4) 0.1293(5) 0.8720(2) 0.0767(17) Uani 1 1 d . . . H92A H -0.1682 0.1224 0.8342 0.115 Uiso 1 1 calc R . . H92B H -0.1822 0.1966 0.8806 0.115 Uiso 1 1 calc R . . H92C H -0.1952 0.0749 0.8858 0.115 Uiso 1 1 calc R . . C93 C 0.3292(5) 0.5642(3) 0.8512(2) 0.0699(15) Uani 1 1 d . . . H93A H 0.3022 0.5540 0.8138 0.105 Uiso 1 1 calc R . . H93B H 0.3965 0.6042 0.8573 0.105 Uiso 1 1 calc R . . H93C H 0.2747 0.6013 0.8653 0.105 Uiso 1 1 calc R . . C102 C 0.2107(4) -0.0751(3) 0.79886(18) 0.0451(11) Uani 1 1 d . . . H10A H 0.2514 -0.0087 0.8047 0.054 Uiso 1 1 calc R . . C103 C 0.4448(4) 0.1432(3) 0.78199(17) 0.0441(11) Uani 1 1 d . . . H10B H 0.3774 0.1186 0.7920 0.053 Uiso 1 1 calc R . . C112 C 0.2939(4) -0.1603(4) 0.8119(2) 0.0644(14) Uani 1 1 d . . . H11D H 0.3434 -0.1571 0.7882 0.097 Uiso 1 1 calc R . . H11E H 0.2569 -0.2270 0.8082 0.097 Uiso 1 1 calc R . . H11F H 0.3352 -0.1521 0.8478 0.097 Uiso 1 1 calc R . . C113 C 0.5297(4) 0.0586(4) 0.7971(2) 0.0644(14) Uani 1 1 d . . . H11G H 0.5471 0.0501 0.8349 0.097 Uiso 1 1 calc R . . H11H H 0.5954 0.0776 0.7854 0.097 Uiso 1 1 calc R . . H11I H 0.5009 -0.0061 0.7806 0.097 Uiso 1 1 calc R . . C122 C 0.1561(5) -0.0793(5) 0.7420(2) 0.0729(16) Uani 1 1 d . . . H12A H 0.2113 -0.0802 0.7212 0.109 Uiso 1 1 calc R . . H12B H 0.1096 -0.0188 0.7329 0.109 Uiso 1 1 calc R . . H12C H 0.1119 -0.1418 0.7351 0.109 Uiso 1 1 calc R . . C123 C 0.4173(5) 0.1571(4) 0.7234(2) 0.0812(18) Uani 1 1 d . . . H12D H 0.3629 0.2115 0.7140 0.122 Uiso 1 1 calc R . . H12E H 0.3884 0.0926 0.7068 0.122 Uiso 1 1 calc R . . H12F H 0.4830 0.1762 0.7117 0.122 Uiso 1 1 calc R . . O3 O 1.0147(9) 0.5940(8) 0.9407(5) 0.128(4) Uiso 0.50 1 d PD A 1 C9S C 0.9064(10) 0.5916(10) 0.9361(6) 0.087(4) Uiso 0.50 1 d PD A 1 H9SA H 0.8689 0.6335 0.9062 0.105 Uiso 0.50 1 calc PR A 1 H9SB H 0.8870 0.6180 0.9680 0.105 Uiso 0.50 1 calc PR A 1 C10S C 0.875(3) 0.4747(19) 0.927(2) 0.27(3) Uiso 0.50 1 d PD A 1 H10C H 0.8670 0.4435 0.9606 0.320 Uiso 0.50 1 calc PR A 1 H10D H 0.8044 0.4684 0.9021 0.320 Uiso 0.50 1 calc PR A 1 C11S C 0.9509(10) 0.4264(8) 0.9099(5) 0.065(3) Uiso 0.50 1 d PD A 1 H11J H 0.9223 0.3996 0.8744 0.078 Uiso 0.50 1 calc PR A 1 H11K H 0.9813 0.3686 0.9330 0.078 Uiso 0.50 1 calc PR A 1 C12S C 1.0432(13) 0.5159(14) 0.9099(7) 0.115(5) Uiso 0.50 1 d PD A 1 H12G H 1.1169 0.4895 0.9250 0.138 Uiso 0.50 1 calc PR A 1 H12H H 1.0407 0.5407 0.8742 0.138 Uiso 0.50 1 calc PR A 1 O3A O 0.9817(15) 0.5668(13) 0.8858(7) 0.193(6) Uiso 0.50 1 d PD B 2 C9A C 0.8735(14) 0.5785(14) 0.8894(7) 0.145(7) Uiso 0.50 1 d PD B 2 H9AA H 0.8249 0.5546 0.8568 0.174 Uiso 0.50 1 calc PR B 2 H9AB H 0.8583 0.6522 0.8939 0.174 Uiso 0.50 1 calc PR B 2 C10A C 0.8502(14) 0.5167(15) 0.9357(8) 0.115(6) Uiso 0.50 1 d PD B 2 H10E H 0.8787 0.5520 0.9691 0.138 Uiso 0.50 1 calc PR B 2 H10F H 0.7716 0.5037 0.9317 0.138 Uiso 0.50 1 calc PR B 2 C11A C 0.9042(19) 0.4303(16) 0.9319(10) 0.140(7) Uiso 0.50 1 d PD B 2 H11L H 0.8545 0.3771 0.9132 0.168 Uiso 0.50 1 calc PR B 2 H11M H 0.9384 0.4039 0.9669 0.168 Uiso 0.50 1 calc PR B 2 C12A C 0.999(2) 0.4599(18) 0.8989(9) 0.165(9) Uiso 0.50 1 d PD B 2 H12I H 1.0730 0.4489 0.9207 0.198 Uiso 0.50 1 calc PR B 2 H12J H 0.9907 0.4173 0.8672 0.198 Uiso 0.50 1 calc PR B 2 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 0.0331(3) 0.0328(3) 0.0294(3) 0.0048(3) 0.0046(2) -0.0023(3) Cl1 0.0381(6) 0.0355(6) 0.0313(5) 0.0064(4) -0.0019(4) 0.0027(4) Cl2 0.0770(9) 0.0579(7) 0.0400(6) -0.0073(6) 0.0205(6) 0.0035(6) O1 0.0330(15) 0.0325(15) 0.0363(15) -0.0044(12) 0.0104(12) 0.0035(12) O2 0.0360(15) 0.0291(14) 0.0309(15) 0.0049(12) 0.0046(12) -0.0010(12) N11 0.0276(17) 0.0265(17) 0.0305(18) 0.0049(14) 0.0035(14) -0.0027(14) N21 0.0283(17) 0.0237(16) 0.0284(17) 0.0031(14) 0.0061(13) -0.0016(13) Mg1 0.0283(9) 0.0256(9) 0.0271(9) 0.0008(8) 0.0058(7) 0.0021(8) C1S 0.086(4) 0.044(3) 0.116(5) -0.010(3) 0.076(4) -0.011(3) C2S 0.219(9) 0.068(4) 0.211(9) -0.066(5) 0.190(8) -0.051(5) C3S 0.085(4) 0.099(5) 0.121(6) -0.072(4) 0.059(4) -0.028(4) C4S 0.055(3) 0.083(4) 0.154(6) -0.082(4) 0.039(4) -0.019(3) C5S 0.034(2) 0.049(3) 0.056(3) 0.012(2) -0.003(2) -0.007(2) C6S 0.051(3) 0.054(3) 0.074(4) 0.006(3) -0.002(3) -0.018(2) C7S 0.074(4) 0.038(3) 0.068(3) 0.011(2) -0.012(3) -0.018(2) C8S 0.079(4) 0.037(3) 0.051(3) 0.021(2) -0.012(3) -0.017(2) C11 0.036(2) 0.060(3) 0.052(3) 0.021(2) -0.008(2) -0.012(2) C12 0.028(2) 0.034(2) 0.033(2) 0.0083(18) -0.0040(17) -0.0096(18) C13 0.033(2) 0.027(2) 0.025(2) 0.0091(16) 0.0048(16) -0.0009(17) C21 0.029(2) 0.034(2) 0.036(2) 0.0059(18) 0.0021(17) -0.0001(18) C22 0.032(2) 0.044(3) 0.042(3) 0.012(2) 0.0024(19) -0.0049(19) C23 0.039(2) 0.028(2) 0.033(2) 0.0067(17) 0.0055(18) -0.0036(18) C31 0.032(2) 0.038(2) 0.035(2) 0.0131(19) -0.0020(17) 0.0049(19) C32 0.040(3) 0.061(3) 0.051(3) 0.015(2) 0.006(2) -0.016(2) C33 0.049(3) 0.037(2) 0.046(3) 0.003(2) 0.003(2) -0.014(2) C41 0.035(2) 0.030(2) 0.030(2) 0.0086(17) 0.0094(18) 0.0020(17) C42 0.055(3) 0.045(3) 0.054(3) 0.017(2) -0.005(2) -0.022(2) C43 0.034(2) 0.056(3) 0.054(3) 0.011(2) 0.012(2) -0.010(2) C51 0.046(3) 0.043(2) 0.041(3) 0.019(2) 0.002(2) -0.002(2) C52 0.056(3) 0.030(2) 0.044(3) 0.003(2) -0.009(2) -0.011(2) C53 0.036(2) 0.056(3) 0.042(3) 0.011(2) 0.0163(19) 0.005(2) C62 0.037(2) 0.033(2) 0.033(2) 0.0018(18) -0.0050(17) -0.0043(19) C63 0.035(2) 0.037(2) 0.027(2) 0.0061(18) 0.0094(17) 0.0009(18) C72 0.041(3) 0.060(3) 0.058(3) 0.015(2) 0.023(2) 0.001(2) C73 0.049(3) 0.027(2) 0.053(3) -0.005(2) 0.013(2) -0.0012(19) C82 0.060(3) 0.081(4) 0.059(3) 0.005(3) 0.028(3) 0.003(3) C83 0.083(4) 0.046(3) 0.060(3) -0.017(2) 0.020(3) -0.002(3) C92 0.045(3) 0.099(4) 0.087(4) 0.022(4) 0.018(3) 0.018(3) C93 0.086(4) 0.037(3) 0.088(4) 0.008(3) 0.024(3) 0.014(3) C102 0.052(3) 0.029(2) 0.054(3) -0.007(2) 0.011(2) -0.004(2) C103 0.047(3) 0.039(2) 0.051(3) -0.005(2) 0.021(2) 0.003(2) C112 0.065(3) 0.061(3) 0.061(3) -0.012(3) 0.003(3) 0.020(3) C113 0.078(4) 0.045(3) 0.073(4) -0.001(3) 0.022(3) 0.016(3) C122 0.078(4) 0.092(4) 0.050(3) 0.010(3) 0.017(3) 0.019(3) C123 0.119(5) 0.072(4) 0.045(3) -0.016(3) 0.003(3) 0.022(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 N21 2.011(3) . ? Fe1 N11 2.014(3) . ? Fe1 Cl2 2.2675(12) . ? Fe1 Cl1 2.3773(11) . ? Cl1 Mg1 2.5201(9) . ? O1 C1S 1.429(5) . ? O1 C4S 1.430(6) . ? O1 Mg1 2.080(2) . ? O2 C5S 1.454(5) . ? O2 C8S 1.455(5) . ? O2 Mg1 2.136(2) . ? N11 C21 1.325(5) . ? N11 C12 1.447(5) . ? N21 C41 1.333(5) . ? N21 C13 1.442(5) . ? Mg1 O1 2.080(2) 3_657 ? Mg1 O2 2.136(2) 3_657 ? Mg1 Cl1 2.5201(9) 3_657 ? C1S C2S 1.502(7) . ? C2S C3S 1.390(8) . ? C3S C4S 1.437(7) . ? C5S C6S 1.483(6) . ? C6S C7S 1.468(7) . ? C7S C8S 1.512(6) . ? C11 C21 1.518(5) . ? C12 C22 1.402(6) . ? C12 C62 1.409(6) . ? C13 C63 1.404(5) . ? C13 C23 1.409(5) . ? C21 C31 1.409(5) . ? C22 C32 1.397(6) . ? C22 C72 1.521(6) . ? C23 C33 1.397(6) . ? C23 C73 1.518(6) . ? C31 C41 1.390(5) . ? C32 C42 1.359(7) . ? C33 C43 1.378(6) . ? C41 C51 1.507(5) . ? C42 C52 1.373(7) . ? C43 C53 1.369(6) . ? C52 C62 1.385(6) . ? C53 C63 1.390(6) . ? C62 C102 1.517(6) . ? C63 C103 1.515(6) . ? C72 C82 1.527(7) . ? C72 C92 1.534(6) . ? C73 C93 1.523(6) . ? C73 C83 1.533(7) . ? C102 C122 1.507(7) . ? C102 C112 1.515(6) . ? C103 C123 1.519(6) . ? C103 C113 1.526(6) . ? O3 C9S 1.349(13) . ? O3 C12S 1.398(17) . ? C9S C10S 1.58(2) . ? C10S C11S 1.32(3) . ? C11S C12S 1.649(19) . ? O3A C9A 1.401(15) . ? O3A C12A 1.438(19) . ? C9A C10A 1.546(19) . ? C10A C11A 1.33(3) . ? C11A C12A 1.68(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 N21 Fe1 N11 92.15(12) . . ? N21 Fe1 Cl2 115.14(9) . . ? N11 Fe1 Cl2 117.98(10) . . ? N21 Fe1 Cl1 115.53(9) . . ? N11 Fe1 Cl1 110.25(9) . . ? Cl2 Fe1 Cl1 105.80(4) . . ? Fe1 Cl1 Mg1 137.05(4) . . ? C1S O1 C4S 108.2(3) . . ? C1S O1 Mg1 124.9(2) . . ? C4S O1 Mg1 126.7(3) . . ? C5S O2 C8S 107.0(3) . . ? C5S O2 Mg1 128.6(2) . . ? C8S O2 Mg1 124.3(2) . . ? C21 N11 C12 120.2(3) . . ? C21 N11 Fe1 123.6(2) . . ? C12 N11 Fe1 116.1(2) . . ? C41 N21 C13 119.2(3) . . ? C41 N21 Fe1 123.2(2) . . ? C13 N21 Fe1 117.6(2) . . ? O1 Mg1 O1 180.000(1) . 3_657 ? O1 Mg1 O2 91.08(10) . 3_657 ? O1 Mg1 O2 88.92(10) 3_657 3_657 ? O1 Mg1 O2 88.92(10) . . ? O1 Mg1 O2 91.08(10) 3_657 . ? O2 Mg1 O2 180.00(13) 3_657 . ? O1 Mg1 Cl1 93.27(7) . . ? O1 Mg1 Cl1 86.73(7) 3_657 . ? O2 Mg1 Cl1 90.16(7) 3_657 . ? O2 Mg1 Cl1 89.84(7) . . ? O1 Mg1 Cl1 86.73(7) . 3_657 ? O1 Mg1 Cl1 93.27(7) 3_657 3_657 ? O2 Mg1 Cl1 89.84(7) 3_657 3_657 ? O2 Mg1 Cl1 90.16(7) . 3_657 ? Cl1 Mg1 Cl1 180.0 . 3_657 ? O1 C1S C2S 104.6(4) . . ? C3S C2S C1S 108.8(4) . . ? C2S C3S C4S 106.2(5) . . ? O1 C4S C3S 109.3(4) . . ? O2 C5S C6S 106.0(3) . . ? C7S C6S C5S 105.6(4) . . ? C6S C7S C8S 106.9(4) . . ? O2 C8S C7S 106.2(3) . . ? C22 C12 C62 121.6(4) . . ? C22 C12 N11 119.9(4) . . ? C62 C12 N11 118.4(3) . . ? C63 C13 C23 120.9(4) . . ? C63 C13 N21 118.6(3) . . ? C23 C13 N21 120.4(3) . . ? N11 C21 C31 122.9(3) . . ? N11 C21 C11 120.9(3) . . ? C31 C21 C11 116.2(3) . . ? C32 C22 C12 117.3(4) . . ? C32 C22 C72 119.8(4) . . ? C12 C22 C72 122.9(4) . . ? C33 C23 C13 117.7(4) . . ? C33 C23 C73 119.8(4) . . ? C13 C23 C73 122.5(3) . . ? C41 C31 C21 129.2(3) . . ? C42 C32 C22 121.7(4) . . ? C43 C33 C23 121.5(4) . . ? N21 C41 C31 123.4(3) . . ? N21 C41 C51 120.7(3) . . ? C31 C41 C51 115.9(3) . . ? C32 C42 C52 120.3(4) . . ? C53 C43 C33 119.9(4) . . ? C42 C52 C62 121.5(4) . . ? C43 C53 C63 121.5(4) . . ? C52 C62 C12 117.6(4) . . ? C52 C62 C102 121.1(4) . . ? C12 C62 C102 121.3(4) . . ? C53 C63 C13 118.4(4) . . ? C53 C63 C103 120.0(4) . . ? C13 C63 C103 121.6(3) . . ? C22 C72 C82 112.1(4) . . ? C22 C72 C92 111.7(4) . . ? C82 C72 C92 109.7(4) . . ? C23 C73 C93 112.1(4) . . ? C23 C73 C83 110.9(4) . . ? C93 C73 C83 109.2(4) . . ? C122 C102 C112 110.0(4) . . ? C122 C102 C62 112.4(4) . . ? C112 C102 C62 113.4(4) . . ? C63 C103 C123 111.7(4) . . ? C63 C103 C113 114.0(4) . . ? C123 C103 C113 109.9(4) . . ? C9S O3 C12S 108.7(12) . . ? O3 C9S C10S 104.8(14) . . ? C11S C10S C9S 109.2(19) . . ? C10S C11S C12S 103.7(13) . . ? O3 C12S C11S 103.8(11) . . ? C9A O3A C12A 101.0(15) . . ? O3A C9A C10A 111.0(14) . . ? C11A C10A C9A 100.9(16) . . ? C10A C11A C12A 106.5(14) . . ? O3A C12A C11A 104.8(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.486 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.061 data_sad2 _database_code_CSD 167180 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point 270-272 _chemical_formula_moiety ? _chemical_formula_sum 'C35 H53 Cl Fe N2' _chemical_formula_weight 593.09 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 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 16.9014(11) _cell_length_b 9.3514(6) _cell_length_c 22.7756(15) _cell_angle_alpha 90.00 _cell_angle_beta 107.2370(10) _cell_angle_gamma 90.00 _cell_volume 3438.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 2132 _cell_measurement_theta_min 2 _cell_measurement_theta_max 23 _exptl_crystal_description Rhombic _exptl_crystal_colour Red/BrownD _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.48 _exptl_crystal_density_meas NA _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7361 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0271 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2463 _reflns_number_gt 2132 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0418P)^2^+2.8195P] 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 2463 _refine_ls_number_parameters 178 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.0917 _refine_ls_wR_factor_gt 0.0874 _refine_ls_goodness_of_fit_ref 1.107 _refine_ls_restrained_S_all 1.107 _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 0.5000 1.83056(5) 0.7500 0.03331(18) Uani 1 2 d S . . Cl1 Cl 0.5000 2.06285(10) 0.7500 0.0688(4) Uani 1 2 d S . . N1 N 0.44760(11) 1.69163(19) 0.68667(8) 0.0246(4) Uani 1 1 d . . . C1 C 0.41405(14) 1.4376(2) 0.64279(10) 0.0275(5) Uani 1 1 d . . . C2 C 0.45486(13) 1.5488(2) 0.69354(10) 0.0236(5) Uani 1 1 d . . . C3 C 0.5000 1.4888(3) 0.7500 0.0269(8) Uani 1 2 d S . . H3A H 0.5000 1.3872 0.7500 0.032 Uiso 1 2 calc SR . . C4 C 0.48206(16) 1.3403(3) 0.63196(11) 0.0378(6) Uani 1 1 d . . . H4A H 0.4568 1.2699 0.6000 0.057 Uiso 1 1 calc R . . H4B H 0.5107 1.2906 0.6702 0.057 Uiso 1 1 calc R . . H4C H 0.5219 1.3986 0.6187 0.057 Uiso 1 1 calc R . . C5 C 0.35341(16) 1.3473(3) 0.66629(12) 0.0399(6) Uani 1 1 d . . . H5A H 0.3267 1.2760 0.6352 0.060 Uiso 1 1 calc R . . H5B H 0.3112 1.4097 0.6742 0.060 Uiso 1 1 calc R . . H5C H 0.3839 1.2986 0.7044 0.060 Uiso 1 1 calc R . . C6 C 0.36433(16) 1.4955(3) 0.57962(11) 0.0368(6) Uani 1 1 d . . . H6A H 0.3420 1.4154 0.5519 0.055 Uiso 1 1 calc R . . H6B H 0.4006 1.5532 0.5625 0.055 Uiso 1 1 calc R . . H6C H 0.3186 1.5549 0.5840 0.055 Uiso 1 1 calc R . . C12 C 0.40984(14) 1.7721(2) 0.63152(10) 0.0270(6) Uani 1 1 d . . . C22 C 0.45735(15) 1.8020(2) 0.59140(11) 0.0305(6) Uani 1 1 d . . . C32 C 0.42264(17) 1.8904(3) 0.54163(12) 0.0439(7) Uani 1 1 d . . . H32A H 0.4529 1.9102 0.5135 0.053 Uiso 1 1 calc R . . C42 C 0.34570(18) 1.9502(3) 0.53193(13) 0.0511(8) Uani 1 1 d . . . H42A H 0.3231 2.0101 0.4973 0.061 Uiso 1 1 calc R . . C52 C 0.30143(17) 1.9229(3) 0.57259(13) 0.0457(7) Uani 1 1 d . . . H52A H 0.2483 1.9650 0.5656 0.055 Uiso 1 1 calc R . . C62 C 0.33227(15) 1.8357(3) 0.62344(11) 0.0339(6) Uani 1 1 d . . . C72 C 0.54393(16) 1.7425(3) 0.60280(11) 0.0381(6) Uani 1 1 d . . . H72A H 0.5493 1.6575 0.6303 0.046 Uiso 1 1 calc R . . C82 C 0.5633(2) 1.6936(4) 0.54469(14) 0.0606(9) Uani 1 1 d . . . H82A H 0.5220 1.6230 0.5231 0.091 Uiso 1 1 calc R . . H82B H 0.6186 1.6504 0.5558 0.091 Uiso 1 1 calc R . . H82C H 0.5617 1.7761 0.5178 0.091 Uiso 1 1 calc R . . C92 C 0.60805(19) 1.8525(4) 0.63630(17) 0.0735(11) Uani 1 1 d . . . H92A H 0.5956 1.8839 0.6737 0.110 Uiso 1 1 calc R . . H92B H 0.6064 1.9349 0.6094 0.110 Uiso 1 1 calc R . . H92C H 0.6633 1.8093 0.6474 0.110 Uiso 1 1 calc R . . C102 C 0.28143(17) 1.8109(3) 0.66760(13) 0.0452(7) Uani 1 1 d . . . H10A H 0.3159 1.7532 0.7029 0.054 Uiso 1 1 calc R . . C112 C 0.2024(2) 1.7269(4) 0.63770(18) 0.0740(11) Uani 1 1 d . . . H11A H 0.2165 1.6367 0.6213 0.111 Uiso 1 1 calc R . . H11B H 0.1661 1.7834 0.6042 0.111 Uiso 1 1 calc R . . H11C H 0.1738 1.7066 0.6684 0.111 Uiso 1 1 calc R . . C122 C 0.2597(2) 1.9519(4) 0.69330(15) 0.0640(9) Uani 1 1 d . . . H12A H 0.3107 2.0056 0.7125 0.096 Uiso 1 1 calc R . . H12B H 0.2312 1.9318 0.7241 0.096 Uiso 1 1 calc R . . H12C H 0.2235 2.0085 0.6598 0.096 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 0.0480(3) 0.0184(3) 0.0284(3) 0.000 0.0036(2) 0.000 Cl1 0.1055(10) 0.0194(5) 0.0658(7) 0.000 0.0012(7) 0.000 N1 0.0306(11) 0.0202(12) 0.0221(10) 0.0005(8) 0.0061(8) 0.0010(8) C1 0.0293(13) 0.0270(13) 0.0248(12) -0.0031(10) 0.0059(10) -0.0025(10) C2 0.0223(12) 0.0243(13) 0.0268(13) -0.0012(10) 0.0110(10) -0.0010(10) C3 0.035(2) 0.0187(17) 0.0270(18) 0.000 0.0086(16) 0.000 C4 0.0463(16) 0.0329(14) 0.0334(14) -0.0065(12) 0.0105(12) 0.0040(12) C5 0.0407(15) 0.0351(15) 0.0424(15) -0.0054(13) 0.0099(12) -0.0099(12) C6 0.0422(16) 0.0328(14) 0.0297(14) -0.0078(11) 0.0017(12) -0.0032(12) C12 0.0304(14) 0.0225(13) 0.0243(13) -0.0002(10) 0.0023(11) -0.0017(10) C22 0.0324(14) 0.0291(14) 0.0281(13) 0.0009(11) 0.0060(11) -0.0048(11) C32 0.0471(18) 0.0512(17) 0.0325(15) 0.0132(13) 0.0103(13) -0.0066(14) C42 0.0469(18) 0.0572(19) 0.0414(16) 0.0250(15) 0.0013(14) 0.0039(15) C52 0.0357(16) 0.0466(18) 0.0493(17) 0.0143(14) 0.0041(14) 0.0088(13) C62 0.0307(14) 0.0313(14) 0.0375(14) 0.0024(12) 0.0068(11) 0.0002(12) C72 0.0373(15) 0.0439(16) 0.0362(15) 0.0037(12) 0.0156(13) -0.0011(12) C82 0.066(2) 0.067(2) 0.0565(19) -0.0032(17) 0.0313(17) 0.0037(17) C92 0.0377(18) 0.100(3) 0.082(2) -0.027(2) 0.0168(17) -0.0124(18) C102 0.0379(16) 0.0467(18) 0.0535(17) 0.0126(14) 0.0175(13) 0.0118(13) C112 0.056(2) 0.065(2) 0.117(3) -0.015(2) 0.051(2) -0.0104(17) C122 0.071(2) 0.062(2) 0.067(2) -0.0040(18) 0.0340(18) 0.0056(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 1.9482(18) . ? Fe1 N1 1.9482(18) 2_656 ? Fe1 Cl1 2.1722(11) . ? N1 C2 1.346(3) . ? N1 C12 1.441(3) . ? C1 C6 1.534(3) . ? C1 C5 1.541(3) . ? C1 C4 1.542(3) . ? C1 C2 1.556(3) . ? C2 C3 1.403(3) . ? C3 C2 1.403(3) 2_656 ? C12 C62 1.401(3) . ? C12 C22 1.412(3) . ? C22 C32 1.385(3) . ? C22 C72 1.514(3) . ? C32 C42 1.372(4) . ? C42 C52 1.376(4) . ? C52 C62 1.386(4) . ? C62 C102 1.522(4) . ? C72 C92 1.525(4) . ? C72 C82 1.524(4) . ? C102 C112 1.525(4) . ? C102 C122 1.531(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 N1 Fe1 N1 96.35(11) . 2_656 ? N1 Fe1 Cl1 131.83(5) . . ? N1 Fe1 Cl1 131.83(5) 2_656 . ? C2 N1 C12 128.38(18) . . ? C2 N1 Fe1 124.74(15) . . ? C12 N1 Fe1 106.50(13) . . ? C6 C1 C5 106.5(2) . . ? C6 C1 C4 106.58(19) . . ? C5 C1 C4 109.6(2) . . ? C6 C1 C2 117.37(19) . . ? C5 C1 C2 107.61(18) . . ? C4 C1 C2 109.01(19) . . ? N1 C2 C3 120.6(2) . . ? N1 C2 C1 124.89(19) . . ? C3 C2 C1 114.5(2) . . ? C2 C3 C2 132.8(3) 2_656 . ? C62 C12 C22 121.3(2) . . ? C62 C12 N1 119.4(2) . . ? C22 C12 N1 118.6(2) . . ? C32 C22 C12 117.6(2) . . ? C32 C22 C72 120.9(2) . . ? C12 C22 C72 121.5(2) . . ? C42 C32 C22 121.8(2) . . ? C32 C42 C52 119.6(2) . . ? C42 C52 C62 121.8(3) . . ? C52 C62 C12 117.7(2) . . ? C52 C62 C102 119.7(2) . . ? C12 C62 C102 122.5(2) . . ? C22 C72 C92 110.2(2) . . ? C22 C72 C82 114.0(2) . . ? C92 C72 C82 109.5(2) . . ? C62 C102 C112 112.0(2) . . ? C62 C102 C122 111.5(2) . . ? C112 C102 C122 109.7(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.252 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.037