data_dm6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 1-Co _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 Cl2 Co N2 O2' _chemical_formula_sum 'C22 H24 Cl2 Co N2 O2' _chemical_formula_weight 478.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_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 15.555(3) _cell_length_b 10.169(2) _cell_length_c 28.108(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.88(3) _cell_angle_gamma 90.00 _cell_volume 4445.8(15) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 688 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 15.73 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1976 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8201 _exptl_absorpt_correction_T_max 0.9038 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _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 31094 _diffrn_reflns_av_R_equivalents 0.1368 _diffrn_reflns_av_sigmaI/netI 0.1497 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 23.26 _reflns_number_total 6389 _reflns_number_gt 3233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0350P)^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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6389 _refine_ls_number_parameters 531 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1027 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.019 _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 Co1 Co 0.00816(4) 0.91516(6) 0.12943(2) 0.01447(18) Uani 1 1 d . . . Co2 Co -0.00631(4) 0.75663(6) 0.35730(2) 0.01310(17) Uani 1 1 d . . . Cl1 Cl -0.01530(10) 1.01892(13) 0.19824(5) 0.0440(5) Uani 1 1 d . . . Cl2 Cl -0.10044(9) 0.92797(14) 0.07545(5) 0.0470(5) Uani 1 1 d . . . Cl3 Cl 0.00523(9) 0.64544(13) 0.28978(5) 0.0407(4) Uani 1 1 d . . . Cl4 Cl 0.10809(9) 0.73751(14) 0.40670(5) 0.0438(4) Uani 1 1 d . . . O1 O 0.0883(2) 0.5504(3) 0.18670(12) 0.0335(10) Uani 1 1 d . . . O2 O 0.2066(2) 1.0422(3) 0.03920(12) 0.0335(10) Uani 1 1 d . . . O3 O -0.0904(2) 1.1231(3) 0.30563(12) 0.0323(10) Uani 1 1 d . . . O4 O -0.1820(2) 0.6463(3) 0.46206(12) 0.0426(11) Uani 1 1 d . . . N1 N 0.0260(2) 0.7244(4) 0.14995(14) 0.0260(12) Uani 1 1 d . . . N2 N 0.1059(3) 1.0096(4) 0.09556(14) 0.0262(12) Uani 1 1 d . . . N3 N -0.0233(3) 0.9484(4) 0.33842(14) 0.0282(12) Uani 1 1 d . . . N4 N -0.0996(3) 0.6682(4) 0.39700(14) 0.0283(12) Uani 1 1 d . . . C1 C -0.0436(3) 0.6230(5) 0.15052(18) 0.0293(15) Uani 1 1 d . . . C2 C -0.0010(3) 0.5097(5) 0.17924(18) 0.0321(16) Uani 1 1 d . . . H2A H -0.0298 0.4973 0.2101 0.039 Uiso 1 1 calc R . . H2B H -0.0039 0.4262 0.1611 0.039 Uiso 1 1 calc R . . C3 C 0.0922(3) 0.6768(5) 0.17074(18) 0.0276(15) Uani 1 1 d . . . C4 C 0.1759(3) 0.7428(5) 0.17823(17) 0.0279(15) Uani 1 1 d . . . C5 C 0.2034(3) 0.7797(5) 0.22371(18) 0.0331(16) Uani 1 1 d . . . H5A H 0.1724 0.7507 0.2506 0.040 Uiso 1 1 calc R . . C6 C 0.2749(3) 0.8573(5) 0.23015(19) 0.0374(17) Uani 1 1 d . . . H6A H 0.2946 0.8798 0.2613 0.045 Uiso 1 1 calc R . . C7 C 0.3181(3) 0.9024(5) 0.1902(2) 0.0419(18) Uani 1 1 d . . . H7A H 0.3656 0.9603 0.1941 0.050 Uiso 1 1 calc R . . C8 C 0.2926(3) 0.8637(5) 0.14510(19) 0.0336(17) Uani 1 1 d . . . H8A H 0.3241 0.8924 0.1184 0.040 Uiso 1 1 calc R . . C9 C 0.2215(3) 0.7835(4) 0.13836(17) 0.0239(14) Uani 1 1 d . . . C10 C 0.1955(3) 0.7326(5) 0.09072(17) 0.0229(14) Uani 1 1 d . . . C11 C 0.1992(3) 0.5973(5) 0.08031(19) 0.0353(16) Uani 1 1 d . . . H11A H 0.2191 0.5371 0.1039 0.042 Uiso 1 1 calc R . . C12 C 0.1741(3) 0.5515(5) 0.0358(2) 0.0434(18) Uani 1 1 d . . . H12A H 0.1756 0.4599 0.0293 0.052 Uiso 1 1 calc R . . C13 C 0.1466(4) 0.6386(5) 0.0009(2) 0.0441(18) Uani 1 1 d . . . H13A H 0.1292 0.6063 -0.0295 0.053 Uiso 1 1 calc R . . C14 C 0.1444(3) 0.7721(5) 0.00989(18) 0.0325(16) Uani 1 1 d . . . H14A H 0.1267 0.8320 -0.0143 0.039 Uiso 1 1 calc R . . C15 C 0.1686(3) 0.8181(5) 0.05506(18) 0.0255(15) Uani 1 1 d . . . C16 C 0.1572(3) 0.9604(5) 0.06514(18) 0.0256(15) Uani 1 1 d . . . C17 C 0.1758(3) 1.1730(5) 0.05051(18) 0.0363(17) Uani 1 1 d . . . H17A H 0.1416 1.2095 0.0236 0.044 Uiso 1 1 calc R . . H17B H 0.2246 1.2328 0.0575 0.044 Uiso 1 1 calc R . . C18 C 0.1194(3) 1.1561(5) 0.09484(19) 0.0305(16) Uani 1 1 d . . . C19 C -0.0620(3) 0.5818(5) 0.09857(16) 0.0382(17) Uani 1 1 d . . . H19A H -0.1000 0.5050 0.0981 0.057 Uiso 1 1 calc R . . H19B H -0.0078 0.5596 0.0832 0.057 Uiso 1 1 calc R . . H19C H -0.0898 0.6546 0.0815 0.057 Uiso 1 1 calc R . . C20 C -0.1227(3) 0.6784(5) 0.17528(18) 0.0375(17) Uani 1 1 d . . . H20A H -0.1062 0.7098 0.2071 0.056 Uiso 1 1 calc R . . H20B H -0.1662 0.6092 0.1781 0.056 Uiso 1 1 calc R . . H20C H -0.1464 0.7515 0.1566 0.056 Uiso 1 1 calc R . . C21 C 0.1653(3) 1.1966(5) 0.14053(18) 0.0425(18) Uani 1 1 d . . . H21A H 0.1286 1.1773 0.1677 0.064 Uiso 1 1 calc R . . H21B H 0.1777 1.2910 0.1396 0.064 Uiso 1 1 calc R . . H21C H 0.2193 1.1475 0.1438 0.064 Uiso 1 1 calc R . . C22 C 0.0329(3) 1.2249(5) 0.0881(2) 0.0483(19) Uani 1 1 d . . . H22A H 0.0029 1.1885 0.0602 0.072 Uiso 1 1 calc R . . H22B H 0.0423 1.3193 0.0835 0.072 Uiso 1 1 calc R . . H22C H -0.0020 1.2112 0.1164 0.072 Uiso 1 1 calc R . . C23 C 0.0441(3) 1.0527(4) 0.33870(17) 0.0258(15) Uani 1 1 d . . . C24 C 0.0008(3) 1.1658(5) 0.30973(19) 0.0335(16) Uani 1 1 d . . . H24A H 0.0058 1.2507 0.3268 0.040 Uiso 1 1 calc R . . H24B H 0.0269 1.1748 0.2780 0.040 Uiso 1 1 calc R . . C25 C -0.0925(3) 0.9966(5) 0.32096(17) 0.0260(15) Uani 1 1 d . . . C26 C -0.1762(3) 0.9298(5) 0.31658(19) 0.0294(15) Uani 1 1 d . . . C27 C -0.2075(3) 0.8914(5) 0.27146(18) 0.0344(16) Uani 1 1 d . . . H27A H -0.1794 0.9185 0.2434 0.041 Uiso 1 1 calc R . . C28 C -0.2796(3) 0.8138(5) 0.2690(2) 0.0449(18) Uani 1 1 d . . . H28A H -0.3019 0.7877 0.2388 0.054 Uiso 1 1 calc R . . C29 C -0.3205(3) 0.7725(5) 0.3103(2) 0.0412(18) Uani 1 1 d . . . H29A H -0.3695 0.7168 0.3082 0.049 Uiso 1 1 calc R . . C30 C -0.2894(3) 0.8132(5) 0.35443(19) 0.0340(17) Uani 1 1 d . . . H30A H -0.3177 0.7860 0.3825 0.041 Uiso 1 1 calc R . . C31 C -0.2178(3) 0.8925(4) 0.35809(18) 0.0258(15) Uani 1 1 d . . . C32 C -0.1866(3) 0.9455(5) 0.40482(18) 0.0277(15) Uani 1 1 d . . . C33 C -0.1940(3) 1.0812(5) 0.41390(17) 0.0310(16) Uani 1 1 d . . . H33A H -0.2194 1.1373 0.3906 0.037 Uiso 1 1 calc R . . C34 C -0.1644(3) 1.1330(5) 0.45643(18) 0.0350(17) Uani 1 1 d . . . H34A H -0.1698 1.2247 0.4621 0.042 Uiso 1 1 calc R . . C35 C -0.1270(4) 1.0534(5) 0.49096(19) 0.0427(18) Uani 1 1 d . . . H35A H -0.1060 1.0900 0.5200 0.051 Uiso 1 1 calc R . . C36 C -0.1207(3) 0.9193(5) 0.48246(18) 0.0375(17) Uani 1 1 d . . . H36A H -0.0963 0.8636 0.5062 0.045 Uiso 1 1 calc R . . C37 C -0.1495(3) 0.8661(5) 0.43995(19) 0.0309(16) Uani 1 1 d . . . C38 C -0.1414(3) 0.7227(5) 0.43135(19) 0.0331(16) Uani 1 1 d . . . C39 C -0.1636(4) 0.5116(5) 0.44855(19) 0.0434(18) Uani 1 1 d . . . H39A H -0.2175 0.4613 0.4436 0.052 Uiso 1 1 calc R . . H39B H -0.1284 0.4673 0.4734 0.052 Uiso 1 1 calc R . . C40 C -0.1131(4) 0.5224(5) 0.40119(19) 0.0352(17) Uani 1 1 d . . . C41 C 0.1244(3) 1.0033(5) 0.31386(17) 0.0340(16) Uani 1 1 d . . . H41A H 0.1495 0.9303 0.3321 0.051 Uiso 1 1 calc R . . H41B H 0.1664 1.0749 0.3118 0.051 Uiso 1 1 calc R . . H41C H 0.1090 0.9730 0.2818 0.051 Uiso 1 1 calc R . . C42 C 0.0616(3) 1.0926(5) 0.39065(16) 0.0357(16) Uani 1 1 d . . . H42A H 0.0070 1.1100 0.4064 0.054 Uiso 1 1 calc R . . H42B H 0.0972 1.1721 0.3915 0.054 Uiso 1 1 calc R . . H42C H 0.0919 1.0211 0.4072 0.054 Uiso 1 1 calc R . . C43 C -0.0268(4) 0.4505(5) 0.4041(2) 0.056(2) Uani 1 1 d . . . H43A H 0.0058 0.4680 0.3752 0.084 Uiso 1 1 calc R . . H43B H -0.0368 0.3557 0.4071 0.084 Uiso 1 1 calc R . . H43C H 0.0060 0.4817 0.4320 0.084 Uiso 1 1 calc R . . C44 C -0.1683(4) 0.4778(5) 0.35851(19) 0.051(2) Uani 1 1 d . . . H44A H -0.2240 0.5229 0.3591 0.076 Uiso 1 1 calc R . . H44B H -0.1774 0.3825 0.3602 0.076 Uiso 1 1 calc R . . H44C H -0.1388 0.4994 0.3289 0.076 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 Co1 0.0123(4) 0.0142(4) 0.0168(4) -0.0012(3) -0.0016(3) 0.0024(3) Co2 0.0126(4) 0.0124(3) 0.0143(4) -0.0019(3) -0.0012(3) 0.0018(3) Cl1 0.0540(10) 0.0414(9) 0.0369(9) -0.0055(8) 0.0062(8) 0.0086(8) Cl2 0.0348(9) 0.0541(10) 0.0517(10) 0.0104(9) -0.0175(8) -0.0036(8) Cl3 0.0497(10) 0.0401(9) 0.0323(9) -0.0062(7) -0.0001(8) 0.0062(8) Cl4 0.0386(9) 0.0459(9) 0.0464(10) -0.0056(8) -0.0131(8) 0.0060(8) O1 0.034(2) 0.026(2) 0.040(2) -0.0051(18) -0.0065(19) -0.0051(18) O2 0.039(2) 0.027(2) 0.035(2) 0.0012(18) -0.0005(19) 0.0017(19) O3 0.031(2) 0.032(2) 0.033(2) 0.0017(18) -0.0072(19) -0.0031(18) O4 0.056(3) 0.027(2) 0.045(3) 0.008(2) 0.023(2) 0.004(2) N1 0.019(3) 0.027(3) 0.032(3) -0.005(2) -0.003(2) 0.004(2) N2 0.028(3) 0.021(2) 0.030(3) -0.011(2) -0.001(2) 0.003(2) N3 0.021(3) 0.036(3) 0.027(3) -0.003(2) -0.004(2) 0.002(2) N4 0.029(3) 0.023(3) 0.033(3) -0.003(2) 0.001(2) 0.006(2) C1 0.032(3) 0.026(3) 0.029(3) -0.002(3) -0.005(3) -0.011(3) C2 0.027(3) 0.030(3) 0.040(4) -0.009(3) -0.001(3) -0.009(3) C3 0.038(4) 0.013(3) 0.033(4) -0.002(3) 0.008(3) -0.014(3) C4 0.027(3) 0.025(3) 0.031(3) -0.006(3) -0.004(3) 0.003(3) C5 0.029(3) 0.043(4) 0.027(3) -0.010(3) 0.003(3) 0.003(3) C6 0.025(3) 0.047(4) 0.040(4) -0.015(3) -0.005(3) 0.003(3) C7 0.024(3) 0.037(4) 0.064(5) -0.007(3) -0.010(3) -0.007(3) C8 0.025(3) 0.033(3) 0.043(4) -0.005(3) 0.000(3) -0.005(3) C9 0.026(3) 0.020(3) 0.026(3) 0.004(3) 0.006(3) 0.008(3) C10 0.021(3) 0.023(3) 0.024(3) -0.001(3) 0.005(3) 0.000(3) C11 0.024(3) 0.033(3) 0.049(4) -0.005(3) 0.002(3) 0.003(3) C12 0.048(4) 0.032(4) 0.050(4) -0.008(3) 0.007(3) -0.007(3) C13 0.056(4) 0.042(4) 0.034(4) -0.011(3) 0.002(3) -0.005(3) C14 0.038(4) 0.031(3) 0.029(3) 0.000(3) 0.001(3) -0.003(3) C15 0.029(3) 0.023(3) 0.025(3) -0.010(3) 0.003(3) -0.005(3) C16 0.034(3) 0.019(3) 0.023(3) 0.003(3) -0.019(3) -0.002(3) C17 0.046(4) 0.018(3) 0.045(4) -0.001(3) -0.007(3) -0.001(3) C18 0.038(4) 0.018(3) 0.036(4) -0.005(3) -0.003(3) -0.004(3) C19 0.041(4) 0.045(4) 0.028(3) -0.012(3) -0.001(3) -0.007(3) C20 0.032(4) 0.048(4) 0.033(4) -0.001(3) 0.004(3) -0.004(3) C21 0.047(4) 0.038(4) 0.043(4) -0.011(3) -0.007(3) -0.003(3) C22 0.043(4) 0.035(4) 0.067(5) 0.000(3) -0.001(3) 0.013(3) C23 0.025(3) 0.023(3) 0.030(3) -0.004(3) 0.003(3) 0.002(3) C24 0.029(4) 0.027(3) 0.044(4) 0.006(3) -0.005(3) -0.008(3) C25 0.038(4) 0.024(3) 0.015(3) -0.003(3) 0.003(3) 0.003(3) C26 0.022(3) 0.025(3) 0.042(4) -0.001(3) -0.004(3) 0.004(3) C27 0.034(4) 0.041(4) 0.027(3) -0.012(3) -0.012(3) 0.006(3) C28 0.038(4) 0.053(4) 0.044(4) -0.010(3) -0.016(3) -0.002(3) C29 0.024(3) 0.035(4) 0.064(5) -0.007(3) -0.010(3) 0.002(3) C30 0.023(4) 0.036(3) 0.043(4) -0.002(3) -0.002(3) -0.007(3) C31 0.022(3) 0.021(3) 0.035(4) -0.001(3) -0.003(3) -0.001(3) C32 0.017(3) 0.032(3) 0.035(3) -0.003(3) 0.008(3) -0.001(3) C33 0.043(4) 0.026(3) 0.024(3) -0.006(3) -0.001(3) 0.002(3) C34 0.045(4) 0.027(3) 0.033(4) 0.000(3) 0.020(3) -0.001(3) C35 0.060(4) 0.042(4) 0.027(4) -0.007(3) -0.004(3) 0.002(3) C36 0.050(4) 0.041(4) 0.022(3) 0.004(3) 0.000(3) 0.009(3) C37 0.031(4) 0.023(3) 0.039(4) -0.007(3) 0.000(3) 0.003(3) C38 0.035(4) 0.031(4) 0.033(4) 0.003(3) 0.002(3) -0.005(3) C39 0.049(4) 0.021(3) 0.061(4) -0.006(3) 0.017(4) 0.015(3) C40 0.043(4) 0.018(3) 0.045(4) 0.001(3) 0.013(3) -0.006(3) C41 0.031(4) 0.036(3) 0.036(4) 0.000(3) 0.011(3) -0.010(3) C42 0.035(4) 0.040(4) 0.032(4) -0.001(3) -0.008(3) -0.005(3) C43 0.059(5) 0.028(4) 0.082(5) 0.012(3) 0.019(4) 0.016(3) C44 0.064(5) 0.035(4) 0.052(4) -0.008(3) 0.001(4) -0.009(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 Co1 N1 2.042(4) . ? Co1 N2 2.045(4) . ? Co1 Cl1 2.2380(16) . ? Co1 Cl2 2.2569(16) . ? Co2 N3 2.037(4) . ? Co2 N4 2.052(4) . ? Co2 Cl3 2.2189(15) . ? Co2 Cl4 2.2486(16) . ? O1 C3 1.364(5) . ? O1 C2 1.460(5) . ? O2 C16 1.352(6) . ? O2 C17 1.451(5) . ? O3 C25 1.356(5) . ? O3 C24 1.486(5) . ? O4 C38 1.329(6) . ? O4 C39 1.451(5) . ? N1 C3 1.272(6) . ? N1 C1 1.495(6) . ? N2 C16 1.281(6) . ? N2 C18 1.505(6) . ? N3 C25 1.275(6) . ? N3 C23 1.490(6) . ? N4 C38 1.296(6) . ? N4 C40 1.503(6) . ? C1 C20 1.530(7) . ? C1 C19 1.542(6) . ? C1 C2 1.551(6) . ? C3 C4 1.477(7) . ? C4 C5 1.393(6) . ? C4 C9 1.398(7) . ? C5 C6 1.373(7) . ? C6 C7 1.396(7) . ? C7 C8 1.380(7) . ? C8 C9 1.385(6) . ? C9 C10 1.486(6) . ? C10 C15 1.387(6) . ? C10 C11 1.408(6) . ? C11 C12 1.385(7) . ? C12 C13 1.385(7) . ? C13 C14 1.382(6) . ? C14 C15 1.399(6) . ? C15 C16 1.486(6) . ? C17 C18 1.544(7) . ? C18 C21 1.517(6) . ? C18 C22 1.526(7) . ? C23 C41 1.526(6) . ? C23 C42 1.536(6) . ? C23 C24 1.556(6) . ? C25 C26 1.472(7) . ? C26 C31 1.396(7) . ? C26 C27 1.407(6) . ? C27 C28 1.372(7) . ? C28 C29 1.397(7) . ? C29 C30 1.388(7) . ? C30 C31 1.377(6) . ? C31 C32 1.494(7) . ? C32 C37 1.394(7) . ? C32 C33 1.408(6) . ? C33 C34 1.379(6) . ? C34 C35 1.385(7) . ? C35 C36 1.388(7) . ? C36 C37 1.381(7) . ? C37 C38 1.483(7) . ? C39 C40 1.560(7) . ? C40 C44 1.533(7) . ? C40 C43 1.530(7) . ? 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 Co1 N2 118.61(15) . . ? N1 Co1 Cl1 103.13(12) . . ? N2 Co1 Cl1 108.25(12) . . ? N1 Co1 Cl2 109.98(11) . . ? N2 Co1 Cl2 102.35(12) . . ? Cl1 Co1 Cl2 115.05(6) . . ? N3 Co2 N4 118.12(16) . . ? N3 Co2 Cl3 106.07(12) . . ? N4 Co2 Cl3 108.01(12) . . ? N3 Co2 Cl4 109.98(12) . . ? N4 Co2 Cl4 100.72(12) . . ? Cl3 Co2 Cl4 114.23(6) . . ? C3 O1 C2 105.5(4) . . ? C16 O2 C17 104.7(4) . . ? C25 O3 C24 106.3(4) . . ? C38 O4 C39 106.5(4) . . ? C3 N1 C1 108.3(4) . . ? C3 N1 Co1 126.6(3) . . ? C1 N1 Co1 124.3(3) . . ? C16 N2 C18 106.7(4) . . ? C16 N2 Co1 127.1(3) . . ? C18 N2 Co1 125.2(3) . . ? C25 N3 C23 108.5(4) . . ? C25 N3 Co2 125.0(3) . . ? C23 N3 Co2 126.3(3) . . ? C38 N4 C40 106.9(4) . . ? C38 N4 Co2 125.8(3) . . ? C40 N4 Co2 125.2(3) . . ? N1 C1 C20 109.8(4) . . ? N1 C1 C19 107.5(4) . . ? C20 C1 C19 113.1(4) . . ? N1 C1 C2 102.3(4) . . ? C20 C1 C2 112.2(4) . . ? C19 C1 C2 111.2(4) . . ? O1 C2 C1 105.2(4) . . ? N1 C3 O1 118.0(4) . . ? N1 C3 C4 126.8(4) . . ? O1 C3 C4 115.2(4) . . ? C5 C4 C9 120.2(5) . . ? C5 C4 C3 120.8(5) . . ? C9 C4 C3 118.5(4) . . ? C6 C5 C4 120.9(5) . . ? C5 C6 C7 118.8(5) . . ? C8 C7 C6 120.6(5) . . ? C7 C8 C9 120.8(5) . . ? C8 C9 C4 118.6(5) . . ? C8 C9 C10 122.3(5) . . ? C4 C9 C10 119.0(4) . . ? C15 C10 C11 118.4(4) . . ? C15 C10 C9 120.5(4) . . ? C11 C10 C9 121.1(4) . . ? C12 C11 C10 120.3(5) . . ? C11 C12 C13 120.4(5) . . ? C14 C13 C12 120.4(5) . . ? C13 C14 C15 119.2(5) . . ? C10 C15 C14 121.3(4) . . ? C10 C15 C16 120.6(4) . . ? C14 C15 C16 117.9(4) . . ? N2 C16 O2 119.0(4) . . ? N2 C16 C15 125.8(5) . . ? O2 C16 C15 115.2(4) . . ? O2 C17 C18 105.6(4) . . ? N2 C18 C21 108.8(4) . . ? N2 C18 C22 109.4(4) . . ? C21 C18 C22 112.5(4) . . ? N2 C18 C17 101.7(4) . . ? C21 C18 C17 112.8(4) . . ? C22 C18 C17 111.1(4) . . ? N3 C23 C41 110.1(4) . . ? N3 C23 C42 107.9(4) . . ? C41 C23 C42 112.7(4) . . ? N3 C23 C24 103.0(4) . . ? C41 C23 C24 110.8(4) . . ? C42 C23 C24 111.8(4) . . ? O3 C24 C23 103.2(4) . . ? N3 C25 O3 117.5(5) . . ? N3 C25 C26 126.6(5) . . ? O3 C25 C26 115.9(4) . . ? C31 C26 C27 121.3(5) . . ? C31 C26 C25 118.4(5) . . ? C27 C26 C25 119.8(5) . . ? C28 C27 C26 118.4(5) . . ? C27 C28 C29 120.9(5) . . ? C30 C29 C28 119.7(5) . . ? C31 C30 C29 120.8(5) . . ? C30 C31 C26 118.8(5) . . ? C30 C31 C32 121.9(5) . . ? C26 C31 C32 119.3(4) . . ? C37 C32 C33 118.2(5) . . ? C37 C32 C31 122.6(4) . . ? C33 C32 C31 119.1(4) . . ? C34 C33 C32 120.3(5) . . ? C33 C34 C35 121.0(5) . . ? C34 C35 C36 118.9(5) . . ? C37 C36 C35 120.8(5) . . ? C36 C37 C32 120.7(5) . . ? C36 C37 C38 119.9(5) . . ? C32 C37 C38 119.3(5) . . ? N4 C38 O4 118.8(5) . . ? N4 C38 C37 125.9(5) . . ? O4 C38 C37 115.2(5) . . ? O4 C39 C40 105.1(4) . . ? N4 C40 C44 107.9(4) . . ? N4 C40 C43 110.6(4) . . ? C44 C40 C43 112.4(5) . . ? N4 C40 C39 102.1(4) . . ? C44 C40 C39 111.3(5) . . ? C43 C40 C39 111.9(5) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.614 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.102 #===end data_ev3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 5-Fe2Li _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H72 Br2 Fe2 Li N3 O7' _chemical_formula_weight 1105.57 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' 'Br' 'Br' -0.2901 2.4595 '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' '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7059(10) _cell_length_b 14.3972(10) _cell_length_c 15.3609(11) _cell_angle_alpha 68.213(3) _cell_angle_beta 84.999(4) _cell_angle_gamma 75.078(4) _cell_volume 2719.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6714 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 21.37 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 2.051 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8212 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _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 57092 _diffrn_reflns_av_R_equivalents 0.0764 _diffrn_reflns_av_sigmaI/netI 0.0929 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.43 _reflns_number_total 13571 _reflns_number_gt 8050 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+3.0822P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13571 _refine_ls_number_parameters 625 _refine_ls_number_restraints 177 _refine_ls_R_factor_all 0.1196 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.2031 _refine_ls_wR_factor_gt 0.1732 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.525 _refine_ls_shift/su_mean 0.013 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 Br1 Br -0.50229(3) 0.25991(3) 0.31286(3) 0.03716(11) Uani 1 1 d . . . Br2 Br -0.06516(3) -0.14019(3) 0.34670(3) 0.03586(11) Uani 1 1 d . . . Fe1 Fe -0.32731(4) 0.23497(4) 0.26832(4) 0.02195(12) Uani 1 1 d . . . Fe2 Fe -0.21141(4) -0.00382(4) 0.26705(4) 0.02339(13) Uani 1 1 d . A . O1 O -0.29659(19) 0.28236(19) 0.13785(17) 0.0247(6) Uani 1 1 d . A . O2 O -0.2527(2) 0.08797(18) 0.33525(18) 0.0270(6) Uani 1 1 d . . . O3 O -0.2055(2) 0.0595(2) 0.13249(19) 0.0323(7) Uani 1 1 d . A . N1 N -0.2596(2) 0.2963(2) -0.0463(2) 0.0235(7) Uani 1 1 d . A . N2 N -0.2339(2) 0.2583(2) 0.3579(2) 0.0218(7) Uani 1 1 d . . . N3 N -0.3067(2) -0.0807(2) 0.2330(2) 0.0227(7) Uani 1 1 d . . . C1 C -0.3791(3) 0.3093(3) 0.0771(3) 0.0279(9) Uani 1 1 d . A . H1B H -0.4366 0.3556 0.0958 0.033 Uiso 1 1 calc R . . H1C H -0.4000 0.2462 0.0837 0.033 Uiso 1 1 calc R . . C2 C -0.3543(3) 0.3631(3) -0.0254(3) 0.0264(9) Uani 1 1 d . . . C3 C -0.2282(3) 0.3178(3) -0.1295(3) 0.0262(9) Uani 1 1 d . . . C4 C -0.2560(3) 0.3940(3) -0.2265(3) 0.0248(9) Uani 1 1 d . . . C5 C -0.3202(3) 0.4838(3) -0.2824(3) 0.0312(10) Uani 1 1 d . . . H5A H -0.3720 0.5239 -0.2568 0.037 Uiso 1 1 calc R . . C6 C -0.3047(3) 0.5120(3) -0.3781(3) 0.0321(10) Uani 1 1 d . . . H6A H -0.3483 0.5722 -0.4195 0.038 Uiso 1 1 calc R . . C7 C -0.2268(3) 0.4544(3) -0.4154(3) 0.0304(10) Uani 1 1 d . . . H7A H -0.2180 0.4772 -0.4814 0.036 Uiso 1 1 calc R . . C8 C -0.1619(3) 0.3652(3) -0.3591(3) 0.0263(9) Uani 1 1 d . . . H8A H -0.1094 0.3253 -0.3843 0.032 Uiso 1 1 calc R . . C9 C -0.1781(3) 0.3378(3) -0.2644(3) 0.0214(8) Uani 1 1 d . . . C10 C -0.1373(3) 0.2575(3) -0.1697(3) 0.0281(10) Uani 1 1 d . . . C11 C -0.3350(4) 0.4682(3) -0.0407(3) 0.0359(11) Uani 1 1 d . . . H11A H -0.2767 0.4584 -0.0029 0.054 Uiso 1 1 calc R . . H11B H -0.3947 0.5108 -0.0219 0.054 Uiso 1 1 calc R . . H11C H -0.3214 0.5025 -0.1072 0.054 Uiso 1 1 calc R . . C12 C -0.4438(3) 0.3713(4) -0.0838(3) 0.0377(11) Uani 1 1 d . . . H12A H -0.4350 0.4126 -0.1496 0.057 Uiso 1 1 calc R . . H12B H -0.5067 0.4043 -0.0604 0.057 Uiso 1 1 calc R . . H12C H -0.4467 0.3021 -0.0785 0.057 Uiso 1 1 calc R . . C13 C -0.1406(4) 0.1469(3) -0.1535(3) 0.0436(13) Uani 1 1 d . . . H13A H -0.0932 0.1213 -0.1958 0.065 Uiso 1 1 calc R . . H13B H -0.2091 0.1458 -0.1661 0.065 Uiso 1 1 calc R . . H13C H -0.1218 0.1029 -0.0884 0.065 Uiso 1 1 calc R . . C14 C -0.0345(3) 0.2633(4) -0.1438(3) 0.0403(12) Uani 1 1 d . . . H14A H 0.0172 0.2408 -0.1849 0.060 Uiso 1 1 calc R . . H14B H -0.0181 0.2182 -0.0784 0.060 Uiso 1 1 calc R . . H14C H -0.0367 0.3345 -0.1515 0.060 Uiso 1 1 calc R . . C15 C -0.2217(3) 0.0763(3) 0.4244(3) 0.0277(9) Uani 1 1 d . . . H15A H -0.1758 0.0072 0.4531 0.033 Uiso 1 1 calc R . . H15B H -0.2815 0.0809 0.4652 0.033 Uiso 1 1 calc R . . C16 C -0.1676(3) 0.1588(3) 0.4189(3) 0.0243(9) Uani 1 1 d . . . C17 C -0.2185(3) 0.3443(3) 0.3483(3) 0.0248(9) Uani 1 1 d . . . C18 C -0.1416(3) 0.3876(3) 0.3745(3) 0.0245(9) Uani 1 1 d . . . C19 C -0.0504(3) 0.3684(3) 0.4169(3) 0.0298(9) Uani 1 1 d . . . H19A H -0.0117 0.3002 0.4486 0.036 Uiso 1 1 calc R . . C20 C -0.0180(3) 0.4546(3) 0.4106(3) 0.0381(10) Uani 1 1 d . . . H20A H 0.0453 0.4449 0.4378 0.046 Uiso 1 1 calc R . . C21 C -0.0750(4) 0.5545(3) 0.3659(3) 0.0422(11) Uani 1 1 d . . . H21A H -0.0506 0.6112 0.3642 0.051 Uiso 1 1 calc R . . C22 C -0.1672(4) 0.5728(3) 0.3235(3) 0.0397(11) Uani 1 1 d . . . H22A H -0.2065 0.6409 0.2926 0.048 Uiso 1 1 calc R . . C23 C -0.1988(3) 0.4878(3) 0.3285(3) 0.0292(9) Uani 1 1 d . . . C24 C -0.2830(3) 0.4554(3) 0.2976(3) 0.0309(10) Uani 1 1 d . . . C25 C -0.1604(3) 0.1568(3) 0.5176(3) 0.0319(10) Uani 1 1 d . . . H25A H -0.1165 0.2007 0.5179 0.048 Uiso 1 1 calc R . . H25B H -0.1322 0.0860 0.5598 0.048 Uiso 1 1 calc R . . H25C H -0.2279 0.1826 0.5389 0.048 Uiso 1 1 calc R . . C26 C -0.0645(3) 0.1400(3) 0.3730(3) 0.0312(10) Uani 1 1 d . . . H26A H -0.0730 0.1350 0.3123 0.047 Uiso 1 1 calc R . . H26B H -0.0207 0.0756 0.4137 0.047 Uiso 1 1 calc R . . H26C H -0.0338 0.1974 0.3635 0.047 Uiso 1 1 calc R . . C27 C -0.2951(4) 0.4888(3) 0.1927(3) 0.0472(13) Uani 1 1 d . . . H27A H -0.3403 0.4528 0.1793 0.071 Uiso 1 1 calc R . . H27B H -0.2290 0.4718 0.1648 0.071 Uiso 1 1 calc R . . H27C H -0.3239 0.5634 0.1660 0.071 Uiso 1 1 calc R . . C28 C -0.3829(4) 0.4776(4) 0.3461(4) 0.0479(13) Uani 1 1 d . . . H28A H -0.4154 0.5514 0.3194 0.072 Uiso 1 1 calc R . . H28B H -0.3709 0.4575 0.4133 0.072 Uiso 1 1 calc R . . H28C H -0.4271 0.4381 0.3368 0.072 Uiso 1 1 calc R . . C29 C -0.2109(3) -0.0137(3) 0.0948(3) 0.0351(10) Uani 1 1 d . . . H29A H -0.1483 -0.0696 0.1111 0.042 Uiso 1 1 calc R . . H29B H -0.2151 0.0192 0.0256 0.042 Uiso 1 1 calc R . . C30 C -0.3019(3) -0.0606(3) 0.1303(3) 0.0289(9) Uani 1 1 d . . . C31 C -0.3687(3) -0.1282(3) 0.2854(3) 0.0251(9) Uani 1 1 d . . . C32 C -0.4512(3) -0.1777(3) 0.2815(3) 0.0322(10) Uani 1 1 d . . . C33 C -0.5087(3) -0.2007(3) 0.2255(4) 0.0444(12) Uani 1 1 d . . . H33A H -0.4991 -0.1830 0.1599 0.053 Uiso 1 1 calc R . . C34 C -0.5820(4) -0.2521(4) 0.2743(4) 0.0531(13) Uani 1 1 d . . . H34A H -0.6243 -0.2694 0.2399 0.064 Uiso 1 1 calc R . . C35 C -0.5959(4) -0.2787(4) 0.3687(4) 0.0568(14) Uani 1 1 d . . . H35A H -0.6460 -0.3152 0.3976 0.068 Uiso 1 1 calc R . . C36 C -0.5395(3) -0.2543(3) 0.4236(4) 0.0465(13) Uani 1 1 d . . . H36A H -0.5497 -0.2717 0.4892 0.056 Uiso 1 1 calc R . . C37 C -0.4673(3) -0.2028(3) 0.3766(3) 0.0338(10) Uani 1 1 d . . . C38 C -0.3872(3) -0.1538(3) 0.3920(3) 0.0301(9) Uani 1 1 d . . . C39 C -0.3985(4) 0.0169(4) 0.0834(3) 0.0458(13) Uani 1 1 d . . . H39A H -0.4565 -0.0128 0.1078 0.069 Uiso 1 1 calc R . . H39B H -0.3943 0.0334 0.0155 0.069 Uiso 1 1 calc R . . H39C H -0.4066 0.0800 0.0967 0.069 Uiso 1 1 calc R . . C40 C -0.2824(4) -0.1593(3) 0.1093(3) 0.0435(12) Uani 1 1 d . . . H40A H -0.2230 -0.2089 0.1449 0.065 Uiso 1 1 calc R . . H40B H -0.2703 -0.1435 0.0421 0.065 Uiso 1 1 calc R . . H40C H -0.3413 -0.1889 0.1274 0.065 Uiso 1 1 calc R . . C41 C -0.2983(4) -0.2272(3) 0.4535(3) 0.0399(12) Uani 1 1 d . . . H41A H -0.2433 -0.1925 0.4451 0.060 Uiso 1 1 calc R . . H41B H -0.2750 -0.2881 0.4360 0.060 Uiso 1 1 calc R . . H41C H -0.3189 -0.2484 0.5193 0.060 Uiso 1 1 calc R . . C42 C -0.4311(4) -0.0595(3) 0.4191(3) 0.0406(11) Uani 1 1 d . . . H42A H -0.4551 -0.0817 0.4838 0.061 Uiso 1 1 calc R . . H42B H -0.4875 -0.0137 0.3769 0.061 Uiso 1 1 calc R . . H42C H -0.3787 -0.0225 0.4139 0.061 Uiso 1 1 calc R . . Li1 Li -0.1908(5) 0.1983(4) 0.0845(4) 0.021 Uani 1 1 d . . . O1S O 0.2006(4) 0.0973(4) 0.3068(5) 0.1217(19) Uani 1 1 d U . . O2S O 0.2697(8) 0.1856(7) 0.1247(7) 0.211(4) Uani 1 1 d U . . C1S C 0.2280(7) 0.1588(8) 0.3498(7) 0.154(3) Uani 1 1 d U . . H1SA H 0.1680 0.1912 0.3774 0.231 Uiso 1 1 calc R . . H1SB H 0.2563 0.2124 0.3027 0.231 Uiso 1 1 calc R . . H1SC H 0.2785 0.1154 0.3991 0.231 Uiso 1 1 calc R . . C2S C 0.2731(6) 0.0390(7) 0.2623(8) 0.129(3) Uani 1 1 d U . . H2SA H 0.3171 -0.0199 0.3106 0.155 Uiso 1 1 calc R . . H2SB H 0.2377 0.0110 0.2280 0.155 Uiso 1 1 calc R . . C3S C 0.3312(12) 0.0981(13) 0.2013(13) 0.260(8) Uani 1 1 d U . . H3SA H 0.3825 0.0546 0.1739 0.312 Uiso 1 1 calc R . . H3SB H 0.3672 0.1254 0.2359 0.312 Uiso 1 1 calc R . . C4S C 0.3104(15) 0.2712(11) 0.0631(12) 0.310(9) Uani 1 1 d U . . H4SA H 0.2591 0.3199 0.0164 0.465 Uiso 1 1 calc R . . H4SB H 0.3700 0.2449 0.0310 0.465 Uiso 1 1 calc R . . H4SC H 0.3296 0.3064 0.1002 0.465 Uiso 1 1 calc R . . O4 O -0.0502(4) 0.2038(5) 0.1013(4) 0.056(3) Uani 0.456(4) 1 d PGU A 1 O5 O 0.0937(6) 0.3117(6) 0.0263(6) 0.110(4) Uani 0.456(4) 1 d PGU A 1 C43 C 0.0247(5) 0.1227(6) 0.1185(6) 0.041(3) Uani 0.456(4) 1 d PGU A 1 H43A H 0.0873 0.1408 0.1248 0.061 Uiso 0.456(4) 1 calc PR A 1 H43B H 0.0311 0.0972 0.0668 0.061 Uiso 0.456(4) 1 calc PR A 1 H43C H 0.0122 0.0689 0.1769 0.061 Uiso 0.456(4) 1 calc PR A 1 C44 C -0.0273(4) 0.2809(5) 0.0898(4) 0.049(2) Uani 0.456(4) 1 d PGU A 1 C45 C -0.0032(5) 0.3482(5) 0.0402(5) 0.069(3) Uani 0.456(4) 1 d PGU A 1 H45A H -0.0120 0.4026 0.0671 0.082 Uiso 0.456(4) 1 calc PR A 1 H45B H -0.0421 0.3771 -0.0192 0.082 Uiso 0.456(4) 1 calc PR A 1 C46 C 0.1442(9) 0.3774(9) -0.0386(9) 0.120(6) Uani 0.456(4) 1 d PGU A 1 H46A H 0.2146 0.3406 -0.0417 0.180 Uiso 0.456(4) 1 calc PR A 1 H46B H 0.1423 0.4361 -0.0201 0.180 Uiso 0.456(4) 1 calc PR A 1 H46F H 0.1119 0.4024 -0.1002 0.180 Uiso 0.456(4) 1 calc PR A 1 O4' O -0.0603(3) 0.1982(3) 0.1146(3) 0.0272(15) Uani 0.544(4) 1 d PGU A 2 O5' O 0.0540(4) 0.4042(4) 0.1136(4) 0.077(2) Uani 0.544(4) 1 d PGU A 2 C43' C 0.0166(4) 0.1060(4) 0.1378(4) 0.037(3) Uani 0.544(4) 1 d PGU A 2 H43D H 0.0794 0.1188 0.1515 0.055 Uiso 0.544(4) 1 calc PR A 2 H43E H 0.0271 0.0820 0.0850 0.055 Uiso 0.544(4) 1 calc PR A 2 H43F H -0.0033 0.0533 0.1931 0.055 Uiso 0.544(4) 1 calc PR A 2 C44' C -0.0442(3) 0.2771(3) 0.1296(3) 0.051(2) Uani 0.544(4) 1 d PGU A 2 C45' C 0.0122(3) 0.3128(3) 0.1580(3) 0.061(2) Uani 0.544(4) 1 d PGU A 2 H45C H 0.0725 0.2549 0.1808 0.073 Uiso 0.544(4) 1 calc PR A 2 H45D H -0.0212 0.3221 0.2150 0.073 Uiso 0.544(4) 1 calc PR A 2 C46' C 0.0989(6) 0.4275(5) 0.1951(6) 0.054(2) Uani 0.544(4) 1 d PGU A 2 H46C H 0.1270 0.4881 0.1668 0.081 Uiso 0.544(4) 1 calc PR A 2 H46D H 0.1521 0.3678 0.2297 0.081 Uiso 0.544(4) 1 calc PR A 2 H46E H 0.0447 0.4409 0.2381 0.081 Uiso 0.544(4) 1 calc PR A 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 Br1 0.0262(2) 0.0391(2) 0.0437(2) -0.01437(19) 0.00566(18) -0.00658(17) Br2 0.0271(2) 0.0381(2) 0.0374(2) -0.01389(18) -0.00610(17) 0.00282(17) Fe1 0.0229(3) 0.0238(2) 0.0187(3) -0.0077(2) -0.0028(2) -0.0040(2) Fe2 0.0253(3) 0.0229(2) 0.0242(3) -0.0097(2) -0.0018(2) -0.0072(2) O1 0.0242(13) 0.0304(13) 0.0167(12) -0.0077(10) -0.0017(10) -0.0028(11) O2 0.0343(14) 0.0200(11) 0.0271(13) -0.0096(10) -0.0097(11) -0.0026(11) O3 0.0459(16) 0.0269(13) 0.0256(14) -0.0060(11) -0.0013(12) -0.0158(12) N1 0.0229(15) 0.0255(15) 0.0217(15) -0.0100(12) 0.0010(13) -0.0034(13) N2 0.0229(15) 0.0219(14) 0.0227(15) -0.0107(12) -0.0015(12) -0.0042(12) N3 0.0237(15) 0.0215(14) 0.0250(16) -0.0103(12) -0.0002(13) -0.0061(12) C1 0.0266(19) 0.0326(19) 0.0230(19) -0.0106(16) 0.0022(16) -0.0043(16) C2 0.0225(18) 0.0308(19) 0.0208(18) -0.0104(15) -0.0029(15) 0.0049(16) C3 0.0261(19) 0.0232(17) 0.028(2) -0.0119(15) 0.0012(16) 0.0006(15) C4 0.0284(19) 0.0246(17) 0.0217(19) -0.0082(15) 0.0003(15) -0.0070(15) C5 0.032(2) 0.0273(19) 0.030(2) -0.0095(17) 0.0028(17) -0.0023(17) C6 0.038(2) 0.0246(19) 0.027(2) -0.0021(16) -0.0057(18) -0.0050(17) C7 0.039(2) 0.033(2) 0.0186(19) -0.0034(16) -0.0007(17) -0.0166(18) C8 0.0256(19) 0.0313(18) 0.0248(19) -0.0119(15) 0.0049(15) -0.0109(16) C9 0.0199(17) 0.0215(16) 0.0229(18) -0.0078(14) 0.0009(14) -0.0060(14) C10 0.027(2) 0.0260(19) 0.0223(19) -0.0039(16) 0.0027(16) -0.0004(16) C11 0.045(3) 0.030(2) 0.031(2) -0.0150(17) 0.0033(19) -0.0010(19) C12 0.026(2) 0.055(3) 0.028(2) -0.0187(19) -0.0056(17) 0.005(2) C13 0.053(3) 0.0207(19) 0.049(3) -0.0141(18) 0.018(2) 0.001(2) C14 0.025(2) 0.057(3) 0.031(2) -0.015(2) 0.0013(18) 0.000(2) C15 0.036(2) 0.0248(18) 0.0221(19) -0.0071(15) -0.0042(16) -0.0079(16) C16 0.0225(18) 0.0255(17) 0.0243(19) -0.0101(15) -0.0037(15) -0.0022(15) C17 0.0238(18) 0.0311(18) 0.0208(18) -0.0122(15) -0.0022(15) -0.0041(16) C18 0.0283(19) 0.0251(17) 0.0232(19) -0.0091(15) 0.0021(15) -0.0118(15) C19 0.030(2) 0.037(2) 0.025(2) -0.0135(16) 0.0003(16) -0.0105(17) C20 0.037(2) 0.056(2) 0.034(2) -0.0238(19) 0.0034(18) -0.023(2) C21 0.065(3) 0.044(2) 0.032(2) -0.0189(18) 0.008(2) -0.033(2) C22 0.065(3) 0.0286(19) 0.032(2) -0.0106(17) 0.004(2) -0.024(2) C23 0.039(2) 0.0302(18) 0.0225(19) -0.0111(15) -0.0016(17) -0.0129(17) C24 0.041(2) 0.0213(17) 0.032(2) -0.0099(16) -0.0100(18) -0.0061(17) C25 0.040(2) 0.0312(19) 0.026(2) -0.0100(16) -0.0090(18) -0.0090(18) C26 0.028(2) 0.0297(19) 0.035(2) -0.0132(17) 0.0007(17) -0.0027(17) C27 0.068(3) 0.031(2) 0.041(3) -0.0124(19) -0.026(2) -0.001(2) C28 0.035(2) 0.037(2) 0.071(3) -0.024(2) -0.005(2) 0.002(2) C29 0.047(2) 0.036(2) 0.027(2) -0.0146(17) 0.0062(19) -0.0168(19) C30 0.042(2) 0.0300(18) 0.0171(18) -0.0087(15) -0.0022(16) -0.0118(17) C31 0.0249(18) 0.0237(17) 0.029(2) -0.0119(15) -0.0016(16) -0.0056(15) C32 0.031(2) 0.0275(18) 0.043(2) -0.0147(17) 0.0014(18) -0.0138(16) C33 0.042(2) 0.041(2) 0.064(3) -0.028(2) -0.004(2) -0.019(2) C34 0.039(2) 0.053(2) 0.091(4) -0.046(2) 0.006(2) -0.023(2) C35 0.041(2) 0.055(2) 0.098(4) -0.047(3) 0.027(3) -0.030(2) C36 0.037(2) 0.042(2) 0.070(3) -0.027(2) 0.021(2) -0.021(2) C37 0.028(2) 0.0309(18) 0.053(3) -0.0229(18) 0.0105(18) -0.0170(16) C38 0.034(2) 0.0300(18) 0.032(2) -0.0133(16) 0.0046(17) -0.0152(17) C39 0.052(3) 0.042(2) 0.040(3) -0.010(2) -0.018(2) -0.008(2) C40 0.062(3) 0.041(2) 0.041(2) -0.0243(19) 0.006(2) -0.024(2) C41 0.045(3) 0.043(2) 0.028(2) -0.0071(19) 0.004(2) -0.016(2) C42 0.055(3) 0.039(2) 0.042(2) -0.0232(18) 0.009(2) -0.026(2) Li1 0.020 0.022 0.017 -0.005 0.001 -0.003 O1S 0.084(3) 0.112(4) 0.177(5) -0.063(3) -0.042(3) -0.008(3) O2S 0.241(9) 0.182(7) 0.205(8) -0.033(5) 0.019(7) -0.105(6) C1S 0.119(6) 0.230(7) 0.170(8) -0.106(6) -0.031(6) -0.079(6) C2S 0.071(5) 0.109(5) 0.201(8) -0.050(4) -0.003(5) -0.018(4) C3S 0.188(10) 0.226(11) 0.260(13) 0.011(8) 0.052(7) -0.037(9) C4S 0.52(2) 0.227(10) 0.246(16) -0.047(9) 0.047(15) -0.266(11) O4 0.071(5) 0.052(4) 0.034(4) -0.008(4) 0.021(4) -0.015(4) O5 0.127(6) 0.080(6) 0.136(8) -0.061(5) 0.079(6) -0.038(5) C43 0.040(5) 0.056(5) 0.030(5) -0.006(5) 0.000(4) -0.034(4) C44 0.031(4) 0.072(4) 0.051(5) -0.038(4) -0.024(4) 0.007(4) C45 0.084(6) 0.077(6) 0.054(6) -0.036(5) 0.004(5) -0.020(5) C46 0.117(10) 0.113(11) 0.161(15) -0.073(9) 0.064(10) -0.065(9) O4' 0.020(3) 0.024(3) 0.036(3) -0.010(2) -0.009(2) 0.001(2) O5' 0.113(6) 0.058(4) 0.067(5) -0.019(3) 0.006(4) -0.040(4) C43' 0.025(4) 0.030(4) 0.032(5) 0.009(4) 0.014(4) -0.001(3) C44' 0.054(5) 0.058(4) 0.047(6) -0.022(4) 0.007(4) -0.019(4) C45' 0.075(6) 0.059(4) 0.067(6) -0.035(4) 0.003(5) -0.027(4) C46' 0.054(5) 0.032(4) 0.084(6) -0.021(4) 0.011(5) -0.028(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 Br1 Fe1 2.4085(7) . ? Br2 Fe2 2.4469(7) . ? Fe1 O1 1.909(3) . ? Fe1 O2 2.009(2) . ? Fe1 N2 2.125(3) . ? Fe2 O2 1.924(3) . ? Fe2 O3 1.929(3) . ? Fe2 N3 2.122(3) . ? Fe2 Li1 3.262(6) . ? O1 C1 1.410(5) . ? O1 Li1 1.966(7) . ? O2 C15 1.407(5) . ? O3 C29 1.397(5) . ? O3 Li1 1.915(7) . ? N1 C3 1.261(5) . ? N1 C2 1.492(5) . ? N1 Li1 2.112(7) . ? N2 C17 1.261(5) . ? N2 C16 1.496(4) . ? N3 C31 1.268(5) . ? N3 C30 1.493(5) . ? C1 C2 1.528(5) . ? C1 Li1 2.650(7) . ? C2 C11 1.531(6) . ? C2 C12 1.536(6) . ? C3 C4 1.498(5) . ? C3 C10 1.548(5) . ? C4 C5 1.380(5) . ? C4 C9 1.389(5) . ? C5 C6 1.385(6) . ? C6 C7 1.395(6) . ? C7 C8 1.382(5) . ? C8 C9 1.373(5) . ? C9 C10 1.525(5) . ? C10 C13 1.530(6) . ? C10 C14 1.527(6) . ? C15 C16 1.529(6) . ? C16 C25 1.518(6) . ? C16 C26 1.529(5) . ? C17 C18 1.502(6) . ? C17 C24 1.554(5) . ? C18 C19 1.377(5) . ? C18 C23 1.397(5) . ? C19 C20 1.391(6) . ? C20 C21 1.390(6) . ? C21 C22 1.391(7) . ? C22 C23 1.375(6) . ? C23 C24 1.519(6) . ? C24 C27 1.512(6) . ? C24 C28 1.518(6) . ? C29 C30 1.533(6) . ? C30 C39 1.525(6) . ? C30 C40 1.524(6) . ? C31 C32 1.500(6) . ? C31 C38 1.553(6) . ? C32 C37 1.382(6) . ? C32 C33 1.390(6) . ? C33 C34 1.400(7) . ? C34 C35 1.365(8) . ? C35 C36 1.381(8) . ? C36 C37 1.380(6) . ? C37 C38 1.526(6) . ? C38 C42 1.527(6) . ? C38 C41 1.514(6) . ? Li1 O4' 1.885(8) . ? Li1 O4 1.992(9) . ? O1S C1S 1.417(10) . ? O1S C2S 1.427(11) . ? O2S C3S 1.486(16) . ? O2S C4S 1.457(15) . ? C2S C3S 1.365(17) . ? O4 C44 1.177(4) . ? O4 C43 1.299(4) . ? O5 C45 1.326(4) . ? O5 C46 1.373(4) . ? C44 C45 1.096(3) . ? O4' C44' 1.3127(19) . ? O4' C43' 1.412(2) . ? O5' C45' 1.476(2) . ? O5' C46' 1.615(2) . ? C44' C45' 1.2181(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 111.89(11) . . ? O1 Fe1 N2 116.35(12) . . ? O2 Fe1 N2 80.74(11) . . ? O1 Fe1 Br1 118.13(8) . . ? O2 Fe1 Br1 110.08(8) . . ? N2 Fe1 Br1 113.49(9) . . ? O2 Fe2 O3 116.61(11) . . ? O2 Fe2 N3 124.91(12) . . ? O3 Fe2 N3 82.40(12) . . ? O2 Fe2 Br2 108.84(8) . . ? O3 Fe2 Br2 117.20(9) . . ? N3 Fe2 Br2 105.05(8) . . ? O2 Fe2 Li1 86.90(14) . . ? O3 Fe2 Li1 31.81(14) . . ? N3 Fe2 Li1 109.32(14) . . ? Br2 Fe2 Li1 122.71(11) . . ? C1 O1 Fe1 115.1(2) . . ? C1 O1 Li1 102.1(3) . . ? Fe1 O1 Li1 121.5(2) . . ? C15 O2 Fe2 129.4(2) . . ? C15 O2 Fe1 109.5(2) . . ? Fe2 O2 Fe1 119.75(13) . . ? C29 O3 Li1 136.3(3) . . ? C29 O3 Fe2 107.6(2) . . ? Li1 O3 Fe2 116.1(2) . . ? C3 N1 C2 119.6(3) . . ? C3 N1 Li1 132.8(3) . . ? C2 N1 Li1 106.3(3) . . ? C17 N2 C16 121.7(3) . . ? C17 N2 Fe1 124.9(2) . . ? C16 N2 Fe1 111.7(2) . . ? C31 N3 C30 121.5(3) . . ? C31 N3 Fe2 128.3(3) . . ? C30 N3 Fe2 109.8(2) . . ? O1 C1 C2 112.6(3) . . ? O1 C1 Li1 46.5(2) . . ? C2 C1 Li1 83.6(2) . . ? N1 C2 C11 108.6(3) . . ? N1 C2 C1 106.8(3) . . ? C11 C2 C1 110.5(3) . . ? N1 C2 C12 111.4(3) . . ? C11 C2 C12 112.8(3) . . ? C1 C2 C12 106.5(3) . . ? N1 C3 C4 140.9(3) . . ? N1 C3 C10 129.4(3) . . ? C4 C3 C10 89.5(3) . . ? C5 C4 C9 121.6(4) . . ? C5 C4 C3 147.2(4) . . ? C9 C4 C3 91.2(3) . . ? C4 C5 C6 116.1(4) . . ? C5 C6 C7 121.8(4) . . ? C8 C7 C6 121.9(4) . . ? C9 C8 C7 115.8(4) . . ? C8 C9 C4 122.7(3) . . ? C8 C9 C10 142.6(3) . . ? C4 C9 C10 94.7(3) . . ? C9 C10 C13 115.4(4) . . ? C9 C10 C14 113.7(3) . . ? C13 C10 C14 112.0(4) . . ? C9 C10 C3 84.4(3) . . ? C13 C10 C3 114.6(3) . . ? C14 C10 C3 114.2(4) . . ? O2 C15 C16 111.6(3) . . ? N2 C16 C25 111.2(3) . . ? N2 C16 C26 109.6(3) . . ? C25 C16 C26 112.9(3) . . ? N2 C16 C15 105.0(3) . . ? C25 C16 C15 107.6(3) . . ? C26 C16 C15 110.2(3) . . ? N2 C17 C18 139.9(3) . . ? N2 C17 C24 130.1(4) . . ? C18 C17 C24 90.0(3) . . ? C19 C18 C23 122.0(4) . . ? C19 C18 C17 147.6(4) . . ? C23 C18 C17 90.4(3) . . ? C18 C19 C20 116.1(4) . . ? C21 C20 C19 122.3(4) . . ? C20 C21 C22 121.1(4) . . ? C23 C22 C21 116.9(4) . . ? C22 C23 C18 121.7(4) . . ? C22 C23 C24 142.7(4) . . ? C18 C23 C24 95.5(3) . . ? C27 C24 C23 115.0(4) . . ? C27 C24 C28 112.5(4) . . ? C23 C24 C28 114.2(4) . . ? C27 C24 C17 116.1(3) . . ? C23 C24 C17 84.1(3) . . ? C28 C24 C17 112.2(3) . . ? O3 C29 C30 112.9(3) . . ? N3 C30 C39 109.0(3) . . ? N3 C30 C40 112.4(3) . . ? C39 C30 C40 112.3(4) . . ? N3 C30 C29 105.5(3) . . ? C39 C30 C29 109.9(3) . . ? C40 C30 C29 107.4(4) . . ? N3 C31 C32 141.2(4) . . ? N3 C31 C38 129.2(4) . . ? C32 C31 C38 89.5(3) . . ? C37 C32 C33 122.1(4) . . ? C37 C32 C31 91.2(3) . . ? C33 C32 C31 146.7(4) . . ? C32 C33 C34 114.1(5) . . ? C35 C34 C33 123.5(5) . . ? C34 C35 C36 122.1(5) . . ? C35 C36 C37 115.4(5) . . ? C32 C37 C36 122.9(4) . . ? C32 C37 C38 95.3(3) . . ? C36 C37 C38 141.8(5) . . ? C42 C38 C41 112.3(4) . . ? C42 C38 C37 113.5(3) . . ? C41 C38 C37 115.9(3) . . ? C42 C38 C31 114.3(3) . . ? C41 C38 C31 114.1(3) . . ? C37 C38 C31 84.0(3) . . ? O4' Li1 O3 109.0(3) . . ? O4' Li1 O1 111.9(4) . . ? O3 Li1 O1 109.0(3) . . ? O4' Li1 O4 6.3(3) . . ? O3 Li1 O4 111.6(3) . . ? O1 Li1 O4 115.3(4) . . ? O4' Li1 N1 121.4(3) . . ? O3 Li1 N1 117.2(3) . . ? O1 Li1 N1 85.6(2) . . ? O4 Li1 N1 115.7(3) . . ? O4' Li1 C1 139.2(4) . . ? O3 Li1 C1 103.2(3) . . ? O1 Li1 C1 31.36(15) . . ? O4 Li1 C1 140.3(4) . . ? N1 Li1 C1 59.95(18) . . ? O4' Li1 Fe2 95.8(2) . . ? O3 Li1 Fe2 32.06(13) . . ? O1 Li1 Fe2 88.3(2) . . ? O4 Li1 Fe2 101.0(3) . . ? N1 Li1 Fe2 141.8(3) . . ? C1 Li1 Fe2 98.4(2) . . ? C1S O1S C2S 122.0(7) . . ? C3S O2S C4S 121.8(13) . . ? C3S C2S O1S 111.4(11) . . ? C2S C3S O2S 111.8(13) . . ? C44 O4 C43 115.0 . . ? C44 O4 Li1 123.2(4) . . ? C43 O4 Li1 121.7(4) . . ? C45 O5 C46 118.1 . . ? C45 C44 O4 147.0 . . ? C44 C45 O5 104.2 . . ? C44' O4' C43' 118.8 . . ? C44' O4' Li1 120.7(3) . . ? C43' O4' Li1 119.5(3) . . ? C45' O5' C46' 108.4 . . ? C45' C44' O4' 148.5 . . ? C44' C45' O5' 132.7 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 3.409 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.127 #===end data_ev5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Cr2(6sub2) _chemical_melting_point ? _chemical_formula_moiety 'C28 H36 Cl2 Cr2 N2 O2' _chemical_formula_sum 'C28 H36 Cl2 Cr2 N2 O2' _chemical_formula_weight 607.49 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' 'Cr' 'Cr' 0.3209 0.6236 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.9943(10) _cell_length_b 26.459(4) _cell_length_c 8.1697(11) _cell_angle_alpha 90.00 _cell_angle_beta 104.974(5) _cell_angle_gamma 90.00 _cell_volume 1460.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 2094 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 22.16 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7629 _exptl_absorpt_correction_T_max 0.9539 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _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 9496 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 23.42 _reflns_number_total 2092 _reflns_number_gt 1516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+2.5196P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2092 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0798 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1499 _refine_ls_wR_factor_gt 0.1344 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.013 _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 Cr1 Cr 0.42626(10) 0.06301(2) 0.44503(8) 0.0398(2) Uani 1 1 d . . . Cl1 Cl 0.3657(2) -0.02099(4) 0.32030(14) 0.0691(4) Uani 1 1 d . . . O1 O 0.1061(5) 0.16579(10) 0.0939(3) 0.0498(9) Uani 1 1 d . . . N1 N 0.2700(5) 0.09928(12) 0.2268(4) 0.0416(9) Uani 1 1 d . . . C1 C 0.2942(7) 0.09531(16) 0.0510(5) 0.0453(12) Uani 1 1 d . . . C2 C 0.2209(9) 0.14731(18) -0.0191(6) 0.0593(15) Uani 1 1 d . . . H2B H 0.132(7) 0.1507(18) -0.126(6) 0.067(14) Uiso 1 1 d . . . H2 H 0.332(7) 0.1723(18) 0.000(6) 0.066(15) Uiso 1 1 d . . . C3 C 0.1636(6) 0.13740(16) 0.2342(5) 0.0431(12) Uani 1 1 d . . . C4 C 0.0982(7) 0.15407(17) 0.3892(5) 0.0472(12) Uani 1 1 d . . . C5 C 0.2871(6) 0.16831(15) 0.5251(5) 0.0417(11) Uani 1 1 d . . . C6 C 0.3042(8) 0.21483(17) 0.6074(6) 0.0521(13) Uani 1 1 d . . . H6 H 0.198(5) 0.2340(14) 0.584(4) 0.031(10) Uiso 1 1 d . . . C7 C 0.4673(8) 0.22768(18) 0.7289(6) 0.0564(14) Uani 1 1 d . . . H7 H 0.486(6) 0.2569(18) 0.782(5) 0.059(13) Uiso 1 1 d . . . C8 C 0.6231(8) 0.19453(18) 0.7744(6) 0.0550(14) Uani 1 1 d . . . H8 H 0.732(6) 0.2009(16) 0.855(5) 0.048(13) Uiso 1 1 d . . . C9 C 0.6080(7) 0.14784(17) 0.6935(5) 0.0433(12) Uani 1 1 d . . . H9 H 0.707(5) 0.1279(14) 0.730(4) 0.031(10) Uiso 1 1 d . . . C10 C 0.4427(6) 0.13298(15) 0.5668(5) 0.0370(11) Uani 1 1 d . . . C11 C 0.5057(8) 0.0863(2) 0.0529(6) 0.0663(16) Uani 1 1 d . . . H11A H 0.5866 0.1138 0.1122 0.099 Uiso 1 1 calc R . . H11B H 0.5180 0.0847 -0.0626 0.099 Uiso 1 1 calc R . . H11C H 0.5499 0.0547 0.1102 0.099 Uiso 1 1 calc R . . C12 C 0.1598(9) 0.05405(19) -0.0424(6) 0.0749(18) Uani 1 1 d . . . H12A H 0.1950 0.0222 0.0163 0.112 Uiso 1 1 calc R . . H12B H 0.1748 0.0513 -0.1568 0.112 Uiso 1 1 calc R . . H12C H 0.0235 0.0622 -0.0465 0.112 Uiso 1 1 calc R . . C13 C -0.0071(7) 0.10892(19) 0.4495(6) 0.0583(14) Uani 1 1 d . . . H13A H -0.1158 0.0976 0.3572 0.087 Uiso 1 1 calc R . . H13B H -0.0578 0.1194 0.5440 0.087 Uiso 1 1 calc R . . H13C H 0.0864 0.0815 0.4851 0.087 Uiso 1 1 calc R . . C14 C -0.0546(8) 0.1972(2) 0.3408(7) 0.0721(17) Uani 1 1 d . . . H14A H 0.0085 0.2268 0.3083 0.108 Uiso 1 1 calc R . . H14B H -0.1061 0.2053 0.4371 0.108 Uiso 1 1 calc R . . H14C H -0.1624 0.1865 0.2466 0.108 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 Cr1 0.0649(4) 0.0257(4) 0.0277(3) 0.0041(3) 0.0097(3) 0.0151(3) Cl1 0.1158(11) 0.0343(6) 0.0397(6) -0.0012(5) -0.0115(7) 0.0215(7) O1 0.076(2) 0.0298(16) 0.0372(16) 0.0136(13) 0.0039(15) 0.0083(15) N1 0.069(2) 0.0264(18) 0.0302(18) 0.0053(15) 0.0148(17) 0.0075(18) C1 0.070(3) 0.036(2) 0.027(2) 0.0008(19) 0.007(2) -0.005(2) C2 0.101(4) 0.040(3) 0.033(2) 0.010(2) 0.011(3) 0.004(3) C3 0.057(3) 0.031(2) 0.037(2) 0.0106(19) 0.004(2) 0.004(2) C4 0.061(3) 0.035(2) 0.047(2) 0.010(2) 0.017(2) 0.021(2) C5 0.066(3) 0.029(2) 0.035(2) 0.0063(18) 0.022(2) 0.007(2) C6 0.081(3) 0.029(2) 0.055(3) 0.010(2) 0.033(2) 0.013(2) C7 0.091(3) 0.025(2) 0.062(3) -0.008(2) 0.036(3) -0.007(3) C8 0.072(3) 0.043(3) 0.054(3) -0.004(2) 0.023(3) -0.016(3) C9 0.055(3) 0.036(3) 0.044(2) 0.005(2) 0.023(2) 0.003(2) C10 0.054(2) 0.033(2) 0.028(2) 0.0055(18) 0.0168(19) 0.004(2) C11 0.094(4) 0.065(3) 0.046(3) 0.004(2) 0.029(3) 0.001(3) C12 0.121(5) 0.047(3) 0.043(3) 0.003(2) -0.003(3) -0.014(3) C13 0.057(3) 0.061(3) 0.060(3) 0.016(3) 0.020(2) 0.010(3) C14 0.082(3) 0.068(4) 0.064(3) 0.015(3) 0.014(3) 0.042(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 Cr1 N1 2.071(3) . ? Cr1 C10 2.091(4) . ? Cr1 Cl1 2.3638(13) 3_656 ? Cr1 Cl1 2.4362(13) . ? Cl1 Cr1 2.3638(13) 3_656 ? O1 C3 1.342(5) . ? O1 C2 1.456(6) . ? N1 C3 1.264(5) . ? N1 C1 1.493(5) . ? C1 C11 1.495(7) . ? C1 C12 1.512(6) . ? C1 C2 1.527(6) . ? C3 C4 1.519(6) . ? C4 C5 1.537(6) . ? C4 C13 1.549(7) . ? C4 C14 1.543(6) . ? C5 C6 1.393(6) . ? C5 C10 1.408(6) . ? C6 C7 1.348(7) . ? C7 C8 1.373(7) . ? C8 C9 1.392(6) . ? C9 C10 1.395(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 N1 Cr1 C10 87.20(14) . . ? N1 Cr1 Cl1 173.58(11) . 3_656 ? C10 Cr1 Cl1 94.82(11) . 3_656 ? N1 Cr1 Cl1 93.82(10) . . ? C10 Cr1 Cl1 171.55(12) . . ? Cl1 Cr1 Cl1 85.08(4) 3_656 . ? Cr1 Cl1 Cr1 94.92(4) 3_656 . ? C3 O1 C2 105.1(3) . . ? C3 N1 C1 108.5(3) . . ? C3 N1 Cr1 121.0(3) . . ? C1 N1 Cr1 129.1(3) . . ? N1 C1 C11 111.0(3) . . ? N1 C1 C12 109.0(4) . . ? C11 C1 C12 112.0(4) . . ? N1 C1 C2 100.8(3) . . ? C11 C1 C2 112.5(4) . . ? C12 C1 C2 110.9(4) . . ? O1 C2 C1 104.6(4) . . ? N1 C3 O1 117.1(4) . . ? N1 C3 C4 125.4(4) . . ? O1 C3 C4 117.4(4) . . ? C3 C4 C5 106.6(4) . . ? C3 C4 C13 108.2(4) . . ? C5 C4 C13 110.5(3) . . ? C3 C4 C14 109.8(4) . . ? C5 C4 C14 114.4(4) . . ? C13 C4 C14 107.3(4) . . ? C6 C5 C10 120.4(4) . . ? C6 C5 C4 121.1(4) . . ? C10 C5 C4 118.6(4) . . ? C7 C6 C5 122.0(4) . . ? C6 C7 C8 120.0(4) . . ? C7 C8 C9 118.7(4) . . ? C8 C9 C10 123.3(4) . . ? C9 C10 C5 115.7(4) . . ? C9 C10 Cr1 122.4(3) . . ? C5 C10 Cr1 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 23.42 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.058 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.078 #===end data_ev4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Fe(PhCMe2Ox)(7) _chemical_melting_point ? _chemical_formula_moiety 'C19 H23 Cl Fe N2 O, 0.5(C6 H6)' _chemical_formula_sum 'C22 H26 Cl Fe N2 O' _chemical_formula_weight 425.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.8720(7) _cell_length_b 9.0323(4) _cell_length_c 15.5493(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.904(3) _cell_angle_gamma 90.00 _cell_volume 2096.00(17) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2119 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 21.59 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7247 _exptl_absorpt_correction_T_max 0.9582 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _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 20134 _diffrn_reflns_av_R_equivalents 0.0814 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.68 _reflns_number_total 3968 _reflns_number_gt 2930 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0858P)^2^+0.8270P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3968 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0774 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1408 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _refine_ls_shift/su_max 0.022 _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 0.18595(3) 0.71274(4) 0.19236(3) 0.01646(11) Uani 1 1 d . . . Cl1 Cl 0.04423(5) 0.74754(9) 0.09229(5) 0.02688(19) Uani 1 1 d . . . O1 O 0.22129(17) 0.7604(3) 0.46785(16) 0.0391(6) Uani 1 1 d . . . N1 N 0.17843(19) 0.6959(3) 0.32120(18) 0.0315(7) Uani 1 1 d . . . N2 N 0.21320(18) 0.4986(3) 0.15810(18) 0.0335(7) Uani 1 1 d . . . C1 C 0.2972(2) 0.8329(4) 0.2293(2) 0.0333(8) Uani 1 1 d . . . C2 C 0.3565(2) 0.8287(4) 0.1804(2) 0.0349(9) Uani 1 1 d . . . H2A H 0.3405 0.7718 0.1258 0.042 Uiso 1 1 calc R . . C3 C 0.4374(2) 0.9038(4) 0.2078(3) 0.0433(10) Uani 1 1 d . . . H3A H 0.4749 0.9003 0.1714 0.052 Uiso 1 1 calc R . . C4 C 0.4634(2) 0.9840(4) 0.2885(3) 0.0427(10) Uani 1 1 d . . . H4A H 0.5188 1.0357 0.3083 0.051 Uiso 1 1 calc R . . C5 C 0.4077(2) 0.9875(4) 0.3398(3) 0.0392(9) Uani 1 1 d . . . H5A H 0.4258 1.0417 0.3954 0.047 Uiso 1 1 calc R . . C6 C 0.3257(2) 0.9141(4) 0.3125(2) 0.0318(8) Uani 1 1 d . . . C7 C 0.2636(2) 0.9335(4) 0.3694(2) 0.0353(9) Uani 1 1 d . . . C8 C 0.2207(2) 0.7878(4) 0.3828(2) 0.0307(8) Uani 1 1 d . . . C9 C 0.1308(2) 0.5906(4) 0.3634(2) 0.0340(8) Uani 1 1 d . . . C10 C 0.1825(3) 0.6135(4) 0.4645(2) 0.0402(9) Uani 1 1 d . . . H10A H 0.1420 0.6098 0.5009 0.048 Uiso 1 1 calc R . . H10B H 0.2298 0.5376 0.4878 0.048 Uiso 1 1 calc R . . C11 C 0.1359(3) 0.4328(4) 0.3331(3) 0.0500(11) Uani 1 1 d . . . H11A H 0.1046 0.4249 0.2670 0.075 Uiso 1 1 calc R . . H11B H 0.1077 0.3666 0.3652 0.075 Uiso 1 1 calc R . . H11C H 0.1989 0.4046 0.3473 0.075 Uiso 1 1 calc R . . C12 C 0.0344(2) 0.6442(5) 0.3382(3) 0.0518(11) Uani 1 1 d . . . H12A H 0.0339 0.7448 0.3617 0.078 Uiso 1 1 calc R . . H12B H 0.0013 0.5780 0.3652 0.078 Uiso 1 1 calc R . . H12C H 0.0059 0.6445 0.2715 0.078 Uiso 1 1 calc R . . C13 C 0.1846(3) 1.0350(4) 0.3161(3) 0.0466(10) Uani 1 1 d . . . H13A H 0.1531 0.9919 0.2559 0.070 Uiso 1 1 calc R . . H13B H 0.2076 1.1330 0.3085 0.070 Uiso 1 1 calc R . . H13C H 0.1431 1.0445 0.3502 0.070 Uiso 1 1 calc R . . C14 C 0.3108(3) 1.0018(5) 0.4634(3) 0.0520(11) Uani 1 1 d . . . H14A H 0.2680 1.0129 0.4959 0.078 Uiso 1 1 calc R . . H14B H 0.3347 1.0992 0.4560 0.078 Uiso 1 1 calc R . . H14C H 0.3601 0.9373 0.4987 0.078 Uiso 1 1 calc R . . C15 C 0.2960(2) 0.4451(4) 0.1991(2) 0.0370(9) Uani 1 1 d . . . H15A H 0.3402 0.5093 0.2379 0.044 Uiso 1 1 calc R . . C16 C 0.3204(3) 0.3022(4) 0.1880(3) 0.0413(10) Uani 1 1 d . . . H16A H 0.3799 0.2684 0.2180 0.050 Uiso 1 1 calc R . . C17 C 0.2562(3) 0.2094(4) 0.1321(3) 0.0436(10) Uani 1 1 d . . . H17A H 0.2702 0.1094 0.1237 0.052 Uiso 1 1 calc R . . C18 C 0.1724(3) 0.2631(4) 0.0892(3) 0.0434(10) Uani 1 1 d . . . H18A H 0.1274 0.2011 0.0497 0.052 Uiso 1 1 calc R . . C19 C 0.1527(2) 0.4084(4) 0.1033(2) 0.0362(9) Uani 1 1 d . . . H19A H 0.0939 0.4447 0.0727 0.043 Uiso 1 1 calc R . . C1S C 0.4266(3) 0.5689(5) 0.4415(3) 0.0595(13) Uani 1 1 d . . . H1SA H 0.3752 0.6159 0.4001 0.071 Uiso 1 1 calc R . . C2S C 0.5063(3) 0.6395(5) 0.4700(3) 0.0598(13) Uani 1 1 d . . . H2SA H 0.5111 0.7374 0.4498 0.072 Uiso 1 1 calc R . . C3S C 0.5796(3) 0.5701(5) 0.5275(3) 0.0640(14) Uani 1 1 d . . . H3SA H 0.6359 0.6191 0.5464 0.077 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0163(2) 0.0167(2) 0.01583(19) -0.00145(16) 0.00479(15) 0.00022(16) Cl1 0.0197(3) 0.0368(4) 0.0213(4) 0.0004(3) 0.0032(3) 0.0085(3) O1 0.0465(14) 0.0423(14) 0.0277(12) 0.0005(11) 0.0117(11) -0.0077(12) N1 0.0349(15) 0.0293(15) 0.0295(14) 0.0000(12) 0.0099(12) -0.0038(12) N2 0.0290(14) 0.0393(17) 0.0311(14) -0.0059(12) 0.0087(12) -0.0044(13) C1 0.0398(18) 0.0286(18) 0.0321(17) 0.0075(14) 0.0130(15) 0.0094(16) C2 0.0340(18) 0.037(2) 0.0328(17) 0.0071(15) 0.0102(15) 0.0025(16) C3 0.041(2) 0.046(2) 0.046(2) 0.0134(17) 0.0190(17) 0.0020(18) C4 0.0282(18) 0.041(2) 0.056(2) 0.0020(18) 0.0103(17) -0.0048(16) C5 0.0387(19) 0.034(2) 0.043(2) -0.0020(16) 0.0119(16) -0.0052(17) C6 0.0377(18) 0.0229(17) 0.0333(17) 0.0011(14) 0.0100(15) 0.0001(15) C7 0.0410(19) 0.0268(18) 0.0399(19) -0.0030(15) 0.0161(16) -0.0029(16) C8 0.0310(17) 0.0307(19) 0.0292(17) 0.0001(14) 0.0086(14) 0.0062(15) C9 0.0361(17) 0.0322(19) 0.0386(18) -0.0004(15) 0.0191(15) -0.0084(15) C10 0.049(2) 0.036(2) 0.0354(18) 0.0020(16) 0.0140(16) -0.0088(18) C11 0.063(2) 0.045(2) 0.051(2) -0.0057(18) 0.0301(19) -0.015(2) C12 0.0361(19) 0.062(3) 0.061(2) 0.003(2) 0.0205(18) -0.006(2) C13 0.053(2) 0.035(2) 0.059(2) 0.0015(18) 0.0293(19) 0.0075(18) C14 0.066(2) 0.047(2) 0.049(2) -0.0206(18) 0.027(2) -0.022(2) C15 0.0334(18) 0.037(2) 0.0375(19) -0.0016(16) 0.0084(15) -0.0043(16) C16 0.043(2) 0.035(2) 0.041(2) 0.0020(16) 0.0085(17) 0.0047(17) C17 0.051(2) 0.032(2) 0.043(2) -0.0029(17) 0.0110(18) 0.0012(18) C18 0.048(2) 0.036(2) 0.044(2) -0.0071(17) 0.0133(18) -0.0045(18) C19 0.0309(17) 0.039(2) 0.0361(18) -0.0014(16) 0.0076(15) 0.0013(16) C1S 0.060(3) 0.054(3) 0.053(3) -0.003(2) 0.004(2) 0.026(2) C2S 0.065(3) 0.044(2) 0.072(3) 0.007(2) 0.025(2) 0.010(2) C3S 0.047(2) 0.046(3) 0.093(3) -0.012(2) 0.016(2) 0.000(2) _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 C1 1.984(4) . ? Fe1 N1 2.053(3) . ? Fe1 N2 2.090(3) . ? Fe1 Cl1 2.2797(8) . ? O1 C8 1.343(4) . ? O1 C10 1.456(4) . ? N1 C8 1.272(4) . ? N1 C9 1.498(4) . ? N2 C19 1.325(4) . ? N2 C15 1.341(4) . ? C1 C2 1.397(5) . ? C1 C6 1.420(5) . ? C2 C3 1.386(5) . ? C3 C4 1.385(5) . ? C4 C5 1.377(5) . ? C5 C6 1.393(5) . ? C6 C7 1.543(5) . ? C7 C8 1.528(5) . ? C7 C14 1.527(5) . ? C7 C13 1.546(5) . ? C9 C11 1.512(5) . ? C9 C10 1.520(5) . ? C9 C12 1.523(5) . ? C15 C16 1.376(5) . ? C16 C17 1.376(5) . ? C17 C18 1.359(5) . ? C18 C19 1.384(5) . ? C1S C2S 1.351(6) . ? C1S C3S 1.360(7) 3_666 ? C2S C3S 1.356(6) . ? C3S C1S 1.360(7) 3_666 ? 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 C1 Fe1 N1 95.73(13) . . ? C1 Fe1 N2 109.82(13) . . ? N1 Fe1 N2 105.43(11) . . ? C1 Fe1 Cl1 134.14(10) . . ? N1 Fe1 Cl1 107.74(8) . . ? N2 Fe1 Cl1 101.26(7) . . ? C8 O1 C10 105.8(3) . . ? C8 N1 C9 107.5(3) . . ? C8 N1 Fe1 119.7(2) . . ? C9 N1 Fe1 132.9(2) . . ? C19 N2 C15 117.6(3) . . ? C19 N2 Fe1 124.4(2) . . ? C15 N2 Fe1 117.8(2) . . ? C2 C1 C6 116.5(3) . . ? C2 C1 Fe1 121.7(3) . . ? C6 C1 Fe1 121.4(3) . . ? C3 C2 C1 123.0(3) . . ? C4 C3 C2 119.5(4) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 C6 122.0(3) . . ? C5 C6 C1 119.8(3) . . ? C5 C6 C7 119.0(3) . . ? C1 C6 C7 121.0(3) . . ? C8 C7 C14 108.3(3) . . ? C8 C7 C6 112.4(3) . . ? C14 C7 C6 113.2(3) . . ? C8 C7 C13 105.5(3) . . ? C14 C7 C13 108.5(3) . . ? C6 C7 C13 108.6(3) . . ? N1 C8 O1 116.5(3) . . ? N1 C8 C7 127.2(3) . . ? O1 C8 C7 116.0(3) . . ? N1 C9 C11 111.9(3) . . ? N1 C9 C10 101.0(3) . . ? C11 C9 C10 112.6(3) . . ? N1 C9 C12 107.3(3) . . ? C11 C9 C12 112.1(3) . . ? C10 C9 C12 111.3(3) . . ? O1 C10 C9 103.5(3) . . ? N2 C15 C16 123.4(3) . . ? C17 C16 C15 118.2(3) . . ? C18 C17 C16 118.9(4) . . ? C17 C18 C19 119.8(4) . . ? N2 C19 C18 122.1(3) . . ? C2S C1S C3S 119.5(4) . 3_666 ? C3S C2S C1S 119.7(4) . . ? C2S C3S C1S 120.8(4) . 3_666 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.68 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.757 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.100 #===end