# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email buxh@nankai.edu.cn _publ_contact_author_name 'Xian-He Bu' _publ_author_name 'Xian-He Bu' data_x _database_code_depnum_ccdc_archive 'CCDC 821285' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H40 Fe5 N3 O24' _chemical_formula_weight 1238.01 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' 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 33.747(7) _cell_length_b 12.808(3) _cell_length_c 14.155(3) _cell_angle_alpha 90.00 _cell_angle_beta 102.27(3) _cell_angle_gamma 90.00 _cell_volume 5979(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.375 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2516 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7198 _exptl_absorpt_correction_T_max 0.7872 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30780 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0625 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6841 _reflns_number_gt 5224 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0892P)^2^+39.7320P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6841 _refine_ls_number_parameters 419 _refine_ls_number_restraints 361 _refine_ls_R_factor_all 0.0992 _refine_ls_R_factor_gt 0.0717 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1679 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.001 _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 0.5000 0.5000 0.0135(2) Uani 1 2 d S . . Fe2 Fe 0.48092(2) 0.73501(5) 0.35519(4) 0.01687(17) Uani 1 1 d U . . Fe3 Fe 0.28460(2) 0.81893(6) 0.00727(5) 0.0282(2) Uani 1 1 d . . . O1 O 0.43584(10) 0.5219(3) 0.4465(3) 0.0294(8) Uani 1 1 d . . . O2 O 0.42770(10) 0.6803(3) 0.3795(3) 0.0302(8) Uani 1 1 d . . . O3 O 0.30355(14) 0.7461(3) 0.1382(3) 0.0495(11) Uani 1 1 d . . . O4 O 0.25053(12) 0.6384(4) 0.1265(3) 0.0506(12) Uani 1 1 d . . . O5 O 0.25215(13) 0.4123(4) 0.4267(3) 0.0572(13) Uani 1 1 d . . . O6 O 0.30711(14) 0.3122(4) 0.4473(4) 0.0585(13) Uani 1 1 d . . . O7 O 0.54186(10) 0.6961(3) 0.3032(2) 0.0270(7) Uani 1 1 d U . . O8 O 0.51005(10) 0.5850(2) 0.3759(2) 0.0229(7) Uani 1 1 d . . . O9 O 0.49689(13) 0.3659(2) 0.4197(2) 0.0327(9) Uani 1 1 d . . . O10 O 0.49899(12) 0.2156(3) 0.5020(2) 0.0300(8) Uani 1 1 d . . . O11 O 0.48530(13) -0.1150(2) 0.3141(2) 0.0326(9) Uani 1 1 d . . . O12 O 0.32914(18) 0.9203(6) -0.0041(6) 0.105(2) Uani 1 1 d . . . C1 C 0.37007(14) 0.5727(4) 0.3671(4) 0.0288(11) Uani 1 1 d . . . C2 C 0.34780(16) 0.6330(4) 0.2916(4) 0.0315(11) Uani 1 1 d . . . H2 H 0.3605 0.6870 0.2657 0.038 Uiso 1 1 calc R . . C3 C 0.30745(16) 0.6133(4) 0.2553(4) 0.0331(12) Uani 1 1 d . . . C4 C 0.28754(17) 0.5369(5) 0.2987(4) 0.0388(13) Uani 1 1 d . . . H4 H 0.2598 0.5262 0.2771 0.047 Uiso 1 1 calc R . . C5 C 0.30928(17) 0.4767(5) 0.3744(4) 0.0389(13) Uani 1 1 d . . . C6 C 0.35087(15) 0.4931(4) 0.4063(4) 0.0322(12) Uani 1 1 d . . . H6 H 0.3658 0.4504 0.4541 0.039 Uiso 1 1 calc R . . C7 C 0.41532(14) 0.5934(4) 0.4020(3) 0.0230(10) Uani 1 1 d . . . C8 C 0.28514(17) 0.6713(5) 0.1664(4) 0.0368(13) Uani 1 1 d . . . C9 C 0.28769(18) 0.3933(5) 0.4200(4) 0.0432(15) Uani 1 1 d . . . C10 C 0.53957(15) 0.6056(4) 0.3371(3) 0.0219(9) Uani 1 1 d . . . C11 C 0.56949(19) 0.5234(5) 0.3268(5) 0.0471(16) Uani 1 1 d . . . H11A H 0.5677 0.4671 0.3704 0.071 Uiso 1 1 calc R . . H11B H 0.5963 0.5524 0.3418 0.071 Uiso 1 1 calc R . . H11C H 0.5638 0.4978 0.2616 0.071 Uiso 1 1 calc R . . C12 C 0.49791(16) 0.2095(3) 0.3348(3) 0.0226(10) Uani 1 1 d . . . C13 C 0.49724(17) 0.1001(3) 0.3336(3) 0.0266(11) Uani 1 1 d . . . H13 H 0.4949 0.0635 0.3890 0.032 Uiso 1 1 calc R . . C14 C 0.5000 0.0457(5) 0.2500 0.0257(15) Uani 1 2 d S . . C15 C 0.5000 0.2630(5) 0.2500 0.0256(15) Uani 1 2 d S . . H15 H 0.5000 0.3356 0.2500 0.031 Uiso 1 2 calc SR . . C16 C 0.49768(15) 0.2680(4) 0.4261(3) 0.0232(10) Uani 1 1 d . . . C17 C 0.5000 -0.0710(5) 0.2500 0.0264(15) Uani 1 2 d S . . N1 N 0.3860(7) 1.006(2) -0.020(3) 0.171(5) Uani 0.50 1 d PDU A 1 C18 C 0.3621(10) 0.918(3) -0.003(5) 0.173(5) Uani 0.50 1 d PDU A 1 C19 C 0.3879(8) 0.838(3) 0.059(3) 0.170(6) Uani 0.50 1 d PDU A 1 H19A H 0.3708 0.7848 0.0770 0.254 Uiso 0.50 1 calc PR A 1 H19B H 0.4031 0.8710 0.1165 0.254 Uiso 0.50 1 calc PR A 1 H19C H 0.4062 0.8071 0.0240 0.254 Uiso 0.50 1 calc PR A 1 C20 C 0.4289(7) 0.994(3) -0.018(3) 0.177(5) Uani 0.50 1 d PDU A 1 H20A H 0.4368 0.9230 -0.0026 0.265 Uiso 0.50 1 calc PR A 1 H20B H 0.4442 1.0394 0.0306 0.265 Uiso 0.50 1 calc PR A 1 H20C H 0.4341 1.0119 -0.0798 0.265 Uiso 0.50 1 calc PR A 1 C21 C 0.3699(9) 1.095(2) -0.081(3) 0.184(6) Uani 0.50 1 d PDU A 1 H21A H 0.3492 1.1291 -0.0549 0.276 Uiso 0.50 1 calc PR A 1 H21B H 0.3586 1.0711 -0.1452 0.276 Uiso 0.50 1 calc PR A 1 H21C H 0.3914 1.1439 -0.0827 0.276 Uiso 0.50 1 calc PR A 1 N1B N 0.3762(6) 1.011(3) -0.057(3) 0.176(5) Uani 0.50 1 d PDU A 2 C18B C 0.3646(10) 0.933(4) 0.004(4) 0.170(5) Uani 0.50 1 d PDU A 2 C19B C 0.4020(9) 0.870(3) 0.044(3) 0.183(6) Uani 0.50 1 d PDU A 2 H19D H 0.3954 0.8146 0.0839 0.274 Uiso 0.50 1 calc PR A 2 H19E H 0.4221 0.9146 0.0830 0.274 Uiso 0.50 1 calc PR A 2 H19F H 0.4126 0.8413 -0.0077 0.274 Uiso 0.50 1 calc PR A 2 C20B C 0.4172(7) 1.049(3) -0.053(3) 0.176(5) Uani 0.50 1 d PDU A 2 H20D H 0.4365 0.9984 -0.0217 0.264 Uiso 0.50 1 calc PR A 2 H20E H 0.4211 1.1135 -0.0182 0.264 Uiso 0.50 1 calc PR A 2 H20F H 0.4210 1.0602 -0.1180 0.264 Uiso 0.50 1 calc PR A 2 C21B C 0.3427(8) 1.076(3) -0.108(3) 0.185(6) Uani 0.50 1 d PDU A 2 H21D H 0.3175 1.0398 -0.1107 0.277 Uiso 0.50 1 calc PR A 2 H21E H 0.3461 1.0889 -0.1726 0.277 Uiso 0.50 1 calc PR A 2 H21F H 0.3425 1.1405 -0.0744 0.277 Uiso 0.50 1 calc PR A 2 N2 N 0.3517(16) 0.203(4) 0.205(4) 0.165(11) Uani 0.25 1 d PDU B 1 H2A H 0.3656 0.1594 0.1734 0.198 Uiso 0.25 1 calc PR B 1 H2B H 0.3396 0.1616 0.2416 0.198 Uiso 0.25 1 calc PR B 1 C22 C 0.3828(17) 0.259(5) 0.273(4) 0.162(12) Uani 0.25 1 d PDU B 1 H22A H 0.3746 0.3302 0.2767 0.243 Uiso 0.25 1 calc PR B 1 H22B H 0.4079 0.2564 0.2514 0.243 Uiso 0.25 1 calc PR B 1 H22C H 0.3863 0.2269 0.3354 0.243 Uiso 0.25 1 calc PR B 1 C23 C 0.3189(17) 0.242(5) 0.130(4) 0.167(12) Uani 0.25 1 d PDU B 1 H23A H 0.3062 0.2998 0.1554 0.251 Uiso 0.25 1 calc PR B 1 H23B H 0.2993 0.1878 0.1103 0.251 Uiso 0.25 1 calc PR B 1 H23C H 0.3294 0.2650 0.0759 0.251 Uiso 0.25 1 calc PR B 1 N2B N 0.3635(17) 0.245(4) 0.173(4) 0.169(11) Uani 0.25 1 d PDU C 2 C22B C 0.3929(18) 0.228(5) 0.113(5) 0.167(12) Uani 0.25 1 d PDU C 2 H22D H 0.4068 0.1635 0.1310 0.250 Uiso 0.25 1 calc PR C 2 H22E H 0.4120 0.2845 0.1223 0.250 Uiso 0.25 1 calc PR C 2 H22F H 0.3791 0.2252 0.0465 0.250 Uiso 0.25 1 calc PR C 2 C23B C 0.3416(19) 0.344(5) 0.156(5) 0.170(12) Uani 0.25 1 d PDU C 2 H23D H 0.3226 0.3485 0.1977 0.256 Uiso 0.25 1 calc PR C 2 H23E H 0.3273 0.3471 0.0899 0.256 Uiso 0.25 1 calc PR C 2 H23F H 0.3605 0.4006 0.1695 0.256 Uiso 0.25 1 calc PR C 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 0.0213(4) 0.0076(4) 0.0117(4) -0.0005(3) 0.0037(3) 0.0012(3) Fe2 0.0300(4) 0.0092(3) 0.0133(3) 0.0009(2) 0.0087(2) -0.0002(2) Fe3 0.0217(4) 0.0314(4) 0.0299(4) 0.0033(3) 0.0023(3) 0.0033(3) O1 0.0187(16) 0.0329(19) 0.0342(19) 0.0156(15) 0.0002(14) 0.0029(14) O2 0.0252(18) 0.0275(19) 0.040(2) 0.0058(15) 0.0118(15) -0.0019(14) O3 0.051(3) 0.050(3) 0.044(2) 0.020(2) 0.000(2) 0.005(2) O4 0.035(2) 0.071(3) 0.038(2) 0.017(2) -0.0103(18) 0.006(2) O5 0.039(2) 0.070(3) 0.063(3) 0.010(2) 0.011(2) -0.021(2) O6 0.049(3) 0.056(3) 0.066(3) 0.023(3) 0.004(2) -0.019(2) O7 0.0324(16) 0.0266(18) 0.0245(17) 0.0057(14) 0.0121(14) -0.0018(14) O8 0.0337(18) 0.0196(16) 0.0194(15) 0.0073(13) 0.0145(14) 0.0064(14) O9 0.073(3) 0.0109(15) 0.0141(16) -0.0056(12) 0.0096(16) 0.0009(16) O10 0.064(2) 0.0152(16) 0.0119(14) -0.0003(12) 0.0098(15) -0.0035(16) O11 0.074(3) 0.0086(15) 0.0205(16) 0.0019(13) 0.0219(17) -0.0007(16) O12 0.054(4) 0.110(5) 0.152(7) 0.015(5) 0.025(4) -0.042(4) C1 0.021(2) 0.036(3) 0.028(2) 0.007(2) 0.002(2) 0.000(2) C2 0.031(3) 0.037(3) 0.027(3) 0.012(2) 0.007(2) -0.002(2) C3 0.028(3) 0.041(3) 0.029(3) 0.008(2) 0.004(2) 0.007(2) C4 0.027(3) 0.049(3) 0.039(3) 0.010(3) 0.005(2) -0.003(2) C5 0.035(3) 0.041(3) 0.040(3) 0.012(3) 0.005(2) -0.008(2) C6 0.024(2) 0.035(3) 0.034(3) 0.013(2) -0.001(2) -0.003(2) C7 0.020(2) 0.033(3) 0.017(2) 0.0015(19) 0.0061(18) -0.0016(19) C8 0.033(3) 0.047(3) 0.030(3) 0.010(2) 0.007(2) 0.015(3) C9 0.032(3) 0.056(4) 0.037(3) 0.009(3) -0.004(2) -0.020(3) C10 0.032(3) 0.023(2) 0.0106(19) -0.0005(17) 0.0043(18) 0.0023(19) C11 0.050(4) 0.049(4) 0.050(4) 0.017(3) 0.029(3) 0.022(3) C12 0.048(3) 0.013(2) 0.0083(19) -0.0023(16) 0.0075(19) -0.0004(19) C13 0.056(3) 0.013(2) 0.014(2) 0.0018(17) 0.014(2) -0.001(2) C14 0.051(4) 0.011(3) 0.017(3) 0.000 0.013(3) 0.000 C15 0.051(4) 0.007(3) 0.019(3) 0.000 0.007(3) 0.000 C16 0.038(3) 0.016(2) 0.017(2) -0.0039(17) 0.0103(19) -0.001(2) C17 0.053(4) 0.009(3) 0.018(3) 0.000 0.010(3) 0.000 N1 0.091(7) 0.169(10) 0.239(12) 0.090(9) 0.002(8) -0.047(7) C18 0.092(7) 0.172(10) 0.239(12) 0.086(9) 0.002(8) -0.043(7) C19 0.086(9) 0.168(12) 0.240(13) 0.099(10) 0.001(9) -0.041(9) C20 0.091(8) 0.177(11) 0.246(13) 0.084(10) 0.000(9) -0.037(8) C21 0.107(9) 0.175(12) 0.251(13) 0.091(10) -0.007(9) -0.038(9) N1B 0.097(7) 0.172(10) 0.244(13) 0.085(9) 0.002(8) -0.046(7) C18B 0.090(7) 0.168(10) 0.238(12) 0.088(9) 0.003(8) -0.048(7) C19B 0.102(9) 0.179(12) 0.248(13) 0.084(10) -0.006(9) -0.033(8) C20B 0.093(8) 0.176(11) 0.246(13) 0.089(10) 0.007(9) -0.049(8) C21B 0.107(9) 0.179(11) 0.250(13) 0.088(10) -0.003(9) -0.039(9) N2 0.15(3) 0.16(2) 0.21(3) 0.03(2) 0.11(2) -0.003(19) C22 0.14(3) 0.16(2) 0.21(3) 0.03(2) 0.11(2) -0.002(19) C23 0.15(3) 0.16(2) 0.22(3) 0.03(2) 0.11(2) -0.009(19) N2B 0.16(2) 0.16(2) 0.22(3) 0.03(2) 0.10(2) 0.000(19) C22B 0.15(3) 0.16(2) 0.22(3) 0.03(2) 0.10(2) -0.004(19) C23B 0.15(3) 0.17(2) 0.22(3) 0.02(2) 0.11(2) -0.005(19) _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 O9 2.049(3) . ? Fe1 O9 2.049(3) 5_666 ? Fe1 O8 2.153(3) 5_666 ? Fe1 O8 2.153(3) . ? Fe1 O1 2.155(3) . ? Fe1 O1 2.155(3) 5_666 ? Fe2 O11 2.022(3) 1_565 ? Fe2 O2 2.024(3) . ? Fe2 O10 2.089(3) 5_666 ? Fe2 O8 2.150(3) . ? Fe2 O7 2.265(3) 2_655 ? Fe2 O7 2.380(3) . ? Fe3 O12 2.019(6) . ? Fe3 O3 2.052(4) . ? Fe3 O5 2.082(4) 4 ? Fe3 O4 2.082(4) 7_565 ? Fe3 O6 2.096(4) 6_565 ? Fe3 Fe3 2.8998(15) 7_565 ? O1 C7 1.237(6) . ? O2 C7 1.253(6) . ? O3 C8 1.252(7) . ? O4 C8 1.257(7) . ? O4 Fe3 2.082(4) 7_565 ? O5 C9 1.247(7) . ? O5 Fe3 2.082(4) 4_545 ? O6 C9 1.245(8) . ? O6 Fe3 2.096(4) 6_566 ? O7 C10 1.263(6) . ? O7 Fe2 2.265(3) 2_655 ? O8 C10 1.264(6) . ? O9 C16 1.257(5) . ? O10 C16 1.260(6) . ? O10 Fe2 2.089(3) 5_666 ? O11 C17 1.257(4) . ? O11 Fe2 2.022(3) 1_545 ? O12 C18 1.11(4) . ? O12 C18B 1.19(3) . ? C1 C6 1.386(7) . ? C1 C2 1.400(7) . ? C1 C7 1.525(6) . ? C2 C3 1.373(7) . ? C2 H2 0.9300 . ? C3 C4 1.401(8) . ? C3 C8 1.517(7) . ? C4 C5 1.395(8) . ? C4 H4 0.9300 . ? C5 C6 1.396(7) . ? C5 C9 1.513(8) . ? C6 H6 0.9300 . ? C10 C11 1.487(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C15 1.396(5) . ? C12 C13 1.403(6) . ? C12 C16 1.495(6) . ? C13 C14 1.393(5) . ? C13 H13 0.9300 . ? C14 C13 1.393(5) 2_655 ? C14 C17 1.494(9) . ? C15 C12 1.396(5) 2_655 ? C15 H15 0.9300 . ? C17 O11 1.257(4) 2_655 ? N1 C18 1.433(10) . ? N1 C20 1.451(10) . ? N1 C21 1.467(10) . ? C18 C19 1.505(10) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? N1B C18B 1.433(10) . ? N1B C20B 1.459(10) . ? N1B C21B 1.463(10) . ? C18B C19B 1.502(10) . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? C20B H20D 0.9600 . ? C20B H20E 0.9600 . ? C20B H20F 0.9600 . ? C21B H21D 0.9600 . ? C21B H21E 0.9600 . ? C21B H21F 0.9600 . ? N2 C23 1.448(10) . ? N2 C22 1.454(10) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? N2B C22B 1.453(10) . ? N2B C23B 1.458(10) . ? C22B H22D 0.9600 . ? C22B H22E 0.9600 . ? C22B H22F 0.9600 . ? C23B H23D 0.9600 . ? C23B H23E 0.9600 . ? C23B H23F 0.9600 . ? 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 O9 Fe1 O9 180.0 . 5_666 ? O9 Fe1 O8 91.72(13) . 5_666 ? O9 Fe1 O8 88.28(12) 5_666 5_666 ? O9 Fe1 O8 88.28(12) . . ? O9 Fe1 O8 91.72(13) 5_666 . ? O8 Fe1 O8 180.0 5_666 . ? O9 Fe1 O1 89.14(15) . . ? O9 Fe1 O1 90.86(15) 5_666 . ? O8 Fe1 O1 91.81(13) 5_666 . ? O8 Fe1 O1 88.19(13) . . ? O9 Fe1 O1 90.86(15) . 5_666 ? O9 Fe1 O1 89.14(15) 5_666 5_666 ? O8 Fe1 O1 88.19(13) 5_666 5_666 ? O8 Fe1 O1 91.81(13) . 5_666 ? O1 Fe1 O1 180.0 . 5_666 ? O11 Fe2 O2 119.99(16) 1_565 . ? O11 Fe2 O10 87.82(13) 1_565 5_666 ? O2 Fe2 O10 93.29(15) . 5_666 ? O11 Fe2 O8 146.03(15) 1_565 . ? O2 Fe2 O8 93.64(13) . . ? O10 Fe2 O8 95.36(13) 5_666 . ? O11 Fe2 O7 87.41(13) 1_565 2_655 ? O2 Fe2 O7 88.02(14) . 2_655 ? O10 Fe2 O7 175.07(13) 5_666 2_655 ? O8 Fe2 O7 89.30(12) . 2_655 ? O11 Fe2 O7 89.38(14) 1_565 . ? O2 Fe2 O7 146.74(13) . . ? O10 Fe2 O7 103.80(14) 5_666 . ? O8 Fe2 O7 56.97(11) . . ? O7 Fe2 O7 77.39(14) 2_655 . ? O12 Fe3 O3 105.7(3) . . ? O12 Fe3 O5 101.0(3) . 4 ? O3 Fe3 O5 87.52(19) . 4 ? O12 Fe3 O4 92.8(3) . 7_565 ? O3 Fe3 O4 161.57(18) . 7_565 ? O5 Fe3 O4 88.78(19) 4 7_565 ? O12 Fe3 O6 98.2(3) . 6_565 ? O3 Fe3 O6 86.1(2) . 6_565 ? O5 Fe3 O6 160.7(2) 4 6_565 ? O4 Fe3 O6 91.6(2) 7_565 6_565 ? O12 Fe3 Fe3 171.2(2) . 7_565 ? O3 Fe3 Fe3 83.05(14) . 7_565 ? O5 Fe3 Fe3 80.46(15) 4 7_565 ? O4 Fe3 Fe3 78.53(13) 7_565 7_565 ? O6 Fe3 Fe3 80.73(15) 6_565 7_565 ? C7 O1 Fe1 133.4(3) . . ? C7 O2 Fe2 134.9(3) . . ? C8 O3 Fe3 123.7(4) . . ? C8 O4 Fe3 128.0(4) . 7_565 ? C9 O5 Fe3 126.6(4) . 4_545 ? C9 O6 Fe3 125.6(4) . 6_566 ? C10 O7 Fe2 122.8(3) . 2_655 ? C10 O7 Fe2 87.0(3) . . ? Fe2 O7 Fe2 97.25(13) 2_655 . ? C10 O8 Fe2 97.7(3) . . ? C10 O8 Fe1 137.4(3) . . ? Fe2 O8 Fe1 114.62(13) . . ? C16 O9 Fe1 143.0(3) . . ? C16 O10 Fe2 127.6(3) . 5_666 ? C17 O11 Fe2 134.3(3) . 1_545 ? C18 O12 C18B 10(6) . . ? C18 O12 Fe3 138.1(19) . . ? C18B O12 Fe3 146.0(18) . . ? C6 C1 C2 119.4(5) . . ? C6 C1 C7 121.3(4) . . ? C2 C1 C7 119.3(4) . . ? C3 C2 C1 120.9(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 C8 119.9(5) . . ? C4 C3 C8 120.4(5) . . ? C5 C4 C3 120.0(5) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.6(5) . . ? C4 C5 C9 119.7(5) . . ? C6 C5 C9 120.7(5) . . ? C1 C6 C5 120.3(5) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? O1 C7 O2 127.3(4) . . ? O1 C7 C1 116.8(4) . . ? O2 C7 C1 115.9(4) . . ? O3 C8 O4 126.2(5) . . ? O3 C8 C3 116.5(5) . . ? O4 C8 C3 117.3(5) . . ? O6 C9 O5 126.2(6) . . ? O6 C9 C5 116.9(5) . . ? O5 C9 C5 116.9(6) . . ? O7 C10 O8 118.3(4) . . ? O7 C10 C11 121.0(4) . . ? O8 C10 C11 120.6(4) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C13 118.9(4) . . ? C15 C12 C16 120.5(4) . . ? C13 C12 C16 120.5(4) . . ? C14 C13 C12 120.4(4) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C13 120.0(6) . 2_655 ? C13 C14 C17 120.0(3) . . ? C13 C14 C17 120.0(3) 2_655 . ? C12 C15 C12 121.3(6) 2_655 . ? C12 C15 H15 119.4 2_655 . ? C12 C15 H15 119.4 . . ? O9 C16 O10 126.0(4) . . ? O9 C16 C12 116.2(4) . . ? O10 C16 C12 117.7(4) . . ? O11 C17 O11 126.7(6) . 2_655 ? O11 C17 C14 116.7(3) . . ? O11 C17 C14 116.7(3) 2_655 . ? C18 N1 C20 120(3) . . ? C18 N1 C21 124(2) . . ? C20 N1 C21 110(2) . . ? O12 C18 N1 125(3) . . ? O12 C18 C19 119(3) . . ? N1 C18 C19 111(2) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 H20A 109.5 . . ? N1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 C21 H21A 109.5 . . ? N1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18B N1B C20B 126(2) . . ? C18B N1B C21B 114(2) . . ? C20B N1B C21B 117(2) . . ? O12 C18B N1B 116(3) . . ? O12 C18B C19B 136(2) . . ? N1B C18B C19B 107(3) . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? N1B C20B H20D 109.5 . . ? N1B C20B H20E 109.5 . . ? H20D C20B H20E 109.5 . . ? N1B C20B H20F 109.5 . . ? H20D C20B H20F 109.5 . . ? H20E C20B H20F 109.5 . . ? N1B C21B H21D 109.5 . . ? N1B C21B H21E 109.5 . . ? H21D C21B H21E 109.5 . . ? N1B C21B H21F 109.5 . . ? H21D C21B H21F 109.5 . . ? H21E C21B H21F 109.5 . . ? C23 N2 C22 130(6) . . ? C23 N2 H2A 104.8 . . ? C22 N2 H2A 104.8 . . ? C23 N2 H2B 104.8 . . ? C22 N2 H2B 104.8 . . ? H2A N2 H2B 105.8 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N2 C23 H23A 109.5 . . ? N2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22B N2B C23B 115(5) . . ? N2B C22B H22D 109.5 . . ? N2B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? N2B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? N2B C23B H23D 109.5 . . ? N2B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? N2B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.829 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.122 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.250 0.250 1.000 92 0 ' ' 2 0.750 0.250 0.500 92 0 ' ' 3 0.250 0.750 0.500 92 0 ' ' 4 0.750 0.750 1.000 92 0 ' ' _platon_squeeze_details ; In order to subtract the contribution from the disordered solvent molecules, the SQUEEZE command was applied, which gave a new HKL file. There is 0 residual electron in four voids per unit cell. This residual electron density show that there is no orther solvent molecule. So SQUEEZE removed none of solvent molecule per formula unit. This value calculated based upon volume/count_electrons analysis, combining with elemental analyses, and TG analyses. See ref. O.V. Dolomanov, D. B. Cordes, N. R. Champness, A. J. Blake, L. R. Hanton, G. B. Jameson, M. Schroder and C. Wilson. Chem. Commun., 2004, 642. ; ###END