Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Antitpin, Mikhail Yu' 'Belsky, Vitaly K.' 'Palchik, Aleksei V.' 'Strizhakova, Nataly G.' 'Varzatskii, Oleg A.' 'Voloshin, Yan Z.' 'Vorontsov, Ivan I.' 'Zavodnik, Valery E.' _publ_contact_author_name 'Prof Yan Z Voloshin' _publ_contact_author_address ; Karpov Institute of Physical Chemistry 10 Vorontsovo Pole Moscow 103064 RUSSIAN FEDERATION ; _publ_contact_author_email 'VOLOSHIN@CC.NIFHI.AC.RU' _publ_section_title ; Meridianally asymmetrical clathrochelate monoribbed-functionalized iron(II) alpha-dioximates: the pathways of the synthesis, structural and electrochemical features ; #------------------------------------------------------------------------ data_6 _database_code_CSD 163718 _audit_creation_method SHELXL _chemical_name_systematic ; 1,8-Bis(fluoroboro)-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19- hexaaza-4,5,11,12-tetraphenyl-17,18-dichlorobicyclo-[6.6.6]eicosa- 3,5,10,12,16,18-hexaene iron(II)x 2(C6H6) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H32 B2 Cl2 F2 Fe N6 O6' _chemical_formula_weight 903.11 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 14.754(2) _cell_length_b 10.3386(11) _cell_length_c 27.126(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.942(2) _cell_angle_gamma 90.00 _cell_volume 4137.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 110(1) _cell_measurement_reflns_used 116 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method ? _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 0.559 _exptl_absorpt_correction_type 'semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.7177335 _exptl_absorpt_correction_T_max 1.0000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Bruker SMART 1K CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45055 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 30.03 _reflns_number_total 12090 _reflns_number_observed 9142 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL PLUS 5.0' _computing_structure_refinement 'SHELXTL PLUS 5.0' _computing_molecular_graphics 'SHELXTL PLUS 5.0' _computing_publication_material 'SHELXTL PLUS 5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 9 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0804P)^2^+0.1263P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment isotropic _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12081 _refine_ls_number_parameters 678 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_obs 0.0426 _refine_ls_wR_factor_all 0.1270 _refine_ls_wR_factor_obs 0.1119 _refine_ls_goodness_of_fit_all 1.024 _refine_ls_goodness_of_fit_obs 1.068 _refine_ls_restrained_S_all 1.047 _refine_ls_restrained_S_obs 1.068 _refine_ls_shift/esd_max 0.004 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.254427(14) 0.30422(2) 0.097921(7) 0.01842(7) Uani 1 d . . Cl1 Cl 0.15064(3) 0.51313(4) -0.032614(14) 0.03112(10) Uani 1 d . . Cl2 Cl 0.37353(3) 0.51067(4) -0.027422(15) 0.03322(10) Uani 1 d . . F1 F -0.03746(6) 0.34856(9) 0.10093(3) 0.0272(2) Uani 1 d . . F2 F 0.54692(7) 0.26256(10) 0.09579(4) 0.0307(2) Uani 1 d . . B1 B 0.05401(12) 0.3341(2) 0.09983(6) 0.0226(3) Uani 1 d . . B2 B 0.45539(13) 0.2751(2) 0.09655(7) 0.0243(3) Uani 1 d . . O1 O 0.08355(7) 0.36172(11) 0.04850(4) 0.0238(2) Uani 1 d . . O2 O 0.43040(7) 0.38572(11) 0.06368(4) 0.0247(2) Uani 1 d . . O3 O 0.09468(7) 0.42905(11) 0.13483(4) 0.0233(2) Uani 1 d . . O4 O 0.42864(8) 0.29797(11) 0.14814(4) 0.0254(2) Uani 1 d . . O5 O 0.07660(7) 0.19951(10) 0.11436(4) 0.0236(2) Uani 1 d . . O6 O 0.41394(8) 0.15439(11) 0.07684(4) 0.0245(2) Uani 1 d . . N1 N 0.17564(9) 0.36649(12) 0.04654(4) 0.0206(2) Uani 1 d . . N2 N 0.33881(9) 0.39495(12) 0.05775(4) 0.0210(2) Uani 1 d . . N3 N 0.18589(9) 0.40851(12) 0.14169(4) 0.0204(2) Uani 1 d . . N4 N 0.33854(9) 0.32914(13) 0.15128(5) 0.0216(3) Uani 1 d . . N5 N 0.16670(9) 0.17155(12) 0.10800(4) 0.0208(2) Uani 1 d . . N6 N 0.32149(9) 0.15242(13) 0.08245(4) 0.0216(3) Uani 1 d . . C1 C 0.21120(11) 0.43700(15) 0.01227(5) 0.0229(3) Uani 1 d . . C2 C 0.30797(11) 0.44630(15) 0.01695(5) 0.0226(3) Uani 1 d . . C3 C 0.22095(11) 0.44064(15) 0.18452(5) 0.0219(3) Uani 1 d . . C4 C 0.31494(11) 0.40055(15) 0.18914(5) 0.0224(3) Uani 1 d . . C5 C 0.18770(11) 0.05035(15) 0.09922(5) 0.0218(3) Uani 1 d . . C6 C 0.28367(11) 0.03859(15) 0.08769(5) 0.0219(3) Uani 1 d . . C7 C 0.17345(12) 0.5112(2) 0.22383(6) 0.0273(3) Uani 1 d . . C8 C 0.17791(14) 0.4653(2) 0.27214(6) 0.0350(4) Uani 1 d . . H8 H 0.2037(16) 0.3865(24) 0.2785(8) 0.044(6) Uiso 1 d . . C9 C 0.1417(2) 0.5401(3) 0.30953(8) 0.0488(6) Uani 1 d . . H9 H 0.1484(18) 0.5012(24) 0.3409(10) 0.054(7) Uiso 1 d . . C10 C 0.1029(2) 0.6588(3) 0.29907(9) 0.0578(7) Uani 1 d . . H10 H 0.0858(22) 0.7142(31) 0.3240(12) 0.086(10) Uiso 1 d . . C11 C 0.0985(2) 0.7030(3) 0.25129(10) 0.0523(6) Uani 1 d . . H11 H 0.0753(19) 0.7776(27) 0.2420(10) 0.058(8) Uiso 1 d . . C12 C 0.13321(14) 0.6298(2) 0.21324(7) 0.0380(4) Uani 1 d . . H12 H 0.1304(17) 0.6618(24) 0.1810(9) 0.052(7) Uiso 1 d . . C13 C 0.37488(11) 0.4350(2) 0.23125(5) 0.0263(3) Uani 1 d . . C14 C 0.42364(13) 0.3387(2) 0.25563(7) 0.0348(4) Uani 1 d . . H14 H 0.4204(15) 0.2636(22) 0.2467(8) 0.034(6) Uiso 1 d . . C15 C 0.4737(2) 0.3686(3) 0.29800(8) 0.0464(5) Uani 1 d . . H15 H 0.5020(17) 0.3034(23) 0.3140(9) 0.046(7) Uiso 1 d . . C16 C 0.47601(15) 0.4938(2) 0.31582(7) 0.0451(5) Uani 1 d . . H16 H 0.5085(18) 0.5075(23) 0.3466(9) 0.054(7) Uiso 1 d . . C17 C 0.42888(14) 0.5901(2) 0.29151(7) 0.0393(4) Uani 1 d . . H17 H 0.4261(17) 0.6830(23) 0.3025(9) 0.048(7) Uiso 1 d . . C18 C 0.37792(13) 0.5616(2) 0.24932(6) 0.0309(4) Uani 1 d . . H18 H 0.3441(15) 0.6213(22) 0.2358(8) 0.036(6) Uiso 1 d . . C19 C 0.12354(11) -0.05900(15) 0.09965(6) 0.0238(3) Uani 1 d . . C20 C 0.12781(13) -0.1540(2) 0.06325(7) 0.0317(4) Uani 1 d . . H20 H 0.1679(14) -0.1432(19) 0.0387(7) 0.027(5) Uiso 1 d . . C21 C 0.06874(15) -0.2591(2) 0.06450(8) 0.0403(4) Uani 1 d . . H21 H 0.0723(17) -0.3221(25) 0.0415(9) 0.055(7) Uiso 1 d . . C22 C 0.00750(13) -0.2724(2) 0.10141(8) 0.0389(4) Uani 1 d . . H22 H -0.0307(18) -0.3476(25) 0.1018(9) 0.054(7) Uiso 1 d . . C23 C 0.00261(13) -0.1778(2) 0.13786(7) 0.0335(4) Uani 1 d . . H23 H -0.0385(16) -0.1896(21) 0.1654(8) 0.042(6) Uiso 1 d . . C24 C 0.05975(12) -0.0715(2) 0.13699(6) 0.0280(3) Uani 1 d . . H24 H 0.0548(15) -0.0048(20) 0.1627(8) 0.037(6) Uiso 1 d . . C25 C 0.33408(11) -0.08393(15) 0.08475(6) 0.0240(3) Uani 1 d . . C26 C 0.39632(13) -0.1031(2) 0.04720(6) 0.0309(4) Uani 1 d . . H26 H 0.4054(14) -0.0360(21) 0.0230(8) 0.035(5) Uiso 1 d . . C27 C 0.44624(14) -0.2162(2) 0.04534(8) 0.0385(4) Uani 1 d . . H27 H 0.4916(17) -0.2273(23) 0.0178(9) 0.050(7) Uiso 1 d . . C28 C 0.43444(14) -0.3109(2) 0.08073(8) 0.0380(4) Uani 1 d . . H28 H 0.4628(16) -0.3882(23) 0.0813(8) 0.046(6) Uiso 1 d . . C29 C 0.37165(14) -0.2944(2) 0.11729(7) 0.0339(4) Uani 1 d . . H29 H 0.3607(14) -0.3529(21) 0.1424(7) 0.034(5) Uiso 1 d . . C30 C 0.32113(12) -0.1807(2) 0.11964(6) 0.0273(3) Uani 1 d . . H30 H 0.2786(14) -0.1695(20) 0.1465(8) 0.033(5) Uiso 1 d . . C1S C 0.3172(2) 0.0010(4) -0.07376(13) 0.0813(10) Uani 1 d . . H1S H 0.3843(31) 0.0004(38) -0.0829(15) 0.119(14) Uiso 1 d . . C2S C 0.2661(2) -0.1037(3) -0.07349(10) 0.0648(8) Uani 1 d . . H2S H 0.2883(23) -0.1953(33) -0.0815(12) 0.095(11) Uiso 1 d . . C3S C 0.1769(2) -0.0981(3) -0.06174(9) 0.0576(7) Uani 1 d . . H3S H 0.1448(32) -0.1682(48) -0.0584(17) 0.150(18) Uiso 1 d . . C4S C 0.1393(2) 0.0176(3) -0.04943(8) 0.0574(7) Uani 1 d . . H4S H 0.0817(21) 0.0175(27) -0.0425(10) 0.063(8) Uiso 1 d . . C5S C 0.1894(3) 0.1260(3) -0.04902(13) 0.0863(12) Uani 1 d . . H5S H 0.1683(26) 0.2059(39) -0.0431(14) 0.108(13) Uiso 1 d . . C6S C 0.2798(3) 0.1180(5) -0.0622(2) 0.112(2) Uani 1 d . . H6S H 0.3069(32) 0.1670(42) -0.0602(17) 0.114(17) Uiso 1 d . . C7S C 0.1905(3) 0.0933(3) 0.24053(11) 0.0774(10) Uani 1 d . . H7S H 0.1439(32) 0.1461(49) 0.2099(18) 0.159(17) Uiso 1 d . . C8S C 0.1451(3) 0.0633(3) 0.28329(15) 0.0804(10) Uani 1 d . . H8S H 0.0786(33) 0.0770(43) 0.2898(17) 0.137(16) Uiso 1 d . . C9S C 0.1903(3) -0.0069(4) 0.32034(12) 0.0842(11) Uani 1 d . . H9S H 0.1657(24) -0.0330(35) 0.3499(13) 0.098(11) Uiso 1 d . . C10S C 0.2786(3) -0.0450(4) 0.31277(13) 0.0836(10) Uani 1 d . . H10S H 0.3129(32) -0.0955(48) 0.3347(18) 0.145(17) Uiso 1 d . . C11S C 0.3193(3) -0.0127(4) 0.26948(14) 0.0804(10) Uani 1 d . . H11S H 0.3772(26) -0.0415(36) 0.2662(13) 0.098(12) Uiso 1 d . . C12S C 0.2748(3) 0.0517(3) 0.23459(11) 0.0763(10) Uani 1 d . . H12S H 0.3027(24) 0.0786(35) 0.2009(13) 0.103(11) Uiso 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 0.01966(11) 0.01856(11) 0.01706(11) 0.00136(7) 0.00110(8) 0.00158(8) Cl1 0.0367(2) 0.0327(2) 0.0238(2) 0.00651(15) -0.0041(2) 0.0044(2) Cl2 0.0363(2) 0.0367(2) 0.0269(2) 0.0079(2) 0.0084(2) -0.0032(2) F1 0.0218(5) 0.0303(5) 0.0295(5) 0.0013(4) -0.0008(4) 0.0021(4) F2 0.0216(5) 0.0342(5) 0.0363(5) 0.0030(4) 0.0038(4) 0.0032(4) B1 0.0227(8) 0.0230(8) 0.0220(7) 0.0023(6) 0.0016(6) 0.0039(6) B2 0.0219(8) 0.0258(8) 0.0253(8) 0.0025(7) 0.0031(7) 0.0035(7) O1 0.0207(5) 0.0287(6) 0.0221(5) 0.0012(4) -0.0017(4) 0.0017(4) O2 0.0192(5) 0.0255(6) 0.0296(5) 0.0044(4) 0.0027(4) 0.0003(4) O3 0.0187(5) 0.0261(5) 0.0249(5) -0.0020(4) -0.0006(4) 0.0047(4) O4 0.0187(5) 0.0340(6) 0.0236(5) 0.0007(4) -0.0002(4) 0.0047(4) O5 0.0190(5) 0.0229(5) 0.0289(5) 0.0035(4) 0.0032(4) 0.0016(4) O6 0.0205(5) 0.0241(5) 0.0292(6) 0.0010(4) 0.0053(4) 0.0028(4) N1 0.0223(6) 0.0209(6) 0.0187(5) -0.0009(4) 0.0003(5) 0.0015(5) N2 0.0217(6) 0.0200(6) 0.0212(6) 0.0003(5) 0.0010(5) 0.0013(5) N3 0.0197(6) 0.0209(6) 0.0207(6) 0.0014(5) 0.0004(5) 0.0026(5) N4 0.0191(6) 0.0241(6) 0.0216(6) 0.0024(5) 0.0006(5) 0.0025(5) N5 0.0201(6) 0.0228(6) 0.0197(6) 0.0020(5) 0.0020(5) 0.0021(5) N6 0.0214(6) 0.0235(6) 0.0200(6) 0.0023(5) 0.0027(5) 0.0026(5) C1 0.0296(8) 0.0217(7) 0.0175(6) 0.0011(5) -0.0015(6) 0.0037(6) C2 0.0290(8) 0.0208(7) 0.0184(6) 0.0013(5) 0.0049(6) -0.0002(6) C3 0.0244(7) 0.0216(7) 0.0196(6) -0.0003(5) 0.0021(6) 0.0001(6) C4 0.0236(7) 0.0250(7) 0.0186(6) 0.0013(5) -0.0018(6) -0.0018(6) C5 0.0241(7) 0.0218(7) 0.0194(6) 0.0012(5) 0.0006(6) 0.0013(6) C6 0.0259(8) 0.0218(7) 0.0182(6) 0.0014(5) 0.0010(6) 0.0030(6) C7 0.0261(8) 0.0328(8) 0.0231(7) -0.0079(6) 0.0026(6) -0.0022(7) C8 0.0370(10) 0.0436(11) 0.0247(8) -0.0045(7) 0.0062(7) -0.0104(8) C9 0.0483(13) 0.070(2) 0.0290(9) -0.0169(10) 0.0151(9) -0.0216(11) C10 0.0469(13) 0.079(2) 0.0484(13) -0.0386(13) 0.0164(10) -0.0073(12) C11 0.0489(13) 0.0525(14) 0.0555(13) -0.0264(11) 0.0003(11) 0.0146(11) C12 0.0359(10) 0.0433(11) 0.0349(9) -0.0129(8) -0.0017(8) 0.0079(8) C13 0.0232(8) 0.0358(9) 0.0200(7) -0.0015(6) -0.0001(6) -0.0022(6) C14 0.0341(10) 0.0406(11) 0.0294(8) -0.0010(7) -0.0061(7) 0.0025(8) C15 0.0405(11) 0.0646(15) 0.0337(10) 0.0032(10) -0.0126(8) 0.0066(10) C16 0.0349(10) 0.0710(15) 0.0290(9) -0.0102(9) -0.0078(8) -0.0046(10) C17 0.0346(10) 0.0498(12) 0.0334(9) -0.0115(8) 0.0021(8) -0.0122(9) C18 0.0303(9) 0.0347(9) 0.0279(8) -0.0022(7) 0.0009(7) -0.0049(7) C19 0.0259(8) 0.0197(7) 0.0257(7) 0.0012(6) -0.0028(6) 0.0003(6) C20 0.0344(9) 0.0300(9) 0.0306(8) -0.0041(7) -0.0021(7) 0.0011(7) C21 0.0430(11) 0.0284(9) 0.0491(11) -0.0129(8) -0.0087(9) 0.0012(8) C22 0.0298(9) 0.0266(9) 0.0599(12) 0.0004(8) -0.0081(9) -0.0049(7) C23 0.0299(9) 0.0255(8) 0.0452(10) 0.0052(7) 0.0034(8) -0.0007(7) C24 0.0276(8) 0.0241(8) 0.0322(8) 0.0017(6) 0.0007(7) -0.0006(6) C25 0.0277(8) 0.0197(7) 0.0244(7) -0.0020(6) -0.0006(6) 0.0022(6) C26 0.0362(10) 0.0257(8) 0.0310(8) -0.0039(7) 0.0051(7) 0.0037(7) C27 0.0386(11) 0.0303(9) 0.0467(11) -0.0112(8) 0.0084(9) 0.0055(8) C28 0.0399(11) 0.0219(8) 0.0519(11) -0.0084(7) -0.0061(9) 0.0091(7) C29 0.0410(10) 0.0212(8) 0.0389(9) 0.0033(7) -0.0101(8) 0.0005(7) C30 0.0309(9) 0.0248(8) 0.0262(7) 0.0013(6) -0.0026(7) 0.0005(6) C1S 0.053(2) 0.115(3) 0.075(2) 0.011(2) -0.006(2) 0.009(2) C2S 0.070(2) 0.072(2) 0.0525(14) -0.0146(13) -0.0110(13) 0.030(2) C3S 0.077(2) 0.0498(14) 0.0453(12) 0.0083(10) -0.0140(12) -0.0009(13) C4S 0.054(2) 0.085(2) 0.0335(10) -0.0051(11) -0.0033(10) 0.0213(14) C5S 0.107(3) 0.057(2) 0.093(2) -0.038(2) -0.059(2) 0.035(2) C6S 0.099(3) 0.080(3) 0.155(4) 0.025(3) -0.073(3) -0.038(3) C7S 0.126(3) 0.052(2) 0.054(2) -0.0078(13) -0.022(2) -0.019(2) C8S 0.067(2) 0.068(2) 0.107(3) -0.034(2) -0.003(2) 0.000(2) C9S 0.109(3) 0.087(2) 0.058(2) -0.006(2) 0.039(2) -0.025(2) C10S 0.104(3) 0.076(2) 0.072(2) 0.022(2) 0.004(2) 0.007(2) C11S 0.070(2) 0.084(2) 0.088(2) 0.000(2) 0.027(2) -0.006(2) C12S 0.109(3) 0.068(2) 0.052(2) -0.0041(14) 0.016(2) -0.031(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 N6 1.9056(13) . ? Fe1 N3 1.9064(12) . ? Fe1 N4 1.9085(13) . ? Fe1 N5 1.9087(13) . ? Fe1 N1 1.9117(13) . ? Fe1 N2 1.9137(13) . ? Cl1 C1 1.692(2) . ? Cl2 C2 1.6928(15) . ? F1 B1 1.359(2) . ? F2 B2 1.357(2) . ? B1 O5 1.482(2) . ? B1 O3 1.486(2) . ? B1 O1 1.493(2) . ? B2 O4 1.479(2) . ? B2 O6 1.485(2) . ? B2 O2 1.493(2) . ? O1 N1 1.362(2) . ? O2 N2 1.362(2) . ? O3 N3 1.372(2) . ? O4 N4 1.372(2) . ? O5 N5 1.374(2) . ? O6 N6 1.375(2) . ? N1 C1 1.299(2) . ? N2 C2 1.303(2) . ? N3 C3 1.307(2) . ? N4 C4 1.316(2) . ? N5 C5 1.313(2) . ? N6 C6 1.311(2) . ? C1 C2 1.435(2) . ? C3 C4 1.451(2) . ? C3 C7 1.478(2) . ? C4 C13 1.477(2) . ? C5 C6 1.460(2) . ? C5 C19 1.475(2) . ? C6 C25 1.472(2) . ? C7 C12 1.390(3) . ? C7 C8 1.395(2) . ? C8 C9 1.389(3) . ? C9 C10 1.382(4) . ? C10 C11 1.375(4) . ? C11 C12 1.385(3) . ? C13 C14 1.389(3) . ? C13 C18 1.399(3) . ? C14 C15 1.391(3) . ? C15 C16 1.382(3) . ? C16 C17 1.376(3) . ? C17 C18 1.391(3) . ? C19 C20 1.395(2) . ? C19 C24 1.400(2) . ? C20 C21 1.394(3) . ? C21 C22 1.366(3) . ? C22 C23 1.393(3) . ? C23 C24 1.386(2) . ? C25 C30 1.392(2) . ? C25 C26 1.397(2) . ? C26 C27 1.383(3) . ? C27 C28 1.384(3) . ? C28 C29 1.379(3) . ? C29 C30 1.394(2) . ? C1S C2S 1.319(5) . ? C1S C6S 1.368(6) . ? C2S C3S 1.361(4) . ? C3S C4S 1.363(4) . ? C4S C5S 1.342(5) . ? C5S C6S 1.389(7) . ? C7S C12S 1.328(5) . ? C7S C8S 1.384(5) . ? C8S C9S 1.400(5) . ? C9S C10S 1.379(5) . ? C10S C11S 1.369(5) . ? C11S C12S 1.322(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Fe1 N3 152.32(5) . . ? N6 Fe1 N4 86.83(6) . . ? N3 Fe1 N4 78.25(5) . . ? N6 Fe1 N5 78.20(6) . . ? N3 Fe1 N5 87.09(5) . . ? N4 Fe1 N5 114.99(5) . . ? N6 Fe1 N1 115.37(5) . . ? N3 Fe1 N1 86.63(5) . . ? N4 Fe1 N1 152.55(6) . . ? N5 Fe1 N1 86.61(5) . . ? N6 Fe1 N2 86.18(5) . . ? N3 Fe1 N2 115.73(6) . . ? N4 Fe1 N2 86.83(6) . . ? N5 Fe1 N2 152.00(5) . . ? N1 Fe1 N2 79.24(6) . . ? F1 B1 O5 108.47(13) . . ? F1 B1 O3 107.70(13) . . ? O5 B1 O3 111.33(13) . . ? F1 B1 O1 107.73(13) . . ? O5 B1 O1 111.09(13) . . ? O3 B1 O1 110.38(13) . . ? F2 B2 O4 108.10(14) . . ? F2 B2 O6 108.55(13) . . ? O4 B2 O6 111.11(13) . . ? F2 B2 O2 107.47(13) . . ? O4 B2 O2 112.05(13) . . ? O6 B2 O2 109.42(13) . . ? N1 O1 B1 110.49(11) . . ? N2 O2 B2 111.05(11) . . ? N3 O3 B1 111.67(11) . . ? N4 O4 B2 111.73(12) . . ? N5 O5 B1 112.20(11) . . ? N6 O6 B2 112.07(11) . . ? C1 N1 O1 117.60(12) . . ? C1 N1 Fe1 117.58(11) . . ? O1 N1 Fe1 123.68(9) . . ? C2 N2 O2 117.46(12) . . ? C2 N2 Fe1 117.52(11) . . ? O2 N2 Fe1 123.50(9) . . ? C3 N3 O3 117.01(12) . . ? C3 N3 Fe1 119.42(11) . . ? O3 N3 Fe1 122.16(9) . . ? C4 N4 O4 116.70(13) . . ? C4 N4 Fe1 119.36(11) . . ? O4 N4 Fe1 122.68(9) . . ? C5 N5 O5 117.07(13) . . ? C5 N5 Fe1 119.81(11) . . ? O5 N5 Fe1 121.77(9) . . ? C6 N6 O6 116.74(13) . . ? C6 N6 Fe1 119.47(11) . . ? O6 N6 Fe1 122.13(10) . . ? N1 C1 C2 112.79(13) . . ? N1 C1 Cl1 124.14(13) . . ? C2 C1 Cl1 123.06(11) . . ? N2 C2 C1 112.41(13) . . ? N2 C2 Cl2 124.65(13) . . ? C1 C2 Cl2 122.88(11) . . ? N3 C3 C4 111.59(13) . . ? N3 C3 C7 125.54(14) . . ? C4 C3 C7 122.86(13) . . ? N4 C4 C3 110.95(13) . . ? N4 C4 C13 125.17(14) . . ? C3 C4 C13 123.87(13) . . ? N5 C5 C6 110.53(13) . . ? N5 C5 C19 125.21(14) . . ? C6 C5 C19 124.24(14) . . ? N6 C6 C5 111.37(13) . . ? N6 C6 C25 123.39(14) . . ? C5 C6 C25 125.17(14) . . ? C12 C7 C8 120.5(2) . . ? C12 C7 C3 119.5(2) . . ? C8 C7 C3 119.6(2) . . ? C9 C8 C7 118.9(2) . . ? C10 C9 C8 120.5(2) . . ? C11 C10 C9 120.1(2) . . ? C10 C11 C12 120.6(2) . . ? C11 C12 C7 119.3(2) . . ? C14 C13 C18 119.4(2) . . ? C14 C13 C4 119.6(2) . . ? C18 C13 C4 120.8(2) . . ? C13 C14 C15 119.9(2) . . ? C16 C15 C14 120.5(2) . . ? C17 C16 C15 120.0(2) . . ? C16 C17 C18 120.2(2) . . ? C17 C18 C13 120.0(2) . . ? C20 C19 C24 119.1(2) . . ? C20 C19 C5 119.85(15) . . ? C24 C19 C5 121.06(14) . . ? C21 C20 C19 119.7(2) . . ? C22 C21 C20 121.1(2) . . ? C21 C22 C23 119.5(2) . . ? C24 C23 C22 120.4(2) . . ? C23 C24 C19 120.1(2) . . ? C30 C25 C26 119.5(2) . . ? C30 C25 C6 120.41(14) . . ? C26 C25 C6 120.04(14) . . ? C27 C26 C25 120.2(2) . . ? C26 C27 C28 120.0(2) . . ? C29 C28 C27 120.3(2) . . ? C28 C29 C30 120.2(2) . . ? C25 C30 C29 119.7(2) . . ? C2S C1S C6S 119.4(4) . . ? C1S C2S C3S 121.5(3) . . ? C2S C3S C4S 119.6(3) . . ? C5S C4S C3S 120.6(3) . . ? C4S C5S C6S 118.6(3) . . ? C1S C6S C5S 120.4(4) . . ? C12S C7S C8S 119.8(3) . . ? C7S C8S C9S 119.1(3) . . ? C10S C9S C8S 118.7(3) . . ? C11S C10S C9S 119.1(4) . . ? C12S C11S C10S 121.1(4) . . ? C11S C12S C7S 122.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 B1 O1 N1 171.53(12) . . . . ? O5 B1 O1 N1 -69.8(2) . . . . ? O3 B1 O1 N1 54.2(2) . . . . ? F2 B2 O2 N2 172.67(12) . . . . ? O4 B2 O2 N2 -68.7(2) . . . . ? O6 B2 O2 N2 55.0(2) . . . . ? F1 B1 O3 N3 170.92(11) . . . . ? O5 B1 O3 N3 52.1(2) . . . . ? O1 B1 O3 N3 -71.72(15) . . . . ? F2 B2 O4 N4 171.75(12) . . . . ? O6 B2 O4 N4 -69.2(2) . . . . ? O2 B2 O4 N4 53.5(2) . . . . ? F1 B1 O5 N5 172.00(11) . . . . ? O3 B1 O5 N5 -69.7(2) . . . . ? O1 B1 O5 N5 53.8(2) . . . . ? F2 B2 O6 N6 171.90(11) . . . . ? O4 B2 O6 N6 53.2(2) . . . . ? O2 B2 O6 N6 -71.10(15) . . . . ? B1 O1 N1 C1 -153.07(13) . . . . ? B1 O1 N1 Fe1 14.4(2) . . . . ? N6 Fe1 N1 C1 -82.03(12) . . . . ? N3 Fe1 N1 C1 115.45(12) . . . . ? N4 Fe1 N1 C1 59.2(2) . . . . ? N5 Fe1 N1 C1 -157.27(12) . . . . ? N2 Fe1 N1 C1 -1.55(11) . . . . ? N6 Fe1 N1 O1 110.50(11) . . . . ? N3 Fe1 N1 O1 -52.03(11) . . . . ? N4 Fe1 N1 O1 -108.24(14) . . . . ? N5 Fe1 N1 O1 35.26(11) . . . . ? N2 Fe1 N1 O1 -169.02(12) . . . . ? B2 O2 N2 C2 -152.33(14) . . . . ? B2 O2 N2 Fe1 13.3(2) . . . . ? N6 Fe1 N2 C2 113.64(12) . . . . ? N3 Fe1 N2 C2 -84.00(12) . . . . ? N4 Fe1 N2 C2 -159.33(12) . . . . ? N5 Fe1 N2 C2 57.8(2) . . . . ? N1 Fe1 N2 C2 -3.10(11) . . . . ? N6 Fe1 N2 O2 -51.96(11) . . . . ? N3 Fe1 N2 O2 110.41(11) . . . . ? N4 Fe1 N2 O2 35.07(11) . . . . ? N5 Fe1 N2 O2 -107.75(14) . . . . ? N1 Fe1 N2 O2 -168.69(12) . . . . ? B1 O3 N3 C3 -150.17(13) . . . . ? B1 O3 N3 Fe1 16.2(2) . . . . ? N6 Fe1 N3 C3 55.5(2) . . . . ? N4 Fe1 N3 C3 -3.29(11) . . . . ? N5 Fe1 N3 C3 112.98(12) . . . . ? N1 Fe1 N3 C3 -160.25(12) . . . . ? N2 Fe1 N3 C3 -83.90(12) . . . . ? N6 Fe1 N3 O3 -110.53(14) . . . . ? N4 Fe1 N3 O3 -169.31(11) . . . . ? N5 Fe1 N3 O3 -53.05(11) . . . . ? N1 Fe1 N3 O3 33.73(11) . . . . ? N2 Fe1 N3 O3 110.07(11) . . . . ? B2 O4 N4 C4 -153.01(14) . . . . ? B2 O4 N4 Fe1 14.0(2) . . . . ? N6 Fe1 N4 C4 -157.81(12) . . . . ? N3 Fe1 N4 C4 -1.26(12) . . . . ? N5 Fe1 N4 C4 -82.39(13) . . . . ? N1 Fe1 N4 C4 56.7(2) . . . . ? N2 Fe1 N4 C4 115.85(12) . . . . ? N6 Fe1 N4 O4 35.48(11) . . . . ? N3 Fe1 N4 O4 -167.97(12) . . . . ? N5 Fe1 N4 O4 110.89(11) . . . . ? N1 Fe1 N4 O4 -110.04(14) . . . . ? N2 Fe1 N4 O4 -50.86(11) . . . . ? B1 O5 N5 C5 -151.97(13) . . . . ? B1 O5 N5 Fe1 14.7(2) . . . . ? N6 Fe1 N5 C5 -2.19(11) . . . . ? N3 Fe1 N5 C5 -158.60(12) . . . . ? N4 Fe1 N5 C5 -83.00(12) . . . . ? N1 Fe1 N5 C5 114.61(12) . . . . ? N2 Fe1 N5 C5 55.3(2) . . . . ? N6 Fe1 N5 O5 -168.49(11) . . . . ? N3 Fe1 N5 O5 35.10(11) . . . . ? N4 Fe1 N5 O5 110.70(11) . . . . ? N1 Fe1 N5 O5 -51.69(11) . . . . ? N2 Fe1 N5 O5 -111.04(13) . . . . ? B2 O6 N6 C6 -150.37(13) . . . . ? B2 O6 N6 Fe1 14.8(2) . . . . ? N3 Fe1 N6 C6 55.9(2) . . . . ? N4 Fe1 N6 C6 112.93(12) . . . . ? N5 Fe1 N6 C6 -3.41(11) . . . . ? N1 Fe1 N6 C6 -83.86(12) . . . . ? N2 Fe1 N6 C6 -160.04(12) . . . . ? N3 Fe1 N6 O6 -108.84(14) . . . . ? N4 Fe1 N6 O6 -51.85(11) . . . . ? N5 Fe1 N6 O6 -168.19(11) . . . . ? N1 Fe1 N6 O6 111.36(11) . . . . ? N2 Fe1 N6 O6 35.18(11) . . . . ? O1 N1 C1 C2 173.59(12) . . . . ? Fe1 N1 C1 C2 5.3(2) . . . . ? O1 N1 C1 Cl1 -5.1(2) . . . . ? Fe1 N1 C1 Cl1 -173.37(8) . . . . ? O2 N2 C2 C1 173.09(12) . . . . ? Fe1 N2 C2 C1 6.6(2) . . . . ? O2 N2 C2 Cl2 -4.0(2) . . . . ? Fe1 N2 C2 Cl2 -170.52(8) . . . . ? N1 C1 C2 N2 -7.6(2) . . . . ? Cl1 C1 C2 N2 171.14(11) . . . . ? N1 C1 C2 Cl2 169.61(11) . . . . ? Cl1 C1 C2 Cl2 -11.7(2) . . . . ? O3 N3 C3 C4 173.33(12) . . . . ? Fe1 N3 C3 C4 6.6(2) . . . . ? O3 N3 C3 C7 -7.8(2) . . . . ? Fe1 N3 C3 C7 -174.53(12) . . . . ? O4 N4 C4 C3 172.36(12) . . . . ? Fe1 N4 C4 C3 4.9(2) . . . . ? O4 N4 C4 C13 -8.3(2) . . . . ? Fe1 N4 C4 C13 -175.78(12) . . . . ? N3 C3 C4 N4 -7.0(2) . . . . ? C7 C3 C4 N4 174.05(14) . . . . ? N3 C3 C4 C13 173.58(14) . . . . ? C7 C3 C4 C13 -5.3(2) . . . . ? O5 N5 C5 C6 173.41(11) . . . . ? Fe1 N5 C5 C6 6.5(2) . . . . ? O5 N5 C5 C19 -5.2(2) . . . . ? Fe1 N5 C5 C19 -172.18(11) . . . . ? O6 N6 C6 C5 173.14(12) . . . . ? Fe1 N6 C6 C5 7.6(2) . . . . ? O6 N6 C6 C25 -3.9(2) . . . . ? Fe1 N6 C6 C25 -169.47(11) . . . . ? N5 C5 C6 N6 -8.6(2) . . . . ? C19 C5 C6 N6 170.08(13) . . . . ? N5 C5 C6 C25 168.36(14) . . . . ? C19 C5 C6 C25 -13.0(2) . . . . ? N3 C3 C7 C12 -54.9(2) . . . . ? C4 C3 C7 C12 123.8(2) . . . . ? N3 C3 C7 C8 132.0(2) . . . . ? C4 C3 C7 C8 -49.2(2) . . . . ? C12 C7 C8 C9 -0.2(3) . . . . ? C3 C7 C8 C9 172.8(2) . . . . ? C7 C8 C9 C10 -0.7(3) . . . . ? C8 C9 C10 C11 1.1(4) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C10 C11 C12 C7 -0.5(4) . . . . ? C8 C7 C12 C11 0.8(3) . . . . ? C3 C7 C12 C11 -172.2(2) . . . . ? N4 C4 C13 C14 -50.0(2) . . . . ? C3 C4 C13 C14 129.3(2) . . . . ? N4 C4 C13 C18 135.0(2) . . . . ? C3 C4 C13 C18 -45.8(2) . . . . ? C18 C13 C14 C15 0.9(3) . . . . ? C4 C13 C14 C15 -174.2(2) . . . . ? C13 C14 C15 C16 -0.6(3) . . . . ? C14 C15 C16 C17 -0.3(3) . . . . ? C15 C16 C17 C18 0.8(3) . . . . ? C16 C17 C18 C13 -0.4(3) . . . . ? C14 C13 C18 C17 -0.5(3) . . . . ? C4 C13 C18 C17 174.6(2) . . . . ? N5 C5 C19 C20 138.0(2) . . . . ? C6 C5 C19 C20 -40.5(2) . . . . ? N5 C5 C19 C24 -44.0(2) . . . . ? C6 C5 C19 C24 137.6(2) . . . . ? C24 C19 C20 C21 0.2(3) . . . . ? C5 C19 C20 C21 178.3(2) . . . . ? C19 C20 C21 C22 -1.3(3) . . . . ? C20 C21 C22 C23 1.4(3) . . . . ? C21 C22 C23 C24 -0.5(3) . . . . ? C22 C23 C24 C19 -0.6(3) . . . . ? C20 C19 C24 C23 0.7(3) . . . . ? C5 C19 C24 C23 -177.3(2) . . . . ? N6 C6 C25 C30 134.3(2) . . . . ? C5 C6 C25 C30 -42.3(2) . . . . ? N6 C6 C25 C26 -44.8(2) . . . . ? C5 C6 C25 C26 138.6(2) . . . . ? C30 C25 C26 C27 -1.5(3) . . . . ? C6 C25 C26 C27 177.7(2) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C29 1.4(3) . . . . ? C27 C28 C29 C30 -1.6(3) . . . . ? C26 C25 C30 C29 1.3(3) . . . . ? C6 C25 C30 C29 -177.8(2) . . . . ? C28 C29 C30 C25 0.3(3) . . . . ? C6S C1S C2S C3S -0.3(5) . . . . ? C1S C2S C3S C4S -0.7(4) . . . . ? C2S C3S C4S C5S 0.3(4) . . . . ? C3S C4S C5S C6S 1.1(5) . . . . ? C2S C1S C6S C5S 1.7(6) . . . . ? C4S C5S C6S C1S -2.1(6) . . . . ? C12S C7S C8S C9S 2.2(5) . . . . ? C7S C8S C9S C10S -0.6(5) . . . . ? C8S C9S C10S C11S 0.3(6) . . . . ? C9S C10S C11S C12S -1.5(6) . . . . ? C10S C11S C12S C7S 3.2(6) . . . . ? C8S C7S C12S C11S -3.5(5) . . . . ? _refine_diff_density_max 1.342 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.079 #----------------------------------------------------------------------- data_9 _database_code_CSD 163719 _audit_creation_method SHELXL _chemical_name_systematic ; 1,8-Bis(fluoroboro)-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19-hexaaza- 4,5,11,12-tetraphenyl-17-chloro-18-diethylaminobicyclo-[6.6.6]eicosa- 3,5,10,12,16,18-hexaene iron(II)x(C6H6) ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C40 H36 B2 Cl F2 Fe N7 O6' _chemical_formula_weight 861.68 _chemical_melting_point ? _chemical_compound_source ? 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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 Orthorombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.077(3) _cell_length_b 21.551(4) _cell_length_c 21.580(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7942.1(24) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 118 _cell_measurement_theta_min 3 _cell_measurement_theta_max 27 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method ? _exptl_crystal_F_000 3552 _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type 'semi-empirical (SADABS)' _exptl_absorpt_correction_T_min 0.779164 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker SMART 1K CCC' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54556 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.53 _reflns_number_total 9138 _reflns_number_observed 5883 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXTL PLUS 5.0' _computing_structure_refinement 'SHELXTL PLUS 5.0' _computing_molecular_graphics 'SHELXTL PLUS 5.0' _computing_publication_material 'SHELXTL PLUS 5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 11 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.1243P)^2^+2.3045P] 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 9127 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_obs 0.0635 _refine_ls_wR_factor_all 0.2201 _refine_ls_wR_factor_obs 0.1884 _refine_ls_goodness_of_fit_all 1.069 _refine_ls_goodness_of_fit_obs 1.206 _refine_ls_restrained_S_all 1.120 _refine_ls_restrained_S_obs 1.206 _refine_ls_shift/esd_max 0.129 _refine_ls_shift/esd_mean 0.010 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.12282(3) 0.38790(2) 0.35880(2) 0.0310(2) Uani 1 d . . Cl1 Cl 0.09848(9) 0.21327(6) 0.25560(6) 0.0715(4) Uani 1 d . . F1 F 0.11697(12) 0.55210(11) 0.24374(10) 0.0450(5) Uani 1 d . . F2 F 0.12807(12) 0.22138(11) 0.47103(13) 0.0533(6) Uani 1 d . . B1 B 0.1188(2) 0.4999(2) 0.2792(2) 0.0384(9) Uani 1 d . . B2 B 0.1256(2) 0.2748(2) 0.4365(2) 0.0426(10) Uani 1 d . . O1 O 0.14276(15) 0.44719(13) 0.23888(12) 0.0430(6) Uani 1 d . . O2 O 0.0918(2) 0.25749(11) 0.37520(14) 0.0453(7) Uani 1 d . . O3 O 0.03871(13) 0.49040(11) 0.30532(11) 0.0362(6) Uani 1 d . . O4 O 0.07674(14) 0.32040(12) 0.46804(12) 0.0421(6) Uani 1 d . . O5 O 0.17641(13) 0.51032(11) 0.32937(12) 0.0365(6) Uani 1 d . . O6 O 0.20767(13) 0.29627(11) 0.42917(12) 0.0381(6) Uani 1 d . . N1 N 0.1368(2) 0.39151(15) 0.2702(2) 0.0397(7) Uani 1 d . . N2 N 0.0968(2) 0.30469(14) 0.3339(2) 0.0404(7) Uani 1 d . . N3 N 0.0377(2) 0.44358(13) 0.34846(13) 0.0320(6) Uani 1 d . . N4 N 0.0619(2) 0.37146(13) 0.43072(14) 0.0342(6) Uani 1 d . . N5 N 0.1907(2) 0.45739(13) 0.36278(13) 0.0318(6) Uani 1 d . . N6 N 0.2111(2) 0.35306(13) 0.40007(13) 0.0321(6) Uani 1 d . . N7 N 0.1205(2) 0.3398(2) 0.1729(2) 0.0629(11) Uani 1 d . . C1 C 0.1202(2) 0.3420(2) 0.2364(2) 0.0461(10) Uani 1 d . . C2 C 0.1030(2) 0.2900(2) 0.2766(2) 0.0472(10) Uani 1 d . . C3 C -0.0193(2) 0.44522(15) 0.3893(2) 0.0296(7) Uani 1 d . . C4 C -0.0065(2) 0.3974(2) 0.4368(2) 0.0321(7) Uani 1 d . . C5 C 0.2626(2) 0.4490(2) 0.3830(2) 0.0308(7) Uani 1 d . . C6 C 0.2710(2) 0.38847(15) 0.4124(2) 0.0298(7) Uani 1 d . . C7 C 0.0681(4) 0.2975(3) 0.1395(3) 0.102(3) Uani 1 d . . H7A H 0.0413(4) 0.3201(3) 0.1069(3) 0.123 Uiso 1 calc R . H7B H 0.0288(4) 0.2816(3) 0.1678(3) 0.123 Uiso 1 calc R . C8 C 0.1134(7) 0.2423(5) 0.1105(4) 0.211(7) Uani 1 d . . H8A H 0.0774(7) 0.2157(5) 0.0890(4) 0.317 Uiso 1 calc R . H8B H 0.1392(7) 0.2193(5) 0.1427(4) 0.317 Uiso 1 calc R . H8C H 0.1517(7) 0.2578(5) 0.0818(4) 0.317 Uiso 1 calc R . C9 C 0.1795(3) 0.3719(2) 0.1389(2) 0.0596(12) Uani 1 d . . H9A H 0.2106(3) 0.3416(2) 0.1166(2) 0.071 Uiso 1 calc R . H9B H 0.2140(3) 0.3925(2) 0.1682(2) 0.071 Uiso 1 calc R . C10 C 0.1506(3) 0.4194(3) 0.0934(2) 0.0718(14) Uani 1 d . . H10A H 0.1944(3) 0.4383(3) 0.0730(2) 0.108 Uiso 1 calc R . H10B H 0.1211(3) 0.4506(3) 0.1149(2) 0.108 Uiso 1 calc R . H10C H 0.1177(3) 0.3996(3) 0.0632(2) 0.108 Uiso 1 calc R . C11 C -0.0855(2) 0.4886(2) 0.3882(2) 0.0327(7) Uani 1 d . . C12 C -0.1242(2) 0.5016(2) 0.3329(2) 0.0437(9) Uani 1 d . . H12A H -0.1074(2) 0.4834(2) 0.2962(2) 0.052 Uiso 1 calc R . C13 C -0.1877(2) 0.5417(2) 0.3323(2) 0.0597(12) Uani 1 d . . H13A H -0.2140(2) 0.5497(2) 0.2954(2) 0.072 Uiso 1 calc R . C14 C -0.2122(3) 0.5699(2) 0.3872(2) 0.0638(13) Uani 1 d . . H14A H -0.2545(3) 0.5971(2) 0.3868(2) 0.077 Uiso 1 calc R . C15 C -0.1735(2) 0.5576(2) 0.4423(2) 0.0517(10) Uani 1 d . . H15A H -0.1893(2) 0.5769(2) 0.4788(2) 0.062 Uiso 1 calc R . C16 C -0.1113(2) 0.5164(2) 0.4429(2) 0.0378(8) Uani 1 d . . H16A H -0.0864(2) 0.5071(2) 0.4801(2) 0.045 Uiso 1 calc R . C17 C -0.0649(2) 0.3790(2) 0.4835(2) 0.0336(7) Uani 1 d . . C18 C -0.1410(2) 0.3639(2) 0.4646(2) 0.0395(8) Uani 1 d . . H18A H -0.1549(2) 0.3668(2) 0.4230(2) 0.047 Uiso 1 calc R . C19 C -0.1951(2) 0.3447(2) 0.5081(2) 0.0454(9) Uani 1 d . . H19A H -0.2453(2) 0.3338(2) 0.4955(2) 0.054 Uiso 1 calc R . C20 C -0.1757(2) 0.3416(2) 0.5698(2) 0.0477(10) Uani 1 d . . H20A H -0.2129(2) 0.3289(2) 0.5986(2) 0.057 Uiso 1 calc R . C21 C -0.1013(3) 0.3575(2) 0.5891(2) 0.0478(10) Uani 1 d . . H21A H -0.0884(3) 0.3563(2) 0.6310(2) 0.057 Uiso 1 calc R . C22 C -0.0458(2) 0.3750(2) 0.5457(2) 0.0426(9) Uani 1 d . . H22A H 0.0049(2) 0.3843(2) 0.5585(2) 0.051 Uiso 1 calc R . C23 C 0.3365(2) 0.3737(2) 0.4549(2) 0.0335(7) Uani 1 d . . C24 C 0.3702(2) 0.3150(2) 0.4565(2) 0.0382(8) Uani 1 d . . H24A H 0.3519(2) 0.2839(2) 0.4303(2) 0.046 Uiso 1 calc R . C25 C 0.4310(2) 0.3029(2) 0.4970(2) 0.0457(9) Uani 1 d . . H25A H 0.4532(2) 0.2635(2) 0.4984(2) 0.055 Uiso 1 calc R . C26 C 0.4588(2) 0.3486(2) 0.5351(2) 0.0496(10) Uani 1 d . . H26A H 0.5001(2) 0.3404(2) 0.5620(2) 0.060 Uiso 1 calc R . C27 C 0.4256(2) 0.4072(2) 0.5335(2) 0.0468(10) Uani 1 d . . H27A H 0.4446(2) 0.4382(2) 0.5595(2) 0.056 Uiso 1 calc R . C28 C 0.3647(2) 0.4198(2) 0.4939(2) 0.0379(8) Uani 1 d . . H28A H 0.3425(2) 0.4592(2) 0.4932(2) 0.046 Uiso 1 calc R . C29 C 0.3281(2) 0.4908(2) 0.3692(2) 0.0320(7) Uani 1 d . . C30 C 0.3990(2) 0.4658(2) 0.3486(2) 0.0334(7) Uani 1 d . . H30A H 0.4051(2) 0.4230(2) 0.3458(2) 0.040 Uiso 1 calc R . C31 C 0.4601(2) 0.5044(2) 0.3325(2) 0.0389(8) Uani 1 d . . H31A H 0.5069(2) 0.4875(2) 0.3184(2) 0.047 Uiso 1 calc R . C32 C 0.4523(2) 0.5677(2) 0.3370(2) 0.0424(9) Uani 1 d . . H32A H 0.4932(2) 0.5934(2) 0.3246(2) 0.051 Uiso 1 calc R . C33 C 0.3833(2) 0.5935(2) 0.3600(2) 0.0486(10) Uani 1 d . . H33A H 0.3784(2) 0.6362(2) 0.3647(2) 0.058 Uiso 1 calc R . C34 C 0.3218(2) 0.5541(2) 0.3759(2) 0.0425(9) Uani 1 d . . H34A H 0.2756(2) 0.5709(2) 0.3913(2) 0.051 Uiso 1 calc R . C1S C 0.3324(3) 0.3139(2) 0.2595(2) 0.0511(10) Uani 1 d . . H1SA H 0.3205(3) 0.3506(2) 0.2801(2) 0.061 Uiso 1 calc R . C2S C 0.3792(3) 0.3153(2) 0.2076(2) 0.0551(11) Uani 1 d . . H2SA H 0.3988(3) 0.3528(2) 0.1931(2) 0.066 Uiso 1 calc R . C3S C 0.3969(3) 0.2613(2) 0.1774(2) 0.0589(12) Uani 1 d . . H3SA H 0.4288(3) 0.2622(2) 0.1425(2) 0.071 Uiso 1 calc R . C4S C 0.3679(3) 0.2059(2) 0.1982(2) 0.0616(12) Uani 1 d . . H4SA H 0.3796(3) 0.1693(2) 0.1774(2) 0.074 Uiso 1 calc R . C5S C 0.3204(3) 0.2048(2) 0.2510(2) 0.0620(12) Uani 1 d . . H5SA H 0.3007(3) 0.1673(2) 0.2656(2) 0.074 Uiso 1 calc R . C6S C 0.3031(3) 0.2581(2) 0.2808(2) 0.0534(11) Uani 1 d . . H6SA H 0.2714(3) 0.2573(2) 0.3158(2) 0.064 Uiso 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 0.0212(2) 0.0288(3) 0.0430(3) 0.0039(2) 0.0003(2) 0.0004(2) Cl1 0.0884(9) 0.0461(7) 0.0800(9) -0.0062(6) -0.0098(7) -0.0111(6) F1 0.0326(11) 0.0472(13) 0.0550(13) 0.0218(11) 0.0013(9) 0.0009(9) F2 0.0308(11) 0.0372(12) 0.092(2) 0.0280(12) -0.0065(11) -0.0044(9) B1 0.024(2) 0.044(2) 0.047(2) 0.013(2) 0.002(2) 0.000(2) B2 0.023(2) 0.032(2) 0.073(3) 0.011(2) -0.001(2) -0.004(2) O1 0.0337(13) 0.051(2) 0.0443(14) 0.0073(13) 0.0050(11) 0.0021(11) O2 0.0353(13) 0.0276(13) 0.073(2) 0.0079(13) -0.0134(12) -0.0046(11) O3 0.0271(12) 0.0360(13) 0.0454(14) 0.0140(11) 0.0031(10) 0.0027(10) O4 0.0291(12) 0.0369(14) 0.060(2) 0.0202(12) 0.0010(11) 0.0003(10) O5 0.0276(12) 0.0297(13) 0.0521(15) 0.0129(11) -0.0011(10) -0.0010(10) O6 0.0250(12) 0.0268(12) 0.062(2) 0.0123(11) -0.0030(11) -0.0017(9) N1 0.0278(15) 0.042(2) 0.050(2) 0.010(2) 0.0001(13) 0.0056(12) N2 0.0275(14) 0.033(2) 0.060(2) -0.002(2) -0.0101(14) -0.0004(12) N3 0.0248(13) 0.032(2) 0.0389(15) 0.0074(12) 0.0012(11) -0.0006(11) N4 0.0243(13) 0.0293(15) 0.049(2) 0.0090(13) -0.0018(12) -0.0010(11) N5 0.0240(13) 0.0276(14) 0.044(2) 0.0057(12) 0.0038(11) 0.0028(11) N6 0.0243(13) 0.0263(14) 0.046(2) 0.0039(13) 0.0015(11) 0.0010(11) N7 0.053(2) 0.075(3) 0.060(2) -0.025(2) -0.001(2) -0.015(2) C1 0.032(2) 0.057(3) 0.049(2) -0.013(2) -0.008(2) 0.002(2) C2 0.034(2) 0.042(2) 0.065(3) -0.004(2) -0.012(2) -0.002(2) C3 0.0233(15) 0.028(2) 0.038(2) 0.0014(14) -0.0011(13) -0.0023(12) C4 0.025(2) 0.030(2) 0.042(2) 0.0020(14) -0.0011(13) -0.0039(13) C5 0.0234(15) 0.031(2) 0.038(2) 0.0016(14) 0.0011(13) -0.0008(13) C6 0.0232(15) 0.026(2) 0.040(2) -0.0023(14) 0.0028(13) 0.0008(12) C7 0.145(6) 0.092(5) 0.070(4) 0.009(3) -0.045(4) -0.058(5) C8 0.364(19) 0.174(10) 0.095(6) -0.068(7) 0.034(8) -0.158(12) C9 0.076(3) 0.058(3) 0.045(2) -0.002(2) -0.003(2) -0.002(2) C10 0.081(4) 0.069(3) 0.065(3) 0.001(3) -0.003(3) 0.017(3) C11 0.0214(15) 0.033(2) 0.043(2) 0.005(2) 0.0028(13) -0.0013(13) C12 0.028(2) 0.057(3) 0.046(2) 0.006(2) 0.0010(15) 0.005(2) C13 0.036(2) 0.082(3) 0.061(3) 0.024(3) 0.001(2) 0.016(2) C14 0.044(2) 0.065(3) 0.082(3) 0.019(3) 0.018(2) 0.026(2) C15 0.043(2) 0.047(2) 0.065(3) 0.001(2) 0.014(2) 0.010(2) C16 0.032(2) 0.030(2) 0.051(2) 0.001(2) 0.0047(15) -0.0012(14) C17 0.029(2) 0.026(2) 0.045(2) 0.0036(15) 0.0054(14) -0.0020(13) C18 0.029(2) 0.034(2) 0.056(2) 0.005(2) 0.004(2) -0.0014(14) C19 0.028(2) 0.037(2) 0.071(3) 0.010(2) 0.011(2) 0.0015(15) C20 0.048(2) 0.029(2) 0.066(3) 0.011(2) 0.025(2) 0.008(2) C21 0.060(3) 0.038(2) 0.046(2) 0.005(2) 0.011(2) 0.001(2) C22 0.041(2) 0.036(2) 0.052(2) 0.005(2) 0.003(2) -0.005(2) C23 0.024(2) 0.037(2) 0.039(2) 0.0034(15) 0.0027(13) 0.0004(13) C24 0.033(2) 0.030(2) 0.051(2) 0.003(2) -0.006(2) -0.0010(14) C25 0.039(2) 0.035(2) 0.063(3) 0.005(2) -0.010(2) 0.006(2) C26 0.042(2) 0.052(2) 0.055(2) -0.001(2) -0.014(2) 0.009(2) C27 0.042(2) 0.049(2) 0.049(2) -0.011(2) -0.013(2) 0.007(2) C28 0.031(2) 0.036(2) 0.046(2) -0.003(2) -0.0007(14) 0.0071(15) C29 0.025(2) 0.029(2) 0.042(2) 0.0020(14) -0.0016(13) -0.0024(13) C30 0.031(2) 0.032(2) 0.037(2) -0.0026(15) -0.0015(13) -0.0019(14) C31 0.026(2) 0.051(2) 0.040(2) 0.000(2) 0.0007(14) -0.005(2) C32 0.032(2) 0.044(2) 0.051(2) 0.008(2) -0.003(2) -0.012(2) C33 0.043(2) 0.031(2) 0.072(3) 0.004(2) -0.010(2) -0.006(2) C34 0.027(2) 0.037(2) 0.064(2) -0.003(2) 0.001(2) -0.0032(15) C1S 0.061(3) 0.044(2) 0.048(2) -0.005(2) -0.003(2) 0.000(2) C2S 0.059(3) 0.049(3) 0.058(3) 0.008(2) -0.002(2) -0.009(2) C3S 0.045(2) 0.073(3) 0.058(3) 0.003(2) 0.011(2) 0.001(2) C4S 0.057(3) 0.053(3) 0.075(3) -0.011(2) 0.009(2) 0.009(2) C5S 0.062(3) 0.050(3) 0.074(3) 0.007(2) 0.007(2) -0.002(2) C6S 0.057(3) 0.057(3) 0.046(2) 0.002(2) 0.006(2) 0.006(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 N5 1.895(3) . ? Fe1 N3 1.898(3) . ? Fe1 N4 1.901(3) . ? Fe1 N6 1.905(3) . ? Fe1 N2 1.924(3) . ? Fe1 N1 1.929(3) . ? Cl1 C2 1.717(4) . ? F1 B1 1.361(5) . ? F2 B2 1.371(5) . ? B1 O5 1.481(5) . ? B1 O1 1.487(6) . ? B1 O3 1.493(4) . ? B2 O4 1.458(5) . ? B2 O6 1.484(4) . ? B2 O2 1.492(6) . ? O1 N1 1.381(4) . ? O2 N2 1.355(4) . ? O3 N3 1.373(3) . ? O4 N4 1.387(4) . ? O5 N5 1.371(3) . ? O6 N6 1.377(3) . ? N1 C1 1.323(5) . ? N2 C2 1.281(5) . ? N3 C3 1.314(4) . ? N4 C4 1.303(4) . ? N5 C5 1.316(4) . ? N6 C6 1.303(4) . ? N7 C1 1.370(6) . ? N7 C9 1.427(6) . ? N7 C7 1.468(6) . ? C1 C2 1.447(6) . ? C3 C11 1.467(4) . ? C3 C4 1.470(5) . ? C4 C17 1.472(5) . ? C5 C6 1.458(5) . ? C5 C29 1.467(4) . ? C6 C23 1.482(5) . ? C7 C8 1.550(13) . ? C9 C10 1.501(7) . ? C11 C12 1.392(5) . ? C11 C16 1.395(5) . ? C12 C13 1.386(6) . ? C13 C14 1.397(7) . ? C14 C15 1.386(7) . ? C15 C16 1.385(5) . ? C17 C22 1.384(5) . ? C17 C18 1.399(5) . ? C18 C19 1.382(5) . ? C19 C20 1.373(6) . ? C20 C21 1.382(6) . ? C21 C22 1.385(5) . ? C23 C28 1.389(5) . ? C23 C24 1.391(5) . ? C24 C25 1.383(5) . ? C25 C26 1.367(6) . ? C26 C27 1.384(6) . ? C27 C28 1.373(5) . ? C29 C34 1.377(5) . ? C29 C30 1.398(5) . ? C30 C31 1.379(5) . ? C31 C32 1.373(5) . ? C32 C33 1.395(6) . ? C33 C34 1.392(5) . ? C1S C2S 1.375(6) . ? C1S C6S 1.382(6) . ? C2S C3S 1.368(7) . ? C3S C4S 1.368(7) . ? C4S C5S 1.399(7) . ? C5S C6S 1.349(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 N5 Fe1 N3 88.50(12) . . ? N5 Fe1 N4 116.39(13) . . ? N3 Fe1 N4 78.17(12) . . ? N5 Fe1 N6 78.85(12) . . ? N3 Fe1 N6 155.52(13) . . ? N4 Fe1 N6 88.72(12) . . ? N5 Fe1 N2 152.91(13) . . ? N3 Fe1 N2 112.30(12) . . ? N4 Fe1 N2 85.87(14) . . ? N6 Fe1 N2 86.90(12) . . ? N5 Fe1 N1 86.40(13) . . ? N3 Fe1 N1 87.31(12) . . ? N4 Fe1 N1 152.21(13) . . ? N6 Fe1 N1 112.40(12) . . ? N2 Fe1 N1 77.84(14) . . ? F1 B1 O5 107.5(3) . . ? F1 B1 O1 108.0(3) . . ? O5 B1 O1 111.2(3) . . ? F1 B1 O3 107.7(3) . . ? O5 B1 O3 110.7(3) . . ? O1 B1 O3 111.6(3) . . ? F2 B2 O4 109.3(4) . . ? F2 B2 O6 106.9(3) . . ? O4 B2 O6 112.3(3) . . ? F2 B2 O2 106.5(3) . . ? O4 B2 O2 111.1(3) . . ? O6 B2 O2 110.4(3) . . ? N1 O1 B1 110.9(3) . . ? N2 O2 B2 111.8(3) . . ? N3 O3 B1 111.6(2) . . ? N4 O4 B2 111.6(3) . . ? N5 O5 B1 112.1(3) . . ? N6 O6 B2 111.5(2) . . ? C1 N1 O1 116.5(3) . . ? C1 N1 Fe1 119.2(3) . . ? O1 N1 Fe1 121.9(2) . . ? C2 N2 O2 117.1(3) . . ? C2 N2 Fe1 118.7(3) . . ? O2 N2 Fe1 122.0(2) . . ? C3 N3 O3 116.4(3) . . ? C3 N3 Fe1 120.4(2) . . ? O3 N3 Fe1 122.3(2) . . ? C4 N4 O4 116.5(3) . . ? C4 N4 Fe1 119.6(2) . . ? O4 N4 Fe1 121.5(2) . . ? C5 N5 O5 117.0(3) . . ? C5 N5 Fe1 118.5(2) . . ? O5 N5 Fe1 121.7(2) . . ? C6 N6 O6 117.5(3) . . ? C6 N6 Fe1 119.0(2) . . ? O6 N6 Fe1 122.0(2) . . ? C1 N7 C9 120.0(4) . . ? C1 N7 C7 120.7(4) . . ? C9 N7 C7 118.6(4) . . ? N1 C1 N7 125.3(4) . . ? N1 C1 C2 109.7(4) . . ? N7 C1 C2 125.0(4) . . ? N2 C2 C1 113.9(4) . . ? N2 C2 Cl1 119.2(3) . . ? C1 C2 Cl1 126.7(3) . . ? N3 C3 C11 125.3(3) . . ? N3 C3 C4 109.8(3) . . ? C11 C3 C4 124.9(3) . . ? N4 C4 C3 111.3(3) . . ? N4 C4 C17 124.1(3) . . ? C3 C4 C17 124.5(3) . . ? N5 C5 C6 111.1(3) . . ? N5 C5 C29 124.2(3) . . ? C6 C5 C29 124.2(3) . . ? N6 C6 C5 111.0(3) . . ? N6 C6 C23 126.4(3) . . ? C5 C6 C23 122.4(3) . . ? N7 C7 C8 111.8(7) . . ? N7 C9 C10 115.7(5) . . ? C12 C11 C16 119.2(3) . . ? C12 C11 C3 120.6(3) . . ? C16 C11 C3 120.2(3) . . ? C13 C12 C11 120.4(4) . . ? C12 C13 C14 119.8(4) . . ? C15 C14 C13 120.2(4) . . ? C14 C15 C16 119.7(4) . . ? C15 C16 C11 120.7(4) . . ? C22 C17 C18 119.2(3) . . ? C22 C17 C4 121.4(3) . . ? C18 C17 C4 119.4(3) . . ? C19 C18 C17 119.5(4) . . ? C20 C19 C18 120.8(4) . . ? C19 C20 C21 120.2(4) . . ? C20 C21 C22 119.5(4) . . ? C21 C22 C17 120.8(4) . . ? C28 C23 C24 119.6(3) . . ? C28 C23 C6 118.9(3) . . ? C24 C23 C6 121.5(3) . . ? C25 C24 C23 119.8(4) . . ? C26 C25 C24 120.4(4) . . ? C25 C26 C27 120.0(4) . . ? C28 C27 C26 120.4(4) . . ? C27 C28 C23 119.9(3) . . ? C34 C29 C30 118.9(3) . . ? C34 C29 C5 121.8(3) . . ? C30 C29 C5 119.3(3) . . ? C31 C30 C29 120.2(3) . . ? C32 C31 C30 120.6(3) . . ? C31 C32 C33 120.2(3) . . ? C34 C33 C32 118.8(4) . . ? C29 C34 C33 121.3(4) . . ? C2S C1S C6S 120.0(4) . . ? C3S C2S C1S 119.9(4) . . ? C2S C3S C4S 120.4(4) . . ? C3S C4S C5S 119.4(4) . . ? C6S C5S C4S 120.1(5) . . ? C5S C6S C1S 120.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 B1 O1 N1 -172.9(3) . . . . ? O5 B1 O1 N1 69.4(3) . . . . ? O3 B1 O1 N1 -54.7(4) . . . . ? F2 B2 O2 N2 -171.1(3) . . . . ? O4 B2 O2 N2 69.9(4) . . . . ? O6 B2 O2 N2 -55.4(4) . . . . ? F1 B1 O3 N3 -171.7(3) . . . . ? O5 B1 O3 N3 -54.5(4) . . . . ? O1 B1 O3 N3 69.9(4) . . . . ? F2 B2 O4 N4 -170.3(3) . . . . ? O6 B2 O4 N4 71.1(4) . . . . ? O2 B2 O4 N4 -53.1(4) . . . . ? F1 B1 O5 N5 -171.6(3) . . . . ? O1 B1 O5 N5 -53.7(4) . . . . ? O3 B1 O5 N5 71.0(4) . . . . ? F2 B2 O6 N6 -174.2(3) . . . . ? O4 B2 O6 N6 -54.3(4) . . . . ? O2 B2 O6 N6 70.3(4) . . . . ? B1 O1 N1 C1 149.3(3) . . . . ? B1 O1 N1 Fe1 -13.1(3) . . . . ? N5 Fe1 N1 C1 161.0(3) . . . . ? N3 Fe1 N1 C1 -110.3(3) . . . . ? N4 Fe1 N1 C1 -52.3(4) . . . . ? N6 Fe1 N1 C1 84.7(3) . . . . ? N2 Fe1 N1 C1 3.2(3) . . . . ? N5 Fe1 N1 O1 -37.0(2) . . . . ? N3 Fe1 N1 O1 51.6(2) . . . . ? N4 Fe1 N1 O1 109.7(3) . . . . ? N6 Fe1 N1 O1 -113.4(2) . . . . ? N2 Fe1 N1 O1 165.1(3) . . . . ? B2 O2 N2 C2 150.2(3) . . . . ? B2 O2 N2 Fe1 -12.8(4) . . . . ? N5 Fe1 N2 C2 -53.2(4) . . . . ? N3 Fe1 N2 C2 84.6(3) . . . . ? N4 Fe1 N2 C2 160.0(3) . . . . ? N6 Fe1 N2 C2 -111.1(3) . . . . ? N1 Fe1 N2 C2 2.6(3) . . . . ? N5 Fe1 N2 O2 109.6(3) . . . . ? N3 Fe1 N2 O2 -112.7(2) . . . . ? N4 Fe1 N2 O2 -37.2(3) . . . . ? N6 Fe1 N2 O2 51.7(3) . . . . ? N1 Fe1 N2 O2 165.4(3) . . . . ? B1 O3 N3 C3 156.7(3) . . . . ? B1 O3 N3 Fe1 -12.4(4) . . . . ? N5 Fe1 N3 C3 -118.7(3) . . . . ? N4 Fe1 N3 C3 -1.4(3) . . . . ? N6 Fe1 N3 C3 -60.4(4) . . . . ? N2 Fe1 N3 C3 79.1(3) . . . . ? N1 Fe1 N3 C3 154.8(3) . . . . ? N5 Fe1 N3 O3 49.9(2) . . . . ? N4 Fe1 N3 O3 167.3(3) . . . . ? N6 Fe1 N3 O3 108.3(3) . . . . ? N2 Fe1 N3 O3 -112.2(2) . . . . ? N1 Fe1 N3 O3 -36.5(2) . . . . ? B2 O4 N4 C4 145.6(3) . . . . ? B2 O4 N4 Fe1 -16.4(4) . . . . ? N5 Fe1 N4 C4 88.9(3) . . . . ? N3 Fe1 N4 C4 6.6(3) . . . . ? N6 Fe1 N4 C4 165.8(3) . . . . ? N2 Fe1 N4 C4 -107.2(3) . . . . ? N1 Fe1 N4 C4 -53.4(4) . . . . ? N5 Fe1 N4 O4 -109.7(2) . . . . ? N3 Fe1 N4 O4 168.0(3) . . . . ? N6 Fe1 N4 O4 -32.8(2) . . . . ? N2 Fe1 N4 O4 54.2(2) . . . . ? N1 Fe1 N4 O4 108.0(3) . . . . ? B1 O5 N5 C5 144.3(3) . . . . ? B1 O5 N5 Fe1 -16.3(3) . . . . ? N3 Fe1 N5 C5 166.2(3) . . . . ? N4 Fe1 N5 C5 90.2(3) . . . . ? N6 Fe1 N5 C5 7.3(3) . . . . ? N2 Fe1 N5 C5 -52.3(4) . . . . ? N1 Fe1 N5 C5 -106.4(3) . . . . ? N3 Fe1 N5 O5 -33.4(2) . . . . ? N4 Fe1 N5 O5 -109.4(2) . . . . ? N6 Fe1 N5 O5 167.6(3) . . . . ? N2 Fe1 N5 O5 108.1(3) . . . . ? N1 Fe1 N5 O5 54.0(2) . . . . ? B2 O6 N6 C6 152.5(3) . . . . ? B2 O6 N6 Fe1 -13.3(4) . . . . ? N5 Fe1 N6 C6 1.3(3) . . . . ? N3 Fe1 N6 C6 -58.9(4) . . . . ? N4 Fe1 N6 C6 -116.0(3) . . . . ? N2 Fe1 N6 C6 158.1(3) . . . . ? N1 Fe1 N6 C6 82.6(3) . . . . ? N5 Fe1 N6 O6 166.8(3) . . . . ? N3 Fe1 N6 O6 106.7(3) . . . . ? N4 Fe1 N6 O6 49.6(2) . . . . ? N2 Fe1 N6 O6 -36.3(3) . . . . ? N1 Fe1 N6 O6 -111.8(2) . . . . ? O1 N1 C1 N7 10.8(5) . . . . ? Fe1 N1 C1 N7 173.7(3) . . . . ? O1 N1 C1 C2 -170.3(3) . . . . ? Fe1 N1 C1 C2 -7.4(4) . . . . ? C9 N7 C1 N1 39.0(6) . . . . ? C7 N7 C1 N1 -150.1(5) . . . . ? C9 N7 C1 C2 -139.7(4) . . . . ? C7 N7 C1 C2 31.2(7) . . . . ? O2 N2 C2 C1 -170.9(3) . . . . ? Fe1 N2 C2 C1 -7.3(4) . . . . ? O2 N2 C2 Cl1 3.9(4) . . . . ? Fe1 N2 C2 Cl1 167.6(2) . . . . ? N1 C1 C2 N2 9.2(5) . . . . ? N7 C1 C2 N2 -171.9(4) . . . . ? N1 C1 C2 Cl1 -165.2(3) . . . . ? N7 C1 C2 Cl1 13.6(6) . . . . ? O3 N3 C3 C11 6.9(5) . . . . ? Fe1 N3 C3 C11 176.3(3) . . . . ? O3 N3 C3 C4 -172.5(3) . . . . ? Fe1 N3 C3 C4 -3.1(4) . . . . ? O4 N4 C4 C3 -172.2(3) . . . . ? Fe1 N4 C4 C3 -9.9(4) . . . . ? O4 N4 C4 C17 5.0(5) . . . . ? Fe1 N4 C4 C17 167.3(3) . . . . ? N3 C3 C4 N4 7.9(4) . . . . ? C11 C3 C4 N4 -171.5(3) . . . . ? N3 C3 C4 C17 -169.3(3) . . . . ? C11 C3 C4 C17 11.3(5) . . . . ? O5 N5 C5 C6 -174.6(3) . . . . ? Fe1 N5 C5 C6 -13.3(4) . . . . ? O5 N5 C5 C29 -3.2(5) . . . . ? Fe1 N5 C5 C29 158.0(3) . . . . ? O6 N6 C6 C5 -174.5(3) . . . . ? Fe1 N6 C6 C5 -8.3(4) . . . . ? O6 N6 C6 C23 0.1(5) . . . . ? Fe1 N6 C6 C23 166.3(3) . . . . ? N5 C5 C6 N6 13.3(4) . . . . ? C29 C5 C6 N6 -158.0(3) . . . . ? N5 C5 C6 C23 -161.5(3) . . . . ? C29 C5 C6 C23 27.2(5) . . . . ? C1 N7 C7 C8 -107.7(7) . . . . ? C9 N7 C7 C8 63.3(8) . . . . ? C1 N7 C9 C10 -121.8(5) . . . . ? C7 N7 C9 C10 67.2(7) . . . . ? N3 C3 C11 C12 43.3(5) . . . . ? C4 C3 C11 C12 -137.4(4) . . . . ? N3 C3 C11 C16 -137.7(4) . . . . ? C4 C3 C11 C16 41.6(5) . . . . ? C16 C11 C12 C13 -0.2(6) . . . . ? C3 C11 C12 C13 178.7(4) . . . . ? C11 C12 C13 C14 1.1(7) . . . . ? C12 C13 C14 C15 -0.5(7) . . . . ? C13 C14 C15 C16 -1.0(7) . . . . ? C14 C15 C16 C11 2.0(6) . . . . ? C12 C11 C16 C15 -1.4(5) . . . . ? C3 C11 C16 C15 179.7(3) . . . . ? N4 C4 C17 C22 52.3(5) . . . . ? C3 C4 C17 C22 -130.9(4) . . . . ? N4 C4 C17 C18 -126.4(4) . . . . ? C3 C4 C17 C18 50.5(5) . . . . ? C22 C17 C18 C19 -0.7(5) . . . . ? C4 C17 C18 C19 178.0(3) . . . . ? C17 C18 C19 C20 1.5(6) . . . . ? C18 C19 C20 C21 -0.4(6) . . . . ? C19 C20 C21 C22 -1.5(6) . . . . ? C20 C21 C22 C17 2.3(6) . . . . ? C18 C17 C22 C21 -1.1(6) . . . . ? C4 C17 C22 C21 -179.8(3) . . . . ? N6 C6 C23 C28 -138.5(4) . . . . ? C5 C6 C23 C28 35.5(5) . . . . ? N6 C6 C23 C24 41.6(5) . . . . ? C5 C6 C23 C24 -144.4(3) . . . . ? C28 C23 C24 C25 0.4(6) . . . . ? C6 C23 C24 C25 -179.7(3) . . . . ? C23 C24 C25 C26 -0.8(6) . . . . ? C24 C25 C26 C27 0.6(7) . . . . ? C25 C26 C27 C28 -0.1(7) . . . . ? C26 C27 C28 C23 -0.3(6) . . . . ? C24 C23 C28 C27 0.1(6) . . . . ? C6 C23 C28 C27 -179.8(3) . . . . ? N5 C5 C29 C34 47.9(5) . . . . ? C6 C5 C29 C34 -141.9(4) . . . . ? N5 C5 C29 C30 -131.9(4) . . . . ? C6 C5 C29 C30 38.3(5) . . . . ? C34 C29 C30 C31 -3.1(5) . . . . ? C5 C29 C30 C31 176.7(3) . . . . ? C29 C30 C31 C32 0.6(5) . . . . ? C30 C31 C32 C33 2.2(6) . . . . ? C31 C32 C33 C34 -2.5(6) . . . . ? C30 C29 C34 C33 2.8(6) . . . . ? C5 C29 C34 C33 -177.0(4) . . . . ? C32 C33 C34 C29 0.0(6) . . . . ? C6S C1S C2S C3S -0.2(7) . . . . ? C1S C2S C3S C4S 0.4(7) . . . . ? C2S C3S C4S C5S -0.5(7) . . . . ? C3S C4S C5S C6S 0.4(8) . . . . ? C4S C5S C6S C1S -0.2(7) . . . . ? C2S C1S C6S C5S 0.1(7) . . . . ? _refine_diff_density_max 1.660 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------- data_13 _database_code_CSD 163720 _audit_creation_method SHELXL-97 _chemical_name_systematic ; 1,8-Bis(fluoroboro)-2,7,9,14,15,20-hexaoxa-3,6,10,13,16,19-hexaaza- 4,5,11,12-tetraphenyl-17,18-methylthiobicyclo-[6.6.6]eicosa-3,5,10,12,16,18- hexaene iron(II) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H26 B2 F2 Fe N6 O6 S2' _chemical_formula_weight 770.18 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 9.9930(10) _cell_length_b 9.9930(10) _cell_length_c 34.575(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3452.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 24 _cell_measurement_theta_min 2 _cell_measurement_theta_max 10 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.622 _exptl_absorpt_correction_type semiempirical _exptl_absorpt_correction_T_min 0.7802 _exptl_absorpt_correction_T_max 0.8258 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator filter _diffrn_measurement_device_type Enraf-Nonius CAD-4 _diffrn_measurement_method \q/2\q scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time 100 _diffrn_standards_decay_% 6.8 _diffrn_reflns_number 2639 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0309 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.95 _reflns_number_total 2402 _reflns_number_gt 2401 _reflns_threshold_expression >2sigma(I) _computing_data_collection CAD4 _computing_cell_refinement CAD4 _computing_data_reduction XCAD4NEW _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL PLUS 5.0 _computing_publication_material 'SHELXL-97' _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^)+(0.1348P)^2^+3.0994P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(4) _refine_ls_number_reflns 2402 _refine_ls_number_parameters 231 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0558 _refine_ls_wR_factor_ref 0.1697 _refine_ls_wR_factor_gt 0.1696 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe Fe 0.31229(8) 0.31229(8) 0.5000 0.0254(3) Uani 1 2 d S . . S1 S -0.09705(16) 0.12937(19) 0.50449(6) 0.0476(5) Uani 1 1 d . . . F1 F 0.0077(4) 0.6164(4) 0.48807(11) 0.0420(9) Uani 1 1 d . . . O1 O 0.2081(5) 0.5718(4) 0.51843(12) 0.0335(9) Uani 1 1 d . . . O2 O 0.4950(4) 0.1604(4) 0.54751(12) 0.0342(10) Uani 1 1 d . . . O3 O 0.0385(4) 0.4001(4) 0.50766(12) 0.0340(10) Uani 1 1 d . . . N1 N 0.2996(5) 0.4738(5) 0.52800(14) 0.0306(11) Uani 1 1 d . . . N2 N 0.4183(5) 0.2729(5) 0.54444(14) 0.0291(11) Uani 1 1 d . . . N3 N 0.1235(4) 0.2916(5) 0.50635(14) 0.0278(10) Uani 1 1 d . . . B1 B 0.1051(7) 0.5192(7) 0.49194(19) 0.0330(15) Uani 1 1 d . . . C1 C 0.3663(7) 0.4899(6) 0.56020(18) 0.0329(13) Uani 1 1 d . . . C2 C 0.4405(6) 0.3725(6) 0.56924(18) 0.0322(13) Uani 1 1 d . . . C3 C 0.3658(6) 0.6125(6) 0.58381(18) 0.0340(13) Uani 1 1 d . . . C4 C 0.3863(8) 0.7366(7) 0.5672(2) 0.0472(17) Uani 1 1 d . . . H4 H 0.3931 0.7437 0.5404 0.057 Uiso 1 1 calc R . . C5 C 0.3967(9) 0.8492(7) 0.5896(2) 0.0520(19) Uani 1 1 d . . . H5 H 0.4124 0.9318 0.5780 0.062 Uiso 1 1 calc R . . C6 C 0.3840(8) 0.8406(8) 0.6291(2) 0.052(2) Uani 1 1 d . . . H6 H 0.3914 0.9170 0.6443 0.063 Uiso 1 1 calc R . . C7 C 0.3605(9) 0.7199(10) 0.6459(2) 0.057(2) Uani 1 1 d . . . H7 H 0.3500 0.7149 0.6726 0.068 Uiso 1 1 calc R . . C8 C 0.3519(6) 0.6034(7) 0.62387(19) 0.0395(15) Uani 1 1 d . . . H8 H 0.3372 0.5211 0.6357 0.047 Uiso 1 1 calc R . . C9 C 0.5371(7) 0.3586(6) 0.6023(2) 0.0366(15) Uani 1 1 d . . . C10 C 0.6409(9) 0.4463(11) 0.6070(3) 0.062(2) Uani 1 1 d . . . H10 H 0.6560 0.5121 0.5884 0.074 Uiso 1 1 calc R . . C11 C 0.7235(10) 0.4386(13) 0.6388(4) 0.084(4) Uani 1 1 d . . . H11 H 0.7945 0.4981 0.6413 0.101 Uiso 1 1 calc R . . C12 C 0.7021(13) 0.3449(13) 0.6665(4) 0.094(4) Uani 1 1 d . . . H12 H 0.7578 0.3405 0.6880 0.113 Uiso 1 1 calc R . . C13 C 0.5960(14) 0.2555(12) 0.6626(3) 0.090(4) Uani 1 1 d . . . H13 H 0.5804 0.1920 0.6817 0.108 Uiso 1 1 calc R . . C14 C 0.5132(11) 0.2602(9) 0.6302(2) 0.062(2) Uani 1 1 d . . . H14 H 0.4435 0.1994 0.6273 0.075 Uiso 1 1 calc R . . C15 C 0.0719(6) 0.1744(6) 0.50259(18) 0.0319(12) Uani 1 1 d . . . C16 C -0.1632(7) 0.2367(8) 0.5421(2) 0.0521(19) Uani 1 1 d . . . H16A H -0.2570 0.2193 0.5454 0.078 Uiso 1 1 calc R . . H16B H -0.1505 0.3286 0.5349 0.078 Uiso 1 1 calc R . . H16C H -0.1172 0.2191 0.5659 0.078 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe 0.0266(4) 0.0266(4) 0.0230(5) 0.0001(3) -0.0001(3) -0.0006(4) S1 0.0282(8) 0.0506(10) 0.0639(12) -0.0068(9) 0.0015(8) -0.0080(7) F1 0.039(2) 0.036(2) 0.050(2) 0.0032(16) -0.0033(16) 0.0094(15) O1 0.039(2) 0.027(2) 0.034(2) -0.0044(17) -0.0068(19) 0.0066(16) O2 0.039(2) 0.034(2) 0.030(2) 0.0042(17) -0.0017(18) 0.0032(17) O3 0.029(2) 0.034(2) 0.039(3) 0.0004(18) 0.0038(18) 0.0054(16) N1 0.032(3) 0.032(2) 0.028(2) -0.003(2) 0.001(2) 0.000(2) N2 0.027(2) 0.034(3) 0.026(3) 0.005(2) -0.003(2) 0.0044(19) N3 0.021(2) 0.034(3) 0.028(3) 0.002(2) -0.0008(18) -0.001(2) B1 0.035(4) 0.030(3) 0.033(4) -0.004(3) 0.001(3) 0.005(3) C1 0.038(3) 0.034(3) 0.027(3) -0.001(3) 0.003(2) -0.001(2) C2 0.035(3) 0.032(3) 0.029(3) -0.001(2) 0.001(2) -0.004(2) C3 0.036(3) 0.032(3) 0.035(3) -0.009(3) -0.002(3) -0.002(2) C4 0.060(5) 0.047(4) 0.034(4) 0.000(3) 0.000(3) 0.001(3) C5 0.071(5) 0.030(3) 0.056(4) -0.008(3) -0.005(4) 0.000(3) C6 0.053(4) 0.039(4) 0.065(5) -0.026(4) -0.015(4) 0.012(3) C7 0.058(5) 0.079(6) 0.034(4) -0.022(4) -0.008(3) 0.011(4) C8 0.039(3) 0.050(4) 0.030(3) -0.005(3) -0.002(3) 0.001(3) C9 0.035(3) 0.036(4) 0.038(4) -0.008(3) -0.005(3) 0.005(3) C10 0.051(5) 0.072(6) 0.062(5) -0.014(5) -0.012(4) -0.001(4) C11 0.055(6) 0.090(8) 0.108(9) -0.039(7) -0.041(6) 0.002(5) C12 0.101(9) 0.099(8) 0.084(7) -0.016(7) -0.061(7) 0.011(7) C13 0.120(10) 0.096(8) 0.053(6) 0.014(5) -0.035(6) 0.017(7) C14 0.080(6) 0.060(5) 0.046(5) 0.002(4) -0.025(4) -0.005(4) C15 0.034(3) 0.033(3) 0.028(3) 0.003(3) -0.004(3) -0.008(2) C16 0.034(4) 0.059(5) 0.063(5) -0.001(4) 0.006(3) 0.000(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 Fe N1 1.886(5) 7_556 ? Fe N1 1.886(5) . ? Fe N2 1.907(5) 7_556 ? Fe N2 1.907(5) . ? Fe N3 1.910(5) . ? Fe N3 1.910(5) 7_556 ? S1 C15 1.749(6) . ? S1 C16 1.810(8) . ? F1 B1 1.382(7) . ? O1 N1 1.380(6) . ? O1 B1 1.475(8) . ? O2 N2 1.365(6) . ? O2 B1 1.491(8) 7_556 ? O3 N3 1.378(6) . ? O3 B1 1.468(8) . ? N1 C1 1.307(8) . ? N2 C2 1.332(8) . ? N3 C15 1.286(7) . ? B1 O2 1.491(8) 7_556 ? C1 C2 1.423(9) . ? C1 C3 1.472(9) . ? C2 C9 1.501(9) . ? C3 C4 1.382(10) . ? C3 C8 1.395(9) . ? C4 C5 1.371(10) . ? C5 C6 1.376(11) . ? C6 C7 1.358(13) . ? C7 C8 1.394(10) . ? C9 C10 1.368(11) . ? C9 C14 1.400(11) . ? C10 C11 1.378(14) . ? C11 C12 1.356(18) . ? C12 C13 1.393(19) . ? C13 C14 1.393(12) . ? C15 C15 1.460(13) 7_556 ? 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 Fe N1 112.2(3) 7_556 . ? N1 Fe N2 78.5(2) 7_556 7_556 ? N1 Fe N2 85.7(2) . 7_556 ? N1 Fe N2 85.7(2) 7_556 . ? N1 Fe N2 78.5(2) . . ? N2 Fe N2 151.4(3) 7_556 . ? N1 Fe N3 153.7(2) 7_556 . ? N1 Fe N3 88.1(2) . . ? N2 Fe N3 87.1(2) 7_556 . ? N2 Fe N3 115.7(2) . . ? N1 Fe N3 88.1(2) 7_556 7_556 ? N1 Fe N3 153.7(2) . 7_556 ? N2 Fe N3 115.7(2) 7_556 7_556 ? N2 Fe N3 87.1(2) . 7_556 ? N3 Fe N3 78.4(3) . 7_556 ? C15 S1 C16 103.1(3) . . ? N1 O1 B1 111.0(4) . . ? N2 O2 B1 109.0(4) . 7_556 ? N3 O3 B1 110.3(4) . . ? C1 N1 O1 117.0(5) . . ? C1 N1 Fe 120.5(4) . . ? O1 N1 Fe 121.9(4) . . ? C2 N2 O2 118.2(5) . . ? C2 N2 Fe 117.2(4) . . ? O2 N2 Fe 123.0(4) . . ? C15 N3 O3 118.2(5) . . ? C15 N3 Fe 118.9(4) . . ? O3 N3 Fe 121.8(4) . . ? F1 B1 O3 106.7(5) . . ? F1 B1 O1 107.5(5) . . ? O3 B1 O1 112.1(5) . . ? F1 B1 O2 106.6(5) . 7_556 ? O3 B1 O2 112.0(5) . 7_556 ? O1 B1 O2 111.5(5) . 7_556 ? N1 C1 C2 110.6(6) . . ? N1 C1 C3 125.0(6) . . ? C2 C1 C3 124.5(6) . . ? N2 C2 C1 112.8(6) . . ? N2 C2 C9 121.8(5) . . ? C1 C2 C9 125.3(6) . . ? C4 C3 C8 119.1(6) . . ? C4 C3 C1 121.0(6) . . ? C8 C3 C1 119.8(6) . . ? C5 C4 C3 120.9(7) . . ? C4 C5 C6 120.2(7) . . ? C7 C6 C5 119.7(7) . . ? C6 C7 C8 121.3(7) . . ? C7 C8 C3 118.8(7) . . ? C10 C9 C14 119.8(8) . . ? C10 C9 C2 121.3(7) . . ? C14 C9 C2 118.7(6) . . ? C9 C10 C11 120.9(11) . . ? C12 C11 C10 120.6(10) . . ? C11 C12 C13 119.6(9) . . ? C14 C13 C12 120.6(11) . . ? C13 C14 C9 118.5(10) . . ? N3 C15 C15 111.7(3) . 7_556 ? N3 C15 S1 128.2(5) . . ? C15 C15 S1 120.1(2) 7_556 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag B1 O1 N1 C1 -157.0(5) . . . . ? B1 O1 N1 Fe 14.8(6) . . . . ? N1 Fe N1 C1 -76.8(5) 7_556 . . . ? N2 Fe N1 C1 -152.4(5) 7_556 . . . ? N2 Fe N1 C1 3.6(5) . . . . ? N3 Fe N1 C1 120.4(5) . . . . ? N3 Fe N1 C1 61.6(7) 7_556 . . . ? N1 Fe N1 O1 111.8(4) 7_556 . . . ? N2 Fe N1 O1 36.1(4) 7_556 . . . ? N2 Fe N1 O1 -167.8(5) . . . . ? N3 Fe N1 O1 -51.1(4) . . . . ? N3 Fe N1 O1 -109.9(6) 7_556 . . . ? B1 O2 N2 C2 -145.2(6) 7_556 . . . ? B1 O2 N2 Fe 19.6(6) 7_556 . . . ? N1 Fe N2 C2 107.9(5) 7_556 . . . ? N1 Fe N2 C2 -5.8(4) . . . . ? N2 Fe N2 C2 51.8(4) 7_556 . . . ? N3 Fe N2 C2 -88.1(5) . . . . ? N3 Fe N2 C2 -163.8(5) 7_556 . . . ? N1 Fe N2 O2 -57.1(4) 7_556 . . . ? N1 Fe N2 O2 -170.8(5) . . . . ? N2 Fe N2 O2 -113.2(4) 7_556 . . . ? N3 Fe N2 O2 106.9(4) . . . . ? N3 Fe N2 O2 31.2(4) 7_556 . . . ? B1 O3 N3 C15 -150.4(5) . . . . ? B1 O3 N3 Fe 17.4(6) . . . . ? N1 Fe N3 C15 58.5(7) 7_556 . . . ? N1 Fe N3 C15 -159.5(5) . . . . ? N2 Fe N3 C15 114.8(5) 7_556 . . . ? N2 Fe N3 C15 -83.2(5) . . . . ? N3 Fe N3 C15 -2.2(3) 7_556 . . . ? N1 Fe N3 O3 -109.3(6) 7_556 . . . ? N1 Fe N3 O3 32.7(4) . . . . ? N2 Fe N3 O3 -53.0(4) 7_556 . . . ? N2 Fe N3 O3 109.0(4) . . . . ? N3 Fe N3 O3 -170.0(5) 7_556 . . . ? N3 O3 B1 F1 169.9(4) . . . . ? N3 O3 B1 O1 -72.6(6) . . . . ? N3 O3 B1 O2 53.6(6) . . . 7_556 ? N1 O1 B1 F1 171.7(5) . . . . ? N1 O1 B1 O3 54.8(6) . . . . ? N1 O1 B1 O2 -71.7(6) . . . 7_556 ? O1 N1 C1 C2 170.9(5) . . . . ? Fe N1 C1 C2 -0.9(7) . . . . ? O1 N1 C1 C3 -9.5(9) . . . . ? Fe N1 C1 C3 178.7(5) . . . . ? O2 N2 C2 C1 172.7(5) . . . . ? Fe N2 C2 C1 7.0(7) . . . . ? O2 N2 C2 C9 -5.9(8) . . . . ? Fe N2 C2 C9 -171.6(5) . . . . ? N1 C1 C2 N2 -3.9(8) . . . . ? C3 C1 C2 N2 176.6(6) . . . . ? N1 C1 C2 C9 174.7(6) . . . . ? C3 C1 C2 C9 -4.8(10) . . . . ? N1 C1 C3 C4 -48.7(10) . . . . ? C2 C1 C3 C4 130.9(7) . . . . ? N1 C1 C3 C8 134.9(7) . . . . ? C2 C1 C3 C8 -45.6(9) . . . . ? C8 C3 C4 C5 1.8(11) . . . . ? C1 C3 C4 C5 -174.6(8) . . . . ? C3 C4 C5 C6 -1.4(13) . . . . ? C4 C5 C6 C7 -0.3(13) . . . . ? C5 C6 C7 C8 1.4(13) . . . . ? C6 C7 C8 C3 -1.0(12) . . . . ? C4 C3 C8 C7 -0.6(10) . . . . ? C1 C3 C8 C7 175.8(7) . . . . ? N2 C2 C9 C10 124.2(8) . . . . ? C1 C2 C9 C10 -54.3(10) . . . . ? N2 C2 C9 C14 -60.9(9) . . . . ? C1 C2 C9 C14 120.6(8) . . . . ? C14 C9 C10 C11 0.6(13) . . . . ? C2 C9 C10 C11 175.4(8) . . . . ? C9 C10 C11 C12 -1.1(16) . . . . ? C10 C11 C12 C13 0.4(19) . . . . ? C11 C12 C13 C14 1(2) . . . . ? C12 C13 C14 C9 -1.4(17) . . . . ? C10 C9 C14 C13 0.7(14) . . . . ? C2 C9 C14 C13 -174.3(9) . . . . ? O3 N3 C15 C15 173.7(6) . . . 7_556 ? Fe N3 C15 C15 5.5(9) . . . 7_556 ? O3 N3 C15 S1 -8.3(8) . . . . ? Fe N3 C15 S1 -176.5(4) . . . . ? C16 S1 C15 N3 -37.7(7) . . . . ? C16 S1 C15 C15 140.1(7) . . . 7_556 ? _diffrn_measured_fraction_theta_max 0.752 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.752 _refine_diff_density_max 0.687 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.087