Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Joanne M. Holland' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Judith A. McAllister' ; Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, UK and Interdisciplinary Research Centre in Superconductivity, University of Cambridge, Madingley Road, Cambridge CB3 0HE, UK ; 'Colin A. Kilner' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Mark Thornton-Pett' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; 'Adam J. Bridgeman' ; Department of Chemistry, University of Hull, Kingston-Upon-Hull HU6 7RX, UK ; 'Malcolm A. Halcrow' ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author 'Dr. Malcolm A. Halcrow' _publ_contact_author_address ; School of Chemistry, University of Leeds, Woodhouse Lane, Leeds LS2 9JT, UK ; _publ_contact_author_phone '+44 (0)113 2336506' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email M.A.HALCROW@CHEM.LEEDS.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_contact_letter ; The following set of data is for two structures included in a manuscript we have just submitted to the Dalton Transactions office. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_requested_journal 'Journal of the Chemical Society, Dalton Transactions' _publ_section_title ; Stereochemical Effects on the Spin-State Transition Shown by Salts of [FeL~2~]^2+^ (L = 2,6-dipyrazol-1-ylpyridine). ; #================================================================= data_mh37a _database_code_CSD 171144 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) ditetrafluoroborate tris-nitromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[C22 H18 N10 Fe] 2[B F4] 2.9[C H3 N O2] 0.25[H2 O]' _chemical_formula_sum 'C24.9 H27.2 B2 F8 Fe N12.9 O6.05' _chemical_formula_weight 833.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.8129(2) _cell_length_b 13.8303(1) _cell_length_c 36.4266(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6958.81(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15894 _cell_measurement_theta_min 1.12 _cell_measurement_theta_max 27.48 _exptl_crystal_description Prism _exptl_crystal_colour Brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.591 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3418 _exptl_absorpt_coefficient_mu 0.538 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7748 _exptl_absorpt_correction_T_max 0.8684 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Crystals were grown at 235K, and mounted on a glass fibre while cooling over solid CO~2~ to avoid decomposition. Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65933 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0509 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15894 _reflns_number_gt 13533 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. The asymmetric unit contains two complex cations, four anions, six nitromethane molecules and one isolated feature (O117), which was modelled as half a molecule of water. The F atoms of two of the BF~4~^-^ anions are disordered. The ion centred on B77 is disordered over three orientations: F78A-F81A, occupancy 0.5 F78B-F81B, occupancy 0.3 F78C-F81C, occupancy 0.2. Attempts to refine distinct partial B atoms for each disorder orientation in this anion were unsuccessful. The ion centred on B82 is disordered over two orientations: B82A-F86A, occupancy 0.6 B82B-F86B, occupancy 0.4. All of the B-F bonds in the disordered anions were restrained to 1.38(2)\%A, and the corresponding non-bonded F...F distances to 2.25(2)\%A. Four of the CH~3~NO~2~ solvent sites are fully occupied. One site is disordered over two distinct orientations: C103-O106, occupancy 0.6 C107-O110, occupancy 0.4. The other solvent site has total occupany 0.8, disordered over two orientations. C111-O114, occupany 0.4 C111, N112, C115, O116, occupancy 0.4. In the latter orientation, a partial O atom is presumed to lie near C111, which has an occupancy of 1.0 (0.4 C + 0.4 O) to reflect this. Attempts to resolve a separate N atom or O atom for this last orientation were unsuccessful. No restraints were applied to the disordered solvent molecules. All non-H atoms with occupancy >=0.5 were refined anisotropically. ; _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^)+(0.1083P)^2^+0.2690P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(12) _refine_ls_number_reflns 15894 _refine_ls_number_parameters 1062 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0665 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1615 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.100 _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 0.34426(3) 0.66841(3) 0.762887(12) 0.02217(11) Uani 1 1 d . . . N2 N 0.2427(2) 0.6743(2) 0.72770(7) 0.0241(6) Uani 1 1 d . . . C3 C 0.2637(3) 0.6843(3) 0.69200(9) 0.0275(7) Uani 1 1 d . . . C4 C 0.1946(3) 0.6817(3) 0.66471(10) 0.0360(8) Uani 1 1 d . . . H4 H 0.2110 0.6889 0.6395 0.043 Uiso 1 1 calc R . . C5 C 0.0991(3) 0.6678(3) 0.67626(10) 0.0397(9) Uani 1 1 d . . . H5 H 0.0491 0.6646 0.6584 0.048 Uiso 1 1 calc R . . C6 C 0.0752(3) 0.6584(3) 0.71337(10) 0.0354(8) Uani 1 1 d . . . H6 H 0.0101 0.6501 0.7212 0.042 Uiso 1 1 calc R . . C7 C 0.1509(3) 0.6617(2) 0.73819(9) 0.0266(6) Uani 1 1 d . . . N8 N 0.3644(2) 0.6929(2) 0.68655(8) 0.0274(6) Uani 1 1 d . . . N9 N 0.4217(2) 0.68380(19) 0.71768(7) 0.0234(6) Uani 1 1 d . . . C10 C 0.5113(3) 0.6794(3) 0.70503(10) 0.0294(7) Uani 1 1 d . . . H10 H 0.5671 0.6719 0.7200 0.035 Uiso 1 1 calc R . . C11 C 0.5134(3) 0.6872(3) 0.66668(10) 0.0342(8) Uani 1 1 d . . . H11 H 0.5690 0.6874 0.6514 0.041 Uiso 1 1 calc R . . C12 C 0.4193(3) 0.6944(3) 0.65588(10) 0.0342(8) Uani 1 1 d . . . H12 H 0.3965 0.6996 0.6313 0.041 Uiso 1 1 calc R . . N13 N 0.1451(2) 0.6493(2) 0.77661(8) 0.0279(6) Uani 1 1 d . . . N14 N 0.2315(2) 0.6481(2) 0.79517(8) 0.0268(6) Uani 1 1 d . . . C15 C 0.2089(3) 0.6295(3) 0.82989(10) 0.0325(8) Uani 1 1 d . . . H15 H 0.2542 0.6235 0.8494 0.039 Uiso 1 1 calc R . . C16 C 0.1066(3) 0.6199(3) 0.83360(11) 0.0364(9) Uani 1 1 d . . . H16 H 0.0716 0.6073 0.8556 0.044 Uiso 1 1 calc R . . C17 C 0.0689(3) 0.6323(3) 0.79934(11) 0.0342(8) Uani 1 1 d . . . H17 H 0.0025 0.6297 0.7927 0.041 Uiso 1 1 calc R . . N18 N 0.4478(2) 0.6597(2) 0.79721(8) 0.0250(6) Uani 1 1 d . . . C19 C 0.4794(3) 0.7396(2) 0.81443(9) 0.0260(7) Uani 1 1 d . . . C20 C 0.5570(3) 0.7373(3) 0.83846(10) 0.0323(8) Uani 1 1 d . . . H20 H 0.5797 0.7939 0.8505 0.039 Uiso 1 1 calc R . . C21 C 0.5998(3) 0.6481(3) 0.84395(11) 0.0375(9) Uani 1 1 d . . . H21 H 0.6530 0.6438 0.8604 0.045 Uiso 1 1 calc R . . C22 C 0.5686(3) 0.5646(3) 0.82659(10) 0.0323(8) Uani 1 1 d . . . H22 H 0.5991 0.5039 0.8305 0.039 Uiso 1 1 calc R . . C23 C 0.4907(3) 0.5750(2) 0.80319(9) 0.0245(6) Uani 1 1 d . . . N24 N 0.4256(2) 0.8204(2) 0.80421(7) 0.0261(6) Uani 1 1 d . . . N25 N 0.3537(2) 0.80619(19) 0.77831(7) 0.0246(6) Uani 1 1 d . . . C26 C 0.3117(3) 0.8916(2) 0.77388(11) 0.0314(8) Uani 1 1 d . . . H26 H 0.2598 0.9041 0.7574 0.038 Uiso 1 1 calc R . . C27 C 0.3547(3) 0.9614(3) 0.79689(11) 0.0362(8) Uani 1 1 d . . . H27 H 0.3371 1.0275 0.7992 0.043 Uiso 1 1 calc R . . C28 C 0.4273(3) 0.9142(3) 0.81525(10) 0.0331(8) Uani 1 1 d . . . H28 H 0.4707 0.9419 0.8325 0.040 Uiso 1 1 calc R . . N29 N 0.4459(2) 0.5018(2) 0.78257(8) 0.0275(6) Uani 1 1 d . . . N30 N 0.3700(2) 0.5299(2) 0.76029(8) 0.0258(6) Uani 1 1 d . . . C31 C 0.3424(3) 0.4505(2) 0.74322(9) 0.0301(7) Uani 1 1 d . . . H31 H 0.2913 0.4475 0.7258 0.036 Uiso 1 1 calc R . . C32 C 0.3984(3) 0.3710(3) 0.75415(11) 0.0382(9) Uani 1 1 d . . . H32 H 0.3927 0.3062 0.7458 0.046 Uiso 1 1 calc R . . C33 C 0.4624(3) 0.4054(3) 0.77914(11) 0.0342(8) Uani 1 1 d . . . H33 H 0.5100 0.3689 0.7919 0.041 Uiso 1 1 calc R . . Fe34 Fe 0.08730(4) 0.92896(3) 0.915731(12) 0.02323(11) Uani 1 1 d . . . N35 N 0.1847(2) 1.0258(2) 0.91570(8) 0.0257(6) Uani 1 1 d . . . C36 C 0.1602(3) 1.1196(2) 0.91826(9) 0.0265(7) Uani 1 1 d . . . C37 C 0.2276(3) 1.1929(3) 0.91809(11) 0.0347(8) Uani 1 1 d . . . H37 H 0.2089 1.2588 0.9201 0.042 Uiso 1 1 calc R . . C38 C 0.3246(3) 1.1661(3) 0.91478(10) 0.0324(7) Uani 1 1 d . . . H38 H 0.3731 1.2148 0.9147 0.039 Uiso 1 1 calc R . . C39 C 0.3519(3) 1.0689(3) 0.91157(9) 0.0306(7) Uani 1 1 d . . . H39 H 0.4178 1.0503 0.9089 0.037 Uiso 1 1 calc R . . C40 C 0.2782(3) 1.0012(2) 0.91250(9) 0.0243(6) Uani 1 1 d . . . N41 N 0.0591(2) 1.1290(2) 0.92028(9) 0.0290(6) Uani 1 1 d . . . N42 N 0.0051(2) 1.0454(2) 0.92015(8) 0.0274(6) Uani 1 1 d . . . C43 C -0.0865(3) 1.0736(3) 0.92162(10) 0.0327(7) Uani 1 1 d . . . H43 H -0.1408 1.0313 0.9218 0.039 Uiso 1 1 calc R . . C44 C -0.0919(3) 1.1754(3) 0.92281(10) 0.0365(8) Uani 1 1 d . . . H44 H -0.1491 1.2134 0.9240 0.044 Uiso 1 1 calc R . . C45 C 0.0014(3) 1.2087(3) 0.92187(10) 0.0337(8) Uani 1 1 d . . . H45 H 0.0218 1.2743 0.9223 0.040 Uiso 1 1 calc R . . N46 N 0.2883(2) 0.9007(2) 0.91000(8) 0.0251(6) Uani 1 1 d . . . N47 N 0.2040(2) 0.8472(2) 0.91208(7) 0.0251(6) Uani 1 1 d . . . C48 C 0.2321(3) 0.7547(3) 0.91117(10) 0.0304(7) Uani 1 1 d . . . H48 H 0.1899 0.7006 0.9122 0.036 Uiso 1 1 calc R . . C49 C 0.3341(3) 0.7496(3) 0.90842(10) 0.0354(8) Uani 1 1 d . . . H49 H 0.3722 0.6925 0.9072 0.042 Uiso 1 1 calc R . . C50 C 0.3671(3) 0.8420(3) 0.90789(9) 0.0304(7) Uani 1 1 d . . . H50 H 0.4328 0.8620 0.9063 0.036 Uiso 1 1 calc R . . N51 N -0.0106(2) 0.8324(2) 0.91352(8) 0.0261(6) Uani 1 1 d . . . C52 C -0.0408(3) 0.7895(3) 0.94421(10) 0.0308(8) Uani 1 1 d . . . C53 C -0.1115(3) 0.7182(3) 0.94385(12) 0.0392(9) Uani 1 1 d . . . H53 H -0.1335 0.6889 0.9659 0.047 Uiso 1 1 calc R . . C54 C -0.1485(3) 0.6917(3) 0.91011(12) 0.0412(9) Uani 1 1 d . . . H54 H -0.1960 0.6422 0.9089 0.049 Uiso 1 1 calc R . . C55 C -0.1179(3) 0.7354(3) 0.87799(11) 0.0360(8) Uani 1 1 d . . . H55 H -0.1435 0.7174 0.8548 0.043 Uiso 1 1 calc R . . C56 C -0.0486(3) 0.8061(2) 0.88125(10) 0.0280(7) Uani 1 1 d . . . N57 N 0.0063(2) 0.8271(2) 0.97487(8) 0.0311(6) Uani 1 1 d . . . N58 N 0.0732(2) 0.8996(2) 0.96874(8) 0.0291(6) Uani 1 1 d . . . C59 C 0.1031(3) 0.9267(3) 1.00156(10) 0.0377(9) Uani 1 1 d . . . H59 H 0.1496 0.9760 1.0059 0.045 Uiso 1 1 calc R . . C60 C 0.0570(4) 0.8728(4) 1.02949(11) 0.0473(11) Uani 1 1 d . . . H60 H 0.0664 0.8786 1.0552 0.057 Uiso 1 1 calc R . . C61 C -0.0040(3) 0.8107(3) 1.01176(11) 0.0437(10) Uani 1 1 d . . . H61 H -0.0458 0.7647 1.0229 0.052 Uiso 1 1 calc R . . N62 N -0.0068(2) 0.8600(2) 0.85281(8) 0.0285(6) Uani 1 1 d . . . N63 N 0.0652(2) 0.9239(2) 0.86217(8) 0.0284(6) Uani 1 1 d . . . C64 C 0.0929(3) 0.9642(3) 0.83096(9) 0.0341(8) Uani 1 1 d . . . H64 H 0.1412 1.0128 0.8289 0.041 Uiso 1 1 calc R . . C65 C 0.0413(3) 0.9254(3) 0.80143(10) 0.0410(9) Uani 1 1 d . . . H65 H 0.0487 0.9413 0.7762 0.049 Uiso 1 1 calc R . . C66 C -0.0215(3) 0.8605(3) 0.81593(10) 0.0356(8) Uani 1 1 d . . . H66 H -0.0672 0.8226 0.8028 0.043 Uiso 1 1 calc R . . B67 B 0.7991(3) 0.6579(3) 0.76647(12) 0.0363(9) Uani 1 1 d . . . F68 F 0.70123(17) 0.6490(2) 0.76031(7) 0.0450(6) Uani 1 1 d . . . F69 F 0.8233(2) 0.6303(2) 0.80168(7) 0.0584(7) Uani 1 1 d . . . F70 F 0.8480(3) 0.5979(3) 0.74224(9) 0.0842(12) Uani 1 1 d . . . F71 F 0.8286(4) 0.7508(3) 0.76081(13) 0.1071(16) Uani 1 1 d . . . B72 B 0.6638(4) -0.0317(3) 0.88107(13) 0.0379(9) Uani 1 1 d . . . F73 F 0.6933(2) 0.05329(19) 0.89804(7) 0.0503(6) Uani 1 1 d . . . F74 F 0.56750(19) -0.0488(2) 0.88974(8) 0.0559(7) Uani 1 1 d . . . F75 F 0.6697(3) -0.0217(2) 0.84331(7) 0.0638(8) Uani 1 1 d . . . F76 F 0.7198(3) -0.1063(3) 0.89291(11) 0.0859(12) Uani 1 1 d . . . B77 B 0.1246(3) 0.4852(3) 0.92153(12) 0.0381(10) Uani 1 1 d D . . F78A F 0.0771(8) 0.5716(6) 0.9283(4) 0.074(4) Uani 0.50 1 d PD A 1 F79A F 0.1525(8) 0.4398(10) 0.9533(2) 0.074(6) Uani 0.50 1 d PD A 1 F80A F 0.0620(9) 0.4317(9) 0.9021(3) 0.095(5) Uani 0.50 1 d PD A 1 F81A F 0.2079(8) 0.5082(9) 0.9001(3) 0.068(4) Uani 0.50 1 d PD A 1 F78B F 0.152(2) 0.4378(17) 0.9535(5) 0.102(13) Uiso 0.30 1 d PD A 2 F79B F 0.0848(15) 0.4213(11) 0.8976(5) 0.051(4) Uiso 0.30 1 d PD A 2 F80B F 0.0599(14) 0.5579(13) 0.9295(6) 0.075(7) Uiso 0.30 1 d PD A 2 F81B F 0.2069(10) 0.5270(13) 0.9056(5) 0.032(3) Uiso 0.30 1 d PD A 2 F78C F 0.1217(13) 0.4174(11) 0.9512(4) 0.044(5) Uiso 0.20 1 d PD A 3 F79C F 0.1997(10) 0.5394(10) 0.9212(5) 0.062(5) Uiso 0.20 1 d PD A 3 F80C F 0.0334(10) 0.5246(13) 0.9184(5) 0.077(5) Uiso 0.20 1 d PD A 3 F81C F 0.1284(15) 0.4172(11) 0.8911(4) 0.073(5) Uiso 0.20 1 d PD A 3 B82A B 0.6738(7) 0.4081(7) 0.9093(4) 0.039(3) Uani 0.60 1 d PD B 1 F83A F 0.7383(5) 0.3317(4) 0.90381(19) 0.0441(14) Uani 0.60 1 d PD B 1 F84A F 0.7164(7) 0.4978(4) 0.9026(3) 0.067(3) Uani 0.60 1 d PD B 1 F85A F 0.5978(4) 0.3964(4) 0.88526(15) 0.0646(14) Uani 0.60 1 d PD B 1 F86A F 0.6377(5) 0.4046(4) 0.94413(14) 0.0706(16) Uani 0.60 1 d PD B 1 B82B B 0.6786(12) 0.4003(13) 0.9010(5) 0.048(7) Uiso 0.40 1 d PD C 2 F83B F 0.6646(7) 0.3900(6) 0.8638(2) 0.069(2) Uiso 0.40 1 d PD C 2 F84B F 0.5965(8) 0.3711(8) 0.9182(3) 0.096(3) Uiso 0.40 1 d PD C 2 F85B F 0.7574(7) 0.3448(8) 0.9107(3) 0.045(3) Uiso 0.40 1 d PD C 2 F86B F 0.7007(15) 0.4956(10) 0.9092(6) 0.100(7) Uiso 0.40 1 d PD C 2 C87 C 0.3954(4) 0.4373(4) 0.93740(14) 0.0553(12) Uani 1 1 d . . . H87A H 0.3809 0.3696 0.9432 0.066 Uiso 1 1 calc R . . H87B H 0.3467 0.4792 0.9488 0.066 Uiso 1 1 calc R . . H87C H 0.4597 0.4539 0.9469 0.066 Uiso 1 1 calc R . . N88 N 0.3940(3) 0.4507(3) 0.89839(11) 0.0470(9) Uani 1 1 d . . . O89 O 0.4124(3) 0.5308(3) 0.88574(12) 0.0726(12) Uani 1 1 d . . . O90 O 0.3742(3) 0.3804(3) 0.87961(11) 0.0689(11) Uani 1 1 d . . . C91 C 0.8022(5) 0.8494(4) 0.67994(15) 0.0652(15) Uani 1 1 d . . . H91A H 0.7363 0.8636 0.6883 0.098 Uiso 1 1 calc R . . H91B H 0.8173 0.8892 0.6584 0.098 Uiso 1 1 calc R . . H91C H 0.8482 0.8638 0.6997 0.098 Uiso 1 1 calc R . . N92 N 0.8095(3) 0.7452(3) 0.66993(9) 0.0423(8) Uani 1 1 d . . . O93 O 0.7397(3) 0.6941(3) 0.67324(11) 0.0747(13) Uani 1 1 d . . . O94 O 0.8871(3) 0.7172(3) 0.65794(10) 0.0632(10) Uani 1 1 d . . . C95 C 0.1397(5) 0.5893(4) 1.02164(18) 0.0715(16) Uani 1 1 d . . . H95A H 0.0957 0.6430 1.0164 0.107 Uiso 1 1 calc R . . H95B H 0.1405 0.5767 1.0481 0.107 Uiso 1 1 calc R . . H95C H 0.1176 0.5312 1.0087 0.107 Uiso 1 1 calc R . . N96 N 0.2387(5) 0.6146(4) 1.00921(11) 0.0675(14) Uani 1 1 d . . . O97 O 0.3029(4) 0.5568(4) 1.01537(13) 0.0860(14) Uani 1 1 d . . . O98 O 0.2476(5) 0.6932(4) 0.99350(13) 0.1046(19) Uani 1 1 d . . . C99 C -0.0980(6) 0.4303(6) 0.96711(19) 0.091(2) Uani 1 1 d . . . H99A H -0.0438 0.4687 0.9577 0.137 Uiso 1 1 calc R . . H99B H -0.1484 0.4258 0.9483 0.137 Uiso 1 1 calc R . . H99C H -0.0751 0.3652 0.9734 0.137 Uiso 1 1 calc R . . N100 N -0.1348(6) 0.4733(4) 0.99752(13) 0.103(3) Uani 1 1 d . . . O101 O -0.1423(4) 0.5472(3) 1.00851(10) 0.0830(15) Uani 1 1 d . . . O102 O -0.2154(4) 0.4119(4) 1.00642(14) 0.0948(15) Uani 1 1 d . . . C103 C -0.1058(12) 0.4470(12) 0.8464(3) 0.051(4) Uani 0.60 1 d P D 1 H10A H -0.1719 0.4316 0.8542 0.077 Uiso 0.60 1 calc PR D 1 H10B H -0.0953 0.5169 0.8482 0.077 Uiso 0.60 1 calc PR D 1 H10C H -0.0595 0.4134 0.8623 0.077 Uiso 0.60 1 calc PR D 1 N104 N -0.0916(10) 0.4151(6) 0.8077(3) 0.068(4) Uani 0.60 1 d P D 1 O105 O -0.0162(7) 0.4234(5) 0.79160(18) 0.0728(19) Uani 0.60 1 d P D 1 O106 O -0.1635(11) 0.3813(5) 0.7906(3) 0.099(4) Uani 0.60 1 d P D 1 C107 C -0.099(3) 0.427(3) 0.8499(9) 0.083(11) Uiso 0.40 1 d P E 2 H10D H -0.1438 0.4465 0.8693 0.124 Uiso 0.40 1 calc PR E 2 H10E H -0.0494 0.4777 0.8467 0.124 Uiso 0.40 1 calc PR E 2 H10F H -0.0671 0.3664 0.8567 0.124 Uiso 0.40 1 calc PR E 2 N108 N -0.1574(12) 0.4129(9) 0.8116(4) 0.048(3) Uiso 0.40 1 d P E 2 O109 O -0.2426(9) 0.4082(8) 0.8125(3) 0.068(3) Uiso 0.40 1 d P E 2 O110 O -0.1025(13) 0.3973(11) 0.7906(5) 0.069(4) Uiso 0.40 1 d P E 2 N112 N 0.5789(6) 0.2216(6) 0.9761(2) 0.090(2) Uani 0.80 1 d P . . C111 C 0.6753(5) 0.1943(5) 0.97450(17) 0.0742(17) Uani 1 1 d . F 1 H11A H 0.7152 0.2432 0.9868 0.111 Uiso 1 1 calc R F 1 H11B H 0.6953 0.1887 0.9488 0.111 Uiso 1 1 calc R F 1 H11C H 0.6836 0.1318 0.9868 0.111 Uiso 1 1 calc R F 1 O113 O 0.5605(10) 0.2806(9) 1.0013(3) 0.076(3) Uiso 0.40 1 d P F 1 O114 O 0.5260(10) 0.1704(10) 0.9621(3) 0.085(3) Uiso 0.40 1 d P F 1 C115 C 0.5355(11) 0.2133(10) 0.9362(4) 0.057(3) Uiso 0.40 1 d P F 2 H11D H 0.5803 0.1769 0.9206 0.085 Uiso 0.40 1 calc PR F 2 H11E H 0.5260 0.2782 0.9260 0.085 Uiso 0.40 1 calc PR F 2 H11F H 0.4731 0.1796 0.9373 0.085 Uiso 0.40 1 calc PR F 2 O116 O 0.5199(11) 0.2632(9) 0.9899(3) 0.079(3) Uiso 0.40 1 d P F 2 O117 O -0.0246(9) 0.4831(8) 1.0195(3) 0.104(3) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0212(2) 0.0213(2) 0.0240(2) 0.00004(17) -0.00259(19) 0.00038(18) N2 0.0255(15) 0.0205(12) 0.0262(13) -0.0011(10) -0.0002(11) 0.0011(12) C3 0.0250(18) 0.0289(17) 0.0284(16) 0.0006(13) -0.0018(14) 0.0027(14) C4 0.033(2) 0.050(2) 0.0251(16) 0.0016(16) -0.0058(15) 0.0021(17) C5 0.029(2) 0.059(2) 0.0314(18) -0.0062(17) -0.0062(16) 0.001(2) C6 0.0229(18) 0.044(2) 0.039(2) 0.0001(16) -0.0033(15) 0.0016(17) C7 0.0254(16) 0.0270(15) 0.0276(15) 0.0000(13) 0.0001(14) 0.0023(14) N8 0.0250(16) 0.0322(15) 0.0251(13) 0.0013(11) 0.0005(12) -0.0001(12) N9 0.0196(14) 0.0219(13) 0.0287(13) 0.0006(10) -0.0042(11) -0.0008(11) C10 0.0243(18) 0.0269(17) 0.0369(18) -0.0036(14) -0.0005(15) -0.0010(14) C11 0.031(2) 0.035(2) 0.0367(19) -0.0028(15) 0.0080(16) -0.0045(15) C12 0.031(2) 0.040(2) 0.0313(17) 0.0024(14) 0.0011(16) -0.0056(16) N13 0.0224(15) 0.0303(15) 0.0310(14) -0.0009(11) 0.0002(12) 0.0015(12) N14 0.0259(15) 0.0268(15) 0.0277(14) -0.0026(11) -0.0026(12) -0.0016(12) C15 0.036(2) 0.0331(18) 0.0279(17) -0.0014(14) 0.0006(16) -0.0007(16) C16 0.030(2) 0.039(2) 0.040(2) 0.0059(16) 0.0091(17) -0.0005(16) C17 0.028(2) 0.0353(19) 0.0395(19) 0.0031(15) 0.0053(16) 0.0007(15) N18 0.0224(14) 0.0267(14) 0.0257(13) 0.0030(11) -0.0006(11) -0.0005(12) C19 0.0245(17) 0.0276(16) 0.0258(16) -0.0006(12) -0.0026(14) -0.0011(14) C20 0.0280(19) 0.0363(19) 0.0326(18) -0.0007(14) -0.0042(15) -0.0018(15) C21 0.032(2) 0.043(2) 0.0372(19) 0.0079(16) -0.0084(17) 0.0001(17) C22 0.0274(19) 0.0332(18) 0.0362(18) 0.0075(14) -0.0019(15) 0.0024(15) C23 0.0240(16) 0.0247(15) 0.0247(14) 0.0035(12) 0.0017(13) -0.0021(13) N24 0.0273(15) 0.0238(13) 0.0273(13) -0.0026(10) -0.0034(12) -0.0019(12) N25 0.0245(15) 0.0239(13) 0.0255(13) -0.0007(10) -0.0038(12) 0.0004(11) C26 0.0295(19) 0.0255(16) 0.0393(19) 0.0025(14) -0.0040(15) 0.0033(14) C27 0.039(2) 0.0253(16) 0.045(2) -0.0011(15) -0.0026(18) 0.0050(16) C28 0.036(2) 0.0274(17) 0.0358(18) -0.0063(14) -0.0043(16) -0.0052(15) N29 0.0246(15) 0.0243(14) 0.0337(15) 0.0022(11) -0.0008(12) 0.0021(11) N30 0.0266(15) 0.0260(13) 0.0248(13) 0.0038(11) -0.0011(12) 0.0002(11) C31 0.035(2) 0.0265(16) 0.0288(16) 0.0008(12) 0.0023(15) -0.0015(15) C32 0.049(3) 0.0231(16) 0.042(2) -0.0012(14) 0.0025(19) 0.0054(17) C33 0.039(2) 0.0235(17) 0.0403(19) 0.0021(14) 0.0016(17) 0.0070(15) Fe34 0.0228(2) 0.0229(2) 0.0241(2) -0.00114(17) 0.00012(19) -0.00157(19) N35 0.0275(15) 0.0237(13) 0.0258(13) 0.0017(11) -0.0023(12) -0.0004(11) C36 0.0275(18) 0.0237(15) 0.0283(16) -0.0017(12) -0.0024(15) 0.0021(14) C37 0.042(2) 0.0252(17) 0.0373(19) -0.0008(14) -0.0022(17) -0.0031(15) C38 0.0308(19) 0.0275(16) 0.0390(18) 0.0043(15) -0.0022(16) -0.0086(15) C39 0.0271(17) 0.0322(16) 0.0324(17) 0.0002(14) -0.0013(15) 0.0003(15) C40 0.0260(17) 0.0233(15) 0.0236(15) 0.0009(12) -0.0011(14) -0.0013(13) N41 0.0273(16) 0.0238(14) 0.0358(16) -0.0020(12) 0.0004(13) 0.0038(11) N42 0.0248(15) 0.0297(14) 0.0275(14) -0.0015(11) -0.0017(12) 0.0018(12) C43 0.0245(17) 0.0428(19) 0.0307(17) -0.0013(15) -0.0019(15) 0.0045(16) C44 0.0306(19) 0.045(2) 0.0334(18) 0.0003(15) -0.0017(15) 0.0159(18) C45 0.034(2) 0.0322(18) 0.0348(19) -0.0030(14) -0.0013(16) 0.0101(16) N46 0.0238(15) 0.0235(13) 0.0280(14) -0.0019(10) -0.0004(12) 0.0012(11) N47 0.0274(15) 0.0253(14) 0.0227(13) 0.0003(10) -0.0017(12) -0.0029(11) C48 0.036(2) 0.0249(16) 0.0306(17) -0.0027(13) -0.0020(15) 0.0034(14) C49 0.043(2) 0.0286(17) 0.0345(19) -0.0013(14) -0.0007(17) 0.0097(17) C50 0.0265(18) 0.0321(17) 0.0326(18) 0.0001(14) -0.0016(14) 0.0054(14) N51 0.0218(14) 0.0280(13) 0.0284(13) -0.0019(12) -0.0005(12) -0.0022(12) C52 0.034(2) 0.0271(17) 0.0317(17) 0.0038(14) 0.0033(15) 0.0008(15) C53 0.037(2) 0.0313(19) 0.049(2) 0.0084(16) 0.0046(18) -0.0066(16) C54 0.031(2) 0.0319(18) 0.061(3) -0.0014(17) 0.004(2) -0.0123(16) C55 0.032(2) 0.0334(19) 0.042(2) -0.0080(15) -0.0067(17) -0.0018(16) C56 0.0254(18) 0.0249(16) 0.0336(17) -0.0001(13) -0.0017(14) 0.0014(13) N57 0.0327(17) 0.0326(15) 0.0280(14) 0.0042(12) 0.0035(12) -0.0031(14) N58 0.0268(16) 0.0305(14) 0.0301(15) -0.0009(11) 0.0008(12) 0.0010(12) C59 0.034(2) 0.051(2) 0.0279(17) -0.0057(16) 0.0007(15) -0.0015(19) C60 0.054(3) 0.059(3) 0.0285(19) -0.0005(18) -0.0008(19) 0.007(2) C61 0.045(3) 0.053(2) 0.0336(19) 0.0079(17) 0.0077(18) 0.001(2) N62 0.0284(16) 0.0299(15) 0.0271(14) -0.0004(11) -0.0039(12) -0.0018(12) N63 0.0280(16) 0.0292(14) 0.0279(14) -0.0030(11) -0.0013(12) -0.0002(12) C64 0.040(2) 0.0371(18) 0.0252(16) 0.0041(14) 0.0052(16) 0.0012(17) C65 0.056(3) 0.042(2) 0.0255(16) 0.0034(16) 0.0001(17) 0.004(2) C66 0.039(2) 0.0376(19) 0.0304(17) -0.0084(15) -0.0084(17) 0.0054(17) B67 0.029(2) 0.041(2) 0.039(2) 0.0006(18) -0.0084(18) -0.0004(18) F68 0.0266(12) 0.0648(16) 0.0438(13) 0.0009(11) -0.0092(10) 0.0009(11) F69 0.0516(17) 0.087(2) 0.0368(13) 0.0051(13) -0.0116(12) 0.0070(15) F70 0.056(2) 0.137(3) 0.0598(18) -0.0211(19) 0.0051(16) 0.037(2) F71 0.120(4) 0.067(2) 0.135(3) 0.034(2) -0.070(3) -0.052(2) B72 0.035(2) 0.039(2) 0.040(2) -0.0045(17) -0.003(2) 0.001(2) F73 0.0473(15) 0.0529(15) 0.0507(14) -0.0096(12) -0.0086(12) -0.0156(12) F74 0.0354(15) 0.0704(18) 0.0620(16) -0.0073(14) -0.0012(12) -0.0193(13) F75 0.079(2) 0.0723(19) 0.0404(13) -0.0138(13) 0.0050(15) -0.0070(17) F76 0.091(3) 0.073(2) 0.093(2) -0.0077(19) -0.017(2) 0.046(2) B77 0.044(3) 0.037(2) 0.033(2) 0.0025(17) -0.0060(19) 0.0039(19) F78A 0.060(5) 0.026(3) 0.135(9) 0.004(3) 0.048(5) 0.012(3) F79A 0.037(4) 0.144(12) 0.041(4) 0.063(6) 0.006(3) 0.013(5) F80A 0.104(10) 0.106(8) 0.074(6) -0.027(5) 0.003(6) -0.066(8) F81A 0.066(5) 0.079(8) 0.060(7) 0.019(6) 0.017(4) 0.006(5) B82A 0.036(5) 0.023(4) 0.057(6) 0.008(4) 0.003(4) 0.004(3) F83A 0.036(3) 0.038(3) 0.058(3) -0.002(2) -0.007(3) 0.011(2) F84A 0.062(4) 0.019(2) 0.119(7) 0.006(2) -0.003(4) -0.007(2) F85A 0.058(3) 0.060(3) 0.076(3) 0.004(2) -0.033(3) 0.003(2) F86A 0.088(4) 0.062(3) 0.062(3) -0.012(2) 0.029(3) 0.013(3) C87 0.051(3) 0.055(3) 0.060(3) -0.010(2) 0.000(2) -0.009(2) N88 0.043(2) 0.0340(19) 0.064(2) -0.0051(16) 0.0097(18) -0.0006(16) O89 0.074(3) 0.0419(18) 0.102(3) 0.0102(18) 0.047(2) 0.0032(18) O90 0.090(3) 0.048(2) 0.070(2) -0.0156(16) -0.006(2) -0.0014(19) C91 0.075(4) 0.064(3) 0.057(3) -0.008(2) 0.001(3) 0.012(3) N92 0.0324(19) 0.057(2) 0.0374(18) 0.0066(16) -0.0054(15) 0.0037(17) O93 0.052(2) 0.107(3) 0.065(2) 0.032(2) -0.0181(18) -0.036(2) O94 0.045(2) 0.087(3) 0.058(2) -0.0101(18) -0.0026(16) 0.0280(19) C95 0.075(4) 0.061(3) 0.078(4) 0.014(3) 0.006(3) 0.008(3) N96 0.092(4) 0.075(3) 0.035(2) 0.001(2) -0.010(2) -0.008(3) O97 0.075(3) 0.111(4) 0.072(3) -0.004(3) -0.004(2) 0.030(3) O98 0.123(5) 0.111(4) 0.080(3) 0.035(3) -0.027(3) -0.034(4) C99 0.090(5) 0.097(5) 0.086(4) -0.045(4) -0.027(4) 0.024(4) N100 0.182(7) 0.078(4) 0.050(3) 0.032(2) 0.052(4) 0.071(4) O101 0.149(5) 0.046(2) 0.054(2) -0.0026(16) 0.032(3) -0.023(3) O102 0.091(4) 0.109(4) 0.085(3) 0.017(3) 0.014(3) -0.010(3) C103 0.067(7) 0.064(7) 0.023(4) 0.018(4) -0.012(4) -0.029(6) N104 0.101(11) 0.039(4) 0.063(5) 0.008(3) -0.063(7) -0.026(5) O105 0.098(6) 0.071(4) 0.049(3) -0.005(3) 0.008(4) 0.005(4) O106 0.150(10) 0.059(4) 0.089(6) 0.018(4) -0.101(6) -0.050(5) N112 0.059(4) 0.099(5) 0.111(6) 0.007(5) 0.037(4) 0.003(4) C111 0.090(5) 0.070(4) 0.063(3) 0.019(3) 0.007(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.902(3) . ? Fe1 N18 1.903(3) . ? Fe1 N30 1.951(3) . ? Fe1 N14 1.972(3) . ? Fe1 N9 1.975(3) . ? Fe1 N25 1.991(3) . ? N2 C7 1.337(5) . ? N2 C3 1.340(4) . ? C3 C4 1.379(5) . ? C3 N8 1.409(5) . ? C4 C5 1.398(6) . ? C5 C6 1.397(5) . ? C6 C7 1.382(5) . ? C7 N13 1.412(4) . ? N8 C12 1.350(5) . ? N8 N9 1.389(4) . ? N9 C10 1.322(5) . ? C10 C11 1.401(5) . ? C11 C12 1.362(6) . ? N13 C17 1.360(5) . ? N13 N14 1.371(4) . ? N14 C15 1.328(5) . ? C15 C16 1.426(6) . ? C16 C17 1.363(6) . ? N18 C23 1.330(5) . ? N18 C19 1.344(5) . ? C19 C20 1.385(5) . ? C19 N24 1.392(4) . ? C20 C21 1.383(6) . ? C21 C22 1.385(6) . ? C22 C23 1.381(5) . ? C23 N29 1.404(4) . ? N24 C28 1.358(5) . ? N24 N25 1.384(4) . ? N25 C26 1.326(5) . ? C26 C27 1.410(5) . ? C27 C28 1.370(6) . ? N29 C33 1.359(5) . ? N29 N30 1.381(4) . ? N30 C31 1.319(5) . ? C31 C32 1.402(5) . ? C32 C33 1.355(6) . ? Fe34 N35 1.899(3) . ? Fe34 N51 1.903(3) . ? Fe34 N47 1.974(3) . ? Fe34 N63 1.976(3) . ? Fe34 N42 1.977(3) . ? Fe34 N58 1.983(3) . ? N35 C40 1.340(5) . ? N35 C36 1.343(4) . ? C36 C37 1.377(5) . ? C36 N41 1.405(5) . ? C37 C38 1.395(6) . ? C38 C39 1.402(5) . ? C39 C40 1.384(5) . ? C40 N46 1.401(4) . ? N41 C45 1.361(5) . ? N41 N42 1.376(4) . ? N42 C43 1.326(5) . ? C43 C44 1.410(6) . ? C44 C45 1.369(6) . ? N46 C50 1.359(5) . ? N46 N47 1.381(4) . ? N47 C48 1.337(5) . ? C48 C49 1.414(6) . ? C49 C50 1.357(5) . ? N51 C52 1.332(5) . ? N51 C56 1.338(5) . ? C52 C53 1.388(6) . ? C52 N57 1.393(5) . ? C53 C54 1.381(6) . ? C54 C55 1.383(6) . ? C55 C56 1.373(5) . ? C56 N62 1.402(5) . ? N57 C61 1.370(5) . ? N57 N58 1.381(4) . ? N58 C59 1.319(5) . ? C59 C60 1.413(6) . ? C60 C61 1.365(7) . ? N62 C66 1.359(5) . ? N62 N63 1.373(4) . ? N63 C64 1.322(5) . ? C64 C65 1.398(6) . ? C65 C66 1.355(6) . ? B67 F71 1.365(6) . ? B67 F68 1.376(5) . ? B67 F69 1.379(5) . ? B67 F70 1.386(6) . ? B72 F76 1.360(6) . ? B72 F75 1.385(5) . ? B72 F74 1.387(6) . ? B72 F73 1.389(5) . ? B77 F79C 1.279(12) . ? B77 F80A 1.340(9) . ? B77 F79B 1.358(13) . ? B77 F79A 1.371(7) . ? B77 F80B 1.377(13) . ? B77 F80C 1.377(12) . ? B77 F78A 1.386(8) . ? B77 F78B 1.388(13) . ? B77 F81B 1.401(13) . ? B77 F81A 1.426(10) . ? B77 F78C 1.430(12) . ? B77 F81C 1.456(12) . ? B82A F86A 1.364(14) . ? B82A F85A 1.377(11) . ? B82A F84A 1.395(9) . ? B82A F83A 1.396(10) . ? B82B F84B 1.358(16) . ? B82B F85B 1.376(16) . ? B82B F83B 1.377(16) . ? B82B F86B 1.386(16) . ? C87 N88 1.433(6) . ? N88 O90 1.219(5) . ? N88 O89 1.227(5) . ? C91 N92 1.490(7) . ? N92 O93 1.201(5) . ? N92 O94 1.221(5) . ? C95 N96 1.482(9) . ? N96 O97 1.215(7) . ? N96 O98 1.235(7) . ? C99 N100 1.356(8) . ? N100 O101 1.104(7) . ? N100 O102 1.438(10) . ? N100 O117 1.726(15) . ? C103 N104 1.492(19) . ? N104 O105 1.200(18) . ? N104 O106 1.261(11) . ? C107 N108 1.62(4) . ? N108 O110 1.101(18) . ? N108 O109 1.18(2) . ? N112 O116 1.117(14) . ? N112 O114 1.139(14) . ? N112 O113 1.254(14) . ? N112 C111 1.386(10) . ? N112 C115 1.576(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N18 178.26(13) . . ? N2 Fe1 N30 98.27(12) . . ? N18 Fe1 N30 80.35(12) . . ? N2 Fe1 N14 79.95(12) . . ? N18 Fe1 N14 101.11(12) . . ? N30 Fe1 N14 91.88(12) . . ? N2 Fe1 N9 80.40(12) . . ? N18 Fe1 N9 98.47(12) . . ? N30 Fe1 N9 88.08(12) . . ? N14 Fe1 N9 160.13(12) . . ? N2 Fe1 N25 101.40(12) . . ? N18 Fe1 N25 80.00(12) . . ? N30 Fe1 N25 160.33(12) . . ? N14 Fe1 N25 91.15(12) . . ? N9 Fe1 N25 95.55(12) . . ? C7 N2 C3 119.8(3) . . ? C7 N2 Fe1 120.1(2) . . ? C3 N2 Fe1 119.9(2) . . ? N2 C3 C4 123.2(3) . . ? N2 C3 N8 111.1(3) . . ? C4 C3 N8 125.7(3) . . ? C3 C4 C5 116.1(3) . . ? C6 C5 C4 121.7(4) . . ? C7 C6 C5 116.8(4) . . ? N2 C7 C6 122.3(3) . . ? N2 C7 N13 110.6(3) . . ? C6 C7 N13 127.0(3) . . ? C12 N8 N9 110.9(3) . . ? C12 N8 C3 132.2(3) . . ? N9 N8 C3 116.1(3) . . ? C10 N9 N8 104.7(3) . . ? C10 N9 Fe1 142.5(2) . . ? N8 N9 Fe1 112.4(2) . . ? N9 C10 C11 111.3(3) . . ? C12 C11 C10 105.9(3) . . ? N8 C12 C11 107.2(3) . . ? C17 N13 N14 111.8(3) . . ? C17 N13 C7 131.9(3) . . ? N14 N13 C7 116.2(3) . . ? C15 N14 N13 105.5(3) . . ? C15 N14 Fe1 141.4(3) . . ? N13 N14 Fe1 113.0(2) . . ? N14 C15 C16 109.9(4) . . ? C17 C16 C15 106.2(4) . . ? N13 C17 C16 106.5(4) . . ? C23 N18 C19 120.2(3) . . ? C23 N18 Fe1 119.9(2) . . ? C19 N18 Fe1 119.9(2) . . ? N18 C19 C20 121.9(3) . . ? N18 C19 N24 111.2(3) . . ? C20 C19 N24 126.9(3) . . ? C21 C20 C19 116.3(3) . . ? C20 C21 C22 123.1(4) . . ? C23 C22 C21 115.9(3) . . ? N18 C23 C22 122.7(3) . . ? N18 C23 N29 110.5(3) . . ? C22 C23 N29 126.8(3) . . ? C28 N24 N25 110.4(3) . . ? C28 N24 C19 132.7(3) . . ? N25 N24 C19 116.8(3) . . ? C26 N25 N24 105.7(3) . . ? C26 N25 Fe1 142.2(3) . . ? N24 N25 Fe1 112.0(2) . . ? N25 C26 C27 110.7(3) . . ? C28 C27 C26 105.7(3) . . ? N24 C28 C27 107.4(3) . . ? C33 N29 N30 110.5(3) . . ? C33 N29 C23 133.0(3) . . ? N30 N29 C23 116.5(3) . . ? C31 N30 N29 105.2(3) . . ? C31 N30 Fe1 142.0(3) . . ? N29 N30 Fe1 112.7(2) . . ? N30 C31 C32 111.1(3) . . ? C33 C32 C31 106.0(3) . . ? C32 C33 N29 107.2(3) . . ? N35 Fe34 N51 177.53(13) . . ? N35 Fe34 N47 79.91(12) . . ? N51 Fe34 N47 100.12(12) . . ? N35 Fe34 N63 97.69(13) . . ? N51 Fe34 N63 79.85(13) . . ? N47 Fe34 N63 92.25(12) . . ? N35 Fe34 N42 80.35(12) . . ? N51 Fe34 N42 99.64(13) . . ? N47 Fe34 N42 160.24(12) . . ? N63 Fe34 N42 91.18(12) . . ? N35 Fe34 N58 102.40(13) . . ? N51 Fe34 N58 80.07(13) . . ? N47 Fe34 N58 91.64(12) . . ? N63 Fe34 N58 159.91(13) . . ? N42 Fe34 N58 91.79(12) . . ? C40 N35 C36 119.6(3) . . ? C40 N35 Fe34 120.3(2) . . ? C36 N35 Fe34 120.1(3) . . ? N35 C36 C37 122.7(3) . . ? N35 C36 N41 110.1(3) . . ? C37 C36 N41 127.1(3) . . ? C36 C37 C38 117.0(3) . . ? C37 C38 C39 121.4(3) . . ? C40 C39 C38 116.6(3) . . ? N35 C40 C39 122.7(3) . . ? N35 C40 N46 110.7(3) . . ? C39 C40 N46 126.6(3) . . ? C45 N41 N42 111.3(3) . . ? C45 N41 C36 131.3(3) . . ? N42 N41 C36 117.4(3) . . ? C43 N42 N41 105.7(3) . . ? C43 N42 Fe34 142.3(3) . . ? N41 N42 Fe34 112.0(2) . . ? N42 C43 C44 110.2(4) . . ? C45 C44 C43 106.6(3) . . ? N41 C45 C44 106.2(4) . . ? C50 N46 N47 111.0(3) . . ? C50 N46 C40 132.5(3) . . ? N47 N46 C40 116.3(3) . . ? C48 N47 N46 105.5(3) . . ? C48 N47 Fe34 141.8(3) . . ? N46 N47 Fe34 112.7(2) . . ? N47 C48 C49 109.8(3) . . ? C50 C49 C48 106.8(3) . . ? C49 C50 N46 107.0(3) . . ? C52 N51 C56 119.6(3) . . ? C52 N51 Fe34 119.9(2) . . ? C56 N51 Fe34 120.5(2) . . ? N51 C52 C53 121.9(3) . . ? N51 C52 N57 111.2(3) . . ? C53 C52 N57 126.9(3) . . ? C54 C53 C52 117.2(4) . . ? C53 C54 C55 121.6(4) . . ? C56 C55 C54 116.8(4) . . ? N51 C56 C55 122.9(3) . . ? N51 C56 N62 110.0(3) . . ? C55 C56 N62 127.1(3) . . ? C61 N57 N58 110.4(3) . . ? C61 N57 C52 132.5(4) . . ? N58 N57 C52 117.0(3) . . ? C59 N58 N57 105.6(3) . . ? C59 N58 Fe34 142.5(3) . . ? N57 N58 Fe34 111.8(2) . . ? N58 C59 C60 111.1(4) . . ? C61 C60 C59 105.6(4) . . ? C60 C61 N57 107.2(4) . . ? C66 N62 N63 110.5(3) . . ? C66 N62 C56 132.2(3) . . ? N63 N62 C56 117.2(3) . . ? C64 N63 N62 105.5(3) . . ? C64 N63 Fe34 142.1(3) . . ? N62 N63 Fe34 112.3(2) . . ? N63 C64 C65 110.6(4) . . ? C66 C65 C64 106.3(3) . . ? C65 C66 N62 107.0(4) . . ? F71 B67 F68 110.6(4) . . ? F71 B67 F69 109.2(4) . . ? F68 B67 F69 111.4(4) . . ? F71 B67 F70 108.8(5) . . ? F68 B67 F70 108.8(4) . . ? F69 B67 F70 108.0(4) . . ? F76 B72 F75 110.9(4) . . ? F76 B72 F74 110.1(4) . . ? F75 B72 F74 107.4(4) . . ? F76 B72 F73 109.5(4) . . ? F75 B72 F73 109.9(4) . . ? F74 B72 F73 108.9(4) . . ? F80A B77 F79A 111.9(8) . . ? F79B B77 F80B 110.4(11) . . ? F79C B77 F80C 120.6(10) . . ? F80A B77 F78A 105.3(8) . . ? F79A B77 F78A 112.2(8) . . ? F79B B77 F78B 110.0(11) . . ? F80B B77 F78B 110.1(12) . . ? F79B B77 F81B 109.3(11) . . ? F80B B77 F81B 108.3(11) . . ? F78B B77 F81B 108.7(12) . . ? F80A B77 F81A 110.8(8) . . ? F79A B77 F81A 109.7(7) . . ? F78A B77 F81A 106.7(7) . . ? F79C B77 F78C 114.4(10) . . ? F80C B77 F78C 107.1(10) . . ? F79C B77 F81C 110.1(10) . . ? F80C B77 F81C 103.0(10) . . ? F78C B77 F81C 98.8(9) . . ? F86A B82A F85A 108.0(8) . . ? F86A B82A F84A 110.4(10) . . ? F85A B82A F84A 108.3(8) . . ? F86A B82A F83A 109.9(7) . . ? F85A B82A F83A 107.8(9) . . ? F84A B82A F83A 112.3(8) . . ? F84B B82B F85B 112.1(14) . . ? F84B B82B F83B 107.9(13) . . ? F85B B82B F83B 107.8(12) . . ? F84B B82B F86B 111.5(14) . . ? F85B B82B F86B 107.5(14) . . ? F83B B82B F86B 110.0(14) . . ? O90 N88 O89 123.7(5) . . ? O90 N88 C87 117.2(4) . . ? O89 N88 C87 119.1(4) . . ? O93 N92 O94 123.7(5) . . ? O93 N92 C91 119.3(5) . . ? O94 N92 C91 116.9(4) . . ? O97 N96 O98 126.3(7) . . ? O97 N96 C95 117.5(5) . . ? O98 N96 C95 116.2(6) . . ? O101 N100 C99 137.6(7) . . ? O101 N100 O102 113.1(6) . . ? C99 N100 O102 102.5(7) . . ? O101 N100 O117 80.9(8) . . ? C99 N100 O117 94.8(7) . . ? O102 N100 O117 128.7(5) . . ? O105 N104 O106 118.6(17) . . ? O105 N104 C103 123.2(9) . . ? O106 N104 C103 118.1(18) . . ? O110 N108 O109 134(3) . . ? O110 N108 C107 106(3) . . ? O109 N108 C107 118.9(18) . . ? O114 N112 O113 127.1(12) . . ? O116 N112 C111 149.4(12) . . ? O114 N112 C111 115.3(10) . . ? O113 N112 C111 113.8(11) . . ? O116 N112 C115 100.1(11) . . ? C111 N112 C115 107.9(8) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.853 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.165 #=END data_mah35lt _database_code_CSD 171145 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis-[2,6-dipyrazol-1-ylpyridine]iron(II) dihexafluorophosphate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H18 Fe N10, 2[P F6]' _chemical_formula_sum 'C22 H18 F12 Fe N10 P2' _chemical_formula_weight 768.25 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/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 14.2478(4) _cell_length_b 9.4974(3) _cell_length_c 20.5607(5) _cell_angle_alpha 90.00 _cell_angle_beta 99.3180(19) _cell_angle_gamma 90.00 _cell_volume 2745.50(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 10414 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 27.52 _exptl_crystal_description Yellow _exptl_crystal_colour Block _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.859 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7190 _exptl_absorpt_correction_T_max 0.8463 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _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_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'Area detector scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10414 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 27.52 _reflns_number_total 3141 _reflns_number_gt 2855 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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. The F atoms of the PF~6~^-^ anion are disordered about two equally occupied orientations F19-F24 and F25-F30. All P-F distances were restrained to 1.60(2) \%A. ; _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^)+(0.0435P)^2^+2.7013P] 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 SHELXL _refine_ls_extinction_coef 0.0049(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3141 _refine_ls_number_parameters 269 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0896 _refine_ls_wR_factor_gt 0.0867 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.009 _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 0.0000 0.81719(3) 0.2500 0.01901(13) Uani 1 2 d S . . N2 N 0.00995(9) 0.76609(14) 0.35388(6) 0.0196(3) Uani 1 1 d . . . C3 C -0.03627(11) 0.84231(17) 0.39286(8) 0.0214(3) Uani 1 1 d . . . C4 C -0.03860(12) 0.80944(18) 0.45820(8) 0.0254(4) Uani 1 1 d . . . H4 H -0.0746 0.8635 0.4843 0.030 Uiso 1 1 calc R . . C5 C 0.01429(13) 0.69362(18) 0.48372(8) 0.0260(4) Uani 1 1 d . . . H5 H 0.0152 0.6678 0.5285 0.031 Uiso 1 1 calc R . . C6 C 0.06595(12) 0.61476(18) 0.44499(8) 0.0240(3) Uani 1 1 d . . . H6 H 0.1035 0.5366 0.4623 0.029 Uiso 1 1 calc R . . C7 C 0.06002(11) 0.65564(17) 0.38007(8) 0.0211(3) Uani 1 1 d . . . N8 N -0.07999(9) 0.96241(14) 0.36135(6) 0.0215(3) Uani 1 1 d . . . N9 N -0.06953(10) 0.98678(15) 0.29733(6) 0.0226(3) Uani 1 1 d . . . C10 C -0.10411(12) 1.11530(18) 0.28413(8) 0.0261(4) Uani 1 1 d . . . H10 H -0.1066 1.1612 0.2428 0.031 Uiso 1 1 calc R . . C11 C -0.13661(13) 1.17495(18) 0.33918(9) 0.0286(4) Uani 1 1 d . . . H11 H -0.1643 1.2652 0.3421 0.034 Uiso 1 1 calc R . . C12 C -0.11968(12) 1.07497(18) 0.38753(9) 0.0265(4) Uani 1 1 d . . . H12 H -0.1331 1.0827 0.4312 0.032 Uiso 1 1 calc R . . N13 N 0.10772(9) 0.58607(14) 0.33432(6) 0.0212(3) Uani 1 1 d . . . N14 N 0.10531(10) 0.64514(15) 0.27351(7) 0.0221(3) Uani 1 1 d . . . C15 C 0.15334(11) 0.55570(18) 0.24131(8) 0.0249(3) Uani 1 1 d . . . H15 H 0.1634 0.5682 0.1971 0.030 Uiso 1 1 calc R . . C16 C 0.18721(12) 0.44060(18) 0.28108(9) 0.0271(4) Uani 1 1 d . . . H16 H 0.2236 0.3635 0.2695 0.032 Uiso 1 1 calc R . . C17 C 0.15702(12) 0.46250(17) 0.33988(9) 0.0252(4) Uani 1 1 d . . . H17 H 0.1682 0.4031 0.3775 0.030 Uiso 1 1 calc R . . P18 P 0.22133(3) 1.02672(5) 0.41593(2) 0.02432(14) Uani 1 1 d D . . F19 F 0.1889(16) 0.961(3) 0.3442(9) 0.036(4) Uani 0.50 1 d PD A 1 F20 F 0.2507(12) 1.089(3) 0.4893(9) 0.029(2) Uani 0.50 1 d PD A 1 F21 F 0.3326(9) 0.987(2) 0.4194(11) 0.0241(17) Uani 0.50 1 d PD A 1 F22 F 0.2055(18) 0.8766(15) 0.4490(12) 0.040(2) Uani 0.50 1 d PD A 1 F23 F 0.1123(9) 1.0651(18) 0.4163(9) 0.042(3) Uani 0.50 1 d PD A 1 F24 F 0.2366(17) 1.1751(17) 0.3823(12) 0.032(2) Uani 0.50 1 d PD A 1 F25 F 0.2513(17) 1.1648(17) 0.3785(13) 0.031(2) Uani 0.50 1 d PD A 2 F26 F 0.1929(16) 0.947(3) 0.3460(9) 0.028(2) Uani 0.50 1 d PD A 2 F27 F 0.1912(18) 0.8934(16) 0.4530(12) 0.050(4) Uani 0.50 1 d PD A 2 F28 F 0.1158(9) 1.0922(18) 0.4120(10) 0.052(3) Uani 0.50 1 d PD A 2 F29 F 0.2531(14) 1.107(3) 0.4838(9) 0.036(4) Uani 0.50 1 d PD A 2 F30 F 0.3250(10) 0.966(2) 0.4129(12) 0.029(2) Uani 0.50 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02291(19) 0.01839(19) 0.01578(19) 0.000 0.00330(12) 0.000 N2 0.0209(6) 0.0201(6) 0.0182(6) 0.0004(5) 0.0038(5) 0.0000(5) C3 0.0211(7) 0.0237(8) 0.0194(8) -0.0014(6) 0.0030(6) -0.0007(6) C4 0.0276(8) 0.0296(9) 0.0202(8) -0.0032(6) 0.0073(6) -0.0023(7) C5 0.0309(9) 0.0297(9) 0.0174(8) 0.0021(6) 0.0044(6) -0.0052(7) C6 0.0280(8) 0.0229(8) 0.0205(8) 0.0036(6) 0.0018(6) -0.0027(6) C7 0.0215(7) 0.0205(7) 0.0213(8) -0.0004(6) 0.0035(6) -0.0018(6) N8 0.0229(6) 0.0232(7) 0.0183(6) -0.0024(5) 0.0031(5) 0.0023(5) N9 0.0264(7) 0.0242(7) 0.0173(6) -0.0003(5) 0.0036(5) 0.0016(6) C10 0.0296(8) 0.0226(8) 0.0253(8) -0.0004(6) 0.0016(7) 0.0032(7) C11 0.0295(9) 0.0239(8) 0.0313(9) -0.0054(7) 0.0019(7) 0.0064(7) C12 0.0253(8) 0.0287(8) 0.0252(8) -0.0076(7) 0.0030(6) 0.0040(7) N13 0.0247(7) 0.0194(7) 0.0196(7) 0.0024(5) 0.0040(5) 0.0025(5) N14 0.0233(7) 0.0247(7) 0.0188(6) 0.0008(5) 0.0050(5) 0.0007(5) C15 0.0236(8) 0.0275(8) 0.0241(8) -0.0035(7) 0.0052(6) 0.0006(7) C16 0.0259(8) 0.0235(8) 0.0318(9) -0.0045(7) 0.0046(7) 0.0024(7) C17 0.0262(8) 0.0194(8) 0.0292(9) 0.0016(6) 0.0020(7) 0.0023(6) P18 0.0246(2) 0.0291(3) 0.0197(2) -0.00090(16) 0.00488(17) -0.00152(17) F19 0.041(6) 0.042(7) 0.023(3) -0.002(3) -0.001(3) -0.011(5) F20 0.030(3) 0.038(6) 0.019(2) -0.006(4) 0.002(2) 0.001(2) F21 0.025(2) 0.025(5) 0.021(3) -0.009(3) -0.001(2) 0.004(2) F22 0.061(6) 0.0289(19) 0.032(3) 0.0047(19) 0.013(3) -0.013(2) F23 0.025(2) 0.064(4) 0.039(6) -0.021(4) 0.010(3) -0.004(2) F24 0.038(6) 0.022(2) 0.035(4) 0.002(2) 0.008(3) 0.011(3) F25 0.040(6) 0.021(3) 0.035(2) 0.004(2) 0.016(3) 0.010(3) F26 0.033(3) 0.032(3) 0.020(3) -0.005(3) 0.005(3) 0.002(2) F27 0.063(7) 0.057(6) 0.030(3) 0.004(5) 0.010(4) -0.029(6) F28 0.027(3) 0.098(9) 0.030(3) 0.005(4) 0.008(3) 0.015(4) F29 0.048(5) 0.034(5) 0.025(4) -0.005(4) 0.008(2) 0.002(2) F30 0.033(3) 0.023(4) 0.027(4) -0.011(3) -0.003(2) 0.005(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 N2 2.1723(13) . ? Fe1 N9 2.1987(14) . ? Fe1 N14 2.2182(14) . ? N2 C3 1.331(2) . ? N2 C7 1.332(2) . ? C3 C4 1.385(2) . ? C3 N8 1.407(2) . ? C4 C5 1.387(2) . ? C5 C6 1.388(2) . ? C6 C7 1.380(2) . ? C7 N13 1.411(2) . ? N8 C12 1.360(2) . ? N8 N9 1.3683(19) . ? N9 C10 1.328(2) . ? C10 C11 1.409(2) . ? C11 C12 1.368(3) . ? N13 C17 1.363(2) . ? N13 N14 1.3656(18) . ? N14 C15 1.332(2) . ? C15 C16 1.403(2) . ? C16 C17 1.363(2) . ? P18 F27 1.573(13) . ? P18 F29 1.593(13) . ? P18 F30 1.595(13) . ? P18 F23 1.597(12) . ? P18 F19 1.597(13) . ? P18 F24 1.600(13) . ? P18 F22 1.611(12) . ? P18 F20 1.612(12) . ? P18 F25 1.612(13) . ? P18 F28 1.617(12) . ? P18 F26 1.618(12) . ? P18 F21 1.618(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 154.18(7) . 2 ? N2 Fe1 N9 72.00(5) . . ? N2 Fe1 N9 129.52(5) . 2 ? N9 Fe1 N9 85.80(7) . 2 ? N2 Fe1 N14 89.08(5) . 2 ? N9 Fe1 N14 107.38(5) . 2 ? N2 Fe1 N14 71.76(5) . . ? N9 Fe1 N14 141.31(5) . . ? N14 Fe1 N14 85.10(7) 2 . ? C3 N2 C7 118.01(14) . . ? C3 N2 Fe1 120.71(11) . . ? C7 N2 Fe1 121.25(11) . . ? N2 C3 C4 123.62(15) . . ? N2 C3 N8 112.91(13) . . ? C4 C3 N8 123.44(15) . . ? C3 C4 C5 116.65(16) . . ? C4 C5 C6 121.13(15) . . ? C7 C6 C5 116.62(15) . . ? N2 C7 C6 123.89(15) . . ? N2 C7 N13 112.55(14) . . ? C6 C7 N13 123.55(15) . . ? C12 N8 N9 111.39(13) . . ? C12 N8 C3 129.54(14) . . ? N9 N8 C3 118.10(13) . . ? C10 N9 N8 104.92(13) . . ? C10 N9 Fe1 139.62(11) . . ? N8 N9 Fe1 115.40(10) . . ? N9 C10 C11 111.39(15) . . ? C12 C11 C10 105.22(15) . . ? N8 C12 C11 107.08(15) . . ? C17 N13 N14 111.51(13) . . ? C17 N13 C7 130.14(14) . . ? N14 N13 C7 118.34(13) . . ? C15 N14 N13 104.73(13) . . ? C15 N14 Fe1 138.17(11) . . ? N13 N14 Fe1 114.71(10) . . ? N14 C15 C16 111.28(15) . . ? C17 C16 C15 105.65(15) . . ? N13 C17 C16 106.82(15) . . ? F27 P18 F29 91.3(15) . . ? F27 P18 F30 93.2(12) . . ? F29 P18 F30 94.2(10) . . ? F23 P18 F19 87.5(10) . . ? F23 P18 F24 90.1(11) . . ? F19 P18 F24 89.0(15) . . ? F23 P18 F22 89.8(11) . . ? F19 P18 F22 90.4(15) . . ? F24 P18 F22 179.4(14) . . ? F23 P18 F20 91.0(8) . . ? F19 P18 F20 177.8(14) . . ? F24 P18 F20 92.7(15) . . ? F22 P18 F20 87.9(15) . . ? F27 P18 F25 179.2(11) . . ? F29 P18 F25 88.2(16) . . ? F30 P18 F25 87.4(12) . . ? F27 P18 F28 90.5(11) . . ? F29 P18 F28 89.3(10) . . ? F30 P18 F28 174.7(12) . . ? F23 P18 F28 9.9(14) . . ? F27 P18 F26 90.3(14) . . ? F29 P18 F26 177.7(13) . . ? F30 P18 F26 84.1(11) . . ? F25 P18 F26 90.2(15) . . ? F28 P18 F26 92.2(11) . . ? F23 P18 F21 177.2(10) . . ? F19 P18 F21 95.0(11) . . ? F24 P18 F21 91.2(11) . . ? F22 P18 F21 88.9(12) . . ? F20 P18 F21 86.5(9) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.366 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.076