Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email malcolmh@chem.leeds.ac.uk _publ_contact_author_name 'Dr. Malcolm A. Halcrow' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0186 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.Elhaik V.A.Money S.A.Barrett C.A.Kilner I.R.Evans ; M.A.Halcrow ; #================================================================= data_je10rt _database_code_CSD 195908 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(pyrazol-1-yl)pyrazine]iron(II) ditetrafluoroborate tris-nitromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Fe N12, 2[B F4], 3[C H3 N O2]' _chemical_formula_sum 'C23 H25 B2 F8 Fe N15 O6' _chemical_formula_weight 837.05 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.9138(2) _cell_length_b 8.3045(1) _cell_length_c 26.3119(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.4285(4) _cell_angle_gamma 90.00 _cell_volume 3526.13(8) _cell_formula_units_Z 4 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 30653 _cell_measurement_theta_min 1.28 _cell_measurement_theta_max 26.00 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.577 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.531 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7960 _exptl_absorpt_correction_T_max 0.8786 _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 300(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 30653 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.28 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6902 _reflns_number_gt 5334 _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 of the structure contains one complex dication, two BF~4~^-^ anions and three molecules of nitromethane. Both of the BF~4~^-^ anions are disordered over three equally occupied orientations. For the anion cetred on B39, two of these orientations shared a common B atom B39B, which hence had a total occupancy of 0.67. All B-F distances were restrained to 1.39(2)\%A, and F...F distances within a given disorder orientation to 2.27(2)\%A. All three nitromethane molecules are also disordered: C44A-O47A (occupancy 0.50) and C44B-O47B (occupancy 0.50). C48A-O51A (occupancy 0.40), C48B-O51B (occupancy 0.40) and C48C, N49B, O50C, O51C (occupancy 0.20, so that N49B has a total occupancy of 0.60). C52A-O55A (occupancy 0.50) and C52B-O55B (occupancy 0.50). All disordered C-N bonds were restrained to 1.49(2)\%A, N-O bonds to 1.21(2)\%A and O...O distances to 2.10(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except that the torsions of the disordered solvent methyl groups were not refined. ; _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^)+(0.1432P)^2^+2.1941P] 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 0.073(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6902 _refine_ls_number_parameters 526 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0788 _refine_ls_wR_factor_ref 0.2376 _refine_ls_wR_factor_gt 0.2077 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.104 _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 0.57301(3) 0.01808(6) 0.34509(2) 0.0466(3) Uani 1 1 d . . . N2 N 0.45594(18) 0.0150(3) 0.28651(12) 0.0432(6) Uani 1 1 d . . . C3 C 0.4064(2) -0.1122(4) 0.28044(14) 0.0465(8) Uani 1 1 d . . . C4 C 0.3295(2) -0.1130(5) 0.24265(16) 0.0566(9) Uani 1 1 d . . . H4 H 0.2963 -0.2043 0.2385 0.068 Uiso 1 1 calc R . . N5 N 0.3023(2) 0.0148(4) 0.21225(15) 0.0634(9) Uani 1 1 d . . . C6 C 0.3515(2) 0.1434(5) 0.21822(17) 0.0592(10) Uani 1 1 d . . . H6 H 0.3336 0.2343 0.1973 0.071 Uiso 1 1 calc R . . C7 C 0.4291(2) 0.1421(4) 0.25542(14) 0.0469(8) Uani 1 1 d . . . N8 N 0.43996(18) -0.2377(3) 0.31617(13) 0.0488(7) Uani 1 1 d . . . N9 N 0.51709(18) -0.2164(4) 0.35105(12) 0.0516(7) Uani 1 1 d . . . C10 C 0.5288(3) -0.3452(5) 0.38215(18) 0.0646(11) Uani 1 1 d . . . H10 H 0.5767 -0.3647 0.4101 0.078 Uiso 1 1 calc R . . C11 C 0.4610(3) -0.4472(5) 0.3679(2) 0.0739(13) Uani 1 1 d . . . H11 H 0.4550 -0.5447 0.3837 0.089 Uiso 1 1 calc R . . C12 C 0.4051(3) -0.3757(5) 0.3259(2) 0.0657(11) Uani 1 1 d . . . H12 H 0.3528 -0.4144 0.3074 0.079 Uiso 1 1 calc R . . N13 N 0.48561(17) 0.2700(4) 0.26590(12) 0.0487(7) Uani 1 1 d . . . N14 N 0.55682(18) 0.2540(4) 0.30714(12) 0.0515(7) Uani 1 1 d . . . C15 C 0.5987(3) 0.3895(5) 0.30591(18) 0.0612(10) Uani 1 1 d . . . H15 H 0.6502 0.4137 0.3297 0.073 Uiso 1 1 calc R . . C16 C 0.5562(3) 0.4892(5) 0.2650(2) 0.0652(11) Uani 1 1 d . . . H16 H 0.5733 0.5891 0.2563 0.078 Uiso 1 1 calc R . . C17 C 0.4842(3) 0.4123(5) 0.23995(17) 0.0578(9) Uani 1 1 d . . . H17 H 0.4422 0.4496 0.2107 0.069 Uiso 1 1 calc R . . N18 N 0.69207(19) -0.0077(3) 0.40135(13) 0.0476(7) Uani 1 1 d . . . C19 C 0.7051(2) 0.0321(5) 0.45226(15) 0.0535(9) Uani 1 1 d . . . C20 C 0.7824(3) 0.0174(6) 0.48863(19) 0.0734(13) Uani 1 1 d . . . H20 H 0.7903 0.0460 0.5240 0.088 Uiso 1 1 calc R . . N21 N 0.8457(3) -0.0367(6) 0.47397(18) 0.0832(12) Uani 1 1 d . . . C22 C 0.8338(3) -0.0752(6) 0.4229(2) 0.0731(12) Uani 1 1 d . . . H22 H 0.8780 -0.1123 0.4120 0.088 Uiso 1 1 calc R . . C23 C 0.7559(2) -0.0603(5) 0.38608(16) 0.0538(9) Uani 1 1 d . . . N24 N 0.6339(2) 0.0883(4) 0.46284(12) 0.0550(8) Uani 1 1 d . . . N25 N 0.56224(19) 0.0999(4) 0.42162(13) 0.0540(8) Uani 1 1 d . . . C26 C 0.5073(3) 0.1610(5) 0.44312(18) 0.0623(10) Uani 1 1 d . . . H26 H 0.4522 0.1819 0.4245 0.075 Uiso 1 1 calc R . . C27 C 0.5428(3) 0.1896(6) 0.4970(2) 0.0769(13) Uani 1 1 d . . . H27 H 0.5168 0.2327 0.5204 0.092 Uiso 1 1 calc R . . C28 C 0.6227(3) 0.1425(6) 0.50877(17) 0.0710(12) Uani 1 1 d . . . H28 H 0.6624 0.1466 0.5420 0.085 Uiso 1 1 calc R . . N29 N 0.73608(19) -0.0923(4) 0.33202(13) 0.0561(8) Uani 1 1 d . . . N30 N 0.65694(19) -0.0597(4) 0.30090(13) 0.0534(7) Uani 1 1 d . . . C31 C 0.6561(3) -0.0954(6) 0.25178(18) 0.0683(11) Uani 1 1 d . . . H31 H 0.6105 -0.0823 0.2218 0.082 Uiso 1 1 calc R . . C32 C 0.7325(3) -0.1552(7) 0.2509(2) 0.0803(14) Uani 1 1 d . . . H32 H 0.7467 -0.1908 0.2212 0.096 Uiso 1 1 calc R . . C33 C 0.7818(3) -0.1510(6) 0.3018(2) 0.0769(13) Uani 1 1 d . . . H33 H 0.8371 -0.1825 0.3139 0.092 Uiso 1 1 calc R . . B34A B 0.2269(11) 0.533(2) 0.1423(7) 0.07(2) Uiso 0.33 1 d PD A 1 F35A F 0.2254(5) 0.6034(11) 0.0931(3) 0.063(2) Uiso 0.33 1 d PD A 1 F36A F 0.3048(7) 0.5476(15) 0.1781(5) 0.091(5) Uiso 0.33 1 d PD A 1 F37A F 0.1682(6) 0.6230(14) 0.1586(5) 0.074(3) Uiso 0.33 1 d PD A 1 F38A F 0.2066(7) 0.3747(12) 0.1332(5) 0.074(4) Uiso 0.33 1 d PD A 1 B34B B 0.2221(9) 0.5548(18) 0.1478(6) 0.052(6) Uiso 0.33 1 d PD B 2 F35B F 0.2565(8) 0.6065(15) 0.1087(4) 0.075(3) Uiso 0.33 1 d PD B 2 F36B F 0.2843(7) 0.5135(15) 0.1947(5) 0.082(5) Uiso 0.33 1 d PD B 2 F37B F 0.1780(6) 0.6793(13) 0.1616(5) 0.066(3) Uiso 0.33 1 d PD B 2 F38B F 0.1682(5) 0.4253(11) 0.1318(4) 0.070(3) Uiso 0.33 1 d PD B 2 B34C B 0.2303(11) 0.533(2) 0.1457(7) 0.060(18) Uiso 0.33 1 d PD C 3 F35C F 0.2560(8) 0.5627(14) 0.1014(5) 0.072(3) Uiso 0.33 1 d PD C 3 F36C F 0.2966(8) 0.5364(17) 0.1914(5) 0.063(4) Uiso 0.33 1 d PD C 3 F37C F 0.1735(9) 0.655(2) 0.1492(6) 0.096(6) Uiso 0.33 1 d PD C 3 F38C F 0.1931(8) 0.3856(12) 0.1412(4) 0.059(3) Uiso 0.33 1 d PD C 3 B39A B 0.4639(8) 0.1967(16) 0.1052(6) 0.050(4) Uiso 0.33 1 d PD D 1 F40A F 0.3990(6) 0.2847(14) 0.1135(6) 0.083(3) Uiso 0.33 1 d PD D 1 F41A F 0.4370(9) 0.0369(14) 0.0945(6) 0.123(6) Uiso 0.33 1 d PD D 1 F42A F 0.4869(6) 0.2527(12) 0.0618(4) 0.087(3) Uiso 0.33 1 d PD D 1 F43A F 0.5338(6) 0.2051(18) 0.1498(5) 0.113(4) Uiso 0.33 1 d PD D 1 B39B B 0.4693(6) 0.1737(13) 0.1162(4) 0.091(4) Uiso 0.67 1 d PD . . F40B F 0.3868(7) 0.2433(18) 0.0948(6) 0.115(4) Uiso 0.33 1 d PD E 2 F41B F 0.4792(11) 0.099(2) 0.0725(6) 0.184(8) Uiso 0.33 1 d PD E 2 F42B F 0.5230(6) 0.3062(14) 0.1315(5) 0.110(3) Uiso 0.33 1 d PD E 2 F43B F 0.4730(11) 0.0803(19) 0.1585(6) 0.153(5) Uiso 0.33 1 d PD E 2 F40C F 0.3982(7) 0.2321(16) 0.1217(5) 0.096(4) Uiso 0.33 1 d PD E 3 F41C F 0.4543(8) 0.0348(11) 0.0841(4) 0.077(3) Uiso 0.33 1 d PD E 3 F42C F 0.5100(8) 0.2797(15) 0.0910(7) 0.128(4) Uiso 0.33 1 d PD E 3 F43C F 0.5194(8) 0.1372(17) 0.1661(4) 0.115(4) Uiso 0.33 1 d PD E 3 C44A C 0.4318(7) 0.6659(13) 0.0941(5) 0.080(3) Uiso 0.50 1 d PD F 1 H44A H 0.4257 0.7471 0.0672 0.120 Uiso 0.50 1 calc PR F 1 H44B H 0.3808 0.6555 0.1028 0.120 Uiso 0.50 1 calc PR F 1 H44C H 0.4452 0.5649 0.0810 0.120 Uiso 0.50 1 calc PR F 1 N45A N 0.4967(5) 0.7110(11) 0.1407(4) 0.064(2) Uiso 0.50 1 d PD F 1 O46A O 0.5709(6) 0.6867(13) 0.1500(4) 0.099(3) Uiso 0.50 1 d PD F 1 O47A O 0.4681(6) 0.7563(12) 0.1759(4) 0.089(3) Uiso 0.50 1 d PD F 1 C44B C 0.4600(8) 0.6623(16) 0.0809(5) 0.096(4) Uiso 0.50 1 d PD G 2 H44D H 0.4892 0.6635 0.0548 0.144 Uiso 0.50 1 calc PR G 2 H44E H 0.4174 0.7430 0.0723 0.144 Uiso 0.50 1 calc PR G 2 H44F H 0.4354 0.5583 0.0813 0.144 Uiso 0.50 1 calc PR G 2 N45B N 0.5184(11) 0.696(3) 0.1339(7) 0.149(7) Uiso 0.50 1 d PD G 2 O46B O 0.5837(8) 0.7174(17) 0.1346(6) 0.135(5) Uiso 0.50 1 d PD G 2 O47B O 0.4881(10) 0.722(2) 0.1706(7) 0.152(6) Uiso 0.50 1 d PD G 2 C48A C 0.2535(12) 0.967(3) 0.0752(7) 0.084(5) Uiso 0.40 1 d PD H 1 H48A H 0.2720 1.0765 0.0767 0.125 Uiso 0.40 1 calc PR H 1 H48B H 0.2985 0.8960 0.0755 0.125 Uiso 0.40 1 calc PR H 1 H48C H 0.2347 0.9446 0.1054 0.125 Uiso 0.40 1 calc PR H 1 N49A N 0.1846(10) 0.941(2) 0.0256(7) 0.112(7) Uiso 0.40 1 d PD H 1 O50A O 0.1145(7) 0.9231(16) 0.0227(5) 0.088(3) Uiso 0.40 1 d PD H 1 O51A O 0.2154(10) 0.867(3) -0.0053(7) 0.135(6) Uiso 0.40 1 d PD H 1 C48B C 0.2310(10) 0.993(2) 0.0815(6) 0.067(4) Uiso 0.40 1 d PD I 2 H48D H 0.1971 1.0860 0.0805 0.101 Uiso 0.40 1 calc PR I 2 H48E H 0.2867 1.0256 0.0849 0.101 Uiso 0.40 1 calc PR I 2 H48F H 0.2306 0.9265 0.1114 0.101 Uiso 0.40 1 calc PR I 2 N49B N 0.1976(6) 0.8989(12) 0.0313(3) 0.076(3) Uiso 0.60 1 d PD . . O50B O 0.1274(8) 0.862(2) 0.0222(6) 0.102(4) Uiso 0.40 1 d PD I 2 O51B O 0.2399(9) 0.8319(19) 0.0062(6) 0.113(5) Uiso 0.40 1 d PD I 2 C48C C 0.245(2) 0.940(4) 0.0880(9) 0.068(8) Uiso 0.20 1 d PD I 3 H48G H 0.2463 1.0549 0.0924 0.102 Uiso 0.20 1 calc PR I 3 H48H H 0.3000 0.8988 0.0962 0.102 Uiso 0.20 1 calc PR I 3 H48I H 0.2172 0.8927 0.1115 0.102 Uiso 0.20 1 calc PR I 3 O50C O 0.2131(19) 0.994(3) -0.0038(11) 0.135(10) Uiso 0.20 1 d PD I 3 O51C O 0.153(2) 0.791(4) 0.0107(14) 0.177(14) Uiso 0.20 1 d PD I 3 C52A C 0.6230(9) 0.9911(18) 0.0389(6) 0.097(4) Uiso 0.50 1 d PD J 1 H52A H 0.5689 0.9769 0.0430 0.146 Uiso 0.50 1 calc PR J 1 H52B H 0.6273 0.9287 0.0091 0.146 Uiso 0.50 1 calc PR J 1 H52C H 0.6315 1.1029 0.0328 0.146 Uiso 0.50 1 calc PR J 1 N53A N 0.6870(5) 0.9367(10) 0.0881(4) 0.068(2) Uiso 0.50 1 d PD J 1 O54A O 0.7250(5) 0.8128(10) 0.0979(4) 0.099(2) Uiso 0.50 1 d PD J 1 O55A O 0.7060(6) 1.0420(10) 0.1194(4) 0.095(2) Uiso 0.50 1 d PD J 1 C52B C 0.6165(7) 0.9337(19) 0.0434(6) 0.092(4) Uiso 0.50 1 d PD K 2 H52D H 0.5813 1.0167 0.0500 0.137 Uiso 0.50 1 calc PR K 2 H52E H 0.5996 0.8313 0.0536 0.137 Uiso 0.50 1 calc PR K 2 H52F H 0.6123 0.9318 0.0063 0.137 Uiso 0.50 1 calc PR K 2 N53B N 0.7062(6) 0.9672(12) 0.0761(4) 0.083(3) Uiso 0.50 1 d PD K 2 O54B O 0.7515(7) 0.8598(12) 0.0697(4) 0.128(3) Uiso 0.50 1 d PD K 2 O55B O 0.7337(6) 1.0715(11) 0.1071(4) 0.095(2) Uiso 0.50 1 d PD K 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 0.0390(3) 0.0533(4) 0.0421(4) 0.0003(2) 0.0039(2) 0.00371(19) N2 0.0376(14) 0.0469(15) 0.0432(16) 0.0009(12) 0.0091(12) 0.0014(11) C3 0.0432(17) 0.0489(18) 0.0476(19) -0.0027(15) 0.0138(15) -0.0034(14) C4 0.0484(19) 0.057(2) 0.058(2) -0.0041(18) 0.0068(17) -0.0073(17) N5 0.0485(18) 0.074(2) 0.056(2) 0.0042(16) -0.0013(16) -0.0047(15) C6 0.051(2) 0.060(2) 0.056(2) 0.0106(18) 0.0006(17) 0.0026(17) C7 0.0453(18) 0.0493(18) 0.0436(19) 0.0016(15) 0.0096(15) 0.0005(14) N8 0.0464(15) 0.0436(15) 0.0572(18) 0.0023(13) 0.0167(14) 0.0021(12) N9 0.0531(17) 0.0490(16) 0.0500(17) 0.0023(14) 0.0115(14) 0.0072(13) C10 0.074(3) 0.060(2) 0.061(2) 0.012(2) 0.022(2) 0.017(2) C11 0.085(3) 0.057(2) 0.092(4) 0.022(2) 0.045(3) 0.012(2) C12 0.062(2) 0.050(2) 0.092(3) 0.006(2) 0.034(2) -0.0013(18) N13 0.0463(15) 0.0513(16) 0.0458(16) 0.0037(13) 0.0096(13) -0.0018(12) N14 0.0451(15) 0.0540(17) 0.0501(17) -0.0028(14) 0.0061(13) -0.0027(13) C15 0.055(2) 0.061(2) 0.068(3) -0.011(2) 0.0193(19) -0.0144(18) C16 0.076(3) 0.053(2) 0.072(3) 0.0034(19) 0.031(2) -0.0093(19) C17 0.064(2) 0.052(2) 0.056(2) 0.0090(18) 0.0166(18) -0.0008(18) N18 0.0433(15) 0.0513(16) 0.0438(17) 0.0022(12) 0.0061(13) 0.0046(12) C19 0.054(2) 0.058(2) 0.041(2) 0.0044(16) 0.0031(16) 0.0022(16) C20 0.067(3) 0.095(3) 0.046(2) -0.001(2) -0.003(2) 0.007(2) N21 0.056(2) 0.116(3) 0.064(3) 0.009(2) -0.0035(19) 0.019(2) C22 0.048(2) 0.091(3) 0.073(3) 0.003(3) 0.007(2) 0.012(2) C23 0.0472(19) 0.056(2) 0.055(2) 0.0050(18) 0.0106(16) 0.0056(16) N24 0.0634(19) 0.0579(18) 0.0406(16) 0.0008(14) 0.0106(14) 0.0055(15) N25 0.0547(17) 0.0570(18) 0.0476(18) 0.0041(14) 0.0112(14) 0.0077(14) C26 0.068(2) 0.058(2) 0.067(3) 0.006(2) 0.029(2) 0.0102(18) C27 0.098(4) 0.074(3) 0.068(3) -0.004(2) 0.040(3) 0.015(3) C28 0.092(3) 0.076(3) 0.046(2) -0.004(2) 0.021(2) 0.002(2) N29 0.0463(16) 0.0655(19) 0.0563(19) -0.0008(15) 0.0151(14) 0.0067(14) N30 0.0492(17) 0.0614(18) 0.0462(17) -0.0045(15) 0.0091(13) 0.0021(14) C31 0.070(3) 0.083(3) 0.053(2) -0.010(2) 0.019(2) -0.007(2) C32 0.076(3) 0.105(4) 0.069(3) -0.017(3) 0.036(3) -0.003(3) C33 0.062(3) 0.091(3) 0.087(4) -0.002(3) 0.037(2) 0.012(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 2.114(3) . ? Fe1 N18 2.123(3) . ? Fe1 N14 2.179(3) . ? Fe1 N25 2.184(3) . ? Fe1 N30 2.185(3) . ? Fe1 N9 2.191(3) . ? N2 C3 1.327(4) . ? N2 C7 1.329(4) . ? C3 C4 1.381(5) . ? C3 N8 1.404(5) . ? C4 N5 1.325(5) . ? N5 C6 1.334(5) . ? C6 C7 1.381(5) . ? C7 N13 1.401(4) . ? N8 C12 1.348(5) . ? N8 N9 1.363(4) . ? N9 C10 1.325(5) . ? C10 C11 1.384(7) . ? C11 C12 1.356(7) . ? N13 C17 1.362(5) . ? N13 N14 1.365(4) . ? N14 C15 1.335(5) . ? C15 C16 1.377(7) . ? C16 C17 1.357(6) . ? N18 C19 1.332(5) . ? N18 C23 1.333(5) . ? C19 C20 1.375(6) . ? C19 N24 1.396(5) . ? C20 N21 1.320(7) . ? N21 C22 1.336(7) . ? C22 C23 1.387(6) . ? C23 N29 1.386(5) . ? N24 C28 1.355(5) . ? N24 N25 1.366(4) . ? N25 C26 1.325(5) . ? C26 C27 1.384(7) . ? C27 C28 1.351(7) . ? N29 C33 1.356(5) . ? N29 N30 1.371(4) . ? N30 C31 1.322(5) . ? C31 C32 1.392(6) . ? C32 C33 1.349(7) . ? B34A F38A 1.364(16) . ? B34A F36A 1.377(17) . ? B34A F37A 1.408(16) . ? B34A F35A 1.412(17) . ? B34B F37B 1.386(16) . ? B34B F38B 1.392(14) . ? B34B F35B 1.393(14) . ? B34B F36B 1.402(15) . ? B34C F38C 1.365(15) . ? B34C F36C 1.377(17) . ? B34C F35C 1.383(16) . ? B34C F37C 1.419(16) . ? B39A F40A 1.389(13) . ? B39A F42A 1.392(14) . ? B39A F43A 1.397(14) . ? B39A F41A 1.403(14) . ? B39B F43B 1.344(13) . ? B39B F40C 1.345(12) . ? B39B F41B 1.359(13) . ? B39B F43C 1.366(13) . ? B39B F42C 1.399(13) . ? B39B F42B 1.407(12) . ? B39B F41C 1.408(12) . ? B39B F40B 1.459(13) . ? C44A N45A 1.429(11) . ? N45A O46A 1.222(13) . ? N45A O47A 1.224(13) . ? C44B N45B 1.474(15) . ? N45B O46B 1.113(15) . ? N45B O47B 1.239(15) . ? C48A N49A 1.481(16) . ? N49A O50A 1.175(14) . ? N49A O51A 1.253(15) . ? N49B O50B 1.179(12) . ? N49B O51C 1.193(18) . ? N49B O51B 1.241(12) . ? N49B O50C 1.301(17) . ? N49B C48B 1.491(13) . ? N49B C48C 1.505(18) . ? C52A N53A 1.487(14) . ? N53A O55A 1.178(10) . ? N53A O54A 1.200(10) . ? C52B N53B 1.528(13) . ? N53B O55B 1.186(10) . ? N53B O54B 1.220(11) . ? 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 173.18(11) . . ? N2 Fe1 N14 73.45(11) . . ? N18 Fe1 N14 111.91(11) . . ? N2 Fe1 N25 110.94(11) . . ? N18 Fe1 N25 73.27(12) . . ? N14 Fe1 N25 96.25(12) . . ? N2 Fe1 N30 102.97(11) . . ? N18 Fe1 N30 73.11(12) . . ? N14 Fe1 N30 91.98(12) . . ? N25 Fe1 N30 146.07(12) . . ? N2 Fe1 N9 73.21(11) . . ? N18 Fe1 N9 101.54(11) . . ? N14 Fe1 N9 146.55(11) . . ? N25 Fe1 N9 93.07(12) . . ? N30 Fe1 N9 97.97(12) . . ? C3 N2 C7 118.1(3) . . ? C3 N2 Fe1 121.1(2) . . ? C7 N2 Fe1 120.8(2) . . ? N2 C3 C4 121.0(3) . . ? N2 C3 N8 113.3(3) . . ? C4 C3 N8 125.7(3) . . ? N5 C4 C3 120.8(3) . . ? C4 N5 C6 118.6(3) . . ? N5 C6 C7 120.2(4) . . ? N2 C7 C6 121.3(3) . . ? N2 C7 N13 113.2(3) . . ? C6 C7 N13 125.5(3) . . ? C12 N8 N9 111.5(3) . . ? C12 N8 C3 130.3(3) . . ? N9 N8 C3 117.9(3) . . ? C10 N9 N8 104.3(3) . . ? C10 N9 Fe1 140.7(3) . . ? N8 N9 Fe1 114.4(2) . . ? N9 C10 C11 111.5(4) . . ? C12 C11 C10 105.8(4) . . ? N8 C12 C11 106.8(4) . . ? C17 N13 N14 111.2(3) . . ? C17 N13 C7 130.6(3) . . ? N14 N13 C7 118.1(3) . . ? C15 N14 N13 104.3(3) . . ? C15 N14 Fe1 140.7(3) . . ? N13 N14 Fe1 114.3(2) . . ? N14 C15 C16 111.6(4) . . ? C17 C16 C15 106.2(4) . . ? C16 C17 N13 106.6(4) . . ? C19 N18 C23 118.6(3) . . ? C19 N18 Fe1 120.9(3) . . ? C23 N18 Fe1 120.5(3) . . ? N18 C19 C20 121.0(4) . . ? N18 C19 N24 113.0(3) . . ? C20 C19 N24 126.1(4) . . ? N21 C20 C19 120.8(4) . . ? C20 N21 C22 118.9(4) . . ? N21 C22 C23 120.5(4) . . ? N18 C23 N29 113.8(3) . . ? N18 C23 C22 120.3(4) . . ? N29 C23 C22 126.0(4) . . ? C28 N24 N25 110.9(3) . . ? C28 N24 C19 130.4(4) . . ? N25 N24 C19 118.6(3) . . ? C26 N25 N24 104.9(3) . . ? C26 N25 Fe1 140.9(3) . . ? N24 N25 Fe1 114.3(2) . . ? N25 C26 C27 111.0(4) . . ? C28 C27 C26 106.5(4) . . ? C27 C28 N24 106.7(4) . . ? C33 N29 N30 110.3(4) . . ? C33 N29 C23 131.8(4) . . ? N30 N29 C23 117.9(3) . . ? C31 N30 N29 105.2(3) . . ? C31 N30 Fe1 140.2(3) . . ? N29 N30 Fe1 114.5(2) . . ? N30 C31 C32 111.0(4) . . ? C33 C32 C31 105.9(4) . . ? C32 C33 N29 107.5(4) . . ? F38A B34A F36A 110.0(13) . . ? F38A B34A F37A 113.7(13) . . ? F36A B34A F37A 111.3(13) . . ? F38A B34A F35A 107.6(13) . . ? F36A B34A F35A 110.0(13) . . ? F37A B34A F35A 104.0(12) . . ? F37B B34B F38B 107.5(12) . . ? F37B B34B F35B 109.9(12) . . ? F38B B34B F35B 113.3(12) . . ? F37B B34B F36B 105.8(12) . . ? F38B B34B F36B 109.2(12) . . ? F35B B34B F36B 110.9(12) . . ? F38C B34C F36C 109.2(14) . . ? F38C B34C F35C 109.8(13) . . ? F36C B34C F35C 110.8(14) . . ? F38C B34C F37C 110.1(14) . . ? F36C B34C F37C 108.6(13) . . ? F35C B34C F37C 108.4(13) . . ? F40A B39A F42A 112.4(12) . . ? F40A B39A F43A 110.6(11) . . ? F42A B39A F43A 107.4(10) . . ? F40A B39A F41A 107.8(11) . . ? F42A B39A F41A 107.8(11) . . ? F43A B39A F41A 110.9(12) . . ? F43B B39B F41B 116.9(12) . . ? F40C B39B F43C 107.0(10) . . ? F40C B39B F42C 114.0(11) . . ? F43C B39B F42C 110.0(10) . . ? F43B B39B F42B 110.4(11) . . ? F41B B39B F42B 111.4(11) . . ? F40C B39B F41C 110.7(10) . . ? F43C B39B F41C 110.1(10) . . ? F42C B39B F41C 104.9(10) . . ? F43B B39B F40B 110.4(10) . . ? F41B B39B F40B 101.6(11) . . ? F42B B39B F40B 105.2(10) . . ? O46A N45A O47A 121.0(10) . . ? O46A N45A C44A 127.3(10) . . ? O47A N45A C44A 110.7(9) . . ? O46B N45B O47B 126.8(18) . . ? O46B N45B C44B 115.2(17) . . ? O47B N45B C44B 117.0(17) . . ? O50A N49A O51A 120.1(17) . . ? O50A N49A C48A 126.0(17) . . ? O51A N49A C48A 105.7(17) . . ? O50B N49B O51B 118.7(12) . . ? O51C N49B O50C 111.7(18) . . ? O50B N49B C48B 114.0(12) . . ? O51B N49B C48B 125.4(12) . . ? O51C N49B C48C 134(2) . . ? O50C N49B C48C 114(2) . . ? O55A N53A O54A 118.0(9) . . ? O55A N53A C52A 111.0(10) . . ? O54A N53A C52A 130.7(10) . . ? O55B N53B O54B 119.7(10) . . ? O55B N53B C52B 129.7(10) . . ? O54B N53B C52B 110.4(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.788 _refine_diff_density_min -0.803 _refine_diff_density_rms 0.207 #=END data_je10lt _database_code_CSD 195909 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(pyrazol-1-yl)pyrazine]iron(II) ditetrafluoroborate tris-nitromethane solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H16 Fe N12, 2[B F4], 3[C H3 N O2]' _chemical_formula_sum 'C23 H25 B2 F8 Fe N15 O6' _chemical_formula_weight 837.05 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 Monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.5404(2) _cell_length_b 8.2833(1) _cell_length_c 25.8237(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.2104(6) _cell_angle_gamma 90.00 _cell_volume 3360.89(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 23212 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.50 _exptl_crystal_description 'Rectangular prism' _exptl_crystal_colour Brown _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7875 _exptl_absorpt_correction_T_max 0.8732 _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 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 23212 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0439 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7664 _reflns_number_gt 6066 _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 of the structure contains one complex dication, two BF~4~^-^ anions and three molecules of nitromethane. Both of the BF~4~^-^ anions are disordered over three orientations: B34A-F38A (occupancy 0.33) B34B-F38B (occupancy 0.33) B34C-F38C (occupancy 0.33) and B39A-F43A (occupancy 0.50) B39B-F43B (occupancy 0.10) B39B, F40C-F43C (occupancy 0.40, so that B39B has total occupancy 0.50). All B-F distances were restrained to 1.39(2)\%A, and F...F distances within a given disorder orientation to 2.27(2)\%A. All three nitromethane molecules are also disordered: C44A-O47A (occupancy 0.50) C44B-O47B (occupancy 0.20) C44B, N44B, O45C, O46C (occupancy 0.40, so that C44B and N44B have total occupancy 0.60). C48A-O51A (occupancy 0.40) C48B-O51B (occupancy 0.40) C48C, N49B, O50C, O51C (occupancy 0.20, so that N49B has a total occupancy of 0.60). C52A-O55A (occupancy 0.40) C52B-O55B (occupancy 0.35) C52B, N53B, O54C, O55C (occupancy 0.25, so that C52B and N53B have total occupancy 0.60). All disordered C-N bonds were restrained to 1.47(2)\%A, N-O bonds to 1.22(2)\%A and O...O distances to 2.11(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except that the torsions of the disordered solvent methyl groups were not refined. ; _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^)+(0.1119P)^2^+4.2499P] 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 0.0115(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7664 _refine_ls_number_parameters 542 _refine_ls_number_restraints 94 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1958 _refine_ls_wR_factor_gt 0.1789 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.003 _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 0.57152(3) 0.00789(5) 0.347666(16) 0.02537(17) Uani 1 1 d . . . N2 N 0.46101(16) 0.0184(3) 0.29627(10) 0.0251(5) Uani 1 1 d . . . C3 C 0.40863(18) -0.1079(3) 0.28891(12) 0.0269(6) Uani 1 1 d . . . C4 C 0.3292(2) -0.1043(4) 0.24988(13) 0.0314(6) Uani 1 1 d . . . H4 H 0.2931 -0.1960 0.2445 0.038 Uiso 1 1 calc R . . N5 N 0.30331(17) 0.0285(3) 0.21979(11) 0.0332(6) Uani 1 1 d . . . C6 C 0.3556(2) 0.1560(4) 0.22692(13) 0.0319(6) Uani 1 1 d . . . H6 H 0.3378 0.2507 0.2057 0.038 Uiso 1 1 calc R . . C7 C 0.43570(18) 0.1494(3) 0.26543(12) 0.0269(6) Uani 1 1 d . . . N8 N 0.44549(16) -0.2335(3) 0.32453(10) 0.0284(5) Uani 1 1 d . . . N9 N 0.52791(16) -0.2087(3) 0.35798(10) 0.0282(5) Uani 1 1 d . . . C10 C 0.5464(2) -0.3365(4) 0.39009(13) 0.0326(7) Uani 1 1 d . . . H10 H 0.5996 -0.3543 0.4172 0.039 Uiso 1 1 calc R . . C11 C 0.4770(2) -0.4425(4) 0.37886(14) 0.0378(7) Uani 1 1 d . . . H11 H 0.4745 -0.5417 0.3967 0.045 Uiso 1 1 calc R . . C12 C 0.4137(2) -0.3746(4) 0.33706(14) 0.0350(7) Uani 1 1 d . . . H12 H 0.3584 -0.4174 0.3201 0.042 Uiso 1 1 calc R . . N13 N 0.49930(16) 0.2667(3) 0.27787(10) 0.0280(5) Uani 1 1 d . . . N14 N 0.57333(16) 0.2288(3) 0.31867(10) 0.0283(5) Uani 1 1 d . . . C15 C 0.6247(2) 0.3527(4) 0.32068(13) 0.0346(7) Uani 1 1 d . . . H15 H 0.6808 0.3612 0.3453 0.042 Uiso 1 1 calc R . . C16 C 0.5854(2) 0.4698(4) 0.28175(14) 0.0383(7) Uani 1 1 d . . . H16 H 0.6092 0.5693 0.2754 0.046 Uiso 1 1 calc R . . C17 C 0.5064(2) 0.4121(4) 0.25494(14) 0.0344(7) Uani 1 1 d . . . H17 H 0.4643 0.4632 0.2258 0.041 Uiso 1 1 calc R . . N18 N 0.68264(17) -0.0112(3) 0.39737(11) 0.0304(6) Uani 1 1 d . . . C19 C 0.6994(2) 0.0283(4) 0.44996(13) 0.0331(7) Uani 1 1 d . . . C20 C 0.7807(2) 0.0113(5) 0.48622(16) 0.0451(9) Uani 1 1 d . . . H20 H 0.7919 0.0420 0.5232 0.054 Uiso 1 1 calc R . . N21 N 0.8434(2) -0.0479(5) 0.46948(14) 0.0497(8) Uani 1 1 d . . . C22 C 0.8270(2) -0.0893(5) 0.41738(16) 0.0466(9) Uani 1 1 d . . . H22 H 0.8710 -0.1325 0.4051 0.056 Uiso 1 1 calc R . . C23 C 0.7460(2) -0.0695(4) 0.38091(14) 0.0361(7) Uani 1 1 d . . . N24 N 0.62622(17) 0.0847(3) 0.46002(10) 0.0329(6) Uani 1 1 d . . . N25 N 0.55244(16) 0.0887(3) 0.41583(10) 0.0296(5) Uani 1 1 d . . . C26 C 0.4941(2) 0.1520(4) 0.43483(13) 0.0330(7) Uani 1 1 d . . . H26 H 0.4364 0.1690 0.4139 0.040 Uiso 1 1 calc R . . C27 C 0.5293(2) 0.1907(4) 0.49047(14) 0.0411(8) Uani 1 1 d . . . H27 H 0.5006 0.2385 0.5132 0.049 Uiso 1 1 calc R . . C28 C 0.6124(2) 0.1462(4) 0.50508(14) 0.0401(8) Uani 1 1 d . . . H28 H 0.6532 0.1562 0.5402 0.048 Uiso 1 1 calc R . . N29 N 0.71803(17) -0.1024(4) 0.32523(12) 0.0371(6) Uani 1 1 d . . . N30 N 0.63329(16) -0.0709(3) 0.29828(11) 0.0309(5) Uani 1 1 d . . . C31 C 0.6242(2) -0.0962(4) 0.24615(14) 0.0368(7) Uani 1 1 d . . . H31 H 0.5722 -0.0841 0.2174 0.044 Uiso 1 1 calc R . . C32 C 0.7011(2) -0.1428(5) 0.23900(16) 0.0491(9) Uani 1 1 d . . . H32 H 0.7106 -0.1673 0.2054 0.059 Uiso 1 1 calc R . . C33 C 0.7596(2) -0.1463(5) 0.28943(17) 0.0479(9) Uani 1 1 d . . . H33 H 0.8181 -0.1739 0.2980 0.057 Uiso 1 1 calc R . . B34A B 0.2434(11) 0.543(2) 0.1462(7) 0.04(2) Uiso 0.33 1 d PD A 1 F35A F 0.2458(5) 0.5986(11) 0.0956(3) 0.0343(18) Uiso 0.33 1 d PD A 1 F36A F 0.3234(5) 0.5522(12) 0.1847(3) 0.039(2) Uiso 0.33 1 d PD A 1 F37A F 0.1819(6) 0.6398(13) 0.1578(6) 0.041(4) Uiso 0.33 1 d PD A 1 F38A F 0.2119(8) 0.3836(10) 0.1414(4) 0.033(2) Uiso 0.33 1 d PD A 1 B34B B 0.2480(10) 0.557(2) 0.1493(6) 0.039(9) Uiso 0.33 1 d PD B 2 F35B F 0.2760(7) 0.6185(12) 0.1079(4) 0.050(2) Uiso 0.33 1 d PD B 2 F36B F 0.3152(7) 0.5458(15) 0.1982(4) 0.037(3) Uiso 0.33 1 d PD B 2 F37B F 0.1888(8) 0.6603(18) 0.1620(5) 0.030(3) Uiso 0.33 1 d PD B 2 F38B F 0.2139(10) 0.4025(14) 0.1340(5) 0.053(4) Uiso 0.33 1 d PD B 2 B34C B 0.2410(11) 0.543(2) 0.1468(7) 0.03(2) Uiso 0.33 1 d PD C 3 F35C F 0.2674(7) 0.5733(11) 0.1013(4) 0.040(2) Uiso 0.33 1 d PD C 3 F36C F 0.3117(6) 0.5208(12) 0.1926(5) 0.036(3) Uiso 0.33 1 d PD C 3 F37C F 0.1935(7) 0.6743(13) 0.1548(5) 0.044(4) Uiso 0.33 1 d PD C 3 F38C F 0.1916(6) 0.4024(11) 0.1371(4) 0.040(2) Uiso 0.33 1 d PD C 3 B39A B 0.4833(9) 0.1672(17) 0.1260(6) 0.057(8) Uiso 0.50 1 d PD D 1 F40A F 0.4170(4) 0.2537(8) 0.1339(3) 0.0639(19) Uiso 0.50 1 d PD D 1 F41A F 0.4641(6) 0.0076(9) 0.1302(4) 0.106(3) Uiso 0.50 1 d PD D 1 F42A F 0.4990(7) 0.2022(13) 0.0788(4) 0.121(4) Uiso 0.50 1 d PD D 1 F43A F 0.5602(5) 0.2022(10) 0.1651(3) 0.070(2) Uiso 0.50 1 d PD D 1 B39B B 0.4808(7) 0.1729(13) 0.1203(5) 0.039(5) Uiso 0.50 1 d PD . . F40B F 0.4152(13) 0.236(3) 0.0818(9) 0.076(8) Uiso 0.10 1 d PD E 2 F41B F 0.5113(16) 0.027(2) 0.1011(9) 0.059(6) Uiso 0.10 1 d PD E 2 F42B F 0.5474(10) 0.271(2) 0.1467(7) 0.036(4) Uiso 0.10 1 d PD E 2 F43B F 0.4522(14) 0.102(3) 0.1631(8) 0.065(7) Uiso 0.10 1 d PD E 2 F40C F 0.4015(5) 0.2431(10) 0.1164(4) 0.066(2) Uiso 0.40 1 d PD E 3 F41C F 0.4736(5) 0.0111(7) 0.1074(3) 0.0495(14) Uiso 0.40 1 d PD E 3 F42C F 0.4948(4) 0.2527(8) 0.0747(2) 0.0414(14) Uiso 0.40 1 d PD E 3 F43C F 0.5401(6) 0.2115(12) 0.1706(3) 0.071(3) Uiso 0.40 1 d PD E 3 C44A C 0.4490(7) 0.6395(13) 0.0921(4) 0.048(2) Uiso 0.40 1 d PD F 1 H44A H 0.4517 0.7342 0.0699 0.072 Uiso 0.40 1 calc PR F 1 H44B H 0.3906 0.6252 0.0928 0.072 Uiso 0.40 1 calc PR F 1 H44C H 0.4666 0.5433 0.0763 0.072 Uiso 0.40 1 calc PR F 1 N45A N 0.5022(7) 0.6617(14) 0.1440(5) 0.074(3) Uiso 0.40 1 d PD F 1 O46A O 0.5732(6) 0.6008(10) 0.1631(3) 0.0382(16) Uiso 0.40 1 d PD F 1 O47A O 0.4628(6) 0.7123(13) 0.1719(4) 0.085(3) Uiso 0.40 1 d PD F 1 C44B C 0.4750(6) 0.6396(12) 0.0793(4) 0.070(2) Uiso 0.60 1 d PD G . H44D H 0.4852 0.6333 0.0439 0.105 Uiso 0.60 1 calc PR . . H44E H 0.4373 0.7309 0.0792 0.105 Uiso 0.60 1 calc PR . . H44F H 0.4482 0.5393 0.0858 0.105 Uiso 0.60 1 calc PR . . N45B N 0.5559(4) 0.6622(8) 0.1224(3) 0.0531(14) Uiso 0.60 1 d PD . . O46B O 0.583(2) 0.731(5) 0.0900(12) 0.165(15) Uiso 0.20 1 d PD G 2 O47B O 0.6003(16) 0.594(3) 0.1600(8) 0.087(9) Uiso 0.20 1 d PD G 2 O46C O 0.6164(5) 0.7237(10) 0.1139(4) 0.060(2) Uiso 0.40 1 d PD G 3 O47C O 0.5515(12) 0.637(2) 0.1677(6) 0.132(7) Uiso 0.40 1 d PD G 3 C48A C 0.2648(10) 0.987(2) 0.0835(5) 0.045(3) Uiso 0.40 1 d PD H 1 H48A H 0.2794 1.1009 0.0810 0.067 Uiso 0.40 1 calc PR H 1 H48B H 0.3151 0.9200 0.0872 0.067 Uiso 0.40 1 calc PR H 1 H48C H 0.2454 0.9714 0.1153 0.067 Uiso 0.40 1 calc PR H 1 N49A N 0.1972(7) 0.9409(16) 0.0343(5) 0.059(3) Uiso 0.40 1 d PD H 1 O50A O 0.1223(6) 0.9420(13) 0.0262(5) 0.054(3) Uiso 0.40 1 d PD H 1 O51A O 0.2203(8) 0.8288(17) 0.0053(6) 0.071(5) Uiso 0.40 1 d PD H 1 N49B N 0.2032(4) 0.8944(8) 0.0381(2) 0.0377(15) Uiso 0.60 1 d PD . . C48B C 0.2444(8) 0.9905(18) 0.0894(5) 0.044(3) Uiso 0.40 1 d PD I 2 H48D H 0.2106 1.0874 0.0896 0.067 Uiso 0.40 1 calc PR I 2 H48E H 0.3020 1.0220 0.0905 0.067 Uiso 0.40 1 calc PR I 2 H48F H 0.2474 0.9242 0.1214 0.067 Uiso 0.40 1 calc PR I 2 O50B O 0.1287(6) 0.8991(18) 0.0331(5) 0.053(3) Uiso 0.40 1 d PD I 2 O51B O 0.2385(7) 0.8279(13) 0.0085(4) 0.047(3) Uiso 0.40 1 d PD I 2 C48C C 0.2656(13) 0.944(2) 0.0914(7) 0.027(4) Uiso 0.20 1 d PD I 3 H48G H 0.2642 1.0614 0.0953 0.041 Uiso 0.20 1 calc PR I 3 H48H H 0.3229 0.9101 0.0927 0.041 Uiso 0.20 1 calc PR I 3 H48I H 0.2504 0.8924 0.1213 0.041 Uiso 0.20 1 calc PR I 3 O50C O 0.2163(18) 1.009(3) 0.0026(11) 0.126(10) Uiso 0.20 1 d PD I 3 O51C O 0.1317(12) 0.853(3) 0.0221(11) 0.094(9) Uiso 0.20 1 d PD I 3 C52A C 0.6141(8) 1.0175(17) 0.0250(5) 0.046(3) Uiso 0.40 1 d PD J 1 H52A H 0.5569 1.0040 0.0281 0.069 Uiso 0.40 1 calc PR J 1 H52B H 0.6179 0.9594 -0.0072 0.069 Uiso 0.40 1 calc PR J 1 H52C H 0.6252 1.1325 0.0214 0.069 Uiso 0.40 1 calc PR J 1 N53A N 0.6775(7) 0.9524(12) 0.0741(4) 0.059(2) Uiso 0.40 1 d PD J 1 O54A O 0.6783(9) 0.8126(15) 0.0941(6) 0.123(4) Uiso 0.40 1 d PD J 1 O55A O 0.7080(6) 1.0467(11) 0.1084(4) 0.051(3) Uiso 0.40 1 d PD J 1 C52B C 0.6112(6) 0.9743(13) 0.0252(4) 0.058(3) Uiso 0.60 1 d PD J . H52D H 0.5816 1.0653 0.0355 0.087 Uiso 0.60 1 calc PR . . H52E H 0.5844 0.8729 0.0307 0.087 Uiso 0.60 1 calc PR . . H52F H 0.6077 0.9843 -0.0132 0.087 Uiso 0.60 1 calc PR . . N53B N 0.7047(4) 0.9745(6) 0.0606(2) 0.0432(12) Uiso 0.60 1 d PD . . O54B O 0.7547(5) 0.8827(9) 0.0477(3) 0.036(2) Uiso 0.35 1 d PD J 2 O55B O 0.7279(11) 1.0605(17) 0.1005(6) 0.040(4) Uiso 0.35 1 d PD J 2 O54C O 0.7375(7) 0.8555(12) 0.0536(4) 0.034(3) Uiso 0.25 1 d PD J 3 O55C O 0.7391(14) 1.074(2) 0.0975(8) 0.058(8) Uiso 0.25 1 d PD J 3 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 0.0242(3) 0.0270(2) 0.0232(2) 0.00081(15) 0.00499(17) 0.00050(15) N2 0.0246(12) 0.0258(11) 0.0246(12) 0.0014(9) 0.0073(10) 0.0016(9) C3 0.0263(14) 0.0267(13) 0.0278(14) -0.0009(11) 0.0086(11) -0.0009(11) C4 0.0295(15) 0.0320(15) 0.0322(15) -0.0013(12) 0.0089(13) -0.0039(12) N5 0.0267(13) 0.0376(14) 0.0314(14) 0.0003(11) 0.0032(11) -0.0003(11) C6 0.0305(15) 0.0332(15) 0.0295(15) 0.0056(12) 0.0058(12) 0.0039(12) C7 0.0288(15) 0.0270(13) 0.0252(13) -0.0001(11) 0.0089(12) -0.0004(11) N8 0.0299(13) 0.0245(11) 0.0301(13) 0.0025(10) 0.0084(10) -0.0007(10) N9 0.0286(12) 0.0293(12) 0.0254(12) 0.0000(10) 0.0065(10) 0.0024(10) C10 0.0373(17) 0.0316(15) 0.0295(15) 0.0048(12) 0.0115(13) 0.0077(12) C11 0.048(2) 0.0278(15) 0.0412(18) 0.0060(13) 0.0188(16) 0.0026(14) C12 0.0381(17) 0.0280(14) 0.0425(18) 0.0018(13) 0.0175(14) -0.0038(13) N13 0.0284(12) 0.0281(12) 0.0261(12) 0.0031(10) 0.0066(10) -0.0010(10) N14 0.0290(12) 0.0301(12) 0.0245(12) 0.0003(10) 0.0065(10) -0.0023(10) C15 0.0361(17) 0.0368(16) 0.0320(16) -0.0036(13) 0.0123(13) -0.0096(13) C16 0.0448(19) 0.0340(16) 0.0389(18) -0.0004(13) 0.0170(15) -0.0086(14) C17 0.0406(17) 0.0296(15) 0.0340(16) 0.0025(12) 0.0131(14) -0.0022(13) N18 0.0274(13) 0.0319(13) 0.0293(13) 0.0027(10) 0.0049(11) 0.0012(10) C19 0.0346(16) 0.0333(15) 0.0276(15) 0.0029(12) 0.0043(13) 0.0002(12) C20 0.0404(19) 0.053(2) 0.0331(18) 0.0042(15) -0.0007(15) 0.0001(16) N21 0.0315(15) 0.065(2) 0.0432(18) 0.0053(16) -0.0016(13) 0.0065(15) C22 0.0275(16) 0.061(2) 0.047(2) 0.0054(18) 0.0040(15) 0.0066(16) C23 0.0292(16) 0.0413(17) 0.0361(17) 0.0048(14) 0.0077(13) 0.0024(13) N24 0.0367(14) 0.0353(13) 0.0231(12) -0.0013(10) 0.0042(11) 0.0003(11) N25 0.0329(13) 0.0276(12) 0.0264(12) 0.0023(10) 0.0063(10) -0.0003(10) C26 0.0392(17) 0.0281(14) 0.0331(16) 0.0016(12) 0.0135(13) 0.0019(12) C27 0.056(2) 0.0381(17) 0.0330(17) -0.0039(14) 0.0193(16) 0.0027(15) C28 0.052(2) 0.0393(17) 0.0265(15) -0.0018(13) 0.0089(15) -0.0030(15) N29 0.0262(13) 0.0490(16) 0.0357(14) -0.0010(12) 0.0088(11) 0.0045(12) N30 0.0259(12) 0.0343(13) 0.0315(13) -0.0005(11) 0.0073(10) 0.0007(10) C31 0.0365(17) 0.0422(18) 0.0324(16) -0.0054(14) 0.0119(14) -0.0038(14) C32 0.040(2) 0.068(3) 0.045(2) -0.0092(19) 0.0216(17) -0.0027(18) C33 0.0347(18) 0.060(2) 0.054(2) -0.0043(18) 0.0209(17) 0.0036(16) _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 N18 1.891(3) . ? Fe1 N2 1.896(3) . ? Fe1 N30 1.978(3) . ? Fe1 N14 1.981(3) . ? Fe1 N9 1.982(3) . ? Fe1 N25 1.998(3) . ? N2 C3 1.333(4) . ? N2 C7 1.333(4) . ? C3 C4 1.384(4) . ? C3 N8 1.396(4) . ? C4 N5 1.337(4) . ? N5 C6 1.341(4) . ? C6 C7 1.387(4) . ? C7 N13 1.394(4) . ? N8 C12 1.362(4) . ? N8 N9 1.382(3) . ? N9 C10 1.320(4) . ? C10 C11 1.401(5) . ? C11 C12 1.368(5) . ? N13 C17 1.363(4) . ? N13 N14 1.379(3) . ? N14 C15 1.322(4) . ? C15 C16 1.402(5) . ? C16 C17 1.361(5) . ? N18 C23 1.337(4) . ? N18 C19 1.339(4) . ? C19 C20 1.384(5) . ? C19 N24 1.396(4) . ? C20 N21 1.336(5) . ? N21 C22 1.331(5) . ? C22 C23 1.386(5) . ? C23 N29 1.393(4) . ? N24 C28 1.353(4) . ? N24 N25 1.386(4) . ? N25 C26 1.319(4) . ? C26 C27 1.408(5) . ? C27 C28 1.359(5) . ? N29 C33 1.363(5) . ? N29 N30 1.381(4) . ? N30 C31 1.324(4) . ? C31 C32 1.395(5) . ? C32 C33 1.359(6) . ? B34A F36A 1.388(16) . ? B34A F35A 1.399(16) . ? B34A F37A 1.401(17) . ? B34A F38A 1.408(16) . ? B34B F35B 1.388(15) . ? B34B F36B 1.400(15) . ? B34B F38B 1.405(16) . ? B34B F37B 1.415(15) . ? B34C F37C 1.391(16) . ? B34C F36C 1.392(15) . ? B34C F35C 1.399(16) . ? B34C F38C 1.401(16) . ? B39A F42A 1.356(14) . ? B39A F41A 1.372(14) . ? B39A F40A 1.377(13) . ? B39A F43A 1.384(14) . ? B39B F40B 1.328(15) . ? B39B F42B 1.365(14) . ? B39B F41C 1.378(11) . ? B39B F43C 1.399(12) . ? B39B F40C 1.409(11) . ? B39B F42C 1.433(12) . ? B39B F43B 1.454(15) . ? B39B F41B 1.454(15) . ? C44A N45A 1.368(13) . ? N45A O47A 1.190(12) . ? N45A O46A 1.230(13) . ? C44B N45B 1.461(10) . ? N45B O47B 1.163(16) . ? N45B O46C 1.203(9) . ? N45B O46B 1.207(18) . ? N45B O47C 1.215(13) . ? C48A N49A 1.458(13) . ? N49A O50A 1.190(12) . ? N49A O51A 1.321(13) . ? N49B O51C 1.176(16) . ? N49B O50B 1.199(10) . ? N49B O51B 1.229(10) . ? N49B O50C 1.382(17) . ? N49B C48C 1.496(14) . ? N49B C48B 1.512(11) . ? C52A N53A 1.472(13) . ? N53A O55A 1.171(11) . ? N53A O54A 1.266(13) . ? C52B N53B 1.532(10) . ? N53B O54C 1.166(10) . ? N53B O55B 1.213(11) . ? N53B O54B 1.243(9) . ? N53B O55C 1.254(14) . ? 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 N18 Fe1 N2 177.40(11) . . ? N18 Fe1 N30 79.73(11) . . ? N2 Fe1 N30 98.23(11) . . ? N18 Fe1 N14 101.98(11) . . ? N2 Fe1 N14 79.53(10) . . ? N30 Fe1 N14 89.38(11) . . ? N18 Fe1 N9 98.65(11) . . ? N2 Fe1 N9 79.85(10) . . ? N30 Fe1 N9 94.07(11) . . ? N14 Fe1 N9 159.37(11) . . ? N18 Fe1 N25 79.50(11) . . ? N2 Fe1 N25 102.60(10) . . ? N30 Fe1 N25 159.11(11) . . ? N14 Fe1 N25 92.79(10) . . ? N9 Fe1 N25 91.18(10) . . ? C3 N2 C7 119.0(3) . . ? C3 N2 Fe1 120.3(2) . . ? C7 N2 Fe1 120.6(2) . . ? N2 C3 C4 120.9(3) . . ? N2 C3 N8 111.1(3) . . ? C4 C3 N8 128.0(3) . . ? N5 C4 C3 120.0(3) . . ? C4 N5 C6 119.5(3) . . ? N5 C6 C7 119.9(3) . . ? N2 C7 C6 120.8(3) . . ? N2 C7 N13 110.9(2) . . ? C6 C7 N13 128.4(3) . . ? C12 N8 N9 111.0(3) . . ? C12 N8 C3 132.4(3) . . ? N9 N8 C3 116.3(2) . . ? C10 N9 N8 105.2(2) . . ? C10 N9 Fe1 142.0(2) . . ? N8 N9 Fe1 112.31(18) . . ? N9 C10 C11 111.0(3) . . ? C12 C11 C10 106.3(3) . . ? N8 C12 C11 106.4(3) . . ? C17 N13 N14 110.9(2) . . ? C17 N13 C7 132.6(3) . . ? N14 N13 C7 116.3(2) . . ? C15 N14 N13 105.1(2) . . ? C15 N14 Fe1 141.9(2) . . ? N13 N14 Fe1 112.58(18) . . ? N14 C15 C16 111.2(3) . . ? C17 C16 C15 106.1(3) . . ? C16 C17 N13 106.8(3) . . ? C23 N18 C19 118.4(3) . . ? C23 N18 Fe1 120.4(2) . . ? C19 N18 Fe1 121.2(2) . . ? N18 C19 C20 120.8(3) . . ? N18 C19 N24 110.7(3) . . ? C20 C19 N24 128.6(3) . . ? N21 C20 C19 120.4(4) . . ? C22 N21 C20 119.2(3) . . ? N21 C22 C23 120.3(3) . . ? N18 C23 C22 120.9(3) . . ? N18 C23 N29 111.0(3) . . ? C22 C23 N29 128.1(3) . . ? C28 N24 N25 110.9(3) . . ? C28 N24 C19 132.4(3) . . ? N25 N24 C19 116.5(2) . . ? C26 N25 N24 105.1(3) . . ? C26 N25 Fe1 142.7(2) . . ? N24 N25 Fe1 112.10(19) . . ? N25 C26 C27 110.7(3) . . ? C28 C27 C26 106.3(3) . . ? N24 C28 C27 106.9(3) . . ? C33 N29 N30 110.9(3) . . ? C33 N29 C23 132.7(3) . . ? N30 N29 C23 116.1(3) . . ? C31 N30 N29 104.9(3) . . ? C31 N30 Fe1 142.3(2) . . ? N29 N30 Fe1 112.6(2) . . ? N30 C31 C32 111.1(3) . . ? C33 C32 C31 106.6(3) . . ? C32 C33 N29 106.6(3) . . ? F36A B34A F35A 110.6(13) . . ? F36A B34A F37A 114.0(13) . . ? F35A B34A F37A 104.1(12) . . ? F36A B34A F38A 111.1(12) . . ? F35A B34A F38A 110.3(13) . . ? F37A B34A F38A 106.4(13) . . ? F35B B34B F36B 110.9(12) . . ? F35B B34B F38B 108.6(12) . . ? F36B B34B F38B 109.3(12) . . ? F35B B34B F37B 112.2(13) . . ? F36B B34B F37B 104.1(11) . . ? F38B B34B F37B 111.7(13) . . ? F37C B34C F36C 110.0(13) . . ? F37C B34C F35C 109.0(12) . . ? F36C B34C F35C 109.7(13) . . ? F37C B34C F38C 110.6(13) . . ? F36C B34C F38C 109.2(12) . . ? F35C B34C F38C 108.3(13) . . ? F42A B39A F41A 113.0(12) . . ? F42A B39A F40A 113.9(12) . . ? F41A B39A F40A 105.9(10) . . ? F42A B39A F43A 102.7(10) . . ? F41A B39A F43A 109.1(11) . . ? F40A B39A F43A 112.2(11) . . ? F40B B39B F42B 119.0(14) . . ? F41C B39B F43C 115.4(9) . . ? F41C B39B F40C 112.2(8) . . ? F43C B39B F40C 109.9(9) . . ? F41C B39B F42C 105.8(8) . . ? F43C B39B F42C 114.3(8) . . ? F40C B39B F42C 97.9(8) . . ? F40B B39B F43B 110.2(13) . . ? F42B B39B F43B 105.3(12) . . ? F40B B39B F41B 111.1(13) . . ? F42B B39B F41B 110.5(12) . . ? F43B B39B F41B 98.8(12) . . ? O47A N45A O46A 122.5(11) . . ? O47A N45A C44A 109.5(11) . . ? O46A N45A C44A 125.4(11) . . ? O47B N45B O46B 122.0(19) . . ? O46C N45B O47C 123.6(11) . . ? O47B N45B C44B 139.7(15) . . ? O46B N45B C44B 89.1(18) . . ? O46C N45B C44B 122.1(11) . . ? O47C N45B C44B 113.3(11) . . ? O50A N49A O51A 112.2(11) . . ? O50A N49A C48A 128.5(12) . . ? O51A N49A C48A 113.5(12) . . ? O50B N49B O51B 128.2(10) . . ? O51C N49B O50C 108.3(15) . . ? O51C N49B C48C 137.1(17) . . ? O50C N49B C48C 102.6(15) . . ? O50B N49B C48B 104.2(9) . . ? O51B N49B C48B 127.6(9) . . ? O55A N53A O54A 110.8(11) . . ? O55A N53A C52A 115.5(10) . . ? O54A N53A C52A 126.9(12) . . ? O55B N53B O54B 121.8(10) . . ? O54C N53B O55C 123.5(12) . . ? O55B N53B C52B 120.1(10) . . ? O54B N53B C52B 118.1(7) . . ? O54C N53B C52B 109.7(11) . . ? O55C N53B C52B 126.0(12) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.955 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.131 #=END data_je12 _database_code_CSD 195910 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3,5-dimethylpyrazol-1-yl)pyrazine]iron(II) ditetrafluoroborate hemiacetone solvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H32 Fe N12, 2[B F4], 0.5[C3 H6 O], 0.1[H2 O]' _chemical_formula_sum 'C29.50 H35 B2 F8 Fe N12 O0.60' _chemical_formula_weight 796.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 '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 Monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.3306(1) _cell_length_b 15.2392(2) _cell_length_c 40.5559(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.8371(6) _cell_angle_gamma 90.00 _cell_volume 6994.17(14) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 62394 _cell_measurement_theta_min 2.76 _cell_measurement_theta_max 27.48 _exptl_crystal_description Plate _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3270 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8476 _exptl_absorpt_correction_T_max 0.9500 _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 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 62394 _diffrn_reflns_av_R_equivalents 0.1278 _diffrn_reflns_av_sigmaI/netI 0.1418 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 2.76 _diffrn_reflns_theta_max 27.48 _reflns_number_total 15966 _reflns_number_gt 7795 _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 of the structure contains two complex dications, four BF~4~^-^ anions, one molecule of acetone, and one weak feature not bonded to any other residue that was modelled as a molecule of water with occupancy 0.2 (O107). Although the H atoms at O107 were not included in the model (see below), O107 makes the following interatomic contacts which could correspond to H-bonds to other residues in the lattice: O107...F89A = 3.69\%A O107...F89B = 3.30\%A O107...F102A = 2.94\%A (but see below). O107...F102B = 3.54\%A O107...O107' = 3.12\%A (related by 1-x, 1-y, -z) However, O107 also makes abnormally short contacts to F100B (2.43\%A) and F100C (2.21\%A), suggesting that O107 can only be occupied when the anion B98A-F102C is in its 'A' disorder orientation (see below). Three of the four BF~4~^-^ anions are disordered: B88, F89A-F92A (occupancy 0.4) B88, F89B-F92B (occupancy 0.4) B88, F89B, F90C-F92C (occupancy 0.2) So that B88 is wholly occupied and F89B was occupany 0.6. Attempts to refine separate partial B atoms for these three disorder orientations were unsuccessful. B93A-F97A (occupancy 0.4) B93B-F97B (occupancy 0.4) B93C-F97C (occupancy 0.2) and B98A-F102A (occupancy 0.4) B98B-F102B (occupancy 0.4) B98B, F99C-F102C (occupancy 0.2) So that B98B has total occupancy 0.6. Attempts to refine separate partial B atoms for these two disorder orientations were unsuccessful. All disordered B-F distances were restrained to 1.39(2)\%A, and F...F distances within a given disorder orientation to 2.27(2)\%A. All non-H atoms with occupancy >=0.5 were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except for those attached to O107 which were not included in the final model. ; _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^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15966 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 89 _refine_ls_R_factor_all 0.1587 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1620 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.973 _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 0.15533(5) 0.33074(3) 0.210607(12) 0.02496(15) Uani 1 1 d . . . N2 N 0.1864(3) 0.31760(18) 0.25631(7) 0.0244(7) Uani 1 1 d . . . C3 C 0.2132(3) 0.2381(2) 0.26929(8) 0.0251(8) Uani 1 1 d . . . C4 C 0.2364(4) 0.2292(2) 0.30319(9) 0.0321(10) Uani 1 1 d . . . H4 H 0.2540 0.1729 0.3122 0.039 Uiso 1 1 calc R . . N5 N 0.2342(3) 0.2988(2) 0.32314(7) 0.0331(8) Uani 1 1 d . . . C6 C 0.2060(4) 0.3773(2) 0.31029(9) 0.0331(10) Uani 1 1 d . . . H6 H 0.2031 0.4271 0.3244 0.040 Uiso 1 1 calc R . . C7 C 0.1808(3) 0.3870(2) 0.27681(8) 0.0253(9) Uani 1 1 d . . . N8 N 0.2106(3) 0.17371(18) 0.24488(7) 0.0261(7) Uani 1 1 d . . . N9 N 0.1892(3) 0.20216(19) 0.21249(7) 0.0257(7) Uani 1 1 d . . . C10 C 0.2013(3) 0.1314(2) 0.19388(9) 0.0296(9) Uani 1 1 d . . . C11 C 0.2285(4) 0.0581(2) 0.21365(9) 0.0315(10) Uani 1 1 d . . . H11 H 0.2405 0.0000 0.2060 0.038 Uiso 1 1 calc R . . C12 C 0.2346(3) 0.0846(2) 0.24571(9) 0.0297(9) Uani 1 1 d . . . C13 C 0.1884(4) 0.1318(2) 0.15699(9) 0.0388(11) Uani 1 1 d . . . H13A H 0.1083 0.1507 0.1500 0.058 Uiso 1 1 calc R . . H13B H 0.2024 0.0726 0.1486 0.058 Uiso 1 1 calc R . . H13C H 0.2460 0.1725 0.1482 0.058 Uiso 1 1 calc R . . C14 C 0.2599(4) 0.0343(2) 0.27682(9) 0.0386(11) Uani 1 1 d . . . H14A H 0.2704 -0.0279 0.2716 0.058 Uiso 1 1 calc R . . H14B H 0.1938 0.0409 0.2913 0.058 Uiso 1 1 calc R . . H14C H 0.3323 0.0569 0.2880 0.058 Uiso 1 1 calc R . . N15 N 0.1452(3) 0.46199(18) 0.25926(7) 0.0267(7) Uani 1 1 d . . . N16 N 0.1341(3) 0.45333(18) 0.22503(7) 0.0268(7) Uani 1 1 d . . . C17 C 0.0990(4) 0.5309(2) 0.21379(9) 0.0316(9) Uani 1 1 d . . . C18 C 0.0826(4) 0.5882(2) 0.24057(9) 0.0358(10) Uani 1 1 d . . . H18 H 0.0551 0.6470 0.2390 0.043 Uiso 1 1 calc R . . C19 C 0.1130(3) 0.5447(2) 0.26882(9) 0.0300(9) Uani 1 1 d . . . C20 C 0.0833(5) 0.5497(3) 0.17787(10) 0.0502(13) Uani 1 1 d . . . H20A H 0.1599 0.5458 0.1678 0.075 Uiso 1 1 calc R . . H20B H 0.0509 0.6089 0.1747 0.075 Uiso 1 1 calc R . . H20C H 0.0287 0.5067 0.1675 0.075 Uiso 1 1 calc R . . C21 C 0.1112(4) 0.5743(2) 0.30374(9) 0.0396(11) Uani 1 1 d . . . H21A H 0.0754 0.6327 0.3046 0.059 Uiso 1 1 calc R . . H21B H 0.1922 0.5767 0.3133 0.059 Uiso 1 1 calc R . . H21C H 0.0649 0.5329 0.3163 0.059 Uiso 1 1 calc R . . N22 N 0.1207(3) 0.33591(17) 0.16479(7) 0.0241(7) Uani 1 1 d . . . C23 C 0.2083(3) 0.3490(2) 0.14380(9) 0.0277(9) Uani 1 1 d . . . C24 C 0.1850(4) 0.3405(2) 0.11017(9) 0.0314(9) Uani 1 1 d . . . H24 H 0.2475 0.3478 0.0957 0.038 Uiso 1 1 calc R . . N25 N 0.0761(3) 0.32226(19) 0.09755(7) 0.0320(8) Uani 1 1 d . . . C26 C -0.0105(4) 0.3107(2) 0.11832(9) 0.0287(9) Uani 1 1 d . . . H26 H -0.0884 0.2984 0.1098 0.034 Uiso 1 1 calc R . . C27 C 0.0126(3) 0.3164(2) 0.15221(8) 0.0252(9) Uani 1 1 d . . . N28 N 0.3143(3) 0.36758(19) 0.16099(7) 0.0300(8) Uani 1 1 d . . . N29 N 0.3148(3) 0.35770(19) 0.19539(7) 0.0284(7) Uani 1 1 d . . . C30 C 0.4219(4) 0.3824(2) 0.20658(9) 0.0312(9) Uani 1 1 d . . . C31 C 0.4902(4) 0.4080(3) 0.18000(9) 0.0367(10) Uani 1 1 d . . . H31 H 0.5699 0.4275 0.1816 0.044 Uiso 1 1 calc R . . C32 C 0.4214(4) 0.3997(2) 0.15176(9) 0.0335(10) Uani 1 1 d . . . C33 C 0.4571(4) 0.3832(3) 0.24249(9) 0.0387(10) Uani 1 1 d . . . H33A H 0.4221 0.4344 0.2529 0.058 Uiso 1 1 calc R . . H33B H 0.5434 0.3863 0.2454 0.058 Uiso 1 1 calc R . . H33C H 0.4289 0.3295 0.2528 0.058 Uiso 1 1 calc R . . C34 C 0.4486(4) 0.4208(3) 0.11701(10) 0.0506(13) Uani 1 1 d . . . H34A H 0.4537 0.3663 0.1043 0.076 Uiso 1 1 calc R . . H34B H 0.5242 0.4520 0.1168 0.076 Uiso 1 1 calc R . . H34C H 0.3859 0.4579 0.1071 0.076 Uiso 1 1 calc R . . N35 N -0.0670(3) 0.30310(18) 0.17717(7) 0.0259(7) Uani 1 1 d . . . N36 N -0.0187(3) 0.31407(18) 0.20933(7) 0.0263(7) Uani 1 1 d . . . C37 C -0.1100(4) 0.3107(2) 0.22868(9) 0.0269(9) Uani 1 1 d . . . C38 C -0.2146(4) 0.2955(2) 0.20945(9) 0.0296(9) Uani 1 1 d . . . H38 H -0.2913 0.2892 0.2176 0.036 Uiso 1 1 calc R . . C39 C -0.1875(3) 0.2914(2) 0.17711(9) 0.0260(9) Uani 1 1 d . . . C40 C -0.0989(3) 0.3267(2) 0.26493(8) 0.0312(9) Uani 1 1 d . . . H40A H -0.0348 0.2907 0.2748 0.047 Uiso 1 1 calc R . . H40B H -0.1733 0.3112 0.2748 0.047 Uiso 1 1 calc R . . H40C H -0.0816 0.3888 0.2691 0.047 Uiso 1 1 calc R . . C41 C -0.2654(4) 0.2743(3) 0.14713(9) 0.0356(10) Uani 1 1 d . . . H41A H -0.2358 0.2233 0.1354 0.053 Uiso 1 1 calc R . . H41B H -0.2655 0.3258 0.1326 0.053 Uiso 1 1 calc R . . H41C H -0.3460 0.2627 0.1537 0.053 Uiso 1 1 calc R . . Fe42 Fe 0.17819(5) 0.74670(3) 0.044921(12) 0.02699(15) Uani 1 1 d . . . N43 N 0.2204(3) 0.73082(19) 0.00095(7) 0.0268(7) Uani 1 1 d . . . C44 C 0.2582(3) 0.7990(2) -0.01670(9) 0.0292(9) Uani 1 1 d . . . C45 C 0.2738(4) 0.7892(3) -0.05028(9) 0.0362(10) Uani 1 1 d . . . H45 H 0.2980 0.8381 -0.0629 0.043 Uiso 1 1 calc R . . N46 N 0.2551(3) 0.7120(2) -0.06494(8) 0.0387(9) Uani 1 1 d . . . C47 C 0.2230(4) 0.6431(3) -0.04720(9) 0.0358(10) Uani 1 1 d . . . H47 H 0.2108 0.5876 -0.0575 0.043 Uiso 1 1 calc R . . C48 C 0.2074(3) 0.6527(2) -0.01382(9) 0.0304(9) Uani 1 1 d . . . N49 N 0.2703(3) 0.87423(19) 0.00275(7) 0.0287(7) Uani 1 1 d . . . N50 N 0.2255(3) 0.86729(19) 0.03440(7) 0.0290(7) Uani 1 1 d . . . C51 C 0.2376(4) 0.9473(2) 0.04728(9) 0.0344(10) Uani 1 1 d . . . C52 C 0.2915(4) 1.0036(3) 0.02522(9) 0.0348(10) Uani 1 1 d . . . H52 H 0.3107 1.0635 0.0291 0.042 Uiso 1 1 calc R . . C53 C 0.3116(3) 0.9578(2) -0.00267(9) 0.0324(9) Uani 1 1 d . . . C54 C 0.1926(4) 0.9699(3) 0.08026(10) 0.0445(12) Uani 1 1 d . . . H54A H 0.1075 0.9581 0.0802 0.067 Uiso 1 1 calc R . . H54B H 0.2071 1.0322 0.0849 0.067 Uiso 1 1 calc R . . H54C H 0.2336 0.9342 0.0973 0.067 Uiso 1 1 calc R . . C55 C 0.3693(4) 0.9849(3) -0.03323(9) 0.0371(10) Uani 1 1 d . . . H55A H 0.3097 0.9892 -0.0515 0.056 Uiso 1 1 calc R . . H55B H 0.4289 0.9413 -0.0386 0.056 Uiso 1 1 calc R . . H55C H 0.4074 1.0421 -0.0297 0.056 Uiso 1 1 calc R . . N56 N 0.1708(3) 0.58845(19) 0.00849(7) 0.0300(8) Uani 1 1 d . . . N57 N 0.1451(3) 0.61912(19) 0.03985(7) 0.0292(8) Uani 1 1 d . . . C58 C 0.1183(4) 0.5484(2) 0.05673(9) 0.0321(9) Uani 1 1 d . . . C59 C 0.1268(4) 0.4726(2) 0.03723(9) 0.0393(11) Uani 1 1 d . . . H59 H 0.1111 0.4142 0.0438 0.047 Uiso 1 1 calc R . . C60 C 0.1619(4) 0.4987(2) 0.00701(9) 0.0348(10) Uani 1 1 d . . . C61 C 0.0842(4) 0.5552(3) 0.09213(9) 0.0455(12) Uani 1 1 d . . . H61A H 0.1551 0.5654 0.1064 0.068 Uiso 1 1 calc R . . H61B H 0.0463 0.5004 0.0986 0.068 Uiso 1 1 calc R . . H61C H 0.0289 0.6041 0.0943 0.068 Uiso 1 1 calc R . . C62 C 0.1902(4) 0.4454(3) -0.02235(10) 0.0460(12) Uani 1 1 d . . . H62A H 0.1851 0.3829 -0.0169 0.069 Uiso 1 1 calc R . . H62B H 0.2704 0.4592 -0.0287 0.069 Uiso 1 1 calc R . . H62C H 0.1336 0.4590 -0.0407 0.069 Uiso 1 1 calc R . . N63 N 0.1348(3) 0.76200(18) 0.08879(7) 0.0265(7) Uani 1 1 d . . . C64 C 0.0225(3) 0.7798(2) 0.09537(9) 0.0259(9) Uani 1 1 d . . . C65 C -0.0099(4) 0.7891(2) 0.12770(9) 0.0309(9) Uani 1 1 d . . . H65 H -0.0900 0.8008 0.1320 0.037 Uiso 1 1 calc R . . N66 N 0.0700(3) 0.7819(2) 0.15263(7) 0.0337(8) Uani 1 1 d . . . C67 C 0.1820(4) 0.7638(2) 0.14636(9) 0.0352(10) Uani 1 1 d . . . H67 H 0.2396 0.7590 0.1641 0.042 Uiso 1 1 calc R . . C68 C 0.2153(3) 0.7520(2) 0.11405(8) 0.0271(9) Uani 1 1 d . . . N69 N -0.0487(3) 0.78604(19) 0.06634(7) 0.0283(7) Uani 1 1 d . . . N70 N 0.0097(3) 0.77792(19) 0.03681(7) 0.0286(7) Uani 1 1 d . . . C71 C -0.0719(4) 0.7922(2) 0.01279(9) 0.0307(9) Uani 1 1 d . . . C72 C -0.1832(4) 0.8070(2) 0.02650(9) 0.0340(10) Uani 1 1 d . . . H72 H -0.2560 0.8170 0.0145 0.041 Uiso 1 1 calc R . . C73 C -0.1668(4) 0.8041(2) 0.05993(9) 0.0291(9) Uani 1 1 d . . . C74 C -0.0446(4) 0.7944(3) -0.02294(9) 0.0434(11) Uani 1 1 d . . . H74A H 0.0064 0.8448 -0.0270 0.065 Uiso 1 1 calc R . . H74B H -0.1183 0.7997 -0.0365 0.065 Uiso 1 1 calc R . . H74C H -0.0040 0.7401 -0.0287 0.065 Uiso 1 1 calc R . . C75 C -0.2522(4) 0.8154(3) 0.08606(10) 0.0395(11) Uani 1 1 d . . . H75A H -0.2457 0.7658 0.1014 0.059 Uiso 1 1 calc R . . H75B H -0.3325 0.8180 0.0760 0.059 Uiso 1 1 calc R . . H75C H -0.2348 0.8701 0.0981 0.059 Uiso 1 1 calc R . . N76 N 0.3249(3) 0.7277(2) 0.10295(7) 0.0309(8) Uani 1 1 d . . . N77 N 0.3310(3) 0.7197(2) 0.06872(7) 0.0320(8) Uani 1 1 d . . . C78 C 0.4376(4) 0.6861(3) 0.06408(10) 0.0387(10) Uani 1 1 d . . . C79 C 0.4986(4) 0.6719(3) 0.09462(10) 0.0439(11) Uani 1 1 d . . . H79 H 0.5760 0.6484 0.0978 0.053 Uiso 1 1 calc R . . C80 C 0.4273(4) 0.6976(3) 0.11888(10) 0.0381(10) Uani 1 1 d . . . C81 C 0.4786(4) 0.6674(4) 0.03026(11) 0.0689(16) Uani 1 1 d . . . H81A H 0.4341 0.6177 0.0207 0.103 Uiso 1 1 calc R . . H81B H 0.5630 0.6530 0.0317 0.103 Uiso 1 1 calc R . . H81C H 0.4656 0.7192 0.0162 0.103 Uiso 1 1 calc R . . C82 C 0.4488(4) 0.6960(3) 0.15527(10) 0.0545(13) Uani 1 1 d . . . H82A H 0.5287 0.6742 0.1607 0.082 Uiso 1 1 calc R . . H82B H 0.3910 0.6573 0.1651 0.082 Uiso 1 1 calc R . . H82C H 0.4408 0.7555 0.1641 0.082 Uiso 1 1 calc R . . B83 B 0.8823(5) 0.0436(3) 0.10727(13) 0.0435(13) Uani 1 1 d . . . F84 F 0.7656(3) 0.0400(2) 0.11548(8) 0.0836(10) Uani 1 1 d . . . F85 F 0.8907(2) 0.0298(2) 0.07399(6) 0.0718(9) Uani 1 1 d . . . F86 F 0.9264(3) 0.12433(15) 0.11620(7) 0.0682(8) Uani 1 1 d . . . F87 F 0.9460(3) -0.01976(16) 0.12472(6) 0.0714(9) Uani 1 1 d . . . B88 B 0.7773(5) 0.5433(3) 0.12554(13) 0.0435(13) Uani 1 1 d D . . F89A F 0.7510(9) 0.5440(7) 0.0943(2) 0.063(4) Uiso 0.40 1 d PD A 1 F90A F 0.8490(6) 0.6192(4) 0.13551(16) 0.0338(19) Uiso 0.40 1 d PD A 1 F91A F 0.8489(7) 0.4773(5) 0.1428(2) 0.056(3) Uiso 0.40 1 d PD A 1 F92A F 0.6772(9) 0.5416(8) 0.1451(2) 0.053(4) Uiso 0.40 1 d PD A 1 F89B F 0.7130(7) 0.5199(5) 0.09421(12) 0.079(2) Uani 0.60 1 d PD A . F90B F 0.8373(8) 0.6206(5) 0.1228(3) 0.054(3) Uiso 0.40 1 d PD A 2 F91B F 0.8470(8) 0.4729(5) 0.1311(3) 0.043(3) Uiso 0.40 1 d PD A 2 F92B F 0.6865(9) 0.5628(6) 0.1460(2) 0.036(3) Uiso 0.40 1 d PD A 2 F90C F 0.8262(16) 0.6194(9) 0.1117(4) 0.081(8) Uiso 0.20 1 d PD A 3 F91C F 0.8592(11) 0.4717(8) 0.1204(3) 0.041(5) Uiso 0.20 1 d PD A 3 F92C F 0.7115(14) 0.5385(13) 0.1491(3) 0.043(5) Uiso 0.20 1 d PD A 3 B93A B 0.4120(12) 0.6533(9) 0.2387(4) 0.029(4) Uani 0.50 1 d PD B 1 F94A F 0.5298(7) 0.6766(6) 0.2338(3) 0.076(4) Uani 0.50 1 d PD B 1 F95A F 0.3388(14) 0.7185(9) 0.2244(4) 0.075(6) Uani 0.50 1 d PD B 1 F96A F 0.3883(9) 0.5744(5) 0.2228(3) 0.075(3) Uani 0.50 1 d PD B 1 F97A F 0.3966(10) 0.6463(7) 0.27175(16) 0.077(3) Uani 0.50 1 d PD B 1 B93B B 0.3961(19) 0.6415(14) 0.2372(5) 0.066(13) Uiso 0.35 1 d PD C 2 F94B F 0.5175(12) 0.6442(9) 0.2334(5) 0.088(7) Uiso 0.35 1 d PD C 2 F95B F 0.3463(17) 0.7214(10) 0.2285(5) 0.033(5) Uiso 0.35 1 d PD C 2 F96B F 0.3557(12) 0.5787(9) 0.2145(3) 0.059(4) Uiso 0.35 1 d PD C 2 F97B F 0.3703(15) 0.6120(10) 0.2682(3) 0.065(5) Uiso 0.35 1 d PD C 2 B93C B 0.422(2) 0.6586(17) 0.2458(6) 0.10(4) Uiso 0.15 1 d PD D 3 F94C F 0.524(2) 0.658(2) 0.2278(5) 0.015(5) Uiso 0.15 1 d PD D 3 F95C F 0.4542(19) 0.6941(13) 0.2762(4) 0.059(7) Uiso 0.15 1 d PD D 3 F96C F 0.335(3) 0.709(2) 0.2294(8) 0.045(14) Uiso 0.15 1 d PD D 3 F97C F 0.380(2) 0.5743(13) 0.2501(7) 0.097(8) Uiso 0.15 1 d PD D 3 B98A B 0.3948(12) 0.2241(9) 0.0574(4) 0.048(5) Uiso 0.40 1 d PD E 1 F99A F 0.4443(8) 0.1812(5) 0.03060(19) 0.048(3) Uiso 0.40 1 d PD E 1 F100A F 0.3012(5) 0.1818(3) 0.06720(13) 0.0407(14) Uiso 0.40 1 d PD E 1 F101A F 0.4830(8) 0.2343(6) 0.0817(2) 0.074(3) Uiso 0.40 1 d PD E 1 F102A F 0.3649(8) 0.3119(4) 0.04816(18) 0.063(2) Uiso 0.40 1 d PD E 1 B98B B 0.4152(7) 0.2451(6) 0.0462(2) 0.044(2) Uani 0.60 1 d PD . . F99B F 0.4316(11) 0.1892(7) 0.0205(3) 0.041(4) Uiso 0.40 1 d PD F 2 F100B F 0.5002(8) 0.3111(6) 0.0475(2) 0.078(4) Uiso 0.40 1 d PD F 2 F101B F 0.4055(11) 0.2060(7) 0.0756(2) 0.112(4) Uiso 0.40 1 d PD F 2 F102B F 0.3063(6) 0.2918(5) 0.03780(17) 0.0540(19) Uiso 0.40 1 d PD F 2 F99C F 0.4525(18) 0.1939(12) 0.0194(4) 0.043(8) Uiso 0.20 1 d PD F 3 F100C F 0.4708(13) 0.3265(8) 0.0424(4) 0.045(5) Uiso 0.20 1 d PD F 3 F101C F 0.4676(16) 0.2049(11) 0.0759(3) 0.055(5) Uiso 0.20 1 d PD F 3 F102C F 0.2982(10) 0.2480(10) 0.0476(4) 0.071(5) Uiso 0.20 1 d PD F 3 C103 C 0.4512(4) -0.0275(3) 0.14431(13) 0.0570(14) Uani 1 1 d . . . O104 O 0.3739(4) -0.0724(2) 0.15495(9) 0.0795(11) Uani 1 1 d . . . C105 C 0.4951(6) -0.0423(5) 0.11110(16) 0.121(3) Uani 1 1 d . . . H105A H 0.4502 -0.0900 0.1002 0.182 Uiso 1 1 calc R . . H105B H 0.5790 -0.0580 0.1130 0.182 Uiso 1 1 calc R . . H105C H 0.4851 0.0115 0.0980 0.182 Uiso 1 1 calc R . . C106 C 0.5024(5) 0.0477(4) 0.16300(16) 0.112(3) Uani 1 1 d . . . H106A H 0.4589 0.0567 0.1830 0.168 Uiso 1 1 calc R . . H106B H 0.4965 0.1006 0.1493 0.168 Uiso 1 1 calc R . . H106C H 0.5856 0.0358 0.1691 0.168 Uiso 1 1 calc R . . O107 O 0.5115(18) 0.4674(12) 0.0365(5) 0.083(6) Uiso 0.20 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 0.0295(3) 0.0225(3) 0.0229(3) 0.0006(2) 0.0012(2) -0.0005(2) N2 0.0286(19) 0.0192(16) 0.0254(16) 0.0004(13) 0.0014(14) 0.0000(14) C3 0.023(2) 0.026(2) 0.0260(19) -0.0026(17) 0.0013(16) -0.0042(17) C4 0.036(3) 0.031(2) 0.029(2) 0.0018(18) 0.0041(18) 0.0033(18) N5 0.041(2) 0.0321(19) 0.0262(17) 0.0025(15) 0.0033(16) 0.0051(16) C6 0.041(3) 0.030(2) 0.028(2) -0.0057(18) 0.0017(19) 0.0015(19) C7 0.028(2) 0.024(2) 0.024(2) -0.0033(16) 0.0015(17) -0.0019(17) N8 0.032(2) 0.0223(16) 0.0240(16) 0.0021(14) -0.0005(14) 0.0000(14) N9 0.027(2) 0.0260(17) 0.0234(16) 0.0016(14) -0.0002(14) 0.0028(14) C10 0.029(2) 0.024(2) 0.035(2) -0.0074(18) -0.0022(18) 0.0000(17) C11 0.041(3) 0.020(2) 0.034(2) -0.0038(17) -0.0012(19) 0.0048(18) C12 0.034(3) 0.020(2) 0.035(2) 0.0030(17) 0.0005(18) -0.0012(17) C13 0.051(3) 0.030(2) 0.035(2) -0.0074(19) -0.001(2) 0.004(2) C14 0.054(3) 0.022(2) 0.039(2) 0.0059(18) -0.003(2) 0.000(2) N15 0.033(2) 0.0241(17) 0.0229(16) -0.0002(13) -0.0010(14) -0.0003(14) N16 0.033(2) 0.0247(17) 0.0220(16) 0.0006(13) -0.0005(14) -0.0009(14) C17 0.038(3) 0.023(2) 0.034(2) 0.0013(17) -0.0020(19) 0.0000(18) C18 0.047(3) 0.019(2) 0.041(2) -0.0015(18) -0.003(2) 0.0036(19) C19 0.034(3) 0.022(2) 0.035(2) -0.0066(18) 0.0031(19) -0.0005(18) C20 0.085(4) 0.030(2) 0.035(2) 0.0074(19) -0.002(2) 0.008(2) C21 0.050(3) 0.029(2) 0.040(2) -0.0075(18) 0.003(2) 0.002(2) N22 0.027(2) 0.0185(15) 0.0271(16) -0.0001(13) 0.0023(14) -0.0004(14) C23 0.032(3) 0.025(2) 0.027(2) -0.0010(16) 0.0033(18) -0.0012(17) C24 0.034(3) 0.034(2) 0.026(2) 0.0017(17) 0.0016(18) -0.0046(19) N25 0.040(2) 0.0313(18) 0.0241(17) 0.0006(14) 0.0007(16) -0.0012(16) C26 0.034(3) 0.027(2) 0.025(2) 0.0015(16) 0.0000(18) -0.0009(17) C27 0.031(2) 0.0199(19) 0.025(2) 0.0017(16) 0.0024(17) 0.0015(17) N28 0.030(2) 0.0350(19) 0.0248(17) 0.0012(14) 0.0038(15) -0.0069(15) N29 0.034(2) 0.0276(17) 0.0235(16) -0.0024(13) 0.0022(15) 0.0007(15) C30 0.030(3) 0.026(2) 0.037(2) -0.0071(18) -0.0002(19) -0.0006(18) C31 0.028(3) 0.043(2) 0.039(2) -0.007(2) 0.003(2) -0.006(2) C32 0.032(3) 0.037(2) 0.032(2) -0.0012(19) 0.0037(19) -0.0067(19) C33 0.034(3) 0.047(3) 0.035(2) -0.002(2) -0.0036(19) -0.004(2) C34 0.043(3) 0.073(3) 0.037(2) 0.003(2) 0.008(2) -0.024(2) N35 0.028(2) 0.0262(17) 0.0230(16) 0.0016(13) -0.0019(14) -0.0015(14) N36 0.034(2) 0.0214(16) 0.0236(16) 0.0019(13) 0.0000(14) -0.0005(14) C37 0.034(3) 0.0191(19) 0.027(2) 0.0012(16) 0.0030(19) -0.0025(17) C38 0.032(3) 0.028(2) 0.030(2) -0.0015(17) 0.0082(18) -0.0004(18) C39 0.024(2) 0.023(2) 0.031(2) 0.0006(16) 0.0018(17) -0.0005(17) C40 0.032(2) 0.034(2) 0.028(2) -0.0017(17) 0.0059(18) -0.0035(19) C41 0.028(2) 0.047(3) 0.031(2) -0.0008(19) 0.0013(18) -0.0008(19) Fe42 0.0293(3) 0.0294(3) 0.0223(3) 0.0015(2) 0.0020(2) 0.0013(3) N43 0.030(2) 0.0271(18) 0.0234(16) -0.0005(14) -0.0018(14) 0.0013(14) C44 0.028(2) 0.029(2) 0.031(2) 0.0048(18) 0.0036(18) 0.0012(18) C45 0.036(3) 0.041(2) 0.033(2) 0.004(2) 0.0064(19) 0.000(2) N46 0.049(3) 0.041(2) 0.0269(18) -0.0009(16) 0.0038(17) -0.0021(18) C47 0.042(3) 0.036(2) 0.029(2) -0.0012(19) 0.0055(19) -0.002(2) C48 0.029(2) 0.034(2) 0.028(2) 0.0023(18) 0.0032(18) 0.0048(18) N49 0.030(2) 0.0297(18) 0.0266(17) 0.0013(14) 0.0039(15) -0.0018(15) N50 0.033(2) 0.0305(18) 0.0240(16) -0.0009(14) 0.0026(14) -0.0001(15) C51 0.036(3) 0.031(2) 0.035(2) 0.0025(19) -0.0015(19) 0.0040(19) C52 0.035(3) 0.031(2) 0.038(2) 0.0026(19) 0.001(2) 0.0008(19) C53 0.028(2) 0.031(2) 0.038(2) 0.0066(19) 0.0012(19) -0.0007(18) C54 0.059(3) 0.034(2) 0.042(3) -0.006(2) 0.012(2) -0.008(2) C55 0.035(3) 0.039(2) 0.038(2) 0.0056(19) 0.006(2) -0.006(2) N56 0.038(2) 0.0284(18) 0.0244(17) 0.0015(14) 0.0061(15) 0.0024(15) N57 0.036(2) 0.0314(18) 0.0201(16) 0.0011(14) 0.0050(14) -0.0010(15) C58 0.032(3) 0.028(2) 0.036(2) 0.0016(18) 0.0037(19) 0.0010(18) C59 0.057(3) 0.025(2) 0.036(2) 0.0009(18) 0.006(2) -0.003(2) C60 0.041(3) 0.029(2) 0.034(2) -0.0001(18) 0.000(2) 0.0004(19) C61 0.069(4) 0.034(2) 0.035(2) 0.0041(19) 0.017(2) -0.002(2) C62 0.065(4) 0.033(2) 0.041(3) 0.000(2) 0.012(2) 0.001(2) N63 0.027(2) 0.0255(17) 0.0266(17) 0.0008(14) -0.0012(14) 0.0001(14) C64 0.028(2) 0.0205(19) 0.029(2) 0.0018(16) 0.0025(18) -0.0020(17) C65 0.032(3) 0.033(2) 0.029(2) 0.0002(17) 0.0050(19) 0.0008(18) N66 0.037(2) 0.0343(19) 0.0295(19) -0.0020(15) 0.0018(17) 0.0018(16) C67 0.041(3) 0.039(2) 0.025(2) -0.0014(18) -0.0018(19) 0.003(2) C68 0.033(2) 0.022(2) 0.027(2) -0.0002(17) 0.0016(17) -0.0007(18) N69 0.028(2) 0.0302(17) 0.0264(17) 0.0009(14) 0.0037(15) 0.0003(15) N70 0.032(2) 0.0302(18) 0.0236(17) 0.0010(14) 0.0047(15) 0.0011(15) C71 0.034(3) 0.026(2) 0.032(2) 0.0005(17) -0.0029(19) -0.0006(18) C72 0.031(3) 0.035(2) 0.036(2) 0.0015(18) -0.0032(19) 0.0055(19) C73 0.030(3) 0.020(2) 0.037(2) -0.0025(17) 0.0005(19) -0.0001(17) C74 0.043(3) 0.053(3) 0.034(2) 0.003(2) -0.002(2) 0.003(2) C75 0.029(3) 0.045(3) 0.045(3) 0.001(2) 0.005(2) 0.004(2) N76 0.033(2) 0.0372(19) 0.0226(16) 0.0005(14) 0.0000(15) 0.0008(16) N77 0.034(2) 0.0368(19) 0.0248(17) 0.0022(14) 0.0028(15) 0.0012(16) C78 0.032(3) 0.044(3) 0.040(2) 0.004(2) 0.001(2) 0.005(2) C79 0.030(3) 0.055(3) 0.047(3) 0.009(2) -0.003(2) 0.008(2) C80 0.032(3) 0.045(3) 0.037(2) 0.003(2) -0.008(2) -0.002(2) C81 0.049(4) 0.116(5) 0.043(3) -0.002(3) 0.010(2) 0.029(3) C82 0.041(3) 0.079(4) 0.042(3) -0.002(2) -0.008(2) 0.008(3) B83 0.044(4) 0.036(3) 0.050(3) -0.002(3) 0.003(3) -0.011(3) F84 0.047(2) 0.112(3) 0.094(2) -0.0430(19) 0.0230(17) -0.0207(17) F85 0.056(2) 0.116(3) 0.0436(16) -0.0116(15) 0.0023(14) 0.0005(17) F86 0.070(2) 0.0331(15) 0.100(2) 0.0001(14) -0.0067(17) -0.0065(14) F87 0.111(3) 0.0388(15) 0.0653(18) 0.0108(13) 0.0166(17) 0.0259(16) B88 0.048(4) 0.029(3) 0.054(3) 0.012(3) 0.009(3) 0.005(2) F89B 0.114(6) 0.090(5) 0.036(3) -0.029(3) 0.025(3) -0.015(5) B93A 0.019(7) 0.036(8) 0.035(7) 0.004(5) 0.016(5) 0.011(5) F94A 0.028(4) 0.052(6) 0.145(9) -0.033(5) -0.015(4) -0.001(4) F95A 0.083(8) 0.082(7) 0.063(9) 0.010(5) 0.025(5) 0.048(5) F96A 0.101(8) 0.031(4) 0.091(7) -0.002(4) -0.015(6) -0.002(4) F97A 0.109(9) 0.090(9) 0.034(4) 0.010(5) 0.017(4) 0.052(8) B98B 0.041(6) 0.046(6) 0.045(6) -0.002(5) 0.006(5) 0.003(5) C103 0.033(3) 0.065(4) 0.072(4) -0.009(3) 0.000(3) 0.004(3) O104 0.073(3) 0.077(3) 0.089(3) 0.006(2) 0.008(2) -0.006(2) C105 0.064(5) 0.186(8) 0.117(6) -0.070(5) 0.039(4) -0.036(5) C106 0.058(5) 0.144(6) 0.136(6) -0.077(5) 0.015(4) -0.027(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.880(3) . ? Fe1 N22 1.882(3) . ? Fe1 N16 1.976(3) . ? Fe1 N29 1.981(3) . ? Fe1 N36 1.986(3) . ? Fe1 N9 1.997(3) . ? N2 C3 1.349(4) . ? N2 C7 1.348(4) . ? C3 C4 1.394(5) . ? C3 N8 1.393(4) . ? C4 N5 1.336(4) . ? N5 C6 1.338(5) . ? C6 C7 1.381(5) . ? C7 N15 1.396(4) . ? N8 C12 1.384(4) . ? N8 N9 1.393(4) . ? N9 C10 1.328(4) . ? C10 C11 1.400(5) . ? C10 C13 1.496(5) . ? C11 C12 1.360(5) . ? C12 C14 1.492(5) . ? N15 C19 1.374(4) . ? N15 N16 1.394(4) . ? N16 C17 1.322(4) . ? C17 C18 1.413(5) . ? C17 C20 1.486(5) . ? C18 C19 1.353(5) . ? C19 C21 1.487(5) . ? N22 C27 1.336(5) . ? N22 C23 1.354(4) . ? C23 C24 1.382(5) . ? C23 N28 1.387(5) . ? C24 N25 1.341(5) . ? N25 C26 1.336(5) . ? C26 C27 1.389(5) . ? C27 N35 1.404(4) . ? N28 C32 1.378(5) . ? N28 N29 1.403(4) . ? N29 C30 1.329(5) . ? C30 C31 1.413(5) . ? C30 C33 1.491(5) . ? C31 C32 1.359(5) . ? C32 C34 1.493(5) . ? N35 C39 1.377(4) . ? N35 N36 1.400(4) . ? N36 C37 1.330(4) . ? C37 C38 1.406(5) . ? C37 C40 1.490(5) . ? C38 C39 1.363(5) . ? C39 C41 1.489(5) . ? Fe42 N63 1.884(3) . ? Fe42 N43 1.885(3) . ? Fe42 N50 1.967(3) . ? Fe42 N70 1.979(3) . ? Fe42 N77 1.984(3) . ? Fe42 N57 1.989(3) . ? N43 C48 1.338(4) . ? N43 C44 1.343(4) . ? C44 C45 1.390(5) . ? C44 N49 1.395(4) . ? C45 N46 1.331(5) . ? N46 C47 1.334(5) . ? C47 C48 1.382(5) . ? C48 N56 1.409(4) . ? N49 C53 1.378(4) . ? N49 N50 1.407(4) . ? N50 C51 1.331(4) . ? C51 C52 1.401(5) . ? C51 C54 1.495(5) . ? C52 C53 1.357(5) . ? C53 C55 1.488(5) . ? N56 C60 1.373(5) . ? N56 N57 1.399(4) . ? N57 C58 1.321(4) . ? C58 C59 1.405(5) . ? C58 C61 1.509(5) . ? C59 C60 1.366(5) . ? C60 C62 1.489(5) . ? N63 C64 1.340(4) . ? N63 C68 1.346(5) . ? C64 C65 1.386(5) . ? C64 N69 1.397(5) . ? C65 N66 1.328(5) . ? N66 C67 1.336(5) . ? C67 C68 1.393(5) . ? C68 N76 1.392(5) . ? N69 C73 1.378(5) . ? N69 N70 1.403(4) . ? N70 C71 1.328(5) . ? C71 C72 1.421(5) . ? C71 C74 1.497(5) . ? C72 C73 1.360(5) . ? C73 C75 1.479(5) . ? N76 C80 1.378(5) . ? N76 N77 1.399(4) . ? N77 C78 1.334(5) . ? C78 C79 1.405(6) . ? C78 C81 1.497(6) . ? C79 C80 1.362(5) . ? C80 C82 1.484(5) . ? B83 F86 1.369(5) . ? B83 F85 1.374(6) . ? B83 F84 1.381(6) . ? B83 F87 1.380(6) . ? B88 F92C 1.244(11) . ? B88 F89A 1.287(9) . ? B88 F91B 1.345(8) . ? B88 F90B 1.368(8) . ? B88 F92B 1.385(9) . ? B88 F90C 1.415(12) . ? B88 F92A 1.417(9) . ? B88 F91A 1.450(8) . ? B88 F91C 1.453(11) . ? B88 F90A 1.460(7) . ? B88 F89B 1.477(7) . ? B93A F97A 1.366(12) . ? B93A F96A 1.383(16) . ? B93A F95A 1.402(12) . ? B93A F94A 1.404(14) . ? B93B F97B 1.379(17) . ? B93B F95B 1.381(17) . ? B93B F96B 1.391(18) . ? B93B F94B 1.393(17) . ? B93C F95C 1.379(19) . ? B93C F97C 1.385(19) . ? B93C F96C 1.386(19) . ? B93C F94C 1.393(19) . ? B98A F100A 1.319(14) . ? B98A F101A 1.378(15) . ? B98A F99A 1.407(14) . ? B98A F102A 1.425(14) . ? B98B F102C 1.330(12) . ? B98B F101B 1.339(11) . ? B98B F99B 1.369(11) . ? B98B F100B 1.392(11) . ? B98B F100C 1.403(13) . ? B98B F99C 1.419(13) . ? B98B F101C 1.451(13) . ? B98B F102B 1.450(10) . ? C103 O104 1.207(5) . ? C103 C105 1.476(7) . ? C103 C106 1.477(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N22 176.10(12) . . ? N2 Fe1 N16 80.12(12) . . ? N22 Fe1 N16 103.32(12) . . ? N2 Fe1 N29 101.53(13) . . ? N22 Fe1 N29 80.37(13) . . ? N16 Fe1 N29 91.27(12) . . ? N2 Fe1 N36 98.59(12) . . ? N22 Fe1 N36 79.70(12) . . ? N16 Fe1 N36 89.63(12) . . ? N29 Fe1 N36 159.71(12) . . ? N2 Fe1 N9 80.30(12) . . ? N22 Fe1 N9 96.27(12) . . ? N16 Fe1 N9 160.41(12) . . ? N29 Fe1 N9 92.24(12) . . ? N36 Fe1 N9 93.67(12) . . ? C3 N2 C7 118.7(3) . . ? C3 N2 Fe1 120.5(2) . . ? C7 N2 Fe1 120.8(2) . . ? N2 C3 C4 120.0(3) . . ? N2 C3 N8 111.0(3) . . ? C4 C3 N8 128.9(3) . . ? N5 C4 C3 120.8(3) . . ? C4 N5 C6 119.1(3) . . ? N5 C6 C7 120.8(3) . . ? N2 C7 C6 120.6(3) . . ? N2 C7 N15 110.4(3) . . ? C6 C7 N15 129.0(3) . . ? C12 N8 N9 110.7(3) . . ? C12 N8 C3 132.6(3) . . ? N9 N8 C3 116.6(3) . . ? C10 N9 N8 105.4(3) . . ? C10 N9 Fe1 143.2(3) . . ? N8 N9 Fe1 111.4(2) . . ? N9 C10 C11 110.4(3) . . ? N9 C10 C13 123.9(3) . . ? C11 C10 C13 125.7(3) . . ? C12 C11 C10 108.0(3) . . ? C11 C12 N8 105.5(3) . . ? C11 C12 C14 130.8(3) . . ? N8 C12 C14 123.6(3) . . ? C19 N15 N16 110.8(3) . . ? C19 N15 C7 133.0(3) . . ? N16 N15 C7 116.1(3) . . ? C17 N16 N15 105.7(3) . . ? C17 N16 Fe1 141.5(3) . . ? N15 N16 Fe1 112.2(2) . . ? N16 C17 C18 109.7(3) . . ? N16 C17 C20 122.0(3) . . ? C18 C17 C20 128.4(3) . . ? C19 C18 C17 108.1(3) . . ? C18 C19 N15 105.7(3) . . ? C18 C19 C21 130.0(3) . . ? N15 C19 C21 124.3(3) . . ? C27 N22 C23 118.7(3) . . ? C27 N22 Fe1 120.7(2) . . ? C23 N22 Fe1 120.2(3) . . ? N22 C23 C24 119.7(4) . . ? N22 C23 N28 111.0(3) . . ? C24 C23 N28 129.3(3) . . ? N25 C24 C23 121.6(4) . . ? C26 N25 C24 118.5(3) . . ? N25 C26 C27 120.5(4) . . ? N22 C27 C26 121.0(3) . . ? N22 C27 N35 111.5(3) . . ? C26 C27 N35 127.5(4) . . ? C32 N28 C23 133.5(3) . . ? C32 N28 N29 110.4(3) . . ? C23 N28 N29 116.0(3) . . ? C30 N29 N28 105.5(3) . . ? C30 N29 Fe1 141.6(3) . . ? N28 N29 Fe1 111.9(2) . . ? N29 C30 C31 110.1(3) . . ? N29 C30 C33 122.1(3) . . ? C31 C30 C33 127.8(4) . . ? C32 C31 C30 107.7(4) . . ? C31 C32 N28 106.3(3) . . ? C31 C32 C34 129.7(4) . . ? N28 C32 C34 124.0(4) . . ? C39 N35 N36 111.1(3) . . ? C39 N35 C27 133.7(3) . . ? N36 N35 C27 114.8(3) . . ? C37 N36 N35 105.4(3) . . ? C37 N36 Fe1 142.2(3) . . ? N35 N36 Fe1 112.5(2) . . ? N36 C37 C38 109.8(3) . . ? N36 C37 C40 123.1(4) . . ? C38 C37 C40 127.0(3) . . ? C39 C38 C37 108.5(3) . . ? C38 C39 N35 105.3(3) . . ? C38 C39 C41 129.9(4) . . ? N35 C39 C41 124.8(3) . . ? N63 Fe42 N43 179.50(14) . . ? N63 Fe42 N50 100.14(12) . . ? N43 Fe42 N50 80.21(12) . . ? N63 Fe42 N70 80.35(13) . . ? N43 Fe42 N70 99.30(13) . . ? N50 Fe42 N70 90.60(12) . . ? N63 Fe42 N77 80.13(13) . . ? N43 Fe42 N77 100.21(13) . . ? N50 Fe42 N77 93.37(13) . . ? N70 Fe42 N77 160.47(12) . . ? N63 Fe42 N57 99.32(12) . . ? N43 Fe42 N57 80.33(12) . . ? N50 Fe42 N57 160.54(12) . . ? N70 Fe42 N57 92.45(12) . . ? N77 Fe42 N57 90.15(13) . . ? C48 N43 C44 118.7(3) . . ? C48 N43 Fe42 120.7(2) . . ? C44 N43 Fe42 120.5(2) . . ? N43 C44 C45 119.9(3) . . ? N43 C44 N49 111.1(3) . . ? C45 C44 N49 128.9(3) . . ? N46 C45 C44 120.5(4) . . ? C45 N46 C47 119.8(3) . . ? N46 C47 C48 119.8(4) . . ? N43 C48 C47 121.1(3) . . ? N43 C48 N56 111.1(3) . . ? C47 C48 N56 127.7(3) . . ? C53 N49 C44 134.0(3) . . ? C53 N49 N50 110.8(3) . . ? C44 N49 N50 115.1(3) . . ? C51 N50 N49 104.7(3) . . ? C51 N50 Fe42 142.6(3) . . ? N49 N50 Fe42 112.5(2) . . ? N50 C51 C52 110.5(3) . . ? N50 C51 C54 121.9(3) . . ? C52 C51 C54 127.6(4) . . ? C53 C52 C51 108.3(4) . . ? C52 C53 N49 105.6(3) . . ? C52 C53 C55 130.5(4) . . ? N49 C53 C55 123.8(3) . . ? C60 N56 N57 110.8(3) . . ? C60 N56 C48 133.4(3) . . ? N57 N56 C48 115.6(3) . . ? C58 N57 N56 105.2(3) . . ? C58 N57 Fe42 142.3(2) . . ? N56 N57 Fe42 112.0(2) . . ? N57 C58 C59 110.8(3) . . ? N57 C58 C61 120.9(3) . . ? C59 C58 C61 128.3(3) . . ? C60 C59 C58 107.3(3) . . ? C59 C60 N56 105.9(3) . . ? C59 C60 C62 130.0(4) . . ? N56 C60 C62 124.1(3) . . ? C64 N63 C68 119.1(3) . . ? C64 N63 Fe42 120.5(3) . . ? C68 N63 Fe42 120.4(3) . . ? N63 C64 C65 120.5(4) . . ? N63 C64 N69 111.1(3) . . ? C65 C64 N69 128.4(4) . . ? N66 C65 C64 120.6(4) . . ? C65 N66 C67 119.4(3) . . ? N66 C67 C68 120.6(4) . . ? N63 C68 N76 111.5(3) . . ? N63 C68 C67 119.8(4) . . ? N76 C68 C67 128.8(4) . . ? C73 N69 C64 133.5(3) . . ? C73 N69 N70 110.6(3) . . ? C64 N69 N70 115.8(3) . . ? C71 N70 N69 105.7(3) . . ? C71 N70 Fe42 142.4(3) . . ? N69 N70 Fe42 111.8(2) . . ? N70 C71 C72 109.8(3) . . ? N70 C71 C74 122.9(4) . . ? C72 C71 C74 127.3(4) . . ? C73 C72 C71 107.8(4) . . ? C72 C73 N69 106.1(3) . . ? C72 C73 C75 130.4(4) . . ? N69 C73 C75 123.4(3) . . ? C80 N76 C68 132.9(3) . . ? C80 N76 N77 110.8(3) . . ? C68 N76 N77 115.7(3) . . ? C78 N77 N76 105.3(3) . . ? C78 N77 Fe42 141.8(3) . . ? N76 N77 Fe42 112.3(2) . . ? N77 C78 C79 110.2(4) . . ? N77 C78 C81 121.8(4) . . ? C79 C78 C81 128.1(4) . . ? C80 C79 C78 108.0(4) . . ? C79 C80 N76 105.9(4) . . ? C79 C80 C82 129.8(4) . . ? N76 C80 C82 124.4(4) . . ? F86 B83 F85 110.8(4) . . ? F86 B83 F84 108.3(4) . . ? F85 B83 F84 110.2(4) . . ? F86 B83 F87 108.5(4) . . ? F85 B83 F87 109.7(4) . . ? F84 B83 F87 109.3(4) . . ? F91B B88 F90B 114.3(7) . . ? F91B B88 F92B 121.3(7) . . ? F90B B88 F92B 104.5(6) . . ? F92C B88 F90C 127.9(11) . . ? F89A B88 F92A 113.5(8) . . ? F89A B88 F91A 125.3(7) . . ? F92A B88 F91A 99.2(7) . . ? F92C B88 F91C 118.6(10) . . ? F90C B88 F91C 107.0(9) . . ? F89A B88 F90A 111.4(6) . . ? F92A B88 F90A 108.0(6) . . ? F91A B88 F90A 97.2(5) . . ? F92C B88 F89B 111.0(9) . . ? F91B B88 F89B 102.2(6) . . ? F90B B88 F89B 111.3(7) . . ? F92B B88 F89B 102.5(6) . . ? F90C B88 F89B 92.4(8) . . ? F91C B88 F89B 89.2(6) . . ? F97A B93A F96A 110.9(11) . . ? F97A B93A F95A 111.1(10) . . ? F96A B93A F95A 109.1(13) . . ? F97A B93A F94A 109.1(13) . . ? F96A B93A F94A 108.6(9) . . ? F95A B93A F94A 108.0(11) . . ? F97B B93B F95B 114.7(16) . . ? F97B B93B F96B 107.7(15) . . ? F95B B93B F96B 108.7(15) . . ? F97B B93B F94B 111.4(15) . . ? F95B B93B F94B 109.8(15) . . ? F96B B93B F94B 103.9(14) . . ? F95C B93C F97C 109.2(17) . . ? F95C B93C F96C 111.4(18) . . ? F97C B93C F96C 109.3(17) . . ? F95C B93C F94C 106.3(16) . . ? F97C B93C F94C 111.0(18) . . ? F96C B93C F94C 109.7(18) . . ? F100A B98A F101A 113.8(11) . . ? F100A B98A F99A 111.3(10) . . ? F101A B98A F99A 107.5(11) . . ? F100A B98A F102A 110.7(11) . . ? F101A B98A F102A 103.7(10) . . ? F99A B98A F102A 109.4(11) . . ? F101B B98B F99B 115.0(9) . . ? F101B B98B F100B 112.0(9) . . ? F99B B98B F100B 111.0(9) . . ? F102C B98B F100C 115.4(10) . . ? F102C B98B F99C 112.7(11) . . ? F100C B98B F99C 104.4(10) . . ? F102C B98B F101C 110.3(11) . . ? F100C B98B F101C 107.3(10) . . ? F99C B98B F101C 106.1(11) . . ? F101B B98B F102B 108.7(8) . . ? F99B B98B F102B 105.7(8) . . ? F100B B98B F102B 103.5(8) . . ? O104 C103 C105 121.5(5) . . ? O104 C103 C106 122.0(5) . . ? C105 C103 C106 116.4(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.560 _refine_diff_density_min -0.554 _refine_diff_density_rms 0.095 data_je28 _database_code_CSD 199771 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis[2,6-bis(3-{2,4,6-trimethylphenyl}pyrazol-1-yl)pyrazine]iron(II) ditetrafluoroborate pentakis-nitromethane solvate ; _chemical_name_common ; Bis(2,6-bis(3-(2,4,6-trimethylphenyl)pyrazol-1- yl)pyrazine)iron(ii) ditetrafluoroborate pentakis-nitromethane solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C56 H56 B2 F8 Fe N12, 2[B F4], 5[C H3 N O2]' _chemical_formula_sum 'C61 H71 B2 F8 Fe N17 O10' _chemical_formula_weight 1431.82 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 Hexagonal _symmetry_space_group_name_H-M 'P 31 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' 'x-y, -y, -z+2/3' '-x, -x+y, -z+1/3' 'y, x, -z' _cell_length_a 15.1838(1) _cell_length_b 15.1838(1) _cell_length_c 24.9779(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 4987.09(6) _cell_formula_units_Z 3 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 89750 _cell_measurement_theta_min 1.55 _cell_measurement_theta_max 27.47 _exptl_crystal_description Block _exptl_crystal_colour 'Dark brown' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8070 _exptl_absorpt_correction_T_max 0.9101 _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 The high value of Rint reflects only the moderate crystal quality, which is probably caused by the large amount of disorder present. ; _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 89750 _diffrn_reflns_av_R_equivalents 0.1573 _diffrn_reflns_av_sigmaI/netI 0.0455 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7623 _reflns_number_gt 7105 _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 of the structure contains half a complex dication, with Fe1 lying across the C~2~ axis at y, x, -z; one BF~4~^-^ anion lying on a general position; two molecules of nitromethane lying on general positions; and, one molecule of nitromethane lying across the C~2~ axis at -x, -x+y, 1/3-z. The BF~4~^-^ anion is disordered over three equally occupied orientations, labelled 'A', 'B' and 'C'. All B-F distances in the model were restrained to 1.39(2)\%A, and F...F distances within a given disorder orientation to 2.27(2)\%A. All the nitromethane molecules are also disordered. Molecule C41-O44 was modelled over three orientations: C41A-O44A (occupancy 0.50) C41B, N42A, O43B, O44B (occupancy 0.25, so that N42B has total occupancy 0.75) C41C-O44C (occupancy 0.25) The second whole molecule C45-O48 was modelled over two equally occupied orientations, labelled 'A' and 'B'. Finally, the half-molecule C49-O52 is also disordered over two orientations. One of these (C49A-O51A) is bisected by the C~2~ axis running through C49A and N50A, and has occupancy 0.50. The other partial molecule, C49B-O52B, is not bisected by the C~2~ axis but is disordered across it, and has occupany 0.25. All disordered C-N bonds were restrained to 1.43(2)\%A, N-O bonds to 1.24(2)\%A, O...O distances to 2.16(2)\%A and C...O distances to 2.29(2)\%A. All wholly occupied non-H atoms were refined anisotropically. All H atoms were placed in calculated positions and refined using a riding model, except that the torsions of the disordered solvent methyl groups were not refined. ; _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^)+(0.0948P)^2^+3.0942P] 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 0.0051(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(19) _refine_ls_number_reflns 7623 _refine_ls_number_parameters 482 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0636 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1603 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.092 _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 Fe1 Fe 0.31434(3) 0.31434(3) 0.0000 0.01962(14) Uani 1 2 d S . . N2 N 0.36245(18) 0.26580(18) 0.05572(9) 0.0234(4) Uani 1 1 d . . . C3 C 0.4155(2) 0.3263(2) 0.09618(10) 0.0259(5) Uani 1 1 d . . . C4 C 0.4512(2) 0.2908(2) 0.13740(11) 0.0310(6) Uani 1 1 d . . . H4 H 0.4908 0.3354 0.1654 0.037 Uiso 1 1 calc R . . N5 N 0.4302(2) 0.1948(2) 0.13771(10) 0.0345(6) Uani 1 1 d . . . C6 C 0.3754(3) 0.1327(3) 0.09797(12) 0.0351(7) Uani 1 1 d . . . H6 H 0.3587 0.0635 0.0984 0.042 Uiso 1 1 calc R . . C7 C 0.3425(2) 0.1698(2) 0.05570(11) 0.0271(5) Uani 1 1 d . . . N8 N 0.42700(19) 0.42298(19) 0.09097(9) 0.0277(5) Uani 1 1 d . . . N9 N 0.38084(18) 0.43856(16) 0.04678(8) 0.0237(4) Uani 1 1 d . . . C10 C 0.4042(2) 0.5358(2) 0.05031(11) 0.0265(6) Uani 1 1 d . . . C11 C 0.4632(2) 0.5809(2) 0.09656(11) 0.0324(6) Uani 1 1 d . . . H11 H 0.4890 0.6489 0.1083 0.039 Uiso 1 1 calc R . . C12 C 0.4760(3) 0.5082(2) 0.12108(12) 0.0341(6) Uani 1 1 d . . . H12 H 0.5124 0.5158 0.1533 0.041 Uiso 1 1 calc R . . C13 C 0.3727(2) 0.5841(2) 0.00824(11) 0.0270(6) Uani 1 1 d . . . C14 C 0.4432(2) 0.6451(2) -0.03125(12) 0.0312(6) Uani 1 1 d . . . C15 C 0.4112(3) 0.6833(2) -0.07295(13) 0.0395(7) Uani 1 1 d . . . H15 H 0.4584 0.7238 -0.0998 0.047 Uiso 1 1 calc R . . C16 C 0.3117(3) 0.6630(3) -0.07587(16) 0.0490(9) Uani 1 1 d . . . C17 C 0.2455(3) 0.6085(3) -0.03534(17) 0.0476(9) Uani 1 1 d . . . H17 H 0.1783 0.5977 -0.0364 0.057 Uiso 1 1 calc R . . C18 C 0.2735(2) 0.5682(2) 0.00738(15) 0.0382(7) Uani 1 1 d . . . C19 C 0.5526(3) 0.6722(3) -0.02977(15) 0.0421(8) Uani 1 1 d . . . H19A H 0.5882 0.7146 -0.0608 0.063 Uiso 1 1 calc R . . H19B H 0.5569 0.6099 -0.0307 0.063 Uiso 1 1 calc R . . H19C H 0.5842 0.7099 0.0032 0.063 Uiso 1 1 calc R . . C20 C 0.2781(5) 0.7022(4) -0.1227(2) 0.0797(17) Uani 1 1 d . . . H20A H 0.2954 0.7726 -0.1158 0.120 Uiso 1 1 calc R . . H20B H 0.2044 0.6597 -0.1274 0.120 Uiso 1 1 calc R . . H20C H 0.3128 0.6997 -0.1552 0.120 Uiso 1 1 calc R . . C21 C 0.1999(3) 0.5137(3) 0.05237(18) 0.0520(10) Uani 1 1 d . . . H21A H 0.1913 0.4457 0.0567 0.078 Uiso 1 1 calc R . . H21B H 0.1341 0.5078 0.0440 0.078 Uiso 1 1 calc R . . H21C H 0.2265 0.5523 0.0856 0.078 Uiso 1 1 calc R . . N22 N 0.2885(2) 0.11775(19) 0.01020(10) 0.0305(5) Uani 1 1 d . . . N23 N 0.26535(17) 0.17212(16) -0.02618(9) 0.0245(4) Uani 1 1 d . . . C24 C 0.2126(2) 0.10557(19) -0.06511(10) 0.0274(5) Uani 1 1 d . . . C25 C 0.2026(3) 0.0100(2) -0.05373(14) 0.0377(7) Uani 1 1 d . . . H25 H 0.1692 -0.0495 -0.0752 0.045 Uiso 1 1 calc R . . C26 C 0.2501(3) 0.0197(2) -0.00590(14) 0.0387(7) Uani 1 1 d . . . H26 H 0.2554 -0.0321 0.0126 0.046 Uiso 1 1 calc R . . C27 C 0.1706(2) 0.1341(2) -0.11169(11) 0.0268(6) Uani 1 1 d . . . C28 C 0.2311(2) 0.1853(2) -0.15553(12) 0.0334(7) Uani 1 1 d . . . C29 C 0.1901(3) 0.2154(3) -0.19756(13) 0.0438(8) Uani 1 1 d . . . H29 H 0.2316 0.2507 -0.2274 0.053 Uiso 1 1 calc R . . C30 C 0.0907(3) 0.1943(3) -0.19613(14) 0.0477(9) Uani 1 1 d . . . C31 C 0.0292(3) 0.1375(3) -0.15378(15) 0.0453(8) Uani 1 1 d . . . H31 H -0.0405 0.1192 -0.1536 0.054 Uiso 1 1 calc R . . C32 C 0.0672(2) 0.1068(3) -0.11170(12) 0.0351(7) Uani 1 1 d . . . C33 C 0.3386(3) 0.2071(4) -0.15999(15) 0.0522(10) Uani 1 1 d . . . H33A H 0.3804 0.2570 -0.1327 0.078 Uiso 1 1 calc R . . H33B H 0.3651 0.2345 -0.1956 0.078 Uiso 1 1 calc R . . H33C H 0.3404 0.1441 -0.1545 0.078 Uiso 1 1 calc R . . C34 C 0.0483(5) 0.2327(4) -0.2404(2) 0.0771(16) Uani 1 1 d . . . H34A H -0.0230 0.1820 -0.2472 0.116 Uiso 1 1 calc R . . H34B H 0.0879 0.2441 -0.2732 0.116 Uiso 1 1 calc R . . H34C H 0.0530 0.2968 -0.2291 0.116 Uiso 1 1 calc R . . C35 C -0.0031(3) 0.0425(4) -0.06745(16) 0.0583(11) Uani 1 1 d . . . H35A H -0.0048 -0.0228 -0.0660 0.088 Uiso 1 1 calc R . . H35B H -0.0718 0.0305 -0.0744 0.088 Uiso 1 1 calc R . . H35C H 0.0214 0.0778 -0.0332 0.088 Uiso 1 1 calc R . . B36A B 0.2267(10) 0.8273(11) 0.1364(5) 0.035(6) Uiso 0.33 1 d PD A 1 F37A F 0.3188(6) 0.9009(6) 0.1569(3) 0.0466(18) Uiso 0.33 1 d PD A 1 F38A F 0.2488(8) 0.7472(7) 0.1238(3) 0.0537(18) Uiso 0.33 1 d PD A 1 F39A F 0.1448(7) 0.7927(7) 0.1690(3) 0.051(2) Uiso 0.33 1 d PD A 1 F40A F 0.1986(6) 0.8564(6) 0.0898(3) 0.0394(19) Uiso 0.33 1 d PD A 1 B36B B 0.2475(13) 0.8257(11) 0.1336(5) 0.040(7) Uiso 0.33 1 d PD B 2 F37B F 0.3018(7) 0.9172(6) 0.1660(3) 0.060(3) Uiso 0.33 1 d PD B 2 F38B F 0.3089(10) 0.7869(10) 0.1264(5) 0.101(3) Uiso 0.33 1 d PD B 2 F39B F 0.1612(7) 0.7666(8) 0.1627(4) 0.076(3) Uiso 0.33 1 d PD B 2 F40B F 0.2309(7) 0.8599(7) 0.0840(3) 0.0454(19) Uiso 0.33 1 d PD B 2 B36C B 0.2334(14) 0.8209(13) 0.1353(7) 0.055(15) Uiso 0.33 1 d PD C 3 F37C F 0.3355(7) 0.8692(8) 0.1495(4) 0.079(3) Uiso 0.33 1 d PD C 3 F38C F 0.2070(8) 0.7245(7) 0.1186(4) 0.073(3) Uiso 0.33 1 d PD C 3 F39C F 0.1727(8) 0.8110(8) 0.1799(4) 0.067(3) Uiso 0.33 1 d PD C 3 F40C F 0.2239(9) 0.8803(7) 0.0959(4) 0.053(3) Uiso 0.33 1 d PD C 3 C41A C -0.0268(9) 0.7105(10) 0.0597(4) 0.076(3) Uiso 0.50 1 d PD D 1 H41A H -0.0753 0.6425 0.0731 0.114 Uiso 0.50 1 calc PR D 1 H41B H -0.0639 0.7402 0.0425 0.114 Uiso 0.50 1 calc PR D 1 H41C H 0.0134 0.7537 0.0896 0.114 Uiso 0.50 1 calc PR D 1 N42A N 0.0443(5) 0.7026(5) 0.0187(3) 0.0798(17) Uiso 0.75 1 d PD . . O43A O 0.0593(8) 0.6335(7) 0.0260(4) 0.079(2) Uiso 0.50 1 d PD D 1 O44A O 0.0741(9) 0.7710(8) -0.0122(4) 0.109(3) Uiso 0.50 1 d PD D 1 C41B C -0.029(3) 0.736(3) 0.0192(19) 0.18(2) Uiso 0.25 1 d PD D 2 H41D H -0.0149 0.7820 0.0496 0.275 Uiso 0.25 1 calc PR D 2 H41E H -0.0971 0.6770 0.0227 0.275 Uiso 0.25 1 calc PR D 2 H41F H -0.0237 0.7719 -0.0142 0.275 Uiso 0.25 1 calc PR D 2 O43B O 0.0197(17) 0.6121(12) 0.0249(8) 0.093(6) Uiso 0.25 1 d PD D 2 O44B O 0.1137(7) 0.7576(8) -0.0192(4) 0.038(2) Uiso 0.25 1 d PD D 2 C41C C -0.0095(13) 0.7894(13) -0.0025(6) 0.051(4) Uiso 0.25 1 d PD E 3 H41G H 0.0180 0.8491 0.0209 0.076 Uiso 0.25 1 calc PR E 3 H41H H -0.0840 0.7527 -0.0005 0.076 Uiso 0.25 1 calc PR E 3 H41I H 0.0120 0.8112 -0.0394 0.076 Uiso 0.25 1 calc PR E 3 N42C N 0.0236(14) 0.7309(13) 0.0127(6) 0.066(4) Uiso 0.25 1 d PD E 3 O43C O -0.0024(19) 0.6773(18) 0.0566(8) 0.133(8) Uiso 0.25 1 d PD E 3 O44C O 0.089(2) 0.718(3) -0.0155(11) 0.156(12) Uiso 0.25 1 d PD E 3 C45A C 0.4134(8) 0.8741(10) 0.0149(4) 0.063(3) Uiso 0.50 1 d PD F 1 H45A H 0.4218 0.8281 -0.0093 0.094 Uiso 0.50 1 calc PR F 1 H45B H 0.4217 0.9332 -0.0052 0.094 Uiso 0.50 1 calc PR F 1 H45C H 0.3453 0.8384 0.0309 0.094 Uiso 0.50 1 calc PR F 1 N46A N 0.4893(7) 0.9078(7) 0.0569(3) 0.061(2) Uiso 0.50 1 d PD F 1 O47A O 0.5095(6) 0.9805(5) 0.0840(3) 0.0686(17) Uiso 0.50 1 d PD F 1 O48A O 0.5337(7) 0.8582(8) 0.0616(4) 0.092(3) Uiso 0.50 1 d PD F 1 C45B C 0.3891(9) 0.8445(9) 0.0199(4) 0.066(3) Uiso 0.50 1 d PD G 2 H45D H 0.3226 0.8174 0.0372 0.099 Uiso 0.50 1 calc PR G 2 H45E H 0.4041 0.7894 0.0146 0.099 Uiso 0.50 1 calc PR G 2 H45F H 0.3880 0.8738 -0.0149 0.099 Uiso 0.50 1 calc PR G 2 N46B N 0.4643(6) 0.9200(6) 0.0524(3) 0.0489(17) Uiso 0.50 1 d PD G 2 O47B O 0.4686(7) 0.9979(7) 0.0652(4) 0.091(2) Uiso 0.50 1 d PD G 2 O48B O 0.5310(8) 0.9023(9) 0.0740(4) 0.109(3) Uiso 0.50 1 d PD G 2 C49A C 0.0000 0.5356(9) 0.1667 0.090(6) Uiso 0.50 2 d SPD H 1 H49A H -0.0207 0.5468 0.2020 0.135 Uiso 0.25 1 calc PR H 1 H49B H -0.0478 0.5333 0.1396 0.135 Uiso 0.25 1 calc PR H 1 H49C H 0.0685 0.5914 0.1584 0.135 Uiso 0.25 1 calc PR H 1 N50A N 0.0000 0.4409(8) 0.1667 0.054(3) Uiso 0.50 2 d SPD . 1 O51A O -0.0213(7) 0.3914(7) 0.1251(3) 0.093(2) Uiso 0.50 1 d PD I 1 C49B C -0.016(2) 0.5179(17) 0.1475(9) 0.080(6) Uiso 0.25 1 d PD J 2 H49D H -0.0395 0.4814 0.1135 0.120 Uiso 0.25 1 calc PR J 2 H49E H 0.0434 0.5852 0.1411 0.120 Uiso 0.25 1 calc PR J 2 H49F H -0.0705 0.5257 0.1636 0.120 Uiso 0.25 1 calc PR J 2 N50B N 0.0123(10) 0.4598(10) 0.1842(6) 0.045(3) Uiso 0.25 1 d PD . 2 O51B O 0.0000 0.3793(9) 0.1667 0.105(4) Uiso 0.50 2 d SPD . 2 O52B O 0.0420(13) 0.4881(13) 0.2284(6) 0.087(4) Uiso 0.25 1 d PD . 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 0.02038(19) 0.02038(19) 0.0181(2) 0.00076(9) -0.00076(9) 0.01020(19) N2 0.0217(10) 0.0265(11) 0.0215(10) 0.0026(9) 0.0007(8) 0.0117(8) C3 0.0230(12) 0.0317(13) 0.0213(12) 0.0024(10) 0.0014(10) 0.0124(10) C4 0.0277(13) 0.0401(16) 0.0251(13) 0.0019(11) -0.0031(11) 0.0169(12) N5 0.0328(13) 0.0419(14) 0.0306(12) 0.0111(11) 0.0003(10) 0.0200(11) C6 0.0377(16) 0.0353(16) 0.0357(16) 0.0087(13) -0.0012(12) 0.0208(14) C7 0.0280(13) 0.0255(13) 0.0280(13) 0.0058(10) 0.0011(11) 0.0135(11) N8 0.0297(12) 0.0317(12) 0.0222(11) -0.0015(9) -0.0064(9) 0.0157(10) N9 0.0257(11) 0.0264(10) 0.0195(9) -0.0007(7) -0.0017(8) 0.0134(9) C10 0.0266(13) 0.0252(13) 0.0252(12) -0.0008(10) 0.0015(10) 0.0111(10) C11 0.0332(15) 0.0308(13) 0.0290(13) -0.0075(10) -0.0062(11) 0.0129(12) C12 0.0368(16) 0.0370(16) 0.0235(13) -0.0059(12) -0.0069(12) 0.0147(13) C13 0.0317(14) 0.0235(12) 0.0286(13) -0.0062(10) -0.0056(11) 0.0159(11) C14 0.0392(16) 0.0288(14) 0.0289(14) -0.0023(11) 0.0000(12) 0.0195(13) C15 0.057(2) 0.0318(15) 0.0338(16) -0.0029(12) -0.0048(14) 0.0249(15) C16 0.064(2) 0.0325(17) 0.054(2) -0.0050(15) -0.0271(18) 0.0267(17) C17 0.0362(17) 0.0362(18) 0.074(3) -0.0066(17) -0.0201(17) 0.0209(15) C18 0.0296(15) 0.0276(15) 0.056(2) -0.0067(13) -0.0068(14) 0.0134(13) C19 0.0425(19) 0.0449(18) 0.0452(18) 0.0113(15) 0.0115(15) 0.0264(16) C20 0.100(4) 0.067(3) 0.081(3) -0.002(3) -0.048(3) 0.049(3) C21 0.0351(18) 0.040(2) 0.082(3) 0.0053(18) 0.0119(18) 0.0196(16) N22 0.0374(13) 0.0254(11) 0.0298(12) 0.0034(9) -0.0035(10) 0.0165(10) N23 0.0278(11) 0.0229(10) 0.0241(10) 0.0028(8) 0.0000(8) 0.0135(9) C24 0.0280(13) 0.0248(12) 0.0265(12) -0.0016(9) 0.0008(11) 0.0111(11) C25 0.0463(18) 0.0247(13) 0.0418(17) -0.0051(12) -0.0071(14) 0.0175(13) C26 0.050(2) 0.0240(14) 0.0450(18) 0.0000(12) -0.0072(15) 0.0211(14) C27 0.0281(13) 0.0215(12) 0.0284(13) -0.0052(10) -0.0042(11) 0.0106(11) C28 0.0341(16) 0.0309(14) 0.0287(14) -0.0046(11) -0.0010(11) 0.0114(12) C29 0.062(2) 0.0289(15) 0.0308(15) -0.0019(12) -0.0066(15) 0.0155(15) C30 0.066(2) 0.0396(18) 0.0451(18) -0.0102(15) -0.0247(16) 0.0318(18) C31 0.0467(19) 0.055(2) 0.0444(18) -0.0212(16) -0.0184(15) 0.0335(18) C32 0.0329(15) 0.0384(16) 0.0327(15) -0.0120(13) -0.0069(12) 0.0168(13) C33 0.0383(18) 0.068(3) 0.0376(18) -0.0060(17) 0.0049(14) 0.0172(18) C34 0.118(5) 0.068(3) 0.067(3) -0.008(2) -0.044(3) 0.062(3) C35 0.0289(16) 0.080(3) 0.047(2) -0.0171(19) 0.0015(15) 0.0127(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.885(2) . ? Fe1 N23 2.009(2) . ? Fe1 N9 2.009(2) . ? N2 C3 1.332(4) . ? N2 C7 1.333(4) . ? C3 C4 1.392(4) . ? C3 N8 1.395(4) . ? C4 N5 1.328(4) . ? N5 C6 1.334(4) . ? C6 C7 1.400(4) . ? C7 N22 1.393(4) . ? N8 C12 1.354(4) . ? N8 N9 1.390(3) . ? N9 C10 1.338(4) . ? C10 C11 1.412(4) . ? C10 C13 1.489(4) . ? C11 C12 1.358(4) . ? C13 C18 1.401(4) . ? C13 C14 1.409(4) . ? C14 C15 1.392(4) . ? C14 C19 1.499(5) . ? C15 C16 1.385(6) . ? C16 C17 1.374(6) . ? C16 C20 1.511(5) . ? C17 C18 1.398(5) . ? C18 C21 1.507(5) . ? N22 C26 1.360(4) . ? N22 N23 1.386(3) . ? N23 C24 1.341(3) . ? C24 C25 1.410(4) . ? C24 C27 1.492(4) . ? C25 C26 1.365(5) . ? C27 C28 1.390(4) . ? C27 C32 1.409(4) . ? C28 C29 1.408(5) . ? C28 C33 1.498(5) . ? C29 C30 1.379(6) . ? C30 C31 1.389(6) . ? C30 C34 1.534(5) . ? C31 C32 1.386(5) . ? C32 C35 1.507(5) . ? B36A F39A 1.354(14) . ? B36A F37A 1.380(13) . ? B36A F40A 1.385(13) . ? B36A F38A 1.447(15) . ? B36B F38B 1.341(15) . ? B36B F39B 1.370(15) . ? B36B F40B 1.413(13) . ? B36B F37B 1.457(14) . ? B36C F38C 1.374(17) . ? B36C F37C 1.390(17) . ? B36C F40C 1.390(16) . ? B36C F39C 1.405(17) . ? C41A N42A 1.535(11) . ? N42A O44A 1.187(10) . ? N42A O43A 1.194(9) . ? N42A O43B 1.240(14) . ? N42A O44B 1.351(11) . ? N42A C41B 1.429(17) . ? C41C N42C 1.277(17) . ? N42C O43C 1.304(16) . ? N42C O44C 1.310(17) . ? C45A N46A 1.450(12) . ? N46A O47A 1.196(10) . ? N46A O48A 1.242(12) . ? C45B N46B 1.404(11) . ? N46B O47B 1.195(10) . ? N46B O48B 1.289(11) . ? C49A N50A 1.439(15) . ? N50A O51A 1.225(9) . ? C49B N50B 1.477(15) . ? N50B O52B 1.189(14) . ? N50B O51B 1.222(14) . ? 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 179.80(17) . 6 ? N2 Fe1 N23 99.77(9) . 6 ? N2 Fe1 N23 80.08(9) . . ? N23 Fe1 N23 87.49(13) 6 . ? N2 Fe1 N9 80.01(9) . . ? N23 Fe1 N9 160.09(9) . . ? N2 Fe1 N9 100.13(10) . 6 ? N23 Fe1 N9 95.79(9) . 6 ? N9 Fe1 N9 87.80(13) . 6 ? C3 N2 C7 118.9(2) . . ? C3 N2 Fe1 120.62(19) . . ? C7 N2 Fe1 120.49(19) . . ? N2 C3 C4 120.8(3) . . ? N2 C3 N8 111.7(2) . . ? C4 C3 N8 127.5(3) . . ? N5 C4 C3 120.2(3) . . ? C4 N5 C6 119.6(2) . . ? N5 C6 C7 119.9(3) . . ? N2 C7 N22 111.5(2) . . ? N2 C7 C6 120.5(3) . . ? N22 C7 C6 127.9(3) . . ? C12 N8 N9 111.2(2) . . ? C12 N8 C3 132.4(3) . . ? N9 N8 C3 116.4(2) . . ? C10 N9 N8 104.9(2) . . ? C10 N9 Fe1 143.66(19) . . ? N8 N9 Fe1 111.20(17) . . ? N9 C10 C11 110.0(2) . . ? N9 C10 C13 121.6(2) . . ? C11 C10 C13 128.4(3) . . ? C12 C11 C10 106.8(3) . . ? N8 C12 C11 107.0(3) . . ? C18 C13 C14 119.9(3) . . ? C18 C13 C10 120.5(3) . . ? C14 C13 C10 119.5(3) . . ? C15 C14 C13 119.3(3) . . ? C15 C14 C19 118.3(3) . . ? C13 C14 C19 122.4(3) . . ? C16 C15 C14 121.1(3) . . ? C17 C16 C15 118.9(3) . . ? C17 C16 C20 121.2(4) . . ? C15 C16 C20 119.9(4) . . ? C16 C17 C18 122.3(3) . . ? C17 C18 C13 118.2(3) . . ? C17 C18 C21 120.3(3) . . ? C13 C18 C21 121.4(3) . . ? C26 N22 N23 111.2(2) . . ? C26 N22 C7 132.1(3) . . ? N23 N22 C7 116.8(2) . . ? C24 N23 N22 105.1(2) . . ? C24 N23 Fe1 143.75(19) . . ? N22 N23 Fe1 111.03(17) . . ? N23 C24 C25 110.2(3) . . ? N23 C24 C27 121.8(2) . . ? C25 C24 C27 127.9(2) . . ? C26 C25 C24 106.7(3) . . ? N22 C26 C25 106.8(3) . . ? C28 C27 C32 119.5(3) . . ? C28 C27 C24 121.1(3) . . ? C32 C27 C24 119.3(3) . . ? C27 C28 C29 119.5(3) . . ? C27 C28 C33 121.7(3) . . ? C29 C28 C33 118.8(3) . . ? C30 C29 C28 121.1(3) . . ? C29 C30 C31 118.8(3) . . ? C29 C30 C34 120.8(4) . . ? C31 C30 C34 120.4(4) . . ? C32 C31 C30 121.6(3) . . ? C31 C32 C27 119.3(3) . . ? C31 C32 C35 119.7(3) . . ? C27 C32 C35 121.0(3) . . ? F39A B36A F37A 116.9(11) . . ? F39A B36A F40A 105.0(10) . . ? F37A B36A F40A 113.7(10) . . ? F39A B36A F38A 111.0(11) . . ? F37A B36A F38A 101.2(11) . . ? F40A B36A F38A 108.9(10) . . ? F38B B36B F39B 115.5(12) . . ? F38B B36B F40B 109.6(11) . . ? F39B B36B F40B 114.8(12) . . ? F38B B36B F37B 107.9(12) . . ? F39B B36B F37B 103.2(10) . . ? F40B B36B F37B 105.0(10) . . ? F38C B36C F37C 107.1(13) . . ? F38C B36C F40C 114.0(13) . . ? F37C B36C F40C 106.8(13) . . ? F38C B36C F39C 107.5(13) . . ? F37C B36C F39C 110.7(13) . . ? F40C B36C F39C 110.8(13) . . ? O44A N42A O43A 135.4(10) . . ? O43B N42A O44B 118.8(11) . . ? O43B N42A C41B 122.3(17) . . ? O44B N42A C41B 106.8(14) . . ? O44A N42A C41A 109.9(9) . . ? O43A N42A C41A 114.7(8) . . ? C41C N42C O43C 125.6(16) . . ? C41C N42C O44C 122.4(16) . . ? O43C N42C O44C 112.0(17) . . ? O47A N46A O48A 122.6(10) . . ? O47A N46A C45A 121.8(10) . . ? O48A N46A C45A 115.5(9) . . ? O47B N46B O48B 115.8(9) . . ? O47B N46B C45B 125.7(9) . . ? O48B N46B C45B 118.3(9) . . ? O51A N50A O51A 122.5(13) 5 . ? O51A N50A C49A 118.7(7) . . ? O52B N50B O51B 122.4(13) . . ? O52B N50B C49B 122.1(14) . . ? O51B N50B C49B 115.5(12) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.720 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.099