# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fepitpf6_10klightoff_revsep2013 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 F12 Fe N8 P2' _chemical_formula_weight 934.58 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.0765(8) _cell_length_b 16.9570(10) _cell_length_c 17.9940(10) _cell_angle_alpha 90.00 _cell_angle_beta 104.200(7) _cell_angle_gamma 90.00 _cell_volume 3868.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 10(2) _cell_measurement_reflns_used 4776 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 27.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.571 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 10(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16851 _diffrn_reflns_av_R_equivalents 0.0478 _diffrn_reflns_av_sigmaI/netI 0.1277 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8242 _reflns_number_gt 4673 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^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 8242 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0964 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1014 _refine_ls_wR_factor_gt 0.0943 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _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 N100 N 0.2843(3) 0.48449(17) -0.11293(18) 0.0291(8) Uani 1 1 d . . . C100 C 0.3539(3) 0.4516(2) -0.0752(2) 0.0181(8) Uani 1 1 d . . . C101 C 0.4427(3) 0.4091(2) -0.0268(2) 0.0261(9) Uani 1 1 d . . . H10A H 0.5081 0.4248 -0.0402 0.029(11) Uiso 1 1 calc R . . H10B H 0.4320 0.3522 -0.0349 0.068(15) Uiso 1 1 calc R . . H10C H 0.4478 0.4217 0.0271 0.041(12) Uiso 1 1 calc R . . C102 C 0.4968(3) 0.11415(18) 0.21368(19) 0.0153(8) Uani 1 1 d . . . C103 C 0.6027(3) 0.09178(19) 0.23275(19) 0.0166(8) Uani 1 1 d . . . H103 H 0.6500 0.1143 0.2762 0.020 Uiso 1 1 calc R . . C104 C 0.6392(3) 0.03646(19) 0.1882(2) 0.0192(8) Uani 1 1 d . . . H104 H 0.7114 0.0215 0.2012 0.023 Uiso 1 1 calc R . . C105 C 0.5706(3) 0.00315(19) 0.1248(2) 0.0187(9) Uani 1 1 d . . . H105 H 0.5957 -0.0348 0.0946 0.022 Uiso 1 1 calc R . . C106 C 0.4663(3) 0.02509(19) 0.1056(2) 0.0187(9) Uani 1 1 d . . . H106 H 0.4193 0.0029 0.0617 0.022 Uiso 1 1 calc R . . C107 C 0.4293(3) 0.08020(19) 0.15080(19) 0.0164(8) Uani 1 1 d . . . H107 H 0.3568 0.0944 0.1380 0.020 Uiso 1 1 calc R . . C108 C 0.4573(3) 0.1751(2) 0.26081(19) 0.0211(9) Uani 1 1 d . . . H10D H 0.3812 0.1823 0.2406 0.032 Uiso 1 1 calc R . . H10E H 0.4936 0.2253 0.2583 0.032 Uiso 1 1 calc R . . H10F H 0.4715 0.1574 0.3142 0.032 Uiso 1 1 calc R . . P1 P 0.27508(8) 0.20071(5) -0.07454(5) 0.0132(2) Uani 1 1 d . . . F1 F 0.30944(15) 0.12425(10) -0.02282(10) 0.0174(5) Uani 1 1 d . . . F2 F 0.39354(15) 0.20865(10) -0.08547(10) 0.0159(5) Uani 1 1 d . . . F3 F 0.24352(15) 0.14655(10) -0.14962(10) 0.0168(5) Uani 1 1 d . . . F4 F 0.24217(16) 0.27838(10) -0.12538(11) 0.0183(5) Uani 1 1 d . . . F5 F 0.15787(15) 0.19324(10) -0.06273(10) 0.0164(5) Uani 1 1 d . . . F6 F 0.30792(15) 0.25501(11) 0.00091(10) 0.0185(5) Uani 1 1 d . . . P2 P 0.34791(8) 0.45123(5) 0.20401(5) 0.0142(2) Uani 1 1 d . . . F7 F 0.31120(16) 0.54181(10) 0.19687(10) 0.0186(5) Uani 1 1 d . . . F8 F 0.43652(16) 0.47237(11) 0.28002(10) 0.0208(5) Uani 1 1 d . . . F9 F 0.43070(16) 0.46954(10) 0.15352(11) 0.0202(5) Uani 1 1 d . . . F10 F 0.38351(16) 0.36086(10) 0.21182(11) 0.0187(5) Uani 1 1 d . . . F11 F 0.25947(16) 0.43072(11) 0.12764(10) 0.0218(5) Uani 1 1 d . . . F12 F 0.26519(15) 0.43368(10) 0.25455(10) 0.0173(5) Uani 1 1 d . . . Fe1 Fe -0.08254(4) 0.24552(3) 0.10874(3) 0.01092(12) Uani 1 1 d . . . N1 N -0.0561(2) 0.32583(15) 0.02719(15) 0.0130(6) Uani 1 1 d . . . N2 N -0.2439(2) 0.26120(15) 0.10196(15) 0.0119(6) Uani 1 1 d . . . N3 N -0.0981(2) 0.13979(15) 0.04705(15) 0.0106(6) Uani 1 1 d . . . N4 N 0.0956(2) 0.25608(15) 0.29253(15) 0.0150(6) Uani 1 1 d . . . N5 N -0.0735(2) 0.33738(15) 0.17635(15) 0.0128(6) Uani 1 1 d . . . N6 N -0.0888(2) 0.17073(15) 0.19194(15) 0.0111(6) Uani 1 1 d . . . N7 N 0.0703(2) 0.23392(15) 0.12495(15) 0.0132(7) Uani 1 1 d . . . C1 C 0.1778(3) 0.22973(18) 0.25857(18) 0.0127(8) Uani 1 1 d . . . H1A H 0.2258 0.1952 0.2958 0.015 Uiso 1 1 calc R . . H1B H 0.2189 0.2763 0.2498 0.015 Uiso 1 1 calc R . . C2 C 0.1419(3) 0.18483(19) 0.18280(18) 0.0150(8) Uani 1 1 d . . . H2A H 0.2043 0.1700 0.1639 0.018 Uiso 1 1 calc R . . H2B H 0.1052 0.1358 0.1913 0.018 Uiso 1 1 calc R . . C3 C 0.0708(3) 0.33913(18) 0.29481(18) 0.0135(8) Uani 1 1 d . . . H3A H 0.1364 0.3677 0.3194 0.016 Uiso 1 1 calc R . . H3B H 0.0211 0.3459 0.3279 0.016 Uiso 1 1 calc R . . C4 C 0.0226(3) 0.37815(19) 0.21727(18) 0.0142(8) Uani 1 1 d . . . H4A H 0.0057 0.4339 0.2256 0.017 Uiso 1 1 calc R . . H4B H 0.0747 0.3774 0.1856 0.017 Uiso 1 1 calc R . . C5 C 0.0317(3) 0.19839(18) 0.31914(19) 0.0134(8) Uani 1 1 d . . . H5A H 0.0309 0.2118 0.3725 0.016 Uiso 1 1 calc R . . H5B H 0.0665 0.1464 0.3203 0.016 Uiso 1 1 calc R . . C6 C -0.0819(3) 0.19022(19) 0.27274(17) 0.0135(8) Uani 1 1 d . . . H6A H -0.1172 0.1483 0.2957 0.016 Uiso 1 1 calc R . . H6B H -0.1198 0.2403 0.2753 0.016 Uiso 1 1 calc R . . C7 C -0.0994(3) 0.09902(19) 0.17245(19) 0.0122(8) Uani 1 1 d . . . H7 H -0.1035 0.0597 0.2092 0.015 Uiso 1 1 calc R . . C8 C -0.1053(3) 0.07725(19) 0.09386(18) 0.0127(8) Uani 1 1 d . . . C9 C -0.1236(3) 0.00109(19) 0.06897(19) 0.0135(8) Uani 1 1 d . . . H9 H -0.1283 -0.0399 0.1040 0.016 Uiso 1 1 calc R . . C10 C -0.1352(3) -0.01525(19) -0.00764(19) 0.0149(8) Uani 1 1 d . . . H10 H -0.1486 -0.0674 -0.0268 0.018 Uiso 1 1 calc R . . C11 C -0.1268(3) 0.04619(19) -0.05534(19) 0.0139(8) Uani 1 1 d . . . H11 H -0.1346 0.0362 -0.1084 0.017 Uiso 1 1 calc R . . C12 C -0.1071(3) 0.12278(19) -0.02795(19) 0.0131(8) Uani 1 1 d . . . C13 C -0.0992(3) 0.18713(18) -0.08304(18) 0.0134(8) Uani 1 1 d . . . H13A H -0.0290 0.2112 -0.0680 0.020 Uiso 1 1 calc R . . H13B H -0.1529 0.2273 -0.0825 0.020 Uiso 1 1 calc R . . H13C H -0.1105 0.1651 -0.1348 0.020 Uiso 1 1 calc R . . C14 C -0.1602(3) 0.36047(18) 0.18819(18) 0.0127(8) Uani 1 1 d . . . H14 H -0.1623 0.4049 0.2199 0.015 Uiso 1 1 calc R . . C15 C -0.2560(3) 0.31856(19) 0.15294(19) 0.0131(8) Uani 1 1 d . . . C16 C -0.3508(3) 0.33711(19) 0.16906(19) 0.0152(8) Uani 1 1 d . . . H16 H -0.3549 0.3780 0.2044 0.018 Uiso 1 1 calc R . . C17 C -0.4393(3) 0.29551(19) 0.13321(19) 0.0162(8) Uani 1 1 d . . . H17 H -0.5055 0.3059 0.1440 0.019 Uiso 1 1 calc R . . C18 C -0.4292(3) 0.23828(18) 0.08117(18) 0.0144(8) Uani 1 1 d . . . H18 H -0.4895 0.2091 0.0555 0.017 Uiso 1 1 calc R . . C19 C -0.3324(3) 0.22244(18) 0.06564(18) 0.0117(8) Uani 1 1 d . . . C20 C -0.3318(3) 0.16333(19) 0.00365(19) 0.0157(8) Uani 1 1 d . . . H20A H -0.2897 0.1837 -0.0303 0.024 Uiso 1 1 calc R . . H20B H -0.4043 0.1539 -0.0261 0.024 Uiso 1 1 calc R . . H20C H -0.3011 0.1137 0.0268 0.024 Uiso 1 1 calc R . . C21 C 0.1136(3) 0.27461(18) 0.08087(18) 0.0131(8) Uani 1 1 d . . . H21 H 0.1868 0.2698 0.0835 0.016 Uiso 1 1 calc R . . C22 C 0.0479(3) 0.32783(18) 0.02715(18) 0.0123(8) Uani 1 1 d . . . C23 C 0.0898(3) 0.37685(18) -0.01927(18) 0.0139(8) Uani 1 1 d . . . H23 H 0.1630 0.3754 -0.0174 0.017 Uiso 1 1 calc R . . C24 C 0.0232(3) 0.42799(19) -0.06842(19) 0.0161(8) Uani 1 1 d . . . H24 H 0.0491 0.4624 -0.1013 0.019 Uiso 1 1 calc R . . C25 C -0.0820(3) 0.42727(19) -0.06807(19) 0.0168(8) Uani 1 1 d . . . H25 H -0.1292 0.4621 -0.1011 0.020 Uiso 1 1 calc R . . C26 C -0.1208(3) 0.37675(19) -0.02049(18) 0.0143(8) Uani 1 1 d . . . C27 C -0.2360(3) 0.3784(2) -0.02387(19) 0.0165(8) Uani 1 1 d . . . H27A H -0.2657 0.3256 -0.0359 0.025 Uiso 1 1 calc R . . H27B H -0.2714 0.4155 -0.0637 0.025 Uiso 1 1 calc R . . H27C H -0.2464 0.3953 0.0258 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N100 0.035(2) 0.0187(17) 0.0305(19) 0.0001(15) 0.0018(18) -0.0002(16) C100 0.022(2) 0.0129(18) 0.020(2) 0.0004(16) 0.0063(18) 0.0010(17) C101 0.026(2) 0.020(2) 0.032(2) -0.0030(19) 0.006(2) 0.0001(18) C102 0.022(2) 0.0104(17) 0.0161(19) 0.0045(15) 0.0098(17) 0.0003(16) C103 0.018(2) 0.0160(18) 0.0166(19) -0.0010(16) 0.0050(17) -0.0049(16) C104 0.018(2) 0.0162(19) 0.027(2) 0.0075(17) 0.0121(18) 0.0031(16) C105 0.029(2) 0.0122(18) 0.019(2) 0.0038(16) 0.0143(19) 0.0043(17) C106 0.030(2) 0.0112(18) 0.0140(19) -0.0003(15) 0.0048(18) 0.0001(16) C107 0.013(2) 0.0160(18) 0.0194(19) 0.0036(16) 0.0030(17) 0.0013(16) C108 0.023(2) 0.023(2) 0.018(2) -0.0004(17) 0.0076(18) 0.0057(17) P1 0.0139(5) 0.0130(5) 0.0145(5) -0.0007(4) 0.0071(4) 0.0010(4) F1 0.0196(12) 0.0184(10) 0.0163(10) 0.0046(9) 0.0084(9) 0.0053(9) F2 0.0128(11) 0.0202(10) 0.0169(10) -0.0007(9) 0.0083(9) -0.0001(9) F3 0.0198(12) 0.0174(10) 0.0149(10) -0.0041(9) 0.0072(9) -0.0014(9) F4 0.0186(12) 0.0167(10) 0.0218(11) 0.0030(9) 0.0090(10) 0.0027(9) F5 0.0152(11) 0.0179(10) 0.0183(10) -0.0034(9) 0.0086(9) -0.0014(9) F6 0.0176(11) 0.0213(11) 0.0182(10) -0.0081(9) 0.0074(9) -0.0012(10) P2 0.0153(5) 0.0130(5) 0.0148(5) 0.0010(4) 0.0048(4) -0.0008(4) F7 0.0276(12) 0.0107(10) 0.0178(11) -0.0003(9) 0.0063(10) -0.0008(9) F8 0.0182(12) 0.0294(12) 0.0153(10) 0.0011(9) 0.0054(9) -0.0054(10) F9 0.0259(13) 0.0217(11) 0.0168(11) 0.0020(9) 0.0124(10) -0.0040(9) F10 0.0233(12) 0.0120(10) 0.0239(11) 0.0035(9) 0.0117(10) 0.0054(9) F11 0.0249(13) 0.0174(11) 0.0196(11) -0.0031(9) -0.0012(10) -0.0005(9) F12 0.0155(11) 0.0161(10) 0.0218(11) 0.0011(9) 0.0073(9) -0.0029(9) Fe1 0.0124(3) 0.0098(2) 0.0120(2) -0.0001(2) 0.0060(2) 0.0000(2) N1 0.0145(16) 0.0120(15) 0.0126(15) -0.0011(12) 0.0032(13) 0.0020(13) N2 0.0137(15) 0.0114(14) 0.0106(14) 0.0008(12) 0.0029(13) -0.0005(12) N3 0.0105(16) 0.0119(14) 0.0101(14) 0.0025(12) 0.0040(13) -0.0011(12) N4 0.0173(16) 0.0116(14) 0.0214(16) -0.0020(13) 0.0147(14) -0.0015(13) N5 0.0117(16) 0.0170(15) 0.0104(14) 0.0048(13) 0.0041(13) -0.0001(13) N6 0.0101(16) 0.0110(15) 0.0141(15) -0.0024(12) 0.0067(13) 0.0002(12) N7 0.0168(16) 0.0103(15) 0.0125(15) -0.0023(12) 0.0039(13) 0.0003(12) C1 0.0106(18) 0.0123(17) 0.0153(18) -0.0001(14) 0.0036(15) -0.0005(14) C2 0.0143(19) 0.0143(18) 0.0185(19) 0.0002(16) 0.0081(16) 0.0051(15) C3 0.0149(19) 0.0140(17) 0.0142(18) -0.0005(15) 0.0087(16) 0.0008(15) C4 0.015(2) 0.0112(17) 0.0162(18) -0.0007(15) 0.0046(16) -0.0019(15) C5 0.016(2) 0.0098(17) 0.0167(19) 0.0034(15) 0.0090(16) -0.0010(15) C6 0.019(2) 0.0135(18) 0.0110(17) 0.0008(15) 0.0087(16) -0.0029(16) C7 0.0077(18) 0.0157(18) 0.0162(18) 0.0039(15) 0.0084(16) -0.0003(15) C8 0.0119(19) 0.0142(18) 0.0140(18) -0.0019(15) 0.0071(16) 0.0015(15) C9 0.0125(19) 0.0133(18) 0.0151(18) 0.0022(15) 0.0042(16) 0.0010(15) C10 0.018(2) 0.0111(17) 0.0179(19) -0.0035(15) 0.0080(17) 0.0014(15) C11 0.0110(19) 0.0198(19) 0.0118(17) -0.0002(15) 0.0043(15) -0.0010(16) C12 0.0058(18) 0.0181(18) 0.0169(19) -0.0050(15) 0.0056(16) 0.0018(15) C13 0.0159(19) 0.0153(18) 0.0105(17) -0.0016(15) 0.0059(16) -0.0008(15) C14 0.021(2) 0.0073(17) 0.0104(17) 0.0015(14) 0.0054(16) 0.0022(15) C15 0.0134(19) 0.0134(18) 0.0117(17) 0.0038(15) 0.0019(16) -0.0002(15) C16 0.020(2) 0.0129(18) 0.0157(18) 0.0013(15) 0.0096(17) 0.0040(16) C17 0.0132(19) 0.0194(19) 0.0176(19) 0.0019(16) 0.0067(16) 0.0028(16) C18 0.0157(19) 0.0124(18) 0.0143(17) 0.0032(15) 0.0019(16) -0.0055(15) C19 0.0155(19) 0.0121(17) 0.0103(17) 0.0063(14) 0.0084(16) 0.0021(15) C20 0.015(2) 0.0133(18) 0.0193(19) 0.0003(15) 0.0054(17) 0.0002(15) C21 0.0109(18) 0.0158(18) 0.0143(18) -0.0062(15) 0.0062(16) 0.0005(15) C22 0.020(2) 0.0099(17) 0.0072(16) -0.0051(14) 0.0045(16) -0.0002(15) C23 0.015(2) 0.0101(17) 0.0180(19) -0.0062(15) 0.0063(16) 0.0015(15) C24 0.025(2) 0.0112(18) 0.0119(18) -0.0037(15) 0.0034(17) -0.0044(16) C25 0.021(2) 0.0131(18) 0.0148(19) -0.0048(15) 0.0008(17) 0.0037(16) C26 0.024(2) 0.0102(17) 0.0095(17) -0.0032(14) 0.0053(17) -0.0013(16) C27 0.017(2) 0.0195(19) 0.0137(18) 0.0039(15) 0.0049(17) 0.0052(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 N100 C100 1.139(4) . ? C100 C101 1.459(5) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C107 1.379(5) . ? C102 C103 1.395(5) . ? C102 C108 1.506(4) . ? C103 C104 1.392(5) . ? C103 H103 0.9500 . ? C104 C105 1.387(5) . ? C104 H104 0.9500 . ? C105 C106 1.374(5) . ? C105 H105 0.9500 . ? C106 C107 1.401(5) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? C108 H10D 0.9800 . ? C108 H10E 0.9800 . ? C108 H10F 0.9800 . ? P1 F1 1.5950(19) . ? P1 F4 1.6011(19) . ? P1 F3 1.6016(19) . ? P1 F5 1.603(2) . ? P1 F6 1.6091(19) . ? P1 F2 1.614(2) . ? P2 F10 1.5977(19) . ? P2 F8 1.601(2) . ? P2 F11 1.602(2) . ? P2 F12 1.603(2) . ? P2 F7 1.6048(19) . ? P2 F9 1.605(2) . ? Fe1 N7 1.958(3) . ? Fe1 N5 1.962(3) . ? Fe1 N6 1.979(3) . ? Fe1 N1 2.092(3) . ? Fe1 N3 2.092(3) . ? Fe1 N2 2.101(3) . ? N1 C26 1.357(4) . ? N1 C22 1.360(4) . ? N2 C19 1.352(4) . ? N2 C15 1.372(4) . ? N3 C12 1.357(4) . ? N3 C8 1.372(4) . ? N4 C1 1.432(4) . ? N4 C5 1.442(4) . ? N4 C3 1.448(4) . ? N5 C14 1.267(4) . ? N5 C4 1.465(4) . ? N6 C7 1.264(4) . ? N6 C6 1.472(4) . ? N7 C21 1.282(4) . ? N7 C2 1.474(4) . ? C1 C2 1.531(4) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.533(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.522(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.445(4) . ? C7 H7 0.9500 . ? C8 C9 1.369(4) . ? C9 C10 1.377(4) . ? C9 H9 0.9500 . ? C10 C11 1.371(4) . ? C10 H10 0.9500 . ? C11 C12 1.391(4) . ? C11 H11 0.9500 . ? C12 C13 1.495(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.444(4) . ? C14 H14 0.9500 . ? C15 C16 1.377(5) . ? C16 C17 1.374(5) . ? C16 H16 0.9500 . ? C17 C18 1.377(4) . ? C17 H17 0.9500 . ? C18 C19 1.387(5) . ? C18 H18 0.9500 . ? C19 C20 1.501(4) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.442(4) . ? C21 H21 0.9500 . ? C22 C23 1.383(4) . ? C23 C24 1.384(4) . ? C23 H23 0.9500 . ? C24 C25 1.377(5) . ? C24 H24 0.9500 . ? C25 C26 1.391(5) . ? C25 H25 0.9500 . ? C26 C27 1.493(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N100 C100 C101 179.7(4) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C107 C102 C103 119.1(3) . . ? C107 C102 C108 120.6(3) . . ? C103 C102 C108 120.3(3) . . ? C104 C103 C102 120.1(3) . . ? C104 C103 H103 120.0 . . ? C102 C103 H103 120.0 . . ? C105 C104 C103 120.3(3) . . ? C105 C104 H104 119.8 . . ? C103 C104 H104 119.8 . . ? C106 C105 C104 119.9(3) . . ? C106 C105 H105 120.1 . . ? C104 C105 H105 120.1 . . ? C105 C106 C107 119.9(3) . . ? C105 C106 H106 120.1 . . ? C107 C106 H106 120.1 . . ? C102 C107 C106 120.8(3) . . ? C102 C107 H107 119.6 . . ? C106 C107 H107 119.6 . . ? C102 C108 H10D 109.5 . . ? C102 C108 H10E 109.5 . . ? H10D C108 H10E 109.5 . . ? C102 C108 H10F 109.5 . . ? H10D C108 H10F 109.5 . . ? H10E C108 H10F 109.5 . . ? F1 P1 F4 178.96(12) . . ? F1 P1 F3 90.20(10) . . ? F4 P1 F3 90.70(10) . . ? F1 P1 F5 90.00(11) . . ? F4 P1 F5 90.52(11) . . ? F3 P1 F5 90.55(10) . . ? F1 P1 F6 89.66(10) . . ? F4 P1 F6 89.44(10) . . ? F3 P1 F6 179.47(12) . . ? F5 P1 F6 89.96(10) . . ? F1 P1 F2 89.86(11) . . ? F4 P1 F2 89.61(11) . . ? F3 P1 F2 90.08(11) . . ? F5 P1 F2 179.35(12) . . ? F6 P1 F2 89.41(10) . . ? F10 P2 F8 90.31(11) . . ? F10 P2 F11 90.04(11) . . ? F8 P2 F11 179.54(13) . . ? F10 P2 F12 89.69(11) . . ? F8 P2 F12 90.26(11) . . ? F11 P2 F12 90.04(11) . . ? F10 P2 F7 179.28(13) . . ? F8 P2 F7 89.64(11) . . ? F11 P2 F7 90.02(10) . . ? F12 P2 F7 89.59(11) . . ? F10 P2 F9 90.74(11) . . ? F8 P2 F9 89.60(11) . . ? F11 P2 F9 90.09(11) . . ? F12 P2 F9 179.55(11) . . ? F7 P2 F9 89.98(11) . . ? N7 Fe1 N5 94.78(11) . . ? N7 Fe1 N6 93.05(11) . . ? N5 Fe1 N6 92.70(11) . . ? N7 Fe1 N1 80.31(11) . . ? N5 Fe1 N1 85.58(11) . . ? N6 Fe1 N1 172.96(11) . . ? N7 Fe1 N3 87.47(11) . . ? N5 Fe1 N3 172.99(11) . . ? N6 Fe1 N3 80.53(10) . . ? N1 Fe1 N3 101.36(10) . . ? N7 Fe1 N2 174.72(11) . . ? N5 Fe1 N2 80.93(11) . . ? N6 Fe1 N2 84.12(11) . . ? N1 Fe1 N2 102.32(11) . . ? N3 Fe1 N2 96.44(11) . . ? C26 N1 C22 116.9(3) . . ? C26 N1 Fe1 132.3(2) . . ? C22 N1 Fe1 110.7(2) . . ? C19 N2 C15 116.3(3) . . ? C19 N2 Fe1 134.1(2) . . ? C15 N2 Fe1 109.2(2) . . ? C12 N3 C8 116.4(3) . . ? C12 N3 Fe1 133.1(2) . . ? C8 N3 Fe1 110.4(2) . . ? C1 N4 C5 119.1(3) . . ? C1 N4 C3 120.8(3) . . ? C5 N4 C3 119.9(3) . . ? C14 N5 C4 117.6(3) . . ? C14 N5 Fe1 115.4(2) . . ? C4 N5 Fe1 126.9(2) . . ? C7 N6 C6 117.8(3) . . ? C7 N6 Fe1 115.4(2) . . ? C6 N6 Fe1 126.8(2) . . ? C21 N7 C2 116.1(3) . . ? C21 N7 Fe1 116.3(2) . . ? C2 N7 Fe1 127.6(2) . . ? N4 C1 C2 115.9(3) . . ? N4 C1 H1A 108.3 . . ? C2 C1 H1A 108.3 . . ? N4 C1 H1B 108.3 . . ? C2 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? N7 C2 C1 110.5(2) . . ? N7 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? N7 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? N4 C3 C4 116.0(3) . . ? N4 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? N4 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? N5 C4 C3 111.4(3) . . ? N5 C4 H4A 109.4 . . ? C3 C4 H4A 109.4 . . ? N5 C4 H4B 109.4 . . ? C3 C4 H4B 109.4 . . ? H4A C4 H4B 108.0 . . ? N4 C5 C6 116.5(3) . . ? N4 C5 H5A 108.2 . . ? C6 C5 H5A 108.2 . . ? N4 C5 H5B 108.2 . . ? C6 C5 H5B 108.2 . . ? H5A C5 H5B 107.3 . . ? N6 C6 C5 112.2(3) . . ? N6 C6 H6A 109.2 . . ? C5 C6 H6A 109.2 . . ? N6 C6 H6B 109.2 . . ? C5 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N6 C7 C8 119.6(3) . . ? N6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C9 C8 N3 124.1(3) . . ? C9 C8 C7 121.6(3) . . ? N3 C8 C7 114.1(3) . . ? C8 C9 C10 119.0(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 117.9(3) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C12 121.6(3) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? N3 C12 C11 121.0(3) . . ? N3 C12 C13 120.1(3) . . ? C11 C12 C13 118.9(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 C15 119.3(3) . . ? N5 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N2 C15 C16 124.0(3) . . ? N2 C15 C14 114.4(3) . . ? C16 C15 C14 121.5(3) . . ? C17 C16 C15 118.8(3) . . ? C17 C16 H16 120.6 . . ? C15 C16 H16 120.6 . . ? C16 C17 C18 118.1(3) . . ? C16 C17 H17 121.0 . . ? C18 C17 H17 121.0 . . ? C17 C18 C19 121.2(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? N2 C19 C18 121.6(3) . . ? N2 C19 C20 121.6(3) . . ? C18 C19 C20 116.8(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 C22 118.1(3) . . ? N7 C21 H21 121.0 . . ? C22 C21 H21 121.0 . . ? N1 C22 C23 124.0(3) . . ? N1 C22 C21 114.5(3) . . ? C23 C22 C21 121.5(3) . . ? C22 C23 C24 118.8(3) . . ? C22 C23 H23 120.6 . . ? C24 C23 H23 120.6 . . ? C25 C24 C23 117.7(3) . . ? C25 C24 H24 121.2 . . ? C23 C24 H24 121.2 . . ? C24 C25 C26 121.5(3) . . ? C24 C25 H25 119.2 . . ? C26 C25 H25 119.2 . . ? N1 C26 C25 121.1(3) . . ? N1 C26 C27 120.2(3) . . ? C25 C26 C27 118.6(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C107 C102 C103 C104 0.6(5) . . . . ? C108 C102 C103 C104 -178.8(3) . . . . ? C102 C103 C104 C105 -0.2(5) . . . . ? C103 C104 C105 C106 0.3(5) . . . . ? C104 C105 C106 C107 -0.9(5) . . . . ? C103 C102 C107 C106 -1.2(5) . . . . ? C108 C102 C107 C106 178.2(3) . . . . ? C105 C106 C107 C102 1.4(5) . . . . ? N7 Fe1 N1 C26 -175.6(3) . . . . ? N5 Fe1 N1 C26 -80.0(3) . . . . ? N3 Fe1 N1 C26 99.0(3) . . . . ? N2 Fe1 N1 C26 -0.3(3) . . . . ? N7 Fe1 N1 C22 0.5(2) . . . . ? N5 Fe1 N1 C22 96.1(2) . . . . ? N3 Fe1 N1 C22 -84.9(2) . . . . ? N2 Fe1 N1 C22 175.8(2) . . . . ? N5 Fe1 N2 C19 -178.6(3) . . . . ? N6 Fe1 N2 C19 -84.9(3) . . . . ? N1 Fe1 N2 C19 98.0(3) . . . . ? N3 Fe1 N2 C19 -5.1(3) . . . . ? N5 Fe1 N2 C15 -6.8(2) . . . . ? N6 Fe1 N2 C15 86.9(2) . . . . ? N1 Fe1 N2 C15 -90.2(2) . . . . ? N3 Fe1 N2 C15 166.7(2) . . . . ? N7 Fe1 N3 C12 -89.5(3) . . . . ? N6 Fe1 N3 C12 177.0(3) . . . . ? N1 Fe1 N3 C12 -9.9(3) . . . . ? N2 Fe1 N3 C12 94.1(3) . . . . ? N7 Fe1 N3 C8 94.2(2) . . . . ? N6 Fe1 N3 C8 0.7(2) . . . . ? N1 Fe1 N3 C8 173.8(2) . . . . ? N2 Fe1 N3 C8 -82.3(2) . . . . ? N7 Fe1 N5 C14 -173.4(2) . . . . ? N6 Fe1 N5 C14 -80.1(2) . . . . ? N1 Fe1 N5 C14 106.7(2) . . . . ? N2 Fe1 N5 C14 3.5(2) . . . . ? N7 Fe1 N5 C4 2.7(3) . . . . ? N6 Fe1 N5 C4 96.0(3) . . . . ? N1 Fe1 N5 C4 -77.2(3) . . . . ? N2 Fe1 N5 C4 179.6(3) . . . . ? N7 Fe1 N6 C7 -87.5(3) . . . . ? N5 Fe1 N6 C7 177.6(3) . . . . ? N3 Fe1 N6 C7 -0.6(2) . . . . ? N2 Fe1 N6 C7 97.0(3) . . . . ? N7 Fe1 N6 C6 92.2(3) . . . . ? N5 Fe1 N6 C6 -2.7(3) . . . . ? N3 Fe1 N6 C6 179.1(3) . . . . ? N2 Fe1 N6 C6 -83.3(3) . . . . ? N5 Fe1 N7 C21 -86.8(2) . . . . ? N6 Fe1 N7 C21 -179.8(2) . . . . ? N1 Fe1 N7 C21 -2.2(2) . . . . ? N3 Fe1 N7 C21 99.8(2) . . . . ? N5 Fe1 N7 C2 92.1(2) . . . . ? N6 Fe1 N7 C2 -0.9(2) . . . . ? N1 Fe1 N7 C2 176.7(3) . . . . ? N3 Fe1 N7 C2 -81.3(2) . . . . ? C5 N4 C1 C2 65.2(4) . . . . ? C3 N4 C1 C2 -109.9(3) . . . . ? C21 N7 C2 C1 93.0(3) . . . . ? Fe1 N7 C2 C1 -85.9(3) . . . . ? N4 C1 C2 N7 58.4(4) . . . . ? C1 N4 C3 C4 67.6(4) . . . . ? C5 N4 C3 C4 -107.5(3) . . . . ? C14 N5 C4 C3 89.8(3) . . . . ? Fe1 N5 C4 C3 -86.3(3) . . . . ? N4 C3 C4 N5 56.4(4) . . . . ? C1 N4 C5 C6 -109.0(3) . . . . ? C3 N4 C5 C6 66.2(4) . . . . ? C7 N6 C6 C5 96.3(4) . . . . ? Fe1 N6 C6 C5 -83.4(3) . . . . ? N4 C5 C6 N6 57.6(4) . . . . ? C6 N6 C7 C8 -179.3(3) . . . . ? Fe1 N6 C7 C8 0.4(4) . . . . ? C12 N3 C8 C9 -1.8(5) . . . . ? Fe1 N3 C8 C9 175.2(3) . . . . ? C12 N3 C8 C7 -177.6(3) . . . . ? Fe1 N3 C8 C7 -0.7(3) . . . . ? N6 C7 C8 C9 -175.7(3) . . . . ? N6 C7 C8 N3 0.2(5) . . . . ? N3 C8 C9 C10 0.4(5) . . . . ? C7 C8 C9 C10 175.9(3) . . . . ? C8 C9 C10 C11 0.5(5) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C8 N3 C12 C11 2.4(5) . . . . ? Fe1 N3 C12 C11 -173.7(2) . . . . ? C8 N3 C12 C13 -179.4(3) . . . . ? Fe1 N3 C12 C13 4.4(5) . . . . ? C10 C11 C12 N3 -1.6(5) . . . . ? C10 C11 C12 C13 -179.8(3) . . . . ? C4 N5 C14 C15 -175.9(3) . . . . ? Fe1 N5 C14 C15 0.6(4) . . . . ? C19 N2 C15 C16 0.9(5) . . . . ? Fe1 N2 C15 C16 -172.5(3) . . . . ? C19 N2 C15 C14 -177.7(3) . . . . ? Fe1 N2 C15 C14 8.8(3) . . . . ? N5 C14 C15 N2 -6.8(4) . . . . ? N5 C14 C15 C16 174.5(3) . . . . ? N2 C15 C16 C17 0.9(5) . . . . ? C14 C15 C16 C17 179.5(3) . . . . ? C15 C16 C17 C18 -1.6(5) . . . . ? C16 C17 C18 C19 0.5(5) . . . . ? C15 N2 C19 C18 -2.0(4) . . . . ? Fe1 N2 C19 C18 169.3(2) . . . . ? C15 N2 C19 C20 174.7(3) . . . . ? Fe1 N2 C19 C20 -14.0(5) . . . . ? C17 C18 C19 N2 1.4(5) . . . . ? C17 C18 C19 C20 -175.4(3) . . . . ? C2 N7 C21 C22 -175.6(3) . . . . ? Fe1 N7 C21 C22 3.4(4) . . . . ? C26 N1 C22 C23 -1.5(5) . . . . ? Fe1 N1 C22 C23 -178.3(2) . . . . ? C26 N1 C22 C21 177.8(3) . . . . ? Fe1 N1 C22 C21 1.0(3) . . . . ? N7 C21 C22 N1 -2.9(4) . . . . ? N7 C21 C22 C23 176.4(3) . . . . ? N1 C22 C23 C24 0.7(5) . . . . ? C21 C22 C23 C24 -178.5(3) . . . . ? C22 C23 C24 C25 0.2(4) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C22 N1 C26 C25 1.2(4) . . . . ? Fe1 N1 C26 C25 177.2(2) . . . . ? C22 N1 C26 C27 -179.9(3) . . . . ? Fe1 N1 C26 C27 -4.0(4) . . . . ? C24 C25 C26 N1 -0.4(5) . . . . ? C24 C25 C26 C27 -179.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.624 _refine_diff_density_min -0.564 _refine_diff_density_rms 0.085 _iucr_refine_instructions_details ; TITL test structure: fepitpf6_10klightoff CELL 0.71069 13.0765 16.9570 17.9940 90.000 104.200 90.000 ZERR 4.00 0.0008 0.0010 0.0010 0.000 0.007 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N F P FE UNIT 144 176 32 48 8 4 MERG 2 OMIT -4.00 54.00 FMAP 2 PLAN 45 ACTA BOND $H CONF LIST 6 WPDB -2 L.S. 18 TEMP -263.00 WGHT 0.041500 FVAR 2.14864 N100 3 0.284302 0.484494 -0.112933 11.00000 0.03490 0.01867 = 0.03055 0.00010 0.00180 -0.00018 C100 1 0.353904 0.451594 -0.075182 11.00000 0.02231 0.01290 = 0.01963 0.00038 0.00626 0.00096 C101 1 0.442722 0.409082 -0.026838 11.00000 0.02575 0.02020 = 0.03156 -0.00303 0.00567 0.00012 AFIX 137 H10A 2 0.508061 0.424802 -0.040245 11.00000 0.02943 H10B 2 0.431960 0.352224 -0.034903 11.00000 0.06771 H10C 2 0.447789 0.421671 0.027100 11.00000 0.04057 AFIX 0 C102 1 0.496797 0.114148 0.213676 11.00000 0.02206 0.01041 = 0.01609 0.00455 0.00976 0.00028 C103 1 0.602698 0.091782 0.232749 11.00000 0.01753 0.01598 = 0.01656 -0.00096 0.00496 -0.00493 AFIX 43 H103 2 0.649985 0.114320 0.276199 11.00000 -1.20000 AFIX 0 C104 1 0.639155 0.036460 0.188166 11.00000 0.01757 0.01623 = 0.02732 0.00749 0.01209 0.00308 AFIX 43 H104 2 0.711357 0.021459 0.201250 11.00000 -1.20000 AFIX 0 C105 1 0.570579 0.003146 0.124752 11.00000 0.02893 0.01223 = 0.01937 0.00383 0.01428 0.00428 AFIX 43 H105 2 0.595695 -0.034775 0.094629 11.00000 -1.20000 AFIX 0 C106 1 0.466254 0.025086 0.105572 11.00000 0.03045 0.01118 = 0.01402 -0.00035 0.00481 0.00007 AFIX 43 H106 2 0.419306 0.002936 0.061740 11.00000 -1.20000 AFIX 0 C107 1 0.429258 0.080203 0.150804 11.00000 0.01322 0.01595 = 0.01943 0.00357 0.00300 0.00130 AFIX 43 H107 2 0.356750 0.094359 0.137996 11.00000 -1.20000 AFIX 0 C108 1 0.457310 0.175096 0.260806 11.00000 0.02348 0.02287 = 0.01833 -0.00043 0.00763 0.00570 AFIX 33 H10D 2 0.381196 0.182298 0.240556 11.00000 -1.50000 H10E 2 0.493556 0.225253 0.258319 11.00000 -1.50000 H10F 2 0.471488 0.157393 0.314206 11.00000 -1.50000 AFIX 0 P1 5 0.275078 0.200712 -0.074540 11.00000 0.01390 0.01301 = 0.01454 -0.00071 0.00708 0.00101 F1 4 0.309444 0.124251 -0.022816 11.00000 0.01960 0.01837 = 0.01629 0.00460 0.00844 0.00527 F2 4 0.393542 0.208654 -0.085474 11.00000 0.01284 0.02022 = 0.01692 -0.00072 0.00828 -0.00015 F3 4 0.243520 0.146554 -0.149618 11.00000 0.01979 0.01743 = 0.01486 -0.00412 0.00724 -0.00138 F4 4 0.242168 0.278380 -0.125384 11.00000 0.01863 0.01669 = 0.02181 0.00300 0.00900 0.00268 F5 4 0.157872 0.193238 -0.062727 11.00000 0.01520 0.01793 = 0.01826 -0.00341 0.00856 -0.00135 F6 4 0.307920 0.255006 0.000913 11.00000 0.01757 0.02126 = 0.01818 -0.00806 0.00742 -0.00123 P2 5 0.347910 0.451234 0.204010 11.00000 0.01528 0.01304 = 0.01480 0.00103 0.00484 -0.00084 F7 4 0.311202 0.541807 0.196873 11.00000 0.02760 0.01070 = 0.01781 -0.00027 0.00627 -0.00081 F8 4 0.436518 0.472372 0.280020 11.00000 0.01820 0.02944 = 0.01527 0.00107 0.00536 -0.00545 F9 4 0.430698 0.469535 0.153520 11.00000 0.02590 0.02169 = 0.01677 0.00196 0.01239 -0.00397 F10 4 0.383507 0.360861 0.211823 11.00000 0.02331 0.01196 = 0.02390 0.00353 0.01175 0.00539 F11 4 0.259468 0.430718 0.127635 11.00000 0.02491 0.01743 = 0.01955 -0.00306 -0.00123 -0.00052 F12 4 0.265187 0.433683 0.254552 11.00000 0.01551 0.01612 = 0.02182 0.00114 0.00727 -0.00293 FE1 6 -0.082536 0.245517 0.108736 11.00000 0.01245 0.00983 = 0.01204 -0.00010 0.00599 -0.00003 N1 3 -0.056113 0.325832 0.027189 11.00000 0.01446 0.01204 = 0.01256 -0.00115 0.00324 0.00197 N2 3 -0.243911 0.261195 0.101963 11.00000 0.01367 0.01145 = 0.01058 0.00077 0.00291 -0.00052 N3 3 -0.098089 0.139785 0.047050 11.00000 0.01054 0.01190 = 0.01006 0.00248 0.00397 -0.00114 N4 3 0.095554 0.256077 0.292526 11.00000 0.01726 0.01157 = 0.02138 -0.00204 0.01468 -0.00154 N5 3 -0.073487 0.337382 0.176349 11.00000 0.01167 0.01696 = 0.01043 0.00477 0.00405 -0.00013 N6 3 -0.088815 0.170730 0.191937 11.00000 0.01011 0.01096 = 0.01405 -0.00237 0.00665 0.00015 N7 3 0.070347 0.233917 0.124950 11.00000 0.01681 0.01033 = 0.01251 -0.00233 0.00387 0.00029 C1 1 0.177756 0.229728 0.258573 11.00000 0.01059 0.01230 = 0.01532 -0.00012 0.00362 -0.00049 AFIX 23 H1A 2 0.225843 0.195233 0.295827 11.00000 -1.20000 H1B 2 0.218950 0.276283 0.249793 11.00000 -1.20000 AFIX 0 C2 1 0.141908 0.184834 0.182799 11.00000 0.01425 0.01427 = 0.01851 0.00022 0.00810 0.00509 AFIX 23 H2A 2 0.204257 0.169977 0.163888 11.00000 -1.20000 H2B 2 0.105186 0.135829 0.191254 11.00000 -1.20000 AFIX 0 C3 1 0.070823 0.339130 0.294807 11.00000 0.01485 0.01402 = 0.01418 -0.00052 0.00865 0.00081 AFIX 23 H3A 2 0.136419 0.367698 0.319409 11.00000 -1.20000 H3B 2 0.021137 0.345877 0.327918 11.00000 -1.20000 AFIX 0 C4 1 0.022593 0.378153 0.217269 11.00000 0.01541 0.01123 = 0.01620 -0.00073 0.00455 -0.00192 AFIX 23 H4A 2 0.005748 0.433880 0.225593 11.00000 -1.20000 H4B 2 0.074692 0.377447 0.185577 11.00000 -1.20000 AFIX 0 C5 1 0.031724 0.198393 0.319135 11.00000 0.01633 0.00978 = 0.01667 0.00336 0.00903 -0.00104 AFIX 23 H5A 2 0.030897 0.211791 0.372535 11.00000 -1.20000 H5B 2 0.066454 0.146373 0.320312 11.00000 -1.20000 AFIX 0 C6 1 -0.081917 0.190220 0.272737 11.00000 0.01879 0.01355 = 0.01095 0.00083 0.00873 -0.00290 AFIX 23 H6A 2 -0.117155 0.148337 0.295660 11.00000 -1.20000 H6B 2 -0.119772 0.240321 0.275297 11.00000 -1.20000 AFIX 0 C7 1 -0.099415 0.099022 0.172451 11.00000 0.00768 0.01567 = 0.01623 0.00394 0.00837 -0.00032 AFIX 43 H7 2 -0.103461 0.059689 0.209218 11.00000 -1.20000 AFIX 0 C8 1 -0.105340 0.077254 0.093855 11.00000 0.01194 0.01424 = 0.01405 -0.00188 0.00713 0.00151 C9 1 -0.123633 0.001088 0.068967 11.00000 0.01254 0.01334 = 0.01507 0.00217 0.00417 0.00100 AFIX 43 H9 2 -0.128281 -0.039889 0.103992 11.00000 -1.20000 AFIX 0 C10 1 -0.135204 -0.015251 -0.007640 11.00000 0.01762 0.01112 = 0.01790 -0.00348 0.00797 0.00136 AFIX 43 H10 2 -0.148570 -0.067418 -0.026813 11.00000 -1.20000 AFIX 0 C11 1 -0.126812 0.046186 -0.055343 11.00000 0.01099 0.01984 = 0.01176 -0.00024 0.00431 -0.00097 AFIX 43 H11 2 -0.134628 0.036180 -0.108390 11.00000 -1.20000 AFIX 0 C12 1 -0.107138 0.122784 -0.027954 11.00000 0.00580 0.01809 = 0.01687 -0.00496 0.00556 0.00184 C13 1 -0.099214 0.187131 -0.083039 11.00000 0.01593 0.01530 = 0.01047 -0.00157 0.00588 -0.00077 AFIX 137 H13A 2 -0.029013 0.211184 -0.068001 11.00000 -1.50000 H13B 2 -0.152933 0.227267 -0.082452 11.00000 -1.50000 H13C 2 -0.110501 0.165129 -0.134781 11.00000 -1.50000 AFIX 0 C14 1 -0.160247 0.360471 0.188191 11.00000 0.02102 0.00733 = 0.01043 0.00150 0.00541 0.00216 AFIX 43 H14 2 -0.162316 0.404909 0.219941 11.00000 -1.20000 AFIX 0 C15 1 -0.255953 0.318561 0.152941 11.00000 0.01345 0.01345 = 0.01172 0.00383 0.00186 -0.00020 C16 1 -0.350764 0.337115 0.169064 11.00000 0.01992 0.01288 = 0.01568 0.00129 0.00960 0.00405 AFIX 43 H16 2 -0.354886 0.377957 0.204351 11.00000 -1.20000 AFIX 0 C17 1 -0.439262 0.295511 0.133209 11.00000 0.01317 0.01936 = 0.01760 0.00190 0.00671 0.00277 AFIX 43 H17 2 -0.505539 0.305918 0.143998 11.00000 -1.20000 AFIX 0 C18 1 -0.429161 0.238278 0.081172 11.00000 0.01567 0.01235 = 0.01426 0.00324 0.00192 -0.00549 AFIX 43 H18 2 -0.489529 0.209124 0.055454 11.00000 -1.20000 AFIX 0 C19 1 -0.332418 0.222444 0.065643 11.00000 0.01548 0.01208 = 0.01031 0.00628 0.00840 0.00206 C20 1 -0.331831 0.163327 0.003646 11.00000 0.01512 0.01332 = 0.01927 0.00029 0.00535 0.00022 AFIX 137 H20A 2 -0.289708 0.183716 -0.030273 11.00000 -1.50000 H20B 2 -0.404289 0.153947 -0.026071 11.00000 -1.50000 H20C 2 -0.301113 0.113724 0.026810 11.00000 -1.50000 AFIX 0 C21 1 0.113568 0.274614 0.080873 11.00000 0.01092 0.01577 = 0.01426 -0.00615 0.00618 0.00049 AFIX 43 H21 2 0.186766 0.269839 0.083540 11.00000 -1.20000 AFIX 0 C22 1 0.047883 0.327825 0.027152 11.00000 0.02027 0.00992 = 0.00722 -0.00514 0.00449 -0.00022 C23 1 0.089761 0.376850 -0.019274 11.00000 0.01489 0.01013 = 0.01796 -0.00617 0.00631 0.00153 AFIX 43 H23 2 0.162963 0.375435 -0.017447 11.00000 -1.20000 AFIX 0 C24 1 0.023169 0.427988 -0.068421 11.00000 0.02460 0.01117 = 0.01188 -0.00370 0.00340 -0.00437 AFIX 43 H24 2 0.049100 0.462385 -0.101253 11.00000 -1.20000 AFIX 0 C25 1 -0.082021 0.427271 -0.068069 11.00000 0.02053 0.01306 = 0.01484 -0.00480 0.00083 0.00372 AFIX 43 H25 2 -0.129239 0.462080 -0.101078 11.00000 -1.20000 AFIX 0 C26 1 -0.120756 0.376751 -0.020493 11.00000 0.02392 0.01015 = 0.00948 -0.00318 0.00534 -0.00128 C27 1 -0.235968 0.378411 -0.023868 11.00000 0.01690 0.01947 = 0.01369 0.00391 0.00495 0.00524 AFIX 137 H27A 2 -0.265706 0.325551 -0.035938 11.00000 -1.50000 H27B 2 -0.271418 0.415454 -0.063712 11.00000 -1.50000 H27C 2 -0.246400 0.395319 0.025831 11.00000 -1.50000 HKLF 4 REM test structure: fepitpf6_10klightoff REM R1 = 0.0467 for 4673 Fo > 4sig(Fo) and 0.0964 for all 8242 data REM 539 parameters refined using 0 restraints END WGHT 0.0413 0.0000 REM Highest difference peak 0.624, deepest hole -0.564, 1-sigma level 0.085 Q1 1 0.5278 0.1964 0.2955 11.00000 0.05 0.62 Q2 1 0.4164 0.2214 0.2246 11.00000 0.05 0.55 Q3 1 0.2755 0.4479 0.1761 11.00000 0.05 0.49 Q4 1 -0.0211 0.2590 0.1456 11.00000 0.05 0.49 Q5 1 0.4041 0.1486 0.2915 11.00000 0.05 0.46 Q6 1 -0.1292 0.2754 0.0633 11.00000 0.05 0.42 Q7 1 0.3719 0.5003 0.2485 11.00000 0.05 0.42 Q8 1 -0.1260 0.2460 0.0594 11.00000 0.05 0.42 Q9 1 0.3742 0.4987 0.1619 11.00000 0.05 0.41 Q10 1 0.0540 0.2484 0.2480 11.00000 0.05 0.38 Q11 1 0.4656 0.1171 0.1657 11.00000 0.05 0.38 Q12 1 0.2990 0.4962 0.2159 11.00000 0.05 0.34 Q13 1 0.3050 0.2612 -0.0781 11.00000 0.05 0.33 Q14 1 0.4350 0.2572 -0.0609 11.00000 0.05 0.32 Q15 1 -0.1659 0.3792 -0.0084 11.00000 0.05 0.32 Q16 1 0.3567 0.1996 -0.0724 11.00000 0.05 0.32 Q17 1 0.0828 0.3170 0.0648 11.00000 0.05 0.31 Q18 1 0.1765 0.2954 0.1015 11.00000 0.05 0.31 Q19 1 0.3578 0.4682 0.1262 11.00000 0.05 0.31 Q20 1 0.2565 0.5785 0.1838 11.00000 0.05 0.30 Q21 1 0.3803 0.2581 -0.1164 11.00000 0.05 0.30 Q22 1 0.3606 0.2991 0.0178 11.00000 0.05 0.30 Q23 1 0.2382 0.5658 0.1687 11.00000 0.05 0.30 Q24 1 -0.0403 0.1272 0.2039 11.00000 0.05 0.30 Q25 1 0.3829 0.4955 0.1076 11.00000 0.05 0.30 Q26 1 -0.2974 0.2591 0.0633 11.00000 0.05 0.29 Q27 1 -0.4434 0.2844 0.0783 11.00000 0.05 0.29 Q28 1 0.2126 0.5195 -0.1588 11.00000 0.05 0.28 Q29 1 0.1960 0.2127 0.1977 11.00000 0.05 0.28 Q30 1 -0.1335 0.1332 -0.0009 11.00000 0.05 0.28 Q31 1 0.2336 0.2426 -0.1146 11.00000 0.05 0.28 Q32 1 0.3008 0.4588 0.2942 11.00000 0.05 0.28 Q33 1 0.0628 0.2236 0.3005 11.00000 0.05 0.28 Q34 1 -0.0817 0.0955 0.1374 11.00000 0.05 0.27 Q35 1 0.2368 0.5492 0.1985 11.00000 0.05 0.27 Q36 1 0.0560 0.2480 0.4272 11.00000 0.05 0.27 Q37 1 -0.3128 0.3407 0.1394 11.00000 0.05 0.27 Q38 1 -0.0632 0.3800 0.0179 11.00000 0.05 0.27 Q39 1 0.2444 0.1629 -0.1209 11.00000 0.05 0.27 Q40 1 0.0779 0.4580 -0.0703 11.00000 0.05 0.27 Q41 1 -0.1972 0.3249 0.1816 11.00000 0.05 0.26 Q42 1 -0.1565 0.0469 0.0756 11.00000 0.05 0.26 Q43 1 0.2777 0.2570 0.2985 11.00000 0.05 0.26 Q44 1 0.1824 0.2437 -0.1624 11.00000 0.05 0.26 Q45 1 0.0567 0.1605 0.3296 11.00000 0.05 0.26 ; _database_code_depnum_ccdc_archive 'CCDC 928909' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_fepitpf6_10k660nm_revsep2013 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 F12 Fe N8 P2' _chemical_formula_weight 934.58 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 13.2599(4) _cell_length_b 16.8595(4) _cell_length_c 18.2715(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.897(3) _cell_angle_gamma 90.00 _cell_volume 3965.13(19) _cell_formula_units_Z 4 _cell_measurement_temperature 10(2) _cell_measurement_reflns_used 6085 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.566 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 10(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Saphire 3 Xcalibur' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean 19.64 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16808 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.1090 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.00 _reflns_number_total 8405 _reflns_number_gt 5002 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,Version 1.171.26' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,Version 1.171.26' _computing_structure_solution 'SIR-97_(Altomare & al., 1998)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON_(Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0301P)^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 8405 _refine_ls_number_parameters 539 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0769 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.848 _refine_ls_restrained_S_all 0.848 _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 N100 N 0.2882(2) 0.48429(14) -0.11066(14) 0.0259(6) Uani 1 1 d . . . C100 C 0.3607(2) 0.45188(17) -0.07678(16) 0.0183(7) Uani 1 1 d . . . C101 C 0.4535(2) 0.41072(19) -0.03407(17) 0.0267(8) Uani 1 1 d . . . H10A H 0.5149 0.4311 -0.0489 0.080(14) Uiso 1 1 calc R . . H10B H 0.4466 0.3537 -0.0447 0.073(13) Uiso 1 1 calc R . . H10C H 0.4611 0.4198 0.0200 0.062(12) Uiso 1 1 calc R . . C102 C 0.4986(2) 0.11498(15) 0.21459(14) 0.0135(6) Uani 1 1 d . . . C103 C 0.6025(2) 0.09403(16) 0.22656(15) 0.0157(7) Uani 1 1 d . . . H103 H 0.6521 0.1172 0.2672 0.019 Uiso 1 1 calc R . . C104 C 0.6350(2) 0.03940(16) 0.17977(16) 0.0185(7) Uani 1 1 d . . . H104 H 0.7065 0.0257 0.1888 0.022 Uiso 1 1 calc R . . C105 C 0.5641(2) 0.00501(16) 0.12019(15) 0.0184(7) Uani 1 1 d . . . H105 H 0.5864 -0.0320 0.0882 0.022 Uiso 1 1 calc R . . C106 C 0.4610(2) 0.02493(16) 0.10787(14) 0.0170(7) Uani 1 1 d . . . H106 H 0.4118 0.0016 0.0671 0.020 Uiso 1 1 calc R . . C107 C 0.4282(2) 0.07909(15) 0.15480(14) 0.0150(6) Uani 1 1 d . . . H107 H 0.3565 0.0918 0.1459 0.018 Uiso 1 1 calc R . . C108 C 0.4625(2) 0.17486(16) 0.26330(15) 0.0194(7) Uani 1 1 d . . . H10D H 0.3876 0.1832 0.2447 0.029 Uiso 1 1 calc R . . H10E H 0.4991 0.2251 0.2617 0.029 Uiso 1 1 calc R . . H10F H 0.4772 0.1554 0.3153 0.029 Uiso 1 1 calc R . . P1 P 0.28330(6) 0.20523(4) -0.07850(4) 0.01019(16) Uani 1 1 d . . . F1 F 0.31922(11) 0.13122(8) -0.02348(8) 0.0136(3) Uani 1 1 d . . . F2 F 0.39946(11) 0.21271(8) -0.09038(7) 0.0124(3) Uani 1 1 d . . . F3 F 0.25312(11) 0.14644(8) -0.14946(7) 0.0142(4) Uani 1 1 d . . . F4 F 0.24847(11) 0.27991(8) -0.13270(8) 0.0151(4) Uani 1 1 d . . . F5 F 0.16787(11) 0.19823(8) -0.06575(8) 0.0121(3) Uani 1 1 d . . . F6 F 0.31463(10) 0.26430(8) -0.00715(7) 0.0136(3) Uani 1 1 d . . . P2 P 0.33885(6) 0.45440(4) 0.20619(4) 0.01131(16) Uani 1 1 d . . . F7 F 0.29691(11) 0.54418(8) 0.19983(8) 0.0160(4) Uani 1 1 d . . . F8 F 0.43001(11) 0.47885(9) 0.27738(8) 0.0197(4) Uani 1 1 d . . . F9 F 0.41307(12) 0.47515(9) 0.15110(8) 0.0175(4) Uani 1 1 d . . . F10 F 0.37955(12) 0.36440(9) 0.21319(8) 0.0180(4) Uani 1 1 d . . . F11 F 0.24730(11) 0.43046(8) 0.13505(8) 0.0152(4) Uani 1 1 d . . . F12 F 0.26448(11) 0.43420(8) 0.26146(8) 0.0142(4) Uani 1 1 d . . . Fe1 Fe -0.07747(3) 0.24754(2) 0.10502(2) 0.00900(9) Uani 1 1 d . . . N1 N -0.04074(17) 0.33550(12) 0.01977(11) 0.0095(5) Uani 1 1 d . . . N2 N -0.25254(16) 0.26598(12) 0.09968(11) 0.0092(5) Uani 1 1 d . . . N3 N -0.09577(16) 0.13016(12) 0.04380(11) 0.0098(5) Uani 1 1 d . . . N4 N 0.07870(16) 0.25696(12) 0.27113(11) 0.0093(5) Uani 1 1 d . . . N5 N -0.08042(16) 0.34677(12) 0.17711(11) 0.0093(5) Uani 1 1 d . . . N6 N -0.08733(16) 0.16180(12) 0.19149(11) 0.0090(5) Uani 1 1 d . . . N7 N 0.08806(16) 0.23990(12) 0.11877(11) 0.0083(5) Uani 1 1 d . . . C1 C 0.17663(18) 0.23994(15) 0.25212(13) 0.0102(6) Uani 1 1 d . . . H1A H 0.2213 0.2085 0.2931 0.012 Uiso 1 1 calc R . . H1B H 0.2130 0.2903 0.2476 0.012 Uiso 1 1 calc R . . C2 C 0.1596(2) 0.19379(15) 0.17779(13) 0.0110(6) Uani 1 1 d . . . H2A H 0.2266 0.1859 0.1640 0.013 Uiso 1 1 calc R . . H2B H 0.1294 0.1411 0.1833 0.013 Uiso 1 1 calc R . . C3 C 0.0598(2) 0.33838(14) 0.29032(14) 0.0104(6) Uani 1 1 d . . . H3A H 0.1261 0.3627 0.3176 0.012 Uiso 1 1 calc R . . H3B H 0.0121 0.3385 0.3246 0.012 Uiso 1 1 calc R . . C4 C 0.0125(2) 0.38822(14) 0.22085(13) 0.0098(6) Uani 1 1 d . . . H4A H -0.0068 0.4413 0.2363 0.012 Uiso 1 1 calc R . . H4B H 0.0636 0.3952 0.1897 0.012 Uiso 1 1 calc R . . C5 C 0.0362(2) 0.19477(15) 0.30925(14) 0.0106(6) Uani 1 1 d . . . H5A H 0.0425 0.2103 0.3624 0.013 Uiso 1 1 calc R . . H5B H 0.0769 0.1456 0.3090 0.013 Uiso 1 1 calc R . . C6 C -0.0774(2) 0.17869(15) 0.27170(13) 0.0113(6) Uani 1 1 d . . . H6A H -0.1025 0.1328 0.2962 0.014 Uiso 1 1 calc R . . H6B H -0.1200 0.2255 0.2772 0.014 Uiso 1 1 calc R . . C7 C -0.09969(19) 0.09060(16) 0.16935(14) 0.0100(6) Uani 1 1 d . . . H7 H -0.1044 0.0501 0.2045 0.012 Uiso 1 1 calc R . . C8 C -0.10681(19) 0.06949(15) 0.09068(13) 0.0095(6) Uani 1 1 d . . . C9 C -0.12798(19) -0.00770(15) 0.06721(14) 0.0120(6) Uani 1 1 d . . . H9 H -0.1341 -0.0481 0.1022 0.014 Uiso 1 1 calc R . . C10 C -0.14011(19) -0.02516(16) -0.00863(14) 0.0127(6) Uani 1 1 d . . . H10 H -0.1566 -0.0774 -0.0270 0.015 Uiso 1 1 calc R . . C11 C -0.1278(2) 0.03476(15) -0.05635(15) 0.0121(6) Uani 1 1 d . . . H11 H -0.1348 0.0238 -0.1083 0.014 Uiso 1 1 calc R . . C12 C -0.1049(2) 0.11196(15) -0.02942(14) 0.0108(6) Uani 1 1 d . . . C13 C -0.0902(2) 0.17758(15) -0.08206(14) 0.0121(6) Uani 1 1 d . . . H13A H -0.1388 0.2208 -0.0799 0.018 Uiso 1 1 calc R . . H13B H -0.1035 0.1570 -0.1337 0.018 Uiso 1 1 calc R . . H13C H -0.0188 0.1975 -0.0668 0.018 Uiso 1 1 calc R . . C14 C -0.1685(2) 0.36432(15) 0.18906(14) 0.0123(6) Uani 1 1 d . . . H14 H -0.1731 0.4062 0.2229 0.015 Uiso 1 1 calc R . . C15 C -0.2624(2) 0.32140(15) 0.15186(14) 0.0102(6) Uani 1 1 d . . . C16 C -0.3551(2) 0.33856(16) 0.16967(14) 0.0126(6) Uani 1 1 d . . . H16 H -0.3583 0.3776 0.2065 0.015 Uiso 1 1 calc R . . C17 C -0.4442(2) 0.29772(16) 0.13277(14) 0.0152(6) Uani 1 1 d . . . H17 H -0.5093 0.3080 0.1439 0.018 Uiso 1 1 calc R . . C18 C -0.4350(2) 0.24246(16) 0.08013(14) 0.0134(6) Uani 1 1 d . . . H18 H -0.4946 0.2137 0.0543 0.016 Uiso 1 1 calc R . . C19 C -0.3397(2) 0.22766(15) 0.06375(14) 0.0105(6) Uani 1 1 d . . . C20 C -0.3343(2) 0.16787(15) 0.00366(14) 0.0137(6) Uani 1 1 d . . . H20A H -0.2885 0.1878 -0.0271 0.021 Uiso 1 1 calc R . . H20B H -0.4041 0.1592 -0.0284 0.021 Uiso 1 1 calc R . . H20C H -0.3068 0.1177 0.0274 0.021 Uiso 1 1 calc R . . C21 C 0.1277(2) 0.28179(14) 0.07465(13) 0.0094(6) Uani 1 1 d . . . H21 H 0.1999 0.2783 0.0770 0.011 Uiso 1 1 calc R . . C22 C 0.0616(2) 0.33520(15) 0.02038(14) 0.0096(6) Uani 1 1 d . . . C23 C 0.1052(2) 0.38302(14) -0.02543(14) 0.0104(6) Uani 1 1 d . . . H23 H 0.1774 0.3806 -0.0233 0.012 Uiso 1 1 calc R . . C24 C 0.0403(2) 0.43468(15) -0.07471(13) 0.0115(6) Uani 1 1 d . . . H24 H 0.0672 0.4680 -0.1074 0.014 Uiso 1 1 calc R . . C25 C -0.0634(2) 0.43647(15) -0.07499(14) 0.0113(6) Uani 1 1 d . . . H25 H -0.1088 0.4717 -0.1079 0.014 Uiso 1 1 calc R . . C26 C -0.1024(2) 0.38681(15) -0.02723(14) 0.0101(6) Uani 1 1 d . . . C27 C -0.2154(2) 0.38939(16) -0.02591(14) 0.0134(6) Uani 1 1 d . . . H27A H -0.2453 0.3361 -0.0353 0.020 Uiso 1 1 calc R . . H27B H -0.2525 0.4257 -0.0651 0.020 Uiso 1 1 calc R . . H27C H -0.2220 0.4080 0.0235 0.020 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N100 0.0281(16) 0.0220(14) 0.0287(16) 0.0001(12) 0.0091(13) 0.0037(14) C100 0.0204(17) 0.0162(15) 0.0198(16) -0.0009(13) 0.0081(13) 0.0010(15) C101 0.026(2) 0.0270(19) 0.0259(19) 0.0010(15) 0.0036(15) -0.0005(17) C102 0.0169(16) 0.0120(14) 0.0123(15) 0.0043(12) 0.0051(12) 0.0048(14) C103 0.0170(17) 0.0125(14) 0.0159(16) 0.0015(12) 0.0005(12) -0.0036(14) C104 0.0139(16) 0.0168(15) 0.0276(17) 0.0087(14) 0.0105(13) 0.0039(15) C105 0.0278(18) 0.0122(15) 0.0197(16) 0.0011(13) 0.0145(14) 0.0076(15) C106 0.0234(17) 0.0154(15) 0.0093(14) -0.0010(12) -0.0016(12) 0.0020(15) C107 0.0108(15) 0.0163(15) 0.0165(15) 0.0014(13) 0.0004(12) 0.0047(14) C108 0.0236(18) 0.0177(15) 0.0159(16) -0.0013(13) 0.0031(13) 0.0032(15) P1 0.0096(4) 0.0121(4) 0.0096(4) 0.0003(3) 0.0038(3) -0.0004(3) F1 0.0148(9) 0.0153(8) 0.0110(8) 0.0050(7) 0.0038(6) 0.0030(8) F2 0.0084(8) 0.0174(8) 0.0124(8) -0.0008(7) 0.0044(6) 0.0015(7) F3 0.0172(9) 0.0152(8) 0.0104(8) -0.0025(7) 0.0035(6) -0.0008(8) F4 0.0163(9) 0.0157(8) 0.0136(8) 0.0059(7) 0.0043(7) 0.0036(8) F5 0.0089(8) 0.0148(8) 0.0132(8) -0.0004(7) 0.0038(6) -0.0009(7) F6 0.0106(8) 0.0180(9) 0.0126(8) -0.0050(7) 0.0035(6) -0.0007(7) P2 0.0113(4) 0.0129(4) 0.0095(4) 0.0008(3) 0.0020(3) -0.0014(3) F7 0.0229(9) 0.0112(8) 0.0140(8) -0.0023(7) 0.0045(7) -0.0025(8) F8 0.0145(9) 0.0310(10) 0.0116(8) 0.0023(7) -0.0006(7) -0.0071(8) F9 0.0208(9) 0.0209(9) 0.0126(8) 0.0030(7) 0.0077(7) -0.0017(8) F10 0.0189(9) 0.0162(8) 0.0212(9) 0.0047(7) 0.0096(7) 0.0074(8) F11 0.0159(9) 0.0143(8) 0.0129(8) -0.0030(7) -0.0016(6) 0.0004(8) F12 0.0117(8) 0.0156(8) 0.0164(8) 0.0002(7) 0.0057(7) -0.0025(8) Fe1 0.00914(19) 0.00995(19) 0.00817(19) -0.00041(17) 0.00261(14) -0.0005(2) N1 0.0123(12) 0.0096(11) 0.0067(11) -0.0013(9) 0.0027(9) -0.0001(11) N2 0.0123(12) 0.0095(11) 0.0061(11) 0.0012(9) 0.0031(9) -0.0017(11) N3 0.0083(12) 0.0117(12) 0.0091(12) 0.0005(10) 0.0012(9) 0.0000(11) N4 0.0099(11) 0.0088(11) 0.0112(11) 0.0003(10) 0.0061(9) 0.0004(11) N5 0.0106(12) 0.0103(11) 0.0065(11) 0.0026(9) 0.0014(9) -0.0004(11) N6 0.0078(12) 0.0127(12) 0.0067(11) -0.0018(10) 0.0025(9) 0.0002(11) N7 0.0100(11) 0.0062(11) 0.0078(11) -0.0023(9) 0.0003(9) 0.0016(11) C1 0.0079(13) 0.0137(14) 0.0092(13) 0.0006(12) 0.0025(10) -0.0013(13) C2 0.0097(14) 0.0107(13) 0.0136(14) 0.0023(12) 0.0048(11) 0.0034(13) C3 0.0091(14) 0.0107(13) 0.0119(14) -0.0045(12) 0.0037(11) -0.0014(13) C4 0.0120(15) 0.0081(13) 0.0093(14) -0.0016(11) 0.0023(11) -0.0011(13) C5 0.0131(15) 0.0121(14) 0.0068(14) -0.0014(11) 0.0030(11) 0.0027(13) C6 0.0164(16) 0.0091(13) 0.0094(14) 0.0004(11) 0.0047(11) 0.0004(13) C7 0.0065(14) 0.0134(14) 0.0110(14) 0.0042(12) 0.0039(11) 0.0002(13) C8 0.0067(14) 0.0148(14) 0.0076(13) 0.0014(12) 0.0031(11) 0.0013(13) C9 0.0114(15) 0.0115(14) 0.0134(15) 0.0021(12) 0.0037(12) 0.0005(13) C10 0.0124(15) 0.0113(14) 0.0150(15) -0.0047(12) 0.0044(12) -0.0005(14) C11 0.0099(14) 0.0153(14) 0.0111(14) -0.0010(12) 0.0026(11) 0.0024(14) C12 0.0066(15) 0.0140(14) 0.0120(15) -0.0007(12) 0.0028(11) 0.0018(13) C13 0.0125(15) 0.0128(14) 0.0105(14) -0.0013(12) 0.0018(11) -0.0002(13) C14 0.0193(16) 0.0096(14) 0.0086(14) 0.0013(12) 0.0045(12) 0.0030(14) C15 0.0114(15) 0.0123(14) 0.0069(14) 0.0064(11) 0.0018(11) 0.0036(13) C16 0.0176(16) 0.0144(14) 0.0071(14) -0.0018(12) 0.0054(11) 0.0020(14) C17 0.0094(15) 0.0230(16) 0.0145(15) 0.0018(13) 0.0051(12) 0.0017(14) C18 0.0096(14) 0.0179(15) 0.0120(14) 0.0014(13) 0.0011(11) -0.0021(14) C19 0.0136(15) 0.0117(14) 0.0059(13) 0.0057(11) 0.0021(11) 0.0008(13) C20 0.0162(16) 0.0148(14) 0.0100(14) 0.0000(12) 0.0032(11) -0.0006(14) C21 0.0086(14) 0.0091(13) 0.0104(14) -0.0048(11) 0.0019(11) -0.0002(13) C22 0.0118(15) 0.0094(13) 0.0078(14) -0.0058(11) 0.0030(11) -0.0012(13) C23 0.0109(15) 0.0100(14) 0.0111(14) -0.0028(11) 0.0043(11) -0.0034(13) C24 0.0172(16) 0.0100(14) 0.0086(14) -0.0003(11) 0.0056(12) 0.0002(14) C25 0.0138(15) 0.0093(14) 0.0092(14) -0.0009(11) -0.0003(11) 0.0013(13) C26 0.0148(16) 0.0076(13) 0.0074(14) -0.0058(11) 0.0014(11) -0.0001(13) C27 0.0131(15) 0.0154(15) 0.0113(14) 0.0054(12) 0.0023(12) 0.0009(14) _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 N100 C100 1.149(3) . ? C100 C101 1.464(4) . ? C101 H10A 0.9800 . ? C101 H10B 0.9800 . ? C101 H10C 0.9800 . ? C102 C103 1.387(4) . ? C102 C107 1.393(4) . ? C102 C108 1.499(3) . ? C103 C104 1.394(4) . ? C103 H103 0.9500 . ? C104 C105 1.384(4) . ? C104 H104 0.9500 . ? C105 C106 1.372(4) . ? C105 H105 0.9500 . ? C106 C107 1.392(4) . ? C106 H106 0.9500 . ? C107 H107 0.9500 . ? C108 H10D 0.9800 . ? C108 H10E 0.9800 . ? C108 H10F 0.9800 . ? P1 F4 1.5999(15) . ? P1 F1 1.6014(15) . ? P1 F3 1.6046(15) . ? P1 F5 1.6069(15) . ? P1 F2 1.6112(15) . ? P1 F6 1.6137(15) . ? P2 F11 1.6025(15) . ? P2 F8 1.6025(15) . ? P2 F10 1.6053(16) . ? P2 F9 1.6060(16) . ? P2 F7 1.6070(15) . ? P2 F12 1.6084(15) . ? Fe1 N5 2.135(2) . ? Fe1 N7 2.152(2) . ? Fe1 N6 2.168(2) . ? Fe1 N3 2.257(2) . ? Fe1 N1 2.286(2) . ? Fe1 N2 2.321(2) . ? N1 C26 1.348(3) . ? N1 C22 1.355(3) . ? N2 C19 1.349(3) . ? N2 C15 1.364(3) . ? N3 C12 1.349(3) . ? N3 C8 1.364(3) . ? N4 C5 1.446(3) . ? N4 C1 1.451(3) . ? N4 C3 1.454(3) . ? N5 C14 1.273(3) . ? N5 C4 1.474(3) . ? N6 C7 1.265(3) . ? N6 C6 1.468(3) . ? N7 C21 1.276(3) . ? N7 C2 1.475(3) . ? C1 C2 1.534(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.526(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(3) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.462(3) . ? C7 H7 0.9500 . ? C8 C9 1.378(3) . ? C9 C10 1.388(3) . ? C9 H9 0.9500 . ? C10 C11 1.370(3) . ? C10 H10 0.9500 . ? C11 C12 1.399(3) . ? C11 H11 0.9500 . ? C12 C13 1.509(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.460(3) . ? C14 H14 0.9500 . ? C15 C16 1.376(3) . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C17 C18 1.365(3) . ? C17 H17 0.9500 . ? C18 C19 1.390(3) . ? C18 H18 0.9500 . ? C19 C20 1.505(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.464(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(3) . ? C23 C24 1.392(3) . ? C23 H23 0.9500 . ? C24 C25 1.375(3) . ? C24 H24 0.9500 . ? C25 C26 1.395(3) . ? C25 H25 0.9500 . ? C26 C27 1.505(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 N100 C100 C101 179.6(3) . . ? C100 C101 H10A 109.5 . . ? C100 C101 H10B 109.5 . . ? H10A C101 H10B 109.5 . . ? C100 C101 H10C 109.5 . . ? H10A C101 H10C 109.5 . . ? H10B C101 H10C 109.5 . . ? C103 C102 C107 117.8(2) . . ? C103 C102 C108 121.7(3) . . ? C107 C102 C108 120.6(3) . . ? C102 C103 C104 120.9(3) . . ? C102 C103 H103 119.5 . . ? C104 C103 H103 119.5 . . ? C105 C104 C103 120.5(3) . . ? C105 C104 H104 119.8 . . ? C103 C104 H104 119.8 . . ? C106 C105 C104 119.3(3) . . ? C106 C105 H105 120.4 . . ? C104 C105 H105 120.4 . . ? C105 C106 C107 120.4(3) . . ? C105 C106 H106 119.8 . . ? C107 C106 H106 119.8 . . ? C106 C107 C102 121.2(3) . . ? C106 C107 H107 119.4 . . ? C102 C107 H107 119.4 . . ? C102 C108 H10D 109.5 . . ? C102 C108 H10E 109.5 . . ? H10D C108 H10E 109.5 . . ? C102 C108 H10F 109.5 . . ? H10D C108 H10F 109.5 . . ? H10E C108 H10F 109.5 . . ? F4 P1 F1 179.24(10) . . ? F4 P1 F3 90.40(8) . . ? F1 P1 F3 90.28(8) . . ? F4 P1 F5 90.23(8) . . ? F1 P1 F5 90.10(8) . . ? F3 P1 F5 90.60(8) . . ? F4 P1 F2 89.89(8) . . ? F1 P1 F2 89.77(8) . . ? F3 P1 F2 90.02(8) . . ? F5 P1 F2 179.37(9) . . ? F4 P1 F6 89.68(8) . . ? F1 P1 F6 89.64(8) . . ? F3 P1 F6 179.54(9) . . ? F5 P1 F6 89.86(8) . . ? F2 P1 F6 89.52(8) . . ? F11 P2 F8 179.64(10) . . ? F11 P2 F10 90.07(8) . . ? F8 P2 F10 90.28(9) . . ? F11 P2 F9 90.31(8) . . ? F8 P2 F9 89.79(8) . . ? F10 P2 F9 90.63(8) . . ? F11 P2 F7 89.83(8) . . ? F8 P2 F7 89.82(9) . . ? F10 P2 F7 179.19(9) . . ? F9 P2 F7 90.18(8) . . ? F11 P2 F12 89.81(8) . . ? F8 P2 F12 90.08(8) . . ? F10 P2 F12 89.70(8) . . ? F9 P2 F12 179.65(9) . . ? F7 P2 F12 89.49(8) . . ? N5 Fe1 N7 98.28(8) . . ? N5 Fe1 N6 93.41(8) . . ? N7 Fe1 N6 96.50(8) . . ? N5 Fe1 N3 167.61(7) . . ? N7 Fe1 N3 89.46(7) . . ? N6 Fe1 N3 76.03(8) . . ? N5 Fe1 N1 87.17(7) . . ? N7 Fe1 N1 74.94(8) . . ? N6 Fe1 N1 171.41(8) . . ? N3 Fe1 N1 104.25(7) . . ? N5 Fe1 N2 75.80(8) . . ? N7 Fe1 N2 174.06(8) . . ? N6 Fe1 N2 83.41(7) . . ? N3 Fe1 N2 96.27(7) . . ? N1 Fe1 N2 105.02(7) . . ? C26 N1 C22 117.5(2) . . ? C26 N1 Fe1 130.87(18) . . ? C22 N1 Fe1 111.65(16) . . ? C19 N2 C15 117.0(2) . . ? C19 N2 Fe1 133.44(17) . . ? C15 N2 Fe1 108.99(16) . . ? C12 N3 C8 117.0(2) . . ? C12 N3 Fe1 131.60(17) . . ? C8 N3 Fe1 111.16(16) . . ? C5 N4 C1 116.5(2) . . ? C5 N4 C3 117.32(19) . . ? C1 N4 C3 117.4(2) . . ? C14 N5 C4 118.6(2) . . ? C14 N5 Fe1 116.19(19) . . ? C4 N5 Fe1 124.69(16) . . ? C7 N6 C6 118.5(2) . . ? C7 N6 Fe1 115.19(17) . . ? C6 N6 Fe1 126.28(16) . . ? C21 N7 C2 117.6(2) . . ? C21 N7 Fe1 117.16(17) . . ? C2 N7 Fe1 125.12(16) . . ? N4 C1 C2 111.2(2) . . ? N4 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N4 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? N7 C2 C1 108.2(2) . . ? N7 C2 H2A 110.1 . . ? C1 C2 H2A 110.1 . . ? N7 C2 H2B 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? N4 C3 C4 112.31(19) . . ? N4 C3 H3A 109.1 . . ? C4 C3 H3A 109.1 . . ? N4 C3 H3B 109.1 . . ? C4 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? N5 C4 C3 108.21(19) . . ? N5 C4 H4A 110.1 . . ? C3 C4 H4A 110.1 . . ? N5 C4 H4B 110.1 . . ? C3 C4 H4B 110.1 . . ? H4A C4 H4B 108.4 . . ? N4 C5 C6 111.7(2) . . ? N4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? N6 C6 C5 109.0(2) . . ? N6 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? N6 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N6 C7 C8 121.2(2) . . ? N6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? N3 C8 C9 123.9(2) . . ? N3 C8 C7 116.3(2) . . ? C9 C8 C7 119.8(2) . . ? C8 C9 C10 118.5(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 118.4(2) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 120.7(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? N3 C12 C11 121.4(2) . . ? N3 C12 C13 118.1(2) . . ? C11 C12 C13 120.5(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 C15 121.3(2) . . ? N5 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? N2 C15 C16 123.4(2) . . ? N2 C15 C14 116.8(2) . . ? C16 C15 C14 119.8(2) . . ? C15 C16 C17 118.9(3) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 C16 118.0(2) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C17 C18 C19 120.9(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? N2 C19 C18 121.8(2) . . ? N2 C19 C20 119.4(2) . . ? C18 C19 C20 118.8(2) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N7 C21 C22 119.8(2) . . ? N7 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? N1 C22 C23 123.7(2) . . ? N1 C22 C21 116.3(2) . . ? C23 C22 C21 119.9(2) . . ? C22 C23 C24 118.2(3) . . ? C22 C23 H23 120.9 . . ? C24 C23 H23 120.9 . . ? C25 C24 C23 118.6(2) . . ? C25 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C24 C25 C26 120.4(2) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? N1 C26 C25 121.6(2) . . ? N1 C26 C27 117.5(2) . . ? C25 C26 C27 120.8(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C107 C102 C103 C104 0.5(4) . . . . ? C108 C102 C103 C104 -178.7(2) . . . . ? C102 C103 C104 C105 0.1(4) . . . . ? C103 C104 C105 C106 -0.4(4) . . . . ? C104 C105 C106 C107 0.0(4) . . . . ? C105 C106 C107 C102 0.7(4) . . . . ? C103 C102 C107 C106 -1.0(4) . . . . ? C108 C102 C107 C106 178.3(2) . . . . ? N5 Fe1 N1 C26 -76.6(2) . . . . ? N7 Fe1 N1 C26 -175.9(2) . . . . ? N3 Fe1 N1 C26 98.6(2) . . . . ? N2 Fe1 N1 C26 -2.1(2) . . . . ? N5 Fe1 N1 C22 101.36(17) . . . . ? N7 Fe1 N1 C22 2.00(16) . . . . ? N3 Fe1 N1 C22 -83.51(17) . . . . ? N2 Fe1 N1 C22 175.84(16) . . . . ? N5 Fe1 N2 C19 -178.8(2) . . . . ? N6 Fe1 N2 C19 -83.6(2) . . . . ? N3 Fe1 N2 C19 -8.5(2) . . . . ? N1 Fe1 N2 C19 98.1(2) . . . . ? N5 Fe1 N2 C15 -8.15(16) . . . . ? N6 Fe1 N2 C15 87.07(16) . . . . ? N3 Fe1 N2 C15 162.17(16) . . . . ? N1 Fe1 N2 C15 -91.22(16) . . . . ? N5 Fe1 N3 C12 144.5(3) . . . . ? N7 Fe1 N3 C12 -86.5(2) . . . . ? N6 Fe1 N3 C12 176.6(2) . . . . ? N1 Fe1 N3 C12 -12.2(2) . . . . ? N2 Fe1 N3 C12 95.0(2) . . . . ? N5 Fe1 N3 C8 -30.0(5) . . . . ? N7 Fe1 N3 C8 98.97(17) . . . . ? N6 Fe1 N3 C8 2.13(16) . . . . ? N1 Fe1 N3 C8 173.28(16) . . . . ? N2 Fe1 N3 C8 -79.45(17) . . . . ? N7 Fe1 N5 C14 -173.23(18) . . . . ? N6 Fe1 N5 C14 -76.14(19) . . . . ? N3 Fe1 N5 C14 -45.0(5) . . . . ? N1 Fe1 N5 C14 112.44(19) . . . . ? N2 Fe1 N5 C14 6.17(18) . . . . ? N7 Fe1 N5 C4 -1.77(18) . . . . ? N6 Fe1 N5 C4 95.31(18) . . . . ? N3 Fe1 N5 C4 126.4(4) . . . . ? N1 Fe1 N5 C4 -76.10(18) . . . . ? N2 Fe1 N5 C4 177.63(19) . . . . ? N5 Fe1 N6 C7 172.4(2) . . . . ? N7 Fe1 N6 C7 -88.9(2) . . . . ? N3 Fe1 N6 C7 -1.07(19) . . . . ? N2 Fe1 N6 C7 97.1(2) . . . . ? N5 Fe1 N6 C6 -9.93(19) . . . . ? N7 Fe1 N6 C6 88.82(19) . . . . ? N3 Fe1 N6 C6 176.6(2) . . . . ? N2 Fe1 N6 C6 -85.20(19) . . . . ? N5 Fe1 N7 C21 -87.51(19) . . . . ? N6 Fe1 N7 C21 178.07(18) . . . . ? N3 Fe1 N7 C21 102.20(19) . . . . ? N1 Fe1 N7 C21 -2.72(18) . . . . ? N5 Fe1 N7 C2 88.78(18) . . . . ? N6 Fe1 N7 C2 -5.64(19) . . . . ? N3 Fe1 N7 C2 -81.51(18) . . . . ? N1 Fe1 N7 C2 173.57(19) . . . . ? C5 N4 C1 C2 83.5(3) . . . . ? C3 N4 C1 C2 -129.7(2) . . . . ? C21 N7 C2 C1 99.4(3) . . . . ? Fe1 N7 C2 C1 -76.8(2) . . . . ? N4 C1 C2 N7 55.8(3) . . . . ? C5 N4 C3 C4 -127.2(2) . . . . ? C1 N4 C3 C4 86.3(3) . . . . ? C14 N5 C4 C3 93.2(3) . . . . ? Fe1 N5 C4 C3 -78.1(2) . . . . ? N4 C3 C4 N5 53.2(3) . . . . ? C1 N4 C5 C6 -130.3(2) . . . . ? C3 N4 C5 C6 82.9(3) . . . . ? C7 N6 C6 C5 103.6(3) . . . . ? Fe1 N6 C6 C5 -74.0(2) . . . . ? N4 C5 C6 N6 54.6(3) . . . . ? C6 N6 C7 C8 -178.0(2) . . . . ? Fe1 N6 C7 C8 -0.1(3) . . . . ? C12 N3 C8 C9 -1.0(4) . . . . ? Fe1 N3 C8 C9 174.4(2) . . . . ? C12 N3 C8 C7 -178.3(2) . . . . ? Fe1 N3 C8 C7 -2.9(3) . . . . ? N6 C7 C8 N3 2.2(4) . . . . ? N6 C7 C8 C9 -175.2(3) . . . . ? N3 C8 C9 C10 -0.8(4) . . . . ? C7 C8 C9 C10 176.4(2) . . . . ? C8 C9 C10 C11 1.7(4) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C8 N3 C12 C11 1.8(4) . . . . ? Fe1 N3 C12 C11 -172.40(19) . . . . ? C8 N3 C12 C13 -178.4(2) . . . . ? Fe1 N3 C12 C13 7.4(3) . . . . ? C10 C11 C12 N3 -0.9(4) . . . . ? C10 C11 C12 C13 179.3(2) . . . . ? C4 N5 C14 C15 -175.3(2) . . . . ? Fe1 N5 C14 C15 -3.3(3) . . . . ? C19 N2 C15 C16 1.0(4) . . . . ? Fe1 N2 C15 C16 -171.5(2) . . . . ? C19 N2 C15 C14 -178.3(2) . . . . ? Fe1 N2 C15 C14 9.3(3) . . . . ? N5 C14 C15 N2 -4.8(4) . . . . ? N5 C14 C15 C16 175.9(2) . . . . ? N2 C15 C16 C17 -0.1(4) . . . . ? C14 C15 C16 C17 179.1(2) . . . . ? C15 C16 C17 C18 -0.3(4) . . . . ? C16 C17 C18 C19 -0.2(4) . . . . ? C15 N2 C19 C18 -1.4(3) . . . . ? Fe1 N2 C19 C18 168.72(18) . . . . ? C15 N2 C19 C20 177.9(2) . . . . ? Fe1 N2 C19 C20 -12.0(3) . . . . ? C17 C18 C19 N2 1.1(4) . . . . ? C17 C18 C19 C20 -178.2(2) . . . . ? C2 N7 C21 C22 -173.5(2) . . . . ? Fe1 N7 C21 C22 3.1(3) . . . . ? C26 N1 C22 C23 -1.5(4) . . . . ? Fe1 N1 C22 C23 -179.7(2) . . . . ? C26 N1 C22 C21 177.0(2) . . . . ? Fe1 N1 C22 C21 -1.2(3) . . . . ? N7 C21 C22 N1 -1.1(3) . . . . ? N7 C21 C22 C23 177.4(2) . . . . ? N1 C22 C23 C24 0.3(4) . . . . ? C21 C22 C23 C24 -178.1(2) . . . . ? C22 C23 C24 C25 0.7(4) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? C22 N1 C26 C25 1.6(4) . . . . ? Fe1 N1 C26 C25 179.42(18) . . . . ? C22 N1 C26 C27 -177.8(2) . . . . ? Fe1 N1 C26 C27 0.1(3) . . . . ? C24 C25 C26 N1 -0.6(4) . . . . ? C24 C25 C26 C27 178.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.617 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.072 _iucr_refine_instructions_details ; TITL test structure: fepitpf6_10k660nm CELL 0.71069 13.2599 16.8595 18.2715 90.000 103.897 90.000 ZERR 4.00 0.0004 0.0004 0.0005 0.000 0.003 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N F P FE UNIT 144 176 32 48 8 4 MERG 2 OMIT -4.00 54.00 FMAP 2 PLAN 45 ACTA BOND $H CONF LIST 6 WPDB -2 L.S. 12 TEMP -263.00 WGHT 0.030100 FVAR 2.03943 N100 3 0.288182 0.484288 -0.110657 11.00000 0.02810 0.02205 = 0.02871 0.00007 0.00905 0.00367 C100 1 0.360705 0.451880 -0.076780 11.00000 0.02041 0.01625 = 0.01985 -0.00086 0.00807 0.00103 C101 1 0.453488 0.410724 -0.034069 11.00000 0.02596 0.02703 = 0.02592 0.00096 0.00361 -0.00051 AFIX 137 H10A 2 0.514856 0.431130 -0.048931 11.00000 0.07955 H10B 2 0.446637 0.353733 -0.044651 11.00000 0.07280 H10C 2 0.461088 0.419755 0.019969 11.00000 0.06200 AFIX 0 C102 1 0.498619 0.114984 0.214594 11.00000 0.01693 0.01203 = 0.01230 0.00431 0.00512 0.00477 C103 1 0.602493 0.094029 0.226558 11.00000 0.01701 0.01248 = 0.01589 0.00147 0.00050 -0.00359 AFIX 43 H103 2 0.652107 0.117234 0.267195 11.00000 -1.20000 AFIX 0 C104 1 0.635043 0.039398 0.179772 11.00000 0.01391 0.01678 = 0.02757 0.00866 0.01054 0.00385 AFIX 43 H104 2 0.706465 0.025674 0.188847 11.00000 -1.20000 AFIX 0 C105 1 0.564057 0.005009 0.120193 11.00000 0.02783 0.01223 = 0.01965 0.00106 0.01452 0.00760 AFIX 43 H105 2 0.586423 -0.031984 0.088175 11.00000 -1.20000 AFIX 0 C106 1 0.461013 0.024930 0.107873 11.00000 0.02335 0.01540 = 0.00935 -0.00103 -0.00163 0.00204 AFIX 43 H106 2 0.411777 0.001622 0.067078 11.00000 -1.20000 AFIX 0 C107 1 0.428197 0.079094 0.154802 11.00000 0.01084 0.01633 = 0.01645 0.00145 0.00043 0.00465 AFIX 43 H107 2 0.356482 0.091822 0.145901 11.00000 -1.20000 AFIX 0 C108 1 0.462480 0.174860 0.263304 11.00000 0.02356 0.01775 = 0.01594 -0.00126 0.00313 0.00318 AFIX 33 H10D 2 0.387553 0.183244 0.244702 11.00000 -1.50000 H10E 2 0.499096 0.225089 0.261731 11.00000 -1.50000 H10F 2 0.477158 0.155404 0.315335 11.00000 -1.50000 AFIX 0 P1 5 0.283304 0.205229 -0.078496 11.00000 0.00960 0.01214 = 0.00957 0.00026 0.00376 -0.00041 F1 4 0.319216 0.131219 -0.023476 11.00000 0.01476 0.01526 = 0.01103 0.00498 0.00384 0.00303 F2 4 0.399456 0.212713 -0.090385 11.00000 0.00844 0.01742 = 0.01244 -0.00083 0.00440 0.00148 F3 4 0.253119 0.146442 -0.149465 11.00000 0.01716 0.01519 = 0.01045 -0.00248 0.00350 -0.00080 F4 4 0.248474 0.279910 -0.132700 11.00000 0.01631 0.01573 = 0.01358 0.00585 0.00435 0.00360 F5 4 0.167872 0.198234 -0.065746 11.00000 0.00892 0.01476 = 0.01318 -0.00045 0.00376 -0.00087 F6 4 0.314634 0.264304 -0.007146 11.00000 0.01063 0.01795 = 0.01259 -0.00504 0.00349 -0.00072 P2 5 0.338851 0.454405 0.206185 11.00000 0.01129 0.01286 = 0.00955 0.00081 0.00202 -0.00136 F7 4 0.296907 0.544176 0.199828 11.00000 0.02285 0.01118 = 0.01397 -0.00233 0.00451 -0.00251 F8 4 0.430010 0.478853 0.277381 11.00000 0.01449 0.03104 = 0.01164 0.00229 -0.00056 -0.00707 F9 4 0.413065 0.475150 0.151105 11.00000 0.02083 0.02091 = 0.01262 0.00298 0.00765 -0.00172 F10 4 0.379550 0.364404 0.213189 11.00000 0.01893 0.01624 = 0.02118 0.00471 0.00965 0.00736 F11 4 0.247301 0.430456 0.135053 11.00000 0.01590 0.01426 = 0.01290 -0.00303 -0.00162 0.00042 F12 4 0.264484 0.434202 0.261460 11.00000 0.01172 0.01556 = 0.01645 0.00025 0.00570 -0.00249 FE1 6 -0.077474 0.247541 0.105019 11.00000 0.00914 0.00995 = 0.00817 -0.00041 0.00261 -0.00051 N1 3 -0.040744 0.335504 0.019770 11.00000 0.01228 0.00963 = 0.00666 -0.00126 0.00269 -0.00006 N2 3 -0.252538 0.265975 0.099679 11.00000 0.01231 0.00950 = 0.00611 0.00123 0.00312 -0.00175 N3 3 -0.095767 0.130160 0.043800 11.00000 0.00827 0.01168 = 0.00910 0.00053 0.00119 -0.00004 N4 3 0.078700 0.256955 0.271132 11.00000 0.00986 0.00877 = 0.01119 0.00035 0.00605 0.00038 N5 3 -0.080418 0.346766 0.177112 11.00000 0.01062 0.01031 = 0.00653 0.00259 0.00139 -0.00042 N6 3 -0.087328 0.161803 0.191489 11.00000 0.00780 0.01274 = 0.00670 -0.00176 0.00251 0.00023 N7 3 0.088064 0.239904 0.118771 11.00000 0.01002 0.00618 = 0.00779 -0.00227 0.00027 0.00164 C1 1 0.176633 0.239936 0.252119 11.00000 0.00789 0.01375 = 0.00923 0.00057 0.00254 -0.00134 AFIX 23 H1A 2 0.221288 0.208451 0.293100 11.00000 -1.20000 H1B 2 0.212961 0.290328 0.247552 11.00000 -1.20000 AFIX 0 C2 1 0.159552 0.193791 0.177792 11.00000 0.00970 0.01067 = 0.01356 0.00234 0.00480 0.00337 AFIX 23 H2A 2 0.226621 0.185936 0.163971 11.00000 -1.20000 H2B 2 0.129356 0.141058 0.183287 11.00000 -1.20000 AFIX 0 C3 1 0.059759 0.338378 0.290322 11.00000 0.00913 0.01070 = 0.01191 -0.00449 0.00368 -0.00135 AFIX 23 H3A 2 0.126150 0.362686 0.317553 11.00000 -1.20000 H3B 2 0.012128 0.338503 0.324561 11.00000 -1.20000 AFIX 0 C4 1 0.012530 0.388224 0.220851 11.00000 0.01200 0.00808 = 0.00932 -0.00164 0.00232 -0.00106 AFIX 23 H4A 2 -0.006802 0.441272 0.236307 11.00000 -1.20000 H4B 2 0.063563 0.395225 0.189727 11.00000 -1.20000 AFIX 0 C5 1 0.036248 0.194768 0.309254 11.00000 0.01307 0.01214 = 0.00683 -0.00138 0.00303 0.00267 AFIX 23 H5A 2 0.042529 0.210301 0.362414 11.00000 -1.20000 H5B 2 0.076926 0.145566 0.309035 11.00000 -1.20000 AFIX 0 C6 1 -0.077386 0.178689 0.271704 11.00000 0.01636 0.00906 = 0.00941 0.00037 0.00465 0.00040 AFIX 23 H6A 2 -0.102539 0.132830 0.296151 11.00000 -1.20000 H6B 2 -0.120038 0.225491 0.277227 11.00000 -1.20000 AFIX 0 C7 1 -0.099687 0.090605 0.169355 11.00000 0.00647 0.01337 = 0.01097 0.00423 0.00388 0.00019 AFIX 43 H7 2 -0.104432 0.050092 0.204510 11.00000 -1.20000 AFIX 0 C8 1 -0.106807 0.069494 0.090681 11.00000 0.00670 0.01479 = 0.00763 0.00135 0.00312 0.00132 C9 1 -0.127982 -0.007699 0.067206 11.00000 0.01144 0.01154 = 0.01336 0.00212 0.00370 0.00053 AFIX 43 H9 2 -0.134143 -0.048059 0.102155 11.00000 -1.20000 AFIX 0 C10 1 -0.140105 -0.025158 -0.008630 11.00000 0.01238 0.01132 = 0.01501 -0.00472 0.00442 -0.00051 AFIX 43 H10 2 -0.156570 -0.077447 -0.027020 11.00000 -1.20000 AFIX 0 C11 1 -0.127778 0.034763 -0.056352 11.00000 0.00988 0.01528 = 0.01110 -0.00095 0.00256 0.00243 AFIX 43 H11 2 -0.134817 0.023763 -0.108330 11.00000 -1.20000 AFIX 0 C12 1 -0.104945 0.111964 -0.029424 11.00000 0.00664 0.01401 = 0.01204 -0.00069 0.00282 0.00183 C13 1 -0.090233 0.177584 -0.082060 11.00000 0.01252 0.01281 = 0.01048 -0.00125 0.00180 -0.00018 AFIX 137 H13A 2 -0.138802 0.220845 -0.079913 11.00000 -1.50000 H13B 2 -0.103534 0.157047 -0.133672 11.00000 -1.50000 H13C 2 -0.018807 0.197475 -0.066778 11.00000 -1.50000 AFIX 0 C14 1 -0.168452 0.364319 0.189062 11.00000 0.01932 0.00956 = 0.00862 0.00126 0.00451 0.00304 AFIX 43 H14 2 -0.173100 0.406200 0.222881 11.00000 -1.20000 AFIX 0 C15 1 -0.262415 0.321403 0.151859 11.00000 0.01135 0.01232 = 0.00686 0.00640 0.00182 0.00358 C16 1 -0.355110 0.338558 0.169666 11.00000 0.01764 0.01442 = 0.00711 -0.00183 0.00539 0.00196 AFIX 43 H16 2 -0.358335 0.377610 0.206517 11.00000 -1.20000 AFIX 0 C17 1 -0.444172 0.297723 0.132774 11.00000 0.00937 0.02296 = 0.01455 0.00176 0.00510 0.00166 AFIX 43 H17 2 -0.509329 0.308017 0.143915 11.00000 -1.20000 AFIX 0 C18 1 -0.435016 0.242464 0.080126 11.00000 0.00964 0.01786 = 0.01199 0.00144 0.00108 -0.00210 AFIX 43 H18 2 -0.494630 0.213743 0.054331 11.00000 -1.20000 AFIX 0 C19 1 -0.339667 0.227656 0.063754 11.00000 0.01364 0.01174 = 0.00588 0.00565 0.00213 0.00083 C20 1 -0.334314 0.167869 0.003657 11.00000 0.01622 0.01476 = 0.01004 -0.00001 0.00318 -0.00057 AFIX 137 H20A 2 -0.288543 0.187768 -0.027095 11.00000 -1.50000 H20B 2 -0.404075 0.159214 -0.028446 11.00000 -1.50000 H20C 2 -0.306836 0.117689 0.027370 11.00000 -1.50000 AFIX 0 C21 1 0.127708 0.281794 0.074654 11.00000 0.00863 0.00905 = 0.01035 -0.00480 0.00189 -0.00018 AFIX 43 H21 2 0.199929 0.278344 0.077014 11.00000 -1.20000 AFIX 0 C22 1 0.061614 0.335198 0.020378 11.00000 0.01178 0.00935 = 0.00783 -0.00575 0.00298 -0.00124 C23 1 0.105172 0.383023 -0.025426 11.00000 0.01094 0.01001 = 0.01107 -0.00280 0.00428 -0.00339 AFIX 43 H23 2 0.177407 0.380643 -0.023275 11.00000 -1.20000 AFIX 0 C24 1 0.040332 0.434678 -0.074705 11.00000 0.01721 0.01001 = 0.00863 -0.00029 0.00561 0.00019 AFIX 43 H24 2 0.067186 0.467993 -0.107447 11.00000 -1.20000 AFIX 0 C25 1 -0.063403 0.436469 -0.074995 11.00000 0.01382 0.00930 = 0.00923 -0.00092 -0.00028 0.00127 AFIX 43 H25 2 -0.108778 0.471707 -0.107890 11.00000 -1.20000 AFIX 0 C26 1 -0.102424 0.386806 -0.027231 11.00000 0.01480 0.00757 = 0.00740 -0.00582 0.00141 -0.00014 C27 1 -0.215423 0.389394 -0.025913 11.00000 0.01308 0.01538 = 0.01130 0.00540 0.00226 0.00087 AFIX 137 H27A 2 -0.245335 0.336132 -0.035290 11.00000 -1.50000 H27B 2 -0.252524 0.425690 -0.065121 11.00000 -1.50000 H27C 2 -0.221993 0.408047 0.023530 11.00000 -1.50000 HKLF 4 REM test structure: fepitpf6_10k660nm REM R1 = 0.0387 for 5002 Fo > 4sig(Fo) and 0.0793 for all 8405 data REM 539 parameters refined using 0 restraints END WGHT 0.0300 0.0000 REM Highest difference peak 0.617, deepest hole -0.659, 1-sigma level 0.072 Q1 1 0.4241 0.2247 0.2277 11.00000 0.05 0.62 Q2 1 0.5330 0.1978 0.3012 11.00000 0.05 0.57 Q3 1 0.4074 0.1487 0.2865 11.00000 0.05 0.47 Q4 1 0.0198 0.2461 0.1094 11.00000 0.05 0.37 Q5 1 0.0968 0.3225 0.0592 11.00000 0.05 0.31 Q6 1 -0.3339 0.1984 0.0354 11.00000 0.05 0.31 Q7 1 -0.1124 0.0848 0.1236 11.00000 0.05 0.28 Q8 1 0.2872 0.2938 -0.0794 11.00000 0.05 0.28 Q9 1 -0.1576 0.2475 0.1111 11.00000 0.05 0.28 Q10 1 -0.0359 0.2024 0.1288 11.00000 0.05 0.28 Q11 1 -0.0692 0.3367 0.0999 11.00000 0.05 0.28 Q12 1 0.5864 0.0222 0.1527 11.00000 0.05 0.26 Q13 1 0.2773 0.2664 -0.0876 11.00000 0.05 0.25 Q14 1 -0.1041 0.3603 -0.0423 11.00000 0.05 0.25 Q15 1 -0.2607 0.3007 0.1211 11.00000 0.05 0.25 Q16 1 0.2675 0.3001 -0.0133 11.00000 0.05 0.25 Q17 1 -0.2081 0.3353 0.1623 11.00000 0.05 0.25 Q18 1 -0.1203 0.2990 0.0905 11.00000 0.05 0.25 Q19 1 -0.2846 0.2433 0.1106 11.00000 0.05 0.25 Q20 1 0.4443 0.4204 0.2682 11.00000 0.05 0.25 Q21 1 0.2439 0.5772 0.2344 11.00000 0.05 0.24 Q22 1 0.0866 0.3758 0.0112 11.00000 0.05 0.24 Q23 1 0.6145 0.0863 0.1833 11.00000 0.05 0.24 Q24 1 0.2962 0.5026 0.1891 11.00000 0.05 0.24 Q25 1 0.3365 0.2438 -0.1216 11.00000 0.05 0.24 Q26 1 0.1171 0.2562 0.1224 11.00000 0.05 0.24 Q27 1 -0.3954 0.3418 0.1414 11.00000 0.05 0.24 Q28 1 0.3109 0.6018 0.1792 11.00000 0.05 0.24 Q29 1 0.5074 -0.0186 0.1472 11.00000 0.05 0.23 Q30 1 -0.0722 0.3822 0.0022 11.00000 0.05 0.23 Q31 1 0.2815 0.4426 0.2391 11.00000 0.05 0.23 Q32 1 0.1201 0.2487 0.2554 11.00000 0.05 0.23 Q33 1 0.0972 0.2042 0.1422 11.00000 0.05 0.23 Q34 1 0.0734 0.4217 -0.0404 11.00000 0.05 0.23 Q35 1 -0.1506 0.4007 -0.0177 11.00000 0.05 0.23 Q36 1 -0.0709 0.0284 0.0781 11.00000 0.05 0.23 Q37 1 -0.1680 0.0204 -0.0271 11.00000 0.05 0.23 Q38 1 -0.3689 0.2636 0.0896 11.00000 0.05 0.23 Q39 1 -0.1261 0.2153 0.1398 11.00000 0.05 0.23 Q40 1 -0.2002 0.2799 0.0866 11.00000 0.05 0.23 Q41 1 -0.3421 0.2570 0.0516 11.00000 0.05 0.23 Q42 1 -0.1417 0.1599 0.2026 11.00000 0.05 0.23 Q43 1 -0.0890 0.2986 0.1448 11.00000 0.05 0.23 Q44 1 -0.0990 0.1803 0.1043 11.00000 0.05 0.23 Q45 1 0.3479 0.2026 -0.0871 11.00000 0.05 0.23 ; _database_code_depnum_ccdc_archive 'CCDC 928910' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_956GuillotICMMO #TrackingRef '956GuillotICMMO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ' C27 H33 Fe N7, 2(F6 P), C7 H8, C2 H3 N ' _chemical_formula_sum 'C36 H44 F12 Fe N8 P2' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 100(1) _chemical_formula_weight 934.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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' F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1026 0.0946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3460 0.8476 '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' _symmetry_int_tables_number 14 _chemical_absolute_configuration . 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 13.3157(4) _cell_length_b 16.9676(6) _cell_length_c 18.1951(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.6200(10) _cell_angle_gamma 90.00 _cell_volume 3995.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9646 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 34.54 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.554 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8764 _exptl_absorpt_correction_T_max 0.9376 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 104190 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0172 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 34.81 _reflns_number_total 14894 _reflns_number_gt 12894 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+3.0226P] 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 14894 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0462 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.1062 _refine_ls_wR_factor_gt 0.0968 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 N100 N 0.29018(12) 0.48505(9) -0.10885(10) 0.0390(3) Uani 1 1 d . . . C100 C 0.36039(12) 0.45188(9) -0.07528(8) 0.0256(3) Uani 1 1 d . . . C101 C 0.44943(12) 0.40932(9) -0.03215(9) 0.0299(3) Uani 1 1 d . . . H10A H 0.4561 0.4185 0.0208 0.045 Uiso 1 1 calc R . . H10B H 0.5106 0.4274 -0.0463 0.045 Uiso 1 1 calc R . . H10C H 0.4405 0.3539 -0.0425 0.045 Uiso 1 1 calc R . . C102 C 0.50076(11) 0.11786(9) 0.21673(8) 0.0254(3) Uani 1 1 d . . . C103 C 0.60448(11) 0.09685(10) 0.23148(10) 0.0310(3) Uani 1 1 d . . . H103 H 0.6514 0.1196 0.2719 0.037 Uiso 1 1 calc R . . C104 C 0.63823(13) 0.04190(11) 0.18584(12) 0.0392(4) Uani 1 1 d . . . H104 H 0.7077 0.0278 0.1962 0.047 Uiso 1 1 calc R . . C105 C 0.56949(17) 0.00806(11) 0.12521(11) 0.0418(4) Uani 1 1 d . . . H105 H 0.5925 -0.0283 0.0946 0.050 Uiso 1 1 calc R . . C106 C 0.46686(17) 0.02853(11) 0.11050(10) 0.0415(4) Uani 1 1 d . . . H106 H 0.4201 0.0059 0.0699 0.050 Uiso 1 1 calc R . . C107 C 0.43311(13) 0.08264(11) 0.15596(10) 0.0345(3) Uani 1 1 d . . . H107 H 0.3634 0.0958 0.1456 0.041 Uiso 1 1 calc R . . C108 C 0.46296(18) 0.17840(12) 0.26427(11) 0.0435(4) Uani 1 1 d . . . H10D H 0.4317 0.2214 0.2328 0.065 Uiso 1 1 calc R . . H10E H 0.5202 0.1976 0.3026 0.065 Uiso 1 1 calc R . . H10F H 0.4129 0.1548 0.2878 0.065 Uiso 1 1 calc R . . P1 P 0.28460(2) 0.202341(19) -0.076664(17) 0.01598(6) Uani 1 1 d . . . F1 F 0.31767(7) 0.12665(6) -0.02466(5) 0.02849(18) Uani 1 1 d . . . F2 F 0.40036(6) 0.20890(6) -0.08841(5) 0.02483(17) Uani 1 1 d . . . F3 F 0.25315(7) 0.14710(6) -0.14949(5) 0.02946(18) Uani 1 1 d . . . F4 F 0.25269(8) 0.27865(6) -0.12796(6) 0.0339(2) Uani 1 1 d . . . F5 F 0.16969(6) 0.19604(5) -0.06410(5) 0.02454(16) Uani 1 1 d . . . F6 F 0.31707(7) 0.25752(6) -0.00306(5) 0.0305(2) Uani 1 1 d . . . P2 P 0.34314(3) 0.45256(2) 0.203538(19) 0.02184(7) Uani 1 1 d . . . F7 F 0.30456(11) 0.54240(6) 0.20140(7) 0.0446(3) Uani 1 1 d . . . F8 F 0.43306(9) 0.47348(11) 0.27544(7) 0.0644(5) Uani 1 1 d . . . F9 F 0.41580(10) 0.47477(8) 0.14854(7) 0.0504(3) Uani 1 1 d . . . F10 F 0.37720(11) 0.36324(8) 0.20603(9) 0.0575(4) Uani 1 1 d . . . F11 F 0.24992(9) 0.43463(7) 0.13292(6) 0.0439(3) Uani 1 1 d . . . F12 F 0.26977(7) 0.43152(6) 0.25903(6) 0.0327(2) Uani 1 1 d . . . Fe1 Fe -0.076055(11) 0.247034(10) 0.104867(9) 0.01162(4) Uani 1 1 d . . . N1 N -0.04062(7) 0.33467(6) 0.01925(6) 0.01610(17) Uani 1 1 d . . . N2 N -0.24902(7) 0.26490(6) 0.09948(6) 0.01565(17) Uani 1 1 d . . . N3 N -0.09325(7) 0.13089(6) 0.04389(5) 0.01493(17) Uani 1 1 d . . . N4 N 0.07985(8) 0.25788(6) 0.27163(6) 0.01783(19) Uani 1 1 d . . . N5 N -0.07854(7) 0.34553(6) 0.17638(5) 0.01515(17) Uani 1 1 d . . . N6 N -0.08501(7) 0.16289(6) 0.19153(5) 0.01422(17) Uani 1 1 d . . . N7 N 0.08804(8) 0.24020(6) 0.11864(6) 0.01534(17) Uani 1 1 d . . . C1 C 0.17667(9) 0.24015(8) 0.25186(7) 0.0178(2) Uani 1 1 d . . . H1A H 0.2199 0.2091 0.2918 0.021 Uiso 1 1 calc R . . H1B H 0.2127 0.2889 0.2472 0.021 Uiso 1 1 calc R . . C2 C 0.15839(9) 0.19454(8) 0.17732(7) 0.0185(3) Uani 1.000(7) 1 d . . . H2A H 0.2235 0.1863 0.1632 0.022 Uiso 1 1 calc R . . H2B H 0.1284 0.1434 0.1830 0.022 Uiso 1 1 calc R . . C3 C 0.06121(9) 0.33880(7) 0.29035(6) 0.0165(2) Uani 1 1 d . . . H3A H 0.1260 0.3629 0.3163 0.020 Uiso 1 1 calc R . . H3B H 0.0151 0.3395 0.3244 0.020 Uiso 1 1 calc R . . C4 C 0.01332(9) 0.38691(7) 0.21937(7) 0.0176(2) Uani 1 1 d . . . H4A H -0.0057 0.4389 0.2337 0.021 Uiso 1 1 calc R . . H4B H 0.0630 0.3931 0.1885 0.021 Uiso 1 1 calc R . . C5 C 0.03691(9) 0.19639(7) 0.31039(6) 0.01637(19) Uani 1 1 d . . . H5A H 0.0419 0.2122 0.3624 0.020 Uiso 1 1 calc R . . H5B H 0.0769 0.1485 0.3110 0.020 Uiso 1 1 calc R . . C6 C -0.07620(9) 0.17996(8) 0.27188(6) 0.0161(2) Uani 1 1 d . . . H6A H -0.1010 0.1354 0.2959 0.019 Uiso 1 1 calc R . . H6B H -0.1182 0.2255 0.2769 0.019 Uiso 1 1 calc R . . C7 C -0.09740(8) 0.09163(7) 0.17008(6) 0.01574(19) Uani 1 1 d . . . H7 H -0.1018 0.0523 0.2048 0.019 Uiso 1 1 calc R . . C8 C -0.10485(9) 0.07112(7) 0.09078(6) 0.01582(19) Uani 1 1 d . . . C9 C -0.12658(10) -0.00580(8) 0.06703(7) 0.0210(2) Uani 1 1 d . . . H9 H -0.1329 -0.0451 0.1013 0.025 Uiso 1 1 calc R . . C10 C -0.13877(11) -0.02305(9) -0.00921(8) 0.0240(2) Uani 1 1 d . . . H10 H -0.1552 -0.0738 -0.0273 0.029 Uiso 1 1 calc R . . C11 C -0.12595(10) 0.03676(9) -0.05741(7) 0.0224(2) Uani 1 1 d . . . H11 H -0.1332 0.0263 -0.1086 0.027 Uiso 1 1 calc R . . C12 C -0.10202(9) 0.11332(8) -0.02959(6) 0.0172(2) Uani 1 1 d . . . C13 C -0.08731(10) 0.17769(8) -0.08227(7) 0.0209(2) Uani 1 1 d . . . H13A H -0.1329 0.2207 -0.0789 0.031 Uiso 1 1 calc R . . H13B H -0.1025 0.1579 -0.1331 0.031 Uiso 1 1 calc R . . H13C H -0.0171 0.1958 -0.0686 0.031 Uiso 1 1 calc R . . C14 C -0.16592(9) 0.36373(8) 0.18863(7) 0.0176(2) Uani 1 1 d . . . H14 H -0.1707 0.4049 0.2214 0.021 Uiso 1 1 calc R . . C15 C -0.25909(9) 0.32017(8) 0.15130(6) 0.0170(2) Uani 1 1 d . . . C16 C -0.35213(10) 0.33768(9) 0.16936(7) 0.0230(2) Uani 1 1 d . . . H16 H -0.3557 0.3762 0.2050 0.028 Uiso 1 1 calc R . . C17 C -0.43988(10) 0.29645(10) 0.13311(8) 0.0254(3) Uani 1 1 d . . . H17 H -0.5033 0.3062 0.1444 0.031 Uiso 1 1 calc R . . C18 C -0.43099(10) 0.24089(9) 0.08012(8) 0.0227(2) Uani 1 1 d . . . H18 H -0.4889 0.2128 0.0551 0.027 Uiso 1 1 calc R . . C19 C -0.33520(9) 0.22640(8) 0.06368(7) 0.0178(2) Uani 1 1 d . . . C20 C -0.32989(10) 0.16743(9) 0.00355(8) 0.0236(2) Uani 1 1 d . . . H20A H -0.2870 0.1876 -0.0278 0.035 Uiso 1 1 calc R . . H20B H -0.3981 0.1578 -0.0268 0.035 Uiso 1 1 calc R . . H20C H -0.3011 0.1191 0.0267 0.035 Uiso 1 1 calc R . . C21 C 0.12780(8) 0.28249(7) 0.07493(6) 0.01618(19) Uani 1 1 d . . . H21 H 0.1983 0.2798 0.0776 0.019 Uiso 1 1 calc R . . C22 C 0.06169(9) 0.33537(7) 0.02048(6) 0.01553(19) Uani 1 1 d . . . C23 C 0.10505(10) 0.38361(8) -0.02496(7) 0.0197(2) Uani 1 1 d . . . H23 H 0.1756 0.3818 -0.0225 0.024 Uiso 1 1 calc R . . C24 C 0.04096(11) 0.43470(8) -0.07428(7) 0.0227(2) Uani 1 1 d . . . H24 H 0.0675 0.4678 -0.1058 0.027 Uiso 1 1 calc R . . C25 C -0.06331(10) 0.43539(8) -0.07547(7) 0.0221(2) Uani 1 1 d . . . H25 H -0.1076 0.4694 -0.1079 0.027 Uiso 1 1 calc R . . C26 C -0.10228(9) 0.38496(8) -0.02800(7) 0.0183(2) Uani 1 1 d . . . C27 C -0.21506(10) 0.38589(10) -0.02847(8) 0.0265(3) Uani 1 1 d . . . H27A H -0.2424 0.3334 -0.0366 0.040 Uiso 1 1 calc R . . H27B H -0.2512 0.4197 -0.0683 0.040 Uiso 1 1 calc R . . H27C H -0.2238 0.4051 0.0192 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N100 0.0364(7) 0.0265(7) 0.0506(9) 0.0000(6) 0.0035(6) 0.0006(6) C100 0.0302(6) 0.0194(6) 0.0288(6) -0.0030(5) 0.0099(5) -0.0042(5) C101 0.0322(7) 0.0217(7) 0.0332(7) -0.0026(5) 0.0025(5) -0.0012(5) C102 0.0282(6) 0.0228(7) 0.0264(6) 0.0063(5) 0.0088(5) 0.0071(5) C103 0.0221(6) 0.0270(7) 0.0426(8) 0.0111(6) 0.0048(5) -0.0015(5) C104 0.0280(7) 0.0336(9) 0.0641(11) 0.0216(8) 0.0270(7) 0.0106(6) C105 0.0659(12) 0.0289(8) 0.0404(9) 0.0115(7) 0.0326(9) 0.0195(8) C106 0.0577(11) 0.0307(9) 0.0306(7) -0.0001(6) -0.0006(7) 0.0106(8) C107 0.0270(6) 0.0326(8) 0.0398(8) 0.0016(6) -0.0004(6) 0.0107(6) C108 0.0648(12) 0.0342(9) 0.0351(8) 0.0029(7) 0.0192(8) 0.0194(9) P1 0.01383(11) 0.01765(15) 0.01802(12) -0.00013(10) 0.00684(9) 0.00070(10) F1 0.0282(4) 0.0301(5) 0.0293(4) 0.0122(3) 0.0110(3) 0.0082(3) F2 0.0169(3) 0.0339(5) 0.0277(4) -0.0015(3) 0.0132(3) 0.0006(3) F3 0.0299(4) 0.0352(5) 0.0227(4) -0.0098(3) 0.0048(3) -0.0007(4) F4 0.0320(4) 0.0262(5) 0.0465(5) 0.0162(4) 0.0154(4) 0.0076(4) F5 0.0143(3) 0.0264(4) 0.0350(4) -0.0022(3) 0.0100(3) -0.0018(3) F6 0.0218(4) 0.0398(5) 0.0333(4) -0.0186(4) 0.0133(3) -0.0076(3) P2 0.02083(14) 0.02486(18) 0.01875(13) 0.00508(12) 0.00247(11) -0.00454(12) F7 0.0754(8) 0.0195(5) 0.0421(6) -0.0059(4) 0.0204(6) -0.0106(5) F8 0.0296(5) 0.1258(13) 0.0310(5) 0.0171(7) -0.0062(4) -0.0355(7) F9 0.0599(7) 0.0617(8) 0.0406(6) 0.0102(5) 0.0338(6) -0.0073(6) F10 0.0603(8) 0.0428(7) 0.0839(9) 0.0303(7) 0.0461(7) 0.0325(6) F11 0.0503(6) 0.0381(6) 0.0320(5) -0.0073(4) -0.0129(4) -0.0035(5) F12 0.0270(4) 0.0358(5) 0.0389(5) 0.0028(4) 0.0153(4) -0.0092(4) Fe1 0.00980(6) 0.01301(8) 0.01311(7) -0.00014(5) 0.00479(5) 0.00011(5) N1 0.0147(4) 0.0177(5) 0.0159(4) -0.0010(3) 0.0036(3) 0.0017(3) N2 0.0140(4) 0.0188(5) 0.0149(4) 0.0018(3) 0.0051(3) 0.0002(3) N3 0.0129(4) 0.0171(5) 0.0161(4) 0.0001(3) 0.0060(3) -0.0007(3) N4 0.0167(4) 0.0152(5) 0.0249(5) 0.0007(4) 0.0115(4) 0.0003(3) N5 0.0150(4) 0.0152(5) 0.0154(4) 0.0005(3) 0.0039(3) -0.0007(3) N6 0.0131(4) 0.0176(5) 0.0135(4) 0.0003(3) 0.0062(3) -0.0003(3) N7 0.0141(4) 0.0166(5) 0.0154(4) -0.0002(3) 0.0037(3) 0.0037(3) C1 0.0116(4) 0.0247(6) 0.0175(5) -0.0002(4) 0.0040(3) 0.0004(4) C2 0.0157(5) 0.0213(7) 0.0188(5) 0.0021(4) 0.0046(4) 0.0074(4) C3 0.0181(4) 0.0160(5) 0.0157(4) -0.0013(4) 0.0043(3) -0.0006(4) C4 0.0181(5) 0.0159(5) 0.0182(5) 0.0003(4) 0.0032(4) -0.0035(4) C5 0.0157(4) 0.0173(5) 0.0165(4) 0.0025(4) 0.0045(3) 0.0002(4) C6 0.0157(4) 0.0205(6) 0.0139(4) 0.0000(4) 0.0069(3) -0.0012(4) C7 0.0149(4) 0.0172(5) 0.0168(4) 0.0018(4) 0.0070(3) -0.0008(4) C8 0.0153(4) 0.0167(5) 0.0171(4) -0.0007(4) 0.0070(3) -0.0007(4) C9 0.0253(5) 0.0177(6) 0.0223(5) -0.0015(4) 0.0098(4) -0.0029(4) C10 0.0304(6) 0.0194(6) 0.0245(6) -0.0059(5) 0.0110(5) -0.0043(5) C11 0.0258(6) 0.0240(6) 0.0196(5) -0.0049(4) 0.0097(4) -0.0035(5) C12 0.0157(4) 0.0208(6) 0.0166(4) -0.0019(4) 0.0071(4) -0.0012(4) C13 0.0244(5) 0.0234(6) 0.0167(5) -0.0013(4) 0.0082(4) -0.0043(5) C14 0.0182(5) 0.0175(6) 0.0177(4) -0.0009(4) 0.0055(4) 0.0028(4) C15 0.0148(4) 0.0204(6) 0.0172(4) 0.0015(4) 0.0065(4) 0.0028(4) C16 0.0189(5) 0.0291(7) 0.0232(5) 0.0007(5) 0.0097(4) 0.0061(5) C17 0.0158(5) 0.0358(8) 0.0274(6) 0.0043(5) 0.0105(4) 0.0044(5) C18 0.0137(4) 0.0303(7) 0.0242(5) 0.0050(5) 0.0051(4) -0.0007(4) C19 0.0147(4) 0.0209(6) 0.0179(5) 0.0032(4) 0.0042(4) -0.0008(4) C20 0.0161(5) 0.0282(7) 0.0252(6) -0.0049(5) 0.0025(4) -0.0023(4) C21 0.0137(4) 0.0187(6) 0.0170(4) -0.0019(4) 0.0051(3) 0.0017(4) C22 0.0152(4) 0.0162(5) 0.0156(4) -0.0016(4) 0.0045(3) 0.0008(4) C23 0.0198(5) 0.0202(6) 0.0204(5) -0.0004(4) 0.0076(4) -0.0015(4) C24 0.0270(6) 0.0209(6) 0.0214(5) 0.0024(4) 0.0079(4) -0.0013(5) C25 0.0248(5) 0.0202(6) 0.0206(5) 0.0034(4) 0.0039(4) 0.0028(5) C26 0.0183(5) 0.0186(6) 0.0176(4) 0.0014(4) 0.0031(4) 0.0029(4) C27 0.0189(5) 0.0326(8) 0.0275(6) 0.0107(5) 0.0047(4) 0.0071(5) _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 N100 C100 1.138(2) . ? C100 C101 1.451(2) . ? C102 C107 1.386(2) . ? C102 C103 1.390(2) . ? C102 C108 1.504(2) . ? C103 C104 1.392(3) . ? C104 C105 1.382(3) . ? C105 C106 1.374(3) . ? C106 C107 1.380(3) . ? P1 F4 1.5942(10) . ? P1 F1 1.5944(9) . ? P1 F3 1.5963(9) . ? P1 F5 1.6030(8) . ? P1 F6 1.6075(9) . ? P1 F2 1.6092(8) . ? P2 F10 1.5794(13) . ? P2 F11 1.5916(10) . ? P2 F8 1.5916(11) . ? P2 F9 1.5923(10) . ? P2 F12 1.6020(10) . ? P2 F7 1.6062(12) . ? Fe1 N5 2.1231(10) . ? Fe1 N7 2.1430(10) . ? Fe1 N6 2.1512(10) . ? Fe1 N3 2.2466(11) . ? Fe1 N1 2.2818(11) . ? Fe1 N2 2.3021(10) . ? N1 C26 1.3449(15) . ? N1 C22 1.3573(14) . ? N2 C19 1.3476(15) . ? N2 C15 1.3587(16) . ? N3 C12 1.3478(15) . ? N3 C8 1.3573(15) . ? N4 C1 1.4492(15) . ? N4 C5 1.4501(15) . ? N4 C3 1.4502(16) . ? N5 C14 1.2732(15) . ? N5 C4 1.4664(15) . ? N6 C7 1.2693(16) . ? N6 C6 1.4677(14) . ? N7 C21 1.2752(15) . ? N7 C2 1.4653(15) . ? C1 C2 1.5305(17) . ? C3 C4 1.5340(17) . ? C5 C6 1.5298(16) . ? C7 C8 1.4647(16) . ? C8 C9 1.3838(18) . ? C9 C10 1.3894(18) . ? C10 C11 1.378(2) . ? C11 C12 1.4034(18) . ? C12 C13 1.4961(18) . ? C14 C15 1.4662(17) . ? C15 C16 1.3866(16) . ? C16 C17 1.388(2) . ? C17 C18 1.373(2) . ? C18 C19 1.3988(17) . ? C19 C20 1.4965(19) . ? C21 C22 1.4665(17) . ? C22 C23 1.3827(17) . ? C23 C24 1.3872(19) . ? C24 C25 1.3835(19) . ? C25 C26 1.3996(18) . ? C26 C27 1.4998(18) . ? 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 N100 C100 C101 179.58(19) . . ? C107 C102 C103 118.22(15) . . ? C107 C102 C108 120.70(15) . . ? C103 C102 C108 121.07(16) . . ? C102 C103 C104 120.16(16) . . ? C105 C104 C103 120.57(15) . . ? C106 C105 C104 119.48(16) . . ? C105 C106 C107 120.06(18) . . ? C106 C107 C102 121.51(15) . . ? F4 P1 F1 179.26(6) . . ? F4 P1 F3 90.53(6) . . ? F1 P1 F3 90.09(5) . . ? F4 P1 F5 90.34(5) . . ? F1 P1 F5 90.07(5) . . ? F3 P1 F5 90.38(5) . . ? F4 P1 F6 89.83(6) . . ? F1 P1 F6 89.56(6) . . ? F3 P1 F6 179.53(6) . . ? F5 P1 F6 89.92(5) . . ? F4 P1 F2 89.86(5) . . ? F1 P1 F2 89.72(5) . . ? F3 P1 F2 90.14(5) . . ? F5 P1 F2 179.43(5) . . ? F6 P1 F2 89.55(5) . . ? F10 P2 F11 90.22(8) . . ? F10 P2 F8 92.01(10) . . ? F11 P2 F8 177.32(9) . . ? F10 P2 F9 91.85(7) . . ? F11 P2 F9 90.67(7) . . ? F8 P2 F9 90.75(7) . . ? F10 P2 F12 88.95(6) . . ? F11 P2 F12 89.47(6) . . ? F8 P2 F12 89.08(6) . . ? F9 P2 F12 179.19(7) . . ? F10 P2 F7 177.95(7) . . ? F11 P2 F7 88.72(7) . . ? F8 P2 F7 89.01(9) . . ? F9 P2 F7 89.91(7) . . ? F12 P2 F7 89.29(6) . . ? N5 Fe1 N7 97.67(4) . . ? N5 Fe1 N6 93.53(4) . . ? N7 Fe1 N6 96.28(4) . . ? N5 Fe1 N3 168.14(4) . . ? N7 Fe1 N3 89.59(4) . . ? N6 Fe1 N3 76.29(4) . . ? N5 Fe1 N1 86.62(4) . . ? N7 Fe1 N1 75.29(4) . . ? N6 Fe1 N1 171.50(4) . . ? N3 Fe1 N1 104.36(4) . . ? N5 Fe1 N2 76.27(4) . . ? N7 Fe1 N2 173.92(4) . . ? N6 Fe1 N2 83.74(4) . . ? N3 Fe1 N2 96.31(4) . . ? N1 Fe1 N2 104.52(4) . . ? C26 N1 C22 117.66(11) . . ? C26 N1 Fe1 131.04(8) . . ? C22 N1 Fe1 111.26(8) . . ? C19 N2 C15 117.27(10) . . ? C19 N2 Fe1 133.33(9) . . ? C15 N2 Fe1 108.82(7) . . ? C12 N3 C8 117.53(11) . . ? C12 N3 Fe1 131.21(9) . . ? C8 N3 Fe1 111.01(7) . . ? C1 N4 C5 116.56(10) . . ? C1 N4 C3 117.79(10) . . ? C5 N4 C3 117.26(9) . . ? C14 N5 C4 118.19(10) . . ? C14 N5 Fe1 116.42(8) . . ? C4 N5 Fe1 124.92(8) . . ? C7 N6 C6 117.93(10) . . ? C7 N6 Fe1 115.62(8) . . ? C6 N6 Fe1 126.44(8) . . ? C21 N7 C2 117.64(10) . . ? C21 N7 Fe1 117.28(8) . . ? C2 N7 Fe1 124.97(8) . . ? N4 C1 C2 111.08(10) . . ? N7 C2 C1 108.62(10) . . ? N4 C3 C4 111.49(10) . . ? N5 C4 C3 108.87(10) . . ? N4 C5 C6 111.51(10) . . ? N6 C6 C5 109.35(9) . . ? N6 C7 C8 120.20(11) . . ? N3 C8 C9 123.70(11) . . ? N3 C8 C7 116.76(11) . . ? C9 C8 C7 119.50(11) . . ? C8 C9 C10 118.50(12) . . ? C11 C10 C9 118.52(13) . . ? C10 C11 C12 120.25(12) . . ? N3 C12 C11 121.45(11) . . ? N3 C12 C13 118.70(11) . . ? C11 C12 C13 119.83(11) . . ? N5 C14 C15 120.34(11) . . ? N2 C15 C16 123.50(12) . . ? N2 C15 C14 117.28(10) . . ? C16 C15 C14 119.21(11) . . ? C15 C16 C17 118.59(13) . . ? C18 C17 C16 118.52(11) . . ? C17 C18 C19 120.30(12) . . ? N2 C19 C18 121.80(12) . . ? N2 C19 C20 119.74(10) . . ? C18 C19 C20 118.45(11) . . ? N7 C21 C22 119.62(10) . . ? N1 C22 C23 123.66(11) . . ? N1 C22 C21 116.51(10) . . ? C23 C22 C21 119.82(10) . . ? C22 C23 C24 118.48(11) . . ? C25 C24 C23 118.54(12) . . ? C24 C25 C26 120.11(12) . . ? N1 C26 C25 121.54(11) . . ? N1 C26 C27 118.04(11) . . ? C25 C26 C27 120.42(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C107 C102 C103 C104 0.1(2) . . . . ? C108 C102 C103 C104 -178.66(15) . . . . ? C102 C103 C104 C105 0.5(2) . . . . ? C103 C104 C105 C106 -0.6(3) . . . . ? C104 C105 C106 C107 0.2(3) . . . . ? C105 C106 C107 C102 0.4(3) . . . . ? C103 C102 C107 C106 -0.5(3) . . . . ? C108 C102 C107 C106 178.26(17) . . . . ? N5 Fe1 N1 C26 -77.41(11) . . . . ? N7 Fe1 N1 C26 -176.26(12) . . . . ? N3 Fe1 N1 C26 98.03(11) . . . . ? N2 Fe1 N1 C26 -2.54(12) . . . . ? N5 Fe1 N1 C22 100.21(8) . . . . ? N7 Fe1 N1 C22 1.36(8) . . . . ? N3 Fe1 N1 C22 -84.34(8) . . . . ? N2 Fe1 N1 C22 175.08(8) . . . . ? N5 Fe1 N2 C19 -178.79(12) . . . . ? N7 Fe1 N2 C19 -174.2(3) . . . . ? N6 Fe1 N2 C19 -83.60(11) . . . . ? N3 Fe1 N2 C19 -8.19(11) . . . . ? N1 Fe1 N2 C19 98.44(11) . . . . ? N5 Fe1 N2 C15 -8.06(8) . . . . ? N7 Fe1 N2 C15 -3.4(4) . . . . ? N6 Fe1 N2 C15 87.13(8) . . . . ? N3 Fe1 N2 C15 162.54(8) . . . . ? N1 Fe1 N2 C15 -90.83(8) . . . . ? N5 Fe1 N3 C12 145.31(16) . . . . ? N7 Fe1 N3 C12 -86.70(10) . . . . ? N6 Fe1 N3 C12 176.74(10) . . . . ? N1 Fe1 N3 C12 -12.00(10) . . . . ? N2 Fe1 N3 C12 94.78(10) . . . . ? N5 Fe1 N3 C8 -28.6(2) . . . . ? N7 Fe1 N3 C8 99.40(8) . . . . ? N6 Fe1 N3 C8 2.83(7) . . . . ? N1 Fe1 N3 C8 174.09(7) . . . . ? N2 Fe1 N3 C8 -79.13(8) . . . . ? N7 Fe1 N5 C14 -173.54(9) . . . . ? N6 Fe1 N5 C14 -76.71(9) . . . . ? N3 Fe1 N5 C14 -46.2(2) . . . . ? N1 Fe1 N5 C14 111.81(9) . . . . ? N2 Fe1 N5 C14 5.96(9) . . . . ? N7 Fe1 N5 C4 -1.58(9) . . . . ? N6 Fe1 N5 C4 95.25(9) . . . . ? N3 Fe1 N5 C4 125.75(17) . . . . ? N1 Fe1 N5 C4 -76.23(9) . . . . ? N2 Fe1 N5 C4 177.93(10) . . . . ? N5 Fe1 N6 C7 172.37(8) . . . . ? N7 Fe1 N6 C7 -89.50(8) . . . . ? N3 Fe1 N6 C7 -1.46(8) . . . . ? N1 Fe1 N6 C7 -96.9(3) . . . . ? N2 Fe1 N6 C7 96.62(8) . . . . ? N5 Fe1 N6 C6 -8.91(9) . . . . ? N7 Fe1 N6 C6 89.21(9) . . . . ? N3 Fe1 N6 C6 177.25(9) . . . . ? N1 Fe1 N6 C6 81.8(3) . . . . ? N2 Fe1 N6 C6 -84.67(9) . . . . ? N5 Fe1 N7 C21 -86.54(9) . . . . ? N6 Fe1 N7 C21 179.03(9) . . . . ? N3 Fe1 N7 C21 102.87(9) . . . . ? N1 Fe1 N7 C21 -2.10(9) . . . . ? N2 Fe1 N7 C21 -91.1(4) . . . . ? N5 Fe1 N7 C2 89.48(10) . . . . ? N6 Fe1 N7 C2 -4.95(10) . . . . ? N3 Fe1 N7 C2 -81.11(10) . . . . ? N1 Fe1 N7 C2 173.92(10) . . . . ? N2 Fe1 N7 C2 84.9(4) . . . . ? C5 N4 C1 C2 83.65(13) . . . . ? C3 N4 C1 C2 -128.96(12) . . . . ? C21 N7 C2 C1 98.03(12) . . . . ? Fe1 N7 C2 C1 -77.98(12) . . . . ? N4 C1 C2 N7 55.78(13) . . . . ? C1 N4 C3 C4 86.41(13) . . . . ? C5 N4 C3 C4 -126.43(11) . . . . ? C14 N5 C4 C3 93.08(13) . . . . ? Fe1 N5 C4 C3 -78.75(11) . . . . ? N4 C3 C4 N5 53.01(12) . . . . ? C1 N4 C5 C6 -128.85(11) . . . . ? C3 N4 C5 C6 83.58(13) . . . . ? C7 N6 C6 C5 104.01(12) . . . . ? Fe1 N6 C6 C5 -74.68(12) . . . . ? N4 C5 C6 N6 54.01(13) . . . . ? C6 N6 C7 C8 -178.94(10) . . . . ? Fe1 N6 C7 C8 -0.11(13) . . . . ? C12 N3 C8 C9 -1.04(17) . . . . ? Fe1 N3 C8 C9 173.79(10) . . . . ? C12 N3 C8 C7 -178.65(10) . . . . ? Fe1 N3 C8 C7 -3.82(12) . . . . ? N6 C7 C8 N3 2.86(16) . . . . ? N6 C7 C8 C9 -174.86(11) . . . . ? N3 C8 C9 C10 -0.95(19) . . . . ? C7 C8 C9 C10 176.59(12) . . . . ? C8 C9 C10 C11 1.7(2) . . . . ? C9 C10 C11 C12 -0.6(2) . . . . ? C8 N3 C12 C11 2.25(17) . . . . ? Fe1 N3 C12 C11 -171.33(9) . . . . ? C8 N3 C12 C13 -178.68(10) . . . . ? Fe1 N3 C12 C13 7.74(16) . . . . ? C10 C11 C12 N3 -1.49(19) . . . . ? C10 C11 C12 C13 179.45(12) . . . . ? C4 N5 C14 C15 -175.50(10) . . . . ? Fe1 N5 C14 C15 -2.98(15) . . . . ? C19 N2 C15 C16 0.84(18) . . . . ? Fe1 N2 C15 C16 -171.59(10) . . . . ? C19 N2 C15 C14 -178.24(11) . . . . ? Fe1 N2 C15 C14 9.34(13) . . . . ? N5 C14 C15 N2 -5.09(17) . . . . ? N5 C14 C15 C16 175.79(12) . . . . ? N2 C15 C16 C17 0.4(2) . . . . ? C14 C15 C16 C17 179.46(12) . . . . ? C15 C16 C17 C18 -0.9(2) . . . . ? C16 C17 C18 C19 0.3(2) . . . . ? C15 N2 C19 C18 -1.55(17) . . . . ? Fe1 N2 C19 C18 168.58(9) . . . . ? C15 N2 C19 C20 177.29(12) . . . . ? Fe1 N2 C19 C20 -12.59(18) . . . . ? C17 C18 C19 N2 1.0(2) . . . . ? C17 C18 C19 C20 -177.81(13) . . . . ? C2 N7 C21 C22 -173.78(10) . . . . ? Fe1 N7 C21 C22 2.53(15) . . . . ? C26 N1 C22 C23 -1.26(18) . . . . ? Fe1 N1 C22 C23 -179.23(10) . . . . ? C26 N1 C22 C21 177.34(11) . . . . ? Fe1 N1 C22 C21 -0.63(12) . . . . ? N7 C21 C22 N1 -1.20(17) . . . . ? N7 C21 C22 C23 177.46(11) . . . . ? N1 C22 C23 C24 0.50(19) . . . . ? C21 C22 C23 C24 -178.07(12) . . . . ? C22 C23 C24 C25 0.35(19) . . . . ? C23 C24 C25 C26 -0.4(2) . . . . ? C22 N1 C26 C25 1.18(18) . . . . ? Fe1 N1 C26 C25 178.68(9) . . . . ? C22 N1 C26 C27 -178.64(12) . . . . ? Fe1 N1 C26 C27 -1.15(18) . . . . ? C24 C25 C26 N1 -0.4(2) . . . . ? C24 C25 C26 C27 179.44(13) . . . . ? _diffrn_measured_fraction_theta_max 0.859 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.912 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 929981' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_957GuillotICMMO #TrackingRef '957GuillotICMMO.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C27 H33 Fe N7, 2(F6 P), C7 H8, C2 H3 N' _chemical_formula_sum 'C36 H44 F12 Fe N8 P2' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour ? _diffrn_ambient_temperature 293(2) _chemical_formula_weight 934.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0031 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' F F 0.0176 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1026 0.0946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3460 0.8476 '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' _symmetry_int_tables_number 14 _chemical_absolute_configuration . 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 13.4040(5) _cell_length_b 17.4684(6) _cell_length_c 18.3855(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.9340(10) _cell_angle_gamma 90.00 _cell_volume 4211.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9149 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 29.82 _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.8964 _exptl_absorpt_correction_T_max 0.9396 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'kappa X8 APEX II Bruker ICMMO' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 101128 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0209 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 30.56 _reflns_number_total 12799 _reflns_number_gt 8740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1191P)^2^+4.8025P] 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 12799 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2584 _refine_ls_wR_factor_gt 0.2146 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 N100 N 0.2990(5) 0.4850(4) -0.1021(4) 0.131(2) Uani 1 1 d . . . C100 C 0.3628(5) 0.4516(3) -0.0704(4) 0.0889(14) Uani 1 1 d . . . C101 C 0.4474(6) 0.4080(4) -0.0287(4) 0.112(2) Uani 1 1 d . . . H10D H 0.4534 0.4174 0.0235 0.168 Uiso 1 1 calc R . . H10E H 0.5093 0.4232 -0.0433 0.168 Uiso 1 1 calc R . . H10F H 0.4358 0.3544 -0.0386 0.168 Uiso 1 1 calc R . . C102 C 0.5027(13) 0.1225(7) 0.2249(8) 0.168(5) Uani 1 1 d . . . C103 C 0.6141(10) 0.1099(7) 0.2424(7) 0.162(4) Uani 1 1 d . . . H103 H 0.6610 0.1341 0.2796 0.195 Uiso 1 1 calc R . . C104 C 0.6356(13) 0.0553(10) 0.1933(12) 0.212(9) Uani 1 1 d . . . H104 H 0.7037 0.0420 0.1973 0.255 Uiso 1 1 calc R . . C105 C 0.560(2) 0.0163(9) 0.1350(13) 0.272(14) Uani 1 1 d . . . H105 H 0.5781 -0.0221 0.1051 0.326 Uiso 1 1 calc R . . C106 C 0.4765(18) 0.0374(9) 0.1294(11) 0.274(12) Uani 1 1 d . . . H106 H 0.4294 0.0146 0.0913 0.329 Uiso 1 1 calc R . . C107 C 0.4395(10) 0.0868(9) 0.1675(8) 0.189(5) Uani 1 1 d . . . H107 H 0.3703 0.0983 0.1563 0.227 Uiso 1 1 calc R . . C108 C 0.4767(19) 0.1798(12) 0.2655(10) 0.330(12) Uani 1 1 d . . . H10A H 0.4331 0.2150 0.2335 0.495 Uiso 1 1 calc R . . H10B H 0.5370 0.2061 0.2905 0.495 Uiso 1 1 calc R . . H10C H 0.4413 0.1596 0.3016 0.495 Uiso 1 1 calc R . . P1 P 0.29371(8) 0.19540(6) -0.07378(6) 0.0623(3) Uani 1 1 d . . . F1 F 0.3222(3) 0.1184(3) -0.0329(3) 0.1453(17) Uani 1 1 d . . . F2 F 0.4087(2) 0.2046(2) -0.0821(2) 0.1107(11) Uani 1 1 d . . . F3 F 0.2679(4) 0.1507(4) -0.1466(2) 0.171(2) Uani 1 1 d . . . F4 F 0.2687(4) 0.2732(3) -0.1130(4) 0.171(2) Uani 1 1 d . . . F5 F 0.1809(2) 0.1876(2) -0.0632(2) 0.1189(12) Uani 1 1 d . . . F6 F 0.3243(3) 0.2409(3) 0.0026(2) 0.1438(18) Uani 1 1 d . . . P2 P 0.35151(9) 0.45467(7) 0.20316(6) 0.0696(3) Uani 1 1 d . . . F7 F 0.3126(6) 0.5373(3) 0.2078(5) 0.231(4) Uani 1 1 d . . . F8 F 0.4298(5) 0.4759(7) 0.2689(3) 0.318(6) Uani 1 1 d . . . F9 F 0.4155(6) 0.4883(4) 0.1526(3) 0.222(3) Uani 1 1 d . . . F10 F 0.3717(5) 0.3721(3) 0.1922(6) 0.273(5) Uani 1 1 d . . . F11 F 0.2532(5) 0.4424(4) 0.1437(4) 0.209(3) Uani 1 1 d . . . F12 F 0.2835(4) 0.4262(3) 0.2592(3) 0.1553(19) Uani 1 1 d . . . Fe1 Fe -0.07195(3) 0.24830(2) 0.10479(2) 0.04091(14) Uani 1 1 d . . . N1 N -0.0397(2) 0.33552(15) 0.01802(14) 0.0473(6) Uani 1 1 d . . . N2 N -0.2448(2) 0.26675(18) 0.10270(15) 0.0507(6) Uani 1 1 d . . . N3 N -0.08866(19) 0.13346(15) 0.04390(14) 0.0460(5) Uani 1 1 d . . . N4 N 0.0824(2) 0.25773(16) 0.26489(17) 0.0538(6) Uani 1 1 d . . . N5 N -0.0754(2) 0.34436(15) 0.17655(15) 0.0478(6) Uani 1 1 d . . . N6 N -0.0797(2) 0.16361(15) 0.19000(14) 0.0458(5) Uani 1 1 d . . . N7 N 0.09037(19) 0.24451(15) 0.11289(15) 0.0448(5) Uani 1 1 d . . . C1 C 0.1779(3) 0.2434(2) 0.2423(2) 0.0604(9) Uani 1 1 d . . . H1A H 0.2222 0.2136 0.2804 0.073 Uiso 1 1 calc R . . H1B H 0.2114 0.2917 0.2372 0.073 Uiso 1 1 calc R . . C2 C 0.1609(3) 0.2002(2) 0.1690(2) 0.0564(12) Uani 0.992(14) 1 d P . . H2A H 0.2252 0.1934 0.1535 0.068 Uiso 1 1 calc R . . H2B H 0.1324 0.1501 0.1747 0.068 Uiso 1 1 calc R . . C3 C 0.0627(3) 0.3364(2) 0.28503(19) 0.0585(8) Uani 1 1 d . . . H3A H 0.1262 0.3600 0.3097 0.070 Uiso 1 1 calc R . . H3B H 0.0169 0.3360 0.3196 0.070 Uiso 1 1 calc R . . C4 C 0.0153(3) 0.3836(2) 0.2169(2) 0.0572(8) Uani 1 1 d . . . H4A H -0.0030 0.4340 0.2321 0.069 Uiso 1 1 calc R . . H4B H 0.0640 0.3899 0.1849 0.069 Uiso 1 1 calc R . . C5 C 0.0422(3) 0.1977(2) 0.30412(18) 0.0569(8) Uani 1 1 d . . . H5A H 0.0475 0.2128 0.3555 0.068 Uiso 1 1 calc R . . H5B H 0.0827 0.1517 0.3036 0.068 Uiso 1 1 calc R . . C6 C -0.0690(3) 0.1799(2) 0.26960(17) 0.0532(7) Uani 1 1 d . . . H6A H -0.0916 0.1361 0.2943 0.064 Uiso 1 1 calc R . . H6B H -0.1115 0.2233 0.2762 0.064 Uiso 1 1 calc R . . C7 C -0.0940(2) 0.09506(19) 0.16837(18) 0.0503(7) Uani 1 1 d . . . H7 H -0.0989 0.0566 0.2025 0.060 Uiso 1 1 calc R . . C8 C -0.1029(3) 0.07596(19) 0.08970(19) 0.0510(7) Uani 1 1 d . . . C9 C -0.1264(3) 0.0016(2) 0.0667(2) 0.0688(10) Uani 1 1 d . . . H9 H -0.1338 -0.0364 0.1006 0.083 Uiso 1 1 calc R . . C10 C -0.1387(4) -0.0147(3) -0.0081(3) 0.0800(12) Uani 1 1 d . . . H10 H -0.1573 -0.0635 -0.0260 0.096 Uiso 1 1 calc R . . C11 C -0.1229(3) 0.0425(3) -0.0555(2) 0.0708(11) Uani 1 1 d . . . H11 H -0.1296 0.0322 -0.1059 0.085 Uiso 1 1 calc R . . C12 C -0.0965(3) 0.1164(2) -0.02846(19) 0.0543(7) Uani 1 1 d . . . C13 C -0.0778(4) 0.1779(3) -0.0799(2) 0.0710(11) Uani 1 1 d . . . H13A H -0.1259 0.2187 -0.0799 0.106 Uiso 1 1 calc R . . H13B H -0.0855 0.1576 -0.1293 0.106 Uiso 1 1 calc R . . H13C H -0.0098 0.1973 -0.0638 0.106 Uiso 1 1 calc R . . C14 C -0.1618(3) 0.3624(2) 0.1887(2) 0.0573(8) Uani 1 1 d . . . H14 H -0.1668 0.4027 0.2208 0.069 Uiso 1 1 calc R . . C15 C -0.2540(3) 0.3214(2) 0.15358(19) 0.0570(8) Uani 1 1 d . . . C16 C -0.3461(3) 0.3383(3) 0.1729(3) 0.0787(12) Uani 1 1 d . . . H16 H -0.3499 0.3755 0.2085 0.094 Uiso 1 1 calc R . . C17 C -0.4320(3) 0.2991(4) 0.1385(3) 0.0902(15) Uani 1 1 d . . . H17 H -0.4947 0.3094 0.1506 0.108 Uiso 1 1 calc R . . C18 C -0.4243(3) 0.2457(3) 0.0874(3) 0.0758(12) Uani 1 1 d . . . H18 H -0.4818 0.2187 0.0641 0.091 Uiso 1 1 calc R . . C19 C -0.3296(3) 0.2307(2) 0.0691(2) 0.0595(8) Uani 1 1 d . . . C20 C -0.3251(3) 0.1743(3) 0.0095(3) 0.0821(13) Uani 1 1 d . . . H20A H -0.2783 0.1920 -0.0199 0.123 Uiso 1 1 calc R . . H20B H -0.3917 0.1687 -0.0216 0.123 Uiso 1 1 calc R . . H20C H -0.3025 0.1258 0.0314 0.123 Uiso 1 1 calc R . . C21 C 0.1273(2) 0.2884(2) 0.07068(18) 0.0514(7) Uani 1 1 d . . . H21 H 0.1973 0.2884 0.0728 0.062 Uiso 1 1 calc R . . C22 C 0.0617(3) 0.33907(19) 0.01861(18) 0.0508(7) Uani 1 1 d . . . C23 C 0.1036(3) 0.3881(2) -0.0258(2) 0.0685(10) Uani 1 1 d . . . H23 H 0.1736 0.3888 -0.0233 0.082 Uiso 1 1 calc R . . C24 C 0.0406(4) 0.4353(3) -0.0733(2) 0.0768(12) Uani 1 1 d . . . H24 H 0.0668 0.4687 -0.1040 0.092 Uiso 1 1 calc R . . C25 C -0.0620(4) 0.4329(2) -0.0753(2) 0.0707(10) Uani 1 1 d . . . H25 H -0.1060 0.4648 -0.1076 0.085 Uiso 1 1 calc R . . C26 C -0.1006(3) 0.3826(2) -0.02884(19) 0.0562(8) Uani 1 1 d . . . C27 C -0.2132(3) 0.3805(3) -0.0305(3) 0.0867(15) Uani 1 1 d . . . H27A H -0.2339 0.3286 -0.0247 0.130 Uiso 1 1 calc R . . H27B H -0.2497 0.4002 -0.0772 0.130 Uiso 1 1 calc R . . H27C H -0.2279 0.4112 0.0092 0.130 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N100 0.120(5) 0.095(4) 0.176(6) 0.014(4) 0.023(4) -0.002(3) C100 0.102(4) 0.067(3) 0.101(4) -0.006(3) 0.030(3) -0.017(3) C101 0.127(5) 0.083(4) 0.118(5) -0.015(3) 0.007(4) -0.020(4) C102 0.242(14) 0.134(8) 0.155(9) 0.059(7) 0.103(9) 0.092(9) C103 0.161(9) 0.147(8) 0.179(10) 0.077(8) 0.035(7) 0.019(7) C104 0.200(14) 0.172(15) 0.31(2) 0.120(15) 0.157(15) 0.044(11) C105 0.47(4) 0.129(11) 0.31(2) 0.119(13) 0.30(3) 0.134(16) C106 0.45(3) 0.156(12) 0.259(17) 0.110(11) 0.164(19) 0.167(17) C107 0.193(11) 0.180(12) 0.167(11) 0.038(9) -0.025(9) 0.048(9) C108 0.53(4) 0.28(2) 0.225(17) 0.107(17) 0.18(2) 0.09(2) P1 0.0575(5) 0.0637(6) 0.0685(6) -0.0019(4) 0.0198(4) -0.0038(4) F1 0.125(3) 0.127(3) 0.189(4) 0.070(3) 0.044(3) 0.026(2) F2 0.0725(17) 0.152(3) 0.120(2) -0.009(2) 0.0473(17) -0.0032(18) F3 0.153(4) 0.233(6) 0.114(3) -0.093(3) -0.001(3) 0.006(4) F4 0.132(4) 0.111(3) 0.275(7) 0.092(4) 0.053(4) 0.023(3) F5 0.0614(16) 0.121(3) 0.182(4) -0.020(2) 0.0415(19) -0.0168(16) F6 0.091(2) 0.223(5) 0.126(3) -0.090(3) 0.042(2) -0.030(2) P2 0.0746(7) 0.0657(6) 0.0653(6) 0.0092(5) 0.0074(5) -0.0077(5) F7 0.301(8) 0.091(3) 0.344(10) -0.061(4) 0.167(8) -0.044(4) F8 0.204(6) 0.566(15) 0.134(4) 0.131(7) -0.082(4) -0.251(8) F9 0.294(8) 0.245(7) 0.180(5) -0.021(5) 0.171(5) -0.109(6) F10 0.194(6) 0.108(4) 0.574(16) 0.007(6) 0.213(8) 0.047(4) F11 0.198(6) 0.187(5) 0.191(5) 0.027(4) -0.080(4) -0.034(4) F12 0.166(4) 0.176(4) 0.137(3) -0.014(3) 0.062(3) -0.092(3) Fe1 0.0374(2) 0.0448(2) 0.0417(2) 0.00155(15) 0.01100(16) 0.00191(15) N1 0.0520(14) 0.0481(14) 0.0436(12) 0.0041(10) 0.0139(10) 0.0022(11) N2 0.0383(12) 0.0671(17) 0.0478(13) 0.0123(12) 0.0115(10) 0.0077(11) N3 0.0425(12) 0.0475(14) 0.0484(13) -0.0036(10) 0.0107(10) -0.0005(10) N4 0.0518(15) 0.0557(16) 0.0543(15) 0.0020(12) 0.0122(12) -0.0019(12) N5 0.0504(13) 0.0449(14) 0.0484(13) -0.0004(10) 0.0109(11) 0.0061(11) N6 0.0469(13) 0.0502(14) 0.0414(12) 0.0024(10) 0.0113(10) -0.0022(10) N7 0.0375(11) 0.0536(15) 0.0451(12) 0.0006(10) 0.0128(9) 0.0053(10) C1 0.0420(15) 0.076(2) 0.0588(19) 0.0050(16) 0.0011(14) 0.0015(15) C2 0.0427(17) 0.064(2) 0.062(2) 0.0083(16) 0.0108(14) 0.0147(14) C3 0.0615(19) 0.061(2) 0.0507(17) -0.0110(15) 0.0052(14) -0.0089(16) C4 0.0631(19) 0.0482(18) 0.0612(19) -0.0062(14) 0.0148(16) -0.0068(15) C5 0.064(2) 0.061(2) 0.0447(16) 0.0060(14) 0.0067(14) -0.0030(15) C6 0.0607(18) 0.0575(19) 0.0441(15) 0.0040(13) 0.0170(13) -0.0044(15) C7 0.0511(16) 0.0468(17) 0.0538(16) 0.0067(13) 0.0130(13) -0.0012(13) C8 0.0502(16) 0.0494(17) 0.0548(17) -0.0042(13) 0.0142(13) -0.0034(13) C9 0.079(3) 0.055(2) 0.075(2) -0.0089(18) 0.020(2) -0.0106(18) C10 0.098(3) 0.060(2) 0.084(3) -0.025(2) 0.025(2) -0.019(2) C11 0.077(3) 0.072(3) 0.064(2) -0.0215(19) 0.0176(19) -0.012(2) C12 0.0520(17) 0.063(2) 0.0496(16) -0.0107(14) 0.0142(13) -0.0031(14) C13 0.086(3) 0.079(3) 0.0494(18) -0.0096(17) 0.0187(18) -0.014(2) C14 0.0627(19) 0.0535(19) 0.0587(18) 0.0002(15) 0.0191(15) 0.0143(15) C15 0.0499(17) 0.071(2) 0.0529(17) 0.0099(15) 0.0178(14) 0.0169(15) C16 0.062(2) 0.099(3) 0.082(3) 0.004(2) 0.032(2) 0.027(2) C17 0.0444(19) 0.134(5) 0.099(3) 0.008(3) 0.030(2) 0.019(2) C18 0.0377(16) 0.100(3) 0.089(3) 0.014(2) 0.0125(18) 0.0056(18) C19 0.0393(15) 0.077(2) 0.0611(19) 0.0161(17) 0.0072(14) 0.0050(15) C20 0.050(2) 0.102(4) 0.087(3) -0.013(3) -0.0016(19) -0.005(2) C21 0.0418(14) 0.061(2) 0.0556(17) -0.0030(14) 0.0199(13) -0.0004(13) C22 0.0557(17) 0.0504(17) 0.0494(16) -0.0002(13) 0.0176(13) -0.0025(13) C23 0.071(2) 0.069(2) 0.072(2) 0.0082(19) 0.0299(19) -0.0098(19) C24 0.091(3) 0.075(3) 0.071(2) 0.021(2) 0.031(2) -0.005(2) C25 0.090(3) 0.065(2) 0.058(2) 0.0195(17) 0.017(2) 0.008(2) C26 0.0609(19) 0.059(2) 0.0483(16) 0.0102(14) 0.0117(14) 0.0067(15) C27 0.065(2) 0.106(4) 0.087(3) 0.041(3) 0.010(2) 0.022(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 N100 C100 1.097(8) . ? C100 C101 1.448(9) . ? C102 C108 1.338(19) . ? C102 C107 1.360(17) . ? C102 C103 1.477(17) . ? C103 C104 1.38(2) . ? C104 C105 1.48(3) . ? C105 C106 1.16(3) . ? C106 C107 1.275(18) . ? P1 F3 1.528(4) . ? P1 F4 1.543(4) . ? P1 F1 1.550(4) . ? P1 F5 1.571(3) . ? P1 F2 1.588(3) . ? P1 F6 1.591(4) . ? P2 F8 1.475(4) . ? P2 F10 1.488(5) . ? P2 F9 1.509(4) . ? P2 F11 1.543(5) . ? P2 F7 1.542(6) . ? P2 F12 1.590(4) . ? Fe1 N5 2.141(3) . ? Fe1 N7 2.151(2) . ? Fe1 N6 2.173(3) . ? Fe1 N3 2.286(3) . ? Fe1 N1 2.310(3) . ? Fe1 N2 2.331(3) . ? N1 C26 1.340(4) . ? N1 C22 1.358(4) . ? N2 C19 1.335(5) . ? N2 C15 1.360(5) . ? N3 C12 1.346(4) . ? N3 C8 1.349(4) . ? N4 C5 1.440(4) . ? N4 C1 1.447(5) . ? N4 C3 1.461(5) . ? N5 C14 1.265(4) . ? N5 C4 1.457(4) . ? N6 C7 1.264(4) . ? N6 C6 1.469(4) . ? N7 C21 1.263(4) . ? N7 C2 1.467(4) . ? C1 C2 1.520(5) . ? C3 C4 1.525(5) . ? C5 C6 1.526(5) . ? C7 C8 1.465(5) . ? C8 C9 1.382(5) . ? C9 C10 1.381(6) . ? C10 C11 1.370(7) . ? C11 C12 1.402(5) . ? C12 C13 1.488(6) . ? C14 C15 1.457(6) . ? C15 C16 1.386(5) . ? C16 C17 1.376(7) . ? C17 C18 1.343(7) . ? C18 C19 1.403(5) . ? C19 C20 1.484(6) . ? C21 C22 1.458(5) . ? C22 C23 1.380(5) . ? C23 C24 1.361(6) . ? C24 C25 1.369(6) . ? C25 C26 1.397(5) . ? C26 C27 1.504(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N100 C100 C101 179.6(8) . . ? C108 C102 C107 125.7(18) . . ? C108 C102 C103 111.0(19) . . ? C107 C102 C103 122.7(11) . . ? C104 C103 C102 107.3(13) . . ? C103 C104 C105 126.0(17) . . ? C106 C105 C104 115(2) . . ? C105 C106 C107 130(3) . . ? C106 C107 C102 119.1(16) . . ? F3 P1 F4 93.1(4) . . ? F3 P1 F1 88.3(3) . . ? F4 P1 F1 178.1(3) . . ? F3 P1 F5 90.9(3) . . ? F4 P1 F5 90.7(2) . . ? F1 P1 F5 90.6(2) . . ? F3 P1 F2 90.9(3) . . ? F4 P1 F2 89.3(2) . . ? F1 P1 F2 89.4(2) . . ? F5 P1 F2 178.3(2) . . ? F3 P1 F6 178.1(3) . . ? F4 P1 F6 87.9(3) . . ? F1 P1 F6 90.7(3) . . ? F5 P1 F6 90.8(2) . . ? F2 P1 F6 87.5(2) . . ? F8 P2 F10 103.7(6) . . ? F8 P2 F9 90.5(4) . . ? F10 P2 F9 98.7(4) . . ? F8 P2 F11 166.9(6) . . ? F10 P2 F11 85.5(5) . . ? F9 P2 F11 97.4(4) . . ? F8 P2 F7 84.9(6) . . ? F10 P2 F7 170.6(5) . . ? F9 P2 F7 84.9(4) . . ? F11 P2 F7 85.4(4) . . ? F8 P2 F12 87.4(3) . . ? F10 P2 F12 85.9(4) . . ? F9 P2 F12 175.3(3) . . ? F11 P2 F12 84.0(4) . . ? F7 P2 F12 90.7(3) . . ? N5 Fe1 N7 97.57(10) . . ? N5 Fe1 N6 94.53(10) . . ? N7 Fe1 N6 97.34(10) . . ? N5 Fe1 N3 167.78(10) . . ? N7 Fe1 N3 90.12(9) . . ? N6 Fe1 N3 74.99(10) . . ? N5 Fe1 N1 86.54(10) . . ? N7 Fe1 N1 74.76(10) . . ? N6 Fe1 N1 172.10(10) . . ? N3 Fe1 N1 104.71(9) . . ? N5 Fe1 N2 75.75(11) . . ? N7 Fe1 N2 173.16(10) . . ? N6 Fe1 N2 84.86(10) . . ? N3 Fe1 N2 96.71(10) . . ? N1 Fe1 N2 102.98(9) . . ? C26 N1 C22 116.9(3) . . ? C26 N1 Fe1 132.3(2) . . ? C22 N1 Fe1 110.8(2) . . ? C19 N2 C15 117.4(3) . . ? C19 N2 Fe1 133.7(3) . . ? C15 N2 Fe1 108.5(2) . . ? C12 N3 C8 117.4(3) . . ? C12 N3 Fe1 131.2(2) . . ? C8 N3 Fe1 111.1(2) . . ? C5 N4 C1 117.5(3) . . ? C5 N4 C3 116.9(3) . . ? C1 N4 C3 116.9(3) . . ? C14 N5 C4 119.4(3) . . ? C14 N5 Fe1 116.2(2) . . ? C4 N5 Fe1 124.1(2) . . ? C7 N6 C6 118.4(3) . . ? C7 N6 Fe1 116.4(2) . . ? C6 N6 Fe1 125.2(2) . . ? C21 N7 C2 118.3(3) . . ? C21 N7 Fe1 117.3(2) . . ? C2 N7 Fe1 124.1(2) . . ? N4 C1 C2 111.1(3) . . ? N7 C2 C1 108.6(3) . . ? N4 C3 C4 111.5(3) . . ? N5 C4 C3 109.0(3) . . ? N4 C5 C6 112.0(3) . . ? N6 C6 C5 109.8(3) . . ? N6 C7 C8 120.2(3) . . ? N3 C8 C9 124.1(3) . . ? N3 C8 C7 117.0(3) . . ? C9 C8 C7 118.9(3) . . ? C10 C9 C8 118.1(4) . . ? C11 C10 C9 118.8(4) . . ? C10 C11 C12 120.4(4) . . ? N3 C12 C11 121.1(3) . . ? N3 C12 C13 118.6(3) . . ? C11 C12 C13 120.2(3) . . ? N5 C14 C15 121.5(3) . . ? N2 C15 C16 122.6(4) . . ? N2 C15 C14 117.4(3) . . ? C16 C15 C14 120.0(4) . . ? C17 C16 C15 118.7(4) . . ? C18 C17 C16 119.3(4) . . ? C17 C18 C19 120.1(4) . . ? N2 C19 C18 121.8(4) . . ? N2 C19 C20 119.6(3) . . ? C18 C19 C20 118.6(4) . . ? N7 C21 C22 120.8(3) . . ? N1 C22 C23 123.6(3) . . ? N1 C22 C21 116.4(3) . . ? C23 C22 C21 120.0(3) . . ? C24 C23 C22 118.7(4) . . ? C25 C24 C23 119.1(4) . . ? C24 C25 C26 119.9(4) . . ? N1 C26 C25 121.8(4) . . ? N1 C26 C27 118.3(3) . . ? C25 C26 C27 120.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C108 C102 C103 C104 -174.2(10) . . . . ? C107 C102 C103 C104 -2.6(14) . . . . ? C102 C103 C104 C105 -1.0(17) . . . . ? C103 C104 C105 C106 4(2) . . . . ? C104 C105 C106 C107 -3(2) . . . . ? C105 C106 C107 C102 -1(2) . . . . ? C108 C102 C107 C106 174.1(13) . . . . ? C103 C102 C107 C106 3.7(18) . . . . ? N5 Fe1 N1 C26 -79.7(3) . . . . ? N7 Fe1 N1 C26 -178.5(3) . . . . ? N6 Fe1 N1 C26 -177.7(6) . . . . ? N3 Fe1 N1 C26 95.5(3) . . . . ? N2 Fe1 N1 C26 -5.2(3) . . . . ? N5 Fe1 N1 C22 98.0(2) . . . . ? N7 Fe1 N1 C22 -0.8(2) . . . . ? N6 Fe1 N1 C22 0.0(8) . . . . ? N3 Fe1 N1 C22 -86.9(2) . . . . ? N2 Fe1 N1 C22 172.5(2) . . . . ? N5 Fe1 N2 C19 -178.9(3) . . . . ? N7 Fe1 N2 C19 168.1(7) . . . . ? N6 Fe1 N2 C19 -82.9(3) . . . . ? N3 Fe1 N2 C19 -8.7(3) . . . . ? N1 Fe1 N2 C19 98.2(3) . . . . ? N5 Fe1 N2 C15 -6.9(2) . . . . ? N7 Fe1 N2 C15 -19.9(9) . . . . ? N6 Fe1 N2 C15 89.1(2) . . . . ? N3 Fe1 N2 C15 163.3(2) . . . . ? N1 Fe1 N2 C15 -89.8(2) . . . . ? N5 Fe1 N3 C12 146.0(4) . . . . ? N7 Fe1 N3 C12 -84.8(3) . . . . ? N6 Fe1 N3 C12 177.6(3) . . . . ? N1 Fe1 N3 C12 -10.5(3) . . . . ? N2 Fe1 N3 C12 94.8(3) . . . . ? N5 Fe1 N3 C8 -26.5(6) . . . . ? N7 Fe1 N3 C8 102.7(2) . . . . ? N6 Fe1 N3 C8 5.1(2) . . . . ? N1 Fe1 N3 C8 177.0(2) . . . . ? N2 Fe1 N3 C8 -77.7(2) . . . . ? N7 Fe1 N5 C14 -176.7(3) . . . . ? N6 Fe1 N5 C14 -78.7(3) . . . . ? N3 Fe1 N5 C14 -48.1(6) . . . . ? N1 Fe1 N5 C14 109.1(3) . . . . ? N2 Fe1 N5 C14 4.8(2) . . . . ? N7 Fe1 N5 C4 -3.3(3) . . . . ? N6 Fe1 N5 C4 94.8(3) . . . . ? N3 Fe1 N5 C4 125.3(4) . . . . ? N1 Fe1 N5 C4 -77.4(3) . . . . ? N2 Fe1 N5 C4 178.3(3) . . . . ? N5 Fe1 N6 C7 170.4(2) . . . . ? N7 Fe1 N6 C7 -91.4(2) . . . . ? N3 Fe1 N6 C7 -3.2(2) . . . . ? N1 Fe1 N6 C7 -92.1(7) . . . . ? N2 Fe1 N6 C7 95.2(2) . . . . ? N5 Fe1 N6 C6 -10.0(3) . . . . ? N7 Fe1 N6 C6 88.2(3) . . . . ? N3 Fe1 N6 C6 176.4(3) . . . . ? N1 Fe1 N6 C6 87.4(7) . . . . ? N2 Fe1 N6 C6 -85.3(3) . . . . ? N5 Fe1 N7 C21 -83.7(3) . . . . ? N6 Fe1 N7 C21 -179.3(2) . . . . ? N3 Fe1 N7 C21 105.8(3) . . . . ? N1 Fe1 N7 C21 0.6(2) . . . . ? N2 Fe1 N7 C21 -71.0(8) . . . . ? N5 Fe1 N7 C2 89.9(3) . . . . ? N6 Fe1 N7 C2 -5.7(3) . . . . ? N3 Fe1 N7 C2 -80.5(3) . . . . ? N1 Fe1 N7 C2 174.2(3) . . . . ? N2 Fe1 N7 C2 102.7(8) . . . . ? C5 N4 C1 C2 84.0(4) . . . . ? C3 N4 C1 C2 -129.2(3) . . . . ? C21 N7 C2 C1 96.0(4) . . . . ? Fe1 N7 C2 C1 -77.6(3) . . . . ? N4 C1 C2 N7 56.8(4) . . . . ? C5 N4 C3 C4 -127.5(3) . . . . ? C1 N4 C3 C4 85.5(4) . . . . ? C14 N5 C4 C3 94.9(4) . . . . ? Fe1 N5 C4 C3 -78.4(3) . . . . ? N4 C3 C4 N5 54.2(4) . . . . ? C1 N4 C5 C6 -129.1(3) . . . . ? C3 N4 C5 C6 84.1(4) . . . . ? C7 N6 C6 C5 106.4(3) . . . . ? Fe1 N6 C6 C5 -73.2(3) . . . . ? N4 C5 C6 N6 53.8(4) . . . . ? C6 N6 C7 C8 -178.7(3) . . . . ? Fe1 N6 C7 C8 0.9(4) . . . . ? C12 N3 C8 C9 -1.0(5) . . . . ? Fe1 N3 C8 C9 172.6(3) . . . . ? C12 N3 C8 C7 179.9(3) . . . . ? Fe1 N3 C8 C7 -6.4(4) . . . . ? N6 C7 C8 N3 4.1(5) . . . . ? N6 C7 C8 C9 -175.0(3) . . . . ? N3 C8 C9 C10 -1.7(6) . . . . ? C7 C8 C9 C10 177.4(4) . . . . ? C8 C9 C10 C11 2.7(7) . . . . ? C9 C10 C11 C12 -1.1(7) . . . . ? C8 N3 C12 C11 2.7(5) . . . . ? Fe1 N3 C12 C11 -169.5(3) . . . . ? C8 N3 C12 C13 -178.0(3) . . . . ? Fe1 N3 C12 C13 9.9(5) . . . . ? C10 C11 C12 N3 -1.7(6) . . . . ? C10 C11 C12 C13 179.0(4) . . . . ? C4 N5 C14 C15 -175.8(3) . . . . ? Fe1 N5 C14 C15 -2.0(4) . . . . ? C19 N2 C15 C16 2.2(5) . . . . ? Fe1 N2 C15 C16 -171.2(3) . . . . ? C19 N2 C15 C14 -178.3(3) . . . . ? Fe1 N2 C15 C14 8.2(4) . . . . ? N5 C14 C15 N2 -4.9(5) . . . . ? N5 C14 C15 C16 174.6(4) . . . . ? N2 C15 C16 C17 -0.9(7) . . . . ? C14 C15 C16 C17 179.6(4) . . . . ? C15 C16 C17 C18 0.0(8) . . . . ? C16 C17 C18 C19 -0.4(8) . . . . ? C15 N2 C19 C18 -2.6(5) . . . . ? Fe1 N2 C19 C18 168.8(3) . . . . ? C15 N2 C19 C20 175.9(4) . . . . ? Fe1 N2 C19 C20 -12.7(5) . . . . ? C17 C18 C19 N2 1.8(7) . . . . ? C17 C18 C19 C20 -176.7(5) . . . . ? C2 N7 C21 C22 -174.3(3) . . . . ? Fe1 N7 C21 C22 -0.2(4) . . . . ? C26 N1 C22 C23 0.2(5) . . . . ? Fe1 N1 C22 C23 -177.9(3) . . . . ? C26 N1 C22 C21 179.1(3) . . . . ? Fe1 N1 C22 C21 1.0(3) . . . . ? N7 C21 C22 N1 -0.6(5) . . . . ? N7 C21 C22 C23 178.4(3) . . . . ? N1 C22 C23 C24 -0.4(6) . . . . ? C21 C22 C23 C24 -179.3(4) . . . . ? C22 C23 C24 C25 0.3(7) . . . . ? C23 C24 C25 C26 0.1(7) . . . . ? C22 N1 C26 C25 0.3(5) . . . . ? Fe1 N1 C26 C25 177.8(3) . . . . ? C22 N1 C26 C27 -179.6(4) . . . . ? Fe1 N1 C26 C27 -2.1(5) . . . . ? C24 C25 C26 N1 -0.4(6) . . . . ? C24 C25 C26 C27 179.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.135 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 929982'