# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Catherine E Housecroft' 'Edwin Constable' 'Markus Neuburger' 'Silvia Schaffner' 'Guoqi Zhang.' _publ_contact_author_name 'Catherine E Housecroft' _publ_contact_author_email CATHERINE.HOUSECROFT@UNIBAS.CH _publ_section_title ; Diastereoselective complex formation with a simple C2-symmetric hexadentate ligand based on a 1,1'-binaphthalene scaffold ; # Attachment 'gq46-RFe.cif' data_gq46_123k _database_code_depnum_ccdc_archive 'CCDC 737256' _audit_creation_date 09-01-05 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'gq46_123k_0m in I-43m' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 30.4864(9) _cell_length_b 30.4864(9) _cell_length_c 30.4864(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 28334.7(14) _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'I 41 3 2 ' _symmetry_space_group_name_Hall 'I 4bd 2c 3' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,y+1/2,z+1/2 y,z,x y+1/2,z+1/2,x+1/2 z,x,y z+1/2,x+1/2,y+1/2 -y+1/4,x+3/4,z+1/4 -y+3/4,x+5/4,z+3/4 -z+1/4,y+3/4,x+1/4 -z+3/4,y+5/4,x+3/4 -x+1/4,z+3/4,y+1/4 -x+3/4,z+5/4,y+3/4 -x+1/2,-y,z+1/2 -x+1,-y+1/2,z+1 -z,x+1/2,-y+1/2 -z+1/2,x+1,-y+1 -x,y+1/2,-z+1/2 -x+1/2,y+1,-z+1 -y+1/2,-z,x+1/2 -y+1,-z+1/2,x+1 -z+1/2,-x,y+1/2 -z+1,-x+1/2,y+1 y+1/4,-x+1/4,z+3/4 y+3/4,-x+3/4,z+5/4 z+1/4,-y+1/4,x+3/4 z+3/4,-y+3/4,x+5/4 x+1/4,-z+1/4,y+3/4 x+3/4,-z+3/4,y+5/4 -y,z+1/2,-x+1/2 -y+1/2,z+1,-x+1 -z+3/4,-y+3/4,-x+3/4 -z+5/4,-y+5/4,-x+5/4 -x+3/4,-z+3/4,-y+3/4 -x+5/4,-z+5/4,-y+5/4 -y+3/4,-x+3/4,-z+3/4 -y+5/4,-x+5/4,-z+5/4 y+1/2,-z+1/2,-x y+1,-z+1,-x+1/2 y+3/4,x+1/4,-z+1/4 y+5/4,x+3/4,-z+3/4 z+3/4,y+1/4,-x+1/4 z+5/4,y+3/4,-x+3/4 x+3/4,z+1/4,-y+1/4 x+5/4,z+3/4,-y+3/4 x+1/2,-y+1/2,-z x+1,-y+1,-z+1/2 z+1/2,-x+1/2,-y z+1,-x+1,-y+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 24 # Given Formula = C42 H32 B2 F8 Fe1 N6 O2 # Dc = 1.24 Fooo = 10704.34 Mu = 3.90 M = 441.10 # Found Formula = C42 H28 B2.00 F8.00 Fe1 N6 O2.00 # Dc = 1.24 FOOO = 10704.34 Mu = 3.89 M = 439.10 _chemical_formula_sum 'C42 H32 B2.00 F8.00 Fe1 N6 O2.00' _chemical_formula_moiety '(C42 H28 Fe N6), 2(B F4), 2(H2 O)' _chemical_compound_source ? _chemical_formula_weight 882.2 _cell_measurement_reflns_used 9103 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _cell_measurement_temperature 123 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_min 0.05 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.25 _exptl_crystal_density_diffrn 1.235 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 10704.337 _exptl_absorpt_coefficient_mu 0.390 # Sheldrick geometric approximatio 0.95 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 0.98 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 80792 _reflns_number_total 4860 _diffrn_reflns_av_R_equivalents 0.064 # Number of reflections with Friedels Law is 2768 # Number of reflections without Friedels Law is 4860 # Theoretical number of reflections is about 2419 _diffrn_reflns_theta_min 1.889 _diffrn_reflns_theta_max 26.390 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.390 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _reflns_limit_h_min -20 _reflns_limit_h_max 22 _reflns_limit_k_min 0 _reflns_limit_k_max 26 _reflns_limit_l_min 2 _reflns_limit_l_max 38 _oxford_diffrn_Wilson_B_factor 3.50 _oxford_diffrn_Wilson_scale 826.74 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.00 _refine_diff_density_max 0.76 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>2.0\s(I) _refine_ls_number_reflns 3554 _refine_ls_number_restraints 562 _refine_ls_number_parameters 387 _oxford_refine_ls_R_factor_ref 0.0763 _refine_ls_wR_factor_ref 0.0796 _refine_ls_goodness_of_fit_ref 1.0281 _refine_ls_shift/su_max 0.006688 # The values computed from all data _oxford_reflns_number_all 4824 _refine_ls_R_factor_all 0.1046 _refine_ls_wR_factor_all 0.1325 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3554 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_gt 0.0796 # The Flack parameter was determined before Friedel pairs were merged _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_abs_structure_details 'Flack (1983), 2092 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.584 0.530 0.241 -0.518E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.51114(3) 0.5000 0.2500 0.0490 1.0000 Uani S T . . . . . N1 N 0.46502(13) 0.45413(10) 0.24970(12) 0.0478 1.0000 Uani . . . . . . . N2 N 0.50891(14) 0.48703(11) 0.18904(11) 0.0520 1.0000 Uani . . . . . . . N3 N 0.56028(14) 0.53653(12) 0.22769(13) 0.0562 1.0000 Uani . . . . . . . C1 C 0.44302(16) 0.43821(13) 0.28451(15) 0.0512 1.0000 Uani . . . . . . . C2 C 0.41018(17) 0.40722(15) 0.28062(17) 0.0562 1.0000 Uani . . . . . . . C3 C 0.39917(16) 0.39153(14) 0.23969(17) 0.0568 1.0000 Uani . . . . . . . C4 C 0.42137(17) 0.40705(14) 0.20294(16) 0.0557 1.0000 Uani . . . . . . . C5 C 0.45391(15) 0.43889(12) 0.21033(13) 0.0474 1.0000 Uani . . . . . . . C6 C 0.47995(17) 0.45829(15) 0.17342(15) 0.0534 1.0000 Uani . . . . . . . C7 C 0.47606(19) 0.45009(15) 0.12896(16) 0.0606 1.0000 Uani . . . . . . . C8 C 0.5030(2) 0.47270(16) 0.10030(16) 0.0654 1.0000 Uani . . . . . . . C9 C 0.5337(2) 0.5022(2) 0.11616(16) 0.0699 1.0000 Uani . . . . . . . C10 C 0.53578(18) 0.50865(15) 0.16139(15) 0.0582 1.0000 Uani . . . . . . . C11 C 0.56693(17) 0.53472(14) 0.18572(16) 0.0586 1.0000 Uani . . . . . . . C12 C 0.5956(2) 0.55089(16) 0.25456(17) 0.0637 1.0000 Uani . . . . . . . C13 C 0.6310(2) 0.52207(18) 0.26116(18) 0.0692 1.0000 Uani . . . . . . . C14 C 0.6651(2) 0.5357(2) 0.2897(2) 0.0765 1.0000 Uani . . . . . . . C15 C 0.7011(3) 0.5073(3) 0.3003(2) 0.0977 1.0000 Uani . . . . . . . C16 C 0.7357(3) 0.5210(4) 0.3243(3) 0.1248 1.0000 Uani . . . . . . . C17 C 0.7350(3) 0.5654(4) 0.3418(4) 0.1356 1.0000 Uani . . . . . . . C18 C 0.7024(3) 0.5931(3) 0.3327(3) 0.1187 1.0000 Uani . . . . . . . C19 C 0.6662(3) 0.5788(2) 0.3067(2) 0.0924 1.0000 Uani . . . . . . . C20 C 0.6286(3) 0.60659(19) 0.2992(2) 0.0860 1.0000 Uani . . . . . . . C21 C 0.5948(2) 0.59237(17) 0.27383(19) 0.0722 1.0000 Uani . . . . . . . B1 B 0.41904(19) 0.41904(19) 0.41904(19) 0.0459 0.5000 Uani DS TU . . . . . B2 B 0.42914(19) 0.42914(19) 0.42914(19) 0.0478 0.5000 Uani DS TU . . . . . B11 B 0.6411(3) 0.4044(2) 0.3895(3) 0.0725 0.5000 Uani D U . . . . . F1 F 0.39227(15) 0.39227(15) 0.39227(15) 0.0475 0.5000 Uani DS TU . . . . . F2 F 0.45598(15) 0.45598(15) 0.45598(15) 0.0561 0.5000 Uani DS TU . . . . . F3 F 0.4536(3) 0.4371(4) 0.3942(3) 0.0641 0.3000 Uani D U . . . . . F4 F 0.43566(14) 0.44168(18) 0.38561(13) 0.0640 0.7000 Uani D U . . . . . F11 F 0.6514(3) 0.3660(2) 0.3652(3) 0.0694 0.5000 Uani D U . . . . . F12 F 0.6584(2) 0.4415(2) 0.3684(3) 0.1004 0.5000 Uani D U . . . . . F13 F 0.5953(2) 0.4094(2) 0.3923(2) 0.0602 0.5000 Uani D U . . . . . F14 F 0.6585(2) 0.4014(2) 0.4322(2) 0.0879 0.5000 Uani D U . . . . . B21 B 0.6334(6) 0.4776(6) 0.0380(5) 0.1239 0.1667 Uani D U . . . . . F21 F 0.6397(5) 0.4639(6) 0.0822(5) 0.1154 0.1670 Uani D U . . . . . F22 F 0.6300(7) 0.5245(6) 0.0369(8) 0.1114 0.1667 Uani D U . . . . . F23 F 0.5927(7) 0.4601(10) 0.0244(9) 0.1360 0.1667 Uani D U . . . . . F24 F 0.6666(8) 0.4584(9) 0.0108(7) 0.1210 0.1667 Uani D U . . . . . O1 O 0.6340(6) 0.4770(6) 0.0392(5) 0.1233 0.1667 Uani . U . . . . . O2 O 0.6333(5) 0.4524(6) 0.0957(5) 0.1029 0.1667 Uani . U . . . . . O3 O 0.5943(14) 0.5054(14) 0.0233(11) 0.1194 0.1670 Uani . U . . . . . O4 O 0.4967(8) 0.5033(8) 0.0033(8) 0.1449 0.4500 Uani S TU . . . . . O5 O 0.5653(19) 0.4969(18) 0.0116(17) 0.1422 0.1500 Uani . U . . . . . O6 O 0.520(2) 0.480(2) -0.020(2) 0.1492 0.1500 Uani S TU . . . . . O8 O 0.5653(17) 0.4347(17) -0.0653(17) 0.1664 0.1500 Uani S TU . . . . . O9 O 0.6784(15) 0.3750 -0.0716(15) 0.1536 0.2000 Uani S TU . . . . . H11 H 0.4497 0.4496 0.3127 0.0616 1.0000 Uiso R . . . . . . H21 H 0.3962 0.3958 0.3060 0.0707 1.0000 Uiso R . . . . . . H31 H 0.3760 0.3709 0.2365 0.0685 1.0000 Uiso R . . . . . . H41 H 0.4155 0.3961 0.1744 0.0716 1.0000 Uiso R . . . . . . H71 H 0.4548 0.4298 0.1186 0.0757 1.0000 Uiso R . . . . . . H81 H 0.5015 0.4674 0.0696 0.0815 1.0000 Uiso R . . . . . . H91 H 0.5520 0.5188 0.0973 0.0820 1.0000 Uiso R . . . . . . H111 H 0.5902 0.5500 0.1717 0.0727 1.0000 Uiso R . . . . . . H151 H 0.7009 0.4774 0.2914 0.1272 1.0000 Uiso R . . . . . . H161 H 0.7603 0.5025 0.3291 0.1203 1.0000 Uiso R . . . . . . H171 H 0.7587 0.5741 0.3600 0.1422 1.0000 Uiso R . . . . . . H181 H 0.7045 0.6221 0.3440 0.1318 1.0000 Uiso R . . . . . . H201 H 0.6292 0.6354 0.3111 0.1164 1.0000 Uiso R . . . . . . H211 H 0.5688 0.6093 0.2713 0.1001 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0720(6) 0.0321(4) 0.0429(4) 0.0116(3) 0.0000 0.0000 N1 0.069(2) 0.0296(14) 0.0443(17) 0.0031(14) -0.0054(18) 0.0089(14) N2 0.079(3) 0.0369(17) 0.0405(17) 0.0104(14) 0.0022(17) 0.0092(17) N3 0.072(2) 0.0383(18) 0.059(2) 0.0177(16) -0.0025(19) -0.0019(18) C1 0.073(3) 0.036(2) 0.045(2) 0.0069(17) 0.002(2) 0.0020(19) C2 0.071(3) 0.041(2) 0.056(3) 0.0115(19) 0.000(2) 0.003(2) C3 0.063(3) 0.038(2) 0.070(3) 0.005(2) 0.004(2) 0.0077(19) C4 0.067(3) 0.041(2) 0.059(3) -0.002(2) -0.007(2) 0.011(2) C5 0.071(3) 0.0318(18) 0.040(2) 0.0069(15) 0.0003(18) 0.0151(18) C6 0.070(3) 0.039(2) 0.051(2) 0.0078(19) -0.008(2) 0.013(2) C7 0.092(4) 0.045(2) 0.045(2) 0.004(2) 0.000(2) 0.017(2) C8 0.097(4) 0.054(3) 0.045(2) 0.0060(19) -0.001(3) 0.021(3) C9 0.083(3) 0.070(3) 0.057(3) 0.019(3) 0.002(2) 0.014(3) C10 0.074(3) 0.049(3) 0.051(2) 0.013(2) 0.006(2) 0.014(2) C11 0.073(3) 0.043(2) 0.060(3) 0.026(2) 0.000(2) -0.008(2) C12 0.084(3) 0.055(3) 0.052(3) 0.023(2) 0.004(2) -0.005(2) C13 0.080(3) 0.062(3) 0.065(3) 0.017(2) 0.003(3) -0.010(3) C14 0.080(4) 0.074(4) 0.075(4) 0.022(3) -0.008(3) -0.020(3) C15 0.097(5) 0.110(5) 0.086(4) 0.017(4) -0.021(4) -0.007(4) C16 0.103(6) 0.142(8) 0.130(7) 0.021(6) -0.032(6) -0.004(5) C17 0.116(7) 0.143(8) 0.148(8) 0.045(7) -0.070(6) -0.036(6) C18 0.136(7) 0.105(6) 0.115(6) 0.015(5) -0.033(6) -0.042(6) C19 0.108(5) 0.080(4) 0.090(4) 0.040(4) -0.028(4) -0.031(4) C20 0.129(6) 0.047(3) 0.082(4) 0.009(3) -0.007(4) -0.021(3) C21 0.099(4) 0.045(3) 0.073(3) 0.013(2) 0.001(3) -0.019(3) B1 0.0459(13) 0.0459(13) 0.0459(13) 0.0063(11) 0.0063(11) 0.0063(11) B2 0.0478(13) 0.0478(13) 0.0478(13) 0.0053(11) 0.0053(11) 0.0053(11) B11 0.069(3) 0.054(3) 0.095(4) 0.015(3) -0.025(3) 0.006(4) F1 0.0475(15) 0.0475(15) 0.0475(15) 0.0053(14) 0.0053(14) 0.0053(14) F2 0.0561(17) 0.0561(17) 0.0561(17) 0.0012(15) 0.0012(15) 0.0012(15) F3 0.042(2) 0.102(4) 0.048(2) 0.0084(19) 0.0007(18) -0.012(3) F4 0.045(2) 0.092(2) 0.0548(14) 0.0272(15) -0.0067(14) -0.015(2) F11 0.061(3) 0.070(3) 0.077(4) 0.011(3) -0.010(3) 0.003(3) F12 0.065(3) 0.068(3) 0.168(5) 0.037(3) -0.032(4) -0.012(3) F13 0.067(3) 0.044(3) 0.070(4) 0.008(3) -0.017(3) -0.001(3) F14 0.093(4) 0.060(3) 0.111(3) -0.014(3) -0.056(3) 0.017(3) B21 0.123(7) 0.142(9) 0.107(7) 0.018(8) 0.020(6) -0.011(7) F21 0.094(9) 0.143(11) 0.110(7) 0.028(8) 0.034(6) 0.000(8) F22 0.092(9) 0.143(9) 0.099(11) 0.033(8) 0.045(8) -0.013(8) F23 0.131(7) 0.147(9) 0.130(9) 0.025(11) 0.007(8) -0.017(7) F24 0.133(9) 0.143(13) 0.087(10) 0.014(11) 0.012(9) -0.004(10) O1 0.158(11) 0.137(9) 0.075(8) -0.034(10) -0.009(8) -0.002(9) O2 0.091(10) 0.106(11) 0.112(8) 0.015(9) 0.035(7) 0.003(9) O3 0.117(8) 0.146(9) 0.095(11) 0.025(10) 0.021(9) -0.016(6) O4 0.145(6) 0.145(6) 0.145(6) 0.023(8) -0.023(8) -0.023(8) O5 0.143(6) 0.144(9) 0.139(12) 0.028(10) -0.014(8) -0.022(7) O6 0.149(8) 0.149(8) 0.149(8) 0.020(7) -0.020(7) -0.020(7) O8 0.17(2) 0.17(2) 0.17(2) -0.03(2) 0.03(2) 0.03(2) O9 0.14(2) 0.18(4) 0.14(2) -0.001(16) 0.09(3) 0.001(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.04582(15) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N3 46_455 1.987(4) yes Fe1 . N1 46_455 1.983(4) yes Fe1 . N2 46_455 1.901(3) yes Fe1 . N1 . 1.983(4) yes Fe1 . N2 . 1.901(3) yes Fe1 . N3 . 1.987(4) yes N1 . C1 . 1.346(6) yes N1 . C5 . 1.331(6) yes N2 . C6 . 1.332(6) yes N2 . C10 . 1.348(6) yes N3 . C11 . 1.297(6) yes N3 . C12 . 1.422(7) yes C1 . C2 . 1.382(7) yes C1 . H11 . 0.950 no C2 . C3 . 1.378(7) yes C2 . H21 . 0.950 no C3 . C4 . 1.392(7) yes C3 . H31 . 0.950 no C4 . C5 . 1.406(7) yes C4 . H41 . 0.950 no C5 . C6 . 1.498(6) yes C6 . C7 . 1.383(7) yes C7 . C8 . 1.383(8) yes C7 . H71 . 0.950 no C8 . C9 . 1.384(9) yes C8 . H81 . 0.950 no C9 . C10 . 1.395(7) yes C9 . H91 . 0.950 no C10 . C11 . 1.443(8) yes C11 . H111 . 0.950 no C12 . C13 . 1.405(8) yes C12 . C21 . 1.395(8) yes C13 . C13 46_455 1.508(11) yes C13 . C14 . 1.418(8) yes C14 . C15 . 1.435(10) yes C14 . C19 . 1.415(10) yes C15 . C16 . 1.349(11) yes C15 . H151 . 0.950 no C16 . C17 . 1.456(15) yes C16 . H161 . 0.950 no C17 . C18 . 1.333(14) yes C17 . H171 . 0.950 no C18 . C19 . 1.426(11) yes C18 . H181 . 0.950 no C19 . C20 . 1.443(11) yes C20 . C21 . 1.359(9) yes C20 . H201 . 0.950 no C21 . H211 . 0.950 no B1 . F3 3_555 1.409(7) yes B1 . F3 5_555 1.409(7) yes B1 . F4 5_555 1.331(4) yes B1 . F4 3_555 1.331(4) yes B1 . F1 . 1.414(8) yes B1 . F2 . 1.950(12) yes B1 . F3 . 1.409(7) yes B1 . F4 . 1.331(4) yes B2 . F4 5_555 1.395(4) yes B2 . F4 3_555 1.395(4) yes B2 . F3 5_555 1.322(7) yes B2 . F3 3_555 1.322(7) yes B2 . F2 . 1.417(8) yes B2 . F3 . 1.322(7) yes B2 . F4 . 1.395(4) yes B11 . F11 . 1.421(8) yes B11 . F12 . 1.404(8) yes B11 . F13 . 1.406(8) yes B11 . F14 . 1.409(8) yes B21 . F21 . 1.423(9) yes B21 . F22 . 1.434(9) yes B21 . F23 . 1.415(9) yes B21 . F24 . 1.434(9) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 46_455 Fe1 . N1 46_455 158.18(16) yes N3 46_455 Fe1 . N2 46_455 78.98(17) yes N1 46_455 Fe1 . N2 46_455 79.84(16) yes N3 46_455 Fe1 . N1 . 98.10(15) yes N1 46_455 Fe1 . N1 . 89.7(2) yes N2 46_455 Fe1 . N1 . 97.23(16) yes N3 46_455 Fe1 . N2 . 104.18(17) yes N1 46_455 Fe1 . N2 . 97.23(16) yes N2 46_455 Fe1 . N2 . 175.9(3) yes N1 . Fe1 . N2 . 79.84(16) yes N3 46_455 Fe1 . N3 . 82.1(2) yes N1 46_455 Fe1 . N3 . 98.10(15) yes N2 46_455 Fe1 . N3 . 104.18(17) yes N1 . Fe1 . N3 . 158.18(16) yes N2 . Fe1 . N3 . 78.98(17) yes Fe1 . N1 . C1 . 127.2(3) yes Fe1 . N1 . C5 . 115.5(3) yes C1 . N1 . C5 . 117.3(4) yes Fe1 . N2 . C6 . 120.7(3) yes Fe1 . N2 . C10 . 119.2(3) yes C6 . N2 . C10 . 120.1(4) yes Fe1 . N3 . C11 . 115.6(3) yes Fe1 . N3 . C12 . 123.1(3) yes C11 . N3 . C12 . 117.6(4) yes N1 . C1 . C2 . 122.7(4) yes N1 . C1 . H11 . 118.4 no C2 . C1 . H11 . 118.9 no C1 . C2 . C3 . 119.5(5) yes C1 . C2 . H21 . 120.3 no C3 . C2 . H21 . 120.2 no C2 . C3 . C4 . 119.5(5) yes C2 . C3 . H31 . 120.3 no C4 . C3 . H31 . 120.2 no C3 . C4 . C5 . 116.7(4) yes C3 . C4 . H41 . 121.8 no C5 . C4 . H41 . 121.5 no C4 . C5 . N1 . 124.4(4) yes C4 . C5 . C6 . 121.7(4) yes N1 . C5 . C6 . 113.9(4) yes C5 . C6 . N2 . 110.0(4) yes C5 . C6 . C7 . 128.2(5) yes N2 . C6 . C7 . 121.7(5) yes C6 . C7 . C8 . 118.6(5) yes C6 . C7 . H71 . 120.2 no C8 . C7 . H71 . 121.2 no C7 . C8 . C9 . 120.3(5) yes C7 . C8 . H81 . 120.6 no C9 . C8 . H81 . 119.1 no C8 . C9 . C10 . 118.0(5) yes C8 . C9 . H91 . 122.3 no C10 . C9 . H91 . 119.7 no C9 . C10 . N2 . 121.4(5) yes C9 . C10 . C11 . 128.1(5) yes N2 . C10 . C11 . 110.4(4) yes C10 . C11 . N3 . 115.3(4) yes C10 . C11 . H111 . 122.0 no N3 . C11 . H111 . 122.7 no N3 . C12 . C13 . 118.1(5) yes N3 . C12 . C21 . 120.6(5) yes C13 . C12 . C21 . 121.3(6) yes C13 46_455 C13 . C12 . 119.6(4) yes C13 46_455 C13 . C14 . 122.5(4) yes C12 . C13 . C14 . 117.9(5) yes C13 . C14 . C15 . 121.6(6) yes C13 . C14 . C19 . 121.0(6) yes C15 . C14 . C19 . 117.3(6) yes C14 . C15 . C16 . 122.3(8) yes C14 . C15 . H151 . 120.6 no C16 . C15 . H151 . 117.1 no C15 . C16 . C17 . 118.4(9) yes C15 . C16 . H161 . 121.1 no C17 . C16 . H161 . 120.6 no C16 . C17 . C18 . 121.6(8) yes C16 . C17 . H171 . 117.6 no C18 . C17 . H171 . 120.9 no C17 . C18 . C19 . 119.9(9) yes C17 . C18 . H181 . 117.6 no C19 . C18 . H181 . 122.5 no C18 . C19 . C14 . 120.4(7) yes C18 . C19 . C20 . 121.6(7) yes C14 . C19 . C20 . 117.9(6) yes C19 . C20 . C21 . 120.4(6) yes C19 . C20 . H201 . 117.8 no C21 . C20 . H201 . 121.8 no C12 . C21 . C20 . 121.0(6) yes C12 . C21 . H211 . 118.3 no C20 . C21 . H211 . 120.4 no F3 3_555 B1 . F3 5_555 108.7(6) yes F3 3_555 B1 . F4 5_555 96.7(6) yes F4 5_555 B1 . F4 3_555 119.41(12) yes F3 3_555 B1 . F1 . 110.2(6) yes F3 5_555 B1 . F1 . 110.2(6) yes F4 5_555 B1 . F1 . 94.4(5) yes F4 3_555 B1 . F1 . 94.4(5) yes F4 5_555 B1 . F2 . 85.6(5) yes F4 3_555 B1 . F2 . 85.6(5) yes F3 3_555 B1 . F3 . 108.7(6) yes F3 5_555 B1 . F3 . 108.7(6) yes F1 . B1 . F3 . 110.2(6) yes F3 3_555 B1 . F4 . 134.6(7) yes F3 5_555 B1 . F4 . 96.7(6) yes F4 5_555 B1 . F4 . 119.41(12) yes F4 3_555 B1 . F4 . 119.41(12) yes F1 . B1 . F4 . 94.4(5) yes F2 . B1 . F4 . 85.6(5) yes F4 5_555 B2 . F4 3_555 110.9(4) yes F4 5_555 B2 . F3 3_555 97.7(7) yes F3 5_555 B2 . F3 3_555 119.88(8) yes F4 5_555 B2 . F1 . 72.0(4) yes F4 3_555 B2 . F1 . 72.0(4) yes F3 5_555 B2 . F1 . 88.0(6) yes F3 3_555 B2 . F1 . 88.0(6) yes F4 5_555 B2 . F2 . 108.0(4) yes F4 3_555 B2 . F2 . 108.0(4) yes F3 5_555 B2 . F2 . 92.0(6) yes F3 3_555 B2 . F2 . 92.0(6) yes F4 5_555 B2 . F3 . 136.9(7) yes F4 3_555 B2 . F3 . 97.7(7) yes F3 5_555 B2 . F3 . 119.88(8) yes F3 3_555 B2 . F3 . 119.88(8) yes F1 . B2 . F3 . 88.0(6) yes F4 5_555 B2 . F4 . 110.9(4) yes F4 3_555 B2 . F4 . 110.9(4) yes F3 5_555 B2 . F4 . 97.7(7) yes F3 3_555 B2 . F4 . 136.9(7) yes F2 . B2 . F3 . 92.0(6) yes F2 . B2 . F4 . 108.0(4) yes F11 . B11 . F12 . 110.0(7) yes F11 . B11 . F13 . 109.9(7) yes F12 . B11 . F13 . 108.4(6) yes F11 . B11 . F14 . 110.0(6) yes F12 . B11 . F14 . 109.5(7) yes F13 . B11 . F14 . 108.9(6) yes F21 . B21 . F22 . 109.1(12) yes F21 . B21 . F23 . 106.5(13) yes F22 . B21 . F23 . 107.9(14) yes F21 . B21 . F24 . 109.4(12) yes F22 . B21 . F24 . 116.4(13) yes F23 . B21 . F24 . 107.1(14) yes _vrf_PLAT430_gq46_123k ; PROBLEM: Short Inter D...A Contact O5 .. O6 .. 1.76 Ang. RESPONSE: Short contacts arise from disorder. ; _vrf_PLAT431_gq46_123k ; PROBLEM: Short Inter HL..A Contact F1 .. F1 .. 1.82 Ang. RESPONSE: Short contacts arise from disorder. ; # end Validation Reply Form # Attachment 'gq55-SFe.cif' data_gq55_123k _database_code_depnum_ccdc_archive 'CCDC 737257' _audit_creation_date 09-02-19 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 'gq55_123k_0ma in P2(1)2(1)2' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 17.8971(6) _cell_length_b 19.2376(7) _cell_length_c 10.9316(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3763.7(2) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 2 ' _symmetry_space_group_name_Hall 'P 2 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x+1/2,y+1/2,-z -x,-y,z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 'International Tables Vol C 4.2.6.8 and 6.1.1.4' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C42 H28 F6 Fe1 N6 P1 # Dc = 1.44 Fooo = 1944.00 Mu = 5.13 M = 817.53 # Found Formula = C42 H28 F12 Fe1 N6 P2 # Dc = 1.70 FOOO = 1944.00 Mu = 5.89 M = 962.50 _chemical_formula_sum 'C42 H28 F12 Fe1 N6 P2' _chemical_formula_moiety 'C42 H28 Fe N6, 2(F6 P)' _chemical_compound_source ? _chemical_formula_weight 962.50 _cell_measurement_reflns_used 9846 _cell_measurement_theta_min 3 _cell_measurement_theta_max 30 _cell_measurement_temperature 123 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_max 0.42 _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.589 # Sheldrick geometric approximatio 0.93 0.98 # No experimental values of Tmin/max available _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.98 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 123 _diffrn_reflns_number 93115 _reflns_number_total 11517 _diffrn_reflns_av_R_equivalents 0.037 # Number of reflections with Friedels Law is 6352 # Number of reflections without Friedels Law is 11517 # Theoretical number of reflections is about 5764 _diffrn_reflns_theta_min 1.863 _diffrn_reflns_theta_max 30.544 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.544 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -25 _reflns_limit_h_max 25 _reflns_limit_k_min 0 _reflns_limit_k_max 27 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 1.42 _oxford_diffrn_Wilson_scale 120.16 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.57 _refine_diff_density_max 0.54 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 9129 _refine_ls_number_restraints 144 _refine_ls_number_parameters 570 _oxford_refine_ls_R_factor_ref 0.0304 _refine_ls_wR_factor_ref 0.0333 _refine_ls_goodness_of_fit_ref 1.2586 _refine_ls_shift/su_max 0.006319 # The values computed from all data _oxford_reflns_number_all 11487 _refine_ls_R_factor_all 0.0391 _refine_ls_wR_factor_all 0.0503 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 10004 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_gt 0.0349 _refine_ls_abs_structure_Flack 0.006(10) _refine_ls_abs_structure_details 'Flack (1983), 5165 Friedel-pairs' # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.132 0.877E-01 0.313E-01 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.5000 0.0000 0.67737(3) 0.0122 1.0000 Uani S T . . . . . Fe2 Fe 0.5000 0.5000 0.73419(3) 0.0133 1.0000 Uani S T . . . . . N1 N 0.42633(8) 0.00504(9) 0.54373(13) 0.0145 1.0000 Uani . . . . . . . N2 N 0.47785(9) 0.09559(8) 0.68095(14) 0.0138 1.0000 Uani . . . . . . . N3 N 0.57182(9) 0.02997(8) 0.80403(14) 0.0145 1.0000 Uani . . . . . . . N4 N 0.52368(9) 0.43440(8) 0.86722(15) 0.0166 1.0000 Uani . . . . . . . N5 N 0.60494(8) 0.50322(9) 0.73050(14) 0.0157 1.0000 Uani . . . . . . . N6 N 0.51333(9) 0.57136(8) 0.60528(14) 0.0161 1.0000 Uani . . . . . . . C1 C 0.47778(10) -0.03292(9) 0.35296(16) 0.0129 1.0000 Uani . . . . . . . C2 C 0.49148(10) -0.08676(9) 0.26591(16) 0.0145 1.0000 Uani . . . . . . . C3 C 0.54681(11) -0.08012(10) 0.17336(18) 0.0182 1.0000 Uani . . . . . . . C4 C 0.56422(13) -0.13475(12) 0.0989(2) 0.0239 1.0000 Uani . . . . . . . C5 C 0.52496(13) -0.19821(11) 0.1102(2) 0.0247 1.0000 Uani . . . . . . . C6 C 0.46942(13) -0.20564(10) 0.1946(2) 0.0227 1.0000 Uani . . . . . . . C7 C 0.45201(11) -0.15067(10) 0.27682(18) 0.0164 1.0000 Uani . . . . . . . C8 C 0.39986(11) -0.15973(10) 0.37306(19) 0.0186 1.0000 Uani . . . . . . . C9 C 0.38923(11) -0.10901(10) 0.45930(18) 0.0165 1.0000 Uani . . . . . . . C10 C 0.42780(10) -0.04527(10) 0.44759(17) 0.0141 1.0000 Uani . . . . . . . C11 C 0.39838(11) 0.06647(10) 0.52342(17) 0.0162 1.0000 Uani . . . . . . . C12 C 0.42448(11) 0.12084(10) 0.60434(17) 0.0156 1.0000 Uani . . . . . . . C13 C 0.40577(12) 0.19061(10) 0.60464(19) 0.0204 1.0000 Uani . . . . . . . C14 C 0.44407(14) 0.23423(10) 0.6834(2) 0.0241 1.0000 Uani . . . . . . . C15 C 0.49911(14) 0.20849(9) 0.76124(17) 0.0209 1.0000 Uani . . . . . . . C16 C 0.51427(10) 0.13735(9) 0.75907(16) 0.0157 1.0000 Uani . . . . . . . C17 C 0.56879(10) 0.09902(10) 0.83294(17) 0.0154 1.0000 Uani . . . . . . . C18 C 0.61310(11) 0.12834(11) 0.92365(18) 0.0187 1.0000 Uani . . . . . . . C19 C 0.66261(12) 0.08585(12) 0.98620(19) 0.0219 1.0000 Uani . . . . . . . C20 C 0.66776(12) 0.01649(11) 0.95453(19) 0.0223 1.0000 Uani . . . . . . . C21 C 0.62163(11) -0.00995(10) 0.86353(18) 0.0187 1.0000 Uani . . . . . . . C31 C 0.47150(11) 0.47136(10) 1.05817(18) 0.0166 1.0000 Uani . . . . . . . C32 C 0.41271(11) 0.46967(10) 1.14613(18) 0.0180 1.0000 Uani . . . . . . . C33 C 0.40376(12) 0.52246(12) 1.23528(19) 0.0229 1.0000 Uani . . . . . . . C34 C 0.34279(13) 0.52264(13) 1.3126(2) 0.0258 1.0000 Uani . . . . . . . C35 C 0.29038(12) 0.46806(13) 1.3071(2) 0.0274 1.0000 Uani . . . . . . . C36 C 0.29814(12) 0.41544(13) 1.2249(2) 0.0265 1.0000 Uani . . . . . . . C37 C 0.35848(12) 0.41524(11) 1.13990(19) 0.0211 1.0000 Uani . . . . . . . C38 C 0.36307(12) 0.36508(11) 1.0460(2) 0.0227 1.0000 Uani . . . . . . . C39 C 0.41728(12) 0.36938(10) 0.95771(19) 0.0205 1.0000 Uani . . . . . . . C40 C 0.47158(11) 0.42260(10) 0.96496(18) 0.0168 1.0000 Uani . . . . . . . C41 C 0.59432(12) 0.42303(10) 0.88557(19) 0.0190 1.0000 Uani . . . . . . . C43 C 0.72197(12) 0.45861(12) 0.8004(2) 0.0230 1.0000 Uani . . . . . . . C44 C 0.75804(11) 0.50616(14) 0.7248(2) 0.0260 1.0000 Uani . . . . . . . C45 C 0.71734(12) 0.55094(12) 0.6512(2) 0.0242 1.0000 Uani . . . . . . . C46 C 0.63971(11) 0.54705(10) 0.65294(18) 0.0178 1.0000 Uani . . . . . . . C47 C 0.58649(11) 0.58575(10) 0.57737(18) 0.0172 1.0000 Uani . . . . . . . C48 C 0.60601(13) 0.63143(11) 0.4850(2) 0.0222 1.0000 Uani . . . . . . . C49 C 0.55013(14) 0.66311(11) 0.4171(2) 0.0244 1.0000 Uani . . . . . . . C50 C 0.47657(13) 0.64961(11) 0.4452(2) 0.0228 1.0000 Uani . . . . . . . C51 C 0.46017(12) 0.60393(10) 0.54077(19) 0.0194 1.0000 Uani . . . . . . . C52 C 0.64421(11) 0.45998(10) 0.80349(18) 0.0180 1.0000 Uani . . . . . . . P1 P 0.25640(3) 0.69799(3) 0.14346(6) 0.0272 1.0000 Uani . . . . . . . P2 P 0.28107(4) 0.72584(3) 0.65048(6) 0.0268 1.0000 Uani D U . . . . . F1 F 0.33697(10) 0.67971(11) 0.1973(3) 0.0807 1.0000 Uani . . . . . . . F2 F 0.17481(9) 0.71600(9) 0.09451(18) 0.0449 1.0000 Uani . . . . . . . F3 F 0.22023(10) 0.64309(9) 0.23629(17) 0.0425 1.0000 Uani . . . . . . . F4 F 0.29152(12) 0.75228(11) 0.0515(2) 0.0634 1.0000 Uani . . . . . . . F5 F 0.24714(15) 0.75773(10) 0.2426(2) 0.0691 1.0000 Uani . . . . . . . F6 F 0.26374(14) 0.63697(10) 0.0455(2) 0.0636 1.0000 Uani . . . . . . . F11 F 0.33280(16) 0.68641(10) 0.7447(2) 0.0806 1.0000 Uani D U . . . . . F12 F 0.23217(15) 0.76607(11) 0.5538(3) 0.0917 1.0000 Uani D U . . . . . F13 F 0.31993(9) 0.79789(8) 0.68568(17) 0.0409 1.0000 Uani D U . . . . . F14 F 0.24236(15) 0.65421(10) 0.6146(2) 0.0783 1.0000 Uani D U . . . . . F15 F 0.22132(17) 0.73902(16) 0.7512(3) 0.1133 1.0000 Uani D U . . . . . F16 F 0.34188(16) 0.71376(13) 0.5496(2) 0.0867 1.0000 Uani D U . . . . . H31 H 0.5718 -0.0376 0.1651 0.0221 1.0000 Uiso R . . . . . . H41 H 0.6027 -0.1291 0.0401 0.0290 1.0000 Uiso R . . . . . . H51 H 0.5376 -0.2349 0.0580 0.0314 1.0000 Uiso R . . . . . . H61 H 0.4424 -0.2474 0.1980 0.0280 1.0000 Uiso R . . . . . . H81 H 0.3733 -0.2011 0.3779 0.0241 1.0000 Uiso R . . . . . . H91 H 0.3566 -0.1173 0.5265 0.0200 1.0000 Uiso R . . . . . . H111 H 0.3662 0.0754 0.4576 0.0200 1.0000 Uiso R . . . . . . H131 H 0.3676 0.2068 0.5534 0.0263 1.0000 Uiso R . . . . . . H141 H 0.4338 0.2816 0.6849 0.0293 1.0000 Uiso R . . . . . . H151 H 0.5247 0.2386 0.8149 0.0267 1.0000 Uiso R . . . . . . H181 H 0.6110 0.1756 0.9421 0.0232 1.0000 Uiso R . . . . . . H191 H 0.6931 0.1051 1.0488 0.0271 1.0000 Uiso R . . . . . . H201 H 0.7025 -0.0131 0.9924 0.0277 1.0000 Uiso R . . . . . . H211 H 0.6248 -0.0569 0.8420 0.0240 1.0000 Uiso R . . . . . . H331 H 0.4402 0.5586 1.2405 0.0282 1.0000 Uiso R . . . . . . H341 H 0.3360 0.5598 1.3694 0.0338 1.0000 Uiso R . . . . . . H351 H 0.2496 0.4686 1.3612 0.0346 1.0000 Uiso R . . . . . . H361 H 0.2638 0.3786 1.2234 0.0334 1.0000 Uiso R . . . . . . H381 H 0.3290 0.3272 1.0438 0.0268 1.0000 Uiso R . . . . . . H391 H 0.4190 0.3380 0.8918 0.0252 1.0000 Uiso R . . . . . . H411 H 0.6116 0.3942 0.9474 0.0234 1.0000 Uiso R . . . . . . H431 H 0.7487 0.4262 0.8478 0.0288 1.0000 Uiso R . . . . . . H441 H 0.8103 0.5080 0.7234 0.0329 1.0000 Uiso R . . . . . . H451 H 0.7419 0.5834 0.5995 0.0298 1.0000 Uiso R . . . . . . H481 H 0.6575 0.6397 0.4698 0.0290 1.0000 Uiso R . . . . . . H491 H 0.5627 0.6936 0.3536 0.0290 1.0000 Uiso R . . . . . . H501 H 0.4381 0.6706 0.4017 0.0294 1.0000 Uiso R . . . . . . H511 H 0.4107 0.5957 0.5616 0.0239 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01355(15) 0.01189(14) 0.01116(14) 0.0000 0.0000 0.00268(15) Fe2 0.01276(15) 0.01355(14) 0.01370(15) 0.0000 0.0000 0.00155(15) N1 0.0129(6) 0.0163(7) 0.0141(6) 0.0002(7) 0.0016(5) -0.0003(6) N2 0.0160(7) 0.0139(6) 0.0114(6) 0.0020(5) 0.0013(5) 0.0022(5) N3 0.0162(7) 0.0151(7) 0.0122(7) 0.0009(6) 0.0012(5) 0.0028(6) N4 0.0193(7) 0.0141(7) 0.0163(7) -0.0016(6) -0.0008(6) 0.0023(6) N5 0.0142(6) 0.0165(6) 0.0163(6) -0.0047(7) 0.0005(5) 0.0012(6) N6 0.0182(9) 0.0144(7) 0.0159(7) -0.0010(5) 0.0016(6) 0.0022(6) C1 0.0143(7) 0.0131(7) 0.0114(7) 0.0020(6) -0.0021(6) -0.0018(6) C2 0.0155(8) 0.0133(7) 0.0147(7) -0.0002(6) -0.0019(7) -0.0002(6) C3 0.0193(8) 0.0182(8) 0.0170(8) 0.0001(7) 0.0003(7) -0.0010(7) C4 0.0269(11) 0.0268(10) 0.0181(9) -0.0029(8) 0.0024(8) 0.0019(8) C5 0.0356(11) 0.0194(9) 0.0191(9) -0.0067(7) -0.0033(8) 0.0054(8) C6 0.0303(10) 0.0136(8) 0.0241(10) -0.0008(7) -0.0072(8) -0.0028(7) C7 0.0175(8) 0.0152(8) 0.0165(8) 0.0010(7) -0.0041(7) -0.0016(7) C8 0.0176(8) 0.0148(8) 0.0233(9) 0.0042(7) -0.0033(7) -0.0042(7) C9 0.0135(8) 0.0178(8) 0.0182(8) 0.0040(7) -0.0014(7) -0.0022(7) C10 0.0128(8) 0.0141(7) 0.0153(8) 0.0018(6) -0.0012(6) 0.0000(6) C11 0.0143(8) 0.0199(9) 0.0144(8) 0.0016(7) 0.0010(7) 0.0032(7) C12 0.0145(8) 0.0178(8) 0.0144(8) 0.0022(7) 0.0014(6) 0.0040(7) C13 0.0254(10) 0.0181(9) 0.0178(8) 0.0030(7) -0.0014(8) 0.0077(7) C14 0.0362(12) 0.0137(8) 0.0223(9) 0.0014(8) -0.0002(9) 0.0072(8) C15 0.0287(9) 0.0161(7) 0.0179(8) -0.0019(6) -0.0023(9) 0.0022(9) C16 0.0185(9) 0.0166(8) 0.0120(7) 0.0010(6) 0.0022(6) 0.0016(6) C17 0.0153(8) 0.0166(8) 0.0143(8) 0.0014(6) 0.0012(6) 0.0014(6) C18 0.0205(9) 0.0198(9) 0.0156(8) -0.0023(7) 0.0005(7) -0.0017(7) C19 0.0205(10) 0.0290(10) 0.0162(9) -0.0006(8) -0.0037(7) -0.0048(8) C20 0.0204(9) 0.0267(11) 0.0198(9) 0.0027(7) -0.0049(7) 0.0024(7) C21 0.0190(8) 0.0197(9) 0.0173(8) 0.0013(7) -0.0010(7) 0.0033(7) C31 0.0183(8) 0.0159(8) 0.0154(8) 0.0037(7) -0.0016(7) -0.0023(7) C32 0.0177(9) 0.0204(8) 0.0159(8) 0.0041(7) -0.0017(7) -0.0026(7) C33 0.0230(9) 0.0282(9) 0.0177(9) 0.0005(8) 0.0017(8) -0.0042(8) C34 0.0249(11) 0.0346(11) 0.0179(9) 0.0022(8) 0.0022(8) 0.0024(8) C35 0.0182(10) 0.0442(13) 0.0198(10) 0.0087(9) 0.0015(8) 0.0008(9) C36 0.0192(10) 0.0362(11) 0.0242(10) 0.0114(9) -0.0038(8) -0.0078(8) C37 0.0189(9) 0.0246(9) 0.0200(9) 0.0084(8) -0.0032(8) -0.0037(7) C38 0.0216(10) 0.0196(9) 0.0268(10) 0.0065(8) -0.0051(8) -0.0054(7) C39 0.0258(10) 0.0149(8) 0.0208(9) 0.0013(7) -0.0069(8) -0.0018(7) C40 0.0191(8) 0.0152(8) 0.0160(8) 0.0041(7) -0.0021(7) 0.0003(7) C41 0.0214(9) 0.0167(8) 0.0189(9) -0.0022(7) -0.0042(7) 0.0033(7) C43 0.0171(9) 0.0289(10) 0.0229(10) -0.0068(8) -0.0058(7) 0.0046(8) C44 0.0132(8) 0.0387(12) 0.0262(9) -0.0062(10) -0.0018(7) 0.0009(9) C45 0.0179(9) 0.0318(11) 0.0229(10) -0.0035(9) 0.0012(8) -0.0048(8) C46 0.0171(9) 0.0194(8) 0.0170(8) -0.0040(7) 0.0010(7) 0.0015(7) C47 0.0154(9) 0.0170(8) 0.0191(9) -0.0045(7) 0.0037(7) 0.0005(7) C48 0.0254(10) 0.0194(9) 0.0217(10) -0.0014(8) 0.0077(8) -0.0019(8) C49 0.0347(11) 0.0189(9) 0.0196(9) 0.0041(8) 0.0065(9) 0.0006(8) C50 0.0291(10) 0.0199(9) 0.0195(9) 0.0043(7) -0.0001(8) 0.0050(8) C51 0.0194(10) 0.0187(9) 0.0202(9) 0.0006(7) 0.0017(7) 0.0031(7) C52 0.0173(9) 0.0183(8) 0.0184(9) -0.0037(7) -0.0027(7) 0.0022(7) P1 0.0224(3) 0.0218(2) 0.0372(3) 0.0017(2) -0.0030(2) -0.0052(2) P2 0.0268(3) 0.0241(3) 0.0294(3) -0.0010(2) -0.0024(2) 0.0002(2) F1 0.0297(9) 0.0555(12) 0.157(3) 0.0486(14) -0.0305(12) -0.0144(8) F2 0.0304(8) 0.0498(10) 0.0546(10) 0.0018(8) -0.0144(8) 0.0015(7) F3 0.0419(9) 0.0402(8) 0.0454(9) 0.0068(7) 0.0068(8) -0.0069(7) F4 0.0552(12) 0.0518(11) 0.0833(17) 0.0316(11) 0.0160(12) -0.0107(10) F5 0.1020(17) 0.0411(10) 0.0641(14) -0.0220(10) -0.0260(14) -0.0105(11) F6 0.0838(16) 0.0470(11) 0.0600(13) -0.0204(10) 0.0348(12) 0.0004(10) F11 0.1249(19) 0.0443(10) 0.0726(14) 0.0284(10) -0.0605(14) -0.0223(12) F12 0.1036(18) 0.0417(11) 0.130(2) -0.0100(12) -0.0879(17) 0.0231(11) F13 0.0416(8) 0.0289(7) 0.0523(10) 0.0018(7) -0.0074(8) -0.0073(6) F14 0.1051(18) 0.0346(9) 0.0952(17) -0.0033(11) -0.0488(15) -0.0195(11) F15 0.1034(19) 0.101(2) 0.135(2) -0.0318(18) 0.0801(19) -0.0416(16) F16 0.113(2) 0.0655(14) 0.0810(16) 0.0014(12) 0.0583(15) 0.0336(13) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.08788(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N3 4_655 1.9753(16) yes Fe1 . N1 4_655 1.9703(15) yes Fe1 . N2 4_655 1.8816(15) yes Fe1 . N1 . 1.9703(15) yes Fe1 . N2 . 1.8816(15) yes Fe1 . N3 . 1.9753(16) yes Fe2 . N6 4_665 1.9818(16) yes Fe2 . N4 4_665 1.9716(16) yes Fe2 . N5 4_665 1.8796(15) yes Fe2 . N4 . 1.9716(16) yes Fe2 . N5 . 1.8796(15) yes Fe2 . N6 . 1.9818(16) yes N1 . C10 . 1.429(2) yes N1 . C11 . 1.302(3) yes N2 . C12 . 1.360(2) yes N2 . C16 . 1.341(2) yes N3 . C17 . 1.366(2) yes N3 . C21 . 1.344(2) yes N4 . C40 . 1.436(3) yes N4 . C41 . 1.299(3) yes N5 . C46 . 1.348(3) yes N5 . C52 . 1.350(3) yes N6 . C47 . 1.373(2) yes N6 . C51 . 1.340(3) yes C1 . C1 4_655 1.496(3) yes C1 . C2 . 1.428(2) yes C1 . C10 . 1.388(3) yes C2 . C3 . 1.421(3) yes C2 . C7 . 1.423(2) yes C3 . C4 . 1.365(3) yes C3 . H31 . 0.936 no C4 . C5 . 1.414(3) yes C4 . H41 . 0.948 no C5 . C6 . 1.364(3) yes C5 . H51 . 0.935 no C6 . C7 . 1.422(3) yes C6 . H61 . 0.939 no C7 . C8 . 1.417(3) yes C8 . C9 . 1.370(3) yes C8 . H81 . 0.928 no C9 . C10 . 1.413(3) yes C9 . H91 . 0.951 no C11 . C12 . 1.447(3) yes C11 . H111 . 0.938 no C12 . C13 . 1.383(3) yes C13 . C14 . 1.384(3) yes C13 . H131 . 0.937 no C14 . C15 . 1.392(3) yes C14 . H141 . 0.930 no C15 . C16 . 1.395(2) yes C15 . H151 . 0.944 no C16 . C17 . 1.466(3) yes C17 . C18 . 1.389(3) yes C18 . C19 . 1.386(3) yes C18 . H181 . 0.932 no C19 . C20 . 1.382(3) yes C19 . H191 . 0.951 no C20 . C21 . 1.389(3) yes C20 . H201 . 0.939 no C21 . H211 . 0.936 no C31 . C31 4_665 1.502(4) yes C31 . C32 . 1.426(3) yes C31 . C40 . 1.385(3) yes C32 . C33 . 1.417(3) yes C32 . C37 . 1.429(3) yes C33 . C34 . 1.380(3) yes C33 . H331 . 0.955 no C34 . C35 . 1.409(3) yes C34 . H341 . 0.954 no C35 . C36 . 1.361(4) yes C35 . H351 . 0.939 no C36 . C37 . 1.424(3) yes C36 . H361 . 0.938 no C37 . C38 . 1.411(3) yes C38 . C39 . 1.371(3) yes C38 . H381 . 0.950 no C39 . C40 . 1.414(3) yes C39 . H391 . 0.941 no C41 . C52 . 1.452(3) yes C41 . H411 . 0.928 no C43 . C44 . 1.391(3) yes C43 . C52 . 1.392(3) yes C43 . H431 . 0.942 no C44 . C45 . 1.386(3) yes C44 . H441 . 0.937 no C45 . C46 . 1.392(3) yes C45 . H451 . 0.949 no C46 . C47 . 1.464(3) yes C47 . C48 . 1.383(3) yes C48 . C49 . 1.386(3) yes C48 . H481 . 0.950 no C49 . C50 . 1.376(3) yes C49 . H491 . 0.937 no C50 . C51 . 1.397(3) yes C50 . H501 . 0.929 no C51 . H511 . 0.927 no P1 . F1 . 1.5967(19) yes P1 . F2 . 1.5934(17) yes P1 . F3 . 1.6013(17) yes P1 . F4 . 1.5798(19) yes P1 . F5 . 1.588(2) yes P1 . F6 . 1.5943(19) yes P2 . F11 . 1.579(2) yes P2 . F12 . 1.575(2) yes P2 . F13 . 1.5977(16) yes P2 . F14 . 1.5915(19) yes P2 . F15 . 1.555(3) yes P2 . F16 . 1.567(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N3 4_655 Fe1 . N1 4_655 160.19(7) yes N3 4_655 Fe1 . N2 4_655 80.63(7) yes N1 4_655 Fe1 . N2 4_655 80.00(7) yes N3 4_655 Fe1 . N1 . 95.66(6) yes N1 4_655 Fe1 . N1 . 84.29(9) yes N2 4_655 Fe1 . N1 . 101.80(7) yes N3 4_655 Fe1 . N2 . 97.68(7) yes N1 4_655 Fe1 . N2 . 101.80(7) yes N2 4_655 Fe1 . N2 . 177.61(10) yes N1 . Fe1 . N2 . 80.00(7) yes N3 4_655 Fe1 . N3 . 90.99(9) yes N1 4_655 Fe1 . N3 . 95.66(6) yes N2 4_655 Fe1 . N3 . 97.68(7) yes N1 . Fe1 . N3 . 160.19(7) yes N2 . Fe1 . N3 . 80.63(7) yes N6 4_665 Fe2 . N4 4_665 160.40(7) yes N6 4_665 Fe2 . N5 4_665 80.89(7) yes N4 4_665 Fe2 . N5 4_665 79.75(7) yes N6 4_665 Fe2 . N4 . 96.14(6) yes N4 4_665 Fe2 . N4 . 84.95(9) yes N5 4_665 Fe2 . N4 . 102.09(7) yes N6 4_665 Fe2 . N5 . 97.35(7) yes N4 4_665 Fe2 . N5 . 102.09(7) yes N5 4_665 Fe2 . N5 . 177.54(9) yes N4 . Fe2 . N5 . 79.75(7) yes N6 4_665 Fe2 . N6 . 89.35(9) yes N4 4_665 Fe2 . N6 . 96.14(6) yes N5 4_665 Fe2 . N6 . 97.35(7) yes N4 . Fe2 . N6 . 160.40(7) yes N5 . Fe2 . N6 . 80.89(7) yes Fe1 . N1 . C10 . 119.98(12) yes Fe1 . N1 . C11 . 115.34(13) yes C10 . N1 . C11 . 119.76(16) yes Fe1 . N2 . C12 . 118.96(13) yes Fe1 . N2 . C16 . 119.75(13) yes C12 . N2 . C16 . 121.29(16) yes Fe1 . N3 . C17 . 114.83(12) yes Fe1 . N3 . C21 . 127.15(13) yes C17 . N3 . C21 . 118.02(17) yes Fe2 . N4 . C40 . 120.69(12) yes Fe2 . N4 . C41 . 115.53(14) yes C40 . N4 . C41 . 119.38(17) yes Fe2 . N5 . C46 . 119.70(13) yes Fe2 . N5 . C52 . 119.16(14) yes C46 . N5 . C52 . 121.12(17) yes Fe2 . N6 . C47 . 114.37(13) yes Fe2 . N6 . C51 . 127.79(14) yes C47 . N6 . C51 . 117.78(17) yes C1 4_655 C1 . C2 . 121.54(15) yes C1 4_655 C1 . C10 . 119.18(14) yes C2 . C1 . C10 . 118.90(16) yes C1 . C2 . C3 . 121.93(16) yes C1 . C2 . C7 . 119.06(16) yes C3 . C2 . C7 . 118.89(16) yes C2 . C3 . C4 . 120.94(18) yes C2 . C3 . H31 . 118.7 no C4 . C3 . H31 . 120.4 no C3 . C4 . C5 . 119.9(2) yes C3 . C4 . H41 . 118.8 no C5 . C4 . H41 . 121.3 no C4 . C5 . C6 . 120.77(19) yes C4 . C5 . H51 . 118.5 no C6 . C5 . H51 . 120.7 no C5 . C6 . C7 . 120.62(19) yes C5 . C6 . H61 . 119.5 no C7 . C6 . H61 . 119.9 no C2 . C7 . C6 . 118.73(18) yes C2 . C7 . C8 . 119.70(17) yes C6 . C7 . C8 . 121.46(18) yes C7 . C8 . C9 . 120.98(17) yes C7 . C8 . H81 . 119.0 no C9 . C8 . H81 . 120.0 no C8 . C9 . C10 . 119.20(18) yes C8 . C9 . H91 . 119.8 no C10 . C9 . H91 . 121.0 no N1 . C10 . C9 . 120.81(17) yes N1 . C10 . C1 . 116.37(16) yes C9 . C10 . C1 . 122.06(17) yes N1 . C11 . C12 . 115.32(17) yes N1 . C11 . H111 . 122.2 no C12 . C11 . H111 . 122.4 no C11 . C12 . N2 . 110.18(16) yes C11 . C12 . C13 . 128.65(18) yes N2 . C12 . C13 . 120.99(18) yes C12 . C13 . C14 . 118.03(19) yes C12 . C13 . H131 . 119.8 no C14 . C13 . H131 . 122.1 no C13 . C14 . C15 . 120.98(18) yes C13 . C14 . H141 . 120.5 no C15 . C14 . H141 . 118.6 no C14 . C15 . C16 . 118.42(18) yes C14 . C15 . H151 . 120.3 no C16 . C15 . H151 . 121.2 no C15 . C16 . N2 . 120.25(17) yes C15 . C16 . C17 . 127.85(18) yes N2 . C16 . C17 . 111.89(16) yes C16 . C17 . N3 . 112.84(16) yes C16 . C17 . C18 . 124.68(17) yes N3 . C17 . C18 . 122.48(17) yes C17 . C18 . C19 . 118.53(19) yes C17 . C18 . H181 . 121.8 no C19 . C18 . H181 . 119.6 no C18 . C19 . C20 . 119.25(19) yes C18 . C19 . H191 . 119.5 no C20 . C19 . H191 . 121.2 no C19 . C20 . C21 . 119.57(19) yes C19 . C20 . H201 . 121.2 no C21 . C20 . H201 . 119.2 no C20 . C21 . N3 . 122.10(18) yes C20 . C21 . H211 . 119.9 no N3 . C21 . H211 . 118.0 no C31 4_665 C31 . C32 . 121.20(16) yes C31 4_665 C31 . C40 . 119.75(15) yes C32 . C31 . C40 . 118.79(18) yes C31 . C32 . C33 . 122.08(18) yes C31 . C32 . C37 . 119.06(19) yes C33 . C32 . C37 . 118.76(19) yes C32 . C33 . C34 . 120.8(2) yes C32 . C33 . H331 . 119.1 no C34 . C33 . H331 . 120.1 no C33 . C34 . C35 . 119.9(2) yes C33 . C34 . H341 . 120.0 no C35 . C34 . H341 . 120.1 no C34 . C35 . C36 . 121.0(2) yes C34 . C35 . H351 . 118.8 no C36 . C35 . H351 . 120.3 no C35 . C36 . C37 . 120.7(2) yes C35 . C36 . H361 . 120.4 no C37 . C36 . H361 . 118.9 no C32 . C37 . C36 . 118.8(2) yes C32 . C37 . C38 . 119.73(19) yes C36 . C37 . C38 . 121.4(2) yes C37 . C38 . C39 . 120.81(19) yes C37 . C38 . H381 . 120.3 no C39 . C38 . H381 . 118.9 no C38 . C39 . C40 . 119.38(19) yes C38 . C39 . H391 . 121.6 no C40 . C39 . H391 . 119.0 no N4 . C40 . C39 . 121.26(18) yes N4 . C40 . C31 . 116.18(17) yes C39 . C40 . C31 . 122.07(19) yes N4 . C41 . C52 . 114.89(18) yes N4 . C41 . H411 . 122.5 no C52 . C41 . H411 . 122.6 no C44 . C43 . C52 . 117.8(2) yes C44 . C43 . H431 . 121.8 no C52 . C43 . H431 . 120.4 no C43 . C44 . C45 . 120.64(19) yes C43 . C44 . H441 . 119.9 no C45 . C44 . H441 . 119.4 no C44 . C45 . C46 . 118.9(2) yes C44 . C45 . H451 . 120.7 no C46 . C45 . H451 . 120.4 no C45 . C46 . N5 . 120.22(19) yes C45 . C46 . C47 . 127.91(19) yes N5 . C46 . C47 . 111.87(17) yes C46 . C47 . N6 . 113.12(17) yes C46 . C47 . C48 . 124.78(19) yes N6 . C47 . C48 . 122.08(19) yes C47 . C48 . C49 . 119.2(2) yes C47 . C48 . H481 . 118.6 no C49 . C48 . H481 . 122.2 no C48 . C49 . C50 . 119.20(19) yes C48 . C49 . H491 . 119.9 no C50 . C49 . H491 . 120.9 no C49 . C50 . C51 . 119.10(19) yes C49 . C50 . H501 . 120.8 no C51 . C50 . H501 . 120.0 no C50 . C51 . N6 . 122.60(19) yes C50 . C51 . H511 . 119.5 no N6 . C51 . H511 . 117.9 no C41 . C52 . C43 . 128.36(19) yes C41 . C52 . N5 . 110.29(17) yes C43 . C52 . N5 . 121.17(19) yes F1 . P1 . F2 . 177.97(14) yes F1 . P1 . F3 . 89.21(11) yes F2 . P1 . F3 . 89.19(10) yes F1 . P1 . F4 . 91.19(12) yes F2 . P1 . F4 . 90.42(11) yes F3 . P1 . F4 . 179.60(11) yes F1 . P1 . F5 . 90.12(14) yes F2 . P1 . F5 . 88.64(12) yes F3 . P1 . F5 . 90.15(12) yes F4 . P1 . F5 . 89.85(13) yes F1 . P1 . F6 . 90.62(15) yes F2 . P1 . F6 . 90.58(12) yes F3 . P1 . F6 . 88.47(10) yes F4 . P1 . F6 . 91.53(13) yes F5 . P1 . F6 . 178.42(13) yes F11 . P2 . F12 . 177.85(17) yes F11 . P2 . F13 . 90.25(10) yes F12 . P2 . F13 . 88.70(10) yes F11 . P2 . F14 . 90.00(11) yes F12 . P2 . F14 . 91.04(12) yes F13 . P2 . F14 . 179.66(12) yes F11 . P2 . F15 . 91.14(19) yes F12 . P2 . F15 . 90.73(19) yes F13 . P2 . F15 . 89.28(13) yes F14 . P2 . F15 . 90.93(15) yes F11 . P2 . F16 . 88.89(15) yes F12 . P2 . F16 . 89.23(16) yes F13 . P2 . F16 . 89.77(13) yes F14 . P2 . F16 . 90.02(15) yes F15 . P2 . F16 . 179.05(16) yes