# Electronic Supplementary Material (ESI) for Chemical Communications # 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_complex[2]PF6 #TrackingRef '19649_web_deposit_cif_file_0_AdamT.Fiedler_1366395186.Fiedler ChemComm CIF 2013.cif' _audit_creation_date 2013-04-02 _audit_creation_method ; Olex2 1.2 (compiled Dec 5 2012 16:20:19, GUI svn.r4385) ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C98 H76 B2 Fe2 N12 O4, 1.04(F6 P), 0.96(C H2 Cl2)' _chemical_formula_sum 'C98.96 H77.93 B2 Cl1.93 F6.22 Fe2 N12 O4 P1.04' _chemical_formula_weight 1851.12 _chemical_melting_point ? _chemical_oxdiff_formula 'Fe C45 B H34 N6 P F6 O2 C4 H4' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_length_a 9.7382(3) _cell_length_b 13.2530(4) _cell_length_c 18.0619(7) _cell_angle_alpha 103.453(3) _cell_angle_beta 104.559(3) _cell_angle_gamma 97.098(3) _cell_volume 2152.89(13) _cell_formula_units_Z 1 _cell_measurement_reflns_used 20404 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 73.7422 _cell_measurement_theta_min 3.4921 _exptl_absorpt_coefficient_mu 4.063 _exptl_absorpt_correction_T_max 0.680 _exptl_absorpt_correction_T_min 0.362 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) Numerical absorption correction based on gaussian integration over a multifaceted crystal model ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 954 _exptl_crystal_size_max 0.368 _exptl_crystal_size_mid 0.1945 _exptl_crystal_size_min 0.1358 _exptl_special_details ; ? ; _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_unetI/netI 0.0240 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 42432 _diffrn_reflns_theta_full 72.00 _diffrn_reflns_theta_max 73.91 _diffrn_reflns_theta_min 3.49 _diffrn_ambient_temperature 100.00(10) _diffrn_detector_area_resol_mean 10.3756 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -49.00 33.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 57.0000 -30.0000 82 #__ type_ start__ end____ width___ exp.time_ 2 omega -48.00 36.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 -180.0000 84 #__ type_ start__ end____ width___ exp.time_ 3 omega -40.00 36.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 37.0000 -120.0000 76 #__ type_ start__ end____ width___ exp.time_ 4 omega -70.00 33.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 57.0000 90.0000 103 #__ type_ start__ end____ width___ exp.time_ 5 omega 46.00 94.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 -125.0000 -90.0000 48 #__ type_ start__ end____ width___ exp.time_ 6 omega 36.00 90.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 150.0000 54 #__ type_ start__ end____ width___ exp.time_ 7 omega 47.00 106.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -30.0000 59 #__ type_ start__ end____ width___ exp.time_ 8 omega 31.00 128.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -77.0000 90.0000 97 #__ type_ start__ end____ width___ exp.time_ 9 omega 33.00 88.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 90.0000 55 #__ type_ start__ end____ width___ exp.time_ 10 omega 44.00 103.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 60.0000 59 #__ type_ start__ end____ width___ exp.time_ 11 omega 60.00 120.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -125.0000 -90.0000 60 #__ type_ start__ end____ width___ exp.time_ 12 omega 44.00 71.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 -30.0000 27 #__ type_ start__ end____ width___ exp.time_ 13 omega 41.00 87.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -45.0000 -60.0000 46 #__ type_ start__ end____ width___ exp.time_ 14 omega 77.00 174.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 0.0000 97 #__ type_ start__ end____ width___ exp.time_ 15 omega 30.00 89.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -30.0000 -150.0000 59 #__ type_ start__ end____ width___ exp.time_ 16 omega 49.00 90.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 -90.0000 41 #__ type_ start__ end____ width___ exp.time_ 17 omega 28.00 113.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -15.0000 0.0000 85 #__ type_ start__ end____ width___ exp.time_ 18 omega -115.00 -11.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -60.0000 104 #__ type_ start__ end____ width___ exp.time_ 19 omega -115.00 -11.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 60.0000 104 #__ type_ start__ end____ width___ exp.time_ 20 omega -115.00 -11.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - -40.6487 -57.0000 -180.0000 104 #__ type_ start__ end____ width___ exp.time_ 21 omega 1.00 83.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 -99.0000 -150.0000 82 #__ type_ start__ end____ width___ exp.time_ 22 omega 7.00 119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 77.0000 60.0000 112 #__ type_ start__ end____ width___ exp.time_ 23 omega -140.00 -28.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - -61.5000 -77.0000 -60.0000 112 #__ type_ start__ end____ width___ exp.time_ 24 omega -140.00 -28.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - -61.5000 -77.0000 30.0000 112 #__ type_ start__ end____ width___ exp.time_ 25 omega -140.00 -28.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - -61.5000 -77.0000 -180.0000 112 #__ type_ start__ end____ width___ exp.time_ 26 omega 77.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 61.0000 -150.0000 101 #__ type_ start__ end____ width___ exp.time_ 27 omega 73.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 77.0000 -30.0000 105 #__ type_ start__ end____ width___ exp.time_ 28 omega 77.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 150.0000 101 #__ type_ start__ end____ width___ exp.time_ 29 omega 73.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 77.0000 150.0000 105 #__ type_ start__ end____ width___ exp.time_ 30 omega 77.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 61.0000 90.0000 101 #__ type_ start__ end____ width___ exp.time_ 31 omega 77.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 -60.0000 101 #__ type_ start__ end____ width___ exp.time_ 32 omega 77.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 30.0000 60.0000 101 #__ type_ start__ end____ width___ exp.time_ 33 omega 7.00 119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 77.0000 150.0000 112 #__ type_ start__ end____ width___ exp.time_ 34 omega 7.00 119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 77.0000 -120.0000 112 #__ type_ start__ end____ width___ exp.time_ 35 omega 23.00 98.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 -125.0000 90.0000 75 #__ type_ start__ end____ width___ exp.time_ 36 omega 1.00 83.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 -99.0000 -60.0000 82 #__ type_ start__ end____ width___ exp.time_ 37 omega 7.00 119.00 1.0000 1.5000 omega____ theta____ kappa____ phi______ frames - 40.6487 77.0000 -30.0000 112 #__ type_ start__ end____ width___ exp.time_ 38 omega 23.00 109.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 -94.0000 60.0000 86 #__ type_ start__ end____ width___ exp.time_ 39 omega 77.00 178.00 1.0000 3.9000 omega____ theta____ kappa____ phi______ frames - 107.0378 61.0000 -120.0000 101 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0678717000 _diffrn_orient_matrix_UB_12 -0.1169585000 _diffrn_orient_matrix_UB_13 -0.0151049000 _diffrn_orient_matrix_UB_21 -0.1487502000 _diffrn_orient_matrix_UB_22 0.0303189000 _diffrn_orient_matrix_UB_23 -0.0035100000 _diffrn_orient_matrix_UB_31 -0.0319311000 _diffrn_orient_matrix_UB_32 -0.0155553000 _diffrn_orient_matrix_UB_33 -0.0903235000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'SuperNova (Cu) X-ray Source' _reflns_number_gt 8283 _reflns_number_total 8566 _reflns_odcompleteness_completeness 99.99 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; XL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 0.556 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.055 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 624 _refine_ls_number_reflns 8566 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0393 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0566P)^2^+1.1484P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.1038 _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. ; _olex2_refinement_description ; 1. Others Fixed Uiso: H2(0.022) H5(0.026) H8(0.028) H11(0.024) H12(0.028) H13(0.029) H14(0.028) H15(0.023) H17(0.04) H18(0.063) H19(0.064) H20(0.058) H21(0.039) H23(0.031) H24(0.038) H25(0.035) H26(0.031) H27(0.026) H29(0.043) H30(0.065) H31(0.077) H32(0.076) H33(0.048) H35(0.027) H36(0.031) H37(0.032) H38(0.029) H39(0.024) H41(0.033) H42(0.042) H43(0.05) H44(0.056) H45(0.044) H48(0.021) H49A(0.037) H49B(0.037) H49C(0.037) H1(0.019) H50A(0.082) H50B(0.082) Fixed X: H2(-0.0806) H5(0.1542) H8(0.6858) H11(-0.1292) H12(-0.104) H13(0.1253) H14(0.33) H15(0.3061) H17(-0.2481) H18(-0.3104) H19(-0.1417) H20(0.0916) H21(0.1553) H23(0.4059) H24(0.5051) H25(0.4091) H26(0.2139) H27(0.1168) H29(0.1671) H30(0.0497) H31(-0.1577) H32(-0.2456) H33(-0.1251) H35(0.6371) H36(0.7012) H37(0.6697) H38(0.5757) H39(0.5104) H41(0.6898) H42(0.7185) H43(0.5571) H44(0.3612) H45(0.3313) H48(-0.1645) H49A(0.2338) H49B(0.3359) H49C(0.3562) H1(0.2764) H50A(0.4719) H50B(0.3685) Fixed Y: H2(0.9196) H5(0.3388) H8(0.7976) H11(0.8219) H12(0.8576) H13(0.9087) H14(0.9336) H15(0.9018) H17(0.8584) H18(0.8866) H19(0.8916) H20(0.8717) H21(0.8422) H23(0.4392) H24(0.4873) H25(0.606) H26(0.6767) H27(0.6312) H29(0.239) H30(0.1076) H31(0.1291) H32(0.2849) H33(0.421) H35(0.9654) H36(1.0599) H37(0.9728) H38(0.7915) H39(0.6969) H41(0.6224) H42(0.5734) H43(0.6061) H44(0.6809) H45(0.7319) H48(0.6176) H49A(0.3449) H49B(0.4206) H49C(0.4387) H1(0.7201) H50A(0.945) H50B(0.9041) Fixed Z: H2(0.3835) H5(0.3963) H8(0.3834) H11(0.5083) H12(0.6446) H13(0.7362) H14(0.6925) H15(0.5566) H17(0.221) H18(0.0936) H19(0.0232) H20(0.079) H21(0.204) H23(0.5279) H24(0.6657) H25(0.7468) H26(0.6896) H27(0.5516) H29(0.2504) H30(0.1332) H31(0.0472) H32(0.0757) H33(0.1923) H35(0.5028) H36(0.6369) H37(0.732) H38(0.6927) H39(0.5588) H41(0.2525) H42(0.1252) H43(0.019) H44(0.0377) H45(0.1646) H48(0.0098) H49A(0.1111) H49B(0.1944) H49C(0.1129) H1(0.485) H50A(0.9482) H50B(0.8585) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.14624(3) 0.621610(19) 0.243102(14) 0.01581(8) Uani 1 1 d . . . O1 O 0.00015(13) 0.61183(10) 0.14495(7) 0.0210(3) Uani 1 1 d . . . O2 O 0.18381(13) 0.48776(10) 0.13892(7) 0.0197(2) Uani 1 1 d . . . N1 N 0.09403(15) 0.75491(11) 0.31398(8) 0.0169(3) Uani 1 1 d . . . N2 N 0.13345(15) 0.76145(11) 0.39342(8) 0.0161(3) Uani 1 1 d . . . N3 N 0.12038(15) 0.52665(11) 0.31715(8) 0.0172(3) Uani 1 1 d . . . N4 N 0.17798(15) 0.57704(11) 0.39678(8) 0.0161(3) Uani 1 1 d . . . N5 N 0.35983(15) 0.68041(11) 0.31231(8) 0.0172(3) Uani 1 1 d . . . N6 N 0.37628(15) 0.71499(11) 0.39249(8) 0.0163(3) Uani 1 1 d . . . C1 C -0.00176(17) 0.55965(13) 0.07493(10) 0.0169(3) Uani 1 1 d . . . C2 C 0.09774(17) 0.48816(13) 0.06706(10) 0.0164(3) Uani 1 1 d . . . C3 C -0.09913(18) 0.57039(13) 0.00571(10) 0.0176(3) Uani 1 1 d . . . H48 H -0.1645 0.6176 0.0098 0.021 Uiso 1 1 calc R . . C4 C 0.2856(2) 0.41734(15) 0.13936(11) 0.0246(4) Uani 1 1 d . . . H49A H 0.2338 0.3449 0.1111 0.037 Uiso 1 1 calc R . . H49B H 0.3359 0.4206 0.1944 0.037 Uiso 1 1 calc R . . H49C H 0.3562 0.4387 0.1129 0.037 Uiso 1 1 calc R . . C5 C 0.06589(17) 0.83133(12) 0.43166(10) 0.0163(3) Uani 1 1 d . . . C6 C -0.01912(18) 0.87044(13) 0.37493(10) 0.0180(3) Uani 1 1 d . . . H2 H -0.0806 0.9196 0.3835 0.022 Uiso 1 1 calc R . . C7 C 0.00425(18) 0.82273(13) 0.30271(10) 0.0175(3) Uani 1 1 d . . . C8 C 0.19702(18) 0.50414(13) 0.43841(10) 0.0181(3) Uani 1 1 d . . . C9 C 0.15205(19) 0.40500(13) 0.38469(11) 0.0213(3) Uani 1 1 d . . . H5 H 0.1542 0.3388 0.3963 0.026 Uiso 1 1 calc R . . C10 C 0.10299(18) 0.42198(13) 0.31001(10) 0.0191(3) Uani 1 1 d . . . C11 C 0.51348(18) 0.76869(13) 0.43071(10) 0.0180(3) Uani 1 1 d . . . C12 C 0.58739(19) 0.76711(15) 0.37427(11) 0.0230(4) Uani 1 1 d . . . H8 H 0.6858 0.7976 0.3834 0.028 Uiso 1 1 calc R . . C13 C 0.48818(18) 0.71169(14) 0.30150(10) 0.0203(3) Uani 1 1 d . . . C14 C 0.08596(18) 0.85597(12) 0.51817(10) 0.0168(3) Uani 1 1 d . . . C15 C -0.03555(19) 0.84424(13) 0.54544(11) 0.0204(3) Uani 1 1 d . . . H11 H -0.1292 0.8219 0.5083 0.024 Uiso 1 1 calc R . . C16 C -0.0206(2) 0.86507(14) 0.62663(11) 0.0230(4) Uani 1 1 d . . . H12 H -0.1040 0.8576 0.6446 0.028 Uiso 1 1 calc R . . C17 C 0.1152(2) 0.89662(14) 0.68102(11) 0.0238(4) Uani 1 1 d . . . H13 H 0.1253 0.9087 0.7362 0.029 Uiso 1 1 calc R . . C18 C 0.2368(2) 0.91061(14) 0.65495(11) 0.0232(4) Uani 1 1 d . . . H14 H 0.3300 0.9336 0.6925 0.028 Uiso 1 1 calc R . . C19 C 0.22255(18) 0.89112(13) 0.57407(10) 0.0188(3) Uani 1 1 d . . . H15 H 0.3061 0.9018 0.5566 0.023 Uiso 1 1 calc R . . C20 C -0.0409(2) 0.84406(13) 0.22440(10) 0.0224(4) Uani 1 1 d . . . C21 C -0.1788(2) 0.85956(15) 0.19218(13) 0.0331(5) Uani 1 1 d . . . H17 H -0.2481 0.8584 0.2210 0.040 Uiso 1 1 calc R . . C22 C -0.2153(3) 0.87705(18) 0.11630(16) 0.0525(7) Uani 1 1 d . . . H18 H -0.3104 0.8866 0.0936 0.063 Uiso 1 1 calc R . . C23 C -0.1153(4) 0.88054(19) 0.07458(14) 0.0536(7) Uani 1 1 d . . . H19 H -0.1417 0.8916 0.0232 0.064 Uiso 1 1 calc R . . C24 C 0.0219(3) 0.86813(18) 0.10726(14) 0.0481(6) Uani 1 1 d . . . H20 H 0.0916 0.8717 0.0790 0.058 Uiso 1 1 calc R . . C25 C 0.0594(3) 0.85033(16) 0.18166(12) 0.0327(4) Uani 1 1 d . . . H21 H 0.1553 0.8422 0.2040 0.039 Uiso 1 1 calc R . . C26 C 0.25339(18) 0.53230(13) 0.52568(10) 0.0183(3) Uani 1 1 d . . . C27 C 0.3678(2) 0.48848(14) 0.56060(11) 0.0254(4) Uani 1 1 d . . . H23 H 0.4059 0.4392 0.5279 0.031 Uiso 1 1 calc R . . C28 C 0.4261(2) 0.51639(16) 0.64243(12) 0.0316(4) Uani 1 1 d . . . H24 H 0.5051 0.4873 0.6657 0.038 Uiso 1 1 calc R . . C29 C 0.3691(2) 0.58685(16) 0.69065(11) 0.0295(4) Uani 1 1 d . . . H25 H 0.4091 0.6060 0.7468 0.035 Uiso 1 1 calc R . . C30 C 0.2536(2) 0.62911(15) 0.65660(11) 0.0258(4) Uani 1 1 d . . . H26 H 0.2139 0.6767 0.6896 0.031 Uiso 1 1 calc R . . C31 C 0.19591(19) 0.60206(14) 0.57457(11) 0.0215(3) Uani 1 1 d . . . H27 H 0.1168 0.6312 0.5516 0.026 Uiso 1 1 calc R . . C32 C 0.0323(2) 0.34265(15) 0.23323(11) 0.0255(4) Uani 1 1 d . . . C33 C 0.0831(3) 0.24905(16) 0.21480(13) 0.0360(5) Uani 1 1 d . . . H29 H 0.1671 0.2390 0.2504 0.043 Uiso 1 1 calc R . . C34 C 0.0131(4) 0.17065(19) 0.14544(16) 0.0539(8) Uani 1 1 d . . . H30 H 0.0497 0.1076 0.1332 0.065 Uiso 1 1 calc R . . C35 C -0.1087(4) 0.1836(2) 0.09448(15) 0.0640(9) Uani 1 1 d . . . H31 H -0.1577 0.1291 0.0472 0.077 Uiso 1 1 calc R . . C36 C -0.1609(3) 0.2762(3) 0.11151(15) 0.0630(9) Uani 1 1 d . . . H32 H -0.2456 0.2849 0.0757 0.076 Uiso 1 1 calc R . . C37 C -0.0899(3) 0.35707(19) 0.18104(13) 0.0396(5) Uani 1 1 d . . . H33 H -0.1251 0.4210 0.1923 0.048 Uiso 1 1 calc R . . C38 C 0.56304(17) 0.82257(14) 0.51705(10) 0.0181(3) Uani 1 1 d . . . C39 C 0.62291(19) 0.93014(14) 0.54120(11) 0.0223(4) Uani 1 1 d . . . H35 H 0.6371 0.9654 0.5028 0.027 Uiso 1 1 calc R . . C40 C 0.6620(2) 0.98628(15) 0.62099(12) 0.0261(4) Uani 1 1 d . . . H36 H 0.7012 1.0599 0.6369 0.031 Uiso 1 1 calc R . . C41 C 0.6437(2) 0.93457(16) 0.67743(11) 0.0264(4) Uani 1 1 d . . . H37 H 0.6697 0.9728 0.7320 0.032 Uiso 1 1 calc R . . C42 C 0.58734(19) 0.82695(15) 0.65400(11) 0.0240(4) Uani 1 1 d . . . H38 H 0.5757 0.7915 0.6927 0.029 Uiso 1 1 calc R . . C43 C 0.54784(18) 0.77076(14) 0.57432(10) 0.0199(3) Uani 1 1 d . . . H39 H 0.5104 0.6969 0.5588 0.024 Uiso 1 1 calc R . . C44 C 0.50783(19) 0.68276(15) 0.22145(11) 0.0234(4) Uani 1 1 d . . . C45 C 0.6228(2) 0.63512(15) 0.20901(12) 0.0273(4) Uani 1 1 d . . . H41 H 0.6898 0.6224 0.2525 0.033 Uiso 1 1 calc R . . C46 C 0.6400(2) 0.60610(17) 0.13337(13) 0.0347(5) Uani 1 1 d . . . H42 H 0.7185 0.5734 0.1252 0.042 Uiso 1 1 calc R . . C47 C 0.5439(3) 0.6246(2) 0.07046(13) 0.0419(5) Uani 1 1 d . . . H43 H 0.5571 0.6061 0.0190 0.050 Uiso 1 1 calc R . . C48 C 0.4289(3) 0.6699(2) 0.08175(13) 0.0467(6) Uani 1 1 d . . . H44 H 0.3612 0.6809 0.0377 0.056 Uiso 1 1 calc R . . C49 C 0.4106(2) 0.6998(2) 0.15718(12) 0.0363(5) Uani 1 1 d . . . H45 H 0.3313 0.7319 0.1646 0.044 Uiso 1 1 calc R . . B1 B 0.2437(2) 0.69643(14) 0.42551(11) 0.0155(3) Uani 1 1 d . . . H1 H 0.2764 0.7201 0.4850 0.019 Uiso 1 1 calc R . . Cl1 Cl 0.5537(3) 1.0383(2) 0.86974(13) 0.0660(6) Uani 0.482(3) 1 d P A 2 Cl2 Cl 0.5617(3) 0.82068(19) 0.87318(15) 0.1020(11) Uani 0.482(3) 1 d P A 2 C50 C 0.4706(9) 0.9261(6) 0.8917(5) 0.068(2) Uani 0.482(3) 1 d P A 2 H50A H 0.4719 0.9450 0.9482 0.082 Uiso 0.482(3) 1 calc PR A 2 H50B H 0.3685 0.9041 0.8585 0.082 Uiso 0.482(3) 1 calc PR A 2 P1 P 0.54808(14) 0.90075(9) 0.88693(6) 0.0340(4) Uani 0.518(3) 1 d P A 1 F1 F 0.5465(3) 0.8024(2) 0.9248(2) 0.0491(8) Uani 0.518(3) 1 d P A 1 F2 F 0.6738(4) 0.8652(3) 0.8494(2) 0.0667(10) Uani 0.518(3) 1 d P A 1 F3 F 0.6703(3) 0.9750(2) 0.96413(16) 0.0500(8) Uani 0.518(3) 1 d P A 1 F4 F 0.4264(3) 0.9379(3) 0.92545(19) 0.0502(8) Uani 0.518(3) 1 d P A 1 F5 F 0.4278(4) 0.8271(3) 0.81105(17) 0.0636(10) Uani 0.518(3) 1 d P A 1 F6 F 0.5509(6) 0.9896(3) 0.8489(3) 0.0659(12) Uani 0.518(3) 1 d P A 1 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 0.01837(14) 0.01956(14) 0.00891(13) 0.00223(10) 0.00245(10) 0.00796(10) O1 0.0255(6) 0.0259(6) 0.0105(6) 0.0007(5) 0.0037(5) 0.0121(5) O2 0.0218(6) 0.0274(6) 0.0105(6) 0.0045(5) 0.0027(5) 0.0127(5) N1 0.0218(7) 0.0195(7) 0.0099(7) 0.0035(5) 0.0037(5) 0.0087(5) N2 0.0192(7) 0.0193(6) 0.0103(6) 0.0029(5) 0.0039(5) 0.0084(5) N3 0.0202(7) 0.0192(7) 0.0111(7) 0.0022(5) 0.0035(5) 0.0060(5) N4 0.0197(7) 0.0193(7) 0.0106(6) 0.0040(5) 0.0047(5) 0.0078(5) N5 0.0189(7) 0.0231(7) 0.0102(6) 0.0028(5) 0.0050(5) 0.0076(5) N6 0.0182(6) 0.0206(7) 0.0108(7) 0.0035(5) 0.0042(5) 0.0080(5) C1 0.0188(8) 0.0187(8) 0.0128(8) 0.0017(6) 0.0050(6) 0.0055(6) C2 0.0168(7) 0.0205(8) 0.0112(8) 0.0038(6) 0.0022(6) 0.0058(6) C3 0.0190(8) 0.0202(8) 0.0138(8) 0.0028(6) 0.0045(6) 0.0091(6) C4 0.0244(9) 0.0348(10) 0.0183(9) 0.0097(8) 0.0049(7) 0.0179(8) C5 0.0172(7) 0.0166(7) 0.0155(8) 0.0022(6) 0.0063(6) 0.0059(6) C6 0.0183(8) 0.0177(7) 0.0179(8) 0.0039(6) 0.0040(6) 0.0078(6) C7 0.0191(8) 0.0167(7) 0.0158(8) 0.0037(6) 0.0030(6) 0.0059(6) C8 0.0201(8) 0.0195(8) 0.0162(8) 0.0055(7) 0.0055(6) 0.0076(6) C9 0.0282(9) 0.0173(8) 0.0194(9) 0.0053(7) 0.0072(7) 0.0073(7) C10 0.0221(8) 0.0183(8) 0.0161(8) 0.0026(7) 0.0056(7) 0.0050(6) C11 0.0186(8) 0.0206(8) 0.0154(8) 0.0046(7) 0.0045(6) 0.0076(6) C12 0.0197(8) 0.0306(9) 0.0185(9) 0.0059(7) 0.0060(7) 0.0048(7) C13 0.0205(8) 0.0270(8) 0.0153(8) 0.0064(7) 0.0064(7) 0.0079(7) C14 0.0220(8) 0.0147(7) 0.0160(8) 0.0038(6) 0.0072(6) 0.0093(6) C15 0.0221(8) 0.0207(8) 0.0200(9) 0.0047(7) 0.0081(7) 0.0083(6) C16 0.0283(9) 0.0221(8) 0.0254(9) 0.0079(7) 0.0159(8) 0.0104(7) C17 0.0360(10) 0.0232(8) 0.0160(8) 0.0054(7) 0.0113(7) 0.0116(7) C18 0.0285(9) 0.0227(8) 0.0170(9) 0.0035(7) 0.0043(7) 0.0082(7) C19 0.0212(8) 0.0190(8) 0.0176(8) 0.0035(7) 0.0076(7) 0.0078(6) C20 0.0323(9) 0.0149(7) 0.0156(8) 0.0021(6) 0.0000(7) 0.0066(7) C21 0.0359(11) 0.0235(9) 0.0314(11) 0.0100(8) -0.0064(9) 0.0044(8) C22 0.0589(16) 0.0317(11) 0.0446(15) 0.0163(11) -0.0254(12) 0.0002(10) C23 0.094(2) 0.0335(12) 0.0215(11) 0.0127(9) -0.0019(13) -0.0003(13) C24 0.092(2) 0.0348(12) 0.0238(11) 0.0133(9) 0.0200(12) 0.0168(12) C25 0.0539(13) 0.0268(9) 0.0226(10) 0.0097(8) 0.0146(9) 0.0141(9) C26 0.0229(8) 0.0185(8) 0.0152(8) 0.0064(6) 0.0060(7) 0.0060(6) C27 0.0351(10) 0.0240(9) 0.0203(9) 0.0076(7) 0.0070(8) 0.0162(8) C28 0.0435(11) 0.0312(10) 0.0199(9) 0.0092(8) 0.0011(8) 0.0198(9) C29 0.0428(11) 0.0309(10) 0.0146(9) 0.0069(8) 0.0050(8) 0.0121(8) C30 0.0352(10) 0.0279(9) 0.0181(9) 0.0065(7) 0.0118(8) 0.0110(8) C31 0.0254(8) 0.0254(8) 0.0182(9) 0.0084(7) 0.0093(7) 0.0103(7) C32 0.0325(10) 0.0246(9) 0.0156(9) 0.0018(7) 0.0078(7) -0.0024(7) C33 0.0527(13) 0.0237(9) 0.0313(11) -0.0006(8) 0.0224(10) 0.0007(9) C34 0.085(2) 0.0305(11) 0.0390(14) -0.0108(10) 0.0364(15) -0.0147(12) C35 0.093(2) 0.0513(16) 0.0256(13) -0.0131(11) 0.0225(15) -0.0351(16) C36 0.0618(17) 0.079(2) 0.0244(12) 0.0144(13) -0.0106(12) -0.0265(15) C37 0.0412(12) 0.0447(12) 0.0240(11) 0.0100(9) 0.0000(9) -0.0056(10) C38 0.0150(7) 0.0243(8) 0.0152(8) 0.0042(7) 0.0040(6) 0.0075(6) C39 0.0209(8) 0.0256(9) 0.0209(9) 0.0064(7) 0.0060(7) 0.0065(7) C40 0.0242(9) 0.0245(9) 0.0253(10) 0.0002(8) 0.0070(8) 0.0026(7) C41 0.0232(9) 0.0349(10) 0.0161(9) -0.0017(8) 0.0051(7) 0.0051(7) C42 0.0210(8) 0.0356(10) 0.0160(9) 0.0075(8) 0.0054(7) 0.0071(7) C43 0.0186(8) 0.0239(8) 0.0176(8) 0.0057(7) 0.0045(7) 0.0071(6) C44 0.0232(8) 0.0305(9) 0.0160(9) 0.0042(7) 0.0075(7) 0.0036(7) C45 0.0265(9) 0.0332(10) 0.0235(10) 0.0054(8) 0.0117(8) 0.0061(8) C46 0.0358(11) 0.0382(11) 0.0315(11) 0.0005(9) 0.0217(9) 0.0043(9) C47 0.0445(12) 0.0575(14) 0.0206(10) 0.0001(10) 0.0181(9) 0.0001(11) C48 0.0458(13) 0.0755(18) 0.0205(11) 0.0163(11) 0.0088(10) 0.0135(12) C49 0.0342(11) 0.0587(14) 0.0231(10) 0.0148(10) 0.0124(9) 0.0194(10) B1 0.0187(8) 0.0183(8) 0.0116(8) 0.0043(7) 0.0057(7) 0.0085(7) Cl1 0.0771(11) 0.0744(14) 0.0596(11) 0.0192(11) 0.0413(9) 0.0167(12) Cl2 0.1157(19) 0.0848(16) 0.0838(16) -0.0140(12) 0.0042(14) 0.0626(14) C50 0.062(4) 0.086(5) 0.068(5) 0.006(4) 0.041(4) 0.038(4) P1 0.0385(7) 0.0432(7) 0.0188(5) 0.0057(4) 0.0041(4) 0.0162(5) F1 0.0641(18) 0.0547(17) 0.0428(18) 0.0303(14) 0.0167(15) 0.0292(14) F2 0.056(2) 0.098(3) 0.055(2) 0.0122(18) 0.0284(16) 0.0406(18) F3 0.0488(16) 0.0526(16) 0.0363(15) 0.0037(12) -0.0006(12) 0.0073(13) F4 0.0471(17) 0.0631(19) 0.0464(18) 0.0139(15) 0.0202(14) 0.0209(14) F5 0.065(2) 0.071(2) 0.0329(16) -0.0027(14) -0.0083(14) 0.0113(16) F6 0.088(3) 0.047(2) 0.082(3) 0.019(2) 0.049(2) 0.029(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1 1.9399(12) . ? Fe1 O2 2.4032(12) . ? Fe1 N1 2.1248(14) . ? Fe1 N3 2.0761(14) . ? Fe1 N5 2.0822(14) . ? O1 C1 1.287(2) . ? O2 C2 1.358(2) . ? O2 C4 1.443(2) . ? N1 C7 1.343(2) . ? N2 N1 1.3678(19) . ? N2 C5 1.360(2) . ? N2 B1 1.543(2) . ? N3 C10 1.348(2) . ? N4 N3 1.3726(19) . ? N4 C8 1.358(2) . ? N4 B1 1.544(2) . ? N5 C13 1.343(2) . ? N6 N5 1.3746(19) . ? N6 C11 1.357(2) . ? N6 B1 1.568(2) . ? C1 C2 1.446(2) . ? C1 C3 1.415(2) . ? C2 C3 1.366(2) 2_565 ? C3 C2 1.366(2) 2_565 ? C3 H48 0.9500 . ? C4 H49A 0.9800 . ? C4 H49B 0.9800 . ? C4 H49C 0.9800 . ? C5 C6 1.389(2) . ? C5 C14 1.476(2) . ? C6 H2 0.9500 . ? C6 C7 1.398(2) . ? C7 C20 1.476(2) . ? C8 C9 1.382(2) . ? C8 C26 1.472(2) . ? C9 H5 0.9500 . ? C9 C10 1.393(2) . ? C10 C32 1.472(2) . ? C11 C12 1.386(2) . ? C11 C38 1.481(2) . ? C12 H8 0.9500 . ? C12 C13 1.392(2) . ? C13 C44 1.474(2) . ? C14 C15 1.397(2) . ? C14 C19 1.399(2) . ? C15 H11 0.9500 . ? C15 C16 1.394(3) . ? C16 H12 0.9500 . ? C16 C17 1.381(3) . ? C17 H13 0.9500 . ? C17 C18 1.388(3) . ? C18 H14 0.9500 . ? C18 C19 1.391(2) . ? C19 H15 0.9500 . ? C20 C21 1.384(3) . ? C20 C25 1.395(3) . ? C21 H17 0.9500 . ? C21 C22 1.408(3) . ? C22 H18 0.9500 . ? C22 C23 1.376(4) . ? C23 H19 0.9500 . ? C23 C24 1.365(4) . ? C24 H20 0.9500 . ? C24 C25 1.385(3) . ? C25 H21 0.9500 . ? C26 C27 1.398(2) . ? C26 C31 1.394(2) . ? C27 H23 0.9500 . ? C27 C28 1.384(3) . ? C28 H24 0.9500 . ? C28 C29 1.390(3) . ? C29 H25 0.9500 . ? C29 C30 1.387(3) . ? C30 H26 0.9500 . ? C30 C31 1.387(3) . ? C31 H27 0.9500 . ? C32 C33 1.392(3) . ? C32 C37 1.385(3) . ? C33 H29 0.9500 . ? C33 C34 1.380(3) . ? C34 H30 0.9500 . ? C34 C35 1.363(5) . ? C35 H31 0.9500 . ? C35 C36 1.384(5) . ? C36 H32 0.9500 . ? C36 C37 1.399(3) . ? C37 H33 0.9500 . ? C38 C39 1.393(2) . ? C38 C43 1.395(2) . ? C39 H35 0.9500 . ? C39 C40 1.389(3) . ? C40 H36 0.9500 . ? C40 C41 1.388(3) . ? C41 H37 0.9500 . ? C41 C42 1.387(3) . ? C42 H38 0.9500 . ? C42 C43 1.388(3) . ? C43 H39 0.9500 . ? C44 C45 1.392(3) . ? C44 C49 1.385(3) . ? C45 H41 0.9500 . ? C45 C46 1.389(3) . ? C46 H42 0.9500 . ? C46 C47 1.371(3) . ? C47 H43 0.9500 . ? C47 C48 1.371(4) . ? C48 H44 0.9500 . ? C48 C49 1.391(3) . ? C49 H45 0.9500 . ? B1 H1 1.0000 . ? Cl1 C50 1.778(9) . ? Cl2 C50 1.757(8) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? P1 F1 1.607(3) . ? P1 F2 1.609(3) . ? P1 F3 1.602(3) . ? P1 F4 1.590(3) . ? P1 F5 1.579(3) . ? P1 F6 1.496(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Fe1 O2 71.99(4) . . ? O1 Fe1 N1 96.61(5) . . ? O1 Fe1 N3 122.90(6) . . ? O1 Fe1 N5 146.62(6) . . ? N1 Fe1 O2 167.06(5) . . ? N3 Fe1 O2 97.09(5) . . ? N3 Fe1 N1 94.29(5) . . ? N3 Fe1 N5 89.75(6) . . ? N5 Fe1 O2 99.51(5) . . ? N5 Fe1 N1 86.64(5) . . ? C1 O1 Fe1 125.57(11) . . ? C2 O2 Fe1 110.29(9) . . ? C2 O2 C4 117.35(13) . . ? C4 O2 Fe1 132.12(10) . . ? N2 N1 Fe1 113.55(10) . . ? C7 N1 Fe1 137.10(11) . . ? C7 N1 N2 107.22(13) . . ? N1 N2 B1 119.25(13) . . ? C5 N2 N1 109.79(13) . . ? C5 N2 B1 130.93(14) . . ? N4 N3 Fe1 114.14(10) . . ? C10 N3 Fe1 135.29(12) . . ? C10 N3 N4 106.75(13) . . ? N3 N4 B1 120.80(13) . . ? C8 N4 N3 109.59(13) . . ? C8 N4 B1 127.78(14) . . ? N6 N5 Fe1 114.00(10) . . ? C13 N5 Fe1 137.92(12) . . ? C13 N5 N6 106.93(13) . . ? N5 N6 B1 120.29(13) . . ? C11 N6 N5 109.50(13) . . ? C11 N6 B1 130.07(14) . . ? O1 C1 C2 119.05(15) . . ? O1 C1 C3 121.55(15) . . ? C3 C1 C2 119.40(15) . . ? O2 C2 C1 111.87(14) . . ? O2 C2 C3 126.54(15) . 2_565 ? C3 C2 C1 121.59(15) 2_565 . ? C1 C3 H48 120.5 . . ? C2 C3 C1 119.01(15) 2_565 . ? C2 C3 H48 120.5 2_565 . ? O2 C4 H49A 109.5 . . ? O2 C4 H49B 109.5 . . ? O2 C4 H49C 109.5 . . ? H49A C4 H49B 109.5 . . ? H49A C4 H49C 109.5 . . ? H49B C4 H49C 109.5 . . ? N2 C5 C6 107.43(14) . . ? N2 C5 C14 122.97(14) . . ? C6 C5 C14 129.61(15) . . ? C5 C6 H2 127.0 . . ? C5 C6 C7 105.98(14) . . ? C7 C6 H2 127.0 . . ? N1 C7 C6 109.53(14) . . ? N1 C7 C20 119.69(15) . . ? C6 C7 C20 130.44(15) . . ? N4 C8 C9 107.87(15) . . ? N4 C8 C26 123.21(15) . . ? C9 C8 C26 128.91(15) . . ? C8 C9 H5 127.0 . . ? C8 C9 C10 105.99(15) . . ? C10 C9 H5 127.0 . . ? N3 C10 C9 109.79(15) . . ? N3 C10 C32 122.07(16) . . ? C9 C10 C32 128.01(16) . . ? N6 C11 C12 107.74(15) . . ? N6 C11 C38 122.81(15) . . ? C12 C11 C38 129.35(16) . . ? C11 C12 H8 127.0 . . ? C11 C12 C13 106.02(15) . . ? C13 C12 H8 127.0 . . ? N5 C13 C12 109.80(15) . . ? N5 C13 C44 120.25(16) . . ? C12 C13 C44 129.91(16) . . ? C15 C14 C5 118.98(15) . . ? C15 C14 C19 118.64(16) . . ? C19 C14 C5 122.39(15) . . ? C14 C15 H11 119.7 . . ? C16 C15 C14 120.58(17) . . ? C16 C15 H11 119.7 . . ? C15 C16 H12 119.9 . . ? C17 C16 C15 120.14(17) . . ? C17 C16 H12 119.9 . . ? C16 C17 H13 120.0 . . ? C16 C17 C18 119.96(17) . . ? C18 C17 H13 120.0 . . ? C17 C18 H14 119.9 . . ? C17 C18 C19 120.18(17) . . ? C19 C18 H14 119.9 . . ? C14 C19 H15 119.8 . . ? C18 C19 C14 120.47(16) . . ? C18 C19 H15 119.8 . . ? C21 C20 C7 122.39(18) . . ? C21 C20 C25 118.68(18) . . ? C25 C20 C7 118.93(17) . . ? C20 C21 H17 120.4 . . ? C20 C21 C22 119.3(2) . . ? C22 C21 H17 120.4 . . ? C21 C22 H18 119.5 . . ? C23 C22 C21 120.9(2) . . ? C23 C22 H18 119.5 . . ? C22 C23 H19 120.1 . . ? C24 C23 C22 119.8(2) . . ? C24 C23 H19 120.1 . . ? C23 C24 H20 120.0 . . ? C23 C24 C25 120.0(3) . . ? C25 C24 H20 120.0 . . ? C20 C25 H21 119.4 . . ? C24 C25 C20 121.3(2) . . ? C24 C25 H21 119.4 . . ? C27 C26 C8 119.30(15) . . ? C31 C26 C8 121.66(15) . . ? C31 C26 C27 119.04(16) . . ? C26 C27 H23 119.8 . . ? C28 C27 C26 120.46(17) . . ? C28 C27 H23 119.8 . . ? C27 C28 H24 120.0 . . ? C27 C28 C29 120.08(18) . . ? C29 C28 H24 120.0 . . ? C28 C29 H25 120.1 . . ? C30 C29 C28 119.86(18) . . ? C30 C29 H25 120.1 . . ? C29 C30 H26 119.9 . . ? C31 C30 C29 120.18(17) . . ? C31 C30 H26 119.9 . . ? C26 C31 H27 119.8 . . ? C30 C31 C26 120.35(17) . . ? C30 C31 H27 119.8 . . ? C33 C32 C10 119.77(18) . . ? C37 C32 C10 120.71(19) . . ? C37 C32 C33 119.4(2) . . ? C32 C33 H29 119.6 . . ? C34 C33 C32 120.8(3) . . ? C34 C33 H29 119.6 . . ? C33 C34 H30 120.0 . . ? C35 C34 C33 120.1(3) . . ? C35 C34 H30 120.0 . . ? C34 C35 H31 120.0 . . ? C34 C35 C36 120.1(2) . . ? C36 C35 H31 120.0 . . ? C35 C36 H32 119.7 . . ? C35 C36 C37 120.6(3) . . ? C37 C36 H32 119.7 . . ? C32 C37 C36 119.1(3) . . ? C32 C37 H33 120.5 . . ? C36 C37 H33 120.5 . . ? C39 C38 C11 118.11(16) . . ? C39 C38 C43 119.18(16) . . ? C43 C38 C11 122.67(16) . . ? C38 C39 H35 119.7 . . ? C40 C39 C38 120.56(17) . . ? C40 C39 H35 119.7 . . ? C39 C40 H36 120.1 . . ? C41 C40 C39 119.86(17) . . ? C41 C40 H36 120.1 . . ? C40 C41 H37 120.1 . . ? C42 C41 C40 119.85(17) . . ? C42 C41 H37 120.1 . . ? C41 C42 H38 119.8 . . ? C41 C42 C43 120.40(17) . . ? C43 C42 H38 119.8 . . ? C38 C43 H39 120.0 . . ? C42 C43 C38 120.10(17) . . ? C42 C43 H39 120.0 . . ? C45 C44 C13 120.27(17) . . ? C49 C44 C13 120.78(17) . . ? C49 C44 C45 118.92(18) . . ? C44 C45 H41 119.8 . . ? C46 C45 C44 120.38(19) . . ? C46 C45 H41 119.8 . . ? C45 C46 H42 120.0 . . ? C47 C46 C45 120.1(2) . . ? C47 C46 H42 120.0 . . ? C46 C47 H43 120.0 . . ? C48 C47 C46 120.1(2) . . ? C48 C47 H43 120.0 . . ? C47 C48 H44 119.8 . . ? C47 C48 C49 120.5(2) . . ? C49 C48 H44 119.8 . . ? C44 C49 C48 120.1(2) . . ? C44 C49 H45 120.0 . . ? C48 C49 H45 120.0 . . ? N2 B1 N4 111.15(13) . . ? N2 B1 N6 108.15(13) . . ? N2 B1 H1 109.8 . . ? N4 B1 N6 108.09(13) . . ? N4 B1 H1 109.8 . . ? N6 B1 H1 109.8 . . ? Cl1 C50 H50A 109.5 . . ? Cl1 C50 H50B 109.5 . . ? Cl2 C50 Cl1 110.8(4) . . ? Cl2 C50 H50A 109.5 . . ? Cl2 C50 H50B 109.5 . . ? H50A C50 H50B 108.1 . . ? F1 P1 F2 90.35(19) . . ? F3 P1 F1 91.94(17) . . ? F3 P1 F2 88.87(18) . . ? F4 P1 F1 89.94(18) . . ? F4 P1 F2 178.8(2) . . ? F4 P1 F3 89.91(17) . . ? F5 P1 F1 87.75(19) . . ? F5 P1 F2 91.1(2) . . ? F5 P1 F3 179.69(19) . . ? F5 P1 F4 90.13(18) . . ? F6 P1 F1 177.7(2) . . ? F6 P1 F2 87.7(2) . . ? F6 P1 F3 89.3(2) . . ? F6 P1 F4 92.0(2) . . ? F6 P1 F5 91.0(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 Fe1 O1 C1 C2 10.5(2) . . . . ? Fe1 O1 C1 C3 -169.76(12) . . . . ? Fe1 O2 C2 C1 -6.55(16) . . . . ? Fe1 O2 C2 C3 173.84(14) . . . 2_565 ? Fe1 N1 C7 C6 159.08(13) . . . . ? Fe1 N1 C7 C20 -26.9(3) . . . . ? Fe1 N3 C10 C9 154.45(13) . . . . ? Fe1 N3 C10 C32 -29.4(3) . . . . ? Fe1 N5 C13 C12 165.81(13) . . . . ? Fe1 N5 C13 C44 -16.2(3) . . . . ? O1 Fe1 O2 C2 8.68(10) . . . . ? O1 Fe1 O2 C4 -177.21(16) . . . . ? O1 Fe1 N1 N2 155.26(11) . . . . ? O1 Fe1 N1 C7 -5.36(18) . . . . ? O1 Fe1 N3 N4 -143.18(10) . . . . ? O1 Fe1 N3 C10 62.43(18) . . . . ? O1 Fe1 N5 N6 141.17(10) . . . . ? O1 Fe1 N5 C13 -24.5(2) . . . . ? O1 C1 C2 O2 -0.6(2) . . . . ? O1 C1 C2 C3 179.04(16) . . . 2_565 ? O1 C1 C3 C2 -179.06(16) . . . 2_565 ? O2 Fe1 O1 C1 -10.30(13) . . . . ? O2 Fe1 N1 N2 -177.04(18) . . . . ? O2 Fe1 N1 C7 22.3(3) . . . . ? O2 Fe1 N3 N4 143.71(10) . . . . ? O2 Fe1 N3 C10 -10.67(17) . . . . ? O2 Fe1 N5 N6 -147.22(10) . . . . ? O2 Fe1 N5 C13 47.16(18) . . . . ? N1 Fe1 O1 C1 163.42(14) . . . . ? N1 Fe1 O2 C2 -20.4(3) . . . . ? N1 Fe1 O2 C4 153.7(2) . . . . ? N1 Fe1 N3 N4 -42.46(11) . . . . ? N1 Fe1 N3 C10 163.15(16) . . . . ? N1 Fe1 N5 N6 44.24(11) . . . . ? N1 Fe1 N5 C13 -121.38(18) . . . . ? N1 N2 C5 C6 0.03(18) . . . . ? N1 N2 C5 C14 179.96(14) . . . . ? N1 N2 B1 N4 -69.62(18) . . . . ? N1 N2 B1 N6 48.89(19) . . . . ? N1 C7 C20 C21 143.10(18) . . . . ? N1 C7 C20 C25 -37.8(2) . . . . ? N2 N1 C7 C6 -2.35(18) . . . . ? N2 N1 C7 C20 171.67(15) . . . . ? N2 C5 C6 C7 -1.42(18) . . . . ? N2 C5 C14 C15 -125.16(17) . . . . ? N2 C5 C14 C19 55.1(2) . . . . ? N3 Fe1 O1 C1 -97.10(14) . . . . ? N3 Fe1 O2 C2 131.04(11) . . . . ? N3 Fe1 O2 C4 -54.86(15) . . . . ? N3 Fe1 N1 N2 31.41(11) . . . . ? N3 Fe1 N1 C7 -129.21(17) . . . . ? N3 Fe1 N5 N6 -50.07(11) . . . . ? N3 Fe1 N5 C13 144.31(18) . . . . ? N3 N4 C8 C9 0.49(19) . . . . ? N3 N4 C8 C26 -178.32(15) . . . . ? N3 N4 B1 N2 55.90(19) . . . . ? N3 N4 B1 N6 -62.64(18) . . . . ? N3 C10 C32 C33 142.93(18) . . . . ? N3 C10 C32 C37 -41.1(3) . . . . ? N4 N3 C10 C9 -1.23(19) . . . . ? N4 N3 C10 C32 174.91(15) . . . . ? N4 C8 C9 C10 -1.20(19) . . . . ? N4 C8 C26 C27 -129.57(18) . . . . ? N4 C8 C26 C31 50.2(2) . . . . ? N5 Fe1 O1 C1 69.48(17) . . . . ? N5 Fe1 O2 C2 -138.02(11) . . . . ? N5 Fe1 O2 C4 36.08(15) . . . . ? N5 Fe1 N1 N2 -58.09(11) . . . . ? N5 Fe1 N1 C7 141.29(17) . . . . ? N5 Fe1 N3 N4 44.16(11) . . . . ? N5 Fe1 N3 C10 -110.23(16) . . . . ? N5 N6 C11 C12 -1.01(18) . . . . ? N5 N6 C11 C38 175.62(14) . . . . ? N5 N6 B1 N2 -65.55(18) . . . . ? N5 N6 B1 N4 54.89(18) . . . . ? N5 C13 C44 C45 -128.33(19) . . . . ? N5 C13 C44 C49 49.9(3) . . . . ? N6 N5 C13 C12 -0.47(19) . . . . ? N6 N5 C13 C44 177.51(15) . . . . ? N6 C11 C12 C13 0.70(19) . . . . ? N6 C11 C38 C39 -123.67(18) . . . . ? N6 C11 C38 C43 54.2(2) . . . . ? C2 C1 C3 C2 0.7(3) . . . 2_565 ? C3 C1 C2 O2 179.64(15) . . . . ? C3 C1 C2 C3 -0.7(3) . . . 2_565 ? C4 O2 C2 C1 178.37(14) . . . . ? C4 O2 C2 C3 -1.2(2) . . . 2_565 ? C5 N2 N1 Fe1 -164.88(11) . . . . ? C5 N2 N1 C7 1.44(18) . . . . ? C5 N2 B1 N4 112.67(18) . . . . ? C5 N2 B1 N6 -128.82(17) . . . . ? C5 C6 C7 N1 2.35(19) . . . . ? C5 C6 C7 C20 -170.81(17) . . . . ? C5 C14 C15 C16 178.94(15) . . . . ? C5 C14 C19 C18 -178.21(15) . . . . ? C6 C5 C14 C15 54.7(2) . . . . ? C6 C5 C14 C19 -125.00(19) . . . . ? C6 C7 C20 C21 -44.3(3) . . . . ? C6 C7 C20 C25 134.8(2) . . . . ? C7 C20 C21 C22 -178.49(18) . . . . ? C7 C20 C25 C24 178.73(18) . . . . ? C8 N4 N3 Fe1 -161.03(11) . . . . ? C8 N4 N3 C10 0.46(18) . . . . ? C8 N4 B1 N2 -141.15(16) . . . . ? C8 N4 B1 N6 100.30(18) . . . . ? C8 C9 C10 N3 1.5(2) . . . . ? C8 C9 C10 C32 -174.32(17) . . . . ? C8 C26 C27 C28 177.81(18) . . . . ? C8 C26 C31 C30 -178.43(17) . . . . ? C9 C8 C26 C27 51.9(3) . . . . ? C9 C8 C26 C31 -128.4(2) . . . . ? C9 C10 C32 C33 -41.7(3) . . . . ? C9 C10 C32 C37 134.3(2) . . . . ? C10 C32 C33 C34 175.86(19) . . . . ? C10 C32 C37 C36 -175.0(2) . . . . ? C11 N6 N5 Fe1 -169.06(10) . . . . ? C11 N6 N5 C13 0.92(18) . . . . ? C11 N6 B1 N2 109.62(18) . . . . ? C11 N6 B1 N4 -129.94(17) . . . . ? C11 C12 C13 N5 -0.1(2) . . . . ? C11 C12 C13 C44 -177.86(18) . . . . ? C11 C38 C39 C40 175.53(16) . . . . ? C11 C38 C43 C42 -175.62(16) . . . . ? C12 C11 C38 C39 52.2(2) . . . . ? C12 C11 C38 C43 -129.9(2) . . . . ? C12 C13 C44 C45 49.2(3) . . . . ? C12 C13 C44 C49 -132.6(2) . . . . ? C13 C44 C45 C46 178.86(18) . . . . ? C13 C44 C49 C48 -178.6(2) . . . . ? C14 C5 C6 C7 178.66(16) . . . . ? C14 C15 C16 C17 -0.7(3) . . . . ? C15 C14 C19 C18 2.0(2) . . . . ? C15 C16 C17 C18 1.9(3) . . . . ? C16 C17 C18 C19 -1.2(3) . . . . ? C17 C18 C19 C14 -0.8(3) . . . . ? C19 C14 C15 C16 -1.3(2) . . . . ? C20 C21 C22 C23 -1.0(3) . . . . ? C21 C20 C25 C24 -2.1(3) . . . . ? C21 C22 C23 C24 -0.8(4) . . . . ? C22 C23 C24 C25 1.1(4) . . . . ? C23 C24 C25 C20 0.4(3) . . . . ? C25 C20 C21 C22 2.4(3) . . . . ? C26 C8 C9 C10 177.51(17) . . . . ? C26 C27 C28 C29 1.3(3) . . . . ? C27 C26 C31 C30 1.3(3) . . . . ? C27 C28 C29 C30 0.1(3) . . . . ? C28 C29 C30 C31 -0.7(3) . . . . ? C29 C30 C31 C26 0.0(3) . . . . ? C31 C26 C27 C28 -1.9(3) . . . . ? C32 C33 C34 C35 -0.9(3) . . . . ? C33 C32 C37 C36 1.1(3) . . . . ? C33 C34 C35 C36 1.1(4) . . . . ? C34 C35 C36 C37 -0.2(4) . . . . ? C35 C36 C37 C32 -0.9(4) . . . . ? C37 C32 C33 C34 -0.2(3) . . . . ? C38 C11 C12 C13 -175.64(17) . . . . ? C38 C39 C40 C41 1.1(3) . . . . ? C39 C38 C43 C42 2.3(2) . . . . ? C39 C40 C41 C42 0.4(3) . . . . ? C40 C41 C42 C43 -0.6(3) . . . . ? C41 C42 C43 C38 -0.8(3) . . . . ? C43 C38 C39 C40 -2.5(3) . . . . ? C44 C45 C46 C47 0.2(3) . . . . ? C45 C44 C49 C48 -0.3(3) . . . . ? C45 C46 C47 C48 -1.3(4) . . . . ? C46 C47 C48 C49 1.6(4) . . . . ? C47 C48 C49 C44 -0.8(4) . . . . ? C49 C44 C45 C46 0.6(3) . . . . ? B1 N2 N1 Fe1 16.96(17) . . . . ? B1 N2 N1 C7 -176.72(14) . . . . ? B1 N2 C5 C6 177.90(16) . . . . ? B1 N2 C5 C14 -2.2(3) . . . . ? B1 N4 N3 Fe1 4.73(17) . . . . ? B1 N4 N3 C10 166.21(14) . . . . ? B1 N4 C8 C9 -164.00(15) . . . . ? B1 N4 C8 C26 17.2(3) . . . . ? B1 N6 N5 Fe1 7.02(17) . . . . ? B1 N6 N5 C13 177.00(14) . . . . ? B1 N6 C11 C12 -176.59(15) . . . . ? B1 N6 C11 C38 0.0(3) . . . . ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 6 -1 -1 0.1507 6.0000 -1.0000 -1.0001 -0.2752 -0.9193 -0.0857 -6 -1 7 0.1358 -6.0000 -1.0000 7.0000 0.4185 0.8376 -0.4251 0 -2 -10 0.0902 -0.0000 -2.0000 -9.9999 0.3850 -0.0255 0.9343 0 8 0 0.0679 0.0000 8.0000 0.0000 -0.9357 0.2426 -0.1244 0 -8 0 0.0679 -0.0000 -8.0000 -0.0000 0.9357 -0.2426 0.1244 0 0 11 0.0653 0.0000 0.0000 10.9999 -0.1662 -0.0386 -0.9935 0 2 -11 0.1097 -0.0000 2.0000 -10.9999 -0.0678 0.0993 0.9624 1 -8 -1 0.0588 1.0000 -8.0000 -1.0000 0.8829 -0.3878 0.1828 5 4 0 0.1302 5.0000 4.0001 -0.0001 -0.8072 -0.6225 -0.2219 1 0 -11 0.1080 1.0000 -0.0000 -10.9999 0.0983 -0.1101 0.9616 _database_code_depnum_ccdc_archive 'CCDC 934969'