# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound1 #TrackingRef '17445_web_deposit_cif_file_0_RobertLanger_1359917457.Compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _symmetry_space_group_name_Hall P2ac2ab _chemical_formula_moiety 'C48 H45 B Fe N2 P4, C H2 Cl2' _chemical_formula_sum 'C49 H47 B Cl2 Fe N2 P4' _chemical_formula_weight 925.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.979(2) _cell_length_b 18.349(4) _cell_length_c 20.219(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4444.2(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 161 _cell_measurement_theta_min 3.37 _cell_measurement_theta_max 17.99 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.641 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9445 _exptl_absorpt_correction_T_max 0.9505 _exptl_absorpt_process_details 'STOE X-RED' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -3 4 -5 0.0460 3 -4 5 0.0440 -4 -3 5 0.0560 4 3 -5 0.0390 -1 -4 0 0.0400 1 4 0 0.0430 -1 0 5 0.0770 0 -3 -4 0.0480 0 3 4 0.0600 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18596 _diffrn_reflns_av_R_equivalents 0.0875 _diffrn_reflns_av_sigmaI/netI 0.2214 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 26.67 _reflns_number_total 9319 _reflns_number_gt 4929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 9319 _refine_ls_number_parameters 512 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.47772(8) 0.63759(5) 0.20135(4) 0.0138(2) Uani 1 1 d . . . H1FE H 0.3598 0.6334 0.2290 0.017 Uiso 1 1 d . . . P1 P 0.53315(17) 0.79921(8) 0.13315(7) 0.0149(4) Uani 1 1 d . . . N1 N 0.5084(4) 0.8176(2) 0.2105(2) 0.0151(12) Uani 1 1 d . . . B1 B 0.5203(7) 0.6941(4) 0.1163(3) 0.0184(16) Uani 1 1 d . . . H3B1 H 0.5830 0.6657 0.1544 0.022 Uiso 1 1 d . . . H2B1 H 0.522(7) 0.677(3) 0.057(3) 0.05(2) Uiso 1 1 d . . . H1B1 H 0.4387 0.6840 0.1435 0.057 Uiso 1 1 d . . . C1 C 0.6701(6) 0.8324(3) 0.1098(3) 0.0158(15) Uani 1 1 d . . . Cl1 Cl 0.9446(3) 0.73227(16) 0.23874(14) 0.0980(8) Uani 1 1 d . . . P2 P 0.47744(16) 0.74470(8) 0.25611(7) 0.0157(4) Uani 1 1 d . . . N2 N 0.4880(4) 0.4855(2) 0.2372(2) 0.0127(12) Uani 1 1 d . . . H1N2 H 0.491(5) 0.429(3) 0.251(2) 0.015 Uiso 1 1 d . . . C2 C 0.7107(6) 0.8282(4) 0.0446(3) 0.0164(16) Uani 1 1 d . . . H2A H 0.6633 0.8110 0.0103 0.020 Uiso 1 1 calc R . . P3 P 0.53595(17) 0.56097(9) 0.27553(7) 0.0150(4) Uani 1 1 d . . . C3 C 0.8174(6) 0.8484(4) 0.0304(4) 0.0283(19) Uani 1 1 d . . . H3A H 0.8435 0.8454 -0.0139 0.034 Uiso 1 1 calc R . . P4 P 0.44176(15) 0.52682(9) 0.16679(7) 0.0141(4) Uani 1 1 d . . . C4 C 0.8892(6) 0.8738(4) 0.0800(3) 0.0316(14) Uani 1 1 d . . . H4A H 0.9635 0.8878 0.0697 0.038 Uiso 1 1 calc R . . C5 C 0.8508(6) 0.8779(4) 0.1426(3) 0.0316(14) Uani 1 1 d . . . H5A H 0.8987 0.8959 0.1764 0.038 Uiso 1 1 calc R . . C6 C 0.7427(6) 0.8563(4) 0.1591(3) 0.0240(16) Uani 1 1 d . . . H6A H 0.7185 0.8579 0.2038 0.029 Uiso 1 1 calc R . . C7 C 0.4345(6) 0.8446(3) 0.0787(3) 0.0191(16) Uani 1 1 d . . . C8 C 0.3247(6) 0.8177(4) 0.0780(3) 0.0219(17) Uani 1 1 d . . . H8A H 0.3055 0.7783 0.1063 0.026 Uiso 1 1 calc R . . C9 C 0.2442(7) 0.8472(4) 0.0372(4) 0.0271(19) Uani 1 1 d . . . H9A H 0.1707 0.8278 0.0378 0.032 Uiso 1 1 calc R . . C10 C 0.2688(7) 0.9039(4) -0.0037(4) 0.0321(19) Uani 1 1 d . . . H10A H 0.2124 0.9243 -0.0312 0.038 Uiso 1 1 calc R . . C11 C 0.3776(6) 0.9323(3) -0.0053(3) 0.0209(16) Uani 1 1 d . . . H11A H 0.3963 0.9708 -0.0346 0.025 Uiso 1 1 calc R . . C12 C 0.4578(6) 0.9029(3) 0.0368(3) 0.0192(15) Uani 1 1 d . . . H12A H 0.5307 0.9233 0.0370 0.023 Uiso 1 1 calc R . . C13 C 0.5706(6) 0.7514(3) 0.3271(3) 0.0213(11) Uani 1 1 d . . . C14 C 0.6806(6) 0.7297(3) 0.3195(3) 0.0206(17) Uani 1 1 d . . . H14A H 0.7052 0.7131 0.2775 0.025 Uiso 1 1 calc R . . C15 C 0.7557(6) 0.7315(4) 0.3716(3) 0.0250(18) Uani 1 1 d . . . H15A H 0.8301 0.7152 0.3648 0.030 Uiso 1 1 calc R . . C16 C 0.7244(7) 0.7563(3) 0.4327(3) 0.0280(18) Uani 1 1 d . . . H16A H 0.7767 0.7567 0.4680 0.034 Uiso 1 1 calc R . . C17 C 0.6169(7) 0.7808(4) 0.4429(3) 0.032(2) Uani 1 1 d . . . H17A H 0.5949 0.7989 0.4849 0.038 Uiso 1 1 calc R . . C18 C 0.5394(7) 0.7787(3) 0.3896(3) 0.0213(11) Uani 1 1 d . . . H18A H 0.4655 0.7959 0.3962 0.026 Uiso 1 1 calc R . . C19 C 0.3400(5) 0.7675(3) 0.2932(3) 0.0149(14) Uani 1 1 d . . . C20 C 0.2820(6) 0.8287(3) 0.2727(3) 0.0199(16) Uani 1 1 d . . . H20A H 0.3131 0.8603 0.2403 0.024 Uiso 1 1 calc R . . C21 C 0.1783(6) 0.8437(4) 0.2997(4) 0.0335(18) Uani 1 1 d . . . H21A H 0.1383 0.8856 0.2857 0.040 Uiso 1 1 calc R . . C22 C 0.1314(6) 0.7972(4) 0.3480(4) 0.034(2) Uani 1 1 d . . . H22A H 0.0603 0.8076 0.3666 0.041 Uiso 1 1 calc R . . C23 C 0.1900(6) 0.7371(4) 0.3674(3) 0.0267(18) Uani 1 1 d . . . H23A H 0.1590 0.7053 0.3996 0.032 Uiso 1 1 calc R . . C24 C 0.2934(6) 0.7221(4) 0.3409(3) 0.0228(17) Uani 1 1 d . . . H24A H 0.3334 0.6803 0.3554 0.027 Uiso 1 1 calc R . . C25 C 0.6845(5) 0.5424(3) 0.2886(3) 0.0162(15) Uani 1 1 d . . . C26 C 0.7605(6) 0.5683(4) 0.2404(3) 0.0215(16) Uani 1 1 d . . . H26A H 0.7338 0.5957 0.2038 0.026 Uiso 1 1 calc R . . C27 C 0.8737(6) 0.5540(4) 0.2464(4) 0.0321(19) Uani 1 1 d . . . H27A H 0.9237 0.5729 0.2142 0.039 Uiso 1 1 calc R . . C28 C 0.9150(6) 0.5136(4) 0.2970(4) 0.0283(17) Uani 1 1 d . . . H28A H 0.9928 0.5040 0.3003 0.034 Uiso 1 1 calc R . . C29 C 0.8422(7) 0.4872(4) 0.3432(3) 0.031(2) Uani 1 1 d . . . H29A H 0.8707 0.4589 0.3787 0.037 Uiso 1 1 calc R . . C30 C 0.7259(6) 0.5004(3) 0.3401(3) 0.0204(16) Uani 1 1 d . . . H30A H 0.6771 0.4809 0.3726 0.024 Uiso 1 1 calc R . . C31 C 0.4730(6) 0.5593(3) 0.3573(3) 0.0184(10) Uani 1 1 d . . . C32 C 0.3664(6) 0.5309(3) 0.3635(3) 0.0184(10) Uani 1 1 d . . . H32A H 0.3326 0.5069 0.3270 0.022 Uiso 1 1 calc R . . C33 C 0.3078(6) 0.5374(3) 0.4235(3) 0.0231(17) Uani 1 1 d . . . H33A H 0.2354 0.5169 0.4277 0.028 Uiso 1 1 calc R . . C34 C 0.3549(6) 0.5731(4) 0.4757(3) 0.0271(18) Uani 1 1 d . . . H34A H 0.3136 0.5780 0.5155 0.033 Uiso 1 1 calc R . . C35 C 0.4608(7) 0.6023(3) 0.4720(3) 0.0257(17) Uani 1 1 d . . . H35A H 0.4925 0.6272 0.5087 0.031 Uiso 1 1 calc R . . C36 C 0.5214(7) 0.5943(3) 0.4120(3) 0.0214(15) Uani 1 1 d . . . H36A H 0.5953 0.6127 0.4089 0.026 Uiso 1 1 calc R . . C37 C 0.2960(6) 0.4991(3) 0.1551(3) 0.0173(16) Uani 1 1 d . . . C38 C 0.2604(6) 0.4288(4) 0.1688(3) 0.0246(17) Uani 1 1 d . . . H38A H 0.3133 0.3929 0.1817 0.030 Uiso 1 1 calc R . . C39 C 0.1475(6) 0.4101(4) 0.1638(3) 0.0217(16) Uani 1 1 d . . . H39A H 0.1229 0.3625 0.1753 0.026 Uiso 1 1 calc R . . C40 C 0.0726(6) 0.4617(3) 0.1420(3) 0.0239(17) Uani 1 1 d . . . H40A H -0.0039 0.4490 0.1372 0.029 Uiso 1 1 calc R . . C41 C 0.1067(6) 0.5313(4) 0.1270(3) 0.0238(16) Uani 1 1 d . . . H41A H 0.0543 0.5664 0.1118 0.029 Uiso 1 1 calc R . . C42 C 0.2200(6) 0.5504(3) 0.1344(3) 0.0207(16) Uani 1 1 d . . . H42A H 0.2438 0.5987 0.1250 0.025 Uiso 1 1 calc R . . C43 C 0.5120(6) 0.4796(3) 0.0980(3) 0.0189(17) Uani 1 1 d . . . C44 C 0.6181(6) 0.4499(3) 0.1062(3) 0.0198(16) Uani 1 1 d . . . H44A H 0.6529 0.4519 0.1483 0.024 Uiso 1 1 calc R . . C45 C 0.6732(7) 0.4179(3) 0.0541(3) 0.0268(18) Uani 1 1 d . . . H45A H 0.7452 0.3973 0.0604 0.032 Uiso 1 1 calc R . . C46 C 0.6220(7) 0.4158(4) -0.0086(4) 0.031(2) Uani 1 1 d . . . H46A H 0.6598 0.3943 -0.0450 0.037 Uiso 1 1 calc R . . C47 C 0.5172(7) 0.4449(3) -0.0172(3) 0.0298(18) Uani 1 1 d . . . H47A H 0.4825 0.4438 -0.0594 0.036 Uiso 1 1 calc R . . C48 C 0.4623(7) 0.4760(3) 0.0363(3) 0.0215(15) Uani 1 1 d . . . H48A H 0.3892 0.4951 0.0305 0.026 Uiso 1 1 calc R . . Cl2 Cl 1.0401(3) 0.71538(15) 0.10777(14) 0.0980(8) Uani 1 1 d . . . C50A C 1.0583(18) 0.7492(11) 0.1804(9) 0.0980(8) Uani 0.60 1 d P A 1 H50A H 1.0686 0.8025 0.1761 0.118 Uiso 0.60 1 calc PR A 1 H50B H 1.1280 0.7288 0.1992 0.118 Uiso 0.60 1 calc PR A 1 C50B C 1.075(3) 0.7003(17) 0.2018(14) 0.0980(8) Uani 0.40 1 d P A 2 H50C H 1.0887 0.6483 0.2119 0.118 Uiso 0.40 1 calc PR A 2 H50D H 1.1393 0.7299 0.2162 0.118 Uiso 0.40 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0164(5) 0.0153(5) 0.0097(4) 0.0007(4) 0.0001(4) 0.0003(4) P1 0.0166(10) 0.0155(8) 0.0124(7) -0.0004(6) -0.0023(8) 0.0007(8) N1 0.011(3) 0.021(3) 0.013(2) -0.005(2) -0.005(2) -0.002(2) B1 0.015(4) 0.022(4) 0.018(3) 0.009(3) -0.002(4) -0.002(4) C1 0.015(4) 0.014(3) 0.019(3) 0.000(3) 0.001(3) -0.001(3) Cl1 0.120(2) 0.0884(14) 0.0853(12) -0.0007(11) 0.0448(15) 0.0071(14) P2 0.0167(9) 0.0172(8) 0.0132(8) 0.0003(6) 0.0000(8) 0.0035(8) N2 0.013(3) 0.008(2) 0.017(2) 0.0024(19) 0.004(2) 0.006(2) C2 0.014(4) 0.022(4) 0.013(3) 0.003(3) 0.000(3) 0.001(3) P3 0.0170(11) 0.0161(7) 0.0120(7) -0.0008(6) -0.0007(8) -0.0011(9) C3 0.027(5) 0.027(4) 0.031(4) -0.007(3) 0.013(4) -0.003(4) P4 0.0177(11) 0.0132(8) 0.0113(7) -0.0003(6) 0.0007(7) 0.0006(7) C4 0.013(3) 0.047(4) 0.034(3) 0.002(3) -0.004(2) -0.008(3) C5 0.013(3) 0.047(4) 0.034(3) 0.002(3) -0.004(2) -0.008(3) C6 0.030(5) 0.028(4) 0.014(3) 0.004(3) 0.001(3) -0.004(4) C7 0.025(4) 0.010(3) 0.022(4) -0.002(3) -0.003(3) 0.007(3) C8 0.020(5) 0.019(4) 0.027(4) 0.001(3) 0.006(3) 0.004(3) C9 0.026(5) 0.022(4) 0.034(4) 0.010(3) -0.011(4) -0.004(3) C10 0.041(6) 0.026(4) 0.030(4) -0.004(3) -0.015(4) 0.008(4) C11 0.031(5) 0.009(3) 0.022(4) 0.000(3) -0.002(3) 0.001(3) C12 0.018(4) 0.021(3) 0.018(3) -0.005(2) -0.007(3) 0.001(3) C13 0.029(3) 0.017(2) 0.018(2) -0.0002(18) -0.003(2) 0.006(2) C14 0.028(5) 0.019(4) 0.014(3) -0.003(3) -0.003(3) -0.001(3) C15 0.025(5) 0.026(4) 0.024(4) 0.001(3) -0.003(3) 0.008(3) C16 0.038(5) 0.017(4) 0.029(4) -0.003(3) -0.019(4) -0.002(4) C17 0.045(6) 0.028(4) 0.021(4) -0.007(3) -0.017(4) 0.009(4) C18 0.029(3) 0.017(2) 0.018(2) -0.0002(18) -0.003(2) 0.006(2) C19 0.021(4) 0.015(3) 0.009(3) -0.003(3) 0.009(3) -0.001(3) C20 0.019(4) 0.027(4) 0.014(3) 0.003(3) 0.005(3) 0.003(3) C21 0.033(5) 0.035(4) 0.033(4) 0.007(4) 0.011(4) 0.009(4) C22 0.021(5) 0.039(5) 0.042(5) 0.005(4) 0.013(4) 0.017(4) C23 0.028(5) 0.036(5) 0.016(4) 0.009(3) 0.012(3) -0.001(4) C24 0.029(5) 0.018(4) 0.021(4) 0.003(3) -0.008(3) 0.007(3) C25 0.015(4) 0.020(4) 0.013(3) -0.003(3) -0.002(3) 0.004(3) C26 0.028(5) 0.024(4) 0.013(3) 0.001(3) 0.002(3) -0.005(3) C27 0.029(5) 0.030(4) 0.037(4) 0.007(4) 0.013(4) 0.000(4) C28 0.016(4) 0.033(4) 0.036(4) -0.009(4) -0.003(4) -0.002(3) C29 0.046(6) 0.027(4) 0.020(4) -0.007(3) -0.017(4) 0.011(4) C30 0.022(5) 0.024(4) 0.016(3) -0.004(3) -0.002(3) 0.006(3) C31 0.025(3) 0.018(2) 0.012(2) -0.0003(19) 0.003(2) 0.005(2) C32 0.025(3) 0.018(2) 0.012(2) -0.0003(19) 0.003(2) 0.005(2) C33 0.021(5) 0.021(4) 0.027(4) 0.009(3) 0.004(3) -0.004(3) C34 0.029(5) 0.033(4) 0.019(4) 0.008(3) 0.016(3) 0.005(4) C35 0.046(5) 0.019(3) 0.012(3) 0.007(2) 0.005(4) 0.001(4) C36 0.025(4) 0.022(3) 0.017(3) 0.007(2) 0.000(3) 0.006(3) C37 0.020(4) 0.018(3) 0.013(3) -0.008(3) -0.002(3) 0.002(3) C38 0.030(5) 0.026(4) 0.018(3) -0.001(3) 0.002(3) 0.004(3) C39 0.030(5) 0.024(4) 0.011(3) -0.004(3) 0.000(3) -0.001(3) C40 0.015(4) 0.030(4) 0.027(4) -0.014(3) 0.006(3) -0.007(3) C41 0.020(4) 0.026(4) 0.025(4) 0.006(3) 0.000(3) 0.014(3) C42 0.024(4) 0.022(4) 0.016(3) 0.004(3) 0.007(3) -0.003(3) C43 0.033(5) 0.013(3) 0.010(3) -0.001(2) 0.003(3) 0.003(3) C44 0.028(5) 0.017(4) 0.014(3) 0.005(3) 0.000(3) 0.001(3) C45 0.029(5) 0.016(4) 0.035(4) 0.007(3) 0.013(4) 0.008(3) C46 0.048(6) 0.021(4) 0.025(4) -0.009(3) 0.019(4) -0.004(4) C47 0.042(6) 0.029(4) 0.018(3) -0.002(3) -0.007(4) -0.003(4) C48 0.023(4) 0.019(3) 0.023(3) -0.007(3) 0.002(3) 0.001(4) Cl2 0.120(2) 0.0884(14) 0.0853(12) -0.0007(11) 0.0448(15) 0.0071(14) C50A 0.120(2) 0.0884(14) 0.0853(12) -0.0007(11) 0.0448(15) 0.0071(14) C50B 0.120(2) 0.0884(14) 0.0853(12) -0.0007(11) 0.0448(15) 0.0071(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 B1 2.072(6) . ? Fe1 P3 2.1707(18) . ? Fe1 P4 2.1920(19) . ? Fe1 P2 2.2558(17) . ? Fe1 H1FE 1.5211 . ? Fe1 H3B1 1.6610 . ? Fe1 H1B1 1.5206 . ? P1 N1 1.628(5) . ? P1 C1 1.812(7) . ? P1 C7 1.818(6) . ? P1 B1 1.965(7) . ? N1 P2 1.666(5) . ? B1 H3B1 1.1953 . ? B1 H2B1 1.24(6) . ? B1 H1B1 1.1370 . ? C1 C6 1.393(9) . ? C1 C2 1.407(8) . ? Cl1 C50B 1.82(3) . ? Cl1 C50A 1.828(18) . ? P2 C13 1.823(7) . ? P2 C19 1.856(6) . ? N2 P3 1.687(5) . ? N2 P4 1.706(5) . ? N2 H1N2 1.07(5) . ? C2 C3 1.362(10) . ? C2 H2A 0.9500 . ? P3 C31 1.818(6) . ? P3 C25 1.831(7) . ? P3 P4 2.549(2) . ? C3 C4 1.400(9) . ? C3 H3A 0.9500 . ? P4 C37 1.834(7) . ? P4 C43 1.842(6) . ? C4 C5 1.350(9) . ? C4 H4A 0.9500 . ? C5 C6 1.395(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.392(8) . ? C7 C8 1.404(9) . ? C8 C9 1.380(9) . ? C8 H8A 0.9500 . ? C9 C10 1.362(10) . ? C9 H9A 0.9500 . ? C10 C11 1.404(10) . ? C10 H10A 0.9500 . ? C11 C12 1.392(9) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.385(9) . ? C13 C18 1.410(8) . ? C14 C15 1.385(9) . ? C14 H14A 0.9500 . ? C15 C16 1.368(9) . ? C15 H15A 0.9500 . ? C16 C17 1.380(11) . ? C16 H16A 0.9500 . ? C17 C18 1.422(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.385(9) . ? C19 C24 1.392(9) . ? C20 C21 1.384(9) . ? C20 H20A 0.9500 . ? C21 C22 1.412(10) . ? C21 H21A 0.9500 . ? C22 C23 1.365(9) . ? C22 H22A 0.9500 . ? C23 C24 1.378(10) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.386(8) . ? C25 C26 1.417(8) . ? C26 C27 1.387(10) . ? C26 H26A 0.9500 . ? C27 C28 1.357(10) . ? C27 H27A 0.9500 . ? C28 C29 1.366(10) . ? C28 H28A 0.9500 . ? C29 C30 1.416(10) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.386(10) . ? C31 C36 1.403(8) . ? C32 C33 1.406(9) . ? C32 H32A 0.9500 . ? C33 C34 1.364(9) . ? C33 H33A 0.9500 . ? C34 C35 1.379(11) . ? C34 H34A 0.9500 . ? C35 C36 1.421(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.376(9) . ? C37 C38 1.386(9) . ? C38 C39 1.399(10) . ? C38 H38A 0.9500 . ? C39 C40 1.378(9) . ? C39 H39A 0.9500 . ? C40 C41 1.375(9) . ? C40 H40A 0.9500 . ? C41 C42 1.408(9) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C48 1.383(8) . ? C43 C44 1.393(9) . ? C44 C45 1.374(9) . ? C44 H44A 0.9500 . ? C45 C46 1.411(10) . ? C45 H45A 0.9500 . ? C46 C47 1.375(11) . ? C46 H46A 0.9500 . ? C47 C48 1.388(8) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? Cl2 C50A 1.610(18) . ? Cl2 C50B 1.97(3) . ? C50A H50A 0.9900 . ? C50A H50B 0.9900 . ? C50B H50C 0.9900 . ? C50B H50D 0.9900 . ? 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 B1 Fe1 P3 144.9(2) . . ? B1 Fe1 P4 104.34(19) . . ? P3 Fe1 P4 71.52(7) . . ? B1 Fe1 P2 88.4(2) . . ? P3 Fe1 P2 103.04(7) . . ? P4 Fe1 P2 164.59(8) . . ? B1 Fe1 H1FE 124.0 . . ? P3 Fe1 H1FE 90.7 . . ? P4 Fe1 H1FE 83.6 . . ? P2 Fe1 H1FE 82.1 . . ? B1 Fe1 H3B1 35.2 . . ? P3 Fe1 H3B1 110.6 . . ? P4 Fe1 H3B1 104.8 . . ? P2 Fe1 H3B1 90.6 . . ? H1FE Fe1 H3B1 158.6 . . ? B1 Fe1 H1B1 32.5 . . ? P3 Fe1 H1B1 173.2 . . ? P4 Fe1 H1B1 102.3 . . ? P2 Fe1 H1B1 83.6 . . ? H1FE Fe1 H1B1 91.5 . . ? H3B1 Fe1 H1B1 67.6 . . ? N1 P1 C1 110.2(3) . . ? N1 P1 C7 111.7(3) . . ? C1 P1 C7 106.0(3) . . ? N1 P1 B1 110.9(3) . . ? C1 P1 B1 110.9(3) . . ? C7 P1 B1 107.1(3) . . ? P1 N1 P2 113.9(3) . . ? P1 B1 Fe1 111.5(3) . . ? P1 B1 H3B1 105.5 . . ? Fe1 B1 H3B1 53.2 . . ? P1 B1 H2B1 115(3) . . ? Fe1 B1 H2B1 133(3) . . ? H3B1 B1 H2B1 120.0 . . ? P1 B1 H1B1 98.2 . . ? Fe1 B1 H1B1 46.0 . . ? H3B1 B1 H1B1 99.0 . . ? H2B1 B1 H1B1 116.1 . . ? C6 C1 C2 118.2(6) . . ? C6 C1 P1 119.0(5) . . ? C2 C1 P1 122.5(5) . . ? N1 P2 C13 104.2(3) . . ? N1 P2 C19 103.9(3) . . ? C13 P2 C19 102.1(3) . . ? N1 P2 Fe1 115.33(16) . . ? C13 P2 Fe1 116.4(2) . . ? C19 P2 Fe1 113.3(2) . . ? P3 N2 P4 97.4(2) . . ? P3 N2 H1N2 131(3) . . ? P4 N2 H1N2 132(3) . . ? C3 C2 C1 120.4(7) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? N2 P3 C31 105.2(3) . . ? N2 P3 C25 104.2(3) . . ? C31 P3 C25 105.6(3) . . ? N2 P3 Fe1 96.03(17) . . ? C31 P3 Fe1 120.4(2) . . ? C25 P3 Fe1 122.2(2) . . ? C31 P3 P4 126.7(2) . . ? C25 P3 P4 120.6(2) . . ? Fe1 P3 P4 54.63(6) . . ? C2 C3 C4 121.1(7) . . ? C2 C3 H3A 119.5 . . ? C4 C3 H3A 119.5 . . ? N2 P4 C37 107.0(3) . . ? N2 P4 C43 105.8(2) . . ? C37 P4 C43 101.9(3) . . ? N2 P4 Fe1 94.71(16) . . ? C37 P4 Fe1 119.1(2) . . ? C43 P4 Fe1 126.0(2) . . ? C37 P4 P3 126.9(2) . . ? C43 P4 P3 124.4(2) . . ? Fe1 P4 P3 53.85(6) . . ? C5 C4 C3 118.8(7) . . ? C5 C4 H4A 120.6 . . ? C3 C4 H4A 120.6 . . ? C4 C5 C6 121.6(7) . . ? C4 C5 H5A 119.2 . . ? C6 C5 H5A 119.2 . . ? C1 C6 C5 119.9(6) . . ? C1 C6 H6A 120.1 . . ? C5 C6 H6A 120.1 . . ? C12 C7 C8 116.9(6) . . ? C12 C7 P1 126.2(6) . . ? C8 C7 P1 117.0(5) . . ? C9 C8 C7 121.5(7) . . ? C9 C8 H8A 119.2 . . ? C7 C8 H8A 119.2 . . ? C10 C9 C8 120.8(7) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 119.8(7) . . ? C9 C10 H10A 120.1 . . ? C11 C10 H10A 120.1 . . ? C12 C11 C10 118.9(6) . . ? C12 C11 H11A 120.5 . . ? C10 C11 H11A 120.5 . . ? C11 C12 C7 122.1(7) . . ? C11 C12 H12A 119.0 . . ? C7 C12 H12A 119.0 . . ? C14 C13 C18 117.0(6) . . ? C14 C13 P2 118.4(5) . . ? C18 C13 P2 124.6(5) . . ? C13 C14 C15 121.7(6) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C16 C15 C14 121.1(7) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C15 C16 C17 119.9(6) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C18 119.2(6) . . ? C16 C17 H17A 120.4 . . ? C18 C17 H17A 120.4 . . ? C13 C18 C17 121.0(7) . . ? C13 C18 H18A 119.5 . . ? C17 C18 H18A 119.5 . . ? C20 C19 C24 119.4(6) . . ? C20 C19 P2 120.5(5) . . ? C24 C19 P2 120.1(5) . . ? C21 C20 C19 119.6(6) . . ? C21 C20 H20A 120.2 . . ? C19 C20 H20A 120.2 . . ? C20 C21 C22 120.7(7) . . ? C20 C21 H21A 119.7 . . ? C22 C21 H21A 119.7 . . ? C23 C22 C21 118.8(7) . . ? C23 C22 H22A 120.6 . . ? C21 C22 H22A 120.6 . . ? C22 C23 C24 120.8(6) . . ? C22 C23 H23A 119.6 . . ? C24 C23 H23A 119.6 . . ? C23 C24 C19 120.7(6) . . ? C23 C24 H24A 119.6 . . ? C19 C24 H24A 119.6 . . ? C30 C25 C26 118.2(6) . . ? C30 C25 P3 124.0(5) . . ? C26 C25 P3 117.6(5) . . ? C27 C26 C25 120.3(6) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C28 C27 C26 121.8(7) . . ? C28 C27 H27A 119.1 . . ? C26 C27 H27A 119.1 . . ? C27 C28 C29 118.4(7) . . ? C27 C28 H28A 120.8 . . ? C29 C28 H28A 120.8 . . ? C28 C29 C30 122.5(6) . . ? C28 C29 H29A 118.7 . . ? C30 C29 H29A 118.7 . . ? C25 C30 C29 118.7(6) . . ? C25 C30 H30A 120.7 . . ? C29 C30 H30A 120.7 . . ? C32 C31 C36 118.7(6) . . ? C32 C31 P3 118.1(5) . . ? C36 C31 P3 122.6(6) . . ? C31 C32 C33 120.4(6) . . ? C31 C32 H32A 119.8 . . ? C33 C32 H32A 119.8 . . ? C34 C33 C32 120.1(7) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C33 C34 C35 121.7(6) . . ? C33 C34 H34A 119.1 . . ? C35 C34 H34A 119.1 . . ? C34 C35 C36 118.4(6) . . ? C34 C35 H35A 120.8 . . ? C36 C35 H35A 120.8 . . ? C31 C36 C35 120.6(7) . . ? C31 C36 H36A 119.7 . . ? C35 C36 H36A 119.7 . . ? C42 C37 C38 119.6(7) . . ? C42 C37 P4 118.6(5) . . ? C38 C37 P4 121.7(5) . . ? C37 C38 C39 120.8(7) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C40 C39 C38 118.9(6) . . ? C40 C39 H39A 120.5 . . ? C38 C39 H39A 120.5 . . ? C39 C40 C41 121.0(7) . . ? C39 C40 H40A 119.5 . . ? C41 C40 H40A 119.5 . . ? C40 C41 C42 119.6(6) . . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 120.2 . . ? C37 C42 C41 120.0(6) . . ? C37 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C48 C43 C44 118.7(6) . . ? C48 C43 P4 120.5(5) . . ? C44 C43 P4 120.7(5) . . ? C45 C44 C43 121.0(6) . . ? C45 C44 H44A 119.5 . . ? C43 C44 H44A 119.5 . . ? C44 C45 C46 119.4(7) . . ? C44 C45 H45A 120.3 . . ? C46 C45 H45A 120.3 . . ? C47 C46 C45 120.0(7) . . ? C47 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C46 C47 C48 119.6(6) . . ? C46 C47 H47A 120.2 . . ? C48 C47 H47A 120.2 . . ? C43 C48 C47 121.2(7) . . ? C43 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? Cl2 C50A Cl1 115.0(12) . . ? Cl2 C50A H50A 108.5 . . ? Cl1 C50A H50A 108.5 . . ? Cl2 C50A H50B 108.5 . . ? Cl1 C50A H50B 108.5 . . ? H50A C50A H50B 107.5 . . ? Cl1 C50B Cl2 99.9(16) . . ? Cl1 C50B H50C 111.8 . . ? Cl2 C50B H50C 111.8 . . ? Cl1 C50B H50D 111.8 . . ? Cl2 C50B H50D 111.8 . . ? H50C C50B H50D 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 P1 N1 P2 -123.7(3) . . . . ? C7 P1 N1 P2 118.8(4) . . . . ? B1 P1 N1 P2 -0.6(5) . . . . ? N1 P1 B1 Fe1 0.5(5) . . . . ? C1 P1 B1 Fe1 123.3(4) . . . . ? C7 P1 B1 Fe1 -121.5(4) . . . . ? P3 Fe1 B1 P1 -110.9(4) . . . . ? P4 Fe1 B1 P1 170.9(3) . . . . ? P2 Fe1 B1 P1 -0.3(4) . . . . ? N1 P1 C1 C6 10.9(6) . . . . ? C7 P1 C1 C6 131.9(5) . . . . ? B1 P1 C1 C6 -112.2(5) . . . . ? N1 P1 C1 C2 -175.9(5) . . . . ? C7 P1 C1 C2 -54.9(6) . . . . ? B1 P1 C1 C2 61.0(6) . . . . ? P1 N1 P2 C13 129.2(3) . . . . ? P1 N1 P2 C19 -124.2(3) . . . . ? P1 N1 P2 Fe1 0.4(4) . . . . ? B1 Fe1 P2 N1 0.0(3) . . . . ? P3 Fe1 P2 N1 146.5(2) . . . . ? P4 Fe1 P2 N1 -146.1(3) . . . . ? B1 Fe1 P2 C13 -122.6(3) . . . . ? P3 Fe1 P2 C13 23.9(3) . . . . ? P4 Fe1 P2 C13 91.3(4) . . . . ? B1 Fe1 P2 C19 119.5(3) . . . . ? P3 Fe1 P2 C19 -94.0(2) . . . . ? P4 Fe1 P2 C19 -26.6(4) . . . . ? C6 C1 C2 C3 -1.4(10) . . . . ? P1 C1 C2 C3 -174.7(5) . . . . ? P4 N2 P3 C31 128.7(3) . . . . ? P4 N2 P3 C25 -120.5(3) . . . . ? P4 N2 P3 Fe1 4.9(2) . . . . ? B1 Fe1 P3 N2 -92.8(4) . . . . ? P4 Fe1 P3 N2 -4.00(19) . . . . ? P2 Fe1 P3 N2 161.01(19) . . . . ? B1 Fe1 P3 C31 155.6(4) . . . . ? P4 Fe1 P3 C31 -115.6(3) . . . . ? P2 Fe1 P3 C31 49.4(3) . . . . ? B1 Fe1 P3 C25 18.2(4) . . . . ? P4 Fe1 P3 C25 106.9(2) . . . . ? P2 Fe1 P3 C25 -88.1(2) . . . . ? B1 Fe1 P3 P4 -88.8(3) . . . . ? P2 Fe1 P3 P4 165.01(8) . . . . ? C1 C2 C3 C4 0.2(11) . . . . ? P3 N2 P4 C37 -127.2(3) . . . . ? P3 N2 P4 C43 124.6(3) . . . . ? P3 N2 P4 Fe1 -4.9(2) . . . . ? B1 Fe1 P4 N2 147.6(3) . . . . ? P3 Fe1 P4 N2 3.95(19) . . . . ? P2 Fe1 P4 N2 -67.5(4) . . . . ? B1 Fe1 P4 C37 -100.0(3) . . . . ? P3 Fe1 P4 C37 116.4(2) . . . . ? P2 Fe1 P4 C37 44.9(4) . . . . ? B1 Fe1 P4 C43 34.1(4) . . . . ? P3 Fe1 P4 C43 -109.5(3) . . . . ? P2 Fe1 P4 C43 179.0(3) . . . . ? B1 Fe1 P4 P3 143.6(3) . . . . ? P2 Fe1 P4 P3 -71.5(3) . . . . ? C31 P3 P4 N2 -69.8(4) . . . . ? C25 P3 P4 N2 76.2(4) . . . . ? Fe1 P3 P4 N2 -174.0(3) . . . . ? N2 P3 P4 C37 72.2(4) . . . . ? C31 P3 P4 C37 2.4(4) . . . . ? C25 P3 P4 C37 148.4(3) . . . . ? Fe1 P3 P4 C37 -101.7(3) . . . . ? N2 P3 P4 C43 -73.6(4) . . . . ? C31 P3 P4 C43 -143.4(3) . . . . ? C25 P3 P4 C43 2.6(3) . . . . ? Fe1 P3 P4 C43 112.4(2) . . . . ? N2 P3 P4 Fe1 174.0(3) . . . . ? C31 P3 P4 Fe1 104.2(3) . . . . ? C25 P3 P4 Fe1 -109.8(2) . . . . ? C2 C3 C4 C5 0.0(11) . . . . ? C3 C4 C5 C6 1.2(11) . . . . ? C2 C1 C6 C5 2.5(10) . . . . ? P1 C1 C6 C5 176.1(5) . . . . ? C4 C5 C6 C1 -2.5(11) . . . . ? N1 P1 C7 C12 108.9(5) . . . . ? C1 P1 C7 C12 -11.1(6) . . . . ? B1 P1 C7 C12 -129.6(6) . . . . ? N1 P1 C7 C8 -72.0(6) . . . . ? C1 P1 C7 C8 167.9(5) . . . . ? B1 P1 C7 C8 49.5(6) . . . . ? C12 C7 C8 C9 0.7(10) . . . . ? P1 C7 C8 C9 -178.5(5) . . . . ? C7 C8 C9 C10 -0.2(11) . . . . ? C8 C9 C10 C11 0.8(11) . . . . ? C9 C10 C11 C12 -1.9(10) . . . . ? C10 C11 C12 C7 2.4(9) . . . . ? C8 C7 C12 C11 -1.8(9) . . . . ? P1 C7 C12 C11 177.3(5) . . . . ? N1 P2 C13 C14 -79.3(5) . . . . ? C19 P2 C13 C14 172.8(5) . . . . ? Fe1 P2 C13 C14 48.9(6) . . . . ? N1 P2 C13 C18 99.4(6) . . . . ? C19 P2 C13 C18 -8.5(6) . . . . ? Fe1 P2 C13 C18 -132.4(5) . . . . ? C18 C13 C14 C15 2.8(10) . . . . ? P2 C13 C14 C15 -178.4(5) . . . . ? C13 C14 C15 C16 -1.3(11) . . . . ? C14 C15 C16 C17 -0.7(11) . . . . ? C15 C16 C17 C18 1.0(11) . . . . ? C14 C13 C18 C17 -2.4(9) . . . . ? P2 C13 C18 C17 178.8(5) . . . . ? C16 C17 C18 C13 0.6(10) . . . . ? N1 P2 C19 C20 8.8(6) . . . . ? C13 P2 C19 C20 116.9(5) . . . . ? Fe1 P2 C19 C20 -117.1(5) . . . . ? N1 P2 C19 C24 -172.5(5) . . . . ? C13 P2 C19 C24 -64.4(5) . . . . ? Fe1 P2 C19 C24 61.6(6) . . . . ? C24 C19 C20 C21 -0.4(9) . . . . ? P2 C19 C20 C21 178.3(5) . . . . ? C19 C20 C21 C22 0.1(11) . . . . ? C20 C21 C22 C23 -0.2(11) . . . . ? C21 C22 C23 C24 0.5(11) . . . . ? C22 C23 C24 C19 -0.7(11) . . . . ? C20 C19 C24 C23 0.7(10) . . . . ? P2 C19 C24 C23 -178.0(5) . . . . ? N2 P3 C25 C30 -80.9(5) . . . . ? C31 P3 C25 C30 29.7(6) . . . . ? Fe1 P3 C25 C30 172.4(4) . . . . ? P4 P3 C25 C30 -122.6(5) . . . . ? N2 P3 C25 C26 94.3(5) . . . . ? C31 P3 C25 C26 -155.1(5) . . . . ? Fe1 P3 C25 C26 -12.3(5) . . . . ? P4 P3 C25 C26 52.7(5) . . . . ? C30 C25 C26 C27 -2.4(9) . . . . ? P3 C25 C26 C27 -177.9(5) . . . . ? C25 C26 C27 C28 1.7(11) . . . . ? C26 C27 C28 C29 -0.4(11) . . . . ? C27 C28 C29 C30 -0.1(10) . . . . ? C26 C25 C30 C29 1.9(9) . . . . ? P3 C25 C30 C29 177.1(5) . . . . ? C28 C29 C30 C25 -0.7(10) . . . . ? N2 P3 C31 C32 -34.1(6) . . . . ? C25 P3 C31 C32 -143.9(5) . . . . ? Fe1 P3 C31 C32 72.6(5) . . . . ? P4 P3 C31 C32 6.1(6) . . . . ? N2 P3 C31 C36 154.8(5) . . . . ? C25 P3 C31 C36 44.9(6) . . . . ? Fe1 P3 C31 C36 -98.6(6) . . . . ? P4 P3 C31 C36 -165.0(4) . . . . ? C36 C31 C32 C33 0.3(9) . . . . ? P3 C31 C32 C33 -171.2(5) . . . . ? C31 C32 C33 C34 1.3(10) . . . . ? C32 C33 C34 C35 -1.4(10) . . . . ? C33 C34 C35 C36 -0.2(10) . . . . ? C32 C31 C36 C35 -1.9(9) . . . . ? P3 C31 C36 C35 169.2(5) . . . . ? C34 C35 C36 C31 1.9(9) . . . . ? N2 P4 C37 C42 139.0(5) . . . . ? C43 P4 C37 C42 -110.1(5) . . . . ? Fe1 P4 C37 C42 33.4(5) . . . . ? P3 P4 C37 C42 98.2(5) . . . . ? N2 P4 C37 C38 -38.8(6) . . . . ? C43 P4 C37 C38 72.1(5) . . . . ? Fe1 P4 C37 C38 -144.4(4) . . . . ? P3 P4 C37 C38 -79.6(6) . . . . ? C42 C37 C38 C39 -2.1(9) . . . . ? P4 C37 C38 C39 175.7(5) . . . . ? C37 C38 C39 C40 3.1(10) . . . . ? C38 C39 C40 C41 -1.9(9) . . . . ? C39 C40 C41 C42 -0.3(9) . . . . ? C38 C37 C42 C41 -0.1(9) . . . . ? P4 C37 C42 C41 -178.0(5) . . . . ? C40 C41 C42 C37 1.3(9) . . . . ? N2 P4 C43 C48 152.0(5) . . . . ? C37 P4 C43 C48 40.2(5) . . . . ? Fe1 P4 C43 C48 -99.8(5) . . . . ? P3 P4 C43 C48 -167.1(4) . . . . ? N2 P4 C43 C44 -31.0(6) . . . . ? C37 P4 C43 C44 -142.8(5) . . . . ? Fe1 P4 C43 C44 77.1(5) . . . . ? P3 P4 C43 C44 9.9(6) . . . . ? C48 C43 C44 C45 0.3(9) . . . . ? P4 C43 C44 C45 -176.7(5) . . . . ? C43 C44 C45 C46 0.8(10) . . . . ? C44 C45 C46 C47 -0.8(11) . . . . ? C45 C46 C47 C48 -0.2(11) . . . . ? C44 C43 C48 C47 -1.4(9) . . . . ? P4 C43 C48 C47 175.6(5) . . . . ? C46 C47 C48 C43 1.3(10) . . . . ? C50B Cl2 C50A Cl1 -74(2) . . . . ? C50B Cl1 C50A Cl2 87(3) . . . . ? C50A Cl1 C50B Cl2 -48.8(19) . . . . ? C50A Cl2 C50B Cl1 62(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.67 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.638 _refine_diff_density_min -1.392 _refine_diff_density_rms 0.100 _database_code_depnum_ccdc_archive 'CCDC 923303' ####################################################################### # # 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_Compound2 #TrackingRef '17446_web_deposit_cif_file_1_RobertLanger_1359917457.compound2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Fe N4 P4, Cl4 Fe, C2 H3 N ' _chemical_formula_sum 'C54 H51 Cl4 Fe2 N5 P4' _chemical_formula_weight 1147.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 22.401(5) _cell_length_b 12.421(3) _cell_length_c 19.403(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5398.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 61659 _cell_measurement_theta_min 1.81 _cell_measurement_theta_max 34.1 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 0.895 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8413 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details 'Stoe, X-Area Ver. 1.56' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE Stadi Vari' _diffrn_measurement_method omega-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69797 _diffrn_reflns_av_R_equivalents 0.0771 _diffrn_reflns_av_sigmaI/netI 0.0850 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 30.51 _reflns_number_total 16368 _reflns_number_gt 11420 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.56 (Stoe 2011)' _computing_cell_refinement 'X-Area 1.56 (Stoe 2011)' _computing_data_reduction 'X-Area 1.56 (Stoe 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2g (Brandenburg 2011)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.015(12) _refine_ls_number_reflns 16368 _refine_ls_number_parameters 619 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0762 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0808 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.971 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.367489(19) 0.50950(3) 1.03238(2) 0.02283(8) Uani 1 1 d . . . P1 P 1.42419(4) 0.46964(6) 0.94049(4) 0.02434(16) Uani 1 1 d . . . P2 P 1.31052(4) 0.42976(7) 0.95099(4) 0.02420(16) Uani 1 1 d . . . P3 P 1.34113(4) 0.68110(7) 1.00918(4) 0.02435(15) Uani 1 1 d . . . P4 P 1.30233(4) 0.56666(7) 1.11380(4) 0.02405(16) Uani 1 1 d . . . N1 N 1.37998(18) 0.3680(3) 1.07728(18) 0.0491(7) Uani 1 1 d . . . N2 N 1.43451(13) 0.5688(2) 1.08879(13) 0.0254(5) Uani 1 1 d . . . N3 N 1.36616(12) 0.4288(2) 0.89221(13) 0.0255(5) Uani 1 1 d . . . H3A H 1.3651 0.4116 0.8482 0.031 Uiso 1 1 calc R . . N4 N 1.29728(13) 0.6902(2) 1.07888(14) 0.0274(6) Uani 1 1 d . . . H4D H 1.2767 0.7460 1.0936 0.033 Uiso 1 1 calc R . . C3 C 1.46383(16) 0.6054(3) 1.1255(2) 0.0360(8) Uani 1 1 d . . . C4 C 1.5037(2) 0.6530(4) 1.1772(2) 0.0574(12) Uani 1 1 d . . . H4A H 1.5288 0.5965 1.1974 0.086 Uiso 1 1 calc R . . H4B H 1.4799 0.6870 1.2135 0.086 Uiso 1 1 calc R . . H4C H 1.5291 0.7073 1.1553 0.086 Uiso 1 1 calc R . . C5 C 1.47755(14) 0.3594(3) 0.94663(18) 0.0287(7) Uani 1 1 d . . . C6 C 1.51437(16) 0.3520(3) 1.0044(2) 0.0357(8) Uani 1 1 d . . . H6A H 1.5107 0.4030 1.0407 0.043 Uiso 1 1 calc R . . C7 C 1.55621(18) 0.2705(3) 1.0090(2) 0.0432(9) Uani 1 1 d . . . H7A H 1.5808 0.2649 1.0487 0.052 Uiso 1 1 calc R . . C8 C 1.56239(17) 0.1972(3) 0.9560(2) 0.0447(10) Uani 1 1 d . . . H8A H 1.5916 0.1419 0.9591 0.054 Uiso 1 1 calc R . . C9 C 1.52632(18) 0.2042(3) 0.8989(2) 0.0433(9) Uani 1 1 d . . . H9A H 1.5301 0.1522 0.8633 0.052 Uiso 1 1 calc R . . C10 C 1.48457(16) 0.2856(3) 0.8924(2) 0.0358(8) Uani 1 1 d . . . H10A H 1.4610 0.2915 0.8519 0.043 Uiso 1 1 calc R . . C11 C 1.46635(14) 0.5682(3) 0.89139(17) 0.0265(6) Uani 1 1 d . . . C12 C 1.45382(16) 0.5927(3) 0.82337(19) 0.0354(8) Uani 1 1 d . . . H12A H 1.4221 0.5569 0.8002 0.043 Uiso 1 1 calc R . . C13 C 1.48753(19) 0.6695(4) 0.7889(2) 0.0454(10) Uani 1 1 d . . . H13A H 1.4790 0.6864 0.7422 0.055 Uiso 1 1 calc R . . C14 C 1.5337(2) 0.7216(4) 0.8230(2) 0.0494(10) Uani 1 1 d . . . H14A H 1.5560 0.7756 0.7999 0.059 Uiso 1 1 calc R . . C15 C 1.54762(18) 0.6951(3) 0.8909(2) 0.0417(9) Uani 1 1 d . . . H15A H 1.5804 0.7287 0.9133 0.050 Uiso 1 1 calc R . . C16 C 1.51361(16) 0.6198(3) 0.92529(18) 0.0319(7) Uani 1 1 d . . . H16A H 1.5222 0.6029 0.9720 0.038 Uiso 1 1 calc R . . C17 C 1.28989(16) 0.2895(3) 0.96586(16) 0.0283(7) Uani 1 1 d . . . C18 C 1.33117(19) 0.2072(3) 0.9561(2) 0.0428(9) Uani 1 1 d . . . H18A H 1.3696 0.2235 0.9382 0.051 Uiso 1 1 calc R . . C19 C 1.3167(2) 0.1016(3) 0.9723(2) 0.0517(11) Uani 1 1 d . . . H19A H 1.3448 0.0456 0.9649 0.062 Uiso 1 1 calc R . . C20 C 1.2606(2) 0.0784(3) 0.9994(2) 0.0517(11) Uani 1 1 d . . . H20A H 1.2507 0.0065 1.0114 0.062 Uiso 1 1 calc R . . C21 C 1.2192(2) 0.1597(3) 1.0090(2) 0.0451(9) Uani 1 1 d . . . H21A H 1.1808 0.1439 1.0272 0.054 Uiso 1 1 calc R . . C22 C 1.23434(17) 0.2644(3) 0.99192(17) 0.0351(8) Uani 1 1 d . . . H22A H 1.2058 0.3202 0.9983 0.042 Uiso 1 1 calc R . . C23 C 1.24305(15) 0.4783(3) 0.90962(17) 0.0275(6) Uani 1 1 d . . . C24 C 1.23043(17) 0.4494(3) 0.84142(19) 0.0359(8) Uani 1 1 d . . . H24A H 1.2593 0.4123 0.8145 0.043 Uiso 1 1 calc R . . C25 C 1.17489(19) 0.4759(4) 0.8133(2) 0.0453(9) Uani 1 1 d . . . H25A H 1.1658 0.4564 0.7671 0.054 Uiso 1 1 calc R . . C26 C 1.13315(18) 0.5303(3) 0.8525(2) 0.0431(9) Uani 1 1 d . . . H26A H 1.0953 0.5476 0.8333 0.052 Uiso 1 1 calc R . . C27 C 1.14613(16) 0.5591(3) 0.9185(2) 0.0383(8) Uani 1 1 d . . . H27A H 1.1172 0.5963 0.9453 0.046 Uiso 1 1 calc R . . C28 C 1.20127(15) 0.5346(3) 0.94697(18) 0.0314(7) Uani 1 1 d . . . H28A H 1.2102 0.5569 0.9926 0.038 Uiso 1 1 calc R . . C29 C 1.29814(15) 0.7295(3) 0.93644(17) 0.0291(7) Uani 1 1 d . . . C30 C 1.31226(17) 0.6993(3) 0.86938(18) 0.0361(8) Uani 1 1 d . . . H30A H 1.3438 0.6496 0.8614 0.043 Uiso 1 1 calc R . . C31 C 1.2807(2) 0.7411(4) 0.8140(2) 0.0468(10) Uani 1 1 d . . . H31A H 1.2909 0.7210 0.7683 0.056 Uiso 1 1 calc R . . C32 C 1.2343(2) 0.8122(4) 0.8257(2) 0.0495(10) Uani 1 1 d . . . H32A H 1.2129 0.8415 0.7879 0.059 Uiso 1 1 calc R . . C33 C 1.21908(19) 0.8406(3) 0.8920(2) 0.0452(9) Uani 1 1 d . . . H33A H 1.1868 0.8887 0.8997 0.054 Uiso 1 1 calc R . . C34 C 1.25055(16) 0.7993(3) 0.94759(19) 0.0350(7) Uani 1 1 d . . . H34A H 1.2396 0.8187 0.9932 0.042 Uiso 1 1 calc R . . C35 C 1.39523(14) 0.7904(3) 1.01824(17) 0.0290(7) Uani 1 1 d . . . C36 C 1.42489(16) 0.8308(3) 0.96075(19) 0.0348(8) Uani 1 1 d . . . H36A H 1.4170 0.8018 0.9164 0.042 Uiso 1 1 calc R . . C37 C 1.46596(17) 0.9132(3) 0.9684(2) 0.0437(9) Uani 1 1 d . . . H37A H 1.4863 0.9404 0.9291 0.052 Uiso 1 1 calc R . . C38 C 1.47768(18) 0.9561(3) 1.0323(3) 0.0486(10) Uani 1 1 d . . . H38A H 1.5054 1.0136 1.0369 0.058 Uiso 1 1 calc R . . C39 C 1.44898(18) 0.9155(3) 1.0901(2) 0.0439(9) Uani 1 1 d . . . H39A H 1.4577 0.9438 1.1344 0.053 Uiso 1 1 calc R . . C40 C 1.40788(16) 0.8340(3) 1.0828(2) 0.0364(8) Uani 1 1 d . . . H40A H 1.3878 0.8071 1.1224 0.044 Uiso 1 1 calc R . . C41 C 1.32486(15) 0.5821(3) 1.20369(16) 0.0273(6) Uani 1 1 d . . . C42 C 1.2946(2) 0.6553(3) 1.24561(19) 0.0443(10) Uani 1 1 d . . . H42A H 1.2631 0.6976 1.2271 0.053 Uiso 1 1 calc R . . C43 C 1.3102(2) 0.6660(4) 1.3135(2) 0.0545(12) Uani 1 1 d . . . H43A H 1.2891 0.7153 1.3419 0.065 Uiso 1 1 calc R . . C44 C 1.35635(19) 0.6057(3) 1.34145(18) 0.0422(9) Uani 1 1 d . . . H44A H 1.3677 0.6151 1.3883 0.051 Uiso 1 1 calc R . . C45 C 1.38545(18) 0.5326(3) 1.30067(19) 0.0378(8) Uani 1 1 d . . . H45A H 1.4168 0.4903 1.3196 0.045 Uiso 1 1 calc R . . C46 C 1.36959(16) 0.5195(3) 1.23194(16) 0.0322(7) Uani 1 1 d . . . H46A H 1.3895 0.4675 1.2044 0.039 Uiso 1 1 calc R . . C47 C 1.22686(14) 0.5156(3) 1.12472(16) 0.0292(7) Uani 1 1 d . . . C48 C 1.17730(15) 0.5830(3) 1.11879(19) 0.0369(8) Uani 1 1 d . . . H48A H 1.1824 0.6580 1.1110 0.044 Uiso 1 1 calc R . . C49 C 1.12070(18) 0.5398(4) 1.1243(2) 0.0482(10) Uani 1 1 d . . . H49A H 1.0869 0.5855 1.1197 0.058 Uiso 1 1 calc R . . C50 C 1.11259(18) 0.4324(4) 1.1363(2) 0.0518(11) Uani 1 1 d . . . H50A H 1.0734 0.4037 1.1393 0.062 Uiso 1 1 calc R . . C51 C 1.1616(2) 0.3653(3) 1.1441(2) 0.0455(9) Uani 1 1 d . . . H51A H 1.1561 0.2909 1.1536 0.055 Uiso 1 1 calc R . . C52 C 1.21845(17) 0.4069(3) 1.13802(17) 0.0371(8) Uani 1 1 d . . . H52A H 1.2520 0.3609 1.1430 0.045 Uiso 1 1 calc R . . Fe2 Fe 0.83888(3) 0.08382(5) 0.65251(3) 0.04061(13) Uani 1 1 d . . . Cl4 Cl 0.73605(4) 0.08170(8) 0.64724(5) 0.0434(2) Uani 1 1 d . . . Cl3 Cl 0.85880(4) 0.19613(8) 0.74790(4) 0.03722(19) Uani 1 1 d . . . Cl2 Cl 0.88348(6) -0.08076(9) 0.66415(6) 0.0603(3) Uani 1 1 d . . . Cl1 Cl 0.87862(6) 0.16144(12) 0.55513(6) 0.0653(4) Uani 1 1 d . . . N5 N 0.9892(4) 0.5094(6) 0.7643(3) 0.1101(18) Uani 1 1 d U . . C53 C 0.9423(5) 0.4953(7) 0.7857(4) 0.1069(17) Uani 1 1 d U . . C54 C 0.8808(4) 0.4791(6) 0.8048(3) 0.1054(18) Uani 1 1 d U . . H54A H 0.8672 0.4092 0.7874 0.158 Uiso 1 1 calc R . . H54B H 0.8562 0.5364 0.7848 0.158 Uiso 1 1 calc R . . H54C H 0.8771 0.4805 0.8551 0.158 Uiso 1 1 calc R . . C1 C 1.3828(2) 0.2903(4) 1.1014(2) 0.0532(12) Uani 1 1 d . . . C2 C 1.3843(2) 0.1808(3) 1.1344(2) 0.0491(7) Uani 1 1 d . . . H2A H 1.4199 0.1748 1.1635 0.074 Uiso 1 1 calc R . . H2B H 1.3855 0.1254 1.0985 0.074 Uiso 1 1 calc R . . H2C H 1.3485 0.1710 1.1627 0.074 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02244(18) 0.0230(2) 0.02305(17) -0.00145(17) -0.0009(2) 0.00284(17) P1 0.0223(4) 0.0258(4) 0.0249(4) -0.0023(3) -0.0007(3) 0.0028(3) P2 0.0221(4) 0.0243(4) 0.0262(4) -0.0014(3) 0.0009(3) 0.0013(3) P3 0.0238(4) 0.0236(4) 0.0256(4) 0.0000(3) -0.0006(3) 0.0018(3) P4 0.0234(4) 0.0244(4) 0.0244(4) -0.0021(3) -0.0005(3) 0.0025(3) N1 0.069(2) 0.0376(14) 0.0409(14) -0.0023(11) -0.0045(13) 0.0081(13) N2 0.0350(15) 0.0249(13) 0.0164(11) 0.0007(10) 0.0010(11) 0.0062(11) N3 0.0224(12) 0.0314(14) 0.0226(12) -0.0031(11) -0.0028(11) -0.0003(11) N4 0.0268(14) 0.0272(13) 0.0280(13) -0.0035(11) 0.0028(11) 0.0081(11) C3 0.0279(18) 0.041(2) 0.039(2) 0.0038(16) 0.0073(16) 0.0050(14) C4 0.045(3) 0.073(3) 0.054(3) -0.012(2) -0.014(2) -0.006(2) C5 0.0254(16) 0.0253(15) 0.0353(17) 0.0012(13) 0.0032(14) 0.0035(12) C6 0.0332(19) 0.0357(19) 0.0381(18) 0.0028(15) 0.0002(16) 0.0089(14) C7 0.038(2) 0.046(2) 0.046(2) 0.0076(17) -0.0064(18) 0.0104(16) C8 0.034(2) 0.0321(19) 0.068(3) 0.0064(18) 0.0094(19) 0.0105(14) C9 0.035(2) 0.033(2) 0.062(3) -0.0094(17) 0.0058(19) 0.0027(15) C10 0.0250(17) 0.037(2) 0.045(2) -0.0068(16) 0.0006(16) 0.0015(14) C11 0.0216(15) 0.0251(15) 0.0330(16) -0.0022(13) 0.0035(13) -0.0002(12) C12 0.0313(19) 0.038(2) 0.0368(19) 0.0037(15) -0.0030(15) -0.0043(14) C13 0.047(3) 0.047(2) 0.042(2) 0.0123(18) 0.0064(19) -0.0051(18) C14 0.046(2) 0.044(2) 0.059(3) 0.0068(19) 0.006(2) -0.0122(18) C15 0.033(2) 0.040(2) 0.052(2) -0.0077(17) 0.0035(18) -0.0092(16) C16 0.0304(18) 0.0354(19) 0.0300(17) -0.0043(13) -0.0013(14) -0.0020(14) C17 0.0332(18) 0.0260(16) 0.0256(15) -0.0003(12) -0.0034(14) -0.0029(13) C18 0.046(2) 0.0290(18) 0.053(2) -0.0013(16) 0.0133(19) 0.0020(15) C19 0.065(3) 0.029(2) 0.061(3) 0.0004(18) 0.016(2) 0.0024(18) C20 0.080(3) 0.032(2) 0.042(2) 0.0040(17) 0.005(2) -0.012(2) C21 0.052(2) 0.044(2) 0.0397(19) 0.0018(17) 0.0070(19) -0.0164(18) C22 0.039(2) 0.036(2) 0.0299(18) -0.0011(14) 0.0024(15) -0.0040(15) C23 0.0267(16) 0.0251(16) 0.0305(16) 0.0005(12) -0.0019(13) -0.0009(12) C24 0.0330(19) 0.041(2) 0.0338(18) -0.0049(14) -0.0009(15) 0.0050(14) C25 0.041(2) 0.051(2) 0.044(2) -0.0047(18) -0.0114(18) 0.0022(18) C26 0.0304(19) 0.045(2) 0.054(2) 0.0093(17) -0.0136(18) 0.0009(16) C27 0.031(2) 0.039(2) 0.045(2) 0.0040(15) 0.0045(16) 0.0094(15) C28 0.0311(17) 0.0327(16) 0.0305(16) 0.0003(13) 0.0008(15) 0.0034(13) C29 0.0282(16) 0.0273(15) 0.0319(17) 0.0053(12) -0.0056(14) -0.0018(12) C30 0.035(2) 0.038(2) 0.0348(18) 0.0044(15) 0.0005(15) 0.0079(15) C31 0.057(3) 0.051(2) 0.032(2) 0.0056(16) -0.0053(19) 0.008(2) C32 0.048(3) 0.056(3) 0.044(2) 0.0132(19) -0.014(2) 0.009(2) C33 0.039(2) 0.043(2) 0.054(2) 0.0061(18) -0.0093(19) 0.0160(17) C34 0.0368(19) 0.0338(18) 0.0344(18) 0.0017(15) -0.0008(16) 0.0055(14) C35 0.0244(16) 0.0263(15) 0.0361(19) 0.0010(12) -0.0050(13) 0.0012(11) C36 0.0314(18) 0.0327(18) 0.040(2) 0.0005(14) -0.0033(15) 0.0041(14) C37 0.032(2) 0.038(2) 0.061(3) 0.0080(18) 0.0011(18) -0.0061(16) C38 0.036(2) 0.0348(19) 0.075(3) -0.004(2) -0.010(2) -0.0081(14) C39 0.038(2) 0.039(2) 0.054(2) -0.0125(18) -0.0154(19) 0.0020(17) C40 0.0322(19) 0.0329(19) 0.044(2) -0.0036(15) -0.0031(16) 0.0001(14) C41 0.0288(17) 0.0277(16) 0.0255(15) 0.0002(12) 0.0016(12) 0.0001(13) C42 0.058(3) 0.045(2) 0.0306(18) -0.0039(16) -0.0038(18) 0.0230(19) C43 0.075(3) 0.057(3) 0.031(2) -0.0091(18) -0.007(2) 0.018(2) C44 0.054(3) 0.048(2) 0.0238(16) 0.0003(14) -0.0054(16) -0.0078(18) C45 0.034(2) 0.047(2) 0.0327(17) 0.0069(15) -0.0037(14) -0.0010(16) C46 0.0340(18) 0.0344(18) 0.0283(15) 0.0008(13) 0.0017(14) 0.0034(15) C47 0.0258(16) 0.0384(18) 0.0234(15) -0.0054(13) -0.0009(12) -0.0016(13) C48 0.0276(17) 0.045(2) 0.0385(19) -0.0085(17) 0.0030(15) -0.0005(15) C49 0.031(2) 0.064(3) 0.050(2) -0.014(2) 0.0062(18) 0.0004(17) C50 0.035(2) 0.076(3) 0.045(2) -0.021(2) 0.0065(18) -0.023(2) C51 0.053(2) 0.048(2) 0.036(2) -0.0058(17) 0.0030(19) -0.0212(19) C52 0.043(2) 0.0357(19) 0.0322(19) 0.0018(14) -0.0011(16) -0.0052(15) Fe2 0.0457(3) 0.0440(3) 0.0321(3) -0.0008(2) -0.0040(3) 0.0125(3) Cl4 0.0462(5) 0.0425(5) 0.0414(5) 0.0058(4) -0.0029(4) 0.0073(4) Cl3 0.0417(5) 0.0410(5) 0.0289(4) 0.0021(3) 0.0007(4) 0.0030(4) Cl2 0.0812(8) 0.0389(5) 0.0607(7) -0.0105(5) -0.0280(6) 0.0178(5) Cl1 0.0668(8) 0.0906(9) 0.0383(5) 0.0130(5) 0.0136(5) 0.0294(7) N5 0.157(5) 0.103(3) 0.071(3) -0.006(2) -0.041(3) 0.003(4) C53 0.160(5) 0.096(3) 0.064(3) -0.005(2) -0.037(3) 0.003(4) C54 0.164(5) 0.091(3) 0.061(3) -0.005(3) -0.032(3) 0.001(4) C1 0.076(3) 0.050(3) 0.034(2) -0.0047(17) -0.006(2) 0.013(2) C2 0.069(2) 0.0376(14) 0.0409(14) -0.0023(11) -0.0045(13) 0.0081(13) _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 N1 1.981(4) . ? Fe1 N2 1.999(3) . ? Fe1 P1 2.2444(10) . ? Fe1 P3 2.2572(10) . ? Fe1 P2 2.2591(10) . ? Fe1 P4 2.2650(10) . ? P1 N3 1.681(3) . ? P1 C11 1.816(3) . ? P1 C5 1.821(3) . ? P1 P2 2.6019(13) . ? P2 N3 1.689(3) . ? P2 C23 1.814(3) . ? P2 C17 1.825(3) . ? P3 N4 1.675(3) . ? P3 C29 1.811(3) . ? P3 C35 1.828(3) . ? P3 P4 2.6263(12) . ? P4 N4 1.682(3) . ? P4 C47 1.818(3) . ? P4 C41 1.826(3) . ? N1 C1 1.074(5) . ? N2 C3 1.070(5) . ? N3 H3A 0.8800 . ? N4 H4D 0.8800 . ? C3 C4 1.468(6) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.395(5) . ? C5 C10 1.404(5) . ? C6 C7 1.383(5) . ? C6 H6A 0.9500 . ? C7 C8 1.379(6) . ? C7 H7A 0.9500 . ? C8 C9 1.374(6) . ? C8 H8A 0.9500 . ? C9 C10 1.383(5) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.383(5) . ? C11 C16 1.401(5) . ? C12 C13 1.388(5) . ? C12 H12A 0.9500 . ? C13 C14 1.387(6) . ? C13 H13A 0.9500 . ? C14 C15 1.393(6) . ? C14 H14A 0.9500 . ? C15 C16 1.379(5) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C22 1.379(5) . ? C17 C18 1.392(5) . ? C18 C19 1.387(5) . ? C18 H18A 0.9500 . ? C19 C20 1.394(6) . ? C19 H19A 0.9500 . ? C20 C21 1.383(7) . ? C20 H20A 0.9500 . ? C21 C22 1.384(5) . ? C21 H21A 0.9500 . ? C22 H22A 0.9500 . ? C23 C28 1.375(5) . ? C23 C24 1.400(5) . ? C24 C25 1.397(5) . ? C24 H24A 0.9500 . ? C25 C26 1.381(6) . ? C25 H25A 0.9500 . ? C26 C27 1.362(6) . ? C26 H26A 0.9500 . ? C27 C28 1.387(5) . ? C27 H27A 0.9500 . ? C28 H28A 0.9500 . ? C29 C30 1.391(5) . ? C29 C34 1.391(5) . ? C30 C31 1.387(5) . ? C30 H30A 0.9500 . ? C31 C32 1.383(6) . ? C31 H31A 0.9500 . ? C32 C33 1.376(6) . ? C32 H32A 0.9500 . ? C33 C34 1.387(5) . ? C33 H33A 0.9500 . ? C34 H34A 0.9500 . ? C35 C36 1.392(5) . ? C35 C40 1.395(5) . ? C36 C37 1.385(5) . ? C36 H36A 0.9500 . ? C37 C38 1.375(6) . ? C37 H37A 0.9500 . ? C38 C39 1.387(6) . ? C38 H38A 0.9500 . ? C39 C40 1.375(5) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C46 1.382(5) . ? C41 C42 1.395(5) . ? C42 C43 1.370(5) . ? C42 H42A 0.9500 . ? C43 C44 1.386(6) . ? C43 H43A 0.9500 . ? C44 C45 1.370(6) . ? C44 H44A 0.9500 . ? C45 C46 1.390(5) . ? C45 H45A 0.9500 . ? C46 H46A 0.9500 . ? C47 C52 1.388(5) . ? C47 C48 1.395(5) . ? C48 C49 1.381(5) . ? C48 H48A 0.9500 . ? C49 C50 1.367(6) . ? C49 H49A 0.9500 . ? C50 C51 1.387(6) . ? C50 H50A 0.9500 . ? C51 C52 1.379(5) . ? C51 H51A 0.9500 . ? C52 H52A 0.9500 . ? Fe2 Cl2 2.2865(12) . ? Fe2 Cl1 2.3005(14) . ? Fe2 Cl4 2.3059(12) . ? Fe2 Cl3 2.3603(11) . ? N5 C53 1.143(11) . ? C53 C54 1.442(12) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C1 C2 1.504(6) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 N2 88.86(14) . . ? N1 Fe1 P1 94.23(11) . . ? N2 Fe1 P1 95.24(8) . . ? N1 Fe1 P3 164.21(11) . . ? N2 Fe1 P3 87.57(8) . . ? P1 Fe1 P3 101.41(4) . . ? N1 Fe1 P2 89.90(11) . . ? N2 Fe1 P2 165.64(8) . . ? P1 Fe1 P2 70.58(3) . . ? P3 Fe1 P2 97.29(4) . . ? N1 Fe1 P4 93.58(11) . . ? N2 Fe1 P4 89.23(8) . . ? P1 Fe1 P4 171.08(4) . . ? P3 Fe1 P4 71.01(3) . . ? P2 Fe1 P4 105.13(4) . . ? N3 P1 C11 108.26(14) . . ? N3 P1 C5 108.50(15) . . ? C11 P1 C5 101.50(15) . . ? N3 P1 Fe1 94.11(10) . . ? C11 P1 Fe1 124.23(11) . . ? C5 P1 Fe1 119.03(12) . . ? C11 P1 P2 132.72(11) . . ? C5 P1 P2 119.61(11) . . ? Fe1 P1 P2 54.97(3) . . ? N3 P2 C23 108.55(14) . . ? N3 P2 C17 106.66(15) . . ? C23 P2 C17 100.14(16) . . ? N3 P2 Fe1 93.35(9) . . ? C23 P2 Fe1 129.36(11) . . ? C17 P2 Fe1 116.81(11) . . ? C23 P2 P1 135.83(11) . . ? C17 P2 P1 116.22(12) . . ? Fe1 P2 P1 54.45(3) . . ? N4 P3 C29 107.14(15) . . ? N4 P3 C35 105.11(15) . . ? C29 P3 C35 100.43(15) . . ? N4 P3 Fe1 93.23(10) . . ? C29 P3 Fe1 127.43(11) . . ? C35 P3 Fe1 120.58(11) . . ? C29 P3 P4 127.29(12) . . ? C35 P3 P4 123.16(11) . . ? Fe1 P3 P4 54.63(3) . . ? N4 P4 C47 107.61(16) . . ? N4 P4 C41 107.91(15) . . ? C47 P4 C41 100.52(15) . . ? N4 P4 Fe1 92.78(10) . . ? C47 P4 Fe1 124.84(11) . . ? C41 P4 Fe1 121.41(11) . . ? C47 P4 P3 125.91(11) . . ? C41 P4 P3 126.15(11) . . ? Fe1 P4 P3 54.36(3) . . ? C1 N1 Fe1 175.2(5) . . ? C3 N2 Fe1 169.1(3) . . ? P1 N3 P2 101.07(14) . . ? P1 N3 H3A 129.5 . . ? P2 N3 H3A 129.5 . . ? P3 N4 P4 102.94(15) . . ? P3 N4 H4D 128.5 . . ? P4 N4 H4D 128.5 . . ? N2 C3 C4 178.4(4) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 C10 119.5(3) . . ? C6 C5 P1 119.4(3) . . ? C10 C5 P1 121.0(3) . . ? C7 C6 C5 120.1(4) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C8 C7 C6 120.2(4) . . ? C8 C7 H7A 119.9 . . ? C6 C7 H7A 119.9 . . ? C9 C8 C7 120.0(4) . . ? C9 C8 H8A 120.0 . . ? C7 C8 H8A 120.0 . . ? C8 C9 C10 121.1(4) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C5 119.0(4) . . ? C9 C10 H10A 120.5 . . ? C5 C10 H10A 120.5 . . ? C12 C11 C16 120.0(3) . . ? C12 C11 P1 122.9(3) . . ? C16 C11 P1 117.1(3) . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? C14 C13 C12 119.7(4) . . ? C14 C13 H13A 120.1 . . ? C12 C13 H13A 120.1 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 119.6(4) . . ? C16 C15 H15A 120.2 . . ? C14 C15 H15A 120.2 . . ? C15 C16 C11 120.0(3) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C22 C17 C18 118.9(3) . . ? C22 C17 P2 120.1(3) . . ? C18 C17 P2 120.8(3) . . ? C19 C18 C17 120.6(4) . . ? C19 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? C18 C19 C20 119.5(4) . . ? C18 C19 H19A 120.3 . . ? C20 C19 H19A 120.3 . . ? C21 C20 C19 120.3(4) . . ? C21 C20 H20A 119.9 . . ? C19 C20 H20A 119.9 . . ? C20 C21 C22 119.3(4) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C17 C22 C21 121.4(4) . . ? C17 C22 H22A 119.3 . . ? C21 C22 H22A 119.3 . . ? C28 C23 C24 119.4(3) . . ? C28 C23 P2 120.2(3) . . ? C24 C23 P2 120.1(3) . . ? C25 C24 C23 119.2(3) . . ? C25 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? C26 C25 C24 120.2(4) . . ? C26 C25 H25A 119.9 . . ? C24 C25 H25A 119.9 . . ? C27 C26 C25 120.1(4) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C26 C27 C28 120.5(4) . . ? C26 C27 H27A 119.8 . . ? C28 C27 H27A 119.8 . . ? C23 C28 C27 120.5(3) . . ? C23 C28 H28A 119.7 . . ? C27 C28 H28A 119.7 . . ? C30 C29 C34 119.2(3) . . ? C30 C29 P3 121.2(3) . . ? C34 C29 P3 119.6(3) . . ? C31 C30 C29 120.5(4) . . ? C31 C30 H30A 119.7 . . ? C29 C30 H30A 119.7 . . ? C32 C31 C30 119.6(4) . . ? C32 C31 H31A 120.2 . . ? C30 C31 H31A 120.2 . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H32A 119.9 . . ? C31 C32 H32A 119.9 . . ? C32 C33 C34 120.4(4) . . ? C32 C33 H33A 119.8 . . ? C34 C33 H33A 119.8 . . ? C33 C34 C29 119.9(4) . . ? C33 C34 H34A 120.0 . . ? C29 C34 H34A 120.0 . . ? C36 C35 C40 118.9(3) . . ? C36 C35 P3 120.5(3) . . ? C40 C35 P3 120.6(3) . . ? C37 C36 C35 119.8(4) . . ? C37 C36 H36A 120.1 . . ? C35 C36 H36A 120.1 . . ? C38 C37 C36 120.7(4) . . ? C38 C37 H37A 119.6 . . ? C36 C37 H37A 119.6 . . ? C37 C38 C39 119.9(4) . . ? C37 C38 H38A 120.0 . . ? C39 C38 H38A 120.0 . . ? C40 C39 C38 119.7(4) . . ? C40 C39 H39A 120.1 . . ? C38 C39 H39A 120.1 . . ? C39 C40 C35 120.9(4) . . ? C39 C40 H40A 119.6 . . ? C35 C40 H40A 119.6 . . ? C46 C41 C42 119.2(3) . . ? C46 C41 P4 121.3(3) . . ? C42 C41 P4 119.4(3) . . ? C43 C42 C41 120.0(4) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 120.9(4) . . ? C42 C43 H43A 119.5 . . ? C44 C43 H43A 119.5 . . ? C45 C44 C43 119.2(3) . . ? C45 C44 H44A 120.4 . . ? C43 C44 H44A 120.4 . . ? C44 C45 C46 120.7(4) . . ? C44 C45 H45A 119.7 . . ? C46 C45 H45A 119.7 . . ? C41 C46 C45 120.0(3) . . ? C41 C46 H46A 120.0 . . ? C45 C46 H46A 120.0 . . ? C52 C47 C48 119.4(3) . . ? C52 C47 P4 119.2(3) . . ? C48 C47 P4 121.4(3) . . ? C49 C48 C47 119.4(4) . . ? C49 C48 H48A 120.3 . . ? C47 C48 H48A 120.3 . . ? C50 C49 C48 121.0(4) . . ? C50 C49 H49A 119.5 . . ? C48 C49 H49A 119.5 . . ? C49 C50 C51 120.0(4) . . ? C49 C50 H50A 120.0 . . ? C51 C50 H50A 120.0 . . ? C52 C51 C50 119.7(4) . . ? C52 C51 H51A 120.1 . . ? C50 C51 H51A 120.1 . . ? C51 C52 C47 120.4(4) . . ? C51 C52 H52A 119.8 . . ? C47 C52 H52A 119.8 . . ? Cl2 Fe2 Cl1 106.67(5) . . ? Cl2 Fe2 Cl4 115.51(5) . . ? Cl1 Fe2 Cl4 110.79(5) . . ? Cl2 Fe2 Cl3 111.61(4) . . ? Cl1 Fe2 Cl3 108.86(5) . . ? Cl4 Fe2 Cl3 103.32(4) . . ? N5 C53 C54 173.5(8) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N1 C1 C2 177.8(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.192 _refine_diff_density_min -1.314 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 923304' ####################################################################### # # 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_compound3 #TrackingRef '17447_web_deposit_cif_file_2_RobertLanger_1359917457.Compound3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H48 Fe N4 P4, 2(B F4), C2 H3 N' _chemical_formula_sum 'C54 H51 B2 F8 Fe N5 P4' _chemical_formula_weight 1123.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.829(2) _cell_length_b 12.626(3) _cell_length_c 19.276(4) _cell_angle_alpha 85.36(3) _cell_angle_beta 83.54(3) _cell_angle_gamma 68.09(3) _cell_volume 2651.6(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 142 _cell_measurement_theta_min 7.09 _cell_measurement_theta_max 54.29 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.407 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_absorpt_coefficient_mu 0.476 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8606 _exptl_absorpt_correction_T_max 0.9119 _exptl_absorpt_process_details 'Stoe, X-Area Ver. 1.56' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type IPDS2T _diffrn_measurement_method Omega-Scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25461 _diffrn_reflns_av_R_equivalents 0.0382 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.74 _reflns_number_total 11169 _reflns_number_gt 9447 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area 1.56 (Stoe 2011)' _computing_cell_refinement 'X-Area 1.56 (Stoe 2011)' _computing_data_reduction 'X-Area 1.56 (Stoe 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2g (Brandenburg 2011)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0518P)^2^+0.4028P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11169 _refine_ls_number_parameters 699 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0870 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.0000 1.0000 0.0000 0.01286(8) Uani 1 2 d S . . P1 P 0.07993(4) 1.10090(3) 0.05780(2) 0.01429(9) Uani 1 1 d . . . C1 C 0.22485(15) 0.78144(15) 0.00633(9) 0.0210(3) Uani 1 1 d . . . B1 B 0.6375(2) 0.7079(2) 0.00335(13) 0.0347(5) Uani 1 1 d . . . N1 N -0.15871(12) 0.87184(12) 0.01499(7) 0.0164(3) Uani 1 1 d . . . H1N H -0.202(2) 0.8326(19) 0.0197(11) 0.027(5) Uiso 1 1 d . . . F1 F 0.7053(2) 0.7276(3) -0.05752(14) 0.0975(10) Uani 0.75 1 d P A 1 F1A F 0.6644(10) 0.6476(8) -0.0555(4) 0.086(3) Uani 0.25 1 d P A 2 Fe2 Fe 0.5000 0.5000 0.5000 0.01324(8) Uani 1 2 d S . . P2 P -0.10328(3) 0.91849(3) 0.07810(2) 0.01423(9) Uani 1 1 d . . . C2 C 0.32283(18) 0.66989(17) 0.00785(13) 0.0390(5) Uani 1 1 d . . . H2A H 0.3002 0.6200 0.0437 0.058 Uiso 1 1 calc R . . H2B H 0.3980 0.6781 0.0188 0.058 Uiso 1 1 calc R . . H2C H 0.3364 0.6363 -0.0379 0.058 Uiso 1 1 calc R . . B2 B 0.69922(19) 0.88265(18) 0.59110(11) 0.0250(4) Uani 1 1 d . . . F2 F 0.6266(3) 0.6065(2) 0.0079(3) 0.0965(14) Uani 0.75 1 d P A 1 F2A F 0.5818(6) 0.6472(8) 0.0546(5) 0.074(3) Uani 0.25 1 d P A 2 N2 N 0.14458(12) 0.86735(11) 0.00529(7) 0.0159(3) Uani 1 1 d . . . P3 P 0.47055(4) 0.61728(3) 0.58908(2) 0.01462(9) Uani 1 1 d . . . C3 C 0.18869(15) 1.03684(14) 0.12229(8) 0.0174(3) Uani 1 1 d . . . F3 F 0.52979(13) 0.79754(13) 0.00293(8) 0.0586(4) Uani 1 1 d . A . N3 N 0.58369(12) 0.66128(12) 0.55440(7) 0.0167(3) Uani 1 1 d . . . H3N H 0.609(2) 0.706(2) 0.5705(12) 0.035(6) Uiso 1 1 d . . . P4 P 0.65316(3) 0.56754(3) 0.49127(2) 0.01459(9) Uani 1 1 d . . . C4 C 0.30534(15) 0.95907(15) 0.10250(9) 0.0223(3) Uani 1 1 d . . . H4A H 0.3299 0.9443 0.0545 0.027 Uiso 1 1 calc R . . F4 F 0.71028(15) 0.71535(13) 0.05177(10) 0.0719(5) Uani 1 1 d . A . N4 N 0.40260(12) 0.63186(12) 0.45022(7) 0.0162(3) Uani 1 1 d . . . C5 C 0.38562(17) 0.90320(17) 0.15231(10) 0.0288(4) Uani 1 1 d . . . H5A H 0.4650 0.8505 0.1384 0.035 Uiso 1 1 calc R . . F5 F 0.62078(14) 0.99380(12) 0.59458(10) 0.0636(4) Uani 1 1 d . . . N5 N -0.01231(17) -0.63944(15) 0.28453(10) 0.0387(4) Uani 1 1 d . . . C6 C 0.35012(18) 0.92416(17) 0.22252(10) 0.0303(4) Uani 1 1 d . . . H6A H 0.4052 0.8857 0.2567 0.036 Uiso 1 1 calc R . . F6 F 0.65435(14) 0.81365(12) 0.63699(7) 0.0519(4) Uani 1 1 d . . . C7 C 0.23458(19) 1.00104(16) 0.24280(10) 0.0287(4) Uani 1 1 d . . . H7A H 0.2105 1.0153 0.2909 0.034 Uiso 1 1 calc R . . F7 F 0.81139(11) 0.87604(12) 0.60857(7) 0.0473(3) Uani 1 1 d . . . C8 C 0.15384(17) 1.05728(15) 0.19324(9) 0.0230(4) Uani 1 1 d . . . H8A H 0.0746 1.1099 0.2075 0.028 Uiso 1 1 calc R . . F8 F 0.71225(12) 0.84171(11) 0.52510(6) 0.0410(3) Uani 1 1 d . . . C9 C -0.02276(14) 1.23650(13) 0.09131(8) 0.0158(3) Uani 1 1 d . . . C10 C -0.01148(16) 1.33821(14) 0.06414(9) 0.0217(3) Uani 1 1 d . . . H10A H 0.0556 1.3364 0.0315 0.026 Uiso 1 1 calc R . . C11 C -0.09861(17) 1.44220(15) 0.08494(10) 0.0253(4) Uani 1 1 d . . . H11A H -0.0918 1.5114 0.0656 0.030 Uiso 1 1 calc R . . C12 C -0.19513(16) 1.44588(15) 0.13355(9) 0.0244(4) Uani 1 1 d . . . H12A H -0.2542 1.5174 0.1476 0.029 Uiso 1 1 calc R . . C13 C -0.20571(15) 1.34542(15) 0.16176(9) 0.0231(4) Uani 1 1 d . . . H13A H -0.2710 1.3480 0.1959 0.028 Uiso 1 1 calc R . . C14 C -0.12109(15) 1.24094(15) 0.14026(9) 0.0200(3) Uani 1 1 d . . . H14A H -0.1299 1.1721 0.1588 0.024 Uiso 1 1 calc R . . C15 C -0.01423(14) 0.79720(14) 0.13096(8) 0.0166(3) Uani 1 1 d . . . C16 C 0.07766(16) 0.80627(15) 0.16704(9) 0.0233(4) Uani 1 1 d . . . H16A H 0.0921 0.8757 0.1637 0.028 Uiso 1 1 calc R . . C17 C 0.14767(17) 0.71483(16) 0.20748(10) 0.0276(4) Uani 1 1 d . . . H17A H 0.2092 0.7219 0.2324 0.033 Uiso 1 1 calc R . . C18 C 0.12806(17) 0.61320(16) 0.21163(10) 0.0283(4) Uani 1 1 d . . . H18A H 0.1761 0.5503 0.2394 0.034 Uiso 1 1 calc R . . C19 C 0.03815(17) 0.60303(16) 0.17528(10) 0.0280(4) Uani 1 1 d . . . H19A H 0.0255 0.5328 0.1778 0.034 Uiso 1 1 calc R . . C20 C -0.03328(15) 0.69469(15) 0.13535(9) 0.0227(4) Uani 1 1 d . . . H20A H -0.0953 0.6874 0.1110 0.027 Uiso 1 1 calc R . . C21 C -0.23666(14) 0.99110(13) 0.13656(8) 0.0174(3) Uani 1 1 d . . . C22 C -0.22462(16) 1.00311(15) 0.20650(9) 0.0219(3) Uani 1 1 d . . . H22A H -0.1459 0.9754 0.2234 0.026 Uiso 1 1 calc R . . C23 C -0.32794(17) 1.05563(15) 0.25118(9) 0.0259(4) Uani 1 1 d . . . H23A H -0.3199 1.0647 0.2986 0.031 Uiso 1 1 calc R . . C24 C -0.44308(17) 1.09489(16) 0.22657(10) 0.0274(4) Uani 1 1 d . . . H24A H -0.5138 1.1277 0.2578 0.033 Uiso 1 1 calc R . . C25 C -0.45536(16) 1.08658(16) 0.15725(10) 0.0289(4) Uani 1 1 d . . . H25A H -0.5342 1.1160 0.1404 0.035 Uiso 1 1 calc R . . C26 C -0.35231(15) 1.03507(15) 0.11191(9) 0.0241(4) Uani 1 1 d . . . H26A H -0.3608 1.0298 0.0640 0.029 Uiso 1 1 calc R . . C27 C 0.33579(15) 0.71287(15) 0.42533(9) 0.0200(3) Uani 1 1 d . . . C28 C 0.24856(19) 0.81595(17) 0.39465(11) 0.0338(4) Uani 1 1 d . . . H28A H 0.1669 0.8307 0.4186 0.051 Uiso 1 1 calc R . . H28B H 0.2471 0.8057 0.3449 0.051 Uiso 1 1 calc R . . H28C H 0.2730 0.8808 0.3998 0.051 Uiso 1 1 calc R . . C29 C 0.33675(14) 0.74720(14) 0.60121(8) 0.0174(3) Uani 1 1 d . . . C30 C 0.33027(16) 0.84944(15) 0.56492(9) 0.0229(4) Uani 1 1 d . . . H30A H 0.3992 0.8532 0.5359 0.027 Uiso 1 1 calc R . . C31 C 0.22343(18) 0.94568(16) 0.57113(10) 0.0297(4) Uani 1 1 d . . . H31A H 0.2196 1.0151 0.5466 0.036 Uiso 1 1 calc R . . C32 C 0.12227(17) 0.94025(17) 0.61317(10) 0.0320(4) Uani 1 1 d . . . H32A H 0.0491 1.0060 0.6171 0.038 Uiso 1 1 calc R . . C33 C 0.12752(16) 0.83926(17) 0.64947(10) 0.0278(4) Uani 1 1 d . . . H33A H 0.0578 0.8358 0.6778 0.033 Uiso 1 1 calc R . . C34 C 0.23453(15) 0.74339(15) 0.64437(9) 0.0209(3) Uani 1 1 d . . . H34A H 0.2386 0.6749 0.6702 0.025 Uiso 1 1 calc R . . C35 C 0.49876(14) 0.56232(14) 0.67809(8) 0.0175(3) Uani 1 1 d . . . C36 C 0.48087(15) 0.46250(14) 0.70266(9) 0.0201(3) Uani 1 1 d . . . H36A H 0.4592 0.4196 0.6718 0.024 Uiso 1 1 calc R . . C37 C 0.49466(16) 0.42528(15) 0.77225(9) 0.0245(4) Uani 1 1 d . . . H37A H 0.4824 0.3571 0.7889 0.029 Uiso 1 1 calc R . . C38 C 0.52624(16) 0.48770(17) 0.81721(9) 0.0274(4) Uani 1 1 d . . . H38A H 0.5351 0.4625 0.8648 0.033 Uiso 1 1 calc R . . C39 C 0.54498(16) 0.58668(17) 0.79317(9) 0.0266(4) Uani 1 1 d . . . H39A H 0.5672 0.6290 0.8242 0.032 Uiso 1 1 calc R . . C40 C 0.53142(15) 0.62421(16) 0.72385(9) 0.0229(4) Uani 1 1 d . . . H40A H 0.5444 0.6922 0.7075 0.027 Uiso 1 1 calc R . . C41 C 0.67920(14) 0.64646(14) 0.41272(8) 0.0169(3) Uani 1 1 d . . . C42 C 0.75840(15) 0.58691(15) 0.35745(9) 0.0215(3) Uani 1 1 d . . . H42A H 0.8052 0.5077 0.3637 0.026 Uiso 1 1 calc R . . C43 C 0.76890(17) 0.64285(17) 0.29371(9) 0.0268(4) Uani 1 1 d . . . H43A H 0.8225 0.6019 0.2563 0.032 Uiso 1 1 calc R . . C44 C 0.70152(17) 0.75829(17) 0.28429(10) 0.0289(4) Uani 1 1 d . . . H44A H 0.7090 0.7965 0.2405 0.035 Uiso 1 1 calc R . . C45 C 0.62310(17) 0.81823(17) 0.33875(10) 0.0268(4) Uani 1 1 d . . . H45A H 0.5772 0.8975 0.3322 0.032 Uiso 1 1 calc R . . C46 C 0.61133(15) 0.76282(15) 0.40300(9) 0.0207(3) Uani 1 1 d . . . H46A H 0.5572 0.8041 0.4401 0.025 Uiso 1 1 calc R . . C47 C 0.80180(14) 0.47735(14) 0.51838(8) 0.0171(3) Uani 1 1 d . . . C48 C 0.86854(15) 0.37518(15) 0.48587(9) 0.0226(4) Uani 1 1 d . . . H48A H 0.8364 0.3539 0.4486 0.027 Uiso 1 1 calc R . . C49 C 0.98101(15) 0.30430(15) 0.50718(10) 0.0250(4) Uani 1 1 d . . . H49A H 1.0266 0.2358 0.4838 0.030 Uiso 1 1 calc R . . C50 C 1.02685(15) 0.33355(16) 0.56261(10) 0.0267(4) Uani 1 1 d . . . H50A H 1.1035 0.2846 0.5779 0.032 Uiso 1 1 calc R . . C51 C 0.96061(16) 0.43446(18) 0.59571(10) 0.0294(4) Uani 1 1 d . . . H51A H 0.9922 0.4543 0.6338 0.035 Uiso 1 1 calc R . . C52 C 0.84866(16) 0.50685(16) 0.57387(9) 0.0238(4) Uani 1 1 d . . . H52A H 0.8042 0.5762 0.5966 0.029 Uiso 1 1 calc R . . C53 C 0.08411(18) -0.66865(16) 0.25795(11) 0.0289(4) Uani 1 1 d . . . C54 C 0.20752(18) -0.70405(18) 0.22297(14) 0.0401(5) Uani 1 1 d . . . H54A H 0.2043 -0.7107 0.1730 0.060 Uiso 1 1 calc R . . H54B H 0.2582 -0.7782 0.2431 0.060 Uiso 1 1 calc R . . H54C H 0.2431 -0.6471 0.2293 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.01464(14) 0.01100(15) 0.01346(15) -0.00142(11) -0.00040(11) -0.00535(12) P1 0.01670(18) 0.0128(2) 0.01456(19) -0.00217(15) -0.00077(15) -0.00667(15) C1 0.0198(8) 0.0204(9) 0.0246(9) -0.0025(7) -0.0047(7) -0.0084(7) B1 0.0247(10) 0.0354(13) 0.0438(13) -0.0004(10) -0.0057(9) -0.0104(9) N1 0.0182(6) 0.0173(7) 0.0170(7) -0.0022(5) 0.0001(5) -0.0105(6) F1 0.0437(12) 0.171(3) 0.0629(16) -0.0038(18) 0.0149(11) -0.0280(16) F1A 0.138(8) 0.070(5) 0.049(4) -0.036(4) -0.014(5) -0.028(5) Fe2 0.01351(14) 0.01205(16) 0.01465(15) -0.00138(12) 0.00025(11) -0.00550(12) P2 0.01625(18) 0.0130(2) 0.01421(19) -0.00120(15) -0.00012(15) -0.00653(15) C2 0.0306(10) 0.0235(10) 0.0557(14) -0.0082(9) -0.0182(9) 0.0037(8) B2 0.0286(10) 0.0210(10) 0.0282(10) -0.0055(8) 0.0035(8) -0.0132(8) F2 0.072(2) 0.0275(12) 0.205(4) -0.0054(18) -0.077(2) -0.0170(12) F2A 0.046(4) 0.092(6) 0.102(6) 0.072(5) -0.034(4) -0.055(4) N2 0.0178(6) 0.0160(7) 0.0167(7) -0.0018(5) -0.0017(5) -0.0091(6) P3 0.01566(18) 0.0134(2) 0.01510(19) -0.00186(15) 0.00064(15) -0.00602(15) C3 0.0229(8) 0.0147(8) 0.0185(8) 0.0003(6) -0.0054(6) -0.0107(6) F3 0.0458(8) 0.0480(9) 0.0651(10) -0.0034(7) -0.0158(7) 0.0057(6) N3 0.0185(6) 0.0168(7) 0.0176(7) -0.0044(5) 0.0014(5) -0.0098(6) P4 0.01461(18) 0.0144(2) 0.01579(19) -0.00200(15) 0.00089(14) -0.00690(15) C4 0.0208(8) 0.0239(9) 0.0245(9) 0.0003(7) -0.0033(7) -0.0108(7) F4 0.0737(10) 0.0444(9) 0.1194(15) 0.0310(9) -0.0637(11) -0.0380(8) N4 0.0169(6) 0.0168(7) 0.0171(7) -0.0035(5) 0.0013(5) -0.0088(6) C5 0.0239(9) 0.0294(10) 0.0341(10) 0.0047(8) -0.0074(7) -0.0107(8) F5 0.0510(8) 0.0253(7) 0.1058(13) -0.0154(8) -0.0078(8) -0.0012(6) N5 0.0382(10) 0.0314(10) 0.0436(10) -0.0015(8) 0.0004(8) -0.0107(8) C6 0.0349(10) 0.0299(10) 0.0313(10) 0.0086(8) -0.0168(8) -0.0158(8) F6 0.0843(10) 0.0545(9) 0.0344(7) -0.0118(6) 0.0215(7) -0.0512(8) C7 0.0447(11) 0.0242(9) 0.0212(9) 0.0010(7) -0.0101(8) -0.0156(8) F7 0.0330(6) 0.0645(9) 0.0505(8) -0.0288(7) -0.0006(5) -0.0205(6) C8 0.0314(9) 0.0181(8) 0.0204(8) -0.0022(7) -0.0038(7) -0.0096(7) F8 0.0558(8) 0.0517(8) 0.0269(6) -0.0068(5) -0.0037(5) -0.0320(6) C9 0.0180(7) 0.0154(8) 0.0154(7) -0.0036(6) -0.0028(6) -0.0067(6) C10 0.0259(8) 0.0176(8) 0.0235(9) -0.0034(7) 0.0009(7) -0.0104(7) C11 0.0326(9) 0.0156(8) 0.0284(9) -0.0026(7) -0.0010(7) -0.0097(7) C12 0.0251(8) 0.0186(9) 0.0266(9) -0.0072(7) -0.0029(7) -0.0035(7) C13 0.0210(8) 0.0258(9) 0.0217(8) -0.0057(7) 0.0009(7) -0.0076(7) C14 0.0230(8) 0.0185(8) 0.0204(8) -0.0021(6) -0.0012(6) -0.0098(7) C15 0.0181(7) 0.0148(8) 0.0162(8) 0.0001(6) 0.0007(6) -0.0059(6) C16 0.0281(9) 0.0202(9) 0.0245(9) 0.0026(7) -0.0054(7) -0.0119(7) C17 0.0280(9) 0.0290(10) 0.0275(9) 0.0030(8) -0.0085(7) -0.0115(8) C18 0.0272(9) 0.0223(9) 0.0315(10) 0.0078(8) -0.0056(8) -0.0054(7) C19 0.0293(9) 0.0178(9) 0.0372(10) 0.0073(8) -0.0052(8) -0.0101(7) C20 0.0209(8) 0.0204(9) 0.0278(9) 0.0012(7) -0.0021(7) -0.0091(7) C21 0.0207(7) 0.0133(8) 0.0186(8) -0.0019(6) 0.0037(6) -0.0079(6) C22 0.0258(8) 0.0191(9) 0.0226(9) -0.0031(7) 0.0002(7) -0.0107(7) C23 0.0353(9) 0.0235(9) 0.0209(9) -0.0076(7) 0.0060(7) -0.0140(8) C24 0.0282(9) 0.0219(9) 0.0308(10) -0.0077(7) 0.0118(7) -0.0105(7) C25 0.0210(8) 0.0276(10) 0.0348(10) -0.0044(8) 0.0029(7) -0.0061(7) C26 0.0228(8) 0.0240(9) 0.0234(9) -0.0032(7) 0.0012(7) -0.0065(7) C27 0.0217(8) 0.0200(9) 0.0199(8) -0.0017(7) -0.0006(6) -0.0096(7) C28 0.0344(10) 0.0255(10) 0.0361(11) 0.0085(8) -0.0095(8) -0.0051(8) C29 0.0187(7) 0.0162(8) 0.0161(8) -0.0045(6) -0.0008(6) -0.0044(6) C30 0.0280(9) 0.0202(9) 0.0180(8) -0.0017(7) 0.0019(7) -0.0070(7) C31 0.0358(10) 0.0202(9) 0.0249(9) 0.0014(7) 0.0018(8) -0.0026(8) C32 0.0268(9) 0.0258(10) 0.0315(10) -0.0041(8) -0.0006(8) 0.0041(8) C33 0.0204(8) 0.0313(10) 0.0287(10) -0.0066(8) 0.0033(7) -0.0067(7) C34 0.0217(8) 0.0211(9) 0.0200(8) -0.0045(7) 0.0006(6) -0.0080(7) C35 0.0148(7) 0.0189(8) 0.0166(8) -0.0007(6) 0.0003(6) -0.0043(6) C36 0.0197(8) 0.0185(8) 0.0205(8) -0.0020(6) 0.0012(6) -0.0059(6) C37 0.0238(8) 0.0212(9) 0.0243(9) 0.0041(7) 0.0015(7) -0.0055(7) C38 0.0222(8) 0.0358(11) 0.0187(8) 0.0042(7) -0.0025(7) -0.0052(7) C39 0.0244(8) 0.0386(11) 0.0194(8) -0.0045(8) -0.0030(7) -0.0134(8) C40 0.0245(8) 0.0255(9) 0.0217(8) -0.0010(7) -0.0011(7) -0.0128(7) C41 0.0161(7) 0.0200(8) 0.0177(8) 0.0004(6) -0.0018(6) -0.0105(6) C42 0.0215(8) 0.0219(9) 0.0230(9) -0.0028(7) 0.0016(7) -0.0110(7) C43 0.0277(9) 0.0352(11) 0.0209(9) -0.0040(7) 0.0059(7) -0.0171(8) C44 0.0329(10) 0.0354(11) 0.0219(9) 0.0072(8) -0.0011(7) -0.0190(8) C45 0.0275(9) 0.0258(9) 0.0280(9) 0.0060(7) -0.0031(7) -0.0120(7) C46 0.0209(8) 0.0209(9) 0.0220(8) -0.0013(7) 0.0003(6) -0.0102(7) C47 0.0147(7) 0.0182(8) 0.0193(8) 0.0021(6) -0.0005(6) -0.0081(6) C48 0.0212(8) 0.0217(9) 0.0268(9) -0.0060(7) -0.0012(7) -0.0094(7) C49 0.0202(8) 0.0202(9) 0.0333(10) -0.0030(7) 0.0005(7) -0.0063(7) C50 0.0167(8) 0.0288(10) 0.0330(10) 0.0040(8) -0.0048(7) -0.0069(7) C51 0.0232(8) 0.0388(11) 0.0278(10) -0.0047(8) -0.0071(7) -0.0113(8) C52 0.0219(8) 0.0258(9) 0.0241(9) -0.0061(7) -0.0011(7) -0.0084(7) C53 0.0332(10) 0.0188(9) 0.0369(10) 0.0009(8) -0.0092(8) -0.0108(8) C54 0.0291(10) 0.0262(10) 0.0661(15) -0.0033(10) -0.0010(10) -0.0120(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N2 1.9012(16) . ? Fe1 N2 1.9012(16) 2_575 ? Fe1 P2 2.2565(8) . ? Fe1 P2 2.2565(8) 2_575 ? Fe1 P1 2.2635(7) 2_575 ? Fe1 P1 2.2635(7) . ? P1 N1 1.6801(15) 2_575 ? P1 C9 1.8096(17) . ? P1 C3 1.8097(18) . ? P1 P2 2.6248(8) 2_575 ? C1 N2 1.145(2) . ? C1 C2 1.453(3) . ? B1 F2 1.328(4) . ? B1 F3 1.353(3) . ? B1 F1A 1.358(6) . ? B1 F4 1.370(3) . ? B1 F1 1.404(3) . ? B1 F2A 1.451(6) . ? N1 P1 1.6800(15) 2_575 ? N1 P2 1.6853(14) . ? Fe2 N4 1.8917(16) 2_666 ? Fe2 N4 1.8917(16) . ? Fe2 P4 2.2580(6) 2_666 ? Fe2 P4 2.2580(6) . ? Fe2 P3 2.2703(8) 2_666 ? Fe2 P3 2.2703(8) . ? P2 C15 1.8105(18) . ? P2 C21 1.8132(17) . ? P2 P1 2.6247(8) 2_575 ? B2 F5 1.365(3) . ? B2 F7 1.376(2) . ? B2 F8 1.383(2) . ? B2 F6 1.392(2) . ? P3 N3 1.6851(15) . ? P3 C29 1.8144(18) . ? P3 C35 1.8166(18) . ? P3 P4 2.6227(11) . ? C3 C4 1.395(2) . ? C3 C8 1.399(2) . ? N3 P4 1.6851(15) . ? P4 C41 1.8055(17) . ? P4 C47 1.8104(18) . ? C4 C5 1.385(3) . ? N4 C27 1.142(2) . ? C5 C6 1.387(3) . ? N5 C53 1.133(3) . ? C6 C7 1.384(3) . ? C7 C8 1.385(3) . ? C9 C10 1.394(2) . ? C9 C14 1.400(2) . ? C10 C11 1.389(2) . ? C11 C12 1.382(3) . ? C12 C13 1.383(3) . ? C13 C14 1.387(2) . ? C15 C20 1.389(2) . ? C15 C16 1.398(2) . ? C16 C17 1.383(3) . ? C17 C18 1.381(3) . ? C18 C19 1.387(3) . ? C19 C20 1.385(3) . ? C21 C26 1.394(2) . ? C21 C22 1.398(2) . ? C22 C23 1.388(2) . ? C23 C24 1.389(3) . ? C24 C25 1.377(3) . ? C25 C26 1.390(2) . ? C27 C28 1.456(3) . ? C29 C30 1.398(2) . ? C29 C34 1.403(2) . ? C30 C31 1.390(3) . ? C31 C32 1.388(3) . ? C32 C33 1.388(3) . ? C33 C34 1.387(3) . ? C35 C36 1.392(2) . ? C35 C40 1.397(2) . ? C36 C37 1.392(2) . ? C37 C38 1.384(3) . ? C38 C39 1.384(3) . ? C39 C40 1.387(3) . ? C41 C46 1.395(2) . ? C41 C42 1.399(2) . ? C42 C43 1.384(3) . ? C43 C44 1.384(3) . ? C44 C45 1.386(3) . ? C45 C46 1.392(3) . ? C47 C48 1.393(2) . ? C47 C52 1.394(2) . ? C48 C49 1.384(3) . ? C49 C50 1.384(3) . ? C50 C51 1.385(3) . ? C51 C52 1.388(3) . ? C53 C54 1.458(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Fe1 N2 180.0 . 2_575 ? N2 Fe1 P2 90.57(5) . . ? N2 Fe1 P2 89.43(5) 2_575 . ? N2 Fe1 P2 89.43(5) . 2_575 ? N2 Fe1 P2 90.57(5) 2_575 2_575 ? P2 Fe1 P2 180.0 . 2_575 ? N2 Fe1 P1 88.72(5) . 2_575 ? N2 Fe1 P1 91.28(5) 2_575 2_575 ? P2 Fe1 P1 71.00(2) . 2_575 ? P2 Fe1 P1 109.00(2) 2_575 2_575 ? N2 Fe1 P1 91.28(5) . . ? N2 Fe1 P1 88.72(5) 2_575 . ? P2 Fe1 P1 109.00(2) . . ? P2 Fe1 P1 71.00(2) 2_575 . ? P1 Fe1 P1 180.0 2_575 . ? N1 P1 C9 107.76(8) 2_575 . ? N1 P1 C3 106.94(8) 2_575 . ? C9 P1 C3 105.99(8) . . ? N1 P1 Fe1 92.63(5) 2_575 . ? C9 P1 Fe1 117.89(5) . . ? C3 P1 Fe1 123.25(6) . . ? C9 P1 P2 117.02(6) . 2_575 ? C3 P1 P2 130.70(6) . 2_575 ? Fe1 P1 P2 54.37(2) . 2_575 ? N2 C1 C2 177.45(18) . . ? F2 B1 F3 114.1(2) . . ? F2 B1 F1A 61.9(5) . . ? F3 B1 F1A 112.5(4) . . ? F2 B1 F4 111.5(2) . . ? F3 B1 F4 113.1(2) . . ? F1A B1 F4 131.5(5) . . ? F2 B1 F1 114.4(3) . . ? F3 B1 F1 103.7(2) . . ? F1A B1 F1 54.6(5) . . ? F4 B1 F1 98.8(2) . . ? F3 B1 F2A 90.0(4) . . ? F1A B1 F2A 105.4(6) . . ? F4 B1 F2A 90.3(4) . . ? F1 B1 F2A 158.9(5) . . ? P1 N1 P2 102.51(8) 2_575 . ? N4 Fe2 N4 180.0 2_666 . ? N4 Fe2 P4 90.13(5) 2_666 2_666 ? N4 Fe2 P4 89.87(5) . 2_666 ? N4 Fe2 P4 89.87(5) 2_666 . ? N4 Fe2 P4 90.13(5) . . ? P4 Fe2 P4 180.000(2) 2_666 . ? N4 Fe2 P3 86.03(5) 2_666 2_666 ? N4 Fe2 P3 93.97(5) . 2_666 ? P4 Fe2 P3 70.78(3) 2_666 2_666 ? P4 Fe2 P3 109.22(3) . 2_666 ? N4 Fe2 P3 93.97(5) 2_666 . ? N4 Fe2 P3 86.03(5) . . ? P4 Fe2 P3 109.22(3) 2_666 . ? P4 Fe2 P3 70.78(3) . . ? P3 Fe2 P3 179.999(2) 2_666 . ? N1 P2 C15 109.17(8) . . ? N1 P2 C21 104.50(7) . . ? C15 P2 C21 103.51(8) . . ? N1 P2 Fe1 92.73(5) . . ? C15 P2 Fe1 117.46(6) . . ? C21 P2 Fe1 127.04(6) . . ? C15 P2 P1 118.01(6) . 2_575 ? C21 P2 P1 130.49(6) . 2_575 ? Fe1 P2 P1 54.63(2) . 2_575 ? F5 B2 F7 108.28(16) . . ? F5 B2 F8 112.01(19) . . ? F7 B2 F8 109.36(16) . . ? F5 B2 F6 109.92(17) . . ? F7 B2 F6 110.35(18) . . ? F8 B2 F6 106.93(15) . . ? C1 N2 Fe1 172.95(13) . . ? N3 P3 C29 105.10(8) . . ? N3 P3 C35 109.37(8) . . ? C29 P3 C35 102.85(8) . . ? N3 P3 Fe2 92.36(6) . . ? C29 P3 Fe2 122.87(6) . . ? C35 P3 Fe2 121.96(6) . . ? C29 P3 P4 130.13(6) . . ? C35 P3 P4 119.57(6) . . ? Fe2 P3 P4 54.39(2) . . ? C4 C3 C8 119.02(16) . . ? C4 C3 P1 120.25(13) . . ? C8 C3 P1 120.52(13) . . ? P3 N3 P4 102.19(8) . . ? N3 P4 C41 108.21(8) . . ? N3 P4 C47 107.17(8) . . ? C41 P4 C47 107.10(8) . . ? N3 P4 Fe2 92.79(6) . . ? C41 P4 Fe2 119.41(6) . . ? C47 P4 Fe2 119.95(6) . . ? C41 P4 P3 131.16(6) . . ? C47 P4 P3 116.24(6) . . ? Fe2 P4 P3 54.83(2) . . ? C5 C4 C3 120.48(17) . . ? C27 N4 Fe2 173.62(13) . . ? C4 C5 C6 120.01(18) . . ? C7 C6 C5 120.05(18) . . ? C6 C7 C8 120.25(17) . . ? C7 C8 C3 120.19(17) . . ? C10 C9 C14 119.24(15) . . ? C10 C9 P1 120.41(12) . . ? C14 C9 P1 120.10(13) . . ? C11 C10 C9 119.82(16) . . ? C12 C11 C10 120.59(17) . . ? C11 C12 C13 119.97(16) . . ? C12 C13 C14 120.10(16) . . ? C13 C14 C9 120.25(16) . . ? C20 C15 C16 119.23(16) . . ? C20 C15 P2 121.61(13) . . ? C16 C15 P2 119.14(13) . . ? C17 C16 C15 120.45(16) . . ? C18 C17 C16 119.96(17) . . ? C17 C18 C19 119.95(18) . . ? C20 C19 C18 120.39(17) . . ? C19 C20 C15 120.01(16) . . ? C26 C21 C22 119.51(15) . . ? C26 C21 P2 120.00(13) . . ? C22 C21 P2 120.49(13) . . ? C23 C22 C21 119.84(17) . . ? C22 C23 C24 120.01(17) . . ? C25 C24 C23 120.45(16) . . ? C24 C25 C26 119.94(18) . . ? C25 C26 C21 120.18(17) . . ? N4 C27 C28 178.80(19) . . ? C30 C29 C34 119.14(15) . . ? C30 C29 P3 121.37(12) . . ? C34 C29 P3 119.36(13) . . ? C31 C30 C29 120.31(16) . . ? C32 C31 C30 119.96(18) . . ? C33 C32 C31 120.29(17) . . ? C34 C33 C32 120.03(17) . . ? C33 C34 C29 120.24(17) . . ? C36 C35 C40 119.33(15) . . ? C36 C35 P3 120.67(13) . . ? C40 C35 P3 119.88(13) . . ? C35 C36 C37 120.24(16) . . ? C38 C37 C36 119.91(17) . . ? C37 C38 C39 120.28(17) . . ? C38 C39 C40 120.08(17) . . ? C39 C40 C35 120.16(17) . . ? C46 C41 C42 119.35(15) . . ? C46 C41 P4 121.21(12) . . ? C42 C41 P4 118.99(13) . . ? C43 C42 C41 120.27(17) . . ? C42 C43 C44 120.20(16) . . ? C43 C44 C45 120.03(17) . . ? C44 C45 C46 120.31(17) . . ? C45 C46 C41 119.83(16) . . ? C48 C47 C52 119.14(16) . . ? C48 C47 P4 120.33(13) . . ? C52 C47 P4 120.48(13) . . ? C49 C48 C47 120.86(16) . . ? C48 C49 C50 119.80(16) . . ? C49 C50 C51 119.75(17) . . ? C50 C51 C52 120.74(17) . . ? C51 C52 C47 119.69(17) . . ? N5 C53 C54 178.8(2) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.74 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.646 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.055 _database_code_depnum_ccdc_archive 'CCDC 923305' ####################################################################### # # 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_compound1EtOH _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H45 B Fe N2 P4, C2 H6 O' _chemical_formula_sum 'C50 H51 B Fe N2 O P4' _chemical_formula_weight 886.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.5776(19) _cell_length_b 21.887(4) _cell_length_c 11.260(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.34(3) _cell_angle_gamma 90.00 _cell_volume 2265.0(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18214 _cell_measurement_theta_min 1.86 _cell_measurement_theta_max 22.92 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9562 _exptl_absorpt_correction_T_max 0.9767 _exptl_absorpt_process_details 'STOE X-Red32 1.53' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 10 -3 0.0460 1 -7 2 0.0440 9 3 -1 0.0720 -1 0 0 0.0410 -2 -10 -3 0.0210 2 9 3 0.0390 -3 0 4 0.0460 5 2 -6 0.0760 -1 7 1 0.0320 3 -5 -2 0.0720 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 32 _diffrn_source_power 1.60 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 351 frames, detector distance = 120 mm ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29969 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.1500 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 26.37 _reflns_number_total 9174 _reflns_number_gt 6753 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0035P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(2) _refine_ls_number_reflns 9174 _refine_ls_number_parameters 552 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_gt 0.0842 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0865 _refine_ls_goodness_of_fit_ref 1.067 _refine_ls_restrained_S_all 1.067 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.51408(9) 0.66670(4) 0.10648(7) 0.0228(2) Uani 1 1 d . . . P1 P 0.72537(17) 0.54627(7) 0.20525(14) 0.0256(4) Uani 1 1 d . . . O1 O 0.2887(5) 0.91301(19) 0.0054(4) 0.0331(11) Uani 1 1 d . . . H1O1 H 0.320(6) 0.955(2) -0.008(5) 0.021(8) Uiso 1 1 d . . . N1 N 0.6458(5) 0.53262(19) 0.0622(4) 0.0242(11) Uani 1 1 d . . . B1 B 0.6649(8) 0.6251(3) 0.2538(7) 0.0252(16) Uani 1 1 d . . . H3B1 H 0.707(4) 0.668(2) 0.183(4) 0.015(11) Uiso 1 1 d . . . H2B1 H 0.712(5) 0.6380(19) 0.354(5) 0.013(13) Uiso 1 1 d . . . H1B1 H 0.541(6) 0.627(2) 0.214(5) 0.033(16) Uiso 1 1 d . . . C1 C 0.9211(6) 0.5392(3) 0.2294(6) 0.0325(15) Uani 1 1 d . . . C2 C 1.0148(7) 0.5366(3) 0.3487(7) 0.050(2) Uani 1 1 d . . . H2A H 0.9784 0.5384 0.4189 0.060 Uiso 1 1 calc R . . C3 C 1.1655(8) 0.5312(3) 0.3625(8) 0.061(3) Uani 1 1 d . . . H3A H 1.2319 0.5280 0.4427 0.073 Uiso 1 1 calc R . . C4 C 1.2163(9) 0.5308(3) 0.2593(9) 0.057(2) Uani 1 1 d . . . H4A H 1.3180 0.5289 0.2695 0.068 Uiso 1 1 calc R . . C5 C 1.1234(8) 0.5330(3) 0.1440(7) 0.0494(19) Uani 1 1 d . . . H5A H 1.1604 0.5311 0.0742 0.059 Uiso 1 1 calc R . . C6 C 0.9756(7) 0.5378(3) 0.1268(6) 0.0363(16) Uani 1 1 d . . . H6A H 0.9112 0.5402 0.0456 0.044 Uiso 1 1 calc R . . C7 C 0.6925(7) 0.4866(3) 0.3043(6) 0.0280(16) Uani 1 1 d . . . C8 C 0.6026(7) 0.4972(3) 0.3799(6) 0.0361(16) Uani 1 1 d . . . H8A H 0.5657 0.5372 0.3848 0.043 Uiso 1 1 calc R . . C9 C 0.5655(7) 0.4496(3) 0.4493(6) 0.0429(18) Uani 1 1 d . . . H9A H 0.5031 0.4574 0.5000 0.051 Uiso 1 1 calc R . . C10 C 0.6195(8) 0.3922(3) 0.4438(6) 0.044(2) Uani 1 1 d . . . H10A H 0.5925 0.3597 0.4888 0.053 Uiso 1 1 calc R . . C11 C 0.7147(8) 0.3813(3) 0.3716(6) 0.0413(19) Uani 1 1 d . . . H11A H 0.7560 0.3419 0.3703 0.050 Uiso 1 1 calc R . . C12 C 0.7477(7) 0.4281(2) 0.3026(6) 0.0341(16) Uani 1 1 d . . . H12A H 0.8103 0.4201 0.2523 0.041 Uiso 1 1 calc R . . C13 C 0.5899(7) 0.6014(2) -0.1499(5) 0.0228(13) Uani 1 1 d . . . C14 C 0.7262(7) 0.6275(3) -0.1291(6) 0.0334(16) Uani 1 1 d . . . H14A H 0.7823 0.6366 -0.0470 0.040 Uiso 1 1 calc R . . C15 C 0.7818(8) 0.6408(3) -0.2288(7) 0.0431(18) Uani 1 1 d . . . H15A H 0.8752 0.6589 -0.2144 0.052 Uiso 1 1 calc R . . C16 C 0.7008(9) 0.6275(3) -0.3472(7) 0.0456(19) Uani 1 1 d . . . H16A H 0.7390 0.6358 -0.4148 0.055 Uiso 1 1 calc R . . C17 C 0.5654(9) 0.6024(3) -0.3681(6) 0.047(2) Uani 1 1 d . . . H17A H 0.5092 0.5942 -0.4506 0.056 Uiso 1 1 calc R . . C18 C 0.5094(7) 0.5886(3) -0.2712(5) 0.0331(16) Uani 1 1 d . . . H18A H 0.4159 0.5705 -0.2870 0.040 Uiso 1 1 calc R . . C19 C 0.3592(6) 0.5442(3) -0.0804(5) 0.0280(14) Uani 1 1 d . . . C20 C 0.3510(7) 0.4812(2) -0.0627(5) 0.0261(15) Uani 1 1 d . . . H20A H 0.4326 0.4603 -0.0112 0.031 Uiso 1 1 calc R . . C21 C 0.2246(7) 0.4488(3) -0.1198(6) 0.0355(17) Uani 1 1 d . . . H21A H 0.2194 0.4060 -0.1071 0.043 Uiso 1 1 calc R . . C22 C 0.1061(7) 0.4802(3) -0.1957(6) 0.0419(18) Uani 1 1 d . . . H22A H 0.0204 0.4584 -0.2372 0.050 Uiso 1 1 calc R . . C23 C 0.1126(7) 0.5418(3) -0.2108(6) 0.0420(17) Uani 1 1 d . . . H23A H 0.0306 0.5625 -0.2624 0.050 Uiso 1 1 calc R . . C24 C 0.2373(7) 0.5750(3) -0.1520(5) 0.0328(16) Uani 1 1 d . . . H24A H 0.2389 0.6182 -0.1607 0.039 Uiso 1 1 calc R . . C25 C 0.3395(6) 0.7414(3) -0.1673(5) 0.0256(13) Uani 1 1 d . . . C26 C 0.3670(7) 0.7231(2) -0.2788(5) 0.0249(14) Uani 1 1 d . . . H26A H 0.4640 0.7166 -0.2820 0.030 Uiso 1 1 calc R . . C27 C 0.2500(7) 0.7148(2) -0.3845(6) 0.0321(16) Uani 1 1 d . . . H27A H 0.2686 0.7025 -0.4596 0.039 Uiso 1 1 calc R . . C28 C 0.1085(7) 0.7239(2) -0.3823(6) 0.0328(16) Uani 1 1 d . . . H28A H 0.0301 0.7168 -0.4543 0.039 Uiso 1 1 calc R . . C29 C 0.0820(7) 0.7438(3) -0.2733(5) 0.0351(15) Uani 1 1 d . . . H29A H -0.0152 0.7514 -0.2718 0.042 Uiso 1 1 calc R . . C30 C 0.1950(6) 0.7528(3) -0.1671(5) 0.0274(15) Uani 1 1 d . . . H30A H 0.1750 0.7667 -0.0937 0.033 Uiso 1 1 calc R . . C31 C 0.6309(6) 0.7834(2) -0.0608(5) 0.0214(13) Uani 1 1 d . . . C32 C 0.7758(7) 0.7678(2) 0.0023(5) 0.0274(15) Uani 1 1 d . . . H32A H 0.7951 0.7354 0.0608 0.033 Uiso 1 1 calc R . . C33 C 0.8912(7) 0.8003(3) -0.0218(6) 0.0317(15) Uani 1 1 d . . . H33A H 0.9889 0.7896 0.0198 0.038 Uiso 1 1 calc R . . C34 C 0.8625(7) 0.8481(3) -0.1064(5) 0.0319(16) Uani 1 1 d . . . H34A H 0.9408 0.8699 -0.1231 0.038 Uiso 1 1 calc R . . C35 C 0.7211(8) 0.8642(3) -0.1661(6) 0.0322(17) Uani 1 1 d . . . H35A H 0.7025 0.8974 -0.2228 0.039 Uiso 1 1 calc R . . C36 C 0.6050(7) 0.8322(3) -0.1442(5) 0.0264(15) Uani 1 1 d . . . H36A H 0.5079 0.8436 -0.1862 0.032 Uiso 1 1 calc R . . C37 C 0.2778(6) 0.7463(3) 0.2400(5) 0.0229(12) Uani 1 1 d . . . C38 C 0.2357(7) 0.7976(3) 0.2957(5) 0.0261(15) Uani 1 1 d . . . H38A H 0.2987 0.8319 0.3152 0.031 Uiso 1 1 calc R . . C39 C 0.1023(7) 0.7990(3) 0.3230(5) 0.0260(14) Uani 1 1 d . . . H39A H 0.0741 0.8343 0.3597 0.031 Uiso 1 1 calc R . . C40 C 0.0121(6) 0.7489(3) 0.2964(5) 0.0321(14) Uani 1 1 d . . . H40A H -0.0795 0.7499 0.3135 0.038 Uiso 1 1 calc R . . C41 C 0.0536(7) 0.6973(3) 0.2453(6) 0.0360(16) Uani 1 1 d . . . H41A H -0.0074 0.6623 0.2308 0.043 Uiso 1 1 calc R . . C42 C 0.1849(7) 0.6962(3) 0.2145(6) 0.0308(15) Uani 1 1 d . . . H42A H 0.2109 0.6611 0.1759 0.037 Uiso 1 1 calc R . . C43 C 0.5694(6) 0.7869(2) 0.3230(5) 0.0240(14) Uani 1 1 d . . . C44 C 0.6451(7) 0.8390(3) 0.3058(6) 0.0257(15) Uani 1 1 d . . . H44A H 0.6292 0.8557 0.2252 0.031 Uiso 1 1 calc R . . C45 C 0.7426(7) 0.8662(3) 0.4048(6) 0.0370(17) Uani 1 1 d . . . H45A H 0.7929 0.9019 0.3915 0.044 Uiso 1 1 calc R . . C46 C 0.7695(7) 0.8431(3) 0.5234(6) 0.0364(17) Uani 1 1 d . . . H46A H 0.8365 0.8629 0.5909 0.044 Uiso 1 1 calc R . . C47 C 0.6972(7) 0.7905(3) 0.5426(6) 0.0348(16) Uani 1 1 d . . . H47A H 0.7159 0.7736 0.6233 0.042 Uiso 1 1 calc R . . C48 C 0.5972(6) 0.7628(3) 0.4427(5) 0.0272(14) Uani 1 1 d . . . H48A H 0.5471 0.7272 0.4560 0.033 Uiso 1 1 calc R . . C49 C 0.2043(7) 0.9188(3) 0.0911(5) 0.0329(15) Uani 1 1 d . . . H49A H 0.1717 0.8778 0.1089 0.039 Uiso 1 1 calc R . . H49B H 0.1166 0.9435 0.0528 0.039 Uiso 1 1 calc R . . C50 C 0.2872(7) 0.9482(3) 0.2100(5) 0.0331(17) Uani 1 1 d . . . H50A H 0.2313 0.9448 0.2705 0.050 Uiso 1 1 calc R . . H50B H 0.3034 0.9914 0.1954 0.050 Uiso 1 1 calc R . . H50C H 0.3812 0.9276 0.2421 0.050 Uiso 1 1 calc R . . P2 P 0.52803(17) 0.58584(7) -0.01134(14) 0.0223(4) Uani 1 1 d . . . N2 N 0.4227(5) 0.7916(2) 0.0694(4) 0.0244(12) Uani 1 1 d . . . H1N2 H 0.381(6) 0.828(2) 0.053(5) 0.021(8) Uiso 1 1 d . . . P3 P 0.48277(17) 0.74268(7) -0.02212(14) 0.0232(4) Uani 1 1 d . . . P4 P 0.44728(17) 0.74587(7) 0.19474(13) 0.0230(3) Uani 1 1 d . . . H1FE H 0.3728 0.6612 0.0301 0.021(8) Uiso 1 1 d 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 0.0238(5) 0.0246(4) 0.0197(4) 0.0005(4) 0.0056(4) 0.0016(4) P1 0.0274(9) 0.0241(8) 0.0249(9) 0.0008(7) 0.0069(7) 0.0009(7) O1 0.043(3) 0.026(2) 0.037(3) 0.004(2) 0.021(2) -0.003(2) N1 0.025(3) 0.025(3) 0.025(3) -0.002(2) 0.011(2) -0.004(2) B1 0.026(4) 0.024(4) 0.024(4) -0.007(3) 0.004(3) 0.002(3) C1 0.023(4) 0.032(3) 0.038(4) 0.003(3) 0.002(3) 0.003(3) C2 0.035(5) 0.055(5) 0.054(5) 0.013(4) 0.004(4) 0.003(4) C3 0.036(5) 0.061(5) 0.066(6) 0.029(4) -0.017(4) -0.004(4) C4 0.032(5) 0.049(5) 0.093(7) -0.003(5) 0.022(5) -0.005(4) C5 0.041(5) 0.041(4) 0.071(6) -0.010(4) 0.022(4) -0.006(3) C6 0.031(4) 0.030(3) 0.049(4) -0.008(3) 0.013(3) -0.002(3) C7 0.023(4) 0.031(4) 0.027(4) 0.000(3) 0.002(3) -0.004(3) C8 0.032(4) 0.036(4) 0.038(4) 0.006(3) 0.005(3) 0.001(3) C9 0.039(5) 0.060(5) 0.031(4) 0.011(3) 0.013(3) 0.000(4) C10 0.046(5) 0.044(4) 0.031(4) 0.015(3) -0.007(4) -0.013(3) C11 0.052(5) 0.024(3) 0.033(4) 0.003(3) -0.012(4) -0.001(3) C12 0.039(4) 0.022(3) 0.037(4) 0.002(3) 0.004(3) 0.000(3) C13 0.035(4) 0.010(3) 0.026(3) 0.003(2) 0.013(3) 0.003(2) C14 0.040(4) 0.030(3) 0.033(4) -0.004(3) 0.016(3) -0.004(3) C15 0.057(5) 0.036(4) 0.050(5) 0.007(3) 0.037(4) 0.001(3) C16 0.070(6) 0.041(4) 0.040(5) 0.012(3) 0.039(4) 0.015(4) C17 0.065(6) 0.047(4) 0.030(4) 0.003(3) 0.017(4) 0.023(4) C18 0.041(4) 0.041(4) 0.019(3) 0.010(3) 0.010(3) 0.019(3) C19 0.023(3) 0.044(4) 0.018(3) 0.000(3) 0.009(3) 0.001(3) C20 0.032(4) 0.026(3) 0.024(4) -0.003(3) 0.013(3) -0.008(3) C21 0.045(4) 0.027(3) 0.042(4) -0.011(3) 0.023(4) -0.008(3) C22 0.028(4) 0.056(5) 0.041(5) -0.018(3) 0.008(3) -0.008(3) C23 0.027(4) 0.050(4) 0.049(4) -0.010(4) 0.011(3) 0.014(3) C24 0.030(4) 0.043(4) 0.022(4) -0.011(3) 0.003(3) -0.002(3) C25 0.021(3) 0.030(3) 0.026(3) 0.007(3) 0.009(3) -0.005(3) C26 0.027(4) 0.028(3) 0.022(3) 0.000(2) 0.009(3) 0.003(3) C27 0.046(5) 0.027(3) 0.022(4) 0.006(3) 0.007(3) 0.004(3) C28 0.033(4) 0.034(4) 0.026(4) 0.007(3) 0.000(3) -0.006(3) C29 0.033(4) 0.042(4) 0.028(4) 0.010(3) 0.006(3) 0.001(3) C30 0.024(3) 0.031(4) 0.027(4) 0.010(3) 0.007(3) 0.003(3) C31 0.030(4) 0.014(3) 0.023(3) -0.001(2) 0.012(3) -0.002(2) C32 0.037(4) 0.027(3) 0.016(3) -0.002(2) 0.005(3) -0.009(3) C33 0.024(4) 0.034(4) 0.036(4) -0.006(3) 0.006(3) -0.002(3) C34 0.039(4) 0.039(4) 0.020(3) -0.003(3) 0.011(3) -0.013(3) C35 0.049(5) 0.025(3) 0.024(4) 0.010(3) 0.012(3) -0.008(3) C36 0.026(4) 0.033(3) 0.021(3) -0.001(3) 0.008(3) -0.009(3) C37 0.026(3) 0.033(3) 0.014(3) 0.005(3) 0.012(2) 0.005(3) C38 0.029(4) 0.025(3) 0.025(4) 0.001(3) 0.009(3) -0.002(3) C39 0.028(4) 0.033(3) 0.017(3) -0.003(3) 0.007(3) 0.006(3) C40 0.028(4) 0.044(4) 0.027(3) 0.005(3) 0.012(3) 0.004(3) C41 0.029(4) 0.041(4) 0.040(4) -0.001(3) 0.013(3) -0.011(3) C42 0.031(4) 0.028(3) 0.035(4) -0.009(3) 0.013(3) -0.001(3) C43 0.020(3) 0.024(3) 0.026(4) -0.008(3) 0.004(3) -0.001(3) C44 0.027(4) 0.027(3) 0.026(4) -0.003(3) 0.013(3) -0.008(3) C45 0.032(4) 0.040(4) 0.045(5) -0.004(3) 0.021(4) -0.006(3) C46 0.031(4) 0.045(4) 0.029(4) -0.010(3) 0.001(3) 0.000(3) C47 0.027(4) 0.050(4) 0.027(4) 0.000(3) 0.006(3) 0.009(3) C48 0.027(4) 0.034(3) 0.020(3) -0.002(3) 0.006(3) 0.000(3) C49 0.040(4) 0.032(3) 0.027(4) 0.004(3) 0.010(3) -0.003(3) C50 0.041(4) 0.031(3) 0.026(4) 0.001(3) 0.008(3) -0.007(3) P2 0.0204(9) 0.0274(8) 0.0189(9) 0.0020(7) 0.0055(7) 0.0025(7) N2 0.029(3) 0.014(2) 0.029(3) 0.000(2) 0.006(2) 0.005(2) P3 0.0229(9) 0.0262(8) 0.0198(9) -0.0004(7) 0.0049(7) -0.0015(7) P4 0.0258(9) 0.0244(8) 0.0191(8) -0.0014(7) 0.0072(7) -0.0010(7) _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 B1 2.078(7) . ? Fe1 P3 2.1697(18) . ? Fe1 P4 2.1811(18) . ? Fe1 P2 2.2381(19) . ? Fe1 H3B1 1.81(4) . ? Fe1 H1B1 1.44(5) . ? Fe1 H1FE 1.3891 . ? P1 N1 1.604(5) . ? P1 C7 1.801(7) . ? P1 C1 1.824(6) . ? P1 B1 1.946(7) . ? O1 C49 1.428(7) . ? O1 H1O1 0.99(5) . ? N1 P2 1.670(5) . ? B1 H3B1 1.36(5) . ? B1 H2B1 1.12(5) . ? B1 H1B1 1.15(6) . ? C1 C2 1.391(8) . ? C1 C6 1.396(8) . ? C2 C3 1.413(10) . ? C2 H2A 0.9500 . ? C3 C4 1.379(11) . ? C3 H3A 0.9500 . ? C4 C5 1.353(10) . ? C4 H4A 0.9500 . ? C5 C6 1.377(9) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C12 1.388(8) . ? C7 C8 1.391(9) . ? C8 C9 1.407(9) . ? C8 H8A 0.9500 . ? C9 C10 1.368(9) . ? C9 H9A 0.9500 . ? C10 C11 1.402(10) . ? C10 H10A 0.9500 . ? C11 C12 1.375(8) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.385(8) . ? C13 C18 1.394(8) . ? C13 P2 1.849(6) . ? C14 C15 1.401(9) . ? C14 H14A 0.9500 . ? C15 C16 1.372(10) . ? C15 H15A 0.9500 . ? C16 C17 1.367(10) . ? C16 H16A 0.9500 . ? C17 C18 1.378(9) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.393(8) . ? C19 C20 1.397(8) . ? C19 P2 1.828(6) . ? C20 C21 1.395(8) . ? C20 H20A 0.9500 . ? C21 C22 1.395(9) . ? C21 H21A 0.9500 . ? C22 C23 1.363(9) . ? C22 H22A 0.9500 . ? C23 C24 1.396(9) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C30 1.406(8) . ? C25 C26 1.411(8) . ? C25 P3 1.815(5) . ? C26 C27 1.399(8) . ? C26 H26A 0.9500 . ? C27 C28 1.377(9) . ? C27 H27A 0.9500 . ? C28 C29 1.392(8) . ? C28 H28A 0.9500 . ? C29 C30 1.382(7) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C36 1.398(7) . ? C31 C32 1.411(8) . ? C31 P3 1.829(6) . ? C32 C33 1.403(8) . ? C32 H32A 0.9500 . ? C33 C34 1.391(8) . ? C33 H33A 0.9500 . ? C34 C35 1.378(9) . ? C34 H34A 0.9500 . ? C35 C36 1.393(8) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.391(8) . ? C37 C38 1.398(8) . ? C37 P4 1.833(6) . ? C38 C39 1.396(8) . ? C38 H38A 0.9500 . ? C39 C40 1.377(8) . ? C39 H39A 0.9500 . ? C40 C41 1.375(8) . ? C40 H40A 0.9500 . ? C41 C42 1.396(9) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C44 1.393(8) . ? C43 C48 1.402(8) . ? C43 P4 1.819(5) . ? C44 C45 1.373(8) . ? C44 H44A 0.9500 . ? C45 C46 1.382(9) . ? C45 H45A 0.9500 . ? C46 C47 1.392(9) . ? C46 H46A 0.9500 . ? C47 C48 1.394(8) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C50 1.496(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? N2 P4 1.691(5) . ? N2 P3 1.695(5) . ? N2 H1N2 0.90(5) . ? P3 P4 2.559(2) . ? 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 B1 Fe1 P3 143.4(2) . . ? B1 Fe1 P4 102.22(19) . . ? P3 Fe1 P4 72.06(7) . . ? B1 Fe1 P2 88.99(19) . . ? P3 Fe1 P2 103.33(6) . . ? P4 Fe1 P2 166.49(7) . . ? B1 Fe1 H3B1 40.3(15) . . ? P3 Fe1 H3B1 103.8(16) . . ? P4 Fe1 H3B1 99.4(15) . . ? P2 Fe1 H3B1 94.0(15) . . ? B1 Fe1 H1B1 32(2) . . ? P3 Fe1 H1B1 167(2) . . ? P4 Fe1 H1B1 96(2) . . ? P2 Fe1 H1B1 90(2) . . ? H3B1 Fe1 H1B1 72(3) . . ? B1 Fe1 H1FE 142.5 . . ? P3 Fe1 H1FE 74.1 . . ? P4 Fe1 H1FE 89.5 . . ? P2 Fe1 H1FE 77.0 . . ? H3B1 Fe1 H1FE 169.8 . . ? H1B1 Fe1 H1FE 112.3 . . ? N1 P1 C7 111.7(3) . . ? N1 P1 C1 108.2(3) . . ? C7 P1 C1 101.4(3) . . ? N1 P1 B1 110.6(3) . . ? C7 P1 B1 110.5(3) . . ? C1 P1 B1 114.1(3) . . ? C49 O1 H1O1 106(3) . . ? P1 N1 P2 115.6(3) . . ? P1 B1 Fe1 111.1(3) . . ? P1 B1 H3B1 107(2) . . ? Fe1 B1 H3B1 59.0(17) . . ? P1 B1 H2B1 116(2) . . ? Fe1 B1 H2B1 133(2) . . ? H3B1 B1 H2B1 108(3) . . ? P1 B1 H1B1 107(3) . . ? H3B1 B1 H1B1 101(3) . . ? H2B1 B1 H1B1 117(4) . . ? C2 C1 C6 120.6(6) . . ? C2 C1 P1 120.3(5) . . ? C6 C1 P1 119.1(4) . . ? C1 C2 C3 118.1(7) . . ? C1 C2 H2A 121.0 . . ? C3 C2 H2A 121.0 . . ? C4 C3 C2 120.0(7) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C5 C4 C3 121.0(8) . . ? C5 C4 H4A 119.5 . . ? C3 C4 H4A 119.5 . . ? C4 C5 C6 120.6(8) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C5 C6 C1 119.6(6) . . ? C5 C6 H6A 120.2 . . ? C1 C6 H6A 120.2 . . ? C12 C7 C8 117.8(6) . . ? C12 C7 P1 121.8(6) . . ? C8 C7 P1 120.3(5) . . ? C7 C8 C9 120.9(6) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C10 C9 C8 119.9(7) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C11 119.9(6) . . ? C9 C10 H10A 120.0 . . ? C11 C10 H10A 120.0 . . ? C12 C11 C10 119.4(6) . . ? C12 C11 H11A 120.3 . . ? C10 C11 H11A 120.3 . . ? C11 C12 C7 122.1(7) . . ? C11 C12 H12A 119.0 . . ? C7 C12 H12A 119.0 . . ? C14 C13 C18 118.9(6) . . ? C14 C13 P2 116.4(4) . . ? C18 C13 P2 124.7(5) . . ? C13 C14 C15 120.2(6) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C17 C16 C15 120.1(7) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 120.9(7) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C13 120.1(7) . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? C24 C19 C20 119.2(6) . . ? C24 C19 P2 120.1(5) . . ? C20 C19 P2 120.6(4) . . ? C21 C20 C19 120.8(6) . . ? C21 C20 H20A 119.6 . . ? C19 C20 H20A 119.6 . . ? C20 C21 C22 118.9(6) . . ? C20 C21 H21A 120.6 . . ? C22 C21 H21A 120.6 . . ? C23 C22 C21 120.4(6) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C24 121.3(6) . . ? C22 C23 H23A 119.4 . . ? C24 C23 H23A 119.4 . . ? C19 C24 C23 119.2(6) . . ? C19 C24 H24A 120.4 . . ? C23 C24 H24A 120.4 . . ? C30 C25 C26 118.8(5) . . ? C30 C25 P3 119.4(4) . . ? C26 C25 P3 121.5(4) . . ? C27 C26 C25 119.3(6) . . ? C27 C26 H26A 120.4 . . ? C25 C26 H26A 120.4 . . ? C28 C27 C26 121.5(6) . . ? C28 C27 H27A 119.2 . . ? C26 C27 H27A 119.2 . . ? C27 C28 C29 119.1(6) . . ? C27 C28 H28A 120.5 . . ? C29 C28 H28A 120.5 . . ? C30 C29 C28 120.9(6) . . ? C30 C29 H29A 119.5 . . ? C28 C29 H29A 119.5 . . ? C29 C30 C25 120.3(6) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? C36 C31 C32 119.1(5) . . ? C36 C31 P3 122.0(4) . . ? C32 C31 P3 118.8(4) . . ? C33 C32 C31 119.8(5) . . ? C33 C32 H32A 120.1 . . ? C31 C32 H32A 120.1 . . ? C34 C33 C32 120.0(6) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C35 C34 C33 120.3(6) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.6(6) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C35 C36 C31 120.2(6) . . ? C35 C36 H36A 119.9 . . ? C31 C36 H36A 119.9 . . ? C42 C37 C38 118.5(5) . . ? C42 C37 P4 120.2(5) . . ? C38 C37 P4 121.3(5) . . ? C39 C38 C37 121.0(6) . . ? C39 C38 H38A 119.5 . . ? C37 C38 H38A 119.5 . . ? C40 C39 C38 119.4(6) . . ? C40 C39 H39A 120.3 . . ? C38 C39 H39A 120.3 . . ? C41 C40 C39 120.5(6) . . ? C41 C40 H40A 119.8 . . ? C39 C40 H40A 119.8 . . ? C40 C41 C42 120.4(6) . . ? C40 C41 H41A 119.8 . . ? C42 C41 H41A 119.8 . . ? C37 C42 C41 120.2(6) . . ? C37 C42 H42A 119.9 . . ? C41 C42 H42A 119.9 . . ? C44 C43 C48 118.4(5) . . ? C44 C43 P4 122.5(5) . . ? C48 C43 P4 118.9(4) . . ? C45 C44 C43 120.3(6) . . ? C45 C44 H44A 119.9 . . ? C43 C44 H44A 119.9 . . ? C44 C45 C46 121.6(6) . . ? C44 C45 H45A 119.2 . . ? C46 C45 H45A 119.2 . . ? C45 C46 C47 119.2(6) . . ? C45 C46 H46A 120.4 . . ? C47 C46 H46A 120.4 . . ? C46 C47 C48 119.5(6) . . ? C46 C47 H47A 120.2 . . ? C48 C47 H47A 120.2 . . ? C47 C48 C43 120.9(6) . . ? C47 C48 H48A 119.5 . . ? C43 C48 H48A 119.5 . . ? O1 C49 C50 112.6(5) . . ? O1 C49 H49A 109.1 . . ? C50 C49 H49A 109.1 . . ? O1 C49 H49B 109.1 . . ? C50 C49 H49B 109.1 . . ? H49A C49 H49B 107.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N1 P2 C19 104.8(3) . . ? N1 P2 C13 102.4(2) . . ? C19 P2 C13 100.8(3) . . ? N1 P2 Fe1 113.72(17) . . ? C19 P2 Fe1 117.0(2) . . ? C13 P2 Fe1 116.20(17) . . ? P4 N2 P3 98.2(2) . . ? P4 N2 H1N2 131(4) . . ? P3 N2 H1N2 130(3) . . ? N2 P3 C25 104.9(3) . . ? N2 P3 C31 104.8(2) . . ? C25 P3 C31 103.5(3) . . ? N2 P3 Fe1 94.88(18) . . ? C25 P3 Fe1 121.1(2) . . ? C31 P3 Fe1 124.16(19) . . ? C25 P3 P4 126.2(2) . . ? C31 P3 P4 122.27(19) . . ? Fe1 P3 P4 54.18(6) . . ? N2 P4 C43 106.1(2) . . ? N2 P4 C37 107.6(2) . . ? C43 P4 C37 101.4(3) . . ? N2 P4 Fe1 94.58(18) . . ? C43 P4 Fe1 123.3(2) . . ? C37 P4 Fe1 121.8(2) . . ? C43 P4 P3 122.8(2) . . ? C37 P4 P3 129.13(17) . . ? Fe1 P4 P3 53.76(6) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.818 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.074 _database_code_depnum_ccdc_archive 'CCDC 937585' ####################################################################### # # 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_rl210b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H46 Fe N3 P4, C2 H3 N, B H4' _chemical_formula_sum 'C52 H53 B Fe N4 P4' _chemical_formula_weight 924.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.018(3) _cell_length_b 19.641(4) _cell_length_c 20.451(4) _cell_angle_alpha 102.39(3) _cell_angle_beta 93.89(3) _cell_angle_gamma 106.63(3) _cell_volume 4846.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 20573 _cell_measurement_theta_min 1.613 _cell_measurement_theta_max 27.18 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.482 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9028 _exptl_absorpt_correction_T_max 0.9496 _exptl_absorpt_process_details 'STOE X-Red32 1.53' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -5 2 -6 0.0980 0 1 -1 0.1280 1 2 -1 0.1060 4 -1 4 0.0990 -3 -5 2 0.0980 3 -5 -4 0.0750 3 -7 1 0.0680 -2 5 -2 0.1040 0 3 -8 0.1390 -3 4 6 0.1330 0 -3 5 0.1610 _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_detector 'image plate ( 34 cm diameter )' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 32 _diffrn_source_power 1.60 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm, multiple pinhole' _diffrn_ambient_temperature 100(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 208 frames, detector distance = 120 mm ; _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37872 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.1428 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 26.20 _reflns_number_total 19049 _reflns_number_gt 10514 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0332P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 19049 _refine_ls_number_parameters 1192 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1053 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.849 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.05409(4) 0.30718(3) 0.75342(3) 0.02533(13) Uani 1 1 d . . . Fe2 Fe 0.47609(4) 0.23041(3) 0.24835(3) 0.02552(13) Uani 1 1 d . . . P1 P -0.09325(7) 0.34093(5) 0.75653(5) 0.0257(2) Uani 1 1 d . . . P2 P -0.02052(7) 0.28928(5) 0.64782(5) 0.0270(2) Uani 1 1 d . . . P3 P 0.11022(7) 0.30680(5) 0.85763(5) 0.0271(2) Uani 1 1 d . . . P4 P 0.18126(7) 0.25331(5) 0.75021(5) 0.0266(2) Uani 1 1 d . . . P5 P 0.61130(8) 0.23271(5) 0.31980(5) 0.0280(2) Uani 1 1 d . . . P6 P 0.45051(7) 0.27926(5) 0.35106(5) 0.0271(2) Uani 1 1 d . . . P7 P 0.50346(7) 0.18584(5) 0.14441(5) 0.0266(2) Uani 1 1 d . . . P8 P 0.37252(7) 0.25951(5) 0.17731(5) 0.0264(2) Uani 1 1 d . . . N1 N -0.1234(2) 0.32088(17) 0.67142(15) 0.0274(7) Uani 1 1 d . . . N2 N 0.2043(2) 0.26555(18) 0.83466(15) 0.0302(7) Uani 1 1 d . . . N3 N 0.1507(2) 0.40195(18) 0.75437(15) 0.0312(7) Uani 1 1 d . . . N4 N 0.5655(2) 0.27370(17) 0.38877(15) 0.0296(8) Uani 1 1 d . . . N5 N 0.4121(2) 0.21648(17) 0.10773(14) 0.0296(7) Uani 1 1 d . . . N6 N 0.3826(2) 0.13645(18) 0.25188(14) 0.0301(7) Uani 1 1 d . . . C1 C -0.0901(3) 0.4356(2) 0.78935(17) 0.0266(8) Uani 1 1 d . . . C2 C -0.1663(3) 0.4645(2) 0.76389(19) 0.0343(9) Uani 1 1 d . . . H2A H -0.2205 0.4350 0.7273 0.041 Uiso 1 1 calc R . . C3 C -0.1632(3) 0.5357(2) 0.7917(2) 0.0369(10) Uani 1 1 d . . . H3A H -0.2150 0.5551 0.7740 0.044 Uiso 1 1 calc R . . C4 C -0.0852(3) 0.5787(2) 0.8450(2) 0.0362(10) Uani 1 1 d . . . H4A H -0.0839 0.6275 0.8646 0.043 Uiso 1 1 calc R . . C5 C -0.0098(3) 0.5512(2) 0.8697(2) 0.0374(10) Uani 1 1 d . . . H5A H 0.0440 0.5810 0.9064 0.045 Uiso 1 1 calc R . . C6 C -0.0111(3) 0.4802(2) 0.84166(19) 0.0328(9) Uani 1 1 d . . . H6A H 0.0427 0.4620 0.8586 0.039 Uiso 1 1 calc R . . C7 C -0.2135(3) 0.28920(19) 0.78677(17) 0.0247(8) Uani 1 1 d . . . C8 C -0.2701(3) 0.2192(2) 0.7508(2) 0.0351(10) Uani 1 1 d . . . H8A H -0.2474 0.1989 0.7099 0.042 Uiso 1 1 calc R . . C9 C -0.3599(3) 0.1774(2) 0.7733(2) 0.0410(10) Uani 1 1 d . . . H9A H -0.3976 0.1288 0.7484 0.049 Uiso 1 1 calc R . . C10 C -0.3936(3) 0.2074(2) 0.8319(2) 0.0382(10) Uani 1 1 d . . . H10A H -0.4563 0.1798 0.8467 0.046 Uiso 1 1 calc R . . C11 C -0.3377(3) 0.2762(2) 0.8687(2) 0.0420(11) Uani 1 1 d . . . H11A H -0.3601 0.2955 0.9101 0.050 Uiso 1 1 calc R . . C12 C -0.2486(3) 0.3184(2) 0.84669(19) 0.0362(10) Uani 1 1 d . . . H12A H -0.2114 0.3669 0.8721 0.043 Uiso 1 1 calc R . . C13 C -0.0847(3) 0.1997(2) 0.58967(18) 0.0315(9) Uani 1 1 d . . . C14 C -0.1066(3) 0.1364(2) 0.6133(2) 0.0363(10) Uani 1 1 d . . . H14A H -0.0785 0.1389 0.6582 0.044 Uiso 1 1 calc R . . C15 C -0.1687(3) 0.0699(2) 0.5719(2) 0.0432(11) Uani 1 1 d . . . H15A H -0.1830 0.0269 0.5884 0.052 Uiso 1 1 calc R . . C16 C -0.2105(3) 0.0652(2) 0.5064(2) 0.0464(11) Uani 1 1 d . . . H16A H -0.2555 0.0197 0.4787 0.056 Uiso 1 1 calc R . . C17 C -0.1864(3) 0.1271(2) 0.4819(2) 0.0415(10) Uani 1 1 d . . . H17A H -0.2121 0.1236 0.4364 0.050 Uiso 1 1 calc R . . C18 C -0.1252(3) 0.1942(2) 0.52267(19) 0.0349(9) Uani 1 1 d . . . H18A H -0.1105 0.2367 0.5054 0.042 Uiso 1 1 calc R . . C19 C 0.0464(3) 0.3464(2) 0.59374(18) 0.0293(9) Uani 1 1 d . . . C20 C 0.1105(3) 0.3209(2) 0.54765(18) 0.0318(9) Uani 1 1 d . . . H20A H 0.1122 0.2718 0.5405 0.038 Uiso 1 1 calc R . . C21 C 0.1714(3) 0.3676(2) 0.51265(19) 0.0361(10) Uani 1 1 d . . . H21A H 0.2144 0.3501 0.4815 0.043 Uiso 1 1 calc R . . C22 C 0.1703(3) 0.4386(2) 0.52240(19) 0.0394(10) Uani 1 1 d . . . H22A H 0.2136 0.4703 0.4988 0.047 Uiso 1 1 calc R . . C23 C 0.1058(3) 0.4643(2) 0.5667(2) 0.0411(10) Uani 1 1 d . . . H23A H 0.1035 0.5131 0.5727 0.049 Uiso 1 1 calc R . . C24 C 0.0440(3) 0.4177(2) 0.60265(19) 0.0366(10) Uani 1 1 d . . . H24A H 0.0002 0.4352 0.6333 0.044 Uiso 1 1 calc R . . C25 C 0.0329(3) 0.2504(2) 0.90833(18) 0.0288(9) Uani 1 1 d . . . C26 C -0.0679(3) 0.2009(2) 0.88208(19) 0.0333(9) Uani 1 1 d . . . H26A H -0.1039 0.2035 0.8411 0.040 Uiso 1 1 calc R . . C27 C -0.1177(3) 0.1472(2) 0.9146(2) 0.0376(10) Uani 1 1 d . . . H27A H -0.1879 0.1144 0.8966 0.045 Uiso 1 1 calc R . . C28 C -0.0646(3) 0.1419(2) 0.9731(2) 0.0415(10) Uani 1 1 d . . . H28A H -0.0960 0.1034 0.9938 0.050 Uiso 1 1 calc R . . C29 C 0.0348(3) 0.1929(2) 1.0017(2) 0.0424(11) Uani 1 1 d . . . H29A H 0.0693 0.1914 1.0436 0.051 Uiso 1 1 calc R . . C30 C 0.0835(3) 0.2461(2) 0.96923(19) 0.0364(10) Uani 1 1 d . . . H30A H 0.1524 0.2802 0.9885 0.044 Uiso 1 1 calc R . . C31 C 0.1835(3) 0.3927(2) 0.91739(18) 0.0328(9) Uani 1 1 d . . . C32 C 0.2865(3) 0.4326(2) 0.90749(19) 0.0380(10) Uani 1 1 d . . . H32A H 0.3217 0.4108 0.8736 0.046 Uiso 1 1 calc R . . C33 C 0.3382(3) 0.5028(2) 0.9456(2) 0.0422(11) Uani 1 1 d . . . H33A H 0.4083 0.5287 0.9379 0.051 Uiso 1 1 calc R . . C34 C 0.2879(4) 0.5358(2) 0.9953(2) 0.0472(12) Uani 1 1 d . . . H34A H 0.3227 0.5843 1.0215 0.057 Uiso 1 1 calc R . . C35 C 0.1859(4) 0.4967(2) 1.0061(2) 0.0464(11) Uani 1 1 d . . . H35A H 0.1519 0.5188 1.0406 0.056 Uiso 1 1 calc R . . C36 C 0.1333(3) 0.4270(2) 0.96804(19) 0.0375(10) Uani 1 1 d . . . H36A H 0.0630 0.4017 0.9758 0.045 Uiso 1 1 calc R . . C37 C 0.3124(3) 0.28794(19) 0.72265(18) 0.0272(8) Uani 1 1 d . . . C38 C 0.4083(3) 0.2873(2) 0.7570(2) 0.0358(10) Uani 1 1 d . . . H38A H 0.4079 0.2724 0.7982 0.043 Uiso 1 1 calc R . . C39 C 0.5044(3) 0.3086(2) 0.7302(2) 0.0414(10) Uani 1 1 d . . . H39A H 0.5703 0.3094 0.7539 0.050 Uiso 1 1 calc R . . C40 C 0.5046(3) 0.3284(2) 0.66971(19) 0.0347(9) Uani 1 1 d . . . H40A H 0.5705 0.3419 0.6514 0.042 Uiso 1 1 calc R . . C41 C 0.4103(3) 0.3291(2) 0.63529(19) 0.0356(10) Uani 1 1 d . . . H41A H 0.4108 0.3422 0.5932 0.043 Uiso 1 1 calc R . . C42 C 0.3141(3) 0.3102(2) 0.66298(18) 0.0315(9) Uani 1 1 d . . . H42A H 0.2493 0.3128 0.6406 0.038 Uiso 1 1 calc R . . C43 C 0.1457(3) 0.1554(2) 0.71294(18) 0.0283(9) Uani 1 1 d . . . C44 C 0.1574(4) 0.1297(2) 0.6462(2) 0.0542(13) Uani 1 1 d . . . H44A H 0.1914 0.1638 0.6215 0.065 Uiso 1 1 calc R . . C45 C 0.1211(4) 0.0566(2) 0.6146(2) 0.0566(13) Uani 1 1 d . . . H45A H 0.1289 0.0408 0.5685 0.068 Uiso 1 1 calc R . . C46 C 0.0737(3) 0.0061(2) 0.6493(2) 0.0490(12) Uani 1 1 d . . . H46A H 0.0500 -0.0448 0.6280 0.059 Uiso 1 1 calc R . . C47 C 0.0610(4) 0.0306(2) 0.7157(2) 0.0597(14) Uani 1 1 d . . . H47A H 0.0274 -0.0037 0.7402 0.072 Uiso 1 1 calc R . . C48 C 0.0967(3) 0.1046(2) 0.7469(2) 0.0462(11) Uani 1 1 d . . . H48A H 0.0872 0.1205 0.7927 0.055 Uiso 1 1 calc R . . C49 C 0.2075(3) 0.4573(2) 0.7523(2) 0.0409(10) Uani 1 1 d . . . C50 C 0.2796(4) 0.5280(3) 0.7476(4) 0.099(2) Uani 1 1 d . . . H50A H 0.2390 0.5521 0.7232 0.149 Uiso 1 1 calc R . . H50B H 0.3392 0.5203 0.7233 0.149 Uiso 1 1 calc R . . H50C H 0.3089 0.5591 0.7932 0.149 Uiso 1 1 calc R . . C51 C 0.6218(3) 0.1464(2) 0.33368(19) 0.0385(10) Uani 1 1 d . . . C52 C 0.5502(3) 0.1069(2) 0.3699(2) 0.0510(12) Uani 1 1 d . . . H52A H 0.5026 0.1285 0.3936 0.061 Uiso 1 1 calc R . . C53 C 0.5479(5) 0.0364(3) 0.3719(3) 0.0755(18) Uani 1 1 d . . . H53A H 0.4990 0.0107 0.3972 0.091 Uiso 1 1 calc R . . C54 C 0.6142(6) 0.0032(3) 0.3383(4) 0.090(2) Uani 1 1 d . . . H54A H 0.6122 -0.0451 0.3402 0.108 Uiso 1 1 calc R . . C55 C 0.6844(5) 0.0412(3) 0.3014(3) 0.0745(18) Uani 1 1 d . . . H55A H 0.7298 0.0180 0.2769 0.089 Uiso 1 1 calc R . . C56 C 0.6905(4) 0.1127(3) 0.2991(2) 0.0541(13) Uani 1 1 d . . . H56A H 0.7408 0.1383 0.2744 0.065 Uiso 1 1 calc R . . C57 C 0.7513(3) 0.2864(2) 0.32516(18) 0.0319(9) Uani 1 1 d . . . C58 C 0.8236(3) 0.2988(2) 0.3833(2) 0.0420(10) Uani 1 1 d . . . H58A H 0.7989 0.2775 0.4191 0.050 Uiso 1 1 calc R . . C59 C 0.9294(3) 0.3410(3) 0.3898(2) 0.0499(12) Uani 1 1 d . . . H59A H 0.9768 0.3495 0.4301 0.060 Uiso 1 1 calc R . . C60 C 0.9674(3) 0.3714(2) 0.3374(2) 0.0479(12) Uani 1 1 d . . . H60A H 1.0409 0.4002 0.3416 0.057 Uiso 1 1 calc R . . C61 C 0.8979(3) 0.3595(2) 0.2791(2) 0.0428(11) Uani 1 1 d . . . H61A H 0.9238 0.3803 0.2432 0.051 Uiso 1 1 calc R . . C62 C 0.7905(3) 0.3174(2) 0.27285(19) 0.0357(10) Uani 1 1 d . . . H62A H 0.7432 0.3096 0.2326 0.043 Uiso 1 1 calc R . . C63 C 0.4475(3) 0.3730(2) 0.38061(17) 0.0261(8) Uani 1 1 d . . . C64 C 0.5413(3) 0.4306(2) 0.40389(19) 0.0326(9) Uani 1 1 d . . . H64A H 0.6088 0.4213 0.4088 0.039 Uiso 1 1 calc R . . C65 C 0.5375(3) 0.5024(2) 0.4203(2) 0.0403(10) Uani 1 1 d . . . H65A H 0.6024 0.5419 0.4364 0.048 Uiso 1 1 calc R . . C66 C 0.4400(3) 0.5163(2) 0.41324(19) 0.0363(10) Uani 1 1 d . . . H66A H 0.4376 0.5653 0.4247 0.044 Uiso 1 1 calc R . . C67 C 0.3460(3) 0.4590(2) 0.38946(18) 0.0314(9) Uani 1 1 d . . . H67A H 0.2787 0.4685 0.3841 0.038 Uiso 1 1 calc R . . C68 C 0.3493(3) 0.3876(2) 0.37337(18) 0.0316(9) Uani 1 1 d . . . H68A H 0.2842 0.3482 0.3573 0.038 Uiso 1 1 calc R . . C69 C 0.3393(3) 0.22919(19) 0.38898(18) 0.0297(9) Uani 1 1 d . . . C70 C 0.2349(3) 0.2025(2) 0.35317(19) 0.0354(10) Uani 1 1 d . . . H70A H 0.2233 0.2085 0.3087 0.042 Uiso 1 1 calc R . . C71 C 0.1478(3) 0.1670(2) 0.3820(2) 0.0441(11) Uani 1 1 d . . . H71A H 0.0768 0.1505 0.3578 0.053 Uiso 1 1 calc R . . C72 C 0.1646(3) 0.1559(2) 0.4459(2) 0.0449(11) Uani 1 1 d . . . H72A H 0.1052 0.1311 0.4653 0.054 Uiso 1 1 calc R . . C73 C 0.2671(3) 0.1807(2) 0.4813(2) 0.0434(11) Uani 1 1 d . . . H73A H 0.2787 0.1726 0.5250 0.052 Uiso 1 1 calc R . . C74 C 0.3542(3) 0.2178(2) 0.4529(2) 0.0381(10) Uani 1 1 d . . . H74A H 0.4248 0.2355 0.4779 0.046 Uiso 1 1 calc R . . C75 C 0.6285(3) 0.21771(19) 0.11004(17) 0.0267(8) Uani 1 1 d . . . C76 C 0.6477(3) 0.2764(2) 0.0802(2) 0.0364(10) Uani 1 1 d . . . H76A H 0.5941 0.3000 0.0762 0.044 Uiso 1 1 calc R . . C77 C 0.7466(3) 0.3008(2) 0.0559(2) 0.0457(11) Uani 1 1 d . . . H77A H 0.7591 0.3403 0.0346 0.055 Uiso 1 1 calc R . . C78 C 0.8253(3) 0.2680(2) 0.0629(2) 0.0379(10) Uani 1 1 d . . . H78A H 0.8919 0.2847 0.0461 0.045 Uiso 1 1 calc R . . C79 C 0.8081(3) 0.2109(2) 0.09412(18) 0.0328(9) Uani 1 1 d . . . H79A H 0.8633 0.1890 0.0997 0.039 Uiso 1 1 calc R . . C80 C 0.7104(3) 0.1854(2) 0.11739(17) 0.0312(9) Uani 1 1 d . . . H80A H 0.6987 0.1458 0.1385 0.037 Uiso 1 1 calc R . . C81 C 0.4630(3) 0.0866(2) 0.10989(18) 0.0275(8) Uani 1 1 d . . . C82 C 0.3965(3) 0.0529(2) 0.04841(19) 0.0338(9) Uani 1 1 d . . . H82A H 0.3714 0.0817 0.0231 0.041 Uiso 1 1 calc R . . C83 C 0.3667(3) -0.0220(2) 0.0240(2) 0.0418(11) Uani 1 1 d . . . H83A H 0.3189 -0.0446 -0.0171 0.050 Uiso 1 1 calc R . . C84 C 0.4055(3) -0.0643(2) 0.0585(2) 0.0380(10) Uani 1 1 d . . . H84A H 0.3867 -0.1157 0.0407 0.046 Uiso 1 1 calc R . . C85 C 0.4724(3) -0.0311(2) 0.1196(2) 0.0400(10) Uani 1 1 d . . . H85A H 0.4989 -0.0600 0.1440 0.048 Uiso 1 1 calc R . . C86 C 0.5005(3) 0.0435(2) 0.14510(19) 0.0365(10) Uani 1 1 d . . . H86A H 0.5459 0.0656 0.1872 0.044 Uiso 1 1 calc R . . C87 C 0.2264(3) 0.2184(2) 0.17036(17) 0.0294(9) Uani 1 1 d . . . C88 C 0.1802(3) 0.1434(2) 0.14738(18) 0.0336(9) Uani 1 1 d . . . H88A H 0.2219 0.1145 0.1266 0.040 Uiso 1 1 calc R . . C89 C 0.0735(3) 0.1099(2) 0.1544(2) 0.0419(11) Uani 1 1 d . . . H89A H 0.0425 0.0583 0.1383 0.050 Uiso 1 1 calc R . . C90 C 0.0126(3) 0.1514(3) 0.1846(2) 0.0452(11) Uani 1 1 d . . . H90A H -0.0600 0.1282 0.1900 0.054 Uiso 1 1 calc R . . C91 C 0.0560(3) 0.2261(2) 0.2069(2) 0.0423(11) Uani 1 1 d . . . H91A H 0.0130 0.2542 0.2272 0.051 Uiso 1 1 calc R . . C92 C 0.1619(3) 0.2607(2) 0.20014(18) 0.0331(9) Uani 1 1 d . . . H92A H 0.1914 0.3125 0.2153 0.040 Uiso 1 1 calc R . . C93 C 0.3885(3) 0.3522(2) 0.16758(18) 0.0274(8) Uani 1 1 d . . . C94 C 0.3549(3) 0.3616(2) 0.10493(19) 0.0350(9) Uani 1 1 d . . . H94A H 0.3217 0.3200 0.0685 0.042 Uiso 1 1 calc R . . C95 C 0.3694(3) 0.4306(2) 0.0956(2) 0.0430(11) Uani 1 1 d . . . H95A H 0.3464 0.4364 0.0526 0.052 Uiso 1 1 calc R . . C96 C 0.4169(3) 0.4916(2) 0.1477(2) 0.0380(10) Uani 1 1 d . . . H96A H 0.4257 0.5392 0.1410 0.046 Uiso 1 1 calc R . . C97 C 0.4517(3) 0.4830(2) 0.21014(19) 0.0353(9) Uani 1 1 d . . . H97A H 0.4858 0.5249 0.2461 0.042 Uiso 1 1 calc R . . C98 C 0.4371(3) 0.4136(2) 0.22040(19) 0.0316(9) Uani 1 1 d . . . H98A H 0.4602 0.4080 0.2634 0.038 Uiso 1 1 calc R . . C99 C 0.3290(3) 0.0805(2) 0.25565(19) 0.0368(10) Uani 1 1 d . . . C100 C 0.2630(4) 0.0085(3) 0.2611(3) 0.0715(16) Uani 1 1 d . . . H10B H 0.2692 -0.0293 0.2230 0.107 Uiso 1 1 calc R . . H10C H 0.1872 0.0073 0.2605 0.107 Uiso 1 1 calc R . . H10D H 0.2883 -0.0008 0.3036 0.107 Uiso 1 1 calc R . . B1 B -0.2862(4) 0.3539(3) 0.5458(2) 0.0369(11) Uani 1 1 d . . . H1B1 H -0.237(3) 0.314(2) 0.5368(18) 0.038(5) Uiso 1 1 d . . . H2B1 H -0.256(3) 0.3995(19) 0.5121(18) 0.038(5) Uiso 1 1 d . . . H4B1 H -0.268(3) 0.3880(19) 0.6053(18) 0.038(5) Uiso 1 1 d . . . H3B1 H -0.382(3) 0.3261(19) 0.5330(17) 0.038(5) Uiso 1 1 d . . . B2 B 0.3900(4) 0.2305(3) -0.0590(2) 0.0416(12) Uani 1 1 d . . . H1B2 H 0.452(2) 0.1977(17) -0.0394(16) 0.024(4) Uiso 1 1 d . . . H2B2 H 0.320(2) 0.2247(17) -0.0297(16) 0.024(4) Uiso 1 1 d . . . H3B2 H 0.445(2) 0.2873(18) -0.0544(16) 0.024(4) Uiso 1 1 d . . . H4B2 H 0.356(2) 0.1974(17) -0.1176(16) 0.024(4) Uiso 1 1 d . . . C200 C -0.395(2) 0.1684(15) 0.5733(15) 0.099(11) Uani 0.50 1 d P A 1 H20B H -0.3783 0.1823 0.5310 0.149 Uiso 0.50 1 calc PR A 1 H20C H -0.3569 0.1337 0.5809 0.149 Uiso 0.50 1 calc PR A 1 H20D H -0.3711 0.2122 0.6110 0.149 Uiso 0.50 1 calc PR A 1 C201 C -0.5026(14) 0.1366(8) 0.5690(7) 0.050(4) Uani 0.50 1 d P A 1 N8 N -0.5957(8) 0.1088(6) 0.5641(9) 0.104(5) Uani 0.50 1 d P A 1 C203 C -0.4025(19) 0.1694(8) 0.5769(10) 0.049(7) Uani 0.50 1 d P B 2 H20E H -0.3446 0.1478 0.5832 0.074 Uiso 0.50 1 calc PR B 2 H20F H -0.4214 0.1891 0.6211 0.074 Uiso 0.50 1 calc PR B 2 H20G H -0.3778 0.2090 0.5541 0.074 Uiso 0.50 1 calc PR B 2 C202 C -0.4982(12) 0.1129(9) 0.5355(8) 0.053(4) Uani 0.50 1 d P B 2 N9 N -0.5641(10) 0.0686(6) 0.5000(6) 0.087(3) Uani 0.50 1 d P B 2 C101 C -0.1999(7) -0.0183(5) 0.1097(5) 0.0620(12) Uani 0.70 1 d P C 1 C102 C -0.1618(6) -0.0697(4) 0.0676(4) 0.0620(12) Uani 0.70 1 d P C 1 H10E H -0.2208 -0.1158 0.0510 0.093 Uiso 0.70 1 calc PR C 1 H10F H -0.1025 -0.0784 0.0934 0.093 Uiso 0.70 1 calc PR C 1 H10G H -0.1355 -0.0508 0.0293 0.093 Uiso 0.70 1 calc PR C 1 N7 N -0.2304(5) 0.0239(3) 0.1444(3) 0.0620(12) Uani 0.70 1 d P C 1 C104 C -0.2288(15) -0.0456(9) 0.1098(9) 0.056(3) Uani 0.30 1 d P D 2 H10H H -0.1844 -0.0244 0.1542 0.084 Uiso 0.30 1 calc PR D 2 H10I H -0.2650 -0.0979 0.1051 0.084 Uiso 0.30 1 calc PR D 2 H10J H -0.2834 -0.0206 0.1058 0.084 Uiso 0.30 1 calc PR D 2 N7A N -0.1010(11) -0.0225(7) 0.0135(7) 0.056(3) Uani 0.30 1 d P D 2 C103 C -0.1500(16) -0.0351(9) 0.0491(10) 0.056(3) Uani 0.30 1 d P D 2 H1N1 H -0.176(3) 0.3284(18) 0.6483(17) 0.023(4) Uiso 1 1 d . . . H1N4 H 0.593(3) 0.2934(19) 0.4272(18) 0.023(4) Uiso 1 1 d . . . H1N2 H 0.251(3) 0.2487(18) 0.8568(17) 0.023(4) Uiso 1 1 d . . . H1N5 H 0.3977(14) 0.2133(11) 0.0717(10) 0.023(4) Uiso 1 1 d . . . H1FE H -0.0238 0.2382 0.7465 0.023(4) Uiso 1 1 d R . . H2FE H 0.5550 0.2982 0.2611 0.023(4) Uiso 1 1 d 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 0.0255(3) 0.0304(3) 0.0227(3) 0.0079(2) 0.0061(2) 0.0110(2) Fe2 0.0290(3) 0.0274(3) 0.0215(3) 0.0070(2) 0.0042(2) 0.0098(2) P1 0.0250(5) 0.0292(5) 0.0237(5) 0.0060(4) 0.0051(4) 0.0095(4) P2 0.0289(5) 0.0318(6) 0.0231(5) 0.0078(4) 0.0061(4) 0.0121(4) P3 0.0262(5) 0.0339(6) 0.0241(5) 0.0084(4) 0.0067(4) 0.0121(4) P4 0.0266(5) 0.0320(6) 0.0239(5) 0.0090(4) 0.0070(4) 0.0109(4) P5 0.0331(5) 0.0308(5) 0.0220(5) 0.0065(4) 0.0033(4) 0.0131(4) P6 0.0289(5) 0.0290(5) 0.0237(5) 0.0076(4) 0.0051(4) 0.0084(4) P7 0.0304(5) 0.0281(5) 0.0224(5) 0.0064(4) 0.0036(4) 0.0107(4) P8 0.0277(5) 0.0284(5) 0.0237(5) 0.0066(4) 0.0029(4) 0.0096(4) N1 0.0249(16) 0.0382(19) 0.0236(17) 0.0089(14) 0.0044(13) 0.0154(15) N2 0.0257(17) 0.045(2) 0.0266(18) 0.0135(15) 0.0049(13) 0.0175(15) N3 0.0305(18) 0.035(2) 0.0292(18) 0.0054(15) 0.0018(13) 0.0143(15) N4 0.0406(19) 0.0313(19) 0.0162(16) 0.0034(14) 0.0050(13) 0.0114(15) N5 0.0345(17) 0.0385(19) 0.0186(16) 0.0098(14) 0.0073(13) 0.0126(15) N6 0.0329(18) 0.036(2) 0.0193(16) 0.0057(14) 0.0041(13) 0.0088(15) C1 0.0248(19) 0.031(2) 0.0234(19) 0.0069(16) 0.0090(15) 0.0055(16) C2 0.032(2) 0.035(2) 0.033(2) 0.0032(18) 0.0008(16) 0.0109(18) C3 0.036(2) 0.034(2) 0.043(2) 0.008(2) 0.0061(18) 0.0161(18) C4 0.039(2) 0.029(2) 0.045(3) 0.0100(19) 0.0153(19) 0.0137(18) C5 0.043(2) 0.030(2) 0.033(2) 0.0025(18) 0.0009(18) 0.0072(19) C6 0.032(2) 0.037(2) 0.033(2) 0.0094(18) 0.0067(17) 0.0146(18) C7 0.0237(19) 0.026(2) 0.027(2) 0.0090(16) 0.0044(15) 0.0096(16) C8 0.030(2) 0.038(2) 0.039(2) 0.0063(19) 0.0134(17) 0.0128(18) C9 0.039(2) 0.030(2) 0.053(3) 0.007(2) 0.010(2) 0.0090(19) C10 0.035(2) 0.040(3) 0.048(3) 0.021(2) 0.0178(19) 0.0154(19) C11 0.047(3) 0.038(3) 0.034(2) 0.003(2) 0.0162(19) 0.006(2) C12 0.037(2) 0.034(2) 0.031(2) 0.0024(18) 0.0085(17) 0.0055(18) C13 0.028(2) 0.041(2) 0.028(2) 0.0086(18) 0.0063(16) 0.0136(17) C14 0.038(2) 0.041(2) 0.029(2) 0.0063(19) 0.0036(17) 0.0142(19) C15 0.050(3) 0.036(2) 0.045(3) 0.008(2) 0.002(2) 0.016(2) C16 0.048(3) 0.044(3) 0.038(3) -0.006(2) -0.002(2) 0.015(2) C17 0.046(2) 0.049(3) 0.028(2) 0.003(2) -0.0021(18) 0.019(2) C18 0.039(2) 0.039(2) 0.030(2) 0.0077(18) 0.0042(17) 0.0189(19) C19 0.0264(19) 0.033(2) 0.028(2) 0.0096(17) 0.0020(15) 0.0087(17) C20 0.033(2) 0.041(2) 0.025(2) 0.0098(18) 0.0024(16) 0.0151(18) C21 0.032(2) 0.051(3) 0.028(2) 0.0125(19) 0.0078(16) 0.0128(19) C22 0.031(2) 0.054(3) 0.033(2) 0.019(2) 0.0050(17) 0.005(2) C23 0.046(2) 0.039(2) 0.042(3) 0.019(2) 0.0070(19) 0.013(2) C24 0.041(2) 0.036(2) 0.037(2) 0.0099(19) 0.0124(18) 0.0150(19) C25 0.032(2) 0.033(2) 0.027(2) 0.0095(17) 0.0133(16) 0.0159(17) C26 0.035(2) 0.038(2) 0.033(2) 0.0112(18) 0.0113(17) 0.0167(19) C27 0.037(2) 0.039(2) 0.035(2) 0.0069(19) 0.0119(18) 0.0090(19) C28 0.049(3) 0.045(3) 0.041(3) 0.020(2) 0.025(2) 0.020(2) C29 0.050(3) 0.061(3) 0.031(2) 0.023(2) 0.0134(19) 0.028(2) C30 0.033(2) 0.050(3) 0.035(2) 0.016(2) 0.0103(17) 0.0212(19) C31 0.036(2) 0.039(2) 0.027(2) 0.0117(18) 0.0017(16) 0.0147(18) C32 0.039(2) 0.043(3) 0.028(2) 0.0097(19) 0.0014(17) 0.007(2) C33 0.043(2) 0.042(3) 0.037(2) 0.015(2) -0.0013(19) 0.005(2) C34 0.063(3) 0.029(2) 0.046(3) 0.009(2) -0.016(2) 0.013(2) C35 0.063(3) 0.041(3) 0.036(2) 0.000(2) 0.000(2) 0.025(2) C36 0.040(2) 0.041(3) 0.034(2) 0.0054(19) 0.0035(18) 0.0195(19) C37 0.029(2) 0.026(2) 0.028(2) 0.0066(16) 0.0084(15) 0.0092(16) C38 0.032(2) 0.045(2) 0.040(2) 0.025(2) 0.0143(17) 0.0157(19) C39 0.027(2) 0.049(3) 0.057(3) 0.025(2) 0.0121(18) 0.0153(19) C40 0.032(2) 0.034(2) 0.040(2) 0.0129(19) 0.0191(18) 0.0077(18) C41 0.039(2) 0.036(2) 0.029(2) 0.0099(18) 0.0105(17) 0.0037(18) C42 0.030(2) 0.035(2) 0.029(2) 0.0111(18) 0.0022(16) 0.0076(17) C43 0.0205(18) 0.033(2) 0.033(2) 0.0110(18) 0.0028(15) 0.0089(16) C44 0.075(3) 0.037(3) 0.047(3) 0.007(2) 0.033(2) 0.008(2) C45 0.073(3) 0.042(3) 0.050(3) 0.000(2) 0.032(2) 0.013(2) C46 0.049(3) 0.031(2) 0.063(3) 0.005(2) 0.005(2) 0.012(2) C47 0.077(3) 0.037(3) 0.057(3) 0.019(2) 0.010(3) -0.002(2) C48 0.060(3) 0.040(3) 0.036(2) 0.014(2) 0.011(2) 0.008(2) C49 0.031(2) 0.035(2) 0.059(3) 0.016(2) 0.0060(19) 0.0117(19) C50 0.040(3) 0.065(4) 0.198(7) 0.075(4) -0.005(3) -0.001(3) C51 0.052(3) 0.033(2) 0.030(2) 0.0049(18) -0.0119(19) 0.018(2) C52 0.049(3) 0.039(3) 0.064(3) 0.024(2) -0.010(2) 0.008(2) C53 0.077(4) 0.039(3) 0.104(5) 0.034(3) -0.030(3) 0.007(3) C54 0.120(6) 0.045(4) 0.088(5) 0.005(3) -0.061(4) 0.027(4) C55 0.120(5) 0.070(4) 0.040(3) -0.017(3) -0.031(3) 0.072(4) C56 0.082(3) 0.062(3) 0.028(2) 0.001(2) -0.008(2) 0.047(3) C57 0.032(2) 0.034(2) 0.028(2) -0.0009(17) 0.0043(16) 0.0149(17) C58 0.034(2) 0.056(3) 0.035(2) 0.008(2) 0.0018(17) 0.015(2) C59 0.041(3) 0.066(3) 0.040(3) 0.005(2) -0.005(2) 0.021(2) C60 0.031(2) 0.053(3) 0.053(3) -0.001(2) 0.006(2) 0.013(2) C61 0.036(2) 0.051(3) 0.041(3) 0.010(2) 0.0124(19) 0.013(2) C62 0.039(2) 0.038(2) 0.029(2) 0.0026(18) 0.0041(17) 0.0152(19) C63 0.031(2) 0.033(2) 0.0181(18) 0.0100(16) 0.0077(15) 0.0123(17) C64 0.032(2) 0.033(2) 0.036(2) 0.0083(18) 0.0070(17) 0.0131(18) C65 0.037(2) 0.034(2) 0.045(3) 0.006(2) 0.0018(18) 0.0072(19) C66 0.043(2) 0.031(2) 0.038(2) 0.0099(18) 0.0068(18) 0.0150(19) C67 0.033(2) 0.039(2) 0.030(2) 0.0167(18) 0.0134(16) 0.0170(18) C68 0.032(2) 0.034(2) 0.027(2) 0.0092(17) 0.0048(16) 0.0062(18) C69 0.037(2) 0.023(2) 0.029(2) 0.0072(17) 0.0082(16) 0.0089(17) C70 0.037(2) 0.034(2) 0.031(2) 0.0076(18) 0.0053(17) 0.0042(18) C71 0.035(2) 0.041(3) 0.048(3) 0.012(2) 0.0056(19) -0.002(2) C72 0.049(3) 0.036(2) 0.043(3) 0.010(2) 0.022(2) 0.000(2) C73 0.056(3) 0.041(2) 0.033(2) 0.014(2) 0.017(2) 0.008(2) C74 0.038(2) 0.040(2) 0.034(2) 0.0101(19) 0.0065(17) 0.0073(19) C75 0.0261(19) 0.026(2) 0.023(2) 0.0007(16) -0.0004(15) 0.0049(16) C76 0.032(2) 0.034(2) 0.044(2) 0.0143(19) 0.0028(17) 0.0086(18) C77 0.034(2) 0.047(3) 0.060(3) 0.032(2) 0.007(2) 0.005(2) C78 0.029(2) 0.039(2) 0.046(3) 0.016(2) 0.0055(18) 0.0084(19) C79 0.032(2) 0.037(2) 0.031(2) 0.0056(18) 0.0039(16) 0.0156(18) C80 0.036(2) 0.032(2) 0.025(2) 0.0045(17) 0.0035(16) 0.0108(18) C81 0.0242(19) 0.032(2) 0.027(2) 0.0087(17) 0.0064(15) 0.0082(16) C82 0.034(2) 0.034(2) 0.031(2) 0.0045(18) 0.0022(17) 0.0087(18) C83 0.038(2) 0.043(3) 0.035(2) 0.000(2) -0.0028(18) 0.006(2) C84 0.040(2) 0.028(2) 0.039(2) 0.0016(19) 0.0121(18) 0.0030(19) C85 0.048(2) 0.031(2) 0.042(3) 0.014(2) 0.0094(19) 0.010(2) C86 0.042(2) 0.038(2) 0.027(2) 0.0063(18) 0.0010(17) 0.0092(19) C87 0.032(2) 0.034(2) 0.022(2) 0.0096(17) -0.0007(15) 0.0077(17) C88 0.030(2) 0.039(2) 0.028(2) 0.0041(18) -0.0005(16) 0.0091(18) C89 0.035(2) 0.039(2) 0.046(3) 0.018(2) -0.0038(19) 0.001(2) C90 0.025(2) 0.066(3) 0.050(3) 0.030(2) 0.0091(19) 0.011(2) C91 0.034(2) 0.057(3) 0.043(3) 0.016(2) 0.0111(18) 0.021(2) C92 0.037(2) 0.033(2) 0.030(2) 0.0085(18) 0.0042(17) 0.0131(18) C93 0.0260(19) 0.032(2) 0.028(2) 0.0116(17) 0.0085(15) 0.0107(16) C94 0.041(2) 0.034(2) 0.032(2) 0.0091(18) -0.0012(17) 0.0137(18) C95 0.057(3) 0.045(3) 0.032(2) 0.018(2) 0.0026(19) 0.018(2) C96 0.043(2) 0.033(2) 0.046(3) 0.019(2) 0.0112(19) 0.0155(19) C97 0.038(2) 0.030(2) 0.034(2) 0.0053(18) 0.0060(17) 0.0067(18) C98 0.033(2) 0.031(2) 0.032(2) 0.0104(18) 0.0059(16) 0.0099(17) C99 0.042(2) 0.034(2) 0.034(2) 0.0089(19) 0.0077(18) 0.010(2) C100 0.081(4) 0.044(3) 0.078(4) 0.023(3) 0.017(3) -0.005(3) B1 0.038(3) 0.047(3) 0.034(3) 0.013(2) 0.009(2) 0.023(2) B2 0.039(3) 0.058(3) 0.034(3) 0.015(2) 0.011(2) 0.020(3) C200 0.085(19) 0.17(2) 0.11(2) 0.084(17) 0.050(15) 0.088(17) C201 0.073(12) 0.040(8) 0.034(7) 0.010(6) -0.015(7) 0.017(8) N8 0.051(7) 0.067(7) 0.205(16) 0.074(9) -0.003(7) 0.008(6) C203 0.055(14) 0.026(8) 0.049(11) 0.003(7) -0.013(9) -0.006(8) C202 0.049(8) 0.060(10) 0.050(9) 0.036(8) 0.003(8) 0.003(8) N9 0.072(7) 0.088(8) 0.099(9) 0.061(7) -0.003(7) 0.000(7) C101 0.051(3) 0.061(3) 0.068(3) 0.011(2) 0.002(2) 0.013(2) C102 0.051(3) 0.061(3) 0.068(3) 0.011(2) 0.002(2) 0.013(2) N7 0.051(3) 0.061(3) 0.068(3) 0.011(2) 0.002(2) 0.013(2) C104 0.061(7) 0.044(6) 0.054(7) 0.012(5) -0.017(5) 0.007(5) N7A 0.061(7) 0.044(6) 0.054(7) 0.012(5) -0.017(5) 0.007(5) C103 0.061(7) 0.044(6) 0.054(7) 0.012(5) -0.017(5) 0.007(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N3 1.920(3) . ? Fe1 P1 2.2019(12) . ? Fe1 P4 2.2028(13) . ? Fe1 P3 2.2079(12) . ? Fe1 P2 2.2191(13) . ? Fe1 H1FE 1.4135 . ? Fe2 N6 1.917(3) . ? Fe2 P8 2.1879(13) . ? Fe2 P5 2.1937(13) . ? Fe2 P6 2.2039(13) . ? Fe2 P7 2.2123(13) . ? Fe2 H2FE 1.3889 . ? P1 N1 1.692(3) . ? P1 C1 1.824(4) . ? P1 C7 1.832(3) . ? P1 P2 2.5953(15) . ? P2 N1 1.687(3) . ? P2 C13 1.826(4) . ? P2 C19 1.829(4) . ? P3 N2 1.692(3) . ? P3 C31 1.813(4) . ? P3 C25 1.820(4) . ? P3 P4 2.5741(15) . ? P4 N2 1.686(3) . ? P4 C43 1.818(4) . ? P4 C37 1.823(3) . ? P5 N4 1.701(3) . ? P5 C57 1.808(4) . ? P5 C51 1.818(4) . ? P5 P6 2.5791(15) . ? P6 N4 1.679(3) . ? P6 C63 1.823(4) . ? P6 C69 1.825(4) . ? P7 N5 1.680(3) . ? P7 C75 1.815(4) . ? P7 C81 1.830(4) . ? P7 P8 2.5693(16) . ? P8 N5 1.684(3) . ? P8 C87 1.824(4) . ? P8 C93 1.829(4) . ? N1 H1N1 0.87(3) . ? N2 H1N2 0.91(3) . ? N3 C49 1.139(5) . ? N4 H1N4 0.81(3) . ? N5 H1N5 0.732(18) . ? N6 C99 1.142(4) . ? C1 C6 1.379(5) . ? C1 C2 1.399(5) . ? C2 C3 1.380(5) . ? C2 H2A 0.9500 . ? C3 C4 1.377(5) . ? C3 H3A 0.9500 . ? C4 C5 1.366(5) . ? C4 H4A 0.9500 . ? C5 C6 1.384(5) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.374(5) . ? C7 C12 1.401(5) . ? C8 C9 1.391(5) . ? C8 H8A 0.9500 . ? C9 C10 1.376(5) . ? C9 H9A 0.9500 . ? C10 C11 1.359(5) . ? C10 H10A 0.9500 . ? C11 C12 1.384(5) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.392(5) . ? C13 C18 1.404(5) . ? C14 C15 1.380(5) . ? C14 H14A 0.9500 . ? C15 C16 1.385(6) . ? C15 H15A 0.9500 . ? C16 C17 1.374(6) . ? C16 H16A 0.9500 . ? C17 C18 1.380(5) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C24 1.382(5) . ? C19 C20 1.407(5) . ? C20 C21 1.387(5) . ? C20 H20A 0.9500 . ? C21 C22 1.371(6) . ? C21 H21A 0.9500 . ? C22 C23 1.389(6) . ? C22 H22A 0.9500 . ? C23 C24 1.405(5) . ? C23 H23A 0.9500 . ? C24 H24A 0.9500 . ? C25 C26 1.380(5) . ? C25 C30 1.399(5) . ? C26 C27 1.395(5) . ? C26 H26A 0.9500 . ? C27 C28 1.379(5) . ? C27 H27A 0.9500 . ? C28 C29 1.387(5) . ? C28 H28A 0.9500 . ? C29 C30 1.382(5) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.399(5) . ? C31 C36 1.413(5) . ? C32 C33 1.378(5) . ? C32 H32A 0.9500 . ? C33 C34 1.389(6) . ? C33 H33A 0.9500 . ? C34 C35 1.389(6) . ? C34 H34A 0.9500 . ? C35 C36 1.373(5) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C42 1.382(5) . ? C37 C38 1.395(5) . ? C38 C39 1.390(5) . ? C38 H38A 0.9500 . ? C39 C40 1.376(5) . ? C39 H39A 0.9500 . ? C40 C41 1.377(5) . ? C40 H40A 0.9500 . ? C41 C42 1.396(5) . ? C41 H41A 0.9500 . ? C42 H42A 0.9500 . ? C43 C48 1.371(5) . ? C43 C44 1.385(5) . ? C44 C45 1.368(6) . ? C44 H44A 0.9500 . ? C45 C46 1.371(6) . ? C45 H45A 0.9500 . ? C46 C47 1.378(6) . ? C46 H46A 0.9500 . ? C47 C48 1.383(6) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? C49 C50 1.463(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.396(6) . ? C51 C56 1.401(6) . ? C52 C53 1.384(7) . ? C52 H52A 0.9500 . ? C53 C54 1.362(9) . ? C53 H53A 0.9500 . ? C54 C55 1.381(8) . ? C54 H54A 0.9500 . ? C55 C56 1.396(7) . ? C55 H55A 0.9500 . ? C56 H56A 0.9500 . ? C57 C62 1.397(5) . ? C57 C58 1.397(5) . ? C58 C59 1.370(5) . ? C58 H58A 0.9500 . ? C59 C60 1.388(6) . ? C59 H59A 0.9500 . ? C60 C61 1.380(6) . ? C60 H60A 0.9500 . ? C61 C62 1.387(5) . ? C61 H61A 0.9500 . ? C62 H62A 0.9500 . ? C63 C64 1.376(5) . ? C63 C68 1.393(5) . ? C64 C65 1.394(6) . ? C64 H64A 0.9500 . ? C65 C66 1.377(5) . ? C65 H65A 0.9500 . ? C66 C67 1.378(5) . ? C66 H66A 0.9500 . ? C67 C68 1.383(5) . ? C67 H67A 0.9500 . ? C68 H68A 0.9500 . ? C69 C74 1.383(5) . ? C69 C70 1.396(5) . ? C70 C71 1.390(5) . ? C70 H70A 0.9500 . ? C71 C72 1.383(6) . ? C71 H71A 0.9500 . ? C72 C73 1.374(6) . ? C72 H72A 0.9500 . ? C73 C74 1.398(5) . ? C73 H73A 0.9500 . ? C74 H74A 0.9500 . ? C75 C76 1.386(5) . ? C75 C80 1.402(5) . ? C76 C77 1.403(5) . ? C76 H76A 0.9500 . ? C77 C78 1.372(6) . ? C77 H77A 0.9500 . ? C78 C79 1.377(5) . ? C78 H78A 0.9500 . ? C79 C80 1.384(5) . ? C79 H79A 0.9500 . ? C80 H80A 0.9500 . ? C81 C86 1.387(5) . ? C81 C82 1.392(5) . ? C82 C83 1.376(5) . ? C82 H82A 0.9500 . ? C83 C84 1.373(6) . ? C83 H83A 0.9500 . ? C84 C85 1.386(5) . ? C84 H84A 0.9500 . ? C85 C86 1.375(5) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C87 C88 1.382(5) . ? C87 C92 1.420(5) . ? C88 C89 1.388(5) . ? C88 H88A 0.9500 . ? C89 C90 1.378(6) . ? C89 H89A 0.9500 . ? C90 C91 1.372(6) . ? C90 H90A 0.9500 . ? C91 C92 1.383(5) . ? C91 H91A 0.9500 . ? C92 H92A 0.9500 . ? C93 C98 1.390(5) . ? C93 C94 1.392(5) . ? C94 C95 1.371(5) . ? C94 H94A 0.9500 . ? C95 C96 1.375(5) . ? C95 H95A 0.9500 . ? C96 C97 1.387(5) . ? C96 H96A 0.9500 . ? C97 C98 1.384(5) . ? C97 H97A 0.9500 . ? C98 H98A 0.9500 . ? C99 C100 1.461(6) . ? C100 H10B 0.9800 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? B1 H1B1 1.15(4) . ? B1 H2B1 1.24(4) . ? B1 H4B1 1.23(3) . ? B1 H3B1 1.19(3) . ? B2 H1B2 1.26(3) . ? B2 H2B2 1.12(3) . ? B2 H3B2 1.12(3) . ? B2 H4B2 1.22(3) . ? C200 C201 1.35(3) . ? C200 H20B 0.9800 . ? C200 H20C 0.9800 . ? C200 H20D 0.9800 . ? C201 N8 1.165(18) . ? C203 C202 1.47(2) . ? C203 H20E 0.9800 . ? C203 H20F 0.9800 . ? C203 H20G 0.9800 . ? C202 N9 1.112(15) . ? C101 N7 1.150(11) . ? C101 C102 1.406(14) . ? C102 H10E 0.9800 . ? C102 H10F 0.9800 . ? C102 H10G 0.9800 . ? C104 C103 1.67(3) . ? C104 H10H 0.9800 . ? C104 H10I 0.9800 . ? C104 H10J 0.9800 . ? N7A C103 1.02(2) . ? 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 N3 Fe1 P1 95.77(10) . . ? N3 Fe1 P4 94.83(10) . . ? P1 Fe1 P4 169.40(4) . . ? N3 Fe1 P3 96.42(10) . . ? P1 Fe1 P3 107.26(5) . . ? P4 Fe1 P3 71.41(5) . . ? N3 Fe1 P2 93.02(10) . . ? P1 Fe1 P2 71.89(5) . . ? P4 Fe1 P2 107.60(5) . . ? P3 Fe1 P2 170.55(4) . . ? N3 Fe1 H1FE 173.7 . . ? P1 Fe1 H1FE 80.6 . . ? P4 Fe1 H1FE 88.9 . . ? P3 Fe1 H1FE 89.6 . . ? P2 Fe1 H1FE 81.0 . . ? N6 Fe2 P8 100.01(10) . . ? N6 Fe2 P5 96.63(10) . . ? P8 Fe2 P5 163.36(4) . . ? N6 Fe2 P6 90.85(10) . . ? P8 Fe2 P6 107.24(5) . . ? P5 Fe2 P6 71.81(5) . . ? N6 Fe2 P7 91.27(10) . . ? P8 Fe2 P7 71.45(5) . . ? P5 Fe2 P7 108.86(5) . . ? P6 Fe2 P7 177.67(5) . . ? N6 Fe2 H2FE 166.0 . . ? P8 Fe2 H2FE 92.8 . . ? P5 Fe2 H2FE 70.6 . . ? P6 Fe2 H2FE 80.0 . . ? P7 Fe2 H2FE 98.1 . . ? N1 P1 C1 107.52(17) . . ? N1 P1 C7 105.87(15) . . ? C1 P1 C7 102.51(16) . . ? N1 P1 Fe1 94.12(12) . . ? C1 P1 Fe1 122.80(12) . . ? C7 P1 Fe1 121.73(12) . . ? C1 P1 P2 126.80(12) . . ? C7 P1 P2 123.61(12) . . ? Fe1 P1 P2 54.36(4) . . ? N1 P2 C13 105.29(16) . . ? N1 P2 C19 105.55(17) . . ? C13 P2 C19 103.91(17) . . ? N1 P2 Fe1 93.64(11) . . ? C13 P2 Fe1 124.94(13) . . ? C19 P2 Fe1 120.14(12) . . ? C13 P2 P1 125.09(12) . . ? C19 P2 P1 123.10(13) . . ? Fe1 P2 P1 53.74(4) . . ? N2 P3 C31 105.75(17) . . ? N2 P3 C25 103.46(17) . . ? C31 P3 C25 104.80(17) . . ? N2 P3 Fe1 94.43(11) . . ? C31 P3 Fe1 119.47(13) . . ? C25 P3 Fe1 125.18(13) . . ? C31 P3 P4 123.85(13) . . ? C25 P3 P4 123.08(13) . . ? Fe1 P3 P4 54.20(4) . . ? N2 P4 C43 107.05(17) . . ? N2 P4 C37 106.73(16) . . ? C43 P4 C37 102.00(17) . . ? N2 P4 Fe1 94.78(12) . . ? C43 P4 Fe1 119.52(12) . . ? C37 P4 Fe1 124.76(13) . . ? C43 P4 P3 122.83(13) . . ? C37 P4 P3 128.46(12) . . ? Fe1 P4 P3 54.39(4) . . ? N4 P5 C57 105.68(16) . . ? N4 P5 C51 106.99(18) . . ? C57 P5 C51 102.76(19) . . ? N4 P5 Fe2 94.22(12) . . ? C57 P5 Fe2 126.06(14) . . ? C51 P5 Fe2 118.64(13) . . ? C57 P5 P6 127.75(13) . . ? C51 P5 P6 122.13(15) . . ? Fe2 P5 P6 54.28(4) . . ? N4 P6 C63 107.75(16) . . ? N4 P6 C69 107.25(17) . . ? C63 P6 C69 101.28(17) . . ? N4 P6 Fe2 94.49(12) . . ? C63 P6 Fe2 124.92(12) . . ? C69 P6 Fe2 119.48(12) . . ? C63 P6 P5 129.34(12) . . ? C69 P6 P5 123.15(13) . . ? Fe2 P6 P5 53.91(4) . . ? N5 P7 C75 106.80(16) . . ? N5 P7 C81 106.98(16) . . ? C75 P7 C81 102.60(16) . . ? N5 P7 Fe2 94.09(11) . . ? C75 P7 Fe2 124.51(12) . . ? C81 P7 Fe2 119.71(12) . . ? C75 P7 P8 125.94(13) . . ? C81 P7 P8 124.90(12) . . ? Fe2 P7 P8 53.83(4) . . ? N5 P8 C87 106.79(16) . . ? N5 P8 C93 105.44(16) . . ? C87 P8 C93 103.90(17) . . ? N5 P8 Fe2 94.84(12) . . ? C87 P8 Fe2 118.02(12) . . ? C93 P8 Fe2 125.31(12) . . ? C87 P8 P7 123.75(14) . . ? C93 P8 P7 125.30(12) . . ? Fe2 P8 P7 54.72(4) . . ? P2 N1 P1 100.34(17) . . ? P2 N1 H1N1 132(2) . . ? P1 N1 H1N1 127(2) . . ? P4 N2 P3 99.32(17) . . ? P4 N2 H1N2 125(2) . . ? P3 N2 H1N2 135(2) . . ? C49 N3 Fe1 177.4(3) . . ? P6 N4 P5 99.44(17) . . ? P6 N4 H1N4 127(3) . . ? P5 N4 H1N4 133(3) . . ? P7 N5 P8 99.58(16) . . ? P7 N5 H1N5 128.5(16) . . ? P8 N5 H1N5 131.9(16) . . ? C99 N6 Fe2 177.9(3) . . ? C6 C1 C2 118.6(3) . . ? C6 C1 P1 119.2(3) . . ? C2 C1 P1 122.2(3) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2A 119.8 . . ? C1 C2 H2A 119.8 . . ? C4 C3 C2 120.1(4) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4A 120.0 . . ? C3 C4 H4A 120.0 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 120.5(4) . . ? C1 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C8 C7 C12 118.6(3) . . ? C8 C7 P1 119.5(3) . . ? C12 C7 P1 121.9(3) . . ? C7 C8 C9 121.1(4) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 C8 119.3(4) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C12 120.7(4) . . ? C10 C11 H11A 119.6 . . ? C12 C11 H11A 119.6 . . ? C11 C12 C7 119.8(3) . . ? C11 C12 H12A 120.1 . . ? C7 C12 H12A 120.1 . . ? C14 C13 C18 118.7(4) . . ? C14 C13 P2 120.3(3) . . ? C18 C13 P2 120.6(3) . . ? C15 C14 C13 120.4(4) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C16 120.6(4) . . ? C14 C15 H15A 119.7 . . ? C16 C15 H15A 119.7 . . ? C17 C16 C15 119.4(4) . . ? C17 C16 H16A 120.3 . . ? C15 C16 H16A 120.3 . . ? C16 C17 C18 120.9(4) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C17 C18 C13 120.0(4) . . ? C17 C18 H18A 120.0 . . ? C13 C18 H18A 120.0 . . ? C24 C19 C20 119.2(4) . . ? C24 C19 P2 120.3(3) . . ? C20 C19 P2 120.1(3) . . ? C21 C20 C19 119.8(4) . . ? C21 C20 H20A 120.1 . . ? C19 C20 H20A 120.1 . . ? C22 C21 C20 120.9(4) . . ? C22 C21 H21A 119.5 . . ? C20 C21 H21A 119.5 . . ? C21 C22 C23 120.0(4) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C22 C23 C24 119.7(4) . . ? C22 C23 H23A 120.2 . . ? C24 C23 H23A 120.2 . . ? C19 C24 C23 120.4(4) . . ? C19 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C26 C25 C30 118.3(3) . . ? C26 C25 P3 120.9(3) . . ? C30 C25 P3 119.7(3) . . ? C25 C26 C27 121.1(4) . . ? C25 C26 H26A 119.4 . . ? C27 C26 H26A 119.4 . . ? C28 C27 C26 119.7(4) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C30 C29 C28 119.8(4) . . ? C30 C29 H29A 120.1 . . ? C28 C29 H29A 120.1 . . ? C29 C30 C25 120.9(4) . . ? C29 C30 H30A 119.5 . . ? C25 C30 H30A 119.5 . . ? C32 C31 C36 117.7(3) . . ? C32 C31 P3 119.8(3) . . ? C36 C31 P3 121.7(3) . . ? C33 C32 C31 121.7(4) . . ? C33 C32 H32A 119.2 . . ? C31 C32 H32A 119.2 . . ? C32 C33 C34 119.9(4) . . ? C32 C33 H33A 120.0 . . ? C34 C33 H33A 120.0 . . ? C35 C34 C33 119.1(4) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C36 C35 C34 121.4(4) . . ? C36 C35 H35A 119.3 . . ? C34 C35 H35A 119.3 . . ? C35 C36 C31 120.2(4) . . ? C35 C36 H36A 119.9 . . ? C31 C36 H36A 119.9 . . ? C42 C37 C38 119.8(3) . . ? C42 C37 P4 117.9(3) . . ? C38 C37 P4 122.1(3) . . ? C39 C38 C37 119.4(4) . . ? C39 C38 H38A 120.3 . . ? C37 C38 H38A 120.3 . . ? C40 C39 C38 120.3(4) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C39 C40 C41 120.8(3) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C40 C41 C42 119.2(4) . . ? C40 C41 H41A 120.4 . . ? C42 C41 H41A 120.4 . . ? C37 C42 C41 120.4(3) . . ? C37 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C48 C43 C44 117.4(4) . . ? C48 C43 P4 121.8(3) . . ? C44 C43 P4 120.5(3) . . ? C45 C44 C43 121.8(4) . . ? C45 C44 H44A 119.1 . . ? C43 C44 H44A 119.1 . . ? C44 C45 C46 120.4(4) . . ? C44 C45 H45A 119.8 . . ? C46 C45 H45A 119.8 . . ? C45 C46 C47 118.6(4) . . ? C45 C46 H46A 120.7 . . ? C47 C46 H46A 120.7 . . ? C46 C47 C48 120.6(4) . . ? C46 C47 H47A 119.7 . . ? C48 C47 H47A 119.7 . . ? C43 C48 C47 121.1(4) . . ? C43 C48 H48A 119.4 . . ? C47 C48 H48A 119.4 . . ? N3 C49 C50 178.4(5) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 C56 118.2(4) . . ? C52 C51 P5 121.0(3) . . ? C56 C51 P5 120.1(3) . . ? C53 C52 C51 120.7(5) . . ? C53 C52 H52A 119.6 . . ? C51 C52 H52A 119.6 . . ? C54 C53 C52 121.5(6) . . ? C54 C53 H53A 119.2 . . ? C52 C53 H53A 119.2 . . ? C53 C54 C55 118.5(6) . . ? C53 C54 H54A 120.7 . . ? C55 C54 H54A 120.7 . . ? C54 C55 C56 121.7(6) . . ? C54 C55 H55A 119.2 . . ? C56 C55 H55A 119.2 . . ? C55 C56 C51 119.4(5) . . ? C55 C56 H56A 120.3 . . ? C51 C56 H56A 120.3 . . ? C62 C57 C58 118.0(3) . . ? C62 C57 P5 122.1(3) . . ? C58 C57 P5 120.0(3) . . ? C59 C58 C57 121.4(4) . . ? C59 C58 H58A 119.3 . . ? C57 C58 H58A 119.3 . . ? C58 C59 C60 120.0(4) . . ? C58 C59 H59A 120.0 . . ? C60 C59 H59A 120.0 . . ? C61 C60 C59 119.8(4) . . ? C61 C60 H60A 120.1 . . ? C59 C60 H60A 120.1 . . ? C60 C61 C62 120.2(4) . . ? C60 C61 H61A 119.9 . . ? C62 C61 H61A 119.9 . . ? C61 C62 C57 120.6(4) . . ? C61 C62 H62A 119.7 . . ? C57 C62 H62A 119.7 . . ? C64 C63 C68 119.1(3) . . ? C64 C63 P6 121.4(3) . . ? C68 C63 P6 119.2(3) . . ? C63 C64 C65 120.2(4) . . ? C63 C64 H64A 119.9 . . ? C65 C64 H64A 119.9 . . ? C66 C65 C64 120.3(4) . . ? C66 C65 H65A 119.8 . . ? C64 C65 H65A 119.8 . . ? C65 C66 C67 119.7(4) . . ? C65 C66 H66A 120.1 . . ? C67 C66 H66A 120.1 . . ? C66 C67 C68 120.2(4) . . ? C66 C67 H67A 119.9 . . ? C68 C67 H67A 119.9 . . ? C67 C68 C63 120.5(3) . . ? C67 C68 H68A 119.8 . . ? C63 C68 H68A 119.8 . . ? C74 C69 C70 118.5(3) . . ? C74 C69 P6 122.2(3) . . ? C70 C69 P6 119.3(3) . . ? C71 C70 C69 120.6(4) . . ? C71 C70 H70A 119.7 . . ? C69 C70 H70A 119.7 . . ? C72 C71 C70 120.0(4) . . ? C72 C71 H71A 120.0 . . ? C70 C71 H71A 120.0 . . ? C73 C72 C71 120.1(4) . . ? C73 C72 H72A 120.0 . . ? C71 C72 H72A 120.0 . . ? C72 C73 C74 119.8(4) . . ? C72 C73 H73A 120.1 . . ? C74 C73 H73A 120.1 . . ? C69 C74 C73 121.0(4) . . ? C69 C74 H74A 119.5 . . ? C73 C74 H74A 119.5 . . ? C76 C75 C80 118.9(3) . . ? C76 C75 P7 121.4(3) . . ? C80 C75 P7 119.5(3) . . ? C75 C76 C77 119.8(4) . . ? C75 C76 H76A 120.1 . . ? C77 C76 H76A 120.1 . . ? C78 C77 C76 120.4(4) . . ? C78 C77 H77A 119.8 . . ? C76 C77 H77A 119.8 . . ? C77 C78 C79 120.2(4) . . ? C77 C78 H78A 119.9 . . ? C79 C78 H78A 119.9 . . ? C78 C79 C80 120.1(4) . . ? C78 C79 H79A 120.0 . . ? C80 C79 H79A 120.0 . . ? C79 C80 C75 120.5(4) . . ? C79 C80 H80A 119.7 . . ? C75 C80 H80A 119.7 . . ? C86 C81 C82 118.7(3) . . ? C86 C81 P7 119.6(3) . . ? C82 C81 P7 121.7(3) . . ? C83 C82 C81 120.3(4) . . ? C83 C82 H82A 119.8 . . ? C81 C82 H82A 119.8 . . ? C84 C83 C82 120.7(4) . . ? C84 C83 H83A 119.6 . . ? C82 C83 H83A 119.6 . . ? C83 C84 C85 119.3(4) . . ? C83 C84 H84A 120.4 . . ? C85 C84 H84A 120.4 . . ? C86 C85 C84 120.4(4) . . ? C86 C85 H85A 119.8 . . ? C84 C85 H85A 119.8 . . ? C85 C86 C81 120.5(3) . . ? C85 C86 H86A 119.7 . . ? C81 C86 H86A 119.7 . . ? C88 C87 C92 118.7(3) . . ? C88 C87 P8 120.2(3) . . ? C92 C87 P8 120.1(3) . . ? C87 C88 C89 120.7(4) . . ? C87 C88 H88A 119.7 . . ? C89 C88 H88A 119.7 . . ? C90 C89 C88 120.0(4) . . ? C90 C89 H89A 120.0 . . ? C88 C89 H89A 120.0 . . ? C91 C90 C89 120.4(4) . . ? C91 C90 H90A 119.8 . . ? C89 C90 H90A 119.8 . . ? C90 C91 C92 120.6(4) . . ? C90 C91 H91A 119.7 . . ? C92 C91 H91A 119.7 . . ? C91 C92 C87 119.6(4) . . ? C91 C92 H92A 120.2 . . ? C87 C92 H92A 120.2 . . ? C98 C93 C94 119.3(3) . . ? C98 C93 P8 121.6(3) . . ? C94 C93 P8 119.1(3) . . ? C95 C94 C93 120.3(4) . . ? C95 C94 H94A 119.9 . . ? C93 C94 H94A 119.9 . . ? C94 C95 C96 120.8(4) . . ? C94 C95 H95A 119.6 . . ? C96 C95 H95A 119.6 . . ? C95 C96 C97 119.5(4) . . ? C95 C96 H96A 120.3 . . ? C97 C96 H96A 120.3 . . ? C98 C97 C96 120.4(4) . . ? C98 C97 H97A 119.8 . . ? C96 C97 H97A 119.8 . . ? C97 C98 C93 119.8(4) . . ? C97 C98 H98A 120.1 . . ? C93 C98 H98A 120.1 . . ? N6 C99 C100 178.5(5) . . ? C99 C100 H10B 109.5 . . ? C99 C100 H10C 109.5 . . ? H10B C100 H10C 109.5 . . ? C99 C100 H10D 109.5 . . ? H10B C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? H1B1 B1 H2B1 109(2) . . ? H1B1 B1 H4B1 110(2) . . ? H2B1 B1 H4B1 107(2) . . ? H1B1 B1 H3B1 115(2) . . ? H2B1 B1 H3B1 110(2) . . ? H4B1 B1 H3B1 106(2) . . ? H1B2 B2 H2B2 110(2) . . ? H1B2 B2 H3B2 104(2) . . ? H2B2 B2 H3B2 117(2) . . ? H1B2 B2 H4B2 104(2) . . ? H2B2 B2 H4B2 108(2) . . ? H3B2 B2 H4B2 112(2) . . ? N8 C201 C200 179(2) . . ? C202 C203 H20E 109.5 . . ? C202 C203 H20F 109.5 . . ? H20E C203 H20F 109.5 . . ? C202 C203 H20G 109.5 . . ? H20E C203 H20G 109.5 . . ? H20F C203 H20G 109.5 . . ? N9 C202 C203 173(2) . . ? N7 C101 C102 179.5(10) . . ? C103 C104 H10H 109.5 . . ? C103 C104 H10I 109.5 . . ? H10H C104 H10I 109.5 . . ? C103 C104 H10J 109.5 . . ? H10H C104 H10J 109.5 . . ? H10I C104 H10J 109.5 . . ? N7A C103 C104 174(2) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 26.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.705 _refine_diff_density_min -0.384 _refine_diff_density_rms 0.058 _database_code_depnum_ccdc_archive 'CCDC 937586'