Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Solvent Dependent Reactivity: Solvent Activation vs. Solvent Coordination in Alkylphosphane Iron Complexes ; _publ_contact_author_name 'Andreas Grohmann' _publ_contact_author_email andreas.grohmann@chem.tu-berlin.de loop_ _publ_author_name S.W.Kohl F.W.Heinemann M.Hummert W.Bauer # Attachment '4-0.705MeOH(CCDC-612669).cif' data_ag0504 _database_code_depnum_ccdc_archive 'CCDC 612669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H41 D4 Fe N O P4, 2(B F4), 0.705(H2 O)' _chemical_formula_sum 'C22 H42.41 B2 D4 F8 Fe N O1.705 P4' _chemical_formula_weight 708.88 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) _symmetry_space_group_name_Hall P2ac2ab _chemical_absolute_configuration ad 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 10.8551(5) _cell_length_b 12.0360(10) _cell_length_c 23.698(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3096.2(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 156 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1465 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.758 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details 'SADABS, Bruker AXS, 2002' _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 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.40 \% and 399 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45185 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6329 _reflns_number_gt 5106 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The atoms of the minor component of the disordered BF4 molecule have been refined isotropically only. The same holds for the partially occupied solvent water molecule. No H atoms have been included for the partially occupied water molecule. ; _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^)+(0.0696P)^2^+2.3966P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 3561 Friedel pairs used in the refinement of Flack parameter ; _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 6329 _refine_ls_number_parameters 400 _refine_ls_number_restraints 40 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1287 _refine_ls_wR_factor_gt 0.1188 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.003 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 0.54580(5) 0.47969(5) 0.60357(2) 0.02810(16) Uani 1 1 d . . . P1 P 0.67533(10) 0.35263(10) 0.64220(5) 0.0364(3) Uani 1 1 d . . . P2 P 0.68301(12) 0.60786(11) 0.61917(5) 0.0374(3) Uani 1 1 d . . . P3 P 0.39525(12) 0.60571(10) 0.59083(4) 0.0355(3) Uani 1 1 d . . . P4 P 0.59418(12) 0.47074(12) 0.51326(5) 0.0438(3) Uani 1 1 d . A . N1 N 0.4701(3) 0.4675(3) 0.68309(13) 0.0247(7) Uani 1 1 d . . . O1 O 0.6122(4) 0.5942(4) 0.48753(14) 0.0672(12) Uani 1 1 d . . . C1 C 0.5319(4) 0.4874(3) 0.73195(17) 0.0287(9) Uani 1 1 d . . . C2 C 0.4719(4) 0.4757(4) 0.78360(17) 0.0338(10) Uani 1 1 d . . . H2A H 0.5156 0.4886 0.8177 0.041 Uiso 1 1 calc R . . C3 C 0.3503(4) 0.4460(4) 0.7854(2) 0.0410(12) Uani 1 1 d . . . H3A H 0.3088 0.4408 0.8206 0.049 Uiso 1 1 calc R . . C4 C 0.2893(4) 0.4238(4) 0.73661(19) 0.0385(11) Uani 1 1 d . . . H4A H 0.2057 0.4006 0.7377 0.046 Uiso 1 1 calc R . . C5 C 0.3486(4) 0.4351(4) 0.68539(18) 0.0312(10) Uani 1 1 d . . . C6 C 0.6690(4) 0.5164(4) 0.73016(17) 0.0343(9) Uani 1 1 d . . . C7 C 0.7423(4) 0.4182(4) 0.7054(2) 0.0413(12) Uani 1 1 d . . . H7A H 0.7511 0.3608 0.7350 0.050 Uiso 1 1 calc R . . H7B H 0.8261 0.4447 0.6958 0.050 Uiso 1 1 calc R . . C8 C 0.6898(4) 0.6244(4) 0.69580(17) 0.0341(10) Uani 1 1 d . . . H8A H 0.7715 0.6551 0.7059 0.041 Uiso 1 1 calc R . . H8B H 0.6269 0.6795 0.7072 0.041 Uiso 1 1 calc R . . C9 C 0.7212(4) 0.5398(4) 0.7898(2) 0.0417(11) Uani 1 1 d . . . H9A H 0.6769 0.6024 0.8068 0.063 Uiso 1 1 calc R . . H9B H 0.8090 0.5579 0.7870 0.063 Uiso 1 1 calc R . . H9C H 0.7108 0.4737 0.8135 0.063 Uiso 1 1 calc R . . C10 C 0.2566(4) 0.5205(4) 0.59905(19) 0.0412(10) Uani 1 1 d . . . H10A H 0.1941 0.5630 0.6205 0.049 Uiso 1 1 calc R . . H10B H 0.2219 0.5039 0.5613 0.049 Uiso 1 1 calc R . . C11 C 0.3639(4) 0.3341(4) 0.59367(19) 0.0386(11) Uani 1 1 d . . . H11A H 0.4467 0.3658 0.5901 0.058 Uiso 1 1 calc R . . H11B H 0.3270 0.3264 0.5561 0.058 Uiso 1 1 calc R . . H11C H 0.3692 0.2609 0.6116 0.058 Uiso 1 1 calc R . . C12 C 0.2836(4) 0.4111(4) 0.62987(18) 0.0329(10) Uani 1 1 d . . . C13 C 0.1610(4) 0.3491(5) 0.6379(2) 0.0476(12) Uani 1 1 d . . . H13A H 0.1040 0.3957 0.6595 0.071 Uiso 1 1 calc R . . H13B H 0.1758 0.2796 0.6584 0.071 Uiso 1 1 calc R . . H13C H 0.1251 0.3323 0.6010 0.071 Uiso 1 1 calc R . . C14 C 0.5966(5) 0.2318(4) 0.6723(2) 0.0421(11) Uani 1 1 d . . . H14A H 0.6538 0.1907 0.6966 0.063 Uiso 1 1 calc R . . H14B H 0.5679 0.1833 0.6418 0.063 Uiso 1 1 calc R . . H14C H 0.5259 0.2567 0.6947 0.063 Uiso 1 1 calc R . . C15 C 0.8078(5) 0.2827(6) 0.6106(3) 0.0673(19) Uani 1 1 d . . . H15A H 0.8532 0.2423 0.6399 0.101 Uiso 1 1 calc R . . H15B H 0.8621 0.3380 0.5932 0.101 Uiso 1 1 calc R . . H15C H 0.7793 0.2303 0.5818 0.101 Uiso 1 1 calc R . . C16 C 0.6663(6) 0.7499(4) 0.5938(2) 0.0549(15) Uani 1 1 d . . . H16A H 0.7352 0.7950 0.6077 0.082 Uiso 1 1 calc R . . H16B H 0.5886 0.7810 0.6077 0.082 Uiso 1 1 calc R . . H16C H 0.6664 0.7503 0.5525 0.082 Uiso 1 1 calc R . . C17 C 0.8416(5) 0.5857(5) 0.5968(2) 0.0568(15) Uani 1 1 d . . . H17A H 0.8944 0.6430 0.6135 0.085 Uiso 1 1 calc R . . H17B H 0.8464 0.5900 0.5556 0.085 Uiso 1 1 calc R . . H17C H 0.8692 0.5123 0.6094 0.085 Uiso 1 1 calc R . . C18 C 0.3743(5) 0.7105(4) 0.6461(2) 0.0458(12) Uani 1 1 d . . . H18A H 0.2867 0.7292 0.6492 0.069 Uiso 1 1 calc R . . H18B H 0.4213 0.7773 0.6364 0.069 Uiso 1 1 calc R . . H18C H 0.4037 0.6809 0.6822 0.069 Uiso 1 1 calc R . . C19 C 0.3652(6) 0.6868(5) 0.5277(2) 0.0587(16) Uani 1 1 d . . . H19A H 0.2851 0.7237 0.5311 0.088 Uiso 0.67(2) 1 calc PR A 1 H19B H 0.3644 0.6376 0.4947 0.088 Uiso 0.67(2) 1 calc PR A 1 H19C H 0.4299 0.7429 0.5230 0.088 Uiso 0.67(2) 1 calc PR A 1 H19D H 0.3436 0.6368 0.4965 0.088 Uiso 0.33(2) 1 calc PR A 2 H19E H 0.4390 0.7293 0.5176 0.088 Uiso 0.33(2) 1 calc PR A 2 H19F H 0.2967 0.7380 0.5347 0.088 Uiso 0.33(2) 1 calc PR A 2 C20 C 0.7267(6) 0.3950(7) 0.4892(3) 0.078(2) Uani 1 1 d . . . H20A H 0.7465 0.4173 0.4505 0.117 Uiso 0.67(2) 1 calc PR A 1 H20B H 0.7091 0.3152 0.4901 0.117 Uiso 0.67(2) 1 calc PR A 1 H20C H 0.7970 0.4112 0.5138 0.117 Uiso 0.67(2) 1 calc PR A 1 H20D H 0.7124 0.3687 0.4506 0.117 Uiso 0.33(2) 1 calc PR A 2 H20E H 0.7410 0.3312 0.5140 0.117 Uiso 0.33(2) 1 calc PR A 2 H20F H 0.7990 0.4437 0.4898 0.117 Uiso 0.33(2) 1 calc PR A 2 C21 C 0.4785(5) 0.4047(5) 0.46948(19) 0.0472(13) Uani 1 1 d . . . H21A H 0.5088 0.3996 0.4306 0.071 Uiso 1 1 calc R A . H21B H 0.4027 0.4488 0.4703 0.071 Uiso 1 1 calc R . . H21C H 0.4616 0.3299 0.4839 0.071 Uiso 1 1 calc R . . C22 C 0.6058(18) 0.6261(12) 0.4259(4) 0.082(5) Uani 0.67(2) 1 d PU A 1 H22A H 0.6215 0.7059 0.4219 0.123 Uiso 0.67(2) 1 calc PR A 1 H22B H 0.5237 0.6087 0.4111 0.123 Uiso 0.67(2) 1 calc PR A 1 H22C H 0.6680 0.5844 0.4047 0.123 Uiso 0.67(2) 1 calc PR A 1 C22' C 0.684(4) 0.584(3) 0.4340(10) 0.084(6) Uani 0.33(2) 1 d PU A 2 H22D H 0.7402 0.6474 0.4303 0.125 Uiso 0.33(2) 1 calc PR A 2 H22E H 0.6276 0.5825 0.4018 0.125 Uiso 0.33(2) 1 calc PR A 2 H22F H 0.7322 0.5149 0.4347 0.125 Uiso 0.33(2) 1 calc PR A 2 B1 B 0.0622(5) 0.4630(5) 0.4578(2) 0.0448(14) Uani 1 1 d D . . F11 F 0.1792(3) 0.4808(3) 0.43986(17) 0.0771(11) Uani 1 1 d D . . F12 F -0.0202(3) 0.4779(4) 0.41555(12) 0.0816(12) Uani 1 1 d D . . F13 F 0.0352(3) 0.5336(4) 0.50048(16) 0.1012(16) Uani 1 1 d D . . F14 F 0.0533(5) 0.3558(4) 0.4769(2) 0.1042(15) Uani 1 1 d D . . B2 B 0.5499(7) 0.8261(8) 0.2741(4) 0.065(3) Uani 0.706(8) 1 d PD B 1 F21 F 0.4711(4) 0.7705(4) 0.2429(2) 0.0708(19) Uani 0.706(8) 1 d PD B 1 F22 F 0.5096(4) 0.9335(4) 0.2869(2) 0.0586(16) Uani 0.706(8) 1 d PD B 1 F23 F 0.6655(4) 0.8374(4) 0.2493(2) 0.0614(16) Uani 0.706(8) 1 d PD B 1 F24 F 0.5722(8) 0.7668(7) 0.3250(3) 0.118(3) Uani 0.706(8) 1 d PD B 1 B2' B 0.520(3) 0.799(3) 0.2726(13) 0.212(10) Uiso 0.294(8) 1 d PDU B 2 F21' F 0.449(3) 0.721(2) 0.2980(13) 0.208(11) Uiso 0.294(8) 1 d PDU B 2 F22' F 0.497(3) 0.902(3) 0.2987(15) 0.200(12) Uiso 0.294(8) 1 d PDU B 2 F23' F 0.536(3) 0.828(3) 0.2168(11) 0.227(11) Uiso 0.294(8) 1 d PDU B 2 F24' F 0.646(3) 0.777(3) 0.2872(14) 0.210(11) Uiso 0.294(8) 1 d PDU B 2 O2 O 0.4351(19) 0.5391(16) 0.3326(8) 0.255(8) Uiso 0.706(8) 1 d P B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0279(3) 0.0293(3) 0.0271(3) -0.0062(3) 0.0027(2) -0.0008(3) P1 0.0258(5) 0.0367(7) 0.0467(7) -0.0162(5) -0.0040(5) 0.0065(5) P2 0.0407(6) 0.0396(7) 0.0320(6) -0.0106(5) 0.0089(5) -0.0131(5) P3 0.0470(7) 0.0343(6) 0.0251(5) 0.0008(5) -0.0033(5) 0.0077(5) P4 0.0456(7) 0.0519(8) 0.0339(6) -0.0182(6) 0.0116(5) -0.0138(6) N1 0.0259(17) 0.0204(16) 0.0278(16) 0.0013(14) 0.0018(13) 0.0013(15) O1 0.097(3) 0.072(3) 0.0325(18) -0.0100(19) 0.014(2) -0.040(3) C1 0.033(2) 0.021(2) 0.031(2) 0.0013(17) -0.0065(17) 0.0054(18) C2 0.046(3) 0.031(2) 0.024(2) 0.0058(19) -0.0057(18) 0.005(2) C3 0.044(3) 0.045(3) 0.033(2) 0.011(2) 0.005(2) 0.000(2) C4 0.034(2) 0.044(3) 0.038(3) 0.004(2) 0.0023(19) -0.005(2) C5 0.029(2) 0.030(2) 0.035(2) -0.0039(18) -0.0002(18) 0.0013(17) C6 0.032(2) 0.037(2) 0.034(2) -0.005(2) -0.0069(18) 0.006(2) C7 0.026(2) 0.045(3) 0.053(3) -0.015(2) -0.013(2) 0.006(2) C8 0.039(2) 0.032(2) 0.032(2) -0.0093(18) 0.0035(18) -0.007(2) C9 0.039(2) 0.043(3) 0.044(3) -0.004(2) -0.011(2) 0.000(2) C10 0.033(2) 0.057(3) 0.033(2) -0.008(2) -0.0090(19) 0.008(2) C11 0.028(2) 0.047(3) 0.041(3) -0.011(2) 0.0000(19) -0.0060(19) C12 0.027(2) 0.036(3) 0.035(2) -0.005(2) -0.0002(17) -0.0007(18) C13 0.031(2) 0.063(3) 0.049(3) -0.012(3) 0.000(2) -0.013(2) C14 0.043(3) 0.028(2) 0.055(3) -0.006(2) -0.011(2) 0.006(2) C15 0.036(3) 0.077(4) 0.089(4) -0.053(4) -0.001(3) 0.021(3) C16 0.089(4) 0.041(3) 0.035(3) -0.002(2) 0.016(3) -0.028(3) C17 0.046(3) 0.072(4) 0.052(3) -0.030(3) 0.013(3) -0.029(3) C18 0.061(3) 0.040(3) 0.036(3) -0.001(2) -0.004(2) 0.014(2) C19 0.090(4) 0.056(4) 0.030(3) 0.005(2) -0.009(3) 0.019(3) C20 0.049(3) 0.132(6) 0.054(4) -0.046(4) 0.017(3) -0.006(4) C21 0.051(3) 0.059(3) 0.033(2) -0.011(2) 0.002(2) -0.016(3) C22 0.134(13) 0.085(9) 0.028(4) 0.001(5) 0.009(7) -0.035(9) C22' 0.131(16) 0.086(12) 0.034(8) -0.008(8) 0.010(10) -0.036(11) B1 0.036(3) 0.064(4) 0.034(3) -0.005(3) -0.005(2) 0.003(3) F11 0.0449(17) 0.066(2) 0.121(3) -0.026(2) 0.0246(19) -0.0063(18) F12 0.070(2) 0.144(4) 0.0309(15) 0.003(2) -0.0048(14) 0.022(2) F13 0.062(2) 0.170(4) 0.071(2) -0.065(3) -0.0147(18) 0.040(3) F14 0.096(3) 0.089(3) 0.128(4) 0.052(3) -0.004(3) -0.012(3) B2 0.025(4) 0.091(8) 0.080(7) -0.040(6) -0.003(4) 0.019(5) F21 0.058(3) 0.066(3) 0.089(4) -0.028(3) -0.039(3) -0.006(2) F22 0.025(2) 0.073(3) 0.078(3) -0.040(3) 0.008(2) 0.0064(19) F23 0.039(2) 0.060(3) 0.086(4) -0.003(3) 0.026(2) 0.009(2) F24 0.127(6) 0.155(7) 0.071(4) 0.036(4) -0.037(4) -0.044(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 N1 2.061(3) . ? Fe1 P2 2.1760(13) . ? Fe1 P4 2.2062(13) . ? Fe1 P3 2.2500(13) . ? Fe1 P1 2.2702(14) . ? Fe1 C11 2.651(5) . ? P1 C14 1.832(5) . ? P1 C15 1.827(5) . ? P1 C7 1.842(4) . ? P2 C17 1.820(5) . ? P2 C16 1.821(5) . ? P2 C8 1.828(4) . ? P3 C19 1.817(5) . ? P3 C18 1.832(5) . ? P3 C10 1.832(5) . ? P4 O1 1.618(4) . ? P4 C21 1.813(5) . ? P4 C20 1.796(6) . ? N1 C1 1.360(5) . ? N1 C5 1.376(5) . ? O1 C22' 1.50(3) . ? O1 C22 1.512(11) . ? C1 C2 1.394(6) . ? C1 C6 1.529(6) . ? C2 C3 1.369(7) . ? C2 H2A 0.9500 . ? C3 C4 1.358(7) . ? C3 H3A 0.9500 . ? C4 C5 1.381(6) . ? C4 H4A 0.9500 . ? C5 C12 1.521(6) . ? C6 C7 1.542(6) . ? C6 C8 1.550(6) . ? C6 C9 1.550(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.535(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.534(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.538(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 H19D 0.9800 . ? C19 H19E 0.9800 . ? C19 H19F 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 H20D 0.9800 . ? C20 H20E 0.9800 . ? C20 H20F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? B1 F13 1.354(7) . ? B1 F12 1.355(6) . ? B1 F11 1.356(6) . ? B1 F14 1.370(7) . ? B2 F21 1.314(10) . ? B2 F23 1.392(10) . ? B2 F22 1.398(10) . ? B2 F24 1.423(11) . ? B2' F21' 1.353(17) . ? B2' F23' 1.379(17) . ? B2' F22' 1.408(18) . ? B2' F24' 1.433(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 P2 99.68(10) . . ? N1 Fe1 P4 168.05(10) . . ? P2 Fe1 P4 92.09(5) . . ? N1 Fe1 P3 83.17(9) . . ? P2 Fe1 P3 92.41(5) . . ? P4 Fe1 P3 94.34(5) . . ? N1 Fe1 P1 80.22(10) . . ? P2 Fe1 P1 89.15(5) . . ? P4 Fe1 P1 102.17(5) . . ? P3 Fe1 P1 163.35(5) . . ? N1 Fe1 C11 74.73(14) . . ? P2 Fe1 C11 173.57(10) . . ? P4 Fe1 C11 93.39(11) . . ? P3 Fe1 C11 83.84(11) . . ? P1 Fe1 C11 92.97(12) . . ? C14 P1 C15 99.3(3) . . ? C14 P1 C7 102.0(2) . . ? C15 P1 C7 102.7(2) . . ? C14 P1 Fe1 113.77(17) . . ? C15 P1 Fe1 129.3(3) . . ? C7 P1 Fe1 106.47(16) . . ? C17 P2 C16 97.8(3) . . ? C17 P2 C8 105.5(2) . . ? C16 P2 C8 103.3(2) . . ? C17 P2 Fe1 119.60(18) . . ? C16 P2 Fe1 122.8(2) . . ? C8 P2 Fe1 105.87(15) . . ? C19 P3 C18 101.4(2) . . ? C19 P3 C10 103.9(3) . . ? C18 P3 C10 102.0(2) . . ? C19 P3 Fe1 127.1(2) . . ? C18 P3 Fe1 117.27(17) . . ? C10 P3 Fe1 101.85(16) . . ? O1 P4 C21 105.7(2) . . ? O1 P4 C20 104.5(3) . . ? C21 P4 C20 98.6(3) . . ? O1 P4 Fe1 110.45(14) . . ? C21 P4 Fe1 114.32(17) . . ? C20 P4 Fe1 121.6(2) . . ? C1 N1 C5 119.3(3) . . ? C1 N1 Fe1 124.7(3) . . ? C5 N1 Fe1 116.0(3) . . ? C22' O1 P4 107.8(13) . . ? P4 O1 C22 126.3(6) . . ? N1 C1 C2 120.0(4) . . ? N1 C1 C6 119.8(4) . . ? C2 C1 C6 120.1(4) . . ? C3 C2 C1 120.3(4) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C3 C4 C5 120.1(4) . . ? C3 C4 H4A 119.9 . . ? C5 C4 H4A 119.9 . . ? N1 C5 C4 120.6(4) . . ? N1 C5 C12 117.6(4) . . ? C4 C5 C12 121.7(4) . . ? C1 C6 C7 109.7(4) . . ? C1 C6 C8 110.4(3) . . ? C7 C6 C8 111.5(4) . . ? C1 C6 C9 111.9(4) . . ? C7 C6 C9 107.3(3) . . ? C8 C6 C9 105.9(4) . . ? C6 C7 P1 115.8(3) . . ? C6 C7 H7A 108.3 . . ? P1 C7 H7A 108.3 . . ? C6 C7 H7B 108.3 . . ? P1 C7 H7B 108.3 . . ? H7A C7 H7B 107.4 . . ? C6 C8 P2 115.1(3) . . ? C6 C8 H8A 108.5 . . ? P2 C8 H8A 108.5 . . ? C6 C8 H8B 108.5 . . ? P2 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 P3 111.9(3) . . ? C12 C10 H10A 109.2 . . ? P3 C10 H10A 109.2 . . ? C12 C10 H10B 109.2 . . ? P3 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? C12 C11 Fe1 88.5(3) . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? Fe1 C11 H11B 116.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? Fe1 C11 H11C 120.8 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 C10 109.7(4) . . ? C5 C12 C11 109.6(4) . . ? C10 C12 C11 111.2(4) . . ? C5 C12 C13 112.7(4) . . ? C10 C12 C13 108.1(4) . . ? C11 C12 C13 105.5(4) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P3 C18 H18A 109.5 . . ? P3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P3 C19 H19A 109.5 . . ? P3 C19 H19B 109.5 . . ? P3 C19 H19C 109.5 . . ? P3 C19 H19D 109.5 . . ? P3 C19 H19E 109.5 . . ? H19D C19 H19E 109.5 . . ? P3 C19 H19F 109.5 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? P4 C20 H20A 109.5 . . ? P4 C20 H20B 109.5 . . ? P4 C20 H20C 109.5 . . ? P4 C20 H20D 109.5 . . ? P4 C20 H20E 109.5 . . ? H20D C20 H20E 109.5 . . ? P4 C20 H20F 109.5 . . ? H20D C20 H20F 109.5 . . ? H20E C20 H20F 109.5 . . ? P4 C21 H21A 109.5 . . ? P4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? O1 C22 H22C 109.5 . . ? O1 C22' H22D 109.5 . . ? O1 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? O1 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? F13 B1 F12 109.0(5) . . ? F13 B1 F11 109.7(5) . . ? F12 B1 F11 111.5(5) . . ? F13 B1 F14 109.2(5) . . ? F12 B1 F14 108.8(5) . . ? F11 B1 F14 108.6(5) . . ? F21 B2 F23 113.5(7) . . ? F21 B2 F22 112.9(6) . . ? F23 B2 F22 106.5(7) . . ? F21 B2 F24 109.4(8) . . ? F23 B2 F24 104.8(6) . . ? F22 B2 F24 109.4(7) . . ? F21' B2' F23' 132(3) . . ? F21' B2' F22' 108(2) . . ? F23' B2' F22' 103(2) . . ? F21' B2' F24' 108(2) . . ? F23' B2' F24' 99(2) . . ? F22' B2' F24' 103(2) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.810 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.080 data_ag0604 _database_code_depnum_ccdc_archive 'CCDC 612670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H44 Fe N2 P4, 2(C F3 O3 S)' _chemical_formula_sum 'C25 H44 F6 Fe N2 O6 P4 S2' _chemical_formula_weight 826.47 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P2(1)/n _symmetry_space_group_name_Hall -P2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.305(1) _cell_length_b 19.793(2) _cell_length_c 25.205(2) _cell_angle_alpha 90.00 _cell_angle_beta 94.336(5) _cell_angle_gamma 90.00 _cell_volume 7116.1(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 624 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description irregular _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3424 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 0.850 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _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 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \f- and \w-rotations with 1.30 \% and 234 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73706 _diffrn_reflns_av_R_equivalents 0.0288 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.10 _reflns_number_total 15335 _reflns_number_gt 11879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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. All anions are subjected to disorder. ; _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^)+(0.0333P)^2^+10.1898P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15335 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 220 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.005 _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 0.77083(2) 0.619363(16) 0.089425(11) 0.00995(7) Uani 1 1 d . . . P1 P 0.89294(4) 0.68437(3) 0.07208(2) 0.01358(12) Uani 1 1 d . . . P2 P 0.69084(4) 0.71250(3) 0.10887(2) 0.01643(13) Uani 1 1 d . . . P3 P 0.64223(4) 0.55553(3) 0.08489(2) 0.01730(13) Uani 1 1 d . . . P4 P 0.85959(4) 0.52625(3) 0.09686(2) 0.01229(12) Uani 1 1 d . . . N1 N 0.79601(12) 0.61711(9) 0.17254(7) 0.0118(4) Uani 1 1 d . . . N2 N 0.75056(13) 0.61763(10) 0.01302(7) 0.0145(4) Uani 1 1 d . . . C1 C 0.83507(15) 0.67209(11) 0.20027(8) 0.0133(4) Uani 1 1 d . . . C2 C 0.85174(17) 0.67003(12) 0.25557(9) 0.0182(5) Uani 1 1 d . . . H2A H 0.8786 0.7082 0.2738 0.022 Uiso 1 1 calc R . . C3 C 0.83007(17) 0.61394(13) 0.28388(9) 0.0207(5) Uani 1 1 d . . . H3A H 0.8409 0.6130 0.3215 0.025 Uiso 1 1 calc R . . C4 C 0.79238(17) 0.55899(13) 0.25682(9) 0.0185(5) Uani 1 1 d . . . H4A H 0.7777 0.5195 0.2760 0.022 Uiso 1 1 calc R . . C5 C 0.77539(15) 0.56020(11) 0.20179(8) 0.0129(4) Uani 1 1 d . . . C6 C 0.86156(17) 0.73775(12) 0.17187(9) 0.0181(5) Uani 1 1 d . . . C7 C 0.93959(17) 0.72355(12) 0.13354(9) 0.0191(5) Uani 1 1 d . . . H7A H 0.9875 0.6935 0.1514 0.023 Uiso 1 1 calc R . . H7B H 0.9706 0.7666 0.1253 0.023 Uiso 1 1 calc R . . C8 C 0.77409(18) 0.77185(12) 0.14294(9) 0.0214(5) Uani 1 1 d . . . H8A H 0.7953 0.8043 0.1165 0.026 Uiso 1 1 calc R . . H8B H 0.7410 0.7979 0.1693 0.026 Uiso 1 1 calc R . . C9 C 0.9035(2) 0.79112(13) 0.21144(10) 0.0282(6) Uani 1 1 d . . . H9A H 0.9617 0.7737 0.2295 0.042 Uiso 1 1 calc R . . H9B H 0.8585 0.8010 0.2379 0.042 Uiso 1 1 calc R . . H9C H 0.9169 0.8326 0.1921 0.042 Uiso 1 1 calc R . . C10 C 0.73274(17) 0.49553(12) 0.17522(9) 0.0174(5) Uani 1 1 d . . . C11 C 0.63493(17) 0.51184(13) 0.14757(9) 0.0205(5) Uani 1 1 d . . . H11A H 0.5997 0.5402 0.1715 0.025 Uiso 1 1 calc R . . H11B H 0.5997 0.4692 0.1412 0.025 Uiso 1 1 calc R . . C12 C 0.80020(17) 0.46411(12) 0.13630(9) 0.0184(5) Uani 1 1 d . . . H12A H 0.7639 0.4331 0.1118 0.022 Uiso 1 1 calc R . . H12B H 0.8482 0.4370 0.1571 0.022 Uiso 1 1 calc R . . C13 C 0.7158(2) 0.43963(13) 0.21615(10) 0.0262(6) Uani 1 1 d . . . H13A H 0.6700 0.4554 0.2404 0.039 Uiso 1 1 calc R . . H13B H 0.7750 0.4289 0.2366 0.039 Uiso 1 1 calc R . . H13C H 0.6918 0.3991 0.1975 0.039 Uiso 1 1 calc R . . C14 C 0.99400(17) 0.65358(13) 0.03934(10) 0.0221(5) Uani 1 1 d . . . H14A H 1.0380 0.6909 0.0352 0.033 Uiso 1 1 calc R . . H14B H 0.9732 0.6355 0.0042 0.033 Uiso 1 1 calc R . . H14C H 1.0252 0.6178 0.0610 0.033 Uiso 1 1 calc R . . C15 C 0.86585(19) 0.75461(13) 0.02599(9) 0.0232(5) Uani 1 1 d . . . H15A H 0.9203 0.7846 0.0258 0.035 Uiso 1 1 calc R . . H15B H 0.8121 0.7799 0.0375 0.035 Uiso 1 1 calc R . . H15C H 0.8507 0.7368 -0.0099 0.035 Uiso 1 1 calc R . . C16 C 0.60830(19) 0.70662(14) 0.16138(10) 0.0267(6) Uani 1 1 d . . . H16A H 0.5879 0.7521 0.1707 0.040 Uiso 1 1 calc R . . H16B H 0.6394 0.6849 0.1929 0.040 Uiso 1 1 calc R . . H16C H 0.5537 0.6798 0.1484 0.040 Uiso 1 1 calc R . . C17 C 0.62339(18) 0.76173(14) 0.05817(10) 0.0261(6) Uani 1 1 d . . . H17A H 0.6176 0.8084 0.0705 0.039 Uiso 1 1 calc R . . H17B H 0.5608 0.7419 0.0516 0.039 Uiso 1 1 calc R . . H17C H 0.6555 0.7613 0.0252 0.039 Uiso 1 1 calc R . . C18 C 0.52474(18) 0.58888(16) 0.06812(11) 0.0324(7) Uani 1 1 d . . . H18A H 0.4794 0.5517 0.0662 0.049 Uiso 1 1 calc R . . H18B H 0.5231 0.6118 0.0336 0.049 Uiso 1 1 calc R . . H18C H 0.5086 0.6211 0.0955 0.049 Uiso 1 1 calc R . . C19 C 0.63776(19) 0.48844(14) 0.03508(10) 0.0279(6) Uani 1 1 d . . . H19A H 0.5892 0.4557 0.0428 0.042 Uiso 1 1 calc R . . H19B H 0.6987 0.4657 0.0360 0.042 Uiso 1 1 calc R . . H19C H 0.6230 0.5079 -0.0003 0.042 Uiso 1 1 calc R . . C20 C 0.97036(16) 0.53281(13) 0.13825(9) 0.0188(5) Uani 1 1 d . . . H20A H 0.9973 0.4876 0.1440 0.028 Uiso 1 1 calc R . . H20B H 0.9587 0.5531 0.1726 0.028 Uiso 1 1 calc R . . H20C H 1.0143 0.5612 0.1202 0.028 Uiso 1 1 calc R . . C21 C 0.89583(19) 0.48010(13) 0.03961(10) 0.0232(5) Uani 1 1 d . . . H21A H 0.9307 0.4396 0.0517 0.035 Uiso 1 1 calc R . . H21B H 0.9360 0.5090 0.0194 0.035 Uiso 1 1 calc R . . H21C H 0.8403 0.4668 0.0168 0.035 Uiso 1 1 calc R . . C22 C 0.74060(16) 0.61142(12) -0.03228(9) 0.0178(5) Uani 1 1 d . . . C23 C 0.7275(2) 0.60043(15) -0.08973(9) 0.0286(6) Uani 1 1 d . . . H23A H 0.7568 0.5576 -0.0987 0.043 Uiso 1 1 calc R . . H23B H 0.7567 0.6375 -0.1083 0.043 Uiso 1 1 calc R . . H23C H 0.6604 0.5988 -0.1007 0.043 Uiso 1 1 calc R . . Fe2 Fe 0.22729(2) 0.498691(15) 0.355325(12) 0.01108(7) Uani 1 1 d . . . P5 P 0.19149(4) 0.57073(3) 0.28861(2) 0.01555(13) Uani 1 1 d . . . P6 P 0.32605(4) 0.57557(3) 0.39408(2) 0.01521(13) Uani 1 1 d . . . P7 P 0.28776(5) 0.41199(3) 0.40343(2) 0.01942(14) Uani 1 1 d . . . P8 P 0.10451(4) 0.43296(3) 0.32843(2) 0.01777(13) Uani 1 1 d . . . N3 N 0.31917(12) 0.46418(9) 0.29967(7) 0.0105(4) Uani 1 1 d . . . N4 N 0.14355(14) 0.53340(10) 0.40452(8) 0.0175(4) Uani 1 1 d . . . C24 C 0.38189(15) 0.50717(11) 0.27749(8) 0.0128(4) Uani 1 1 d . . . C25 C 0.44002(17) 0.48410(13) 0.23958(10) 0.0210(5) Uani 1 1 d . . . H25A H 0.4836 0.5143 0.2256 0.025 Uiso 1 1 calc R . . C26 C 0.43563(18) 0.41839(13) 0.22186(10) 0.0242(6) Uani 1 1 d . . . H26A H 0.4751 0.4030 0.1957 0.029 Uiso 1 1 calc R . . C27 C 0.37286(17) 0.37586(12) 0.24289(9) 0.0198(5) Uani 1 1 d . . . H27A H 0.3681 0.3304 0.2308 0.024 Uiso 1 1 calc R . . C28 C 0.31581(16) 0.39799(11) 0.28176(8) 0.0137(5) Uani 1 1 d . . . C29 C 0.38936(15) 0.58303(11) 0.29186(8) 0.0130(4) Uani 1 1 d . . . C30 C 0.29593(16) 0.62053(11) 0.27660(9) 0.0158(5) Uani 1 1 d . . . H30A H 0.2936 0.6328 0.2384 0.019 Uiso 1 1 calc R . . H30B H 0.2948 0.6630 0.2973 0.019 Uiso 1 1 calc R . . C31 C 0.42009(16) 0.59176(12) 0.35163(8) 0.0154(5) Uani 1 1 d . . . H31A H 0.4433 0.6384 0.3579 0.019 Uiso 1 1 calc R . . H31B H 0.4726 0.5605 0.3614 0.019 Uiso 1 1 calc R . . C32 C 0.46396(17) 0.62020(13) 0.26163(9) 0.0200(5) Uani 1 1 d . . . H32A H 0.4640 0.6683 0.2709 0.030 Uiso 1 1 calc R . . H32B H 0.4494 0.6150 0.2232 0.030 Uiso 1 1 calc R . . H32C H 0.5259 0.6009 0.2716 0.030 Uiso 1 1 calc R . . C33 C 0.24760(18) 0.34555(11) 0.30327(9) 0.0184(5) Uani 1 1 d . . . C34 C 0.26592(19) 0.33482(12) 0.36414(9) 0.0209(5) Uani 1 1 d . . . H34A H 0.3207 0.3045 0.3705 0.025 Uiso 1 1 calc R . . H34B H 0.2110 0.3114 0.3773 0.025 Uiso 1 1 calc R . . C35 C 0.14483(18) 0.36552(12) 0.28746(9) 0.0207(5) Uani 1 1 d . . . H35A H 0.1041 0.3255 0.2907 0.025 Uiso 1 1 calc R . . H35B H 0.1392 0.3800 0.2498 0.025 Uiso 1 1 calc R . . C36 C 0.2595(2) 0.27519(12) 0.27841(10) 0.0272(6) Uani 1 1 d . . . H36A H 0.2180 0.2429 0.2944 0.041 Uiso 1 1 calc R . . H36B H 0.3247 0.2604 0.2850 0.041 Uiso 1 1 calc R . . H36C H 0.2432 0.2776 0.2400 0.041 Uiso 1 1 calc R . . C37 C 0.17140(17) 0.53183(14) 0.22240(9) 0.0226(5) Uani 1 1 d . . . H37A H 0.1427 0.5650 0.1973 0.034 Uiso 1 1 calc R . . H37B H 0.1295 0.4929 0.2245 0.034 Uiso 1 1 calc R . . H37C H 0.2314 0.5168 0.2101 0.034 Uiso 1 1 calc R . . C38 C 0.09723(18) 0.63269(14) 0.28914(12) 0.0299(6) Uani 1 1 d . . . H38A H 0.0978 0.6615 0.2576 0.045 Uiso 1 1 calc R . . H38B H 0.1063 0.6606 0.3212 0.045 Uiso 1 1 calc R . . H38C H 0.0369 0.6092 0.2889 0.045 Uiso 1 1 calc R . . C39 C 0.3879(2) 0.56744(14) 0.46012(9) 0.0257(6) Uani 1 1 d . . . H39A H 0.4214 0.6095 0.4693 0.039 Uiso 1 1 calc R . . H39B H 0.4328 0.5301 0.4599 0.039 Uiso 1 1 calc R . . H39C H 0.3425 0.5584 0.4865 0.039 Uiso 1 1 calc R . . C40 C 0.27300(19) 0.65830(13) 0.40508(11) 0.0260(6) Uani 1 1 d . . . H40A H 0.3220 0.6930 0.4075 0.039 Uiso 1 1 calc R . . H40B H 0.2416 0.6573 0.4383 0.039 Uiso 1 1 calc R . . H40C H 0.2271 0.6687 0.3754 0.039 Uiso 1 1 calc R . . C41 C 0.4157(2) 0.40513(15) 0.41385(13) 0.0379(7) Uani 1 1 d . . . H41A H 0.4324 0.3606 0.4287 0.057 Uiso 1 1 calc R . . H41B H 0.4395 0.4404 0.4387 0.057 Uiso 1 1 calc R . . H41C H 0.4435 0.4108 0.3798 0.057 Uiso 1 1 calc R . . C42 C 0.2519(3) 0.39256(15) 0.46964(10) 0.0401(8) Uani 1 1 d . . . H42A H 0.2792 0.3493 0.4816 0.060 Uiso 1 1 calc R . . H42B H 0.1833 0.3897 0.4684 0.060 Uiso 1 1 calc R . . H42C H 0.2738 0.4283 0.4945 0.060 Uiso 1 1 calc R . . C43 C 0.04521(19) 0.38966(14) 0.38089(11) 0.0278(6) Uani 1 1 d . . . H43A H -0.0068 0.3626 0.3647 0.042 Uiso 1 1 calc R . . H43B H 0.0209 0.4232 0.4049 0.042 Uiso 1 1 calc R . . H43C H 0.0899 0.3601 0.4010 0.042 Uiso 1 1 calc R . . C44 C -0.00225(17) 0.46578(14) 0.29280(11) 0.0276(6) Uani 1 1 d . . . H44A H -0.0424 0.4280 0.2803 0.041 Uiso 1 1 calc R . . H44B H 0.0145 0.4926 0.2622 0.041 Uiso 1 1 calc R . . H44C H -0.0360 0.4943 0.3168 0.041 Uiso 1 1 calc R . . C45 C 0.09468(17) 0.55667(12) 0.43331(9) 0.0197(5) Uani 1 1 d . . . C46 C 0.03350(18) 0.58823(14) 0.47004(10) 0.0270(6) Uani 1 1 d . . . H46A H 0.0380 0.6375 0.4672 0.040 Uiso 1 1 calc R . . H46B H 0.0529 0.5742 0.5065 0.040 Uiso 1 1 calc R . . H46C H -0.0314 0.5741 0.4610 0.040 Uiso 1 1 calc R . . C100 C 0.2905(3) 0.6738(2) 0.05913(13) 0.0288(8) Uani 0.9369(16) 1 d PDU A 1 F11 F 0.35439(12) 0.71795(9) 0.07914(8) 0.0394(5) Uani 0.9369(16) 1 d PDU A 1 F12 F 0.22200(13) 0.71104(9) 0.03352(7) 0.0371(5) Uani 0.9369(16) 1 d PDU A 1 F13 F 0.33234(14) 0.63980(9) 0.02092(7) 0.0297(4) Uani 0.9369(16) 1 d PDU A 1 S100 S 0.24821(5) 0.61872(4) 0.10836(2) 0.01931(17) Uani 0.9369(16) 1 d PDU A 1 O11 O 0.20159(15) 0.56471(10) 0.07791(8) 0.0311(5) Uani 0.9369(16) 1 d PDU A 1 O12 O 0.33178(15) 0.59842(14) 0.13907(8) 0.0428(6) Uani 0.9369(16) 1 d PDU A 1 O13 O 0.18408(19) 0.66132(13) 0.13528(11) 0.0316(6) Uani 0.9369(16) 1 d PDU A 1 C101 C 0.2774(19) 0.6317(12) 0.1035(8) 0.0258(18) Uani 0.0631(16) 1 d PDU A 2 F11A F 0.2765(18) 0.5637(10) 0.0974(9) 0.034(3) Uani 0.0631(16) 1 d PDU A 2 F12A F 0.3452(14) 0.6556(13) 0.1375(7) 0.028(3) Uani 0.0631(16) 1 d PDU A 2 F13A F 0.196(2) 0.6447(17) 0.1254(13) 0.027(3) Uani 0.0631(16) 1 d PDU A 2 S101 S 0.2799(12) 0.6715(9) 0.0416(6) 0.0354(19) Uani 0.0631(16) 1 d PDU A 2 O11A O 0.276(2) 0.7432(10) 0.0452(11) 0.030(3) Uani 0.0631(16) 1 d PDU A 2 O12A O 0.2040(14) 0.6481(12) 0.0061(8) 0.020(4) Uani 0.0631(16) 1 d PDU A 2 O13A O 0.3696(17) 0.6547(18) 0.0217(14) 0.032(3) Uani 0.0631(16) 1 d PDU A 2 C200 C 0.66877(19) 0.49821(16) 0.38626(10) 0.0319(7) Uani 1 1 d . . . F21 F 0.62838(11) 0.52259(9) 0.42778(6) 0.0364(4) Uani 1 1 d . B . F22 F 0.6774(6) 0.5556(4) 0.3558(4) 0.057(2) Uani 0.70(3) 1 d P B 1 F23 F 0.6107(4) 0.4588(5) 0.3582(3) 0.059(2) Uani 0.70(3) 1 d P B 1 F22A F 0.6497(11) 0.5214(19) 0.3439(4) 0.065(8) Uani 0.30(3) 1 d P B 2 F23A F 0.6143(12) 0.4338(12) 0.3865(15) 0.087(9) Uani 0.30(3) 1 d P B 2 S200 S 0.78333(4) 0.46180(3) 0.40235(2) 0.02241(14) Uani 1 1 d . B . O21 O 0.80623(13) 0.43184(10) 0.35326(7) 0.0332(5) Uani 1 1 d . . . O22 O 0.7580(7) 0.4100(3) 0.4405(3) 0.0365(15) Uani 0.70(3) 1 d P B 1 O23 O 0.8403(5) 0.5130(5) 0.4250(6) 0.055(2) Uani 0.70(3) 1 d P B 1 O22A O 0.7900(19) 0.4311(17) 0.4503(8) 0.062(7) Uani 0.30(3) 1 d P B 2 O23A O 0.8348(12) 0.5296(9) 0.4030(8) 0.036(3) Uani 0.30(3) 1 d P B 2 C300 C 0.9322(2) 0.27187(18) 0.11327(14) 0.0461(8) Uani 1 1 d D . . F31 F 0.86848(13) 0.31179(10) 0.08843(8) 0.0535(5) Uani 1 1 d . C . F32 F 0.8941(5) 0.2322(3) 0.1477(3) 0.0487(17) Uani 0.570(14) 1 d PD C 1 F33 F 0.9604(4) 0.2298(2) 0.07411(16) 0.0360(14) Uani 0.570(14) 1 d PD C 1 F32A F 0.8874(11) 0.2601(14) 0.1611(7) 0.191(9) Uani 0.430(14) 1 d PD C 2 F33A F 0.9422(11) 0.2162(6) 0.0882(8) 0.197(10) Uani 0.430(14) 1 d PD C 2 S300 S 1.03469(5) 0.31777(3) 0.13991(3) 0.02858(15) Uani 1 1 d D C . O31 O 1.09443(15) 0.26731(10) 0.16460(9) 0.0451(6) Uani 1 1 d . . . O32 O 1.0590(8) 0.3568(4) 0.0947(4) 0.046(2) Uani 0.570(14) 1 d PD C 1 O33 O 0.9930(14) 0.3613(11) 0.1781(9) 0.051(3) Uani 0.570(14) 1 d PD C 1 O32A O 1.0746(11) 0.3294(10) 0.0892(5) 0.084(5) Uani 0.430(14) 1 d PD C 2 O33A O 1.013(2) 0.3721(15) 0.1700(12) 0.082(9) Uani 0.430(14) 1 d P C 2 C400 C 0.6009(5) 0.2500(5) 0.0834(4) 0.0279(17) Uani 0.681(13) 1 d P D 1 F41 F 0.5931(3) 0.2425(2) 0.02989(17) 0.0401(10) Uani 0.681(13) 1 d P D 1 F42 F 0.6745(2) 0.2923(2) 0.0933(3) 0.067(2) Uani 0.681(13) 1 d P D 1 C401 C 0.607(2) 0.2628(11) 0.0991(12) 0.071(10) Uani 0.319(13) 1 d P D 2 F41A F 0.6703(5) 0.2795(4) 0.1363(7) 0.074(5) Uani 0.319(13) 1 d P D 2 F42A F 0.6335(12) 0.2606(9) 0.0517(7) 0.099(10) Uani 0.319(13) 1 d P D 2 F43 F 0.61362(17) 0.19054(10) 0.10561(8) 0.0655(6) Uani 1 1 d . . . S400 S 0.49357(5) 0.28982(3) 0.10588(3) 0.02594(14) Uani 1 1 d . . . O41 O 0.5002(2) 0.28432(13) 0.16201(8) 0.0710(9) Uani 1 1 d . D . O42 O 0.42382(17) 0.24657(14) 0.08013(12) 0.0676(8) Uani 1 1 d . D . O43 O 0.49621(18) 0.35739(12) 0.08663(12) 0.0668(8) Uani 1 1 d . D . 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 0.00902(15) 0.01194(16) 0.00884(14) -0.00117(12) 0.00034(11) 0.00105(13) P1 0.0146(3) 0.0139(3) 0.0122(3) 0.0030(2) 0.0007(2) -0.0014(2) P2 0.0180(3) 0.0169(3) 0.0144(3) 0.0003(2) 0.0013(2) 0.0073(3) P3 0.0110(3) 0.0252(3) 0.0157(3) -0.0048(2) 0.0015(2) -0.0045(3) P4 0.0123(3) 0.0115(3) 0.0135(3) -0.0007(2) 0.0039(2) 0.0014(2) N1 0.0112(9) 0.0133(9) 0.0111(8) -0.0012(7) 0.0026(7) 0.0014(8) N2 0.0106(9) 0.0177(10) 0.0152(9) -0.0006(8) 0.0001(7) 0.0017(8) C1 0.0142(11) 0.0123(11) 0.0134(10) -0.0024(8) 0.0007(8) 0.0020(9) C2 0.0195(12) 0.0209(12) 0.0140(11) -0.0062(9) -0.0004(9) 0.0002(10) C3 0.0244(13) 0.0271(13) 0.0104(10) -0.0004(10) 0.0005(9) 0.0022(11) C4 0.0195(12) 0.0214(13) 0.0152(11) 0.0034(9) 0.0048(9) 0.0019(10) C5 0.0105(11) 0.0142(11) 0.0147(10) 0.0006(9) 0.0047(8) 0.0005(9) C6 0.0247(13) 0.0130(11) 0.0161(11) -0.0022(9) -0.0016(9) -0.0024(10) C7 0.0214(13) 0.0174(12) 0.0180(11) 0.0024(9) -0.0013(9) -0.0088(10) C8 0.0321(14) 0.0133(12) 0.0189(11) -0.0016(9) 0.0020(10) 0.0054(11) C9 0.0443(17) 0.0185(13) 0.0210(12) -0.0038(10) -0.0029(11) -0.0068(12) C10 0.0216(12) 0.0151(12) 0.0159(11) -0.0014(9) 0.0051(9) -0.0046(10) C11 0.0153(12) 0.0260(14) 0.0207(12) -0.0035(10) 0.0059(9) -0.0091(10) C12 0.0222(13) 0.0114(11) 0.0224(12) -0.0014(9) 0.0077(10) -0.0016(10) C13 0.0340(15) 0.0201(13) 0.0256(13) 0.0026(11) 0.0099(11) -0.0096(12) C14 0.0176(13) 0.0278(14) 0.0215(12) 0.0074(10) 0.0064(10) -0.0002(11) C15 0.0294(14) 0.0207(13) 0.0195(12) 0.0067(10) 0.0011(10) -0.0009(11) C16 0.0273(14) 0.0309(15) 0.0227(12) -0.0025(11) 0.0076(11) 0.0113(12) C17 0.0253(14) 0.0284(14) 0.0241(13) 0.0050(11) -0.0007(10) 0.0144(12) C18 0.0150(13) 0.0486(18) 0.0327(15) -0.0061(13) -0.0042(11) -0.0005(12) C19 0.0275(14) 0.0318(15) 0.0248(13) -0.0137(11) 0.0035(11) -0.0155(12) C20 0.0130(12) 0.0220(13) 0.0212(12) 0.0059(10) 0.0004(9) 0.0046(10) C21 0.0263(14) 0.0217(13) 0.0231(12) -0.0043(10) 0.0107(10) 0.0045(11) C22 0.0140(12) 0.0215(12) 0.0177(12) -0.0017(10) -0.0013(9) 0.0032(10) C23 0.0321(15) 0.0408(17) 0.0124(11) -0.0042(11) -0.0014(10) 0.0048(13) Fe2 0.01433(16) 0.00849(15) 0.01083(14) -0.00064(12) 0.00359(12) -0.00179(13) P5 0.0129(3) 0.0144(3) 0.0195(3) 0.0043(2) 0.0018(2) 0.0009(2) P6 0.0185(3) 0.0142(3) 0.0133(3) -0.0024(2) 0.0035(2) -0.0036(2) P7 0.0324(4) 0.0125(3) 0.0130(3) 0.0014(2) -0.0010(2) -0.0001(3) P8 0.0181(3) 0.0173(3) 0.0184(3) 0.0002(2) 0.0040(2) -0.0059(3) N3 0.0124(9) 0.0098(9) 0.0092(8) 0.0004(7) 0.0002(7) 0.0010(7) N4 0.0206(11) 0.0139(10) 0.0185(10) -0.0020(8) 0.0043(8) -0.0052(8) C24 0.0125(11) 0.0143(11) 0.0114(10) 0.0010(8) -0.0009(8) 0.0014(9) C25 0.0176(12) 0.0230(13) 0.0234(12) -0.0013(10) 0.0078(10) -0.0022(10) C26 0.0239(14) 0.0256(14) 0.0241(12) -0.0069(11) 0.0082(10) 0.0057(11) C27 0.0252(13) 0.0137(12) 0.0204(11) -0.0050(9) 0.0010(10) 0.0057(10) C28 0.0166(12) 0.0108(11) 0.0134(10) 0.0000(8) -0.0012(9) 0.0029(9) C29 0.0134(11) 0.0125(11) 0.0133(10) 0.0013(8) 0.0023(8) -0.0033(9) C30 0.0187(12) 0.0110(11) 0.0180(11) 0.0049(9) 0.0027(9) -0.0004(9) C31 0.0153(12) 0.0152(11) 0.0157(11) -0.0005(9) 0.0013(9) -0.0032(9) C32 0.0202(13) 0.0216(13) 0.0189(11) 0.0035(10) 0.0051(9) -0.0081(10) C33 0.0299(14) 0.0090(11) 0.0163(11) -0.0025(9) 0.0015(10) -0.0017(10) C34 0.0339(15) 0.0110(11) 0.0176(11) 0.0014(9) 0.0016(10) -0.0025(11) C35 0.0259(14) 0.0157(12) 0.0205(12) -0.0040(10) 0.0022(10) -0.0090(10) C36 0.0470(17) 0.0094(12) 0.0257(13) -0.0047(10) 0.0049(12) -0.0022(12) C37 0.0178(13) 0.0323(15) 0.0168(11) 0.0058(10) -0.0042(9) -0.0042(11) C38 0.0179(13) 0.0227(14) 0.0493(17) 0.0094(12) 0.0041(12) 0.0065(11) C39 0.0388(16) 0.0247(14) 0.0132(11) -0.0029(10) -0.0009(10) -0.0069(12) C40 0.0318(15) 0.0163(12) 0.0308(14) -0.0099(11) 0.0083(11) -0.0036(11) C41 0.0367(17) 0.0247(15) 0.0489(18) -0.0021(13) -0.0182(14) 0.0056(13) C42 0.079(2) 0.0270(15) 0.0151(12) 0.0050(11) 0.0055(14) -0.0035(16) C43 0.0294(15) 0.0239(14) 0.0316(14) 0.0037(11) 0.0122(11) -0.0110(12) C44 0.0150(13) 0.0336(15) 0.0341(14) 0.0032(12) 0.0008(11) -0.0064(11) C45 0.0229(13) 0.0164(12) 0.0206(12) -0.0030(10) 0.0060(10) -0.0050(10) C46 0.0235(14) 0.0321(15) 0.0266(13) -0.0103(11) 0.0107(11) -0.0014(12) C100 0.0340(16) 0.0281(15) 0.0248(16) -0.0070(15) 0.0059(14) 0.0041(13) F11 0.0309(10) 0.0282(9) 0.0608(12) -0.0178(9) 0.0155(9) -0.0084(8) F12 0.0342(10) 0.0342(10) 0.0440(10) 0.0165(8) 0.0096(8) 0.0151(9) F13 0.0409(11) 0.0261(10) 0.0242(8) -0.0041(7) 0.0161(9) 0.0099(8) S100 0.0211(4) 0.0245(4) 0.0121(3) -0.0019(3) -0.0004(3) 0.0039(3) O11 0.0415(13) 0.0212(10) 0.0306(11) -0.0036(8) 0.0026(9) -0.0052(9) O12 0.0292(12) 0.0745(18) 0.0237(10) 0.0141(11) -0.0038(9) 0.0055(12) O13 0.0321(12) 0.0309(15) 0.0341(14) -0.0088(10) 0.0179(10) -0.0004(11) C101 0.027(3) 0.032(3) 0.019(3) -0.003(3) 0.004(3) 0.005(3) F11A 0.036(5) 0.039(5) 0.026(5) 0.009(5) 0.002(5) 0.001(5) F12A 0.024(5) 0.046(6) 0.014(5) 0.000(5) -0.003(5) 0.008(5) F13A 0.030(6) 0.026(6) 0.025(6) -0.008(6) 0.008(6) -0.003(6) S101 0.039(3) 0.032(3) 0.037(4) 0.001(3) 0.013(3) -0.003(3) O11A 0.030(5) 0.026(5) 0.037(5) -0.001(5) 0.016(5) 0.001(5) O12A 0.019(7) 0.028(7) 0.016(6) 0.003(6) 0.011(6) 0.002(6) O13A 0.034(6) 0.032(6) 0.030(6) -0.002(6) 0.012(6) 0.002(6) C200 0.0221(14) 0.0548(19) 0.0194(13) -0.0009(13) 0.0049(11) 0.0041(14) F21 0.0371(9) 0.0516(11) 0.0213(8) 0.0012(7) 0.0076(7) 0.0183(8) F22 0.057(3) 0.065(4) 0.055(4) 0.046(3) 0.035(3) 0.037(3) F23 0.0223(19) 0.095(4) 0.055(4) -0.038(3) -0.012(2) 0.006(2) F22A 0.039(7) 0.14(2) 0.017(3) 0.014(6) 0.001(4) 0.053(10) F23A 0.035(6) 0.109(11) 0.120(18) -0.060(12) 0.033(9) -0.044(6) S200 0.0210(3) 0.0212(3) 0.0243(3) -0.0002(3) -0.0031(2) 0.0034(3) O21 0.0288(11) 0.0401(12) 0.0325(10) 0.0020(9) 0.0147(8) 0.0039(9) O22 0.057(4) 0.029(2) 0.026(3) 0.0094(17) 0.015(2) 0.016(2) O23 0.030(2) 0.034(3) 0.097(6) -0.019(4) -0.024(3) -0.001(2) O22A 0.074(12) 0.085(16) 0.029(7) 0.031(8) 0.010(7) 0.050(11) O23A 0.025(5) 0.027(7) 0.056(8) -0.012(5) -0.005(5) -0.006(4) C300 0.0337(18) 0.038(2) 0.065(2) 0.0160(17) -0.0079(16) 0.0036(15) F31 0.0376(11) 0.0478(12) 0.0719(13) 0.0047(10) -0.0163(9) 0.0140(9) F32 0.044(3) 0.048(3) 0.054(3) 0.019(2) 0.0030(19) -0.014(2) F33 0.047(2) 0.021(2) 0.039(2) -0.0193(15) -0.0065(17) 0.0033(17) F32A 0.089(9) 0.28(2) 0.199(15) 0.155(14) -0.011(9) -0.076(12) F33A 0.143(11) 0.023(4) 0.40(2) 0.014(8) -0.181(13) -0.003(5) S300 0.0347(4) 0.0242(3) 0.0257(3) -0.0023(3) -0.0058(3) 0.0030(3) O31 0.0419(13) 0.0299(11) 0.0602(14) -0.0122(10) -0.0173(11) 0.0162(10) O32 0.047(5) 0.043(3) 0.046(4) 0.013(3) -0.009(3) -0.017(3) O33 0.060(4) 0.052(9) 0.039(4) -0.018(4) -0.019(3) 0.030(4) O32A 0.053(5) 0.177(15) 0.022(4) 0.017(8) 0.006(3) -0.007(10) O33A 0.14(2) 0.029(7) 0.067(13) -0.025(7) -0.055(12) 0.056(12) C400 0.020(3) 0.021(4) 0.043(5) -0.007(3) 0.000(3) 0.004(2) F41 0.044(2) 0.0488(19) 0.029(2) 0.0045(14) 0.0144(14) 0.0035(16) F42 0.0219(17) 0.081(3) 0.097(6) -0.015(3) -0.007(2) -0.0123(18) C401 0.14(2) 0.017(8) 0.060(14) -0.021(8) 0.038(14) -0.005(9) F41A 0.032(4) 0.078(6) 0.111(12) 0.013(6) 0.007(5) -0.002(4) F42A 0.094(14) 0.125(16) 0.087(12) 0.061(13) 0.070(13) 0.075(13) F43 0.0994(17) 0.0466(12) 0.0493(12) 0.0097(10) -0.0033(11) 0.0416(12) S400 0.0318(4) 0.0219(3) 0.0247(3) 0.0021(3) 0.0058(3) -0.0009(3) O41 0.136(3) 0.0526(16) 0.0243(11) -0.0082(11) 0.0059(14) 0.0397(17) O42 0.0420(14) 0.0730(19) 0.087(2) -0.0418(16) -0.0007(13) -0.0078(13) O43 0.0583(16) 0.0336(13) 0.114(2) 0.0376(14) 0.0452(16) 0.0176(12) _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 1.9259(18) . ? Fe1 N1 2.0992(17) . ? Fe1 P3 2.2275(7) . ? Fe1 P4 2.2379(7) . ? Fe1 P1 2.2391(7) . ? Fe1 P2 2.2434(7) . ? P1 C7 1.814(2) . ? P1 C14 1.823(2) . ? P1 C15 1.834(2) . ? P2 C17 1.824(2) . ? P2 C8 1.839(3) . ? P2 C16 1.843(3) . ? P3 C11 1.811(2) . ? P3 C19 1.825(2) . ? P3 C18 1.825(3) . ? P4 C21 1.816(2) . ? P4 C12 1.830(2) . ? P4 C20 1.835(2) . ? N1 C1 1.388(3) . ? N1 C5 1.390(3) . ? N2 C22 1.147(3) . ? C1 C2 1.397(3) . ? C1 C6 1.545(3) . ? C2 C3 1.368(3) . ? C2 H2A 0.9500 . ? C3 C4 1.372(3) . ? C3 H3A 0.9500 . ? C4 C5 1.390(3) . ? C4 H4A 0.9500 . ? C5 C10 1.548(3) . ? C6 C9 1.543(3) . ? C6 C8 1.554(3) . ? C6 C7 1.556(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C13 1.544(3) . ? C10 C11 1.549(3) . ? C10 C12 1.557(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.462(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? Fe2 N4 1.915(2) . ? Fe2 N3 2.1072(18) . ? Fe2 P5 2.2344(7) . ? Fe2 P7 2.2370(7) . ? Fe2 P8 2.2488(7) . ? Fe2 P6 2.2488(7) . ? P5 C38 1.824(3) . ? P5 C30 1.834(2) . ? P5 C37 1.841(2) . ? P6 C31 1.810(2) . ? P6 C39 1.832(2) . ? P6 C40 1.834(3) . ? P7 C42 1.824(3) . ? P7 C41 1.834(3) . ? P7 C34 1.834(2) . ? P8 C35 1.809(2) . ? P8 C44 1.831(3) . ? P8 C43 1.836(2) . ? N3 C24 1.385(3) . ? N3 C28 1.385(3) . ? N4 C45 1.142(3) . ? C24 C25 1.391(3) . ? C24 C29 1.546(3) . ? C25 C26 1.375(3) . ? C25 H25A 0.9500 . ? C26 C27 1.367(4) . ? C26 H26A 0.9500 . ? C27 C28 1.393(3) . ? C27 H27A 0.9500 . ? C28 C33 1.550(3) . ? C29 C32 1.544(3) . ? C29 C31 1.547(3) . ? C29 C30 1.552(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.542(3) . ? C33 C35 1.545(3) . ? C33 C34 1.551(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.461(3) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C100 F11 1.335(4) . ? C100 F12 1.350(4) . ? C100 F13 1.352(4) . ? C100 S100 1.791(4) . ? S100 O12 1.432(2) . ? S100 O11 1.449(2) . ? S100 O13 1.451(2) . ? C101 F12A 1.331(18) . ? C101 F13A 1.353(19) . ? C101 F11A 1.355(19) . ? C101 S101 1.751(17) . ? S101 O11A 1.423(17) . ? S101 O12A 1.431(16) . ? S101 O13A 1.452(18) . ? C200 F22A 1.175(15) . ? C200 F23 1.308(6) . ? C200 F21 1.324(3) . ? C200 F22 1.381(5) . ? C200 F23A 1.494(16) . ? C200 S200 1.808(3) . ? S200 O22A 1.350(16) . ? S200 O23 1.395(7) . ? S200 O21 1.432(2) . ? S200 O22 1.470(7) . ? S200 O23A 1.530(15) . ? C300 F33A 1.284(11) . ? C300 F32 1.319(7) . ? C300 F31 1.327(3) . ? C300 F33 1.375(5) . ? C300 F32A 1.427(12) . ? C300 S300 1.810(3) . ? S300 O33A 1.36(3) . ? S300 O31 1.426(2) . ? S300 O32 1.442(10) . ? S300 O33 1.45(2) . ? S300 O32A 1.456(14) . ? C400 F43 1.310(9) . ? C400 F41 1.353(11) . ? C400 F42 1.353(10) . ? C400 S400 1.852(8) . ? C401 F42A 1.28(3) . ? C401 F41A 1.30(3) . ? C401 F43 1.44(2) . ? C401 S400 1.73(3) . ? S400 O41 1.415(2) . ? S400 O43 1.424(2) . ? S400 O42 1.432(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 N2 Fe1 N1 177.45(8) . . ? N2 Fe1 P3 82.95(6) . . ? N1 Fe1 P3 96.77(5) . . ? N2 Fe1 P4 96.35(6) . . ? N1 Fe1 P4 81.11(5) . . ? P3 Fe1 P4 89.90(3) . . ? N2 Fe1 P1 82.86(6) . . ? N1 Fe1 P1 97.44(5) . . ? P3 Fe1 P1 165.78(2) . . ? P4 Fe1 P1 92.49(2) . . ? N2 Fe1 P2 101.09(6) . . ? N1 Fe1 P2 81.45(5) . . ? P3 Fe1 P2 92.55(3) . . ? P4 Fe1 P2 162.55(2) . . ? P1 Fe1 P2 89.36(3) . . ? C7 P1 C14 106.05(12) . . ? C7 P1 C15 105.27(11) . . ? C14 P1 C15 95.94(12) . . ? C7 P1 Fe1 108.72(8) . . ? C14 P1 Fe1 123.60(9) . . ? C15 P1 Fe1 115.38(9) . . ? C17 P2 C8 106.00(12) . . ? C17 P2 C16 101.73(12) . . ? C8 P2 C16 97.61(12) . . ? C17 P2 Fe1 122.50(9) . . ? C8 P2 Fe1 107.70(8) . . ? C16 P2 Fe1 118.04(9) . . ? C11 P3 C19 104.56(12) . . ? C11 P3 C18 105.18(13) . . ? C19 P3 C18 96.90(13) . . ? C11 P3 Fe1 109.14(8) . . ? C19 P3 Fe1 115.71(9) . . ? C18 P3 Fe1 123.31(10) . . ? C21 P4 C12 105.40(11) . . ? C21 P4 C20 101.61(12) . . ? C12 P4 C20 98.92(11) . . ? C21 P4 Fe1 122.82(9) . . ? C12 P4 Fe1 108.37(8) . . ? C20 P4 Fe1 116.71(8) . . ? C1 N1 C5 117.51(18) . . ? C1 N1 Fe1 121.21(14) . . ? C5 N1 Fe1 121.28(14) . . ? C22 N2 Fe1 174.7(2) . . ? N1 C1 C2 120.8(2) . . ? N1 C1 C6 122.00(18) . . ? C2 C1 C6 117.2(2) . . ? C3 C2 C1 121.1(2) . . ? C3 C2 H2A 119.5 . . ? C1 C2 H2A 119.5 . . ? C2 C3 C4 118.7(2) . . ? C2 C3 H3A 120.7 . . ? C4 C3 H3A 120.7 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C4 C5 N1 121.0(2) . . ? C4 C5 C10 116.8(2) . . ? N1 C5 C10 122.21(18) . . ? C9 C6 C1 111.93(19) . . ? C9 C6 C8 105.42(19) . . ? C1 C6 C8 111.5(2) . . ? C9 C6 C7 105.2(2) . . ? C1 C6 C7 110.39(19) . . ? C8 C6 C7 112.16(19) . . ? C6 C7 P1 111.88(16) . . ? C6 C7 H7A 109.2 . . ? P1 C7 H7A 109.2 . . ? C6 C7 H7B 109.2 . . ? P1 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C6 C8 P2 114.32(16) . . ? C6 C8 H8A 108.7 . . ? P2 C8 H8A 108.7 . . ? C6 C8 H8B 108.7 . . ? P2 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C13 C10 C5 112.32(19) . . ? C13 C10 C11 105.5(2) . . ? C5 C10 C11 109.59(19) . . ? C13 C10 C12 105.7(2) . . ? C5 C10 C12 111.11(19) . . ? C11 C10 C12 112.43(19) . . ? C10 C11 P3 112.48(16) . . ? C10 C11 H11A 109.1 . . ? P3 C11 H11A 109.1 . . ? C10 C11 H11B 109.1 . . ? P3 C11 H11B 109.1 . . ? H11A C11 H11B 107.8 . . ? C10 C12 P4 114.15(16) . . ? C10 C12 H12A 108.7 . . ? P4 C12 H12A 108.7 . . ? C10 C12 H12B 108.7 . . ? P4 C12 H12B 108.7 . . ? H12A C12 H12B 107.6 . . ? C10 C13 H13A 109.5 . . ? C10 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C10 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P3 C18 H18A 109.5 . . ? P3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P3 C19 H19A 109.5 . . ? P3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P4 C20 H20A 109.5 . . ? P4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P4 C21 H21A 109.5 . . ? P4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 C23 177.6(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 Fe2 N3 177.76(8) . . ? N4 Fe2 P5 98.01(6) . . ? N3 Fe2 P5 79.92(5) . . ? N4 Fe2 P7 99.17(6) . . ? N3 Fe2 P7 82.94(5) . . ? P5 Fe2 P7 162.67(3) . . ? N4 Fe2 P8 83.69(6) . . ? N3 Fe2 P8 97.13(5) . . ? P5 Fe2 P8 90.74(3) . . ? P7 Fe2 P8 88.90(3) . . ? N4 Fe2 P6 83.06(6) . . ? N3 Fe2 P6 96.06(5) . . ? P5 Fe2 P6 89.76(3) . . ? P7 Fe2 P6 94.54(3) . . ? P8 Fe2 P6 166.69(3) . . ? C38 P5 C30 104.58(12) . . ? C38 P5 C37 102.89(13) . . ? C30 P5 C37 98.54(11) . . ? C38 P5 Fe2 123.45(10) . . ? C30 P5 Fe2 108.90(7) . . ? C37 P5 Fe2 115.25(9) . . ? C31 P6 C39 102.91(12) . . ? C31 P6 C40 105.41(12) . . ? C39 P6 C40 96.77(12) . . ? C31 P6 Fe2 109.49(8) . . ? C39 P6 Fe2 125.41(9) . . ? C40 P6 Fe2 114.59(9) . . ? C42 P7 C41 101.55(16) . . ? C42 P7 C34 105.67(12) . . ? C41 P7 C34 98.22(13) . . ? C42 P7 Fe2 122.25(11) . . ? C41 P7 Fe2 118.37(10) . . ? C34 P7 Fe2 107.64(8) . . ? C35 P8 C44 105.78(12) . . ? C35 P8 C43 104.55(12) . . ? C44 P8 C43 96.04(13) . . ? C35 P8 Fe2 108.88(8) . . ? C44 P8 Fe2 123.10(9) . . ? C43 P8 Fe2 116.47(9) . . ? C24 N3 C28 117.20(18) . . ? C24 N3 Fe2 121.69(14) . . ? C28 N3 Fe2 121.02(15) . . ? C45 N4 Fe2 177.2(2) . . ? N3 C24 C25 121.0(2) . . ? N3 C24 C29 122.52(19) . . ? C25 C24 C29 116.4(2) . . ? C26 C25 C24 121.3(2) . . ? C26 C25 H25A 119.4 . . ? C24 C25 H25A 119.4 . . ? C27 C26 C25 118.2(2) . . ? C27 C26 H26A 120.9 . . ? C25 C26 H26A 120.9 . . ? C26 C27 C28 121.1(2) . . ? C26 C27 H27A 119.5 . . ? C28 C27 H27A 119.5 . . ? N3 C28 C27 121.3(2) . . ? N3 C28 C33 121.77(19) . . ? C27 C28 C33 117.0(2) . . ? C32 C29 C24 112.66(19) . . ? C32 C29 C31 105.74(18) . . ? C24 C29 C31 110.25(17) . . ? C32 C29 C30 105.32(18) . . ? C24 C29 C30 111.31(18) . . ? C31 C29 C30 111.34(18) . . ? C29 C30 P5 113.52(15) . . ? C29 C30 H30A 108.9 . . ? P5 C30 H30A 108.9 . . ? C29 C30 H30B 108.9 . . ? P5 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? C29 C31 P6 112.76(15) . . ? C29 C31 H31A 109.0 . . ? P6 C31 H31A 109.0 . . ? C29 C31 H31B 109.0 . . ? P6 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 C35 104.9(2) . . ? C36 C33 C28 111.8(2) . . ? C35 C33 C28 110.50(18) . . ? C36 C33 C34 105.24(19) . . ? C35 C33 C34 112.1(2) . . ? C28 C33 C34 111.95(19) . . ? C33 C34 P7 115.41(16) . . ? C33 C34 H34A 108.4 . . ? P7 C34 H34A 108.4 . . ? C33 C34 H34B 108.4 . . ? P7 C34 H34B 108.4 . . ? H34A C34 H34B 107.5 . . ? C33 C35 P8 112.32(16) . . ? C33 C35 H35A 109.1 . . ? P8 C35 H35A 109.1 . . ? C33 C35 H35B 109.1 . . ? P8 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P5 C37 H37A 109.5 . . ? P5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P5 C38 H38A 109.5 . . ? P5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P6 C39 H39A 109.5 . . ? P6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P6 C40 H40A 109.5 . . ? P6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? P7 C41 H41A 109.5 . . ? P7 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P7 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P7 C42 H42A 109.5 . . ? P7 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P7 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P8 C43 H43A 109.5 . . ? P8 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? P8 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? P8 C44 H44A 109.5 . . ? P8 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? P8 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N4 C45 C46 178.4(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? F11 C100 F12 106.0(3) . . ? F11 C100 F13 105.5(3) . . ? F12 C100 F13 106.0(3) . . ? F11 C100 S100 113.2(2) . . ? F12 C100 S100 113.1(3) . . ? F13 C100 S100 112.4(3) . . ? O12 S100 O11 114.29(15) . . ? O12 S100 O13 116.22(15) . . ? O11 S100 O13 113.22(15) . . ? O12 S100 C100 103.50(16) . . ? O11 S100 C100 104.38(14) . . ? O13 S100 C100 103.21(17) . . ? F12A C101 F13A 106(2) . . ? F12A C101 F11A 115(2) . . ? F13A C101 F11A 104(2) . . ? F12A C101 S101 110.5(16) . . ? F13A C101 S101 111(2) . . ? F11A C101 S101 110.2(16) . . ? O11A S101 O12A 109.2(18) . . ? O11A S101 O13A 107.1(18) . . ? O12A S101 O13A 110.9(18) . . ? O11A S101 C101 112.9(15) . . ? O12A S101 C101 110.3(14) . . ? O13A S101 C101 106.4(17) . . ? F22A C200 F23 69.3(14) . . ? F22A C200 F21 119.4(9) . . ? F23 C200 F21 110.3(4) . . ? F23 C200 F22 105.6(4) . . ? F21 C200 F22 101.7(4) . . ? F22A C200 F23A 104.6(8) . . ? F21 C200 F23A 92.8(7) . . ? F22 C200 F23A 140.5(12) . . ? F22A C200 S200 120.3(6) . . ? F23 C200 S200 114.3(3) . . ? F21 C200 S200 114.22(18) . . ? F22 C200 S200 109.6(4) . . ? F23A C200 S200 97.1(12) . . ? O22A S200 O23 87.8(12) . . ? O22A S200 O21 125.6(12) . . ? O23 S200 O21 119.3(6) . . ? O23 S200 O22 113.9(4) . . ? O21 S200 O22 111.1(3) . . ? O22A S200 O23A 112.5(12) . . ? O21 S200 O23A 103.4(6) . . ? O22 S200 O23A 138.3(6) . . ? O22A S200 C200 112.4(9) . . ? O23 S200 C200 107.1(3) . . ? O21 S200 C200 103.53(12) . . ? O22 S200 C200 99.3(4) . . ? O23A S200 C200 94.6(8) . . ? F33A C300 F32 83.1(10) . . ? F33A C300 F31 112.1(6) . . ? F32 C300 F31 111.2(4) . . ? F32 C300 F33 105.6(4) . . ? F31 C300 F33 104.5(3) . . ? F33A C300 F32A 110.5(10) . . ? F31 C300 F32A 99.2(9) . . ? F33 C300 F32A 133.0(12) . . ? F33A C300 S300 119.8(7) . . ? F32 C300 S300 114.7(4) . . ? F31 C300 S300 112.6(2) . . ? F33 C300 S300 107.3(3) . . ? F32A C300 S300 99.9(9) . . ? O33A S300 O31 117.6(13) . . ? O33A S300 O32 95.5(13) . . ? O31 S300 O32 123.2(4) . . ? O31 S300 O33 112.9(9) . . ? O32 S300 O33 110.0(9) . . ? O33A S300 O32A 119.0(13) . . ? O31 S300 O32A 103.4(7) . . ? O33 S300 O32A 134.1(11) . . ? O33A S300 C300 112.9(13) . . ? O31 S300 C300 104.61(14) . . ? O32 S300 C300 102.3(4) . . ? O33 S300 C300 100.5(8) . . ? O32A S300 C300 96.5(7) . . ? F43 C400 F41 109.0(8) . . ? F43 C400 F42 113.3(5) . . ? F41 C400 F42 104.8(7) . . ? F43 C400 S400 110.1(6) . . ? F41 C400 S400 110.1(4) . . ? F42 C400 S400 109.4(6) . . ? F42A C401 F41A 116(3) . . ? F42A C401 F43 93.0(13) . . ? F41A C401 F43 97.7(19) . . ? F42A C401 S400 117(2) . . ? F41A C401 S400 117.3(14) . . ? F43 C401 S400 110.5(19) . . ? O41 S400 O43 114.30(17) . . ? O41 S400 O42 113.48(19) . . ? O43 S400 O42 116.26(19) . . ? O41 S400 C401 94.8(10) . . ? O43 S400 C401 102.0(9) . . ? O42 S400 C401 113.4(8) . . ? O41 S400 C400 106.2(3) . . ? O43 S400 C400 104.6(3) . . ? O42 S400 C400 99.9(3) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.848 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.071 # Attachment '7-MeOH(CCDC-612671).cif' data_ag0616a _database_code_depnum_ccdc_archive 'CCDC 612671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H44 Fe N O P4, C H4 O, 2(Br)' _chemical_formula_sum 'C23 H48 Br2 Fe N O2 P4' _chemical_formula_weight 710.17 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall P2yb _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.5483(6) _cell_length_b 12.300(2) _cell_length_c 12.043(2) _cell_angle_alpha 90.00 _cell_angle_beta 110.330(7) _cell_angle_gamma 90.00 _cell_volume 1465.2(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 283 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 730 _exptl_absorpt_coefficient_mu 3.482 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.550 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _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 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \w-rotations with 2.00 \% and 156 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27988 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 27.10 _reflns_number_total 6467 _reflns_number_gt 5722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0114P)^2^+0.0929P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack H D (1983), Acta Cryst. A39, 876-881 3080 Friedel pairs used in the refinement of Flack parameter ; _refine_ls_abs_structure_Flack 0.021(5) _refine_ls_number_reflns 6467 _refine_ls_number_parameters 340 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0264 _refine_ls_wR_factor_ref 0.0514 _refine_ls_wR_factor_gt 0.0491 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.031 _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 Br1 Br 0.34432(3) 0.83258(4) 0.09794(2) 0.01958(7) Uani 1 1 d . . . Br2 Br 0.06136(15) 0.5407(2) 0.62602(16) 0.0269(4) Uani 0.611(6) 1 d P A 1 Br2A Br 0.0575(2) 0.4992(3) 0.6305(2) 0.0199(4) Uani 0.389(6) 1 d P A 2 Fe1 Fe 0.35011(4) 0.35417(4) 0.20186(3) 0.00954(9) Uani 1 1 d . . . P1 P 0.23977(7) 0.48248(7) 0.26838(6) 0.01284(16) Uani 1 1 d . . . P2 P 0.19689(7) 0.23257(7) 0.22409(7) 0.01451(16) Uani 1 1 d . . . P3 P 0.49757(7) 0.21949(7) 0.19361(6) 0.01230(16) Uani 1 1 d . . . P4 P 0.23666(7) 0.38418(7) 0.01036(6) 0.01211(15) Uani 1 1 d . . . N1 N 0.4836(2) 0.36963(18) 0.36736(19) 0.0120(5) Uani 1 1 d . . . O1 O 0.08658(17) 0.33292(19) -0.02279(15) 0.0182(4) Uani 1 1 d . . . C1 C 0.4578(3) 0.3515(2) 0.4693(2) 0.0128(5) Uani 1 1 d . . . C2 C 0.5604(3) 0.3663(2) 0.5779(2) 0.0179(7) Uani 1 1 d . . . H2A H 0.5439 0.3519 0.6493 0.021 Uiso 1 1 calc R . . C3 C 0.6865(3) 0.4019(3) 0.5822(3) 0.0249(7) Uani 1 1 d . . . H3A H 0.7567 0.4117 0.6564 0.030 Uiso 1 1 calc R . . C4 C 0.7100(3) 0.4232(3) 0.4787(3) 0.0212(7) Uani 1 1 d . . . H4A H 0.7950 0.4505 0.4807 0.025 Uiso 1 1 calc R . . C5 C 0.6076(3) 0.4039(2) 0.3717(2) 0.0144(6) Uani 1 1 d . . . C6 C 0.3128(3) 0.3235(3) 0.4586(2) 0.0165(6) Uani 1 1 d . . . C7 C 0.2222(3) 0.4244(2) 0.4034(2) 0.0154(6) Uani 1 1 d . . . H7A H 0.2427 0.4823 0.4642 0.018 Uiso 1 1 calc R . . H7B H 0.1265 0.4033 0.3850 0.018 Uiso 1 1 calc R . . C8 C 0.2611(3) 0.2181(2) 0.3856(3) 0.0167(6) Uani 1 1 d . . . H8A H 0.1881 0.1869 0.4098 0.020 Uiso 1 1 calc R . . H8B H 0.3361 0.1648 0.4073 0.020 Uiso 1 1 calc R . . C9 C 0.3033(3) 0.3037(3) 0.5818(3) 0.0241(8) Uani 1 1 d . . . H9A H 0.3642 0.2444 0.6213 0.036 Uiso 1 1 calc R . . H9B H 0.2103 0.2842 0.5732 0.036 Uiso 1 1 calc R . . H9C H 0.3294 0.3701 0.6295 0.036 Uiso 1 1 calc R . . C10 C 0.6508(3) 0.2990(2) 0.2140(3) 0.0162(6) Uani 1 1 d . . . H10A H 0.7293 0.2655 0.2757 0.019 Uiso 1 1 calc R . . H10B H 0.6698 0.3023 0.1392 0.019 Uiso 1 1 calc R . . C11 C 0.4876(3) 0.4517(2) 0.1624(2) 0.0143(6) Uani 1 1 d . . . H11A H 0.4839 0.4399 0.0800 0.017 Uiso 1 1 calc R . . H11B H 0.4709 0.5295 0.1732 0.017 Uiso 1 1 calc R . . C12 C 0.6248(3) 0.4145(2) 0.2523(2) 0.0149(6) Uani 1 1 d . . . C13 C 0.7398(3) 0.4909(3) 0.2528(3) 0.0245(7) Uani 1 1 d . . . H13A H 0.7237 0.5634 0.2792 0.037 Uiso 1 1 calc R . . H13B H 0.7433 0.4958 0.1727 0.037 Uiso 1 1 calc R . . H13C H 0.8259 0.4625 0.3070 0.037 Uiso 1 1 calc R . . C14 C 0.3347(3) 0.6063(2) 0.3218(3) 0.0220(7) Uani 1 1 d . . . H14A H 0.3436 0.6467 0.2548 0.033 Uiso 0.611(6) 1 calc PR A 1 H14B H 0.4247 0.5879 0.3775 0.033 Uiso 0.611(6) 1 calc PR A 1 H14C H 0.2870 0.6511 0.3620 0.033 Uiso 0.611(6) 1 calc PR A 1 H14D H 0.4186 0.6045 0.3042 0.033 Uiso 0.389(6) 1 calc PR A 2 H14E H 0.3562 0.6122 0.4075 0.033 Uiso 0.389(6) 1 calc PR A 2 H14F H 0.2804 0.6691 0.2825 0.033 Uiso 0.389(6) 1 calc PR A 2 C15 C 0.0718(3) 0.5380(3) 0.1876(3) 0.0210(7) Uani 1 1 d . . . H15A H 0.0295 0.5620 0.2441 0.032 Uiso 1 1 calc R . . H15B H 0.0157 0.4817 0.1360 0.032 Uiso 1 1 calc R . . H15C H 0.0803 0.5999 0.1394 0.032 Uiso 1 1 calc R . . C16 C 0.1839(3) 0.0957(2) 0.1657(3) 0.0219(7) Uani 1 1 d . . . H16A H 0.1256 0.0522 0.1964 0.033 Uiso 1 1 calc R . . H16B H 0.2740 0.0628 0.1899 0.033 Uiso 1 1 calc R . . H16C H 0.1450 0.0981 0.0790 0.033 Uiso 1 1 calc R . . C17 C 0.0161(3) 0.2591(3) 0.1906(3) 0.0224(7) Uani 1 1 d . . . H17A H -0.0225 0.2017 0.2256 0.034 Uiso 1 1 calc R . . H17B H -0.0302 0.2600 0.1046 0.034 Uiso 1 1 calc R . . H17C H 0.0047 0.3296 0.2239 0.034 Uiso 1 1 calc R . . C18 C 0.5515(3) 0.1248(2) 0.3189(3) 0.0185(7) Uani 1 1 d . . . H18A H 0.6363 0.0898 0.3225 0.028 Uiso 1 1 calc R . . H18B H 0.4817 0.0693 0.3085 0.028 Uiso 1 1 calc R . . H18C H 0.5654 0.1647 0.3926 0.028 Uiso 1 1 calc R . . C19 C 0.4809(3) 0.1282(3) 0.0703(3) 0.0207(7) Uani 1 1 d . . . H19A H 0.5514 0.0724 0.0953 0.031 Uiso 1 1 calc R . . H19B H 0.4905 0.1698 0.0042 0.031 Uiso 1 1 calc R . . H19C H 0.3918 0.0935 0.0450 0.031 Uiso 1 1 calc R . . C20 C 0.2065(3) 0.5257(2) -0.0339(2) 0.0179(6) Uani 1 1 d . . . H20A H 0.1869 0.5318 -0.1194 0.027 Uiso 1 1 calc R . . H20B H 0.2870 0.5687 0.0085 0.027 Uiso 1 1 calc R . . H20C H 0.1293 0.5529 -0.0146 0.027 Uiso 1 1 calc R . . C21 C 0.2965(3) 0.3277(3) -0.1017(2) 0.0198(6) Uani 1 1 d . . . H21A H 0.2441 0.3585 -0.1791 0.030 Uiso 1 1 calc R . . H21B H 0.2853 0.2486 -0.1041 0.030 Uiso 1 1 calc R . . H21C H 0.3923 0.3456 -0.0823 0.030 Uiso 1 1 calc R . . C22 C -0.0052(3) 0.3303(3) -0.1441(2) 0.0215(6) Uani 1 1 d . . . H22A H -0.0985 0.3259 -0.1453 0.032 Uiso 1 1 calc R . . H22B H 0.0146 0.2666 -0.1842 0.032 Uiso 1 1 calc R . . H22D H 0.0060 0.3966 -0.1849 0.032 Uiso 1 1 calc R . . O100 O -0.0188(6) 0.6601(5) 0.3973(5) 0.0672(18) Uani 0.611(6) 1 d PDU A 1 H100 H -0.0117 0.6095 0.4460 0.101 Uiso 0.611(6) 1 calc PR A 1 C100 C 0.0550(10) 0.7466(7) 0.4542(8) 0.052(2) Uani 0.611(6) 1 d PDU A 1 H10C H 0.0587 0.7475 0.5366 0.078 Uiso 0.611(6) 1 calc PR A 1 H10D H 0.0129 0.8138 0.4147 0.078 Uiso 0.611(6) 1 calc PR A 1 H10E H 0.1470 0.7410 0.4523 0.078 Uiso 0.611(6) 1 calc PR A 1 O101 O 0.0490(9) 0.7188(7) 0.4005(8) 0.038(2) Uani 0.389(6) 1 d PDU A 2 H101 H 0.0729 0.7804 0.3849 0.057 Uiso 0.389(6) 1 calc PR A 2 C101 C 0.1512(13) 0.6702(11) 0.4767(12) 0.074(3) Uani 0.389(6) 1 d PDU A 2 H10F H 0.2171 0.6512 0.4392 0.111 Uiso 0.389(6) 1 calc PR A 2 H10G H 0.1204 0.6039 0.5046 0.111 Uiso 0.389(6) 1 calc PR A 2 H10H H 0.1936 0.7187 0.5439 0.111 Uiso 0.389(6) 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 Br1 0.02187(15) 0.02468(16) 0.01448(14) -0.00173(13) 0.00919(12) -0.00049(14) Br2 0.0169(4) 0.0408(9) 0.0245(5) -0.0110(6) 0.0090(3) 0.0000(6) Br2A 0.0183(6) 0.0242(10) 0.0182(6) 0.0046(8) 0.0077(4) 0.0020(8) Fe1 0.00904(18) 0.0102(2) 0.00909(19) -0.00053(16) 0.00276(15) -0.00098(15) P1 0.0163(4) 0.0099(4) 0.0130(4) -0.0002(3) 0.0059(3) 0.0006(3) P2 0.0123(4) 0.0120(4) 0.0210(4) -0.0018(3) 0.0081(3) -0.0022(3) P3 0.0113(3) 0.0142(4) 0.0123(4) 0.0004(3) 0.0052(3) 0.0014(3) P4 0.0093(3) 0.0154(4) 0.0107(3) -0.0008(3) 0.0023(3) 0.0007(3) N1 0.0145(12) 0.0114(12) 0.0089(11) 0.0018(9) 0.0024(9) 0.0001(9) O1 0.0101(9) 0.0249(11) 0.0165(9) -0.0016(10) 0.0007(8) -0.0026(10) C1 0.0218(14) 0.0072(13) 0.0104(13) 0.0021(11) 0.0069(11) 0.0040(11) C2 0.0242(16) 0.0190(16) 0.0097(14) 0.0007(12) 0.0050(12) 0.0043(12) C3 0.0254(18) 0.0325(19) 0.0103(15) -0.0018(14) -0.0021(13) 0.0018(15) C4 0.0142(15) 0.0292(18) 0.0160(15) -0.0014(14) -0.0002(13) -0.0035(13) C5 0.0144(14) 0.0147(15) 0.0127(14) 0.0025(12) 0.0030(12) 0.0004(12) C6 0.0219(15) 0.0158(14) 0.0148(14) 0.0027(13) 0.0102(12) 0.0030(13) C7 0.0230(16) 0.0136(15) 0.0130(14) 0.0000(12) 0.0107(12) 0.0006(12) C8 0.0165(14) 0.0119(14) 0.0251(16) 0.0039(13) 0.0114(13) -0.0004(12) C9 0.0286(18) 0.029(2) 0.0208(16) 0.0068(14) 0.0159(15) 0.0066(14) C10 0.0102(14) 0.0232(17) 0.0161(14) 0.0019(12) 0.0057(12) 0.0001(11) C11 0.0119(14) 0.0157(15) 0.0131(14) -0.0019(12) 0.0016(12) -0.0031(11) C12 0.0096(14) 0.0201(16) 0.0138(14) 0.0031(12) 0.0025(11) -0.0030(12) C13 0.0158(15) 0.0321(18) 0.0254(17) 0.0052(15) 0.0069(13) -0.0072(14) C14 0.0334(18) 0.0152(16) 0.0201(16) -0.0032(13) 0.0128(14) -0.0027(13) C15 0.0214(15) 0.0199(16) 0.0227(15) 0.0043(14) 0.0088(13) 0.0083(13) C16 0.0198(16) 0.0140(15) 0.0338(18) -0.0076(14) 0.0116(14) -0.0054(13) C17 0.0134(15) 0.0244(18) 0.0306(18) -0.0047(15) 0.0090(14) -0.0044(13) C18 0.0175(15) 0.0183(16) 0.0212(16) 0.0075(13) 0.0085(13) 0.0055(12) C19 0.0216(17) 0.0191(16) 0.0231(17) -0.0043(13) 0.0100(14) 0.0024(13) C20 0.0187(15) 0.0186(15) 0.0145(14) 0.0016(13) 0.0033(12) 0.0018(13) C21 0.0177(14) 0.0284(17) 0.0131(13) -0.0042(14) 0.0052(11) 0.0075(15) C22 0.0125(13) 0.0219(16) 0.0234(15) -0.0035(15) -0.0024(12) -0.0042(14) O100 0.076(4) 0.065(4) 0.053(3) -0.001(3) 0.013(3) 0.005(3) C100 0.052(4) 0.044(4) 0.053(5) -0.001(4) 0.008(4) 0.000(3) O101 0.044(4) 0.022(4) 0.053(5) 0.005(4) 0.022(4) -0.018(3) C101 0.077(5) 0.066(5) 0.077(6) -0.003(5) 0.026(5) -0.006(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 N1 2.010(2) . ? Fe1 C11 2.061(3) . ? Fe1 P4 2.2292(9) . ? Fe1 P1 2.2662(8) . ? Fe1 P2 2.2851(8) . ? Fe1 P3 2.2980(8) . ? P1 C14 1.813(3) . ? P1 C15 1.832(3) . ? P1 C7 1.843(3) . ? P2 C16 1.811(3) . ? P2 C8 1.833(3) . ? P2 C17 1.836(3) . ? P3 C19 1.821(3) . ? P3 C10 1.831(3) . ? P3 C18 1.833(3) . ? P4 O1 1.6199(19) . ? P4 C21 1.814(3) . ? P4 C20 1.816(3) . ? N1 C5 1.358(4) . ? N1 C1 1.365(3) . ? O1 C22 1.445(3) . ? C1 C2 1.389(4) . ? C1 C6 1.530(4) . ? C2 C3 1.384(4) . ? C2 H2A 0.9500 . ? C3 C4 1.378(4) . ? C3 H3A 0.9500 . ? C4 C5 1.385(4) . ? C4 H4A 0.9500 . ? C5 C12 1.516(4) . ? C6 C9 1.541(4) . ? C6 C8 1.556(4) . ? C6 C7 1.567(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.547(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.545(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.533(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22D 0.9800 . ? O100 C100 1.355(7) . ? O100 H100 0.8400 . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? O101 C101 1.294(12) . ? O101 H101 0.8400 . ? C101 H10F 0.9800 . ? C101 H10G 0.9800 . ? C101 H10H 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 C11 82.36(10) . . ? N1 Fe1 P4 161.70(7) . . ? C11 Fe1 P4 80.38(8) . . ? N1 Fe1 P1 81.51(7) . . ? C11 Fe1 P1 99.52(9) . . ? P4 Fe1 P1 95.36(3) . . ? N1 Fe1 P2 103.06(7) . . ? C11 Fe1 P2 172.33(8) . . ? P4 Fe1 P2 94.72(3) . . ? P1 Fe1 P2 86.75(3) . . ? N1 Fe1 P3 81.93(7) . . ? C11 Fe1 P3 82.43(8) . . ? P4 Fe1 P3 101.70(3) . . ? P1 Fe1 P3 162.91(3) . . ? P2 Fe1 P3 92.87(3) . . ? C14 P1 C15 100.86(15) . . ? C14 P1 C7 102.99(14) . . ? C15 P1 C7 103.77(14) . . ? C14 P1 Fe1 114.98(11) . . ? C15 P1 Fe1 126.34(10) . . ? C7 P1 Fe1 105.28(9) . . ? C16 P2 C8 105.79(14) . . ? C16 P2 C17 98.45(15) . . ? C8 P2 C17 102.87(14) . . ? C16 P2 Fe1 121.60(11) . . ? C8 P2 Fe1 99.94(9) . . ? C17 P2 Fe1 125.53(11) . . ? C19 P3 C10 105.64(14) . . ? C19 P3 C18 101.19(14) . . ? C10 P3 C18 102.83(13) . . ? C19 P3 Fe1 127.19(10) . . ? C10 P3 Fe1 100.83(10) . . ? C18 P3 Fe1 116.34(10) . . ? O1 P4 C21 103.32(12) . . ? O1 P4 C20 104.13(12) . . ? C21 P4 C20 102.67(14) . . ? O1 P4 Fe1 108.54(8) . . ? C21 P4 Fe1 120.37(10) . . ? C20 P4 Fe1 116.02(9) . . ? C5 N1 C1 120.4(2) . . ? C5 N1 Fe1 113.62(18) . . ? C1 N1 Fe1 125.93(19) . . ? C22 O1 P4 120.80(18) . . ? N1 C1 C2 119.5(3) . . ? N1 C1 C6 117.8(2) . . ? C2 C1 C6 122.5(3) . . ? C3 C2 C1 120.0(3) . . ? C3 C2 H2A 120.0 . . ? C1 C2 H2A 120.0 . . ? C4 C3 C2 120.0(3) . . ? C4 C3 H3A 120.0 . . ? C2 C3 H3A 120.0 . . ? C3 C4 C5 118.8(3) . . ? C3 C4 H4A 120.6 . . ? C5 C4 H4A 120.6 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 C12 114.9(2) . . ? C4 C5 C12 123.8(3) . . ? C1 C6 C9 110.6(2) . . ? C1 C6 C8 112.3(2) . . ? C9 C6 C8 106.6(2) . . ? C1 C6 C7 107.6(2) . . ? C9 C6 C7 107.5(2) . . ? C8 C6 C7 112.2(2) . . ? C6 C7 P1 116.6(2) . . ? C6 C7 H7A 108.1 . . ? P1 C7 H7A 108.1 . . ? C6 C7 H7B 108.1 . . ? P1 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C6 C8 P2 116.52(19) . . ? C6 C8 H8A 108.2 . . ? P2 C8 H8A 108.2 . . ? C6 C8 H8B 108.2 . . ? P2 C8 H8B 108.2 . . ? H8A C8 H8B 107.3 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 P3 106.93(19) . . ? C12 C10 H10A 110.3 . . ? P3 C10 H10A 110.3 . . ? C12 C10 H10B 110.3 . . ? P3 C10 H10B 110.3 . . ? H10A C10 H10B 108.6 . . ? C12 C11 Fe1 103.26(18) . . ? C12 C11 H11A 111.1 . . ? Fe1 C11 H11A 111.1 . . ? C12 C11 H11B 111.1 . . ? Fe1 C11 H11B 111.1 . . ? H11A C11 H11B 109.1 . . ? C5 C12 C13 113.8(2) . . ? C5 C12 C11 107.4(2) . . ? C13 C12 C11 111.7(2) . . ? C5 C12 C10 107.2(2) . . ? C13 C12 C10 110.0(2) . . ? C11 C12 C10 106.4(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? P1 C14 H14D 109.5 . . ? P1 C14 H14E 109.5 . . ? H14D C14 H14E 109.5 . . ? P1 C14 H14F 109.5 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P3 C18 H18A 109.5 . . ? P3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P3 C19 H19A 109.5 . . ? P3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P4 C20 H20A 109.5 . . ? P4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P4 C21 H21A 109.5 . . ? P4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O1 C22 H22A 109.5 . . ? O1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? O1 C22 H22D 109.5 . . ? H22A C22 H22D 109.5 . . ? H22B C22 H22D 109.5 . . ? O100 C100 H10C 109.5 . . ? O100 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? O100 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C101 O101 H101 109.5 . . ? O101 C101 H10F 109.5 . . ? O101 C101 H10G 109.5 . . ? H10F C101 H10G 109.5 . . ? O101 C101 H10H 109.5 . . ? H10F C101 H10H 109.5 . . ? H10G C101 H10H 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O100 H100 Br2 0.84 2.20 2.973(7) 152.5 . O101 H101 Br2 0.84 3.49 4.108(9) 133.4 2_556 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.483 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.071 # Attachment '5 (CCDC-612672).cif' data_xmh171 _database_code_depnum_ccdc_archive 'CCDC 612672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H47 B2 F8 Fe N O P4' _chemical_formula_weight 706.97 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 10.9275(9) _cell_length_b 12.1691(19) _cell_length_c 23.218(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3087.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6962 _cell_measurement_theta_min 3.0529 _cell_measurement_theta_max 28.7010 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8939 _exptl_absorpt_correction_T_max 0.9414 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14703 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0733 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 28.80 _reflns_number_total 6515 _reflns_number_gt 4846 _reflns_threshold_expression >2sigma(I) _diffrn_orient_matrix_UB_11 -0.0101034138 _diffrn_orient_matrix_UB_12 -0.0507775276 _diffrn_orient_matrix_UB_13 0.0143099676 _diffrn_orient_matrix_UB_21 -0.0239084982 _diffrn_orient_matrix_UB_22 0.0286448995 _diffrn_orient_matrix_UB_23 0.0241294118 _diffrn_orient_matrix_UB_31 -0.0595089541 _diffrn_orient_matrix_UB_32 -0.0029481511 _diffrn_orient_matrix_UB_33 -0.0121051444 _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^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 constrained _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 0.038(19) _refine_ls_number_reflns 6515 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1087 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5212(3) 0.4807(4) 0.76459(15) 0.0243(8) Uani 1 1 d . . . C2 C 0.4619(3) 0.4732(4) 0.71269(16) 0.0301(8) Uani 1 1 d . . . H2 H 0.5049 0.4882 0.6780 0.036 Uiso 1 1 calc R . . C3 C 0.3396(4) 0.4437(3) 0.71078(17) 0.0324(10) Uani 1 1 d . . . H3 H 0.2974 0.4411 0.6750 0.039 Uiso 1 1 calc R . . C4 C 0.2804(4) 0.4184(4) 0.76058(17) 0.0313(10) Uani 1 1 d . . . H4 H 0.1980 0.3937 0.7597 0.038 Uiso 1 1 calc R . . C5 C 0.3412(3) 0.4291(3) 0.81252(16) 0.0271(9) Uani 1 1 d . . . C6 C 0.6577(3) 0.5114(3) 0.76694(15) 0.0276(9) Uani 1 1 d . . . C7 C 0.7310(4) 0.4141(4) 0.79209(17) 0.0336(10) Uani 1 1 d . . . H7A H 0.8147 0.4400 0.8011 0.040 Uiso 1 1 calc R . . H7B H 0.7383 0.3568 0.7620 0.040 Uiso 1 1 calc R . . C8 C 0.6787(4) 0.6177(4) 0.80217(17) 0.0319(10) Uani 1 1 d . . . H8A H 0.6167 0.6726 0.7903 0.038 Uiso 1 1 calc R . . H8B H 0.7601 0.6477 0.7920 0.038 Uiso 1 1 calc R . . C9 C 0.7082(3) 0.5327(4) 0.70612(17) 0.0379(10) Uani 1 1 d . . . H9A H 0.6670 0.5966 0.6893 0.057 Uiso 1 1 calc R . . H9B H 0.6935 0.4681 0.6819 0.057 Uiso 1 1 calc R . . H9C H 0.7964 0.5468 0.7084 0.057 Uiso 1 1 calc R . . C10 C 0.2767(3) 0.4045(4) 0.86925(16) 0.0306(9) Uani 1 1 d . . . C11 C 0.3579(4) 0.3298(4) 0.90692(18) 0.0348(10) Uani 1 1 d . . . H11A H 0.3646 0.2571 0.8890 0.052 Uiso 1 1 calc R . . H11B H 0.3212 0.3224 0.9452 0.052 Uiso 1 1 calc R . . H11C H 0.4396 0.3624 0.9105 0.052 Uiso 1 1 calc R . . C12 C 0.2481(3) 0.5118(4) 0.90061(17) 0.0349(10) Uani 1 1 d . . . H12A H 0.2147 0.4949 0.9392 0.042 Uiso 1 1 calc R . . H12B H 0.1848 0.5526 0.8789 0.042 Uiso 1 1 calc R . . C13 C 0.1549(4) 0.3432(4) 0.86101(19) 0.0427(12) Uani 1 1 d . . . H13A H 0.0994 0.3883 0.8378 0.064 Uiso 1 1 calc R . . H13B H 0.1177 0.3290 0.8987 0.064 Uiso 1 1 calc R . . H13C H 0.1700 0.2733 0.8413 0.064 Uiso 1 1 calc R . . C14 C 0.5898(4) 0.2301(4) 0.82727(19) 0.0393(11) Uani 1 1 d . . . H14A H 0.6478 0.1881 0.8038 0.059 Uiso 1 1 calc R . . H14B H 0.5210 0.2538 0.8032 0.059 Uiso 1 1 calc R . . H14C H 0.5593 0.1837 0.8587 0.059 Uiso 1 1 calc R . . C15 C 0.7973(4) 0.2809(4) 0.8895(2) 0.0452(12) Uani 1 1 d . . . H15A H 0.7684 0.2221 0.9150 0.068 Uiso 1 1 calc R . . H15B H 0.8453 0.3339 0.9119 0.068 Uiso 1 1 calc R . . H15C H 0.8486 0.2495 0.8591 0.068 Uiso 1 1 calc R . . C16 C 0.8283(4) 0.5810(4) 0.90227(18) 0.0419(11) Uani 1 1 d . . . H16A H 0.8540 0.5064 0.8920 0.063 Uiso 1 1 calc R . . H16B H 0.8349 0.5908 0.9441 0.063 Uiso 1 1 calc R . . H16C H 0.8812 0.6344 0.8828 0.063 Uiso 1 1 calc R . . C17 C 0.6527(4) 0.7426(4) 0.90628(18) 0.0399(11) Uani 1 1 d . . . H17A H 0.7239 0.7865 0.8949 0.060 Uiso 1 1 calc R . . H17B H 0.6458 0.7419 0.9484 0.060 Uiso 1 1 calc R . . H17C H 0.5785 0.7747 0.8896 0.060 Uiso 1 1 calc R . . C18 C 0.3611(4) 0.6997(4) 0.85147(18) 0.0382(11) Uani 1 1 d . . . H18A H 0.2732 0.7097 0.8447 0.057 Uiso 1 1 calc R . . H18B H 0.4002 0.6739 0.8160 0.057 Uiso 1 1 calc R . . H18C H 0.3975 0.7698 0.8631 0.057 Uiso 1 1 calc R . . C19 C 0.3524(4) 0.6796(4) 0.97217(18) 0.0426(12) Uani 1 1 d . . . H19A H 0.4197 0.7314 0.9786 0.064 Uiso 1 1 calc R . . H19B H 0.3447 0.6309 1.0056 0.064 Uiso 1 1 calc R . . H19C H 0.2759 0.7203 0.9668 0.064 Uiso 1 1 calc R . . C20 C 0.4699(4) 0.4015(5) 1.03343(17) 0.0431(11) Uani 1 1 d . . . H20A H 0.4915 0.4112 1.0741 0.065 Uiso 1 1 calc R . . H20B H 0.4667 0.3229 1.0243 0.065 Uiso 1 1 calc R . . H20C H 0.3897 0.4346 1.0261 0.065 Uiso 1 1 calc R . . C21 C 0.7160(4) 0.3905(5) 1.0126(2) 0.0538(15) Uani 1 1 d . . . H21A H 0.7887 0.4153 0.9916 0.081 Uiso 1 1 calc R . . H21B H 0.7028 0.3121 1.0052 0.081 Uiso 1 1 calc R . . H21C H 0.7281 0.4023 1.0540 0.081 Uiso 1 1 calc R . . P1 P 0.66641(9) 0.35030(10) 0.85727(5) 0.0292(3) Uani 1 1 d . . . P2 P 0.67102(10) 0.60213(10) 0.88008(4) 0.0300(2) Uani 1 1 d . . . P3 P 0.38387(9) 0.59836(10) 0.90844(4) 0.0291(2) Uani 1 1 d . . . P4 P 0.58406(9) 0.46751(11) 0.98862(5) 0.0337(3) Uani 1 1 d . . . Fe1 Fe 0.53619(5) 0.47551(5) 0.89648(2) 0.02452(14) Uani 1 1 d . . . N1 N 0.4612(3) 0.4620(3) 0.81492(12) 0.0238(7) Uani 1 1 d . . . B1 B 0.0373(5) 0.6373(6) 0.7513(3) 0.063(2) Uani 1 1 d . . . B2 B 0.5516(4) 0.0341(6) 0.9603(2) 0.0425(13) Uani 1 1 d . . . F1 F 0.0101(2) 0.5525(3) 0.78601(14) 0.0668(9) Uani 1 1 d . . . F2 F 0.1563(3) 0.6678(3) 0.75528(14) 0.0701(9) Uani 1 1 d . . . F3 F 0.0222(4) 0.5971(5) 0.69318(15) 0.127(2) Uani 1 1 d . . . F4 F -0.0435(3) 0.7206(3) 0.75954(19) 0.0937(13) Uani 1 1 d . . . F5 F 0.5472(4) 0.1338(4) 0.9837(2) 0.1284(18) Uani 1 1 d . . . F6 F 0.6663(3) 0.0157(3) 0.93836(13) 0.0722(9) Uani 1 1 d . . . F7 F 0.5304(3) -0.0437(5) 1.00177(14) 0.1128(18) Uani 1 1 d . . . F8 F 0.4670(2) 0.0237(4) 0.91798(11) 0.0818(12) Uani 1 1 d . . . O1 O 0.6031(3) 0.5861(3) 1.01640(13) 0.0487(8) Uani 1 1 d . . . C22 C 0.6370(9) 0.5930(8) 1.0780(3) 0.128(3) Uani 1 1 d . . . H22A H 0.7160 0.6325 1.0809 0.153 Uiso 1 1 calc R . . H22B H 0.6506 0.5174 1.0924 0.153 Uiso 1 1 calc R . . C23 C 0.5444(8) 0.6502(13) 1.1186(5) 0.266(10) Uani 1 1 d . . . H23A H 0.5864 0.6738 1.1538 0.400 Uiso 1 1 calc R . . H23B H 0.4789 0.5987 1.1285 0.400 Uiso 1 1 calc R . . H23C H 0.5094 0.7144 1.0991 0.400 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 C1 0.0262(18) 0.0209(19) 0.0257(19) 0.0006(18) 0.0041(15) 0.0009(19) C2 0.0321(19) 0.032(2) 0.0260(18) 0.001(2) 0.0034(16) -0.001(2) C3 0.037(2) 0.032(3) 0.028(2) -0.0025(19) -0.0065(18) 0.006(2) C4 0.0270(19) 0.032(2) 0.035(2) -0.005(2) -0.0002(17) -0.0001(19) C5 0.0203(18) 0.028(2) 0.033(2) 0.0039(19) -0.0008(16) 0.0021(18) C6 0.0259(18) 0.028(2) 0.030(2) 0.0039(19) 0.0017(16) -0.0015(19) C7 0.025(2) 0.041(3) 0.035(2) -0.003(2) 0.0031(17) -0.001(2) C8 0.031(2) 0.032(3) 0.033(2) 0.008(2) 0.0024(17) -0.004(2) C9 0.035(2) 0.044(3) 0.034(2) 0.004(2) 0.0088(17) -0.004(2) C10 0.0275(19) 0.039(3) 0.025(2) 0.003(2) 0.0015(15) -0.002(2) C11 0.030(2) 0.035(3) 0.039(2) 0.009(2) 0.0015(18) -0.0090(19) C12 0.0256(18) 0.047(3) 0.032(2) -0.002(2) 0.0035(16) 0.001(2) C13 0.027(2) 0.059(3) 0.042(2) 0.008(3) 0.0017(19) -0.005(2) C14 0.036(2) 0.031(3) 0.051(3) -0.001(2) 0.007(2) 0.000(2) C15 0.040(2) 0.048(3) 0.048(3) 0.015(3) 0.003(2) 0.011(2) C16 0.032(2) 0.052(3) 0.042(2) 0.005(2) -0.010(2) -0.008(2) C17 0.054(2) 0.034(3) 0.032(2) -0.001(2) -0.007(2) -0.007(2) C18 0.039(2) 0.039(3) 0.036(2) 0.002(2) -0.0009(19) 0.008(2) C19 0.047(3) 0.049(3) 0.032(2) -0.011(2) -0.002(2) 0.012(2) C20 0.048(3) 0.056(3) 0.026(2) 0.007(2) 0.0040(19) -0.001(3) C21 0.042(3) 0.080(4) 0.039(3) 0.016(3) -0.010(2) 0.012(3) P1 0.0258(5) 0.0276(6) 0.0343(5) 0.0066(5) 0.0010(4) 0.0031(5) P2 0.0299(5) 0.0303(6) 0.0298(5) 0.0055(5) -0.0040(4) -0.0044(5) P3 0.0321(5) 0.0316(6) 0.0236(5) -0.0013(5) -0.0003(4) 0.0053(5) P4 0.0315(5) 0.0412(7) 0.0285(5) 0.0081(6) -0.0055(4) -0.0003(6) Fe1 0.0236(3) 0.0258(3) 0.0241(3) 0.0041(3) -0.0013(2) 0.0003(3) N1 0.0239(14) 0.0233(18) 0.0241(15) 0.0032(15) 0.0020(12) 0.0019(16) B1 0.033(3) 0.076(5) 0.081(5) 0.033(4) -0.008(3) -0.003(3) B2 0.035(3) 0.061(4) 0.031(2) -0.003(3) -0.001(2) 0.002(3) F1 0.0557(17) 0.067(2) 0.077(2) 0.0322(19) 0.0104(15) -0.0057(16) F2 0.0387(15) 0.080(2) 0.092(2) 0.017(2) -0.0025(15) -0.0179(17) F3 0.109(3) 0.214(6) 0.057(2) 0.004(3) -0.006(2) -0.061(4) F4 0.058(2) 0.076(3) 0.147(4) 0.037(3) -0.003(2) 0.020(2) F5 0.117(3) 0.108(4) 0.159(4) -0.083(3) -0.028(3) 0.028(3) F6 0.0455(15) 0.078(2) 0.093(2) 0.013(2) 0.0181(15) -0.0023(17) F7 0.067(2) 0.204(5) 0.067(2) 0.069(3) -0.0109(17) -0.045(3) F8 0.0594(17) 0.155(4) 0.0308(13) -0.012(2) -0.0086(13) 0.002(2) O1 0.062(2) 0.048(2) 0.0359(16) 0.0027(17) -0.0171(15) -0.0120(19) C22 0.191(9) 0.105(6) 0.087(5) -0.007(5) -0.058(6) -0.042(7) C23 0.111(7) 0.41(2) 0.280(15) -0.305(16) -0.060(8) 0.091(10) _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 C1 N1 1.359(4) . ? C1 C2 1.371(5) . ? C1 C6 1.539(5) . ? C2 C3 1.385(6) . ? C3 C4 1.360(6) . ? C4 C5 1.383(5) . ? C5 N1 1.372(5) . ? C5 C10 1.523(5) . ? C6 C9 1.538(5) . ? C6 C7 1.545(6) . ? C6 C8 1.548(6) . ? C7 P1 1.842(4) . ? C8 P2 1.821(4) . ? C10 C12 1.528(6) . ? C10 C13 1.538(6) . ? C10 C11 1.542(6) . ? C12 P3 1.828(4) . ? C14 P1 1.824(5) . ? C15 P1 1.822(4) . ? C16 P2 1.813(4) . ? C17 P2 1.825(5) . ? C18 P3 1.825(4) . ? C19 P3 1.812(4) . ? C20 P4 1.813(4) . ? C21 P4 1.808(5) . ? P1 Fe1 2.2750(13) . ? P2 Fe1 2.1657(12) . ? P3 Fe1 2.2545(12) . ? P4 O1 1.594(4) . ? P4 Fe1 2.2044(12) . ? Fe1 N1 2.070(3) . ? B1 F1 1.342(7) . ? B1 F2 1.355(6) . ? B1 F4 1.358(8) . ? B1 F3 1.445(9) . ? B2 F5 1.330(7) . ? B2 F8 1.356(6) . ? B2 F7 1.371(7) . ? B2 F6 1.371(6) . ? O1 C22 1.480(7) . ? C22 C23 1.547(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 121.1(3) . . ? N1 C1 C6 118.6(3) . . ? C2 C1 C6 120.3(3) . . ? C1 C2 C3 120.1(4) . . ? C4 C3 C2 119.4(4) . . ? C3 C4 C5 119.5(4) . . ? N1 C5 C4 121.4(3) . . ? N1 C5 C10 117.6(3) . . ? C4 C5 C10 120.9(3) . . ? C9 C6 C1 110.9(3) . . ? C9 C6 C7 106.8(3) . . ? C1 C6 C7 109.2(3) . . ? C9 C6 C8 107.0(3) . . ? C1 C6 C8 111.4(3) . . ? C7 C6 C8 111.4(3) . . ? C6 C7 P1 115.8(3) . . ? C6 C8 P2 115.5(3) . . ? C5 C10 C12 109.8(4) . . ? C5 C10 C13 112.8(3) . . ? C12 C10 C13 107.3(3) . . ? C5 C10 C11 109.9(3) . . ? C12 C10 C11 110.6(3) . . ? C13 C10 C11 106.4(3) . . ? C10 C12 P3 111.9(3) . . ? C15 P1 C14 98.4(2) . . ? C15 P1 C7 103.4(2) . . ? C14 P1 C7 101.6(2) . . ? C15 P1 Fe1 129.54(17) . . ? C14 P1 Fe1 113.75(14) . . ? C7 P1 Fe1 106.64(15) . . ? C16 P2 C8 104.7(2) . . ? C16 P2 C17 98.2(2) . . ? C8 P2 C17 103.8(2) . . ? C16 P2 Fe1 119.62(17) . . ? C8 P2 Fe1 106.27(14) . . ? C17 P2 Fe1 122.21(15) . . ? C19 P3 C18 101.4(2) . . ? C19 P3 C12 104.0(2) . . ? C18 P3 C12 101.9(2) . . ? C19 P3 Fe1 127.02(16) . . ? C18 P3 Fe1 117.35(15) . . ? C12 P3 Fe1 101.82(14) . . ? O1 P4 C21 103.9(2) . . ? O1 P4 C20 105.0(2) . . ? C21 P4 C20 98.2(2) . . ? O1 P4 Fe1 112.56(12) . . ? C21 P4 Fe1 120.73(17) . . ? C20 P4 Fe1 114.41(15) . . ? N1 Fe1 P2 99.51(9) . . ? N1 Fe1 P4 168.01(10) . . ? P2 Fe1 P4 92.33(5) . . ? N1 Fe1 P3 82.70(9) . . ? P2 Fe1 P3 92.99(5) . . ? P4 Fe1 P3 94.87(4) . . ? N1 Fe1 P1 80.12(9) . . ? P2 Fe1 P1 88.89(5) . . ? P4 Fe1 P1 102.14(5) . . ? P3 Fe1 P1 162.79(4) . . ? C1 N1 C5 118.4(3) . . ? C1 N1 Fe1 125.6(2) . . ? C5 N1 Fe1 116.0(2) . . ? F1 B1 F2 112.5(5) . . ? F1 B1 F4 110.2(5) . . ? F2 B1 F4 114.2(6) . . ? F1 B1 F3 106.0(6) . . ? F2 B1 F3 105.4(5) . . ? F4 B1 F3 108.0(5) . . ? F5 B2 F8 110.9(5) . . ? F5 B2 F7 109.7(5) . . ? F8 B2 F7 109.2(5) . . ? F5 B2 F6 109.6(5) . . ? F8 B2 F6 109.8(4) . . ? F7 B2 F6 107.6(5) . . ? C22 O1 P4 118.4(4) . . ? O1 C22 C23 116.8(8) . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 28.80 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 0.671 _refine_diff_density_min -0.468 _refine_diff_density_rms 0.071 # Attachment '2 (CCDC-612673)neu.cif' data_xmh172 _database_code_depnum_ccdc_archive 'CCDC 612673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H43 B F4 Fe N O P4' _chemical_formula_weight 592.10 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_cell_setting orthorhombic 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 10.933(3) _cell_length_b 12.2962(9) _cell_length_c 22.860(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3073.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9843 _cell_measurement_theta_min 3.0578 _cell_measurement_theta_max 28.7144 _exptl_crystal_description bipyramidal _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8429 _exptl_absorpt_correction_T_max 0.8975 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 16.3031 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18867 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0654 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 28.76 _reflns_number_total 6883 _reflns_number_gt 5176 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0798P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.02(2) _refine_ls_number_reflns 6883 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0554 _refine_ls_R_factor_gt 0.0430 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1291 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5257(3) 0.4980(3) 0.23744(15) 0.0225(7) Uani 1 1 d . . . C2 C 0.4708(4) 0.5038(4) 0.29222(16) 0.0291(9) Uani 1 1 d . . . H2 H 0.5174 0.4873 0.3262 0.035 Uiso 1 1 calc R . . C3 C 0.3498(4) 0.5332(3) 0.29791(17) 0.0306(10) Uani 1 1 d . . . H3 H 0.3119 0.5349 0.3353 0.037 Uiso 1 1 calc R . . C4 C 0.2846(4) 0.5604(4) 0.24798(18) 0.0327(10) Uani 1 1 d . . . H4 H 0.2024 0.5846 0.2511 0.039 Uiso 1 1 calc R . . C5 C 0.3391(4) 0.5522(3) 0.19385(17) 0.0262(9) Uani 1 1 d . . . C6 C 0.6616(4) 0.4677(3) 0.23105(16) 0.0257(9) Uani 1 1 d . . . C7 C 0.7306(4) 0.5659(4) 0.20281(18) 0.0293(10) Uani 1 1 d . . . H7A H 0.8137 0.5413 0.1919 0.035 Uiso 1 1 calc R . . H7B H 0.7399 0.6230 0.2330 0.035 Uiso 1 1 calc R . . C8 C 0.6772(4) 0.3615(3) 0.19481(15) 0.0238(9) Uani 1 1 d . . . H8A H 0.6178 0.3070 0.2093 0.029 Uiso 1 1 calc R . . H8B H 0.7602 0.3322 0.2020 0.029 Uiso 1 1 calc R . . C9 C 0.7221(4) 0.4445(4) 0.29126(18) 0.0366(11) Uani 1 1 d . . . H9A H 0.7134 0.5084 0.3165 0.055 Uiso 1 1 calc R . . H9B H 0.8091 0.4284 0.2856 0.055 Uiso 1 1 calc R . . H9C H 0.6819 0.3820 0.3096 0.055 Uiso 1 1 calc R . . C10 C 0.2677(4) 0.5797(4) 0.13822(18) 0.0311(10) Uani 1 1 d . . . C11 C 0.3462(4) 0.6501(4) 0.09846(19) 0.0341(10) Uani 1 1 d . . . H11A H 0.3593 0.7211 0.1168 0.051 Uiso 1 1 calc R . . H11B H 0.3047 0.6599 0.0608 0.051 Uiso 1 1 calc R . . H11C H 0.4253 0.6145 0.0921 0.051 Uiso 1 1 calc R . . C12 C 0.2322(4) 0.4724(4) 0.10623(19) 0.0331(11) Uani 1 1 d . . . H12A H 0.1973 0.4897 0.0674 0.040 Uiso 1 1 calc R . . H12B H 0.1691 0.4334 0.1292 0.040 Uiso 1 1 calc R . . C13 C 0.1467(4) 0.6425(4) 0.1509(2) 0.0447(13) Uani 1 1 d . . . H13A H 0.0932 0.5976 0.1753 0.067 Uiso 1 1 calc R . . H13B H 0.1054 0.6590 0.1139 0.067 Uiso 1 1 calc R . . H13C H 0.1656 0.7105 0.1714 0.067 Uiso 1 1 calc R . . C14 C 0.5896(5) 0.7468(3) 0.17139(18) 0.0338(10) Uani 1 1 d . . . H14A H 0.6511 0.7877 0.1935 0.051 Uiso 1 1 calc R . . H14B H 0.5239 0.7237 0.1978 0.051 Uiso 1 1 calc R . . H14C H 0.5555 0.7931 0.1406 0.051 Uiso 1 1 calc R . . C15 C 0.7886(4) 0.6914(4) 0.1021(2) 0.0371(11) Uani 1 1 d . . . H15A H 0.7584 0.7388 0.0708 0.056 Uiso 1 1 calc R . . H15B H 0.8417 0.6353 0.0854 0.056 Uiso 1 1 calc R . . H15C H 0.8350 0.7347 0.1304 0.056 Uiso 1 1 calc R . . C16 C 0.8104(4) 0.3960(4) 0.08768(18) 0.0315(10) Uani 1 1 d . . . H16A H 0.8671 0.3485 0.1089 0.047 Uiso 1 1 calc R . . H16B H 0.8350 0.4720 0.0929 0.047 Uiso 1 1 calc R . . H16C H 0.8120 0.3776 0.0460 0.047 Uiso 1 1 calc R . . C17 C 0.6303(4) 0.2395(3) 0.09124(18) 0.0314(10) Uani 1 1 d . . . H17A H 0.7044 0.1962 0.0976 0.047 Uiso 1 1 calc R . . H17B H 0.6103 0.2402 0.0495 0.047 Uiso 1 1 calc R . . H17C H 0.5623 0.2075 0.1132 0.047 Uiso 1 1 calc R . . C18 C 0.3482(4) 0.2898(4) 0.15757(18) 0.0330(10) Uani 1 1 d . . . H18A H 0.2661 0.2578 0.1559 0.050 Uiso 1 1 calc R . . H18B H 0.3587 0.3281 0.1948 0.050 Uiso 1 1 calc R . . H18C H 0.4096 0.2320 0.1544 0.050 Uiso 1 1 calc R . . C19 C 0.3288(5) 0.3007(4) 0.03528(19) 0.0430(12) Uani 1 1 d . . . H19A H 0.2498 0.2653 0.0422 0.064 Uiso 1 1 calc R . . H19B H 0.3922 0.2452 0.0300 0.064 Uiso 1 1 calc R . . H19C H 0.3237 0.3458 0.0000 0.064 Uiso 1 1 calc R . . C20 C 0.4376(4) 0.5684(4) -0.03586(18) 0.0334(11) Uani 1 1 d . . . H20A H 0.4483 0.5467 -0.0768 0.050 Uiso 1 1 calc R . . H20B H 0.4412 0.6478 -0.0329 0.050 Uiso 1 1 calc R . . H20C H 0.3581 0.5427 -0.0217 0.050 Uiso 1 1 calc R . . C21 C 0.6852(4) 0.5816(4) -0.0219(2) 0.0389(11) Uani 1 1 d . . . H21A H 0.7609 0.5579 -0.0027 0.058 Uiso 1 1 calc R . . H21B H 0.6736 0.6597 -0.0155 0.058 Uiso 1 1 calc R . . H21C H 0.6905 0.5670 -0.0639 0.058 Uiso 1 1 calc R . . N1 N 0.4583(3) 0.5189(3) 0.18794(13) 0.0222(7) Uani 1 1 d . . . P1 P 0.66051(10) 0.62757(9) 0.13851(4) 0.0249(2) Uani 1 1 d . . . P2 P 0.65605(10) 0.37701(9) 0.11602(4) 0.0236(2) Uani 1 1 d . . . P3 P 0.36711(9) 0.38530(9) 0.09730(5) 0.0253(2) Uani 1 1 d . . . P4 P 0.55873(9) 0.50888(10) 0.00829(4) 0.0244(2) Uani 1 1 d . . . Fe1 Fe 0.52207(5) 0.50549(5) 0.10358(2) 0.01987(14) Uani 1 1 d . . . O1 O 0.5744(3) 0.3875(2) -0.01731(12) 0.0356(7) Uani 1 1 d . . . H1 H 0.5581 0.3874 -0.0532 0.053 Uiso 1 1 calc R . . B1A B 0.5059(11) 0.3275(11) 0.8282(5) 0.027(3) Uiso 0.607(15) 1 d P A 1 F1A F 0.5228(6) 0.2215(6) 0.8233(3) 0.068(2) Uiso 0.607(15) 1 d P A 1 F2A F 0.3989(6) 0.3640(6) 0.8606(3) 0.0537(19) Uiso 0.607(15) 1 d P A 1 F3A F 0.5215(5) 0.3734(7) 0.7749(2) 0.0541(19) Uiso 0.607(15) 1 d P A 1 F4A F 0.5984(6) 0.3884(7) 0.8669(2) 0.0466(19) Uiso 0.607(15) 1 d P A 1 B1B B 0.5074(18) 0.3566(18) 0.8308(8) 0.036(6) Uiso 0.393(15) 1 d P A 2 F1B F 0.3967(8) 0.3368(8) 0.8469(4) 0.035(2) Uiso 0.393(15) 1 d P A 2 F2B F 0.6002(7) 0.3532(8) 0.8665(3) 0.022(2) Uiso 0.393(15) 1 d P A 2 F3B F 0.5126(7) 0.4255(9) 0.7830(3) 0.038(3) Uiso 0.393(15) 1 d P A 2 F4B F 0.5171(14) 0.2504(14) 0.7985(8) 0.121(6) Uiso 0.393(15) 1 d P 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 C1 0.0261(19) 0.0170(18) 0.0244(18) -0.0055(16) 0.0001(14) -0.002(2) C2 0.040(2) 0.023(2) 0.0246(19) 0.0034(17) -0.0062(16) -0.008(2) C3 0.040(3) 0.028(2) 0.024(2) -0.0035(15) 0.0103(18) -0.006(2) C4 0.028(2) 0.036(3) 0.034(2) -0.0076(19) 0.0116(18) 0.002(2) C5 0.027(2) 0.024(2) 0.027(2) -0.0026(16) 0.0015(18) -0.0026(19) C6 0.027(2) 0.030(2) 0.0205(19) 0.0023(15) -0.0074(16) -0.0055(18) C7 0.023(2) 0.036(3) 0.029(2) 0.0064(18) -0.0058(17) -0.011(2) C8 0.029(2) 0.020(2) 0.0228(19) 0.0033(15) -0.0055(16) 0.0026(19) C9 0.034(3) 0.044(3) 0.032(3) 0.0024(19) -0.0082(19) -0.011(2) C10 0.024(2) 0.040(3) 0.029(2) -0.0059(19) 0.0010(17) 0.006(2) C11 0.026(2) 0.040(3) 0.036(2) 0.0051(19) -0.001(2) 0.004(2) C12 0.021(2) 0.046(3) 0.032(2) -0.001(2) -0.0039(17) 0.0000(19) C13 0.027(3) 0.066(4) 0.041(3) 0.009(2) 0.006(2) 0.015(3) C14 0.045(3) 0.023(2) 0.033(2) -0.0036(18) -0.004(2) -0.008(2) C15 0.030(3) 0.039(3) 0.043(3) 0.012(2) -0.001(2) -0.013(2) C16 0.023(2) 0.036(3) 0.036(2) 0.0080(18) 0.0011(17) 0.004(2) C17 0.043(3) 0.023(2) 0.029(2) -0.0016(16) 0.0018(18) 0.001(2) C18 0.028(2) 0.037(3) 0.034(2) 0.0016(18) 0.0018(18) -0.006(2) C19 0.042(3) 0.055(3) 0.032(2) -0.012(2) -0.005(2) -0.014(3) C20 0.034(3) 0.042(3) 0.024(2) 0.0034(18) -0.0025(18) 0.011(2) C21 0.037(3) 0.043(3) 0.037(3) 0.012(2) 0.008(2) -0.002(2) N1 0.0203(17) 0.0233(19) 0.0228(16) -0.0014(13) 0.0021(12) -0.0032(15) P1 0.0241(6) 0.0228(6) 0.0276(5) 0.0014(4) -0.0007(4) -0.0043(5) P2 0.0225(6) 0.0232(5) 0.0252(5) 0.0026(4) 0.0007(4) 0.0019(5) P3 0.0237(6) 0.0294(6) 0.0229(5) -0.0018(4) -0.0021(4) -0.0057(5) P4 0.0253(5) 0.0267(6) 0.0210(5) 0.0028(4) 0.0025(4) 0.0040(5) Fe1 0.0178(3) 0.0223(3) 0.0195(3) 0.0007(2) 0.0006(2) 0.0000(3) O1 0.0439(19) 0.0383(18) 0.0247(15) 0.0013(13) 0.0000(13) 0.0070(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.374(5) . ? C1 C2 1.391(5) . ? C1 C6 1.539(6) . ? C2 C3 1.377(6) . ? C3 C4 1.386(6) . ? C4 C5 1.377(5) . ? C5 N1 1.374(5) . ? C5 C10 1.530(6) . ? C6 C9 1.553(5) . ? C6 C8 1.556(5) . ? C6 C7 1.563(5) . ? C7 P1 1.823(4) . ? C8 P2 1.826(4) . ? C10 C11 1.521(6) . ? C10 C12 1.557(6) . ? C10 C13 1.559(6) . ? C12 P3 1.835(4) . ? C14 P1 1.821(4) . ? C15 P1 1.808(4) . ? C16 P2 1.822(4) . ? C17 P2 1.805(4) . ? C18 P3 1.822(4) . ? C19 P3 1.807(4) . ? C20 P4 1.818(4) . ? C21 P4 1.785(5) . ? N1 Fe1 2.057(3) . ? P1 Fe1 2.2763(12) . ? P2 Fe1 2.1732(12) . ? P3 Fe1 2.2529(12) . ? P4 O1 1.613(3) . ? P4 Fe1 2.2154(10) . ? B1A F1A 1.321(14) . ? B1A F3A 1.352(12) . ? B1A F2A 1.456(14) . ? B1A F4A 1.540(14) . ? B1B F1B 1.29(2) . ? B1B F2B 1.30(2) . ? B1B F3B 1.39(2) . ? B1B F4B 1.51(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 N1 C1 C2 120.0(3) . . ? N1 C1 C6 119.0(3) . . ? C2 C1 C6 121.0(3) . . ? C3 C2 C1 120.9(4) . . ? C2 C3 C4 118.7(4) . . ? C5 C4 C3 120.0(4) . . ? N1 C5 C4 121.4(4) . . ? N1 C5 C10 117.9(3) . . ? C4 C5 C10 120.7(4) . . ? C1 C6 C9 111.8(3) . . ? C1 C6 C8 111.1(3) . . ? C9 C6 C8 105.7(3) . . ? C1 C6 C7 108.5(3) . . ? C9 C6 C7 107.6(3) . . ? C8 C6 C7 112.1(3) . . ? C6 C7 P1 116.9(3) . . ? C6 C8 P2 115.1(3) . . ? C11 C10 C5 109.6(4) . . ? C11 C10 C12 110.0(3) . . ? C5 C10 C12 109.3(4) . . ? C11 C10 C13 107.9(4) . . ? C5 C10 C13 112.8(3) . . ? C12 C10 C13 107.2(4) . . ? C10 C12 P3 110.2(3) . . ? C5 N1 C1 118.9(3) . . ? C5 N1 Fe1 115.9(3) . . ? C1 N1 Fe1 125.1(2) . . ? C15 P1 C14 99.8(2) . . ? C15 P1 C7 103.1(2) . . ? C14 P1 C7 100.4(2) . . ? C15 P1 Fe1 129.78(17) . . ? C14 P1 Fe1 113.11(16) . . ? C7 P1 Fe1 106.74(14) . . ? C17 P2 C16 98.8(2) . . ? C17 P2 C8 103.38(19) . . ? C16 P2 C8 104.3(2) . . ? C17 P2 Fe1 122.32(16) . . ? C16 P2 Fe1 118.98(15) . . ? C8 P2 Fe1 106.89(14) . . ? C19 P3 C18 101.3(2) . . ? C19 P3 C12 103.7(2) . . ? C18 P3 C12 101.6(2) . . ? C19 P3 Fe1 126.98(17) . . ? C18 P3 Fe1 117.39(15) . . ? C12 P3 Fe1 102.39(14) . . ? O1 P4 C21 104.0(2) . . ? O1 P4 C20 104.38(19) . . ? C21 P4 C20 98.5(2) . . ? O1 P4 Fe1 111.02(11) . . ? C21 P4 Fe1 121.97(17) . . ? C20 P4 Fe1 114.93(15) . . ? N1 Fe1 P2 99.42(10) . . ? N1 Fe1 P4 169.00(10) . . ? P2 Fe1 P4 91.17(4) . . ? N1 Fe1 P3 81.80(9) . . ? P2 Fe1 P3 92.20(5) . . ? P4 Fe1 P3 94.92(4) . . ? N1 Fe1 P1 81.01(9) . . ? P2 Fe1 P1 89.16(4) . . ? P4 Fe1 P1 102.25(4) . . ? P3 Fe1 P1 162.75(4) . . ? F1A B1A F3A 108.5(9) . . ? F1A B1A F2A 117.4(9) . . ? F3A B1A F2A 115.6(9) . . ? F1A B1A F4A 115.9(9) . . ? F3A B1A F4A 103.4(9) . . ? F2A B1A F4A 94.8(8) . . ? F1B B1B F2B 123.2(15) . . ? F1B B1B F3B 112.2(15) . . ? F2B B1B F3B 118.9(16) . . ? F1B B1B F4B 92.4(15) . . ? F2B B1B F4B 103.0(15) . . ? F3B B1B F4B 98.0(13) . . ? _diffrn_measured_fraction_theta_max 0.896 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_full 0.896 _refine_diff_density_max 0.573 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.086 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 -0.021 0.049 0.535 77.7 18.7 2 0.006 0.350 0.320 8.7 0.3 3 0.021 0.549 0.965 77.8 18.9 4 -0.006 0.850 0.180 9.0 0.6 5 0.148 0.388 0.288 6.1 0.7 6 0.479 0.451 0.465 77.8 18.9 7 0.521 -0.049 0.035 77.8 18.8 8 0.367 0.617 0.792 6.8 0.8 9 0.508 0.653 0.823 8.0 0.3 10 0.506 0.150 0.680 8.6 0.4 11 0.648 0.113 0.711 6.2 0.8 12 0.852 0.888 0.212 5.8 0.7 _platon_squeeze_details ; ; # 4.1 RESULTS FOR 23 * 8 H2O data_ag0613 _database_code_depnum_ccdc_archive 'CCDC 613419' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H43 Fe N O P4, 2(B F4), H2 O' _chemical_formula_sum 'C21 H45 B2 F8 Fe N O2 P4' _chemical_formula_weight 696.93 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) _symmetry_space_group_name_Hall P2yb _chemical_absolute_configuration ad loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 10.9961(8) _cell_length_b 12.0964(7) _cell_length_c 23.0207(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.104(4) _cell_angle_gamma 90.00 _cell_volume 3061.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 173 _cell_measurement_theta_min 6.00 _cell_measurement_theta_max 20.00 _exptl_crystal_description plate _exptl_crystal_colour 'orange brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.512 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details 'SADABS, Bruker-AXS, 2002' _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 'Bruker-Nonius KappaCCD' _diffrn_measurement_method ; \w-rotations with 1.40 \% and 112 sec per frame ; _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56583 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0614 _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 -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.48 _diffrn_reflns_theta_max 27.10 _reflns_number_total 13280 _reflns_number_gt 10915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Bruker-Nonius, 2002)' _computing_cell_refinement 'EVALCCD (Duisenberg, 2003)' _computing_data_reduction 'EVALCCD (Duisenberg, 2003)' _computing_structure_solution 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_structure_refinement 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_molecular_graphics 'SHELXTL 6.12 (Bruker AXS, 2002)' _computing_publication_material 'SHELXTL 6.12 (Bruker AXS, 2002)' _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^)+(0.0450P)^2^+2.4976P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except water bound hydrogens difmap' _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 6234 Friedel pairs used in the refinement of Flack parameter ; _refine_ls_abs_structure_Flack 0.029(12) _refine_ls_number_reflns 13280 _refine_ls_number_parameters 737 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0970 _refine_ls_wR_factor_gt 0.0906 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 0.97003(4) 0.02152(4) 0.14601(2) 0.01174(11) Uani 1 1 d . . . P1 P 0.83717(8) 0.14573(8) 0.10723(4) 0.0146(2) Uani 1 1 d . . . P2 P 0.83788(9) -0.10774(8) 0.12817(4) 0.0152(2) Uani 1 1 d . . . P3 P 1.12329(9) -0.10112(8) 0.15725(4) 0.0155(2) Uani 1 1 d . . . P4 P 0.92468(8) 0.02412(8) 0.23902(4) 0.0160(2) Uani 1 1 d . . . N1 N 1.0437(3) 0.0381(2) 0.06481(12) 0.0124(6) Uani 1 1 d . . . O1 O 0.9073(3) -0.0999(2) 0.26417(11) 0.0249(6) Uani 1 1 d . . . H1A H 0.8902 -0.0966 0.2995 0.037 Uiso 1 1 calc R . . C1 C 0.9824(3) 0.0181(3) 0.01342(14) 0.0144(7) Uani 1 1 d . . . C2 C 1.0428(3) 0.0272(3) -0.03939(15) 0.0159(7) Uani 1 1 d . . . H2A H 1.0003 0.0129 -0.0749 0.019 Uiso 1 1 calc R . . C3 C 1.1631(3) 0.0568(3) -0.04003(16) 0.0173(8) Uani 1 1 d . . . H3A H 1.2052 0.0594 -0.0757 0.021 Uiso 1 1 calc R . . C4 C 1.2221(3) 0.0824(3) 0.01107(16) 0.0168(8) Uani 1 1 d . . . H4A H 1.3043 0.1065 0.0106 0.020 Uiso 1 1 calc R . . C5 C 1.1629(3) 0.0735(3) 0.06387(15) 0.0136(7) Uani 1 1 d . . . C6 C 0.8466(3) -0.0131(3) 0.01471(14) 0.0158(8) Uani 1 1 d . . . C7 C 0.7722(3) 0.0828(3) 0.04071(16) 0.0170(8) Uani 1 1 d . . . H7A H 0.6898 0.0550 0.0493 0.020 Uiso 1 1 calc R . . H7B H 0.7629 0.1413 0.0109 0.020 Uiso 1 1 calc R . . C8 C 0.8293(3) -0.1228(3) 0.04892(15) 0.0165(8) Uani 1 1 d . . . H8A H 0.8924 -0.1760 0.0369 0.020 Uiso 1 1 calc R . . H8B H 0.7491 -0.1546 0.0380 0.020 Uiso 1 1 calc R . . C9 C 0.7953(3) -0.0343(3) -0.04726(16) 0.0216(9) Uani 1 1 d . . . H9A H 0.8062 0.0321 -0.0710 0.032 Uiso 1 1 calc R . . H9B H 0.7086 -0.0521 -0.0454 0.032 Uiso 1 1 calc R . . H9C H 0.8388 -0.0963 -0.0647 0.032 Uiso 1 1 calc R . . C10 C 1.2576(3) -0.0128(3) 0.15200(16) 0.0190(8) Uani 1 1 d . . . H10A H 1.2904 0.0029 0.1915 0.023 Uiso 1 1 calc R . . H10B H 1.3212 -0.0523 0.1303 0.023 Uiso 1 1 calc R . . C11 C 1.1464(3) 0.1691(3) 0.15962(16) 0.0179(8) Uani 1 1 d . . . H11A H 1.0673 0.1331 0.1642 0.027 Uiso 1 1 calc R . . H11B H 1.1347 0.2416 0.1413 0.027 Uiso 1 1 calc R . . H11C H 1.1858 0.1786 0.1979 0.027 Uiso 1 1 calc R . . C12 C 1.2274(3) 0.0967(3) 0.12114(15) 0.0150(8) Uani 1 1 d . . . C13 C 1.3461(3) 0.1609(3) 0.11398(17) 0.0227(9) Uani 1 1 d . . . H13A H 1.4049 0.1147 0.0937 0.034 Uiso 1 1 calc R . . H13B H 1.3794 0.1810 0.1523 0.034 Uiso 1 1 calc R . . H13C H 1.3301 0.2281 0.0913 0.034 Uiso 1 1 calc R . . C14 C 0.9097(4) 0.2688(3) 0.07828(17) 0.0219(9) Uani 1 1 d . . . H14A H 0.8490 0.3133 0.0571 0.033 Uiso 1 1 calc R . . H14B H 0.9742 0.2469 0.0518 0.033 Uiso 1 1 calc R . . H14C H 0.9448 0.3124 0.1103 0.033 Uiso 1 1 calc R . . C15 C 0.7057(3) 0.2118(4) 0.14054(18) 0.0246(9) Uani 1 1 d . . . H15A H 0.6554 0.2473 0.1103 0.037 Uiso 1 1 calc R . . H15B H 0.7339 0.2676 0.1686 0.037 Uiso 1 1 calc R . . H15C H 0.6575 0.1558 0.1605 0.037 Uiso 1 1 calc R . . C16 C 0.8578(4) -0.2488(3) 0.15430(17) 0.0217(9) Uani 1 1 d . . . H16A H 0.7888 -0.2941 0.1410 0.033 Uiso 1 1 calc R . . H16B H 0.8620 -0.2489 0.1969 0.033 Uiso 1 1 calc R . . H16C H 0.9333 -0.2794 0.1391 0.033 Uiso 1 1 calc R . . C17 C 0.6811(3) -0.0898(3) 0.15001(17) 0.0223(9) Uani 1 1 d . . . H17A H 0.6302 -0.1471 0.1318 0.033 Uiso 1 1 calc R . . H17B H 0.6520 -0.0168 0.1376 0.033 Uiso 1 1 calc R . . H17C H 0.6765 -0.0959 0.1924 0.033 Uiso 1 1 calc R . . C18 C 1.1469(4) -0.1988(3) 0.09796(16) 0.0211(9) Uani 1 1 d . . . H18A H 1.2263 -0.2346 0.1032 0.032 Uiso 1 1 calc R . . H18B H 1.1443 -0.1592 0.0608 0.032 Uiso 1 1 calc R . . H18C H 1.0826 -0.2550 0.0981 0.032 Uiso 1 1 calc R . . C19 C 1.1548(4) -0.1875(3) 0.21963(17) 0.0251(9) Uani 1 1 d . . . H19A H 1.2335 -0.2242 0.2151 0.038 Uiso 1 1 calc R . . H19B H 1.0908 -0.2433 0.2229 0.038 Uiso 1 1 calc R . . H19C H 1.1573 -0.1418 0.2548 0.038 Uiso 1 1 calc R . . C20 C 0.7925(4) 0.0977(4) 0.26508(18) 0.0290(10) Uani 1 1 d . . . H20A H 0.7871 0.0881 0.3072 0.043 Uiso 1 1 calc R . . H20B H 0.7189 0.0681 0.2461 0.043 Uiso 1 1 calc R . . H20C H 0.8002 0.1765 0.2560 0.043 Uiso 1 1 calc R . . C21 C 1.0412(4) 0.0849(4) 0.28608(16) 0.0247(9) Uani 1 1 d . . . H21A H 1.0234 0.0680 0.3267 0.037 Uiso 1 1 calc R . . H21B H 1.0422 0.1652 0.2806 0.037 Uiso 1 1 calc R . . H21C H 1.1207 0.0542 0.2764 0.037 Uiso 1 1 calc R . . Fe2 Fe 0.47962(4) 0.49826(4) 0.34979(2) 0.01472(12) Uani 1 1 d . . . P5 P 0.33989(9) 0.37553(8) 0.38254(4) 0.0178(2) Uani 1 1 d . . . P6 P 0.34876(9) 0.62991(8) 0.36011(4) 0.0177(2) Uani 1 1 d . . . P7 P 0.63615(9) 0.61799(9) 0.34559(4) 0.0190(2) Uani 1 1 d . . . P8 P 0.44552(9) 0.49408(9) 0.25449(4) 0.0207(2) Uani 1 1 d . . . N2 N 0.5405(3) 0.4826(3) 0.43434(12) 0.0147(6) Uani 1 1 d . . . O2 O 0.4360(3) 0.6159(2) 0.22607(12) 0.0296(7) Uani 1 1 d . . . H2B H 0.4484 0.6117 0.1902 0.044 Uiso 1 1 calc R . . C22 C 0.4730(3) 0.5051(3) 0.48208(15) 0.0176(8) Uani 1 1 d . . . C23 C 0.5245(3) 0.4965(3) 0.53764(15) 0.0209(8) Uani 1 1 d . . . H23A H 0.4771 0.5128 0.5706 0.025 Uiso 1 1 calc R . . C24 C 0.6445(4) 0.4644(3) 0.54496(18) 0.0264(10) Uani 1 1 d . . . H24A H 0.6804 0.4617 0.5828 0.032 Uiso 1 1 calc R . . C25 C 0.7112(4) 0.4368(3) 0.49785(18) 0.0250(9) Uani 1 1 d . . . H25A H 0.7924 0.4111 0.5026 0.030 Uiso 1 1 calc R . . C26 C 0.6580(3) 0.4470(3) 0.44204(17) 0.0186(8) Uani 1 1 d . . . C27 C 0.3389(3) 0.5381(3) 0.47405(16) 0.0198(8) Uani 1 1 d . . . C28 C 0.2674(3) 0.4420(3) 0.44515(17) 0.0211(9) Uani 1 1 d . . . H28A H 0.1868 0.4703 0.4322 0.025 Uiso 1 1 calc R . . H28B H 0.2532 0.3847 0.4750 0.025 Uiso 1 1 calc R . . C29 C 0.3275(3) 0.6464(3) 0.43829(16) 0.0197(8) Uani 1 1 d . . . H29A H 0.3885 0.6999 0.4534 0.024 Uiso 1 1 calc R . . H29B H 0.2460 0.6785 0.4445 0.024 Uiso 1 1 calc R . . C30 C 0.2796(4) 0.5606(4) 0.53286(18) 0.0268(9) Uani 1 1 d . . . H30A H 0.3212 0.6225 0.5522 0.040 Uiso 1 1 calc R . . H30B H 0.2862 0.4945 0.5573 0.040 Uiso 1 1 calc R . . H30C H 0.1936 0.5792 0.5265 0.040 Uiso 1 1 calc R . . C31 C 0.7678(3) 0.5274(4) 0.35724(17) 0.0236(9) Uani 1 1 d . . . H31A H 0.8037 0.5090 0.3193 0.028 Uiso 1 1 calc R . . H31B H 0.8303 0.5666 0.3809 0.028 Uiso 1 1 calc R . . C32 C 0.6545(4) 0.3470(3) 0.34679(18) 0.0238(9) Uani 1 1 d . . . H32A H 0.5772 0.3841 0.3378 0.036 Uiso 1 1 calc R . . H32B H 0.6386 0.2756 0.3652 0.036 Uiso 1 1 calc R . . H32C H 0.6991 0.3352 0.3108 0.036 Uiso 1 1 calc R . . C33 C 0.7311(3) 0.4195(4) 0.38846(17) 0.0239(9) Uani 1 1 d . . . C34 C 0.8488(4) 0.3544(4) 0.4024(2) 0.0356(11) Uani 1 1 d . . . H34A H 0.9041 0.4005 0.4259 0.053 Uiso 1 1 calc R . . H34B H 0.8883 0.3342 0.3661 0.053 Uiso 1 1 calc R . . H34C H 0.8289 0.2873 0.4241 0.053 Uiso 1 1 calc R . . C35 C 0.4057(4) 0.2529(3) 0.41686(18) 0.0229(9) Uani 1 1 d . . . H35A H 0.3427 0.2136 0.4381 0.034 Uiso 1 1 calc R . . H35B H 0.4712 0.2751 0.4439 0.034 Uiso 1 1 calc R . . H35C H 0.4387 0.2043 0.3870 0.034 Uiso 1 1 calc R . . C36 C 0.2120(4) 0.3100(4) 0.34445(18) 0.0253(9) Uani 1 1 d . . . H36A H 0.1566 0.2782 0.3728 0.038 Uiso 1 1 calc R . . H36B H 0.2422 0.2514 0.3192 0.038 Uiso 1 1 calc R . . H36C H 0.1684 0.3653 0.3209 0.038 Uiso 1 1 calc R . . C37 C 0.3768(4) 0.7701(3) 0.33500(17) 0.0236(9) Uani 1 1 d . . . H37A H 0.3071 0.8170 0.3441 0.035 Uiso 1 1 calc R . . H37B H 0.3884 0.7695 0.2929 0.035 Uiso 1 1 calc R . . H37C H 0.4501 0.7992 0.3544 0.035 Uiso 1 1 calc R . . C38 C 0.1944(4) 0.6123(4) 0.32980(19) 0.0269(9) Uani 1 1 d . . . H38A H 0.1416 0.6707 0.3446 0.040 Uiso 1 1 calc R . . H38B H 0.1626 0.5399 0.3413 0.040 Uiso 1 1 calc R . . H38C H 0.1965 0.6168 0.2873 0.040 Uiso 1 1 calc R . . C39 C 0.6544(4) 0.7158(3) 0.40657(17) 0.0229(9) Uani 1 1 d . . . H39A H 0.7325 0.7542 0.4036 0.034 Uiso 1 1 calc R . . H39B H 0.6522 0.6753 0.4434 0.034 Uiso 1 1 calc R . . H39C H 0.5881 0.7700 0.4051 0.034 Uiso 1 1 calc R . . C40 C 0.6777(4) 0.7037(4) 0.28390(18) 0.0317(11) Uani 1 1 d . . . H40A H 0.7564 0.7390 0.2920 0.047 Uiso 1 1 calc R . . H40B H 0.6155 0.7607 0.2775 0.047 Uiso 1 1 calc R . . H40C H 0.6834 0.6576 0.2491 0.047 Uiso 1 1 calc R . . C41 C 0.3159(4) 0.4224(4) 0.22273(18) 0.0315(10) Uani 1 1 d . . . H41A H 0.3170 0.4298 0.1804 0.047 Uiso 1 1 calc R . . H41B H 0.2407 0.4545 0.2374 0.047 Uiso 1 1 calc R . . H41C H 0.3199 0.3439 0.2332 0.047 Uiso 1 1 calc R . . C42 C 0.5660(4) 0.4260(4) 0.21487(18) 0.0318(10) Uani 1 1 d . . . H42A H 0.5513 0.4351 0.1730 0.048 Uiso 1 1 calc R . . H42B H 0.5671 0.3471 0.2245 0.048 Uiso 1 1 calc R . . H42C H 0.6445 0.4591 0.2258 0.048 Uiso 1 1 calc R . . B1 B 0.9534(5) 0.4517(5) 0.2137(2) 0.0322(12) Uani 1 1 d . . . F11 F 1.0424(2) 0.4588(3) 0.17258(11) 0.0603(10) Uani 1 1 d . . . F12 F 0.8468(2) 0.4885(3) 0.18895(16) 0.0637(9) Uani 1 1 d . . . F13 F 0.9853(3) 0.5091(5) 0.26123(15) 0.1100(19) Uani 1 1 d . . . F14 F 0.9382(4) 0.3423(3) 0.22777(18) 0.0935(14) Uani 1 1 d . . . B2 B 0.4637(5) 0.8690(5) -0.0010(3) 0.0390(14) Uani 1 1 d . . . F21 F 0.4894(4) 0.8962(4) -0.05783(14) 0.0851(13) Uani 1 1 d . . . F22 F 0.3466(2) 0.8363(3) 0.00094(14) 0.0504(8) Uani 1 1 d . . . F23 F 0.4902(2) 0.9557(2) 0.03484(12) 0.0429(7) Uani 1 1 d . . . F24 F 0.5430(3) 0.7810(3) 0.01309(18) 0.0760(12) Uani 1 1 d . . . B3 B 0.4623(4) 0.0698(4) 0.2866(2) 0.0233(10) Uani 1 1 d . . . F31 F 0.3434(2) 0.0421(2) 0.30118(12) 0.0414(7) Uani 1 1 d . . . F32 F 0.4969(2) 0.0086(3) 0.23908(11) 0.0590(9) Uani 1 1 d . . . F33 F 0.5390(2) 0.0509(3) 0.33278(10) 0.0432(7) Uani 1 1 d . . . F34 F 0.4644(3) 0.1808(3) 0.27221(14) 0.0587(9) Uani 1 1 d . . . B4 B 1.0007(5) 0.8543(6) 0.4155(2) 0.0457(16) Uani 1 1 d . . . F41 F 0.9010(2) 0.8811(3) 0.38037(10) 0.0422(7) Uani 1 1 d . . . F42 F 1.1065(2) 0.8715(3) 0.38667(13) 0.0552(8) Uani 1 1 d . . . F43 F 0.9929(4) 0.9125(7) 0.46464(18) 0.165(3) Uani 1 1 d . . . F44 F 0.9952(5) 0.7442(5) 0.4289(3) 0.150(3) Uani 1 1 d . . . O3 O 0.4733(7) 0.6197(5) 0.1076(2) 0.108(2) Uani 1 1 d D . . H3C H 0.483(10) 0.675(7) 0.084(4) 0.162 Uiso 1 1 d D . . H3D H 0.517(9) 0.561(7) 0.091(4) 0.162 Uiso 1 1 d D . . O4 O 0.8884(7) 0.6686(7) 0.5342(4) 0.144(3) Uani 1 1 d D . . H4C H 0.951(10) 0.619(10) 0.543(7) 0.215 Uiso 1 1 d D . . H4D H 0.921(12) 0.704(10) 0.500(4) 0.215 Uiso 1 1 d D . . 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 0.0116(2) 0.0122(3) 0.0114(2) -0.0010(2) 0.00028(19) -0.0005(2) P1 0.0126(5) 0.0140(5) 0.0171(5) -0.0022(4) -0.0001(4) 0.0016(4) P2 0.0165(5) 0.0140(5) 0.0152(5) -0.0019(4) 0.0021(4) -0.0035(4) P3 0.0172(5) 0.0151(5) 0.0143(5) 0.0011(4) -0.0009(4) 0.0022(4) P4 0.0157(4) 0.0173(5) 0.0151(4) -0.0016(4) 0.0019(3) -0.0033(4) N1 0.0130(14) 0.0089(16) 0.0154(15) -0.0007(12) 0.0026(12) 0.0002(12) O1 0.0339(16) 0.0231(16) 0.0178(13) -0.0022(12) 0.0042(12) -0.0088(13) C1 0.0185(17) 0.0099(18) 0.0146(17) 0.0009(15) -0.0036(13) 0.0021(15) C2 0.0262(19) 0.0071(18) 0.0142(17) 0.0018(15) -0.0025(14) 0.0056(15) C3 0.026(2) 0.0113(19) 0.0150(18) 0.0029(14) 0.0060(16) 0.0039(15) C4 0.0137(18) 0.016(2) 0.0204(19) 0.0063(15) 0.0016(15) 0.0003(15) C5 0.0140(18) 0.0099(19) 0.0168(18) 0.0020(14) -0.0017(15) 0.0024(14) C6 0.0146(17) 0.018(2) 0.0146(17) -0.0013(15) -0.0026(14) -0.0008(15) C7 0.0134(18) 0.022(2) 0.0157(18) 0.0037(15) -0.0048(15) -0.0026(15) C8 0.0162(18) 0.018(2) 0.0155(17) -0.0032(15) 0.0032(14) -0.0058(15) C9 0.021(2) 0.025(2) 0.0188(19) -0.0035(16) -0.0049(16) -0.0023(16) C10 0.0152(17) 0.022(2) 0.0191(18) -0.0038(16) -0.0053(15) 0.0066(16) C11 0.0137(19) 0.020(2) 0.0204(19) -0.0001(16) -0.0011(15) -0.0061(15) C12 0.0104(17) 0.018(2) 0.0168(18) -0.0020(15) -0.0009(14) -0.0004(14) C13 0.018(2) 0.028(2) 0.022(2) -0.0047(17) 0.0004(16) -0.0031(17) C14 0.024(2) 0.018(2) 0.023(2) 0.0043(16) -0.0006(17) 0.0030(16) C15 0.016(2) 0.032(3) 0.026(2) -0.0071(18) 0.0005(17) 0.0111(17) C16 0.032(2) 0.014(2) 0.019(2) 0.0008(16) 0.0022(17) -0.0044(17) C17 0.0164(19) 0.026(2) 0.025(2) -0.0032(17) 0.0048(16) -0.0113(17) C18 0.026(2) 0.022(2) 0.0147(19) -0.0004(16) 0.0014(16) 0.0085(17) C19 0.032(2) 0.024(2) 0.019(2) 0.0004(17) -0.0022(18) 0.0063(18) C20 0.024(2) 0.041(3) 0.022(2) -0.0053(19) 0.0059(17) -0.0005(19) C21 0.027(2) 0.030(2) 0.0170(19) -0.0052(17) -0.0034(17) -0.0102(18) Fe2 0.0138(2) 0.0144(3) 0.0159(3) -0.0018(2) -0.0015(2) -0.0014(2) P5 0.0165(5) 0.0140(5) 0.0228(5) -0.0017(4) -0.0012(4) -0.0030(4) P6 0.0169(5) 0.0155(5) 0.0207(5) -0.0011(4) -0.0027(4) 0.0004(4) P7 0.0190(5) 0.0201(6) 0.0180(5) -0.0020(4) 0.0014(4) -0.0061(4) P8 0.0224(5) 0.0209(6) 0.0185(5) -0.0044(4) -0.0026(4) -0.0029(4) N2 0.0160(15) 0.0113(16) 0.0168(15) -0.0007(13) -0.0010(12) -0.0040(12) O2 0.0455(18) 0.0256(17) 0.0175(14) 0.0035(12) -0.0046(13) -0.0038(14) C22 0.0223(18) 0.011(2) 0.0190(18) -0.0006(15) -0.0006(15) -0.0063(16) C23 0.031(2) 0.014(2) 0.0176(18) 0.0011(16) 0.0025(16) -0.0062(17) C24 0.033(2) 0.022(2) 0.023(2) 0.0027(17) -0.0128(18) -0.0055(18) C25 0.024(2) 0.020(2) 0.030(2) 0.0041(17) -0.0050(18) 0.0011(17) C26 0.0154(19) 0.013(2) 0.027(2) -0.0020(16) -0.0051(16) -0.0035(15) C27 0.0201(19) 0.016(2) 0.0230(19) 0.0003(16) 0.0033(16) -0.0029(15) C28 0.0162(19) 0.023(2) 0.024(2) -0.0028(16) 0.0030(16) -0.0059(16) C29 0.0158(19) 0.019(2) 0.024(2) -0.0045(16) 0.0013(16) 0.0020(16) C30 0.027(2) 0.026(2) 0.028(2) -0.0054(18) 0.0076(18) -0.0040(18) C31 0.0156(18) 0.028(2) 0.027(2) -0.0077(19) 0.0052(16) -0.0044(18) C32 0.020(2) 0.021(2) 0.031(2) -0.0090(18) 0.0029(17) 0.0068(17) C33 0.017(2) 0.029(2) 0.026(2) -0.0024(17) -0.0040(16) 0.0022(16) C34 0.016(2) 0.045(3) 0.046(3) -0.012(2) -0.001(2) 0.004(2) C35 0.026(2) 0.016(2) 0.026(2) -0.0017(16) -0.0010(17) -0.0037(16) C36 0.022(2) 0.022(2) 0.032(2) -0.0028(18) -0.0046(18) -0.0075(17) C37 0.033(2) 0.013(2) 0.024(2) -0.0014(16) -0.0032(18) 0.0007(17) C38 0.021(2) 0.025(2) 0.035(2) -0.0012(18) -0.0054(18) -0.0001(17) C39 0.022(2) 0.024(2) 0.022(2) -0.0035(17) -0.0004(17) -0.0110(17) C40 0.041(3) 0.031(3) 0.024(2) 0.0050(19) 0.008(2) -0.019(2) C41 0.033(2) 0.035(3) 0.026(2) -0.0061(19) -0.0110(19) -0.006(2) C42 0.037(3) 0.038(3) 0.020(2) -0.0101(19) 0.0008(19) 0.003(2) B1 0.024(3) 0.045(3) 0.028(3) -0.008(2) 0.002(2) -0.006(2) F11 0.0281(15) 0.130(3) 0.0226(13) -0.0029(16) 0.0040(12) -0.0015(16) F12 0.0256(14) 0.053(2) 0.112(3) 0.011(2) -0.0054(16) 0.0050(14) F13 0.072(2) 0.199(5) 0.061(2) -0.085(3) 0.0327(19) -0.077(3) F14 0.122(4) 0.068(3) 0.089(3) 0.046(2) -0.024(3) -0.002(2) B2 0.020(3) 0.047(4) 0.050(3) -0.014(3) -0.001(2) -0.007(2) F21 0.087(3) 0.126(4) 0.0429(19) -0.002(2) 0.0055(19) -0.046(3) F22 0.0257(14) 0.055(2) 0.071(2) -0.0108(16) 0.0043(14) -0.0071(13) F23 0.0386(15) 0.0427(17) 0.0470(16) -0.0215(13) -0.0104(13) 0.0024(12) F24 0.0425(19) 0.053(2) 0.132(4) -0.036(2) -0.013(2) 0.0140(16) B3 0.018(2) 0.031(3) 0.021(2) 0.000(2) 0.0002(19) -0.0009(19) F31 0.0192(12) 0.0478(18) 0.0576(17) -0.0127(14) 0.0100(12) -0.0053(11) F32 0.0252(13) 0.106(3) 0.0453(16) -0.0448(19) -0.0044(12) 0.0105(18) F33 0.0310(14) 0.079(2) 0.0199(12) 0.0052(13) -0.0006(11) 0.0044(13) F34 0.071(2) 0.044(2) 0.061(2) 0.0160(16) -0.0015(17) -0.0104(16) B4 0.035(3) 0.072(5) 0.029(3) 0.004(3) -0.006(2) 0.012(3) F41 0.0285(13) 0.075(2) 0.0229(12) 0.0041(13) -0.0022(11) -0.0059(14) F42 0.0234(14) 0.074(2) 0.069(2) -0.0249(18) 0.0024(14) 0.0011(14) F43 0.051(2) 0.378(9) 0.066(3) -0.106(4) -0.030(2) 0.081(4) F44 0.114(4) 0.128(5) 0.210(6) 0.110(5) 0.086(4) 0.052(3) O3 0.189(7) 0.097(5) 0.037(3) -0.008(3) -0.016(3) -0.025(5) O4 0.145(6) 0.161(7) 0.128(6) -0.058(5) 0.087(5) -0.089(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 N1 2.061(3) . ? Fe1 P2 2.1684(11) . ? Fe1 P4 2.2080(10) . ? Fe1 P3 2.2563(11) . ? Fe1 P1 2.2668(10) . ? P1 C14 1.821(4) . ? P1 C15 1.833(4) . ? P1 C7 1.842(4) . ? P2 C17 1.818(4) . ? P2 C16 1.822(4) . ? P2 C8 1.834(4) . ? P3 C19 1.804(4) . ? P3 C18 1.828(4) . ? P3 C10 1.829(4) . ? P4 O1 1.620(3) . ? P4 C20 1.816(4) . ? P4 C21 1.817(4) . ? N1 C1 1.372(4) . ? N1 C5 1.379(4) . ? O1 H1A 0.8400 . ? C1 C2 1.401(5) . ? C1 C6 1.540(5) . ? C2 C3 1.371(5) . ? C2 H2A 0.9500 . ? C3 C4 1.368(5) . ? C3 H3A 0.9500 . ? C4 C5 1.394(5) . ? C4 H4A 0.9500 . ? C5 C12 1.512(5) . ? C6 C9 1.545(5) . ? C6 C7 1.547(5) . ? C6 C8 1.557(5) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.537(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.541(5) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C13 1.530(5) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? Fe2 N2 2.055(3) . ? Fe2 P6 2.1625(11) . ? Fe2 P8 2.2190(11) . ? Fe2 P7 2.2530(11) . ? Fe2 P5 2.2755(11) . ? P5 C35 1.823(4) . ? P5 C36 1.824(4) . ? P5 C28 1.845(4) . ? P6 C37 1.820(4) . ? P6 C29 1.830(4) . ? P6 C38 1.836(4) . ? P7 C40 1.824(4) . ? P7 C31 1.831(4) . ? P7 C39 1.844(4) . ? P8 O2 1.615(3) . ? P8 C41 1.810(4) . ? P8 C42 1.820(4) . ? N2 C22 1.365(5) . ? N2 C26 1.370(5) . ? O2 H2B 0.8400 . ? C22 C23 1.393(5) . ? C22 C27 1.536(5) . ? C23 C24 1.383(6) . ? C23 H23A 0.9500 . ? C24 C25 1.363(6) . ? C24 H24A 0.9500 . ? C25 C26 1.407(6) . ? C25 H25A 0.9500 . ? C26 C33 1.522(6) . ? C27 C30 1.538(5) . ? C27 C28 1.547(5) . ? C27 C29 1.551(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C33 1.547(6) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.538(6) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.544(6) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? B1 F13 1.337(6) . ? B1 F12 1.368(6) . ? B1 F14 1.373(7) . ? B1 F11 1.377(6) . ? B2 F22 1.349(6) . ? B2 F23 1.361(6) . ? B2 F21 1.384(7) . ? B2 F24 1.410(7) . ? B3 F33 1.364(5) . ? B3 F32 1.380(5) . ? B3 F34 1.384(6) . ? B3 F31 1.396(5) . ? B4 F43 1.337(7) . ? B4 F42 1.366(7) . ? B4 F44 1.368(9) . ? B4 F41 1.387(6) . ? O3 H3C 0.87(5) . ? O3 H3D 0.94(5) . ? O4 H4C 0.93(5) . ? O4 H4D 0.97(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Fe1 P2 99.91(9) . . ? N1 Fe1 P4 167.96(9) . . ? P2 Fe1 P4 91.77(4) . . ? N1 Fe1 P3 82.06(8) . . ? P2 Fe1 P3 92.52(4) . . ? P4 Fe1 P3 94.61(4) . . ? N1 Fe1 P1 80.81(8) . . ? P2 Fe1 P1 88.79(4) . . ? P4 Fe1 P1 102.51(4) . . ? P3 Fe1 P1 162.79(4) . . ? C14 P1 C15 98.7(2) . . ? C14 P1 C7 101.46(18) . . ? C15 P1 C7 103.38(18) . . ? C14 P1 Fe1 113.75(13) . . ? C15 P1 Fe1 129.18(14) . . ? C7 P1 Fe1 106.88(13) . . ? C17 P2 C16 97.43(19) . . ? C17 P2 C8 104.82(17) . . ? C16 P2 C8 103.82(18) . . ? C17 P2 Fe1 119.82(14) . . ? C16 P2 Fe1 122.49(14) . . ? C8 P2 Fe1 106.35(12) . . ? C19 P3 C18 101.10(19) . . ? C19 P3 C10 104.34(19) . . ? C18 P3 C10 101.65(18) . . ? C19 P3 Fe1 127.12(15) . . ? C18 P3 Fe1 117.12(13) . . ? C10 P3 Fe1 102.17(12) . . ? O1 P4 C20 103.60(18) . . ? O1 P4 C21 104.34(18) . . ? C20 P4 C21 99.5(2) . . ? O1 P4 Fe1 111.32(10) . . ? C20 P4 Fe1 121.63(14) . . ? C21 P4 Fe1 114.48(13) . . ? C1 N1 C5 119.5(3) . . ? C1 N1 Fe1 124.7(2) . . ? C5 N1 Fe1 115.8(2) . . ? P4 O1 H1A 109.5 . . ? N1 C1 C2 120.0(3) . . ? N1 C1 C6 119.2(3) . . ? C2 C1 C6 120.8(3) . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2A 119.9 . . ? C1 C2 H2A 119.9 . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4A 119.6 . . ? C5 C4 H4A 119.6 . . ? N1 C5 C4 119.8(3) . . ? N1 C5 C12 118.3(3) . . ? C4 C5 C12 121.8(3) . . ? C1 C6 C9 111.0(3) . . ? C1 C6 C7 110.1(3) . . ? C9 C6 C7 107.2(3) . . ? C1 C6 C8 110.3(3) . . ? C9 C6 C8 106.2(3) . . ? C7 C6 C8 111.9(3) . . ? C6 C7 P1 115.6(2) . . ? C6 C7 H7A 108.4 . . ? P1 C7 H7A 108.4 . . ? C6 C7 H7B 108.4 . . ? P1 C7 H7B 108.4 . . ? H7A C7 H7B 107.4 . . ? C6 C8 P2 114.5(2) . . ? C6 C8 H8A 108.6 . . ? P2 C8 H8A 108.6 . . ? C6 C8 H8B 108.6 . . ? P2 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 P3 111.5(2) . . ? C12 C10 H10A 109.3 . . ? P3 C10 H10A 109.3 . . ? C12 C10 H10B 109.3 . . ? P3 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C12 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C5 C12 C13 112.8(3) . . ? C5 C12 C10 109.7(3) . . ? C13 C12 C10 108.1(3) . . ? C5 C12 C11 109.9(3) . . ? C13 C12 C11 106.1(3) . . ? C10 C12 C11 110.3(3) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? P1 C15 H15A 109.5 . . ? P1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P2 C16 H16A 109.5 . . ? P2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C17 H17A 109.5 . . ? P2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P3 C18 H18A 109.5 . . ? P3 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P3 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P3 C19 H19A 109.5 . . ? P3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P4 C20 H20A 109.5 . . ? P4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P4 C21 H21A 109.5 . . ? P4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 Fe2 P6 99.73(9) . . ? N2 Fe2 P8 168.56(9) . . ? P6 Fe2 P8 91.45(4) . . ? N2 Fe2 P7 82.21(9) . . ? P6 Fe2 P7 92.40(4) . . ? P8 Fe2 P7 94.98(4) . . ? N2 Fe2 P5 80.55(9) . . ? P6 Fe2 P5 89.37(4) . . ? P8 Fe2 P5 102.15(4) . . ? P7 Fe2 P5 162.73(4) . . ? C35 P5 C36 98.69(19) . . ? C35 P5 C28 100.94(19) . . ? C36 P5 C28 102.94(19) . . ? C35 P5 Fe2 114.15(14) . . ? C36 P5 Fe2 130.04(15) . . ? C28 P5 Fe2 106.23(13) . . ? C37 P6 C29 103.68(18) . . ? C37 P6 C38 98.6(2) . . ? C29 P6 C38 104.59(19) . . ? C37 P6 Fe2 122.27(15) . . ? C29 P6 Fe2 106.63(13) . . ? C38 P6 Fe2 119.02(15) . . ? C40 P7 C31 104.2(2) . . ? C40 P7 C39 101.7(2) . . ? C31 P7 C39 101.45(19) . . ? C40 P7 Fe2 127.02(15) . . ? C31 P7 Fe2 102.20(14) . . ? C39 P7 Fe2 116.86(13) . . ? O2 P8 C41 103.26(19) . . ? O2 P8 C42 104.6(2) . . ? C41 P8 C42 99.0(2) . . ? O2 P8 Fe2 112.84(11) . . ? C41 P8 Fe2 121.79(15) . . ? C42 P8 Fe2 113.26(15) . . ? C22 N2 C26 119.0(3) . . ? C22 N2 Fe2 124.9(2) . . ? C26 N2 Fe2 116.1(2) . . ? P8 O2 H2B 109.5 . . ? N2 C22 C23 120.4(3) . . ? N2 C22 C27 119.4(3) . . ? C23 C22 C27 120.2(3) . . ? C24 C23 C22 120.2(4) . . ? C24 C23 H23A 119.9 . . ? C22 C23 H23A 119.9 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24A 120.0 . . ? C23 C24 H24A 120.0 . . ? C24 C25 C26 119.0(4) . . ? C24 C25 H25A 120.5 . . ? C26 C25 H25A 120.5 . . ? N2 C26 C25 121.4(4) . . ? N2 C26 C33 118.4(3) . . ? C25 C26 C33 120.2(3) . . ? C22 C27 C30 111.3(3) . . ? C22 C27 C28 109.6(3) . . ? C30 C27 C28 106.9(3) . . ? C22 C27 C29 110.6(3) . . ? C30 C27 C29 106.6(3) . . ? C28 C27 C29 111.8(3) . . ? C27 C28 P5 116.1(3) . . ? C27 C28 H28A 108.3 . . ? P5 C28 H28A 108.3 . . ? C27 C28 H28B 108.3 . . ? P5 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C27 C29 P6 114.8(3) . . ? C27 C29 H29A 108.6 . . ? P6 C29 H29A 108.6 . . ? C27 C29 H29B 108.6 . . ? P6 C29 H29B 108.6 . . ? H29A C29 H29B 107.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C33 C31 P7 111.1(3) . . ? C33 C31 H31A 109.4 . . ? P7 C31 H31A 109.4 . . ? C33 C31 H31B 109.4 . . ? P7 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C33 C32 H32A 109.5 . . ? C33 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C33 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C26 C33 C32 109.8(3) . . ? C26 C33 C34 113.4(3) . . ? C32 C33 C34 106.6(3) . . ? C26 C33 C31 109.8(3) . . ? C32 C33 C31 109.6(3) . . ? C34 C33 C31 107.5(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? P5 C35 H35A 109.5 . . ? P5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P5 C36 H36A 109.5 . . ? P5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P6 C37 H37A 109.5 . . ? P6 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P6 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P6 C38 H38A 109.5 . . ? P6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P7 C39 H39A 109.5 . . ? P7 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P7 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P7 C40 H40A 109.5 . . ? P7 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P7 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? P8 C41 H41A 109.5 . . ? P8 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P8 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? P8 C42 H42A 109.5 . . ? P8 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P8 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? F13 B1 F12 112.4(5) . . ? F13 B1 F14 109.8(5) . . ? F12 B1 F14 107.7(4) . . ? F13 B1 F11 110.6(4) . . ? F12 B1 F11 108.0(4) . . ? F14 B1 F11 108.3(5) . . ? F22 B2 F23 113.6(4) . . ? F22 B2 F21 108.2(4) . . ? F23 B2 F21 110.1(5) . . ? F22 B2 F24 111.0(5) . . ? F23 B2 F24 108.6(4) . . ? F21 B2 F24 105.0(4) . . ? F33 B3 F32 110.6(4) . . ? F33 B3 F34 109.6(4) . . ? F32 B3 F34 108.9(4) . . ? F33 B3 F31 109.9(4) . . ? F32 B3 F31 109.6(4) . . ? F34 B3 F31 108.1(4) . . ? F43 B4 F42 113.5(6) . . ? F43 B4 F44 108.5(6) . . ? F42 B4 F44 107.5(5) . . ? F43 B4 F41 107.9(5) . . ? F42 B4 F41 110.6(4) . . ? F44 B4 F41 108.7(6) . . ? H3C O3 H3D 105(9) . . ? H4C O4 H4D 100(10) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1A F41 0.84 1.88 2.687(3) 160.1 1_545 O2 H2B O3 0.84 1.93 2.766(6) 173.6 . O3 H3C F24 0.87(5) 2.19(5) 3.032(7) 164(10) . O3 H3D F21 0.94(5) 2.14(7) 2.968(8) 147(9) 2_645 O4 H4C F43 0.93(5) 2.58(10) 3.362(12) 142(13) 2_746 O4 H4D F44 0.97(5) 1.91(6) 2.863(9) 169(12) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.803 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.081 #===END OF ALL DATA