################################################################### # # # for any questions concerning this structure please contact: # # # # Roland Schoch # # Paderborn University # # Faculty of Science / Department of Chemistry # # Warburger Str. 100 # # D-33098 Paderborn, Germany # # # # e-mail: roland.schoch@uni-paderborn.de # # phone: +49 (0)5251 60 5775 # # # ################################################################### data_js_0169_0m_a_sq _audit_creation_method 'SHELXL-2018/3' _shelx_SHELXL_version_number '2018/3' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C28 H26 N8 Fe), (P F6)' _chemical_formula_sum 'C28 H26 F6 Fe N8 P' _chemical_formula_weight 675.40 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' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.6367(12) _cell_length_b 8.7801(8) _cell_length_c 27.099(3) _cell_angle_alpha 90 _cell_angle_beta 96.285(2) _cell_angle_gamma 90 _cell_volume 3225.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 473(2) _cell_measurement_reflns_used 3869 _cell_measurement_theta_min 2.2455 _cell_measurement_theta_max 21.8965 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.391 _exptl_crystal_F_000 1380 _exptl_transmission_factor_min 0.6763 _exptl_transmission_factor_max 0.7454 _exptl_crystal_size_max 0.420 _exptl_crystal_size_mid 0.370 _exptl_crystal_size_min 0.250 _exptl_absorpt_coefficient_mu 0.583 _shelx_estimated_absorpt_T_min 0.792 _shelx_estimated_absorpt_T_max 0.868 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ; ' SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10. SHELX Sheldrick, G. M. Acta Cryst. (2015) C71, 3-8.' ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 473(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker AXS SMART APEX' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28802 _diffrn_reflns_av_unetI/netI 0.0393 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.512 _diffrn_reflns_theta_max 26.462 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6622 _reflns_number_gt 4696 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'APEX 3, SAINT (Bruker, 2018)' _computing_data_reduction 'APEX 3, SAINT (Bruker, 2018)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'SHELX' _computing_publication_material 'SHELXTL, ShelXle, Olex2 and local programs' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0831P)^2^+3.5698P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary dual _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 6622 _refine_ls_number_parameters 416 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1683 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _publ_section_exptl_refinement ; 'Hydrogen atoms were located from difference Fourier maps, refined at idealized positions riding on the carbon atoms with isotropic displacement parameters Uiso(H) = 1.2U~eq~(C) or 1.5U~eq~(-CH~3~ hydrogens) and C-H 0.96 \%A. All CH~3~ hydrogen atoms were allowed to rotate but not to tip. REFERENCES Bruker (2002). SMART (Version 5.63), SAINT (Version 6.02). Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2015). Acta Cryst. C71, 3-8. C. B. Hübschle, G. M. Sheldrick and B. Dittrich ShelXle: a Qt graphical user interface for SHELXL J. Appl. Cryst., 44, (2011) 1281-1284. O.V. Dolomanov, L.J. Bourhis, R.J. Gildea, J.A.K. Howard, H. Puschmann OLEX2: A complete structure solution, refinement and analysis program J. Appl. Cryst., 42, (2009) 339-341.' ; 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.73418(3) 0.99674(5) 0.37894(2) 0.03028(15) Uani 1 1 d . . . . . N11 N 0.8869(2) 1.2651(4) 0.38710(11) 0.0400(7) Uani 1 1 d . . . . . N12 N 0.7554(2) 1.2945(3) 0.42212(11) 0.0380(7) Uani 1 1 d . . . . . N13 N 0.5509(2) 0.8839(4) 0.40683(11) 0.0398(7) Uani 1 1 d . . . . . N14 N 0.6085(2) 0.6956(3) 0.36866(11) 0.0398(7) Uani 1 1 d . . . . . N21 N 0.5973(2) 1.1226(4) 0.28724(12) 0.0501(8) Uani 1 1 d . . . . . N22 N 0.7219(3) 0.9862(4) 0.27269(11) 0.0472(8) Uani 1 1 d . . . . . N23 N 0.9080(2) 0.8229(3) 0.41257(11) 0.0371(7) Uani 1 1 d . . . . . N24 N 0.8534(2) 0.9002(3) 0.47947(11) 0.0383(7) Uani 1 1 d . . . . . C101 C 0.8005(2) 1.1953(4) 0.39319(12) 0.0336(7) Uani 1 1 d . . . . . C102 C 0.9618(3) 1.2051(5) 0.35724(16) 0.0554(11) Uani 1 1 d . . . . . H10A H 0.929920 1.151552 0.329025 0.083 Uiso 1 1 calc R U . . . H10B H 1.004555 1.136600 0.377062 0.083 Uiso 1 1 calc R U . . . H10C H 0.999812 1.287804 0.346126 0.083 Uiso 1 1 calc R U . . . C103 C 0.8947(3) 1.4031(5) 0.41250(15) 0.0490(10) Uani 1 1 d . . . . . H103 H 0.947528 1.470490 0.413938 0.059 Uiso 1 1 calc R U . . . C104 C 0.8133(3) 1.4208(4) 0.43420(15) 0.0489(10) Uani 1 1 d . . . . . H104 H 0.797970 1.502497 0.453799 0.059 Uiso 1 1 calc R U . . . C105 C 0.6616(3) 1.2467(4) 0.43476(13) 0.0375(8) Uani 1 1 d . . . . . C106 C 0.5941(3) 1.3294(5) 0.45865(14) 0.0507(10) Uani 1 1 d . . . . . H106 H 0.607661 1.427975 0.469981 0.061 Uiso 1 1 calc R U . . . C107 C 0.5055(3) 1.2580(6) 0.46484(15) 0.0555(11) Uani 1 1 d . . . . . H107 H 0.458729 1.311475 0.480412 0.067 Uiso 1 1 calc R U . . . C108 C 0.4837(3) 1.1112(5) 0.44891(15) 0.0512(10) Uani 1 1 d . . . . . H108 H 0.423454 1.066396 0.453258 0.061 Uiso 1 1 calc R U . . . C109 C 0.5550(3) 1.0329(4) 0.42618(13) 0.0392(8) Uani 1 1 d . . . . . C110 C 0.6432(2) 1.1008(4) 0.41811(12) 0.0337(7) Uani 1 1 d . . . . . C111 C 0.4825(3) 0.7663(5) 0.40718(14) 0.0494(10) Uani 1 1 d . . . . . H111 H 0.423292 0.768292 0.421268 0.059 Uiso 1 1 calc R U . . . C112 C 0.5186(3) 0.6511(5) 0.38347(14) 0.0475(10) Uani 1 1 d . . . . . H112 H 0.488904 0.556457 0.377704 0.057 Uiso 1 1 calc R U . . . C113 C 0.6679(3) 0.6033(4) 0.33864(15) 0.0489(10) Uani 1 1 d . . . . . H11A H 0.650011 0.625542 0.304146 0.073 Uiso 1 1 calc R U . . . H11B H 0.656331 0.497374 0.344645 0.073 Uiso 1 1 calc R U . . . H11C H 0.736456 0.626023 0.347338 0.073 Uiso 1 1 calc R U . . . C114 C 0.6301(2) 0.8410(4) 0.38318(13) 0.0361(8) Uani 1 1 d . . . . . C201 C 0.6758(3) 1.0467(4) 0.31064(13) 0.0392(8) Uani 1 1 d . . . . . C202 C 0.5238(3) 1.2067(6) 0.31099(18) 0.0665(13) Uani 1 1 d . . . . . H20A H 0.505127 1.296264 0.291922 0.100 Uiso 1 1 calc R U . . . H20B H 0.550736 1.235741 0.343847 0.100 Uiso 1 1 calc R U . . . H20C H 0.466784 1.143636 0.312903 0.100 Uiso 1 1 calc R U . . . C203 C 0.5952(4) 1.1093(6) 0.23623(16) 0.0679(14) Uani 1 1 d . . . . . H203 H 0.548379 1.151549 0.212644 0.081 Uiso 1 1 calc R U . . . C204 C 0.6721(4) 1.0255(6) 0.22707(16) 0.0670(14) Uani 1 1 d . . . . . H204 H 0.689330 0.998231 0.195994 0.080 Uiso 1 1 calc R U . . . C205 C 0.8078(3) 0.9003(5) 0.28708(14) 0.0477(10) Uani 1 1 d . . . . . C206 C 0.8698(4) 0.8263(6) 0.25757(17) 0.0658(13) Uani 1 1 d . . . . . H206 H 0.858365 0.830157 0.223130 0.079 Uiso 1 1 calc R U . . . C207 C 0.9492(4) 0.7465(6) 0.28099(19) 0.0703(14) Uani 1 1 d . . . . . H207 H 0.991561 0.696962 0.261628 0.084 Uiso 1 1 calc R U . . . C208 C 0.9679(3) 0.7378(5) 0.33213(17) 0.0567(11) Uani 1 1 d . . . . . H208 H 1.021145 0.682634 0.347244 0.068 Uiso 1 1 calc R U . . . C209 C 0.9044(3) 0.8141(4) 0.35986(15) 0.0425(9) Uani 1 1 d . . . . . C210 C 0.8239(3) 0.8938(4) 0.33857(13) 0.0380(8) Uani 1 1 d . . . . . C211 C 0.9742(3) 0.7728(4) 0.45127(17) 0.0491(10) Uani 1 1 d . . . . . H211 H 1.031240 0.716478 0.448885 0.059 Uiso 1 1 calc R U . . . C212 C 0.9402(3) 0.8214(5) 0.49281(16) 0.0496(10) Uani 1 1 d . . . . . H212 H 0.969493 0.805140 0.525005 0.060 Uiso 1 1 calc R U . . . C213 C 0.7948(3) 0.9711(5) 0.51481(14) 0.0514(10) Uani 1 1 d . . . . . H21A H 0.726811 0.973304 0.501186 0.077 Uiso 1 1 calc R U . . . H21B H 0.817672 1.073207 0.521467 0.077 Uiso 1 1 calc R U . . . H21C H 0.801222 0.913547 0.545114 0.077 Uiso 1 1 calc R U . . . C214 C 0.8321(2) 0.9038(4) 0.42965(13) 0.0329(7) Uani 1 1 d . . . . . P1 P 0.22520(7) 0.47403(12) 0.41468(4) 0.0423(3) Uani 1 1 d . . . . . F111 F 0.1239(7) 0.4917(14) 0.4394(3) 0.052(2) Uiso 0.400(3) 1 d . . P A 1 F121 F 0.1960(8) 0.3041(10) 0.3971(3) 0.055(2) Uiso 0.400(3) 1 d . . P A 1 F131 F 0.3288(5) 0.4613(11) 0.3920(2) 0.0415(15) Uiso 0.400(3) 1 d . . P A 1 F141 F 0.2574(9) 0.6383(13) 0.4365(5) 0.080(3) Uiso 0.400(3) 1 d . . P A 1 F112 F 0.1353(12) 0.538(2) 0.4374(6) 0.076(6) Uiso 0.236(3) 1 d . . P A 2 F122 F 0.1664(15) 0.311(2) 0.4096(7) 0.111(8) Uiso 0.236(3) 1 d . . P A 2 F132 F 0.3159(8) 0.3935(16) 0.3866(4) 0.053(3) Uiso 0.236(3) 1 d . . P A 2 F142 F 0.2656(14) 0.633(2) 0.4171(7) 0.095(6) Uiso 0.236(3) 1 d . . P A 2 F113 F 0.2166(9) 0.6423(13) 0.4409(4) 0.094(4) Uiso 0.364(3) 1 d . . P B 3 F123 F 0.1159(7) 0.4478(12) 0.4285(4) 0.074(3) Uiso 0.364(3) 1 d . . P A 3 F133 F 0.2256(9) 0.3210(14) 0.3879(4) 0.095(5) Uiso 0.364(3) 1 d . . P A 3 F143 F 0.3267(8) 0.5215(14) 0.4008(4) 0.090(4) Uiso 0.364(3) 1 d . . P A 3 F15 F 0.1754(3) 0.5354(5) 0.36293(12) 0.1040(12) Uani 1 1 d . . . . . F16 F 0.2732(2) 0.4058(4) 0.46595(9) 0.0749(8) Uani 1 1 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 0.0261(2) 0.0362(3) 0.0288(3) -0.0003(2) 0.00382(18) -0.00307(19) N11 0.0372(16) 0.0458(18) 0.0359(16) 0.0032(13) -0.0013(13) -0.0111(13) N12 0.0392(16) 0.0378(16) 0.0360(16) 0.0009(13) -0.0008(13) -0.0007(13) N13 0.0299(15) 0.0522(19) 0.0371(16) 0.0034(14) 0.0031(12) -0.0085(13) N14 0.0391(17) 0.0418(17) 0.0362(16) 0.0051(13) -0.0055(13) -0.0104(13) N21 0.0489(19) 0.058(2) 0.0396(18) 0.0060(15) -0.0118(15) -0.0122(16) N22 0.0505(19) 0.061(2) 0.0293(16) -0.0018(14) 0.0028(14) -0.0157(16) N23 0.0294(15) 0.0390(16) 0.0429(17) -0.0032(13) 0.0037(13) 0.0005(12) N24 0.0377(16) 0.0402(17) 0.0364(16) 0.0038(13) 0.0021(13) 0.0003(13) C101 0.0323(18) 0.0403(19) 0.0273(17) 0.0041(14) -0.0009(14) -0.0027(15) C102 0.040(2) 0.073(3) 0.055(3) -0.006(2) 0.0155(19) -0.018(2) C103 0.051(2) 0.042(2) 0.051(2) 0.0012(18) -0.0074(19) -0.0143(18) C104 0.057(3) 0.037(2) 0.049(2) -0.0039(18) -0.0070(19) -0.0068(18) C105 0.0386(19) 0.040(2) 0.0329(18) 0.0028(15) -0.0003(15) 0.0060(15) C106 0.050(2) 0.056(2) 0.045(2) -0.0069(19) 0.0000(18) 0.017(2) C107 0.042(2) 0.078(3) 0.048(2) -0.003(2) 0.0090(18) 0.024(2) C108 0.0303(19) 0.078(3) 0.046(2) 0.007(2) 0.0065(16) 0.0077(19) C109 0.0291(18) 0.055(2) 0.0332(18) 0.0059(16) 0.0020(14) 0.0010(15) C110 0.0264(17) 0.045(2) 0.0288(17) 0.0019(15) 0.0009(13) 0.0029(14) C111 0.035(2) 0.071(3) 0.041(2) 0.013(2) -0.0021(17) -0.0200(19) C112 0.043(2) 0.057(3) 0.039(2) 0.0099(19) -0.0070(17) -0.0214(19) C113 0.049(2) 0.042(2) 0.054(2) -0.0047(18) -0.0058(18) -0.0049(18) C114 0.0314(18) 0.043(2) 0.0328(18) 0.0043(15) -0.0022(14) -0.0025(15) C201 0.0369(19) 0.0410(19) 0.038(2) 0.0004(16) -0.0019(15) -0.0130(16) C202 0.056(3) 0.066(3) 0.073(3) 0.004(2) -0.015(2) 0.012(2) C203 0.067(3) 0.090(4) 0.042(3) 0.011(2) -0.017(2) -0.015(3) C204 0.077(3) 0.094(4) 0.029(2) -0.001(2) -0.001(2) -0.031(3) C205 0.049(2) 0.055(2) 0.041(2) -0.0075(18) 0.0143(18) -0.0153(19) C206 0.069(3) 0.086(4) 0.047(3) -0.017(2) 0.030(2) -0.015(3) C207 0.067(3) 0.082(3) 0.070(3) -0.020(3) 0.042(3) -0.004(3) C208 0.042(2) 0.060(3) 0.071(3) -0.008(2) 0.022(2) 0.002(2) C209 0.0332(19) 0.043(2) 0.053(2) -0.0054(17) 0.0144(17) -0.0058(16) C210 0.0356(19) 0.0394(19) 0.041(2) -0.0045(15) 0.0107(15) -0.0101(15) C211 0.0314(19) 0.039(2) 0.074(3) 0.000(2) -0.0051(19) 0.0033(16) C212 0.048(2) 0.048(2) 0.049(2) 0.0097(19) -0.0103(19) 0.0050(18) C213 0.054(2) 0.065(3) 0.035(2) 0.0044(18) 0.0060(18) 0.005(2) C214 0.0289(17) 0.0318(17) 0.0382(19) 0.0012(14) 0.0042(14) -0.0038(14) P1 0.0275(5) 0.0533(6) 0.0460(6) 0.0027(4) 0.0034(4) -0.0014(4) F15 0.090(2) 0.149(3) 0.071(2) 0.038(2) -0.0016(17) 0.042(2) F16 0.0675(17) 0.102(2) 0.0539(16) 0.0073(15) 0.0005(13) 0.0206(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 Fe1 C110 1.946(3) . ? Fe1 C210 1.950(3) . ? Fe1 C101 1.982(3) . ? Fe1 C201 1.982(4) . ? Fe1 C114 1.983(3) . ? Fe1 C214 1.984(3) . ? N11 C101 1.355(4) . ? N11 C103 1.391(5) . ? N11 C102 1.469(5) . ? N12 C101 1.362(4) . ? N12 C104 1.379(5) . ? N12 C105 1.424(4) . ? N13 C114 1.368(4) . ? N13 C111 1.392(5) . ? N13 C109 1.408(5) . ? N14 C114 1.358(5) . ? N14 C112 1.387(5) . ? N14 C113 1.456(5) . ? N21 C201 1.358(5) . ? N21 C203 1.384(5) . ? N21 C202 1.451(6) . ? N22 C201 1.369(5) . ? N22 C204 1.387(6) . ? N22 C205 1.411(5) . ? N23 C214 1.376(4) . ? N23 C211 1.379(5) . ? N23 C209 1.426(5) . ? N24 C214 1.350(4) . ? N24 C212 1.384(5) . ? N24 C213 1.453(5) . ? C102 H10A 0.9600 . ? C102 H10B 0.9600 . ? C102 H10C 0.9600 . ? C103 C104 1.321(6) . ? C103 H103 0.9300 . ? C104 H104 0.9300 . ? C105 C110 1.372(5) . ? C105 C106 1.387(5) . ? C106 C107 1.387(6) . ? C106 H106 0.9300 . ? C107 C108 1.382(6) . ? C107 H107 0.9300 . ? C108 C109 1.389(5) . ? C108 H108 0.9300 . ? C109 C110 1.381(5) . ? C111 C112 1.322(6) . ? C111 H111 0.9300 . ? C112 H112 0.9300 . ? C113 H11A 0.9600 . ? C113 H11B 0.9600 . ? C113 H11C 0.9600 . ? C202 H20A 0.9600 . ? C202 H20B 0.9600 . ? C202 H20C 0.9600 . ? C203 C204 1.326(7) . ? C203 H203 0.9300 . ? C204 H204 0.9300 . ? C205 C206 1.388(6) . ? C205 C210 1.390(5) . ? C206 C207 1.384(7) . ? C206 H206 0.9300 . ? C207 C208 1.384(7) . ? C207 H207 0.9300 . ? C208 C209 1.381(5) . ? C208 H208 0.9300 . ? C209 C210 1.374(5) . ? C211 C212 1.334(6) . ? C211 H211 0.9300 . ? C212 H212 0.9300 . ? C213 H21A 0.9600 . ? C213 H21B 0.9600 . ? C213 H21C 0.9600 . ? P1 F142 1.497(19) . ? P1 F133 1.527(12) . ? P1 F143 1.532(11) . ? P1 F112 1.536(17) . ? P1 F15 1.585(3) . ? P1 F16 1.587(3) . ? P1 F123 1.592(10) . ? P1 F141 1.602(11) . ? P1 F121 1.604(9) . ? P1 F131 1.605(6) . ? P1 F111 1.607(10) . ? P1 F122 1.64(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 C110 Fe1 C210 178.93(15) . . ? C110 Fe1 C101 77.59(14) . . ? C210 Fe1 C101 102.49(14) . . ? C110 Fe1 C201 101.00(15) . . ? C210 Fe1 C201 77.92(16) . . ? C101 Fe1 C201 96.62(14) . . ? C110 Fe1 C114 77.84(15) . . ? C210 Fe1 C114 102.10(15) . . ? C101 Fe1 C114 155.39(15) . . ? C201 Fe1 C114 89.43(14) . . ? C110 Fe1 C214 103.66(14) . . ? C210 Fe1 C214 77.41(15) . . ? C101 Fe1 C214 88.21(13) . . ? C201 Fe1 C214 155.33(15) . . ? C114 Fe1 C214 96.20(13) . . ? C101 N11 C103 110.8(3) . . ? C101 N11 C102 124.8(3) . . ? C103 N11 C102 124.4(3) . . ? C101 N12 C104 111.6(3) . . ? C101 N12 C105 115.0(3) . . ? C104 N12 C105 133.3(3) . . ? C114 N13 C111 111.3(3) . . ? C114 N13 C109 115.4(3) . . ? C111 N13 C109 133.3(3) . . ? C114 N14 C112 110.6(3) . . ? C114 N14 C113 124.7(3) . . ? C112 N14 C113 124.6(3) . . ? C201 N21 C203 110.7(4) . . ? C201 N21 C202 126.2(3) . . ? C203 N21 C202 123.1(4) . . ? C201 N22 C204 110.7(4) . . ? C201 N22 C205 115.7(3) . . ? C204 N22 C205 133.6(4) . . ? C214 N23 C211 111.3(3) . . ? C214 N23 C209 114.8(3) . . ? C211 N23 C209 133.8(3) . . ? C214 N24 C212 110.9(3) . . ? C214 N24 C213 125.1(3) . . ? C212 N24 C213 123.9(3) . . ? N11 C101 N12 103.5(3) . . ? N11 C101 Fe1 139.4(3) . . ? N12 C101 Fe1 116.7(2) . . ? N11 C102 H10A 109.5 . . ? N11 C102 H10B 109.5 . . ? H10A C102 H10B 109.5 . . ? N11 C102 H10C 109.5 . . ? H10A C102 H10C 109.5 . . ? H10B C102 H10C 109.5 . . ? C104 C103 N11 107.5(3) . . ? C104 C103 H103 126.3 . . ? N11 C103 H103 126.3 . . ? C103 C104 N12 106.7(4) . . ? C103 C104 H104 126.7 . . ? N12 C104 H104 126.7 . . ? C110 C105 C106 122.4(4) . . ? C110 C105 N12 109.4(3) . . ? C106 C105 N12 128.1(4) . . ? C105 C106 C107 116.8(4) . . ? C105 C106 H106 121.6 . . ? C107 C106 H106 121.6 . . ? C108 C107 C106 123.0(4) . . ? C108 C107 H107 118.5 . . ? C106 C107 H107 118.5 . . ? C107 C108 C109 117.6(4) . . ? C107 C108 H108 121.2 . . ? C109 C108 H108 121.2 . . ? C110 C109 C108 121.4(4) . . ? C110 C109 N13 110.0(3) . . ? C108 C109 N13 128.5(3) . . ? C105 C110 C109 118.8(3) . . ? C105 C110 Fe1 120.9(3) . . ? C109 C110 Fe1 120.1(3) . . ? C112 C111 N13 106.2(3) . . ? C112 C111 H111 126.9 . . ? N13 C111 H111 126.9 . . ? C111 C112 N14 108.2(3) . . ? C111 C112 H112 125.9 . . ? N14 C112 H112 125.9 . . ? N14 C113 H11A 109.5 . . ? N14 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? N14 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? N14 C114 N13 103.7(3) . . ? N14 C114 Fe1 139.9(3) . . ? N13 C114 Fe1 116.4(3) . . ? N21 C201 N22 104.0(3) . . ? N21 C201 Fe1 139.4(3) . . ? N22 C201 Fe1 116.4(3) . . ? N21 C202 H20A 109.5 . . ? N21 C202 H20B 109.5 . . ? H20A C202 H20B 109.5 . . ? N21 C202 H20C 109.5 . . ? H20A C202 H20C 109.5 . . ? H20B C202 H20C 109.5 . . ? C204 C203 N21 107.7(4) . . ? C204 C203 H203 126.2 . . ? N21 C203 H203 126.2 . . ? C203 C204 N22 106.9(4) . . ? C203 C204 H204 126.5 . . ? N22 C204 H204 126.5 . . ? C206 C205 C210 121.3(4) . . ? C206 C205 N22 129.1(4) . . ? C210 C205 N22 109.5(3) . . ? C207 C206 C205 117.9(4) . . ? C207 C206 H206 121.0 . . ? C205 C206 H206 121.0 . . ? C208 C207 C206 122.4(4) . . ? C208 C207 H207 118.8 . . ? C206 C207 H207 118.8 . . ? C209 C208 C207 117.4(4) . . ? C209 C208 H208 121.3 . . ? C207 C208 H208 121.3 . . ? C210 C209 C208 122.6(4) . . ? C210 C209 N23 109.3(3) . . ? C208 C209 N23 128.1(4) . . ? C209 C210 C205 118.3(3) . . ? C209 C210 Fe1 121.5(3) . . ? C205 C210 Fe1 120.3(3) . . ? C212 C211 N23 106.3(3) . . ? C212 C211 H211 126.9 . . ? N23 C211 H211 126.9 . . ? C211 C212 N24 107.8(3) . . ? C211 C212 H212 126.1 . . ? N24 C212 H212 126.1 . . ? N24 C213 H21A 109.5 . . ? N24 C213 H21B 109.5 . . ? H21A C213 H21B 109.5 . . ? N24 C213 H21C 109.5 . . ? H21A C213 H21C 109.5 . . ? H21B C213 H21C 109.5 . . ? N24 C214 N23 103.7(3) . . ? N24 C214 Fe1 139.2(3) . . ? N23 C214 Fe1 116.9(2) . . ? F133 P1 F143 94.1(6) . . ? F142 P1 F112 87.1(10) . . ? F142 P1 F15 80.9(7) . . ? F133 P1 F15 84.4(4) . . ? F143 P1 F15 90.1(4) . . ? F112 P1 F15 87.0(6) . . ? F142 P1 F16 101.5(7) . . ? F133 P1 F16 93.5(4) . . ? F143 P1 F16 91.2(4) . . ? F112 P1 F16 93.3(6) . . ? F15 P1 F16 177.6(2) . . ? F133 P1 F123 92.1(6) . . ? F143 P1 F123 172.5(6) . . ? F15 P1 F123 86.3(4) . . ? F16 P1 F123 92.7(4) . . ? F15 P1 F141 95.4(4) . . ? F16 P1 F141 87.0(4) . . ? F15 P1 F121 89.1(3) . . ? F16 P1 F121 88.5(3) . . ? F141 P1 F121 175.5(5) . . ? F15 P1 F131 89.7(3) . . ? F16 P1 F131 90.7(2) . . ? F141 P1 F131 89.2(6) . . ? F121 P1 F131 91.2(5) . . ? F15 P1 F111 91.8(3) . . ? F16 P1 F111 87.9(3) . . ? F141 P1 F111 88.5(6) . . ? F121 P1 F111 91.0(6) . . ? F131 P1 F111 177.4(5) . . ? F142 P1 F122 172.2(10) . . ? F112 P1 F122 87.0(10) . . ? F15 P1 F122 93.7(6) . . ? F16 P1 F122 83.9(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C103 N11 C101 N12 0.9(4) . . . . ? C102 N11 C101 N12 -178.3(3) . . . . ? C103 N11 C101 Fe1 -171.1(3) . . . . ? C102 N11 C101 Fe1 9.7(6) . . . . ? C104 N12 C101 N11 -1.0(4) . . . . ? C105 N12 C101 N11 -179.4(3) . . . . ? C104 N12 C101 Fe1 173.1(2) . . . . ? C105 N12 C101 Fe1 -5.2(4) . . . . ? C101 N11 C103 C104 -0.5(4) . . . . ? C102 N11 C103 C104 178.7(4) . . . . ? N11 C103 C104 N12 -0.2(4) . . . . ? C101 N12 C104 C103 0.7(4) . . . . ? C105 N12 C104 C103 178.7(4) . . . . ? C101 N12 C105 C110 6.0(4) . . . . ? C104 N12 C105 C110 -171.9(4) . . . . ? C101 N12 C105 C106 -172.1(4) . . . . ? C104 N12 C105 C106 10.0(6) . . . . ? C110 C105 C106 C107 -0.5(6) . . . . ? N12 C105 C106 C107 177.4(3) . . . . ? C105 C106 C107 C108 0.7(6) . . . . ? C106 C107 C108 C109 0.6(6) . . . . ? C107 C108 C109 C110 -2.3(6) . . . . ? C107 C108 C109 N13 -179.9(4) . . . . ? C114 N13 C109 C110 -2.5(4) . . . . ? C111 N13 C109 C110 176.3(4) . . . . ? C114 N13 C109 C108 175.4(4) . . . . ? C111 N13 C109 C108 -5.9(6) . . . . ? C106 C105 C110 C109 -1.1(5) . . . . ? N12 C105 C110 C109 -179.4(3) . . . . ? C106 C105 C110 Fe1 173.7(3) . . . . ? N12 C105 C110 Fe1 -4.5(4) . . . . ? C108 C109 C110 C105 2.5(5) . . . . ? N13 C109 C110 C105 -179.5(3) . . . . ? C108 C109 C110 Fe1 -172.4(3) . . . . ? N13 C109 C110 Fe1 5.6(4) . . . . ? C114 N13 C111 C112 -0.5(4) . . . . ? C109 N13 C111 C112 -179.3(4) . . . . ? N13 C111 C112 N14 0.3(4) . . . . ? C114 N14 C112 C111 0.1(4) . . . . ? C113 N14 C112 C111 -175.8(3) . . . . ? C112 N14 C114 N13 -0.4(4) . . . . ? C113 N14 C114 N13 175.5(3) . . . . ? C112 N14 C114 Fe1 -178.9(3) . . . . ? C113 N14 C114 Fe1 -3.1(6) . . . . ? C111 N13 C114 N14 0.6(4) . . . . ? C109 N13 C114 N14 179.6(3) . . . . ? C111 N13 C114 Fe1 179.5(2) . . . . ? C109 N13 C114 Fe1 -1.5(4) . . . . ? C203 N21 C201 N22 -0.1(4) . . . . ? C202 N21 C201 N22 179.6(4) . . . . ? C203 N21 C201 Fe1 -177.1(3) . . . . ? C202 N21 C201 Fe1 2.6(7) . . . . ? C204 N22 C201 N21 0.2(4) . . . . ? C205 N22 C201 N21 179.8(3) . . . . ? C204 N22 C201 Fe1 178.0(3) . . . . ? C205 N22 C201 Fe1 -2.4(4) . . . . ? C201 N21 C203 C204 -0.1(5) . . . . ? C202 N21 C203 C204 -179.8(4) . . . . ? N21 C203 C204 N22 0.2(5) . . . . ? C201 N22 C204 C203 -0.3(5) . . . . ? C205 N22 C204 C203 -179.8(4) . . . . ? C201 N22 C205 C206 -179.8(4) . . . . ? C204 N22 C205 C206 -0.3(7) . . . . ? C201 N22 C205 C210 1.9(5) . . . . ? C204 N22 C205 C210 -178.7(4) . . . . ? C210 C205 C206 C207 -0.6(7) . . . . ? N22 C205 C206 C207 -178.8(4) . . . . ? C205 C206 C207 C208 0.4(7) . . . . ? C206 C207 C208 C209 -0.8(7) . . . . ? C207 C208 C209 C210 1.4(6) . . . . ? C207 C208 C209 N23 -179.8(4) . . . . ? C214 N23 C209 C210 1.0(4) . . . . ? C211 N23 C209 C210 -175.6(4) . . . . ? C214 N23 C209 C208 -177.9(4) . . . . ? C211 N23 C209 C208 5.4(7) . . . . ? C208 C209 C210 C205 -1.6(6) . . . . ? N23 C209 C210 C205 179.4(3) . . . . ? C208 C209 C210 Fe1 178.7(3) . . . . ? N23 C209 C210 Fe1 -0.3(4) . . . . ? C206 C205 C210 C209 1.2(6) . . . . ? N22 C205 C210 C209 179.7(3) . . . . ? C206 C205 C210 Fe1 -179.1(3) . . . . ? N22 C205 C210 Fe1 -0.6(4) . . . . ? C214 N23 C211 C212 0.3(4) . . . . ? C209 N23 C211 C212 177.0(4) . . . . ? N23 C211 C212 N24 0.2(4) . . . . ? C214 N24 C212 C211 -0.6(4) . . . . ? C213 N24 C212 C211 -179.7(4) . . . . ? C212 N24 C214 N23 0.7(4) . . . . ? C213 N24 C214 N23 179.8(3) . . . . ? C212 N24 C214 Fe1 -174.7(3) . . . . ? C213 N24 C214 Fe1 4.4(6) . . . . ? C211 N23 C214 N24 -0.6(4) . . . . ? C209 N23 C214 N24 -178.0(3) . . . . ? C211 N23 C214 Fe1 176.1(2) . . . . ? C209 N23 C214 Fe1 -1.4(4) . . . . ? _refine_diff_density_max 0.804 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.073 _shelx_res_file ; TITL JS_0169_0m_a.res in P2(1)/c js_0169_0m_a_sq.res created by SHELXL-2018/3 at 21:17:12 on 18-Mar-2020 REM Old TITL JS_0169_0m in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.266, Rweak 0.010, Alpha 0.031, Orientation as input REM Formula found by SHELXT: C46 Fe CELL 0.71073 13.6367 8.7801 27.0994 90.000 96.285 90.000 ZERR 4.000 0.0012 0.0008 0.0025 0.000 0.002 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H FE N P F UNIT 112 104 4 32 4 24.0026 LIST 4 SIZE 0.42 0.37 0.25 TEMP 200 L.S. 50 BOND $H CONF FMAP 2 PLAN 20 ABIN ACTA FLAT P1 F111 F121 F131 F141 F112 F122 F132 F142 F113 F123 F133 F143 OMIT 1 0 0 SUMP 1.0 0.0001 1 2 1 3 1 4 WGHT 0.083100 3.569800 FVAR 0.26573 0.39967 0.23608 0.36426 FE1 3 0.734179 0.996738 0.378940 11.00000 0.02607 0.03615 = 0.02879 -0.00028 0.00382 -0.00307 N11 4 0.886889 1.265147 0.387100 11.00000 0.03721 0.04577 = 0.03587 0.00321 -0.00128 -0.01115 N12 4 0.755434 1.294489 0.422123 11.00000 0.03919 0.03779 = 0.03601 0.00087 -0.00084 -0.00066 N13 4 0.550860 0.883917 0.406826 11.00000 0.02991 0.05217 = 0.03707 0.00336 0.00310 -0.00849 N14 4 0.608519 0.695643 0.368657 11.00000 0.03913 0.04184 = 0.03616 0.00512 -0.00548 -0.01042 N21 4 0.597311 1.122569 0.287242 11.00000 0.04892 0.05809 = 0.03964 0.00597 -0.01180 -0.01220 N22 4 0.721900 0.986197 0.272685 11.00000 0.05047 0.06135 = 0.02933 -0.00183 0.00282 -0.01571 N23 4 0.907970 0.822910 0.412569 11.00000 0.02939 0.03905 = 0.04290 -0.00325 0.00373 0.00049 N24 4 0.853432 0.900180 0.479471 11.00000 0.03767 0.04021 = 0.03644 0.00380 0.00213 0.00027 C101 1 0.800461 1.195261 0.393192 11.00000 0.03226 0.04034 = 0.02726 0.00414 -0.00089 -0.00270 C102 1 0.961778 1.205075 0.357244 11.00000 0.04024 0.07333 = 0.05483 -0.00557 0.01553 -0.01753 AFIX 137 H10A 2 0.929920 1.151552 0.329025 11.00000 -1.50000 H10B 2 1.004555 1.136600 0.377062 11.00000 -1.50000 H10C 2 0.999812 1.287804 0.346126 11.00000 -1.50000 AFIX 0 C103 1 0.894684 1.403087 0.412500 11.00000 0.05084 0.04229 = 0.05095 0.00121 -0.00742 -0.01432 AFIX 43 H103 2 0.947528 1.470490 0.413938 11.00000 -1.20000 AFIX 0 C104 1 0.813289 1.420782 0.434196 11.00000 0.05746 0.03727 = 0.04911 -0.00389 -0.00702 -0.00679 AFIX 43 H104 2 0.797970 1.502497 0.453799 11.00000 -1.20000 AFIX 0 C105 1 0.661555 1.246660 0.434760 11.00000 0.03861 0.04018 = 0.03292 0.00276 -0.00031 0.00598 C106 1 0.594142 1.329404 0.458651 11.00000 0.05040 0.05587 = 0.04463 -0.00689 0.00001 0.01687 AFIX 43 H106 2 0.607661 1.427975 0.469981 11.00000 -1.20000 AFIX 0 C107 1 0.505550 1.258043 0.464837 11.00000 0.04173 0.07811 = 0.04760 -0.00285 0.00895 0.02352 AFIX 43 H107 2 0.458729 1.311475 0.480412 11.00000 -1.20000 AFIX 0 C108 1 0.483708 1.111193 0.448911 11.00000 0.03029 0.07819 = 0.04571 0.00704 0.00650 0.00774 AFIX 43 H108 2 0.423454 1.066396 0.453258 11.00000 -1.20000 AFIX 0 C109 1 0.555023 1.032945 0.426177 11.00000 0.02906 0.05500 = 0.03322 0.00586 0.00202 0.00097 C110 1 0.643223 1.100801 0.418107 11.00000 0.02641 0.04539 = 0.02878 0.00194 0.00089 0.00290 C111 1 0.482479 0.766263 0.407183 11.00000 0.03463 0.07149 = 0.04066 0.01278 -0.00214 -0.01999 AFIX 43 H111 2 0.423292 0.768292 0.421268 11.00000 -1.20000 AFIX 0 C112 1 0.518625 0.651072 0.383466 11.00000 0.04304 0.05746 = 0.03931 0.00986 -0.00696 -0.02140 AFIX 43 H112 2 0.488904 0.556457 0.377704 11.00000 -1.20000 AFIX 0 C113 1 0.667882 0.603284 0.338642 11.00000 0.04890 0.04167 = 0.05363 -0.00472 -0.00583 -0.00493 AFIX 137 H11A 2 0.650011 0.625542 0.304146 11.00000 -1.50000 H11B 2 0.656331 0.497374 0.344645 11.00000 -1.50000 H11C 2 0.736456 0.626023 0.347338 11.00000 -1.50000 AFIX 0 C114 1 0.630123 0.841021 0.383177 11.00000 0.03135 0.04300 = 0.03281 0.00434 -0.00221 -0.00254 C201 1 0.675850 1.046674 0.310636 11.00000 0.03686 0.04103 = 0.03840 0.00040 -0.00190 -0.01301 C202 1 0.523765 1.206671 0.310989 11.00000 0.05590 0.06553 = 0.07309 0.00423 -0.01481 0.01154 AFIX 137 H20A 2 0.505127 1.296264 0.291922 11.00000 -1.50000 H20B 2 0.550736 1.235741 0.343847 11.00000 -1.50000 H20C 2 0.466784 1.143636 0.312903 11.00000 -1.50000 AFIX 0 C203 1 0.595228 1.109304 0.236231 11.00000 0.06724 0.08978 = 0.04161 0.01076 -0.01706 -0.01501 AFIX 43 H203 2 0.548379 1.151549 0.212644 11.00000 -1.20000 AFIX 0 C204 1 0.672102 1.025476 0.227070 11.00000 0.07673 0.09352 = 0.02916 -0.00110 -0.00150 -0.03083 AFIX 43 H204 2 0.689330 0.998231 0.195994 11.00000 -1.20000 AFIX 0 C205 1 0.807759 0.900337 0.287077 11.00000 0.04893 0.05499 = 0.04121 -0.00754 0.01434 -0.01529 C206 1 0.869795 0.826292 0.257575 11.00000 0.06927 0.08641 = 0.04691 -0.01729 0.02969 -0.01469 AFIX 43 H206 2 0.858365 0.830157 0.223130 11.00000 -1.20000 AFIX 0 C207 1 0.949187 0.746529 0.280987 11.00000 0.06664 0.08193 = 0.06998 -0.02018 0.04204 -0.00434 AFIX 43 H207 2 0.991561 0.696962 0.261628 11.00000 -1.20000 AFIX 0 C208 1 0.967868 0.737781 0.332130 11.00000 0.04222 0.06018 = 0.07114 -0.00846 0.02195 0.00180 AFIX 43 H208 2 1.021145 0.682634 0.347244 11.00000 -1.20000 AFIX 0 C209 1 0.904353 0.814091 0.359857 11.00000 0.03315 0.04293 = 0.05349 -0.00537 0.01438 -0.00580 C210 1 0.823852 0.893819 0.338573 11.00000 0.03563 0.03942 = 0.04054 -0.00446 0.01068 -0.01011 C211 1 0.974211 0.772839 0.451274 11.00000 0.03142 0.03893 = 0.07445 0.00002 -0.00511 0.00330 AFIX 43 H211 2 1.031240 0.716478 0.448885 11.00000 -1.20000 AFIX 0 C212 1 0.940169 0.821369 0.492812 11.00000 0.04760 0.04841 = 0.04942 0.00968 -0.01029 0.00501 AFIX 43 H212 2 0.969493 0.805140 0.525005 11.00000 -1.20000 AFIX 0 C213 1 0.794812 0.971072 0.514806 11.00000 0.05416 0.06518 = 0.03524 0.00437 0.00599 0.00496 AFIX 137 H21A 2 0.726811 0.973304 0.501186 11.00000 -1.50000 H21B 2 0.817672 1.073207 0.521467 11.00000 -1.50000 H21C 2 0.801222 0.913547 0.545114 11.00000 -1.50000 AFIX 0 C214 1 0.832101 0.903806 0.429650 11.00000 0.02895 0.03182 = 0.03818 0.00125 0.00424 -0.00378 P1 5 0.225204 0.474032 0.414682 11.00000 0.02754 0.05327 = 0.04601 0.00274 0.00343 -0.00138 PART 1 F111 6 0.123907 0.491661 0.439378 21.00000 0.05176 F121 6 0.195977 0.304059 0.397071 21.00000 0.05491 F131 6 0.328818 0.461289 0.392006 21.00000 0.04151 F141 6 0.257397 0.638322 0.436491 21.00000 0.07977 PART 0 PART 2 F112 6 0.135325 0.537722 0.437400 31.00000 0.07648 F122 6 0.166377 0.310686 0.409629 31.00000 0.11075 F132 6 0.315942 0.393529 0.386593 31.00000 0.05332 F142 6 0.265552 0.632768 0.417115 31.00000 0.09486 PART 0 PART 3 F113 6 0.216553 0.642261 0.440901 41.00000 0.09428 F123 6 0.115907 0.447774 0.428460 41.00000 0.07440 F133 6 0.225645 0.321010 0.387904 41.00000 0.09465 F143 6 0.326728 0.521498 0.400781 41.00000 0.09021 PART 0 F15 6 0.175361 0.535434 0.362928 11.00000 0.09012 0.14851 = 0.07091 0.03796 -0.00163 0.04236 F16 6 0.273247 0.405761 0.465949 11.00000 0.06748 0.10195 = 0.05392 0.00727 0.00052 0.02056 HKLF 4 REM JS_0169_0m_a.res in P2(1)/c REM wR2 = 0.168338, GooF = S = 1.03075, Restrained GooF = 1.03750 for all data REM R1 = 0.057086 for 4696 Fo > 4sig(Fo) and 0.083129 for all 6622 data REM 416 parameters refined using 11 restraints END WGHT 0.0831 3.5700 REM Highest difference peak 0.804, deepest hole -0.578, 1-sigma level 0.073 Q1 1 0.1074 0.5064 0.4163 11.00000 0.05 0.80 Q2 1 0.3028 0.5072 0.4595 11.00000 0.05 0.59 Q3 1 0.1886 0.3535 0.3796 11.00000 0.05 0.59 Q4 1 0.2260 0.6640 0.4193 11.00000 0.05 0.59 Q5 1 0.1406 0.4909 0.4633 11.00000 0.05 0.57 Q6 1 0.3194 0.5783 0.4326 11.00000 0.05 0.55 Q7 1 0.3106 0.5195 0.3792 11.00000 0.05 0.54 Q8 1 0.3475 0.4880 0.4196 11.00000 0.05 0.53 Q9 1 0.1311 0.4179 0.4526 11.00000 0.05 0.53 Q10 1 0.2674 0.6248 0.3815 11.00000 0.05 0.42 Q11 1 0.2813 0.3278 0.3930 11.00000 0.05 0.38 Q12 1 0.6726 1.0749 0.4033 11.00000 0.05 0.37 Q13 1 0.1753 0.5959 0.4544 11.00000 0.05 0.35 Q14 1 0.2292 0.6234 0.4607 11.00000 0.05 0.35 Q15 1 0.8069 0.9685 0.4063 11.00000 0.05 0.34 Q16 1 0.2113 0.2786 0.4186 11.00000 0.05 0.33 Q17 1 0.9092 0.8184 0.3831 11.00000 0.05 0.32 Q18 1 0.6657 1.0095 0.4001 11.00000 0.05 0.32 Q19 1 0.7408 1.0544 0.4112 11.00000 0.05 0.30 Q20 1 0.2392 0.3106 0.4301 11.00000 0.05 0.30 ; _shelx_res_checksum 10491 _shelx_hkl_file ; 1 0 0 12.40 0.60 -1 0 0 11.20 0.70 2 0 0 6374.26 129.39 -2 0 0 6192.88 129.09 -2 0 0 6267.87 129.69 -3 0 0 1138.99 23.40 3 0 0 1101.69 24.60 -3 0 0 1148.69 23.60 -3 0 0 1120.49 25.00 -4 0 0 1636.34 33.80 -4 0 0 1622.94 34.00 -4 0 0 1633.84 36.00 -5 0 0 0.80 0.40 -5 0 0 1.10 1.00 -5 0 0 1.10 0.40 5 0 0 2.80 1.00 6 0 0 32.70 2.80 -6 0 0 29.50 1.30 -6 0 0 27.20 2.90 7 0 0 84.09 4.20 -7 0 0 85.29 2.50 -7 0 0 92.69 4.90 8 0 0 89.29 4.50 -8 0 0 90.49 5.20 -8 0 0 78.39 2.30 9 0 0 12.20 2.50 -9 0 0 16.20 3.10 -10 0 0 -3.10 1.50 10 0 0 2.00 1.50 11 0 0 11.10 2.90 -11 0 0 9.00 2.80 12 0 0 4.50 2.40 -12 0 0 3.10 2.50 13 0 0 163.48 8.40 -13 0 0 162.88 9.20 14 0 0 36.20 5.00 -14 0 0 35.40 5.80 -15 0 0 32.40 5.60 15 0 0 22.30 4.60 16 0 0 14.60 4.10 -16 0 0 13.80 4.70 0 -1 0 4.10 0.50 0 -1 0 3.00 0.40 0 1 0 5.10 0.50 0 1 0 4.40 0.70 1 -1 0 15.90 0.90 -1 -1 0 16.50 1.00 -1 1 0 23.70 1.40 -1 1 0 23.60 1.10 -2 -1 0 544.45 12.40 2 -1 0 559.44 12.40 2 1 0 529.55 11.80 -2 1 0 558.54 13.00 2 1 0 549.35 12.80 2 1 0 552.64 12.20 -2 1 0 567.44 12.80 -3 -1 0 388.36 9.60 3 -1 0 382.96 9.40 -3 1 0 397.66 9.70 3 1 0 386.76 9.70 3 1 0 385.46 8.50 3 1 0 374.06 8.20 -3 1 0 380.56 9.90 -4 -1 0 351.06 9.40 -4 1 0 357.16 9.10 4 1 0 343.67 9.20 -4 1 0 340.37 9.70 5 -1 0 3.00 1.10 -5 -1 0 3.00 1.10 5 1 0 1.40 0.90 -5 1 0 0.40 1.00 -5 1 0 1.20 0.90 -6 -1 0 11.20 1.90 6 -1 0 10.30 1.70 -6 1 0 6.10 1.80 6 1 0 9.50 1.80 -6 1 0 12.00 1.70 7 -1 0 32.10 3.10 -7 -1 0 34.30 3.40 7 1 0 33.90 3.20 -7 1 0 34.00 2.60 -7 1 0 36.50 3.70 -8 -1 0 71.49 4.70 8 -1 0 79.49 4.40 -8 1 0 79.59 5.00 8 1 0 84.59 4.70 -8 1 0 75.29 3.40 9 -1 0 13.50 2.60 -9 -1 0 6.80 2.10 -9 1 0 7.10 2.60 9 1 0 13.50 2.60 -9 1 0 11.00 1.80 -10 -1 0 43.20 4.80 10 -1 0 34.40 4.00 10 1 0 40.30 4.30 -10 1 0 36.60 2.70 -10 1 0 38.70 4.90 11 -1 0 2.10 2.20 -11 -1 0 -1.40 2.10 -11 1 0 5.80 2.50 11 1 0 2.80 2.10 -12 -1 0 -3.90 1.70 12 -1 0 0.20 2.20 12 1 0 -0.70 2.20 -12 1 0 0.00 2.10 -13 -1 0 -1.80 2.20 13 -1 0 2.60 2.60 -13 1 0 0.90 2.40 13 1 0 1.00 2.30 14 -1 0 50.69 5.90 -14 -1 0 43.50 6.20 14 1 0 53.69 6.10 -14 1 0 35.90 5.90 -15 -1 0 -1.60 2.60 15 -1 0 -1.40 2.50 15 1 0 -1.30 2.70 -15 1 0 4.20 3.20 -16 -1 0 -3.30 2.60 16 -1 0 3.90 3.50 16 1 0 2.50 3.90 -16 1 0 3.10 3.70 0 -2 0 1020.40 22.70 0 2 0 1038.60 23.80 0 2 0 1047.20 22.40 1 -2 0 294.97 7.60 -1 -2 0 295.87 7.60 -1 -2 0 304.57 7.10 -1 2 0 310.87 8.80 -1 2 0 294.27 7.40 1 2 0 289.37 8.30 2 -2 0 9866.31 200.88 -2 -2 0 9840.92 200.68 -2 -2 0 9999.00 200.48 -2 2 0 9628.54 200.98 2 2 0 9547.75 201.28 -2 2 0 9562.04 202.18 -3 -2 0 16.90 1.60 3 -2 0 17.20 1.70 -3 2 0 17.90 2.20 -3 2 0 13.40 1.70 3 2 0 15.70 1.70 3 2 0 16.00 2.00 -4 -2 0 244.68 7.00 4 -2 0 233.78 6.90 -4 2 0 228.58 7.40 4 2 0 222.28 7.30 4 2 0 230.48 6.30 -4 2 0 235.28 7.70 -5 -2 0 77.49 3.80 5 -2 0 82.39 3.80 5 2 0 80.69 4.00 -5 2 0 84.99 4.20 5 2 0 79.59 2.80 -5 2 0 89.39 4.30 -6 -2 0 64.99 3.80 6 -2 0 78.99 3.90 -6 2 0 65.09 4.10 6 2 0 73.39 2.60 6 2 0 66.09 3.90 -6 2 0 72.29 4.00 6 2 0 64.09 2.10 -7 -2 0 418.46 12.70 7 -2 0 443.86 12.40 7 2 0 442.06 12.60 -7 2 0 432.76 12.30 -7 2 0 430.06 13.30 -8 -2 0 0.00 1.40 8 -2 0 1.60 1.40 8 2 0 1.20 1.60 -8 2 0 0.90 1.50 -8 2 0 -0.30 1.20 -9 -2 0 -0.10 1.40 9 -2 0 1.40 1.50 -9 2 0 1.00 1.30 9 2 0 -2.20 1.30 -9 2 0 -0.60 1.50 10 -2 0 79.09 5.90 -10 -2 0 60.39 5.80 -10 2 0 60.79 5.80 -10 2 0 60.49 3.90 10 2 0 68.69 5.60 11 -2 0 74.89 6.20 -11 -2 0 63.39 6.10 11 2 0 65.69 5.70 -11 2 0 65.99 6.50 12 -2 0 4.60 2.20 -12 -2 0 4.90 2.80 -12 2 0 3.40 2.90 12 2 0 2.20 2.30 -13 -2 0 1.90 2.80 13 -2 0 4.90 2.50 13 2 0 9.60 2.90 -13 2 0 5.60 3.10 -14 -2 0 3.10 3.30 14 -2 0 4.20 2.60 -14 2 0 6.60 3.50 14 2 0 5.90 3.30 15 -2 0 47.60 6.10 -15 -2 0 39.20 6.10 15 2 0 49.20 6.70 -15 2 0 40.70 6.60 -16 -2 0 -2.10 3.70 16 -2 0 2.30 3.20 -16 2 0 0.60 4.00 16 2 0 0.80 3.70 0 -3 0 0.20 0.70 0 3 0 -0.30 1.00 0 3 0 0.40 0.70 -1 -3 0 110.99 3.50 -1 -3 0 104.39 4.00 1 -3 0 108.59 4.20 1 3 0 116.79 5.10 -1 3 0 115.49 3.90 -1 3 0 113.29 5.30 -2 -3 0 2.00 0.80 2 -3 0 2.90 1.10 -2 -3 0 4.10 1.20 2 3 0 6.00 1.70 -2 3 0 2.30 1.10 -2 3 0 0.00 1.20 -3 -3 0 247.18 7.20 -3 -3 0 249.18 6.90 3 -3 0 238.38 7.30 -3 3 0 243.48 7.50 -3 3 0 241.08 8.60 3 3 0 245.08 7.90 -4 -3 0 31.10 2.60 4 -3 0 27.80 2.50 4 3 0 26.50 2.70 4 3 0 29.20 3.20 -4 3 0 27.80 3.30 -4 3 0 32.40 3.10 5 -3 0 4.50 1.40 -5 -3 0 6.10 1.50 5 3 0 6.20 1.40 -5 3 0 6.20 1.70 -5 3 0 3.90 1.70 5 3 0 6.00 2.00 -6 -3 0 507.55 13.90 6 -3 0 506.85 13.80 6 3 0 507.85 12.60 6 3 0 519.65 14.50 -6 3 0 508.95 14.60 -6 3 0 493.25 14.80 -7 -3 0 6.40 1.80 7 -3 0 8.00 1.90 -7 3 0 7.70 2.40 7 3 0 5.10 1.10 -7 3 0 5.40 2.00 7 3 0 7.20 2.10 -8 -3 0 40.10 4.00 8 -3 0 38.60 3.80 -8 3 0 38.60 4.00 -8 3 0 45.00 4.70 8 3 0 34.60 3.80 8 3 0 35.80 1.60 9 -3 0 82.49 5.00 -9 -3 0 94.69 5.80 9 3 0 88.69 5.40 -9 3 0 96.29 5.40 -9 3 0 101.99 6.20 10 -3 0 2.40 2.10 -10 -3 0 5.30 2.40 -10 3 0 6.90 2.30 -10 3 0 5.20 2.50 10 3 0 5.60 2.30 11 -3 0 6.90 2.60 -11 -3 0 7.10 2.80 11 3 0 12.00 3.10 -11 3 0 5.50 2.60 -11 3 0 10.30 2.40 -12 -3 0 11.00 3.30 12 -3 0 10.50 2.90 -12 3 0 22.30 4.40 12 3 0 12.20 3.50 13 -3 0 2.00 2.50 -13 -3 0 0.50 2.50 -13 3 0 2.60 3.30 13 3 0 4.20 2.60 -14 -3 0 2.00 4.20 14 -3 0 2.50 2.60 -14 3 0 7.50 3.50 14 3 0 3.90 3.10 -15 -3 0 -4.90 2.80 15 -3 0 4.70 2.90 15 3 0 4.30 3.10 -15 3 0 3.10 3.40 16 -3 0 3.90 3.50 -16 -3 0 4.70 4.20 16 3 0 7.80 4.20 -16 3 0 4.70 4.10 0 -4 0 272.67 8.40 0 4 0 299.97 10.30 0 4 0 280.37 7.80 1 -4 0 42.80 3.30 -1 -4 0 39.10 3.10 -1 4 0 47.10 4.50 1 4 0 44.10 4.20 -1 4 0 44.00 2.60 1 4 0 45.40 2.70 -2 -4 0 130.29 5.10 -2 -4 0 129.29 4.40 2 -4 0 127.59 5.20 -2 4 0 130.79 6.50 -2 4 0 131.09 4.80 2 4 0 129.29 6.20 -3 -4 0 413.86 10.70 3 -4 0 405.66 11.60 -3 -4 0 420.56 11.40 -3 4 0 415.86 11.40 3 4 0 407.16 12.50 -3 4 0 394.46 13.30 4 -4 0 709.63 17.90 -4 -4 0 688.43 17.00 -4 -4 0 703.13 17.40 4 4 0 714.43 18.40 -4 4 0 679.53 19.70 -4 4 0 681.93 17.70 -5 -4 0 434.16 11.80 5 -4 0 428.26 12.40 -5 4 0 429.16 12.70 5 4 0 429.26 12.40 5 4 0 422.36 13.60 -5 4 0 430.06 14.10 6 -4 0 81.89 4.50 -6 -4 0 84.59 4.50 6 4 0 77.69 4.20 6 4 0 84.19 5.30 -6 4 0 83.79 6.40 -6 4 0 86.99 5.00 7 -4 0 49.00 4.40 -7 -4 0 37.30 3.70 7 4 0 44.70 3.40 -7 4 0 41.20 4.60 -7 4 0 48.20 4.60 7 4 0 39.50 4.30 8 -4 0 93.99 5.30 -8 -4 0 89.49 5.40 8 4 0 86.39 5.50 -8 4 0 91.49 6.00 -8 4 0 92.99 7.20 8 4 0 89.59 4.00 9 -4 0 0.10 1.40 -9 -4 0 -1.60 1.90 9 4 0 4.30 2.10 -9 4 0 -2.60 1.60 -9 4 0 -1.40 1.70 -10 -4 0 37.30 4.60 10 -4 0 36.00 4.40 10 4 0 39.10 4.80 -10 4 0 38.80 5.20 -10 4 0 37.20 4.50 -11 -4 0 0.90 2.10 11 -4 0 3.70 2.10 11 4 0 -0.30 1.80 -11 4 0 -1.40 1.90 -11 4 0 4.70 3.00 12 -4 0 0.00 2.20 -12 -4 0 3.20 2.40 12 4 0 -1.30 2.10 -12 4 0 -1.10 2.10 13 -4 0 42.60 5.40 -13 -4 0 51.09 6.40 -13 4 0 40.40 5.90 13 4 0 53.59 6.60 -14 -4 0 2.20 3.10 14 -4 0 -0.60 2.60 -14 4 0 -1.60 2.70 14 4 0 3.10 3.10 15 -4 0 4.00 3.30 -15 -4 0 9.40 4.60 -15 4 0 7.30 4.40 15 4 0 5.30 4.00 0 -5 0 0.00 1.20 0 5 0 1.10 1.80 0 5 0 -0.10 1.00 1 -5 0 26.70 3.00 -1 -5 0 16.50 2.40 1 5 0 21.00 3.50 -1 5 0 20.30 2.20 -1 5 0 17.50 3.60 1 5 0 25.30 2.50 -2 -5 0 7.20 1.80 2 -5 0 6.10 1.90 2 5 0 9.60 2.00 -2 5 0 4.20 1.50 2 5 0 7.00 2.30 -2 5 0 3.10 2.20 -3 -5 0 355.46 10.80 -3 -5 0 364.06 9.90 3 -5 0 381.76 11.30 -3 5 0 323.17 12.70 3 5 0 362.86 12.30 -3 5 0 349.87 10.50 -4 -5 0 12.20 2.20 -4 -5 0 14.10 2.10 4 -5 0 11.30 2.30 -4 5 0 12.30 3.10 -4 5 0 13.40 2.40 4 5 0 8.80 2.40 5 -5 0 232.58 8.60 -5 -5 0 227.28 7.70 5 5 0 226.98 8.90 -5 5 0 217.98 8.40 -5 5 0 217.08 9.90 5 5 0 241.68 10.00 -6 -5 0 143.99 6.20 6 -5 0 145.89 6.70 6 5 0 148.59 6.70 -6 5 0 132.19 6.80 6 5 0 169.38 8.10 -6 5 0 164.08 8.50 7 -5 0 80.69 5.00 -7 -5 0 71.29 4.50 -7 5 0 67.39 5.70 -7 5 0 78.59 7.10 7 5 0 74.29 5.20 7 5 0 79.69 6.60 -8 -5 0 37.00 4.10 8 -5 0 28.70 3.70 -8 5 0 43.80 4.80 -8 5 0 39.00 5.10 8 5 0 27.60 4.20 -9 -5 0 1.60 2.10 9 -5 0 -1.30 1.50 9 5 0 -2.00 1.90 -9 5 0 0.10 2.10 -9 5 0 3.60 2.70 -10 -5 0 30.20 4.30 10 -5 0 33.80 4.40 -10 5 0 40.10 5.40 10 5 0 39.50 5.10 -10 5 0 43.10 5.40 11 -5 0 3.70 2.20 -11 -5 0 3.90 2.60 11 5 0 2.60 2.40 -11 5 0 4.40 3.00 -11 5 0 -1.10 2.60 -12 -5 0 4.50 3.00 12 -5 0 3.30 2.60 12 5 0 1.10 2.70 -12 5 0 -0.60 2.70 -12 5 0 2.40 3.30 13 -5 0 3.70 2.80 -13 -5 0 6.60 3.60 13 5 0 7.80 3.80 -13 5 0 2.90 3.10 -14 -5 0 -2.20 3.60 14 -5 0 -1.70 2.70 14 5 0 4.20 3.70 -14 5 0 1.50 3.60 15 -5 0 8.30 3.90 -15 -5 0 2.10 3.80 15 5 0 3.90 4.30 -15 5 0 6.70 4.00 0 -6 0 140.59 6.40 0 6 0 131.09 5.30 0 6 0 141.29 8.00 1 -6 0 1.50 1.70 -1 -6 0 7.00 2.20 1 6 0 6.50 1.80 1 6 0 2.90 2.20 -1 6 0 1.30 1.30 -1 6 0 3.40 2.20 -2 -6 0 248.08 8.90 2 -6 0 242.88 9.00 2 6 0 245.78 8.10 -2 6 0 233.48 7.90 2 6 0 230.28 10.30 -2 6 0 245.88 11.10 -3 -6 0 20.90 3.00 3 -6 0 23.20 3.20 -3 6 0 16.70 3.90 -3 6 0 23.20 2.90 3 6 0 26.60 3.30 3 6 0 21.70 3.70 4 -6 0 123.89 6.30 -4 -6 0 133.29 5.40 -4 -6 0 123.09 6.00 -4 6 0 134.59 6.10 4 6 0 129.49 7.30 -4 6 0 128.89 8.10 5 -6 0 21.10 3.30 -5 -6 0 22.10 3.10 -5 -6 0 25.10 3.00 -5 6 0 25.20 4.60 5 6 0 21.60 3.70 -5 6 0 22.40 3.30 -6 -6 0 313.57 10.40 6 -6 0 316.17 11.50 6 6 0 352.06 12.10 -6 6 0 329.97 11.60 6 6 0 333.27 13.30 -6 6 0 341.67 13.80 -7 -6 0 13.00 2.70 7 -6 0 17.60 3.40 7 6 0 18.50 3.90 -7 6 0 11.40 3.10 7 6 0 14.80 3.10 -7 6 0 15.40 4.30 -8 -6 0 60.79 5.20 8 -6 0 61.39 5.90 -8 6 0 63.19 7.10 -8 6 0 70.09 6.50 8 6 0 59.89 6.40 9 -6 0 10.20 2.90 -9 -6 0 14.50 3.40 -9 6 0 11.80 3.60 9 6 0 8.90 3.40 -9 6 0 9.00 3.30 10 -6 0 -0.60 2.20 -10 -6 0 -3.00 2.40 -10 6 0 1.80 2.40 -10 6 0 0.00 2.60 10 6 0 1.70 2.20 -11 -6 0 11.50 3.80 11 -6 0 14.40 3.70 -11 6 0 11.20 3.70 -11 6 0 13.20 3.80 11 6 0 19.90 4.70 12 -6 0 2.90 3.00 -12 -6 0 4.60 3.40 -12 6 0 3.10 3.60 12 6 0 2.30 3.70 -12 6 0 -1.10 2.60 -13 -6 0 -3.30 3.50 13 -6 0 2.30 2.80 13 6 0 0.40 3.30 -13 6 0 2.50 3.60 -14 -6 0 1.00 4.60 14 -6 0 1.00 3.20 14 6 0 2.60 4.10 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2.70 8 4 -4 25.90 3.70 -7 -4 4 48.50 3.90 7 -4 -4 35.30 3.70 -7 4 4 42.80 4.50 -7 4 4 38.00 4.60 7 4 -4 51.59 5.10 7 4 -4 45.10 3.20 -6 -4 4 182.08 6.40 6 -4 -4 184.38 7.10 -6 4 4 171.98 8.40 6 4 -4 193.48 8.30 6 4 -4 190.78 6.50 -6 4 4 170.48 7.60 5 -4 -4 9.40 1.90 -5 -4 4 5.90 1.40 5 4 -4 7.00 1.80 -5 4 4 6.80 2.70 5 4 -4 7.30 2.40 -5 4 4 10.10 2.20 4 -4 -4 104.79 4.80 -4 -4 4 97.29 3.70 4 4 -4 105.49 5.80 -4 4 4 111.99 5.40 4 4 -4 98.89 4.90 3 -4 -4 41.60 3.50 -3 -4 4 46.80 3.50 3 -4 -4 45.60 3.60 -3 -4 4 42.30 2.00 3 4 -4 43.40 3.80 -3 4 4 41.40 3.80 -2 -4 4 291.87 8.90 2 -4 -4 283.17 9.10 2 -4 -4 310.57 9.10 2 4 -4 296.47 9.90 -2 4 4 292.17 9.40 1 -4 -4 0.10 0.90 1 -4 -4 -0.70 0.90 -1 -4 4 0.30 1.00 1 4 -4 -0.10 1.20 -1 4 4 -0.90 1.10 0 -4 -4 1067.49 24.70 0 -4 -4 1031.40 24.90 0 -4 4 1075.79 24.80 0 4 4 1025.00 25.30 0 4 -4 1006.00 22.30 0 4 -4 1116.09 22.50 0 4 -4 1066.59 26.50 -1 -4 -4 92.29 4.10 1 -4 4 90.39 4.20 -1 -4 -4 97.49 4.30 -1 4 -4 92.89 5.30 1 4 4 96.29 4.90 -1 4 -4 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4 5.40 2.80 9 5 -4 0.30 2.50 8 -5 -4 4.80 2.10 -8 -5 4 10.40 2.30 -8 5 4 1.60 2.70 8 5 -4 7.20 2.00 8 5 -4 7.90 3.00 -8 5 4 5.50 2.40 7 -5 -4 10.40 2.50 -7 -5 4 14.30 2.30 7 5 -4 14.10 3.40 7 5 -4 12.20 2.80 -7 5 4 12.00 3.50 -7 5 4 13.20 3.10 -6 -5 4 13.20 2.10 6 -5 -4 15.00 2.60 6 5 -4 15.60 3.30 -6 5 4 17.90 3.90 6 5 -4 20.50 2.80 -6 5 4 13.80 2.90 -5 -5 4 3.60 1.40 5 -5 -4 5.40 1.90 -5 5 4 -0.50 1.90 5 5 -4 4.20 2.40 5 5 -4 0.90 1.70 -5 5 4 6.30 2.20 -4 -5 4 21.40 2.00 4 -5 -4 17.80 2.70 -4 -5 4 17.10 2.50 -4 5 4 21.40 4.00 -4 5 4 18.20 2.90 4 5 -4 17.90 2.80 -3 -5 4 27.20 3.00 3 -5 -4 27.30 3.20 -3 -5 4 26.50 1.70 -3 5 4 31.20 3.50 3 5 -4 35.30 4.00 -3 5 4 21.50 3.90 -2 -5 4 5.50 1.70 2 -5 -4 4.40 1.60 -2 5 4 5.20 2.40 -2 5 4 3.60 1.60 2 5 -4 2.30 0.90 2 5 -4 3.80 2.10 1 -5 -4 52.49 4.00 -1 -5 4 63.29 3.80 1 5 -4 51.69 1.80 1 5 -4 52.29 5.00 -1 5 4 52.89 4.40 0 -5 4 194.18 7.20 0 -5 -4 195.38 7.10 0 5 -4 180.78 4.90 0 5 -4 197.18 8.60 0 5 4 199.78 7.70 1 -5 4 17.30 2.40 -1 -5 -4 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10.70 3 -5 -9 48.70 4.10 3 -5 -9 54.79 4.70 -3 -5 9 58.79 4.60 3 5 -9 46.80 4.40 -3 5 9 57.59 5.40 2 -5 -9 133.29 6.30 2 -5 -9 147.89 6.10 -2 -5 9 132.09 5.90 -2 5 9 132.99 7.20 2 5 -9 132.99 6.60 1 -5 -9 39.10 3.50 -1 -5 9 35.70 3.40 1 -5 -9 32.80 3.70 -1 5 9 32.90 4.10 1 5 -9 32.10 4.10 0 -5 9 93.39 4.70 0 -5 -9 80.19 4.80 0 -5 -9 86.29 4.50 0 5 9 94.39 6.10 0 5 -9 76.29 6.20 1 -5 9 2.30 1.50 -1 -5 -9 2.30 1.50 -1 -5 -9 -1.10 0.90 1 5 9 -0.50 2.00 -1 5 -9 -0.20 1.80 -1 5 -9 0.80 0.70 -2 -5 -9 24.90 3.20 2 -5 9 26.70 3.00 -2 -5 -9 27.50 3.00 -2 5 -9 31.30 2.20 -2 5 -9 23.50 3.70 -3 -5 -9 13.50 2.30 -3 -5 -9 8.70 1.90 3 -5 9 10.40 2.10 -3 -5 -9 14.60 2.70 -3 5 -9 11.80 1.80 -3 5 -9 15.50 3.20 -4 -5 -9 5.00 2.00 -4 -5 -9 6.00 1.80 4 -5 9 10.60 2.30 -4 -5 -9 5.10 1.70 -4 5 -9 4.30 1.60 -4 5 -9 4.80 2.30 5 -5 9 68.89 5.20 -5 -5 -9 73.09 6.00 -5 -5 -9 77.49 4.60 -5 5 -9 70.59 6.10 -5 5 -9 76.39 4.30 5 5 9 87.69 5.60 -6 -5 -9 32.90 4.30 6 -5 9 31.20 3.50 -6 -5 -9 40.00 3.70 6 5 9 30.90 4.00 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3.30 9 -6 -9 0.00 2.50 -9 6 9 -0.30 2.40 -9 6 9 5.40 3.90 9 6 -9 6.20 3.30 8 -6 -9 25.10 4.00 -8 6 9 28.70 4.70 -8 6 9 34.70 6.00 8 6 -9 32.20 5.30 8 6 -9 25.40 4.70 7 -6 -9 35.20 4.40 7 6 -9 34.60 5.20 7 6 -9 36.50 4.10 -7 6 9 35.20 4.90 6 -6 -9 54.49 5.30 6 -6 -9 65.79 5.90 -6 6 9 66.49 6.60 6 6 -9 43.50 5.70 6 6 -9 54.99 4.90 5 -6 -9 65.19 5.80 5 -6 -9 63.19 5.40 5 6 -9 65.39 5.40 -5 6 9 59.79 6.00 5 6 -9 68.09 6.90 4 -6 -9 44.30 4.70 4 -6 -9 50.09 4.70 -4 6 9 40.60 4.90 4 6 -9 42.30 4.50 -3 -6 9 0.60 1.50 3 -6 -9 -0.90 1.40 3 -6 -9 -0.80 1.70 3 6 -9 2.30 1.80 -3 6 9 -4.20 1.70 -2 -6 9 121.89 6.20 2 -6 -9 118.69 6.40 2 -6 -9 118.29 5.90 -2 6 9 108.49 6.80 2 6 -9 104.99 6.50 -1 -6 9 5.40 2.10 1 -6 -9 5.80 2.20 1 -6 -9 7.80 2.10 -1 6 9 9.30 2.90 1 6 -9 8.50 2.70 0 -6 -9 69.59 4.40 0 -6 9 68.49 4.50 0 -6 -9 70.59 5.60 0 6 9 73.99 6.60 0 6 -9 66.19 6.30 1 -6 9 49.60 4.60 -1 -6 -9 27.00 3.20 -1 -6 -9 36.60 4.20 1 6 9 46.90 5.40 -1 6 -9 37.60 5.00 2 -6 9 113.99 6.10 -2 -6 -9 130.39 6.10 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3.20 4.00 -4 8 10 3.50 3.10 3 -8 -10 53.19 5.50 -3 -8 10 60.89 5.90 3 8 -10 55.49 6.20 -3 8 10 63.29 8.40 -3 8 10 62.39 6.70 -2 -8 10 5.10 2.60 2 -8 -10 4.20 2.70 -2 8 10 7.70 3.80 -2 8 10 6.10 4.00 2 8 -10 6.50 3.20 -1 -8 10 47.00 5.20 1 -8 -10 46.70 5.10 1 8 -10 50.09 6.40 -1 8 10 49.70 6.00 0 -8 10 4.20 2.50 0 -8 -10 -0.70 2.10 0 8 -10 3.10 2.60 0 8 10 2.10 3.00 -1 -8 -10 103.49 6.30 1 -8 10 100.89 6.40 1 8 10 94.19 8.40 -1 8 -10 109.89 9.50 2 -8 10 -4.10 1.80 -2 -8 -10 0.80 2.10 2 8 10 3.00 3.30 -2 8 -10 -2.20 2.30 -3 -8 -10 83.69 6.60 3 -8 10 79.29 6.90 3 8 10 77.69 8.90 3 8 10 74.59 7.80 -3 8 -10 68.69 7.60 4 -8 10 -0.40 2.00 -4 -8 -10 2.60 2.50 4 8 10 1.80 3.50 -4 8 -10 2.70 3.50 4 8 10 4.90 3.90 5 -8 10 60.69 6.30 -5 -8 -10 51.29 5.20 -5 8 -10 50.29 7.00 5 8 10 46.70 7.30 5 8 10 44.10 6.60 -6 -8 -10 -1.40 2.90 6 -8 10 3.70 2.50 6 8 10 -6.80 2.70 6 8 10 1.90 3.90 -6 8 -10 -0.10 2.70 -7 -8 -10 68.09 7.10 7 -8 10 58.79 6.30 7 8 10 63.49 7.90 -7 8 -10 49.90 6.80 -8 -8 -10 0.60 3.70 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33 -0.50 0.00 -3 4 33 0.47 0.00 -2 4 33 0.20 0.00 -1 4 33 -0.08 0.00 0 4 33 0.06 0.00 -6 0 34 0.39 0.00 -5 0 34 -0.43 0.00 -4 0 34 -0.87 0.00 -3 0 34 0.05 0.00 -2 0 34 0.86 0.00 -1 0 34 0.29 0.00 0 0 34 0.39 0.00 1 0 34 0.63 0.00 2 0 34 -0.81 0.00 3 0 34 -1.10 0.00 -6 1 34 0.06 0.00 -5 1 34 0.49 0.00 -4 1 34 0.14 0.00 -3 1 34 -0.48 0.00 -2 1 34 -0.70 0.00 -1 1 34 -0.38 0.00 0 1 34 0.09 0.00 1 1 34 0.74 0.00 2 1 34 0.78 0.00 -5 2 34 -0.16 0.00 -4 2 34 0.98 0.00 -3 2 34 0.47 0.00 -2 2 34 -0.26 0.00 -1 2 34 -0.19 0.00 0 2 34 -0.39 0.00 1 2 34 -0.36 0.00 2 2 34 0.07 0.00 -3 3 34 -0.18 0.00 -2 3 34 -0.54 0.00 -1 3 34 0.29 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 160617) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material 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 _platon_squeeze_void_content 1 0.230 -0.056 0.300 126 40 ' ' 2 0.770 0.056 0.700 126 40 ' ' 3 0.770 0.444 0.200 126 40 ' ' 4 0.230 0.556 0.800 126 40 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL JS_0169_0m_a.res in P2(1)/c CELL 13.6367 8.7801 27.0990 90.00 96.29 90.00 SPGR P21/c # Solvent Accessible Volume = 505 # Electrons Found in S.A.V. = 161 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.793 0.377 0.259 ! 15.82 eA-3 C102 0.253 0.026 0.343 ! 8.89 eA-3 C103 0.208 0.874 0.308 ! 3.55 eA-3 Q104 0.234 0.652 0.439 ! 1.92 eA-3 Q105 0.118 0.429 0.427 ! 1.92 eA-3 Q106 0.683 0.916 0.107 ! 1.91 eA-3 Q107 0.324 0.539 0.398 ! 1.54 eA-3 Q108 0.182 0.496 0.367 ! 1.19 eA-3 Q109 0.750 0.655 0.621 ! 1.17 eA-3 Q110 0.547 0.226 0.957 ! 1.12 eA-3 Q111 0.160 0.182 0.914 ! 1.09 eA-3 Q112 0.750 0.505 0.861 ! 1.09 eA-3 Q113 0.268 0.088 0.981 ! 1.02 eA-3 Q114 0.370 0.322 0.618 ! 1.01 eA-3 Q115 0.772 0.969 0.384 ! 0.95 eA-3 Q116 0.702 0.026 0.230 ! 0.94 eA-3 Q117 0.465 0.410 0.092 ! 0.91 eA-3 Q118 0.714 0.304 0.420 ! 0.90 eA-3 Q119 0.735 0.966 0.400 ! 0.88 eA-3 Q120 0.498 0.309 0.091 ! 0.88 eA-3 Q121 0.685 0.092 0.302 ! 0.87 eA-3 Q122 0.685 0.405 0.807 ! 0.87 eA-3 Q123 0.161 0.910 0.941 ! 0.86 eA-3 Q124 0.235 0.032 0.894 ! 0.85 eA-3 Q125 0.719 0.025 0.271 ! 0.83 eA-3 Q126 0.281 0.975 0.729 ! 0.83 eA-3 Q127 0.855 0.873 0.474 ! 0.82 eA-3 Q128 0.037 0.303-0.001 ! 0.82 eA-3 Q129 0.928 0.775 0.772 ! 0.81 eA-3 Q130 0.644 0.693 0.877 ! 0.79 eA-3 Q131 0.793 0.387 0.426 ! 0.77 eA-3 Q132 0.888 0.684 0.749 ! 0.74 eA-3 Q133 0.595 0.073 0.424 ! 0.74 eA-3 Q134 0.385 0.661 0.263 ! 0.72 eA-3 Q135 0.516 0.616 0.077 ! 0.71 eA-3 Q136 0.018 0.215 0.664 ! 0.71 eA-3 Q137 0.623 0.078 0.304 ! 0.70 eA-3 Q138 0.382 0.533 0.791 ! 0.66 eA-3 Q139 0.812 0.559 0.848 ! 0.66 eA-3 Q140 0.064 0.721 0.157 ! 0.65 eA-3 Q141 0.791 0.238 0.204 ! 0.65 eA-3 Q142 0.936 0.277 0.871 ! 0.64 eA-3 Q143 0.491 0.621 0.379 ! 0.64 eA-3 Q144 0.091 0.307 0.156 ! 0.63 eA-3 Q145 0.173 0.150 0.718 ! 0.62 eA-3 Q146 0.064 0.309 0.080 ! 0.61 eA-3 Q147 0.860 0.829 0.413 ! 0.60 eA-3 Q148 0.356 0.686 0.069 ! 0.59 eA-3 Q149 0.811 0.565 0.807 ! 0.59 eA-3 Q150 0.486 0.791 0.700 ! 0.58 eA-3 Q151 0.949 0.698 0.971 ! 0.57 eA-3 Q152 0.106 0.842 0.107 ! 0.57 eA-3 Q153 0.811 0.040 0.511 ! 0.56 eA-3 Q154 0.730 0.376 0.609 ! 0.53 eA-3 Q155 0.688 0.569 0.338 ! 0.52 eA-3 Q156 0.154 0.909 0.055 ! 0.51 eA-3 Q157 0.297 0.738 0.324 ! 0.50 eA-3 ) ; _shelx_fab_checksum 38088