data_jcm11921a_0m _audit_creation_date 2022-03-13 _audit_creation_method ; Olex2 1.5 (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396) ; _shelx_SHELXL_version_number '2014/7' _audit_contact_author_address . _audit_contact_author_email 'marina.perez-jimenez@imperial.ac.uk' _audit_contact_author_name 'Marina Perez-Jimenez' _audit_contact_author_phone . _publ_contact_author_id_orcid '0000-0001-7891-4273' _publ_section_references ; D. Kratzert, I. Krossing, (2018), J. Appl. Cryst. 51, 928-934. Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C39 H48 Al F15 Fe O2 P4, 2.5(C6 H6)' _chemical_formula_sum 'C54 H63 Al F15 Fe O2 P4' _chemical_formula_weight 1235.75 _chemical_melting_point 'not measured' 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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.580(2) _cell_length_b 12.520(2) _cell_length_c 21.393(4) _cell_angle_alpha 73.425(4) _cell_angle_beta 86.006(5) _cell_angle_gamma 73.472(4) _cell_volume 2849.6(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5210 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 26.142 _cell_measurement_theta_min 2.261 _shelx_estimated_absorpt_T_max 0.986 _shelx_estimated_absorpt_T_min 0.963 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_correction_T_min 0.6352 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0863 before and 0.0779 after correction. The Ratio of minimum to maximum transmission is 0.8523. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details . _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_meas . _exptl_crystal_density_method . _exptl_crystal_description Block _exptl_crystal_F_000 1274 _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_transmission_factor_max . _exptl_transmission_factor_min . _diffrn_reflns_av_R_equivalents 0.2019 _diffrn_reflns_av_unetI/netI 0.1012 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 90185 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.790 _diffrn_reflns_theta_min 1.987 _diffrn_ambient_temperature 193.00 _diffrn_detector_area_resol_mean . _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6431 _reflns_number_total 10897 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution ? _refine_diff_density_max 1.125 _refine_diff_density_min -0.717 _refine_diff_density_rms 0.130 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 702 _refine_ls_number_reflns 10897 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1675 _refine_ls_R_factor_gt 0.1065 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0996P)^2^+34.2450P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2779 _refine_ls_wR_factor_ref 0.3129 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C17-C18 1.5 with sigma of 0.02 3. Rigid bond restraints C17, C18 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints C17 \\sim C18: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C9(H9A,H9B), C11(H11A,H11B), C7(H7A,H7B), C5(H5A, H5B), C15(H15A,H15B), C3(H3A,H3B), C4(H4A,H4B), C17(H17A,H17B), C19(H19A,H19B), C13(H13A,H13B) 5.b Aromatic/amide H refined with riding coordinates: C44(H44), C43(H43), C42(H42), C41(H41), C45(H45), C40(H40), C53(H53), C54(H54), C52(H52), C49(H49), C50(H50), C51(H51), C46(H46), C47(H47), C48(H48) 5.c Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C14(H14A,H14B, H14C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? 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 0.77991(11) 0.55699(11) 0.30598(6) 0.0313(3) Uani 1 1 d . . . . . P1 P 0.9102(2) 0.4106(2) 0.27123(12) 0.0366(6) Uani 1 1 d . . . . . P2 P 0.7726(2) 0.6627(2) 0.19900(12) 0.0356(6) Uani 1 1 d . . . . . P3 P 0.6656(2) 0.7032(2) 0.34644(12) 0.0363(6) Uani 1 1 d . . . . . P4 P 0.7643(3) 0.4444(2) 0.40734(12) 0.0437(7) Uani 1 1 d . . . . . Al1 Al 0.4976(2) 0.5017(2) 0.27277(12) 0.0288(6) Uani 1 1 d . . . . . O1 O 0.6310(5) 0.5160(5) 0.2905(3) 0.0319(13) Uani 1 1 d . . . . . F1 F 0.2598(5) 0.4691(5) 0.3755(3) 0.0538(15) Uani 1 1 d . . . . . F2 F 0.2215(6) 0.2792(6) 0.4563(3) 0.0602(17) Uani 1 1 d . . . . . F5 F 0.6221(5) 0.2384(5) 0.3093(3) 0.0489(14) Uani 1 1 d . . . . . F4 F 0.5824(6) 0.0526(5) 0.3928(3) 0.0636(18) Uani 1 1 d . . . . . F3 F 0.3782(6) 0.0696(6) 0.4665(3) 0.072(2) Uani 1 1 d . . . . . F8 F 0.0904(7) 0.9683(7) 0.2359(6) 0.126(4) Uani 1 1 d . . . . . F9 F 0.1930(7) 0.9003(6) 0.1308(5) 0.097(3) Uani 1 1 d . . . . . F10 F 0.3573(5) 0.6995(6) 0.1444(3) 0.0571(16) Uani 1 1 d . . . . . F7 F 0.1718(7) 0.8325(8) 0.3582(5) 0.097(3) Uani 1 1 d . . . . . F6 F 0.3501(5) 0.6369(6) 0.3733(3) 0.0537(15) Uani 1 1 d . . . . . F14 F 0.6092(5) 0.3924(5) 0.0407(3) 0.0516(15) Uani 1 1 d . . . . . F12 F 0.2219(6) 0.3947(7) 0.1242(3) 0.0657(19) Uani 1 1 d . . . . . F11 F 0.2733(5) 0.4568(6) 0.2257(3) 0.0575(17) Uani 1 1 d . . . . . F13 F 0.3861(6) 0.3643(6) 0.0301(3) 0.0604(17) Uani 1 1 d . . . . . F15 F 0.6630(5) 0.4504(5) 0.1427(3) 0.0454(14) Uani 1 1 d . . . . . O2 O 0.9920(7) 0.6079(7) 0.3390(5) 0.067(2) Uani 1 1 d . . . . . C44 C 0.407(3) 0.0873(18) 0.1557(16) 0.160(11) Uani 1 1 d . . . . . H44 H 0.3273 0.0830 0.1665 0.192 Uiso 1 1 calc R U . . . C43 C 0.468(4) 0.063(3) 0.1003(16) 0.19(2) Uani 1 1 d . . . . . H43 H 0.4255 0.0385 0.0733 0.231 Uiso 1 1 calc R U . . . C42 C 0.578(4) 0.071(3) 0.0804(19) 0.18(2) Uani 1 1 d . . . . . H42 H 0.6096 0.0545 0.0409 0.220 Uiso 1 1 calc R U . . . C41 C 0.648(3) 0.1043(17) 0.1218(14) 0.147(10) Uani 1 1 d . . . . . H41 H 0.7278 0.1090 0.1109 0.177 Uiso 1 1 calc R U . . . C45 C 0.486(3) 0.1211(17) 0.1960(11) 0.139(10) Uani 1 1 d . . . . . H45 H 0.4563 0.1372 0.2359 0.167 Uiso 1 1 calc R U . . . C40 C 0.595(3) 0.1286(16) 0.1763(13) 0.134(9) Uani 1 1 d . . . . . H40 H 0.6398 0.1529 0.2026 0.160 Uiso 1 1 calc R U . . . C1 C 0.9729(9) 0.4790(9) 0.1946(5) 0.047(2) Uani 1 1 d . . . . . H1A H 1.0315 0.5172 0.2034 0.057 Uiso 1 1 calc R U . . . H1B H 1.0154 0.4196 0.1726 0.057 Uiso 1 1 calc R U . . . C2 C 0.8684(9) 0.5709(9) 0.1498(5) 0.044(2) Uani 1 1 d . . . . . H2A H 0.8198 0.5314 0.1329 0.053 Uiso 1 1 calc R U . . . H2B H 0.9020 0.6195 0.1122 0.053 Uiso 1 1 calc R U . . . C9 C 0.8240(11) 0.7949(10) 0.1728(6) 0.053(3) Uani 1 1 d . . . . . H9A H 0.8040 0.8311 0.1258 0.064 Uiso 1 1 calc R U . . . H9B H 0.7770 0.8500 0.1966 0.064 Uiso 1 1 calc R U . . . C10 C 0.9539(11) 0.7812(12) 0.1820(7) 0.072(4) Uani 1 1 d . . . . . H10A H 0.9699 0.7721 0.2279 0.108 Uiso 1 1 calc R U . . . H10B H 0.9754 0.8499 0.1547 0.108 Uiso 1 1 calc R U . . . H10C H 1.0022 0.7123 0.1697 0.108 Uiso 1 1 calc R U . . . C11 C 0.6263(8) 0.7147(9) 0.1579(5) 0.042(2) Uani 1 1 d . . . . . H11A H 0.5846 0.6531 0.1729 0.050 Uiso 1 1 calc R U . . . H11B H 0.5781 0.7825 0.1722 0.050 Uiso 1 1 calc R U . . . C12 C 0.6266(10) 0.7503(10) 0.0825(5) 0.053(3) Uani 1 1 d . . . . . H12A H 0.6662 0.8123 0.0665 0.079 Uiso 1 1 calc R U . . . H12B H 0.5434 0.7779 0.0660 0.079 Uiso 1 1 calc R U . . . H12C H 0.6702 0.6831 0.0673 0.079 Uiso 1 1 calc R U . . . C7 C 0.8500(9) 0.3002(9) 0.2559(5) 0.041(2) Uani 1 1 d . . . . . H7A H 0.8639 0.2339 0.2957 0.049 Uiso 1 1 calc R U . . . H7B H 0.7618 0.3330 0.2496 0.049 Uiso 1 1 calc R U . . . C8 C 0.9007(10) 0.2522(10) 0.1970(6) 0.054(3) Uani 1 1 d . . . . . H8A H 0.8841 0.3156 0.1566 0.081 Uiso 1 1 calc R U . . . H8B H 0.8619 0.1932 0.1947 0.081 Uiso 1 1 calc R U . . . H8C H 0.9878 0.2173 0.2027 0.081 Uiso 1 1 calc R U . . . C5 C 1.0463(9) 0.3290(9) 0.3199(6) 0.051(3) Uani 1 1 d . . . . . H5A H 1.0864 0.3853 0.3262 0.061 Uiso 1 1 calc R U . . . H5B H 1.0217 0.2888 0.3634 0.061 Uiso 1 1 calc R U . . . C6 C 1.1388(9) 0.2400(10) 0.2941(6) 0.053(3) Uani 1 1 d . . . . . H6A H 1.1040 0.1782 0.2922 0.080 Uiso 1 1 calc R U . . . H6B H 1.2096 0.2069 0.3232 0.080 Uiso 1 1 calc R U . . . H6C H 1.1627 0.2771 0.2503 0.080 Uiso 1 1 calc R U . . . C15 C 0.5386(9) 0.8140(8) 0.2984(5) 0.040(2) Uani 1 1 d . . . . . H15A H 0.5719 0.8635 0.2611 0.048 Uiso 1 1 calc R U . . . H15B H 0.4925 0.7741 0.2802 0.048 Uiso 1 1 calc R U . . . C16 C 0.4509(10) 0.8926(9) 0.3334(5) 0.049(3) Uani 1 1 d . . . . . H16A H 0.4157 0.8455 0.3702 0.074 Uiso 1 1 calc R U . . . H16B H 0.3867 0.9464 0.3031 0.074 Uiso 1 1 calc R U . . . H16C H 0.4937 0.9368 0.3496 0.074 Uiso 1 1 calc R U . . . C3 C 0.5998(12) 0.6395(9) 0.4244(5) 0.055(3) Uani 1 1 d . . . . . H3A H 0.6386 0.6519 0.4605 0.066 Uiso 1 1 calc R U . . . H3B H 0.5129 0.6804 0.4241 0.066 Uiso 1 1 calc R U . . . C4 C 0.6146(11) 0.5106(9) 0.4370(5) 0.057(3) Uani 1 1 d . . . . . H4A H 0.5505 0.4984 0.4139 0.068 Uiso 1 1 calc R U . . . H4B H 0.6085 0.4743 0.4843 0.068 Uiso 1 1 calc R U . . . C17 C 0.868(2) 0.4419(12) 0.4674(8) 0.137(9) Uani 1 1 d D U . . . H17A H 0.9349 0.4664 0.4420 0.165 Uiso 1 1 calc R U . . . H17B H 0.8252 0.5060 0.4863 0.165 Uiso 1 1 calc R U . . . C18 C 0.920(2) 0.3536(13) 0.5186(11) 0.175(12) Uani 1 1 d D U . . . H18A H 0.9615 0.2856 0.5035 0.263 Uiso 1 1 calc R U . . . H18B H 0.8586 0.3345 0.5502 0.263 Uiso 1 1 calc R U . . . H18C H 0.9787 0.3763 0.5393 0.263 Uiso 1 1 calc R U . . . C19 C 0.7615(11) 0.2950(9) 0.4183(5) 0.051(3) Uani 1 1 d . . . . . H19A H 0.7283 0.2909 0.3779 0.062 Uiso 1 1 calc R U . . . H19B H 0.8456 0.2452 0.4234 0.062 Uiso 1 1 calc R U . . . C20 C 0.6895(10) 0.2445(9) 0.4756(5) 0.048(3) Uani 1 1 d . . . . . H20A H 0.7197 0.2497 0.5161 0.073 Uiso 1 1 calc R U . . . H20B H 0.6983 0.1630 0.4785 0.073 Uiso 1 1 calc R U . . . H20C H 0.6043 0.2881 0.4693 0.073 Uiso 1 1 calc R U . . . C13 C 0.7418(9) 0.7903(9) 0.3760(5) 0.046(3) Uani 1 1 d . . . . . H13A H 0.6843 0.8327 0.4030 0.055 Uiso 1 1 calc R U . . . H13B H 0.8096 0.7365 0.4049 0.055 Uiso 1 1 calc R U . . . C14 C 0.7906(11) 0.8772(10) 0.3248(6) 0.060(3) Uani 1 1 d . . . . . H14A H 0.8455 0.8375 0.2964 0.090 Uiso 1 1 calc R U . . . H14B H 0.8343 0.9139 0.3462 0.090 Uiso 1 1 calc R U . . . H14C H 0.7237 0.9366 0.2987 0.090 Uiso 1 1 calc R U . . . C22 C 0.4474(8) 0.3681(8) 0.3399(4) 0.035(2) Uani 1 1 d . . . . . C27 C 0.3463(9) 0.3691(9) 0.3785(5) 0.040(2) Uani 1 1 d . . . . . C26 C 0.3216(9) 0.2715(10) 0.4203(5) 0.044(2) Uani 1 1 d . . . . . C25 C 0.4023(10) 0.1635(9) 0.4257(5) 0.047(3) Uani 1 1 d . . . . . C24 C 0.5029(9) 0.1558(8) 0.3877(5) 0.043(2) Uani 1 1 d . . . . . C23 C 0.5196(9) 0.2562(9) 0.3464(5) 0.039(2) Uani 1 1 d . . . . . C34 C 0.3601(8) 0.6530(8) 0.2606(5) 0.037(2) Uani 1 1 d . . . . . C35 C 0.3082(9) 0.6944(9) 0.3122(6) 0.049(3) Uani 1 1 d . . . . . C36 C 0.2160(10) 0.7971(11) 0.3048(9) 0.071(4) Uani 1 1 d . . . . . C37 C 0.1783(11) 0.8649(11) 0.2461(9) 0.068(4) Uani 1 1 d . . . . . C38 C 0.2276(11) 0.8327(10) 0.1922(8) 0.072(4) Uani 1 1 d . . . . . C39 C 0.3151(9) 0.7278(9) 0.2002(6) 0.048(3) Uani 1 1 d . . . . . C28 C 0.4740(8) 0.4543(8) 0.1912(4) 0.035(2) Uani 1 1 d . . . . . C29 C 0.5514(7) 0.4363(8) 0.1417(4) 0.0312(19) Uani 1 1 d . . . . . C30 C 0.5263(8) 0.4080(8) 0.0874(4) 0.036(2) Uani 1 1 d . . . . . C31 C 0.4150(9) 0.3938(9) 0.0816(4) 0.042(2) Uani 1 1 d . . . . . C32 C 0.3300(9) 0.4104(9) 0.1290(5) 0.044(2) Uani 1 1 d . . . . . C33 C 0.3616(8) 0.4399(9) 0.1820(5) 0.041(2) Uani 1 1 d . . . . . C21 C 0.9071(9) 0.5890(9) 0.3237(5) 0.045(2) Uani 1 1 d . . . . . C53 C 0.0040(11) 1.0046(11) 0.5643(7) 0.067(3) Uani 1 1 d . . . . . H53 H 0.0051 1.0083 0.6080 0.080 Uiso 1 1 calc R U . . . C54 C -0.0834(12) 0.9675(12) 0.5425(7) 0.070(4) Uani 1 1 d . . . . . H54 H -0.1416 0.9436 0.5726 0.084 Uiso 1 1 calc R U . . . C52 C 0.0899(11) 1.0362(10) 0.5200(7) 0.065(3) Uani 1 1 d . . . . . H52 H 0.1527 1.0603 0.5333 0.078 Uiso 1 1 calc R U . . . C49 C 0.957(2) 0.173(2) -0.0100(13) 0.141(9) Uani 1 1 d . . . . . H49 H 0.9344 0.1138 -0.0220 0.169 Uiso 1 1 calc R U . . . C50 C 0.8725(18) 0.283(2) -0.0156(9) 0.110(6) Uani 1 1 d . . . . . H50 H 0.7944 0.3011 -0.0337 0.132 Uiso 1 1 calc R U . . . C51 C 0.9070(15) 0.3609(16) 0.0057(7) 0.086(4) Uani 1 1 d . . . . . H51 H 0.8502 0.4337 0.0032 0.103 Uiso 1 1 calc R U . . . C46 C 1.0216(18) 0.3405(18) 0.0311(9) 0.101(5) Uani 1 1 d . . . . . H46 H 1.0442 0.3995 0.0428 0.121 Uiso 1 1 calc R U . . . C47 C 1.0959(19) 0.239(3) 0.0381(8) 0.119(7) Uani 1 1 d . . . . . H47 H 1.1695 0.2214 0.0608 0.143 Uiso 1 1 calc R U . . . C48 C 1.074(3) 0.1531(19) 0.0137(13) 0.143(9) Uani 1 1 d . . . . . H48 H 1.1353 0.0845 0.0133 0.172 Uiso 1 1 calc R U . . . 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 0.0289(7) 0.0329(7) 0.0324(7) -0.0113(5) -0.0076(5) -0.0051(5) P1 0.0271(12) 0.0402(14) 0.0430(14) -0.0161(11) -0.0051(10) -0.0041(10) P2 0.0315(12) 0.0400(13) 0.0363(13) -0.0085(11) -0.0005(10) -0.0129(10) P3 0.0418(14) 0.0322(12) 0.0358(13) -0.0135(10) -0.0067(11) -0.0061(10) P4 0.0657(18) 0.0314(13) 0.0308(13) -0.0084(10) -0.0188(12) -0.0043(12) Al1 0.0272(13) 0.0326(14) 0.0283(13) -0.0114(11) 0.0017(10) -0.0084(11) O1 0.031(3) 0.039(3) 0.028(3) -0.011(3) -0.002(2) -0.010(3) F1 0.044(3) 0.053(4) 0.063(4) -0.016(3) 0.014(3) -0.013(3) F2 0.054(4) 0.091(5) 0.042(3) -0.009(3) 0.015(3) -0.041(4) F5 0.047(3) 0.044(3) 0.057(4) -0.022(3) 0.014(3) -0.010(3) F4 0.068(4) 0.039(3) 0.083(5) -0.012(3) -0.002(4) -0.018(3) F3 0.074(5) 0.066(4) 0.065(4) 0.020(3) -0.007(4) -0.041(4) F8 0.061(5) 0.070(5) 0.242(13) -0.072(7) -0.033(6) 0.025(4) F9 0.088(6) 0.048(4) 0.130(7) 0.016(4) -0.060(5) -0.005(4) F10 0.048(4) 0.063(4) 0.049(4) -0.001(3) -0.007(3) -0.010(3) F7 0.061(5) 0.103(6) 0.149(8) -0.094(6) 0.026(5) -0.004(4) F6 0.053(4) 0.066(4) 0.051(4) -0.032(3) 0.012(3) -0.018(3) F14 0.053(4) 0.071(4) 0.034(3) -0.019(3) 0.011(3) -0.018(3) F12 0.048(4) 0.105(6) 0.061(4) -0.034(4) -0.003(3) -0.036(4) F11 0.030(3) 0.102(5) 0.053(4) -0.041(4) 0.013(3) -0.021(3) F13 0.074(4) 0.078(5) 0.041(3) -0.027(3) -0.010(3) -0.028(4) F15 0.031(3) 0.075(4) 0.040(3) -0.024(3) 0.007(2) -0.023(3) O2 0.043(4) 0.066(5) 0.105(7) -0.038(5) -0.030(4) -0.012(4) C44 0.21(3) 0.070(13) 0.16(3) 0.023(14) -0.06(2) -0.028(16) C43 0.35(6) 0.086(16) 0.10(2) -0.036(16) -0.10(3) 0.03(3) C42 0.27(5) 0.084(17) 0.13(3) -0.032(17) -0.06(3) 0.06(3) C41 0.22(3) 0.075(13) 0.109(18) -0.022(12) -0.032(19) 0.023(15) C45 0.25(3) 0.069(12) 0.093(15) 0.005(10) 0.00(2) -0.059(18) C40 0.21(3) 0.055(11) 0.11(2) 0.015(12) -0.053(19) -0.026(15) C1 0.029(5) 0.053(6) 0.057(7) -0.015(5) -0.007(4) -0.005(4) C2 0.035(5) 0.051(6) 0.041(6) -0.008(5) 0.000(4) -0.005(4) C9 0.068(8) 0.051(6) 0.050(6) -0.009(5) 0.008(5) -0.037(6) C10 0.058(8) 0.085(9) 0.085(10) -0.019(8) 0.004(7) -0.044(7) C11 0.033(5) 0.046(6) 0.039(5) -0.003(4) -0.006(4) -0.008(4) C12 0.058(7) 0.069(7) 0.030(5) -0.006(5) -0.005(5) -0.023(6) C7 0.037(5) 0.050(6) 0.045(6) -0.023(5) -0.003(4) -0.014(4) C8 0.047(6) 0.064(7) 0.062(7) -0.032(6) 0.002(5) -0.016(5) C5 0.038(6) 0.050(6) 0.061(7) -0.020(5) -0.016(5) 0.002(5) C6 0.036(6) 0.053(7) 0.064(7) -0.020(6) -0.006(5) 0.003(5) C15 0.047(6) 0.034(5) 0.043(6) -0.016(4) -0.001(4) -0.011(4) C16 0.051(6) 0.040(6) 0.055(7) -0.018(5) -0.004(5) -0.005(5) C3 0.084(8) 0.043(6) 0.030(5) -0.014(5) 0.004(5) -0.003(6) C4 0.083(9) 0.050(6) 0.034(6) -0.011(5) 0.009(5) -0.014(6) C17 0.24(2) 0.058(9) 0.122(14) -0.016(8) -0.124(15) -0.036(12) C18 0.22(2) 0.062(10) 0.23(2) -0.038(11) -0.19(2) 0.024(12) C19 0.065(7) 0.042(6) 0.043(6) -0.009(5) -0.021(5) -0.006(5) C20 0.051(6) 0.043(6) 0.046(6) -0.002(5) -0.008(5) -0.014(5) C13 0.048(6) 0.044(6) 0.044(6) -0.016(5) -0.020(5) -0.001(5) C14 0.060(7) 0.062(7) 0.074(8) -0.033(6) -0.013(6) -0.025(6) C22 0.040(5) 0.042(5) 0.031(5) -0.014(4) 0.001(4) -0.018(4) C27 0.036(5) 0.053(6) 0.037(5) -0.020(5) 0.006(4) -0.016(5) C26 0.039(5) 0.064(7) 0.041(6) -0.019(5) 0.001(4) -0.031(5) C25 0.056(7) 0.046(6) 0.042(6) 0.002(5) -0.007(5) -0.030(5) C24 0.054(6) 0.030(5) 0.052(6) -0.016(4) -0.004(5) -0.019(5) C23 0.042(5) 0.051(6) 0.038(5) -0.026(5) 0.006(4) -0.023(5) C34 0.026(5) 0.043(5) 0.045(6) -0.017(4) 0.002(4) -0.012(4) C35 0.034(5) 0.045(6) 0.077(8) -0.029(6) 0.003(5) -0.012(5) C36 0.035(6) 0.058(8) 0.139(14) -0.067(9) 0.007(7) -0.004(6) C37 0.039(6) 0.042(7) 0.120(12) -0.033(8) -0.012(7) 0.005(5) C38 0.047(7) 0.030(6) 0.127(13) 0.000(7) -0.029(8) -0.007(5) C39 0.039(6) 0.039(6) 0.066(7) -0.013(5) -0.001(5) -0.013(4) C28 0.034(5) 0.037(5) 0.038(5) -0.010(4) -0.002(4) -0.014(4) C29 0.025(4) 0.035(5) 0.032(5) -0.010(4) -0.002(4) -0.005(4) C30 0.041(5) 0.041(5) 0.024(4) -0.006(4) -0.001(4) -0.008(4) C31 0.054(6) 0.051(6) 0.028(5) -0.015(4) 0.002(4) -0.022(5) C32 0.041(6) 0.064(7) 0.040(6) -0.022(5) -0.003(4) -0.026(5) C33 0.033(5) 0.052(6) 0.040(5) -0.015(5) 0.006(4) -0.014(4) C21 0.032(5) 0.039(5) 0.063(7) -0.022(5) -0.009(5) 0.001(4) C53 0.057(8) 0.059(8) 0.080(9) -0.027(7) 0.008(7) -0.003(6) C54 0.056(8) 0.069(8) 0.070(9) -0.011(7) 0.020(7) -0.009(6) C52 0.054(7) 0.054(7) 0.097(11) -0.033(7) 0.012(7) -0.021(6) C49 0.107(17) 0.13(2) 0.20(3) -0.066(18) 0.053(18) -0.050(15) C50 0.095(14) 0.150(19) 0.093(13) -0.038(13) 0.008(10) -0.042(14) C51 0.083(11) 0.106(13) 0.062(9) -0.025(9) 0.005(8) -0.014(9) C46 0.097(14) 0.109(15) 0.087(12) -0.019(11) 0.014(10) -0.024(12) C47 0.097(15) 0.17(2) 0.059(10) 0.014(13) -0.007(9) -0.033(16) C48 0.15(2) 0.082(14) 0.15(2) 0.018(14) -0.004(17) -0.006(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 P1 2.288(3) . ? Fe1 P2 2.287(3) . ? Fe1 P3 2.284(3) . ? Fe1 P4 2.251(3) . ? Fe1 O1 2.007(6) . ? Fe1 C21 1.724(10) . ? P1 C1 1.825(11) . ? P1 C7 1.828(9) . ? P1 C5 1.821(10) . ? P2 C2 1.861(10) . ? P2 C9 1.843(10) . ? P2 C11 1.822(9) . ? P3 C15 1.839(10) . ? P3 C3 1.846(11) . ? P3 C13 1.840(10) . ? P4 C4 1.850(12) . ? P4 C17 1.803(13) . ? P4 C19 1.826(11) . ? Al1 O1 1.685(6) . ? Al1 C22 2.065(10) . ? Al1 C34 2.062(10) . ? Al1 C28 2.053(9) . ? F1 C27 1.351(11) . ? F2 C26 1.341(11) . ? F5 C23 1.381(11) . ? F4 C24 1.336(11) . ? F3 C25 1.337(11) . ? F8 C37 1.371(13) . ? F9 C38 1.359(16) . ? F10 C39 1.360(13) . ? F7 C36 1.357(15) . ? F6 C35 1.346(13) . ? F14 C30 1.352(10) . ? F12 C32 1.335(11) . ? F11 C33 1.350(11) . ? F13 C31 1.347(10) . ? F15 C29 1.356(10) . ? O2 C21 1.164(11) . ? C44 H44 0.9500 . ? C44 C43 1.40(4) . ? C44 C45 1.51(3) . ? C43 H43 0.9500 . ? C43 C42 1.34(5) . ? C42 H42 0.9500 . ? C42 C41 1.46(4) . ? C41 H41 0.9500 . ? C41 C40 1.35(3) . ? C45 H45 0.9500 . ? C45 C40 1.33(3) . ? C40 H40 0.9500 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.564(13) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.485(16) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.545(13) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.556(14) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.511(14) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.520(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.520(15) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.347(15) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.522(15) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.512(16) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C22 C27 1.383(13) . ? C22 C23 1.385(14) . ? C27 C26 1.384(14) . ? C26 C25 1.387(15) . ? C25 C24 1.370(15) . ? C24 C23 1.371(14) . ? C34 C35 1.380(14) . ? C34 C39 1.395(14) . ? C35 C36 1.394(15) . ? C36 C37 1.32(2) . ? C37 C38 1.36(2) . ? C38 C39 1.385(15) . ? C28 C29 1.366(12) . ? C28 C33 1.399(12) . ? C29 C30 1.378(12) . ? C30 C31 1.369(13) . ? C31 C32 1.380(14) . ? C32 C33 1.389(13) . ? C53 H53 0.9500 . ? C53 C54 1.383(19) . ? C53 C52 1.386(17) . ? C54 H54 0.9500 . ? C54 C52 1.360(18) 2_576 ? C52 C54 1.360(18) 2_576 ? C52 H52 0.9500 . ? C49 H49 0.9500 . ? C49 C50 1.42(3) . ? C49 C48 1.41(3) . ? C50 H50 0.9500 . ? C50 C51 1.35(2) . ? C51 H51 0.9500 . ? C51 C46 1.40(2) . ? C46 H46 0.9500 . ? C46 C47 1.29(3) . ? C47 H47 0.9500 . ? C47 C48 1.41(3) . ? C48 H48 0.9500 . ? 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 P2 Fe1 P1 85.16(10) . . ? P3 Fe1 P1 174.27(10) . . ? P3 Fe1 P2 97.17(10) . . ? P4 Fe1 P1 94.57(11) . . ? P4 Fe1 P2 171.44(11) . . ? P4 Fe1 P3 83.91(10) . . ? O1 Fe1 P1 95.00(18) . . ? O1 Fe1 P2 89.07(18) . . ? O1 Fe1 P3 90.28(18) . . ? O1 Fe1 P4 82.43(19) . . ? C21 Fe1 P1 85.8(3) . . ? C21 Fe1 P2 94.0(4) . . ? C21 Fe1 P3 88.9(3) . . ? C21 Fe1 P4 94.6(4) . . ? C21 Fe1 O1 176.9(4) . . ? C1 P1 Fe1 106.7(4) . . ? C1 P1 C7 107.1(5) . . ? C7 P1 Fe1 118.0(3) . . ? C5 P1 Fe1 117.4(4) . . ? C5 P1 C1 101.5(5) . . ? C5 P1 C7 104.7(5) . . ? C2 P2 Fe1 109.5(3) . . ? C9 P2 Fe1 121.9(4) . . ? C9 P2 C2 102.2(5) . . ? C11 P2 Fe1 116.9(3) . . ? C11 P2 C2 103.5(5) . . ? C11 P2 C9 100.5(5) . . ? C15 P3 Fe1 120.3(3) . . ? C15 P3 C3 105.2(5) . . ? C3 P3 Fe1 109.0(3) . . ? C13 P3 Fe1 118.7(4) . . ? C13 P3 C15 102.6(4) . . ? C13 P3 C3 98.1(5) . . ? C4 P4 Fe1 106.2(4) . . ? C17 P4 Fe1 115.7(7) . . ? C17 P4 C4 103.7(9) . . ? C17 P4 C19 107.4(6) . . ? C19 P4 Fe1 119.1(4) . . ? C19 P4 C4 102.7(5) . . ? O1 Al1 C22 113.5(3) . . ? O1 Al1 C34 112.8(3) . . ? O1 Al1 C28 121.6(3) . . ? C34 Al1 C22 109.5(4) . . ? C28 Al1 C22 96.7(4) . . ? C28 Al1 C34 101.1(4) . . ? Al1 O1 Fe1 171.9(4) . . ? C43 C44 H44 124.6 . . ? C43 C44 C45 111(3) . . ? C45 C44 H44 124.6 . . ? C44 C43 H43 115.7 . . ? C42 C43 C44 129(4) . . ? C42 C43 H43 115.7 . . ? C43 C42 H42 121.3 . . ? C43 C42 C41 117(4) . . ? C41 C42 H42 121.3 . . ? C42 C41 H41 121.3 . . ? C40 C41 C42 117(3) . . ? C40 C41 H41 121.3 . . ? C44 C45 H45 119.6 . . ? C40 C45 C44 121(3) . . ? C40 C45 H45 119.6 . . ? C41 C40 C45 125(3) . . ? C41 C40 H40 117.5 . . ? C45 C40 H40 117.5 . . ? P1 C1 H1A 109.8 . . ? P1 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? C2 C1 P1 109.2(7) . . ? C2 C1 H1A 109.8 . . ? C2 C1 H1B 109.8 . . ? P2 C2 H2A 110.1 . . ? P2 C2 H2B 110.1 . . ? C1 C2 P2 108.2(7) . . ? C1 C2 H2A 110.1 . . ? C1 C2 H2B 110.1 . . ? H2A C2 H2B 108.4 . . ? P2 C9 H9A 108.0 . . ? P2 C9 H9B 108.0 . . ? H9A C9 H9B 107.3 . . ? C10 C9 P2 117.1(9) . . ? C10 C9 H9A 108.0 . . ? C10 C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P2 C11 H11A 108.1 . . ? P2 C11 H11B 108.1 . . ? H11A C11 H11B 107.3 . . ? C12 C11 P2 116.8(7) . . ? C12 C11 H11A 108.1 . . ? C12 C11 H11B 108.1 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P1 C7 H7A 107.9 . . ? P1 C7 H7B 107.9 . . ? H7A C7 H7B 107.2 . . ? C8 C7 P1 117.8(7) . . ? C8 C7 H7A 107.9 . . ? C8 C7 H7B 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8B 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? P1 C5 H5A 107.8 . . ? P1 C5 H5B 107.8 . . ? H5A C5 H5B 107.2 . . ? C6 C5 P1 117.9(8) . . ? C6 C5 H5A 107.8 . . ? C6 C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? P3 C15 H15A 108.0 . . ? P3 C15 H15B 108.0 . . ? H15A C15 H15B 107.2 . . ? C16 C15 P3 117.3(7) . . ? C16 C15 H15A 108.0 . . ? C16 C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P3 C3 H3A 109.0 . . ? P3 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C4 C3 P3 112.9(7) . . ? C4 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? P4 C4 H4A 110.0 . . ? P4 C4 H4B 110.0 . . ? C3 C4 P4 108.3(8) . . ? C3 C4 H4A 110.0 . . ? C3 C4 H4B 110.0 . . ? H4A C4 H4B 108.4 . . ? P4 C17 H17A 105.1 . . ? P4 C17 H17B 105.1 . . ? H17A C17 H17B 105.9 . . ? C18 C17 P4 128.8(12) . . ? C18 C17 H17A 105.1 . . ? C18 C17 H17B 105.1 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P4 C19 H19A 108.2 . . ? P4 C19 H19B 108.2 . . ? H19A C19 H19B 107.4 . . ? C20 C19 P4 116.3(8) . . ? C20 C19 H19A 108.2 . . ? C20 C19 H19B 108.2 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P3 C13 H13A 108.1 . . ? P3 C13 H13B 108.1 . . ? H13A C13 H13B 107.3 . . ? C14 C13 P3 116.8(7) . . ? C14 C13 H13A 108.1 . . ? C14 C13 H13B 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C27 C22 Al1 130.6(7) . . ? C23 C22 Al1 117.6(7) . . ? C23 C22 C27 111.6(9) . . ? F1 C27 C22 120.8(9) . . ? F1 C27 C26 114.4(8) . . ? C26 C27 C22 124.7(9) . . ? F2 C26 C27 121.4(10) . . ? F2 C26 C25 119.2(9) . . ? C25 C26 C27 119.5(9) . . ? F3 C25 C26 119.1(10) . . ? F3 C25 C24 121.9(10) . . ? C24 C25 C26 118.9(9) . . ? F4 C24 C25 119.7(9) . . ? F4 C24 C23 122.2(9) . . ? C23 C24 C25 118.1(9) . . ? F5 C23 C22 119.5(8) . . ? C24 C23 F5 113.4(9) . . ? C24 C23 C22 127.1(9) . . ? C35 C34 Al1 122.8(8) . . ? C35 C34 C39 112.9(9) . . ? C39 C34 Al1 124.3(7) . . ? F6 C35 C34 119.7(9) . . ? F6 C35 C36 116.7(11) . . ? C34 C35 C36 123.5(12) . . ? F7 C36 C35 119.6(14) . . ? C37 C36 F7 119.6(12) . . ? C37 C36 C35 120.6(13) . . ? C36 C37 F8 123.1(14) . . ? C36 C37 C38 119.8(11) . . ? C38 C37 F8 117.1(14) . . ? F9 C38 C37 121.9(12) . . ? F9 C38 C39 118.9(14) . . ? C37 C38 C39 119.1(13) . . ? F10 C39 C34 120.0(9) . . ? F10 C39 C38 116.0(11) . . ? C38 C39 C34 124.0(12) . . ? C29 C28 Al1 130.1(7) . . ? C29 C28 C33 112.3(8) . . ? C33 C28 Al1 117.5(7) . . ? F15 C29 C28 119.4(8) . . ? F15 C29 C30 114.4(8) . . ? C28 C29 C30 126.2(8) . . ? F14 C30 C29 121.7(8) . . ? F14 C30 C31 119.7(8) . . ? C31 C30 C29 118.6(8) . . ? F13 C31 C30 121.2(9) . . ? F13 C31 C32 119.0(9) . . ? C30 C31 C32 119.8(8) . . ? F12 C32 C31 120.1(8) . . ? F12 C32 C33 121.6(9) . . ? C33 C32 C31 118.2(9) . . ? F11 C33 C28 120.2(8) . . ? F11 C33 C32 114.9(8) . . ? C32 C33 C28 124.9(9) . . ? O2 C21 Fe1 176.5(11) . . ? C54 C53 H53 121.2 . . ? C54 C53 C52 117.6(13) . . ? C52 C53 H53 121.2 . . ? C53 C54 H54 118.5 . . ? C52 C54 C53 123.0(12) 2_576 . ? C52 C54 H54 118.5 2_576 . ? C53 C52 H52 120.3 . . ? C54 C52 C53 119.4(12) 2_576 . ? C54 C52 H52 120.3 2_576 . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C48 C49 C50 118(2) . . ? C49 C50 H50 121.0 . . ? C51 C50 C49 118(2) . . ? C51 C50 H50 121.0 . . ? C50 C51 H51 118.2 . . ? C50 C51 C46 123.6(18) . . ? C46 C51 H51 118.2 . . ? C51 C46 H46 121.0 . . ? C47 C46 C51 118(2) . . ? C47 C46 H46 121.0 . . ? C46 C47 H47 118.2 . . ? C46 C47 C48 124(2) . . ? C48 C47 H47 118.2 . . ? C49 C48 H48 121.2 . . ? C47 C48 C49 118(2) . . ? C47 C48 H48 121.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Fe1 P1 C1 C2 -46.9(8) . . . . ? Fe1 P1 C7 C8 142.4(7) . . . . ? Fe1 P1 C5 C6 -174.2(7) . . . . ? Fe1 P2 C2 C1 -29.2(8) . . . . ? Fe1 P2 C9 C10 64.4(11) . . . . ? Fe1 P2 C11 C12 -160.9(7) . . . . ? Fe1 P3 C15 C16 167.2(6) . . . . ? Fe1 P3 C3 C4 -11.3(10) . . . . ? Fe1 P3 C13 C14 74.2(9) . . . . ? Fe1 P4 C4 C3 -48.7(8) . . . . ? Fe1 P4 C17 C18 -146(2) . . . . ? Fe1 P4 C19 C20 -149.3(6) . . . . ? P1 C1 C2 P2 48.2(9) . . . . ? P3 C3 C4 P4 37.6(11) . . . . ? Al1 C22 C27 F1 0.4(14) . . . . ? Al1 C22 C27 C26 177.7(7) . . . . ? Al1 C22 C23 F5 1.2(11) . . . . ? Al1 C22 C23 C24 180.0(8) . . . . ? Al1 C34 C35 F6 2.1(13) . . . . ? Al1 C34 C35 C36 179.4(8) . . . . ? Al1 C34 C39 F10 3.8(13) . . . . ? Al1 C34 C39 C38 -176.1(8) . . . . ? Al1 C28 C29 F15 -0.2(13) . . . . ? Al1 C28 C29 C30 -177.8(7) . . . . ? Al1 C28 C33 F11 -0.1(13) . . . . ? Al1 C28 C33 C32 178.7(8) . . . . ? F1 C27 C26 F2 -2.6(13) . . . . ? F1 C27 C26 C25 178.0(8) . . . . ? F2 C26 C25 F3 0.3(14) . . . . ? F2 C26 C25 C24 178.5(8) . . . . ? F4 C24 C23 F5 2.9(13) . . . . ? F4 C24 C23 C22 -175.9(9) . . . . ? F3 C25 C24 F4 -2.6(15) . . . . ? F3 C25 C24 C23 178.8(9) . . . . ? F8 C37 C38 F9 0.8(18) . . . . ? F8 C37 C38 C39 -178.8(10) . . . . ? F9 C38 C39 F10 -1.8(15) . . . . ? F9 C38 C39 C34 178.0(9) . . . . ? F7 C36 C37 F8 -3.7(19) . . . . ? F7 C36 C37 C38 176.2(11) . . . . ? F6 C35 C36 F7 -1.3(15) . . . . ? F6 C35 C36 C37 173.0(11) . . . . ? F14 C30 C31 F13 0.1(15) . . . . ? F14 C30 C31 C32 -179.6(9) . . . . ? F12 C32 C33 F11 -3.2(15) . . . . ? F12 C32 C33 C28 178.0(10) . . . . ? F13 C31 C32 F12 1.5(16) . . . . ? F13 C31 C32 C33 179.5(9) . . . . ? F15 C29 C30 F14 2.0(13) . . . . ? F15 C29 C30 C31 -179.0(8) . . . . ? C44 C43 C42 C41 2(6) . . . . ? C44 C45 C40 C41 -2(3) . . . . ? C43 C44 C45 C40 2(3) . . . . ? C43 C42 C41 C40 -2(4) . . . . ? C42 C41 C40 C45 2(3) . . . . ? C45 C44 C43 C42 -2(5) . . . . ? C1 P1 C7 C8 22.3(9) . . . . ? C1 P1 C5 C6 -58.5(10) . . . . ? C2 P2 C9 C10 -58.1(10) . . . . ? C2 P2 C11 C12 -40.4(9) . . . . ? C9 P2 C2 C1 101.4(8) . . . . ? C9 P2 C11 C12 65.0(9) . . . . ? C11 P2 C2 C1 -154.5(7) . . . . ? C11 P2 C9 C10 -164.6(10) . . . . ? C7 P1 C1 C2 80.3(8) . . . . ? C7 P1 C5 C6 52.8(10) . . . . ? C5 P1 C1 C2 -170.3(7) . . . . ? C5 P1 C7 C8 -84.9(9) . . . . ? C15 P3 C3 C4 119.0(9) . . . . ? C15 P3 C13 C14 -61.2(9) . . . . ? C3 P3 C15 C16 43.9(9) . . . . ? C3 P3 C13 C14 -168.8(9) . . . . ? C4 P4 C17 C18 98(3) . . . . ? C4 P4 C19 C20 -32.3(9) . . . . ? C17 P4 C4 C3 73.8(9) . . . . ? C17 P4 C19 C20 76.7(12) . . . . ? C19 P4 C4 C3 -174.5(7) . . . . ? C19 P4 C17 C18 -10(3) . . . . ? C13 P3 C15 C16 -58.2(9) . . . . ? C13 P3 C3 C4 -135.5(9) . . . . ? C22 C27 C26 F2 179.9(8) . . . . ? C22 C27 C26 C25 0.6(15) . . . . ? C27 C22 C23 F5 177.3(8) . . . . ? C27 C22 C23 C24 -3.9(14) . . . . ? C27 C26 C25 F3 179.7(9) . . . . ? C27 C26 C25 C24 -2.1(15) . . . . ? C26 C25 C24 F4 179.3(9) . . . . ? C26 C25 C24 C23 0.7(14) . . . . ? C25 C24 C23 F5 -178.6(8) . . . . ? C25 C24 C23 C22 2.6(15) . . . . ? C23 C22 C27 F1 -175.0(8) . . . . ? C23 C22 C27 C26 2.3(13) . . . . ? C34 C35 C36 F7 -178.7(10) . . . . ? C34 C35 C36 C37 -4.3(18) . . . . ? C35 C34 C39 F10 179.9(8) . . . . ? C35 C34 C39 C38 0.0(14) . . . . ? C35 C36 C37 F8 -178.1(11) . . . . ? C35 C36 C37 C38 1.8(19) . . . . ? C36 C37 C38 F9 -179.1(11) . . . . ? C36 C37 C38 C39 1.3(19) . . . . ? C37 C38 C39 F10 177.8(10) . . . . ? C37 C38 C39 C34 -2.3(17) . . . . ? C39 C34 C35 F6 -174.1(8) . . . . ? C39 C34 C35 C36 3.2(14) . . . . ? C28 C29 C30 F14 179.7(9) . . . . ? C28 C29 C30 C31 -1.4(15) . . . . ? C29 C28 C33 F11 -178.7(9) . . . . ? C29 C28 C33 C32 0.1(15) . . . . ? C29 C30 C31 F13 -178.9(9) . . . . ? C29 C30 C31 C32 1.4(15) . . . . ? C30 C31 C32 F12 -178.8(9) . . . . ? C30 C31 C32 C33 -0.8(16) . . . . ? C31 C32 C33 F11 178.9(9) . . . . ? C31 C32 C33 C28 0.1(17) . . . . ? C33 C28 C29 F15 178.1(8) . . . . ? C33 C28 C29 C30 0.6(14) . . . . ? C54 C53 C52 C54 2(2) . . . 2_576 ? C52 C53 C54 C52 -2(2) . . . 2_576 ? C49 C50 C51 C46 2(3) . . . . ? C50 C49 C48 C47 8(3) . . . . ? C50 C51 C46 C47 -4(3) . . . . ? C51 C46 C47 C48 9(3) . . . . ? C46 C47 C48 C49 -11(3) . . . . ? C48 C49 C50 C51 -4(3) . . . . ? _shelx_res_file ; jcm11921a_0m.res created by SHELXL-2014/7 TITL jcm11921a_0m_a.res in P-1 CELL 0.71073 11.5797 12.5201 21.393 73.425 86.006 73.472 ZERR 2 0.0022 0.0021 0.0039 0.004 0.005 0.004 LATT 1 SFAC C H Al F Fe O P UNIT 108 126 2 30 2 4 8 SIMU C17 C18 DELU C17 C18 DFIX 1.5 C17 C18 L.S. 20 PLAN 20 0 0 SIZE 0.03 0.04 0.08 TEMP -80.15 CONF HTAB BOND $H MORE -1 fmap 2 acta OMIT 1 -2 5 OMIT 5 2 2 OMIT -1 2 9 OMIT -2 -2 2 OMIT -3 -2 9 REM REM REM WGHT 0.099600 34.245003 FVAR 0.41385 FE1 5 0.779912 0.556986 0.305980 11.00000 0.02893 0.03291 = 0.03239 -0.01130 -0.00758 -0.00510 P1 7 0.910220 0.410643 0.271226 11.00000 0.02709 0.04020 = 0.04297 -0.01613 -0.00510 -0.00411 P2 7 0.772635 0.662658 0.198999 11.00000 0.03149 0.03998 = 0.03625 -0.00853 -0.00050 -0.01294 P3 7 0.665629 0.703185 0.346442 11.00000 0.04178 0.03224 = 0.03577 -0.01345 -0.00666 -0.00609 P4 7 0.764261 0.444368 0.407338 11.00000 0.06570 0.03138 = 0.03078 -0.00839 -0.01878 -0.00432 AL1 3 0.497591 0.501678 0.272774 11.00000 0.02717 0.03258 = 0.02834 -0.01138 0.00167 -0.00843 O1 6 0.630956 0.515975 0.290482 11.00000 0.03062 0.03920 = 0.02756 -0.01078 -0.00166 -0.01005 F1 4 0.259772 0.469126 0.375487 11.00000 0.04365 0.05297 = 0.06262 -0.01613 0.01375 -0.01308 F2 4 0.221537 0.279192 0.456319 11.00000 0.05389 0.09070 = 0.04150 -0.00920 0.01453 -0.04118 F5 4 0.622096 0.238438 0.309317 11.00000 0.04716 0.04416 = 0.05715 -0.02239 0.01399 -0.01034 F4 4 0.582394 0.052607 0.392802 11.00000 0.06833 0.03897 = 0.08313 -0.01231 -0.00179 -0.01829 F3 4 0.378195 0.069588 0.466488 11.00000 0.07383 0.06568 = 0.06541 0.01959 -0.00651 -0.04059 F8 4 0.090390 0.968336 0.235945 11.00000 0.06134 0.07006 = 0.24170 -0.07232 -0.03269 0.02495 F9 4 0.193008 0.900287 0.130813 11.00000 0.08789 0.04827 = 0.12993 0.01637 -0.05952 -0.00528 F10 4 0.357338 0.699461 0.144434 11.00000 0.04765 0.06290 = 0.04892 -0.00097 -0.00687 -0.00969 F7 4 0.171827 0.832456 0.358245 11.00000 0.06093 0.10281 = 0.14855 -0.09387 0.02592 -0.00362 F6 4 0.350075 0.636930 0.373284 11.00000 0.05282 0.06638 = 0.05103 -0.03150 0.01219 -0.01804 F14 4 0.609186 0.392364 0.040674 11.00000 0.05259 0.07100 = 0.03356 -0.01939 0.01105 -0.01840 F12 4 0.221920 0.394733 0.124247 11.00000 0.04826 0.10476 = 0.06118 -0.03419 -0.00280 -0.03588 F11 4 0.273318 0.456787 0.225712 11.00000 0.03038 0.10215 = 0.05267 -0.04115 0.01338 -0.02128 F13 4 0.386079 0.364286 0.030118 11.00000 0.07409 0.07847 = 0.04111 -0.02662 -0.00984 -0.02806 F15 4 0.662992 0.450354 0.142672 11.00000 0.03093 0.07458 = 0.04044 -0.02449 0.00699 -0.02256 O2 6 0.992040 0.607890 0.339016 11.00000 0.04295 0.06554 = 0.10465 -0.03755 -0.02987 -0.01191 C44 1 0.407088 0.087310 0.155721 11.00000 0.21495 0.06956 = 0.16159 0.02294 -0.05825 -0.02789 AFIX 43 H44 2 0.327261 0.082960 0.166518 11.00000 -1.20000 AFIX 0 C43 1 0.468082 0.063286 0.100335 11.00000 0.35086 0.08609 = 0.10319 -0.03589 -0.09893 0.03299 AFIX 43 H43 2 0.425511 0.038495 0.073318 11.00000 -1.20000 AFIX 0 C42 1 0.578143 0.070586 0.080434 11.00000 0.27373 0.08370 = 0.13114 -0.03225 -0.05503 0.06283 AFIX 43 H42 2 0.609631 0.054456 0.040876 11.00000 -1.20000 AFIX 0 C41 1 0.648125 0.104310 0.121836 11.00000 0.21901 0.07524 = 0.10944 -0.02162 -0.03188 0.02343 AFIX 43 H41 2 0.727812 0.108991 0.110903 11.00000 -1.20000 AFIX 0 C45 1 0.485578 0.121108 0.195991 11.00000 0.24801 0.06852 = 0.09301 0.00463 -0.00012 -0.05933 AFIX 43 H45 2 0.456261 0.137203 0.235870 11.00000 -1.20000 AFIX 0 C40 1 0.595229 0.128599 0.176278 11.00000 0.21053 0.05542 = 0.11193 0.01523 -0.05312 -0.02646 AFIX 43 H40 2 0.639753 0.152936 0.202567 11.00000 -1.20000 AFIX 0 C1 1 0.972850 0.479036 0.194648 11.00000 0.02891 0.05270 = 0.05735 -0.01541 -0.00692 -0.00514 AFIX 23 H1A 2 1.031549 0.517229 0.203439 11.00000 -1.20000 H1B 2 1.015407 0.419570 0.172555 11.00000 -1.20000 AFIX 0 C2 1 0.868434 0.570855 0.149793 11.00000 0.03481 0.05065 = 0.04064 -0.00817 0.00030 -0.00515 AFIX 23 H2A 2 0.819785 0.531430 0.132893 11.00000 -1.20000 H2B 2 0.901984 0.619539 0.112227 11.00000 -1.20000 AFIX 0 C9 1 0.824041 0.794924 0.172761 11.00000 0.06839 0.05109 = 0.04965 -0.00857 0.00757 -0.03744 AFIX 23 H9A 2 0.803987 0.831141 0.125838 11.00000 -1.20000 H9B 2 0.777037 0.849964 0.196617 11.00000 -1.20000 AFIX 0 C10 1 0.953935 0.781150 0.182045 11.00000 0.05803 0.08504 = 0.08539 -0.01875 0.00383 -0.04408 AFIX 137 H10A 2 0.969871 0.772098 0.227931 11.00000 -1.50000 H10B 2 0.975415 0.849929 0.154655 11.00000 -1.50000 H10C 2 1.002223 0.712336 0.169672 11.00000 -1.50000 AFIX 0 C11 1 0.626339 0.714701 0.157867 11.00000 0.03333 0.04605 = 0.03928 -0.00305 -0.00551 -0.00759 AFIX 23 H11A 2 0.584588 0.653143 0.172904 11.00000 -1.20000 H11B 2 0.578052 0.782459 0.172160 11.00000 -1.20000 AFIX 0 C12 1 0.626566 0.750269 0.082516 11.00000 0.05847 0.06879 = 0.03037 -0.00604 -0.00473 -0.02305 AFIX 137 H12A 2 0.666210 0.812305 0.066535 11.00000 -1.50000 H12B 2 0.543410 0.777931 0.065959 11.00000 -1.50000 H12C 2 0.670222 0.683129 0.067262 11.00000 -1.50000 AFIX 0 C7 1 0.850044 0.300236 0.255912 11.00000 0.03679 0.05021 = 0.04477 -0.02313 -0.00325 -0.01434 AFIX 23 H7A 2 0.863877 0.233935 0.295724 11.00000 -1.20000 H7B 2 0.761781 0.332978 0.249610 11.00000 -1.20000 AFIX 0 C8 1 0.900650 0.252168 0.197030 11.00000 0.04725 0.06396 = 0.06168 -0.03227 0.00172 -0.01632 AFIX 137 H8A 2 0.884087 0.315644 0.156609 11.00000 -1.50000 H8B 2 0.861902 0.193241 0.194712 11.00000 -1.50000 H8C 2 0.987833 0.217347 0.202685 11.00000 -1.50000 AFIX 0 C5 1 1.046325 0.329025 0.319891 11.00000 0.03771 0.04962 = 0.06116 -0.01976 -0.01604 0.00198 AFIX 23 H5A 2 1.086412 0.385317 0.326234 11.00000 -1.20000 H5B 2 1.021662 0.288841 0.363446 11.00000 -1.20000 AFIX 0 C6 1 1.138770 0.239981 0.294124 11.00000 0.03607 0.05315 = 0.06437 -0.02022 -0.00632 0.00279 AFIX 137 H6A 2 1.103999 0.178169 0.292209 11.00000 -1.50000 H6B 2 1.209579 0.206900 0.323150 11.00000 -1.50000 H6C 2 1.162705 0.277109 0.250298 11.00000 -1.50000 AFIX 0 C15 1 0.538597 0.813998 0.298398 11.00000 0.04654 0.03366 = 0.04345 -0.01631 -0.00103 -0.01106 AFIX 23 H15A 2 0.571902 0.863548 0.261140 11.00000 -1.20000 H15B 2 0.492472 0.774058 0.280151 11.00000 -1.20000 AFIX 0 C16 1 0.450867 0.892647 0.333443 11.00000 0.05093 0.03966 = 0.05539 -0.01796 -0.00420 -0.00489 AFIX 137 H16A 2 0.415692 0.845493 0.370212 11.00000 -1.50000 H16B 2 0.386662 0.946359 0.303084 11.00000 -1.50000 H16C 2 0.493674 0.936805 0.349632 11.00000 -1.50000 AFIX 0 C3 1 0.599753 0.639545 0.424408 11.00000 0.08405 0.04301 = 0.02961 -0.01450 0.00390 -0.00261 AFIX 23 H3A 2 0.638630 0.651945 0.460517 11.00000 -1.20000 H3B 2 0.512862 0.680367 0.424117 11.00000 -1.20000 AFIX 0 C4 1 0.614630 0.510574 0.437033 11.00000 0.08262 0.04967 = 0.03432 -0.01114 0.00865 -0.01394 AFIX 23 H4A 2 0.550483 0.498357 0.413861 11.00000 -1.20000 H4B 2 0.608480 0.474256 0.484293 11.00000 -1.20000 AFIX 0 C17 1 0.867500 0.441890 0.467391 11.00000 0.24141 0.05780 = 0.12153 -0.01557 -0.12369 -0.03554 AFIX 23 H17A 2 0.934876 0.466419 0.442004 11.00000 -1.20000 H17B 2 0.825175 0.505967 0.486253 11.00000 -1.20000 AFIX 0 C18 1 0.920160 0.353575 0.518607 11.00000 0.21932 0.06226 = 0.23127 -0.03793 -0.19468 0.02387 AFIX 137 H18A 2 0.961529 0.285624 0.503532 11.00000 -1.50000 H18B 2 0.858606 0.334496 0.550235 11.00000 -1.50000 H18C 2 0.978669 0.376330 0.539327 11.00000 -1.50000 AFIX 0 C19 1 0.761520 0.295031 0.418264 11.00000 0.06466 0.04204 = 0.04346 -0.00938 -0.02108 -0.00566 AFIX 23 H19A 2 0.728317 0.290907 0.377874 11.00000 -1.20000 H19B 2 0.845626 0.245178 0.423390 11.00000 -1.20000 AFIX 0 C20 1 0.689544 0.244455 0.475648 11.00000 0.05104 0.04349 = 0.04625 -0.00205 -0.00839 -0.01407 AFIX 137 H20A 2 0.719680 0.249651 0.516059 11.00000 -1.50000 H20B 2 0.698277 0.163005 0.478517 11.00000 -1.50000 H20C 2 0.604335 0.288147 0.469315 11.00000 -1.50000 AFIX 0 C13 1 0.741815 0.790268 0.376003 11.00000 0.04757 0.04422 = 0.04426 -0.01573 -0.02027 -0.00070 AFIX 23 H13A 2 0.684306 0.832678 0.403032 11.00000 -1.20000 H13B 2 0.809556 0.736467 0.404879 11.00000 -1.20000 AFIX 0 C14 1 0.790612 0.877206 0.324839 11.00000 0.05996 0.06247 = 0.07402 -0.03311 -0.01280 -0.02512 AFIX 137 H14A 2 0.845458 0.837455 0.296396 11.00000 -1.50000 H14B 2 0.834296 0.913905 0.346213 11.00000 -1.50000 H14C 2 0.723711 0.936605 0.298747 11.00000 -1.50000 AFIX 0 C22 1 0.447353 0.368101 0.339906 11.00000 0.04034 0.04175 = 0.03099 -0.01408 0.00132 -0.01816 C27 1 0.346278 0.369079 0.378458 11.00000 0.03618 0.05261 = 0.03714 -0.01954 0.00593 -0.01580 C26 1 0.321573 0.271495 0.420320 11.00000 0.03900 0.06443 = 0.04142 -0.01923 0.00085 -0.03070 C25 1 0.402349 0.163457 0.425734 11.00000 0.05569 0.04601 = 0.04212 0.00150 -0.00685 -0.02958 C24 1 0.502916 0.155842 0.387700 11.00000 0.05389 0.03041 = 0.05178 -0.01586 -0.00367 -0.01863 C23 1 0.519578 0.256230 0.346388 11.00000 0.04165 0.05112 = 0.03822 -0.02636 0.00578 -0.02283 C34 1 0.360122 0.653049 0.260626 11.00000 0.02628 0.04270 = 0.04523 -0.01657 0.00186 -0.01173 C35 1 0.308226 0.694408 0.312214 11.00000 0.03394 0.04519 = 0.07683 -0.02906 0.00274 -0.01201 C36 1 0.215993 0.797065 0.304843 11.00000 0.03526 0.05800 = 0.13940 -0.06704 0.00712 -0.00441 C37 1 0.178270 0.864868 0.246135 11.00000 0.03915 0.04195 = 0.11996 -0.03339 -0.01169 0.00529 C38 1 0.227606 0.832707 0.192214 11.00000 0.04726 0.03042 = 0.12725 0.00034 -0.02905 -0.00668 C39 1 0.315062 0.727849 0.200161 11.00000 0.03864 0.03895 = 0.06587 -0.01308 -0.00106 -0.01270 C28 1 0.474011 0.454346 0.191249 11.00000 0.03364 0.03667 = 0.03763 -0.00973 -0.00221 -0.01432 C29 1 0.551356 0.436286 0.141688 11.00000 0.02513 0.03509 = 0.03185 -0.00986 -0.00165 -0.00505 C30 1 0.526323 0.407996 0.087381 11.00000 0.04051 0.04055 = 0.02380 -0.00551 -0.00144 -0.00784 C31 1 0.414966 0.393772 0.081600 11.00000 0.05373 0.05146 = 0.02845 -0.01477 0.00242 -0.02183 C32 1 0.329955 0.410399 0.128976 11.00000 0.04146 0.06375 = 0.04017 -0.02215 -0.00332 -0.02578 C33 1 0.361609 0.439886 0.181955 11.00000 0.03347 0.05200 = 0.03994 -0.01534 0.00648 -0.01417 C21 1 0.907077 0.588956 0.323679 11.00000 0.03183 0.03924 = 0.06321 -0.02196 -0.00920 0.00102 C53 1 0.003967 1.004640 0.564285 11.00000 0.05729 0.05861 = 0.07970 -0.02741 0.00762 -0.00252 AFIX 43 H53 2 0.005074 1.008342 0.607972 11.00000 -1.20000 AFIX 0 C54 1 -0.083411 0.967534 0.542527 11.00000 0.05604 0.06949 = 0.07032 -0.01069 0.01996 -0.00928 AFIX 43 H54 2 -0.141566 0.943589 0.572635 11.00000 -1.20000 AFIX 0 C52 1 0.089872 1.036232 0.520026 11.00000 0.05404 0.05420 = 0.09728 -0.03277 0.01170 -0.02068 AFIX 43 H52 2 0.152705 1.060303 0.533260 11.00000 -1.20000 AFIX 0 C49 1 0.956558 0.172801 -0.010022 11.00000 0.10677 0.13254 = 0.20039 -0.06615 0.05307 -0.05014 AFIX 43 H49 2 0.934402 0.113809 -0.022027 11.00000 -1.20000 AFIX 0 C50 1 0.872511 0.282938 -0.015564 11.00000 0.09499 0.14974 = 0.09287 -0.03834 0.00763 -0.04177 AFIX 43 H50 2 0.794362 0.301051 -0.033680 11.00000 -1.20000 AFIX 0 C51 1 0.906986 0.360923 0.005651 11.00000 0.08258 0.10625 = 0.06248 -0.02513 0.00460 -0.01397 AFIX 43 H51 2 0.850203 0.433736 0.003179 11.00000 -1.20000 AFIX 0 C46 1 1.021624 0.340491 0.031063 11.00000 0.09651 0.10944 = 0.08690 -0.01868 0.01379 -0.02393 AFIX 43 H46 2 1.044160 0.399520 0.042821 11.00000 -1.20000 AFIX 0 C47 1 1.095871 0.239167 0.038071 11.00000 0.09734 0.17066 = 0.05921 0.01356 -0.00712 -0.03256 AFIX 43 H47 2 1.169532 0.221377 0.060849 11.00000 -1.20000 AFIX 0 C48 1 1.073684 0.153139 0.013729 11.00000 0.15129 0.08199 = 0.14733 0.01839 -0.00440 -0.00579 AFIX 43 H48 2 1.135348 0.084499 0.013348 11.00000 -1.20000 AFIX 0 HKLF 4 REM jcm11921a_0m_a.res in P-1 REM R1 = 0.1065 for 6431 Fo > 4sig(Fo) and 0.1675 for all 10897 data REM 702 parameters refined using 8 restraints END WGHT 0.1158 26.3690 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB C1 F12_$1 HTAB C2 F15 HTAB C10 O2 HTAB C11 O1 HTAB C11 F10 EQIV $2 -x+1, -y+1, -z HTAB C12 F13_$2 HTAB C7 F5 HTAB C7 F15 HTAB C8 F15 EQIV $3 x, y+1, z HTAB C16 F4_$3 HTAB C3 F6 HTAB C4 F6 HTAB C17 O2 EQIV $4 -x+1, -y+1, -z+1 HTAB C18 F7_$4 HTAB C19 F5 HTAB C13 F4_$3 REM Highest difference peak 1.125, deepest hole -0.717, 1-sigma level 0.130 Q1 1 0.7877 1.0592 0.3051 11.00000 0.05 1.12 Q2 1 0.9596 0.3807 0.4796 11.00000 0.05 1.05 Q3 1 0.2020 0.4166 0.2261 11.00000 0.05 1.03 Q4 1 0.1955 0.5314 0.1209 11.00000 0.05 0.73 Q5 1 0.7763 0.4750 0.3009 11.00000 0.05 0.73 Q6 1 0.6845 0.2151 0.3506 11.00000 0.05 0.66 Q7 1 0.6446 0.4187 0.5226 11.00000 0.05 0.61 Q8 1 0.8770 0.3724 0.5219 11.00000 0.05 0.61 Q9 1 0.7762 0.5778 0.1980 11.00000 0.05 0.57 Q10 1 0.8244 0.4314 0.4902 11.00000 0.05 0.56 Q11 1 0.9193 0.3775 0.1956 11.00000 0.05 0.53 Q12 1 1.0113 0.4071 0.4384 11.00000 0.05 0.53 Q13 1 0.7889 0.9474 0.4057 11.00000 0.05 0.52 Q14 1 0.7053 0.7417 0.3679 11.00000 0.05 0.50 Q15 1 0.7489 0.1352 0.2015 11.00000 0.05 0.49 Q16 1 0.3339 0.2661 0.1938 11.00000 0.05 0.48 Q17 1 0.9128 0.8969 0.2696 11.00000 0.05 0.46 Q18 1 1.2063 0.3011 0.3258 11.00000 0.05 0.46 Q19 1 0.7610 0.2394 0.5444 11.00000 0.05 0.46 Q20 1 0.5198 0.4119 0.2779 11.00000 0.05 0.46 ; _shelx_res_checksum 67025 _shelx_hkl_file ; -2 0 0 282.97 26.10 -2 0 0 274.37 26.00 -2 0 0 379.86 27.50 -2 0 0 284.67 24.40 -2 0 0 232.38 23.00 2 0 0 293.97 23.50 2 0 0 259.17 22.80 2 0 0 261.17 23.30 2 0 0 278.17 23.00 2 0 0 306.27 25.30 -3 0 0 118.19 22.70 -3 0 0 103.29 23.30 -3 0 0 101.99 19.20 -3 0 0 133.49 20.20 -3 0 0 82.69 19.90 3 0 0 116.59 24.20 3 0 0 97.69 17.80 3 0 0 97.39 21.80 3 0 0 118.59 18.60 3 0 0 143.09 21.70 -4 0 0 257.57 30.90 -4 0 0 212.88 28.40 -4 0 0 187.98 26.30 -4 0 0 228.58 30.30 -4 0 0 326.17 50.39 4 0 0 227.38 29.60 4 0 0 222.38 30.20 4 0 0 225.68 33.30 4 0 0 234.98 27.30 4 0 0 209.18 28.00 -5 0 0 791.72 62.09 -5 0 0 852.91 62.69 -5 0 0 856.51 64.39 -5 0 0 779.72 62.69 -5 0 0 908.01 62.49 5 0 0 881.11 62.59 5 0 0 919.51 65.99 5 0 0 959.10 64.89 5 0 0 969.70 66.69 5 0 0 832.52 65.69 -6 0 0 18.30 20.60 -6 0 0 62.79 22.00 -6 0 0 11.30 18.40 -6 0 0 35.10 26.60 6 0 0 60.49 24.60 6 0 0 103.09 26.80 6 0 0 61.69 22.50 6 0 0 17.50 22.60 6 0 0 28.30 25.60 -7 0 0 2563.54 160.08 -7 0 0 2630.24 161.08 -7 0 0 2614.24 160.88 -7 0 0 2639.54 158.48 7 0 0 2603.34 159.08 7 0 0 2120.39 157.98 7 0 0 2414.36 157.38 7 0 0 2431.46 158.98 7 0 0 2572.44 161.18 -8 0 0 474.95 52.89 -8 0 0 351.96 51.09 -8 0 0 514.45 52.39 -8 0 0 417.66 50.99 8 0 0 513.25 58.79 8 0 0 434.96 52.69 8 0 0 456.35 50.59 8 0 0 400.26 55.59 8 0 0 476.75 53.49 -9 0 0 460.25 56.69 -9 0 0 390.26 52.59 -9 0 0 433.56 52.69 -9 0 0 404.86 57.69 9 0 0 384.36 50.49 9 0 0 430.36 54.39 9 0 0 602.34 65.99 9 0 0 421.86 60.09 9 0 0 436.06 54.69 -10 0 0 39.00 30.70 -10 0 0 69.49 32.40 -10 0 0 12.30 27.90 -10 0 0 29.40 32.60 10 0 0 -2.20 30.60 10 0 0 0.00 31.20 10 0 0 221.58 44.70 10 0 0 11.50 32.30 10 0 0 47.70 24.10 -11 0 0 -27.40 25.80 -11 0 0 -1.50 23.60 -11 0 0 16.60 36.50 -11 0 0 36.30 35.10 11 0 0 11.30 29.80 11 0 0 56.39 39.80 11 0 0 23.20 33.60 11 0 0 24.80 26.80 11 0 0 -5.70 29.00 -12 0 0 -14.90 29.20 -12 0 0 -1.90 30.90 -12 0 0 2.50 32.60 -12 0 0 23.30 40.40 -12 0 0 -7.90 34.70 12 0 0 31.20 34.40 12 0 0 -31.20 27.00 12 0 0 -61.79 22.10 12 0 0 57.69 33.40 12 0 0 -0.80 35.90 -13 0 0 -18.60 34.50 -13 0 0 23.90 30.10 -13 0 0 32.60 43.40 -13 0 0 6.40 32.90 -13 0 0 -62.79 34.20 13 0 0 11.60 38.80 13 0 0 0.10 21.50 13 0 0 33.40 45.80 13 0 0 22.00 43.00 13 -1 0 46.70 43.70 13 -1 0 7.60 42.40 13 -1 0 31.80 50.79 13 -1 0 40.80 27.30 13 -1 0 -18.90 36.80 -13 1 0 -0.40 34.80 -13 1 0 -26.90 37.10 -13 1 0 -10.30 40.60 -13 1 0 -23.50 30.70 -13 1 0 8.50 28.00 12 -1 0 28.10 35.20 12 -1 0 3.80 23.80 12 -1 0 -31.40 32.00 12 -1 0 28.50 39.10 12 -1 0 18.90 33.10 -12 1 0 56.79 35.30 -12 1 0 -47.50 35.50 -12 1 0 2.60 23.20 -12 1 0 -27.00 28.80 11 -1 0 16.70 33.00 11 -1 0 20.10 28.40 11 -1 0 11.20 31.20 11 -1 0 11.30 33.40 11 -1 0 25.60 24.10 -11 1 0 83.79 35.50 -11 1 0 -23.00 36.70 -11 1 0 36.90 32.00 -11 1 0 -2.50 31.30 10 -1 0 104.09 38.90 10 -1 0 124.19 43.20 10 -1 0 108.79 36.60 10 -1 0 169.88 31.00 10 -1 0 124.49 40.70 -10 1 0 172.58 44.20 -10 1 0 77.19 35.70 -10 1 0 127.09 37.80 -10 1 0 99.09 35.10 9 -1 0 103.19 34.40 9 -1 0 140.89 41.30 9 -1 0 81.99 37.10 9 -1 0 74.19 35.40 -9 1 0 81.29 37.20 -9 1 0 98.29 31.40 -9 1 0 126.69 39.00 -9 1 0 75.99 32.30 8 -1 0 436.16 56.19 8 -1 0 459.95 54.89 8 -1 0 448.06 58.19 8 -1 0 473.35 52.99 -8 1 0 483.75 58.09 -8 1 0 435.46 56.89 -8 1 0 490.05 58.49 -8 1 0 448.56 49.20 -8 1 0 436.56 52.99 7 -1 0 726.23 59.29 7 -1 0 574.84 54.09 7 -1 0 638.64 57.39 7 -1 0 570.84 53.19 7 -1 0 570.14 57.29 -7 1 0 636.44 58.49 -7 1 0 633.04 53.79 -7 1 0 631.24 53.69 -7 1 0 622.04 54.59 -7 1 0 611.44 55.49 6 -1 0 200.68 37.50 6 -1 0 244.38 33.60 6 -1 0 220.58 40.90 6 -1 0 206.08 32.70 6 -1 0 217.08 33.30 -6 1 0 218.78 35.50 -6 1 0 299.17 50.29 -6 1 0 219.78 33.00 -6 1 0 245.68 35.50 -6 1 0 237.98 38.70 5 -1 0 252.07 32.10 5 -1 0 274.17 37.90 5 -1 0 240.28 34.40 5 -1 0 224.98 32.60 5 -1 0 247.58 32.90 -5 1 0 242.18 36.40 -5 1 0 287.97 36.30 -5 1 0 340.77 42.00 -5 1 0 268.47 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429.66 42.80 5 4 0 436.06 43.30 5 4 0 386.96 39.00 5 4 0 401.16 34.70 5 4 0 380.56 39.00 -6 -4 0 20.90 18.70 -6 -4 0 15.80 13.90 -6 -4 0 74.19 24.70 -6 -4 0 54.69 18.90 -6 -4 0 74.19 23.30 6 4 0 38.90 19.60 6 4 0 12.20 25.40 6 4 0 23.70 22.60 6 4 0 25.10 18.80 -7 -4 0 22.90 16.40 -7 -4 0 46.90 24.80 -7 -4 0 65.59 25.20 -7 -4 0 23.00 22.20 -7 -4 0 53.39 18.00 7 4 0 41.60 24.30 7 4 0 8.70 15.50 7 4 0 17.70 24.40 7 4 0 49.30 21.10 7 4 0 9.30 17.40 -8 -4 0 256.07 41.70 -8 -4 0 212.38 31.70 -8 -4 0 234.48 40.70 -8 -4 0 275.07 35.20 -8 -4 0 226.58 37.40 8 4 0 298.47 54.19 8 4 0 280.97 33.70 8 4 0 288.27 43.90 8 4 0 302.27 42.30 8 4 0 280.37 41.60 -9 -4 0 2.10 23.50 -9 -4 0 71.79 24.70 -9 -4 0 19.50 22.50 -9 -4 0 55.39 30.80 -9 -4 0 57.59 32.70 9 4 0 -22.10 24.90 9 4 0 39.40 31.50 9 4 0 23.20 21.70 9 4 0 24.10 31.00 9 4 0 46.70 32.60 9 4 0 31.00 29.40 -10 -4 0 3.90 26.80 -10 -4 0 8.30 32.80 -10 -4 0 -21.80 20.60 -10 -4 0 16.00 25.40 -10 -4 0 -27.30 20.80 10 4 0 -13.10 29.00 10 4 0 -15.20 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25.80 -5 5 0 41.40 26.70 -5 5 0 55.89 30.70 -5 5 0 91.89 28.30 -5 5 0 49.80 23.60 -5 5 0 41.60 17.50 4 -5 0 14.60 12.90 4 -5 0 8.50 18.30 4 -5 0 -0.20 16.90 4 -5 0 -26.30 22.40 -4 5 0 3.50 25.00 -4 5 0 5.60 12.70 -4 5 0 -13.40 22.30 -4 5 0 5.60 21.10 -4 5 0 33.80 22.70 3 -5 0 382.56 30.90 3 -5 0 450.75 49.30 3 -5 0 330.67 36.10 -3 5 0 311.47 33.70 -3 5 0 431.66 43.60 -3 5 0 419.56 46.00 -3 5 0 341.67 27.50 -3 5 0 330.47 33.90 2 -5 0 427.66 43.30 2 -5 0 440.46 37.20 2 -5 0 360.16 34.50 2 -5 0 412.66 34.10 -2 5 0 397.06 34.60 -2 5 0 426.46 33.70 -2 5 0 402.66 43.70 -2 5 0 416.26 28.20 -2 5 0 430.66 36.70 1 -5 0 1689.23 100.09 1 -5 0 1532.05 98.39 1 -5 0 1600.64 104.49 1 -5 0 1605.74 98.99 -1 5 0 1483.05 93.39 -1 5 0 1644.14 99.59 -1 5 0 1666.23 105.99 -1 5 0 1689.93 99.29 -1 5 0 1587.94 98.49 0 -5 0 37.40 19.00 0 -5 0 32.60 13.80 0 -5 0 11.70 20.80 0 -5 0 37.60 14.30 0 5 0 39.50 27.50 0 5 0 26.70 8.60 0 5 0 5.70 20.10 0 5 0 50.79 14.00 0 5 0 34.70 14.60 -1 -5 0 363.86 28.50 -1 -5 0 338.27 28.00 -1 -5 0 401.86 28.50 -1 -5 0 406.26 35.40 1 5 0 371.76 28.90 1 5 0 364.26 28.30 1 5 0 321.87 33.70 1 5 0 324.27 34.00 1 5 0 334.97 27.50 -2 -5 0 12.50 19.40 -2 -5 0 18.90 14.20 -2 -5 0 31.30 14.80 -2 -5 0 25.30 15.10 2 5 0 52.29 20.80 2 5 0 48.80 14.20 2 5 0 28.00 13.80 2 5 0 46.70 14.30 -3 -5 0 86.89 19.20 -3 -5 0 103.39 20.30 -3 -5 0 104.79 24.30 3 5 0 97.09 19.10 3 5 0 104.29 20.60 3 5 0 85.39 21.30 3 5 0 111.49 28.60 -4 -5 0 34.30 19.90 -4 -5 0 32.80 20.40 -4 -5 0 21.20 20.70 4 5 0 58.89 21.60 4 5 0 46.00 18.70 4 5 0 73.59 17.70 4 5 0 51.29 24.00 4 5 0 60.69 21.50 -5 -5 0 195.98 17.90 -5 -5 0 169.38 31.00 -5 -5 0 211.18 30.40 -5 -5 0 287.27 33.00 5 5 0 215.48 30.40 5 5 0 199.68 29.30 5 5 0 189.88 25.40 5 5 0 261.77 36.10 5 5 0 176.28 32.80 -6 -5 0 771.12 50.79 -6 -5 0 789.12 59.09 -6 -5 0 807.42 59.69 -6 -5 0 706.43 61.69 6 5 0 794.62 54.79 6 5 0 760.32 62.29 6 5 0 743.13 58.39 6 5 0 776.42 63.29 6 5 0 703.23 58.49 -7 -5 0 74.69 27.20 -7 -5 0 46.90 18.40 -7 -5 0 75.89 17.50 -7 -5 0 69.89 25.90 7 5 0 45.40 28.40 7 5 0 50.19 24.50 7 5 0 49.40 18.30 7 5 0 92.09 28.60 7 5 0 31.70 22.00 -8 -5 0 23.60 26.20 -8 -5 0 10.50 25.50 -8 -5 0 29.10 24.60 -8 -5 0 27.00 19.00 -8 -5 0 -7.60 17.00 8 5 0 5.30 16.80 8 5 0 -17.60 24.60 8 5 0 0.60 26.30 8 5 0 -9.60 24.60 8 5 0 22.30 25.30 -9 -5 0 -40.60 26.20 -9 -5 0 -20.80 30.20 -9 -5 0 -15.00 19.80 -9 -5 0 15.20 20.90 -9 -5 0 -20.90 32.80 9 5 0 1.00 24.60 9 5 0 5.80 30.50 9 5 0 11.10 31.50 9 5 0 -5.90 17.50 9 5 0 -40.40 23.40 -10 -5 0 117.59 30.50 -10 -5 0 77.39 27.60 -10 -5 0 148.19 42.10 -10 -5 0 86.39 30.40 -10 -5 0 108.29 34.20 10 5 0 107.49 28.10 10 5 0 95.29 37.50 10 5 0 104.39 36.00 10 5 0 52.39 34.80 10 5 0 66.49 33.70 10 5 0 161.78 41.50 -11 -5 0 29.40 28.80 -11 -5 0 22.30 25.40 -11 -5 0 -9.50 23.00 -11 -5 0 29.10 34.20 11 5 0 7.00 34.20 11 5 0 22.10 37.40 11 5 0 37.70 24.60 11 5 0 32.60 35.60 11 5 0 -17.90 26.80 11 5 0 4.90 28.40 -12 -5 0 -17.40 23.70 -12 -5 0 -3.00 28.30 -12 -5 0 -31.90 32.60 -12 -5 0 17.10 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44.10 17.70 -6 -6 0 317.27 24.70 -6 -6 0 426.06 44.70 -6 -6 0 359.26 37.20 -6 -6 0 346.87 35.80 6 6 0 427.66 48.20 6 6 0 449.76 47.10 6 6 0 369.06 37.30 6 6 0 309.37 38.10 6 6 0 320.17 33.00 -7 -6 0 91.49 15.10 -7 -6 0 57.89 24.00 -7 -6 0 58.19 28.40 -7 -6 0 89.89 29.80 7 6 0 67.49 26.80 7 6 0 76.79 20.30 7 6 0 76.69 30.90 7 6 0 101.69 32.60 7 6 0 47.00 24.30 -8 -6 0 4.00 21.90 -8 -6 0 21.20 29.90 -8 -6 0 20.80 25.90 -8 -6 0 -37.10 19.80 8 6 0 23.00 25.50 8 6 0 16.80 16.90 8 6 0 -17.30 23.00 8 6 0 60.69 26.70 8 6 0 10.60 27.80 -9 -6 0 118.49 32.20 -9 -6 0 177.58 40.10 -9 -6 0 233.08 29.20 -9 -6 0 155.48 38.80 9 6 0 109.19 35.10 9 6 0 141.39 39.60 9 6 0 90.79 34.00 9 6 0 160.88 28.90 9 6 0 173.18 39.20 -10 -6 0 15.50 25.20 -10 -6 0 -17.10 20.70 -10 -6 0 13.20 27.50 -10 -6 0 27.20 32.60 10 6 0 -13.50 18.50 10 6 0 32.50 29.40 10 6 0 -16.70 27.80 10 6 0 -30.60 33.00 10 6 0 19.50 32.50 -11 -6 0 13.90 23.80 -11 -6 0 -3.10 33.10 -11 -6 0 -13.30 34.20 -11 -6 0 23.30 28.30 -11 -6 0 -13.10 23.80 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-6 -25 4.00 39.70 -1 -6 -25 -0.70 22.00 -1 -6 -25 -17.10 52.79 -1 -6 -25 13.10 34.30 1 6 25 -8.40 34.50 1 6 25 27.30 30.20 1 6 25 33.70 43.20 1 6 25 -44.50 31.60 -2 -6 -25 39.20 27.60 -2 -6 -25 96.09 38.50 -2 -6 -25 77.49 36.60 2 6 25 24.70 39.10 2 6 25 128.19 40.90 2 6 25 66.69 31.20 2 6 25 117.79 57.89 -3 -6 -25 95.29 41.30 -3 -6 -25 -4.50 26.40 -3 -6 -25 29.30 31.10 3 6 25 5.50 41.70 3 6 25 17.20 39.40 3 6 25 8.80 41.20 3 6 25 3.60 27.40 3 6 25 29.80 35.90 -4 -6 -25 75.39 33.50 -4 -6 -25 8.80 31.00 -4 -6 -25 33.00 39.30 -4 -6 -25 157.68 45.90 4 6 25 60.39 38.90 4 6 25 -16.20 34.00 4 6 25 9.70 41.70 4 6 25 -2.70 37.00 5 6 25 15.30 23.80 5 6 25 31.30 49.70 1 -7 -25 -9.70 22.50 1 -7 -25 -27.60 30.40 1 -7 -25 -0.40 30.70 -1 7 25 -14.60 35.70 -1 7 25 36.70 33.80 -1 7 25 -14.90 35.60 -1 7 25 -14.20 34.80 -1 7 25 -17.20 18.80 0 -7 -25 95.99 36.60 0 -7 -25 43.50 26.10 0 -7 -25 15.60 35.70 0 7 25 19.00 36.00 0 7 25 32.90 32.10 0 7 25 38.40 25.90 0 7 25 95.29 38.10 -1 -7 -25 70.69 28.50 -1 -7 -25 18.60 33.60 -1 -7 -25 -45.90 37.20 -1 -7 -25 63.19 35.00 1 7 25 -17.40 32.40 1 7 25 2.70 33.90 1 7 25 21.90 33.80 -2 -7 -25 22.70 30.80 -2 -7 -25 -10.60 21.60 -2 -7 -25 7.30 33.30 2 7 25 30.10 39.80 2 7 25 80.09 42.10 2 7 25 36.30 39.50 2 7 25 72.19 42.10 -3 -7 -25 28.20 31.70 -3 -7 -25 34.90 45.60 -3 -7 -25 15.20 21.70 -3 -7 -25 -30.00 31.60 3 7 25 -21.70 32.40 3 7 25 -20.30 35.50 3 7 25 -40.10 34.60 3 7 25 39.60 33.00 -4 -7 -25 60.49 38.10 -4 -7 -25 71.19 32.80 -4 -7 -25 17.70 34.60 -4 -7 -25 35.30 29.20 4 7 25 -46.90 35.10 4 7 25 48.10 44.20 4 7 25 -1.00 30.10 4 7 25 14.50 25.00 4 7 25 54.49 44.50 -1 -8 -25 6.80 31.80 -1 -8 -25 51.69 32.80 -1 -8 -25 37.80 24.80 1 8 25 15.20 23.80 1 8 25 80.99 35.30 1 8 25 36.50 37.70 1 8 25 -55.19 34.90 -2 -8 -25 -60.89 30.40 -2 -8 -25 -8.40 19.50 -2 -8 -25 -27.40 26.70 -2 -8 -25 -46.70 29.20 2 8 25 -17.60 37.20 2 8 25 -49.99 27.50 2 8 25 21.00 26.00 2 8 25 24.00 37.60 -3 -8 -25 78.79 39.90 -3 -8 -25 10.30 30.10 -3 -8 -25 46.90 35.00 -3 -8 -25 19.60 27.00 3 8 25 66.69 42.70 3 8 25 38.50 41.40 3 8 25 86.49 30.60 3 8 25 27.80 29.50 0 3 26 -48.70 32.80 0 3 26 23.20 27.60 -1 -3 -26 -25.60 32.90 1 3 26 4.50 34.70 1 3 26 20.80 25.40 1 3 26 3.20 39.60 0 -4 -26 98.69 39.30 0 -4 -26 25.50 35.00 0 -4 -26 3.90 28.50 0 4 26 5.10 40.10 0 4 26 28.80 38.50 -1 -4 -26 8.30 34.70 -1 -4 -26 -9.80 26.70 -1 -4 -26 -29.60 34.70 -1 -4 -26 61.39 38.60 1 4 26 148.09 47.30 1 4 26 -37.70 36.40 1 4 26 -30.60 34.90 -2 -4 -26 53.29 36.80 -2 -4 -26 2.80 26.10 -2 -4 -26 -20.00 37.20 2 4 26 19.40 37.00 2 4 26 -11.90 37.40 0 -5 -26 11.40 36.80 0 5 26 52.89 42.90 0 5 26 52.29 37.10 0 5 26 -29.90 19.40 -1 -5 -26 17.90 25.90 -1 -5 -26 2.10 37.10 -1 -5 -26 62.59 40.10 -1 -5 -26 10.10 34.50 1 5 26 32.50 35.70 1 5 26 95.79 46.00 1 5 26 -12.30 32.00 1 5 26 16.30 37.00 -2 -5 -26 39.10 32.50 -2 -5 -26 28.80 27.40 -2 -5 -26 -30.90 34.20 2 5 26 -6.90 23.80 2 5 26 -98.49 34.40 2 5 26 23.40 35.70 1 6 26 -0.60 22.50 2 6 26 -1.00 23.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 26901 _olex2_submission_special_instructions 'No special instructions were received' _vrf_RINTA01_jcm11921a_0m ; PROBLEM:The value of Rint is greater than 0.18 Rint given 0.202 RESPONSE: Despite the value for the Rint is above 0.18, the final model is of a reasonable quality. The data measured allowed for an unambiguous structure solution and refinement which are fully consistent with the spectroscopic characterization of the compound. ; _vrf_PLAT020_jcm11921a_0m ; PROBLEM:The Value of Rint is Greater Than 0.12 ......... 0.202 Report RESPONSE: same as RINTA01. ;