data_jcm10221a_0ma _audit_creation_date 2021-11-04 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _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 ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common . _chemical_name_systematic . _chemical_formula_moiety 'C32 H48 F10 Fe P4 Zn' _chemical_formula_sum 'C32 H48 F10 Fe P4 Zn' _chemical_formula_weight 867.80 _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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 '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 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.5085(16) _cell_length_b 11.3314(16) _cell_length_c 20.086(3) _cell_angle_alpha 90 _cell_angle_beta 111.281(6) _cell_angle_gamma 90 _cell_volume 3713.2(8) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3381 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 25.77 _cell_measurement_theta_min 2.18 _shelx_estimated_absorpt_T_max 0.882 _shelx_estimated_absorpt_T_min 0.882 _exptl_absorpt_coefficient_mu 1.282 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0968 before and 0.0866 after correction. The Ratio of minimum to maximum transmission is 0.8980. 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 1.552 _exptl_crystal_density_meas . _exptl_crystal_density_method . _exptl_crystal_description Block _exptl_crystal_F_000 1784 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1746 _diffrn_reflns_av_unetI/netI 0.0527 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 55341 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.350 _diffrn_reflns_theta_min 2.176 _diffrn_ambient_temperature 193.00 _diffrn_detector_area_resol_mean . _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _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 2443 _reflns_number_total 3417 _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 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 0.810 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.097 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 222 _refine_ls_number_reflns 3417 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0418 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+15.2022P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.1044 _refine_special_details . _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B) 2.b Idealised Me refined as rotating group: C10(H10A,H10B,H10C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B, H16C) ; _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 Zn1 Zn 0.5000 0.82901(6) 0.2500 0.02603(19) Uani 1 2 d S T P . . Fe1 Fe 0.5000 0.60302(7) 0.2500 0.0198(2) Uani 1 2 d S T P . . P1 P 0.56431(6) 0.60346(10) 0.17167(6) 0.0226(2) Uani 1 1 d . . . . . P2 P 0.40926(7) 0.48727(10) 0.16867(6) 0.0240(3) Uani 1 1 d . . . . . F1 F 0.38046(19) 1.0517(3) -0.00828(16) 0.0608(9) Uani 1 1 d . . . . . F2 F 0.5084(2) 1.2047(3) 0.02581(16) 0.0563(8) Uani 1 1 d . . . . . F3 F 0.63189(18) 1.1901(3) 0.15457(16) 0.0520(8) Uani 1 1 d . . . . . F4 F 0.62909(17) 1.0241(3) 0.24946(15) 0.0481(8) Uani 1 1 d . . . . . F5 F 0.37605(18) 0.8857(3) 0.08579(16) 0.0575(9) Uani 1 1 d . . . . . C1 C 0.5029(3) 0.9463(4) 0.1718(2) 0.0293(10) Uani 1 1 d . . . . . C2 C 0.4422(3) 0.9594(4) 0.1057(2) 0.0336(11) Uani 1 1 d . . . . . C3 C 0.4425(3) 1.0433(4) 0.0562(2) 0.0378(12) Uani 1 1 d . . . . . C4 C 0.5063(3) 1.1209(4) 0.0729(2) 0.0367(11) Uani 1 1 d . . . . . C5 C 0.5686(3) 1.1129(4) 0.1384(3) 0.0337(11) Uani 1 1 d . . . . . C6 C 0.5649(3) 1.0270(4) 0.1856(2) 0.0315(10) Uani 1 1 d . . . . . C7 C 0.4850(3) 0.5875(4) 0.0827(2) 0.0276(10) Uani 1 1 d . . . . . H7A H 0.4509 0.6597 0.0697 0.033 Uiso 1 1 calc R U . . . H7B H 0.5104 0.5746 0.0465 0.033 Uiso 1 1 calc R U . . . C8 C 0.4327(3) 0.4814(4) 0.0857(2) 0.0322(11) Uani 1 1 d . . . . . H8A H 0.4625 0.4076 0.0847 0.039 Uiso 1 1 calc R U . . . H8B H 0.3811 0.4819 0.0435 0.039 Uiso 1 1 calc R U . . . C9 C 0.3011(3) 0.5359(4) 0.1330(2) 0.0331(11) Uani 1 1 d . . . . . H9A H 0.2672 0.4700 0.1051 0.040 Uiso 1 1 calc R U . . . H9B H 0.2835 0.5512 0.1738 0.040 Uiso 1 1 calc R U . . . C10 C 0.2827(3) 0.6448(5) 0.0860(3) 0.0447(13) Uani 1 1 d . . . . . H10A H 0.2978 0.6302 0.0442 0.067 Uiso 1 1 calc R U . . . H10B H 0.3143 0.7117 0.1132 0.067 Uiso 1 1 calc R U . . . H10C H 0.2240 0.6628 0.0701 0.067 Uiso 1 1 calc R U . . . C11 C 0.3982(3) 0.3275(4) 0.1806(2) 0.0325(10) Uani 1 1 d . . . . . H11A H 0.4531 0.2912 0.1933 0.039 Uiso 1 1 calc R U . . . H11B H 0.3812 0.3170 0.2221 0.039 Uiso 1 1 calc R U . . . C12 C 0.3384(3) 0.2571(4) 0.1178(3) 0.0420(13) Uani 1 1 d . . . . . H12A H 0.3512 0.2709 0.0748 0.063 Uiso 1 1 calc R U . . . H12B H 0.2822 0.2827 0.1092 0.063 Uiso 1 1 calc R U . . . H12C H 0.3437 0.1728 0.1294 0.063 Uiso 1 1 calc R U . . . C13 C 0.6218(3) 0.7282(4) 0.1563(2) 0.0288(10) Uani 1 1 d . . . . . H13A H 0.6393 0.7087 0.1159 0.035 Uiso 1 1 calc R U . . . H13B H 0.5849 0.7973 0.1420 0.035 Uiso 1 1 calc R U . . . C14 C 0.6977(3) 0.7625(5) 0.2207(3) 0.0460(13) Uani 1 1 d . . . . . H14A H 0.7215 0.8348 0.2098 0.069 Uiso 1 1 calc R U . . . H14B H 0.7381 0.6987 0.2314 0.069 Uiso 1 1 calc R U . . . H14C H 0.6819 0.7760 0.2622 0.069 Uiso 1 1 calc R U . . . C15 C 0.6331(3) 0.4789(4) 0.1739(2) 0.0332(11) Uani 1 1 d . . . . . H15A H 0.6803 0.4834 0.2198 0.040 Uiso 1 1 calc R U . . . H15B H 0.6032 0.4052 0.1750 0.040 Uiso 1 1 calc R U . . . C16 C 0.6673(3) 0.4665(5) 0.1148(3) 0.0406(12) Uani 1 1 d . . . . . H16A H 0.6221 0.4583 0.0687 0.061 Uiso 1 1 calc R U . . . H16B H 0.7025 0.3965 0.1236 0.061 Uiso 1 1 calc R U . . . H16C H 0.6996 0.5367 0.1138 0.061 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 Zn1 0.0289(4) 0.0232(4) 0.0238(4) 0.000 0.0069(3) 0.000 Fe1 0.0211(4) 0.0213(5) 0.0164(4) 0.000 0.0059(3) 0.000 P1 0.0246(6) 0.0243(6) 0.0194(5) 0.0004(5) 0.0085(4) -0.0001(5) P2 0.0267(6) 0.0251(6) 0.0203(6) -0.0027(5) 0.0087(5) -0.0041(5) F1 0.060(2) 0.065(2) 0.0366(17) 0.0159(16) -0.0073(15) -0.0074(17) F2 0.080(2) 0.0449(19) 0.0468(18) 0.0208(15) 0.0258(16) -0.0035(17) F3 0.0533(18) 0.0412(18) 0.060(2) 0.0027(15) 0.0191(16) -0.0198(15) F4 0.0427(17) 0.0466(18) 0.0400(17) 0.0054(14) -0.0032(14) -0.0100(14) F5 0.0486(18) 0.057(2) 0.0493(19) 0.0107(16) -0.0032(15) -0.0262(16) C1 0.032(2) 0.024(2) 0.030(2) -0.0009(19) 0.009(2) 0.0013(19) C2 0.034(3) 0.026(2) 0.037(3) 0.001(2) 0.009(2) -0.007(2) C3 0.038(3) 0.039(3) 0.028(3) 0.006(2) 0.003(2) 0.003(2) C4 0.052(3) 0.029(3) 0.033(3) 0.012(2) 0.019(2) 0.004(2) C5 0.043(3) 0.022(2) 0.040(3) -0.004(2) 0.020(2) -0.006(2) C6 0.033(3) 0.029(2) 0.028(2) 0.000(2) 0.005(2) 0.003(2) C7 0.027(2) 0.038(3) 0.018(2) -0.0013(19) 0.0086(18) -0.005(2) C8 0.036(3) 0.037(3) 0.025(2) -0.009(2) 0.012(2) -0.012(2) C9 0.029(2) 0.036(3) 0.031(3) -0.001(2) 0.007(2) -0.007(2) C10 0.035(3) 0.049(3) 0.043(3) 0.012(3) 0.006(2) 0.002(2) C11 0.038(3) 0.028(2) 0.034(3) -0.005(2) 0.015(2) -0.004(2) C12 0.050(3) 0.036(3) 0.046(3) -0.017(2) 0.025(3) -0.016(2) C13 0.032(2) 0.030(2) 0.028(2) 0.000(2) 0.015(2) -0.003(2) C14 0.039(3) 0.052(3) 0.048(3) -0.007(3) 0.017(2) -0.018(3) C15 0.040(3) 0.032(3) 0.030(2) 0.003(2) 0.015(2) 0.008(2) C16 0.051(3) 0.043(3) 0.036(3) 0.001(2) 0.026(2) 0.010(3) _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 Zn1 Fe1 2.5607(12) . ? Zn1 C1 2.073(5) . ? Zn1 C1 2.073(4) 2_655 ? Fe1 P1 2.2426(11) . ? Fe1 P1 2.2426(11) 2_655 ? Fe1 P2 2.2426(12) . ? Fe1 P2 2.2426(12) 2_655 ? P1 C7 1.831(4) . ? P1 C13 1.825(4) . ? P1 C15 1.845(5) . ? P2 C8 1.858(4) . ? P2 C9 1.849(4) . ? P2 C11 1.845(5) . ? F1 C3 1.358(5) . ? F2 C4 1.350(5) . ? F3 C5 1.356(5) . ? F4 C6 1.365(5) . ? F5 C2 1.364(5) . ? C1 C2 1.375(6) . ? C1 C6 1.369(6) . ? C2 C3 1.378(6) . ? C3 C4 1.364(7) . ? C4 C5 1.374(6) . ? C5 C6 1.376(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C7 C8 1.525(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C9 C10 1.516(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.538(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.530(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.520(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn1 Fe1 129.88(12) . . ? C1 Zn1 Fe1 129.88(12) 2_655 . ? C1 Zn1 C1 100.2(2) . 2_655 ? P1 Fe1 Zn1 89.87(4) 2_655 . ? P1 Fe1 Zn1 89.87(4) . . ? P1 Fe1 P1 179.75(7) 2_655 . ? P1 Fe1 P2 96.26(4) . 2_655 ? P1 Fe1 P2 83.89(4) 2_655 2_655 ? P2 Fe1 Zn1 125.79(3) 2_655 . ? P2 Fe1 Zn1 125.79(3) . . ? P2 Fe1 P1 83.89(4) . . ? P2 Fe1 P1 96.26(4) . 2_655 ? P2 Fe1 P2 108.41(7) . 2_655 ? C7 P1 Fe1 106.78(14) . . ? C7 P1 C15 101.9(2) . . ? C13 P1 Fe1 124.64(15) . . ? C13 P1 C7 100.4(2) . . ? C13 P1 C15 101.6(2) . . ? C15 P1 Fe1 118.07(15) . . ? C8 P2 Fe1 110.22(14) . . ? C9 P2 Fe1 117.62(16) . . ? C9 P2 C8 101.0(2) . . ? C11 P2 Fe1 124.00(15) . . ? C11 P2 C8 98.6(2) . . ? C11 P2 C9 101.6(2) . . ? C2 C1 Zn1 125.3(3) . . ? C6 C1 Zn1 120.7(3) . . ? C6 C1 C2 113.7(4) . . ? F5 C2 C1 119.5(4) . . ? F5 C2 C3 115.9(4) . . ? C1 C2 C3 124.6(4) . . ? F1 C3 C2 121.7(4) . . ? F1 C3 C4 119.3(4) . . ? C4 C3 C2 119.0(4) . . ? F2 C4 C3 120.6(4) . . ? F2 C4 C5 120.3(4) . . ? C3 C4 C5 119.2(4) . . ? F3 C5 C4 118.8(4) . . ? F3 C5 C6 122.0(4) . . ? C4 C5 C6 119.2(4) . . ? F4 C6 C1 119.8(4) . . ? F4 C6 C5 115.8(4) . . ? C1 C6 C5 124.4(4) . . ? P1 C7 H7A 110.3 . . ? P1 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C8 C7 P1 107.0(3) . . ? C8 C7 H7A 110.3 . . ? C8 C7 H7B 110.3 . . ? P2 C8 H8A 109.7 . . ? P2 C8 H8B 109.7 . . ? C7 C8 P2 109.8(3) . . ? C7 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? P2 C9 H9A 108.3 . . ? P2 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C10 C9 P2 116.1(3) . . ? C10 C9 H9A 108.3 . . ? C10 C9 H9B 108.3 . . ? 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 107.7 . . ? P2 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? C12 C11 P2 118.4(3) . . ? C12 C11 H11A 107.7 . . ? C12 C11 H11B 107.7 . . ? 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 C13 H13A 108.6 . . ? P1 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C14 C13 P1 114.6(3) . . ? C14 C13 H13A 108.6 . . ? C14 C13 H13B 108.6 . . ? 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 . . ? P1 C15 H15A 107.5 . . ? P1 C15 H15B 107.5 . . ? H15A C15 H15B 107.0 . . ? C16 C15 P1 119.4(3) . . ? C16 C15 H15A 107.5 . . ? C16 C15 H15B 107.5 . . ? 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 . . ? 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 Zn1 C1 C2 F5 -4.8(7) . . . . ? Zn1 C1 C2 C3 175.3(4) . . . . ? Zn1 C1 C6 F4 5.5(6) . . . . ? Zn1 C1 C6 C5 -175.5(4) . . . . ? Fe1 P1 C7 C8 -51.1(3) . . . . ? Fe1 P1 C13 C14 64.1(4) . . . . ? Fe1 P1 C15 C16 170.7(3) . . . . ? Fe1 P2 C8 C7 -20.7(4) . . . . ? Fe1 P2 C9 C10 68.4(4) . . . . ? Fe1 P2 C11 C12 -175.0(3) . . . . ? P1 C7 C8 P2 44.5(4) . . . . ? F1 C3 C4 F2 -0.7(7) . . . . ? F1 C3 C4 C5 179.4(4) . . . . ? F2 C4 C5 F3 -0.2(7) . . . . ? F2 C4 C5 C6 179.8(4) . . . . ? F3 C5 C6 F4 -0.2(7) . . . . ? F3 C5 C6 C1 -179.3(4) . . . . ? F5 C2 C3 F1 0.2(7) . . . . ? F5 C2 C3 C4 179.2(4) . . . . ? C1 C2 C3 F1 -179.9(5) . . . . ? C1 C2 C3 C4 -1.0(8) . . . . ? C2 C1 C6 F4 179.8(4) . . . . ? C2 C1 C6 C5 -1.1(7) . . . . ? C2 C3 C4 F2 -179.6(4) . . . . ? C2 C3 C4 C5 0.4(8) . . . . ? C3 C4 C5 F3 179.7(4) . . . . ? C3 C4 C5 C6 -0.2(7) . . . . ? C4 C5 C6 F4 179.7(4) . . . . ? C4 C5 C6 C1 0.6(7) . . . . ? C6 C1 C2 F5 -178.9(4) . . . . ? C6 C1 C2 C3 1.3(7) . . . . ? C7 P1 C13 C14 -177.0(4) . . . . ? C7 P1 C15 C16 54.2(4) . . . . ? C8 P2 C9 C10 -51.5(4) . . . . ? C8 P2 C11 C12 -53.4(4) . . . . ? C9 P2 C8 C7 104.4(3) . . . . ? C9 P2 C11 C12 49.8(4) . . . . ? C11 P2 C8 C7 -151.8(3) . . . . ? C11 P2 C9 C10 -152.8(4) . . . . ? C13 P1 C7 C8 177.7(3) . . . . ? C13 P1 C15 C16 -49.2(4) . . . . ? C15 P1 C7 C8 73.3(3) . . . . ? C15 P1 C13 C14 -72.5(4) . . . . ? _shelx_res_file ; jcm10221a_0ma.res created by SHELXL-2014/7 TITL jcm10221a_0ma_a.res in C2/c CELL 0.71073 17.5085 11.3314 20.0859 90 111.281 90 ZERR 4 0.0016 0.0016 0.0026 0 0.006 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F Fe P Zn UNIT 128 192 40 4 16 4 L.S. 4 PLAN 10 0 0 SIZE 0.1 0.1 0.1 TEMP -80.15 CONF HTAB MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.028800 15.202200 FVAR 0.19853 ZN1 6 0.500000 0.829005 0.250000 10.50000 0.02888 0.02322 = 0.02379 0.00000 0.00691 0.00000 FE1 4 0.500000 0.603021 0.250000 10.50000 0.02111 0.02125 = 0.01637 0.00000 0.00588 0.00000 P1 5 0.564309 0.603460 0.171667 11.00000 0.02461 0.02426 = 0.01944 0.00040 0.00854 -0.00010 P2 5 0.409257 0.487270 0.168670 11.00000 0.02668 0.02510 = 0.02029 -0.00275 0.00872 -0.00411 F1 3 0.380465 1.051742 -0.008277 11.00000 0.05979 0.06533 = 0.03662 0.01592 -0.00727 -0.00741 F2 3 0.508377 1.204679 0.025812 11.00000 0.07957 0.04486 = 0.04679 0.02083 0.02582 -0.00354 F3 3 0.631886 1.190088 0.154569 11.00000 0.05330 0.04121 = 0.06016 0.00269 0.01907 -0.01977 F4 3 0.629087 1.024144 0.249463 11.00000 0.04266 0.04656 = 0.03995 0.00541 -0.00320 -0.01001 F5 3 0.376050 0.885671 0.085793 11.00000 0.04861 0.05711 = 0.04934 0.01066 -0.00320 -0.02623 C1 1 0.502883 0.946282 0.171763 11.00000 0.03211 0.02407 = 0.03004 -0.00090 0.00942 0.00127 C2 1 0.442156 0.959395 0.105675 11.00000 0.03385 0.02635 = 0.03718 0.00066 0.00870 -0.00734 C3 1 0.442504 1.043313 0.056155 11.00000 0.03824 0.03911 = 0.02840 0.00587 0.00308 0.00342 C4 1 0.506287 1.120944 0.072905 11.00000 0.05160 0.02920 = 0.03273 0.01212 0.01947 0.00389 C5 1 0.568570 1.112900 0.138443 11.00000 0.04253 0.02203 = 0.04047 -0.00379 0.01993 -0.00613 C6 1 0.564894 1.027021 0.185602 11.00000 0.03270 0.02882 = 0.02797 -0.00004 0.00507 0.00272 C7 1 0.485009 0.587548 0.082685 11.00000 0.02673 0.03811 = 0.01838 -0.00131 0.00860 -0.00535 AFIX 23 H7A 2 0.450858 0.659664 0.069709 11.00000 -1.20000 H7B 2 0.510385 0.574587 0.046543 11.00000 -1.20000 AFIX 0 C8 1 0.432721 0.481438 0.085660 11.00000 0.03580 0.03670 = 0.02457 -0.00879 0.01162 -0.01174 AFIX 23 H8A 2 0.462537 0.407602 0.084713 11.00000 -1.20000 H8B 2 0.381057 0.481889 0.043463 11.00000 -1.20000 AFIX 0 C9 1 0.301079 0.535854 0.132967 11.00000 0.02875 0.03596 = 0.03106 -0.00076 0.00666 -0.00741 AFIX 23 H9A 2 0.267249 0.470006 0.105108 11.00000 -1.20000 H9B 2 0.283526 0.551209 0.173793 11.00000 -1.20000 AFIX 0 C10 1 0.282693 0.644773 0.085954 11.00000 0.03514 0.04912 = 0.04310 0.01180 0.00629 0.00244 AFIX 137 H10A 2 0.297822 0.630217 0.044243 11.00000 -1.50000 H10B 2 0.314328 0.711681 0.113153 11.00000 -1.50000 H10C 2 0.224041 0.662837 0.070073 11.00000 -1.50000 AFIX 0 C11 1 0.398244 0.327510 0.180566 11.00000 0.03765 0.02763 = 0.03425 -0.00490 0.01540 -0.00393 AFIX 23 H11A 2 0.453127 0.291156 0.193291 11.00000 -1.20000 H11B 2 0.381178 0.317036 0.222095 11.00000 -1.20000 AFIX 0 C12 1 0.338405 0.257101 0.117800 11.00000 0.05021 0.03555 = 0.04624 -0.01724 0.02461 -0.01640 AFIX 137 H12A 2 0.351221 0.270945 0.074831 11.00000 -1.50000 H12B 2 0.282152 0.282719 0.109164 11.00000 -1.50000 H12C 2 0.343710 0.172770 0.129405 11.00000 -1.50000 AFIX 0 C13 1 0.621839 0.728159 0.156335 11.00000 0.03226 0.02980 = 0.02802 0.00020 0.01529 -0.00253 AFIX 23 H13A 2 0.639253 0.708704 0.115922 11.00000 -1.20000 H13B 2 0.584883 0.797302 0.142041 11.00000 -1.20000 AFIX 0 C14 1 0.697654 0.762515 0.220734 11.00000 0.03858 0.05163 = 0.04843 -0.00714 0.01653 -0.01817 AFIX 137 H14A 2 0.721513 0.834838 0.209836 11.00000 -1.50000 H14B 2 0.738095 0.698678 0.231399 11.00000 -1.50000 H14C 2 0.681920 0.776039 0.262221 11.00000 -1.50000 AFIX 0 C15 1 0.633115 0.478930 0.173934 11.00000 0.04014 0.03170 = 0.02976 0.00345 0.01518 0.00797 AFIX 23 H15A 2 0.680251 0.483399 0.219784 11.00000 -1.20000 H15B 2 0.603219 0.405220 0.174989 11.00000 -1.20000 AFIX 0 C16 1 0.667340 0.466495 0.114750 11.00000 0.05101 0.04299 = 0.03607 0.00125 0.02565 0.00965 AFIX 137 H16A 2 0.622052 0.458266 0.068708 11.00000 -1.50000 H16B 2 0.702465 0.396455 0.123576 11.00000 -1.50000 H16C 2 0.699575 0.536747 0.113799 11.00000 -1.50000 AFIX 0 HKLF 4 REM jcm10221a_0ma_a.res in C2/c REM R1 = 0.0418 for 2443 Fo > 4sig(Fo) and 0.0812 for all 3417 data REM 222 parameters refined using 0 restraints END WGHT 0.0285 15.3165 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, -y+3/2, -z HTAB C9 F1_$1 HTAB C10 F5 EQIV $2 -x+3/2, y-1/2, -z+1/2 HTAB C14 F3_$2 EQIV $3 x, y-1, z HTAB C15 F3_$3 REM Highest difference peak 0.810, deepest hole -0.489, 1-sigma level 0.097 Q1 1 0.5547 0.7051 0.2840 11.00000 0.05 0.81 Q2 1 0.5611 0.7672 0.3089 11.00000 0.05 0.62 Q3 1 0.5635 0.8271 0.1723 11.00000 0.05 0.58 Q4 1 0.5455 0.6636 0.3181 11.00000 0.05 0.50 Q5 1 0.5000 0.3775 0.2500 10.50000 0.05 0.50 Q6 1 0.4138 0.7147 0.1701 11.00000 0.05 0.45 Q7 1 0.4095 0.9409 0.1613 11.00000 0.05 0.38 Q8 1 0.6266 0.6047 0.0892 11.00000 0.05 0.37 Q9 1 0.4086 0.1683 0.1604 11.00000 0.05 0.36 Q10 1 0.4475 0.5507 0.1864 11.00000 0.05 0.35 ; _shelx_res_checksum 82975 _shelx_hkl_file ; -1 -1 0 30.00 7.60 -1 -1 0 21.30 5.90 -1 -1 0 27.30 7.10 1 1 0 22.30 8.10 1 1 0 22.50 6.20 1 1 0 19.90 6.00 1 1 0 20.80 5.90 -2 -2 0 614.74 30.20 -2 -2 0 627.24 30.40 -2 -2 0 592.04 33.50 2 2 0 630.94 30.20 2 2 0 625.24 34.70 2 2 0 602.74 30.10 2 2 0 616.54 30.30 -3 -3 0 12.30 16.80 -3 -3 0 13.90 12.70 -3 -3 0 2.90 10.30 3 3 0 23.30 13.50 3 3 0 2.40 15.60 3 3 0 9.20 14.00 3 3 0 3.70 12.00 -4 -4 0 2026.40 73.89 -4 -4 0 2067.99 76.59 -4 -4 0 1974.10 87.39 -4 -4 0 2065.99 74.29 4 4 0 2148.98 77.59 4 4 0 2131.69 91.39 4 4 0 2044.70 74.39 4 4 0 2045.40 74.79 4 4 0 1927.21 44.50 -5 -5 0 1348.47 64.29 -5 -5 0 1504.75 81.39 -5 -5 0 1303.87 64.29 5 5 0 1374.46 67.29 5 5 0 1346.97 65.29 5 5 0 1526.75 85.29 5 5 0 1382.26 66.29 -6 -6 0 20.20 18.80 -6 -6 0 72.29 28.40 -6 -6 0 92.69 23.20 -6 -6 0 46.20 19.00 6 6 0 44.60 23.70 6 6 0 40.70 21.70 6 6 0 78.79 21.70 6 6 0 54.29 21.20 -7 -7 0 132.89 38.10 -7 -7 0 100.99 28.30 -7 -7 0 108.69 29.40 -7 -7 0 150.38 34.30 7 7 0 100.99 29.40 7 7 0 117.79 30.80 7 7 0 94.69 25.50 7 7 0 123.69 38.20 -8 -8 0 157.38 36.00 -8 -8 0 150.58 42.00 -8 -8 0 162.08 34.60 8 8 0 149.09 34.70 8 8 0 180.38 38.20 8 8 0 128.79 46.80 8 8 0 210.98 53.29 8 8 0 173.28 39.20 -9 -9 0 81.19 24.80 -9 -9 0 29.40 23.70 -9 -9 0 51.59 27.50 -9 -9 0 93.79 43.70 9 9 0 71.29 38.90 9 9 0 95.99 35.10 9 9 0 65.49 30.60 9 9 0 83.39 27.30 9 9 0 73.29 28.50 -10 -10 0 16.10 21.20 -10 -10 0 -36.10 19.10 -10 -10 0 40.10 39.10 -10 -10 0 -7.80 19.30 10 10 0 7.40 28.60 10 10 0 5.50 22.50 10 10 0 -12.80 28.90 10 10 0 27.10 23.60 -11 -11 0 22.00 27.30 -11 -11 0 29.60 22.60 -11 -11 0 34.10 27.90 11 11 0 27.30 20.30 11 11 0 17.10 22.90 11 11 0 18.30 31.70 11 11 0 22.60 39.40 12 10 -1 8.80 22.10 12 10 -1 -26.70 22.80 12 10 -1 39.50 28.30 12 10 -1 -9.80 26.50 12 10 -1 102.19 36.30 -12 -10 1 30.30 28.30 -12 -10 1 12.40 23.00 11 9 -1 65.09 27.60 11 9 -1 69.59 27.60 11 9 -1 -4.90 32.30 11 9 -1 31.70 33.80 11 9 -1 65.39 25.90 -11 -9 1 50.89 24.40 -11 -9 1 27.50 27.30 10 8 -1 86.59 27.20 10 8 -1 96.69 34.60 10 8 -1 118.19 42.00 10 8 -1 87.29 27.70 10 8 -1 122.39 42.80 -10 -8 1 85.59 30.00 -10 -8 1 82.79 28.80 -10 -8 1 83.99 27.60 9 7 -1 12.00 16.50 9 7 -1 -14.30 14.90 9 7 -1 5.60 17.10 9 7 -1 -2.20 19.20 -9 -7 1 9.60 15.80 -9 -7 1 1.10 20.60 -9 -7 1 47.60 20.40 -9 -7 1 -1.50 19.30 8 6 -1 51.29 5.70 8 6 -1 87.69 32.50 8 6 -1 54.39 20.90 8 6 -1 57.09 22.20 8 6 -1 52.69 5.80 8 6 -1 77.29 23.30 -8 -6 1 38.30 19.50 -8 -6 1 38.90 19.30 -8 -6 1 57.39 22.50 -8 -6 1 85.59 33.00 7 5 -1 0.60 17.20 7 5 -1 4.50 6.10 7 5 -1 -3.80 11.90 7 5 -1 9.80 14.20 7 5 -1 4.90 14.50 -7 -5 1 22.00 15.10 -7 -5 1 -6.20 12.80 -7 -5 1 36.60 25.00 -7 -5 1 8.80 12.50 6 4 -1 3.90 11.30 6 4 -1 3.60 8.30 6 4 -1 14.60 11.60 6 4 -1 -9.50 15.80 6 4 -1 -3.00 11.90 -6 -4 1 2.40 19.10 -6 -4 1 7.10 13.40 -6 -4 1 5.30 13.30 5 3 -1 85.89 13.30 5 3 -1 80.99 16.80 5 3 -1 95.59 21.30 5 3 -1 69.39 19.90 5 3 -1 91.69 15.80 -5 -3 1 86.19 21.50 -5 -3 1 102.09 18.50 -5 -3 1 90.99 17.00 -5 -3 1 72.49 18.30 4 2 -1 222.28 17.50 4 2 -1 213.28 17.20 4 2 -1 234.18 19.30 4 2 -1 195.58 25.90 4 2 -1 232.38 25.40 -4 -2 1 266.37 26.50 -4 -2 1 224.38 17.20 -4 -2 1 214.88 16.80 3 1 -1 730.53 21.10 3 1 -1 763.72 21.40 3 1 -1 763.02 30.80 3 1 -1 721.93 33.70 -3 -1 1 743.93 30.00 -3 -1 1 712.83 20.70 -3 -1 1 703.33 32.90 -3 -1 1 729.13 21.10 2 0 -1 3.40 3.90 2 0 -1 0.10 4.10 2 0 -1 -4.70 3.60 2 0 -1 2.90 5.90 -2 0 1 0.60 4.40 -2 0 1 1.90 4.80 -2 0 1 1.40 4.10 -2 0 1 -3.00 4.30 1 -1 -1 1137.99 36.90 1 -1 -1 1185.48 37.40 1 -1 -1 1177.98 37.20 1 -1 -1 1117.79 36.10 1 -1 -1 1142.79 36.40 -1 1 1 1145.39 36.90 -1 1 1 1257.67 38.80 -1 1 1 1134.39 36.30 -1 1 1 1139.29 36.20 -1 1 1 1126.69 36.90 0 -2 -1 616.84 33.80 0 -2 -1 627.84 34.30 0 -2 -1 539.45 32.60 0 -2 -1 579.34 26.40 0 2 1 585.04 31.30 0 2 1 580.74 33.70 0 2 1 617.14 26.50 0 2 1 538.65 34.40 -1 -3 -1 100.89 24.70 -1 -3 -1 95.69 19.30 -1 -3 -1 72.29 16.50 -1 -3 -1 86.49 12.10 -1 -3 -1 93.39 23.20 1 3 1 99.59 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6 6 -3 16.40 17.00 6 6 -3 23.30 20.00 6 6 -3 49.40 26.40 6 6 -3 37.50 22.90 -6 -6 3 19.80 25.20 -6 -6 3 7.10 20.00 -6 -6 3 42.60 22.70 -6 -6 3 60.59 25.10 5 5 -3 27.60 18.60 5 5 -3 71.39 25.60 5 5 -3 57.49 22.90 5 5 -3 56.59 28.20 5 5 -3 53.69 21.10 -5 -5 3 53.99 25.40 -5 -5 3 55.49 23.60 -5 -5 3 19.90 20.20 4 4 -3 202.18 31.50 4 4 -3 247.88 34.60 4 4 -3 246.98 33.60 4 4 -3 210.98 34.80 4 4 -3 249.28 39.90 -4 -4 3 285.67 38.30 -4 -4 3 183.38 33.40 -4 -4 3 216.48 33.10 -4 -4 3 186.48 12.50 3 3 -3 892.81 53.19 3 3 -3 952.10 43.20 3 3 -3 992.60 49.10 3 3 -3 893.81 50.49 -3 -3 3 979.20 48.80 -3 -3 3 942.51 33.40 -3 -3 3 956.20 54.09 2 2 -3 2412.76 62.49 2 2 -3 2406.56 72.29 2 2 -3 2251.77 72.99 2 2 -3 2268.17 72.29 2 2 -3 2312.97 78.09 -2 -2 3 2204.58 60.89 -2 -2 3 2073.79 74.59 -2 -2 3 2288.17 61.79 -2 -2 3 2305.37 71.19 -2 -2 3 2262.27 71.59 1 1 -3 813.42 36.40 1 1 -3 768.32 38.40 1 1 -3 851.11 36.60 1 1 -3 792.22 29.80 1 1 -3 775.62 38.50 -1 -1 3 831.92 30.90 -1 -1 3 885.51 37.40 -1 -1 3 787.42 35.90 0 0 -3 5.40 10.80 0 0 -3 -0.90 7.30 0 0 -3 -6.00 7.80 0 0 -3 5.10 12.20 0 0 3 2.80 10.90 0 0 3 -2.50 7.40 0 0 3 3.00 11.70 0 0 3 -0.40 10.70 -1 -1 -3 1878.61 39.60 -1 -1 -3 1977.50 59.29 -1 -1 -3 1920.51 59.79 -1 -1 -3 1938.81 65.29 1 1 3 1968.50 66.09 1 1 3 1963.10 60.49 1 1 3 1867.21 59.19 1 1 3 1903.11 38.40 1 1 3 2013.70 59.09 -2 -2 -3 790.22 48.10 -2 -2 -3 887.01 42.00 -2 -2 -3 832.42 44.40 2 2 3 784.52 39.50 2 2 3 856.41 47.70 2 2 3 791.12 39.10 2 2 3 761.52 44.20 -3 -3 -3 794.02 27.30 -3 -3 -3 949.31 47.20 -3 -3 -3 831.12 44.00 3 3 3 919.71 55.39 3 3 3 826.12 56.09 3 3 3 875.81 45.30 3 3 3 744.53 42.80 -4 -4 -3 951.20 52.89 -4 -4 -3 911.21 62.29 -4 -4 -3 972.40 52.09 -4 -4 -3 971.00 38.20 4 4 3 873.91 62.39 4 4 3 913.41 47.10 4 4 3 917.11 52.19 4 4 3 958.40 38.40 4 4 3 946.01 52.09 4 4 3 917.51 63.59 -5 -5 -3 111.29 18.70 -5 -5 -3 116.19 31.20 -5 -5 -3 111.29 25.80 -5 -5 -3 131.09 25.80 5 5 3 117.79 27.00 5 5 3 132.49 33.70 5 5 3 121.09 20.70 5 5 3 164.18 32.00 5 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65.59 34.40 -5 -13 1 91.09 56.49 4 12 -1 5.70 32.40 4 12 -1 25.40 38.70 4 12 -1 -12.50 37.00 4 12 -1 26.00 36.40 -4 -12 1 16.50 25.40 -4 -12 1 -15.20 29.20 -4 -12 1 -3.10 19.70 -4 -12 1 6.60 27.80 3 11 -1 -20.80 26.40 3 11 -1 -28.50 25.60 3 11 -1 9.80 26.30 3 11 -1 -19.90 18.80 -3 -11 1 -4.30 33.20 -3 -11 1 -11.40 27.10 -3 -11 1 29.10 28.00 -3 -11 1 19.00 35.40 2 10 -1 19.60 25.60 2 10 -1 49.40 28.60 2 10 -1 84.99 33.10 -2 -10 1 73.19 42.20 -2 -10 1 9.60 23.50 -2 -10 1 54.99 13.50 -2 -10 1 99.09 37.20 -2 -10 1 44.20 50.19 1 9 -1 339.77 65.29 1 9 -1 380.36 67.89 1 9 -1 268.67 56.19 1 9 -1 306.27 57.29 -1 -9 1 262.97 50.89 -1 -9 1 357.46 61.39 -1 -9 1 267.97 32.10 -1 -9 1 308.77 59.79 -1 -9 1 269.17 57.59 0 8 -1 973.70 80.79 0 8 -1 1071.79 83.39 0 8 -1 892.81 76.69 0 8 -1 1020.90 84.89 0 -8 1 1050.29 59.09 0 -8 1 1148.19 83.99 0 -8 1 936.41 78.99 0 -8 1 1146.29 86.69 0 -8 1 995.00 81.09 -1 7 -1 552.24 74.19 -1 7 -1 700.73 61.39 -1 7 -1 663.73 64.69 -1 7 -1 565.44 73.69 1 -7 1 564.24 68.19 1 -7 1 635.84 76.49 1 -7 1 574.34 44.90 1 -7 1 549.45 56.39 1 -7 1 611.14 59.29 -2 6 -1 1043.70 71.29 -2 6 -1 1000.60 74.39 -2 6 -1 908.61 71.89 -2 6 -1 937.21 66.49 2 -6 1 833.62 62.09 2 -6 1 819.82 57.09 2 -6 1 1017.20 74.99 2 -6 1 840.42 69.49 2 -6 1 921.91 68.79 2 -6 1 920.51 68.19 -3 5 -1 -11.70 13.10 -3 5 -1 -11.00 24.30 -3 5 -1 16.90 26.00 -3 5 -1 -5.30 24.40 3 -5 1 11.40 15.50 3 -5 1 15.60 23.40 3 -5 1 27.70 21.30 3 -5 1 6.40 18.80 3 -5 1 9.70 24.60 -4 4 -1 1212.68 72.19 -4 4 -1 1244.18 60.49 -4 4 -1 1397.26 75.89 -4 4 -1 1424.46 82.79 4 -4 1 1219.28 59.89 4 -4 1 1268.67 71.59 4 -4 1 1315.47 76.89 4 -4 1 1369.56 76.09 4 -4 1 1317.07 74.49 -5 3 -1 932.71 57.29 -5 3 -1 917.01 57.69 -5 3 -1 882.51 41.80 -5 3 -1 883.31 62.69 -5 3 -1 927.11 47.80 5 -3 1 871.31 42.00 5 -3 1 859.31 60.19 5 -3 1 965.30 62.89 5 -3 1 907.61 54.89 5 -3 1 949.21 58.39 -6 2 -1 134.89 27.70 -6 2 -1 143.29 31.70 -6 2 -1 144.79 22.20 6 -2 1 141.59 21.90 6 -2 1 119.09 31.30 6 -2 1 170.38 28.90 6 -2 1 137.29 27.70 6 -2 1 145.79 18.20 -7 1 -1 40.50 17.80 -7 1 -1 20.10 14.70 -7 1 -1 37.10 22.30 -7 1 -1 52.59 18.90 7 -1 1 48.80 17.70 7 -1 1 48.00 17.30 7 -1 1 18.10 23.00 7 -1 1 40.40 16.30 -8 0 -1 12.80 13.80 -8 0 -1 -9.40 16.60 -8 0 -1 -5.70 9.70 -8 0 -1 6.80 11.60 8 0 1 -6.80 6.90 8 0 1 -6.80 8.40 8 0 1 8.60 17.80 8 0 1 3.50 10.90 8 0 1 -3.40 12.10 -9 -1 -1 124.69 9.40 -9 -1 -1 151.48 10.50 9 1 1 135.69 10.50 9 1 1 164.18 11.00 9 1 1 166.18 25.20 9 1 1 139.39 35.20 9 1 1 144.69 27.70 9 1 1 124.89 32.00 10 2 1 238.18 35.50 10 2 1 184.58 41.00 10 2 1 161.38 33.30 10 2 1 184.78 32.60 10 2 1 213.58 37.80 11 3 1 28.10 18.30 11 3 1 30.30 20.20 11 3 1 -8.10 12.90 11 3 1 -9.20 14.20 11 3 1 18.50 18.60 12 4 1 35.40 25.70 12 4 1 -1.50 20.60 12 4 1 13.80 21.50 12 4 1 5.00 16.40 12 4 1 38.60 22.30 13 5 1 140.69 41.70 13 5 1 105.69 28.10 13 5 1 217.08 49.50 13 5 1 135.49 43.20 13 5 1 111.99 30.50 14 6 1 -9.90 19.90 14 6 1 34.00 20.10 14 6 1 29.10 26.30 14 6 1 -22.90 26.30 14 6 1 21.50 18.00 15 7 1 5.20 33.30 15 7 1 36.40 27.80 15 7 1 -42.80 21.90 15 7 1 -18.90 16.20 15 7 1 4.00 16.20 6 12 -2 -28.60 31.60 6 12 -2 -20.10 25.50 6 12 -2 -7.70 26.40 6 12 -2 44.90 34.10 -6 -12 2 -65.79 19.70 -6 -12 2 12.00 20.70 -6 -12 2 -28.10 25.60 -6 -12 2 21.20 32.20 5 11 -2 -4.50 24.70 5 11 -2 3.50 30.60 5 11 -2 -23.30 17.00 5 11 -2 2.70 26.20 -5 -11 2 -16.20 22.20 -5 -11 2 -6.40 32.50 -5 -11 2 60.79 35.70 -5 -11 2 35.40 33.70 4 10 -2 28.60 34.20 4 10 -2 -11.50 19.60 4 10 -2 41.70 30.20 4 10 -2 58.19 32.00 -4 -10 2 22.70 24.70 -4 -10 2 38.00 21.40 -4 -10 2 60.09 32.50 -4 -10 2 104.09 38.50 3 9 -2 533.55 74.09 3 9 -2 563.64 76.89 3 9 -2 609.94 80.09 3 9 -2 623.74 80.69 -3 -9 2 430.76 68.39 -3 -9 2 623.04 77.19 -3 -9 2 565.64 72.09 -3 -9 2 383.56 58.79 2 8 -2 56.59 31.00 2 8 -2 69.19 35.20 2 8 -2 50.69 30.60 2 8 -2 61.59 32.80 -2 -8 2 37.80 29.80 -2 -8 2 -0.80 26.10 -2 -8 2 29.00 27.00 -2 -8 2 50.79 14.20 -2 -8 2 56.29 27.40 1 7 -2 35.20 25.10 1 7 -2 52.69 26.30 1 7 -2 28.70 18.00 1 7 -2 36.10 26.20 -1 -7 2 6.00 15.70 -1 -7 2 -4.60 20.00 -1 -7 2 -2.90 17.40 -1 -7 2 28.10 12.00 -1 -7 2 13.30 26.70 0 6 -2 253.87 46.20 0 6 -2 241.18 43.50 0 6 -2 243.18 49.40 0 6 -2 297.57 43.20 0 -6 2 318.57 50.09 0 -6 2 270.87 42.30 0 -6 2 285.77 29.80 0 -6 2 313.67 52.19 0 -6 2 216.58 37.80 0 -6 2 226.18 42.60 -1 5 -2 2019.00 93.79 -1 5 -2 1990.90 94.79 -1 5 -2 2002.50 95.89 -1 5 -2 2009.80 88.69 1 -5 2 1902.41 94.29 1 -5 2 1957.70 84.39 1 -5 2 2151.28 99.19 1 -5 2 1929.51 77.29 1 -5 2 1950.60 93.49 1 -5 2 2097.59 97.39 -2 4 -2 1440.96 75.69 -2 4 -2 1408.66 76.29 -2 4 -2 1542.95 91.09 -2 4 -2 1433.16 65.19 2 -4 2 1602.14 80.19 2 -4 2 1454.65 63.59 2 -4 2 1448.66 73.59 2 -4 2 1602.74 78.99 2 -4 2 1424.36 73.59 -3 3 -2 171.18 25.30 -3 3 -2 215.88 36.00 -3 3 -2 220.38 37.70 -3 3 -2 168.08 22.30 -3 3 -2 194.88 35.00 3 -3 2 173.28 32.20 3 -3 2 156.78 21.20 3 -3 2 191.18 34.60 -4 2 -2 452.65 21.20 -4 2 -2 475.15 42.80 -4 2 -2 472.65 37.40 -4 2 -2 424.06 35.90 -4 2 -2 469.15 35.10 4 -2 2 444.86 43.00 4 -2 2 489.25 34.50 4 -2 2 491.15 37.80 4 -2 2 448.66 21.20 4 -2 2 389.86 35.20 -5 1 -2 827.92 45.10 -5 1 -2 738.63 51.89 -5 1 -2 841.72 42.60 -5 1 -2 842.42 42.30 5 -1 2 811.22 43.50 5 -1 2 815.52 21.00 5 -1 2 876.81 46.40 5 -1 2 728.13 52.19 -6 0 -2 40.90 23.60 -6 0 -2 13.70 12.90 -6 0 -2 14.90 12.90 -6 0 -2 19.90 14.50 6 0 2 28.10 17.70 6 0 2 -6.60 12.20 6 0 2 17.80 15.70 6 0 2 13.30 12.20 6 0 2 8.50 8.40 -7 -1 -2 21.40 18.40 -7 -1 -2 4.30 10.30 -7 -1 -2 7.90 10.60 7 1 2 18.60 11.10 7 1 2 7.20 11.10 7 1 2 15.20 18.10 7 1 2 6.40 10.00 7 1 2 16.60 21.20 -8 -2 -2 204.58 14.40 8 2 2 229.68 30.00 8 2 2 183.88 36.70 8 2 2 250.07 22.60 8 2 2 216.98 15.40 8 2 2 264.67 35.60 8 2 2 234.38 38.10 -9 -3 -2 501.85 18.10 9 3 2 444.26 18.40 9 3 2 519.15 45.20 9 3 2 341.77 48.50 9 3 2 447.26 18.40 9 3 2 528.35 62.69 10 4 2 335.17 14.80 10 4 2 331.47 14.90 10 4 2 316.17 53.79 10 4 2 354.86 54.89 10 4 2 361.66 35.70 11 5 2 8.60 4.70 11 5 2 9.60 11.70 11 5 2 -3.80 14.10 11 5 2 0.80 4.50 11 5 2 -14.60 14.70 11 5 2 -14.10 19.10 12 6 2 24.70 19.50 12 6 2 18.70 24.40 12 6 2 -6.50 10.00 12 6 2 22.70 32.70 13 7 2 -25.90 13.10 13 7 2 5.60 23.70 13 7 2 -24.20 24.90 13 7 2 37.00 18.40 14 8 2 42.20 19.50 14 8 2 5.40 38.30 14 8 2 0.00 32.00 14 8 2 34.30 16.50 14 8 2 34.60 16.60 8 12 -3 41.90 36.30 8 12 -3 70.89 36.40 8 12 -3 70.69 35.90 8 12 -3 22.70 31.70 -8 -12 3 68.39 39.40 -8 -12 3 77.79 41.40 7 11 -3 31.90 26.30 7 11 -3 -7.60 24.70 7 11 -3 22.90 31.50 7 11 -3 0.90 25.20 7 11 -3 -19.30 26.90 -7 -11 3 -20.20 26.90 -7 -11 3 7.00 20.70 -7 -11 3 3.10 29.40 6 10 -3 48.40 31.50 6 10 -3 66.09 38.70 6 10 -3 -4.50 23.70 6 10 -3 39.70 28.50 6 10 -3 29.20 36.30 -6 -10 3 22.40 28.60 -6 -10 3 28.20 31.80 -6 -10 3 3.40 21.30 -6 -10 3 -30.40 16.50 5 9 -3 4.50 21.70 5 9 -3 -0.30 26.50 5 9 -3 5.20 26.90 5 9 -3 31.10 27.80 -5 -9 3 -4.10 17.20 -5 -9 3 14.60 24.90 -5 -9 3 51.89 27.80 4 8 -3 313.57 52.99 4 8 -3 564.94 72.79 4 8 -3 533.45 70.19 4 8 -3 357.56 57.49 4 8 -3 452.65 68.39 -4 -8 3 382.46 59.19 -4 -8 3 457.45 65.69 -4 -8 3 511.15 67.89 -4 -8 3 370.06 53.89 3 7 -3 164.58 39.50 3 7 -3 200.38 45.90 3 7 -3 179.78 41.20 3 7 -3 182.78 39.20 3 7 -3 168.58 39.80 -3 -7 3 163.58 38.80 -3 -7 3 172.28 39.00 -3 -7 3 234.08 45.20 -3 -7 3 154.58 39.00 -3 -7 3 175.28 15.30 2 6 -3 215.98 43.10 2 6 -3 371.56 53.39 2 6 -3 283.07 46.10 2 6 -3 367.26 52.69 2 6 -3 406.36 53.59 -2 -6 3 350.26 51.89 -2 -6 3 296.57 24.50 -2 -6 3 394.36 55.69 -2 -6 3 346.17 49.90 -2 -6 3 312.07 47.90 1 5 -3 46.20 23.90 1 5 -3 50.89 26.00 1 5 -3 104.39 29.30 1 5 -3 59.19 26.50 1 5 -3 84.09 28.30 -1 -5 3 32.40 19.60 -1 -5 3 73.29 24.90 -1 -5 3 83.29 27.00 -1 -5 3 56.39 26.60 -1 -5 3 64.79 21.80 0 4 -3 2001.70 88.99 0 4 -3 2139.89 89.49 0 4 -3 2166.18 83.49 0 4 -3 2066.89 90.99 0 4 -3 2151.68 91.99 0 -4 3 2252.57 94.99 0 -4 3 2119.69 89.69 0 -4 3 2113.99 86.29 0 -4 3 2188.38 94.59 0 -4 3 2281.07 108.19 -1 3 -3 296.77 34.00 -1 3 -3 359.46 41.50 -1 3 -3 288.27 27.00 -1 3 -3 274.57 37.30 -1 3 -3 314.07 39.50 1 -3 3 326.77 40.00 1 -3 3 304.57 36.60 1 -3 3 307.97 26.40 1 -3 3 316.47 39.40 -2 2 -3 761.12 46.10 -2 2 -3 754.62 45.00 -2 2 -3 825.42 32.30 -2 2 -3 820.62 49.70 -2 2 -3 818.12 47.60 2 -2 3 916.71 51.59 2 -2 3 788.42 48.60 2 -2 3 757.12 46.90 -3 1 -3 1394.96 56.39 -3 1 -3 1465.25 61.79 -3 1 -3 1534.05 65.99 3 -1 3 1503.75 58.39 3 -1 3 1505.55 61.69 3 -1 3 1424.56 65.89 -4 0 -3 -6.40 12.50 -4 0 -3 3.80 5.30 -4 0 -3 -7.00 8.20 -4 0 -3 0.70 12.60 4 0 3 -6.40 4.70 4 0 3 10.00 14.60 4 0 3 -1.20 15.80 4 0 3 -3.50 14.00 4 0 3 5.70 11.70 -5 -1 -3 2328.07 68.49 -5 -1 -3 2279.67 67.49 -5 -1 -3 2337.47 68.29 -5 -1 -3 2350.66 89.09 5 1 3 2261.47 68.19 5 1 3 2334.67 68.09 5 1 3 2459.65 91.99 5 1 3 2405.36 93.49 5 1 3 2301.87 69.89 -6 -2 -3 128.69 19.30 -6 -2 -3 133.69 20.40 -6 -2 -3 159.98 32.20 -6 -2 -3 94.19 20.60 6 2 3 131.19 20.00 6 2 3 135.39 26.80 6 2 3 127.29 29.00 6 2 3 131.59 20.40 6 2 3 131.89 17.90 -7 -3 -3 4.70 11.30 -7 -3 -3 26.30 13.40 -7 -3 -3 2.60 9.60 7 3 3 10.20 10.60 7 3 3 13.80 10.50 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64.69 -6 4 -18 147.69 62.19 -6 4 -18 49.50 49.50 6 -4 18 202.08 62.59 6 -4 18 151.68 60.89 6 -4 18 56.29 47.50 6 -4 18 34.50 33.80 -2 6 -19 18.90 51.79 -2 6 -19 1.20 37.80 -2 6 -19 -28.20 18.70 -2 6 -19 -64.19 33.20 2 -6 19 -45.10 26.40 2 -6 19 -18.80 40.80 2 -6 19 44.60 34.50 2 -6 19 -9.70 41.10 -3 5 -19 40.80 24.50 -3 5 -19 63.59 47.20 -3 5 -19 19.90 42.80 -3 5 -19 82.59 49.00 3 -5 19 5.70 35.90 3 -5 19 -33.20 33.10 3 -5 19 121.09 50.49 3 -5 19 -20.40 34.40 -4 4 -19 16.00 19.60 -4 4 -19 147.89 63.49 -4 4 -19 58.09 23.60 -4 4 -19 106.49 46.00 -4 4 -19 -25.10 33.00 4 -4 19 -3.00 39.90 4 -4 19 59.39 39.90 4 -4 19 73.69 36.20 4 -4 19 9.70 32.50 -5 3 -19 29.80 40.40 -5 3 -19 117.39 48.30 -5 3 -19 38.50 45.70 -5 3 -19 41.90 17.70 5 -3 19 47.40 36.60 5 -3 19 70.49 44.60 5 -3 19 78.99 50.19 5 -3 19 35.80 25.70 0 6 -20 -16.70 22.60 0 6 -20 44.20 46.20 0 6 -20 59.49 53.39 0 6 -20 -47.80 36.40 0 -6 20 -12.80 31.90 0 -6 20 -16.30 32.90 0 -6 20 -24.60 49.20 0 -6 20 -53.89 42.00 0 -6 20 7.00 31.90 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21 -30.80 40.30 0 -4 21 -13.30 30.00 0 -4 21 -24.70 32.80 0 -4 21 -77.59 29.90 0 -4 21 79.29 43.00 -1 3 -21 -12.90 29.60 -1 3 -21 -38.80 21.50 -1 3 -21 -35.00 24.90 -1 3 -21 -79.29 35.60 1 -3 21 -11.50 27.80 1 -3 21 -47.60 18.10 1 -3 21 7.50 25.60 1 -3 21 -43.60 19.80 1 -3 21 -2.30 27.80 -2 2 -21 -7.50 30.10 -2 2 -21 -8.90 39.50 -2 2 -21 -43.90 20.80 -2 2 -21 16.90 22.70 2 -2 21 -18.60 24.40 2 -2 21 -12.40 30.80 2 -2 21 -34.50 30.00 2 -2 21 -21.60 38.60 2 -2 21 -45.30 18.50 -3 1 -21 -15.20 38.30 -3 1 -21 -8.70 7.10 -3 1 -21 11.80 23.90 3 -1 21 55.89 41.10 3 -1 21 -95.89 31.30 3 -1 21 6.00 23.90 3 -1 21 -4.90 36.60 3 -1 21 44.20 35.70 3 -1 21 9.70 35.70 2 4 -22 75.59 58.09 2 4 -22 241.58 62.69 -2 -4 22 242.28 61.79 -2 -4 22 209.88 61.19 -2 -4 22 156.48 57.89 -2 -4 22 155.28 43.40 -2 -4 22 298.17 75.99 1 3 -22 -39.50 23.10 1 3 -22 8.10 29.00 1 3 -22 16.40 39.10 1 3 -22 -12.40 42.00 -1 -3 22 -85.29 27.70 -1 -3 22 0.00 39.20 -1 -3 22 38.30 33.40 -1 -3 22 -29.10 30.50 0 2 -22 -1.10 27.80 0 2 -22 -20.80 31.10 0 2 -22 -21.80 30.60 0 2 -22 -0.60 20.20 0 -2 22 27.90 37.00 0 -2 22 36.40 41.60 0 -2 22 19.70 32.40 0 -2 22 -49.90 33.20 0 -2 22 53.69 33.00 -1 1 -22 20.50 29.80 -1 1 -22 -28.90 20.90 -1 1 -22 -20.90 26.90 1 -1 22 82.09 52.89 1 -1 22 66.29 37.40 1 -1 22 -39.90 32.40 1 -1 22 -34.60 39.10 1 -1 22 -78.99 28.20 1 -1 22 4.70 31.10 3 3 -23 70.19 35.10 3 3 -23 163.38 56.29 3 3 -23 83.59 50.39 3 3 -23 100.39 41.30 -3 -3 23 194.08 53.99 -3 -3 23 212.58 72.19 -3 -3 23 178.08 64.49 -3 -3 23 187.48 68.69 -3 -3 23 158.28 49.70 2 2 -23 -9.70 34.60 2 2 -23 42.30 54.19 2 2 -23 -18.40 21.60 2 2 -23 33.70 29.00 2 2 -23 15.60 36.10 -2 -2 23 -26.40 33.80 -2 -2 23 34.30 39.40 -2 -2 23 69.29 51.69 -2 -2 23 71.79 53.89 -2 -2 23 54.79 35.40 -2 -2 23 26.10 29.60 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 53666 _olex2_submission_special_instructions 'No special instructions were received'