# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_complex_123k _database_code_depnum_ccdc_archive 'CCDC 1835730' _audit_update_record ; 2019-07-29 deposited with the CCDC. 2020-05-27 downloaded from the CCDC. ; _publcif_datablock.id {06dd0d42-84c7-48a6-bc60-1890e8396b5c} # publcif _publ_body_element loop end _audit_creation_date 2019-07-26 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number 2014/7 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '2(C36 H34 Fe N4 O6 S6), 0.5(C2 H4 Cl4)' _chemical_formula_sum 'C73 H70 Cl2 Fe2 N8 O12 S12' _chemical_formula_weight 1818.69 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0148 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe -0.2784 2.5795 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0253 0.0136 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0412 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.2924 0.4247 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3294 0.5404 '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 11.3618(9) _cell_length_b 12.1577(10) _cell_length_c 18.2103(14) _cell_angle_alpha 98.637(3) _cell_angle_beta 99.864(3) _cell_angle_gamma 113.651(3) _cell_volume 2202.3(3) _cell_formula_units_Z 1 _cell_measurement_reflns_used 3768 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 54.17 _cell_measurement_theta_min 3.71 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 4.191 _exptl_absorpt_correction_T_max 0.7513 _exptl_absorpt_correction_T_min 0.5516 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1820 before and 0.0770 after correction. The Ratio of minimum to maximum transmission is 0.7342. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 938 _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0784 _diffrn_reflns_av_unetI/netI 0.1066 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 20722 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 51.238 _diffrn_reflns_theta_max 51.238 _diffrn_reflns_theta_min 2.208 _diffrn_ambient_temperature 123.01 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type GaK\a _diffrn_radiation_wavelength 1.34139 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4591 _reflns_number_total 7221 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 0.869 _refine_diff_density_min -0.473 _refine_diff_density_rms 0.077 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 643 _refine_ls_number_reflns 7221 _refine_ls_number_restraints 665 _refine_ls_R_factor_all 0.1106 _refine_ls_R_factor_gt 0.0654 _refine_ls_restrained_S_all 1.041 _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^)+(0.0912P)^2^+1.1403P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1690 _refine_ls_wR_factor_ref 0.1932 _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 C27-C28 1.54 with sigma of 0.01 C18-C19 = C18'-C19' 1.54 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 4. Same fragment restrains {S4, S2, S1, S3, C3, C4, C5, C6, C1', C2} sigma for 1-2: 0.01, 1-3: 0.04 as {S4', S2', S1', S3', C3', C4', C5', C6, C1, C2'} {O6, C18, C19} sigma for 1-2: 0.02, 1-3: 0.04 as {O6', C18', C19'} {O6', C18', C19'} sigma for 1-2: 0.02, 1-3: 0.04 as {O5, C27, C28} 5. Others Sof(O6)=1-FVAR(1) Sof(C18)=Sof(H18C)=Sof(H18D)=Sof(C19)=Sof(H19D)=Sof(H19E)=Sof(H19F)=0.5*(1- FVAR(2)) Sof(C18')=Sof(H18A)=Sof(H18B)=Sof(C19')=Sof(H19A)=Sof(H19B)=Sof(H19C)=0.5* FVAR(2) Sof(O6')=FVAR(1) Sof(S2)=Sof(S1)=Sof(S4)=Sof(S3)=Sof(C2)=Sof(C5)=Sof(C4)=Sof(C1')=Sof(H1'A)= Sof(H1'B)=Sof(H1'C)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=1-FVAR(2) Sof(S4')=Sof(S2')=Sof(S1')=Sof(S3')=Sof(C3')=Sof(H3'A)=Sof(H3'B)=Sof(H3'C)= Sof(C4')=Sof(C5')=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C2')=FVAR(2) Fixed Sof: Cl1(0.5) Cl2(0.5) C27(0.5) H27A(0.5) H27B(0.5) C28(0.5) H28A(0.5) H28B(0.5) H28C(0.5) C29(0.5) H29A(0.5) H29B(0.5) 6.a Secondary CH2 refined with riding coordinates: C18'(H18A,H18B), C27(H27A,H27B), C18(H18C,H18D), C29(H29A,H29B), C25(H25A,H25B) 6.b Aromatic/amide H refined with riding coordinates: C37(H37), C33(H33), C31(H31), C39(H39), C11(H11), C34(H34), C13(H13), C36(H36), C38(H38), C20(H20), C30(H30), C8(H8) 6.c Idealised Me refined as rotating group: C3'(H3'A,H3'B,H3'C), C1(H1A,H1B,H1C), C19'(H19A,H19B,H19C), C28(H28A,H28B, H28C), C26(H26A,H26B,H26C), C23(H23A,H23B,H23C), C1'(H1'A,H1'B,H1'C), C3(H3A, H3B,H3C), C19(H19D,H19E,H19F), 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 Fe1 Fe 0.22338(7) 0.77298(6) 0.29430(4) 0.0375(2) Uani 1 1 d . U . . . Cl1 Cl 0.0990(5) 0.2878(3) 0.4774(2) 0.0891(12) Uani 0.5 1 d . U P A 2 Cl2 Cl 0.0542(4) 0.0312(3) 0.4614(2) 0.0907(12) Uani 0.5 1 d . U P A 2 S1 S 0.307(3) 0.5367(18) 0.9700(11) 0.089(4) Uani 0.170(8) 1 d D U P B 2 S2 S 0.434(2) 0.8411(13) 1.0309(6) 0.081(4) Uani 0.170(8) 1 d D U P B 2 S3 S 0.241(3) 0.5697(14) 0.8075(9) 0.065(4) Uani 0.170(8) 1 d D U P B 2 S4 S 0.3570(15) 0.8401(12) 0.8644(6) 0.053(3) Uani 0.170(8) 1 d D U P B 2 S5 S 0.27403(16) 0.87393(12) 0.68556(8) 0.0553(4) Uani 1 1 d . U . . . S6 S 0.16285(15) 0.60070(12) 0.63678(7) 0.0491(4) Uani 1 1 d . U . . . S1' S 0.2780(5) 0.5681(3) 0.97877(18) 0.0793(11) Uani 0.830(8) 1 d D U P B 1 S2' S 0.3599(4) 0.8651(2) 1.03131(11) 0.0699(11) Uani 0.830(8) 1 d D U P B 1 S3' S 0.2172(4) 0.5902(3) 0.81487(18) 0.0563(10) Uani 0.830(8) 1 d D U P B 1 S4' S 0.3054(4) 0.8615(2) 0.86321(13) 0.0610(9) Uani 0.830(8) 1 d D U P B 1 O1 O 0.2796(3) 0.9200(3) 0.25122(17) 0.0369(8) Uani 1 1 d . U . . . O2 O 0.1472(4) 0.6342(4) 0.2003(2) 0.0514(10) Uani 1 1 d . U . . . O3 O 0.4815(4) 1.2930(3) 0.3567(2) 0.0576(10) Uani 1 1 d . U . . . O4 O 0.4594(4) 1.2547(3) 0.4705(2) 0.0550(11) Uani 1 1 d . U . . . O5 O 0.0919(6) 0.2871(4) 0.3040(3) 0.0902(15) Uani 1 1 d D U . . . O6 O 0.0925(12) 0.2582(7) 0.1873(6) 0.078(3) Uani 0.587(14) 1 d D U P C 3 O6' O 0.0252(19) 0.2784(11) 0.1596(9) 0.088(4) Uani 0.413(14) 1 d D U P C 2 N1 N 0.2918(4) 0.8863(3) 0.4000(2) 0.0304(9) Uani 1 1 d . U . . . N2 N 0.1895(4) 0.6454(3) 0.3569(2) 0.0316(9) Uani 1 1 d . U . . . N3 N 0.4125(4) 0.7803(4) 0.2934(3) 0.0475(11) Uani 1 1 d . U . . . N4 N 1.0347(5) 0.7739(4) 0.2872(3) 0.0480(11) Uani 1 1 d . U . . . C1 C 0.1890(16) 0.4137(11) 0.9182(8) 0.090(4) Uani 0.830(8) 1 d D U P B 1 H1A H 0.2434 0.3984 0.8853 0.135 Uiso 0.830(8) 1 calc GR . P B 1 H1B H 0.1055 0.4046 0.8861 0.135 Uiso 0.830(8) 1 calc GR . P B 1 H1C H 0.1697 0.3538 0.9502 0.135 Uiso 0.830(8) 1 calc GR . P B 1 C1' C 0.161(8) 0.394(4) 0.925(4) 0.089(9) Uani 0.170(8) 1 d D U P B 2 H1'A H 0.1491 0.3377 0.9593 0.134 Uiso 0.170(8) 1 calc GR . P B 2 H1'B H 0.1698 0.3564 0.8765 0.134 Uiso 0.170(8) 1 calc GR . P B 2 H1'C H 0.0828 0.4116 0.9155 0.134 Uiso 0.170(8) 1 calc GR . P B 2 C2 C 0.304(5) 0.6316(17) 0.9073(11) 0.070(3) Uani 0.170(8) 1 d D U P B 2 C2' C 0.2761(9) 0.6594(7) 0.9137(4) 0.061(2) Uani 0.830(8) 1 d D U P B 1 C3 C 0.282(4) 0.841(5) 1.052(3) 0.081(9) Uani 0.170(8) 1 d D U P B 2 H3A H 0.2205 0.7564 1.0515 0.121 Uiso 0.170(8) 1 calc GR . P B 2 H3B H 0.2395 0.8695 1.0122 0.121 Uiso 0.170(8) 1 calc GR . P B 2 H3C H 0.3036 0.8958 1.1021 0.121 Uiso 0.170(8) 1 calc GR . P B 2 C3' C 0.1966(10) 0.8161(7) 1.0518(4) 0.071(3) Uani 0.830(8) 1 d D U P B 1 H3'A H 0.2076 0.8510 1.1060 0.106 Uiso 0.830(8) 1 calc GR . P B 1 H3'B H 0.1518 0.7255 1.0408 0.106 Uiso 0.830(8) 1 calc GR . P B 1 H3'C H 0.1429 0.8454 1.0194 0.106 Uiso 0.830(8) 1 calc GR . P B 1 C4 C 0.365(4) 0.7564(17) 0.9341(8) 0.065(4) Uani 0.170(8) 1 d D U P B 2 C4' C 0.3122(9) 0.7820(7) 0.9354(4) 0.0621(19) Uani 0.830(8) 1 d D U P B 1 C5 C 0.269(7) 0.7127(16) 0.7829(9) 0.057(4) Uani 0.170(8) 1 d D U P B 2 C5' C 0.2483(11) 0.7297(6) 0.7868(3) 0.054(2) Uani 0.830(8) 1 d D U P B 1 C6 C 0.2339(6) 0.7336(5) 0.7132(3) 0.0522(14) Uani 1 1 d D U . . . C7 C 0.2046(5) 0.6817(4) 0.5656(3) 0.0401(12) Uani 1 1 d . U . . . C8 C 0.1807(5) 0.6235(4) 0.4900(3) 0.0367(12) Uani 1 1 d . U . . . H8 H 0.1430 0.5358 0.4744 0.044 Uiso 1 1 calc R . . . . C9 C 0.2123(5) 0.6943(4) 0.4367(3) 0.0319(10) Uani 1 1 d . U . . . C10 C 0.2670(5) 0.8243(4) 0.4598(3) 0.0329(11) Uani 1 1 d . U . . . C11 C 0.2879(5) 0.8813(4) 0.5360(3) 0.0383(12) Uani 1 1 d . U . . . H11 H 0.3233 0.9688 0.5516 0.046 Uiso 1 1 calc R . . . . C12 C 0.2573(5) 0.8108(4) 0.5896(3) 0.0404(12) Uani 1 1 d . U . . . C13 C 0.1591(5) 0.5280(4) 0.3314(3) 0.0411(12) Uani 1 1 d . U . . . H13 H 0.1596 0.4816 0.3689 0.049 Uiso 1 1 calc R . . . . C14 C 0.1257(6) 0.4638(5) 0.2542(3) 0.0552(15) Uani 1 1 d . U . . . C15 C 0.1190(6) 0.5199(6) 0.1924(3) 0.0573(16) Uani 1 1 d . U . . . C16 C 0.0742(8) 0.4473(8) 0.1086(4) 0.102(3) Uani 1 1 d . U . . . H16A H -0.0062 0.3705 0.1011 0.153 Uiso 1 1 calc GR . . . . H16B H 0.1449 0.4275 0.0958 0.153 Uiso 1 1 calc GR . . . . H16C H 0.0552 0.4973 0.0751 0.153 Uiso 1 1 calc GR . . . . C17 C 0.0940(8) 0.3311(6) 0.2447(4) 0.0776(19) Uani 1 1 d . U . . . C18 C 0.054(3) 0.1277(14) 0.1677(13) 0.088(5) Uani 0.294(7) 1 d D U P C 3 H18A H -0.1123 0.1063 0.1135 0.099 Uiso 0.206(7) 1 calc R . P C 2 H18B H -0.0151 0.1219 0.1925 0.099 Uiso 0.206(7) 1 calc R . P C 2 C18' C -0.018(4) 0.1460(18) 0.143(2) 0.083(5) Uani 0.206(7) 1 d D U P C 2 H18'A H 0.0006 0.0995 0.2046 0.106 Uiso 0.294(7) 1 calc R . P C 3 H18'B H 0.1392 0.1252 0.1886 0.106 Uiso 0.294(7) 1 calc R . P C 3 C19 C -0.013(3) 0.012(2) 0.0996(14) 0.118(7) Uani 0.294(7) 1 d D U P C 3 H19A H -0.0136 -0.0598 0.1177 0.177 Uiso 0.294(7) 1 calc GR . P C 3 H19B H 0.0368 0.0259 0.0602 0.177 Uiso 0.294(7) 1 calc GR . P C 3 H19C H -0.1044 -0.0021 0.0778 0.177 Uiso 0.294(7) 1 calc GR . P C 3 C19' C 0.056(4) 0.089(3) 0.098(2) 0.087(7) Uani 0.206(7) 1 d D U P C 2 H19'A H -0.0073 0.0070 0.0657 0.131 Uiso 0.206(7) 1 calc GR . P C 2 H19'B H 0.1240 0.0798 0.1350 0.131 Uiso 0.206(7) 1 calc GR . P C 2 H19'C H 0.0988 0.1425 0.0665 0.131 Uiso 0.206(7) 1 calc GR . P C 2 C20 C 0.3508(5) 1.0073(4) 0.4162(3) 0.0359(11) Uani 1 1 d . U . . . H20 H 0.3777 1.0492 0.4690 0.043 Uiso 1 1 calc R . . . . C21 C 0.3789(5) 1.0828(4) 0.3625(3) 0.0355(11) Uani 1 1 d . U . . . C22 C 0.3454(5) 1.0360(5) 0.2827(3) 0.0402(12) Uani 1 1 d . U . . . C23 C 0.3806(7) 1.1147(5) 0.2266(3) 0.0655(18) Uani 1 1 d . U . . . H23A H 0.4770 1.1653 0.2402 0.098 Uiso 1 1 calc GR . . . . H23B H 0.3358 1.1688 0.2283 0.098 Uiso 1 1 calc GR . . . . H23C H 0.3520 1.0615 0.1747 0.098 Uiso 1 1 calc GR . . . . C24 C 0.4420(6) 1.2158(5) 0.4021(3) 0.0445(13) Uani 1 1 d . U . . . C25 C 0.5337(7) 1.4239(5) 0.3922(4) 0.0662(17) Uani 1 1 d . U . . . H25A H 0.5898 1.4423 0.4447 0.079 Uiso 1 1 calc R . . . . H25B H 0.5904 1.4727 0.3621 0.079 Uiso 1 1 calc R . . . . C26 C 0.4284(8) 1.4600(7) 0.3965(5) 0.088(2) Uani 1 1 d . U . . . H26A H 0.4666 1.5473 0.4240 0.132 Uiso 1 1 calc GR . . . . H26B H 0.3695 1.4088 0.4240 0.132 Uiso 1 1 calc GR . . . . H26C H 0.3775 1.4487 0.3445 0.132 Uiso 1 1 calc GR . . . . C27 C 0.0807(15) 0.1659(10) 0.3133(8) 0.075(3) Uani 0.5 1 d D U P D 1 H27A H 0.1522 0.1527 0.2949 0.090 Uiso 0.5 1 calc R . P D 1 H27B H -0.0050 0.1018 0.2792 0.090 Uiso 0.5 1 calc R . P D 1 C28 C 0.088(3) 0.144(2) 0.3951(9) 0.076(5) Uani 0.5 1 d D U P D 1 H28A H 0.1051 0.0713 0.3970 0.115 Uiso 0.5 1 calc GR . P D 1 H28B H 0.0043 0.1302 0.4082 0.115 Uiso 0.5 1 calc GR . P D 1 H28C H 0.1610 0.2168 0.4321 0.115 Uiso 0.5 1 calc GR . P D 1 C29 C 0.076(3) 0.158(2) 0.4144(13) 0.085(4) Uani 0.5 1 d . U P A 2 H29A H 0.1545 0.1761 0.3927 0.102 Uiso 0.5 1 calc R . P A 2 H29B H -0.0028 0.1326 0.3714 0.102 Uiso 0.5 1 calc R . P A 2 C30 C 0.4947(6) 0.7795(5) 0.3558(3) 0.0466(13) Uani 1 1 d . U . . . H30 H 0.4670 0.7773 0.4022 0.056 Uiso 1 1 calc R . . . . C31 C 0.6166(5) 0.7817(5) 0.3559(3) 0.0455(13) Uani 1 1 d . U . . . H31 H 0.6699 0.7795 0.4014 0.055 Uiso 1 1 calc R . . . . C32 C 0.6626(5) 0.7872(4) 0.2897(3) 0.0426(12) Uani 1 1 d . U . . . C33 C 0.5775(6) 0.7914(5) 0.2263(3) 0.0560(15) Uani 1 1 d . U . . . H33 H 0.6035 0.7968 0.1796 0.067 Uiso 1 1 calc R . . . . C34 C 0.4580(6) 0.7877(5) 0.2306(4) 0.0548(15) Uani 1 1 d . U . . . H34 H 0.4032 0.7905 0.1859 0.066 Uiso 1 1 calc R . . . . C35 C 0.7889(6) 0.7832(5) 0.2879(3) 0.0455(13) Uani 1 1 d . U . . . C36 C 0.8343(6) 0.7152(5) 0.3298(4) 0.0554(15) Uani 1 1 d . U . . . H36 H 0.7838 0.6711 0.3612 0.066 Uiso 1 1 calc R . . . . C37 C 0.9523(6) 0.7118(5) 0.3258(4) 0.0617(16) Uani 1 1 d . U . . . H37 H 0.9772 0.6605 0.3530 0.074 Uiso 1 1 calc R . . . . C38 C 0.9896(6) 0.8380(6) 0.2462(3) 0.0609(16) Uani 1 1 d . U . . . H38 H 1.0431 0.8819 0.2158 0.073 Uiso 1 1 calc R . . . . C39 C 0.8710(6) 0.8449(6) 0.2448(3) 0.0594(16) Uani 1 1 d . U . . . H39 H 0.8455 0.8922 0.2141 0.071 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0396(5) 0.0248(4) 0.0461(5) 0.0078(3) 0.0101(3) 0.0128(3) Cl1 0.136(3) 0.0535(19) 0.108(3) 0.0335(19) 0.069(3) 0.052(2) Cl2 0.123(3) 0.0424(17) 0.092(3) 0.0167(17) 0.009(2) 0.0297(19) S4' 0.092(2) 0.0383(11) 0.0275(10) 0.0031(8) 0.0140(12) 0.0060(11) S2' 0.093(3) 0.0530(12) 0.0295(11) 0.0020(8) 0.0067(12) 0.0042(13) S1' 0.133(3) 0.0509(16) 0.0372(13) 0.0147(11) 0.0198(13) 0.0232(14) S3' 0.081(2) 0.0404(12) 0.0285(12) 0.0063(9) 0.0175(11) 0.0076(10) C3' 0.096(7) 0.056(5) 0.034(4) -0.002(3) 0.012(5) 0.015(5) C4' 0.088(4) 0.049(3) 0.030(3) 0.005(2) 0.016(3) 0.011(3) C5' 0.075(4) 0.039(3) 0.028(3) 0.007(2) 0.016(3) 0.006(3) C6 0.064(3) 0.039(3) 0.032(3) 0.006(2) 0.016(2) 0.000(2) C1 0.147(9) 0.053(5) 0.062(6) 0.024(4) 0.042(6) 0.026(5) C2' 0.093(4) 0.047(3) 0.028(3) 0.012(2) 0.016(3) 0.014(3) S5 0.0779(11) 0.0357(7) 0.0306(8) 0.0022(6) 0.0182(7) 0.0040(7) S2 0.106(6) 0.067(5) 0.039(4) 0.006(4) 0.007(5) 0.013(5) S1 0.130(7) 0.068(6) 0.051(5) 0.021(5) 0.019(5) 0.023(6) S4 0.080(5) 0.046(4) 0.029(4) 0.007(3) 0.020(4) 0.022(4) S6 0.0665(10) 0.0350(7) 0.0290(7) 0.0095(5) 0.0115(6) 0.0056(6) S3 0.087(6) 0.059(5) 0.029(4) 0.012(4) 0.022(4) 0.008(5) O3 0.093(3) 0.0313(19) 0.049(2) 0.0191(16) 0.025(2) 0.0219(19) O6 0.126(6) 0.038(3) 0.070(5) -0.002(3) 0.044(4) 0.033(4) O6' 0.132(7) 0.041(5) 0.075(6) -0.009(4) 0.038(6) 0.024(5) C18' 0.131(8) 0.032(6) 0.081(7) 0.005(6) 0.039(7) 0.031(6) C19' 0.134(13) 0.023(10) 0.105(13) 0.003(10) 0.046(12) 0.035(10) O4 0.085(3) 0.0304(19) 0.037(2) 0.0068(16) 0.011(2) 0.0153(19) O2 0.044(2) 0.073(3) 0.035(2) 0.0144(18) 0.0105(16) 0.023(2) O5 0.132(4) 0.035(2) 0.118(4) 0.021(2) 0.072(3) 0.034(2) C27 0.111(6) 0.031(5) 0.103(6) 0.020(5) 0.054(5) 0.039(4) C28 0.098(8) 0.037(7) 0.109(10) 0.016(7) 0.048(8) 0.037(6) O1 0.043(2) 0.0365(18) 0.0264(17) 0.0040(14) 0.0060(14) 0.0149(15) N3 0.055(3) 0.028(2) 0.048(3) 0.0049(19) -0.008(2) 0.016(2) N2 0.036(2) 0.027(2) 0.029(2) 0.0031(16) 0.0061(17) 0.0124(17) N1 0.037(2) 0.0240(19) 0.030(2) 0.0083(16) 0.0114(17) 0.0119(17) N4 0.068(3) 0.028(2) 0.053(3) 0.0097(19) 0.032(2) 0.020(2) C37 0.071(4) 0.048(3) 0.092(4) 0.037(3) 0.040(3) 0.037(3) C26 0.102(6) 0.059(4) 0.091(5) 0.008(4) 0.000(4) 0.037(4) C22 0.051(3) 0.041(3) 0.032(3) 0.014(2) 0.012(2) 0.022(2) C33 0.056(4) 0.051(3) 0.052(3) 0.015(3) 0.004(3) 0.018(3) C2 0.101(5) 0.053(4) 0.034(4) 0.011(4) 0.018(4) 0.013(4) C24 0.058(3) 0.034(3) 0.042(3) 0.017(2) 0.012(2) 0.018(2) C31 0.050(3) 0.039(3) 0.042(3) 0.002(2) 0.002(2) 0.021(2) C35 0.054(3) 0.035(3) 0.046(3) 0.009(2) 0.012(2) 0.017(2) C5 0.079(5) 0.044(4) 0.028(4) 0.006(4) 0.019(4) 0.007(4) C39 0.054(4) 0.061(3) 0.054(3) 0.026(3) 0.004(3) 0.015(3) C18 0.131(9) 0.037(6) 0.087(8) 0.014(6) 0.035(8) 0.025(7) C4 0.094(5) 0.052(5) 0.030(5) 0.010(5) 0.014(5) 0.015(5) C23 0.103(5) 0.046(3) 0.040(3) 0.016(3) 0.015(3) 0.024(3) C29 0.120(7) 0.037(6) 0.101(6) 0.020(6) 0.032(6) 0.035(5) C25 0.098(5) 0.030(3) 0.068(4) 0.018(3) 0.024(3) 0.022(3) C10 0.038(3) 0.029(2) 0.027(2) 0.0061(19) 0.007(2) 0.011(2) C11 0.050(3) 0.024(2) 0.032(3) 0.000(2) 0.013(2) 0.008(2) C32 0.050(3) 0.032(2) 0.039(3) 0.006(2) 0.002(2) 0.017(2) C12 0.055(3) 0.033(2) 0.025(2) 0.0031(19) 0.013(2) 0.011(2) C34 0.057(4) 0.043(3) 0.050(3) 0.014(2) -0.008(3) 0.016(3) C13 0.054(3) 0.028(2) 0.039(3) 0.005(2) 0.020(2) 0.014(2) C36 0.065(4) 0.053(3) 0.073(4) 0.039(3) 0.037(3) 0.035(3) C14 0.072(4) 0.036(3) 0.043(3) -0.003(2) 0.032(3) 0.006(2) C38 0.061(4) 0.063(4) 0.043(3) 0.019(3) 0.014(3) 0.010(3) C15 0.047(3) 0.063(3) 0.038(3) -0.005(3) 0.013(3) 0.005(3) C1' 0.134(13) 0.059(12) 0.056(12) 0.003(11) 0.034(12) 0.023(11) C17 0.115(4) 0.037(3) 0.065(4) -0.007(3) 0.051(3) 0.013(3) C3 0.103(13) 0.063(11) 0.041(11) 0.003(10) 0.007(12) 0.010(12) C20 0.043(3) 0.029(2) 0.033(3) 0.005(2) 0.007(2) 0.016(2) C21 0.050(3) 0.026(2) 0.033(3) 0.0112(19) 0.015(2) 0.016(2) C19 0.155(13) 0.068(11) 0.115(12) 0.028(11) 0.051(11) 0.024(11) C7 0.049(3) 0.034(2) 0.028(3) 0.010(2) 0.009(2) 0.010(2) C30 0.052(3) 0.036(3) 0.044(3) 0.000(2) -0.002(3) 0.020(2) C8 0.045(3) 0.023(2) 0.034(3) 0.0058(19) 0.009(2) 0.008(2) C9 0.036(3) 0.030(2) 0.028(2) 0.0053(19) 0.007(2) 0.014(2) C16 0.084(5) 0.121(6) 0.030(4) -0.023(4) 0.017(4) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O2 1.995(4) . ? Fe1 O1 1.973(3) . ? Fe1 N3 2.117(5) . ? Fe1 N2 2.014(4) . ? Fe1 N1 2.009(4) . ? Fe1 N4 2.130(5) 1_455 ? Cl1 C29 1.71(2) . ? Cl2 Cl2 2.057(9) 2_556 ? Cl2 C29 1.82(2) . ? S4' C4' 1.753(7) . ? S4' C5' 1.764(6) . ? S2' C3' 1.831(9) . ? S2' C4' 1.753(7) . ? S1' C1 1.799(12) . ? S1' C2' 1.744(7) . ? S3' C5' 1.762(7) . ? S3' C2' 1.754(6) . ? C3' H3'A 0.9800 . ? C3' H3'B 0.9800 . ? C3' H3'C 0.9800 . ? C4' C2' 1.350(10) . ? C5' C6 1.332(8) . ? C6 S5 1.756(5) . ? C6 S6 1.759(5) . ? C6 C5 1.356(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? S5 C12 1.745(5) . ? S2 C4 1.766(11) . ? S2 C3 1.835(14) . ? S1 C2 1.747(11) . ? S1 C1' 1.798(15) . ? S4 C5 1.777(11) . ? S4 C4 1.753(12) . ? S6 C7 1.759(5) . ? S3 C2 1.760(11) . ? S3 C5 1.777(11) . ? O3 C24 1.339(6) . ? O3 C25 1.450(6) . ? O6 C18 1.433(15) . ? O6 C17 1.258(9) . ? O6' C18' 1.446(17) . ? O6' C17 1.518(17) . ? C18' H18A 0.9900 . ? C18' H18B 0.9900 . ? C18' C19' 1.545(9) . ? C19' H19A 0.9800 . ? C19' H19B 0.9800 . ? C19' H19C 0.9800 . ? O4 C24 1.216(6) . ? O2 C15 1.273(7) . ? O5 C27 1.466(10) . ? O5 C17 1.276(8) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.546(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? O1 C22 1.281(6) . ? N3 C34 1.334(7) . ? N3 C30 1.346(7) . ? N2 C13 1.312(6) . ? N2 C9 1.421(6) . ? N1 C10 1.419(6) . ? N1 C20 1.309(6) . ? N4 Fe1 2.130(5) 1_655 ? N4 C37 1.325(7) . ? N4 C38 1.339(7) . ? C37 H37 0.9500 . ? C37 C36 1.372(8) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 C25 1.441(9) . ? C22 C23 1.498(7) . ? C22 C21 1.402(7) . ? C33 H33 0.9500 . ? C33 C32 1.395(8) . ? C33 C34 1.357(8) . ? C2 C4 1.356(13) . ? C24 C21 1.480(7) . ? C31 H31 0.9500 . ? C31 C32 1.392(7) . ? C31 C30 1.375(7) . ? C35 C39 1.384(8) . ? C35 C32 1.461(8) . ? C35 C36 1.388(7) . ? C39 H39 0.9500 . ? C39 C38 1.379(9) . ? C18 H18C 0.9900 . ? C18 H18D 0.9900 . ? C18 C19 1.543(9) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C10 C11 1.388(6) . ? C10 C9 1.409(6) . ? C11 H11 0.9500 . ? C11 C12 1.391(6) . ? C12 C7 1.401(7) . ? C34 H34 0.9500 . ? C13 H13 0.9500 . ? C13 C14 1.407(7) . ? C36 H36 0.9500 . ? C14 C15 1.408(8) . ? C14 C17 1.480(8) . ? C38 H38 0.9500 . ? C15 C16 1.529(8) . ? C1' H1'A 0.9800 . ? C1' H1'B 0.9800 . ? C1' H1'C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C20 H20 0.9500 . ? C20 C21 1.430(6) . ? C19 H19D 0.9800 . ? C19 H19E 0.9800 . ? C19 H19F 0.9800 . ? C7 C8 1.376(7) . ? C30 H30 0.9500 . ? C8 H8 0.9500 . ? C8 C9 1.392(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 O2 Fe1 N3 87.96(16) . . ? O2 Fe1 N2 87.93(15) . . ? O2 Fe1 N1 168.80(15) . . ? O2 Fe1 N4 90.90(16) . 1_455 ? O1 Fe1 O2 102.32(14) . . ? O1 Fe1 N3 86.06(15) . . ? O1 Fe1 N2 169.21(14) . . ? O1 Fe1 N1 88.88(13) . . ? O1 Fe1 N4 89.34(15) . 1_455 ? N3 Fe1 N4 174.91(18) . 1_455 ? N2 Fe1 N3 90.98(16) . . ? N2 Fe1 N4 93.93(16) . 1_455 ? N1 Fe1 N3 92.45(16) . . ? N1 Fe1 N2 80.88(14) . . ? N1 Fe1 N4 89.63(16) . 1_455 ? C29 Cl2 Cl2 132.0(10) . 2_556 ? C4' S4' C5' 94.7(3) . . ? C4' S2' C3' 99.8(4) . . ? C2' S1' C1 102.5(4) . . ? C2' S3' C5' 95.1(3) . . ? S2' C3' H3'A 109.5 . . ? S2' C3' H3'B 109.5 . . ? S2' C3' H3'C 109.5 . . ? H3'A C3' H3'B 109.5 . . ? H3'A C3' H3'C 109.5 . . ? H3'B C3' H3'C 109.5 . . ? S2' C4' S4' 118.1(4) . . ? C2' C4' S4' 118.0(5) . . ? C2' C4' S2' 123.8(5) . . ? S3' C5' S4' 114.9(3) . . ? C6 C5' S4' 123.7(5) . . ? C6 C5' S3' 121.4(5) . . ? C5' C6 S5 121.5(5) . . ? C5' C6 S6 123.4(5) . . ? S5 C6 S6 114.9(3) . . ? C5 C6 S5 129.9(9) . . ? C5 C6 S6 114.2(9) . . ? S1' C1 H1A 109.5 . . ? S1' C1 H1B 109.5 . . ? S1' C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? S1' C2' S3' 119.6(4) . . ? C4' C2' S1' 123.3(5) . . ? C4' C2' S3' 117.0(5) . . ? C12 S5 C6 95.0(2) . . ? C4 S2 C3 97.5(16) . . ? C2 S1 C1' 103.7(19) . . ? C4 S4 C5 98.1(7) . . ? C7 S6 C6 95.2(2) . . ? C2 S3 C5 96.3(9) . . ? C24 O3 C25 116.1(4) . . ? C17 O6 C18 133.6(13) . . ? C18' O6' C17 108.1(19) . . ? O6' C18' H18A 107.4 . . ? O6' C18' H18B 107.4 . . ? O6' C18' C19' 119.9(19) . . ? H18A C18' H18B 106.9 . . ? C19' C18' H18A 107.4 . . ? C19' C18' H18B 107.4 . . ? C18' C19' H19A 109.5 . . ? C18' C19' H19B 109.5 . . ? C18' C19' H19C 109.5 . . ? H19A C19' H19B 109.5 . . ? H19A C19' H19C 109.5 . . ? H19B C19' H19C 109.5 . . ? C15 O2 Fe1 130.8(4) . . ? C17 O5 C27 130.3(7) . . ? O5 C27 H27A 108.0 . . ? O5 C27 H27B 108.0 . . ? O5 C27 C28 117.2(12) . . ? H27A C27 H27B 107.2 . . ? C28 C27 H27A 108.0 . . ? C28 C27 H27B 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C22 O1 Fe1 132.3(3) . . ? C34 N3 Fe1 121.6(4) . . ? C34 N3 C30 115.9(5) . . ? C30 N3 Fe1 122.5(4) . . ? C13 N2 Fe1 126.0(3) . . ? C13 N2 C9 119.7(4) . . ? C9 N2 Fe1 114.1(3) . . ? C10 N1 Fe1 114.2(3) . . ? C20 N1 Fe1 125.9(3) . . ? C20 N1 C10 119.8(4) . . ? C37 N4 Fe1 121.7(4) . 1_655 ? C37 N4 C38 113.9(5) . . ? C38 N4 Fe1 124.3(4) . 1_655 ? N4 C37 H37 117.1 . . ? N4 C37 C36 125.8(5) . . ? C36 C37 H37 117.1 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? O1 C22 C23 113.8(4) . . ? O1 C22 C21 122.1(4) . . ? C21 C22 C23 124.1(5) . . ? C32 C33 H33 119.7 . . ? C34 C33 H33 119.7 . . ? C34 C33 C32 120.7(6) . . ? S1 C2 S3 121.1(12) . . ? C4 C2 S1 120.0(13) . . ? C4 C2 S3 118.4(12) . . ? O3 C24 C21 114.6(5) . . ? O4 C24 O3 121.2(5) . . ? O4 C24 C21 124.2(5) . . ? C32 C31 H31 119.7 . . ? C30 C31 H31 119.7 . . ? C30 C31 C32 120.5(5) . . ? C39 C35 C32 123.3(5) . . ? C39 C35 C36 115.3(5) . . ? C36 C35 C32 121.4(5) . . ? C6 C5 S4 119.4(11) . . ? C6 C5 S3 128.9(12) . . ? S3 C5 S4 111.7(8) . . ? C35 C39 H39 119.8 . . ? C38 C39 C35 120.4(5) . . ? C38 C39 H39 119.8 . . ? O6 C18 H18C 101.3 . . ? O6 C18 H18D 101.3 . . ? O6 C18 C19 143(2) . . ? H18C C18 H18D 104.5 . . ? C19 C18 H18C 101.3 . . ? C19 C18 H18D 101.3 . . ? S4 C4 S2 117.3(10) . . ? C2 C4 S2 127.2(12) . . ? C2 C4 S4 115.1(11) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Cl1 C29 Cl2 111.1(12) . . ? Cl1 C29 H29A 109.4 . . ? Cl1 C29 H29B 109.4 . . ? Cl2 C29 H29A 109.4 . . ? Cl2 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? O3 C25 H25A 109.4 . . ? O3 C25 H25B 109.4 . . ? C26 C25 O3 111.4(6) . . ? C26 C25 H25A 109.4 . . ? C26 C25 H25B 109.4 . . ? H25A C25 H25B 108.0 . . ? C11 C10 N1 125.3(4) . . ? C11 C10 C9 119.6(4) . . ? C9 C10 N1 115.1(4) . . ? C10 C11 H11 119.8 . . ? C10 C11 C12 120.4(4) . . ? C12 C11 H11 119.8 . . ? C33 C32 C35 123.6(5) . . ? C31 C32 C33 115.3(6) . . ? C31 C32 C35 121.0(5) . . ? C11 C12 S5 123.5(4) . . ? C11 C12 C7 119.2(4) . . ? C7 C12 S5 117.3(4) . . ? N3 C34 C33 124.3(5) . . ? N3 C34 H34 117.8 . . ? C33 C34 H34 117.8 . . ? N2 C13 H13 116.6 . . ? N2 C13 C14 126.8(5) . . ? C14 C13 H13 116.6 . . ? C37 C36 C35 119.9(5) . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C13 C14 C15 122.9(5) . . ? C13 C14 C17 113.3(5) . . ? C15 C14 C17 123.7(5) . . ? N4 C38 C39 124.7(5) . . ? N4 C38 H38 117.7 . . ? C39 C38 H38 117.7 . . ? O2 C15 C14 124.0(5) . . ? O2 C15 C16 113.6(6) . . ? C14 C15 C16 122.4(6) . . ? S1 C1' H1'A 109.5 . . ? S1 C1' H1'B 109.5 . . ? S1 C1' H1'C 109.5 . . ? H1'A C1' H1'B 109.5 . . ? H1'A C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? O6 C17 O5 112.3(8) . . ? O6 C17 C14 127.6(7) . . ? O5 C17 O6' 135.0(7) . . ? O5 C17 C14 118.7(5) . . ? C14 C17 O6' 102.2(8) . . ? S2 C3 H3A 109.5 . . ? S2 C3 H3B 109.5 . . ? S2 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C20 H20 116.8 . . ? N1 C20 C21 126.4(4) . . ? C21 C20 H20 116.8 . . ? C22 C21 C24 125.1(4) . . ? C22 C21 C20 124.0(4) . . ? C20 C21 C24 110.8(4) . . ? C18 C19 H19D 109.5 . . ? C18 C19 H19E 109.5 . . ? C18 C19 H19F 109.5 . . ? H19D C19 H19E 109.5 . . ? H19D C19 H19F 109.5 . . ? H19E C19 H19F 109.5 . . ? C12 C7 S6 115.7(4) . . ? C8 C7 S6 123.0(4) . . ? C8 C7 C12 121.2(4) . . ? N3 C30 C31 123.3(6) . . ? N3 C30 H30 118.4 . . ? C31 C30 H30 118.4 . . ? C7 C8 H8 120.3 . . ? C7 C8 C9 119.4(4) . . ? C9 C8 H8 120.3 . . ? C10 C9 N2 114.9(4) . . ? C8 C9 N2 124.9(4) . . ? C8 C9 C10 120.2(4) . . ? 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 . . ? _shelx_res_file ; zjl_123k_0m_a_sq.res created by SHELXL-2014/7 TITL ZJL_123K_0m_a.res in P-1 REM Old TITL ZJL_123K_0m in P-1 REM SHELXT solution in P-1 REM R1 0.256, Rweak 0.033, Alpha 0.076, Orientation as input REM Formula found by SHELXT: C39 Fe N2 O7 S2' CELL 1.34139 11.3618 12.1577 18.2103 98.637 99.864 113.651 ZERR 1 0.0009 0.001 0.0014 0.003 0.003 0.003 LATT 1 SFAC C H Fe N O S Cl DISP C 0.0148 0.007 57.7477 DISP Cl 0.3294 0.5404 4086.1782 DISP Fe -0.2784 2.5795 18880.1977 DISP H -0 0 0.6481 DISP N 0.0253 0.0136 110.5121 DISP O 0.0412 0.025 193.9543 DISP S 0.2924 0.4247 3241.7632 UNIT 73 70 2 8 12 12 2 DFIX 1.54 0.01 C27 C28 DFIX 1.54 0.01 C18 C19 C18' C19' SIMU 0.01 0.02 2 L.S. 5 0 39 PLAN 20 TEMP -150.14 LIST 6 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.091200 1.140300 FVAR 0.27679 0.41278 0.83043 FE1 3 0.223377 0.772976 0.294296 11.00000 0.03960 0.02478 = 0.04611 0.00776 0.01011 0.01275 PART 2 CL1 7 0.099006 0.287804 0.477399 10.50000 0.13589 0.05352 = 0.10841 0.03353 0.06869 0.05173 CL2 7 0.054230 0.031174 0.461403 10.50000 0.12330 0.04242 = 0.09233 0.01670 0.00897 0.02974 SAME 0.01 0.04 S4 S2 S1 S3 C3 C4 C5 C6 C1' C2 PART 0 PART 1 S4' 6 0.305440 0.861500 0.863214 31.00000 0.09191 0.03829 = 0.02751 0.00306 0.01398 0.00598 S2' 6 0.359853 0.865060 1.031312 31.00000 0.09256 0.05300 = 0.02945 0.00196 0.00665 0.00423 S1' 6 0.277970 0.568090 0.978775 31.00000 0.13299 0.05089 = 0.03719 0.01475 0.01981 0.02320 S3' 6 0.217209 0.590196 0.814869 31.00000 0.08135 0.04036 = 0.02847 0.00631 0.01750 0.00761 C3' 1 0.196562 0.816051 1.051780 31.00000 0.09635 0.05604 = 0.03368 -0.00241 0.01203 0.01457 AFIX 137 H3'A 2 0.207646 0.851024 1.106016 31.00000 -1.50000 H3'B 2 0.151751 0.725506 1.040835 31.00000 -1.50000 H3'C 2 0.142893 0.845392 1.019444 31.00000 -1.50000 AFIX 0 C4' 1 0.312220 0.781974 0.935370 31.00000 0.08787 0.04854 = 0.02990 0.00472 0.01648 0.01142 C5' 1 0.248296 0.729743 0.786811 31.00000 0.07546 0.03911 = 0.02828 0.00747 0.01554 0.00594 PART 0 C6 1 0.233932 0.733616 0.713239 11.00000 0.06351 0.03929 = 0.03185 0.00603 0.01571 0.00048 PART 1 C1 1 0.188996 0.413679 0.918220 31.00000 0.14687 0.05297 = 0.06165 0.02354 0.04202 0.02617 AFIX 137 H1A 2 0.243358 0.398441 0.885303 31.00000 -1.50000 H1B 2 0.105509 0.404623 0.886128 31.00000 -1.50000 H1C 2 0.169651 0.353849 0.950238 31.00000 -1.50000 AFIX 0 C2' 1 0.276147 0.659395 0.913702 31.00000 0.09296 0.04696 = 0.02781 0.01186 0.01645 0.01392 PART 0 S5 6 0.274032 0.873933 0.685562 11.00000 0.07790 0.03567 = 0.03060 0.00217 0.01819 0.00400 PART 2 S2 6 0.434397 0.841129 1.030924 -31.00000 0.10551 0.06656 = 0.03877 0.00592 0.00696 0.01316 S1 6 0.307208 0.536714 0.970037 -31.00000 0.12974 0.06783 = 0.05060 0.02113 0.01851 0.02285 S4 6 0.356976 0.840118 0.864404 -31.00000 0.07954 0.04570 = 0.02941 0.00678 0.01981 0.02235 PART 0 S6 6 0.162848 0.600698 0.636775 11.00000 0.06648 0.03501 = 0.02904 0.00950 0.01145 0.00556 PART 2 S3 6 0.240502 0.569745 0.807483 -31.00000 0.08675 0.05882 = 0.02893 0.01158 0.02177 0.00764 PART 0 O3 5 0.481471 1.293035 0.356659 11.00000 0.09300 0.03126 = 0.04929 0.01908 0.02536 0.02193 PART 3 O6 5 0.092482 0.258188 0.187292 -21.00000 0.12590 0.03767 = 0.07011 -0.00195 0.04439 0.03288 SAME 0.02 0.04 O6 C18 C19 PART 0 PART 2 O6' 5 0.025237 0.278364 0.159635 21.00000 0.13187 0.04064 = 0.07480 -0.00891 0.03790 0.02379 C18' 1 -0.017943 0.146036 0.142892 20.50000 0.13147 0.03234 = 0.08064 0.00469 0.03932 0.03117 AFIX 23 H18A 2 -0.112344 0.106293 0.113506 20.50000 -1.20000 H18B 2 -0.015102 0.121860 0.192477 20.50000 -1.20000 AFIX 0 C19' 1 0.056140 0.088585 0.098483 20.50000 0.13444 0.02326 = 0.10504 0.00308 0.04563 0.03455 AFIX 137 H19A 2 -0.007294 0.007006 0.065729 20.50000 -1.50000 H19B 2 0.123959 0.079776 0.135048 20.50000 -1.50000 H19C 2 0.098761 0.142520 0.066495 20.50000 -1.50000 AFIX 0 PART 0 O4 5 0.459415 1.254713 0.470529 11.00000 0.08500 0.03038 = 0.03699 0.00682 0.01105 0.01530 O2 5 0.147248 0.634248 0.200283 11.00000 0.04380 0.07346 = 0.03475 0.01445 0.01052 0.02290 SAME 0.02 0.04 O6' C18' C19' O5 5 0.091943 0.287136 0.304047 11.00000 0.13209 0.03489 = 0.11774 0.02074 0.07176 0.03399 PART 1 C27 1 0.080736 0.165903 0.313318 10.50000 0.11054 0.03060 = 0.10345 0.01979 0.05356 0.03891 AFIX 23 H27A 2 0.152221 0.152662 0.294898 10.50000 -1.20000 H27B 2 -0.005010 0.101838 0.279212 10.50000 -1.20000 AFIX 0 C28 1 0.088475 0.144032 0.395140 10.50000 0.09826 0.03720 = 0.10947 0.01554 0.04796 0.03750 AFIX 137 H28A 2 0.105065 0.071252 0.397030 10.50000 -1.50000 H28B 2 0.004268 0.130217 0.408152 10.50000 -1.50000 H28C 2 0.160995 0.216768 0.432091 10.50000 -1.50000 AFIX 0 PART 0 O1 5 0.279562 0.919977 0.251220 11.00000 0.04277 0.03647 = 0.02641 0.00401 0.00604 0.01486 N3 4 0.412461 0.780336 0.293371 11.00000 0.05468 0.02796 = 0.04774 0.00487 -0.00830 0.01626 N2 4 0.189545 0.645386 0.356876 11.00000 0.03609 0.02654 = 0.02875 0.00310 0.00608 0.01238 N1 4 0.291814 0.886259 0.399977 11.00000 0.03747 0.02398 = 0.02997 0.00828 0.01142 0.01195 N4 4 1.034723 0.773852 0.287189 11.00000 0.06799 0.02844 = 0.05273 0.00967 0.03152 0.01999 C37 1 0.952344 0.711842 0.325768 11.00000 0.07112 0.04776 = 0.09250 0.03734 0.03999 0.03733 AFIX 43 H37 2 0.977216 0.660515 0.353046 11.00000 -1.20000 AFIX 0 C26 1 0.428411 1.460045 0.396514 11.00000 0.10184 0.05915 = 0.09076 0.00757 -0.00044 0.03696 AFIX 137 H26A 2 0.466563 1.547274 0.423990 11.00000 -1.50000 H26B 2 0.369505 1.408792 0.423994 11.00000 -1.50000 H26C 2 0.377515 1.448674 0.344472 11.00000 -1.50000 AFIX 0 C22 1 0.345401 1.035953 0.282708 11.00000 0.05061 0.04131 = 0.03225 0.01365 0.01184 0.02163 C33 1 0.577517 0.791360 0.226277 11.00000 0.05628 0.05091 = 0.05217 0.01463 0.00436 0.01790 AFIX 43 H33 2 0.603541 0.796846 0.179576 11.00000 -1.20000 AFIX 0 PART 2 C2 1 0.303831 0.631646 0.907346 -31.00000 0.10095 0.05333 = 0.03398 0.01094 0.01815 0.01290 PART 0 C24 1 0.442045 1.215785 0.402146 11.00000 0.05828 0.03373 = 0.04183 0.01656 0.01236 0.01806 C31 1 0.616621 0.781704 0.355856 11.00000 0.04987 0.03915 = 0.04230 0.00188 0.00234 0.02093 AFIX 43 H31 2 0.669938 0.779475 0.401368 11.00000 -1.20000 AFIX 0 C35 1 0.788935 0.783172 0.287914 11.00000 0.05386 0.03456 = 0.04567 0.00901 0.01215 0.01739 PART 2 C5 1 0.269018 0.712732 0.782948 -31.00000 0.07912 0.04413 = 0.02818 0.00632 0.01871 0.00698 PART 0 C39 1 0.870974 0.844865 0.244810 11.00000 0.05374 0.06060 = 0.05358 0.02599 0.00361 0.01468 AFIX 43 H39 2 0.845492 0.892210 0.214115 11.00000 -1.20000 AFIX 0 PART 3 C18 1 0.054124 0.127738 0.167743 -20.50000 0.13107 0.03667 = 0.08705 0.01371 0.03451 0.02490 AFIX 23 H18C 2 0.000572 0.099500 0.204601 -20.50000 -1.20000 H18D 2 0.139159 0.125200 0.188566 -20.50000 -1.20000 AFIX 0 PART 0 PART 2 C4 1 0.364843 0.756447 0.934082 -31.00000 0.09423 0.05238 = 0.02997 0.00960 0.01418 0.01455 PART 0 C23 1 0.380573 1.114685 0.226636 11.00000 0.10288 0.04582 = 0.04011 0.01638 0.01540 0.02403 AFIX 137 H23A 2 0.476981 1.165306 0.240175 11.00000 -1.50000 H23B 2 0.335762 1.168768 0.228343 11.00000 -1.50000 H23C 2 0.351980 1.061476 0.174716 11.00000 -1.50000 AFIX 0 PART 2 C29 1 0.076429 0.157797 0.414357 10.50000 0.11983 0.03732 = 0.10128 0.02000 0.03188 0.03511 AFIX 23 H29A 2 0.154530 0.176067 0.392713 10.50000 -1.20000 H29B 2 -0.002763 0.132559 0.371438 10.50000 -1.20000 AFIX 0 PART 0 C25 1 0.533741 1.423872 0.392232 11.00000 0.09782 0.02998 = 0.06761 0.01819 0.02417 0.02158 AFIX 23 H25A 2 0.589816 1.442316 0.444651 11.00000 -1.20000 H25B 2 0.590368 1.472651 0.362071 11.00000 -1.20000 AFIX 0 C10 1 0.267049 0.824301 0.459795 11.00000 0.03791 0.02938 = 0.02735 0.00614 0.00691 0.01145 C11 1 0.287912 0.881251 0.535975 11.00000 0.04996 0.02409 = 0.03170 0.00047 0.01298 0.00845 AFIX 43 H11 2 0.323305 0.968823 0.551598 11.00000 -1.20000 AFIX 0 C32 1 0.662624 0.787180 0.289741 11.00000 0.05040 0.03195 = 0.03924 0.00629 0.00206 0.01652 C12 1 0.257275 0.810793 0.589572 11.00000 0.05468 0.03335 = 0.02454 0.00306 0.01335 0.01083 C34 1 0.458017 0.787674 0.230572 11.00000 0.05740 0.04317 = 0.04954 0.01420 -0.00768 0.01554 AFIX 43 H34 2 0.403162 0.790502 0.185930 11.00000 -1.20000 AFIX 0 C13 1 0.159066 0.528046 0.331359 11.00000 0.05378 0.02811 = 0.03936 0.00485 0.02012 0.01383 AFIX 43 H13 2 0.159565 0.481636 0.368888 11.00000 -1.20000 AFIX 0 C36 1 0.834339 0.715214 0.329799 11.00000 0.06540 0.05314 = 0.07263 0.03858 0.03735 0.03465 AFIX 43 H36 2 0.783760 0.671105 0.361209 11.00000 -1.20000 AFIX 0 C14 1 0.125712 0.463773 0.254184 11.00000 0.07179 0.03585 = 0.04270 -0.00307 0.03234 0.00584 C38 1 0.989578 0.837998 0.246164 11.00000 0.06131 0.06288 = 0.04346 0.01890 0.01445 0.00993 AFIX 43 H38 2 1.043057 0.881901 0.215833 11.00000 -1.20000 AFIX 0 C15 1 0.118959 0.519948 0.192391 11.00000 0.04679 0.06265 = 0.03805 -0.00456 0.01306 0.00489 PART 2 C1' 1 0.160565 0.394410 0.925224 -31.00000 0.13365 0.05869 = 0.05629 0.00348 0.03406 0.02302 AFIX 137 H1'A 2 0.149112 0.337743 0.959286 -31.00000 -1.50000 H1'B 2 0.169824 0.356352 0.876492 -31.00000 -1.50000 H1'C 2 0.082827 0.411569 0.915467 -31.00000 -1.50000 AFIX 0 PART 0 C17 1 0.093987 0.331113 0.244680 11.00000 0.11451 0.03706 = 0.06513 -0.00716 0.05111 0.01294 PART 2 C3 1 0.281735 0.840671 1.051597 -31.00000 0.10301 0.06250 = 0.04147 0.00279 0.00693 0.01016 AFIX 137 H3A 2 0.220547 0.756431 1.051541 -31.00000 -1.50000 H3B 2 0.239543 0.869506 1.012182 -31.00000 -1.50000 H3C 2 0.303580 0.895830 1.102109 -31.00000 -1.50000 AFIX 0 PART 0 C20 1 0.350835 1.007331 0.416240 11.00000 0.04268 0.02935 = 0.03347 0.00529 0.00663 0.01580 AFIX 43 H20 2 0.377705 1.049195 0.468973 11.00000 -1.20000 AFIX 0 C21 1 0.378864 1.082819 0.362454 11.00000 0.04974 0.02597 = 0.03309 0.01125 0.01474 0.01588 PART 3 C19 1 -0.012865 0.012389 0.099632 -20.50000 0.15487 0.06752 = 0.11471 0.02837 0.05134 0.02362 AFIX 137 H19D 2 -0.013591 -0.059824 0.117664 -20.50000 -1.50000 H19E 2 0.036818 0.025854 0.060223 -20.50000 -1.50000 H19F 2 -0.104358 -0.002104 0.077760 -20.50000 -1.50000 AFIX 0 PART 0 C7 1 0.204625 0.681671 0.565620 11.00000 0.04879 0.03447 = 0.02834 0.00950 0.00851 0.00958 C30 1 0.494651 0.779495 0.355810 11.00000 0.05210 0.03553 = 0.04353 0.00023 -0.00197 0.01961 AFIX 43 H30 2 0.467006 0.777264 0.402154 11.00000 -1.20000 AFIX 0 C8 1 0.180732 0.623510 0.490048 11.00000 0.04544 0.02268 = 0.03430 0.00576 0.00935 0.00800 AFIX 43 H8 2 0.143010 0.535781 0.474441 11.00000 -1.20000 AFIX 0 C9 1 0.212288 0.694272 0.436669 11.00000 0.03587 0.02981 = 0.02837 0.00529 0.00700 0.01391 C16 1 0.074197 0.447287 0.108584 11.00000 0.08408 0.12119 = 0.03028 -0.02262 0.01688 -0.01033 AFIX 137 H16A 2 -0.006215 0.370463 0.101148 11.00000 -1.50000 H16B 2 0.144901 0.427472 0.095773 11.00000 -1.50000 H16C 2 0.055209 0.497347 0.075103 11.00000 -1.50000 AFIX 0 HKLF 4 REM ZJL_123K_0m_a.res in P-1 REM R1 = 0.0654 for 4591 Fo > 4sig(Fo) and 0.1106 for all 7221 data REM 643 parameters refined using 665 restraints END WGHT 0.0913 1.1389 REM Highest difference peak 0.869, deepest hole -0.473, 1-sigma level 0.077 Q1 1 -0.1245 -0.0659 0.0512 11.00000 0.05 0.87 Q2 1 0.4995 1.4776 0.3237 11.00000 0.05 0.63 Q3 1 0.1226 0.0798 0.4298 11.00000 0.05 0.43 Q4 1 0.0182 0.2845 0.2700 11.00000 0.05 0.34 Q5 1 0.2156 0.4988 0.7910 11.00000 0.05 0.33 Q6 1 0.1389 0.1186 0.0284 11.00000 0.05 0.33 Q7 1 0.9856 0.7478 0.3668 11.00000 0.05 0.31 Q8 1 0.3286 0.4582 0.9372 11.00000 0.05 0.30 Q9 1 0.1053 0.1126 0.1473 11.00000 0.05 0.30 Q10 1 0.3812 0.7599 1.0252 11.00000 0.05 0.28 Q11 1 0.2692 0.7972 0.6689 11.00000 0.05 0.28 Q12 1 0.1701 0.5801 0.8619 11.00000 0.05 0.27 Q13 1 0.2589 0.8569 0.3276 11.00000 0.05 0.27 Q14 1 0.0800 0.4581 0.5373 11.00000 0.05 0.27 Q15 1 0.1794 0.6246 0.5837 11.00000 0.05 0.26 Q16 1 0.2483 0.8028 0.2366 11.00000 0.05 0.26 Q17 1 0.3393 0.7667 0.8566 11.00000 0.05 0.26 Q18 1 0.0346 0.3495 0.2096 11.00000 0.05 0.26 Q19 1 0.3227 0.8350 0.6895 11.00000 0.05 0.26 Q20 1 0.2817 0.6845 1.0455 11.00000 0.05 0.25 ; _shelx_res_checksum 53511 _shelx_fab_file ; 2 0 0 -2.29 0.00 3 0 0 11.48 0.00 4 0 0 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-0.37 0.00 -1 1 3 -0.16 0.00 -13 3 3 0.10 0.00 9 4 3 0.88 0.00 -13 8 3 0.66 0.00 0 12 3 0.40 0.00 -9 13 3 0.25 0.00 3 -14 4 0.64 0.00 7 -14 4 0.00 0.00 0 -13 4 0.94 0.00 -2 -12 4 -0.80 0.00 -6 -9 4 -0.81 0.00 -7 -8 4 -0.73 0.00 12 -3 4 0.84 0.00 10 2 4 -0.15 0.00 -13 3 4 -0.02 0.00 8 5 4 1.12 0.00 -13 8 4 0.32 0.00 -3 13 4 -0.06 0.00 0 -13 5 0.61 0.00 -2 -12 5 0.18 0.00 11 -11 5 0.62 0.00 -6 -9 5 -1.36 0.00 -7 -8 5 -1.30 0.00 -13 3 5 -0.07 0.00 6 7 5 0.11 0.00 -13 8 5 0.12 0.00 1 11 5 -0.44 0.00 -1 12 5 0.73 0.00 -8 13 5 0.13 0.00 4 -14 6 -0.21 0.00 6 -14 6 0.24 0.00 0 -13 6 -0.85 0.00 -2 -12 6 1.62 0.00 10 -12 6 0.37 0.00 -6 -9 6 -0.88 0.00 -7 -8 6 -0.92 0.00 -8 -7 6 -0.99 0.00 -13 3 6 -0.19 0.00 -13 7 6 -0.50 0.00 -12 10 6 0.26 0.00 2 10 6 -0.38 0.00 -11 11 6 -0.06 0.00 5 -14 7 -0.47 0.00 0 -13 7 -1.20 0.00 1 -13 7 1.78 0.00 -2 -12 7 0.87 0.00 11 -10 7 0.10 0.00 -6 -9 7 -0.13 0.00 -7 -8 7 -0.41 0.00 10 0 7 -0.54 0.00 9 2 7 -0.63 0.00 -13 4 7 0.57 0.00 -13 6 7 0.35 0.00 4 8 7 -0.16 0.00 -9 12 7 -0.66 0.00 8 -13 8 -0.07 0.00 10 -11 8 0.34 0.00 -6 -9 8 -0.03 0.00 11 -9 8 -0.82 0.00 -7 -8 8 -0.34 0.00 11 -4 8 -0.22 0.00 -12 0 8 -0.49 0.00 8 3 8 -1.32 0.00 -13 5 8 0.41 0.00 -12 9 8 -0.75 0.00 -1 11 8 0.25 0.00 -8 12 8 0.83 0.00 -4 12 8 -0.39 0.00 -10 -4 9 -0.34 0.00 -12 0 9 -0.16 0.00 6 5 9 -0.49 0.00 3 8 9 -0.86 0.00 0 10 9 0.64 0.00 -3 11 9 0.26 0.00 -2 11 9 -0.18 0.00 3 -13 10 -0.60 0.00 10 -3 10 -0.50 0.00 -11 -2 10 -0.27 0.00 1 9 10 -0.01 0.00 2 -13 11 0.59 0.00 5 -13 11 -1.08 0.00 -1 -12 11 1.10 0.00 -2 -11 11 0.72 0.00 -5 -9 11 -0.11 0.00 10 -7 11 -0.44 0.00 10 -6 11 -0.50 0.00 5 5 11 0.47 0.00 4 6 11 -0.01 0.00 3 7 11 -0.25 0.00 -2 10 11 0.41 0.00 8 -11 12 -0.34 0.00 -4 -10 12 -0.12 0.00 9 -9 12 -0.76 0.00 9 -3 12 -0.67 0.00 -12 3 12 0.19 0.00 6 3 12 0.02 0.00 -12 5 12 -0.34 0.00 -11 8 12 0.41 0.00 -10 9 12 0.54 0.00 -2 -11 13 0.11 0.00 7 -11 13 -0.18 0.00 8 -10 13 -0.10 0.00 -5 -9 13 -0.08 0.00 -6 -8 13 0.41 0.00 -7 -7 13 0.23 0.00 9 -6 13 0.61 0.00 -11 7 13 -0.28 0.00 0 8 13 0.65 0.00 -9 9 13 -0.22 0.00 -2 9 13 -0.01 0.00 2 -12 14 -0.18 0.00 3 -12 14 -0.72 0.00 6 -11 14 0.98 0.00 -9 -4 14 -0.64 0.00 3 5 14 -0.16 0.00 -7 9 14 0.15 0.00 -4 9 14 -0.17 0.00 0 -11 15 0.41 0.00 3 -11 15 1.24 0.00 -4 -9 15 0.23 0.00 7 -9 15 -0.24 0.00 -8 -5 15 -1.22 0.00 6 0 15 -1.38 0.00 4 3 15 0.10 0.00 2 5 15 0.31 0.00 -8 8 15 0.51 0.00 -3 8 15 -0.15 0.00 5 -10 16 -0.56 0.00 6 -9 16 0.53 0.00 -10 0 16 0.53 0.00 4 2 16 -0.41 0.00 1 5 16 -0.23 0.00 -8 7 16 0.01 0.00 0 -10 17 0.01 0.00 3 -10 17 -0.03 0.00 -4 -8 17 -0.10 0.00 6 -6 17 0.36 0.00 -7 -5 17 0.50 0.00 6 -5 17 0.19 0.00 5 -1 17 0.31 0.00 3 2 17 0.16 0.00 1 4 17 -0.21 0.00 -8 6 17 -1.01 0.00 -2 6 17 0.76 0.00 3 -9 18 -0.75 0.00 -3 -8 18 0.29 0.00 4 -8 18 0.31 0.00 5 -6 18 -0.79 0.00 5 -5 18 -0.20 0.00 -7 -4 18 0.92 0.00 5 -4 18 -0.39 0.00 4 -1 18 0.18 0.00 2 2 18 0.35 0.00 1 3 18 0.03 0.00 -2 5 18 -0.41 0.00 -1 -8 19 0.78 0.00 2 -8 19 -0.38 0.00 -3 -7 19 -0.27 0.00 3 -7 19 0.03 0.00 -8 1 19 -1.44 0.00 -6 4 19 0.78 0.00 -4 -5 20 -1.31 0.00 2 -5 20 -1.60 0.00 -5 -4 20 -0.23 0.00 -4 -4 20 -0.71 0.00 -6 -2 20 0.13 0.00 -6 2 20 0.65 0.00 -2 -4 21 -0.42 0.00 -1 -4 21 0.64 0.00 0 -3 21 0.09 0.00 -4 -2 21 0.40 0.00 -4 -1 21 -1.46 0.00 -1 -1 21 0.19 0.00 -4 0 21 0.94 0.00 -3 0 21 0.28 0.00 -2 0 21 -0.67 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 201118) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 0.000 294 70 ' ' # Missing Reflections Below sin(th)/lambda = 0.25 loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 1 0 0 3.822 -2 1 0 6.886 -1 1 0 3.919 -1 2 0 6.446 2 -1 1 7.563 -2 0 1 7.410 -2 1 1 6.890 -1 1 1 4.443 0 1 1 4.624 1 1 1 7.240 -1 2 1 7.058 0 2 1 7.969 -1 0 2 5.052 -2 1 2 7.575 -1 1 2 5.826 0 1 2 6.319 -1 1 3 7.618 _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details ) TITL ZJL_123K_0m_a P -1 R = 0.11 CELL 11.3618 12.1577 18.2103 98.64 99.86 113.65 SPGR P-1 # Solvent Accessible Volume = 295 # Electrons Found in S.A.V. = 70 # Note: Atoms in Void are Labelled as Cxxx and Qxxx for all Others C101 0.331 0.311 0.059 ! 3.39 eA-3 C102 0.437 0.464 0.130 ! 2.98 eA-3 C103 0.389 0.338 0.129 ! 2.10 eA-3 C104 0.408 0.429 0.194 ! 2.03 eA-3 Q105 0.733 0.859 0.026 ! 1.89 eA-3 C106 0.300 0.193 0.998 ! 1.88 eA-3 Q107 0.457 0.843 0.027 ! 1.55 eA-3 Q108 0.626 0.168 0.142 ! 1.10 eA-3 Q109 0.391 0.060 0.469 ! 0.90 eA-3 Q110 0.488 0.470 0.313 ! 0.82 eA-3 Q111 0.971 0.160 0.139 ! 0.77 eA-3 Q112 0.077 0.498 0.106 ! 0.76 eA-3 Q113 0.370 0.076 0.251 ! 0.74 eA-3 Q114 0.751 0.467 0.206 ! 0.74 eA-3 C115 0.325 0.123 0.036 ! 0.74 eA-3 Q116 0.028 0.399 0.093 ! 0.72 eA-3 Q117 0.673 0.156 0.313 ! 0.71 eA-3 Q118 0.114 0.082 0.420 ! 0.71 eA-3 Q119 0.452 0.764 0.329 ! 0.68 eA-3 Q120 0.717 0.521 0.046 ! 0.68 eA-3 Q121 0.169 0.761 0.281 ! 0.68 eA-3 Q122 0.581 0.787 0.186 ! 0.65 eA-3 Q123 0.409 0.782 0.172 ! 0.64 eA-3 Q124 0.050 0.891 0.219 ! 0.64 eA-3 Q125 0.143 0.536 0.466 ! 0.62 eA-3 Q126 0.263 0.838 0.328 ! 0.61 eA-3 Q127 0.813 0.546 0.068 ! 0.60 eA-3 Q128 0.659 0.013 0.439 ! 0.59 eA-3 Q129 0.826 0.648 0.045 ! 0.59 eA-3 Q130 0.394 0.121 0.391 ! 0.57 eA-3 Q131 0.481 0.171 0.247 ! 0.57 eA-3 Q132 0.429 0.544 0.211 ! 0.57 eA-3 Q133 0.656 0.519 0.062 ! 0.56 eA-3 Q134 0.332 0.266 0.157 ! 0.55 eA-3 Q135 0.998 0.645 0.381 ! 0.55 eA-3 Q136 0.623 0.442 0.442 ! 0.55 eA-3 Q137 0.970 0.925 0.080 ! 0.55 eA-3 Q138 0.057 0.133 0.063 ! 0.54 eA-3 Q139 0.017 0.794 0.309 ! 0.54 eA-3 Q140 0.593 0.480 0.342 ! 0.54 eA-3 Q141 0.330 0.171 0.220 ! 0.54 eA-3 Q142 0.684 0.791 0.421 ! 0.53 eA-3 Q143 0.812 0.775 0.296 ! 0.53 eA-3 Q144 0.090 0.797 0.297 ! 0.53 eA-3 Q145 0.123 0.587 0.170 ! 0.53 eA-3 Q146 0.749 0.231 0.299 ! 0.53 eA-3 Q147 0.176 0.210 0.077 ! 0.53 eA-3 Q148 0.219 0.640 0.470 ! 0.53 eA-3 Q149 0.843 0.473 0.368 ! 0.52 eA-3 Q150 0.283 0.684 0.044 ! 0.52 eA-3 Q151 0.611 0.345 0.390 ! 0.51 eA-3 Q152 0.359 0.402 0.256 ! 0.51 eA-3 Q153 0.871 0.416 0.495 ! 0.50 eA-3 Q154 0.202 0.813 0.451 ! 0.50 eA-3 ) ; _shelx_fab_checksum 4702 _olex2_submission_special_instructions 'No special instructions were received' _publcif_funding_html ; ; ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_350K _database_code_depnum_ccdc_archive 'CCDC 1835731' _audit_update_record ; 2019-11-11 deposited with the CCDC. 2020-05-27 downloaded from the CCDC. ; _publcif_datablock.id {1087d51c-676b-47c6-b0f0-2c763ec199b5} _audit_creation_method SHELXL-2018/3 _shelx_SHELXL_version_number 2018/3 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H34 Fe N4 O6 S6' _chemical_formula_weight 866.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.360(11) _cell_length_b 12.085(10) _cell_length_c 16.842(14) _cell_angle_alpha 91.22(2) _cell_angle_beta 109.72(2) _cell_angle_gamma 111.47(2) _cell_volume 1998(3) _cell_formula_units_Z 2 _cell_measurement_temperature 350(2) _cell_measurement_reflns_used 3388 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 23.60 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_F_000 896 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 0.740 _shelx_estimated_absorpt_T_min 0.897 _shelx_estimated_absorpt_T_max 0.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3502 _exptl_absorpt_correction_T_max 0.7451 _exptl_absorpt_process_details sadabs _exptl_absorpt_special_details ? _diffrn_ambient_temperature 350(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12227 _diffrn_reflns_av_unetI/netI 0.2683 _diffrn_reflns_av_R_equivalents 0.1317 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.420 _diffrn_reflns_theta_max 24.405 _diffrn_reflns_theta_full 24.405 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measured_fraction_theta_full 0.966 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_Laue_measured_fraction_full 0.966 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_point_group_measured_fraction_full 0.966 _reflns_number_total 6358 _reflns_number_gt 1890 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+3.1000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6358 _refine_ls_number_parameters 484 _refine_ls_number_restraints 414 _refine_ls_R_factor_all 0.2822 _refine_ls_R_factor_gt 0.1290 _refine_ls_wR_factor_ref 0.3013 _refine_ls_wR_factor_gt 0.2426 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.099 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.8509(2) 0.22935(17) 0.71523(11) 0.0701(7) Uani 1 1 d . . . . . S1 S 0.6267(4) 0.0889(3) 0.2756(2) 0.0900(14) Uani 1 1 d . U . . . S2 S 0.7358(4) 0.3521(3) 0.3022(2) 0.0951(14) Uani 1 1 d . U . . . S4 S 0.5609(6) 0.3380(4) 0.1013(3) 0.1287(19) Uani 1 1 d . U . . . S3 S 0.4749(6) 0.0793(4) 0.0796(3) 0.131(2) Uani 1 1 d . U . . . O1 O 0.9481(9) 0.3786(8) 0.8034(5) 0.072(3) Uani 1 1 d . U . . . O2 O 0.8189(8) 0.0839(8) 0.7714(4) 0.066(2) Uani 1 1 d . U . . . N2 N 0.7467(9) 0.1091(9) 0.6012(6) 0.051(2) Uani 1 1 d . U . . . N1 N 0.8519(10) 0.3492(9) 0.6279(6) 0.066(3) Uani 1 1 d . U . . . S5 S 0.2265(8) 0.0308(6) -0.0727(4) 0.216(3) Uani 1 1 d . U . . . O3 O 0.9379(11) 0.6876(8) 0.6488(7) 0.101(3) Uani 1 1 d . U . . . N4 N 0.0456(11) 0.2313(9) 0.7211(6) 0.069(3) Uani 1 1 d . U . . . S6 S 0.3183(9) 0.3235(7) -0.0478(4) 0.221(3) Uani 1 1 d . U . . . N3 N 0.6572(11) 0.2295(8) 0.7190(7) 0.064(3) Uani 1 1 d . U . . . O6 O 0.5686(12) -0.2464(8) 0.5542(7) 0.119(4) Uani 1 1 d . U . . . C29 C 0.4228(15) 0.2356(10) 0.7225(10) 0.067(4) Uani 1 1 d . U . . . C15 C 0.8003(12) 0.2891(11) 0.5411(8) 0.063(4) Uani 1 1 d . U . . . C20 C 0.7412(11) 0.1638(12) 0.5280(8) 0.062(3) Uani 1 1 d . U . . . C8 C 0.6896(12) -0.0061(11) 0.5966(7) 0.057(3) Uani 1 1 d . U . . . H8 H 0.637989 -0.050869 0.541944 0.069 Uiso 1 1 calc R U . . . C1 C 0.8812(13) 0.4608(13) 0.6435(8) 0.076(4) Uani 1 1 d . U . . . H1 H 0.863034 0.500174 0.596790 0.092 Uiso 1 1 calc R U . . . C18 C 0.6898(13) 0.1623(12) 0.3778(7) 0.066(4) Uani 1 1 d . U . . . C32 C 0.2916(15) 0.2331(12) 0.7194(9) 0.084(4) Uani 1 1 d . U . . . C17 C 0.7450(13) 0.2889(12) 0.3921(8) 0.067(4) Uani 1 1 d . U . . . C9 C 0.6964(13) -0.0693(11) 0.6623(9) 0.060(3) Uani 1 1 d . U . . . C19 C 0.6895(12) 0.1040(10) 0.4477(8) 0.066(4) Uani 1 1 d . U . . . H19 H 0.652097 0.020163 0.438702 0.079 Uiso 1 1 calc R U . . . C2 C 0.9381(14) 0.5296(13) 0.7241(10) 0.080(4) Uani 1 1 d . U . . . C5 C 0.9656(16) 0.6582(17) 0.7271(11) 0.097(5) Uani 1 1 d . U . . . C28 C 0.4413(15) 0.2324(12) 0.6493(9) 0.080(4) Uani 1 1 d . U . . . H28 H 0.373406 0.229002 0.598235 0.097 Uiso 1 1 calc R U . . . C10 C 0.7613(14) -0.0261(12) 0.7494(11) 0.071(4) Uani 1 1 d . U . . . C3 C 0.9684(15) 0.4887(13) 0.7978(10) 0.083(5) Uani 1 1 d . U . . . C31 C 0.6363(15) 0.2288(11) 0.7889(8) 0.077(4) Uani 1 1 d . U . . . H31 H 0.704853 0.228773 0.838421 0.092 Uiso 1 1 calc R U . . . C16 C 0.7999(13) 0.3486(11) 0.4732(8) 0.069(4) Uani 1 1 d . U . . . H16 H 0.838254 0.432446 0.482908 0.083 Uiso 1 1 calc R U . . . C12 C 0.6209(18) -0.2014(16) 0.6272(12) 0.098(5) Uani 1 1 d . U . . . O4 O 1.0030(14) 0.7295(9) 0.7870(7) 0.152(6) Uani 1 1 d . U . . . O5 O 0.6126(13) -0.2705(10) 0.6853(7) 0.135(4) Uani 1 1 d . U . . . C21 C 0.6393(15) 0.2189(12) 0.2328(9) 0.084(4) Uani 1 1 d . U . . . C30 C 0.5157(16) 0.2282(13) 0.7956(10) 0.101(5) Uani 1 1 d . U . . . H30 H 0.500869 0.223082 0.846731 0.121 Uiso 1 1 calc R U . . . C27 C 0.5609(17) 0.2341(12) 0.6507(9) 0.089(5) Uani 1 1 d . U . . . H27 H 0.576397 0.238791 0.599797 0.107 Uiso 1 1 calc R U . . . C11 C 0.7720(16) -0.1004(12) 0.8177(8) 0.112(6) Uani 1 1 d . U . . . H11A H 0.846537 -0.052925 0.868948 0.169 Uiso 1 1 calc R U . . . H11B H 0.787422 -0.168323 0.800200 0.169 Uiso 1 1 calc R U . . . H11C H 0.688889 -0.128319 0.828408 0.169 Uiso 1 1 calc R U . . . C36 C 0.193(2) 0.1358(16) 0.7228(10) 0.127(6) Uani 1 1 d . U . . . H36 H 0.205189 0.063724 0.725432 0.152 Uiso 1 1 calc R U . . . C22 C 0.5652(17) 0.2132(13) 0.1499(10) 0.103(5) Uani 1 1 d . U . . . C6 C 0.971(2) 0.8114(16) 0.6457(12) 0.144(7) Uani 1 1 d . U . . . H6A H 1.067723 0.857439 0.675917 0.173 Uiso 1 1 calc R U . . . H6B H 0.921330 0.840859 0.671594 0.173 Uiso 1 1 calc R U . . . C4 C 1.0307(17) 0.5602(12) 0.8889(7) 0.128(7) Uani 1 1 d . U . . . H4A H 0.988033 0.512717 0.924214 0.193 Uiso 1 1 calc R U . . . H4B H 1.016195 0.633662 0.887222 0.193 Uiso 1 1 calc R U . . . H4C H 1.126640 0.578724 0.912249 0.193 Uiso 1 1 calc R U . . . C35 C 0.0728(18) 0.1374(15) 0.7225(10) 0.120(5) Uani 1 1 d . U . . . H35 H 0.006126 0.064801 0.723413 0.144 Uiso 1 1 calc R U . . . C33 C 0.2643(18) 0.3284(15) 0.7168(10) 0.121(5) Uani 1 1 d . U . . . H33 H 0.328528 0.400771 0.713374 0.145 Uiso 1 1 calc R U . . . C7 C 0.932(2) 0.8221(14) 0.5563(13) 0.173(10) Uani 1 1 d . U . . . H7A H 0.986375 0.797562 0.532518 0.259 Uiso 1 1 calc R U . . . H7B H 0.946736 0.904352 0.550269 0.259 Uiso 1 1 calc R U . . . H7C H 0.837649 0.771409 0.526544 0.259 Uiso 1 1 calc R U . . . C34 C 0.1406(19) 0.3260(14) 0.7190(10) 0.116(5) Uani 1 1 d . U . . . H34 H 0.128165 0.397853 0.718907 0.139 Uiso 1 1 calc R U . . . C24 C 0.367(2) 0.1314(18) 0.0104(10) 0.137(6) Uani 1 1 d . U . . . C23 C 0.409(2) 0.2505(18) 0.0224(12) 0.137(6) Uani 1 1 d . U . . . C26 C 0.177(2) -0.0955(18) -0.0251(12) 0.215(9) Uani 1 1 d . U . . . H26A H 0.178189 -0.162743 -0.055747 0.323 Uiso 1 1 calc R U . . . H26B H 0.086630 -0.113895 -0.026438 0.323 Uiso 1 1 calc R U . . . H26C H 0.238903 -0.079650 0.033141 0.323 Uiso 1 1 calc R U . . . C13 C 0.557(2) -0.4071(15) 0.6418(12) 0.190(8) Uani 1 1 d . U . . . H13A H 0.458327 -0.443967 0.612987 0.228 Uiso 1 1 calc R U . . . H13B H 0.601446 -0.419391 0.604652 0.228 Uiso 1 1 calc R U . . . C14 C 0.610(2) -0.4433(18) 0.7340(13) 0.228(9) Uani 1 1 d . U . . . H14A H 0.587730 -0.528480 0.727850 0.341 Uiso 1 1 calc R U . . . H14B H 0.567360 -0.422686 0.769078 0.341 Uiso 1 1 calc R U . . . H14C H 0.706980 -0.400461 0.760306 0.341 Uiso 1 1 calc R U . . . C25 C 0.273(3) 0.387(2) 0.0172(16) 0.293(13) Uani 1 1 d . U . . . H25A H 0.188856 0.331563 0.019095 0.440 Uiso 1 1 calc R U . . . H25B H 0.261631 0.457813 -0.002983 0.440 Uiso 1 1 calc R U . . . H25C H 0.342519 0.410017 0.073466 0.440 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 0.0419(13) 0.0769(14) 0.0934(14) -0.0025(10) 0.0319(11) 0.0203(11) S1 0.103(4) 0.083(3) 0.086(3) 0.002(2) 0.037(2) 0.038(3) S2 0.100(4) 0.080(3) 0.101(3) 0.016(2) 0.049(3) 0.021(3) S4 0.143(5) 0.134(4) 0.108(3) 0.028(3) 0.043(3) 0.055(4) S3 0.156(5) 0.144(4) 0.088(3) -0.012(3) 0.028(3) 0.071(4) O1 0.054(6) 0.086(6) 0.075(5) -0.001(5) 0.025(4) 0.027(6) O2 0.036(6) 0.088(6) 0.075(5) 0.014(5) 0.022(4) 0.026(5) N2 0.025(6) 0.063(7) 0.062(6) -0.002(5) 0.023(5) 0.011(5) N1 0.037(7) 0.069(7) 0.099(8) -0.001(6) 0.043(6) 0.012(6) S5 0.211(8) 0.217(6) 0.126(4) 0.015(4) -0.019(4) 0.059(6) O3 0.102(9) 0.060(7) 0.146(9) 0.005(6) 0.052(7) 0.031(6) N4 0.069(6) 0.052(5) 0.095(6) 0.019(5) 0.045(5) 0.022(5) S6 0.259(9) 0.235(7) 0.164(5) 0.070(5) 0.036(5) 0.130(6) N3 0.035(7) 0.073(7) 0.073(7) -0.005(6) 0.027(6) 0.004(6) O6 0.128(11) 0.076(7) 0.129(9) -0.004(7) 0.045(8) 0.018(7) C29 0.044(9) 0.062(8) 0.092(10) -0.004(7) 0.039(8) 0.006(7) C15 0.044(9) 0.064(8) 0.072(8) -0.010(7) 0.030(7) 0.006(7) C20 0.017(7) 0.082(9) 0.077(9) -0.012(8) 0.018(6) 0.011(7) C8 0.038(9) 0.072(9) 0.056(7) -0.001(7) 0.022(6) 0.012(7) C1 0.043(9) 0.093(10) 0.082(9) 0.007(8) 0.023(7) 0.017(8) C18 0.043(9) 0.088(9) 0.061(8) 0.010(7) 0.021(6) 0.019(8) C32 0.047(10) 0.039(8) 0.169(12) 0.000(8) 0.043(9) 0.021(7) C17 0.052(9) 0.073(9) 0.072(8) 0.026(7) 0.023(7) 0.018(7) C9 0.060(9) 0.057(8) 0.092(9) 0.036(7) 0.056(8) 0.027(7) C19 0.047(9) 0.058(8) 0.076(8) -0.017(7) 0.024(7) 0.004(7) C2 0.060(10) 0.076(10) 0.087(10) -0.035(8) 0.038(8) 0.001(8) C5 0.063(11) 0.113(13) 0.110(12) -0.011(12) 0.039(10) 0.027(10) C28 0.036(10) 0.105(10) 0.085(10) 0.007(8) 0.014(8) 0.019(9) C10 0.046(9) 0.065(9) 0.130(12) 0.020(9) 0.068(9) 0.020(8) C3 0.066(11) 0.073(10) 0.113(11) -0.013(10) 0.053(9) 0.015(9) C31 0.061(11) 0.093(10) 0.074(9) 0.015(7) 0.023(8) 0.031(9) C16 0.056(10) 0.073(9) 0.086(9) 0.005(8) 0.044(8) 0.021(7) C12 0.091(13) 0.093(12) 0.121(13) 0.036(10) 0.068(11) 0.021(10) O4 0.201(15) 0.081(8) 0.138(10) -0.032(7) 0.036(9) 0.044(8) O5 0.149(10) 0.108(7) 0.148(9) 0.030(6) 0.073(8) 0.035(7) C21 0.072(11) 0.087(10) 0.116(10) 0.015(9) 0.056(9) 0.038(8) C30 0.063(12) 0.146(13) 0.123(12) 0.040(10) 0.063(10) 0.047(11) C27 0.066(12) 0.107(11) 0.077(10) 0.006(8) 0.028(9) 0.015(10) C11 0.157(18) 0.109(12) 0.102(11) 0.031(9) 0.074(11) 0.061(12) C36 0.118(9) 0.107(9) 0.179(9) 0.013(7) 0.058(7) 0.070(7) C22 0.088(12) 0.113(11) 0.119(11) 0.021(10) 0.046(10) 0.045(10) C6 0.116(17) 0.093(13) 0.213(19) 0.029(15) 0.064(15) 0.027(12) C4 0.157(19) 0.111(12) 0.083(10) -0.021(9) 0.013(11) 0.048(12) C35 0.105(9) 0.102(7) 0.169(9) 0.020(7) 0.056(7) 0.055(7) C33 0.092(8) 0.103(8) 0.180(9) 0.035(7) 0.065(7) 0.038(7) C7 0.15(2) 0.082(13) 0.24(2) 0.025(16) 0.035(19) 0.033(13) C34 0.097(8) 0.088(7) 0.177(9) 0.025(7) 0.061(7) 0.042(6) C24 0.172(16) 0.159(14) 0.076(10) 0.013(11) 0.026(10) 0.079(13) C23 0.144(15) 0.160(14) 0.143(13) 0.048(13) 0.059(11) 0.094(13) C26 0.222(13) 0.208(12) 0.201(12) 0.015(8) 0.067(9) 0.080(9) C13 0.197(16) 0.120(11) 0.209(13) 0.059(10) 0.068(12) 0.019(11) C14 0.236(13) 0.196(10) 0.244(12) 0.062(9) 0.076(9) 0.090(9) C25 0.298(16) 0.293(16) 0.295(16) 0.053(9) 0.098(10) 0.135(11) _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 O2 1.988(9) . ? Fe1 O1 2.000(8) . ? Fe1 N2 2.071(8) . ? Fe1 N1 2.086(10) . ? Fe1 N4 2.171(11) 1_655 ? Fe1 N3 2.223(11) . ? S1 C18 1.703(12) . ? S1 C21 1.721(14) . ? S2 C17 1.699(12) . ? S2 C21 1.709(14) . ? S4 C23 1.71(2) . ? S4 C22 1.740(15) . ? S3 C24 1.704(18) . ? S3 C22 1.719(15) . ? O1 C3 1.276(14) . ? O2 C10 1.229(13) . ? N2 C8 1.291(12) . ? N2 C20 1.405(13) . ? N1 C1 1.264(13) . ? N1 C15 1.439(13) . ? S5 C24 1.725(18) . ? S5 C26 1.74(2) . ? O3 C5 1.336(16) . ? O3 C6 1.409(17) . ? N4 C35 1.281(15) . ? N4 C34 1.264(17) . ? S6 C25 1.64(3) . ? S6 C23 1.771(17) . ? N3 C31 1.276(14) . ? N3 C27 1.313(15) . ? O6 C12 1.184(16) . ? C29 C30 1.354(16) . ? C29 C28 1.321(16) . ? C29 C32 1.463(17) . ? C15 C16 1.363(14) . ? C15 C20 1.391(14) . ? C20 C19 1.344(13) . ? C8 C9 1.355(14) . ? C8 H8 0.9300 . ? C1 C2 1.385(15) . ? C1 H1 0.9300 . ? C18 C17 1.403(15) . ? C18 C19 1.385(14) . ? C32 C33 1.295(16) . ? C32 C36 1.31(2) . ? C17 C16 1.353(14) . ? C9 C10 1.386(16) . ? C9 C12 1.500(19) . ? C19 H19 0.9300 . ? C2 C3 1.330(17) . ? C2 C5 1.47(2) . ? C5 O4 1.160(15) . ? C28 C27 1.343(17) . ? C28 H28 0.9300 . ? C10 C11 1.475(16) . ? C3 C4 1.537(16) . ? C31 C30 1.410(17) . ? C31 H31 0.9300 . ? C16 H16 0.9300 . ? C12 O5 1.305(15) . ? O5 C13 1.590(18) . ? C21 C22 1.350(17) . ? C30 H30 0.9300 . ? C27 H27 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C36 C35 1.37(2) . ? C36 H36 0.9300 . ? C6 C7 1.44(2) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C35 H35 0.9300 . ? C33 C34 1.41(2) . ? C33 H33 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C34 H34 0.9300 . ? C24 C23 1.33(2) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C13 C14 1.60(2) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? 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 O2 Fe1 O1 110.1(3) . . ? O2 Fe1 N2 85.7(4) . . ? O1 Fe1 N2 164.1(4) . . ? O2 Fe1 N1 165.2(4) . . ? O1 Fe1 N1 84.5(4) . . ? N2 Fe1 N1 79.7(4) . . ? O2 Fe1 N4 90.2(4) . 1_655 ? O1 Fe1 N4 89.8(4) . 1_655 ? N2 Fe1 N4 92.3(4) . 1_655 ? N1 Fe1 N4 92.1(4) . 1_655 ? O2 Fe1 N3 88.0(4) . . ? O1 Fe1 N3 87.5(3) . . ? N2 Fe1 N3 91.1(4) . . ? N1 Fe1 N3 90.5(4) . . ? N4 Fe1 N3 176.1(4) 1_655 . ? C18 S1 C21 93.1(7) . . ? C17 S2 C21 95.2(7) . . ? C23 S4 C22 90.7(9) . . ? C24 S3 C22 94.2(8) . . ? C3 O1 Fe1 132.0(9) . . ? C10 O2 Fe1 137.5(9) . . ? C8 N2 C20 122.1(10) . . ? C8 N2 Fe1 123.7(8) . . ? C20 N2 Fe1 114.2(8) . . ? C1 N1 C15 120.3(12) . . ? C1 N1 Fe1 127.0(9) . . ? C15 N1 Fe1 112.4(8) . . ? C24 S5 C26 102.1(10) . . ? C5 O3 C6 115.5(14) . . ? C35 N4 C34 113.8(16) . . ? C35 N4 Fe1 123.9(11) . 1_455 ? C34 N4 Fe1 122.3(11) . 1_455 ? C25 S6 C23 100.9(11) . . ? C31 N3 C27 116.7(13) . . ? C31 N3 Fe1 121.2(11) . . ? C27 N3 Fe1 122.1(10) . . ? C30 C29 C28 121.0(15) . . ? C30 C29 C32 121.4(14) . . ? C28 C29 C32 117.2(15) . . ? C16 C15 C20 120.1(11) . . ? C16 C15 N1 123.4(12) . . ? C20 C15 N1 116.3(12) . . ? C19 C20 C15 118.3(13) . . ? C19 C20 N2 124.9(12) . . ? C15 C20 N2 116.7(11) . . ? N2 C8 C9 127.3(11) . . ? N2 C8 H8 116.4 . . ? C9 C8 H8 116.4 . . ? N1 C1 C2 125.6(14) . . ? N1 C1 H1 117.2 . . ? C2 C1 H1 117.2 . . ? C17 C18 C19 118.1(10) . . ? C17 C18 S1 118.3(10) . . ? C19 C18 S1 123.6(10) . . ? C33 C32 C36 113.7(17) . . ? C33 C32 C29 122.9(15) . . ? C36 C32 C29 123.3(14) . . ? C16 C17 C18 119.0(11) . . ? C16 C17 S2 126.3(11) . . ? C18 C17 S2 114.7(10) . . ? C10 C9 C8 128.6(13) . . ? C10 C9 C12 122.3(13) . . ? C8 C9 C12 109.1(13) . . ? C20 C19 C18 122.6(12) . . ? C20 C19 H19 118.7 . . ? C18 C19 H19 118.7 . . ? C3 C2 C1 125.7(15) . . ? C3 C2 C5 118.0(13) . . ? C1 C2 C5 116.3(16) . . ? O4 C5 O3 121.1(18) . . ? O4 C5 C2 127.5(18) . . ? O3 C5 C2 111.4(14) . . ? C27 C28 C29 118.2(14) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? O2 C10 C9 117.1(13) . . ? O2 C10 C11 117.1(14) . . ? C9 C10 C11 125.8(13) . . ? O1 C3 C2 123.7(14) . . ? O1 C3 C4 108.2(14) . . ? C2 C3 C4 128.1(14) . . ? N3 C31 C30 124.1(14) . . ? N3 C31 H31 118.0 . . ? C30 C31 H31 118.0 . . ? C17 C16 C15 121.7(12) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? O6 C12 O5 118.9(17) . . ? O6 C12 C9 126.8(16) . . ? O5 C12 C9 114.3(15) . . ? C12 O5 C13 109.1(13) . . ? C22 C21 S1 120.3(12) . . ? C22 C21 S2 122.6(12) . . ? S1 C21 S2 116.7(9) . . ? C29 C30 C31 115.3(14) . . ? C29 C30 H30 122.3 . . ? C31 C30 H30 122.3 . . ? N3 C27 C28 124.3(14) . . ? N3 C27 H27 117.8 . . ? C28 C27 H27 117.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C35 C36 C32 121.9(16) . . ? C35 C36 H36 119.1 . . ? C32 C36 H36 119.1 . . ? C21 C22 S3 122.1(12) . . ? C21 C22 S4 124.5(12) . . ? S3 C22 S4 113.2(9) . . ? O3 C6 C7 106.0(16) . . ? O3 C6 H6A 110.5 . . ? C7 C6 H6A 110.5 . . ? O3 C6 H6B 110.5 . . ? C7 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C35 C36 124.8(18) . . ? N4 C35 H35 117.6 . . ? C36 C35 H35 117.6 . . ? C32 C33 C34 122.2(17) . . ? C32 C33 H33 118.9 . . ? C34 C33 H33 118.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C34 C33 123.5(16) . . ? N4 C34 H34 118.2 . . ? C33 C34 H34 118.2 . . ? C23 C24 S3 113.9(15) . . ? C23 C24 S5 126.7(16) . . ? S3 C24 S5 119.0(12) . . ? C24 C23 S4 120.7(15) . . ? C24 C23 S6 121.1(17) . . ? S4 C23 S6 118.1(12) . . ? S5 C26 H26A 109.5 . . ? S5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C14 C13 O5 89.9(13) . . ? C14 C13 H13A 113.7 . . ? O5 C13 H13A 113.7 . . ? C14 C13 H13B 113.7 . . ? O5 C13 H13B 113.7 . . ? H13A C13 H13B 110.9 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? S6 C25 H25A 109.5 . . ? S6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _refine_diff_density_max 0.531 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.099 _shelx_res_file ; TITL 111_a.res in P-1 111_a.res created by SHELXL-2018/3 at 14:36:01 on 01-Aug-2019 REM Old TITL 111 in P-1 REM SHELXT solution in P-1: R1 0.323, Rweak 0.048, Alpha 0.192 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C31 Fe N3 O11 S3 CELL 0.71073 11.3602 12.085 16.8416 91.216 109.716 111.473 ZERR 2 0.0105 0.01 0.014 0.02 0.022 0.021 LATT 1 SFAC C H Fe N O S UNIT 72 68 2 8 12 12 SIMU $C $N $O $S delu 0.02 0.01 O5 C13 C14 C25 S6 S5 C26 isor 0.02 0.01 O5 C13 C14 C25 S6 S5 C26 delu 0.01 0.01 C34 C35 C33 C36 N4 isor 0.01 0.01 C34 C35 C33 C36 N4 L.S. 50 PLAN -7 TEMP 83 BOND $H HTAB SIZE 0.15*0.12*0.08 LIST 6 fmap 2 acta SHEL 999 0.86 OMIT -1 1 1 OMIT -2 -6 2 OMIT -2 -7 2 OMIT -2 -6 4 OMIT 0 -1 11 OMIT -5 -5 3 OMIT -1 -1 13 OMIT -4 -6 5 OMIT -5 8 3 OMIT 0 9 1 REM REM REM WGHT 0.000010 3.100000 FVAR 0.26413 FE1 3 0.850908 0.229351 0.715227 11.00000 0.04193 0.07690 = 0.09339 -0.00246 0.03193 0.02034 S1 6 0.626694 0.088949 0.275598 11.00000 0.10275 0.08340 = 0.08588 0.00197 0.03652 0.03840 S2 6 0.735774 0.352077 0.302159 11.00000 0.10002 0.08041 = 0.10086 0.01576 0.04868 0.02096 S4 6 0.560928 0.338024 0.101299 11.00000 0.14263 0.13372 = 0.10769 0.02845 0.04263 0.05542 S3 6 0.474938 0.079282 0.079633 11.00000 0.15587 0.14374 = 0.08821 -0.01241 0.02846 0.07092 O1 5 0.948062 0.378555 0.803419 11.00000 0.05403 0.08556 = 0.07478 -0.00142 0.02535 0.02668 O2 5 0.818908 0.083944 0.771417 11.00000 0.03587 0.08773 = 0.07541 0.01384 0.02163 0.02597 N2 4 0.746706 0.109135 0.601202 11.00000 0.02537 0.06310 = 0.06203 -0.00184 0.02293 0.01097 N1 4 0.851853 0.349182 0.627860 11.00000 0.03693 0.06851 = 0.09903 -0.00054 0.04322 0.01197 S5 6 0.226475 0.030775 -0.072683 11.00000 0.21053 0.21701 = 0.12617 0.01468 -0.01858 0.05857 O3 5 0.937864 0.687601 0.648784 11.00000 0.10170 0.06031 = 0.14585 0.00496 0.05202 0.03149 N4 4 0.045551 0.231343 0.721060 11.00000 0.06923 0.05224 = 0.09494 0.01851 0.04492 0.02226 S6 6 0.318327 0.323487 -0.047828 11.00000 0.25926 0.23477 = 0.16388 0.06996 0.03578 0.12976 N3 4 0.657231 0.229509 0.719026 11.00000 0.03526 0.07278 = 0.07302 -0.00481 0.02698 0.00365 O6 5 0.568606 -0.246436 0.554206 11.00000 0.12811 0.07583 = 0.12912 -0.00448 0.04465 0.01767 C29 1 0.422826 0.235647 0.722518 11.00000 0.04359 0.06169 = 0.09225 -0.00446 0.03918 0.00643 C15 1 0.800342 0.289133 0.541098 11.00000 0.04385 0.06367 = 0.07236 -0.01007 0.03004 0.00639 C20 1 0.741249 0.163802 0.527956 11.00000 0.01701 0.08201 = 0.07696 -0.01156 0.01838 0.01071 C8 1 0.689592 -0.006145 0.596558 11.00000 0.03843 0.07153 = 0.05595 -0.00140 0.02195 0.01181 AFIX 43 H8 2 0.637989 -0.050869 0.541944 11.00000 -1.20000 AFIX 0 C1 1 0.881198 0.460805 0.643454 11.00000 0.04316 0.09319 = 0.08247 0.00671 0.02323 0.01666 AFIX 43 H1 2 0.863034 0.500174 0.596790 11.00000 -1.20000 AFIX 0 C18 1 0.689779 0.162332 0.377801 11.00000 0.04260 0.08817 = 0.06109 0.00973 0.02057 0.01915 C32 1 0.291592 0.233113 0.719378 11.00000 0.04728 0.03920 = 0.16927 0.00003 0.04294 0.02087 C17 1 0.745025 0.288855 0.392069 11.00000 0.05151 0.07306 = 0.07182 0.02613 0.02308 0.01803 C9 1 0.696408 -0.069283 0.662348 11.00000 0.06031 0.05731 = 0.09204 0.03553 0.05639 0.02724 C19 1 0.689522 0.104000 0.447670 11.00000 0.04730 0.05817 = 0.07570 -0.01659 0.02411 0.00443 AFIX 43 H19 2 0.652097 0.020163 0.438702 11.00000 -1.20000 AFIX 0 C2 1 0.938081 0.529572 0.724053 11.00000 0.05973 0.07576 = 0.08659 -0.03499 0.03801 0.00052 C5 1 0.965583 0.658210 0.727071 11.00000 0.06302 0.11348 = 0.11045 -0.01108 0.03929 0.02689 C28 1 0.441323 0.232382 0.649330 11.00000 0.03565 0.10488 = 0.08468 0.00721 0.01393 0.01857 AFIX 43 H28 2 0.373406 0.229002 0.598235 11.00000 -1.20000 AFIX 0 C10 1 0.761328 -0.026052 0.749356 11.00000 0.04575 0.06473 = 0.12955 0.01987 0.06806 0.01959 C3 1 0.968404 0.488709 0.797847 11.00000 0.06591 0.07333 = 0.11255 -0.01283 0.05272 0.01461 C31 1 0.636289 0.228849 0.788880 11.00000 0.06144 0.09330 = 0.07383 0.01455 0.02291 0.03077 AFIX 43 H31 2 0.704853 0.228773 0.838421 11.00000 -1.20000 AFIX 0 C16 1 0.799874 0.348604 0.473215 11.00000 0.05629 0.07314 = 0.08644 0.00452 0.04381 0.02053 AFIX 43 H16 2 0.838254 0.432446 0.482908 11.00000 -1.20000 AFIX 0 C12 1 0.620894 -0.201416 0.627212 11.00000 0.09086 0.09260 = 0.12144 0.03553 0.06751 0.02111 O4 5 1.003025 0.729484 0.786971 11.00000 0.20121 0.08084 = 0.13841 -0.03230 0.03601 0.04377 O5 5 0.612582 -0.270550 0.685260 11.00000 0.14892 0.10847 = 0.14827 0.02992 0.07259 0.03511 C21 1 0.639337 0.218928 0.232782 11.00000 0.07159 0.08713 = 0.11577 0.01540 0.05592 0.03803 C30 1 0.515651 0.228228 0.795629 11.00000 0.06309 0.14601 = 0.12327 0.04003 0.06291 0.04743 AFIX 43 H30 2 0.500869 0.223082 0.846731 11.00000 -1.20000 AFIX 0 C27 1 0.560867 0.234074 0.650662 11.00000 0.06620 0.10728 = 0.07681 0.00560 0.02818 0.01459 AFIX 43 H27 2 0.576397 0.238791 0.599797 11.00000 -1.20000 AFIX 0 C11 1 0.771973 -0.100395 0.817694 11.00000 0.15672 0.10874 = 0.10220 0.03148 0.07440 0.06102 AFIX 137 H11A 2 0.846537 -0.052925 0.868948 11.00000 -1.50000 H11B 2 0.787422 -0.168323 0.800200 11.00000 -1.50000 H11C 2 0.688889 -0.128319 0.828408 11.00000 -1.50000 AFIX 0 C36 1 0.193123 0.135821 0.722767 11.00000 0.11793 0.10724 = 0.17938 0.01337 0.05754 0.06950 AFIX 43 H36 2 0.205189 0.063724 0.725432 11.00000 -1.20000 AFIX 0 C22 1 0.565199 0.213158 0.149908 11.00000 0.08788 0.11322 = 0.11917 0.02098 0.04602 0.04492 C6 1 0.970898 0.811372 0.645669 11.00000 0.11582 0.09329 = 0.21272 0.02901 0.06372 0.02728 AFIX 23 H6A 2 1.067723 0.857439 0.675917 11.00000 -1.20000 H6B 2 0.921330 0.840859 0.671594 11.00000 -1.20000 AFIX 0 C4 1 1.030664 0.560163 0.888936 11.00000 0.15701 0.11124 = 0.08327 -0.02085 0.01259 0.04780 AFIX 137 H4A 2 0.988033 0.512717 0.924214 11.00000 -1.50000 H4B 2 1.016195 0.633662 0.887222 11.00000 -1.50000 H4C 2 1.126640 0.578724 0.912249 11.00000 -1.50000 AFIX 0 C35 1 0.072791 0.137352 0.722492 11.00000 0.10497 0.10216 = 0.16938 0.02039 0.05598 0.05501 AFIX 43 H35 2 0.006126 0.064801 0.723413 11.00000 -1.20000 AFIX 0 C33 1 0.264267 0.328354 0.716794 11.00000 0.09196 0.10286 = 0.18010 0.03534 0.06480 0.03825 AFIX 43 H33 2 0.328528 0.400771 0.713374 11.00000 -1.20000 AFIX 0 C7 1 0.932179 0.822067 0.556279 11.00000 0.14881 0.08173 = 0.24442 0.02468 0.03541 0.03308 AFIX 137 H7A 2 0.986375 0.797562 0.532518 11.00000 -1.50000 H7B 2 0.946736 0.904352 0.550269 11.00000 -1.50000 H7C 2 0.837649 0.771409 0.526544 11.00000 -1.50000 AFIX 0 C34 1 0.140611 0.325951 0.718987 11.00000 0.09684 0.08827 = 0.17653 0.02481 0.06072 0.04240 AFIX 43 H34 2 0.128165 0.397853 0.718907 11.00000 -1.20000 AFIX 0 C24 1 0.366539 0.131373 0.010393 11.00000 0.17164 0.15909 = 0.07636 0.01339 0.02611 0.07887 C23 1 0.409463 0.250515 0.022398 11.00000 0.14385 0.16034 = 0.14276 0.04814 0.05854 0.09419 C26 1 0.177023 -0.095488 -0.025116 11.00000 0.22195 0.20760 = 0.20090 0.01499 0.06711 0.07967 AFIX 137 H26A 2 0.178189 -0.162743 -0.055747 11.00000 -1.50000 H26B 2 0.086630 -0.113895 -0.026438 11.00000 -1.50000 H26C 2 0.238903 -0.079650 0.033141 11.00000 -1.50000 AFIX 0 C13 1 0.556563 -0.407110 0.641829 11.00000 0.19659 0.12013 = 0.20865 0.05921 0.06848 0.01896 AFIX 23 H13A 2 0.458327 -0.443967 0.612987 11.00000 -1.20000 H13B 2 0.601446 -0.419391 0.604652 11.00000 -1.20000 AFIX 0 C14 1 0.609994 -0.443298 0.733967 11.00000 0.23637 0.19646 = 0.24399 0.06209 0.07567 0.09031 AFIX 137 H14A 2 0.587730 -0.528480 0.727850 11.00000 -1.50000 H14B 2 0.567360 -0.422686 0.769078 11.00000 -1.50000 H14C 2 0.706980 -0.400461 0.760306 11.00000 -1.50000 AFIX 0 C25 1 0.273149 0.387341 0.017178 11.00000 0.29847 0.29289 = 0.29483 0.05272 0.09819 0.13494 AFIX 137 H25A 2 0.188856 0.331563 0.019095 11.00000 -1.50000 H25B 2 0.261631 0.457813 -0.002983 11.00000 -1.50000 H25C 2 0.342519 0.410017 0.073466 11.00000 -1.50000 AFIX 0 HKLF 4 REM 111_a.res in P-1 REM wR2 = 0.3013, GooF = S = 1.092, Restrained GooF = 1.099 for all data REM R1 = 0.1290 for 1890 Fo > 4sig(Fo) and 0.2822 for all 6358 data REM 484 parameters refined using 414 restraints END WGHT 0.1408 0.0000 REM Instructions for potential hydrogen bonds EQIV $3 -x+1, -y, -z+1 HTAB C27 O6_$3 HTAB C11 S3_$3 HTAB C4 O4 EQIV $1 x-1, y, z HTAB C35 O2_$1 EQIV $4 -x+1, -y+1, -z+1 HTAB C34 S2_$4 EQIV $5 x-1, y-1, z-1 HTAB C26 O4_$5 HTAB C26 S3 HTAB C25 S4 REM Highest difference peak 0.531, deepest hole -0.460, 1-sigma level 0.099 Q1 1 0.6051 -0.4393 0.5658 11.00000 0.05 0.46 Q2 1 0.7991 0.2204 0.6267 11.00000 0.05 0.45 Q3 1 0.8356 0.2164 0.7835 11.00000 0.05 0.42 Q4 1 0.8835 0.3411 0.7034 11.00000 0.05 0.41 Q5 1 0.6968 0.3198 0.3579 11.00000 0.05 0.40 Q6 1 0.8625 0.2600 0.6487 11.00000 0.05 0.38 Q7 1 0.2041 0.2850 0.6394 11.00000 0.05 0.38 ; _shelx_res_checksum 5800 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_H2L _database_code_depnum_ccdc_archive 'CCDC 1942248' _audit_update_record ; 2019-11-11 deposited with the CCDC. 2020-05-27 downloaded from the CCDC. ; _publcif_datablock.id {feb299df-fb7b-47c0-898c-5c8d0abee79f} _audit_creation_method SHELXL-2018/3 _shelx_SHELXL_version_number 2018/3 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H31 N3 O6 S6' _chemical_formula_weight 697.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 4.7950(15) _cell_length_b 25.807(8) _cell_length_c 26.902(8) _cell_angle_alpha 90 _cell_angle_beta 91.827(6) _cell_angle_gamma 90 _cell_volume 3327.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2413 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 20.41 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.393 _exptl_crystal_F_000 1456 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 0.455 _shelx_estimated_absorpt_T_min 0.914 _shelx_estimated_absorpt_T_max 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5960 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18416 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.578 _diffrn_reflns_theta_max 25.010 _diffrn_reflns_theta_full 25.010 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 5874 _reflns_number_gt 3423 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0630P)^2^+1.9001P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5874 _refine_ls_number_parameters 395 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1152 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1391 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 S1 S 1.1667(2) 0.35766(4) 0.28533(4) 0.0526(3) Uani 1 1 d . . . . . S2 S 1.0173(3) 0.27133(5) 0.35281(4) 0.0607(4) Uani 1 1 d . . . . . S3 S 1.5689(3) 0.40579(5) 0.36984(4) 0.0644(4) Uani 1 1 d . . . . . S4 S 1.4281(3) 0.32188(5) 0.43911(4) 0.0664(4) Uani 1 1 d . . . . . S5 S 1.9181(3) 0.46311(5) 0.44636(5) 0.0746(4) Uani 1 1 d . . . . . S6 S 1.7901(3) 0.36693(6) 0.52270(5) 0.0729(4) Uani 1 1 d . . . . . O1 O 0.1022(9) 0.14152(16) 0.14868(13) 0.0930(12) Uani 1 1 d . . . . . O2 O 0.0441(7) 0.25809(14) 0.09112(13) 0.0769(10) Uani 1 1 d . . . . . O3 O -0.0875(9) 0.12329(13) 0.31622(14) 0.0950(13) Uani 1 1 d . . . . . O4 O -0.2542(12) 0.06341(19) 0.26642(17) 0.147(2) Uani 1 1 d . . . . . O5 O 0.6193(9) 0.39949(13) 0.06313(13) 0.0865(12) Uani 1 1 d . . . . . O6 O 0.3111(9) 0.38116(15) 0.00266(13) 0.1000(13) Uani 1 1 d . . . . . N1 N 0.3218(7) 0.20267(13) 0.21613(12) 0.0486(9) Uani 1 1 d . . . . . H1 H 0.292442 0.198890 0.184637 0.058 Uiso 1 1 calc R U . . . N2 N 0.4371(7) 0.28666(12) 0.15449(12) 0.0459(8) Uani 1 1 d . . . . . H2 H 0.306227 0.264594 0.148237 0.055 Uiso 1 1 calc R U . . . C1 C 0.1832(9) 0.17240(16) 0.24622(15) 0.0480(11) Uani 1 1 d . . . . . H1A H 0.197297 0.180080 0.279981 0.058 Uiso 1 1 calc R U . . . C2 C 0.0192(9) 0.13046(16) 0.23254(16) 0.0533(11) Uani 1 1 d . . . . . C3 C -0.0141(11) 0.1156(2) 0.1807(2) 0.0700(14) Uani 1 1 d . . . . . C4 C -0.1898(14) 0.0703(2) 0.1637(2) 0.105(2) Uani 1 1 d . . . . . H4A H -0.378182 0.075270 0.173765 0.158 Uiso 1 1 calc R U . . . H4B H -0.116143 0.039047 0.178278 0.158 Uiso 1 1 calc R U . . . H4C H -0.187214 0.067737 0.128094 0.158 Uiso 1 1 calc R U . . . C5 C -0.1210(12) 0.1016(2) 0.2718(2) 0.0717(14) Uani 1 1 d . . . . . C6 C -0.2257(19) 0.0970(3) 0.3570(3) 0.138(3) Uani 1 1 d D U . . . H6A H -0.400087 0.081994 0.344673 0.165 Uiso 1 1 calc R U . . . H6B H -0.107822 0.069101 0.369658 0.165 Uiso 1 1 calc R U . . . C7 C -0.279(2) 0.1325(3) 0.3961(3) 0.185(4) Uani 1 1 d D U . . . H7A H -0.105659 0.145357 0.409950 0.278 Uiso 1 1 calc R U . . . H7B H -0.380008 0.115249 0.421538 0.278 Uiso 1 1 calc R U . . . H7C H -0.388401 0.160981 0.383163 0.278 Uiso 1 1 calc R U . . . C8 C 0.4848(9) 0.32210(16) 0.11991(15) 0.0502(11) Uani 1 1 d . . . . . H8 H 0.626722 0.345862 0.126761 0.060 Uiso 1 1 calc R U . . . C9 C 0.3414(10) 0.32674(16) 0.07447(15) 0.0527(11) Uani 1 1 d . . . . . C10 C 0.1248(10) 0.28987(19) 0.06013(17) 0.0602(12) Uani 1 1 d . . . . . C11 C 0.0041(12) 0.2875(2) 0.00845(17) 0.0828(17) Uani 1 1 d . . . . . H11A H -0.104676 0.256413 0.004434 0.124 Uiso 1 1 calc R U . . . H11B H 0.152124 0.287281 -0.014747 0.124 Uiso 1 1 calc R U . . . H11C H -0.112988 0.317103 0.002367 0.124 Uiso 1 1 calc R U . . . C12 C 0.4176(12) 0.37078(19) 0.04235(18) 0.0653(13) Uani 1 1 d . . . . . C13 C 0.6985(15) 0.4458(2) 0.0363(2) 0.104(2) Uani 1 1 d . . . . . H13A H 0.836768 0.437353 0.012037 0.124 Uiso 1 1 calc R U . . . H13B H 0.536836 0.460509 0.018883 0.124 Uiso 1 1 calc R U . . . C14 C 0.8117(17) 0.4825(3) 0.0717(3) 0.133(3) Uani 1 1 d . U . . . H14A H 0.665119 0.495292 0.091863 0.200 Uiso 1 1 calc R U . . . H14B H 0.894899 0.510778 0.054446 0.200 Uiso 1 1 calc R U . . . H14C H 0.950887 0.465748 0.092584 0.200 Uiso 1 1 calc R U . . . C15 C 0.5159(8) 0.24098(15) 0.23232(14) 0.0427(10) Uani 1 1 d . . . . . C16 C 0.6456(9) 0.23799(15) 0.27904(15) 0.0480(11) Uani 1 1 d . . . . . H16 H 0.601246 0.210839 0.300095 0.058 Uiso 1 1 calc R U . . . C17 C 0.8388(8) 0.27438(15) 0.29494(14) 0.0433(10) Uani 1 1 d . . . . . C18 C 0.9108(8) 0.31430(15) 0.26289(14) 0.0423(10) Uani 1 1 d . . . . . C19 C 0.7849(8) 0.31793(15) 0.21603(14) 0.0452(10) Uani 1 1 d . . . . . H19 H 0.835782 0.344466 0.194766 0.054 Uiso 1 1 calc R U . . . C20 C 0.5831(8) 0.28234(15) 0.20042(14) 0.0411(9) Uani 1 1 d . . . . . C21 C 1.2042(9) 0.32937(15) 0.34478(15) 0.0472(10) Uani 1 1 d . . . . . C22 C 1.3718(9) 0.34963(16) 0.38018(15) 0.0527(11) Uani 1 1 d . . . . . C23 C 1.6383(9) 0.37268(17) 0.46284(16) 0.0536(11) Uani 1 1 d . . . . . C24 C 1.6965(9) 0.41086(17) 0.43170(16) 0.0556(12) Uani 1 1 d . . . . . C25 C 1.5439(11) 0.3306(2) 0.55646(18) 0.0775(15) Uani 1 1 d . . . . . H25A H 1.372083 0.349581 0.557741 0.116 Uiso 1 1 calc R U . . . H25B H 1.616210 0.324639 0.589654 0.116 Uiso 1 1 calc R U . . . H25C H 1.510511 0.297964 0.540201 0.116 Uiso 1 1 calc R U . . . C26 C 1.6880(12) 0.51677(19) 0.4356(2) 0.0885(18) Uani 1 1 d . . . . . H26A H 1.634389 0.518260 0.400917 0.133 Uiso 1 1 calc R U . . . H26B H 1.781379 0.548321 0.445094 0.133 Uiso 1 1 calc R U . . . H26C H 1.524756 0.512537 0.454922 0.133 Uiso 1 1 calc R U . . . N3 N 0.2567(19) 0.4272(3) 0.1755(3) 0.142(3) Uani 1 1 d . . . . . C27 C 0.430(2) 0.4446(3) 0.1993(3) 0.108(3) Uani 1 1 d . U . . . C28 C 0.6416(17) 0.4671(3) 0.2307(3) 0.131(3) Uani 1 1 d . . . . . H28A H 0.620723 0.504099 0.230657 0.196 Uiso 1 1 calc R U . . . H28B H 0.821681 0.458186 0.218600 0.196 Uiso 1 1 calc R U . . . H28C H 0.625229 0.454210 0.263921 0.196 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 S1 0.0610(8) 0.0505(7) 0.0458(6) 0.0006(5) -0.0039(5) -0.0107(6) S2 0.0757(9) 0.0603(7) 0.0452(7) 0.0081(5) -0.0117(6) -0.0115(6) S3 0.0751(9) 0.0658(8) 0.0517(7) 0.0016(6) -0.0073(6) -0.0134(7) S4 0.0849(10) 0.0666(8) 0.0469(7) 0.0028(6) -0.0126(6) -0.0172(7) S5 0.0578(8) 0.0707(9) 0.0937(10) -0.0008(7) -0.0241(7) -0.0126(7) S6 0.0648(9) 0.0976(10) 0.0552(8) 0.0057(7) -0.0179(6) -0.0127(7) O1 0.109(3) 0.110(3) 0.060(2) -0.010(2) 0.002(2) -0.049(3) O2 0.078(3) 0.083(2) 0.068(2) 0.0116(19) -0.0207(19) -0.022(2) O3 0.151(4) 0.070(2) 0.066(2) 0.016(2) 0.032(2) -0.026(2) O4 0.210(6) 0.114(4) 0.118(4) 0.003(3) 0.029(3) -0.104(4) O5 0.119(3) 0.065(2) 0.074(2) 0.0296(18) -0.015(2) -0.027(2) O6 0.126(4) 0.111(3) 0.061(2) 0.036(2) -0.022(2) -0.015(3) N1 0.056(2) 0.050(2) 0.0399(19) 0.0082(16) -0.0013(17) -0.0075(18) N2 0.050(2) 0.042(2) 0.045(2) 0.0057(16) -0.0044(16) -0.0054(16) C1 0.056(3) 0.044(2) 0.043(2) 0.0052(19) -0.004(2) 0.000(2) C2 0.053(3) 0.048(3) 0.059(3) 0.003(2) 0.003(2) -0.006(2) C3 0.068(4) 0.072(3) 0.070(4) -0.009(3) -0.003(3) -0.016(3) C4 0.119(5) 0.100(5) 0.096(4) -0.026(3) -0.008(4) -0.049(4) C5 0.092(4) 0.051(3) 0.073(4) 0.006(3) 0.010(3) -0.010(3) C6 0.194(7) 0.113(5) 0.109(5) 0.041(4) 0.049(5) -0.033(5) C7 0.255(9) 0.176(7) 0.128(6) 0.017(5) 0.064(6) -0.035(6) C8 0.058(3) 0.044(2) 0.048(3) 0.003(2) -0.002(2) 0.001(2) C9 0.063(3) 0.050(3) 0.045(3) 0.004(2) -0.001(2) 0.006(2) C10 0.067(3) 0.060(3) 0.053(3) -0.001(2) -0.006(2) 0.012(3) C11 0.099(4) 0.090(4) 0.057(3) -0.004(3) -0.025(3) -0.002(3) C12 0.085(4) 0.060(3) 0.050(3) 0.009(2) 0.000(3) 0.003(3) C13 0.152(6) 0.071(4) 0.088(4) 0.034(3) 0.000(4) -0.025(4) C14 0.183(7) 0.101(5) 0.115(5) 0.024(4) -0.004(5) -0.050(5) C15 0.046(3) 0.040(2) 0.042(2) 0.0011(18) -0.0004(19) 0.0012(19) C16 0.056(3) 0.044(2) 0.043(2) 0.0099(19) 0.001(2) 0.001(2) C17 0.049(3) 0.042(2) 0.038(2) 0.0025(18) -0.0016(19) 0.002(2) C18 0.046(3) 0.041(2) 0.039(2) -0.0019(18) 0.0012(19) 0.0033(19) C19 0.051(3) 0.040(2) 0.045(2) 0.0041(18) 0.003(2) 0.000(2) C20 0.042(2) 0.044(2) 0.037(2) 0.0051(18) 0.0034(18) 0.0016(19) C21 0.051(3) 0.048(2) 0.042(2) -0.0044(19) -0.001(2) 0.004(2) C22 0.060(3) 0.052(3) 0.046(3) -0.006(2) -0.006(2) 0.002(2) C23 0.051(3) 0.059(3) 0.051(3) -0.004(2) -0.006(2) 0.003(2) C24 0.049(3) 0.059(3) 0.058(3) 0.000(2) -0.011(2) 0.000(2) C25 0.070(4) 0.103(4) 0.059(3) 0.006(3) -0.009(3) 0.006(3) C26 0.093(4) 0.061(3) 0.110(5) 0.013(3) -0.033(4) -0.011(3) N3 0.164(8) 0.150(7) 0.114(6) 0.014(5) 0.025(5) 0.042(6) C27 0.118(6) 0.100(5) 0.108(6) 0.027(4) 0.032(5) 0.038(5) C28 0.111(6) 0.097(6) 0.184(8) 0.016(5) 0.023(6) 0.035(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 C18 1.754(4) . ? S1 C21 1.762(4) . ? S2 C17 1.754(4) . ? S2 C21 1.762(4) . ? S3 C22 1.757(5) . ? S3 C24 1.759(4) . ? S4 C22 1.752(4) . ? S4 C23 1.761(4) . ? S5 C24 1.754(5) . ? S5 C26 1.788(5) . ? S6 C23 1.752(4) . ? S6 C25 1.779(5) . ? O1 C3 1.238(6) . ? O2 C10 1.240(5) . ? O3 C5 1.326(6) . ? O3 C6 1.466(6) . ? O4 C5 1.180(6) . ? O5 C12 1.328(6) . ? O5 C13 1.454(6) . ? O6 C12 1.199(5) . ? N1 C1 1.320(5) . ? N1 C15 1.417(5) . ? N1 H1 0.8600 . ? N2 C8 1.330(5) . ? N2 C20 1.405(5) . ? N2 H2 0.8600 . ? C1 C2 1.381(6) . ? C1 H1A 0.9300 . ? C2 C3 1.449(6) . ? C2 C5 1.472(6) . ? C3 C4 1.504(7) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C6 C7 1.426(7) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.389(6) . ? C8 H8 0.9300 . ? C9 C10 1.452(6) . ? C9 C12 1.481(6) . ? C10 C11 1.490(6) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 C14 1.436(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.387(5) . ? C15 C20 1.413(5) . ? C16 C17 1.377(5) . ? C16 H16 0.9300 . ? C17 C18 1.394(5) . ? C18 C19 1.383(5) . ? C19 C20 1.389(5) . ? C19 H19 0.9300 . ? C21 C22 1.333(5) . ? C23 C24 1.328(6) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? N3 C27 1.125(10) . ? C27 C28 1.424(11) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? 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 C18 S1 C21 95.62(19) . . ? C17 S2 C21 95.09(19) . . ? C22 S3 C24 94.8(2) . . ? C22 S4 C23 95.4(2) . . ? C24 S5 C26 101.1(2) . . ? C23 S6 C25 104.5(2) . . ? C5 O3 C6 115.7(5) . . ? C12 O5 C13 116.6(4) . . ? C1 N1 C15 124.3(3) . . ? C1 N1 H1 117.9 . . ? C15 N1 H1 117.9 . . ? C8 N2 C20 125.3(4) . . ? C8 N2 H2 117.4 . . ? C20 N2 H2 117.4 . . ? N1 C1 C2 126.5(4) . . ? N1 C1 H1A 116.8 . . ? C2 C1 H1A 116.8 . . ? C1 C2 C3 120.5(4) . . ? C1 C2 C5 118.4(4) . . ? C3 C2 C5 121.1(4) . . ? O1 C3 C2 119.3(4) . . ? O1 C3 C4 117.9(5) . . ? C2 C3 C4 122.8(5) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O4 C5 O3 120.8(5) . . ? O4 C5 C2 126.4(5) . . ? O3 C5 C2 112.8(4) . . ? C7 C6 O3 110.5(6) . . ? C7 C6 H6A 109.5 . . ? O3 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? O3 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C9 125.7(4) . . ? N2 C8 H8 117.1 . . ? C9 C8 H8 117.1 . . ? C8 C9 C10 120.5(4) . . ? C8 C9 C12 117.1(4) . . ? C10 C9 C12 122.4(4) . . ? O2 C10 C9 119.4(4) . . ? O2 C10 C11 118.6(5) . . ? C9 C10 C11 121.9(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O6 C12 O5 122.3(5) . . ? O6 C12 C9 125.8(5) . . ? O5 C12 C9 111.9(4) . . ? C14 C13 O5 108.1(5) . . ? C14 C13 H13A 110.1 . . ? O5 C13 H13A 110.1 . . ? C14 C13 H13B 110.1 . . ? O5 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 N1 120.7(3) . . ? C16 C15 C20 119.2(4) . . ? N1 C15 C20 120.1(3) . . ? C17 C16 C15 121.4(4) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C18 119.3(4) . . ? C16 C17 S2 123.3(3) . . ? C18 C17 S2 117.3(3) . . ? C19 C18 C17 120.3(4) . . ? C19 C18 S1 123.4(3) . . ? C17 C18 S1 116.3(3) . . ? C18 C19 C20 120.7(4) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C19 C20 N2 122.4(3) . . ? C19 C20 C15 119.1(3) . . ? N2 C20 C15 118.5(4) . . ? C22 C21 S1 121.9(3) . . ? C22 C21 S2 122.9(3) . . ? S1 C21 S2 115.2(2) . . ? C21 C22 S4 123.9(4) . . ? C21 C22 S3 121.7(3) . . ? S4 C22 S3 114.3(2) . . ? C24 C23 S6 123.6(3) . . ? C24 C23 S4 116.9(3) . . ? S6 C23 S4 119.1(3) . . ? C23 C24 S5 124.5(3) . . ? C23 C24 S3 117.9(3) . . ? S5 C24 S3 117.4(3) . . ? S6 C25 H25A 109.5 . . ? S6 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S6 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S5 C26 H26A 109.5 . . ? S5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 177.8(10) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 C15 N1 C1 C2 -171.4(4) . . . . ? N1 C1 C2 C3 0.2(7) . . . . ? N1 C1 C2 C5 -179.6(4) . . . . ? C1 C2 C3 O1 -1.3(8) . . . . ? C5 C2 C3 O1 178.4(5) . . . . ? C1 C2 C3 C4 180.0(5) . . . . ? C5 C2 C3 C4 -0.3(8) . . . . ? C6 O3 C5 O4 -0.1(9) . . . . ? C6 O3 C5 C2 179.0(5) . . . . ? C1 C2 C5 O4 -175.4(6) . . . . ? C3 C2 C5 O4 4.8(9) . . . . ? C1 C2 C5 O3 5.5(7) . . . . ? C3 C2 C5 O3 -174.3(4) . . . . ? C5 O3 C6 C7 -155.3(8) . . . . ? C20 N2 C8 C9 -179.9(4) . . . . ? N2 C8 C9 C10 -2.5(7) . . . . ? N2 C8 C9 C12 176.8(4) . . . . ? C8 C9 C10 O2 9.0(7) . . . . ? C12 C9 C10 O2 -170.3(4) . . . . ? C8 C9 C10 C11 -168.3(4) . . . . ? C12 C9 C10 C11 12.4(7) . . . . ? C13 O5 C12 O6 2.5(8) . . . . ? C13 O5 C12 C9 -176.1(5) . . . . ? C8 C9 C12 O6 -178.3(5) . . . . ? C10 C9 C12 O6 1.1(8) . . . . ? C8 C9 C12 O5 0.3(6) . . . . ? C10 C9 C12 O5 179.6(4) . . . . ? C12 O5 C13 C14 153.8(6) . . . . ? C1 N1 C15 C16 22.4(6) . . . . ? C1 N1 C15 C20 -158.7(4) . . . . ? N1 C15 C16 C17 178.7(4) . . . . ? C20 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C18 -1.7(6) . . . . ? C15 C16 C17 S2 -177.9(3) . . . . ? C21 S2 C17 C16 -178.7(4) . . . . ? C21 S2 C17 C18 5.1(4) . . . . ? C16 C17 C18 C19 1.4(6) . . . . ? S2 C17 C18 C19 177.8(3) . . . . ? C16 C17 C18 S1 -177.9(3) . . . . ? S2 C17 C18 S1 -1.5(4) . . . . ? C21 S1 C18 C19 177.8(4) . . . . ? C21 S1 C18 C17 -2.9(3) . . . . ? C17 C18 C19 C20 0.7(6) . . . . ? S1 C18 C19 C20 -180.0(3) . . . . ? C18 C19 C20 N2 175.6(4) . . . . ? C18 C19 C20 C15 -2.6(6) . . . . ? C8 N2 C20 C19 4.6(6) . . . . ? C8 N2 C20 C15 -177.1(4) . . . . ? C16 C15 C20 C19 2.3(6) . . . . ? N1 C15 C20 C19 -176.6(4) . . . . ? C16 C15 C20 N2 -176.0(4) . . . . ? N1 C15 C20 N2 5.1(6) . . . . ? C18 S1 C21 C22 -176.3(4) . . . . ? C18 S1 C21 S2 6.3(3) . . . . ? C17 S2 C21 C22 175.8(4) . . . . ? C17 S2 C21 S1 -6.9(3) . . . . ? S1 C21 C22 S4 -177.4(2) . . . . ? S2 C21 C22 S4 -0.3(6) . . . . ? S1 C21 C22 S3 -0.4(5) . . . . ? S2 C21 C22 S3 176.7(2) . . . . ? C23 S4 C22 C21 -175.5(4) . . . . ? C23 S4 C22 S3 7.3(3) . . . . ? C24 S3 C22 C21 174.6(4) . . . . ? C24 S3 C22 S4 -8.2(3) . . . . ? C25 S6 C23 C24 154.8(4) . . . . ? C25 S6 C23 S4 -32.8(3) . . . . ? C22 S4 C23 C24 -3.2(4) . . . . ? C22 S4 C23 S6 -176.1(3) . . . . ? S6 C23 C24 S5 -3.5(6) . . . . ? S4 C23 C24 S5 -176.0(3) . . . . ? S6 C23 C24 S3 170.4(3) . . . . ? S4 C23 C24 S3 -2.1(5) . . . . ? C26 S5 C24 C23 -121.8(5) . . . . ? C26 S5 C24 S3 64.2(3) . . . . ? C22 S3 C24 C23 6.3(4) . . . . ? C22 S3 C24 S5 -179.4(3) . . . . ? _refine_diff_density_max 1.222 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.057 _shelx_res_file ; TITL 1 in P2(1)/c 1.res created by SHELXL-2018/3 at 22:57:37 on 06-Nov-2019 CELL 0.71073 4.795 25.8069 26.9017 90 91.827 90 ZERR 4 0.0015 0.0077 0.0081 0 0.006 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S UNIT 112 124 12 24 24 DFIX 1.56 0.01 C6 C7 DELU C6 C7 C27 C14 ISOR 0.01 0.01 C6 C7 C27 C14 L.S. 50 PLAN 7 SIZE 0.2 0.15 0.12 TEMP 23 CONF BOND MORE -1 BOND $H fmap 2 acta OMIT -1 50.02 OMIT 0 0 2 OMIT 0 1 1 OMIT 0 0 4 OMIT 0 3 2 OMIT 0 10 1 OMIT 0 3 9 OMIT -1 2 4 OMIT -1 5 1 REM REM REM WGHT 0.063000 1.900100 FVAR 0.12748 S1 5 1.166727 0.357664 0.285325 11.00000 0.06100 0.05055 = 0.04584 0.00059 -0.00389 -0.01074 S2 5 1.017329 0.271325 0.352813 11.00000 0.07570 0.06030 = 0.04520 0.00813 -0.01169 -0.01148 S3 5 1.568884 0.405788 0.369841 11.00000 0.07510 0.06580 = 0.05168 0.00161 -0.00726 -0.01336 S4 5 1.428108 0.321877 0.439109 11.00000 0.08490 0.06655 = 0.04690 0.00277 -0.01256 -0.01721 S5 5 1.918106 0.463113 0.446365 11.00000 0.05783 0.07065 = 0.09374 -0.00078 -0.02415 -0.01255 S6 5 1.790055 0.366931 0.522696 11.00000 0.06478 0.09756 = 0.05520 0.00575 -0.01791 -0.01268 O1 4 0.102164 0.141522 0.148676 11.00000 0.10933 0.10966 = 0.05988 -0.00968 0.00166 -0.04916 O2 4 0.044132 0.258090 0.091122 11.00000 0.07838 0.08305 = 0.06773 0.01165 -0.02071 -0.02238 O3 4 -0.087547 0.123285 0.316217 11.00000 0.15050 0.07038 = 0.06603 0.01624 0.03191 -0.02594 O4 4 -0.254195 0.063405 0.266425 11.00000 0.20957 0.11385 = 0.11795 0.00313 0.02853 -0.10408 O5 4 0.619289 0.399492 0.063134 11.00000 0.11874 0.06535 = 0.07441 0.02955 -0.01472 -0.02691 O6 4 0.311082 0.381156 0.002663 11.00000 0.12598 0.11128 = 0.06122 0.03601 -0.02182 -0.01539 N1 3 0.321817 0.202669 0.216132 11.00000 0.05603 0.04955 = 0.03991 0.00819 -0.00130 -0.00749 AFIX 43 H1 2 0.292442 0.198890 0.184637 11.00000 -1.20000 AFIX 0 N2 3 0.437090 0.286661 0.154490 11.00000 0.05033 0.04244 = 0.04466 0.00574 -0.00441 -0.00536 AFIX 43 H2 2 0.306227 0.264594 0.148237 11.00000 -1.20000 AFIX 0 C1 1 0.183163 0.172401 0.246218 11.00000 0.05646 0.04361 = 0.04343 0.00522 -0.00407 -0.00012 AFIX 43 H1A 2 0.197297 0.180080 0.279981 11.00000 -1.20000 AFIX 0 C2 1 0.019176 0.130461 0.232541 11.00000 0.05265 0.04809 = 0.05936 0.00297 0.00269 -0.00594 C3 1 -0.014109 0.115610 0.180732 11.00000 0.06767 0.07180 = 0.07009 -0.00920 -0.00314 -0.01614 C4 1 -0.189796 0.070322 0.163675 11.00000 0.11880 0.10009 = 0.09554 -0.02617 -0.00822 -0.04880 AFIX 137 H4A 2 -0.378182 0.075270 0.173765 11.00000 -1.50000 H4B 2 -0.116143 0.039047 0.178278 11.00000 -1.50000 H4C 2 -0.187214 0.067737 0.128094 11.00000 -1.50000 AFIX 0 C5 1 -0.121026 0.101551 0.271753 11.00000 0.09163 0.05139 = 0.07259 0.00634 0.00972 -0.01018 C6 1 -0.225667 0.096977 0.356978 11.00000 0.19362 0.11349 = 0.10897 0.04125 0.04898 -0.03295 AFIX 23 H6A 2 -0.400087 0.081994 0.344673 11.00000 -1.20000 H6B 2 -0.107822 0.069101 0.369658 11.00000 -1.20000 AFIX 0 C7 1 -0.279318 0.132548 0.396105 11.00000 0.25535 0.17642 = 0.12785 0.01727 0.06435 -0.03482 AFIX 137 H7A 2 -0.105659 0.145357 0.409950 11.00000 -1.50000 H7B 2 -0.380008 0.115249 0.421538 11.00000 -1.50000 H7C 2 -0.388401 0.160981 0.383163 11.00000 -1.50000 AFIX 0 C8 1 0.484829 0.322100 0.119914 11.00000 0.05803 0.04406 = 0.04844 0.00275 -0.00182 0.00084 AFIX 43 H8 2 0.626722 0.345862 0.126761 11.00000 -1.20000 AFIX 0 C9 1 0.341373 0.326741 0.074472 11.00000 0.06319 0.04959 = 0.04522 0.00352 -0.00147 0.00638 C10 1 0.124811 0.289866 0.060130 11.00000 0.06660 0.06039 = 0.05319 -0.00084 -0.00570 0.01241 C11 1 0.004079 0.287451 0.008449 11.00000 0.09914 0.09010 = 0.05733 -0.00435 -0.02459 -0.00189 AFIX 137 H11A 2 -0.104676 0.256413 0.004434 11.00000 -1.50000 H11B 2 0.152124 0.287281 -0.014747 11.00000 -1.50000 H11C 2 -0.112988 0.317103 0.002367 11.00000 -1.50000 AFIX 0 C12 1 0.417595 0.370785 0.042350 11.00000 0.08526 0.06009 = 0.05029 0.00896 0.00046 0.00303 C13 1 0.698545 0.445842 0.036300 11.00000 0.15215 0.07096 = 0.08777 0.03387 0.00038 -0.02484 AFIX 23 H13A 2 0.836768 0.437353 0.012037 11.00000 -1.20000 H13B 2 0.536836 0.460509 0.018883 11.00000 -1.20000 AFIX 0 C14 1 0.811747 0.482450 0.071736 11.00000 0.18341 0.10115 = 0.11531 0.02446 -0.00396 -0.05044 AFIX 137 H14A 2 0.665119 0.495292 0.091863 11.00000 -1.50000 H14B 2 0.894899 0.510778 0.054446 11.00000 -1.50000 H14C 2 0.950887 0.465748 0.092584 11.00000 -1.50000 AFIX 0 C15 1 0.515880 0.240976 0.232316 11.00000 0.04609 0.04009 = 0.04184 0.00111 -0.00038 0.00124 C16 1 0.645625 0.237994 0.279040 11.00000 0.05627 0.04434 = 0.04339 0.00992 0.00080 0.00059 AFIX 43 H16 2 0.601246 0.210839 0.300095 11.00000 -1.20000 AFIX 0 C17 1 0.838802 0.274377 0.294945 11.00000 0.04891 0.04244 = 0.03837 0.00247 -0.00161 0.00217 C18 1 0.910774 0.314304 0.262892 11.00000 0.04643 0.04115 = 0.03943 -0.00192 0.00119 0.00328 C19 1 0.784851 0.317929 0.216033 11.00000 0.05064 0.03990 = 0.04503 0.00406 0.00316 -0.00030 AFIX 43 H19 2 0.835782 0.344466 0.194766 11.00000 -1.20000 AFIX 0 C20 1 0.583112 0.282339 0.200418 11.00000 0.04236 0.04371 = 0.03737 0.00511 0.00338 0.00157 C21 1 1.204228 0.329372 0.344776 11.00000 0.05097 0.04846 = 0.04209 -0.00443 -0.00070 0.00372 C22 1 1.371823 0.349626 0.380184 11.00000 0.05995 0.05199 = 0.04578 -0.00561 -0.00566 0.00170 C23 1 1.638340 0.372685 0.462840 11.00000 0.05084 0.05874 = 0.05061 -0.00433 -0.00585 0.00301 C24 1 1.696476 0.410855 0.431696 11.00000 0.04898 0.05932 = 0.05761 -0.00018 -0.01073 -0.00001 C25 1 1.543875 0.330596 0.556460 11.00000 0.07004 0.10299 = 0.05884 0.00605 -0.00877 0.00585 AFIX 137 H25A 2 1.372083 0.349581 0.557741 11.00000 -1.50000 H25B 2 1.616210 0.324639 0.589654 11.00000 -1.50000 H25C 2 1.510511 0.297964 0.540201 11.00000 -1.50000 AFIX 0 C26 1 1.688011 0.516772 0.435575 11.00000 0.09282 0.06055 = 0.10965 0.01334 -0.03329 -0.01065 AFIX 137 H26A 2 1.634389 0.518260 0.400917 11.00000 -1.50000 H26B 2 1.781379 0.548321 0.445094 11.00000 -1.50000 H26C 2 1.524756 0.512537 0.454922 11.00000 -1.50000 AFIX 0 N3 3 0.256706 0.427192 0.175544 11.00000 0.16368 0.15024 = 0.11408 0.01406 0.02545 0.04234 C27 1 0.429961 0.444584 0.199271 11.00000 0.11847 0.10011 = 0.10808 0.02744 0.03243 0.03806 C28 1 0.641631 0.467103 0.230668 11.00000 0.11138 0.09739 = 0.18429 0.01584 0.02260 0.03472 AFIX 137 H28A 2 0.620723 0.504099 0.230657 11.00000 -1.50000 H28B 2 0.821681 0.458186 0.218600 11.00000 -1.50000 H28C 2 0.625229 0.454210 0.263921 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P2(1)/c REM wR2 = 0.1608, GooF = S = 1.029, Restrained GooF = 1.070 for all data REM R1 = 0.0621 for 3423 Fo > 4sig(Fo) and 0.1152 for all 5874 data REM 395 parameters refined using 26 restraints END WGHT 0.0780 0.9285 REM Highest difference peak 1.222, deepest hole -0.324, 1-sigma level 0.057 Q1 1 0.2148 0.2267 0.1530 11.00000 0.05 1.22 Q2 1 -0.4518 0.1147 0.3709 11.00000 0.05 0.48 Q3 1 -0.0586 0.1194 0.3974 11.00000 0.05 0.34 Q4 1 1.5743 0.3419 0.4603 11.00000 0.05 0.25 Q5 1 1.1961 0.3437 0.3720 11.00000 0.05 0.23 Q6 1 0.8428 0.2519 0.2815 11.00000 0.05 0.23 Q7 1 1.6400 0.3801 0.4976 11.00000 0.05 0.22 ; _shelx_res_checksum 63863 _publcif_funding_html ; ;