#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 3 _journal_year 2020 _journal_page_first 250 _journal_page_last 254 #=============================================================================== data_KOKO497 _publ_contact_author_email 'rusanova_j@yahoo.com' _publ_contact_author_address ; Department of Chemistry, Taras Shevchenko National University of Kyiv, 64/13, Volodymyrska str., Kyiv 01601, Ukraine ; # Loop of author details loop_ _publ_author_name _publ_author_address _publ_author_footnote _publ_author_email 'Rusanova, Julia A.' ; Department of Chemistry, Taras Shevchenko National University of Kyiv, 64/13, Volodymyrska str., Kyiv 01601, Ukraine ; . ; rusanova_j@yahoo.com ; 'Chygorin, Eduard N.' ; Department of Chemistry, Taras Shevchenko National University of Kyiv, 64/13, Volodymyrska str., Kyiv 01601, Ukraine ; . ; chygorin@mail.univ.kiev.ua ; 'Kokozay, Volodymyr N.' ; Department of Chemistry, Taras Shevchenko National University of Kyiv, 64/13, Volodymyrska str., Kyiv 01601, Ukraine ; . ; kokozay@univ.kiev.ua ; 'Omelchenko, Irina V.' ; STC "Institute for Single Crystals" National Academy of Sciences of Ukraine 60 Lenina ave. Kharkiv, 61072 Ukraine ; . ; irina@xray.isc.kharkov.com ; _audit_update_record 2020-03-12 # Formatted by publCIF _audit_creation_method 'SHELXL-2016/4' _shelx_SHELXL_version_number '2016/4' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H38 Cl2 Co2 Fe2 N8 O20, 6(C2 H6 O S)' _chemical_formula_sum 'C52 H74 Cl2 Co2 Fe2 N8 O26 S6' _chemical_formula_weight 1720.01 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Co' 'Co' 0.3494 0.9721 '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 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 16.353(3) _cell_length_b 15.234(2) _cell_length_c 15.201(3) _cell_angle_alpha 90 _cell_angle_beta 113.99(2) _cell_angle_gamma 90 _cell_volume 3460.0(12) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1096 _cell_measurement_theta_min 2.8441 _cell_measurement_theta_max 28.5698 _exptl_crystal_description block _exptl_crystal_colour 'clear light brown' _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.651 _exptl_crystal_F_000 1772 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 1.225 _shelx_estimated_absorpt_T_min 0.887 _shelx_estimated_absorpt_T_max 0.941 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8873 _exptl_absorpt_correction_T_max 0.9413 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, 2011, Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator graphite _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.1827 _diffrn_detector_type Sapphire3 _diffrn_reflns_number 14130 _diffrn_reflns_av_unetI/netI 0.2148 _diffrn_reflns_av_R_equivalents 0.1051 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.850 _diffrn_reflns_theta_max 28.633 _diffrn_reflns_theta_full 26.000 _diffrn_measured_fraction_theta_max 0.873 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.873 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.873 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 7748 _reflns_number_gt 3314 _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 ; CrysAlisPro, Agilent Technologies, 2014 ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, 2014 ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, 2014 ; _computing_structure_solution 'SHELXT (Sheldrick, 2015a)' _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_diff_density_max 0.978 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.126 _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^)+(0.0646P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7748 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2083 _refine_ls_R_factor_gt 0.0914 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.1694 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _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, All O(H) groups 2.a Riding coordinates: O8(H8) 2.b Ternary CH refined with riding coordinates: C16(H16), C19(H19) 2.c Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C17(H17A,H17B), C18(H18A,H18B), C20(H20A,H20B) 2.d Me refined with riding coordinates: C1S(H1SA,H1SB,H1SC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC), C4S(H4SA,H4SB, H4SC), C5S(H5SA,H5SB,H5SC), C6S(H6SA,H6SB,H6SC) 2.e Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C6(H6), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14) ; 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 0.41507(8) 0.53259(7) 0.40453(7) 0.0305(3) Uani 1 1 d . . . . . S1S S 0.0399(2) -0.01226(18) -0.34822(19) 0.0656(8) Uani 1 1 d . . . . . CO1 Co 0.42423(8) 0.45222(7) 0.22628(7) 0.0320(3) Uani 1 1 d . . . . . CL1 Cl 0.29102(14) 0.52798(14) 0.44012(14) 0.0394(5) Uani 1 1 d . . . . . O1 O 0.3993(4) 0.3416(4) 0.1691(4) 0.0372(14) Uani 1 1 d . . . . . C1 C 0.2538(6) 0.3770(5) 0.0485(5) 0.034(2) Uani 1 1 d . . . . . N1 N 0.3184(5) 0.5063(4) 0.1406(4) 0.0332(17) Uani 1 1 d . . . . . O1S O -0.0533(4) 0.0222(5) -0.4049(5) 0.080(2) Uani 1 1 d . . . . . C1S C 0.1092(6) 0.0806(7) -0.3171(6) 0.059(3) Uani 1 1 d . . . . . H1SA H 0.171253 0.062527 -0.279821 0.088 Uiso 1 1 calc R U . . . H1SB H 0.104794 0.110780 -0.375806 0.088 Uiso 1 1 calc R U . . . H1SC H 0.090142 0.120403 -0.278374 0.088 Uiso 1 1 calc R U . . . S2S S 0.13770(18) 0.68051(17) 0.51724(19) 0.0576(8) Uani 1 1 d . . . . . N2 N 0.5338(5) 0.4030(4) 0.3171(4) 0.0311(16) Uani 1 1 d . . . . . O2S O 0.2148(4) 0.6942(4) 0.6083(5) 0.067(2) Uani 1 1 d . . . . . C2 C 0.3258(6) 0.3203(5) 0.0988(6) 0.035(2) Uani 1 1 d . . . . . O2 O 0.0289(5) 0.2760(5) -0.1679(5) 0.069(2) Uani 1 1 d . . . . . C2S C 0.0436(7) -0.0357(7) -0.2331(6) 0.066(3) Uani 1 1 d . . . . . H2SA H 0.102868 -0.058697 -0.191816 0.100 Uiso 1 1 calc R U . . . H2SB H 0.032102 0.018044 -0.204588 0.100 Uiso 1 1 calc R U . . . H2SC H -0.002087 -0.079645 -0.238759 0.100 Uiso 1 1 calc R U . . . S3S S 0.76187(18) 0.32517(16) 0.08676(17) 0.0513(7) Uani 1 1 d . . . . . O3S O 0.6680(4) 0.2935(4) 0.0532(4) 0.0593(19) Uani 1 1 d . . . . . C3 C 0.3151(6) 0.2293(6) 0.0705(5) 0.036(2) Uani 1 1 d . . . . . H3 H 0.363355 0.189815 0.101021 0.043 Uiso 1 1 calc R U . . . O3 O 0.0740(5) 0.1438(5) -0.1285(5) 0.076(2) Uani 1 1 d . . . . . N3 N 0.0866(6) 0.2247(6) -0.1184(6) 0.054(2) Uani 1 1 d . . . . . C3S C 0.0766(7) 0.5917(7) 0.5313(8) 0.080(4) Uani 1 1 d . . . . . H3SA H 0.024457 0.581362 0.470838 0.121 Uiso 1 1 calc R U . . . H3SB H 0.114559 0.539228 0.548426 0.121 Uiso 1 1 calc R U . . . H3SC H 0.056650 0.604715 0.582563 0.121 Uiso 1 1 calc R U . . . O4 O 0.4772(4) 0.4881(4) 0.1424(3) 0.0371(14) Uani 1 1 d . . . . . N4 N 0.8075(6) 0.6518(5) 0.2860(6) 0.051(2) Uani 1 1 d . . . . . C4 C 0.2373(6) 0.1982(6) 0.0008(6) 0.044(2) Uani 1 1 d . . . . . H4 H 0.230581 0.137486 -0.014776 0.053 Uiso 1 1 calc R U . . . C4S C 0.0588(6) 0.7635(7) 0.5034(7) 0.064(3) Uani 1 1 d . . . . . H4SA H 0.006670 0.755024 0.442410 0.097 Uiso 1 1 calc R U . . . H4SB H 0.040074 0.760848 0.556877 0.097 Uiso 1 1 calc R U . . . H4SC H 0.085782 0.820891 0.503085 0.097 Uiso 1 1 calc R U . . . O5 O 0.8177(5) 0.7172(5) 0.2418(5) 0.064(2) Uani 1 1 d . . . . . C5 C 0.1685(6) 0.2567(7) -0.0467(6) 0.044(2) Uani 1 1 d . . . . . C5S C 0.8272(7) 0.2634(9) 0.1870(6) 0.085(4) Uani 1 1 d . . . . . H5SA H 0.889581 0.283035 0.210619 0.127 Uiso 1 1 calc R U . . . H5SB H 0.805362 0.271237 0.237748 0.127 Uiso 1 1 calc R U . . . H5SC H 0.823527 0.201290 0.169205 0.127 Uiso 1 1 calc R U . . . C6 C 0.1768(6) 0.3446(6) -0.0256(6) 0.044(2) Uani 1 1 d . . . . . H6 H 0.129858 0.383716 -0.061747 0.052 Uiso 1 1 calc R U . . . C6S C 0.7674(10) 0.4235(8) 0.1496(9) 0.106(5) Uani 1 1 d . . . . . H6SA H 0.828280 0.447139 0.173294 0.159 Uiso 1 1 calc R U . . . H6SB H 0.725339 0.466137 0.106272 0.159 Uiso 1 1 calc R U . . . H6SC H 0.751545 0.411873 0.204119 0.159 Uiso 1 1 calc R U . . . O6 O 0.8661(4) 0.6260(5) 0.3612(5) 0.0567(18) Uani 1 1 d . . . . . O7 O 0.4526(3) 0.5596(3) 0.2947(3) 0.0298(13) Uani 1 1 d . . . . . C7 C 0.2544(6) 0.4696(6) 0.0706(6) 0.040(2) Uani 1 1 d . . . . . H7 H 0.205058 0.504622 0.031135 0.048 Uiso 1 1 calc R U . . . O8 O 0.3783(4) 0.6665(3) 0.3664(4) 0.0415(15) Uani 1 1 d . . . . . H8 H 0.362087 0.704603 0.394146 0.062 Uiso 1 1 d R U . . . C8 C 0.6231(6) 0.5018(5) 0.2689(5) 0.034(2) Uani 1 1 d . . . . . O9 O 0.4875(3) 0.4267(3) 0.4766(3) 0.0323(14) Uani 1 1 d . . . . . C9 C 0.5568(6) 0.5225(5) 0.1753(5) 0.0313(19) Uani 1 1 d . . . . . O10 O 0.3603(4) 0.4334(3) 0.3059(4) 0.0349(14) Uani 1 1 d . . . . . C10 C 0.5800(6) 0.5841(5) 0.1193(6) 0.035(2) Uani 1 1 d . . . . . H10 H 0.538066 0.597715 0.055970 0.042 Uiso 1 1 calc R U . . . C11 C 0.6617(6) 0.6242(6) 0.1550(6) 0.041(2) Uani 1 1 d . . . . . H11 H 0.676015 0.664817 0.115988 0.049 Uiso 1 1 calc R U . . . C12 C 0.7239(6) 0.6066(5) 0.2474(6) 0.035(2) Uani 1 1 d . . . . . C13 C 0.7064(6) 0.5438(6) 0.3028(6) 0.037(2) Uani 1 1 d . . . . . H13 H 0.751001 0.528993 0.364298 0.044 Uiso 1 1 calc R U . . . C14 C 0.6088(6) 0.4328(5) 0.3261(5) 0.032(2) Uani 1 1 d . . . . . H14 H 0.660499 0.407541 0.374929 0.039 Uiso 1 1 calc R U . . . C15 C 0.3099(6) 0.5983(5) 0.1688(6) 0.041(2) Uani 1 1 d . . . . . H15A H 0.271238 0.600522 0.204783 0.049 Uiso 1 1 calc R U . . . H15B H 0.282962 0.635778 0.110907 0.049 Uiso 1 1 calc R U . . . C16 C 0.4042(5) 0.6302(5) 0.2323(5) 0.031(2) Uani 1 1 d . . . . . H16 H 0.435621 0.647900 0.190706 0.037 Uiso 1 1 calc R U . . . C17 C 0.4041(6) 0.7058(5) 0.2953(5) 0.037(2) Uani 1 1 d . . . . . H17A H 0.464225 0.732724 0.325766 0.044 Uiso 1 1 calc R U . . . H17B H 0.360480 0.751183 0.257906 0.044 Uiso 1 1 calc R U . . . C18 C 0.5305(5) 0.3282(5) 0.3774(5) 0.032(2) Uani 1 1 d . . . . . H18A H 0.591318 0.317181 0.427267 0.038 Uiso 1 1 calc R U . . . H18B H 0.511119 0.274989 0.336702 0.038 Uiso 1 1 calc R U . . . C19 C 0.4675(6) 0.3439(5) 0.4257(5) 0.033(2) Uani 1 1 d . . . . . H19 H 0.473579 0.295268 0.472123 0.040 Uiso 1 1 calc R U . . . C20 C 0.3715(6) 0.3515(5) 0.3555(6) 0.037(2) Uani 1 1 d . . . . . H20A H 0.355809 0.302332 0.308907 0.044 Uiso 1 1 calc R U . . . H20B H 0.331677 0.348942 0.390080 0.044 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 0.0413(7) 0.0110(5) 0.0380(6) 0.0013(5) 0.0147(6) 0.0012(6) S1S 0.074(2) 0.0382(16) 0.0710(17) 0.0010(15) 0.0154(16) -0.0038(16) CO1 0.0448(7) 0.0119(5) 0.0368(6) 0.0015(5) 0.0139(5) 0.0010(6) CL1 0.0465(13) 0.0236(11) 0.0490(12) -0.0023(10) 0.0203(11) -0.0002(11) O1 0.046(4) 0.019(3) 0.039(3) -0.002(3) 0.010(3) 0.003(3) C1 0.053(6) 0.017(4) 0.034(4) -0.002(4) 0.017(4) -0.002(5) N1 0.051(5) 0.015(3) 0.032(3) -0.001(3) 0.015(3) 0.001(4) O1S 0.052(4) 0.056(5) 0.095(5) 0.033(4) -0.007(4) -0.010(4) C1S 0.058(7) 0.051(7) 0.064(6) 0.004(6) 0.021(5) -0.005(6) S2S 0.0596(17) 0.0318(14) 0.0699(17) -0.0011(14) 0.0145(15) -0.0024(14) N2 0.037(4) 0.018(4) 0.038(4) -0.002(3) 0.015(3) 0.001(3) O2S 0.063(5) 0.040(4) 0.080(4) -0.017(4) 0.012(4) -0.003(4) C2 0.059(6) 0.020(4) 0.037(5) -0.004(4) 0.030(5) -0.006(5) O2 0.053(4) 0.055(5) 0.077(5) -0.012(4) 0.003(4) 0.000(4) C2S 0.071(7) 0.035(6) 0.077(7) -0.003(6) 0.014(6) 0.006(6) S3S 0.0630(17) 0.0325(14) 0.0591(15) -0.0087(13) 0.0256(14) -0.0042(14) O3S 0.059(4) 0.041(4) 0.064(4) 0.002(4) 0.012(3) -0.019(4) C3 0.045(5) 0.021(4) 0.041(5) -0.002(4) 0.016(4) -0.010(4) O3 0.073(5) 0.040(5) 0.096(5) -0.033(4) 0.016(4) -0.016(4) N3 0.048(5) 0.054(6) 0.060(5) -0.019(5) 0.022(5) -0.013(5) C3S 0.053(7) 0.032(6) 0.127(9) 0.025(7) 0.006(7) -0.009(6) O4 0.046(4) 0.026(3) 0.037(3) 0.006(3) 0.015(3) 0.004(3) N4 0.063(6) 0.033(5) 0.061(5) 0.004(5) 0.029(5) -0.005(5) C4 0.067(7) 0.028(5) 0.052(5) -0.004(5) 0.038(5) 0.001(5) C4S 0.053(6) 0.038(6) 0.106(8) -0.004(6) 0.037(6) -0.003(6) O5 0.066(5) 0.042(4) 0.087(5) 0.008(4) 0.033(4) -0.007(4) C5 0.043(6) 0.039(6) 0.053(5) -0.014(5) 0.022(5) -0.014(5) C5S 0.083(8) 0.116(12) 0.050(6) 0.009(7) 0.022(6) 0.028(9) C6 0.041(5) 0.040(6) 0.052(5) -0.004(5) 0.021(5) 0.001(5) C6S 0.175(14) 0.052(8) 0.138(10) -0.052(8) 0.113(11) -0.045(9) O6 0.048(4) 0.042(4) 0.073(4) 0.010(4) 0.017(4) -0.005(4) O7 0.045(3) 0.009(3) 0.032(3) 0.003(2) 0.013(3) 0.003(3) C7 0.049(6) 0.024(5) 0.048(5) -0.003(5) 0.023(5) 0.002(5) O8 0.069(4) 0.010(3) 0.045(3) 0.004(3) 0.022(3) 0.011(3) C8 0.053(6) 0.019(4) 0.034(4) 0.002(4) 0.022(4) 0.007(4) O9 0.044(3) 0.012(3) 0.033(3) -0.002(2) 0.007(3) -0.001(3) C9 0.043(5) 0.017(4) 0.038(5) -0.004(4) 0.021(4) 0.001(4) O10 0.046(4) 0.012(3) 0.049(3) 0.007(3) 0.023(3) -0.001(3) C10 0.049(6) 0.019(4) 0.040(5) -0.003(4) 0.021(4) 0.007(4) C11 0.054(6) 0.025(5) 0.050(5) -0.007(5) 0.028(5) -0.005(5) C12 0.044(5) 0.017(4) 0.045(5) -0.004(4) 0.019(5) -0.005(4) C13 0.045(5) 0.024(5) 0.039(4) -0.001(4) 0.015(4) 0.009(5) C14 0.039(5) 0.024(5) 0.023(4) -0.004(4) 0.003(4) 0.002(4) C15 0.053(6) 0.013(4) 0.050(5) 0.003(4) 0.013(5) 0.009(5) C16 0.047(5) 0.013(4) 0.023(4) 0.007(4) 0.004(4) 0.000(4) C17 0.050(6) 0.019(4) 0.039(5) 0.003(4) 0.016(4) -0.001(4) C18 0.040(5) 0.012(4) 0.039(4) 0.000(4) 0.011(4) 0.000(4) C19 0.056(6) 0.008(4) 0.033(4) -0.004(4) 0.015(4) -0.003(4) C20 0.051(6) 0.009(4) 0.051(5) 0.004(4) 0.021(5) -0.001(4) _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 O9 1.961(5) 3_666 ? FE1 O9 2.037(5) . ? FE1 O7 2.041(5) . ? FE1 O10 2.059(5) . ? FE1 O8 2.139(5) . ? FE1 CL1 2.303(3) . ? S1S O1S 1.508(7) . ? S1S C1S 1.753(10) . ? S1S C2S 1.764(10) . ? CO1 O1 1.863(5) . ? CO1 N1 1.881(7) . ? CO1 O4 1.891(6) . ? CO1 O7 1.892(5) . ? CO1 N2 1.915(6) . ? CO1 O10 1.916(5) . ? O1 C2 1.283(9) . ? C1 C6 1.395(11) . ? C1 C2 1.408(11) . ? C1 C7 1.449(11) . ? N1 C7 1.279(9) . ? N1 C15 1.488(10) . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? S2S O2S 1.460(6) . ? S2S C3S 1.745(10) . ? S2S C4S 1.756(10) . ? N2 C14 1.263(10) . ? N2 C18 1.477(9) . ? C2 C3 1.442(11) . ? O2 N3 1.221(10) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? S3S O3S 1.488(6) . ? S3S C5S 1.739(10) . ? S3S C6S 1.758(10) . ? C3 C4 1.366(11) . ? C3 H3 0.9500 . ? O3 N3 1.249(10) . ? N3 C5 1.425(11) . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? O4 C9 1.299(9) . ? N4 O6 1.220(9) . ? N4 O5 1.250(9) . ? N4 C12 1.427(11) . ? C4 C5 1.386(12) . ? C4 H4 0.9500 . ? C4S H4SA 0.9800 . ? C4S H4SB 0.9800 . ? C4S H4SC 0.9800 . ? C5 C6 1.372(12) . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? C6 H6 0.9500 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? C6S H6SC 0.9800 . ? O7 C16 1.440(8) . ? C7 H7 0.9500 . ? O8 C17 1.441(9) . ? O8 H8 0.8224 . ? C8 C13 1.399(12) . ? C8 C9 1.430(10) . ? C8 C14 1.443(11) . ? O9 C19 1.446(8) . ? O9 FE1 1.961(5) 3_666 ? C9 C10 1.419(11) . ? O10 C20 1.431(8) . ? C10 C11 1.364(11) . ? C10 H10 0.9500 . ? C11 C12 1.385(11) . ? C11 H11 0.9500 . ? C12 C13 1.380(11) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.529(11) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.497(11) . ? C16 H16 1.0000 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.508(11) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.502(10) . ? C19 H19 1.0000 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? 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 O9 FE1 O9 71.2(2) 3_666 . ? O9 FE1 O7 106.8(2) 3_666 . ? O9 FE1 O7 107.3(2) . . ? O9 FE1 O10 148.5(2) 3_666 . ? O9 FE1 O10 78.3(2) . . ? O7 FE1 O10 74.9(2) . . ? O9 FE1 O8 89.0(2) 3_666 . ? O9 FE1 O8 159.8(2) . . ? O7 FE1 O8 74.4(2) . . ? O10 FE1 O8 120.7(2) . . ? O9 FE1 CL1 104.85(17) 3_666 . ? O9 FE1 CL1 102.99(17) . . ? O7 FE1 CL1 141.69(16) . . ? O10 FE1 CL1 89.11(17) . . ? O8 FE1 CL1 85.14(17) . . ? O1S S1S C1S 105.4(5) . . ? O1S S1S C2S 104.9(5) . . ? C1S S1S C2S 98.0(5) . . ? O1 CO1 N1 96.2(3) . . ? O1 CO1 O4 91.2(2) . . ? N1 CO1 O4 87.2(3) . . ? O1 CO1 O7 175.1(2) . . ? N1 CO1 O7 87.3(3) . . ? O4 CO1 O7 92.5(2) . . ? O1 CO1 N2 86.9(3) . . ? N1 CO1 N2 176.9(3) . . ? O4 CO1 N2 92.8(3) . . ? O7 CO1 N2 89.7(2) . . ? O1 CO1 O10 95.0(2) . . ? N1 CO1 O10 85.3(2) . . ? O4 CO1 O10 170.8(2) . . ? O7 CO1 O10 81.8(2) . . ? N2 CO1 O10 94.4(3) . . ? C2 O1 CO1 124.8(5) . . ? C6 C1 C2 120.2(8) . . ? C6 C1 C7 116.7(8) . . ? C2 C1 C7 123.1(8) . . ? C7 N1 C15 120.7(7) . . ? C7 N1 CO1 126.6(6) . . ? C15 N1 CO1 112.4(5) . . ? S1S C1S H1SA 109.5 . . ? S1S C1S H1SB 109.5 . . ? H1SA C1S H1SB 109.5 . . ? S1S C1S H1SC 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O2S S2S C3S 108.1(5) . . ? O2S S2S C4S 108.6(4) . . ? C3S S2S C4S 98.3(5) . . ? C14 N2 C18 119.3(7) . . ? C14 N2 CO1 121.4(6) . . ? C18 N2 CO1 119.3(5) . . ? O1 C2 C1 126.1(8) . . ? O1 C2 C3 116.8(8) . . ? C1 C2 C3 117.0(8) . . ? S1S C2S H2SA 109.5 . . ? S1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? S1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O3S S3S C5S 107.8(5) . . ? O3S S3S C6S 106.3(6) . . ? C5S S3S C6S 96.1(6) . . ? C4 C3 C2 121.8(8) . . ? C4 C3 H3 119.1 . . ? C2 C3 H3 119.1 . . ? O2 N3 O3 120.6(9) . . ? O2 N3 C5 120.3(9) . . ? O3 N3 C5 119.2(9) . . ? S2S C3S H3SA 109.5 . . ? S2S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? S2S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? C9 O4 CO1 121.3(5) . . ? O6 N4 O5 122.3(9) . . ? O6 N4 C12 119.1(8) . . ? O5 N4 C12 118.6(8) . . ? C3 C4 C5 119.0(8) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? S2S C4S H4SA 109.5 . . ? S2S C4S H4SB 109.5 . . ? H4SA C4S H4SB 109.5 . . ? S2S C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? C6 C5 C4 121.6(9) . . ? C6 C5 N3 119.0(9) . . ? C4 C5 N3 119.4(9) . . ? S3S C5S H5SA 109.5 . . ? S3S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? S3S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C5 C6 C1 120.3(9) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? S3S C6S H6SA 109.5 . . ? S3S C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? S3S C6S H6SC 109.5 . . ? H6SA C6S H6SC 109.5 . . ? H6SB C6S H6SC 109.5 . . ? C16 O7 CO1 109.8(4) . . ? C16 O7 FE1 115.0(4) . . ? CO1 O7 FE1 100.8(2) . . ? N1 C7 C1 123.0(8) . . ? N1 C7 H7 118.5 . . ? C1 C7 H7 118.5 . . ? C17 O8 FE1 117.6(5) . . ? C17 O8 H8 110.2 . . ? FE1 O8 H8 130.4 . . ? C13 C8 C9 119.8(7) . . ? C13 C8 C14 118.8(7) . . ? C9 C8 C14 121.2(8) . . ? C19 O9 FE1 133.7(5) . 3_666 ? C19 O9 FE1 116.6(4) . . ? FE1 O9 FE1 108.8(2) 3_666 . ? O4 C9 C10 120.4(7) . . ? O4 C9 C8 122.0(7) . . ? C10 C9 C8 117.6(8) . . ? C20 O10 CO1 118.5(5) . . ? C20 O10 FE1 109.4(4) . . ? CO1 O10 FE1 99.3(2) . . ? C11 C10 C9 121.0(8) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 120.9(8) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 120.2(8) . . ? C13 C12 N4 119.1(8) . . ? C11 C12 N4 120.7(8) . . ? C12 C13 C8 120.3(8) . . ? C12 C13 H13 119.8 . . ? C8 C13 H13 119.8 . . ? N2 C14 C8 125.8(8) . . ? N2 C14 H14 117.1 . . ? C8 C14 H14 117.1 . . ? N1 C15 C16 107.0(7) . . ? N1 C15 H15A 110.3 . . ? C16 C15 H15A 110.3 . . ? N1 C15 H15B 110.3 . . ? C16 C15 H15B 110.3 . . ? H15A C15 H15B 108.6 . . ? O7 C16 C17 107.3(5) . . ? O7 C16 C15 108.7(6) . . ? C17 C16 C15 112.6(7) . . ? O7 C16 H16 109.4 . . ? C17 C16 H16 109.4 . . ? C15 C16 H16 109.4 . . ? O8 C17 C16 103.7(6) . . ? O8 C17 H17A 111.0 . . ? C16 C17 H17A 111.0 . . ? O8 C17 H17B 111.0 . . ? C16 C17 H17B 111.0 . . ? H17A C17 H17B 109.0 . . ? N2 C18 C19 112.6(6) . . ? N2 C18 H18A 109.1 . . ? C19 C18 H18A 109.1 . . ? N2 C18 H18B 109.1 . . ? C19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? O9 C19 C20 104.9(6) . . ? O9 C19 C18 110.4(6) . . ? C20 C19 C18 112.9(6) . . ? O9 C19 H19 109.5 . . ? C20 C19 H19 109.5 . . ? C18 C19 H19 109.5 . . ? O10 C20 C19 108.3(7) . . ? O10 C20 H20A 110.0 . . ? C19 C20 H20A 110.0 . . ? O10 C20 H20B 110.0 . . ? C19 C20 H20B 110.0 . . ? H20A C20 H20B 108.4 . . ? 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 N1 CO1 O1 C2 -4.9(6) . . . . ? O4 CO1 O1 C2 -92.3(6) . . . . ? N2 CO1 O1 C2 175.0(6) . . . . ? O10 CO1 O1 C2 80.9(6) . . . . ? O1 CO1 N1 C7 1.8(7) . . . . ? O4 CO1 N1 C7 92.7(7) . . . . ? O7 CO1 N1 C7 -174.7(7) . . . . ? O10 CO1 N1 C7 -92.7(7) . . . . ? O1 CO1 N1 C15 175.3(6) . . . . ? O4 CO1 N1 C15 -93.9(6) . . . . ? O7 CO1 N1 C15 -1.3(6) . . . . ? O10 CO1 N1 C15 80.7(6) . . . . ? CO1 O1 C2 C1 4.5(11) . . . . ? CO1 O1 C2 C3 -173.9(5) . . . . ? C6 C1 C2 O1 -178.9(7) . . . . ? C7 C1 C2 O1 0.4(13) . . . . ? C6 C1 C2 C3 -0.5(11) . . . . ? C7 C1 C2 C3 178.7(8) . . . . ? O1 C2 C3 C4 175.8(7) . . . . ? C1 C2 C3 C4 -2.7(12) . . . . ? O1 CO1 O4 C9 -128.2(6) . . . . ? N1 CO1 O4 C9 135.7(6) . . . . ? O7 CO1 O4 C9 48.5(6) . . . . ? N2 CO1 O4 C9 -41.3(6) . . . . ? C2 C3 C4 C5 3.0(12) . . . . ? C3 C4 C5 C6 0.2(13) . . . . ? C3 C4 C5 N3 -179.0(8) . . . . ? O2 N3 C5 C6 8.5(13) . . . . ? O3 N3 C5 C6 -170.2(9) . . . . ? O2 N3 C5 C4 -172.3(8) . . . . ? O3 N3 C5 C4 9.0(13) . . . . ? C4 C5 C6 C1 -3.5(14) . . . . ? N3 C5 C6 C1 175.7(8) . . . . ? C2 C1 C6 C5 3.6(13) . . . . ? C7 C1 C6 C5 -175.7(8) . . . . ? N1 CO1 O7 C16 -22.0(5) . . . . ? O4 CO1 O7 C16 65.1(5) . . . . ? N2 CO1 O7 C16 157.9(5) . . . . ? O10 CO1 O7 C16 -107.6(5) . . . . ? N1 CO1 O7 FE1 99.7(3) . . . . ? O4 CO1 O7 FE1 -173.2(2) . . . . ? N2 CO1 O7 FE1 -80.4(3) . . . . ? O10 CO1 O7 FE1 14.1(2) . . . . ? C15 N1 C7 C1 -171.1(8) . . . . ? CO1 N1 C7 C1 1.9(12) . . . . ? C6 C1 C7 N1 175.5(8) . . . . ? C2 C1 C7 N1 -3.8(13) . . . . ? CO1 O4 C9 C10 -150.4(6) . . . . ? CO1 O4 C9 C8 28.1(10) . . . . ? C13 C8 C9 O4 -176.9(7) . . . . ? C14 C8 C9 O4 8.5(12) . . . . ? C13 C8 C9 C10 1.7(11) . . . . ? C14 C8 C9 C10 -173.0(7) . . . . ? O4 C9 C10 C11 176.4(7) . . . . ? C8 C9 C10 C11 -2.1(12) . . . . ? C9 C10 C11 C12 -0.7(13) . . . . ? C10 C11 C12 C13 4.1(13) . . . . ? C10 C11 C12 N4 -177.0(8) . . . . ? O6 N4 C12 C13 9.9(12) . . . . ? O5 N4 C12 C13 -169.4(8) . . . . ? O6 N4 C12 C11 -169.0(8) . . . . ? O5 N4 C12 C11 11.6(13) . . . . ? C11 C12 C13 C8 -4.5(13) . . . . ? N4 C12 C13 C8 176.6(7) . . . . ? C9 C8 C13 C12 1.6(12) . . . . ? C14 C8 C13 C12 176.4(8) . . . . ? C18 N2 C14 C8 176.2(7) . . . . ? CO1 N2 C14 C8 -3.4(11) . . . . ? C13 C8 C14 N2 163.0(8) . . . . ? C9 C8 C14 N2 -22.4(13) . . . . ? C7 N1 C15 C16 -163.7(7) . . . . ? CO1 N1 C15 C16 22.4(8) . . . . ? CO1 O7 C16 C17 161.4(5) . . . . ? FE1 O7 C16 C17 48.6(7) . . . . ? CO1 O7 C16 C15 39.3(7) . . . . ? FE1 O7 C16 C15 -73.4(6) . . . . ? N1 C15 C16 O7 -39.5(8) . . . . ? N1 C15 C16 C17 -158.2(6) . . . . ? FE1 O8 C17 C16 30.3(8) . . . . ? O7 C16 C17 O8 -47.6(8) . . . . ? C15 C16 C17 O8 72.0(8) . . . . ? C14 N2 C18 C19 131.0(8) . . . . ? CO1 N2 C18 C19 -49.4(8) . . . . ? FE1 O9 C19 C20 165.3(5) 3_666 . . . ? FE1 O9 C19 C20 -27.1(7) . . . . ? FE1 O9 C19 C18 -72.7(8) 3_666 . . . ? FE1 O9 C19 C18 94.9(6) . . . . ? N2 C18 C19 O9 -52.0(8) . . . . ? N2 C18 C19 C20 65.1(8) . . . . ? CO1 O10 C20 C19 63.6(7) . . . . ? FE1 O10 C20 C19 -49.2(7) . . . . ? O9 C19 C20 O10 48.5(8) . . . . ? C18 C19 C20 O10 -71.8(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H8 O3S 0.82 1.74 2.562(8) 173.9 2_655 C4 H4 Cl1 0.95 2.89 3.762(9) 153.1 4_565 C6 H6 O1S 0.95 2.40 3.283(12) 154.5 2_554 C7 H7 O1S 0.95 2.46 3.326(11) 152.0 2_554 C14 H14 O2S 0.95 2.49 3.274(11) 139.7 3_666 C15 H15B S3S 0.99 2.85 3.758(9) 152.7 3_665 C18 H18A O3S 0.99 2.48 3.279(9) 138.0 4_566 C1S H1SB O3 0.98 2.42 3.289(12) 147.0 . C2S H2SC O3 0.98 2.20 3.101(12) 152.4 . C4S H4SC O2 0.98 2.39 3.357(13) 168.0 2 C5S H5SA O2 0.98 2.45 3.192(11) 132.5 4_666 _shelx_res_file ; TITL k497 in P2(1)/c KOKO497.res created by SHELXL-2016/4 at 18:21:37 on 30-Jan-2020 REM dfix 0.820 0.005 O8 H8 REM dfix 1.717 0.010 H8 O3S_$1 CELL 0.71073 16.3535 15.2344 15.2012 90 113.99 90 ZERR 2 0.0033 0.0021 0.0026 0 0.023 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl Co Fe N O S UNIT 104 148 4 4 4 16 52 12 L.S. 4 PLAN 20 SIZE 0.1 0.1 0.05 TEMP -100.15 conf BOND $h fmap 2 acta 52 OMIT 3 4 7 OMIT -1 2 1 OMIT 4 13 12 OMIT -12 15 10 OMIT -1 6 4 OMIT 1 2 0 OMIT -2 4 7 OMIT -12 1 4 REM REM REM WGHT 0.064600 FVAR 0.11630 FE1 5 0.415067 0.532588 0.404527 11.00000 0.04127 0.01103 = 0.03795 0.00131 0.01467 0.00123 S1S 8 0.039892 -0.012259 -0.348223 11.00000 0.07401 0.03818 = 0.07096 0.00099 0.01540 -0.00384 CO1 4 0.424230 0.452224 0.226279 11.00000 0.04478 0.01194 = 0.03677 0.00153 0.01393 0.00096 CL1 3 0.291025 0.527979 0.440119 11.00000 0.04647 0.02358 = 0.04900 -0.00227 0.02026 -0.00017 O1 7 0.399273 0.341649 0.169053 11.00000 0.04639 0.01932 = 0.03902 -0.00165 0.01016 0.00280 C1 1 0.253789 0.376964 0.048533 11.00000 0.05280 0.01656 = 0.03358 -0.00227 0.01705 -0.00167 N1 6 0.318404 0.506314 0.140636 11.00000 0.05057 0.01488 = 0.03216 -0.00073 0.01480 0.00138 O1S 7 -0.053345 0.022244 -0.404925 11.00000 0.05152 0.05643 = 0.09542 0.03322 -0.00724 -0.01036 C1S 1 0.109155 0.080597 -0.317129 11.00000 0.05820 0.05117 = 0.06382 0.00361 0.02142 -0.00500 AFIX 33 H1SA 2 0.171253 0.062527 -0.279821 11.00000 -1.50000 H1SB 2 0.104794 0.110780 -0.375806 11.00000 -1.50000 H1SC 2 0.090142 0.120403 -0.278374 11.00000 -1.50000 AFIX 0 S2S 8 0.137703 0.680513 0.517240 11.00000 0.05955 0.03177 = 0.06988 -0.00114 0.01448 -0.00237 N2 6 0.533763 0.402978 0.317085 11.00000 0.03735 0.01767 = 0.03797 -0.00197 0.01508 0.00069 O2S 7 0.214809 0.694235 0.608324 11.00000 0.06270 0.03998 = 0.08043 -0.01715 0.01185 -0.00333 C2 1 0.325755 0.320286 0.098831 11.00000 0.05892 0.02048 = 0.03702 -0.00409 0.02971 -0.00563 O2 7 0.028893 0.276025 -0.167913 11.00000 0.05287 0.05545 = 0.07657 -0.01166 0.00262 0.00005 C2S 1 0.043607 -0.035748 -0.233054 11.00000 0.07118 0.03510 = 0.07693 -0.00305 0.01377 0.00646 AFIX 33 H2SA 2 0.102868 -0.058697 -0.191816 11.00000 -1.50000 H2SB 2 0.032102 0.018044 -0.204588 11.00000 -1.50000 H2SC 2 -0.002087 -0.079645 -0.238759 11.00000 -1.50000 AFIX 0 S3S 8 0.761866 0.325170 0.086757 11.00000 0.06295 0.03252 = 0.05911 -0.00866 0.02563 -0.00424 O3S 7 0.667992 0.293515 0.053236 11.00000 0.05939 0.04085 = 0.06449 0.00164 0.01174 -0.01859 C3 1 0.315053 0.229260 0.070458 11.00000 0.04485 0.02079 = 0.04122 -0.00215 0.01623 -0.00965 AFIX 43 H3 2 0.363355 0.189815 0.101021 11.00000 -1.20000 AFIX 0 O3 7 0.074043 0.143849 -0.128533 11.00000 0.07349 0.04025 = 0.09557 -0.03317 0.01574 -0.01613 N3 6 0.086601 0.224748 -0.118380 11.00000 0.04763 0.05350 = 0.06002 -0.01917 0.02163 -0.01345 C3S 1 0.076650 0.591721 0.531309 11.00000 0.05257 0.03184 = 0.12694 0.02459 0.00566 -0.00903 AFIX 33 H3SA 2 0.024457 0.581362 0.470838 11.00000 -1.50000 H3SB 2 0.114559 0.539228 0.548426 11.00000 -1.50000 H3SC 2 0.056650 0.604715 0.582563 11.00000 -1.50000 AFIX 0 O4 7 0.477234 0.488127 0.142419 11.00000 0.04605 0.02615 = 0.03713 0.00561 0.01497 0.00376 N4 6 0.807528 0.651841 0.285969 11.00000 0.06265 0.03326 = 0.06129 0.00400 0.02908 -0.00469 C4 1 0.237340 0.198196 0.000818 11.00000 0.06668 0.02761 = 0.05228 -0.00377 0.03813 0.00110 AFIX 43 H4 2 0.230581 0.137486 -0.014776 11.00000 -1.20000 AFIX 0 C4S 1 0.058843 0.763487 0.503371 11.00000 0.05350 0.03790 = 0.10595 -0.00378 0.03681 -0.00254 AFIX 33 H4SA 2 0.006670 0.755024 0.442410 11.00000 -1.50000 H4SB 2 0.040074 0.760848 0.556877 11.00000 -1.50000 H4SC 2 0.085782 0.820891 0.503085 11.00000 -1.50000 AFIX 0 O5 7 0.817733 0.717204 0.241800 11.00000 0.06618 0.04235 = 0.08701 0.00775 0.03339 -0.00662 C5 1 0.168494 0.256651 -0.046741 11.00000 0.04313 0.03922 = 0.05258 -0.01385 0.02220 -0.01352 C5S 1 0.827216 0.263447 0.187025 11.00000 0.08310 0.11647 = 0.05015 0.00929 0.02233 0.02822 AFIX 33 H5SA 2 0.889581 0.283035 0.210619 11.00000 -1.50000 H5SB 2 0.805362 0.271237 0.237748 11.00000 -1.50000 H5SC 2 0.823527 0.201290 0.169205 11.00000 -1.50000 AFIX 0 C6 1 0.176795 0.344624 -0.025644 11.00000 0.04117 0.03952 = 0.05198 -0.00430 0.02070 0.00075 AFIX 43 H6 2 0.129858 0.383716 -0.061747 11.00000 -1.20000 AFIX 0 C6S 1 0.767366 0.423456 0.149560 11.00000 0.17500 0.05177 = 0.13831 -0.05225 0.11258 -0.04531 AFIX 33 H6SA 2 0.828280 0.447139 0.173294 11.00000 -1.50000 H6SB 2 0.725339 0.466137 0.106272 11.00000 -1.50000 H6SC 2 0.751545 0.411873 0.204119 11.00000 -1.50000 AFIX 0 O6 7 0.866149 0.626001 0.361157 11.00000 0.04794 0.04231 = 0.07285 0.00972 0.01729 -0.00462 O7 7 0.452588 0.559562 0.294685 11.00000 0.04525 0.00889 = 0.03239 0.00262 0.01278 0.00289 C7 1 0.254425 0.469578 0.070556 11.00000 0.04948 0.02423 = 0.04802 -0.00290 0.02265 0.00236 AFIX 43 H7 2 0.205058 0.504622 0.031135 11.00000 -1.20000 AFIX 0 O8 7 0.378317 0.666473 0.366426 11.00000 0.06859 0.00976 = 0.04491 0.00398 0.02175 0.01117 AFIX 3 H8 2 0.362087 0.704603 0.394146 11.00000 -1.50000 AFIX 0 C8 1 0.623108 0.501794 0.268857 11.00000 0.05264 0.01879 = 0.03386 0.00189 0.02212 0.00679 O9 7 0.487517 0.426730 0.476593 11.00000 0.04360 0.01167 = 0.03295 -0.00210 0.00665 -0.00097 C9 1 0.556791 0.522475 0.175268 11.00000 0.04273 0.01685 = 0.03838 -0.00434 0.02060 0.00097 O10 7 0.360260 0.433424 0.305905 11.00000 0.04640 0.01234 = 0.04933 0.00738 0.02290 -0.00143 C10 1 0.580005 0.584146 0.119276 11.00000 0.04902 0.01923 = 0.03969 -0.00273 0.02089 0.00707 AFIX 43 H10 2 0.538066 0.597715 0.055970 11.00000 -1.20000 AFIX 0 C11 1 0.661666 0.624240 0.155022 11.00000 0.05361 0.02508 = 0.05025 -0.00725 0.02822 -0.00535 AFIX 43 H11 2 0.676015 0.664817 0.115988 11.00000 -1.20000 AFIX 0 C12 1 0.723930 0.606626 0.247393 11.00000 0.04376 0.01703 = 0.04505 -0.00377 0.01948 -0.00522 C13 1 0.706360 0.543793 0.302813 11.00000 0.04543 0.02431 = 0.03858 -0.00130 0.01461 0.00889 AFIX 43 H13 2 0.751001 0.528993 0.364298 11.00000 -1.20000 AFIX 0 C14 1 0.608843 0.432790 0.326113 11.00000 0.03947 0.02427 = 0.02307 -0.00380 0.00293 0.00218 AFIX 43 H14 2 0.660499 0.407541 0.374929 11.00000 -1.20000 AFIX 0 C15 1 0.309873 0.598273 0.168819 11.00000 0.05304 0.01335 = 0.04966 0.00253 0.01301 0.00914 AFIX 23 H15A 2 0.271238 0.600522 0.204783 11.00000 -1.20000 H15B 2 0.282962 0.635778 0.110907 11.00000 -1.20000 AFIX 0 C16 1 0.404240 0.630236 0.232323 11.00000 0.04658 0.01304 = 0.02279 0.00653 0.00383 0.00023 AFIX 13 H16 2 0.435621 0.647900 0.190706 11.00000 -1.20000 AFIX 0 C17 1 0.404081 0.705776 0.295256 11.00000 0.04963 0.01865 = 0.03889 0.00271 0.01557 -0.00148 AFIX 23 H17A 2 0.464225 0.732724 0.325766 11.00000 -1.20000 H17B 2 0.360480 0.751183 0.257906 11.00000 -1.20000 AFIX 0 C18 1 0.530453 0.328183 0.377382 11.00000 0.03966 0.01158 = 0.03903 0.00047 0.01136 -0.00005 AFIX 23 H18A 2 0.591318 0.317181 0.427267 11.00000 -1.20000 H18B 2 0.511119 0.274989 0.336702 11.00000 -1.20000 AFIX 0 C19 1 0.467486 0.343940 0.425727 11.00000 0.05586 0.00765 = 0.03332 -0.00366 0.01549 -0.00254 AFIX 13 H19 2 0.473579 0.295268 0.472123 11.00000 -1.20000 AFIX 0 C20 1 0.371484 0.351477 0.355490 11.00000 0.05064 0.00893 = 0.05120 0.00379 0.02110 -0.00095 AFIX 23 H20A 2 0.355809 0.302332 0.308907 11.00000 -1.20000 H20B 2 0.331677 0.348942 0.390080 11.00000 -1.20000 AFIX 0 HKLF 4 REM k497 in P2(1)/c REM R1 = 0.0914 for 3314 Fo > 4sig(Fo) and 0.2083 for all 7748 data REM 442 parameters refined using 0 restraints END WGHT 0.0645 0.0000 REM Highest difference peak 0.978, deepest hole -0.634, 1-sigma level 0.126 Q1 1 0.3578 0.5332 0.4240 11.00000 0.05 0.98 Q2 1 0.4824 0.4595 0.2144 11.00000 0.05 0.94 Q3 1 0.3637 0.4534 0.2261 11.00000 0.05 0.83 Q4 1 0.3556 0.5226 0.3449 11.00000 0.05 0.83 Q5 1 0.3992 0.4615 0.1453 11.00000 0.05 0.74 Q6 1 0.0410 0.0288 -0.2884 11.00000 0.05 0.73 Q7 1 0.5283 0.4696 0.5258 11.00000 0.05 0.73 Q8 1 0.4818 0.4421 0.2871 11.00000 0.05 0.67 Q9 1 0.0917 0.7080 0.5505 11.00000 0.05 0.58 Q10 1 0.3488 0.5499 0.5020 11.00000 0.05 0.58 Q11 1 0.4709 0.5425 0.3957 11.00000 0.05 0.57 Q12 1 0.8634 0.3837 0.1913 11.00000 0.05 0.53 Q13 1 0.7443 0.2469 0.1133 11.00000 0.05 0.52 Q14 1 0.1158 -0.0491 -0.3363 11.00000 0.05 0.52 Q15 1 0.1353 0.6854 0.6200 11.00000 0.05 0.51 Q16 1 0.2112 0.7024 0.5386 11.00000 0.05 0.49 Q17 1 -0.0329 -0.0283 -0.3947 11.00000 0.05 0.49 Q18 1 0.2254 0.5375 0.3881 11.00000 0.05 0.48 Q19 1 0.7838 0.3240 0.1756 11.00000 0.05 0.48 Q20 1 -0.0031 0.0381 -0.4099 11.00000 0.05 0.47 ; _shelx_res_checksum 83516 _shelx_hkl_file ; 3 0 0 12.96 1.81 4 0 0 45.46 3.62 -4 0 0 44.47 5.17 5 0 0 81.33 5.69 -5 0 0 89.03 7.41 6 0 0 287.55 13.26 6 0 0 262.08 12.06 -6 0 0 259.55 14.74 7 0 0 90.79 7.12 -7 0 0 81.54 8.29 -8 0 0 98.25 9.63 8 0 0 102.60 8.15 9 0 0 15.23 3.13 -9 0 0 13.80 4.55 -10 0 0 -3.34 3.05 10 0 0 -1.92 1.89 11 0 0 122.05 10.01 -11 0 0 117.79 12.46 -12 0 0 14.87 5.25 12 0 0 7.75 2.46 13 0 0 10.90 3.26 -13 0 0 6.44 3.35 -14 0 0 -5.29 4.16 14 0 0 0.47 1.81 -15 0 0 3.51 4.07 -16 0 0 0.92 3.81 -17 0 0 16.25 7.42 -18 0 0 17.42 7.28 -19 0 0 2.55 5.09 -2 -1 0 3.61 0.72 -2 1 0 3.96 1.25 2 1 0 2.69 0.65 -2 -1 0 4.78 0.75 2 -1 0 5.65 1.34 -3 -1 0 1.57 0.66 3 1 0 1.41 0.65 -3 -1 0 0.77 0.65 3 -1 0 1.44 1.08 3 1 0 1.77 0.50 -3 1 0 0.23 1.09 -4 -1 0 9.02 1.45 4 1 0 10.19 1.57 -4 -1 0 9.89 2.19 4 1 0 9.27 1.77 -4 1 0 11.19 3.05 -5 1 0 12.54 3.24 5 1 0 17.27 2.38 -5 -1 0 13.35 1.99 5 1 0 15.24 2.10 -6 1 0 -0.34 1.26 6 1 0 -0.66 1.23 -6 -1 0 -1.11 1.24 6 1 0 0.56 0.73 -7 1 0 22.26 5.08 7 1 0 29.43 3.82 8 1 0 4.22 1.73 -8 1 0 3.14 2.59 -8 -1 0 0.47 2.02 -9 -1 0 13.52 3.81 9 1 0 17.55 3.11 -9 1 0 16.50 4.62 10 1 0 7.84 2.02 10 -1 0 8.73 3.25 -10 1 0 8.41 3.50 -10 -1 0 8.86 3.52 11 1 0 -0.99 1.30 -11 -1 0 2.93 3.52 11 -1 0 -2.11 1.78 -11 1 0 1.78 2.71 -12 -1 0 40.39 7.98 12 1 0 42.16 5.77 12 -1 0 41.56 6.19 -12 1 0 35.03 7.44 -13 1 0 4.92 4.21 -13 -1 0 9.63 4.45 13 -1 0 3.90 2.31 13 1 0 4.92 1.82 -14 -1 0 3.42 3.96 14 -1 0 0.04 1.77 14 1 0 0.57 1.23 -14 1 0 1.23 3.51 -15 1 0 -3.18 2.55 -15 -1 0 -1.15 3.01 -16 -1 0 4.69 3.46 -16 1 0 -1.06 3.05 -17 1 0 3.44 4.23 -17 -1 0 -3.53 2.78 -18 1 0 8.99 5.46 -18 -1 0 8.21 5.62 -19 1 0 -0.20 3.44 -19 -1 0 -7.73 6.08 1 -2 0 1109.34 37.13 -1 2 0 1060.99 36.91 -1 -2 0 1300.05 36.43 1 2 0 1255.38 36.33 -2 2 0 668.78 24.03 2 -2 0 648.65 23.67 -3 2 0 201.28 10.83 -3 -2 0 196.05 9.02 3 -2 0 212.67 10.79 -4 2 0 33.89 4.53 -4 -2 0 26.09 2.94 -4 -2 0 37.22 2.98 -5 2 0 0.11 1.53 -5 -2 0 0.31 1.31 5 2 0 0.38 0.83 -5 -2 0 2.05 0.89 6 2 0 332.48 13.50 -6 -2 0 337.19 13.65 6 2 0 340.92 14.59 -6 2 0 325.09 17.95 -7 -2 0 258.06 11.80 7 2 0 272.06 12.07 7 2 0 256.71 12.96 -7 2 0 282.91 17.16 -8 -2 0 73.07 5.96 8 2 0 81.30 6.69 -8 2 0 68.36 8.84 -9 2 0 6.02 2.91 9 2 0 11.82 2.70 10 2 0 10.37 2.71 -10 2 0 10.43 4.25 -11 -2 0 14.99 4.75 11 2 0 16.37 3.57 -11 2 0 16.47 4.62 12 2 0 0.58 1.68 -12 2 0 -1.30 2.54 -12 -2 0 1.16 2.20 12 -2 0 2.51 2.50 13 -2 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_publcif_info_datablock.structure '{3ba6ec4f-9989-4aba-b0cf-6b83ca638f36}' y y y loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? loop_ _publcif_info_tables.block_id _publcif_info_tables.reference_item "{3ba6ec4f-9989-4aba-b0cf-6b83ca638f36}" "_publcif_info_datablock.publ_exptl" loop_ _publcif_info_cif.paper_type EE