#------------------------------------------------------------------------------ #$Date: 2022-05-25 01:50:28 +0300 (Wed, 25 May 2022) $ #$Revision: 275631 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/03/7710313.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7710313 loop_ _publ_author_name 'Bhar, Kishalay' 'Guo, Wenbin' 'Gonidec, Mathieu' 'Nikhil Raj M. , Venkata' 'Bhatt, Surabhi' 'Perdih, Franc' 'Guionneau, Philippe' 'Chastanet, Guillaume' 'Sharma, Anuj' _publ_section_title ; High temperature spin crossover behaviour of mononuclear bis-(thiocyanato)iron(II) complexes with judiciously designed bidentate N-donor Schiff bases with varying substituent ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D2DT00416J _journal_year 2022 _chemical_absolute_configuration ad _chemical_formula_moiety 'C40 H32 Fe N6 S2' _chemical_formula_sum 'C40 H32 Fe N6 S2' _chemical_formula_weight 716.68 _space_group_crystal_system tetragonal _space_group_IT_number 92 _space_group_name_Hall 'P 4abw 2nw' _space_group_name_H-M_alt 'P 41 21 2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2022-04-14 deposited with the CCDC. 2022-05-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 17.7428(6) _cell_length_b 17.7428(6) _cell_length_c 12.2100(4) _cell_measurement_reflns_used 3963 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 26.0910 _cell_measurement_theta_min 3.6140 _cell_volume 3843.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4933 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_unetI/netI 0.0398 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 13625 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.482 _diffrn_reflns_theta_min 2.838 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 0.536 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82558 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.238 _exptl_crystal_description needle _exptl_crystal_F_000 1488 _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.120 _refine_diff_density_max 0.282 _refine_diff_density_min -0.153 _refine_diff_density_rms 0.035 _refine_ls_abs_structure_details ; Flack x determined using 1205 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.014(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 4404 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0386 _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^)+(0.0308P)^2^+0.7974P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0768 _refine_ls_wR_factor_ref 0.0848 _reflns_Friedel_coverage 0.738 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 1.000 _reflns_number_gt 3394 _reflns_number_total 4404 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt00416j2.cif _cod_data_source_block mob423 _cod_original_cell_volume 3843.8(3) _cod_database_code 7710313 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_min 0.794 _shelx_estimated_absorpt_t_max 0.938 _shelx_res_file ; TITL mob423 in P4(1)2(1)2 mob423.res created by SHELXL-2018/3 at 15:31:24 on 13-Apr-2022 CELL 0.71073 17.7428 17.7428 12.21 90 90 90 ZERR 4 0.0006 0.0006 0.0004 0 0 0 LATT -1 SYMM -X,-Y,0.5+Z SYMM 0.5-Y,0.5+X,0.25+Z SYMM 0.5+Y,0.5-X,0.75+Z SYMM 0.5-X,0.5+Y,0.25-Z SYMM 0.5+X,0.5-Y,0.75-Z SYMM +Y,+X,-Z SYMM -Y,-X,0.5-Z SFAC C H Fe N S UNIT 160 128 4 24 8 L.S. 10 PLAN 20 SIZE 0.12 0.15 0.45 BOND $H CONF fmap 2 acta ABIN SHEL 20.1 0.77 REM REM REM WGHT 0.030800 0.797400 FVAR 0.39280 FE1 3 0.406186 0.406186 0.500000 10.50000 0.04053 0.04053 = 0.03631 -0.00276 0.00276 -0.00263 S1 5 0.668486 0.396243 0.572047 11.00000 0.05049 0.08313 = 0.11947 -0.00900 -0.01413 0.00564 N1 4 0.384342 0.418855 0.657176 11.00000 0.04212 0.04332 = 0.03701 -0.00525 -0.00103 -0.00381 N2 4 0.295892 0.407225 0.494575 11.00000 0.03843 0.03760 = 0.03672 0.00096 -0.00023 -0.00287 N3 4 0.515816 0.405746 0.521199 11.00000 0.04290 0.05193 = 0.05199 -0.00573 0.00720 -0.00344 C1 1 0.433587 0.425526 0.739156 11.00000 0.04610 0.06235 = 0.04309 -0.00688 -0.00316 -0.00182 AFIX 43 H1 2 0.484789 0.423535 0.723119 11.00000 -1.20000 AFIX 0 C2 1 0.411783 0.435272 0.846941 11.00000 0.05608 0.08890 = 0.04064 -0.00938 -0.00749 -0.00002 AFIX 43 H2 2 0.447819 0.440467 0.901735 11.00000 -1.20000 AFIX 0 C3 1 0.336898 0.437194 0.872145 11.00000 0.06267 0.10317 = 0.03780 -0.01450 0.00461 0.00277 AFIX 43 H3 2 0.321198 0.443101 0.944306 11.00000 -1.20000 AFIX 0 C4 1 0.284787 0.430225 0.788730 11.00000 0.04428 0.08845 = 0.04519 -0.01563 0.00614 0.00125 AFIX 43 H4 2 0.233421 0.431918 0.803691 11.00000 -1.20000 AFIX 0 C5 1 0.310254 0.420690 0.682612 11.00000 0.04179 0.04598 = 0.03967 -0.00757 0.00106 -0.00107 C6 1 0.260332 0.414135 0.586845 11.00000 0.03595 0.04086 = 0.04381 -0.00560 0.00186 -0.00205 C7 1 0.177701 0.416869 0.599635 11.00000 0.04333 0.05718 = 0.03772 -0.00625 0.00179 0.00092 C8 1 0.139104 0.357329 0.645448 11.00000 0.05077 0.06808 = 0.07338 -0.00589 0.00534 -0.00585 AFIX 43 H8 2 0.165350 0.314905 0.668819 11.00000 -1.20000 AFIX 0 C9 1 0.061405 0.360193 0.656970 11.00000 0.05419 0.09559 = 0.07682 -0.00797 0.00866 -0.02161 AFIX 43 H9 2 0.035649 0.319885 0.688111 11.00000 -1.20000 AFIX 0 C10 1 0.022840 0.422428 0.622418 11.00000 0.04435 0.13722 = 0.06533 -0.01298 -0.00019 -0.00042 AFIX 43 H10 2 -0.029432 0.423813 0.627684 11.00000 -1.20000 AFIX 0 C11 1 0.060851 0.482419 0.580283 11.00000 0.06026 0.11484 = 0.07067 0.00983 0.00089 0.03111 AFIX 43 H11 2 0.034526 0.525388 0.559321 11.00000 -1.20000 AFIX 0 C12 1 0.138530 0.479953 0.568378 11.00000 0.06222 0.06935 = 0.05354 0.00546 0.00827 0.00836 AFIX 43 H12 2 0.164078 0.521079 0.539195 11.00000 -1.20000 AFIX 0 C13 1 0.254137 0.397193 0.394083 11.00000 0.03770 0.04462 = 0.03884 0.00166 -0.00010 0.00206 C14 1 0.223741 0.328109 0.368230 11.00000 0.05543 0.04784 = 0.05060 0.00495 -0.01087 -0.00168 AFIX 43 H14 2 0.225656 0.288776 0.418497 11.00000 -1.20000 AFIX 0 C15 1 0.190349 0.317495 0.267154 11.00000 0.06168 0.06068 = 0.06138 -0.00818 -0.01443 -0.01027 AFIX 43 H15 2 0.170039 0.270636 0.250014 11.00000 -1.20000 AFIX 0 C16 1 0.186482 0.374774 0.191240 11.00000 0.05269 0.09319 = 0.04468 0.00834 -0.00809 -0.00838 C17 1 0.215752 0.443516 0.219504 11.00000 0.07201 0.08142 = 0.05717 0.02623 -0.01544 -0.01475 AFIX 43 H17 2 0.212281 0.483270 0.170120 11.00000 -1.20000 AFIX 0 C18 1 0.250377 0.455371 0.319682 11.00000 0.06147 0.05439 = 0.05893 0.00844 -0.00900 -0.01129 AFIX 43 H18 2 0.270894 0.502189 0.336535 11.00000 -1.20000 AFIX 0 C19 1 0.150319 0.361943 0.079823 11.00000 0.10315 0.16027 = 0.05906 0.01101 -0.02961 -0.03529 AFIX 137 H19A 2 0.153502 0.309491 0.061090 11.00000 -1.50000 H19B 2 0.176268 0.391294 0.025594 11.00000 -1.50000 H19C 2 0.098367 0.376946 0.082474 11.00000 -1.50000 AFIX 0 C20 1 0.579144 0.401116 0.541313 11.00000 0.05361 0.03822 = 0.04972 -0.00690 0.00506 -0.00278 HKLF 4 REM mob423 in P4(1)2(1)2 REM wR2 = 0.0848, GooF = S = 1.015, Restrained GooF = 1.015 for all data REM R1 = 0.0386 for 3394 Fo > 4sig(Fo) and 0.0597 for all 4404 data REM 223 parameters refined using 0 restraints END WGHT 0.0307 0.8006 REM Highest difference peak 0.282, deepest hole -0.153, 1-sigma level 0.035 Q1 1 0.6629 0.3973 0.4948 11.00000 0.05 0.28 Q2 1 0.2013 0.3365 0.0326 11.00000 0.05 0.15 Q3 1 0.3240 0.3985 0.9635 11.00000 0.05 0.14 Q4 1 0.3940 0.4176 0.5884 11.00000 0.05 0.13 Q5 1 0.2839 0.4075 0.6395 11.00000 0.05 0.12 Q6 1 0.5356 0.4015 0.5804 11.00000 0.05 0.12 Q7 1 0.3400 0.4103 0.4783 11.00000 0.05 0.12 Q8 1 0.2808 0.4176 0.3490 11.00000 0.05 0.12 Q9 1 0.1794 0.3644 0.1373 11.00000 0.05 0.12 Q10 1 -0.0221 0.4642 0.6451 11.00000 0.05 0.11 Q11 1 0.2004 0.3009 0.4529 11.00000 0.05 0.11 Q12 1 0.2421 0.2403 0.0837 11.00000 0.05 0.11 Q13 1 0.5219 0.3806 0.4969 11.00000 0.05 0.11 Q14 1 0.4192 0.4417 0.7896 11.00000 0.05 0.11 Q15 1 0.4099 0.4100 1.0000 10.50000 0.05 0.11 Q16 1 0.3783 0.4597 0.5413 11.00000 0.05 0.11 Q17 1 0.0943 0.2826 0.7466 11.00000 0.05 0.11 Q18 1 0.0328 0.3637 0.7509 11.00000 0.05 0.11 Q19 1 0.2260 0.4310 0.3704 11.00000 0.05 0.11 Q20 1 0.1986 0.3391 0.2117 11.00000 0.05 0.11 ; _shelx_res_checksum 2460 _shelx_fab_file ; -22 -6 -2 0.1884 -0.1780 -22 -6 -1 0.1016 -0.7299 -22 -5 -3 -0.3933 -0.6721 -22 -5 -2 0.0948 0.7069 -22 -5 -1 -0.1575 -0.5431 -22 -4 -3 -0.1123 -0.4101 -22 -4 -2 -0.8549 0.3481 -22 -4 -1 -0.3880 -0.0478 -22 -3 -4 -0.7205 0.2582 -22 -3 -3 0.5728 0.1803 -22 -3 -2 -0.2247 0.3679 -22 -3 -1 1.1401 0.2157 -22 -2 -4 0.7575 -0.0341 -22 -2 -3 0.6054 0.7772 -22 -2 -2 0.2234 -0.6953 -22 -2 -1 -0.2819 -0.4205 -22 -1 -4 0.3661 0.1929 -22 -1 -3 -0.7027 -0.6857 -22 -1 -2 -0.3725 -0.5779 -22 -1 -1 -0.4476 0.2507 -21 -9 -2 0.3239 -0.2326 -21 -9 -1 0.3041 0.4760 -21 -8 -3 -0.1761 -0.1769 -21 -8 -2 0.4480 -0.4498 -21 -8 -1 0.0754 -0.1505 -21 -7 -4 0.2278 0.4376 -21 -7 -3 -0.3138 -0.0336 -21 -7 -2 0.3334 -0.0113 -21 -7 -1 -0.2133 -0.6966 -21 -6 -5 0.2159 0.1363 -21 -6 -4 -0.0359 0.4182 -21 -6 -3 -0.6122 -0.4265 -21 -6 -2 -0.2681 0.4488 -21 -6 -1 -0.8566 -0.8541 -21 -5 -5 -0.6602 -0.2066 -21 -5 -4 -0.7494 0.4942 -21 -5 -3 0.4299 -0.4206 -21 -5 -2 -0.5996 0.6134 -21 -5 -1 0.8315 -0.2085 -21 -4 -5 0.2993 0.3455 -21 -4 -4 0.1007 0.2693 -21 -4 -3 0.8123 0.3877 -21 -4 -2 -0.3488 0.0409 -21 -4 -1 0.4065 -0.1632 -21 -3 -6 1.3568 -0.1159 -21 -3 -5 0.8161 0.3902 -21 -3 -4 -0.1282 0.0919 -21 -3 -3 -0.0485 0.3752 -21 -3 -2 -0.5039 -0.8472 -21 -3 -1 -0.2765 0.3534 -21 -2 -6 0.3889 0.1005 -21 -2 -5 -0.3368 0.1623 -21 -2 -4 -0.0113 -0.3027 -21 -2 -3 -0.1175 0.0336 -21 -2 -2 0.4202 0.1961 -21 -2 -1 0.1711 0.2621 -21 -1 -6 0.2357 0.3860 -21 -1 -5 0.1406 -0.4772 -21 -1 -4 0.2477 -0.0298 -21 -1 -3 0.3666 0.1292 -21 -1 -2 -0.1146 0.1140 -21 -1 -1 -0.5129 -0.3391 -20 -11 -2 0.0684 -0.1031 -20 -11 -1 0.4710 0.3765 -20 -10 -3 0.2922 -0.6883 -20 -10 -2 0.2460 0.0008 -20 -10 -1 -0.0369 0.8506 -20 -9 -4 -0.5038 -0.0942 -20 -9 -3 0.1106 0.1287 -20 -9 -2 0.2032 -0.4162 -20 -9 -1 -0.0603 0.2353 -20 -8 -5 -0.2484 0.5393 -20 -8 -4 -0.6340 0.3900 -20 -8 -3 -0.7165 -0.1756 -20 -8 -2 0.1281 -0.1181 -20 -8 -1 -0.4190 -0.8400 -20 -7 -6 0.0593 0.5775 -20 -7 -5 -0.2763 0.4510 -20 -7 -4 -0.4593 0.0337 -20 -7 -3 0.0448 0.2910 -20 -7 -2 0.0564 0.1406 -20 -7 -1 0.2819 -1.2017 -20 -6 -6 -0.4308 0.0840 -20 -6 -5 0.0128 -0.0696 -20 -6 -4 0.8367 0.4610 -20 -6 -3 0.2592 -0.2326 -20 -6 -2 -0.3062 0.1798 -20 -6 -1 -0.0113 -0.4965 -20 -5 -7 -0.4567 0.1081 -20 -5 -6 0.3040 0.0099 -20 -5 -5 0.8861 0.0685 -20 -5 -4 -0.5178 -0.0408 -20 -5 -3 -0.1804 -0.2099 -20 -5 -2 -0.7200 0.1141 -20 -5 -1 -0.4866 0.1769 -20 -4 -7 0.5375 0.5713 -20 -4 -6 0.2322 0.0347 -20 -4 -5 -0.6112 0.3208 -20 -4 -4 -0.8434 -0.0500 -20 -4 -3 0.4320 0.5147 -20 -4 -2 -0.3495 0.1128 -20 -4 -1 0.6776 0.3098 -20 -3 -7 -1.1869 0.0841 -20 -3 -6 -0.1113 0.0309 -20 -3 -5 0.2078 0.4182 -20 -3 -4 0.9090 -0.0418 -20 -3 -3 0.4699 0.7202 -20 -3 -2 0.1035 -0.4144 -20 -3 -1 -0.0241 -0.0765 -20 -2 -7 -0.1920 -0.8536 -20 -2 -6 1.2085 0.0332 -20 -2 -5 0.4071 -0.2387 -20 -2 -4 0.5977 -0.2524 -20 -2 -3 -0.4639 -0.2517 -20 -2 -2 -0.2701 -0.4365 -20 -2 -1 -0.2556 0.5598 -20 -1 -7 0.3879 -1.3185 -20 -1 -6 -0.5021 0.4912 -20 -1 -5 -0.1494 -0.5304 -20 -1 -4 -0.2778 -0.2450 -20 -1 -3 -0.2880 -0.1044 -20 -1 -2 0.3436 0.5049 -20 -1 -1 0.0017 0.6920 -19 -12 -3 0.0606 -0.3923 -19 -12 -2 -0.2783 0.2212 -19 -12 -1 -0.8378 0.6414 -19 -11 -4 0.1491 -0.1742 -19 -11 -3 0.1625 0.5933 -19 -11 -2 -0.1558 0.2425 -19 -11 -1 -0.0189 0.6034 -19 -10 -5 -0.4340 -0.1170 -19 -10 -4 -0.3444 0.2657 -19 -10 -3 -0.1012 -0.6480 -19 -10 -2 0.2994 -0.5373 -19 -10 -1 0.2620 0.2836 -19 -9 -6 -0.1260 0.4275 -19 -9 -5 -0.4498 0.2877 -19 -9 -4 -0.9365 -0.8381 -19 -9 -3 -0.1526 0.0490 -19 -9 -2 0.5065 -0.0625 -19 -9 -1 0.1795 -0.8410 -19 -8 -7 0.1514 -0.0523 -19 -8 -6 -0.1222 0.8239 -19 -8 -5 -0.4670 0.0132 -19 -8 -4 0.2308 0.4825 -19 -8 -3 -0.2711 0.5325 -19 -8 -2 -0.1065 -0.2990 -19 -8 -1 -0.5421 -1.1831 -19 -7 -7 0.2265 0.0731 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19 9 3 -0.1526 -0.0490 19 9 4 -0.9365 0.8381 19 9 5 -0.4498 -0.2877 19 9 6 -0.1260 -0.4275 19 10 0 1.3511 0.0066 19 10 1 0.2620 -0.2836 19 10 2 0.2994 0.5373 19 10 3 -0.1012 0.6480 19 10 4 -0.3444 -0.2657 19 10 5 -0.4340 0.1170 19 11 0 0.6290 -0.0168 19 11 1 -0.0189 -0.6034 19 11 2 -0.1558 -0.2425 19 11 3 0.1625 -0.5933 19 11 4 0.1491 0.1742 19 12 0 -0.9371 0.0202 19 12 1 -0.8378 -0.6414 19 12 2 -0.2783 -0.2212 19 12 3 0.0606 0.3923 19 13 0 -1.4301 0.0155 20 0 0 0.8001 0.1119 20 0 1 -0.1102 0.0058 20 0 2 0.0144 -0.1269 20 0 3 0.3234 -0.3397 20 0 4 -0.2633 -0.0146 20 0 5 0.1661 0.2008 20 0 6 -0.0101 -0.2004 20 0 7 0.2232 -0.2613 20 1 0 -0.1195 0.0832 20 1 1 0.0017 -0.6920 20 1 2 0.3436 -0.5049 20 1 3 -0.2880 0.1044 20 1 4 -0.2778 0.2450 20 1 5 -0.1494 0.5304 20 1 6 -0.5021 -0.4912 20 1 7 0.3879 1.3185 20 2 0 -0.1959 -0.0001 20 2 1 -0.2556 -0.5598 20 2 2 -0.2701 0.4365 20 2 3 -0.4639 0.2517 20 2 4 0.5977 0.2524 20 2 5 0.4071 0.2387 20 2 6 1.2085 -0.0332 20 2 7 -0.1920 0.8536 20 3 0 -0.9197 0.0264 20 3 1 -0.0241 0.0765 20 3 2 0.1035 0.4144 20 3 3 0.4699 -0.7202 20 3 4 0.9090 0.0418 20 3 5 0.2078 -0.4182 20 3 6 -0.1113 -0.0309 20 3 7 -1.1869 -0.0841 20 4 0 0.2051 -0.0246 20 4 1 0.6776 -0.3098 20 4 2 -0.3495 -0.1128 20 4 3 0.4320 -0.5147 20 4 4 -0.8434 0.0500 20 4 5 -0.6112 -0.3208 20 4 6 0.2322 -0.0347 20 4 7 0.5375 -0.5713 20 5 0 -0.3843 -0.0031 20 5 1 -0.4866 -0.1769 20 5 2 -0.7200 -0.1141 20 5 3 -0.1804 0.2099 20 5 4 -0.5178 0.0408 20 5 5 0.8861 -0.0685 20 5 6 0.3040 -0.0099 20 5 7 -0.4567 -0.1081 20 6 0 -1.8676 -0.0619 20 6 1 -0.0113 0.4965 20 6 2 -0.3062 -0.1798 20 6 3 0.2592 0.2326 20 6 4 0.8367 -0.4610 20 6 5 0.0128 0.0696 20 6 6 -0.4308 -0.0840 20 7 0 0.1428 -0.0233 20 7 1 0.2819 1.2017 20 7 2 0.0564 -0.1406 20 7 3 0.0448 -0.2910 20 7 4 -0.4593 -0.0337 20 7 5 -0.2763 -0.4510 20 7 6 0.0593 -0.5775 20 8 0 1.3567 0.0209 20 8 1 -0.4190 0.8400 20 8 2 0.1281 0.1181 20 8 3 -0.7165 0.1756 20 8 4 -0.6340 -0.3900 20 8 5 -0.2484 -0.5393 20 9 0 1.2150 0.0035 20 9 1 -0.0603 -0.2353 20 9 2 0.2032 0.4162 20 9 3 0.1106 -0.1287 20 9 4 -0.5038 0.0942 20 10 0 0.3066 0.0262 20 10 1 -0.0369 -0.8506 20 10 2 0.2460 -0.0008 20 10 3 0.2922 0.6883 20 11 0 -1.1251 0.0083 20 11 1 0.4710 -0.3765 20 11 2 0.0684 0.1031 21 0 1 0.3561 -0.3680 21 0 2 -0.5901 0.0596 21 0 3 -0.0238 -0.0074 21 0 4 0.0131 0.0456 21 0 5 -0.0978 0.0952 21 0 6 0.1789 -0.0076 21 1 0 -0.3248 0.0736 21 1 1 -0.5129 0.3391 21 1 2 -0.1146 -0.1140 21 1 3 0.3666 -0.1292 21 1 4 0.2477 0.0298 21 1 5 0.1406 0.4772 21 1 6 0.2357 -0.3860 21 2 0 -0.1383 0.0056 21 2 1 0.1711 -0.2621 21 2 2 0.4202 -0.1961 21 2 3 -0.1175 -0.0336 21 2 4 -0.0113 0.3027 21 2 5 -0.3368 -0.1623 21 2 6 0.3889 -0.1005 21 3 0 0.1474 -0.0256 21 3 1 -0.2765 -0.3534 21 3 2 -0.5039 0.8472 21 3 3 -0.0485 -0.3752 21 3 4 -0.1282 -0.0919 21 3 5 0.8161 -0.3902 21 3 6 1.3568 0.1159 21 4 0 -1.3121 -0.0263 21 4 1 0.4065 0.1632 21 4 2 -0.3488 -0.0409 21 4 3 0.8123 -0.3877 21 4 4 0.1007 -0.2693 21 4 5 0.2993 -0.3455 21 5 0 0.0714 -0.0554 21 5 1 0.8315 0.2085 21 5 2 -0.5996 -0.6134 21 5 3 0.4299 0.4206 21 5 4 -0.7494 -0.4942 21 5 5 -0.6602 0.2066 21 6 0 0.0212 0.0027 21 6 1 -0.8566 0.8541 21 6 2 -0.2681 -0.4488 21 6 3 -0.6122 0.4265 21 6 4 -0.0359 -0.4182 21 6 5 0.2159 -0.1363 21 7 0 -0.1131 -0.0088 21 7 1 -0.2133 0.6966 21 7 2 0.3334 0.0113 21 7 3 -0.3138 0.0336 21 7 4 0.2278 -0.4376 21 8 0 1.4451 0.0267 21 8 1 0.0754 0.1505 21 8 2 0.4480 0.4498 21 8 3 -0.1761 0.1769 21 9 0 0.3971 0.0339 21 9 1 0.3041 -0.4760 21 9 2 0.3239 0.2326 22 0 0 -0.2154 0.0988 22 0 1 0.0296 -0.0150 22 0 2 0.0173 -1.1623 22 0 3 -0.3389 0.3217 22 0 4 -0.6834 -0.0149 22 1 0 0.3308 -0.0318 22 1 1 -0.4476 -0.2507 22 1 2 -0.3725 0.5779 22 1 3 -0.7027 0.6857 22 1 4 0.3661 -0.1929 22 2 0 -0.7194 -0.0214 22 2 1 -0.2819 0.4205 22 2 2 0.2234 0.6953 22 2 3 0.6054 -0.7772 22 2 4 0.7575 0.0341 22 3 0 0.2131 -0.0342 22 3 1 1.1401 -0.2157 22 3 2 -0.2247 -0.3679 22 3 3 0.5728 -0.1803 22 3 4 -0.7205 -0.2582 22 4 0 0.2189 -0.0138 22 4 1 -0.3880 0.0478 22 4 2 -0.8549 -0.3481 22 4 3 -0.1123 0.4101 22 5 0 -1.3924 -0.0231 22 5 1 -0.1575 0.5431 22 5 2 0.0948 -0.7069 22 5 3 -0.3933 0.6721 22 6 0 0.6363 -0.0227 22 6 1 0.1016 0.7299 22 6 2 0.1884 0.1780 23 1 0 0.2033 0.0191 0 0 0 0.0 0.0 ; _shelx_fab_checksum 7327 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' 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 0.40619(2) 0.40619(2) 0.500000 0.03912(16) Uani 1 2 d S T P . . S1 S 0.66849(6) 0.39624(8) 0.57205(11) 0.0844(4) Uani 1 1 d . . . . . N1 N 0.38434(14) 0.41886(14) 0.65718(17) 0.0408(6) Uani 1 1 d . . . . . N2 N 0.29589(13) 0.40723(14) 0.49458(17) 0.0376(5) Uani 1 1 d . . . . . N3 N 0.51582(16) 0.40575(17) 0.52120(19) 0.0489(7) Uani 1 1 d . . . . . C1 C 0.43359(19) 0.42553(19) 0.7392(2) 0.0505(8) Uani 1 1 d . . . . . H1 H 0.484789 0.423535 0.723119 0.061 Uiso 1 1 calc R U . . . C2 C 0.4118(2) 0.4353(2) 0.8469(2) 0.0619(10) Uani 1 1 d . . . . . H2 H 0.447819 0.440467 0.901735 0.074 Uiso 1 1 calc R U . . . C3 C 0.3369(2) 0.4372(2) 0.8721(3) 0.0679(12) Uani 1 1 d . . . . . H3 H 0.321198 0.443101 0.944306 0.081 Uiso 1 1 calc R U . . . C4 C 0.2848(2) 0.4302(2) 0.7887(2) 0.0593(11) Uani 1 1 d . . . . . H4 H 0.233421 0.431918 0.803691 0.071 Uiso 1 1 calc R U . . . C5 C 0.31025(18) 0.42069(18) 0.6826(2) 0.0425(8) Uani 1 1 d . . . . . C6 C 0.26033(16) 0.41414(19) 0.5868(2) 0.0402(7) Uani 1 1 d . . . . . C7 C 0.17770(19) 0.4169(2) 0.5996(2) 0.0461(8) Uani 1 1 d . . . . . C8 C 0.1391(2) 0.3573(2) 0.6454(3) 0.0641(10) Uani 1 1 d . . . . . H8 H 0.165350 0.314905 0.668819 0.077 Uiso 1 1 calc R U . . . C9 C 0.0614(2) 0.3602(3) 0.6570(3) 0.0755(13) Uani 1 1 d . . . . . H9 H 0.035649 0.319885 0.688111 0.091 Uiso 1 1 calc R U . . . C10 C 0.0228(2) 0.4224(3) 0.6224(3) 0.0823(15) Uani 1 1 d . . . . . H10 H -0.029432 0.423813 0.627684 0.099 Uiso 1 1 calc R U . . . C11 C 0.0609(3) 0.4824(3) 0.5803(3) 0.0819(14) Uani 1 1 d . . . . . H11 H 0.034526 0.525388 0.559321 0.098 Uiso 1 1 calc R U . . . C12 C 0.1385(2) 0.4800(2) 0.5684(3) 0.0617(11) Uani 1 1 d . . . . . H12 H 0.164078 0.521079 0.539195 0.074 Uiso 1 1 calc R U . . . C13 C 0.25414(17) 0.3972(2) 0.3941(2) 0.0404(7) Uani 1 1 d . . . . . C14 C 0.2237(2) 0.3281(2) 0.3682(3) 0.0513(9) Uani 1 1 d . . . . . H14 H 0.225656 0.288776 0.418497 0.062 Uiso 1 1 calc R U . . . C15 C 0.1903(2) 0.3175(2) 0.2672(3) 0.0612(10) Uani 1 1 d . . . . . H15 H 0.170039 0.270636 0.250014 0.073 Uiso 1 1 calc R U . . . C16 C 0.1865(2) 0.3748(3) 0.1912(3) 0.0635(11) Uani 1 1 d . . . . . C17 C 0.2158(2) 0.4435(3) 0.2195(3) 0.0702(12) Uani 1 1 d . . . . . H17 H 0.212281 0.483270 0.170120 0.084 Uiso 1 1 calc R U . . . C18 C 0.2504(2) 0.4554(2) 0.3197(3) 0.0583(10) Uani 1 1 d . . . . . H18 H 0.270894 0.502189 0.336535 0.070 Uiso 1 1 calc R U . . . C19 C 0.1503(3) 0.3619(3) 0.0798(3) 0.1075(19) Uani 1 1 d . . . . . H19A H 0.153502 0.309491 0.061090 0.161 Uiso 1 1 calc R U . . . H19B H 0.176268 0.391294 0.025594 0.161 Uiso 1 1 calc R U . . . H19C H 0.098367 0.376946 0.082474 0.161 Uiso 1 1 calc R U . . . C20 C 0.5791(2) 0.40112(18) 0.5413(2) 0.0472(8) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0405(2) 0.0405(2) 0.0363(3) -0.00276(18) 0.00276(18) -0.0026(3) S1 0.0505(7) 0.0831(9) 0.1195(9) -0.0090(7) -0.0141(6) 0.0056(6) N1 0.0421(16) 0.0433(16) 0.0370(11) -0.0053(10) -0.0010(10) -0.0038(12) N2 0.0384(14) 0.0376(14) 0.0367(11) 0.0010(13) -0.0002(10) -0.0029(12) N3 0.0429(17) 0.0519(18) 0.0520(14) -0.0057(14) 0.0072(12) -0.0034(15) C1 0.0461(19) 0.062(2) 0.0431(15) -0.0069(15) -0.0032(14) -0.0018(15) C2 0.056(2) 0.089(3) 0.0406(15) -0.0094(15) -0.0075(16) 0.000(2) C3 0.063(3) 0.103(4) 0.0378(16) -0.0145(18) 0.0046(17) 0.003(2) C4 0.044(2) 0.088(3) 0.0452(16) -0.0156(17) 0.0061(14) 0.0012(19) C5 0.0418(19) 0.046(2) 0.0397(14) -0.0076(13) 0.0011(13) -0.0011(15) C6 0.0359(17) 0.0409(19) 0.0438(14) -0.0056(14) 0.0019(12) -0.0020(15) C7 0.0433(19) 0.057(2) 0.0377(14) -0.0062(15) 0.0018(13) 0.0009(17) C8 0.051(3) 0.068(3) 0.073(2) -0.006(2) 0.0053(19) -0.006(2) C9 0.054(3) 0.096(4) 0.077(3) -0.008(2) 0.009(2) -0.022(2) C10 0.044(3) 0.137(5) 0.065(2) -0.013(3) -0.0002(19) 0.000(3) C11 0.060(3) 0.115(4) 0.071(3) 0.010(3) 0.001(2) 0.031(3) C12 0.062(3) 0.069(3) 0.054(2) 0.0055(19) 0.0083(18) 0.008(2) C13 0.0377(17) 0.045(2) 0.0388(14) 0.0017(14) -0.0001(12) 0.0021(15) C14 0.055(2) 0.048(2) 0.0506(17) 0.0050(15) -0.0109(16) -0.0017(17) C15 0.062(3) 0.061(2) 0.061(2) -0.0082(18) -0.0144(18) -0.0103(19) C16 0.053(2) 0.093(3) 0.0447(17) 0.0083(19) -0.0081(16) -0.008(2) C17 0.072(3) 0.081(3) 0.057(2) 0.026(2) -0.0154(19) -0.015(2) C18 0.061(3) 0.054(2) 0.0589(19) 0.0084(18) -0.0090(17) -0.0113(19) C19 0.103(4) 0.160(6) 0.059(2) 0.011(3) -0.030(3) -0.035(4) C20 0.054(2) 0.0382(19) 0.0497(14) -0.0069(13) 0.0051(14) -0.0028(17) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 N2 Fe1 N2 91.14(15) 7_556 . ? N2 Fe1 N3 88.98(12) 7_556 . ? N2 Fe1 N3 174.35(9) . . ? N2 Fe1 N3 174.35(9) 7_556 7_556 ? N2 Fe1 N3 88.98(12) . 7_556 ? N3 Fe1 N3 91.45(18) . 7_556 ? N2 Fe1 N1 94.76(10) 7_556 . ? N2 Fe1 N1 80.52(10) . . ? N3 Fe1 N1 93.84(10) . . ? N3 Fe1 N1 90.84(10) 7_556 . ? N2 Fe1 N1 80.52(10) 7_556 7_556 ? N2 Fe1 N1 94.76(10) . 7_556 ? N3 Fe1 N1 90.84(10) . 7_556 ? N3 Fe1 N1 93.84(10) 7_556 7_556 ? N1 Fe1 N1 173.30(15) . 7_556 ? C1 N1 C5 117.6(2) . . ? C1 N1 Fe1 127.7(2) . . ? C5 N1 Fe1 114.70(18) . . ? C6 N2 C13 120.0(2) . . ? C6 N2 Fe1 117.24(19) . . ? C13 N2 Fe1 122.70(18) . . ? C20 N3 Fe1 173.9(3) . . ? N1 C1 C2 122.8(3) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C3 C2 C1 119.4(3) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? C2 C3 C4 118.9(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C4 C5 118.9(3) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? N1 C5 C4 122.4(3) . . ? N1 C5 C6 113.6(2) . . ? C4 C5 C6 123.9(3) . . ? N2 C6 C5 113.9(3) . . ? N2 C6 C7 125.3(3) . . ? C5 C6 C7 120.8(2) . . ? C12 C7 C8 119.1(3) . . ? C12 C7 C6 120.1(3) . . ? C8 C7 C6 120.8(3) . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C11 C10 C9 120.1(4) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 120.5(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C7 C12 C11 120.0(4) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C18 119.8(3) . . ? C14 C13 N2 120.4(3) . . ? C18 C13 N2 119.5(3) . . ? C13 C14 C15 119.6(3) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 121.5(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C17 C16 C15 117.9(3) . . ? C17 C16 C19 121.2(4) . . ? C15 C16 C19 120.8(4) . . ? C16 C17 C18 121.7(4) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C13 C18 C17 119.4(4) . . ? C13 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 S1 178.6(3) . . ? 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 N2 1.958(2) 7_556 ? Fe1 N2 1.958(2) . ? Fe1 N3 1.962(3) . ? Fe1 N3 1.962(3) 7_556 ? Fe1 N1 1.971(2) . ? Fe1 N1 1.971(2) 7_556 ? S1 C20 1.631(4) . ? N1 C1 1.334(4) . ? N1 C5 1.351(4) . ? N2 C6 1.297(3) . ? N2 C13 1.444(3) . ? N3 C20 1.153(4) . ? C1 C2 1.383(4) . ? C1 H1 0.9300 . ? C2 C3 1.364(5) . ? C2 H2 0.9300 . ? C3 C4 1.381(5) . ? C3 H3 0.9300 . ? C4 C5 1.383(4) . ? C4 H4 0.9300 . ? C5 C6 1.472(4) . ? C6 C7 1.475(4) . ? C7 C12 1.372(5) . ? C7 C8 1.378(5) . ? C8 C9 1.387(5) . ? C8 H8 0.9300 . ? C9 C10 1.366(7) . ? C9 H9 0.9300 . ? C10 C11 1.361(7) . ? C10 H10 0.9300 . ? C11 C12 1.387(6) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.376(5) . ? C13 C18 1.377(5) . ? C14 C15 1.382(4) . ? C14 H14 0.9300 . ? C15 C16 1.377(5) . ? C15 H15 0.9300 . ? C16 C17 1.370(5) . ? C16 C19 1.521(5) . ? C17 C18 1.385(5) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? 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 C5 N1 C1 C2 -1.0(5) . . . . ? Fe1 N1 C1 C2 179.1(3) . . . . ? N1 C1 C2 C3 1.0(6) . . . . ? C1 C2 C3 C4 -0.8(6) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C1 N1 C5 C4 1.0(5) . . . . ? Fe1 N1 C5 C4 -179.1(3) . . . . ? C1 N1 C5 C6 179.1(3) . . . . ? Fe1 N1 C5 C6 -1.0(4) . . . . ? C3 C4 C5 N1 -0.8(6) . . . . ? C3 C4 C5 C6 -178.7(3) . . . . ? C13 N2 C6 C5 177.5(3) . . . . ? Fe1 N2 C6 C5 0.4(4) . . . . ? C13 N2 C6 C7 -3.5(5) . . . . ? Fe1 N2 C6 C7 179.3(3) . . . . ? N1 C5 C6 N2 0.4(4) . . . . ? C4 C5 C6 N2 178.5(3) . . . . ? N1 C5 C6 C7 -178.6(3) . . . . ? C4 C5 C6 C7 -0.5(5) . . . . ? N2 C6 C7 C12 -72.9(4) . . . . ? C5 C6 C7 C12 106.0(4) . . . . ? N2 C6 C7 C8 108.8(4) . . . . ? C5 C6 C7 C8 -72.3(4) . . . . ? C12 C7 C8 C9 1.8(5) . . . . ? C6 C7 C8 C9 -179.8(3) . . . . ? C7 C8 C9 C10 0.1(6) . . . . ? C8 C9 C10 C11 -2.2(7) . . . . ? C9 C10 C11 C12 2.3(7) . . . . ? C8 C7 C12 C11 -1.8(5) . . . . ? C6 C7 C12 C11 179.9(3) . . . . ? C10 C11 C12 C7 -0.3(7) . . . . ? C6 N2 C13 C14 -77.6(4) . . . . ? Fe1 N2 C13 C14 99.3(3) . . . . ? C6 N2 C13 C18 107.9(4) . . . . ? Fe1 N2 C13 C18 -75.1(4) . . . . ? C18 C13 C14 C15 0.7(5) . . . . ? N2 C13 C14 C15 -173.7(3) . . . . ? C13 C14 C15 C16 -0.2(6) . . . . ? C14 C15 C16 C17 -1.1(6) . . . . ? C14 C15 C16 C19 179.3(4) . . . . ? C15 C16 C17 C18 1.9(7) . . . . ? C19 C16 C17 C18 -178.5(4) . . . . ? C14 C13 C18 C17 0.1(5) . . . . ? N2 C13 C18 C17 174.6(3) . . . . ? C16 C17 C18 C13 -1.5(6) . . . . ?