#------------------------------------------------------------------------------ #$Date: 2022-05-25 01:50:28 +0300 (Wed, 25 May 2022) $ #$Revision: 275631 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/71/03/7710319.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_7710319 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_formula_moiety '2(C38 H26 Br2 Fe N6 S2)' _chemical_formula_sum 'C76 H52 Br4 Fe2 N12 S4' _chemical_formula_weight 1692.87 _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 difmap _audit_creation_date 2022-05-05 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2022-05-08 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 2 _cell_length_a 17.7390(4) _cell_length_b 17.7390(4) _cell_length_c 12.1851(4) _cell_measurement_reflns_used 9828 _cell_measurement_temperature 299(2) _cell_measurement_theta_max 26.35 _cell_measurement_theta_min 2.30 _cell_volume 3834.31(18) _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 298.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0632 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 81914 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.425 _diffrn_reflns_theta_min 2.296 _exptl_absorpt_coefficient_mu 2.621 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.5202 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1187 before and 0.0663 after correction. The Ratio of minimum to maximum transmission is 0.6979. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.466 _exptl_crystal_description block _exptl_crystal_F_000 1696 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.362 _refine_diff_density_min -0.371 _refine_diff_density_rms 0.049 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.046(16) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment noref _refine_ls_matrix_type full _refine_ls_number_parameters 223 _refine_ls_number_reflns 3939 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0596 _refine_ls_R_factor_gt 0.0450 _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^)+(0.0263P)^2^+3.1668P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.0821 _reflns_Friedel_coverage 0.728 _reflns_Friedel_fraction_full 1.000 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 3239 _reflns_number_total 3939 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2dt00416j2.cif _cod_data_source_block 327brrt_0ma _cod_original_cell_volume 3834.3(2) _cod_database_code 7710319 _shelx_shelxl_version_number 2014/7 _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_max 0.859 _shelx_estimated_absorpt_t_min 0.572 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.954(16) 0.046(16) 2. Others Fixed Uiso: H1(0.058) H2(0.073) H3(0.08) H4(0.067) H8(0.071) H9(0.092) H10(0.092) H11(0.09) H12(0.073) H14(0.059) H15(0.068) H17(0.075) H18(0.067) Fixed X: H1(0.483809) H2(0.446508) H3(0.318901) H4(0.232659) H8(0.16431) H9(0.03424) H10(-0.02872) H11(0.034439) H12(0.16503) H14(0.22854) H15(0.17599) H17(0.21594) H18(0.273629) Fixed Y: H1(0.42383) H2(0.439139) H3(0.44111) H4(0.430519) H8(0.31799) H9(0.32497) H10(0.42752) H11(0.52429) H12(0.52031) H14(0.29028) H15(0.26972) H17(0.484369) H18(0.50344) Fixed Z: Fe1(0.5) H1(0.725181) H2(0.902909) H3(0.944679) H4(0.80239) H8(0.67149) H9(0.688931) H10(0.620821) H11(0.54433) H12(0.52608) H14(0.41616) H15(0.24297) H17(0.165381) H18(0.3354) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; 327brrt_0ma.res created by SHELXL-2014/7 TITL 327BRRT_0ma in P41212 #92 REM reset to P41212 #92 CELL 0.71073 17.739 17.739 12.1851 90 90 90 ZERR 2 0.00042 0.00042 0.0004 0 0 0 LATT -1 SYMM 0.5-Y,0.5+X,0.25+Z SYMM -X,-Y,0.5+Z SYMM 0.5+Y,0.5-X,0.75+Z SYMM 0.5+X,0.5-Y,0.75-Z SYMM 0.5-X,0.5+Y,0.25-Z SYMM +Y,+X,-Z SYMM -Y,-X,0.5-Z SFAC C H Br Fe N S UNIT 152 104 8 4 24 8 L.S. 10 PLAN 5 SIZE 0.24 0.1 0.06 TEMP 25 CONF BOND MORE -1 BOND $H ABIN fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 2 2 1 OMIT 0 1 1 OMIT 1 1 0 OMIT 3 6 2 REM REM REM WGHT 0.026300 3.166800 BASF 0.04572 FVAR 0.12022 BR1 3 0.149323 0.358380 0.049546 11.00000 0.12705 0.13717 = 0.05323 0.01607 -0.04217 -0.04818 FE1 4 0.407184 0.407184 10.500000 10.50000 0.03813 0.03813 = 0.03039 -0.00282 0.00282 -0.00280 S1 6 0.669825 0.395316 0.568811 11.00000 0.04938 0.07851 = 0.12880 -0.01304 -0.01893 0.00562 N1 5 0.384010 0.419933 0.657609 11.00000 0.03706 0.03799 = 0.03569 -0.00793 -0.00047 -0.00534 N2 5 0.296308 0.407995 0.493855 11.00000 0.03545 0.03108 = 0.03155 0.00061 0.00019 -0.00497 N3 5 0.516858 0.406344 0.523003 11.00000 0.04336 0.04519 = 0.04791 -0.00299 0.00853 -0.00217 C1 1 0.432631 0.426736 0.739639 11.00000 0.03742 0.05771 = 0.03893 -0.00800 -0.00023 -0.00082 H1 2 10.483809 10.423830 10.725181 11.00000 10.05800 C2 1 0.410400 0.435097 0.848214 11.00000 0.05462 0.08301 = 0.04108 -0.01318 -0.00202 0.00121 H2 2 10.446508 10.439139 10.902909 11.00000 10.07300 C3 1 0.335179 0.436551 0.872657 11.00000 0.06056 0.09703 = 0.03303 -0.01883 0.00501 -0.00051 H3 2 10.318901 10.441110 10.944679 11.00000 10.08000 C4 1 0.283930 0.429977 0.788672 11.00000 0.03792 0.07889 = 0.04323 -0.01377 0.00791 0.00051 H4 2 10.232659 10.430519 10.802390 11.00000 10.06700 C5 1 0.309854 0.422161 0.681420 11.00000 0.03304 0.04644 = 0.03474 -0.00802 0.00158 -0.00250 C6 1 0.260689 0.415368 0.585186 11.00000 0.04239 0.03880 = 0.03506 -0.00575 0.00250 -0.00312 C7 1 0.177605 0.418387 0.596808 11.00000 0.03754 0.05545 = 0.03177 -0.00845 0.00046 -0.00174 C8 1 0.137850 0.359587 0.645589 11.00000 0.04553 0.06010 = 0.06261 -0.00140 0.00754 -0.00445 H8 2 10.164310 10.317990 10.671490 11.00000 10.07100 C9 1 0.060737 0.363391 0.655428 11.00000 0.04975 0.10295 = 0.06527 -0.01011 0.00850 -0.02895 H9 2 10.034240 10.324970 10.688931 11.00000 10.09200 C10 1 0.023382 0.424509 0.615905 11.00000 0.03753 0.12125 = 0.06214 -0.01315 -0.00580 0.00813 H10 2 9.971280 10.427520 10.620821 11.00000 10.09200 C11 1 0.061057 0.483692 0.570020 11.00000 0.05428 0.10226 = 0.06355 0.00780 -0.00498 0.01803 H11 2 10.034439 10.524290 10.544330 11.00000 10.09000 C12 1 0.138660 0.480181 0.559342 11.00000 0.05090 0.07199 = 0.05140 0.00258 0.00461 0.00866 H12 2 10.165030 10.520310 10.526080 11.00000 10.07300 C13 1 0.255990 0.398135 0.391903 11.00000 0.03308 0.04010 = 0.03340 -0.00217 0.00035 -0.00026 C14 1 0.226259 0.328765 0.365610 11.00000 0.05286 0.04224 = 0.04055 0.00159 -0.00905 -0.00242 H14 2 10.228540 10.290280 10.416160 11.00000 10.05900 C15 1 0.194537 0.316766 0.263041 11.00000 0.05556 0.05400 = 0.05164 -0.00579 -0.01392 -0.01053 H15 2 10.175990 10.269720 10.242970 11.00000 10.06800 C16 1 0.191984 0.375487 0.190638 11.00000 0.05113 0.07766 = 0.03431 0.00484 -0.01050 -0.00809 C17 1 0.219171 0.445536 0.216824 11.00000 0.06507 0.06421 = 0.05171 0.02453 -0.01555 -0.01186 H17 2 10.215940 10.484369 10.165381 11.00000 10.07500 C18 1 0.251945 0.456574 0.317719 11.00000 0.05958 0.04671 = 0.04688 0.00137 -0.01129 -0.01229 H18 2 10.273629 10.503440 10.335400 11.00000 10.06700 C19 1 0.580135 0.401429 0.540830 11.00000 0.05058 0.03226 = 0.04832 -0.00417 0.00401 -0.00314 HKLF 4 REM 327BRRT_0ma in P41212 #92 REM R1 = 0.0450 for 3239 Fo > 4sig(Fo) and 0.0596 for all 3939 data REM 223 parameters refined using 0 restraints END WGHT 0.0263 3.1670 REM Highest difference peak 0.362, deepest hole -0.371, 1-sigma level 0.049 Q1 1 0.1612 0.3019 0.0610 11.00000 0.05 0.36 Q2 1 0.1340 0.3859 0.0829 11.00000 0.05 0.31 Q3 1 0.4442 0.4379 0.5443 11.00000 0.05 0.28 Q4 1 0.1419 0.3621 0.0232 11.00000 0.05 0.27 Q5 1 0.3590 0.4377 0.5425 11.00000 0.05 0.27 ; _shelx_res_checksum 93174 _shelx_fab_file ; -22 -2 -1 -0.0044 0.4059 -22 -1 -1 0.1451 0.2767 -21 -7 -1 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0.7299 0.4924 -20 -4 -6 -0.0588 -0.2995 -20 -4 -5 -0.2422 0.7582 -20 -4 -4 0.0608 -0.4236 -20 -4 -3 0.3220 -0.0179 -20 -4 -2 0.2694 0.1764 -20 -4 -1 -0.3590 0.0091 -20 -3 -6 -0.2851 0.0555 -20 -3 -5 -0.2252 -0.5094 -20 -3 -4 0.3118 -0.5239 -20 -3 -3 0.2222 0.3910 -20 -3 -2 0.0401 0.0720 -20 -3 -1 0.1766 -0.1746 -20 -2 -6 -0.2477 -0.1906 -20 -2 -5 -0.0534 -0.1616 -20 -2 -4 -0.0224 0.4808 -20 -2 -3 -0.1317 -0.2273 -20 -2 -2 -0.0681 -0.1477 -20 -2 -1 -0.1198 0.0148 -20 -1 -6 -0.0990 0.2718 -20 -1 -5 -0.0598 0.5254 -20 -1 -4 -0.5546 -0.3167 -20 -1 -3 0.2232 -0.0082 -20 -1 -2 0.0179 0.3374 -20 -1 -1 0.3608 0.0913 -19 -11 -2 0.2484 0.5758 -19 -11 -1 -0.1759 1.1846 -19 -10 -3 1.0328 0.5300 -19 -10 -2 0.2169 1.0399 -19 -10 -1 0.5920 -0.1383 -19 -9 -4 0.9771 0.1715 -19 -9 -3 0.9717 0.9061 -19 -9 -2 -0.1244 -0.5482 -19 -9 -1 -0.4767 -0.7138 -19 -8 -5 1.0608 -0.7319 -19 -8 -4 0.8980 -0.1526 -19 -8 -3 -0.8417 -0.1514 -19 -8 -2 -0.2672 -0.5008 -19 -8 -1 -0.0136 -0.3949 -19 -7 -6 -0.2339 -0.5529 -19 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-1 -6 0.2622 0.4757 -19 -1 -5 0.0074 0.1410 -19 -1 -4 0.1448 -0.0611 -19 -1 -3 0.0792 0.1732 -19 -1 -2 -0.3706 -0.8643 -19 -1 -1 -0.0553 0.2376 -18 -12 -3 0.3105 0.9692 -18 -12 -2 -0.0148 2.0010 -18 -12 -1 0.4108 1.3437 -18 -11 -4 -0.3218 1.1434 -18 -11 -3 1.0009 0.7843 -18 -11 -2 0.6690 -0.5123 -18 -11 -1 0.1588 -0.4639 -18 -10 -5 1.0958 0.5188 -18 -10 -4 0.1325 -0.6231 -18 -10 -3 0.3771 -0.1233 -18 -10 -2 -0.1003 -0.6230 -18 -10 -1 0.4820 -0.1774 -18 -9 -6 0.6031 -0.4717 -18 -9 -5 0.3314 -0.1834 -18 -9 -4 -0.0373 -0.7722 -18 -9 -3 0.1591 0.4318 -18 -9 -2 1.3224 -0.1887 -18 -9 -1 0.6161 -0.8432 -18 -8 -7 0.3606 -0.3891 -18 -8 -6 -0.3599 -0.3519 -18 -8 -5 -0.4673 -0.4655 -18 -8 -4 1.0207 -0.4243 -18 -8 -3 0.6074 -0.7110 -18 -8 -2 -0.1011 -0.1089 -18 -8 -1 -1.5196 -0.8552 -18 -7 -7 0.0087 0.4243 -18 -7 -6 -1.1769 -0.1523 -18 -7 -5 0.1464 -0.2909 -18 -7 -4 -0.5181 -0.8467 -18 -7 -3 -0.7781 -0.5700 -18 -7 -2 -1.4693 0.0320 -18 -7 -1 0.2755 0.0859 -18 -6 -7 -0.5815 0.6032 -18 -6 -6 -0.2908 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0.1089 18 8 3 0.6074 0.7110 18 8 4 1.0207 0.4243 18 8 5 -0.4673 0.4655 18 8 6 -0.3599 0.3519 18 8 7 0.3606 0.3891 18 9 0 -0.9180 0.0232 18 9 1 0.6161 0.8432 18 9 2 1.3224 0.1887 18 9 3 0.1591 -0.4318 18 9 4 -0.0373 0.7722 18 9 5 0.3314 0.1834 18 9 6 0.6031 0.4717 18 10 0 1.6074 0.0333 18 10 1 0.4820 0.1774 18 10 2 -0.1003 0.6230 18 10 3 0.3771 0.1233 18 10 4 0.1325 0.6231 18 10 5 1.0958 -0.5188 18 11 0 1.0780 -0.0067 18 11 1 0.1588 0.4639 18 11 2 0.6690 0.5123 18 11 3 1.0009 -0.7843 18 11 4 -0.3218 -1.1434 18 12 0 1.2468 -0.0288 18 12 1 0.4108 -1.3437 18 12 2 -0.0148 -2.0010 18 12 3 0.3105 -0.9692 18 13 0 -1.1445 0.0489 19 0 1 0.3867 -0.5888 19 0 2 0.1400 -0.0082 19 0 3 -0.2486 -0.1802 19 0 4 0.0176 0.1012 19 0 5 0.1549 -0.0518 19 0 6 0.5794 -0.0090 19 0 7 0.6435 0.6674 19 1 0 0.0621 0.0386 19 1 1 -0.0553 -0.2376 19 1 2 -0.3706 0.8643 19 1 3 0.0792 -0.1732 19 1 4 0.1448 0.0611 19 1 5 0.0074 -0.1410 19 1 6 0.2622 -0.4757 19 1 7 -0.2893 -0.4244 19 2 0 -0.4344 0.1616 19 2 1 0.5427 0.0420 19 2 2 -0.1521 -0.4157 19 2 3 0.6028 -0.1594 19 2 4 -0.3661 0.3887 19 2 5 -0.2696 -0.2033 19 2 6 -0.1462 -0.3814 19 2 7 -0.5279 0.0071 19 3 0 0.1380 -0.0268 19 3 1 -0.1055 -0.3945 19 3 2 0.0491 -0.1685 19 3 3 -0.1032 1.1039 19 3 4 -0.1953 -0.1957 19 3 5 -0.1333 -0.1741 19 3 6 -0.0106 0.1347 19 3 7 0.1148 -0.3247 19 4 0 -0.9974 -0.0004 19 4 1 0.2715 -0.0331 19 4 2 0.4653 0.5220 19 4 3 -0.2880 -0.3308 19 4 4 0.6941 -0.3565 19 4 5 -0.2789 0.2040 19 4 6 0.2608 -0.0692 19 4 7 -0.2333 -0.3288 19 5 0 0.6489 0.0179 19 5 1 0.6858 -0.0130 19 5 2 -0.4402 0.0978 19 5 3 0.1747 -0.8567 19 5 4 -0.0398 1.1000 19 5 5 -0.3268 -0.6105 19 5 6 -0.6033 -0.1468 19 5 7 -0.2894 -0.3687 19 6 0 -0.6524 -0.0467 19 6 1 -0.7629 0.0541 19 6 2 -0.4388 -0.6888 19 6 3 0.8861 0.1339 19 6 4 -0.5844 0.3365 19 6 5 -0.2247 -0.4844 19 6 6 -0.7477 0.5592 19 7 0 -1.1979 -0.0407 19 7 1 0.4431 -0.0524 19 7 2 0.6006 -0.4642 19 7 3 0.1973 0.6912 19 7 4 -0.8972 -0.1045 19 7 5 0.4285 1.1774 19 7 6 -0.2339 0.5529 19 8 0 0.7284 -0.0281 19 8 1 -0.0136 0.3949 19 8 2 -0.2672 0.5008 19 8 3 -0.8417 0.1514 19 8 4 0.8980 0.1526 19 8 5 1.0608 0.7319 19 9 0 0.0681 0.0171 19 9 1 -0.4767 0.7138 19 9 2 -0.1244 0.5482 19 9 3 0.9717 -0.9061 19 9 4 0.9771 -0.1715 19 10 0 0.6668 -0.0084 19 10 1 0.5920 0.1383 19 10 2 0.2169 -1.0399 19 10 3 1.0328 -0.5300 19 11 0 0.9236 0.0192 19 11 1 -0.1759 -1.1846 19 11 2 0.2484 -0.5758 20 0 0 -0.6679 0.1689 20 0 1 0.1896 0.3379 20 0 2 0.0539 0.2636 20 0 3 0.4097 -0.5269 20 0 4 0.3089 -0.0586 20 0 5 -0.2170 -0.2479 20 0 6 0.0682 -0.7891 20 1 0 0.3098 0.0928 20 1 1 0.3608 -0.0913 20 1 2 0.0179 -0.3374 20 1 3 0.2232 0.0082 20 1 4 -0.5546 0.3167 20 1 5 -0.0598 -0.5254 20 1 6 -0.0990 -0.2718 20 2 0 -0.2567 -0.0551 20 2 1 -0.1198 -0.0148 20 2 2 -0.0681 0.1477 20 2 3 -0.1317 0.2273 20 2 4 -0.0224 -0.4808 20 2 5 -0.0534 0.1616 20 2 6 -0.2477 0.1906 20 3 0 0.0234 0.0185 20 3 1 0.1766 0.1746 20 3 2 0.0401 -0.0720 20 3 3 0.2222 -0.3910 20 3 4 0.3118 0.5239 20 3 5 -0.2252 0.5094 20 3 6 -0.2851 -0.0555 20 4 0 -0.0623 -0.0030 20 4 1 -0.3590 -0.0091 20 4 2 0.2694 -0.1764 20 4 3 0.3220 0.0179 20 4 4 0.0608 0.4236 20 4 5 -0.2422 -0.7582 20 4 6 -0.0588 0.2995 20 5 0 -0.5790 0.0017 20 5 1 0.7299 -0.4924 20 5 2 0.1449 -0.0923 20 5 3 0.4488 -0.3529 20 5 4 -0.6945 -0.3532 20 5 5 0.3487 0.2797 20 6 0 0.5361 -0.0595 20 6 1 0.0648 0.1089 20 6 2 -0.9184 -0.2468 20 6 3 -0.2214 -0.0663 20 6 4 -0.2999 0.1045 20 6 5 0.7582 0.7159 20 7 0 -0.6814 -0.0655 20 7 1 -0.9973 0.6158 20 7 2 -0.3101 -0.5621 20 7 3 0.3441 0.3154 20 7 4 0.8818 -0.4338 20 8 0 -0.0603 0.0083 20 8 1 0.1178 0.1489 20 8 2 0.6359 -0.1420 20 8 3 0.1047 -0.0507 20 9 0 0.6919 0.0044 20 9 1 0.1084 -0.1607 20 9 2 -0.1623 0.3877 21 0 1 -0.1324 0.0979 21 0 2 -0.0205 0.1370 21 0 3 -0.1259 -0.1016 21 0 4 0.0007 -0.0473 21 1 0 0.1677 0.0668 21 1 1 0.2463 0.1959 21 1 2 -0.1580 0.0326 21 1 3 0.5490 -0.3712 21 1 4 -0.1786 -0.0846 21 2 0 0.4915 -0.0105 21 2 1 -0.2322 -0.0952 21 2 2 0.2790 -0.4590 21 2 3 0.0939 0.3168 21 2 4 -0.4120 0.1990 21 3 0 -0.3689 -0.0357 21 3 1 0.1160 -0.5330 21 3 2 0.1582 0.2785 21 3 3 -0.3011 0.0933 21 3 4 0.2238 -0.6520 21 4 0 0.2867 0.0255 21 4 1 0.2781 0.0200 21 4 2 -0.5175 0.3552 21 4 3 0.1911 -0.9034 21 4 4 0.1807 0.4981 21 5 0 -0.5097 -0.0494 21 5 1 -0.3218 0.2266 21 5 2 -0.4689 -0.9703 21 5 3 0.6377 0.1365 21 6 0 -0.2634 -0.0612 21 6 1 0.0861 -0.1859 21 6 2 0.1095 -0.4994 21 7 0 0.3239 -0.0259 21 7 1 -0.5162 0.3074 22 0 0 0.6221 0.0571 22 0 1 0.2398 0.1295 22 0 2 0.0137 0.1399 22 1 0 0.2393 -0.0538 22 1 1 0.1451 -0.2767 22 2 0 0.2522 -0.0217 22 2 1 -0.0044 -0.4059 22 3 0 -0.5552 0.0162 0 0 0 0.0 0.0 ; _shelx_fab_checksum 31331 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y+1/2, x+1/2, z+1/4' '-x, -y, z+1/2' 'y+1/2, -x+1/2, z+3/4' 'x+1/2, -y+1/2, -z+3/4' '-x+1/2, y+1/2, -z+1/4' '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 Br1 Br 0.14932(5) 0.35838(5) 0.04955(5) 0.1058(3) Uani 1 1 d . . . . . Fe1 Fe 0.40718(3) 0.40718(3) 0.5000 0.0355(2) Uani 1 2 d S T P . . S1 S 0.66983(9) 0.39532(10) 0.56881(17) 0.0856(6) Uani 1 1 d . . . . . N1 N 0.38401(19) 0.41993(19) 0.6576(3) 0.0369(9) Uani 1 1 d . . . . . N2 N 0.29631(18) 0.40799(19) 0.4939(3) 0.0327(7) Uani 1 1 d . . . . . N3 N 0.5169(2) 0.4063(2) 0.5230(3) 0.0455(9) Uani 1 1 d . . . . . C1 C 0.4326(2) 0.4267(3) 0.7396(4) 0.0447(11) Uani 1 1 d . . . . . H1 H 0.4838 0.4238 0.7252 0.058 Uiso 1 1 d . U . . . C2 C 0.4104(3) 0.4351(3) 0.8482(4) 0.0596(14) Uani 1 1 d . . . . . H2 H 0.4465 0.4391 0.9029 0.073 Uiso 1 1 d . U . . . C3 C 0.3352(3) 0.4366(4) 0.8727(4) 0.0635(16) Uani 1 1 d . . . . . H3 H 0.3189 0.4411 0.9447 0.080 Uiso 1 1 d . U . . . C4 C 0.2839(3) 0.4300(3) 0.7887(4) 0.0533(13) Uani 1 1 d . . . . . H4 H 0.2327 0.4305 0.8024 0.067 Uiso 1 1 d . U . . . C5 C 0.3099(2) 0.4222(3) 0.6814(3) 0.0381(11) Uani 1 1 d . . . . . C6 C 0.2607(2) 0.4154(3) 0.5852(3) 0.0388(11) Uani 1 1 d . . . . . C7 C 0.1776(2) 0.4184(3) 0.5968(3) 0.0416(11) Uani 1 1 d . . . . . C8 C 0.1379(3) 0.3596(3) 0.6456(4) 0.0561(13) Uani 1 1 d . . . . . H8 H 0.1643 0.3180 0.6715 0.071 Uiso 1 1 d . U . . . C9 C 0.0607(3) 0.3634(4) 0.6554(5) 0.0727(18) Uani 1 1 d . . . . . H9 H 0.0342 0.3250 0.6889 0.092 Uiso 1 1 d . U . . . C10 C 0.0234(3) 0.4245(5) 0.6159(5) 0.0736(19) Uani 1 1 d . . . . . H10 H -0.0287 0.4275 0.6208 0.092 Uiso 1 1 d . U . . . C11 C 0.0611(4) 0.4837(4) 0.5700(5) 0.0734(18) Uani 1 1 d . . . . . H11 H 0.0344 0.5243 0.5443 0.090 Uiso 1 1 d . U . . . C12 C 0.1387(3) 0.4802(3) 0.5593(4) 0.0581(14) Uani 1 1 d . . . . . H12 H 0.1650 0.5203 0.5261 0.073 Uiso 1 1 d . U . . . C13 C 0.2560(2) 0.3981(3) 0.3919(3) 0.0355(10) Uani 1 1 d . . . . . C14 C 0.2263(3) 0.3288(3) 0.3656(4) 0.0452(12) Uani 1 1 d . . . . . H14 H 0.2285 0.2903 0.4162 0.059 Uiso 1 1 d . U . . . C15 C 0.1945(3) 0.3168(3) 0.2630(4) 0.0537(13) Uani 1 1 d . . . . . H15 H 0.1760 0.2697 0.2430 0.068 Uiso 1 1 d . U . . . C16 C 0.1920(3) 0.3755(3) 0.1906(4) 0.0544(13) Uani 1 1 d . . . . . C17 C 0.2192(3) 0.4455(3) 0.2168(4) 0.0603(15) Uani 1 1 d . . . . . H17 H 0.2159 0.4844 0.1654 0.075 Uiso 1 1 d . U . . . C18 C 0.2519(3) 0.4566(3) 0.3177(4) 0.0511(12) Uani 1 1 d . . . . . H18 H 0.2736 0.5034 0.3354 0.067 Uiso 1 1 d . U . . . C19 C 0.5801(3) 0.4014(2) 0.5408(4) 0.0437(11) 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 Br1 0.1270(7) 0.1372(7) 0.0532(3) 0.0161(4) -0.0422(4) -0.0482(5) Fe1 0.0381(3) 0.0381(3) 0.0304(4) -0.0028(3) 0.0028(3) -0.0028(4) S1 0.0494(9) 0.0785(11) 0.1288(15) -0.0130(11) -0.0189(9) 0.0056(8) N1 0.037(2) 0.038(2) 0.0357(19) -0.0079(16) -0.0005(15) -0.0053(16) N2 0.0354(18) 0.0311(18) 0.0315(17) 0.0006(17) 0.0002(15) -0.0050(16) N3 0.043(2) 0.045(2) 0.048(2) -0.003(2) 0.0085(19) -0.002(2) C1 0.037(2) 0.058(3) 0.039(2) -0.008(2) 0.000(2) -0.001(2) C2 0.055(3) 0.083(4) 0.041(3) -0.013(2) -0.002(3) 0.001(3) C3 0.061(4) 0.097(5) 0.033(2) -0.019(3) 0.005(2) -0.001(3) C4 0.038(3) 0.079(4) 0.043(3) -0.014(3) 0.008(2) 0.001(2) C5 0.033(2) 0.046(3) 0.035(2) -0.008(2) 0.0016(19) -0.002(2) C6 0.042(3) 0.039(3) 0.035(2) -0.006(2) 0.0025(19) -0.003(2) C7 0.038(3) 0.055(3) 0.032(2) -0.008(2) 0.0005(19) -0.002(2) C8 0.046(3) 0.060(3) 0.063(3) -0.001(3) 0.008(2) -0.004(3) C9 0.050(4) 0.103(5) 0.065(4) -0.010(4) 0.009(3) -0.029(3) C10 0.038(3) 0.121(6) 0.062(4) -0.013(4) -0.006(3) 0.008(4) C11 0.054(4) 0.102(5) 0.064(4) 0.008(4) -0.005(3) 0.018(4) C12 0.051(3) 0.072(4) 0.051(3) 0.003(3) 0.005(3) 0.009(3) C13 0.033(2) 0.040(3) 0.033(2) -0.002(2) 0.0003(18) 0.000(2) C14 0.053(3) 0.042(3) 0.041(2) 0.002(2) -0.009(2) -0.002(2) C15 0.056(3) 0.054(3) 0.052(3) -0.006(3) -0.014(3) -0.011(2) C16 0.051(3) 0.078(4) 0.034(2) 0.005(3) -0.011(2) -0.008(3) C17 0.065(4) 0.064(4) 0.052(3) 0.025(3) -0.016(3) -0.012(3) C18 0.060(3) 0.047(3) 0.047(3) 0.001(2) -0.011(2) -0.012(2) C19 0.051(3) 0.032(2) 0.048(2) -0.004(2) 0.004(2) -0.003(2) 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' Br Br -0.2901 2.4595 '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 N1 Fe1 N1 172.4(2) 7_556 . ? N2 Fe1 N1 80.12(14) . . ? N2 Fe1 N1 80.12(14) 7_556 7_556 ? N2 Fe1 N1 94.52(14) 7_556 . ? N2 Fe1 N1 94.52(14) . 7_556 ? N2 Fe1 N2 90.9(2) 7_556 . ? N3 Fe1 N1 93.91(15) 7_556 7_556 ? N3 Fe1 N1 93.91(15) . . ? N3 Fe1 N1 91.36(15) . 7_556 ? N3 Fe1 N1 91.36(15) 7_556 . ? N3 Fe1 N2 88.84(15) 7_556 . ? N3 Fe1 N2 173.98(14) 7_556 7_556 ? N3 Fe1 N2 88.84(15) . 7_556 ? N3 Fe1 N2 173.98(14) . . ? N3 Fe1 N3 92.0(2) . 7_556 ? C1 N1 Fe1 127.4(3) . . ? C1 N1 C5 118.0(4) . . ? C5 N1 Fe1 114.5(3) . . ? C6 N2 Fe1 117.3(3) . . ? C6 N2 C13 120.9(3) . . ? C13 N2 Fe1 121.8(3) . . ? C19 N3 Fe1 175.2(4) . . ? N1 C1 H1 119.3(4) . . ? N1 C1 C2 122.9(4) . . ? C2 C1 H1 117.7(5) . . ? C1 C2 H2 119.8(5) . . ? C3 C2 C1 119.1(5) . . ? C3 C2 H2 121.1(5) . . ? C2 C3 H3 120.8(5) . . ? C2 C3 C4 118.8(4) . . ? C4 C3 H3 120.4(5) . . ? C3 C4 H4 121.0(5) . . ? C3 C4 C5 119.3(4) . . ? C5 C4 H4 119.7(5) . . ? N1 C5 C4 121.8(4) . . ? N1 C5 C6 114.0(4) . . ? C4 C5 C6 124.2(4) . . ? N2 C6 C5 114.1(4) . . ? N2 C6 C7 125.1(4) . . ? C5 C6 C7 120.8(4) . . ? C8 C7 C6 121.2(4) . . ? C12 C7 C6 119.8(4) . . ? C12 C7 C8 119.0(4) . . ? C7 C8 H8 118.9(5) . . ? C9 C8 C7 120.3(5) . . ? C9 C8 H8 120.8(6) . . ? C8 C9 H9 120.6(8) . . ? C10 C9 C8 119.6(6) . . ? C10 C9 H9 119.8(6) . . ? C9 C10 H10 120.6(8) . . ? C9 C10 C11 121.4(5) . . ? C11 C10 H10 118.0(8) . . ? C10 C11 H11 119.5(7) . . ? C10 C11 C12 119.4(6) . . ? C12 C11 H11 121.0(7) . . ? C7 C12 C11 120.3(5) . . ? C7 C12 H12 119.7(5) . . ? C11 C12 H12 120.0(6) . . ? C14 C13 N2 119.9(4) . . ? C14 C13 C18 120.0(4) . . ? C18 C13 N2 120.0(4) . . ? C13 C14 H14 119.4(4) . . ? C13 C14 C15 120.2(4) . . ? C15 C14 H14 120.5(5) . . ? C14 C15 H15 121.2(5) . . ? C16 C15 C14 118.6(5) . . ? C16 C15 H15 120.2(5) . . ? C15 C16 Br1 118.4(4) . . ? C15 C16 C17 122.0(4) . . ? C17 C16 Br1 119.7(4) . . ? C16 C17 H17 119.4(5) . . ? C16 C17 C18 119.1(5) . . ? C18 C17 H17 121.5(6) . . ? C13 C18 H18 119.6(5) . . ? C17 C18 C13 120.1(5) . . ? C17 C18 H18 120.2(5) . . ? N3 C19 S1 178.7(5) . . ? 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 Br1 C16 1.903(4) . ? Fe1 N1 1.977(3) 7_556 ? Fe1 N1 1.977(3) . ? Fe1 N2 1.968(3) 7_556 ? Fe1 N2 1.968(3) . ? Fe1 N3 1.966(4) 7_556 ? Fe1 N3 1.966(4) . ? S1 C19 1.631(5) . ? N1 C1 1.326(5) . ? N1 C5 1.348(5) . ? N2 C6 1.286(5) . ? N2 C13 1.444(5) . ? N3 C19 1.147(5) . ? C1 H1 0.926(4) . ? C1 C2 1.388(6) . ? C2 H2 0.927(5) . ? C2 C3 1.367(7) . ? C3 H3 0.927(5) . ? C3 C4 1.374(7) . ? C4 H4 0.925(5) . ? C4 C5 1.392(6) . ? C5 C6 1.466(6) . ? C6 C7 1.482(6) . ? C7 C8 1.392(7) . ? C7 C12 1.374(7) . ? C8 H8 0.930(5) . ? C8 C9 1.375(7) . ? C9 H9 0.923(6) . ? C9 C10 1.359(9) . ? C10 H10 0.928(6) . ? C10 C11 1.364(9) . ? C11 H11 0.916(6) . ? C11 C12 1.384(8) . ? C12 H12 0.943(6) . ? C13 C14 1.377(6) . ? C13 C18 1.377(6) . ? C14 H14 0.920(5) . ? C14 C15 1.387(6) . ? C15 H15 0.930(5) . ? C15 C16 1.366(7) . ? C16 C17 1.371(7) . ? C17 H17 0.933(5) . ? C17 C18 1.374(7) . ? C18 H18 0.941(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 Br1 C16 C17 C18 -178.0(4) . . . . ? Fe1 N1 C1 C2 -179.7(4) . . . . ? Fe1 N1 C5 C4 179.2(4) . . . . ? Fe1 N1 C5 C6 -0.5(5) . . . . ? Fe1 N2 C6 C5 0.0(5) . . . . ? Fe1 N2 C6 C7 179.0(4) . . . . ? Fe1 N2 C13 C14 99.6(4) . . . . ? Fe1 N2 C13 C18 -75.8(5) . . . . ? N1 C1 C2 C3 -0.1(8) . . . . ? N1 C5 C6 N2 0.3(6) . . . . ? N1 C5 C6 C7 -178.7(4) . . . . ? N2 C6 C7 C8 110.4(5) . . . . ? N2 C6 C7 C12 -69.8(6) . . . . ? N2 C13 C14 C15 -173.1(4) . . . . ? N2 C13 C18 C17 174.5(5) . . . . ? C1 N1 C5 C4 -1.1(7) . . . . ? C1 N1 C5 C6 179.1(4) . . . . ? C1 C2 C3 C4 -0.3(9) . . . . ? C2 C3 C4 C5 -0.1(9) . . . . ? C3 C4 C5 N1 0.8(8) . . . . ? C3 C4 C5 C6 -179.4(5) . . . . ? C4 C5 C6 N2 -179.4(5) . . . . ? C4 C5 C6 C7 1.5(7) . . . . ? C5 N1 C1 C2 0.8(7) . . . . ? C5 C6 C7 C8 -70.6(6) . . . . ? C5 C6 C7 C12 109.2(5) . . . . ? C6 N2 C13 C14 -78.2(6) . . . . ? C6 N2 C13 C18 106.4(5) . . . . ? C6 C7 C8 C9 -179.9(5) . . . . ? C6 C7 C12 C11 -179.8(5) . . . . ? C7 C8 C9 C10 0.9(9) . . . . ? C8 C7 C12 C11 0.0(8) . . . . ? C8 C9 C10 C11 -2.4(10) . . . . ? C9 C10 C11 C12 2.7(10) . . . . ? C10 C11 C12 C7 -1.4(9) . . . . ? C12 C7 C8 C9 0.3(8) . . . . ? C13 N2 C6 C5 177.9(4) . . . . ? C13 N2 C6 C7 -3.1(7) . . . . ? C13 C14 C15 C16 -1.5(8) . . . . ? C14 C13 C18 C17 -0.9(8) . . . . ? C14 C15 C16 Br1 179.4(4) . . . . ? C14 C15 C16 C17 -0.5(8) . . . . ? C15 C16 C17 C18 1.9(9) . . . . ? C16 C17 C18 C13 -1.2(9) . . . . ? C18 C13 C14 C15 2.3(7) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.954(16) 2 0.046(16) loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.149 0.149 0.500 75.9 15.3 ? 2 0.351 0.649 0.750 75.9 13.9 ? 3 0.649 0.351 0.250 75.9 14.5 ? 4 0.851 0.851 0.000 75.9 15.1 ?