#------------------------------------------------------------------------------ #$Date: 2019-10-08 03:56:35 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219141 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234441.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_7234441 loop_ _publ_author_name 'Tailleur, Elodie' 'Marchivie, Mathieu' 'Negrier, Philippe' 'Denux, Dominique' 'Massip, St\'ephane' 'Mondieig, Denise' 'Chastanet, Guillaume' 'Guionneau, Philippe' _publ_section_title ; Using polymorphism to master the spin crossover mechanism in [Fe(PM-PeA)2(NCSe)2] ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C9CE01137D _journal_year 2019 _chemical_formula_moiety 'C42 H28 Fe N6 Se2' _chemical_formula_sum 'C42 H28 Fe N6 Se2' _chemical_formula_weight 830.47 _chemical_name_systematic '[Fe(PM-PeA)2(NCSe)2]_polymorph-II' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2019-07-01 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2019-07-01 deposited with the CCDC. 2019-09-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 117.901(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.8161(3) _cell_length_b 14.6779(2) _cell_length_c 17.1039(3) _cell_measurement_reflns_used 13334 _cell_measurement_temperature 100 _cell_measurement_theta_max 72.5380 _cell_measurement_theta_min 2.9630 _cell_volume 3730.93(15) _computing_cell_refinement 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (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 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 100 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -195.00 -15.00 1.00 20.00 -- -105.00 60.00 -36.00 180 2 \w -85.00 -37.00 1.00 5.00 -- 5.00 48.00-108.00 48 3 \w -195.00 -15.00 1.00 20.00 -- -105.00 36.00 144.00 180 4 \w -131.00 49.00 1.00 10.00 -- -41.00 60.00-108.00 180 5 \w -195.00 -15.00 1.00 20.00 -- -105.00 60.00-108.00 180 6 \w -194.00 -15.00 1.00 20.00 -- -105.00 48.00 72.00 179 7 \w -105.00 48.00 1.00 10.00 -- -41.00 48.00 -72.00 153 8 \w -184.00-127.00 1.00 20.00 -- -105.00 12.00 -72.00 57 9 \w -128.00 -67.00 1.00 10.00 -- -41.00 36.00 72.00 61 10 \w -179.00-134.00 1.00 20.00 -- -105.00 60.00-144.00 45 11 \w -60.00 -15.00 1.00 20.00 -- -105.00 12.00-108.00 45 12 \w -190.00-145.00 1.00 20.00 -- -105.00 60.00 0.00 45 13 \w -158.00 -74.00 1.00 20.00 -- -105.00 60.00 -72.00 84 14 \w -195.00-115.00 1.00 20.00 -- -105.00 60.00 72.00 80 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0337407000 _diffrn_orient_matrix_UB_12 0.0990055000 _diffrn_orient_matrix_UB_13 0.0207241000 _diffrn_orient_matrix_UB_21 -0.0911526000 _diffrn_orient_matrix_UB_22 0.0340971000 _diffrn_orient_matrix_UB_23 -0.0733171000 _diffrn_orient_matrix_UB_31 -0.0360509000 _diffrn_orient_matrix_UB_32 0.0065318000 _diffrn_orient_matrix_UB_33 0.0677152000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0254 _diffrn_reflns_av_unetI/netI 0.0187 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 27081 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.199 _diffrn_reflns_theta_min 2.974 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.771 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.71631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'dark black' _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.478 _exptl_crystal_description block _exptl_crystal_F_000 1664 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.966 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.089 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 460 _refine_ls_number_reflns 7269 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0529 _refine_ls_R_factor_gt 0.0492 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0993P)^2^+2.4223P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1422 _refine_ls_wR_factor_ref 0.1452 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6541 _reflns_number_total 7269 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01137d2.cif _cod_data_source_block mmet29_amb-100kb _cod_original_cell_volume 3730.93(14) _cod_database_code 7234441 _shelx_shelxl_version_number 2016/6 _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 0.596 _shelx_estimated_absorpt_t_min 0.160 _reflns_odcompleteness_completeness 97.36 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 73.04 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26), C28(H28), C29(H29), C30(H30), C32(H32), C33(H33), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41) ; _shelx_res_file ; TITL MMET29_amb-100Kb in P21/c #14 mmet29_amb-100kb.res created by SHELXL-2016/6 at 17:00:15 on 01-Jul-2019 REM reset to P21/c #14 CELL 1.54184 16.816081 14.677896 17.103877 90 117.9007 90 ZERR 4 0.000348 0.000216 0.000307 0 0.0025 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Fe N Se UNIT 168 112 4 24 8 L.S. 4 0 0 PLAN 20 SIZE 0.5 0.1 0.1 TEMP -173.15 BOND fmap 2 53 acta OMIT 1 4 4 OMIT 0 3 3 OMIT 2 0 0 OMIT 1 6 2 OMIT -2 6 4 OMIT -4 1 8 OMIT 3 0 2 OMIT -3 5 4 OMIT 0 6 0 OMIT 3 2 3 OMIT -2 5 4 OMIT -3 0 8 OMIT -2 3 1 OMIT 4 6 0 OMIT 2 6 1 OMIT 3 3 2 OMIT 3 1 4 OMIT -1 2 2 OMIT -2 8 3 OMIT -1 7 5 OMIT -8 1 5 OMIT -4 1 5 OMIT -6 0 4 OMIT -8 2 3 OMIT 1 2 4 OMIT -3 5 2 OMIT 0 8 0 OMIT 5 5 0 OMIT 3 5 1 OMIT -2 2 9 OMIT 3 6 0 OMIT 5 0 4 OMIT 0 2 8 OMIT -4 4 3 REM REM REM WGHT 0.099300 2.422300 FVAR 2.99268 SE1 5 0.472401 0.337066 0.075957 11.00000 0.06790 0.09358 = 0.05386 -0.02698 0.03550 -0.03282 SE2 5 0.001676 0.215185 -0.136948 11.00000 0.05508 0.04967 = 0.03947 -0.00154 0.01951 -0.00301 FE1 3 0.241234 0.264394 0.163674 11.00000 0.04347 0.04857 = 0.03101 -0.00049 0.01789 -0.00041 N1 4 0.328510 0.302679 0.125539 11.00000 0.05515 0.05600 = 0.03745 -0.00446 0.02276 -0.00419 N2 4 0.290088 0.140143 0.185304 11.00000 0.04803 0.05507 = 0.03766 0.00059 0.02272 0.00242 N3 4 0.330000 0.275816 0.290594 11.00000 0.04418 0.05772 = 0.03509 -0.00241 0.01977 -0.00216 N4 4 0.152224 0.238076 0.043106 11.00000 0.05477 0.04748 = 0.04196 0.00191 0.02410 0.00095 N5 4 0.185760 0.386007 0.148070 11.00000 0.04900 0.05150 = 0.03213 -0.00265 0.01762 -0.00252 N6 4 0.153908 0.238755 0.207813 11.00000 0.04341 0.05441 = 0.03317 0.00067 0.01661 -0.00151 C1 1 0.383810 0.317051 0.105411 11.00000 0.05660 0.05252 = 0.03464 -0.01013 0.02164 -0.01113 C2 1 0.271462 0.072766 0.126082 11.00000 0.06066 0.05715 = 0.04292 -0.00216 0.02519 0.00439 AFIX 43 H2 2 0.236449 0.086121 0.064939 11.00000 -1.20000 AFIX 0 C3 1 0.301435 -0.014891 0.151105 11.00000 0.07108 0.06150 = 0.05548 -0.00433 0.03015 0.00942 AFIX 43 H3 2 0.288230 -0.060579 0.107398 11.00000 -1.20000 AFIX 0 C4 1 0.350398 -0.036527 0.239107 11.00000 0.06620 0.05952 = 0.06565 0.00754 0.03083 0.01571 AFIX 43 H4 2 0.368174 -0.097606 0.257235 11.00000 -1.20000 AFIX 0 C5 1 0.373132 0.032389 0.300468 11.00000 0.05444 0.06836 = 0.04694 0.00782 0.02126 0.01389 AFIX 43 H5 2 0.409159 0.020079 0.361692 11.00000 -1.20000 AFIX 0 C6 1 0.342749 0.119932 0.271701 11.00000 0.04392 0.06070 = 0.03887 0.00143 0.01983 0.00495 C7 1 0.364344 0.199518 0.328467 11.00000 0.04402 0.06670 = 0.03677 0.00137 0.01824 0.00088 AFIX 43 H7 2 0.401991 0.195468 0.390542 11.00000 -1.20000 AFIX 0 C8 1 0.364847 0.436607 0.312789 11.00000 0.06135 0.06707 = 0.03950 -0.00628 0.02539 -0.01633 AFIX 43 H8 2 0.365357 0.437939 0.257495 11.00000 -1.20000 AFIX 0 C9 1 0.380963 0.515342 0.361825 11.00000 0.06665 0.07060 = 0.04621 -0.00643 0.02791 -0.01896 AFIX 43 H9 2 0.392782 0.570577 0.340194 11.00000 -1.20000 AFIX 0 C10 1 0.380051 0.514569 0.443651 11.00000 0.05217 0.06706 = 0.04233 -0.00923 0.02129 -0.00780 C11 1 0.365051 0.432344 0.474294 11.00000 0.06092 0.06976 = 0.04036 -0.00226 0.02609 0.00085 AFIX 43 H11 2 0.366570 0.430197 0.530490 11.00000 -1.20000 AFIX 0 C12 1 0.347909 0.353273 0.424981 11.00000 0.06046 0.06180 = 0.03804 0.00317 0.02579 0.00478 AFIX 43 H12 2 0.336232 0.297868 0.446468 11.00000 -1.20000 AFIX 0 C13 1 0.347911 0.355555 0.343765 11.00000 0.04479 0.05980 = 0.03501 -0.00128 0.01852 -0.00194 C14 1 0.392504 0.596695 0.492373 11.00000 0.05590 0.07111 = 0.05068 -0.00511 0.02702 -0.00723 C15 1 0.399376 0.666050 0.532155 11.00000 0.05332 0.07121 = 0.05274 -0.01154 0.02562 -0.01061 C16 1 0.378732 0.831182 0.528996 11.00000 0.04862 0.07894 = 0.06897 -0.00902 0.02348 -0.00089 AFIX 43 H16 2 0.354789 0.830231 0.466487 11.00000 -1.20000 AFIX 0 C17 1 0.386598 0.912342 0.572006 11.00000 0.06023 0.07249 = 0.09692 -0.00895 0.03168 0.00892 AFIX 43 H17 2 0.368101 0.967568 0.539399 11.00000 -1.20000 AFIX 0 C18 1 0.421931 0.913259 0.663927 11.00000 0.06233 0.08549 = 0.10242 -0.03920 0.03897 0.00066 AFIX 43 H18 2 0.427242 0.969545 0.693400 11.00000 -1.20000 AFIX 0 C19 1 0.449037 0.834636 0.712325 11.00000 0.06529 0.08802 = 0.07215 -0.02697 0.03549 -0.00434 AFIX 43 H19 2 0.473306 0.836301 0.774855 11.00000 -1.20000 AFIX 0 C20 1 0.440608 0.751590 0.668640 11.00000 0.06062 0.07513 = 0.06617 -0.01798 0.03605 -0.00936 AFIX 43 H20 2 0.458535 0.696429 0.701413 11.00000 -1.20000 AFIX 0 C21 1 0.405840 0.750202 0.576957 11.00000 0.04519 0.06989 = 0.06319 -0.01451 0.02611 -0.00829 C22 1 0.093049 0.228869 -0.028065 11.00000 0.05519 0.03918 = 0.03682 0.00177 0.02378 -0.00004 C23 1 0.202112 0.459582 0.110784 11.00000 0.06550 0.05415 = 0.03840 -0.00039 0.02255 -0.00262 AFIX 43 H23 2 0.247153 0.455745 0.092231 11.00000 -1.20000 AFIX 0 C24 1 0.155976 0.540028 0.098606 11.00000 0.08654 0.05272 = 0.05404 0.00391 0.03079 0.00148 AFIX 43 H24 2 0.169231 0.590823 0.072267 11.00000 -1.20000 AFIX 0 C25 1 0.089622 0.546323 0.125260 11.00000 0.08221 0.05375 = 0.07159 -0.00200 0.02991 0.01208 AFIX 43 H25 2 0.056983 0.601334 0.117466 11.00000 -1.20000 AFIX 0 C26 1 0.072185 0.471285 0.163144 11.00000 0.06547 0.06582 = 0.06030 -0.00234 0.03049 0.01134 AFIX 43 H26 2 0.027390 0.473661 0.182107 11.00000 -1.20000 AFIX 0 C27 1 0.121343 0.391892 0.173169 11.00000 0.05180 0.05701 = 0.03807 -0.00274 0.01771 0.00236 C28 1 0.107193 0.307374 0.209620 11.00000 0.04514 0.06452 = 0.04153 -0.00121 0.02157 0.00189 AFIX 43 H28 2 0.066157 0.303211 0.233179 11.00000 -1.20000 AFIX 0 C29 1 0.125240 0.075993 0.194163 11.00000 0.05309 0.06555 = 0.03761 0.00153 0.02060 -0.01000 AFIX 43 H29 2 0.110181 0.080329 0.133383 11.00000 -1.20000 AFIX 0 C30 1 0.124812 -0.007729 0.230405 11.00000 0.05740 0.06267 = 0.04443 0.00099 0.02013 -0.00977 AFIX 43 H30 2 0.109832 -0.060902 0.194645 11.00000 -1.20000 AFIX 0 C31 1 0.146523 -0.014681 0.320321 11.00000 0.04627 0.06551 = 0.04682 0.01088 0.02131 0.00104 C32 1 0.168329 0.063646 0.371095 11.00000 0.05879 0.06867 = 0.04442 0.01231 0.02820 0.00794 AFIX 43 H32 2 0.183182 0.059591 0.431839 11.00000 -1.20000 AFIX 0 C33 1 0.168888 0.148388 0.334695 11.00000 0.05672 0.06116 = 0.04127 0.00249 0.02674 0.00656 AFIX 43 H33 2 0.183707 0.201740 0.370199 11.00000 -1.20000 AFIX 0 C34 1 0.147572 0.154102 0.246010 11.00000 0.04139 0.06242 = 0.03847 0.00555 0.01944 0.00040 C35 1 0.143642 -0.103998 0.354907 11.00000 0.05035 0.06681 = 0.04724 0.00783 0.02140 0.00179 C36 1 0.138513 -0.179229 0.378869 11.00000 0.04781 0.06641 = 0.04490 0.00824 0.01829 0.00323 C37 1 0.152198 -0.343285 0.362521 11.00000 0.06704 0.07378 = 0.05261 0.00567 0.02613 0.01504 AFIX 43 H37 2 0.175701 -0.331215 0.322731 11.00000 -1.20000 AFIX 0 C38 1 0.139985 -0.432864 0.381997 11.00000 0.07485 0.06964 = 0.05745 -0.00508 0.01932 0.02095 AFIX 43 H38 2 0.154833 -0.481975 0.355030 11.00000 -1.20000 AFIX 0 C39 1 0.106278 -0.450545 0.440529 11.00000 0.06805 0.04991 = 0.05440 0.00072 0.01319 0.00345 AFIX 43 H39 2 0.096813 -0.511670 0.452479 11.00000 -1.20000 AFIX 0 C40 1 0.086544 -0.380031 0.481257 11.00000 0.06792 0.05836 = 0.05216 0.00097 0.02478 -0.00407 AFIX 43 H40 2 0.065021 -0.392570 0.522536 11.00000 -1.20000 AFIX 0 C41 1 0.097915 -0.290310 0.462362 11.00000 0.05839 0.04799 = 0.04521 -0.00300 0.02328 -0.00282 AFIX 43 H41 2 0.084052 -0.241761 0.490685 11.00000 -1.20000 AFIX 0 C42 1 0.129581 -0.271422 0.402011 11.00000 0.04655 0.05963 = 0.04123 0.00287 0.01243 0.00533 HKLF 4 REM MMET29_amb-100Kb in P21/c #14 REM R1 = 0.0492 for 6541 Fo > 4sig(Fo) and 0.0529 for all 7269 data REM 460 parameters refined using 0 restraints END WGHT 0.0991 2.4113 REM Highest difference peak 0.966, deepest hole -0.957, 1-sigma level 0.089 Q1 1 0.4206 0.3833 0.0538 11.00000 0.05 0.97 Q2 1 0.4775 0.2771 0.1022 11.00000 0.05 0.54 Q3 1 0.5420 0.2844 0.0944 11.00000 0.05 0.52 Q4 1 -0.0687 0.2326 -0.1568 11.00000 0.05 0.42 Q5 1 0.2167 0.3652 0.1617 11.00000 0.05 0.38 Q6 1 0.1238 0.1999 -0.0185 11.00000 0.05 0.38 Q7 1 0.1550 -0.3007 0.3962 11.00000 0.05 0.38 Q8 1 0.5574 0.3183 0.1154 11.00000 0.05 0.37 Q9 1 0.3386 0.3382 0.0871 11.00000 0.05 0.36 Q10 1 0.0619 0.1795 -0.1174 11.00000 0.05 0.36 Q11 1 0.1191 0.3593 0.1948 11.00000 0.05 0.36 Q12 1 0.3600 0.1549 0.3007 11.00000 0.05 0.36 Q13 1 0.1186 0.2539 0.1879 11.00000 0.05 0.33 Q14 1 0.4788 0.3860 0.0169 11.00000 0.05 0.33 Q15 1 0.3839 0.7753 0.5536 11.00000 0.05 0.33 Q16 1 -0.1359 0.2250 -0.1492 11.00000 0.05 0.33 Q17 1 0.0797 0.2166 -0.1036 11.00000 0.05 0.32 Q18 1 0.1459 -0.3800 0.3721 11.00000 0.05 0.31 Q19 1 0.1332 0.5378 0.1276 11.00000 0.05 0.31 Q20 1 0.3804 -0.0055 0.2588 11.00000 0.05 0.29 ; _shelx_res_checksum 17105 _olex2_submission_original_sample_id MMET40B _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.634 _oxdiff_exptl_absorpt_empirical_full_min 0.610 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' 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 Se1 Se 0.47240(3) 0.33707(4) 0.07596(3) 0.06898(17) Uani 1 1 d . Se2 Se 0.00168(3) 0.21519(3) -0.13695(2) 0.04912(13) Uani 1 1 d . Fe1 Fe 0.24123(3) 0.26439(4) 0.16367(3) 0.04083(14) Uani 1 1 d . N1 N 0.3285(2) 0.3027(2) 0.12554(18) 0.0491(6) Uani 1 1 d . N2 N 0.29009(19) 0.1401(2) 0.18530(18) 0.0459(6) Uani 1 1 d . N3 N 0.33000(19) 0.2758(2) 0.29059(18) 0.0452(6) Uani 1 1 d . N4 N 0.1522(2) 0.23808(19) 0.04311(19) 0.0475(6) Uani 1 1 d . N5 N 0.18576(19) 0.38601(19) 0.14807(17) 0.0448(6) Uani 1 1 d . N6 N 0.15391(18) 0.2388(2) 0.20781(17) 0.0442(6) Uani 1 1 d . C1 C 0.3838(2) 0.3171(2) 0.1054(2) 0.0478(7) Uani 1 1 d . C2 C 0.2715(3) 0.0728(3) 0.1261(2) 0.0532(8) Uani 1 1 d . H2 H 0.236449 0.086121 0.064939 0.064 Uiso 1 1 calc R C3 C 0.3014(3) -0.0149(3) 0.1511(3) 0.0625(10) Uani 1 1 d . H3 H 0.288230 -0.060579 0.107398 0.075 Uiso 1 1 calc R C4 C 0.3504(3) -0.0365(3) 0.2391(3) 0.0638(10) Uani 1 1 d . H4 H 0.368174 -0.097606 0.257235 0.077 Uiso 1 1 calc R C5 C 0.3731(3) 0.0324(3) 0.3005(3) 0.0576(9) Uani 1 1 d . H5 H 0.409159 0.020079 0.361692 0.069 Uiso 1 1 calc R C6 C 0.3427(2) 0.1199(3) 0.2717(2) 0.0476(7) Uani 1 1 d . C7 C 0.3643(2) 0.1995(3) 0.3285(2) 0.0494(8) Uani 1 1 d . H7 H 0.401991 0.195468 0.390542 0.059 Uiso 1 1 calc R C8 C 0.3648(3) 0.4366(3) 0.3128(2) 0.0553(9) Uani 1 1 d . H8 H 0.365357 0.437939 0.257495 0.066 Uiso 1 1 calc R C9 C 0.3810(3) 0.5153(3) 0.3618(2) 0.0606(9) Uani 1 1 d . H9 H 0.392782 0.570577 0.340194 0.073 Uiso 1 1 calc R C10 C 0.3801(2) 0.5146(3) 0.4437(2) 0.0542(8) Uani 1 1 d . C11 C 0.3651(3) 0.4323(3) 0.4743(2) 0.0561(8) Uani 1 1 d . H11 H 0.366570 0.430197 0.530490 0.067 Uiso 1 1 calc R C12 C 0.3479(3) 0.3533(3) 0.4250(2) 0.0523(8) Uani 1 1 d . H12 H 0.336232 0.297868 0.446468 0.063 Uiso 1 1 calc R C13 C 0.3479(2) 0.3556(2) 0.3438(2) 0.0466(7) Uani 1 1 d . C14 C 0.3925(3) 0.5967(3) 0.4924(3) 0.0584(9) Uani 1 1 d . C15 C 0.3994(3) 0.6661(3) 0.5322(3) 0.0588(9) Uani 1 1 d . C16 C 0.3787(3) 0.8312(3) 0.5290(3) 0.0671(11) Uani 1 1 d . H16 H 0.354789 0.830231 0.466487 0.081 Uiso 1 1 calc R C17 C 0.3866(3) 0.9123(4) 0.5720(4) 0.0786(13) Uani 1 1 d . H17 H 0.368101 0.967568 0.539399 0.094 Uiso 1 1 calc R C18 C 0.4219(3) 0.9133(4) 0.6639(4) 0.0832(15) Uani 1 1 d . H18 H 0.427242 0.969545 0.693400 0.100 Uiso 1 1 calc R C19 C 0.4490(3) 0.8346(4) 0.7123(3) 0.0738(12) Uani 1 1 d . H19 H 0.473306 0.836301 0.774855 0.089 Uiso 1 1 calc R C20 C 0.4406(3) 0.7516(3) 0.6686(3) 0.0648(10) Uani 1 1 d . H20 H 0.458535 0.696429 0.701413 0.078 Uiso 1 1 calc R C21 C 0.4058(3) 0.7502(3) 0.5770(3) 0.0591(9) Uani 1 1 d . C22 C 0.0930(2) 0.2289(2) -0.0281(2) 0.0428(7) Uani 1 1 d . C23 C 0.2021(3) 0.4596(3) 0.1108(2) 0.0534(8) Uani 1 1 d . H23 H 0.247153 0.455745 0.092231 0.064 Uiso 1 1 calc R C24 C 0.1560(3) 0.5400(3) 0.0986(3) 0.0653(10) Uani 1 1 d . H24 H 0.169231 0.590823 0.072267 0.078 Uiso 1 1 calc R C25 C 0.0896(3) 0.5463(3) 0.1253(3) 0.0716(11) Uani 1 1 d . H25 H 0.056983 0.601334 0.117466 0.086 Uiso 1 1 calc R C26 C 0.0722(3) 0.4713(3) 0.1631(3) 0.0634(10) Uani 1 1 d . H26 H 0.027390 0.473661 0.182107 0.076 Uiso 1 1 calc R C27 C 0.1213(2) 0.3919(3) 0.1732(2) 0.0503(8) Uani 1 1 d . C28 C 0.1072(2) 0.3074(3) 0.2096(2) 0.0499(7) Uani 1 1 d . H28 H 0.066157 0.303211 0.233179 0.060 Uiso 1 1 calc R C29 C 0.1252(2) 0.0760(3) 0.1942(2) 0.0523(8) Uani 1 1 d . H29 H 0.110181 0.080329 0.133383 0.063 Uiso 1 1 calc R C30 C 0.1248(3) -0.0077(3) 0.2304(2) 0.0563(8) Uani 1 1 d . H30 H 0.109832 -0.060902 0.194645 0.068 Uiso 1 1 calc R C31 C 0.1465(2) -0.0147(3) 0.3203(2) 0.0531(8) Uani 1 1 d . C32 C 0.1683(3) 0.0636(3) 0.3711(2) 0.0557(8) Uani 1 1 d . H32 H 0.183182 0.059591 0.431839 0.067 Uiso 1 1 calc R C33 C 0.1689(2) 0.1484(3) 0.3347(2) 0.0515(8) Uani 1 1 d . H33 H 0.183707 0.201740 0.370199 0.062 Uiso 1 1 calc R C34 C 0.1476(2) 0.1541(3) 0.2460(2) 0.0471(7) Uani 1 1 d . C35 C 0.1436(2) -0.1040(3) 0.3549(2) 0.0554(8) Uani 1 1 d . C36 C 0.1385(2) -0.1792(3) 0.3789(2) 0.0544(8) Uani 1 1 d . C37 C 0.1522(3) -0.3433(3) 0.3625(3) 0.0652(10) Uani 1 1 d . H37 H 0.175701 -0.331215 0.322731 0.078 Uiso 1 1 calc R C38 C 0.1400(3) -0.4329(3) 0.3820(3) 0.0720(12) Uani 1 1 d . H38 H 0.154833 -0.481975 0.355030 0.086 Uiso 1 1 calc R C39 C 0.1063(3) -0.4505(3) 0.4405(3) 0.0636(10) Uani 1 1 d . H39 H 0.096813 -0.511670 0.452479 0.076 Uiso 1 1 calc R C40 C 0.0865(3) -0.3800(3) 0.4813(3) 0.0608(9) Uani 1 1 d . H40 H 0.065021 -0.392570 0.522536 0.073 Uiso 1 1 calc R C41 C 0.0979(3) -0.2903(2) 0.4624(2) 0.0509(8) Uani 1 1 d . H41 H 0.084052 -0.241761 0.490685 0.061 Uiso 1 1 calc R C42 C 0.1296(2) -0.2714(3) 0.4020(2) 0.0524(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 Se1 0.0679(3) 0.0936(4) 0.0539(2) -0.0270(2) 0.0355(2) -0.0328(2) Se2 0.0551(2) 0.0497(2) 0.0395(2) -0.00154(14) 0.01951(16) -0.00301(15) Fe1 0.0435(3) 0.0486(3) 0.0310(2) -0.00049(19) 0.0179(2) -0.0004(2) N1 0.0552(16) 0.0560(16) 0.0375(13) -0.0045(12) 0.0228(13) -0.0042(13) N2 0.0480(14) 0.0551(15) 0.0377(13) 0.0006(11) 0.0227(12) 0.0024(12) N3 0.0442(14) 0.0577(16) 0.0351(13) -0.0024(11) 0.0198(11) -0.0022(12) N4 0.0548(16) 0.0475(15) 0.0420(15) 0.0019(11) 0.0241(14) 0.0010(12) N5 0.0490(14) 0.0515(15) 0.0321(12) -0.0027(11) 0.0176(11) -0.0025(11) N6 0.0434(14) 0.0544(16) 0.0332(12) 0.0007(11) 0.0166(11) -0.0015(11) C1 0.0566(19) 0.0525(18) 0.0346(15) -0.0101(13) 0.0216(14) -0.0111(15) C2 0.061(2) 0.057(2) 0.0429(17) -0.0022(15) 0.0252(16) 0.0044(16) C3 0.071(2) 0.061(2) 0.055(2) -0.0043(17) 0.0302(19) 0.0094(19) C4 0.066(2) 0.060(2) 0.066(2) 0.0075(18) 0.031(2) 0.0157(18) C5 0.054(2) 0.068(2) 0.0469(18) 0.0078(17) 0.0213(16) 0.0139(17) C6 0.0439(16) 0.061(2) 0.0389(15) 0.0014(14) 0.0198(13) 0.0049(14) C7 0.0440(16) 0.067(2) 0.0368(15) 0.0014(15) 0.0182(14) 0.0009(15) C8 0.061(2) 0.067(2) 0.0395(16) -0.0063(15) 0.0254(16) -0.0163(17) C9 0.067(2) 0.071(2) 0.0462(18) -0.0064(17) 0.0279(17) -0.0190(19) C10 0.0522(19) 0.067(2) 0.0423(17) -0.0092(16) 0.0213(15) -0.0078(16) C11 0.061(2) 0.070(2) 0.0404(17) -0.0023(16) 0.0261(16) 0.0009(17) C12 0.060(2) 0.062(2) 0.0380(16) 0.0032(14) 0.0258(15) 0.0048(16) C13 0.0448(16) 0.0598(19) 0.0350(15) -0.0013(13) 0.0185(13) -0.0019(14) C14 0.056(2) 0.071(2) 0.0507(19) -0.0051(18) 0.0270(17) -0.0072(17) C15 0.0533(19) 0.071(2) 0.053(2) -0.0115(18) 0.0256(17) -0.0106(17) C16 0.049(2) 0.079(3) 0.069(3) -0.009(2) 0.0235(19) -0.0009(18) C17 0.060(2) 0.072(3) 0.097(4) -0.009(3) 0.032(2) 0.009(2) C18 0.062(3) 0.085(3) 0.102(4) -0.039(3) 0.039(3) 0.001(2) C19 0.065(2) 0.088(3) 0.072(3) -0.027(2) 0.035(2) -0.004(2) C20 0.061(2) 0.075(3) 0.066(2) -0.018(2) 0.036(2) -0.0094(19) C21 0.0452(18) 0.070(2) 0.063(2) -0.0145(19) 0.0261(17) -0.0083(17) C22 0.0552(18) 0.0392(15) 0.0368(16) 0.0018(12) 0.0238(15) 0.0000(13) C23 0.066(2) 0.0542(19) 0.0384(16) -0.0004(14) 0.0226(16) -0.0026(16) C24 0.087(3) 0.053(2) 0.054(2) 0.0039(17) 0.031(2) 0.0015(19) C25 0.082(3) 0.054(2) 0.072(3) -0.0020(19) 0.030(2) 0.012(2) C26 0.065(2) 0.066(2) 0.060(2) -0.0023(18) 0.0305(19) 0.0113(19) C27 0.0518(18) 0.057(2) 0.0381(16) -0.0027(14) 0.0177(14) 0.0024(15) C28 0.0451(17) 0.065(2) 0.0415(16) -0.0012(15) 0.0216(14) 0.0019(15) C29 0.0531(18) 0.066(2) 0.0376(16) 0.0015(15) 0.0206(15) -0.0100(16) C30 0.057(2) 0.063(2) 0.0444(17) 0.0010(16) 0.0201(16) -0.0098(17) C31 0.0463(17) 0.066(2) 0.0468(18) 0.0109(16) 0.0213(15) 0.0010(15) C32 0.059(2) 0.069(2) 0.0444(17) 0.0123(16) 0.0282(16) 0.0079(17) C33 0.0567(19) 0.061(2) 0.0413(16) 0.0025(15) 0.0267(15) 0.0066(16) C34 0.0414(16) 0.062(2) 0.0385(16) 0.0055(14) 0.0194(13) 0.0004(14) C35 0.0504(19) 0.067(2) 0.0472(18) 0.0078(16) 0.0214(16) 0.0018(16) C36 0.0478(18) 0.066(2) 0.0449(18) 0.0082(17) 0.0183(15) 0.0032(16) C37 0.067(2) 0.074(3) 0.053(2) 0.0057(18) 0.0261(19) 0.015(2) C38 0.075(3) 0.070(3) 0.057(2) -0.005(2) 0.019(2) 0.021(2) C39 0.068(2) 0.050(2) 0.054(2) 0.0007(16) 0.0132(18) 0.0035(17) C40 0.068(2) 0.058(2) 0.052(2) 0.0010(17) 0.0248(18) -0.0041(18) C41 0.0584(19) 0.0480(18) 0.0452(17) -0.0030(14) 0.0233(16) -0.0028(15) C42 0.0465(18) 0.060(2) 0.0412(17) 0.0029(14) 0.0124(15) 0.0053(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.7943 1.1372 '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 N1 Fe1 N2 90.96(12) N1 Fe1 N3 92.47(12) N1 Fe1 N5 94.38(12) N1 Fe1 N6 173.85(12) N2 Fe1 N3 80.68(12) N2 Fe1 N5 174.54(12) N2 Fe1 N6 94.09(12) N4 Fe1 N1 91.66(12) N4 Fe1 N2 93.56(12) N4 Fe1 N3 172.97(12) N4 Fe1 N5 87.45(12) N4 Fe1 N6 91.52(12) N5 Fe1 N3 97.91(11) N5 Fe1 N6 80.51(12) N6 Fe1 N3 84.91(11) C1 N1 Fe1 173.3(3) C2 N2 Fe1 127.8(2) C2 N2 C6 117.7(3) C6 N2 Fe1 114.3(2) C7 N3 Fe1 114.1(2) C7 N3 C13 118.8(3) C13 N3 Fe1 126.4(2) C22 N4 Fe1 172.9(3) C23 N5 Fe1 127.0(2) C27 N5 Fe1 114.6(2) C27 N5 C23 118.3(3) C28 N6 Fe1 115.6(2) C28 N6 C34 119.5(3) C34 N6 Fe1 124.6(2) N1 C1 Se1 178.4(4) N2 C2 C3 122.1(3) C4 C3 C2 120.1(4) C3 C4 C5 118.4(4) C4 C5 C6 119.1(3) N2 C6 C5 122.4(3) N2 C6 C7 112.6(3) C5 C6 C7 125.0(3) N3 C7 C6 116.8(3) C9 C8 C13 120.3(3) C8 C9 C10 120.5(4) C9 C10 C14 120.5(4) C11 C10 C9 118.2(4) C11 C10 C14 121.3(3) C12 C11 C10 121.5(3) C11 C12 C13 119.5(4) C8 C13 N3 118.8(3) C8 C13 C12 120.0(3) C12 C13 N3 121.3(3) C15 C14 C10 177.4(4) C14 C15 C21 178.2(5) C17 C16 C21 120.1(5) C16 C17 C18 119.7(5) C19 C18 C17 121.2(4) C18 C19 C20 119.3(5) C21 C20 C19 119.8(5) C16 C21 C15 119.9(4) C16 C21 C20 119.9(4) C20 C21 C15 120.1(4) N4 C22 Se2 179.5(3) N5 C23 C24 122.3(4) C23 C24 C25 119.3(4) C26 C25 C24 118.7(4) C25 C26 C27 118.8(4) N5 C27 C26 122.4(4) N5 C27 C28 113.6(3) C26 C27 C28 124.0(4) N6 C28 C27 115.6(3) C30 C29 C34 120.4(3) C29 C30 C31 120.2(4) C30 C31 C35 118.1(4) C32 C31 C30 118.9(3) C32 C31 C35 123.1(3) C31 C32 C33 121.1(3) C34 C33 C32 119.3(4) C29 C34 N6 118.7(3) C33 C34 N6 121.0(3) C33 C34 C29 120.1(3) C36 C35 C31 176.5(4) C35 C36 C42 176.4(4) C38 C37 C42 119.5(4) C39 C38 C37 120.3(4) C40 C39 C38 120.2(4) C39 C40 C41 120.3(4) C40 C41 C42 120.2(4) C37 C42 C36 119.4(4) C41 C42 C36 121.1(4) C41 C42 C37 119.5(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se1 C1 1.806(4) Se2 C22 1.786(3) Fe1 N1 1.947(3) Fe1 N2 1.963(3) Fe1 N3 1.984(3) Fe1 N4 1.937(3) Fe1 N5 1.974(3) Fe1 N6 1.976(3) N1 C1 1.152(5) N2 C2 1.344(5) N2 C6 1.353(4) N3 C7 1.287(5) N3 C13 1.425(4) N4 C22 1.165(5) N5 C23 1.346(5) N5 C27 1.342(5) N6 C28 1.287(5) N6 C34 1.431(4) C2 C3 1.375(6) C3 C4 1.373(6) C4 C5 1.377(6) C5 C6 1.385(5) C6 C7 1.452(5) C8 C9 1.378(6) C8 C13 1.385(5) C9 C10 1.407(5) C10 C11 1.385(6) C10 C14 1.424(6) C11 C12 1.383(5) C12 C13 1.390(5) C14 C15 1.200(6) C15 C21 1.431(6) C16 C17 1.374(7) C16 C21 1.394(7) C17 C18 1.397(8) C18 C19 1.368(8) C19 C20 1.402(6) C20 C21 1.394(6) C23 C24 1.374(6) C24 C25 1.392(7) C25 C26 1.377(7) C26 C27 1.392(5) C27 C28 1.457(5) C29 C30 1.378(5) C29 C34 1.389(5) C30 C31 1.408(5) C31 C32 1.383(6) C31 C35 1.448(5) C32 C33 1.393(5) C33 C34 1.388(5) C35 C36 1.195(6) C36 C42 1.437(6) C37 C38 1.395(7) C37 C42 1.398(6) C38 C39 1.386(7) C39 C40 1.372(6) C40 C41 1.390(5) C41 C42 1.393(5)