#------------------------------------------------------------------------------ #$Date: 2019-10-08 03:56:35 +0300 (Tue, 08 Oct 2019) $ #$Revision: 219141 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234440.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_7234440 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 117.370(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.9943(7) _cell_length_b 14.9296(5) _cell_length_c 17.2155(6) _cell_measurement_reflns_used 9276 _cell_measurement_temperature 293 _cell_measurement_theta_max 70.8760 _cell_measurement_theta_min 2.9030 _cell_volume 3878.9(3) _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 293 _diffrn_detector 'CCD plate' _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.972 _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 25.00 -- -105.00 24.00 144.00 180 2 \w -38.00 10.00 1.00 5.00 -- 5.00 24.00 144.00 48 3 \w -164.00 -15.00 1.00 25.00 -- -105.00 60.00-180.00 149 4 \w -131.00 49.00 1.00 5.00 -- -41.00 60.00-144.00 180 5 \w -178.00 -52.00 1.00 25.00 -- -105.00 60.00 108.00 126 6 \w -195.00 -46.00 1.00 25.00 -- -105.00 48.00 -36.00 149 7 \w -131.00 49.00 1.00 5.00 -- -41.00 36.00 0.00 180 8 \w -164.00 -33.00 1.00 25.00 -- -105.00 60.00-144.00 131 9 \w -182.00 -88.00 1.00 25.00 -- -105.00 60.00 144.00 94 10 \w -194.00 -62.00 1.00 25.00 -- -105.00 60.00-108.00 132 11 \w -124.00 -70.00 1.00 5.00 -- -41.00 60.00 0.00 54 12 \w -195.00-115.00 1.00 25.00 -- -105.00 60.00 -36.00 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 -0.0958221000 _diffrn_orient_matrix_UB_12 0.0050449000 _diffrn_orient_matrix_UB_13 -0.0739575000 _diffrn_orient_matrix_UB_21 -0.0075019000 _diffrn_orient_matrix_UB_22 -0.1027942000 _diffrn_orient_matrix_UB_23 0.0018841000 _diffrn_orient_matrix_UB_31 -0.0342581000 _diffrn_orient_matrix_UB_32 0.0083047000 _diffrn_orient_matrix_UB_33 0.0684048000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0312 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 28515 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 73.354 _diffrn_reflns_theta_min 2.928 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 5.551 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.58925 _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 1.422 _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 0.430 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.054 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 460 _refine_ls_number_reflns 7579 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0737 _refine_ls_R_factor_gt 0.0561 _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^)+(0.0976P)^2^+0.6487P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1645 _refine_ls_wR_factor_ref 0.1775 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5366 _reflns_number_total 7579 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01137d2.cif _cod_data_source_block mmet29_amb _cod_database_code 7234440 _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 0.607 _shelx_estimated_absorpt_t_min 0.168 _reflns_odcompleteness_completeness 97.12 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 73.20 _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 in P21/c #14 mmet29_amb.res created by SHELXL-2016/6 at 16:50:35 on 01-Jul-2019 REM reset to P21/c #14 CELL 1.54184 16.99428 14.929601 17.215497 90 117.37 90 ZERR 4 0.000733 0.000451 0.000597 0 0.005 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 PLAN 20 SIZE 0.5 0.1 0.1 TEMP 19.85 BOND fmap 2 acta OMIT -1 6 5 OMIT -4 1 8 OMIT 0 11 1 OMIT 1 12 0 OMIT 1 6 3 OMIT -1 1 8 OMIT -3 6 4 OMIT -3 1 7 OMIT -4 5 6 REM REM REM WGHT 0.097600 0.648700 FVAR 3.16694 SE1 5 0.465014 0.358749 0.065472 11.00000 0.13592 0.15666 = 0.10798 -0.04330 0.06787 -0.05544 SE2 5 -0.005298 0.209203 -0.137403 11.00000 0.10862 0.10784 = 0.09289 -0.01077 0.04280 -0.01634 FE1 3 0.238851 0.273434 0.155242 11.00000 0.08199 0.08060 = 0.07245 -0.00056 0.03362 0.00080 N1 4 0.323983 0.326247 0.113532 11.00000 0.10454 0.14197 = 0.08902 -0.01448 0.04543 0.00290 N2 4 0.293557 0.144727 0.183103 11.00000 0.08756 0.08305 = 0.07273 -0.00230 0.03849 0.00231 N3 4 0.332187 0.282123 0.290417 11.00000 0.08028 0.08453 = 0.06811 0.00071 0.03909 -0.00385 N4 4 0.146134 0.238306 0.032742 11.00000 0.10427 0.10215 = 0.09896 0.00832 0.04081 -0.00014 N5 4 0.174384 0.394094 0.146471 11.00000 0.09565 0.08367 = 0.07422 0.00480 0.03438 -0.00152 N6 4 0.151314 0.241784 0.209423 11.00000 0.07590 0.08455 = 0.07402 -0.00211 0.03601 -0.00446 C1 1 0.378267 0.339462 0.095392 11.00000 0.11034 0.09381 = 0.07122 -0.01611 0.04124 -0.00733 C2 1 0.275561 0.076654 0.127132 11.00000 0.11541 0.11112 = 0.08156 -0.01111 0.04813 0.00974 AFIX 43 H2 2 0.241757 0.087820 0.067674 11.00000 -1.20000 AFIX 0 C3 1 0.304721 -0.008846 0.153499 11.00000 0.13226 0.10365 = 0.10712 -0.01564 0.05668 0.01669 AFIX 43 H3 2 0.291009 -0.054535 0.112579 11.00000 -1.20000 AFIX 0 C4 1 0.354030 -0.026143 0.240347 11.00000 0.12646 0.08965 = 0.11812 0.00185 0.05171 0.03149 AFIX 43 H4 2 0.373507 -0.083972 0.259755 11.00000 -1.20000 AFIX 0 C5 1 0.374602 0.043482 0.299029 11.00000 0.10274 0.09980 = 0.09153 0.00832 0.03795 0.02576 AFIX 43 H5 2 0.408319 0.033362 0.358689 11.00000 -1.20000 AFIX 0 C6 1 0.344648 0.127960 0.268216 11.00000 0.08048 0.08955 = 0.07905 -0.00070 0.04000 0.00752 C7 1 0.365745 0.206741 0.324613 11.00000 0.07752 0.09041 = 0.06815 0.00056 0.03070 0.00515 AFIX 43 H7 2 0.402964 0.202057 0.384366 11.00000 -1.20000 AFIX 0 C8 1 0.359674 0.439878 0.313809 11.00000 0.10733 0.08965 = 0.07433 -0.00441 0.04259 -0.01995 AFIX 43 H8 2 0.355514 0.443876 0.258135 11.00000 -1.20000 AFIX 0 C9 1 0.375324 0.516221 0.364331 11.00000 0.11699 0.09081 = 0.08983 -0.00233 0.04625 -0.01618 AFIX 43 H9 2 0.381391 0.571181 0.342219 11.00000 -1.20000 AFIX 0 C10 1 0.382017 0.511639 0.447161 11.00000 0.09368 0.09263 = 0.08950 -0.01374 0.04196 -0.00847 C11 1 0.374264 0.429334 0.478992 11.00000 0.12149 0.10270 = 0.08056 -0.00558 0.05609 -0.00054 AFIX 43 H11 2 0.380886 0.425220 0.535587 11.00000 -1.20000 AFIX 0 C12 1 0.356908 0.352844 0.428916 11.00000 0.11221 0.08414 = 0.07877 -0.00036 0.05057 0.00086 AFIX 43 H12 2 0.349699 0.298091 0.450619 11.00000 -1.20000 AFIX 0 C13 1 0.350294 0.358680 0.345137 11.00000 0.07865 0.08324 = 0.06795 -0.00302 0.03357 -0.00498 C14 1 0.394904 0.590837 0.498765 11.00000 0.09961 0.09097 = 0.10297 -0.01278 0.04725 -0.00809 C15 1 0.402605 0.657831 0.539016 11.00000 0.09427 0.09980 = 0.10941 -0.01452 0.05073 -0.01312 C16 1 0.380319 0.818054 0.541237 11.00000 0.10419 0.11617 = 0.14031 -0.01389 0.04691 -0.00062 AFIX 43 H16 2 0.357727 0.819421 0.480738 11.00000 -1.20000 AFIX 0 C17 1 0.386481 0.896330 0.587935 11.00000 0.12290 0.09500 = 0.21856 -0.01100 0.07196 0.00784 AFIX 43 H17 2 0.366178 0.950149 0.558149 11.00000 -1.20000 AFIX 0 C18 1 0.421967 0.894648 0.676771 11.00000 0.14430 0.11779 = 0.19795 -0.06519 0.09735 -0.02022 AFIX 43 H18 2 0.427151 0.947815 0.706904 11.00000 -1.20000 AFIX 0 C19 1 0.449582 0.817847 0.721650 11.00000 0.14509 0.13368 = 0.14847 -0.05033 0.08867 -0.02370 AFIX 43 H19 2 0.472909 0.818199 0.782237 11.00000 -1.20000 AFIX 0 C20 1 0.443514 0.737415 0.677965 11.00000 0.11966 0.10190 = 0.13384 -0.02619 0.07790 -0.02028 AFIX 43 H20 2 0.462478 0.684158 0.709127 11.00000 -1.20000 AFIX 0 C21 1 0.408738 0.737642 0.587124 11.00000 0.08634 0.08556 = 0.12230 -0.01877 0.05470 -0.01437 C22 1 0.086741 0.226758 -0.033848 11.00000 0.09829 0.06471 = 0.08341 0.00444 0.04398 -0.00110 C23 1 0.183000 0.469727 0.109285 11.00000 0.14872 0.09638 = 0.09212 0.01018 0.04646 -0.00810 AFIX 43 H23 2 0.224026 0.471362 0.087619 11.00000 -1.20000 AFIX 0 C24 1 0.133321 0.545377 0.101873 11.00000 0.19105 0.09662 = 0.13957 0.01908 0.04521 0.00931 AFIX 43 H24 2 0.140540 0.596637 0.075114 11.00000 -1.20000 AFIX 0 C25 1 0.073777 0.544239 0.134041 11.00000 0.17820 0.08093 = 0.18382 0.00692 0.04256 0.03214 AFIX 43 H25 2 0.041380 0.595378 0.131375 11.00000 -1.20000 AFIX 0 C26 1 0.061732 0.466020 0.170935 11.00000 0.11557 0.11173 = 0.15678 -0.01360 0.05962 0.02352 AFIX 43 H26 2 0.019920 0.462963 0.191554 11.00000 -1.20000 AFIX 0 C27 1 0.113753 0.392840 0.176094 11.00000 0.08526 0.09008 = 0.09153 -0.00599 0.03200 0.00126 C28 1 0.106513 0.308271 0.214278 11.00000 0.08233 0.09909 = 0.10397 -0.00710 0.05221 -0.00326 AFIX 43 H28 2 0.070381 0.302795 0.241382 11.00000 -1.20000 AFIX 0 C29 1 0.125128 0.082177 0.196852 11.00000 0.09934 0.09640 = 0.07895 -0.00061 0.03707 -0.01889 AFIX 43 H29 2 0.107818 0.086881 0.137311 11.00000 -1.20000 AFIX 0 C30 1 0.127714 -0.000146 0.233441 11.00000 0.10161 0.09517 = 0.10118 -0.00344 0.03970 -0.02002 AFIX 43 H30 2 0.112614 -0.051014 0.198356 11.00000 -1.20000 AFIX 0 C31 1 0.152316 -0.008608 0.321289 11.00000 0.08465 0.09874 = 0.09987 0.01141 0.04006 -0.00339 C32 1 0.175794 0.068610 0.373039 11.00000 0.10762 0.11369 = 0.08310 0.01592 0.04558 0.00190 AFIX 43 H32 2 0.193514 0.064248 0.432682 11.00000 -1.20000 AFIX 0 C33 1 0.172779 0.150581 0.336198 11.00000 0.10280 0.09351 = 0.08633 -0.00453 0.05105 -0.00068 AFIX 43 H33 2 0.187494 0.201688 0.370939 11.00000 -1.20000 AFIX 0 C34 1 0.148342 0.158273 0.248738 11.00000 0.07195 0.08799 = 0.08000 0.00296 0.03728 -0.00394 C35 1 0.152098 -0.096229 0.356311 11.00000 0.09457 0.10150 = 0.11323 0.02129 0.04247 -0.00118 C36 1 0.147729 -0.170914 0.378651 11.00000 0.09549 0.10463 = 0.10112 0.00987 0.03332 0.00024 C37 1 0.161517 -0.332805 0.361997 11.00000 0.13941 0.11408 = 0.11801 0.01421 0.06173 0.01757 AFIX 43 H37 2 0.183981 -0.320583 0.323018 11.00000 -1.20000 AFIX 0 C38 1 0.150815 -0.419357 0.380396 11.00000 0.14170 0.10782 = 0.12863 -0.00747 0.04052 0.02722 AFIX 43 H38 2 0.166940 -0.466018 0.354836 11.00000 -1.20000 AFIX 0 C39 1 0.115365 -0.438052 0.438072 11.00000 0.12841 0.09430 = 0.13237 0.01733 0.03276 -0.00155 AFIX 43 H39 2 0.106975 -0.497080 0.449877 11.00000 -1.20000 AFIX 0 C40 1 0.093785 -0.370944 0.475835 11.00000 0.16197 0.11243 = 0.12790 0.00466 0.07490 -0.00732 AFIX 43 H40 2 0.070714 -0.383263 0.514305 11.00000 -1.20000 AFIX 0 C41 1 0.105536 -0.283908 0.458072 11.00000 0.14130 0.09336 = 0.11072 0.00244 0.06630 -0.00388 AFIX 43 H41 2 0.090414 -0.238056 0.485288 11.00000 -1.20000 AFIX 0 C42 1 0.138901 -0.262107 0.401417 11.00000 0.08555 0.09433 = 0.09311 0.01083 0.02978 0.00601 HKLF 4 REM MMET29_amb in P21/c #14 REM R1 = 0.0561 for 5366 Fo > 4sig(Fo) and 0.0737 for all 7579 data REM 460 parameters refined using 0 restraints END WGHT 0.0976 0.6488 REM Highest difference peak 0.430, deepest hole -0.528, 1-sigma level 0.054 Q1 1 0.4774 0.2895 0.0831 11.00000 0.05 0.43 Q2 1 0.0417 0.1568 -0.1093 11.00000 0.05 0.41 Q3 1 0.2599 0.2325 0.1665 11.00000 0.05 0.38 Q4 1 0.2083 0.2581 0.1529 11.00000 0.05 0.31 Q5 1 -0.0501 0.1995 -0.1085 11.00000 0.05 0.29 Q6 1 0.3902 0.3744 0.0445 11.00000 0.05 0.28 Q7 1 0.3932 0.4001 0.0145 11.00000 0.05 0.27 Q8 1 0.3184 0.2902 0.1301 11.00000 0.05 0.26 Q9 1 0.1230 0.2581 -0.0025 11.00000 0.05 0.23 Q10 1 0.2925 0.2769 0.2582 11.00000 0.05 0.23 Q11 1 0.3559 0.1689 0.2948 11.00000 0.05 0.22 Q12 1 0.1375 0.2034 0.0097 11.00000 0.05 0.21 Q13 1 0.4145 0.3092 0.1177 11.00000 0.05 0.21 Q14 1 0.3936 0.7635 0.5564 11.00000 0.05 0.21 Q15 1 0.3413 0.1466 0.2204 11.00000 0.05 0.21 Q16 1 0.1466 0.2030 0.2222 11.00000 0.05 0.19 Q17 1 0.5530 0.4063 0.0823 11.00000 0.05 0.19 Q18 1 0.3115 0.3323 0.0686 11.00000 0.05 0.19 Q19 1 0.3702 0.3487 0.3875 11.00000 0.05 0.19 Q20 1 0.0679 0.4649 0.2146 11.00000 0.05 0.17 ; _shelx_res_checksum 48951 _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 1.583 _oxdiff_exptl_absorpt_empirical_full_min 0.659 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 0.46501(5) 0.35875(6) 0.06547(4) 0.1289(3) Uani 1 1 d . Se2 Se -0.00530(4) 0.20920(4) -0.13740(3) 0.1045(2) Uani 1 1 d . Fe1 Fe 0.23885(4) 0.27343(5) 0.15524(4) 0.0791(2) Uani 1 1 d . N1 N 0.3240(3) 0.3262(4) 0.1135(3) 0.1115(13) Uani 1 1 d . N2 N 0.2936(2) 0.1447(2) 0.1831(2) 0.0805(8) Uani 1 1 d . N3 N 0.3322(2) 0.2821(2) 0.2904(2) 0.0757(8) Uani 1 1 d . N4 N 0.1461(3) 0.2383(3) 0.0327(3) 0.1041(11) Uani 1 1 d . N5 N 0.1744(2) 0.3941(2) 0.1465(2) 0.0863(9) Uani 1 1 d . N6 N 0.1513(2) 0.2418(2) 0.2094(2) 0.0776(8) Uani 1 1 d . C1 C 0.3783(4) 0.3395(3) 0.0954(3) 0.0920(12) Uani 1 1 d . C2 C 0.2756(4) 0.0767(4) 0.1271(3) 0.1016(14) Uani 1 1 d . H2 H 0.241757 0.087820 0.067674 0.122 Uiso 1 1 calc R C3 C 0.3047(4) -0.0088(4) 0.1535(4) 0.1137(16) Uani 1 1 d . H3 H 0.291009 -0.054535 0.112579 0.136 Uiso 1 1 calc R C4 C 0.3540(4) -0.0261(4) 0.2403(4) 0.1132(16) Uani 1 1 d . H4 H 0.373507 -0.083972 0.259755 0.136 Uiso 1 1 calc R C5 C 0.3746(3) 0.0435(4) 0.2990(3) 0.1006(13) Uani 1 1 d . H5 H 0.408319 0.033362 0.358689 0.121 Uiso 1 1 calc R C6 C 0.3446(3) 0.1280(3) 0.2682(3) 0.0817(10) Uani 1 1 d . C7 C 0.3657(3) 0.2067(3) 0.3246(2) 0.0798(10) Uani 1 1 d . H7 H 0.402964 0.202057 0.384366 0.096 Uiso 1 1 calc R C8 C 0.3597(3) 0.4399(3) 0.3138(3) 0.0901(11) Uani 1 1 d . H8 H 0.355514 0.443876 0.258135 0.108 Uiso 1 1 calc R C9 C 0.3753(3) 0.5162(3) 0.3643(3) 0.0997(13) Uani 1 1 d . H9 H 0.381391 0.571181 0.342219 0.120 Uiso 1 1 calc R C10 C 0.3820(3) 0.5116(3) 0.4472(3) 0.0920(12) Uani 1 1 d . C11 C 0.3743(4) 0.4293(4) 0.4790(3) 0.0978(13) Uani 1 1 d . H11 H 0.380886 0.425220 0.535587 0.117 Uiso 1 1 calc R C12 C 0.3569(3) 0.3528(3) 0.4289(3) 0.0891(11) Uani 1 1 d . H12 H 0.349699 0.298091 0.450619 0.107 Uiso 1 1 calc R C13 C 0.3503(3) 0.3587(3) 0.3451(2) 0.0767(9) Uani 1 1 d . C14 C 0.3949(3) 0.5908(3) 0.4988(3) 0.0976(12) Uani 1 1 d . C15 C 0.4026(3) 0.6578(4) 0.5390(3) 0.0996(13) Uani 1 1 d . C16 C 0.3803(4) 0.8181(5) 0.5412(5) 0.1238(18) Uani 1 1 d . H16 H 0.357727 0.819421 0.480738 0.149 Uiso 1 1 calc R C17 C 0.3865(5) 0.8963(5) 0.5879(7) 0.148(3) Uani 1 1 d . H17 H 0.366178 0.950149 0.558149 0.178 Uiso 1 1 calc R C18 C 0.4220(5) 0.8946(6) 0.6768(7) 0.146(3) Uani 1 1 d . H18 H 0.427151 0.947815 0.706904 0.175 Uiso 1 1 calc R C19 C 0.4496(5) 0.8178(6) 0.7217(5) 0.134(2) Uani 1 1 d . H19 H 0.472909 0.818199 0.782237 0.161 Uiso 1 1 calc R C20 C 0.4435(4) 0.7374(4) 0.6780(4) 0.1108(16) Uani 1 1 d . H20 H 0.462478 0.684158 0.709127 0.133 Uiso 1 1 calc R C21 C 0.4087(3) 0.7376(3) 0.5871(4) 0.0954(13) Uani 1 1 d . C22 C 0.0867(3) 0.2268(3) -0.0338(3) 0.0813(10) Uani 1 1 d . C23 C 0.1830(4) 0.4697(4) 0.1093(3) 0.1159(17) Uani 1 1 d . H23 H 0.224026 0.471362 0.087619 0.139 Uiso 1 1 calc R C24 C 0.1333(7) 0.5454(5) 0.1019(5) 0.154(3) Uani 1 1 d . H24 H 0.140540 0.596637 0.075114 0.185 Uiso 1 1 calc R C25 C 0.0738(6) 0.5442(5) 0.1340(6) 0.163(3) Uani 1 1 d . H25 H 0.041380 0.595378 0.131375 0.196 Uiso 1 1 calc R C26 C 0.0617(4) 0.4660(5) 0.1709(5) 0.129(2) Uani 1 1 d . H26 H 0.019920 0.462963 0.191554 0.155 Uiso 1 1 calc R C27 C 0.1138(3) 0.3928(3) 0.1761(3) 0.0923(12) Uani 1 1 d . C28 C 0.1065(3) 0.3083(3) 0.2143(3) 0.0915(12) Uani 1 1 d . H28 H 0.070381 0.302795 0.241382 0.110 Uiso 1 1 calc R C29 C 0.1251(3) 0.0822(3) 0.1969(3) 0.0931(12) Uani 1 1 d . H29 H 0.107818 0.086881 0.137311 0.112 Uiso 1 1 calc R C30 C 0.1277(3) -0.0001(4) 0.2334(3) 0.1020(13) Uani 1 1 d . H30 H 0.112614 -0.051014 0.198356 0.122 Uiso 1 1 calc R C31 C 0.1523(3) -0.0086(4) 0.3213(3) 0.0953(12) Uani 1 1 d . C32 C 0.1758(3) 0.0686(4) 0.3730(3) 0.1008(13) Uani 1 1 d . H32 H 0.193514 0.064248 0.432682 0.121 Uiso 1 1 calc R C33 C 0.1728(3) 0.1506(3) 0.3362(3) 0.0913(11) Uani 1 1 d . H33 H 0.187494 0.201688 0.370939 0.110 Uiso 1 1 calc R C34 C 0.1483(3) 0.1583(3) 0.2487(3) 0.0791(9) Uani 1 1 d . C35 C 0.1521(3) -0.0962(4) 0.3563(4) 0.1052(14) Uani 1 1 d . C36 C 0.1477(3) -0.1709(4) 0.3787(3) 0.1050(14) Uani 1 1 d . C37 C 0.1615(4) -0.3328(5) 0.3620(4) 0.1228(18) Uani 1 1 d . H37 H 0.183981 -0.320583 0.323018 0.147 Uiso 1 1 calc R C38 C 0.1508(5) -0.4194(5) 0.3804(5) 0.134(2) Uani 1 1 d . H38 H 0.166940 -0.466018 0.354836 0.161 Uiso 1 1 calc R C39 C 0.1154(4) -0.4381(4) 0.4381(5) 0.129(2) Uani 1 1 d . H39 H 0.106975 -0.497080 0.449877 0.155 Uiso 1 1 calc R C40 C 0.0938(5) -0.3709(5) 0.4758(5) 0.131(2) Uani 1 1 d . H40 H 0.070714 -0.383263 0.514305 0.157 Uiso 1 1 calc R C41 C 0.1055(4) -0.2839(4) 0.4581(4) 0.1119(16) Uani 1 1 d . H41 H 0.090414 -0.238056 0.485288 0.134 Uiso 1 1 calc R C42 C 0.1389(3) -0.2621(4) 0.4014(3) 0.0954(12) 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 0.1359(5) 0.1567(6) 0.1080(4) -0.0433(4) 0.0679(4) -0.0554(4) Se2 0.1086(4) 0.1078(4) 0.0929(3) -0.0108(3) 0.0428(3) -0.0163(3) Fe1 0.0820(4) 0.0806(4) 0.0725(3) -0.0006(3) 0.0336(3) 0.0008(3) N1 0.105(3) 0.142(4) 0.089(2) -0.014(2) 0.045(2) 0.003(3) N2 0.088(2) 0.083(2) 0.0727(17) -0.0023(15) 0.0385(16) 0.0023(16) N3 0.0803(18) 0.085(2) 0.0681(15) 0.0007(14) 0.0391(14) -0.0039(16) N4 0.104(3) 0.102(3) 0.099(3) 0.008(2) 0.041(2) 0.000(2) N5 0.096(2) 0.084(2) 0.0742(17) 0.0048(16) 0.0344(17) -0.0015(17) N6 0.0759(18) 0.085(2) 0.0740(17) -0.0021(15) 0.0360(15) -0.0045(16) C1 0.110(3) 0.094(3) 0.071(2) -0.016(2) 0.041(2) -0.007(2) C2 0.115(3) 0.111(4) 0.082(2) -0.011(2) 0.048(2) 0.010(3) C3 0.132(4) 0.104(4) 0.107(4) -0.016(3) 0.057(3) 0.017(3) C4 0.126(4) 0.090(3) 0.118(4) 0.002(3) 0.052(3) 0.031(3) C5 0.103(3) 0.100(3) 0.092(3) 0.008(2) 0.038(2) 0.026(3) C6 0.080(2) 0.090(3) 0.079(2) -0.0007(19) 0.0400(19) 0.0075(19) C7 0.078(2) 0.090(3) 0.0682(19) 0.0006(18) 0.0307(17) 0.0051(19) C8 0.107(3) 0.090(3) 0.074(2) -0.0044(19) 0.043(2) -0.020(2) C9 0.117(3) 0.091(3) 0.090(3) -0.002(2) 0.046(3) -0.016(3) C10 0.094(3) 0.093(3) 0.090(3) -0.014(2) 0.042(2) -0.008(2) C11 0.121(4) 0.103(3) 0.081(2) -0.006(2) 0.056(2) -0.001(3) C12 0.112(3) 0.084(3) 0.079(2) -0.0004(19) 0.051(2) 0.001(2) C13 0.079(2) 0.083(2) 0.0679(18) -0.0030(17) 0.0336(17) -0.0050(18) C14 0.100(3) 0.091(3) 0.103(3) -0.013(2) 0.047(2) -0.008(2) C15 0.094(3) 0.100(3) 0.109(3) -0.015(3) 0.051(3) -0.013(2) C16 0.104(4) 0.116(5) 0.140(5) -0.014(4) 0.047(3) -0.001(3) C17 0.123(5) 0.095(4) 0.219(9) -0.011(5) 0.072(6) 0.008(3) C18 0.144(6) 0.118(6) 0.198(8) -0.065(6) 0.097(6) -0.020(4) C19 0.145(5) 0.134(6) 0.148(5) -0.050(5) 0.089(5) -0.024(4) C20 0.120(4) 0.102(4) 0.134(4) -0.026(3) 0.078(3) -0.020(3) C21 0.086(3) 0.086(3) 0.122(4) -0.019(3) 0.055(3) -0.014(2) C22 0.098(3) 0.065(2) 0.083(2) 0.0044(17) 0.044(2) -0.0011(19) C23 0.149(5) 0.096(4) 0.092(3) 0.010(3) 0.046(3) -0.008(3) C24 0.191(8) 0.097(5) 0.140(5) 0.019(4) 0.045(5) 0.009(5) C25 0.178(8) 0.081(4) 0.184(8) 0.007(4) 0.043(6) 0.032(4) C26 0.116(4) 0.112(5) 0.157(5) -0.014(4) 0.060(4) 0.024(3) C27 0.085(3) 0.090(3) 0.092(3) -0.006(2) 0.032(2) 0.001(2) C28 0.082(3) 0.099(3) 0.104(3) -0.007(2) 0.052(2) -0.003(2) C29 0.099(3) 0.096(3) 0.079(2) -0.001(2) 0.037(2) -0.019(2) C30 0.102(3) 0.095(3) 0.101(3) -0.003(2) 0.040(3) -0.020(3) C31 0.085(3) 0.099(3) 0.100(3) 0.011(2) 0.040(2) -0.003(2) C32 0.108(3) 0.114(4) 0.083(2) 0.016(2) 0.046(2) 0.002(3) C33 0.103(3) 0.094(3) 0.086(2) -0.005(2) 0.051(2) -0.001(2) C34 0.072(2) 0.088(3) 0.080(2) 0.0030(19) 0.0373(18) -0.0039(18) C35 0.095(3) 0.102(4) 0.113(3) 0.021(3) 0.042(3) -0.001(3) C36 0.095(3) 0.105(4) 0.101(3) 0.010(3) 0.033(3) 0.000(3) C37 0.139(5) 0.114(5) 0.118(4) 0.014(3) 0.062(4) 0.018(4) C38 0.142(5) 0.108(5) 0.129(5) -0.007(4) 0.041(4) 0.027(4) C39 0.128(5) 0.094(4) 0.132(5) 0.017(3) 0.033(4) -0.002(3) C40 0.162(6) 0.112(5) 0.128(4) 0.005(4) 0.075(4) -0.007(4) C41 0.141(5) 0.093(4) 0.111(3) 0.002(3) 0.066(3) -0.004(3) C42 0.086(3) 0.094(3) 0.093(3) 0.011(2) 0.030(2) 0.006(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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 97.07(18) N1 Fe1 N3 93.91(15) N1 Fe1 N5 94.28(18) N1 Fe1 N6 169.50(17) N2 Fe1 N3 77.09(13) N2 Fe1 N6 91.26(14) N3 Fe1 N6 81.68(12) N4 Fe1 N1 94.08(18) N4 Fe1 N2 92.96(16) N4 Fe1 N3 167.94(16) N4 Fe1 N5 90.97(16) N4 Fe1 N6 91.87(16) N5 Fe1 N2 167.69(14) N5 Fe1 N3 97.43(13) N5 Fe1 N6 76.95(14) C1 N1 Fe1 166.5(5) C2 N2 Fe1 127.1(3) C2 N2 C6 117.7(4) C6 N2 Fe1 114.8(3) C7 N3 Fe1 113.6(3) C7 N3 C13 119.2(3) C13 N3 Fe1 126.7(3) C22 N4 Fe1 170.4(4) C23 N5 Fe1 126.6(4) C23 N5 C27 117.7(5) C27 N5 Fe1 115.5(3) C28 N6 Fe1 114.3(3) C28 N6 C34 119.7(4) C34 N6 Fe1 125.5(3) N1 C1 Se1 179.0(5) N2 C2 C3 122.8(5) C4 C3 C2 119.2(5) C3 C4 C5 118.9(5) C6 C5 C4 119.1(4) N2 C6 C5 122.2(4) N2 C6 C7 114.5(4) C5 C6 C7 123.3(4) N3 C7 C6 118.8(4) C13 C8 C9 120.4(4) C10 C9 C8 120.7(5) C9 C10 C14 121.1(5) C11 C10 C9 118.6(4) C11 C10 C14 120.3(4) C10 C11 C12 121.5(4) C11 C12 C13 119.1(4) C8 C13 N3 118.7(3) C8 C13 C12 119.6(4) C12 C13 N3 121.6(4) C15 C14 C10 177.4(6) C14 C15 C21 177.9(5) C17 C16 C21 118.7(7) C18 C17 C16 120.6(7) C19 C18 C17 121.3(7) C18 C19 C20 120.4(7) C21 C20 C19 119.4(7) C16 C21 C15 118.4(5) C20 C21 C15 121.9(5) C20 C21 C16 119.7(5) N4 C22 Se2 179.8(5) N5 C23 C24 122.5(7) C25 C24 C23 119.4(7) C24 C25 C26 119.4(7) C27 C26 C25 118.0(7) N5 C27 C26 123.0(5) N5 C27 C28 115.0(4) C26 C27 C28 122.0(5) N6 C28 C27 117.9(4) C30 C29 C34 119.9(4) C29 C30 C31 121.0(5) C30 C31 C32 118.5(5) C30 C31 C35 119.0(5) C32 C31 C35 122.5(5) C33 C32 C31 120.2(4) C32 C33 C34 120.8(5) C29 C34 N6 118.1(4) C33 C34 N6 122.3(4) C33 C34 C29 119.5(4) C36 C35 C31 174.8(6) C35 C36 C42 177.2(6) C38 C37 C42 120.4(6) C37 C38 C39 119.9(6) C40 C39 C38 119.9(6) C39 C40 C41 120.2(7) C40 C41 C42 122.2(6) C37 C42 C36 119.6(5) C41 C42 C36 123.0(5) C41 C42 C37 117.4(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Se1 C1 1.794(6) Se2 C22 1.769(5) Fe1 N1 2.046(5) Fe1 N2 2.092(4) Fe1 N3 2.134(3) Fe1 N4 2.037(5) Fe1 N5 2.077(4) Fe1 N6 2.141(3) N1 C1 1.119(6) N2 C2 1.336(6) N2 C6 1.339(5) N3 C7 1.277(5) N3 C13 1.422(5) N4 C22 1.140(6) N5 C23 1.339(6) N5 C27 1.344(6) N6 C28 1.277(6) N6 C34 1.431(5) C2 C3 1.369(8) C3 C4 1.361(8) C4 C5 1.378(7) C5 C6 1.372(6) C6 C7 1.461(6) C8 C9 1.383(7) C8 C13 1.366(6) C9 C10 1.379(7) C10 C11 1.376(7) C10 C14 1.434(7) C11 C12 1.379(6) C12 C13 1.397(5) C14 C15 1.189(7) C15 C21 1.427(7) C16 C17 1.395(10) C16 C21 1.396(9) C17 C18 1.362(11) C18 C19 1.341(11) C19 C20 1.395(8) C20 C21 1.395(8) C23 C24 1.380(10) C24 C25 1.359(13) C25 C26 1.389(11) C26 C27 1.382(8) C27 C28 1.455(7) C29 C30 1.373(7) C29 C34 1.386(6) C30 C31 1.377(7) C31 C32 1.398(7) C31 C35 1.441(7) C32 C33 1.368(7) C33 C34 1.370(6) C35 C36 1.193(7) C36 C42 1.444(8) C37 C38 1.362(10) C37 C42 1.401(8) C38 C39 1.406(10) C39 C40 1.334(10) C40 C41 1.370(8) C41 C42 1.374(8)