# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_aral26 _audit_creation_date 2013-11-12 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _shelxl_version_number 2013-2 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C24 H20 Fe Se4, 2(C11 H21 N2), 2(C2 H3 N)' _chemical_formula_sum 'C50 H68 Fe N6 Se4' _chemical_formula_weight 1124.79 _chemical_melting_point ? _chemical_oxdiff_formula C23H30N2Se2Fe1 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' N N 0.0061 0.0033 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.1328(7) _cell_length_b 11.4406(3) _cell_length_c 25.8000(9) _cell_angle_alpha 90 _cell_angle_beta 98.655(4) _cell_angle_gamma 90 _cell_volume 5291.3(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3591 _cell_measurement_temperature 150.03(10) _cell_measurement_theta_max 27.3530 _cell_measurement_theta_min 3.5560 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 3.074 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.78224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Green _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2288 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_unetI/netI 0.0569 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 10803 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.562 _diffrn_ambient_temperature 150.03(10) _diffrn_detector_area_resol_mean 8.0714 _diffrn_measured_fraction_theta_full 0.9974 _diffrn_measured_fraction_theta_max 0.8521 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -76.00 -25.00 1.0000 3.5000 omega____ theta____ kappa____ phi______ frames - -21.1798 117.0000 -114.0000 51 #__ type_ start__ end____ width___ exp.time_ 2 omega -82.00 26.00 1.0000 3.5000 omega____ theta____ kappa____ phi______ frames - -21.1798 19.0000 -150.0000 108 #__ type_ start__ end____ width___ exp.time_ 3 omega -45.00 35.00 1.0000 3.5000 omega____ theta____ kappa____ phi______ frames - -21.1798 -19.0000 120.0000 80 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0095460000 _diffrn_orient_matrix_UB_12 -0.0069370000 _diffrn_orient_matrix_UB_13 -0.0254889000 _diffrn_orient_matrix_UB_21 -0.0382907000 _diffrn_orient_matrix_UB_22 -0.0065881000 _diffrn_orient_matrix_UB_23 -0.0103513000 _diffrn_orient_matrix_UB_31 -0.0030168000 _diffrn_orient_matrix_UB_32 0.0612570000 _diffrn_orient_matrix_UB_33 -0.0039979000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 4325 _reflns_number_total 5419 _reflns_odcompleteness_completeness 99.74 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.875 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.092 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 283 _refine_ls_number_reflns 5419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0420 _refine_ls_restrained_S_all 1.032 _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^)+(0.0327P)^2^+6.3357P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0824 _refine_ls_wR_factor_ref 0.0902 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15) 2.b Idealised Me refined as rotating group: C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C), C21(H21A,H21B, H21C), C22(H22A,H22B,H22C), C23(H23A,H23B,H23C), C25(H25A,H25B,H25C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 Se1 Se 0.07835(2) 0.45307(3) 0.30139(2) 0.02238(10) Uani 1 1 d . . . . . Se2 Se 0.05792(2) 0.73813(3) 0.19565(2) 0.02574(11) Uani 1 1 d . . . . . Fe1 Fe 0.0000 0.59991(5) 0.2500 0.01792(16) Uani 1 2 d S T P . . C1 C 0.15539(18) 0.5271(3) 0.34923(12) 0.0197(7) Uani 1 1 d . . . . . C2 C 0.2070(2) 0.4590(3) 0.38124(13) 0.0282(8) Uani 1 1 d . . . . . H2 H 0.2046 0.3779 0.3786 0.034 Uiso 1 1 calc R U . . . C3 C 0.2619(2) 0.5102(4) 0.41697(15) 0.0399(10) Uani 1 1 d . . . . . H3 H 0.2962 0.4632 0.4379 0.048 Uiso 1 1 calc R U . . . C4 C 0.2666(2) 0.6303(4) 0.42211(16) 0.0425(11) Uani 1 1 d . . . . . H4 H 0.3033 0.6646 0.4465 0.051 Uiso 1 1 calc R U . . . C5 C 0.2157(2) 0.6982(3) 0.39034(16) 0.0380(10) Uani 1 1 d . . . . . H5 H 0.2186 0.7792 0.3931 0.046 Uiso 1 1 calc R U . . . C6 C 0.1602(2) 0.6480(3) 0.35429(14) 0.0266(8) Uani 1 1 d . . . . . H6 H 0.1262 0.6954 0.3334 0.032 Uiso 1 1 calc R U . . . C7 C 0.10872(19) 0.6493(3) 0.14892(14) 0.0264(8) Uani 1 1 d . . . . . C8 C 0.1347(2) 0.7052(3) 0.10708(15) 0.0370(10) Uani 1 1 d . . . . . H8 H 0.1271 0.7852 0.1024 0.044 Uiso 1 1 calc R U . . . C9 C 0.1713(3) 0.6443(4) 0.07251(17) 0.0501(12) Uani 1 1 d . . . . . H9 H 0.1880 0.6834 0.0449 0.060 Uiso 1 1 calc R U . . . C10 C 0.1834(3) 0.5255(4) 0.07854(19) 0.0547(13) Uani 1 1 d . . . . . H10 H 0.2079 0.4843 0.0551 0.066 Uiso 1 1 calc R U . . . C11 C 0.1584(3) 0.4690(4) 0.11998(18) 0.0469(11) Uani 1 1 d . . . . . H11 H 0.1665 0.3891 0.1244 0.056 Uiso 1 1 calc R U . . . C12 C 0.1213(2) 0.5291(3) 0.15506(15) 0.0338(9) Uani 1 1 d . . . . . H12 H 0.1049 0.4894 0.1826 0.041 Uiso 1 1 calc R U . . . N1 N 0.13020(15) 1.0722(2) 0.29940(10) 0.0192(6) Uani 1 1 d . . . . . N2 N 0.08106(16) 1.0762(2) 0.37130(10) 0.0204(6) Uani 1 1 d . . . . . C13 C 0.10778(19) 1.1404(3) 0.33548(13) 0.0198(7) Uani 1 1 d . . . . . H13 H 0.1104 1.2216 0.3357 0.024 Uiso 1 1 calc R U . . . C14 C 0.1161(3) 0.9587(3) 0.31230(15) 0.0352(10) Uani 1 1 d . . . . . H14 H 0.1251 0.8923 0.2934 0.042 Uiso 1 1 calc R U . . . C15 C 0.0869(2) 0.9610(3) 0.35712(15) 0.0357(10) Uani 1 1 d . . . . . H15 H 0.0732 0.8964 0.3753 0.043 Uiso 1 1 calc R U . . . C16 C 0.15968(19) 1.1135(3) 0.25117(13) 0.0227(8) Uani 1 1 d . . . . . C17 C 0.2156(2) 1.2114(3) 0.26651(15) 0.0297(8) Uani 1 1 d . . . . . H17A H 0.1905 1.2772 0.2789 0.045 Uiso 1 1 calc R U . . . H17B H 0.2378 1.2342 0.2365 0.045 Uiso 1 1 calc R U . . . H17C H 0.2538 1.1845 0.2937 0.045 Uiso 1 1 calc R U . . . C18 C 0.0934(2) 1.1573(4) 0.21295(14) 0.0414(11) Uani 1 1 d . . . . . H18A H 0.0590 1.0942 0.2038 0.062 Uiso 1 1 calc R U . . . H18B H 0.1105 1.1863 0.1819 0.062 Uiso 1 1 calc R U . . . H18C H 0.0690 1.2189 0.2290 0.062 Uiso 1 1 calc R U . . . C19 C 0.1978(3) 1.0122(3) 0.22816(19) 0.0523(13) Uani 1 1 d . . . . . H19A H 0.2377 0.9837 0.2537 0.078 Uiso 1 1 calc R U . . . H19B H 0.2174 1.0381 0.1976 0.078 Uiso 1 1 calc R U . . . H19C H 0.1623 0.9507 0.2187 0.078 Uiso 1 1 calc R U . . . C20 C 0.0529(2) 1.1183(3) 0.41986(13) 0.0226(8) Uani 1 1 d . . . . . C21 C -0.0185(2) 1.0526(3) 0.42504(14) 0.0298(9) Uani 1 1 d . . . . . H21A H -0.0540 1.0638 0.3939 0.045 Uiso 1 1 calc R U . . . H21B H -0.0388 1.0816 0.4548 0.045 Uiso 1 1 calc R U . . . H21C H -0.0077 0.9707 0.4297 0.045 Uiso 1 1 calc R U . . . C22 C 0.1129(2) 1.0928(3) 0.46602(13) 0.0333(9) Uani 1 1 d . . . . . H22A H 0.1219 1.0101 0.4683 0.050 Uiso 1 1 calc R U . . . H22B H 0.0967 1.1195 0.4978 0.050 Uiso 1 1 calc R U . . . H22C H 0.1580 1.1326 0.4613 0.050 Uiso 1 1 calc R U . . . C23 C 0.0380(2) 1.2488(3) 0.41509(15) 0.0362(10) Uani 1 1 d . . . . . H23A H 0.0840 1.2893 0.4135 0.054 Uiso 1 1 calc R U . . . H23B H 0.0169 1.2754 0.4450 0.054 Uiso 1 1 calc R U . . . H23C H 0.0037 1.2642 0.3837 0.054 Uiso 1 1 calc R U . . . N3 N 0.0674(3) 0.7765(3) 0.46850(15) 0.0564(11) Uani 1 1 d . . . . . C24 C 0.0554(2) 0.6823(4) 0.45665(14) 0.0354(10) Uani 1 1 d . . . . . C25 C 0.0406(2) 0.5617(3) 0.44178(15) 0.0379(10) Uani 1 1 d . . . . . H25A H 0.0398 0.5534 0.4047 0.057 Uiso 1 1 calc R U . . . H25B H -0.0069 0.5389 0.4507 0.057 Uiso 1 1 calc R U . . . H25C H 0.0790 0.5128 0.4601 0.057 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0257(2) 0.01632(18) 0.02325(19) 0.00205(13) -0.00250(14) 0.00230(14) Se2 0.0278(2) 0.01939(19) 0.0297(2) 0.00230(14) 0.00301(15) -0.00325(15) Fe1 0.0181(4) 0.0164(3) 0.0181(4) 0.000 -0.0010(3) 0.000 C1 0.0168(17) 0.0258(18) 0.0168(17) 0.0019(14) 0.0043(14) 0.0013(14) C2 0.030(2) 0.032(2) 0.0219(19) 0.0044(15) 0.0018(16) 0.0030(17) C3 0.030(2) 0.052(3) 0.034(2) 0.0031(19) -0.0077(18) 0.011(2) C4 0.024(2) 0.060(3) 0.039(2) -0.011(2) -0.0092(19) -0.004(2) C5 0.028(2) 0.035(2) 0.050(3) -0.0086(19) 0.0025(19) -0.0061(18) C6 0.0192(19) 0.0271(19) 0.033(2) 0.0041(16) 0.0016(16) 0.0017(15) C7 0.0173(18) 0.036(2) 0.026(2) 0.0035(16) 0.0012(15) -0.0039(16) C8 0.032(2) 0.039(2) 0.040(2) 0.0126(19) 0.0062(19) -0.0004(19) C9 0.044(3) 0.069(3) 0.042(3) 0.018(2) 0.023(2) 0.010(2) C10 0.054(3) 0.066(3) 0.050(3) 0.001(2) 0.027(2) 0.018(3) C11 0.045(3) 0.043(2) 0.056(3) 0.005(2) 0.018(2) 0.014(2) C12 0.031(2) 0.037(2) 0.035(2) 0.0055(17) 0.0096(18) 0.0023(18) N1 0.0201(15) 0.0185(14) 0.0185(15) -0.0030(11) 0.0011(12) -0.0007(12) N2 0.0285(17) 0.0162(13) 0.0158(14) 0.0004(11) 0.0010(12) -0.0022(12) C13 0.0207(18) 0.0167(16) 0.0214(18) -0.0005(13) 0.0014(14) -0.0017(14) C14 0.063(3) 0.0176(18) 0.028(2) -0.0022(15) 0.015(2) 0.0004(18) C15 0.062(3) 0.0166(18) 0.030(2) 0.0002(15) 0.012(2) -0.0082(18) C16 0.0205(19) 0.0277(18) 0.0218(18) -0.0046(14) 0.0095(15) -0.0046(15) C17 0.024(2) 0.0309(19) 0.035(2) -0.0054(16) 0.0071(17) -0.0061(17) C18 0.041(3) 0.065(3) 0.018(2) 0.0032(19) -0.0001(18) -0.019(2) C19 0.064(3) 0.033(2) 0.071(3) -0.020(2) 0.046(3) -0.016(2) C20 0.028(2) 0.0230(17) 0.0173(17) 0.0004(14) 0.0040(15) -0.0013(15) C21 0.032(2) 0.036(2) 0.0217(19) 0.0058(16) 0.0052(16) -0.0011(17) C22 0.032(2) 0.047(2) 0.0184(19) 0.0000(17) -0.0039(16) -0.0068(19) C23 0.055(3) 0.030(2) 0.027(2) -0.0022(16) 0.019(2) 0.0031(19) N3 0.084(3) 0.040(2) 0.051(3) -0.0039(19) 0.027(2) 0.000(2) C24 0.048(3) 0.038(2) 0.023(2) 0.0003(17) 0.0148(18) 0.007(2) C25 0.047(3) 0.036(2) 0.033(2) -0.0028(17) 0.015(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 Fe1 2.4559(5) . ? Se1 C1 1.917(3) . ? Se2 Fe1 2.4522(5) . ? Se2 C7 1.915(4) . ? Fe1 Se1 2.4559(5) 2 ? Fe1 Se2 2.4522(5) 2 ? C1 C2 1.390(5) . ? C1 C6 1.391(5) . ? C2 C3 1.382(5) . ? C3 C4 1.382(6) . ? C4 C5 1.378(6) . ? C5 C6 1.387(5) . ? C7 C8 1.396(5) . ? C7 C12 1.400(5) . ? C8 C9 1.379(6) . ? C9 C10 1.381(6) . ? C10 C11 1.383(6) . ? C11 C12 1.387(5) . ? N1 C13 1.325(4) . ? N1 C14 1.374(4) . ? N1 C16 1.503(4) . ? N2 C13 1.328(4) . ? N2 C15 1.376(4) . ? N2 C20 1.502(4) . ? C14 C15 1.342(5) . ? C16 C17 1.522(5) . ? C16 C18 1.519(5) . ? C16 C19 1.516(5) . ? C20 C21 1.521(5) . ? C20 C22 1.516(5) . ? C20 C23 1.519(4) . ? N3 C24 1.133(5) . ? C24 C25 1.446(5) . ? 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 C1 Se1 Fe1 110.60(10) . . ? C7 Se2 Fe1 107.81(10) . . ? Se1 Fe1 Se1 93.68(3) 2 . ? Se2 Fe1 Se1 113.272(12) . 2 ? Se2 Fe1 Se1 119.150(12) 2 2 ? Se2 Fe1 Se1 119.150(12) . . ? Se2 Fe1 Se1 113.272(12) 2 . ? Se2 Fe1 Se2 99.69(3) . 2 ? C2 C1 Se1 119.7(3) . . ? C2 C1 C6 118.3(3) . . ? C6 C1 Se1 122.0(3) . . ? C3 C2 C1 120.8(3) . . ? C2 C3 C4 120.9(4) . . ? C5 C4 C3 118.5(4) . . ? C4 C5 C6 121.2(4) . . ? C5 C6 C1 120.2(3) . . ? C8 C7 Se2 119.6(3) . . ? C8 C7 C12 118.0(3) . . ? C12 C7 Se2 122.4(3) . . ? C9 C8 C7 121.3(4) . . ? C8 C9 C10 120.5(4) . . ? C9 C10 C11 118.8(4) . . ? C10 C11 C12 121.3(4) . . ? C11 C12 C7 120.0(4) . . ? C13 N1 C14 107.4(3) . . ? C13 N1 C16 125.5(3) . . ? C14 N1 C16 126.9(3) . . ? C13 N2 C15 107.1(3) . . ? C13 N2 C20 127.5(3) . . ? C15 N2 C20 125.4(3) . . ? N1 C13 N2 110.2(3) . . ? C15 C14 N1 107.6(3) . . ? C14 C15 N2 107.7(3) . . ? N1 C16 C17 108.8(3) . . ? N1 C16 C18 107.2(3) . . ? N1 C16 C19 108.9(3) . . ? C18 C16 C17 110.9(3) . . ? C19 C16 C17 109.8(3) . . ? C19 C16 C18 111.1(3) . . ? N2 C20 C21 108.4(3) . . ? N2 C20 C22 107.4(3) . . ? N2 C20 C23 109.1(3) . . ? C22 C20 C21 110.8(3) . . ? C22 C20 C23 110.6(3) . . ? C23 C20 C21 110.5(3) . . ? N3 C24 C25 179.5(6) . . ? _shelx_res_file ; TITL aral26 in C2/c #15 CELL 0.71073 18.132779 11.440603 25.799981 90 98.6548 90 ZERR 4 0.000688 0.000345 0.000942 0 0.0036 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N Fe Se UNIT 200 272 24 4 16 L.S. 4 0 0 PLAN 20 REM reset to C2/c #15 BOND fmap 2 acta SHEL 6 0.8 REM C:/XTAL%20DATA/aral26/aral26.hkl WGHT 0.032700 6.335701 FVAR 1.68484 SE1 5 0.078345 0.453069 0.301393 11.00000 0.02565 0.01632 = 0.02325 0.00205 -0.00250 0.00230 SE2 5 0.057924 0.738129 0.195650 11.00000 0.02778 0.01939 = 0.02965 0.00230 0.00301 -0.00325 FE1 4 0.000000 0.599909 0.250000 10.50000 0.01811 0.01642 = 0.01809 0.00000 -0.00104 0.00000 C1 1 0.155389 0.527083 0.349233 11.00000 0.01684 0.02583 = 0.01684 0.00190 0.00428 0.00127 C2 1 0.207019 0.458958 0.381235 11.00000 0.03008 0.03198 = 0.02190 0.00443 0.00177 0.00300 AFIX 43 H2 2 0.204558 0.377944 0.378552 11.00000 -1.20000 AFIX 0 C3 1 0.261936 0.510168 0.416975 11.00000 0.03017 0.05207 = 0.03357 0.00308 -0.00770 0.01067 AFIX 43 H3 2 0.296224 0.463184 0.437855 11.00000 -1.20000 AFIX 0 C4 1 0.266590 0.630334 0.422108 11.00000 0.02404 0.05992 = 0.03938 -0.01134 -0.00924 -0.00397 AFIX 43 H4 2 0.303256 0.664606 0.446463 11.00000 -1.20000 AFIX 0 C5 1 0.215697 0.698193 0.390337 11.00000 0.02823 0.03511 = 0.04969 -0.00862 0.00246 -0.00607 AFIX 43 H5 2 0.218578 0.779166 0.393116 11.00000 -1.20000 AFIX 0 C6 1 0.160244 0.648014 0.354286 11.00000 0.01916 0.02709 = 0.03286 0.00406 0.00158 0.00174 AFIX 43 H6 2 0.126187 0.695387 0.333418 11.00000 -1.20000 AFIX 0 C7 1 0.108718 0.649336 0.148919 11.00000 0.01726 0.03558 = 0.02567 0.00347 0.00117 -0.00391 C8 1 0.134686 0.705210 0.107080 11.00000 0.03172 0.03912 = 0.04026 0.01259 0.00616 -0.00038 AFIX 43 H8 2 0.127127 0.785162 0.102429 11.00000 -1.20000 AFIX 0 C9 1 0.171312 0.644272 0.072510 11.00000 0.04441 0.06948 = 0.04151 0.01826 0.02307 0.01032 AFIX 43 H9 2 0.188038 0.683448 0.044911 11.00000 -1.20000 AFIX 0 C10 1 0.183364 0.525524 0.078536 11.00000 0.05357 0.06649 = 0.04997 0.00088 0.02661 0.01764 AFIX 43 H10 2 0.207855 0.484292 0.055137 11.00000 -1.20000 AFIX 0 C11 1 0.158366 0.469002 0.119985 11.00000 0.04492 0.04331 = 0.05550 0.00534 0.01766 0.01434 AFIX 43 H11 2 0.166543 0.389136 0.124433 11.00000 -1.20000 AFIX 0 C12 1 0.121336 0.529072 0.155056 11.00000 0.03087 0.03679 = 0.03507 0.00545 0.00959 0.00227 AFIX 43 H12 2 0.104896 0.489442 0.182644 11.00000 -1.20000 AFIX 0 N1 3 0.130199 1.072174 0.299396 11.00000 0.02015 0.01852 = 0.01847 -0.00303 0.00111 -0.00075 N2 3 0.081059 1.076189 0.371300 11.00000 0.02847 0.01616 = 0.01583 0.00045 0.00101 -0.00222 C13 1 0.107780 1.140439 0.335476 11.00000 0.02070 0.01668 = 0.02137 -0.00048 0.00142 -0.00167 AFIX 43 H13 2 0.110380 1.221626 0.335687 11.00000 -1.20000 AFIX 0 C14 1 0.116090 0.958717 0.312296 11.00000 0.06272 0.01763 = 0.02780 -0.00221 0.01512 0.00038 AFIX 43 H14 2 0.125098 0.892342 0.293402 11.00000 -1.20000 AFIX 0 C15 1 0.086943 0.961046 0.357122 11.00000 0.06197 0.01664 = 0.03017 0.00023 0.01198 -0.00815 AFIX 43 H15 2 0.073192 0.896410 0.375329 11.00000 -1.20000 AFIX 0 C16 1 0.159676 1.113545 0.251166 11.00000 0.02053 0.02773 = 0.02181 -0.00461 0.00945 -0.00463 C17 1 0.215605 1.211385 0.266514 11.00000 0.02440 0.03093 = 0.03468 -0.00540 0.00707 -0.00608 AFIX 137 H17A 2 0.190511 1.277248 0.278944 11.00000 -1.50000 H17B 2 0.237781 1.234151 0.236529 11.00000 -1.50000 H17C 2 0.253793 1.184458 0.293745 11.00000 -1.50000 AFIX 0 C18 1 0.093443 1.157273 0.212948 11.00000 0.04073 0.06457 = 0.01763 0.00321 -0.00009 -0.01903 AFIX 137 H18A 2 0.059033 1.094195 0.203782 11.00000 -1.50000 H18B 2 0.110470 1.186313 0.181905 11.00000 -1.50000 H18C 2 0.068977 1.218939 0.229010 11.00000 -1.50000 AFIX 0 C19 1 0.197765 1.012205 0.228158 11.00000 0.06417 0.03289 = 0.07080 -0.02035 0.04580 -0.01571 AFIX 137 H19A 2 0.237741 0.983660 0.253664 11.00000 -1.50000 H19B 2 0.217389 1.038072 0.197568 11.00000 -1.50000 H19C 2 0.162289 0.950692 0.218667 11.00000 -1.50000 AFIX 0 C20 1 0.052876 1.118326 0.419860 11.00000 0.02786 0.02302 = 0.01725 0.00042 0.00402 -0.00130 C21 1 -0.018517 1.052558 0.425039 11.00000 0.03225 0.03581 = 0.02175 0.00579 0.00523 -0.00109 AFIX 137 H21A 2 -0.054047 1.063765 0.393888 11.00000 -1.50000 H21B 2 -0.038847 1.081635 0.454807 11.00000 -1.50000 H21C 2 -0.007731 0.970748 0.429692 11.00000 -1.50000 AFIX 0 C22 1 0.112889 1.092776 0.466024 11.00000 0.03166 0.04746 = 0.01843 0.00005 -0.00390 -0.00684 AFIX 137 H22A 2 0.121942 1.010123 0.468269 11.00000 -1.50000 H22B 2 0.096717 1.119470 0.497753 11.00000 -1.50000 H22C 2 0.158012 1.132554 0.461286 11.00000 -1.50000 AFIX 0 C23 1 0.037992 1.248811 0.415085 11.00000 0.05488 0.03044 = 0.02734 -0.00217 0.01938 0.00309 AFIX 137 H23A 2 0.083968 1.289346 0.413548 11.00000 -1.50000 H23B 2 0.016921 1.275372 0.444973 11.00000 -1.50000 H23C 2 0.003677 1.264196 0.383716 11.00000 -1.50000 AFIX 0 N3 3 0.067392 0.776492 0.468503 11.00000 0.08353 0.04001 = 0.05095 -0.00388 0.02684 0.00049 C24 1 0.055353 0.682291 0.456648 11.00000 0.04821 0.03840 = 0.02254 0.00031 0.01477 0.00743 C25 1 0.040562 0.561724 0.441777 11.00000 0.04743 0.03579 = 0.03325 -0.00282 0.01466 -0.00016 AFIX 137 H25A 2 0.039813 0.553409 0.404675 11.00000 -1.50000 H25B 2 -0.006902 0.538875 0.450695 11.00000 -1.50000 H25C 2 0.078956 0.512842 0.460087 11.00000 -1.50000 AFIX 0 HKLF 4 REM aral26 in C2/c #15 REM R1 = 0.0420 for 4325 Fo > 4sig(Fo) and 0.0598 for all 5419 data REM 283 parameters refined using 0 restraints END WGHT 0.0327 6.3359 REM Highest difference peak 0.875, deepest hole -0.744, 1-sigma level 0.092 Q1 1 0.0899 0.7389 0.3014 11.00000 0.05 0.87 Q2 1 0.1308 0.4583 0.2987 11.00000 0.05 0.73 Q3 1 0.0072 0.7346 0.1993 11.00000 0.05 0.65 Q4 1 0.0616 0.4428 0.1985 11.00000 0.05 0.60 Q5 1 0.0221 0.4693 0.3031 11.00000 0.05 0.57 Q6 1 0.0828 0.4035 0.2719 11.00000 0.05 0.54 Q7 1 0.0491 0.6168 0.2484 11.00000 0.05 0.54 Q8 1 0.1035 0.7083 0.1910 11.00000 0.05 0.51 Q9 1 0.0154 0.6156 0.2831 11.00000 0.05 0.46 Q10 1 0.0563 0.4990 0.3421 11.00000 0.05 0.45 Q11 1 0.0297 0.7375 0.1603 11.00000 0.05 0.44 Q12 1 0.0658 0.8026 0.1712 11.00000 0.05 0.43 Q13 1 0.0498 0.5596 0.2507 11.00000 0.05 0.42 Q14 1 0.0666 0.3963 0.3314 11.00000 0.05 0.41 Q15 1 0.0740 0.6808 0.1683 11.00000 0.05 0.40 Q16 1 0.0799 0.7153 0.2338 11.00000 0.05 0.39 Q17 1 0.0822 0.4991 0.2734 11.00000 0.05 0.39 Q18 1 0.0763 1.0801 0.1946 11.00000 0.05 0.37 Q19 1 -0.0118 0.7357 0.1542 11.00000 0.05 0.35 Q20 1 0.1411 0.4539 0.3412 11.00000 0.05 0.35 ; _shelx_res_checksum 46815 _shelx_hkl_file ; 0 0 -4 9019.36 501.960 3 0 0 -5 656.395 194.647 3 0 0 5 604.461 204.082 3 0 0 6 35579.8 1355.16 3 0 0 -6 35244.4 1310.18 3 0 0 -7 931.691 294.779 3 0 0 7 169.976 174.194 3 0 0 -8 345111. 7354.78 3 0 0 -9-80.3996 228.971 3 0 0 -10 137299. 3784.69 3 0 0 -11 236.560 286.646 3 0 0 -12 96824.2 3180.29 3 0 0 -13 32.5706 295.319 3 0 0 -14 957.184 405.103 3 0 0 -15 187.261 402.129 3 0 0 -16 103128. 3692.61 3 0 0 -17 1182.42 711.881 3 0 0 -18 432828. 10344.4 3 0 0 -19 3146.74 858.356 3 0 0 -20 190818. 5917.68 3 0 0 -21 2060.64 839.885 3 0 0 -22 109113. 4366.61 3 0 0 -23 759.099 576.271 3 0 0 -24 10970.9 1430.98 3 0 0 -25 2719.11 899.691 3 0 0 -26 75088.8 3818.80 3 0 0 -27 4279.87 1244.71 3 0 0 -28 26289.0 2342.83 3 0 0 -29 2376.26 1044.28 3 0 0 -30 11109.0 1746.52 3 0 0 -31 1585.46 1008.33 3 0 0 -32 3118.92 1167.10 3 0 0 -33 845.204 877.033 3 0 2 0 121857. 2834.40 1 0 -2 -1 366779. 7078.91 3 0 2 1 367261. 7097.44 3 0 2 -1 376919. 7340.48 1 0 2 1 364007. 7326.90 1 0 -2 1 381572. 7334.73 1 0 -2 -1 390373. 7342.93 1 0 -2 2 10744.1 571.548 1 0 2 2 9841.24 570.016 1 0 -2 -2 9926.15 545.285 1 0 2 2 9339.86 518.264 3 0 -2 -2 9421.08 512.604 3 0 2 -2 9191.86 545.756 1 0 -2 3 61075.6 1661.23 1 0 -2 -3 58571.6 1701.89 3 0 2 3 57642.3 1724.69 3 0 -2 -3 59245.0 1637.15 1 0 -2 3 61123.0 1444.35 2 0 2 -3 59515.0 1655.68 1 0 2 3 58522.8 1659.68 1 0 -2 4 24802.0 919.848 1 0 2 -4 23225.2 664.630 3 0 -2 -4 23410.4 1032.27 3 0 2 4 23533.0 918.470 1 0 -2 4 22434.2 694.240 3 0 2 -4 22529.1 889.075 1 0 -2 -4 23892.6 889.588 1 0 2 4 22648.4 1028.80 3 0 -2 -5 129293. 3258.20 3 0 -2 -5 135835. 2924.36 1 0 2 5 124354. 3269.17 3 0 2 -5 127205. 2924.99 1 0 2 -5 126924. 2710.13 3 0 -2 5 126050. 2765.44 3 0 -2 5 125289. 2917.81 1 0 2 5 125221. 2951.62 1 0 -2 6 2673.33 307.537 3 0 2 6 2487.11 295.618 1 0 2 -6 2527.36 296.929 1 0 -2 -6 2559.82 390.902 3 0 -2 -6 2595.76 282.654 1 0 2 -6 2556.73 270.433 3 0 -2 6 2882.05 305.498 1 0 2 -7 25370.1 1010.61 3 0 -2 7 26657.5 1071.48 3 0 -2 7 26542.9 964.726 1 0 2 7 27367.4 1015.72 1 0 -2 -7 27600.4 958.402 1 0 2 -7 27895.3 994.380 1 0 -2 -7 26220.6 1316.36 3 0 2 8 1729.66 253.057 1 0 -2 -8 2047.66 440.286 3 0 2 -8 1527.43 240.639 1 0 -2 8 1655.40 337.759 3 0 -2 -8 1662.31 217.705 1 0 -2 8 1929.79 248.792 1 0 2 -8 2080.30 316.112 3 0 2 9 60725.5 1697.46 1 0 2 -9 59942.7 1672.65 1 0 -2 -9 60143.2 2303.61 3 0 -2 9 58433.7 2007.77 3 0 2 -9 60420.9 1918.84 3 0 2 -10 20017.2 1063.98 3 0 2 -10 19705.4 809.469 1 0 2 10 18507.6 810.525 1 0 -2 -10 19648.9 1294.23 3 0 2 11 182844. 3999.90 1 0 -2 -11 191861. 5124.07 3 0 2 -11 191133. 3979.85 1 0 2 -11 184210. 4586.90 3 0 -2 -12-255.398 411.819 3 0 2 -12 241.704 270.991 3 0 -2 -13 17213.6 1335.51 3 0 2 -13 18091.4 1178.84 3 0 2 -14 31931.1 1627.79 3 0 -2 -14 29737.3 1861.14 3 0 2 -15 181.444 327.239 3 0 -2 -15 402.818 440.966 3 0 -2 -16 3900.98 724.451 3 0 2 -16 4444.14 660.670 3 0 -2 -17 1222.49 633.873 3 0 2 -17 1319.92 465.105 3 0 -2 -18 4234.55 903.529 3 0 2 -18 3539.25 674.708 3 0 2 -19 2032.77 552.486 3 0 -2 -19 1600.78 649.560 3 0 2 -20-26.3636 474.048 3 0 -2 -20 569.110 559.813 3 0 2 -21-544.803 534.806 3 0 -2 -21 371.657 628.204 3 0 -2 -22 9816.26 1377.32 3 0 2 -22 9757.45 1189.85 3 0 2 -23 12732.5 1366.53 3 0 -2 -23 10478.9 1451.91 3 0 2 -24 6927.61 1155.37 3 0 -2 -24 6530.28 1140.88 3 0 2 -25 4614.23 998.642 3 0 -2 -25 2419.14 861.182 3 0 -2 -26 765.017 762.697 3 0 2 -26 932.086 770.266 3 0 2 -27 8482.01 1284.93 3 0 -2 -27 7965.27 1390.88 3 0 -2 -28-344.497 746.862 3 0 2 -28 1527.58 839.110 3 0 -2 -29 19638.0 2218.55 3 0 2 -29 19269.2 1977.03 3 0 -2 -30 2048.12 1129.74 3 0 2 -30 1206.19 832.100 3 0 2 -31 4614.12 1187.80 3 0 -2 -31 2684.15 1211.27 3 0 2 -32 786.307 873.766 3 0 -2 -32 1720.52 1108.64 3 0 2 -33 4813.88 1241.36 3 0 4 0 252318. 5931.28 1 0 4 0 260728. 4972.12 2 0 4 0 260820. 5237.06 3 0 -4 0 255300. 5163.72 3 0 4 1 186874. 4756.57 1 0 4 1 199823. 3978.74 2 0 -4 1 192711. 3861.56 3 0 -4 -1 186557. 4196.50 3 0 4 -1 189279. 4764.28 1 0 4 -2 58597.8 2133.62 1 0 4 2 61687.0 2177.45 1 0 -4 -2 59361.4 1855.07 3 0 4 2 62882.7 1905.21 3 0 4 -3 43413.4 1744.70 1 0 4 3 42396.2 1760.27 1 0 -4 -3 41133.6 1540.39 3 0 4 3 42916.8 1588.26 3 0 -4 4 3510.21 262.734 2 0 4 -4 3263.19 466.984 1 0 4 4 4360.16 566.231 1 0 -4 -4 3678.38 475.658 3 0 4 5 62989.1 2268.30 1 0 4 -5 68552.2 2320.35 1 0 -4 5 67054.4 1732.92 2 0 -4 -5 69275.0 2308.60 3 0 -4 6 52664.8 1583.41 2 0 4 -6 53393.9 1984.68 1 0 4 6 51150.5 1991.34 1 0 -4 -6 52687.6 2035.45 3 0 -4 7 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-21 3 -5 11556.5 1934.52 2 -21 -3 -5 13385.9 1995.14 2 -21 -3 -6 1377.29 1068.83 2 -21 -3 -7 7936.33 1703.65 2 -21 5 10 1519.91 1013.55 2 -21 -5 9 6331.71 1407.25 2 -21 5 9 4401.70 1291.82 2 -21 -5 8 6811.45 1412.77 2 -21 5 8 5629.12 1519.36 2 -21 -5 7 1321.33 872.151 2 -21 5 7 992.279 968.361 2 -21 5 6 3912.76 1170.55 2 -21 -5 6 6090.48 1500.89 2 -21 5 5 178.314 882.092 2 -21 -5 5 808.528 927.576 2 -21 5 4 7574.21 1609.98 2 -21 -5 4 8290.97 1475.32 2 -21 5 3 2825.90 1124.07 2 -21 -5 3 2221.01 946.233 2 -21 5 2 3569.09 1284.49 2 -21 -5 2 292.018 828.222 2 -21 5 1 14413.6 2124.33 2 -21 -5 1 11789.7 1749.64 2 -21 5 0 3967.74 1257.93 2 -21 -5 0 1270.07 990.820 2 -21 5 -1 4973.22 1440.92 2 -21 -5 -1 5579.76 1380.70 2 -21 5 -2 1044.80 1132.96 2 -21 -5 -2 1884.39 1063.19 2 -21 -5 -3 435.908 880.027 2 -21 -5 -4 2626.85 1208.60 2 -21 -5 -5 796.324 1111.56 2 -21 -5 -6 366.972 1020.45 2 -21 -5 -7 3266.00 1255.06 2 -22 0 14 38604.6 3321.34 2 -22 0 13-793.532 824.926 2 -22 0 12 24726.8 2730.89 2 -22 0 11-170.364 966.703 2 -22 0 10-435.811 887.696 2 -22 0 9 269.111 888.222 2 -22 0 8 12739.6 2010.50 2 -22 0 7-195.148 923.261 2 -22 0 6 4597.65 1272.68 2 -22 0 5 1694.54 1243.65 2 -22 0 4 19832.7 2370.97 2 -22 0 3-253.333 883.667 2 -22 0 2 26111.4 2706.79 2 -22 0 1 707.089 1013.73 2 -22 0 0 4021.66 1418.17 2 -22 0 -1 723.105 941.284 2 -22 0 -2 19098.8 2367.97 2 -22 0 -3 1622.20 1409.78 2 -22 -2 15-321.915 985.432 2 -22 -2 14-347.126 1006.81 2 -22 -2 13 385.507 813.910 2 -22 -2 12 396.723 918.042 2 -22 2 11 1397.62 1063.03 2 -22 -2 11 3706.09 1243.47 2 -22 -2 10-1360.49 1129.83 2 -22 2 10-1700.23 1059.87 2 -22 -2 9-106.790 786.480 2 -22 2 9 61.9679 967.974 2 -22 -2 8-1106.61 951.153 2 -22 2 8 1474.94 923.444 2 -22 2 7 6057.45 1470.93 2 -22 -2 7 5607.26 1386.54 2 -22 2 6 875.238 987.343 2 -22 -2 6-244.623 843.810 2 -22 2 5 8965.70 1653.00 2 -22 -2 5 8427.16 1668.26 2 -22 2 4 733.656 960.217 2 -22 -2 4 4415.88 1351.04 2 -22 2 3 4363.43 1501.54 2 -22 -2 3 1407.43 1078.73 2 -22 2 2 535.464 869.329 2 -22 -2 2 1829.62 1195.32 2 -22 2 1 2677.00 1275.03 2 -22 -2 1 3387.64 1249.66 2 -22 2 0 1534.32 1089.20 2 -22 -2 0-1736.76 1130.37 2 -22 2 -1 1923.87 1096.05 2 -22 -2 -1-377.537 852.634 2 -22 -2 -2-437.599 1064.07 2 -22 -2 -3-322.384 911.154 2 -22 -4 16 880.238 946.834 2 -22 -4 15-677.992 844.478 2 -22 -4 14 6050.02 1420.15 2 -22 -4 13 4384.60 1337.46 2 -22 -4 12 4216.71 1308.23 2 -22 -4 11 730.780 1037.56 2 -22 -4 10 2186.78 1091.43 2 -22 -4 9 881.456 940.776 2 -22 -4 8 7107.91 1575.71 2 -22 -4 7 4530.29 1562.32 2 -22 -4 6 19072.7 2330.28 2 -22 -4 5 14271.7 2049.62 2 -22 -4 4 16539.4 2191.52 2 -22 -4 3 17269.5 2196.73 2 -22 -4 2 11972.4 1920.72 2 -22 -4 1 3895.74 1307.34 2 -22 -4 0 699.691 894.166 2 -22 -4 -1-294.496 943.352 2 -22 -4 -2 3220.82 1313.54 2 -22 -4 -3 5916.79 1503.12 2 -23 -1 6 694.668 1040.12 2 -23 -3 10 2615.65 1215.19 2 -23 -3 9 2484.53 1182.65 2 -23 -3 8 5327.27 1450.51 2 -23 -3 7 11075.0 1925.68 2 -23 -3 6 6960.21 2028.72 2 -23 -3 5 39654.3 3428.82 2 -23 -3 4 2435.11 1270.67 2 -23 -3 3 22278.1 2541.30 2 -23 -5 4 2927.09 1096.82 2 -23 -5 3 1268.29 944.940 2 0 0 0 0.00 0.00 0 TITL aral26 in C2/c REM C2/c (#15 in standard setting) CELL 0.71073 18.132779 11.440603 25.799981 90.0000 98.6548 90.0000 ZERR 11.00 0.000688 0.000345 0.000942 0.0000 0.0036 0.0000 LATT 7 SYMM -x, y,-z+1/2 SFAC C H N Fe Se UNIT 253.00 330.00 22.00 11.00 22.00 TREF HKLF 4 END ; _shelx_hkl_checksum 96622 _database_code_depnum_ccdc_archive 'CCDC 971588' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_aral62 _audit_creation_date 2013-11-12 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _shelxl_version_number 2013-2 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C39 H59 Fe N3 Se Si2' _chemical_formula_sum 'C39 H59 Fe N3 Se Si2' _chemical_formula_weight 760.88 _chemical_melting_point ? _chemical_oxdiff_formula Fe1Se1N3Si2C30H40 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5662(4) _cell_length_b 18.9572(5) _cell_length_c 17.9664(8) _cell_angle_alpha 90 _cell_angle_beta 107.200(4) _cell_angle_gamma 90 _cell_volume 4088.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3409 _cell_measurement_temperature 150.04(13) _cell_measurement_theta_max 27.9880 _cell_measurement_theta_min 3.1780 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.97010 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Colourless _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.236 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1608 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_unetI/netI 0.0799 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 13520 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.372 _diffrn_reflns_theta_min 3.421 _diffrn_ambient_temperature 150.04(13) _diffrn_detector_area_resol_mean 8.0714 _diffrn_measured_fraction_theta_full 0.9869 _diffrn_measured_fraction_theta_max 0.8372 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -7.00 89.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 20.8673 77.0000 -180.0000 96 #__ type_ start__ end____ width___ exp.time_ 2 omega -50.00 45.00 1.0000 5.0000 omega____ theta____ kappa____ phi______ frames - 20.8673 -57.0000 -30.0000 95 ; _diffrn_measurement_device_type 'SuperNova, Single source at offset, Eos' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0231952000 _diffrn_orient_matrix_UB_12 -0.0228078000 _diffrn_orient_matrix_UB_13 -0.0319895000 _diffrn_orient_matrix_UB_21 -0.0216208000 _diffrn_orient_matrix_UB_22 0.0295732000 _diffrn_orient_matrix_UB_23 -0.0238640000 _diffrn_orient_matrix_UB_31 0.0498577000 _diffrn_orient_matrix_UB_32 0.0022064000 _diffrn_orient_matrix_UB_33 -0.0107481000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5805 _reflns_number_total 8272 _reflns_odcompleteness_completeness 98.69 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.604 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.076 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 429 _refine_ls_number_reflns 8272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0870 _refine_ls_R_factor_gt 0.0539 _refine_ls_restrained_S_all 1.041 _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^)+(0.0252P)^2^+1.9201P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0912 _refine_ls_wR_factor_ref 0.1047 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C10(H10), C13(H13), C22(H22), C25(H25) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C18(H18), C19(H19), C20(H20), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33) 2.c Idealised Me refined as rotating group: C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C15(H15A,H15B, H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A, H27B,H27C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 Se1 Se 0.80387(3) 0.20250(2) 0.70627(3) 0.04679(15) Uani 1 1 d . . . . . Fe1 Fe 0.91942(4) 0.30754(2) 0.74141(3) 0.01878(12) Uani 1 1 d . . . . . Si1 Si 1.11443(7) 0.29785(5) 0.66695(6) 0.0231(2) Uani 1 1 d . . . . . Si2 Si 1.16291(7) 0.29598(5) 0.84410(6) 0.0238(2) Uani 1 1 d . . . . . N1 N 0.73408(19) 0.39802(13) 0.77911(15) 0.0142(6) Uani 1 1 d . . . . . N2 N 0.86571(19) 0.46733(13) 0.77369(15) 0.0145(6) Uani 1 1 d . . . . . N3 N 1.0760(2) 0.30260(13) 0.75099(16) 0.0194(6) Uani 1 1 d . . . . . C1 C 0.8342(2) 0.39817(16) 0.76358(18) 0.0140(7) Uani 1 1 d . . . . . C2 C 0.7055(2) 0.46433(16) 0.79792(19) 0.0181(7) Uani 1 1 d . . . . . H2 H 0.6412 0.4765 0.8105 0.022 Uiso 1 1 calc R U . . . C3 C 0.7876(2) 0.50795(17) 0.79477(19) 0.0192(7) Uani 1 1 d . . . . . H3 H 0.7915 0.5562 0.8048 0.023 Uiso 1 1 calc R U . . . C4 C 0.6569(2) 0.33893(16) 0.7649(2) 0.0170(7) Uani 1 1 d . . . . . C5 C 0.6519(2) 0.29727(16) 0.82756(19) 0.0187(7) Uani 1 1 d . . . . . C6 C 0.5769(3) 0.24112(18) 0.8120(2) 0.0256(8) Uani 1 1 d . . . . . H6 H 0.5716 0.2120 0.8524 0.031 Uiso 1 1 calc R U . . . C7 C 0.5100(3) 0.22842(19) 0.7367(2) 0.0291(9) Uani 1 1 d . . . . . H7 H 0.4614 0.1902 0.7267 0.035 Uiso 1 1 calc R U . . . C8 C 0.5153(3) 0.27191(18) 0.6770(2) 0.0283(9) Uani 1 1 d . . . . . H8 H 0.4687 0.2630 0.6271 0.034 Uiso 1 1 calc R U . . . C9 C 0.5881(2) 0.32884(17) 0.6885(2) 0.0211(8) Uani 1 1 d . . . . . C10 C 0.5887(3) 0.37858(19) 0.6223(2) 0.0266(8) Uani 1 1 d . . . . . H10 H 0.6513 0.4112 0.6417 0.032 Uiso 1 1 calc R U . . . C11 C 0.4823(3) 0.4223(2) 0.5986(3) 0.0520(12) Uani 1 1 d . . . . . H11A H 0.4197 0.3918 0.5769 0.078 Uiso 1 1 calc R U . . . H11B H 0.4871 0.4565 0.5604 0.078 Uiso 1 1 calc R U . . . H11C H 0.4731 0.4459 0.6435 0.078 Uiso 1 1 calc R U . . . C12 C 0.6053(4) 0.3403(2) 0.5525(3) 0.0580(13) Uani 1 1 d . . . . . H12A H 0.6720 0.3124 0.5687 0.087 Uiso 1 1 calc R U . . . H12B H 0.6118 0.3741 0.5143 0.087 Uiso 1 1 calc R U . . . H12C H 0.5427 0.3101 0.5302 0.087 Uiso 1 1 calc R U . . . C13 C 0.7187(3) 0.31417(18) 0.9112(2) 0.0272(8) Uani 1 1 d . . . . . H13 H 0.7767 0.3482 0.9098 0.033 Uiso 1 1 calc R U . . . C14 C 0.7757(3) 0.2486(2) 0.9550(2) 0.0403(10) Uani 1 1 d . . . . . H14A H 0.7203 0.2163 0.9614 0.061 Uiso 1 1 calc R U . . . H14B H 0.8237 0.2622 1.0052 0.061 Uiso 1 1 calc R U . . . H14C H 0.8190 0.2262 0.9257 0.061 Uiso 1 1 calc R U . . . C15 C 0.6428(3) 0.3486(2) 0.9529(2) 0.0377(10) Uani 1 1 d . . . . . H15A H 0.6106 0.3905 0.9255 0.057 Uiso 1 1 calc R U . . . H15B H 0.6853 0.3606 1.0051 0.057 Uiso 1 1 calc R U . . . H15C H 0.5846 0.3163 0.9543 0.057 Uiso 1 1 calc R U . . . C16 C 0.9616(2) 0.49844(15) 0.7565(2) 0.0169(7) Uani 1 1 d . . . . . C17 C 0.9555(3) 0.50940(16) 0.6784(2) 0.0191(7) Uani 1 1 d . . . . . C18 C 1.0465(3) 0.54136(16) 0.6637(2) 0.0248(8) Uani 1 1 d . . . . . H18 H 1.0456 0.5494 0.6124 0.030 Uiso 1 1 calc R U . . . C19 C 1.1389(3) 0.56156(17) 0.7240(2) 0.0251(8) Uani 1 1 d . . . . . H19 H 1.1999 0.5818 0.7129 0.030 Uiso 1 1 calc R U . . . C20 C 1.1407(3) 0.55175(17) 0.8000(2) 0.0249(8) Uani 1 1 d . . . . . H20 H 1.2028 0.5660 0.8398 0.030 Uiso 1 1 calc R U . . . C21 C 1.0512(2) 0.52093(16) 0.8187(2) 0.0187(7) Uani 1 1 d . . . . . C22 C 0.8517(3) 0.49063(19) 0.6119(2) 0.0271(8) Uani 1 1 d . . . . . H22 H 0.8227 0.4458 0.6251 0.032 Uiso 1 1 calc R U . . . C23 C 0.7605(3) 0.5470(2) 0.6035(2) 0.0462(11) Uani 1 1 d . . . . . H23A H 0.7448 0.5525 0.6524 0.069 Uiso 1 1 calc R U . . . H23B H 0.6940 0.5325 0.5643 0.069 Uiso 1 1 calc R U . . . H23C H 0.7858 0.5911 0.5887 0.069 Uiso 1 1 calc R U . . . C24 C 0.8730(3) 0.4815(2) 0.5330(2) 0.0453(11) Uani 1 1 d . . . . . H24A H 0.8932 0.5262 0.5159 0.068 Uiso 1 1 calc R U . . . H24B H 0.8067 0.4643 0.4956 0.068 Uiso 1 1 calc R U . . . H24C H 0.9325 0.4484 0.5379 0.068 Uiso 1 1 calc R U . . . C25 C 1.0507(3) 0.51954(16) 0.9032(2) 0.0217(8) Uani 1 1 d . . . . . H25 H 0.9913 0.4876 0.9071 0.026 Uiso 1 1 calc R U . . . C26 C 1.1604(3) 0.49403(18) 0.9603(2) 0.0325(9) Uani 1 1 d . . . . . H26A H 1.2194 0.5258 0.9590 0.049 Uiso 1 1 calc R U . . . H26B H 1.1773 0.4476 0.9456 0.049 Uiso 1 1 calc R U . . . H26C H 1.1533 0.4927 1.0120 0.049 Uiso 1 1 calc R U . . . C27 C 1.0239(3) 0.59384(18) 0.9271(2) 0.0306(9) Uani 1 1 d . . . . . H27A H 1.0815 0.6260 0.9242 0.046 Uiso 1 1 calc R U . . . H27B H 1.0194 0.5926 0.9795 0.046 Uiso 1 1 calc R U . . . H27C H 0.9539 0.6093 0.8926 0.046 Uiso 1 1 calc R U . . . C28 C 0.9044(3) 0.13457(17) 0.6844(2) 0.0294(9) Uani 1 1 d . . . . . C29 C 0.8899(3) 0.11380(19) 0.6075(3) 0.0372(10) Uani 1 1 d . . . . . H29 H 0.8343 0.1345 0.5674 0.045 Uiso 1 1 calc R U . . . C30 C 0.9577(3) 0.0628(2) 0.5906(3) 0.0477(12) Uani 1 1 d . . . . . H30 H 0.9476 0.0496 0.5391 0.057 Uiso 1 1 calc R U . . . C31 C 1.0397(3) 0.0313(2) 0.6489(3) 0.0504(13) Uani 1 1 d . . . . . H31 H 1.0847 -0.0032 0.6371 0.060 Uiso 1 1 calc R U . . . C32 C 1.0549(3) 0.0509(2) 0.7249(3) 0.0456(12) Uani 1 1 d . . . . . H32 H 1.1103 0.0295 0.7646 0.055 Uiso 1 1 calc R U . . . C33 C 0.9875(3) 0.1030(2) 0.7431(3) 0.0373(10) Uani 1 1 d . . . . . H33 H 0.9986 0.1163 0.7946 0.045 Uiso 1 1 calc R U . . . C34 C 0.9879(3) 0.2958(2) 0.5795(2) 0.0381(10) Uani 1 1 d . . . . . H34A H 0.9508 0.2512 0.5774 0.057 Uiso 1 1 calc R U . . . H34B H 1.0100 0.3020 0.5332 0.057 Uiso 1 1 calc R U . . . H34C H 0.9382 0.3332 0.5834 0.057 Uiso 1 1 calc R U . . . C35 C 1.2031(3) 0.37401(19) 0.6541(2) 0.0411(11) Uani 1 1 d . . . . . H35A H 1.1682 0.4175 0.6611 0.062 Uiso 1 1 calc R U . . . H35B H 1.2113 0.3726 0.6027 0.062 Uiso 1 1 calc R U . . . H35C H 1.2752 0.3708 0.6920 0.062 Uiso 1 1 calc R U . . . C36 C 1.1961(3) 0.21609(18) 0.6640(2) 0.0305(9) Uani 1 1 d . . . . . H36A H 1.2615 0.2152 0.7083 0.046 Uiso 1 1 calc R U . . . H36B H 1.2178 0.2156 0.6171 0.046 Uiso 1 1 calc R U . . . H36C H 1.1511 0.1754 0.6652 0.046 Uiso 1 1 calc R U . . . C37 C 1.0785(3) 0.31372(19) 0.9129(2) 0.0290(9) Uani 1 1 d . . . . . H37A H 1.0429 0.3589 0.9012 0.043 Uiso 1 1 calc R U . . . H37B H 1.1267 0.3137 0.9655 0.043 Uiso 1 1 calc R U . . . H37C H 1.0230 0.2777 0.9070 0.043 Uiso 1 1 calc R U . . . C38 C 1.2834(3) 0.3593(2) 0.8621(2) 0.0424(11) Uani 1 1 d . . . . . H38A H 1.3296 0.3465 0.8301 0.064 Uiso 1 1 calc R U . . . H38B H 1.3265 0.3574 0.9159 0.064 Uiso 1 1 calc R U . . . H38C H 1.2556 0.4063 0.8493 0.064 Uiso 1 1 calc R U . . . C39 C 1.2281(3) 0.20690(19) 0.8726(2) 0.0419(11) Uani 1 1 d . . . . . H39A H 1.1709 0.1715 0.8620 0.063 Uiso 1 1 calc R U . . . H39B H 1.2677 0.2068 0.9272 0.063 Uiso 1 1 calc R U . . . H39C H 1.2789 0.1970 0.8432 0.063 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0285(2) 0.0211(2) 0.0994(4) -0.0212(2) 0.0322(2) -0.00764(17) Fe1 0.0175(2) 0.0140(2) 0.0268(3) -0.0033(2) 0.0096(2) 0.00021(19) Si1 0.0236(5) 0.0209(5) 0.0278(6) 0.0028(5) 0.0123(4) 0.0036(4) Si2 0.0216(5) 0.0220(5) 0.0268(6) -0.0060(4) 0.0054(4) 0.0016(4) N1 0.0119(13) 0.0129(13) 0.0168(15) -0.0013(12) 0.0028(11) -0.0002(11) N2 0.0141(13) 0.0114(13) 0.0177(15) 0.0001(11) 0.0043(11) 0.0007(10) N3 0.0185(13) 0.0181(14) 0.0240(16) -0.0047(13) 0.0101(12) 0.0018(12) C1 0.0142(15) 0.0144(16) 0.0112(17) 0.0026(13) 0.0006(13) -0.0008(13) C2 0.0176(16) 0.0157(17) 0.0230(19) -0.0022(15) 0.0090(15) 0.0021(14) C3 0.0203(17) 0.0122(16) 0.026(2) -0.0013(14) 0.0077(15) 0.0039(13) C4 0.0112(15) 0.0142(16) 0.026(2) -0.0002(14) 0.0065(14) 0.0002(13) C5 0.0175(16) 0.0178(17) 0.0200(18) -0.0017(15) 0.0045(14) -0.0009(14) C6 0.0240(18) 0.0217(18) 0.031(2) 0.0049(16) 0.0084(16) -0.0053(15) C7 0.0199(18) 0.0249(19) 0.040(2) -0.0044(18) 0.0053(17) -0.0108(15) C8 0.0226(18) 0.030(2) 0.027(2) -0.0091(17) -0.0014(16) -0.0083(16) C9 0.0170(17) 0.0240(18) 0.022(2) -0.0046(15) 0.0057(15) -0.0027(14) C10 0.0232(18) 0.032(2) 0.021(2) 0.0031(17) 0.0012(16) -0.0066(16) C11 0.049(3) 0.059(3) 0.047(3) 0.028(2) 0.012(2) 0.014(2) C12 0.083(3) 0.059(3) 0.039(3) 0.000(2) 0.029(3) -0.001(3) C13 0.0302(19) 0.0267(19) 0.021(2) 0.0029(16) 0.0010(16) -0.0114(16) C14 0.041(2) 0.042(2) 0.031(2) 0.009(2) -0.0013(19) 0.0022(19) C15 0.053(2) 0.035(2) 0.025(2) -0.0012(19) 0.0112(19) -0.002(2) C16 0.0149(16) 0.0098(15) 0.028(2) 0.0009(14) 0.0093(14) 0.0009(13) C17 0.0232(17) 0.0107(16) 0.026(2) 0.0034(14) 0.0110(15) -0.0008(13) C18 0.0293(19) 0.0175(17) 0.032(2) 0.0043(16) 0.0151(17) -0.0005(15) C19 0.0224(18) 0.0165(17) 0.043(2) 0.0013(17) 0.0199(18) -0.0044(14) C20 0.0175(17) 0.0164(17) 0.039(2) 0.0010(17) 0.0059(16) -0.0024(14) C21 0.0195(17) 0.0121(16) 0.025(2) 0.0034(14) 0.0070(15) 0.0035(13) C22 0.034(2) 0.0271(19) 0.021(2) 0.0047(16) 0.0098(17) -0.0030(16) C23 0.033(2) 0.059(3) 0.039(3) 0.010(2) -0.001(2) 0.005(2) C24 0.060(3) 0.051(3) 0.025(2) 0.005(2) 0.014(2) -0.011(2) C25 0.0220(17) 0.0163(17) 0.025(2) -0.0003(15) 0.0045(15) -0.0052(14) C26 0.031(2) 0.0233(19) 0.037(2) -0.0004(18) 0.0003(18) -0.0033(16) C27 0.040(2) 0.028(2) 0.025(2) -0.0071(17) 0.0101(17) 0.0010(17) C28 0.0179(18) 0.0151(17) 0.057(3) -0.0082(18) 0.0132(18) -0.0060(14) C29 0.033(2) 0.025(2) 0.052(3) -0.006(2) 0.010(2) -0.0017(17) C30 0.054(3) 0.034(2) 0.066(3) -0.015(2) 0.035(3) -0.005(2) C31 0.031(2) 0.022(2) 0.109(4) -0.011(3) 0.038(3) -0.0014(18) C32 0.020(2) 0.031(2) 0.080(4) 0.013(2) 0.006(2) -0.0056(17) C33 0.024(2) 0.034(2) 0.053(3) -0.007(2) 0.0101(19) -0.0126(18) C34 0.039(2) 0.047(2) 0.027(2) 0.004(2) 0.0083(18) 0.009(2) C35 0.042(2) 0.029(2) 0.062(3) 0.007(2) 0.030(2) -0.0005(18) C36 0.035(2) 0.029(2) 0.032(2) -0.0008(17) 0.0160(18) 0.0056(16) C37 0.034(2) 0.033(2) 0.020(2) -0.0020(17) 0.0079(16) -0.0010(17) C38 0.029(2) 0.052(3) 0.043(3) -0.017(2) 0.0069(19) -0.0099(19) C39 0.047(2) 0.034(2) 0.035(2) -0.007(2) -0.003(2) 0.0183(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 Fe1 2.4351(6) . ? Se1 C28 1.925(3) . ? Fe1 N3 1.926(2) . ? Fe1 C1 2.124(3) . ? Si1 N3 1.718(3) . ? Si1 C34 1.876(3) . ? Si1 C35 1.880(4) . ? Si1 C36 1.869(3) . ? Si2 N3 1.711(3) . ? Si2 C37 1.881(4) . ? Si2 C38 1.884(4) . ? Si2 C39 1.881(3) . ? N1 C1 1.367(4) . ? N1 C2 1.377(4) . ? N1 C4 1.454(4) . ? N2 C1 1.366(4) . ? N2 C3 1.386(4) . ? N2 C16 1.455(4) . ? C2 C3 1.336(4) . ? C4 C5 1.392(4) . ? C4 C9 1.402(4) . ? C5 C6 1.395(4) . ? C5 C13 1.523(4) . ? C6 C7 1.385(5) . ? C7 C8 1.371(5) . ? C8 C9 1.390(4) . ? C9 C10 1.519(5) . ? C10 C11 1.522(5) . ? C10 C12 1.517(5) . ? C13 C14 1.530(5) . ? C13 C15 1.523(5) . ? C16 C17 1.397(5) . ? C16 C21 1.398(4) . ? C17 C18 1.387(4) . ? C17 C22 1.528(4) . ? C18 C19 1.388(4) . ? C19 C20 1.370(5) . ? C20 C21 1.393(4) . ? C21 C25 1.520(5) . ? C22 C23 1.541(5) . ? C22 C24 1.529(5) . ? C25 C26 1.533(4) . ? C25 C27 1.539(4) . ? C28 C29 1.395(5) . ? C28 C33 1.382(5) . ? C29 C30 1.380(5) . ? C30 C31 1.370(6) . ? C31 C32 1.373(6) . ? C32 C33 1.400(5) . ? 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 C28 Se1 Fe1 102.88(9) . . ? N3 Fe1 Se1 119.90(8) . . ? N3 Fe1 C1 125.53(11) . . ? C1 Fe1 Se1 114.52(8) . . ? N3 Si1 C34 110.36(15) . . ? N3 Si1 C35 113.49(16) . . ? N3 Si1 C36 111.58(15) . . ? C34 Si1 C35 107.44(18) . . ? C36 Si1 C34 107.23(17) . . ? C36 Si1 C35 106.43(17) . . ? N3 Si2 C37 107.95(14) . . ? N3 Si2 C38 111.66(16) . . ? N3 Si2 C39 115.66(15) . . ? C37 Si2 C38 110.74(17) . . ? C39 Si2 C37 105.45(18) . . ? C39 Si2 C38 105.21(18) . . ? C1 N1 C2 111.8(2) . . ? C1 N1 C4 124.9(3) . . ? C2 N1 C4 122.5(2) . . ? C1 N2 C3 111.6(3) . . ? C1 N2 C16 125.9(3) . . ? C3 N2 C16 122.1(2) . . ? Si1 N3 Fe1 117.98(14) . . ? Si2 N3 Fe1 115.53(15) . . ? Si2 N3 Si1 126.26(15) . . ? N1 C1 Fe1 125.6(2) . . ? N2 C1 Fe1 131.2(2) . . ? N2 C1 N1 102.9(3) . . ? C3 C2 N1 107.1(3) . . ? C2 C3 N2 106.6(3) . . ? C5 C4 N1 118.8(3) . . ? C5 C4 C9 123.5(3) . . ? C9 C4 N1 117.6(3) . . ? C4 C5 C6 117.4(3) . . ? C4 C5 C13 122.4(3) . . ? C6 C5 C13 120.1(3) . . ? C7 C6 C5 120.5(3) . . ? C8 C7 C6 120.3(3) . . ? C7 C8 C9 122.1(3) . . ? C4 C9 C10 122.5(3) . . ? C8 C9 C4 116.1(3) . . ? C8 C9 C10 121.3(3) . . ? C9 C10 C11 110.5(3) . . ? C12 C10 C9 112.6(3) . . ? C12 C10 C11 110.7(3) . . ? C5 C13 C14 111.9(3) . . ? C15 C13 C5 109.4(3) . . ? C15 C13 C14 111.2(3) . . ? C17 C16 N2 118.1(3) . . ? C17 C16 C21 123.3(3) . . ? C21 C16 N2 118.4(3) . . ? C16 C17 C22 122.0(3) . . ? C18 C17 C16 117.0(3) . . ? C18 C17 C22 120.9(3) . . ? C17 C18 C19 121.1(3) . . ? C20 C19 C18 120.3(3) . . ? C19 C20 C21 121.4(3) . . ? C16 C21 C25 123.6(3) . . ? C20 C21 C16 116.8(3) . . ? C20 C21 C25 119.4(3) . . ? C17 C22 C23 110.7(3) . . ? C17 C22 C24 114.0(3) . . ? C24 C22 C23 108.5(3) . . ? C21 C25 C26 113.9(3) . . ? C21 C25 C27 109.2(3) . . ? C26 C25 C27 109.3(3) . . ? C29 C28 Se1 119.3(3) . . ? C33 C28 Se1 121.8(3) . . ? C33 C28 C29 118.8(3) . . ? C30 C29 C28 120.4(4) . . ? C31 C30 C29 120.7(4) . . ? C30 C31 C32 119.6(4) . . ? C31 C32 C33 120.5(4) . . ? C28 C33 C32 120.0(4) . . ? _shelx_res_file ; TITL aral62 in P21/n #14 CELL 0.71073 12.566197 18.957195 17.966391 90 107.2003 90 ZERR 4 0.00041 0.000524 0.000818 0 0.0041 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N Si Fe Se UNIT 156 236 12 8 4 4 L.S. 5 PLAN 20 SHEL6 0.8 REM reset to P21/n #14 BOND fmap 2 acta REM C:/XTAL%20DATA/aral62%20-%20solution%20Fe(HMDS)(SePh)IPr/aral62.hkl WGHT 0.025200 1.920100 FVAR 3.02618 SE1 6 0.803872 0.202498 0.706273 11.00000 0.02850 0.02111 = 0.09935 -0.02116 0.03219 -0.00764 FE1 5 0.919416 0.307536 0.741411 11.00000 0.01754 0.01402 = 0.02677 -0.00331 0.00960 0.00021 SI1 4 1.114426 0.297847 0.666947 11.00000 0.02364 0.02093 = 0.02775 0.00281 0.01230 0.00360 SI2 4 1.162913 0.295978 0.844103 11.00000 0.02158 0.02196 = 0.02677 -0.00598 0.00536 0.00157 N1 3 0.734077 0.398018 0.779105 11.00000 0.01194 0.01288 = 0.01683 -0.00127 0.00283 -0.00017 N2 3 0.865712 0.467330 0.773689 11.00000 0.01410 0.01144 = 0.01767 0.00011 0.00434 0.00069 N3 3 1.075999 0.302605 0.750995 11.00000 0.01852 0.01809 = 0.02403 -0.00474 0.01006 0.00177 C1 1 0.834176 0.398171 0.763583 11.00000 0.01423 0.01442 = 0.01121 0.00256 0.00057 -0.00081 C2 1 0.705517 0.464326 0.797918 11.00000 0.01758 0.01571 = 0.02303 -0.00216 0.00898 0.00206 AFIX 43 H2 2 0.641192 0.476472 0.810461 11.00000 -1.20000 AFIX 0 C3 1 0.787575 0.507954 0.794773 11.00000 0.02026 0.01222 = 0.02562 -0.00129 0.00773 0.00394 AFIX 43 H3 2 0.791495 0.556168 0.804777 11.00000 -1.20000 AFIX 0 C4 1 0.656897 0.338928 0.764894 11.00000 0.01119 0.01421 = 0.02627 -0.00020 0.00647 0.00021 C5 1 0.651941 0.297270 0.827565 11.00000 0.01752 0.01782 = 0.02005 -0.00167 0.00455 -0.00092 C6 1 0.576868 0.241122 0.811978 11.00000 0.02399 0.02173 = 0.03123 0.00487 0.00845 -0.00530 AFIX 43 H6 2 0.571633 0.211992 0.852398 11.00000 -1.20000 AFIX 0 C7 1 0.510045 0.228418 0.736749 11.00000 0.01990 0.02495 = 0.04024 -0.00435 0.00527 -0.01081 AFIX 43 H7 2 0.461404 0.190234 0.726748 11.00000 -1.20000 AFIX 0 C8 1 0.515325 0.271911 0.676973 11.00000 0.02259 0.03003 = 0.02678 -0.00906 -0.00140 -0.00835 AFIX 43 H8 2 0.468709 0.263026 0.627064 11.00000 -1.20000 AFIX 0 C9 1 0.588079 0.328845 0.688541 11.00000 0.01704 0.02403 = 0.02219 -0.00456 0.00574 -0.00270 C10 1 0.588672 0.378582 0.622347 11.00000 0.02319 0.03243 = 0.02091 0.00314 0.00125 -0.00658 AFIX 13 H10 2 0.651295 0.411187 0.641712 11.00000 -1.20000 AFIX 0 C11 1 0.482328 0.422255 0.598580 11.00000 0.04892 0.05916 = 0.04687 0.02818 0.01248 0.01398 AFIX 137 H11A 2 0.419729 0.391845 0.576906 11.00000 -1.50000 H11B 2 0.487110 0.456524 0.560359 11.00000 -1.50000 H11C 2 0.473064 0.445945 0.643482 11.00000 -1.50000 AFIX 0 C12 1 0.605336 0.340278 0.552497 11.00000 0.08297 0.05886 = 0.03934 -0.00002 0.02934 -0.00134 AFIX 137 H12A 2 0.672041 0.312441 0.568742 11.00000 -1.50000 H12B 2 0.611822 0.374095 0.514303 11.00000 -1.50000 H12C 2 0.542690 0.310058 0.530246 11.00000 -1.50000 AFIX 0 C13 1 0.718723 0.314165 0.911231 11.00000 0.03016 0.02673 = 0.02055 0.00286 0.00099 -0.01141 AFIX 13 H13 2 0.776738 0.348237 0.909804 11.00000 -1.20000 AFIX 0 C14 1 0.775728 0.248612 0.954966 11.00000 0.04087 0.04176 = 0.03069 0.00872 -0.00130 0.00217 AFIX 137 H14A 2 0.720261 0.216342 0.961446 11.00000 -1.50000 H14B 2 0.823684 0.262182 1.005176 11.00000 -1.50000 H14C 2 0.818997 0.226190 0.925711 11.00000 -1.50000 AFIX 0 C15 1 0.642769 0.348575 0.952904 11.00000 0.05312 0.03450 = 0.02531 -0.00120 0.01116 -0.00223 AFIX 137 H15A 2 0.610556 0.390549 0.925496 11.00000 -1.50000 H15B 2 0.685312 0.360583 1.005138 11.00000 -1.50000 H15C 2 0.584565 0.316282 0.954345 11.00000 -1.50000 AFIX 0 C16 1 0.961595 0.498444 0.756479 11.00000 0.01492 0.00975 = 0.02783 0.00087 0.00930 0.00093 C17 1 0.955547 0.509404 0.678417 11.00000 0.02321 0.01071 = 0.02581 0.00337 0.01102 -0.00078 C18 1 1.046513 0.541364 0.663652 11.00000 0.02930 0.01755 = 0.03150 0.00427 0.01506 -0.00052 AFIX 43 H18 2 1.045590 0.549404 0.612402 11.00000 -1.20000 AFIX 0 C19 1 1.138915 0.561564 0.724043 11.00000 0.02235 0.01655 = 0.04290 0.00126 0.01987 -0.00435 AFIX 43 H19 2 1.199884 0.581835 0.712936 11.00000 -1.20000 AFIX 0 C20 1 1.140650 0.551753 0.799960 11.00000 0.01753 0.01643 = 0.03927 0.00100 0.00590 -0.00235 AFIX 43 H20 2 1.202825 0.565967 0.839816 11.00000 -1.20000 AFIX 0 C21 1 1.051226 0.520933 0.818688 11.00000 0.01954 0.01206 = 0.02480 0.00342 0.00700 0.00354 C22 1 0.851654 0.490628 0.611930 11.00000 0.03415 0.02707 = 0.02103 0.00465 0.00982 -0.00297 AFIX 13 H22 2 0.822664 0.445842 0.625091 11.00000 -1.20000 AFIX 0 C23 1 0.760484 0.546993 0.603515 11.00000 0.03290 0.05938 = 0.03907 0.00987 -0.00061 0.00509 AFIX 137 H23A 2 0.744833 0.552521 0.652352 11.00000 -1.50000 H23B 2 0.694030 0.532476 0.564294 11.00000 -1.50000 H23C 2 0.785793 0.591095 0.588657 11.00000 -1.50000 AFIX 0 C24 1 0.873021 0.481526 0.532983 11.00000 0.05992 0.05118 = 0.02543 0.00528 0.01373 -0.01142 AFIX 137 H24A 2 0.893217 0.526172 0.515857 11.00000 -1.50000 H24B 2 0.806715 0.464260 0.495594 11.00000 -1.50000 H24C 2 0.932545 0.448432 0.537941 11.00000 -1.50000 AFIX 0 C25 1 1.050740 0.519536 0.903185 11.00000 0.02201 0.01626 = 0.02507 -0.00032 0.00445 -0.00519 AFIX 13 H25 2 0.991318 0.487588 0.907103 11.00000 -1.20000 AFIX 0 C26 1 1.160449 0.494034 0.960266 11.00000 0.03114 0.02328 = 0.03683 -0.00037 0.00032 -0.00328 AFIX 137 H26A 2 1.219366 0.525800 0.958961 11.00000 -1.50000 H26B 2 1.177339 0.447630 0.945584 11.00000 -1.50000 H26C 2 1.153347 0.492701 1.012001 11.00000 -1.50000 AFIX 0 C27 1 1.023858 0.593838 0.927118 11.00000 0.03982 0.02756 = 0.02486 -0.00706 0.01011 0.00098 AFIX 137 H27A 2 1.081545 0.625954 0.924177 11.00000 -1.50000 H27B 2 1.019394 0.592620 0.979529 11.00000 -1.50000 H27C 2 0.953868 0.609284 0.892576 11.00000 -1.50000 AFIX 0 C28 1 0.904436 0.134571 0.684368 11.00000 0.01788 0.01506 = 0.05659 -0.00819 0.01324 -0.00597 C29 1 0.889943 0.113798 0.607496 11.00000 0.03275 0.02539 = 0.05190 -0.00610 0.01001 -0.00165 AFIX 43 H29 2 0.834255 0.134470 0.567355 11.00000 -1.20000 AFIX 0 C30 1 0.957709 0.062771 0.590632 11.00000 0.05403 0.03433 = 0.06573 -0.01532 0.03480 -0.00480 AFIX 43 H30 2 0.947612 0.049640 0.539128 11.00000 -1.20000 AFIX 0 C31 1 1.039674 0.031258 0.648928 11.00000 0.03115 0.02206 = 0.10916 -0.01131 0.03807 -0.00143 AFIX 43 H31 2 1.084748 -0.003245 0.637104 11.00000 -1.20000 AFIX 0 C32 1 1.054871 0.050923 0.724914 11.00000 0.02033 0.03053 = 0.08050 0.01286 0.00642 -0.00562 AFIX 43 H32 2 1.110319 0.029521 0.764612 11.00000 -1.20000 AFIX 0 C33 1 0.987483 0.102967 0.743055 11.00000 0.02404 0.03394 = 0.05323 -0.00690 0.01014 -0.01261 AFIX 43 H33 2 0.998621 0.116271 0.794623 11.00000 -1.20000 AFIX 0 C34 1 0.987890 0.295807 0.579533 11.00000 0.03941 0.04702 = 0.02681 0.00420 0.00834 0.00908 AFIX 137 H34A 2 0.950793 0.251249 0.577362 11.00000 -1.50000 H34B 2 1.009953 0.301976 0.533151 11.00000 -1.50000 H34C 2 0.938174 0.333153 0.583354 11.00000 -1.50000 AFIX 0 C35 1 1.203139 0.374013 0.654093 11.00000 0.04222 0.02913 = 0.06157 0.00679 0.03009 -0.00050 AFIX 137 H35A 2 1.168229 0.417530 0.661111 11.00000 -1.50000 H35B 2 1.211321 0.372616 0.602654 11.00000 -1.50000 H35C 2 1.275173 0.370794 0.691951 11.00000 -1.50000 AFIX 0 C36 1 1.196146 0.216089 0.664033 11.00000 0.03464 0.02888 = 0.03188 -0.00078 0.01602 0.00557 AFIX 137 H36A 2 1.261500 0.215231 0.708332 11.00000 -1.50000 H36B 2 1.217781 0.215608 0.617069 11.00000 -1.50000 H36C 2 1.151143 0.175422 0.665199 11.00000 -1.50000 AFIX 0 C37 1 1.078537 0.313720 0.912871 11.00000 0.03378 0.03317 = 0.01997 -0.00199 0.00790 -0.00099 AFIX 137 H37A 2 1.042853 0.358856 0.901189 11.00000 -1.50000 H37B 2 1.126679 0.313696 0.965495 11.00000 -1.50000 H37C 2 1.023020 0.277664 0.907025 11.00000 -1.50000 AFIX 0 C38 1 1.283417 0.359306 0.862061 11.00000 0.02925 0.05206 = 0.04330 -0.01667 0.00693 -0.00995 AFIX 137 H38A 2 1.329570 0.346482 0.830120 11.00000 -1.50000 H38B 2 1.326473 0.357389 0.915949 11.00000 -1.50000 H38C 2 1.255612 0.406315 0.849264 11.00000 -1.50000 AFIX 0 C39 1 1.228092 0.206900 0.872614 11.00000 0.04664 0.03450 = 0.03485 -0.00703 -0.00302 0.01830 AFIX 137 H39A 2 1.170924 0.171505 0.861959 11.00000 -1.50000 H39B 2 1.267721 0.206762 0.927222 11.00000 -1.50000 H39C 2 1.278902 0.196960 0.843216 11.00000 -1.50000 AFIX 0 HKLF 4 REM aral62 in P21/n #14 REM R1 = 0.0539 for 5805 Fo > 4sig(Fo) and 0.0870 for all 8272 data REM 429 parameters refined using 0 restraints END WGHT 0.0252 1.9200 REM Highest difference peak 0.604, deepest hole -0.775, 1-sigma level 0.076 Q1 1 0.8574 0.1940 0.7574 11.00000 0.05 0.60 Q2 1 1.1571 0.3429 0.6630 11.00000 0.05 0.41 Q3 1 0.6183 0.2608 0.8054 11.00000 0.05 0.35 Q4 1 0.9958 0.2875 0.7733 11.00000 0.05 0.32 Q5 1 1.1661 0.2521 0.6772 11.00000 0.05 0.32 Q6 1 1.0017 0.5617 0.5827 11.00000 0.05 0.31 Q7 1 1.1567 0.3912 1.0423 11.00000 0.05 0.30 Q8 1 0.6298 0.3362 0.7972 11.00000 0.05 0.30 Q9 1 0.7102 0.3660 0.7850 11.00000 0.05 0.29 Q10 1 0.8596 0.3542 0.7368 11.00000 0.05 0.29 Q11 1 0.8637 0.2565 0.7984 11.00000 0.05 0.28 Q12 1 1.0406 0.0867 0.7173 11.00000 0.05 0.28 Q13 1 1.0871 0.2909 0.7934 11.00000 0.05 0.28 Q14 1 0.9599 0.3516 0.7600 11.00000 0.05 0.27 Q15 1 0.9238 0.4014 0.8614 11.00000 0.05 0.27 Q16 1 0.7798 0.4993 0.4243 11.00000 0.05 0.27 Q17 1 0.8669 0.2394 0.7366 11.00000 0.05 0.27 Q18 1 0.5998 0.2867 0.8172 11.00000 0.05 0.27 Q19 1 1.0576 0.2952 0.7028 11.00000 0.05 0.26 Q20 1 0.9868 0.4920 0.6606 11.00000 0.05 0.26 ; _shelx_res_checksum 36321 _shelx_hkl_file ; 0 0 3 23.9151 89.7867 1 0 0 3 76.6969 124.887 2 0 0 -4 33675.2 1332.25 1 0 0 4 33795.5 1311.24 1 0 0 4 36453.5 1317.50 2 0 0 -4 33100.9 1261.77 2 0 0 5 2484.48 461.632 2 0 0 -5 3094.46 519.358 2 0 0 -5 2812.00 533.509 1 0 0 -6 107385. 2923.87 1 0 0 -6 107710. 2803.47 2 0 0 -7 24487.4 1535.82 2 0 0 -7 20061.9 1455.56 1 0 0 -8 13319.6 1215.54 2 0 0 -9 1085.38 480.784 2 0 0 -10 15990.0 1439.58 2 0 0 -11 58.3248 369.444 2 0 0 -12 42106.8 2591.16 2 0 0 -13-201.125 320.349 2 0 0 -14 33570.1 2518.67 2 0 0 -15 876.600 585.512 2 0 0 -16 584.713 547.730 2 0 0 -17-567.515 579.926 2 0 0 -18-156.818 539.893 2 0 0 -19 2279.77 1054.08 2 0 0 -20 2181.52 958.221 2 0 0 -21 184.140 732.651 2 0 1 3 51109.1 1354.68 2 0 -1 3 52135.2 1413.81 1 0 -1 3 53555.1 1434.65 2 0 -1 -3 53314.7 1436.67 1 0 1 3 51651.9 1432.09 1 0 -1 -3 52613.6 1384.07 2 0 1 -3 53004.3 1430.95 2 0 -1 -4 160908. 2802.05 2 0 1 -4 176189. 2994.53 2 0 1 4 172595. 3006.86 1 0 -1 -4 177883. 3008.30 1 0 -1 4 174631. 2939.47 2 0 -1 4 174116. 2980.58 1 0 1 4 164954. 2828.10 2 0 1 5 85310.6 2261.28 2 0 -1 -5 85146.0 2371.97 1 0 -1 5 84887.4 2276.30 2 0 1 -5 86409.3 2332.27 2 0 -1 -5 82481.4 2257.24 2 0 -1 -6 115738. 2901.65 2 0 -1 -6 113327. 2967.58 1 0 1 -6 115043. 2942.76 2 0 -1 -7 142355. 3499.71 2 0 -1 -7 144972. 3653.58 1 0 1 -7 143293. 3552.51 2 0 -1 -8 48685.8 2294.16 1 0 1 -8 50949.8 2262.35 2 0 -1 -8 48210.0 2196.28 2 0 -1 -9 11804.0 1199.89 1 0 -1 -9 11095.0 1134.13 2 0 1 -9 12582.6 1230.51 2 0 1 -10 94.8703 279.183 2 0 -1 -10-57.6877 373.132 2 0 -1 -11 2035.63 602.125 2 0 1 -11 2289.98 640.220 2 0 1 -12 1638.97 573.134 2 0 -1 -12 2301.88 691.196 2 0 1 -13 2105.65 708.796 2 0 -1 -13 3262.52 826.540 2 0 -1 -14 1345.68 723.788 2 0 1 -14 476.085 574.228 2 0 1 -15 2724.68 877.878 2 0 -1 -15 1887.26 723.422 2 0 -1 -16 2353.52 822.967 2 0 1 -16 2398.63 806.051 2 0 -1 -17 5632.77 1249.46 2 0 1 -17 4755.32 1222.00 2 0 -1 -18 14358.9 2006.93 2 0 1 -18 9446.40 1656.20 2 0 -1 -19-1020.46 695.105 2 0 1 -19-148.037 478.143 2 0 -1 -20-584.206 888.913 2 0 -1 -21 2893.74 1058.94 2 0 -1 -22-1692.35 1073.09 2 0 -1 -23-169.411 708.348 2 0 2 2 173113. 2348.37 2 0 2 2 171630. 2269.07 1 0 -2 -3 5777.34 508.536 1 0 -2 3 5269.59 502.612 2 0 2 3 5570.60 488.779 2 0 2 3 6449.41 543.097 1 0 -2 -3 6268.69 524.243 2 0 -2 -4 8269.93 670.919 2 0 2 4 8917.02 716.364 1 0 -2 4 8885.32 722.449 2 0 2 4 10359.7 740.553 2 0 -2 -4 8516.18 694.921 1 0 -2 -5 18800.0 1103.66 2 0 -2 -5 19718.6 1144.50 1 0 2 -5 19443.3 1163.04 2 0 -2 -6 4196.73 598.127 1 0 2 -6 5212.37 678.864 2 0 -2 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37738.3 1243.64 2 0 -3 -3 6953.25 603.353 2 0 -3 -3 7203.64 607.232 1 0 3 3 5563.68 515.373 1 0 3 3 6511.86 581.508 2 0 3 4 210031. 3465.66 1 0 -3 -4 204349. 3471.01 2 0 -3 -4 207751. 3442.44 1 0 3 4 205439. 3427.10 2 0 -3 -5 1045.27 307.210 2 0 -3 -5 952.270 336.315 1 0 -3 -6 121522. 3105.92 2 0 -3 -6 122156. 3147.61 1 0 -3 -7 185.548 279.730 1 0 -3 -7 436.662 315.924 2 0 -3 -8 37081.4 2008.17 1 0 -3 -8 35694.6 1960.39 2 0 -3 -9 1106.16 484.312 2 0 -3 -9 1062.37 469.936 1 0 -3 -10 12541.4 1333.77 1 0 -3 -10 11812.5 1271.31 2 0 -3 -11 4186.27 914.950 1 0 -3 -11 1595.60 634.242 2 0 -3 -12 11222.7 1376.59 2 0 -3 -12 10052.2 1337.80 1 0 -3 -13 71.5737 441.312 2 0 -3 -14 4544.72 978.483 2 0 -3 -15 691.445 478.118 2 0 -3 -16 6077.67 1224.44 2 0 -3 -17 8994.02 1606.56 2 0 -3 -18 5300.12 1351.12 2 0 -3 -19 4988.39 1273.86 2 0 -3 -20 1967.60 1087.25 2 0 -3 -21 358.604 656.123 2 0 -3 -22 1110.53 907.471 2 0 -3 -23 436.838 733.892 2 0 -4 0 404397. 3444.71 1 0 -4 -1 384598. 3509.26 1 0 4 1 377712. 3465.76 1 0 4 2 86264.9 1836.39 1 0 -4 -2 85470.3 1832.85 1 0 -4 -2 87096.3 2104.97 2 0 -4 -3 22027.5 1054.51 1 0 4 3 23691.9 1161.66 2 0 -4 -3 23242.9 1150.57 2 0 4 3 23441.4 1077.26 1 0 4 4 11282.2 837.467 1 0 -4 -4 11690.9 860.525 1 0 -4 -4 12452.8 915.461 2 0 -4 -5 16112.5 1115.29 2 0 -4 -5 19496.2 1195.84 1 0 -4 -6 51016.6 2080.92 1 0 -4 -6 53716.2 2141.80 2 0 -4 -7 17569.9 1318.42 1 0 -4 -7 15078.7 1203.70 2 0 -4 -8 24874.1 1661.43 1 0 -4 -8 26503.8 1724.53 2 0 -4 -9 30756.4 1945.96 1 0 -4 -9 29664.1 1931.14 2 0 -4 -10 334.932 329.804 1 0 -4 -10 409.740 367.906 2 0 -4 -11 199536. 5411.67 2 0 -4 -11 193151. 5398.44 1 0 -4 -12 1629.09 590.055 2 0 -4 -12 1580.42 717.062 1 0 -4 -13 111821. 4436.38 2 0 -4 -13 104827. 4382.43 1 0 -4 -14 8500.72 1361.93 2 0 -4 -15 4634.24 1040.03 2 0 -4 -16 1552.74 765.029 2 0 -4 -17-619.847 627.238 2 0 -4 -18 756.455 731.843 2 0 -4 -19 1276.40 852.614 2 0 -4 -20 1080.31 755.947 2 0 -4 -21 170.568 554.583 2 0 -4 -22 2577.73 1298.35 2 0 -5 0 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1345.67 834.589 1 -14 -3 5 4296.41 1204.35 1 -14 -3 4 1196.43 942.201 1 -14 -3 3 8786.58 1680.25 1 -14 -3 2 3256.10 1119.35 1 -14 -3 1 9626.68 1762.20 1 -14 -3 0 3509.98 1214.96 1 -14 -3 -1 2220.00 993.357 1 -14 -3 -2 2808.66 1118.86 1 -14 -3 -3 8364.59 1681.22 1 -14 -3 -4-197.347 633.422 1 -14 -3 -5 11355.9 2029.43 1 -14 -3 -6 2170.21 1117.77 1 14 -4 -18 1501.53 959.819 2 14 -4 -17 2026.52 899.828 2 -14 -4 14 62.3323 769.764 1 -14 -4 13 13835.1 2154.67 1 -14 -4 12-223.381 628.321 1 -14 -4 11 11358.0 1932.60 1 -14 -4 10 1325.30 802.291 1 -14 -4 9 11824.7 1923.26 1 -14 -4 8 5922.68 1331.03 1 -14 -4 7 40313.9 3370.98 1 -14 -4 6 1587.16 845.289 1 -14 -4 5 75599.5 4619.06 1 -14 -4 4-713.476 830.746 1 -14 -4 3 45013.9 3613.82 1 -14 -4 2 1142.69 852.003 1 -14 -4 1 15098.4 2137.13 1 -14 -4 0 1124.11 640.140 1 -14 -4 -1-620.902 664.488 1 -14 -4 -2 879.163 857.558 1 -14 -4 -3 2594.73 1307.70 1 -14 -4 -4 1155.67 896.213 1 -14 -4 -5 1963.25 1036.80 1 14 -5 -18 314.812 650.943 2 14 -5 -17 513.416 667.331 2 -14 -5 14 224.631 627.790 1 -14 -5 13 5294.52 1384.12 1 -14 -5 12 12.1949 664.889 1 -14 -5 11 22960.3 2722.80 1 -14 -5 10 1281.46 794.302 1 -14 -5 9 13882.1 2124.79 1 -14 -5 8 231.473 561.573 1 -14 -5 7 3785.47 1219.84 1 -14 -5 6 1995.65 900.537 1 -14 -5 5 13825.3 2107.13 1 -14 -5 4-154.219 617.456 1 -14 -5 3 25863.5 2829.96 1 -14 -5 2 90.1116 650.213 1 -14 -5 1 23132.6 2730.22 1 -14 -5 0 1381.58 914.530 1 -14 -5 -1 12120.2 2056.46 1 -14 -5 -2 1687.76 1086.48 1 -14 -5 -3 1769.90 792.077 1 -14 -5 -4-737.174 899.300 1 14 -6 -18 3814.49 1412.39 2 -14 -6 14 2246.38 1062.32 1 -14 -6 13 7491.70 1762.74 1 -14 -6 12 2986.16 1105.75 1 -14 -6 11 1955.19 934.263 1 -14 -6 10 739.259 564.608 1 -14 -6 9 4287.24 1203.96 1 -14 -6 8 547.286 812.297 1 -14 -6 7 37068.0 3429.96 1 -14 -6 6 1954.14 1063.51 1 -14 -6 5 40619.8 3547.40 1 -14 -6 4 681.251 711.791 1 -14 -6 3 30221.1 3122.75 1 -14 -6 2 730.918 672.807 1 -14 -6 1 7327.86 1547.69 1 -14 -6 0 1607.75 968.338 1 -14 -6 -1 768.223 686.063 1 -14 -6 -2 483.288 801.394 1 -14 -6 -3 4633.52 1434.44 1 -14 -6 -4-605.985 694.847 1 -14 -7 14 5237.88 1566.29 1 -14 -7 13 1266.94 899.469 1 -14 -7 12 1696.64 999.957 1 -14 -7 11 19091.2 2569.42 1 -14 -7 10 2012.39 1127.32 1 -14 -7 9 7147.92 1607.97 1 -14 -7 8 3455.30 1151.38 1 -14 -7 7 1250.48 895.279 1 -14 -7 6 646.121 827.840 1 -14 -7 5 10114.5 1920.85 1 -14 -7 4 2460.83 1139.47 1 -14 -7 3 15130.9 2268.97 1 -14 -7 2 1768.82 804.912 1 -14 -7 1 14664.0 2259.05 1 -14 -7 0 2134.96 928.656 1 -14 -7 -1 6746.78 1591.66 1 -14 -7 -2-352.722 637.821 1 -14 -7 -3 1672.96 930.399 1 -14 -8 13 1164.00 1132.33 1 -14 -8 12 10831.5 2070.99 1 -14 -8 11 1092.76 821.802 1 -14 -8 10 305.312 833.400 1 -14 -8 9-630.694 737.917 1 -14 -8 8 142.189 757.428 1 -14 -8 7 6368.91 1513.58 1 -14 -8 6 1763.46 1018.50 1 -14 -8 5 17467.0 2498.83 1 -14 -8 4 4465.48 1341.60 1 -14 -8 3 9341.62 1855.13 1 -14 -8 2 10791.2 2026.39 1 -14 -8 1-381.468 800.526 1 -14 -8 0 2997.63 1248.13 1 -14 -8 -1 8247.77 1768.46 1 -14 -8 -2 1642.07 1023.87 1 -14 -9 12 8644.04 1851.18 1 -14 -9 11 2614.93 1164.42 1 -14 -9 10 3050.10 1205.68 1 -14 -9 9 964.183 814.227 1 -14 -9 8 5860.93 1504.57 1 -14 -9 7 240.900 723.798 1 -14 -9 6 4281.22 1400.97 1 -14 -9 5 2662.29 1123.98 1 -14 -9 4 343.085 746.335 1 -14 -9 3 2488.53 984.925 1 -14 -9 2-252.456 816.996 1 -14 -9 1 140.951 753.903 1 -14 -9 0 379.900 735.464 1 -14 -10 11 1700.35 1019.41 1 -14 -10 10 3075.06 1334.11 1 -14 -10 9 1535.93 867.382 1 -14 -10 8 1632.34 906.356 1 -14 -10 7-570.635 637.282 1 -14 -10 6-834.258 779.761 1 -14 -10 5 2915.49 1221.31 1 -14 -10 4 344.982 701.167 1 -14 -10 3 1706.71 1098.97 1 -14 -10 2-66.8114 722.213 1 -14 -10 1 797.431 733.793 1 -14 -11 8-277.341 870.237 1 -14 -11 7 98.6639 734.678 1 -14 -11 6 510.285 874.544 1 -14 -11 5 927.115 893.520 1 -14 -11 4 474.067 744.869 1 -15 -2 15 8961.47 1751.44 1 -15 -2 14 1039.72 858.982 1 -15 -2 13 11956.1 1962.11 1 -15 -2 12 586.480 651.658 1 -15 -2 11 9049.77 1726.34 1 -15 -2 10 2775.67 1084.13 1 -15 -2 9 3914.21 1312.75 1 -15 -2 8 6295.74 1456.03 1 -15 -2 7-86.8777 692.117 1 -15 -2 6 12135.2 1920.57 1 -15 -2 5 1615.76 913.089 1 -15 -2 4 5054.07 1294.87 1 -15 -2 3 5845.73 1396.62 1 -15 -2 2 2894.62 1095.88 1 -15 -2 1 48.0849 584.058 1 -15 -2 0 7989.27 1668.74 1 -15 -2 -1 8995.14 1714.63 1 -15 -2 -2 3356.21 1281.66 1 -15 -2 -3 11537.9 2007.34 1 -15 -2 -4 1402.50 1120.47 1 -15 -3 16 6960.12 1580.71 1 -15 -3 15 2560.87 1123.13 1 -15 -3 14 17630.4 2506.74 1 -15 -3 13 1369.62 894.238 1 -15 -3 12 8046.69 1674.70 1 -15 -3 11 6641.57 1587.99 1 -15 -3 10 5359.20 1381.39 1 -15 -3 9 12305.0 1973.32 1 -15 -3 8 11476.6 1891.23 1 -15 -3 7-67.8454 618.876 1 -15 -3 6 14753.3 2165.53 1 -15 -3 5 1490.49 887.034 1 -15 -3 4 14357.1 2086.26 1 -15 -3 3 3484.44 1114.58 1 -15 -3 2 535.308 607.018 1 -15 -3 1 835.942 804.050 1 -15 -3 0 1322.28 779.468 1 -15 -3 -1-64.7503 591.552 1 -15 -3 -2 7129.08 1619.45 1 -15 -3 -3 861.947 793.795 1 -15 -4 15 392.870 788.568 1 -15 -4 14-443.999 794.903 1 -15 -4 13 3079.61 1081.26 1 -15 -4 12 721.887 738.501 1 -15 -4 11 553.752 682.712 1 -15 -4 10 2988.39 1123.07 1 -15 -4 9 1760.02 956.206 1 -15 -4 8 7518.95 1590.62 1 -15 -4 7 2746.42 1052.52 1 -15 -4 6 8516.67 1678.33 1 -15 -4 5 6287.93 1411.77 1 -15 -4 4 15076.1 2240.35 1 -15 -4 3 1076.82 711.155 1 -15 -4 2 24008.1 2796.61 1 -15 -4 1 1695.58 948.582 1 -15 -4 0 19931.9 2631.55 1 -15 -4 -1 4075.28 1230.59 1 -15 -4 -2 3368.54 1284.03 1 -15 -4 -3 101.306 774.954 1 -15 -5 14 22173.4 2829.00 1 -15 -5 13 1249.41 964.846 1 -15 -5 12 18822.1 2567.55 1 -15 -5 11 206.866 554.141 1 -15 -5 10 9354.50 1826.88 1 -15 -5 9-531.665 714.685 1 -15 -5 8 12254.3 2094.98 1 -15 -5 7 151.609 704.267 1 -15 -5 6 22690.7 2740.18 1 -15 -5 5 348.578 653.090 1 -15 -5 4 4955.64 1288.10 1 -15 -5 3 1800.51 1031.65 1 -15 -5 2 1814.28 991.645 1 -15 -5 1 1446.63 941.889 1 -15 -5 0 7617.75 1740.62 1 -15 -5 -1-798.254 833.606 1 -15 -5 -2 3554.99 1288.09 1 -15 -6 13 1011.58 937.377 1 -15 -6 12 800.699 788.027 1 -15 -6 11 217.151 602.980 1 -15 -6 10 2685.64 1165.20 1 -15 -6 9 1547.86 912.741 1 -15 -6 8 5270.52 1388.10 1 -15 -6 7 1810.69 966.420 1 -15 -6 6 11045.4 1964.44 1 -15 -6 5 586.244 633.148 1 -15 -6 4 11899.9 2049.26 1 -15 -6 3 1433.93 943.616 1 -15 -6 2 15632.1 2339.24 1 -15 -6 1 1548.81 1040.82 1 -15 -6 0 6954.36 1695.70 1 -15 -6 -1 2752.57 1112.87 1 -15 -7 12 2378.71 1077.35 1 -15 -7 11 389.695 699.488 1 -15 -7 10 1069.60 822.085 1 -15 -7 9 923.997 877.004 1 -15 -7 8 5894.15 1548.22 1 -15 -7 7 2727.78 1158.01 1 -15 -7 6 25950.9 3059.17 1 -15 -7 5 2456.99 951.297 1 -15 -7 4 12941.8 2233.91 1 -15 -7 3 9479.37 1967.94 1 -15 -7 2-2309.55 1214.15 1 -15 -7 1 6051.57 1626.21 1 -15 -8 10 655.020 868.091 1 -15 -8 9 4275.71 1411.62 1 -15 -8 8 2319.65 1142.71 1 -15 -8 7 1621.04 941.238 1 -15 -8 6 3827.22 1317.72 1 -15 -8 5 3081.07 1251.47 1 -15 -8 4 2310.84 1143.81 1 -15 -8 3 922.590 762.919 1 -16 -3 11 20818.5 2659.87 1 -16 -3 10 510.997 647.400 1 -16 -3 9 25344.4 2882.61 1 -16 -3 8-452.697 591.621 1 -16 -3 7 10285.3 1858.07 1 -16 -3 6 714.206 669.252 1 -16 -3 5 4023.35 1251.32 1 -16 -3 4 3928.69 1257.51 1 -16 -3 3 987.343 746.057 1 -16 -3 2 362.449 865.889 1 -16 -4 13 14963.1 2372.81 1 -16 -4 12 1139.70 838.713 1 -16 -4 11 3150.95 1162.02 1 -16 -4 10 1217.19 973.735 1 -16 -4 9 1368.71 974.637 1 -16 -4 8-217.233 840.992 1 -16 -4 7 234.689 772.933 1 -16 -4 6-498.302 683.260 1 -16 -4 5 954.930 828.671 1 -16 -4 4 2334.97 1099.94 1 -16 -4 3 3784.38 1265.61 1 -16 -4 2 1100.46 794.819 1 -16 -4 1 6017.88 1601.26 1 -16 -5 11 29148.9 3230.14 1 -16 -5 10-1736.15 980.999 1 -16 -5 9 42164.2 3851.62 1 -16 -5 8-581.187 695.356 1 -16 -5 7 21707.0 2743.50 1 -16 -5 6 1106.52 828.957 1 -16 -5 5 4200.04 1405.64 1 -16 -5 4-1556.74 1100.55 1 -16 -5 3 1892.74 1126.47 1 -16 -5 2-699.572 768.248 1 -16 -6 9 3129.99 1160.07 1 -16 -6 8 1057.18 844.308 1 -16 -6 7 3710.96 1381.07 1 -16 -6 6 1017.74 884.236 1 -16 -6 5 5382.42 1502.13 1 0 0 0 0.00 0.00 0 TITL aral62 in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 12.566197 18.957195 17.966391 90.0000 107.2003 90.0000 ZERR 6.00 0.000410 0.000524 0.000818 0.0000 0.0041 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N Si Fe Se UNIT 180.00 240.00 18.00 12.00 6.00 6.00 TREF HKLF 4 END ; _shelx_hkl_checksum 4917 _database_code_depnum_ccdc_archive 'CCDC 971589' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_xral8 _audit_creation_date 2013-11-12 _audit_creation_method ; Olex2 1.2 (compiled 2013.09.17 svn.r2790 for OlexSys, GUI svn.r4601) ; _shelxl_version_number 2013-2 _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C29 H35 Fe N2 Se3, C4 H8 O, C11 H21 N2' _chemical_formula_sum 'C44 H64 Fe N4 O Se3' _chemical_formula_weight 957.72 _chemical_melting_point Unknown 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' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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' Se Se -0.7943 1.1372 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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. ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.4281(4) _cell_length_b 9.40903(17) _cell_length_c 24.0280(4) _cell_angle_alpha 90 _cell_angle_beta 103.3807(16) _cell_angle_gamma 90 _cell_volume 4493.02(13) _cell_formula_units_Z 4 _cell_measurement_reflns_used 12788 _cell_measurement_temperature 100 _cell_measurement_theta_max 73.5525 _cell_measurement_theta_min 2.2213 _shelx_estimated_absorpt_T_max ? _shelx_estimated_absorpt_T_min ? _exptl_absorpt_coefficient_mu 5.742 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.01345 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour Yellow _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1968 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_unetI/netI 0.0780 _diffrn_reflns_Laue_measured_fraction_full 0.948 _diffrn_reflns_Laue_measured_fraction_max 0.973 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 20942 _diffrn_reflns_point_group_measured_fraction_full 0.948 _diffrn_reflns_point_group_measured_fraction_max 0.973 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 66.599 _diffrn_reflns_theta_min 7.389 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.9333 _diffrn_measured_fraction_theta_max 0.9990 _diffrn_measurement_device_type 'Saxi-CrysAlisPro-abstract goniometer imported SAXI images' _diffrn_measurement_method '\w and \p scans' _diffrn_orient_matrix_UB_11 -0.0646763000 _diffrn_orient_matrix_UB_12 0.0143599000 _diffrn_orient_matrix_UB_13 -0.0476225000 _diffrn_orient_matrix_UB_21 -0.0426665000 _diffrn_orient_matrix_UB_22 -0.0289176000 _diffrn_orient_matrix_UB_23 0.0439346000 _diffrn_orient_matrix_UB_31 -0.0019237000 _diffrn_orient_matrix_UB_32 0.1604780000 _diffrn_orient_matrix_UB_33 0.0121853000 _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.5418 _diffrn_source 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6379 _reflns_number_total 7709 _reflns_odcompleteness_completeness 93.33 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 73.55 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET) (compiled Jul 11 2012,15:38:31) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution ; SHELX, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _refine_diff_density_max 0.973 _refine_diff_density_min -1.031 _refine_diff_density_rms 0.132 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 490 _refine_ls_number_reflns 7709 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0561 _refine_ls_restrained_S_all 1.043 _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^)+(0.0863P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1415 _refine_ls_wR_factor_ref 0.1530 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C41(H41A,H41B), C42(H42A,H42B), C43(H43A,H43B), C44(H44A,H44B) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32) 2.c Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C9(H9A,H9B,H9C), C10(H10A, H10B,H10C), C11(H11A,H11B,H11C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B, H40C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 Se1 Se 0.36621(2) 0.37936(6) 0.80349(2) 0.02022(15) Uani 1 1 d . . . . . Se2 Se 0.35523(2) 0.45031(6) 0.65906(2) 0.02156(15) Uani 1 1 d . . . . . Se3 Se 0.20476(3) 0.63861(6) 0.72727(2) 0.02641(16) Uani 1 1 d . . . . . Fe3A Fe 0.27164(3) 0.42159(8) 0.71953(3) 0.01660(18) Uani 1 1 d . . . . . N1 N 0.15745(18) 0.0983(4) 0.61914(15) 0.0164(8) Uani 1 1 d . . . . . N2 N 0.17970(18) 0.1332(4) 0.71084(15) 0.0157(8) Uani 1 1 d . . . . . C1 C 0.2122(2) 0.2437(5) 0.68878(18) 0.0169(9) Uani 1 1 d . . . . . C2 C 0.1973(2) 0.2174(5) 0.63173(18) 0.0161(9) Uani 1 1 d . . . . . H2 H 0.2122 0.2735 0.6042 0.019 Uiso 1 1 calc R U . . . C3 C 0.1489(2) 0.0458(5) 0.66871(17) 0.0177(9) Uani 1 1 d . . . . . H3 H 0.1252 -0.0386 0.6733 0.021 Uiso 1 1 calc R U . . . C4 C 0.1329(2) 0.0346(5) 0.56096(17) 0.0194(10) Uani 1 1 d . . . . . C5 C 0.1926(3) -0.0296(8) 0.5431(2) 0.0475(18) Uani 1 1 d . . . . . H5A H 0.2279 0.0425 0.5459 0.071 Uiso 1 1 calc R U . . . H5B H 0.1787 -0.0631 0.5035 0.071 Uiso 1 1 calc R U . . . H5C H 0.2100 -0.1097 0.5682 0.071 Uiso 1 1 calc R U . . . C6 C 0.1028(3) 0.1552(6) 0.5202(2) 0.0338(12) Uani 1 1 d . . . . . H6A H 0.0660 0.2001 0.5336 0.051 Uiso 1 1 calc R U . . . H6B H 0.0855 0.1166 0.4817 0.051 Uiso 1 1 calc R U . . . H6C H 0.1377 0.2259 0.5191 0.051 Uiso 1 1 calc R U . . . C7 C 0.0785(3) -0.0740(7) 0.5619(2) 0.0404(15) Uani 1 1 d . . . . . H7A H 0.0971 -0.1512 0.5882 0.061 Uiso 1 1 calc R U . . . H7B H 0.0617 -0.1126 0.5234 0.061 Uiso 1 1 calc R U . . . H7C H 0.0415 -0.0285 0.5748 0.061 Uiso 1 1 calc R U . . . C8 C 0.1835(2) 0.1069(5) 0.77309(17) 0.0171(9) Uani 1 1 d . . . . . C9 C 0.1293(2) -0.0002(5) 0.77911(18) 0.0213(10) Uani 1 1 d . . . . . H9A H 0.0854 0.0326 0.7570 0.032 Uiso 1 1 calc R U . . . H9B H 0.1281 -0.0088 0.8195 0.032 Uiso 1 1 calc R U . . . H9C H 0.1396 -0.0929 0.7647 0.032 Uiso 1 1 calc R U . . . C10 C 0.1716(3) 0.2476(5) 0.80011(18) 0.0261(11) Uani 1 1 d . . . . . H10A H 0.2068 0.3153 0.7962 0.039 Uiso 1 1 calc R U . . . H10B H 0.1730 0.2330 0.8407 0.039 Uiso 1 1 calc R U . . . H10C H 0.1275 0.2853 0.7808 0.039 Uiso 1 1 calc R U . . . C11 C 0.2527(2) 0.0460(6) 0.7996(2) 0.0283(11) Uani 1 1 d . . . . . H11A H 0.2597 -0.0406 0.7791 0.042 Uiso 1 1 calc R U . . . H11B H 0.2555 0.0233 0.8399 0.042 Uiso 1 1 calc R U . . . H11C H 0.2873 0.1161 0.7969 0.042 Uiso 1 1 calc R U . . . C12 C 0.3523(2) 0.4464(5) 0.87534(19) 0.0205(10) Uani 1 1 d . . . . . C13 C 0.2952(2) 0.5227(6) 0.87961(19) 0.0251(11) Uani 1 1 d . . . . . H13 H 0.2601 0.5369 0.8465 0.030 Uiso 1 1 calc R U . . . C14 C 0.2891(3) 0.5783(6) 0.9318(2) 0.0301(12) Uani 1 1 d . . . . . H14 H 0.2498 0.6297 0.9340 0.036 Uiso 1 1 calc R U . . . C15 C 0.3399(3) 0.5593(6) 0.9806(2) 0.0318(12) Uani 1 1 d . . . . . H15 H 0.3359 0.5985 1.0160 0.038 Uiso 1 1 calc R U . . . C16 C 0.3964(3) 0.4828(6) 0.97706(19) 0.0296(12) Uani 1 1 d . . . . . H16 H 0.4313 0.4684 1.0104 0.036 Uiso 1 1 calc R U . . . C17 C 0.4026(3) 0.4269(5) 0.9250(2) 0.0260(11) Uani 1 1 d . . . . . H17 H 0.4417 0.3742 0.9232 0.031 Uiso 1 1 calc R U . . . C18 C 0.3051(2) 0.4560(6) 0.58116(19) 0.0230(10) Uani 1 1 d . . . . . C19 C 0.2633(3) 0.5704(6) 0.5602(2) 0.0326(12) Uani 1 1 d . . . . . H19 H 0.2602 0.6480 0.5847 0.039 Uiso 1 1 calc R U . . . C20 C 0.2259(3) 0.5728(7) 0.5035(2) 0.0399(14) Uani 1 1 d . . . . . H20 H 0.1982 0.6524 0.4900 0.048 Uiso 1 1 calc R U . . . C21 C 0.2288(3) 0.4607(7) 0.4671(2) 0.0377(14) Uani 1 1 d . . . . . H21 H 0.2021 0.4613 0.4290 0.045 Uiso 1 1 calc R U . . . C22 C 0.2709(3) 0.3479(7) 0.4867(2) 0.0350(13) Uani 1 1 d . . . . . H22 H 0.2743 0.2717 0.4616 0.042 Uiso 1 1 calc R U . . . C23 C 0.3086(2) 0.3449(6) 0.5433(2) 0.0281(11) Uani 1 1 d . . . . . H23 H 0.3370 0.2659 0.5563 0.034 Uiso 1 1 calc R U . . . C24 C 0.1215(2) 0.6167(5) 0.67125(18) 0.0191(9) Uani 1 1 d . . . . . C25 C 0.0626(2) 0.6735(6) 0.6828(2) 0.0263(11) Uani 1 1 d . . . . . H25 H 0.0639 0.7175 0.7186 0.032 Uiso 1 1 calc R U . . . C26 C 0.0018(3) 0.6653(6) 0.6416(2) 0.0338(12) Uani 1 1 d . . . . . H26 H -0.0377 0.7054 0.6495 0.041 Uiso 1 1 calc R U . . . C27 C -0.0016(3) 0.6000(6) 0.5898(2) 0.0342(13) Uani 1 1 d . . . . . H27 H -0.0431 0.5947 0.5622 0.041 Uiso 1 1 calc R U . . . C28 C 0.0564(3) 0.5421(6) 0.5784(2) 0.0342(13) Uani 1 1 d . . . . . H28 H 0.0546 0.4960 0.5429 0.041 Uiso 1 1 calc R U . . . C29 C 0.1170(3) 0.5514(5) 0.6187(2) 0.0277(11) Uani 1 1 d . . . . . H29 H 0.1564 0.5122 0.6101 0.033 Uiso 1 1 calc R U . . . O1 O 0.1049(3) 0.6460(6) 0.91567(19) 0.0699(17) Uani 1 1 d . . . . . C41 C 0.0617(3) 0.7594(7) 0.8965(2) 0.0404(14) Uani 1 1 d . . . . . H41A H 0.0883 0.8451 0.8924 0.048 Uiso 1 1 calc R U . . . H41B H 0.0349 0.7805 0.9250 0.048 Uiso 1 1 calc R U . . . C42 C 0.0150(3) 0.7237(8) 0.8396(3) 0.0483(17) Uani 1 1 d . . . . . H42A H 0.0205 0.7910 0.8093 0.058 Uiso 1 1 calc R U . . . H42B H -0.0326 0.7230 0.8422 0.058 Uiso 1 1 calc R U . . . C43 C 0.0398(3) 0.5716(7) 0.8286(3) 0.0464(16) Uani 1 1 d . . . . . H43A H 0.0109 0.4975 0.8397 0.056 Uiso 1 1 calc R U . . . H43B H 0.0410 0.5585 0.7880 0.056 Uiso 1 1 calc R U . . . C44 C 0.1080(3) 0.5691(9) 0.8660(3) 0.058(2) Uani 1 1 d . . . . . H44A H 0.1224 0.4700 0.8759 0.070 Uiso 1 1 calc R U . . . H44B H 0.1405 0.6137 0.8465 0.070 Uiso 1 1 calc R U . . . N3 N 0.42868(19) 0.8922(4) 0.84003(15) 0.0184(8) Uani 1 1 d . . . . . N4 N 0.41280(18) 0.9049(4) 0.74744(15) 0.0169(8) Uani 1 1 d . . . . . C30 C 0.4407(2) 0.9689(5) 0.79682(18) 0.0179(9) Uani 1 1 d . . . . . H30 H 0.4653 1.0555 0.8006 0.021 Uiso 1 1 calc R U . . . C31 C 0.3922(2) 0.7745(5) 0.81717(19) 0.0216(10) Uani 1 1 d . . . . . H31 H 0.3766 0.7015 0.8382 0.026 Uiso 1 1 calc R U . . . C32 C 0.3823(2) 0.7809(5) 0.75969(19) 0.0204(10) Uani 1 1 d . . . . . H32 H 0.3589 0.7136 0.7329 0.025 Uiso 1 1 calc R U . . . C33 C 0.4518(2) 0.9243(5) 0.90256(18) 0.0209(10) Uani 1 1 d . . . . . C34 C 0.4962(3) 0.8010(6) 0.92928(19) 0.0304(12) Uani 1 1 d . . . . . H34A H 0.4704 0.7124 0.9224 0.046 Uiso 1 1 calc R U . . . H34B H 0.5117 0.8168 0.9706 0.046 Uiso 1 1 calc R U . . . H34C H 0.5352 0.7945 0.9121 0.046 Uiso 1 1 calc R U . . . C35 C 0.3897(2) 0.9398(7) 0.9264(2) 0.0336(13) Uani 1 1 d . . . . . H35A H 0.4033 0.9571 0.9677 0.050 Uiso 1 1 calc R U . . . H35B H 0.3630 0.8524 0.9192 0.050 Uiso 1 1 calc R U . . . H35C H 0.3627 1.0199 0.9077 0.050 Uiso 1 1 calc R U . . . C36 C 0.4922(3) 1.0622(6) 0.9088(2) 0.0311(12) Uani 1 1 d . . . . . H36A H 0.5310 1.0504 0.8917 0.047 Uiso 1 1 calc R U . . . H36B H 0.5080 1.0853 0.9495 0.047 Uiso 1 1 calc R U . . . H36C H 0.4636 1.1394 0.8894 0.047 Uiso 1 1 calc R U . . . C37 C 0.4110(2) 0.9604(5) 0.68890(18) 0.0208(10) Uani 1 1 d . . . . . C38 C 0.4579(3) 1.0871(5) 0.6936(2) 0.0286(11) Uani 1 1 d . . . . . H38A H 0.5032 1.0592 0.7143 0.043 Uiso 1 1 calc R U . . . H38B H 0.4415 1.1640 0.7143 0.043 Uiso 1 1 calc R U . . . H38C H 0.4593 1.1200 0.6552 0.043 Uiso 1 1 calc R U . . . C39 C 0.3388(3) 1.0006(7) 0.6624(2) 0.0351(13) Uani 1 1 d . . . . . H39A H 0.3249 1.0776 0.6846 0.053 Uiso 1 1 calc R U . . . H39B H 0.3097 0.9179 0.6625 0.053 Uiso 1 1 calc R U . . . H39C H 0.3351 1.0324 0.6229 0.053 Uiso 1 1 calc R U . . . C40 C 0.4357(2) 0.8407(6) 0.65557(19) 0.0272(11) Uani 1 1 d . . . . . H40A H 0.4077 0.7561 0.6557 0.041 Uiso 1 1 calc R U . . . H40B H 0.4826 0.8180 0.6737 0.041 Uiso 1 1 calc R U . . . H40C H 0.4325 0.8713 0.6161 0.041 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Se1 0.0189(3) 0.0233(3) 0.0181(2) -0.00256(18) 0.00347(19) 0.00006(19) Se2 0.0243(3) 0.0227(3) 0.0198(2) 0.00001(19) 0.0095(2) -0.0039(2) Se3 0.0279(3) 0.0215(3) 0.0265(3) -0.0079(2) -0.0003(2) 0.0044(2) Fe3A 0.0201(4) 0.0152(4) 0.0148(3) -0.0017(3) 0.0048(3) -0.0013(3) N1 0.0175(19) 0.019(2) 0.0136(17) -0.0019(15) 0.0052(14) -0.0031(15) N2 0.0181(19) 0.015(2) 0.0150(17) -0.0005(14) 0.0061(14) 0.0009(14) C1 0.020(2) 0.012(2) 0.022(2) -0.0007(17) 0.0114(17) -0.0004(17) C2 0.017(2) 0.014(2) 0.019(2) -0.0003(17) 0.0076(17) -0.0010(17) C3 0.018(2) 0.022(3) 0.0131(19) 0.0014(17) 0.0039(17) -0.0021(18) C4 0.020(2) 0.026(3) 0.0127(19) -0.0076(18) 0.0040(17) -0.0042(19) C5 0.030(3) 0.073(5) 0.035(3) -0.032(3) -0.001(2) 0.015(3) C6 0.047(3) 0.027(3) 0.022(2) 0.002(2) -0.003(2) -0.008(2) C7 0.056(4) 0.044(4) 0.020(2) -0.006(2) 0.005(2) -0.026(3) C8 0.021(2) 0.020(3) 0.0113(19) -0.0035(17) 0.0061(17) -0.0019(18) C9 0.029(3) 0.023(3) 0.015(2) -0.0031(18) 0.0129(19) -0.002(2) C10 0.040(3) 0.024(3) 0.019(2) -0.0033(19) 0.017(2) -0.004(2) C11 0.026(3) 0.039(3) 0.019(2) 0.007(2) 0.0036(19) 0.000(2) C12 0.021(2) 0.021(3) 0.020(2) -0.0016(18) 0.0048(18) -0.0030(19) C13 0.019(2) 0.036(3) 0.019(2) 0.006(2) 0.0008(18) -0.002(2) C14 0.024(3) 0.044(4) 0.025(2) -0.002(2) 0.011(2) -0.002(2) C15 0.033(3) 0.044(4) 0.019(2) -0.004(2) 0.007(2) -0.001(2) C16 0.037(3) 0.034(3) 0.015(2) 0.001(2) 0.001(2) -0.004(2) C17 0.028(3) 0.026(3) 0.023(2) 0.003(2) 0.004(2) 0.003(2) C18 0.018(2) 0.030(3) 0.021(2) 0.001(2) 0.0048(18) -0.0060(19) C19 0.053(3) 0.018(3) 0.027(3) 0.002(2) 0.011(2) 0.003(2) C20 0.052(4) 0.036(4) 0.029(3) 0.013(2) 0.004(3) 0.004(3) C21 0.043(3) 0.055(4) 0.015(2) 0.005(2) 0.006(2) -0.009(3) C22 0.042(3) 0.042(4) 0.025(2) -0.006(2) 0.017(2) -0.009(3) C23 0.027(3) 0.029(3) 0.032(3) 0.003(2) 0.015(2) -0.003(2) C24 0.024(2) 0.015(2) 0.017(2) -0.0016(17) 0.0032(18) -0.0002(18) C25 0.027(3) 0.023(3) 0.031(2) -0.001(2) 0.012(2) -0.007(2) C26 0.023(3) 0.032(3) 0.050(3) 0.005(3) 0.015(2) -0.004(2) C27 0.032(3) 0.029(3) 0.034(3) 0.006(2) -0.009(2) -0.006(2) C28 0.045(3) 0.028(3) 0.025(2) -0.001(2) -0.003(2) 0.002(2) C29 0.036(3) 0.020(3) 0.026(2) -0.001(2) 0.006(2) 0.008(2) O1 0.083(4) 0.083(4) 0.032(2) -0.012(2) -0.010(2) 0.042(3) C41 0.042(3) 0.038(4) 0.040(3) 0.010(3) 0.010(3) 0.006(3) C42 0.035(3) 0.057(5) 0.050(3) 0.021(3) 0.005(3) -0.007(3) C43 0.051(4) 0.049(4) 0.039(3) -0.001(3) 0.010(3) -0.012(3) C44 0.048(4) 0.087(6) 0.036(3) -0.019(4) 0.002(3) 0.016(4) N3 0.023(2) 0.019(2) 0.0150(17) -0.0010(15) 0.0078(15) -0.0004(16) N4 0.0173(19) 0.018(2) 0.0150(17) 0.0001(15) 0.0022(14) -0.0006(15) C30 0.025(2) 0.011(2) 0.016(2) -0.0019(17) 0.0024(17) -0.0038(18) C31 0.025(2) 0.019(3) 0.022(2) 0.0005(19) 0.0074(19) -0.0016(19) C32 0.023(2) 0.019(3) 0.020(2) -0.0038(18) 0.0064(18) -0.0048(19) C33 0.023(2) 0.030(3) 0.0105(19) -0.0039(18) 0.0046(17) 0.006(2) C34 0.037(3) 0.038(3) 0.014(2) 0.000(2) 0.001(2) 0.009(2) C35 0.023(3) 0.060(4) 0.018(2) -0.005(2) 0.005(2) 0.006(2) C36 0.043(3) 0.034(3) 0.017(2) -0.013(2) 0.009(2) -0.006(2) C37 0.024(2) 0.023(3) 0.015(2) 0.0024(18) 0.0054(18) 0.0024(19) C38 0.040(3) 0.024(3) 0.025(2) 0.009(2) 0.012(2) -0.003(2) C39 0.032(3) 0.051(4) 0.022(2) 0.013(2) 0.005(2) 0.009(3) C40 0.031(3) 0.032(3) 0.021(2) -0.007(2) 0.013(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Se1 Fe3A 2.4812(8) . ? Se1 C12 1.920(4) . ? Se2 Fe3A 2.4995(8) . ? Se2 C18 1.915(5) . ? Se3 Fe3A 2.4876(9) . ? Se3 C24 1.920(4) . ? Fe3A C1 2.099(5) . ? N1 C2 1.377(6) . ? N1 C3 1.337(6) . ? N1 C4 1.497(5) . ? N2 C1 1.403(5) . ? N2 C3 1.342(6) . ? N2 C8 1.500(5) . ? C1 C2 1.356(6) . ? C4 C5 1.510(7) . ? C4 C6 1.532(7) . ? C4 C7 1.513(7) . ? C8 C9 1.529(6) . ? C8 C10 1.518(6) . ? C8 C11 1.522(6) . ? C12 C13 1.393(7) . ? C12 C17 1.394(7) . ? C13 C14 1.391(7) . ? C14 C15 1.385(7) . ? C15 C16 1.379(7) . ? C16 C17 1.389(7) . ? C18 C19 1.394(7) . ? C18 C23 1.398(7) . ? C19 C20 1.398(8) . ? C20 C21 1.381(8) . ? C21 C22 1.378(8) . ? C22 C23 1.401(7) . ? C24 C25 1.402(7) . ? C24 C29 1.388(7) . ? C25 C26 1.399(7) . ? C26 C27 1.374(8) . ? C27 C28 1.387(8) . ? C28 C29 1.386(7) . ? O1 C41 1.394(7) . ? O1 C44 1.410(7) . ? C41 C42 1.514(8) . ? C42 C43 1.560(9) . ? C43 C44 1.472(9) . ? N3 C30 1.333(6) . ? N3 C31 1.376(6) . ? N3 C33 1.498(5) . ? N4 C30 1.336(6) . ? N4 C32 1.386(6) . ? N4 C37 1.493(5) . ? C31 C32 1.350(6) . ? C33 C34 1.520(7) . ? C33 C35 1.515(6) . ? C33 C36 1.527(7) . ? C37 C38 1.517(7) . ? C37 C39 1.513(7) . ? C37 C40 1.534(6) . ? 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 C12 Se1 Fe3A 115.43(14) . . ? C18 Se2 Fe3A 106.78(13) . . ? C24 Se3 Fe3A 105.78(14) . . ? Se1 Fe3A Se2 88.96(3) . . ? Se1 Fe3A Se3 114.10(3) . . ? Se3 Fe3A Se2 114.56(3) . . ? C1 Fe3A Se1 115.89(13) . . ? C1 Fe3A Se2 107.39(11) . . ? C1 Fe3A Se3 113.45(12) . . ? C2 N1 C4 125.8(4) . . ? C3 N1 C2 107.3(4) . . ? C3 N1 C4 126.8(4) . . ? C1 N2 C8 125.4(4) . . ? C3 N2 C1 110.5(3) . . ? C3 N2 C8 123.9(4) . . ? N2 C1 Fe3A 138.1(3) . . ? C2 C1 Fe3A 118.5(3) . . ? C2 C1 N2 103.4(4) . . ? C1 C2 N1 110.7(4) . . ? N1 C3 N2 108.1(4) . . ? N1 C4 C5 107.9(4) . . ? N1 C4 C6 107.4(4) . . ? N1 C4 C7 110.2(4) . . ? C5 C4 C6 110.1(4) . . ? C5 C4 C7 112.3(5) . . ? C7 C4 C6 108.8(4) . . ? N2 C8 C9 109.4(3) . . ? N2 C8 C10 107.8(4) . . ? N2 C8 C11 107.9(3) . . ? C10 C8 C9 110.1(4) . . ? C10 C8 C11 111.9(4) . . ? C11 C8 C9 109.6(4) . . ? C13 C12 Se1 122.4(3) . . ? C13 C12 C17 117.9(4) . . ? C17 C12 Se1 119.6(3) . . ? C14 C13 C12 120.7(4) . . ? C15 C14 C13 120.5(5) . . ? C16 C15 C14 119.3(5) . . ? C15 C16 C17 120.2(5) . . ? C16 C17 C12 121.3(5) . . ? C19 C18 Se2 121.3(4) . . ? C19 C18 C23 117.5(5) . . ? C23 C18 Se2 121.2(4) . . ? C18 C19 C20 121.1(5) . . ? C21 C20 C19 120.7(5) . . ? C22 C21 C20 119.1(5) . . ? C21 C22 C23 120.5(5) . . ? C18 C23 C22 121.2(5) . . ? C25 C24 Se3 118.8(3) . . ? C29 C24 Se3 123.2(4) . . ? C29 C24 C25 118.0(4) . . ? C26 C25 C24 120.0(5) . . ? C27 C26 C25 121.1(5) . . ? C26 C27 C28 119.2(5) . . ? C29 C28 C27 120.2(5) . . ? C28 C29 C24 121.6(5) . . ? C41 O1 C44 105.2(5) . . ? O1 C41 C42 110.3(5) . . ? C41 C42 C43 101.3(5) . . ? C44 C43 C42 102.1(5) . . ? O1 C44 C43 106.7(5) . . ? C30 N3 C31 107.8(4) . . ? C30 N3 C33 126.9(4) . . ? C31 N3 C33 125.3(4) . . ? C30 N4 C32 108.2(4) . . ? C30 N4 C37 126.3(4) . . ? C32 N4 C37 125.5(4) . . ? N3 C30 N4 109.2(4) . . ? C32 C31 N3 108.2(4) . . ? C31 C32 N4 106.6(4) . . ? N3 C33 C34 106.8(4) . . ? N3 C33 C35 107.5(4) . . ? N3 C33 C36 107.9(4) . . ? C34 C33 C36 110.5(4) . . ? C35 C33 C34 112.6(4) . . ? C35 C33 C36 111.2(4) . . ? N4 C37 C38 109.1(4) . . ? N4 C37 C39 107.0(4) . . ? N4 C37 C40 107.2(4) . . ? C38 C37 C40 109.7(4) . . ? C39 C37 C38 111.9(4) . . ? C39 C37 C40 111.7(4) . . ? _shelx_res_file ; TITL CELL 1.54184 20.428112 9.40903 24.027989 90 103.3807 90 ZERR 4 0.000351 0.000168 0.000371 0 0.0016 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O Fe Se UNIT 176 256 16 4 4 12 L.S. 6 PLAN 28 TEMP -173.15 fmap 2 acta SHEL 6 0.84 REM C:/XTAL%20DATA/xral8/struct/olex2_xral8/xral8.hkl WGHT 0.086300 FVAR 2.37210 SE1 6 0.366208 0.379357 0.803491 11.00000 0.01887 0.02329 = 0.01809 -0.00256 0.00347 0.00006 SE2 6 0.355227 0.450307 0.659065 11.00000 0.02427 0.02272 = 0.01982 0.00001 0.00947 -0.00393 SE3 6 0.204763 0.638611 0.727267 11.00000 0.02794 0.02153 = 0.02651 -0.00792 -0.00031 0.00436 FE3A 5 0.271641 0.421588 0.719528 11.00000 0.02014 0.01520 = 0.01482 -0.00167 0.00478 -0.00134 N1 3 0.157453 0.098262 0.619142 11.00000 0.01746 0.01880 = 0.01361 -0.00194 0.00524 -0.00313 N2 3 0.179696 0.133155 0.710835 11.00000 0.01807 0.01513 = 0.01504 -0.00054 0.00614 0.00088 C1 1 0.212219 0.243729 0.688779 11.00000 0.02003 0.01224 = 0.02162 -0.00069 0.01144 -0.00044 C2 1 0.197273 0.217433 0.631732 11.00000 0.01713 0.01387 = 0.01908 -0.00034 0.00762 -0.00098 AFIX 43 H2 2 0.212228 0.273546 0.604222 11.00000 -1.20000 AFIX 0 C3 1 0.148919 0.045782 0.668707 11.00000 0.01806 0.02203 = 0.01313 0.00136 0.00388 -0.00214 AFIX 43 H3 2 0.125202 -0.038637 0.673295 11.00000 -1.20000 AFIX 0 C4 1 0.132871 0.034574 0.560958 11.00000 0.01964 0.02605 = 0.01274 -0.00761 0.00405 -0.00423 C5 1 0.192619 -0.029563 0.543068 11.00000 0.02997 0.07293 = 0.03527 -0.03223 -0.00129 0.01472 AFIX 137 H5A 2 0.227879 0.042487 0.545890 11.00000 -1.50000 H5B 2 0.178718 -0.063134 0.503476 11.00000 -1.50000 H5C 2 0.210025 -0.109655 0.568232 11.00000 -1.50000 AFIX 0 C6 1 0.102826 0.155161 0.520158 11.00000 0.04667 0.02688 = 0.02243 0.00164 -0.00287 -0.00775 AFIX 137 H6A 2 0.066025 0.200121 0.533583 11.00000 -1.50000 H6B 2 0.085501 0.116601 0.481676 11.00000 -1.50000 H6C 2 0.137730 0.225906 0.519114 11.00000 -1.50000 AFIX 0 C7 1 0.078507 -0.074005 0.561914 11.00000 0.05578 0.04387 = 0.01986 -0.00626 0.00518 -0.02602 AFIX 137 H7A 2 0.097144 -0.151230 0.588195 11.00000 -1.50000 H7B 2 0.061711 -0.112576 0.523362 11.00000 -1.50000 H7C 2 0.041454 -0.028536 0.574804 11.00000 -1.50000 AFIX 0 C8 1 0.183463 0.106910 0.773092 11.00000 0.02093 0.02024 = 0.01125 -0.00348 0.00610 -0.00194 C9 1 0.129257 -0.000172 0.779112 11.00000 0.02940 0.02277 = 0.01545 -0.00314 0.01295 -0.00237 AFIX 137 H9A 2 0.085370 0.032588 0.757013 11.00000 -1.50000 H9B 2 0.128054 -0.008838 0.819508 11.00000 -1.50000 H9C 2 0.139594 -0.092922 0.764675 11.00000 -1.50000 AFIX 0 C10 1 0.171643 0.247611 0.800109 11.00000 0.04047 0.02352 = 0.01949 -0.00328 0.01738 -0.00414 AFIX 137 H10A 2 0.206779 0.315284 0.796222 11.00000 -1.50000 H10B 2 0.173006 0.233034 0.840746 11.00000 -1.50000 H10C 2 0.127512 0.285338 0.780799 11.00000 -1.50000 AFIX 0 C11 1 0.252667 0.045983 0.799625 11.00000 0.02600 0.03899 = 0.01919 0.00687 0.00359 0.00021 AFIX 137 H11A 2 0.259740 -0.040620 0.779125 11.00000 -1.50000 H11B 2 0.255537 0.023283 0.839924 11.00000 -1.50000 H11C 2 0.287285 0.116055 0.796909 11.00000 -1.50000 AFIX 0 C12 1 0.352327 0.446394 0.875345 11.00000 0.02114 0.02075 = 0.01953 -0.00160 0.00476 -0.00304 C13 1 0.295228 0.522674 0.879607 11.00000 0.01854 0.03614 = 0.01891 0.00550 0.00076 -0.00164 AFIX 43 H13 2 0.260066 0.536868 0.846488 11.00000 -1.20000 AFIX 0 C14 1 0.289134 0.578280 0.931817 11.00000 0.02391 0.04405 = 0.02526 -0.00202 0.01139 -0.00244 AFIX 43 H14 2 0.249805 0.629714 0.934050 11.00000 -1.20000 AFIX 0 C15 1 0.339912 0.559283 0.980552 11.00000 0.03279 0.04446 = 0.01879 -0.00425 0.00710 -0.00097 AFIX 43 H15 2 0.335863 0.598495 1.016036 11.00000 -1.20000 AFIX 0 C16 1 0.396431 0.482849 0.977057 11.00000 0.03722 0.03436 = 0.01504 0.00074 0.00138 -0.00367 AFIX 43 H16 2 0.431302 0.468448 1.010367 11.00000 -1.20000 AFIX 0 C17 1 0.402555 0.426859 0.925024 11.00000 0.02819 0.02571 = 0.02345 0.00340 0.00444 0.00295 AFIX 43 H17 2 0.441708 0.374245 0.923241 11.00000 -1.20000 AFIX 0 C18 1 0.305118 0.456030 0.581156 11.00000 0.01779 0.03002 = 0.02147 0.00053 0.00484 -0.00597 C19 1 0.263332 0.570431 0.560164 11.00000 0.05298 0.01836 = 0.02722 0.00221 0.01064 0.00309 AFIX 43 H19 2 0.260238 0.648033 0.584719 11.00000 -1.20000 AFIX 0 C20 1 0.225894 0.572807 0.503541 11.00000 0.05214 0.03591 = 0.02886 0.01330 0.00371 0.00376 AFIX 43 H20 2 0.198167 0.652414 0.489991 11.00000 -1.20000 AFIX 0 C21 1 0.228785 0.460691 0.467099 11.00000 0.04301 0.05460 = 0.01503 0.00538 0.00584 -0.00875 AFIX 43 H21 2 0.202133 0.461303 0.429034 11.00000 -1.20000 AFIX 0 C22 1 0.270861 0.347888 0.486698 11.00000 0.04189 0.04206 = 0.02541 -0.00594 0.01658 -0.00902 AFIX 43 H22 2 0.274313 0.271662 0.461607 11.00000 -1.20000 AFIX 0 C23 1 0.308561 0.344865 0.543348 11.00000 0.02692 0.02921 = 0.03207 0.00269 0.01461 -0.00281 AFIX 43 H23 2 0.336972 0.265876 0.556305 11.00000 -1.20000 AFIX 0 C24 1 0.121528 0.616685 0.671255 11.00000 0.02369 0.01540 = 0.01739 -0.00163 0.00323 -0.00025 C25 1 0.062598 0.673454 0.682817 11.00000 0.02734 0.02312 = 0.03108 -0.00080 0.01230 -0.00740 AFIX 43 H25 2 0.063917 0.717479 0.718641 11.00000 -1.20000 AFIX 0 C26 1 0.001846 0.665260 0.641592 11.00000 0.02270 0.03203 = 0.04987 0.00503 0.01517 -0.00377 AFIX 43 H26 2 -0.037683 0.705450 0.649518 11.00000 -1.20000 AFIX 0 C27 1 -0.001562 0.600030 0.589834 11.00000 0.03164 0.02889 = 0.03410 0.00613 -0.00850 -0.00650 AFIX 43 H27 2 -0.043097 0.594658 0.562205 11.00000 -1.20000 AFIX 0 C28 1 0.056403 0.542120 0.578431 11.00000 0.04454 0.02801 = 0.02491 -0.00094 -0.00276 0.00204 AFIX 43 H28 2 0.054570 0.495979 0.542936 11.00000 -1.20000 AFIX 0 C29 1 0.116991 0.551408 0.618693 11.00000 0.03646 0.01968 = 0.02639 -0.00112 0.00631 0.00813 AFIX 43 H29 2 0.156358 0.512152 0.610108 11.00000 -1.20000 AFIX 0 O1 4 0.104933 0.645952 0.915669 11.00000 0.08308 0.08304 = 0.03249 -0.01151 -0.00960 0.04197 C41 1 0.061684 0.759430 0.896533 11.00000 0.04240 0.03848 = 0.04029 0.01004 0.00957 0.00553 AFIX 23 H41A 2 0.088310 0.845068 0.892390 11.00000 -1.20000 H41B 2 0.034858 0.780506 0.924977 11.00000 -1.20000 AFIX 0 C42 1 0.015024 0.723694 0.839562 11.00000 0.03533 0.05704 = 0.05023 0.02089 0.00509 -0.00667 AFIX 23 H42A 2 0.020528 0.791048 0.809321 11.00000 -1.20000 H42B 2 -0.032635 0.722988 0.842173 11.00000 -1.20000 AFIX 0 C43 1 0.039813 0.571632 0.828614 11.00000 0.05118 0.04866 = 0.03901 -0.00087 0.00995 -0.01245 AFIX 23 H43A 2 0.010883 0.497452 0.839693 11.00000 -1.20000 H43B 2 0.040986 0.558465 0.787978 11.00000 -1.20000 AFIX 0 C44 1 0.107993 0.569082 0.865974 11.00000 0.04822 0.08693 = 0.03571 -0.01901 0.00187 0.01578 AFIX 23 H44A 2 0.122386 0.469987 0.875884 11.00000 -1.20000 H44B 2 0.140501 0.613749 0.846511 11.00000 -1.20000 AFIX 0 N3 3 0.428678 0.892217 0.840032 11.00000 0.02315 0.01887 = 0.01497 -0.00101 0.00778 -0.00045 N4 3 0.412796 0.904859 0.747435 11.00000 0.01726 0.01780 = 0.01497 0.00008 0.00221 -0.00062 C30 1 0.440722 0.968930 0.796821 11.00000 0.02455 0.01138 = 0.01650 -0.00191 0.00239 -0.00376 AFIX 43 H30 2 0.465290 1.055497 0.800570 11.00000 -1.20000 AFIX 0 C31 1 0.392175 0.774549 0.817169 11.00000 0.02505 0.01881 = 0.02196 0.00048 0.00737 -0.00163 AFIX 43 H31 2 0.376640 0.701495 0.838190 11.00000 -1.20000 AFIX 0 C32 1 0.382270 0.780925 0.759690 11.00000 0.02265 0.01900 = 0.02039 -0.00382 0.00645 -0.00477 AFIX 43 H32 2 0.358917 0.713558 0.732864 11.00000 -1.20000 AFIX 0 C33 1 0.451795 0.924262 0.902557 11.00000 0.02277 0.02983 = 0.01049 -0.00390 0.00459 0.00559 C34 1 0.496201 0.801047 0.929285 11.00000 0.03652 0.03817 = 0.01425 -0.00020 0.00142 0.00863 AFIX 137 H34A 2 0.470412 0.712386 0.922441 11.00000 -1.50000 H34B 2 0.511658 0.816797 0.970562 11.00000 -1.50000 H34C 2 0.535166 0.794506 0.912086 11.00000 -1.50000 AFIX 0 C35 1 0.389680 0.939784 0.926404 11.00000 0.02333 0.05952 = 0.01817 -0.00517 0.00536 0.00641 AFIX 137 H35A 2 0.403254 0.957066 0.967696 11.00000 -1.50000 H35B 2 0.362963 0.852380 0.919211 11.00000 -1.50000 H35C 2 0.362653 1.019943 0.907727 11.00000 -1.50000 AFIX 0 C36 1 0.492231 1.062194 0.908845 11.00000 0.04300 0.03402 = 0.01732 -0.01324 0.00909 -0.00602 AFIX 137 H36A 2 0.530967 1.050426 0.891651 11.00000 -1.50000 H36B 2 0.508048 1.085319 0.949511 11.00000 -1.50000 H36C 2 0.463629 1.139362 0.889407 11.00000 -1.50000 AFIX 0 C37 1 0.411003 0.960414 0.688898 11.00000 0.02405 0.02331 = 0.01546 0.00244 0.00536 0.00245 C38 1 0.457916 1.087118 0.693582 11.00000 0.03967 0.02377 = 0.02462 0.00891 0.01200 -0.00311 AFIX 137 H38A 2 0.503238 1.059200 0.714279 11.00000 -1.50000 H38B 2 0.441538 1.163969 0.714325 11.00000 -1.50000 H38C 2 0.459271 1.120018 0.655167 11.00000 -1.50000 AFIX 0 C39 1 0.338826 1.000597 0.662395 11.00000 0.03197 0.05127 = 0.02154 0.01336 0.00519 0.00869 AFIX 137 H39A 2 0.324893 1.077609 0.684578 11.00000 -1.50000 H39B 2 0.309716 0.917853 0.662492 11.00000 -1.50000 H39C 2 0.335105 1.032364 0.622942 11.00000 -1.50000 AFIX 0 C40 1 0.435669 0.840651 0.655571 11.00000 0.03128 0.03235 = 0.02134 -0.00652 0.01299 -0.00400 AFIX 137 H40A 2 0.407699 0.756070 0.655664 11.00000 -1.50000 H40B 2 0.482587 0.818025 0.673695 11.00000 -1.50000 H40C 2 0.432483 0.871325 0.616056 11.00000 -1.50000 AFIX 0 HKLF 4 REM REM R1 = 0.0561 for 6379 Fo > 4sig(Fo) and 0.0675 for all 7709 data REM 490 parameters refined using 0 restraints END WGHT 0.0863 0.0000 REM Highest difference peak 0.973, deepest hole -1.031, 1-sigma level 0.132 Q1 1 0.0028 0.6594 0.8012 11.00000 0.05 0.97 Q2 1 0.3572 0.5265 0.6934 11.00000 0.05 0.84 Q3 1 0.4096 0.4474 0.6328 11.00000 0.05 0.81 Q4 1 0.3673 0.4500 0.7660 11.00000 0.05 0.80 Q5 1 0.2576 0.6312 0.7034 11.00000 0.05 0.78 Q6 1 0.2038 0.5570 0.7682 11.00000 0.05 0.78 Q7 1 0.3128 0.3847 0.8358 11.00000 0.05 0.77 Q8 1 0.1967 0.6051 0.6863 11.00000 0.05 0.74 Q9 1 0.2942 0.2337 0.7283 11.00000 0.05 0.73 Q10 1 0.4196 0.3861 0.7770 11.00000 0.05 0.72 Q11 1 0.2031 0.7020 0.6933 11.00000 0.05 0.71 Q12 1 0.2538 0.7099 0.7534 11.00000 0.05 0.70 Q13 1 0.3585 0.4001 0.6967 11.00000 0.05 0.68 Q14 1 0.4191 0.3736 0.7612 11.00000 0.05 0.68 Q15 1 0.1583 0.5852 0.6994 11.00000 0.05 0.67 Q16 1 0.4040 0.5299 0.6830 11.00000 0.05 0.67 Q17 1 0.3515 0.5516 0.7970 11.00000 0.05 0.67 Q18 1 0.2544 0.5763 0.7572 11.00000 0.05 0.65 Q19 1 0.2194 0.3485 0.6911 11.00000 0.05 0.64 Q20 1 0.5677 1.0803 0.7616 11.00000 0.05 0.63 Q21 1 0.3016 0.3778 0.6434 11.00000 0.05 0.60 Q22 1 0.2187 0.4302 0.7420 11.00000 0.05 0.60 Q23 1 0.3534 0.3999 0.6197 11.00000 0.05 0.59 Q24 1 0.3687 0.4251 0.8423 11.00000 0.05 0.58 Q25 1 0.3537 0.5158 0.6197 11.00000 0.05 0.58 Q26 1 0.3182 0.2942 0.7796 11.00000 0.05 0.56 Q27 1 0.2785 0.2650 0.8412 11.00000 0.05 0.56 Q28 1 0.2726 0.3391 0.6838 11.00000 0.05 0.56 ; _shelx_res_checksum 73830 _shelx_hkl_file ; 0 0 -2 594776. 4820.80 3 0 0 -3 146.170 124.667 3 0 0 -3 304.359 227.282 6 0 0 -4 1285.71 348.725 3 0 0 -4 1610.49 533.272 6 0 0 -5 193.860 208.410 3 0 0 -5 186.582 284.864 6 0 0 -6 13461.8 1725.85 6 0 0 -6 26565.4 1889.96 3 0 0 -7-717.144 471.279 6 0 0 -7 550.018 347.281 3 0 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3 3 64.5852 358.309 4 -24 3 2 5107.13 1412.00 4 -24 3 1 688.619 595.306 4 -25 0 10-90.1156 287.065 5 -25 0 9 302.873 409.149 5 -25 0 8-184.140 444.110 5 -25 0 7-59.0737 414.585 5 -25 0 6 871.423 644.000 5 -25 0 5-338.105 509.044 5 -25 0 4 3354.27 1126.08 5 -25 0 3-301.257 500.061 5 -25 0 2 22454.8 2736.75 5 -25 -1 11-513.185 465.006 5 -25 -1 10 5931.66 1300.15 5 -25 -1 9 1554.11 794.060 5 -25 -1 8 11502.6 1972.46 5 -25 -1 7 2970.37 1111.62 5 -25 -1 6 7654.60 1723.14 5 -25 -1 5 2181.79 974.131 5 -25 -1 4 2346.20 1027.15 5 -25 -1 3 2997.65 1120.39 5 0 0 0 0.00 0.00 0 TITL xral8 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 1.54184 20.428112 9.409030 24.027989 90.0000 103.3807 90.0000 ZERR 4.00 0.000351 0.000168 0.000371 0.0000 0.0016 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N O Fe Se UNIT 160.00 200.00 16.00 8.00 4.00 12.00 TREF HKLF 4 END ; _shelx_hkl_checksum 68436 _database_code_depnum_ccdc_archive 'CCDC 971590'