# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matouzenko, Galina' _publ_contact_author_email Galina.Matouzenko@ens-lyon.fr _publ_section_title ; Spin crossover and polymorphism in a family of 1,2-bis(4-pyridyl)ethene-bridged iron(II) complexes. A key role of structural distortion in the spin crossover of binuclear compounds ; loop_ _publ_author_name G.Matouzenko E.Jeanneau A.Verat A.Bousseksou # Attachment '- compound 2.txt' data_2 _database_code_depnum_ccdc_archive 'CCDC 807891' #TrackingRef '- compound 2.txt' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 10.3050(10) _cell_length_b 16.467(2) _cell_length_c 14.0430(10) _cell_angle_alpha 90 _cell_angle_beta 96.612(9) _cell_angle_gamma 90 _cell_volume 2367.1(4) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1 ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C25 H25 Fe2.50 N2.50 O2.50 S2.50 # Dc = 1.74 Fooo = 1024.00 Mu = 17.72 M = 620.27 # Found Formula = C21 H22 Fe1 N6 O1 S2 # Dc = 1.39 FOOO = 1024.00 Mu = 8.38 M = 494.42 _chemical_formula_sum 'C42 H44 Fe2 N12 O2 S4' _chemical_formula_moiety 'C40 H36 Fe2 N12 S4, 2(C H4 O)' _chemical_compound_source ? _chemical_formula_weight 988.87 _cell_measurement_reflns_used 7944 _cell_measurement_theta_min 3.5546 _cell_measurement_theta_max 29.4874 _cell_measurement_temperature 290 _exptl_crystal_description needle _exptl_crystal_colour 'dark brown' _exptl_crystal_size_min 0.141 _exptl_crystal_size_mid 0.216 _exptl_crystal_size_max 0.687 _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1024 _exptl_absorpt_coefficient_mu 0.838 # Sheldrick geometric approximatio 0.83 0.89 # No experimental values of Tmin/max available _exptl_absorpt_correction_T_min 0.731 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.4685 # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 290 _diffrn_reflns_number 21686 _reflns_number_total 5911 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 5911 # Theoretical number of reflections is about 13255 _diffrn_reflns_theta_min 3.562 _diffrn_reflns_theta_max 29.550 _diffrn_measured_fraction_theta_max 0.893 _diffrn_reflns_theta_full 26.300 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.82 _refine_diff_density_max 1.04 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5911 _refine_ls_number_restraints 0 _refine_ls_number_parameters 280 _oxford_refine_ls_R_factor_ref 0.0942 _refine_ls_wR_factor_ref 0.2112 _refine_ls_goodness_of_fit_ref 1.0006 _refine_ls_shift/su_max 0.0001703 _refine_ls_shift/su_mean 0.0000110 # The values computed from all data _oxford_reflns_number_all 5911 _refine_ls_R_factor_all 0.0942 _refine_ls_wR_factor_all 0.2112 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3130 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_gt 0.1386 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.131E+04 0.218E+04 0.134E+04 570. 136. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. De Meulenaer, J. & Tompa, H. (1965). Acta Cryst. 19, 1014. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2006). Gemini User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens C1 C 0.3164(5) 0.0977(3) 0.2045(3) 0.0636 1.0000 Uani . . . . . . . C2 C 0.7248(5) 0.1666(3) 0.3106(3) 0.0651 1.0000 Uani . . . . . . . C3 C 0.3597(5) 0.0739(3) 0.4863(4) 0.0677 1.0000 Uani . . . . . . . C4 C 0.3619(6) 0.0255(4) 0.5655(5) 0.0817 1.0000 Uani . . . . . . . C5 C 0.4501(7) 0.0430(4) 0.6437(4) 0.0911 1.0000 Uani . . . . . . . C6 C 0.5289(7) 0.1084(4) 0.6418(4) 0.0879 1.0000 Uani . . . . . . . C7 C 0.5207(5) 0.1566(3) 0.5591(3) 0.0692 1.0000 Uani . . . . . . . C8 C 0.6078(6) 0.2285(4) 0.5505(4) 0.0872 1.0000 Uani . . . . . . . C9 C 0.4535(7) 0.3442(4) 0.5273(5) 0.0919 1.0000 Uani . . . . . . . C10 C 0.3117(6) 0.3297(3) 0.4943(3) 0.0675 1.0000 Uani . . . . . . . C11 C 0.2173(8) 0.3668(4) 0.5420(4) 0.0920 1.0000 Uani . . . . . . . C12 C 0.0870(8) 0.3556(4) 0.5078(5) 0.1011 1.0000 Uani . . . . . . . C13 C 0.0545(7) 0.3069(4) 0.4303(6) 0.0984 1.0000 Uani . . . . . . . C14 C 0.1543(6) 0.2723(3) 0.3867(4) 0.0749 1.0000 Uani . . . . . . . C15 C 0.4885(7) 0.3022(3) 0.1663(4) 0.0856 1.0000 Uani . . . . . . . C16 C 0.4998(7) 0.3588(3) 0.0964(4) 0.0857 1.0000 Uani . . . . . . . C17 C 0.4684(5) 0.4389(3) 0.1116(3) 0.0611 1.0000 Uani . . . . . . . C18 C 0.4219(5) 0.4552(3) 0.1972(4) 0.0694 1.0000 Uani . . . . . . . C19 C 0.4124(5) 0.3946(3) 0.2633(3) 0.0664 1.0000 Uani . . . . . . . C20 C 0.4815(5) 0.5046(3) 0.0431(3) 0.0639 1.0000 Uani . . . . . . . C21 C 0.7681(8) 0.4225(5) 0.3364(6) 0.1196 1.0000 Uani . . . . . . . N1 N 0.3222(5) 0.1471(3) 0.2625(3) 0.0746 1.0000 Uani . . . . . . . N2 N 0.6204(5) 0.1796(3) 0.3257(4) 0.0801 1.0000 Uani . . . . . . . N3 N 0.4377(4) 0.1387(2) 0.4824(3) 0.0590 1.0000 Uani . . . . . . . N4 N 0.5427(4) 0.2897(3) 0.4842(3) 0.0716 1.0000 Uani . . . . . . . N5 N 0.2811(4) 0.2832(2) 0.4180(3) 0.0616 1.0000 Uani . . . . . . . N6 N 0.4455(4) 0.3186(2) 0.2497(3) 0.0633 1.0000 Uani . . . . . . . Fe1 Fe 0.43974(7) 0.22201(4) 0.35937(4) 0.0560 1.0000 Uani . . . . . . . S1 S 0.3125(2) 0.02540(11) 0.12682(11) 0.1027 1.0000 Uani . . . . . . . S2 S 0.87083(18) 0.14799(19) 0.28827(15) 0.1300 1.0000 Uani . . . . . . . O1 O 0.7281(8) 0.3983(5) 0.4183(5) 0.1936 1.0000 Uani . . . . . . . H31 H 0.3009 0.0621 0.4314 0.0811 1.0000 Uiso R . . . . . . H41 H 0.3047 -0.0187 0.5667 0.0980 1.0000 Uiso R . . . . . . H51 H 0.4566 0.0103 0.6977 0.1088 1.0000 Uiso R . . . . . . H61 H 0.5874 0.1218 0.6940 0.1060 1.0000 Uiso R . . . . . . H81 H 0.6288 0.2529 0.6128 0.1049 1.0000 Uiso R . . . . . . H82 H 0.6875 0.2111 0.5266 0.1051 1.0000 Uiso R . . . . . . H91 H 0.4684 0.3376 0.5967 0.1101 1.0000 Uiso R . . . . . . H92 H 0.4739 0.3995 0.5110 0.1102 1.0000 Uiso R . . . . . . H111 H 0.2420 0.3985 0.5967 0.1099 1.0000 Uiso R . . . . . . H121 H 0.0213 0.3811 0.5376 0.1210 1.0000 Uiso R . . . . . . H131 H -0.0325 0.2982 0.4066 0.1180 1.0000 Uiso R . . . . . . H141 H 0.1331 0.2399 0.3329 0.0902 1.0000 Uiso R . . . . . . H151 H 0.5130 0.2494 0.1552 0.1028 1.0000 Uiso R . . . . . . H161 H 0.5299 0.3429 0.0395 0.1027 1.0000 Uiso R . . . . . . H181 H 0.3955 0.5079 0.2099 0.0831 1.0000 Uiso R . . . . . . H191 H 0.3813 0.4081 0.3216 0.0802 1.0000 Uiso R . . . . . . H201 H 0.4640 0.5572 0.0630 0.0770 1.0000 Uiso R . . . . . . H4 H 0.6039 0.3199 0.4626 0.1070 1.0000 Uiso R . . . . . . H211 H 0.8546 0.4469 0.3496 0.1790 1.0000 Uiso R . . . . . . H213 H 0.7710 0.3760 0.2944 0.1790 1.0000 Uiso R . . . . . . H212 H 0.7069 0.4621 0.3064 0.1791 1.0000 Uiso R . . . . . . H1 H 0.7310 0.4289 0.4659 0.2901 1.0000 Uiso R . . . . . . 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 C1 0.080(3) 0.062(3) 0.049(2) 0.008(2) 0.008(2) -0.014(2) C2 0.079(3) 0.065(3) 0.052(2) 0.003(2) 0.012(2) 0.008(2) C3 0.064(3) 0.066(3) 0.074(3) 0.014(2) 0.013(2) -0.001(2) C4 0.087(4) 0.073(3) 0.090(4) 0.026(3) 0.031(3) 0.011(3) C5 0.121(5) 0.084(4) 0.073(4) 0.030(3) 0.031(4) 0.025(4) C6 0.106(4) 0.103(5) 0.053(3) 0.006(3) -0.002(3) 0.019(4) C7 0.076(3) 0.079(3) 0.053(2) 0.003(2) 0.008(2) 0.005(3) C8 0.079(4) 0.106(5) 0.074(3) -0.001(3) -0.007(3) -0.014(3) C9 0.117(5) 0.081(4) 0.082(4) -0.023(3) 0.028(3) -0.014(3) C10 0.096(4) 0.055(2) 0.057(2) 0.010(2) 0.030(2) 0.006(2) C11 0.137(6) 0.073(3) 0.074(3) 0.011(3) 0.048(4) 0.027(4) C12 0.115(6) 0.094(4) 0.102(5) 0.020(4) 0.048(4) 0.044(4) C13 0.088(4) 0.098(4) 0.115(5) 0.029(4) 0.032(4) 0.023(4) C14 0.083(3) 0.069(3) 0.074(3) 0.018(2) 0.017(3) 0.011(3) C15 0.146(6) 0.057(3) 0.061(3) 0.003(2) 0.045(3) 0.013(3) C16 0.143(5) 0.066(3) 0.055(3) 0.008(2) 0.042(3) 0.010(3) C17 0.075(3) 0.058(2) 0.052(2) 0.0087(19) 0.016(2) 0.004(2) C18 0.090(3) 0.055(2) 0.067(3) 0.012(2) 0.028(3) 0.013(2) C19 0.088(3) 0.061(3) 0.055(2) 0.010(2) 0.027(2) 0.010(2) C20 0.079(3) 0.060(2) 0.056(2) 0.008(2) 0.018(2) 0.006(2) C21 0.114(6) 0.122(6) 0.121(6) 0.023(5) 0.009(5) -0.012(5) N1 0.101(3) 0.065(2) 0.058(2) -0.0036(19) 0.006(2) -0.002(2) N2 0.089(3) 0.075(3) 0.082(3) 0.014(2) 0.034(3) 0.011(2) N3 0.060(2) 0.065(2) 0.0526(19) 0.0101(16) 0.0096(16) 0.0008(17) N4 0.076(3) 0.073(3) 0.068(2) -0.007(2) 0.019(2) -0.017(2) N5 0.073(2) 0.059(2) 0.056(2) 0.0115(16) 0.0213(18) 0.0046(18) N6 0.086(3) 0.053(2) 0.054(2) 0.0077(16) 0.0230(19) 0.0028(18) Fe1 0.0689(4) 0.0534(3) 0.0477(3) 0.0035(2) 0.0146(3) -0.0006(3) S1 0.1565(17) 0.0887(10) 0.0673(9) -0.0199(7) 0.0313(10) -0.0430(11) S2 0.0726(10) 0.225(3) 0.0921(12) -0.0116(15) 0.0062(9) 0.0344(13) O1 0.220(8) 0.243(8) 0.126(5) -0.031(5) 0.058(5) -0.149(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 3.04(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . N1 . 1.148(6) yes C1 . S1 . 1.613(5) yes C2 . N2 . 1.140(7) yes C2 . S2 . 1.602(6) yes C3 . C4 . 1.366(7) yes C3 . N3 . 1.341(6) yes C3 . H31 . 0.944 no C4 . C5 . 1.373(9) yes C4 . H41 . 0.939 no C5 . C6 . 1.350(9) yes C5 . H51 . 0.927 no C6 . C7 . 1.402(7) yes C6 . H61 . 0.920 no C7 . C8 . 1.499(8) yes C7 . N3 . 1.329(6) yes C8 . N4 . 1.479(8) yes C8 . H81 . 0.965 no C8 . H82 . 0.965 no C9 . C10 . 1.500(9) yes C9 . N4 . 1.464(7) yes C9 . H91 . 0.976 no C9 . H92 . 0.968 no C10 . C11 . 1.386(7) yes C10 . N5 . 1.325(6) yes C11 . C12 . 1.385(10) yes C11 . H111 . 0.940 no C12 . C13 . 1.362(10) yes C12 . H121 . 0.936 no C13 . C14 . 1.380(8) yes C13 . H131 . 0.931 no C14 . N5 . 1.342(7) yes C14 . H141 . 0.930 no C15 . C16 . 1.368(7) yes C15 . N6 . 1.327(6) yes C15 . H151 . 0.925 no C16 . C17 . 1.381(7) yes C16 . H161 . 0.928 no C17 . C18 . 1.371(6) yes C17 . C20 . 1.464(6) yes C18 . C19 . 1.375(6) yes C18 . H181 . 0.933 no C19 . N6 . 1.316(6) yes C19 . H191 . 0.940 no C20 . C20 2_665 1.318(9) yes C20 . H201 . 0.934 no C21 . O1 . 1.326(9) yes C21 . H211 . 0.976 no C21 . H213 . 0.968 no C21 . H212 . 0.969 no N1 . Fe1 . 2.111(4) yes N2 . Fe1 . 2.093(5) yes N3 . Fe1 . 2.208(4) yes N4 . Fe1 . 2.239(4) yes N4 . H4 . 0.884 no N5 . Fe1 . 2.163(4) yes N6 . Fe1 . 2.219(4) yes O1 . H1 . 0.835 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . C1 . S1 . 177.1(5) yes N2 . C2 . S2 . 179.4(5) yes C4 . C3 . N3 . 122.9(5) yes C4 . C3 . H31 . 119.6 no N3 . C3 . H31 . 117.5 no C3 . C4 . C5 . 118.4(6) yes C3 . C4 . H41 . 121.1 no C5 . C4 . H41 . 120.5 no C4 . C5 . C6 . 119.7(5) yes C4 . C5 . H51 . 120.8 no C6 . C5 . H51 . 119.5 no C5 . C6 . C7 . 119.3(6) yes C5 . C6 . H61 . 121.1 no C7 . C6 . H61 . 119.6 no C6 . C7 . C8 . 122.3(5) yes C6 . C7 . N3 . 121.2(5) yes C8 . C7 . N3 . 116.4(4) yes C7 . C8 . N4 . 110.9(4) yes C7 . C8 . H81 . 109.3 no N4 . C8 . H81 . 108.9 no C7 . C8 . H82 . 109.6 no N4 . C8 . H82 . 109.0 no H81 . C8 . H82 . 109.1 no C10 . C9 . N4 . 114.2(5) yes C10 . C9 . H91 . 109.0 no N4 . C9 . H91 . 108.1 no C10 . C9 . H92 . 107.9 no N4 . C9 . H92 . 108.4 no H91 . C9 . H92 . 109.1 no C9 . C10 . C11 . 119.6(6) yes C9 . C10 . N5 . 118.3(5) yes C11 . C10 . N5 . 122.1(6) yes C10 . C11 . C12 . 118.7(6) yes C10 . C11 . H111 . 120.1 no C12 . C11 . H111 . 121.2 no C11 . C12 . C13 . 119.7(6) yes C11 . C12 . H121 . 120.4 no C13 . C12 . H121 . 119.9 no C12 . C13 . C14 . 118.1(7) yes C12 . C13 . H131 . 120.9 no C14 . C13 . H131 . 121.0 no C13 . C14 . N5 . 123.1(6) yes C13 . C14 . H141 . 118.6 no N5 . C14 . H141 . 118.2 no C16 . C15 . N6 . 124.0(5) yes C16 . C15 . H151 . 118.2 no N6 . C15 . H151 . 117.7 no C15 . C16 . C17 . 120.0(5) yes C15 . C16 . H161 . 119.4 no C17 . C16 . H161 . 120.7 no C16 . C17 . C18 . 115.7(4) yes C16 . C17 . C20 . 124.3(4) yes C18 . C17 . C20 . 120.0(4) yes C17 . C18 . C19 . 120.6(4) yes C17 . C18 . H181 . 119.3 no C19 . C18 . H181 . 120.1 no C18 . C19 . N6 . 123.6(4) yes C18 . C19 . H191 . 118.3 no N6 . C19 . H191 . 118.1 no C17 . C20 . C20 2_665 125.2(6) yes C17 . C20 . H201 . 116.9 no C20 2_665 C20 . H201 . 117.9 no O1 . C21 . H211 . 109.1 no O1 . C21 . H213 . 109.0 no H211 . C21 . H213 . 110.5 no O1 . C21 . H212 . 109.1 no H211 . C21 . H212 . 109.8 no H213 . C21 . H212 . 109.4 no C1 . N1 . Fe1 . 148.2(5) yes C2 . N2 . Fe1 . 170.9(5) yes C3 . N3 . C7 . 118.4(4) yes C3 . N3 . Fe1 . 125.9(3) yes C7 . N3 . Fe1 . 115.7(3) yes C8 . N4 . C9 . 114.7(5) yes C8 . N4 . Fe1 . 107.0(3) yes C9 . N4 . Fe1 . 111.4(4) yes C8 . N4 . H4 . 108.0 no C9 . N4 . H4 . 107.6 no Fe1 . N4 . H4 . 107.8 no C14 . N5 . C10 . 118.4(5) yes C14 . N5 . Fe1 . 124.2(4) yes C10 . N5 . Fe1 . 117.2(4) yes C15 . N6 . C19 . 116.0(4) yes C15 . N6 . Fe1 . 120.3(3) yes C19 . N6 . Fe1 . 123.6(3) yes N3 . Fe1 . N6 . 172.54(15) yes N3 . Fe1 . N5 . 85.18(14) yes N6 . Fe1 . N5 . 90.68(14) yes N3 . Fe1 . N4 . 75.11(15) yes N6 . Fe1 . N4 . 97.95(16) yes N5 . Fe1 . N4 . 77.33(16) yes N3 . Fe1 . N1 . 94.86(16) yes N6 . Fe1 . N1 . 91.77(16) yes N5 . Fe1 . N1 . 96.59(18) yes N4 . Fe1 . N1 . 168.54(16) yes N3 . Fe1 . N2 . 93.33(16) yes N6 . Fe1 . N2 . 89.26(16) yes N5 . Fe1 . N2 . 166.58(19) yes N4 . Fe1 . N2 . 89.38(19) yes N1 . Fe1 . N2 . 96.8(2) yes C21 . O1 . H1 . 121.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag N4 . H4 . O1 . 173 0.88 1.97 2.849(8) yes # Attachment '- compound 1(183K).txt' data_1(183K) _database_code_depnum_ccdc_archive 'CCDC 807892' #TrackingRef '- compound 1(183K).txt' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 21.017(3) _cell_length_b 12.4290(10) _cell_length_c 19.390(3) _cell_angle_alpha 90 _cell_angle_beta 114.08(2) _cell_angle_gamma 90 _cell_volume 4624.3(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C40 H40 Fe2 N16 O4 S4 # Dc = 1.51 Fooo = 1904.00 Mu = 8.68 M = 524.41 # Found Formula = C40 H36 Fe2 N12 S4 # Dc = 1.33 FOOO = 1904.00 Mu = 8.50 M = 462.38 _chemical_formula_sum 'C40 H36 Fe2 N12 S4' _chemical_formula_moiety 'C40 H36 Fe2 N12 S4' _chemical_compound_source ? _chemical_formula_weight 924.79 _cell_measurement_reflns_used 5576 _cell_measurement_theta_min 3.3412 _cell_measurement_theta_max 29.4941 _cell_measurement_temperature 183 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_max 0.3 _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 2230 _exptl_absorpt_coefficient_mu 0.868 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details ; Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897 ; # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 183 _diffrn_reflns_number 5693 _reflns_number_total 5693 _diffrn_reflns_av_R_equivalents 0.062 # Number of reflections without Friedels Law is 10570 # Number of reflections with Friedels Law is 5693 # Theoretical number of reflections is about 6436 _diffrn_reflns_theta_min 3.341 _diffrn_reflns_theta_max 29.488 _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 26.539 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -28 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.20 _refine_diff_density_max 1.33 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5693 _refine_ls_number_restraints 0 _refine_ls_number_parameters 262 _oxford_refine_ls_R_factor_ref 0.1006 _refine_ls_wR_factor_ref 0.1018 _refine_ls_goodness_of_fit_ref 0.9792 _refine_ls_shift/su_max 0.0009257 _refine_ls_shift/su_mean 0.2730211 # The values computed from all data _oxford_reflns_number_all 5693 _refine_ls_R_factor_all 0.1006 _refine_ls_wR_factor_all 0.1018 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3574 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_gt 0.0880 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 763. 0.106E+04 496. 120. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Oxford Diffraction, (2002). CrysAlis RED. Oxford Diffraction, (2002). Xcalibur User Manual. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens C1 C 0.6989(2) 0.4327(3) 0.8439(3) 0.0508 1.0000 Uani . . . . . . . C3 C 0.6154(2) 0.7086(4) 0.8234(3) 0.0582 1.0000 Uani . . . . . . . C4 C 0.5855(2) 0.7869(5) 0.8500(3) 0.0630 1.0000 Uani . . . . . . . C5 C 0.5774(2) 0.8889(5) 0.8195(3) 0.0624 1.0000 Uani . . . . . . . C6 C 0.5984(2) 0.9071(4) 0.7623(3) 0.0533 1.0000 Uani . . . . . . . C7 C 0.6271(2) 0.8250(3) 0.7378(2) 0.0464 1.0000 Uani . . . . . . . C8 C 0.6532(2) 0.8392(3) 0.6772(2) 0.0531 1.0000 Uani . . . . . . . C9 C 0.5884(2) 0.7118(4) 0.5726(2) 0.0584 1.0000 Uani . . . . . . . C10 C 0.54497(19) 0.6299(3) 0.5895(2) 0.0426 1.0000 Uani . . . . . . . C11 C 0.4754(2) 0.6124(4) 0.5396(2) 0.0520 1.0000 Uani . . . . . . . C12 C 0.4385(2) 0.5330(4) 0.5556(3) 0.0581 1.0000 Uani . . . . . . . C13 C 0.4695(2) 0.4726(4) 0.6202(3) 0.0520 1.0000 Uani . . . . . . . C14 C 0.5379(2) 0.4952(3) 0.6671(2) 0.0469 1.0000 Uani . . . . . . . C15 C 0.6854(2) 0.4065(3) 0.6410(2) 0.0427 1.0000 Uani . . . . . . . C16 C 0.7003(2) 0.3373(3) 0.5943(2) 0.0431 1.0000 Uani . . . . . . . C17 C 0.73986(19) 0.3704(3) 0.5571(2) 0.0394 1.0000 Uani . . . . . . . C18 C 0.7636(2) 0.4769(3) 0.5695(2) 0.0444 1.0000 Uani . . . . . . . C19 C 0.74713(19) 0.5402(3) 0.6176(2) 0.0448 1.0000 Uani . . . . . . . H191 H 0.7642 0.6098 0.6274 0.0540 1.0000 Uiso R . . . . . . Fe1 Fe 0.67778(3) 0.61143(5) 0.71958(4) 0.0460 1.0000 Uani . . . . . . . N2 N 0.7773(2) 0.6554(3) 0.7705(2) 0.0601 1.0000 Uani . . . . . . . N5 N 0.57503(16) 0.5719(2) 0.65253(19) 0.0431 1.0000 Uani . . . . . . . N4 N 0.65368(17) 0.7360(3) 0.63862(19) 0.0476 1.0000 Uani . . . . . . . N3 N 0.63684(16) 0.7252(3) 0.7684(2) 0.0488 1.0000 Uani . . . . . . . N6 N 0.70750(16) 0.5094(2) 0.65287(18) 0.0396 1.0000 Uani . . . . . . . N1 N 0.68765(17) 0.4980(3) 0.7975(2) 0.0573 1.0000 Uani . . . . . . . S1 S 0.71429(8) 0.34180(11) 0.90926(8) 0.0716 1.0000 Uani . . . . . . . H31 H 0.6206 0.6396 0.8448 0.0689 1.0000 Uiso R . . . . . . H41 H 0.5707 0.7720 0.8880 0.0708 1.0000 Uiso R . . . . . . H51 H 0.5581 0.9435 0.8371 0.0728 1.0000 Uiso R . . . . . . H61 H 0.5931 0.9731 0.7404 0.0632 1.0000 Uiso R . . . . . . H81 H 0.7008 0.8663 0.6997 0.0608 1.0000 Uiso R . . . . . . H82 H 0.6253 0.8903 0.6411 0.0605 1.0000 Uiso R . . . . . . H91 H 0.5620 0.7760 0.5545 0.0672 1.0000 Uiso R . . . . . . H92 H 0.6012 0.6824 0.5323 0.0670 1.0000 Uiso R . . . . . . H111 H 0.4551 0.6552 0.4975 0.0566 1.0000 Uiso R . . . . . . H121 H 0.3927 0.5210 0.5234 0.0647 1.0000 Uiso R . . . . . . H131 H 0.4450 0.4187 0.6322 0.0616 1.0000 Uiso R . . . . . . H141 H 0.5584 0.4547 0.7112 0.0557 1.0000 Uiso R . . . . . . H151 H 0.6588 0.3833 0.6663 0.0499 1.0000 Uiso R . . . . . . H161 H 0.6837 0.2688 0.5886 0.0519 1.0000 Uiso R . . . . . . H181 H 0.7904 0.5042 0.5448 0.0518 1.0000 Uiso R . . . . . . H4 H 0.6886 0.7395 0.6237 0.0632 1.0000 Uiso R . . . . . . S2 S 0.92050(9) 0.68478(16) 0.83457(16) 0.1516 1.0000 Uani . . . . 2 . . C2 C 0.8367(3) 0.6661(4) 0.7968(4) 0.0829 1.0000 Uani . . . . 2 . . C20 C 0.7578(2) 0.3027(3) 0.5062(2) 0.0444 1.0000 Uani . . . . . . . H201 H 0.7821 0.3345 0.4795 0.0543 1.0000 Uiso R . . . . . . 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 C1 0.039(2) 0.034(2) 0.060(3) -0.009(2) 0.000(2) 0.0053(18) C3 0.036(2) 0.068(3) 0.053(3) 0.013(2) 0.001(2) -0.011(2) C4 0.038(2) 0.089(4) 0.051(3) 0.008(3) 0.007(2) -0.018(3) C5 0.042(2) 0.069(3) 0.060(3) -0.012(3) 0.005(2) -0.014(3) C6 0.053(3) 0.041(2) 0.054(3) 0.000(2) 0.009(2) -0.009(2) C7 0.037(2) 0.039(2) 0.046(2) 0.0022(19) 0.0000(19) -0.0109(18) C8 0.058(3) 0.036(2) 0.057(3) 0.003(2) 0.015(2) -0.008(2) C9 0.056(3) 0.046(3) 0.047(3) 0.007(2) -0.006(2) -0.005(2) C10 0.036(2) 0.036(2) 0.040(2) -0.0042(17) -0.0003(17) 0.0037(17) C11 0.042(2) 0.044(2) 0.044(2) -0.006(2) -0.0099(18) 0.008(2) C12 0.031(2) 0.058(3) 0.064(3) -0.017(2) -0.002(2) 0.002(2) C13 0.034(2) 0.047(2) 0.067(3) -0.013(2) 0.012(2) -0.0051(19) C14 0.039(2) 0.043(2) 0.047(2) -0.0024(19) 0.0064(19) -0.0036(18) C15 0.044(2) 0.034(2) 0.040(2) 0.0047(17) 0.0068(18) -0.0026(17) C16 0.046(2) 0.0296(19) 0.042(2) -0.0009(17) 0.0066(19) -0.0014(17) C17 0.0356(19) 0.035(2) 0.033(2) 0.0007(16) -0.0008(16) 0.0019(16) C18 0.036(2) 0.035(2) 0.054(3) 0.0014(19) 0.0115(19) -0.0003(17) C19 0.035(2) 0.0307(19) 0.056(3) -0.0003(19) 0.0059(19) -0.0043(16) Fe1 0.0402(3) 0.0291(3) 0.0612(4) 0.0032(3) 0.0131(3) 0.0019(3) N2 0.066(3) 0.037(2) 0.072(3) -0.0121(19) 0.023(2) -0.0053(19) N5 0.0345(17) 0.0346(17) 0.046(2) 0.0002(15) 0.0018(15) 0.0021(14) N4 0.044(2) 0.0414(19) 0.047(2) 0.0023(16) 0.0076(16) -0.0037(16) N3 0.0319(17) 0.048(2) 0.050(2) 0.0131(17) -0.0002(16) -0.0089(15) N6 0.0359(17) 0.0277(15) 0.0412(19) -0.0003(14) 0.0014(15) -0.0031(13) N1 0.0372(19) 0.0354(19) 0.079(3) -0.0009(19) 0.0028(19) 0.0000(16) S1 0.0870(10) 0.0598(8) 0.0615(8) 0.0093(7) 0.0235(7) 0.0282(7) S2 0.0649(11) 0.0860(13) 0.252(3) -0.0820(16) 0.0112(14) -0.0031(9) C2 0.075(4) 0.047(3) 0.106(5) -0.033(3) 0.016(4) -0.001(3) C20 0.042(2) 0.040(2) 0.040(2) 0.0016(19) 0.0047(18) -0.0011(18) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.675(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . N1 . 1.163(5) yes C1 . S1 . 1.629(5) yes C3 . C4 . 1.368(7) yes C3 . N3 . 1.332(6) yes C3 . H31 . 0.940 no C4 . C5 . 1.380(7) yes C4 . H41 . 0.928 no C5 . C6 . 1.368(6) yes C5 . H51 . 0.924 no C6 . C7 . 1.367(6) yes C6 . H61 . 0.909 no C7 . C8 . 1.495(6) yes C7 . N3 . 1.354(5) yes C8 . N4 . 1.486(5) yes C8 . H81 . 0.975 no C8 . H82 . 0.950 no C9 . C10 . 1.491(6) yes C9 . N4 . 1.476(5) yes C9 . H91 . 0.953 no C9 . H92 . 0.994 no C10 . C11 . 1.402(5) yes C10 . N5 . 1.335(5) yes C11 . C12 . 1.367(6) yes C11 . H111 . 0.921 no C12 . C13 . 1.375(6) yes C12 . H121 . 0.920 no C13 . C14 . 1.380(5) yes C13 . H131 . 0.931 no C14 . N5 . 1.334(5) yes C14 . H141 . 0.933 no C15 . C16 . 1.372(5) yes C15 . N6 . 1.348(4) yes C15 . H151 . 0.928 no C16 . C17 . 1.368(5) yes C16 . H161 . 0.909 no C17 . C18 . 1.400(5) yes C17 . C20 . 1.459(6) yes C18 . C19 . 1.368(6) yes C18 . H181 . 0.938 no C19 . H191 . 0.925 no C19 . N6 . 1.332(5) yes Fe1 . N2 . 1.991(4) yes Fe1 . N5 . 2.075(3) yes Fe1 . N4 . 2.114(3) yes Fe1 . N3 . 2.073(4) yes Fe1 . N6 . 2.081(3) yes Fe1 . N1 . 2.014(4) yes N2 . C2 . 1.149(6) yes N4 . H4 . 0.893 no S2 . C2 . 1.624(6) yes C20 . C20 4_656 1.348(7) yes C20 . H201 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . C1 . S1 . 179.5(4) yes C4 . C3 . N3 . 123.3(5) yes C4 . C3 . H31 . 118.1 no N3 . C3 . H31 . 118.6 no C3 . C4 . C5 . 119.1(5) yes C3 . C4 . H41 . 120.8 no C5 . C4 . H41 . 120.1 no C4 . C5 . C6 . 118.4(5) yes C4 . C5 . H51 . 120.7 no C6 . C5 . H51 . 120.9 no C5 . C6 . C7 . 119.5(5) yes C5 . C6 . H61 . 120.6 no C7 . C6 . H61 . 119.9 no C6 . C7 . C8 . 122.8(4) yes C6 . C7 . N3 . 122.7(4) yes C8 . C7 . N3 . 114.5(4) yes C7 . C8 . N4 . 112.0(3) yes C7 . C8 . H81 . 109.1 no N4 . C8 . H81 . 107.8 no C7 . C8 . H82 . 110.1 no N4 . C8 . H82 . 109.6 no H81 . C8 . H82 . 108.1 no C10 . C9 . N4 . 112.6(3) yes C10 . C9 . H91 . 109.7 no N4 . C9 . H91 . 110.1 no C10 . C9 . H92 . 107.9 no N4 . C9 . H92 . 107.7 no H91 . C9 . H92 . 108.8 no C9 . C10 . C11 . 120.9(4) yes C9 . C10 . N5 . 117.8(3) yes C11 . C10 . N5 . 121.2(4) yes C10 . C11 . C12 . 119.0(4) yes C10 . C11 . H111 . 119.9 no C12 . C11 . H111 . 121.2 no C11 . C12 . C13 . 119.9(4) yes C11 . C12 . H121 . 119.8 no C13 . C12 . H121 . 120.3 no C12 . C13 . C14 . 118.0(4) yes C12 . C13 . H131 . 121.1 no C14 . C13 . H131 . 121.0 no C13 . C14 . N5 . 123.2(4) yes C13 . C14 . H141 . 117.6 no N5 . C14 . H141 . 119.2 no C16 . C15 . N6 . 123.5(4) yes C16 . C15 . H151 . 120.2 no N6 . C15 . H151 . 116.3 no C15 . C16 . C17 . 120.7(4) yes C15 . C16 . H161 . 119.2 no C17 . C16 . H161 . 120.1 no C16 . C17 . C18 . 116.4(4) yes C16 . C17 . C20 . 124.3(4) yes C18 . C17 . C20 . 119.3(4) yes C17 . C18 . C19 . 119.3(4) yes C17 . C18 . H181 . 120.0 no C19 . C18 . H181 . 120.7 no C18 . C19 . H191 . 119.5 no C18 . C19 . N6 . 124.7(4) yes H191 . C19 . N6 . 115.8 no N2 . Fe1 . N5 . 171.98(17) yes N2 . Fe1 . N4 . 92.99(15) yes N5 . Fe1 . N4 . 80.52(13) yes N2 . Fe1 . N3 . 97.71(14) yes N5 . Fe1 . N3 . 85.85(13) yes N4 . Fe1 . N3 . 79.69(14) yes N2 . Fe1 . N6 . 87.41(14) yes N5 . Fe1 . N6 . 88.05(13) yes N4 . Fe1 . N6 . 91.53(13) yes N3 . Fe1 . N6 . 170.02(13) yes N2 . Fe1 . N1 . 93.11(16) yes N5 . Fe1 . N1 . 93.82(14) yes N4 . Fe1 . N1 . 171.77(15) yes N3 . Fe1 . N1 . 94.01(15) yes N6 . Fe1 . N1 . 94.25(15) yes Fe1 . N2 . C2 . 169.9(4) yes Fe1 . N5 . C10 . 115.4(3) yes Fe1 . N5 . C14 . 125.9(3) yes C10 . N5 . C14 . 118.7(3) yes C8 . N4 . C9 . 114.6(3) yes C8 . N4 . Fe1 . 107.9(3) yes C9 . N4 . Fe1 . 110.6(3) yes C8 . N4 . H4 . 107.3 no C9 . N4 . H4 . 109.0 no Fe1 . N4 . H4 . 107.2 no Fe1 . N3 . C7 . 116.2(3) yes Fe1 . N3 . C3 . 126.8(3) yes C7 . N3 . C3 . 116.9(4) yes Fe1 . N6 . C15 . 121.0(3) yes Fe1 . N6 . C19 . 123.6(3) yes C15 . N6 . C19 . 115.4(4) yes Fe1 . N1 . C1 . 174.7(4) yes S2 . C2 . N2 . 178.3(5) yes C17 . C20 . C20 4_656 124.8(6) yes C17 . C20 . H201 . 118.3 no C20 4_656 C20 . H201 . 116.9 no # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 164 79 ' ' 2 0.500 0.000 0.500 164 79 ' ' 3 0.000 0.183 0.250 7 2 ' ' 4 1.000 0.501 -0.001 163 79 ' ' 5 0.000 0.501 0.501 163 79 ' ' 6 0.500 0.324 0.750 6 2 ' ' 7 0.500 0.675 0.250 6 2 ' ' 8 0.000 0.824 0.750 6 2 ' ' _platon_squeeze_details ; ; # Attachment '- compound 1(90K).txt' data_1(90K) _database_code_depnum_ccdc_archive 'CCDC 807893' #TrackingRef '- compound 1(90K).txt' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 20.7590(10) _cell_length_b 12.2493(5) _cell_length_c 19.3996(8) _cell_angle_alpha 90 _cell_angle_beta 114.008(2) _cell_angle_gamma 90 _cell_volume 4506.2(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C50 H52.50 Fe2.50 N7.50 S5 # Dc = 1.56 Fooo = 1904.00 Mu = 10.78 M = 529.23 # Found Formula = C40 H36 Fe2 N12 S4 # Dc = 1.36 FOOO = 1904.00 Mu = 8.72 M = 462.38 _chemical_formula_sum 'C40 H36 Fe2 N12 S4' _chemical_formula_moiety 'C40 H36 Fe2 N12 S4' _chemical_compound_source ? _chemical_formula_weight 924.79 _cell_measurement_reflns_used 4981 _cell_measurement_theta_min 0.679 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 90 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_max 0.3 _exptl_crystal_density_diffrn 1.363 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.872 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details ; Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897 ; # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 90 _diffrn_reflns_number 5269 _reflns_number_total 5269 _diffrn_reflns_av_R_equivalents 0.034 # Number of reflections with Friedels Law is 5269 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 5380 _diffrn_reflns_theta_min 1.979 _diffrn_reflns_theta_max 27.885 _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.327 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _reflns_limit_h_min -27 _reflns_limit_h_max 24 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min 0 _reflns_limit_l_max 25 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.19 _refine_diff_density_max 2.18 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5252 _refine_ls_number_restraints 0 _refine_ls_number_parameters 262 _oxford_refine_ls_R_factor_ref 0.0853 _refine_ls_wR_factor_ref 0.2128 _refine_ls_goodness_of_fit_ref 1.0645 _refine_ls_shift/su_max 0.0005366 _refine_ls_shift/su_mean 1.2220287 # The values computed from all data _oxford_reflns_number_all 5252 _refine_ls_R_factor_all 0.0853 _refine_ls_wR_factor_all 0.2128 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4197 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_gt 0.1964 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 38.5 60.0 29.9 7.76 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens C2 C 0.1668(2) 0.6706(3) 0.2100(2) 0.0393 1.0000 Uani . . . . . . . C1 C 0.30175(19) 0.4392(3) 0.1626(2) 0.0345 1.0000 Uani . . . . . . . C3 C 0.38402(16) 0.7016(3) 0.1789(2) 0.0352 1.0000 Uani D . . . . . . C4 C 0.41343(17) 0.7803(3) 0.1506(2) 0.0381 1.0000 Uani D . . . . . . C5 C 0.42224(17) 0.8853(3) 0.1798(2) 0.0387 1.0000 Uani D . . . . . . C6 C 0.40176(17) 0.9068(3) 0.2383(2) 0.0369 1.0000 Uani D . . . . . . C7 C 0.37218(18) 0.8241(3) 0.2638(2) 0.0340 1.0000 Uani D . . . . . . C8 C 0.3455(2) 0.8409(3) 0.3243(2) 0.0376 1.0000 Uani D . . . . . . C9 C 0.4100(2) 0.7115(3) 0.4300(2) 0.0401 1.0000 Uani D . . . . . . C10 C 0.4553(2) 0.6313(3) 0.4132(2) 0.0353 1.0000 Uani D . . . . . . C11 C 0.5245(2) 0.6119(3) 0.4621(2) 0.0400 1.0000 Uani D . . . . . . C12 C 0.56286(19) 0.5318(3) 0.4442(2) 0.0430 1.0000 Uani D . . . . . . C13 C 0.53102(19) 0.4737(3) 0.3784(2) 0.0404 1.0000 Uani D . . . . . . C14 C 0.46127(19) 0.4966(3) 0.3310(2) 0.0365 1.0000 Uani D . . . . . . C15 C 0.31656(17) 0.4089(3) 0.35928(18) 0.0327 1.0000 Uani D . . . . . . C16 C 0.30036(18) 0.3367(3) 0.40465(18) 0.0328 1.0000 Uani D . . . . . . C17 C 0.25944(17) 0.3718(3) 0.44213(19) 0.0315 1.0000 Uani D . . . . . . C18 C 0.23415(17) 0.4796(3) 0.42856(19) 0.0338 1.0000 Uani D . . . . . . C19 C 0.25125(17) 0.5463(3) 0.38145(19) 0.0328 1.0000 Uani D . . . . . . C20 C 0.24073(17) 0.3031(3) 0.49278(19) 0.0325 1.0000 Uani D . . . . . . Fe1 Fe 0.32517(2) 0.61398(4) 0.28620(3) 0.0305 1.0000 Uani D . . . . . . N6 N 0.29361(14) 0.5134(2) 0.34741(16) 0.0302 1.0000 Uani D . . . . . . N4 N 0.34464(16) 0.7356(3) 0.36211(17) 0.0339 1.0000 Uani D . . . . . . N3 N 0.36232(15) 0.7224(3) 0.23502(17) 0.0329 1.0000 Uani D . . . . . . N5 N 0.42370(15) 0.5733(3) 0.34764(17) 0.0330 1.0000 Uani D . . . . . . N2 N 0.22673(16) 0.6588(3) 0.23398(18) 0.0342 1.0000 Uani . . . . . . . S2 S 0.08054(6) 0.69132(10) 0.17441(8) 0.0555 1.0000 Uani . . . . . . . N1 N 0.31188(16) 0.5017(3) 0.21021(18) 0.0341 1.0000 Uani . . . . . . . S1 S 0.28666(7) 0.34977(9) 0.09348(6) 0.0464 1.0000 Uani . . . . . . . H31 H 0.3784 0.6317 0.1559 0.0365 1.0000 Uiso DR . . . . . . H41 H 0.4265 0.7619 0.1126 0.0423 1.0000 Uiso DR . . . . . . H51 H 0.4402 0.9418 0.1595 0.0427 1.0000 Uiso DR . . . . . . H61 H 0.4048 0.9753 0.2585 0.0353 1.0000 Uiso DR . . . . . . H81 H 0.2978 0.8751 0.3027 0.0423 1.0000 Uiso DR . . . . . . H82 H 0.3755 0.8917 0.3615 0.0414 1.0000 Uiso DR . . . . . . H91 H 0.4360 0.7764 0.4561 0.0445 1.0000 Uiso DR . . . . . . H92 H 0.3963 0.6811 0.4654 0.0456 1.0000 Uiso DR . . . . . . H111 H 0.5445 0.6617 0.5061 0.0448 1.0000 Uiso DR . . . . . . H121 H 0.6109 0.5170 0.4742 0.0500 1.0000 Uiso DR . . . . . . H131 H 0.5560 0.4169 0.3656 0.0444 1.0000 Uiso DR . . . . . . H141 H 0.4375 0.4543 0.2862 0.0403 1.0000 Uiso DR . . . . . . H151 H 0.3472 0.3856 0.3373 0.0355 1.0000 Uiso DR . . . . . . H161 H 0.3160 0.2626 0.4098 0.0337 1.0000 Uiso DR . . . . . . H181 H 0.2054 0.5046 0.4516 0.0348 1.0000 Uiso DR . . . . . . H191 H 0.2330 0.6147 0.3703 0.0342 1.0000 Uiso DR . . . . . . H201 H 0.2166 0.3424 0.5194 0.0344 1.0000 Uiso DR . . . . . . H4 H 0.3105 0.7393 0.3765 0.0434 1.0000 Uiso DR . . . . . . 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 C2 0.0332(18) 0.0346(19) 0.043(2) 0.0090(15) 0.0080(15) -0.0002(14) C1 0.0311(16) 0.0340(18) 0.0341(17) 0.0034(14) 0.0088(13) -0.0031(13) C3 0.0267(16) 0.0380(18) 0.0359(17) -0.0011(14) 0.0076(13) 0.0036(13) C4 0.0275(16) 0.046(2) 0.0367(17) 0.0009(16) 0.0085(14) 0.0043(15) C5 0.0291(17) 0.041(2) 0.041(2) 0.0057(15) 0.0102(15) -0.0008(14) C6 0.0293(17) 0.0350(18) 0.0386(18) 0.0000(15) 0.0059(14) 0.0024(14) C7 0.0250(15) 0.0331(17) 0.0365(17) 0.0007(13) 0.0048(13) 0.0050(13) C8 0.0396(19) 0.0311(17) 0.0402(19) 0.0016(14) 0.0143(16) 0.0032(14) C9 0.0368(19) 0.041(2) 0.0312(17) -0.0031(15) 0.0019(15) -0.0026(15) C10 0.0291(17) 0.0348(17) 0.0324(17) 0.0051(14) 0.0027(14) -0.0039(13) C11 0.0288(17) 0.042(2) 0.0375(19) 0.0042(15) 0.0015(14) -0.0043(14) C12 0.0265(16) 0.050(2) 0.042(2) 0.0139(17) 0.0031(15) -0.0009(15) C13 0.0271(16) 0.045(2) 0.047(2) 0.0110(17) 0.0127(15) 0.0038(14) C14 0.0280(16) 0.0400(19) 0.0375(18) 0.0051(15) 0.0092(14) 0.0011(14) C15 0.0313(16) 0.0325(17) 0.0299(16) -0.0010(13) 0.0079(13) 0.0025(13) C16 0.0329(17) 0.0319(16) 0.0312(16) -0.0029(13) 0.0105(14) 0.0009(13) C17 0.0241(15) 0.0361(17) 0.0277(15) -0.0003(13) 0.0037(12) -0.0013(13) C18 0.0262(15) 0.0342(17) 0.0359(17) -0.0025(13) 0.0075(13) 0.0000(13) C19 0.0264(15) 0.0299(16) 0.0343(16) -0.0008(13) 0.0042(13) 0.0011(12) C20 0.0289(16) 0.0372(18) 0.0273(15) -0.0008(13) 0.0073(12) 0.0005(13) Fe1 0.0238(3) 0.0300(3) 0.0321(3) 0.00056(18) 0.0057(2) 0.00020(17) N6 0.0263(13) 0.0292(14) 0.0301(13) 0.0006(11) 0.0063(11) 0.0013(10) N4 0.0308(14) 0.0328(15) 0.0343(14) -0.0007(12) 0.0093(12) 0.0004(11) N3 0.0239(13) 0.0342(15) 0.0335(14) -0.0004(12) 0.0043(11) 0.0021(11) N5 0.0251(13) 0.0319(15) 0.0360(15) 0.0020(12) 0.0063(11) -0.0016(11) N2 0.0305(15) 0.0335(15) 0.0362(15) 0.0038(12) 0.0109(12) -0.0001(12) S2 0.0303(5) 0.0494(6) 0.0778(8) 0.0190(6) 0.0127(5) 0.0033(4) N1 0.0263(13) 0.0329(14) 0.0365(15) 0.0025(12) 0.0059(12) 0.0000(11) S1 0.0597(7) 0.0435(6) 0.0380(5) -0.0069(4) 0.0219(5) -0.0171(5) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1746(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C2 . N2 . 1.146(5) yes C2 . S2 . 1.656(4) yes C1 . N1 . 1.152(5) yes C1 . S1 . 1.659(4) yes C3 . C4 . 1.369(6) yes C3 . N3 . 1.361(5) yes C3 . H31 . 0.950 no C4 . C5 . 1.386(6) yes C4 . H41 . 0.913 no C5 . C6 . 1.389(6) yes C5 . H51 . 0.945 no C6 . C7 . 1.377(6) yes C6 . H61 . 0.918 no C7 . C8 . 1.502(5) yes C7 . N3 . 1.346(5) yes C8 . N4 . 1.487(5) yes C8 . H81 . 0.996 no C8 . H82 . 0.965 no C9 . C10 . 1.485(6) yes C9 . N4 . 1.486(5) yes C9 . H91 . 0.978 no C9 . H92 . 0.922 no C10 . C11 . 1.382(5) yes C10 . N5 . 1.369(5) yes C11 . C12 . 1.394(6) yes C11 . H111 . 0.993 no C12 . C13 . 1.374(6) yes C12 . H121 . 0.945 no C13 . C14 . 1.392(5) yes C13 . H131 . 0.959 no C14 . N5 . 1.343(5) yes C14 . H141 . 0.958 no C15 . C16 . 1.382(5) yes C15 . N6 . 1.353(5) yes C15 . H151 . 0.941 no C16 . C17 . 1.392(5) yes C16 . H161 . 0.956 no C17 . C18 . 1.405(5) yes C17 . C20 . 1.461(5) yes C18 . C19 . 1.376(5) yes C18 . H181 . 0.932 no C19 . N6 . 1.358(5) yes C19 . H191 . 0.909 no C20 . C20 4_556 1.353(7) yes C20 . H201 . 0.980 no Fe1 . N6 . 1.997(3) yes Fe1 . N4 . 2.017(3) yes Fe1 . N3 . 1.992(3) yes Fe1 . N5 . 1.967(3) yes Fe1 . N2 . 1.954(3) yes Fe1 . N1 . 1.952(3) yes N4 . H4 . 0.862 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N2 . C2 . S2 . 178.3(4) yes N1 . C1 . S1 . 179.5(3) yes C4 . C3 . N3 . 122.4(4) yes C4 . C3 . H31 . 115.9 no N3 . C3 . H31 . 121.7 no C3 . C4 . C5 . 119.7(4) yes C3 . C4 . H41 . 118.5 no C5 . C4 . H41 . 121.7 no C4 . C5 . C6 . 118.4(4) yes C4 . C5 . H51 . 121.2 no C6 . C5 . H51 . 120.4 no C5 . C6 . C7 . 118.9(4) yes C5 . C6 . H61 . 122.2 no C7 . C6 . H61 . 118.8 no C6 . C7 . C8 . 122.7(3) yes C6 . C7 . N3 . 123.1(4) yes C8 . C7 . N3 . 114.1(3) yes C7 . C8 . N4 . 110.4(3) yes C7 . C8 . H81 . 110.4 no N4 . C8 . H81 . 111.3 no C7 . C8 . H82 . 110.0 no N4 . C8 . H82 . 108.9 no H81 . C8 . H82 . 105.7 no C10 . C9 . N4 . 111.7(3) yes C10 . C9 . H91 . 112.7 no N4 . C9 . H91 . 114.3 no C10 . C9 . H92 . 108.1 no N4 . C9 . H92 . 107.1 no H91 . C9 . H92 . 102.3 no C9 . C10 . C11 . 122.5(4) yes C9 . C10 . N5 . 116.1(3) yes C11 . C10 . N5 . 121.3(4) yes C10 . C11 . C12 . 119.3(4) yes C10 . C11 . H111 . 116.0 no C12 . C11 . H111 . 124.4 no C11 . C12 . C13 . 119.2(3) yes C11 . C12 . H121 . 123.3 no C13 . C12 . H121 . 117.4 no C12 . C13 . C14 . 119.2(4) yes C12 . C13 . H131 . 120.7 no C14 . C13 . H131 . 120.1 no C13 . C14 . N5 . 122.1(4) yes C13 . C14 . H141 . 120.3 no N5 . C14 . H141 . 117.5 no C16 . C15 . N6 . 123.6(3) yes C16 . C15 . H151 . 118.6 no N6 . C15 . H151 . 117.7 no C15 . C16 . C17 . 119.6(3) yes C15 . C16 . H161 . 120.9 no C17 . C16 . H161 . 119.5 no C16 . C17 . C18 . 116.9(3) yes C16 . C17 . C20 . 124.0(3) yes C18 . C17 . C20 . 119.1(3) yes C17 . C18 . C19 . 120.3(3) yes C17 . C18 . H181 . 118.9 no C19 . C18 . H181 . 120.8 no C18 . C19 . N6 . 122.7(3) yes C18 . C19 . H191 . 120.8 no N6 . C19 . H191 . 116.5 no C17 . C20 . C20 4_556 124.2(4) yes C17 . C20 . H201 . 113.8 no C20 4_556 C20 . H201 . 121.8 no N6 . Fe1 . N4 . 92.20(12) yes N6 . Fe1 . N3 . 174.10(12) yes N4 . Fe1 . N3 . 82.43(13) yes N6 . Fe1 . N5 . 89.73(12) yes N4 . Fe1 . N5 . 83.94(13) yes N3 . Fe1 . N5 . 87.29(12) yes N6 . Fe1 . N2 . 87.41(12) yes N4 . Fe1 . N2 . 91.57(13) yes N3 . Fe1 . N2 . 95.14(12) yes N5 . Fe1 . N2 . 174.59(13) yes N6 . Fe1 . N1 . 92.00(12) yes N4 . Fe1 . N1 . 175.37(13) yes N3 . Fe1 . N1 . 93.30(13) yes N5 . Fe1 . N1 . 94.13(13) yes N2 . Fe1 . N1 . 90.57(13) yes C19 . N6 . C15 . 116.8(3) yes C19 . N6 . Fe1 . 122.7(2) yes C15 . N6 . Fe1 . 120.5(2) yes C8 . N4 . C9 . 114.8(3) yes C8 . N4 . Fe1 . 108.6(2) yes C9 . N4 . Fe1 . 109.9(2) yes C8 . N4 . H4 . 106.9 no C9 . N4 . H4 . 107.4 no Fe1 . N4 . H4 . 109.1 no C3 . N3 . C7 . 117.4(3) yes C3 . N3 . Fe1 . 126.6(3) yes C7 . N3 . Fe1 . 115.8(3) yes C10 . N5 . C14 . 118.8(3) yes C10 . N5 . Fe1 . 114.8(3) yes C14 . N5 . Fe1 . 126.5(3) yes Fe1 . N2 . C2 . 168.3(3) yes Fe1 . N1 . C1 . 176.4(3) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C8 . H81 . C1 7_555 142 1.00 2.55 3.390(5) yes # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.000 172 90 ' ' 2 0.500 0.000 0.500 172 90 ' ' 3 0.000 0.183 0.750 7 1 ' ' 4 1.000 0.501 0.499 171 89 ' ' 5 0.000 0.501 1.001 171 89 ' ' 6 0.500 0.325 0.250 6 1 ' ' 7 0.500 0.675 0.750 6 1 ' ' 8 0.000 0.825 0.250 6 1 ' ' _platon_squeeze_details ; ; # Attachment '- compound 1(300K).txt' data_1(300k) _database_code_depnum_ccdc_archive 'CCDC 807894' #TrackingRef '- compound 1(300K).txt' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 20.8126(8) _cell_length_b 12.7451(5) _cell_length_c 18.9354(7) _cell_angle_alpha 90 _cell_angle_beta 111.389(2) _cell_angle_gamma 90 _cell_volume 4676.8(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1 ' _symmetry_space_group_name_Hall '-C 2yc ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z x+1/2,y+1/2,z -x+1/2,-y+1/2,-z -x,y,-z+1/2 x,-y,z+1/2 -x+1/2,y+1/2,-z+1/2 x+1/2,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C25 H26.25 Fe1.25 N3.75 S2.50 # Dc = 1.50 Fooo = 1904.00 Mu = 10.38 M = 529.23 # Found Formula = C20 H18 Fe1 N6 S1 # Dc = 1.31 FOOO = 1904.00 Mu = 8.40 M = 462.38 _chemical_formula_sum 'C40 H36 Fe2 N12 S4 ' _chemical_formula_moiety 'C40 H36 Fe2 N12 S4 ' _chemical_compound_source ? _chemical_formula_weight 924.79 _cell_measurement_reflns_used 4878 _cell_measurement_theta_min 0.730 _cell_measurement_theta_max 27.878 _cell_measurement_temperature 300 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_min 0.12 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_max 0.3 _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.840 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.921 _exptl_absorpt_process_details ; Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897 ; # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 300 _diffrn_reflns_number 5115 _reflns_number_total 5115 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections without Friedels Law is 5115 # Number of reflections with Friedels Law is 5115 # Theoretical number of reflections is about 5574 _diffrn_reflns_theta_min 1.912 _diffrn_reflns_theta_max 27.868 _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 25.081 _diffrn_measured_fraction_theta_full 0.947 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 16 _reflns_limit_l_min -24 _reflns_limit_l_max 20 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.45 _refine_diff_density_max 0.40 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 5097 _refine_ls_number_restraints 0 _refine_ls_number_parameters 280 _oxford_refine_ls_R_factor_ref 0.1080 _refine_ls_wR_factor_ref 0.2345 _refine_ls_goodness_of_fit_ref 0.9640 _refine_ls_shift/su_max 0.0004316 _refine_ls_shift/su_mean 0.0001728 # The values computed from all data _oxford_reflns_number_all 5097 _refine_ls_R_factor_all 0.1080 _refine_ls_wR_factor_all 0.2345 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2823 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_gt 0.1687 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 76.1 115. 57.3 15.1 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. & Spagna, R. (1999). J. App. Cryst. 32, 115-119. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens C1 C 0.3095(3) 0.4350(4) 0.1493(3) 0.0778 1.0000 Uani . U . . . . . C3 C 0.3868(3) 0.7306(4) 0.1680(3) 0.0860 1.0000 Uani . . . . . . . C4 C 0.4186(3) 0.8105(5) 0.1435(4) 0.0924 1.0000 Uani . . . . . . . C5 C 0.4246(3) 0.9070(5) 0.1774(4) 0.0965 1.0000 Uani . . . . . . . C6 C 0.4011(3) 0.9192(4) 0.2366(3) 0.0889 1.0000 Uani . . . . . . . C7 C 0.3705(2) 0.8360(4) 0.2587(3) 0.0755 1.0000 Uani . . . . . . . C8 C 0.3408(3) 0.8470(4) 0.3196(3) 0.0903 1.0000 Uani . . . . . . . C9 C 0.4016(3) 0.7223(5) 0.4244(3) 0.1016 1.0000 Uani . . . . . . . C10 C 0.4486(3) 0.6436(4) 0.4089(3) 0.0780 1.0000 Uani . . . . . . . C11 C 0.5152(3) 0.6267(5) 0.4608(3) 0.0911 1.0000 Uani . . . . . . . C12 C 0.5542(3) 0.5484(5) 0.4468(4) 0.0966 1.0000 Uani . . . . . . . C13 C 0.5277(3) 0.4892(5) 0.3826(4) 0.0955 1.0000 Uani . . . . . . . C14 C 0.4624(3) 0.5104(5) 0.3330(3) 0.0884 1.0000 Uani . . . . . . . C15 C 0.3101(3) 0.4129(4) 0.3552(3) 0.0820 1.0000 Uani . . . . . . . C16 C 0.2989(3) 0.3432(4) 0.4039(3) 0.0820 1.0000 Uani . . . . . . . C17 C 0.2602(3) 0.3736(4) 0.4469(3) 0.0736 1.0000 Uani . . . . . . . C18 C 0.2371(3) 0.4759(4) 0.4382(3) 0.0832 1.0000 Uani . . . . . . . C19 C 0.2501(3) 0.5411(4) 0.3869(3) 0.0858 1.0000 Uani . . . . . . . C20 C 0.2450(3) 0.3014(4) 0.4984(3) 0.0798 1.0000 Uani . . . . . . . Fe1 Fe 0.31457(3) 0.61891(5) 0.26987(4) 0.0755 1.0000 Uani . . . . . . . N6 N 0.2868(2) 0.5119(3) 0.3455(2) 0.0770 1.0000 Uani . . . . . . . N4 N 0.3386(2) 0.7474(3) 0.3570(3) 0.0845 1.0000 Uani . . . . . . . N3 N 0.36223(19) 0.7424(3) 0.2242(2) 0.0763 1.0000 Uani . . . . . . . N5 N 0.4224(2) 0.5858(3) 0.3460(2) 0.0780 1.0000 Uani . . . . . . . N1 N 0.3170(2) 0.5047(4) 0.1903(3) 0.0893 1.0000 Uani . . . . . . . S1 S 0.30037(10) 0.33653(13) 0.09202(10) 0.1022 1.0000 Uani . U . . . . . H31 H 0.3828 0.6657 0.1458 0.0973 1.0000 Uiso R . . . . . . H41 H 0.4331 0.7990 0.1043 0.1067 1.0000 Uiso R . . . . . . H51 H 0.4424 0.9669 0.1608 0.1100 1.0000 Uiso R . . . . . . H61 H 0.4055 0.9864 0.2595 0.1016 1.0000 Uiso R . . . . . . H81 H 0.2947 0.8742 0.2970 0.1028 1.0000 Uiso R . . . . . . H82 H 0.3702 0.9010 0.3568 0.1017 1.0000 Uiso R . . . . . . H91 H 0.4266 0.7914 0.4452 0.1155 1.0000 Uiso R . . . . . . H92 H 0.3885 0.6893 0.4617 0.1124 1.0000 Uiso R . . . . . . H111 H 0.5322 0.6696 0.5032 0.1067 1.0000 Uiso R . . . . . . H121 H 0.6014 0.5352 0.4808 0.1125 1.0000 Uiso R . . . . . . H131 H 0.5545 0.4369 0.3716 0.1065 1.0000 Uiso R . . . . . . H141 H 0.4412 0.4683 0.2879 0.1028 1.0000 Uiso R . . . . . . H151 H 0.3378 0.3930 0.3299 0.0901 1.0000 Uiso R . . . . . . H161 H 0.3159 0.2719 0.4089 0.0943 1.0000 Uiso R . . . . . . H181 H 0.2088 0.5000 0.4633 0.0920 1.0000 Uiso R . . . . . . H191 H 0.2328 0.6131 0.3802 0.1009 1.0000 Uiso R . . . . . . H201 H 0.2264 0.3321 0.5286 0.0891 1.0000 Uiso R . . . . . . H4 H 0.3054 0.7503 0.3723 0.1207 1.0000 Uiso R . . . . . . N2 N 0.2097(2) 0.6536(4) 0.2176(3) 0.1021 1.0000 Uani . . . . . . . C2A C 0.1525(13) 0.6665(19) 0.1979(11) 0.0959 0.5000 Uani . . . 1 1 . . C2B C 0.1556(11) 0.6412(17) 0.1656(10) 0.0961 0.5000 Uani . . . 1 2 . . S2A S 0.0704(3) 0.6828(5) 0.1519(6) 0.1901 0.5000 Uani . . . 1 1 . . S2B S 0.0792(3) 0.6238(6) 0.1032(5) 0.1965 0.5000 Uani . . . 1 2 . . 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 C1 0.078(3) 0.075(3) 0.079(3) -0.005(2) 0.027(2) -0.014(2) C3 0.081(3) 0.083(3) 0.093(3) -0.011(3) 0.031(3) 0.005(2) C4 0.085(3) 0.099(4) 0.102(4) -0.006(3) 0.044(3) 0.006(3) C5 0.080(3) 0.092(4) 0.117(5) 0.006(3) 0.035(3) 0.000(3) C6 0.082(3) 0.072(3) 0.107(4) -0.005(3) 0.027(3) 0.001(2) C7 0.066(2) 0.070(3) 0.087(3) -0.005(2) 0.024(2) 0.007(2) C8 0.097(4) 0.075(3) 0.102(4) -0.008(3) 0.040(3) 0.012(3) C9 0.111(4) 0.093(4) 0.086(4) -0.013(3) 0.018(3) 0.001(3) C10 0.079(3) 0.076(3) 0.076(3) 0.001(2) 0.025(3) -0.008(2) C11 0.085(3) 0.096(4) 0.078(3) 0.013(3) 0.012(3) -0.018(3) C12 0.069(3) 0.110(4) 0.102(4) 0.025(3) 0.020(3) -0.003(3) C13 0.070(3) 0.113(4) 0.108(4) 0.021(3) 0.037(3) 0.015(3) C14 0.077(3) 0.097(4) 0.093(4) 0.005(3) 0.033(3) 0.011(3) C15 0.091(3) 0.075(3) 0.081(3) -0.003(2) 0.032(3) 0.007(2) C16 0.100(3) 0.066(2) 0.078(3) -0.001(2) 0.030(3) 0.010(2) C17 0.075(3) 0.070(3) 0.068(3) -0.007(2) 0.017(2) 0.002(2) C18 0.085(3) 0.073(3) 0.097(4) -0.007(2) 0.040(3) 0.005(2) C19 0.078(3) 0.067(3) 0.113(4) 0.005(3) 0.035(3) 0.009(2) C20 0.086(3) 0.080(3) 0.069(3) -0.007(2) 0.022(2) 0.007(2) Fe1 0.0681(4) 0.0697(4) 0.0830(5) -0.0045(3) 0.0209(4) -0.0002(3) N6 0.073(2) 0.069(2) 0.086(3) 0.0022(18) 0.026(2) 0.0047(17) N4 0.086(3) 0.076(2) 0.096(3) -0.008(2) 0.039(2) 0.006(2) N3 0.068(2) 0.071(2) 0.087(3) -0.0087(19) 0.0241(19) 0.0039(17) N5 0.066(2) 0.084(2) 0.081(3) -0.004(2) 0.022(2) 0.0043(18) N1 0.089(3) 0.080(3) 0.093(3) -0.011(2) 0.026(2) -0.010(2) S1 0.1266(12) 0.0874(9) 0.1069(11) -0.0241(8) 0.0596(10) -0.0308(8) N2 0.074(3) 0.096(3) 0.128(4) 0.037(3) 0.028(3) 0.009(2) C2A 0.081(9) 0.113(12) 0.098(13) 0.038(10) 0.038(10) 0.002(7) C2B 0.070(8) 0.108(12) 0.098(13) 0.053(10) 0.016(10) 0.001(7) S2A 0.068(2) 0.154(5) 0.309(11) 0.126(6) 0.022(4) 0.002(3) S2B 0.102(4) 0.158(6) 0.243(9) 0.113(5) -0.040(5) -0.039(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1746(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag C1 . N1 . 1.153(6) yes C1 . S1 . 1.624(5) yes C3 . C4 . 1.384(8) yes C3 . N3 . 1.346(6) yes C3 . H31 . 0.918 no C4 . C5 . 1.372(8) yes C4 . H41 . 0.910 no C5 . C6 . 1.385(8) yes C5 . H51 . 0.950 no C6 . C7 . 1.379(7) yes C6 . H61 . 0.949 no C7 . C8 . 1.501(7) yes C7 . N3 . 1.340(6) yes C8 . N4 . 1.463(7) yes C8 . H81 . 0.961 no C8 . H82 . 1.016 no C9 . C10 . 1.504(8) yes C9 . N4 . 1.492(7) yes C9 . H91 . 1.026 no C9 . H92 . 0.942 no C10 . C11 . 1.393(7) yes C10 . N5 . 1.335(6) yes C11 . C12 . 1.371(8) yes C11 . H111 . 0.929 no C12 . C13 . 1.366(9) yes C12 . H121 . 0.972 no C13 . C14 . 1.367(7) yes C13 . H131 . 0.939 no C14 . N5 . 1.352(6) yes C14 . H141 . 0.968 no C15 . C16 . 1.361(7) yes C15 . N6 . 1.339(6) yes C15 . H151 . 0.911 no C16 . C17 . 1.391(7) yes C16 . H161 . 0.968 no C17 . C18 . 1.379(6) yes C17 . C20 . 1.457(7) yes C18 . C19 . 1.379(7) yes C18 . H181 . 0.933 no C19 . N6 . 1.331(6) yes C19 . H191 . 0.977 no C20 . C20 4_556 1.324(9) yes C20 . H201 . 0.891 no Fe1 . N6 . 2.202(4) yes Fe1 . N4 . 2.248(4) yes Fe1 . N3 . 2.199(4) yes Fe1 . N5 . 2.222(4) yes Fe1 . N1 . 2.108(5) yes Fe1 . N2 . 2.089(5) yes N4 . H4 . 0.842 no N2 . C2A . 1.12(2) yes N2 . C2B . 1.21(2) yes C2A . S2A . 1.62(3) yes C2B . S2B . 1.61(2) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . C1 . S1 . 179.0(5) yes C4 . C3 . N3 . 123.3(5) yes C4 . C3 . H31 . 119.0 no N3 . C3 . H31 . 117.8 no C3 . C4 . C5 . 118.5(5) yes C3 . C4 . H41 . 119.8 no C5 . C4 . H41 . 121.7 no C4 . C5 . C6 . 118.7(6) yes C4 . C5 . H51 . 123.0 no C6 . C5 . H51 . 118.2 no C5 . C6 . C7 . 119.9(5) yes C5 . C6 . H61 . 117.8 no C7 . C6 . H61 . 122.3 no C6 . C7 . C8 . 121.8(5) yes C6 . C7 . N3 . 121.8(5) yes C8 . C7 . N3 . 116.3(4) yes C7 . C8 . N4 . 112.6(4) yes C7 . C8 . H81 . 108.4 no N4 . C8 . H81 . 109.0 no C7 . C8 . H82 . 106.4 no N4 . C8 . H82 . 111.7 no H81 . C8 . H82 . 108.5 no C10 . C9 . N4 . 114.0(4) yes C10 . C9 . H91 . 111.9 no N4 . C9 . H91 . 108.0 no C10 . C9 . H92 . 103.6 no N4 . C9 . H92 . 109.4 no H91 . C9 . H92 . 109.8 no C9 . C10 . C11 . 121.1(5) yes C9 . C10 . N5 . 117.3(5) yes C11 . C10 . N5 . 121.4(5) yes C10 . C11 . C12 . 118.9(6) yes C10 . C11 . H111 . 119.0 no C12 . C11 . H111 . 122.1 no C11 . C12 . C13 . 119.9(5) yes C11 . C12 . H121 . 121.6 no C13 . C12 . H121 . 118.4 no C12 . C13 . C14 . 118.7(6) yes C12 . C13 . H131 . 120.5 no C14 . C13 . H131 . 120.7 no C13 . C14 . N5 . 122.6(6) yes C13 . C14 . H141 . 121.0 no N5 . C14 . H141 . 116.3 no C16 . C15 . N6 . 124.4(5) yes C16 . C15 . H151 . 118.3 no N6 . C15 . H151 . 117.2 no C15 . C16 . C17 . 119.6(5) yes C15 . C16 . H161 . 122.1 no C17 . C16 . H161 . 118.3 no C16 . C17 . C18 . 116.4(5) yes C16 . C17 . C20 . 121.9(4) yes C18 . C17 . C20 . 121.7(5) yes C17 . C18 . C19 . 120.3(5) yes C17 . C18 . H181 . 120.5 no C19 . C18 . H181 . 118.9 no C18 . C19 . N6 . 123.3(5) yes C18 . C19 . H191 . 120.0 no N6 . C19 . H191 . 116.8 no C17 . C20 . C20 4_556 126.0(6) yes C17 . C20 . H201 . 113.8 no C20 4_556 C20 . H201 . 120.2 no N6 . Fe1 . N4 . 90.83(16) yes N6 . Fe1 . N3 . 164.18(15) yes N4 . Fe1 . N3 . 75.86(16) yes N6 . Fe1 . N5 . 84.39(15) yes N4 . Fe1 . N5 . 76.12(16) yes N3 . Fe1 . N5 . 84.12(15) yes N6 . Fe1 . N1 . 96.74(17) yes N4 . Fe1 . N1 . 166.06(17) yes N3 . Fe1 . N1 . 94.68(16) yes N5 . Fe1 . N1 . 92.93(17) yes N6 . Fe1 . N2 . 87.88(17) yes N4 . Fe1 . N2 . 96.2(2) yes N3 . Fe1 . N2 . 101.84(16) yes N5 . Fe1 . N2 . 169.0(2) yes N1 . Fe1 . N2 . 95.8(2) yes Fe1 . N6 . C15 . 120.3(3) yes Fe1 . N6 . C19 . 123.5(3) yes C15 . N6 . C19 . 116.1(4) yes Fe1 . N4 . C9 . 111.2(3) yes Fe1 . N4 . C8 . 108.3(3) yes C9 . N4 . C8 . 115.3(5) yes Fe1 . N4 . H4 . 107.1 no C9 . N4 . H4 . 106.9 no C8 . N4 . H4 . 107.6 no Fe1 . N3 . C3 . 125.9(3) yes Fe1 . N3 . C7 . 116.2(3) yes C3 . N3 . C7 . 117.8(4) yes Fe1 . N5 . C14 . 124.1(4) yes Fe1 . N5 . C10 . 117.5(3) yes C14 . N5 . C10 . 118.5(5) yes Fe1 . N1 . C1 . 168.8(4) yes Fe1 . N2 . C2A . 170.7(10) yes Fe1 . N2 . C2B . 149.6(12) yes N2 . C2A . S2A . 168.0(16) yes N2 . C2B . S2B . 173.5(16) yes loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C16 . H161 . C2B 7_545 139 0.97 2.39 3.190(10) yes # Attachment '- CCDC 807895.txt' data_5 _database_code_depnum_ccdc_archive 'CCDC 807895' #TrackingRef '- CCDC 807895.txt' _audit_creation_date 10-06-04 _audit_creation_method CRYSTALS_ver_14.06 _oxford_structure_analysis_title 'exp_347 in P 1 21/c 1' _chemical_name_systematic ? _chemical_melting_point ? _publ_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_related_literature # Not in version 2.3.1 ############################################################### # Essential references (e.g. to the origin of the material studied, related # structural studies, and to information supporting the reported structure) # should be cited in this section, with appropriate very brief explanatory # text, for example `The synthesis of the complex is described by Jones # (2001). The anhydrous complex has essentially the same coordination # geometry (Smith, 2003).' In addition, all references included in the # supplementary materials, but not elsewhere in the published article, # should be given here. The simple text `For related literature, see:...' # may be used, but further details should be provided in the Comment # section, which forms part of the supplementary material. ############################################################### ; ? ; _publ_section_comment # Text of the paper # Note that atoms are referenced as N2, not N(2) or N~2~ # If text containing () occur within (), the outer ones should be [] # Figures should be referenced as Fig. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; In the absence of significant anomalous scattering, Friedel pairs were merged. The absolute configuration was arbitrarily assigned. The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # Hand-made tables can be put in the cif. The number of columns # is set in the loop header. # The contants of each column can either be a piece of text # without any spaces (eg a number) or other text enclosed in " " # Remove the leading # in the following example #geom_extra_table_head_A #; #Table 2. #Molecular parameters deviating most from MOGUL averages #; # #loop_ #_geom_extra_tableA_col_1 #_geom_extra_tableA_col_2 #_geom_extra_tableA_col_3 #_geom_extra_tableA_col_4 # #Parameter "Observed Value" "MOGUL Value" "MOGUL e.s.d" #N5-C6-C4 129 124 "7 (\%)" #C3-O10-C2 105 109 "2 (\%)" #C6-O7 1.25 1.22 ".02 (\%A)" # _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 17.084(5) _cell_length_b 16.804(5) _cell_length_c 16.316(5) _cell_angle_alpha 90 _cell_angle_beta 106.911(5) _cell_angle_gamma 90 _cell_volume 4481(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C33 H55 Fe2.75 N22 O3 S5.50 # Dc = 1.69 Fooo = 1904.00 Mu = 12.02 M = 1137.89 # Found Formula = C40 H36 Fe2 N12 S4 # Dc = 1.37 FOOO = 1904.00 Mu = 8.77 M = 924.76 _chemical_formula_sum 'C40 H36 Fe2 N12 S4' _chemical_formula_moiety 'C40 H36 Fe2 N12 S4' _chemical_compound_source ? _chemical_formula_weight 924.76 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 293 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_min ? _exptl_crystal_size_mid ? _exptl_crystal_size_max ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.877 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 1.0000 _exptl_absorpt_correction_T_max 1.0000 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'USER DEFINED DATA COLLECTION' _computing_cell_refinement 'USER DEFINED CELL REFINEMENT' _computing_data_reduction 'USER DEFINED DATA REDUCTION' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 10295 _reflns_number_total 10303 _diffrn_reflns_av_R_equivalents 0.108 # Number of reflections without Friedels Law is 10303 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 12265 _diffrn_reflns_theta_min 2.861 _diffrn_reflns_theta_max 29.306 _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 26.082 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -22 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.82 _refine_diff_density_max 1.48 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 10295 _refine_ls_number_restraints 0 _refine_ls_number_parameters 523 _oxford_refine_ls_R_factor_ref 0.2297 _refine_ls_wR_factor_ref 0.3065 _refine_ls_goodness_of_fit_ref 1.0625 _refine_ls_shift/su_max 0.0003993 _refine_ls_shift/su_mean 0.0000606 # The values computed from all data _oxford_reflns_number_all 10295 _refine_ls_R_factor_all 0.2297 _refine_ls_wR_factor_all 0.3065 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3229 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_gt 0.1837 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 677. 0.102E+04 610. 265. 66.0 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.95452(10) 0.73419(10) 0.02622(10) 0.0517 1.0000 Uani . . . . . . . Fe2 Fe 0.53112(10) 0.20673(11) 0.39228(11) 0.0566 1.0000 Uani . . . . . . . S101 S 0.9507(3) 0.5807(2) -0.2247(2) 0.0838 1.0000 Uani . . . . . . . S202 S 0.8093(2) 0.2164(3) 0.5598(2) 0.0866 1.0000 Uani . . . . . . . S102 S 0.7134(3) 0.9006(3) -0.0786(3) 0.0909 1.0000 Uani . . . . . . . S201 S 0.5565(4) 0.0268(3) 0.1772(4) 0.1384 1.0000 Uani . . . . . . . N105 N 1.0665(6) 0.6593(6) 0.0942(6) 0.0542 1.0000 Uani . . . . . . . N106 N 0.8874(6) 0.6573(5) 0.0934(6) 0.0533 1.0000 Uani . . . . . . . C117 C 0.7995(7) 0.5598(7) 0.1762(8) 0.0555 1.0000 Uani . . . . . . . N104 N 1.0226(6) 0.8006(5) 0.1424(5) 0.0586 1.0000 Uani . . . . . . . C216 C 0.6321(7) 0.4166(7) 0.2871(8) 0.0629 1.0000 Uani . . . . . . . N203 N 0.4657(6) 0.1345(6) 0.4639(6) 0.0594 1.0000 Uani . . . . . . . N204 N 0.5174(6) 0.2878(7) 0.4932(7) 0.0719 1.0000 Uani . . . . . . . C201 C 0.5323(8) 0.0836(8) 0.2445(9) 0.0680 1.0000 Uani . . . . . . . C118 C 0.7965(8) 0.6393(7) 0.1799(9) 0.0733 1.0000 Uani . . . . . . . N103 N 1.0142(6) 0.8307(6) -0.0238(6) 0.0586 1.0000 Uani . . . . . . . C218 C 0.6965(7) 0.3034(8) 0.2513(7) 0.0582 1.0000 Uani . . . . . . . N206 N 0.5971(5) 0.2864(6) 0.3263(6) 0.0538 1.0000 Uani . . . . . . . C101 C 0.9419(6) 0.6303(7) -0.1435(7) 0.0546 1.0000 Uani . . . . . . . C220 C 0.7394(7) 0.4334(8) 0.2078(7) 0.0585 1.0000 Uani . . . . . . . C110 C 1.0986(7) 0.6755(7) 0.1766(8) 0.0561 1.0000 Uani . . . . . . . C217 C 0.6894(7) 0.3847(7) 0.2505(7) 0.0534 1.0000 Uani . . . . . . . C219 C 0.6525(7) 0.2579(7) 0.2910(8) 0.0591 1.0000 Uani . . . . . . . C210 C 0.3905(8) 0.3219(8) 0.3795(9) 0.0667 1.0000 Uani . . . . . . . C102 C 0.7948(8) 0.8473(8) -0.0356(8) 0.0609 1.0000 Uani . . . . . . . N205 N 0.4161(6) 0.2693(6) 0.3305(6) 0.0602 1.0000 Uani . . . . . . . C202 C 0.7160(7) 0.1916(8) 0.5093(8) 0.0627 1.0000 Uani . . . . . . . C107 C 1.0650(7) 0.8783(7) 0.0351(7) 0.0562 1.0000 Uani . . . . . . . C120 C 0.7504(7) 0.5105(8) 0.2168(8) 0.0632 1.0000 Uani . . . . . . . C203 C 0.4250(7) 0.0675(8) 0.4394(9) 0.0717 1.0000 Uani . . . . . . . C103 C 0.9938(9) 0.8538(8) -0.1046(8) 0.0710 1.0000 Uani . . . . . . . C115 C 0.8907(7) 0.5782(7) 0.0917(8) 0.0631 1.0000 Uani . . . . . . . C116 C 0.8481(7) 0.5280(8) 0.1301(8) 0.0670 1.0000 Uani . . . . . . . C104 C 1.0258(10) 0.9202(9) -0.1337(11) 0.0908 1.0000 Uani . . . . . . . C215 C 0.5873(8) 0.3648(8) 0.3242(9) 0.0714 1.0000 Uani . . . . . . . C119 C 0.8381(9) 0.6861(7) 0.1364(9) 0.0757 1.0000 Uani . . . . . . . C114 C 1.1003(8) 0.6004(7) 0.0597(8) 0.0637 1.0000 Uani . . . . . . . N202 N 0.6491(6) 0.1742(7) 0.4722(7) 0.0707 1.0000 Uani . . . . . . . N102 N 0.8509(7) 0.8074(7) -0.0062(8) 0.0743 1.0000 Uani . . . . . . . N101 N 0.9360(7) 0.6654(7) -0.0841(7) 0.0717 1.0000 Uani . . . . . . . C206 C 0.4373(10) 0.1224(13) 0.5967(10) 0.1027 1.0000 Uani . . . . . . . C113 C 1.1673(9) 0.5584(9) 0.1087(11) 0.0834 1.0000 Uani . . . . . . . C111 C 1.1647(9) 0.6352(9) 0.2286(9) 0.0782 1.0000 Uani . . . . . . . C204 C 0.3878(9) 0.0244(10) 0.4889(12) 0.0960 1.0000 Uani . . . . . . . C207 C 0.4711(8) 0.1624(9) 0.5408(8) 0.0689 1.0000 Uani . . . . . . . C214 C 0.3688(8) 0.2556(9) 0.2512(9) 0.0778 1.0000 Uani . . . . . . . C211 C 0.3158(9) 0.3609(9) 0.3476(12) 0.0907 1.0000 Uani . . . . . . . N201 N 0.5144(7) 0.1213(7) 0.2943(7) 0.0735 1.0000 Uani . . . . . . . C106 C 1.0985(8) 0.9471(8) 0.0125(10) 0.0767 1.0000 Uani . . . . . . . C108 C 1.0874(8) 0.8519(8) 0.1250(8) 0.0766 1.0000 Uani . . . . . . . C109 C 1.0573(8) 0.7423(8) 0.2106(7) 0.0717 1.0000 Uani . . . . . . . C213 C 0.2965(9) 0.2937(9) 0.2156(10) 0.0818 1.0000 Uani . . . . . . . C205 C 0.3976(10) 0.0523(13) 0.5689(14) 0.1092 1.0000 Uani . . . . . . . C209 C 0.4443(10) 0.3398(10) 0.4672(10) 0.0987 1.0000 Uani . . . . . . . C105 C 1.0783(10) 0.9681(9) -0.0717(12) 0.0890 1.0000 Uani . . . . . . . C112 C 1.1991(8) 0.5764(9) 0.1941(11) 0.0823 1.0000 Uani . . . . . . . C212 C 0.2709(10) 0.3484(10) 0.2636(13) 0.1028 1.0000 Uani . . . . . . . C208 C 0.5192(9) 0.2374(10) 0.5690(8) 0.0932 1.0000 Uani . . . . . . . H2161 H 0.6238 0.4711 0.2871 0.0759 1.0000 Uiso R . . . . . . H1181 H 0.7658 0.6634 0.2115 0.0880 1.0000 Uiso R . . . . . . H2181 H 0.7319 0.2788 0.2245 0.0699 1.0000 Uiso R . . . . . . H2201 H 0.7654 0.4069 0.1730 0.0712 1.0000 Uiso R . . . . . . H2191 H 0.6619 0.2034 0.2939 0.0711 1.0000 Uiso R . . . . . . H1201 H 0.7245 0.5366 0.2519 0.0741 1.0000 Uiso R . . . . . . H2031 H 0.4210 0.0485 0.3846 0.0860 1.0000 Uiso R . . . . . . H1031 H 0.9550 0.8236 -0.1445 0.0860 1.0000 Uiso R . . . . . . H1151 H 0.9245 0.5552 0.0627 0.0771 1.0000 Uiso R . . . . . . H1161 H 0.8522 0.4733 0.1249 0.0800 1.0000 Uiso R . . . . . . H1041 H 1.0134 0.9317 -0.1920 0.1100 1.0000 Uiso R . . . . . . H2151 H 0.5491 0.3868 0.3478 0.0849 1.0000 Uiso R . . . . . . H1191 H 0.8319 0.7410 0.1376 0.0899 1.0000 Uiso R . . . . . . H1141 H 1.0787 0.5882 0.0017 0.0769 1.0000 Uiso R . . . . . . H2061 H 0.4414 0.1428 0.6508 0.1230 1.0000 Uiso R . . . . . . H1131 H 1.1901 0.5179 0.0841 0.1009 1.0000 Uiso R . . . . . . H1111 H 1.1853 0.6481 0.2861 0.0940 1.0000 Uiso R . . . . . . H2041 H 0.3577 -0.0214 0.4687 0.1150 1.0000 Uiso R . . . . . . H2141 H 0.3864 0.2181 0.2184 0.0928 1.0000 Uiso R . . . . . . H2111 H 0.2967 0.3944 0.3829 0.1080 1.0000 Uiso R . . . . . . H1061 H 1.1345 0.9779 0.0541 0.0920 1.0000 Uiso R . . . . . . H1081 H 1.0968 0.8980 0.1618 0.0939 1.0000 Uiso R . . . . . . H1082 H 1.1373 0.8210 0.1371 0.0940 1.0000 Uiso R . . . . . . H1091 H 1.0964 0.7683 0.2579 0.0879 1.0000 Uiso R . . . . . . H1092 H 1.0134 0.7202 0.2302 0.0879 1.0000 Uiso R . . . . . . H2131 H 0.2652 0.2822 0.1601 0.0979 1.0000 Uiso R . . . . . . H2051 H 0.3769 0.0230 0.6064 0.1320 1.0000 Uiso R . . . . . . H2091 H 0.4617 0.3946 0.4683 0.1191 1.0000 Uiso R . . . . . . H2092 H 0.4134 0.3326 0.5080 0.1190 1.0000 Uiso R . . . . . . H1051 H 1.0994 1.0145 -0.0879 0.1070 1.0000 Uiso R . . . . . . H1121 H 1.2441 0.5487 0.2276 0.0980 1.0000 Uiso R . . . . . . H2121 H 0.2239 0.3781 0.2395 0.1249 1.0000 Uiso R . . . . . . H2081 H 0.5751 0.2238 0.5993 0.1149 1.0000 Uiso R . . . . . . H2082 H 0.4956 0.2671 0.6069 0.1149 1.0000 Uiso R . . . . . . H2042 H 0.5616 0.3190 0.5077 0.1052 1.0000 Uiso R . . . . . . H1042 H 0.9878 0.8317 0.1593 0.0882 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0549(10) 0.0592(10) 0.0423(8) -0.0009(8) 0.0163(7) -0.0065(8) Fe2 0.0526(10) 0.0654(11) 0.0540(10) -0.0004(9) 0.0191(8) -0.0043(9) S101 0.116(3) 0.080(3) 0.073(2) -0.0155(19) 0.056(2) -0.004(2) S202 0.060(2) 0.119(3) 0.079(2) -0.018(2) 0.0177(18) -0.009(2) S102 0.086(3) 0.102(3) 0.090(3) 0.022(2) 0.033(2) 0.025(2) S201 0.161(5) 0.131(4) 0.161(5) -0.065(4) 0.106(4) -0.029(4) N105 0.055(6) 0.062(6) 0.046(5) 0.005(5) 0.015(5) -0.003(5) N106 0.056(6) 0.044(6) 0.067(6) -0.010(5) 0.028(5) -0.001(4) C117 0.053(7) 0.053(7) 0.071(8) -0.003(6) 0.033(6) -0.002(6) N104 0.083(7) 0.048(6) 0.041(5) -0.005(4) 0.012(5) 0.004(5) C216 0.064(8) 0.052(7) 0.079(9) 0.005(6) 0.031(7) -0.008(6) N203 0.049(6) 0.079(8) 0.047(6) 0.003(5) 0.009(4) 0.001(5) N204 0.064(7) 0.086(8) 0.068(7) -0.007(6) 0.024(5) -0.006(6) C201 0.077(9) 0.064(9) 0.070(9) 0.007(7) 0.033(7) -0.016(7) C118 0.086(10) 0.052(8) 0.105(11) -0.005(7) 0.064(9) 0.007(7) N103 0.058(6) 0.072(7) 0.048(6) 0.009(5) 0.017(5) -0.001(5) C218 0.051(7) 0.071(9) 0.062(7) -0.003(6) 0.031(6) -0.009(6) N206 0.055(6) 0.048(6) 0.058(6) -0.001(5) 0.016(5) 0.003(5) C101 0.041(6) 0.069(8) 0.050(7) 0.009(6) 0.007(5) -0.013(6) C220 0.053(7) 0.076(9) 0.053(7) 0.004(6) 0.025(6) 0.000(6) C110 0.056(7) 0.050(7) 0.062(7) 0.021(6) 0.016(6) -0.001(6) C217 0.047(6) 0.068(8) 0.049(6) -0.002(6) 0.020(5) -0.007(6) C219 0.054(7) 0.051(7) 0.076(8) 0.002(6) 0.024(6) -0.005(6) C210 0.057(8) 0.073(9) 0.076(9) 0.000(7) 0.028(7) 0.007(7) C102 0.073(9) 0.064(8) 0.052(7) 0.004(6) 0.028(7) -0.011(7) N205 0.058(6) 0.069(7) 0.051(6) 0.013(5) 0.011(5) -0.007(5) C202 0.047(7) 0.080(9) 0.069(8) 0.023(7) 0.028(6) 0.012(6) C107 0.058(7) 0.062(8) 0.056(7) 0.005(6) 0.028(6) 0.009(6) C120 0.060(8) 0.075(10) 0.061(8) -0.014(7) 0.027(6) -0.007(7) C203 0.054(8) 0.071(9) 0.088(10) 0.011(8) 0.019(7) -0.016(7) C103 0.096(10) 0.077(9) 0.045(7) -0.006(6) 0.028(7) -0.006(8) C115 0.070(8) 0.057(8) 0.072(8) 0.002(6) 0.037(7) 0.009(6) C116 0.067(8) 0.058(8) 0.090(9) -0.002(7) 0.045(7) -0.005(7) C104 0.117(13) 0.084(11) 0.092(11) 0.023(9) 0.062(11) 0.011(10) C215 0.064(8) 0.064(9) 0.087(10) -0.018(7) 0.023(7) -0.009(7) C119 0.104(11) 0.041(7) 0.106(11) -0.007(7) 0.069(9) 0.003(7) C114 0.072(9) 0.061(8) 0.065(8) -0.007(7) 0.031(7) -0.007(7) N202 0.046(6) 0.085(8) 0.081(8) 0.018(6) 0.018(6) 0.002(6) N102 0.067(7) 0.071(8) 0.092(8) 0.018(7) 0.034(6) 0.003(6) N101 0.089(8) 0.074(8) 0.054(6) -0.017(6) 0.024(6) -0.016(6) C206 0.099(13) 0.149(17) 0.073(10) 0.026(11) 0.045(10) 0.022(12) C113 0.070(9) 0.069(10) 0.114(13) 0.009(9) 0.032(9) 0.026(8) C111 0.081(10) 0.072(10) 0.067(9) 0.019(8) -0.002(8) -0.004(8) C204 0.081(11) 0.105(13) 0.095(12) 0.030(11) 0.016(9) -0.027(9) C207 0.065(8) 0.092(10) 0.051(7) 0.007(7) 0.019(6) 0.002(8) C214 0.069(9) 0.093(11) 0.066(8) 0.014(8) 0.011(7) -0.015(8) C211 0.073(10) 0.073(10) 0.129(15) 0.000(10) 0.033(10) 0.002(8) N201 0.080(8) 0.074(8) 0.074(7) -0.012(6) 0.035(6) -0.006(6) C106 0.070(9) 0.060(9) 0.099(11) 0.010(8) 0.022(8) -0.012(7) C108 0.079(10) 0.079(10) 0.061(8) 0.004(7) 0.004(7) -0.023(8) C109 0.090(10) 0.087(10) 0.034(6) 0.005(6) 0.011(6) -0.005(8) C213 0.069(9) 0.071(10) 0.089(11) 0.009(9) -0.002(8) -0.003(8) C205 0.067(10) 0.134(17) 0.132(17) 0.074(14) 0.038(11) 0.006(11) C209 0.100(12) 0.109(13) 0.084(11) -0.017(10) 0.023(10) 0.015(11) C105 0.108(13) 0.061(9) 0.120(14) 0.015(10) 0.067(11) -0.005(9) C112 0.057(8) 0.080(11) 0.099(12) 0.020(9) 0.005(8) 0.014(8) C212 0.076(11) 0.085(12) 0.127(16) 0.024(11) -0.002(11) 0.008(9) C208 0.090(11) 0.140(15) 0.042(7) -0.016(9) 0.007(7) 0.011(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.094(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N105 . 2.289(10) yes Fe1 . N106 . 2.218(9) yes Fe1 . N104 . 2.216(9) yes Fe1 . N103 . 2.196(10) yes Fe1 . N102 . 2.095(12) yes Fe1 . N101 . 2.085(10) yes Fe2 . N203 . 2.202(10) yes Fe2 . N204 . 2.201(11) yes Fe2 . N206 . 2.220(9) yes Fe2 . N205 . 2.198(10) yes Fe2 . N202 . 2.129(10) yes Fe2 . N201 . 2.106(11) yes S101 . C101 . 1.610(13) yes S202 . C202 . 1.621(13) yes S102 . C102 . 1.631(15) yes S201 . C201 . 1.599(15) yes N105 . C110 . 1.323(14) yes N105 . C114 . 1.351(14) yes N106 . C115 . 1.332(14) yes N106 . C119 . 1.333(13) yes C117 . C118 . 1.339(16) yes C117 . C120 . 1.466(16) yes C117 . C116 . 1.380(15) yes N104 . C108 . 1.493(15) yes N104 . C109 . 1.471(14) yes N104 . H1042 . 0.894 no C216 . C217 . 1.394(15) yes C216 . C215 . 1.407(16) yes C216 . H2161 . 0.927 no N203 . C203 . 1.322(15) yes N203 . C207 . 1.318(15) yes N204 . C209 . 1.481(17) yes N204 . C208 . 1.493(17) yes N204 . H2042 . 0.894 no C201 . N201 . 1.139(15) yes C118 . C119 . 1.386(16) yes C118 . H1181 . 0.928 no N103 . C107 . 1.353(14) yes N103 . C103 . 1.319(14) yes C218 . C217 . 1.372(16) yes C218 . C219 . 1.362(14) yes C218 . H2181 . 0.938 no N206 . C219 . 1.331(14) yes N206 . C215 . 1.327(15) yes C101 . N101 . 1.163(14) yes C220 . C217 . 1.493(15) yes C220 . C120 . 1.312(16) yes C220 . H2201 . 0.930 no C110 . C111 . 1.378(16) yes C110 . C109 . 1.515(17) yes C219 . H2191 . 0.928 no C210 . N205 . 1.347(15) yes C210 . C211 . 1.393(18) yes C210 . C209 . 1.490(18) yes C102 . N102 . 1.152(15) yes N205 . C214 . 1.331(15) yes C202 . N202 . 1.165(14) yes C107 . C106 . 1.388(16) yes C107 . C108 . 1.471(16) yes C120 . H1201 . 0.931 no C203 . C204 . 1.371(18) yes C203 . H2031 . 0.931 no C103 . C104 . 1.388(18) yes C103 . H1031 . 0.932 no C115 . C116 . 1.378(16) yes C115 . H1151 . 0.931 no C116 . H1161 . 0.927 no C104 . C105 . 1.40(2) yes C104 . H1041 . 0.932 no C215 . H2151 . 0.926 no C119 . H1191 . 0.930 no C114 . C113 . 1.384(17) yes C114 . H1141 . 0.933 no C206 . C207 . 1.386(19) yes C206 . C205 . 1.37(2) yes C206 . H2061 . 0.931 no C113 . C112 . 1.373(19) yes C113 . H1131 . 0.931 no C111 . C112 . 1.352(19) yes C111 . H1111 . 0.927 no C204 . C205 . 1.35(2) yes C204 . H2041 . 0.930 no C207 . C208 . 1.502(19) yes C214 . C213 . 1.362(18) yes C214 . H2141 . 0.930 no C211 . C212 . 1.38(2) yes C211 . H2111 . 0.929 no C106 . C105 . 1.361(19) yes C106 . H1061 . 0.929 no C108 . H1081 . 0.965 no C108 . H1082 . 0.968 no C109 . H1091 . 0.966 no C109 . H1092 . 0.972 no C213 . C212 . 1.36(2) yes C213 . H2131 . 0.928 no C205 . H2051 . 0.933 no C209 . H2091 . 0.967 no C209 . H2092 . 0.970 no C105 . H1051 . 0.929 no C112 . H1121 . 0.928 no C212 . H2121 . 0.929 no C208 . H2081 . 0.967 no C208 . H2082 . 0.968 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N105 . Fe1 . N106 . 85.4(3) yes N105 . Fe1 . N104 . 72.9(3) yes N106 . Fe1 . N104 . 95.1(4) yes N105 . Fe1 . N103 . 100.0(3) yes N106 . Fe1 . N103 . 167.7(4) yes N104 . Fe1 . N103 . 76.2(4) yes N105 . Fe1 . N102 . 166.3(4) yes N106 . Fe1 . N102 . 86.9(4) yes N104 . Fe1 . N102 . 96.6(4) yes N103 . Fe1 . N102 . 85.5(4) yes N105 . Fe1 . N101 . 90.5(4) yes N106 . Fe1 . N101 . 97.7(4) yes N104 . Fe1 . N101 . 158.1(4) yes N103 . Fe1 . N101 . 93.4(4) yes N102 . Fe1 . N101 . 101.7(5) yes N203 . Fe2 . N204 . 76.3(4) yes N203 . Fe2 . N206 . 176.0(4) yes N204 . Fe2 . N206 . 99.7(4) yes N203 . Fe2 . N205 . 89.0(3) yes N204 . Fe2 . N205 . 76.8(4) yes N206 . Fe2 . N205 . 90.1(3) yes N203 . Fe2 . N202 . 94.0(4) yes N204 . Fe2 . N202 . 89.4(4) yes N206 . Fe2 . N202 . 85.9(4) yes N205 . Fe2 . N202 . 164.7(4) yes N203 . Fe2 . N201 . 92.8(4) yes N204 . Fe2 . N201 . 165.8(4) yes N206 . Fe2 . N201 . 91.1(4) yes N205 . Fe2 . N201 . 94.2(4) yes N202 . Fe2 . N201 . 100.6(4) yes Fe1 . N105 . C110 . 114.9(8) yes Fe1 . N105 . C114 . 126.8(8) yes C110 . N105 . C114 . 118.3(11) yes Fe1 . N106 . C115 . 122.7(8) yes Fe1 . N106 . C119 . 123.0(8) yes C115 . N106 . C119 . 114.3(10) yes C118 . C117 . C120 . 120.7(11) yes C118 . C117 . C116 . 116.6(11) yes C120 . C117 . C116 . 122.7(11) yes Fe1 . N104 . C108 . 111.2(7) yes Fe1 . N104 . C109 . 107.9(7) yes C108 . N104 . C109 . 111.8(10) yes Fe1 . N104 . H1042 . 109.1 no C108 . N104 . H1042 . 108.5 no C109 . N104 . H1042 . 108.3 no C217 . C216 . C215 . 119.0(12) yes C217 . C216 . H2161 . 120.4 no C215 . C216 . H2161 . 120.6 no Fe2 . N203 . C203 . 127.7(9) yes Fe2 . N203 . C207 . 113.8(9) yes C203 . N203 . C207 . 118.5(12) yes Fe2 . N204 . C209 . 114.6(8) yes Fe2 . N204 . C208 . 106.8(9) yes C209 . N204 . C208 . 112.6(11) yes Fe2 . N204 . H2042 . 107.2 no C209 . N204 . H2042 . 107.8 no C208 . N204 . H2042 . 107.5 no S201 . C201 . N201 . 177.1(12) yes C117 . C118 . C119 . 120.7(11) yes C117 . C118 . H1181 . 119.7 no C119 . C118 . H1181 . 119.6 no Fe1 . N103 . C107 . 116.3(7) yes Fe1 . N103 . C103 . 124.8(9) yes C107 . N103 . C103 . 117.8(11) yes C217 . C218 . C219 . 120.3(11) yes C217 . C218 . H2181 . 120.2 no C219 . C218 . H2181 . 119.6 no Fe2 . N206 . C219 . 121.2(8) yes Fe2 . N206 . C215 . 122.2(8) yes C219 . N206 . C215 . 116.5(11) yes S101 . C101 . N101 . 179.2(12) yes C217 . C220 . C120 . 124.9(11) yes C217 . C220 . H2201 . 117.6 no C120 . C220 . H2201 . 117.5 no N105 . C110 . C111 . 123.2(13) yes N105 . C110 . C109 . 115.1(10) yes C111 . C110 . C109 . 121.7(12) yes C220 . C217 . C216 . 124.0(11) yes C220 . C217 . C218 . 119.2(10) yes C216 . C217 . C218 . 116.7(11) yes C218 . C219 . N206 . 124.4(11) yes C218 . C219 . H2191 . 117.8 no N206 . C219 . H2191 . 117.9 no N205 . C210 . C211 . 120.5(13) yes N205 . C210 . C209 . 119.1(12) yes C211 . C210 . C209 . 120.4(14) yes S102 . C102 . N102 . 177.7(12) yes Fe2 . N205 . C210 . 116.3(8) yes Fe2 . N205 . C214 . 124.9(10) yes C210 . N205 . C214 . 118.7(12) yes S202 . C202 . N202 . 179.3(11) yes N103 . C107 . C106 . 122.1(11) yes N103 . C107 . C108 . 117.2(11) yes C106 . C107 . C108 . 120.6(12) yes C117 . C120 . C220 . 126.2(11) yes C117 . C120 . H1201 . 116.7 no C220 . C120 . H1201 . 117.1 no N203 . C203 . C204 . 124.4(15) yes N203 . C203 . H2031 . 117.9 no C204 . C203 . H2031 . 117.8 no N103 . C103 . C104 . 124.2(14) yes N103 . C103 . H1031 . 117.9 no C104 . C103 . H1031 . 117.9 no N106 . C115 . C116 . 124.7(11) yes N106 . C115 . H1151 . 117.5 no C116 . C115 . H1151 . 117.8 no C117 . C116 . C115 . 119.5(12) yes C117 . C116 . H1161 . 120.5 no C115 . C116 . H1161 . 119.9 no C103 . C104 . C105 . 116.7(14) yes C103 . C104 . H1041 . 121.4 no C105 . C104 . H1041 . 121.9 no C216 . C215 . N206 . 123.0(12) yes C216 . C215 . H2151 . 118.1 no N206 . C215 . H2151 . 118.9 no C118 . C119 . N106 . 124.0(11) yes C118 . C119 . H1191 . 118.2 no N106 . C119 . H1191 . 117.7 no N105 . C114 . C113 . 121.0(12) yes N105 . C114 . H1141 . 119.5 no C113 . C114 . H1141 . 119.5 no Fe2 . N202 . C202 . 149.9(11) yes Fe1 . N102 . C102 . 170.3(11) yes Fe1 . N101 . C101 . 166.5(10) yes C207 . C206 . C205 . 117.4(16) yes C207 . C206 . H2061 . 121.0 no C205 . C206 . H2061 . 121.6 no C114 . C113 . C112 . 119.4(13) yes C114 . C113 . H1131 . 120.1 no C112 . C113 . H1131 . 120.5 no C110 . C111 . C112 . 118.7(14) yes C110 . C111 . H1111 . 120.7 no C112 . C111 . H1111 . 120.6 no C203 . C204 . C205 . 115.9(16) yes C203 . C204 . H2041 . 122.1 no C205 . C204 . H2041 . 121.9 no C206 . C207 . N203 . 121.8(15) yes C206 . C207 . C208 . 120.0(14) yes N203 . C207 . C208 . 118.1(12) yes N205 . C214 . C213 . 123.5(15) yes N205 . C214 . H2141 . 118.1 no C213 . C214 . H2141 . 118.5 no C210 . C211 . C212 . 119.0(16) yes C210 . C211 . H2111 . 120.2 no C212 . C211 . H2111 . 120.9 no Fe2 . N201 . C201 . 156.2(11) yes C107 . C106 . C105 . 118.7(14) yes C107 . C106 . H1061 . 120.4 no C105 . C106 . H1061 . 120.8 no N104 . C108 . C107 . 111.8(10) yes N104 . C108 . H1081 . 110.0 no C107 . C108 . H1081 . 109.1 no N104 . C108 . H1082 . 108.0 no C107 . C108 . H1082 . 108.9 no H1081 . C108 . H1082 . 109.0 no C110 . C109 . N104 . 110.2(9) yes C110 . C109 . H1091 . 109.8 no N104 . C109 . H1091 . 109.7 no C110 . C109 . H1092 . 108.8 no N104 . C109 . H1092 . 109.0 no H1091 . C109 . H1092 . 109.3 no C214 . C213 . C212 . 118.4(15) yes C214 . C213 . H2131 . 120.8 no C212 . C213 . H2131 . 120.8 no C206 . C205 . C204 . 121.9(16) yes C206 . C205 . H2051 . 118.9 no C204 . C205 . H2051 . 119.2 no C210 . C209 . N204 . 112.9(12) yes C210 . C209 . H2091 . 108.0 no N204 . C209 . H2091 . 109.2 no C210 . C209 . H2092 . 109.1 no N204 . C209 . H2092 . 108.2 no H2091 . C209 . H2092 . 109.4 no C104 . C105 . C106 . 120.2(14) yes C104 . C105 . H1051 . 119.8 no C106 . C105 . H1051 . 120.0 no C113 . C112 . C111 . 119.4(13) yes C113 . C112 . H1121 . 120.1 no C111 . C112 . H1121 . 120.5 no C211 . C212 . C213 . 119.7(15) yes C211 . C212 . H2121 . 120.1 no C213 . C212 . H2121 . 120.2 no C207 . C208 . N204 . 110.1(10) yes C207 . C208 . H2081 . 109.1 no N204 . C208 . H2081 . 109.7 no C207 . C208 . H2082 . 109.7 no N204 . C208 . H2082 . 109.0 no H2081 . C208 . H2082 . 109.2 no # Attachment '- compound 3.txt' data_3 _database_code_depnum_ccdc_archive 'CCDC 821198' #TrackingRef '- compound 3.txt' _exptl_special_details ; The crystal was placed in the cold stream of an Oxford Cryosystems open-flow nitrogen cryostat (Cosier & Glazer, 1986) with a nominal stability of 0.1K. Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105 107. ; _refine_special_details ; ? ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 17.092(5) _cell_length_b 16.804(5) _cell_length_c 16.316(5) _cell_angle_alpha 90 _cell_angle_beta 106.911(5) _cell_angle_gamma 90 _cell_volume 4484(2) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C33 H55 Fe2.75 N22 O3 S5.50 # Dc = 1.69 Fooo = 1904.00 Mu = 12.02 M = 1137.89 # Found Formula = C40 H36 Fe2 N12 S4 # Dc = 1.37 FOOO = 1904.00 Mu = 8.77 M = 924.76 _chemical_formula_sum 'C40 H36 Fe2 N12 S4' _chemical_formula_moiety 'C40 H36 Fe2 N12 S4' _chemical_compound_source ? _chemical_formula_weight 924.79 _cell_measurement_reflns_used 3224 _cell_measurement_theta_min 2.8592 _cell_measurement_theta_max 29.2831 _cell_measurement_temperature 293 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.2436 _exptl_crystal_size_mid 0.1149 _exptl_crystal_size_min 0.0959 _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 0.877 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.934 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Mova (Mo) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Eos, Nova' _diffrn_detector_area_resol_mean 15.9897 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 22339 _reflns_number_total 10303 _diffrn_reflns_av_R_equivalents 0.108 # Number of reflections without Friedels Law is 10303 # Number of reflections with Friedels Law is 0 # Theoretical number of reflections is about 12265 _diffrn_reflns_theta_min 2.861 _diffrn_reflns_theta_max 29.306 _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 26.082 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min -22 _reflns_limit_h_max 21 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 21 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.82 _refine_diff_density_max 1.48 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _refine_ls_number_reflns 10295 _refine_ls_number_restraints 0 _refine_ls_number_parameters 523 _oxford_refine_ls_R_factor_ref 0.2297 _refine_ls_wR_factor_ref 0.3065 _refine_ls_goodness_of_fit_ref 1.0625 _refine_ls_shift/su_max 0.0003993 _refine_ls_shift/su_mean 0.0000606 # The values computed from all data _oxford_reflns_number_all 10295 _refine_ls_R_factor_all 0.2297 _refine_ls_wR_factor_all 0.3065 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3229 _refine_ls_R_factor_gt 0.0843 _refine_ls_wR_factor_gt 0.1837 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment none # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 677. 0.102E+04 610. 265. 66.0 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined data collection reference User defined data reduction User defined cell refinement Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.95452(10) 0.73419(10) 0.02622(10) 0.0517 1.0000 Uani . . . . . . . Fe2 Fe 0.53112(10) 0.20673(11) 0.39228(11) 0.0566 1.0000 Uani . . . . . . . S101 S 0.9507(3) 0.5807(2) -0.2247(2) 0.0838 1.0000 Uani . . . . . . . S202 S 0.8093(2) 0.2164(3) 0.5598(2) 0.0866 1.0000 Uani . . . . . . . S102 S 0.7134(3) 0.9006(3) -0.0786(3) 0.0909 1.0000 Uani . . . . . . . S201 S 0.5565(4) 0.0268(3) 0.1772(4) 0.1384 1.0000 Uani . . . . . . . N105 N 1.0665(6) 0.6593(6) 0.0942(6) 0.0542 1.0000 Uani . . . . . . . N106 N 0.8874(6) 0.6573(5) 0.0934(6) 0.0533 1.0000 Uani . . . . . . . C117 C 0.7995(7) 0.5598(7) 0.1762(8) 0.0555 1.0000 Uani . . . . . . . N104 N 1.0226(6) 0.8006(5) 0.1424(5) 0.0586 1.0000 Uani . . . . . . . C216 C 0.6321(7) 0.4166(7) 0.2871(8) 0.0629 1.0000 Uani . . . . . . . N203 N 0.4657(6) 0.1345(6) 0.4639(6) 0.0594 1.0000 Uani . . . . . . . N204 N 0.5174(6) 0.2878(7) 0.4932(7) 0.0719 1.0000 Uani . . . . . . . C201 C 0.5323(8) 0.0836(8) 0.2445(9) 0.0680 1.0000 Uani . . . . . . . C118 C 0.7965(8) 0.6393(7) 0.1799(9) 0.0733 1.0000 Uani . . . . . . . N103 N 1.0142(6) 0.8307(6) -0.0238(6) 0.0586 1.0000 Uani . . . . . . . C218 C 0.6965(7) 0.3034(8) 0.2513(7) 0.0582 1.0000 Uani . . . . . . . N206 N 0.5971(5) 0.2864(6) 0.3263(6) 0.0538 1.0000 Uani . . . . . . . C101 C 0.9419(6) 0.6303(7) -0.1435(7) 0.0546 1.0000 Uani . . . . . . . C220 C 0.7394(7) 0.4334(8) 0.2078(7) 0.0585 1.0000 Uani . . . . . . . C110 C 1.0986(7) 0.6755(7) 0.1766(8) 0.0561 1.0000 Uani . . . . . . . C217 C 0.6894(7) 0.3847(7) 0.2505(7) 0.0534 1.0000 Uani . . . . . . . C219 C 0.6525(7) 0.2579(7) 0.2910(8) 0.0591 1.0000 Uani . . . . . . . C210 C 0.3905(8) 0.3219(8) 0.3795(9) 0.0667 1.0000 Uani . . . . . . . C102 C 0.7948(8) 0.8473(8) -0.0356(8) 0.0609 1.0000 Uani . . . . . . . N205 N 0.4161(6) 0.2693(6) 0.3305(6) 0.0602 1.0000 Uani . . . . . . . C202 C 0.7160(7) 0.1916(8) 0.5093(8) 0.0627 1.0000 Uani . . . . . . . C107 C 1.0650(7) 0.8783(7) 0.0351(7) 0.0562 1.0000 Uani . . . . . . . C120 C 0.7504(7) 0.5105(8) 0.2168(8) 0.0632 1.0000 Uani . . . . . . . C203 C 0.4250(7) 0.0675(8) 0.4394(9) 0.0717 1.0000 Uani . . . . . . . C103 C 0.9938(9) 0.8538(8) -0.1046(8) 0.0710 1.0000 Uani . . . . . . . C115 C 0.8907(7) 0.5782(7) 0.0917(8) 0.0631 1.0000 Uani . . . . . . . C116 C 0.8481(7) 0.5280(8) 0.1301(8) 0.0670 1.0000 Uani . . . . . . . C104 C 1.0258(10) 0.9202(9) -0.1337(11) 0.0908 1.0000 Uani . . . . . . . C215 C 0.5873(8) 0.3648(8) 0.3242(9) 0.0714 1.0000 Uani . . . . . . . C119 C 0.8381(9) 0.6861(7) 0.1364(9) 0.0757 1.0000 Uani . . . . . . . C114 C 1.1003(8) 0.6004(7) 0.0597(8) 0.0637 1.0000 Uani . . . . . . . N202 N 0.6491(6) 0.1742(7) 0.4722(7) 0.0707 1.0000 Uani . . . . . . . N102 N 0.8509(7) 0.8074(7) -0.0062(8) 0.0743 1.0000 Uani . . . . . . . N101 N 0.9360(7) 0.6654(7) -0.0841(7) 0.0717 1.0000 Uani . . . . . . . C206 C 0.4373(10) 0.1224(13) 0.5967(10) 0.1027 1.0000 Uani . . . . . . . C113 C 1.1673(9) 0.5584(9) 0.1087(11) 0.0834 1.0000 Uani . . . . . . . C111 C 1.1647(9) 0.6352(9) 0.2286(9) 0.0782 1.0000 Uani . . . . . . . C204 C 0.3878(9) 0.0244(10) 0.4889(12) 0.0960 1.0000 Uani . . . . . . . C207 C 0.4711(8) 0.1624(9) 0.5408(8) 0.0689 1.0000 Uani . . . . . . . C214 C 0.3688(8) 0.2556(9) 0.2512(9) 0.0778 1.0000 Uani . . . . . . . C211 C 0.3158(9) 0.3609(9) 0.3476(12) 0.0907 1.0000 Uani . . . . . . . N201 N 0.5144(7) 0.1213(7) 0.2943(7) 0.0735 1.0000 Uani . . . . . . . C106 C 1.0985(8) 0.9471(8) 0.0125(10) 0.0767 1.0000 Uani . . . . . . . C108 C 1.0874(8) 0.8519(8) 0.1250(8) 0.0766 1.0000 Uani . . . . . . . C109 C 1.0573(8) 0.7423(8) 0.2106(7) 0.0717 1.0000 Uani . . . . . . . C213 C 0.2965(9) 0.2937(9) 0.2156(10) 0.0818 1.0000 Uani . . . . . . . C205 C 0.3976(10) 0.0523(13) 0.5689(14) 0.1092 1.0000 Uani . . . . . . . C209 C 0.4443(10) 0.3398(10) 0.4672(10) 0.0987 1.0000 Uani . . . . . . . C105 C 1.0783(10) 0.9681(9) -0.0717(12) 0.0890 1.0000 Uani . . . . . . . C112 C 1.1991(8) 0.5764(9) 0.1941(11) 0.0823 1.0000 Uani . . . . . . . C212 C 0.2709(10) 0.3484(10) 0.2636(13) 0.1028 1.0000 Uani . . . . . . . C208 C 0.5192(9) 0.2374(10) 0.5690(8) 0.0932 1.0000 Uani . . . . . . . H2161 H 0.6238 0.4711 0.2871 0.0759 1.0000 Uiso R . . . . . . H1181 H 0.7658 0.6634 0.2115 0.0880 1.0000 Uiso R . . . . . . H2181 H 0.7319 0.2788 0.2245 0.0699 1.0000 Uiso R . . . . . . H2201 H 0.7654 0.4069 0.1730 0.0712 1.0000 Uiso R . . . . . . H2191 H 0.6619 0.2034 0.2939 0.0711 1.0000 Uiso R . . . . . . H1201 H 0.7245 0.5366 0.2519 0.0741 1.0000 Uiso R . . . . . . H2031 H 0.4210 0.0485 0.3846 0.0860 1.0000 Uiso R . . . . . . H1031 H 0.9550 0.8236 -0.1445 0.0860 1.0000 Uiso R . . . . . . H1151 H 0.9245 0.5552 0.0627 0.0771 1.0000 Uiso R . . . . . . H1161 H 0.8522 0.4733 0.1249 0.0800 1.0000 Uiso R . . . . . . H1041 H 1.0134 0.9317 -0.1920 0.1100 1.0000 Uiso R . . . . . . H2151 H 0.5491 0.3868 0.3478 0.0849 1.0000 Uiso R . . . . . . H1191 H 0.8319 0.7410 0.1376 0.0899 1.0000 Uiso R . . . . . . H1141 H 1.0787 0.5882 0.0017 0.0769 1.0000 Uiso R . . . . . . H2061 H 0.4414 0.1428 0.6508 0.1230 1.0000 Uiso R . . . . . . H1131 H 1.1901 0.5179 0.0841 0.1009 1.0000 Uiso R . . . . . . H1111 H 1.1853 0.6481 0.2861 0.0940 1.0000 Uiso R . . . . . . H2041 H 0.3577 -0.0214 0.4687 0.1150 1.0000 Uiso R . . . . . . H2141 H 0.3864 0.2181 0.2184 0.0928 1.0000 Uiso R . . . . . . H2111 H 0.2967 0.3944 0.3829 0.1080 1.0000 Uiso R . . . . . . H1061 H 1.1345 0.9779 0.0541 0.0920 1.0000 Uiso R . . . . . . H1081 H 1.0968 0.8980 0.1618 0.0939 1.0000 Uiso R . . . . . . H1082 H 1.1373 0.8210 0.1371 0.0940 1.0000 Uiso R . . . . . . H1091 H 1.0964 0.7683 0.2579 0.0879 1.0000 Uiso R . . . . . . H1092 H 1.0134 0.7202 0.2302 0.0879 1.0000 Uiso R . . . . . . H2131 H 0.2652 0.2822 0.1601 0.0979 1.0000 Uiso R . . . . . . H2051 H 0.3769 0.0230 0.6064 0.1320 1.0000 Uiso R . . . . . . H2091 H 0.4617 0.3946 0.4683 0.1191 1.0000 Uiso R . . . . . . H2092 H 0.4134 0.3326 0.5080 0.1190 1.0000 Uiso R . . . . . . H1051 H 1.0994 1.0145 -0.0879 0.1070 1.0000 Uiso R . . . . . . H1121 H 1.2441 0.5487 0.2276 0.0980 1.0000 Uiso R . . . . . . H2121 H 0.2239 0.3781 0.2395 0.1249 1.0000 Uiso R . . . . . . H2081 H 0.5751 0.2238 0.5993 0.1149 1.0000 Uiso R . . . . . . H2082 H 0.4956 0.2671 0.6069 0.1149 1.0000 Uiso R . . . . . . H2042 H 0.5616 0.3190 0.5077 0.1052 1.0000 Uiso R . . . . . . H1042 H 0.9878 0.8317 0.1593 0.0882 1.0000 Uiso R . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0549(10) 0.0592(10) 0.0423(8) -0.0009(8) 0.0163(7) -0.0065(8) Fe2 0.0526(10) 0.0654(11) 0.0540(10) -0.0004(9) 0.0191(8) -0.0043(9) S101 0.116(3) 0.080(3) 0.073(2) -0.0155(19) 0.056(2) -0.004(2) S202 0.060(2) 0.119(3) 0.079(2) -0.018(2) 0.0177(18) -0.009(2) S102 0.086(3) 0.102(3) 0.090(3) 0.022(2) 0.033(2) 0.025(2) S201 0.161(5) 0.131(4) 0.161(5) -0.065(4) 0.106(4) -0.029(4) N105 0.055(6) 0.062(6) 0.046(5) 0.005(5) 0.015(5) -0.003(5) N106 0.056(6) 0.044(6) 0.067(6) -0.010(5) 0.028(5) -0.001(4) C117 0.053(7) 0.053(7) 0.071(8) -0.003(6) 0.033(6) -0.002(6) N104 0.083(7) 0.048(6) 0.041(5) -0.005(4) 0.012(5) 0.004(5) C216 0.064(8) 0.052(7) 0.079(9) 0.005(6) 0.031(7) -0.008(6) N203 0.049(6) 0.079(8) 0.047(6) 0.003(5) 0.009(4) 0.001(5) N204 0.064(7) 0.086(8) 0.068(7) -0.007(6) 0.024(5) -0.006(6) C201 0.077(9) 0.064(9) 0.070(9) 0.007(7) 0.033(7) -0.016(7) C118 0.086(10) 0.052(8) 0.105(11) -0.005(7) 0.064(9) 0.007(7) N103 0.058(6) 0.072(7) 0.048(6) 0.009(5) 0.017(5) -0.001(5) C218 0.051(7) 0.071(9) 0.062(7) -0.003(6) 0.031(6) -0.009(6) N206 0.055(6) 0.048(6) 0.058(6) -0.001(5) 0.016(5) 0.003(5) C101 0.041(6) 0.069(8) 0.050(7) 0.009(6) 0.007(5) -0.013(6) C220 0.053(7) 0.076(9) 0.053(7) 0.004(6) 0.025(6) 0.000(6) C110 0.056(7) 0.050(7) 0.062(7) 0.021(6) 0.016(6) -0.001(6) C217 0.047(6) 0.068(8) 0.049(6) -0.002(6) 0.020(5) -0.007(6) C219 0.054(7) 0.051(7) 0.076(8) 0.002(6) 0.024(6) -0.005(6) C210 0.057(8) 0.073(9) 0.076(9) 0.000(7) 0.028(7) 0.007(7) C102 0.073(9) 0.064(8) 0.052(7) 0.004(6) 0.028(7) -0.011(7) N205 0.058(6) 0.069(7) 0.051(6) 0.013(5) 0.011(5) -0.007(5) C202 0.047(7) 0.080(9) 0.069(8) 0.023(7) 0.028(6) 0.012(6) C107 0.058(7) 0.062(8) 0.056(7) 0.005(6) 0.028(6) 0.009(6) C120 0.060(8) 0.075(10) 0.061(8) -0.014(7) 0.027(6) -0.007(7) C203 0.054(8) 0.071(9) 0.088(10) 0.011(8) 0.019(7) -0.016(7) C103 0.096(10) 0.077(9) 0.045(7) -0.006(6) 0.028(7) -0.006(8) C115 0.070(8) 0.057(8) 0.072(8) 0.002(6) 0.037(7) 0.009(6) C116 0.067(8) 0.058(8) 0.090(9) -0.002(7) 0.045(7) -0.005(7) C104 0.117(13) 0.084(11) 0.092(11) 0.023(9) 0.062(11) 0.011(10) C215 0.064(8) 0.064(9) 0.087(10) -0.018(7) 0.023(7) -0.009(7) C119 0.104(11) 0.041(7) 0.106(11) -0.007(7) 0.069(9) 0.003(7) C114 0.072(9) 0.061(8) 0.065(8) -0.007(7) 0.031(7) -0.007(7) N202 0.046(6) 0.085(8) 0.081(8) 0.018(6) 0.018(6) 0.002(6) N102 0.067(7) 0.071(8) 0.092(8) 0.018(7) 0.034(6) 0.003(6) N101 0.089(8) 0.074(8) 0.054(6) -0.017(6) 0.024(6) -0.016(6) C206 0.099(13) 0.149(17) 0.073(10) 0.026(11) 0.045(10) 0.022(12) C113 0.070(9) 0.069(10) 0.114(13) 0.009(9) 0.032(9) 0.026(8) C111 0.081(10) 0.072(10) 0.067(9) 0.019(8) -0.002(8) -0.004(8) C204 0.081(11) 0.105(13) 0.095(12) 0.030(11) 0.016(9) -0.027(9) C207 0.065(8) 0.092(10) 0.051(7) 0.007(7) 0.019(6) 0.002(8) C214 0.069(9) 0.093(11) 0.066(8) 0.014(8) 0.011(7) -0.015(8) C211 0.073(10) 0.073(10) 0.129(15) 0.000(10) 0.033(10) 0.002(8) N201 0.080(8) 0.074(8) 0.074(7) -0.012(6) 0.035(6) -0.006(6) C106 0.070(9) 0.060(9) 0.099(11) 0.010(8) 0.022(8) -0.012(7) C108 0.079(10) 0.079(10) 0.061(8) 0.004(7) 0.004(7) -0.023(8) C109 0.090(10) 0.087(10) 0.034(6) 0.005(6) 0.011(6) -0.005(8) C213 0.069(9) 0.071(10) 0.089(11) 0.009(9) -0.002(8) -0.003(8) C205 0.067(10) 0.134(17) 0.132(17) 0.074(14) 0.038(11) 0.006(11) C209 0.100(12) 0.109(13) 0.084(11) -0.017(10) 0.023(10) 0.015(11) C105 0.108(13) 0.061(9) 0.120(14) 0.015(10) 0.067(11) -0.005(9) C112 0.057(8) 0.080(11) 0.099(12) 0.020(9) 0.005(8) 0.014(8) C212 0.076(11) 0.085(12) 0.127(16) 0.024(11) -0.002(11) 0.008(9) C208 0.090(11) 0.140(15) 0.042(7) -0.016(9) 0.007(7) 0.011(11) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.094(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . N105 . 2.289(10) yes Fe1 . N106 . 2.218(9) yes Fe1 . N104 . 2.216(9) yes Fe1 . N103 . 2.196(10) yes Fe1 . N102 . 2.095(12) yes Fe1 . N101 . 2.085(10) yes Fe2 . N203 . 2.202(10) yes Fe2 . N204 . 2.201(11) yes Fe2 . N206 . 2.220(9) yes Fe2 . N205 . 2.198(10) yes Fe2 . N202 . 2.129(10) yes Fe2 . N201 . 2.106(11) yes S101 . C101 . 1.610(13) yes S202 . C202 . 1.621(13) yes S102 . C102 . 1.631(15) yes S201 . C201 . 1.599(15) yes N105 . C110 . 1.323(14) yes N105 . C114 . 1.351(14) yes N106 . C115 . 1.332(14) yes N106 . C119 . 1.333(13) yes C117 . C118 . 1.339(16) yes C117 . C120 . 1.466(16) yes C117 . C116 . 1.380(15) yes N104 . C108 . 1.493(15) yes N104 . C109 . 1.471(14) yes N104 . H1042 . 0.894 no C216 . C217 . 1.394(15) yes C216 . C215 . 1.407(16) yes C216 . H2161 . 0.927 no N203 . C203 . 1.322(15) yes N203 . C207 . 1.318(15) yes N204 . C209 . 1.481(17) yes N204 . C208 . 1.493(17) yes N204 . H2042 . 0.894 no C201 . N201 . 1.139(15) yes C118 . C119 . 1.386(16) yes C118 . H1181 . 0.928 no N103 . C107 . 1.353(14) yes N103 . C103 . 1.319(14) yes C218 . C217 . 1.372(16) yes C218 . C219 . 1.362(14) yes C218 . H2181 . 0.938 no N206 . C219 . 1.331(14) yes N206 . C215 . 1.327(15) yes C101 . N101 . 1.163(14) yes C220 . C217 . 1.493(15) yes C220 . C120 . 1.312(16) yes C220 . H2201 . 0.930 no C110 . C111 . 1.378(16) yes C110 . C109 . 1.515(17) yes C219 . H2191 . 0.928 no C210 . N205 . 1.347(15) yes C210 . C211 . 1.393(18) yes C210 . C209 . 1.490(18) yes C102 . N102 . 1.152(15) yes N205 . C214 . 1.331(15) yes C202 . N202 . 1.165(14) yes C107 . C106 . 1.388(16) yes C107 . C108 . 1.471(16) yes C120 . H1201 . 0.931 no C203 . C204 . 1.371(18) yes C203 . H2031 . 0.931 no C103 . C104 . 1.388(18) yes C103 . H1031 . 0.932 no C115 . C116 . 1.378(16) yes C115 . H1151 . 0.931 no C116 . H1161 . 0.927 no C104 . C105 . 1.40(2) yes C104 . H1041 . 0.932 no C215 . H2151 . 0.926 no C119 . H1191 . 0.930 no C114 . C113 . 1.384(17) yes C114 . H1141 . 0.933 no C206 . C207 . 1.386(19) yes C206 . C205 . 1.37(2) yes C206 . H2061 . 0.931 no C113 . C112 . 1.373(19) yes C113 . H1131 . 0.931 no C111 . C112 . 1.352(19) yes C111 . H1111 . 0.927 no C204 . C205 . 1.35(2) yes C204 . H2041 . 0.930 no C207 . C208 . 1.502(19) yes C214 . C213 . 1.362(18) yes C214 . H2141 . 0.930 no C211 . C212 . 1.38(2) yes C211 . H2111 . 0.929 no C106 . C105 . 1.361(19) yes C106 . H1061 . 0.929 no C108 . H1081 . 0.965 no C108 . H1082 . 0.968 no C109 . H1091 . 0.966 no C109 . H1092 . 0.972 no C213 . C212 . 1.36(2) yes C213 . H2131 . 0.928 no C205 . H2051 . 0.933 no C209 . H2091 . 0.967 no C209 . H2092 . 0.970 no C105 . H1051 . 0.929 no C112 . H1121 . 0.928 no C212 . H2121 . 0.929 no C208 . H2081 . 0.967 no C208 . H2082 . 0.968 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N105 . Fe1 . N106 . 85.4(3) yes N105 . Fe1 . N104 . 72.9(3) yes N106 . Fe1 . N104 . 95.1(4) yes N105 . Fe1 . N103 . 100.0(3) yes N106 . Fe1 . N103 . 167.7(4) yes N104 . Fe1 . N103 . 76.2(4) yes N105 . Fe1 . N102 . 166.3(4) yes N106 . Fe1 . N102 . 86.9(4) yes N104 . Fe1 . N102 . 96.6(4) yes N103 . Fe1 . N102 . 85.5(4) yes N105 . Fe1 . N101 . 90.5(4) yes N106 . Fe1 . N101 . 97.7(4) yes N104 . Fe1 . N101 . 158.1(4) yes N103 . Fe1 . N101 . 93.4(4) yes N102 . Fe1 . N101 . 101.7(5) yes N203 . Fe2 . N204 . 76.3(4) yes N203 . Fe2 . N206 . 176.0(4) yes N204 . Fe2 . N206 . 99.7(4) yes N203 . Fe2 . N205 . 89.0(3) yes N204 . Fe2 . N205 . 76.8(4) yes N206 . Fe2 . N205 . 90.1(3) yes N203 . Fe2 . N202 . 94.0(4) yes N204 . Fe2 . N202 . 89.4(4) yes N206 . Fe2 . N202 . 85.9(4) yes N205 . Fe2 . N202 . 164.7(4) yes N203 . Fe2 . N201 . 92.8(4) yes N204 . Fe2 . N201 . 165.8(4) yes N206 . Fe2 . N201 . 91.1(4) yes N205 . Fe2 . N201 . 94.2(4) yes N202 . Fe2 . N201 . 100.6(4) yes Fe1 . N105 . C110 . 114.9(8) yes Fe1 . N105 . C114 . 126.8(8) yes C110 . N105 . C114 . 118.3(11) yes Fe1 . N106 . C115 . 122.7(8) yes Fe1 . N106 . C119 . 123.0(8) yes C115 . N106 . C119 . 114.3(10) yes C118 . C117 . C120 . 120.7(11) yes C118 . C117 . C116 . 116.6(11) yes C120 . C117 . C116 . 122.7(11) yes Fe1 . N104 . C108 . 111.2(7) yes Fe1 . N104 . C109 . 107.9(7) yes C108 . N104 . C109 . 111.8(10) yes Fe1 . N104 . H1042 . 109.1 no C108 . N104 . H1042 . 108.5 no C109 . N104 . H1042 . 108.3 no C217 . C216 . C215 . 119.0(12) yes C217 . C216 . H2161 . 120.4 no C215 . C216 . H2161 . 120.6 no Fe2 . N203 . C203 . 127.7(9) yes Fe2 . N203 . C207 . 113.8(9) yes C203 . N203 . C207 . 118.5(12) yes Fe2 . N204 . C209 . 114.6(8) yes Fe2 . N204 . C208 . 106.8(9) yes C209 . N204 . C208 . 112.6(11) yes Fe2 . N204 . H2042 . 107.2 no C209 . N204 . H2042 . 107.8 no C208 . N204 . H2042 . 107.5 no S201 . C201 . N201 . 177.1(12) yes C117 . C118 . C119 . 120.7(11) yes C117 . C118 . H1181 . 119.7 no C119 . C118 . H1181 . 119.6 no Fe1 . N103 . C107 . 116.3(7) yes Fe1 . N103 . C103 . 124.8(9) yes C107 . N103 . C103 . 117.8(11) yes C217 . C218 . C219 . 120.3(11) yes C217 . C218 . H2181 . 120.2 no C219 . C218 . H2181 . 119.6 no Fe2 . N206 . C219 . 121.2(8) yes Fe2 . N206 . C215 . 122.2(8) yes C219 . N206 . C215 . 116.5(11) yes S101 . C101 . N101 . 179.2(12) yes C217 . C220 . C120 . 124.9(11) yes C217 . C220 . H2201 . 117.6 no C120 . C220 . H2201 . 117.5 no N105 . C110 . C111 . 123.2(13) yes N105 . C110 . C109 . 115.1(10) yes C111 . C110 . C109 . 121.7(12) yes C220 . C217 . C216 . 124.0(11) yes C220 . C217 . C218 . 119.2(10) yes C216 . C217 . C218 . 116.7(11) yes C218 . C219 . N206 . 124.4(11) yes C218 . C219 . H2191 . 117.8 no N206 . C219 . H2191 . 117.9 no N205 . C210 . C211 . 120.5(13) yes N205 . C210 . C209 . 119.1(12) yes C211 . C210 . C209 . 120.4(14) yes S102 . C102 . N102 . 177.7(12) yes Fe2 . N205 . C210 . 116.3(8) yes Fe2 . N205 . C214 . 124.9(10) yes C210 . N205 . C214 . 118.7(12) yes S202 . C202 . N202 . 179.3(11) yes N103 . C107 . C106 . 122.1(11) yes N103 . C107 . C108 . 117.2(11) yes C106 . C107 . C108 . 120.6(12) yes C117 . C120 . C220 . 126.2(11) yes C117 . C120 . H1201 . 116.7 no C220 . C120 . H1201 . 117.1 no N203 . C203 . C204 . 124.4(15) yes N203 . C203 . H2031 . 117.9 no C204 . C203 . H2031 . 117.8 no N103 . C103 . C104 . 124.2(14) yes N103 . C103 . H1031 . 117.9 no C104 . C103 . H1031 . 117.9 no N106 . C115 . C116 . 124.7(11) yes N106 . C115 . H1151 . 117.5 no C116 . C115 . H1151 . 117.8 no C117 . C116 . C115 . 119.5(12) yes C117 . C116 . H1161 . 120.5 no C115 . C116 . H1161 . 119.9 no C103 . C104 . C105 . 116.7(14) yes C103 . C104 . H1041 . 121.4 no C105 . C104 . H1041 . 121.9 no C216 . C215 . N206 . 123.0(12) yes C216 . C215 . H2151 . 118.1 no N206 . C215 . H2151 . 118.9 no C118 . C119 . N106 . 124.0(11) yes C118 . C119 . H1191 . 118.2 no N106 . C119 . H1191 . 117.7 no N105 . C114 . C113 . 121.0(12) yes N105 . C114 . H1141 . 119.5 no C113 . C114 . H1141 . 119.5 no Fe2 . N202 . C202 . 149.9(11) yes Fe1 . N102 . C102 . 170.3(11) yes Fe1 . N101 . C101 . 166.5(10) yes C207 . C206 . C205 . 117.4(16) yes C207 . C206 . H2061 . 121.0 no C205 . C206 . H2061 . 121.6 no C114 . C113 . C112 . 119.4(13) yes C114 . C113 . H1131 . 120.1 no C112 . C113 . H1131 . 120.5 no C110 . C111 . C112 . 118.7(14) yes C110 . C111 . H1111 . 120.7 no C112 . C111 . H1111 . 120.6 no C203 . C204 . C205 . 115.9(16) yes C203 . C204 . H2041 . 122.1 no C205 . C204 . H2041 . 121.9 no C206 . C207 . N203 . 121.8(15) yes C206 . C207 . C208 . 120.0(14) yes N203 . C207 . C208 . 118.1(12) yes N205 . C214 . C213 . 123.5(15) yes N205 . C214 . H2141 . 118.1 no C213 . C214 . H2141 . 118.5 no C210 . C211 . C212 . 119.0(16) yes C210 . C211 . H2111 . 120.2 no C212 . C211 . H2111 . 120.9 no Fe2 . N201 . C201 . 156.2(11) yes C107 . C106 . C105 . 118.7(14) yes C107 . C106 . H1061 . 120.4 no C105 . C106 . H1061 . 120.8 no N104 . C108 . C107 . 111.8(10) yes N104 . C108 . H1081 . 110.0 no C107 . C108 . H1081 . 109.1 no N104 . C108 . H1082 . 108.0 no C107 . C108 . H1082 . 108.9 no H1081 . C108 . H1082 . 109.0 no C110 . C109 . N104 . 110.2(9) yes C110 . C109 . H1091 . 109.8 no N104 . C109 . H1091 . 109.7 no C110 . C109 . H1092 . 108.8 no N104 . C109 . H1092 . 109.0 no H1091 . C109 . H1092 . 109.3 no C214 . C213 . C212 . 118.4(15) yes C214 . C213 . H2131 . 120.8 no C212 . C213 . H2131 . 120.8 no C206 . C205 . C204 . 121.9(16) yes C206 . C205 . H2051 . 118.9 no C204 . C205 . H2051 . 119.2 no C210 . C209 . N204 . 112.9(12) yes C210 . C209 . H2091 . 108.0 no N204 . C209 . H2091 . 109.2 no C210 . C209 . H2092 . 109.1 no N204 . C209 . H2092 . 108.2 no H2091 . C209 . H2092 . 109.4 no C104 . C105 . C106 . 120.2(14) yes C104 . C105 . H1051 . 119.8 no C106 . C105 . H1051 . 120.0 no C113 . C112 . C111 . 119.4(13) yes C113 . C112 . H1121 . 120.1 no C111 . C112 . H1121 . 120.5 no C211 . C212 . C213 . 119.7(15) yes C211 . C212 . H2121 . 120.1 no C213 . C212 . H2121 . 120.2 no C207 . C208 . N204 . 110.1(10) yes C207 . C208 . H2081 . 109.1 no N204 . C208 . H2081 . 109.7 no C207 . C208 . H2082 . 109.7 no N204 . C208 . H2082 . 109.0 no H2081 . C208 . H2082 . 109.2 no # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.687 0.083 0.048 64 15 ' ' 2 0.313 0.917 -0.049 64 15 ' ' 3 0.313 0.583 0.451 64 15 ' ' 4 0.687 0.417 0.548 64 15 ' ' _platon_squeeze_details ; ;