# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name _publ_author_address 'Evans, Nicholas' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, United Kingdom ; 'Davis, Jason' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, United Kingdom ; 'Beer, P. D.' ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, United Kingdom ; _publ_contact_author_name 'Mr Nicholas Evans' _publ_contact_author_email nicholas.evans@durham.ac.uk _publ_section_title ; Solution and surface-confined chloride anion templated redox-active ferrocene catenanes ; _publ_contact_author_address ; Chemistry Research Laboratory, University of Oxford, Mansfield Road, Oxford OX1 3TA, UK. ; _publ_contact_author_fax '+44 1865 272690' _publ_contact_author_phone '+44 1865 285142' #looking for refcif # Check this file using the IUCr facility at: # http://checkcif.iucr.org/ # The content below is held in the file 'script/refcif.dat'. This is a text # file which you may edit to reflect local conditions. # Items which need looking at are represented by a '?'. # Items for which there are choices are prefixed with 'choose from'. _publ_contact_letter ; ; _publ_requested_category FA # choose from: FI FM FO CI CM CO AD _publ_requested_journal Journal # Attachment '- 1 Macrocycle 1 003CJS11.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 853868' #TrackingRef '- 1 Macrocycle 1 003CJS11.cif' _audit_creation_date 11-02-04 _audit_creation_method CRYSTALS_ver_14.07 _oxford_structure_analysis_title 003CJS11 _chemical_name_systematic . _chemical_melting_point . # start Validation Reply Form _vrf_REFNR01_8 ; PROBLEM: Ratio of reflections to parameters is < 6 for a centrosymmetric structure sine(theta)/lambda 0.4166 Proportion of unique data used 0.9728 Ratio reflections to parameters 4.6920 RESPONSE: The sample diffracted very weakly, and at high angles the reflections were completely absent, even when subjected to synchrotron radiation. Dispite the poor quality of the data, the connectivity and gross conformation are not in doubt. ; _vrf_THETM01_8 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 Calculated sin(theta_max)/wavelength = 0.4166 RESPONSE: The sample diffracted very weakly, and at high angles the reflections were completely absent, even when subjected to synchrotron radiation. Dispite the poor quality of the data, the connectivity and gross conformation are not in doubt. ; _vrf_PLAT023_8 ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 16.68 Deg. RESPONSE: The sample diffracted very weakly, and at high angles the reflections were completely absent, even when subjected to synchrotron radiation. Dispite the poor quality of the data, the connectivity and gross conformation are not in doubt. ; _vrf_PLAT027_8 ; PROBLEM: _diffrn_reflns_theta_full (too) Low ............ 14.34 Deg. RESPONSE: The sample diffracted very weakly, and at high angles the reflections were completely absent, even when subjected to synchrotron radiation. Dispite the poor quality of the data, the connectivity and gross conformation are not in doubt. ; _vrf_PLAT088_8 ; PROBLEM: Poor Data / Parameter Ratio .................... 4.69 RESPONSE: The sample diffracted very weakly, and at high angles the reflections were completely absent, even when subjected to synchrotron radiation. This resulted in a low total number of reflections, and hence a poor data:parameter ratio. Dispite the low quality of the data, the connectivity and gross conformation are not in doubt. ; # end Validation Reply Form _refine_special_details ; After partial structure solution using Superflip, the remainder of the molecule was assembled using cycles of Fourier refinement. After geometric placement of hydrogen atoms, a small solvent void remained, in which no satisfactory solvent model could be constructed. PLATON SQUEEZE was used in include this volume in the refinement. ; # 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 0.237 0.121 0.211 39 5 ' ' 2 0.237 0.379 0.711 39 5 ' ' 3 0.763 0.621 0.289 39 5 ' ' 4 0.763 0.879 0.789 39 5 ' ' _platon_squeeze_details ; ; _cell_length_a 13.831(6) _cell_length_b 16.175(7) _cell_length_c 18.572(9) _cell_angle_alpha 90 _cell_angle_beta 111.60(6) _cell_angle_gamma 90 _cell_volume 3863(3) _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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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' 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' _cell_formula_units_Z 4 # Given Formula = C18 Fe1 N2 O9 # Dc = 0.76 Fooo = 1640.00 Mu = 4.17 M = 444.05 # Found Formula = C42 H46 Fe1 N2 O9 # Dc = 1.34 FOOO = 1640.00 Mu = 4.49 M = 778.68 _chemical_formula_sum 'C42 H46 Fe1 N2 O9' _chemical_formula_moiety 'C42 H46 Fe1 N2 O9' _chemical_compound_source . _chemical_formula_weight 778.68 _cell_measurement_reflns_used 2618 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.011 _exptl_crystal_size_mid 0.021 _exptl_crystal_size_max 0.032 _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 0.449 # Sheldrick geometric approximatio 0.99 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.61 _exptl_absorpt_correction_T_max 1.00 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.68890 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 150 _diffrn_reflns_number 2325 _reflns_number_total 2349 _diffrn_reflns_av_R_equivalents 0.174 # Number of reflections without Friedels Law is 4441 # Number of reflections with Friedels Law is 2349 # Theoretical number of reflections is about 2340 _diffrn_reflns_theta_min 1.535 _diffrn_reflns_theta_max 16.679 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 14.344 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min 0 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 15 _oxford_diffrn_Wilson_B_factor 4.87 _oxford_diffrn_Wilson_scale 0.22 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.85 _refine_diff_density_max 0.73 # 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>-3.0\s(I) _refine_ls_number_reflns 2285 _refine_ls_number_restraints 606 _refine_ls_number_parameters 487 _oxford_refine_ls_R_factor_ref 0.1588 _refine_ls_wR_factor_ref 0.2217 _refine_ls_goodness_of_fit_ref 1.0844 _refine_ls_shift/su_max 0.0001150 _refine_ls_shift/su_mean 0.0000180 # The values computed from all data _oxford_reflns_number_all 2285 _refine_ls_R_factor_all 0.1588 _refine_ls_wR_factor_all 0.2217 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1132 _refine_ls_R_factor_gt 0.0841 _refine_ls_wR_factor_gt 0.1624 # 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: 0.218E+04 0.304E+04 0.166E+04 549. ; # 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. 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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. 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 Fe1 Fe 0.3287(2) 0.4143(2) 0.19551(16) 0.0768 1.0000 Uani . U . . . . . O2 O 0.3019(10) 0.0946(9) 1.0194(7) 0.0811 1.0000 Uani . U . . . . . C3 C 0.3898(15) 0.1422(13) 1.0507(12) 0.0843 1.0000 Uani . U . . . . . C4 C 0.4813(15) 0.1021(14) 1.0394(12) 0.0863 1.0000 Uani . U . . . . . O5 O 0.5662(11) 0.1612(8) 1.0621(7) 0.0796 1.0000 Uani . U . . . . . C6 C 0.6670(15) 0.1288(13) 1.0785(11) 0.0798 1.0000 Uani . U . . . . . C7 C 0.6892(17) 0.1044(14) 1.0082(11) 0.0859 1.0000 Uani . U . . . . . O8 O 0.6883(11) 0.1785(9) 0.9657(8) 0.0902 1.0000 Uani . U . . . . . C9 C 0.6922(16) 0.1704(15) 0.8911(13) 0.0786 1.0000 Uani . U . . . . . C10 C 0.2182(15) 0.1348(13) 1.0286(11) 0.0799 1.0000 Uani . U . . . . . C11 C 0.1187(15) 0.0878(14) 0.9899(10) 0.0812 1.0000 Uani . U . . . . . O12 O 0.0883(10) 0.0862(9) 0.9067(7) 0.0799 1.0000 Uani . U . . . . . C13 C -0.0080(16) 0.0427(14) 0.8688(10) 0.0866 1.0000 Uani . U . . . . . C14 C -0.0265(16) 0.0447(13) 0.7842(10) 0.0800 1.0000 Uani . U . . . . . O15 O -0.0406(10) 0.1268(8) 0.7571(7) 0.0793 1.0000 Uani . U . . . . . C16 C -0.0438(16) 0.1450(14) 0.6824(12) 0.0748 1.0000 Uani . U . . . . . O17 O 0.0985(11) 0.1032(9) 0.3384(7) 0.0912 1.0000 Uani . U . . . . . C18 C 0.1184(18) 0.1790(16) 0.3518(11) 0.0732 1.0000 Uani . U . . . . . N19 N 0.0441(12) 0.2273(11) 0.3554(8) 0.0703 1.0000 Uani . U . . . . . C20 C -0.0587(15) 0.1985(13) 0.3417(10) 0.0756 1.0000 Uani . U . . . . . C21 C -0.0643(16) 0.1563(13) 0.4114(10) 0.0785 1.0000 Uani . U . . . . . O22 O -0.0542(10) 0.2181(8) 0.4677(7) 0.0784 1.0000 Uani . U . . . . . C23 C -0.0519(14) 0.1880(14) 0.5376(11) 0.0659 1.0000 Uani . U . . . . . O24 O 0.6860(10) 0.1747(9) 0.6673(8) 0.0812 1.0000 Uani . U . . . . . C25 C 0.6788(15) 0.0976(13) 0.6246(10) 0.0764 1.0000 Uani . U . . . . . C26 C 0.6724(15) 0.1229(13) 0.5457(11) 0.0829 1.0000 Uani . U . . . . . N27 N 0.5751(12) 0.1674(10) 0.5025(8) 0.0718 1.0000 Uani . U . . . . . C28 C 0.498(2) 0.1343(17) 0.4428(15) 0.0947 1.0000 Uani . U . . . . . O29 O 0.4985(13) 0.0634(11) 0.4228(11) 0.1545 1.0000 Uani . U . . . . . C30 C 0.6883(15) 0.1670(15) 0.7429(13) 0.0745 1.0000 Uani . U . . . . . C1 C 0.7076(15) 0.0982(15) 0.8603(12) 0.0790 1.0000 Uani . U . . . . . C2 C 0.3664(19) 0.4076(15) 0.0991(11) 0.0943 1.0000 Uani . U . . . . . C5 C -0.0522(14) 0.2491(14) 0.5901(11) 0.0746 1.0000 Uani . U . . . . . C8 C 0.6740(15) 0.2411(14) 0.7742(12) 0.0803 1.0000 Uani . U . . . . . C12 C 0.3059(18) 0.5212(14) 0.2425(11) 0.0841 1.0000 Uani . U . . . . . C15 C 0.4113(18) 0.5102(14) 0.2637(11) 0.0873 1.0000 Uani . U . . . . . C17 C 0.2227(17) 0.2083(14) 0.3609(10) 0.0690 1.0000 Uani . U . . . . . C19 C 0.7049(15) 0.0917(14) 0.7846(11) 0.0805 1.0000 Uani . U . . . . . C22 C 0.3110(17) 0.1608(14) 0.3946(10) 0.0748 1.0000 Uani . U . . . . . C24 C 0.2330(16) 0.2875(13) 0.3355(10) 0.0707 1.0000 Uani . U . . . . . C27 C 0.4076(17) 0.1884(14) 0.4061(10) 0.0661 1.0000 Uani . U . . . . . C29 C -0.0561(14) 0.1048(13) 0.5584(11) 0.0727 1.0000 Uani . U . . . . . C31 C 0.2216(19) 0.3442(15) 0.1111(12) 0.0962 1.0000 Uani . U . . . . . C32 C 0.6758(15) 0.2433(14) 0.8473(12) 0.0818 1.0000 Uani . U . . . . . C33 C 0.3428(17) 0.4017(15) 0.3070(11) 0.0815 1.0000 Uani . U . . . . . C34 C 0.4183(17) 0.2681(14) 0.3791(11) 0.0794 1.0000 Uani . U . . . . . C35 C 0.2610(18) 0.4584(13) 0.2683(11) 0.0801 1.0000 Uani . U . . . . . C36 C 0.3957(19) 0.3370(14) 0.1433(12) 0.0888 1.0000 Uani . U . . . . . C37 C 0.3301(16) 0.3207(13) 0.3396(10) 0.0630 1.0000 Uani . U . . . . . C38 C 0.4337(18) 0.4343(14) 0.3083(11) 0.0871 1.0000 Uani . U . . . . . C39 C 0.3134(18) 0.2989(14) 0.1537(12) 0.0895 1.0000 Uani . U . . . . . C40 C 0.2572(19) 0.4132(16) 0.0797(11) 0.0984 1.0000 Uani . U . . . . . C41 C -0.0452(15) 0.2267(13) 0.6655(11) 0.0793 1.0000 Uani . U . . . . . C42 C -0.0503(14) 0.0852(14) 0.6300(10) 0.0680 1.0000 Uani . U . . . . . H31 H 0.4066 0.1492 1.1056 0.0870 1.0000 Uiso R . . . . . . H32 H 0.3778 0.1957 1.0257 0.0870 1.0000 Uiso R . . . . . . H41 H 0.5024 0.0527 1.0712 0.1059 1.0000 Uiso R . . . . . . H42 H 0.4625 0.0877 0.9853 0.1059 1.0000 Uiso R . . . . . . H61 H 0.7160 0.1719 1.1059 0.0901 1.0000 Uiso R . . . . . . H62 H 0.6767 0.0807 1.1115 0.0899 1.0000 Uiso R . . . . . . H72 H 0.7573 0.0781 1.0242 0.1030 1.0000 Uiso R . . . . . . H71 H 0.6367 0.0664 0.9763 0.1030 1.0000 Uiso R . . . . . . H102 H 0.2301 0.1428 1.0831 0.0979 1.0000 Uiso R . . . . . . H101 H 0.2102 0.1884 1.0030 0.0980 1.0000 Uiso R . . . . . . H111 H 0.0639 0.1124 1.0036 0.1010 1.0000 Uiso R . . . . . . H112 H 0.1300 0.0312 1.0083 0.1010 1.0000 Uiso R . . . . . . H132 H -0.0645 0.0717 0.8773 0.1059 1.0000 Uiso R . . . . . . H131 H -0.0031 -0.0133 0.8880 0.1060 1.0000 Uiso R . . . . . . H142 H -0.0883 0.0125 0.7560 0.0979 1.0000 Uiso R . . . . . . H141 H 0.0333 0.0207 0.7762 0.0980 1.0000 Uiso R . . . . . . H201 H -0.1051 0.2458 0.3306 0.0911 1.0000 Uiso R . . . . . . H202 H -0.0808 0.1608 0.2979 0.0910 1.0000 Uiso R . . . . . . H211 H -0.1301 0.1276 0.3982 0.0960 1.0000 Uiso R . . . . . . H212 H -0.0077 0.1168 0.4293 0.0960 1.0000 Uiso R . . . . . . H251 H 0.7411 0.0650 0.6498 0.1000 1.0000 Uiso R . . . . . . H252 H 0.6183 0.0657 0.6226 0.1000 1.0000 Uiso R . . . . . . H261 H 0.7315 0.1570 0.5497 0.0969 1.0000 Uiso R . . . . . . H262 H 0.6736 0.0727 0.5176 0.0970 1.0000 Uiso R . . . . . . H11 H 0.7183 0.0501 0.8898 0.0890 1.0000 Uiso R . . . . . . H21 H 0.4099 0.4465 0.0838 0.1159 1.0000 Uiso R . . . . . . H51 H -0.0545 0.3048 0.5763 0.0930 1.0000 Uiso R . . . . . . H81 H 0.6615 0.2892 0.7448 0.0861 1.0000 Uiso R . . . . . . H121 H 0.2666 0.5678 0.2121 0.1010 1.0000 Uiso R . . . . . . H151 H 0.4613 0.5471 0.2543 0.1020 1.0000 Uiso R . . . . . . H191 H 0.7149 0.0425 0.7626 0.0909 1.0000 Uiso R . . . . . . H221 H 0.3024 0.1081 0.4118 0.0910 1.0000 Uiso R . . . . . . H291 H -0.0616 0.0636 0.5221 0.0939 1.0000 Uiso R . . . . . . H311 H 0.1506 0.3313 0.1073 0.1191 1.0000 Uiso R . . . . . . H321 H 0.6653 0.2929 0.8687 0.0890 1.0000 Uiso R . . . . . . H341 H 0.4847 0.2867 0.3861 0.0860 1.0000 Uiso R . . . . . . H351 H 0.1873 0.4523 0.2612 0.0970 1.0000 Uiso R . . . . . . H361 H 0.4679 0.3188 0.1660 0.1091 1.0000 Uiso R . . . . . . H381 H 0.5028 0.4094 0.3297 0.0981 1.0000 Uiso R . . . . . . H391 H 0.3162 0.2475 0.1820 0.1080 1.0000 Uiso R . . . . . . H401 H 0.2119 0.4565 0.0487 0.1230 1.0000 Uiso R . . . . . . H411 H -0.0407 0.2664 0.7028 0.0960 1.0000 Uiso R . . . . . . H421 H -0.0501 0.0299 0.6440 0.0880 1.0000 Uiso R . . . . . . H241 H 0.1745 0.3208 0.3133 0.0910 1.0000 Uiso R . . . . . . H192 H 0.0586 0.2782 0.3680 0.0920 1.0000 Uiso R . . . . . . H271 H 0.5691 0.2164 0.5184 0.0949 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 0.089(2) 0.081(2) 0.0602(19) -0.0028(17) 0.0271(16) -0.008(2) O2 0.079(8) 0.077(10) 0.086(9) 0.019(8) 0.029(8) -0.008(7) C3 0.088(10) 0.088(15) 0.088(13) 0.018(12) 0.044(12) -0.021(9) C4 0.083(9) 0.106(15) 0.075(13) 0.018(12) 0.035(11) -0.016(8) O5 0.085(8) 0.085(10) 0.082(9) -0.003(8) 0.047(9) -0.008(7) C6 0.083(8) 0.085(14) 0.083(12) -0.025(9) 0.043(11) -0.013(9) C7 0.105(13) 0.090(13) 0.073(11) -0.003(9) 0.044(11) 0.014(13) O8 0.104(10) 0.089(10) 0.077(9) -0.005(7) 0.034(9) -0.001(9) C9 0.075(12) 0.085(9) 0.080(10) -0.002(7) 0.032(11) -0.007(12) C10 0.076(9) 0.096(15) 0.061(10) 0.011(10) 0.017(10) -0.005(9) C11 0.084(8) 0.111(14) 0.060(7) -0.005(11) 0.040(10) -0.020(10) O12 0.093(9) 0.089(10) 0.056(6) -0.002(8) 0.025(7) -0.012(8) C13 0.084(12) 0.108(15) 0.063(8) 0.019(9) 0.021(10) -0.014(10) C14 0.088(13) 0.079(9) 0.055(7) 0.017(9) 0.005(9) 0.016(12) O15 0.104(10) 0.072(8) 0.060(7) 0.008(7) 0.027(8) 0.014(8) C16 0.082(12) 0.078(8) 0.053(9) 0.009(7) 0.013(11) 0.011(13) O17 0.117(11) 0.088(9) 0.077(10) -0.020(10) 0.045(9) -0.017(8) C18 0.081(8) 0.087(9) 0.053(11) -0.016(12) 0.027(10) -0.013(7) N19 0.076(9) 0.089(11) 0.052(9) -0.013(9) 0.030(9) -0.017(8) C20 0.073(8) 0.094(15) 0.057(10) 0.018(8) 0.020(11) -0.014(9) C21 0.084(12) 0.094(14) 0.054(10) 0.016(7) 0.021(11) -0.016(12) O22 0.079(9) 0.096(10) 0.061(8) 0.015(6) 0.027(8) -0.006(8) C23 0.054(10) 0.085(9) 0.059(9) 0.016(7) 0.021(10) 0.007(12) O24 0.073(9) 0.085(9) 0.079(8) 0.001(7) 0.020(8) -0.005(8) C25 0.071(12) 0.077(11) 0.073(9) 0.007(7) 0.017(10) -0.011(12) C26 0.085(11) 0.087(15) 0.083(9) 0.014(8) 0.039(9) 0.018(9) N27 0.086(10) 0.070(11) 0.062(10) -0.001(7) 0.030(7) 0.012(8) C28 0.092(9) 0.082(9) 0.100(14) -0.027(8) 0.023(8) 0.011(9) O29 0.115(13) 0.096(12) 0.209(18) -0.067(12) 0.009(12) 0.015(10) C30 0.055(11) 0.083(9) 0.088(9) 0.000(7) 0.030(11) -0.012(12) C1 0.066(12) 0.091(10) 0.086(10) 0.003(9) 0.036(12) 0.009(13) C2 0.129(11) 0.092(11) 0.071(7) -0.005(7) 0.048(7) -0.004(10) C5 0.071(12) 0.087(10) 0.061(10) 0.011(7) 0.018(12) 0.006(12) C8 0.079(13) 0.077(9) 0.083(10) 0.000(9) 0.028(12) -0.017(12) C12 0.107(10) 0.085(5) 0.063(9) -0.008(4) 0.034(8) -0.011(6) C15 0.104(9) 0.091(7) 0.068(8) -0.009(5) 0.033(8) -0.021(7) C17 0.079(7) 0.097(10) 0.038(11) -0.004(9) 0.029(10) -0.005(7) C19 0.082(13) 0.079(9) 0.080(10) -0.006(8) 0.030(12) -0.013(12) C22 0.085(8) 0.104(12) 0.038(11) 0.002(10) 0.026(12) -0.001(8) C24 0.077(8) 0.089(11) 0.048(11) -0.013(10) 0.025(10) -0.009(8) C27 0.083(7) 0.093(10) 0.034(10) -0.011(9) 0.036(9) 0.008(8) C29 0.076(12) 0.086(8) 0.063(9) 0.012(8) 0.033(11) -0.001(12) C31 0.100(8) 0.111(11) 0.074(8) -0.030(7) 0.028(6) -0.009(7) C32 0.078(13) 0.083(9) 0.090(11) -0.001(8) 0.037(13) -0.013(12) C33 0.089(8) 0.094(8) 0.058(4) -0.003(5) 0.023(6) -0.014(6) C34 0.082(9) 0.093(11) 0.075(13) -0.007(10) 0.042(10) 0.006(8) C35 0.095(8) 0.084(9) 0.060(8) -0.010(6) 0.028(6) -0.011(6) C36 0.103(9) 0.088(9) 0.082(9) -0.006(7) 0.042(8) -0.004(7) C37 0.080(8) 0.075(8) 0.048(8) -0.022(6) 0.040(10) -0.001(6) C38 0.091(7) 0.101(10) 0.064(5) -0.002(6) 0.023(4) -0.019(6) C39 0.108(12) 0.086(5) 0.082(9) -0.012(5) 0.043(9) -0.010(6) C40 0.126(10) 0.105(10) 0.059(2) -0.012(5) 0.028(5) 0.012(9) C41 0.093(13) 0.079(8) 0.058(9) 0.006(8) 0.018(11) -0.005(13) C42 0.070(12) 0.078(9) 0.055(9) 0.003(7) 0.021(11) -0.018(12) _refine_ls_extinction_method None _oxford_refine_ls_scale 2.10(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 Fe1 . C2 . 2.04(2) yes Fe1 . C12 . 2.01(2) yes Fe1 . C15 . 2.06(2) yes Fe1 . C31 . 2.06(2) yes Fe1 . C33 . 2.018(19) yes Fe1 . C35 . 2.04(2) yes Fe1 . C36 . 2.01(2) yes Fe1 . C38 . 2.088(19) yes Fe1 . C39 . 2.00(2) yes Fe1 . C40 . 2.01(2) yes O2 . C3 . 1.37(2) yes O2 . C10 . 1.39(2) yes C3 . C4 . 1.50(2) yes C3 . H31 . 0.966 no C3 . H32 . 0.965 no C4 . O5 . 1.45(2) yes C4 . H41 . 0.973 no C4 . H42 . 0.969 no O5 . C6 . 1.41(2) yes C6 . C7 . 1.50(2) yes C6 . H61 . 0.974 no C6 . H62 . 0.969 no C7 . O8 . 1.43(2) yes C7 . H72 . 0.976 no C7 . H71 . 0.969 no O8 . C9 . 1.41(2) yes C9 . C1 . 1.35(3) yes C9 . C32 . 1.40(3) yes C10 . C11 . 1.50(2) yes C10 . H102 . 0.973 no C10 . H101 . 0.976 no C11 . O12 . 1.445(19) yes C11 . H111 . 0.969 no C11 . H112 . 0.970 no O12 . C13 . 1.44(2) yes C13 . C14 . 1.50(2) yes C13 . H132 . 0.972 no C13 . H131 . 0.966 no C14 . O15 . 1.41(2) yes C14 . H142 . 0.972 no C14 . H141 . 0.974 no O15 . C16 . 1.40(2) yes C16 . C41 . 1.36(3) yes C16 . C42 . 1.35(2) yes O17 . C18 . 1.26(2) yes C18 . N19 . 1.31(2) yes C18 . C17 . 1.47(3) yes N19 . C20 . 1.43(2) yes N19 . H192 . 0.859 no C20 . C21 . 1.49(2) yes C20 . H201 . 0.971 no C20 . H202 . 0.972 no C21 . O22 . 1.42(2) yes C21 . H211 . 0.969 no C21 . H212 . 0.970 no O22 . C23 . 1.38(2) yes C23 . C5 . 1.39(2) yes C23 . C29 . 1.41(3) yes O24 . C25 . 1.46(2) yes O24 . C30 . 1.40(2) yes C25 . C26 . 1.49(2) yes C25 . H251 . 0.971 no C25 . H252 . 0.971 no C26 . N27 . 1.48(2) yes C26 . H261 . 0.965 no C26 . H262 . 0.969 no N27 . C28 . 1.33(2) yes N27 . H271 . 0.861 no C28 . O29 . 1.20(2) yes C28 . C27 . 1.48(3) yes C30 . C8 . 1.38(3) yes C30 . C19 . 1.42(3) yes C1 . C19 . 1.40(2) yes C1 . H11 . 0.932 no C2 . C36 . 1.38(3) yes C2 . C40 . 1.42(3) yes C2 . H21 . 0.983 no C5 . C41 . 1.41(2) yes C5 . H51 . 0.934 no C8 . C32 . 1.35(2) yes C8 . H81 . 0.929 no C12 . C15 . 1.37(3) yes C12 . C35 . 1.37(2) yes C12 . H121 . 0.979 no C15 . C38 . 1.45(3) yes C15 . H151 . 0.977 no C17 . C22 . 1.38(3) yes C17 . C24 . 1.39(2) yes C19 . H191 . 0.927 no C22 . C27 . 1.35(2) yes C22 . H221 . 0.932 no C24 . C37 . 1.42(2) yes C24 . H241 . 0.932 no C27 . C34 . 1.41(3) yes C29 . C42 . 1.34(2) yes C29 . H291 . 0.931 no C31 . C39 . 1.43(3) yes C31 . C40 . 1.43(3) yes C31 . H311 . 0.980 no C32 . H321 . 0.930 no C33 . C35 . 1.43(3) yes C33 . C37 . 1.48(3) yes C33 . C38 . 1.36(2) yes C34 . C37 . 1.45(3) yes C34 . H341 . 0.929 no C35 . H351 . 0.984 no C36 . C39 . 1.37(3) yes C36 . H361 . 0.975 no C38 . H381 . 0.977 no C39 . H391 . 0.977 no C40 . H401 . 0.974 no C41 . H411 . 0.930 no C42 . H421 . 0.932 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 C2 . Fe1 . C12 . 123.9(9) yes C2 . Fe1 . C15 . 108.4(9) yes C12 . Fe1 . C15 . 39.4(7) yes C2 . Fe1 . C31 . 69.3(9) yes C12 . Fe1 . C31 . 128.3(10) yes C15 . Fe1 . C31 . 164.6(10) yes C2 . Fe1 . C33 . 159.1(10) yes C12 . Fe1 . C33 . 67.2(9) yes C15 . Fe1 . C33 . 67.9(9) yes C31 . Fe1 . C33 . 119.8(9) yes C2 . Fe1 . C35 . 158.2(9) yes C12 . Fe1 . C35 . 39.4(7) yes C15 . Fe1 . C35 . 67.4(8) yes C31 . Fe1 . C35 . 108.7(9) yes C33 . Fe1 . C35 . 41.3(7) yes C2 . Fe1 . C36 . 39.7(8) yes C12 . Fe1 . C36 . 156.8(9) yes C15 . Fe1 . C36 . 121.1(9) yes C31 . Fe1 . C36 . 67.6(9) yes C33 . Fe1 . C36 . 123.1(10) yes C2 . Fe1 . C38 . 125.5(9) yes C12 . Fe1 . C38 . 66.1(9) yes C15 . Fe1 . C38 . 40.9(7) yes C31 . Fe1 . C38 . 152.8(9) yes C33 . Fe1 . C38 . 38.5(7) yes C2 . Fe1 . C39 . 68.6(9) yes C12 . Fe1 . C39 . 163.2(9) yes C15 . Fe1 . C39 . 153.5(10) yes C31 . Fe1 . C39 . 41.1(8) yes C33 . Fe1 . C39 . 105.0(10) yes C2 . Fe1 . C40 . 41.0(8) yes C12 . Fe1 . C40 . 112.2(10) yes C15 . Fe1 . C40 . 127.4(10) yes C31 . Fe1 . C40 . 41.1(8) yes C33 . Fe1 . C40 . 157.1(10) yes C35 . Fe1 . C36 . 161.2(9) yes C35 . Fe1 . C38 . 66.4(8) yes C36 . Fe1 . C38 . 107.9(9) yes C35 . Fe1 . C39 . 125.1(9) yes C36 . Fe1 . C39 . 39.9(8) yes C38 . Fe1 . C39 . 117.9(9) yes C35 . Fe1 . C40 . 123.2(9) yes C36 . Fe1 . C40 . 67.0(9) yes C38 . Fe1 . C40 . 164.1(10) yes C39 . Fe1 . C40 . 68.7(10) yes C3 . O2 . C10 . 109.4(17) yes O2 . C3 . C4 . 111.0(19) yes O2 . C3 . H31 . 110.0 no C4 . C3 . H31 . 108.0 no O2 . C3 . H32 . 109.3 no C4 . C3 . H32 . 108.9 no H31 . C3 . H32 . 109.6 no C3 . C4 . O5 . 108.0(18) yes C3 . C4 . H41 . 110.6 no O5 . C4 . H41 . 109.6 no C3 . C4 . H42 . 109.3 no O5 . C4 . H42 . 109.8 no H41 . C4 . H42 . 109.7 no C4 . O5 . C6 . 116.6(16) yes O5 . C6 . C7 . 114.2(17) yes O5 . C6 . H61 . 106.9 no C7 . C6 . H61 . 108.5 no O5 . C6 . H62 . 109.2 no C7 . C6 . H62 . 108.3 no H61 . C6 . H62 . 109.7 no C6 . C7 . O8 . 107.2(17) yes C6 . C7 . H72 . 109.5 no O8 . C7 . H72 . 110.1 no C6 . C7 . H71 . 110.7 no O8 . C7 . H71 . 109.9 no H72 . C7 . H71 . 109.3 no C7 . O8 . C9 . 117.8(17) yes O8 . C9 . C1 . 124(2) yes O8 . C9 . C32 . 116(2) yes C1 . C9 . C32 . 120(2) yes O2 . C10 . C11 . 111.2(18) yes O2 . C10 . H102 . 111.1 no C11 . C10 . H102 . 109.8 no O2 . C10 . H101 . 107.8 no C11 . C10 . H101 . 107.3 no H102 . C10 . H101 . 109.5 no C10 . C11 . O12 . 112.0(15) yes C10 . C11 . H111 . 109.5 no O12 . C11 . H111 . 110.0 no C10 . C11 . H112 . 108.0 no O12 . C11 . H112 . 107.8 no H111 . C11 . H112 . 109.6 no C11 . O12 . C13 . 112.5(14) yes O12 . C13 . C14 . 105.8(16) yes O12 . C13 . H132 . 109.8 no C14 . C13 . H132 . 108.8 no O12 . C13 . H131 . 110.5 no C14 . C13 . H131 . 111.7 no H132 . C13 . H131 . 110.1 no C13 . C14 . O15 . 110.1(17) yes C13 . C14 . H142 . 109.3 no O15 . C14 . H142 . 109.4 no C13 . C14 . H141 . 109.0 no O15 . C14 . H141 . 109.5 no H142 . C14 . H141 . 109.5 no C14 . O15 . C16 . 120.0(16) yes O15 . C16 . C41 . 115(2) yes O15 . C16 . C42 . 122(2) yes C41 . C16 . C42 . 123(2) yes O17 . C18 . N19 . 118(2) yes O17 . C18 . C17 . 118(2) yes N19 . C18 . C17 . 124(2) yes C18 . N19 . C20 . 122.9(20) yes C18 . N19 . H192 . 118.4 no C20 . N19 . H192 . 118.7 no N19 . C20 . C21 . 111.2(15) yes N19 . C20 . H201 . 108.5 no C21 . C20 . H201 . 107.6 no N19 . C20 . H202 . 109.9 no C21 . C20 . H202 . 109.8 no H201 . C20 . H202 . 109.7 no C20 . C21 . O22 . 107.2(17) yes C20 . C21 . H211 . 110.2 no O22 . C21 . H211 . 110.7 no C20 . C21 . H212 . 107.8 no O22 . C21 . H212 . 111.3 no H211 . C21 . H212 . 109.6 no C21 . O22 . C23 . 114.1(16) yes O22 . C23 . C5 . 113.9(19) yes O22 . C23 . C29 . 127.5(20) yes C5 . C23 . C29 . 118.4(20) yes C25 . O24 . C30 . 116.2(16) yes O24 . C25 . C26 . 105.4(16) yes O24 . C25 . H251 . 109.3 no C26 . C25 . H251 . 110.1 no O24 . C25 . H252 . 111.1 no C26 . C25 . H252 . 111.6 no H251 . C25 . H252 . 109.2 no C25 . C26 . N27 . 112.3(16) yes C25 . C26 . H261 . 109.7 no N27 . C26 . H261 . 110.0 no C25 . C26 . H262 . 106.9 no N27 . C26 . H262 . 108.1 no H261 . C26 . H262 . 109.7 no C26 . N27 . C28 . 122.9(19) yes C26 . N27 . H271 . 116.5 no C28 . N27 . H271 . 120.6 no N27 . C28 . O29 . 123(3) yes N27 . C28 . C27 . 115(2) yes O29 . C28 . C27 . 121(2) yes O24 . C30 . C8 . 113(2) yes O24 . C30 . C19 . 124(2) yes C8 . C30 . C19 . 123(2) yes C9 . C1 . C19 . 123(2) yes C9 . C1 . H11 . 119.2 no C19 . C1 . H11 . 118.0 no Fe1 . C2 . C36 . 68.7(12) yes Fe1 . C2 . C40 . 68.3(12) yes C36 . C2 . C40 . 105(2) yes Fe1 . C2 . H21 . 127.0 no C36 . C2 . H21 . 128.7 no C40 . C2 . H21 . 126.4 no C23 . C5 . C41 . 120(2) yes C23 . C5 . H51 . 120.1 no C41 . C5 . H51 . 120.2 no C30 . C8 . C32 . 120(2) yes C30 . C8 . H81 . 120.4 no C32 . C8 . H81 . 120.0 no Fe1 . C12 . C15 . 72.2(13) yes Fe1 . C12 . C35 . 71.2(13) yes C15 . C12 . C35 . 112(2) yes Fe1 . C12 . H121 . 123.6 no C15 . C12 . H121 . 124.7 no C35 . C12 . H121 . 123.3 no Fe1 . C15 . C12 . 68.4(13) yes Fe1 . C15 . C38 . 70.6(12) yes C12 . C15 . C38 . 105(2) yes Fe1 . C15 . H151 . 128.2 no C12 . C15 . H151 . 128.1 no C38 . C15 . H151 . 127.1 no C18 . C17 . C22 . 123(2) yes C18 . C17 . C24 . 119(2) yes C22 . C17 . C24 . 119(2) yes C30 . C19 . C1 . 115(2) yes C30 . C19 . H191 . 121.2 no C1 . C19 . H191 . 123.7 no C17 . C22 . C27 . 123(2) yes C17 . C22 . H221 . 117.4 no C27 . C22 . H221 . 119.5 no C17 . C24 . C37 . 123(2) yes C17 . C24 . H241 . 120.1 no C37 . C24 . H241 . 117.0 no C28 . C27 . C22 . 120(2) yes C28 . C27 . C34 . 122(2) yes C22 . C27 . C34 . 118(2) yes C23 . C29 . C42 . 120(2) yes C23 . C29 . H291 . 119.2 no C42 . C29 . H291 . 120.4 no Fe1 . C31 . C39 . 67.4(12) yes Fe1 . C31 . C40 . 67.7(12) yes C39 . C31 . C40 . 105(2) yes Fe1 . C31 . H311 . 126.3 no C39 . C31 . H311 . 126.4 no C40 . C31 . H311 . 128.6 no C9 . C32 . C8 . 120(2) yes C9 . C32 . H321 . 119.6 no C8 . C32 . H321 . 120.3 no Fe1 . C33 . C35 . 70.0(12) yes Fe1 . C33 . C37 . 121.9(14) yes C35 . C33 . C37 . 126(2) yes Fe1 . C33 . C38 . 73.6(12) yes C35 . C33 . C38 . 108(2) yes C37 . C33 . C38 . 126(2) yes C27 . C34 . C37 . 123(2) yes C27 . C34 . H341 . 118.3 no C37 . C34 . H341 . 119.0 no C33 . C35 . Fe1 . 68.7(12) yes C33 . C35 . C12 . 106(2) yes Fe1 . C35 . C12 . 69.4(12) yes C33 . C35 . H351 . 126.4 no Fe1 . C35 . H351 . 125.8 no C12 . C35 . H351 . 127.6 no C2 . C36 . Fe1 . 71.5(13) yes C2 . C36 . C39 . 112(2) yes Fe1 . C36 . C39 . 69.9(13) yes C2 . C36 . H361 . 122.6 no Fe1 . C36 . H361 . 124.1 no C39 . C36 . H361 . 125.0 no C33 . C37 . C34 . 121.5(20) yes C33 . C37 . C24 . 124(2) yes C34 . C37 . C24 . 114.1(20) yes C15 . C38 . Fe1 . 68.5(11) yes C15 . C38 . C33 . 109(2) yes Fe1 . C38 . C33 . 67.9(12) yes C15 . C38 . H381 . 123.6 no Fe1 . C38 . H381 . 124.0 no C33 . C38 . H381 . 127.4 no C31 . C39 . C36 . 108(2) yes C31 . C39 . Fe1 . 71.5(13) yes C36 . C39 . Fe1 . 70.1(13) yes C31 . C39 . H391 . 125.9 no C36 . C39 . H391 . 126.1 no Fe1 . C39 . H391 . 127.4 no C31 . C40 . C2 . 110(2) yes C31 . C40 . Fe1 . 71.2(12) yes C2 . C40 . Fe1 . 70.7(12) yes C31 . C40 . H401 . 124.0 no C2 . C40 . H401 . 126.1 no Fe1 . C40 . H401 . 125.6 no C5 . C41 . C16 . 118(2) yes C5 . C41 . H411 . 121.4 no C16 . C41 . H411 . 120.7 no C16 . C42 . C29 . 121(2) yes C16 . C42 . H421 . 119.6 no C29 . C42 . H421 . 119.9 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 C14 . H142 . O17 2_556 126 0.97 2.53 3.20(3) yes C25 . H252 . O29 2_656 150 0.97 2.58 3.46(3) yes C2 . H21 . O29 3_655 161 0.98 2.30 3.25(3) yes C42 . H421 . O17 2_556 164 0.93 2.31 3.22(3) yes N19 . H192 . O12 4_554 175 0.86 2.30 3.16(3) yes N27 . H271 . O5 4_554 176 0.86 2.15 3.01(3) yes # Attachment '- 2 2Catenane 3Cl 051NLK10.cif' data_051NLK10 _database_code_depnum_ccdc_archive 'CCDC 853869' #TrackingRef '- 2 2Catenane 3Cl 051NLK10.cif' _audit_creation_date 10-08-12 _audit_creation_method CRYSTALS_ver_14.07 _audit_update_record ; 2010-08-22 - Report on 051NLK10 by Nathan L. Kilah for Paul D. Beer and Nicholas H. Evans 2010-08-22 - Passes Checkcif with minor warnings. ; # start Validation Reply Form _vrf_REFNR01_051NLK10 ; PROBLEM: Ratio of reflections to parameters is < 6 for a RESPONSE: The crystal diffracted very weakly and suffered from severe radiation damage. Copious restraints were used to control the refinement. See the _publ_section_comment section for more information. ; _vrf_RINTA01_051NLK10 ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: The crystal diffracted very weakly and suffered from severe radiation damage. Copious restraints were used to control the refinement. See the _publ_section_comment section for more information. ; _vrf_PLAT020_051NLK10 ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.27 RESPONSE: The crystal diffracted very weakly and suffered from severe radiation damage. Copious restraints were used to control the refinement. See the _publ_section_comment section for more information. ; _vrf_PLAT026_051NLK10 ; PROBLEM: Ratio Observed / Unique Reflections too Low .... 18 Perc. RESPONSE: The crystal diffracted very weakly and suffered from severe radiation damage. Copious restraints were used to control the refinement. See the _publ_section_comment section for more information. ; # end Validation Reply Form _oxford_structure_analysis_title '051NLK10 in P-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). ; The crystal structure of a catenane containing a ferrocene-based macrocycle and a pyridinium-based macrocycle. ; _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. ; The asymmetric unit contains a ferrocene-based macrocycle interlocked with a pyridinium-based macrocycle, arranged around a chloride anion. The crystals were small and poorly diffracting. Data were therefore collected on I19 (EH1) at Diamond Light Source. Unfortunately, several attempts demonstrated that the crystals suffered severe radiation damage, resulting in a shortage of data. Copious restraints were necessary to try to ensure that the refinement remained stable and maintained sensible geometric parameters. The parameters for the restraints were obtained from a Mogul analysis of a preliminary refinement. Thermal and vibrational restraints were also used within CRYSTALS to try to ensure the displacement parameters were sensible. Hydrogen atoms were included geometrically, and ride to the atoms to which they are bound. Residual electron density indicated solvent inclusion, however the poor quality data made modelling the solvent extremely problematic. The structure was processed with SQUEEZE in PLATON, indicating a void of 308 \%A^3^ containing 130 electrons per cell. Despite the poor availabilty of quality data and the need for numerous restraints, the interlocked structure is unambiguously identified. ; _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_prep # Brief details or a reference. Include solvent if known ; Crystals were grown from evaporation of a acetonitrile/chloroform solution ; _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 ; ? ; # 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 0.000 0.000 0.500 259 117 ' ' 2 0.503 0.314 0.666 9 3 ' ' 3 0.496 0.686 0.334 9 2 ' ' _platon_squeeze_details ; Refer to _publ_section_comment ; # End of 'script/refcif.dat' #end of refcif _cell_length_a 11.106(3) _cell_length_b 17.783(4) _cell_length_c 19.841(5) _cell_angle_alpha 95.61(4) _cell_angle_beta 100.94(3) _cell_angle_gamma 106.08(3) _cell_volume 3649.4(18) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 '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 2 # Given Formula = C57 Cl3 Fe3 N5 O11 # Dc = 1.10 Fooo = 1484.00 Mu = 7.46 M = 1204.55 # Found Formula = C74 H84 Cl1 Fe1 N5 O17 # Dc = 1.28 FOOO = 1484.00 Mu = 3.14 M = 1406.80 _chemical_formula_sum 'C74 H84 Cl1 Fe1 N5 O17' _chemical_formula_moiety 'C42 H46 Fe1 N2 O9, C32 H38 N3 O8, Cl1' _chemical_compound_source ? _chemical_formula_weight 1406.80 _cell_measurement_reflns_used 4021 _cell_measurement_theta_min 1 _cell_measurement_theta_max 19.5 _cell_measurement_temperature 100 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.006 _exptl_crystal_size_mid 0.012 _exptl_crystal_size_max 0.090 _exptl_crystal_density_diffrn 1.280 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1484 _exptl_absorpt_coefficient_mu 0.314 # Sheldrick geometric approximatio 1.00 1.00 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_process_details ; CrystalClear (Rigaku, 1997--2002) ; _exptl_absorpt_correction_T_min 0.261 _exptl_absorpt_correction_T_max 1.000 _diffrn_measurement_device_type Serial _diffrn_measurement_device ; Crystal-Logic kappa goniometer and Rigaku Saturn 724+ CCD detector ; _diffrn_radiation_monochromator 'Si(1 1 1) double-crystal monochromator' _diffrn_source Synchrotron _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.68890 _diffrn_measurement_method \w/2\q # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection ; CrystalClear (Rigaku, 1997--2002) ; _computing_cell_refinement ; CrystalClear (Rigaku, 1997--2002) ; _computing_data_reduction ; CrystalClear (Rigaku, 1997--2002) ; _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 100 _diffrn_reflns_number 14965 _reflns_number_total 13022 _diffrn_reflns_av_R_equivalents 0.274 # Number of reflections without Friedels Law is 14965 # Number of reflections with Friedels Law is 13022 # Theoretical number of reflections is about 5111 _diffrn_reflns_theta_min 1.059 _diffrn_reflns_theta_max 28.532 _diffrn_measured_fraction_theta_max 0.807 _diffrn_reflns_theta_full 25.108 _diffrn_measured_fraction_theta_full 0.967 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _reflns_limit_h_min -15 _reflns_limit_h_max 15 _reflns_limit_k_min -24 _reflns_limit_k_max 24 _reflns_limit_l_min -27 _reflns_limit_l_max 27 _oxford_diffrn_Wilson_B_factor 7.25 _oxford_diffrn_Wilson_scale 37.21 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.63 _refine_diff_density_max 0.75 # 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>-3.0\s(I) _refine_ls_number_reflns 5016 _refine_ls_number_restraints 1293 _refine_ls_number_parameters 883 _oxford_refine_ls_R_factor_ref 0.2361 _refine_ls_wR_factor_ref 0.3955 _refine_ls_goodness_of_fit_ref 0.8743 _refine_ls_shift/su_max 0.0017630 _refine_ls_shift/su_mean 0.0000291 # The values computed from all data _oxford_reflns_number_all 5016 _refine_ls_R_factor_all 0.2361 _refine_ls_wR_factor_all 0.3955 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2297 _refine_ls_R_factor_gt 0.1631 _refine_ls_wR_factor_gt 0.2994 # 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: 47.7 63.7 19.2 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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. CrystalClear: An Integrated Program for the Collection and Processing of Area Detector Data, Rigaku Corporation, 1997--2002. 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. SQUEEZE A. Spek, J. Appl. Crystallogr. 2003, 36, 7-13; P. van der Sluis & A. L. Spek, Acta Cryst. (1990). A46, 194-201. ; # 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 Cl1 Cl -0.0760(5) 0.2563(3) -0.0405(3) 0.1217 1.0000 Uani . . . . . . . Fe2 Fe 0.2102(5) 0.4892(2) 0.43105(19) 0.1746 1.0000 Uani D U . . . . . C3 C 0.278(2) 0.6027(6) 0.4839(10) 0.1923 1.0000 Uani D U . . . . . C4 C 0.3820(18) 0.5729(8) 0.4755(12) 0.1961 1.0000 Uani D U . . . . . C5 C 0.3715(19) 0.5539(7) 0.4060(13) 0.1895 1.0000 Uani D U . . . . . C6 C 0.264(2) 0.5708(8) 0.3697(9) 0.1860 1.0000 Uani D U . . . . . C7 C 0.2054(16) 0.6010(6) 0.4177(13) 0.1848 1.0000 Uani D U . . . . . C8 C 0.0279(12) 0.4162(6) 0.4116(8) 0.1661 1.0000 Uani D U . . . . . C9 C 0.0907(18) 0.4253(6) 0.4832(8) 0.1743 1.0000 Uani D U . . . . . C10 C 0.2012(17) 0.3993(6) 0.4865(8) 0.1782 1.0000 Uani D U . . . . . C11 C 0.2086(14) 0.3742(5) 0.4174(8) 0.1695 1.0000 Uani D U . . . . . C12 C 0.1017(12) 0.3842(5) 0.3702(6) 0.1654 1.0000 Uani D U . . . . . C13 C 0.0737(11) 0.3648(6) 0.2931(6) 0.1368 1.0000 Uani D U . . . . . C14 C 0.1436(11) 0.3241(6) 0.2610(7) 0.1363 1.0000 Uani D U . . . . . C15 C 0.1135(11) 0.3024(6) 0.1885(7) 0.1151 1.0000 Uani D U . . . . . C16 C 0.0124(12) 0.3223(6) 0.1482(6) 0.0974 1.0000 Uani D U . . . . . C17 C -0.0586(10) 0.3625(6) 0.1795(7) 0.1069 1.0000 Uani D U . . . . . C18 C -0.0274(11) 0.3834(6) 0.2514(7) 0.1242 1.0000 Uani D U . . . . . C19 C 0.1973(18) 0.2614(12) 0.1589(8) 0.1191 1.0000 Uani D U . . . . . O20 O 0.2874(14) 0.2478(11) 0.1978(8) 0.1646 1.0000 Uani D U . . . . . N21 N 0.1693(14) 0.2381(10) 0.0896(8) 0.1205 1.0000 Uani D U . . . . . C22 C 0.2556(18) 0.2064(14) 0.0579(11) 0.1375 1.0000 Uani D U . . . . . C23 C 0.2071(19) 0.1816(13) -0.0195(10) 0.1399 1.0000 Uani D U . . . . . O24 O 0.1016(10) 0.1073(8) -0.0304(7) 0.1297 1.0000 Uani D U . . . . . C25 C 0.0526(12) 0.0665(10) -0.0970(8) 0.1352 1.0000 Uani D U . . . . . C26 C 0.0834(11) 0.1024(9) -0.1527(10) 0.1422 1.0000 Uani D U . . . . . C27 C 0.0337(14) 0.0610(12) -0.2196(9) 0.1565 1.0000 Uani D U . . . . . C28 C -0.0481(14) -0.0163(12) -0.2311(8) 0.1681 1.0000 Uani D U . . . . . C29 C -0.0791(11) -0.0517(9) -0.1747(11) 0.1525 1.0000 Uani D U . . . . . C30 C -0.0288(13) -0.0103(11) -0.1076(9) 0.1355 1.0000 Uani D U . . . . . O31 O -0.0962(14) -0.0546(12) -0.2991(8) 0.1995 1.0000 Uani D U . . . . . H31 H 0.2627 0.6221 0.5258 0.2361 1.0000 Uiso . . . . . . . C32 C -0.087(4) -0.1261(17) -0.3141(14) 0.2339 1.0000 Uani D U . . . . . C33 C -0.120(3) -0.145(2) -0.3937(15) 0.2364 1.0000 Uani D U . . . . . O34 O -0.252(2) -0.1577(16) -0.4141(10) 0.2331 1.0000 Uani D U . . . . . C35 C -0.307(3) -0.197(2) -0.4824(15) 0.2323 1.0000 Uani D U . . . . . C36 C -0.451(3) -0.2190(19) -0.4956(16) 0.2177 1.0000 Uani D U . . . . . O37 O -0.485(2) -0.1487(14) -0.4860(10) 0.2187 1.0000 Uani D U . . . . . C38 C -0.615(3) -0.1670(19) -0.4983(16) 0.2243 1.0000 Uani D U . . . . . C39 C -0.655(3) -0.093(2) -0.4966(13) 0.2238 1.0000 Uani D U . . . . . O40 O -0.619(2) -0.0515(15) -0.4253(10) 0.2268 1.0000 Uani D U . . . . . C41 C -0.694(3) 0.002(2) -0.4176(14) 0.2248 1.0000 Uani D U . . . . . H41 H 0.4471 0.5690 0.5119 0.2383 1.0000 Uiso . . . . . . . C42 C -0.616(3) 0.0717(15) -0.3617(12) 0.1979 1.0000 Uani D U . . . . . O43 O -0.6247(10) 0.0432(8) -0.2978(7) 0.1488 1.0000 Uani D U . . . . . C44 C -0.5705(11) 0.0965(9) -0.2368(7) 0.1045 1.0000 Uani D U . . . . . C45 C -0.4947(12) 0.1739(11) -0.2337(8) 0.1298 1.0000 Uani D U . . . . . C46 C -0.4436(10) 0.2236(8) -0.1695(9) 0.1092 1.0000 Uani D U . . . . . C47 C -0.4680(10) 0.1959(8) -0.1092(7) 0.1081 1.0000 Uani D U . . . . . C48 C -0.5438(11) 0.1190(9) -0.1122(7) 0.0941 1.0000 Uani D U . . . . . C49 C -0.5951(10) 0.0685(8) -0.1756(9) 0.1131 1.0000 Uani D U . . . . . O50 O -0.4201(8) 0.2427(6) -0.0449(6) 0.1044 1.0000 Uani D U . . . . . C51 C -0.358(2) 0.3256(11) -0.0412(10) 0.1255 1.0000 Uani D U . . . . . H51 H 0.4296 0.5330 0.3858 0.2315 1.0000 Uiso . . . . . . . C52 C -0.3269(18) 0.3661(11) 0.0328(10) 0.1142 1.0000 Uani D U . . . . . N53 N -0.2184(14) 0.3479(8) 0.0733(7) 0.1009 1.0000 Uani D U . . . . . C54 C -0.1635(16) 0.3862(10) 0.1380(8) 0.1082 1.0000 Uani D U . . . . . O55 O -0.2090(15) 0.4351(8) 0.1661(7) 0.1305 1.0000 Uani D U . . . . . C56 C -0.4338(11) -0.1155(11) -0.3119(10) 0.1433 1.0000 Uani D U . . . . . N57 N -0.3739(8) -0.0422(7) -0.2610(6) 0.1066 1.0000 Uani D U . . . . . C58 C -0.3181(9) 0.0249(8) -0.2831(6) 0.1158 1.0000 Uani D U . . . . . C59 C -0.2607(9) 0.0943(7) -0.2375(7) 0.1069 1.0000 Uani D U . . . . . C60 C -0.2598(9) 0.0936(7) -0.1679(7) 0.1005 1.0000 Uani D U . . . . . C61 C -0.3182(9) 0.0239(8) -0.1458(6) 0.0972 1.0000 Uani D U . . . . . H61 H 0.2381 0.5631 0.3204 0.2290 1.0000 Uiso . . . . . . . C62 C -0.3741(9) -0.0437(7) -0.1940(7) 0.1000 1.0000 Uani D U . . . . . C63 C -0.205(2) 0.1678(9) -0.2681(9) 0.1380 1.0000 Uani D U . . . . . O64 O -0.2121(19) 0.1626(10) -0.3314(8) 0.1710 1.0000 Uani D U . . . . . N65 N -0.1346(18) 0.2326(10) -0.2232(8) 0.1435 1.0000 Uani D U . . . . . C66 C -0.073(2) 0.3070(13) -0.2456(12) 0.1608 1.0000 Uani D U . . . . . C67 C -0.062(2) 0.3775(13) -0.1946(13) 0.1546 1.0000 Uani D U . . . . . O68 O -0.1861(16) 0.3907(7) -0.2082(7) 0.1573 1.0000 Uani D U . . . . . C69 C -0.2075(19) 0.4432(8) -0.1593(9) 0.1504 1.0000 Uani D U . . . . . C70 C -0.3257(19) 0.4537(9) -0.1742(9) 0.1633 1.0000 Uani D U . . . . . C71 C -0.3586(16) 0.5041(11) -0.1290(12) 0.1722 1.0000 Uani D U . . . . . H71 H 0.1332 0.6184 0.4064 0.2284 1.0000 Uiso . . . . . . . C72 C -0.272(2) 0.5444(8) -0.0685(10) 0.1767 1.0000 Uani D U . . . . . C73 C -0.1527(19) 0.5346(9) -0.0531(8) 0.1640 1.0000 Uani D U . . . . . C74 C -0.1193(15) 0.4843(10) -0.0987(11) 0.1599 1.0000 Uani D U . . . . . O75 O -0.3130(17) 0.5937(9) -0.0251(10) 0.2123 1.0000 Uani D U . . . . . C76 C -0.248(3) 0.6055(19) 0.0481(15) 0.2071 1.0000 Uani D U . . . . . C77 C -0.323(3) 0.638(2) 0.0935(18) 0.2244 1.0000 Uani D U . . . . . O78 O -0.247(2) 0.6749(15) 0.1616(14) 0.2584 1.0000 Uani D U . . . . . C79 C -0.3276(10) 0.6830(12) 0.2101(17) 0.2589 1.0000 Uani D U . . . . . C80 C -0.3038(12) 0.6396(13) 0.2690(13) 0.2744 1.0000 Uani D U . . . . . C81 C -0.2631(12) 0.5775(13) 0.2678(12) 0.2602 1.0000 Uani D U . . . . . H81 H -0.0478 0.4303 0.3941 0.2019 1.0000 Uiso . . . . . . . C82 C -0.2395(14) 0.5355(18) 0.3248(16) 0.2531 1.0000 Uani D U . . . . . O83 O -0.351(3) 0.4953(14) 0.3403(12) 0.2545 1.0000 Uani D U . . . . . C84 C -0.429(3) 0.4321(18) 0.2906(14) 0.2097 1.0000 Uani D U . . . . . C85 C -0.472(3) 0.3615(15) 0.3257(13) 0.1689 1.0000 Uani D U . . . . . O86 O -0.3641(13) 0.3330(7) 0.3420(7) 0.1517 1.0000 Uani D U . . . . . C87 C -0.3417(13) 0.2835(7) 0.2910(8) 0.1310 1.0000 Uani D U . . . . . C88 C -0.2489(13) 0.2498(8) 0.3137(7) 0.1270 1.0000 Uani D U . . . . . C89 C -0.2181(11) 0.1993(8) 0.2687(8) 0.1222 1.0000 Uani D U . . . . . C90 C -0.2816(11) 0.1829(6) 0.1993(7) 0.0941 1.0000 Uani D U . . . . . C91 C -0.3747(12) 0.2173(7) 0.1760(7) 0.0959 1.0000 Uani D U . . . . . H91 H 0.0636 0.4462 0.5221 0.2089 1.0000 Uiso . . . . . . . C92 C -0.4049(11) 0.2680(7) 0.2224(9) 0.1153 1.0000 Uani D U . . . . . O93 O -0.2437(10) 0.1314(6) 0.1564(7) 0.1145 1.0000 Uani D U . . . . . C94 C -0.2917(18) 0.1225(12) 0.0826(9) 0.1099 1.0000 Uani D U . . . . . C95 C -0.2164(18) 0.0786(10) 0.0487(9) 0.1047 1.0000 Uani D U . . . . . N96 N -0.2374(13) 0.0771(8) -0.0251(7) 0.1000 1.0000 Uani D U . . . . . C97 C -0.3137(15) 0.0150(9) -0.0719(6) 0.0895 1.0000 Uani D U . . . . . O98 O -0.3791(12) -0.0474(7) -0.0565(6) 0.1032 1.0000 Uani D U . . . . . H101 H 0.2626 0.4000 0.5276 0.2094 1.0000 Uiso . . . . . . . H111 H 0.2748 0.3557 0.4044 0.2003 1.0000 Uiso . . . . . . . H141 H 0.2114 0.3101 0.2884 0.1736 1.0000 Uiso . . . . . . . H161 H -0.0091 0.3068 0.0993 0.1174 1.0000 Uiso . . . . . . . H181 H -0.0755 0.4115 0.2726 0.1511 1.0000 Uiso . . . . . . . H211 H 0.0993 0.2401 0.0644 0.1357 1.0000 Uiso . . . . . . . H221 H 0.2641 0.1600 0.0796 0.1659 1.0000 Uiso . . . . . . . H222 H 0.3369 0.2442 0.0685 0.1659 1.0000 Uiso . . . . . . . H231 H 0.2754 0.1707 -0.0385 0.1720 1.0000 Uiso . . . . . . . H232 H 0.1798 0.2199 -0.0391 0.1720 1.0000 Uiso . . . . . . . H261 H 0.1377 0.1552 -0.1449 0.1738 1.0000 Uiso . . . . . . . H271 H 0.0543 0.0856 -0.2577 0.1905 1.0000 Uiso . . . . . . . H291 H -0.1341 -0.1046 -0.1822 0.1832 1.0000 Uiso . . . . . . . H301 H -0.0503 -0.0349 -0.0694 0.1671 1.0000 Uiso . . . . . . . H321 H -0.1513 -0.1627 -0.2959 0.2844 1.0000 Uiso . . . . . . . H322 H -0.0060 -0.1289 -0.2944 0.2844 1.0000 Uiso . . . . . . . H331 H -0.0983 -0.1912 -0.4075 0.2882 1.0000 Uiso . . . . . . . H332 H -0.0723 -0.1016 -0.4115 0.2882 1.0000 Uiso . . . . . . . H351 H -0.2759 -0.2388 -0.4934 0.2944 1.0000 Uiso . . . . . . . H352 H -0.2761 -0.1572 -0.5148 0.2944 1.0000 Uiso . . . . . . . H361 H -0.4857 -0.2453 -0.5425 0.2759 1.0000 Uiso . . . . . . . H362 H -0.4751 -0.2515 -0.4643 0.2759 1.0000 Uiso . . . . . . . H381 H -0.6551 -0.1977 -0.5421 0.2688 1.0000 Uiso . . . . . . . H382 H -0.6462 -0.1922 -0.4627 0.2688 1.0000 Uiso . . . . . . . H391 H -0.7457 -0.1041 -0.5152 0.2633 1.0000 Uiso . . . . . . . H392 H -0.6116 -0.0578 -0.5255 0.2633 1.0000 Uiso . . . . . . . H411 H -0.7222 0.0172 -0.4586 0.2761 1.0000 Uiso . . . . . . . H412 H -0.7694 -0.0271 -0.4004 0.2761 1.0000 Uiso . . . . . . . H421 H -0.6439 0.1163 -0.3648 0.2385 1.0000 Uiso . . . . . . . H422 H -0.5250 0.0866 -0.3646 0.2385 1.0000 Uiso . . . . . . . H451 H -0.4779 0.1920 -0.2750 0.1619 1.0000 Uiso . . . . . . . H461 H -0.3914 0.2766 -0.1679 0.1332 1.0000 Uiso . . . . . . . H481 H -0.5611 0.1014 -0.0707 0.1202 1.0000 Uiso . . . . . . . H491 H -0.6462 0.0158 -0.1767 0.1406 1.0000 Uiso . . . . . . . H511 H -0.4185 0.3459 -0.0695 0.1492 1.0000 Uiso . . . . . . . H512 H -0.2846 0.3322 -0.0582 0.1492 1.0000 Uiso . . . . . . . H521 H -0.4005 0.3503 0.0523 0.1324 1.0000 Uiso . . . . . . . H522 H -0.3053 0.4222 0.0326 0.1324 1.0000 Uiso . . . . . . . H531 H -0.1925 0.3115 0.0560 0.1212 1.0000 Uiso . . . . . . . H561 H -0.4699 -0.1578 -0.2879 0.1802 1.0000 Uiso . . . . . . . H562 H -0.5021 -0.1086 -0.3453 0.1802 1.0000 Uiso . . . . . . . H563 H -0.3726 -0.1281 -0.3334 0.1802 1.0000 Uiso . . . . . . . H581 H -0.3196 0.0248 -0.3313 0.1415 1.0000 Uiso . . . . . . . H601 H -0.2192 0.1408 -0.1352 0.1246 1.0000 Uiso . . . . . . . H621 H -0.4130 -0.0923 -0.1793 0.1264 1.0000 Uiso . . . . . . . H651 H -0.1243 0.2312 -0.1800 0.1704 1.0000 Uiso . . . . . . . H661 H -0.1235 0.3111 -0.2898 0.1908 1.0000 Uiso . . . . . . . H662 H 0.0103 0.3093 -0.2506 0.1908 1.0000 Uiso . . . . . . . H671 H -0.0002 0.4241 -0.2029 0.1820 1.0000 Uiso . . . . . . . H672 H -0.0405 0.3695 -0.1494 0.1820 1.0000 Uiso . . . . . . . H701 H -0.3895 0.4253 -0.2158 0.1965 1.0000 Uiso . . . . . . . H711 H -0.4433 0.5105 -0.1388 0.2004 1.0000 Uiso . . . . . . . H731 H -0.0907 0.5640 -0.0132 0.1927 1.0000 Uiso . . . . . . . H741 H -0.0361 0.4787 -0.0911 0.1886 1.0000 Uiso . . . . . . . H761 H -0.2397 0.5590 0.0597 0.2490 1.0000 Uiso . . . . . . . H762 H -0.1641 0.6443 0.0524 0.2490 1.0000 Uiso . . . . . . . H771 H -0.3497 0.6807 0.0663 0.2799 1.0000 Uiso . . . . . . . H772 H -0.3986 0.5991 0.0897 0.2799 1.0000 Uiso . . . . . . . H791 H -0.4165 0.6473 0.1854 0.3155 1.0000 Uiso . . . . . . . H792 H -0.3258 0.7311 0.2197 0.3155 1.0000 Uiso . . . . . . . H801 H -0.2854 0.6769 0.3159 0.3401 1.0000 Uiso . . . . . . . H811 H -0.2893 0.5562 0.2226 0.3164 1.0000 Uiso . . . . . . . H821 H -0.2111 0.4912 0.2992 0.2883 1.0000 Uiso . . . . . . . H822 H -0.1758 0.5624 0.3588 0.2883 1.0000 Uiso . . . . . . . H841 H -0.5065 0.4475 0.2739 0.2552 1.0000 Uiso . . . . . . . H842 H -0.3910 0.4219 0.2578 0.2552 1.0000 Uiso . . . . . . . H851 H -0.5419 0.3225 0.2951 0.2013 1.0000 Uiso . . . . . . . H852 H -0.4986 0.3752 0.3677 0.2013 1.0000 Uiso . . . . . . . H881 H -0.2044 0.2612 0.3617 0.1591 1.0000 Uiso . . . . . . . H891 H -0.1536 0.1747 0.2847 0.1441 1.0000 Uiso . . . . . . . H911 H -0.4170 0.2064 0.1280 0.1227 1.0000 Uiso . . . . . . . H921 H -0.4691 0.2923 0.2071 0.1528 1.0000 Uiso . . . . . . . H941 H -0.3785 0.0990 0.0687 0.1365 1.0000 Uiso . . . . . . . H942 H -0.2711 0.1766 0.0693 0.1365 1.0000 Uiso . . . . . . . H951 H -0.2455 0.0262 0.0585 0.1299 1.0000 Uiso . . . . . . . H952 H -0.1286 0.1018 0.0700 0.1299 1.0000 Uiso . . . . . . . H961 H -0.1981 0.1184 -0.0396 0.1176 1.0000 Uiso . . . . . . . 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 Cl1 0.113(4) 0.101(4) 0.129(5) -0.004(3) 0.018(4) 0.011(3) Fe2 0.250(5) 0.165(3) 0.090(3) -0.012(2) 0.008(3) 0.063(3) C3 0.264(15) 0.166(6) 0.118(10) -0.019(7) 0.005(10) 0.060(8) C4 0.258(9) 0.175(10) 0.122(10) -0.027(9) 0.003(8) 0.057(7) C5 0.250(10) 0.171(12) 0.120(12) -0.010(10) 0.010(9) 0.053(8) C6 0.252(15) 0.171(10) 0.119(9) 0.000(7) 0.022(9) 0.058(10) C7 0.262(15) 0.161(6) 0.112(12) -0.005(8) 0.020(11) 0.057(8) C8 0.250(7) 0.152(10) 0.089(8) -0.015(8) 0.026(6) 0.069(6) C9 0.267(12) 0.159(11) 0.094(6) -0.004(7) 0.022(7) 0.080(9) C10 0.265(14) 0.174(9) 0.094(6) -0.005(6) 0.024(8) 0.083(10) C11 0.237(13) 0.167(5) 0.088(8) -0.013(8) 0.010(8) 0.065(8) C12 0.227(10) 0.161(7) 0.098(5) -0.015(6) 0.018(5) 0.069(7) C13 0.164(15) 0.144(14) 0.098(5) -0.008(7) 0.020(6) 0.055(10) C14 0.146(15) 0.140(16) 0.107(7) -0.023(12) 0.003(10) 0.049(11) C15 0.095(12) 0.124(14) 0.106(7) -0.017(10) 0.013(8) 0.019(9) C16 0.075(11) 0.097(13) 0.102(10) 0.003(9) 0.029(7) -0.003(8) C17 0.084(11) 0.115(13) 0.107(6) 0.000(10) 0.029(7) 0.008(8) C18 0.126(14) 0.123(14) 0.109(6) -0.013(12) 0.024(9) 0.029(10) C19 0.097(13) 0.129(15) 0.113(8) -0.016(12) 0.011(9) 0.025(10) O20 0.105(12) 0.207(17) 0.150(11) -0.047(12) -0.023(9) 0.054(10) N21 0.088(10) 0.123(12) 0.120(8) -0.038(10) 0.009(8) 0.012(8) C22 0.103(13) 0.151(16) 0.136(11) -0.040(11) 0.013(9) 0.033(11) C23 0.090(13) 0.171(15) 0.140(10) -0.056(11) 0.009(9) 0.048(8) O24 0.109(10) 0.150(11) 0.115(8) -0.029(7) -0.009(8) 0.056(7) C25 0.112(14) 0.154(12) 0.113(8) -0.027(8) -0.005(11) 0.034(10) C26 0.122(15) 0.167(14) 0.124(9) -0.031(9) 0.030(13) 0.039(12) C27 0.128(17) 0.197(16) 0.120(8) -0.028(10) 0.014(13) 0.035(12) C28 0.138(16) 0.188(15) 0.133(9) -0.033(9) -0.031(13) 0.038(12) C29 0.128(16) 0.142(13) 0.149(11) -0.023(9) -0.043(13) 0.043(11) C30 0.112(15) 0.136(12) 0.139(9) -0.015(9) -0.022(12) 0.053(10) O31 0.178(15) 0.228(17) 0.145(10) -0.062(11) -0.022(11) 0.057(13) C32 0.23(2) 0.25(2) 0.173(16) -0.076(17) -0.032(15) 0.09(2) C33 0.214(17) 0.28(2) 0.175(16) -0.091(16) -0.032(17) 0.11(2) O34 0.208(15) 0.32(2) 0.141(13) -0.087(14) -0.001(12) 0.104(18) C35 0.233(17) 0.30(3) 0.142(16) -0.073(18) -0.035(17) 0.127(18) C36 0.233(17) 0.27(2) 0.135(18) -0.050(19) -0.028(16) 0.122(19) O37 0.242(16) 0.27(2) 0.122(13) -0.054(14) -0.037(14) 0.130(17) C38 0.240(16) 0.26(2) 0.137(18) -0.066(16) -0.06(2) 0.129(19) C39 0.26(2) 0.27(2) 0.129(15) -0.056(16) -0.030(17) 0.141(18) O40 0.26(2) 0.255(19) 0.133(12) -0.060(13) -0.038(14) 0.115(15) C41 0.28(2) 0.26(2) 0.112(9) -0.064(14) -0.032(17) 0.123(16) C42 0.26(2) 0.220(18) 0.094(8) -0.025(10) -0.015(16) 0.089(16) O43 0.150(12) 0.174(12) 0.102(7) -0.031(7) -0.017(9) 0.065(10) C44 0.093(12) 0.125(10) 0.095(7) -0.011(6) 0.007(9) 0.052(9) C45 0.141(16) 0.130(11) 0.120(8) 0.011(8) 0.022(12) 0.050(11) C46 0.117(14) 0.092(10) 0.122(8) 0.020(7) 0.027(11) 0.035(9) C47 0.107(13) 0.093(9) 0.118(7) 0.021(6) 0.014(11) 0.026(8) C48 0.084(12) 0.096(9) 0.095(7) 0.010(6) 0.014(9) 0.023(8) C49 0.089(12) 0.127(11) 0.096(8) 0.005(6) -0.027(10) 0.024(9) O50 0.088(8) 0.092(6) 0.115(7) 0.026(6) 0.012(7) 0.003(7) C51 0.136(15) 0.091(7) 0.121(10) 0.027(8) 0.006(9) 0.000(11) C52 0.114(13) 0.088(10) 0.134(10) 0.017(8) 0.022(8) 0.026(10) N53 0.102(11) 0.071(9) 0.115(9) 0.003(7) 0.018(7) 0.011(8) C54 0.110(12) 0.084(13) 0.117(9) -0.007(8) 0.024(8) 0.016(8) O55 0.169(13) 0.108(11) 0.123(10) 0.004(8) 0.042(9) 0.053(9) C56 0.16(2) 0.124(10) 0.112(11) -0.003(9) 0.025(15) -0.008(15) N57 0.070(9) 0.124(7) 0.094(6) 0.007(6) 0.002(8) -0.007(8) C58 0.072(12) 0.138(9) 0.098(10) 0.000(6) 0.025(10) -0.027(11) C59 0.071(11) 0.122(8) 0.101(7) 0.008(6) 0.016(10) -0.008(9) C60 0.070(11) 0.118(10) 0.100(7) 0.008(7) 0.016(10) 0.011(10) C61 0.048(10) 0.126(9) 0.098(5) 0.009(5) 0.010(9) 0.003(9) C62 0.067(11) 0.120(10) 0.100(7) 0.010(7) 0.017(10) 0.011(9) C63 0.115(15) 0.140(10) 0.127(10) 0.018(7) 0.045(13) -0.022(12) O64 0.195(16) 0.159(13) 0.123(9) 0.031(8) 0.038(13) -0.009(12) N65 0.134(14) 0.127(9) 0.139(12) 0.020(8) 0.047(11) -0.019(10) C66 0.158(16) 0.144(9) 0.143(17) 0.028(9) 0.058(14) -0.031(10) C67 0.131(13) 0.128(9) 0.163(17) 0.026(11) 0.034(14) -0.030(12) O68 0.142(11) 0.146(13) 0.149(12) 0.049(9) 0.024(11) -0.013(10) C69 0.132(12) 0.142(16) 0.150(15) 0.056(9) 0.018(10) -0.005(11) C70 0.145(13) 0.148(18) 0.176(16) 0.075(11) 0.012(12) 0.009(13) C71 0.137(14) 0.150(19) 0.209(18) 0.068(12) 0.015(11) 0.014(13) C72 0.148(14) 0.134(17) 0.220(16) 0.051(12) 0.019(11) 0.004(13) C73 0.125(13) 0.128(18) 0.193(17) 0.027(11) 0.016(12) -0.023(12) C74 0.140(13) 0.122(18) 0.178(17) 0.036(11) 0.008(11) -0.009(12) O75 0.174(15) 0.181(16) 0.257(15) 0.029(13) 0.022(14) 0.034(12) C76 0.18(2) 0.20(2) 0.235(15) 0.053(18) 0.065(15) 0.029(18) C77 0.21(2) 0.20(2) 0.281(19) 0.06(2) 0.082(16) 0.062(19) O78 0.26(2) 0.23(2) 0.292(19) 0.010(16) 0.086(16) 0.079(18) C79 0.24(2) 0.26(3) 0.29(2) 0.037(19) 0.082(19) 0.10(2) C80 0.26(3) 0.27(3) 0.28(2) 0.03(2) 0.05(2) 0.07(2) C81 0.28(3) 0.24(3) 0.23(2) 0.028(18) 0.04(2) 0.05(2) C82 0.29(3) 0.23(2) 0.18(2) -0.005(17) 0.02(2) 0.023(18) O83 0.32(3) 0.181(16) 0.197(18) -0.030(12) 0.032(17) 0.002(16) C84 0.28(2) 0.162(18) 0.15(2) -0.005(11) -0.001(17) 0.054(15) C85 0.22(2) 0.147(16) 0.128(17) -0.021(12) 0.004(14) 0.070(13) O86 0.159(13) 0.180(14) 0.098(9) -0.004(8) 0.019(9) 0.038(10) C87 0.125(14) 0.163(16) 0.087(8) 0.004(10) 0.005(9) 0.032(10) C88 0.102(14) 0.175(18) 0.075(9) 0.009(9) -0.008(9) 0.017(10) C89 0.108(13) 0.155(17) 0.084(8) 0.022(10) -0.014(9) 0.031(10) C90 0.082(11) 0.111(13) 0.077(7) 0.025(8) 0.002(7) 0.016(8) C91 0.091(12) 0.107(13) 0.077(8) 0.021(8) -0.001(8) 0.019(8) C92 0.115(13) 0.131(15) 0.091(9) 0.012(10) 0.002(9) 0.038(10) O93 0.108(9) 0.116(10) 0.110(7) 0.017(7) 0.014(7) 0.028(7) C94 0.101(13) 0.103(13) 0.105(6) 0.001(10) 0.018(9) 0.006(10) C95 0.104(13) 0.090(12) 0.103(6) 0.006(8) -0.007(9) 0.025(10) N96 0.068(9) 0.112(9) 0.104(6) 0.008(7) 0.007(7) 0.014(7) C97 0.064(11) 0.102(10) 0.097(5) 0.012(6) 0.004(8) 0.029(7) O98 0.106(10) 0.096(8) 0.091(8) 0.004(6) 0.007(7) 0.018(7) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2740(8) 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 Fe2 . C3 . 2.046(11) yes Fe2 . C4 . 2.041(11) yes Fe2 . C5 . 2.022(12) yes Fe2 . C6 . 2.022(11) yes Fe2 . C7 . 2.046(12) yes Fe2 . C8 . 2.020(10) yes Fe2 . C9 . 2.009(10) yes Fe2 . C10 . 2.017(11) yes Fe2 . C11 . 2.031(10) yes Fe2 . C12 . 2.039(10) yes C3 . C4 . 1.42(2) yes C3 . C7 . 1.40(2) yes C3 . H31 . 0.933 no C4 . C5 . 1.36(2) yes C4 . H41 . 0.943 no C5 . C6 . 1.39(2) yes C5 . H51 . 0.957 no C6 . C7 . 1.40(2) yes C6 . H61 . 0.952 no C7 . H71 . 0.934 no C8 . C9 . 1.432(15) yes C8 . C12 . 1.447(13) yes C8 . H81 . 0.956 no C9 . C10 . 1.42(2) yes C9 . H91 . 0.958 no C10 . C11 . 1.424(15) yes C10 . H101 . 0.956 no C11 . C12 . 1.431(14) yes C11 . H111 . 0.951 no C12 . C13 . 1.486(12) yes C13 . C14 . 1.393(12) yes C13 . C18 . 1.401(12) yes C14 . C15 . 1.402(12) yes C14 . H141 . 0.949 no C15 . C16 . 1.400(12) yes C15 . C19 . 1.498(14) yes C16 . C17 . 1.389(12) yes C16 . H161 . 0.947 no C17 . C18 . 1.390(12) yes C17 . C54 . 1.480(14) yes C18 . H181 . 0.949 no C19 . O20 . 1.237(14) yes C19 . N21 . 1.348(15) yes N21 . C22 . 1.446(16) yes N21 . H211 . 0.853 no C22 . C23 . 1.51(2) yes C22 . H221 . 0.986 no C22 . H222 . 0.936 no C23 . O24 . 1.47(2) yes C23 . H231 . 0.964 no C23 . H232 . 0.911 no O24 . C25 . 1.375(14) yes C25 . C26 . 1.380(16) yes C25 . C30 . 1.384(16) yes C26 . C27 . 1.383(15) yes C26 . H261 . 0.945 no C27 . C28 . 1.390(16) yes C27 . H271 . 0.944 no C28 . C29 . 1.389(16) yes C28 . O31 . 1.383(12) yes C29 . C30 . 1.387(15) yes C29 . H291 . 0.950 no C30 . H301 . 0.947 no O31 . C32 . 1.31(2) yes C32 . C33 . 1.53(3) yes C32 . H321 . 0.973 no C32 . H322 . 0.930 no C33 . O34 . 1.39(3) yes C33 . H331 . 0.942 no C33 . H332 . 0.956 no O34 . C35 . 1.40(2) yes C35 . C36 . 1.50(3) yes C35 . H351 . 0.936 no C35 . H352 . 1.030 no C36 . O37 . 1.41(3) yes C36 . H361 . 0.954 no C36 . H362 . 0.917 no O37 . C38 . 1.36(3) yes C38 . C39 . 1.50(3) yes C38 . H381 . 0.935 no C38 . H382 . 0.942 no C39 . O40 . 1.46(2) yes C39 . H391 . 0.958 no C39 . H392 . 0.985 no O40 . C41 . 1.44(3) yes C41 . C42 . 1.52(3) yes C41 . H411 . 0.912 no C41 . H412 . 0.993 no C42 . O43 . 1.42(2) yes C42 . H421 . 0.930 no C42 . H422 . 0.987 no O43 . C44 . 1.382(14) yes C44 . C45 . 1.388(15) yes C44 . C49 . 1.402(15) yes C45 . C46 . 1.397(14) yes C45 . H451 . 0.942 no C46 . C47 . 1.384(15) yes C46 . H461 . 0.953 no C47 . C48 . 1.381(14) yes C47 . O50 . 1.376(11) yes C48 . C49 . 1.392(14) yes C48 . H481 . 0.944 no C49 . H491 . 0.947 no O50 . C51 . 1.431(18) yes C51 . C52 . 1.50(2) yes C51 . H511 . 0.961 no C51 . H512 . 0.926 no C52 . N53 . 1.448(16) yes C52 . H521 . 0.955 no C52 . H522 . 0.960 no N53 . C54 . 1.336(14) yes N53 . H531 . 0.846 no C54 . O55 . 1.256(13) yes C56 . N57 . 1.473(17) yes C56 . H561 . 0.963 no C56 . H562 . 0.953 no C56 . H563 . 0.932 no N57 . C58 . 1.339(12) yes N57 . C62 . 1.333(12) yes C58 . C59 . 1.368(11) yes C58 . H581 . 0.953 no C59 . C60 . 1.381(12) yes C59 . C63 . 1.520(14) yes C60 . C61 . 1.384(12) yes C60 . H601 . 0.949 no C61 . C62 . 1.372(11) yes C61 . C97 . 1.483(14) yes C62 . H621 . 0.954 no C63 . O64 . 1.236(14) yes C63 . N65 . 1.331(15) yes N65 . C66 . 1.466(17) yes N65 . H651 . 0.847 no C66 . C67 . 1.50(2) yes C66 . H661 . 0.968 no C66 . H662 . 0.937 no C67 . O68 . 1.44(2) yes C67 . H671 . 0.970 no C67 . H672 . 0.919 no O68 . C69 . 1.380(16) yes C69 . C70 . 1.358(16) yes C69 . C74 . 1.388(16) yes C70 . C71 . 1.374(16) yes C70 . H701 . 0.968 no C71 . C72 . 1.374(17) yes C71 . H711 . 0.964 no C72 . C73 . 1.368(17) yes C72 . O75 . 1.392(16) yes C73 . C74 . 1.382(15) yes C73 . H731 . 0.941 no C74 . H741 . 0.943 no O75 . C76 . 1.46(2) yes C76 . C77 . 1.51(3) yes C76 . H761 . 0.904 no C76 . H762 . 0.981 no C77 . O78 . 1.44(3) yes C77 . H771 . 1.048 no C77 . H772 . 0.911 no O78 . C79 . 1.46(3) yes C79 . C80 . 1.486(10) yes C79 . H791 . 1.013 no C79 . H792 . 0.851 no C80 . C81 . 1.304(14) yes C80 . H801 . 1.039 no C81 . C82 . 1.44(3) yes C81 . H811 . 0.898 no C82 . O83 . 1.35(2) yes C82 . H821 . 1.046 no C82 . H822 . 0.868 no O83 . C84 . 1.38(3) yes C84 . C85 . 1.50(3) yes C84 . H841 . 0.985 no C84 . H842 . 0.870 no C85 . O86 . 1.42(2) yes C85 . H851 . 0.944 no C85 . H852 . 0.966 no O86 . C87 . 1.379(15) yes C87 . C88 . 1.358(15) yes C87 . C92 . 1.371(15) yes C88 . C89 . 1.361(14) yes C88 . H881 . 0.959 no C89 . C90 . 1.384(15) yes C89 . H891 . 0.960 no C90 . C91 . 1.372(15) yes C90 . O93 . 1.390(14) yes C91 . C92 . 1.377(14) yes C91 . H911 . 0.953 no C92 . H921 . 0.950 no O93 . C94 . 1.439(18) yes C94 . C95 . 1.49(2) yes C94 . H941 . 0.912 no C94 . H942 . 0.999 no C95 . N96 . 1.435(16) yes C95 . H951 . 0.950 no C95 . H952 . 0.942 no N96 . C97 . 1.335(14) yes N96 . H961 . 0.850 no C97 . O98 . 1.247(13) 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 C3 . Fe2 . C4 . 40.8(6) yes C3 . Fe2 . C5 . 67.1(6) yes C4 . Fe2 . C5 . 39.2(6) yes C3 . Fe2 . C6 . 67.0(6) yes C4 . Fe2 . C6 . 67.0(6) yes C5 . Fe2 . C6 . 40.3(6) yes C3 . Fe2 . C7 . 40.0(6) yes C4 . Fe2 . C7 . 67.9(6) yes C5 . Fe2 . C7 . 67.8(6) yes C6 . Fe2 . C7 . 40.2(6) yes C3 . Fe2 . C8 . 126.9(8) yes C4 . Fe2 . C8 . 164.2(9) yes C5 . Fe2 . C8 . 155.5(9) yes C6 . Fe2 . C8 . 121.3(8) yes C7 . Fe2 . C8 . 108.9(6) yes C3 . Fe2 . C9 . 107.0(6) yes C4 . Fe2 . C9 . 125.3(8) yes C5 . Fe2 . C9 . 161.9(10) yes C6 . Fe2 . C9 . 155.3(11) yes C7 . Fe2 . C9 . 119.7(8) yes C3 . Fe2 . C10 . 118.2(7) yes C4 . Fe2 . C10 . 105.8(6) yes C5 . Fe2 . C10 . 124.7(9) yes C6 . Fe2 . C10 . 163.2(11) yes C7 . Fe2 . C10 . 153.1(9) yes C3 . Fe2 . C11 . 152.4(9) yes C4 . Fe2 . C11 . 117.5(8) yes C5 . Fe2 . C11 . 107.1(6) yes C6 . Fe2 . C11 . 127.1(8) yes C7 . Fe2 . C11 . 165.3(9) yes C3 . Fe2 . C12 . 165.5(9) yes C4 . Fe2 . C12 . 152.3(9) yes C5 . Fe2 . C12 . 119.9(7) yes C6 . Fe2 . C12 . 109.3(5) yes C7 . Fe2 . C12 . 128.2(7) yes C8 . Fe2 . C9 . 41.6(5) yes C8 . Fe2 . C10 . 69.7(5) yes C9 . Fe2 . C10 . 41.3(6) yes C8 . Fe2 . C11 . 69.7(5) yes C9 . Fe2 . C11 . 69.6(5) yes C10 . Fe2 . C11 . 41.2(5) yes C8 . Fe2 . C12 . 41.8(4) yes C9 . Fe2 . C12 . 70.1(4) yes C10 . Fe2 . C12 . 69.6(4) yes C11 . Fe2 . C12 . 41.2(4) yes Fe2 . C3 . C4 . 69.4(7) yes Fe2 . C3 . C7 . 70.0(6) yes C4 . C3 . C7 . 108.0(11) yes Fe2 . C3 . H31 . 128.0 no C4 . C3 . H31 . 126.7 no C7 . C3 . H31 . 125.3 no C3 . C4 . Fe2 . 69.8(7) yes C3 . C4 . C5 . 107.6(11) yes Fe2 . C4 . C5 . 69.6(6) yes C3 . C4 . H41 . 125.5 no Fe2 . C4 . H41 . 127.5 no C5 . C4 . H41 . 126.9 no C4 . C5 . Fe2 . 71.2(7) yes C4 . C5 . C6 . 109.0(11) yes Fe2 . C5 . C6 . 69.9(7) yes C4 . C5 . H51 . 125.1 no Fe2 . C5 . H51 . 125.8 no C6 . C5 . H51 . 126.0 no C5 . C6 . Fe2 . 69.8(7) yes C5 . C6 . C7 . 108.7(11) yes Fe2 . C6 . C7 . 70.8(7) yes C5 . C6 . H61 . 124.4 no Fe2 . C6 . H61 . 125.7 no C7 . C6 . H61 . 126.9 no C3 . C7 . C6 . 106.8(11) yes C3 . C7 . Fe2 . 70.0(6) yes C6 . C7 . Fe2 . 69.0(6) yes C3 . C7 . H71 . 127.8 no C6 . C7 . H71 . 125.3 no Fe2 . C7 . H71 . 127.8 no Fe2 . C8 . C9 . 68.8(5) yes Fe2 . C8 . C12 . 69.8(5) yes C9 . C8 . C12 . 107.8(8) yes Fe2 . C8 . H81 . 125.4 no C9 . C8 . H81 . 126.1 no C12 . C8 . H81 . 126.0 no C8 . C9 . Fe2 . 69.6(5) yes C8 . C9 . C10 . 108.1(8) yes Fe2 . C9 . C10 . 69.6(6) yes C8 . C9 . H91 . 125.9 no Fe2 . C9 . H91 . 125.6 no C10 . C9 . H91 . 126.0 no C9 . C10 . Fe2 . 69.1(6) yes C9 . C10 . C11 . 108.5(8) yes Fe2 . C10 . C11 . 69.9(5) yes C9 . C10 . H101 . 126.4 no Fe2 . C10 . H101 . 125.2 no C11 . C10 . H101 . 125.1 no C10 . C11 . Fe2 . 68.9(5) yes C10 . C11 . C12 . 108.5(8) yes Fe2 . C11 . C12 . 69.7(6) yes C10 . C11 . H111 . 126.2 no Fe2 . C11 . H111 . 125.4 no C12 . C11 . H111 . 125.3 no C8 . C12 . C11 . 107.1(7) yes C8 . C12 . Fe2 . 68.4(5) yes C11 . C12 . Fe2 . 69.1(5) yes C8 . C12 . C13 . 127.3(7) yes C11 . C12 . C13 . 125.6(7) yes Fe2 . C12 . C13 . 127.6(7) yes C12 . C13 . C14 . 120.5(5) yes C12 . C13 . C18 . 120.9(5) yes C14 . C13 . C18 . 118.5(6) yes C13 . C14 . C15 . 120.7(7) yes C13 . C14 . H141 . 119.8 no C15 . C14 . H141 . 119.4 no C14 . C15 . C16 . 119.4(8) yes C14 . C15 . C19 . 116.6(10) yes C16 . C15 . C19 . 124.0(10) yes C15 . C16 . C17 . 120.5(7) yes C15 . C16 . H161 . 119.5 no C17 . C16 . H161 . 120.0 no C16 . C17 . C18 . 119.2(8) yes C16 . C17 . C54 . 121.6(10) yes C18 . C17 . C54 . 119.1(10) yes C13 . C18 . C17 . 121.6(7) yes C13 . C18 . H181 . 119.4 no C17 . C18 . H181 . 119.0 no C15 . C19 . O20 . 120.3(11) yes C15 . C19 . N21 . 118.1(11) yes O20 . C19 . N21 . 121.6(12) yes C19 . N21 . C22 . 119.9(12) yes C19 . N21 . H211 . 120.4 no C22 . N21 . H211 . 119.7 no N21 . C22 . C23 . 112.6(14) yes N21 . C22 . H221 . 107.3 no C23 . C22 . H221 . 109.4 no N21 . C22 . H222 . 108.9 no C23 . C22 . H222 . 110.8 no H221 . C22 . H222 . 107.6 no C22 . C23 . O24 . 106.6(15) yes C22 . C23 . H231 . 108.4 no O24 . C23 . H231 . 108.3 no C22 . C23 . H232 . 110.5 no O24 . C23 . H232 . 111.3 no H231 . C23 . H232 . 111.6 no C23 . O24 . C25 . 117.8(13) yes O24 . C25 . C26 . 120.2(15) yes O24 . C25 . C30 . 119.4(15) yes C26 . C25 . C30 . 120.5(9) yes C25 . C26 . C27 . 119.8(9) yes C25 . C26 . H261 . 119.8 no C27 . C26 . H261 . 120.4 no C26 . C27 . C28 . 120.4(9) yes C26 . C27 . H271 . 119.9 no C28 . C27 . H271 . 119.7 no C27 . C28 . C29 . 119.3(9) yes C27 . C28 . O31 . 118.0(17) yes C29 . C28 . O31 . 122.6(17) yes C28 . C29 . C30 . 120.3(9) yes C28 . C29 . H291 . 119.7 no C30 . C29 . H291 . 120.0 no C29 . C30 . C25 . 119.7(9) yes C29 . C30 . H301 . 119.8 no C25 . C30 . H301 . 120.5 no C28 . O31 . C32 . 118.1(14) yes O31 . C32 . C33 . 106.1(20) yes O31 . C32 . H321 . 108.1 no C33 . C32 . H321 . 109.3 no O31 . C32 . H322 . 111.4 no C33 . C32 . H322 . 112.6 no H321 . C32 . H322 . 109.2 no C32 . C33 . O34 . 106(2) yes C32 . C33 . H331 . 109.5 no O34 . C33 . H331 . 111.6 no C32 . C33 . H332 . 108.5 no O34 . C33 . H332 . 111.8 no H331 . C33 . H332 . 109.6 no C33 . O34 . C35 . 114.2(20) yes O34 . C35 . C36 . 110(2) yes O34 . C35 . H351 . 112.1 no C36 . C35 . H351 . 113.9 no O34 . C35 . H352 . 107.2 no C36 . C35 . H352 . 108.9 no H351 . C35 . H352 . 104.1 no C35 . C36 . O37 . 108(2) yes C35 . C36 . H361 . 108.2 no O37 . C36 . H361 . 110.2 no C35 . C36 . H362 . 106.6 no O37 . C36 . H362 . 112.0 no H361 . C36 . H362 . 112.0 no C36 . O37 . C38 . 109(2) yes O37 . C38 . C39 . 111(3) yes O37 . C38 . H381 . 111.6 no C39 . C38 . H381 . 107.1 no O37 . C38 . H382 . 110.5 no C39 . C38 . H382 . 105.3 no H381 . C38 . H382 . 111.4 no C38 . C39 . O40 . 109(2) yes C38 . C39 . H391 . 112.4 no O40 . C39 . H391 . 110.7 no C38 . C39 . H392 . 110.3 no O40 . C39 . H392 . 108.2 no H391 . C39 . H392 . 106.0 no C39 . O40 . C41 . 109.8(18) yes O40 . C41 . C42 . 109(2) yes O40 . C41 . H411 . 112.3 no C42 . C41 . H411 . 112.1 no O40 . C41 . H412 . 107.3 no C42 . C41 . H412 . 106.8 no H411 . C41 . H412 . 108.9 no C41 . C42 . O43 . 105.1(18) yes C41 . C42 . H421 . 113.7 no O43 . C42 . H421 . 112.3 no C41 . C42 . H422 . 109.6 no O43 . C42 . H422 . 108.0 no H421 . C42 . H422 . 108.0 no C42 . O43 . C44 . 118.1(12) yes O43 . C44 . C45 . 123.8(13) yes O43 . C44 . C49 . 116.3(13) yes C45 . C44 . C49 . 119.9(9) yes C44 . C45 . C46 . 119.8(9) yes C44 . C45 . H451 . 119.4 no C46 . C45 . H451 . 120.8 no C45 . C46 . C47 . 120.2(9) yes C45 . C46 . H461 . 119.2 no C47 . C46 . H461 . 120.6 no C46 . C47 . C48 . 120.1(9) yes C46 . C47 . O50 . 122.3(12) yes C48 . C47 . O50 . 117.6(12) yes C47 . C48 . C49 . 120.6(9) yes C47 . C48 . H481 . 119.0 no C49 . C48 . H481 . 120.4 no C44 . C49 . C48 . 119.4(9) yes C44 . C49 . H491 . 121.1 no C48 . C49 . H491 . 119.5 no C47 . O50 . C51 . 118.7(11) yes O50 . C51 . C52 . 109.4(13) yes O50 . C51 . H511 . 106.9 no C52 . C51 . H511 . 109.8 no O50 . C51 . H512 . 109.2 no C52 . C51 . H512 . 110.9 no H511 . C51 . H512 . 110.6 no C51 . C52 . N53 . 110.4(14) yes C51 . C52 . H521 . 109.8 no N53 . C52 . H521 . 110.9 no C51 . C52 . H522 . 107.9 no N53 . C52 . H522 . 109.4 no H521 . C52 . H522 . 108.3 no C52 . N53 . C54 . 120.2(12) yes C52 . N53 . H531 . 119.1 no C54 . N53 . H531 . 120.7 no C17 . C54 . N53 . 118.7(11) yes C17 . C54 . O55 . 119.9(11) yes N53 . C54 . O55 . 120.9(11) yes N57 . C56 . H561 . 108.7 no N57 . C56 . H562 . 109.2 no H561 . C56 . H562 . 108.1 no N57 . C56 . H563 . 110.2 no H561 . C56 . H563 . 109.9 no H562 . C56 . H563 . 110.7 no C56 . N57 . C58 . 119.1(8) yes C56 . N57 . C62 . 119.8(8) yes C58 . N57 . C62 . 121.2(7) yes N57 . C58 . C59 . 120.9(7) yes N57 . C58 . H581 . 119.7 no C59 . C58 . H581 . 119.3 no C58 . C59 . C60 . 118.7(7) yes C58 . C59 . C63 . 116.8(10) yes C60 . C59 . C63 . 124.5(10) yes C59 . C60 . C61 . 119.8(7) yes C59 . C60 . H601 . 120.1 no C61 . C60 . H601 . 120.1 no C60 . C61 . C62 . 118.8(7) yes C60 . C61 . C97 . 124.2(10) yes C62 . C61 . C97 . 116.7(9) yes C61 . C62 . N57 . 120.6(7) yes C61 . C62 . H621 . 119.5 no N57 . C62 . H621 . 119.9 no C59 . C63 . O64 . 119.7(11) yes C59 . C63 . N65 . 116.6(11) yes O64 . C63 . N65 . 122.9(12) yes C63 . N65 . C66 . 122.4(13) yes C63 . N65 . H651 . 119.4 no C66 . N65 . H651 . 118.2 no N65 . C66 . C67 . 111.7(15) yes N65 . C66 . H661 . 109.6 no C67 . C66 . H661 . 107.7 no N65 . C66 . H662 . 110.9 no C67 . C66 . H662 . 107.9 no H661 . C66 . H662 . 109.0 no C66 . C67 . O68 . 106.5(16) yes C66 . C67 . H671 . 109.9 no O68 . C67 . H671 . 107.6 no C66 . C67 . H672 . 111.9 no O68 . C67 . H672 . 110.3 no H671 . C67 . H672 . 110.3 no C67 . O68 . C69 . 116.9(14) yes O68 . C69 . C70 . 114.9(17) yes O68 . C69 . C74 . 125.3(16) yes C70 . C69 . C74 . 119.8(10) yes C69 . C70 . C71 . 120.2(9) yes C69 . C70 . H701 . 121.5 no C71 . C70 . H701 . 118.3 no C70 . C71 . C72 . 120.3(9) yes C70 . C71 . H711 . 120.4 no C72 . C71 . H711 . 119.2 no C71 . C72 . C73 . 120.0(10) yes C71 . C72 . O75 . 117.0(17) yes C73 . C72 . O75 . 123.0(17) yes C72 . C73 . C74 . 119.7(9) yes C72 . C73 . H731 . 121.1 no C74 . C73 . H731 . 119.1 no C69 . C74 . C73 . 120.0(9) yes C69 . C74 . H741 . 118.1 no C73 . C74 . H741 . 121.9 no C72 . O75 . C76 . 114.1(13) yes O75 . C76 . C77 . 110.6(19) yes O75 . C76 . H761 . 109.7 no C77 . C76 . H761 . 110.4 no O75 . C76 . H762 . 105.4 no C77 . C76 . H762 . 110.0 no H761 . C76 . H762 . 110.7 no C76 . C77 . O78 . 113(2) yes C76 . C77 . H771 . 102.7 no O78 . C77 . H771 . 109.8 no C76 . C77 . H772 . 106.9 no O78 . C77 . H772 . 118.7 no H771 . C77 . H772 . 104.5 no C77 . O78 . C79 . 111(2) yes O78 . C79 . C80 . 111.0(7) yes O78 . C79 . H791 . 104.5 no C80 . C79 . H791 . 98.8 no O78 . C79 . H792 . 111.2 no C80 . C79 . H792 . 117.7 no H791 . C79 . H792 . 112.3 no C79 . C80 . C81 . 126.3(3) yes C79 . C80 . H801 . 110.0 no C81 . C80 . H801 . 119.2 no C80 . C81 . C82 . 126.5(3) yes C80 . C81 . H811 . 102.0 no C82 . C81 . H811 . 126.0 no C81 . C82 . O83 . 111.3(19) yes C81 . C82 . H821 . 98.7 no O83 . C82 . H821 . 103.9 no C81 . C82 . H822 . 114.3 no O83 . C82 . H822 . 118.2 no H821 . C82 . H822 . 107.9 no C82 . O83 . C84 . 115(2) yes O83 . C84 . C85 . 109(2) yes O83 . C84 . H841 . 104.5 no C85 . C84 . H841 . 105.7 no O83 . C84 . H842 . 112.0 no C85 . C84 . H842 . 112.0 no H841 . C84 . H842 . 113.4 no C84 . C85 . O86 . 106(2) yes C84 . C85 . H851 . 109.9 no O86 . C85 . H851 . 110.6 no C84 . C85 . H852 . 112.2 no O86 . C85 . H852 . 109.8 no H851 . C85 . H852 . 108.6 no C85 . O86 . C87 . 118.6(13) yes O86 . C87 . C88 . 114.5(14) yes O86 . C87 . C92 . 124.8(14) yes C88 . C87 . C92 . 120.7(9) yes C87 . C88 . C89 . 120.4(9) yes C87 . C88 . H881 . 120.4 no C89 . C88 . H881 . 119.2 no C88 . C89 . C90 . 119.5(9) yes C88 . C89 . H891 . 120.5 no C90 . C89 . H891 . 120.0 no C89 . C90 . C91 . 120.4(9) yes C89 . C90 . O93 . 116.0(12) yes C91 . C90 . O93 . 123.6(12) yes C90 . C91 . C92 . 119.3(8) yes C90 . C91 . H911 . 119.9 no C92 . C91 . H911 . 120.8 no C91 . C92 . C87 . 119.8(9) yes C91 . C92 . H921 . 120.3 no C87 . C92 . H921 . 119.9 no C90 . O93 . C94 . 117.9(11) yes O93 . C94 . C95 . 106.9(13) yes O93 . C94 . H941 . 113.3 no C95 . C94 . H941 . 113.1 no O93 . C94 . H942 . 107.6 no C95 . C94 . H942 . 107.2 no H941 . C94 . H942 . 108.4 no C94 . C95 . N96 . 113.5(13) yes C94 . C95 . H951 . 104.4 no N96 . C95 . H951 . 109.7 no C94 . C95 . H952 . 108.3 no N96 . C95 . H952 . 110.5 no H951 . C95 . H952 . 110.2 no C95 . N96 . C97 . 124.0(12) yes C95 . N96 . H961 . 117.5 no C97 . N96 . H961 . 118.5 no C61 . C97 . N96 . 115.8(10) yes C61 . C97 . O98 . 120.3(10) yes N96 . C97 . O98 . 123.9(11) 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 C6 . H61 . O68 2_565 153 0.95 2.47 3.35(3) yes C29 . H291 . O20 2_555 178 0.95 2.59 3.54(3) yes C30 . H301 . O24 2_555 176 0.95 2.53 3.48(3) yes C56 . H561 . C87 2_455 147 0.96 2.59 3.44(3) yes C56 . H562 . O40 . 161 0.95 2.34 3.26(3) yes C56 . H563 . O34 . 166 0.93 2.38 3.29(3) yes C85 . H851 . O20 1_455 165 0.94 2.41 3.33(3) yes C92 . H921 . O20 1_455 131 0.95 2.56 3.27(3) yes C94 . H941 . O98 2_455 167 0.91 2.55 3.44(3) yes # Attachment '- 3 3Catenane 4Cl2 012CJS11.cif' #============================================================================== #============================================================================== data_3Catenane _database_code_depnum_ccdc_archive 'CCDC 853870' #TrackingRef '- 3 3Catenane 4Cl2 012CJS11.cif' #============================================================================== _audit_creation_date 11-02-24 _audit_creation_method CRYSTALS_ver_14.07 _oxford_structure_analysis_title 012CJS11 _chemical_name_systematic . _chemical_melting_point . # start Validation Reply Form _vrf_DIFMX01_3Catenane ; PROBLEM: The maximum difference density is > 0.1*ZMAX*1.00 _refine_diff_density_max given = 3.450 Test value = 2.600 RESPONSE: The residual electron density corresponds to a third set of atomic coordinates for the disorded portion of the polyether chain, in particular another oxygen atom close to O(336) and O(636) would be required. However, it was not possible to construct a meaningful model which would take this into account. For this reason, a two-component disorder model was used. ; # end Validation Reply Form _cell_length_a 15.7014(11) _cell_length_b 18.6485(8) _cell_length_c 28.3126(16) _cell_angle_alpha 98.202(4) _cell_angle_beta 99.703(5) _cell_angle_gamma 102.308(5) _cell_volume 7845.2(8) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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 0.0181 0.0091 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 0.0311 0.0180 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 0.0492 0.0322 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' Cl 0.3639 0.7018 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe -1.1336 3.1974 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 2 # Given Formula = C60 Cl4.80 Fe1.60 N3.20 O15.20 # Dc = 1.34 Fooo = 3432.00 Mu = 54.38 M = 3170.50 # Found Formula = C60.80 H68.80 Cl5.60 Fe0.80 N4 O13.60 # Dc = 1.39 FOOO = 3432.00 Mu = 43.14 M = 3291.14 _chemical_formula_sum 'C152 H172 Cl14 Fe2 N10 O34' _chemical_formula_moiety ; C64 H76 N6 O16, 2(C42 H46 Fe N2 O9), 4(C H Cl3), 2(Cl) ; _chemical_compound_source . _chemical_formula_weight 3291.00 _cell_measurement_reflns_used 7358 _cell_measurement_theta_min 3.1856 _cell_measurement_theta_max 73.6431 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.032 _exptl_crystal_size_mid 0.053 _exptl_crystal_size_max 0.071 _exptl_crystal_density_diffrn 1.393 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 4.314 # Sheldrick geometric approximatio 0.80 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.87 _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _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 150 _diffrn_reflns_number 55569 _reflns_number_total 30672 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections without Friedels Law is 0 # Number of reflections with Friedels Law is 30672 # Theoretical number of reflections is about 63521 _diffrn_reflns_theta_min 3.188 _diffrn_reflns_theta_max 73.806 _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 68.639 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -19 _reflns_limit_h_max 19 _reflns_limit_k_min -23 _reflns_limit_k_max 22 _reflns_limit_l_min 0 _reflns_limit_l_max 35 _oxford_diffrn_Wilson_B_factor 3.67 _oxford_diffrn_Wilson_scale 0.54 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.73 _refine_diff_density_max 3.45 # 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>-3.0\s(I) _refine_ls_number_reflns 30531 _refine_ls_number_restraints 249 _refine_ls_number_parameters 1984 _oxford_refine_ls_R_factor_ref 0.1311 _refine_ls_wR_factor_ref 0.1707 _refine_ls_goodness_of_fit_ref 0.9936 _refine_ls_shift/su_max 0.0006841 _refine_ls_shift/su_mean 0.0000247 # The values computed from all data _oxford_reflns_number_all 30547 _refine_ls_R_factor_all 0.1313 _refine_ls_wR_factor_all 0.1713 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 17212 _refine_ls_R_factor_gt 0.0813 _refine_ls_wR_factor_gt 0.1301 # 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: 0.110E+04 0.161E+04 813. 204. ; # Insert your own references if required - in alphabetical order _publ_section_references ; Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst. 40, 786-790. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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. 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 Cl1 Cl 0.54935(9) 0.22432(8) 0.62784(5) 0.0391 1.0000 Uani . . . . . . . C2 C 0.7249(4) 0.5083(3) 0.4753(2) 0.0375 1.0000 Uani . . . . . . . N3 N 0.6891(3) 0.4469(2) 0.49983(15) 0.0287 1.0000 Uani . . . . . . . C4 C 0.6055(3) 0.4361(3) 0.50675(19) 0.0306 1.0000 Uani . . . . . . . C5 C 0.5726(3) 0.3795(3) 0.53074(19) 0.0299 1.0000 Uani . . . . . . . C6 C 0.6280(3) 0.3361(3) 0.5477(2) 0.0318 1.0000 Uani . . . . . . . C7 C 0.7135(3) 0.3485(3) 0.5392(2) 0.0317 1.0000 Uani . . . . . . . C8 C 0.7427(3) 0.4042(3) 0.51483(19) 0.0318 1.0000 Uani . . . . . . . C9 C 0.4770(4) 0.3711(3) 0.5359(2) 0.0350 1.0000 Uani . . . . . . . O10 O 0.4312(3) 0.4076(2) 0.51549(16) 0.0446 1.0000 Uani . . . . . . . N11 N 0.4489(3) 0.3227(3) 0.56372(18) 0.0387 1.0000 Uani . . . . . . . C12 C 0.3610(4) 0.3107(4) 0.5758(2) 0.0428 1.0000 Uani . . . . . . . C13 C 0.3674(4) 0.3505(4) 0.6261(2) 0.0466 1.0000 Uani . . . . . . . O14 O 0.3856(3) 0.4280(2) 0.62643(16) 0.0461 1.0000 Uani . . . . . . . C15 C 0.4022(4) 0.4754(4) 0.6706(2) 0.0427 1.0000 Uani . . . . . . . C16 C 0.4112(4) 0.5498(4) 0.6697(2) 0.0428 1.0000 Uani . . . . . . . C17 C 0.4273(4) 0.6021(4) 0.7121(2) 0.0437 1.0000 Uani . . . . . . . C18 C 0.4362(4) 0.5780(4) 0.7569(2) 0.0439 1.0000 Uani . . . . . . . C19 C 0.4275(5) 0.5040(4) 0.7577(2) 0.0511 1.0000 Uani . . . . . . . C20 C 0.4095(5) 0.4513(4) 0.7151(2) 0.0513 1.0000 Uani . . . . . . . O21 O 0.4549(3) 0.6247(3) 0.80119(16) 0.0533 1.0000 Uani . . . . . . . C22 C 0.4544(5) 0.6999(4) 0.8013(2) 0.0492 1.0000 Uani . . . . . . . C23 C 0.4811(5) 0.7414(4) 0.8528(3) 0.0536 1.0000 Uani . . . . . . . O24 O 0.4051(3) 0.7302(3) 0.87456(16) 0.0533 1.0000 Uani . . . . . . . C25 C 0.4278(5) 0.7772(4) 0.9220(3) 0.0632 1.0000 Uani D . . . . . . C26 C 0.3512(5) 0.7517(5) 0.9464(3) 0.0677 1.0000 Uani D . . . . . . C27 C 0.7787(4) 0.3026(3) 0.5532(2) 0.0387 1.0000 Uani . . . . . . . O28 O 0.8431(3) 0.3063(3) 0.5340(2) 0.0671 1.0000 Uani . . . . . . . N29 N 0.7615(3) 0.2577(3) 0.58471(19) 0.0422 1.0000 Uani . . . . . . . C30 C 0.8248(5) 0.2143(4) 0.6012(3) 0.0531 1.0000 Uani . . . . . . . C31 C 0.8504(4) 0.2292(4) 0.6563(3) 0.0523 1.0000 Uani . . . . . . . O32 O 0.7718(3) 0.2007(3) 0.67260(17) 0.0533 1.0000 Uani . . . . . . . C33 C 0.7717(4) 0.2180(4) 0.7217(2) 0.0453 1.0000 Uani . . . . . . . C34 C 0.8437(4) 0.2596(4) 0.7567(3) 0.0525 1.0000 Uani . . . . . . . C35 C 0.8353(4) 0.2740(4) 0.8050(3) 0.0557 1.0000 Uani . . . . . . . C36 C 0.7561(5) 0.2464(4) 0.8178(3) 0.0500 1.0000 Uani . . . . . . . C37 C 0.6839(5) 0.2053(4) 0.7830(3) 0.0514 1.0000 Uani . . . . . . . C38 C 0.6918(5) 0.1907(4) 0.7347(3) 0.0504 1.0000 Uani . . . . . . . O39 O 0.7554(4) 0.2630(3) 0.86712(19) 0.0656 1.0000 Uani . . . . . . . C40 C 0.6722(5) 0.2385(5) 0.8812(3) 0.0664 1.0000 Uani . . . . . . . C41 C 0.6864(6) 0.2579(5) 0.9350(3) 0.0757 1.0000 Uani . . . . . . . O42 O 0.7368(4) 0.2062(3) 0.95271(19) 0.0757 1.0000 Uani . . . . . . . C43 C 0.7565(7) 0.2212(6) 1.0036(3) 0.0880 1.0000 Uani . . . . . . . C44 C 0.6801(6) 0.1961(5) 1.0276(3) 0.0718 1.0000 Uani . . . . . . . Fe101 Fe 0.07096(8) 0.05292(6) 0.77710(5) 0.0583 1.0000 Uani . . . . . . . C102 C 0.0979(8) -0.0473(5) 0.7732(4) 0.1189 1.0000 Uani D U . . . . . C103 C 0.0259(6) -0.0446(5) 0.7978(4) 0.1177 1.0000 Uani D U . . . . . C104 C 0.0599(7) 0.0103(6) 0.8399(4) 0.1101 1.0000 Uani D U . . . . . C105 C 0.1498(6) 0.0400(5) 0.8421(3) 0.1075 1.0000 Uani D U . . . . . C106 C 0.1715(6) 0.0040(5) 0.8014(4) 0.0964 1.0000 Uani D U . . . . . C107 C 0.0355(4) 0.0767(4) 0.7100(3) 0.0549 1.0000 Uani . . . . . . . C108 C -0.0295(5) 0.0855(4) 0.7376(3) 0.0594 1.0000 Uani . . . . . . . C109 C 0.0112(4) 0.1386(4) 0.7800(3) 0.0516 1.0000 Uani . . . . . . . C110 C 0.1026(4) 0.1643(3) 0.7792(2) 0.0452 1.0000 Uani . . . . . . . C111 C 0.1184(4) 0.1258(3) 0.7351(2) 0.0394 1.0000 Uani . . . . . . . C112 C 0.2038(4) 0.1386(3) 0.7181(2) 0.0345 1.0000 Uani . . . . . . . C113 C 0.2779(4) 0.1934(3) 0.7449(2) 0.0363 1.0000 Uani . . . . . . . C114 C 0.3559(4) 0.2100(3) 0.72734(19) 0.0312 1.0000 Uani . . . . . . . C115 C 0.3612(4) 0.1713(3) 0.6826(2) 0.0328 1.0000 Uani . . . . . . . C116 C 0.2887(4) 0.1157(3) 0.6557(2) 0.0329 1.0000 Uani . . . . . . . C117 C 0.2112(4) 0.0991(3) 0.6737(2) 0.0338 1.0000 Uani . . . . . . . C118 C 0.4316(4) 0.2709(3) 0.7581(2) 0.0349 1.0000 Uani . . . . . . . O119 O 0.4273(3) 0.3003(3) 0.79951(16) 0.0534 1.0000 Uani . . . . . . . N120 N 0.5036(3) 0.2928(2) 0.74015(16) 0.0312 1.0000 Uani . . . . . . . C121 C 0.5779(4) 0.3521(3) 0.7688(2) 0.0339 1.0000 Uani . . . . . . . C122 C 0.6500(4) 0.3724(3) 0.7405(2) 0.0349 1.0000 Uani . . . . . . . O123 O 0.6156(2) 0.4111(2) 0.70422(14) 0.0342 1.0000 Uani . . . . . . . C124 C 0.6761(3) 0.4418(3) 0.67818(19) 0.0294 1.0000 Uani . . . . . . . C125 C 0.6496(4) 0.4901(3) 0.6487(2) 0.0334 1.0000 Uani . . . . . . . C126 C 0.7065(4) 0.5258(3) 0.6227(2) 0.0332 1.0000 Uani . . . . . . . C127 C 0.7908(3) 0.5135(3) 0.6255(2) 0.0314 1.0000 Uani . . . . . . . C128 C 0.8177(3) 0.4637(3) 0.6536(2) 0.0324 1.0000 Uani . . . . . . . C129 C 0.7592(4) 0.4282(3) 0.6802(2) 0.0336 1.0000 Uani . . . . . . . O130 O 0.8444(2) 0.5530(2) 0.59902(14) 0.0340 1.0000 Uani . . . . . . . C131 C 0.9317(4) 0.5404(3) 0.6015(2) 0.0364 1.0000 Uani . . . . . . . C132 C 0.9810(4) 0.5936(3) 0.5744(2) 0.0370 1.0000 Uani . . . . . . . O133 O 0.9343(2) 0.5805(2) 0.52548(13) 0.0356 1.0000 Uani . . . . . . . C134 C 0.9871(4) 0.6197(3) 0.4965(2) 0.0398 1.0000 Uani . . . . . . . C135 C 0.9295(4) 0.6195(3) 0.4487(2) 0.0412 1.0000 Uani . . . . . . . O136 O 0.9038(2) 0.5451(2) 0.42155(14) 0.0372 1.0000 Uani . . . . . . . C137 C 0.8361(4) 0.5373(3) 0.3798(2) 0.0391 1.0000 Uani . . . . . . . C138 C 0.8147(4) 0.4586(3) 0.3526(2) 0.0379 1.0000 Uani . . . . . . . O139 O 0.7791(3) 0.4108(2) 0.38354(14) 0.0373 1.0000 Uani . . . . . . . C140 C 0.7638(4) 0.3344(3) 0.3613(2) 0.0396 1.0000 Uani . . . . . . . C141 C 0.7251(4) 0.2859(3) 0.3940(2) 0.0366 1.0000 Uani . . . . . . . O142 O 0.6360(3) 0.2939(2) 0.39331(15) 0.0402 1.0000 Uani . . . . . . . C143 C 0.5873(4) 0.2504(3) 0.4201(2) 0.0349 1.0000 Uani . . . . . . . C144 C 0.5011(4) 0.2596(3) 0.4184(2) 0.0399 1.0000 Uani . . . . . . . C145 C 0.4469(4) 0.2213(3) 0.4445(2) 0.0376 1.0000 Uani . . . . . . . C146 C 0.4781(4) 0.1730(3) 0.4727(2) 0.0334 1.0000 Uani . . . . . . . C147 C 0.5633(4) 0.1627(3) 0.4742(2) 0.0349 1.0000 Uani . . . . . . . C148 C 0.6177(4) 0.2023(3) 0.4470(2) 0.0345 1.0000 Uani . . . . . . . O149 O 0.4184(3) 0.1377(2) 0.49797(15) 0.0392 1.0000 Uani . . . . . . . C150 C 0.4441(4) 0.0811(3) 0.5218(2) 0.0406 1.0000 Uani . . . . . . . C151 C 0.3669(4) 0.0445(3) 0.5429(2) 0.0410 1.0000 Uani . . . . . . . N152 N 0.3591(3) 0.0921(2) 0.58623(16) 0.0344 1.0000 Uani . . . . . . . C153 C 0.2896(4) 0.0713(3) 0.6077(2) 0.0352 1.0000 Uani . . . . . . . O154 O 0.2284(3) 0.0164(2) 0.58792(15) 0.0472 1.0000 Uani . . . . . . . Cl155 Cl -0.05320(10) 0.77741(8) 0.86581(5) 0.0409 1.0000 Uani . . . . . . . C202 C -0.2251(4) 0.5007(3) 1.0231(2) 0.0414 1.0000 Uani . . . . . . . N203 N -0.1899(3) 0.5566(2) 0.99446(16) 0.0304 1.0000 Uani . . . . . . . C204 C -0.2389(4) 0.6030(3) 0.98066(19) 0.0331 1.0000 Uani . . . . . . . C205 C -0.2085(3) 0.6567(3) 0.95449(19) 0.0299 1.0000 Uani . . . . . . . C206 C -0.1254(3) 0.6605(3) 0.9428(2) 0.0313 1.0000 Uani . . . . . . . C207 C -0.0764(3) 0.6115(3) 0.9566(2) 0.0316 1.0000 Uani . . . . . . . C208 C -0.1094(3) 0.5601(3) 0.9837(2) 0.0308 1.0000 Uani . . . . . . . O210 O -0.3334(3) 0.7072(3) 0.95855(17) 0.0529 1.0000 Uani . . . . . . . N211 N -0.2356(3) 0.7586(3) 0.91541(17) 0.0414 1.0000 Uani . . . . . . . C212 C -0.2781(5) 0.8181(4) 0.9039(2) 0.0501 1.0000 Uani . . . . . . . C213 C -0.2660(5) 0.8337(4) 0.8532(2) 0.0497 1.0000 Uani . . . . . . . O214 O -0.3151(3) 0.7697(3) 0.81931(15) 0.0519 1.0000 Uani . . . . . . . C215 C -0.2983(4) 0.7656(4) 0.7723(2) 0.0426 1.0000 Uani . . . . . . . C216 C -0.2386(5) 0.8155(4) 0.7571(2) 0.0541 1.0000 Uani . . . . . . . C217 C -0.2263(5) 0.8015(4) 0.7086(3) 0.0606 1.0000 Uani . . . . . . . C218 C -0.2778(5) 0.7373(4) 0.6773(2) 0.0513 1.0000 Uani . . . . . . . C219 C -0.3397(5) 0.6884(4) 0.6928(2) 0.0526 1.0000 Uani . . . . . . . C220 C -0.3510(4) 0.7011(4) 0.7400(2) 0.0464 1.0000 Uani . . . . . . . O221 O -0.2705(4) 0.7172(3) 0.62915(17) 0.0649 1.0000 Uani . . . . . . . C222 C -0.2028(6) 0.7603(5) 0.6121(3) 0.0710 1.0000 Uani . . . . . . . C223 C -0.2101(6) 0.7201(5) 0.5603(3) 0.0734 1.0000 Uani . . . . . . . O224 O -0.1625(4) 0.7600(3) 0.5327(2) 0.0799 1.0000 Uani . . . . . . . C225 C -0.1949(6) 0.8220(4) 0.5194(3) 0.0640 1.0000 Uani . . . . . . . C226 C -0.1468(5) 0.8509(4) 0.4826(2) 0.0544 1.0000 Uani . . . . . . . C227 C 0.0141(4) 0.6104(3) 0.9453(2) 0.0394 1.0000 Uani . . . . . . . O228 O 0.0599(3) 0.5737(3) 0.96620(18) 0.0532 1.0000 Uani . . . . . . . N229 N 0.0384(3) 0.6517(3) 0.9127(2) 0.0435 1.0000 Uani . . . . . . . C230 C 0.4439(7) 0.9791(6) 0.6717(4) 0.0822 1.0000 Uani . . . . . . . C231 C 0.3590(7) 0.9476(6) 0.6713(4) 0.0892 1.0000 Uani . . . . . . . O232 O 0.0870(3) 0.5330(2) 0.84715(18) 0.0516 1.0000 Uani . . . . . . . C233 C 0.5044(4) 0.8495(4) 0.7282(3) 0.0484 1.0000 Uani . . . . . . . C234 C 0.5442(4) 0.9032(4) 0.7712(3) 0.0555 1.0000 Uani . . . . . . . C235 C 0.4779(4) 0.9086(4) 0.7995(2) 0.0500 1.0000 Uani . . . . . . . C236 C 0.3960(4) 0.8567(3) 0.7743(2) 0.0390 1.0000 Uani . . . . . . . C237 C 0.3112(4) 0.8431(3) 0.7908(2) 0.0352 1.0000 Uani . . . . . . . C238 C 0.0560(5) 0.5003(4) 0.7579(3) 0.0548 1.0000 Uani . . . . . . . O239 O 0.0553(3) 0.3290(3) 0.67900(17) 0.0506 1.0000 Uani . . . . . . . C240 C 0.1495(4) 0.8148(3) 0.8229(2) 0.0345 1.0000 Uani . . . . . . . C241 C 0.2231(4) 0.8678(3) 0.8515(2) 0.0351 1.0000 Uani . . . . . . . O242 O 0.0250(3) 0.1951(3) 0.60704(18) 0.0652 1.0000 Uani . . . . . . . C243 C 0.0782(4) 0.7188(3) 0.7450(2) 0.0334 1.0000 Uani . . . . . . . C244 C -0.0790(4) 0.6546(3) 0.7275(2) 0.0350 1.0000 Uani . . . . . . . Fe301 Fe 0.43879(6) 0.93286(6) 0.73258(4) 0.0438 1.0000 Uani . . . . . . . C302 C 0.3384(7) 0.9794(6) 0.7108(5) 0.0923 1.0000 Uani . . . . . . . C303 C 0.1059(5) 0.6101(4) 0.8442(3) 0.0533 1.0000 Uani . . . . . . . C304 C 0.1215(4) 0.6542(4) 0.8948(3) 0.0476 1.0000 Uani . . . . . . . C305 C 0.4837(7) 1.0316(5) 0.7134(4) 0.0906 1.0000 Uani . . . . . . . C306 C 0.4138(12) 1.0346(6) 0.7417(4) 0.1218 1.0000 Uani . . . . . . . C307 C 0.4142(4) 0.8210(3) 0.7300(2) 0.0426 1.0000 Uani . . . . . . . C308 C 0.0764(4) 0.4830(4) 0.8047(3) 0.0480 1.0000 Uani . . . . . . . C309 C 0.0863(4) 0.4128(4) 0.8089(3) 0.0458 1.0000 Uani . . . . . . . C310 C 0.0795(4) 0.3596(4) 0.7681(2) 0.0472 1.0000 Uani . . . . . . . C311 C 0.0609(4) 0.3775(4) 0.7217(2) 0.0441 1.0000 Uani . . . . . . . C312 C 0.0479(4) 0.4470(4) 0.7177(3) 0.0532 1.0000 Uani . . . . . . . C313 C 0.3029(4) 0.8808(3) 0.8354(2) 0.0388 1.0000 Uani . . . . . . . C314 C 0.1099(5) 0.2383(4) 0.6331(3) 0.0576 1.0000 Uani . . . . . . . C315 C 0.0999(5) 0.2715(4) 0.6833(3) 0.0590 1.0000 Uani . . . . . . . C316 C 0.1554(4) 0.7757(3) 0.7781(2) 0.0309 1.0000 Uani . . . . . . . C317 C 0.2352(4) 0.7897(3) 0.7625(2) 0.0351 1.0000 Uani . . . . . . . C318 C 0.2192(4) 0.9155(3) 0.8980(2) 0.0432 1.0000 Uani . . . . . . . O319 O 0.2830(3) 0.9670(3) 0.91956(16) 0.0586 1.0000 Uani . . . . . . . N320 N 0.1440(3) 0.8998(3) 0.91521(17) 0.0395 1.0000 Uani . . . . . . . C321 C 0.1326(5) 0.9500(3) 0.9565(2) 0.0470 1.0000 Uani . . . . . . . C322 C 0.0523(5) 0.9165(3) 0.9760(2) 0.0444 1.0000 Uani . . . . . . . O323 O 0.0742(3) 0.8580(2) 0.99947(14) 0.0404 1.0000 Uani . . . . . . . C324 C 0.0124(4) 0.8225(3) 1.0233(2) 0.0348 1.0000 Uani . . . . . . . C325 C 0.0399(4) 0.7703(3) 1.0490(2) 0.0362 1.0000 Uani . . . . . . . C326 C -0.0169(4) 0.7322(3) 1.0743(2) 0.0379 1.0000 Uani . . . . . . . C327 C -0.1000(4) 0.7460(3) 1.0746(2) 0.0349 1.0000 Uani . . . . . . . C328 C -0.1272(4) 0.7986(3) 1.0497(2) 0.0370 1.0000 Uani . . . . . . . C329 C -0.0702(4) 0.8371(3) 1.0237(2) 0.0358 1.0000 Uani . . . . . . . O330 O -0.1501(3) 0.7038(2) 1.10108(15) 0.0429 1.0000 Uani D . . . . . . C331 C -0.2377(4) 0.7145(3) 1.1012(2) 0.0415 1.0000 Uani D . . . . . . C332 C -0.2780(4) 0.6651(4) 1.1342(2) 0.0446 1.0000 Uani D . . . . . . O333 O -0.2897(3) 0.58916(18) 1.11255(14) 0.0433 1.0000 Uani D . . . . . . C334 C -0.3273(3) 0.5377(2) 1.14080(11) 0.0480 1.0000 Uani D . . . . . . C335 C -0.3232(3) 0.4617(2) 1.12441(11) 0.0504 0.649(11) Uani D U P . 1 . . O336 O -0.3493(4) 0.4291(4) 1.07198(12) 0.0504 0.649(11) Uani D U P . 1 . . C337 C -0.4463(4) 0.4197(4) 1.05733(14) 0.0442 0.649(11) Uani D U P . 1 . . C338 C -0.4689(4) 0.3872(4) 0.99840(14) 0.0490 0.649(11) Uani D U P . 1 . . O339 O -0.4343(3) 0.4254(2) 0.97524(13) 0.0473 1.0000 Uani D U . . . . . C340 C -0.4703(4) 0.3977(3) 0.9245(2) 0.0394 1.0000 Uani D . . . . . . C341 C -0.4240(4) 0.4499(4) 0.89518(19) 0.0386 1.0000 Uani D . . . . . . O342 O -0.3348(2) 0.4412(2) 0.89787(14) 0.0369 1.0000 Uani D . . . . . . C343 C -0.2852(3) 0.4809(3) 0.8700(2) 0.0324 1.0000 Uani . . . . . . . C344 C -0.2045(4) 0.4637(3) 0.8668(2) 0.0334 1.0000 Uani . . . . . . . C345 C -0.1485(3) 0.5002(3) 0.8400(2) 0.0337 1.0000 Uani . . . . . . . C346 C -0.1752(3) 0.5535(3) 0.81547(19) 0.0306 1.0000 Uani . . . . . . . C347 C -0.2560(4) 0.5709(3) 0.8181(2) 0.0340 1.0000 Uani . . . . . . . C348 C -0.3112(4) 0.5343(3) 0.8455(2) 0.0345 1.0000 Uani . . . . . . . O349 O -0.1170(2) 0.5860(2) 0.78848(14) 0.0346 1.0000 Uani . . . . . . . C350 C -0.1500(4) 0.6308(3) 0.7555(2) 0.0342 1.0000 Uani . . . . . . . C351 C 0.0805(6) 0.1727(5) 0.5325(3) 0.0668 1.0000 Uani . . . . . . . N352 N -0.0013(3) 0.7077(3) 0.75813(17) 0.0336 1.0000 Uani . . . . . . . C353 C 0.0290(6) 0.1402(5) 0.5668(3) 0.0670 1.0000 Uani . . . . . . . O354 O 0.0875(3) 0.6827(3) 0.70714(16) 0.0518 1.0000 Uani . . . . . . . C501 C 0.1121(5) 0.8792(4) 0.6051(3) 0.0539 1.0000 Uani . U . . . . . Cl502 Cl 0.12430(13) 0.82738(11) 0.55016(8) 0.0669 1.0000 Uani . U . . . . . Cl503 Cl 0.01705(13) 0.91469(12) 0.59678(9) 0.0762 1.0000 Uani . U . . . . . Cl504 Cl 0.10841(16) 0.82226(12) 0.64896(9) 0.0796 1.0000 Uani . U . . . . . C505 C 0.7299(5) 1.0229(5) 0.6435(3) 0.0692 0.553(14) Uani D U P . 3 . . Cl506 Cl 0.8138(6) 1.0041(4) 0.6130(4) 0.1560 0.553(14) Uani D U P . 3 . . Cl507 Cl 0.6310(6) 1.0124(10) 0.6005(3) 0.1919 0.553(14) Uani D U P . 3 . . Cl508 Cl 0.7095(7) 0.9576(6) 0.6820(4) 0.1978 0.553(14) Uani D U P . 3 . . C509 C 0.7804(8) 1.0579(6) 0.8958(4) 0.0643 0.778(8) Uani . U P 1 1 . . Cl510 Cl 0.7550(4) 1.0671(2) 0.83468(16) 0.1333 0.778(8) Uani . U P 1 1 . . Cl511 Cl 0.6883(2) 1.01027(18) 0.91384(16) 0.0890 0.778(8) Uani . U P 1 1 . . Cl512 Cl 0.8646(2) 1.0081(3) 0.90208(14) 0.0763 0.778(8) Uani . U P 1 1 . . C513 C 0.6023(5) 0.8857(4) 1.0899(3) 0.0626 1.0000 Uani . U . . . . . Cl514 Cl 0.61871(14) 0.83057(12) 1.03769(8) 0.0741 1.0000 Uani . U . . . . . C514 C -0.2659(4) 0.7093(3) 0.9424(2) 0.0379 1.0000 Uani . . . . . . . Cl515 Cl 0.50264(15) 0.91453(15) 1.07830(12) 0.1026 1.0000 Uani . U . . . . . Cl516 Cl 0.60194(16) 0.83485(13) 1.13707(9) 0.0817 1.0000 Uani . U . . . . . C517 C 0.6952(4) 0.9751(3) 0.6206(2) 0.1261 0.447(14) Uani D U P . 4 . . Cl518 Cl 0.6352(4) 1.0412(3) 0.6055(2) 0.0683 0.447(14) Uani D U P . 4 . . Cl519 Cl 0.8040(4) 1.0041(3) 0.6108(2) 0.1096 0.447(14) Uani D U P . 4 . . Cl520 Cl 0.6985(4) 0.9701(3) 0.6825(2) 0.1605 0.447(14) Uani D U P . 4 . . C521 C 0.817(5) 1.069(4) 0.866(3) 0.1354 0.222(8) Uani . U P 1 2 . . Cl522 Cl 0.7874(9) 1.0440(8) 0.8037(7) 0.1150 0.222(8) Uani . U P 1 2 . . Cl523 Cl 0.7095(14) 1.0423(11) 0.8867(8) 0.1444 0.222(8) Uani . U P 1 2 . . Cl524 Cl 0.8864(16) 1.0155(14) 0.8863(9) 0.1391 0.222(8) Uani . U P 1 2 . . C635 C -0.3232(3) 0.4617(2) 1.12441(11) 0.0504 0.351(11) Uani D U P . 2 . . O636 O -0.3755(5) 0.4361(2) 1.07418(12) 0.0496 0.351(11) Uani D U P . 2 . . C637 C -0.4686(5) 0.3926(2) 1.05666(12) 0.0492 0.351(11) Uani D U P . 2 . . C638 C -0.4890(5) 0.3813(2) 1.00701(12) 0.0490 0.351(11) Uani D U P . 2 . . H21 H 0.7582 0.4921 0.4524 0.0604 1.0000 Uiso R . . . . . . H22 H 0.7631 0.5502 0.4993 0.0604 1.0000 Uiso R . . . . . . H23 H 0.6771 0.5254 0.4585 0.0598 1.0000 Uiso R . . . . . . H41 H 0.5701 0.4664 0.4944 0.0392 1.0000 Uiso R . . . . . . H61 H 0.6080 0.2979 0.5643 0.0420 1.0000 Uiso R . . . . . . H81 H 0.7997 0.4131 0.5090 0.0412 1.0000 Uiso R . . . . . . H121 H 0.3371 0.2578 0.5741 0.0535 1.0000 Uiso R . . . . . . H122 H 0.3213 0.3286 0.5526 0.0541 1.0000 Uiso R . . . . . . H131 H 0.4155 0.3398 0.6491 0.0569 1.0000 Uiso R . . . . . . H132 H 0.3110 0.3336 0.6371 0.0567 1.0000 Uiso R . . . . . . H161 H 0.4066 0.5660 0.6399 0.0546 1.0000 Uiso R . . . . . . H171 H 0.4329 0.6526 0.7108 0.0558 1.0000 Uiso R . . . . . . H191 H 0.4346 0.4884 0.7875 0.0623 1.0000 Uiso R . . . . . . H201 H 0.4024 0.3998 0.7159 0.0643 1.0000 Uiso R . . . . . . H221 H 0.4963 0.7208 0.7816 0.0583 1.0000 Uiso R . . . . . . H222 H 0.3931 0.7021 0.7885 0.0578 1.0000 Uiso R . . . . . . H232 H 0.5014 0.7955 0.8543 0.0650 1.0000 Uiso R . . . . . . H231 H 0.5281 0.7224 0.8708 0.0649 1.0000 Uiso R . . . . . . H252 H 0.4797 0.7656 0.9407 0.0730 1.0000 Uiso R . . . . . . H251 H 0.4426 0.8309 0.9202 0.0728 1.0000 Uiso R . . . . . . H261 H 0.3233 0.7005 0.9428 0.0805 1.0000 Uiso R . . . . . . H301 H 0.8780 0.2260 0.5875 0.0669 1.0000 Uiso R . . . . . . H302 H 0.7958 0.1612 0.5898 0.0668 1.0000 Uiso R . . . . . . H311 H 0.8953 0.2028 0.6662 0.0669 1.0000 Uiso R . . . . . . H312 H 0.8727 0.2822 0.6692 0.0670 1.0000 Uiso R . . . . . . H341 H 0.8980 0.2777 0.7483 0.0650 1.0000 Uiso R . . . . . . H351 H 0.8832 0.3030 0.8286 0.0697 1.0000 Uiso R . . . . . . H371 H 0.6295 0.1882 0.7912 0.0655 1.0000 Uiso R . . . . . . H381 H 0.6433 0.1625 0.7114 0.0603 1.0000 Uiso R . . . . . . H401 H 0.6521 0.1840 0.8710 0.0801 1.0000 Uiso R . . . . . . H402 H 0.6277 0.2619 0.8661 0.0800 1.0000 Uiso R . . . . . . H411 H 0.7214 0.3089 0.9479 0.0882 1.0000 Uiso R . . . . . . H412 H 0.6306 0.2503 0.9470 0.0889 1.0000 Uiso R . . . . . . H431 H 0.8043 0.1987 1.0157 0.1111 1.0000 Uiso R . . . . . . H432 H 0.7750 0.2760 1.0119 0.1110 1.0000 Uiso R . . . . . . H441 H 0.6527 0.1459 1.0239 0.0879 1.0000 Uiso R . . . . . . H1021 H 0.1018 -0.0792 0.7437 0.1479 1.0000 Uiso R . . . . . . H1031 H -0.0338 -0.0762 0.7880 0.1710 1.0000 Uiso R . . . . . . H1041 H 0.0261 0.0275 0.8633 0.1580 1.0000 Uiso R . . . . . . H1051 H 0.1896 0.0801 0.8683 0.1334 1.0000 Uiso R . . . . . . H1061 H 0.2317 0.0188 0.7947 0.0984 1.0000 Uiso R . . . . . . H1071 H 0.0250 0.0432 0.6783 0.0712 1.0000 Uiso R . . . . . . H1081 H -0.0920 0.0570 0.7296 0.0762 1.0000 Uiso R . . . . . . H1091 H -0.0180 0.1563 0.8060 0.0660 1.0000 Uiso R . . . . . . H1101 H 0.1484 0.1999 0.8045 0.0552 1.0000 Uiso R . . . . . . H1131 H 0.2743 0.2190 0.7752 0.0456 1.0000 Uiso R . . . . . . H1151 H 0.4132 0.1820 0.6700 0.0439 1.0000 Uiso R . . . . . . H1171 H 0.1629 0.0613 0.6557 0.0436 1.0000 Uiso R . . . . . . H1211 H 0.6026 0.3366 0.7978 0.0462 1.0000 Uiso R . . . . . . H1212 H 0.5564 0.3958 0.7781 0.0458 1.0000 Uiso R . . . . . . H1222 H 0.7031 0.4041 0.7622 0.0438 1.0000 Uiso R . . . . . . H1221 H 0.6640 0.3269 0.7253 0.0440 1.0000 Uiso R . . . . . . H1251 H 0.5928 0.4988 0.6470 0.0432 1.0000 Uiso R . . . . . . H1261 H 0.6879 0.5589 0.6033 0.0422 1.0000 Uiso R . . . . . . H1281 H 0.8740 0.4539 0.6553 0.0411 1.0000 Uiso R . . . . . . H1291 H 0.7767 0.3944 0.6986 0.0410 1.0000 Uiso R . . . . . . H1311 H 0.9634 0.5520 0.6355 0.0461 1.0000 Uiso R . . . . . . H1312 H 0.9296 0.4887 0.5880 0.0455 1.0000 Uiso R . . . . . . H1321 H 0.9856 0.6448 0.5898 0.0471 1.0000 Uiso R . . . . . . H1322 H 1.0404 0.5848 0.5754 0.0468 1.0000 Uiso R . . . . . . H1342 H 1.0127 0.6712 0.5134 0.0538 1.0000 Uiso R . . . . . . H1341 H 1.0350 0.5954 0.4919 0.0542 1.0000 Uiso R . . . . . . H1351 H 0.9637 0.6526 0.4309 0.0529 1.0000 Uiso R . . . . . . H1352 H 0.8774 0.6377 0.4533 0.0532 1.0000 Uiso R . . . . . . H1371 H 0.8564 0.5710 0.3587 0.0485 1.0000 Uiso R . . . . . . H1372 H 0.7833 0.5484 0.3904 0.0479 1.0000 Uiso R . . . . . . H1382 H 0.8688 0.4464 0.3444 0.0490 1.0000 Uiso R . . . . . . H1381 H 0.7701 0.4538 0.3223 0.0491 1.0000 Uiso R . . . . . . H1402 H 0.8192 0.3236 0.3566 0.0495 1.0000 Uiso R . . . . . . H1401 H 0.7228 0.3257 0.3298 0.0493 1.0000 Uiso R . . . . . . H1411 H 0.7612 0.3013 0.4265 0.0468 1.0000 Uiso R . . . . . . H1412 H 0.7243 0.2341 0.3820 0.0470 1.0000 Uiso R . . . . . . H1441 H 0.4800 0.2914 0.3996 0.0533 1.0000 Uiso R . . . . . . H1451 H 0.3895 0.2289 0.4442 0.0486 1.0000 Uiso R . . . . . . H1471 H 0.5833 0.1300 0.4925 0.0454 1.0000 Uiso R . . . . . . H1481 H 0.6753 0.1973 0.4481 0.0447 1.0000 Uiso R . . . . . . H1502 H 0.4968 0.1015 0.5471 0.0490 1.0000 Uiso R . . . . . . H1501 H 0.4563 0.0449 0.4976 0.0489 1.0000 Uiso R . . . . . . H1511 H 0.3776 -0.0018 0.5512 0.0542 1.0000 Uiso R . . . . . . H1512 H 0.3117 0.0334 0.5186 0.0540 1.0000 Uiso R . . . . . . H2021 H -0.1813 0.4751 1.0332 0.0676 1.0000 Uiso R . . . . . . H2023 H -0.2408 0.5252 1.0513 0.0671 1.0000 Uiso R . . . . . . H2022 H -0.2777 0.4662 1.0036 0.0669 1.0000 Uiso R . . . . . . H2041 H -0.2939 0.5996 0.9889 0.0422 1.0000 Uiso R . . . . . . H2061 H -0.1040 0.6955 0.9250 0.0413 1.0000 Uiso R . . . . . . H2081 H -0.0755 0.5271 0.9939 0.0393 1.0000 Uiso R . . . . . . H2121 H -0.2515 0.8637 0.9286 0.0612 1.0000 Uiso R . . . . . . H2122 H -0.3407 0.8005 0.9028 0.0608 1.0000 Uiso R . . . . . . H2132 H -0.2905 0.8770 0.8465 0.0594 1.0000 Uiso R . . . . . . H2131 H -0.2027 0.8449 0.8515 0.0589 1.0000 Uiso R . . . . . . H2161 H -0.2058 0.8588 0.7785 0.0650 1.0000 Uiso R . . . . . . H2171 H -0.1842 0.8342 0.6979 0.0739 1.0000 Uiso R . . . . . . H2191 H -0.3752 0.6459 0.6708 0.0650 1.0000 Uiso R . . . . . . H2201 H -0.3939 0.6673 0.7509 0.0604 1.0000 Uiso R . . . . . . H2221 H -0.2130 0.8095 0.6111 0.0839 1.0000 Uiso R . . . . . . H2222 H -0.1445 0.7657 0.6318 0.0834 1.0000 Uiso R . . . . . . H2232 H -0.2724 0.7102 0.5435 0.0871 1.0000 Uiso R . . . . . . H2231 H -0.1903 0.6734 0.5621 0.0870 1.0000 Uiso R . . . . . . H2251 H -0.1874 0.8604 0.5480 0.0761 1.0000 Uiso R . . . . . . H2252 H -0.2589 0.8030 0.5052 0.0757 1.0000 Uiso R . . . . . . H2261 H -0.1636 0.8892 0.4689 0.0669 1.0000 Uiso R . . . . . . H2301 H 0.4760 0.9634 0.6464 0.0972 1.0000 Uiso R . . . . . . H2311 H 0.3196 0.9068 0.6461 0.1072 1.0000 Uiso R . . . . . . H2331 H 0.5348 0.8340 0.7027 0.0649 1.0000 Uiso R . . . . . . H2341 H 0.6064 0.9320 0.7797 0.0692 1.0000 Uiso R . . . . . . H2351 H 0.4865 0.9418 0.8305 0.0626 1.0000 Uiso R . . . . . . H2381 H 0.0483 0.5480 0.7542 0.0661 1.0000 Uiso R . . . . . . H2401 H 0.0959 0.8050 0.8336 0.0452 1.0000 Uiso R . . . . . . H2441 H -0.1037 0.6770 0.7009 0.0458 1.0000 Uiso R . . . . . . H2442 H -0.0595 0.6118 0.7140 0.0460 1.0000 Uiso R . . . . . . H3021 H 0.2791 0.9655 0.7191 0.1052 1.0000 Uiso R . . . . . . H3031 H 0.0563 0.6213 0.8235 0.0620 1.0000 Uiso R . . . . . . H3032 H 0.1585 0.6226 0.8305 0.0621 1.0000 Uiso R . . . . . . H3041 H 0.1597 0.6322 0.9163 0.0601 1.0000 Uiso R . . . . . . H3042 H 0.1503 0.7058 0.8954 0.0599 1.0000 Uiso R . . . . . . H3051 H 0.5448 1.0619 0.7218 0.1141 1.0000 Uiso R . . . . . . H3061 H 0.4150 1.0672 0.7714 0.1580 1.0000 Uiso R . . . . . . H3071 H 0.3702 0.7848 0.7042 0.0527 1.0000 Uiso R . . . . . . H3091 H 0.0980 0.4004 0.8395 0.0570 1.0000 Uiso R . . . . . . H3101 H 0.0861 0.3119 0.7712 0.0588 1.0000 Uiso R . . . . . . H3121 H 0.0336 0.4584 0.6863 0.0680 1.0000 Uiso R . . . . . . H3131 H 0.3525 0.9170 0.8549 0.0489 1.0000 Uiso R . . . . . . H3141 H 0.1510 0.2061 0.6370 0.0727 1.0000 Uiso R . . . . . . H3142 H 0.1320 0.2774 0.6155 0.0728 1.0000 Uiso R . . . . . . H3151 H 0.1586 0.2916 0.7047 0.0742 1.0000 Uiso R . . . . . . H3152 H 0.0642 0.2326 0.6970 0.0738 1.0000 Uiso R . . . . . . H3171 H 0.2391 0.7626 0.7327 0.0456 1.0000 Uiso R . . . . . . H3211 H 0.1854 0.9613 0.9820 0.0577 1.0000 Uiso R . . . . . . H3212 H 0.1241 0.9952 0.9454 0.0581 1.0000 Uiso R . . . . . . H3222 H 0.0406 0.9543 0.9995 0.0588 1.0000 Uiso R . . . . . . H3221 H 0.0003 0.8956 0.9498 0.0586 1.0000 Uiso R . . . . . . H3251 H 0.0965 0.7615 1.0493 0.0467 1.0000 Uiso R . . . . . . H3261 H 0.0004 0.6967 1.0912 0.0497 1.0000 Uiso R . . . . . . H3281 H -0.1833 0.8078 1.0499 0.0460 1.0000 Uiso R . . . . . . H3291 H -0.0872 0.8724 1.0067 0.0489 1.0000 Uiso R . . . . . . H3311 H -0.2349 0.7660 1.1141 0.0528 1.0000 Uiso R . . . . . . H3312 H -0.2742 0.7014 1.0687 0.0534 1.0000 Uiso R . . . . . . H3321 H -0.2383 0.6754 1.1660 0.0580 1.0000 Uiso R . . . . . . H3322 H -0.3353 0.6737 1.1384 0.0579 1.0000 Uiso R . . . . . . H3351 H -0.3616 0.4303 1.1409 0.0760 0.649(11) Uiso R . P . 1 . . H3352 H -0.2626 0.4574 1.1345 0.0758 0.649(11) Uiso R . P . 1 . . H3371 H -0.4776 0.3913 1.0777 0.0548 0.649(11) Uiso R . P . 1 . . H3372 H -0.4551 0.4688 1.0623 0.0550 0.649(11) Uiso R . P . 1 . . H3381 H -0.5321 0.3825 0.9882 0.0569 0.649(11) Uiso R . P . 1 . . H3382 H -0.4572 0.3375 0.9951 0.0569 0.649(11) Uiso R . P . 1 . . H3401 H -0.5327 0.3979 0.9186 0.0504 1.0000 Uiso R . . . . . . H3402 H -0.4635 0.3473 0.9146 0.0500 1.0000 Uiso R . . . . . . H3411 H -0.4226 0.5009 0.9094 0.0504 1.0000 Uiso R . . . . . . H3412 H -0.4552 0.4376 0.8616 0.0497 1.0000 Uiso R . . . . . . H3441 H -0.1873 0.4283 0.8838 0.0424 1.0000 Uiso R . . . . . . H3451 H -0.0943 0.4882 0.8380 0.0453 1.0000 Uiso R . . . . . . H3471 H -0.2730 0.6074 0.8021 0.0437 1.0000 Uiso R . . . . . . H3481 H -0.3662 0.5448 0.8467 0.0428 1.0000 Uiso R . . . . . . H3501 H -0.1620 0.6746 0.7736 0.0443 1.0000 Uiso R . . . . . . H3502 H -0.2052 0.6012 0.7337 0.0455 1.0000 Uiso R . . . . . . H3511 H 0.0657 0.2147 0.5209 0.0800 1.0000 Uiso R . . . . . . H3531 H 0.0584 0.1033 0.5799 0.0859 1.0000 Uiso R . . . . . . H3532 H -0.0318 0.1149 0.5502 0.0859 1.0000 Uiso R . . . . . . H5011 H 0.1642 0.9206 0.6163 0.0637 1.0000 Uiso R . . . . . . H5051 H 0.7483 1.0733 0.6628 0.0909 0.553(14) Uiso R . P . 3 . . H5091 H 0.8026 1.1081 0.9162 0.0750 0.778(8) Uiso R . P 1 1 . . H5131 H 0.6523 0.9295 1.1005 0.0760 1.0000 Uiso R . . . . . . H5171 H 0.6655 0.9261 0.6008 0.1450 0.447(14) Uiso R . P . 4 . . H5211 H 0.8462 1.1221 0.8782 0.2160 0.222(8) Uiso R . P 1 2 . . H6352 H -0.3413 0.4255 1.1446 0.0759 0.351(11) Uiso R . P . 2 . . H6351 H -0.2685 0.4546 1.1153 0.0760 0.351(11) Uiso R . P . 2 . . H6382 H -0.5430 0.3981 1.0082 0.0571 0.351(11) Uiso R . P . 2 . . H6381 H -0.5049 0.3287 0.9918 0.0571 0.351(11) Uiso R . P . 2 . . H3201 H 0.0987 0.8669 0.8987 0.0499 1.0000 Uiso R . . . . . . H291 H 0.7147 0.2570 0.5969 0.0528 1.0000 Uiso R . . . . . . H2111 H -0.1965 0.7499 0.8996 0.0528 1.0000 Uiso R . . . . . . H1521 H 0.4027 0.1292 0.6011 0.0436 1.0000 Uiso R . . . . . . H2291 H 0.0017 0.6751 0.8998 0.0552 1.0000 Uiso R . . . . . . H111 H 0.4869 0.3024 0.5786 0.0490 1.0000 Uiso R . . . . . . H1201 H 0.5092 0.2680 0.7129 0.0420 1.0000 Uiso R . . . . . . H3521 H -0.0067 0.7345 0.7844 0.0439 1.0000 Uiso R . . . . . . H3341 H -0.2916 0.5514 1.1728 0.0591 1.0000 Uiso R . . . . . . H3342 H -0.3862 0.5421 1.1419 0.0591 1.0000 Uiso R . . . . . . H6371 H -0.5242 0.3939 1.0653 0.0614 0.351(11) Uiso R . P . 2 . . H6372 H -0.4530 0.3479 1.0631 0.0614 0.351(11) Uiso R . P . 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 Cl1 0.0351(7) 0.0445(8) 0.0383(7) 0.0092(6) 0.0126(6) 0.0058(6) C2 0.033(3) 0.043(3) 0.044(3) 0.019(3) 0.017(3) 0.009(3) N3 0.024(2) 0.033(2) 0.031(2) 0.0076(19) 0.0124(18) 0.0045(18) C4 0.028(3) 0.035(3) 0.031(3) 0.006(2) 0.012(2) 0.011(2) C5 0.025(3) 0.034(3) 0.031(3) 0.003(2) 0.010(2) 0.005(2) C6 0.027(3) 0.032(3) 0.038(3) 0.007(2) 0.011(2) 0.006(2) C7 0.029(3) 0.032(3) 0.034(3) 0.003(2) 0.009(2) 0.007(2) C8 0.025(3) 0.038(3) 0.033(3) 0.006(2) 0.008(2) 0.009(2) C9 0.027(3) 0.037(3) 0.042(3) 0.006(3) 0.014(2) 0.005(2) O10 0.032(2) 0.048(2) 0.065(3) 0.027(2) 0.018(2) 0.0181(19) N11 0.028(2) 0.043(3) 0.052(3) 0.017(2) 0.018(2) 0.011(2) C12 0.028(3) 0.048(4) 0.056(4) 0.015(3) 0.018(3) 0.006(3) C13 0.040(3) 0.056(4) 0.055(4) 0.023(3) 0.023(3) 0.019(3) O14 0.055(3) 0.050(3) 0.047(3) 0.023(2) 0.021(2) 0.024(2) C15 0.034(3) 0.054(4) 0.054(4) 0.027(3) 0.016(3) 0.022(3) C16 0.035(3) 0.056(4) 0.042(3) 0.019(3) 0.008(3) 0.013(3) C17 0.038(3) 0.049(4) 0.050(4) 0.028(3) 0.011(3) 0.010(3) C18 0.046(4) 0.050(4) 0.042(3) 0.015(3) 0.016(3) 0.015(3) C19 0.062(4) 0.064(4) 0.045(4) 0.031(3) 0.026(3) 0.026(4) C20 0.071(5) 0.054(4) 0.047(4) 0.023(3) 0.030(3) 0.029(4) O21 0.066(3) 0.052(3) 0.047(3) 0.020(2) 0.016(2) 0.015(2) C22 0.059(4) 0.049(4) 0.045(4) 0.012(3) 0.016(3) 0.018(3) C23 0.058(4) 0.053(4) 0.055(4) 0.015(3) 0.022(3) 0.014(3) O24 0.057(3) 0.064(3) 0.045(3) 0.007(2) 0.022(2) 0.020(2) C25 0.062(5) 0.082(6) 0.046(4) 0.003(4) 0.015(4) 0.019(4) C26 0.057(5) 0.093(6) 0.056(5) 0.018(4) 0.016(4) 0.019(4) C27 0.035(3) 0.040(3) 0.051(4) 0.014(3) 0.018(3) 0.019(3) O28 0.050(3) 0.085(4) 0.099(4) 0.056(3) 0.046(3) 0.038(3) N29 0.038(3) 0.048(3) 0.051(3) 0.019(2) 0.018(2) 0.021(2) C30 0.058(4) 0.060(4) 0.061(4) 0.028(4) 0.026(3) 0.033(4) C31 0.049(4) 0.060(4) 0.061(4) 0.025(4) 0.022(3) 0.023(3) O32 0.052(3) 0.060(3) 0.053(3) 0.018(2) 0.020(2) 0.012(2) C33 0.045(4) 0.046(4) 0.055(4) 0.019(3) 0.018(3) 0.021(3) C34 0.037(3) 0.068(5) 0.061(4) 0.024(4) 0.016(3) 0.016(3) C35 0.039(4) 0.072(5) 0.056(4) 0.016(4) 0.012(3) 0.008(3) C36 0.058(4) 0.050(4) 0.053(4) 0.021(3) 0.025(3) 0.019(3) C37 0.050(4) 0.044(4) 0.069(5) 0.020(3) 0.027(4) 0.011(3) C38 0.048(4) 0.046(4) 0.058(4) 0.013(3) 0.021(3) 0.006(3) O39 0.070(3) 0.073(4) 0.061(3) 0.021(3) 0.029(3) 0.017(3) C40 0.069(5) 0.089(6) 0.069(5) 0.042(5) 0.039(4) 0.042(5) C41 0.082(6) 0.104(7) 0.071(5) 0.045(5) 0.035(5) 0.054(5) O42 0.082(4) 0.104(5) 0.056(3) 0.025(3) 0.023(3) 0.041(3) C43 0.108(7) 0.132(9) 0.052(5) 0.018(5) 0.038(5) 0.073(7) C44 0.090(6) 0.096(6) 0.046(4) 0.023(4) 0.024(4) 0.045(5) Fe101 0.0489(6) 0.0523(7) 0.0935(9) 0.0395(6) 0.0405(6) 0.0172(5) C102 0.145(7) 0.076(6) 0.162(9) 0.056(6) 0.049(6) 0.046(6) C103 0.129(5) 0.082(5) 0.165(8) 0.086(5) 0.049(5) 0.017(5) C104 0.115(7) 0.108(7) 0.143(8) 0.086(5) 0.056(6) 0.039(5) C105 0.091(7) 0.134(9) 0.127(9) 0.080(7) 0.030(5) 0.049(5) C106 0.115(5) 0.093(7) 0.143(10) 0.084(7) 0.076(7) 0.080(5) C107 0.033(3) 0.063(4) 0.061(4) 0.001(4) 0.012(3) 0.001(3) C108 0.039(4) 0.074(5) 0.068(5) 0.014(4) 0.019(3) 0.011(3) C109 0.044(4) 0.056(4) 0.067(5) 0.025(4) 0.028(3) 0.017(3) C110 0.047(4) 0.041(3) 0.053(4) 0.014(3) 0.024(3) 0.009(3) C111 0.038(3) 0.036(3) 0.050(4) 0.015(3) 0.018(3) 0.011(3) C112 0.035(3) 0.031(3) 0.043(3) 0.011(2) 0.018(3) 0.009(2) C113 0.040(3) 0.034(3) 0.038(3) 0.009(2) 0.016(3) 0.006(2) C114 0.031(3) 0.031(3) 0.032(3) 0.007(2) 0.013(2) 0.003(2) C115 0.036(3) 0.026(3) 0.040(3) 0.012(2) 0.016(2) 0.006(2) C116 0.038(3) 0.029(3) 0.033(3) 0.008(2) 0.011(2) 0.005(2) C117 0.031(3) 0.025(3) 0.047(3) 0.011(2) 0.012(2) 0.006(2) C118 0.036(3) 0.034(3) 0.037(3) 0.010(2) 0.017(2) 0.005(2) O119 0.050(3) 0.057(3) 0.044(3) -0.008(2) 0.027(2) -0.009(2) N120 0.029(2) 0.032(2) 0.032(2) 0.0044(19) 0.0116(19) 0.0038(19) C121 0.033(3) 0.038(3) 0.031(3) 0.005(2) 0.012(2) 0.004(2) C122 0.034(3) 0.036(3) 0.033(3) 0.006(2) 0.009(2) 0.003(2) O123 0.0283(19) 0.037(2) 0.038(2) 0.0108(17) 0.0118(16) 0.0030(16) C124 0.026(3) 0.029(3) 0.031(3) 0.002(2) 0.009(2) 0.001(2) C125 0.030(3) 0.036(3) 0.037(3) 0.006(2) 0.008(2) 0.011(2) C126 0.031(3) 0.034(3) 0.035(3) 0.004(2) 0.007(2) 0.011(2) C127 0.030(3) 0.032(3) 0.033(3) 0.006(2) 0.013(2) 0.005(2) C128 0.025(3) 0.039(3) 0.036(3) 0.010(2) 0.010(2) 0.009(2) C129 0.031(3) 0.033(3) 0.040(3) 0.012(2) 0.012(2) 0.008(2) O130 0.0290(19) 0.039(2) 0.041(2) 0.0158(17) 0.0159(17) 0.0102(16) C131 0.030(3) 0.046(3) 0.040(3) 0.015(3) 0.015(2) 0.013(3) C132 0.029(3) 0.046(3) 0.033(3) 0.009(3) 0.008(2) 0.000(2) O133 0.031(2) 0.041(2) 0.033(2) 0.0115(17) 0.0106(16) -0.0004(17) C134 0.038(3) 0.041(3) 0.039(3) 0.011(3) 0.019(3) -0.004(3) C135 0.045(3) 0.034(3) 0.047(4) 0.015(3) 0.018(3) 0.004(3) O136 0.034(2) 0.039(2) 0.039(2) 0.0081(18) 0.0085(17) 0.0094(17) C137 0.037(3) 0.047(3) 0.037(3) 0.014(3) 0.015(3) 0.007(3) C138 0.034(3) 0.047(3) 0.034(3) 0.012(3) 0.016(2) 0.004(3) O139 0.042(2) 0.037(2) 0.033(2) 0.0050(17) 0.0180(18) 0.0036(17) C140 0.042(3) 0.038(3) 0.038(3) -0.001(3) 0.019(3) 0.004(3) C141 0.036(3) 0.036(3) 0.041(3) 0.007(3) 0.013(3) 0.011(2) O142 0.037(2) 0.046(2) 0.045(2) 0.0175(19) 0.0207(18) 0.0103(18) C143 0.037(3) 0.034(3) 0.038(3) 0.008(2) 0.015(2) 0.009(2) C144 0.039(3) 0.041(3) 0.046(3) 0.017(3) 0.015(3) 0.012(3) C145 0.033(3) 0.041(3) 0.044(3) 0.012(3) 0.012(3) 0.014(3) C146 0.033(3) 0.033(3) 0.035(3) 0.006(2) 0.011(2) 0.006(2) C147 0.039(3) 0.031(3) 0.036(3) 0.006(2) 0.010(2) 0.010(2) C148 0.034(3) 0.038(3) 0.037(3) 0.009(2) 0.013(2) 0.014(2) O149 0.042(2) 0.041(2) 0.046(2) 0.0171(19) 0.0259(19) 0.0152(18) C150 0.050(4) 0.038(3) 0.042(3) 0.012(3) 0.019(3) 0.017(3) C151 0.058(4) 0.030(3) 0.039(3) 0.006(2) 0.020(3) 0.010(3) N152 0.041(3) 0.029(2) 0.033(2) 0.0043(19) 0.013(2) 0.006(2) C153 0.044(3) 0.033(3) 0.032(3) 0.009(2) 0.017(3) 0.007(3) O154 0.050(3) 0.040(2) 0.041(2) 0.0002(19) 0.013(2) -0.010(2) Cl155 0.0416(8) 0.0440(8) 0.0456(8) 0.0153(6) 0.0219(6) 0.0137(6) C202 0.035(3) 0.050(4) 0.045(3) 0.022(3) 0.018(3) 0.007(3) N203 0.027(2) 0.033(2) 0.030(2) 0.0056(19) 0.0096(18) 0.0023(19) C204 0.029(3) 0.039(3) 0.030(3) 0.002(2) 0.009(2) 0.006(2) C205 0.027(3) 0.034(3) 0.030(3) 0.003(2) 0.006(2) 0.012(2) C206 0.029(3) 0.029(3) 0.038(3) 0.007(2) 0.010(2) 0.008(2) C207 0.026(3) 0.033(3) 0.037(3) 0.008(2) 0.010(2) 0.007(2) C208 0.025(3) 0.031(3) 0.040(3) 0.010(2) 0.011(2) 0.009(2) O210 0.044(3) 0.070(3) 0.064(3) 0.027(2) 0.027(2) 0.032(2) N211 0.050(3) 0.051(3) 0.037(3) 0.018(2) 0.017(2) 0.028(3) C212 0.061(4) 0.059(4) 0.041(4) 0.014(3) 0.015(3) 0.031(3) C213 0.053(4) 0.051(4) 0.048(4) 0.014(3) 0.008(3) 0.017(3) O214 0.067(3) 0.051(3) 0.038(2) 0.008(2) 0.008(2) 0.019(2) C215 0.046(4) 0.047(4) 0.038(3) 0.008(3) 0.005(3) 0.020(3) C216 0.068(5) 0.050(4) 0.037(4) 0.002(3) 0.009(3) 0.005(3) C217 0.079(5) 0.061(5) 0.047(4) 0.016(4) 0.020(4) 0.017(4) C218 0.057(4) 0.065(5) 0.036(3) 0.001(3) 0.007(3) 0.031(4) C219 0.046(4) 0.061(4) 0.047(4) -0.001(3) 0.005(3) 0.018(3) C220 0.037(3) 0.055(4) 0.047(4) 0.004(3) 0.006(3) 0.016(3) O221 0.079(4) 0.074(4) 0.044(3) 0.002(2) 0.020(3) 0.022(3) C222 0.106(7) 0.073(5) 0.041(4) 0.018(4) 0.023(4) 0.025(5) C223 0.113(7) 0.078(6) 0.053(5) 0.023(4) 0.044(5) 0.049(5) O224 0.113(5) 0.075(4) 0.067(4) 0.019(3) 0.037(3) 0.037(4) C225 0.080(6) 0.066(5) 0.048(4) 0.004(4) 0.011(4) 0.027(4) C226 0.065(5) 0.064(5) 0.038(4) 0.011(3) 0.004(3) 0.029(4) C227 0.037(3) 0.038(3) 0.051(4) 0.016(3) 0.021(3) 0.012(3) O228 0.040(2) 0.063(3) 0.078(3) 0.044(3) 0.029(2) 0.026(2) N229 0.035(3) 0.046(3) 0.064(3) 0.028(3) 0.025(2) 0.018(2) C230 0.082(7) 0.090(7) 0.097(7) 0.060(6) 0.033(6) 0.029(5) C231 0.084(7) 0.087(7) 0.108(8) 0.038(6) 0.014(6) 0.038(6) O232 0.055(3) 0.049(3) 0.072(3) 0.035(2) 0.034(2) 0.027(2) C233 0.038(3) 0.053(4) 0.064(4) 0.020(3) 0.023(3) 0.017(3) C234 0.031(3) 0.073(5) 0.066(5) 0.026(4) 0.014(3) 0.006(3) C235 0.040(4) 0.062(4) 0.044(4) 0.008(3) 0.007(3) 0.007(3) C236 0.033(3) 0.036(3) 0.048(4) 0.011(3) 0.011(3) 0.005(2) C237 0.036(3) 0.032(3) 0.042(3) 0.014(2) 0.015(3) 0.007(2) C238 0.060(4) 0.059(4) 0.077(5) 0.044(4) 0.041(4) 0.041(4) O239 0.050(3) 0.058(3) 0.054(3) 0.027(2) 0.011(2) 0.023(2) C240 0.039(3) 0.032(3) 0.037(3) 0.011(2) 0.017(2) 0.007(2) C241 0.043(3) 0.031(3) 0.033(3) 0.009(2) 0.013(2) 0.008(2) O242 0.064(3) 0.085(4) 0.056(3) 0.015(3) 0.020(3) 0.028(3) C243 0.032(3) 0.034(3) 0.036(3) 0.009(2) 0.013(2) 0.006(2) C244 0.033(3) 0.038(3) 0.032(3) 0.002(2) 0.010(2) 0.005(2) Fe301 0.0345(5) 0.0412(6) 0.0610(7) 0.0198(5) 0.0177(5) 0.0076(4) C302 0.098(8) 0.084(7) 0.141(10) 0.067(7) 0.059(7) 0.063(6) C303 0.055(4) 0.054(4) 0.078(5) 0.036(4) 0.041(4) 0.032(3) C304 0.040(3) 0.041(3) 0.077(5) 0.029(3) 0.029(3) 0.018(3) C305 0.099(7) 0.051(5) 0.118(9) 0.046(6) 0.012(7) -0.003(5) C306 0.265(17) 0.064(6) 0.082(7) 0.032(6) 0.061(10) 0.105(9) C307 0.044(3) 0.037(3) 0.050(4) 0.010(3) 0.017(3) 0.009(3) C308 0.043(4) 0.053(4) 0.070(5) 0.036(4) 0.033(3) 0.027(3) C309 0.038(3) 0.053(4) 0.059(4) 0.032(3) 0.016(3) 0.018(3) C310 0.044(4) 0.049(4) 0.057(4) 0.030(3) 0.008(3) 0.017(3) C311 0.030(3) 0.055(4) 0.060(4) 0.029(3) 0.020(3) 0.019(3) C312 0.055(4) 0.070(5) 0.064(4) 0.042(4) 0.036(4) 0.041(4) C313 0.041(3) 0.037(3) 0.039(3) 0.009(3) 0.011(3) 0.007(3) C314 0.049(4) 0.070(5) 0.058(4) 0.013(4) 0.010(3) 0.025(4) C315 0.071(5) 0.067(5) 0.052(4) 0.026(4) 0.012(4) 0.036(4) C316 0.032(3) 0.029(3) 0.034(3) 0.008(2) 0.013(2) 0.006(2) C317 0.035(3) 0.034(3) 0.038(3) 0.006(2) 0.014(2) 0.005(2) C318 0.051(4) 0.042(3) 0.036(3) 0.009(3) 0.014(3) 0.006(3) O319 0.063(3) 0.057(3) 0.040(3) -0.005(2) 0.015(2) -0.012(2) N320 0.050(3) 0.035(3) 0.035(3) 0.006(2) 0.016(2) 0.007(2) C321 0.072(5) 0.036(3) 0.041(3) 0.008(3) 0.029(3) 0.017(3) C322 0.071(4) 0.034(3) 0.038(3) 0.013(3) 0.024(3) 0.020(3) O323 0.052(3) 0.036(2) 0.042(2) 0.0146(18) 0.020(2) 0.0173(19) C324 0.043(3) 0.032(3) 0.030(3) 0.003(2) 0.011(2) 0.011(2) C325 0.034(3) 0.036(3) 0.041(3) 0.008(3) 0.009(2) 0.014(2) C326 0.038(3) 0.040(3) 0.039(3) 0.013(3) 0.008(3) 0.013(3) C327 0.036(3) 0.037(3) 0.033(3) 0.007(2) 0.010(2) 0.010(2) C328 0.035(3) 0.043(3) 0.035(3) 0.005(3) 0.008(2) 0.015(3) C329 0.041(3) 0.034(3) 0.037(3) 0.007(2) 0.011(3) 0.015(3) O330 0.039(2) 0.053(3) 0.047(2) 0.021(2) 0.0174(19) 0.018(2) C331 0.038(3) 0.050(4) 0.039(3) 0.006(3) 0.014(3) 0.015(3) C332 0.040(3) 0.062(4) 0.034(3) 0.006(3) 0.016(3) 0.014(3) O333 0.045(2) 0.055(3) 0.037(2) 0.013(2) 0.0210(19) 0.012(2) C334 0.041(3) 0.076(5) 0.038(3) 0.026(3) 0.019(3) 0.017(3) C335 0.0447(18) 0.061(2) 0.0403(16) 0.0159(15) 0.0144(14) -0.0072(16) O336 0.034(2) 0.070(3) 0.055(3) 0.011(3) 0.024(2) 0.017(3) C337 0.029(2) 0.064(3) 0.0408(15) 0.0155(17) 0.0214(15) -0.001(2) C338 0.0430(18) 0.0603(19) 0.0397(15) 0.0169(14) 0.0153(13) -0.0066(15) O339 0.0410(17) 0.0591(19) 0.0384(15) 0.0160(14) 0.0151(13) -0.0047(15) C340 0.035(3) 0.047(3) 0.033(3) 0.005(3) 0.009(2) 0.002(3) C341 0.029(3) 0.055(4) 0.034(3) 0.012(3) 0.011(2) 0.009(3) O342 0.031(2) 0.046(2) 0.039(2) 0.0150(18) 0.0133(17) 0.0090(17) C343 0.028(3) 0.035(3) 0.031(3) 0.003(2) 0.008(2) 0.001(2) C344 0.030(3) 0.033(3) 0.037(3) 0.005(2) 0.010(2) 0.006(2) C345 0.024(3) 0.035(3) 0.043(3) 0.007(2) 0.010(2) 0.005(2) C346 0.026(3) 0.032(3) 0.031(3) 0.003(2) 0.008(2) 0.001(2) C347 0.033(3) 0.035(3) 0.039(3) 0.011(2) 0.013(2) 0.011(2) C348 0.030(3) 0.041(3) 0.034(3) 0.008(2) 0.011(2) 0.007(2) O349 0.0280(19) 0.039(2) 0.041(2) 0.0111(17) 0.0161(17) 0.0096(16) C350 0.029(3) 0.037(3) 0.039(3) 0.010(2) 0.013(2) 0.008(2) C351 0.089(6) 0.067(5) 0.060(5) 0.025(4) 0.023(4) 0.037(5) N352 0.030(2) 0.036(3) 0.036(3) 0.004(2) 0.016(2) 0.005(2) C353 0.072(5) 0.082(6) 0.059(5) 0.018(4) 0.026(4) 0.031(4) O354 0.044(2) 0.058(3) 0.047(3) -0.008(2) 0.027(2) -0.003(2) C501 0.049(3) 0.041(4) 0.068(3) 0.011(2) 0.007(3) 0.006(3) Cl502 0.0633(11) 0.0587(11) 0.0736(12) 0.0042(9) 0.0099(9) 0.0127(9) Cl503 0.0572(11) 0.0652(12) 0.0959(16) -0.0040(11) -0.0039(10) 0.0203(9) Cl504 0.0903(15) 0.0718(13) 0.0933(15) 0.0389(12) 0.0364(13) 0.0259(11) C505 0.075(7) 0.036(7) 0.077(9) -0.010(5) 0.000(4) -0.005(6) Cl506 0.102(5) 0.107(7) 0.241(12) -0.033(7) 0.069(6) 0.002(5) Cl507 0.107(5) 0.320(14) 0.109(6) -0.010(7) -0.030(5) 0.038(8) Cl508 0.140(8) 0.158(9) 0.349(15) 0.182(10) 0.078(8) 0.041(7) C509 0.074(5) 0.042(5) 0.063(4) -0.005(4) 0.002(5) 0.005(3) Cl510 0.238(6) 0.082(2) 0.077(3) 0.0226(19) 0.003(3) 0.051(3) Cl511 0.0628(17) 0.0658(19) 0.143(3) 0.0068(18) 0.0326(18) 0.0243(14) Cl512 0.0541(17) 0.090(2) 0.076(2) -0.0089(17) 0.0140(14) 0.0125(15) C513 0.047(3) 0.055(4) 0.084(4) 0.006(2) 0.013(4) 0.013(3) Cl514 0.0726(13) 0.0724(13) 0.0714(13) 0.0026(10) 0.0073(10) 0.0178(10) C514 0.037(3) 0.046(3) 0.034(3) 0.007(3) 0.008(3) 0.017(3) Cl515 0.0571(13) 0.0888(17) 0.164(3) 0.0199(17) 0.0158(15) 0.0302(12) Cl516 0.0861(15) 0.0845(15) 0.0861(15) 0.0189(12) 0.0353(12) 0.0297(12) C517 0.112(12) 0.13(2) 0.172(12) 0.098(18) 0.031(17) 0.067(13) Cl518 0.063(3) 0.069(4) 0.075(4) 0.023(3) 0.003(3) 0.022(2) Cl519 0.135(7) 0.127(9) 0.124(8) 0.051(7) 0.070(6) 0.104(7) Cl520 0.107(7) 0.242(15) 0.220(12) 0.195(12) 0.084(7) 0.091(9) C521 0.129(9) 0.116(8) 0.137(10) -0.019(7) 0.044(7) -0.007(7) Cl522 0.102(8) 0.096(8) 0.134(10) -0.003(7) 0.047(7) -0.005(6) Cl523 0.150(10) 0.125(9) 0.142(10) -0.027(8) 0.067(8) 0.002(8) Cl524 0.128(10) 0.126(9) 0.127(11) -0.022(8) 0.019(8) -0.012(8) C635 0.0447(18) 0.061(2) 0.0403(16) 0.0159(15) 0.0144(14) -0.0072(16) O636 0.0436(18) 0.061(2) 0.0399(16) 0.0168(14) 0.0151(14) -0.0072(15) C637 0.0433(18) 0.0604(19) 0.0397(15) 0.0168(14) 0.0152(13) -0.0067(15) C638 0.0430(18) 0.0603(19) 0.0397(15) 0.0169(14) 0.0153(13) -0.0066(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 1.555(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 C2 . N3 . 1.481(6) yes C2 . H21 . 0.953 no C2 . H22 . 0.973 no C2 . H23 . 0.957 no N3 . C4 . 1.337(6) yes N3 . C8 . 1.337(7) yes C4 . C5 . 1.390(7) yes C4 . H41 . 0.934 no C5 . C6 . 1.384(7) yes C5 . C9 . 1.509(7) yes C6 . C7 . 1.380(7) yes C6 . H61 . 0.936 no C7 . C8 . 1.369(7) yes C7 . C27 . 1.507(7) yes C8 . H81 . 0.923 no C9 . O10 . 1.222(7) yes C9 . N11 . 1.335(7) yes N11 . C12 . 1.457(7) yes N11 . H111 . 0.857 no C12 . C13 . 1.486(9) yes C12 . H121 . 0.969 no C12 . H122 . 0.972 no C13 . O14 . 1.410(7) yes C13 . H131 . 0.985 no C13 . H132 . 0.991 no O14 . C15 . 1.375(8) yes C15 . C16 . 1.369(8) yes C15 . C20 . 1.392(8) yes C16 . C17 . 1.384(9) yes C16 . H161 . 0.933 no C17 . C18 . 1.400(8) yes C17 . H171 . 0.933 no C18 . C19 . 1.361(9) yes C18 . O21 . 1.368(8) yes C19 . C20 . 1.389(9) yes C19 . H191 . 0.928 no C20 . H201 . 0.947 no O21 . C22 . 1.405(7) yes C22 . C23 . 1.494(9) yes C22 . H221 . 0.987 no C22 . H222 . 0.980 no C23 . O24 . 1.424(7) yes C23 . H232 . 0.984 no C23 . H231 . 0.984 no O24 . C25 . 1.439(8) yes C25 . C26 . 1.510(10) yes C25 . H252 . 0.977 no C25 . H251 . 0.989 no C26 . C44 2_667 1.361(10) yes C26 . H261 . 0.946 no C27 . O28 . 1.220(7) yes C27 . N29 . 1.329(7) yes N29 . C30 . 1.468(7) yes N29 . H291 . 0.861 no C30 . C31 . 1.513(9) yes C30 . H301 . 0.974 no C30 . H302 . 0.979 no C31 . O32 . 1.415(7) yes C31 . H311 . 0.968 no C31 . H312 . 0.969 no O32 . C33 . 1.381(8) yes C33 . C34 . 1.376(9) yes C33 . C38 . 1.380(8) yes C34 . C35 . 1.390(9) yes C34 . H341 . 0.929 no C35 . C36 . 1.369(9) yes C35 . H351 . 0.927 no C36 . C37 . 1.371(10) yes C36 . O39 . 1.389(8) yes C37 . C38 . 1.387(9) yes C37 . H371 . 0.926 no C38 . H381 . 0.923 no O39 . C40 . 1.431(8) yes C40 . C41 . 1.483(11) yes C40 . H401 . 0.983 no C40 . H402 . 0.971 no C41 . O42 . 1.462(9) yes C41 . H411 . 0.975 no C41 . H412 . 0.980 no O42 . C43 . 1.395(9) yes C43 . C44 . 1.498(12) yes C43 . H431 . 0.973 no C43 . H432 . 0.982 no C44 . H441 . 0.927 no Fe101 . C102 . 1.995(9) yes Fe101 . C103 . 2.011(8) yes Fe101 . C104 . 2.067(9) yes Fe101 . C105 . 2.114(9) yes Fe101 . C106 . 2.056(8) yes Fe101 . C107 . 2.027(8) yes Fe101 . C108 . 2.029(7) yes Fe101 . C109 . 2.017(7) yes Fe101 . C110 . 2.020(6) yes Fe101 . C111 . 2.035(6) yes C102 . C103 . 1.429(8) yes C102 . C106 . 1.374(11) yes C102 . H1021 . 0.973 no C103 . C104 . 1.399(8) yes C103 . H1031 . 0.966 no C104 . C105 . 1.389(7) yes C104 . H1041 . 0.978 no C105 . C106 . 1.381(8) yes C105 . H1051 . 0.993 no C106 . H1061 . 0.985 no C107 . C108 . 1.409(9) yes C107 . C111 . 1.427(9) yes C107 . H1071 . 0.983 no C108 . C109 . 1.399(10) yes C108 . H1081 . 0.981 no C109 . C110 . 1.418(8) yes C109 . H1091 . 0.986 no C110 . C111 . 1.433(8) yes C110 . H1101 . 0.979 no C111 . C112 . 1.483(7) yes C112 . C113 . 1.396(8) yes C112 . C117 . 1.399(8) yes C113 . C114 . 1.390(7) yes C113 . H1131 . 0.935 no C114 . C115 . 1.391(7) yes C114 . C118 . 1.502(8) yes C115 . C116 . 1.389(7) yes C115 . H1151 . 0.938 no C116 . C117 . 1.390(7) yes C116 . C153 . 1.490(7) yes C117 . H1171 . 0.934 no C118 . O119 . 1.240(7) yes C118 . N120 . 1.327(7) yes N120 . C121 . 1.456(7) yes N120 . H1201 . 0.869 no C121 . C122 . 1.509(7) yes C121 . H1211 . 0.957 no C121 . H1212 . 0.965 no C122 . O123 . 1.434(6) yes C122 . H1222 . 0.967 no C122 . H1221 . 0.979 no O123 . C124 . 1.378(6) yes C124 . C125 . 1.392(7) yes C124 . C129 . 1.375(7) yes C125 . C126 . 1.376(7) yes C125 . H1251 . 0.934 no C126 . C127 . 1.383(7) yes C126 . H1261 . 0.942 no C127 . C128 . 1.393(7) yes C127 . O130 . 1.385(6) yes C128 . C129 . 1.403(7) yes C128 . H1281 . 0.934 no C129 . H1291 . 0.929 no O130 . C131 . 1.430(6) yes C131 . C132 . 1.504(7) yes C131 . H1311 . 0.978 no C131 . H1312 . 0.978 no C132 . O133 . 1.414(6) yes C132 . H1321 . 0.975 no C132 . H1322 . 0.976 no O133 . C134 . 1.428(6) yes C134 . C135 . 1.494(8) yes C134 . H1342 . 0.976 no C134 . H1341 . 0.974 no C135 . O136 . 1.424(7) yes C135 . H1351 . 0.982 no C135 . H1352 . 0.972 no O136 . C137 . 1.419(7) yes C137 . C138 . 1.496(8) yes C137 . H1371 . 0.969 no C137 . H1372 . 0.980 no C138 . O139 . 1.433(6) yes C138 . H1382 . 0.979 no C138 . H1381 . 0.991 no O139 . C140 . 1.425(6) yes C140 . C141 . 1.495(8) yes C140 . H1402 . 0.960 no C140 . H1401 . 0.978 no C141 . O142 . 1.436(6) yes C141 . H1411 . 0.964 no C141 . H1412 . 0.973 no O142 . C143 . 1.386(6) yes C143 . C144 . 1.394(8) yes C143 . C148 . 1.368(8) yes C144 . C145 . 1.373(8) yes C144 . H1441 . 0.926 no C145 . C146 . 1.396(8) yes C145 . H1451 . 0.941 no C146 . C147 . 1.386(8) yes C146 . O149 . 1.386(6) yes C147 . C148 . 1.408(7) yes C147 . H1471 . 0.926 no C148 . H1481 . 0.924 no O149 . C150 . 1.424(7) yes C150 . C151 . 1.516(8) yes C150 . H1502 . 0.965 no C150 . H1501 . 0.965 no C151 . N152 . 1.448(7) yes C151 . H1511 . 0.967 no C151 . H1512 . 0.973 no N152 . C153 . 1.350(7) yes N152 . H1521 . 0.862 no C153 . O154 . 1.232(7) yes C202 . N203 . 1.483(6) yes C202 . H2021 . 0.946 no C202 . H2023 . 0.958 no C202 . H2022 . 0.958 no N203 . C204 . 1.332(7) yes N203 . C208 . 1.340(6) yes C204 . C205 . 1.381(7) yes C204 . H2041 . 0.923 no C205 . C206 . 1.389(7) yes C205 . C514 . 1.504(7) yes C206 . C207 . 1.370(7) yes C206 . H2061 . 0.922 no C207 . C208 . 1.381(7) yes C207 . C227 . 1.512(7) yes C208 . H2081 . 0.940 no O210 . C514 . 1.217(7) yes N211 . C212 . 1.460(7) yes N211 . C514 . 1.338(7) yes N211 . H2111 . 0.847 no C212 . C213 . 1.542(8) yes C212 . H2121 . 0.983 no C212 . H2122 . 0.960 no C213 . O214 . 1.404(8) yes C213 . H2132 . 0.993 no C213 . H2131 . 0.983 no O214 . C215 . 1.394(7) yes C215 . C216 . 1.344(9) yes C215 . C220 . 1.405(9) yes C216 . C217 . 1.414(9) yes C216 . H2161 . 0.928 no C217 . C218 . 1.385(10) yes C217 . H2171 . 0.921 no C218 . C219 . 1.361(10) yes C218 . O221 . 1.391(7) yes C219 . C220 . 1.371(9) yes C219 . H2191 . 0.939 no C220 . H2201 . 0.944 no O221 . C222 . 1.390(9) yes C222 . C223 . 1.522(10) yes C222 . H2221 . 0.968 no C222 . H2222 . 0.965 no C223 . O224 . 1.359(9) yes C223 . H2232 . 0.979 no C223 . H2231 . 0.989 no O224 . C225 . 1.431(9) yes C225 . C226 . 1.484(10) yes C225 . H2251 . 0.973 no C225 . H2252 . 0.985 no C226 . C351 2_566 1.322(10) yes C226 . H2261 . 0.925 no C227 . O228 . 1.232(7) yes C227 . N229 . 1.336(7) yes N229 . C304 . 1.472(7) yes N229 . H2291 . 0.859 no C230 . C231 . 1.335(12) yes C230 . Fe301 . 2.040(8) yes C230 . C305 . 1.380(13) yes C230 . H2301 . 0.988 no C231 . Fe301 . 2.050(10) yes C231 . C302 . 1.312(14) yes C231 . H2311 . 0.982 no O232 . C303 . 1.422(7) yes O232 . C308 . 1.374(8) yes C233 . C234 . 1.416(10) yes C233 . Fe301 . 2.041(6) yes C233 . C307 . 1.415(8) yes C233 . H2331 . 0.973 no C234 . C235 . 1.427(9) yes C234 . Fe301 . 2.048(7) yes C234 . H2341 . 0.980 no C235 . C236 . 1.436(8) yes C235 . Fe301 . 2.035(7) yes C235 . H2351 . 0.971 no C236 . C237 . 1.469(8) yes C236 . Fe301 . 2.049(6) yes C236 . C307 . 1.435(8) yes C237 . C313 . 1.394(8) yes C237 . C317 . 1.414(8) yes C238 . C308 . 1.411(9) yes C238 . C312 . 1.368(10) yes C238 . H2381 . 0.940 no O239 . C311 . 1.381(8) yes O239 . C315 . 1.408(7) yes C240 . C241 . 1.391(8) yes C240 . C316 . 1.399(7) yes C240 . H2401 . 0.932 no C241 . C313 . 1.389(8) yes C241 . C318 . 1.497(8) yes O242 . C314 . 1.419(8) yes O242 . C353 . 1.438(9) yes C243 . C316 . 1.503(7) yes C243 . N352 . 1.344(7) yes C243 . O354 . 1.229(7) yes C244 . C350 . 1.501(7) yes C244 . N352 . 1.450(7) yes C244 . H2441 . 0.977 no C244 . H2442 . 0.967 no Fe301 . C302 . 2.007(9) yes Fe301 . C305 . 2.010(8) yes Fe301 . C306 . 2.008(8) yes Fe301 . C307 . 2.028(6) yes C302 . C306 . 1.449(16) yes C302 . H3021 . 0.989 no C303 . C304 . 1.501(10) yes C303 . H3031 . 0.973 no C303 . H3032 . 0.967 no C304 . H3041 . 0.975 no C304 . H3042 . 0.969 no C305 . C306 . 1.469(15) yes C305 . H3051 . 0.975 no C306 . H3061 . 0.961 no C307 . H3071 . 0.978 no C308 . C309 . 1.370(8) yes C309 . C310 . 1.384(9) yes C309 . H3091 . 0.927 no C310 . C311 . 1.399(8) yes C310 . H3101 . 0.932 no C311 . C312 . 1.373(8) yes C312 . H3121 . 0.945 no C313 . H3131 . 0.944 no C314 . C315 . 1.514(9) yes C314 . H3141 . 0.973 no C314 . H3142 . 0.978 no C315 . H3151 . 0.978 no C315 . H3152 . 0.987 no C316 . C317 . 1.383(7) yes C317 . H3171 . 0.939 no C318 . O319 . 1.231(7) yes C318 . N320 . 1.344(8) yes N320 . C321 . 1.452(7) yes N320 . H3201 . 0.849 no C321 . C322 . 1.510(8) yes C321 . H3211 . 0.965 no C321 . H3212 . 0.969 no C322 . O323 . 1.429(6) yes C322 . H3222 . 0.968 no C322 . H3221 . 0.971 no O323 . C324 . 1.382(7) yes C324 . C325 . 1.393(8) yes C324 . C329 . 1.383(8) yes C325 . C326 . 1.379(8) yes C325 . H3251 . 0.937 no C326 . C327 . 1.384(8) yes C326 . H3261 . 0.930 no C327 . C328 . 1.384(8) yes C327 . O330 . 1.380(6) yes C328 . C329 . 1.398(8) yes C328 . H3281 . 0.933 no C329 . H3291 . 0.926 no O330 . C331 . 1.433(7) yes C331 . C332 . 1.522(7) yes C331 . H3311 . 0.967 no C331 . H3312 . 0.967 no C332 . O333 . 1.421(7) yes C332 . H3321 . 0.973 no C332 . H3322 . 0.970 no O333 . C334 . 1.430(4) yes C334 . C335 . 1.44651(7) yes C334 . H3341 . 0.950 no C334 . H3342 . 0.950 no C335 . O336 . 1.4737(10) yes C335 . H3351 . 0.973 no C335 . H3352 . 0.969 no O336 . C337 . 1.4739(10) yes C337 . C338 . 1.64247(10) yes C337 . H3371 . 0.963 no C337 . H3372 . 0.949 no C338 . O339 . 1.149(7) yes C338 . H3381 . 0.968 no C338 . H3382 . 0.977 no O339 . C340 . 1.429(6) yes C340 . C341 . 1.515(7) yes C340 . H3401 . 0.966 no C340 . H3402 . 0.976 no C341 . O342 . 1.435(6) yes C341 . H3411 . 0.972 no C341 . H3412 . 0.963 no O342 . C343 . 1.380(6) yes C343 . C344 . 1.385(7) yes C343 . C348 . 1.384(8) yes C344 . C345 . 1.391(7) yes C344 . H3441 . 0.928 no C345 . C346 . 1.385(7) yes C345 . H3451 . 0.934 no C346 . C347 . 1.386(7) yes C346 . O349 . 1.384(6) yes C347 . C348 . 1.395(7) yes C347 . H3471 . 0.929 no C348 . H3481 . 0.932 no O349 . C350 . 1.443(6) yes C350 . H3501 . 0.973 no C350 . H3502 . 0.977 no C351 . C353 . 1.480(10) yes C351 . H3511 . 0.947 no N352 . H3521 . 0.862 no C353 . H3531 . 0.987 no C353 . H3532 . 0.975 no C501 . Cl502 . 1.771(7) yes C501 . Cl503 . 1.752(7) yes C501 . Cl504 . 1.745(7) yes C501 . H5011 . 0.969 no C505 . Cl506 . 1.7603(10) yes C505 . Cl507 . 1.7600(10) yes C505 . Cl508 . 1.7602(10) yes C505 . H5051 . 0.975 no C509 . Cl510 . 1.752(11) yes C509 . Cl511 . 1.724(13) yes C509 . Cl512 . 1.769(12) yes C509 . H5091 . 0.984 no C513 . Cl514 . 1.765(8) yes C513 . Cl515 . 1.755(7) yes C513 . Cl516 . 1.746(8) yes C513 . H5131 . 0.975 no C517 . Cl518 . 1.76001(9) yes C517 . Cl519 . 1.76017(12) yes C517 . Cl520 . 1.76040(10) yes C517 . H5171 . 0.976 no C521 . Cl522 . 1.73(7) yes C521 . Cl523 . 1.86(6) yes C521 . Cl524 . 1.71(8) yes C521 . H5211 . 0.980 no C635 . O636 . 1.4733(10) yes C635 . H6352 . 0.972 no C635 . H6351 . 0.967 no O636 . C637 . 1.47493(12) yes C637 . C638 . 1.36297(8) yes C637 . H6371 . 0.950 no C637 . H6372 . 0.950 no C638 . H6382 . 0.968 no C638 . H6381 . 0.974 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 N3 . C2 . H21 . 110.9 no N3 . C2 . H22 . 109.9 no H21 . C2 . H22 . 109.2 no N3 . C2 . H23 . 110.0 no H21 . C2 . H23 . 109.1 no H22 . C2 . H23 . 107.7 no C2 . N3 . C4 . 119.8(4) yes C2 . N3 . C8 . 118.2(4) yes C4 . N3 . C8 . 122.0(5) yes N3 . C4 . C5 . 119.8(5) yes N3 . C4 . H41 . 118.6 no C5 . C4 . H41 . 121.6 no C4 . C5 . C6 . 118.9(5) yes C4 . C5 . C9 . 115.6(5) yes C6 . C5 . C9 . 125.5(5) yes C5 . C6 . C7 . 119.4(5) yes C5 . C6 . H61 . 121.0 no C7 . C6 . H61 . 119.6 no C6 . C7 . C8 . 119.6(5) yes C6 . C7 . C27 . 124.8(5) yes C8 . C7 . C27 . 115.6(5) yes C7 . C8 . N3 . 120.2(5) yes C7 . C8 . H81 . 120.4 no N3 . C8 . H81 . 119.3 no C5 . C9 . O10 . 120.2(5) yes C5 . C9 . N11 . 115.3(5) yes O10 . C9 . N11 . 124.5(5) yes C9 . N11 . C12 . 123.5(5) yes C9 . N11 . H111 . 118.2 no C12 . N11 . H111 . 117.8 no N11 . C12 . C13 . 109.9(5) yes N11 . C12 . H121 . 109.5 no C13 . C12 . H121 . 108.8 no N11 . C12 . H122 . 109.6 no C13 . C12 . H122 . 110.1 no H121 . C12 . H122 . 108.8 no C12 . C13 . O14 . 108.8(5) yes C12 . C13 . H131 . 110.8 no O14 . C13 . H131 . 109.2 no C12 . C13 . H132 . 109.9 no O14 . C13 . H132 . 110.6 no H131 . C13 . H132 . 107.6 no C13 . O14 . C15 . 118.0(5) yes O14 . C15 . C16 . 117.0(5) yes O14 . C15 . C20 . 123.4(6) yes C16 . C15 . C20 . 119.6(6) yes C15 . C16 . C17 . 121.5(6) yes C15 . C16 . H161 . 119.6 no C17 . C16 . H161 . 118.9 no C16 . C17 . C18 . 118.8(6) yes C16 . C17 . H171 . 120.5 no C18 . C17 . H171 . 120.7 no C17 . C18 . C19 . 119.6(6) yes C17 . C18 . O21 . 124.0(6) yes C19 . C18 . O21 . 116.4(6) yes C18 . C19 . C20 . 121.7(6) yes C18 . C19 . H191 . 119.1 no C20 . C19 . H191 . 119.2 no C15 . C20 . C19 . 118.8(6) yes C15 . C20 . H201 . 119.9 no C19 . C20 . H201 . 121.2 no C18 . O21 . C22 . 117.5(5) yes O21 . C22 . C23 . 108.7(5) yes O21 . C22 . H221 . 109.0 no C23 . C22 . H221 . 110.8 no O21 . C22 . H222 . 107.9 no C23 . C22 . H222 . 108.0 no H221 . C22 . H222 . 112.4 no C22 . C23 . O24 . 108.6(6) yes C22 . C23 . H232 . 111.6 no O24 . C23 . H232 . 106.8 no C22 . C23 . H231 . 109.4 no O24 . C23 . H231 . 109.9 no H232 . C23 . H231 . 110.5 no C23 . O24 . C25 . 108.6(5) yes O24 . C25 . C26 . 105.4(6) yes O24 . C25 . H252 . 108.1 no C26 . C25 . H252 . 106.3 no O24 . C25 . H251 . 112.3 no C26 . C25 . H251 . 115.8 no H252 . C25 . H251 . 108.6 no C25 . C26 . C44 2_667 119.1(8) yes C25 . C26 . H261 . 121.2 no C44 2_667 C26 . H261 . 119.7 no C7 . C27 . O28 . 118.8(5) yes C7 . C27 . N29 . 118.2(5) yes O28 . C27 . N29 . 123.0(5) yes C27 . N29 . C30 . 120.3(5) yes C27 . N29 . H291 . 118.9 no C30 . N29 . H291 . 120.6 no N29 . C30 . C31 . 110.6(5) yes N29 . C30 . H301 . 110.9 no C31 . C30 . H301 . 109.9 no N29 . C30 . H302 . 108.1 no C31 . C30 . H302 . 108.7 no H301 . C30 . H302 . 108.5 no C30 . C31 . O32 . 106.0(6) yes C30 . C31 . H311 . 109.2 no O32 . C31 . H311 . 110.1 no C30 . C31 . H312 . 111.1 no O32 . C31 . H312 . 110.3 no H311 . C31 . H312 . 110.1 no C31 . O32 . C33 . 118.4(5) yes O32 . C33 . C34 . 124.8(6) yes O32 . C33 . C38 . 115.3(6) yes C34 . C33 . C38 . 119.9(6) yes C33 . C34 . C35 . 119.6(6) yes C33 . C34 . H341 . 120.5 no C35 . C34 . H341 . 119.9 no C34 . C35 . C36 . 120.3(7) yes C34 . C35 . H351 . 119.9 no C36 . C35 . H351 . 119.8 no C35 . C36 . C37 . 120.4(7) yes C35 . C36 . O39 . 115.6(7) yes C37 . C36 . O39 . 124.1(6) yes C36 . C37 . C38 . 119.7(6) yes C36 . C37 . H371 . 120.9 no C38 . C37 . H371 . 119.4 no C37 . C38 . C33 . 120.1(7) yes C37 . C38 . H381 . 119.5 no C33 . C38 . H381 . 120.4 no C36 . O39 . C40 . 116.8(6) yes O39 . C40 . C41 . 108.5(7) yes O39 . C40 . H401 . 108.4 no C41 . C40 . H401 . 109.0 no O39 . C40 . H402 . 111.0 no C41 . C40 . H402 . 110.0 no H401 . C40 . H402 . 109.8 no C40 . C41 . O42 . 104.3(6) yes C40 . C41 . H411 . 112.5 no O42 . C41 . H411 . 108.9 no C40 . C41 . H412 . 113.0 no O42 . C41 . H412 . 108.6 no H411 . C41 . H412 . 109.3 no C41 . O42 . C43 . 109.2(6) yes O42 . C43 . C44 . 115.6(8) yes O42 . C43 . H431 . 110.0 no C44 . C43 . H431 . 108.2 no O42 . C43 . H432 . 103.9 no C44 . C43 . H432 . 107.7 no H431 . C43 . H432 . 111.4 no C43 . C44 . C26 2_667 119.2(9) yes C43 . C44 . H441 . 120.9 no C26 2_667 C44 . H441 . 119.8 no C102 . Fe101 . C103 . 41.8(3) yes C102 . Fe101 . C104 . 67.9(3) yes C103 . Fe101 . C104 . 40.1(2) yes C102 . Fe101 . C105 . 66.7(3) yes C103 . Fe101 . C105 . 66.7(3) yes C104 . Fe101 . C105 . 38.8(2) yes C102 . Fe101 . C106 . 39.6(3) yes C103 . Fe101 . C106 . 67.2(3) yes C104 . Fe101 . C106 . 65.5(3) yes C105 . Fe101 . C106 . 38.7(2) yes C102 . Fe101 . C107 . 111.7(4) yes C103 . Fe101 . C107 . 125.7(4) yes C104 . Fe101 . C107 . 159.7(3) yes C105 . Fe101 . C107 . 161.2(3) yes C106 . Fe101 . C107 . 128.1(3) yes C102 . Fe101 . C108 . 130.0(4) yes C103 . Fe101 . C108 . 111.3(3) yes C104 . Fe101 . C108 . 123.0(3) yes C105 . Fe101 . C108 . 154.6(4) yes C106 . Fe101 . C108 . 166.2(4) yes C102 . Fe101 . C109 . 165.0(4) yes C103 . Fe101 . C109 . 125.0(4) yes C104 . Fe101 . C109 . 106.4(3) yes C105 . Fe101 . C109 . 118.1(4) yes C106 . Fe101 . C109 . 152.1(4) yes C102 . Fe101 . C110 . 153.8(4) yes C103 . Fe101 . C110 . 158.8(4) yes C104 . Fe101 . C110 . 120.8(4) yes C105 . Fe101 . C110 . 103.7(3) yes C106 . Fe101 . C110 . 117.9(4) yes C102 . Fe101 . C111 . 121.5(3) yes C103 . Fe101 . C111 . 159.7(4) yes C104 . Fe101 . C111 . 157.4(4) yes C105 . Fe101 . C111 . 122.3(3) yes C106 . Fe101 . C111 . 107.4(3) yes C107 . Fe101 . C108 . 40.7(3) yes C107 . Fe101 . C109 . 68.6(3) yes C108 . Fe101 . C109 . 40.5(3) yes C107 . Fe101 . C110 . 69.2(3) yes C108 . Fe101 . C110 . 68.8(3) yes C109 . Fe101 . C110 . 41.1(2) yes C107 . Fe101 . C111 . 41.1(2) yes C108 . Fe101 . C111 . 68.9(3) yes C109 . Fe101 . C111 . 69.3(2) yes C110 . Fe101 . C111 . 41.4(2) yes Fe101 . C102 . C103 . 69.7(5) yes Fe101 . C102 . C106 . 72.6(5) yes C103 . C102 . C106 . 106.8(5) yes Fe101 . C102 . H1021 . 125.9 no C103 . C102 . H1021 . 131.7 no C106 . C102 . H1021 . 121.3 no C102 . C103 . Fe101 . 68.5(5) yes C102 . C103 . C104 . 106.7(5) yes Fe101 . C103 . C104 . 72.1(5) yes C102 . C103 . H1031 . 126.5 no Fe101 . C103 . H1031 . 126.5 no C104 . C103 . H1031 . 126.7 no Fe101 . C104 . C103 . 67.8(5) yes Fe101 . C104 . C105 . 72.4(5) yes C103 . C104 . C105 . 109.0(5) yes Fe101 . C104 . H1041 . 123.3 no C103 . C104 . H1041 . 126.4 no C105 . C104 . H1041 . 124.6 no Fe101 . C105 . C104 . 68.8(5) yes Fe101 . C105 . C106 . 68.4(5) yes C104 . C105 . C106 . 107.2(5) yes Fe101 . C105 . H1051 . 127.4 no C104 . C105 . H1051 . 125.3 no C106 . C105 . H1051 . 127.5 no Fe101 . C106 . C105 . 72.9(5) yes Fe101 . C106 . C102 . 67.8(5) yes C105 . C106 . C102 . 110.3(5) yes Fe101 . C106 . H1061 . 122.5 no C105 . C106 . H1061 . 120.7 no C102 . C106 . H1061 . 128.8 no Fe101 . C107 . C108 . 69.7(4) yes Fe101 . C107 . C111 . 69.8(4) yes C108 . C107 . C111 . 108.4(6) yes Fe101 . C107 . H1071 . 127.3 no C108 . C107 . H1071 . 125.7 no C111 . C107 . H1071 . 125.9 no C107 . C108 . Fe101 . 69.6(4) yes C107 . C108 . C109 . 108.5(6) yes Fe101 . C108 . C109 . 69.3(4) yes C107 . C108 . H1081 . 125.8 no Fe101 . C108 . H1081 . 124.1 no C109 . C108 . H1081 . 125.7 no C108 . C109 . Fe101 . 70.2(4) yes C108 . C109 . C110 . 108.5(6) yes Fe101 . C109 . C110 . 69.5(4) yes C108 . C109 . H1091 . 126.6 no Fe101 . C109 . H1091 . 126.8 no C110 . C109 . H1091 . 124.9 no C109 . C110 . Fe101 . 69.3(4) yes C109 . C110 . C111 . 107.8(6) yes Fe101 . C110 . C111 . 69.9(3) yes C109 . C110 . H1101 . 127.2 no Fe101 . C110 . H1101 . 124.0 no C111 . C110 . H1101 . 125.0 no C110 . C111 . C107 . 106.8(5) yes C110 . C111 . Fe101 . 68.7(3) yes C107 . C111 . Fe101 . 69.1(4) yes C110 . C111 . C112 . 126.0(6) yes C107 . C111 . C112 . 127.1(6) yes Fe101 . C111 . C112 . 129.7(4) yes C111 . C112 . C113 . 120.6(5) yes C111 . C112 . C117 . 121.3(5) yes C113 . C112 . C117 . 118.1(5) yes C112 . C113 . C114 . 121.0(5) yes C112 . C113 . H1131 . 118.8 no C114 . C113 . H1131 . 120.2 no C113 . C114 . C115 . 120.0(5) yes C113 . C114 . C118 . 117.4(5) yes C115 . C114 . C118 . 122.6(5) yes C114 . C115 . C116 . 119.9(5) yes C114 . C115 . H1151 . 121.1 no C116 . C115 . H1151 . 119.0 no C115 . C116 . C117 . 119.7(5) yes C115 . C116 . C153 . 123.1(5) yes C117 . C116 . C153 . 117.2(5) yes C112 . C117 . C116 . 121.3(5) yes C112 . C117 . H1171 . 119.3 no C116 . C117 . H1171 . 119.4 no C114 . C118 . O119 . 121.0(5) yes C114 . C118 . N120 . 118.6(5) yes O119 . C118 . N120 . 120.4(5) yes C118 . N120 . C121 . 120.1(5) yes C118 . N120 . H1201 . 119.7 no C121 . N120 . H1201 . 119.7 no N120 . C121 . C122 . 111.7(4) yes N120 . C121 . H1211 . 109.7 no C122 . C121 . H1211 . 109.1 no N120 . C121 . H1212 . 108.9 no C122 . C121 . H1212 . 108.9 no H1211 . C121 . H1212 . 108.5 no C121 . C122 . O123 . 106.5(4) yes C121 . C122 . H1222 . 109.8 no O123 . C122 . H1222 . 110.7 no C121 . C122 . H1221 . 109.7 no O123 . C122 . H1221 . 111.0 no H1222 . C122 . H1221 . 109.1 no C122 . O123 . C124 . 115.0(4) yes O123 . C124 . C125 . 116.3(5) yes O123 . C124 . C129 . 124.2(5) yes C125 . C124 . C129 . 119.5(5) yes C124 . C125 . C126 . 120.7(5) yes C124 . C125 . H1251 . 119.5 no C126 . C125 . H1251 . 119.8 no C125 . C126 . C127 . 119.9(5) yes C125 . C126 . H1261 . 119.7 no C127 . C126 . H1261 . 120.4 no C126 . C127 . C128 . 120.3(5) yes C126 . C127 . O130 . 116.1(5) yes C128 . C127 . O130 . 123.6(5) yes C127 . C128 . C129 . 119.0(5) yes C127 . C128 . H1281 . 121.5 no C129 . C128 . H1281 . 119.5 no C128 . C129 . C124 . 120.5(5) yes C128 . C129 . H1291 . 119.1 no C124 . C129 . H1291 . 120.4 no C127 . O130 . C131 . 116.5(4) yes O130 . C131 . C132 . 107.8(4) yes O130 . C131 . H1311 . 109.3 no C132 . C131 . H1311 . 108.0 no O130 . C131 . H1312 . 111.9 no C132 . C131 . H1312 . 111.1 no H1311 . C131 . H1312 . 108.6 no C131 . C132 . O133 . 109.3(4) yes C131 . C132 . H1321 . 109.5 no O133 . C132 . H1321 . 109.6 no C131 . C132 . H1322 . 108.4 no O133 . C132 . H1322 . 110.0 no H1321 . C132 . H1322 . 110.1 no C132 . O133 . C134 . 110.8(4) yes O133 . C134 . C135 . 109.3(5) yes O133 . C134 . H1342 . 109.3 no C135 . C134 . H1342 . 109.2 no O133 . C134 . H1341 . 108.6 no C135 . C134 . H1341 . 111.2 no H1342 . C134 . H1341 . 109.2 no C134 . C135 . O136 . 108.2(5) yes C134 . C135 . H1351 . 109.0 no O136 . C135 . H1351 . 109.7 no C134 . C135 . H1352 . 111.2 no O136 . C135 . H1352 . 110.7 no H1351 . C135 . H1352 . 108.0 no C135 . O136 . C137 . 111.6(4) yes O136 . C137 . C138 . 108.4(5) yes O136 . C137 . H1371 . 110.4 no C138 . C137 . H1371 . 109.0 no O136 . C137 . H1372 . 108.7 no C138 . C137 . H1372 . 110.3 no H1371 . C137 . H1372 . 110.1 no C137 . C138 . O139 . 107.5(4) yes C137 . C138 . H1382 . 110.0 no O139 . C138 . H1382 . 110.3 no C137 . C138 . H1381 . 108.6 no O139 . C138 . H1381 . 110.5 no H1382 . C138 . H1381 . 109.9 no C138 . O139 . C140 . 110.4(4) yes O139 . C140 . C141 . 109.2(4) yes O139 . C140 . H1402 . 109.6 no C141 . C140 . H1402 . 109.0 no O139 . C140 . H1401 . 108.5 no C141 . C140 . H1401 . 110.8 no H1402 . C140 . H1401 . 109.8 no C140 . C141 . O142 . 107.4(5) yes C140 . C141 . H1411 . 109.5 no O142 . C141 . H1411 . 111.1 no C140 . C141 . H1412 . 109.8 no O142 . C141 . H1412 . 110.1 no H1411 . C141 . H1412 . 108.9 no C141 . O142 . C143 . 116.1(4) yes O142 . C143 . C144 . 114.3(5) yes O142 . C143 . C148 . 125.4(5) yes C144 . C143 . C148 . 120.3(5) yes C143 . C144 . C145 . 120.0(5) yes C143 . C144 . H1441 . 120.2 no C145 . C144 . H1441 . 119.8 no C144 . C145 . C146 . 120.0(5) yes C144 . C145 . H1451 . 119.9 no C146 . C145 . H1451 . 120.1 no C145 . C146 . C147 . 120.6(5) yes C145 . C146 . O149 . 115.3(5) yes C147 . C146 . O149 . 124.1(5) yes C146 . C147 . C148 . 118.6(5) yes C146 . C147 . H1471 . 120.3 no C148 . C147 . H1471 . 121.1 no C147 . C148 . C143 . 120.5(5) yes C147 . C148 . H1481 . 120.2 no C143 . C148 . H1481 . 119.2 no C146 . O149 . C150 . 116.4(4) yes O149 . C150 . C151 . 108.2(5) yes O149 . C150 . H1502 . 111.2 no C151 . C150 . H1502 . 110.7 no O149 . C150 . H1501 . 107.5 no C151 . C150 . H1501 . 109.8 no H1502 . C150 . H1501 . 109.4 no C150 . C151 . N152 . 111.2(5) yes C150 . C151 . H1511 . 108.1 no N152 . C151 . H1511 . 109.2 no C150 . C151 . H1512 . 109.8 no N152 . C151 . H1512 . 109.6 no H1511 . C151 . H1512 . 109.0 no C151 . N152 . C153 . 119.5(5) yes C151 . N152 . H1521 . 120.1 no C153 . N152 . H1521 . 119.5 no C116 . C153 . N152 . 118.7(5) yes C116 . C153 . O154 . 121.1(5) yes N152 . C153 . O154 . 120.3(5) yes N203 . C202 . H2021 . 109.8 no N203 . C202 . H2023 . 109.7 no H2021 . C202 . H2023 . 109.1 no N203 . C202 . H2022 . 109.5 no H2021 . C202 . H2022 . 110.4 no H2023 . C202 . H2022 . 108.3 no C202 . N203 . C204 . 118.8(4) yes C202 . N203 . C208 . 119.6(5) yes C204 . N203 . C208 . 121.6(5) yes N203 . C204 . C205 . 121.0(5) yes N203 . C204 . H2041 . 119.6 no C205 . C204 . H2041 . 119.4 no C204 . C205 . C206 . 117.9(5) yes C204 . C205 . C514 . 117.7(5) yes C206 . C205 . C514 . 124.3(5) yes C205 . C206 . C207 . 120.3(5) yes C205 . C206 . H2061 . 119.4 no C207 . C206 . H2061 . 120.2 no C206 . C207 . C208 . 119.2(5) yes C206 . C207 . C227 . 124.5(5) yes C208 . C207 . C227 . 116.3(5) yes C207 . C208 . N203 . 119.9(5) yes C207 . C208 . H2081 . 119.6 no N203 . C208 . H2081 . 120.4 no C212 . N211 . C514 . 123.3(5) yes C212 . N211 . H2111 . 117.3 no C514 . N211 . H2111 . 118.3 no N211 . C212 . C213 . 109.4(5) yes N211 . C212 . H2121 . 110.0 no C213 . C212 . H2121 . 109.7 no N211 . C212 . H2122 . 107.4 no C213 . C212 . H2122 . 108.3 no H2121 . C212 . H2122 . 111.9 no C212 . C213 . O214 . 106.6(5) yes C212 . C213 . H2132 . 109.4 no O214 . C213 . H2132 . 109.3 no C212 . C213 . H2131 . 110.7 no O214 . C213 . H2131 . 111.6 no H2132 . C213 . H2131 . 109.2 no C213 . O214 . C215 . 115.7(5) yes O214 . C215 . C216 . 126.5(6) yes O214 . C215 . C220 . 112.8(6) yes C216 . C215 . C220 . 120.7(6) yes C215 . C216 . C217 . 119.7(7) yes C215 . C216 . H2161 . 119.9 no C217 . C216 . H2161 . 120.4 no C216 . C217 . C218 . 119.1(7) yes C216 . C217 . H2171 . 120.9 no C218 . C217 . H2171 . 120.0 no C217 . C218 . C219 . 120.5(6) yes C217 . C218 . O221 . 124.2(7) yes C219 . C218 . O221 . 115.3(6) yes C218 . C219 . C220 . 120.7(7) yes C218 . C219 . H2191 . 119.3 no C220 . C219 . H2191 . 120.1 no C215 . C220 . C219 . 119.3(6) yes C215 . C220 . H2201 . 119.8 no C219 . C220 . H2201 . 120.8 no C218 . O221 . C222 . 118.7(6) yes O221 . C222 . C223 . 104.9(7) yes O221 . C222 . H2221 . 109.9 no C223 . C222 . H2221 . 109.1 no O221 . C222 . H2222 . 112.9 no C223 . C222 . H2222 . 111.3 no H2221 . C222 . H2222 . 108.6 no C222 . C223 . O224 . 115.3(7) yes C222 . C223 . H2232 . 107.4 no O224 . C223 . H2232 . 105.3 no C222 . C223 . H2231 . 108.2 no O224 . C223 . H2231 . 108.9 no H2232 . C223 . H2231 . 112.0 no C223 . O224 . C225 . 114.9(6) yes O224 . C225 . C226 . 108.2(6) yes O224 . C225 . H2251 . 110.8 no C226 . C225 . H2251 . 111.8 no O224 . C225 . H2252 . 106.9 no C226 . C225 . H2252 . 110.2 no H2251 . C225 . H2252 . 108.8 no C225 . C226 . C351 2_566 125.9(7) yes C225 . C226 . H2261 . 117.9 no C351 2_566 C226 . H2261 . 116.3 no C207 . C227 . O228 . 119.8(5) yes C207 . C227 . N229 . 115.3(5) yes O228 . C227 . N229 . 124.9(5) yes C227 . N229 . C304 . 123.3(5) yes C227 . N229 . H2291 . 118.4 no C304 . N229 . H2291 . 118.1 no C231 . C230 . Fe301 . 71.4(6) yes C231 . C230 . C305 . 112.2(10) yes Fe301 . C230 . C305 . 68.9(5) yes C231 . C230 . H2301 . 123.8 no Fe301 . C230 . H2301 . 123.2 no C305 . C230 . H2301 . 123.8 no C230 . C231 . Fe301 . 70.6(6) yes C230 . C231 . C302 . 108.1(11) yes Fe301 . C231 . C302 . 69.4(6) yes C230 . C231 . H2311 . 125.6 no Fe301 . C231 . H2311 . 124.7 no C302 . C231 . H2311 . 126.3 no C303 . O232 . C308 . 117.0(5) yes C234 . C233 . Fe301 . 70.0(4) yes C234 . C233 . C307 . 107.7(6) yes Fe301 . C233 . C307 . 69.1(3) yes C234 . C233 . H2331 . 125.6 no Fe301 . C233 . H2331 . 128.0 no C307 . C233 . H2331 . 126.7 no C233 . C234 . C235 . 108.2(6) yes C233 . C234 . Fe301 . 69.5(4) yes C235 . C234 . Fe301 . 69.0(4) yes C233 . C234 . H2341 . 125.6 no C235 . C234 . H2341 . 126.2 no Fe301 . C234 . H2341 . 126.6 no C234 . C235 . C236 . 108.6(6) yes C234 . C235 . Fe301 . 70.0(4) yes C236 . C235 . Fe301 . 70.0(4) yes C234 . C235 . H2351 . 125.8 no C236 . C235 . H2351 . 125.6 no Fe301 . C235 . H2351 . 125.7 no C235 . C236 . C237 . 126.7(6) yes C235 . C236 . Fe301 . 68.9(4) yes C237 . C236 . Fe301 . 127.4(4) yes C235 . C236 . C307 . 106.0(5) yes C237 . C236 . C307 . 127.3(5) yes Fe301 . C236 . C307 . 68.6(3) yes C236 . C237 . C313 . 121.5(5) yes C236 . C237 . C317 . 121.0(5) yes C313 . C237 . C317 . 117.5(5) yes C308 . C238 . C312 . 119.3(6) yes C308 . C238 . H2381 . 120.4 no C312 . C238 . H2381 . 120.3 no C311 . O239 . C315 . 116.0(5) yes C241 . C240 . C316 . 120.3(5) yes C241 . C240 . H2401 . 120.3 no C316 . C240 . H2401 . 119.4 no C240 . C241 . C313 . 119.4(5) yes C240 . C241 . C318 . 122.8(5) yes C313 . C241 . C318 . 117.6(5) yes C314 . O242 . C353 . 113.4(6) yes C316 . C243 . N352 . 118.2(5) yes C316 . C243 . O354 . 121.1(5) yes N352 . C243 . O354 . 120.7(5) yes C350 . C244 . N352 . 112.1(4) yes C350 . C244 . H2441 . 108.7 no N352 . C244 . H2441 . 109.5 no C350 . C244 . H2442 . 110.0 no N352 . C244 . H2442 . 107.4 no H2441 . C244 . H2442 . 108.9 no C231 . Fe301 . C236 . 122.9(4) yes C231 . Fe301 . C234 . 155.9(4) yes C236 . Fe301 . C234 . 69.1(2) yes C231 . Fe301 . C233 . 119.9(4) yes C236 . Fe301 . C233 . 69.3(2) yes C234 . Fe301 . C233 . 40.5(3) yes C231 . Fe301 . C230 . 38.1(4) yes C236 . Fe301 . C230 . 157.8(4) yes C234 . Fe301 . C230 . 123.9(3) yes C233 . Fe301 . C230 . 107.8(3) yes C231 . Fe301 . C235 . 160.9(4) yes C236 . Fe301 . C235 . 41.2(2) yes C234 . Fe301 . C235 . 40.9(3) yes C233 . Fe301 . C235 . 68.8(3) yes C230 . Fe301 . C235 . 160.1(4) yes C231 . Fe301 . C302 . 37.7(4) yes C236 . Fe301 . C302 . 108.2(3) yes C234 . Fe301 . C302 . 165.4(5) yes C233 . Fe301 . C302 . 153.3(5) yes C230 . Fe301 . C302 . 63.9(4) yes C231 . Fe301 . C305 . 67.4(4) yes C236 . Fe301 . C305 . 160.1(4) yes C234 . Fe301 . C305 . 108.7(4) yes C233 . Fe301 . C305 . 122.7(4) yes C230 . Fe301 . C305 . 39.8(4) yes C231 . Fe301 . C306 . 68.7(5) yes C236 . Fe301 . C306 . 121.2(4) yes C234 . Fe301 . C306 . 125.8(5) yes C233 . Fe301 . C306 . 161.9(6) yes C230 . Fe301 . C306 . 68.3(4) yes C231 . Fe301 . C307 . 105.9(4) yes C236 . Fe301 . C307 . 41.2(2) yes C234 . Fe301 . C307 . 68.2(3) yes C233 . Fe301 . C307 . 40.7(2) yes C230 . Fe301 . C307 . 122.3(4) yes C235 . Fe301 . C302 . 127.8(4) yes C235 . Fe301 . C305 . 124.3(4) yes C302 . Fe301 . C305 . 68.7(4) yes C235 . Fe301 . C306 . 108.5(4) yes C302 . Fe301 . C306 . 42.3(5) yes C305 . Fe301 . C306 . 42.9(4) yes C235 . Fe301 . C307 . 68.7(3) yes C302 . Fe301 . C307 . 119.8(4) yes C305 . Fe301 . C307 . 157.9(4) yes C306 . Fe301 . C307 . 156.6(5) yes Fe301 . C302 . C231 . 72.9(6) yes Fe301 . C302 . C306 . 68.9(5) yes C231 . C302 . C306 . 112.0(10) yes Fe301 . C302 . H3021 . 123.5 no C231 . C302 . H3021 . 123.7 no C306 . C302 . H3021 . 124.2 no O232 . C303 . C304 . 107.9(5) yes O232 . C303 . H3031 . 110.6 no C304 . C303 . H3031 . 109.7 no O232 . C303 . H3032 . 109.5 no C304 . C303 . H3032 . 110.3 no H3031 . C303 . H3032 . 108.9 no C303 . C304 . N229 . 112.5(6) yes C303 . C304 . H3041 . 107.4 no N229 . C304 . H3041 . 108.3 no C303 . C304 . H3042 . 109.5 no N229 . C304 . H3042 . 108.8 no H3041 . C304 . H3042 . 110.3 no C230 . C305 . Fe301 . 71.3(5) yes C230 . C305 . C306 . 105.7(10) yes Fe301 . C305 . C306 . 68.5(5) yes C230 . C305 . H3051 . 127.3 no Fe301 . C305 . H3051 . 126.6 no C306 . C305 . H3051 . 126.9 no C305 . C306 . C302 . 101.8(9) yes C305 . C306 . Fe301 . 68.6(5) yes C302 . C306 . Fe301 . 68.8(5) yes C305 . C306 . H3061 . 130.0 no C302 . C306 . H3061 . 128.0 no Fe301 . C306 . H3061 . 128.9 no C236 . C307 . C233 . 109.5(6) yes C236 . C307 . Fe301 . 70.2(3) yes C233 . C307 . Fe301 . 70.2(4) yes C236 . C307 . H3071 . 125.2 no C233 . C307 . H3071 . 125.2 no Fe301 . C307 . H3071 . 123.2 no C238 . C308 . O232 . 123.5(6) yes C238 . C308 . C309 . 119.1(7) yes O232 . C308 . C309 . 117.4(6) yes C308 . C309 . C310 . 121.2(6) yes C308 . C309 . H3091 . 119.8 no C310 . C309 . H3091 . 119.0 no C309 . C310 . C311 . 119.4(6) yes C309 . C310 . H3101 . 120.6 no C311 . C310 . H3101 . 119.9 no C310 . C311 . O239 . 123.6(6) yes C310 . C311 . C312 . 119.2(7) yes O239 . C311 . C312 . 117.2(6) yes C311 . C312 . C238 . 121.6(6) yes C311 . C312 . H3121 . 119.0 no C238 . C312 . H3121 . 119.4 no C237 . C313 . C241 . 121.8(6) yes C237 . C313 . H3131 . 119.2 no C241 . C313 . H3131 . 119.0 no O242 . C314 . C315 . 107.9(6) yes O242 . C314 . H3141 . 109.7 no C315 . C314 . H3141 . 108.3 no O242 . C314 . H3142 . 109.6 no C315 . C314 . H3142 . 111.0 no H3141 . C314 . H3142 . 110.3 no C314 . C315 . O239 . 108.9(5) yes C314 . C315 . H3151 . 109.9 no O239 . C315 . H3151 . 109.9 no C314 . C315 . H3152 . 109.5 no O239 . C315 . H3152 . 108.8 no H3151 . C315 . H3152 . 109.8 no C243 . C316 . C240 . 123.2(5) yes C243 . C316 . C317 . 117.4(5) yes C240 . C316 . C317 . 119.4(5) yes C237 . C317 . C316 . 121.5(5) yes C237 . C317 . H3171 . 119.4 no C316 . C317 . H3171 . 119.1 no C241 . C318 . O319 . 120.9(6) yes C241 . C318 . N320 . 117.6(5) yes O319 . C318 . N320 . 121.4(6) yes C318 . N320 . C321 . 119.6(5) yes C318 . N320 . H3201 . 120.6 no C321 . N320 . H3201 . 118.3 no N320 . C321 . C322 . 111.7(5) yes N320 . C321 . H3211 . 109.2 no C322 . C321 . H3211 . 109.6 no N320 . C321 . H3212 . 107.5 no C322 . C321 . H3212 . 108.7 no H3211 . C321 . H3212 . 110.0 no C321 . C322 . O323 . 106.7(5) yes C321 . C322 . H3222 . 109.4 no O323 . C322 . H3222 . 109.6 no C321 . C322 . H3221 . 111.4 no O323 . C322 . H3221 . 109.0 no H3222 . C322 . H3221 . 110.7 no C322 . O323 . C324 . 117.0(4) yes O323 . C324 . C325 . 114.9(5) yes O323 . C324 . C329 . 124.6(5) yes C325 . C324 . C329 . 120.5(5) yes C324 . C325 . C326 . 119.3(5) yes C324 . C325 . H3251 . 120.2 no C326 . C325 . H3251 . 120.5 no C325 . C326 . C327 . 120.6(5) yes C325 . C326 . H3261 . 120.0 no C327 . C326 . H3261 . 119.4 no C326 . C327 . C328 . 120.4(5) yes C326 . C327 . O330 . 114.6(5) yes C328 . C327 . O330 . 125.1(5) yes C327 . C328 . C329 . 119.4(5) yes C327 . C328 . H3281 . 120.3 no C329 . C328 . H3281 . 120.3 no C328 . C329 . C324 . 119.9(5) yes C328 . C329 . H3291 . 120.7 no C324 . C329 . H3291 . 119.5 no C327 . O330 . C331 . 116.6(4) yes O330 . C331 . C332 . 107.0(4) yes O330 . C331 . H3311 . 110.5 no C332 . C331 . H3311 . 109.2 no O330 . C331 . H3312 . 111.2 no C332 . C331 . H3312 . 110.5 no H3311 . C331 . H3312 . 108.3 no C331 . C332 . O333 . 108.6(4) yes C331 . C332 . H3321 . 110.1 no O333 . C332 . H3321 . 109.1 no C331 . C332 . H3322 . 110.9 no O333 . C332 . H3322 . 109.1 no H3321 . C332 . H3322 . 109.0 no C332 . O333 . C334 . 113.3(4) yes O333 . C334 . C335 . 113.6(2) yes O333 . C334 . H3341 . 107.3 no C335 . C334 . H3341 . 104.6 no O333 . C334 . H3342 . 108.7 no C335 . C334 . H3342 . 112.8 no H3341 . C334 . H3342 . 109.5 no C334 . C335 . O336 . 119.6(3) yes C334 . C335 . H3351 . 106.6 no O336 . C335 . H3351 . 107.1 no C334 . C335 . H3352 . 108.9 no O336 . C335 . H3352 . 105.6 no H3351 . C335 . H3352 . 108.7 no C335 . O336 . C337 . 107.5(3) yes O336 . C337 . C338 . 104.31(17) yes O336 . C337 . H3371 . 111.0 no C338 . C337 . H3371 . 118.3 no O336 . C337 . H3372 . 105.3 no C338 . C337 . H3372 . 108.4 no H3371 . C337 . H3372 . 108.8 no C337 . C338 . O339 . 115.7(3) yes C337 . C338 . H3381 . 104.9 no O339 . C338 . H3381 . 106.3 no C337 . C338 . H3382 . 105.4 no O339 . C338 . H3382 . 114.6 no H3381 . C338 . H3382 . 109.3 no C338 . O339 . C340 . 110.7(5) yes O339 . C340 . C341 . 109.2(4) yes O339 . C340 . H3401 . 107.8 no C341 . C340 . H3401 . 108.3 no O339 . C340 . H3402 . 111.6 no C341 . C340 . H3402 . 109.9 no H3401 . C340 . H3402 . 110.0 no C340 . C341 . O342 . 108.5(4) yes C340 . C341 . H3411 . 108.5 no O342 . C341 . H3411 . 109.8 no C340 . C341 . H3412 . 110.0 no O342 . C341 . H3412 . 109.3 no H3411 . C341 . H3412 . 110.8 no C341 . O342 . C343 . 115.9(4) yes O342 . C343 . C344 . 115.6(5) yes O342 . C343 . C348 . 124.8(5) yes C344 . C343 . C348 . 119.6(5) yes C343 . C344 . C345 . 120.9(5) yes C343 . C344 . H3441 . 119.0 no C345 . C344 . H3441 . 120.1 no C344 . C345 . C346 . 119.1(5) yes C344 . C345 . H3451 . 120.2 no C346 . C345 . H3451 . 120.8 no C345 . C346 . C347 . 120.7(5) yes C345 . C346 . O349 . 115.7(5) yes C347 . C346 . O349 . 123.7(5) yes C346 . C347 . C348 . 119.7(5) yes C346 . C347 . H3471 . 120.2 no C348 . C347 . H3471 . 120.1 no C347 . C348 . C343 . 120.1(5) yes C347 . C348 . H3481 . 120.1 no C343 . C348 . H3481 . 119.8 no C346 . O349 . C350 . 116.8(4) yes C244 . C350 . O349 . 107.3(4) yes C244 . C350 . H3501 . 109.7 no O349 . C350 . H3501 . 110.4 no C244 . C350 . H3502 . 111.3 no O349 . C350 . H3502 . 109.3 no H3501 . C350 . H3502 . 108.9 no C226 2_566 C351 . C353 . 125.4(7) yes C226 2_566 C351 . H3511 . 117.3 no C353 . C351 . H3511 . 117.2 no C244 . N352 . C243 . 121.2(5) yes C244 . N352 . H3521 . 119.5 no C243 . N352 . H3521 . 119.2 no C351 . C353 . O242 . 113.0(7) yes C351 . C353 . H3531 . 107.8 no O242 . C353 . H3531 . 108.4 no C351 . C353 . H3532 . 110.8 no O242 . C353 . H3532 . 108.0 no H3531 . C353 . H3532 . 108.7 no Cl502 . C501 . Cl503 . 112.0(4) yes Cl502 . C501 . Cl504 . 109.0(4) yes Cl503 . C501 . Cl504 . 110.7(4) yes Cl502 . C501 . H5011 . 107.9 no Cl503 . C501 . H5011 . 108.7 no Cl504 . C501 . H5011 . 108.4 no Cl506 . C505 . Cl507 . 109.4(4) yes Cl506 . C505 . Cl508 . 108.8(4) yes Cl507 . C505 . Cl508 . 108.2(4) yes Cl506 . C505 . H5051 . 110.5 no Cl507 . C505 . H5051 . 110.2 no Cl508 . C505 . H5051 . 109.7 no Cl510 . C509 . Cl511 . 111.3(7) yes Cl510 . C509 . Cl512 . 108.0(7) yes Cl511 . C509 . Cl512 . 109.4(6) yes Cl510 . C509 . H5091 . 108.6 no Cl511 . C509 . H5091 . 109.7 no Cl512 . C509 . H5091 . 109.8 no Cl514 . C513 . Cl515 . 111.9(4) yes Cl514 . C513 . Cl516 . 109.2(4) yes Cl515 . C513 . Cl516 . 110.0(4) yes Cl514 . C513 . H5131 . 108.8 no Cl515 . C513 . H5131 . 109.4 no Cl516 . C513 . H5131 . 107.4 no C205 . C514 . N211 . 115.7(5) yes C205 . C514 . O210 . 120.0(5) yes N211 . C514 . O210 . 124.2(5) yes Cl518 . C517 . Cl519 . 108.920(5) yes Cl518 . C517 . Cl520 . 108.414(5) yes Cl519 . C517 . Cl520 . 110.057(6) yes Cl518 . C517 . H5171 . 109.9 no Cl519 . C517 . H5171 . 110.5 no Cl520 . C517 . H5171 . 109.0 no Cl522 . C521 . Cl523 . 104(4) yes Cl522 . C521 . Cl524 . 107(4) yes Cl523 . C521 . Cl524 . 110(4) yes Cl522 . C521 . H5211 . 114.0 no Cl523 . C521 . H5211 . 112.1 no Cl524 . C521 . H5211 . 109.6 no C334 . C635 . O636 . 108.4(2) yes C334 . C635 . H6352 . 117.0 no O636 . C635 . H6352 . 110.0 no C334 . C635 . H6351 . 116.9 no O636 . C635 . H6351 . 93.4 no H6352 . C635 . H6351 . 108.5 no C635 . O636 . C637 . 129.6(3) yes O636 . C637 . C638 . 109.335(6) yes O636 . C637 . H6371 . 136.1 no C638 . C637 . H6371 . 102.8 no O636 . C637 . H6372 . 91.6 no C638 . C637 . H6372 . 103.4 no H6371 . C637 . H6372 . 109.5 no O339 . C638 . C637 . 124.78(19) yes O339 . C638 . H6382 . 109.8 no C637 . C638 . H6382 . 90.3 no O339 . C638 . H6381 . 107.8 no C637 . C638 . H6381 . 113.2 no H6382 . C638 . H6381 . 109.0 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 C2 . H21 . O139 . 154 0.95 2.41 3.291(10) yes C2 . H22 . O133 . 127 0.97 2.58 3.261(10) yes C2 . H23 . O10 2_666 134 0.96 2.46 3.205(10) yes C4 . H41 . O10 2_666 144 0.93 2.41 3.215(10) yes C26 . H261 . O336 2_567 143 0.95 2.52 3.331(10) yes C30 . H301 . O242 1_655 132 0.97 2.49 3.218(10) yes C43 . H431 . O323 2_667 149 0.97 2.44 3.313(10) yes C137 . H1371 . O239 2_666 165 0.97 2.55 3.496(10) yes C140 . H1402 . O354 2_666 141 0.96 2.51 3.314(10) yes C202 . H2021 . O228 2_567 160 0.95 2.28 3.183(10) yes C202 . H2023 . O333 . 173 0.96 2.30 3.249(10) yes C202 . H2022 . O339 . 152 0.96 2.37 3.254(10) yes C208 . H2081 . O228 2_567 150 0.94 2.36 3.211(10) yes C325 . H3251 . O42 2_667 156 0.94 2.57 3.450(10) yes C332 . H3322 . O119 2_567 144 0.97 2.51 3.348(10) yes C335 . H3351 . O21 2_567 167 0.97 2.56 3.511(10) yes C635 . H3351 . O21 2_567 167 0.97 2.56 3.511(10) yes C501 . H5011 . O154 1_565 137 0.97 2.18 2.964(10) yes C505 . H5051 . O32 1_565 154 0.97 2.29 3.197(10) yes C509 . H5091 . O42 1_565 137 0.98 2.47 3.258(10) yes C513 . H5131 . O319 2_677 144 0.97 2.18 3.020(10) yes C637 . H6371 . O210 2_467 128 0.95 2.52 3.189(10) yes C637 . H6372 . O24 2_567 149 0.95 2.56 3.409(10) yes C637 . H6372 . C25 2_567 174 0.95 2.53 3.476(10) yes # Attachment '- 4 Pseudorotaxane 15Cl 063CJS09.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 853871' #TrackingRef '- 4 Pseudorotaxane 15Cl 063CJS09.cif' _audit_creation_date 10-07-26 _audit_creation_method CRYSTALS_ver_14.07 _oxford_structure_analysis_title 063CJS09 _chemical_name_systematic . _chemical_melting_point . _refine_special_details ; Although the crystals grown were of a reasonable size large, they were found to diffract exceptionally poorly, especially at high angle. Diffraction data were measured using synchrotron radiation at Diamond Light Source I19, but the resultant diffraction pattern was suboptimal nonetheless After partial structure solution using SIR92, cycles of least-squares refinement (F^2) and examination of the Fourier difference map, the whole of the pseudorotaxane could be obtained. The disordered end of one of the thiol chains was modelled over two sites using refined occupancies. Copius restraints were applied (with the aid of MOGUL) to correct unreasonable geometries. Further restraints were used to ensure that anisotropic displacement factors were physically reasonable. Hydrogen atoms were placed geometrically and subsequently restrained using rides. Absent data were pruned using the Wilson plot, and after optimisation of weights, the refinement converged. ; # start Validation Reply Form _vrf_REFNR01_1 ; PROBLEM: Ratio of reflections to parameters is < 6 for a RESPONSE: Due to the poorly crystalline nature of the sample (as evidenced by the degree of disorder and the size of the thermal ellipsoids), data at high angles was absent, even using synchrotron radiation. Refer to supplementary information for a representative frame of the diffraction data. This problem is exacerbated by the large number of atoms present. ; _vrf_THETM01_1 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Due to the poorly crystalline nature of the sample (as evidenced by the degree of disorder and the size of the thermal ellipsoids), data at high angles was absent, even using synchrotron radiation. Refer to supplementary information for a representative frame of the diffraction data. ; _vrf_PLAT071_1 ; PROBLEM: Uninterpretable Atom Label on Input ............ Cl101 RESPONSE: The large number of atoms in this structure necessitates the use of high figures in order to generate a logical numbering scheme. ; _vrf_PLAT731_1 ; PROBLEM: Bond Calc 1.45(2), Rep 1.4498(9) ...... 9.90 su-Ra RESPONSE: Due to the lack of high quality data and the quantity of disorder present, a large number of restraints were used to ensure a chemically reasonable model. This results in a much greater off-diagonal elements in the variance-covariance matrix because the restraints correlate the parameters. Only the diagonal of this matrix is given in the .cif, whereas the bond distances and s.u.s are calculated within CRYSTALS using the full matrix. ; _vrf_PLAT732_1 ; PROBLEM: Angle Calc 120.0(12), Rep 119.98(8) ...... 9.90 su-Ra RESPONSE: Due to the lack of high quality data and the quantity of disorder present, a large number of restraints were used to ensure a chemically reasonable model. This results in a much greater off-diagonal elements in the variance-covariance matrix because the restraints correlate the parameters. Only the diagonal of this matrix is given in the .cif, whereas the bond distances and s.u.s are calculated within CRYSTALS using the full matrix. ; # end Validation Reply Form _cell_length_a 14.2600(10) _cell_length_b 39.5000(10) _cell_length_c 14.2600(10) _cell_angle_alpha 90 _cell_angle_beta 95.550(10) _cell_angle_gamma 90 _cell_volume 7994.6(8) _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' 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' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C95 H115 Cl0.50 Fe1.25 N6.25 O16.25 S2.50 # Dc = 1.47 Fooo = 3176.00 Mu = 3.93 M = 1772.19 # Found Formula = C76 H92.00 Cl1 Fe1 N5 O17 S2 # Dc = 1.25 FOOO = 3176.00 Mu = 3.41 M = 1503.02 _chemical_formula_sum 'C76 H92 Cl1 Fe1 N5 O17 S2' _chemical_formula_moiety 'C34 H46 N3 O8 S2, C42 H46 Fe N2 O9, Cl' _chemical_compound_source . _chemical_formula_weight 1503.02 _cell_measurement_reflns_used 4060 _cell_measurement_theta_min 1 _cell_measurement_theta_max 18 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.010 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.120 _exptl_crystal_density_diffrn 1.249 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 3175.999 _exptl_absorpt_coefficient_mu 0.341 # Sheldrick geometric approximatio 0.97 1.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrystalClear (Rigaku, 1997--2009)' _exptl_absorpt_correction_T_min 0.62 _exptl_absorpt_correction_T_max 1.00 _diffrn_measurement_device_type Unknown _diffrn_measurement_device Serial _diffrn_radiation_monochromator 'Si(1 1 1) double-crystal monochromator' _diffrn_radiation_type Synchrotron _diffrn_radiation_wavelength 0.68890 _diffrn_measurement_method \w-scans # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'CrystalClear (Rigaku, 1997--2009)' _computing_cell_refinement 'CrystalClear (Rigaku, 1997--2009)' _computing_data_reduction 'CrystalClear (Rigaku, 1997--2009)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _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 0 _diffrn_standards_interval_count 0 _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_ambient_temperature 150 _diffrn_reflns_number 28409 _reflns_number_total 6066 _diffrn_reflns_av_R_equivalents 0.114 # Number of reflections without Friedels Law is 6196 # Number of reflections with Friedels Law is 6066 # Theoretical number of reflections is about 12250 _diffrn_reflns_theta_min 1.391 _diffrn_reflns_theta_max 18.082 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 16.635 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 35 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _oxford_diffrn_Wilson_B_factor 6.16 _oxford_diffrn_Wilson_scale 55.02 _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 0.95 # 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>-3.0\s(I) _refine_ls_number_reflns 3210 _refine_ls_number_restraints 1221 _refine_ls_number_parameters 956 _oxford_refine_ls_R_factor_ref 0.1922 _refine_ls_wR_factor_ref 0.3951 _refine_ls_goodness_of_fit_ref 1.0676 _refine_ls_shift/su_max 0.0038820 _refine_ls_shift/su_mean 0.0002137 # The values computed from all data _oxford_reflns_number_all 3210 _refine_ls_R_factor_all 0.1922 _refine_ls_wR_factor_all 0.3951 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 2525 _refine_ls_R_factor_gt 0.1730 _refine_ls_wR_factor_gt 0.3682 # 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: 169. 265. 132. 31.6 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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. Rigaku Americas and Rigaku Corporation. (2009). CrystalClear (Version 2.0). Rigaku Americas, 9009 TX, USA 77381-5209. 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 0.3135(3) 0.24654(9) 0.7516(2) 0.1781 1.0000 Uani D U . . . . . C2 C 0.3163(19) 0.2706(6) 0.6254(12) 0.1934 1.0000 Uani D U . . . . . C3 C 0.2368(19) 0.2786(5) 0.6708(16) 0.1881 1.0000 Uani D U . . . . . C4 C 0.1821(12) 0.2482(6) 0.6803(15) 0.1779 1.0000 Uani D U . . . . . C5 C 0.2336(15) 0.2213(5) 0.6505(13) 0.1805 1.0000 Uani D U . . . . . C6 C 0.3175(17) 0.2366(6) 0.6123(11) 0.1940 1.0000 Uani D U . . . . . C7 C 0.3034(13) 0.2512(5) 0.8915(14) 0.1494 1.0000 Uani D U . . . . . C8 C 0.3330(14) 0.2182(4) 0.8727(14) 0.1544 1.0000 Uani D U . . . . . C9 C 0.4129(16) 0.2205(4) 0.8228(15) 0.1681 1.0000 Uani D U . . . . . C10 C 0.4422(13) 0.2553(4) 0.8240(15) 0.1626 1.0000 Uani D U . . . . . C11 C 0.3689(14) 0.2745(4) 0.8619(13) 0.1535 1.0000 Uani D U . . . . . C12 C 0.3701(12) 0.3116(3) 0.8660(13) 0.1500 1.0000 Uani D U . . . . . C13 C 0.4267(13) 0.3292(3) 0.8085(12) 0.1484 1.0000 Uani D U . . . . . C14 C 0.4253(12) 0.3644(3) 0.8071(12) 0.1366 1.0000 Uani D U . . . . . C15 C 0.3688(10) 0.3820(3) 0.8644(11) 0.1205 1.0000 Uani D U . . . . . C16 C 0.3103(11) 0.3644(3) 0.9200(10) 0.1209 1.0000 Uani D U . . . . . C17 C 0.3116(12) 0.3292(3) 0.9214(12) 0.1445 1.0000 Uani D U . . . . . C18 C 0.2507(13) 0.3805(4) 0.9855(13) 0.1326 1.0000 Uani D U . . . . . O19 O 0.2089(11) 0.3626(3) 1.0384(9) 0.1687 1.0000 Uani D U . . . . . N20 N 0.2339(9) 0.4129(4) 0.9743(9) 0.1266 1.0000 Uani D U . . . . . C21 C 0.1766(12) 0.4316(4) 1.0358(10) 0.1121 1.0000 Uani D U . . . . . C22 C 0.1650(12) 0.4673(5) 1.0082(12) 0.1202 1.0000 Uani . U . . . . . O23 O 0.1018(7) 0.4710(3) 0.9245(8) 0.1178 1.0000 Uani D U . . . . . C24 C 0.0766(10) 0.5038(3) 0.8964(10) 0.1051 1.0000 Uani D U . . . . . C25 C 0.0064(9) 0.5059(3) 0.8222(10) 0.1070 1.0000 Uani D U . . . . . C26 C -0.0270(8) 0.5372(4) 0.7909(8) 0.1044 1.0000 Uani D U . . . . . C27 C 0.0129(11) 0.5665(3) 0.8306(10) 0.1143 1.0000 Uani D U . . . . . C28 C 0.0840(9) 0.5644(3) 0.9041(10) 0.1133 1.0000 Uani D U . . . . . C29 C 0.1178(8) 0.5330(4) 0.9348(8) 0.1144 1.0000 Uani D U . . . . . O30 O -0.0207(8) 0.5954(4) 0.7962(9) 0.1361 1.0000 Uani D U . . . . . C31 C 0.0143(17) 0.6272(6) 0.8335(15) 0.1550 1.0000 Uani . U . . . . . C32 C -0.0427(18) 0.6554(6) 0.7927(14) 0.1633 1.0000 Uani . U . . . . . O33 O -0.0308(9) 0.6569(3) 0.6962(9) 0.1400 1.0000 Uani . U . . . . . C34 C -0.0785(18) 0.6812(7) 0.6478(17) 0.1812 1.0000 Uani . U . . . . . C35 C -0.0847(18) 0.6830(6) 0.5469(17) 0.1798 1.0000 Uani . U . . . . . O36 O 0.0101(10) 0.6847(4) 0.5242(11) 0.1731 1.0000 Uani D U . . . . . C37 C 0.0190(15) 0.6813(6) 0.4251(15) 0.1830 1.0000 Uani D U . . . . . C38 C 0.1210(16) 0.6809(6) 0.4058(16) 0.1738 1.0000 Uani D U . . . . . O39 O 0.1670(10) 0.6530(3) 0.4530(10) 0.1586 1.0000 Uani D U . . . . . C40 C 0.2587(15) 0.6490(6) 0.4240(17) 0.1675 1.0000 Uani . U . . . . . C41 C 0.3038(15) 0.6240(6) 0.4889(17) 0.1604 1.0000 Uani . U . . . . . O42 O 0.2607(7) 0.5898(3) 0.4707(7) 0.1229 1.0000 Uani D U . . . . . C43 C 0.3078(10) 0.5612(3) 0.5063(10) 0.1186 1.0000 Uani D U . . . . . C44 C 0.3864(10) 0.5606(3) 0.5714(10) 0.1170 1.0000 Uani D U . . . . . C45 C 0.4245(8) 0.5299(4) 0.6031(9) 0.1110 1.0000 Uani D U . . . . . C46 C 0.3810(10) 0.4999(3) 0.5735(10) 0.1034 1.0000 Uani D U . . . . . C47 C 0.3026(10) 0.5004(3) 0.5079(10) 0.1155 1.0000 Uani D U . . . . . C48 C 0.2663(8) 0.5310(4) 0.4740(9) 0.1180 1.0000 Uani D U . . . . . O49 O 0.4181(7) 0.4690(3) 0.5990(7) 0.1054 1.0000 Uani D U . . . . . C50 C 0.5063(11) 0.4678(4) 0.6516(11) 0.0992 1.0000 Uani D U . . . . . C51 C 0.5360(10) 0.4313(4) 0.6628(10) 0.1015 1.0000 Uani D U . . . . . N52 N 0.4819(9) 0.4147(4) 0.7304(9) 0.1218 1.0000 Uani D U . . . . . C53 C 0.4916(14) 0.3814(5) 0.7433(15) 0.1373 1.0000 Uani D U . . . . . O54 O 0.5493(10) 0.3663(4) 0.7009(9) 0.1664 1.0000 Uani . U . . . . . Cl101 Cl 0.3501(3) 0.46970(11) 0.8428(3) 0.1015 1.0000 Uani . . . . . . . C102 C 0.0360(11) 0.5960(4) 0.5533(10) 0.1059 1.0000 Uani D U . . . . . N103 N 0.0945(7) 0.5712(2) 0.6094(7) 0.0985 1.0000 Uani D U . . . . . C104 C 0.1661(8) 0.5834(2) 0.6730(8) 0.0873 1.0000 Uani D U . . . . . C105 C 0.2209(7) 0.5610(3) 0.7297(7) 0.0923 1.0000 Uani D U . . . . . C106 C 0.2092(8) 0.5265(3) 0.7172(8) 0.0888 1.0000 Uani D U . . . . . C107 C 0.1386(9) 0.5144(2) 0.6532(9) 0.1019 1.0000 Uani D U . . . . . C108 C 0.0826(8) 0.5370(3) 0.5971(7) 0.0893 1.0000 Uani D U . . . . . C109 C 0.2925(9) 0.5777(5) 0.7972(11) 0.1082 1.0000 Uani D U . . . . . O110 O 0.2898(9) 0.6076(4) 0.8114(11) 0.1726 1.0000 Uani D U . . . . . N111 N 0.3521(9) 0.5557(3) 0.8429(9) 0.1173 1.0000 Uani D U . . . . . C112 C 0.4301(13) 0.5678(5) 0.9138(13) 0.1399 1.0000 Uani D U . . . . . C113 C 0.5076(13) 0.5418(5) 0.9327(13) 0.1351 1.0000 Uani D U . . . . . O114 O 0.5513(9) 0.5461(4) 0.8516(9) 0.1620 1.0000 Uani D U . . . . . C115 C 0.6169(11) 0.5201(4) 0.8338(13) 0.1451 1.0000 Uani D U . . . . . C116 C 0.6767(12) 0.5281(4) 0.7657(12) 0.1547 1.0000 Uani D U . . . . . C117 C 0.7455(11) 0.5052(5) 0.7446(10) 0.1593 1.0000 Uani D U . . . . . C118 C 0.7511(10) 0.4736(4) 0.7878(12) 0.1491 1.0000 Uani D U . . . . . C119 C 0.6925(12) 0.4659(3) 0.8571(12) 0.1444 1.0000 Uani D U . . . . . C120 C 0.6264(11) 0.4894(5) 0.8811(11) 0.1544 1.0000 Uani D U . . . . . O121 O 0.8265(8) 0.4534(4) 0.7557(10) 0.1684 1.0000 Uani D U . . . . . C122 C 0.8329(17) 0.4193(4) 0.7933(18) 0.2022 1.0000 Uani D U . . . . . C123 C 0.9151(18) 0.4036(6) 0.751(2) 0.2383 1.0000 Uani D U . . . . . O124 O 0.9228(16) 0.3691(5) 0.7855(18) 0.2723 1.0000 Uani D U . . . . . C125 C 1.010(2) 0.3657(5) 0.846(2) 0.3253 1.0000 Uani D U . . . . . C126 C 1.033(2) 0.3289(6) 0.860(2) 0.3519 1.0000 Uani D U . . . . . C127 C 1.006(3) 0.3175(4) 0.9541(19) 0.3652 1.0000 Uani D U . . . . . S128 S 1.0162(14) 0.2724(4) 0.9628(14) 0.4290 1.0000 Uani D U . . . . . C129 C 0.1203(11) 0.4775(4) 0.6338(12) 0.1129 1.0000 Uani D U . . . . . O130 O 0.0479(10) 0.4689(3) 0.5854(9) 0.1450 1.0000 Uani D U . . . . . N131 N 0.1810(10) 0.4555(4) 0.6786(9) 0.1145 1.0000 Uani D U . . . . . C132 C 0.1669(13) 0.4188(4) 0.6742(14) 0.1330 1.0000 Uani D U . . . . . C133 C 0.2407(12) 0.4016(5) 0.6195(14) 0.1360 1.0000 Uani D U . . . . . O134 O 0.2121(7) 0.4071(3) 0.5226(9) 0.1362 1.0000 Uani D U . . . . . C135 C 0.2755(8) 0.3957(2) 0.4601(9) 0.1535 1.0000 Uani D U . . . . . C136 C 0.2382(7) 0.3966(2) 0.3667(10) 0.1469 1.0000 Uani D U . . . . . C137 C 0.2883(10) 0.3828(2) 0.2973(8) 0.1778 1.0000 Uani D U . . . . . C138 C 0.3758(9) 0.3682(2) 0.3213(10) 0.1892 1.0000 Uani D U . . . . . C139 C 0.4126(7) 0.36677(18) 0.4151(11) 0.1809 1.0000 Uani D U . . . . . C140 C 0.3639(7) 0.3813(3) 0.4841(9) 0.1748 1.0000 Uani D U . . . . . O141 O 0.4495(12) 0.3604(4) 0.2614(14) 0.2182 1.0000 Uani D U . . . . . C142 C 0.4092(16) 0.3563(9) 0.1648(16) 0.2615 1.0000 Uani D U . . . . . C143 C 0.506(2) 0.3484(7) 0.137(3) 0.3089 1.0000 Uani D U . . . . . O144 O 0.5327(17) 0.3138(6) 0.1191(18) 0.3310 1.0000 Uani D U . . . . . C145 C 0.614(3) 0.3062(15) 0.069(4) 0.3298 0.55(2) Uani D U P . 2 . . C146 C 0.607(3) 0.3250(10) -0.022(2) 0.3609 0.55(2) Uani D U P . 2 . . C147 C 0.704(4) 0.3305(8) -0.053(5) 0.3688 0.55(2) Uani D U P . 2 . . S148 S 0.7398(13) 0.3736(6) -0.0283(14) 0.2786 0.55(2) Uani D U P . 2 . . C165 C 0.567(5) 0.2938(9) 0.044(3) 0.3578 0.45(2) Uani D U P . 1 . . C166 C 0.587(4) 0.2585(9) 0.079(5) 0.3945 0.45(2) Uani D U P . 1 . . C167 C 0.539(7) 0.2335(11) 0.011(4) 0.4185 0.45(2) Uani D U P . 1 . . S168 S 0.546(3) 0.1919(10) 0.062(4) 0.5048 0.45(2) Uani D U P . 1 . . H21 H 0.3620 0.2868 0.6113 0.2642 1.0000 Uiso R . . . . . . H31 H 0.2150 0.3001 0.6892 0.2645 1.0000 Uiso R . . . . . . H41 H 0.1244 0.2452 0.7074 0.2621 1.0000 Uiso R . . . . . . H51 H 0.2185 0.1979 0.6508 0.2625 1.0000 Uiso R . . . . . . H61 H 0.3667 0.2244 0.5870 0.2652 1.0000 Uiso R . . . . . . H71 H 0.2481 0.2575 0.9194 0.2263 1.0000 Uiso R . . . . . . H81 H 0.2993 0.1982 0.8849 0.2317 1.0000 Uiso R . . . . . . H91 H 0.4469 0.2017 0.8022 0.2350 1.0000 Uiso R . . . . . . H101 H 0.4973 0.2636 0.7991 0.2286 1.0000 Uiso R . . . . . . H131 H 0.4678 0.3173 0.7715 0.2005 1.0000 Uiso R . . . . . . H151 H 0.3668 0.4060 0.8631 0.1752 1.0000 Uiso R . . . . . . H171 H 0.2725 0.3170 0.9599 0.2087 1.0000 Uiso R . . . . . . H211 H 0.2024 0.4289 1.0993 0.1306 1.0000 Uiso R . . . . . . H212 H 0.1156 0.4217 1.0278 0.1306 1.0000 Uiso R . . . . . . H221 H 0.1429 0.4800 1.0583 0.1449 1.0000 Uiso R . . . . . . H222 H 0.2248 0.4758 0.9951 0.1449 1.0000 Uiso R . . . . . . H251 H -0.0203 0.4859 0.7935 0.1378 1.0000 Uiso R . . . . . . H261 H -0.0761 0.5389 0.7411 0.1427 1.0000 Uiso R . . . . . . H281 H 0.1097 0.5843 0.9337 0.1361 1.0000 Uiso R . . . . . . H291 H 0.1681 0.5313 0.9834 0.1402 1.0000 Uiso R . . . . . . H311 H 0.0173 0.6270 0.9003 0.1931 1.0000 Uiso R . . . . . . H312 H 0.0754 0.6312 0.8145 0.1931 1.0000 Uiso R . . . . . . H321 H -0.0343 0.6766 0.8242 0.1961 1.0000 Uiso R . . . . . . H322 H -0.1047 0.6473 0.7983 0.1961 1.0000 Uiso R . . . . . . H341 H -0.0458 0.7016 0.6643 0.2159 1.0000 Uiso R . . . . . . H342 H -0.1404 0.6824 0.6669 0.2159 1.0000 Uiso R . . . . . . H351 H -0.1203 0.7003 0.5139 0.2163 1.0000 Uiso R . . . . . . H352 H -0.1099 0.6615 0.5281 0.2163 1.0000 Uiso R . . . . . . H371 H -0.0181 0.6981 0.3914 0.2192 1.0000 Uiso R . . . . . . H372 H -0.0038 0.6595 0.4064 0.2192 1.0000 Uiso R . . . . . . H381 H 0.1477 0.7018 0.4279 0.2153 1.0000 Uiso R . . . . . . H382 H 0.1233 0.6794 0.3396 0.2153 1.0000 Uiso R . . . . . . H401 H 0.2929 0.6696 0.4233 0.2025 1.0000 Uiso R . . . . . . H402 H 0.2519 0.6396 0.3624 0.2025 1.0000 Uiso R . . . . . . H411 H 0.2989 0.6306 0.5524 0.1888 1.0000 Uiso R . . . . . . H412 H 0.3683 0.6229 0.4778 0.1888 1.0000 Uiso R . . . . . . H441 H 0.4132 0.5814 0.5943 0.1418 1.0000 Uiso R . . . . . . H451 H 0.4791 0.5298 0.6469 0.1359 1.0000 Uiso R . . . . . . H471 H 0.2736 0.4797 0.4878 0.1399 1.0000 Uiso R . . . . . . H481 H 0.2117 0.5311 0.4303 0.1462 1.0000 Uiso R . . . . . . H501 H 0.5022 0.4770 0.7127 0.1448 1.0000 Uiso R . . . . . . H502 H 0.5505 0.4804 0.6202 0.1448 1.0000 Uiso R . . . . . . H511 H 0.6013 0.4292 0.6826 0.1337 1.0000 Uiso R . . . . . . H512 H 0.5227 0.4205 0.6034 0.1337 1.0000 Uiso R . . . . . . H1021 H -0.0077 0.5837 0.5116 0.1390 1.0000 Uiso R . . . . . . H1022 H 0.0027 0.6097 0.5936 0.1390 1.0000 Uiso R . . . . . . H1023 H 0.0739 0.6099 0.5179 0.1390 1.0000 Uiso R . . . . . . H1041 H 0.1743 0.6071 0.6814 0.1323 1.0000 Uiso R . . . . . . H1061 H 0.2492 0.5112 0.7534 0.1240 1.0000 Uiso R . . . . . . H1081 H 0.0348 0.5287 0.5519 0.1211 1.0000 Uiso R . . . . . . H1121 H 0.4063 0.5753 0.9702 0.1943 1.0000 Uiso R . . . . . . H1122 H 0.4593 0.5863 0.8851 0.1943 1.0000 Uiso R . . . . . . H1131 H 0.5480 0.5442 0.9893 0.1957 1.0000 Uiso R . . . . . . H1132 H 0.4768 0.5205 0.9325 0.1957 1.0000 Uiso R . . . . . . H1161 H 0.6719 0.5497 0.7366 0.1922 1.0000 Uiso R . . . . . . H1171 H 0.7869 0.5111 0.6990 0.1937 1.0000 Uiso R . . . . . . H1191 H 0.6999 0.4448 0.8890 0.2045 1.0000 Uiso R . . . . . . H1201 H 0.5857 0.4835 0.9275 0.2115 1.0000 Uiso R . . . . . . H1221 H 0.8405 0.4193 0.8602 0.2663 1.0000 Uiso R . . . . . . H1222 H 0.7819 0.4049 0.7719 0.2663 1.0000 Uiso R . . . . . . H1231 H 0.9671 0.4164 0.7787 0.3269 1.0000 Uiso R . . . . . . H1232 H 0.9094 0.4066 0.6848 0.3269 1.0000 Uiso R . . . . . . H1251 H 1.0664 0.3763 0.8322 0.4229 1.0000 Uiso R . . . . . . H1252 H 0.9924 0.3740 0.9048 0.4229 1.0000 Uiso R . . . . . . H1261 H 1.0987 0.3241 0.8661 0.4598 1.0000 Uiso R . . . . . . H1262 H 1.0041 0.3183 0.8049 0.4598 1.0000 Uiso R . . . . . . H1271 H 1.0249 0.3313 1.0072 0.5060 1.0000 Uiso R . . . . . . H1272 H 0.9392 0.3179 0.9424 0.5060 1.0000 Uiso R . . . . . . H1321 H 0.1642 0.4097 0.7355 0.1627 1.0000 Uiso R . . . . . . H1322 H 0.1088 0.4148 0.6375 0.1627 1.0000 Uiso R . . . . . . H1331 H 0.2992 0.4124 0.6372 0.1736 1.0000 Uiso R . . . . . . H1332 H 0.2454 0.3783 0.6359 0.1736 1.0000 Uiso R . . . . . . H1361 H 0.1790 0.4070 0.3492 0.2161 1.0000 Uiso R . . . . . . H1371 H 0.2637 0.3835 0.2330 0.2289 1.0000 Uiso R . . . . . . H1391 H 0.4707 0.3557 0.4328 0.2409 1.0000 Uiso R . . . . . . H1401 H 0.3894 0.3813 0.5482 0.2468 1.0000 Uiso R . . . . . . H1421 H 0.3854 0.3782 0.1482 0.3219 1.0000 Uiso R . . . . . . H1422 H 0.3610 0.3399 0.1511 0.3219 1.0000 Uiso R . . . . . . H1651 H 0.6216 0.3064 0.0642 0.4697 0.45(2) Uiso R . P . 1 . . H1652 H 0.5516 0.2968 -0.0217 0.4697 0.45(2) Uiso R . P . 1 . . H1661 H 0.6445 0.2518 0.0550 0.5033 0.45(2) Uiso R . P . 1 . . H1662 H 0.5923 0.2549 0.1451 0.5033 0.45(2) Uiso R . P . 1 . . H1671 H 0.5353 0.2365 -0.0550 0.5532 0.45(2) Uiso R . P . 1 . . H1672 H 0.4814 0.2408 0.0337 0.5532 0.45(2) Uiso R . P . 1 . . H1111 H 0.3513 0.5342 0.8426 0.1555 1.0000 Uiso R . . . . . . H201 H 0.2630 0.4268 0.9419 0.1456 1.0000 Uiso R . . . . . . H1311 H 0.2260 0.4593 0.7209 0.1377 1.0000 Uiso R . . . . . . H521 H 0.4479 0.4285 0.7582 0.1355 1.0000 Uiso R . . . . . . H1481 H 0.7296 0.3822 0.0618 0.4656 0.55(2) Uiso R . P . 2 . . H1281 H 0.9524 0.2477 0.9410 0.6277 1.0000 Uiso R . . . . . . H1681 H 0.5090 0.1801 0.1395 0.7006 0.45(2) Uiso R . P . 1 . . H1451 H 0.6743 0.3103 0.1024 0.3770 0.55(2) Uiso R . P . 2 . . H1452 H 0.6124 0.2839 0.0445 0.3770 0.55(2) Uiso R . P . 2 . . H1471 H 0.6881 0.3337 -0.1182 0.4141 0.55(2) Uiso R . P . 2 . . H1472 H 0.7420 0.3108 -0.0426 0.4141 0.55(2) Uiso R . P . 2 . . H1461 H 0.5761 0.3458 -0.0136 0.4232 0.55(2) Uiso R . P . 2 . . H1462 H 0.5680 0.3110 -0.0642 0.4232 0.55(2) Uiso R . P . 2 . . H1431 H 0.5499 0.3558 0.1869 0.3547 1.0000 Uiso R . . . . . . H1432 H 0.5118 0.3619 0.0826 0.3547 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 0.221(4) 0.171(3) 0.151(3) 0.0096(19) 0.056(2) 0.007(2) C2 0.274(13) 0.164(11) 0.151(6) 0.004(7) 0.064(8) -0.023(10) C3 0.245(12) 0.167(9) 0.156(10) 0.024(7) 0.042(8) -0.009(7) C4 0.239(7) 0.157(13) 0.142(10) 0.016(9) 0.039(6) -0.001(7) C5 0.236(12) 0.172(10) 0.144(9) 0.006(7) 0.073(8) -0.013(8) C6 0.271(13) 0.164(12) 0.159(4) 0.000(7) 0.085(7) -0.042(10) C7 0.157(10) 0.148(8) 0.151(4) 0.012(7) 0.054(6) 0.004(7) C8 0.158(11) 0.149(6) 0.165(8) 0.014(6) 0.058(7) 0.006(8) C9 0.182(9) 0.149(7) 0.186(11) 0.011(7) 0.083(7) 0.005(6) C10 0.189(6) 0.148(9) 0.164(10) 0.011(8) 0.086(5) 0.005(6) C11 0.169(9) 0.150(6) 0.152(8) 0.016(5) 0.068(6) 0.007(6) C12 0.159(15) 0.150(6) 0.153(13) 0.020(6) 0.077(9) 0.009(7) C13 0.157(15) 0.153(7) 0.148(14) 0.024(12) 0.078(10) 0.016(12) C14 0.124(13) 0.152(7) 0.147(14) 0.019(11) 0.080(9) 0.013(11) C15 0.100(14) 0.161(11) 0.108(14) 0.013(9) 0.050(8) 0.008(9) C16 0.127(13) 0.160(7) 0.083(11) 0.034(10) 0.050(8) 0.025(10) C17 0.161(15) 0.159(7) 0.124(13) 0.017(11) 0.068(10) 0.005(12) C18 0.134(14) 0.176(9) 0.098(14) 0.041(10) 0.059(8) 0.041(11) O19 0.226(15) 0.173(10) 0.127(11) 0.033(9) 0.120(10) 0.039(10) N20 0.117(11) 0.167(9) 0.104(10) 0.023(9) 0.049(8) 0.025(10) C21 0.099(12) 0.173(10) 0.065(10) -0.005(8) 0.014(8) 0.007(9) C22 0.096(12) 0.180(10) 0.090(11) 0.006(9) 0.031(7) 0.026(11) O23 0.088(8) 0.176(8) 0.093(8) 0.020(8) 0.031(6) 0.007(8) C24 0.063(11) 0.168(8) 0.088(12) 0.010(9) 0.027(6) -0.003(9) C25 0.038(10) 0.178(9) 0.109(12) 0.017(9) 0.027(6) -0.009(9) C26 0.078(11) 0.180(9) 0.060(10) 0.004(9) 0.035(7) 0.009(9) C27 0.078(12) 0.179(9) 0.094(13) -0.018(9) 0.046(6) 0.021(9) C28 0.048(11) 0.171(8) 0.127(13) -0.017(10) 0.041(6) -0.002(9) C29 0.071(11) 0.179(9) 0.098(11) -0.036(10) 0.030(7) 0.023(10) O30 0.110(9) 0.179(9) 0.124(10) -0.001(8) 0.039(7) 0.014(8) C31 0.179(17) 0.179(10) 0.112(12) -0.001(11) 0.041(12) 0.003(12) C32 0.209(17) 0.178(10) 0.110(10) -0.001(13) 0.051(14) 0.016(13) O33 0.133(10) 0.174(11) 0.126(10) 0.015(9) 0.077(9) 0.038(8) C34 0.177(17) 0.214(18) 0.162(12) 0.056(14) 0.066(14) 0.047(13) C35 0.158(12) 0.229(17) 0.164(13) 0.067(14) 0.074(15) 0.045(15) O36 0.143(10) 0.220(12) 0.164(10) 0.049(11) 0.056(11) 0.063(10) C37 0.154(12) 0.242(18) 0.165(11) 0.075(15) 0.074(15) 0.048(13) C38 0.155(13) 0.187(17) 0.191(16) 0.048(13) 0.080(13) 0.033(13) O39 0.139(10) 0.166(11) 0.182(12) 0.033(9) 0.077(10) 0.020(9) C40 0.145(13) 0.178(10) 0.193(17) 0.039(12) 0.086(13) 0.023(12) C41 0.131(12) 0.173(7) 0.186(16) 0.021(11) 0.060(12) 0.014(8) O42 0.094(7) 0.175(7) 0.108(7) 0.022(6) 0.053(5) 0.023(5) C43 0.088(7) 0.174(7) 0.102(7) 0.021(6) 0.056(5) 0.021(5) C44 0.087(7) 0.172(7) 0.101(7) 0.020(6) 0.057(5) 0.018(6) C45 0.072(10) 0.163(8) 0.105(11) 0.015(10) 0.048(7) 0.005(8) C46 0.063(11) 0.169(7) 0.087(11) 0.015(10) 0.050(6) 0.003(8) C47 0.083(11) 0.172(8) 0.096(12) 0.011(9) 0.034(6) 0.017(8) C48 0.087(7) 0.175(7) 0.101(7) 0.020(6) 0.054(5) 0.022(6) O49 0.071(7) 0.165(7) 0.086(8) 0.001(7) 0.036(5) 0.006(7) C50 0.081(9) 0.158(9) 0.064(10) -0.001(9) 0.033(7) 0.006(9) C51 0.078(10) 0.157(9) 0.076(10) -0.007(8) 0.036(8) 0.006(8) N52 0.119(11) 0.158(8) 0.094(10) -0.011(9) 0.036(8) -0.042(9) C53 0.115(14) 0.172(9) 0.136(15) 0.019(12) 0.071(9) 0.007(11) O54 0.157(13) 0.213(10) 0.145(11) 0.017(10) 0.099(9) 0.022(9) Cl101 0.070(3) 0.157(4) 0.082(3) 0.010(3) 0.030(2) -0.002(3) C102 0.086(11) 0.146(10) 0.088(12) 0.017(9) 0.025(7) -0.007(9) N103 0.058(9) 0.140(7) 0.101(10) 0.012(8) 0.025(5) -0.013(7) C104 0.056(10) 0.133(9) 0.079(12) -0.011(7) 0.041(5) 0.001(7) C105 0.057(10) 0.148(7) 0.078(10) 0.006(8) 0.038(5) -0.010(8) C106 0.081(10) 0.146(7) 0.044(9) 0.007(8) 0.030(6) 0.000(8) C107 0.094(12) 0.143(7) 0.069(11) 0.016(8) 0.015(6) -0.013(8) C108 0.069(10) 0.141(7) 0.061(10) 0.019(9) 0.022(7) -0.024(9) C109 0.076(12) 0.158(10) 0.094(12) -0.002(10) 0.024(6) -0.010(9) O110 0.133(11) 0.162(10) 0.211(14) -0.023(11) -0.050(10) -0.002(9) N111 0.091(11) 0.168(11) 0.093(11) -0.007(8) 0.011(6) -0.004(8) C112 0.130(12) 0.155(14) 0.128(13) -0.037(11) -0.023(6) 0.020(8) C113 0.100(12) 0.177(14) 0.129(12) 0.034(11) 0.014(7) 0.010(9) O114 0.118(11) 0.263(12) 0.105(9) -0.007(10) 0.010(7) 0.003(8) C115 0.091(13) 0.234(14) 0.109(13) -0.012(10) 0.002(8) -0.024(9) C116 0.098(14) 0.237(14) 0.130(14) 0.006(11) 0.015(9) -0.010(9) C117 0.116(14) 0.243(15) 0.120(14) 0.001(12) 0.020(10) -0.003(10) C118 0.109(13) 0.216(12) 0.121(15) -0.027(10) 0.005(8) -0.023(9) C119 0.113(15) 0.185(12) 0.135(14) -0.041(10) 0.008(9) -0.059(8) C120 0.097(14) 0.231(15) 0.136(14) -0.006(11) 0.015(10) -0.033(10) O121 0.124(10) 0.231(12) 0.149(11) -0.032(10) 0.013(9) -0.010(8) C122 0.158(16) 0.242(15) 0.205(19) -0.010(15) 0.008(14) 0.013(13) C123 0.193(18) 0.261(16) 0.26(2) -0.025(17) 0.031(15) 0.036(14) O124 0.242(17) 0.262(15) 0.31(2) -0.016(16) 0.029(14) 0.050(14) C125 0.29(2) 0.314(19) 0.36(3) 0.04(2) -0.019(19) 0.05(2) C126 0.33(3) 0.32(2) 0.39(3) 0.014(19) -0.03(3) 0.081(19) C127 0.39(3) 0.273(13) 0.42(3) 0.03(2) -0.02(3) 0.04(3) S128 0.52(2) 0.264(11) 0.49(2) -0.010(13) -0.027(19) 0.020(14) C129 0.092(13) 0.143(7) 0.106(14) 0.024(9) 0.022(8) -0.025(8) O130 0.161(12) 0.143(9) 0.120(10) 0.024(7) -0.040(8) -0.024(7) N131 0.102(10) 0.138(7) 0.103(10) 0.004(9) 0.008(7) -0.019(8) C132 0.117(13) 0.137(7) 0.137(10) -0.007(11) -0.024(10) -0.012(9) C133 0.099(13) 0.139(12) 0.160(9) -0.013(12) -0.035(9) -0.005(10) O134 0.076(8) 0.174(10) 0.155(8) -0.004(9) -0.011(7) 0.016(8) C135 0.071(10) 0.199(15) 0.189(10) -0.006(13) 0.008(8) 0.010(10) C136 0.107(12) 0.169(16) 0.169(10) 0.012(13) 0.036(9) 0.001(10) C137 0.171(14) 0.167(17) 0.204(12) 0.010(13) 0.059(10) 0.045(13) C138 0.136(14) 0.174(15) 0.264(13) -0.021(15) 0.053(9) 0.015(12) C139 0.100(12) 0.148(15) 0.292(14) -0.085(15) 0.004(10) 0.005(10) C140 0.082(11) 0.163(16) 0.270(14) -0.099(13) -0.03(1) 0.017(10) O141 0.151(13) 0.186(12) 0.332(16) -0.018(14) 0.098(11) -0.002(10) C142 0.21(2) 0.28(2) 0.307(16) -0.05(2) 0.136(15) -0.037(18) C143 0.224(19) 0.35(2) 0.38(2) -0.07(2) 0.147(18) -0.02(2) O144 0.239(19) 0.37(2) 0.40(2) -0.10(2) 0.127(17) 0.001(18) C145 0.24(3) 0.39(3) 0.38(3) -0.09(3) 0.12(2) 0.01(2) C146 0.27(3) 0.42(3) 0.41(3) -0.06(3) 0.12(3) -0.04(2) C147 0.24(3) 0.44(3) 0.44(4) -0.02(4) 0.07(3) -0.07(3) S148 0.207(17) 0.39(3) 0.241(19) 0.036(17) 0.012(13) 0.010(15) C165 0.26(3) 0.41(3) 0.43(4) -0.08(3) 0.16(3) 0.06(3) C166 0.30(4) 0.42(3) 0.48(5) -0.09(3) 0.12(4) 0.10(3) C167 0.33(4) 0.41(3) 0.52(5) -0.08(3) 0.09(4) 0.07(4) S168 0.40(4) 0.42(3) 0.69(7) -0.02(4) 0.06(4) 0.06(4) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2233(10) 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 . C2 . 2.038(14) yes Fe1 . C3 . 1.97(2) yes Fe1 . C4 . 2.045(15) yes Fe1 . C5 . 2.014(14) yes Fe1 . C6 . 2.031(14) yes Fe1 . C7 . 2.022(19) yes Fe1 . C8 . 2.053(19) yes Fe1 . C9 . 1.95(2) yes Fe1 . C10 . 2.05(2) yes Fe1 . C11 . 2.02(2) yes C2 . C3 . 1.40(3) yes C2 . C6 . 1.36(3) yes C2 . H21 . 0.950 no C3 . C4 . 1.44(2) yes C3 . H31 . 0.950 no C4 . C5 . 1.38(3) yes C4 . H41 . 0.950 no C5 . C6 . 1.49(2) yes C5 . H51 . 0.950 no C6 . H61 . 0.950 no C7 . C8 . 1.403(14) yes C7 . C11 . 1.41(2) yes C7 . H71 . 0.950 no C8 . C9 . 1.40(2) yes C8 . H81 . 0.950 no C9 . C10 . 1.435(14) yes C9 . H91 . 0.950 no C10 . C11 . 1.439(13) yes C10 . H101 . 0.950 no C11 . C12 . 1.466(18) yes C12 . C13 . 1.390(7) yes C12 . C17 . 1.390(7) yes C13 . C14 . 1.392(7) yes C13 . H131 . 0.950 no C14 . C15 . 1.388(7) yes C14 . C53 . 1.53(2) yes C15 . C16 . 1.391(7) yes C15 . H151 . 0.950 no C16 . C17 . 1.391(7) yes C16 . C18 . 1.468(13) yes C17 . H171 . 0.950 no C18 . O19 . 1.230(12) yes C18 . N20 . 1.310(13) yes N20 . C21 . 1.456(14) yes N20 . H201 . 0.850 no C21 . C22 . 1.47(2) yes C21 . H211 . 0.950 no C21 . H212 . 0.950 no C22 . O23 . 1.433(18) yes C22 . H221 . 0.950 no C22 . H222 . 0.950 no O23 . C24 . 1.391(13) yes C24 . C25 . 1.387(7) yes C24 . C29 . 1.386(7) yes C25 . C26 . 1.386(7) yes C25 . H251 . 0.950 no C26 . C27 . 1.387(7) yes C26 . H261 . 0.950 no C27 . C28 . 1.387(7) yes C27 . O30 . 1.315(15) yes C28 . C29 . 1.386(7) yes C28 . H281 . 0.950 no C29 . H291 . 0.950 no O30 . C31 . 1.43(2) yes C31 . C32 . 1.47(3) yes C31 . H311 . 0.950 no C31 . H312 . 0.950 no C32 . O33 . 1.40(2) yes C32 . H321 . 0.950 no C32 . H322 . 0.950 no O33 . C34 . 1.33(2) yes C34 . C35 . 1.43(3) yes C34 . H341 . 0.950 no C34 . H342 . 0.950 no C35 . O36 . 1.42(2) yes C35 . H351 . 0.950 no C35 . H352 . 0.950 no O36 . C37 . 1.437(19) yes C37 . C38 . 1.51(3) yes C37 . H371 . 0.950 no C37 . H372 . 0.950 no C38 . O39 . 1.42(2) yes C38 . H381 . 0.950 no C38 . H382 . 0.950 no O39 . C40 . 1.42(2) yes C40 . C41 . 1.46(3) yes C40 . H401 . 0.950 no C40 . H402 . 0.950 no C41 . O42 . 1.50(2) yes C41 . H411 . 0.950 no C41 . H412 . 0.950 no O42 . C43 . 1.387(11) yes C43 . C44 . 1.385(7) yes C43 . C48 . 1.388(7) yes C44 . C45 . 1.384(7) yes C44 . H441 . 0.950 no C45 . C46 . 1.386(7) yes C45 . H451 . 0.950 no C46 . C47 . 1.387(7) yes C46 . O49 . 1.364(13) yes C47 . C48 . 1.383(7) yes C47 . H471 . 0.950 no C48 . H481 . 0.950 no O49 . C50 . 1.401(17) yes C50 . C51 . 1.507(19) yes C50 . H501 . 0.950 no C50 . H502 . 0.950 no C51 . N52 . 1.448(13) yes C51 . H511 . 0.950 no C51 . H512 . 0.950 no N52 . C53 . 1.334(15) yes N52 . H521 . 0.850 no C53 . O54 . 1.222(18) yes C102 . N103 . 1.470(16) yes C102 . H1021 . 0.950 no C102 . H1022 . 0.950 no C102 . H1023 . 0.950 no N103 . C104 . 1.384(6) yes N103 . C108 . 1.372(6) yes C104 . C105 . 1.387(6) yes C104 . H1041 . 0.950 no C105 . C106 . 1.381(6) yes C105 . C109 . 1.489(14) yes C106 . C107 . 1.378(6) yes C106 . H1061 . 0.950 no C107 . C108 . 1.397(6) yes C107 . C129 . 1.504(17) yes C108 . H1081 . 0.950 no C109 . O110 . 1.199(17) yes C109 . N111 . 1.341(13) yes N111 . C112 . 1.508(19) yes N111 . H1111 . 0.850 no C112 . C113 . 1.51(2) yes C112 . H1121 . 0.950 no C112 . H1122 . 0.950 no C113 . O114 . 1.376(16) yes C113 . H1131 . 0.950 no C113 . H1132 . 0.950 no O114 . C115 . 1.428(17) yes C115 . C116 . 1.388(7) yes C115 . C120 . 1.390(7) yes C116 . C117 . 1.388(7) yes C116 . H1161 . 0.950 no C117 . C118 . 1.388(7) yes C117 . H1171 . 0.950 no C118 . C119 . 1.389(7) yes C118 . O121 . 1.4498(9) yes C119 . C120 . 1.388(7) yes C119 . H1191 . 0.950 no C120 . H1201 . 0.950 no O121 . C122 . 1.4500(9) yes C122 . C123 . 1.5000(9) yes C122 . H1221 . 0.950 no C122 . H1222 . 0.950 no C123 . O124 . 1.4500(9) yes C123 . H1231 . 0.950 no C123 . H1232 . 0.950 no O124 . C125 . 1.4499(9) yes C125 . C126 . 1.5000(9) yes C125 . H1251 . 0.950 no C125 . H1252 . 0.950 no C126 . C127 . 1.5000(9) yes C126 . H1261 . 0.950 no C126 . H1262 . 0.950 no C127 . S128 . 1.789(8) yes C127 . H1271 . 0.950 no C127 . H1272 . 0.950 no S128 . H1281 . 1.350 no C129 . O130 . 1.232(12) yes C129 . N131 . 1.344(17) yes N131 . C132 . 1.462(18) yes N131 . H1311 . 0.850 no C132 . C133 . 1.53(2) yes C132 . H1321 . 0.950 no C132 . H1322 . 0.950 no C133 . O134 . 1.42(2) yes C133 . H1331 . 0.950 no C133 . H1332 . 0.950 no O134 . C135 . 1.403(12) yes C135 . C136 . 1.386(7) yes C135 . C140 . 1.396(7) yes C136 . C137 . 1.386(7) yes C136 . H1361 . 0.950 no C137 . C138 . 1.389(7) yes C137 . H1371 . 0.950 no C138 . C139 . 1.389(7) yes C138 . O141 . 1.4499(9) yes C139 . C140 . 1.382(7) yes C139 . H1391 . 0.950 no C140 . H1401 . 0.950 no O141 . C142 . 1.4500(9) yes C142 . C143 . 1.5000(9) yes C142 . H1421 . 0.950 no C142 . H1422 . 0.950 no C143 . O144 . 1.4499(9) yes C143 . H1431 . 0.950 no C143 . H1432 . 0.950 no O144 . C165 . 1.4500(9) yes C145 . C146 . 1.5001(9) yes C145 . H1451 . 0.950 no C145 . H1452 . 0.950 no C146 . C147 . 1.5000(9) yes C146 . H1461 . 0.950 no C146 . H1462 . 0.950 no C147 . S148 . 1.803(9) yes C147 . H1471 . 0.950 no C147 . H1472 . 0.950 no S148 . H1481 . 1.350 no C165 . C166 . 1.5000(9) yes C165 . H1651 . 0.950 no C165 . H1652 . 0.950 no C166 . C167 . 1.5000(9) yes C166 . H1661 . 0.950 no C166 . H1662 . 0.950 no C167 . S168 . 1.798(9) yes C167 . H1671 . 0.950 no C167 . H1672 . 0.950 no S168 . H1681 . 1.350 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 C2 . Fe1 . C3 . 40.7(8) yes C2 . Fe1 . C4 . 68.9(9) yes C3 . Fe1 . C4 . 42.1(6) yes C2 . Fe1 . C5 . 69.9(8) yes C3 . Fe1 . C5 . 69.8(9) yes C4 . Fe1 . C5 . 39.8(8) yes C2 . Fe1 . C6 . 38.9(8) yes C3 . Fe1 . C6 . 67.6(9) yes C4 . Fe1 . C6 . 68.3(9) yes C5 . Fe1 . C6 . 43.2(6) yes C2 . Fe1 . C7 . 146.9(9) yes C3 . Fe1 . C7 . 115.4(9) yes C4 . Fe1 . C7 . 109.7(8) yes C5 . Fe1 . C7 . 131.4(8) yes C6 . Fe1 . C7 . 173.5(9) yes C2 . Fe1 . C8 . 169.6(10) yes C3 . Fe1 . C8 . 149.7(9) yes C4 . Fe1 . C8 . 118.6(8) yes C5 . Fe1 . C8 . 110.7(8) yes C6 . Fe1 . C8 . 134.6(9) yes C2 . Fe1 . C9 . 129.0(10) yes C3 . Fe1 . C9 . 167.3(9) yes C4 . Fe1 . C9 . 149.3(8) yes C5 . Fe1 . C9 . 116.3(9) yes C6 . Fe1 . C9 . 108.6(9) yes C2 . Fe1 . C10 . 105.9(9) yes C3 . Fe1 . C10 . 127.4(8) yes C4 . Fe1 . C10 . 168.4(8) yes C5 . Fe1 . C10 . 149.6(8) yes C6 . Fe1 . C10 . 114.7(8) yes C2 . Fe1 . C11 . 113.2(9) yes C3 . Fe1 . C11 . 104.9(8) yes C4 . Fe1 . C11 . 129.8(8) yes C5 . Fe1 . C11 . 168.6(8) yes C6 . Fe1 . C11 . 145.3(8) yes C7 . Fe1 . C8 . 40.3(5) yes C7 . Fe1 . C9 . 69.7(7) yes C8 . Fe1 . C9 . 40.9(7) yes C7 . Fe1 . C10 . 68.5(7) yes C8 . Fe1 . C10 . 68.1(7) yes C9 . Fe1 . C10 . 42.0(5) yes C7 . Fe1 . C11 . 40.7(6) yes C8 . Fe1 . C11 . 68.4(7) yes C9 . Fe1 . C11 . 70.9(7) yes C10 . Fe1 . C11 . 41.5(5) yes Fe1 . C2 . C3 . 67.1(11) yes Fe1 . C2 . C6 . 70.3(9) yes C3 . C2 . C6 . 108.1(15) yes Fe1 . C2 . H21 . 124.9 no C3 . C2 . H21 . 123.4 no C6 . C2 . H21 . 128.4 no C2 . C3 . Fe1 . 72.2(12) yes C2 . C3 . C4 . 109.0(14) yes Fe1 . C3 . C4 . 71.7(10) yes C2 . C3 . H31 . 129.2 no Fe1 . C3 . H31 . 126.2 no C4 . C3 . H31 . 121.6 no C3 . C4 . Fe1 . 66.2(11) yes C3 . C4 . C5 . 107.6(17) yes Fe1 . C4 . C5 . 68.9(9) yes C3 . C4 . H41 . 129.8 no Fe1 . C4 . H41 . 125.6 no C5 . C4 . H41 . 122.2 no C4 . C5 . Fe1 . 71.3(9) yes C4 . C5 . C6 . 105.6(16) yes Fe1 . C5 . C6 . 69.0(8) yes C4 . C5 . H51 . 128.4 no Fe1 . C5 . H51 . 126.3 no C6 . C5 . H51 . 125.9 no C5 . C6 . Fe1 . 67.8(8) yes C5 . C6 . C2 . 109.3(13) yes Fe1 . C6 . C2 . 70.8(9) yes C5 . C6 . H61 . 125.7 no Fe1 . C6 . H61 . 124.1 no C2 . C6 . H61 . 124.9 no Fe1 . C7 . C8 . 71.1(10) yes Fe1 . C7 . C11 . 69.5(11) yes C8 . C7 . C11 . 109.3(9) yes Fe1 . C7 . H71 . 125.3 no C8 . C7 . H71 . 126.9 no C11 . C7 . H71 . 123.8 no C7 . C8 . Fe1 . 68.7(10) yes C7 . C8 . C9 . 108.1(8) yes Fe1 . C8 . C9 . 65.7(11) yes C7 . C8 . H81 . 124.8 no Fe1 . C8 . H81 . 125.4 no C9 . C8 . H81 . 126.6 no C8 . C9 . Fe1 . 73.4(12) yes C8 . C9 . C10 . 107.8(8) yes Fe1 . C9 . C10 . 72.5(11) yes C8 . C9 . H91 . 124.7 no Fe1 . C9 . H91 . 128.2 no C10 . C9 . H91 . 126.6 no C9 . C10 . Fe1 . 65.6(11) yes C9 . C10 . C11 . 106.7(9) yes Fe1 . C10 . C11 . 68.3(11) yes C9 . C10 . H101 . 125.1 no Fe1 . C10 . H101 . 127.1 no C11 . C10 . H101 . 128.0 no C10 . C11 . C7 . 107.2(12) yes C10 . C11 . Fe1 . 70.3(11) yes C7 . C11 . Fe1 . 69.8(12) yes C10 . C11 . C12 . 122.4(12) yes C7 . C11 . C12 . 130.4(12) yes Fe1 . C11 . C12 . 125.4(15) yes C11 . C12 . C13 . 118.8(6) yes C11 . C12 . C17 . 121.1(6) yes C13 . C12 . C17 . 119.98(8) yes C12 . C13 . C14 . 119.99(8) yes C12 . C13 . H131 . 120.4 no C14 . C13 . H131 . 119.6 no C13 . C14 . C15 . 119.99(8) yes C13 . C14 . C53 . 116.0(10) yes C15 . C14 . C53 . 123.9(10) yes C14 . C15 . C16 . 119.98(8) yes C14 . C15 . H151 . 120.4 no C16 . C15 . H151 . 119.5 no C15 . C16 . C17 . 119.99(8) yes C15 . C16 . C18 . 124.2(9) yes C17 . C16 . C18 . 115.7(9) yes C16 . C17 . C12 . 120.00(8) yes C16 . C17 . H171 . 120.5 no C12 . C17 . H171 . 119.5 no C16 . C18 . O19 . 119.0(11) yes C16 . C18 . N20 . 117.2(12) yes O19 . C18 . N20 . 123.0(12) yes C18 . N20 . C21 . 121.9(12) yes C18 . N20 . H201 . 127.2 no C21 . N20 . H201 . 109.4 no N20 . C21 . C22 . 112.3(14) yes N20 . C21 . H211 . 109.1 no C22 . C21 . H211 . 112.8 no N20 . C21 . H212 . 106.2 no C22 . C21 . H212 . 106.6 no H211 . C21 . H212 . 109.5 no C21 . C22 . O23 . 111.4(16) yes C21 . C22 . H221 . 110.0 no O23 . C22 . H221 . 110.1 no C21 . C22 . H222 . 108.1 no O23 . C22 . H222 . 107.7 no H221 . C22 . H222 . 109.5 no C22 . O23 . C24 . 117.3(14) yes O23 . C24 . C25 . 115.0(12) yes O23 . C24 . C29 . 125.0(12) yes C25 . C24 . C29 . 119.97(8) yes C24 . C25 . C26 . 119.97(8) yes C24 . C25 . H251 . 120.6 no C26 . C25 . H251 . 119.4 no C25 . C26 . C27 . 119.97(8) yes C25 . C26 . H261 . 120.6 no C27 . C26 . H261 . 119.4 no C26 . C27 . C28 . 119.96(8) yes C26 . C27 . O30 . 116.8(13) yes C28 . C27 . O30 . 123.2(13) yes C27 . C28 . C29 . 119.96(8) yes C27 . C28 . H281 . 120.6 no C29 . C28 . H281 . 119.5 no C28 . C29 . C24 . 119.96(8) yes C28 . C29 . H291 . 120.6 no C24 . C29 . H291 . 119.4 no C27 . O30 . C31 . 121.3(16) yes O30 . C31 . C32 . 111(2) yes O30 . C31 . H311 . 110.2 no C32 . C31 . H311 . 111.8 no O30 . C31 . H312 . 109.7 no C32 . C31 . H312 . 104.4 no H311 . C31 . H312 . 109.5 no C31 . C32 . O33 . 107.7(19) yes C31 . C32 . H321 . 116.2 no O33 . C32 . H321 . 113.9 no C31 . C32 . H322 . 101.2 no O33 . C32 . H322 . 107.3 no H321 . C32 . H322 . 109.5 no C32 . O33 . C34 . 115.7(19) yes O33 . C34 . C35 . 122(2) yes O33 . C34 . H341 . 105.7 no C35 . C34 . H341 . 100.8 no O33 . C34 . H342 . 109.3 no C35 . C34 . H342 . 108.4 no H341 . C34 . H342 . 109.5 no C34 . C35 . O36 . 105(2) yes C34 . C35 . H351 . 120.7 no O36 . C35 . H351 . 109.1 no C34 . C35 . H352 . 103.0 no O36 . C35 . H352 . 108.7 no H351 . C35 . H352 . 109.5 no C35 . O36 . C37 . 113.4(18) yes O36 . C37 . C38 . 111.1(19) yes O36 . C37 . H371 . 109.5 no C38 . C37 . H371 . 114.5 no O36 . C37 . H372 . 107.4 no C38 . C37 . H372 . 104.5 no H371 . C37 . H372 . 109.5 no C37 . C38 . O39 . 109.3(16) yes C37 . C38 . H381 . 107.0 no O39 . C38 . H381 . 111.5 no C37 . C38 . H382 . 108.0 no O39 . C38 . H382 . 111.3 no H381 . C38 . H382 . 109.5 no C38 . O39 . C40 . 110.1(16) yes O39 . C40 . C41 . 104.6(16) yes O39 . C40 . H401 . 113.4 no C41 . C40 . H401 . 113.1 no O39 . C40 . H402 . 107.3 no C41 . C40 . H402 . 108.7 no H401 . C40 . H402 . 109.5 no C40 . C41 . O42 . 111(2) yes C40 . C41 . H411 . 110.7 no O42 . C41 . H411 . 110.1 no C40 . C41 . H412 . 107.6 no O42 . C41 . H412 . 108.3 no H411 . C41 . H412 . 109.5 no C41 . O42 . C43 . 119.9(14) yes O42 . C43 . C44 . 126.2(12) yes O42 . C43 . C48 . 113.7(12) yes C44 . C43 . C48 . 119.99(8) yes C43 . C44 . C45 . 119.98(8) yes C43 . C44 . H441 . 119.2 no C45 . C44 . H441 . 120.8 no C44 . C45 . C46 . 119.98(8) yes C44 . C45 . H451 . 119.3 no C46 . C45 . H451 . 120.7 no C45 . C46 . C47 . 119.97(8) yes C45 . C46 . O49 . 122.3(12) yes C47 . C46 . O49 . 117.4(12) yes C46 . C47 . C48 . 119.98(8) yes C46 . C47 . H471 . 119.3 no C48 . C47 . H471 . 120.7 no C43 . C48 . C47 . 120.00(8) yes C43 . C48 . H481 . 120.7 no C47 . C48 . H481 . 119.3 no C46 . O49 . C50 . 118.5(14) yes O49 . C50 . C51 . 108.5(14) yes O49 . C50 . H501 . 110.3 no C51 . C50 . H501 . 108.1 no O49 . C50 . H502 . 109.4 no C51 . C50 . H502 . 111.1 no H501 . C50 . H502 . 109.5 no C50 . C51 . N52 . 109.8(11) yes C50 . C51 . H511 . 111.7 no N52 . C51 . H511 . 109.5 no C50 . C51 . H512 . 107.7 no N52 . C51 . H512 . 108.5 no H511 . C51 . H512 . 109.5 no C51 . N52 . C53 . 118.8(13) yes C51 . N52 . H521 . 112.8 no C53 . N52 . H521 . 128.4 no C14 . C53 . N52 . 116.9(16) yes C14 . C53 . O54 . 124.3(17) yes N52 . C53 . O54 . 118.7(18) yes N103 . C102 . H1021 . 107.8 no N103 . C102 . H1022 . 109.9 no H1021 . C102 . H1022 . 109.5 no N103 . C102 . H1023 . 110.6 no H1021 . C102 . H1023 . 109.5 no H1022 . C102 . H1023 . 109.5 no C102 . N103 . C104 . 118.1(8) yes C102 . N103 . C108 . 121.9(8) yes C104 . N103 . C108 . 119.98(8) yes N103 . C104 . C105 . 119.97(8) yes N103 . C104 . H1041 . 119.9 no C105 . C104 . H1041 . 119.9 no C104 . C105 . C106 . 119.93(8) yes C104 . C105 . C109 . 114.0(9) yes C106 . C105 . C109 . 126.0(9) yes C105 . C106 . C107 . 119.92(8) yes C105 . C106 . H1061 . 120.0 no C107 . C106 . H1061 . 120.0 no C106 . C107 . C108 . 119.91(8) yes C106 . C107 . C129 . 124.1(9) yes C108 . C107 . C129 . 115.8(9) yes C107 . C108 . N103 . 119.96(8) yes C107 . C108 . H1081 . 120.0 no N103 . C108 . H1081 . 120.0 no C105 . C109 . O110 . 121.0(10) yes C105 . C109 . N111 . 112.9(15) yes O110 . C109 . N111 . 125.9(15) yes C109 . N111 . C112 . 120.7(12) yes C109 . N111 . H1111 . 129.8 no C112 . N111 . H1111 . 109.3 no N111 . C112 . C113 . 112.4(14) yes N111 . C112 . H1121 . 111.5 no C113 . C112 . H1121 . 112.0 no N111 . C112 . H1122 . 106.4 no C113 . C112 . H1122 . 104.7 no H1121 . C112 . H1122 . 109.5 no C112 . C113 . O114 . 98.5(15) yes C112 . C113 . H1131 . 117.1 no O114 . C113 . H1131 . 114.5 no C112 . C113 . H1132 . 105.9 no O114 . C113 . H1132 . 110.7 no H1131 . C113 . H1132 . 109.5 no C113 . O114 . C115 . 114.8(16) yes O114 . C115 . C116 . 114.8(14) yes O114 . C115 . C120 . 125.1(14) yes C116 . C115 . C120 . 119.97(8) yes C115 . C116 . C117 . 119.96(8) yes C115 . C116 . H1161 . 119.0 no C117 . C116 . H1161 . 120.9 no C116 . C117 . C118 . 119.96(8) yes C116 . C117 . H1171 . 119.1 no C118 . C117 . H1171 . 120.9 no C117 . C118 . C119 . 119.97(8) yes C117 . C118 . O121 . 111.6(14) yes C119 . C118 . O121 . 128.3(14) yes C118 . C119 . C120 . 119.96(8) yes C118 . C119 . H1191 . 119.1 no C120 . C119 . H1191 . 120.9 no C115 . C120 . C119 . 119.97(8) yes C115 . C120 . H1201 . 120.9 no C119 . C120 . H1201 . 119.0 no C118 . O121 . C122 . 114.8(15) yes O121 . C122 . C123 . 105.0(14) yes O121 . C122 . H1221 . 111.5 no C123 . C122 . H1221 . 112.7 no O121 . C122 . H1222 . 114.6 no C123 . C122 . H1222 . 103.2 no H1221 . C122 . H1222 . 109.5 no C122 . C123 . O124 . 106.9(16) yes C122 . C123 . H1231 . 103.0 no O124 . C123 . H1231 . 109.4 no C122 . C123 . H1232 . 110.7 no O124 . C123 . H1232 . 116.5 no H1231 . C123 . H1232 . 109.5 no C123 . O124 . C125 . 109(2) yes O124 . C125 . C126 . 109.50(9) yes O124 . C125 . H1251 . 121.9 no C126 . C125 . H1251 . 105.7 no O124 . C125 . H1252 . 102.3 no C126 . C125 . H1252 . 107.2 no H1251 . C125 . H1252 . 109.5 no C125 . C126 . C127 . 109.50(9) yes C125 . C126 . H1261 . 114.2 no C127 . C126 . H1261 . 101.3 no C125 . C126 . H1262 . 104.1 no C127 . C126 . H1262 . 118.7 no H1261 . C126 . H1262 . 109.5 no C126 . C127 . S128 . 109.49(9) yes C126 . C127 . H1271 . 117.5 no S128 . C127 . H1271 . 120.0 no C126 . C127 . H1272 . 100.3 no S128 . C127 . H1272 . 95.9 no H1271 . C127 . H1272 . 109.5 no C127 . S128 . H1281 . 130.8 no C107 . C129 . O130 . 119.4(12) yes C107 . C129 . N131 . 116.6(14) yes O130 . C129 . N131 . 123.7(14) yes C129 . N131 . C132 . 122.6(14) yes C129 . N131 . H1311 . 129.1 no C132 . N131 . H1311 . 107.3 no N131 . C132 . C133 . 111.4(16) yes N131 . C132 . H1321 . 110.9 no C133 . C132 . H1321 . 112.9 no N131 . C132 . H1322 . 107.4 no C133 . C132 . H1322 . 104.5 no H1321 . C132 . H1322 . 109.5 no C132 . C133 . O134 . 106.3(14) yes C132 . C133 . H1331 . 107.0 no O134 . C133 . H1331 . 110.5 no C132 . C133 . H1332 . 110.1 no O134 . C133 . H1332 . 113.2 no H1331 . C133 . H1332 . 109.5 no C133 . O134 . C135 . 115.3(11) yes O134 . C135 . C136 . 113.0(10) yes O134 . C135 . C140 . 126.6(10) yes C136 . C135 . C140 . 119.99(9) yes C135 . C136 . C137 . 120.00(9) yes C135 . C136 . H1361 . 120.8 no C137 . C136 . H1361 . 119.2 no C136 . C137 . C138 . 120.01(8) yes C136 . C137 . H1371 . 120.8 no C138 . C137 . H1371 . 119.2 no C137 . C138 . C139 . 120.02(9) yes C137 . C138 . O141 . 128.9(13) yes C139 . C138 . O141 . 109.4(13) yes C138 . C139 . C140 . 120.03(9) yes C138 . C139 . H1391 . 120.8 no C140 . C139 . H1391 . 119.2 no C135 . C140 . C139 . 119.87(18) yes C135 . C140 . H1401 . 119.3 no C139 . C140 . H1401 . 120.8 no C138 . O141 . C142 . 109.9(17) yes O141 . C142 . C143 . 89.2(16) yes O141 . C142 . H1421 . 103.5 no C143 . C142 . H1421 . 115.9 no O141 . C142 . H1422 . 118.9 no C143 . C142 . H1422 . 118.0 no H1421 . C142 . H1422 . 109.5 no C142 . C143 . O144 . 121(2) yes C142 . C143 . H1431 . 107.3 no O144 . C143 . H1431 . 104.5 no C142 . C143 . H1432 . 105.1 no O144 . C143 . H1432 . 109.8 no H1431 . C143 . H1432 . 109.5 no C143 . O144 . C165 . 139(2) yes O144 . C145 . C146 . 109.51(9) yes O144 . C145 . H1451 . 116.7 no C146 . C145 . H1451 . 109.3 no O144 . C145 . H1452 . 112.4 no C146 . C145 . H1452 . 97.8 no H1451 . C145 . H1452 . 109.5 no C145 . C146 . C147 . 109.51(9) yes C145 . C146 . H1461 . 107.8 no C147 . C146 . H1461 . 111.4 no C145 . C146 . H1462 . 104.3 no C147 . C146 . H1462 . 113.9 no H1461 . C146 . H1462 . 109.5 no C146 . C147 . S148 . 109.51(9) yes C146 . C147 . H1471 . 99.4 no S148 . C147 . H1471 . 95.7 no C146 . C147 . H1472 . 111.6 no S148 . C147 . H1472 . 126.6 no H1471 . C147 . H1472 . 109.5 no C147 . S148 . H1481 . 111.4 no O144 . C165 . C166 . 109.50(9) yes O144 . C165 . H1651 . 79.4 no C166 . C165 . H1651 . 105.0 no O144 . C165 . H1652 . 126.8 no C166 . C165 . H1652 . 117.5 no H1651 . C165 . H1652 . 109.5 no C165 . C166 . C167 . 109.50(9) yes C165 . C166 . H1661 . 106.8 no C167 . C166 . H1661 . 86.9 no C165 . C166 . H1662 . 117.3 no C167 . C166 . H1662 . 121.7 no H1661 . C166 . H1662 . 109.5 no C166 . C167 . S168 . 109.50(9) yes C166 . C167 . H1671 . 122.3 no S168 . C167 . H1671 . 120.8 no C166 . C167 . H1672 . 87.0 no S168 . C167 . H1672 . 99.1 no H1671 . C167 . H1672 . 109.5 no C167 . S168 . H1681 . 129.3 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 C9 . H91 . O141 4_555 148 0.95 2.52 3.37(3) yes C25 . H251 . O121 1_455 144 0.95 2.55 3.36(3) yes C102 . H1021 . O130 2_566 149 0.95 2.53 3.38(3) yes C102 . H1022 . O33 . 159 0.95 2.45 3.35(3) yes C102 . H1023 . O39 . 169 0.95 2.40 3.34(3) yes C108 . H1081 . O130 2_566 152 0.95 2.19 3.06(3) yes C167 . H1671 . C9 1_554 130 0.95 2.43 3.13(3) yes C167 . H1671 . C10 1_554 142 0.95 2.20 3.01(3) yes C145 . H1452 . C166 . 129 0.95 1.19 1.93(3) yes C166 . H1452 . C146 . 160 1.19 1.88 3.02(3) yes C145 . H1452 . C167 . 152 0.95 2.28 3.15(3) yes