data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year 2008 _journal_page_first 2043 _publ_section_title ; Polymetallic clusters of iron(III) with derivatised salicylaldoximes ; _publ_contact_author_email EBRECHIN@STAFFMAIL.ED.AC.UK _publ_contact_author_address ; Department of Chemistry University of Edinburgh West Mains Raod Edinburgh EH9 3JJ UNITED KINGDOM ; _publ_contact_author_name 'Euan Brechin' loop_ _publ_author_name 'Ian A. Gass' 'Constantinos J. Milios' 'Anna Collins' F.J.White L.Budd S.Parsons 'Mark Murrie' S.P.Perlepes E.K.Brechin # Attachment 'Complex 4 cif.cif' data_EB7004 _database_code_depnum_ccdc_archive 'CCDC 667681' _audit_creation_date 07-01-22 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'EB7004 in Pbca' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 19.9693(6) _cell_length_b 14.2060(4) _cell_length_c 22.7462(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6452.7(3) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x+1/2,y+1/2,z x+1/2,-y+1/2,-z x,-y+1/2,z+1/2 -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 x+1/2,y,-z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C50 H82 Fe6 N6 O24 S2 # Dc = 1.60 Fooo = 3208.00 Mu = 14.58 M = 775.22 # Found Formula = C50 H80 Fe6 N6 O24 S2 # Dc = 1.59 FOOO = 3208.00 Mu = 14.58 M = 774.21 _chemical_formula_sum 'C50 H80 Fe6 N6 O24 S2' _chemical_formula_moiety 'C38 H48 Fe6 N4 O24 S2, 2(C6 H16 N)' _chemical_compound_source ? _chemical_formula_weight 1548.43 _cell_measurement_reflns_used 0 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _cell_measurement_temperature 150 _exptl_crystal_description wedge _exptl_crystal_colour black _exptl_crystal_size_min 0.31 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_max 0.47 _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 1.458 # Sheldrick geometric approximatio 0.63 0.64 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.45 _exptl_absorpt_correction_T_max 0.64 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method '\f & \w scans' # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _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 ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 149468 _reflns_number_total 9291 _diffrn_reflns_av_R_equivalents 0.046 # Number of reflections with Friedels Law is 9291 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 9390 _diffrn_reflns_theta_min 1.974 _diffrn_reflns_theta_max 29.976 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 29.377 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 31 _reflns_limit_h_min 0 _reflns_limit_h_max 27 _reflns_limit_k_min 0 _reflns_limit_k_max 19 _reflns_limit_l_min 0 _reflns_limit_l_max 31 _oxford_diffrn_Wilson_B_factor 1.54 _oxford_diffrn_Wilson_scale 28.68 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.89 _refine_diff_density_max 1.71 _refine_ls_number_reflns 9264 _refine_ls_number_restraints 0 _refine_ls_number_parameters 397 #_refine_ls_R_factor_ref 0.0485 _refine_ls_wR_factor_ref 0.0732 _refine_ls_goodness_of_fit_ref 1.0215 #_reflns_number_all 9264 _refine_ls_R_factor_all 0.0485 _refine_ls_wR_factor_all 0.0732 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6354 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_gt 0.0579 _refine_ls_shift/su_max 0.002422 # 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 constr # 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: 7.51 9.08 2.21 ; # 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_section_abstract # Text of the abstract # (a) The Abstract must be self-contained and comprehensible # without the rest of the paper. This means no references # to atom names or to compound numbers; compounds must be # identified as the title compound, or by name or by some other # means such as derivatives of each other (e.g. "the # corresponding ketone"). # (b) The chemical formula of "the title compound" must be given. # (c) Any crystallographic molecular symmetry should be # mentioned, and also the presence of more than one molecule # in the asymmetric unit (i.e. anything other than Z'=1). ; ? ; _publ_section_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 Fih. ; ? ; _publ_section_acknowledgements # Acknowledgments ; ? ; _publ_section_figure_captions # Captions to figures - Start each caption on a new line after a blank line ; Fig. 1. The title compound with displacement ellipsoids drawn at the 50% probability level. H atoms are shown as spheres of arbitary radius. ; _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; The relatively large ratio of minimum to maximum corrections applied in the multiscan process (1:nnn) reflect changes in the illuminated volume of the crystal. Changes in illuminated volume were kept to a minimum, and were taken into account (G\"orbitz, 1999) by the multi-scan inter-frame scaling (DENZO/SCALEPACK, Otwinowski & Minor, 1997). G\"orbitz, C. H. (1999). Acta Cryst. B55, 1090-1098. The H atoms in the main molecule of the complex were located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98, N---H in the range 0.86--0.89 N---H to 0.86 O---H = 0.82 \%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. Hydrogen atoms attached in the triethylamine solvent were attached geometrically with C--H distances of 0.94\%A. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.88 Sadabs corrects for all systematic errors that lead to disparities in the intensities of equivalent data. It is possible that the larger than expected range of transmission is accounted for by crystal decay or absorption by the mounting fibre. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 2.73 Ratio Part of a MeOH ligand. 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C43 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N38 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for C41 The triethylamine ligand is clearly dynamic within the crystal. The disorder cannot be modelled using partial occupancy of atomic sites, but is too localised to use the special shapes modelling function. This accounts for the differences in Ueq in the solvent. 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.94 360_ALERT_2_C Short C(sp3)-C(sp3) Bond C39 - C40 ... 1.40 Ang. 360_ALERT_2_C Short C(sp3)-C(sp3) Bond C43 - C44 ... 1.37 Ang. 412_ALERT_2_C Short Intra XH3 .. XHn H392 .. H422 .. 1.89 Ang. This results from disorder in the solvent. 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 1 912_ALERT_3_C # Missing FCF Reflections Above STH/L=0.6 ...... 92 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 1 The data is complete to Acta standards. #=============================================================================== Resolution & Completeness Statistics (Cumulative) #=============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------- 20.82 0.500 1.000 3384 3383 1 23.01 0.550 1.000 4493 4492 1 25.24 0.600 1.000 5832 5831 1 #----------------------------------------------------------- ACTA Min. Res. ---- 27.51 0.650 1.000 7421 7420 1 29.84 0.700 0.995 9274 9223 51 29.98 0.703 0.990 9384 9291 93 ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; # End of 'script/refcif.dat' # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, G., 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. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. 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 _atom_site_attached_hydrogens Fe1 Fe 0.545374(16) 1.04912(2) 0.455953(14) 0.0165 1.0000 Uani . . . . . . Fe2 Fe 0.521895(17) 0.83488(2) 0.427305(14) 0.0189 1.0000 Uani . . . . . . Fe3 Fe 0.602499(17) 0.84291(2) 0.541362(14) 0.0182 1.0000 Uani . . . . . . O4 O 0.66092(9) 0.76609(13) 0.58516(8) 0.0276 1.0000 Uani . . . . . . C5 C 0.66152(13) 0.74034(17) 0.64102(11) 0.0237 1.0000 Uani . . . . . . C6 C 0.72286(14) 0.71109(18) 0.66484(12) 0.0284 1.0000 Uani . . . . . . C7 C 0.72731(15) 0.6802(2) 0.72229(12) 0.0332 1.0000 Uani . . . . . . C8 C 0.67110(16) 0.6782(2) 0.75743(12) 0.0343 1.0000 Uani . . . . . . C9 C 0.61036(15) 0.70727(18) 0.73539(11) 0.0292 1.0000 Uani . . . . . . C10 C 0.60326(13) 0.73860(16) 0.67661(10) 0.0229 1.0000 Uani . . . . . . C11 C 0.53635(13) 0.76570(16) 0.65538(11) 0.0230 1.0000 Uani . . . . . . N12 N 0.52992(11) 0.81515(14) 0.60733(9) 0.0228 1.0000 Uani . . . . . . O13 O 0.46575(8) 0.83916(12) 0.59267(7) 0.0235 1.0000 Uani . . . . . . C14 C 0.47474(15) 0.7374(2) 0.68836(13) 0.0347 1.0000 Uani . . . . . . O15 O 0.50200(9) 0.74994(13) 0.36528(8) 0.0284 1.0000 Uani . . . . . . C16 C 0.46118(13) 0.67678(18) 0.36539(11) 0.0247 1.0000 Uani . . . . . . C17 C 0.47282(15) 0.60496(19) 0.32354(12) 0.0324 1.0000 Uani . . . . . . C18 C 0.43429(17) 0.5247(2) 0.32184(15) 0.0414 1.0000 Uani . . . . . . C19 C 0.38202(17) 0.5138(2) 0.36105(16) 0.0438 1.0000 Uani . . . . . . C20 C 0.36943(16) 0.5827(2) 0.40172(14) 0.0372 1.0000 Uani . . . . . . C21 C 0.40680(13) 0.66585(18) 0.40493(11) 0.0264 1.0000 Uani . . . . . . C22 C 0.38613(13) 0.74025(18) 0.44613(12) 0.0268 1.0000 Uani . . . . . . N23 N 0.42346(10) 0.81459(14) 0.45263(9) 0.0226 1.0000 Uani . . . . . . O24 O 0.39652(9) 0.88675(12) 0.48517(8) 0.0246 1.0000 Uani . . . . . . C25 C 0.32237(16) 0.7315(2) 0.48049(17) 0.0495 1.0000 Uani . . . . . . O26 O 0.50431(8) 0.96157(12) 0.39466(7) 0.0208 1.0000 Uani . . . . . . C27 C 0.50520(15) 0.9779(2) 0.33310(11) 0.0318 1.0000 Uani . . . . . . O28 O 0.63184(9) 0.96550(13) 0.58752(9) 0.0315 1.0000 Uani . . . . . . C29 C 0.69394(19) 0.9847(3) 0.6130(2) 0.0623 1.0000 Uani . . . . . . O30 O 0.56276(9) 0.74601(12) 0.48813(8) 0.0239 1.0000 Uani . . . . . . C31 C 0.53507(15) 0.65997(18) 0.50822(13) 0.0323 1.0000 Uani . . . . . . O32 O 0.53820(8) 0.92352(11) 0.49965(7) 0.0170 1.0000 Uani . . . . . . O33 O 0.64012(8) 1.00862(11) 0.42428(7) 0.0201 1.0000 Uani . . . . . . S34 S 0.66725(3) 0.91104(4) 0.42283(3) 0.0179 1.0000 Uani . . . . . . O35 O 0.73023(8) 0.91053(12) 0.39056(8) 0.0235 1.0000 Uani . . . . . . O36 O 0.61808(8) 0.84797(12) 0.39395(7) 0.0203 1.0000 Uani . . . . . . O37 O 0.67823(8) 0.87706(12) 0.48380(7) 0.0221 1.0000 Uani . . . . . . N38 N 0.77877(15) 1.0920(2) 0.36753(14) 0.0501 1.0000 Uani . . . . . . C39 C 0.8354(3) 1.0784(4) 0.3271(3) 0.1144 1.0000 Uani . . . . . . C40 C 0.8664(3) 0.9901(4) 0.3244(4) 0.1588 1.0000 Uani . . . . . . C41 C 0.7227(2) 1.1484(3) 0.3384(2) 0.0621 1.0000 Uani . . . . . . C42 C 0.6946(3) 1.1044(4) 0.2852(3) 0.1145 1.0000 Uani . . . . . . C43 C 0.7958(4) 1.1379(4) 0.4252(3) 0.1146 1.0000 Uani . . . . . . C44 C 0.8008(3) 1.0832(3) 0.4747(2) 0.0775 1.0000 Uani . . . . . . H61 H 0.7606 0.7134 0.6410 0.0334 1.0000 Uiso R . . . . . H71 H 0.7690 0.6620 0.7372 0.0395 1.0000 Uiso R . . . . . H81 H 0.6742 0.6576 0.7954 0.0410 1.0000 Uiso R . . . . . H91 H 0.5730 0.7069 0.7599 0.0340 1.0000 Uiso R . . . . . H141 H 0.4392 0.7268 0.6621 0.0518 1.0000 Uiso R . . . . . H142 H 0.4613 0.7865 0.7137 0.0527 1.0000 Uiso R . . . . . H143 H 0.4808 0.6822 0.7106 0.0526 1.0000 Uiso R . . . . . H171 H 0.5082 0.6131 0.2966 0.0389 1.0000 Uiso R . . . . . H181 H 0.4434 0.4773 0.2937 0.0500 1.0000 Uiso R . . . . . H191 H 0.3562 0.4601 0.3600 0.0516 1.0000 Uiso R . . . . . H201 H 0.3336 0.5739 0.4287 0.0447 1.0000 Uiso R . . . . . H251 H 0.3166 0.7878 0.5037 0.0751 1.0000 Uiso R . . . . . H252 H 0.3254 0.6771 0.5058 0.0749 1.0000 Uiso R . . . . . H253 H 0.2859 0.7230 0.4545 0.0743 1.0000 Uiso R . . . . . H271 H 0.5494 0.9874 0.3179 0.0486 1.0000 Uiso R . . . . . H272 H 0.4807 1.0339 0.3234 0.0483 1.0000 Uiso R . . . . . H273 H 0.4855 0.9272 0.3123 0.0487 1.0000 Uiso R . . . . . H281 H 0.6103 0.9987 0.6043 0.0500 1.0000 Uiso R . . . . . H291 H 0.7211 1.0181 0.5861 0.0947 1.0000 Uiso R . . . . . H292 H 0.6853 1.0231 0.6465 0.0937 1.0000 Uiso R . . . . . H293 H 0.7144 0.9270 0.6249 0.0940 1.0000 Uiso R . . . . . H311 H 0.5656 0.6303 0.5359 0.0487 1.0000 Uiso R . . . . . H312 H 0.4912 0.6699 0.5269 0.0489 1.0000 Uiso R . . . . . H313 H 0.5271 0.6160 0.4748 0.0491 1.0000 Uiso R . . . . . H381 H 0.7626 1.0354 0.3755 0.0757 1.0000 Uiso R . . . . . H411 H 0.7405 1.2085 0.3285 0.0751 1.0000 Uiso R . . . . . H412 H 0.6865 1.1598 0.3658 0.0752 1.0000 Uiso R . . . . . H421 H 0.6608 1.1432 0.2674 0.1710 1.0000 Uiso R . . . . . H422 H 0.7314 1.0952 0.2584 0.1710 1.0000 Uiso R . . . . . H423 H 0.6762 1.0431 0.2938 0.1707 1.0000 Uiso R . . . . . H441 H 0.8112 1.1195 0.5080 0.0920 1.0000 Uiso R . . . . . H442 H 0.8348 1.0386 0.4685 0.0920 1.0000 Uiso R . . . . . H443 H 0.7598 1.0521 0.4807 0.0920 1.0000 Uiso R . . . . . H391 H 0.8689 1.1226 0.3380 0.1439 1.0000 Uiso R . . . . . H392 H 0.8197 1.0925 0.2887 0.1439 1.0000 Uiso R . . . . . H401 H 0.9019 0.9919 0.2967 0.1870 1.0000 Uiso R . . . . . H402 H 0.8836 0.9742 0.3620 0.1870 1.0000 Uiso R . . . . . H403 H 0.8345 0.9442 0.3127 0.1870 1.0000 Uiso R . . . . . H431 H 0.8380 1.1661 0.4200 0.1399 1.0000 Uiso R . . . . . H432 H 0.7636 1.1848 0.4324 0.1399 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 0.01744(15) 0.01571(14) 0.01648(14) -0.00088(12) 0.00110(12) 0.00102(12) Fe2 0.01934(15) 0.01969(15) 0.01774(15) -0.00293(12) 0.00116(12) -0.00473(13) Fe3 0.01948(15) 0.01882(15) 0.01630(14) 0.00061(12) 0.00022(12) 0.00308(12) O4 0.0298(9) 0.0329(10) 0.0201(8) 0.0060(7) 0.0010(7) 0.0114(8) C5 0.0321(13) 0.0180(11) 0.0209(11) 0.0014(9) -0.0021(10) 0.0039(10) C6 0.0325(13) 0.0263(12) 0.0264(12) 0.0019(10) -0.0050(11) 0.0031(11) C7 0.0379(15) 0.0317(14) 0.0300(13) 0.0045(11) -0.0122(12) 0.0020(12) C8 0.0496(17) 0.0324(14) 0.0208(12) 0.0064(10) -0.0086(12) -0.0014(13) C9 0.0418(15) 0.0247(12) 0.0209(11) 0.0029(9) 0.0010(11) -0.0044(11) C10 0.0326(12) 0.0169(10) 0.0190(10) 0.0009(8) -0.0014(10) -0.0003(9) C11 0.0291(12) 0.0190(11) 0.0210(11) 0.0006(9) 0.0026(9) 0.0012(9) N12 0.0258(10) 0.0204(9) 0.0222(9) 0.0016(8) 0.0030(8) 0.0028(8) O13 0.0211(8) 0.0236(8) 0.0259(8) 0.0051(7) 0.0037(7) 0.0034(7) C14 0.0353(14) 0.0380(15) 0.0309(14) 0.0117(12) 0.0058(12) -0.0019(12) O15 0.0298(9) 0.0272(9) 0.0281(9) -0.0098(8) 0.0043(8) -0.0079(8) C16 0.0261(12) 0.0238(11) 0.0242(11) -0.0039(9) -0.0024(9) -0.0039(10) C17 0.0375(15) 0.0287(13) 0.0309(13) -0.0099(11) -0.0012(12) -0.0007(11) C18 0.0536(19) 0.0279(14) 0.0429(17) -0.0136(13) 0.0005(15) -0.0047(13) C19 0.0500(19) 0.0267(14) 0.055(2) -0.0129(14) 0.0063(16) -0.0160(14) C20 0.0405(16) 0.0271(13) 0.0441(17) -0.0029(12) 0.0052(13) -0.0107(12) C21 0.0280(12) 0.0220(11) 0.0291(12) -0.0033(10) -0.0018(10) -0.0035(10) C22 0.0249(12) 0.0253(12) 0.0302(13) -0.0032(10) 0.0023(10) -0.0036(10) N23 0.0211(9) 0.0223(10) 0.0244(10) -0.0040(8) 0.0003(8) -0.0001(8) O24 0.0262(9) 0.0214(8) 0.0260(9) -0.0066(7) -0.0014(7) 0.0008(7) C25 0.0386(17) 0.0387(17) 0.071(2) -0.0202(17) 0.0262(17) -0.0164(14) O26 0.0212(8) 0.0253(8) 0.0160(7) -0.0031(6) -0.0002(6) -0.0014(7) C27 0.0453(16) 0.0322(14) 0.0178(11) -0.0013(10) -0.0030(11) 0.0044(12) O28 0.0297(10) 0.0300(10) 0.0349(10) -0.0125(8) -0.0110(8) 0.0066(8) C29 0.058(2) 0.0437(19) 0.085(3) 0.003(2) -0.042(2) -0.0110(18) O30 0.0285(9) 0.0153(7) 0.0279(9) -0.0011(7) 0.0045(7) -0.0012(7) C31 0.0371(15) 0.0210(12) 0.0388(15) 0.0041(11) -0.0002(12) -0.0034(11) O32 0.0192(8) 0.0151(7) 0.0169(7) -0.0009(6) 0.0007(6) 0.0009(6) O33 0.0188(8) 0.0176(7) 0.0239(8) -0.0013(6) 0.0034(6) -0.0018(6) S34 0.0160(2) 0.0180(2) 0.0199(2) -0.0012(2) 0.0022(2) -0.0014(2) O35 0.0186(8) 0.0227(8) 0.0292(9) -0.0017(7) 0.0065(7) -0.0013(7) O36 0.0200(8) 0.0197(8) 0.0214(8) -0.0032(6) 0.0028(6) -0.0031(6) O37 0.0182(8) 0.0258(8) 0.0223(8) 0.0019(7) -0.0004(7) 0.0003(7) N38 0.0517(17) 0.0299(13) 0.069(2) 0.0069(14) 0.0115(15) -0.0134(13) C39 0.061(3) 0.086(4) 0.196(7) 0.050(4) 0.073(4) 0.015(3) C40 0.088(4) 0.064(4) 0.325(12) 0.024(5) 0.104(6) -0.006(3) C41 0.068(3) 0.0391(19) 0.079(3) 0.018(2) 0.025(2) -0.0004(19) C42 0.126(5) 0.077(4) 0.140(6) 0.047(4) -0.061(5) -0.020(4) C43 0.189(7) 0.052(3) 0.103(4) -0.002(3) -0.036(5) -0.040(4) C44 0.081(3) 0.064(3) 0.087(4) -0.022(3) -0.021(3) -0.019(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.16217(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 . Fe1 2_676 3.0408(6) yes Fe1 . O24 2_676 1.9925(17) yes Fe1 . O32 2_676 1.9890(16) yes Fe1 . O13 2_676 1.9472(17) yes Fe1 . Fe3 2_676 3.3281(5) yes Fe1 . Fe2 2_676 3.4017(5) yes Fe1 . O26 . 2.0403(16) yes Fe1 . O32 . 2.0473(15) yes Fe1 . O33 . 2.1047(16) yes Fe2 . Fe3 . 3.0553(5) yes Fe2 . O15 . 1.8985(18) yes Fe2 . N23 . 2.069(2) yes Fe2 . O26 . 1.9784(17) yes Fe2 . O30 . 2.0431(18) yes Fe2 . O32 . 2.0975(15) yes Fe2 . O36 . 2.0736(16) yes Fe3 . O4 . 1.8827(17) yes Fe3 . N12 . 2.123(2) yes Fe3 . O28 . 2.1162(18) yes Fe3 . O30 . 1.9977(18) yes Fe3 . O32 . 1.9648(16) yes Fe3 . O37 . 2.0583(17) yes O4 . C5 . 1.322(3) yes C5 . C6 . 1.402(3) yes C5 . C10 . 1.418(4) yes C6 . C7 . 1.381(4) yes C6 . H61 . 0.929 no C7 . C8 . 1.378(4) yes C7 . H71 . 0.936 no C8 . C9 . 1.376(4) yes C8 . H81 . 0.914 no C9 . C10 . 1.416(3) yes C9 . H91 . 0.932 no C10 . C11 . 1.472(3) yes C11 . N12 . 1.305(3) yes C11 . C14 . 1.496(4) yes N12 . O13 . 1.367(3) yes C14 . H141 . 0.938 no C14 . H142 . 0.944 no C14 . H143 . 0.942 no O15 . C16 . 1.321(3) yes C16 . C17 . 1.415(3) yes C16 . C21 . 1.419(4) yes C17 . C18 . 1.376(4) yes C17 . H171 . 0.942 no C18 . C19 . 1.382(5) yes C18 . H181 . 0.947 no C19 . C20 . 1.370(4) yes C19 . H191 . 0.921 no C20 . C21 . 1.399(4) yes C20 . H201 . 0.951 no C21 . C22 . 1.472(4) yes C22 . N23 . 1.301(3) yes C22 . C25 . 1.499(4) yes N23 . O24 . 1.374(2) yes C25 . H251 . 0.964 no C25 . H252 . 0.966 no C25 . H253 . 0.947 no O26 . C27 . 1.419(3) yes C27 . H271 . 0.958 no C27 . H272 . 0.961 no C27 . H273 . 0.948 no O28 . C29 . 1.396(4) yes O28 . H281 . 0.744 no C29 . H291 . 0.946 no C29 . H292 . 0.952 no C29 . H293 . 0.955 no O30 . C31 . 1.417(3) yes C31 . H311 . 0.971 no C31 . H312 . 0.984 no C31 . H313 . 0.997 no O33 . S34 . 1.4886(17) yes S34 . O35 . 1.4563(17) yes S34 . O36 . 1.4827(17) yes S34 . O37 . 1.4847(18) yes N38 . C39 . 1.471(5) yes N38 . C41 . 1.528(5) yes N38 . C43 . 1.505(6) yes N38 . H381 . 0.886 no C39 . C40 . 1.400(7) yes C39 . H391 . 0.950 no C39 . H392 . 0.950 no C40 . H401 . 0.950 no C40 . H402 . 0.950 no C40 . H403 . 0.950 no C41 . C42 . 1.473(7) yes C41 . H411 . 0.951 no C41 . H412 . 0.968 no C42 . H421 . 0.961 no C42 . H422 . 0.963 no C42 . H423 . 0.965 no C43 . C44 . 1.372(7) yes C43 . H431 . 0.940 no C43 . H432 . 0.940 no C44 . H441 . 0.940 no C44 . H442 . 0.940 no C44 . H443 . 0.940 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 Fe1 2_676 Fe1 . O24 2_676 96.55(5) yes Fe1 2_676 Fe1 . O32 2_676 41.85(4) yes O24 2_676 Fe1 . O32 2_676 93.33(7) yes Fe1 2_676 Fe1 . O13 2_676 132.87(5) yes O24 2_676 Fe1 . O13 2_676 94.33(8) yes O32 2_676 Fe1 . O13 2_676 91.92(7) yes Fe1 2_676 Fe1 . Fe3 2_676 70.771(13) yes O24 2_676 Fe1 . Fe3 2_676 107.08(5) yes O32 2_676 Fe1 . Fe3 2_676 32.45(4) yes O13 2_676 Fe1 . Fe3 2_676 62.20(5) yes Fe1 2_676 Fe1 . Fe2 2_676 58.170(12) yes O24 2_676 Fe1 . Fe2 2_676 58.92(5) yes O32 2_676 Fe1 . Fe2 2_676 34.68(4) yes O13 2_676 Fe1 . Fe2 2_676 90.20(5) yes Fe3 2_676 Fe1 . Fe2 2_676 53.986(10) yes Fe1 2_676 Fe1 . O26 . 86.05(5) yes O24 2_676 Fe1 . O26 . 166.42(7) yes O32 2_676 Fe1 . O26 . 97.40(7) yes O13 2_676 Fe1 . O26 . 93.60(7) yes Fe3 2_676 Fe1 . O26 . 86.38(5) yes Fe1 2_676 Fe1 . O32 . 40.40(4) yes O24 2_676 Fe1 . O32 . 96.49(7) yes O32 2_676 Fe1 . O32 . 82.25(7) yes O13 2_676 Fe1 . O32 . 167.98(7) yes Fe3 2_676 Fe1 . O32 . 109.31(5) yes Fe1 2_676 Fe1 . O33 . 129.48(5) yes O24 2_676 Fe1 . O33 . 80.30(7) yes O32 2_676 Fe1 . O33 . 168.96(7) yes O13 2_676 Fe1 . O33 . 97.52(7) yes Fe3 2_676 Fe1 . O33 . 158.41(5) yes Fe2 2_676 Fe1 . O26 . 132.07(5) yes Fe2 2_676 Fe1 . O32 . 90.89(4) yes O26 . Fe1 . O32 . 76.85(6) yes Fe2 2_676 Fe1 . O33 . 138.99(5) yes O26 . Fe1 . O33 . 87.75(7) yes O32 . Fe1 . O33 . 89.48(6) yes Fe1 2_676 Fe2 . Fe3 . 61.777(10) yes Fe1 2_676 Fe2 . O15 . 143.65(6) yes Fe3 . Fe2 . O15 . 139.91(6) yes Fe1 2_676 Fe2 . N23 . 58.32(6) yes Fe3 . Fe2 . N23 . 105.63(6) yes O15 . Fe2 . N23 . 85.39(8) yes Fe1 2_676 Fe2 . O26 . 77.42(5) yes Fe3 . Fe2 . O26 . 112.23(5) yes O15 . Fe2 . O26 . 105.19(8) yes N23 . Fe2 . O26 . 93.59(8) yes Fe1 2_676 Fe2 . O30 . 85.90(5) yes Fe3 . Fe2 . O30 . 40.32(5) yes O15 . Fe2 . O30 . 101.19(8) yes N23 . Fe2 . O30 . 96.02(8) yes O26 . Fe2 . O30 . 152.53(7) yes Fe1 2_676 Fe2 . O32 . 32.65(4) yes Fe3 . Fe2 . O32 . 39.61(4) yes O15 . Fe2 . O32 . 175.61(7) yes N23 . Fe2 . O32 . 90.73(7) yes O26 . Fe2 . O32 . 77.05(6) yes Fe1 2_676 Fe2 . O36 . 127.44(5) yes Fe3 . Fe2 . O36 . 79.59(5) yes O15 . Fe2 . O36 . 88.79(7) yes N23 . Fe2 . O36 . 174.08(7) yes O26 . Fe2 . O36 . 86.87(7) yes O30 . Fe2 . O32 . 77.16(6) yes O30 . Fe2 . O36 . 86.17(7) yes O32 . Fe2 . O36 . 95.13(6) yes Fe2 . Fe3 . Fe1 2_676 64.237(11) yes Fe2 . Fe3 . O4 . 138.95(6) yes Fe1 2_676 Fe3 . O4 . 143.83(6) yes Fe2 . Fe3 . N12 . 103.51(6) yes Fe1 2_676 Fe3 . N12 . 57.79(6) yes O4 . Fe3 . N12 . 86.64(8) yes Fe2 . Fe3 . O28 . 126.71(5) yes Fe1 2_676 Fe3 . O28 . 81.79(5) yes O4 . Fe3 . O28 . 92.46(8) yes N12 . Fe3 . O28 . 89.50(8) yes Fe2 . Fe3 . O30 . 41.44(5) yes Fe1 2_676 Fe3 . O30 . 88.64(5) yes O4 . Fe3 . O30 . 99.64(8) yes N12 . Fe3 . O30 . 91.67(8) yes O28 . Fe3 . O30 . 167.89(7) yes Fe2 . Fe3 . O32 . 42.90(4) yes Fe1 2_676 Fe3 . O32 . 32.90(5) yes O4 . Fe3 . O32 . 176.71(7) yes N12 . Fe3 . O32 . 90.20(7) yes O28 . Fe3 . O32 . 86.61(7) yes Fe2 . Fe3 . O37 . 81.70(5) yes Fe1 2_676 Fe3 . O37 . 123.71(5) yes O4 . Fe3 . O37 . 91.03(7) yes N12 . Fe3 . O37 . 174.21(8) yes O28 . Fe3 . O37 . 85.31(7) yes O30 . Fe3 . O32 . 81.33(7) yes O30 . Fe3 . O37 . 93.94(7) yes O32 . Fe3 . O37 . 92.04(7) yes Fe3 . O4 . C5 . 132.41(17) yes O4 . C5 . C6 . 117.5(2) yes O4 . C5 . C10 . 123.1(2) yes C6 . C5 . C10 . 119.4(2) yes C5 . C6 . C7 . 121.1(3) yes C5 . C6 . H61 . 118.1 no C7 . C6 . H61 . 120.8 no C6 . C7 . C8 . 120.2(3) yes C6 . C7 . H71 . 119.2 no C8 . C7 . H71 . 120.6 no C7 . C8 . C9 . 120.0(2) yes C7 . C8 . H81 . 120.0 no C9 . C8 . H81 . 120.0 no C8 . C9 . C10 . 121.8(3) yes C8 . C9 . H91 . 119.1 no C10 . C9 . H91 . 119.1 no C5 . C10 . C9 . 117.5(2) yes C5 . C10 . C11 . 123.6(2) yes C9 . C10 . C11 . 118.9(2) yes C10 . C11 . N12 . 120.3(2) yes C10 . C11 . C14 . 120.8(2) yes N12 . C11 . C14 . 118.9(2) yes Fe3 . N12 . C11 . 128.65(18) yes Fe3 . N12 . O13 . 114.91(14) yes C11 . N12 . O13 . 115.5(2) yes N12 . O13 . Fe1 2_676 116.66(13) yes C11 . C14 . H141 . 110.2 no C11 . C14 . H142 . 110.0 no H141 . C14 . H142 . 107.0 no C11 . C14 . H143 . 112.8 no H141 . C14 . H143 . 107.8 no H142 . C14 . H143 . 108.8 no Fe2 . O15 . C16 . 128.88(16) yes O15 . C16 . C17 . 117.7(2) yes O15 . C16 . C21 . 124.0(2) yes C17 . C16 . C21 . 118.3(2) yes C16 . C17 . C18 . 121.7(3) yes C16 . C17 . H171 . 118.2 no C18 . C17 . H171 . 120.1 no C17 . C18 . C19 . 119.8(3) yes C17 . C18 . H181 . 120.1 no C19 . C18 . H181 . 120.2 no C18 . C19 . C20 . 119.7(3) yes C18 . C19 . H191 . 119.9 no C20 . C19 . H191 . 120.4 no C19 . C20 . C21 . 122.7(3) yes C19 . C20 . H201 . 118.6 no C21 . C20 . H201 . 118.6 no C16 . C21 . C20 . 117.9(2) yes C16 . C21 . C22 . 122.7(2) yes C20 . C21 . C22 . 119.4(2) yes C21 . C22 . N23 . 119.7(2) yes C21 . C22 . C25 . 120.7(2) yes N23 . C22 . C25 . 119.6(2) yes Fe2 . N23 . C22 . 128.75(17) yes Fe2 . N23 . O24 . 114.71(14) yes C22 . N23 . O24 . 116.3(2) yes N23 . O24 . Fe1 2_676 118.37(14) yes C22 . C25 . H251 . 108.6 no C22 . C25 . H252 . 108.9 no H251 . C25 . H252 . 110.2 no C22 . C25 . H253 . 109.8 no H251 . C25 . H253 . 110.9 no H252 . C25 . H253 . 108.5 no Fe1 . O26 . Fe2 . 103.10(7) yes Fe1 . O26 . C27 . 124.74(16) yes Fe2 . O26 . C27 . 121.09(15) yes O26 . C27 . H271 . 113.1 no O26 . C27 . H272 . 110.9 no H271 . C27 . H272 . 105.6 no O26 . C27 . H273 . 111.4 no H271 . C27 . H273 . 108.0 no H272 . C27 . H273 . 107.7 no Fe3 . O28 . C29 . 127.8(2) yes Fe3 . O28 . H281 . 128.0 no C29 . O28 . H281 . 100.2 no O28 . C29 . H291 . 109.7 no O28 . C29 . H292 . 106.5 no H291 . C29 . H292 . 109.5 no O28 . C29 . H293 . 109.3 no H291 . C29 . H293 . 111.7 no H292 . C29 . H293 . 110.1 no Fe2 . O30 . Fe3 . 98.24(7) yes Fe2 . O30 . C31 . 126.54(16) yes Fe3 . O30 . C31 . 123.64(16) yes O30 . C31 . H311 . 109.8 no O30 . C31 . H312 . 111.3 no H311 . C31 . H312 . 109.9 no O30 . C31 . H313 . 110.9 no H311 . C31 . H313 . 108.7 no H312 . C31 . H313 . 106.2 no Fe2 . O32 . Fe1 . 98.81(7) yes Fe2 . O32 . Fe1 2_676 112.67(7) yes Fe1 . O32 . Fe1 2_676 97.75(7) yes Fe2 . O32 . Fe3 . 97.49(7) yes Fe1 . O32 . Fe3 . 134.16(8) yes Fe1 2_676 O32 . Fe3 . 114.65(8) yes Fe1 . O33 . S34 . 126.11(10) yes O33 . S34 . O35 . 109.28(10) yes O33 . S34 . O36 . 109.36(10) yes O35 . S34 . O36 . 110.21(10) yes O33 . S34 . O37 . 109.62(10) yes O35 . S34 . O37 . 109.99(10) yes O36 . S34 . O37 . 108.37(10) yes Fe2 . O36 . S34 . 120.37(9) yes Fe3 . O37 . S34 . 124.22(10) yes C39 . N38 . C41 . 111.2(4) yes C39 . N38 . C43 . 115.4(5) yes C41 . N38 . C43 . 108.5(4) yes C39 . N38 . H381 . 106.9 no C41 . N38 . H381 . 107.3 no C43 . N38 . H381 . 107.3 no N38 . C39 . C40 . 119.0(5) yes N38 . C39 . H391 . 106.9 no C40 . C39 . H391 . 107.0 no N38 . C39 . H392 . 107.1 no C40 . C39 . H392 . 107.1 no H391 . C39 . H392 . 109.5 no C39 . C40 . H401 . 109.6 no C39 . C40 . H402 . 109.5 no H401 . C40 . H402 . 109.5 no C39 . C40 . H403 . 109.3 no H401 . C40 . H403 . 109.5 no H402 . C40 . H403 . 109.5 no N38 . C41 . C42 . 114.4(4) yes N38 . C41 . H411 . 107.4 no C42 . C41 . H411 . 109.3 no N38 . C41 . H412 . 110.8 no C42 . C41 . H412 . 108.4 no H411 . C41 . H412 . 106.3 no C41 . C42 . H421 . 111.7 no C41 . C42 . H422 . 106.7 no H421 . C42 . H422 . 110.4 no C41 . C42 . H423 . 111.2 no H421 . C42 . H423 . 109.6 no H422 . C42 . H423 . 107.2 no N38 . C43 . C44 . 119.1(4) yes N38 . C43 . H431 . 106.1 no C44 . C43 . H431 . 106.3 no N38 . C43 . H432 . 107.7 no C44 . C43 . H432 . 107.9 no H431 . C43 . H432 . 109.5 no C43 . C44 . H441 . 111.5 no C43 . C44 . H442 . 108.1 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 108.8 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no # Attachment 'Complex 7 Fe8.cif' data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 667684' _audit_creation_date 06-11-12 _audit_creation_method CRYSTALS_ver_12.84 _oxford_structure_analysis_title 'eb6103 in P-1' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 16.2363(5) _cell_length_b 17.6493(6) _cell_length_c 18.6823(6) _cell_angle_alpha 108.435(2) _cell_angle_beta 98.275(2) _cell_angle_gamma 105.150(2) _cell_volume 4749.9(3) _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' 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' _cell_formula_units_Z 2 # Given Formula = C73 H103 Fe8 N7 O31 # Dc = 1.41 Fooo = 1948.00 Mu = 12.62 M = 2021.43 # Found Formula = C69 H87 Fe8 N7 O27 # Dc = 1.32 FOOO = 1948.00 Mu = 12.54 M = 1893.26 _chemical_formula_sum 'C73 H103 Fe8 N7 O31' _chemical_formula_moiety '[C69 H87 Fe8 N7 O27] 4[CH3OH]' _chemical_compound_source 'Ian gass' _chemical_formula_weight 2021.43 _cell_measurement_reflns_used 5841 _cell_measurement_theta_min 2 _cell_measurement_theta_max 24 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_min 0.19 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_max 0.28 _exptl_crystal_density_diffrn 1.41 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 1.262 # Sheldrick geometric approximatio 0.71 0.79 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Siemens, 1996)' _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_T_max 0.79 _diffrn_measurement_device_type 'Bruker SMART' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w # If a reference occurs more than once, delete the author # and date from subsequent references. _computing_data_collection 'SMART (Siemens, 1993)' _computing_cell_refinement 'SAINT (Siemens ,1995)' _computing_data_reduction 'SAINT (Siemens ,1995)' _computing_structure_solution 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 113796 _reflns_number_total 27792 _diffrn_reflns_av_R_equivalents 0.094 # Number of reflections with Friedels Law is 27792 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 29186 _diffrn_reflns_theta_min 1.390 _diffrn_reflns_theta_max 30.579 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 28.133 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _reflns_limit_h_min -23 _reflns_limit_h_max 22 _reflns_limit_k_min -25 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 26 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.29 _refine_diff_density_max 1.80 _refine_ls_number_reflns 19878 _refine_ls_number_restraints 42 _refine_ls_number_parameters 1000 #_refine_ls_R_factor_ref 0.1049 _refine_ls_wR_factor_ref 0.1600 _refine_ls_goodness_of_fit_ref 0.6171 #_reflns_number_all 19878 _refine_ls_R_factor_all 0.1049 _refine_ls_wR_factor_all 0.1600 # No actual I/u(I) cutoff was used for refinement. The # threshold below is used for "_gt" information ONLY: _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9803 _refine_ls_R_factor_gt 0.0500 _refine_ls_wR_factor_gt 0.1088 _refine_ls_shift/su_max 0.000470 # 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 mixed # none, undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; _exptl_crystal_recrystallization_method ; grown from methanol ; _refine_special_details ; The solvent region was treated using the SQUEEZE technique. This accounted for 141 electrons per unit cell. This corresponds to 4 methanol molecules per formula unit and has been included in the formula given. The formula weight, Fooo, density and mu have been updated accordingly. Checkcif output; 912_ALERT_3_A # Missing FCF Reflections Above STH/L=0.6 ...... 1394 910_ALERT_3_C # Missing FCF Reflections Below TH(Min) ........ 3 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 0.600 8 913_ALERT_3_C # Missing Very Strong Reflections in FCF ....... 5 919_ALERT_3_B # Reflections Likely Effected by the Beamstop .. 1 026_ALERT_3_B Ratio Observed / Unique Reflections too Low .... 35 Perc. The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. The data were weak, therefore a cutoff of d=0.8 Ang was applied during refinement. See completeness statistics below. 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.07 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.63 Ratio There was some disorder in this region which could not be modelled any better. 420_ALERT_2_B D-H Without Acceptor O435 - H8654 ... ? 420_ALERT_2_B D-H Without Acceptor O437 - H8655 ... ? There was disordered solvent in this region which could not be modelled, see above. 061_ALERT_3_C Tmax/Tmin Range Test RR' too Large ............. 0.77 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. 220_ALERT_2_C Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.09 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C833 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 602_ALERT_4_C VERY LARGE Solvent Accessible VOID(S) in Structure ! 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 68 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C19 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O119 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N16 Noted but no action taken. Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.999 9950 9945 5 23.01 0.550 1.000 13241 13236 5 25.24 0.600 0.999 17200 17189 11 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.997 21854 21799 55 29.84 0.700 0.973 27308 26576 732 30.58 0.716 0.952 29197 27792 1405 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Larson, A.C. (1970) Crystallographic Computing, Ed Ahmed, F.R., Munksgaard, Copenhagen, 291-294. Siemens Industrial Automation, Inc (1993). SMART: Area-Detector Software Package; Madison, WI. Siemens Industrial Automation, Inc (1995). SAINT: Area-Detector Integration Software.; Madison, WI. Siemens Industrial Automation, Inc (1996). SADABS: Area-Detector Absorption Correction;: Madison, WI. Sheldrick, G.M. (1986). SHELXS86. Program for the solution of crystal structures. Univ. of G\"ottingen, Federal Republic of Germany. 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 _atom_site_attached_hydrogens Fe1 Fe 0.36907(5) 0.60318(5) 0.31562(5) 0.0296 1.0000 Uani . . . . . . Fe2 Fe 0.29227(5) 0.67023(6) 0.21368(5) 0.0309 1.0000 Uani . . . . . . Fe3 Fe 0.48331(5) 0.78410(5) 0.26942(5) 0.0321 1.0000 Uani . . . . . . Fe4 Fe 0.48414(5) 0.59082(5) 0.19679(5) 0.0301 1.0000 Uani . . . . . . Fe5 Fe 0.25474(5) 0.48888(6) 0.10524(5) 0.0316 1.0000 Uani . . . . . . Fe6 Fe 0.17717(5) 0.47942(6) 0.25367(5) 0.0311 1.0000 Uani . . . . . . Fe7 Fe 0.18716(5) 0.69363(6) 0.33584(5) 0.0327 1.0000 Uani . . . . . . Fe8 Fe 0.39102(5) 0.78269(6) 0.43099(5) 0.0317 1.0000 Uani . . . . . . C18 C 0.2654(4) 0.8825(4) 0.4117(3) 0.0406 1.0000 Uani . . . . . . C28 C 0.2525(5) 0.9668(5) 0.4331(5) 0.0650 1.0000 Uani . . . . . . O118 O 0.2019(3) 0.8192(3) 0.3662(2) 0.0420 1.0000 Uani . . . . . . O128 O 0.3393(3) 0.8797(3) 0.4423(2) 0.0391 1.0000 Uani . . . . . . C19 C 0.0611(4) 0.4324(4) 0.0901(3) 0.0374 1.0000 Uani . . . . . . C29 C -0.0320(4) 0.3969(5) 0.0411(4) 0.0506 1.0000 Uani . . . . . . O119 O 0.0715(3) 0.4384(3) 0.1596(2) 0.0374 1.0000 Uani . . . . . . O129 O 0.1215(3) 0.4540(3) 0.0583(2) 0.0402 1.0000 Uani . . . . . . N17 N 0.2605(3) 0.4667(3) -0.0212(3) 0.0385 1.0000 Uani . . . . . . C217 C 0.3551(4) 0.4772(4) -0.0231(4) 0.0388 1.0000 Uani . . . . . . C227 C 0.3975(4) 0.4568(4) 0.0424(3) 0.0377 1.0000 Uani . . . . . . O237 O 0.3824(3) 0.5064(3) 0.1128(2) 0.0364 1.0000 Uani . . . . . . C317 C 0.2350(4) 0.5368(4) -0.0341(4) 0.0425 1.0000 Uani . . . . . . C327 C 0.2774(4) 0.6198(4) 0.0354(4) 0.0407 1.0000 Uani . . . . . . O337 O 0.2617(3) 0.6039(3) 0.1024(2) 0.0343 1.0000 Uani . . . . . . C417 C 0.2009(4) 0.3861(5) -0.0823(4) 0.0479 1.0000 Uani . . . . . . C427 C 0.2197(6) 0.3084(5) -0.0788(4) 0.0616 1.0000 Uani . . . . . . O437 O 0.1533(5) 0.2381(4) -0.1394(4) 0.0900 1.0000 Uani . . . . . . N16 N 0.0429(3) 0.6815(4) 0.2984(3) 0.0402 1.0000 Uani . . . . . . C216 C -0.0078(4) 0.5897(4) 0.2747(4) 0.0408 1.0000 Uani . . . . . . C226 C 0.0430(4) 0.5491(4) 0.3158(4) 0.0421 1.0000 Uani . . . . . . O236 O 0.1297(3) 0.5699(3) 0.3044(2) 0.0366 1.0000 Uani . . . . . . C316 C 0.0421(4) 0.7062(5) 0.2289(4) 0.0437 1.0000 Uani . . . . . . C326 C 0.0974(4) 0.6689(5) 0.1776(3) 0.0399 1.0000 Uani . . . . . . O336 O 0.1820(2) 0.6889(3) 0.2262(2) 0.0360 1.0000 Uani . . . . . . C416 C 0.0030(4) 0.7367(5) 0.3516(4) 0.0472 1.0000 Uani . . . . . . C426 C -0.0016(4) 0.7267(5) 0.4275(4) 0.0535 1.0000 Uani . . . . . . O436 O 0.0779(3) 0.7726(4) 0.4875(3) 0.0680 1.0000 Uani . . . . . . N15 N 0.5122(3) 0.9222(4) 0.2864(3) 0.0417 1.0000 Uani . . . . . . C215 C 0.4345(5) 0.9207(5) 0.2320(4) 0.0486 1.0000 Uani . . . . . . C225 C 0.3506(4) 0.8604(4) 0.2335(4) 0.0460 1.0000 Uani . . . . . . O235 O 0.3610(3) 0.7801(3) 0.2202(2) 0.0364 1.0000 Uani . . . . . . C315 C 0.5139(5) 0.9681(4) 0.3699(4) 0.0460 1.0000 Uani . . . . . . C325 C 0.5328(4) 0.9178(4) 0.4167(4) 0.0390 1.0000 Uani . . . . . . O335 O 0.4731(3) 0.8334(3) 0.3784(2) 0.0337 1.0000 Uani . . . . . . C415 C 0.5929(5) 0.9646(4) 0.2667(4) 0.0496 1.0000 Uani . . . . . . C425 C 0.6781(5) 0.9684(5) 0.3165(5) 0.0563 1.0000 Uani . . . . . . O435 O 0.7479(4) 1.0009(4) 0.2844(4) 0.0711 1.0000 Uani . . . . . . N14 N 0.4499(3) 0.5379(3) 0.4232(3) 0.0376 1.0000 Uani . . . . . . C214 C 0.5036(4) 0.6178(4) 0.4841(3) 0.0384 1.0000 Uani . . . . . . C224 C 0.5215(4) 0.6861(4) 0.4521(3) 0.0329 1.0000 Uani . . . . . . O234 O 0.4394(2) 0.6879(3) 0.4149(2) 0.0326 1.0000 Uani . . . . . . C314 C 0.4945(4) 0.4915(4) 0.3719(4) 0.0370 1.0000 Uani . . . . . . C324 C 0.4501(4) 0.4689(4) 0.2874(4) 0.0374 1.0000 Uani . . . . . . O334 O 0.4467(3) 0.5430(3) 0.2751(2) 0.0318 1.0000 Uani . . . . . . C414 C 0.3691(4) 0.4907(4) 0.4362(4) 0.0394 1.0000 Uani . . . . . . C424 C 0.2956(4) 0.5251(4) 0.4195(3) 0.0345 1.0000 Uani . . . . . . O434 O 0.2841(2) 0.5242(3) 0.3423(2) 0.0322 1.0000 Uani . . . . . . O13 O 0.1154(3) 0.3966(3) 0.2913(3) 0.0386 1.0000 Uani . . . . . . C23 C 0.1498(4) 0.3452(4) 0.3140(4) 0.0394 1.0000 Uani . . . . . . C33 C 0.1335(4) 0.3305(4) 0.3809(4) 0.0449 1.0000 Uani . . . . . . C43 C 0.1708(5) 0.2817(5) 0.4103(5) 0.0567 1.0000 Uani . . . . . . C53 C 0.2261(6) 0.2444(5) 0.3729(5) 0.0650 1.0000 Uani . . . . . . C63 C 0.2404(5) 0.2556(5) 0.3054(5) 0.0575 1.0000 Uani . . . . . . C73 C 0.2032(4) 0.3043(4) 0.2738(4) 0.0436 1.0000 Uani . . . . . . C83 C 0.2209(4) 0.3121(4) 0.2007(4) 0.0440 1.0000 Uani . U . . . . N93 N 0.2167(3) 0.3762(3) 0.1855(3) 0.0337 1.0000 Uani . . . . . . O103 O 0.2330(3) 0.3798(3) 0.1162(2) 0.0383 1.0000 Uani . . . . . . C813 C 0.2464(6) 0.2435(5) 0.1478(5) 0.0634 1.0000 Uani . U . . . . C823 C 0.1938(9) 0.1608(7) 0.1262(7) 0.1057 1.0000 Uani . U . . . . C833 C 0.2210(11) 0.0947(8) 0.0832(8) 0.1337 1.0000 Uani . U . . . . C843 C 0.3004(10) 0.1149(8) 0.0639(8) 0.1211 1.0000 Uani . U . . . . C853 C 0.3533(8) 0.1933(7) 0.0877(6) 0.0859 1.0000 Uani . U . . . . C863 C 0.3265(6) 0.2581(6) 0.1302(5) 0.0681 1.0000 Uani . U . . . . O12 O 0.5639(3) 0.5275(3) 0.1768(2) 0.0371 1.0000 Uani . . . . . . C22 C 0.6319(4) 0.5274(4) 0.2254(4) 0.0370 1.0000 Uani . . . . . . C32 C 0.6513(4) 0.4519(4) 0.2114(4) 0.0438 1.0000 Uani . . . . . . C42 C 0.7200(5) 0.4472(5) 0.2614(5) 0.0539 1.0000 Uani . . . . . . C52 C 0.7721(5) 0.5175(5) 0.3254(5) 0.0581 1.0000 Uani . . . . . . C62 C 0.7563(4) 0.5933(5) 0.3379(5) 0.0507 1.0000 Uani . . . . . . C72 C 0.6861(4) 0.5996(4) 0.2892(4) 0.0385 1.0000 Uani . . . . . . C82 C 0.6740(4) 0.6829(4) 0.3075(4) 0.0340 1.0000 Uani . . . . . . N92 N 0.5992(3) 0.6899(3) 0.2793(3) 0.0335 1.0000 Uani . . . . . . O102 O 0.5954(3) 0.7696(3) 0.3025(3) 0.0405 1.0000 Uani . . . . . . C812 C 0.7469(4) 0.7619(4) 0.3598(4) 0.0403 1.0000 Uani . . . . . . C822 C 0.7559(4) 0.7934(5) 0.4394(4) 0.0487 1.0000 Uani . . . . . . C832 C 0.8225(5) 0.8665(5) 0.4866(5) 0.0580 1.0000 Uani . . . . . . C842 C 0.8786(5) 0.9096(5) 0.4536(6) 0.0666 1.0000 Uani . . . . . . C852 C 0.8706(5) 0.8795(6) 0.3745(7) 0.0751 1.0000 Uani . . . . . . C862 C 0.8044(5) 0.8045(5) 0.3272(5) 0.0540 1.0000 Uani . . . . . . O11 O 0.4641(3) 0.8412(3) 0.5356(2) 0.0372 1.0000 Uani . . . . . . C21 C 0.4665(4) 0.8156(4) 0.5946(3) 0.0365 1.0000 Uani . . . . . . C31 C 0.5488(4) 0.8436(5) 0.6495(4) 0.0438 1.0000 Uani . . . . . . C41 C 0.5566(5) 0.8179(5) 0.7112(4) 0.0523 1.0000 Uani . . . . . . C51 C 0.4862(5) 0.7628(6) 0.7210(5) 0.0611 1.0000 Uani . . . . . . C61 C 0.4053(5) 0.7367(5) 0.6704(4) 0.0533 1.0000 Uani . . . . . . C71 C 0.3935(4) 0.7626(4) 0.6076(3) 0.0380 1.0000 Uani . . . . . . C81 C 0.3034(4) 0.7361(4) 0.5576(3) 0.0372 1.0000 Uani . . . . . . N91 N 0.2927(3) 0.7367(3) 0.4883(3) 0.0346 1.0000 Uani . . . . . . O101 O 0.2061(3) 0.7101(3) 0.4466(2) 0.0406 1.0000 Uani . . . . . . C811 C 0.2270(4) 0.7092(4) 0.5907(4) 0.0389 1.0000 Uani . . . . . . C821 C 0.2187(5) 0.7667(5) 0.6579(4) 0.0539 1.0000 Uani . . . . . . C831 C 0.1508(5) 0.7434(6) 0.6908(5) 0.0616 1.0000 Uani . . . . . . C841 C 0.0906(5) 0.6626(6) 0.6590(4) 0.0550 1.0000 Uani . . . . . . C851 C 0.0981(4) 0.6048(5) 0.5919(5) 0.0517 1.0000 Uani . . . . . . C861 C 0.1665(4) 0.6290(5) 0.5586(4) 0.0468 1.0000 Uani . . . . . . O3 O 0.2611(2) 0.5486(3) 0.2139(2) 0.0306 1.0000 Uani . . . . . . O7 O 0.3060(2) 0.6979(2) 0.3334(2) 0.0292 1.0000 Uani . . . . . . O29 O 0.5168(3) 0.6459(3) 0.1174(2) 0.0377 1.0000 Uani . . . . . . C30 C 0.5205(4) 0.7160(4) 0.1132(4) 0.0357 1.0000 Uani . . . . . . O31 O 0.5109(3) 0.7770(3) 0.1650(3) 0.0412 1.0000 Uani . . . . . . C865 C 0.5384(5) 0.7317(5) 0.0416(4) 0.0550 1.0000 Uani . . . . . . O2 O 0.4186(2) 0.6660(2) 0.2434(2) 0.0294 1.0000 Uani . . . . . . H281 H 0.3018 1.0077 0.4289 0.0861 1.0000 Uiso R . . . . . H282 H 0.2453 0.9854 0.4851 0.0859 1.0000 Uiso R . . . . . H283 H 0.1994 0.9617 0.3974 0.0858 1.0000 Uiso R . . . . . H291 H -0.0439 0.4335 0.0161 0.0619 1.0000 Uiso R . . . . . H292 H -0.0744 0.3899 0.0716 0.0619 1.0000 Uiso R . . . . . H293 H -0.0419 0.3442 0.0028 0.0619 1.0000 Uiso R . . . . . H2171 H 0.3837 0.5352 -0.0159 0.0410 1.0000 Uiso R . . . . . H2172 H 0.3588 0.4418 -0.0732 0.0410 1.0000 Uiso R . . . . . H2271 H 0.4596 0.4730 0.0461 0.0379 1.0000 Uiso R . . . . . H2272 H 0.3738 0.3970 0.0335 0.0379 1.0000 Uiso R . . . . . H3171 H 0.2482 0.5434 -0.0808 0.0481 1.0000 Uiso R . . . . . H3172 H 0.1710 0.5219 -0.0413 0.0480 1.0000 Uiso R . . . . . H3271 H 0.2519 0.6628 0.0287 0.0457 1.0000 Uiso R . . . . . H3272 H 0.3398 0.6427 0.0417 0.0457 1.0000 Uiso R . . . . . H4171 H 0.2033 0.3898 -0.1330 0.0439 1.0000 Uiso R . . . . . H4172 H 0.1424 0.3833 -0.0741 0.0439 1.0000 Uiso R . . . . . H4271 H 0.2779 0.3097 -0.0901 0.0641 1.0000 Uiso R . . . . . H4272 H 0.2204 0.3022 -0.0283 0.0645 1.0000 Uiso R . . . . . H2161 H -0.0633 0.5861 0.2885 0.0451 1.0000 Uiso R . . . . . H2162 H -0.0185 0.5626 0.2186 0.0449 1.0000 Uiso R . . . . . H2261 H 0.0471 0.5736 0.3723 0.0490 1.0000 Uiso R . . . . . H2262 H 0.0147 0.4891 0.2974 0.0489 1.0000 Uiso R . . . . . H3161 H 0.0636 0.7673 0.2474 0.0448 1.0000 Uiso R . . . . . H3162 H -0.0184 0.6864 0.2000 0.0449 1.0000 Uiso R . . . . . H3261 H 0.1024 0.6918 0.1370 0.0450 1.0000 Uiso R . . . . . H3262 H 0.0716 0.6061 0.1528 0.0446 1.0000 Uiso R . . . . . H4161 H 0.0356 0.7949 0.3616 0.0499 1.0000 Uiso R . . . . . H4162 H -0.0566 0.7251 0.3227 0.0497 1.0000 Uiso R . . . . . H4261 H -0.0496 0.7444 0.4438 0.0578 1.0000 Uiso R . . . . . H4262 H -0.0142 0.6673 0.4186 0.0581 1.0000 Uiso R . . . . . H2151 H 0.4286 0.9766 0.2477 0.0526 1.0000 Uiso R . . . . . H2152 H 0.4423 0.9046 0.1794 0.0528 1.0000 Uiso R . . . . . H2251 H 0.3369 0.8811 0.2821 0.0511 1.0000 Uiso R . . . . . H2252 H 0.3039 0.8547 0.1920 0.0510 1.0000 Uiso R . . . . . H3151 H 0.5601 1.0233 0.3912 0.0509 1.0000 Uiso R . . . . . H3152 H 0.4581 0.9769 0.3740 0.0511 1.0000 Uiso R . . . . . H3251 H 0.5216 0.9423 0.4681 0.0366 1.0000 Uiso R . . . . . H3252 H 0.5916 0.9168 0.4218 0.0371 1.0000 Uiso R . . . . . H4151 H 0.5946 1.0216 0.2727 0.0480 1.0000 Uiso R . . . . . H4152 H 0.5893 0.9309 0.2132 0.0482 1.0000 Uiso R . . . . . H4251 H 0.6877 1.0052 0.3703 0.0578 1.0000 Uiso R . . . . . H4252 H 0.6774 0.9126 0.3145 0.0578 1.0000 Uiso R . . . . . H2141 H 0.5583 0.6132 0.5075 0.0397 1.0000 Uiso R . . . . . H2142 H 0.4730 0.6328 0.5250 0.0401 1.0000 Uiso R . . . . . H2241 H 0.5564 0.7402 0.4940 0.0302 1.0000 Uiso R . . . . . H2242 H 0.5552 0.6718 0.4128 0.0298 1.0000 Uiso R . . . . . H3141 H 0.5545 0.5259 0.3813 0.0429 1.0000 Uiso R . . . . . H3142 H 0.4924 0.4385 0.3789 0.0429 1.0000 Uiso R . . . . . H3241 H 0.4842 0.4429 0.2550 0.0395 1.0000 Uiso R . . . . . H3242 H 0.3908 0.4302 0.2741 0.0398 1.0000 Uiso R . . . . . H4141 H 0.3796 0.4952 0.4905 0.0460 1.0000 Uiso R . . . . . H4142 H 0.3516 0.4303 0.4011 0.0459 1.0000 Uiso R . . . . . H4241 H 0.3103 0.5832 0.4564 0.0380 1.0000 Uiso R . . . . . H4242 H 0.2409 0.4908 0.4248 0.0378 1.0000 Uiso R . . . . . H331 H 0.0950 0.3551 0.4064 0.0526 1.0000 Uiso R . . . . . H431 H 0.1614 0.2764 0.4572 0.0738 1.0000 Uiso R . . . . . H531 H 0.2531 0.2112 0.3919 0.0830 1.0000 Uiso R . . . . . H631 H 0.2783 0.2308 0.2811 0.0719 1.0000 Uiso R . . . . . H8231 H 0.1425 0.1517 0.1439 0.1222 1.0000 Uiso R . . . . . H8331 H 0.1836 0.0392 0.0658 0.1380 1.0000 Uiso R . . . . . H8431 H 0.3165 0.0725 0.0298 0.1322 1.0000 Uiso R . . . . . H8531 H 0.4106 0.2063 0.0817 0.1161 1.0000 Uiso R . . . . . H8631 H 0.3626 0.3137 0.1458 0.0970 1.0000 Uiso R . . . . . H321 H 0.6192 0.4060 0.1680 0.0494 1.0000 Uiso R . . . . . H421 H 0.7281 0.3956 0.2544 0.0648 1.0000 Uiso R . . . . . H521 H 0.8179 0.5154 0.3602 0.0638 1.0000 Uiso R . . . . . H621 H 0.7937 0.6415 0.3783 0.0548 1.0000 Uiso R . . . . . H8221 H 0.7168 0.7629 0.4603 0.0490 1.0000 Uiso R . . . . . H8321 H 0.8273 0.8879 0.5407 0.0622 1.0000 Uiso R . . . . . H8421 H 0.9217 0.9620 0.4846 0.0781 1.0000 Uiso R . . . . . H8521 H 0.9098 0.9078 0.3526 0.0830 1.0000 Uiso R . . . . . H8621 H 0.7972 0.7829 0.2731 0.0587 1.0000 Uiso R . . . . . H311 H 0.5973 0.8805 0.6434 0.0449 1.0000 Uiso R . . . . . H411 H 0.6118 0.8363 0.7445 0.0551 1.0000 Uiso R . . . . . H511 H 0.4949 0.7418 0.7611 0.0808 1.0000 Uiso R . . . . . H611 H 0.3567 0.6998 0.6765 0.0588 1.0000 Uiso R . . . . . H8211 H 0.2610 0.8200 0.6804 0.0549 1.0000 Uiso R . . . . . H8311 H 0.1431 0.7843 0.7345 0.0711 1.0000 Uiso R . . . . . H8411 H 0.0458 0.6468 0.6819 0.0660 1.0000 Uiso R . . . . . H8511 H 0.0585 0.5485 0.5704 0.0600 1.0000 Uiso R . . . . . H8611 H 0.1691 0.5908 0.5117 0.0547 1.0000 Uiso R . . . . . H8651 H 0.5164 0.7761 0.0373 0.0787 1.0000 Uiso R . . . . . H8652 H 0.6008 0.7497 0.0479 0.0792 1.0000 Uiso R . . . . . H8653 H 0.5116 0.6820 -0.0023 0.0789 1.0000 Uiso R . . . . . H1 H 0.1159 0.7515 0.4727 0.0860 1.0000 Uiso R . . . . . H8654 H 0.7971 1.0082 0.3120 0.0941 1.0000 Uiso R . . . . . H8655 H 0.1903 0.2126 -0.1410 0.1053 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 Fe1 0.0238(4) 0.0366(5) 0.0258(4) 0.0054(3) 0.0065(3) 0.0132(3) Fe2 0.0247(4) 0.0393(5) 0.0255(4) 0.0049(4) 0.0047(3) 0.0147(4) Fe3 0.0260(4) 0.0352(5) 0.0307(4) 0.0046(4) 0.0048(3) 0.0134(4) Fe4 0.0249(4) 0.0375(5) 0.0280(4) 0.0075(4) 0.0081(3) 0.0154(4) Fe5 0.0251(4) 0.0405(5) 0.0241(4) 0.0041(4) 0.0055(3) 0.0125(4) Fe6 0.0226(4) 0.0406(5) 0.0274(4) 0.0077(4) 0.0060(3) 0.0123(4) Fe7 0.0247(4) 0.0445(5) 0.0239(4) 0.0023(4) 0.0043(3) 0.0171(4) Fe8 0.0261(4) 0.0381(5) 0.0256(4) 0.0026(4) 0.0030(3) 0.0151(4) C18 0.041(4) 0.047(4) 0.027(3) 0.001(3) 0.005(3) 0.023(3) C28 0.053(5) 0.061(5) 0.062(5) -0.003(4) -0.014(4) 0.034(4) O118 0.033(2) 0.048(3) 0.037(2) 0.002(2) 0.0026(19) 0.022(2) O128 0.036(2) 0.042(3) 0.034(2) 0.0020(19) 0.0031(18) 0.021(2) C19 0.034(3) 0.041(4) 0.030(3) 0.004(3) 0.003(3) 0.015(3) C29 0.028(3) 0.071(5) 0.040(4) 0.013(4) -0.001(3) 0.010(3) O119 0.025(2) 0.052(3) 0.030(2) 0.0085(19) 0.0068(17) 0.0134(19) O129 0.030(2) 0.055(3) 0.030(2) 0.009(2) 0.0066(18) 0.015(2) N17 0.036(3) 0.048(3) 0.027(3) 0.003(2) 0.008(2) 0.018(2) C217 0.033(3) 0.045(4) 0.035(3) 0.003(3) 0.016(3) 0.018(3) C227 0.032(3) 0.042(4) 0.031(3) 0.000(3) 0.013(2) 0.013(3) O237 0.028(2) 0.046(3) 0.029(2) 0.0020(18) 0.0105(17) 0.0162(19) C317 0.040(3) 0.063(5) 0.030(3) 0.017(3) 0.011(3) 0.023(3) C327 0.042(4) 0.049(4) 0.035(3) 0.014(3) 0.015(3) 0.021(3) O337 0.031(2) 0.045(3) 0.025(2) 0.0079(18) 0.0075(16) 0.0160(19) C417 0.040(4) 0.061(5) 0.028(3) 0.000(3) 0.007(3) 0.014(3) C427 0.065(5) 0.054(5) 0.041(4) -0.001(3) 0.000(4) 0.010(4) O437 0.086(5) 0.073(4) 0.063(4) -0.005(3) -0.012(3) 0.003(4) N16 0.028(3) 0.056(3) 0.033(3) 0.005(2) 0.005(2) 0.023(2) C216 0.021(3) 0.058(4) 0.038(3) 0.007(3) 0.011(2) 0.014(3) C226 0.026(3) 0.052(4) 0.046(4) 0.011(3) 0.015(3) 0.016(3) O236 0.026(2) 0.050(3) 0.033(2) 0.0080(19) 0.0104(17) 0.0168(19) C316 0.030(3) 0.059(4) 0.038(3) 0.010(3) 0.001(3) 0.021(3) C326 0.029(3) 0.063(4) 0.024(3) 0.007(3) 0.002(2) 0.022(3) O336 0.025(2) 0.049(3) 0.027(2) 0.0039(18) 0.0036(16) 0.0158(19) C416 0.033(3) 0.065(5) 0.040(4) 0.006(3) 0.009(3) 0.027(3) C426 0.032(3) 0.079(5) 0.042(4) 0.004(4) 0.011(3) 0.029(4) O436 0.047(3) 0.101(4) 0.041(3) -0.006(3) 0.004(2) 0.042(3) N15 0.033(3) 0.048(3) 0.038(3) 0.008(2) 0.006(2) 0.014(2) C215 0.056(4) 0.046(4) 0.049(4) 0.016(3) 0.010(3) 0.028(4) C225 0.039(4) 0.054(4) 0.047(4) 0.014(3) 0.006(3) 0.026(3) O235 0.030(2) 0.043(3) 0.035(2) 0.0100(19) 0.0046(17) 0.0196(19) C315 0.046(4) 0.034(4) 0.045(4) -0.002(3) 0.008(3) 0.014(3) C325 0.031(3) 0.034(3) 0.039(3) 0.000(3) 0.005(3) 0.009(3) O335 0.029(2) 0.037(2) 0.028(2) 0.0043(17) 0.0013(16) 0.0118(18) C415 0.050(4) 0.037(4) 0.051(4) 0.006(3) 0.008(3) 0.014(3) C425 0.040(4) 0.051(5) 0.059(5) 0.013(4) 0.001(3) 0.002(3) O435 0.048(3) 0.066(4) 0.083(4) 0.017(3) 0.010(3) 0.009(3) N14 0.032(3) 0.040(3) 0.038(3) 0.008(2) 0.011(2) 0.014(2) C214 0.032(3) 0.045(4) 0.030(3) 0.002(3) -0.001(2) 0.019(3) C224 0.023(3) 0.040(3) 0.031(3) 0.006(3) 0.004(2) 0.013(2) O234 0.028(2) 0.043(2) 0.025(2) 0.0036(17) 0.0034(16) 0.0215(18) C314 0.034(3) 0.040(4) 0.040(3) 0.012(3) 0.015(3) 0.018(3) C324 0.036(3) 0.039(4) 0.038(3) 0.009(3) 0.014(3) 0.018(3) O334 0.030(2) 0.040(2) 0.029(2) 0.0103(18) 0.0111(17) 0.0177(18) C414 0.042(4) 0.041(4) 0.035(3) 0.012(3) 0.007(3) 0.019(3) C424 0.031(3) 0.044(4) 0.029(3) 0.008(3) 0.012(2) 0.016(3) O434 0.028(2) 0.042(2) 0.026(2) 0.0095(18) 0.0059(16) 0.0135(18) O13 0.030(2) 0.043(3) 0.043(2) 0.014(2) 0.0119(19) 0.0121(19) C23 0.027(3) 0.038(4) 0.046(4) 0.011(3) 0.005(3) 0.006(3) C33 0.035(3) 0.049(4) 0.052(4) 0.020(3) 0.011(3) 0.014(3) C43 0.052(4) 0.061(5) 0.064(5) 0.031(4) 0.018(4) 0.018(4) C53 0.073(6) 0.066(6) 0.080(6) 0.042(5) 0.029(5) 0.037(5) C63 0.056(5) 0.057(5) 0.074(5) 0.032(4) 0.028(4) 0.028(4) C73 0.039(4) 0.044(4) 0.046(4) 0.013(3) 0.010(3) 0.013(3) C83 0.042(3) 0.048(4) 0.045(4) 0.014(3) 0.014(3) 0.022(3) N93 0.022(2) 0.041(3) 0.030(3) 0.006(2) 0.0063(19) 0.007(2) O103 0.036(2) 0.043(3) 0.033(2) 0.0079(19) 0.0114(18) 0.014(2) C813 0.085(4) 0.052(4) 0.064(4) 0.017(3) 0.032(4) 0.037(3) C823 0.137(7) 0.065(5) 0.104(6) 0.007(5) 0.051(5) 0.035(5) C833 0.174(8) 0.078(6) 0.132(7) 0.006(5) 0.060(6) 0.042(6) C843 0.164(8) 0.095(6) 0.112(6) 0.011(5) 0.072(6) 0.067(6) C853 0.126(6) 0.094(5) 0.074(5) 0.033(4) 0.057(5) 0.073(5) C863 0.096(5) 0.078(5) 0.055(4) 0.026(4) 0.036(4) 0.059(4) O12 0.033(2) 0.046(3) 0.033(2) 0.0075(19) 0.0117(18) 0.021(2) C22 0.028(3) 0.051(4) 0.042(3) 0.020(3) 0.018(3) 0.018(3) C32 0.037(3) 0.047(4) 0.054(4) 0.020(3) 0.017(3) 0.021(3) C42 0.044(4) 0.052(5) 0.075(5) 0.029(4) 0.013(4) 0.026(4) C52 0.034(4) 0.056(5) 0.085(6) 0.031(4) 0.000(4) 0.017(3) C62 0.032(3) 0.056(5) 0.065(5) 0.024(4) 0.008(3) 0.016(3) C72 0.019(3) 0.049(4) 0.053(4) 0.023(3) 0.011(3) 0.013(3) C82 0.025(3) 0.042(4) 0.037(3) 0.017(3) 0.010(2) 0.011(3) N92 0.028(2) 0.037(3) 0.034(3) 0.008(2) 0.007(2) 0.015(2) O102 0.030(2) 0.040(3) 0.043(2) 0.005(2) 0.0033(19) 0.0147(19) C812 0.020(3) 0.043(4) 0.058(4) 0.020(3) 0.004(3) 0.012(3) C822 0.029(3) 0.054(4) 0.053(4) 0.019(4) -0.001(3) 0.006(3) C832 0.036(4) 0.055(5) 0.072(5) 0.018(4) -0.005(4) 0.014(3) C842 0.033(4) 0.039(4) 0.101(7) 0.003(4) 0.003(4) 0.004(3) C852 0.039(4) 0.061(6) 0.122(9) 0.032(6) 0.029(5) 0.009(4) C862 0.043(4) 0.053(5) 0.073(5) 0.028(4) 0.019(4) 0.018(3) O11 0.036(2) 0.043(3) 0.027(2) 0.0047(18) 0.0012(17) 0.019(2) C21 0.035(3) 0.042(4) 0.025(3) -0.002(3) 0.000(2) 0.022(3) C31 0.031(3) 0.055(4) 0.038(3) 0.008(3) 0.004(3) 0.017(3) C41 0.040(4) 0.080(6) 0.037(4) 0.018(4) 0.000(3) 0.029(4) C51 0.043(4) 0.095(7) 0.048(4) 0.031(4) 0.007(3) 0.022(4) C61 0.033(3) 0.084(6) 0.048(4) 0.032(4) 0.011(3) 0.016(4) C71 0.036(3) 0.052(4) 0.027(3) 0.008(3) 0.010(2) 0.022(3) C81 0.029(3) 0.050(4) 0.031(3) 0.009(3) 0.005(2) 0.019(3) N91 0.022(2) 0.042(3) 0.029(3) 0.000(2) 0.0024(19) 0.014(2) O101 0.024(2) 0.064(3) 0.027(2) 0.007(2) 0.0039(17) 0.018(2) C811 0.032(3) 0.048(4) 0.035(3) 0.011(3) 0.010(3) 0.015(3) C821 0.038(4) 0.064(5) 0.046(4) 0.007(4) 0.012(3) 0.011(3) C831 0.054(5) 0.078(6) 0.047(4) 0.010(4) 0.023(4) 0.023(4) C841 0.035(4) 0.086(6) 0.057(5) 0.035(4) 0.022(3) 0.026(4) C851 0.032(3) 0.061(5) 0.062(5) 0.024(4) 0.015(3) 0.012(3) C861 0.040(4) 0.053(4) 0.048(4) 0.013(3) 0.014(3) 0.021(3) O3 0.0230(19) 0.044(2) 0.0209(18) 0.0043(17) 0.0062(15) 0.0131(17) O7 0.0245(19) 0.036(2) 0.0208(18) 0.0004(16) 0.0051(15) 0.0128(17) O29 0.034(2) 0.043(3) 0.037(2) 0.010(2) 0.0125(18) 0.017(2) C30 0.027(3) 0.042(4) 0.039(3) 0.014(3) 0.010(3) 0.014(3) O31 0.041(2) 0.039(3) 0.044(3) 0.012(2) 0.014(2) 0.017(2) C865 0.072(5) 0.051(4) 0.053(4) 0.019(4) 0.031(4) 0.030(4) O2 0.0216(18) 0.035(2) 0.0269(19) 0.0023(17) 0.0043(15) 0.0144(16) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.17871(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . O234 . 1.930(4) yes Fe1 . O334 . 1.937(4) yes Fe1 . O434 . 1.931(4) yes Fe1 . O3 . 2.148(4) yes Fe1 . O7 . 2.144(4) yes Fe1 . O2 . 2.120(4) yes Fe2 . O337 . 1.950(4) yes Fe2 . O336 . 1.937(4) yes Fe2 . O235 . 1.924(4) yes Fe2 . O3 . 2.075(4) yes Fe2 . O7 . 2.097(4) yes Fe2 . O2 . 2.073(4) yes Fe3 . N15 . 2.265(6) yes Fe3 . O235 . 2.039(4) yes Fe3 . O335 . 1.995(4) yes Fe3 . O102 . 1.944(4) yes Fe3 . O31 . 2.038(4) yes Fe3 . O2 . 1.936(4) yes Fe4 . O237 . 1.975(4) yes Fe4 . O334 . 1.998(4) yes Fe4 . O12 . 1.923(4) yes Fe4 . N92 . 2.164(5) yes Fe4 . O29 . 2.073(4) yes Fe4 . O2 . 1.981(4) yes Fe5 . O129 . 2.060(4) yes Fe5 . N17 . 2.289(5) yes Fe5 . O237 . 1.992(4) yes Fe5 . O337 . 2.022(4) yes Fe5 . O103 . 1.946(5) yes Fe5 . O3 . 1.943(4) yes Fe6 . O119 . 2.058(4) yes Fe6 . O236 . 1.984(4) yes Fe6 . O434 . 2.002(4) yes Fe6 . O13 . 1.930(4) yes Fe6 . N93 . 2.175(5) yes Fe6 . O3 . 1.973(4) yes Fe7 . O118 . 2.044(5) yes Fe7 . N16 . 2.279(5) yes Fe7 . O236 . 1.988(4) yes Fe7 . O336 . 2.011(4) yes Fe7 . O101 . 1.962(4) yes Fe7 . O7 . 1.919(4) yes Fe8 . O128 . 2.062(4) yes Fe8 . O335 . 1.963(4) yes Fe8 . O234 . 1.986(4) yes Fe8 . O11 . 1.926(4) yes Fe8 . N91 . 2.173(5) yes Fe8 . O7 . 1.985(4) yes C18 . C28 . 1.492(9) yes C18 . O118 . 1.257(7) yes C18 . O128 . 1.273(7) yes C28 . H281 . 0.959 no C28 . H282 . 0.957 no C28 . H283 . 0.976 no C19 . C29 . 1.502(8) yes C19 . O119 . 1.252(7) yes C19 . O129 . 1.256(7) yes C29 . H291 . 0.949 no C29 . H292 . 0.963 no C29 . H293 . 0.932 no N17 . C217 . 1.505(7) yes N17 . C317 . 1.479(8) yes N17 . C417 . 1.483(8) yes C217 . C227 . 1.506(9) yes C217 . H2171 . 0.964 no C217 . H2172 . 0.968 no C227 . O237 . 1.425(6) yes C227 . H2271 . 0.960 no C227 . H2272 . 0.974 no C317 . C327 . 1.524(9) yes C317 . H3171 . 0.962 no C317 . H3172 . 0.981 no C327 . O337 . 1.409(7) yes C327 . H3271 . 0.985 no C327 . H3272 . 0.962 no C417 . C427 . 1.499(11) yes C417 . H4171 . 0.974 no C417 . H4172 . 0.975 no C427 . O437 . 1.430(9) yes C427 . H4271 . 0.993 no C427 . H4272 . 0.982 no O437 . H8655 . 0.838 no N16 . C216 . 1.497(8) yes N16 . C316 . 1.493(8) yes N16 . C416 . 1.503(7) yes C216 . C226 . 1.504(9) yes C216 . H2161 . 0.964 no C216 . H2162 . 0.972 no C226 . O236 . 1.425(7) yes C226 . H2261 . 0.990 no C226 . H2262 . 0.959 no C316 . C326 . 1.521(8) yes C316 . H3161 . 0.968 no C316 . H3162 . 0.964 no C326 . O336 . 1.421(6) yes C326 . H3261 . 0.969 no C326 . H3262 . 0.998 no C416 . C426 . 1.495(10) yes C416 . H4161 . 0.967 no C416 . H4162 . 0.972 no C426 . O436 . 1.428(8) yes C426 . H4261 . 0.966 no C426 . H4262 . 0.968 no O436 . H1 . 0.838 no N15 . C215 . 1.491(8) yes N15 . C315 . 1.506(8) yes N15 . C415 . 1.487(9) yes C215 . C225 . 1.503(10) yes C215 . H2151 . 0.973 no C215 . H2152 . 0.970 no C225 . O235 . 1.420(8) yes C225 . H2251 . 0.947 no C225 . H2252 . 0.961 no C315 . C325 . 1.484(9) yes C315 . H3151 . 0.978 no C315 . H3152 . 0.968 no C325 . O335 . 1.429(7) yes C325 . H3251 . 0.986 no C325 . H3252 . 0.951 no C415 . C425 . 1.525(10) yes C415 . H4151 . 0.970 no C415 . H4152 . 0.972 no C425 . O435 . 1.431(9) yes C425 . H4251 . 0.972 no C425 . H4252 . 0.970 no O435 . H8654 . 0.839 no N14 . C214 . 1.448(8) yes N14 . C314 . 1.459(7) yes N14 . C414 . 1.457(8) yes C214 . C224 . 1.490(9) yes C214 . H2141 . 0.967 no C214 . H2142 . 0.975 no C224 . O234 . 1.424(6) yes C224 . H2241 . 0.982 no C224 . H2242 . 0.986 no C314 . C324 . 1.514(8) yes C314 . H3141 . 0.961 no C314 . H3142 . 0.977 no C324 . O334 . 1.411(7) yes C324 . H3241 . 0.968 no C324 . H3242 . 0.968 no C414 . C424 . 1.512(8) yes C414 . H4141 . 0.978 no C414 . H4142 . 0.996 no C424 . O434 . 1.423(7) yes C424 . H4241 . 0.979 no C424 . H4242 . 0.973 no O13 . C23 . 1.326(8) yes C23 . C33 . 1.402(9) yes C23 . C73 . 1.417(9) yes C33 . C43 . 1.373(10) yes C33 . H331 . 0.951 no C43 . C53 . 1.388(11) yes C43 . H431 . 0.940 no C53 . C63 . 1.378(11) yes C53 . H531 . 0.941 no C63 . C73 . 1.394(10) yes C63 . H631 . 0.934 no C73 . C83 . 1.476(10) yes C83 . N93 . 1.267(8) yes C83 . C813 . 1.496(9) yes N93 . O103 . 1.375(6) yes C813 . C823 . 1.378(13) yes C813 . C863 . 1.367(12) yes C823 . C833 . 1.406(15) yes C823 . H8231 . 0.935 no C833 . C843 . 1.377(18) yes C833 . H8331 . 0.930 no C843 . C853 . 1.316(16) yes C843 . H8431 . 0.939 no C853 . C863 . 1.383(11) yes C853 . H8531 . 0.929 no C863 . H8631 . 0.929 no O12 . C22 . 1.325(7) yes C22 . C32 . 1.401(9) yes C22 . C72 . 1.404(9) yes C32 . C42 . 1.386(9) yes C32 . H321 . 0.909 no C42 . C52 . 1.381(11) yes C42 . H421 . 0.925 no C52 . C62 . 1.382(10) yes C52 . H521 . 0.932 no C62 . C72 . 1.405(9) yes C62 . H621 . 0.924 no C72 . C82 . 1.473(9) yes C82 . N92 . 1.304(7) yes C82 . C812 . 1.497(8) yes N92 . O102 . 1.356(6) yes C812 . C822 . 1.383(10) yes C812 . C862 . 1.376(10) yes C822 . C832 . 1.375(10) yes C822 . H8221 . 0.934 no C832 . C842 . 1.372(12) yes C832 . H8321 . 0.943 no C842 . C852 . 1.376(13) yes C842 . H8421 . 0.942 no C852 . C862 . 1.390(11) yes C852 . H8521 . 0.928 no C862 . H8621 . 0.938 no O11 . C21 . 1.316(8) yes C21 . C31 . 1.422(8) yes C21 . C71 . 1.410(9) yes C31 . C41 . 1.368(10) yes C31 . H311 . 0.928 no C41 . C51 . 1.372(11) yes C41 . H411 . 0.926 no C51 . C61 . 1.372(10) yes C51 . H511 . 0.944 no C61 . C71 . 1.393(9) yes C61 . H611 . 0.930 no C71 . C81 . 1.484(8) yes C81 . N91 . 1.285(8) yes C81 . C811 . 1.498(8) yes N91 . O101 . 1.383(6) yes C811 . C821 . 1.391(9) yes C811 . C861 . 1.376(9) yes C821 . C831 . 1.372(10) yes C821 . H8211 . 0.928 no C831 . C841 . 1.382(11) yes C831 . H8311 . 0.953 no C841 . C851 . 1.388(10) yes C841 . H8411 . 0.923 no C851 . C861 . 1.387(9) yes C851 . H8511 . 0.949 no C861 . H8611 . 0.936 no O29 . C30 . 1.251(7) yes C30 . O31 . 1.260(7) yes C30 . C865 . 1.502(9) yes C865 . H8651 . 0.962 no C865 . H8652 . 0.957 no C865 . H8653 . 0.935 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 O234 . Fe1 . O334 . 104.86(16) yes O234 . Fe1 . O434 . 104.17(17) yes O334 . Fe1 . O434 . 104.96(17) yes O234 . Fe1 . O3 . 154.81(15) yes O334 . Fe1 . O3 . 98.75(15) yes O434 . Fe1 . O3 . 77.57(16) yes O234 . Fe1 . O7 . 77.05(15) yes O334 . Fe1 . O7 . 156.58(17) yes O434 . Fe1 . O7 . 96.97(16) yes O3 . Fe1 . O7 . 77.80(14) yes O234 . Fe1 . O2 . 98.12(16) yes O334 . Fe1 . O2 . 77.91(15) yes O434 . Fe1 . O2 . 155.76(15) yes O3 . Fe1 . O2 . 78.21(15) yes O7 . Fe1 . O2 . 78.71(14) yes O337 . Fe2 . O336 . 100.79(16) yes O337 . Fe2 . O235 . 102.63(18) yes O336 . Fe2 . O235 . 100.53(18) yes O337 . Fe2 . O3 . 79.18(16) yes O336 . Fe2 . O3 . 98.35(17) yes O235 . Fe2 . O3 . 160.30(16) yes O337 . Fe2 . O7 . 159.36(17) yes O336 . Fe2 . O7 . 78.69(15) yes O235 . Fe2 . O7 . 97.70(17) yes O3 . Fe2 . O7 . 80.49(15) yes O337 . Fe2 . O2 . 99.33(15) yes O336 . Fe2 . O2 . 159.35(16) yes O235 . Fe2 . O2 . 79.43(16) yes O3 . Fe2 . O2 . 80.92(15) yes O7 . Fe2 . O2 . 80.85(14) yes N15 . Fe3 . O235 . 80.70(18) yes N15 . Fe3 . O335 . 78.51(18) yes O235 . Fe3 . O335 . 94.21(16) yes N15 . Fe3 . O102 . 106.83(19) yes O235 . Fe3 . O102 . 170.40(17) yes O335 . Fe3 . O102 . 93.16(17) yes N15 . Fe3 . O31 . 82.00(19) yes O235 . Fe3 . O31 . 86.18(17) yes O335 . Fe3 . O31 . 160.18(18) yes O102 . Fe3 . O31 . 88.97(18) yes N15 . Fe3 . O2 . 160.56(17) yes O235 . Fe3 . O2 . 80.01(16) yes O335 . Fe3 . O2 . 100.57(17) yes O102 . Fe3 . O2 . 92.61(17) yes O31 . Fe3 . O2 . 99.02(17) yes O237 . Fe4 . O334 . 92.25(17) yes O237 . Fe4 . O12 . 95.93(17) yes O334 . Fe4 . O12 . 92.55(17) yes O237 . Fe4 . N92 . 173.46(19) yes O334 . Fe4 . N92 . 94.27(18) yes O12 . Fe4 . N92 . 84.36(18) yes O237 . Fe4 . O29 . 87.47(18) yes O334 . Fe4 . O29 . 175.65(16) yes O12 . Fe4 . O29 . 91.79(17) yes N92 . Fe4 . O29 . 85.99(18) yes O237 . Fe4 . O2 . 95.78(15) yes O334 . Fe4 . O2 . 79.89(16) yes O12 . Fe4 . O2 . 166.29(17) yes N92 . Fe4 . O2 . 84.82(16) yes O29 . Fe4 . O2 . 95.82(17) yes O129 . Fe5 . N17 . 82.51(17) yes O129 . Fe5 . O237 . 160.66(16) yes N17 . Fe5 . O237 . 78.70(17) yes O129 . Fe5 . O337 . 86.30(17) yes N17 . Fe5 . O337 . 79.36(18) yes O237 . Fe5 . O337 . 94.65(17) yes O129 . Fe5 . O103 . 87.88(18) yes N17 . Fe5 . O103 . 106.80(19) yes O237 . Fe5 . O103 . 93.16(18) yes O337 . Fe5 . O103 . 170.90(17) yes O129 . Fe5 . O3 . 100.19(16) yes N17 . Fe5 . O3 . 159.62(19) yes O237 . Fe5 . O3 . 99.03(16) yes O337 . Fe5 . O3 . 80.66(16) yes O103 . Fe5 . O3 . 93.52(18) yes O119 . Fe6 . O236 . 87.02(17) yes O119 . Fe6 . O434 . 176.42(17) yes O236 . Fe6 . O434 . 92.89(16) yes O119 . Fe6 . O13 . 90.45(18) yes O236 . Fe6 . O13 . 97.08(18) yes O434 . Fe6 . O13 . 93.11(18) yes O119 . Fe6 . N93 . 86.06(17) yes O236 . Fe6 . N93 . 173.04(18) yes O434 . Fe6 . N93 . 93.97(17) yes O13 . Fe6 . N93 . 83.75(19) yes O119 . Fe6 . O3 . 96.25(16) yes O236 . Fe6 . O3 . 95.66(17) yes O434 . Fe6 . O3 . 80.19(16) yes O13 . Fe6 . O3 . 165.89(17) yes N93 . Fe6 . O3 . 84.33(17) yes O118 . Fe7 . N16 . 81.61(19) yes O118 . Fe7 . O236 . 160.08(16) yes N16 . Fe7 . O236 . 79.06(18) yes O118 . Fe7 . O336 . 87.03(18) yes N16 . Fe7 . O336 . 80.74(17) yes O236 . Fe7 . O336 . 94.53(17) yes O118 . Fe7 . O101 . 88.61(19) yes N16 . Fe7 . O101 . 104.28(18) yes O236 . Fe7 . O101 . 91.52(19) yes O336 . Fe7 . O101 . 172.80(18) yes O118 . Fe7 . O7 . 99.61(17) yes N16 . Fe7 . O7 . 161.89(18) yes O236 . Fe7 . O7 . 100.25(16) yes O336 . Fe7 . O7 . 81.27(16) yes O101 . Fe7 . O7 . 93.82(16) yes O128 . Fe8 . O335 . 88.39(18) yes O128 . Fe8 . O234 . 177.43(17) yes O335 . Fe8 . O234 . 90.31(17) yes O128 . Fe8 . O11 . 90.67(17) yes O335 . Fe8 . O11 . 97.48(18) yes O234 . Fe8 . O11 . 91.69(16) yes O128 . Fe8 . N91 . 85.28(18) yes O335 . Fe8 . N91 . 173.58(18) yes O234 . Fe8 . N91 . 95.97(18) yes O11 . Fe8 . N91 . 83.67(18) yes O128 . Fe8 . O7 . 98.27(16) yes O335 . Fe8 . O7 . 94.96(16) yes O234 . Fe8 . O7 . 79.64(15) yes O11 . Fe8 . O7 . 164.87(19) yes N91 . Fe8 . O7 . 84.93(17) yes C28 . C18 . O118 . 117.8(6) yes C28 . C18 . O128 . 117.6(6) yes O118 . C18 . O128 . 124.6(6) yes C18 . C28 . H281 . 110.4 no C18 . C28 . H282 . 110.6 no H281 . C28 . H282 . 109.5 no C18 . C28 . H283 . 108.5 no H281 . C28 . H283 . 109.0 no H282 . C28 . H283 . 108.7 no Fe7 . O118 . C18 . 129.4(4) yes Fe8 . O128 . C18 . 133.1(4) yes C29 . C19 . O119 . 116.8(6) yes C29 . C19 . O129 . 117.6(6) yes O119 . C19 . O129 . 125.6(6) yes C19 . C29 . H291 . 110.8 no C19 . C29 . H292 . 112.1 no H291 . C29 . H292 . 107.0 no C19 . C29 . H293 . 110.9 no H291 . C29 . H293 . 108.3 no H292 . C29 . H293 . 107.6 no Fe6 . O119 . C19 . 135.9(4) yes Fe5 . O129 . C19 . 126.3(4) yes Fe5 . N17 . C217 . 106.2(4) yes Fe5 . N17 . C317 . 102.5(3) yes C217 . N17 . C317 . 110.9(5) yes Fe5 . N17 . C417 . 117.8(4) yes C217 . N17 . C417 . 110.8(5) yes C317 . N17 . C417 . 108.3(5) yes N17 . C217 . C227 . 108.4(5) yes N17 . C217 . H2171 . 107.8 no C227 . C217 . H2171 . 110.2 no N17 . C217 . H2172 . 110.6 no C227 . C217 . H2172 . 111.9 no H2171 . C217 . H2172 . 107.8 no C217 . C227 . O237 . 108.2(5) yes C217 . C227 . H2271 . 107.5 no O237 . C227 . H2271 . 109.0 no C217 . C227 . H2272 . 111.6 no O237 . C227 . H2272 . 110.0 no H2271 . C227 . H2272 . 110.5 no C227 . O237 . Fe5 . 111.9(3) yes C227 . O237 . Fe4 . 119.1(3) yes Fe5 . O237 . Fe4 . 128.39(19) yes N17 . C317 . C327 . 112.3(5) yes N17 . C317 . H3171 . 111.2 no C327 . C317 . H3171 . 110.5 no N17 . C317 . H3172 . 107.3 no C327 . C317 . H3172 . 107.6 no H3171 . C317 . H3172 . 107.6 no C317 . C327 . O337 . 107.5(5) yes C317 . C327 . H3271 . 110.4 no O337 . C327 . H3271 . 110.4 no C317 . C327 . H3272 . 112.5 no O337 . C327 . H3272 . 109.4 no H3271 . C327 . H3272 . 106.6 no C327 . O337 . Fe5 . 118.4(4) yes C327 . O337 . Fe2 . 135.8(4) yes Fe5 . O337 . Fe2 . 99.90(18) yes N17 . C417 . C427 . 115.0(6) yes N17 . C417 . H4171 . 108.3 no C427 . C417 . H4171 . 110.1 no N17 . C417 . H4172 . 104.6 no C427 . C417 . H4172 . 109.1 no H4171 . C417 . H4172 . 109.5 no C417 . C427 . O437 . 106.4(7) yes C417 . C427 . H4271 . 109.2 no O437 . C427 . H4271 . 108.4 no C417 . C427 . H4272 . 114.0 no O437 . C427 . H4272 . 110.5 no H4271 . C427 . H4272 . 108.2 no C427 . O437 . H8655 . 86.8 no Fe7 . N16 . C216 . 105.8(3) yes Fe7 . N16 . C316 . 101.5(4) yes C216 . N16 . C316 . 110.7(5) yes Fe7 . N16 . C416 . 120.2(4) yes C216 . N16 . C416 . 111.6(5) yes C316 . N16 . C416 . 106.4(5) yes N16 . C216 . C226 . 110.1(5) yes N16 . C216 . H2161 . 107.4 no C226 . C216 . H2161 . 110.7 no N16 . C216 . H2162 . 108.7 no C226 . C216 . H2162 . 110.5 no H2161 . C216 . H2162 . 109.4 no C216 . C226 . O236 . 107.7(5) yes C216 . C226 . H2261 . 108.7 no O236 . C226 . H2261 . 108.2 no C216 . C226 . H2262 . 111.5 no O236 . C226 . H2262 . 111.7 no H2261 . C226 . H2262 . 108.9 no C226 . O236 . Fe7 . 112.5(4) yes C226 . O236 . Fe6 . 120.5(4) yes Fe7 . O236 . Fe6 . 126.8(2) yes N16 . C316 . C326 . 112.5(5) yes N16 . C316 . H3161 . 107.8 no C326 . C316 . H3161 . 110.7 no N16 . C316 . H3162 . 106.9 no C326 . C316 . H3162 . 110.2 no H3161 . C316 . H3162 . 108.7 no C316 . C326 . O336 . 107.5(5) yes C316 . C326 . H3261 . 111.0 no O336 . C326 . H3261 . 110.3 no C316 . C326 . H3262 . 111.5 no O336 . C326 . H3262 . 107.8 no H3261 . C326 . H3262 . 108.6 no C326 . O336 . Fe7 . 117.0(3) yes C326 . O336 . Fe2 . 137.1(3) yes Fe7 . O336 . Fe2 . 100.26(18) yes N16 . C416 . C426 . 117.5(6) yes N16 . C416 . H4161 . 107.8 no C426 . C416 . H4161 . 108.9 no N16 . C416 . H4162 . 106.7 no C426 . C416 . H4162 . 108.1 no H4161 . C416 . H4162 . 107.4 no C416 . C426 . O436 . 114.2(6) yes C416 . C426 . H4261 . 107.9 no O436 . C426 . H4261 . 110.0 no C416 . C426 . H4262 . 107.6 no O436 . C426 . H4262 . 107.9 no H4261 . C426 . H4262 . 109.2 no C426 . O436 . H1 . 106.2 no Fe3 . N15 . C215 . 102.6(4) yes Fe3 . N15 . C315 . 106.6(4) yes C215 . N15 . C315 . 111.3(5) yes Fe3 . N15 . C415 . 117.8(4) yes C215 . N15 . C415 . 107.9(5) yes C315 . N15 . C415 . 110.4(5) yes N15 . C215 . C225 . 111.6(6) yes N15 . C215 . H2151 . 109.4 no C225 . C215 . H2151 . 107.4 no N15 . C215 . H2152 . 110.0 no C225 . C215 . H2152 . 109.5 no H2151 . C215 . H2152 . 108.9 no C215 . C225 . O235 . 108.9(5) yes C215 . C225 . H2251 . 110.1 no O235 . C225 . H2251 . 110.5 no C215 . C225 . H2252 . 108.7 no O235 . C225 . H2252 . 108.4 no H2251 . C225 . H2252 . 110.1 no C225 . O235 . Fe3 . 114.6(4) yes C225 . O235 . Fe2 . 137.7(4) yes Fe3 . O235 . Fe2 . 100.09(18) yes N15 . C315 . C325 . 109.3(5) yes N15 . C315 . H3151 . 110.3 no C325 . C315 . H3151 . 108.6 no N15 . C315 . H3152 . 110.8 no C325 . C315 . H3152 . 109.6 no H3151 . C315 . H3152 . 108.2 no C315 . C325 . O335 . 108.1(5) yes C315 . C325 . H3251 . 108.1 no O335 . C325 . H3251 . 108.7 no C315 . C325 . H3252 . 111.6 no O335 . C325 . H3252 . 109.2 no H3251 . C325 . H3252 . 111.1 no C325 . O335 . Fe3 . 110.9(4) yes C325 . O335 . Fe8 . 120.7(4) yes Fe3 . O335 . Fe8 . 128.3(2) yes N15 . C415 . C425 . 113.7(6) yes N15 . C415 . H4151 . 109.0 no C425 . C415 . H4151 . 108.9 no N15 . C415 . H4152 . 106.7 no C425 . C415 . H4152 . 106.9 no H4151 . C415 . H4152 . 111.7 no C415 . C425 . O435 . 106.8(6) yes C415 . C425 . H4251 . 110.6 no O435 . C425 . H4251 . 110.1 no C415 . C425 . H4252 . 111.4 no O435 . C425 . H4252 . 108.3 no H4251 . C425 . H4252 . 109.6 no C425 . O435 . H8654 . 110.8 no C214 . N14 . C314 . 117.4(5) yes C214 . N14 . C414 . 118.1(5) yes C314 . N14 . C414 . 118.6(5) yes N14 . C214 . C224 . 110.3(5) yes N14 . C214 . H2141 . 110.1 no C224 . C214 . H2141 . 110.3 no N14 . C214 . H2142 . 109.9 no C224 . C214 . H2142 . 108.5 no H2141 . C214 . H2142 . 107.7 no C214 . C224 . O234 . 108.4(5) yes C214 . C224 . H2241 . 109.8 no O234 . C224 . H2241 . 112.4 no C214 . C224 . H2242 . 107.9 no O234 . C224 . H2242 . 108.9 no H2241 . C224 . H2242 . 109.4 no C224 . O234 . Fe8 . 130.2(3) yes C224 . O234 . Fe1 . 122.3(3) yes Fe8 . O234 . Fe1 . 105.22(17) yes N14 . C314 . C324 . 110.5(5) yes N14 . C314 . H3141 . 110.0 no C324 . C314 . H3141 . 107.6 no N14 . C314 . H3142 . 111.3 no C324 . C314 . H3142 . 107.0 no H3141 . C314 . H3142 . 110.4 no C314 . C324 . O334 . 109.4(5) yes C314 . C324 . H3241 . 108.7 no O334 . C324 . H3241 . 109.5 no C314 . C324 . H3242 . 110.5 no O334 . C324 . H3242 . 109.0 no H3241 . C324 . H3242 . 109.7 no C324 . O334 . Fe4 . 132.0(3) yes C324 . O334 . Fe1 . 122.3(3) yes Fe4 . O334 . Fe1 . 103.63(18) yes N14 . C414 . C424 . 110.9(5) yes N14 . C414 . H4141 . 109.1 no C424 . C414 . H4141 . 108.8 no N14 . C414 . H4142 . 108.9 no C424 . C414 . H4142 . 109.2 no H4141 . C414 . H4142 . 109.8 no C414 . C424 . O434 . 109.1(5) yes C414 . C424 . H4241 . 109.8 no O434 . C424 . H4241 . 109.5 no C414 . C424 . H4242 . 110.4 no O434 . C424 . H4242 . 109.3 no H4241 . C424 . H4242 . 108.7 no C424 . O434 . Fe6 . 132.0(3) yes C424 . O434 . Fe1 . 121.1(4) yes Fe6 . O434 . Fe1 . 104.14(18) yes Fe6 . O13 . C23 . 124.3(4) yes O13 . C23 . C33 . 119.0(6) yes O13 . C23 . C73 . 123.0(6) yes C33 . C23 . C73 . 118.0(6) yes C23 . C33 . C43 . 122.3(7) yes C23 . C33 . H331 . 118.4 no C43 . C33 . H331 . 119.3 no C33 . C43 . C53 . 119.8(7) yes C33 . C43 . H431 . 119.8 no C53 . C43 . H431 . 120.3 no C43 . C53 . C63 . 118.8(8) yes C43 . C53 . H531 . 121.8 no C63 . C53 . H531 . 119.4 no C53 . C63 . C73 . 122.9(7) yes C53 . C63 . H631 . 118.1 no C73 . C63 . H631 . 119.0 no C23 . C73 . C63 . 118.1(7) yes C23 . C73 . C83 . 122.4(6) yes C63 . C73 . C83 . 119.5(6) yes C73 . C83 . N93 . 120.2(6) yes C73 . C83 . C813 . 117.6(6) yes N93 . C83 . C813 . 122.2(6) yes Fe6 . N93 . C83 . 127.0(4) yes Fe6 . N93 . O103 . 115.1(4) yes C83 . N93 . O103 . 117.8(5) yes N93 . O103 . Fe5 . 116.8(3) yes C83 . C813 . C823 . 118.8(8) yes C83 . C813 . C863 . 122.4(8) yes C823 . C813 . C863 . 118.0(8) yes C813 . C823 . C833 . 119.9(12) yes C813 . C823 . H8231 . 116.9 no C833 . C823 . H8231 . 123.1 no C823 . C833 . C843 . 118.5(13) yes C823 . C833 . H8331 . 119.6 no C843 . C833 . H8331 . 121.7 no C833 . C843 . C853 . 122.1(11) yes C833 . C843 . H8431 . 120.1 no C853 . C843 . H8431 . 117.6 no C843 . C853 . C863 . 119.1(11) yes C843 . C853 . H8531 . 122.1 no C863 . C853 . H8531 . 118.4 no C853 . C863 . C813 . 122.2(10) yes C853 . C863 . H8631 . 119.7 no C813 . C863 . H8631 . 118.1 no Fe4 . O12 . C22 . 129.7(4) yes O12 . C22 . C32 . 118.3(6) yes O12 . C22 . C72 . 123.0(6) yes C32 . C22 . C72 . 118.7(6) yes C22 . C32 . C42 . 121.0(7) yes C22 . C32 . H321 . 119.1 no C42 . C32 . H321 . 119.9 no C32 . C42 . C52 . 120.5(7) yes C32 . C42 . H421 . 119.8 no C52 . C42 . H421 . 119.4 no C42 . C52 . C62 . 119.2(7) yes C42 . C52 . H521 . 121.9 no C62 . C52 . H521 . 118.9 no C52 . C62 . C72 . 121.5(7) yes C52 . C62 . H621 . 119.5 no C72 . C62 . H621 . 118.9 no C62 . C72 . C22 . 119.0(6) yes C62 . C72 . C82 . 117.7(6) yes C22 . C72 . C82 . 123.3(6) yes C72 . C82 . N92 . 121.0(5) yes C72 . C82 . C812 . 120.8(5) yes N92 . C82 . C812 . 118.2(5) yes Fe4 . N92 . C82 . 127.8(4) yes Fe4 . N92 . O102 . 116.9(3) yes C82 . N92 . O102 . 115.3(5) yes N92 . O102 . Fe3 . 117.7(3) yes C82 . C812 . C822 . 121.2(6) yes C82 . C812 . C862 . 118.8(7) yes C822 . C812 . C862 . 119.9(7) yes C812 . C822 . C832 . 120.6(7) yes C812 . C822 . H8221 . 118.5 no C832 . C822 . H8221 . 120.9 no C822 . C832 . C842 . 119.2(8) yes C822 . C832 . H8321 . 119.9 no C842 . C832 . H8321 . 120.9 no C832 . C842 . C852 . 121.1(8) yes C832 . C842 . H8421 . 120.3 no C852 . C842 . H8421 . 118.6 no C842 . C852 . C862 . 119.6(8) yes C842 . C852 . H8521 . 120.8 no C862 . C852 . H8521 . 119.6 no C852 . C862 . C812 . 119.6(8) yes C852 . C862 . H8621 . 121.2 no C812 . C862 . H8621 . 119.1 no Fe8 . O11 . C21 . 128.7(4) yes O11 . C21 . C31 . 117.6(6) yes O11 . C21 . C71 . 124.9(5) yes C31 . C21 . C71 . 117.5(6) yes C21 . C31 . C41 . 120.8(7) yes C21 . C31 . H311 . 119.2 no C41 . C31 . H311 . 120.0 no C31 . C41 . C51 . 121.3(7) yes C31 . C41 . H411 . 117.9 no C51 . C41 . H411 . 120.7 no C41 . C51 . C61 . 119.2(7) yes C41 . C51 . H511 . 119.3 no C61 . C51 . H511 . 121.5 no C51 . C61 . C71 . 121.7(7) yes C51 . C61 . H611 . 120.4 no C71 . C61 . H611 . 117.9 no C21 . C71 . C61 . 119.5(6) yes C21 . C71 . C81 . 121.5(6) yes C61 . C71 . C81 . 119.0(6) yes C71 . C81 . N91 . 120.2(6) yes C71 . C81 . C811 . 117.9(5) yes N91 . C81 . C811 . 122.0(5) yes Fe8 . N91 . C81 . 129.0(4) yes Fe8 . N91 . O101 . 115.5(4) yes C81 . N91 . O101 . 115.4(5) yes N91 . O101 . Fe7 . 116.4(3) yes C81 . C811 . C821 . 118.6(6) yes C81 . C811 . C861 . 122.4(6) yes C821 . C811 . C861 . 118.9(6) yes C811 . C821 . C831 . 120.1(7) yes C811 . C821 . H8211 . 118.6 no C831 . C821 . H8211 . 121.3 no C821 . C831 . C841 . 120.9(7) yes C821 . C831 . H8311 . 119.6 no C841 . C831 . H8311 . 119.4 no C831 . C841 . C851 . 119.5(7) yes C831 . C841 . H8411 . 120.6 no C851 . C841 . H8411 . 119.9 no C841 . C851 . C861 . 119.3(7) yes C841 . C851 . H8511 . 120.4 no C861 . C851 . H8511 . 120.3 no C851 . C861 . C811 . 121.3(7) yes C851 . C861 . H8611 . 118.8 no C811 . C861 . H8611 . 119.8 no Fe1 . O3 . Fe2 . 84.71(14) yes Fe1 . O3 . Fe6 . 97.60(16) yes Fe2 . O3 . Fe6 . 136.09(19) yes Fe1 . O3 . Fe5 . 131.27(18) yes Fe2 . O3 . Fe5 . 98.30(17) yes Fe6 . O3 . Fe5 . 111.63(19) yes Fe1 . O7 . Fe2 . 84.27(13) yes Fe1 . O7 . Fe8 . 97.70(16) yes Fe2 . O7 . Fe8 . 136.3(2) yes Fe1 . O7 . Fe7 . 132.3(2) yes Fe2 . O7 . Fe7 . 97.91(16) yes Fe8 . O7 . Fe7 . 111.43(17) yes Fe4 . O29 . C30 . 133.5(4) yes O29 . C30 . O31 . 125.7(6) yes O29 . C30 . C865 . 119.0(6) yes O31 . C30 . C865 . 115.4(6) yes Fe3 . O31 . C30 . 129.3(4) yes C30 . C865 . H8651 . 108.5 no C30 . C865 . H8652 . 107.9 no H8651 . C865 . H8652 . 109.2 no C30 . C865 . H8653 . 109.9 no H8651 . C865 . H8653 . 111.2 no H8652 . C865 . H8653 . 109.9 no Fe1 . O2 . Fe2 . 85.46(14) yes Fe1 . O2 . Fe4 . 97.85(17) yes Fe2 . O2 . Fe4 . 135.20(19) yes Fe1 . O2 . Fe3 . 129.73(19) yes Fe2 . O2 . Fe3 . 98.49(16) yes Fe4 . O2 . Fe3 . 112.25(18) yes # Attachment '- pt9019-(1).cif' data_pt9019 _database_code_depnum_ccdc_archive 'CCDC 794871' #TrackingRef '- pt9019-(1).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Kevin Mason' _exptl_crystal_recrystallization_method 'Diffusion of Et2O into MeOH/pyridine solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H74 Br4 Fe8 N10 O18, 2Et2O, MeOH' _chemical_formula_sum 'C81 H98 Br4 Fe8 N10 O21' _chemical_formula_weight 2314.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting hexagonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 42.1099(11) _cell_length_b 42.1099(11) _cell_length_c 13.8971(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 21341.4(10) _cell_formula_units_Z 9 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7220 _cell_measurement_theta_min 2.4905 _cell_measurement_theta_max 25.521 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.621 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 10530 _exptl_absorpt_coefficient_mu 2.943 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6050 _exptl_absorpt_correction_T_max 0.8117 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 41524 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0902 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 57 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 29.83 _reflns_number_total 12493 _reflns_number_gt 7412 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<< #============================================================================== 602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure ! 043_ALERT_1_B Check Reported Molecular Weight ................ 2314.13 044_ALERT_1_B Calculated and Reported Dx Differ .............. ? 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? Platon squeeze has been used to treat diffuse solvent. Identification of solvent was not possible on the basis of q peaks and so the solvent was determined to be 2 molecules of ether and one molecule of MeOH per Fe8 unit from a best guess based on the electron count and reaction/recrystallisation solvents. F000, Dx, M and formulae have been given using this assumption. 232_ALERT_2_C Hirshfeld Test Diff (M-X) Br1 -- Fe1 .. 5.61 su Ok this often occurs with heavy elements in clusters. 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 2 913_ALERT_3_C Missing # of Very Strong Reflections in FCF .... 1 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 1127 The data collection strategy used was to collect fully complete data to 2TH= 53deg. Some higher angle data were collected in the process and these have been included in the refinement. Please refer to the completeness statistics below #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 1.000 4968 4966 2 23.01 0.550 1.000 6621 6619 2 25.24 0.600 1.000 8588 8585 3 #----------------------------------------------------------- ACTA Min. Res. --- 27.51 0.650 0.999 10907 10891 16 29.83 0.700 0.917 13623 12493 1130 060_ALERT_4_C Ratio Tmax/Tmin (Exp-to-Rep) (too) Large ....... 1.17 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay etc. The crystal was a rather irregular shape, being a fragment of a larger block; this precluded integration methods for correcting for absorption. 950_ALERT_1_C Reported and Calculated Hmax Values Differ by .. 3 Platon is treating H and K as equivalent for this calculation (i.e. post merged data) due to the equivalence in a and b for hexagonal axes. This is slightly different from the physically measured Hmax value prior to merging which shelx is reporting in the cif but not the FCF. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 1 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 6 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12493 _refine_ls_number_parameters 505 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1181 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.820457(13) 0.182065(13) -0.01626(3) 0.02556(12) Uani 1 1 d U . . Fe2 Fe 0.867989(13) 0.167269(13) 0.13160(4) 0.02537(12) Uani 1 1 d . . . Fe3 Fe 0.808118(13) 0.083679(13) 0.22354(4) 0.02689(12) Uani 1 1 d . . . Fe4 Fe 0.786186(14) 0.036258(14) 0.41066(4) 0.03091(13) Uani 1 1 d . . . Br1 Br 0.790328(10) 0.161095(11) -0.16897(3) 0.03820(11) Uani 1 1 d U . . Br2 Br 0.720972(10) -0.013727(10) 0.40408(3) 0.03876(11) Uani 1 1 d . . . O123 O 0.82203(6) 0.13509(6) 0.21211(16) 0.0254(5) Uani 1 1 d . . . C1A C 0.86208(9) 0.14776(10) -0.0835(3) 0.0302(8) Uani 1 1 d . . . O1A O 0.84322(6) 0.15063(6) -0.00747(16) 0.0272(5) Uani 1 1 d . . . C2A C 0.88643(9) 0.17840(9) -0.1392(3) 0.0276(8) Uani 1 1 d . . . C3A C 0.90331(10) 0.17263(10) -0.2189(3) 0.0344(9) Uani 1 1 d . . . H3A H 0.9193 0.1930 -0.2579 0.041 Uiso 1 1 calc R . . C4A C 0.89748(11) 0.13855(11) -0.2423(3) 0.0401(10) Uani 1 1 d . . . H4A H 0.9088 0.1352 -0.2976 0.048 Uiso 1 1 calc R . . C5A C 0.87495(12) 0.10902(11) -0.1844(3) 0.0462(11) Uani 1 1 d . . . H5A H 0.8716 0.0854 -0.1986 0.055 Uiso 1 1 calc R . . C6A C 0.85719(10) 0.11358(10) -0.1055(3) 0.0350(9) Uani 1 1 d . . . H6A H 0.8416 0.0931 -0.0665 0.042 Uiso 1 1 calc R . . C21A C 0.89763(9) 0.21608(9) -0.1087(2) 0.0273(8) Uani 1 1 d . . . N22A N 0.87492(7) 0.22142(7) -0.0607(2) 0.0258(6) Uani 1 1 d . . . O23A O 0.88842(6) 0.25613(6) -0.01870(16) 0.0276(5) Uani 1 1 d . . . C24A C 0.93565(9) 0.24645(9) -0.1310(3) 0.0329(9) Uani 1 1 d . . . H24A H 0.9419 0.2673 -0.0886 0.049 Uiso 1 1 calc R . . H24B H 0.9368 0.2540 -0.1982 0.049 Uiso 1 1 calc R . . H24C H 0.9531 0.2378 -0.1208 0.049 Uiso 1 1 calc R . . C1B C 0.94251(9) 0.18735(10) 0.0729(2) 0.0328(9) Uani 1 1 d . . . O1B O 0.91504(6) 0.19399(7) 0.07593(17) 0.0325(6) Uani 1 1 d . . . C2B C 0.93844(10) 0.15204(11) 0.0845(3) 0.0350(9) Uani 1 1 d . . . C3B C 0.97034(11) 0.14937(12) 0.0808(3) 0.0457(10) Uani 1 1 d . . . H3B H 0.9683 0.1260 0.0888 0.055 Uiso 1 1 calc R . . C4B C 1.00446(11) 0.17936(13) 0.0659(3) 0.0535(12) Uani 1 1 d . . . H4B H 1.0255 0.1766 0.0642 0.064 Uiso 1 1 calc R . . C5B C 1.00800(11) 0.21332(13) 0.0535(3) 0.0519(12) Uani 1 1 d . . . H5B H 1.0316 0.2340 0.0428 0.062 Uiso 1 1 calc R . . C6B C 0.97793(10) 0.21779(11) 0.0564(3) 0.0404(10) Uani 1 1 d . . . H6B H 0.9808 0.2415 0.0472 0.048 Uiso 1 1 calc R . . C21B C 0.90302(10) 0.11842(10) 0.0991(3) 0.0352(9) Uani 1 1 d . . . N22B N 0.87400(8) 0.12063(8) 0.1193(2) 0.0288(7) Uani 1 1 d . . . O23B O 0.84135(6) 0.08736(6) 0.12520(17) 0.0304(6) Uani 1 1 d . . . C24B C 0.90028(12) 0.08162(12) 0.0907(4) 0.0590(13) Uani 1 1 d . . . H24D H 0.8745 0.0623 0.0962 0.088 Uiso 1 1 calc R . . H24E H 0.9146 0.0788 0.1422 0.088 Uiso 1 1 calc R . . H24F H 0.9099 0.0797 0.0281 0.088 Uiso 1 1 calc R . . O1C O 0.80699(7) 0.00914(7) 0.4627(2) 0.0418(7) Uani 1 1 d . . . C1C C 0.83370(12) 0.02175(11) 0.5268(3) 0.0422(10) Uani 1 1 d . . . C2C C 0.86628(11) 0.05609(11) 0.5186(3) 0.0399(9) Uani 1 1 d . . . C3C C 0.89461(13) 0.06615(13) 0.5871(3) 0.0513(11) Uani 1 1 d . . . H3C H 0.9166 0.0891 0.5812 0.062 Uiso 1 1 calc R . . C4C C 0.89079(15) 0.04327(14) 0.6621(4) 0.0650(14) Uani 1 1 d . . . H4C H 0.9103 0.0500 0.7064 0.078 Uiso 1 1 calc R . . C5C C 0.85818(15) 0.01026(14) 0.6726(4) 0.0614(14) Uani 1 1 d . . . H5C H 0.8550 -0.0051 0.7261 0.074 Uiso 1 1 calc R . . C6C C 0.83026(13) -0.00043(12) 0.6060(3) 0.0497(11) Uani 1 1 d . . . H6C H 0.8083 -0.0233 0.6140 0.060 Uiso 1 1 calc R . . C21C C 0.87200(11) 0.08174(11) 0.4401(3) 0.0388(9) Uani 1 1 d . . . N22C N 0.84320(8) 0.08056(8) 0.4027(2) 0.0317(7) Uani 1 1 d . . . O23C O 0.85037(6) 0.10540(6) 0.32813(16) 0.0283(5) Uani 1 1 d . . . C24C C 0.90936(11) 0.10829(12) 0.4062(3) 0.0529(12) Uani 1 1 d . . . H24G H 0.9089 0.1119 0.3367 0.079 Uiso 1 1 calc R . . H24H H 0.9259 0.0988 0.4203 0.079 Uiso 1 1 calc R . . H24I H 0.9181 0.1318 0.4393 0.079 Uiso 1 1 calc R . . N1D N 0.76053(8) 0.06197(8) 0.1340(2) 0.0294(7) Uani 1 1 d . . . C2D C 0.72776(10) 0.03663(10) 0.1702(3) 0.0365(9) Uani 1 1 d . . . H2D H 0.7262 0.0297 0.2359 0.044 Uiso 1 1 calc R . . C3D C 0.69665(10) 0.02059(10) 0.1150(3) 0.0336(9) Uani 1 1 d . . . H3D H 0.6739 0.0028 0.1421 0.040 Uiso 1 1 calc R . . C4D C 0.69859(11) 0.03048(10) 0.0205(3) 0.0383(9) Uani 1 1 d . . . H4D H 0.6773 0.0193 -0.0188 0.046 Uiso 1 1 calc R . . C5D C 0.73156(11) 0.05663(11) -0.0169(3) 0.0385(9) Uani 1 1 d . . . H5D H 0.7334 0.0642 -0.0820 0.046 Uiso 1 1 calc R . . C6D C 0.76195(10) 0.07162(10) 0.0417(3) 0.0323(8) Uani 1 1 d . . . H6D H 0.7848 0.0895 0.0155 0.039 Uiso 1 1 calc R . . N1E N 0.78232(8) 0.05180(8) 0.5580(2) 0.0318(7) Uani 1 1 d . . . C2E C 0.76039(11) 0.02612(11) 0.6207(3) 0.0433(10) Uani 1 1 d . . . H2E H 0.7453 0.0016 0.5991 0.052 Uiso 1 1 calc R . . C3E C 0.75923(12) 0.03449(13) 0.7174(3) 0.0584(13) Uani 1 1 d . . . H3E H 0.7438 0.0159 0.7613 0.070 Uiso 1 1 calc R . . C4E C 0.78042(13) 0.06948(14) 0.7476(3) 0.0638(14) Uani 1 1 d . . . H4E H 0.7793 0.0758 0.8126 0.077 Uiso 1 1 calc R . . C5E C 0.80342(11) 0.09567(12) 0.6842(3) 0.0471(11) Uani 1 1 d . . . H5E H 0.8187 0.1203 0.7045 0.056 Uiso 1 1 calc R . . C6E C 0.80400(10) 0.08580(10) 0.5916(3) 0.0358(9) Uani 1 1 d . . . H6E H 0.8207 0.1040 0.5483 0.043 Uiso 1 1 calc R . . O1F O 0.88810(6) 0.18111(6) 0.26542(17) 0.0276(5) Uani 1 1 d . . . C2F C 0.92613(9) 0.19588(10) 0.2878(3) 0.0337(9) Uani 1 1 d . . . H2F1 H 0.9411 0.2096 0.2324 0.050 Uiso 1 1 calc R . . H2F2 H 0.9308 0.1758 0.3030 0.050 Uiso 1 1 calc R . . H2F3 H 0.9326 0.2123 0.3434 0.050 Uiso 1 1 calc R . . O1G O 0.79343(6) 0.03420(6) 0.27106(17) 0.0295(6) Uani 1 1 d . . . C2G C 0.79665(14) 0.00644(11) 0.2231(3) 0.0550(12) Uani 1 1 d . . . H2G1 H 0.8000 0.0118 0.1540 0.083 Uiso 1 1 calc R . . H2G2 H 0.7743 -0.0172 0.2334 0.083 Uiso 1 1 calc R . . H2G3 H 0.8178 0.0054 0.2485 0.083 Uiso 1 1 calc 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 0.0240(3) 0.0258(3) 0.0211(3) 0.0023(2) -0.0001(2) 0.0082(2) Fe2 0.0223(2) 0.0275(3) 0.0216(3) 0.0028(2) 0.0007(2) 0.0089(2) Fe3 0.0262(3) 0.0260(3) 0.0229(3) 0.0009(2) 0.0006(2) 0.0089(2) Fe4 0.0334(3) 0.0280(3) 0.0279(3) 0.0032(2) 0.0045(2) 0.0128(2) Br1 0.0381(2) 0.0404(2) 0.0258(2) -0.00125(17) -0.00502(17) 0.01184(18) Br2 0.0360(2) 0.0324(2) 0.0392(2) 0.00307(17) 0.00496(18) 0.01049(17) O123 0.0236(12) 0.0274(12) 0.0215(13) 0.0025(10) 0.0022(10) 0.0099(10) C1A 0.0289(19) 0.033(2) 0.025(2) -0.0027(16) -0.0058(16) 0.0123(16) O1A 0.0278(13) 0.0291(13) 0.0195(12) -0.0012(10) 0.0005(10) 0.0102(11) C2A 0.0287(18) 0.0259(18) 0.026(2) -0.0003(15) -0.0010(15) 0.0119(15) C3A 0.034(2) 0.033(2) 0.030(2) 0.0024(17) 0.0043(17) 0.0114(17) C4A 0.047(2) 0.041(2) 0.031(2) -0.0047(18) 0.0081(19) 0.020(2) C5A 0.061(3) 0.040(2) 0.040(3) -0.007(2) 0.001(2) 0.027(2) C6A 0.039(2) 0.030(2) 0.032(2) 0.0012(17) -0.0026(18) 0.0140(17) C21A 0.0281(18) 0.0321(19) 0.0196(18) 0.0058(15) 0.0024(15) 0.0134(16) N22A 0.0300(16) 0.0247(15) 0.0183(15) 0.0010(12) 0.0013(12) 0.0104(13) O23A 0.0300(13) 0.0239(12) 0.0223(13) 0.0013(10) 0.0022(10) 0.0086(11) C24A 0.0299(19) 0.034(2) 0.029(2) 0.0018(16) 0.0102(16) 0.0110(16) C1B 0.0263(19) 0.049(2) 0.0161(18) 0.0025(17) 0.0008(15) 0.0134(17) O1B 0.0217(12) 0.0385(14) 0.0313(15) 0.0064(12) 0.0039(11) 0.0105(11) C2B 0.0264(19) 0.045(2) 0.025(2) -0.0028(18) 0.0033(16) 0.0122(17) C3B 0.042(2) 0.053(3) 0.048(3) -0.002(2) 0.001(2) 0.028(2) C4B 0.029(2) 0.075(3) 0.058(3) -0.003(3) 0.001(2) 0.027(2) C5B 0.026(2) 0.066(3) 0.049(3) 0.005(2) 0.0042(19) 0.012(2) C6B 0.027(2) 0.048(2) 0.031(2) 0.0066(19) 0.0006(17) 0.0069(18) C21B 0.037(2) 0.041(2) 0.030(2) -0.0020(18) 0.0003(17) 0.0213(18) N22B 0.0287(16) 0.0309(16) 0.0221(16) 0.0043(13) 0.0025(13) 0.0112(13) O23B 0.0268(13) 0.0286(13) 0.0287(14) -0.0003(11) 0.0042(11) 0.0085(11) C24B 0.039(2) 0.051(3) 0.088(4) -0.007(3) 0.006(3) 0.024(2) O1C 0.0434(16) 0.0333(15) 0.0415(17) 0.0073(13) -0.0031(14) 0.0138(13) C1C 0.054(3) 0.041(2) 0.040(2) 0.002(2) 0.003(2) 0.031(2) C2C 0.044(2) 0.044(2) 0.037(2) 0.0047(19) -0.0016(19) 0.026(2) C3C 0.058(3) 0.055(3) 0.051(3) 0.004(2) -0.007(2) 0.035(2) C4C 0.084(4) 0.070(4) 0.050(3) 0.003(3) -0.018(3) 0.046(3) C5C 0.089(4) 0.059(3) 0.050(3) 0.015(2) 0.000(3) 0.047(3) C6C 0.064(3) 0.044(3) 0.047(3) 0.014(2) 0.009(2) 0.031(2) C21C 0.039(2) 0.040(2) 0.035(2) 0.0046(18) -0.0034(18) 0.0184(19) N22C 0.0353(17) 0.0314(17) 0.0264(17) 0.0057(13) 0.0045(14) 0.0150(14) O23C 0.0283(13) 0.0258(13) 0.0275(14) 0.0042(10) 0.0003(11) 0.0110(11) C24C 0.041(2) 0.058(3) 0.060(3) 0.017(2) 0.003(2) 0.025(2) N1D 0.0297(16) 0.0266(15) 0.0298(18) -0.0005(13) -0.0010(13) 0.0124(13) C2D 0.034(2) 0.036(2) 0.033(2) 0.0049(17) 0.0058(17) 0.0122(18) C3D 0.0280(19) 0.0294(19) 0.037(2) -0.0031(17) -0.0012(17) 0.0093(16) C4D 0.036(2) 0.039(2) 0.038(2) -0.0143(19) -0.0114(18) 0.0181(19) C5D 0.044(2) 0.046(2) 0.026(2) -0.0018(18) -0.0035(18) 0.023(2) C6D 0.033(2) 0.035(2) 0.024(2) 0.0013(16) 0.0032(16) 0.0132(17) N1E 0.0336(17) 0.0328(17) 0.0266(17) 0.0056(14) 0.0021(14) 0.0148(14) C2E 0.041(2) 0.040(2) 0.036(2) 0.0092(19) 0.0022(19) 0.0108(19) C3E 0.050(3) 0.065(3) 0.030(2) 0.011(2) 0.005(2) 0.006(2) C4E 0.051(3) 0.082(4) 0.026(2) -0.012(2) 0.005(2) 0.009(3) C5E 0.047(3) 0.055(3) 0.028(2) -0.008(2) -0.003(2) 0.017(2) C6E 0.036(2) 0.036(2) 0.030(2) 0.0037(17) -0.0045(17) 0.0142(18) O1F 0.0223(12) 0.0287(13) 0.0240(13) 0.0030(10) -0.0007(10) 0.0068(10) C2F 0.0246(18) 0.037(2) 0.030(2) -0.0017(17) -0.0049(16) 0.0085(16) O1G 0.0329(13) 0.0266(12) 0.0243(13) 0.0003(11) 0.0021(11) 0.0113(11) C2G 0.083(3) 0.041(2) 0.045(3) -0.001(2) 0.013(3) 0.034(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1F 1.960(2) 13_655 ? Fe1 O1A 1.989(2) . ? Fe1 O23C 2.047(2) 13_655 ? Fe1 O123 2.111(2) 13_655 ? Fe1 N22A 2.142(3) . ? Fe1 Br1 2.4026(6) . ? Fe2 O1B 1.887(2) . ? Fe2 O123 1.993(2) 13_655 ? Fe2 O1F 2.006(2) . ? Fe2 O123 2.052(2) . ? Fe2 N22B 2.109(3) . ? Fe2 O1A 2.141(2) . ? Fe3 O23B 1.906(2) . ? Fe3 O123 1.946(2) . ? Fe3 O1G 1.967(2) . ? Fe3 O23C 2.118(2) . ? Fe3 O23A 2.122(2) 13_655 ? Fe3 N1D 2.137(3) . ? Fe4 O1C 1.896(3) . ? Fe4 O1G 1.972(2) . ? Fe4 O23A 2.080(2) 13_655 ? Fe4 N1E 2.180(3) . ? Fe4 N22C 2.186(3) . ? Fe4 Br2 2.4900(6) . ? O123 Fe2 1.993(2) 13_655 ? O123 Fe1 2.111(2) 13_655 ? C1A O1A 1.364(4) . ? C1A C6A 1.382(5) . ? C1A C2A 1.411(5) . ? C2A C3A 1.402(5) . ? C2A C21A 1.473(5) . ? C3A C4A 1.368(5) . ? C3A H3A 0.9500 . ? C4A C5A 1.383(6) . ? C4A H4A 0.9500 . ? C5A C6A 1.394(5) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C21A N22A 1.275(4) . ? C21A C24A 1.499(4) . ? N22A O23A 1.403(3) . ? O23A Fe4 2.080(2) 13_655 ? O23A Fe3 2.122(2) 13_655 ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C1B O1B 1.319(4) . ? C1B C6B 1.417(5) . ? C1B C2B 1.418(5) . ? C2B C3B 1.404(5) . ? C2B C21B 1.469(5) . ? C3B C4B 1.374(6) . ? C3B H3B 0.9500 . ? C4B C5B 1.372(6) . ? C4B H4B 0.9500 . ? C5B C6B 1.371(6) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C21B N22B 1.301(4) . ? C21B C24B 1.500(5) . ? N22B O23B 1.391(3) . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? O1C C1C 1.320(5) . ? C1C C6C 1.403(6) . ? C1C C2C 1.415(6) . ? C2C C3C 1.416(6) . ? C2C C21C 1.468(5) . ? C3C C4C 1.373(6) . ? C3C H3C 0.9500 . ? C4C C5C 1.390(7) . ? C4C H4C 0.9500 . ? C5C C6C 1.383(6) . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? C21C N22C 1.297(5) . ? C21C C24C 1.479(5) . ? N22C O23C 1.394(3) . ? O23C Fe1 2.047(2) 13_655 ? C24C H24G 0.9800 . ? C24C H24H 0.9800 . ? C24C H24I 0.9800 . ? N1D C6D 1.339(5) . ? N1D C2D 1.350(4) . ? C2D C3D 1.370(5) . ? C2D H2D 0.9500 . ? C3D C4D 1.367(5) . ? C3D H3D 0.9500 . ? C4D C5D 1.372(5) . ? C4D H4D 0.9500 . ? C5D C6D 1.375(5) . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? N1E C2E 1.336(5) . ? N1E C6E 1.340(4) . ? C2E C3E 1.395(6) . ? C2E H2E 0.9500 . ? C3E C4E 1.352(6) . ? C3E H3E 0.9500 . ? C4E C5E 1.364(6) . ? C4E H4E 0.9500 . ? C5E C6E 1.356(5) . ? C5E H5E 0.9500 . ? C6E H6E 0.9500 . ? O1F C2F 1.433(4) . ? O1F Fe1 1.960(2) 13_655 ? C2F H2F1 0.9800 . ? C2F H2F2 0.9800 . ? C2F H2F3 0.9800 . ? O1G C2G 1.410(4) . ? C2G H2G1 0.9800 . ? C2G H2G2 0.9800 . ? C2G H2G3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1F Fe1 O1A 96.62(10) 13_655 . ? O1F Fe1 O23C 92.50(9) 13_655 13_655 ? O1A Fe1 O23C 156.41(9) . 13_655 ? O1F Fe1 O123 78.52(9) 13_655 13_655 ? O1A Fe1 O123 81.04(9) . 13_655 ? O23C Fe1 O123 79.54(9) 13_655 13_655 ? O1F Fe1 N22A 160.13(10) 13_655 . ? O1A Fe1 N22A 81.19(10) . . ? O23C Fe1 N22A 82.86(10) 13_655 . ? O123 Fe1 N22A 81.63(9) 13_655 . ? O1F Fe1 Br1 98.68(7) 13_655 . ? O1A Fe1 Br1 98.70(7) . . ? O23C Fe1 Br1 101.36(7) 13_655 . ? O123 Fe1 Br1 177.12(7) 13_655 . ? N22A Fe1 Br1 101.18(8) . . ? O1B Fe2 O123 107.14(10) . 13_655 ? O1B Fe2 O1F 92.40(10) . . ? O123 Fe2 O1F 98.73(9) 13_655 . ? O1B Fe2 O123 168.42(10) . . ? O123 Fe2 O123 81.99(9) 13_655 . ? O1F Fe2 O123 78.94(9) . . ? O1B Fe2 N22B 86.72(11) . . ? O123 Fe2 N22B 158.73(10) 13_655 . ? O1F Fe2 N22B 96.67(10) . . ? O123 Fe2 N22B 86.68(10) . . ? O1B Fe2 O1A 91.12(10) . . ? O123 Fe2 O1A 80.20(9) 13_655 . ? O1F Fe2 O1A 176.47(9) . . ? O123 Fe2 O1A 97.57(9) . . ? N22B Fe2 O1A 83.54(10) . . ? O23B Fe3 O123 92.90(10) . . ? O23B Fe3 O1G 98.97(10) . . ? O123 Fe3 O1G 164.98(10) . . ? O23B Fe3 O23C 91.88(10) . . ? O123 Fe3 O23C 81.66(9) . . ? O1G Fe3 O23C 88.76(9) . . ? O23B Fe3 O23A 167.90(10) . 13_655 ? O123 Fe3 O23A 92.35(9) . 13_655 ? O1G Fe3 O23A 74.29(9) . 13_655 ? O23C Fe3 O23A 78.12(9) . 13_655 ? O23B Fe3 N1D 96.37(11) . . ? O123 Fe3 N1D 97.17(10) . . ? O1G Fe3 N1D 90.65(10) . . ? O23C Fe3 N1D 171.73(10) . . ? O23A Fe3 N1D 93.78(10) 13_655 . ? O1C Fe4 O1G 102.76(11) . . ? O1C Fe4 O23A 164.37(10) . 13_655 ? O1G Fe4 O23A 75.15(9) . 13_655 ? O1C Fe4 N1E 87.05(12) . . ? O1G Fe4 N1E 166.71(10) . . ? O23A Fe4 N1E 92.97(10) 13_655 . ? O1C Fe4 N22C 83.82(11) . . ? O1G Fe4 N22C 81.93(10) . . ? O23A Fe4 N22C 80.55(10) 13_655 . ? N1E Fe4 N22C 90.37(11) . . ? O1C Fe4 Br2 98.70(8) . . ? O1G Fe4 Br2 93.22(7) . . ? O23A Fe4 Br2 96.89(7) 13_655 . ? N1E Fe4 Br2 94.12(8) . . ? N22C Fe4 Br2 174.95(8) . . ? Fe3 O123 Fe2 139.58(12) . 13_655 ? Fe3 O123 Fe2 116.05(11) . . ? Fe2 O123 Fe2 98.01(9) 13_655 . ? Fe3 O123 Fe1 96.52(9) . 13_655 ? Fe2 O123 Fe1 99.81(10) 13_655 13_655 ? Fe2 O123 Fe1 97.88(9) . 13_655 ? O1A C1A C6A 118.2(3) . . ? O1A C1A C2A 122.2(3) . . ? C6A C1A C2A 119.6(3) . . ? C1A O1A Fe1 120.5(2) . . ? C1A O1A Fe2 121.2(2) . . ? Fe1 O1A Fe2 98.96(10) . . ? C3A C2A C1A 118.3(3) . . ? C3A C2A C21A 119.8(3) . . ? C1A C2A C21A 121.5(3) . . ? C4A C3A C2A 121.9(3) . . ? C4A C3A H3A 119.0 . . ? C2A C3A H3A 119.0 . . ? C3A C4A C5A 119.2(4) . . ? C3A C4A H4A 120.4 . . ? C5A C4A H4A 120.4 . . ? C4A C5A C6A 120.5(4) . . ? C4A C5A H5A 119.8 . . ? C6A C5A H5A 119.8 . . ? C1A C6A C5A 120.4(4) . . ? C1A C6A H6A 119.8 . . ? C5A C6A H6A 119.8 . . ? N22A C21A C2A 118.4(3) . . ? N22A C21A C24A 122.2(3) . . ? C2A C21A C24A 119.3(3) . . ? C21A N22A O23A 116.9(3) . . ? C21A N22A Fe1 128.5(2) . . ? O23A N22A Fe1 113.90(18) . . ? N22A O23A Fe4 123.44(18) . 13_655 ? N22A O23A Fe3 108.12(16) . 13_655 ? Fe4 O23A Fe3 96.04(9) 13_655 13_655 ? C21A C24A H24A 109.5 . . ? C21A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C21A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? O1B C1B C6B 116.8(4) . . ? O1B C1B C2B 124.0(3) . . ? C6B C1B C2B 119.2(3) . . ? C1B O1B Fe2 131.1(2) . . ? C3B C2B C1B 117.4(3) . . ? C3B C2B C21B 118.6(4) . . ? C1B C2B C21B 123.9(3) . . ? C4B C3B C2B 122.3(4) . . ? C4B C3B H3B 118.8 . . ? C2B C3B H3B 118.8 . . ? C5B C4B C3B 119.7(4) . . ? C5B C4B H4B 120.1 . . ? C3B C4B H4B 120.1 . . ? C6B C5B C4B 120.9(4) . . ? C6B C5B H5B 119.6 . . ? C4B C5B H5B 119.6 . . ? C5B C6B C1B 120.5(4) . . ? C5B C6B H6B 119.8 . . ? C1B C6B H6B 119.8 . . ? N22B C21B C2B 119.9(3) . . ? N22B C21B C24B 120.0(3) . . ? C2B C21B C24B 120.1(3) . . ? C21B N22B O23B 115.6(3) . . ? C21B N22B Fe2 129.7(2) . . ? O23B N22B Fe2 114.5(2) . . ? N22B O23B Fe3 116.13(19) . . ? C21B C24B H24D 109.5 . . ? C21B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C21B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C1C O1C Fe4 124.9(2) . . ? O1C C1C C6C 118.5(4) . . ? O1C C1C C2C 123.5(4) . . ? C6C C1C C2C 117.9(4) . . ? C1C C2C C3C 119.5(4) . . ? C1C C2C C21C 122.0(4) . . ? C3C C2C C21C 118.4(4) . . ? C4C C3C C2C 121.0(4) . . ? C4C C3C H3C 119.5 . . ? C2C C3C H3C 119.5 . . ? C3C C4C C5C 119.5(5) . . ? C3C C4C H4C 120.3 . . ? C5C C4C H4C 120.3 . . ? C6C C5C C4C 120.6(4) . . ? C6C C5C H5C 119.7 . . ? C4C C5C H5C 119.7 . . ? C5C C6C C1C 121.4(4) . . ? C5C C6C H6C 119.3 . . ? C1C C6C H6C 119.3 . . ? N22C C21C C2C 117.6(3) . . ? N22C C21C C24C 121.5(3) . . ? C2C C21C C24C 120.9(3) . . ? C21C N22C O23C 114.9(3) . . ? C21C N22C Fe4 128.3(3) . . ? O23C N22C Fe4 114.30(19) . . ? N22C O23C Fe1 120.73(19) . 13_655 ? N22C O23C Fe3 111.47(17) . . ? Fe1 O23C Fe3 93.30(9) 13_655 . ? C21C C24C H24G 109.5 . . ? C21C C24C H24H 109.5 . . ? H24G C24C H24H 109.5 . . ? C21C C24C H24I 109.5 . . ? H24G C24C H24I 109.5 . . ? H24H C24C H24I 109.5 . . ? C6D N1D C2D 118.0(3) . . ? C6D N1D Fe3 122.6(2) . . ? C2D N1D Fe3 119.4(2) . . ? N1D C2D C3D 121.9(4) . . ? N1D C2D H2D 119.0 . . ? C3D C2D H2D 119.0 . . ? C4D C3D C2D 119.4(4) . . ? C4D C3D H3D 120.3 . . ? C2D C3D H3D 120.3 . . ? C3D C4D C5D 119.4(3) . . ? C3D C4D H4D 120.3 . . ? C5D C4D H4D 120.3 . . ? C4D C5D C6D 118.7(4) . . ? C4D C5D H5D 120.6 . . ? C6D C5D H5D 120.6 . . ? N1D C6D C5D 122.5(3) . . ? N1D C6D H6D 118.7 . . ? C5D C6D H6D 118.7 . . ? C2E N1E C6E 117.6(3) . . ? C2E N1E Fe4 119.7(3) . . ? C6E N1E Fe4 122.4(2) . . ? N1E C2E C3E 121.4(4) . . ? N1E C2E H2E 119.3 . . ? C3E C2E H2E 119.3 . . ? C4E C3E C2E 119.1(4) . . ? C4E C3E H3E 120.4 . . ? C2E C3E H3E 120.4 . . ? C3E C4E C5E 119.7(4) . . ? C3E C4E H4E 120.2 . . ? C5E C4E H4E 120.2 . . ? C6E C5E C4E 118.6(4) . . ? C6E C5E H5E 120.7 . . ? C4E C5E H5E 120.7 . . ? N1E C6E C5E 123.5(4) . . ? N1E C6E H6E 118.3 . . ? C5E C6E H6E 118.3 . . ? C2F O1F Fe1 127.0(2) . 13_655 ? C2F O1F Fe2 123.1(2) . . ? Fe1 O1F Fe2 104.66(10) 13_655 . ? O1F C2F H2F1 109.5 . . ? O1F C2F H2F2 109.5 . . ? H2F1 C2F H2F2 109.5 . . ? O1F C2F H2F3 109.5 . . ? H2F1 C2F H2F3 109.5 . . ? H2F2 C2F H2F3 109.5 . . ? C2G O1G Fe3 127.6(2) . . ? C2G O1G Fe4 125.6(2) . . ? Fe3 O1G Fe4 104.91(11) . . ? O1G C2G H2G1 109.5 . . ? O1G C2G H2G2 109.5 . . ? H2G1 C2G H2G2 109.5 . . ? O1G C2G H2G3 109.5 . . ? H2G1 C2G H2G3 109.5 . . ? H2G2 C2G H2G3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.649 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.107 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 -0.004 1517 320 ' ' 2 0.333 0.667 0.793 1515 319 ' ' 3 0.667 0.333 0.459 1515 320 ' ' _platon_squeeze_details ; ; # Attachment '- pt9026-(2).cif' data_pt9026 _database_code_depnum_ccdc_archive 'CCDC 794872' #TrackingRef '- pt9026-(2).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Kevin Mason' _exptl_crystal_recrystallization_method 'slow evaporation of MeOH/pyridine solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C71.70 H73.10 Fe8 N22.90 O17.70' _chemical_formula_sum 'C71.70 H73.10 Fe8 N22.90 O17.70' _chemical_formula_weight 1985.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9923(4) _cell_length_b 28.0040(10) _cell_length_c 13.3217(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.382(2) _cell_angle_gamma 90.00 _cell_volume 4074.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8144 _cell_measurement_theta_min 2.365 _cell_measurement_theta_max 26.2575 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2026 _exptl_absorpt_coefficient_mu 1.463 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6566 _exptl_absorpt_correction_T_max 0.8423 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 38657 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 26.42 _reflns_number_total 8336 _reflns_number_gt 6650 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2 220_ALERT_2_B Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.81 Ratio 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for N2H 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 29.20 Deg. N2H -N1H -N2H' 1.555 1.555 1.555 One of the azide ligand labelled H has two position disorder. Some atoms did not refine well anisotropically and so were left isotropic. Thermal motion is as expected for a 3 atom chain tethered at one end. N2H is in the middle adjacent to N3H which has the highest thermal motion. 213_ALERT_2_C Atom N3F has ADP max/min Ratio ............. 3.50 prola 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? 077_ALERT_4_C Unitcell contains non-integer number of atoms .. ? There is substitutional disorder in one of the ligand positions. Either a methoxy, MeO or azide, N3 occupy the site and relative occupancies were determined approximately by refinement then fixed to 0.85 for the MeO, and 0.15 for the N3. This has lead to non integer values for unit cell contents. A rounding error seems to have been made during calculation of F000 as all other formulae and parameters calculated from the formula match. 220_ALERT_2_C Large Non-Solvent C Ueq(max)/Ueq(min) ... 3.19 Ratio 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C3E There is slight thermal motion in one of the pyriding rings. C3E is at the point of maximum motion and so appears slightly more stretched out. 910_ALERT_3_C Missing # of FCF Reflections Below Th(Min) ..... 1 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 29 301_ALERT_3_G Note Main Residue Disorder .................... 6.00 Perc. Yes see above. Both substitutional and positional disorder are present. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 8 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0439P)^2^+3.7867P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8336 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0586 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0941 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.61922(4) 0.028358(15) 0.05800(3) 0.01830(11) Uani 1 1 d . . . Fe2 Fe 0.37034(4) 0.083783(15) -0.05245(3) 0.01881(11) Uani 1 1 d . . . Fe3 Fe 0.35704(4) 0.147256(16) -0.34707(4) 0.02147(12) Uani 1 1 d . . . Fe4 Fe 0.42615(4) 0.045663(15) -0.23926(3) 0.01912(11) Uani 1 1 d . . . O123 O 0.47126(18) 0.02921(7) -0.08528(16) 0.0176(4) Uani 1 1 d . . . C1A C 0.8391(3) 0.08944(11) 0.1186(3) 0.0230(7) Uani 1 1 d . . . O1A O 0.73268(19) 0.07209(7) 0.04740(17) 0.0231(5) Uani 1 1 d . . . C2A C 0.8819(3) 0.08434(11) 0.2345(3) 0.0244(7) Uani 1 1 d . . . C3A C 0.9908(3) 0.10806(12) 0.3012(3) 0.0317(8) Uani 1 1 d . . . H3A H 1.0197 0.1058 0.3791 0.038 Uiso 1 1 calc R . . C4A C 1.0568(3) 0.13444(13) 0.2577(3) 0.0374(9) Uani 1 1 d . . . H4A H 1.1290 0.1506 0.3052 0.045 Uiso 1 1 calc R . . C5A C 1.0182(3) 0.13747(13) 0.1449(3) 0.0356(9) Uani 1 1 d . . . H5A H 1.0648 0.1549 0.1145 0.043 Uiso 1 1 calc R . . C6A C 0.9106(3) 0.11473(12) 0.0762(3) 0.0290(8) Uani 1 1 d . . . H6A H 0.8850 0.1164 -0.0013 0.035 Uiso 1 1 calc R . . C21A C 0.8168(3) 0.05759(11) 0.2885(3) 0.0255(7) Uani 1 1 d . . . N22A N 0.7189(2) 0.03265(9) 0.2309(2) 0.0215(6) Uani 1 1 d . . . O23A O 0.66159(19) 0.01242(8) 0.29148(17) 0.0241(5) Uani 1 1 d . . . C24A C 0.8624(4) 0.05977(16) 0.4119(3) 0.0451(10) Uani 1 1 d . . . H24A H 0.8039 0.0437 0.4345 0.068 Uiso 1 1 calc R . . H24B H 0.8712 0.0932 0.4357 0.068 Uiso 1 1 calc R . . H24C H 0.9421 0.0438 0.4460 0.068 Uiso 1 1 calc R . . C1B C 0.5686(3) 0.12631(11) 0.1393(3) 0.0231(7) Uani 1 1 d . . . O1B O 0.51470(18) 0.08456(7) 0.09117(16) 0.0205(5) Uani 1 1 d . . . C2B C 0.5891(3) 0.16379(11) 0.0784(3) 0.0241(7) Uani 1 1 d . . . C3B C 0.6438(3) 0.20582(12) 0.1340(3) 0.0296(8) Uani 1 1 d . . . H3B H 0.6564 0.2316 0.0936 0.036 Uiso 1 1 calc R . . C4B C 0.6798(3) 0.21072(13) 0.2467(3) 0.0345(8) Uani 1 1 d . . . H4B H 0.7157 0.2396 0.2828 0.041 Uiso 1 1 calc R . . C5B C 0.6627(3) 0.17292(13) 0.3058(3) 0.0356(8) Uani 1 1 d . . . H5B H 0.6897 0.1755 0.3834 0.043 Uiso 1 1 calc R . . C6B C 0.6066(3) 0.13142(12) 0.2526(3) 0.0290(8) Uani 1 1 d . . . H6B H 0.5937 0.1060 0.2939 0.035 Uiso 1 1 calc R . . C21B C 0.5695(3) 0.15805(11) -0.0378(3) 0.0232(7) Uani 1 1 d . . . N22B N 0.4880(2) 0.12763(9) -0.0971(2) 0.0194(5) Uani 1 1 d . . . O23B O 0.48531(18) 0.11745(7) -0.20075(16) 0.0206(5) Uani 1 1 d . . . C24B C 0.6473(3) 0.18513(12) -0.0818(3) 0.0313(8) Uani 1 1 d . . . H24D H 0.6425 0.1700 -0.1497 0.047 Uiso 1 1 calc R . . H24E H 0.7324 0.1850 -0.0269 0.047 Uiso 1 1 calc R . . H24F H 0.6179 0.2181 -0.0974 0.047 Uiso 1 1 calc R . . O1C O 0.2130(2) 0.16637(8) -0.46972(17) 0.0258(5) Uani 1 1 d . . . C1C C 0.1130(3) 0.18472(12) -0.4628(3) 0.0246(7) Uani 1 1 d . . . C2C C 0.0621(3) 0.16497(12) -0.3935(3) 0.0269(7) Uani 1 1 d . . . C3C C -0.0412(3) 0.18642(13) -0.3892(3) 0.0347(8) Uani 1 1 d . . . H3C H -0.0770 0.1727 -0.3442 0.042 Uiso 1 1 calc R . . C4C C -0.0919(3) 0.22691(14) -0.4487(3) 0.0435(10) Uani 1 1 d . . . H4C H -0.1599 0.2419 -0.4426 0.052 Uiso 1 1 calc R . . C5C C -0.0424(3) 0.24572(14) -0.5181(3) 0.0400(9) Uani 1 1 d . . . H5C H -0.0778 0.2735 -0.5602 0.048 Uiso 1 1 calc R . . C6C C 0.0568(3) 0.22468(12) -0.5263(3) 0.0324(8) Uani 1 1 d . . . H6C H 0.0877 0.2374 -0.5759 0.039 Uiso 1 1 calc R . . C21C C 0.1142(3) 0.12251(11) -0.3254(2) 0.0226(7) Uani 1 1 d . . . N22C N 0.2311(2) 0.11701(9) -0.2847(2) 0.0212(6) Uani 1 1 d . . . O23C O 0.27472(18) 0.07628(7) -0.21945(16) 0.0197(4) Uani 1 1 d . . . C24C C 0.0333(3) 0.08693(13) -0.3045(3) 0.0319(8) Uani 1 1 d . . . H24G H 0.0603 0.0546 -0.3115 0.048 Uiso 1 1 calc R . . H24H H -0.0514 0.0914 -0.3584 0.048 Uiso 1 1 calc R . . H24I H 0.0379 0.0914 -0.2299 0.048 Uiso 1 1 calc R . . N1D N 0.3532(2) 0.21556(9) -0.2691(2) 0.0230(6) Uani 1 1 d . . . C2D C 0.3696(3) 0.25491(12) -0.3184(3) 0.0316(8) Uani 1 1 d . . . H2D H 0.3870 0.2514 -0.3814 0.038 Uiso 1 1 calc R . . C3D C 0.3621(3) 0.30039(13) -0.2813(3) 0.0367(9) Uani 1 1 d . . . H3D H 0.3716 0.3276 -0.3197 0.044 Uiso 1 1 calc R . . C4D C 0.3408(3) 0.30574(13) -0.1881(3) 0.0348(8) Uani 1 1 d . . . H4D H 0.3399 0.3365 -0.1586 0.042 Uiso 1 1 calc R . . C5D C 0.3209(3) 0.26561(12) -0.1387(3) 0.0311(8) Uani 1 1 d . . . H5D H 0.3035 0.2683 -0.0755 0.037 Uiso 1 1 calc R . . C6D C 0.3262(3) 0.22158(12) -0.1814(3) 0.0256(7) Uani 1 1 d . . . H6D H 0.3102 0.1941 -0.1476 0.031 Uiso 1 1 calc R . . N1E N 0.5933(2) 0.02125(10) -0.2417(2) 0.0254(6) Uani 1 1 d . . . C2E C 0.6743(4) 0.05131(16) -0.2499(4) 0.0544(12) Uani 1 1 d . . . H2E H 0.6561 0.0845 -0.2561 0.065 Uiso 1 1 calc R . . C3E C 0.7847(4) 0.03625(18) -0.2496(5) 0.0723(16) Uani 1 1 d . . . H3E H 0.8413 0.0589 -0.2545 0.087 Uiso 1 1 calc R . . C4E C 0.8111(4) -0.01119(17) -0.2423(4) 0.0518(11) Uani 1 1 d . . . H4E H 0.8856 -0.0223 -0.2430 0.062 Uiso 1 1 calc R . . C5E C 0.7278(3) -0.04244(15) -0.2338(3) 0.0403(9) Uani 1 1 d . . . H5E H 0.7434 -0.0758 -0.2288 0.048 Uiso 1 1 calc R . . C6E C 0.6213(3) -0.02495(12) -0.2326(3) 0.0309(8) Uani 1 1 d . . . H6E H 0.5650 -0.0469 -0.2249 0.037 Uiso 1 1 calc R . . O1F O 0.70841(19) -0.02643(7) 0.02536(18) 0.0214(5) Uani 0.85 1 d P . 1 C2F C 0.8295(3) -0.02310(12) 0.0372(3) 0.0295(7) Uani 0.85 1 d P A 1 H2F1 H 0.8835 -0.0175 0.1148 0.044 Uiso 0.85 1 calc PR A 1 H2F2 H 0.8369 0.0034 -0.0076 0.044 Uiso 0.85 1 calc PR A 1 H2F3 H 0.8529 -0.0530 0.0127 0.044 Uiso 0.85 1 calc PR A 1 N1F N 0.70841(19) -0.02643(7) 0.02536(18) 0.0214(5) Uani 0.15 1 d P . 2 N2F N 0.8295(3) -0.02310(12) 0.0372(3) 0.0295(7) Uani 0.15 1 d P B 2 N3F N 0.9159(17) -0.0239(8) 0.0464(17) 0.041(6) Uani 0.15 1 d P B 2 N1G N 0.2754(2) 0.13393(10) -0.0221(2) 0.0263(6) Uani 1 1 d . . . N2G N 0.1709(3) 0.14576(10) -0.0588(2) 0.0338(7) Uani 1 1 d . . . N3G N 0.0711(3) 0.15827(15) -0.0924(3) 0.0616(11) Uani 1 1 d . . . N1H N 0.4752(3) 0.17226(11) -0.4033(2) 0.0336(7) Uani 1 1 d . . . N2H N 0.5807(5) 0.16807(18) -0.3787(4) 0.0316(12) Uiso 0.65 1 d P . 1 N3H N 0.6851(6) 0.1650(2) -0.3525(6) 0.0681(18) Uiso 0.65 1 d P . 1 N2H' N 0.5581(11) 0.1568(4) -0.4202(10) 0.051(3) Uiso 0.35 1 d P . 2 N3H' N 0.6558(13) 0.1501(5) -0.4170(12) 0.074(4) Uiso 0.35 1 d P . 2 O1J O 0.37454(19) 0.07893(8) -0.38174(17) 0.0245(5) Uani 1 1 d . . . C2J C 0.3276(5) 0.05924(15) -0.4880(3) 0.0577(13) Uani 1 1 d . . . H2J1 H 0.3324 0.0829 -0.5402 0.086 Uiso 1 1 calc R . . H2J2 H 0.2420 0.0500 -0.5094 0.086 Uiso 1 1 calc R . . H2J3 H 0.3756 0.0310 -0.4886 0.086 Uiso 1 1 calc 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 0.0182(2) 0.0187(2) 0.0158(2) -0.00162(17) 0.00480(18) -0.00298(17) Fe2 0.0203(2) 0.0194(2) 0.0160(2) -0.00091(17) 0.00686(19) -0.00153(17) Fe3 0.0234(2) 0.0228(2) 0.0188(2) 0.00252(18) 0.0093(2) -0.00006(18) Fe4 0.0206(2) 0.0199(2) 0.0162(2) -0.00031(18) 0.00705(19) -0.00126(18) O123 0.0189(10) 0.0177(11) 0.0142(10) -0.0004(8) 0.0048(9) -0.0023(8) C1A 0.0205(16) 0.0195(16) 0.0270(18) -0.0025(13) 0.0078(14) -0.0003(12) O1A 0.0215(11) 0.0243(12) 0.0208(12) -0.0014(9) 0.0060(10) -0.0064(9) C2A 0.0227(16) 0.0220(17) 0.0252(18) -0.0049(13) 0.0067(14) -0.0024(13) C3A 0.0257(18) 0.036(2) 0.0278(19) -0.0044(15) 0.0055(15) -0.0039(15) C4A 0.0215(17) 0.040(2) 0.044(2) -0.0099(18) 0.0063(17) -0.0132(15) C5A 0.0264(18) 0.035(2) 0.047(2) -0.0033(17) 0.0157(18) -0.0113(15) C6A 0.0273(18) 0.0282(18) 0.032(2) 0.0010(15) 0.0131(16) -0.0013(14) C21A 0.0225(16) 0.0249(17) 0.0220(17) -0.0013(14) 0.0020(14) -0.0024(13) N22A 0.0220(13) 0.0205(14) 0.0199(14) 0.0008(11) 0.0065(11) -0.0003(11) O23A 0.0283(12) 0.0264(12) 0.0177(11) -0.0023(9) 0.0096(10) -0.0063(9) C24A 0.039(2) 0.065(3) 0.0203(19) -0.0041(18) 0.0018(17) -0.021(2) C1B 0.0247(16) 0.0202(16) 0.0218(17) -0.0032(13) 0.0070(14) -0.0001(13) O1B 0.0243(11) 0.0184(11) 0.0170(11) -0.0029(9) 0.0067(9) -0.0023(9) C2B 0.0241(16) 0.0228(17) 0.0218(17) -0.0048(13) 0.0057(14) -0.0006(13) C3B 0.0317(18) 0.0251(18) 0.0294(19) -0.0055(15) 0.0100(16) -0.0040(14) C4B 0.039(2) 0.0281(19) 0.032(2) -0.0149(16) 0.0106(17) -0.0061(16) C5B 0.044(2) 0.034(2) 0.0258(19) -0.0117(16) 0.0104(17) -0.0018(17) C6B 0.0308(18) 0.0309(19) 0.0229(18) -0.0038(14) 0.0087(15) -0.0005(15) C21B 0.0235(16) 0.0182(16) 0.0263(17) 0.0015(13) 0.0087(14) -0.0007(13) N22B 0.0241(13) 0.0170(13) 0.0169(13) 0.0008(10) 0.0083(11) 0.0007(11) O23B 0.0224(11) 0.0231(11) 0.0156(11) -0.0002(9) 0.0071(9) -0.0033(9) C24B 0.0333(19) 0.0290(19) 0.0308(19) -0.0014(15) 0.0125(16) -0.0102(15) O1C 0.0274(12) 0.0291(12) 0.0196(12) 0.0039(9) 0.0083(10) 0.0022(10) C1C 0.0228(16) 0.0258(17) 0.0196(17) -0.0004(13) 0.0030(14) -0.0003(13) C2C 0.0198(16) 0.0329(19) 0.0217(17) -0.0004(14) 0.0021(14) -0.0019(14) C3C 0.0247(18) 0.042(2) 0.036(2) 0.0069(17) 0.0112(16) 0.0043(15) C4C 0.029(2) 0.048(2) 0.053(3) 0.015(2) 0.0163(19) 0.0148(17) C5C 0.0297(19) 0.038(2) 0.043(2) 0.0128(18) 0.0048(18) 0.0077(16) C6C 0.0312(19) 0.033(2) 0.0279(19) 0.0056(15) 0.0068(16) 0.0016(15) C21C 0.0229(16) 0.0283(18) 0.0157(16) 0.0001(13) 0.0072(13) -0.0015(13) N22C 0.0225(13) 0.0223(14) 0.0169(13) 0.0027(11) 0.0060(11) 0.0007(11) O23C 0.0211(11) 0.0194(11) 0.0169(11) 0.0024(9) 0.0061(9) -0.0002(8) C24C 0.0224(17) 0.043(2) 0.0253(19) 0.0073(16) 0.0047(15) -0.0045(15) N1D 0.0249(14) 0.0230(14) 0.0192(14) 0.0024(11) 0.0071(12) -0.0021(11) C2D 0.0351(19) 0.032(2) 0.0270(19) 0.0022(15) 0.0116(16) -0.0028(15) C3D 0.041(2) 0.027(2) 0.041(2) 0.0074(16) 0.0145(18) -0.0059(16) C4D 0.0336(19) 0.0264(19) 0.041(2) -0.0040(16) 0.0117(17) 0.0040(15) C5D 0.0319(19) 0.0327(19) 0.0292(19) -0.0009(15) 0.0132(16) 0.0055(15) C6D 0.0250(17) 0.0262(18) 0.0245(18) 0.0028(14) 0.0092(14) 0.0005(13) N1E 0.0255(14) 0.0288(16) 0.0225(15) 0.0008(11) 0.0106(12) 0.0018(11) C2E 0.045(2) 0.042(2) 0.092(4) 0.012(2) 0.044(3) 0.0004(19) C3E 0.051(3) 0.065(3) 0.129(5) 0.009(3) 0.066(3) -0.006(2) C4E 0.035(2) 0.071(3) 0.058(3) -0.010(2) 0.028(2) 0.005(2) C5E 0.034(2) 0.047(2) 0.035(2) -0.0125(18) 0.0092(18) 0.0099(18) C6E 0.0301(18) 0.031(2) 0.0307(19) -0.0071(15) 0.0115(16) -0.0028(15) O1F 0.0205(11) 0.0222(12) 0.0211(12) -0.0005(9) 0.0083(10) -0.0024(9) C2F 0.0287(19) 0.0297(19) 0.032(2) -0.0010(15) 0.0147(16) -0.0017(14) N1F 0.0205(11) 0.0222(12) 0.0211(12) -0.0005(9) 0.0083(10) -0.0024(9) N2F 0.0287(19) 0.0297(19) 0.032(2) -0.0010(15) 0.0147(16) -0.0017(14) N3F 0.009(9) 0.079(17) 0.038(12) -0.002(11) 0.011(9) 0.003(9) N1G 0.0295(15) 0.0237(15) 0.0262(15) -0.0040(12) 0.0120(13) 0.0018(12) N2G 0.0389(19) 0.0326(17) 0.0306(17) -0.0046(13) 0.0150(15) 0.0035(14) N3G 0.043(2) 0.079(3) 0.056(2) -0.008(2) 0.0135(19) 0.022(2) N1H 0.0351(17) 0.0371(17) 0.0361(18) 0.0091(14) 0.0224(15) 0.0008(13) O1J 0.0299(12) 0.0262(12) 0.0168(11) 0.0003(9) 0.0090(10) 0.0024(9) C2J 0.094(4) 0.037(2) 0.021(2) -0.0045(17) 0.004(2) 0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1A 1.879(2) . ? Fe1 O123 1.999(2) . ? Fe1 O1F 2.018(2) . ? Fe1 O123 2.0577(19) 3_655 ? Fe1 N22A 2.115(3) . ? Fe1 O1B 2.168(2) . ? Fe2 N1G 1.953(3) . ? Fe2 N1F 1.970(2) 3_655 ? Fe2 O1F 1.970(2) 3_655 ? Fe2 O1B 1.981(2) . ? Fe2 O23C 2.050(2) . ? Fe2 O123 2.104(2) . ? Fe2 N22B 2.132(2) . ? Fe3 O1C 1.900(2) . ? Fe3 N1H 1.984(3) . ? Fe3 O1J 2.000(2) . ? Fe3 O23B 2.094(2) . ? Fe3 N22C 2.174(2) . ? Fe3 N1D 2.186(3) . ? Fe4 O23A 1.906(2) 3_655 ? Fe4 O123 1.948(2) . ? Fe4 O1J 1.971(2) . ? Fe4 O23C 2.121(2) . ? Fe4 O23B 2.123(2) . ? Fe4 N1E 2.131(3) . ? O123 Fe1 2.0578(19) 3_655 ? C1A O1A 1.329(4) . ? C1A C6A 1.398(4) . ? C1A C2A 1.419(4) . ? C2A C3A 1.406(4) . ? C2A C21A 1.467(4) . ? C3A C4A 1.374(5) . ? C3A H3A 0.9500 . ? C4A C5A 1.379(5) . ? C4A H4A 0.9500 . ? C5A C6A 1.390(5) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C21A N22A 1.308(4) . ? C21A C24A 1.505(5) . ? N22A O23A 1.380(3) . ? O23A Fe4 1.906(2) 3_655 ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C1B O1B 1.362(4) . ? C1B C6B 1.392(4) . ? C1B C2B 1.409(4) . ? C2B C3B 1.401(4) . ? C2B C21B 1.476(4) . ? C3B C4B 1.386(5) . ? C3B H3B 0.9500 . ? C4B C5B 1.384(5) . ? C4B H4B 0.9500 . ? C5B C6B 1.383(5) . ? C5B H5B 0.9500 . ? C6B H6B 0.9500 . ? C21B N22B 1.291(4) . ? C21B C24B 1.497(4) . ? N22B O23B 1.398(3) . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? O1C C1C 1.343(4) . ? C1C C6C 1.397(5) . ? C1C C2C 1.412(4) . ? C2C C3C 1.400(5) . ? C2C C21C 1.470(4) . ? C3C C4C 1.373(5) . ? C3C H3C 0.9500 . ? C4C C5C 1.391(5) . ? C4C H4C 0.9500 . ? C5C C6C 1.372(5) . ? C5C H5C 0.9500 . ? C6C H6C 0.9500 . ? C21C N22C 1.286(4) . ? C21C C24C 1.495(4) . ? N22C O23C 1.398(3) . ? C24C H24G 0.9800 . ? C24C H24H 0.9800 . ? C24C H24I 0.9800 . ? N1D C2D 1.338(4) . ? N1D C6D 1.345(4) . ? C2D C3D 1.382(5) . ? C2D H2D 0.9500 . ? C3D C4D 1.375(5) . ? C3D H3D 0.9500 . ? C4D C5D 1.372(5) . ? C4D H4D 0.9500 . ? C5D C6D 1.371(5) . ? C5D H5D 0.9500 . ? C6D H6D 0.9500 . ? N1E C2E 1.323(4) . ? N1E C6E 1.329(4) . ? C2E C3E 1.389(6) . ? C2E H2E 0.9500 . ? C3E C4E 1.360(6) . ? C3E H3E 0.9500 . ? C4E C5E 1.367(6) . ? C4E H4E 0.9500 . ? C5E C6E 1.374(5) . ? C5E H5E 0.9500 . ? C6E H6E 0.9500 . ? O1F C2F 1.398(4) . ? O1F Fe2 1.971(2) 3_655 ? C2F H2F1 0.9800 . ? C2F H2F2 0.9800 . ? C2F H2F3 0.9800 . ? N1G N2G 1.189(4) . ? N2G N3G 1.146(4) . ? N1H N2H 1.174(6) . ? N1H N2H' 1.188(12) . ? N2H N3H 1.157(7) . ? N2H' N3H' 1.170(15) . ? O1J C2J 1.402(4) . ? C2J H2J1 0.9800 . ? C2J H2J2 0.9800 . ? C2J H2J3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Fe1 O123 107.78(9) . . ? O1A Fe1 O1F 90.84(9) . . ? O123 Fe1 O1F 98.27(8) . . ? O1A Fe1 O123 167.17(9) . 3_655 ? O123 Fe1 O123 81.55(8) . 3_655 ? O1F Fe1 O123 78.89(8) . 3_655 ? O1A Fe1 N22A 86.76(9) . . ? O123 Fe1 N22A 156.75(9) . . ? O1F Fe1 N22A 99.57(9) . . ? O123 Fe1 N22A 87.39(9) 3_655 . ? O1A Fe1 O1B 92.28(9) . . ? O123 Fe1 O1B 79.98(8) . . ? O1F Fe1 O1B 176.77(8) . . ? O123 Fe1 O1B 98.12(8) 3_655 . ? N22A Fe1 O1B 81.44(9) . . ? N1G Fe2 N1F 100.58(10) . 3_655 ? N1G Fe2 O1F 100.58(10) . 3_655 ? N1F Fe2 O1F 0.00(14) 3_655 3_655 ? N1G Fe2 O1B 98.27(10) . . ? N1F Fe2 O1B 97.23(9) 3_655 . ? O1F Fe2 O1B 97.23(9) 3_655 . ? N1G Fe2 O23C 100.71(10) . . ? N1F Fe2 O23C 91.12(8) 3_655 . ? O1F Fe2 O23C 91.12(8) 3_655 . ? O1B Fe2 O23C 157.47(8) . . ? N1G Fe2 O123 179.40(10) . . ? N1F Fe2 O123 78.84(8) 3_655 . ? O1F Fe2 O123 78.84(8) 3_655 . ? O1B Fe2 O123 81.98(8) . . ? O23C Fe2 O123 79.17(8) . . ? N1G Fe2 N22B 98.80(10) . . ? N1F Fe2 N22B 160.56(9) 3_655 . ? O1F Fe2 N22B 160.56(9) 3_655 . ? O1B Fe2 N22B 81.25(9) . . ? O23C Fe2 N22B 83.95(9) . . ? O123 Fe2 N22B 81.77(8) . . ? O1C Fe3 N1H 96.50(11) . . ? O1C Fe3 O1J 102.47(9) . . ? N1H Fe3 O1J 95.23(11) . . ? O1C Fe3 O23B 166.00(9) . . ? N1H Fe3 O23B 97.34(10) . . ? O1J Fe3 O23B 74.14(8) . . ? O1C Fe3 N22C 84.83(9) . . ? N1H Fe3 N22C 177.66(11) . . ? O1J Fe3 N22C 82.59(9) . . ? O23B Fe3 N22C 81.27(8) . . ? O1C Fe3 N1D 88.40(10) . . ? N1H Fe3 N1D 91.67(11) . . ? O1J Fe3 N1D 166.34(9) . . ? O23B Fe3 N1D 93.32(9) . . ? N22C Fe3 N1D 90.29(9) . . ? O23A Fe4 O123 93.10(8) 3_655 . ? O23A Fe4 O1J 98.36(9) 3_655 . ? O123 Fe4 O1J 165.03(9) . . ? O23A Fe4 O23C 91.06(9) 3_655 . ? O123 Fe4 O23C 81.05(8) . . ? O1J Fe4 O23C 89.09(8) . . ? O23A Fe4 O23B 167.26(9) 3_655 . ? O123 Fe4 O23B 92.85(8) . . ? O1J Fe4 O23B 74.09(8) . . ? O23C Fe4 O23B 78.76(8) . . ? O23A Fe4 N1E 95.83(10) 3_655 . ? O123 Fe4 N1E 94.95(9) . . ? O1J Fe4 N1E 93.45(9) . . ? O23C Fe4 N1E 172.23(9) . . ? O23B Fe4 N1E 94.87(9) . . ? Fe4 O123 Fe1 139.40(11) . . ? Fe4 O123 Fe1 115.70(9) . 3_655 ? Fe1 O123 Fe1 98.45(8) . 3_655 ? Fe4 O123 Fe2 96.52(8) . . ? Fe1 O123 Fe2 99.80(8) . . ? Fe1 O123 Fe2 98.15(8) 3_655 . ? O1A C1A C6A 117.7(3) . . ? O1A C1A C2A 123.3(3) . . ? C6A C1A C2A 118.9(3) . . ? C1A O1A Fe1 134.2(2) . . ? C3A C2A C1A 117.7(3) . . ? C3A C2A C21A 118.3(3) . . ? C1A C2A C21A 123.9(3) . . ? C4A C3A C2A 122.2(3) . . ? C4A C3A H3A 118.9 . . ? C2A C3A H3A 118.9 . . ? C3A C4A C5A 120.0(3) . . ? C3A C4A H4A 120.0 . . ? C5A C4A H4A 120.0 . . ? C4A C5A C6A 119.4(3) . . ? C4A C5A H5A 120.3 . . ? C6A C5A H5A 120.3 . . ? C5A C6A C1A 121.6(3) . . ? C5A C6A H6A 119.2 . . ? C1A C6A H6A 119.2 . . ? N22A C21A C2A 121.0(3) . . ? N22A C21A C24A 119.8(3) . . ? C2A C21A C24A 119.2(3) . . ? C21A N22A O23A 114.8(3) . . ? C21A N22A Fe1 129.5(2) . . ? O23A N22A Fe1 114.83(17) . . ? N22A O23A Fe4 118.04(17) . 3_655 ? C21A C24A H24A 109.5 . . ? C21A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C21A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? O1B C1B C6B 118.5(3) . . ? O1B C1B C2B 122.1(3) . . ? C6B C1B C2B 119.4(3) . . ? C1B O1B Fe2 121.33(19) . . ? C1B O1B Fe1 121.13(18) . . ? Fe2 O1B Fe1 98.25(8) . . ? C3B C2B C1B 118.4(3) . . ? C3B C2B C21B 118.9(3) . . ? C1B C2B C21B 122.2(3) . . ? C4B C3B C2B 121.6(3) . . ? C4B C3B H3B 119.2 . . ? C2B C3B H3B 119.2 . . ? C5B C4B C3B 119.1(3) . . ? C5B C4B H4B 120.4 . . ? C3B C4B H4B 120.4 . . ? C6B C5B C4B 120.4(3) . . ? C6B C5B H5B 119.8 . . ? C4B C5B H5B 119.8 . . ? C5B C6B C1B 120.9(3) . . ? C5B C6B H6B 119.5 . . ? C1B C6B H6B 119.5 . . ? N22B C21B C2B 117.8(3) . . ? N22B C21B C24B 122.2(3) . . ? C2B C21B C24B 120.0(3) . . ? C21B N22B O23B 116.2(2) . . ? C21B N22B Fe2 129.1(2) . . ? O23B N22B Fe2 114.21(16) . . ? N22B O23B Fe3 123.15(16) . . ? N22B O23B Fe4 107.52(15) . . ? Fe3 O23B Fe4 96.24(8) . . ? C21B C24B H24D 109.5 . . ? C21B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C21B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C1C O1C Fe3 124.71(19) . . ? O1C C1C C6C 119.1(3) . . ? O1C C1C C2C 122.3(3) . . ? C6C C1C C2C 118.6(3) . . ? C3C C2C C1C 119.2(3) . . ? C3C C2C C21C 118.7(3) . . ? C1C C2C C21C 122.2(3) . . ? C4C C3C C2C 121.3(3) . . ? C4C C3C H3C 119.4 . . ? C2C C3C H3C 119.4 . . ? C3C C4C C5C 119.2(3) . . ? C3C C4C H4C 120.4 . . ? C5C C4C H4C 120.4 . . ? C6C C5C C4C 120.8(3) . . ? C6C C5C H5C 119.6 . . ? C4C C5C H5C 119.6 . . ? C5C C6C C1C 120.8(3) . . ? C5C C6C H6C 119.6 . . ? C1C C6C H6C 119.6 . . ? N22C C21C C2C 117.9(3) . . ? N22C C21C C24C 121.3(3) . . ? C2C C21C C24C 120.7(3) . . ? C21C N22C O23C 115.0(2) . . ? C21C N22C Fe3 126.9(2) . . ? O23C N22C Fe3 114.51(16) . . ? N22C O23C Fe2 119.30(16) . . ? N22C O23C Fe4 111.85(15) . . ? Fe2 O23C Fe4 93.00(8) . . ? C21C C24C H24G 109.5 . . ? C21C C24C H24H 109.5 . . ? H24G C24C H24H 109.5 . . ? C21C C24C H24I 109.5 . . ? H24G C24C H24I 109.5 . . ? H24H C24C H24I 109.5 . . ? C2D N1D C6D 117.4(3) . . ? C2D N1D Fe3 116.8(2) . . ? C6D N1D Fe3 125.6(2) . . ? N1D C2D C3D 122.7(3) . . ? N1D C2D H2D 118.7 . . ? C3D C2D H2D 118.7 . . ? C4D C3D C2D 119.1(3) . . ? C4D C3D H3D 120.5 . . ? C2D C3D H3D 120.5 . . ? C5D C4D C3D 118.6(3) . . ? C5D C4D H4D 120.7 . . ? C3D C4D H4D 120.7 . . ? C6D C5D C4D 119.4(3) . . ? C6D C5D H5D 120.3 . . ? C4D C5D H5D 120.3 . . ? N1D C6D C5D 122.8(3) . . ? N1D C6D H6D 118.6 . . ? C5D C6D H6D 118.6 . . ? C2E N1E C6E 117.4(3) . . ? C2E N1E Fe4 121.6(2) . . ? C6E N1E Fe4 121.0(2) . . ? N1E C2E C3E 122.5(4) . . ? N1E C2E H2E 118.7 . . ? C3E C2E H2E 118.7 . . ? C4E C3E C2E 119.4(4) . . ? C4E C3E H3E 120.3 . . ? C2E C3E H3E 120.3 . . ? C3E C4E C5E 118.4(4) . . ? C3E C4E H4E 120.8 . . ? C5E C4E H4E 120.8 . . ? C4E C5E C6E 119.2(4) . . ? C4E C5E H5E 120.4 . . ? C6E C5E H5E 120.4 . . ? N1E C6E C5E 123.1(3) . . ? N1E C6E H6E 118.4 . . ? C5E C6E H6E 118.4 . . ? C2F O1F Fe2 126.01(19) . 3_655 ? C2F O1F Fe1 122.92(19) . . ? Fe2 O1F Fe1 104.10(9) 3_655 . ? N2G N1G Fe2 136.1(2) . . ? N3G N2G N1G 178.1(4) . . ? N2H N1H N2H' 29.2(6) . . ? N2H N1H Fe3 135.5(3) . . ? N2H' N1H Fe3 136.6(6) . . ? N3H N2H N1H 178.1(8) . . ? N3H' N2H' N1H 162.9(15) . . ? C2J O1J Fe4 128.5(2) . . ? C2J O1J Fe3 124.9(2) . . ? Fe4 O1J Fe3 104.54(9) . . ? O1J C2J H2J1 109.5 . . ? O1J C2J H2J2 109.5 . . ? H2J1 C2J H2J2 109.5 . . ? O1J C2J H2J3 109.5 . . ? H2J1 C2J H2J3 109.5 . . ? H2J2 C2J H2J3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.647 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.083 # Attachment '- pt9053-(4).cif' data_pt9053 _database_code_depnum_ccdc_archive 'CCDC 794873' #TrackingRef '- pt9053-(4).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Brian Tung' _exptl_crystal_recrystallization_method 'Et2O diffusion of into MeOH/pyr solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H56 Cl2 Fe6 N8 O26, 2(C4 H10 O), C H4 O' _chemical_formula_sum 'C69 H80 Cl2 Fe6 N8 O29' _chemical_formula_weight 1891.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.5512(19) _cell_length_b 29.198(4) _cell_length_c 21.050(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.368(6) _cell_angle_gamma 90.00 _cell_volume 8165(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.02 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3888 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4634 _exptl_absorpt_correction_T_max 0.9114 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 40827 _diffrn_reflns_av_R_equivalents 0.0830 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.49 _reflns_number_total 15647 _reflns_number_gt 9754 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93 022_ALERT_3_C Ratio Unique / Expected Reflections too Low .... 0.93 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 611 341_ALERT_3_C Low Bond Precision on C-C Bonds (x 1000) Ang ... 10 234_ALERT_4_C Large Hirshfeld Difference N41F -- C4F .. 0.17 Ang. 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 322 951_ALERT_1_C Reported and Calculated Kmax Values Differ by .. 4 There is a completeness problem with this sample. Recollection was not possible immediately after data collection due to sample going off. This has likely affected precision as well as some other parameters. #============================================================================== Resolution & Completeness Statistics (Cumulative and Friedel Pairs Averaged) #============================================================================== Theta sin(th)/Lambda Complete Expected Measured Missing #------------------------------------------------------------------------------ 20.82 0.500 0.997 8546 8523 23 23.01 0.550 0.984 11371 11192 179 25.24 0.600 0.958 14670 14059 611 #----------------------------------------------------------- ACTA Min. Res. --- 26.49 0.628 0.944 16580 15647 933 201_ALERT_2_B Isotropic non-H Atoms in Main Residue(s) ....... 2 301_ALERT_3_G Note Main Residue Disorder .................... 2.00 Perc. 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 35.90 Deg. O42' -N41F -O42F 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 21.00 Deg. O43F -N41F -O43' 1.555 1.555 1.555 These atoms were part of a disordered group. They have been left isotropic due to poor ellipsoid shapes. 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 3.83 Ratio 220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.04 Ratio These atoms are in a position where high thermal motion is expected. They have been modelled using enlarged ADP's rather than with multiple components as this is more reflective of their motion. 410_ALERT_2_C Short Intra H...H Contact H3BA .. H24D .. 1.97 Ang. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 14 Confirmed 061_ALERT_4_B Tmax/Tmin Range Test RR' too Large ............. 0.65 This was a plate. Absorption problems are not unexpected. 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbours of O1T 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C4 H10 O 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 4 C H4 O 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 69 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? No action taken ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15647 _refine_ls_number_parameters 1026 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1177 _refine_ls_R_factor_gt 0.0701 _refine_ls_wR_factor_ref 0.2073 _refine_ls_wR_factor_gt 0.1772 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.33088(6) 0.66192(3) 0.46020(4) 0.0231(2) Uani 1 1 d . . . Fe2 Fe 0.06493(6) 0.71989(3) 0.48308(4) 0.0244(2) Uani 1 1 d . . . Fe3 Fe 0.09665(6) 0.61621(3) 0.46788(4) 0.0236(2) Uani 1 1 d . . . Fe4 Fe 0.13979(6) 0.66653(3) 0.35438(4) 0.0241(2) Uani 1 1 d . . . Fe5 Fe 0.27348(6) 0.55910(3) 0.45190(4) 0.0257(2) Uani 1 1 d . . . Fe6 Fe -0.07102(6) 0.70025(3) 0.34860(4) 0.0282(2) Uani 1 1 d . . . O134 O 0.2105(3) 0.62019(13) 0.41946(17) 0.0227(9) Uani 1 1 d . . . O234 O 0.0401(3) 0.66887(13) 0.41249(18) 0.0235(9) Uani 1 1 d . . . Cl1 Cl 0.34339(11) 0.49327(5) 0.50071(8) 0.0331(4) Uani 1 1 d . . . Cl2 Cl -0.18747(11) 0.74022(6) 0.27721(8) 0.0417(4) Uani 1 1 d . . . O1A O 0.4348(3) 0.69990(14) 0.50406(18) 0.0275(9) Uani 1 1 d . . . C1A C 0.4674(4) 0.7081(2) 0.5672(3) 0.0286(14) Uani 1 1 d . . . C2A C 0.4080(4) 0.7010(2) 0.6148(3) 0.0265(13) Uani 1 1 d . . . C3A C 0.4550(5) 0.7068(2) 0.6801(3) 0.0341(15) Uani 1 1 d . . . H3AA H 0.4177 0.7010 0.7130 0.041 Uiso 1 1 calc R . . C4A C 0.5539(5) 0.7209(2) 0.6976(3) 0.0397(17) Uani 1 1 d . . . H4AA H 0.5848 0.7236 0.7420 0.048 Uiso 1 1 calc R . . C5A C 0.6081(5) 0.7312(3) 0.6498(3) 0.0442(19) Uani 1 1 d . . . H5AA H 0.6750 0.7424 0.6619 0.053 Uiso 1 1 calc R . . C6A C 0.5662(4) 0.7254(2) 0.5854(3) 0.0354(16) Uani 1 1 d . . . H6AA H 0.6035 0.7331 0.5532 0.042 Uiso 1 1 calc R . . C21A C 0.3005(4) 0.6892(2) 0.5985(3) 0.0244(13) Uani 1 1 d . . . N22A N 0.2624(3) 0.67467(16) 0.5409(2) 0.0233(11) Uani 1 1 d . . . O23A O 0.1577(3) 0.66802(13) 0.52893(18) 0.0235(9) Uani 1 1 d . . . C24A C 0.2343(4) 0.6956(2) 0.6473(3) 0.0313(15) Uani 1 1 d . . . H24A H 0.1709 0.7105 0.6259 0.038 Uiso 1 1 calc R . . H24B H 0.2685 0.7163 0.6820 0.038 Uiso 1 1 calc R . . C25A C 0.2092(6) 0.6507(3) 0.6779(3) 0.052(2) Uani 1 1 d . . . H25A H 0.1665 0.6571 0.7094 0.078 Uiso 1 1 calc R . . H25B H 0.2715 0.6359 0.6999 0.078 Uiso 1 1 calc R . . H25C H 0.1734 0.6304 0.6441 0.078 Uiso 1 1 calc R . . O1B O 0.0954(3) 0.76912(14) 0.54114(19) 0.0296(10) Uani 1 1 d . . . C1B C 0.1390(4) 0.8101(2) 0.5364(3) 0.0292(14) Uani 1 1 d . . . C2B C 0.2046(4) 0.8182(2) 0.4939(3) 0.0279(14) Uani 1 1 d . . . C3B C 0.2432(5) 0.8630(2) 0.4907(3) 0.0333(15) Uani 1 1 d . . . H3BA H 0.2850 0.8694 0.4605 0.040 Uiso 1 1 calc R . . C4B C 0.2213(5) 0.8979(2) 0.5310(3) 0.0392(17) Uani 1 1 d . . . H4BA H 0.2476 0.9278 0.5281 0.047 Uiso 1 1 calc R . . C5B C 0.1610(5) 0.8883(2) 0.5750(4) 0.0413(18) Uani 1 1 d . . . H5BA H 0.1476 0.9117 0.6035 0.050 Uiso 1 1 calc R . . C6B C 0.1196(5) 0.8450(2) 0.5781(3) 0.0354(16) Uani 1 1 d . . . H6BA H 0.0779 0.8390 0.6086 0.043 Uiso 1 1 calc R . . C21B C 0.2379(4) 0.7828(2) 0.4533(3) 0.0260(13) Uani 1 1 d . . . N22B N 0.1904(3) 0.74341(17) 0.4472(2) 0.0245(11) Uani 1 1 d . . . O23B O 0.2331(3) 0.71094(13) 0.41124(17) 0.0240(9) Uani 1 1 d . . . C24B C 0.3251(4) 0.7907(2) 0.4201(3) 0.0327(15) Uani 1 1 d . . . H24C H 0.3689 0.7633 0.4256 0.039 Uiso 1 1 calc R . . H24D H 0.3654 0.8169 0.4408 0.039 Uiso 1 1 calc R . . C25B C 0.2901(5) 0.8005(3) 0.3479(3) 0.0454(18) Uani 1 1 d . . . H25D H 0.3488 0.8057 0.3281 0.068 Uiso 1 1 calc R . . H25E H 0.2473 0.8278 0.3423 0.068 Uiso 1 1 calc R . . H25F H 0.2518 0.7742 0.3270 0.068 Uiso 1 1 calc R . . C1C C 0.3977(4) 0.6681(2) 0.2644(3) 0.0276(14) Uani 1 1 d . . . C2C C 0.3443(5) 0.6726(2) 0.2008(3) 0.0347(15) Uani 1 1 d . . . H2CA H 0.2733 0.6764 0.1925 0.042 Uiso 1 1 calc R . . C3C C 0.3959(5) 0.6715(2) 0.1497(3) 0.0348(16) Uani 1 1 d . . . H3CA H 0.3610 0.6748 0.1062 0.042 Uiso 1 1 calc R . . C4C C 0.4977(5) 0.6654(2) 0.1636(3) 0.0357(16) Uani 1 1 d . . . C5C C 0.5534(5) 0.6627(3) 0.2267(3) 0.0422(18) Uani 1 1 d . . . H5CA H 0.6248 0.6604 0.2347 0.051 Uiso 1 1 calc R . . C6C C 0.5023(5) 0.6634(2) 0.2772(3) 0.0369(16) Uani 1 1 d . . . H6CA H 0.5381 0.6607 0.3206 0.044 Uiso 1 1 calc R . . C11C C 0.3408(4) 0.6660(2) 0.3184(3) 0.0295(14) Uani 1 1 d . . . O12C O 0.3880(3) 0.66279(14) 0.37607(18) 0.0270(9) Uani 1 1 d . . . O13C O 0.2453(3) 0.66776(14) 0.30109(18) 0.0291(10) Uani 1 1 d . . . N41C N 0.5504(4) 0.6626(2) 0.1091(3) 0.0452(15) Uani 1 1 d . . . O42C O 0.6424(4) 0.6560(2) 0.1211(3) 0.0599(16) Uani 1 1 d . . . O43C O 0.5018(4) 0.6663(2) 0.0537(2) 0.0575(15) Uani 1 1 d . . . C1D C -0.1210(4) 0.6385(2) 0.5883(3) 0.0285(14) Uani 1 1 d . . . C2D C -0.1784(5) 0.5986(2) 0.5792(3) 0.0325(15) Uani 1 1 d . . . H2DA H -0.1705 0.5773 0.5463 0.039 Uiso 1 1 calc R . . C3D C -0.2470(5) 0.5902(2) 0.6185(3) 0.0397(17) Uani 1 1 d . . . H3DA H -0.2913 0.5647 0.6099 0.048 Uiso 1 1 calc R . . C4D C -0.2512(5) 0.6180(2) 0.6689(3) 0.0416(17) Uani 1 1 d . . . C5D C -0.1931(5) 0.6582(2) 0.6805(3) 0.0392(17) Uani 1 1 d . . . H5DA H -0.1971 0.6777 0.7160 0.047 Uiso 1 1 calc R . . C6D C -0.1302(5) 0.6681(2) 0.6384(3) 0.0359(16) Uani 1 1 d . . . H6DA H -0.0924 0.6957 0.6437 0.043 Uiso 1 1 calc R . . C11D C -0.0504(4) 0.6488(2) 0.5442(3) 0.0245(13) Uani 1 1 d . . . O12D O -0.0137(3) 0.61505(13) 0.51873(18) 0.0249(9) Uani 1 1 d . . . O13D O -0.0312(3) 0.69072(14) 0.53526(18) 0.0274(9) Uani 1 1 d . . . N41D N -0.3234(5) 0.6083(2) 0.7110(3) 0.0557(17) Uani 1 1 d . . . O42D O -0.3161(5) 0.6309(2) 0.7615(3) 0.0694(17) Uani 1 1 d . . . O43D O -0.3871(5) 0.5789(3) 0.6940(3) 0.088(2) Uani 1 1 d . . . C1E C -0.0635(4) 0.5935(2) 0.2064(3) 0.0282(14) Uani 1 1 d . . . C2E C -0.0007(5) 0.5644(2) 0.1807(3) 0.0383(16) Uani 1 1 d . . . H2EA H 0.0676 0.5612 0.2020 0.046 Uiso 1 1 calc R . . C3E C -0.0362(5) 0.5397(3) 0.1243(3) 0.0452(18) Uani 1 1 d . . . H3EA H 0.0066 0.5200 0.1062 0.054 Uiso 1 1 calc R . . C4E C -0.1365(5) 0.5453(3) 0.0958(3) 0.0436(18) Uani 1 1 d . . . C5E C -0.1998(5) 0.5732(3) 0.1195(3) 0.0457(19) Uani 1 1 d . . . H5EA H -0.2682 0.5759 0.0982 0.055 Uiso 1 1 calc R . . C6E C -0.1636(5) 0.5979(2) 0.1755(3) 0.0393(17) Uani 1 1 d . . . H6EA H -0.2071 0.6178 0.1927 0.047 Uiso 1 1 calc R . . C11E C -0.0261(4) 0.6204(2) 0.2662(3) 0.0275(14) Uani 1 1 d . . . O12E O -0.0899(3) 0.64288(15) 0.29006(19) 0.0304(10) Uani 1 1 d . . . O13E O 0.0685(3) 0.61932(14) 0.28988(18) 0.0288(10) Uani 1 1 d . . . N41E N -0.1745(6) 0.5201(3) 0.0353(3) 0.064(2) Uani 1 1 d . . . O42E O -0.2637(4) 0.5238(2) 0.0096(3) 0.084(2) Uani 1 1 d . . . O43E O -0.1131(5) 0.4978(3) 0.0105(3) 0.084(2) Uani 1 1 d . . . C1F C 0.0012(5) 0.5071(2) 0.3283(3) 0.0330(15) Uani 1 1 d . . . C2F C -0.1004(5) 0.5137(2) 0.3085(3) 0.0407(17) Uani 1 1 d . . . H2FA H -0.1341 0.5360 0.3293 0.049 Uiso 1 1 calc R . . C3F C -0.1551(5) 0.4873(3) 0.2570(3) 0.048(2) Uani 1 1 d . . . H3FA H -0.2254 0.4916 0.2425 0.058 Uiso 1 1 calc R . . C4F C -0.1034(6) 0.4550(3) 0.2284(3) 0.051(2) Uani 1 1 d . A . C5F C -0.0023(6) 0.4470(3) 0.2480(3) 0.054(2) Uani 1 1 d . . . H5FA H 0.0309 0.4241 0.2280 0.065 Uiso 1 1 calc R . . C6F C 0.0498(5) 0.4737(2) 0.2983(3) 0.0432(18) Uani 1 1 d . . . H6FA H 0.1201 0.4690 0.3125 0.052 Uiso 1 1 calc R . . C11F C 0.0632(4) 0.5357(2) 0.3806(3) 0.0278(14) Uani 1 1 d . . . O12F O 0.1558(3) 0.52620(14) 0.3944(2) 0.0321(10) Uani 1 1 d . . . O13F O 0.0204(3) 0.56711(14) 0.40673(19) 0.0296(10) Uani 1 1 d . . . N41F N -0.1584(6) 0.4274(3) 0.1727(4) 0.072(2) Uani 1 1 d . . . O42F O -0.2350(6) 0.4465(4) 0.1389(6) 0.048(4) Uiso 0.64(3) 1 d P A 1 O43F O -0.1322(13) 0.3920(5) 0.1650(7) 0.076(4) Uiso 0.64(3) 1 d P A 1 O42' O -0.2407(18) 0.4290(11) 0.1637(15) 0.086(9) Uiso 0.36(3) 1 d P A 2 O43' O -0.1003(18) 0.3922(7) 0.1532(10) 0.055(6) Uiso 0.36(3) 1 d P A 2 N1G N 0.3442(4) 0.55043(17) 0.3696(2) 0.0303(12) Uani 1 1 d . . . C2G C 0.2961(5) 0.5567(2) 0.3079(3) 0.0380(16) Uani 1 1 d . . . H2GA H 0.2275 0.5658 0.3000 0.046 Uiso 1 1 calc R . . C3G C 0.3419(5) 0.5505(3) 0.2562(3) 0.0479(19) Uani 1 1 d . . . H3GA H 0.3052 0.5554 0.2134 0.057 Uiso 1 1 calc R . . C4G C 0.4412(6) 0.5373(3) 0.2663(4) 0.051(2) Uani 1 1 d . . . H4GA H 0.4742 0.5329 0.2309 0.062 Uiso 1 1 calc R . . C5G C 0.4909(5) 0.5306(3) 0.3288(4) 0.0482(19) Uani 1 1 d . . . H5GA H 0.5594 0.5212 0.3374 0.058 Uiso 1 1 calc R . . C6G C 0.4412(5) 0.5376(2) 0.3791(3) 0.0368(16) Uani 1 1 d . . . H6GA H 0.4770 0.5331 0.4222 0.044 Uiso 1 1 calc R . . N1H N -0.1861(3) 0.67071(19) 0.3938(2) 0.0317(13) Uani 1 1 d . . . C2H C -0.2511(5) 0.6979(3) 0.4164(3) 0.0461(19) Uani 1 1 d . . . H2HA H -0.2407 0.7300 0.4163 0.055 Uiso 1 1 calc R . . C3H C -0.3318(5) 0.6814(3) 0.4395(3) 0.054(2) Uani 1 1 d . . . H3HA H -0.3761 0.7017 0.4552 0.065 Uiso 1 1 calc R . . C4H C -0.3479(5) 0.6343(3) 0.4397(3) 0.054(2) Uani 1 1 d . . . H4HA H -0.4042 0.6221 0.4546 0.065 Uiso 1 1 calc R . . C5H C -0.2808(5) 0.6057(3) 0.4178(3) 0.0458(19) Uani 1 1 d . . . H5HA H -0.2893 0.5735 0.4182 0.055 Uiso 1 1 calc R . . C6H C -0.2003(4) 0.6250(2) 0.3950(3) 0.0343(15) Uani 1 1 d . . . H6HA H -0.1541 0.6053 0.3798 0.041 Uiso 1 1 calc R . . O1J O 0.3840(3) 0.60089(13) 0.49067(18) 0.0248(9) Uani 1 1 d . . . C2J C 0.4549(4) 0.5932(2) 0.5495(3) 0.0319(15) Uani 1 1 d . . . H2JA H 0.4698 0.5604 0.5543 0.048 Uiso 1 1 calc R . . H2JB H 0.4266 0.6039 0.5862 0.048 Uiso 1 1 calc R . . H2JC H 0.5171 0.6100 0.5482 0.048 Uiso 1 1 calc R . . O1K O -0.0411(3) 0.74776(14) 0.41618(19) 0.0306(10) Uani 1 1 d . . . C2K C -0.0480(5) 0.7964(2) 0.4029(4) 0.048(2) Uani 1 1 d . . . H2KA H -0.0301 0.8135 0.4437 0.073 Uiso 1 1 calc R . . H2KB H -0.1170 0.8042 0.3816 0.073 Uiso 1 1 calc R . . H2KC H -0.0016 0.8047 0.3745 0.073 Uiso 1 1 calc R . . O1L O 0.1853(3) 0.56944(13) 0.51583(18) 0.0261(9) Uani 1 1 d . . . C2L C 0.1527(5) 0.5365(2) 0.5577(3) 0.0420(17) Uani 1 1 d . . . H2LA H 0.1102 0.5516 0.5841 0.063 Uiso 1 1 calc R . . H2LB H 0.2115 0.5230 0.5861 0.063 Uiso 1 1 calc R . . H2LC H 0.1140 0.5124 0.5316 0.063 Uiso 1 1 calc R . . O1M O 0.0500(3) 0.71458(14) 0.30920(18) 0.0289(10) Uani 1 1 d . . . C2M C 0.0494(5) 0.7303(3) 0.2456(3) 0.0409(17) Uani 1 1 d . . . H2MA H 0.1188 0.7345 0.2397 0.061 Uiso 1 1 calc R . . H2MB H 0.0134 0.7595 0.2386 0.061 Uiso 1 1 calc R . . H2MC H 0.0156 0.7077 0.2143 0.061 Uiso 1 1 calc R . . O1S O -0.2830(5) 0.8009(2) 0.4692(3) 0.087(2) Uani 1 1 d D . . C2S C -0.2166(8) 0.8247(4) 0.5164(5) 0.082(3) Uani 1 1 d D . . H2SA H -0.2542 0.8476 0.5369 0.099 Uiso 1 1 calc R . . H2SB H -0.1670 0.8413 0.4961 0.099 Uiso 1 1 calc R . . C3S C -0.1635(6) 0.7932(3) 0.5661(4) 0.071(3) Uani 1 1 d D . . H3SA H -0.1168 0.8105 0.5989 0.107 Uiso 1 1 calc R . . H3SB H -0.1257 0.7707 0.5458 0.107 Uiso 1 1 calc R . . H3SC H -0.2125 0.7772 0.5867 0.107 Uiso 1 1 calc R . . C4S C -0.3416(9) 0.8300(4) 0.4232(5) 0.115(5) Uani 1 1 d D . . H4SA H -0.2981 0.8468 0.3984 0.138 Uiso 1 1 calc R . . H4SB H -0.3783 0.8525 0.4449 0.138 Uiso 1 1 calc R . . C5S C -0.4139(8) 0.8001(5) 0.3790(5) 0.126(6) Uani 1 1 d D . . H5SA H -0.4560 0.8190 0.3459 0.189 Uiso 1 1 calc R . . H5SB H -0.4567 0.7838 0.4041 0.189 Uiso 1 1 calc R . . H5SC H -0.3766 0.7778 0.3581 0.189 Uiso 1 1 calc R . . O1T O 0.5314(6) 0.4807(3) 0.1512(5) 0.111(3) Uani 1 1 d D . . C2T C 0.5088(10) 0.4989(5) 0.0871(5) 0.121(5) Uani 1 1 d D . . H2TA H 0.4455 0.4853 0.0630 0.145 Uiso 1 1 calc R . . H2TB H 0.5634 0.4911 0.0639 0.145 Uiso 1 1 calc R . . C3T C 0.4980(10) 0.5497(4) 0.0895(6) 0.113(4) Uani 1 1 d D . . H3TA H 0.4832 0.5619 0.0453 0.169 Uiso 1 1 calc R . . H3TB H 0.5609 0.5631 0.1133 0.169 Uiso 1 1 calc R . . H3TC H 0.4429 0.5574 0.1115 0.169 Uiso 1 1 calc R . . C4T C 0.5309(10) 0.4316(4) 0.1544(9) 0.166(8) Uani 1 1 d D . . H4TA H 0.5745 0.4186 0.1263 0.199 Uiso 1 1 calc R . . H4TB H 0.4617 0.4198 0.1395 0.199 Uiso 1 1 calc R . . C5T C 0.5700(12) 0.4181(5) 0.2247(9) 0.191(9) Uani 1 1 d D . . H5TA H 0.5713 0.3846 0.2284 0.287 Uiso 1 1 calc R . . H5TB H 0.5258 0.4308 0.2519 0.287 Uiso 1 1 calc R . . H5TC H 0.6383 0.4301 0.2390 0.287 Uiso 1 1 calc R . . O1U O -0.1982(7) 0.4998(3) -0.1323(4) 0.147(4) Uani 1 1 d U . . H1U H -0.1660 0.5029 -0.0941 0.220 Uiso 1 1 d R . . C2U C -0.2279(13) 0.5406(4) -0.1568(7) 0.162(6) Uani 1 1 d U . . H2U1 H -0.2971 0.5457 -0.1511 0.243 Uiso 1 1 d R . . H2U2 H -0.2258 0.5416 -0.2030 0.243 Uiso 1 1 d R . . H2U3 H -0.1841 0.5646 -0.1340 0.243 Uiso 1 1 d 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 0.0232(4) 0.0170(5) 0.0245(4) -0.0010(3) -0.0068(3) 0.0005(3) Fe2 0.0250(4) 0.0151(5) 0.0297(4) 0.0013(4) -0.0028(3) 0.0013(3) Fe3 0.0251(4) 0.0136(5) 0.0282(4) 0.0001(3) -0.0043(3) 0.0006(3) Fe4 0.0234(4) 0.0198(5) 0.0245(4) 0.0012(3) -0.0068(3) 0.0011(3) Fe5 0.0273(4) 0.0147(5) 0.0303(5) -0.0023(4) -0.0059(4) 0.0023(3) Fe6 0.0243(4) 0.0224(5) 0.0329(5) 0.0036(4) -0.0071(4) 0.0028(4) O134 0.0260(19) 0.015(2) 0.0222(19) -0.0013(16) -0.0070(16) 0.0026(16) O234 0.0235(19) 0.014(2) 0.029(2) 0.0037(17) -0.0045(16) 0.0017(16) Cl1 0.0340(8) 0.0159(9) 0.0446(9) 0.0025(7) -0.0040(7) 0.0048(6) Cl2 0.0330(8) 0.0388(11) 0.0448(9) 0.0098(8) -0.0127(7) 0.0090(7) O1A 0.029(2) 0.024(3) 0.026(2) -0.0023(18) -0.0044(17) -0.0047(17) C1A 0.029(3) 0.021(4) 0.029(3) -0.007(3) -0.010(3) -0.003(3) C2A 0.031(3) 0.015(3) 0.028(3) -0.006(2) -0.006(3) 0.002(2) C3A 0.045(4) 0.027(4) 0.026(3) -0.002(3) -0.005(3) -0.003(3) C4A 0.040(4) 0.037(4) 0.032(3) -0.006(3) -0.017(3) 0.003(3) C5A 0.031(3) 0.054(5) 0.041(4) -0.014(4) -0.010(3) -0.004(3) C6A 0.028(3) 0.042(4) 0.034(3) -0.006(3) -0.002(3) -0.005(3) C21A 0.032(3) 0.012(3) 0.024(3) 0.003(2) -0.008(2) 0.000(2) N22A 0.022(2) 0.018(3) 0.027(3) 0.005(2) -0.005(2) 0.0020(19) O23A 0.0220(19) 0.018(2) 0.027(2) -0.0001(17) -0.0051(16) 0.0021(16) C24A 0.035(3) 0.031(4) 0.026(3) -0.005(3) 0.001(3) -0.003(3) C25A 0.072(5) 0.046(5) 0.036(4) 0.004(4) 0.004(4) -0.021(4) O1B 0.035(2) 0.021(3) 0.031(2) -0.0021(18) -0.0002(18) -0.0002(18) C1B 0.029(3) 0.013(3) 0.040(4) -0.001(3) -0.006(3) 0.003(2) C2B 0.033(3) 0.012(3) 0.031(3) 0.000(2) -0.012(3) 0.004(2) C3B 0.038(3) 0.020(4) 0.035(3) 0.006(3) -0.008(3) -0.002(3) C4B 0.043(4) 0.012(4) 0.058(4) 0.000(3) -0.003(3) -0.001(3) C5B 0.046(4) 0.013(4) 0.059(5) -0.012(3) -0.004(3) 0.005(3) C6B 0.031(3) 0.031(4) 0.043(4) -0.004(3) 0.003(3) 0.005(3) C21B 0.029(3) 0.022(4) 0.023(3) 0.004(2) -0.006(2) -0.004(2) N22B 0.026(2) 0.017(3) 0.026(2) 0.002(2) -0.005(2) 0.002(2) O23B 0.026(2) 0.017(2) 0.026(2) -0.0030(17) -0.0007(16) 0.0029(16) C24B 0.032(3) 0.022(4) 0.042(4) 0.000(3) 0.002(3) -0.006(3) C25B 0.059(4) 0.032(5) 0.042(4) 0.011(3) 0.003(3) -0.006(3) C1C 0.032(3) 0.019(4) 0.029(3) 0.000(3) -0.001(3) 0.000(3) C2C 0.031(3) 0.038(4) 0.032(3) -0.001(3) -0.003(3) 0.002(3) C3C 0.039(3) 0.036(4) 0.026(3) 0.005(3) -0.001(3) 0.004(3) C4C 0.038(3) 0.034(4) 0.035(3) 0.007(3) 0.006(3) 0.006(3) C5C 0.032(3) 0.050(5) 0.042(4) 0.002(3) -0.001(3) 0.003(3) C6C 0.033(3) 0.041(5) 0.033(3) 0.005(3) -0.002(3) 0.002(3) C11C 0.032(3) 0.019(4) 0.035(3) -0.001(3) 0.001(3) -0.001(3) O12C 0.028(2) 0.025(3) 0.024(2) -0.0010(18) -0.0044(17) -0.0007(17) O13C 0.028(2) 0.029(3) 0.027(2) 0.0007(18) -0.0039(17) -0.0013(18) N41C 0.048(4) 0.040(4) 0.047(4) 0.001(3) 0.009(3) 0.006(3) O42C 0.041(3) 0.081(5) 0.058(3) 0.013(3) 0.013(3) 0.022(3) O43C 0.051(3) 0.084(5) 0.037(3) 0.006(3) 0.006(2) 0.010(3) C1D 0.027(3) 0.024(4) 0.029(3) 0.001(3) -0.005(3) 0.000(3) C2D 0.043(4) 0.019(4) 0.033(3) -0.004(3) 0.002(3) -0.001(3) C3D 0.041(4) 0.028(4) 0.048(4) -0.008(3) 0.004(3) -0.005(3) C4D 0.052(4) 0.029(4) 0.047(4) 0.000(3) 0.017(3) 0.002(3) C5D 0.057(4) 0.023(4) 0.038(4) -0.004(3) 0.008(3) 0.010(3) C6D 0.044(4) 0.017(4) 0.045(4) -0.003(3) 0.006(3) 0.001(3) C11D 0.028(3) 0.015(4) 0.025(3) 0.001(2) -0.009(2) 0.000(2) O12D 0.028(2) 0.015(2) 0.030(2) -0.0010(17) 0.0006(17) -0.0006(17) O13D 0.025(2) 0.023(3) 0.032(2) -0.0007(19) 0.0006(17) -0.0008(17) N41D 0.072(5) 0.044(5) 0.057(4) 0.000(4) 0.028(4) -0.007(4) O42D 0.106(5) 0.043(4) 0.073(4) 0.002(3) 0.051(4) 0.001(3) O43D 0.098(5) 0.086(6) 0.088(5) -0.008(4) 0.043(4) -0.042(4) C1E 0.028(3) 0.027(4) 0.025(3) 0.004(3) -0.007(2) -0.008(3) C2E 0.032(3) 0.037(4) 0.042(4) -0.001(3) -0.005(3) -0.006(3) C3E 0.043(4) 0.045(5) 0.043(4) -0.007(3) -0.004(3) -0.005(3) C4E 0.052(4) 0.037(5) 0.035(4) -0.004(3) -0.009(3) -0.014(3) C5E 0.040(4) 0.037(5) 0.049(4) -0.004(4) -0.017(3) -0.005(3) C6E 0.033(3) 0.038(4) 0.040(4) -0.007(3) -0.010(3) 0.005(3) C11E 0.026(3) 0.022(4) 0.030(3) 0.006(3) -0.006(3) -0.004(2) O12E 0.024(2) 0.033(3) 0.031(2) 0.001(2) -0.0031(18) 0.0016(18) O13E 0.027(2) 0.026(3) 0.029(2) 0.0007(18) -0.0067(17) 0.0002(17) N41E 0.077(5) 0.050(5) 0.054(4) -0.014(4) -0.012(4) -0.012(4) O42E 0.064(4) 0.097(6) 0.072(4) -0.034(4) -0.033(3) -0.005(4) O43E 0.082(4) 0.090(6) 0.076(4) -0.044(4) 0.006(4) -0.022(4) C1F 0.042(4) 0.023(4) 0.029(3) 0.004(3) -0.006(3) -0.006(3) C2F 0.044(4) 0.028(4) 0.045(4) -0.001(3) -0.004(3) -0.015(3) C3F 0.044(4) 0.054(5) 0.041(4) 0.005(4) -0.007(3) -0.017(4) C4F 0.063(5) 0.048(5) 0.037(4) -0.010(4) -0.001(4) -0.026(4) C5F 0.072(5) 0.038(5) 0.045(4) -0.012(4) -0.005(4) -0.008(4) C6F 0.057(4) 0.025(4) 0.039(4) -0.010(3) -0.012(3) -0.009(3) C11F 0.036(3) 0.015(4) 0.029(3) 0.000(3) -0.002(3) -0.003(3) O12F 0.031(2) 0.020(3) 0.041(2) -0.0046(19) -0.0048(19) -0.0003(18) O13F 0.029(2) 0.019(2) 0.037(2) -0.0032(19) -0.0048(18) -0.0010(18) N41F 0.069(5) 0.064(6) 0.080(5) -0.020(5) 0.007(4) -0.012(4) N1G 0.038(3) 0.018(3) 0.031(3) -0.005(2) -0.003(2) 0.001(2) C2G 0.039(3) 0.037(4) 0.034(4) -0.011(3) -0.004(3) -0.002(3) C3G 0.050(4) 0.050(5) 0.040(4) -0.013(4) 0.000(3) 0.001(4) C4G 0.058(5) 0.051(5) 0.045(4) -0.014(4) 0.008(4) -0.006(4) C5G 0.042(4) 0.045(5) 0.057(5) -0.006(4) 0.008(4) -0.001(3) C6G 0.034(3) 0.029(4) 0.044(4) -0.004(3) -0.001(3) 0.000(3) N1H 0.026(3) 0.032(4) 0.032(3) -0.001(2) -0.007(2) 0.005(2) C2H 0.041(4) 0.054(5) 0.038(4) -0.007(4) -0.006(3) 0.003(4) C3H 0.043(4) 0.080(7) 0.038(4) -0.010(4) 0.005(3) 0.013(4) C4H 0.035(4) 0.094(8) 0.032(4) -0.001(4) 0.001(3) -0.014(4) C5H 0.046(4) 0.045(5) 0.041(4) 0.009(4) -0.005(3) -0.005(3) C6H 0.031(3) 0.033(4) 0.035(3) 0.005(3) -0.003(3) 0.004(3) O1J 0.0232(19) 0.017(2) 0.029(2) -0.0018(17) -0.0089(16) 0.0023(16) C2J 0.033(3) 0.021(4) 0.035(3) 0.001(3) -0.011(3) 0.003(3) O1K 0.030(2) 0.017(2) 0.038(2) 0.0035(19) -0.0084(18) 0.0015(17) C2K 0.045(4) 0.026(4) 0.063(5) 0.005(4) -0.016(4) 0.008(3) O1L 0.030(2) 0.015(2) 0.030(2) 0.0037(17) -0.0034(17) 0.0025(17) C2L 0.050(4) 0.028(4) 0.048(4) 0.021(3) 0.010(3) 0.012(3) O1M 0.027(2) 0.030(3) 0.026(2) 0.0067(18) -0.0044(17) 0.0027(18) C2M 0.036(3) 0.045(5) 0.036(4) 0.015(3) -0.008(3) 0.004(3) O1S 0.095(5) 0.078(5) 0.079(4) -0.006(4) -0.009(4) 0.038(4) C2S 0.102(8) 0.071(8) 0.076(7) -0.007(6) 0.023(6) 0.019(6) C3S 0.054(5) 0.089(8) 0.069(6) -0.019(5) 0.007(4) 0.011(5) C4S 0.134(10) 0.123(12) 0.074(7) 0.003(7) -0.013(7) 0.078(9) C5S 0.087(8) 0.210(17) 0.074(7) 0.015(9) -0.002(6) 0.061(9) O1T 0.131(7) 0.057(5) 0.161(8) -0.004(5) 0.067(6) 0.016(5) C2T 0.141(12) 0.150(15) 0.071(8) -0.009(9) 0.020(8) -0.020(10) C3T 0.149(12) 0.076(10) 0.122(10) -0.008(8) 0.047(9) -0.030(8) C4T 0.086(9) 0.061(10) 0.35(3) -0.023(13) 0.048(13) 0.000(7) C5T 0.151(15) 0.131(15) 0.29(2) 0.125(16) 0.036(15) 0.041(11) O1U 0.209(9) 0.071(6) 0.123(6) -0.013(5) -0.054(6) 0.039(6) C2U 0.265(15) 0.063(9) 0.141(11) 0.009(8) -0.006(11) 0.047(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O1A 1.885(4) . ? Fe1 O1J 1.981(4) . ? Fe1 O12C 2.068(4) . ? Fe1 O23B 2.080(4) . ? Fe1 O134 2.081(4) . ? Fe1 N22A 2.122(5) . ? Fe2 O1B 1.879(4) . ? Fe2 O1K 1.978(4) . ? Fe2 O13D 2.048(4) . ? Fe2 O23A 2.081(4) . ? Fe2 O234 2.084(4) . ? Fe2 N22B 2.106(5) . ? Fe3 O1L 1.962(4) . ? Fe3 O234 1.990(4) . ? Fe3 O12D 2.004(4) . ? Fe3 O134 2.013(4) . ? Fe3 O23A 2.051(4) . ? Fe3 O13F 2.063(4) . ? Fe3 Fe4 2.9593(12) . ? Fe4 O1M 1.974(4) . ? Fe4 O13C 1.984(4) . ? Fe4 O234 1.995(4) . ? Fe4 O134 2.027(4) . ? Fe4 O23B 2.029(4) . ? Fe4 O13E 2.040(4) . ? Fe5 O1J 1.979(4) . ? Fe5 O1L 1.991(4) . ? Fe5 O134 2.036(4) . ? Fe5 O12F 2.042(4) . ? Fe5 N1G 2.154(5) . ? Fe5 Cl1 2.2944(17) . ? Fe6 O1K 1.971(4) . ? Fe6 O1M 2.022(4) . ? Fe6 O234 2.029(4) . ? Fe6 O12E 2.065(4) . ? Fe6 N1H 2.160(5) . ? Fe6 Cl2 2.2749(16) . ? O1A C1A 1.337(6) . ? C1A C6A 1.412(8) . ? C1A C2A 1.418(9) . ? C2A C3A 1.406(8) . ? C2A C21A 1.470(8) . ? C3A C4A 1.381(9) . ? C3A H3AA 0.9500 . ? C4A C5A 1.389(10) . ? C4A H4AA 0.9500 . ? C5A C6A 1.373(8) . ? C5A H5AA 0.9500 . ? C6A H6AA 0.9500 . ? C21A N22A 1.292(7) . ? C21A C24A 1.503(8) . ? N22A O23A 1.405(5) . ? C24A C25A 1.527(9) . ? C24A H24A 0.9900 . ? C24A H24B 0.9900 . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? O1B C1B 1.346(7) . ? C1B C2B 1.401(9) . ? C1B C6B 1.403(9) . ? C2B C3B 1.412(9) . ? C2B C21B 1.468(8) . ? C3B C4B 1.395(9) . ? C3B H3BA 0.9500 . ? C4B C5B 1.379(10) . ? C4B H4BA 0.9500 . ? C5B C6B 1.392(9) . ? C5B H5BA 0.9500 . ? C6B H6BA 0.9500 . ? C21B N22B 1.312(7) . ? C21B C24B 1.505(8) . ? N22B O23B 1.408(6) . ? C24B C25B 1.527(8) . ? C24B H24C 0.9900 . ? C24B H24D 0.9900 . ? C25B H25D 0.9800 . ? C25B H25E 0.9800 . ? C25B H25F 0.9800 . ? C1C C6C 1.396(8) . ? C1C C2C 1.396(8) . ? C1C C11C 1.496(9) . ? C2C C3C 1.395(9) . ? C2C H2CA 0.9500 . ? C3C C4C 1.364(8) . ? C3C H3CA 0.9500 . ? C4C C5C 1.394(9) . ? C4C N41C 1.469(8) . ? C5C C6C 1.379(9) . ? C5C H5CA 0.9500 . ? C6C H6CA 0.9500 . ? C11C O12C 1.259(7) . ? C11C O13C 1.275(7) . ? N41C O43C 1.225(7) . ? N41C O42C 1.237(7) . ? C1D C6D 1.387(9) . ? C1D C2D 1.395(8) . ? C1D C11D 1.489(8) . ? C2D C3D 1.382(9) . ? C2D H2DA 0.9500 . ? C3D C4D 1.346(9) . ? C3D H3DA 0.9500 . ? C4D C5D 1.407(10) . ? C4D N41D 1.471(9) . ? C5D C6D 1.377(9) . ? C5D H5DA 0.9500 . ? C6D H6DA 0.9500 . ? C11D O12D 1.268(7) . ? C11D O13D 1.274(7) . ? N41D O43D 1.221(8) . ? N41D O42D 1.236(8) . ? C1E C2E 1.385(9) . ? C1E C6E 1.390(8) . ? C1E C11E 1.486(8) . ? C2E C3E 1.389(9) . ? C2E H2EA 0.9500 . ? C3E C4E 1.384(9) . ? C3E H3EA 0.9500 . ? C4E C5E 1.349(10) . ? C4E N41E 1.472(9) . ? C5E C6E 1.385(9) . ? C5E H5EA 0.9500 . ? C6E H6EA 0.9500 . ? C11E O12E 1.266(7) . ? C11E O13E 1.280(6) . ? N41E O42E 1.229(8) . ? N41E O43E 1.248(9) . ? C1F C2F 1.372(8) . ? C1F C6F 1.397(10) . ? C1F C11F 1.500(8) . ? C2F C3F 1.414(9) . ? C2F H2FA 0.9500 . ? C3F C4F 1.381(11) . ? C3F H3FA 0.9500 . ? C4F C5F 1.371(10) . ? C4F N41F 1.498(9) . ? C5F C6F 1.388(9) . ? C5F H5FA 0.9500 . ? C6F H6FA 0.9500 . ? C11F O12F 1.262(7) . ? C11F O13F 1.267(7) . ? N41F O42' 1.10(2) . ? N41F O43F 1.116(14) . ? N41F O42F 1.266(14) . ? N41F O43' 1.40(3) . ? N1G C6G 1.344(7) . ? N1G C2G 1.345(7) . ? C2G C3G 1.366(9) . ? C2G H2GA 0.9500 . ? C3G C4G 1.376(10) . ? C3G H3GA 0.9500 . ? C4G C5G 1.368(10) . ? C4G H4GA 0.9500 . ? C5G C6G 1.377(10) . ? C5G H5GA 0.9500 . ? C6G H6GA 0.9500 . ? N1H C2H 1.340(9) . ? N1H C6H 1.351(8) . ? C2H C3H 1.370(10) . ? C2H H2HA 0.9500 . ? C3H C4H 1.391(12) . ? C3H H3HA 0.9500 . ? C4H C5H 1.379(11) . ? C4H H4HA 0.9500 . ? C5H C6H 1.393(9) . ? C5H H5HA 0.9500 . ? C6H H6HA 0.9500 . ? O1J C2J 1.427(6) . ? C2J H2JA 0.9800 . ? C2J H2JB 0.9800 . ? C2J H2JC 0.9800 . ? O1K C2K 1.448(8) . ? C2K H2KA 0.9800 . ? C2K H2KB 0.9800 . ? C2K H2KC 0.9800 . ? O1L C2L 1.432(7) . ? C2L H2LA 0.9800 . ? C2L H2LB 0.9800 . ? C2L H2LC 0.9800 . ? O1M C2M 1.414(7) . ? C2M H2MA 0.9800 . ? C2M H2MB 0.9800 . ? C2M H2MC 0.9800 . ? O1S C2S 1.389(10) . ? O1S C4S 1.410(10) . ? C2S C3S 1.471(11) . ? C2S H2SA 0.9900 . ? C2S H2SB 0.9900 . ? C3S H3SA 0.9800 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C4S C5S 1.492(14) . ? C4S H4SA 0.9900 . ? C4S H4SB 0.9900 . ? C5S H5SA 0.9800 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? O1T C2T 1.427(11) . ? O1T C4T 1.434(12) . ? C2T C3T 1.490(13) . ? C2T H2TA 0.9900 . ? C2T H2TB 0.9900 . ? C3T H3TA 0.9800 . ? C3T H3TB 0.9800 . ? C3T H3TC 0.9800 . ? C4T C5T 1.522(16) . ? C4T H4TA 0.9900 . ? C4T H4TB 0.9900 . ? C5T H5TA 0.9800 . ? C5T H5TB 0.9800 . ? C5T H5TC 0.9800 . ? O1U C2U 1.330(13) . ? O1U H1U 0.8399 . ? C2U H2U1 0.9799 . ? C2U H2U2 0.9801 . ? C2U H2U3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A Fe1 O1J 100.49(16) . . ? O1A Fe1 O12C 92.46(16) . . ? O1J Fe1 O12C 96.60(16) . . ? O1A Fe1 O23B 100.31(16) . . ? O1J Fe1 O23B 159.20(15) . . ? O12C Fe1 O23B 82.89(15) . . ? O1A Fe1 O134 174.71(17) . . ? O1J Fe1 O134 79.17(14) . . ? O12C Fe1 O134 92.83(15) . . ? O23B Fe1 O134 80.09(15) . . ? O1A Fe1 N22A 84.65(17) . . ? O1J Fe1 N22A 94.99(17) . . ? O12C Fe1 N22A 168.38(17) . . ? O23B Fe1 N22A 86.55(16) . . ? O134 Fe1 N22A 90.11(16) . . ? O1B Fe2 O1K 100.60(17) . . ? O1B Fe2 O13D 92.92(17) . . ? O1K Fe2 O13D 95.93(16) . . ? O1B Fe2 O23A 102.70(16) . . ? O1K Fe2 O23A 156.59(16) . . ? O13D Fe2 O23A 80.72(15) . . ? O1B Fe2 O234 173.91(17) . . ? O1K Fe2 O234 78.09(15) . . ? O13D Fe2 O234 93.13(16) . . ? O23A Fe2 O234 78.96(14) . . ? O1B Fe2 N22B 83.91(18) . . ? O1K Fe2 N22B 97.78(17) . . ? O13D Fe2 N22B 166.28(16) . . ? O23A Fe2 N22B 86.94(16) . . ? O234 Fe2 N22B 90.36(17) . . ? O1L Fe3 O234 164.93(17) . . ? O1L Fe3 O12D 99.16(16) . . ? O234 Fe3 O12D 94.82(16) . . ? O1L Fe3 O134 81.25(16) . . ? O234 Fe3 O134 84.50(15) . . ? O12D Fe3 O134 177.07(16) . . ? O1L Fe3 O23A 93.47(15) . . ? O234 Fe3 O23A 81.87(15) . . ? O12D Fe3 O23A 85.95(15) . . ? O134 Fe3 O23A 91.13(15) . . ? O1L Fe3 O13F 91.02(16) . . ? O234 Fe3 O13F 94.79(15) . . ? O12D Fe3 O13F 89.22(16) . . ? O134 Fe3 O13F 93.68(16) . . ? O23A Fe3 O13F 173.87(16) . . ? O1L Fe3 Fe4 124.23(12) . . ? O234 Fe3 Fe4 42.10(11) . . ? O12D Fe3 Fe4 136.61(11) . . ? O134 Fe3 Fe4 43.09(10) . . ? O23A Fe3 Fe4 91.16(11) . . ? O13F Fe3 Fe4 89.76(12) . . ? O1M Fe4 O13C 99.15(17) . . ? O1M Fe4 O234 80.99(16) . . ? O13C Fe4 O234 175.53(16) . . ? O1M Fe4 O134 164.68(17) . . ? O13C Fe4 O134 95.55(16) . . ? O234 Fe4 O134 84.02(15) . . ? O1M Fe4 O23B 94.78(16) . . ? O13C Fe4 O23B 83.51(16) . . ? O234 Fe4 O23B 92.03(15) . . ? O134 Fe4 O23B 82.60(15) . . ? O1M Fe4 O13E 89.62(16) . . ? O13C Fe4 O13E 86.31(16) . . ? O234 Fe4 O13E 98.16(16) . . ? O134 Fe4 O13E 95.61(15) . . ? O23B Fe4 O13E 169.43(16) . . ? O1M Fe4 Fe3 122.73(12) . . ? O13C Fe4 Fe3 138.12(12) . . ? O234 Fe4 Fe3 41.97(10) . . ? O134 Fe4 Fe3 42.73(11) . . ? O23B Fe4 Fe3 92.32(11) . . ? O13E Fe4 Fe3 93.38(12) . . ? O1J Fe5 O1L 97.71(16) . . ? O1J Fe5 O134 80.29(15) . . ? O1L Fe5 O134 79.99(16) . . ? O1J Fe5 O12F 166.81(17) . . ? O1L Fe5 O12F 88.25(16) . . ? O134 Fe5 O12F 89.24(15) . . ? O1J Fe5 N1G 89.06(18) . . ? O1L Fe5 N1G 169.43(16) . . ? O134 Fe5 N1G 93.25(17) . . ? O12F Fe5 N1G 83.52(18) . . ? O1J Fe5 Cl1 96.87(12) . . ? O1L Fe5 Cl1 94.26(12) . . ? O134 Fe5 Cl1 173.12(12) . . ? O12F Fe5 Cl1 94.39(12) . . ? N1G Fe5 Cl1 92.97(14) . . ? O1K Fe6 O1M 94.73(17) . . ? O1K Fe6 O234 79.59(15) . . ? O1M Fe6 O234 79.02(15) . . ? O1K Fe6 O12E 170.09(16) . . ? O1M Fe6 O12E 86.46(17) . . ? O234 Fe6 O12E 91.01(15) . . ? O1K Fe6 N1H 91.52(19) . . ? O1M Fe6 N1H 167.84(19) . . ? O234 Fe6 N1H 91.90(17) . . ? O12E Fe6 N1H 85.63(18) . . ? O1K Fe6 Cl2 97.64(12) . . ? O1M Fe6 Cl2 97.82(12) . . ? O234 Fe6 Cl2 175.54(12) . . ? O12E Fe6 Cl2 91.93(12) . . ? N1H Fe6 Cl2 91.66(13) . . ? Fe3 O134 Fe4 94.19(15) . . ? Fe3 O134 Fe5 95.28(16) . . ? Fe4 O134 Fe5 157.3(2) . . ? Fe3 O134 Fe1 116.22(17) . . ? Fe4 O134 Fe1 96.64(16) . . ? Fe5 O134 Fe1 97.60(14) . . ? Fe3 O234 Fe4 95.93(16) . . ? Fe3 O234 Fe6 152.5(2) . . ? Fe4 O234 Fe6 96.48(16) . . ? Fe3 O234 Fe2 98.34(16) . . ? Fe4 O234 Fe2 115.33(18) . . ? Fe6 O234 Fe2 98.30(16) . . ? C1A O1A Fe1 131.3(4) . . ? O1A C1A C6A 116.3(6) . . ? O1A C1A C2A 123.6(5) . . ? C6A C1A C2A 120.0(5) . . ? C3A C2A C1A 117.5(5) . . ? C3A C2A C21A 119.6(6) . . ? C1A C2A C21A 122.9(5) . . ? C4A C3A C2A 121.7(6) . . ? C4A C3A H3AA 119.1 . . ? C2A C3A H3AA 119.1 . . ? C3A C4A C5A 119.6(5) . . ? C3A C4A H4AA 120.2 . . ? C5A C4A H4AA 120.2 . . ? C6A C5A C4A 120.9(6) . . ? C6A C5A H5AA 119.6 . . ? C4A C5A H5AA 119.6 . . ? C5A C6A C1A 119.8(6) . . ? C5A C6A H6AA 120.1 . . ? C1A C6A H6AA 120.1 . . ? N22A C21A C2A 119.3(5) . . ? N22A C21A C24A 120.0(5) . . ? C2A C21A C24A 120.6(5) . . ? C21A N22A O23A 114.6(5) . . ? C21A N22A Fe1 130.7(4) . . ? O23A N22A Fe1 114.7(3) . . ? N22A O23A Fe3 118.9(3) . . ? N22A O23A Fe2 118.6(3) . . ? Fe3 O23A Fe2 96.53(14) . . ? C21A C24A C25A 113.3(6) . . ? C21A C24A H24A 108.9 . . ? C25A C24A H24A 108.9 . . ? C21A C24A H24B 108.9 . . ? C25A C24A H24B 108.9 . . ? H24A C24A H24B 107.7 . . ? C24A C25A H25A 109.5 . . ? C24A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C24A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C1B O1B Fe2 132.4(4) . . ? O1B C1B C2B 122.8(5) . . ? O1B C1B C6B 117.3(6) . . ? C2B C1B C6B 119.8(6) . . ? C1B C2B C3B 118.3(6) . . ? C1B C2B C21B 123.9(5) . . ? C3B C2B C21B 117.7(6) . . ? C4B C3B C2B 121.5(6) . . ? C4B C3B H3BA 119.3 . . ? C2B C3B H3BA 119.3 . . ? C5B C4B C3B 119.1(6) . . ? C5B C4B H4BA 120.5 . . ? C3B C4B H4BA 120.5 . . ? C4B C5B C6B 120.9(6) . . ? C4B C5B H5BA 119.6 . . ? C6B C5B H5BA 119.6 . . ? C5B C6B C1B 120.2(7) . . ? C5B C6B H6BA 119.9 . . ? C1B C6B H6BA 119.9 . . ? N22B C21B C2B 118.3(5) . . ? N22B C21B C24B 120.3(6) . . ? C2B C21B C24B 121.5(5) . . ? C21B N22B O23B 113.4(5) . . ? C21B N22B Fe2 131.8(4) . . ? O23B N22B Fe2 114.8(3) . . ? N22B O23B Fe4 118.2(3) . . ? N22B O23B Fe1 119.1(3) . . ? Fe4 O23B Fe1 96.58(17) . . ? C21B C24B C25B 111.9(5) . . ? C21B C24B H24C 109.2 . . ? C25B C24B H24C 109.2 . . ? C21B C24B H24D 109.2 . . ? C25B C24B H24D 109.2 . . ? H24C C24B H24D 107.9 . . ? C24B C25B H25D 109.5 . . ? C24B C25B H25E 109.5 . . ? H25D C25B H25E 109.5 . . ? C24B C25B H25F 109.5 . . ? H25D C25B H25F 109.5 . . ? H25E C25B H25F 109.5 . . ? C6C C1C C2C 120.6(6) . . ? C6C C1C C11C 120.3(5) . . ? C2C C1C C11C 119.0(5) . . ? C3C C2C C1C 119.5(6) . . ? C3C C2C H2CA 120.2 . . ? C1C C2C H2CA 120.2 . . ? C4C C3C C2C 118.5(5) . . ? C4C C3C H3CA 120.7 . . ? C2C C3C H3CA 120.7 . . ? C3C C4C C5C 123.2(6) . . ? C3C C4C N41C 117.8(5) . . ? C5C C4C N41C 119.0(6) . . ? C6C C5C C4C 118.2(6) . . ? C6C C5C H5CA 120.9 . . ? C4C C5C H5CA 120.9 . . ? C5C C6C C1C 119.9(6) . . ? C5C C6C H6CA 120.1 . . ? C1C C6C H6CA 120.1 . . ? O12C C11C O13C 124.9(6) . . ? O12C C11C C1C 119.7(5) . . ? O13C C11C C1C 115.3(5) . . ? C11C O12C Fe1 128.5(4) . . ? C11C O13C Fe4 129.9(4) . . ? O43C N41C O42C 122.7(6) . . ? O43C N41C C4C 119.0(5) . . ? O42C N41C C4C 118.3(5) . . ? C6D C1D C2D 119.6(6) . . ? C6D C1D C11D 120.9(6) . . ? C2D C1D C11D 119.5(6) . . ? C3D C2D C1D 119.2(6) . . ? C3D C2D H2DA 120.4 . . ? C1D C2D H2DA 120.4 . . ? C4D C3D C2D 120.2(6) . . ? C4D C3D H3DA 119.9 . . ? C2D C3D H3DA 119.9 . . ? C3D C4D C5D 122.0(7) . . ? C3D C4D N41D 119.8(7) . . ? C5D C4D N41D 118.1(6) . . ? C6D C5D C4D 117.4(6) . . ? C6D C5D H5DA 121.3 . . ? C4D C5D H5DA 121.3 . . ? C5D C6D C1D 121.2(6) . . ? C5D C6D H6DA 119.4 . . ? C1D C6D H6DA 119.4 . . ? O12D C11D O13D 125.2(6) . . ? O12D C11D C1D 117.4(5) . . ? O13D C11D C1D 117.4(5) . . ? C11D O12D Fe3 127.4(4) . . ? C11D O13D Fe2 130.5(4) . . ? O43D N41D O42D 124.0(7) . . ? O43D N41D C4D 118.3(7) . . ? O42D N41D C4D 117.7(7) . . ? C2E C1E C6E 119.5(6) . . ? C2E C1E C11E 121.5(5) . . ? C6E C1E C11E 119.0(6) . . ? C1E C2E C3E 121.0(6) . . ? C1E C2E H2EA 119.5 . . ? C3E C2E H2EA 119.5 . . ? C4E C3E C2E 117.0(7) . . ? C4E C3E H3EA 121.5 . . ? C2E C3E H3EA 121.5 . . ? C5E C4E C3E 123.5(6) . . ? C5E C4E N41E 118.9(6) . . ? C3E C4E N41E 117.6(7) . . ? C4E C5E C6E 119.0(6) . . ? C4E C5E H5EA 120.5 . . ? C6E C5E H5EA 120.5 . . ? C5E C6E C1E 119.9(6) . . ? C5E C6E H6EA 120.1 . . ? C1E C6E H6EA 120.1 . . ? O12E C11E O13E 124.6(5) . . ? O12E C11E C1E 117.7(5) . . ? O13E C11E C1E 117.7(5) . . ? C11E O12E Fe6 130.0(4) . . ? C11E O13E Fe4 123.3(4) . . ? O42E N41E O43E 122.7(7) . . ? O42E N41E C4E 118.9(8) . . ? O43E N41E C4E 118.3(7) . . ? C2F C1F C6F 119.7(6) . . ? C2F C1F C11F 121.9(6) . . ? C6F C1F C11F 118.4(6) . . ? C1F C2F C3F 120.0(7) . . ? C1F C2F H2FA 120.0 . . ? C3F C2F H2FA 120.0 . . ? C4F C3F C2F 118.1(7) . . ? C4F C3F H3FA 120.9 . . ? C2F C3F H3FA 120.9 . . ? C5F C4F C3F 123.3(6) . . ? C5F C4F N41F 117.2(8) . . ? C3F C4F N41F 119.5(7) . . ? C4F C5F C6F 117.5(7) . . ? C4F C5F H5FA 121.2 . . ? C6F C5F H5FA 121.2 . . ? C5F C6F C1F 121.5(7) . . ? C5F C6F H6FA 119.3 . . ? C1F C6F H6FA 119.3 . . ? O12F C11F O13F 125.4(5) . . ? O12F C11F C1F 115.7(5) . . ? O13F C11F C1F 118.9(5) . . ? C11F O12F Fe5 131.1(4) . . ? C11F O13F Fe3 123.9(4) . . ? O42' N41F O43F 110.9(16) . . ? O42' N41F O42F 35.9(18) . . ? O43F N41F O42F 125.2(10) . . ? O42' N41F O43' 126.3(16) . . ? O43F N41F O43' 21.0(11) . . ? O42F N41F O43' 127.1(10) . . ? O42' N41F C4F 116.4(14) . . ? O43F N41F C4F 119.3(10) . . ? O42F N41F C4F 115.4(8) . . ? O43' N41F C4F 113.7(10) . . ? C6G N1G C2G 117.0(6) . . ? C6G N1G Fe5 119.4(4) . . ? C2G N1G Fe5 123.6(4) . . ? N1G C2G C3G 122.8(6) . . ? N1G C2G H2GA 118.6 . . ? C3G C2G H2GA 118.6 . . ? C2G C3G C4G 119.9(7) . . ? C2G C3G H3GA 120.1 . . ? C4G C3G H3GA 120.1 . . ? C5G C4G C3G 118.0(7) . . ? C5G C4G H4GA 121.0 . . ? C3G C4G H4GA 121.0 . . ? C4G C5G C6G 119.7(7) . . ? C4G C5G H5GA 120.2 . . ? C6G C5G H5GA 120.2 . . ? N1G C6G C5G 122.6(6) . . ? N1G C6G H6GA 118.7 . . ? C5G C6G H6GA 118.7 . . ? C2H N1H C6H 118.2(6) . . ? C2H N1H Fe6 120.1(5) . . ? C6H N1H Fe6 121.4(4) . . ? N1H C2H C3H 123.0(8) . . ? N1H C2H H2HA 118.5 . . ? C3H C2H H2HA 118.5 . . ? C2H C3H C4H 119.0(7) . . ? C2H C3H H3HA 120.5 . . ? C4H C3H H3HA 120.5 . . ? C5H C4H C3H 118.8(7) . . ? C5H C4H H4HA 120.6 . . ? C3H C4H H4HA 120.6 . . ? C4H C5H C6H 119.0(8) . . ? C4H C5H H5HA 120.5 . . ? C6H C5H H5HA 120.5 . . ? N1H C6H C5H 121.9(6) . . ? N1H C6H H6HA 119.0 . . ? C5H C6H H6HA 119.0 . . ? C2J O1J Fe5 125.9(4) . . ? C2J O1J Fe1 124.2(3) . . ? Fe5 O1J Fe1 102.93(15) . . ? O1J C2J H2JA 109.5 . . ? O1J C2J H2JB 109.5 . . ? H2JA C2J H2JB 109.5 . . ? O1J C2J H2JC 109.5 . . ? H2JA C2J H2JC 109.5 . . ? H2JB C2J H2JC 109.5 . . ? C2K O1K Fe6 123.7(4) . . ? C2K O1K Fe2 123.4(4) . . ? Fe6 O1K Fe2 103.97(19) . . ? O1K C2K H2KA 109.5 . . ? O1K C2K H2KB 109.5 . . ? H2KA C2K H2KB 109.5 . . ? O1K C2K H2KC 109.5 . . ? H2KA C2K H2KC 109.5 . . ? H2KB C2K H2KC 109.5 . . ? C2L O1L Fe3 123.5(4) . . ? C2L O1L Fe5 127.8(4) . . ? Fe3 O1L Fe5 98.40(17) . . ? O1L C2L H2LA 109.5 . . ? O1L C2L H2LB 109.5 . . ? H2LA C2L H2LB 109.5 . . ? O1L C2L H2LC 109.5 . . ? H2LA C2L H2LC 109.5 . . ? H2LB C2L H2LC 109.5 . . ? C2M O1M Fe4 125.1(4) . . ? C2M O1M Fe6 127.0(3) . . ? Fe4 O1M Fe6 97.35(17) . . ? O1M C2M H2MA 109.5 . . ? O1M C2M H2MB 109.5 . . ? H2MA C2M H2MB 109.5 . . ? O1M C2M H2MC 109.5 . . ? H2MA C2M H2MC 109.5 . . ? H2MB C2M H2MC 109.5 . . ? C2S O1S C4S 112.8(8) . . ? O1S C2S C3S 110.6(8) . . ? O1S C2S H2SA 109.5 . . ? C3S C2S H2SA 109.5 . . ? O1S C2S H2SB 109.5 . . ? C3S C2S H2SB 109.5 . . ? H2SA C2S H2SB 108.1 . . ? C2S C3S H3SA 109.5 . . ? C2S C3S H3SB 109.5 . . ? H3SA C3S H3SB 109.5 . . ? C2S C3S H3SC 109.5 . . ? H3SA C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O1S C4S C5S 106.7(10) . . ? O1S C4S H4SA 110.4 . . ? C5S C4S H4SA 110.4 . . ? O1S C4S H4SB 110.4 . . ? C5S C4S H4SB 110.4 . . ? H4SA C4S H4SB 108.6 . . ? C4S C5S H5SA 109.5 . . ? C4S C5S H5SB 109.5 . . ? H5SA C5S H5SB 109.5 . . ? C4S C5S H5SC 109.5 . . ? H5SA C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? C2T O1T C4T 114.6(11) . . ? O1T C2T C3T 110.1(10) . . ? O1T C2T H2TA 109.6 . . ? C3T C2T H2TA 109.6 . . ? O1T C2T H2TB 109.6 . . ? C3T C2T H2TB 109.6 . . ? H2TA C2T H2TB 108.2 . . ? C2T C3T H3TA 109.5 . . ? C2T C3T H3TB 109.5 . . ? H3TA C3T H3TB 109.5 . . ? C2T C3T H3TC 109.5 . . ? H3TA C3T H3TC 109.5 . . ? H3TB C3T H3TC 109.5 . . ? O1T C4T C5T 107.6(13) . . ? O1T C4T H4TA 110.2 . . ? C5T C4T H4TA 110.2 . . ? O1T C4T H4TB 110.2 . . ? C5T C4T H4TB 110.2 . . ? H4TA C4T H4TB 108.5 . . ? C4T C5T H5TA 109.5 . . ? C4T C5T H5TB 109.5 . . ? H5TA C5T H5TB 109.5 . . ? C4T C5T H5TC 109.5 . . ? H5TA C5T H5TC 109.5 . . ? H5TB C5T H5TC 109.5 . . ? C2U O1U H1U 109.5 . . ? O1U C2U H2U1 108.3 . . ? O1U C2U H2U2 110.2 . . ? H2U1 C2U H2U2 109.5 . . ? O1U C2U H2U3 110.0 . . ? H2U1 C2U H2U3 109.5 . . ? H2U2 C2U H2U3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 26.49 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.740 _refine_diff_density_min -1.098 _refine_diff_density_rms 0.154 # Attachment '- pt9056-(3).cif' data_pt9056 _database_code_depnum_ccdc_archive 'CCDC 794874' #TrackingRef '- pt9056-(3).cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_compound_source 'Brian Tung' _exptl_crystal_recrystallization_method 'diffusion of ether into MeOH solution' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60.83 H60.83 Cl2 Fe6 N8.17 O28' _chemical_formula_weight 1760.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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' _cell_length_a 16.1705(4) _cell_length_b 27.5304(7) _cell_length_c 29.7123(8) _cell_angle_alpha 114.5420(10) _cell_angle_beta 90.8730(10) _cell_angle_gamma 93.4590(10) _cell_volume 11998.6(5) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9632 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 26.26 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5382 _exptl_absorpt_coefficient_mu 1.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6499 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details 'SADABS 2007/2' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 145524 _diffrn_reflns_av_R_equivalents 0.0531 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.75 _diffrn_reflns_theta_max 26.41 _reflns_number_total 48626 _reflns_number_gt 31507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex 2 suite 2009/1' _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution 'Shelxs Sheldrick' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics Shelxp _computing_publication_material 'Platon, encifer' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 432_ALERT_2_A Short Inter X...Y Contact O43E_1 .. C2L'_2 .. 2.43 Ang. There is disorder here 602_ALERT_2_A VERY LARGE Solvent Accessible VOID(S) in Structure ! 041_ALERT_1_C Calc. and Reported SumFormula Strings Differ ? 043_ALERT_1_C Check Reported Molecular Weight ................ 10562.06 044_ALERT_1_C Calculated and Reported Dx Differ .............. ? 068_ALERT_1_C Reported F000 Differs from Calcd (or Missing)... ? The solvent region was treated with SQUEEZE. 12 molecules of MeOH and one pyridine were removed from the asymmetric unit. 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.75 Ratio 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.08 Ratio 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.31 Ratio 220_ALERT_2_B Large Non-Solvent O Ueq(max)/Ueq(min) ... 4.37 Ratio 213_ALERT_2_C Atom O18# has ADP max/min Ratio ..... 3.40 prola 213_ALERT_2_C Atom O39# has ADP max/min Ratio ..... 3.30 prola 215_ALERT_3_C Disordered C178# has ADP max/min Ratio ..... 3.10 220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.32 Ratio 220_ALERT_2_C Large Non-Solvent N Ueq(max)/Ueq(min) ... 3.33 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.13 Ratio 222_ALERT_3_C Large Non-Solvent H Ueq(max)/Ueq(min) ... 3.39 Ratio High thermal motion is expected in these regions. 230_ALERT_2_C Hirshfeld Test Diff for C9# -- C10# .. 5.74 su 230_ALERT_2_C Hirshfeld Test Diff for O42# -- C91# .. 6.65 su 230_ALERT_2_C Hirshfeld Test Diff for O55# -- C119# .. 5.05 su 230_ALERT_2_C Hirshfeld Test Diff for C99# -- C104# .. 5.46 su 230_ALERT_2_C Hirshfeld Test Diff for C152# -- C153# .. 5.19 su 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5E_1 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C2F_1 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C2E_2 241_ALERT_2_C Check High Ueq as Compared to Neighbors for C5H_2 No action taken. 313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O21# 313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O22# 313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O23# 313_ALERT_2_C Oxygen with three covalent bonds (rare) ........ O24# This is due to atoms in different disorder components being incorrectly listed as bonded in the cif. 366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C1F_1 - C2F_1 ... 1.39 Ang. 366_ALERT_2_C Short? C(sp?)-C(sp?) Bond C1F_1 - C6F_1 ... 1.38 Ang. 432_ALERT_2_C Short Inter X...Y Contact C24B_1 .. C24B_3 .. 3.17 Ang. No action taken 911_ALERT_3_C Missing # FCF Refl Between THmin & STh/L= 0.600 299 912_ALERT_4_C Missing # of FCF Reflections Above STh/L= 0.600 321 Completeness meets IUCr minimum requirements. 301_ALERT_3_G Note: Main Residue Disorder ................... 4.00 Perc. 860_ALERT_3_G Note: Number of Least-Squares Restraints ....... 157 Note that same distance restraints, thermal similarity and vibration restraints were applied to control geometry and thermal behavior in disordered regions. 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 1 C58 H52 Cl2 Fe6 N8 O26 790_ALERT_4_C Centre of Gravity not Within Unit Cell: Resd. # 2 C58 H52 Cl2 Fe6 N8 O26 154_ALERT_1_G The su's on the Cell Angles are Equal (x 10000) 100 Deg. 720_ALERT_4_G Number of Unusual/Non-Standard Labels .......... 482 760_ALERT_1_G CIF Contains no Torsion Angles ................. ? 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 23.00 Deg. O42'_-N41E_-O42E_ 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 23.70 Deg. C3F_1-C2F_1-C3F"_ 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 15.10 Deg. C5F"_-C6F_1-C5F_1 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 27.70 Deg. C2J'_-O1J_2-C2J_2 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 28.30 Deg. C2K'_-O1K_3-C2K_3 1.555 1.555 1.555 779_ALERT_4_G Suspect or Irrelevant (Bond) Angle in CIF ...... 33.70 Deg. C2L_3-O1L_3-C2L'_ 1.555 1.555 1.555 No action taken ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 48626 _refine_ls_number_parameters 2770 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1203 _refine_ls_goodness_of_fit_ref 1.002 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1_1 Fe 0.66021(3) 0.383905(19) 0.653252(19) 0.02412(12) Uani 1 1 d . . . Fe2_1 Fe 0.45831(3) 0.355428(19) 0.55806(2) 0.02416(12) Uani 1 1 d . . . Fe3_1 Fe 0.52584(3) 0.273080(19) 0.590369(19) 0.02245(12) Uani 1 1 d . . . Fe4_1 Fe 0.65738(3) 0.313080(19) 0.542384(19) 0.02236(12) Uani 1 1 d . . . Fe5_1 Fe 0.66680(3) 0.273140(19) 0.65669(2) 0.02553(13) Uani 1 1 d . . . Fe6_1 Fe 0.52699(3) 0.27551(2) 0.45967(2) 0.02603(13) Uani 1 1 d . . . Cl1_1 Cl 0.67989(6) 0.24564(4) 0.71864(4) 0.0334(2) Uani 1 1 d . . . Cl2_1 Cl 0.52415(6) 0.26617(4) 0.37889(4) 0.0377(2) Uani 1 1 d . . . O134_1 O 0.64389(14) 0.30387(9) 0.60567(9) 0.0239(6) Uani 1 1 d . . . O234_1 O 0.53487(14) 0.29212(9) 0.53241(9) 0.0221(5) Uani 1 1 d . . . C1A_1 C 0.6202(3) 0.47946(14) 0.73823(14) 0.0312(9) Uani 1 1 d . . . O1A_1 O 0.66607(15) 0.45606(9) 0.69848(9) 0.0283(6) Uani 1 1 d . . . C2A_1 C 0.5361(3) 0.46457(14) 0.73920(15) 0.0359(10) Uani 1 1 d . . . C3A_1 C 0.4952(3) 0.49116(17) 0.78294(17) 0.0509(13) Uani 1 1 d . . . H3A_1 H 0.4382 0.4815 0.7845 0.061 Uiso 1 1 calc R . . C4A_1 C 0.5361(3) 0.53110(19) 0.82387(19) 0.0640(15) Uani 1 1 d . . . H4A_1 H 0.5080 0.5475 0.8537 0.077 Uiso 1 1 calc R . . C5A_1 C 0.6176(3) 0.54733(17) 0.82161(18) 0.0547(13) Uani 1 1 d . . . H5A_1 H 0.6446 0.5761 0.8493 0.066 Uiso 1 1 calc R . . C6A_1 C 0.6601(3) 0.52193(15) 0.77916(15) 0.0389(11) Uani 1 1 d . . . H6A_1 H 0.7162 0.5332 0.7777 0.047 Uiso 1 1 calc R . . C21A_1 C 0.4897(2) 0.42169(14) 0.69636(15) 0.0304(9) Uani 1 1 d . . . N22A_1 N 0.53087(19) 0.38680(11) 0.66181(11) 0.0248(7) Uani 1 1 d . . . O23A_1 O 0.48112(14) 0.34739(9) 0.62322(9) 0.0237(6) Uani 1 1 d . . . C24A_1 C 0.3977(2) 0.41883(15) 0.69272(16) 0.0398(11) Uani 1 1 d . . . H24A_1 H 0.3751 0.3914 0.7030 0.060 Uiso 1 1 calc R . . H24B_1 H 0.3791 0.4095 0.6584 0.060 Uiso 1 1 calc R . . H24C_1 H 0.3783 0.4536 0.7143 0.060 Uiso 1 1 calc R . . C1B_1 C 0.4198(2) 0.46254(14) 0.57283(14) 0.0268(9) Uani 1 1 d . . . O1B_1 O 0.40256(15) 0.41774(9) 0.57870(10) 0.0296(6) Uani 1 1 d . . . C2B_1 C 0.5013(2) 0.48313(13) 0.57205(13) 0.0222(8) Uani 1 1 d . . . C3B_1 C 0.5127(2) 0.52960(13) 0.56355(13) 0.0271(9) Uani 1 1 d . . . H3B_1 H 0.5673 0.5445 0.5640 0.033 Uiso 1 1 calc R . . C4B_1 C 0.4461(2) 0.55403(14) 0.55461(13) 0.0282(9) Uani 1 1 d . . . H4B_1 H 0.4552 0.5846 0.5477 0.034 Uiso 1 1 calc R . . C5B_1 C 0.3678(3) 0.53410(14) 0.55583(14) 0.0311(9) Uani 1 1 d . . . H5B_1 H 0.3221 0.5512 0.5500 0.037 Uiso 1 1 calc R . . C6B_1 C 0.3530(2) 0.48879(15) 0.56544(15) 0.0328(10) Uani 1 1 d . . . H6B_1 H 0.2978 0.4759 0.5670 0.039 Uiso 1 1 calc R . . C21B_1 C 0.5734(2) 0.45831(13) 0.58164(13) 0.0230(8) Uani 1 1 d . . . N22B_1 N 0.56485(18) 0.40935(11) 0.57664(11) 0.0230(7) Uani 1 1 d . . . O23B_1 O 0.63858(14) 0.39032(9) 0.58655(9) 0.0242(6) Uani 1 1 d . . . C24B_1 C 0.6568(2) 0.48834(14) 0.59507(15) 0.0313(9) Uani 1 1 d . . . H24D_1 H 0.6786 0.4885 0.6261 0.047 Uiso 1 1 calc R . . H24E_1 H 0.6518 0.5253 0.5993 0.047 Uiso 1 1 calc R . . H24F_1 H 0.6948 0.4710 0.5686 0.047 Uiso 1 1 calc R . . C1C_1 C 0.9063(2) 0.37870(13) 0.59439(14) 0.0256(9) Uani 1 1 d . . . C2C_1 C 0.9485(2) 0.41830(14) 0.63562(14) 0.0288(9) Uani 1 1 d . . . H2C_1 H 0.9187 0.4388 0.6638 0.035 Uiso 1 1 calc R . . C3C_1 C 1.0337(2) 0.42820(14) 0.63596(15) 0.0311(10) Uani 1 1 d . . . H3C_1 H 1.0629 0.4554 0.6639 0.037 Uiso 1 1 calc R . . C4C_1 C 1.0743(2) 0.39777(14) 0.59502(15) 0.0295(9) Uani 1 1 d . . . C5C_1 C 1.0346(2) 0.35788(14) 0.55310(15) 0.0279(9) Uani 1 1 d . . . H5C_1 H 1.0651 0.3373 0.5253 0.034 Uiso 1 1 calc R . . C6C_1 C 0.9506(2) 0.34900(14) 0.55282(14) 0.0268(9) Uani 1 1 d . . . H6C_1 H 0.9219 0.3225 0.5242 0.032 Uiso 1 1 calc R . . C11C_1 C 0.8152(2) 0.36801(13) 0.59468(14) 0.0246(9) Uani 1 1 d . . . O12C_1 O 0.78073(15) 0.38893(9) 0.63558(9) 0.0266(6) Uani 1 1 d . . . O13C_1 O 0.77813(15) 0.33704(9) 0.55371(9) 0.0262(6) Uani 1 1 d . . . N41C_1 N 1.1656(2) 0.40837(13) 0.59486(15) 0.0364(9) Uani 1 1 d . . . O42C_1 O 1.20102(17) 0.44114(11) 0.63312(12) 0.0462(8) Uani 1 1 d . . . O43C_1 O 1.20049(17) 0.38416(11) 0.55640(14) 0.0483(8) Uani 1 1 d . . . C1D_1 C 0.2658(2) 0.23293(13) 0.54801(13) 0.0233(8) Uani 1 1 d . . . C2D_1 C 0.2568(2) 0.18525(14) 0.55400(13) 0.0278(9) Uani 1 1 d . . . H2D_1 H 0.3023 0.1736 0.5666 0.033 Uiso 1 1 calc R . . C3D_1 C 0.1818(3) 0.15502(14) 0.54170(14) 0.0321(10) Uani 1 1 d . . . H3D_1 H 0.1756 0.1220 0.5447 0.039 Uiso 1 1 calc R . . C4D_1 C 0.1164(2) 0.17365(15) 0.52505(14) 0.0320(9) Uani 1 1 d . . . C5D_1 C 0.1244(2) 0.22114(15) 0.51854(14) 0.0330(10) Uani 1 1 d . . . H5D_1 H 0.0788 0.2327 0.5059 0.040 Uiso 1 1 calc R . . C6D_1 C 0.1992(2) 0.25090(14) 0.53068(14) 0.0299(9) Uani 1 1 d . . . H6D_1 H 0.2054 0.2837 0.5272 0.036 Uiso 1 1 calc R . . C11D_1 C 0.3480(2) 0.26380(13) 0.55949(13) 0.0239(8) Uani 1 1 d . . . O12D_1 O 0.40663(14) 0.24567(9) 0.57567(9) 0.0250(6) Uani 1 1 d . . . O13D_1 O 0.35574(14) 0.30592(9) 0.55193(9) 0.0261(6) Uani 1 1 d . . . N41D_1 N 0.0362(2) 0.14286(14) 0.51244(12) 0.0391(9) Uani 1 1 d . . . O42D_1 O 0.0287(2) 0.10182(12) 0.51939(11) 0.0546(9) Uani 1 1 d . . . O43D_1 O -0.02125(18) 0.15946(12) 0.49671(12) 0.0515(9) Uani 1 1 d . . . C1E_1 C 0.6978(2) 0.15119(14) 0.44261(14) 0.0304(9) Uani 1 1 d . . . C2E_1 C 0.7731(2) 0.14482(15) 0.46108(16) 0.0385(11) Uani 1 1 d . . . H2E_1 H 0.8037 0.1752 0.4854 0.046 Uiso 1 1 calc R . . C3E_1 C 0.8052(3) 0.09499(15) 0.44502(17) 0.0478(13) Uani 1 1 d . . . H3E_1 H 0.8566 0.0905 0.4583 0.057 Uiso 1 1 calc R . . C4E_1 C 0.7604(3) 0.05325(15) 0.40973(17) 0.0482(13) Uani 1 1 d . A . C5E_1 C 0.6848(3) 0.05716(17) 0.38936(19) 0.0663(17) Uani 1 1 d . . . H5E_1 H 0.6553 0.0266 0.3646 0.080 Uiso 1 1 calc R . . C6E_1 C 0.6536(3) 0.10738(16) 0.40642(17) 0.0508(13) Uani 1 1 d . . . H6E_1 H 0.6020 0.1116 0.3933 0.061 Uiso 1 1 calc R . . C11E_1 C 0.6605(2) 0.20382(14) 0.46402(14) 0.0287(9) Uani 1 1 d . . . O12E_1 O 0.69482(15) 0.23932(9) 0.50390(9) 0.0268(6) Uani 1 1 d . . . O13E_1 O 0.59534(15) 0.20880(9) 0.44247(9) 0.0287(6) Uani 1 1 d . . . N41E_1 N 0.7896(3) -0.00114(15) 0.39388(19) 0.0767(16) Uani 1 1 d U . . O42E_1 O 0.8471(13) -0.0065(6) 0.4184(4) 0.057(3) Uani 0.60 1 d PU A 1 O43E_1 O 0.7682(6) -0.0352(2) 0.3508(3) 0.101(3) Uani 0.60 1 d PU A 1 O42'_1 O 0.856(2) -0.0086(12) 0.4022(9) 0.105(9) Uani 0.40 1 d PU A 2 O43'_1 O 0.7266(5) -0.0409(3) 0.3816(4) 0.059(3) Uani 0.40 1 d PU A 2 C1F_1 C 0.6146(3) 0.11495(14) 0.53522(14) 0.0300(9) Uani 1 1 d . C . C2F_1 C 0.5522(3) 0.08644(15) 0.49961(16) 0.0483(12) Uani 1 1 d DU . . H2F_1 H 0.5151 0.1072 0.4913 0.058 Uiso 1 1 calc R B 1 C3F_1 C 0.5377(6) 0.0307(2) 0.4746(3) 0.031(2) Uani 0.50 1 d PDU C 1 H3F_1 H 0.4888 0.0131 0.4551 0.037 Uiso 0.50 1 calc PR C 1 C4F_1 C 0.6031(6) 0.0045(3) 0.4816(3) 0.037(3) Uiso 0.50 1 d PDU C 1 C5F_1 C 0.6760(6) 0.0325(3) 0.5104(4) 0.039(3) Uiso 0.50 1 d PDU C 1 H5F_1 H 0.7244 0.0137 0.5076 0.047 Uiso 0.50 1 calc PR C 1 N41F_1 N 0.6033(5) -0.0551(3) 0.4538(3) 0.045(2) Uiso 0.50 1 d PDU C 1 O42F_1 O 0.5525(4) -0.0748(2) 0.4199(2) 0.0356(15) Uiso 0.50 1 d PDU C 1 O43F_1 O 0.6537(5) -0.0766(3) 0.4698(3) 0.052(2) Uiso 0.50 1 d PDU C 1 C3F"_1 C 0.5704(6) 0.0335(3) 0.4679(3) 0.035(2) Uiso 0.50 1 d PDU C 2 H3F"_1 H 0.5381 0.0148 0.4380 0.042 Uiso 0.50 1 calc PR C 2 C4F"_1 C 0.6338(6) 0.0085(3) 0.4793(3) 0.026(2) Uiso 0.50 1 d PDU C 2 C5F"_1 C 0.6880(6) 0.0335(3) 0.5216(4) 0.038(3) Uiso 0.50 1 d PDU C 2 H5F"_1 H 0.7254 0.0156 0.5333 0.046 Uiso 0.50 1 calc PR C 2 N41"_1 N 0.6404(5) -0.0497(3) 0.4475(3) 0.040(2) Uiso 0.50 1 d PDU C 2 O42"_1 O 0.5960(6) -0.0725(3) 0.4121(3) 0.085(3) Uiso 0.50 1 d PDU C 2 O43"_1 O 0.6892(5) -0.0727(3) 0.4601(3) 0.071(3) Uiso 0.50 1 d PDU C 2 C6F_1 C 0.6787(3) 0.08797(16) 0.54336(17) 0.0439(11) Uani 1 1 d DU . . H6F_1 H 0.7208 0.1049 0.5687 0.053 Uiso 1 1 calc R C 1 C11F_1 C 0.6117(2) 0.17380(13) 0.56546(14) 0.0258(9) Uani 1 1 d . . . O12F_1 O 0.55581(15) 0.19641(9) 0.55213(9) 0.0268(6) Uani 1 1 d . C . O13F_1 O 0.66319(15) 0.19635(9) 0.60090(9) 0.0265(6) Uani 1 1 d . C . N1G_1 N 0.79850(19) 0.27552(11) 0.64662(12) 0.0288(8) Uani 1 1 d . . . C2G_1 C 0.8518(3) 0.30031(15) 0.68627(17) 0.0390(11) Uani 1 1 d . . . H2G_1 H 0.8300 0.3164 0.7183 0.047 Uiso 1 1 calc R . . C3G_1 C 0.9360(3) 0.30303(17) 0.68206(18) 0.0441(11) Uani 1 1 d . . . H3G_1 H 0.9716 0.3207 0.7108 0.053 Uiso 1 1 calc R . . C4G_1 C 0.9684(3) 0.28009(17) 0.63630(19) 0.0445(12) Uani 1 1 d . . . H4G_1 H 1.0267 0.2816 0.6327 0.053 Uiso 1 1 calc R . . C5G_1 C 0.9151(3) 0.25477(15) 0.59558(17) 0.0382(10) Uani 1 1 d . . . H5G_1 H 0.9361 0.2384 0.5634 0.046 Uiso 1 1 calc R . . C6G_1 C 0.8303(2) 0.25333(15) 0.60181(16) 0.0321(10) Uani 1 1 d . . . H6G_1 H 0.7938 0.2361 0.5735 0.039 Uiso 1 1 calc R . . N1H_1 N 0.42163(19) 0.21753(12) 0.44379(11) 0.0292(8) Uani 1 1 d . . . C2H_1 C 0.4217(3) 0.17716(15) 0.45814(14) 0.0331(10) Uani 1 1 d . . . H2H_1 H 0.4696 0.1741 0.4754 0.040 Uiso 1 1 calc R . . C3H_1 C 0.3552(3) 0.14010(15) 0.44876(15) 0.0370(10) Uani 1 1 d . . . H3H_1 H 0.3579 0.1118 0.4589 0.044 Uiso 1 1 calc R . . C4H_1 C 0.2841(3) 0.14449(16) 0.42433(15) 0.0388(11) Uani 1 1 d . . . H4H_1 H 0.2377 0.1192 0.4173 0.047 Uiso 1 1 calc R . . C5H_1 C 0.2825(3) 0.18627(16) 0.41054(15) 0.0397(11) Uani 1 1 d . . . H5H_1 H 0.2342 0.1910 0.3946 0.048 Uiso 1 1 calc R . . C6H_1 C 0.3520(3) 0.22135(15) 0.42012(14) 0.0360(10) Uani 1 1 d . . . H6H_1 H 0.3508 0.2495 0.4096 0.043 Uiso 1 1 calc R . . O1I_1 O 0.67965(16) 0.35095(9) 0.69967(9) 0.0280(6) Uani 1 1 d . . . C2I_1 C 0.6736(3) 0.37574(16) 0.75230(14) 0.0485(13) Uani 1 1 d . . . H2I1_1 H 0.6864 0.3503 0.7662 0.073 Uiso 1 1 calc R . . H2I2_1 H 0.6171 0.3866 0.7604 0.073 Uiso 1 1 calc R . . H2I3_1 H 0.7130 0.4073 0.7664 0.073 Uiso 1 1 calc R . . O1J_1 O 0.45476(14) 0.33566(9) 0.48601(9) 0.0260(6) Uani 1 1 d . . . C2J_1 C 0.3948(2) 0.35485(15) 0.46284(16) 0.0349(10) Uani 1 1 d . . . H2J1_1 H 0.4034 0.3406 0.4272 0.052 Uiso 1 1 calc R . . H2J2_1 H 0.4009 0.3941 0.4771 0.052 Uiso 1 1 calc R . . H2J3_1 H 0.3389 0.3430 0.4683 0.052 Uiso 1 1 calc R . . O1K_1 O 0.54344(15) 0.26677(9) 0.65271(9) 0.0260(6) Uani 1 1 d . . . C2K_1 C 0.4834(3) 0.2651(2) 0.68514(19) 0.0665(16) Uani 1 1 d . . . H2K1_1 H 0.5099 0.2619 0.7136 0.100 Uiso 1 1 calc R . . H2K2_1 H 0.4436 0.2342 0.6680 0.100 Uiso 1 1 calc R . . H2K3_1 H 0.4542 0.2981 0.6967 0.100 Uiso 1 1 calc R . . O1L_1 O 0.63490(14) 0.32084(9) 0.48041(9) 0.0252(6) Uani 1 1 d . . . C2L_1 C 0.6980(2) 0.32576(17) 0.44862(15) 0.0356(10) Uani 1 1 d . . . H2L1_1 H 0.6719 0.3290 0.4201 0.053 Uiso 1 1 calc R . . H2L2_1 H 0.7298 0.2939 0.4370 0.053 Uiso 1 1 calc R . . H2L3_1 H 0.7352 0.3577 0.4671 0.053 Uiso 1 1 calc R . . Fe1_2 Fe 0.69825(3) 0.77182(2) 0.226094(19) 0.02436(13) Uani 1 1 d . . . Fe2_2 Fe 0.92715(3) 0.81579(2) 0.19118(2) 0.02645(13) Uani 1 1 d . D . Fe3_2 Fe 0.77641(3) 0.76904(2) 0.11784(2) 0.02763(13) Uani 1 1 d . . . Fe4_2 Fe 0.73724(3) 0.86847(2) 0.20313(2) 0.02670(13) Uani 1 1 d . D . Fe5_2 Fe 0.60031(3) 0.73258(2) 0.12515(2) 0.02955(14) Uani 1 1 d . . . Fe6_2 Fe 0.88616(3) 0.91463(2) 0.17181(2) 0.03104(14) Uani 1 1 d . D . Cl1_2 Cl 0.51566(7) 0.65779(4) 0.07920(4) 0.0451(3) Uani 1 1 d . . . Cl2_2 Cl 0.94584(6) 0.99966(4) 0.19612(4) 0.0430(3) Uani 1 1 d . . . O134_2 O 0.68771(14) 0.79253(9) 0.16739(9) 0.0263(6) Uani 1 1 d . . . O234_2 O 0.83388(14) 0.84116(9) 0.16019(9) 0.0265(6) Uani 1 1 d . . . C1A_2 C 0.7561(2) 0.71102(13) 0.28125(14) 0.0256(9) Uani 1 1 d . . . O1A_2 O 0.71334(15) 0.74760(9) 0.27591(9) 0.0262(6) Uani 1 1 d . . . C2A_2 C 0.8161(2) 0.68342(14) 0.24801(14) 0.0273(9) Uani 1 1 d . . . C3A_2 C 0.8550(2) 0.64277(15) 0.25712(15) 0.0343(10) Uani 1 1 d . . . H3A_2 H 0.8937 0.6223 0.2345 0.041 Uiso 1 1 calc R . . C4A_2 C 0.8376(3) 0.63261(16) 0.29765(16) 0.0375(10) Uani 1 1 d . . . H4A_2 H 0.8638 0.6051 0.3025 0.045 Uiso 1 1 calc R . . C5A_2 C 0.7827(2) 0.66205(15) 0.33119(15) 0.0350(10) Uani 1 1 d . . . H5A_2 H 0.7722 0.6558 0.3598 0.042 Uiso 1 1 calc R . . C6A_2 C 0.7429(2) 0.70091(15) 0.32299(14) 0.0299(9) Uani 1 1 d . . . H6A_2 H 0.7053 0.7214 0.3465 0.036 Uiso 1 1 calc R . . C21A_2 C 0.8441(2) 0.69643(14) 0.20744(14) 0.0274(9) Uani 1 1 d . . . N22A_2 N 0.80603(19) 0.73130(11) 0.19741(11) 0.0248(7) Uani 1 1 d . . . O23A_2 O 0.84540(15) 0.74664(9) 0.16320(9) 0.0253(6) Uani 1 1 d . . . C24A_2 C 0.9181(3) 0.67180(16) 0.17951(16) 0.0405(11) Uani 1 1 d . . . H24A_2 H 0.9262 0.6832 0.1526 0.061 Uiso 1 1 calc R . . H24B_2 H 0.9090 0.6327 0.1656 0.061 Uiso 1 1 calc R . . H24C_2 H 0.9674 0.6833 0.2020 0.061 Uiso 1 1 calc R . . C1B_2 C 1.0330(2) 0.81690(13) 0.27312(14) 0.0274(9) Uani 1 1 d . . . O1B_2 O 1.01008(15) 0.79750(10) 0.22507(9) 0.0329(6) Uani 1 1 d . . . C2B_2 C 0.9771(2) 0.83963(13) 0.31103(14) 0.0258(9) Uani 1 1 d . . . C3B_2 C 1.0081(3) 0.85890(14) 0.35998(15) 0.0322(10) Uani 1 1 d . . . H3B_2 H 0.9715 0.8747 0.3860 0.039 Uiso 1 1 calc R . . C4B_2 C 1.0895(3) 0.85590(15) 0.37188(16) 0.0371(10) Uani 1 1 d . . . H4B_2 H 1.1085 0.8695 0.4056 0.045 Uiso 1 1 calc R . . C5B_2 C 1.1429(3) 0.83315(15) 0.33481(15) 0.0345(10) Uani 1 1 d . . . H5B_2 H 1.1993 0.8309 0.3428 0.041 Uiso 1 1 calc R . . C6B_2 C 1.1151(3) 0.81345(14) 0.28587(15) 0.0336(10) Uani 1 1 d . . . H6B_2 H 1.1525 0.7973 0.2604 0.040 Uiso 1 1 calc R . . C21B_2 C 0.8881(2) 0.84317(13) 0.30159(13) 0.0251(9) Uani 1 1 d . . . N22B_2 N 0.86348(18) 0.83759(11) 0.25768(11) 0.0249(7) Uani 1 1 d . . . O23B_2 O 0.77790(15) 0.84075(9) 0.25209(9) 0.0264(6) Uani 1 1 d . . . C24B_2 C 0.8300(2) 0.85307(14) 0.34243(13) 0.0297(9) Uani 1 1 d . . . H24D_2 H 0.7731 0.8516 0.3298 0.045 Uiso 1 1 calc R . . H24E_2 H 0.8445 0.8885 0.3692 0.045 Uiso 1 1 calc R . . H24F_2 H 0.8342 0.8256 0.3551 0.045 Uiso 1 1 calc R . . C1C_2 C 0.5291(2) 0.89626(14) 0.29684(14) 0.0280(9) Uani 1 1 d . . . C2C_2 C 0.5212(2) 0.95023(14) 0.30846(14) 0.0320(10) Uani 1 1 d . . . H2C_2 H 0.5627 0.9700 0.2993 0.038 Uiso 1 1 calc R . . C3C_2 C 0.4544(2) 0.97478(15) 0.33286(16) 0.0371(11) Uani 1 1 d . . . H3C_2 H 0.4498 1.0119 0.3420 0.045 Uiso 1 1 calc R . . C4C_2 C 0.3933(3) 0.94479(15) 0.34405(16) 0.0403(11) Uani 1 1 d . . . C5C_2 C 0.3986(3) 0.89109(15) 0.33341(16) 0.0437(11) Uani 1 1 d . . . H5C_2 H 0.3566 0.8714 0.3422 0.052 Uiso 1 1 calc R . . C6C_2 C 0.4681(3) 0.86726(15) 0.30931(16) 0.0378(10) Uani 1 1 d . . . H6C_2 H 0.4738 0.8305 0.3013 0.045 Uiso 1 1 calc R . . C11C_2 C 0.6001(2) 0.86930(14) 0.26826(14) 0.0270(9) Uani 1 1 d . . . O12C_2 O 0.64373(15) 0.89442(9) 0.24811(9) 0.0288(6) Uani 1 1 d . . . O13C_2 O 0.61201(15) 0.82255(9) 0.26403(9) 0.0267(6) Uani 1 1 d . . . N41C_2 N 0.3198(2) 0.97040(15) 0.36853(16) 0.0569(12) Uani 1 1 d . . . O42C_2 O 0.3214(2) 1.01962(13) 0.38606(18) 0.1046(17) Uani 1 1 d . . . O43C_2 O 0.2608(2) 0.94308(12) 0.37089(13) 0.0600(10) Uani 1 1 d . . . C1D_2 C 1.0031(3) 0.72297(17) 0.04134(15) 0.0376(10) Uani 1 1 d . . . C2D_2 C 1.0868(3) 0.72251(18) 0.05046(16) 0.0468(12) Uani 1 1 d . . . H2D_2 H 1.1097 0.7403 0.0834 0.056 Uiso 1 1 calc R . . C3D_2 C 1.1383(3) 0.69628(19) 0.01200(17) 0.0539(13) Uani 1 1 d . . . H3D_2 H 1.1958 0.6951 0.0181 0.065 Uiso 1 1 calc R . . C4D_2 C 1.1031(3) 0.6723(2) -0.03474(17) 0.0566(14) Uani 1 1 d . . . C5D_2 C 1.0213(3) 0.6731(2) -0.04514(18) 0.0747(19) Uani 1 1 d . . . H5D_2 H 0.9999 0.6572 -0.0785 0.090 Uiso 1 1 calc R . . C6D_2 C 0.9691(3) 0.6973(2) -0.00668(17) 0.0664(16) Uani 1 1 d . . . H6D_2 H 0.9112 0.6963 -0.0131 0.080 Uiso 1 1 calc R . . C11D_2 C 0.9464(3) 0.75005(16) 0.08259(15) 0.0338(10) Uani 1 1 d . . . O12D_2 O 0.86959(16) 0.74395(11) 0.07202(9) 0.0338(7) Uani 1 1 d . . . O13D_2 O 0.98011(15) 0.77712(10) 0.12527(9) 0.0323(6) Uani 1 1 d . . . N41D_2 N 1.1564(3) 0.6453(2) -0.07653(16) 0.0828(17) Uani 1 1 d . . . O42D_2 O 1.2280(3) 0.64009(19) -0.06640(14) 0.1007(16) Uani 1 1 d . . . O43D_2 O 1.1265(3) 0.6279(2) -0.11818(14) 0.1090(18) Uani 1 1 d . . . C1E_2 C 0.6172(2) 0.80132(15) 0.01693(14) 0.0281(9) Uani 1 1 d . . . C2E_2 C 0.5351(3) 0.7950(2) 0.00243(18) 0.0612(15) Uani 1 1 d . . . H2E_2 H 0.4961 0.7817 0.0189 0.073 Uiso 1 1 calc R . . C3E_2 C 0.5075(3) 0.8074(2) -0.03515(18) 0.0592(15) Uani 1 1 d . . . H3E_2 H 0.4503 0.8023 -0.0451 0.071 Uiso 1 1 calc R . . C4E_2 C 0.5648(2) 0.82730(14) -0.05792(13) 0.0269(9) Uani 1 1 d . . . C5E_2 C 0.6482(2) 0.83481(17) -0.04416(15) 0.0370(10) Uani 1 1 d . . . H5E_2 H 0.6871 0.8486 -0.0603 0.044 Uiso 1 1 calc R . . C6E_2 C 0.6734(2) 0.82171(16) -0.00612(14) 0.0339(10) Uani 1 1 d . . . H6E_2 H 0.7304 0.8269 0.0042 0.041 Uiso 1 1 calc R . . C11E_2 C 0.6451(2) 0.78553(15) 0.05707(14) 0.0303(9) Uani 1 1 d . . . O12E_2 O 0.59081(16) 0.76645(11) 0.07576(10) 0.0358(7) Uani 1 1 d . . . O13E_2 O 0.72250(15) 0.79291(10) 0.06916(9) 0.0307(6) Uani 1 1 d . . . N41E_2 N 0.5381(2) 0.83896(12) -0.09979(11) 0.0304(8) Uani 1 1 d . . . O42E_2 O 0.46516(17) 0.82506(11) -0.11554(10) 0.0379(7) Uani 1 1 d . . . O43E_2 O 0.58863(18) 0.86009(11) -0.11744(10) 0.0357(7) Uani 1 1 d . . . C1F_2 C 0.6570(2) 0.94363(14) 0.10986(14) 0.0301(9) Uani 1 1 d . . . C2F_2 C 0.5722(3) 0.93587(18) 0.11141(17) 0.0478(12) Uani 1 1 d . . . H2F_2 H 0.5505 0.9124 0.1251 0.057 Uiso 1 1 calc R . . C3F_2 C 0.5181(3) 0.96134(17) 0.09360(16) 0.0428(11) Uani 1 1 d . . . H3F_2 H 0.4597 0.9559 0.0947 0.051 Uiso 1 1 calc R . . C4F_2 C 0.5524(3) 0.99463(15) 0.07432(14) 0.0347(10) Uani 1 1 d . . . C5F_2 C 0.6355(3) 1.00265(17) 0.07053(15) 0.0437(12) Uani 1 1 d . . . H5F_2 H 0.6568 1.0255 0.0560 0.052 Uiso 1 1 calc R . . C6F_2 C 0.6884(3) 0.97592(16) 0.08883(15) 0.0398(11) Uani 1 1 d . . . H6F_2 H 0.7466 0.9804 0.0866 0.048 Uiso 1 1 calc R . . C11F_2 C 0.7141(3) 0.91864(15) 0.13343(15) 0.0332(10) Uani 1 1 d . . . O12F_2 O 0.67961(16) 0.89323(10) 0.15606(10) 0.0328(6) Uani 1 1 d . . . O13F_2 O 0.79083(16) 0.92551(11) 0.12988(10) 0.0362(7) Uani 1 1 d . . . N41F_2 N 0.4945(3) 1.02433(14) 0.05730(12) 0.0378(9) Uani 1 1 d . . . O42F_2 O 0.4196(2) 1.01404(12) 0.05726(11) 0.0488(8) Uani 1 1 d . . . O43F_2 O 0.5264(2) 1.05748(12) 0.04408(11) 0.0473(8) Uani 1 1 d . . . N1G_2 N 0.49679(19) 0.78054(13) 0.15696(12) 0.0314(8) Uani 1 1 d . . . C2G_2 C 0.4253(3) 0.76025(17) 0.16857(16) 0.0409(11) Uani 1 1 d . . . H2G_2 H 0.4218 0.7239 0.1641 0.049 Uiso 1 1 calc R . . C3G_2 C 0.3583(3) 0.78985(19) 0.18644(16) 0.0466(12) Uani 1 1 d . . . H3G_2 H 0.3095 0.7743 0.1941 0.056 Uiso 1 1 calc R . . C4G_2 C 0.3634(3) 0.8427(2) 0.19311(17) 0.0509(13) Uani 1 1 d . . . H4G_2 H 0.3181 0.8641 0.2056 0.061 Uiso 1 1 calc R . . C5G_2 C 0.4352(3) 0.86389(18) 0.18144(16) 0.0425(11) Uani 1 1 d . . . H5G_2 H 0.4398 0.9002 0.1858 0.051 Uiso 1 1 calc R . . C6G_2 C 0.4998(3) 0.83200(16) 0.16349(14) 0.0345(10) Uani 1 1 d . . . H6G_2 H 0.5487 0.8469 0.1553 0.041 Uiso 1 1 calc R . . N1H_2 N 0.9508(2) 0.88492(13) 0.10360(12) 0.0350(8) Uani 1 1 d . . . C2H_2 C 1.0332(3) 0.89141(18) 0.10480(17) 0.0475(12) Uani 1 1 d . . . H2H_2 H 1.0616 0.9091 0.1362 0.057 Uiso 1 1 calc R . . C3H_2 C 1.0798(3) 0.8742(2) 0.06351(18) 0.0627(15) Uani 1 1 d . . . H3H_2 H 1.1385 0.8801 0.0663 0.075 Uiso 1 1 calc R . . C4H_2 C 1.0390(4) 0.8482(3) 0.01833(19) 0.085(2) Uani 1 1 d . . . H4H_2 H 1.0687 0.8360 -0.0113 0.102 Uiso 1 1 calc R . . C5H_2 C 0.9537(4) 0.8402(3) 0.0167(2) 0.102(3) Uani 1 1 d . . . H5H_2 H 0.9238 0.8217 -0.0142 0.122 Uiso 1 1 calc R . . C6H_2 C 0.9130(3) 0.8589(2) 0.05952(18) 0.0632(15) Uani 1 1 d . . . H6H_2 H 0.8543 0.8529 0.0577 0.076 Uiso 1 1 calc R . . O1I_2 O 0.61571(15) 0.71490(9) 0.18252(9) 0.0277(6) Uani 1 1 d . . . C2I_2 C 0.5896(3) 0.66752(17) 0.18820(18) 0.0566(14) Uani 1 1 d . . . H2I1_2 H 0.6070 0.6714 0.2213 0.085 Uiso 1 1 calc R . . H2I2_2 H 0.6148 0.6369 0.1632 0.085 Uiso 1 1 calc R . . H2I3_2 H 0.5291 0.6617 0.1840 0.085 Uiso 1 1 calc R . . O1J_2 O 0.97311(15) 0.88839(10) 0.20236(9) 0.0311(6) Uani 1 1 d DU . . C2J_2 C 1.0319(6) 0.9202(5) 0.2419(4) 0.049(3) Uani 0.50 1 d PDU D 1 H2J1_2 H 1.0449 0.9548 0.2406 0.073 Uiso 0.50 1 calc PR D 1 H2J2_2 H 1.0826 0.9015 0.2384 0.073 Uiso 0.50 1 calc PR D 1 H2J3_2 H 1.0081 0.9261 0.2737 0.073 Uiso 0.50 1 calc PR D 1 C2J'_2 C 1.0558(5) 0.9078(5) 0.2220(4) 0.037(3) Uani 0.50 1 d PDU D 2 H2J4_2 H 1.0664 0.9445 0.2251 0.056 Uiso 0.50 1 calc PR D 2 H2J5_2 H 1.0952 0.8848 0.1997 0.056 Uiso 0.50 1 calc PR D 2 H2J6_2 H 1.0623 0.9073 0.2547 0.056 Uiso 0.50 1 calc PR D 2 O1K_2 O 0.70401(16) 0.70260(10) 0.09171(9) 0.0334(6) Uani 1 1 d . . . C2K_2 C 0.7284(3) 0.64985(19) 0.0768(2) 0.0679(16) Uani 1 1 d . . . H2K1_2 H 0.6794 0.6245 0.0652 0.102 Uiso 1 1 calc R . . H2K2_2 H 0.7558 0.6466 0.1049 0.102 Uiso 1 1 calc R . . H2K3_2 H 0.7670 0.6420 0.0499 0.102 Uiso 1 1 calc R . . O1L_2 O 0.80986(15) 0.93448(10) 0.22785(10) 0.0318(6) Uani 1 1 d DU . . C2L_2 C 0.7801(4) 0.9866(2) 0.2532(3) 0.0438(16) Uani 0.70 1 d PDU D 1 H2L1_2 H 0.8268 1.0138 0.2623 0.066 Uiso 0.70 1 calc PR D 1 H2L2_2 H 0.7530 0.9888 0.2832 0.066 Uiso 0.70 1 calc PR D 1 H2L3_2 H 0.7402 0.9930 0.2315 0.066 Uiso 0.70 1 calc PR D 1 C2L'_2 C 0.8200(9) 0.9734(6) 0.2778(4) 0.046(4) Uani 0.30 1 d PDU D 2 H2L4_2 H 0.8394 1.0081 0.2783 0.069 Uiso 0.30 1 calc PR D 2 H2L5_2 H 0.8608 0.9623 0.2957 0.069 Uiso 0.30 1 calc PR D 2 H2L6_2 H 0.7667 0.9767 0.2937 0.069 Uiso 0.30 1 calc PR D 2 Fe1_3 Fe 0.14773(3) 0.38275(2) 0.25270(2) 0.02592(13) Uani 1 1 d . . . Fe2_3 Fe -0.04382(3) 0.34383(2) 0.320881(19) 0.02542(13) Uani 1 1 d . . . Fe3_3 Fe 0.02164(3) 0.26582(2) 0.222869(19) 0.02547(13) Uani 1 1 d . E . Fe4_3 Fe 0.15658(3) 0.30398(2) 0.301455(19) 0.02360(12) Uani 1 1 d . E . Fe5_3 Fe 0.03278(3) 0.26360(2) 0.35514(2) 0.02772(13) Uani 1 1 d . E . Fe6_3 Fe 0.15939(3) 0.27698(2) 0.16003(2) 0.02835(13) Uani 1 1 d . F . Cl1_3 Cl 0.03583(7) 0.25494(4) 0.42856(4) 0.0403(3) Uani 1 1 d . . . Cl2_3 Cl 0.17324(7) 0.25545(4) 0.07790(4) 0.0394(3) Uani 1 1 d . . . O134_3 O 0.13803(14) 0.30093(9) 0.23342(8) 0.0243(6) Uani 1 1 d . . . O234_3 O 0.03516(14) 0.28154(9) 0.29489(9) 0.0237(6) Uani 1 1 d . . . C1A_3 C 0.0946(3) 0.47992(14) 0.24752(14) 0.0330(10) Uani 1 1 d . . . O1A_3 O 0.14511(16) 0.45618(9) 0.26754(9) 0.0320(6) Uani 1 1 d . . . C2A_3 C 0.0110(3) 0.46087(15) 0.23246(14) 0.0314(10) Uani 1 1 d . . . C3A_3 C -0.0338(3) 0.48753(16) 0.20980(15) 0.0444(12) Uani 1 1 d . . . H3A_3 H -0.0899 0.4755 0.1989 0.053 Uiso 1 1 calc R . . C4A_3 C 0.0021(3) 0.53125(17) 0.20299(17) 0.0491(13) Uani 1 1 d . . . H4A_3 H -0.0289 0.5478 0.1865 0.059 Uiso 1 1 calc R . . C5A_3 C 0.0811(3) 0.55019(16) 0.21991(16) 0.0485(13) Uani 1 1 d . . . H5A_3 H 0.1047 0.5807 0.2161 0.058 Uiso 1 1 calc R . . C6A_3 C 0.1280(3) 0.52534(15) 0.24281(15) 0.0382(10) Uani 1 1 d . . . H6A_3 H 0.1828 0.5394 0.2552 0.046 Uiso 1 1 calc R . . C21A_3 C -0.0283(2) 0.41534(15) 0.23874(13) 0.0306(9) Uani 1 1 d . . . N22A_3 N 0.01721(19) 0.38122(12) 0.24465(11) 0.0296(8) Uani 1 1 d . . . O23A_3 O -0.02743(15) 0.33909(9) 0.25059(9) 0.0258(6) Uani 1 1 d . . . C24A_3 C -0.1226(2) 0.40800(16) 0.23904(15) 0.0371(10) Uani 1 1 d . . . H24A_3 H -0.1424 0.3740 0.2119 0.056 Uiso 1 1 calc R . . H24B_3 H -0.1473 0.4375 0.2348 0.056 Uiso 1 1 calc R . . H24C_3 H -0.1385 0.4078 0.2707 0.056 Uiso 1 1 calc R . . C1B_3 C -0.0855(2) 0.44878(14) 0.39188(13) 0.0268(9) Uani 1 1 d . . . O1B_3 O -0.10299(15) 0.40454(10) 0.35127(9) 0.0319(7) Uani 1 1 d . . . C2B_3 C -0.0053(2) 0.47169(14) 0.40797(13) 0.0250(8) Uani 1 1 d . . . C3B_3 C 0.0052(3) 0.51876(14) 0.45246(13) 0.0288(9) Uani 1 1 d . . . H3B_3 H 0.0595 0.5353 0.4633 0.035 Uiso 1 1 calc R . . C4B_3 C -0.0601(3) 0.54127(15) 0.48030(15) 0.0347(10) Uani 1 1 d . . . H4B_3 H -0.0513 0.5726 0.5104 0.042 Uiso 1 1 calc R . . C5B_3 C -0.1394(3) 0.51782(15) 0.46411(14) 0.0346(10) Uani 1 1 d . . . H5B_3 H -0.1853 0.5330 0.4833 0.042 Uiso 1 1 calc R . . C6B_3 C -0.1522(2) 0.47276(15) 0.42059(14) 0.0335(10) Uani 1 1 d . . . H6B_3 H -0.2071 0.4575 0.4097 0.040 Uiso 1 1 calc R . . C21B_3 C 0.0676(2) 0.44841(14) 0.38004(13) 0.0255(9) Uani 1 1 d . . . N22B_3 N 0.05924(18) 0.39973(11) 0.34617(11) 0.0239(7) Uani 1 1 d . . . O23B_3 O 0.13302(14) 0.38261(9) 0.32170(9) 0.0246(6) Uani 1 1 d . . . C24B_3 C 0.1502(2) 0.47933(14) 0.39014(14) 0.0294(9) Uani 1 1 d . . . H24D_3 H 0.1698 0.4802 0.3594 0.044 Uiso 1 1 calc R . . H24E_3 H 0.1900 0.4621 0.4028 0.044 Uiso 1 1 calc R . . H24F_3 H 0.1449 0.5160 0.4148 0.044 Uiso 1 1 calc R . . C1C_3 C 0.3999(2) 0.37712(13) 0.30298(13) 0.0254(9) Uani 1 1 d . . . C2C_3 C 0.4382(2) 0.41649(15) 0.29074(14) 0.0322(9) Uani 1 1 d . . . H2C_3 H 0.4054 0.4364 0.2787 0.039 Uiso 1 1 calc R . . C3C_3 C 0.5227(3) 0.42679(16) 0.29585(16) 0.0393(11) Uani 1 1 d . . . H3C_3 H 0.5491 0.4536 0.2876 0.047 Uiso 1 1 calc R . . C4C_3 C 0.5681(2) 0.39702(15) 0.31334(15) 0.0355(10) Uani 1 1 d . . . C5C_3 C 0.5329(2) 0.35820(15) 0.32600(14) 0.0307(9) Uani 1 1 d . . . H5C_3 H 0.5665 0.3385 0.3379 0.037 Uiso 1 1 calc R . . C6C_3 C 0.4471(2) 0.34807(14) 0.32117(13) 0.0285(9) Uani 1 1 d . . . H6C_3 H 0.4211 0.3217 0.3302 0.034 Uiso 1 1 calc R . . C11C_3 C 0.3083(2) 0.36532(13) 0.29465(13) 0.0242(8) Uani 1 1 d . . . O12C_3 O 0.26992(15) 0.38847(9) 0.27316(9) 0.0283(6) Uani 1 1 d . . . O13C_3 O 0.27565(14) 0.33123(9) 0.30931(9) 0.0259(6) Uani 1 1 d . . . N41C_3 N 0.6602(2) 0.40714(15) 0.31781(15) 0.0493(11) Uani 1 1 d . . . O42C_3 O 0.6914(2) 0.43992(14) 0.30505(14) 0.0696(11) Uani 1 1 d . . . O43C_3 O 0.69876(19) 0.38102(12) 0.33479(14) 0.0665(11) Uani 1 1 d . . . C1D_3 C -0.2372(2) 0.22381(13) 0.23308(13) 0.0240(8) Uani 1 1 d . . . C2D_3 C -0.3010(2) 0.24253(14) 0.26571(14) 0.0292(9) Uani 1 1 d . . . H2D_3 H -0.2916 0.2748 0.2948 0.035 Uiso 1 1 calc R . . C3D_3 C -0.3771(2) 0.21475(14) 0.25608(13) 0.0279(9) Uani 1 1 d . . . H3D_3 H -0.4210 0.2277 0.2779 0.034 Uiso 1 1 calc R . . C4D_3 C -0.3886(2) 0.16722(13) 0.21374(13) 0.0235(8) Uani 1 1 d . . . C5D_3 C -0.3274(2) 0.14820(15) 0.18085(15) 0.0330(10) Uani 1 1 d . . . H5D_3 H -0.3372 0.1159 0.1518 0.040 Uiso 1 1 calc R . . C6D_3 C -0.2519(2) 0.17670(15) 0.19068(14) 0.0349(10) Uani 1 1 d . . . H6D_3 H -0.2090 0.1640 0.1681 0.042 Uiso 1 1 calc R . . C11D_3 C -0.1533(2) 0.25353(15) 0.24564(14) 0.0277(9) Uani 1 1 d . . . O12D_3 O -0.14388(15) 0.29306(10) 0.28706(9) 0.0307(6) Uani 1 1 d . . . O13D_3 O -0.09694(15) 0.23600(10) 0.21509(9) 0.0300(6) Uani 1 1 d . . . N41D_3 N -0.4695(2) 0.13640(12) 0.20474(12) 0.0286(7) Uani 1 1 d . . . O42D_3 O -0.52736(17) 0.15826(11) 0.22940(10) 0.0371(7) Uani 1 1 d . . . O43D_3 O -0.47491(17) 0.09031(10) 0.17309(11) 0.0427(8) Uani 1 1 d . . . C1E_3 C 0.1501(2) 0.11918(15) 0.15974(15) 0.0315(9) Uani 1 1 d . . . C2E_3 C 0.1063(2) 0.08383(15) 0.17393(15) 0.0349(10) Uani 1 1 d . . . H2E_3 H 0.0553 0.0931 0.1896 0.042 Uiso 1 1 calc R . . C3E_3 C 0.1361(3) 0.03466(15) 0.16557(15) 0.0379(10) Uani 1 1 d . . . H3E_3 H 0.1072 0.0104 0.1761 0.045 Uiso 1 1 calc R . . C4E_3 C 0.2094(3) 0.02248(16) 0.14132(18) 0.0450(12) Uani 1 1 d . . . C5E_3 C 0.2534(3) 0.05603(18) 0.12547(19) 0.0535(13) Uani 1 1 d . . . H5E_3 H 0.3032 0.0460 0.1085 0.064 Uiso 1 1 calc R . . C6E_3 C 0.2227(3) 0.10487(17) 0.13512(17) 0.0488(12) Uani 1 1 d . . . H6E_3 H 0.2520 0.1291 0.1247 0.059 Uiso 1 1 calc R . . C11E_3 C 0.1221(2) 0.17390(14) 0.17104(14) 0.0279(9) Uani 1 1 d . . . O12E_3 O 0.16478(15) 0.20087(10) 0.15279(9) 0.0306(6) Uani 1 1 d . . . O13E_3 O 0.06046(15) 0.18961(9) 0.19781(9) 0.0288(6) Uani 1 1 d . . . N41E_3 N 0.2429(3) -0.02955(15) 0.13340(18) 0.0577(12) Uani 1 1 d . . . O42E_3 O 0.2963(3) -0.04551(15) 0.10352(19) 0.1038(17) Uani 1 1 d . . . O43E_3 O 0.21353(19) -0.05408(11) 0.15605(12) 0.0505(8) Uani 1 1 d . . . C1F_3 C 0.2065(2) 0.14409(14) 0.28368(14) 0.0275(9) Uani 1 1 d . . . C2F_3 C 0.1700(3) 0.10574(15) 0.29809(15) 0.0356(10) Uani 1 1 d . . . H2F_3 H 0.1196 0.1123 0.3149 0.043 Uiso 1 1 calc R . . C3F_3 C 0.2064(3) 0.05851(16) 0.28812(16) 0.0413(11) Uani 1 1 d . . . H3F_3 H 0.1827 0.0327 0.2985 0.050 Uiso 1 1 calc R . . C4F_3 C 0.2781(3) 0.05006(16) 0.26267(18) 0.0430(12) Uani 1 1 d . . . C5F_3 C 0.3155(3) 0.08662(16) 0.24738(19) 0.0488(13) Uani 1 1 d . . . H5F_3 H 0.3649 0.0792 0.2296 0.059 Uiso 1 1 calc R . . C6F_3 C 0.2792(3) 0.13447(15) 0.25862(17) 0.0410(11) Uani 1 1 d . . . H6F_3 H 0.3044 0.1606 0.2491 0.049 Uiso 1 1 calc R . . C11F_3 C 0.1655(2) 0.19481(15) 0.29552(15) 0.0291(9) Uani 1 1 d . . . O12F_3 O 0.10091(16) 0.19977(9) 0.31971(10) 0.0309(6) Uani 1 1 d . . . O13F_3 O 0.19636(15) 0.22897(9) 0.28075(9) 0.0276(6) Uani 1 1 d . . . N41F_3 N 0.3166(3) -0.00137(15) 0.25055(18) 0.0582(12) Uani 1 1 d . . . O42F_3 O 0.2832(2) -0.03351(13) 0.26445(14) 0.0703(11) Uani 1 1 d . . . O43F_3 O 0.3789(2) -0.00889(13) 0.22730(16) 0.0753(12) Uani 1 1 d . . . N1G_3 N -0.0714(2) 0.20460(12) 0.32477(12) 0.0303(8) Uani 1 1 d . . . C2G_3 C -0.0727(3) 0.16505(15) 0.27905(16) 0.0380(10) Uani 1 1 d . . . H2G_3 H -0.0267 0.1632 0.2591 0.046 Uiso 1 1 calc R . . C3G_3 C -0.1388(3) 0.12657(16) 0.25970(17) 0.0446(12) Uani 1 1 d . . . H3G_3 H -0.1372 0.0988 0.2273 0.054 Uiso 1 1 calc R . . C4G_3 C -0.2066(3) 0.12900(18) 0.28777(18) 0.0532(13) Uani 1 1 d . . . H4G_3 H -0.2525 0.1031 0.2754 0.064 Uiso 1 1 calc R . . C5G_3 C -0.2059(3) 0.17012(19) 0.33437(18) 0.0577(14) Uani 1 1 d . . . H5G_3 H -0.2525 0.1734 0.3543 0.069 Uiso 1 1 calc R . . C6G_3 C -0.1390(3) 0.20606(18) 0.35206(17) 0.0489(12) Uani 1 1 d . . . H6G_3 H -0.1393 0.2333 0.3848 0.059 Uiso 1 1 calc R . . N1H_3 N 0.29300(19) 0.28161(12) 0.17272(11) 0.0294(8) Uani 1 1 d . . . C2H_3 C 0.3298(2) 0.25656(14) 0.19641(14) 0.0316(9) Uani 1 1 d . . . H2H_3 H 0.2960 0.2363 0.2093 0.038 Uiso 1 1 calc R . . C3H_3 C 0.4146(3) 0.25852(16) 0.20312(15) 0.0375(10) Uani 1 1 d . . . H3H_3 H 0.4387 0.2404 0.2206 0.045 Uiso 1 1 calc R . . C4H_3 C 0.4645(3) 0.28784(17) 0.18356(16) 0.0454(12) Uani 1 1 d . . . H4H_3 H 0.5233 0.2895 0.1870 0.054 Uiso 1 1 calc R . . C5H_3 C 0.4271(3) 0.31383(18) 0.15959(16) 0.0439(11) Uani 1 1 d . . . H5H_3 H 0.4594 0.3343 0.1463 0.053 Uiso 1 1 calc R . . C6H_3 C 0.3422(3) 0.31028(16) 0.15474(16) 0.0425(11) Uani 1 1 d . . . H6H_3 H 0.3169 0.3288 0.1380 0.051 Uiso 1 1 calc R . . O1I_3 O 0.16667(16) 0.35531(10) 0.18110(9) 0.0300(6) Uani 1 1 d . . . C2I_3 C 0.1517(3) 0.38354(15) 0.15111(15) 0.0396(11) Uani 1 1 d . . . H2I1_3 H 0.1604 0.4222 0.1714 0.059 Uiso 1 1 calc R . . H2I2_3 H 0.0944 0.3748 0.1375 0.059 Uiso 1 1 calc R . . H2I3_3 H 0.1899 0.3729 0.1239 0.059 Uiso 1 1 calc R . . O1J_3 O -0.04120(15) 0.32219(9) 0.37669(9) 0.0280(6) Uani 1 1 d . . . C2J_3 C -0.0928(3) 0.34303(17) 0.41770(15) 0.0404(11) Uani 1 1 d . . . H2J1_3 H -0.1216 0.3727 0.4162 0.061 Uiso 1 1 calc R . . H2J2_3 H -0.0587 0.3560 0.4486 0.061 Uiso 1 1 calc R . . H2J3_3 H -0.1336 0.3148 0.4167 0.061 Uiso 1 1 calc R . . O1K_3 O 0.13969(15) 0.30895(9) 0.36857(9) 0.0275(6) Uani 1 1 d DU . . C2K_3 C 0.1744(6) 0.3485(3) 0.4132(3) 0.030(2) Uani 0.50 1 d PDU E 1 H2K1_3 H 0.1547 0.3411 0.4409 0.045 Uiso 0.50 1 calc PR E 1 H2K2_3 H 0.1578 0.3836 0.4170 0.045 Uiso 0.50 1 calc PR E 1 H2K3_3 H 0.2350 0.3485 0.4129 0.045 Uiso 0.50 1 calc PR E 1 C2K'_3 C 0.1938(6) 0.3260(4) 0.4099(3) 0.042(3) Uani 0.50 1 d PDU E 2 H2K4_3 H 0.2205 0.3612 0.4161 0.063 Uiso 0.50 1 calc PR E 2 H2K5_3 H 0.2362 0.3003 0.4040 0.063 Uiso 0.50 1 calc PR E 2 H2K6_3 H 0.1629 0.3284 0.4388 0.063 Uiso 0.50 1 calc PR E 2 O1L_3 O 0.03482(15) 0.26580(10) 0.15752(9) 0.0300(6) Uani 1 1 d DU . . C2L_3 C -0.0199(4) 0.2347(3) 0.1161(2) 0.048(2) Uani 0.70 1 d PDU F 1 H2L1_3 H -0.0025 0.2404 0.0871 0.072 Uiso 0.70 1 calc PR F 1 H2L2_3 H -0.0765 0.2456 0.1236 0.072 Uiso 0.70 1 calc PR F 1 H2L3_3 H -0.0185 0.1967 0.1091 0.072 Uiso 0.70 1 calc PR F 1 C2L'_3 C -0.0305(10) 0.2663(7) 0.1244(6) 0.052(5) Uani 0.30 1 d PDU F 2 H2L4_3 H -0.0066 0.2662 0.0943 0.079 Uiso 0.30 1 calc PR F 2 H2L5_3 H -0.0606 0.2985 0.1406 0.079 Uiso 0.30 1 calc PR F 2 H2L6_3 H -0.0688 0.2344 0.1158 0.079 Uiso 0.30 1 calc PR F 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 Fe1_1 0.0272(3) 0.0192(3) 0.0278(3) 0.0113(2) 0.0040(2) 0.0040(2) Fe2_1 0.0208(3) 0.0230(3) 0.0356(3) 0.0185(2) 0.0059(2) 0.0053(2) Fe3_1 0.0227(3) 0.0190(3) 0.0295(3) 0.0135(2) 0.0027(2) 0.0048(2) Fe4_1 0.0200(3) 0.0212(3) 0.0271(3) 0.0107(2) 0.0035(2) 0.0051(2) Fe5_1 0.0287(3) 0.0208(3) 0.0300(3) 0.0134(2) -0.0011(2) 0.0030(2) Fe6_1 0.0226(3) 0.0302(3) 0.0302(3) 0.0169(2) 0.0025(2) 0.0056(2) Cl1_1 0.0385(6) 0.0316(5) 0.0369(6) 0.0218(4) -0.0054(5) -0.0011(4) Cl2_1 0.0365(6) 0.0506(6) 0.0342(6) 0.0251(5) 0.0033(5) 0.0075(5) O134_1 0.0256(14) 0.0207(12) 0.0283(14) 0.0126(11) 0.0023(11) 0.0049(10) O234_1 0.0202(13) 0.0230(12) 0.0286(14) 0.0158(11) 0.0038(11) 0.0041(10) C1A_1 0.043(3) 0.0219(19) 0.031(2) 0.0129(18) 0.012(2) 0.0052(18) O1A_1 0.0315(15) 0.0189(12) 0.0328(15) 0.0090(11) 0.0071(12) 0.0007(11) C2A_1 0.044(3) 0.0206(19) 0.039(3) 0.0085(18) 0.009(2) 0.0009(18) C3A_1 0.048(3) 0.041(3) 0.052(3) 0.007(2) 0.028(2) 0.000(2) C4A_1 0.069(4) 0.046(3) 0.051(3) -0.005(2) 0.025(3) -0.006(3) C5A_1 0.071(4) 0.032(2) 0.047(3) 0.003(2) 0.015(3) -0.007(2) C6A_1 0.052(3) 0.024(2) 0.037(3) 0.0093(19) 0.010(2) -0.0003(19) C21A_1 0.036(2) 0.0225(19) 0.038(2) 0.0173(18) 0.0144(19) 0.0034(17) N22A_1 0.0323(18) 0.0154(15) 0.0269(18) 0.0089(13) 0.0059(15) 0.0011(13) O23A_1 0.0253(14) 0.0188(12) 0.0312(15) 0.0142(11) 0.0049(11) 0.0037(10) C24A_1 0.037(3) 0.027(2) 0.053(3) 0.015(2) 0.018(2) 0.0028(18) C1B_1 0.035(2) 0.0214(19) 0.032(2) 0.0171(17) 0.0115(18) 0.0121(16) O1B_1 0.0221(14) 0.0265(14) 0.0497(17) 0.0242(13) 0.0113(12) 0.0070(11) C2B_1 0.022(2) 0.0185(17) 0.030(2) 0.0132(16) 0.0132(16) 0.0064(15) C3B_1 0.031(2) 0.0206(18) 0.030(2) 0.0101(17) 0.0087(18) 0.0105(16) C4B_1 0.037(2) 0.0208(19) 0.031(2) 0.0136(17) 0.0072(18) 0.0066(17) C5B_1 0.037(2) 0.026(2) 0.034(2) 0.0133(18) 0.0100(19) 0.0171(18) C6B_1 0.024(2) 0.032(2) 0.050(3) 0.023(2) 0.0126(19) 0.0098(17) C21B_1 0.026(2) 0.0225(19) 0.026(2) 0.0147(16) 0.0114(16) 0.0049(15) N22B_1 0.0240(17) 0.0203(15) 0.0291(18) 0.0136(13) 0.0072(14) 0.0085(13) O23B_1 0.0215(14) 0.0224(13) 0.0330(15) 0.0145(11) 0.0085(11) 0.0089(10) C24B_1 0.026(2) 0.026(2) 0.045(3) 0.0163(18) 0.0052(19) 0.0081(16) C1C_1 0.030(2) 0.0210(18) 0.032(2) 0.0156(17) 0.0006(18) 0.0087(16) C2C_1 0.034(2) 0.0216(19) 0.032(2) 0.0121(17) -0.0030(18) 0.0057(17) C3C_1 0.030(2) 0.025(2) 0.043(3) 0.0195(19) -0.013(2) -0.0042(17) C4C_1 0.027(2) 0.025(2) 0.046(3) 0.0238(19) -0.006(2) 0.0033(17) C5C_1 0.027(2) 0.0242(19) 0.041(2) 0.0214(18) 0.0054(18) 0.0049(16) C6C_1 0.024(2) 0.0225(19) 0.036(2) 0.0147(17) -0.0054(18) 0.0048(16) C11C_1 0.030(2) 0.0181(18) 0.032(2) 0.0164(17) -0.0038(19) 0.0058(16) O12C_1 0.0272(15) 0.0227(13) 0.0303(15) 0.0111(12) 0.0029(12) 0.0030(11) O13C_1 0.0233(14) 0.0267(13) 0.0292(15) 0.0123(12) -0.0019(12) 0.0025(11) N41C_1 0.026(2) 0.0312(19) 0.065(3) 0.0333(19) -0.010(2) -0.0008(16) O42C_1 0.0315(17) 0.0497(18) 0.068(2) 0.0386(17) -0.0193(16) -0.0131(14) O43C_1 0.0218(16) 0.0386(17) 0.089(3) 0.0297(18) 0.0076(17) 0.0090(13) C1D_1 0.024(2) 0.0233(18) 0.022(2) 0.0086(16) 0.0045(16) 0.0054(15) C2D_1 0.031(2) 0.0250(19) 0.029(2) 0.0135(17) -0.0027(18) 0.0009(17) C3D_1 0.047(3) 0.0215(19) 0.028(2) 0.0109(17) 0.0005(19) 0.0022(18) C4D_1 0.034(2) 0.029(2) 0.028(2) 0.0082(18) -0.0044(19) -0.0051(17) C5D_1 0.028(2) 0.034(2) 0.037(2) 0.0151(19) -0.0018(19) 0.0027(18) C6D_1 0.035(2) 0.0242(19) 0.034(2) 0.0152(17) -0.0017(19) 0.0060(17) C11D_1 0.028(2) 0.0201(18) 0.024(2) 0.0087(16) 0.0073(17) 0.0033(16) O12D_1 0.0232(14) 0.0207(12) 0.0357(15) 0.0158(11) 0.0030(12) 0.0057(10) O13D_1 0.0221(14) 0.0248(13) 0.0394(16) 0.0212(12) 0.0027(12) 0.0032(11) N41D_1 0.042(2) 0.034(2) 0.032(2) 0.0074(17) -0.0052(17) -0.0106(17) O42D_1 0.063(2) 0.0489(19) 0.050(2) 0.0230(16) -0.0170(17) -0.0274(16) O43D_1 0.0307(18) 0.0485(19) 0.064(2) 0.0147(17) -0.0097(16) -0.0083(14) C1E_1 0.031(2) 0.028(2) 0.029(2) 0.0081(17) -0.0013(18) 0.0103(17) C2E_1 0.023(2) 0.028(2) 0.050(3) 0.003(2) -0.003(2) 0.0014(17) C3E_1 0.034(3) 0.026(2) 0.065(3) 0.002(2) -0.015(2) 0.0074(19) C4E_1 0.055(3) 0.021(2) 0.056(3) 0.003(2) -0.013(2) 0.017(2) C5E_1 0.070(4) 0.029(2) 0.075(4) -0.003(2) -0.033(3) 0.010(2) C6E_1 0.055(3) 0.035(2) 0.053(3) 0.008(2) -0.020(2) 0.013(2) C11E_1 0.030(2) 0.0238(19) 0.034(2) 0.0128(18) 0.0068(19) 0.0068(17) O12E_1 0.0256(14) 0.0250(13) 0.0262(14) 0.0062(12) 0.0043(12) 0.0088(11) O13E_1 0.0260(15) 0.0324(14) 0.0280(15) 0.0123(12) -0.0020(12) 0.0075(11) N41E_1 0.079(3) 0.029(2) 0.098(4) 0.003(2) -0.038(3) 0.017(2) O42E_1 0.067(6) 0.025(4) 0.063(5) 0.001(4) -0.021(4) 0.026(4) O43E_1 0.172(8) 0.030(3) 0.075(5) -0.005(4) -0.055(5) 0.040(5) O42'_1 0.063(10) 0.044(8) 0.151(17) -0.015(11) -0.041(14) 0.015(7) O43'_1 0.038(5) 0.025(4) 0.091(7) 0.003(5) -0.008(5) 0.001(3) C1F_1 0.044(3) 0.0211(19) 0.026(2) 0.0115(17) -0.0018(19) 0.0041(17) C2F_1 0.075(3) 0.027(2) 0.044(3) 0.0153(19) -0.017(2) 0.010(2) C3F_1 0.032(4) 0.030(4) 0.034(4) 0.016(3) -0.004(4) -0.003(3) C6F_1 0.038(2) 0.030(2) 0.062(3) 0.016(2) -0.001(2) 0.0114(18) C11F_1 0.027(2) 0.0193(18) 0.033(2) 0.0131(17) 0.0062(18) 0.0042(16) O12F_1 0.0311(15) 0.0217(13) 0.0304(15) 0.0131(11) -0.0011(12) 0.0060(11) O13F_1 0.0244(14) 0.0207(12) 0.0350(15) 0.0120(12) -0.0031(12) 0.0052(11) N1G_1 0.0304(19) 0.0241(16) 0.037(2) 0.0176(15) -0.0009(16) 0.0046(14) C2G_1 0.032(2) 0.034(2) 0.051(3) 0.018(2) -0.006(2) -0.0024(19) C3G_1 0.033(3) 0.048(3) 0.058(3) 0.030(2) -0.009(2) -0.004(2) C4G_1 0.024(2) 0.042(3) 0.078(4) 0.036(3) -0.003(2) 0.004(2) C5G_1 0.038(3) 0.034(2) 0.056(3) 0.030(2) 0.009(2) 0.0123(19) C6G_1 0.031(2) 0.030(2) 0.045(3) 0.025(2) -0.002(2) 0.0034(17) N1H_1 0.0297(19) 0.0308(17) 0.0296(19) 0.0149(15) 0.0010(15) 0.0045(14) C2H_1 0.041(3) 0.032(2) 0.029(2) 0.0146(18) 0.0022(19) 0.0106(19) C3H_1 0.048(3) 0.027(2) 0.037(2) 0.0146(19) 0.007(2) 0.0006(19) C4H_1 0.044(3) 0.034(2) 0.035(2) 0.012(2) 0.000(2) -0.0105(19) C5H_1 0.037(3) 0.040(2) 0.039(3) 0.016(2) -0.011(2) -0.006(2) C6H_1 0.042(3) 0.033(2) 0.035(2) 0.0164(19) -0.008(2) 0.0005(19) O1I_1 0.0369(16) 0.0219(13) 0.0266(15) 0.0111(11) 0.0012(12) 0.0044(11) C2I_1 0.091(4) 0.031(2) 0.026(2) 0.0125(19) 0.006(2) 0.012(2) O1J_1 0.0193(13) 0.0327(14) 0.0358(15) 0.0235(12) 0.0026(11) 0.0063(11) C2J_1 0.024(2) 0.036(2) 0.053(3) 0.027(2) -0.009(2) 0.0017(17) O1K_1 0.0266(14) 0.0253(13) 0.0297(15) 0.0150(12) 0.0017(12) 0.0030(11) C2K_1 0.046(3) 0.117(5) 0.073(4) 0.074(4) 0.019(3) 0.019(3) O1L_1 0.0170(13) 0.0341(14) 0.0313(15) 0.0198(12) 0.0059(11) 0.0051(11) C2L_1 0.026(2) 0.052(3) 0.035(2) 0.024(2) 0.0079(19) 0.0015(19) Fe1_2 0.0264(3) 0.0235(3) 0.0277(3) 0.0150(2) -0.0001(2) 0.0036(2) Fe2_2 0.0228(3) 0.0311(3) 0.0270(3) 0.0137(2) -0.0016(2) 0.0021(2) Fe3_2 0.0232(3) 0.0367(3) 0.0273(3) 0.0182(3) -0.0027(2) -0.0005(2) Fe4_2 0.0225(3) 0.0289(3) 0.0366(3) 0.0216(3) -0.0005(2) 0.0012(2) Fe5_2 0.0259(3) 0.0362(3) 0.0314(3) 0.0198(3) -0.0032(3) -0.0034(2) Fe6_2 0.0250(3) 0.0354(3) 0.0398(4) 0.0233(3) 0.0002(3) -0.0021(2) Cl1_2 0.0386(6) 0.0497(6) 0.0460(7) 0.0216(5) -0.0085(5) -0.0123(5) Cl2_2 0.0347(6) 0.0346(5) 0.0628(7) 0.0241(5) 0.0090(5) -0.0042(4) O134_2 0.0207(14) 0.0332(14) 0.0322(15) 0.0210(12) 0.0003(11) 0.0002(11) O234_2 0.0222(14) 0.0322(14) 0.0317(15) 0.0203(12) -0.0002(12) -0.0006(11) C1A_2 0.027(2) 0.0210(18) 0.031(2) 0.0132(17) -0.0038(17) 0.0006(16) O1A_2 0.0310(15) 0.0248(13) 0.0278(14) 0.0149(11) 0.0004(12) 0.0094(11) C2A_2 0.031(2) 0.0251(19) 0.027(2) 0.0119(17) 0.0003(18) 0.0062(17) C3A_2 0.036(2) 0.029(2) 0.042(3) 0.0174(19) -0.003(2) 0.0081(18) C4A_2 0.038(3) 0.036(2) 0.047(3) 0.026(2) -0.006(2) 0.007(2) C5A_2 0.036(2) 0.041(2) 0.040(3) 0.029(2) 0.001(2) 0.0036(19) C6A_2 0.032(2) 0.034(2) 0.029(2) 0.0181(18) 0.0014(18) 0.0035(17) C21A_2 0.027(2) 0.0219(19) 0.030(2) 0.0084(17) -0.0021(17) -0.0006(16) N22A_2 0.0291(18) 0.0234(16) 0.0209(17) 0.0087(13) -0.0009(14) -0.0024(13) O23A_2 0.0253(14) 0.0301(14) 0.0244(14) 0.0149(12) 0.0009(11) 0.0049(11) C24A_2 0.041(3) 0.042(2) 0.045(3) 0.022(2) 0.009(2) 0.015(2) C1B_2 0.034(2) 0.0184(18) 0.032(2) 0.0123(17) -0.0078(19) 0.0015(16) O1B_2 0.0280(15) 0.0408(15) 0.0303(16) 0.0150(13) -0.0032(12) 0.0063(12) C2B_2 0.031(2) 0.0184(18) 0.029(2) 0.0116(16) -0.0023(18) 0.0015(16) C3B_2 0.040(3) 0.026(2) 0.032(2) 0.0126(18) -0.0017(19) 0.0040(18) C4B_2 0.043(3) 0.032(2) 0.037(3) 0.017(2) -0.012(2) -0.0076(19) C5B_2 0.033(2) 0.035(2) 0.040(3) 0.021(2) -0.013(2) -0.0013(19) C6B_2 0.039(2) 0.025(2) 0.041(3) 0.0179(19) -0.002(2) 0.0061(18) C21B_2 0.034(2) 0.0156(17) 0.024(2) 0.0072(16) -0.0012(18) 0.0011(16) N22B_2 0.0219(17) 0.0224(16) 0.0307(19) 0.0111(14) -0.0019(14) 0.0049(13) O23B_2 0.0238(14) 0.0256(13) 0.0338(15) 0.0158(12) 0.0020(12) 0.0064(11) C24B_2 0.037(2) 0.025(2) 0.027(2) 0.0096(17) -0.0056(18) 0.0052(17) C1C_2 0.027(2) 0.028(2) 0.030(2) 0.0129(17) -0.0009(18) 0.0037(17) C2C_2 0.035(2) 0.025(2) 0.034(2) 0.0120(18) -0.0059(19) -0.0041(17) C3C_2 0.028(2) 0.0199(19) 0.058(3) 0.0108(19) -0.001(2) 0.0004(17) C4C_2 0.034(2) 0.027(2) 0.049(3) 0.004(2) 0.007(2) 0.0057(18) C5C_2 0.044(3) 0.027(2) 0.051(3) 0.007(2) 0.012(2) 0.000(2) C6C_2 0.042(3) 0.023(2) 0.048(3) 0.0139(19) 0.011(2) 0.0057(19) C11C_2 0.025(2) 0.028(2) 0.031(2) 0.0158(18) -0.0043(18) -0.0009(16) O12C_2 0.0255(15) 0.0307(14) 0.0369(16) 0.0208(12) 0.0026(12) 0.0007(11) O13C_2 0.0270(15) 0.0239(13) 0.0322(15) 0.0141(12) 0.0025(12) 0.0065(11) N41C_2 0.037(2) 0.038(2) 0.077(3) 0.004(2) 0.016(2) 0.0030(19) O42C_2 0.072(3) 0.0250(19) 0.177(5) 0.000(2) 0.048(3) 0.0090(18) O43C_2 0.040(2) 0.0430(19) 0.092(3) 0.0220(18) 0.0234(19) 0.0064(16) C1D_2 0.029(2) 0.052(3) 0.030(2) 0.017(2) -0.0023(19) 0.000(2) C2D_2 0.040(3) 0.059(3) 0.035(3) 0.014(2) -0.005(2) 0.002(2) C3D_2 0.033(3) 0.074(3) 0.042(3) 0.010(3) 0.010(2) 0.012(2) C4D_2 0.043(3) 0.084(4) 0.032(3) 0.012(3) 0.014(2) 0.014(3) C5D_2 0.043(3) 0.132(5) 0.025(3) 0.009(3) 0.000(2) 0.004(3) C6D_2 0.040(3) 0.110(4) 0.033(3) 0.013(3) -0.003(2) 0.008(3) C11D_2 0.030(2) 0.040(2) 0.038(3) 0.022(2) 0.007(2) 0.0050(19) O12D_2 0.0230(15) 0.0511(17) 0.0300(15) 0.0204(13) -0.0029(12) -0.0005(13) O13D_2 0.0281(15) 0.0414(16) 0.0244(15) 0.0111(13) -0.0019(12) 0.0000(12) N41D_2 0.056(3) 0.129(4) 0.034(3) 0.004(3) 0.013(2) 0.011(3) O42D_2 0.056(3) 0.152(4) 0.060(3) 0.006(3) 0.020(2) 0.031(3) O43D_2 0.079(3) 0.178(5) 0.029(2) 0.002(3) 0.011(2) 0.012(3) C1E_2 0.028(2) 0.034(2) 0.025(2) 0.0154(18) -0.0020(17) 0.0028(17) C2E_2 0.026(3) 0.120(5) 0.069(3) 0.073(3) -0.010(2) -0.019(3) C3E_2 0.028(3) 0.107(4) 0.070(4) 0.066(3) -0.014(2) -0.010(3) C4E_2 0.031(2) 0.026(2) 0.023(2) 0.0099(17) -0.0030(17) 0.0046(17) C5E_2 0.028(2) 0.059(3) 0.035(2) 0.031(2) 0.0041(19) -0.003(2) C6E_2 0.020(2) 0.057(3) 0.029(2) 0.023(2) -0.0011(18) -0.0004(19) C11E_2 0.025(2) 0.038(2) 0.033(2) 0.0200(19) -0.0016(18) 0.0019(18) O12E_2 0.0234(15) 0.0576(18) 0.0368(17) 0.0309(15) -0.0041(13) -0.0033(13) O13E_2 0.0234(15) 0.0441(16) 0.0304(15) 0.0216(13) -0.0025(12) -0.0001(12) N41E_2 0.031(2) 0.0332(18) 0.0240(18) 0.0082(15) 0.0017(16) 0.0106(15) O42E_2 0.0345(17) 0.0460(17) 0.0349(17) 0.0184(14) -0.0077(14) 0.0068(14) O43E_2 0.0406(18) 0.0455(17) 0.0293(16) 0.0226(14) 0.0085(13) 0.0107(14) C1F_2 0.035(2) 0.028(2) 0.035(2) 0.0214(18) -0.0020(19) 0.0003(17) C2F_2 0.042(3) 0.055(3) 0.063(3) 0.043(3) -0.010(2) -0.002(2) C3F_2 0.036(3) 0.050(3) 0.055(3) 0.034(2) -0.005(2) 0.003(2) C4F_2 0.048(3) 0.030(2) 0.026(2) 0.0094(18) -0.001(2) 0.013(2) C5F_2 0.060(3) 0.048(3) 0.039(3) 0.030(2) 0.018(2) 0.027(2) C6F_2 0.047(3) 0.043(2) 0.038(3) 0.023(2) 0.007(2) 0.016(2) C11F_2 0.028(2) 0.035(2) 0.045(3) 0.024(2) -0.002(2) 0.0019(18) O12F_2 0.0271(15) 0.0361(15) 0.0469(17) 0.0296(14) -0.0029(13) -0.0013(12) O13F_2 0.0292(16) 0.0449(16) 0.0477(18) 0.0330(14) -0.0007(14) -0.0009(13) N41F_2 0.058(3) 0.033(2) 0.0216(19) 0.0087(16) 0.0061(18) 0.0186(19) O42F_2 0.050(2) 0.056(2) 0.0449(19) 0.0237(16) 0.0002(16) 0.0243(17) O43F_2 0.068(2) 0.0436(18) 0.0404(18) 0.0242(15) 0.0178(16) 0.0284(16) N1G_2 0.0250(18) 0.043(2) 0.0338(19) 0.0246(16) -0.0024(15) 0.0002(15) C2G_2 0.041(3) 0.044(3) 0.048(3) 0.030(2) 0.001(2) 0.000(2) C3G_2 0.040(3) 0.062(3) 0.048(3) 0.032(2) 0.011(2) 0.009(2) C4G_2 0.045(3) 0.062(3) 0.048(3) 0.024(3) 0.001(2) 0.019(2) C5G_2 0.036(3) 0.048(3) 0.048(3) 0.023(2) 0.004(2) 0.010(2) C6G_2 0.034(2) 0.040(2) 0.033(2) 0.020(2) -0.0048(19) -0.0034(19) N1H_2 0.031(2) 0.041(2) 0.035(2) 0.0200(17) -0.0020(16) -0.0118(16) C2H_2 0.043(3) 0.055(3) 0.033(3) 0.009(2) -0.005(2) -0.007(2) C3H_2 0.049(3) 0.073(4) 0.043(3) 0.004(3) 0.011(3) -0.017(3) C4H_2 0.069(4) 0.119(5) 0.038(3) 0.009(3) 0.012(3) -0.031(4) C5H_2 0.075(5) 0.162(7) 0.034(3) 0.016(4) -0.004(3) -0.058(4) C6H_2 0.046(3) 0.093(4) 0.043(3) 0.027(3) -0.005(3) -0.032(3) O1I_2 0.0265(15) 0.0278(13) 0.0332(15) 0.0179(12) -0.0025(12) -0.0040(11) C2I_2 0.077(4) 0.041(3) 0.056(3) 0.028(2) -0.019(3) -0.022(2) O1J_2 0.0265(15) 0.0324(14) 0.0363(16) 0.0171(12) -0.0039(12) -0.0032(11) C2J_2 0.041(7) 0.055(7) 0.054(7) 0.029(6) -0.006(5) -0.020(6) C2J'_2 0.014(5) 0.059(7) 0.048(7) 0.034(6) -0.011(5) -0.008(4) O1K_2 0.0316(16) 0.0377(15) 0.0317(16) 0.0157(13) -0.0016(13) 0.0001(12) C2K_2 0.055(3) 0.049(3) 0.082(4) 0.010(3) 0.009(3) -0.002(3) O1L_2 0.0267(15) 0.0307(14) 0.0413(16) 0.0190(13) 0.0007(13) -0.0027(11) C2L_2 0.037(4) 0.035(3) 0.055(4) 0.016(3) -0.002(3) -0.010(3) C2L'_2 0.034(8) 0.058(8) 0.034(7) 0.009(6) 0.020(6) -0.014(7) Fe1_3 0.0256(3) 0.0259(3) 0.0280(3) 0.0126(2) 0.0015(2) 0.0045(2) Fe2_3 0.0190(3) 0.0296(3) 0.0233(3) 0.0066(2) 0.0009(2) 0.0037(2) Fe3_3 0.0210(3) 0.0278(3) 0.0246(3) 0.0075(2) 0.0035(2) 0.0037(2) Fe4_3 0.0187(3) 0.0250(3) 0.0286(3) 0.0126(2) 0.0021(2) 0.0026(2) Fe5_3 0.0245(3) 0.0298(3) 0.0293(3) 0.0126(2) 0.0055(2) 0.0024(2) Fe6_3 0.0263(3) 0.0295(3) 0.0298(3) 0.0123(2) 0.0064(2) 0.0051(2) Cl1_3 0.0447(7) 0.0481(6) 0.0347(6) 0.0232(5) 0.0069(5) 0.0070(5) Cl2_3 0.0432(6) 0.0443(6) 0.0296(6) 0.0134(5) 0.0088(5) 0.0082(5) O134_3 0.0233(14) 0.0266(13) 0.0239(14) 0.0111(11) 0.0034(11) 0.0034(11) O234_3 0.0179(13) 0.0276(13) 0.0259(14) 0.0110(11) 0.0023(11) 0.0037(10) C1A_3 0.050(3) 0.023(2) 0.028(2) 0.0103(17) 0.005(2) 0.0155(19) O1A_3 0.0359(16) 0.0278(14) 0.0355(16) 0.0158(12) 0.0005(13) 0.0057(12) C2A_3 0.038(2) 0.028(2) 0.024(2) 0.0050(17) 0.0011(18) 0.0140(18) C3A_3 0.054(3) 0.035(2) 0.040(3) 0.009(2) 0.000(2) 0.023(2) C4A_3 0.066(3) 0.035(2) 0.051(3) 0.021(2) -0.004(3) 0.018(2) C5A_3 0.073(4) 0.027(2) 0.049(3) 0.018(2) 0.000(3) 0.013(2) C6A_3 0.048(3) 0.032(2) 0.036(2) 0.0152(19) 0.004(2) 0.007(2) C21A_3 0.031(2) 0.032(2) 0.022(2) 0.0035(17) -0.0001(17) 0.0117(18) N22A_3 0.035(2) 0.0257(17) 0.0247(18) 0.0070(14) -0.0051(15) 0.0030(14) O23A_3 0.0218(14) 0.0291(14) 0.0248(14) 0.0091(11) 0.0041(11) 0.0034(11) C24A_3 0.027(2) 0.042(2) 0.043(3) 0.018(2) 0.001(2) 0.0101(19) C1B_3 0.032(2) 0.027(2) 0.023(2) 0.0107(17) 0.0034(17) 0.0154(17) O1B_3 0.0237(14) 0.0374(15) 0.0267(15) 0.0043(12) -0.0009(12) 0.0112(12) C2B_3 0.025(2) 0.028(2) 0.027(2) 0.0154(17) 0.0024(17) 0.0090(16) C3B_3 0.041(2) 0.0205(19) 0.026(2) 0.0096(17) 0.0003(18) 0.0121(17) C4B_3 0.052(3) 0.024(2) 0.029(2) 0.0110(18) -0.003(2) 0.014(2) C5B_3 0.041(3) 0.041(2) 0.030(2) 0.020(2) 0.011(2) 0.025(2) C6B_3 0.029(2) 0.036(2) 0.036(2) 0.015(2) 0.0000(19) 0.0121(18) C21B_3 0.032(2) 0.026(2) 0.023(2) 0.0146(17) -0.0057(17) 0.0089(17) N22B_3 0.0220(17) 0.0273(17) 0.0246(17) 0.0122(14) -0.0011(14) 0.0074(13) O23B_3 0.0211(14) 0.0255(13) 0.0269(14) 0.0102(11) 0.0016(11) 0.0052(11) C24B_3 0.027(2) 0.026(2) 0.036(2) 0.0124(18) -0.0017(18) 0.0038(16) C1C_3 0.027(2) 0.0205(18) 0.025(2) 0.0053(16) 0.0061(17) 0.0051(16) C2C_3 0.030(2) 0.030(2) 0.039(2) 0.0162(19) 0.0072(19) 0.0042(17) C3C_3 0.036(3) 0.033(2) 0.048(3) 0.017(2) 0.006(2) -0.0064(19) C4C_3 0.022(2) 0.029(2) 0.043(3) 0.0036(19) 0.0088(19) -0.0053(17) C5C_3 0.022(2) 0.031(2) 0.032(2) 0.0062(18) 0.0023(18) 0.0021(17) C6C_3 0.030(2) 0.027(2) 0.026(2) 0.0081(17) 0.0063(17) 0.0018(17) C11C_3 0.023(2) 0.0205(18) 0.028(2) 0.0086(16) 0.0039(17) 0.0013(15) O12C_3 0.0254(15) 0.0280(14) 0.0339(15) 0.0152(12) -0.0002(12) 0.0026(11) O13C_3 0.0184(14) 0.0285(14) 0.0351(15) 0.0175(12) 0.0024(11) 0.0017(11) N41C_3 0.031(2) 0.035(2) 0.065(3) 0.003(2) 0.011(2) 0.0002(18) O42C_3 0.038(2) 0.064(2) 0.097(3) 0.027(2) 0.0192(19) -0.0202(17) O43C_3 0.0275(18) 0.0355(18) 0.108(3) 0.0011(19) 0.0036(19) 0.0040(15) C1D_3 0.021(2) 0.0241(19) 0.025(2) 0.0086(16) 0.0004(16) 0.0049(15) C2D_3 0.029(2) 0.025(2) 0.026(2) 0.0039(17) 0.0038(18) 0.0018(17) C3D_3 0.024(2) 0.031(2) 0.025(2) 0.0076(17) 0.0044(17) 0.0069(17) C4D_3 0.023(2) 0.0234(19) 0.026(2) 0.0123(16) -0.0019(17) 0.0006(15) C5D_3 0.029(2) 0.031(2) 0.030(2) 0.0032(18) -0.0028(19) 0.0032(18) C6D_3 0.026(2) 0.037(2) 0.031(2) 0.0024(19) 0.0029(18) 0.0052(18) C11D_3 0.022(2) 0.034(2) 0.026(2) 0.0111(18) 0.0004(17) 0.0060(17) O12D_3 0.0231(14) 0.0357(15) 0.0248(15) 0.0043(12) 0.0021(12) 0.0010(12) O13D_3 0.0251(15) 0.0340(15) 0.0251(15) 0.0065(12) 0.0009(12) 0.0039(12) N41D_3 0.0287(19) 0.0303(18) 0.0293(19) 0.0154(16) 0.0005(16) -0.0027(15) O42D_3 0.0285(16) 0.0414(16) 0.0390(17) 0.0152(14) 0.0034(14) -0.0036(13) O43D_3 0.0416(18) 0.0253(15) 0.0538(19) 0.0105(14) -0.0038(15) -0.0073(13) C1E_3 0.025(2) 0.029(2) 0.042(2) 0.0151(19) 0.0107(19) 0.0019(17) C2E_3 0.022(2) 0.034(2) 0.042(3) 0.0089(19) 0.0042(19) 0.0035(17) C3E_3 0.032(2) 0.031(2) 0.047(3) 0.014(2) 0.001(2) -0.0053(18) C4E_3 0.033(3) 0.031(2) 0.072(3) 0.022(2) 0.017(2) 0.0072(19) C5E_3 0.048(3) 0.046(3) 0.074(4) 0.029(3) 0.033(3) 0.020(2) C6E_3 0.051(3) 0.041(3) 0.063(3) 0.028(2) 0.029(3) 0.015(2) C11E_3 0.022(2) 0.026(2) 0.027(2) 0.0033(17) 0.0020(17) -0.0008(16) O12E_3 0.0250(15) 0.0299(14) 0.0377(16) 0.0145(13) 0.0104(12) 0.0024(11) O13E_3 0.0246(15) 0.0252(13) 0.0331(15) 0.0080(12) 0.0103(12) 0.0029(11) N41E_3 0.045(3) 0.035(2) 0.095(4) 0.028(2) 0.017(2) 0.0088(19) O42E_3 0.094(3) 0.063(2) 0.179(5) 0.065(3) 0.092(3) 0.049(2) O43E_3 0.0406(19) 0.0375(17) 0.077(2) 0.0273(17) 0.0003(17) 0.0033(14) C1F_3 0.024(2) 0.0228(19) 0.037(2) 0.0131(17) 0.0035(18) 0.0041(16) C2F_3 0.035(2) 0.030(2) 0.042(3) 0.0161(19) 0.002(2) -0.0004(18) C3F_3 0.045(3) 0.032(2) 0.048(3) 0.019(2) -0.001(2) 0.002(2) C4F_3 0.036(3) 0.027(2) 0.069(3) 0.024(2) -0.008(2) 0.0021(19) C5F_3 0.022(2) 0.039(3) 0.086(4) 0.026(3) 0.009(2) 0.0064(19) C6F_3 0.032(2) 0.028(2) 0.065(3) 0.021(2) 0.006(2) 0.0020(18) C11F_3 0.023(2) 0.029(2) 0.035(2) 0.0132(18) -0.0022(18) 0.0026(17) O12F_3 0.0275(15) 0.0283(14) 0.0401(16) 0.0170(13) 0.0102(13) 0.0042(12) O13F_3 0.0217(14) 0.0258(13) 0.0396(16) 0.0174(12) 0.0046(12) 0.0029(11) N41F_3 0.041(3) 0.037(2) 0.096(4) 0.027(2) -0.005(2) 0.008(2) O42F_3 0.082(3) 0.0399(19) 0.099(3) 0.038(2) -0.004(2) 0.0131(19) O43F_3 0.040(2) 0.048(2) 0.141(4) 0.040(2) 0.010(2) 0.0173(17) N1G_3 0.0324(19) 0.0313(18) 0.0292(19) 0.0143(15) 0.0071(15) 0.0024(15) C2G_3 0.037(3) 0.035(2) 0.041(3) 0.014(2) 0.009(2) 0.0050(19) C3G_3 0.049(3) 0.032(2) 0.045(3) 0.008(2) 0.001(2) 0.005(2) C4G_3 0.059(3) 0.047(3) 0.053(3) 0.024(3) -0.008(3) -0.020(2) C5G_3 0.047(3) 0.065(3) 0.054(3) 0.021(3) 0.014(2) -0.024(3) C6G_3 0.052(3) 0.049(3) 0.038(3) 0.012(2) 0.014(2) -0.008(2) N1H_3 0.0250(18) 0.0297(17) 0.0328(19) 0.0116(15) 0.0108(15) 0.0060(14) C2H_3 0.031(2) 0.028(2) 0.034(2) 0.0109(18) 0.0066(19) 0.0052(17) C3H_3 0.032(2) 0.034(2) 0.038(3) 0.006(2) 0.003(2) 0.0083(19) C4H_3 0.036(3) 0.042(3) 0.043(3) 0.001(2) 0.008(2) 0.005(2) C5H_3 0.032(3) 0.052(3) 0.045(3) 0.018(2) 0.012(2) -0.007(2) C6H_3 0.043(3) 0.040(2) 0.048(3) 0.021(2) 0.005(2) 0.001(2) O1I_3 0.0329(16) 0.0327(14) 0.0274(15) 0.0148(12) 0.0048(12) 0.0081(12) C2I_3 0.057(3) 0.034(2) 0.029(2) 0.0143(19) 0.000(2) 0.000(2) O1J_3 0.0242(14) 0.0335(14) 0.0229(14) 0.0080(12) 0.0071(11) 0.0047(11) C2J_3 0.040(3) 0.044(2) 0.035(2) 0.014(2) 0.017(2) 0.006(2) O1K_3 0.0250(14) 0.0315(14) 0.0247(14) 0.0109(12) 0.0009(11) -0.0026(11) C2K_3 0.008(5) 0.041(5) 0.048(5) 0.026(4) -0.006(4) 0.003(4) C2K'_3 0.011(5) 0.071(7) 0.050(6) 0.031(6) -0.009(4) 0.000(5) O1L_3 0.0249(14) 0.0371(15) 0.0255(15) 0.0099(12) 0.0029(12) 0.0068(12) C2L_3 0.031(4) 0.074(5) 0.027(4) 0.010(4) 0.002(3) -0.003(4) C2L'_3 0.039(8) 0.066(10) 0.034(8) 0.003(8) 0.010(7) 0.001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1_1 O1A_1 1.875(2) . ? Fe1_1 O1I_1 1.971(2) . ? Fe1_1 O12C_1 2.038(3) . ? Fe1_1 O134_1 2.063(2) . ? Fe1_1 O23B_1 2.088(2) . ? Fe1_1 N22A_1 2.113(3) . ? Fe2_1 O1B_1 1.860(2) . ? Fe2_1 O1J_1 1.977(3) . ? Fe2_1 O13D_1 2.038(2) . ? Fe2_1 O23A_1 2.068(2) . ? Fe2_1 O234_1 2.083(2) . ? Fe2_1 N22B_1 2.111(3) . ? Fe3_1 O1K_1 1.949(2) . ? Fe3_1 O12D_1 2.000(2) . ? Fe3_1 O234_1 2.002(2) . ? Fe3_1 O134_1 2.007(2) . ? Fe3_1 O12F_1 2.032(2) . ? Fe3_1 O23A_1 2.050(2) . ? Fe4_1 O1L_1 1.971(2) . ? Fe4_1 O13C_1 2.000(2) . ? Fe4_1 O12E_1 2.009(2) . ? Fe4_1 O234_1 2.012(2) . ? Fe4_1 O134_1 2.012(2) . ? Fe4_1 O23B_1 2.027(2) . ? Fe5_1 O1I_1 1.982(2) . ? Fe5_1 O1K_1 1.989(2) . ? Fe5_1 O134_1 2.059(2) . ? Fe5_1 O13F_1 2.072(2) . ? Fe5_1 N1G_1 2.156(3) . ? Fe5_1 Cl1_1 2.2739(11) . ? Fe6_1 O1J_1 1.976(2) . ? Fe6_1 O1L_1 2.012(2) . ? Fe6_1 O234_1 2.015(2) . ? Fe6_1 O13E_1 2.083(2) . ? Fe6_1 N1H_1 2.167(3) . ? Fe6_1 Cl2_1 2.3048(11) . ? C1A_1 O1A_1 1.347(4) . ? C1A_1 C2A_1 1.400(6) . ? C1A_1 C6A_1 1.402(5) . ? C2A_1 C3A_1 1.399(6) . ? C2A_1 C21A_1 1.481(5) . ? C3A_1 C4A_1 1.380(6) . ? C3A_1 H3A_1 0.9500 . ? C4A_1 C5A_1 1.377(7) . ? C4A_1 H4A_1 0.9500 . ? C5A_1 C6A_1 1.379(6) . ? C5A_1 H5A_1 0.9500 . ? C6A_1 H6A_1 0.9500 . ? C21A_1 N22A_1 1.303(4) . ? C21A_1 C24A_1 1.484(5) . ? N22A_1 O23A_1 1.404(4) . ? C24A_1 H24A_1 0.9800 . ? C24A_1 H24B_1 0.9800 . ? C24A_1 H24C_1 0.9800 . ? C1B_1 O1B_1 1.330(4) . ? C1B_1 C6B_1 1.399(5) . ? C1B_1 C2B_1 1.407(5) . ? C2B_1 C3B_1 1.405(5) . ? C2B_1 C21B_1 1.467(5) . ? C3B_1 C4B_1 1.381(5) . ? C3B_1 H3B_1 0.9500 . ? C4B_1 C5B_1 1.357(5) . ? C4B_1 H4B_1 0.9500 . ? C5B_1 C6B_1 1.399(5) . ? C5B_1 H5B_1 0.9500 . ? C6B_1 H6B_1 0.9500 . ? C21B_1 N22B_1 1.292(4) . ? C21B_1 C24B_1 1.496(5) . ? N22B_1 O23B_1 1.406(3) . ? C24B_1 H24D_1 0.9800 . ? C24B_1 H24E_1 0.9800 . ? C24B_1 H24F_1 0.9800 . ? C1C_1 C2C_1 1.389(5) . ? C1C_1 C6C_1 1.402(5) . ? C1C_1 C11C_1 1.486(5) . ? C2C_1 C3C_1 1.388(5) . ? C2C_1 H2C_1 0.9500 . ? C3C_1 C4C_1 1.363(5) . ? C3C_1 H3C_1 0.9500 . ? C4C_1 C5C_1 1.387(5) . ? C4C_1 N41C_1 1.489(5) . ? C5C_1 C6C_1 1.365(5) . ? C5C_1 H5C_1 0.9500 . ? C6C_1 H6C_1 0.9500 . ? C11C_1 O12C_1 1.264(4) . ? C11C_1 O13C_1 1.274(4) . ? N41C_1 O43C_1 1.225(4) . ? N41C_1 O42C_1 1.225(4) . ? C1D_1 C6D_1 1.389(5) . ? C1D_1 C2D_1 1.396(5) . ? C1D_1 C11D_1 1.488(5) . ? C2D_1 C3D_1 1.381(5) . ? C2D_1 H2D_1 0.9500 . ? C3D_1 C4D_1 1.374(5) . ? C3D_1 H3D_1 0.9500 . ? C4D_1 C5D_1 1.398(5) . ? C4D_1 N41D_1 1.459(5) . ? C5D_1 C6D_1 1.374(5) . ? C5D_1 H5D_1 0.9500 . ? C6D_1 H6D_1 0.9500 . ? C11D_1 O13D_1 1.269(4) . ? C11D_1 O12D_1 1.274(4) . ? N41D_1 O43D_1 1.227(4) . ? N41D_1 O42D_1 1.230(4) . ? C1E_1 C2E_1 1.378(5) . ? C1E_1 C6E_1 1.385(5) . ? C1E_1 C11E_1 1.490(5) . ? C2E_1 C3E_1 1.389(5) . ? C2E_1 H2E_1 0.9500 . ? C3E_1 C4E_1 1.349(5) . ? C3E_1 H3E_1 0.9500 . ? C4E_1 C5E_1 1.386(6) . ? C4E_1 N41E_1 1.481(5) . ? C5E_1 C6E_1 1.390(6) . ? C5E_1 H5E_1 0.9500 . ? C6E_1 H6E_1 0.9500 . ? C11E_1 O13E_1 1.269(4) . ? C11E_1 O12E_1 1.272(4) . ? N41E_1 O42'_1 1.14(3) . ? N41E_1 O42E_1 1.226(17) . ? N41E_1 O43E_1 1.260(7) . ? N41E_1 O43'_1 1.373(9) . ? C1F_1 C6F_1 1.385(5) . ? C1F_1 C2F_1 1.391(5) . ? C1F_1 C11F_1 1.495(5) . ? C2F_1 C3F_1 1.403(7) . ? C2F_1 C3F"_1 1.420(7) . ? C2F_1 H2F_1 0.9500 . ? C3F_1 C4F_1 1.376(9) . ? C3F_1 H3F_1 0.9500 . ? C4F_1 C5F_1 1.424(9) . ? C4F_1 N41F_1 1.499(7) . ? C5F_1 C6F_1 1.429(7) . ? C5F_1 H5F_1 0.9500 . ? N41F_1 O42F_1 1.205(7) . ? N41F_1 O43F_1 1.235(7) . ? C3F"_1 C4F"_1 1.381(9) . ? C3F"_1 H3F"_1 0.9500 . ? C4F"_1 C5F"_1 1.412(9) . ? C4F"_1 N41"_1 1.497(7) . ? C5F"_1 C6F_1 1.383(7) . ? C5F"_1 H5F"_1 0.9500 . ? N41"_1 O42"_1 1.180(8) . ? N41"_1 O43"_1 1.187(7) . ? C6F_1 H6F_1 0.9500 . ? C11F_1 O13F_1 1.247(4) . ? C11F_1 O12F_1 1.275(4) . ? N1G_1 C6G_1 1.339(5) . ? N1G_1 C2G_1 1.351(5) . ? C2G_1 C3G_1 1.369(6) . ? C2G_1 H2G_1 0.9500 . ? C3G_1 C4G_1 1.368(6) . ? C3G_1 H3G_1 0.9500 . ? C4G_1 C5G_1 1.374(6) . ? C4G_1 H4G_1 0.9500 . ? C5G_1 C6G_1 1.386(5) . ? C5G_1 H5G_1 0.9500 . ? C6G_1 H6G_1 0.9500 . ? N1H_1 C2H_1 1.346(5) . ? N1H_1 C6H_1 1.351(5) . ? C2H_1 C3H_1 1.378(6) . ? C2H_1 H2H_1 0.9500 . ? C3H_1 C4H_1 1.388(6) . ? C3H_1 H3H_1 0.9500 . ? C4H_1 C5H_1 1.374(6) . ? C4H_1 H4H_1 0.9500 . ? C5H_1 C6H_1 1.381(6) . ? C5H_1 H5H_1 0.9500 . ? C6H_1 H6H_1 0.9500 . ? O1I_1 C2I_1 1.431(4) . ? C2I_1 H2I1_1 0.9800 . ? C2I_1 H2I2_1 0.9800 . ? C2I_1 H2I3_1 0.9800 . ? O1J_1 C2J_1 1.428(4) . ? C2J_1 H2J1_1 0.9800 . ? C2J_1 H2J2_1 0.9800 . ? C2J_1 H2J3_1 0.9800 . ? O1K_1 C2K_1 1.391(5) . ? C2K_1 H2K1_1 0.9800 . ? C2K_1 H2K2_1 0.9800 . ? C2K_1 H2K3_1 0.9800 . ? O1L_1 C2L_1 1.439(4) . ? C2L_1 H2L1_1 0.9800 . ? C2L_1 H2L2_1 0.9800 . ? C2L_1 H2L3_1 0.9800 . ? Fe1_2 O1A_2 1.877(2) . ? Fe1_2 O1I_2 1.981(2) . ? Fe1_2 O13C_2 2.035(2) . ? Fe1_2 O134_2 2.056(2) . ? Fe1_2 O23B_2 2.077(2) . ? Fe1_2 N22A_2 2.121(3) . ? Fe2_2 O1B_2 1.878(2) . ? Fe2_2 O1J_2 1.980(3) . ? Fe2_2 O13D_2 2.033(3) . ? Fe2_2 O234_2 2.056(2) . ? Fe2_2 O23A_2 2.100(2) . ? Fe2_2 N22B_2 2.116(3) . ? Fe3_2 O1K_2 1.963(3) . ? Fe3_2 O12D_2 2.002(3) . ? Fe3_2 O134_2 2.007(3) . ? Fe3_2 O234_2 2.014(2) . ? Fe3_2 O13E_2 2.026(2) . ? Fe3_2 O23A_2 2.042(2) . ? Fe3_2 Fe4_2 2.9684(8) . ? Fe4_2 O1L_2 1.957(2) . ? Fe4_2 O12C_2 1.995(3) . ? Fe4_2 O234_2 2.010(3) . ? Fe4_2 O134_2 2.017(2) . ? Fe4_2 O23B_2 2.021(2) . ? Fe4_2 O12F_2 2.029(2) . ? Fe5_2 O1I_2 1.974(2) . ? Fe5_2 O1K_2 2.004(3) . ? Fe5_2 O12E_2 2.048(3) . ? Fe5_2 O134_2 2.059(2) . ? Fe5_2 N1G_2 2.172(3) . ? Fe5_2 Cl1_2 2.2904(11) . ? Fe6_2 O1J_2 1.988(2) . ? Fe6_2 O1L_2 1.995(3) . ? Fe6_2 O234_2 2.032(2) . ? Fe6_2 O13F_2 2.080(3) . ? Fe6_2 N1H_2 2.159(3) . ? Fe6_2 Cl2_2 2.2878(11) . ? C1A_2 O1A_2 1.315(4) . ? C1A_2 C6A_2 1.396(5) . ? C1A_2 C2A_2 1.411(5) . ? C2A_2 C3A_2 1.432(5) . ? C2A_2 C21A_2 1.464(5) . ? C3A_2 C4A_2 1.374(6) . ? C3A_2 H3A_2 0.9500 . ? C4A_2 C5A_2 1.371(6) . ? C4A_2 H4A_2 0.9500 . ? C5A_2 C6A_2 1.383(5) . ? C5A_2 H5A_2 0.9500 . ? C6A_2 H6A_2 0.9500 . ? C21A_2 N22A_2 1.301(4) . ? C21A_2 C24A_2 1.496(5) . ? N22A_2 O23A_2 1.400(4) . ? C24A_2 H24A_2 0.9800 . ? C24A_2 H24B_2 0.9800 . ? C24A_2 H24C_2 0.9800 . ? C1B_2 O1B_2 1.337(4) . ? C1B_2 C6B_2 1.395(5) . ? C1B_2 C2B_2 1.410(5) . ? C2B_2 C3B_2 1.397(5) . ? C2B_2 C21B_2 1.480(5) . ? C3B_2 C4B_2 1.374(5) . ? C3B_2 H3B_2 0.9500 . ? C4B_2 C5B_2 1.369(6) . ? C4B_2 H4B_2 0.9500 . ? C5B_2 C6B_2 1.381(5) . ? C5B_2 H5B_2 0.9500 . ? C6B_2 H6B_2 0.9500 . ? C21B_2 N22B_2 1.302(4) . ? C21B_2 C24B_2 1.489(5) . ? N22B_2 O23B_2 1.404(3) . ? C24B_2 H24D_2 0.9800 . ? C24B_2 H24E_2 0.9800 . ? C24B_2 H24F_2 0.9800 . ? C1C_2 C6C_2 1.382(5) . ? C1C_2 C2C_2 1.393(5) . ? C1C_2 C11C_2 1.482(5) . ? C2C_2 C3C_2 1.363(5) . ? C2C_2 H2C_2 0.9500 . ? C3C_2 C4C_2 1.381(6) . ? C3C_2 H3C_2 0.9500 . ? C4C_2 C5C_2 1.386(5) . ? C4C_2 N41C_2 1.463(5) . ? C5C_2 C6C_2 1.389(6) . ? C5C_2 H5C_2 0.9500 . ? C6C_2 H6C_2 0.9500 . ? C11C_2 O13C_2 1.267(4) . ? C11C_2 O12C_2 1.278(4) . ? N41C_2 O43C_2 1.201(5) . ? N41C_2 O42C_2 1.232(5) . ? C1D_2 C2D_2 1.379(6) . ? C1D_2 C6D_2 1.389(6) . ? C1D_2 C11D_2 1.502(6) . ? C2D_2 C3D_2 1.391(6) . ? C2D_2 H2D_2 0.9500 . ? C3D_2 C4D_2 1.363(6) . ? C3D_2 H3D_2 0.9500 . ? C4D_2 C5D_2 1.357(6) . ? C4D_2 N41D_2 1.477(6) . ? C5D_2 C6D_2 1.388(6) . ? C5D_2 H5D_2 0.9500 . ? C6D_2 H6D_2 0.9500 . ? C11D_2 O12D_2 1.260(4) . ? C11D_2 O13D_2 1.267(4) . ? N41D_2 O43D_2 1.207(5) . ? N41D_2 O42D_2 1.223(5) . ? C1E_2 C2E_2 1.367(5) . ? C1E_2 C6E_2 1.374(5) . ? C1E_2 C11E_2 1.501(5) . ? C2E_2 C3E_2 1.371(6) . ? C2E_2 H2E_2 0.9500 . ? C3E_2 C4E_2 1.373(6) . ? C3E_2 H3E_2 0.9500 . ? C4E_2 C5E_2 1.381(5) . ? C4E_2 N41E_2 1.473(5) . ? C5E_2 C6E_2 1.384(5) . ? C5E_2 H5E_2 0.9500 . ? C6E_2 H6E_2 0.9500 . ? C11E_2 O12E_2 1.247(4) . ? C11E_2 O13E_2 1.278(4) . ? N41E_2 O43E_2 1.221(4) . ? N41E_2 O42E_2 1.239(4) . ? C1F_2 C6F_2 1.362(5) . ? C1F_2 C2F_2 1.380(6) . ? C1F_2 C11F_2 1.507(5) . ? C2F_2 C3F_2 1.381(5) . ? C2F_2 H2F_2 0.9500 . ? C3F_2 C4F_2 1.364(6) . ? C3F_2 H3F_2 0.9500 . ? C4F_2 C5F_2 1.363(6) . ? C4F_2 N41F_2 1.491(5) . ? C5F_2 C6F_2 1.401(5) . ? C5F_2 H5F_2 0.9500 . ? C6F_2 H6F_2 0.9500 . ? C11F_2 O13F_2 1.257(5) . ? C11F_2 O12F_2 1.267(5) . ? N41F_2 O43F_2 1.225(4) . ? N41F_2 O42F_2 1.226(5) . ? N1G_2 C6G_2 1.346(5) . ? N1G_2 C2G_2 1.364(5) . ? C2G_2 C3G_2 1.373(6) . ? C2G_2 H2G_2 0.9500 . ? C3G_2 C4G_2 1.380(6) . ? C3G_2 H3G_2 0.9500 . ? C4G_2 C5G_2 1.381(6) . ? C4G_2 H4G_2 0.9500 . ? C5G_2 C6G_2 1.373(5) . ? C5G_2 H5G_2 0.9500 . ? C6G_2 H6G_2 0.9500 . ? N1H_2 C6H_2 1.321(5) . ? N1H_2 C2H_2 1.332(5) . ? C2H_2 C3H_2 1.373(6) . ? C2H_2 H2H_2 0.9500 . ? C3H_2 C4H_2 1.366(7) . ? C3H_2 H3H_2 0.9500 . ? C4H_2 C5H_2 1.380(7) . ? C4H_2 H4H_2 0.9500 . ? C5H_2 C6H_2 1.357(7) . ? C5H_2 H5H_2 0.9500 . ? C6H_2 H6H_2 0.9500 . ? O1I_2 C2I_2 1.424(5) . ? C2I_2 H2I1_2 0.9800 . ? C2I_2 H2I2_2 0.9800 . ? C2I_2 H2I3_2 0.9800 . ? O1J_2 C2J'_2 1.430(7) . ? O1J_2 C2J_2 1.435(7) . ? C2J_2 H2J1_2 0.9800 . ? C2J_2 H2J2_2 0.9800 . ? C2J_2 H2J3_2 0.9800 . ? C2J'_2 H2J4_2 0.9800 . ? C2J'_2 H2J5_2 0.9800 . ? C2J'_2 H2J6_2 0.9800 . ? O1K_2 C2K_2 1.415(5) . ? C2K_2 H2K1_2 0.9800 . ? C2K_2 H2K2_2 0.9800 . ? C2K_2 H2K3_2 0.9800 . ? O1L_2 C2L'_2 1.423(9) . ? O1L_2 C2L_2 1.434(6) . ? C2L_2 H2L1_2 0.9800 . ? C2L_2 H2L2_2 0.9800 . ? C2L_2 H2L3_2 0.9800 . ? C2L'_2 H2L4_2 0.9800 . ? C2L'_2 H2L5_2 0.9800 . ? C2L'_2 H2L6_2 0.9800 . ? Fe1_3 O1A_3 1.885(2) . ? Fe1_3 O1I_3 1.975(3) . ? Fe1_3 O12C_3 2.036(2) . ? Fe1_3 O23B_3 2.069(3) . ? Fe1_3 O134_3 2.076(2) . ? Fe1_3 N22A_3 2.116(3) . ? Fe2_3 O1B_3 1.868(2) . ? Fe2_3 O1J_3 1.982(3) . ? Fe2_3 O12D_3 2.023(2) . ? Fe2_3 O23A_3 2.060(3) . ? Fe2_3 O234_3 2.089(2) . ? Fe2_3 N22B_3 2.098(3) . ? Fe3_3 O1L_3 1.956(3) . ? Fe3_3 O234_3 2.005(2) . ? Fe3_3 O13D_3 2.011(3) . ? Fe3_3 O134_3 2.021(2) . ? Fe3_3 O23A_3 2.052(2) . ? Fe3_3 O13E_3 2.056(2) . ? Fe3_3 Fe4_3 2.9745(7) . ? Fe4_3 O1K_3 1.966(3) . ? Fe4_3 O13C_3 1.998(2) . ? Fe4_3 O234_3 2.004(2) . ? Fe4_3 O134_3 2.005(2) . ? Fe4_3 O13F_3 2.043(2) . ? Fe4_3 O23B_3 2.054(2) . ? Fe5_3 O1J_3 1.960(2) . ? Fe5_3 O1K_3 2.003(2) . ? Fe5_3 O12F_3 2.035(2) . ? Fe5_3 O234_3 2.046(2) . ? Fe5_3 N1G_3 2.167(3) . ? Fe5_3 Cl1_3 2.2911(12) . ? Fe6_3 O1I_3 1.975(2) . ? Fe6_3 O1L_3 2.015(3) . ? Fe6_3 O12E_3 2.023(3) . ? Fe6_3 O134_3 2.041(2) . ? Fe6_3 N1H_3 2.174(3) . ? Fe6_3 Cl2_3 2.2776(12) . ? C1A_3 O1A_3 1.349(4) . ? C1A_3 C6A_3 1.393(6) . ? C1A_3 C2A_3 1.416(6) . ? C2A_3 C3A_3 1.406(5) . ? C2A_3 C21A_3 1.453(6) . ? C3A_3 C4A_3 1.396(6) . ? C3A_3 H3A_3 0.9500 . ? C4A_3 C5A_3 1.356(6) . ? C4A_3 H4A_3 0.9500 . ? C5A_3 C6A_3 1.393(5) . ? C5A_3 H5A_3 0.9500 . ? C6A_3 H6A_3 0.9500 . ? C21A_3 N22A_3 1.292(4) . ? C21A_3 C24A_3 1.527(5) . ? N22A_3 O23A_3 1.404(4) . ? C24A_3 H24A_3 0.9800 . ? C24A_3 H24B_3 0.9800 . ? C24A_3 H24C_3 0.9800 . ? C1B_3 O1B_3 1.322(4) . ? C1B_3 C2B_3 1.393(5) . ? C1B_3 C6B_3 1.405(5) . ? C2B_3 C3B_3 1.414(5) . ? C2B_3 C21B_3 1.472(5) . ? C3B_3 C4B_3 1.365(5) . ? C3B_3 H3B_3 0.9500 . ? C4B_3 C5B_3 1.384(6) . ? C4B_3 H4B_3 0.9500 . ? C5B_3 C6B_3 1.372(5) . ? C5B_3 H5B_3 0.9500 . ? C6B_3 H6B_3 0.9500 . ? C21B_3 N22B_3 1.296(4) . ? C21B_3 C24B_3 1.496(5) . ? N22B_3 O23B_3 1.408(4) . ? C24B_3 H24D_3 0.9800 . ? C24B_3 H24E_3 0.9800 . ? C24B_3 H24F_3 0.9800 . ? C1C_3 C6C_3 1.390(5) . ? C1C_3 C2C_3 1.394(5) . ? C1C_3 C11C_3 1.492(5) . ? C2C_3 C3C_3 1.373(5) . ? C2C_3 H2C_3 0.9500 . ? C3C_3 C4C_3 1.377(6) . ? C3C_3 H3C_3 0.9500 . ? C4C_3 C5C_3 1.369(6) . ? C4C_3 N41C_3 1.492(5) . ? C5C_3 C6C_3 1.392(5) . ? C5C_3 H5C_3 0.9500 . ? C6C_3 H6C_3 0.9500 . ? C11C_3 O12C_3 1.254(4) . ? C11C_3 O13C_3 1.279(4) . ? N41C_3 O42C_3 1.203(5) . ? N41C_3 O43C_3 1.228(5) . ? C1D_3 C6D_3 1.386(5) . ? C1D_3 C2D_3 1.396(5) . ? C1D_3 C11D_3 1.499(5) . ? C2D_3 C3D_3 1.369(5) . ? C2D_3 H2D_3 0.9500 . ? C3D_3 C4D_3 1.388(5) . ? C3D_3 H3D_3 0.9500 . ? C4D_3 C5D_3 1.369(5) . ? C4D_3 N41D_3 1.474(5) . ? C5D_3 C6D_3 1.369(5) . ? C5D_3 H5D_3 0.9500 . ? C6D_3 H6D_3 0.9500 . ? C11D_3 O12D_3 1.258(4) . ? C11D_3 O13D_3 1.266(4) . ? N41D_3 O43D_3 1.223(4) . ? N41D_3 O42D_3 1.223(4) . ? C1E_3 C2E_3 1.376(5) . ? C1E_3 C6E_3 1.383(5) . ? C1E_3 C11E_3 1.501(5) . ? C2E_3 C3E_3 1.389(5) . ? C2E_3 H2E_3 0.9500 . ? C3E_3 C4E_3 1.382(6) . ? C3E_3 H3E_3 0.9500 . ? C4E_3 C5E_3 1.369(6) . ? C4E_3 N41E_3 1.490(5) . ? C5E_3 C6E_3 1.378(6) . ? C5E_3 H5E_3 0.9500 . ? C6E_3 H6E_3 0.9500 . ? C11E_3 O13E_3 1.266(4) . ? C11E_3 O12E_3 1.267(4) . ? N41E_3 O42E_3 1.213(5) . ? N41E_3 O43E_3 1.218(5) . ? C1F_3 C6F_3 1.381(5) . ? C1F_3 C2F_3 1.398(5) . ? C1F_3 C11F_3 1.491(5) . ? C2F_3 C3F_3 1.380(5) . ? C2F_3 H2F_3 0.9500 . ? C3F_3 C4F_3 1.372(6) . ? C3F_3 H3F_3 0.9500 . ? C4F_3 C5F_3 1.378(6) . ? C4F_3 N41F_3 1.487(5) . ? C5F_3 C6F_3 1.387(5) . ? C5F_3 H5F_3 0.9500 . ? C6F_3 H6F_3 0.9500 . ? C11F_3 O12F_3 1.259(4) . ? C11F_3 O13F_3 1.272(4) . ? N41F_3 O43F_3 1.210(5) . ? N41F_3 O42F_3 1.224(5) . ? N1G_3 C2G_3 1.341(5) . ? N1G_3 C6G_3 1.364(5) . ? C2G_3 C3G_3 1.391(6) . ? C2G_3 H2G_3 0.9500 . ? C3G_3 C4G_3 1.376(6) . ? C3G_3 H3G_3 0.9500 . ? C4G_3 C5G_3 1.376(6) . ? C4G_3 H4G_3 0.9500 . ? C5G_3 C6G_3 1.359(6) . ? C5G_3 H5G_3 0.9500 . ? C6G_3 H6G_3 0.9500 . ? N1H_3 C2H_3 1.328(5) . ? N1H_3 C6H_3 1.353(5) . ? C2H_3 C3H_3 1.377(5) . ? C2H_3 H2H_3 0.9500 . ? C3H_3 C4H_3 1.403(6) . ? C3H_3 H3H_3 0.9500 . ? C4H_3 C5H_3 1.360(6) . ? C4H_3 H4H_3 0.9500 . ? C5H_3 C6H_3 1.370(6) . ? C5H_3 H5H_3 0.9500 . ? C6H_3 H6H_3 0.9500 . ? O1I_3 C2I_3 1.431(4) . ? C2I_3 H2I1_3 0.9800 . ? C2I_3 H2I2_3 0.9800 . ? C2I_3 H2I3_3 0.9800 . ? O1J_3 C2J_3 1.420(4) . ? C2J_3 H2J1_3 0.9800 . ? C2J_3 H2J2_3 0.9800 . ? C2J_3 H2J3_3 0.9800 . ? O1K_3 C2K'_3 1.391(7) . ? O1K_3 C2K_3 1.401(7) . ? C2K_3 H2K1_3 0.9800 . ? C2K_3 H2K2_3 0.9800 . ? C2K_3 H2K3_3 0.9800 . ? C2K'_3 H2K4_3 0.9800 . ? C2K'_3 H2K5_3 0.9800 . ? C2K'_3 H2K6_3 0.9800 . ? O1L_3 C2L_3 1.426(6) . ? O1L_3 C2L'_3 1.436(9) . ? C2L_3 H2L1_3 0.9800 . ? C2L_3 H2L2_3 0.9800 . ? C2L_3 H2L3_3 0.9800 . ? C2L'_3 H2L4_3 0.9800 . ? C2L'_3 H2L5_3 0.9800 . ? C2L'_3 H2L6_3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1A_1 Fe1_1 O1I_1 99.21(10) . . ? O1A_1 Fe1_1 O12C_1 92.45(11) . . ? O1I_1 Fe1_1 O12C_1 96.41(10) . . ? O1A_1 Fe1_1 O134_1 175.11(11) . . ? O1I_1 Fe1_1 O134_1 79.58(10) . . ? O12C_1 Fe1_1 O134_1 92.39(10) . . ? O1A_1 Fe1_1 O23B_1 101.16(10) . . ? O1I_1 Fe1_1 O23B_1 159.62(9) . . ? O12C_1 Fe1_1 O23B_1 82.25(10) . . ? O134_1 Fe1_1 O23B_1 80.16(9) . . ? O1A_1 Fe1_1 N22A_1 85.07(11) . . ? O1I_1 Fe1_1 N22A_1 95.54(11) . . ? O12C_1 Fe1_1 N22A_1 168.04(11) . . ? O134_1 Fe1_1 N22A_1 90.32(10) . . ? O23B_1 Fe1_1 N22A_1 86.74(10) . . ? O1B_1 Fe2_1 O1J_1 99.13(11) . . ? O1B_1 Fe2_1 O13D_1 95.56(10) . . ? O1J_1 Fe2_1 O13D_1 91.99(10) . . ? O1B_1 Fe2_1 O23A_1 103.14(10) . . ? O1J_1 Fe2_1 O23A_1 157.60(9) . . ? O13D_1 Fe2_1 O23A_1 83.53(10) . . ? O1B_1 Fe2_1 O234_1 171.45(11) . . ? O1J_1 Fe2_1 O234_1 77.93(9) . . ? O13D_1 Fe2_1 O234_1 92.57(9) . . ? O23A_1 Fe2_1 O234_1 80.35(9) . . ? O1B_1 Fe2_1 N22B_1 83.36(11) . . ? O1J_1 Fe2_1 N22B_1 97.23(11) . . ? O13D_1 Fe2_1 N22B_1 170.77(11) . . ? O23A_1 Fe2_1 N22B_1 87.78(10) . . ? O234_1 Fe2_1 N22B_1 89.03(10) . . ? O1K_1 Fe3_1 O12D_1 99.27(11) . . ? O1K_1 Fe3_1 O234_1 165.04(10) . . ? O12D_1 Fe3_1 O234_1 95.04(10) . . ? O1K_1 Fe3_1 O134_1 81.65(10) . . ? O12D_1 Fe3_1 O134_1 177.42(9) . . ? O234_1 Fe3_1 O134_1 83.88(10) . . ? O1K_1 Fe3_1 O12F_1 90.37(10) . . ? O12D_1 Fe3_1 O12F_1 87.71(10) . . ? O234_1 Fe3_1 O12F_1 94.55(10) . . ? O134_1 Fe3_1 O12F_1 94.70(10) . . ? O1K_1 Fe3_1 O23A_1 94.06(10) . . ? O12D_1 Fe3_1 O23A_1 85.38(9) . . ? O234_1 Fe3_1 O23A_1 82.72(9) . . ? O134_1 Fe3_1 O23A_1 92.15(9) . . ? O12F_1 Fe3_1 O23A_1 172.32(10) . . ? O1L_1 Fe4_1 O13C_1 99.76(10) . . ? O1L_1 Fe4_1 O12E_1 90.60(10) . . ? O13C_1 Fe4_1 O12E_1 85.71(10) . . ? O1L_1 Fe4_1 O234_1 80.08(10) . . ? O13C_1 Fe4_1 O234_1 177.67(10) . . ? O12E_1 Fe4_1 O234_1 96.62(10) . . ? O1L_1 Fe4_1 O134_1 163.19(10) . . ? O13C_1 Fe4_1 O134_1 96.51(10) . . ? O12E_1 Fe4_1 O134_1 94.83(10) . . ? O234_1 Fe4_1 O134_1 83.49(10) . . ? O1L_1 Fe4_1 O23B_1 94.19(10) . . ? O13C_1 Fe4_1 O23B_1 85.50(10) . . ? O12E_1 Fe4_1 O23B_1 170.59(10) . . ? O234_1 Fe4_1 O23B_1 92.18(9) . . ? O134_1 Fe4_1 O23B_1 82.84(9) . . ? O1I_1 Fe5_1 O1K_1 96.46(10) . . ? O1I_1 Fe5_1 O134_1 79.42(10) . . ? O1K_1 Fe5_1 O134_1 79.41(10) . . ? O1I_1 Fe5_1 O13F_1 168.31(11) . . ? O1K_1 Fe5_1 O13F_1 87.87(10) . . ? O134_1 Fe5_1 O13F_1 90.77(9) . . ? O1I_1 Fe5_1 N1G_1 88.45(11) . . ? O1K_1 Fe5_1 N1G_1 169.54(11) . . ? O134_1 Fe5_1 N1G_1 92.49(11) . . ? O13F_1 Fe5_1 N1G_1 85.62(11) . . ? O1I_1 Fe5_1 Cl1_1 96.26(8) . . ? O1K_1 Fe5_1 Cl1_1 95.63(8) . . ? O134_1 Fe5_1 Cl1_1 172.92(7) . . ? O13F_1 Fe5_1 Cl1_1 94.10(7) . . ? N1G_1 Fe5_1 Cl1_1 93.00(9) . . ? O1J_1 Fe6_1 O1L_1 95.99(10) . . ? O1J_1 Fe6_1 O234_1 79.57(9) . . ? O1L_1 Fe6_1 O234_1 79.03(10) . . ? O1J_1 Fe6_1 O13E_1 169.46(11) . . ? O1L_1 Fe6_1 O13E_1 87.68(10) . . ? O234_1 Fe6_1 O13E_1 91.49(9) . . ? O1J_1 Fe6_1 N1H_1 91.46(11) . . ? O1L_1 Fe6_1 N1H_1 168.90(11) . . ? O234_1 Fe6_1 N1H_1 94.31(11) . . ? O13E_1 Fe6_1 N1H_1 83.60(11) . . ? O1J_1 Fe6_1 Cl2_1 97.21(8) . . ? O1L_1 Fe6_1 Cl2_1 95.88(8) . . ? O234_1 Fe6_1 Cl2_1 173.58(7) . . ? O13E_1 Fe6_1 Cl2_1 92.22(8) . . ? N1H_1 Fe6_1 Cl2_1 91.31(9) . . ? Fe3_1 O134_1 Fe4_1 95.73(10) . . ? Fe3_1 O134_1 Fe5_1 94.68(10) . . ? Fe4_1 O134_1 Fe5_1 156.32(13) . . ? Fe3_1 O134_1 Fe1_1 115.63(11) . . ? Fe4_1 O134_1 Fe1_1 96.92(10) . . ? Fe5_1 O134_1 Fe1_1 97.63(10) . . ? Fe3_1 O234_1 Fe4_1 95.89(10) . . ? Fe3_1 O234_1 Fe6_1 153.68(12) . . ? Fe4_1 O234_1 Fe6_1 96.48(10) . . ? Fe3_1 O234_1 Fe2_1 96.77(10) . . ? Fe4_1 O234_1 Fe2_1 115.46(11) . . ? Fe6_1 O234_1 Fe2_1 98.73(9) . . ? O1A_1 C1A_1 C2A_1 123.2(3) . . ? O1A_1 C1A_1 C6A_1 116.5(4) . . ? C2A_1 C1A_1 C6A_1 120.3(4) . . ? C1A_1 O1A_1 Fe1_1 128.2(2) . . ? C3A_1 C2A_1 C1A_1 118.0(4) . . ? C3A_1 C2A_1 C21A_1 119.1(4) . . ? C1A_1 C2A_1 C21A_1 122.8(4) . . ? C4A_1 C3A_1 C2A_1 121.1(4) . . ? C4A_1 C3A_1 H3A_1 119.5 . . ? C2A_1 C3A_1 H3A_1 119.5 . . ? C5A_1 C4A_1 C3A_1 120.3(5) . . ? C5A_1 C4A_1 H4A_1 119.9 . . ? C3A_1 C4A_1 H4A_1 119.9 . . ? C4A_1 C5A_1 C6A_1 120.2(4) . . ? C4A_1 C5A_1 H5A_1 119.9 . . ? C6A_1 C5A_1 H5A_1 119.9 . . ? C5A_1 C6A_1 C1A_1 119.9(4) . . ? C5A_1 C6A_1 H6A_1 120.0 . . ? C1A_1 C6A_1 H6A_1 120.0 . . ? N22A_1 C21A_1 C2A_1 119.0(4) . . ? N22A_1 C21A_1 C24A_1 120.6(4) . . ? C2A_1 C21A_1 C24A_1 120.4(3) . . ? C21A_1 N22A_1 O23A_1 114.5(3) . . ? C21A_1 N22A_1 Fe1_1 129.6(3) . . ? O23A_1 N22A_1 Fe1_1 115.8(2) . . ? N22A_1 O23A_1 Fe3_1 116.65(18) . . ? N22A_1 O23A_1 Fe2_1 120.32(18) . . ? Fe3_1 O23A_1 Fe2_1 95.74(10) . . ? C21A_1 C24A_1 H24A_1 109.5 . . ? C21A_1 C24A_1 H24B_1 109.5 . . ? H24A_1 C24A_1 H24B_1 109.5 . . ? C21A_1 C24A_1 H24C_1 109.5 . . ? H24A_1 C24A_1 H24C_1 109.5 . . ? H24B_1 C24A_1 H24C_1 109.5 . . ? O1B_1 C1B_1 C6B_1 117.5(3) . . ? O1B_1 C1B_1 C2B_1 123.0(3) . . ? C6B_1 C1B_1 C2B_1 119.4(3) . . ? C1B_1 O1B_1 Fe2_1 130.3(2) . . ? C3B_1 C2B_1 C1B_1 118.4(3) . . ? C3B_1 C2B_1 C21B_1 120.1(3) . . ? C1B_1 C2B_1 C21B_1 121.4(3) . . ? C4B_1 C3B_1 C2B_1 121.5(4) . . ? C4B_1 C3B_1 H3B_1 119.2 . . ? C2B_1 C3B_1 H3B_1 119.2 . . ? C5B_1 C4B_1 C3B_1 119.6(4) . . ? C5B_1 C4B_1 H4B_1 120.2 . . ? C3B_1 C4B_1 H4B_1 120.2 . . ? C4B_1 C5B_1 C6B_1 121.2(4) . . ? C4B_1 C5B_1 H5B_1 119.4 . . ? C6B_1 C5B_1 H5B_1 119.4 . . ? C1B_1 C6B_1 C5B_1 119.8(4) . . ? C1B_1 C6B_1 H6B_1 120.1 . . ? C5B_1 C6B_1 H6B_1 120.1 . . ? N22B_1 C21B_1 C2B_1 119.3(3) . . ? N22B_1 C21B_1 C24B_1 119.9(3) . . ? C2B_1 C21B_1 C24B_1 120.7(3) . . ? C21B_1 N22B_1 O23B_1 113.6(3) . . ? C21B_1 N22B_1 Fe2_1 130.3(2) . . ? O23B_1 N22B_1 Fe2_1 116.14(19) . . ? N22B_1 O23B_1 Fe4_1 116.02(18) . . ? N22B_1 O23B_1 Fe1_1 121.48(19) . . ? Fe4_1 O23B_1 Fe1_1 95.68(9) . . ? C21B_1 C24B_1 H24D_1 109.5 . . ? C21B_1 C24B_1 H24E_1 109.5 . . ? H24D_1 C24B_1 H24E_1 109.5 . . ? C21B_1 C24B_1 H24F_1 109.5 . . ? H24D_1 C24B_1 H24F_1 109.5 . . ? H24E_1 C24B_1 H24F_1 109.5 . . ? C2C_1 C1C_1 C6C_1 119.4(4) . . ? C2C_1 C1C_1 C11C_1 120.0(3) . . ? C6C_1 C1C_1 C11C_1 120.6(3) . . ? C3C_1 C2C_1 C1C_1 120.5(4) . . ? C3C_1 C2C_1 H2C_1 119.8 . . ? C1C_1 C2C_1 H2C_1 119.8 . . ? C4C_1 C3C_1 C2C_1 118.1(4) . . ? C4C_1 C3C_1 H3C_1 121.0 . . ? C2C_1 C3C_1 H3C_1 121.0 . . ? C3C_1 C4C_1 C5C_1 123.3(4) . . ? C3C_1 C4C_1 N41C_1 118.5(4) . . ? C5C_1 C4C_1 N41C_1 118.2(4) . . ? C6C_1 C5C_1 C4C_1 118.2(4) . . ? C6C_1 C5C_1 H5C_1 120.9 . . ? C4C_1 C5C_1 H5C_1 120.9 . . ? C5C_1 C6C_1 C1C_1 120.5(4) . . ? C5C_1 C6C_1 H6C_1 119.7 . . ? C1C_1 C6C_1 H6C_1 119.7 . . ? O12C_1 C11C_1 O13C_1 124.9(3) . . ? O12C_1 C11C_1 C1C_1 117.9(3) . . ? O13C_1 C11C_1 C1C_1 117.2(3) . . ? C11C_1 O12C_1 Fe1_1 131.1(2) . . ? C11C_1 O13C_1 Fe4_1 126.8(2) . . ? O43C_1 N41C_1 O42C_1 124.2(4) . . ? O43C_1 N41C_1 C4C_1 118.0(3) . . ? O42C_1 N41C_1 C4C_1 117.8(4) . . ? C6D_1 C1D_1 C2D_1 120.4(3) . . ? C6D_1 C1D_1 C11D_1 120.3(3) . . ? C2D_1 C1D_1 C11D_1 119.3(3) . . ? C3D_1 C2D_1 C1D_1 120.1(3) . . ? C3D_1 C2D_1 H2D_1 120.0 . . ? C1D_1 C2D_1 H2D_1 120.0 . . ? C4D_1 C3D_1 C2D_1 118.8(4) . . ? C4D_1 C3D_1 H3D_1 120.6 . . ? C2D_1 C3D_1 H3D_1 120.6 . . ? C3D_1 C4D_1 C5D_1 122.0(4) . . ? C3D_1 C4D_1 N41D_1 119.9(4) . . ? C5D_1 C4D_1 N41D_1 118.1(4) . . ? C6D_1 C5D_1 C4D_1 118.9(4) . . ? C6D_1 C5D_1 H5D_1 120.5 . . ? C4D_1 C5D_1 H5D_1 120.5 . . ? C5D_1 C6D_1 C1D_1 119.9(4) . . ? C5D_1 C6D_1 H6D_1 120.1 . . ? C1D_1 C6D_1 H6D_1 120.1 . . ? O13D_1 C11D_1 O12D_1 124.1(3) . . ? O13D_1 C11D_1 C1D_1 118.3(3) . . ? O12D_1 C11D_1 C1D_1 117.6(3) . . ? C11D_1 O12D_1 Fe3_1 128.8(2) . . ? C11D_1 O13D_1 Fe2_1 130.1(2) . . ? O43D_1 N41D_1 O42D_1 122.8(4) . . ? O43D_1 N41D_1 C4D_1 119.2(4) . . ? O42D_1 N41D_1 C4D_1 118.0(4) . . ? C2E_1 C1E_1 C6E_1 119.7(3) . . ? C2E_1 C1E_1 C11E_1 120.5(3) . . ? C6E_1 C1E_1 C11E_1 119.6(3) . . ? C1E_1 C2E_1 C3E_1 121.5(4) . . ? C1E_1 C2E_1 H2E_1 119.3 . . ? C3E_1 C2E_1 H2E_1 119.3 . . ? C4E_1 C3E_1 C2E_1 117.1(4) . . ? C4E_1 C3E_1 H3E_1 121.5 . . ? C2E_1 C3E_1 H3E_1 121.5 . . ? C3E_1 C4E_1 C5E_1 124.1(4) . . ? C3E_1 C4E_1 N41E_1 118.9(4) . . ? C5E_1 C4E_1 N41E_1 116.8(4) . . ? C4E_1 C5E_1 C6E_1 117.7(4) . . ? C4E_1 C5E_1 H5E_1 121.2 . . ? C6E_1 C5E_1 H5E_1 121.2 . . ? C1E_1 C6E_1 C5E_1 119.9(4) . . ? C1E_1 C6E_1 H6E_1 120.0 . . ? C5E_1 C6E_1 H6E_1 120.0 . . ? O13E_1 C11E_1 O12E_1 125.4(3) . . ? O13E_1 C11E_1 C1E_1 117.7(3) . . ? O12E_1 C11E_1 C1E_1 116.9(3) . . ? C11E_1 O12E_1 Fe4_1 126.2(2) . . ? C11E_1 O13E_1 Fe6_1 129.3(2) . . ? O42'_1 N41E_1 O42E_1 23(2) . . ? O42'_1 N41E_1 O43E_1 107.3(13) . . ? O42E_1 N41E_1 O43E_1 122.9(8) . . ? O42'_1 N41E_1 O43'_1 120.9(17) . . ? O42E_1 N41E_1 O43'_1 113.6(11) . . ? O43E_1 N41E_1 O43'_1 54.0(5) . . ? O42'_1 N41E_1 C4E_1 122.8(15) . . ? O42E_1 N41E_1 C4E_1 117.2(8) . . ? O43E_1 N41E_1 C4E_1 117.7(5) . . ? O43'_1 N41E_1 C4E_1 113.9(5) . . ? C6F_1 C1F_1 C2F_1 119.2(4) . . ? C6F_1 C1F_1 C11F_1 120.0(3) . . ? C2F_1 C1F_1 C11F_1 120.7(3) . . ? C1F_1 C2F_1 C3F_1 127.7(5) . . ? C1F_1 C2F_1 C3F"_1 114.3(5) . . ? C3F_1 C2F_1 C3F"_1 23.7(5) . . ? C1F_1 C2F_1 H2F_1 116.2 . . ? C3F_1 C2F_1 H2F_1 116.2 . . ? C3F"_1 C2F_1 H2F_1 124.9 . . ? C4F_1 C3F_1 C2F_1 111.7(7) . . ? C4F_1 C3F_1 H3F_1 124.1 . . ? C2F_1 C3F_1 H3F_1 124.1 . . ? C3F_1 C4F_1 C5F_1 122.1(7) . . ? C3F_1 C4F_1 N41F_1 119.8(7) . . ? C5F_1 C4F_1 N41F_1 117.7(7) . . ? C4F_1 C5F_1 C6F_1 122.1(7) . . ? C4F_1 C5F_1 H5F_1 118.9 . . ? C6F_1 C5F_1 H5F_1 118.9 . . ? O42F_1 N41F_1 O43F_1 129.9(7) . . ? O42F_1 N41F_1 C4F_1 114.7(7) . . ? O43F_1 N41F_1 C4F_1 115.3(7) . . ? C4F"_1 C3F"_1 C2F_1 121.9(7) . . ? C4F"_1 C3F"_1 H3F"_1 119.0 . . ? C2F_1 C3F"_1 H3F"_1 119.0 . . ? C3F"_1 C4F"_1 C5F"_1 123.7(7) . . ? C3F"_1 C4F"_1 N41"_1 117.9(7) . . ? C5F"_1 C4F"_1 N41"_1 118.2(6) . . ? C6F_1 C5F"_1 C4F"_1 110.0(7) . . ? C6F_1 C5F"_1 H5F"_1 125.0 . . ? C4F"_1 C5F"_1 H5F"_1 125.0 . . ? O42"_1 N41"_1 O43"_1 121.2(8) . . ? O42"_1 N41"_1 C4F"_1 120.7(8) . . ? O43"_1 N41"_1 C4F"_1 118.0(7) . . ? C5F"_1 C6F_1 C1F_1 127.8(5) . . ? C5F"_1 C6F_1 C5F_1 15.1(6) . . ? C1F_1 C6F_1 C5F_1 114.2(5) . . ? C5F"_1 C6F_1 H6F_1 108.9 . . ? C1F_1 C6F_1 H6F_1 122.9 . . ? C5F_1 C6F_1 H6F_1 122.9 . . ? O13F_1 C11F_1 O12F_1 125.9(3) . . ? O13F_1 C11F_1 C1F_1 118.3(3) . . ? O12F_1 C11F_1 C1F_1 115.8(3) . . ? C11F_1 O12F_1 Fe3_1 125.4(2) . . ? C11F_1 O13F_1 Fe5_1 129.0(2) . . ? C6G_1 N1G_1 C2G_1 117.9(4) . . ? C6G_1 N1G_1 Fe5_1 122.2(3) . . ? C2G_1 N1G_1 Fe5_1 119.9(3) . . ? N1G_1 C2G_1 C3G_1 122.4(4) . . ? N1G_1 C2G_1 H2G_1 118.8 . . ? C3G_1 C2G_1 H2G_1 118.8 . . ? C4G_1 C3G_1 C2G_1 119.6(4) . . ? C4G_1 C3G_1 H3G_1 120.2 . . ? C2G_1 C3G_1 H3G_1 120.2 . . ? C3G_1 C4G_1 C5G_1 118.7(4) . . ? C3G_1 C4G_1 H4G_1 120.7 . . ? C5G_1 C4G_1 H4G_1 120.7 . . ? C4G_1 C5G_1 C6G_1 119.5(4) . . ? C4G_1 C5G_1 H5G_1 120.3 . . ? C6G_1 C5G_1 H5G_1 120.3 . . ? N1G_1 C6G_1 C5G_1 121.9(4) . . ? N1G_1 C6G_1 H6G_1 119.0 . . ? C5G_1 C6G_1 H6G_1 119.0 . . ? C2H_1 N1H_1 C6H_1 117.2(3) . . ? C2H_1 N1H_1 Fe6_1 121.7(3) . . ? C6H_1 N1H_1 Fe6_1 121.1(3) . . ? N1H_1 C2H_1 C3H_1 122.6(4) . . ? N1H_1 C2H_1 H2H_1 118.7 . . ? C3H_1 C2H_1 H2H_1 118.7 . . ? C2H_1 C3H_1 C4H_1 119.5(4) . . ? C2H_1 C3H_1 H3H_1 120.2 . . ? C4H_1 C3H_1 H3H_1 120.2 . . ? C5H_1 C4H_1 C3H_1 118.4(4) . . ? C5H_1 C4H_1 H4H_1 120.8 . . ? C3H_1 C4H_1 H4H_1 120.8 . . ? C4H_1 C5H_1 C6H_1 119.1(4) . . ? C4H_1 C5H_1 H5H_1 120.4 . . ? C6H_1 C5H_1 H5H_1 120.4 . . ? N1H_1 C6H_1 C5H_1 123.1(4) . . ? N1H_1 C6H_1 H6H_1 118.4 . . ? C5H_1 C6H_1 H6H_1 118.4 . . ? C2I_1 O1I_1 Fe1_1 126.6(2) . . ? C2I_1 O1I_1 Fe5_1 126.5(2) . . ? Fe1_1 O1I_1 Fe5_1 103.36(11) . . ? O1I_1 C2I_1 H2I1_1 109.5 . . ? O1I_1 C2I_1 H2I2_1 109.5 . . ? H2I1_1 C2I_1 H2I2_1 109.5 . . ? O1I_1 C2I_1 H2I3_1 109.5 . . ? H2I1_1 C2I_1 H2I3_1 109.5 . . ? H2I2_1 C2I_1 H2I3_1 109.5 . . ? C2J_1 O1J_1 Fe6_1 132.5(2) . . ? C2J_1 O1J_1 Fe2_1 122.0(2) . . ? Fe6_1 O1J_1 Fe2_1 103.78(10) . . ? O1J_1 C2J_1 H2J1_1 109.5 . . ? O1J_1 C2J_1 H2J2_1 109.5 . . ? H2J1_1 C2J_1 H2J2_1 109.5 . . ? O1J_1 C2J_1 H2J3_1 109.5 . . ? H2J1_1 C2J_1 H2J3_1 109.5 . . ? H2J2_1 C2J_1 H2J3_1 109.5 . . ? C2K_1 O1K_1 Fe3_1 127.1(2) . . ? C2K_1 O1K_1 Fe5_1 133.7(3) . . ? Fe3_1 O1K_1 Fe5_1 98.77(12) . . ? O1K_1 C2K_1 H2K1_1 109.5 . . ? O1K_1 C2K_1 H2K2_1 109.5 . . ? H2K1_1 C2K_1 H2K2_1 109.5 . . ? O1K_1 C2K_1 H2K3_1 109.5 . . ? H2K1_1 C2K_1 H2K3_1 109.5 . . ? H2K2_1 C2K_1 H2K3_1 109.5 . . ? C2L_1 O1L_1 Fe4_1 124.3(2) . . ? C2L_1 O1L_1 Fe6_1 127.1(2) . . ? Fe4_1 O1L_1 Fe6_1 97.91(11) . . ? O1L_1 C2L_1 H2L1_1 109.5 . . ? O1L_1 C2L_1 H2L2_1 109.5 . . ? H2L1_1 C2L_1 H2L2_1 109.5 . . ? O1L_1 C2L_1 H2L3_1 109.5 . . ? H2L1_1 C2L_1 H2L3_1 109.5 . . ? H2L2_1 C2L_1 H2L3_1 109.5 . . ? O1A_2 Fe1_2 O1I_2 99.11(10) . . ? O1A_2 Fe1_2 O13C_2 92.99(10) . . ? O1I_2 Fe1_2 O13C_2 94.64(10) . . ? O1A_2 Fe1_2 O134_2 174.71(10) . . ? O1I_2 Fe1_2 O134_2 79.31(10) . . ? O13C_2 Fe1_2 O134_2 92.18(10) . . ? O1A_2 Fe1_2 O23B_2 101.37(10) . . ? O1I_2 Fe1_2 O23B_2 159.52(10) . . ? O13C_2 Fe1_2 O23B_2 84.11(10) . . ? O134_2 Fe1_2 O23B_2 80.31(10) . . ? O1A_2 Fe1_2 N22A_2 84.12(11) . . ? O1I_2 Fe1_2 N22A_2 97.35(11) . . ? O13C_2 Fe1_2 N22A_2 167.97(10) . . ? O134_2 Fe1_2 N22A_2 91.05(11) . . ? O23B_2 Fe1_2 N22A_2 85.02(10) . . ? O1B_2 Fe2_2 O1J_2 99.28(11) . . ? O1B_2 Fe2_2 O13D_2 91.69(11) . . ? O1J_2 Fe2_2 O13D_2 95.81(11) . . ? O1B_2 Fe2_2 O234_2 174.79(11) . . ? O1J_2 Fe2_2 O234_2 78.58(10) . . ? O13D_2 Fe2_2 O234_2 93.25(10) . . ? O1B_2 Fe2_2 O23A_2 102.86(10) . . ? O1J_2 Fe2_2 O23A_2 157.81(10) . . ? O13D_2 Fe2_2 O23A_2 82.03(10) . . ? O234_2 Fe2_2 O23A_2 79.49(9) . . ? O1B_2 Fe2_2 N22B_2 84.73(11) . . ? O1J_2 Fe2_2 N22B_2 97.58(11) . . ? O13D_2 Fe2_2 N22B_2 166.53(11) . . ? O234_2 Fe2_2 N22B_2 90.82(10) . . ? O23A_2 Fe2_2 N22B_2 86.10(10) . . ? O1K_2 Fe3_2 O12D_2 98.63(11) . . ? O1K_2 Fe3_2 O134_2 81.58(10) . . ? O12D_2 Fe3_2 O134_2 175.61(10) . . ? O1K_2 Fe3_2 O234_2 165.33(11) . . ? O12D_2 Fe3_2 O234_2 95.01(11) . . ? O134_2 Fe3_2 O234_2 84.41(10) . . ? O1K_2 Fe3_2 O13E_2 90.44(10) . . ? O12D_2 Fe3_2 O13E_2 88.90(10) . . ? O134_2 Fe3_2 O13E_2 95.48(10) . . ? O234_2 Fe3_2 O13E_2 95.22(10) . . ? O1K_2 Fe3_2 O23A_2 94.05(10) . . ? O12D_2 Fe3_2 O23A_2 84.32(10) . . ? O134_2 Fe3_2 O23A_2 91.29(10) . . ? O234_2 Fe3_2 O23A_2 81.90(9) . . ? O13E_2 Fe3_2 O23A_2 172.36(11) . . ? O1K_2 Fe3_2 Fe4_2 124.06(8) . . ? O12D_2 Fe3_2 Fe4_2 137.29(8) . . ? O134_2 Fe3_2 Fe4_2 42.59(7) . . ? O234_2 Fe3_2 Fe4_2 42.42(7) . . ? O13E_2 Fe3_2 Fe4_2 91.65(7) . . ? O23A_2 Fe3_2 Fe4_2 90.95(7) . . ? O1L_2 Fe4_2 O12C_2 99.05(11) . . ? O1L_2 Fe4_2 O234_2 81.05(10) . . ? O12C_2 Fe4_2 O234_2 177.22(10) . . ? O1L_2 Fe4_2 O134_2 165.27(11) . . ? O12C_2 Fe4_2 O134_2 95.57(10) . . ? O234_2 Fe4_2 O134_2 84.25(10) . . ? O1L_2 Fe4_2 O23B_2 96.73(10) . . ? O12C_2 Fe4_2 O23B_2 85.47(10) . . ? O234_2 Fe4_2 O23B_2 91.76(10) . . ? O134_2 Fe4_2 O23B_2 82.60(9) . . ? O1L_2 Fe4_2 O12F_2 89.21(10) . . ? O12C_2 Fe4_2 O12F_2 87.84(11) . . ? O234_2 Fe4_2 O12F_2 94.94(10) . . ? O134_2 Fe4_2 O12F_2 93.14(10) . . ? O23B_2 Fe4_2 O12F_2 171.67(11) . . ? O1L_2 Fe4_2 Fe3_2 123.21(8) . . ? O12C_2 Fe4_2 Fe3_2 137.64(7) . . ? O234_2 Fe4_2 Fe3_2 42.51(7) . . ? O134_2 Fe4_2 Fe3_2 42.33(7) . . ? O23B_2 Fe4_2 Fe3_2 91.73(7) . . ? O12F_2 Fe4_2 Fe3_2 89.88(8) . . ? O1I_2 Fe5_2 O1K_2 96.81(10) . . ? O1I_2 Fe5_2 O12E_2 168.41(11) . . ? O1K_2 Fe5_2 O12E_2 86.57(11) . . ? O1I_2 Fe5_2 O134_2 79.39(10) . . ? O1K_2 Fe5_2 O134_2 79.32(10) . . ? O12E_2 Fe5_2 O134_2 90.41(10) . . ? O1I_2 Fe5_2 N1G_2 92.96(11) . . ? O1K_2 Fe5_2 N1G_2 166.54(12) . . ? O12E_2 Fe5_2 N1G_2 82.10(11) . . ? O134_2 Fe5_2 N1G_2 93.48(11) . . ? O1I_2 Fe5_2 Cl1_2 95.74(8) . . ? O1K_2 Fe5_2 Cl1_2 95.03(8) . . ? O12E_2 Fe5_2 Cl1_2 94.99(8) . . ? O134_2 Fe5_2 Cl1_2 171.96(8) . . ? N1G_2 Fe5_2 Cl1_2 93.16(9) . . ? O1J_2 Fe6_2 O1L_2 96.42(11) . . ? O1J_2 Fe6_2 O234_2 78.98(10) . . ? O1L_2 Fe6_2 O234_2 79.59(10) . . ? O1J_2 Fe6_2 O13F_2 168.16(11) . . ? O1L_2 Fe6_2 O13F_2 87.84(11) . . ? O234_2 Fe6_2 O13F_2 90.99(10) . . ? O1J_2 Fe6_2 N1H_2 89.13(12) . . ? O1L_2 Fe6_2 N1H_2 170.29(11) . . ? O234_2 Fe6_2 N1H_2 93.72(11) . . ? O13F_2 Fe6_2 N1H_2 85.22(12) . . ? O1J_2 Fe6_2 Cl2_2 96.69(8) . . ? O1L_2 Fe6_2 Cl2_2 94.52(8) . . ? O234_2 Fe6_2 Cl2_2 172.16(8) . . ? O13F_2 Fe6_2 Cl2_2 93.97(8) . . ? N1H_2 Fe6_2 Cl2_2 92.73(9) . . ? Fe3_2 O134_2 Fe4_2 95.07(10) . . ? Fe3_2 O134_2 Fe1_2 116.07(11) . . ? Fe4_2 O134_2 Fe1_2 96.71(10) . . ? Fe3_2 O134_2 Fe5_2 95.21(10) . . ? Fe4_2 O134_2 Fe5_2 156.24(13) . . ? Fe1_2 O134_2 Fe5_2 97.89(10) . . ? Fe4_2 O234_2 Fe3_2 95.07(10) . . ? Fe4_2 O234_2 Fe6_2 95.56(10) . . ? Fe3_2 O234_2 Fe6_2 153.37(13) . . ? Fe4_2 O234_2 Fe2_2 115.30(12) . . ? Fe3_2 O234_2 Fe2_2 98.27(10) . . ? Fe6_2 O234_2 Fe2_2 99.11(10) . . ? O1A_2 C1A_2 C6A_2 117.7(3) . . ? O1A_2 C1A_2 C2A_2 123.2(3) . . ? C6A_2 C1A_2 C2A_2 119.1(3) . . ? C1A_2 O1A_2 Fe1_2 135.6(2) . . ? C1A_2 C2A_2 C3A_2 117.1(4) . . ? C1A_2 C2A_2 C21A_2 123.8(3) . . ? C3A_2 C2A_2 C21A_2 119.0(4) . . ? C4A_2 C3A_2 C2A_2 121.7(4) . . ? C4A_2 C3A_2 H3A_2 119.1 . . ? C2A_2 C3A_2 H3A_2 119.1 . . ? C5A_2 C4A_2 C3A_2 120.3(4) . . ? C5A_2 C4A_2 H4A_2 119.8 . . ? C3A_2 C4A_2 H4A_2 119.8 . . ? C4A_2 C5A_2 C6A_2 119.4(4) . . ? C4A_2 C5A_2 H5A_2 120.3 . . ? C6A_2 C5A_2 H5A_2 120.3 . . ? C5A_2 C6A_2 C1A_2 122.1(4) . . ? C5A_2 C6A_2 H6A_2 118.9 . . ? C1A_2 C6A_2 H6A_2 118.9 . . ? N22A_2 C21A_2 C2A_2 119.1(3) . . ? N22A_2 C21A_2 C24A_2 120.6(4) . . ? C2A_2 C21A_2 C24A_2 120.3(3) . . ? C21A_2 N22A_2 O23A_2 114.2(3) . . ? C21A_2 N22A_2 Fe1_2 131.6(3) . . ? O23A_2 N22A_2 Fe1_2 114.2(2) . . ? N22A_2 O23A_2 Fe3_2 119.72(19) . . ? N22A_2 O23A_2 Fe2_2 117.63(18) . . ? Fe3_2 O23A_2 Fe2_2 96.00(10) . . ? C21A_2 C24A_2 H24A_2 109.5 . . ? C21A_2 C24A_2 H24B_2 109.5 . . ? H24A_2 C24A_2 H24B_2 109.5 . . ? C21A_2 C24A_2 H24C_2 109.5 . . ? H24A_2 C24A_2 H24C_2 109.5 . . ? H24B_2 C24A_2 H24C_2 109.5 . . ? O1B_2 C1B_2 C6B_2 118.2(4) . . ? O1B_2 C1B_2 C2B_2 122.6(3) . . ? C6B_2 C1B_2 C2B_2 119.2(3) . . ? C1B_2 O1B_2 Fe2_2 131.8(2) . . ? C3B_2 C2B_2 C1B_2 117.6(3) . . ? C3B_2 C2B_2 C21B_2 118.8(4) . . ? C1B_2 C2B_2 C21B_2 123.5(3) . . ? C4B_2 C3B_2 C2B_2 122.4(4) . . ? C4B_2 C3B_2 H3B_2 118.8 . . ? C2B_2 C3B_2 H3B_2 118.8 . . ? C5B_2 C4B_2 C3B_2 119.5(4) . . ? C5B_2 C4B_2 H4B_2 120.3 . . ? C3B_2 C4B_2 H4B_2 120.3 . . ? C4B_2 C5B_2 C6B_2 120.1(4) . . ? C4B_2 C5B_2 H5B_2 119.9 . . ? C6B_2 C5B_2 H5B_2 119.9 . . ? C5B_2 C6B_2 C1B_2 121.1(4) . . ? C5B_2 C6B_2 H6B_2 119.4 . . ? C1B_2 C6B_2 H6B_2 119.4 . . ? N22B_2 C21B_2 C2B_2 118.4(3) . . ? N22B_2 C21B_2 C24B_2 122.4(3) . . ? C2B_2 C21B_2 C24B_2 119.1(3) . . ? C21B_2 N22B_2 O23B_2 114.3(3) . . ? C21B_2 N22B_2 Fe2_2 131.2(3) . . ? O23B_2 N22B_2 Fe2_2 114.1(2) . . ? N22B_2 O23B_2 Fe4_2 118.6(2) . . ? N22B_2 O23B_2 Fe1_2 120.31(18) . . ? Fe4_2 O23B_2 Fe1_2 95.91(10) . . ? C21B_2 C24B_2 H24D_2 109.5 . . ? C21B_2 C24B_2 H24E_2 109.5 . . ? H24D_2 C24B_2 H24E_2 109.5 . . ? C21B_2 C24B_2 H24F_2 109.5 . . ? H24D_2 C24B_2 H24F_2 109.5 . . ? H24E_2 C24B_2 H24F_2 109.5 . . ? C6C_2 C1C_2 C2C_2 119.9(4) . . ? C6C_2 C1C_2 C11C_2 120.2(3) . . ? C2C_2 C1C_2 C11C_2 119.8(4) . . ? C3C_2 C2C_2 C1C_2 120.3(4) . . ? C3C_2 C2C_2 H2C_2 119.9 . . ? C1C_2 C2C_2 H2C_2 119.9 . . ? C2C_2 C3C_2 C4C_2 118.9(4) . . ? C2C_2 C3C_2 H3C_2 120.6 . . ? C4C_2 C3C_2 H3C_2 120.6 . . ? C3C_2 C4C_2 C5C_2 122.8(4) . . ? C3C_2 C4C_2 N41C_2 119.2(4) . . ? C5C_2 C4C_2 N41C_2 118.0(4) . . ? C4C_2 C5C_2 C6C_2 117.1(4) . . ? C4C_2 C5C_2 H5C_2 121.4 . . ? C6C_2 C5C_2 H5C_2 121.4 . . ? C1C_2 C6C_2 C5C_2 121.0(4) . . ? C1C_2 C6C_2 H6C_2 119.5 . . ? C5C_2 C6C_2 H6C_2 119.5 . . ? O13C_2 C11C_2 O12C_2 124.3(4) . . ? O13C_2 C11C_2 C1C_2 118.4(3) . . ? O12C_2 C11C_2 C1C_2 117.3(3) . . ? C11C_2 O12C_2 Fe4_2 128.2(2) . . ? C11C_2 O13C_2 Fe1_2 130.2(3) . . ? O43C_2 N41C_2 O42C_2 122.6(4) . . ? O43C_2 N41C_2 C4C_2 119.4(4) . . ? O42C_2 N41C_2 C4C_2 118.0(4) . . ? C2D_2 C1D_2 C6D_2 120.1(4) . . ? C2D_2 C1D_2 C11D_2 121.4(4) . . ? C6D_2 C1D_2 C11D_2 118.5(4) . . ? C1D_2 C2D_2 C3D_2 120.8(4) . . ? C1D_2 C2D_2 H2D_2 119.6 . . ? C3D_2 C2D_2 H2D_2 119.6 . . ? C4D_2 C3D_2 C2D_2 117.5(4) . . ? C4D_2 C3D_2 H3D_2 121.2 . . ? C2D_2 C3D_2 H3D_2 121.2 . . ? C5D_2 C4D_2 C3D_2 123.2(4) . . ? C5D_2 C4D_2 N41D_2 117.9(4) . . ? C3D_2 C4D_2 N41D_2 118.8(4) . . ? C4D_2 C5D_2 C6D_2 119.4(4) . . ? C4D_2 C5D_2 H5D_2 120.3 . . ? C6D_2 C5D_2 H5D_2 120.3 . . ? C5D_2 C6D_2 C1D_2 118.9(4) . . ? C5D_2 C6D_2 H6D_2 120.6 . . ? C1D_2 C6D_2 H6D_2 120.6 . . ? O12D_2 C11D_2 O13D_2 125.5(4) . . ? O12D_2 C11D_2 C1D_2 117.6(4) . . ? O13D_2 C11D_2 C1D_2 116.9(3) . . ? C11D_2 O12D_2 Fe3_2 128.4(3) . . ? C11D_2 O13D_2 Fe2_2 129.7(3) . . ? O43D_2 N41D_2 O42D_2 123.9(5) . . ? O43D_2 N41D_2 C4D_2 118.7(5) . . ? O42D_2 N41D_2 C4D_2 117.2(4) . . ? C2E_2 C1E_2 C6E_2 119.0(4) . . ? C2E_2 C1E_2 C11E_2 120.2(4) . . ? C6E_2 C1E_2 C11E_2 120.8(3) . . ? C1E_2 C2E_2 C3E_2 122.0(4) . . ? C1E_2 C2E_2 H2E_2 119.0 . . ? C3E_2 C2E_2 H2E_2 119.0 . . ? C2E_2 C3E_2 C4E_2 118.0(4) . . ? C2E_2 C3E_2 H3E_2 121.0 . . ? C4E_2 C3E_2 H3E_2 121.0 . . ? C3E_2 C4E_2 C5E_2 122.0(4) . . ? C3E_2 C4E_2 N41E_2 119.6(3) . . ? C5E_2 C4E_2 N41E_2 118.3(4) . . ? C4E_2 C5E_2 C6E_2 118.1(4) . . ? C4E_2 C5E_2 H5E_2 121.0 . . ? C6E_2 C5E_2 H5E_2 121.0 . . ? C1E_2 C6E_2 C5E_2 120.9(4) . . ? C1E_2 C6E_2 H6E_2 119.5 . . ? C5E_2 C6E_2 H6E_2 119.5 . . ? O12E_2 C11E_2 O13E_2 125.7(4) . . ? O12E_2 C11E_2 C1E_2 117.3(3) . . ? O13E_2 C11E_2 C1E_2 117.0(4) . . ? C11E_2 O12E_2 Fe5_2 131.1(2) . . ? C11E_2 O13E_2 Fe3_2 124.3(3) . . ? O43E_2 N41E_2 O42E_2 124.4(3) . . ? O43E_2 N41E_2 C4E_2 118.8(3) . . ? O42E_2 N41E_2 C4E_2 116.7(3) . . ? C6F_2 C1F_2 C2F_2 119.3(4) . . ? C6F_2 C1F_2 C11F_2 120.6(4) . . ? C2F_2 C1F_2 C11F_2 120.0(4) . . ? C1F_2 C2F_2 C3F_2 121.8(4) . . ? C1F_2 C2F_2 H2F_2 119.1 . . ? C3F_2 C2F_2 H2F_2 119.1 . . ? C4F_2 C3F_2 C2F_2 116.8(4) . . ? C4F_2 C3F_2 H3F_2 121.6 . . ? C2F_2 C3F_2 H3F_2 121.6 . . ? C5F_2 C4F_2 C3F_2 124.0(4) . . ? C5F_2 C4F_2 N41F_2 118.9(4) . . ? C3F_2 C4F_2 N41F_2 117.1(4) . . ? C4F_2 C5F_2 C6F_2 117.4(4) . . ? C4F_2 C5F_2 H5F_2 121.3 . . ? C6F_2 C5F_2 H5F_2 121.3 . . ? C1F_2 C6F_2 C5F_2 120.7(4) . . ? C1F_2 C6F_2 H6F_2 119.7 . . ? C5F_2 C6F_2 H6F_2 119.7 . . ? O13F_2 C11F_2 O12F_2 125.8(4) . . ? O13F_2 C11F_2 C1F_2 117.8(4) . . ? O12F_2 C11F_2 C1F_2 116.3(4) . . ? C11F_2 O12F_2 Fe4_2 126.0(2) . . ? C11F_2 O13F_2 Fe6_2 127.7(3) . . ? O43F_2 N41F_2 O42F_2 124.9(4) . . ? O43F_2 N41F_2 C4F_2 116.4(4) . . ? O42F_2 N41F_2 C4F_2 118.7(4) . . ? C6G_2 N1G_2 C2G_2 117.1(4) . . ? C6G_2 N1G_2 Fe5_2 119.8(3) . . ? C2G_2 N1G_2 Fe5_2 123.0(3) . . ? N1G_2 C2G_2 C3G_2 123.1(4) . . ? N1G_2 C2G_2 H2G_2 118.5 . . ? C3G_2 C2G_2 H2G_2 118.5 . . ? C2G_2 C3G_2 C4G_2 118.6(4) . . ? C2G_2 C3G_2 H3G_2 120.7 . . ? C4G_2 C3G_2 H3G_2 120.7 . . ? C3G_2 C4G_2 C5G_2 119.2(4) . . ? C3G_2 C4G_2 H4G_2 120.4 . . ? C5G_2 C4G_2 H4G_2 120.4 . . ? C6G_2 C5G_2 C4G_2 119.3(4) . . ? C6G_2 C5G_2 H5G_2 120.4 . . ? C4G_2 C5G_2 H5G_2 120.4 . . ? N1G_2 C6G_2 C5G_2 122.8(4) . . ? N1G_2 C6G_2 H6G_2 118.6 . . ? C5G_2 C6G_2 H6G_2 118.6 . . ? C6H_2 N1H_2 C2H_2 116.7(4) . . ? C6H_2 N1H_2 Fe6_2 123.4(3) . . ? C2H_2 N1H_2 Fe6_2 119.9(3) . . ? N1H_2 C2H_2 C3H_2 124.2(4) . . ? N1H_2 C2H_2 H2H_2 117.9 . . ? C3H_2 C2H_2 H2H_2 117.9 . . ? C4H_2 C3H_2 C2H_2 117.9(5) . . ? C4H_2 C3H_2 H3H_2 121.0 . . ? C2H_2 C3H_2 H3H_2 121.0 . . ? C3H_2 C4H_2 C5H_2 118.4(5) . . ? C3H_2 C4H_2 H4H_2 120.8 . . ? C5H_2 C4H_2 H4H_2 120.8 . . ? C6H_2 C5H_2 C4H_2 119.4(5) . . ? C6H_2 C5H_2 H5H_2 120.3 . . ? C4H_2 C5H_2 H5H_2 120.3 . . ? N1H_2 C6H_2 C5H_2 123.3(5) . . ? N1H_2 C6H_2 H6H_2 118.3 . . ? C5H_2 C6H_2 H6H_2 118.3 . . ? C2I_2 O1I_2 Fe5_2 129.7(2) . . ? C2I_2 O1I_2 Fe1_2 125.7(2) . . ? Fe5_2 O1I_2 Fe1_2 103.39(11) . . ? O1I_2 C2I_2 H2I1_2 109.5 . . ? O1I_2 C2I_2 H2I2_2 109.5 . . ? H2I1_2 C2I_2 H2I2_2 109.5 . . ? O1I_2 C2I_2 H2I3_2 109.5 . . ? H2I1_2 C2I_2 H2I3_2 109.5 . . ? H2I2_2 C2I_2 H2I3_2 109.5 . . ? C2J'_2 O1J_2 C2J_2 27.7(6) . . ? C2J'_2 O1J_2 Fe2_2 121.9(6) . . ? C2J_2 O1J_2 Fe2_2 123.7(7) . . ? C2J'_2 O1J_2 Fe6_2 134.2(6) . . ? C2J_2 O1J_2 Fe6_2 127.1(6) . . ? Fe2_2 O1J_2 Fe6_2 103.31(11) . . ? O1J_2 C2J_2 H2J1_2 109.5 . . ? O1J_2 C2J_2 H2J2_2 109.5 . . ? H2J1_2 C2J_2 H2J2_2 109.5 . . ? O1J_2 C2J_2 H2J3_2 109.5 . . ? H2J1_2 C2J_2 H2J3_2 109.5 . . ? H2J2_2 C2J_2 H2J3_2 109.5 . . ? O1J_2 C2J'_2 H2J4_2 109.5 . . ? O1J_2 C2J'_2 H2J5_2 109.5 . . ? H2J4_2 C2J'_2 H2J5_2 109.5 . . ? O1J_2 C2J'_2 H2J6_2 109.5 . . ? H2J4_2 C2J'_2 H2J6_2 109.5 . . ? H2J5_2 C2J'_2 H2J6_2 109.5 . . ? C2K_2 O1K_2 Fe3_2 127.0(3) . . ? C2K_2 O1K_2 Fe5_2 127.7(3) . . ? Fe3_2 O1K_2 Fe5_2 98.39(11) . . ? O1K_2 C2K_2 H2K1_2 109.5 . . ? O1K_2 C2K_2 H2K2_2 109.5 . . ? H2K1_2 C2K_2 H2K2_2 109.5 . . ? O1K_2 C2K_2 H2K3_2 109.5 . . ? H2K1_2 C2K_2 H2K3_2 109.5 . . ? H2K2_2 C2K_2 H2K3_2 109.5 . . ? C2L'_2 O1L_2 C2L_2 47.3(7) . . ? C2L'_2 O1L_2 Fe4_2 126.6(6) . . ? C2L_2 O1L_2 Fe4_2 123.1(3) . . ? C2L'_2 O1L_2 Fe6_2 131.3(6) . . ? C2L_2 O1L_2 Fe6_2 124.4(3) . . ? Fe4_2 O1L_2 Fe6_2 98.48(11) . . ? O1L_2 C2L_2 H2L1_2 109.5 . . ? O1L_2 C2L_2 H2L2_2 109.5 . . ? H2L1_2 C2L_2 H2L2_2 109.5 . . ? O1L_2 C2L_2 H2L3_2 109.5 . . ? H2L1_2 C2L_2 H2L3_2 109.5 . . ? H2L2_2 C2L_2 H2L3_2 109.5 . . ? O1L_2 C2L'_2 H2L4_2 109.5 . . ? O1L_2 C2L'_2 H2L5_2 109.5 . . ? H2L4_2 C2L'_2 H2L5_2 109.5 . . ? O1L_2 C2L'_2 H2L6_2 109.5 . . ? H2L4_2 C2L'_2 H2L6_2 109.5 . . ? H2L5_2 C2L'_2 H2L6_2 109.5 . . ? O1A_3 Fe1_3 O1I_3 99.22(11) . . ? O1A_3 Fe1_3 O12C_3 94.34(10) . . ? O1I_3 Fe1_3 O12C_3 94.69(10) . . ? O1A_3 Fe1_3 O23B_3 101.57(10) . . ? O1I_3 Fe1_3 O23B_3 159.13(10) . . ? O12C_3 Fe1_3 O23B_3 82.00(10) . . ? O1A_3 Fe1_3 O134_3 174.04(10) . . ? O1I_3 Fe1_3 O134_3 79.69(10) . . ? O12C_3 Fe1_3 O134_3 91.59(9) . . ? O23B_3 Fe1_3 O134_3 79.81(9) . . ? O1A_3 Fe1_3 N22A_3 84.56(11) . . ? O1I_3 Fe1_3 N22A_3 95.22(11) . . ? O12C_3 Fe1_3 N22A_3 170.07(11) . . ? O23B_3 Fe1_3 N22A_3 88.54(11) . . ? O134_3 Fe1_3 N22A_3 89.70(10) . . ? O1B_3 Fe2_3 O1J_3 97.48(11) . . ? O1B_3 Fe2_3 O12D_3 95.82(10) . . ? O1J_3 Fe2_3 O12D_3 92.87(11) . . ? O1B_3 Fe2_3 O23A_3 103.95(11) . . ? O1J_3 Fe2_3 O23A_3 158.41(10) . . ? O12D_3 Fe2_3 O23A_3 82.45(10) . . ? O1B_3 Fe2_3 O234_3 171.89(10) . . ? O1J_3 Fe2_3 O234_3 78.80(10) . . ? O12D_3 Fe2_3 O234_3 91.58(9) . . ? O23A_3 Fe2_3 O234_3 80.27(9) . . ? O1B_3 Fe2_3 N22B_3 83.18(11) . . ? O1J_3 Fe2_3 N22B_3 96.37(11) . . ? O12D_3 Fe2_3 N22B_3 170.76(11) . . ? O23A_3 Fe2_3 N22B_3 88.86(11) . . ? O234_3 Fe2_3 N22B_3 90.04(10) . . ? O1L_3 Fe3_3 O234_3 163.73(10) . . ? O1L_3 Fe3_3 O13D_3 99.77(10) . . ? O234_3 Fe3_3 O13D_3 95.32(10) . . ? O1L_3 Fe3_3 O134_3 81.07(10) . . ? O234_3 Fe3_3 O134_3 83.47(10) . . ? O13D_3 Fe3_3 O134_3 176.00(10) . . ? O1L_3 Fe3_3 O23A_3 92.78(10) . . ? O234_3 Fe3_3 O23A_3 82.48(9) . . ? O13D_3 Fe3_3 O23A_3 84.93(10) . . ? O134_3 Fe3_3 O23A_3 91.13(9) . . ? O1L_3 Fe3_3 O13E_3 90.91(10) . . ? O234_3 Fe3_3 O13E_3 95.17(10) . . ? O13D_3 Fe3_3 O13E_3 89.94(10) . . ? O134_3 Fe3_3 O13E_3 93.97(10) . . ? O23A_3 Fe3_3 O13E_3 174.12(11) . . ? O1L_3 Fe3_3 Fe4_3 123.10(8) . . ? O234_3 Fe3_3 Fe4_3 42.09(7) . . ? O13D_3 Fe3_3 Fe4_3 137.13(8) . . ? O134_3 Fe3_3 Fe4_3 42.17(7) . . ? O23A_3 Fe3_3 Fe4_3 92.06(7) . . ? O13E_3 Fe3_3 Fe4_3 89.75(7) . . ? O1K_3 Fe4_3 O13C_3 99.58(10) . . ? O1K_3 Fe4_3 O234_3 80.50(10) . . ? O13C_3 Fe4_3 O234_3 176.28(9) . . ? O1K_3 Fe4_3 O134_3 163.24(10) . . ? O13C_3 Fe4_3 O134_3 95.59(10) . . ? O234_3 Fe4_3 O134_3 83.90(10) . . ? O1K_3 Fe4_3 O13F_3 90.02(10) . . ? O13C_3 Fe4_3 O13F_3 87.70(10) . . ? O234_3 Fe4_3 O13F_3 96.02(10) . . ? O134_3 Fe4_3 O13F_3 97.70(10) . . ? O1K_3 Fe4_3 O23B_3 92.47(10) . . ? O13C_3 Fe4_3 O23B_3 84.64(10) . . ? O234_3 Fe4_3 O23B_3 91.64(9) . . ? O134_3 Fe4_3 O23B_3 81.86(9) . . ? O13F_3 Fe4_3 O23B_3 172.24(10) . . ? O1K_3 Fe4_3 Fe3_3 122.53(7) . . ? O13C_3 Fe4_3 Fe3_3 137.88(8) . . ? O234_3 Fe4_3 Fe3_3 42.11(7) . . ? O134_3 Fe4_3 Fe3_3 42.59(7) . . ? O13F_3 Fe4_3 Fe3_3 92.81(7) . . ? O23B_3 Fe4_3 Fe3_3 92.05(7) . . ? O1J_3 Fe5_3 O1K_3 97.11(10) . . ? O1J_3 Fe5_3 O12F_3 169.18(10) . . ? O1K_3 Fe5_3 O12F_3 86.50(10) . . ? O1J_3 Fe5_3 O234_3 80.36(10) . . ? O1K_3 Fe5_3 O234_3 78.63(10) . . ? O12F_3 Fe5_3 O234_3 90.41(10) . . ? O1J_3 Fe5_3 N1G_3 91.34(11) . . ? O1K_3 Fe5_3 N1G_3 167.22(11) . . ? O12F_3 Fe5_3 N1G_3 83.53(11) . . ? O234_3 Fe5_3 N1G_3 93.44(11) . . ? O1J_3 Fe5_3 Cl1_3 95.46(8) . . ? O1K_3 Fe5_3 Cl1_3 95.88(8) . . ? O12F_3 Fe5_3 Cl1_3 94.30(8) . . ? O234_3 Fe5_3 Cl1_3 172.55(7) . . ? N1G_3 Fe5_3 Cl1_3 92.82(9) . . ? O1I_3 Fe6_3 O1L_3 97.46(10) . . ? O1I_3 Fe6_3 O12E_3 167.57(11) . . ? O1L_3 Fe6_3 O12E_3 88.12(10) . . ? O1I_3 Fe6_3 O134_3 80.56(10) . . ? O1L_3 Fe6_3 O134_3 79.21(10) . . ? O12E_3 Fe6_3 O134_3 89.65(10) . . ? O1I_3 Fe6_3 N1H_3 88.79(11) . . ? O1L_3 Fe6_3 N1H_3 168.79(12) . . ? O12E_3 Fe6_3 N1H_3 84.02(11) . . ? O134_3 Fe6_3 N1H_3 92.74(11) . . ? O1I_3 Fe6_3 Cl2_3 95.90(8) . . ? O1L_3 Fe6_3 Cl2_3 97.01(8) . . ? O12E_3 Fe6_3 Cl2_3 94.42(8) . . ? O134_3 Fe6_3 Cl2_3 174.36(7) . . ? N1H_3 Fe6_3 Cl2_3 91.56(9) . . ? Fe4_3 O134_3 Fe3_3 95.25(11) . . ? Fe4_3 O134_3 Fe6_3 155.39(13) . . ? Fe3_3 O134_3 Fe6_3 95.65(10) . . ? Fe4_3 O134_3 Fe1_3 97.82(10) . . ? Fe3_3 O134_3 Fe1_3 116.10(11) . . ? Fe6_3 O134_3 Fe1_3 97.07(10) . . ? Fe4_3 O234_3 Fe3_3 95.80(11) . . ? Fe4_3 O234_3 Fe5_3 96.22(10) . . ? Fe3_3 O234_3 Fe5_3 155.40(13) . . ? Fe4_3 O234_3 Fe2_3 115.61(11) . . ? Fe3_3 O234_3 Fe2_3 96.89(10) . . ? Fe5_3 O234_3 Fe2_3 97.14(10) . . ? O1A_3 C1A_3 C6A_3 116.9(4) . . ? O1A_3 C1A_3 C2A_3 122.6(4) . . ? C6A_3 C1A_3 C2A_3 120.5(4) . . ? C1A_3 O1A_3 Fe1_3 128.4(2) . . ? C3A_3 C2A_3 C1A_3 117.0(4) . . ? C3A_3 C2A_3 C21A_3 120.1(4) . . ? C1A_3 C2A_3 C21A_3 122.9(3) . . ? C4A_3 C3A_3 C2A_3 121.6(4) . . ? C4A_3 C3A_3 H3A_3 119.2 . . ? C2A_3 C3A_3 H3A_3 119.2 . . ? C5A_3 C4A_3 C3A_3 120.1(4) . . ? C5A_3 C4A_3 H4A_3 120.0 . . ? C3A_3 C4A_3 H4A_3 120.0 . . ? C4A_3 C5A_3 C6A_3 120.5(4) . . ? C4A_3 C5A_3 H5A_3 119.7 . . ? C6A_3 C5A_3 H5A_3 119.7 . . ? C5A_3 C6A_3 C1A_3 120.1(4) . . ? C5A_3 C6A_3 H6A_3 119.9 . . ? C1A_3 C6A_3 H6A_3 119.9 . . ? N22A_3 C21A_3 C2A_3 119.6(4) . . ? N22A_3 C21A_3 C24A_3 120.0(4) . . ? C2A_3 C21A_3 C24A_3 120.4(3) . . ? C21A_3 N22A_3 O23A_3 114.5(3) . . ? C21A_3 N22A_3 Fe1_3 129.9(3) . . ? O23A_3 N22A_3 Fe1_3 115.3(2) . . ? N22A_3 O23A_3 Fe3_3 117.48(19) . . ? N22A_3 O23A_3 Fe2_3 119.32(18) . . ? Fe3_3 O23A_3 Fe2_3 96.34(10) . . ? C21A_3 C24A_3 H24A_3 109.5 . . ? C21A_3 C24A_3 H24B_3 109.5 . . ? H24A_3 C24A_3 H24B_3 109.5 . . ? C21A_3 C24A_3 H24C_3 109.5 . . ? H24A_3 C24A_3 H24C_3 109.5 . . ? H24B_3 C24A_3 H24C_3 109.5 . . ? O1B_3 C1B_3 C2B_3 123.8(3) . . ? O1B_3 C1B_3 C6B_3 117.2(3) . . ? C2B_3 C1B_3 C6B_3 119.0(3) . . ? C1B_3 O1B_3 Fe2_3 130.8(2) . . ? C1B_3 C2B_3 C3B_3 118.2(3) . . ? C1B_3 C2B_3 C21B_3 121.9(3) . . ? C3B_3 C2B_3 C21B_3 119.9(3) . . ? C4B_3 C3B_3 C2B_3 122.2(4) . . ? C4B_3 C3B_3 H3B_3 118.9 . . ? C2B_3 C3B_3 H3B_3 118.9 . . ? C3B_3 C4B_3 C5B_3 119.0(4) . . ? C3B_3 C4B_3 H4B_3 120.5 . . ? C5B_3 C4B_3 H4B_3 120.5 . . ? C6B_3 C5B_3 C4B_3 120.5(4) . . ? C6B_3 C5B_3 H5B_3 119.8 . . ? C4B_3 C5B_3 H5B_3 119.8 . . ? C5B_3 C6B_3 C1B_3 121.1(4) . . ? C5B_3 C6B_3 H6B_3 119.5 . . ? C1B_3 C6B_3 H6B_3 119.5 . . ? N22B_3 C21B_3 C2B_3 118.5(3) . . ? N22B_3 C21B_3 C24B_3 119.8(3) . . ? C2B_3 C21B_3 C24B_3 121.6(3) . . ? C21B_3 N22B_3 O23B_3 112.9(3) . . ? C21B_3 N22B_3 Fe2_3 131.7(3) . . ? O23B_3 N22B_3 Fe2_3 115.46(19) . . ? N22B_3 O23B_3 Fe4_3 117.20(19) . . ? N22B_3 O23B_3 Fe1_3 119.13(18) . . ? Fe4_3 O23B_3 Fe1_3 96.51(10) . . ? C21B_3 C24B_3 H24D_3 109.5 . . ? C21B_3 C24B_3 H24E_3 109.5 . . ? H24D_3 C24B_3 H24E_3 109.5 . . ? C21B_3 C24B_3 H24F_3 109.5 . . ? H24D_3 C24B_3 H24F_3 109.5 . . ? H24E_3 C24B_3 H24F_3 109.5 . . ? C6C_3 C1C_3 C2C_3 120.2(4) . . ? C6C_3 C1C_3 C11C_3 120.6(3) . . ? C2C_3 C1C_3 C11C_3 119.2(3) . . ? C3C_3 C2C_3 C1C_3 120.8(4) . . ? C3C_3 C2C_3 H2C_3 119.6 . . ? C1C_3 C2C_3 H2C_3 119.6 . . ? C2C_3 C3C_3 C4C_3 117.9(4) . . ? C2C_3 C3C_3 H3C_3 121.1 . . ? C4C_3 C3C_3 H3C_3 121.1 . . ? C5C_3 C4C_3 C3C_3 123.2(4) . . ? C5C_3 C4C_3 N41C_3 118.8(4) . . ? C3C_3 C4C_3 N41C_3 118.1(4) . . ? C4C_3 C5C_3 C6C_3 118.9(4) . . ? C4C_3 C5C_3 H5C_3 120.5 . . ? C6C_3 C5C_3 H5C_3 120.5 . . ? C1C_3 C6C_3 C5C_3 119.0(4) . . ? C1C_3 C6C_3 H6C_3 120.5 . . ? C5C_3 C6C_3 H6C_3 120.5 . . ? O12C_3 C11C_3 O13C_3 125.4(3) . . ? O12C_3 C11C_3 C1C_3 118.0(3) . . ? O13C_3 C11C_3 C1C_3 116.6(3) . . ? C11C_3 O12C_3 Fe1_3 131.1(2) . . ? C11C_3 O13C_3 Fe4_3 127.1(2) . . ? O42C_3 N41C_3 O43C_3 124.7(4) . . ? O42C_3 N41C_3 C4C_3 118.8(4) . . ? O43C_3 N41C_3 C4C_3 116.5(4) . . ? C6D_3 C1D_3 C2D_3 119.1(3) . . ? C6D_3 C1D_3 C11D_3 121.3(3) . . ? C2D_3 C1D_3 C11D_3 119.5(3) . . ? C3D_3 C2D_3 C1D_3 120.5(3) . . ? C3D_3 C2D_3 H2D_3 119.7 . . ? C1D_3 C2D_3 H2D_3 119.7 . . ? C2D_3 C3D_3 C4D_3 118.4(4) . . ? C2D_3 C3D_3 H3D_3 120.8 . . ? C4D_3 C3D_3 H3D_3 120.8 . . ? C5D_3 C4D_3 C3D_3 122.3(3) . . ? C5D_3 C4D_3 N41D_3 119.6(3) . . ? C3D_3 C4D_3 N41D_3 118.1(3) . . ? C4D_3 C5D_3 C6D_3 118.6(3) . . ? C4D_3 C5D_3 H5D_3 120.7 . . ? C6D_3 C5D_3 H5D_3 120.7 . . ? C5D_3 C6D_3 C1D_3 121.0(4) . . ? C5D_3 C6D_3 H6D_3 119.5 . . ? C1D_3 C6D_3 H6D_3 119.5 . . ? O12D_3 C11D_3 O13D_3 125.1(3) . . ? O12D_3 C11D_3 C1D_3 116.7(3) . . ? O13D_3 C11D_3 C1D_3 118.1(3) . . ? C11D_3 O12D_3 Fe2_3 131.4(2) . . ? C11D_3 O13D_3 Fe3_3 127.0(2) . . ? O43D_3 N41D_3 O42D_3 123.8(3) . . ? O43D_3 N41D_3 C4D_3 118.0(3) . . ? O42D_3 N41D_3 C4D_3 118.2(3) . . ? C2E_3 C1E_3 C6E_3 119.8(4) . . ? C2E_3 C1E_3 C11E_3 121.8(4) . . ? C6E_3 C1E_3 C11E_3 118.4(4) . . ? C1E_3 C2E_3 C3E_3 120.6(4) . . ? C1E_3 C2E_3 H2E_3 119.7 . . ? C3E_3 C2E_3 H2E_3 119.7 . . ? C4E_3 C3E_3 C2E_3 117.3(4) . . ? C4E_3 C3E_3 H3E_3 121.4 . . ? C2E_3 C3E_3 H3E_3 121.4 . . ? C5E_3 C4E_3 C3E_3 123.7(4) . . ? C5E_3 C4E_3 N41E_3 118.6(4) . . ? C3E_3 C4E_3 N41E_3 117.6(4) . . ? C4E_3 C5E_3 C6E_3 117.5(4) . . ? C4E_3 C5E_3 H5E_3 121.3 . . ? C6E_3 C5E_3 H5E_3 121.3 . . ? C5E_3 C6E_3 C1E_3 121.1(4) . . ? C5E_3 C6E_3 H6E_3 119.5 . . ? C1E_3 C6E_3 H6E_3 119.5 . . ? O13E_3 C11E_3 O12E_3 125.7(3) . . ? O13E_3 C11E_3 C1E_3 119.1(4) . . ? O12E_3 C11E_3 C1E_3 115.2(3) . . ? C11E_3 O12E_3 Fe6_3 131.5(2) . . ? C11E_3 O13E_3 Fe3_3 124.1(2) . . ? O42E_3 N41E_3 O43E_3 124.2(4) . . ? O42E_3 N41E_3 C4E_3 117.5(4) . . ? O43E_3 N41E_3 C4E_3 118.2(4) . . ? C6F_3 C1F_3 C2F_3 119.9(3) . . ? C6F_3 C1F_3 C11F_3 121.1(4) . . ? C2F_3 C1F_3 C11F_3 119.0(4) . . ? C3F_3 C2F_3 C1F_3 120.7(4) . . ? C3F_3 C2F_3 H2F_3 119.7 . . ? C1F_3 C2F_3 H2F_3 119.7 . . ? C4F_3 C3F_3 C2F_3 117.8(4) . . ? C4F_3 C3F_3 H3F_3 121.1 . . ? C2F_3 C3F_3 H3F_3 121.1 . . ? C3F_3 C4F_3 C5F_3 123.2(4) . . ? C3F_3 C4F_3 N41F_3 118.2(4) . . ? C5F_3 C4F_3 N41F_3 118.6(4) . . ? C4F_3 C5F_3 C6F_3 118.4(4) . . ? C4F_3 C5F_3 H5F_3 120.8 . . ? C6F_3 C5F_3 H5F_3 120.8 . . ? C1F_3 C6F_3 C5F_3 120.0(4) . . ? C1F_3 C6F_3 H6F_3 120.0 . . ? C5F_3 C6F_3 H6F_3 120.0 . . ? O12F_3 C11F_3 O13F_3 125.1(3) . . ? O12F_3 C11F_3 C1F_3 115.4(4) . . ? O13F_3 C11F_3 C1F_3 119.5(4) . . ? C11F_3 O12F_3 Fe5_3 131.9(2) . . ? C11F_3 O13F_3 Fe4_3 124.0(2) . . ? O43F_3 N41F_3 O42F_3 124.1(4) . . ? O43F_3 N41F_3 C4F_3 117.8(4) . . ? O42F_3 N41F_3 C4F_3 118.1(4) . . ? C2G_3 N1G_3 C6G_3 116.8(4) . . ? C2G_3 N1G_3 Fe5_3 122.4(3) . . ? C6G_3 N1G_3 Fe5_3 120.7(3) . . ? N1G_3 C2G_3 C3G_3 122.6(4) . . ? N1G_3 C2G_3 H2G_3 118.7 . . ? C3G_3 C2G_3 H2G_3 118.7 . . ? C4G_3 C3G_3 C2G_3 119.5(4) . . ? C4G_3 C3G_3 H3G_3 120.2 . . ? C2G_3 C3G_3 H3G_3 120.2 . . ? C3G_3 C4G_3 C5G_3 117.9(4) . . ? C3G_3 C4G_3 H4G_3 121.1 . . ? C5G_3 C4G_3 H4G_3 121.1 . . ? C6G_3 C5G_3 C4G_3 120.4(5) . . ? C6G_3 C5G_3 H5G_3 119.8 . . ? C4G_3 C5G_3 H5G_3 119.8 . . ? C5G_3 C6G_3 N1G_3 122.7(4) . . ? C5G_3 C6G_3 H6G_3 118.6 . . ? N1G_3 C6G_3 H6G_3 118.6 . . ? C2H_3 N1H_3 C6H_3 117.5(3) . . ? C2H_3 N1H_3 Fe6_3 123.4(3) . . ? C6H_3 N1H_3 Fe6_3 119.0(3) . . ? N1H_3 C2H_3 C3H_3 123.1(4) . . ? N1H_3 C2H_3 H2H_3 118.5 . . ? C3H_3 C2H_3 H2H_3 118.5 . . ? C2H_3 C3H_3 C4H_3 118.5(4) . . ? C2H_3 C3H_3 H3H_3 120.7 . . ? C4H_3 C3H_3 H3H_3 120.7 . . ? C5H_3 C4H_3 C3H_3 118.6(4) . . ? C5H_3 C4H_3 H4H_3 120.7 . . ? C3H_3 C4H_3 H4H_3 120.7 . . ? C4H_3 C5H_3 C6H_3 119.5(4) . . ? C4H_3 C5H_3 H5H_3 120.3 . . ? C6H_3 C5H_3 H5H_3 120.3 . . ? N1H_3 C6H_3 C5H_3 122.9(4) . . ? N1H_3 C6H_3 H6H_3 118.6 . . ? C5H_3 C6H_3 H6H_3 118.6 . . ? C2I_3 O1I_3 Fe6_3 127.4(2) . . ? C2I_3 O1I_3 Fe1_3 124.8(2) . . ? Fe6_3 O1I_3 Fe1_3 102.68(12) . . ? O1I_3 C2I_3 H2I1_3 109.5 . . ? O1I_3 C2I_3 H2I2_3 109.5 . . ? H2I1_3 C2I_3 H2I2_3 109.5 . . ? O1I_3 C2I_3 H2I3_3 109.5 . . ? H2I1_3 C2I_3 H2I3_3 109.5 . . ? H2I2_3 C2I_3 H2I3_3 109.5 . . ? C2J_3 O1J_3 Fe5_3 132.7(2) . . ? C2J_3 O1J_3 Fe2_3 123.1(2) . . ? Fe5_3 O1J_3 Fe2_3 103.70(11) . . ? O1J_3 C2J_3 H2J1_3 109.5 . . ? O1J_3 C2J_3 H2J2_3 109.5 . . ? H2J1_3 C2J_3 H2J2_3 109.5 . . ? O1J_3 C2J_3 H2J3_3 109.5 . . ? H2J1_3 C2J_3 H2J3_3 109.5 . . ? H2J2_3 C2J_3 H2J3_3 109.5 . . ? C2K'_3 O1K_3 C2K_3 28.3(4) . . ? C2K'_3 O1K_3 Fe4_3 131.0(6) . . ? C2K_3 O1K_3 Fe4_3 127.2(5) . . ? C2K'_3 O1K_3 Fe5_3 128.2(6) . . ? C2K_3 O1K_3 Fe5_3 129.8(5) . . ? Fe4_3 O1K_3 Fe5_3 98.87(10) . . ? O1K_3 C2K_3 H2K1_3 109.5 . . ? O1K_3 C2K_3 H2K2_3 109.5 . . ? H2K1_3 C2K_3 H2K2_3 109.5 . . ? O1K_3 C2K_3 H2K3_3 109.5 . . ? H2K1_3 C2K_3 H2K3_3 109.5 . . ? H2K2_3 C2K_3 H2K3_3 109.5 . . ? O1K_3 C2K'_3 H2K4_3 109.5 . . ? O1K_3 C2K'_3 H2K5_3 109.5 . . ? H2K4_3 C2K'_3 H2K5_3 109.5 . . ? O1K_3 C2K'_3 H2K6_3 109.5 . . ? H2K4_3 C2K'_3 H2K6_3 109.5 . . ? H2K5_3 C2K'_3 H2K6_3 109.5 . . ? C2L_3 O1L_3 C2L'_3 33.7(7) . . ? C2L_3 O1L_3 Fe3_3 122.5(4) . . ? C2L'_3 O1L_3 Fe3_3 126.4(8) . . ? C2L_3 O1L_3 Fe6_3 128.7(4) . . ? C2L'_3 O1L_3 Fe6_3 134.3(9) . . ? Fe3_3 O1L_3 Fe6_3 98.58(11) . . ? O1L_3 C2L_3 H2L1_3 109.5 . . ? O1L_3 C2L_3 H2L2_3 109.5 . . ? H2L1_3 C2L_3 H2L2_3 109.5 . . ? O1L_3 C2L_3 H2L3_3 109.5 . . ? H2L1_3 C2L_3 H2L3_3 109.5 . . ? H2L2_3 C2L_3 H2L3_3 109.5 . . ? O1L_3 C2L'_3 H2L4_3 109.5 . . ? O1L_3 C2L'_3 H2L5_3 109.5 . . ? H2L4_3 C2L'_3 H2L5_3 109.5 . . ? O1L_3 C2L'_3 H2L6_3 109.5 . . ? H2L4_3 C2L'_3 H2L6_3 109.5 . . ? H2L5_3 C2L'_3 H2L6_3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 26.41 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.899 _refine_diff_density_min -0.677 _refine_diff_density_rms 0.090 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 0.000 336 101 ' ' 2 0.082 -0.014 0.478 27 4 ' ' 3 0.909 0.016 0.524 25 3 ' ' 4 0.814 0.190 0.847 13 2 ' ' 5 0.659 0.500 1.000 1331 462 ' ' 6 0.186 0.810 0.153 13 2 ' ' _platon_squeeze_details ; ; # Attachment '- eb7016-(6).cif' data_eb7016 _database_code_depnum_ccdc_archive 'CCDC 794875' _audit_creation_date 19-02-07 _audit_creation_method SHELXL-97 _chemical_compound_source 'I.Gass Reaction IAG1591' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety (NEtH)2[Fe6O2(Sal)4(OMe)6(SO4)2] _chemical_formula_sum 'C54 H88 Fe6 N6 O24 S2' _chemical_formula_weight 1604.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.4582(4) _cell_length_b 14.4149(3) _cell_length_c 22.6752(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6687.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7512 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 29.54 _exptl_crystal_description Block _exptl_crystal_colour Black _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.594 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3336 _exptl_absorpt_coefficient_mu 1.410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.432 _exptl_absorpt_correction_T_max 0.81 _exptl_absorpt_process_details 'SADABS version 2006/1' _exptl_special_details ; SLOW EVAPORATION OF SOLUTION ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex CCD' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73693 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.03 _reflns_number_total 5902 _reflns_number_gt 5602 _reflns_threshold_expression >2sigma(I) _computing_data_collection Smart _computing_cell_refinement Saint _computing_data_reduction Saint _computing_structure_solution Sir92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Shelx-97 _computing_publication_material Platon _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Note that restraints were used to control geometry and thermal behaviour in the disorder regions. CHECKCIF OUTPUT: 413_ALERT_2_A Short Inter XH3 .. XHn H2A .. H32B .. 1.66 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H2B .. H22B .. 1.81 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H2B .. H32B .. 1.37 Ang. 413_ALERT_2_A Short Inter XH3 .. XHn H2C .. H32B .. 1.73 Ang. 432_ALERT_2_A Short Inter X...Y Contact C2 .. C32B .. 2.46 Ang. 411_ALERT_2_B Short Inter H...H Contact H3B .. H82B .. 2.04 Ang. 413_ALERT_2_B Short Inter XH3 .. XHn H4C .. H82C .. 1.98 Ang. 432_ALERT_2_B Short Inter X...Y Contact C2 .. C22B .. 3.02 Ang. ALL THE ABOVE INTERMOLECULAR CONTACTS ARE TO DISORDERED ATOMS 911_ALERT_3_C # Missing FCF Refl Between THmin & STh/l= 5 The data collection strategy used aimed to achieve a complete data set to 2\q = 53 deg. Some higher angle data were collected in the process and these have been included in the refinement. 061_ALERT_3_B Tmax/Tmin Range Test RR' too Large ............. 0.62 Sadabs corrects for all systematic errors that lead to disparities in the intensities of symmetry-equivalent data. These may include absorption by the mount, crystal decay, changes in the volume of the crystal illuminated, etc. 301_ALERT_3_B Main Residue Disorder ......................... 26.00 Perc. THIS HAS BEEN MODELLED 241_ALERT_2_B Check High Ueq as Compared to Neighbors for C42B 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.00 Ratio 222_ALERT_3_B Large Non-Solvent H Ueq(max)/Ueq(min) ... 4.48 Ratio 242_ALERT_2_C Check Low Ueq as Compared to Neighbors for C32B 250_ALERT_2_C Large U3/U1 Ratio for Average U(i,j) Tensor .... 2.11 THIS IS NORMAL FOR A DISORDERED STRUCTURE 720_ALERT_4_C Number of Unusual/Non-Standard Label(s) ........ 6 795_ALERT_4_C C-Atom in CIF Coordinate List out of Sequence .. C13 796_ALERT_4_C O-Atom in CIF Coordinate List out of Sequence .. O11 797_ALERT_4_C N-Atom in CIF Coordinate List out of Sequence .. N1 THE NUMBERING SCHEME USED IS REASONABLE 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C3 243_ALERT_4_C High 'Solvent' Ueq as Compared to Neighbors for C5 244_ALERT_4_C Low 'Solvent' Ueq as Compared to Neighbors for N1 THESE ATOMS WILL HAVE HIGH THERMAL MOTION DUE TO FREEDOM OF MOVEMENT. 042_ALERT_1_C Calc. and Rep. MoietyFormula Strings Differ .... ? 045_ALERT_1_C Calculated and Reported Z Differ by ............ 2.00 Ratio THE ONE GIVEN IS INTENDED TO BE MORE CHEMICALLY SIGNIFICANT 360_ALERT_2_B Short C(sp3)-C(sp3) Bond C5 - C6 ... 1.32 Ang. 341_ALERT_3_C Low Bond Precision on C-C bonds (x 1000) Ang ... 12 410_ALERT_2_C Short Intra H...H Contact H51 .. H81A .. 1.90 Ang. NO ACTION TAKEN ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0253P)^2^+37.3381P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5902 _refine_ls_number_parameters 454 _refine_ls_number_restraints 130 _refine_ls_R_factor_all 0.0881 _refine_ls_R_factor_gt 0.0826 _refine_ls_wR_factor_ref 0.1547 _refine_ls_wR_factor_gt 0.1526 _refine_ls_goodness_of_fit_ref 1.362 _refine_ls_restrained_S_all 1.349 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 0.10410(4) 0.15253(6) 0.46150(4) 0.0250(2) Uani 1 1 d . . . Fe2 Fe -0.04151(4) 0.05011(6) 0.45485(4) 0.0236(2) Uani 1 1 d . . . Fe3 Fe 0.02005(5) 0.16135(6) 0.57423(4) 0.0308(2) Uani 1 1 d . . . O123 O 0.03866(19) 0.0750(3) 0.50144(16) 0.0228(9) Uani 1 1 d . . . O11 O 0.1634(2) 0.2243(3) 0.41751(18) 0.0393(12) Uani 1 1 d D A . C11 C 0.1646(3) 0.2571(4) 0.3627(2) 0.0319(15) Uani 1 1 d D . . C21 C 0.2248(3) 0.2906(4) 0.3427(3) 0.0361(16) Uani 1 1 d D A . H21 H 0.2620 0.2865 0.3676 0.043 Uiso 1 1 calc R . . C31 C 0.2310(3) 0.3295(4) 0.2875(3) 0.0388(17) Uani 1 1 d D . . H31 H 0.2721 0.3523 0.2745 0.047 Uiso 1 1 calc R A . C41 C 0.1769(3) 0.3350(4) 0.2512(3) 0.0400(17) Uani 1 1 d D A . H41 H 0.1807 0.3627 0.2133 0.048 Uiso 1 1 calc R . . C51 C 0.1174(3) 0.3004(4) 0.2697(2) 0.0345(15) Uani 1 1 d D . . H51 H 0.0809 0.3034 0.2438 0.041 Uiso 1 1 calc R A . C61 C 0.1098(3) 0.2609(4) 0.3257(2) 0.0296(14) Uani 1 1 d D A . C71 C 0.0442(3) 0.2264(4) 0.3430(3) 0.0335(15) Uani 1 1 d D . . N71 N 0.0361(2) 0.1829(3) 0.3930(2) 0.0295(12) Uani 1 1 d D A . O71 O -0.0272(2) 0.1582(3) 0.40561(19) 0.0339(10) Uani 1 1 d D A . C81 C -0.0137(4) 0.2393(6) 0.3036(3) 0.055(2) Uani 1 1 d . A . H81A H 0.0015 0.2412 0.2622 0.066 Uiso 1 1 calc R . . H81B H -0.0428 0.1848 0.3078 0.066 Uiso 1 1 calc R . . C91 C -0.0521(5) 0.3246(8) 0.3160(5) 0.092(4) Uani 1 1 d . . . H91A H -0.0722 0.3198 0.3551 0.139 Uiso 1 1 calc R A . H91B H -0.0864 0.3316 0.2861 0.139 Uiso 1 1 calc R . . H91C H -0.0231 0.3787 0.3148 0.139 Uiso 1 1 calc R . . C13 C 0.1944(5) 0.0122(6) 0.3938(5) 0.080(3) Uani 1 1 d . . . H13A H 0.2189 0.0702 0.3898 0.120 Uiso 1 1 calc R A . H13B H 0.1905 -0.0177 0.3551 0.120 Uiso 1 1 calc R . . H13C H 0.2173 -0.0293 0.4210 0.120 Uiso 1 1 calc R . . O13 O 0.1326(2) 0.0311(3) 0.4155(2) 0.0374(11) Uani 1 1 d . A . H13D H 0.1222 -0.0211 0.4423 0.045 Uiso 1 1 d R . . C14 C 0.0011(4) -0.0228(5) 0.3325(3) 0.0423(18) Uani 1 1 d . . . H14A H 0.0118 -0.0813 0.3126 0.063 Uiso 1 1 calc R A . H14B H 0.0342 0.0239 0.3229 0.063 Uiso 1 1 calc R . . H14C H -0.0419 -0.0012 0.3192 0.063 Uiso 1 1 calc R . . O14 O -0.0002(2) -0.0371(3) 0.39415(16) 0.0281(9) Uani 1 1 d . . . S16 S 0.16082(7) 0.08093(10) 0.58256(6) 0.0251(3) Uani 1 1 d . . . O16 O 0.2207(2) 0.0773(3) 0.61713(18) 0.0333(10) Uani 1 1 d . A . O26 O 0.1749(2) 0.1161(3) 0.52228(17) 0.0281(9) Uani 1 1 d . A . O36 O 0.13293(19) -0.0142(3) 0.57897(17) 0.0263(9) Uani 1 1 d . . . O46 O 0.1134(2) 0.1435(3) 0.61046(17) 0.0291(10) Uani 1 1 d . A . N1 N 0.2695(5) -0.1029(7) 0.6371(5) 0.094(3) Uani 1 1 d . . . H1 H 0.2564 -0.0439 0.6315 0.112 Uiso 1 1 calc R . . C1 C 0.2114(8) -0.1596(8) 0.6709(5) 0.114(5) Uani 1 1 d . . . H1A H 0.1728 -0.1641 0.6447 0.137 Uiso 1 1 calc R . . H1B H 0.2265 -0.2233 0.6797 0.137 Uiso 1 1 calc R . . C2 C 0.1927(8) -0.1128(10) 0.7262(6) 0.138(6) Uani 1 1 d . . . H2A H 0.2320 -0.0997 0.7494 0.206 Uiso 1 1 calc R . . H2B H 0.1634 -0.1531 0.7488 0.206 Uiso 1 1 calc R . . H2C H 0.1703 -0.0545 0.7170 0.206 Uiso 1 1 calc R . . C3 C 0.2788(9) -0.1483(10) 0.5779(8) 0.137(6) Uani 1 1 d . . . H3A H 0.3086 -0.2020 0.5826 0.164 Uiso 1 1 calc R . . H3B H 0.2362 -0.1722 0.5640 0.164 Uiso 1 1 calc R . . C4 C 0.3055(6) -0.0863(9) 0.5334(7) 0.133(6) Uani 1 1 d . . . H4A H 0.2738 -0.0371 0.5249 0.199 Uiso 1 1 calc R . . H4B H 0.3146 -0.1214 0.4973 0.199 Uiso 1 1 calc R . . H4C H 0.3461 -0.0585 0.5480 0.199 Uiso 1 1 calc R . . C5 C 0.3280(12) -0.1029(12) 0.6727(11) 0.217(11) Uani 1 1 d . . . H5A H 0.3209 -0.1423 0.7079 0.261 Uiso 1 1 calc R . . H5B H 0.3645 -0.1300 0.6497 0.261 Uiso 1 1 calc R . . C6 C 0.3439(7) -0.0186(10) 0.6896(8) 0.150(7) Uani 1 1 d . . . H6A H 0.3540 0.0193 0.6548 0.225 Uiso 1 1 calc R . . H6B H 0.3823 -0.0214 0.7153 0.225 Uiso 1 1 calc R . . H6C H 0.3072 0.0092 0.7111 0.225 Uiso 1 1 calc R . . O12A O 0.0023(3) 0.2511(4) 0.6351(2) 0.0343(13) Uani 0.832(5) 1 d PDU A 1 C12A C -0.0378(3) 0.3243(3) 0.6342(2) 0.0350(18) Uani 0.832(5) 1 d PGDU A 1 C22A C -0.0240(3) 0.3943(4) 0.6745(2) 0.046(2) Uani 0.832(5) 1 d PGDU A 1 H22A H 0.0120 0.3882 0.7007 0.056 Uiso 0.832(5) 1 calc PR A 1 C32A C -0.0630(3) 0.4733(3) 0.6765(3) 0.058(3) Uani 0.832(5) 1 d PGDU A 1 H32A H -0.0536 0.5211 0.7041 0.070 Uiso 0.832(5) 1 calc PR A 1 C42A C -0.1157(3) 0.4822(3) 0.6382(3) 0.053(4) Uani 0.832(5) 1 d PGDU A 1 H42A H -0.1423 0.5362 0.6396 0.064 Uiso 0.832(5) 1 calc PR A 1 C52A C -0.1294(2) 0.4123(4) 0.5979(2) 0.048(2) Uani 0.832(5) 1 d PGDU A 1 H52A H -0.1654 0.4184 0.5718 0.057 Uiso 0.832(5) 1 calc PR A 1 C62A C -0.0905(3) 0.3333(3) 0.5959(2) 0.0359(17) Uani 0.832(5) 1 d PGDU A 1 C72A C -0.1117(3) 0.2573(5) 0.5558(3) 0.0330(17) Uani 0.832(5) 1 d PDU A 1 N72A N -0.0744(3) 0.1852(4) 0.5472(2) 0.0273(14) Uani 0.832(5) 1 d PDU A 1 O72A O -0.0993(3) 0.1148(3) 0.5133(2) 0.0286(13) Uani 0.832(5) 1 d PDU A 1 C82A C -0.1740(4) 0.2669(6) 0.5211(4) 0.040(2) Uani 0.832(5) 1 d PU A 1 H82A H -0.2055 0.3058 0.5431 0.048 Uiso 0.832(5) 1 calc PR A 1 H82B H -0.1939 0.2051 0.5148 0.048 Uiso 0.832(5) 1 calc PR A 1 C92A C -0.1579(5) 0.3119(7) 0.4620(4) 0.055(3) Uani 0.832(5) 1 d PU A 1 H92A H -0.1980 0.3183 0.4387 0.083 Uiso 0.832(5) 1 calc PR A 1 H92B H -0.1267 0.2729 0.4405 0.083 Uiso 0.832(5) 1 calc PR A 1 H92C H -0.1387 0.3732 0.4687 0.083 Uiso 0.832(5) 1 calc PR A 1 O12B O -0.0299(12) 0.2119(17) 0.6356(10) 0.020(6) Uiso 0.168(5) 1 d PU A 2 C12B C -0.0583(12) 0.2967(14) 0.6340(11) 0.023(10) Uiso 0.168(5) 1 d PGU A 2 C22B C -0.1045(12) 0.3155(15) 0.6773(10) 0.032(9) Uiso 0.168(5) 1 d PGU A 2 H22B H -0.1157 0.2692 0.7053 0.038 Uiso 0.168(5) 1 calc PR A 2 C32B C -0.1342(12) 0.4022(17) 0.6797(10) 0.026(8) Uiso 0.168(5) 1 d PGU A 2 H32B H -0.1658 0.4150 0.7094 0.031 Uiso 0.168(5) 1 calc PR A 2 C42B C -0.1177(15) 0.4700(14) 0.6388(13) 0.08(3) Uiso 0.168(5) 1 d PGU A 2 H42B H -0.1380 0.5292 0.6404 0.097 Uiso 0.168(5) 1 calc PR A 2 C52B C -0.0715(15) 0.4512(16) 0.5954(11) 0.047(11) Uiso 0.168(5) 1 d PGU A 2 H52B H -0.0603 0.4976 0.5675 0.057 Uiso 0.168(5) 1 calc PR A 2 C62B C -0.0418(12) 0.3646(18) 0.5930(10) 0.030(9) Uiso 0.168(5) 1 d PGU A 2 C72B C 0.008(2) 0.352(3) 0.5464(18) 0.037(10) Uiso 0.168(5) 1 d PU A 2 N72B N 0.0324(15) 0.271(2) 0.5375(13) 0.020(6) Uiso 0.168(5) 1 d PU A 2 O72B O 0.0815(15) 0.262(2) 0.4948(12) 0.019(8) Uiso 0.168(5) 1 d PU A 2 C82B C 0.028(2) 0.432(3) 0.5084(17) 0.036(9) Uiso 0.168(5) 1 d PU A 2 H82C H 0.0751 0.4266 0.4979 0.043 Uiso 0.168(5) 1 calc PR A 2 H82D H 0.0219 0.4909 0.5301 0.043 Uiso 0.168(5) 1 calc PR A 2 C92B C -0.0140(19) 0.431(3) 0.4520(16) 0.034(9) Uiso 0.168(5) 1 d PU A 2 H92D H -0.0021 0.4840 0.4270 0.051 Uiso 0.168(5) 1 calc PR A 2 H92E H -0.0603 0.4357 0.4628 0.051 Uiso 0.168(5) 1 calc PR A 2 H92F H -0.0065 0.3733 0.4303 0.051 Uiso 0.168(5) 1 calc PR A 2 O1A O 0.0649(3) 0.2489(4) 0.5157(3) 0.0275(13) Uani 0.832(5) 1 d PDU A 1 C1A C 0.0411(4) 0.3353(5) 0.4946(4) 0.040(2) Uani 0.832(5) 1 d PDU A 1 H1A1 H 0.0243 0.3718 0.5278 0.061 Uiso 0.832(5) 1 calc PR A 1 H1A2 H 0.0058 0.3244 0.4662 0.061 Uiso 0.832(5) 1 calc PR A 1 H1A3 H 0.0766 0.3692 0.4753 0.061 Uiso 0.832(5) 1 calc PR A 1 O1B O -0.0709(16) 0.121(2) 0.5221(15) 0.035(10) Uiso 0.168(5) 1 d PDU A 2 C1B C -0.1268(17) 0.178(3) 0.5148(19) 0.042(10) Uiso 0.168(5) 1 d PDU A 2 H1B1 H -0.1354 0.2114 0.5514 0.063 Uiso 0.168(5) 1 calc PR A 2 H1B2 H -0.1646 0.1388 0.5050 0.063 Uiso 0.168(5) 1 calc PR A 2 H1B3 H -0.1190 0.2219 0.4827 0.063 Uiso 0.168(5) 1 calc PR A 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 Fe1 0.0309(5) 0.0224(4) 0.0215(4) 0.0028(3) -0.0019(4) -0.0045(4) Fe2 0.0282(5) 0.0204(4) 0.0222(4) 0.0020(3) -0.0028(4) -0.0028(4) Fe3 0.0367(5) 0.0320(5) 0.0238(4) -0.0017(4) 0.0012(4) 0.0138(4) O123 0.029(2) 0.018(2) 0.0216(19) 0.0023(16) -0.0022(17) -0.0007(17) O11 0.039(3) 0.048(3) 0.031(2) 0.019(2) -0.006(2) -0.019(2) C11 0.046(4) 0.025(3) 0.025(3) 0.003(3) 0.000(3) -0.001(3) C21 0.044(4) 0.029(3) 0.035(4) 0.002(3) 0.002(3) -0.002(3) C31 0.045(4) 0.030(4) 0.041(4) 0.001(3) 0.016(3) -0.003(3) C41 0.056(5) 0.035(4) 0.029(3) 0.007(3) 0.011(3) 0.002(4) C51 0.048(4) 0.027(3) 0.029(3) 0.009(3) -0.002(3) 0.001(3) C61 0.041(4) 0.018(3) 0.030(3) 0.002(2) -0.002(3) 0.001(3) C71 0.048(4) 0.026(3) 0.027(3) 0.005(3) -0.004(3) 0.002(3) N71 0.034(3) 0.024(3) 0.030(3) 0.007(2) -0.006(2) -0.005(2) O71 0.032(2) 0.032(2) 0.037(2) 0.013(2) -0.008(2) -0.006(2) C81 0.053(5) 0.072(6) 0.041(4) 0.031(4) -0.013(4) -0.010(4) C91 0.080(7) 0.114(9) 0.083(7) 0.040(7) -0.008(6) 0.029(7) C13 0.083(7) 0.053(5) 0.103(8) 0.006(5) 0.052(6) 0.010(5) O13 0.037(3) 0.037(3) 0.038(3) -0.012(2) 0.016(2) -0.007(2) C14 0.059(5) 0.040(4) 0.028(3) 0.002(3) 0.001(3) -0.012(4) O14 0.030(2) 0.035(2) 0.019(2) -0.0027(18) 0.0012(17) 0.004(2) S16 0.0247(8) 0.0265(8) 0.0240(7) 0.0009(6) -0.0019(6) 0.0005(6) O16 0.031(2) 0.039(3) 0.030(2) 0.007(2) -0.0062(19) 0.000(2) O26 0.027(2) 0.030(2) 0.028(2) 0.0032(18) 0.0000(18) -0.0025(19) O36 0.025(2) 0.025(2) 0.029(2) 0.0015(18) -0.0051(18) 0.0025(18) O46 0.032(2) 0.031(2) 0.025(2) -0.0024(18) 0.0012(18) 0.0014(19) N1 0.087(7) 0.082(7) 0.112(8) 0.038(6) -0.034(6) 0.014(6) C1 0.186(15) 0.078(8) 0.078(8) 0.031(7) -0.031(9) 0.009(9) C2 0.200(17) 0.100(10) 0.113(12) 0.030(9) 0.001(12) 0.001(11) C3 0.156(15) 0.084(10) 0.171(16) -0.040(11) -0.029(13) 0.016(10) C4 0.097(10) 0.091(9) 0.210(17) -0.045(11) 0.086(11) 0.005(8) C5 0.26(3) 0.092(13) 0.30(3) 0.008(17) -0.05(2) -0.019(16) C6 0.101(11) 0.086(10) 0.26(2) 0.021(12) -0.019(13) 0.017(9) O12A 0.042(3) 0.028(3) 0.033(3) -0.011(2) 0.000(2) 0.006(3) C12A 0.043(5) 0.027(4) 0.034(4) -0.004(3) 0.009(3) 0.001(4) C22A 0.056(6) 0.037(4) 0.046(5) -0.015(4) 0.002(4) 0.006(4) C32A 0.071(7) 0.042(5) 0.062(6) -0.021(5) 0.002(5) 0.010(5) C42A 0.060(7) 0.034(5) 0.066(7) -0.012(4) 0.008(4) 0.023(4) C52A 0.058(6) 0.036(4) 0.050(5) -0.005(4) 0.009(4) 0.014(4) C62A 0.042(4) 0.028(4) 0.038(4) 0.000(3) 0.013(3) 0.003(3) C72A 0.029(4) 0.034(4) 0.035(4) 0.000(3) 0.009(3) 0.004(3) N72A 0.031(3) 0.027(3) 0.023(3) -0.002(3) 0.002(3) -0.001(3) O72A 0.024(3) 0.026(3) 0.036(3) -0.002(2) 0.000(3) 0.003(3) C82A 0.027(4) 0.043(5) 0.051(5) 0.007(4) 0.000(3) 0.013(4) C92A 0.051(6) 0.065(6) 0.049(5) 0.011(5) -0.002(4) 0.019(5) O1A 0.034(4) 0.018(3) 0.031(3) -0.003(3) -0.002(3) -0.001(3) C1A 0.048(5) 0.030(4) 0.043(5) 0.007(4) 0.007(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 O72B 1.81(3) . ? Fe1 O11 1.882(4) . ? Fe1 O123 1.966(4) . ? Fe1 O1A 2.021(6) . ? Fe1 O26 2.067(4) . ? Fe1 O13 2.119(4) . ? Fe1 N71 2.131(5) . ? Fe2 O1B 1.93(3) . ? Fe2 O71 1.939(4) . ? Fe2 O123 1.983(4) . ? Fe2 O72A 2.007(5) . ? Fe2 O14 2.046(4) . ? Fe2 O123 2.058(4) 5_556 ? Fe2 O36 2.087(4) 5_556 ? Fe3 N72B 1.81(3) . ? Fe3 O12B 1.87(2) . ? Fe3 O12A 1.927(5) . ? Fe3 O14 1.971(4) 5_556 ? Fe3 O1A 2.048(7) . ? Fe3 N72A 2.056(6) . ? Fe3 O46 2.094(4) . ? Fe3 O123 2.103(4) . ? Fe3 O1B 2.28(3) . ? O123 Fe2 2.058(4) 5_556 ? O11 C11 1.330(6) . ? C11 C21 1.398(6) . ? C11 C61 1.402(6) . ? C21 C31 1.377(6) . ? C21 H21 0.9500 . ? C31 C41 1.382(7) . ? C31 H31 0.9500 . ? C41 C51 1.381(7) . ? C41 H41 0.9500 . ? C51 C61 1.401(6) . ? C51 H51 0.9500 . ? C61 C71 1.483(7) . ? C71 N71 1.306(7) . ? C71 C81 1.496(9) . ? N71 O71 1.372(6) . ? C81 C91 1.486(13) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C13 O13 1.383(9) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O13 H13D 0.9900 . ? C14 O14 1.414(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O14 Fe3 1.971(4) 5_556 ? S16 O16 1.455(4) . ? S16 O46 1.468(4) . ? S16 O26 1.486(4) . ? S16 O36 1.488(4) . ? O36 Fe2 2.087(4) 5_556 ? N1 C5 1.44(2) . ? N1 C3 1.505(16) . ? N1 C1 1.632(16) . ? N1 H1 0.9000 . ? C1 C2 1.474(17) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.455(18) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.32(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O12A C12A 1.337(5) . ? C12A C22A 1.3900 . ? C12A C62A 1.3900 . ? C22A C32A 1.3900 . ? C22A H22A 0.9500 . ? C32A C42A 1.3900 . ? C32A H32A 0.9500 . ? C42A C52A 1.3900 . ? C42A H42A 0.9500 . ? C52A C62A 1.3900 . ? C52A H52A 0.9500 . ? C62A C72A 1.488(7) . ? C72A N72A 1.304(8) . ? C72A C82A 1.503(10) . ? N72A O72A 1.370(7) . ? C82A C92A 1.525(12) . ? C82A H82A 0.9900 . ? C82A H82B 0.9900 . ? C92A H92A 0.9800 . ? C92A H92B 0.9800 . ? C92A H92C 0.9800 . ? O12B C12B 1.35(3) . ? C12B C22B 1.3900 . ? C12B C62B 1.3900 . ? C22B C32B 1.3900 . ? C22B H22B 0.9500 . ? C32B C42B 1.3900 . ? C32B H32B 0.9500 . ? C42B C52B 1.3900 . ? C42B H42B 0.9500 . ? C52B C62B 1.3900 . ? C52B H52B 0.9500 . ? C62B C72B 1.49(4) . ? C72B N72B 1.28(5) . ? C72B C82B 1.50(5) . ? N72B O72B 1.40(4) . ? C82B C92B 1.55(5) . ? C82B H82C 0.9900 . ? C82B H82D 0.9900 . ? C92B H92D 0.9800 . ? C92B H92E 0.9800 . ? C92B H92F 0.9800 . ? O1A C1A 1.420(9) . ? C1A H1A1 0.9800 . ? C1A H1A2 0.9800 . ? C1A H1A3 0.9800 . ? O1B C1B 1.42(2) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O72B Fe1 O11 84.7(9) . . ? O72B Fe1 O123 97.4(9) . . ? O11 Fe1 O123 175.39(17) . . ? O72B Fe1 O1A 17.2(8) . . ? O11 Fe1 O1A 101.6(2) . . ? O123 Fe1 O1A 80.8(2) . . ? O72B Fe1 O26 97.0(9) . . ? O11 Fe1 O26 92.36(17) . . ? O123 Fe1 O26 91.46(16) . . ? O1A Fe1 O26 92.7(2) . . ? O72B Fe1 O13 174.9(9) . . ? O11 Fe1 O13 90.9(2) . . ? O123 Fe1 O13 86.80(16) . . ? O1A Fe1 O13 167.5(2) . . ? O26 Fe1 O13 85.70(18) . . ? O72B Fe1 N71 87.6(9) . . ? O11 Fe1 N71 85.54(18) . . ? O123 Fe1 N71 90.44(17) . . ? O1A Fe1 N71 92.4(2) . . ? O26 Fe1 N71 174.72(19) . . ? O13 Fe1 N71 89.5(2) . . ? O1B Fe2 O71 94.5(10) . . ? O1B Fe2 O123 75.0(10) . . ? O71 Fe2 O123 92.11(16) . . ? O1B Fe2 O72A 18.0(9) . . ? O71 Fe2 O72A 95.5(2) . . ? O123 Fe2 O72A 92.9(2) . . ? O1B Fe2 O14 169.8(9) . . ? O71 Fe2 O14 92.52(18) . . ? O123 Fe2 O14 97.36(16) . . ? O72A Fe2 O14 166.7(2) . . ? O1B Fe2 O123 95.2(10) . 5_556 ? O71 Fe2 O123 167.64(18) . 5_556 ? O123 Fe2 O123 83.00(16) . 5_556 ? O72A Fe2 O123 96.06(19) . 5_556 ? O14 Fe2 O123 76.94(16) . 5_556 ? O1B Fe2 O36 98.2(10) . 5_556 ? O71 Fe2 O36 97.07(17) . 5_556 ? O123 Fe2 O36 169.01(16) . 5_556 ? O72A Fe2 O36 80.2(2) . 5_556 ? O14 Fe2 O36 88.30(16) . 5_556 ? O123 Fe2 O36 89.15(16) 5_556 5_556 ? N72B Fe3 O12B 94.4(13) . . ? N72B Fe3 O12A 76.6(10) . . ? O12B Fe3 O12A 26.4(8) . . ? N72B Fe3 O14 173.0(9) . 5_556 ? O12B Fe3 O14 88.3(8) . 5_556 ? O12A Fe3 O14 108.1(2) . 5_556 ? N72B Fe3 O1A 25.7(10) . . ? O12B Fe3 O1A 119.1(8) . . ? O12A Fe3 O1A 97.8(2) . . ? O14 Fe3 O1A 152.6(2) 5_556 . ? N72B Fe3 N72A 81.2(10) . . ? O12B Fe3 N72A 69.2(8) . . ? O12A Fe3 N72A 85.7(2) . . ? O14 Fe3 N72A 93.8(2) 5_556 . ? O1A Fe3 N72A 97.2(2) . . ? N72B Fe3 O46 99.3(9) . . ? O12B Fe3 O46 104.7(8) . . ? O12A Fe3 O46 88.5(2) . . ? O14 Fe3 O46 86.16(17) 5_556 . ? O1A Fe3 O46 85.5(2) . . ? N72A Fe3 O46 173.81(19) . . ? N72B Fe3 O123 97.6(10) . . ? O12B Fe3 O123 155.8(8) . . ? O12A Fe3 O123 173.98(19) . . ? O14 Fe3 O123 77.56(15) 5_556 . ? O1A Fe3 O123 77.00(19) . . ? N72A Fe3 O123 92.03(19) . . ? O46 Fe3 O123 94.02(16) . . ? N72B Fe3 O1B 95.8(12) . . ? O12B Fe3 O1B 92.3(12) . . ? O12A Fe3 O1B 113.0(9) . . ? O14 Fe3 O1B 77.7(9) 5_556 . ? O1A Fe3 O1B 100.8(9) . . ? N72A Fe3 O1B 28.6(8) . . ? O46 Fe3 O1B 156.2(8) . . ? O123 Fe3 O1B 65.7(9) . . ? Fe1 O123 Fe2 114.87(18) . . ? Fe1 O123 Fe2 134.5(2) . 5_556 ? Fe2 O123 Fe2 97.00(16) . 5_556 ? Fe1 O123 Fe3 98.51(16) . . ? Fe2 O123 Fe3 112.05(19) . . ? Fe2 O123 Fe3 98.39(16) 5_556 . ? C11 O11 Fe1 134.6(4) . . ? O11 C11 C21 116.2(5) . . ? O11 C11 C61 124.0(5) . . ? C21 C11 C61 119.8(5) . . ? C31 C21 C11 121.2(6) . . ? C31 C21 H21 119.4 . . ? C11 C21 H21 119.4 . . ? C21 C31 C41 119.4(6) . . ? C21 C31 H31 120.3 . . ? C41 C31 H31 120.3 . . ? C51 C41 C31 120.3(5) . . ? C51 C41 H41 119.9 . . ? C31 C41 H41 119.9 . . ? C41 C51 C61 121.4(5) . . ? C41 C51 H51 119.3 . . ? C61 C51 H51 119.3 . . ? C51 C61 C11 118.0(5) . . ? C51 C61 C71 118.5(5) . . ? C11 C61 C71 123.5(5) . . ? N71 C71 C61 120.4(5) . . ? N71 C71 C81 118.4(6) . . ? C61 C71 C81 121.1(5) . . ? C71 N71 O71 115.2(5) . . ? C71 N71 Fe1 130.4(4) . . ? O71 N71 Fe1 114.3(3) . . ? N71 O71 Fe2 118.1(3) . . ? C91 C81 C71 114.1(8) . . ? C91 C81 H81A 108.7 . . ? C71 C81 H81A 108.7 . . ? C91 C81 H81B 108.7 . . ? C71 C81 H81B 108.7 . . ? H81A C81 H81B 107.6 . . ? C81 C91 H91A 109.5 . . ? C81 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C81 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? O13 C13 H13A 109.5 . . ? O13 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O13 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C13 O13 Fe1 126.1(5) . . ? C13 O13 H13D 105.4 . . ? Fe1 O13 H13D 105.5 . . ? O14 C14 H14A 109.5 . . ? O14 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O14 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C14 O14 Fe3 119.7(4) . 5_556 ? C14 O14 Fe2 125.7(4) . . ? Fe3 O14 Fe2 103.23(18) 5_556 . ? O16 S16 O46 110.3(3) . . ? O16 S16 O26 110.2(2) . . ? O46 S16 O26 108.3(2) . . ? O16 S16 O36 108.6(2) . . ? O46 S16 O36 109.7(2) . . ? O26 S16 O36 109.8(2) . . ? S16 O26 Fe1 124.4(2) . . ? S16 O36 Fe2 126.3(2) . 5_556 ? S16 O46 Fe3 120.6(2) . . ? C5 N1 C3 113.1(14) . . ? C5 N1 C1 109.9(12) . . ? C3 N1 C1 107.1(11) . . ? C5 N1 H1 108.9 . . ? C3 N1 H1 108.9 . . ? C1 N1 H1 108.9 . . ? C2 C1 N1 111.0(11) . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N1 C1 H1B 109.4 . . ? H1A C1 H1B 108.0 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 N1 113.5(11) . . ? C4 C3 H3A 108.9 . . ? N1 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? N1 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 N1 111.6(18) . . ? C6 C5 H5A 109.3 . . ? N1 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? N1 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12A O12A Fe3 129.4(4) . . ? O12A C12A C22A 116.0(4) . . ? O12A C12A C62A 124.0(4) . . ? C22A C12A C62A 120.0 . . ? C32A C22A C12A 120.0 . . ? C32A C22A H22A 120.0 . . ? C12A C22A H22A 120.0 . . ? C22A C32A C42A 120.0 . . ? C22A C32A H32A 120.0 . . ? C42A C32A H32A 120.0 . . ? C52A C42A C32A 120.0 . . ? C52A C42A H42A 120.0 . . ? C32A C42A H42A 120.0 . . ? C62A C52A C42A 120.0 . . ? C62A C52A H52A 120.0 . . ? C42A C52A H52A 120.0 . . ? C52A C62A C12A 120.0 . . ? C52A C62A C72A 117.1(4) . . ? C12A C62A C72A 122.6(4) . . ? N72A C72A C62A 120.5(6) . . ? N72A C72A C82A 119.4(6) . . ? C62A C72A C82A 119.9(6) . . ? C72A N72A O72A 117.2(6) . . ? C72A N72A Fe3 129.7(5) . . ? O72A N72A Fe3 113.1(4) . . ? N72A O72A Fe2 119.7(5) . . ? C72A C82A C92A 108.4(7) . . ? C72A C82A H82A 110.0 . . ? C92A C82A H82A 110.0 . . ? C72A C82A H82B 110.0 . . ? C92A C82A H82B 110.0 . . ? H82A C82A H82B 108.4 . . ? C82A C92A H92A 109.5 . . ? C82A C92A H92B 109.5 . . ? H92A C92A H92B 109.5 . . ? C82A C92A H92C 109.5 . . ? H92A C92A H92C 109.5 . . ? H92B C92A H92C 109.5 . . ? C12B O12B Fe3 124.4(18) . . ? O12B C12B C22B 116.6(19) . . ? O12B C12B C62B 123.3(19) . . ? C22B C12B C62B 120.0 . . ? C32B C22B C12B 120.0 . . ? C32B C22B H22B 120.0 . . ? C12B C22B H22B 120.0 . . ? C42B C32B C22B 120.0 . . ? C42B C32B H32B 120.0 . . ? C22B C32B H32B 120.0 . . ? C32B C42B C52B 120.0 . . ? C32B C42B H42B 120.0 . . ? C52B C42B H42B 120.0 . . ? C62B C52B C42B 120.0 . . ? C62B C52B H52B 120.0 . . ? C42B C52B H52B 120.0 . . ? C52B C62B C12B 120.0 . . ? C52B C62B C72B 116(2) . . ? C12B C62B C72B 124(2) . . ? N72B C72B C62B 119(3) . . ? N72B C72B C82B 120(4) . . ? C62B C72B C82B 120(3) . . ? C72B N72B O72B 118(3) . . ? C72B N72B Fe3 132(3) . . ? O72B N72B Fe3 109(2) . . ? N72B O72B Fe1 124(2) . . ? C72B C82B C92B 108(3) . . ? C72B C82B H82C 110.0 . . ? C92B C82B H82C 110.0 . . ? C72B C82B H82D 110.0 . . ? C92B C82B H82D 110.0 . . ? H82C C82B H82D 108.4 . . ? C82B C92B H92D 109.5 . . ? C82B C92B H92E 109.5 . . ? H92D C92B H92E 109.5 . . ? C82B C92B H92F 109.5 . . ? H92D C92B H92F 109.5 . . ? H92E C92B H92F 109.5 . . ? C1A O1A Fe1 122.3(6) . . ? C1A O1A Fe3 127.2(6) . . ? Fe1 O1A Fe3 98.5(2) . . ? O1A C1A H1A1 109.5 . . ? O1A C1A H1A2 109.5 . . ? H1A1 C1A H1A2 109.5 . . ? O1A C1A H1A3 109.5 . . ? H1A1 C1A H1A3 109.5 . . ? H1A2 C1A H1A3 109.5 . . ? C1B O1B Fe2 118(3) . . ? C1B O1B Fe3 125(3) . . ? Fe2 O1B Fe3 106.9(14) . . ? O1B C1B H1B1 109.5 . . ? O1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? O1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.242 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.100