Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'S. Aldridge' _publ_contact_author_address ; Inorganic Chemistry Oxford University South Parks Road Oxford OX1 3QR UNITED KINGDOM ; _publ_contact_author_email SIMON.ALDRIDGE@CHEM.OX.AC.UK _publ_section_title ; Synthesis of polymeric and macrocyclic Lewis acids: influence of backbone on degree of aggregation ; loop_ _publ_author_name 'S. Aldridge' 'C. Bresner' 'Simon Coles' 'Andrew Cowley' 'Joanne K. Day' 'Ian Fallis' 'Louise Male' # Attachment '2_revised.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 645159' _publ_section_exptl_refinement # Some potentially useful phrases are donated by Bill Clegg: ; The H atoms were all located in a difference map, but those attached to carbon atoms were repositioned geometrically. The H atoms were initially refined with soft restraints on the bond lengths and angles to regularise their geometry (C---H in the range 0.93--0.98\%A) and U~iso~(H) (in the range 1.2-1.5 times U~eq~ of the parent atom), after which the positions were refined with riding constraints. ; _publ_section_exptl_prep # Brief details or a reference. Include solvent if known ; ? ; _cell_length_a 11.9633(6) _cell_length_b 9.9176(5) _cell_length_c 13.4452(6) _cell_angle_alpha 90 _cell_angle_beta 114.899(3) _cell_angle_gamma 90 _cell_volume 1446.96(13) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-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' B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403 -0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C30 H32 B4 Fe2 O8 # Dc = 1.55 Fooo = 696.00 Mu = 10.55 M = 675.52 # Found Formula = C30 H32 B4 Fe2 O8 # Dc = 1.55 FOOO = 696.00 Mu = 10.55 M = 675.52 _chemical_formula_sum 'C30 H32 B4 Fe2 O8' _chemical_formula_moiety 'C30 H32 B4 Fe2 O8' _chemical_compound_source ? _chemical_formula_weight 675.52 _cell_measurement_reflns_used 1684 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description lath _exptl_crystal_colour colourless _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.055 # Sheldrick geometric approximatio 0.81 0.90 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.79 _exptl_absorpt_correction_T_max 0.90 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device_type 'Nonius KappaCCD' _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 'COLLECT (Nonius, 1997-2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'USER DEFINED STRUCTURE SOLUTION' _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 19546 _reflns_number_total 4291 _diffrn_reflns_av_R_equivalents 0.039 # Number of reflections with Friedels Law is 3181 # Number of reflections without Friedels Law is 4291 # Theoretical number of reflections is about 3311 _reflns_Friedel_coverage 0.22 _diffrn_reflns_theta_min 5.131 _diffrn_reflns_theta_max 27.460 _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 25.263 _diffrn_measured_fraction_theta_full 0.941 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -15 _reflns_limit_h_max 13 _reflns_limit_k_min -12 _reflns_limit_k_max 9 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 1.49 _oxford_diffrn_Wilson_scale 10.12 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.73 _refine_diff_density_max 0.65 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>-3.0\s(I) _refine_ls_number_reflns 4043 _refine_ls_number_restraints 1 _refine_ls_number_parameters 398 _oxford_refine_ls_R_factor_ref 0.0474 _refine_ls_wR_factor_ref 0.0939 _refine_ls_goodness_of_fit_ref 0.9908 _refine_ls_shift/su_max 0.008856 # The values computed from all data _oxford_reflns_number_all 4043 _refine_ls_R_factor_all 0.0474 _refine_ls_wR_factor_all 0.0939 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 3623 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_gt 0.0882 _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_abs_structure_details 'Flack (1983), 785 Friedel-pairs' # 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 ad _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= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.00P)^2^ + 1.48P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; User-defined structure solution reference Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (1997-2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atomsattached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _oxford_atom_site_special_shape _atom_site_attached_hydrogens Fe1 Fe 0.63937(6) 0.57543(11) 0.61400(5) 0.0211 1.0000 Uani . . . . . . . C2 C 0.7115(4) 0.5117(5) 0.7747(3) 0.0231 1.0000 Uani . . . . . . . C3 C 0.7673(5) 0.6349(5) 0.7648(4) 0.0290 1.0000 Uani . . . . . . . C4 C 0.6751(5) 0.7359(5) 0.7198(4) 0.0322 1.0000 Uani . . . . . . . C5 C 0.5599(5) 0.6763(6) 0.7002(4) 0.0330 1.0000 Uani . . . . . . . C6 C 0.5822(4) 0.5395(5) 0.7333(3) 0.0274 1.0000 Uani . . . . . . . C7 C 0.7281(4) 0.5211(5) 0.5183(3) 0.0222 1.0000 Uani . . . . . . . C8 C 0.6528(5) 0.6373(5) 0.4741(3) 0.0264 1.0000 Uani . . . . . . . C9 C 0.5280(5) 0.6047(5) 0.4505(4) 0.0283 1.0000 Uani . . . . . . . C10 C 0.5244(4) 0.4684(5) 0.4797(4) 0.0292 1.0000 Uani . . . . . . . C11 C 0.6459(5) 0.4161(5) 0.5203(3) 0.0251 1.0000 Uani . . . . . . . B12 B 0.8676(5) 0.5087(6) 0.5561(3) 0.0212 1.0000 Uani . . . . . . . O13 O 0.9188(3) 0.3821(3) 0.5748(2) 0.0249 1.0000 Uani . . . . . . . C14 C 1.0472(4) 0.3677(6) 0.5983(4) 0.0247 1.0000 Uani . . . . . . . C15 C 1.1224(4) 0.4875(5) 0.6626(3) 0.0191 1.0000 Uani . . . . . . . C16 C 1.2537(5) 0.4789(5) 0.6734(4) 0.0287 1.0000 Uani . . . . . . . O17 O 1.3218(3) 0.3726(4) 0.7432(2) 0.0273 1.0000 Uani . . . . . . . C18 C 1.0662(5) 0.6166(6) 0.5999(4) 0.0293 1.0000 Uani . . . . . . . O19 O 0.9346(3) 0.6239(3) 0.5679(3) 0.0259 1.0000 Uani . . . . . . . C20 C 1.1269(4) 0.4919(5) 0.7781(3) 0.0214 1.0000 Uani . . . . . . . O21 O 1.1970(3) 0.3817(3) 0.8448(2) 0.0251 1.0000 Uani . . . . . . . O121 O 0.8981(3) 0.3630(3) 0.8531(2) 0.0253 1.0000 Uani . . . . . . . C120 C 0.9581(5) 0.2370(5) 0.8997(4) 0.0273 1.0000 Uani . . . . . . . C115 C 0.8761(4) 0.1164(5) 0.8419(4) 0.0216 1.0000 Uani . . . . . . . C114 C 0.8632(4) 0.1042(5) 0.7249(3) 0.0244 1.0000 Uani . . . . . . . O113 O 0.9773(3) 0.0634(4) 0.7213(2) 0.0286 1.0000 Uani . . . . . . . B112 B 1.0565(5) -0.0182(6) 0.8018(4) 0.0248 1.0000 Uani . . . . . . . C107 C 1.1734(4) -0.0682(5) 0.7909(3) 0.0229 1.0000 Uani . . . . . . . C111 C 1.2177(4) -0.0216(5) 0.7127(3) 0.0233 1.0000 Uani . . . . . . . Fe101 Fe 1.34794(6) 0.01285(11) 0.86851(5) 0.0199 1.0000 Uani . . . . . . . C110 C 1.3281(5) -0.0910(5) 0.7302(4) 0.0280 1.0000 Uani . . . . . . . C109 C 1.3553(5) -0.1805(5) 0.8199(4) 0.0268 1.0000 Uani . . . . . . . C108 C 1.2610(4) -0.1654(5) 0.8580(4) 0.0244 1.0000 Uani . . . . . . . C102 C 1.3715(4) 0.2157(5) 0.9018(4) 0.0236 1.0000 Uani . . . . . . . C106 C 1.4792(4) 0.1577(5) 0.8951(4) 0.0241 1.0000 Uani . . . . . . . C105 C 1.5263(4) 0.0537(5) 0.9746(3) 0.0283 1.0000 Uani . . . . . . . C104 C 1.4494(4) 0.0443(5) 1.0319(3) 0.0261 1.0000 Uani . . . . . . . C103 C 1.3564(4) 0.1445(5) 0.9878(3) 0.0255 1.0000 Uani . . . . . . . O119 O 1.0373(3) -0.0594(4) 0.8898(2) 0.0289 1.0000 Uani . . . . . . . C118 C 0.9305(5) -0.0143(5) 0.9035(4) 0.0249 1.0000 Uani . . . . . . . C116 C 0.7515(5) 0.1357(5) 0.8449(4) 0.0258 1.0000 Uani . . . . . . . O117 O 0.6989(3) 0.2656(3) 0.8068(3) 0.0278 1.0000 Uani . . . . . . . B122 B 0.7733(5) 0.3735(6) 0.8135(4) 0.0221 1.0000 Uani . . . . . . . B22 B 1.2921(5) 0.3278(6) 0.8264(4) 0.0229 1.0000 Uani . . . . . . . H31 H 0.8549 0.6474 0.7848 0.0329 1.0000 Uiso R . . . . . . H41 H 0.6885 0.8288 0.7047 0.0362 1.0000 Uiso R . . . . . . H51 H 0.4790 0.7192 0.6646 0.0412 1.0000 Uiso R . . . . . . H61 H 0.5195 0.4739 0.7283 0.0340 1.0000 Uiso R . . . . . . H81 H 0.6810 0.7247 0.4626 0.0317 1.0000 Uiso R . . . . . . H91 H 0.4572 0.6662 0.4207 0.0340 1.0000 Uiso R . . . . . . H101 H 0.4503 0.4192 0.4734 0.0351 1.0000 Uiso R . . . . . . H111 H 0.6718 0.3252 0.5486 0.0300 1.0000 Uiso R . . . . . . H141 H 1.0782 0.2858 0.6413 0.0299 1.0000 Uiso R . . . . . . H142 H 1.0556 0.3596 0.5298 0.0304 1.0000 Uiso R . . . . . . H161 H 1.2955 0.5636 0.7015 0.0350 1.0000 Uiso R . . . . . . H162 H 1.2501 0.4622 0.6010 0.0347 1.0000 Uiso R . . . . . . H181 H 1.1057 0.6935 0.6467 0.0341 1.0000 Uiso R . . . . . . H182 H 1.0798 0.6191 0.5334 0.0342 1.0000 Uiso R . . . . . . H201 H 1.1658 0.5766 0.8125 0.0260 1.0000 Uiso R . . . . . . H202 H 1.0431 0.4899 0.7730 0.0261 1.0000 Uiso R . . . . . . H1201 H 0.9771 0.2347 0.9773 0.0320 1.0000 Uiso R . . . . . . H1202 H 1.0345 0.2312 0.8906 0.0313 1.0000 Uiso R . . . . . . H1141 H 0.8373 0.1912 0.6891 0.0270 1.0000 Uiso R . . . . . . H1142 H 0.7997 0.0385 0.6859 0.0279 1.0000 Uiso R . . . . . . H1111 H 1.1775 0.0465 0.6569 0.0268 1.0000 Uiso R . . . . . . H1101 H 1.3780 -0.0761 0.6898 0.0338 1.0000 Uiso R . . . . . . H1091 H 1.4260 -0.2400 0.8515 0.0288 1.0000 Uiso R . . . . . . H1081 H 1.2579 -0.2116 0.9205 0.0322 1.0000 Uiso R . . . . . . H1061 H 1.5143 0.1851 0.8443 0.0281 1.0000 Uiso R . . . . . . H1051 H 1.5971 -0.0057 0.9875 0.0321 1.0000 Uiso R . . . . . . H1041 H 1.4610 -0.0176 1.0917 0.0303 1.0000 Uiso R . . . . . . H1031 H 1.2910 0.1577 1.0117 0.0293 1.0000 Uiso R . . . . . . H1181 H 0.9549 -0.0004 0.9823 0.0320 1.0000 Uiso R . . . . . . H1182 H 0.8687 -0.0858 0.8758 0.0320 1.0000 Uiso R . . . . . . H1161 H 0.7615 0.1244 0.9199 0.0307 1.0000 Uiso R . . . . . . H1162 H 0.6951 0.0671 0.7981 0.0309 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 0.0221(3) 0.0191(4) 0.0218(3) -0.0005(3) 0.0089(3) 0.0013(3) C2 0.028(2) 0.019(2) 0.0212(18) -0.005(2) 0.0093(18) -0.002(2) C3 0.032(3) 0.022(3) 0.025(2) -0.004(2) 0.004(2) -0.003(2) C4 0.048(3) 0.021(3) 0.025(2) -0.004(2) 0.013(2) 0.004(3) C5 0.041(3) 0.032(3) 0.026(2) 0.002(2) 0.014(2) 0.014(3) C6 0.029(2) 0.029(3) 0.026(2) 0.000(2) 0.0136(19) 0.006(2) C7 0.023(2) 0.025(2) 0.0176(17) -0.005(2) 0.0078(17) -0.003(2) C8 0.034(3) 0.024(3) 0.022(2) 0.002(2) 0.013(2) 0.001(2) C9 0.024(3) 0.036(4) 0.023(2) -0.001(2) 0.008(2) 0.008(2) C10 0.020(3) 0.036(3) 0.028(2) -0.004(2) 0.007(2) -0.002(2) C11 0.032(3) 0.021(3) 0.021(2) -0.006(2) 0.010(2) -0.005(2) B12 0.025(3) 0.022(3) 0.0198(19) 0.004(2) 0.013(2) 0.005(3) O13 0.0203(17) 0.0193(17) 0.0316(16) -0.0022(14) 0.0075(14) 0.0006(15) C14 0.018(3) 0.030(3) 0.027(2) -0.002(2) 0.010(2) 0.001(2) C15 0.017(2) 0.015(3) 0.0264(19) -0.0006(19) 0.0097(18) -0.001(2) C16 0.028(3) 0.026(3) 0.032(2) 0.005(2) 0.012(2) 0.005(2) O17 0.0237(17) 0.0255(19) 0.0339(16) 0.0093(15) 0.0133(14) 0.0040(16) C18 0.024(3) 0.023(3) 0.037(3) 0.006(2) 0.009(2) -0.002(2) O19 0.0265(19) 0.0169(17) 0.0343(17) 0.0061(14) 0.0129(16) 0.0036(15) C20 0.018(2) 0.016(3) 0.0276(19) 0.000(2) 0.0065(17) -0.001(2) O21 0.0255(17) 0.0244(18) 0.0263(15) 0.0033(14) 0.0118(14) 0.0036(15) O121 0.0270(18) 0.0175(17) 0.0280(15) 0.0034(14) 0.0084(14) 0.0024(15) C120 0.038(3) 0.019(3) 0.022(2) 0.001(2) 0.010(2) 0.004(2) C115 0.019(2) 0.020(3) 0.025(2) 0.0046(19) 0.0083(19) 0.003(2) C114 0.017(2) 0.021(3) 0.028(2) 0.000(2) 0.0029(18) 0.002(2) O113 0.0268(17) 0.0334(19) 0.0261(14) 0.0023(16) 0.0116(13) 0.0066(17) B112 0.024(3) 0.024(3) 0.024(2) -0.005(2) 0.007(2) -0.001(2) C107 0.021(2) 0.022(3) 0.022(2) -0.0034(19) 0.0054(19) 0.000(2) C111 0.023(2) 0.023(3) 0.0193(18) -0.0009(18) 0.0038(17) 0.007(2) Fe101 0.0217(4) 0.0172(4) 0.0202(3) 0.0007(3) 0.0084(2) 0.0019(3) C110 0.033(3) 0.027(3) 0.023(2) -0.001(2) 0.011(2) 0.008(2) C109 0.024(3) 0.023(3) 0.027(2) -0.004(2) 0.004(2) 0.007(2) C108 0.028(3) 0.017(2) 0.028(2) 0.0002(19) 0.012(2) 0.001(2) C102 0.022(2) 0.018(3) 0.031(2) -0.004(2) 0.010(2) -0.002(2) C106 0.020(2) 0.021(3) 0.029(2) 0.003(2) 0.0078(19) 0.001(2) C105 0.021(2) 0.029(3) 0.027(2) 0.005(2) 0.0020(18) 0.007(2) C104 0.032(3) 0.025(3) 0.0176(18) -0.0015(19) 0.0070(18) -0.001(2) C103 0.021(3) 0.027(3) 0.024(2) -0.001(2) 0.0059(19) 0.001(2) O119 0.0266(19) 0.028(2) 0.0335(16) 0.0087(15) 0.0145(15) 0.0061(16) C118 0.019(2) 0.026(3) 0.032(2) 0.006(2) 0.0131(19) 0.003(2) C116 0.021(2) 0.024(3) 0.033(2) 0.006(2) 0.011(2) -0.001(2) O117 0.0234(18) 0.0210(18) 0.0419(18) 0.0067(15) 0.0167(16) 0.0036(15) B122 0.022(3) 0.022(3) 0.019(2) -0.001(2) 0.006(2) 0.006(2) B22 0.020(3) 0.020(3) 0.024(2) -0.002(2) 0.006(2) -0.004(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.3263(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C2 . 2.059(4) no Fe1 . C3 . 2.046(5) no Fe1 . C4 . 2.056(5) no Fe1 . C5 . 2.044(5) no Fe1 . C6 . 2.023(4) no Fe1 . C7 . 2.055(4) no Fe1 . C8 . 2.048(4) no Fe1 . C9 . 2.056(5) no Fe1 . C10 . 2.046(5) no Fe1 . C11 . 2.043(5) no C2 . C3 . 1.425(7) no C2 . C6 . 1.433(6) no C2 . B122 . 1.540(7) no C3 . C4 . 1.423(7) no C3 . H31 . 0.975 no C4 . C5 . 1.419(8) no C4 . H41 . 0.971 no C5 . C6 . 1.418(7) no C5 . H51 . 0.978 no C6 . H61 . 0.973 no C7 . C8 . 1.429(7) no C7 . C11 . 1.440(7) no C7 . B12 . 1.531(6) no C8 . C9 . 1.427(7) no C8 . H81 . 0.967 no C9 . C10 . 1.414(7) no C9 . H91 . 0.982 no C10 . C11 . 1.418(7) no C10 . H101 . 0.984 no C11 . H111 . 0.977 no B12 . O13 . 1.372(6) no B12 . O19 . 1.366(7) no O13 . C14 . 1.440(6) no C14 . C15 . 1.521(7) no C14 . H141 . 0.975 no C14 . H142 . 0.970 no C15 . C16 . 1.519(7) no C15 . C18 . 1.524(7) no C15 . C20 . 1.531(6) no C16 . O17 . 1.418(6) no C16 . H161 . 0.969 no C16 . H162 . 0.970 no O17 . B22 . 1.383(6) no C18 . O19 . 1.449(6) no C18 . H181 . 0.975 no C18 . H182 . 0.974 no C20 . O21 . 1.438(6) no C20 . H201 . 0.977 no C20 . H202 . 0.975 no O21 . B22 . 1.371(6) no O121 . C120 . 1.445(6) no O121 . B122 . 1.362(6) no C120 . C115 . 1.534(7) no C120 . H1201 . 0.969 no C120 . H1202 . 0.974 no C115 . C114 . 1.520(6) no C115 . C118 . 1.529(6) no C115 . C116 . 1.520(7) no C114 . O113 . 1.444(5) no C114 . H1141 . 0.973 no C114 . H1142 . 0.970 no O113 . B112 . 1.364(6) no B112 . C107 . 1.549(7) no B112 . O119 . 1.360(6) no C107 . C111 . 1.438(6) no C107 . Fe101 . 2.064(5) no C107 . C108 . 1.430(6) no C111 . Fe101 . 2.046(4) no C111 . C110 . 1.418(7) no C111 . H1111 . 0.973 no Fe101 . C110 . 2.050(4) no Fe101 . C109 . 2.040(5) no Fe101 . C108 . 2.025(5) no Fe101 . C102 . 2.055(5) no Fe101 . C106 . 2.046(5) no Fe101 . C105 . 2.047(5) no Fe101 . C104 . 2.037(4) no Fe101 . C103 . 2.037(5) no C110 . C109 . 1.420(7) no C110 . H1101 . 0.974 no C109 . C108 . 1.430(7) no C109 . H1091 . 0.971 no C108 . H1081 . 0.971 no C102 . C106 . 1.448(7) no C102 . C103 . 1.429(7) no C102 . B22 . 1.534(7) no C106 . C105 . 1.420(6) no C106 . H1061 . 0.978 no C105 . C104 . 1.430(6) no C105 . H1051 . 0.985 no C104 . C103 . 1.422(7) no C104 . H1041 . 0.975 no C103 . H1031 . 0.972 no O119 . C118 . 1.437(6) no C118 . H1181 . 0.982 no C118 . H1182 . 0.978 no C116 . O117 . 1.431(6) no C116 . H1161 . 0.971 no C116 . H1162 . 0.978 no O117 . B122 . 1.371(7) no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C2 . Fe1 . C3 . 40.61(19) no C2 . Fe1 . C4 . 68.8(2) no C3 . Fe1 . C4 . 40.6(2) no C2 . Fe1 . C5 . 69.18(19) no C3 . Fe1 . C5 . 68.2(2) no C4 . Fe1 . C5 . 40.5(2) no C2 . Fe1 . C6 . 41.09(18) no C3 . Fe1 . C6 . 68.1(2) no C4 . Fe1 . C6 . 68.2(2) no C5 . Fe1 . C6 . 40.8(2) no C2 . Fe1 . C7 . 118.54(18) no C3 . Fe1 . C7 . 109.16(19) no C4 . Fe1 . C7 . 128.6(2) no C5 . Fe1 . C7 . 165.9(2) no C6 . Fe1 . C7 . 152.5(2) no C2 . Fe1 . C8 . 153.54(19) no C3 . Fe1 . C8 . 120.6(2) no C4 . Fe1 . C8 . 109.2(2) no C5 . Fe1 . C8 . 127.5(2) no C6 . Fe1 . C8 . 164.68(19) no C2 . Fe1 . C9 . 164.1(2) no C3 . Fe1 . C9 . 153.7(2) no C4 . Fe1 . C9 . 118.9(2) no C5 . Fe1 . C9 . 106.9(2) no C6 . Fe1 . C9 . 126.11(19) no C2 . Fe1 . C10 . 126.5(2) no C3 . Fe1 . C10 . 165.5(2) no C4 . Fe1 . C10 . 151.5(2) no C5 . Fe1 . C10 . 117.0(2) no C6 . Fe1 . C10 . 106.4(2) no C2 . Fe1 . C11 . 107.6(2) no C3 . Fe1 . C11 . 128.8(2) no C4 . Fe1 . C11 . 167.1(2) no C5 . Fe1 . C11 . 151.2(2) no C6 . Fe1 . C11 . 117.8(2) no C7 . Fe1 . C8 . 40.76(19) no C7 . Fe1 . C9 . 68.94(17) no C8 . Fe1 . C9 . 40.69(19) no C7 . Fe1 . C10 . 69.14(18) no C8 . Fe1 . C10 . 68.2(2) no C9 . Fe1 . C10 . 40.3(2) no C7 . Fe1 . C11 . 41.15(19) no C8 . Fe1 . C11 . 68.1(2) no C9 . Fe1 . C11 . 68.0(2) no C10 . Fe1 . C11 . 40.59(19) no Fe1 . C2 . C3 . 69.2(3) no Fe1 . C2 . C6 . 68.1(2) no C3 . C2 . C6 . 105.7(4) no Fe1 . C2 . B122 . 123.9(3) no C3 . C2 . B122 . 128.1(4) no C6 . C2 . B122 . 126.0(5) no C2 . C3 . Fe1 . 70.2(3) no C2 . C3 . C4 . 109.5(5) no Fe1 . C3 . C4 . 70.1(3) no C2 . C3 . H31 . 125.1 no Fe1 . C3 . H31 . 125.4 no C4 . C3 . H31 . 125.4 no C3 . C4 . Fe1 . 69.3(3) no C3 . C4 . C5 . 107.7(5) no Fe1 . C4 . C5 . 69.3(3) no C3 . C4 . H41 . 126.2 no Fe1 . C4 . H41 . 126.5 no C5 . C4 . H41 . 126.2 no C4 . C5 . Fe1 . 70.2(3) no C4 . C5 . C6 . 107.5(5) no Fe1 . C5 . C6 . 68.8(3) no C4 . C5 . H51 . 126.4 no Fe1 . C5 . H51 . 122.4 no C6 . C5 . H51 . 125.9 no C2 . C6 . C5 . 109.6(5) no C2 . C6 . Fe1 . 70.8(2) no C5 . C6 . Fe1 . 70.4(3) no C2 . C6 . H61 . 124.9 no C5 . C6 . H61 . 125.5 no Fe1 . C6 . H61 . 124.8 no Fe1 . C7 . C8 . 69.3(2) no Fe1 . C7 . C11 . 68.9(2) no C8 . C7 . C11 . 105.9(4) no Fe1 . C7 . B12 . 126.3(3) no C8 . C7 . B12 . 127.7(4) no C11 . C7 . B12 . 126.4(5) no C7 . C8 . Fe1 . 69.9(2) no C7 . C8 . C9 . 109.1(4) no Fe1 . C8 . C9 . 69.9(2) no C7 . C8 . H81 . 126.0 no Fe1 . C8 . H81 . 125.7 no C9 . C8 . H81 . 124.9 no C8 . C9 . Fe1 . 69.4(3) no C8 . C9 . C10 . 107.8(5) no Fe1 . C9 . C10 . 69.5(3) no C8 . C9 . H91 . 126.3 no Fe1 . C9 . H91 . 125.7 no C10 . C9 . H91 . 125.8 no C9 . C10 . Fe1 . 70.2(3) no C9 . C10 . C11 . 108.1(5) no Fe1 . C10 . C11 . 69.6(3) no C9 . C10 . H101 . 125.6 no Fe1 . C10 . H101 . 125.5 no C11 . C10 . H101 . 126.3 no C7 . C11 . C10 . 109.0(4) no C7 . C11 . Fe1 . 69.9(3) no C10 . C11 . Fe1 . 69.9(3) no C7 . C11 . H111 . 124.5 no C10 . C11 . H111 . 126.4 no Fe1 . C11 . H111 . 124.2 no C7 . B12 . O13 . 118.3(5) no C7 . B12 . O19 . 118.4(4) no O13 . B12 . O19 . 123.3(4) no B12 . O13 . C14 . 118.9(4) no O13 . C14 . C15 . 111.6(4) no O13 . C14 . H141 . 108.5 no C15 . C14 . H141 . 109.1 no O13 . C14 . H142 . 109.1 no C15 . C14 . H142 . 109.4 no H141 . C14 . H142 . 109.1 no C14 . C15 . C16 . 110.5(4) no C14 . C15 . C18 . 108.9(3) no C16 . C15 . C18 . 107.3(4) no C14 . C15 . C20 . 111.1(4) no C16 . C15 . C20 . 108.2(4) no C18 . C15 . C20 . 110.9(4) no C15 . C16 . O17 . 112.8(4) no C15 . C16 . H161 . 109.3 no O17 . C16 . H161 . 109.2 no C15 . C16 . H162 . 107.8 no O17 . C16 . H162 . 107.9 no H161 . C16 . H162 . 109.7 no C16 . O17 . B22 . 120.2(4) no C15 . C18 . O19 . 112.1(4) no C15 . C18 . H181 . 108.6 no O19 . C18 . H181 . 108.8 no C15 . C18 . H182 . 109.0 no O19 . C18 . H182 . 107.9 no H181 . C18 . H182 . 110.5 no C18 . O19 . B12 . 120.3(4) no C15 . C20 . O21 . 111.9(4) no C15 . C20 . H201 . 108.2 no O21 . C20 . H201 . 108.8 no C15 . C20 . H202 . 109.4 no O21 . C20 . H202 . 109.8 no H201 . C20 . H202 . 108.7 no C20 . O21 . B22 . 119.6(3) no C120 . O121 . B122 . 119.9(4) no O121 . C120 . C115 . 111.1(4) no O121 . C120 . H1201 . 109.6 no C115 . C120 . H1201 . 109.7 no O121 . C120 . H1202 . 108.5 no C115 . C120 . H1202 . 108.9 no H1201 . C120 . H1202 . 109.1 no C120 . C115 . C114 . 110.6(4) no C120 . C115 . C118 . 110.5(4) no C114 . C115 . C118 . 109.1(4) no C120 . C115 . C116 . 108.3(4) no C114 . C115 . C116 . 111.4(4) no C118 . C115 . C116 . 106.9(4) no C115 . C114 . O113 . 111.8(4) no C115 . C114 . H1141 . 108.3 no O113 . C114 . H1141 . 109.9 no C115 . C114 . H1142 . 109.1 no O113 . C114 . H1142 . 109.3 no H1141 . C114 . H1142 . 108.4 no C114 . O113 . B112 . 119.3(3) no O113 . B112 . C107 . 117.9(4) no O113 . B112 . O119 . 123.6(4) no C107 . B112 . O119 . 118.5(4) no B112 . C107 . C111 . 126.3(4) no B112 . C107 . Fe101 . 126.1(3) no C111 . C107 . Fe101 . 68.9(3) no B112 . C107 . C108 . 127.3(4) no C111 . C107 . C108 . 106.3(4) no Fe101 . C107 . C108 . 68.1(3) no C107 . C111 . Fe101 . 70.2(2) no C107 . C111 . C110 . 109.0(4) no Fe101 . C111 . C110 . 69.9(3) no C107 . C111 . H1111 . 124.9 no Fe101 . C111 . H1111 . 126.1 no C110 . C111 . H1111 . 126.1 no C107 . Fe101 . C111 . 40.96(18) no C107 . Fe101 . C110 . 68.85(19) no C111 . Fe101 . C110 . 40.50(19) no C107 . Fe101 . C109 . 69.07(19) no C111 . Fe101 . C109 . 68.38(19) no C110 . Fe101 . C109 . 40.62(19) no C107 . Fe101 . C108 . 40.93(18) no C111 . Fe101 . C108 . 68.63(19) no C110 . Fe101 . C108 . 68.8(2) no C109 . Fe101 . C108 . 41.20(19) no C107 . Fe101 . C102 . 120.55(19) no C111 . Fe101 . C102 . 111.24(19) no C110 . Fe101 . C102 . 129.99(19) no C109 . Fe101 . C102 . 165.9(2) no C108 . Fe101 . C102 . 152.75(19) no C107 . Fe101 . C106 . 154.23(18) no C111 . Fe101 . C106 . 119.60(18) no C110 . Fe101 . C106 . 107.4(2) no C109 . Fe101 . C106 . 125.6(2) no C108 . Fe101 . C106 . 163.51(19) no C107 . Fe101 . C105 . 164.90(18) no C111 . Fe101 . C105 . 150.21(18) no C110 . Fe101 . C105 . 114.9(2) no C109 . Fe101 . C105 . 103.7(2) no C108 . Fe101 . C105 . 125.14(19) no C107 . Fe101 . C104 . 128.43(18) no C111 . Fe101 . C104 . 168.8(2) no C110 . Fe101 . C104 . 147.5(2) no C109 . Fe101 . C104 . 113.77(19) no C108 . Fe101 . C104 . 105.31(19) no C107 . Fe101 . C103 . 110.63(19) no C111 . Fe101 . C103 . 132.64(19) no C110 . Fe101 . C103 . 169.9(2) no C109 . Fe101 . C103 . 149.4(2) no C108 . Fe101 . C103 . 117.91(19) no C102 . Fe101 . C106 . 41.37(19) no C102 . Fe101 . C105 . 69.3(2) no C106 . Fe101 . C105 . 40.59(18) no C102 . Fe101 . C104 . 69.53(19) no C106 . Fe101 . C104 . 68.83(19) no C105 . Fe101 . C104 . 40.99(18) no C102 . Fe101 . C103 . 40.88(19) no C106 . Fe101 . C103 . 68.42(19) no C105 . Fe101 . C103 . 68.44(19) no C104 . Fe101 . C103 . 40.84(19) no C111 . C110 . Fe101 . 69.6(3) no C111 . C110 . C109 . 108.0(4) no Fe101 . C110 . C109 . 69.3(3) no C111 . C110 . H1101 . 125.5 no Fe101 . C110 . H1101 . 124.5 no C109 . C110 . H1101 . 126.4 no C110 . C109 . Fe101 . 70.1(3) no C110 . C109 . C108 . 107.8(4) no Fe101 . C109 . C108 . 68.9(3) no C110 . C109 . H1091 . 126.7 no Fe101 . C109 . H1091 . 125.3 no C108 . C109 . H1091 . 125.5 no C109 . C108 . C107 . 108.8(4) no C109 . C108 . Fe101 . 69.9(3) no C107 . C108 . Fe101 . 71.0(3) no C109 . C108 . H1081 . 125.7 no C107 . C108 . H1081 . 125.4 no Fe101 . C108 . H1081 . 123.9 no Fe101 . C102 . C106 . 69.0(3) no Fe101 . C102 . C103 . 68.9(3) no C106 . C102 . C103 . 105.8(4) no Fe101 . C102 . B22 . 125.1(3) no C106 . C102 . B22 . 124.5(4) no C103 . C102 . B22 . 129.7(4) no C102 . C106 . Fe101 . 69.6(3) no C102 . C106 . C105 . 108.9(4) no Fe101 . C106 . C105 . 69.8(3) no C102 . C106 . H1061 . 126.0 no Fe101 . C106 . H1061 . 126.6 no C105 . C106 . H1061 . 125.2 no C106 . C105 . Fe101 . 69.6(3) no C106 . C105 . C104 . 108.1(4) no Fe101 . C105 . C104 . 69.1(3) no C106 . C105 . H1051 . 127.3 no Fe101 . C105 . H1051 . 124.8 no C104 . C105 . H1051 . 124.5 no C105 . C104 . Fe101 . 69.9(2) no C105 . C104 . C103 . 107.3(4) no Fe101 . C104 . C103 . 69.6(2) no C105 . C104 . H1041 . 125.8 no Fe101 . C104 . H1041 . 127.4 no C103 . C104 . H1041 . 126.8 no C102 . C103 . C104 . 109.9(4) no C102 . C103 . Fe101 . 70.2(3) no C104 . C103 . Fe101 . 69.6(3) no C102 . C103 . H1031 . 126.5 no C104 . C103 . H1031 . 123.6 no Fe101 . C103 . H1031 . 124.5 no B112 . O119 . C118 . 120.2(4) no C115 . C118 . O119 . 113.2(4) no C115 . C118 . H1181 . 109.3 no O119 . C118 . H1181 . 107.7 no C115 . C118 . H1182 . 109.1 no O119 . C118 . H1182 . 107.2 no H1181 . C118 . H1182 . 110.2 no C115 . C116 . O117 . 113.1(4) no C115 . C116 . H1161 . 108.7 no O117 . C116 . H1161 . 108.6 no C115 . C116 . H1162 . 108.3 no O117 . C116 . H1162 . 108.4 no H1161 . C116 . H1162 . 109.7 no C116 . O117 . B122 . 120.2(4) no C2 . B122 . O117 . 117.8(4) no C2 . B122 . O121 . 119.5(4) no O117 . B122 . O121 . 122.7(4) no C102 . B22 . O17 . 118.0(4) no C102 . B22 . O21 . 119.6(4) no O17 . B22 . O21 . 122.4(4) no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C106 . H1061 . O117 1_655 151 0.98 2.59 3.477(7) no C118 . H1181 . O121 2_747 130 0.98 2.56 3.278(7) no data_sa0613 _database_code_depnum_ccdc_archive 'CCDC 645160' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sa0613 _chemical_melting_point ? _chemical_formula_moiety 'C1 H1 CL3' _chemical_formula_sum 'C31 H33 B4 Cl3 Fe2 O8' _chemical_formula_weight 794.86 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' O O 0.0106 0.0060 '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' B B 0.0013 0.0007 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 16.7826(3) _cell_length_b 9.9148(2) _cell_length_c 20.8325(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.3390(10) _cell_angle_gamma 90.00 _cell_volume 3290.39(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 48634 _cell_measurement_theta_min 2.753 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.605 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 1.176 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7987 _exptl_absorpt_correction_T_max 0.9435 _exptl_absorpt_process_details 'Sortav (Blessing, 1995)' _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 KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46133 _diffrn_reflns_av_R_equivalents 0.1368 _diffrn_reflns_av_sigmaI/netI 0.0669 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 26.37 _reflns_number_total 6702 _reflns_number_gt 5558 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1999' _computing_structure_solution 'Sir-92 (A.Altomare et al. 1992)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Disorder in the chloroform molecule was modelled and refined based on 3 positions for each Chlorine atom and summed to unity. The weightings respectively are Cl1A:Cl1B:Cl1C - 0.45:0.35;0.20; Cl2A:Cl2B:Cl2C - 0.4:0.3:0.3 and Cl3A:Cl3B:Cl3C- 0.20:0.50:0.30. ISOR Restraints were also applied to all parts of the disordered chlorine atoms and the two Fe centres to approximate to isotropic behaviour due to large thermal parameters. 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. ; _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^)+(0.0254P)^2^+10.1006P] 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 6702 _refine_ls_number_parameters 490 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1358 _refine_ls_wR_factor_gt 0.1297 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.114 _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 C1 C 0.4594(2) 0.0981(4) 0.5727(2) 0.0277(9) Uani 1 1 d . . . C2 C 0.4653(2) -0.0245(4) 0.6103(2) 0.0292(9) Uani 1 1 d . . . H2 H 0.4932 -0.0352 0.6573 0.035 Uiso 1 1 calc R . . C3 C 0.4224(2) -0.1269(5) 0.5654(2) 0.0333(10) Uani 1 1 d . . . H3 H 0.4165 -0.2179 0.5774 0.040 Uiso 1 1 calc R . . C4 C 0.3898(3) -0.0722(4) 0.5001(2) 0.0320(10) Uani 1 1 d . . . H4 H 0.3586 -0.1194 0.4604 0.038 Uiso 1 1 calc R . . C5 C 0.4121(3) 0.0669(5) 0.5043(2) 0.0325(10) Uani 1 1 d . . . H5 H 0.3979 0.1288 0.4676 0.039 Uiso 1 1 calc R . . C6 C 0.2878(2) 0.0719(4) 0.6391(2) 0.0286(9) Uani 1 1 d . . . C7 C 0.2524(2) -0.0492(5) 0.6031(2) 0.0327(10) Uani 1 1 d . . . H7 H 0.2532 -0.1362 0.6224 0.039 Uiso 1 1 calc R . . C8 C 0.2160(2) -0.0155(5) 0.5337(2) 0.0357(11) Uani 1 1 d . . . H8 H 0.1876 -0.0759 0.4986 0.043 Uiso 1 1 calc R . . C9 C 0.2296(3) 0.1240(5) 0.5261(2) 0.0353(10) Uani 1 1 d . . . H9 H 0.2123 0.1731 0.4848 0.042 Uiso 1 1 calc R . . C10 C 0.2731(2) 0.1771(5) 0.5902(2) 0.0304(9) Uani 1 1 d . . . H10 H 0.2900 0.2685 0.5994 0.036 Uiso 1 1 calc R . . C11 C 0.5892(2) 0.3647(4) 0.6942(2) 0.0285(9) Uani 1 1 d . . . H11A H 0.6445 0.3687 0.6866 0.034 Uiso 1 1 calc R . . H11B H 0.5989 0.3671 0.7435 0.034 Uiso 1 1 calc R . . C12 C 0.5166(3) 0.4746(4) 0.5844(2) 0.0295(9) Uani 1 1 d . . . H12A H 0.4767 0.5467 0.5620 0.035 Uiso 1 1 calc R . . H12B H 0.5688 0.4877 0.5726 0.035 Uiso 1 1 calc R . . C13 C 0.5366(3) 0.4869(4) 0.6609(2) 0.0261(9) Uani 1 1 d . . . C14 C 0.5855(3) 0.6180(5) 0.6835(2) 0.0304(9) Uani 1 1 d . . . H14A H 0.6428 0.6071 0.6803 0.036 Uiso 1 1 calc R . . H14B H 0.5576 0.6915 0.6523 0.036 Uiso 1 1 calc R . . C15 C 0.4553(2) 0.4935(4) 0.67958(19) 0.0268(9) Uani 1 1 d . . . H15A H 0.4185 0.5649 0.6526 0.032 Uiso 1 1 calc R . . H15B H 0.4252 0.4064 0.6684 0.032 Uiso 1 1 calc R . . C16 C 0.4078(3) -0.0379(4) 0.8204(2) 0.0315(9) Uani 1 1 d . . . H16A H 0.4454 -0.1174 0.8300 0.038 Uiso 1 1 calc R . . H16B H 0.3692 -0.0467 0.8476 0.038 Uiso 1 1 calc R . . C17 C 0.4038(3) 0.2110(4) 0.8167(2) 0.0291(9) Uani 1 1 d . . . H17A H 0.3617 0.2163 0.8410 0.035 Uiso 1 1 calc R . . H17B H 0.4383 0.2939 0.8270 0.035 Uiso 1 1 calc R . . C18 C 0.4600(3) 0.0884(4) 0.8418(2) 0.0255(9) Uani 1 1 d . . . C19 C 0.5342(2) 0.0905(4) 0.8142(2) 0.0252(8) Uani 1 1 d . . . H19A H 0.5645 0.0036 0.8246 0.030 Uiso 1 1 calc R . . H19B H 0.5131 0.1008 0.7644 0.030 Uiso 1 1 calc R . . C20 C 0.4947(3) 0.0873(4) 0.9188(2) 0.0303(9) Uani 1 1 d . . . H20A H 0.4477 0.0979 0.9376 0.036 Uiso 1 1 calc R . . H20B H 0.5213 -0.0013 0.9339 0.036 Uiso 1 1 calc R . . C21 C 0.5513(2) 0.6454(4) 0.8567(2) 0.0254(9) Uani 1 1 d . . . C22 C 0.5101(2) 0.5905(4) 0.9015(2) 0.0272(9) Uani 1 1 d . . . H22 H 0.4671 0.5241 0.8900 0.033 Uiso 1 1 calc R . . C23 C 0.5443(3) 0.6519(4) 0.9658(2) 0.0321(10) Uani 1 1 d . . . H23 H 0.5282 0.6336 1.0047 0.038 Uiso 1 1 calc R . . C24 C 0.6063(3) 0.7445(4) 0.9621(2) 0.0296(9) Uani 1 1 d . . . H24 H 0.6392 0.7993 0.9981 0.035 Uiso 1 1 calc R . . C25 C 0.6109(3) 0.7417(4) 0.8953(2) 0.0295(9) Uani 1 1 d . . . H25 H 0.6474 0.7949 0.8788 0.035 Uiso 1 1 calc R . . C26 C 0.6654(3) 0.3539(4) 0.9388(2) 0.0288(9) Uani 1 1 d . . . C27 C 0.7138(3) 0.4316(4) 0.9060(2) 0.0299(9) Uani 1 1 d . . . H27 H 0.7135 0.4204 0.8607 0.036 Uiso 1 1 calc R . . C28 C 0.7621(3) 0.5279(5) 0.9527(2) 0.0344(10) Uani 1 1 d . . . H28 H 0.7994 0.5923 0.9439 0.041 Uiso 1 1 calc R . . C29 C 0.7450(3) 0.5108(5) 1.0144(2) 0.0349(10) Uani 1 1 d . . . H29 H 0.7691 0.5615 1.0545 0.042 Uiso 1 1 calc R . . C30 C 0.6859(3) 0.4058(4) 1.0064(2) 0.0310(10) Uani 1 1 d . . . H30 H 0.6634 0.3746 1.0402 0.037 Uiso 1 1 calc R . . O1 O 0.48088(18) 0.3460(3) 0.55947(14) 0.0307(7) Uani 1 1 d . . . O2 O 0.54761(17) 0.2411(3) 0.66670(14) 0.0296(6) Uani 1 1 d . . . O3 O 0.36106(18) 0.2041(3) 0.74499(14) 0.0301(7) Uani 1 1 d . . . O4 O 0.35958(19) -0.0375(3) 0.74996(15) 0.0343(7) Uani 1 1 d . . . O5 O 0.47221(17) 0.5214(3) 0.75026(14) 0.0285(6) Uani 1 1 d . . . O6 O 0.59149(19) 0.6556(3) 0.75127(14) 0.0334(7) Uani 1 1 d . . . O7 O 0.59111(17) 0.1989(3) 0.84291(14) 0.0275(6) Uani 1 1 d . . . O8 O 0.55479(18) 0.1909(3) 0.94536(14) 0.0301(7) Uani 1 1 d . . . Fe1 Fe 0.34151(3) 0.02679(6) 0.56574(3) 0.02362(16) Uani 1 1 d U . . Fe2 Fe 0.63738(3) 0.55659(6) 0.93837(3) 0.02371(15) Uani 1 1 d U . . B1 B 0.4975(3) 0.2363(5) 0.6012(2) 0.0264(10) Uani 1 1 d . . . B2 B 0.3392(3) 0.0811(5) 0.7156(2) 0.0281(10) Uani 1 1 d . . . B3 B 0.5379(3) 0.6038(5) 0.7822(2) 0.0255(10) Uani 1 1 d . . . B4 B 0.6001(3) 0.2432(5) 0.9068(2) 0.0276(10) Uani 1 1 d . . . C31 C 0.2775(3) 0.5196(5) 0.7491(2) 0.0361(10) Uani 1 1 d . . . H31 H 0.3365 0.4929 0.7537 0.043 Uiso 1 1 calc R A 1 Cl1A Cl 0.2327(3) 0.5528(5) 0.6641(2) 0.0613(11) Uani 0.45 1 d PU B 1 Cl2A Cl 0.2887(3) 0.6763(5) 0.7987(2) 0.0539(13) Uani 0.40 1 d PU B 1 Cl3A Cl 0.2683(5) 0.4891(8) 0.8291(4) 0.0543(16) Uani 0.20 1 d PU B 1 Cl1B Cl 0.2152(4) 0.5049(6) 0.6613(3) 0.0603(14) Uani 0.35 1 d PU B 2 Cl2B Cl 0.2953(4) 0.6805(6) 0.7772(4) 0.0435(13) Uani 0.30 1 d PU B 2 Cl3B Cl 0.2251(2) 0.4242(4) 0.79537(19) 0.0425(9) Uani 0.50 1 d PU B 2 Cl1C Cl 0.1865(6) 0.4599(10) 0.6900(5) 0.074(2) Uani 0.20 1 d PU B 3 Cl2C Cl 0.2992(3) 0.6876(5) 0.7431(3) 0.0561(13) Uani 0.30 1 d PU B 3 Cl3C Cl 0.2124(4) 0.4117(6) 0.7745(3) 0.0384(14) Uani 0.30 1 d PU B 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0221(19) 0.031(2) 0.033(2) -0.0038(18) 0.0143(17) -0.0029(17) C2 0.0183(19) 0.031(2) 0.038(2) -0.0007(19) 0.0088(17) 0.0057(17) C3 0.022(2) 0.029(2) 0.051(3) -0.005(2) 0.014(2) 0.0004(18) C4 0.024(2) 0.034(2) 0.041(3) -0.015(2) 0.0147(19) -0.0059(18) C5 0.030(2) 0.039(3) 0.035(2) -0.003(2) 0.0187(19) -0.0053(19) C6 0.0218(19) 0.033(2) 0.034(2) -0.0006(19) 0.0133(17) 0.0033(17) C7 0.021(2) 0.036(3) 0.045(3) -0.002(2) 0.0167(19) -0.0068(18) C8 0.0124(18) 0.055(3) 0.038(3) -0.011(2) 0.0057(17) -0.0013(19) C9 0.026(2) 0.044(3) 0.035(2) 0.001(2) 0.0067(19) 0.013(2) C10 0.023(2) 0.032(2) 0.036(2) 0.0010(19) 0.0088(18) 0.0088(17) C11 0.024(2) 0.032(2) 0.028(2) -0.0042(18) 0.0066(17) -0.0045(17) C12 0.037(2) 0.027(2) 0.027(2) 0.0035(18) 0.0140(18) -0.0037(18) C13 0.029(2) 0.025(2) 0.026(2) 0.0001(17) 0.0111(17) -0.0047(17) C14 0.030(2) 0.036(2) 0.029(2) 0.0001(19) 0.0147(18) -0.0075(19) C15 0.025(2) 0.032(2) 0.023(2) -0.0005(17) 0.0073(16) -0.0007(17) C16 0.037(2) 0.028(2) 0.030(2) 0.0036(18) 0.0115(19) -0.0015(19) C17 0.034(2) 0.026(2) 0.028(2) -0.0020(18) 0.0091(18) 0.0027(18) C18 0.031(2) 0.021(2) 0.025(2) 0.0050(16) 0.0112(17) 0.0043(17) C19 0.030(2) 0.019(2) 0.026(2) 0.0004(16) 0.0089(17) 0.0029(16) C20 0.040(2) 0.024(2) 0.030(2) 0.0028(18) 0.0150(19) 0.0043(18) C21 0.0240(19) 0.021(2) 0.032(2) 0.0026(17) 0.0093(17) 0.0060(16) C22 0.024(2) 0.025(2) 0.034(2) -0.0038(18) 0.0123(17) 0.0015(16) C23 0.036(2) 0.031(2) 0.032(2) -0.0018(19) 0.0155(19) 0.0061(19) C24 0.035(2) 0.020(2) 0.034(2) -0.0084(18) 0.0104(19) 0.0027(17) C25 0.034(2) 0.018(2) 0.038(2) -0.0003(18) 0.0124(19) 0.0020(17) C26 0.028(2) 0.021(2) 0.035(2) 0.0016(18) 0.0065(18) 0.0081(17) C27 0.027(2) 0.027(2) 0.036(2) -0.0020(19) 0.0110(18) 0.0068(18) C28 0.026(2) 0.031(2) 0.043(3) -0.004(2) 0.0052(19) 0.0006(18) C29 0.033(2) 0.032(3) 0.031(2) -0.0026(19) -0.0038(19) 0.0042(19) C30 0.032(2) 0.028(2) 0.028(2) 0.0023(18) 0.0022(18) 0.0052(18) O1 0.0363(16) 0.0320(17) 0.0252(15) -0.0018(13) 0.0115(13) -0.0074(13) O2 0.0296(15) 0.0257(16) 0.0309(16) 0.0012(13) 0.0058(13) -0.0020(12) O3 0.0331(15) 0.0244(16) 0.0308(16) -0.0001(12) 0.0072(13) 0.0040(12) O4 0.0424(17) 0.0274(17) 0.0306(16) -0.0002(13) 0.0081(14) -0.0084(14) O5 0.0279(14) 0.0335(17) 0.0278(15) -0.0042(13) 0.0141(12) -0.0047(13) O6 0.0393(17) 0.0355(18) 0.0279(16) -0.0070(13) 0.0141(13) -0.0134(14) O7 0.0299(15) 0.0231(15) 0.0305(16) -0.0026(12) 0.0111(12) -0.0016(12) O8 0.0367(16) 0.0303(17) 0.0234(15) -0.0036(12) 0.0096(13) 0.0005(13) Fe1 0.0191(3) 0.0254(3) 0.0273(3) -0.0011(2) 0.0086(2) 0.0007(2) Fe2 0.0252(3) 0.0207(3) 0.0249(3) -0.0027(2) 0.0074(2) 0.0014(2) B1 0.019(2) 0.034(3) 0.030(3) -0.003(2) 0.0135(19) -0.0001(19) B2 0.023(2) 0.031(3) 0.034(3) 0.000(2) 0.015(2) -0.0028(19) B3 0.022(2) 0.022(2) 0.033(3) 0.0041(19) 0.0102(19) 0.0028(18) B4 0.027(2) 0.021(2) 0.032(3) 0.002(2) 0.006(2) 0.0096(19) C31 0.028(2) 0.033(3) 0.047(3) 0.007(2) 0.013(2) 0.0006(19) Cl1A 0.0624(14) 0.0618(14) 0.0574(13) 0.0042(9) 0.0154(9) -0.0018(9) Cl2A 0.0571(15) 0.0519(15) 0.0535(15) -0.0016(10) 0.0185(10) -0.0064(9) Cl3A 0.0550(18) 0.0558(19) 0.0539(18) -0.0001(10) 0.0195(11) 0.0017(10) Cl1B 0.0622(16) 0.0595(17) 0.0564(16) 0.0019(10) 0.0147(10) -0.0018(10) Cl2B 0.0465(15) 0.0404(15) 0.0436(16) -0.0025(10) 0.0142(10) -0.0044(9) Cl3B 0.0417(12) 0.0479(12) 0.0424(12) 0.0034(9) 0.0197(9) -0.0013(8) Cl1C 0.073(2) 0.074(2) 0.075(2) -0.0023(10) 0.0220(12) -0.0005(10) Cl2C 0.0559(15) 0.0527(15) 0.0587(15) 0.0008(10) 0.0163(10) -0.0013(10) Cl3C 0.0364(16) 0.0393(17) 0.0399(17) -0.0009(10) 0.0128(10) -0.0042(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 C1 C5 1.429(6) . ? C1 C2 1.433(6) . ? C1 B1 1.550(6) . ? C1 Fe1 2.063(4) . ? C2 C3 1.414(6) . ? C2 Fe1 2.054(4) . ? C2 H2 0.9500 . ? C3 C4 1.406(6) . ? C3 Fe1 2.042(4) . ? C3 H3 0.9500 . ? C4 C5 1.425(6) . ? C4 Fe1 2.047(4) . ? C4 H4 0.9500 . ? C5 Fe1 2.039(4) . ? C5 H5 0.9500 . ? C6 C10 1.424(6) . ? C6 C7 1.441(6) . ? C6 B2 1.556(6) . ? C6 Fe1 2.053(4) . ? C7 C8 1.421(6) . ? C7 Fe1 2.036(4) . ? C7 H7 0.9500 . ? C8 C9 1.419(7) . ? C8 Fe1 2.042(4) . ? C8 H8 0.9500 . ? C9 C10 1.409(6) . ? C9 Fe1 2.040(4) . ? C9 H9 0.9500 . ? C10 Fe1 2.042(4) . ? C10 H10 0.9500 . ? C11 O2 1.438(5) . ? C11 C13 1.531(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O1 1.434(5) . ? C12 C13 1.527(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.531(6) . ? C13 C15 1.532(5) . ? C14 O6 1.434(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O5 1.436(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 O4 1.436(5) . ? C16 C18 1.513(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 O3 1.441(5) . ? C17 C18 1.526(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C20 1.525(6) . ? C18 C19 1.527(5) . ? C19 O7 1.437(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 O8 1.424(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.432(6) . ? C21 C25 1.432(6) . ? C21 B3 1.553(6) . ? C21 Fe2 2.052(4) . ? C22 C23 1.418(6) . ? C22 Fe2 2.057(4) . ? C22 H22 0.9500 . ? C23 C24 1.406(6) . ? C23 Fe2 2.053(4) . ? C23 H23 0.9500 . ? C24 C25 1.419(6) . ? C24 Fe2 2.037(4) . ? C24 H24 0.9500 . ? C25 Fe2 2.030(4) . ? C25 H25 0.9500 . ? C26 C30 1.435(6) . ? C26 C27 1.438(6) . ? C26 B4 1.547(7) . ? C26 Fe2 2.063(4) . ? C27 C28 1.420(6) . ? C27 Fe2 2.044(4) . ? C27 H27 0.9500 . ? C28 C29 1.414(6) . ? C28 Fe2 2.040(4) . ? C28 H28 0.9500 . ? C29 C30 1.410(6) . ? C29 Fe2 2.043(4) . ? C29 H29 0.9500 . ? C30 Fe2 2.045(4) . ? C30 H30 0.9500 . ? O1 B1 1.365(6) . ? O2 B1 1.360(5) . ? O3 B2 1.363(6) . ? O4 B2 1.364(6) . ? O5 B3 1.365(6) . ? O6 B3 1.361(5) . ? O7 B4 1.364(5) . ? O8 B4 1.370(6) . ? C31 Cl2B 1.693(7) . ? C31 Cl2C 1.718(7) . ? C31 Cl1A 1.725(6) . ? C31 Cl3C 1.727(7) . ? C31 Cl1C 1.737(10) . ? C31 Cl3A 1.748(8) . ? C31 Cl3B 1.769(5) . ? C31 Cl1B 1.805(7) . ? C31 Cl2A 1.843(7) . ? C31 H31 1.0000 . ? Cl2A Cl3A 2.025(9) . ? Cl1C Cl3C 1.743(11) . ? 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 C5 C1 C2 106.4(4) . . ? C5 C1 B1 127.3(4) . . ? C2 C1 B1 126.2(4) . . ? C5 C1 Fe1 68.7(2) . . ? C2 C1 Fe1 69.3(2) . . ? B1 C1 Fe1 126.9(3) . . ? C3 C2 C1 108.3(4) . . ? C3 C2 Fe1 69.3(2) . . ? C1 C2 Fe1 70.0(2) . . ? C3 C2 H2 125.9 . . ? C1 C2 H2 125.9 . . ? Fe1 C2 H2 126.4 . . ? C4 C3 C2 109.0(4) . . ? C4 C3 Fe1 70.1(2) . . ? C2 C3 Fe1 70.3(2) . . ? C4 C3 H3 125.5 . . ? C2 C3 H3 125.5 . . ? Fe1 C3 H3 125.7 . . ? C3 C4 C5 107.4(4) . . ? C3 C4 Fe1 69.7(2) . . ? C5 C4 Fe1 69.3(2) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Fe1 C4 H4 126.3 . . ? C4 C5 C1 108.9(4) . . ? C4 C5 Fe1 69.9(2) . . ? C1 C5 Fe1 70.5(2) . . ? C4 C5 H5 125.6 . . ? C1 C5 H5 125.6 . . ? Fe1 C5 H5 125.6 . . ? C10 C6 C7 106.7(4) . . ? C10 C6 B2 127.2(4) . . ? C7 C6 B2 125.9(4) . . ? C10 C6 Fe1 69.2(2) . . ? C7 C6 Fe1 68.7(2) . . ? B2 C6 Fe1 122.9(3) . . ? C8 C7 C6 108.0(4) . . ? C8 C7 Fe1 69.9(2) . . ? C6 C7 Fe1 70.0(2) . . ? C8 C7 H7 126.0 . . ? C6 C7 H7 126.0 . . ? Fe1 C7 H7 125.7 . . ? C9 C8 C7 108.1(4) . . ? C9 C8 Fe1 69.6(2) . . ? C7 C8 Fe1 69.4(2) . . ? C9 C8 H8 125.9 . . ? C7 C8 H8 125.9 . . ? Fe1 C8 H8 126.7 . . ? C10 C9 C8 108.1(4) . . ? C10 C9 Fe1 69.9(2) . . ? C8 C9 Fe1 69.7(2) . . ? C10 C9 H9 125.9 . . ? C8 C9 H9 125.9 . . ? Fe1 C9 H9 126.1 . . ? C9 C10 C6 109.0(4) . . ? C9 C10 Fe1 69.8(2) . . ? C6 C10 Fe1 70.1(2) . . ? C9 C10 H10 125.5 . . ? C6 C10 H10 125.5 . . ? Fe1 C10 H10 126.3 . . ? O2 C11 C13 110.8(3) . . ? O2 C11 H11A 109.5 . . ? C13 C11 H11A 109.5 . . ? O2 C11 H11B 109.5 . . ? C13 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? O1 C12 C13 112.3(3) . . ? O1 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? O1 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C12 C13 C11 108.3(3) . . ? C12 C13 C14 108.0(3) . . ? C11 C13 C14 110.8(3) . . ? C12 C13 C15 110.3(3) . . ? C11 C13 C15 110.6(3) . . ? C14 C13 C15 108.7(3) . . ? O6 C14 C13 112.8(3) . . ? O6 C14 H14A 109.0 . . ? C13 C14 H14A 109.0 . . ? O6 C14 H14B 109.0 . . ? C13 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? O5 C15 C13 111.3(3) . . ? O5 C15 H15A 109.4 . . ? C13 C15 H15A 109.4 . . ? O5 C15 H15B 109.4 . . ? C13 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? O4 C16 C18 112.7(3) . . ? O4 C16 H16A 109.0 . . ? C18 C16 H16A 109.0 . . ? O4 C16 H16B 109.0 . . ? C18 C16 H16B 109.0 . . ? H16A C16 H16B 107.8 . . ? O3 C17 C18 111.7(3) . . ? O3 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? O3 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C16 C18 C20 107.3(3) . . ? C16 C18 C17 108.7(3) . . ? C20 C18 C17 110.9(3) . . ? C16 C18 C19 111.4(3) . . ? C20 C18 C19 108.0(3) . . ? C17 C18 C19 110.4(3) . . ? O7 C19 C18 111.6(3) . . ? O7 C19 H19A 109.3 . . ? C18 C19 H19A 109.3 . . ? O7 C19 H19B 109.3 . . ? C18 C19 H19B 109.3 . . ? H19A C19 H19B 108.0 . . ? O8 C20 C18 113.1(3) . . ? O8 C20 H20A 109.0 . . ? C18 C20 H20A 109.0 . . ? O8 C20 H20B 109.0 . . ? C18 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C25 106.5(4) . . ? C22 C21 B3 127.0(4) . . ? C25 C21 B3 126.4(4) . . ? C22 C21 Fe2 69.8(2) . . ? C25 C21 Fe2 68.7(2) . . ? B3 C21 Fe2 123.9(3) . . ? C23 C22 C21 108.4(4) . . ? C23 C22 Fe2 69.7(2) . . ? C21 C22 Fe2 69.4(2) . . ? C23 C22 H22 125.8 . . ? C21 C22 H22 125.8 . . ? Fe2 C22 H22 126.7 . . ? C24 C23 C22 108.4(4) . . ? C24 C23 Fe2 69.3(2) . . ? C22 C23 Fe2 70.0(2) . . ? C24 C23 H23 125.8 . . ? C22 C23 H23 125.8 . . ? Fe2 C23 H23 126.5 . . ? C23 C24 C25 108.1(4) . . ? C23 C24 Fe2 70.5(2) . . ? C25 C24 Fe2 69.3(2) . . ? C23 C24 H24 126.0 . . ? C25 C24 H24 126.0 . . ? Fe2 C24 H24 125.8 . . ? C24 C25 C21 108.6(4) . . ? C24 C25 Fe2 69.8(2) . . ? C21 C25 Fe2 70.3(2) . . ? C24 C25 H25 125.7 . . ? C21 C25 H25 125.7 . . ? Fe2 C25 H25 125.8 . . ? C30 C26 C27 106.1(4) . . ? C30 C26 B4 126.6(4) . . ? C27 C26 B4 127.2(4) . . ? C30 C26 Fe2 68.9(2) . . ? C27 C26 Fe2 68.8(2) . . ? B4 C26 Fe2 124.1(3) . . ? C28 C27 C26 108.8(4) . . ? C28 C27 Fe2 69.5(2) . . ? C26 C27 Fe2 70.2(2) . . ? C28 C27 H27 125.6 . . ? C26 C27 H27 125.6 . . ? Fe2 C27 H27 126.3 . . ? C29 C28 C27 107.8(4) . . ? C29 C28 Fe2 69.9(3) . . ? C27 C28 Fe2 69.8(2) . . ? C29 C28 H28 126.1 . . ? C27 C28 H28 126.1 . . ? Fe2 C28 H28 125.8 . . ? C30 C29 C28 108.6(4) . . ? C30 C29 Fe2 69.9(2) . . ? C28 C29 Fe2 69.6(2) . . ? C30 C29 H29 125.7 . . ? C28 C29 H29 125.7 . . ? Fe2 C29 H29 126.4 . . ? C29 C30 C26 108.8(4) . . ? C29 C30 Fe2 69.8(2) . . ? C26 C30 Fe2 70.2(2) . . ? C29 C30 H30 125.6 . . ? C26 C30 H30 125.6 . . ? Fe2 C30 H30 126.0 . . ? B1 O1 C12 119.9(3) . . ? B1 O2 C11 119.9(3) . . ? B2 O3 C17 119.0(3) . . ? B2 O4 C16 120.5(3) . . ? B3 O5 C15 118.9(3) . . ? B3 O6 C14 121.1(3) . . ? B4 O7 C19 120.1(3) . . ? B4 O8 C20 120.1(3) . . ? C7 Fe1 C5 162.69(18) . . ? C7 Fe1 C9 68.69(19) . . ? C5 Fe1 C9 107.25(19) . . ? C7 Fe1 C10 68.67(18) . . ? C5 Fe1 C10 119.88(18) . . ? C9 Fe1 C10 40.37(17) . . ? C7 Fe1 C3 107.11(18) . . ? C5 Fe1 C3 67.97(19) . . ? C9 Fe1 C3 151.56(18) . . ? C10 Fe1 C3 166.45(18) . . ? C7 Fe1 C8 40.79(18) . . ? C5 Fe1 C8 125.34(18) . . ? C9 Fe1 C8 40.68(19) . . ? C10 Fe1 C8 68.20(18) . . ? C3 Fe1 C8 117.64(19) . . ? C7 Fe1 C4 124.83(18) . . ? C5 Fe1 C4 40.82(17) . . ? C9 Fe1 C4 117.61(18) . . ? C10 Fe1 C4 152.78(18) . . ? C3 Fe1 C4 40.22(18) . . ? C8 Fe1 C4 105.53(17) . . ? C7 Fe1 C6 41.28(17) . . ? C5 Fe1 C6 154.56(18) . . ? C9 Fe1 C6 68.60(17) . . ? C10 Fe1 C6 40.71(17) . . ? C3 Fe1 C6 127.80(18) . . ? C8 Fe1 C6 68.84(17) . . ? C4 Fe1 C6 163.92(18) . . ? C7 Fe1 C2 119.70(18) . . ? C5 Fe1 C2 68.10(18) . . ? C9 Fe1 C2 166.13(19) . . ? C10 Fe1 C2 129.46(17) . . ? C3 Fe1 C2 40.39(17) . . ? C8 Fe1 C2 152.71(19) . . ? C4 Fe1 C2 68.08(17) . . ? C6 Fe1 C2 109.60(17) . . ? C7 Fe1 C1 154.68(17) . . ? C5 Fe1 C1 40.78(17) . . ? C9 Fe1 C1 127.36(19) . . ? C10 Fe1 C1 109.54(17) . . ? C3 Fe1 C1 68.41(17) . . ? C8 Fe1 C1 163.92(18) . . ? C4 Fe1 C1 68.80(16) . . ? C6 Fe1 C1 120.60(17) . . ? C2 Fe1 C1 40.73(17) . . ? C25 Fe2 C24 40.85(17) . . ? C25 Fe2 C28 105.21(18) . . ? C24 Fe2 C28 114.95(18) . . ? C25 Fe2 C29 124.11(18) . . ? C24 Fe2 C29 104.27(18) . . ? C28 Fe2 C29 40.51(18) . . ? C25 Fe2 C27 118.37(17) . . ? C24 Fe2 C27 150.44(18) . . ? C28 Fe2 C27 40.71(17) . . ? C29 Fe2 C27 68.13(18) . . ? C25 Fe2 C30 162.10(17) . . ? C24 Fe2 C30 125.23(17) . . ? C28 Fe2 C30 68.29(18) . . ? C29 Fe2 C30 40.36(18) . . ? C27 Fe2 C30 68.33(18) . . ? C25 Fe2 C21 41.07(16) . . ? C24 Fe2 C21 68.98(17) . . ? C28 Fe2 C21 127.11(17) . . ? C29 Fe2 C21 163.31(18) . . ? C27 Fe2 C21 109.76(17) . . ? C30 Fe2 C21 155.74(17) . . ? C25 Fe2 C23 68.11(17) . . ? C24 Fe2 C23 40.21(17) . . ? C28 Fe2 C23 149.19(18) . . ? C29 Fe2 C23 116.79(18) . . ? C27 Fe2 C23 168.91(18) . . ? C30 Fe2 C23 108.40(18) . . ? C21 Fe2 C23 68.55(16) . . ? C25 Fe2 C22 68.28(17) . . ? C24 Fe2 C22 68.03(17) . . ? C28 Fe2 C22 167.06(17) . . ? C29 Fe2 C22 152.40(18) . . ? C27 Fe2 C22 131.40(17) . . ? C30 Fe2 C22 121.25(17) . . ? C21 Fe2 C22 40.79(16) . . ? C23 Fe2 C22 40.34(16) . . ? C25 Fe2 C26 154.23(17) . . ? C24 Fe2 C26 164.79(17) . . ? C28 Fe2 C26 68.99(18) . . ? C29 Fe2 C26 68.61(17) . . ? C27 Fe2 C26 41.00(17) . . ? C30 Fe2 C26 40.90(17) . . ? C21 Fe2 C26 121.47(17) . . ? C23 Fe2 C26 129.72(18) . . ? C22 Fe2 C26 111.67(17) . . ? O2 B1 O1 123.3(4) . . ? O2 B1 C1 117.8(4) . . ? O1 B1 C1 118.9(4) . . ? O3 B2 O4 123.2(4) . . ? O3 B2 C6 119.8(4) . . ? O4 B2 C6 117.0(4) . . ? O6 B3 O5 123.2(4) . . ? O6 B3 C21 117.6(4) . . ? O5 B3 C21 119.1(4) . . ? O7 B4 O8 122.6(4) . . ? O7 B4 C26 119.7(4) . . ? O8 B4 C26 117.7(4) . . ? Cl2B C31 Cl2C 25.0(2) . . ? Cl2B C31 Cl1A 98.5(4) . . ? Cl2C C31 Cl1A 76.9(3) . . ? Cl2B C31 Cl3C 122.5(4) . . ? Cl2C C31 Cl3C 142.4(4) . . ? Cl1A C31 Cl3C 108.6(3) . . ? Cl2B C31 Cl1C 125.9(5) . . ? Cl2C C31 Cl1C 115.9(5) . . ? Cl1A C31 Cl1C 48.3(4) . . ? Cl3C C31 Cl1C 60.4(4) . . ? Cl2B C31 Cl3A 83.8(4) . . ? Cl2C C31 Cl3A 108.8(4) . . ? Cl1A C31 Cl3A 150.6(4) . . ? Cl3C C31 Cl3A 49.2(3) . . ? Cl1C C31 Cl3A 107.2(5) . . ? Cl2B C31 Cl3B 112.3(4) . . ? Cl2C C31 Cl3B 135.3(4) . . ? Cl1A C31 Cl3B 122.0(3) . . ? Cl3C C31 Cl3B 14.3(2) . . ? Cl1C C31 Cl3B 74.1(4) . . ? Cl3A C31 Cl3B 34.9(3) . . ? Cl2B C31 Cl1B 114.1(4) . . ? Cl2C C31 Cl1B 94.1(4) . . ? Cl1A C31 Cl1B 17.8(2) . . ? Cl3C C31 Cl1B 92.3(4) . . ? Cl1C C31 Cl1B 32.2(3) . . ? Cl3A C31 Cl1B 139.1(4) . . ? Cl3B C31 Cl1B 106.3(3) . . ? Cl2B C31 Cl2A 15.4(2) . . ? Cl2C C31 Cl2A 40.2(3) . . ? Cl1A C31 Cl2A 110.4(3) . . ? Cl3C C31 Cl2A 108.3(3) . . ? Cl1C C31 Cl2A 126.6(4) . . ? Cl3A C31 Cl2A 68.6(3) . . ? Cl3B C31 Cl2A 97.3(3) . . ? Cl1B C31 Cl2A 124.1(3) . . ? Cl2B C31 H31 98.9 . . ? Cl2C C31 H31 92.1 . . ? Cl1A C31 H31 104.3 . . ? Cl3C C31 H31 120.7 . . ? Cl1C C31 H31 126.9 . . ? Cl3A C31 H31 104.3 . . ? Cl3B C31 H31 117.1 . . ? Cl1B C31 H31 108.4 . . ? Cl2A C31 H31 104.3 . . ? C31 Cl2A Cl3A 53.5(3) . . ? C31 Cl3A Cl2A 57.9(3) . . ? C31 Cl1C Cl3C 59.5(4) . . ? C31 Cl3C Cl1C 60.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 0.0(4) . . . . ? B1 C1 C2 C3 -179.8(4) . . . . ? Fe1 C1 C2 C3 58.9(3) . . . . ? C5 C1 C2 Fe1 -58.9(3) . . . . ? B1 C1 C2 Fe1 121.3(4) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? Fe1 C2 C3 C4 59.6(3) . . . . ? C1 C2 C3 Fe1 -59.3(3) . . . . ? C2 C3 C4 C5 -0.4(5) . . . . ? Fe1 C3 C4 C5 59.3(3) . . . . ? C2 C3 C4 Fe1 -59.7(3) . . . . ? C3 C4 C5 C1 0.4(4) . . . . ? Fe1 C4 C5 C1 60.0(3) . . . . ? C3 C4 C5 Fe1 -59.5(3) . . . . ? C2 C1 C5 C4 -0.3(4) . . . . ? B1 C1 C5 C4 179.5(4) . . . . ? Fe1 C1 C5 C4 -59.6(3) . . . . ? C2 C1 C5 Fe1 59.3(3) . . . . ? B1 C1 C5 Fe1 -120.9(4) . . . . ? C10 C6 C7 C8 -0.8(4) . . . . ? B2 C6 C7 C8 -175.8(4) . . . . ? Fe1 C6 C7 C8 -59.8(3) . . . . ? C10 C6 C7 Fe1 59.0(3) . . . . ? B2 C6 C7 Fe1 -116.0(4) . . . . ? C6 C7 C8 C9 0.9(4) . . . . ? Fe1 C7 C8 C9 -59.0(3) . . . . ? C6 C7 C8 Fe1 59.9(3) . . . . ? C7 C8 C9 C10 -0.7(5) . . . . ? Fe1 C8 C9 C10 -59.5(3) . . . . ? C7 C8 C9 Fe1 58.8(3) . . . . ? C8 C9 C10 C6 0.2(5) . . . . ? Fe1 C9 C10 C6 -59.3(3) . . . . ? C8 C9 C10 Fe1 59.4(3) . . . . ? C7 C6 C10 C9 0.4(4) . . . . ? B2 C6 C10 C9 175.2(4) . . . . ? Fe1 C6 C10 C9 59.1(3) . . . . ? C7 C6 C10 Fe1 -58.7(3) . . . . ? B2 C6 C10 Fe1 116.2(4) . . . . ? O1 C12 C13 C11 51.9(4) . . . . ? O1 C12 C13 C14 171.9(3) . . . . ? O1 C12 C13 C15 -69.4(4) . . . . ? O2 C11 C13 C12 -54.5(4) . . . . ? O2 C11 C13 C14 -172.8(3) . . . . ? O2 C11 C13 C15 66.6(4) . . . . ? C12 C13 C14 O6 166.9(3) . . . . ? C11 C13 C14 O6 -74.6(4) . . . . ? C15 C13 C14 O6 47.2(5) . . . . ? C12 C13 C15 O5 -173.0(3) . . . . ? C11 C13 C15 O5 67.1(4) . . . . ? C14 C13 C15 O5 -54.8(4) . . . . ? O4 C16 C18 C20 169.7(3) . . . . ? O4 C16 C18 C17 49.7(4) . . . . ? O4 C16 C18 C19 -72.2(4) . . . . ? O3 C17 C18 C16 -54.1(4) . . . . ? O3 C17 C18 C20 -171.9(3) . . . . ? O3 C17 C18 C19 68.4(4) . . . . ? C16 C18 C19 O7 -170.9(3) . . . . ? C20 C18 C19 O7 -53.2(4) . . . . ? C17 C18 C19 O7 68.3(4) . . . . ? C16 C18 C20 O8 171.6(3) . . . . ? C17 C18 C20 O8 -69.8(4) . . . . ? C19 C18 C20 O8 51.4(4) . . . . ? C25 C21 C22 C23 -0.3(4) . . . . ? B3 C21 C22 C23 176.7(4) . . . . ? Fe2 C21 C22 C23 58.9(3) . . . . ? C25 C21 C22 Fe2 -59.1(3) . . . . ? B3 C21 C22 Fe2 117.9(4) . . . . ? C21 C22 C23 C24 0.1(5) . . . . ? Fe2 C22 C23 C24 58.8(3) . . . . ? C21 C22 C23 Fe2 -58.7(3) . . . . ? C22 C23 C24 C25 0.2(5) . . . . ? Fe2 C23 C24 C25 59.4(3) . . . . ? C22 C23 C24 Fe2 -59.2(3) . . . . ? C23 C24 C25 C21 -0.3(5) . . . . ? Fe2 C24 C25 C21 59.8(3) . . . . ? C23 C24 C25 Fe2 -60.1(3) . . . . ? C22 C21 C25 C24 0.4(4) . . . . ? B3 C21 C25 C24 -176.7(4) . . . . ? Fe2 C21 C25 C24 -59.5(3) . . . . ? C22 C21 C25 Fe2 59.9(3) . . . . ? B3 C21 C25 Fe2 -117.1(4) . . . . ? C30 C26 C27 C28 -0.1(5) . . . . ? B4 C26 C27 C28 176.3(4) . . . . ? Fe2 C26 C27 C28 59.0(3) . . . . ? C30 C26 C27 Fe2 -59.1(3) . . . . ? B4 C26 C27 Fe2 117.4(4) . . . . ? C26 C27 C28 C29 0.4(5) . . . . ? Fe2 C27 C28 C29 59.8(3) . . . . ? C26 C27 C28 Fe2 -59.4(3) . . . . ? C27 C28 C29 C30 -0.5(5) . . . . ? Fe2 C28 C29 C30 59.2(3) . . . . ? C27 C28 C29 Fe2 -59.8(3) . . . . ? C28 C29 C30 C26 0.5(5) . . . . ? Fe2 C29 C30 C26 59.6(3) . . . . ? C28 C29 C30 Fe2 -59.1(3) . . . . ? C27 C26 C30 C29 -0.3(5) . . . . ? B4 C26 C30 C29 -176.7(4) . . . . ? Fe2 C26 C30 C29 -59.3(3) . . . . ? C27 C26 C30 Fe2 59.0(3) . . . . ? B4 C26 C30 Fe2 -117.4(4) . . . . ? C13 C12 O1 B1 -25.6(5) . . . . ? C13 C11 O2 B1 31.5(5) . . . . ? C18 C17 O3 B2 32.2(5) . . . . ? C18 C16 O4 B2 -23.5(5) . . . . ? C13 C15 O5 B3 34.3(5) . . . . ? C13 C14 O6 B3 -19.0(6) . . . . ? C18 C19 O7 B4 30.4(5) . . . . ? C18 C20 O8 B4 -25.7(5) . . . . ? C8 C7 Fe1 C5 -42.1(7) . . . . ? C6 C7 Fe1 C5 -160.9(6) . . . . ? C8 C7 Fe1 C9 37.4(3) . . . . ? C6 C7 Fe1 C9 -81.4(3) . . . . ? C8 C7 Fe1 C10 80.9(3) . . . . ? C6 C7 Fe1 C10 -37.9(2) . . . . ? C8 C7 Fe1 C3 -112.7(3) . . . . ? C6 C7 Fe1 C3 128.4(3) . . . . ? C6 C7 Fe1 C8 -118.9(4) . . . . ? C8 C7 Fe1 C4 -72.1(3) . . . . ? C6 C7 Fe1 C4 169.0(2) . . . . ? C8 C7 Fe1 C6 118.9(4) . . . . ? C8 C7 Fe1 C2 -154.8(3) . . . . ? C6 C7 Fe1 C2 86.3(3) . . . . ? C8 C7 Fe1 C1 171.7(4) . . . . ? C6 C7 Fe1 C1 52.9(5) . . . . ? C4 C5 Fe1 C7 -39.0(7) . . . . ? C1 C5 Fe1 C7 -158.6(6) . . . . ? C4 C5 Fe1 C9 -112.5(3) . . . . ? C1 C5 Fe1 C9 127.8(3) . . . . ? C4 C5 Fe1 C10 -154.6(3) . . . . ? C1 C5 Fe1 C10 85.7(3) . . . . ? C4 C5 Fe1 C3 37.7(3) . . . . ? C1 C5 Fe1 C3 -82.0(3) . . . . ? C4 C5 Fe1 C8 -71.4(3) . . . . ? C1 C5 Fe1 C8 168.9(3) . . . . ? C1 C5 Fe1 C4 -119.7(4) . . . . ? C4 C5 Fe1 C6 171.2(4) . . . . ? C1 C5 Fe1 C6 51.5(5) . . . . ? C4 C5 Fe1 C2 81.4(3) . . . . ? C1 C5 Fe1 C2 -38.3(3) . . . . ? C4 C5 Fe1 C1 119.7(4) . . . . ? C10 C9 Fe1 C7 81.7(3) . . . . ? C8 C9 Fe1 C7 -37.5(3) . . . . ? C10 C9 Fe1 C5 -116.1(3) . . . . ? C8 C9 Fe1 C5 124.6(3) . . . . ? C8 C9 Fe1 C10 -119.3(4) . . . . ? C10 C9 Fe1 C3 168.5(4) . . . . ? C8 C9 Fe1 C3 49.2(5) . . . . ? C10 C9 Fe1 C8 119.3(4) . . . . ? C10 C9 Fe1 C4 -159.1(3) . . . . ? C8 C9 Fe1 C4 81.7(3) . . . . ? C10 C9 Fe1 C6 37.2(3) . . . . ? C8 C9 Fe1 C6 -82.0(3) . . . . ? C10 C9 Fe1 C2 -47.9(8) . . . . ? C8 C9 Fe1 C2 -167.2(7) . . . . ? C10 C9 Fe1 C1 -75.6(3) . . . . ? C8 C9 Fe1 C1 165.1(2) . . . . ? C9 C10 Fe1 C7 -81.8(3) . . . . ? C6 C10 Fe1 C7 38.5(2) . . . . ? C9 C10 Fe1 C5 81.5(3) . . . . ? C6 C10 Fe1 C5 -158.3(2) . . . . ? C6 C10 Fe1 C9 120.2(4) . . . . ? C9 C10 Fe1 C3 -156.0(7) . . . . ? C6 C10 Fe1 C3 -35.8(9) . . . . ? C9 C10 Fe1 C8 -37.8(3) . . . . ? C6 C10 Fe1 C8 82.5(3) . . . . ? C9 C10 Fe1 C4 43.8(5) . . . . ? C6 C10 Fe1 C4 164.0(3) . . . . ? C9 C10 Fe1 C6 -120.2(4) . . . . ? C9 C10 Fe1 C2 166.7(3) . . . . ? C6 C10 Fe1 C2 -73.1(3) . . . . ? C9 C10 Fe1 C1 125.2(3) . . . . ? C6 C10 Fe1 C1 -114.6(3) . . . . ? C4 C3 Fe1 C7 124.2(3) . . . . ? C2 C3 Fe1 C7 -116.0(3) . . . . ? C4 C3 Fe1 C5 -38.2(2) . . . . ? C2 C3 Fe1 C5 81.7(3) . . . . ? C4 C3 Fe1 C9 47.5(5) . . . . ? C2 C3 Fe1 C9 167.3(4) . . . . ? C4 C3 Fe1 C10 -166.1(7) . . . . ? C2 C3 Fe1 C10 -46.3(9) . . . . ? C4 C3 Fe1 C8 81.3(3) . . . . ? C2 C3 Fe1 C8 -158.8(3) . . . . ? C2 C3 Fe1 C4 119.9(4) . . . . ? C4 C3 Fe1 C6 165.0(2) . . . . ? C2 C3 Fe1 C6 -75.1(3) . . . . ? C4 C3 Fe1 C2 -119.9(4) . . . . ? C4 C3 Fe1 C1 -82.3(3) . . . . ? C2 C3 Fe1 C1 37.6(3) . . . . ? C9 C8 Fe1 C7 119.7(4) . . . . ? C9 C8 Fe1 C5 -74.5(3) . . . . ? C7 C8 Fe1 C5 165.9(3) . . . . ? C7 C8 Fe1 C9 -119.7(4) . . . . ? C9 C8 Fe1 C10 37.5(3) . . . . ? C7 C8 Fe1 C10 -82.2(3) . . . . ? C9 C8 Fe1 C3 -156.0(3) . . . . ? C7 C8 Fe1 C3 84.3(3) . . . . ? C9 C8 Fe1 C4 -114.5(3) . . . . ? C7 C8 Fe1 C4 125.8(3) . . . . ? C9 C8 Fe1 C6 81.4(3) . . . . ? C7 C8 Fe1 C6 -38.3(3) . . . . ? C9 C8 Fe1 C2 173.3(3) . . . . ? C7 C8 Fe1 C2 53.7(5) . . . . ? C9 C8 Fe1 C1 -47.5(7) . . . . ? C7 C8 Fe1 C1 -167.2(6) . . . . ? C3 C4 Fe1 C7 -74.5(3) . . . . ? C5 C4 Fe1 C7 166.8(3) . . . . ? C3 C4 Fe1 C5 118.7(4) . . . . ? C3 C4 Fe1 C9 -156.7(3) . . . . ? C5 C4 Fe1 C9 84.6(3) . . . . ? C3 C4 Fe1 C10 173.0(3) . . . . ? C5 C4 Fe1 C10 54.2(5) . . . . ? C5 C4 Fe1 C3 -118.7(4) . . . . ? C3 C4 Fe1 C8 -114.7(3) . . . . ? C5 C4 Fe1 C8 126.6(3) . . . . ? C3 C4 Fe1 C6 -47.5(7) . . . . ? C5 C4 Fe1 C6 -166.2(5) . . . . ? C3 C4 Fe1 C2 37.3(2) . . . . ? C5 C4 Fe1 C2 -81.4(3) . . . . ? C3 C4 Fe1 C1 81.2(3) . . . . ? C5 C4 Fe1 C1 -37.5(3) . . . . ? C10 C6 Fe1 C7 -118.6(4) . . . . ? B2 C6 Fe1 C7 119.8(5) . . . . ? C10 C6 Fe1 C5 48.3(5) . . . . ? C7 C6 Fe1 C5 166.9(4) . . . . ? B2 C6 Fe1 C5 -73.3(6) . . . . ? C10 C6 Fe1 C9 -37.0(3) . . . . ? C7 C6 Fe1 C9 81.6(3) . . . . ? B2 C6 Fe1 C9 -158.5(4) . . . . ? C7 C6 Fe1 C10 118.6(4) . . . . ? B2 C6 Fe1 C10 -121.6(5) . . . . ? C10 C6 Fe1 C3 170.0(2) . . . . ? C7 C6 Fe1 C3 -71.4(3) . . . . ? B2 C6 Fe1 C3 48.4(4) . . . . ? C10 C6 Fe1 C8 -80.7(3) . . . . ? C7 C6 Fe1 C8 37.8(3) . . . . ? B2 C6 Fe1 C8 157.7(4) . . . . ? C10 C6 Fe1 C4 -152.9(6) . . . . ? C7 C6 Fe1 C4 -34.3(7) . . . . ? B2 C6 Fe1 C4 85.5(7) . . . . ? C10 C6 Fe1 C2 128.4(3) . . . . ? C7 C6 Fe1 C2 -113.1(3) . . . . ? B2 C6 Fe1 C2 6.8(4) . . . . ? C10 C6 Fe1 C1 84.7(3) . . . . ? C7 C6 Fe1 C1 -156.7(3) . . . . ? B2 C6 Fe1 C1 -36.8(4) . . . . ? C3 C2 Fe1 C7 81.5(3) . . . . ? C1 C2 Fe1 C7 -158.8(2) . . . . ? C3 C2 Fe1 C5 -81.3(3) . . . . ? C1 C2 Fe1 C5 38.4(2) . . . . ? C3 C2 Fe1 C9 -154.1(7) . . . . ? C1 C2 Fe1 C9 -34.5(8) . . . . ? C3 C2 Fe1 C10 167.3(3) . . . . ? C1 C2 Fe1 C10 -73.0(3) . . . . ? C1 C2 Fe1 C3 119.7(4) . . . . ? C3 C2 Fe1 C8 44.2(5) . . . . ? C1 C2 Fe1 C8 163.9(3) . . . . ? C3 C2 Fe1 C4 -37.1(3) . . . . ? C1 C2 Fe1 C4 82.5(3) . . . . ? C3 C2 Fe1 C6 125.8(3) . . . . ? C1 C2 Fe1 C6 -114.5(3) . . . . ? C3 C2 Fe1 C1 -119.7(4) . . . . ? C5 C1 Fe1 C7 165.3(4) . . . . ? C2 C1 Fe1 C7 47.2(5) . . . . ? B1 C1 Fe1 C7 -73.3(6) . . . . ? C2 C1 Fe1 C5 -118.1(4) . . . . ? B1 C1 Fe1 C5 121.4(5) . . . . ? C5 C1 Fe1 C9 -71.7(3) . . . . ? C2 C1 Fe1 C9 170.2(2) . . . . ? B1 C1 Fe1 C9 49.7(4) . . . . ? C5 C1 Fe1 C10 -113.4(3) . . . . ? C2 C1 Fe1 C10 128.4(3) . . . . ? B1 C1 Fe1 C10 8.0(4) . . . . ? C5 C1 Fe1 C3 80.9(3) . . . . ? C2 C1 Fe1 C3 -37.3(3) . . . . ? B1 C1 Fe1 C3 -157.7(4) . . . . ? C5 C1 Fe1 C8 -34.5(7) . . . . ? C2 C1 Fe1 C8 -152.6(6) . . . . ? B1 C1 Fe1 C8 86.9(7) . . . . ? C5 C1 Fe1 C4 37.5(3) . . . . ? C2 C1 Fe1 C4 -80.6(3) . . . . ? B1 C1 Fe1 C4 158.9(4) . . . . ? C5 C1 Fe1 C6 -157.0(3) . . . . ? C2 C1 Fe1 C6 84.9(3) . . . . ? B1 C1 Fe1 C6 -35.6(4) . . . . ? C5 C1 Fe1 C2 118.1(4) . . . . ? B1 C1 Fe1 C2 -120.4(5) . . . . ? C21 C25 Fe2 C24 -119.5(3) . . . . ? C24 C25 Fe2 C28 -110.7(3) . . . . ? C21 C25 Fe2 C28 129.8(2) . . . . ? C24 C25 Fe2 C29 -70.8(3) . . . . ? C21 C25 Fe2 C29 169.6(2) . . . . ? C24 C25 Fe2 C27 -152.5(3) . . . . ? C21 C25 Fe2 C27 88.0(3) . . . . ? C24 C25 Fe2 C30 -44.6(7) . . . . ? C21 C25 Fe2 C30 -164.1(5) . . . . ? C24 C25 Fe2 C21 119.5(3) . . . . ? C24 C25 Fe2 C23 37.5(3) . . . . ? C21 C25 Fe2 C23 -82.0(3) . . . . ? C24 C25 Fe2 C22 81.1(3) . . . . ? C21 C25 Fe2 C22 -38.4(2) . . . . ? C24 C25 Fe2 C26 176.2(4) . . . . ? C21 C25 Fe2 C26 56.7(5) . . . . ? C23 C24 Fe2 C25 119.0(4) . . . . ? C23 C24 Fe2 C28 -156.5(3) . . . . ? C25 C24 Fe2 C28 84.5(3) . . . . ? C23 C24 Fe2 C29 -114.8(3) . . . . ? C25 C24 Fe2 C29 126.2(3) . . . . ? C23 C24 Fe2 C27 174.5(3) . . . . ? C25 C24 Fe2 C27 55.5(4) . . . . ? C23 C24 Fe2 C30 -76.3(3) . . . . ? C25 C24 Fe2 C30 164.7(2) . . . . ? C23 C24 Fe2 C21 81.2(3) . . . . ? C25 C24 Fe2 C21 -37.8(2) . . . . ? C25 C24 Fe2 C23 -119.0(4) . . . . ? C23 C24 Fe2 C22 37.3(2) . . . . ? C25 C24 Fe2 C22 -81.7(3) . . . . ? C23 C24 Fe2 C26 -54.7(7) . . . . ? C25 C24 Fe2 C26 -173.7(6) . . . . ? C29 C28 Fe2 C25 125.2(3) . . . . ? C27 C28 Fe2 C25 -116.0(3) . . . . ? C29 C28 Fe2 C24 82.8(3) . . . . ? C27 C28 Fe2 C24 -158.5(3) . . . . ? C27 C28 Fe2 C29 118.8(4) . . . . ? C29 C28 Fe2 C27 -118.8(4) . . . . ? C29 C28 Fe2 C30 -37.2(3) . . . . ? C27 C28 Fe2 C30 81.6(3) . . . . ? C29 C28 Fe2 C21 164.5(3) . . . . ? C27 C28 Fe2 C21 -76.7(3) . . . . ? C29 C28 Fe2 C23 52.6(5) . . . . ? C27 C28 Fe2 C23 171.3(3) . . . . ? C29 C28 Fe2 C22 -176.7(7) . . . . ? C27 C28 Fe2 C22 -57.9(9) . . . . ? C29 C28 Fe2 C26 -81.3(3) . . . . ? C27 C28 Fe2 C26 37.5(3) . . . . ? C30 C29 Fe2 C25 167.9(2) . . . . ? C28 C29 Fe2 C25 -72.3(3) . . . . ? C30 C29 Fe2 C24 128.3(3) . . . . ? C28 C29 Fe2 C24 -111.9(3) . . . . ? C30 C29 Fe2 C28 -119.8(4) . . . . ? C30 C29 Fe2 C27 -81.8(3) . . . . ? C28 C29 Fe2 C27 38.0(3) . . . . ? C28 C29 Fe2 C30 119.8(4) . . . . ? C30 C29 Fe2 C21 -167.8(5) . . . . ? C28 C29 Fe2 C21 -48.0(7) . . . . ? C30 C29 Fe2 C23 87.3(3) . . . . ? C28 C29 Fe2 C23 -152.9(3) . . . . ? C30 C29 Fe2 C22 58.6(5) . . . . ? C28 C29 Fe2 C22 178.4(3) . . . . ? C30 C29 Fe2 C26 -37.6(3) . . . . ? C28 C29 Fe2 C26 82.3(3) . . . . ? C28 C27 Fe2 C25 80.2(3) . . . . ? C26 C27 Fe2 C25 -159.8(2) . . . . ? C28 C27 Fe2 C24 42.4(5) . . . . ? C26 C27 Fe2 C24 162.4(3) . . . . ? C26 C27 Fe2 C28 120.0(4) . . . . ? C28 C27 Fe2 C29 -37.8(3) . . . . ? C26 C27 Fe2 C29 82.1(3) . . . . ? C28 C27 Fe2 C30 -81.5(3) . . . . ? C26 C27 Fe2 C30 38.5(2) . . . . ? C28 C27 Fe2 C21 124.4(3) . . . . ? C26 C27 Fe2 C21 -115.6(3) . . . . ? C28 C27 Fe2 C23 -156.3(9) . . . . ? C26 C27 Fe2 C23 -36.4(10) . . . . ? C28 C27 Fe2 C22 165.3(3) . . . . ? C26 C27 Fe2 C22 -74.7(3) . . . . ? C28 C27 Fe2 C26 -120.0(4) . . . . ? C29 C30 Fe2 C25 -34.4(7) . . . . ? C26 C30 Fe2 C25 -154.3(5) . . . . ? C29 C30 Fe2 C24 -68.6(3) . . . . ? C26 C30 Fe2 C24 171.5(2) . . . . ? C29 C30 Fe2 C28 37.3(3) . . . . ? C26 C30 Fe2 C28 -82.5(3) . . . . ? C26 C30 Fe2 C29 -119.9(4) . . . . ? C29 C30 Fe2 C27 81.3(3) . . . . ? C26 C30 Fe2 C27 -38.6(2) . . . . ? C29 C30 Fe2 C21 171.5(4) . . . . ? C26 C30 Fe2 C21 51.6(5) . . . . ? C29 C30 Fe2 C23 -110.0(3) . . . . ? C26 C30 Fe2 C23 130.1(3) . . . . ? C29 C30 Fe2 C22 -152.5(3) . . . . ? C26 C30 Fe2 C22 87.7(3) . . . . ? C29 C30 Fe2 C26 119.9(4) . . . . ? C22 C21 Fe2 C25 -117.9(3) . . . . ? B3 C21 Fe2 C25 120.4(4) . . . . ? C22 C21 Fe2 C24 -80.3(3) . . . . ? C25 C21 Fe2 C24 37.6(2) . . . . ? B3 C21 Fe2 C24 157.9(4) . . . . ? C22 C21 Fe2 C28 173.7(2) . . . . ? C25 C21 Fe2 C28 -68.4(3) . . . . ? B3 C21 Fe2 C28 51.9(4) . . . . ? C22 C21 Fe2 C29 -149.1(6) . . . . ? C25 C21 Fe2 C29 -31.2(7) . . . . ? B3 C21 Fe2 C29 89.2(7) . . . . ? C22 C21 Fe2 C27 131.2(2) . . . . ? C25 C21 Fe2 C27 -110.9(3) . . . . ? B3 C21 Fe2 C27 9.5(4) . . . . ? C22 C21 Fe2 C30 50.3(5) . . . . ? C25 C21 Fe2 C30 168.2(4) . . . . ? B3 C21 Fe2 C30 -71.4(5) . . . . ? C22 C21 Fe2 C23 -37.0(2) . . . . ? C25 C21 Fe2 C23 80.9(3) . . . . ? B3 C21 Fe2 C23 -158.8(4) . . . . ? C25 C21 Fe2 C22 117.9(3) . . . . ? B3 C21 Fe2 C22 -121.7(4) . . . . ? C22 C21 Fe2 C26 87.3(3) . . . . ? C25 C21 Fe2 C26 -154.8(2) . . . . ? B3 C21 Fe2 C26 -34.4(4) . . . . ? C24 C23 Fe2 C25 -38.1(3) . . . . ? C22 C23 Fe2 C25 81.8(3) . . . . ? C22 C23 Fe2 C24 119.8(4) . . . . ? C24 C23 Fe2 C28 45.0(5) . . . . ? C22 C23 Fe2 C28 164.8(3) . . . . ? C24 C23 Fe2 C29 80.3(3) . . . . ? C22 C23 Fe2 C29 -159.9(3) . . . . ? C24 C23 Fe2 C27 -165.8(8) . . . . ? C22 C23 Fe2 C27 -45.9(10) . . . . ? C24 C23 Fe2 C30 123.2(3) . . . . ? C22 C23 Fe2 C30 -116.9(3) . . . . ? C24 C23 Fe2 C21 -82.4(3) . . . . ? C22 C23 Fe2 C21 37.4(2) . . . . ? C24 C23 Fe2 C22 -119.8(4) . . . . ? C24 C23 Fe2 C26 163.8(3) . . . . ? C22 C23 Fe2 C26 -76.3(3) . . . . ? C23 C22 Fe2 C25 -81.3(3) . . . . ? C21 C22 Fe2 C25 38.7(2) . . . . ? C23 C22 Fe2 C24 -37.1(3) . . . . ? C21 C22 Fe2 C24 82.8(3) . . . . ? C23 C22 Fe2 C28 -143.2(7) . . . . ? C21 C22 Fe2 C28 -23.2(9) . . . . ? C23 C22 Fe2 C29 41.5(5) . . . . ? C21 C22 Fe2 C29 161.4(4) . . . . ? C23 C22 Fe2 C27 169.4(3) . . . . ? C21 C22 Fe2 C27 -70.6(3) . . . . ? C23 C22 Fe2 C30 81.7(3) . . . . ? C21 C22 Fe2 C30 -158.3(2) . . . . ? C23 C22 Fe2 C21 -120.0(4) . . . . ? C21 C22 Fe2 C23 120.0(4) . . . . ? C23 C22 Fe2 C26 126.5(3) . . . . ? C21 C22 Fe2 C26 -113.5(3) . . . . ? C30 C26 Fe2 C25 162.1(4) . . . . ? C27 C26 Fe2 C25 44.2(5) . . . . ? B4 C26 Fe2 C25 -77.2(5) . . . . ? C30 C26 Fe2 C24 -27.4(8) . . . . ? C27 C26 Fe2 C24 -145.3(6) . . . . ? B4 C26 Fe2 C24 93.3(7) . . . . ? C30 C26 Fe2 C28 80.7(3) . . . . ? C27 C26 Fe2 C28 -37.2(3) . . . . ? B4 C26 Fe2 C28 -158.6(4) . . . . ? C30 C26 Fe2 C29 37.1(3) . . . . ? C27 C26 Fe2 C29 -80.8(3) . . . . ? B4 C26 Fe2 C29 157.8(4) . . . . ? C30 C26 Fe2 C27 117.9(4) . . . . ? B4 C26 Fe2 C27 -121.4(5) . . . . ? C27 C26 Fe2 C30 -117.9(4) . . . . ? B4 C26 Fe2 C30 120.7(5) . . . . ? C30 C26 Fe2 C21 -157.8(2) . . . . ? C27 C26 Fe2 C21 84.3(3) . . . . ? B4 C26 Fe2 C21 -37.1(4) . . . . ? C30 C26 Fe2 C23 -70.6(3) . . . . ? C27 C26 Fe2 C23 171.5(3) . . . . ? B4 C26 Fe2 C23 50.1(4) . . . . ? C30 C26 Fe2 C22 -113.2(3) . . . . ? C27 C26 Fe2 C22 128.9(2) . . . . ? B4 C26 Fe2 C22 7.5(4) . . . . ? C11 O2 B1 O1 -3.0(6) . . . . ? C11 O2 B1 C1 175.6(3) . . . . ? C12 O1 B1 O2 -0.4(6) . . . . ? C12 O1 B1 C1 -179.0(3) . . . . ? C5 C1 B1 O2 -173.5(4) . . . . ? C2 C1 B1 O2 6.2(6) . . . . ? Fe1 C1 B1 O2 96.4(4) . . . . ? C5 C1 B1 O1 5.1(6) . . . . ? C2 C1 B1 O1 -175.2(4) . . . . ? Fe1 C1 B1 O1 -85.0(4) . . . . ? C17 O3 B2 O4 -3.6(6) . . . . ? C17 O3 B2 C6 176.0(3) . . . . ? C16 O4 B2 O3 -1.2(6) . . . . ? C16 O4 B2 C6 179.2(3) . . . . ? C10 C6 B2 O3 13.4(6) . . . . ? C7 C6 B2 O3 -172.6(4) . . . . ? Fe1 C6 B2 O3 101.1(4) . . . . ? C10 C6 B2 O4 -167.0(4) . . . . ? C7 C6 B2 O4 7.0(6) . . . . ? Fe1 C6 B2 O4 -79.3(4) . . . . ? C14 O6 B3 O5 -4.6(6) . . . . ? C14 O6 B3 C21 177.4(4) . . . . ? C15 O5 B3 O6 -3.7(6) . . . . ? C15 O5 B3 C21 174.2(3) . . . . ? C22 C21 B3 O6 -171.3(4) . . . . ? C25 C21 B3 O6 5.2(6) . . . . ? Fe2 C21 B3 O6 -82.0(5) . . . . ? C22 C21 B3 O5 10.7(6) . . . . ? C25 C21 B3 O5 -172.9(4) . . . . ? Fe2 C21 B3 O5 99.9(4) . . . . ? C19 O7 B4 O8 -1.9(6) . . . . ? C19 O7 B4 C26 176.3(3) . . . . ? C20 O8 B4 O7 -0.7(6) . . . . ? C20 O8 B4 C26 -179.0(3) . . . . ? C30 C26 B4 O7 -176.2(4) . . . . ? C27 C26 B4 O7 8.1(6) . . . . ? Fe2 C26 B4 O7 96.1(4) . . . . ? C30 C26 B4 O8 2.1(6) . . . . ? C27 C26 B4 O8 -173.6(4) . . . . ? Fe2 C26 B4 O8 -85.6(5) . . . . ? Cl2B C31 Cl2A Cl3A -171.0(12) . . . . ? Cl2C C31 Cl2A Cl3A -176.0(5) . . . . ? Cl1A C31 Cl2A Cl3A 148.5(4) . . . . ? Cl3C C31 Cl2A Cl3A 29.7(4) . . . . ? Cl1C C31 Cl2A Cl3A 96.0(6) . . . . ? Cl3B C31 Cl2A Cl3A 20.4(3) . . . . ? Cl1B C31 Cl2A Cl3A 135.6(5) . . . . ? Cl2B C31 Cl3A Cl2A 2.4(3) . . . . ? Cl2C C31 Cl3A Cl2A 2.7(3) . . . . ? Cl1A C31 Cl3A Cl2A -93.9(8) . . . . ? Cl3C C31 Cl3A Cl2A -141.5(4) . . . . ? Cl1C C31 Cl3A Cl2A -123.3(5) . . . . ? Cl3B C31 Cl3A Cl2A -142.9(5) . . . . ? Cl1B C31 Cl3A Cl2A -117.8(6) . . . . ? Cl2B C31 Cl1C Cl3C -110.6(6) . . . . ? Cl2C C31 Cl1C Cl3C -137.4(5) . . . . ? Cl1A C31 Cl1C Cl3C -176.9(6) . . . . ? Cl3A C31 Cl1C Cl3C -15.8(4) . . . . ? Cl3B C31 Cl1C Cl3C -4.3(3) . . . . ? Cl1B C31 Cl1C Cl3C 171.0(8) . . . . ? Cl2A C31 Cl1C Cl3C -91.6(5) . . . . ? Cl2B C31 Cl3C Cl1C 115.9(6) . . . . ? Cl2C C31 Cl3C Cl1C 95.0(7) . . . . ? Cl1A C31 Cl3C Cl1C 2.4(4) . . . . ? Cl3A C31 Cl3C Cl1C 159.9(6) . . . . ? Cl3B C31 Cl3C Cl1C 163.1(13) . . . . ? Cl1B C31 Cl3C Cl1C -4.8(4) . . . . ? Cl2A C31 Cl3C Cl1C 122.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.883 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.086 # Attachment '4_revised.cif' data_2006src1374 _database_code_depnum_ccdc_archive 'CCDC 645161' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dr S. Aldridge ; _chemical_name_common 'Dr S. Aldridge' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H40 B4 Fe2 O8' _chemical_formula_weight 755.62 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' O O 0.0106 0.0060 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P bcn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 19.6222(11) _cell_length_b 7.8609(3) _cell_length_c 21.3982(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3300.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4105 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description Plate _exptl_crystal_colour Brown _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 0.934 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8425 _exptl_absorpt_correction_T_max 0.9907 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; SADABS was used to perform the Absorption correction Parameter refinement on 19154 reflections reduced R(int) from 0.2526 to 0.1054 Ratio of minimum to maximum apparent transmission: 0.669862 The given Tmin and Tmax were generated using the SHELX SIZE command. ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25134 _diffrn_reflns_av_R_equivalents 0.1290 _diffrn_reflns_av_sigmaI/netI 0.0793 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3366 _reflns_number_gt 2254 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep3 for Windows (Farrugia, L.J., 1997)' _computing_publication_material 'WinGX (Farrugia, 1999)' _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. ; _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^)+(0.0000P)^2^+18.2477P] 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 3366 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1451 _refine_ls_R_factor_gt 0.0905 _refine_ls_wR_factor_ref 0.1676 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.219 _refine_ls_restrained_S_all 1.219 _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 C1 C 0.5953(3) 0.2405(8) 0.4634(3) 0.0303(15) Uani 1 1 d . . . C2 C 0.6610(3) 0.1926(8) 0.4393(3) 0.0313(15) Uani 1 1 d . . . H2 H 0.6702 0.0933 0.4155 0.038 Uiso 1 1 calc R . . C3 C 0.7095(4) 0.3159(8) 0.4566(3) 0.0387(17) Uani 1 1 d . . . H3 H 0.7565 0.3157 0.4459 0.046 Uiso 1 1 calc R . . C4 C 0.6756(4) 0.4399(8) 0.4928(3) 0.0342(16) Uani 1 1 d . . . H4 H 0.6962 0.5368 0.5115 0.041 Uiso 1 1 calc R . . C5 C 0.6055(4) 0.3954(8) 0.4966(3) 0.0320(15) Uani 1 1 d . . . H5 H 0.5713 0.4584 0.5178 0.038 Uiso 1 1 calc R . . C6 C 0.6293(3) 0.4174(8) 0.3101(2) 0.0302(14) Uani 1 1 d . . . C7 C 0.6692(4) 0.5590(8) 0.3318(3) 0.0336(15) Uani 1 1 d . . . H7 H 0.7160 0.5791 0.3231 0.040 Uiso 1 1 calc R . . C8 C 0.6256(4) 0.6638(8) 0.3688(3) 0.0367(17) Uani 1 1 d . . . H8 H 0.6386 0.7666 0.3888 0.044 Uiso 1 1 calc R . . C9 C 0.5609(4) 0.5916(8) 0.3708(3) 0.0382(17) Uani 1 1 d . . . H9 H 0.5226 0.6358 0.3926 0.046 Uiso 1 1 calc R . . C10 C 0.5621(3) 0.4419(8) 0.3350(3) 0.0326(15) Uani 1 1 d . . . H10 H 0.5243 0.3684 0.3283 0.039 Uiso 1 1 calc R . . C11 C 0.4505(3) -0.0236(7) 0.4009(3) 0.0298(14) Uani 1 1 d . . . H11 H 0.4295 -0.1284 0.4192 0.036 Uiso 1 1 calc R . . C12 C 0.4122(3) 0.1345(8) 0.4264(3) 0.0301(15) Uani 1 1 d . . . H12 H 0.3854 0.1008 0.4642 0.036 Uiso 1 1 calc R . . C13 C 0.3660(3) 0.2235(8) 0.3813(3) 0.0321(14) Uani 1 1 d . . . H13A H 0.3915 0.2484 0.3425 0.039 Uiso 1 1 calc R . . H13B H 0.3514 0.3334 0.3996 0.039 Uiso 1 1 calc R . . C14 C 0.3024(3) 0.1176(8) 0.3651(3) 0.0330(15) Uani 1 1 d . . . H14A H 0.3058 0.0066 0.3868 0.040 Uiso 1 1 calc R . . H14B H 0.2618 0.1769 0.3816 0.040 Uiso 1 1 calc R . . C15 C 0.2919(3) 0.0850(8) 0.2955(3) 0.0310(14) Uani 1 1 d . . . H15 H 0.2470 0.0272 0.2894 0.037 Uiso 1 1 calc R . . C16 C 0.3476(3) -0.0168(8) 0.2604(3) 0.0325(15) Uani 1 1 d . . . H16 H 0.3239 -0.0903 0.2290 0.039 Uiso 1 1 calc R . . C17 C 0.3968(4) -0.1314(8) 0.2968(3) 0.0339(15) Uani 1 1 d . . . H17A H 0.3701 -0.1939 0.3286 0.041 Uiso 1 1 calc R . . H17B H 0.4154 -0.2169 0.2673 0.041 Uiso 1 1 calc R . . C18 C 0.4567(3) -0.0464(7) 0.3298(3) 0.0269(14) Uani 1 1 d . . . H18A H 0.4637 0.0671 0.3108 0.032 Uiso 1 1 calc R . . H18B H 0.4982 -0.1144 0.3212 0.032 Uiso 1 1 calc R . . O1 O 0.5194(2) -0.0051(5) 0.42534(18) 0.0335(11) Uani 1 1 d . . . O2 O 0.4665(2) 0.2486(5) 0.44525(18) 0.0315(10) Uani 1 1 d . . . O3 O 0.2909(2) 0.2472(5) 0.26278(19) 0.0332(10) Uani 1 1 d . . . O4 O 0.3857(2) 0.1106(5) 0.22565(17) 0.0325(11) Uani 1 1 d . . . Fe1 Fe 0.63157(5) 0.42479(10) 0.40583(4) 0.0275(2) Uani 1 1 d . . . B1 B 0.5271(4) 0.1592(9) 0.4453(3) 0.0286(17) Uani 1 1 d . . . B2 B 0.3486(4) 0.2561(9) 0.2260(3) 0.0301(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(4) 0.028(3) 0.023(3) 0.009(3) -0.001(3) 0.002(3) C2 0.046(4) 0.024(3) 0.024(3) 0.004(3) 0.000(3) 0.012(3) C3 0.037(4) 0.036(4) 0.043(4) 0.008(3) -0.004(3) 0.002(3) C4 0.049(4) 0.031(4) 0.023(3) 0.002(3) -0.009(3) -0.002(3) C5 0.047(4) 0.031(4) 0.018(3) 0.001(3) -0.004(3) 0.002(3) C6 0.046(4) 0.027(3) 0.017(2) 0.002(2) 0.001(3) 0.001(3) C7 0.049(4) 0.031(3) 0.021(3) 0.006(3) 0.001(3) -0.007(3) C8 0.067(5) 0.020(3) 0.023(3) 0.003(2) 0.001(3) -0.003(3) C9 0.054(5) 0.031(4) 0.029(3) 0.010(3) 0.009(3) 0.015(4) C10 0.037(4) 0.040(4) 0.020(3) 0.005(3) -0.006(3) 0.000(3) C11 0.038(4) 0.024(3) 0.027(3) 0.007(3) 0.002(3) -0.005(3) C12 0.042(4) 0.026(3) 0.022(3) 0.005(2) 0.007(3) 0.002(3) C13 0.041(4) 0.028(3) 0.027(3) 0.000(3) 0.010(3) 0.002(3) C14 0.037(4) 0.032(4) 0.030(3) 0.002(3) 0.006(3) -0.005(3) C15 0.038(4) 0.023(3) 0.032(3) 0.003(3) -0.002(3) -0.004(3) C16 0.043(4) 0.025(3) 0.029(3) -0.002(3) -0.004(3) -0.005(3) C17 0.047(4) 0.030(3) 0.025(3) -0.001(3) 0.001(3) -0.004(3) C18 0.037(4) 0.021(3) 0.023(3) -0.001(2) 0.007(3) 0.009(3) O1 0.047(3) 0.026(2) 0.027(2) -0.0015(18) -0.003(2) 0.007(2) O2 0.037(3) 0.029(2) 0.029(2) -0.0049(19) 0.0005(19) -0.001(2) O3 0.038(3) 0.032(2) 0.030(2) 0.0003(19) 0.001(2) 0.002(2) O4 0.045(3) 0.030(2) 0.022(2) 0.0005(17) 0.0049(19) 0.002(2) Fe1 0.0417(5) 0.0229(4) 0.0178(4) 0.0010(4) 0.0021(4) 0.0044(4) B1 0.041(5) 0.031(4) 0.014(3) 0.005(3) 0.001(3) 0.003(4) B2 0.034(4) 0.031(4) 0.024(3) -0.008(3) -0.001(3) 0.000(3) _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 C1 C5 1.424(8) . ? C1 C2 1.439(9) . ? C1 B1 1.533(10) . ? C1 Fe1 2.031(6) . ? C2 C3 1.408(9) . ? C2 Fe1 2.044(6) . ? C2 H2 0.9500 . ? C3 C4 1.412(9) . ? C3 Fe1 2.063(7) . ? C3 H3 0.9500 . ? C4 C5 1.421(9) . ? C4 Fe1 2.056(6) . ? C4 H4 0.9500 . ? C5 Fe1 2.023(6) . ? C5 H5 0.9500 . ? C6 C10 1.434(9) . ? C6 C7 1.438(9) . ? C6 B2 1.547(9) 4_655 ? C6 Fe1 2.049(5) . ? C7 C8 1.427(9) . ? C7 Fe1 2.042(6) . ? C7 H7 0.9500 . ? C8 C9 1.391(9) . ? C8 Fe1 2.043(6) . ? C8 H8 0.9500 . ? C9 C10 1.404(9) . ? C9 Fe1 2.050(7) . ? C9 H9 0.9500 . ? C10 Fe1 2.043(6) . ? C10 H10 0.9500 . ? C11 O1 1.457(7) . ? C11 C18 1.538(7) . ? C11 C12 1.551(8) . ? C11 H11 1.0000 . ? C12 O2 1.450(7) . ? C12 C13 1.498(8) . ? C12 H12 1.0000 . ? C13 C14 1.539(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(8) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 O3 1.455(7) . ? C15 C16 1.550(8) . ? C15 H15 1.0000 . ? C16 O4 1.454(7) . ? C16 C17 1.532(9) . ? C16 H16 1.0000 . ? C17 C18 1.526(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? O1 B1 1.369(8) . ? O2 B1 1.382(9) . ? O3 B2 1.380(8) . ? O4 B2 1.356(8) . ? B2 C6 1.547(9) 4_655 ? 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 C5 C1 C2 106.1(6) . . ? C5 C1 B1 127.3(6) . . ? C2 C1 B1 125.6(6) . . ? C5 C1 Fe1 69.1(3) . . ? C2 C1 Fe1 69.8(3) . . ? B1 C1 Fe1 116.7(4) . . ? C3 C2 C1 109.3(6) . . ? C3 C2 Fe1 70.7(4) . . ? C1 C2 Fe1 68.8(3) . . ? C3 C2 H2 125.3 . . ? C1 C2 H2 125.3 . . ? Fe1 C2 H2 126.8 . . ? C2 C3 C4 107.5(6) . . ? C2 C3 Fe1 69.2(4) . . ? C4 C3 Fe1 69.7(4) . . ? C2 C3 H3 126.3 . . ? C4 C3 H3 126.3 . . ? Fe1 C3 H3 126.4 . . ? C3 C4 C5 108.5(6) . . ? C3 C4 Fe1 70.2(4) . . ? C5 C4 Fe1 68.4(3) . . ? C3 C4 H4 125.7 . . ? C5 C4 H4 125.7 . . ? Fe1 C4 H4 127.3 . . ? C4 C5 C1 108.5(6) . . ? C4 C5 Fe1 70.9(4) . . ? C1 C5 Fe1 69.7(3) . . ? C4 C5 H5 125.7 . . ? C1 C5 H5 125.7 . . ? Fe1 C5 H5 125.3 . . ? C10 C6 C7 106.1(5) . . ? C10 C6 B2 123.6(6) . 4_655 ? C7 C6 B2 129.9(6) . 4_655 ? C10 C6 Fe1 69.3(3) . . ? C7 C6 Fe1 69.1(3) . . ? B2 C6 Fe1 121.0(4) 4_655 . ? C8 C7 C6 107.3(6) . . ? C8 C7 Fe1 69.6(3) . . ? C6 C7 Fe1 69.7(3) . . ? C8 C7 H7 126.3 . . ? C6 C7 H7 126.3 . . ? Fe1 C7 H7 126.0 . . ? C9 C8 C7 109.2(6) . . ? C9 C8 Fe1 70.4(4) . . ? C7 C8 Fe1 69.5(3) . . ? C9 C8 H8 125.4 . . ? C7 C8 H8 125.4 . . ? Fe1 C8 H8 126.3 . . ? C8 C9 C10 108.1(6) . . ? C8 C9 Fe1 69.8(4) . . ? C10 C9 Fe1 69.7(4) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? Fe1 C9 H9 126.1 . . ? C9 C10 C6 109.2(6) . . ? C9 C10 Fe1 70.2(4) . . ? C6 C10 Fe1 69.7(3) . . ? C9 C10 H10 125.4 . . ? C6 C10 H10 125.4 . . ? Fe1 C10 H10 126.3 . . ? O1 C11 C18 107.0(5) . . ? O1 C11 C12 104.1(5) . . ? C18 C11 C12 118.7(5) . . ? O1 C11 H11 108.9 . . ? C18 C11 H11 108.9 . . ? C12 C11 H11 108.9 . . ? O2 C12 C13 109.6(5) . . ? O2 C12 C11 103.8(5) . . ? C13 C12 C11 116.2(5) . . ? O2 C12 H12 109.0 . . ? C13 C12 H12 109.0 . . ? C11 C12 H12 109.0 . . ? C12 C13 C14 112.5(5) . . ? C12 C13 H13A 109.1 . . ? C14 C13 H13A 109.1 . . ? C12 C13 H13B 109.1 . . ? C14 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C13 114.9(5) . . ? C15 C14 H14A 108.5 . . ? C13 C14 H14A 108.5 . . ? C15 C14 H14B 108.5 . . ? C13 C14 H14B 108.5 . . ? H14A C14 H14B 107.5 . . ? O3 C15 C14 109.0(5) . . ? O3 C15 C16 103.1(4) . . ? C14 C15 C16 117.7(5) . . ? O3 C15 H15 108.9 . . ? C14 C15 H15 108.9 . . ? C16 C15 H15 108.9 . . ? O4 C16 C17 109.9(5) . . ? O4 C16 C15 104.8(4) . . ? C17 C16 C15 120.1(5) . . ? O4 C16 H16 107.1 . . ? C17 C16 H16 107.1 . . ? C15 C16 H16 107.1 . . ? C18 C17 C16 117.6(5) . . ? C18 C17 H17A 107.9 . . ? C16 C17 H17A 107.9 . . ? C18 C17 H17B 107.9 . . ? C16 C17 H17B 107.9 . . ? H17A C17 H17B 107.2 . . ? C17 C18 C11 116.6(5) . . ? C17 C18 H18A 108.1 . . ? C11 C18 H18A 108.1 . . ? C17 C18 H18B 108.1 . . ? C11 C18 H18B 108.1 . . ? H18A C18 H18B 107.3 . . ? B1 O1 C11 108.0(5) . . ? B1 O2 C12 108.6(5) . . ? B2 O3 C15 108.0(5) . . ? B2 O4 C16 107.6(5) . . ? C5 Fe1 C1 41.1(2) . . ? C5 Fe1 C7 153.6(2) . . ? C1 Fe1 C7 165.1(2) . . ? C5 Fe1 C8 117.6(2) . . ? C1 Fe1 C8 150.7(3) . . ? C7 Fe1 C8 40.9(2) . . ? C5 Fe1 C10 123.5(3) . . ? C1 Fe1 C10 105.3(3) . . ? C7 Fe1 C10 68.4(3) . . ? C8 Fe1 C10 67.2(3) . . ? C5 Fe1 C2 68.4(2) . . ? C1 Fe1 C2 41.3(2) . . ? C7 Fe1 C2 129.1(3) . . ? C8 Fe1 C2 166.8(3) . . ? C10 Fe1 C2 120.5(3) . . ? C5 Fe1 C6 162.1(3) . . ? C1 Fe1 C6 125.4(3) . . ? C7 Fe1 C6 41.2(2) . . ? C8 Fe1 C6 68.7(2) . . ? C10 Fe1 C6 41.0(2) . . ? C2 Fe1 C6 109.4(2) . . ? C5 Fe1 C9 104.7(3) . . ? C1 Fe1 C9 116.2(3) . . ? C7 Fe1 C9 68.3(3) . . ? C8 Fe1 C9 39.7(3) . . ? C10 Fe1 C9 40.1(3) . . ? C2 Fe1 C9 152.9(3) . . ? C6 Fe1 C9 68.8(3) . . ? C5 Fe1 C4 40.8(2) . . ? C1 Fe1 C4 68.8(3) . . ? C7 Fe1 C4 121.4(3) . . ? C8 Fe1 C4 108.8(3) . . ? C10 Fe1 C4 161.5(3) . . ? C2 Fe1 C4 67.4(2) . . ? C6 Fe1 C4 156.3(3) . . ? C9 Fe1 C4 125.3(3) . . ? C5 Fe1 C3 68.5(3) . . ? C1 Fe1 C3 69.1(3) . . ? C7 Fe1 C3 110.8(3) . . ? C8 Fe1 C3 129.0(3) . . ? C10 Fe1 C3 155.9(3) . . ? C2 Fe1 C3 40.1(3) . . ? C6 Fe1 C3 122.1(3) . . ? C9 Fe1 C3 163.7(3) . . ? C4 Fe1 C3 40.1(3) . . ? O1 B1 O2 112.6(6) . . ? O1 B1 C1 124.7(6) . . ? O2 B1 C1 122.7(6) . . ? O4 B2 O3 113.6(6) . . ? O4 B2 C6 122.5(6) . 4_655 ? O3 B2 C6 123.9(6) . 4_655 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.546 _refine_diff_density_min -0.476 _refine_diff_density_rms 0.109 # Attachment '5_revised.cif' data_2006src0670 _database_code_depnum_ccdc_archive 'CCDC 645162' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H30 B2 Fe2 O4' _chemical_formula_weight 563.84 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' B B 0.0013 0.0007 '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' 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 Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 29.8942(10) _cell_length_b 10.7482(3) _cell_length_c 7.4301(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2387.36(14) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4930 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 1.251 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8444 _exptl_absorpt_correction_T_max 0.9754 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius APEX2 Area Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 20380 _diffrn_reflns_av_R_equivalents 0.1209 _diffrn_reflns_av_sigmaI/netI 0.0858 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.33 _diffrn_reflns_theta_max 27.50 _reflns_number_total 2868 _reflns_number_gt 2236 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'DENZO, COLLECT' _computing_data_reduction 'DENZO, COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material ? _refine_special_details ; The molecular structure of 5 lies about a crystallographic mirror plane and contains some disorder in the central region (8 membered ring and both 5-membered BO2C2 rings). These fused rings occupy two distinct orientations in a 50:50 ratio and are generated by a x,1/2-y,z symmetry operation. A number of restraints in the refinement were applied to maintain a sensible geometry and thermal motion for these orientations. These restraints are to approximate isotropic thermal motion (SHELX ISOR), to generate the correct connectivity (SHELX BIND & FREE) and to impose chemically reasonable geometry (SHELX DFIX). ; _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^)+(0.0338P)^2^+5.3915P] 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 2868 _refine_ls_number_parameters 229 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.1277 _refine_ls_wR_factor_gt 0.1183 _refine_ls_goodness_of_fit_ref 1.138 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.006 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 C1 C 0.2894(2) 0.2500 0.7744(6) 0.0282(14) Uani 1 2 d S . . H1 H 0.3144 0.2500 0.6954 0.034 Uiso 1 2 calc SR . . C2 C 0.26743(14) 0.1430(4) 0.8439(5) 0.0280(10) Uani 1 1 d . . . H2 H 0.2751 0.0589 0.8201 0.034 Uiso 1 1 calc R . . C3 C 0.23205(13) 0.1845(4) 0.9548(5) 0.0305(10) Uani 1 1 d . . . H3 H 0.2117 0.1328 1.0185 0.037 Uiso 1 1 calc R . . C4 C 0.35787(18) 0.2500 1.1228(6) 0.0213(12) Uani 1 2 d S . . C5 C 0.33545(14) 0.1432(4) 1.1943(4) 0.0232(9) Uani 1 1 d . . . H5 H 0.3430 0.0589 1.1705 0.028 Uiso 1 1 calc R . . C6 C 0.30017(14) 0.1848(4) 1.3065(4) 0.0278(10) Uani 1 1 d . . . H6 H 0.2800 0.1330 1.3708 0.033 Uiso 1 1 calc R . . C13 C 0.55214(16) 0.2500 -0.0129(6) 0.0186(11) Uani 1 2 d S . . C14 C 0.56945(13) 0.1433(4) -0.1052(5) 0.0211(9) Uani 1 1 d . . . H14 H 0.5639 0.0590 -0.0735 0.025 Uiso 1 1 calc R . . C15 C 0.59631(12) 0.1839(4) -0.2520(4) 0.0205(8) Uani 1 1 d . . . H15 H 0.6115 0.1319 -0.3352 0.025 Uiso 1 1 calc R . . C16 C 0.63878(19) 0.2500 0.2514(7) 0.0334(16) Uani 1 2 d S . . H16 H 0.6191 0.2500 0.3518 0.040 Uiso 1 2 calc SR . . C17 C 0.65616(14) 0.1436(5) 0.1626(5) 0.0323(11) Uani 1 1 d . . . H17 H 0.6499 0.0595 0.1929 0.039 Uiso 1 1 calc R . . C18 C 0.68423(13) 0.1839(4) 0.0218(5) 0.0309(10) Uani 1 1 d . . . H18 H 0.7003 0.1319 -0.0588 0.037 Uiso 1 1 calc R . . Fe1 Fe 0.29190(3) 0.2500 1.04955(9) 0.0189(2) Uani 1 2 d S . . Fe2 Fe 0.62057(2) 0.2500 -0.01257(9) 0.0174(2) Uani 1 2 d S . . B1 B 0.3936(2) 0.2500 0.9728(7) 0.0276(16) Uani 1 2 d S . . B2 B 0.5270(2) 0.2500 0.1695(8) 0.0193(13) Uani 1 2 d S . . O1 O 0.42280(19) 0.1713(5) 0.9333(6) 0.0207(12) Uani 0.50 1 d P . 1 C8 C 0.4441(3) 0.2016(8) 0.7646(10) 0.0146(18) Uani 0.50 1 d P . 1 H8 H 0.4771 0.1888 0.7750 0.018 Uiso 0.50 1 calc PR . 1 C9 C 0.4247(3) 0.1105(7) 0.6273(10) 0.0139(16) Uani 0.50 1 d P . 1 H9A H 0.3918 0.1219 0.6261 0.017 Uiso 0.50 1 calc PR . 1 H9B H 0.4306 0.0252 0.6718 0.017 Uiso 0.50 1 calc PR . 1 C10 C 0.4413(3) 0.1174(8) 0.4302(10) 0.0155(19) Uani 0.50 1 d PU . 1 H10A H 0.4391 0.0334 0.3763 0.019 Uiso 0.50 1 calc PR . 1 H10B H 0.4210 0.1729 0.3618 0.019 Uiso 0.50 1 calc PR . 1 C11 C 0.4890(3) 0.1643(9) 0.4080(11) 0.015(2) Uani 0.50 1 d PU . 1 H11 H 0.5092 0.1174 0.4912 0.018 Uiso 0.50 1 calc PR . 1 O2 O 0.50305(19) 0.1428(5) 0.2223(6) 0.0198(12) Uani 0.50 1 d P . 1 O1' O 0.39722(18) 0.1337(5) 0.8623(6) 0.0185(11) Uani 0.50 1 d P . 2 C8' C 0.4340(3) 0.1589(9) 0.7354(12) 0.015(2) Uani 0.50 1 d PU . 2 H8' H 0.4607 0.1092 0.7722 0.018 Uiso 0.50 1 calc PR . 2 C9' C 0.4189(3) 0.1161(8) 0.5517(11) 0.0147(19) Uani 0.50 1 d PU . 2 H9'1 H 0.3954 0.1733 0.5079 0.018 Uiso 0.50 1 calc PR . 2 H9'2 H 0.4054 0.0324 0.5633 0.018 Uiso 0.50 1 calc PR . 2 C10' C 0.4563(3) 0.1102(8) 0.4107(10) 0.0143(18) Uani 0.50 1 d PU . 2 H10C H 0.4674 0.0233 0.4063 0.017 Uiso 0.50 1 calc PR . 2 H10D H 0.4429 0.1286 0.2919 0.017 Uiso 0.50 1 calc PR . 2 C11' C 0.4965(3) 0.1944(8) 0.4338(11) 0.014(2) Uani 0.50 1 d PU . 2 H11' H 0.5105 0.1790 0.5540 0.017 Uiso 0.50 1 calc PR . 2 O2' O 0.52780(19) 0.1604(5) 0.2927(6) 0.0179(11) Uani 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(3) 0.052(4) 0.009(2) 0.000 -0.003(2) 0.000 C2 0.024(2) 0.037(3) 0.0231(19) -0.0096(17) -0.0115(16) 0.005(2) C3 0.014(2) 0.052(3) 0.0255(19) 0.0025(18) -0.0066(15) -0.0093(19) C4 0.015(3) 0.036(4) 0.013(2) 0.000 -0.0051(19) 0.000 C5 0.026(2) 0.027(2) 0.0169(16) 0.0026(15) -0.0035(15) 0.0031(19) C6 0.025(2) 0.044(2) 0.0142(16) 0.0059(16) -0.0024(15) -0.005(2) C13 0.010(3) 0.028(3) 0.018(2) 0.000 -0.0041(19) 0.000 C14 0.020(2) 0.022(2) 0.0214(17) -0.0027(15) -0.0012(15) -0.0038(17) C15 0.022(2) 0.027(2) 0.0132(15) -0.0039(15) 0.0000(14) -0.0008(17) C16 0.016(3) 0.072(5) 0.012(2) 0.000 0.000(2) 0.000 C17 0.022(2) 0.050(3) 0.0254(19) 0.0152(19) -0.0056(16) 0.006(2) C18 0.018(2) 0.051(3) 0.0240(19) -0.0018(18) -0.0018(16) 0.009(2) Fe1 0.0148(4) 0.0302(5) 0.0115(3) 0.000 -0.0003(3) 0.000 Fe2 0.0128(4) 0.0275(5) 0.0118(3) 0.000 0.0000(3) 0.000 B1 0.018(3) 0.055(5) 0.009(2) 0.000 -0.004(2) 0.000 B2 0.008(3) 0.024(4) 0.026(3) 0.000 -0.003(2) 0.000 O1 0.024(3) 0.026(3) 0.012(2) 0.008(2) 0.001(2) 0.004(3) C8 0.014(4) 0.019(5) 0.011(3) 0.003(3) -0.001(3) 0.005(3) C9 0.013(4) 0.017(4) 0.011(4) 0.003(3) 0.000(3) -0.004(3) C10 0.015(2) 0.015(2) 0.016(2) -0.0002(10) -0.0004(10) -0.0001(10) C11 0.015(2) 0.014(2) 0.015(2) -0.0002(10) -0.0006(10) 0.0005(10) O2 0.022(3) 0.022(3) 0.015(2) -0.005(2) 0.004(2) -0.002(3) O1' 0.018(3) 0.019(3) 0.018(2) 0.000(2) 0.009(2) -0.002(2) C8' 0.015(2) 0.015(2) 0.015(2) 0.0000(10) -0.0005(10) 0.0003(10) C9' 0.015(2) 0.014(2) 0.015(2) 0.0003(10) -0.0001(10) -0.0008(10) C10' 0.015(2) 0.014(2) 0.014(2) -0.0001(10) 0.0005(10) 0.0002(10) C11' 0.014(2) 0.015(2) 0.015(2) 0.0000(10) 0.0004(10) 0.0002(10) O2' 0.016(3) 0.021(3) 0.017(2) 0.002(2) 0.006(2) 0.005(3) _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 C1 C2 1.421(5) . ? C1 C2 1.421(5) 7_565 ? C1 Fe1 2.046(5) . ? C2 C3 1.413(5) . ? C2 Fe1 2.048(4) . ? C3 C3 1.408(9) 7_565 ? C3 Fe1 2.048(4) . ? C4 C5 1.431(5) . ? C4 C5 1.431(5) 7_565 ? C4 B1 1.543(8) . ? C4 Fe1 2.046(5) . ? C5 C6 1.417(5) . ? C5 Fe1 2.042(4) . ? C6 C6 1.402(9) 7_565 ? C6 Fe1 2.049(3) . ? C13 C14 1.433(5) . ? C13 C14 1.433(5) 7_565 ? C13 B2 1.551(8) . ? C13 Fe2 2.046(5) . ? C14 C15 1.423(5) . ? C14 Fe2 2.031(4) . ? C15 C15 1.421(8) 7_565 ? C15 Fe2 2.048(3) . ? C16 C17 1.419(6) 7_565 ? C16 C17 1.419(6) . ? C16 Fe2 2.035(5) . ? C17 C18 1.409(5) . ? C17 Fe2 2.033(4) . ? C18 C18 1.421(9) 7_565 ? C18 Fe2 2.047(4) . ? Fe1 C5 2.042(4) 7_565 ? Fe1 C2 2.048(4) 7_565 ? Fe1 C6 2.049(3) 7_565 ? Fe1 C3 2.048(4) 7_565 ? Fe2 C14 2.031(4) 7_565 ? Fe2 C17 2.033(4) 7_565 ? Fe2 C18 2.047(4) 7_565 ? Fe2 C15 2.048(3) 7_565 ? B1 O1 1.251(7) 7_565 ? B1 O1 1.251(7) . ? B1 O1' 1.500(6) . ? B1 O1' 1.500(6) 7_565 ? B2 O2' 1.329(6) 7_565 ? B2 O2' 1.329(6) . ? B2 O2 1.411(6) . ? B2 O2 1.411(6) 7_565 ? O1 C8 1.443(9) . ? C8 C8' 1.546(13) 7_565 ? C8 C9 1.528(11) . ? C9 C10 1.548(10) . ? C10 C11 1.522(12) . ? C11 O2 1.460(9) . ? C11 C11' 1.547(12) 7_565 ? O1' C8' 1.473(10) . ? C8' C9' 1.509(11) . ? C8' C8 1.546(13) 7_565 ? C9' C10' 1.534(10) . ? C10' C11' 1.513(12) . ? C11' O2' 1.452(9) . ? C11' C11 1.547(12) 7_565 ? 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 C2 C1 C2 108.0(5) . 7_565 ? C2 C1 Fe1 69.8(2) . . ? C2 C1 Fe1 69.8(2) 7_565 . ? C3 C2 C1 107.6(4) . . ? C3 C2 Fe1 69.8(2) . . ? C1 C2 Fe1 69.6(2) . . ? C3 C3 C2 108.4(3) 7_565 . ? C3 C3 Fe1 69.89(12) 7_565 . ? C2 C3 Fe1 69.8(2) . . ? C5 C4 C5 106.6(5) . 7_565 ? C5 C4 B1 126.3(2) . . ? C5 C4 B1 126.3(2) 7_565 . ? C5 C4 Fe1 69.4(3) . . ? C5 C4 Fe1 69.4(3) 7_565 . ? B1 C4 Fe1 118.4(3) . . ? C6 C5 C4 108.3(4) . . ? C6 C5 Fe1 70.0(2) . . ? C4 C5 Fe1 69.6(3) . . ? C6 C6 C5 108.4(2) 7_565 . ? C6 C6 Fe1 69.99(12) 7_565 . ? C5 C6 Fe1 69.5(2) . . ? C14 C13 C14 106.4(4) . 7_565 ? C14 C13 B2 126.4(2) . . ? C14 C13 B2 126.4(2) 7_565 . ? C14 C13 Fe2 68.9(2) . . ? C14 C13 Fe2 68.9(2) 7_565 . ? B2 C13 Fe2 119.0(3) . . ? C15 C14 C13 108.9(3) . . ? C15 C14 Fe2 70.2(2) . . ? C13 C14 Fe2 70.0(2) . . ? C14 C15 C15 107.9(2) . 7_565 ? C14 C15 Fe2 68.9(2) . . ? C15 C15 Fe2 69.71(11) 7_565 . ? C17 C16 C17 107.4(5) 7_565 . ? C17 C16 Fe2 69.5(2) 7_565 . ? C17 C16 Fe2 69.5(2) . . ? C18 C17 C16 108.4(4) . . ? C18 C17 Fe2 70.3(2) . . ? C16 C17 Fe2 69.7(3) . . ? C17 C18 C18 107.9(3) . 7_565 ? C17 C18 Fe2 69.3(2) . . ? C18 C18 Fe2 69.70(13) 7_565 . ? C5 Fe1 C5 68.4(2) 7_565 . ? C5 Fe1 C1 123.35(16) 7_565 . ? C5 Fe1 C1 123.35(16) . . ? C5 Fe1 C4 40.99(13) 7_565 . ? C5 Fe1 C4 40.99(13) . . ? C1 Fe1 C4 107.5(2) . . ? C5 Fe1 C2 159.48(16) 7_565 . ? C5 Fe1 C2 107.77(16) . . ? C1 Fe1 C2 40.63(14) . . ? C4 Fe1 C2 122.88(16) . . ? C5 Fe1 C2 107.77(16) 7_565 7_565 ? C5 Fe1 C2 159.48(16) . 7_565 ? C1 Fe1 C2 40.63(14) . 7_565 ? C4 Fe1 C2 122.88(16) . 7_565 ? C2 Fe1 C2 68.3(2) . 7_565 ? C5 Fe1 C6 40.53(15) 7_565 7_565 ? C5 Fe1 C6 67.96(16) . 7_565 ? C1 Fe1 C6 159.33(13) . 7_565 ? C4 Fe1 C6 68.65(17) . 7_565 ? C2 Fe1 C6 158.55(17) . 7_565 ? C2 Fe1 C6 123.12(17) 7_565 7_565 ? C5 Fe1 C6 67.96(16) 7_565 . ? C5 Fe1 C6 40.53(15) . . ? C1 Fe1 C6 159.33(13) . . ? C4 Fe1 C6 68.65(17) . . ? C2 Fe1 C6 123.12(17) . . ? C2 Fe1 C6 158.55(17) 7_565 . ? C6 Fe1 C6 40.0(2) 7_565 . ? C5 Fe1 C3 158.68(17) 7_565 . ? C5 Fe1 C3 123.03(17) . . ? C1 Fe1 C3 67.93(19) . . ? C4 Fe1 C3 159.04(13) . . ? C2 Fe1 C3 40.37(16) . . ? C2 Fe1 C3 67.93(17) 7_565 . ? C6 Fe1 C3 122.92(16) 7_565 . ? C6 Fe1 C3 107.95(16) . . ? C5 Fe1 C3 123.03(17) 7_565 7_565 ? C5 Fe1 C3 158.68(17) . 7_565 ? C1 Fe1 C3 67.93(19) . 7_565 ? C4 Fe1 C3 159.04(13) . 7_565 ? C2 Fe1 C3 67.93(17) . 7_565 ? C2 Fe1 C3 40.37(16) 7_565 7_565 ? C6 Fe1 C3 107.95(16) 7_565 7_565 ? C6 Fe1 C3 122.92(16) . 7_565 ? C3 Fe1 C3 40.2(3) . 7_565 ? C14 Fe2 C14 68.8(2) . 7_565 ? C14 Fe2 C17 158.17(16) . 7_565 ? C14 Fe2 C17 107.04(18) 7_565 7_565 ? C14 Fe2 C17 107.04(18) . . ? C14 Fe2 C17 158.17(16) 7_565 . ? C17 Fe2 C17 68.4(3) 7_565 . ? C14 Fe2 C16 121.84(16) . . ? C14 Fe2 C16 121.84(16) 7_565 . ? C17 Fe2 C16 40.81(15) 7_565 . ? C17 Fe2 C16 40.81(15) . . ? C14 Fe2 C13 41.16(13) . . ? C14 Fe2 C13 41.16(13) 7_565 . ? C17 Fe2 C13 121.61(16) 7_565 . ? C17 Fe2 C13 121.61(16) . . ? C16 Fe2 C13 105.6(2) . . ? C14 Fe2 C18 159.67(16) . 7_565 ? C14 Fe2 C18 123.08(17) 7_565 7_565 ? C17 Fe2 C18 40.40(16) 7_565 7_565 ? C17 Fe2 C18 68.21(18) . 7_565 ? C16 Fe2 C18 68.36(18) . 7_565 ? C13 Fe2 C18 158.38(14) . 7_565 ? C14 Fe2 C18 123.08(17) . . ? C14 Fe2 C18 159.67(16) 7_565 . ? C17 Fe2 C18 68.21(18) 7_565 . ? C17 Fe2 C18 40.40(16) . . ? C16 Fe2 C18 68.36(18) . . ? C13 Fe2 C18 158.38(14) . . ? C18 Fe2 C18 40.6(3) 7_565 . ? C14 Fe2 C15 40.84(14) . . ? C14 Fe2 C15 68.61(15) 7_565 . ? C17 Fe2 C15 159.46(17) 7_565 . ? C17 Fe2 C15 123.11(17) . . ? C16 Fe2 C15 158.68(12) . . ? C13 Fe2 C15 69.20(16) . . ? C18 Fe2 C15 123.91(15) 7_565 . ? C18 Fe2 C15 108.50(15) . . ? C14 Fe2 C15 68.61(15) . 7_565 ? C14 Fe2 C15 40.84(14) 7_565 7_565 ? C17 Fe2 C15 123.11(17) 7_565 7_565 ? C17 Fe2 C15 159.46(17) . 7_565 ? C16 Fe2 C15 158.68(12) . 7_565 ? C13 Fe2 C15 69.20(16) . 7_565 ? C18 Fe2 C15 108.50(15) 7_565 7_565 ? C18 Fe2 C15 123.91(15) . 7_565 ? C15 Fe2 C15 40.6(2) . 7_565 ? O1 B1 O1 85.1(7) 7_565 . ? O1 B1 O1' 112.6(5) 7_565 . ? O1 B1 O1' 42.0(3) . . ? O1 B1 O1' 42.0(3) 7_565 7_565 ? O1 B1 O1' 112.6(5) . 7_565 ? O1' B1 O1' 112.9(5) . 7_565 ? O1 B1 C4 130.7(3) 7_565 . ? O1 B1 C4 130.7(3) . . ? O1' B1 C4 116.5(3) . . ? O1' B1 C4 116.5(3) 7_565 . ? O2' B2 O2' 92.9(6) 7_565 . ? O2' B2 O2 114.2(5) 7_565 . ? O2' B2 O2 39.3(3) . . ? O2' B2 O2 39.3(3) 7_565 7_565 ? O2' B2 O2 114.2(5) . 7_565 ? O2 B2 O2 109.4(6) . 7_565 ? O2' B2 C13 126.4(4) 7_565 . ? O2' B2 C13 126.4(4) . . ? O2 B2 C13 119.3(3) . . ? O2 B2 C13 119.3(3) 7_565 . ? B1 O1 C8 111.1(5) . . ? O1 C8 C8' 104.8(7) . 7_565 ? O1 C8 C9 105.6(7) . . ? C8' C8 C9 117.0(7) 7_565 . ? C8 C9 C10 118.6(6) . . ? C11 C10 C9 114.8(6) . . ? O2 C11 C11' 103.3(8) . 7_565 ? O2 C11 C10 108.6(7) . . ? C11' C11 C10 116.5(8) 7_565 . ? B2 O2 C11 106.2(6) . . ? C8' O1' B1 104.6(5) . . ? O1' C8' C9' 107.5(7) . . ? O1' C8' C8 103.5(8) . 7_565 ? C9' C8' C8 118.8(8) . 7_565 ? C8' C9' C10' 114.4(7) . . ? C11' C10' C9' 118.4(7) . . ? O2' C11' C10' 106.2(7) . . ? O2' C11' C11 104.5(7) . 7_565 ? C10' C11' C11 117.3(8) . 7_565 ? B2 O2' C11' 107.6(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.573 _refine_diff_density_min -0.624 _refine_diff_density_rms 0.109