# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Simon Aldridge' _publ_contact_author_email SIMON.ALDRIDGE@CHEM.OX.AC.UK _publ_section_title ; Facile Syntheses of Dissymmetric Ferrocene-Functionalized Lewis Acids and Acid/Base Pairs ; loop_ _publ_author_name 'Simon Aldridge' 'A.Di Paolo' 'Ian Fallis' 'Ian R. Morgan' 'Dragoslav Vidovic' # Attachment 'Combined_cif.txt' #============================================================================== data_2 _database_code_depnum_ccdc_archive 'CCDC 742657' #============================================================================== _audit_creation_date 09-07-27 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 055imdv08 _chemical_name_systematic . _chemical_melting_point 'not measured' _refine_special_details ; The data for this structure are particularly poor for reasons that are not clear. Although strong, the reflections are noisy. The data have been examined by ROTAX (R. I. Cooper, R. O. Gould, S. Parsons & D. J. Watkin, J. Appl. Cryst. (2002), 35, 168-174.) and TWINROTMAT within PLATON (PLATON, A Multipurpose Crystallographic Tool, A. L. Spek. Utrecht, the Netherlands, 1998.; A. Spek, J. Appl. Cryst. (2003), 36, 7-13.) with no success. Results are included here for completeness only, and despite the issues outlined above it seems unlikely that the connectivity is incorrect. ; _cell_length_a 11.6882(2) _cell_length_b 13.3858(2) _cell_length_c 17.8620(3) _cell_angle_alpha 70.2595(7) _cell_angle_beta 75.9181(7) _cell_angle_gamma 67.4647(8) _cell_volume 2408.61(7) _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328 2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C0.50 B29.50 Br1 Fe1 # Dc = 1.27 Fooo = 1056.00 Mu = 22.74 M = 921.36 # Found Formula = C28 H30 B1 Br1 Fe1 # Dc = 1.41 FOOO = 1056.00 Mu = 22.98 M = 1026.22 _chemical_formula_sum 'C28 H30 B1 Br1 Fe1' _chemical_formula_moiety 'C28 H30 B1 Br1 Fe1' _chemical_compound_source . _chemical_formula_weight 513.11 _cell_measurement_reflns_used 10034 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_max 0.32 _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1056 _exptl_absorpt_coefficient_mu 2.298 # Sheldrick geometric approximatio 0.62 0.91 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.73 _exptl_absorpt_correction_T_max 0.91 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _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 'SHELXS 86 (Sheldrick, 1986)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 36161 _reflns_number_total 10994 _diffrn_reflns_av_R_equivalents 0.066 # Number of reflections with Friedels Law is 10994 # Number of reflections without Friedels Law is 19594 # Theoretical number of reflections is about 11165 _diffrn_reflns_theta_min 5.151 _diffrn_reflns_theta_max 27.588 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.761 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min -14 _reflns_limit_h_max 15 _reflns_limit_k_min -16 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.36 _oxford_diffrn_Wilson_scale 8.07 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.81 _refine_diff_density_max 5.39 # 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 10994 _refine_ls_number_restraints 0 _refine_ls_number_parameters 560 _oxford_refine_ls_R_factor_ref 0.1285 _refine_ls_wR_factor_ref 0.2555 _refine_ls_goodness_of_fit_ref 1.5016 _refine_ls_shift/su_max 0.000362 # The values computed from all data _oxford_reflns_number_all 10994 _refine_ls_R_factor_all 0.1285 _refine_ls_wR_factor_all 0.2555 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 9258 _refine_ls_R_factor_gt 0.1175 _refine_ls_wR_factor_gt 0.2498 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr # none, undef, noref, refall, # refxyz, refU, constr or mixed # WARNING. The IUCr will not accept Unit Weights _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method= Quasi-Unit weights W = 1.0 or 1./2F ; # Insert your own references if required - in alphabetical order _publ_section_references ; Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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. Sheldrick, G. M. (2008). Acta Cryst A64, 112-122. 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 Br1 Br 0.57301(9) 0.48073(8) 0.34576(6) 0.0343 1.0000 Uani . . . . . . . C2 C 0.4228(8) 0.5997(7) 0.3548(5) 0.0266 1.0000 Uani . . . . . . . Fe3 Fe 0.24573(12) 0.59448(11) 0.37889(8) 0.0294 1.0000 Uani . . . . . . . C4 C 0.3550(8) 0.6828(7) 0.2905(5) 0.0239 1.0000 Uani . . . . . . . C5 C 0.2482(8) 0.7552(7) 0.3313(6) 0.0283 1.0000 Uani . . . . . . . C6 C 0.2555(8) 0.7209(8) 0.4130(6) 0.0306 1.0000 Uani . . . . . . . C7 C 0.3636(8) 0.6231(8) 0.4298(6) 0.0298 1.0000 Uani . . . . . . . B8 B 0.3902(9) 0.7121(8) 0.1968(6) 0.0264 1.0000 Uani . . . . . . . C9 C 0.5088(8) 0.6385(7) 0.1503(5) 0.0276 1.0000 Uani . . . . . . . C10 C 0.5257(9) 0.5278(8) 0.1519(6) 0.0334 1.0000 Uani . . . . . . . C11 C 0.4278(10) 0.4726(9) 0.1940(7) 0.0407 1.0000 Uani . . . . . . . C12 C 0.6333(10) 0.4670(8) 0.1111(6) 0.0365 1.0000 Uani . . . . . . . C13 C 0.7269(9) 0.5094(9) 0.0694(6) 0.0395 1.0000 Uani . . . . . . . C14 C 0.7085(9) 0.6179(8) 0.0679(7) 0.0382 1.0000 Uani . . . . . . . C15 C 0.6034(9) 0.6845(8) 0.1040(6) 0.0329 1.0000 Uani . . . . . . . C16 C 0.5981(10) 0.8018(9) 0.0964(8) 0.0480 1.0000 Uani . . . . . . . C17 C 0.8479(11) 0.4379(10) 0.0313(8) 0.0533 1.0000 Uani . . . . . . . C18 C 0.3061(8) 0.8316(7) 0.1487(5) 0.0264 1.0000 Uani . . . . . . . C19 C 0.2423(8) 0.8364(7) 0.0896(5) 0.0261 1.0000 Uani . . . . . . . C20 C 0.1674(7) 0.9426(7) 0.0510(7) 0.0340 1.0000 Uani . . . . . . . C21 C 0.1601(8) 1.0415(8) 0.0571(6) 0.0320 1.0000 Uani . . . . . . . C22 C 0.0798(10) 1.1522(9) 0.0107(7) 0.0448 1.0000 Uani . . . . . . . C23 C 0.2241(9) 1.0367(8) 0.1165(6) 0.0328 1.0000 Uani . . . . . . . C24 C 0.2958(8) 0.9327(7) 0.1615(6) 0.0294 1.0000 Uani . . . . . . . C25 C 0.3642(9) 0.9387(8) 0.2203(6) 0.0367 1.0000 Uani . . . . . . . C26 C 0.2460(9) 0.7315(8) 0.0734(6) 0.0357 1.0000 Uani . . . . . . . C27 C 0.2444(11) 0.4393(9) 0.3834(8) 0.0501 1.0000 Uani . . . . . . . C28 C 0.1580(10) 0.5231(10) 0.3343(8) 0.0461 1.0000 Uani . . . . . . . C29 C 0.0688(10) 0.5942(10) 0.3814(8) 0.0471 1.0000 Uani . . . . . . . C30 C 0.2115(12) 0.4550(10) 0.4637(8) 0.0551 1.0000 Uani . . . . . . . Br31 Br 0.08837(9) 0.13599(8) 0.57038(6) 0.0359 1.0000 Uani . . . . . . . C32 C 0.2006(8) -0.0116(7) 0.5838(5) 0.0250 1.0000 Uani . . . . . . . Fe33 Fe 0.17199(11) -0.15846(10) 0.64996(8) 0.0264 1.0000 Uani . . . . . . . C34 C 0.2920(7) -0.0736(7) 0.6392(5) 0.0246 1.0000 Uani . . . . . . . C35 C 0.3574(8) -0.1786(8) 0.6218(5) 0.0286 1.0000 Uani . . . . . . . C36 C 0.3133(8) -0.1810(7) 0.5564(5) 0.0282 1.0000 Uani . . . . . . . C37 C 0.2126(8) -0.0779(7) 0.5324(5) 0.0283 1.0000 Uani . . . . . . . B38 B 0.3403(9) -0.0292(8) 0.6945(6) 0.0239 1.0000 Uani . . . . . . . C39 C 0.2747(8) 0.0923(8) 0.7106(5) 0.0281 1.0000 Uani . . . . . . . C40 C 0.3353(9) 0.1725(8) 0.6795(6) 0.0318 1.0000 Uani . . . . . . . C41 C 0.2826(10) 0.2761(8) 0.6998(6) 0.0372 1.0000 Uani . . . . . . . C42 C 0.1738(10) 0.3012(9) 0.7497(7) 0.0420 1.0000 Uani . . . . . . . C43 C 0.1104(9) 0.2232(8) 0.7785(6) 0.0365 1.0000 Uani . . . . . . . C44 C 0.1582(9) 0.1204(8) 0.7595(6) 0.0335 1.0000 Uani . . . . . . . C45 C 0.0805(9) 0.0436(9) 0.7927(7) 0.0391 1.0000 Uani . . . . . . . C46 C 0.1214(12) 0.4116(10) 0.7715(9) 0.0569 1.0000 Uani . . . . . . . C47 C 0.4545(9) 0.1548(9) 0.6204(6) 0.0363 1.0000 Uani . . . . . . . C48 C 0.4679(8) -0.1082(7) 0.7279(5) 0.0246 1.0000 Uani . . . . . . . C49 C 0.5818(8) -0.1448(7) 0.6769(5) 0.0255 1.0000 Uani . . . . . . . C50 C 0.5924(9) -0.1041(8) 0.5864(5) 0.0319 1.0000 Uani . . . . . . . C51 C 0.6919(8) -0.2141(7) 0.7098(5) 0.0278 1.0000 Uani . . . . . . . C52 C 0.6959(8) -0.2547(7) 0.7919(6) 0.0302 1.0000 Uani . . . . . . . C53 C 0.8148(9) -0.3331(9) 0.8246(7) 0.0389 1.0000 Uani . . . . . . . C54 C 0.5864(9) -0.2220(8) 0.8422(5) 0.0304 1.0000 Uani . . . . . . . C55 C 0.4744(9) -0.1490(7) 0.8119(5) 0.0285 1.0000 Uani . . . . . . . C56 C 0.3602(10) -0.1172(10) 0.8720(6) 0.0436 1.0000 Uani . . . . . . . C57 C 0.1491(9) -0.2995(8) 0.7374(6) 0.0352 1.0000 Uani . . . . . . . C58 C 0.0844(9) -0.2037(8) 0.7651(6) 0.0371 1.0000 Uani . . . . . . . C59 C -0.0040(10) -0.1272(9) 0.7126(7) 0.0440 1.0000 Uani . . . . . . . C60 C 0.0048(10) -0.1755(10) 0.6526(7) 0.0455 1.0000 Uani . . . . . . . C61 C 0.1000(10) -0.2842(9) 0.6674(7) 0.0412 1.0000 Uani . . . . . . . C1 C 0.1017(11) 0.5539(10) 0.4589(7) 0.0485 1.0000 Uani . . . . . . . H51 H 0.1804 0.8192 0.3044 0.0339 1.0000 Uiso R . . . . . . H61 H 0.1940 0.7570 0.4534 0.0382 1.0000 Uiso R . . . . . . H71 H 0.3924 0.5794 0.4828 0.0351 1.0000 Uiso R . . . . . . H111 H 0.4655 0.3918 0.2056 0.0641 1.0000 Uiso R . . . . . . H112 H 0.3894 0.4921 0.2437 0.0641 1.0000 Uiso R . . . . . . H113 H 0.3639 0.4960 0.1604 0.0641 1.0000 Uiso R . . . . . . H121 H 0.6409 0.3938 0.1121 0.0400 1.0000 Uiso R . . . . . . H141 H 0.7725 0.6486 0.0408 0.0472 1.0000 Uiso R . . . . . . H161 H 0.6696 0.8170 0.0593 0.0731 1.0000 Uiso R . . . . . . H163 H 0.5986 0.8097 0.1470 0.0731 1.0000 Uiso R . . . . . . H162 H 0.5226 0.8556 0.0746 0.0729 1.0000 Uiso R . . . . . . H171 H 0.8843 0.4842 -0.0153 0.0679 1.0000 Uiso R . . . . . . H173 H 0.9086 0.3975 0.0690 0.0681 1.0000 Uiso R . . . . . . H172 H 0.8325 0.3827 0.0146 0.0680 1.0000 Uiso R . . . . . . H201 H 0.1170 0.9444 0.0168 0.0351 1.0000 Uiso R . . . . . . H221 H 0.1202 1.2087 -0.0021 0.0622 1.0000 Uiso R . . . . . . H222 H 0.0683 1.1461 -0.0384 0.0620 1.0000 Uiso R . . . . . . H223 H -0.0001 1.1777 0.0409 0.0621 1.0000 Uiso R . . . . . . H231 H 0.2161 1.1037 0.1269 0.0356 1.0000 Uiso R . . . . . . H251 H 0.3067 0.9783 0.2574 0.0581 1.0000 Uiso R . . . . . . H253 H 0.4236 0.9767 0.1917 0.0580 1.0000 Uiso R . . . . . . H252 H 0.4093 0.8633 0.2498 0.0580 1.0000 Uiso R . . . . . . H261 H 0.1824 0.7487 0.0409 0.0580 1.0000 Uiso R . . . . . . H262 H 0.3265 0.6982 0.0452 0.0580 1.0000 Uiso R . . . . . . H263 H 0.2335 0.6761 0.1245 0.0578 1.0000 Uiso R . . . . . . H271 H 0.3188 0.3805 0.3655 0.0611 1.0000 Uiso R . . . . . . H281 H 0.1595 0.5323 0.2765 0.0610 1.0000 Uiso R . . . . . . H291 H -0.0034 0.6618 0.3614 0.0630 1.0000 Uiso R . . . . . . H301 H 0.2536 0.4016 0.5154 0.0648 1.0000 Uiso R . . . . . . H351 H 0.4246 -0.2409 0.6516 0.0350 1.0000 Uiso R . . . . . . H361 H 0.3434 -0.2445 0.5322 0.0321 1.0000 Uiso R . . . . . . H411 H 0.3247 0.3284 0.6788 0.0460 1.0000 Uiso R . . . . . . H431 H 0.0337 0.2396 0.8121 0.0411 1.0000 Uiso R . . . . . . H452 H -0.0057 0.0866 0.8060 0.0570 1.0000 Uiso R . . . . . . H451 H 0.1095 -0.0130 0.8403 0.0570 1.0000 Uiso R . . . . . . H453 H 0.0851 0.0066 0.7540 0.0571 1.0000 Uiso R . . . . . . H463 H 0.0487 0.4122 0.8118 0.0901 1.0000 Uiso R . . . . . . H462 H 0.1833 0.4215 0.7919 0.0899 1.0000 Uiso R . . . . . . H461 H 0.0961 0.4731 0.7243 0.0900 1.0000 Uiso R . . . . . . H471 H 0.4845 0.2172 0.6064 0.0581 1.0000 Uiso R . . . . . . H473 H 0.5179 0.0879 0.6442 0.0579 1.0000 Uiso R . . . . . . H472 H 0.4409 0.1466 0.5719 0.0580 1.0000 Uiso R . . . . . . H501 H 0.6182 -0.1683 0.5654 0.0458 1.0000 Uiso R . . . . . . H502 H 0.6543 -0.0667 0.5654 0.0460 1.0000 Uiso R . . . . . . H503 H 0.5130 -0.0528 0.5699 0.0461 1.0000 Uiso R . . . . . . H511 H 0.7656 -0.2337 0.6746 0.0331 1.0000 Uiso R . . . . . . H531 H 0.7996 -0.3592 0.8824 0.0571 1.0000 Uiso R . . . . . . H532 H 0.8746 -0.2947 0.8116 0.0571 1.0000 Uiso R . . . . . . H533 H 0.8497 -0.3968 0.8035 0.0572 1.0000 Uiso R . . . . . . H541 H 0.5877 -0.2496 0.8982 0.0361 1.0000 Uiso R . . . . . . H561 H 0.3796 -0.1527 0.9259 0.0569 1.0000 Uiso R . . . . . . H563 H 0.3295 -0.0359 0.8635 0.0570 1.0000 Uiso R . . . . . . H562 H 0.2945 -0.1392 0.8644 0.0570 1.0000 Uiso R . . . . . . H571 H 0.2181 -0.3657 0.7622 0.0410 1.0000 Uiso R . . . . . . H581 H 0.1001 -0.1907 0.8124 0.0431 1.0000 Uiso R . . . . . . H591 H -0.0620 -0.0524 0.7179 0.0480 1.0000 Uiso R . . . . . . H601 H -0.0458 -0.1402 0.6074 0.0570 1.0000 Uiso R . . . . . . H11 H 0.0558 0.5879 0.5039 0.0580 1.0000 Uiso R . . . . . . H371 H 0.1578 -0.0588 0.4914 0.0349 1.0000 Uiso R . . . . . . H611 H 0.1306 -0.3357 0.6309 0.0523 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 Br1 0.0298(5) 0.0275(5) 0.0393(5) -0.0083(4) -0.0077(4) -0.0017(4) C2 0.024(4) 0.025(4) 0.029(4) -0.007(3) -0.002(3) -0.006(3) Fe3 0.0271(6) 0.0270(6) 0.0362(7) -0.0102(5) -0.0014(5) -0.0113(5) C4 0.022(4) 0.019(4) 0.032(4) -0.007(3) -0.003(3) -0.008(3) C5 0.025(4) 0.023(4) 0.038(5) -0.009(4) -0.007(4) -0.007(3) C6 0.030(4) 0.029(4) 0.039(5) -0.018(4) 0.001(4) -0.012(4) C7 0.028(4) 0.029(4) 0.033(5) -0.010(4) -0.003(4) -0.010(4) B8 0.022(4) 0.024(4) 0.036(5) -0.008(4) -0.002(4) -0.013(4) C9 0.026(4) 0.027(4) 0.027(4) -0.007(3) -0.004(3) -0.005(3) C10 0.036(5) 0.032(5) 0.033(5) -0.009(4) -0.007(4) -0.010(4) C11 0.043(6) 0.037(5) 0.049(6) -0.018(5) 0.002(5) -0.019(4) C12 0.046(6) 0.022(4) 0.039(5) -0.011(4) -0.008(4) -0.004(4) C13 0.033(5) 0.037(5) 0.042(6) -0.014(4) -0.002(4) -0.002(4) C14 0.028(5) 0.034(5) 0.056(6) -0.022(5) -0.013(4) -0.001(4) C15 0.030(5) 0.029(5) 0.039(5) -0.008(4) -0.004(4) -0.011(4) C16 0.036(5) 0.035(5) 0.074(8) -0.020(5) 0.010(5) -0.018(4) C17 0.048(7) 0.043(6) 0.052(7) -0.016(5) 0.005(5) 0.000(5) C18 0.025(4) 0.025(4) 0.030(4) -0.007(3) -0.004(3) -0.009(3) C19 0.023(4) 0.031(4) 0.025(4) -0.010(3) 0.001(3) -0.010(3) C20 0.009(3) 0.017(4) 0.065(6) 0.005(4) -0.013(4) -0.003(3) C21 0.025(4) 0.029(5) 0.035(5) -0.007(4) 0.000(4) -0.005(4) C22 0.039(6) 0.036(5) 0.048(6) 0.000(5) -0.007(5) -0.009(4) C23 0.033(5) 0.026(4) 0.036(5) -0.001(4) -0.006(4) -0.012(4) C24 0.030(4) 0.023(4) 0.035(5) -0.008(4) -0.004(4) -0.009(3) C25 0.038(5) 0.031(5) 0.046(6) -0.010(4) -0.008(4) -0.015(4) C26 0.037(5) 0.033(5) 0.045(6) -0.013(4) -0.016(4) -0.010(4) C27 0.050(6) 0.030(5) 0.073(8) -0.016(5) 0.002(6) -0.022(5) C28 0.043(6) 0.052(7) 0.061(7) -0.032(6) 0.001(5) -0.025(5) C29 0.030(5) 0.055(7) 0.068(8) -0.027(6) 0.000(5) -0.022(5) C30 0.062(8) 0.044(6) 0.059(7) -0.008(5) 0.012(6) -0.034(6) Br31 0.0353(5) 0.0253(5) 0.0417(6) -0.0077(4) -0.0098(4) -0.0026(4) C32 0.024(4) 0.026(4) 0.026(4) -0.006(3) -0.004(3) -0.010(3) Fe33 0.0245(6) 0.0234(6) 0.0311(7) -0.0054(5) -0.0033(5) -0.0098(5) C34 0.016(3) 0.028(4) 0.021(4) -0.007(3) -0.001(3) 0.002(3) C35 0.026(4) 0.029(4) 0.031(5) -0.009(4) -0.001(3) -0.011(3) C36 0.033(4) 0.024(4) 0.028(4) -0.013(3) 0.001(3) -0.008(3) C37 0.031(4) 0.026(4) 0.030(4) -0.007(3) -0.004(3) -0.012(4) B38 0.024(4) 0.025(4) 0.023(4) -0.007(4) 0.004(3) -0.012(4) C39 0.025(4) 0.031(4) 0.029(4) -0.013(4) -0.002(3) -0.006(3) C40 0.040(5) 0.028(4) 0.034(5) -0.009(4) -0.008(4) -0.015(4) C41 0.044(5) 0.026(5) 0.049(6) -0.016(4) -0.005(4) -0.015(4) C42 0.045(6) 0.034(5) 0.054(6) -0.021(5) -0.016(5) -0.008(4) C43 0.031(5) 0.036(5) 0.038(5) -0.018(4) -0.005(4) 0.001(4) C44 0.033(5) 0.035(5) 0.032(5) -0.014(4) -0.004(4) -0.006(4) C45 0.031(5) 0.038(5) 0.045(6) -0.016(4) 0.012(4) -0.015(4) C46 0.053(7) 0.044(6) 0.088(10) -0.042(7) -0.007(7) -0.011(5) C47 0.041(5) 0.040(5) 0.037(5) -0.011(4) 0.000(4) -0.026(4) C48 0.026(4) 0.023(4) 0.029(4) -0.008(3) -0.002(3) -0.012(3) C49 0.027(4) 0.025(4) 0.025(4) -0.006(3) -0.001(3) -0.011(3) C50 0.029(4) 0.041(5) 0.025(4) -0.005(4) 0.000(3) -0.015(4) C51 0.023(4) 0.028(4) 0.034(5) -0.009(4) 0.000(3) -0.011(3) C52 0.028(4) 0.022(4) 0.040(5) -0.003(4) -0.011(4) -0.008(3) C53 0.032(5) 0.038(5) 0.045(6) -0.008(4) -0.012(4) -0.008(4) C54 0.034(5) 0.033(5) 0.023(4) -0.003(3) -0.006(3) -0.012(4) C55 0.034(5) 0.028(4) 0.024(4) -0.008(3) 0.004(3) -0.014(4) C56 0.041(6) 0.050(6) 0.023(5) -0.007(4) 0.004(4) -0.006(5) C57 0.037(5) 0.026(4) 0.039(5) -0.001(4) -0.003(4) -0.015(4) C58 0.040(5) 0.038(5) 0.032(5) -0.008(4) 0.008(4) -0.020(4) C59 0.032(5) 0.033(5) 0.055(7) -0.005(5) 0.008(5) -0.012(4) C60 0.035(5) 0.049(6) 0.056(7) 0.001(5) -0.014(5) -0.027(5) C61 0.044(6) 0.047(6) 0.041(6) -0.010(5) -0.001(4) -0.028(5) C1 0.045(6) 0.055(7) 0.051(7) -0.018(5) 0.012(5) -0.030(5) _refine_ls_extinction_coef 350(40) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.3554(9) 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 Br1 . C2 . 1.881(8) yes C2 . Fe3 . 2.032(9) yes C2 . C4 . 1.446(12) yes C2 . C7 . 1.426(12) yes Fe3 . C4 . 2.107(8) yes Fe3 . C5 . 2.038(9) yes Fe3 . C6 . 2.031(9) yes Fe3 . C7 . 2.030(9) yes Fe3 . C27 . 2.057(10) yes Fe3 . C28 . 2.064(10) yes Fe3 . C29 . 2.059(10) yes Fe3 . C30 . 2.076(11) yes Fe3 . C1 . 2.044(11) yes C4 . C5 . 1.462(12) yes C4 . B8 . 1.572(13) yes C5 . C6 . 1.389(13) yes C5 . H51 . 0.989 no C6 . C7 . 1.432(12) yes C6 . H61 . 0.994 no C7 . H71 . 0.991 no B8 . C9 . 1.589(13) yes B8 . C18 . 1.593(13) yes C9 . C10 . 1.409(13) yes C9 . C15 . 1.421(12) yes C10 . C11 . 1.508(13) yes C10 . C12 . 1.396(13) yes C11 . H111 . 0.967 no C11 . H112 . 0.965 no C11 . H113 . 0.963 no C12 . C13 . 1.366(15) yes C12 . H121 . 0.943 no C13 . C14 . 1.377(14) yes C13 . C17 . 1.521(14) yes C14 . C15 . 1.372(13) yes C14 . H141 . 0.942 no C15 . C16 . 1.507(13) yes C16 . H161 . 0.974 no C16 . H163 . 0.946 no C16 . H162 . 0.970 no C17 . H171 . 0.969 no C17 . H173 . 0.970 no C17 . H172 . 0.972 no C18 . C19 . 1.407(12) yes C18 . C24 . 1.403(12) yes C19 . C20 . 1.393(11) yes C19 . C26 . 1.508(12) yes C20 . C21 . 1.333(13) yes C20 . H201 . 0.935 no C21 . C22 . 1.498(13) yes C21 . C23 . 1.412(13) yes C22 . H221 . 0.976 no C22 . H222 . 0.953 no C22 . H223 . 0.956 no C23 . C24 . 1.401(12) yes C23 . H231 . 0.943 no C24 . C25 . 1.506(13) yes C25 . H251 . 0.958 no C25 . H253 . 0.961 no C25 . H252 . 0.971 no C26 . H261 . 0.965 no C26 . H262 . 0.969 no C26 . H263 . 0.982 no C27 . C28 . 1.396(17) yes C27 . C30 . 1.457(18) yes C27 . H271 . 0.994 no C28 . C29 . 1.433(15) yes C28 . H281 . 0.995 no C29 . C1 . 1.398(17) yes C29 . H291 . 1.000 no C30 . C1 . 1.443(18) yes C30 . H301 . 1.054 no Br31 . C32 . 1.878(8) yes C32 . Fe33 . 2.029(8) yes C32 . C34 . 1.445(11) yes C32 . C37 . 1.431(12) yes Fe33 . C34 . 2.059(9) yes Fe33 . C35 . 2.033(9) yes Fe33 . C36 . 2.057(9) yes Fe33 . C37 . 2.044(9) yes Fe33 . C57 . 2.065(9) yes Fe33 . C58 . 2.062(9) yes Fe33 . C59 . 2.048(10) yes Fe33 . C60 . 2.040(10) yes Fe33 . C61 . 2.060(10) yes C34 . C35 . 1.419(12) yes C34 . B38 . 1.603(13) yes C35 . C36 . 1.401(12) yes C35 . H351 . 0.999 no C36 . C37 . 1.440(12) yes C36 . H361 . 0.988 no C37 . H371 . 0.993 no B38 . C39 . 1.603(13) yes B38 . C48 . 1.580(12) yes C39 . C40 . 1.396(12) yes C39 . C44 . 1.418(12) yes C40 . C41 . 1.418(12) yes C40 . C47 . 1.520(13) yes C41 . C42 . 1.360(15) yes C41 . H411 . 0.933 no C42 . C43 . 1.396(15) yes C42 . C46 . 1.513(14) yes C43 . C44 . 1.397(13) yes C43 . H431 . 0.943 no C44 . C45 . 1.509(13) yes C45 . H452 . 0.966 no C45 . H451 . 0.960 no C45 . H453 . 0.958 no C46 . H463 . 0.970 no C46 . H462 . 0.954 no C46 . H461 . 0.971 no C47 . H471 . 0.962 no C47 . H473 . 0.958 no C47 . H472 . 0.965 no C48 . C49 . 1.432(11) yes C48 . C55 . 1.423(12) yes C49 . C50 . 1.512(12) yes C49 . C51 . 1.395(12) yes C50 . H501 . 0.968 no C50 . H502 . 0.966 no C50 . H503 . 0.963 no C51 . C52 . 1.387(13) yes C51 . H511 . 0.939 no C52 . C53 . 1.495(12) yes C52 . C54 . 1.384(13) yes C53 . H531 . 0.966 no C53 . H532 . 0.961 no C53 . H533 . 0.955 no C54 . C55 . 1.403(13) yes C54 . H541 . 0.943 no C55 . C56 . 1.513(12) yes C56 . H561 . 0.959 no C56 . H563 . 0.976 no C56 . H562 . 0.972 no C57 . C58 . 1.401(14) yes C57 . C61 . 1.420(14) yes C57 . H571 . 0.997 no C58 . C59 . 1.417(15) yes C58 . H581 . 0.989 no C59 . C60 . 1.394(17) yes C59 . H591 . 0.991 no C60 . C61 . 1.438(16) yes C60 . H601 . 0.993 no C61 . H611 . 1.016 no C1 . H11 . 0.995 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 Br1 . C2 . Fe3 . 127.7(5) yes Br1 . C2 . C4 . 127.2(6) yes Fe3 . C2 . C4 . 72.4(5) yes Br1 . C2 . C7 . 122.3(7) yes Fe3 . C2 . C7 . 69.4(5) yes C4 . C2 . C7 . 110.3(7) yes C2 . Fe3 . C4 . 40.8(3) yes C2 . Fe3 . C5 . 68.5(3) yes C4 . Fe3 . C5 . 41.3(3) yes C2 . Fe3 . C6 . 68.7(4) yes C4 . Fe3 . C6 . 68.8(3) yes C5 . Fe3 . C6 . 39.9(4) yes C2 . Fe3 . C7 . 41.1(3) yes C4 . Fe3 . C7 . 69.4(4) yes C5 . Fe3 . C7 . 68.7(4) yes C6 . Fe3 . C7 . 41.3(4) yes C2 . Fe3 . C27 . 111.2(4) yes C4 . Fe3 . C27 . 124.5(4) yes C5 . Fe3 . C27 . 159.1(5) yes C6 . Fe3 . C27 . 160.9(5) yes C7 . Fe3 . C27 . 125.8(5) yes C2 . Fe3 . C28 . 132.0(4) yes C4 . Fe3 . C28 . 114.1(4) yes C5 . Fe3 . C28 . 124.2(4) yes C6 . Fe3 . C28 . 153.5(4) yes C7 . Fe3 . C28 . 165.0(4) yes C2 . Fe3 . C29 . 169.7(4) yes C4 . Fe3 . C29 . 130.7(4) yes C5 . Fe3 . C29 . 108.8(4) yes C6 . Fe3 . C29 . 116.1(4) yes C7 . Fe3 . C29 . 148.3(4) yes C2 . Fe3 . C30 . 118.1(5) yes C4 . Fe3 . C30 . 155.6(4) yes C5 . Fe3 . C30 . 158.5(5) yes C6 . Fe3 . C30 . 120.8(5) yes C7 . Fe3 . C30 . 102.2(5) yes C2 . Fe3 . C1 . 150.2(4) yes C4 . Fe3 . C1 . 163.4(4) yes C5 . Fe3 . C1 . 123.1(4) yes C6 . Fe3 . C1 . 101.9(4) yes C7 . Fe3 . C1 . 113.2(4) yes C27 . Fe3 . C28 . 39.6(5) yes C27 . Fe3 . C29 . 67.6(5) yes C28 . Fe3 . C29 . 40.7(4) yes C27 . Fe3 . C30 . 41.3(5) yes C28 . Fe3 . C30 . 68.4(5) yes C29 . Fe3 . C30 . 68.2(5) yes C27 . Fe3 . C1 . 68.3(5) yes C28 . Fe3 . C1 . 67.9(5) yes C29 . Fe3 . C1 . 39.8(5) yes C30 . Fe3 . C1 . 41.0(5) yes Fe3 . C4 . C2 . 66.8(5) yes Fe3 . C4 . C5 . 66.9(5) yes C2 . C4 . C5 . 103.9(7) yes Fe3 . C4 . B8 . 137.8(6) yes C2 . C4 . B8 . 131.9(7) yes C5 . C4 . B8 . 123.2(7) yes C4 . C5 . Fe3 . 71.9(5) yes C4 . C5 . C6 . 110.2(8) yes Fe3 . C5 . C6 . 69.8(5) yes C4 . C5 . H51 . 124.8 no Fe3 . C5 . H51 . 124.7 no C6 . C5 . H51 . 125.0 no C5 . C6 . Fe3 . 70.3(5) yes C5 . C6 . C7 . 108.9(8) yes Fe3 . C6 . C7 . 69.3(5) yes C5 . C6 . H61 . 125.4 no Fe3 . C6 . H61 . 124.9 no C7 . C6 . H61 . 125.7 no C6 . C7 . C2 . 106.6(8) yes C6 . C7 . Fe3 . 69.4(5) yes C2 . C7 . Fe3 . 69.5(5) yes C6 . C7 . H71 . 127.3 no C2 . C7 . H71 . 126.1 no Fe3 . C7 . H71 . 125.8 no C4 . B8 . C9 . 124.8(8) yes C4 . B8 . C18 . 115.0(7) yes C9 . B8 . C18 . 119.8(8) yes B8 . C9 . C10 . 123.1(8) yes B8 . C9 . C15 . 119.8(8) yes C10 . C9 . C15 . 117.1(8) yes C9 . C10 . C11 . 122.1(9) yes C9 . C10 . C12 . 120.1(9) yes C11 . C10 . C12 . 117.7(9) yes C10 . C11 . H111 . 109.9 no C10 . C11 . H112 . 110.7 no H111 . C11 . H112 . 108.7 no C10 . C11 . H113 . 110.4 no H111 . C11 . H113 . 108.3 no H112 . C11 . H113 . 108.8 no C10 . C12 . C13 . 122.8(9) yes C10 . C12 . H121 . 118.1 no C13 . C12 . H121 . 119.0 no C12 . C13 . C14 . 116.3(9) yes C12 . C13 . C17 . 121.7(10) yes C14 . C13 . C17 . 121.9(10) yes C13 . C14 . C15 . 124.3(10) yes C13 . C14 . H141 . 118.1 no C15 . C14 . H141 . 117.6 no C9 . C15 . C14 . 119.2(9) yes C9 . C15 . C16 . 123.1(9) yes C14 . C15 . C16 . 117.6(9) yes C15 . C16 . H161 . 109.0 no C15 . C16 . H163 . 110.8 no H161 . C16 . H163 . 110.1 no C15 . C16 . H162 . 109.4 no H161 . C16 . H162 . 108.2 no H163 . C16 . H162 . 109.3 no C13 . C17 . H171 . 110.9 no C13 . C17 . H173 . 111.1 no H171 . C17 . H173 . 108.2 no C13 . C17 . H172 . 110.4 no H171 . C17 . H172 . 108.4 no H173 . C17 . H172 . 107.7 no B8 . C18 . C19 . 118.8(8) yes B8 . C18 . C24 . 122.7(8) yes C19 . C18 . C24 . 118.5(8) yes C18 . C19 . C20 . 116.4(8) yes C18 . C19 . C26 . 121.9(8) yes C20 . C19 . C26 . 121.5(8) yes C19 . C20 . C21 . 127.4(9) yes C19 . C20 . H201 . 116.0 no C21 . C20 . H201 . 116.6 no C20 . C21 . C22 . 123.5(9) yes C20 . C21 . C23 . 115.7(9) yes C22 . C21 . C23 . 120.5(9) yes C21 . C22 . H221 . 109.7 no C21 . C22 . H222 . 110.3 no H221 . C22 . H222 . 108.1 no C21 . C22 . H223 . 111.4 no H221 . C22 . H223 . 108.0 no H222 . C22 . H223 . 109.2 no C21 . C23 . C24 . 120.2(9) yes C21 . C23 . H231 . 119.5 no C24 . C23 . H231 . 120.2 no C18 . C24 . C23 . 121.3(9) yes C18 . C24 . C25 . 123.4(8) yes C23 . C24 . C25 . 115.3(8) yes C24 . C25 . H251 . 110.5 no C24 . C25 . H253 . 109.4 no H251 . C25 . H253 . 109.6 no C24 . C25 . H252 . 109.7 no H251 . C25 . H252 . 109.3 no H253 . C25 . H252 . 108.4 no C19 . C26 . H261 . 110.7 no C19 . C26 . H262 . 110.4 no H261 . C26 . H262 . 108.2 no C19 . C26 . H263 . 109.7 no H261 . C26 . H263 . 109.8 no H262 . C26 . H263 . 107.9 no Fe3 . C27 . C28 . 70.5(6) yes Fe3 . C27 . C30 . 70.1(6) yes C28 . C27 . C30 . 109.2(11) yes Fe3 . C27 . H271 . 123.5 no C28 . C27 . H271 . 125.0 no C30 . C27 . H271 . 125.7 no Fe3 . C28 . C27 . 69.9(6) yes Fe3 . C28 . C29 . 69.5(6) yes C27 . C28 . C29 . 108.0(11) yes Fe3 . C28 . H281 . 125.4 no C27 . C28 . H281 . 125.6 no C29 . C28 . H281 . 126.3 no C28 . C29 . Fe3 . 69.9(6) yes C28 . C29 . C1 . 108.2(11) yes Fe3 . C29 . C1 . 69.5(6) yes C28 . C29 . H291 . 125.4 no Fe3 . C29 . H291 . 125.5 no C1 . C29 . H291 . 126.4 no C27 . C30 . Fe3 . 68.7(6) yes C27 . C30 . C1 . 105.1(12) yes Fe3 . C30 . C1 . 68.3(6) yes C27 . C30 . H301 . 127.5 no Fe3 . C30 . H301 . 131.1 no C1 . C30 . H301 . 127.3 no Br31 . C32 . Fe33 . 129.1(4) yes Br31 . C32 . C34 . 128.9(6) yes Fe33 . C32 . C34 . 70.4(5) yes Br31 . C32 . C37 . 121.9(6) yes Fe33 . C32 . C37 . 70.0(5) yes C34 . C32 . C37 . 109.1(7) yes C32 . Fe33 . C34 . 41.4(3) yes C32 . Fe33 . C35 . 68.7(3) yes C34 . Fe33 . C35 . 40.6(3) yes C32 . Fe33 . C36 . 68.4(3) yes C34 . Fe33 . C36 . 68.1(3) yes C35 . Fe33 . C36 . 40.1(4) yes C32 . Fe33 . C37 . 41.1(3) yes C34 . Fe33 . C37 . 69.6(3) yes C35 . Fe33 . C37 . 69.1(4) yes C36 . Fe33 . C37 . 41.1(3) yes C32 . Fe33 . C57 . 167.8(4) yes C34 . Fe33 . C57 . 129.1(4) yes C35 . Fe33 . C57 . 108.9(4) yes C36 . Fe33 . C57 . 118.1(4) yes C37 . Fe33 . C57 . 150.4(4) yes C32 . Fe33 . C58 . 131.0(4) yes C34 . Fe33 . C58 . 113.8(4) yes C35 . Fe33 . C58 . 124.3(4) yes C36 . Fe33 . C58 . 154.7(4) yes C37 . Fe33 . C58 . 164.0(4) yes C32 . Fe33 . C59 . 110.0(4) yes C34 . Fe33 . C59 . 124.9(4) yes C35 . Fe33 . C59 . 159.6(4) yes C36 . Fe33 . C59 . 159.9(4) yes C37 . Fe33 . C59 . 124.3(4) yes C32 . Fe33 . C60 . 118.5(4) yes C34 . Fe33 . C60 . 156.2(4) yes C35 . Fe33 . C60 . 159.5(4) yes C36 . Fe33 . C60 . 121.9(4) yes C37 . Fe33 . C60 . 103.0(4) yes C32 . Fe33 . C61 . 151.3(4) yes C34 . Fe33 . C61 . 162.7(4) yes C35 . Fe33 . C61 . 123.5(4) yes C36 . Fe33 . C61 . 103.5(4) yes C37 . Fe33 . C61 . 114.6(4) yes C57 . Fe33 . C58 . 39.7(4) yes C57 . Fe33 . C59 . 67.7(4) yes C58 . Fe33 . C59 . 40.3(4) yes C57 . Fe33 . C60 . 68.1(4) yes C58 . Fe33 . C60 . 67.3(5) yes C59 . Fe33 . C60 . 39.9(5) yes C57 . Fe33 . C61 . 40.3(4) yes C58 . Fe33 . C61 . 67.2(4) yes C59 . Fe33 . C61 . 67.9(4) yes C60 . Fe33 . C61 . 41.1(4) yes C32 . C34 . Fe33 . 68.2(5) yes C32 . C34 . C35 . 106.3(7) yes Fe33 . C34 . C35 . 68.7(5) yes C32 . C34 . B38 . 129.2(7) yes Fe33 . C34 . B38 . 139.1(6) yes C35 . C34 . B38 . 122.8(7) yes C34 . C35 . Fe33 . 70.7(5) yes C34 . C35 . C36 . 109.5(8) yes Fe33 . C35 . C36 . 70.9(5) yes C34 . C35 . H351 . 125.0 no Fe33 . C35 . H351 . 125.0 no C36 . C35 . H351 . 125.4 no C35 . C36 . Fe33 . 69.1(5) yes C35 . C36 . C37 . 108.9(8) yes Fe33 . C36 . C37 . 69.0(5) yes C35 . C36 . H361 . 125.7 no Fe33 . C36 . H361 . 125.7 no C37 . C36 . H361 . 125.4 no C36 . C37 . C32 . 106.1(8) yes C36 . C37 . Fe33 . 69.9(5) yes C32 . C37 . Fe33 . 68.9(5) yes C36 . C37 . H371 . 127.1 no C32 . C37 . H371 . 126.5 no Fe33 . C37 . H371 . 122.3 no C34 . B38 . C39 . 124.4(7) yes C34 . B38 . C48 . 116.2(7) yes C39 . B38 . C48 . 119.2(7) yes B38 . C39 . C40 . 120.0(8) yes B38 . C39 . C44 . 122.1(8) yes C40 . C39 . C44 . 117.8(8) yes C39 . C40 . C41 . 120.0(9) yes C39 . C40 . C47 . 121.8(8) yes C41 . C40 . C47 . 118.1(8) yes C40 . C41 . C42 . 122.3(9) yes C40 . C41 . H411 . 118.9 no C42 . C41 . H411 . 118.7 no C41 . C42 . C43 . 117.9(9) yes C41 . C42 . C46 . 121.0(10) yes C43 . C42 . C46 . 121.1(10) yes C42 . C43 . C44 . 121.7(9) yes C42 . C43 . H431 . 119.4 no C44 . C43 . H431 . 118.8 no C39 . C44 . C43 . 120.1(9) yes C39 . C44 . C45 . 122.7(8) yes C43 . C44 . C45 . 117.2(9) yes C44 . C45 . H452 . 109.9 no C44 . C45 . H451 . 111.0 no H452 . C45 . H451 . 108.4 no C44 . C45 . H453 . 110.4 no H452 . C45 . H453 . 109.0 no H451 . C45 . H453 . 108.1 no C42 . C46 . H463 . 110.0 no C42 . C46 . H462 . 109.8 no H463 . C46 . H462 . 109.4 no C42 . C46 . H461 . 109.6 no H463 . C46 . H461 . 108.4 no H462 . C46 . H461 . 109.5 no C40 . C47 . H471 . 110.7 no C40 . C47 . H473 . 109.7 no H471 . C47 . H473 . 108.3 no C40 . C47 . H472 . 111.2 no H471 . C47 . H472 . 108.5 no H473 . C47 . H472 . 108.3 no B38 . C48 . C49 . 123.0(7) yes B38 . C48 . C55 . 120.8(7) yes C49 . C48 . C55 . 116.2(8) yes C48 . C49 . C50 . 122.8(8) yes C48 . C49 . C51 . 120.4(8) yes C50 . C49 . C51 . 116.6(8) yes C49 . C50 . H501 . 108.7 no C49 . C50 . H502 . 110.3 no H501 . C50 . H502 . 108.7 no C49 . C50 . H503 . 110.2 no H501 . C50 . H503 . 109.6 no H502 . C50 . H503 . 109.4 no C49 . C51 . C52 . 122.5(8) yes C49 . C51 . H511 . 118.2 no C52 . C51 . H511 . 119.3 no C51 . C52 . C53 . 120.8(9) yes C51 . C52 . C54 . 117.9(8) yes C53 . C52 . C54 . 121.3(9) yes C52 . C53 . H531 . 110.2 no C52 . C53 . H532 . 110.1 no H531 . C53 . H532 . 107.5 no C52 . C53 . H533 . 111.3 no H531 . C53 . H533 . 108.6 no H532 . C53 . H533 . 109.0 no C52 . C54 . C55 . 121.6(8) yes C52 . C54 . H541 . 118.8 no C55 . C54 . H541 . 119.7 no C48 . C55 . C54 . 121.3(8) yes C48 . C55 . C56 . 121.3(8) yes C54 . C55 . C56 . 117.4(8) yes C55 . C56 . H561 . 111.1 no C55 . C56 . H563 . 109.5 no H561 . C56 . H563 . 108.6 no C55 . C56 . H562 . 109.8 no H561 . C56 . H562 . 109.6 no H563 . C56 . H562 . 108.3 no Fe33 . C57 . C58 . 70.0(5) yes Fe33 . C57 . C61 . 69.6(6) yes C58 . C57 . C61 . 107.8(9) yes Fe33 . C57 . H571 . 125.2 no C58 . C57 . H571 . 125.7 no C61 . C57 . H571 . 126.5 no Fe33 . C58 . C57 . 70.3(5) yes Fe33 . C58 . C59 . 69.3(6) yes C57 . C58 . C59 . 108.8(10) yes Fe33 . C58 . H581 . 124.7 no C57 . C58 . H581 . 125.5 no C59 . C58 . H581 . 125.7 no C58 . C59 . Fe33 . 70.4(6) yes C58 . C59 . C60 . 108.0(10) yes Fe33 . C59 . C60 . 69.8(6) yes C58 . C59 . H591 . 125.7 no Fe33 . C59 . H591 . 125.6 no C60 . C59 . H591 . 126.2 no C59 . C60 . Fe33 . 70.4(6) yes C59 . C60 . C61 . 108.1(10) yes Fe33 . C60 . C61 . 70.2(6) yes C59 . C60 . H601 . 125.5 no Fe33 . C60 . H601 . 124.7 no C61 . C60 . H601 . 126.4 no C60 . C61 . C57 . 107.2(10) yes C60 . C61 . Fe33 . 68.7(6) yes C57 . C61 . Fe33 . 70.1(5) yes C60 . C61 . H611 . 125.1 no C57 . C61 . H611 . 127.5 no Fe33 . C61 . H611 . 122.0 no C30 . C1 . C29 . 109.4(11) yes C30 . C1 . Fe3 . 70.7(6) yes C29 . C1 . Fe3 . 70.7(6) yes C30 . C1 . H11 . 125.5 no C29 . C1 . H11 . 125.1 no Fe3 . C1 . H11 . 125.4 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 C25 . H252 . C4 . 130 0.97 2.56 3.261(15) yes _chemical_name_common . #============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 742658' #============================================================================== _audit_creation_date 09-07-23 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 059imdv08 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 10.8437(3) _cell_length_b 11.0155(3) _cell_length_c 13.9298(4) _cell_angle_alpha 103.6776(11) _cell_angle_beta 98.4755(11) _cell_angle_gamma 95.9081(11) _cell_volume 1582.54(8) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 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' P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C40 H40 B1 Fe1 P1 # Dc = 1.30 Fooo = 652.00 Mu = 5.55 M = 618.39 # Found Formula = C40 H40 B1 Fe1 P1 # Dc = 1.30 FOOO = 652.00 Mu = 5.55 M = 618.39 _chemical_formula_sum 'C40 H40 B1 Fe1 P1' _chemical_formula_moiety 'C40 H40 B1 Fe1 P1' _chemical_compound_source ? _chemical_formula_weight 618.39 _cell_measurement_reflns_used 6481 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_min 0.04 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.38 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 0.555 # Sheldrick geometric approximatio 0.93 0.98 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.98 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _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 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 24749 _reflns_number_total 7156 _diffrn_reflns_av_R_equivalents 0.089 # Number of reflections with Friedels Law is 7156 # Number of reflections without Friedels Law is 12024 # Theoretical number of reflections is about 7234 _diffrn_reflns_theta_min 5.102 _diffrn_reflns_theta_max 27.449 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.626 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _reflns_limit_h_min -14 _reflns_limit_h_max 13 _reflns_limit_k_min -14 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 18 _oxford_diffrn_Wilson_B_factor 1.54 _oxford_diffrn_Wilson_scale 21.19 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -1.03 _refine_diff_density_max 1.19 # 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 7156 _refine_ls_number_restraints 0 _refine_ls_number_parameters 389 _oxford_refine_ls_R_factor_ref 0.1073 _refine_ls_wR_factor_ref 0.1057 _refine_ls_goodness_of_fit_ref 0.9560 _refine_ls_shift/su_max 0.000422 # The values computed from all data _oxford_reflns_number_all 7156 _refine_ls_R_factor_all 0.1073 _refine_ls_wR_factor_all 0.1057 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4419 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_gt 0.0880 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_hydrogen_treatment 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^) + ( 0.03P)^2^ + 1.11P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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 0.45240(4) 0.49563(4) 0.19954(3) 0.0213 1.0000 Uani . . . . . . . C2 C 0.2796(2) 0.5599(2) 0.20993(19) 0.0186 1.0000 Uani . . . . . . . C3 C 0.3651(2) 0.6441(2) 0.17374(19) 0.0189 1.0000 Uani . . . . . . . C4 C 0.3957(2) 0.5726(2) 0.0830(2) 0.0215 1.0000 Uani . . . . . . . C5 C 0.3359(2) 0.4468(2) 0.06194(19) 0.0220 1.0000 Uani . . . . . . . C6 C 0.2671(2) 0.4379(2) 0.13934(19) 0.0213 1.0000 Uani . . . . . . . P7 P 0.42676(6) 0.80995(6) 0.23523(5) 0.0207 1.0000 Uani . . . . . . . C8 C 0.5377(2) 0.8407(2) 0.1525(2) 0.0217 1.0000 Uani . . . . . . . C9 C 0.5033(3) 0.8602(2) 0.0583(2) 0.0246 1.0000 Uani . . . . . . . C10 C 0.5942(3) 0.8843(3) 0.0012(2) 0.0301 1.0000 Uani . . . . . . . C11 C 0.7205(3) 0.8896(3) 0.0391(2) 0.0333 1.0000 Uani . . . . . . . C12 C 0.7558(3) 0.8697(3) 0.1324(2) 0.0362 1.0000 Uani . . . . . . . C13 C 0.6656(3) 0.8456(3) 0.1891(2) 0.0298 1.0000 Uani . . . . . . . C14 C 0.2964(2) 0.8911(2) 0.1946(2) 0.0213 1.0000 Uani . . . . . . . C15 C 0.1926(3) 0.8340(3) 0.1211(2) 0.0283 1.0000 Uani . . . . . . . C16 C 0.0944(3) 0.9004(3) 0.0987(2) 0.0364 1.0000 Uani . . . . . . . C17 C 0.0988(3) 1.0246(3) 0.1501(2) 0.0388 1.0000 Uani . . . . . . . C18 C 0.2019(3) 1.0841(3) 0.2223(2) 0.0381 1.0000 Uani . . . . . . . C19 C 0.2997(3) 1.0176(3) 0.2451(2) 0.0295 1.0000 Uani . . . . . . . B20 B 0.1971(3) 0.5863(3) 0.2931(2) 0.0215 1.0000 Uani . . . . . . . C21 C 0.2004(2) 0.7248(2) 0.36314(19) 0.0216 1.0000 Uani . . . . . . . C22 C 0.3071(2) 0.7947(2) 0.43319(19) 0.0216 1.0000 Uani . . . . . . . C23 C 0.3087(3) 0.9212(3) 0.4807(2) 0.0255 1.0000 Uani . . . . . . . C24 C 0.2073(3) 0.9843(3) 0.4620(2) 0.0251 1.0000 Uani . . . . . . . C25 C 0.0991(3) 0.9145(3) 0.3986(2) 0.0266 1.0000 Uani . . . . . . . C26 C 0.0929(2) 0.7866(3) 0.35042(19) 0.0223 1.0000 Uani . . . . . . . C27 C -0.0291(3) 0.7214(3) 0.2843(2) 0.0335 1.0000 Uani . . . . . . . C28 C 0.2139(3) 1.1238(3) 0.5073(2) 0.0371 1.0000 Uani . . . . . . . C29 C 0.4202(3) 0.7344(3) 0.4623(2) 0.0286 1.0000 Uani . . . . . . . C30 C 0.0963(2) 0.4728(2) 0.29559(19) 0.0191 1.0000 Uani . . . . . . . C31 C 0.0005(2) 0.4121(2) 0.2123(2) 0.0239 1.0000 Uani . . . . . . . C32 C -0.0163(3) 0.4496(3) 0.1137(2) 0.0272 1.0000 Uani . . . . . . . C33 C -0.0897(3) 0.3155(3) 0.2193(2) 0.0289 1.0000 Uani . . . . . . . C34 C -0.0898(3) 0.2764(3) 0.3061(2) 0.0305 1.0000 Uani . . . . . . . C35 C 0.0047(3) 0.3344(3) 0.3885(2) 0.0301 1.0000 Uani . . . . . . . C36 C 0.0965(3) 0.4300(3) 0.3837(2) 0.0240 1.0000 Uani . . . . . . . C37 C 0.1974(3) 0.4855(3) 0.4750(2) 0.0328 1.0000 Uani . . . . . . . C38 C -0.1917(3) 0.1760(3) 0.3139(3) 0.0513 1.0000 Uani . . . . . . . C39 C 0.6080(3) 0.5571(3) 0.3110(2) 0.0323 1.0000 Uani . . . . . . . C40 C 0.6449(3) 0.5115(3) 0.2173(2) 0.0327 1.0000 Uani . . . . . . . C41 C 0.5906(3) 0.3830(3) 0.1796(2) 0.0309 1.0000 Uani . . . . . . . C42 C 0.5197(3) 0.3500(3) 0.2495(2) 0.0330 1.0000 Uani . . . . . . . C43 C 0.5303(3) 0.4581(3) 0.3311(2) 0.0320 1.0000 Uani . . . . . . . H41 H 0.4514 0.6069 0.0426 0.0291 1.0000 Uiso R . . . . . . H51 H 0.3419 0.3766 0.0039 0.0270 1.0000 Uiso R . . . . . . H61 H 0.2168 0.3597 0.1449 0.0269 1.0000 Uiso R . . . . . . H91 H 0.4161 0.8582 0.0326 0.0353 1.0000 Uiso R . . . . . . H101 H 0.5689 0.8980 -0.0633 0.0393 1.0000 Uiso R . . . . . . H111 H 0.7833 0.9064 0.0009 0.0469 1.0000 Uiso R . . . . . . H121 H 0.8419 0.8717 0.1579 0.0451 1.0000 Uiso R . . . . . . H131 H 0.6916 0.8332 0.2548 0.0380 1.0000 Uiso R . . . . . . H151 H 0.1890 0.7478 0.0853 0.0394 1.0000 Uiso R . . . . . . H161 H 0.0237 0.8602 0.0481 0.0526 1.0000 Uiso R . . . . . . H171 H 0.0309 1.0699 0.1369 0.0559 1.0000 Uiso R . . . . . . H181 H 0.2059 1.1707 0.2572 0.0552 1.0000 Uiso R . . . . . . H191 H 0.3712 1.0587 0.2970 0.0421 1.0000 Uiso R . . . . . . H231 H 0.3811 0.9653 0.5272 0.0350 1.0000 Uiso R . . . . . . H251 H 0.0267 0.9544 0.3874 0.0361 1.0000 Uiso R . . . . . . H273 H -0.0939 0.7736 0.2932 0.0531 1.0000 Uiso R . . . . . . H272 H -0.0551 0.6420 0.3016 0.0531 1.0000 Uiso R . . . . . . H271 H -0.0200 0.7012 0.2145 0.0530 1.0000 Uiso R . . . . . . H281 H 0.1345 1.1432 0.5252 0.0550 1.0000 Uiso R . . . . . . H282 H 0.2779 1.1511 0.5672 0.0552 1.0000 Uiso R . . . . . . H283 H 0.2347 1.1709 0.4593 0.0554 1.0000 Uiso R . . . . . . H293 H 0.4968 0.7923 0.4713 0.0465 1.0000 Uiso R . . . . . . H292 H 0.4159 0.7113 0.5253 0.0461 1.0000 Uiso R . . . . . . H291 H 0.4227 0.6589 0.4104 0.0459 1.0000 Uiso R . . . . . . H321 H -0.1008 0.4666 0.0972 0.0460 1.0000 Uiso R . . . . . . H322 H 0.0413 0.5239 0.1178 0.0460 1.0000 Uiso R . . . . . . H323 H -0.0011 0.3809 0.0596 0.0463 1.0000 Uiso R . . . . . . H331 H -0.1534 0.2769 0.1623 0.0382 1.0000 Uiso R . . . . . . H351 H 0.0069 0.3085 0.4493 0.0416 1.0000 Uiso R . . . . . . H371 H 0.1810 0.4501 0.5300 0.0550 1.0000 Uiso R . . . . . . H372 H 0.2018 0.5761 0.4966 0.0551 1.0000 Uiso R . . . . . . H373 H 0.2787 0.4664 0.4606 0.0549 1.0000 Uiso R . . . . . . H383 H -0.1560 0.1170 0.3472 0.0842 1.0000 Uiso R . . . . . . H382 H -0.2524 0.2130 0.3510 0.0842 1.0000 Uiso R . . . . . . H381 H -0.2369 0.1278 0.2474 0.0842 1.0000 Uiso R . . . . . . H401 H 0.6975 0.5607 0.1833 0.0410 1.0000 Uiso R . . . . . . H421 H 0.4696 0.2659 0.2419 0.0399 1.0000 Uiso R . . . . . . H431 H 0.4903 0.4624 0.3914 0.0452 1.0000 Uiso R . . . . . . H391 H 0.6307 0.6448 0.3542 0.0401 1.0000 Uiso R . . . . . . H411 H 0.5993 0.3264 0.1148 0.0421 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 0.0194(2) 0.0210(2) 0.0242(2) 0.00667(17) 0.00400(17) 0.00459(16) C2 0.0129(13) 0.0248(14) 0.0196(14) 0.0087(11) 0.0033(11) 0.0020(11) C3 0.0172(13) 0.0205(14) 0.0193(14) 0.0066(11) 0.0010(11) 0.0040(11) C4 0.0146(13) 0.0251(15) 0.0274(15) 0.0079(12) 0.0088(12) 0.0050(11) C5 0.0207(14) 0.0246(15) 0.0195(14) 0.0031(11) 0.0021(12) 0.0059(12) C6 0.0185(14) 0.0210(14) 0.0247(15) 0.0063(12) 0.0051(12) 0.0010(11) P7 0.0184(4) 0.0206(4) 0.0234(4) 0.0056(3) 0.0062(3) 0.0012(3) C8 0.0220(15) 0.0164(13) 0.0283(16) 0.0057(12) 0.0089(12) 0.0030(11) C9 0.0228(15) 0.0216(14) 0.0321(16) 0.0093(12) 0.0080(13) 0.0052(12) C10 0.0386(18) 0.0263(16) 0.0302(17) 0.0109(13) 0.0127(14) 0.0079(13) C11 0.0348(18) 0.0271(16) 0.047(2) 0.0140(14) 0.0254(16) 0.0061(13) C12 0.0200(16) 0.0427(19) 0.048(2) 0.0151(16) 0.0103(15) 0.0018(14) C13 0.0204(15) 0.0369(17) 0.0346(17) 0.0147(14) 0.0056(13) 0.0011(13) C14 0.0187(14) 0.0232(14) 0.0276(15) 0.0101(12) 0.0150(12) 0.0048(11) C15 0.0215(15) 0.0289(16) 0.0367(17) 0.0106(13) 0.0068(13) 0.0061(12) C16 0.0269(17) 0.049(2) 0.0424(19) 0.0232(16) 0.0101(14) 0.0124(15) C17 0.0371(19) 0.049(2) 0.050(2) 0.0311(17) 0.0254(17) 0.0245(16) C18 0.057(2) 0.0277(17) 0.045(2) 0.0184(15) 0.0308(18) 0.0234(16) C19 0.0387(18) 0.0246(16) 0.0297(17) 0.0094(13) 0.0137(14) 0.0079(13) B20 0.0188(16) 0.0292(17) 0.0170(16) 0.0100(13) -0.0024(13) 0.0034(13) C21 0.0213(14) 0.0256(15) 0.0200(14) 0.0090(12) 0.0061(12) 0.0025(12) C22 0.0219(14) 0.0291(15) 0.0147(14) 0.0066(12) 0.0051(11) 0.0035(12) C23 0.0258(15) 0.0285(16) 0.0196(15) 0.0033(12) 0.0045(12) -0.0014(12) C24 0.0260(16) 0.0251(15) 0.0275(16) 0.0081(12) 0.0130(13) 0.0039(12) C25 0.0239(15) 0.0297(16) 0.0319(17) 0.0103(13) 0.0154(13) 0.0094(12) C26 0.0191(14) 0.0283(15) 0.0215(15) 0.0078(12) 0.0077(12) 0.0032(12) C27 0.0242(16) 0.0341(17) 0.0404(19) 0.0048(14) 0.0022(14) 0.0125(13) C28 0.0403(19) 0.0274(16) 0.0421(19) 0.0023(14) 0.0143(16) 0.0030(14) C29 0.0236(15) 0.0329(17) 0.0286(16) 0.0065(13) 0.0060(13) 0.0019(13) C30 0.0175(13) 0.0227(14) 0.0185(14) 0.0062(11) 0.0052(11) 0.0047(11) C31 0.0213(14) 0.0220(14) 0.0296(16) 0.0054(12) 0.0095(12) 0.0046(12) C32 0.0204(15) 0.0332(16) 0.0253(16) 0.0058(13) 0.0015(12) -0.0003(12) C33 0.0273(16) 0.0238(15) 0.0337(17) 0.0021(13) 0.0080(14) 0.0039(13) C34 0.0312(17) 0.0228(15) 0.0430(19) 0.0107(14) 0.0193(15) 0.0049(13) C35 0.0360(18) 0.0290(16) 0.0325(17) 0.0133(13) 0.0172(15) 0.0089(14) C36 0.0227(15) 0.0279(15) 0.0247(15) 0.0086(12) 0.0091(12) 0.0075(12) C37 0.0285(16) 0.0443(19) 0.0299(17) 0.0184(14) 0.0041(13) 0.0059(14) C38 0.050(2) 0.037(2) 0.067(2) 0.0140(18) 0.023(2) -0.0123(16) C39 0.0290(17) 0.0292(16) 0.0340(18) 0.0051(14) -0.0074(14) 0.0075(13) C40 0.0176(15) 0.0377(18) 0.0427(19) 0.0095(15) 0.0039(14) 0.0073(13) C41 0.0242(16) 0.0326(17) 0.0354(17) 0.0052(14) 0.0024(14) 0.0135(13) C42 0.0380(18) 0.0229(15) 0.0382(18) 0.0108(14) -0.0016(15) 0.0100(13) C43 0.0361(18) 0.0365(17) 0.0277(16) 0.0151(14) 0.0011(14) 0.0151(14) _refine_ls_extinction_coef 46(16) _refine_ls_extinction_method 'Larson (1970), Equation 22' _oxford_refine_ls_scale 0.22569(16) 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 . 2.083(2) yes Fe1 . C3 . 2.048(3) yes Fe1 . C4 . 2.049(3) yes Fe1 . C5 . 2.053(3) yes Fe1 . C6 . 2.033(3) yes Fe1 . C39 . 2.052(3) yes Fe1 . C40 . 2.050(3) yes Fe1 . C41 . 2.051(3) yes Fe1 . C42 . 2.052(3) yes Fe1 . C43 . 2.053(3) yes C2 . C3 . 1.469(3) yes C2 . C6 . 1.446(3) yes C2 . B20 . 1.558(4) yes C3 . C4 . 1.426(3) yes C3 . P7 . 1.832(3) yes C4 . C5 . 1.412(4) yes C4 . H41 . 0.989 no C5 . C6 . 1.414(3) yes C5 . H51 . 0.993 no C6 . H61 . 0.996 no P7 . C8 . 1.844(3) yes P7 . C14 . 1.839(3) yes C8 . C9 . 1.383(4) yes C8 . C13 . 1.396(4) yes C9 . C10 . 1.397(4) yes C9 . H91 . 0.956 no C10 . C11 . 1.383(4) yes C10 . H101 . 0.952 no C11 . C12 . 1.375(4) yes C11 . H111 . 0.953 no C12 . C13 . 1.388(4) yes C12 . H121 . 0.945 no C13 . H131 . 0.963 no C14 . C15 . 1.386(4) yes C14 . C19 . 1.398(4) yes C15 . C16 . 1.392(4) yes C15 . H151 . 0.956 no C16 . C17 . 1.378(4) yes C16 . H161 . 0.951 no C17 . C18 . 1.377(5) yes C17 . H171 . 0.951 no C18 . C19 . 1.391(4) yes C18 . H181 . 0.955 no C19 . H191 . 0.967 no B20 . C21 . 1.598(4) yes B20 . C30 . 1.584(4) yes C21 . C22 . 1.418(4) yes C21 . C26 . 1.419(4) yes C22 . C23 . 1.392(4) yes C22 . C29 . 1.503(4) yes C23 . C24 . 1.385(4) yes C23 . H231 . 0.946 no C24 . C25 . 1.391(4) yes C24 . C28 . 1.507(4) yes C25 . C26 . 1.400(4) yes C25 . H251 . 0.949 no C26 . C27 . 1.500(4) yes C27 . H273 . 0.957 no C27 . H272 . 0.985 no C27 . H271 . 0.967 no C28 . H281 . 0.962 no C28 . H282 . 0.967 no C28 . H283 . 0.975 no C29 . H293 . 0.967 no C29 . H292 . 0.976 no C29 . H291 . 0.970 no C30 . C31 . 1.416(4) yes C30 . C36 . 1.415(4) yes C31 . C32 . 1.516(4) yes C31 . C33 . 1.400(4) yes C32 . H321 . 0.959 no C32 . H322 . 0.963 no C32 . H323 . 0.980 no C33 . C34 . 1.377(4) yes C33 . H331 . 0.952 no C34 . C35 . 1.395(4) yes C34 . C38 . 1.514(4) yes C35 . C36 . 1.394(4) yes C35 . H351 . 0.953 no C36 . C37 . 1.507(4) yes C37 . H371 . 0.968 no C37 . H372 . 0.965 no C37 . H373 . 0.965 no C38 . H383 . 0.963 no C38 . H382 . 0.961 no C38 . H381 . 0.980 no C39 . C40 . 1.415(4) yes C39 . C43 . 1.414(4) yes C39 . H391 . 0.994 no C40 . C41 . 1.419(4) yes C40 . H401 . 0.989 no C41 . C42 . 1.415(4) yes C41 . H411 . 0.992 no C42 . C43 . 1.420(4) yes C42 . H421 . 0.998 no C43 . H431 . 0.995 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 . 41.64(9) yes C2 . Fe1 . C4 . 68.94(10) yes C3 . Fe1 . C4 . 40.74(10) yes C2 . Fe1 . C5 . 68.99(10) yes C3 . Fe1 . C5 . 68.74(10) yes C4 . Fe1 . C5 . 40.27(10) yes C2 . Fe1 . C6 . 41.11(10) yes C3 . Fe1 . C6 . 69.10(10) yes C4 . Fe1 . C6 . 68.00(10) yes C5 . Fe1 . C6 . 40.50(10) yes C2 . Fe1 . C39 . 123.19(11) yes C3 . Fe1 . C39 . 110.95(11) yes C4 . Fe1 . C39 . 128.13(11) yes C5 . Fe1 . C39 . 162.53(11) yes C6 . Fe1 . C39 . 156.85(11) yes C2 . Fe1 . C40 . 155.79(11) yes C3 . Fe1 . C40 . 119.19(11) yes C4 . Fe1 . C40 . 106.15(11) yes C5 . Fe1 . C40 . 123.44(11) yes C6 . Fe1 . C40 . 160.87(11) yes C2 . Fe1 . C41 . 163.50(11) yes C3 . Fe1 . C41 . 151.10(11) yes C4 . Fe1 . C41 . 115.64(11) yes C5 . Fe1 . C41 . 103.69(11) yes C6 . Fe1 . C41 . 124.02(11) yes C2 . Fe1 . C42 . 128.33(11) yes C3 . Fe1 . C42 . 168.16(11) yes C4 . Fe1 . C42 . 149.50(11) yes C5 . Fe1 . C42 . 116.25(11) yes C6 . Fe1 . C42 . 107.17(12) yes C2 . Fe1 . C43 . 111.35(11) yes C3 . Fe1 . C43 . 131.02(11) yes C4 . Fe1 . C43 . 167.24(11) yes C5 . Fe1 . C43 . 152.44(11) yes C6 . Fe1 . C43 . 121.18(11) yes C39 . Fe1 . C40 . 40.36(11) yes C39 . Fe1 . C41 . 67.74(12) yes C40 . Fe1 . C41 . 40.48(11) yes C39 . Fe1 . C42 . 67.79(12) yes C40 . Fe1 . C42 . 68.07(12) yes C41 . Fe1 . C42 . 40.36(11) yes C39 . Fe1 . C43 . 40.30(11) yes C40 . Fe1 . C43 . 68.06(12) yes C41 . Fe1 . C43 . 67.93(12) yes C42 . Fe1 . C43 . 40.47(11) yes Fe1 . C2 . C3 . 67.91(13) yes Fe1 . C2 . C6 . 67.57(14) yes C3 . C2 . C6 . 105.1(2) yes Fe1 . C2 . B20 . 135.29(19) yes C3 . C2 . B20 . 132.0(2) yes C6 . C2 . B20 . 122.2(2) yes C2 . C3 . Fe1 . 70.45(14) yes C2 . C3 . C4 . 107.8(2) yes Fe1 . C3 . C4 . 69.64(15) yes C2 . C3 . P7 . 126.65(18) yes Fe1 . C3 . P7 . 123.88(13) yes C4 . C3 . P7 . 125.57(19) yes C3 . C4 . Fe1 . 69.62(15) yes C3 . C4 . C5 . 109.3(2) yes Fe1 . C4 . C5 . 70.05(15) yes C3 . C4 . H41 . 124.5 no Fe1 . C4 . H41 . 125.8 no C5 . C4 . H41 . 126.2 no C4 . C5 . Fe1 . 69.69(15) yes C4 . C5 . C6 . 107.7(2) yes Fe1 . C5 . C6 . 68.96(15) yes C4 . C5 . H51 . 126.4 no Fe1 . C5 . H51 . 126.1 no C6 . C5 . H51 . 125.9 no C2 . C6 . C5 . 110.0(2) yes C2 . C6 . Fe1 . 71.32(14) yes C5 . C6 . Fe1 . 70.54(15) yes C2 . C6 . H61 . 124.4 no C5 . C6 . H61 . 125.6 no Fe1 . C6 . H61 . 125.0 no C3 . P7 . C8 . 99.84(11) yes C3 . P7 . C14 . 102.08(12) yes C8 . P7 . C14 . 101.18(12) yes P7 . C8 . C9 . 124.8(2) yes P7 . C8 . C13 . 116.8(2) yes C9 . C8 . C13 . 118.4(2) yes C8 . C9 . C10 . 120.9(3) yes C8 . C9 . H91 . 119.2 no C10 . C9 . H91 . 119.9 no C9 . C10 . C11 . 119.9(3) yes C9 . C10 . H101 . 119.8 no C11 . C10 . H101 . 120.3 no C10 . C11 . C12 . 119.7(3) yes C10 . C11 . H111 . 120.6 no C12 . C11 . H111 . 119.6 no C11 . C12 . C13 . 120.4(3) yes C11 . C12 . H121 . 119.9 no C13 . C12 . H121 . 119.7 no C8 . C13 . C12 . 120.7(3) yes C8 . C13 . H131 . 119.7 no C12 . C13 . H131 . 119.6 no P7 . C14 . C15 . 124.6(2) yes P7 . C14 . C19 . 117.4(2) yes C15 . C14 . C19 . 118.0(3) yes C14 . C15 . C16 . 120.9(3) yes C14 . C15 . H151 . 119.2 no C16 . C15 . H151 . 119.9 no C15 . C16 . C17 . 120.2(3) yes C15 . C16 . H161 . 120.1 no C17 . C16 . H161 . 119.7 no C16 . C17 . C18 . 120.0(3) yes C16 . C17 . H171 . 120.7 no C18 . C17 . H171 . 119.3 no C17 . C18 . C19 . 119.8(3) yes C17 . C18 . H181 . 120.2 no C19 . C18 . H181 . 120.0 no C14 . C19 . C18 . 121.1(3) yes C14 . C19 . H191 . 119.0 no C18 . C19 . H191 . 119.9 no C2 . B20 . C21 . 122.0(2) yes C2 . B20 . C30 . 116.6(2) yes C21 . B20 . C30 . 121.0(2) yes B20 . C21 . C22 . 124.5(2) yes B20 . C21 . C26 . 118.4(2) yes C22 . C21 . C26 . 117.0(2) yes C21 . C22 . C23 . 120.9(2) yes C21 . C22 . C29 . 121.7(2) yes C23 . C22 . C29 . 117.4(2) yes C22 . C23 . C24 . 121.9(3) yes C22 . C23 . H231 . 119.0 no C24 . C23 . H231 . 119.1 no C23 . C24 . C25 . 117.6(2) yes C23 . C24 . C28 . 121.5(3) yes C25 . C24 . C28 . 121.0(3) yes C24 . C25 . C26 . 122.2(3) yes C24 . C25 . H251 . 119.3 no C26 . C25 . H251 . 118.5 no C21 . C26 . C25 . 120.1(2) yes C21 . C26 . C27 . 122.7(2) yes C25 . C26 . C27 . 117.3(2) yes C26 . C27 . H273 . 110.6 no C26 . C27 . H272 . 109.7 no H273 . C27 . H272 . 108.5 no C26 . C27 . H271 . 110.6 no H273 . C27 . H271 . 109.2 no H272 . C27 . H271 . 108.2 no C24 . C28 . H281 . 110.8 no C24 . C28 . H282 . 110.3 no H281 . C28 . H282 . 108.4 no C24 . C28 . H283 . 110.0 no H281 . C28 . H283 . 108.5 no H282 . C28 . H283 . 108.7 no C22 . C29 . H293 . 110.5 no C22 . C29 . H292 . 110.0 no H293 . C29 . H292 . 108.4 no C22 . C29 . H291 . 109.8 no H293 . C29 . H291 . 109.1 no H292 . C29 . H291 . 108.9 no B20 . C30 . C31 . 122.4(2) yes B20 . C30 . C36 . 120.6(2) yes C31 . C30 . C36 . 117.0(2) yes C30 . C31 . C32 . 123.8(2) yes C30 . C31 . C33 . 120.4(3) yes C32 . C31 . C33 . 115.7(3) yes C31 . C32 . H321 . 109.8 no C31 . C32 . H322 . 111.0 no H321 . C32 . H322 . 108.7 no C31 . C32 . H323 . 110.2 no H321 . C32 . H323 . 108.5 no H322 . C32 . H323 . 108.5 no C31 . C33 . C34 . 122.0(3) yes C31 . C33 . H331 . 118.6 no C34 . C33 . H331 . 119.3 no C33 . C34 . C35 . 118.2(3) yes C33 . C34 . C38 . 121.3(3) yes C35 . C34 . C38 . 120.4(3) yes C34 . C35 . C36 . 121.2(3) yes C34 . C35 . H351 . 119.8 no C36 . C35 . H351 . 119.1 no C30 . C36 . C35 . 121.2(3) yes C30 . C36 . C37 . 120.9(2) yes C35 . C36 . C37 . 118.0(3) yes C36 . C37 . H371 . 110.6 no C36 . C37 . H372 . 111.3 no H371 . C37 . H372 . 108.6 no C36 . C37 . H373 . 110.5 no H371 . C37 . H373 . 107.5 no H372 . C37 . H373 . 108.3 no C34 . C38 . H383 . 110.8 no C34 . C38 . H382 . 111.0 no H383 . C38 . H382 . 108.2 no C34 . C38 . H381 . 111.4 no H383 . C38 . H381 . 107.5 no H382 . C38 . H381 . 107.7 no Fe1 . C39 . C40 . 69.73(16) yes Fe1 . C39 . C43 . 69.89(17) yes C40 . C39 . C43 . 108.5(3) yes Fe1 . C39 . H391 . 124.7 no C40 . C39 . H391 . 125.5 no C43 . C39 . H391 . 126.0 no C39 . C40 . Fe1 . 69.91(16) yes C39 . C40 . C41 . 107.6(3) yes Fe1 . C40 . C41 . 69.79(16) yes C39 . C40 . H401 . 126.4 no Fe1 . C40 . H401 . 124.7 no C41 . C40 . H401 . 126.0 no C40 . C41 . Fe1 . 69.73(15) yes C40 . C41 . C42 . 108.2(3) yes Fe1 . C41 . C42 . 69.86(16) yes C40 . C41 . H411 . 126.0 no Fe1 . C41 . H411 . 125.1 no C42 . C41 . H411 . 125.8 no C41 . C42 . Fe1 . 69.78(16) yes C41 . C42 . C43 . 108.0(3) yes Fe1 . C42 . C43 . 69.83(16) yes C41 . C42 . H421 . 125.8 no Fe1 . C42 . H421 . 125.0 no C43 . C42 . H421 . 126.2 no C42 . C43 . C39 . 107.7(3) yes C42 . C43 . Fe1 . 69.71(17) yes C39 . C43 . Fe1 . 69.82(17) yes C42 . C43 . H431 . 125.6 no C39 . C43 . H431 . 126.6 no Fe1 . C43 . H431 . 126.1 no _chemical_name_common . #============================================================================== data_5 _database_code_depnum_ccdc_archive 'CCDC 742659' #============================================================================== _audit_creation_date 09-05-18 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 090addv09 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 9.3714(2) _cell_length_b 11.8431(2) _cell_length_c 25.5848(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2839.57(10) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz x,y,z x+1/2,-y+1/2,-z -x,y+1/2,-z+1/2 -x+1/2,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' 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' Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805 1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C35 H50 B1 Fe1 O1 S1 # Dc = 1.37 Fooo = 1208.00 Mu = 6.33 M = 585.51 # Found Formula = C35 H37 B1 Fe1 O1 S1 # Dc = 1.34 FOOO = 1208.00 Mu = 6.32 M = 572.40 _chemical_formula_sum 'C35 H37 B1 Fe1 O1 S1' _chemical_formula_moiety 'C35 H37 B1 Fe1 O1 S1' _chemical_compound_source . _chemical_formula_weight 572.40 _cell_measurement_reflns_used 3420 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_min 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_max 0.30 _exptl_crystal_density_diffrn 1.339 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.632 # Sheldrick geometric approximatio 0.89 0.89 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.89 # For a Kappa CCD, set Tmin to 1.0 and # Tmax to the ratio of max:min frame scales in scale_all.log _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_device_type Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _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 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% . _diffrn_ambient_temperature 150 _diffrn_reflns_number 20354 _reflns_number_total 6016 _diffrn_reflns_av_R_equivalents 0.064 # Number of reflections with Friedels Law is 5995 # Number of reflections without Friedels Law is 6016 # Theoretical number of reflections is about 2674 _diffrn_reflns_theta_min 5.172 _diffrn_reflns_theta_max 27.518 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.592 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 33 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min 0 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 32 _oxford_diffrn_Wilson_B_factor 2.37 _oxford_diffrn_Wilson_scale 15.46 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.87 _refine_diff_density_max 1.64 # 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 5123 _refine_ls_number_restraints 0 _refine_ls_number_parameters 353 _oxford_refine_ls_R_factor_ref 0.0536 _refine_ls_wR_factor_ref 0.1055 _refine_ls_goodness_of_fit_ref 0.9797 _refine_ls_shift/su_max 0.001390 # The values computed from all data _oxford_reflns_number_all 5123 _refine_ls_R_factor_all 0.0536 _refine_ls_wR_factor_all 0.1055 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 4476 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_gt 0.0990 # The Flack parameter was determined before Friedel pairs were merged _refine_ls_abs_structure_Flack 0.022(19) _refine_ls_abs_structure_details 'Flack (1983), 0 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^) + ( 0.05P)^2^ + 2.84P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # Insert your own references if required - in alphabetical order _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. 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 0.47673(5) 0.53333(4) 0.546364(19) 0.0295 1.0000 Uani . . . . . . . C2 C 0.4697(4) 0.5184(3) 0.62512(12) 0.0311 1.0000 Uani . . . . . . . C3 C 0.3303(4) 0.5002(3) 0.60372(14) 0.0356 1.0000 Uani . . . . . . . C4 C 0.3383(4) 0.4090(3) 0.56788(14) 0.0326 1.0000 Uani . . . . . . . C5 C 0.4824(4) 0.3694(3) 0.56939(12) 0.0265 1.0000 Uani . . . . . . . C6 C 0.5665(3) 0.4347(3) 0.60521(13) 0.0272 1.0000 Uani . . . . . . . B7 B 0.7142(4) 0.4119(3) 0.63160(14) 0.0279 1.0000 Uani . . . . . . . C8 C 0.7422(3) 0.2975(3) 0.66215(13) 0.0260 1.0000 Uani . . . . . . . C9 C 0.8766(4) 0.2440(3) 0.66224(13) 0.0281 1.0000 Uani . . . . . . . C10 C 0.9005(4) 0.1472(3) 0.69076(13) 0.0306 1.0000 Uani . . . . . . . C11 C 0.7961(4) 0.1003(3) 0.72310(14) 0.0340 1.0000 Uani . . . . . . . C12 C 0.6636(4) 0.1524(3) 0.72366(13) 0.0307 1.0000 Uani . . . . . . . C13 C 0.6332(4) 0.2462(3) 0.69354(13) 0.0285 1.0000 Uani . . . . . . . C14 C 0.4826(4) 0.2905(3) 0.69704(12) 0.0313 1.0000 Uani . . . . . . . C15 C 0.8241(4) -0.0046(3) 0.75552(16) 0.0462 1.0000 Uani . . . . . . . C16 C 0.9991(4) 0.2868(3) 0.62905(14) 0.0381 1.0000 Uani . . . . . . . C17 C 0.8155(3) 0.5181(3) 0.63945(13) 0.0263 1.0000 Uani . . . . . . . C18 C 0.9023(3) 0.5636(3) 0.59950(13) 0.0294 1.0000 Uani . . . . . . . C19 C 0.9230(4) 0.5048(3) 0.54761(14) 0.0370 1.0000 Uani . . . . . . . C20 C 0.9801(4) 0.6621(3) 0.60839(14) 0.0339 1.0000 Uani . . . . . . . C21 C 0.9745(4) 0.7189(3) 0.65552(14) 0.0362 1.0000 Uani . . . . . . . C22 C 0.8885(4) 0.6745(3) 0.69505(14) 0.0335 1.0000 Uani . . . . . . . C23 C 0.8125(4) 0.5752(3) 0.68810(13) 0.0291 1.0000 Uani . . . . . . . C24 C 0.7291(4) 0.5285(3) 0.73402(14) 0.0357 1.0000 Uani . . . . . . . C25 C 1.0616(5) 0.8233(4) 0.66453(19) 0.0576 1.0000 Uani . . . . . . . S26 S 0.54459(12) 0.26423(8) 0.52562(4) 0.0399 1.0000 Uani . . . . . . . O27 O 0.7005(3) 0.2814(2) 0.51771(12) 0.0527 1.0000 Uani . . . . . . . C28 C 0.5291(4) 0.1429(3) 0.56748(13) 0.0343 1.0000 Uani . . . . . . . C29 C 0.3961(4) 0.1081(3) 0.58418(15) 0.0371 1.0000 Uani . . . . . . . C30 C 0.3857(4) 0.0112(3) 0.61428(14) 0.0400 1.0000 Uani . . . . . . . C31 C 0.5067(4) -0.0512(3) 0.62692(13) 0.0382 1.0000 Uani . . . . . . . C32 C 0.6380(4) -0.0150(3) 0.60926(15) 0.0403 1.0000 Uani . . . . . . . C33 C 0.6501(4) 0.0817(3) 0.57924(15) 0.0397 1.0000 Uani . . . . . . . C34 C 0.4935(6) -0.1575(3) 0.65991(16) 0.0548 1.0000 Uani . . . . . . . C35 C 0.6021(5) 0.6632(4) 0.52262(18) 0.0580 1.0000 Uani . . . . . . . C36 C 0.4561(6) 0.6977(3) 0.52407(15) 0.0530 1.0000 Uani . . . . . . . C37 C 0.3807(4) 0.6263(3) 0.48940(16) 0.0428 1.0000 Uani . . . . . . . C38 C 0.4798(4) 0.5520(3) 0.46646(14) 0.0407 1.0000 Uani . . . . . . . C39 C 0.6151(4) 0.5748(4) 0.48664(17) 0.0504 1.0000 Uani . . . . . . . H22 H 0.4957 0.5773 0.6487 0.0379 1.0000 Uiso R . . . . . . H31 H 0.2441 0.5435 0.6115 0.0433 1.0000 Uiso R . . . . . . H41 H 0.2603 0.3783 0.5478 0.0401 1.0000 Uiso R . . . . . . H101 H 0.9882 0.1125 0.6886 0.0374 1.0000 Uiso R . . . . . . H121 H 0.5917 0.1234 0.7449 0.0378 1.0000 Uiso R . . . . . . H143 H 0.4330 0.2511 0.7246 0.0484 1.0000 Uiso R . . . . . . H142 H 0.4852 0.3689 0.7062 0.0483 1.0000 Uiso R . . . . . . H141 H 0.4309 0.2805 0.6646 0.0480 1.0000 Uiso R . . . . . . H151 H 0.7684 0.0001 0.7865 0.0702 1.0000 Uiso R . . . . . . H152 H 0.9225 -0.0118 0.7637 0.0703 1.0000 Uiso R . . . . . . H153 H 0.7935 -0.0686 0.7354 0.0701 1.0000 Uiso R . . . . . . H162 H 1.0826 0.2399 0.6347 0.0579 1.0000 Uiso R . . . . . . H163 H 1.0213 0.3644 0.6379 0.0583 1.0000 Uiso R . . . . . . H161 H 0.9717 0.2840 0.5926 0.0580 1.0000 Uiso R . . . . . . H193 H 0.9266 0.5584 0.5192 0.0558 1.0000 Uiso R . . . . . . H192 H 1.0136 0.4638 0.5473 0.0556 1.0000 Uiso R . . . . . . H191 H 0.8463 0.4515 0.5409 0.0560 1.0000 Uiso R . . . . . . H201 H 1.0378 0.6888 0.5814 0.0411 1.0000 Uiso R . . . . . . H221 H 0.8787 0.7116 0.7263 0.0415 1.0000 Uiso R . . . . . . H241 H 0.7473 0.5769 0.7639 0.0546 1.0000 Uiso R . . . . . . H242 H 0.7594 0.4530 0.7422 0.0548 1.0000 Uiso R . . . . . . H243 H 0.6275 0.5267 0.7258 0.0542 1.0000 Uiso R . . . . . . H252 H 1.1119 0.8180 0.6967 0.0873 1.0000 Uiso R . . . . . . H253 H 1.1286 0.8326 0.6365 0.0877 1.0000 Uiso R . . . . . . H251 H 0.9986 0.8879 0.6654 0.0872 1.0000 Uiso R . . . . . . H291 H 0.3142 0.1494 0.5760 0.0448 1.0000 Uiso R . . . . . . H301 H 0.2960 -0.0123 0.6260 0.0494 1.0000 Uiso R . . . . . . H321 H 0.7188 -0.0552 0.6178 0.0484 1.0000 Uiso R . . . . . . H331 H 0.7370 0.1050 0.5666 0.0466 1.0000 Uiso R . . . . . . H341 H 0.5850 -0.1922 0.6633 0.0843 1.0000 Uiso R . . . . . . H342 H 0.4582 -0.1398 0.6945 0.0842 1.0000 Uiso R . . . . . . H343 H 0.4291 -0.2099 0.6430 0.0845 1.0000 Uiso R . . . . . . H351 H 0.6778 0.6937 0.5434 0.0697 1.0000 Uiso R . . . . . . H361 H 0.4146 0.7577 0.5446 0.0650 1.0000 Uiso R . . . . . . H371 H 0.2761 0.6279 0.4842 0.0513 1.0000 Uiso R . . . . . . H381 H 0.4564 0.4925 0.4413 0.0491 1.0000 Uiso R . . . . . . H391 H 0.7033 0.5337 0.4791 0.0602 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 0.0270(2) 0.0272(2) 0.0342(2) 0.0083(2) -0.0044(2) -0.0014(2) C2 0.0344(17) 0.0274(17) 0.0315(16) 0.0063(14) -0.0025(15) 0.0034(17) C3 0.0285(18) 0.038(2) 0.040(2) 0.0078(16) 0.0024(15) 0.0073(16) C4 0.0240(18) 0.036(2) 0.0375(18) 0.0094(16) -0.0039(14) -0.0031(16) C5 0.0271(17) 0.0224(15) 0.0299(15) 0.0032(13) -0.0016(14) -0.0034(15) C6 0.0289(18) 0.0185(16) 0.0341(18) 0.0034(14) -0.0007(14) -0.0020(13) B7 0.0261(19) 0.030(2) 0.0275(19) 0.0008(17) 0.0023(16) 0.0009(17) C8 0.0257(18) 0.0246(17) 0.0277(16) -0.0033(14) -0.0004(13) -0.0025(14) C9 0.0260(17) 0.0267(18) 0.0317(17) -0.0004(14) -0.0015(14) -0.0001(15) C10 0.0241(18) 0.0269(18) 0.041(2) 0.0027(15) -0.0011(15) 0.0043(15) C11 0.038(2) 0.0279(19) 0.0359(19) 0.0051(15) -0.0006(17) -0.0001(16) C12 0.0307(19) 0.0266(18) 0.0349(18) 0.0026(15) -0.0008(15) -0.0039(16) C13 0.0255(17) 0.0271(18) 0.0328(18) -0.0031(14) 0.0013(14) -0.0061(15) C14 0.0248(17) 0.0335(18) 0.0356(17) 0.0057(14) 0.0024(15) -0.0021(16) C15 0.048(2) 0.037(2) 0.054(2) 0.0194(18) 0.0013(19) 0.0007(18) C16 0.028(2) 0.039(2) 0.0467(19) 0.0107(16) 0.0083(16) 0.0051(16) C17 0.0217(15) 0.0224(17) 0.0348(17) 0.0014(14) -0.0035(13) 0.0020(14) C18 0.0240(17) 0.0266(18) 0.0376(19) 0.0008(14) -0.0059(14) 0.0014(15) C19 0.0365(18) 0.040(2) 0.0341(18) 0.0028(17) -0.0007(16) -0.0025(15) C20 0.0265(17) 0.0319(18) 0.0433(19) 0.0086(15) -0.0010(16) -0.0019(17) C21 0.0319(18) 0.0258(17) 0.051(2) 0.0012(15) -0.0066(18) -0.0028(17) C22 0.036(2) 0.0245(17) 0.040(2) -0.0007(15) -0.0056(16) 0.0010(16) C23 0.0254(18) 0.0257(17) 0.0363(18) 0.0046(15) -0.0039(14) 0.0012(14) C24 0.0380(19) 0.0332(19) 0.0359(19) -0.0023(17) 0.0009(15) 0.0008(18) C25 0.062(3) 0.042(2) 0.069(3) -0.005(2) -0.004(2) -0.023(2) S26 0.0511(6) 0.0313(5) 0.0372(5) 0.0037(4) 0.0086(4) -0.0014(5) O27 0.0515(17) 0.0390(16) 0.0675(18) -0.0020(14) 0.0250(15) -0.0051(14) C28 0.045(2) 0.0252(17) 0.0322(16) -0.0004(14) 0.0000(17) -0.0053(18) C29 0.040(2) 0.0301(19) 0.041(2) 0.0024(17) -0.0060(17) -0.0019(17) C30 0.042(2) 0.039(2) 0.039(2) 0.0056(17) -0.0031(17) -0.0125(18) C31 0.058(3) 0.0276(18) 0.0293(16) 0.0004(13) -0.0036(17) -0.0032(18) C32 0.047(2) 0.035(2) 0.038(2) 0.0004(17) -0.0037(17) 0.0103(18) C33 0.045(2) 0.034(2) 0.040(2) -0.0066(18) 0.0084(17) 0.0032(18) C34 0.084(4) 0.033(2) 0.048(2) 0.0095(17) -0.001(2) -0.001(2) C35 0.060(3) 0.055(3) 0.059(3) 0.032(2) -0.022(2) -0.030(2) C36 0.090(4) 0.0259(18) 0.043(2) 0.0127(17) -0.007(2) 0.003(2) C37 0.039(2) 0.042(2) 0.047(2) 0.0167(18) -0.0045(18) 0.0008(19) C38 0.043(2) 0.043(2) 0.0358(19) 0.0149(15) 0.0014(16) 0.0002(19) C39 0.036(2) 0.057(3) 0.058(3) 0.024(2) 0.0017(19) -0.002(2) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2602(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Fe1 . C2 . 2.024(3) yes Fe1 . C3 . 2.047(4) yes Fe1 . C4 . 2.038(4) yes Fe1 . C5 . 2.030(3) yes Fe1 . C6 . 2.083(3) yes Fe1 . C35 . 2.028(4) yes Fe1 . C36 . 2.038(4) yes Fe1 . C37 . 2.036(4) yes Fe1 . C38 . 2.056(3) yes Fe1 . C39 . 2.063(4) yes C2 . C3 . 1.432(5) yes C2 . C6 . 1.437(5) yes C2 . H22 . 0.954 no C3 . C4 . 1.418(5) yes C3 . H31 . 0.978 no C4 . C5 . 1.430(5) yes C4 . H41 . 0.965 no C5 . C6 . 1.435(5) yes C5 . S26 . 1.773(3) yes C6 . B7 . 1.564(5) yes B7 . C8 . 1.585(5) yes B7 . C17 . 1.589(5) yes C8 . C9 . 1.410(5) yes C8 . C13 . 1.435(5) yes C9 . C10 . 1.377(5) yes C9 . C16 . 1.515(5) yes C10 . C11 . 1.397(5) yes C10 . H101 . 0.921 no C11 . C12 . 1.386(5) yes C11 . C15 . 1.517(5) yes C12 . C13 . 1.382(5) yes C12 . H121 . 0.932 no C13 . C14 . 1.509(5) yes C14 . H143 . 0.965 no C14 . H142 . 0.957 no C14 . H141 . 0.968 no C15 . H151 . 0.949 no C15 . H152 . 0.949 no C15 . H153 . 0.960 no C16 . H162 . 0.970 no C16 . H163 . 0.970 no C16 . H161 . 0.968 no C17 . C18 . 1.413(5) yes C17 . C23 . 1.417(5) yes C18 . C19 . 1.512(5) yes C18 . C20 . 1.395(5) yes C19 . H193 . 0.966 no C19 . H192 . 0.978 no C19 . H191 . 0.972 no C20 . C21 . 1.381(5) yes C20 . H201 . 0.931 no C21 . C22 . 1.396(5) yes C21 . C25 . 1.500(5) yes C22 . C23 . 1.386(5) yes C22 . H221 . 0.917 no C23 . C24 . 1.516(5) yes C24 . H241 . 0.971 no C24 . H242 . 0.962 no C24 . H243 . 0.975 no C25 . H252 . 0.950 no C25 . H253 . 0.959 no C25 . H251 . 0.966 no S26 . O27 . 1.489(3) yes S26 . C28 . 1.798(3) yes C28 . C29 . 1.381(5) yes C28 . C33 . 1.379(5) yes C29 . C30 . 1.385(5) yes C29 . H291 . 0.934 no C30 . C31 . 1.391(5) yes C30 . H301 . 0.935 no C31 . C32 . 1.379(5) yes C31 . C34 . 1.521(5) yes C32 . C33 . 1.383(5) yes C32 . H321 . 0.920 no C33 . H331 . 0.919 no C34 . H341 . 0.955 no C34 . H342 . 0.968 no C34 . H343 . 0.969 no C35 . C36 . 1.429(7) yes C35 . C39 . 1.399(7) yes C35 . H351 . 0.958 no C36 . C37 . 1.415(6) yes C36 . H361 . 0.965 no C37 . C38 . 1.407(6) yes C37 . H371 . 0.989 no C38 . C39 . 1.395(6) yes C38 . H381 . 0.979 no C39 . H391 . 0.978 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 . 41.20(14) yes C2 . Fe1 . C4 . 69.33(14) yes C3 . Fe1 . C4 . 40.64(15) yes C2 . Fe1 . C5 . 68.17(13) yes C3 . Fe1 . C5 . 68.04(14) yes C4 . Fe1 . C5 . 41.17(14) yes C2 . Fe1 . C6 . 40.93(13) yes C3 . Fe1 . C6 . 69.21(13) yes C4 . Fe1 . C6 . 69.93(13) yes C5 . Fe1 . C6 . 40.82(13) yes C2 . Fe1 . C35 . 112.55(17) yes C3 . Fe1 . C35 . 138.45(19) yes C4 . Fe1 . C35 . 175.78(17) yes C5 . Fe1 . C35 . 142.84(18) yes C6 . Fe1 . C35 . 114.06(15) yes C2 . Fe1 . C36 . 111.06(15) yes C3 . Fe1 . C36 . 108.67(17) yes C4 . Fe1 . C36 . 134.85(18) yes C5 . Fe1 . C36 . 176.01(19) yes C6 . Fe1 . C36 . 140.93(16) yes C2 . Fe1 . C37 . 138.21(16) yes C3 . Fe1 . C37 . 108.69(15) yes C4 . Fe1 . C37 . 107.60(15) yes C5 . Fe1 . C37 . 137.43(15) yes C6 . Fe1 . C37 . 177.49(15) yes C2 . Fe1 . C38 . 178.43(14) yes C3 . Fe1 . C38 . 137.95(15) yes C4 . Fe1 . C38 . 110.80(15) yes C5 . Fe1 . C38 . 113.02(14) yes C6 . Fe1 . C38 . 140.65(14) yes C2 . Fe1 . C39 . 141.14(16) yes C3 . Fe1 . C39 . 176.17(16) yes C4 . Fe1 . C39 . 140.53(18) yes C5 . Fe1 . C39 . 115.22(17) yes C6 . Fe1 . C39 . 114.51(15) yes C35 . Fe1 . C36 . 41.14(19) yes C35 . Fe1 . C37 . 68.40(17) yes C36 . Fe1 . C37 . 40.65(17) yes C35 . Fe1 . C38 . 67.21(17) yes C36 . Fe1 . C38 . 67.68(16) yes C37 . Fe1 . C38 . 40.22(16) yes C35 . Fe1 . C39 . 39.99(19) yes C36 . Fe1 . C39 . 67.98(19) yes C37 . Fe1 . C39 . 67.61(17) yes C38 . Fe1 . C39 . 39.60(16) yes Fe1 . C2 . C3 . 70.26(19) yes Fe1 . C2 . C6 . 71.76(19) yes C3 . C2 . C6 . 109.7(3) yes Fe1 . C2 . H22 . 123.9 no C3 . C2 . H22 . 125.8 no C6 . C2 . H22 . 124.6 no C2 . C3 . Fe1 . 68.54(19) yes C2 . C3 . C4 . 108.3(3) yes Fe1 . C3 . C4 . 69.4(2) yes C2 . C3 . H31 . 126.7 no Fe1 . C3 . H31 . 126.9 no C4 . C3 . H31 . 125.1 no C3 . C4 . Fe1 . 70.0(2) yes C3 . C4 . C5 . 106.4(3) yes Fe1 . C4 . C5 . 69.10(18) yes C3 . C4 . H41 . 126.3 no Fe1 . C4 . H41 . 127.6 no C5 . C4 . H41 . 127.3 no C4 . C5 . Fe1 . 69.73(19) yes C4 . C5 . C6 . 111.0(3) yes Fe1 . C5 . C6 . 71.60(18) yes C4 . C5 . S26 . 121.6(3) yes Fe1 . C5 . S26 . 119.81(16) yes C6 . C5 . S26 . 126.9(3) yes C2 . C6 . C5 . 104.5(3) yes C2 . C6 . Fe1 . 67.31(17) yes C5 . C6 . Fe1 . 67.59(18) yes C2 . C6 . B7 . 121.7(3) yes C5 . C6 . B7 . 132.0(3) yes Fe1 . C6 . B7 . 140.1(2) yes C6 . B7 . C8 . 120.5(3) yes C6 . B7 . C17 . 116.5(3) yes C8 . B7 . C17 . 121.0(3) yes B7 . C8 . C9 . 122.2(3) yes B7 . C8 . C13 . 121.4(3) yes C9 . C8 . C13 . 116.4(3) yes C8 . C9 . C10 . 121.4(3) yes C8 . C9 . C16 . 121.7(3) yes C10 . C9 . C16 . 116.8(3) yes C9 . C10 . C11 . 122.0(3) yes C9 . C10 . H101 . 119.0 no C11 . C10 . H101 . 119.0 no C10 . C11 . C12 . 117.2(3) yes C10 . C11 . C15 . 121.9(3) yes C12 . C11 . C15 . 120.9(3) yes C11 . C12 . C13 . 122.5(3) yes C11 . C12 . H121 . 119.3 no C13 . C12 . H121 . 118.2 no C8 . C13 . C12 . 120.4(3) yes C8 . C13 . C14 . 123.5(3) yes C12 . C13 . C14 . 116.1(3) yes C13 . C14 . H143 . 109.0 no C13 . C14 . H142 . 109.1 no H143 . C14 . H142 . 107.6 no C13 . C14 . H141 . 112.0 no H143 . C14 . H141 . 109.1 no H142 . C14 . H141 . 110.0 no C11 . C15 . H151 . 108.2 no C11 . C15 . H152 . 111.2 no H151 . C15 . H152 . 110.9 no C11 . C15 . H153 . 107.6 no H151 . C15 . H153 . 109.2 no H152 . C15 . H153 . 109.7 no C9 . C16 . H162 . 109.7 no C9 . C16 . H163 . 110.4 no H162 . C16 . H163 . 109.6 no C9 . C16 . H161 . 109.1 no H162 . C16 . H161 . 109.7 no H163 . C16 . H161 . 108.3 no B7 . C17 . C18 . 123.7(3) yes B7 . C17 . C23 . 118.5(3) yes C18 . C17 . C23 . 117.7(3) yes C17 . C18 . C19 . 122.2(3) yes C17 . C18 . C20 . 120.1(3) yes C19 . C18 . C20 . 117.5(3) yes C18 . C19 . H193 . 111.2 no C18 . C19 . H192 . 110.4 no H193 . C19 . H192 . 106.8 no C18 . C19 . H191 . 111.0 no H193 . C19 . H191 . 108.7 no H192 . C19 . H191 . 108.6 no C18 . C20 . C21 . 122.0(3) yes C18 . C20 . H201 . 117.8 no C21 . C20 . H201 . 120.2 no C20 . C21 . C22 . 118.1(3) yes C20 . C21 . C25 . 121.0(4) yes C22 . C21 . C25 . 120.9(3) yes C21 . C22 . C23 . 121.5(3) yes C21 . C22 . H221 . 120.6 no C23 . C22 . H221 . 117.8 no C17 . C23 . C22 . 120.5(3) yes C17 . C23 . C24 . 121.1(3) yes C22 . C23 . C24 . 118.3(3) yes C23 . C24 . H241 . 107.8 no C23 . C24 . H242 . 110.9 no H241 . C24 . H242 . 108.9 no C23 . C24 . H243 . 110.1 no H241 . C24 . H243 . 110.8 no H242 . C24 . H243 . 108.3 no C21 . C25 . H252 . 110.3 no C21 . C25 . H253 . 109.6 no H252 . C25 . H253 . 109.3 no C21 . C25 . H251 . 108.9 no H252 . C25 . H251 . 109.7 no H253 . C25 . H251 . 109.0 no C5 . S26 . O27 . 108.20(16) yes C5 . S26 . C28 . 99.12(15) yes O27 . S26 . C28 . 105.63(18) yes S26 . C28 . C29 . 119.7(3) yes S26 . C28 . C33 . 118.9(3) yes C29 . C28 . C33 . 121.2(3) yes C28 . C29 . C30 . 118.8(4) yes C28 . C29 . H291 . 121.1 no C30 . C29 . H291 . 120.1 no C29 . C30 . C31 . 120.8(4) yes C29 . C30 . H301 . 119.2 no C31 . C30 . H301 . 120.0 no C30 . C31 . C32 . 119.1(3) yes C30 . C31 . C34 . 120.2(4) yes C32 . C31 . C34 . 120.7(4) yes C31 . C32 . C33 . 120.8(4) yes C31 . C32 . H321 . 119.7 no C33 . C32 . H321 . 119.5 no C32 . C33 . C28 . 119.3(4) yes C32 . C33 . H331 . 121.2 no C28 . C33 . H331 . 119.6 no C31 . C34 . H341 . 109.5 no C31 . C34 . H342 . 110.8 no H341 . C34 . H342 . 108.5 no C31 . C34 . H343 . 109.5 no H341 . C34 . H343 . 109.0 no H342 . C34 . H343 . 109.5 no Fe1 . C35 . C36 . 69.8(2) yes Fe1 . C35 . C39 . 71.4(2) yes C36 . C35 . C39 . 108.3(4) yes Fe1 . C35 . H351 . 123.3 no C36 . C35 . H351 . 125.9 no C39 . C35 . H351 . 125.7 no C35 . C36 . Fe1 . 69.1(2) yes C35 . C36 . C37 . 106.9(4) yes Fe1 . C36 . C37 . 69.6(2) yes C35 . C36 . H361 . 127.6 no Fe1 . C36 . H361 . 126.1 no C37 . C36 . H361 . 125.4 no C36 . C37 . Fe1 . 69.7(2) yes C36 . C37 . C38 . 107.8(4) yes Fe1 . C37 . C38 . 70.7(2) yes C36 . C37 . H371 . 124.6 no Fe1 . C37 . H371 . 123.0 no C38 . C37 . H371 . 127.6 no C37 . C38 . Fe1 . 69.1(2) yes C37 . C38 . C39 . 108.9(4) yes Fe1 . C38 . C39 . 70.5(2) yes C37 . C38 . H381 . 125.2 no Fe1 . C38 . H381 . 125.0 no C39 . C38 . H381 . 125.8 no Fe1 . C39 . C35 . 68.7(2) yes Fe1 . C39 . C38 . 69.9(2) yes C35 . C39 . C38 . 108.0(4) yes Fe1 . C39 . H391 . 124.0 no C35 . C39 . H391 . 125.1 no C38 . C39 . H391 . 126.8 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C4 . H41 . O27 2_456 142 0.97 2.59 3.398(5) yes C19 . H191 . O27 . 165 0.97 2.50 3.454(5) yes _chemical_name_common .