# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email simon.aldridge@chem.ox.ac.uk _publ_contact_author_name 'Simon Aldridge' loop_ _publ_author_name 'Inke Siewert' 'Philip Fitzpatrick' 'Alexander E.J. Broomsgrove' 'Michael Kelly' 'Dragoslav Vidovic' 'Simon Aldridge' data_041pfdv10 _database_code_depnum_ccdc_archive 'CCDC 809729' #TrackingRef '041pfdv10.cif' _audit_creation_date 10-05-07 _audit_creation_method CRYSTALS_ver_14.03 _oxford_structure_analysis_title 041fpdv10 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 15.3409(6) _cell_length_b 7.4354(3) _cell_length_c 16.5260(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1885.05(13) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall ? 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 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' _cell_formula_units_Z 4 # Given Formula = C24 B1 Fe1 # Dc = 1.25 Fooo = 792.00 Mu = 8.01 M = 354.92 # Found Formula = C24 H23 B1 Fe1 # Dc = 1.33 FOOO = 792.00 Mu = 8.04 M = 378.10 _chemical_formula_sum 'C24 H23 B1 Fe1' _chemical_formula_moiety 'C24 H23 B1 Fe1' _chemical_compound_source ? _chemical_formula_weight 378.10 _cell_measurement_reflns_used 2380 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_min 0.070 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.130 _exptl_crystal_density_diffrn 1.332 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.804 # Sheldrick geometric approximatio 0.92 0.95 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.95 # 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_measurement_device 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, 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 13079 _reflns_number_total 2211 _diffrn_reflns_av_R_equivalents 0.000 # Number of reflections without Friedels Law is 2211 # Number of reflections with Friedels Law is 2211 # Theoretical number of reflections is about 2159 _diffrn_reflns_theta_min 5.319 _diffrn_reflns_theta_max 27.470 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.920 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _reflns_limit_h_min 0 _reflns_limit_h_max 19 _reflns_limit_k_min 0 _reflns_limit_k_max 9 _reflns_limit_l_min -21 _reflns_limit_l_max 0 _oxford_diffrn_Wilson_B_factor 3.49 _oxford_diffrn_Wilson_scale 3.94 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.46 _refine_diff_density_max 0.56 # 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 1623 _refine_ls_number_restraints 330 _refine_ls_number_parameters 236 _oxford_refine_ls_R_factor_ref 0.0488 _refine_ls_wR_factor_ref 0.1183 _refine_ls_goodness_of_fit_ref 0.9742 _refine_ls_shift/su_max 0.0006546 _refine_ls_shift/su_mean 0.5636141 # The values computed from all data _oxford_reflns_number_all 1623 _refine_ls_R_factor_all 0.0488 _refine_ls_wR_factor_all 0.1183 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 1459 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_gt 0.1130 _refine_ls_abs_structure_Flack 0.45(8) _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 none # 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^) + ( 0.08P)^2^ + 1.20P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; # 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. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. 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 Fe1 Fe 0.63273(4) 0.73013(7) 0.12926(19) 0.0463 1.0000 Uani . . . . . . . C2 C 0.6211(4) 0.9832(7) 0.0817(4) 0.0570 1.0000 Uani . . . . . . . C3 C 0.5773(4) 0.9748(8) 0.1562(3) 0.0547 1.0000 Uani . . . . . . . C4 C 0.5140(4) 0.8408(9) 0.1501(4) 0.0716 1.0000 Uani . . . . . . . C5 C 0.5167(4) 0.7680(9) 0.0709(5) 0.0778 1.0000 Uani . . . . . . . C6 C 0.5834(4) 0.8575(8) 0.0286(4) 0.0676 1.0000 Uani . . . . . . . C7 C 0.6483(4) 0.4581(6) 0.1281(6) 0.0665 1.0000 Uani . . . . . . . C8 C 0.7166(4) 0.5418(8) 0.0834(4) 0.0652 1.0000 Uani . . . . . . . C9 C 0.7611(3) 0.6600(6) 0.1364(4) 0.0528 1.0000 Uani . . . . . . . C10 C 0.7210(3) 0.6497(6) 0.2156(3) 0.0485 1.0000 Uani . . . . . . . C11 C 0.6499(4) 0.5215(7) 0.2062(3) 0.0547 1.0000 Uani . . . . . . . B12 B 0.7380(4) 0.7722(7) 0.2877(4) 0.0469 1.0000 Uani . . . . . . . C13 C 0.8094(3) 0.9248(7) 0.2857(3) 0.0471 1.0000 Uani . . . . . . . C14 C 0.8832(3) 0.9229(7) 0.3361(3) 0.0498 1.0000 Uani . . . . . . . C15 C 0.9011(5) 0.7644(9) 0.3898(5) 0.0793 1.0000 Uani . . . . . . . C16 C 0.9405(4) 1.0647(8) 0.3354(3) 0.0620 1.0000 Uani . . . . . . . C17 C 0.9259(4) 1.2141(7) 0.2872(4) 0.0626 1.0000 Uani . . . . . . . C18 C 0.8565(5) 1.2207(8) 0.2368(5) 0.0649 1.0000 Uani . . . . . . . C19 C 0.7985(4) 1.0764(7) 0.2359(4) 0.0590 1.0000 Uani . . . . . . . C20 C 0.6899(4) 0.7271(8) 0.3699(4) 0.0595 1.0000 Uani . . . . . . . C21 C 0.6471(4) 0.8428(9) 0.4197(4) 0.0707 1.0000 Uani . . . . . . . C22 C 0.6127(5) 0.7925(14) 0.4977(5) 0.0819 1.0000 Uani . . . . . . . C23 C 0.6287(4) 0.6248(12) 0.5210(5) 0.0816 1.0000 Uani . . . . . . . C24 C 0.6702(6) 0.4912(11) 0.4753(5) 0.0883 1.0000 Uani . . . . . . . C25 C 0.6992(4) 0.5395(10) 0.4010(4) 0.0782 1.0000 Uani . . . . . . . C26 C 0.6338(5) 1.0238(10) 0.3927(4) 0.0800 1.0000 Uani . . . . . . . H21 H 0.6670 1.0705 0.0684 0.0667 1.0000 Uiso R . . . . . . H31 H 0.5896 1.0459 0.2038 0.0676 1.0000 Uiso R . . . . . . H41 H 0.4730 0.8078 0.1929 0.0831 1.0000 Uiso R . . . . . . H51 H 0.4786 0.6735 0.0490 0.0882 1.0000 Uiso R . . . . . . H61 H 0.6035 0.8305 -0.0266 0.0823 1.0000 Uiso R . . . . . . H71 H 0.6055 0.3724 0.1068 0.0821 1.0000 Uiso R . . . . . . H81 H 0.7317 0.5126 0.0270 0.0767 1.0000 Uiso R . . . . . . H91 H 0.8097 0.7422 0.1217 0.0643 1.0000 Uiso R . . . . . . H111 H 0.6081 0.4883 0.2491 0.0631 1.0000 Uiso R . . . . . . H151 H 0.9591 0.7702 0.4118 0.1170 1.0000 Uiso R . . . . . . H152 H 0.8956 0.6574 0.3579 0.1171 1.0000 Uiso R . . . . . . H153 H 0.8595 0.7614 0.4332 0.1170 1.0000 Uiso R . . . . . . H161 H 0.9897 1.0623 0.3681 0.0732 1.0000 Uiso R . . . . . . H171 H 0.9657 1.3083 0.2886 0.0681 1.0000 Uiso R . . . . . . H181 H 0.8466 1.3190 0.2047 0.0705 1.0000 Uiso R . . . . . . H191 H 0.7518 1.0797 0.2004 0.0730 1.0000 Uiso R . . . . . . H221 H 0.5819 0.8753 0.5294 0.0919 1.0000 Uiso R . . . . . . H231 H 0.6106 0.5913 0.5726 0.0943 1.0000 Uiso R . . . . . . H241 H 0.6766 0.3741 0.4947 0.1011 1.0000 Uiso R . . . . . . H251 H 0.7259 0.4552 0.3679 0.0855 1.0000 Uiso R . . . . . . H261 H 0.5999 1.0865 0.4326 0.1272 1.0000 Uiso R . . . . . . H262 H 0.6895 1.0813 0.3862 0.1270 1.0000 Uiso R . . . . . . H263 H 0.6037 1.0224 0.3419 0.1270 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 0.0515(4) 0.0368(3) 0.0507(4) -0.0041(5) 0.0030(5) -0.0040(3) C2 0.064(3) 0.037(2) 0.070(3) -0.002(2) -0.004(3) 0.001(2) C3 0.053(3) 0.048(3) 0.063(3) -0.007(2) -0.004(2) 0.014(2) C4 0.054(3) 0.080(4) 0.081(4) 0.009(3) 0.011(3) 0.002(3) C5 0.062(3) 0.072(4) 0.099(5) 0.004(3) -0.024(3) -0.015(3) C6 0.084(3) 0.058(3) 0.061(3) -0.004(3) -0.011(3) 0.007(3) C7 0.085(3) 0.0314(19) 0.084(3) -0.005(4) -0.012(4) -0.005(2) C8 0.079(3) 0.050(3) 0.067(3) -0.016(3) 0.009(3) 0.010(3) C9 0.054(2) 0.043(2) 0.062(3) 0.001(3) 0.009(3) 0.0053(18) C10 0.055(2) 0.034(2) 0.056(3) 0.002(2) 0.005(2) 0.003(2) C11 0.065(3) 0.035(2) 0.065(3) 0.000(2) 0.007(3) -0.008(2) B12 0.042(3) 0.040(3) 0.058(3) 0.016(2) -0.004(2) 0.009(2) C13 0.049(3) 0.045(3) 0.047(2) 0.003(2) 0.003(2) 0.003(2) C14 0.047(2) 0.052(3) 0.050(3) 0.001(2) -0.002(2) 0.006(2) C15 0.057(3) 0.098(4) 0.083(4) 0.036(3) -0.014(3) 0.004(3) C16 0.050(3) 0.081(4) 0.055(3) -0.004(3) -0.005(2) -0.011(3) C17 0.071(3) 0.051(3) 0.066(3) -0.007(3) 0.009(3) -0.017(3) C18 0.074(4) 0.045(3) 0.076(4) 0.013(3) 0.002(3) -0.001(3) C19 0.058(3) 0.051(3) 0.068(3) 0.012(3) -0.012(3) -0.007(2) C20 0.046(3) 0.078(3) 0.054(3) 0.000(3) -0.006(2) -0.007(2) C21 0.068(3) 0.074(4) 0.070(4) -0.006(3) -0.011(3) -0.006(3) C22 0.077(4) 0.118(5) 0.050(3) 0.017(4) -0.015(3) -0.042(4) C23 0.088(4) 0.083(5) 0.074(4) -0.028(4) -0.013(3) -0.015(3) C24 0.105(4) 0.069(4) 0.091(4) 0.019(4) -0.028(4) -0.038(4) C25 0.073(3) 0.100(4) 0.062(3) 0.019(3) -0.007(3) -0.033(3) C26 0.083(4) 0.089(4) 0.068(4) 0.004(3) -0.007(3) -0.002(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5395(18) 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 . 2.047(6) yes Fe1 . C3 . 2.057(5) yes Fe1 . C4 . 2.029(6) yes Fe1 . C5 . 2.044(7) yes Fe1 . C6 . 2.058(7) yes Fe1 . C7 . 2.037(4) yes Fe1 . C8 . 2.047(5) yes Fe1 . C9 . 2.041(5) yes Fe1 . C10 . 2.057(6) yes Fe1 . C11 . 2.023(6) yes C2 . C3 . 1.403(8) yes C2 . C6 . 1.407(8) yes C2 . H21 . 0.983 no C3 . C4 . 1.396(9) yes C3 . H31 . 0.965 no C4 . C5 . 1.417(10) yes C4 . H41 . 0.978 no C5 . C6 . 1.406(10) yes C5 . H51 . 0.983 no C6 . H61 . 0.984 no C7 . C8 . 1.426(9) yes C7 . C11 . 1.373(10) yes C7 . H71 . 0.980 no C8 . C9 . 1.416(8) yes C8 . H81 . 0.984 no C9 . C10 . 1.448(8) yes C9 . H91 . 0.994 no C10 . C11 . 1.457(7) yes C10 . B12 . 1.521(8) yes C11 . H111 . 0.988 no B12 . C13 . 1.578(8) yes B12 . C20 . 1.582(8) yes C13 . C14 . 1.406(7) yes C13 . C19 . 1.405(7) yes C14 . C15 . 1.500(8) yes C14 . C16 . 1.373(8) yes C15 . H151 . 0.963 no C15 . H152 . 0.958 no C15 . H153 . 0.960 no C16 . C17 . 1.384(9) yes C16 . H161 . 0.930 no C17 . C18 . 1.352(11) yes C17 . H171 . 0.929 no C18 . C19 . 1.394(8) yes C18 . H181 . 0.916 no C19 . H191 . 0.927 no C20 . C21 . 1.359(9) yes C20 . C25 . 1.494(9) yes C21 . C22 . 1.442(10) yes C21 . C26 . 1.433(10) yes C22 . C23 . 1.328(12) yes C22 . H221 . 0.937 no C23 . C24 . 1.401(12) yes C23 . H231 . 0.931 no C24 . C25 . 1.354(10) yes C24 . H241 . 0.933 no C25 . H251 . 0.928 no C26 . H261 . 0.960 no C26 . H262 . 0.961 no C26 . H263 . 0.958 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 . 40.0(2) yes C2 . Fe1 . C4 . 67.3(3) yes C3 . Fe1 . C4 . 39.9(2) yes C2 . Fe1 . C5 . 67.4(2) yes C3 . Fe1 . C5 . 67.7(3) yes C4 . Fe1 . C5 . 40.7(3) yes C2 . Fe1 . C6 . 40.1(2) yes C3 . Fe1 . C6 . 67.4(2) yes C4 . Fe1 . C6 . 67.7(3) yes C5 . Fe1 . C6 . 40.1(3) yes C2 . Fe1 . C7 . 156.9(4) yes C3 . Fe1 . C7 . 158.2(3) yes C4 . Fe1 . C7 . 120.6(3) yes C5 . Fe1 . C7 . 103.6(3) yes C6 . Fe1 . C7 . 119.5(3) yes C2 . Fe1 . C8 . 122.8(3) yes C3 . Fe1 . C8 . 160.9(3) yes C4 . Fe1 . C8 . 154.8(3) yes C5 . Fe1 . C8 . 117.8(3) yes C6 . Fe1 . C8 . 104.3(3) yes C2 . Fe1 . C9 . 110.0(2) yes C3 . Fe1 . C9 . 127.7(2) yes C4 . Fe1 . C9 . 163.9(3) yes C5 . Fe1 . C9 . 154.5(3) yes C6 . Fe1 . C9 . 121.3(3) yes C2 . Fe1 . C10 . 126.2(2) yes C3 . Fe1 . C10 . 112.3(2) yes C4 . Fe1 . C10 . 126.3(3) yes C5 . Fe1 . C10 . 160.2(3) yes C6 . Fe1 . C10 . 159.5(2) yes C2 . Fe1 . C11 . 163.2(3) yes C3 . Fe1 . C11 . 126.6(3) yes C4 . Fe1 . C11 . 108.8(3) yes C5 . Fe1 . C11 . 121.0(3) yes C6 . Fe1 . C11 . 155.3(3) yes C7 . Fe1 . C8 . 40.9(3) yes C7 . Fe1 . C9 . 68.5(2) yes C8 . Fe1 . C9 . 40.5(2) yes C7 . Fe1 . C10 . 68.9(3) yes C8 . Fe1 . C10 . 69.1(2) yes C9 . Fe1 . C10 . 41.4(2) yes C7 . Fe1 . C11 . 39.5(3) yes C8 . Fe1 . C11 . 68.1(2) yes C9 . Fe1 . C11 . 69.0(2) yes C10 . Fe1 . C11 . 41.8(2) yes Fe1 . C2 . C3 . 70.4(4) yes Fe1 . C2 . C6 . 70.4(3) yes C3 . C2 . C6 . 108.7(5) yes Fe1 . C2 . H21 . 129.1 no C3 . C2 . H21 . 124.6 no C6 . C2 . H21 . 126.5 no C2 . C3 . Fe1 . 69.6(3) yes C2 . C3 . C4 . 107.5(5) yes Fe1 . C3 . C4 . 68.9(3) yes C2 . C3 . H31 . 126.6 no Fe1 . C3 . H31 . 125.5 no C4 . C3 . H31 . 125.9 no C3 . C4 . Fe1 . 71.1(3) yes C3 . C4 . C5 . 108.6(6) yes Fe1 . C4 . C5 . 70.2(4) yes C3 . C4 . H41 . 125.1 no Fe1 . C4 . H41 . 126.7 no C5 . C4 . H41 . 126.2 no C4 . C5 . Fe1 . 69.1(4) yes C4 . C5 . C6 . 107.4(5) yes Fe1 . C5 . C6 . 70.5(4) yes C4 . C5 . H51 . 126.6 no Fe1 . C5 . H51 . 126.4 no C6 . C5 . H51 . 126.0 no C2 . C6 . C5 . 107.7(6) yes C2 . C6 . Fe1 . 69.5(3) yes C5 . C6 . Fe1 . 69.4(4) yes C2 . C6 . H61 . 125.8 no C5 . C6 . H61 . 126.3 no Fe1 . C6 . H61 . 122.7 no Fe1 . C7 . C8 . 70.0(3) yes Fe1 . C7 . C11 . 69.7(3) yes C8 . C7 . C11 . 108.9(5) yes Fe1 . C7 . H71 . 124.8 no C8 . C7 . H71 . 126.1 no C11 . C7 . H71 . 125.0 no C7 . C8 . Fe1 . 69.2(3) yes C7 . C8 . C9 . 107.7(5) yes Fe1 . C8 . C9 . 69.5(3) yes C7 . C8 . H81 . 124.6 no Fe1 . C8 . H81 . 130.5 no C9 . C8 . H81 . 127.5 no C8 . C9 . Fe1 . 70.0(3) yes C8 . C9 . C10 . 108.8(5) yes Fe1 . C9 . C10 . 69.9(3) yes C8 . C9 . H91 . 126.2 no Fe1 . C9 . H91 . 123.5 no C10 . C9 . H91 . 124.9 no C9 . C10 . Fe1 . 68.7(3) yes C9 . C10 . C11 . 104.8(4) yes Fe1 . C10 . C11 . 67.8(3) yes C9 . C10 . B12 . 127.1(4) yes Fe1 . C10 . B12 . 118.8(3) yes C11 . C10 . B12 . 127.1(5) yes C10 . C11 . C7 . 109.8(5) yes C10 . C11 . Fe1 . 70.3(3) yes C7 . C11 . Fe1 . 70.8(3) yes C10 . C11 . H111 . 125.0 no C7 . C11 . H111 . 125.2 no Fe1 . C11 . H111 . 123.9 no C10 . B12 . C13 . 122.3(5) yes C10 . B12 . C20 . 117.7(4) yes C13 . B12 . C20 . 119.6(5) yes B12 . C13 . C14 . 122.7(5) yes B12 . C13 . C19 . 120.4(5) yes C14 . C13 . C19 . 116.8(5) yes C13 . C14 . C15 . 120.3(5) yes C13 . C14 . C16 . 120.2(5) yes C15 . C14 . C16 . 119.5(5) yes C14 . C15 . H151 . 110.9 no C14 . C15 . H152 . 108.1 no H151 . C15 . H152 . 109.1 no C14 . C15 . H153 . 109.8 no H151 . C15 . H153 . 109.4 no H152 . C15 . H153 . 109.5 no C14 . C16 . C17 . 121.2(5) yes C14 . C16 . H161 . 120.0 no C17 . C16 . H161 . 118.8 no C16 . C17 . C18 . 120.7(5) yes C16 . C17 . H171 . 119.1 no C18 . C17 . H171 . 120.2 no C17 . C18 . C19 . 118.8(6) yes C17 . C18 . H181 . 121.1 no C19 . C18 . H181 . 120.1 no C13 . C19 . C18 . 122.4(6) yes C13 . C19 . H191 . 118.9 no C18 . C19 . H191 . 118.7 no B12 . C20 . C21 . 127.7(6) yes B12 . C20 . C25 . 116.7(5) yes C21 . C20 . C25 . 115.4(6) yes C20 . C21 . C22 . 123.6(8) yes C20 . C21 . C26 . 118.3(7) yes C22 . C21 . C26 . 118.0(7) yes C21 . C22 . C23 . 115.8(9) yes C21 . C22 . H221 . 121.0 no C23 . C22 . H221 . 123.3 no C22 . C23 . C24 . 126.4(8) yes C22 . C23 . H231 . 117.5 no C24 . C23 . H231 . 116.1 no C23 . C24 . C25 . 116.7(8) yes C23 . C24 . H241 . 121.6 no C25 . C24 . H241 . 121.7 no C20 . C25 . C24 . 121.9(8) yes C20 . C25 . H251 . 118.0 no C24 . C25 . H251 . 120.0 no C21 . C26 . H261 . 108.6 no C21 . C26 . H262 . 109.0 no H261 . C26 . H262 . 109.9 no C21 . C26 . H263 . 109.4 no H261 . C26 . H263 . 110.2 no H262 . C26 . H263 . 109.6 no # Attachment '047pfdv10.cif' data_047pfdv10 _database_code_depnum_ccdc_archive 'CCDC 809730' #TrackingRef '047pfdv10.cif' _audit_creation_date 10-05-21 _audit_creation_method CRYSTALS_ver_14.03 _oxford_structure_analysis_title 047pfdv10 _chemical_name_systematic . _chemical_melting_point . _cell_length_a 8.55170(10) _cell_length_b 22.6990(3) _cell_length_c 10.3460(2) _cell_angle_alpha 90 _cell_angle_beta 101.3943(5) _cell_angle_gamma 90 _cell_volume 1968.73(5) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall 'P 2yb' 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' 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' 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' F 0.0171 0.0103 3.5392 10.2825 2.6412 4.2944 1.5170 0.2615 1.0243 26.1476 0.2776 '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' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C41 H50 B1 Cl3 F1 Fe1 K1 O6 # Dc = 1.47 Fooo = 856.00 Mu = 7.45 M = 869.96 # Found Formula = C37 H48 B1 Cl3 F1 Fe1 K1 O6 # Dc = 1.38 FOOO = 856.00 Mu = 7.40 M = 819.90 _chemical_formula_sum 'C37 H48 B1 Cl3 F1 Fe1 K1 O6' _chemical_formula_moiety 'C36 H47 B F Fe K O6, C H Cl3' _chemical_compound_source . _chemical_formula_weight 819.90 _cell_measurement_reflns_used 7329 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.330 _exptl_crystal_size_mid 0.430 _exptl_crystal_size_max 0.500 _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 0.740 # Sheldrick geometric approximatio 0.73 0.78 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.69 _exptl_absorpt_correction_T_max 0.78 # 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_measurement_device 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, 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 27162 _reflns_number_total 8428 _diffrn_reflns_av_R_equivalents 0.050 # Number of reflections without Friedels Law is 8428 # Number of reflections with Friedels Law is 4541 # Theoretical number of reflections is about 4478 _diffrn_reflns_theta_min 5.107 _diffrn_reflns_theta_max 27.401 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 26.853 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _reflns_limit_h_min -11 _reflns_limit_h_max 10 _reflns_limit_k_min -29 _reflns_limit_k_max 29 _reflns_limit_l_min 0 _reflns_limit_l_max 13 _oxford_diffrn_Wilson_B_factor 2.65 _oxford_diffrn_Wilson_scale 6.25 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.65 _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 8428 _refine_ls_number_restraints 1 _refine_ls_number_parameters 452 _oxford_refine_ls_R_factor_ref 0.0492 _refine_ls_wR_factor_ref 0.0780 _refine_ls_goodness_of_fit_ref 0.9872 _refine_ls_shift/su_max 0.0005197 _refine_ls_shift/su_mean 1.0256064 # The values computed from all data _oxford_reflns_number_all 8428 _refine_ls_R_factor_all 0.0492 _refine_ls_wR_factor_all 0.0780 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 7093 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_gt 0.0719 _refine_ls_abs_structure_Flack -0.013(12) _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 none # 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^ + 0.78P] ,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 (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 0.57472(4) 0.82330(3) 0.71530(3) 0.0272 1.0000 Uani . . . . . . . C2 C 0.4980(3) 0.75181(11) 0.5920(2) 0.0268 1.0000 Uani . . . . . . . C3 C 0.3997(3) 0.80251(11) 0.5570(3) 0.0318 1.0000 Uani . . . . . . . C4 C 0.3330(3) 0.82098(15) 0.6660(3) 0.0395 1.0000 Uani . . . . . . . C5 C 0.3895(4) 0.78188(12) 0.7727(3) 0.0412 1.0000 Uani . . . . . . . C6 C 0.4905(4) 0.73964(12) 0.7257(3) 0.0342 1.0000 Uani . . . . . . . B7 B 0.5953(3) 0.71268(12) 0.5031(3) 0.0240 1.0000 Uani . . . . . . . F8 F 0.72576(17) 0.68373(7) 0.59700(14) 0.0299 1.0000 Uani . . . . . . . C9 C 0.6763(3) 0.75378(11) 0.4022(2) 0.0260 1.0000 Uani . . . . . . . C10 C 0.5938(3) 0.78057(11) 0.2871(2) 0.0308 1.0000 Uani . . . . . . . C11 C 0.6762(4) 0.81751(13) 0.2138(3) 0.0432 1.0000 Uani . . . . . . . C12 C 0.8367(4) 0.82806(14) 0.2508(3) 0.0480 1.0000 Uani . . . . . . . C13 C 0.9209(4) 0.80109(13) 0.3623(3) 0.0456 1.0000 Uani . . . . . . . C14 C 0.8405(3) 0.76435(12) 0.4354(3) 0.0355 1.0000 Uani . . . . . . . C15 C 0.4179(4) 0.77117(14) 0.2317(3) 0.0437 1.0000 Uani . . . . . . . C16 C 0.4832(3) 0.65908(10) 0.4286(2) 0.0268 1.0000 Uani . . . . . . . C17 C 0.5478(3) 0.61184(11) 0.3677(2) 0.0294 1.0000 Uani . . . . . . . C18 C 0.7241(3) 0.60739(12) 0.3666(3) 0.0361 1.0000 Uani . . . . . . . C19 C 0.4485(4) 0.56722(12) 0.3053(3) 0.0389 1.0000 Uani . . . . . . . C20 C 0.2853(4) 0.56833(13) 0.2995(3) 0.0447 1.0000 Uani . . . . . . . C21 C 0.2203(4) 0.61385(13) 0.3573(3) 0.0405 1.0000 Uani . . . . . . . C22 C 0.3181(3) 0.65806(12) 0.4214(3) 0.0329 1.0000 Uani . . . . . . . C23 C 0.7474(3) 0.87359(13) 0.6587(3) 0.0395 1.0000 Uani . . . . . . . C24 C 0.8176(3) 0.82817(14) 0.7435(3) 0.0381 1.0000 Uani . . . . . . . C25 C 0.7660(3) 0.83449(13) 0.8648(3) 0.0410 1.0000 Uani . . . . . . . C26 C 0.6641(4) 0.88464(14) 0.8537(3) 0.0451 1.0000 Uani . . . . . . . C27 C 0.6530(4) 0.90830(12) 0.7248(3) 0.0425 1.0000 Uani . . . . . . . K28 K 0.73856(6) 0.59398(4) 0.76211(5) 0.0295 1.0000 Uani . . . . . . . Cl29 Cl 0.99006(10) 0.49570(5) -0.02299(9) 0.0659 1.0000 Uani . . . . . . . C30 C 0.9436(4) 0.44110(14) 0.0826(3) 0.0420 1.0000 Uani . . . . . . . Cl31 Cl 0.83213(12) 0.38441(5) -0.00727(12) 0.0795 1.0000 Uani . . . . . . . Cl32 Cl 0.83952(15) 0.47171(6) 0.19468(11) 0.0842 1.0000 Uani . . . . . . . O33 O 0.9347(2) 0.53047(8) 0.62394(19) 0.0353 1.0000 Uani . . . . . . . C34 C 1.0976(3) 0.54651(14) 0.6421(3) 0.0431 1.0000 Uani . . . . . . . C35 C 1.1134(3) 0.61091(13) 0.6703(3) 0.0414 1.0000 Uani . . . . . . . O36 O 1.0708(2) 0.62206(8) 0.79440(18) 0.0352 1.0000 Uani . . . . . . . C37 C 1.0809(3) 0.68325(13) 0.8260(3) 0.0432 1.0000 Uani . . . . . . . C38 C 1.0453(4) 0.69150(14) 0.9598(3) 0.0449 1.0000 Uani . . . . . . . O39 O 0.8813(2) 0.67941(9) 0.95304(18) 0.0365 1.0000 Uani . . . . . . . C40 C 0.8382(3) 0.67908(14) 1.0795(3) 0.0406 1.0000 Uani . . . . . . . C41 C 0.6609(4) 0.67301(13) 1.0588(3) 0.0390 1.0000 Uani . . . . . . . O42 O 0.6203(2) 0.61764(9) 0.99524(18) 0.0378 1.0000 Uani . . . . . . . C43 C 0.4543(3) 0.60565(14) 0.9763(3) 0.0425 1.0000 Uani . . . . . . . C44 C 0.4301(4) 0.54209(15) 0.9459(3) 0.0476 1.0000 Uani . . . . . . . O45 O 0.4697(2) 0.52974(9) 0.8206(2) 0.0386 1.0000 Uani . . . . . . . C46 C 0.4586(3) 0.46877(13) 0.7896(3) 0.0484 1.0000 Uani . . . . . . . C47 C 0.5056(4) 0.45920(13) 0.6610(3) 0.0492 1.0000 Uani . . . . . . . O48 O 0.6702(2) 0.47323(9) 0.6748(2) 0.0414 1.0000 Uani . . . . . . . C49 C 0.7329(4) 0.45999(14) 0.5616(3) 0.0499 1.0000 Uani . . . . . . . C50 C 0.9082(4) 0.46991(13) 0.5929(3) 0.0481 1.0000 Uani . . . . . . . H31 H 0.3795 0.8229 0.4736 0.0371 1.0000 Uiso R . . . . . . H41 H 0.2556 0.8531 0.6602 0.0478 1.0000 Uiso R . . . . . . H51 H 0.3495 0.7839 0.8564 0.0493 1.0000 Uiso R . . . . . . H61 H 0.5638 0.7120 0.7921 0.0417 1.0000 Uiso R . . . . . . H111 H 0.6212 0.8374 0.1391 0.0516 1.0000 Uiso R . . . . . . H121 H 0.8910 0.8521 0.2017 0.0606 1.0000 Uiso R . . . . . . H131 H 1.0300 0.8064 0.3900 0.0559 1.0000 Uiso R . . . . . . H141 H 0.9119 0.7471 0.5128 0.0447 1.0000 Uiso R . . . . . . H151 H 0.3949 0.7890 0.1455 0.0671 1.0000 Uiso R . . . . . . H153 H 0.3959 0.7288 0.2282 0.0648 1.0000 Uiso R . . . . . . H152 H 0.3600 0.7913 0.2882 0.0669 1.0000 Uiso R . . . . . . H181 H 0.7550 0.5683 0.3399 0.0533 1.0000 Uiso R . . . . . . H183 H 0.7517 0.6351 0.3071 0.0506 1.0000 Uiso R . . . . . . H182 H 0.7816 0.6195 0.4490 0.0509 1.0000 Uiso R . . . . . . H191 H 0.4819 0.5341 0.2614 0.0501 1.0000 Uiso R . . . . . . H201 H 0.2234 0.5363 0.2559 0.0542 1.0000 Uiso R . . . . . . H211 H 0.1096 0.6170 0.3521 0.0482 1.0000 Uiso R . . . . . . H221 H 0.2774 0.6880 0.4695 0.0431 1.0000 Uiso R . . . . . . H231 H 0.7473 0.8773 0.5607 0.0494 1.0000 Uiso R . . . . . . H241 H 0.8748 0.7967 0.7192 0.0441 1.0000 Uiso R . . . . . . H251 H 0.7894 0.8075 0.9433 0.0478 1.0000 Uiso R . . . . . . H261 H 0.5997 0.8998 0.9178 0.0527 1.0000 Uiso R . . . . . . H271 H 0.5864 0.9426 0.6905 0.0455 1.0000 Uiso R . . . . . . H301 H 1.0417 0.4229 0.1370 0.0453 1.0000 Uiso R . . . . . . H342 H 1.1294 0.5402 0.5625 0.0544 1.0000 Uiso R . . . . . . H341 H 1.1606 0.5218 0.7077 0.0569 1.0000 Uiso R . . . . . . H351 H 1.2182 0.6252 0.6732 0.0485 1.0000 Uiso R . . . . . . H352 H 1.0318 0.6303 0.6005 0.0453 1.0000 Uiso R . . . . . . H372 H 1.2005 0.6922 0.8343 0.0524 1.0000 Uiso R . . . . . . H371 H 1.0027 0.7053 0.7520 0.0545 1.0000 Uiso R . . . . . . H382 H 1.1166 0.6618 1.0165 0.0555 1.0000 Uiso R . . . . . . H381 H 1.0701 0.7306 0.9943 0.0541 1.0000 Uiso R . . . . . . H401 H 0.8889 0.6466 1.1326 0.0486 1.0000 Uiso R . . . . . . H402 H 0.8767 0.7158 1.1276 0.0530 1.0000 Uiso R . . . . . . H412 H 0.6301 0.6779 1.1436 0.0510 1.0000 Uiso R . . . . . . H411 H 0.6161 0.7042 0.9956 0.0458 1.0000 Uiso R . . . . . . H432 H 0.4135 0.6140 1.0549 0.0474 1.0000 Uiso R . . . . . . H431 H 0.3962 0.6293 0.9115 0.0436 1.0000 Uiso R . . . . . . H441 H 0.3278 0.5308 0.9501 0.0547 1.0000 Uiso R . . . . . . H442 H 0.5030 0.5203 1.0132 0.0522 1.0000 Uiso R . . . . . . H462 H 0.3405 0.4598 0.7751 0.0598 1.0000 Uiso R . . . . . . H461 H 0.5208 0.4444 0.8572 0.0593 1.0000 Uiso R . . . . . . H472 H 0.4913 0.4173 0.6336 0.0593 1.0000 Uiso R . . . . . . H471 H 0.4352 0.4817 0.5883 0.0624 1.0000 Uiso R . . . . . . H491 H 0.7135 0.4194 0.5428 0.0575 1.0000 Uiso R . . . . . . H492 H 0.6801 0.4819 0.4833 0.0589 1.0000 Uiso R . . . . . . H502 H 0.9630 0.4603 0.5195 0.0565 1.0000 Uiso R . . . . . . H501 H 0.9508 0.4457 0.6684 0.0609 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 0.03545(19) 0.01906(16) 0.02746(18) -0.00240(15) 0.00688(14) -0.00328(16) C2 0.0280(13) 0.0228(12) 0.0297(14) -0.0052(10) 0.0058(10) -0.0074(10) C3 0.0328(14) 0.0296(13) 0.0315(14) -0.0054(11) 0.0025(11) 0.0002(11) C4 0.0315(14) 0.0358(14) 0.0524(16) -0.0127(16) 0.0110(12) -0.0026(14) C5 0.0519(18) 0.0350(15) 0.0443(17) -0.0138(13) 0.0282(15) -0.0151(14) C6 0.0479(17) 0.0237(13) 0.0336(15) -0.0038(11) 0.0144(13) -0.0113(12) B7 0.0257(15) 0.0202(13) 0.0249(14) 0.0009(11) 0.0020(11) 0.0027(11) F8 0.0318(8) 0.0286(8) 0.0269(8) 0.0037(6) 0.0000(6) 0.0029(6) C9 0.0348(14) 0.0198(12) 0.0237(13) -0.0039(10) 0.0069(11) -0.0007(11) C10 0.0413(16) 0.0232(12) 0.0296(14) -0.0004(10) 0.0111(12) 0.0060(11) C11 0.073(2) 0.0257(14) 0.0356(14) 0.0026(13) 0.0218(14) 0.0026(15) C12 0.075(2) 0.0325(15) 0.0443(17) -0.0047(15) 0.0303(15) -0.0142(17) C13 0.0486(18) 0.0456(17) 0.0473(18) -0.0162(14) 0.0210(15) -0.0209(14) C14 0.0403(16) 0.0351(15) 0.0320(15) -0.0072(12) 0.0089(12) -0.0071(13) C15 0.0506(18) 0.0486(18) 0.0301(15) 0.0078(13) 0.0037(13) 0.0118(15) C16 0.0359(14) 0.0208(12) 0.0224(12) 0.0031(10) 0.0025(10) -0.0029(11) C17 0.0447(16) 0.0206(12) 0.0231(13) 0.0018(10) 0.0077(11) 0.0007(11) C18 0.0493(17) 0.0267(14) 0.0340(15) 0.0000(11) 0.0122(12) 0.0071(12) C19 0.063(2) 0.0233(13) 0.0289(14) -0.0025(11) 0.0058(13) -0.0043(13) C20 0.058(2) 0.0362(16) 0.0371(16) -0.0029(13) 0.0036(14) -0.0212(15) C21 0.0407(16) 0.0399(17) 0.0399(16) 0.0003(13) 0.0055(13) -0.0102(13) C22 0.0387(16) 0.0294(14) 0.0315(14) -0.0036(11) 0.0090(12) -0.0077(12) C23 0.0440(17) 0.0364(16) 0.0351(15) 0.0028(12) 0.0007(13) -0.0144(14) C24 0.0375(14) 0.0295(14) 0.0451(16) -0.0079(14) 0.0025(12) -0.0023(14) C25 0.0497(17) 0.0339(17) 0.0354(15) -0.0002(12) -0.0015(13) -0.0123(13) C26 0.0487(18) 0.0427(17) 0.0462(18) -0.0214(15) 0.0147(14) -0.0140(15) C27 0.0416(17) 0.0188(13) 0.062(2) -0.0023(13) -0.0032(14) -0.0042(12) K28 0.0287(3) 0.0256(3) 0.0345(3) 0.0005(2) 0.0074(2) 0.0002(2) Cl29 0.0505(5) 0.0864(7) 0.0593(6) 0.0288(5) 0.0072(4) -0.0054(5) C30 0.0372(16) 0.0432(17) 0.0440(17) 0.0043(14) 0.0041(13) 0.0074(13) Cl31 0.0607(6) 0.0539(5) 0.1077(8) -0.0122(5) -0.0226(5) -0.0010(5) Cl32 0.1080(8) 0.0815(7) 0.0768(7) 0.0085(6) 0.0514(6) 0.0364(6) O33 0.0331(10) 0.0314(10) 0.0410(11) 0.0021(8) 0.0064(8) 0.0065(8) C34 0.0371(17) 0.0553(19) 0.0395(17) 0.0045(14) 0.0140(13) 0.0110(14) C35 0.0291(14) 0.057(2) 0.0398(16) 0.0093(14) 0.0112(12) -0.0033(13) O36 0.0282(10) 0.0373(10) 0.0407(11) 0.0063(9) 0.0080(8) -0.0022(8) C37 0.0323(15) 0.0331(15) 0.064(2) 0.0053(15) 0.0094(14) -0.0025(13) C38 0.0342(16) 0.0333(16) 0.064(2) -0.0110(15) 0.0020(14) -0.0044(13) O39 0.0312(10) 0.0384(11) 0.0378(11) -0.0045(9) 0.0018(8) -0.0028(8) C40 0.0475(17) 0.0409(16) 0.0295(15) -0.0079(13) -0.0019(13) 0.0062(14) C41 0.0504(18) 0.0419(16) 0.0251(14) -0.0025(12) 0.0080(12) 0.0145(14) O42 0.0302(10) 0.0441(11) 0.0396(11) -0.0048(9) 0.0083(8) 0.0035(8) C43 0.0294(14) 0.065(2) 0.0352(15) 0.0063(14) 0.0116(12) 0.0059(14) C44 0.0341(16) 0.069(2) 0.0414(18) 0.0154(15) 0.0118(13) -0.0070(15) O45 0.0336(10) 0.0354(11) 0.0458(12) 0.0074(9) 0.0059(9) -0.0034(9) C46 0.0305(16) 0.0376(16) 0.074(2) 0.0178(16) 0.0037(15) -0.0016(13) C47 0.0377(17) 0.0304(16) 0.072(2) -0.0081(15) -0.0079(15) -0.0023(13) O48 0.0412(11) 0.0343(11) 0.0457(12) -0.0059(9) 0.0011(9) -0.0025(9) C49 0.073(2) 0.0376(18) 0.0375(17) -0.0087(14) 0.0069(16) -0.0120(16) C50 0.070(2) 0.0335(16) 0.0445(18) -0.0060(13) 0.0204(16) 0.0095(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.4268(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 . 2.089(2) yes Fe1 . C3 . 2.044(3) yes Fe1 . C4 . 2.029(3) yes Fe1 . C5 . 2.029(3) yes Fe1 . C6 . 2.042(3) yes Fe1 . C23 . 2.042(3) yes Fe1 . C24 . 2.042(3) yes Fe1 . C25 . 2.033(3) yes Fe1 . C26 . 2.035(3) yes Fe1 . C27 . 2.038(3) yes C2 . C3 . 1.429(4) yes C2 . C6 . 1.425(4) yes C2 . B7 . 1.621(4) yes C3 . C4 . 1.424(4) yes C3 . H31 . 0.964 no C4 . C5 . 1.424(4) yes C4 . H41 . 0.979 no C5 . C6 . 1.438(4) yes C5 . H51 . 0.993 no C6 . H61 . 1.044 no B7 . F8 . 1.481(3) yes B7 . C9 . 1.652(4) yes B7 . C16 . 1.644(4) yes C9 . C10 . 1.397(3) yes C9 . C14 . 1.399(4) yes C10 . C11 . 1.409(4) yes C10 . C15 . 1.516(4) yes C11 . C12 . 1.371(4) yes C11 . H111 . 0.937 no C12 . C13 . 1.377(5) yes C12 . H121 . 0.931 no C13 . C14 . 1.395(4) yes C13 . H131 . 0.928 no C14 . H141 . 0.988 no C15 . H151 . 0.963 no C15 . H153 . 0.980 no C15 . H152 . 0.954 no C16 . C17 . 1.410(3) yes C16 . C22 . 1.399(4) yes C17 . C18 . 1.513(4) yes C17 . C19 . 1.396(4) yes C18 . H181 . 0.980 no C18 . H183 . 0.942 no C18 . H182 . 0.937 no C19 . C20 . 1.385(4) yes C19 . H191 . 0.951 no C20 . C21 . 1.366(4) yes C20 . H201 . 0.958 no C21 . C22 . 1.389(4) yes C21 . H211 . 0.941 no C22 . H221 . 0.948 no C23 . C24 . 1.409(4) yes C23 . C27 . 1.400(4) yes C23 . H231 . 1.017 no C24 . C25 . 1.417(4) yes C24 . H241 . 0.929 no C25 . C26 . 1.424(4) yes C25 . H251 . 1.005 no C26 . C27 . 1.423(4) yes C26 . H261 . 1.003 no C27 . H271 . 0.987 no Cl29 . C30 . 1.749(3) yes C30 . Cl31 . 1.755(3) yes C30 . Cl32 . 1.740(3) yes C30 . H301 . 1.003 no O33 . C34 . 1.416(3) yes O33 . C50 . 1.420(3) yes C34 . C35 . 1.492(4) yes C34 . H342 . 0.928 no C34 . H341 . 0.960 no C35 . O36 . 1.425(3) yes C35 . H351 . 0.948 no C35 . H352 . 1.002 no O36 . C37 . 1.426(3) yes C37 . C38 . 1.487(4) yes C37 . H372 . 1.030 no C37 . H371 . 1.040 no C38 . O39 . 1.417(3) yes C38 . H382 . 1.014 no C38 . H381 . 0.965 no O39 . C40 . 1.428(3) yes C40 . C41 . 1.495(4) yes C40 . H401 . 0.969 no C40 . H402 . 0.994 no C41 . O42 . 1.429(3) yes C41 . H412 . 0.971 no C41 . H411 . 0.988 no O42 . C43 . 1.421(3) yes C43 . C44 . 1.482(5) yes C43 . H432 . 0.965 no C43 . H431 . 0.923 no C44 . O45 . 1.431(4) yes C44 . H441 . 0.921 no C44 . H442 . 0.972 no O45 . C46 . 1.420(4) yes C46 . C47 . 1.480(5) yes C46 . H462 . 1.012 no C46 . H461 . 0.966 no C47 . O48 . 1.422(4) yes C47 . H472 . 0.992 no C47 . H471 . 1.005 no O48 . C49 . 1.413(4) yes C49 . C50 . 1.487(5) yes C49 . H491 . 0.951 no C49 . H492 . 0.981 no C50 . H502 . 0.992 no C50 . H501 . 0.966 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 . 40.44(10) yes C2 . Fe1 . C4 . 69.20(11) yes C3 . Fe1 . C4 . 40.92(10) yes C2 . Fe1 . C5 . 69.48(10) yes C3 . Fe1 . C5 . 68.71(11) yes C4 . Fe1 . C5 . 41.08(13) yes C2 . Fe1 . C6 . 40.33(10) yes C3 . Fe1 . C6 . 67.48(11) yes C4 . Fe1 . C6 . 68.68(13) yes C5 . Fe1 . C6 . 41.37(11) yes C2 . Fe1 . C23 . 114.63(11) yes C3 . Fe1 . C23 . 110.84(11) yes C4 . Fe1 . C23 . 134.50(12) yes C5 . Fe1 . C23 . 173.56(13) yes C6 . Fe1 . C23 . 144.87(12) yes C2 . Fe1 . C24 . 108.50(11) yes C3 . Fe1 . C24 . 133.64(11) yes C4 . Fe1 . C24 . 173.60(12) yes C5 . Fe1 . C24 . 144.47(13) yes C6 . Fe1 . C24 . 113.73(12) yes C2 . Fe1 . C25 . 132.10(11) yes C3 . Fe1 . C25 . 172.04(11) yes C4 . Fe1 . C25 . 145.17(12) yes C5 . Fe1 . C25 . 113.11(12) yes C6 . Fe1 . C25 . 108.39(12) yes C2 . Fe1 . C26 . 172.16(12) yes C3 . Fe1 . C26 . 146.70(12) yes C4 . Fe1 . C26 . 114.66(12) yes C5 . Fe1 . C26 . 108.53(12) yes C6 . Fe1 . C26 . 133.40(12) yes C2 . Fe1 . C27 . 145.64(12) yes C3 . Fe1 . C27 . 116.03(11) yes C4 . Fe1 . C27 . 110.20(13) yes C5 . Fe1 . C27 . 133.83(12) yes C6 . Fe1 . C27 . 173.73(13) yes C23 . Fe1 . C24 . 40.36(12) yes C23 . Fe1 . C25 . 68.27(11) yes C24 . Fe1 . C25 . 40.70(11) yes C23 . Fe1 . C26 . 68.09(12) yes C24 . Fe1 . C26 . 68.41(12) yes C25 . Fe1 . C26 . 40.99(13) yes C23 . Fe1 . C27 . 40.12(13) yes C24 . Fe1 . C27 . 68.08(12) yes C25 . Fe1 . C27 . 68.77(12) yes C26 . Fe1 . C27 . 40.90(13) yes Fe1 . C2 . C3 . 68.09(14) yes Fe1 . C2 . C6 . 68.06(14) yes C3 . C2 . C6 . 105.4(2) yes Fe1 . C2 . B7 . 129.62(17) yes C3 . C2 . B7 . 129.8(2) yes C6 . C2 . B7 . 124.8(2) yes C2 . C3 . Fe1 . 71.46(14) yes C2 . C3 . C4 . 110.1(2) yes Fe1 . C3 . C4 . 68.99(15) yes C2 . C3 . H31 . 127.3 no Fe1 . C3 . H31 . 125.4 no C4 . C3 . H31 . 122.6 no C3 . C4 . Fe1 . 70.09(14) yes C3 . C4 . C5 . 107.6(2) yes Fe1 . C4 . C5 . 69.46(16) yes C3 . C4 . H41 . 122.8 no Fe1 . C4 . H41 . 129.7 no C5 . C4 . H41 . 129.3 no C4 . C5 . Fe1 . 69.46(15) yes C4 . C5 . C6 . 106.7(2) yes Fe1 . C5 . C6 . 69.77(15) yes C4 . C5 . H51 . 121.7 no Fe1 . C5 . H51 . 131.0 no C6 . C5 . H51 . 131.2 no C5 . C6 . C2 . 110.2(3) yes C5 . C6 . Fe1 . 68.86(15) yes C2 . C6 . Fe1 . 71.61(14) yes C5 . C6 . H61 . 120.1 no C2 . C6 . H61 . 128.3 no Fe1 . C6 . H61 . 114.9 no C2 . B7 . F8 . 106.01(19) yes C2 . B7 . C9 . 112.05(19) yes F8 . B7 . C9 . 108.04(19) yes C2 . B7 . C16 . 110.8(2) yes F8 . B7 . C16 . 105.87(18) yes C9 . B7 . C16 . 113.6(2) yes B7 . C9 . C10 . 125.5(2) yes B7 . C9 . C14 . 117.9(2) yes C10 . C9 . C14 . 116.6(2) yes C9 . C10 . C11 . 119.7(3) yes C9 . C10 . C15 . 123.9(2) yes C11 . C10 . C15 . 116.4(2) yes C10 . C11 . C12 . 122.2(3) yes C10 . C11 . H111 . 120.5 no C12 . C11 . H111 . 117.2 no C11 . C12 . C13 . 119.1(3) yes C11 . C12 . H121 . 122.0 no C13 . C12 . H121 . 118.9 no C12 . C13 . C14 . 119.2(3) yes C12 . C13 . H131 . 121.9 no C14 . C13 . H131 . 119.0 no C9 . C14 . C13 . 123.2(3) yes C9 . C14 . H141 . 124.1 no C13 . C14 . H141 . 112.6 no C10 . C15 . H151 . 107.3 no C10 . C15 . H153 . 108.7 no H151 . C15 . H153 . 112.0 no C10 . C15 . H152 . 107.3 no H151 . C15 . H152 . 109.3 no H153 . C15 . H152 . 111.9 no B7 . C16 . C17 . 121.9(2) yes B7 . C16 . C22 . 121.7(2) yes C17 . C16 . C22 . 116.4(2) yes C16 . C17 . C18 . 122.2(2) yes C16 . C17 . C19 . 120.1(2) yes C18 . C17 . C19 . 117.6(2) yes C17 . C18 . H181 . 112.8 no C17 . C18 . H183 . 109.8 no H181 . C18 . H183 . 107.7 no C17 . C18 . H182 . 108.5 no H181 . C18 . H182 . 113.5 no H183 . C18 . H182 . 104.1 no C17 . C19 . C20 . 121.5(3) yes C17 . C19 . H191 . 125.6 no C20 . C19 . H191 . 112.9 no C19 . C20 . C21 . 119.2(3) yes C19 . C20 . H201 . 117.7 no C21 . C20 . H201 . 123.0 no C20 . C21 . C22 . 119.8(3) yes C20 . C21 . H211 . 121.6 no C22 . C21 . H211 . 118.5 no C16 . C22 . C21 . 122.9(3) yes C16 . C22 . H221 . 115.6 no C21 . C22 . H221 . 121.3 no Fe1 . C23 . C24 . 69.82(16) yes Fe1 . C23 . C27 . 69.80(16) yes C24 . C23 . C27 . 108.8(3) yes Fe1 . C23 . H231 . 118.3 no C24 . C23 . H231 . 126.7 no C27 . C23 . H231 . 123.7 no C23 . C24 . Fe1 . 69.81(16) yes C23 . C24 . C25 . 108.0(3) yes Fe1 . C24 . C25 . 69.31(16) yes C23 . C24 . H241 . 125.2 no Fe1 . C24 . H241 . 119.7 no C25 . C24 . H241 . 126.2 no C24 . C25 . Fe1 . 69.99(15) yes C24 . C25 . C26 . 107.5(3) yes Fe1 . C25 . C26 . 69.56(16) yes C24 . C25 . H251 . 127.3 no Fe1 . C25 . H251 . 122.7 no C26 . C25 . H251 . 125.0 no C25 . C26 . Fe1 . 69.45(16) yes C25 . C26 . C27 . 107.7(3) yes Fe1 . C26 . C27 . 69.69(16) yes C25 . C26 . H261 . 128.9 no Fe1 . C26 . H261 . 121.4 no C27 . C26 . H261 . 123.1 no C26 . C27 . C23 . 107.9(3) yes C26 . C27 . Fe1 . 69.41(16) yes C23 . C27 . Fe1 . 70.08(16) yes C26 . C27 . H271 . 124.1 no C23 . C27 . H271 . 127.9 no Fe1 . C27 . H271 . 124.6 no Cl29 . C30 . Cl31 . 110.81(17) yes Cl29 . C30 . Cl32 . 110.03(17) yes Cl31 . C30 . Cl32 . 110.48(17) yes Cl29 . C30 . H301 . 112.0 no Cl31 . C30 . H301 . 107.6 no Cl32 . C30 . H301 . 105.8 no C34 . O33 . C50 . 112.8(2) yes O33 . C34 . C35 . 109.1(2) yes O33 . C34 . H342 . 107.2 no C35 . C34 . H342 . 107.1 no O33 . C34 . H341 . 110.1 no C35 . C34 . H341 . 114.7 no H342 . C34 . H341 . 108.4 no C34 . C35 . O36 . 108.7(2) yes C34 . C35 . H351 . 112.9 no O36 . C35 . H351 . 108.7 no C34 . C35 . H352 . 105.4 no O36 . C35 . H352 . 107.8 no H351 . C35 . H352 . 113.1 no C35 . O36 . C37 . 111.4(2) yes O36 . C37 . C38 . 108.8(2) yes O36 . C37 . H372 . 103.1 no C38 . C37 . H372 . 106.3 no O36 . C37 . H371 . 107.3 no C38 . C37 . H371 . 113.9 no H372 . C37 . H371 . 116.8 no C37 . C38 . O39 . 108.2(2) yes C37 . C38 . H382 . 104.2 no O39 . C38 . H382 . 112.0 no C37 . C38 . H381 . 112.9 no O39 . C38 . H381 . 109.9 no H382 . C38 . H381 . 109.6 no C38 . O39 . C40 . 112.8(2) yes O39 . C40 . C41 . 107.9(2) yes O39 . C40 . H401 . 110.8 no C41 . C40 . H401 . 109.8 no O39 . C40 . H402 . 109.5 no C41 . C40 . H402 . 112.1 no H401 . C40 . H402 . 106.8 no C40 . C41 . O42 . 107.1(2) yes C40 . C41 . H412 . 108.0 no O42 . C41 . H412 . 115.6 no C40 . C41 . H411 . 106.2 no O42 . C41 . H411 . 107.3 no H412 . C41 . H411 . 112.2 no C41 . O42 . C43 . 112.2(2) yes O42 . C43 . C44 . 108.0(2) yes O42 . C43 . H432 . 111.4 no C44 . C43 . H432 . 108.2 no O42 . C43 . H431 . 111.7 no C44 . C43 . H431 . 112.2 no H432 . C43 . H431 . 105.4 no C43 . C44 . O45 . 109.6(2) yes C43 . C44 . H441 . 110.8 no O45 . C44 . H441 . 112.6 no C43 . C44 . H442 . 107.5 no O45 . C44 . H442 . 108.4 no H441 . C44 . H442 . 107.8 no C44 . O45 . C46 . 112.3(2) yes O45 . C46 . C47 . 109.2(2) yes O45 . C46 . H462 . 104.4 no C47 . C46 . H462 . 106.2 no O45 . C46 . H461 . 113.1 no C47 . C46 . H461 . 111.0 no H462 . C46 . H461 . 112.5 no C46 . C47 . O48 . 108.5(2) yes C46 . C47 . H472 . 110.9 no O48 . C47 . H472 . 107.9 no C46 . C47 . H471 . 111.7 no O48 . C47 . H471 . 113.3 no H472 . C47 . H471 . 104.5 no C47 . O48 . C49 . 113.5(2) yes O48 . C49 . C50 . 108.6(2) yes O48 . C49 . H491 . 107.3 no C50 . C49 . H491 . 108.6 no O48 . C49 . H492 . 112.8 no C50 . C49 . H492 . 112.5 no H491 . C49 . H492 . 106.9 no C49 . C50 . O33 . 107.7(2) yes C49 . C50 . H502 . 114.1 no O33 . C50 . H502 . 107.9 no C49 . C50 . H501 . 107.0 no O33 . C50 . H501 . 110.5 no H502 . C50 . H501 . 109.5 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 C15 . H153 . C16 . 123 0.98 2.60 3.238(4) yes C30 . H301 . C25 2_746 141 1.00 2.60 3.433(4) yes # Attachment '123pfdv09.cif' data_123pfdv09 _database_code_depnum_ccdc_archive 'CCDC 809731' #TrackingRef '123pfdv09.cif' _audit_creation_date 09-12-16 _audit_creation_method CRYSTALS_ver_12.86 _oxford_structure_analysis_title 123pfdv09 _chemical_name_systematic . _chemical_melting_point 'not measured' _cell_length_a 11.5278(2) _cell_length_b 13.2927(2) _cell_length_c 13.7154(2) _cell_angle_alpha 84.1631(7) _cell_angle_beta 71.6023(7) _cell_angle_gamma 65.2619(7) _cell_volume 1810.13(5) _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' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' K 0.2009 0.2494 8.2186 12.7949 7.4398 0.7748 1.0519 213.1870 0.8659 41.6841 1.4228 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 # Given Formula = C37 H50 B1 Fe1 K1 N1 O6 # Dc = 1.30 Fooo = 748.00 Mu = 5.77 M = 710.56 # Found Formula = C37 H47 B1 Fe1 K1 N1 O6 # Dc = 1.30 FOOO = 748.00 Mu = 5.76 M = 707.54 _chemical_formula_sum 'C37 H47 B1 Fe1 K1 N1 O6' _chemical_formula_moiety 'C37 H47 B1 Fe1 K1 N1 O6' _chemical_compound_source . _chemical_formula_weight 707.54 _cell_measurement_reflns_used 7037 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.25 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_max 0.50 _exptl_crystal_density_diffrn 1.298 _exptl_crystal_density_meas . _exptl_crystal_density_method 'not measured' # Non-dispersive F(000): _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.576 # Sheldrick geometric approximatio 0.78 0.87 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.87 # 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 25142 _reflns_number_total 8175 _diffrn_reflns_av_R_equivalents 0.032 # Number of reflections with Friedels Law is 8175 # Number of reflections without Friedels Law is 13155 # Theoretical number of reflections is about 8364 _diffrn_reflns_theta_min 5.144 _diffrn_reflns_theta_max 27.556 _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.076 _diffrn_measured_fraction_theta_full 0.985 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _reflns_limit_h_min -13 _reflns_limit_h_max 14 _reflns_limit_k_min -17 _reflns_limit_k_max 17 _reflns_limit_l_min 0 _reflns_limit_l_max 17 _oxford_diffrn_Wilson_B_factor 2.54 _oxford_diffrn_Wilson_scale 1.82 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.45 _refine_diff_density_max 0.52 # 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 8174 _refine_ls_number_restraints 0 _refine_ls_number_parameters 424 _oxford_refine_ls_R_factor_ref 0.0535 _refine_ls_wR_factor_ref 0.0896 _refine_ls_goodness_of_fit_ref 0.9684 _refine_ls_shift/su_max 0.000646 # The values computed from all data _oxford_reflns_number_all 8175 _refine_ls_R_factor_all 0.0536 _refine_ls_wR_factor_all 0.0897 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6465 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_gt 0.0820 # 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 noref # 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 0.34698(2) 0.51903(2) 0.718376(19) 0.0324 1.0000 Uani . . . . . . . C2 C 0.50266(16) 0.37861(14) 0.74810(12) 0.0274 1.0000 Uani . . . . . . . C3 C 0.53310(17) 0.40634(16) 0.64166(13) 0.0346 1.0000 Uani . . . . . . . C4 C 0.52806(19) 0.51578(17) 0.63216(16) 0.0425 1.0000 Uani . . . . . . . C5 C 0.4930(2) 0.55888(17) 0.73264(17) 0.0458 1.0000 Uani . . . . . . . C6 C 0.4771(2) 0.47515(15) 0.80319(14) 0.0367 1.0000 Uani . . . . . . . B7 B 0.50459(18) 0.26085(16) 0.79544(14) 0.0259 1.0000 Uani . . . . . . . C8 C 0.41182(16) 0.27836(13) 0.91646(12) 0.0261 1.0000 Uani . . . . . . . C9 C 0.45359(17) 0.29373(13) 0.99794(13) 0.0296 1.0000 Uani . . . . . . . C10 C 0.59110(19) 0.28947(16) 0.97959(14) 0.0355 1.0000 Uani . . . . . . . C11 C 0.36721(19) 0.31087(15) 1.09913(13) 0.0361 1.0000 Uani . . . . . . . C12 C 0.2406(2) 0.31350(15) 1.12251(14) 0.0392 1.0000 Uani . . . . . . . C13 C 0.19731(18) 0.29959(15) 1.04439(14) 0.0367 1.0000 Uani . . . . . . . C14 C 0.28164(17) 0.28261(14) 0.94371(13) 0.0312 1.0000 Uani . . . . . . . C15 C 0.66027(16) 0.16435(14) 0.76981(12) 0.0271 1.0000 Uani . . . . . . . C16 C 0.69435(17) 0.05680(14) 0.80919(13) 0.0316 1.0000 Uani . . . . . . . C17 C 0.5906(2) 0.02268(16) 0.88248(16) 0.0435 1.0000 Uani . . . . . . . C18 C 0.82697(19) -0.02205(16) 0.77973(15) 0.0403 1.0000 Uani . . . . . . . C19 C 0.92836(19) 0.00104(18) 0.70908(17) 0.0483 1.0000 Uani . . . . . . . C20 C 0.89761(18) 0.10457(19) 0.66789(17) 0.0467 1.0000 Uani . . . . . . . C21 C 0.76618(17) 0.18422(16) 0.69929(15) 0.0365 1.0000 Uani . . . . . . . C22 C 0.43476(16) 0.21876(14) 0.73214(13) 0.0299 1.0000 Uani . . . . . . . N23 N 0.38400(15) 0.18944(14) 0.68803(13) 0.0410 1.0000 Uani . . . . . . . C24 C 0.2175(2) 0.5219(2) 0.64460(18) 0.0609 1.0000 Uani . . . . . . . C25 C 0.18766(19) 0.47800(19) 0.74402(18) 0.0496 1.0000 Uani . . . . . . . C26 C 0.1577(2) 0.55957(19) 0.81661(17) 0.0531 1.0000 Uani . . . . . . . C27 C 0.1682(2) 0.65457(19) 0.7638(2) 0.0601 1.0000 Uani . . . . . . . C28 C 0.2055(2) 0.6319(2) 0.6576(2) 0.0637 1.0000 Uani . . . . . . . K29 K 0.15836(4) 0.16487(3) 0.68449(3) 0.0308 1.0000 Uani . . . . . . . O30 O 0.05148(13) 0.32910(11) 0.54611(10) 0.0400 1.0000 Uani . . . . . . . C31 C -0.08246(19) 0.40747(16) 0.58779(16) 0.0407 1.0000 Uani . . . . . . . C32 C -0.10109(19) 0.44528(15) 0.69328(16) 0.0400 1.0000 Uani . . . . . . . O33 O -0.07759(13) 0.35277(10) 0.75764(10) 0.0399 1.0000 Uani . . . . . . . C34 C -0.1131(2) 0.38399(17) 0.86234(16) 0.0439 1.0000 Uani . . . . . . . C35 C -0.09430(19) 0.28176(17) 0.92468(16) 0.0441 1.0000 Uani . . . . . . . O36 O 0.04350(12) 0.20979(10) 0.89841(10) 0.0356 1.0000 Uani . . . . . . . C37 C 0.0649(2) 0.11488(17) 0.95978(15) 0.0449 1.0000 Uani . . . . . . . C38 C 0.2071(2) 0.03259(17) 0.91896(15) 0.0443 1.0000 Uani . . . . . . . O39 O 0.22303(14) -0.01132(11) 0.82304(10) 0.0420 1.0000 Uani . . . . . . . C40 C 0.3551(2) -0.09029(18) 0.77689(17) 0.0509 1.0000 Uani . . . . . . . C41 C 0.3589(2) -0.13503(16) 0.67925(17) 0.0512 1.0000 Uani . . . . . . . O42 O 0.33538(15) -0.04813(10) 0.60973(10) 0.0435 1.0000 Uani . . . . . . . C43 C 0.3316(2) -0.08099(16) 0.51580(16) 0.0454 1.0000 Uani . . . . . . . C44 C 0.3335(2) 0.00921(17) 0.44091(16) 0.0481 1.0000 Uani . . . . . . . O45 O 0.21611(14) 0.10695(11) 0.47995(10) 0.0415 1.0000 Uani . . . . . . . C46 C 0.2099(2) 0.19528(18) 0.41216(16) 0.0505 1.0000 Uani . . . . . . . C47 C 0.0713(2) 0.28682(18) 0.44845(16) 0.0489 1.0000 Uani . . . . . . . H31 H 0.5536 0.3561 0.5834 0.0412 1.0000 Uiso . . . . . . . H41 H 0.5436 0.5545 0.5677 0.0534 1.0000 Uiso . . . . . . . H51 H 0.4781 0.6352 0.7511 0.0615 1.0000 Uiso . . . . . . . H61 H 0.4460 0.4849 0.8803 0.0505 1.0000 Uiso . . . . . . . H101 H 0.5946 0.3223 1.0376 0.0583 1.0000 Uiso . . . . . . . H102 H 0.6175 0.3276 0.9197 0.0578 1.0000 Uiso . . . . . . . H103 H 0.6577 0.2130 0.9710 0.0585 1.0000 Uiso . . . . . . . H111 H 0.3984 0.3213 1.1526 0.0407 1.0000 Uiso . . . . . . . H121 H 0.1824 0.3247 1.1933 0.0420 1.0000 Uiso . . . . . . . H131 H 0.1088 0.3014 1.0594 0.0417 1.0000 Uiso . . . . . . . H141 H 0.2490 0.2735 0.8917 0.0364 1.0000 Uiso . . . . . . . H171 H 0.6261 -0.0572 0.8932 0.0625 1.0000 Uiso . . . . . . . H173 H 0.5557 0.0612 0.9485 0.0620 1.0000 Uiso . . . . . . . H172 H 0.5143 0.0404 0.8566 0.0619 1.0000 Uiso . . . . . . . H181 H 0.8468 -0.0952 0.8088 0.0465 1.0000 Uiso . . . . . . . H191 H 1.0198 -0.0546 0.6890 0.0536 1.0000 Uiso . . . . . . . H201 H 0.9679 0.1228 0.6166 0.0542 1.0000 Uiso . . . . . . . H211 H 0.7468 0.2576 0.6708 0.0445 1.0000 Uiso . . . . . . . H241 H 0.2438 0.4807 0.5780 0.0735 1.0000 Uiso . . . . . . . H251 H 0.1934 0.3999 0.7591 0.0590 1.0000 Uiso . . . . . . . H261 H 0.1388 0.5495 0.8931 0.0558 1.0000 Uiso . . . . . . . H271 H 0.1534 0.7263 0.7961 0.0642 1.0000 Uiso . . . . . . . H281 H 0.2247 0.6831 0.6005 0.0739 1.0000 Uiso . . . . . . . H311 H -0.1007 0.4709 0.5421 0.0499 1.0000 Uiso . . . . . . . H312 H -0.1455 0.3729 0.5915 0.0506 1.0000 Uiso . . . . . . . H322 H -0.0379 0.4821 0.6915 0.0476 1.0000 Uiso . . . . . . . H321 H -0.1954 0.5000 0.7228 0.0470 1.0000 Uiso . . . . . . . H341 H -0.0569 0.4204 0.8702 0.0479 1.0000 Uiso . . . . . . . H342 H -0.2074 0.4387 0.8858 0.0478 1.0000 Uiso . . . . . . . H351 H -0.1288 0.3028 0.9981 0.0477 1.0000 Uiso . . . . . . . H352 H -0.1451 0.2424 0.9096 0.0480 1.0000 Uiso . . . . . . . H372 H 0.0442 0.1373 1.0321 0.0525 1.0000 Uiso . . . . . . . H371 H 0.0019 0.0827 0.9580 0.0525 1.0000 Uiso . . . . . . . H381 H 0.2262 -0.0297 0.9681 0.0525 1.0000 Uiso . . . . . . . H382 H 0.2711 0.0689 0.9104 0.0528 1.0000 Uiso . . . . . . . H402 H 0.3808 -0.1507 0.8252 0.0564 1.0000 Uiso . . . . . . . H401 H 0.4189 -0.0516 0.7610 0.0572 1.0000 Uiso . . . . . . . H411 H 0.4478 -0.1972 0.6476 0.0577 1.0000 Uiso . . . . . . . H412 H 0.2832 -0.1626 0.6951 0.0584 1.0000 Uiso . . . . . . . H431 H 0.4099 -0.1501 0.4886 0.0513 1.0000 Uiso . . . . . . . H432 H 0.2476 -0.0925 0.5291 0.0516 1.0000 Uiso . . . . . . . H442 H 0.4169 0.0246 0.4309 0.0511 1.0000 Uiso . . . . . . . H441 H 0.3351 -0.0121 0.3744 0.0500 1.0000 Uiso . . . . . . . H461 H 0.2803 0.2242 0.4127 0.0583 1.0000 Uiso . . . . . . . H462 H 0.2319 0.1696 0.3407 0.0573 1.0000 Uiso . . . . . . . H471 H 0.0610 0.3476 0.3977 0.0568 1.0000 Uiso . . . . . . . H472 H 0.0018 0.2544 0.4557 0.0576 1.0000 Uiso . . . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02781(13) 0.03444(15) 0.03046(14) 0.00408(10) -0.01130(10) -0.00730(11) C2 0.0224(8) 0.0317(9) 0.0292(8) 0.0025(7) -0.0107(6) -0.0104(7) C3 0.0250(8) 0.0437(10) 0.0296(9) 0.0050(8) -0.0076(7) -0.0101(8) C4 0.0332(10) 0.0482(11) 0.0474(11) 0.0225(9) -0.0181(9) -0.0185(9) C5 0.0559(12) 0.0365(10) 0.0638(13) 0.0191(9) -0.0399(11) -0.0246(10) C6 0.0486(11) 0.0303(9) 0.0404(10) 0.0073(8) -0.0274(9) -0.0160(8) B7 0.0226(8) 0.0292(9) 0.0268(9) -0.0017(7) -0.0069(7) -0.0112(8) C8 0.0256(8) 0.0213(8) 0.0280(8) -0.0009(6) -0.0060(6) -0.0074(6) C9 0.0314(8) 0.0234(8) 0.0306(8) 0.0003(7) -0.0108(7) -0.0070(7) C10 0.0377(10) 0.0378(10) 0.0352(9) 0.0020(8) -0.0177(8) -0.0148(8) C11 0.0441(10) 0.0286(9) 0.0289(9) -0.0027(7) -0.0114(8) -0.0076(8) C12 0.0411(10) 0.0307(9) 0.0309(9) -0.0031(7) 0.0015(8) -0.0086(8) C13 0.0277(9) 0.0324(9) 0.0404(10) -0.0023(8) 0.0015(7) -0.0111(8) C14 0.0268(8) 0.0310(9) 0.0333(9) -0.0023(7) -0.0056(7) -0.0112(7) C15 0.0239(8) 0.0296(8) 0.0287(8) -0.0026(7) -0.0082(6) -0.0107(7) C16 0.0308(9) 0.0307(9) 0.0314(9) -0.0011(7) -0.0089(7) -0.0107(7) C17 0.0385(10) 0.0326(10) 0.0478(11) 0.0072(8) -0.0027(9) -0.0124(8) C18 0.0337(10) 0.0347(10) 0.0435(11) 0.0014(8) -0.0132(8) -0.0044(8) C19 0.0240(9) 0.0474(12) 0.0572(13) -0.0011(10) -0.0075(9) -0.0021(9) C20 0.0239(9) 0.0535(12) 0.0558(13) 0.0032(10) -0.0043(8) -0.0153(9) C21 0.0258(8) 0.0372(10) 0.0456(10) 0.0029(8) -0.0083(8) -0.0142(8) C22 0.0224(8) 0.0317(9) 0.0300(9) -0.0065(7) -0.0030(7) -0.0078(7) N23 0.0316(8) 0.0460(9) 0.0457(9) -0.0131(7) -0.0111(7) -0.0132(7) C24 0.0306(10) 0.094(2) 0.0558(14) 0.0024(13) -0.0239(10) -0.0152(12) C25 0.0255(9) 0.0516(13) 0.0662(14) 0.0038(11) -0.0153(9) -0.0098(9) C26 0.0353(11) 0.0508(13) 0.0513(13) 0.0022(10) 0.0002(9) -0.0067(10) C27 0.0392(12) 0.0410(12) 0.0757(17) 0.0053(11) -0.0068(11) -0.0017(10) C28 0.0366(11) 0.0721(17) 0.0739(17) 0.0328(14) -0.0275(11) -0.0131(11) K29 0.03256(19) 0.02637(18) 0.03266(19) 0.00222(14) -0.01457(15) -0.00810(15) O30 0.0390(7) 0.0359(7) 0.0429(7) 0.0037(6) -0.0187(6) -0.0092(6) C31 0.0362(10) 0.0317(9) 0.0572(12) 0.0113(9) -0.0236(9) -0.0119(8) C32 0.0369(10) 0.0265(9) 0.0542(12) 0.0074(8) -0.0208(9) -0.0070(8) O33 0.0410(7) 0.0298(7) 0.0445(7) 0.0052(6) -0.0152(6) -0.0097(6) C34 0.0362(10) 0.0361(10) 0.0459(11) -0.0016(9) -0.0042(9) -0.0074(8) C35 0.0333(10) 0.0396(11) 0.0463(11) 0.0035(9) -0.0017(8) -0.0104(9) O36 0.0331(6) 0.0340(7) 0.0397(7) 0.0084(5) -0.0124(5) -0.0142(6) C37 0.0540(12) 0.0401(11) 0.0381(10) 0.0132(8) -0.0145(9) -0.0191(10) C38 0.0511(12) 0.0405(11) 0.0410(11) 0.0108(9) -0.0226(9) -0.0142(9) O39 0.0438(8) 0.0365(7) 0.0428(7) 0.0058(6) -0.0181(6) -0.0111(6) C40 0.0498(12) 0.0384(11) 0.0508(12) 0.0119(9) -0.0204(10) -0.0038(10) C41 0.0609(14) 0.0276(10) 0.0500(12) 0.0082(9) -0.0169(10) -0.0054(9) O42 0.0572(9) 0.0287(7) 0.0392(7) 0.0033(5) -0.0164(6) -0.0119(6) C43 0.0533(12) 0.0331(10) 0.0412(11) -0.0073(8) -0.0094(9) -0.0114(9) C44 0.0534(12) 0.0393(11) 0.0365(10) -0.0055(8) -0.0079(9) -0.0073(10) O45 0.0459(8) 0.0351(7) 0.0344(7) 0.0017(5) -0.0118(6) -0.0086(6) C46 0.0628(14) 0.0470(12) 0.0342(10) 0.0070(9) -0.0137(10) -0.0174(11) C47 0.0605(13) 0.0446(12) 0.0394(11) 0.0100(9) -0.0256(10) -0.0136(10) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.7613(12) 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 . 2.0915(16) yes Fe1 . C3 . 2.0397(18) yes Fe1 . C4 . 2.0333(19) yes Fe1 . C5 . 2.032(2) yes Fe1 . C6 . 2.0429(17) yes Fe1 . C24 . 2.038(2) yes Fe1 . C25 . 2.046(2) yes Fe1 . C26 . 2.043(2) yes Fe1 . C27 . 2.048(2) yes Fe1 . C28 . 2.040(2) yes C2 . C3 . 1.437(2) yes C2 . C6 . 1.430(2) yes C2 . B7 . 1.627(2) yes C3 . C4 . 1.426(3) yes C3 . H31 . 0.999 no C4 . C5 . 1.416(3) yes C4 . H41 . 0.981 no C5 . C6 . 1.431(3) yes C5 . H51 . 1.001 no C6 . H61 . 1.007 no B7 . C8 . 1.644(2) yes B7 . C15 . 1.660(2) yes B7 . C22 . 1.622(2) yes C8 . C9 . 1.411(2) yes C8 . C14 . 1.405(2) yes C9 . C10 . 1.502(3) yes C9 . C11 . 1.404(2) yes C10 . H101 . 0.965 no C10 . H102 . 0.954 no C10 . H103 . 0.975 no C11 . C12 . 1.378(3) yes C11 . H111 . 0.957 no C12 . C13 . 1.373(3) yes C12 . H121 . 0.975 no C13 . C14 . 1.391(2) yes C13 . H131 . 0.966 no C14 . H141 . 0.943 no C15 . C16 . 1.413(2) yes C15 . C21 . 1.403(2) yes C16 . C17 . 1.500(3) yes C16 . C18 . 1.398(2) yes C17 . H171 . 0.980 no C17 . H173 . 0.967 no C17 . H172 . 0.981 no C18 . C19 . 1.387(3) yes C18 . H181 . 0.974 no C19 . C20 . 1.378(3) yes C19 . H191 . 0.969 no C20 . C21 . 1.393(3) yes C20 . H201 . 0.990 no C21 . H211 . 0.974 no C22 . N23 . 1.150(2) yes C24 . C25 . 1.424(3) yes C24 . C28 . 1.435(4) yes C24 . H241 . 1.007 no C25 . C26 . 1.405(3) yes C25 . H251 . 1.016 no C26 . C27 . 1.421(3) yes C26 . H261 . 1.009 no C27 . C28 . 1.407(4) yes C27 . H271 . 1.018 no C28 . H281 . 1.017 no O30 . C31 . 1.419(2) yes O30 . C47 . 1.419(2) yes C31 . C32 . 1.501(3) yes C31 . H311 . 0.988 no C31 . H312 . 0.996 no C32 . O33 . 1.420(2) yes C32 . H322 . 1.027 no C32 . H321 . 0.998 no O33 . C34 . 1.418(2) yes C34 . C35 . 1.503(3) yes C34 . H341 . 0.991 no C34 . H342 . 0.989 no C35 . O36 . 1.416(2) yes C35 . H351 . 0.981 no C35 . H352 . 1.007 no O36 . C37 . 1.420(2) yes C37 . C38 . 1.497(3) yes C37 . H372 . 0.991 no C37 . H371 . 0.993 no C38 . O39 . 1.421(2) yes C38 . H381 . 1.007 no C38 . H382 . 1.011 no O39 . C40 . 1.418(2) yes C40 . C41 . 1.501(3) yes C40 . H402 . 0.994 no C40 . H401 . 1.022 no C41 . O42 . 1.412(2) yes C41 . H411 . 1.003 no C41 . H412 . 1.037 no O42 . C43 . 1.421(2) yes C43 . C44 . 1.500(3) yes C43 . H431 . 0.980 no C43 . H432 . 1.000 no C44 . O45 . 1.421(2) yes C44 . H442 . 1.029 no C44 . H441 . 0.975 no O45 . C46 . 1.413(2) yes C46 . C47 . 1.508(3) yes C46 . H461 . 1.035 no C46 . H462 . 0.990 no C47 . H471 . 1.004 no C47 . H472 . 1.034 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 . 40.69(6) yes C2 . Fe1 . C4 . 69.30(7) yes C3 . Fe1 . C4 . 40.98(8) yes C2 . Fe1 . C5 . 69.23(7) yes C3 . Fe1 . C5 . 68.49(9) yes C4 . Fe1 . C5 . 40.78(9) yes C2 . Fe1 . C6 . 40.45(7) yes C3 . Fe1 . C6 . 67.74(7) yes C4 . Fe1 . C6 . 68.61(8) yes C5 . Fe1 . C6 . 41.13(7) yes C2 . Fe1 . C24 . 126.57(10) yes C3 . Fe1 . C24 . 107.71(9) yes C4 . Fe1 . C24 . 118.40(9) yes C5 . Fe1 . C24 . 152.69(10) yes C6 . Fe1 . C24 . 164.54(10) yes C2 . Fe1 . C25 . 106.79(8) yes C3 . Fe1 . C25 . 118.31(8) yes C4 . Fe1 . C25 . 152.44(9) yes C5 . Fe1 . C25 . 165.34(9) yes C6 . Fe1 . C25 . 126.98(8) yes C2 . Fe1 . C26 . 118.13(8) yes C3 . Fe1 . C26 . 152.03(9) yes C4 . Fe1 . C26 . 165.93(10) yes C5 . Fe1 . C26 . 128.14(10) yes C6 . Fe1 . C26 . 108.56(9) yes C2 . Fe1 . C27 . 152.58(9) yes C3 . Fe1 . C27 . 165.79(9) yes C4 . Fe1 . C27 . 127.70(9) yes C5 . Fe1 . C27 . 108.34(10) yes C6 . Fe1 . C27 . 119.66(10) yes C2 . Fe1 . C28 . 165.37(10) yes C3 . Fe1 . C28 . 127.93(9) yes C4 . Fe1 . C28 . 107.71(9) yes C5 . Fe1 . C28 . 118.49(10) yes C6 . Fe1 . C28 . 153.12(10) yes C24 . Fe1 . C25 . 40.82(10) yes C24 . Fe1 . C26 . 68.07(10) yes C25 . Fe1 . C26 . 40.20(9) yes C24 . Fe1 . C27 . 68.35(11) yes C25 . Fe1 . C27 . 68.31(10) yes C26 . Fe1 . C27 . 40.67(9) yes C24 . Fe1 . C28 . 41.20(11) yes C25 . Fe1 . C28 . 68.86(10) yes C26 . Fe1 . C28 . 68.20(9) yes C27 . Fe1 . C28 . 40.27(11) yes Fe1 . C2 . C3 . 67.72(9) yes Fe1 . C2 . C6 . 67.95(10) yes C3 . C2 . C6 . 105.04(15) yes Fe1 . C2 . B7 . 130.65(11) yes C3 . C2 . B7 . 127.56(15) yes C6 . C2 . B7 . 127.33(15) yes C2 . C3 . Fe1 . 71.59(9) yes C2 . C3 . C4 . 110.05(17) yes Fe1 . C3 . C4 . 69.27(11) yes C2 . C3 . H31 . 124.5 no Fe1 . C3 . H31 . 125.2 no C4 . C3 . H31 . 125.5 no C3 . C4 . Fe1 . 69.75(10) yes C3 . C4 . C5 . 107.43(16) yes Fe1 . C4 . C5 . 69.54(12) yes C3 . C4 . H41 . 125.9 no Fe1 . C4 . H41 . 124.7 no C5 . C4 . H41 . 126.6 no C4 . C5 . Fe1 . 69.68(11) yes C4 . C5 . C6 . 107.55(17) yes Fe1 . C5 . C6 . 69.86(11) yes C4 . C5 . H51 . 126.2 no Fe1 . C5 . H51 . 123.8 no C6 . C5 . H51 . 126.2 no C5 . C6 . C2 . 109.92(17) yes C5 . C6 . Fe1 . 69.01(10) yes C2 . C6 . Fe1 . 71.61(9) yes C5 . C6 . H61 . 124.9 no C2 . C6 . H61 . 125.1 no Fe1 . C6 . H61 . 122.6 no C2 . B7 . C8 . 110.49(13) yes C2 . B7 . C15 . 111.02(13) yes C8 . B7 . C15 . 116.51(13) yes C2 . B7 . C22 . 106.44(13) yes C8 . B7 . C22 . 107.06(13) yes C15 . B7 . C22 . 104.60(13) yes B7 . C8 . C9 . 123.47(14) yes B7 . C8 . C14 . 120.51(14) yes C9 . C8 . C14 . 115.99(15) yes C8 . C9 . C10 . 121.39(15) yes C8 . C9 . C11 . 120.08(16) yes C10 . C9 . C11 . 118.51(16) yes C9 . C10 . H101 . 110.4 no C9 . C10 . H102 . 112.4 no H101 . C10 . H102 . 108.1 no C9 . C10 . H103 . 110.7 no H101 . C10 . H103 . 107.3 no H102 . C10 . H103 . 107.7 no C9 . C11 . C12 . 121.99(17) yes C9 . C11 . H111 . 118.1 no C12 . C11 . H111 . 119.9 no C11 . C12 . C13 . 118.99(16) yes C11 . C12 . H121 . 120.8 no C13 . C12 . H121 . 120.2 no C12 . C13 . C14 . 119.73(17) yes C12 . C13 . H131 . 120.1 no C14 . C13 . H131 . 120.2 no C8 . C14 . C13 . 123.21(16) yes C8 . C14 . H141 . 119.0 no C13 . C14 . H141 . 117.8 no B7 . C15 . C16 . 123.87(14) yes B7 . C15 . C21 . 120.12(15) yes C16 . C15 . C21 . 115.84(15) yes C15 . C16 . C17 . 121.65(15) yes C15 . C16 . C18 . 120.60(16) yes C17 . C16 . C18 . 117.75(16) yes C16 . C17 . H171 . 112.1 no C16 . C17 . H173 . 111.0 no H171 . C17 . H173 . 108.5 no C16 . C17 . H172 . 111.3 no H171 . C17 . H172 . 106.7 no H173 . C17 . H172 . 107.0 no C16 . C18 . C19 . 121.55(17) yes C16 . C18 . H181 . 118.3 no C19 . C18 . H181 . 120.1 no C18 . C19 . C20 . 119.11(17) yes C18 . C19 . H191 . 120.6 no C20 . C19 . H191 . 120.3 no C19 . C20 . C21 . 119.42(18) yes C19 . C20 . H201 . 120.7 no C21 . C20 . H201 . 119.9 no C15 . C21 . C20 . 123.45(17) yes C15 . C21 . H211 . 118.3 no C20 . C21 . H211 . 118.3 no B7 . C22 . N23 . 179.29(17) yes Fe1 . C24 . C25 . 69.91(12) yes Fe1 . C24 . C28 . 69.49(13) yes C25 . C24 . C28 . 107.8(2) yes Fe1 . C24 . H241 . 125.2 no C25 . C24 . H241 . 124.8 no C28 . C24 . H241 . 127.4 no C24 . C25 . Fe1 . 69.27(13) yes C24 . C25 . C26 . 107.6(2) yes Fe1 . C25 . C26 . 69.80(13) yes C24 . C25 . H251 . 125.9 no Fe1 . C25 . H251 . 123.2 no C26 . C25 . H251 . 126.4 no C25 . C26 . Fe1 . 70.00(12) yes C25 . C26 . C27 . 108.8(2) yes Fe1 . C26 . C27 . 69.83(12) yes C25 . C26 . H261 . 125.0 no Fe1 . C26 . H261 . 122.7 no C27 . C26 . H261 . 126.0 no C26 . C27 . Fe1 . 69.50(12) yes C26 . C27 . C28 . 108.1(2) yes Fe1 . C27 . C28 . 69.58(13) yes C26 . C27 . H271 . 126.6 no Fe1 . C27 . H271 . 125.6 no C28 . C27 . H271 . 125.3 no C24 . C28 . C27 . 107.7(2) yes C24 . C28 . Fe1 . 69.30(12) yes C27 . C28 . Fe1 . 70.15(13) yes C24 . C28 . H281 . 126.2 no C27 . C28 . H281 . 126.0 no Fe1 . C28 . H281 . 123.9 no C31 . O30 . C47 . 111.00(15) yes O30 . C31 . C32 . 109.26(15) yes O30 . C31 . H311 . 109.1 no C32 . C31 . H311 . 110.5 no O30 . C31 . H312 . 109.6 no C32 . C31 . H312 . 110.0 no H311 . C31 . H312 . 108.3 no C31 . C32 . O33 . 109.07(15) yes C31 . C32 . H322 . 111.6 no O33 . C32 . H322 . 110.0 no C31 . C32 . H321 . 109.3 no O33 . C32 . H321 . 108.3 no H322 . C32 . H321 . 108.6 no C32 . O33 . C34 . 112.50(15) yes O33 . C34 . C35 . 108.35(16) yes O33 . C34 . H341 . 109.7 no C35 . C34 . H341 . 111.3 no O33 . C34 . H342 . 110.1 no C35 . C34 . H342 . 110.3 no H341 . C34 . H342 . 107.1 no C34 . C35 . O36 . 109.68(15) yes C34 . C35 . H351 . 109.5 no O36 . C35 . H351 . 110.0 no C34 . C35 . H352 . 109.5 no O36 . C35 . H352 . 109.1 no H351 . C35 . H352 . 109.0 no C35 . O36 . C37 . 110.88(14) yes O36 . C37 . C38 . 109.37(16) yes O36 . C37 . H372 . 109.5 no C38 . C37 . H372 . 111.0 no O36 . C37 . H371 . 108.7 no C38 . C37 . H371 . 110.8 no H372 . C37 . H371 . 107.5 no C37 . C38 . O39 . 107.99(16) yes C37 . C38 . H381 . 109.4 no O39 . C38 . H381 . 108.8 no C37 . C38 . H382 . 110.7 no O39 . C38 . H382 . 110.6 no H381 . C38 . H382 . 109.3 no C38 . O39 . C40 . 112.82(15) yes O39 . C40 . C41 . 108.35(17) yes O39 . C40 . H402 . 109.6 no C41 . C40 . H402 . 110.9 no O39 . C40 . H401 . 108.5 no C41 . C40 . H401 . 110.1 no H402 . C40 . H401 . 109.3 no C40 . C41 . O42 . 108.39(17) yes C40 . C41 . H411 . 111.3 no O42 . C41 . H411 . 109.5 no C40 . C41 . H412 . 109.0 no O42 . C41 . H412 . 108.7 no H411 . C41 . H412 . 109.9 no C41 . O42 . C43 . 112.84(16) yes O42 . C43 . C44 . 108.20(16) yes O42 . C43 . H431 . 109.7 no C44 . C43 . H431 . 109.8 no O42 . C43 . H432 . 108.8 no C44 . C43 . H432 . 110.5 no H431 . C43 . H432 . 109.9 no C43 . C44 . O45 . 108.67(16) yes C43 . C44 . H442 . 110.5 no O45 . C44 . H442 . 109.5 no C43 . C44 . H441 . 110.4 no O45 . C44 . H441 . 109.1 no H442 . C44 . H441 . 108.6 no C44 . O45 . C46 . 111.83(15) yes O45 . C46 . C47 . 108.07(17) yes O45 . C46 . H461 . 110.0 no C47 . C46 . H461 . 109.6 no O45 . C46 . H462 . 110.5 no C47 . C46 . H462 . 111.9 no H461 . C46 . H462 . 106.8 no C46 . C47 . O30 . 109.27(16) yes C46 . C47 . H471 . 109.8 no O30 . C47 . H471 . 109.9 no C46 . C47 . H472 . 108.7 no O30 . C47 . H472 . 108.8 no H471 . C47 . H472 . 110.3 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C21 . H211 . C3 . 132 0.97 2.55 3.284(3) yes