data_cmpd9(up3185) _audit_creation_method SHELXL _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL93. Program for crystal structure refinement. University of Gottingen, Germany, 1993. ; _chemical_formula_sum 'C22 H25 B7 Fe' _chemical_formula_weight 420.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.304(2) _cell_length_b 13.901(3) _cell_length_c 7.5662(14) _cell_angle_alpha 105.688(8) _cell_angle_beta 109.808(13) _cell_angle_gamma 100.349(15) _cell_volume 1027.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.003 _exptl_crystal_density_diffrn 1.361 _exptl_crystal_F_000 436 _exptl_absorpt_coefficient_mu 0.741 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'image plate area detector' _diffrn_measurement_device_type 'Rigaku R-AXIS IIc' _diffrn_measurement_method 'phi oscillations' _diffrn_reflns_number 8252 _diffrn_reflns_av_R_equivalents 0.0519 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 25.38 _reflns_number_total 5746 _reflns_number_observed 5292 _reflns_observed_criterion >2sigma(I) _computing_structure_solution 'SIR92 (Altomare, 1993)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^+2.0796P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0201(22) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 5746 _refine_ls_number_parameters 542 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_obs 0.0607 _refine_ls_wR_factor_all 0.1616 _refine_ls_wR_factor_obs 0.1547 _refine_ls_goodness_of_fit_all 1.081 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.081 _refine_ls_restrained_S_obs 1.082 _refine_ls_shift/esd_max 0.024 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Fe1 Fe 0.44665(8) 0.71590(7) 0.62838(11) 0.0368(3) Uani 1 d . . C2 C 0.2803(7) 0.7366(5) 0.4725(10) 0.037(2) Uani 1 d . . C3 C 0.4665(8) 0.5837(6) 0.4860(12) 0.048(2) Uani 1 d . . C4 C 0.2311(8) 0.6273(7) 0.4683(13) 0.040(2) Uani 1 d . . B5 B 0.3556(8) 0.7312(6) 0.3285(10) 0.032(2) Uani 1 d . . B6 B 0.4595(9) 0.6427(8) 0.3336(13) 0.043(2) Uani 1 d . . B7 B 0.3279(11) 0.5424(7) 0.4891(15) 0.043(2) Uani 1 d . . B8 B 0.1891(8) 0.6493(7) 0.2390(11) 0.037(2) Uani 1 d . . B9 B 0.3535(10) 0.5117(8) 0.2540(14) 0.051(2) Uani 1 d . . B10 B 0.2029(8) 0.5287(7) 0.2521(13) 0.044(2) Uani 1 d . . B11 B 0.2938(9) 0.6002(6) 0.1461(12) 0.040(2) Uani 1 d . . C12 C 0.2188(7) 0.8250(6) 0.5438(10) 0.0352(15) Uani 1 d . . H12 H 0.2837(7) 0.8731(6) 0.6771(10) 0.047 Uiso 1 calc R . C13 C 0.0946(7) 0.7818(6) 0.5687(10) 0.040(2) Uani 1 d . . C14 C 0.1061(8) 0.7487(7) 0.7358(11) 0.049(2) Uani 1 d . . H14 H 0.1884(8) 0.7601(7) 0.8351(11) 0.066 Uiso 1 calc R . C15 C -0.0101(11) 0.6985(8) 0.7464(14) 0.065(3) Uani 1 d . . H15 H -0.0033(11) 0.6739(8) 0.8511(14) 0.086 Uiso 1 calc R . C16 C -0.1328(9) 0.6850(8) 0.6066(13) 0.059(2) Uani 1 d . . H16 H -0.2084(9) 0.6515(8) 0.6155(13) 0.078 Uiso 1 calc R . C17 C -0.1413(8) 0.7220(6) 0.4534(12) 0.043(2) Uani 1 d . . H17 H -0.2243(8) 0.7157(6) 0.3617(12) 0.057 Uiso 1 calc R . C18 C -0.0302(7) 0.7688(6) 0.4297(10) 0.039(2) Uani 1 d . . C19 C -0.0486(7) 0.8030(6) 0.2528(11) 0.043(2) Uani 1 d . . H19A H -0.1168(7) 0.8375(6) 0.2367(11) 0.057 Uiso 1 calc R . H19B H -0.0792(7) 0.7413(6) 0.1325(11) 0.057 Uiso 1 calc R . C20 C 0.0743(8) 0.8762(6) 0.2703(11) 0.042(2) Uani 1 d . . C21 C 0.0583(8) 0.9309(6) 0.1344(11) 0.044(2) Uani 1 d . . H21 H -0.0251(8) 0.9225(6) 0.0414(11) 0.059 Uiso 1 calc R . C22 C 0.1694(10) 0.9973(6) 0.1426(14) 0.058(2) Uani 1 d . . H22 H 0.1596(10) 1.0320(6) 0.0517(14) 0.078 Uiso 1 calc R . C23 C 0.2915(10) 1.0126(7) 0.2800(14) 0.057(2) Uani 1 d . . H23 H 0.3642(10) 1.0581(7) 0.2837(14) 0.076 Uiso 1 calc R . C24 C 0.3086(8) 0.9602(6) 0.4161(11) 0.043(2) Uani 1 d . . H24 H 0.3923(8) 0.9723(6) 0.5125(11) 0.057 Uiso 1 calc R . C25 C 0.1980(7) 0.8884(5) 0.4074(10) 0.039(2) Uani 1 d . . C26 C 0.4804(9) 0.8212(8) 0.9054(11) 0.061(2) Uani 1 d . . H26 H 0.4157(9) 0.8415(8) 0.9426(11) 0.081 Uiso 1 calc R . C27 C 0.5478(9) 0.8700(8) 0.8109(13) 0.057(3) Uani 1 d . . H27 H 0.5357(9) 0.9277(8) 0.7753(13) 0.075 Uiso 1 calc R . C28 C 0.6382(10) 0.8140(9) 0.7799(15) 0.060(3) Uani 1 d . . H28 H 0.6948(10) 0.8279(9) 0.7188(15) 0.080 Uiso 1 calc R . C29 C 0.6252(9) 0.7344(8) 0.8592(12) 0.059(2) Uani 1 d . . H29 H 0.6738(9) 0.6871(8) 0.8621(12) 0.078 Uiso 1 calc R . C30 C 0.5267(10) 0.7376(9) 0.9340(12) 0.062(2) Uani 1 d . . H30 H 0.4979(10) 0.6923(9) 0.9918(12) 0.082 Uiso 1 calc R . Fe1' Fe 0.94641(8) 0.21588(7) 0.52689(10) 0.0368(3) Uani 1 d . . C2' C 0.7783(7) 0.2373(5) 0.5398(11) 0.039(2) Uani 1 d . . C3' C 0.9656(8) 0.0826(7) 0.5589(12) 0.047(2) Uani 1 d . . C5' C 0.7277(9) 0.1256(7) 0.3801(13) 0.044(2) Uani 1 d . . B4' B 0.8560(9) 0.2304(6) 0.7515(12) 0.036(2) Uani 1 d . . B6' B 0.8253(11) 0.0406(8) 0.3739(16) 0.052(3) Uani 1 d . . B7' B 0.9600(9) 0.1427(7) 0.7624(12) 0.044(2) Uani 1 d . . B8' B 0.6875(8) 0.1497(7) 0.5927(14) 0.042(2) Uani 1 d . . B9' B 0.8513(10) 0.0114(8) 0.6028(16) 0.050(2) Uani 1 d . . B10' B 0.7939(9) 0.1000(7) 0.7421(13) 0.042(2) Uani 1 d . . B11' B 0.7024(10) 0.0280(7) 0.4728(14) 0.048(2) Uani 1 d . . C12' C 0.7191(7) 0.3258(6) 0.4939(10) 0.038(2) Uani 1 d . . H12' H 0.7843(7) 0.3738(6) 0.4744(10) 0.051 Uiso 1 calc R . C13' C 0.6975(7) 0.3881(6) 0.6729(11) 0.038(2) Uani 1 d . . C14' C 0.8063(8) 0.4599(6) 0.8430(11) 0.046(2) Uani 1 d . . H14' H 0.8886(8) 0.4729(6) 0.8385(11) 0.062 Uiso 1 calc R . C15' C 0.7953(9) 0.5125(6) 1.0187(12) 0.050(2) Uani 1 d . . H15' H 0.8693(9) 0.5560(6) 1.1341(12) 0.067 Uiso 1 calc R . C16' C 0.6657(9) 0.4970(6) 1.0147(13) 0.056(2) Uani 1 d . . H16' H 0.6539(9) 0.5333(6) 1.1271(13) 0.074 Uiso 1 calc R . C17' C 0.5603(9) 0.4299(7) 0.8481(12) 0.052(2) Uani 1 d . . H17' H 0.4772(9) 0.4186(7) 0.8498(12) 0.070 Uiso 1 calc R . C18' C 0.5731(7) 0.3769(6) 0.6732(11) 0.041(2) Uani 1 d . . C19' C 0.4524(8) 0.3029(6) 0.4940(12) 0.046(2) Uani 1 d . . H19C H 0.3833(8) 0.3365(6) 0.4744(12) 0.061 Uiso 1 calc R . H19D H 0.4228(8) 0.2415(6) 0.5234(12) 0.061 Uiso 1 calc R . C20' C 0.4698(8) 0.2677(6) 0.3004(11) 0.042(2) Uani 1 d . . C21' C 0.3590(9) 0.2218(6) 0.1199(12) 0.051(2) Uani 1 d . . H21' H 0.2761(9) 0.2162(6) 0.1211(12) 0.068 Uiso 1 calc R . C22' C 0.3689(9) 0.1839(7) -0.0626(12) 0.057(2) Uani 1 d . . H22' H 0.2940(9) 0.1486(7) -0.1818(12) 0.075 Uiso 1 calc R . C23' C 0.4932(11) 0.2003(8) -0.0618(13) 0.064(3) Uani 1 d . . H23' H 0.5017(11) 0.1776(8) -0.1831(13) 0.085 Uiso 1 calc R . C24' C 0.6027(9) 0.2485(7) 0.1107(12) 0.054(2) Uani 1 d . . H24' H 0.6850(9) 0.2607(7) 0.1061(12) 0.072 Uiso 1 calc R . C25' C 0.5939(8) 0.2807(6) 0.2984(11) 0.043(2) Uani 1 d . . C26' C 1.0465(10) 0.3697(8) 0.5986(17) 0.062(3) Uani 1 d . . H26' H 1.0339(10) 0.4270(8) 0.6794(17) 0.082 Uiso 1 calc R . C27' C 0.9812(8) 0.3215(9) 0.3918(15) 0.066(3) Uani 1 d . . H27' H 0.9157(8) 0.3417(9) 0.3106(15) 0.088 Uiso 1 calc R . C28' C 1.0269(9) 0.2383(9) 0.3213(13) 0.064(3) Uani 1 d . . H28' H 0.9989(9) 0.1948(9) 0.1883(13) 0.085 Uiso 1 calc R . C29' C 1.1229(8) 0.2337(8) 0.4904(13) 0.056(2) Uani 1 d . . H29' H 1.1701(8) 0.1854(8) 0.4899(13) 0.075 Uiso 1 calc R . C30' C 1.1363(11) 0.3146(9) 0.6627(15) 0.066(3) Uani 1 d . . H30' H 1.1939(11) 0.3290(9) 0.7946(15) 0.088 Uiso 1 calc R . H3 H 0.5555 0.5624 0.5909 0.063 Uiso 1 d . . H4 H 0.1654 0.6191 0.5460 0.063 Uiso 1 d . . H5 H 0.3877 0.8016 0.2967 0.063 Uiso 1 d . . H6 H 0.5464 0.6651 0.3017 0.063 Uiso 1 d . . H7 H 0.3155 0.4913 0.5738 0.063 Uiso 1 d . . H8 H 0.0971 0.6545 0.1348 0.063 Uiso 1 d . . H9 H 0.3565 0.4376 0.1587 0.063 Uiso 1 d . . H10 H 0.1140 0.4604 0.1721 0.063 Uiso 1 d . . H11 H 0.2726 0.5851 -0.0137 0.063 Uiso 1 d . . H3' H 1.0439 0.0623 0.5472 0.063 Uiso 1 d . . H4' H 0.8898 0.3007 0.8869 0.063 Uiso 1 d . . H5' H 0.6616 0.1166 0.2278 0.063 Uiso 1 d . . H6' H 0.8124 -0.0110 0.2255 0.063 Uiso 1 d . . H7' H 1.0474 0.1652 0.9036 0.063 Uiso 1 d . . H8' H 0.5956 0.1553 0.6093 0.063 Uiso 1 d . . H9' H 0.8534 -0.0630 0.6263 0.063 Uiso 1 d . . H10' H 0.7738 0.0850 0.8662 0.063 Uiso 1 d . . H11' H 0.6136 -0.0403 0.3961 0.063 Uiso 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0298(6) 0.0507(7) 0.0321(5) 0.0172(5) 0.0124(5) 0.0136(5) C2 0.041(4) 0.036(4) 0.040(4) 0.013(3) 0.022(3) 0.014(3) C3 0.048(5) 0.053(5) 0.045(4) 0.019(4) 0.018(4) 0.018(4) C4 0.013(4) 0.053(5) 0.048(4) 0.021(4) 0.003(3) 0.010(3) B5 0.030(4) 0.041(4) 0.021(3) 0.013(3) 0.005(3) 0.013(3) B6 0.036(5) 0.062(6) 0.041(4) 0.021(4) 0.020(4) 0.024(4) B7 0.045(6) 0.031(4) 0.053(5) 0.020(4) 0.015(4) 0.011(4) B8 0.027(4) 0.046(5) 0.033(4) 0.012(3) 0.005(3) 0.016(3) B9 0.055(6) 0.047(5) 0.051(5) 0.013(4) 0.026(5) 0.020(4) B10 0.028(4) 0.038(5) 0.052(5) 0.009(4) 0.006(4) 0.013(3) B11 0.042(5) 0.033(4) 0.038(4) 0.007(3) 0.015(4) 0.011(3) C12 0.028(4) 0.042(4) 0.034(3) 0.010(3) 0.011(3) 0.014(3) C13 0.038(4) 0.052(4) 0.030(3) 0.010(3) 0.015(3) 0.015(3) C14 0.045(5) 0.081(6) 0.038(4) 0.027(4) 0.024(4) 0.032(4) C15 0.079(8) 0.074(7) 0.061(6) 0.024(5) 0.051(6) 0.024(5) C16 0.057(6) 0.071(6) 0.060(5) 0.021(4) 0.041(5) 0.020(5) C17 0.033(4) 0.038(4) 0.055(4) 0.006(3) 0.021(4) 0.014(3) C18 0.026(4) 0.052(4) 0.036(3) 0.010(3) 0.013(3) 0.016(3) C19 0.033(4) 0.045(4) 0.045(4) 0.010(3) 0.012(4) 0.017(3) C20 0.038(5) 0.043(4) 0.047(4) 0.015(3) 0.015(4) 0.021(3) C21 0.042(5) 0.047(4) 0.039(4) 0.022(3) 0.003(4) 0.019(3) C22 0.077(7) 0.039(5) 0.070(5) 0.028(4) 0.034(6) 0.020(4) C23 0.064(6) 0.045(5) 0.069(5) 0.028(4) 0.028(5) 0.017(4) C24 0.035(4) 0.038(4) 0.048(4) 0.014(3) 0.007(4) 0.015(3) C25 0.043(5) 0.033(4) 0.041(3) 0.011(3) 0.018(4) 0.014(3) C26 0.044(5) 0.096(7) 0.034(4) 0.011(4) 0.010(4) 0.032(5) C27 0.037(5) 0.069(6) 0.036(4) 0.012(4) -0.008(4) 0.006(4) C28 0.047(6) 0.077(7) 0.045(5) 0.014(5) 0.020(5) 0.004(5) C29 0.047(6) 0.081(7) 0.043(4) 0.023(4) 0.007(4) 0.028(5) C30 0.055(6) 0.091(7) 0.041(4) 0.029(5) 0.018(4) 0.019(5) Fe1' 0.0294(6) 0.0504(7) 0.0315(5) 0.0124(5) 0.0146(5) 0.0129(5) C2' 0.043(4) 0.034(4) 0.049(4) 0.012(3) 0.031(4) 0.014(3) C3' 0.044(5) 0.064(5) 0.053(4) 0.029(4) 0.027(4) 0.033(4) C5' 0.033(5) 0.055(5) 0.040(4) 0.012(4) 0.014(4) 0.013(4) B4' 0.043(5) 0.037(4) 0.035(4) 0.010(3) 0.024(4) 0.014(4) B6' 0.055(6) 0.050(6) 0.052(5) 0.007(4) 0.030(5) 0.019(5) B7' 0.044(5) 0.049(5) 0.035(4) 0.016(4) 0.015(4) 0.010(4) B8' 0.041(5) 0.050(5) 0.061(5) 0.031(4) 0.038(5) 0.023(4) B9' 0.049(6) 0.045(5) 0.067(6) 0.024(4) 0.027(5) 0.022(4) B10' 0.046(5) 0.042(5) 0.052(5) 0.021(4) 0.030(4) 0.015(4) B11' 0.044(5) 0.046(5) 0.051(5) 0.013(4) 0.018(4) 0.015(4) C12' 0.033(4) 0.046(4) 0.042(4) 0.017(3) 0.019(3) 0.017(3) C13' 0.043(4) 0.036(4) 0.046(4) 0.016(3) 0.024(4) 0.020(3) C14' 0.043(5) 0.036(4) 0.051(4) 0.006(3) 0.016(4) 0.009(3) C15' 0.055(5) 0.037(4) 0.049(4) 0.005(3) 0.016(4) 0.013(4) C16' 0.068(6) 0.046(5) 0.056(5) 0.010(4) 0.031(5) 0.027(4) C17' 0.057(5) 0.047(5) 0.059(5) 0.010(4) 0.036(5) 0.019(4) C18' 0.039(4) 0.034(4) 0.050(4) 0.013(3) 0.020(4) 0.013(3) C19' 0.045(5) 0.042(4) 0.054(4) 0.018(4) 0.022(4) 0.017(3) C20' 0.042(5) 0.044(4) 0.046(4) 0.022(3) 0.018(4) 0.022(3) C21' 0.048(5) 0.048(5) 0.054(5) 0.023(4) 0.013(4) 0.013(4) C22' 0.053(6) 0.066(6) 0.040(4) 0.022(4) 0.003(4) 0.017(4) C23' 0.073(7) 0.083(7) 0.040(4) 0.027(5) 0.021(5) 0.030(5) C24' 0.074(6) 0.061(5) 0.050(5) 0.031(4) 0.039(5) 0.029(5) C25' 0.049(5) 0.050(4) 0.044(4) 0.026(3) 0.021(4) 0.026(4) C26' 0.050(6) 0.059(6) 0.085(7) 0.023(5) 0.045(6) 0.005(5) C27' 0.030(5) 0.123(9) 0.068(6) 0.059(6) 0.023(5) 0.027(5) C28' 0.046(5) 0.101(8) 0.043(4) 0.019(5) 0.026(4) 0.013(5) C29' 0.034(5) 0.080(6) 0.066(5) 0.032(5) 0.025(5) 0.025(4) C30' 0.065(7) 0.083(8) 0.038(5) 0.015(5) 0.024(5) -0.003(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C3 1.957(8) . ? Fe1 C2 1.970(8) . ? Fe1 C27 2.062(10) . ? Fe1 C28 2.067(11) . ? Fe1 C26 2.069(8) . ? Fe1 C30 2.089(8) . ? Fe1 C29 2.091(9) . ? Fe1 B5 2.238(7) . ? Fe1 C4 2.244(8) . ? Fe1 B6 2.253(8) . ? Fe1 B7 2.287(9) . ? C2 C4 1.509(11) . ? C2 C12 1.578(9) . ? C2 B5 1.589(9) . ? C2 B8 1.677(10) . ? C3 B6 1.576(11) . ? C3 B7 1.579(13) . ? C3 B9 1.669(13) . ? C4 B10 1.712(12) . ? C4 B7 1.749(13) . ? C4 B8 1.764(11) . ? B5 B11 1.800(11) . ? B5 B8 1.801(11) . ? B5 B6 1.846(12) . ? B6 B11 1.794(12) . ? B6 B9 1.802(14) . ? B7 B10 1.802(14) . ? B7 B9 1.847(13) . ? B8 B11 1.719(11) . ? B8 B10 1.737(12) . ? B9 B10 1.757(12) . ? B9 B11 1.761(13) . ? B10 B11 1.820(12) . ? C12 C25 1.515(9) . ? C12 C13 1.518(9) . ? C13 C18 1.388(11) . ? C13 C14 1.432(10) . ? C14 C15 1.411(12) . ? C15 C16 1.372(14) . ? C16 C17 1.372(11) . ? C17 C18 1.399(10) . ? C18 C19 1.500(10) . ? C19 C20 1.509(10) . ? C20 C25 1.377(11) . ? C20 C21 1.420(10) . ? C21 C22 1.389(12) . ? C22 C23 1.354(13) . ? C23 C24 1.396(11) . ? C24 C25 1.423(10) . ? C26 C30 1.397(14) . ? C26 C27 1.414(13) . ? C27 C28 1.433(15) . ? C28 C29 1.402(14) . ? C29 C30 1.412(13) . ? Fe1' C3' 1.972(8) . ? Fe1' C2' 2.006(7) . ? Fe1' C30' 2.057(11) . ? Fe1' C27' 2.057(9) . ? Fe1' C26' 2.058(10) . ? Fe1' C29' 2.085(8) . ? Fe1' C28' 2.113(7) . ? Fe1' B4' 2.245(7) . ? Fe1' B7' 2.255(8) . ? Fe1' C5' 2.278(9) . ? Fe1' B6' 2.314(11) . ? C2' C5' 1.548(11) . ? C2' C12' 1.566(10) . ? C2' B4' 1.583(11) . ? C2' B8' 1.670(10) . ? C3' B7' 1.569(11) . ? C3' B6' 1.593(15) . ? C3' B9' 1.664(12) . ? C5' B11' 1.710(13) . ? C5' B6' 1.757(14) . ? C5' B8' 1.780(11) . ? B4' B10' 1.795(11) . ? B4' B8' 1.811(13) . ? B4' B7' 1.839(13) . ? B6' B11' 1.791(13) . ? B6' B9' 1.824(15) . ? B7' B10' 1.805(12) . ? B7' B9' 1.815(14) . ? B8' B10' 1.733(12) . ? B8' B11' 1.757(12) . ? B9' B11' 1.731(14) . ? B9' B10' 1.760(12) . ? B10' B11' 1.822(13) . ? C12' C13' 1.520(9) . ? C12' C25' 1.531(11) . ? C13' C18' 1.387(10) . ? C13' C14' 1.399(11) . ? C14' C15' 1.391(10) . ? C15' C16' 1.431(12) . ? C16' C17' 1.351(12) . ? C17' C18' 1.398(10) . ? C18' C19' 1.498(11) . ? C19' C20' 1.505(10) . ? C20' C21' 1.387(11) . ? C20' C25' 1.388(11) . ? C21' C22' 1.389(11) . ? C22' C23' 1.381(13) . ? C23' C24' 1.348(13) . ? C24' C25' 1.412(10) . ? C26' C27' 1.384(14) . ? C26' C30' 1.41(2) . ? C27' C28' 1.399(14) . ? C28' C29' 1.395(13) . ? C29' C30' 1.414(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Fe1 C2 111.5(3) . . ? C3 Fe1 C27 143.7(4) . . ? C2 Fe1 C27 98.3(4) . . ? C3 Fe1 C28 103.2(4) . . ? C2 Fe1 C28 132.3(4) . . ? C27 Fe1 C28 40.6(4) . . ? C3 Fe1 C26 145.8(4) . . ? C2 Fe1 C26 97.1(3) . . ? C27 Fe1 C26 40.0(4) . . ? C28 Fe1 C26 67.3(4) . . ? C3 Fe1 C30 106.5(4) . . ? C2 Fe1 C30 128.0(3) . . ? C27 Fe1 C30 66.9(4) . . ? C28 Fe1 C30 67.0(4) . . ? C26 Fe1 C30 39.2(4) . . ? C3 Fe1 C29 85.8(4) . . ? C2 Fe1 C29 162.6(3) . . ? C27 Fe1 C29 66.6(4) . . ? C28 Fe1 C29 39.4(4) . . ? C26 Fe1 C29 66.0(4) . . ? C30 Fe1 C29 39.5(4) . . ? C3 Fe1 B5 87.3(3) . . ? C2 Fe1 B5 43.8(3) . . ? C27 Fe1 B5 101.3(3) . . ? C28 Fe1 B5 109.4(4) . . ? C26 Fe1 B5 126.9(3) . . ? C30 Fe1 B5 166.1(4) . . ? C29 Fe1 B5 144.2(3) . . ? C3 Fe1 C4 83.3(3) . . ? C2 Fe1 C4 41.3(3) . . ? C27 Fe1 C4 132.7(4) . . ? C28 Fe1 C4 173.0(4) . . ? C26 Fe1 C4 108.6(4) . . ? C30 Fe1 C4 113.8(4) . . ? C29 Fe1 C4 145.2(3) . . ? B5 Fe1 C4 68.1(3) . . ? C3 Fe1 B6 43.3(3) . . ? C2 Fe1 B6 87.4(3) . . ? C27 Fe1 B6 122.1(4) . . ? C28 Fe1 B6 96.8(4) . . ? C26 Fe1 B6 162.0(4) . . ? C30 Fe1 B6 143.6(4) . . ? C29 Fe1 B6 107.6(3) . . ? B5 Fe1 B6 48.5(3) . . ? C4 Fe1 B6 86.3(3) . . ? C3 Fe1 B7 42.8(4) . . ? C2 Fe1 B7 84.5(3) . . ? C27 Fe1 B7 167.0(3) . . ? C28 Fe1 B7 141.6(4) . . ? C26 Fe1 B7 127.2(4) . . ? C30 Fe1 B7 101.4(4) . . ? C29 Fe1 B7 108.4(4) . . ? B5 Fe1 B7 89.5(3) . . ? C4 Fe1 B7 45.4(3) . . ? B6 Fe1 B7 70.5(4) . . ? C4 C2 C12 121.3(6) . . ? C4 C2 B5 108.1(6) . . ? C12 C2 B5 127.0(6) . . ? C4 C2 B8 67.0(5) . . ? C12 C2 B8 114.9(6) . . ? B5 C2 B8 66.9(5) . . ? C4 C2 Fe1 79.1(4) . . ? C12 C2 Fe1 127.5(5) . . ? B5 C2 Fe1 77.1(4) . . ? B8 C2 Fe1 117.6(5) . . ? B6 C3 B7 112.4(7) . . ? B6 C3 B9 67.4(6) . . ? B7 C3 B9 69.3(6) . . ? B6 C3 Fe1 78.4(5) . . ? B7 C3 Fe1 79.8(5) . . ? B9 C3 Fe1 118.6(6) . . ? C2 C4 B10 115.0(7) . . ? C2 C4 B7 123.4(6) . . ? B10 C4 B7 62.7(5) . . ? C2 C4 B8 61.1(5) . . ? B10 C4 B8 60.0(5) . . ? B7 C4 B8 113.1(6) . . ? C2 C4 Fe1 59.6(4) . . ? B10 C4 Fe1 109.8(5) . . ? B7 C4 Fe1 68.6(4) . . ? B8 C4 Fe1 101.7(5) . . ? C2 B5 B11 108.1(6) . . ? C2 B5 B8 58.9(4) . . ? B11 B5 B8 57.0(4) . . ? C2 B5 B6 116.6(5) . . ? B11 B5 B6 58.9(5) . . ? B8 B5 B6 106.3(6) . . ? C2 B5 Fe1 59.1(3) . . ? B11 B5 Fe1 105.8(4) . . ? B8 B5 Fe1 100.7(4) . . ? B6 B5 Fe1 66.2(3) . . ? C3 B6 B11 109.1(7) . . ? C3 B6 B9 58.8(5) . . ? B11 B6 B9 58.6(5) . . ? C3 B6 B5 115.9(6) . . ? B11 B6 B5 59.3(4) . . ? B9 B6 B5 107.5(6) . . ? C3 B6 Fe1 58.3(4) . . ? B11 B6 Fe1 105.4(4) . . ? B9 B6 Fe1 100.1(4) . . ? B5 B6 Fe1 65.3(3) . . ? C3 B7 C4 114.5(6) . . ? C3 B7 B10 107.7(7) . . ? C4 B7 B10 57.6(5) . . ? C3 B7 B9 57.7(5) . . ? C4 B7 B9 104.0(6) . . ? B10 B7 B9 57.5(5) . . ? C3 B7 Fe1 57.4(4) . . ? C4 B7 Fe1 66.0(4) . . ? B10 B7 Fe1 104.7(5) . . ? B9 B7 Fe1 97.5(5) . . ? C2 B8 B11 107.9(6) . . ? C2 B8 B10 105.5(6) . . ? B11 B8 B10 63.5(5) . . ? C2 B8 C4 51.9(4) . . ? B11 B8 C4 102.3(6) . . ? B10 B8 C4 58.5(5) . . ? C2 B8 B5 54.2(4) . . ? B11 B8 B5 61.4(4) . . ? B10 B8 B5 105.5(5) . . ? C4 B8 B5 89.4(5) . . ? C3 B9 B10 105.8(6) . . ? C3 B9 B11 106.5(7) . . ? B10 B9 B11 62.3(5) . . ? C3 B9 B6 53.8(5) . . ? B10 B9 B6 104.5(6) . . ? B11 B9 B6 60.4(5) . . ? C3 B9 B7 53.1(5) . . ? B10 B9 B7 59.9(5) . . ? B11 B9 B7 104.0(6) . . ? B6 B9 B7 91.8(6) . . ? C4 B10 B8 61.5(5) . . ? C4 B10 B9 109.6(6) . . ? B8 B10 B9 111.8(6) . . ? C4 B10 B7 59.6(5) . . ? B8 B10 B7 111.8(6) . . ? B9 B10 B7 62.5(5) . . ? C4 B10 B11 100.3(6) . . ? B8 B10 B11 57.8(4) . . ? B9 B10 B11 59.0(5) . . ? B7 B10 B11 103.5(6) . . ? B8 B11 B9 112.5(6) . . ? B8 B11 B6 112.3(6) . . ? B9 B11 B6 60.9(5) . . ? B8 B11 B5 61.5(4) . . ? B9 B11 B5 111.5(6) . . ? B6 B11 B5 61.8(5) . . ? B8 B11 B10 58.7(5) . . ? B9 B11 B10 58.7(5) . . ? B6 B11 B10 102.3(5) . . ? B5 B11 B10 102.2(5) . . ? C25 C12 C13 112.6(6) . . ? C25 C12 C2 111.2(5) . . ? C13 C12 C2 112.1(6) . . ? C18 C13 C14 118.9(7) . . ? C18 C13 C12 122.1(6) . . ? C14 C13 C12 118.9(7) . . ? C15 C14 C13 118.6(8) . . ? C16 C15 C14 121.8(8) . . ? C17 C16 C15 118.5(8) . . ? C16 C17 C18 122.6(8) . . ? C13 C18 C17 119.5(7) . . ? C13 C18 C19 121.4(6) . . ? C17 C18 C19 119.1(7) . . ? C18 C19 C20 114.2(7) . . ? C25 C20 C21 120.5(7) . . ? C25 C20 C19 122.4(7) . . ? C21 C20 C19 117.2(7) . . ? C22 C21 C20 118.9(8) . . ? C23 C22 C21 121.5(8) . . ? C22 C23 C24 120.2(8) . . ? C23 C24 C25 120.0(8) . . ? C20 C25 C24 118.8(7) . . ? C20 C25 C12 121.5(6) . . ? C24 C25 C12 119.7(7) . . ? C30 C26 C27 109.0(8) . . ? C30 C26 Fe1 71.2(5) . . ? C27 C26 Fe1 69.7(5) . . ? C26 C27 C28 107.2(9) . . ? C26 C27 Fe1 70.2(6) . . ? C28 C27 Fe1 69.9(6) . . ? C29 C28 C27 107.1(9) . . ? C29 C28 Fe1 71.2(6) . . ? C27 C28 Fe1 69.5(6) . . ? C28 C29 C30 109.2(9) . . ? C28 C29 Fe1 69.4(6) . . ? C30 C29 Fe1 70.2(6) . . ? C26 C30 C29 107.5(8) . . ? C26 C30 Fe1 69.6(5) . . ? C29 C30 Fe1 70.3(5) . . ? C3' Fe1' C2' 110.8(3) . . ? C3' Fe1' C30' 104.2(4) . . ? C2' Fe1' C30' 131.7(4) . . ? C3' Fe1' C27' 146.3(3) . . ? C2' Fe1' C27' 97.8(3) . . ? C30' Fe1' C27' 66.0(4) . . ? C3' Fe1' C26' 144.2(4) . . ? C2' Fe1' C26' 98.1(3) . . ? C30' Fe1' C26' 40.2(4) . . ? C27' Fe1' C26' 39.3(4) . . ? C3' Fe1' C29' 86.3(3) . . ? C2' Fe1' C29' 162.7(3) . . ? C30' Fe1' C29' 39.9(4) . . ? C27' Fe1' C29' 65.3(3) . . ? C26' Fe1' C29' 66.9(4) . . ? C3' Fe1' C28' 107.1(4) . . ? C2' Fe1' C28' 128.6(3) . . ? C30' Fe1' C28' 66.4(4) . . ? C27' Fe1' C28' 39.2(4) . . ? C26' Fe1' C28' 66.7(4) . . ? C29' Fe1' C28' 38.8(3) . . ? C3' Fe1' B4' 86.6(3) . . ? C2' Fe1' B4' 43.3(3) . . ? C30' Fe1' B4' 109.8(3) . . ? C27' Fe1' B4' 127.1(4) . . ? C26' Fe1' B4' 101.6(3) . . ? C29' Fe1' B4' 144.9(3) . . ? C28' Fe1' B4' 166.3(4) . . ? C3' Fe1' B7' 42.9(3) . . ? C2' Fe1' B7' 86.8(3) . . ? C30' Fe1' B7' 97.5(4) . . ? C27' Fe1' B7' 161.4(4) . . ? C26' Fe1' B7' 122.3(4) . . ? C29' Fe1' B7' 108.1(3) . . ? C28' Fe1' B7' 143.6(4) . . ? B4' Fe1' B7' 48.2(3) . . ? C3' Fe1' C5' 82.9(3) . . ? C2' Fe1' C5' 41.8(3) . . ? C30' Fe1' C5' 172.6(5) . . ? C27' Fe1' C5' 109.4(3) . . ? C26' Fe1' C5' 132.6(4) . . ? C29' Fe1' C5' 144.6(3) . . ? C28' Fe1' C5' 114.1(3) . . ? B4' Fe1' C5' 67.9(3) . . ? B7' Fe1' C5' 86.1(3) . . ? C3' Fe1' B6' 42.7(4) . . ? C2' Fe1' B6' 84.3(3) . . ? C30' Fe1' B6' 142.4(5) . . ? C27' Fe1' B6' 128.1(4) . . ? C26' Fe1' B6' 167.3(4) . . ? C29' Fe1' B6' 108.5(4) . . ? C28' Fe1' B6' 102.1(4) . . ? B4' Fe1' B6' 88.7(3) . . ? B7' Fe1' B6' 70.2(4) . . ? C5' Fe1' B6' 45.0(4) . . ? C5' C2' C12' 121.1(7) . . ? C5' C2' B4' 107.7(6) . . ? C12' C2' B4' 128.5(6) . . ? C5' C2' B8' 67.0(5) . . ? C12' C2' B8' 116.0(6) . . ? B4' C2' B8' 67.6(5) . . ? C5' C2' Fe1' 78.6(4) . . ? C12' C2' Fe1' 126.2(4) . . ? B4' C2' Fe1' 76.4(4) . . ? B8' C2' Fe1' 117.7(5) . . ? B7' C3' B6' 112.4(6) . . ? B7' C3' B9' 68.2(5) . . ? B6' C3' B9' 68.1(6) . . ? B7' C3' Fe1' 78.2(5) . . ? B6' C3' Fe1' 80.2(5) . . ? B9' C3' Fe1' 118.3(5) . . ? C2' C5' B11' 113.9(7) . . ? C2' C5' B6' 123.1(7) . . ? B11' C5' B6' 62.2(6) . . ? C2' C5' B8' 59.8(5) . . ? B11' C5' B8' 60.4(5) . . ? B6' C5' B8' 113.0(7) . . ? C2' C5' Fe1' 59.7(4) . . ? B11' C5' Fe1' 109.1(6) . . ? B6' C5' Fe1' 68.6(5) . . ? B8' C5' Fe1' 101.2(5) . . ? C2' B4' B10' 108.5(6) . . ? C2' B4' B8' 58.5(4) . . ? B10' B4' B8' 57.4(5) . . ? C2' B4' B7' 117.9(5) . . ? B10' B4' B7' 59.5(5) . . ? B8' B4' B7' 107.3(6) . . ? C2' B4' Fe1' 60.3(3) . . ? B10' B4' Fe1' 106.4(4) . . ? B8' B4' Fe1' 101.4(4) . . ? B7' B4' Fe1' 66.2(3) . . ? C3' B6' C5' 114.7(7) . . ? C3' B6' B11' 107.5(7) . . ? C5' B6' B11' 57.6(5) . . ? C3' B6' B9' 57.8(6) . . ? C5' B6' B9' 104.0(6) . . ? B11' B6' B9' 57.2(5) . . ? C3' B6' Fe1' 57.1(4) . . ? C5' B6' Fe1' 66.4(5) . . ? B11' B6' Fe1' 104.7(5) . . ? B9' B6' Fe1' 97.4(6) . . ? C3' B7' B10' 109.0(7) . . ? C3' B7' B9' 58.4(5) . . ? B10' B7' B9' 58.2(5) . . ? C3' B7' B4' 116.3(6) . . ? B10' B7' B4' 59.0(5) . . ? B9' B7' B4' 106.6(6) . . ? C3' B7' Fe1' 58.9(4) . . ? B10' B7' Fe1' 105.7(5) . . ? B9' B7' Fe1' 99.8(5) . . ? B4' B7' Fe1' 65.6(3) . . ? C2' B8' B10' 107.5(6) . . ? C2' B8' B11' 105.7(5) . . ? B10' B8' B11' 63.0(5) . . ? C2' B8' C5' 53.2(4) . . ? B10' B8' C5' 101.8(6) . . ? B11' B8' C5' 57.8(5) . . ? C2' B8' B4' 53.9(4) . . ? B10' B8' B4' 60.8(5) . . ? B11' B8' B4' 104.2(6) . . ? C5' B8' B4' 89.5(5) . . ? C3' B9' B11' 107.1(7) . . ? C3' B9' B10' 106.8(6) . . ? B11' B9' B10' 62.9(5) . . ? C3' B9' B7' 53.4(5) . . ? B11' B9' B7' 105.2(7) . . ? B10' B9' B7' 60.6(5) . . ? C3' B9' B6' 54.1(5) . . ? B11' B9' B6' 60.4(6) . . ? B10' B9' B6' 105.1(6) . . ? B7' B9' B6' 92.5(6) . . ? B8' B10' B9' 112.1(6) . . ? B8' B10' B4' 61.8(5) . . ? B9' B10' B4' 111.0(5) . . ? B8' B10' B7' 112.4(5) . . ? B9' B10' B7' 61.2(5) . . ? B4' B10' B7' 61.4(5) . . ? B8' B10' B11' 59.2(5) . . ? B9' B10' B11' 57.8(5) . . ? B4' B10' B11' 102.2(6) . . ? B7' B10' B11' 102.0(5) . . ? C5' B11' B9' 110.1(7) . . ? C5' B11' B8' 61.7(5) . . ? B9' B11' B8' 112.3(7) . . ? C5' B11' B6' 60.2(5) . . ? B9' B11' B6' 62.3(6) . . ? B8' B11' B6' 112.5(7) . . ? C5' B11' B10' 100.9(6) . . ? B9' B11' B10' 59.3(5) . . ? B8' B11' B10' 57.9(5) . . ? B6' B11' B10' 103.9(7) . . ? C13' C12' C25' 112.9(6) . . ? C13' C12' C2' 110.3(5) . . ? C25' C12' C2' 111.0(6) . . ? C18' C13' C14' 118.6(6) . . ? C18' C13' C12' 122.3(7) . . ? C14' C13' C12' 119.1(6) . . ? C15' C14' C13' 122.2(7) . . ? C14' C15' C16' 117.3(8) . . ? C17' C16' C15' 120.2(7) . . ? C16' C17' C18' 121.7(7) . . ? C13' C18' C17' 119.6(7) . . ? C13' C18' C19' 121.2(6) . . ? C17' C18' C19' 119.1(7) . . ? C18' C19' C20' 115.3(6) . . ? C21' C20' C25' 119.4(7) . . ? C21' C20' C19' 119.1(7) . . ? C25' C20' C19' 121.5(7) . . ? C20' C21' C22' 121.6(8) . . ? C23' C22' C21' 118.0(8) . . ? C24' C23' C22' 121.5(8) . . ? C23' C24' C25' 120.9(8) . . ? C20' C25' C24' 118.4(7) . . ? C20' C25' C12' 121.4(6) . . ? C24' C25' C12' 120.2(7) . . ? C27' C26' C30' 106.3(9) . . ? C27' C26' Fe1' 70.3(6) . . ? C30' C26' Fe1' 69.9(6) . . ? C26' C27' C28' 111.0(9) . . ? C26' C27' Fe1' 70.4(5) . . ? C28' C27' Fe1' 72.6(6) . . ? C29' C28' C27' 106.2(8) . . ? C29' C28' Fe1' 69.5(4) . . ? C27' C28' Fe1' 68.3(4) . . ? C28' C29' C30' 108.7(9) . . ? C28' C29' Fe1' 71.7(4) . . ? C30' C29' Fe1' 69.0(5) . . ? C29' C30' C26' 107.8(9) . . ? C29' C30' Fe1' 71.1(6) . . ? C26' C30' Fe1' 69.9(6) . . ? _refine_diff_density_max 0.507 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.072