data_061112am _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H108 B6 F24 Fe3 N54' _chemical_formula_weight 2418.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 19.0308(13) _cell_length_b 19.0308(13) _cell_length_c 25.288(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 7931.7(11) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2435 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 23.6 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.519 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3726 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8517 _exptl_absorpt_correction_T_max 0.8771 _exptl_absorpt_process_details 'SADABS; Bruker(2000)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16157 _diffrn_reflns_av_R_equivalents 0.1171 _diffrn_reflns_av_sigmaI/netI 0.1797 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 28.02 _reflns_number_total 4171 _reflns_number_gt 1861 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4171 _refine_ls_number_parameters 268 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.2237 _refine_ls_R_factor_gt 0.1082 _refine_ls_wR_factor_ref 0.1879 _refine_ls_wR_factor_gt 0.1489 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Fe1 Fe 1.0000 0.0000 0.33736(6) 0.0210(3) Uani 1 3 d S . . Fe2 Fe 0.6667 0.3333 0.3333 0.0701(9) Uani 1 6 d S . . C1 C 1.1795(3) 0.0996(3) 0.3857(2) 0.0397(16) Uani 1 1 d . . . H1 H 1.1960 0.1402 0.3602 0.048 Uiso 1 1 calc R . . C2 C 1.1125(4) -0.0031(3) 0.4313(3) 0.0449(17) Uani 1 1 d . . . H2 H 1.0692 -0.0515 0.4436 0.054 Uiso 1 1 calc R . . C3 C 0.8852(3) 0.0114(3) 0.2500(3) 0.0489(18) Uani 1 1 d . . . H3 H 0.9285 0.0601 0.2381 0.059 Uiso 1 1 calc R . . C4 C 0.8185(3) -0.0956(3) 0.2917(2) 0.0404(15) Uani 1 1 d . . . H4 H 0.8025 -0.1388 0.3149 0.048 Uiso 1 1 calc R . . C5 C 1.3132(3) 0.1546(3) 0.4333(2) 0.0482(17) Uani 1 1 d . . . H5A H 1.3343 0.1942 0.4050 0.058 Uiso 1 1 calc R . . H5B H 1.3416 0.1242 0.4322 0.058 Uiso 1 1 calc R . . C6 C 1.3314(3) 0.1992(3) 0.4856(3) 0.0472(17) Uani 1 1 d . . . H6A H 1.2931 0.2180 0.4909 0.057 Uiso 1 1 calc R . . H6B H 1.3853 0.2465 0.4840 0.057 Uiso 1 1 calc R . . C7 C 0.6818(3) -0.1425(4) 0.2519(3) 0.0505(17) Uani 1 1 d . . . H7A H 0.6545 -0.1111 0.2549 0.061 Uiso 1 1 calc R . . H7B H 0.6623 -0.1821 0.2802 0.061 Uiso 1 1 calc R . . C8 C 0.6604(3) -0.1863(3) 0.1993(3) 0.0465(17) Uani 1 1 d . . . H8A H 0.6058 -0.2324 0.2015 0.056 Uiso 1 1 calc R . . H8B H 0.6969 -0.2071 0.1930 0.056 Uiso 1 1 calc R . . C9 C 0.5543(5) 0.1611(5) 0.3839(4) 0.074(2) Uani 1 1 d . . . H9 H 0.5696 0.1360 0.3584 0.089 Uiso 1 1 calc R . . C10 C 0.5414(4) 0.2454(5) 0.4297(4) 0.092(3) Uani 1 1 d . . . H10 H 0.5467 0.2941 0.4414 0.110 Uiso 1 1 calc R . . C11 C 0.4691(5) 0.0388(4) 0.4410(3) 0.086(3) Uani 1 1 d . . . H11A H 0.4760 0.0071 0.4136 0.103 Uiso 1 1 calc R . . H11B H 0.4115 0.0171 0.4468 0.103 Uiso 1 1 calc R . . C12 C 0.5109(7) 0.0359(4) 0.4925(4) 0.139(4) Uani 1 1 d . . . H12A H 0.5692 0.0653 0.4871 0.167 Uiso 1 1 calc R . . H12B H 0.4986 0.0633 0.5202 0.167 Uiso 1 1 calc R . . N1 N 1.1064(3) 0.0357(3) 0.38854(19) 0.0327(12) Uani 1 1 d . . . N2 N 1.2263(3) 0.0985(3) 0.4238(2) 0.0378(12) Uani 1 1 d . . . N3 N 1.1839(3) 0.0321(3) 0.4544(2) 0.0507(15) Uani 1 1 d . . . N4 N 0.8936(3) -0.0330(3) 0.28789(18) 0.0324(12) Uani 1 1 d . . . N5 N 0.7698(3) -0.0880(3) 0.2579(2) 0.0402(13) Uani 1 1 d . . . N6 N 0.8119(3) -0.0184(3) 0.2307(2) 0.0582(17) Uani 1 1 d . . . N7 N 0.5758(3) 0.2396(4) 0.3845(3) 0.076(2) Uani 1 1 d . . . N8 N 0.5083(4) 0.1249(4) 0.4253(3) 0.0690(19) Uani 1 1 d . . . N9 N 0.5000(4) 0.1775(5) 0.4559(3) 0.088(2) Uani 1 1 d . . . B1 B 0.3332(4) 0.0254(4) 0.3087(3) 0.095(4) Uani 1 1 d D . . F1 F 0.3331(4) -0.0442(4) 0.3145(3) 0.197(3) Uani 1 1 d D A . F2 F 0.4021(9) 0.0909(8) 0.3240(8) 0.145(8) Uani 0.517(19) 1 d PD A 1 F3 F 0.2789(8) 0.0428(12) 0.2881(13) 0.207(12) Uani 0.517(19) 1 d PD A 1 F4 F 0.2716(6) 0.0129(8) 0.3405(6) 0.107(6) Uani 0.517(19) 1 d PD A 1 F2' F 0.4064(8) 0.0811(9) 0.2900(12) 0.141(9) Uani 0.483(19) 1 d PD A 2 F3' F 0.3176(12) 0.0163(8) 0.2569(4) 0.126(7) Uani 0.483(19) 1 d PD A 2 F4' F 0.332(3) 0.0352(18) 0.3611(4) 0.264(14) Uani 0.483(19) 1 d PD A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0233(4) 0.0233(4) 0.0163(7) 0.000 0.000 0.0117(2) Fe2 0.0528(11) 0.0528(11) 0.105(3) 0.000 0.000 0.0264(5) C1 0.045(4) 0.047(4) 0.036(4) -0.005(3) -0.011(3) 0.029(3) C2 0.048(4) 0.027(3) 0.049(5) 0.005(3) -0.005(3) 0.010(3) C3 0.037(4) 0.038(4) 0.050(5) 0.004(3) -0.018(3) 0.002(3) C4 0.042(4) 0.038(4) 0.034(4) 0.015(3) 0.008(3) 0.015(3) C5 0.033(4) 0.058(4) 0.046(5) 0.002(3) -0.003(3) 0.018(3) C6 0.029(3) 0.044(4) 0.056(5) -0.006(3) -0.016(3) 0.009(3) C7 0.028(3) 0.075(5) 0.041(4) -0.010(4) -0.007(3) 0.021(3) C8 0.031(3) 0.050(4) 0.050(5) -0.011(3) -0.012(3) 0.014(3) C9 0.067(6) 0.073(6) 0.085(7) -0.013(5) -0.007(5) 0.039(5) C10 0.055(5) 0.066(6) 0.160(11) -0.020(6) 0.017(6) 0.034(5) C11 0.100(6) 0.070(6) 0.078(7) 0.014(5) -0.021(5) 0.036(5) C12 0.236(11) 0.087(8) 0.079(8) -0.010(7) -0.046(8) 0.069(10) N1 0.028(3) 0.026(3) 0.039(3) -0.004(2) -0.003(2) 0.010(2) N2 0.029(3) 0.036(3) 0.037(3) -0.005(2) -0.009(2) 0.008(2) N3 0.048(3) 0.042(3) 0.051(4) 0.006(3) -0.021(3) 0.014(3) N4 0.037(3) 0.033(3) 0.030(3) 0.003(2) -0.004(2) 0.020(2) N5 0.032(3) 0.047(3) 0.040(4) -0.001(3) -0.007(2) 0.019(3) N6 0.053(4) 0.038(3) 0.067(5) 0.010(3) -0.022(3) 0.010(3) N7 0.055(4) 0.056(4) 0.119(7) -0.003(4) 0.013(4) 0.029(3) N8 0.054(4) 0.073(5) 0.088(6) -0.018(4) -0.018(4) 0.038(4) N9 0.065(5) 0.076(5) 0.128(7) 0.006(5) 0.021(4) 0.039(4) B1 0.083(9) 0.089(10) 0.128(13) 0.016(9) 0.041(10) 0.053(8) F1 0.194(6) 0.145(6) 0.286(11) 0.040(6) 0.085(6) 0.112(5) F2 0.069(9) 0.128(11) 0.110(15) -0.002(9) -0.025(7) -0.047(7) F3 0.120(11) 0.262(19) 0.26(3) 0.126(19) 0.024(14) 0.109(11) F4 0.065(7) 0.111(9) 0.146(14) -0.027(9) 0.005(7) 0.046(7) F2' 0.122(13) 0.105(11) 0.20(2) 0.037(11) 0.045(12) 0.062(11) F3' 0.139(16) 0.157(12) 0.049(8) -0.035(8) -0.041(8) 0.049(10) F4' 0.34(4) 0.29(3) 0.18(2) -0.06(2) 0.03(2) 0.17(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 N4 2.189(4) 2_645 ? Fe1 N4 2.189(4) . ? Fe1 N4 2.189(4) 3_765 ? Fe1 N1 2.205(4) . ? Fe1 N1 2.205(4) 3_765 ? Fe1 N1 2.205(4) 2_645 ? Fe2 N7 2.182(6) 17 ? Fe2 N7 2.182(6) 2_655 ? Fe2 N7 2.182(6) . ? Fe2 N7 2.182(6) 3_665 ? Fe2 N7 2.182(6) 16_655 ? Fe2 N7 2.182(6) 18_545 ? C1 N1 1.315(6) . ? C1 N2 1.321(6) . ? C1 H1 0.9300 . ? C2 N3 1.314(6) . ? C2 N1 1.346(6) . ? C2 H2 0.9300 . ? C3 N6 1.309(6) . ? C3 N4 1.340(6) . ? C3 H3 0.9300 . ? C4 N5 1.320(6) . ? C4 N4 1.329(6) . ? C4 H4 0.9300 . ? C5 N2 1.473(6) . ? C5 C6 1.513(7) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C8 1.524(8) 4 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 N5 1.472(6) . ? C7 C8 1.512(7) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C6 1.524(8) 7_444 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 N8 1.316(9) . ? C9 N7 1.338(8) . ? C9 H9 0.9300 . ? C10 N9 1.307(9) . ? C10 N7 1.349(9) . ? C10 H10 0.9300 . ? C11 N8 1.475(8) . ? C11 C12 1.541(10) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C12 1.273(13) 10_656 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N2 N3 1.351(6) . ? N5 N6 1.344(6) . ? N8 N9 1.335(8) . ? B1 F1 1.333(5) . ? B1 F3' 1.335(5) . ? B1 F2 1.337(5) . ? B1 F3 1.338(5) . ? B1 F4 1.341(5) . ? B1 F4' 1.342(5) . ? B1 F2' 1.346(5) . ? 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 N4 Fe1 N4 90.57(17) 2_645 . ? N4 Fe1 N4 90.57(17) 2_645 3_765 ? N4 Fe1 N4 90.57(17) . 3_765 ? N4 Fe1 N1 91.12(16) 2_645 . ? N4 Fe1 N1 178.30(17) . . ? N4 Fe1 N1 89.29(16) 3_765 . ? N4 Fe1 N1 89.29(16) 2_645 3_765 ? N4 Fe1 N1 91.12(16) . 3_765 ? N4 Fe1 N1 178.31(17) 3_765 3_765 ? N1 Fe1 N1 89.03(18) . 3_765 ? N4 Fe1 N1 178.31(17) 2_645 2_645 ? N4 Fe1 N1 89.29(16) . 2_645 ? N4 Fe1 N1 91.12(16) 3_765 2_645 ? N1 Fe1 N1 89.03(18) . 2_645 ? N1 Fe1 N1 89.03(18) 3_765 2_645 ? N7 Fe2 N7 179.997(1) 17 2_655 ? N7 Fe2 N7 91.6(3) 17 . ? N7 Fe2 N7 88.4(3) 2_655 . ? N7 Fe2 N7 91.6(3) 17 3_665 ? N7 Fe2 N7 88.4(3) 2_655 3_665 ? N7 Fe2 N7 88.4(3) . 3_665 ? N7 Fe2 N7 88.4(3) 17 16_655 ? N7 Fe2 N7 91.6(3) 2_655 16_655 ? N7 Fe2 N7 179.997(1) . 16_655 ? N7 Fe2 N7 91.6(3) 3_665 16_655 ? N7 Fe2 N7 88.4(3) 17 18_545 ? N7 Fe2 N7 91.6(3) 2_655 18_545 ? N7 Fe2 N7 91.6(3) . 18_545 ? N7 Fe2 N7 179.999(1) 3_665 18_545 ? N7 Fe2 N7 88.4(3) 16_655 18_545 ? N1 C1 N2 110.7(5) . . ? N1 C1 H1 124.6 . . ? N2 C1 H1 124.6 . . ? N3 C2 N1 115.4(5) . . ? N3 C2 H2 122.3 . . ? N1 C2 H2 122.3 . . ? N6 C3 N4 115.4(5) . . ? N6 C3 H3 122.3 . . ? N4 C3 H3 122.3 . . ? N5 C4 N4 110.8(5) . . ? N5 C4 H4 124.6 . . ? N4 C4 H4 124.6 . . ? N2 C5 C6 114.1(5) . . ? N2 C5 H5A 108.7 . . ? C6 C5 H5A 108.7 . . ? N2 C5 H5B 108.7 . . ? C6 C5 H5B 108.7 . . ? H5A C5 H5B 107.6 . . ? C5 C6 C8 113.2(5) . 4 ? C5 C6 H6A 108.9 . . ? C8 C6 H6A 108.9 4 . ? C5 C6 H6B 108.9 . . ? C8 C6 H6B 108.9 4 . ? H6A C6 H6B 107.7 . . ? N5 C7 C8 112.2(5) . . ? N5 C7 H7A 109.2 . . ? C8 C7 H7A 109.2 . . ? N5 C7 H7B 109.2 . . ? C8 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C6 114.6(5) . 7_444 ? C7 C8 H8A 108.6 . . ? C6 C8 H8A 108.6 7_444 . ? C7 C8 H8B 108.6 . . ? C6 C8 H8B 108.6 7_444 . ? H8A C8 H8B 107.6 . . ? N8 C9 N7 109.1(7) . . ? N8 C9 H9 125.5 . . ? N7 C9 H9 125.5 . . ? N9 C10 N7 115.2(8) . . ? N9 C10 H10 122.4 . . ? N7 C10 H10 122.4 . . ? N8 C11 C12 106.5(6) . . ? N8 C11 H11A 110.4 . . ? C12 C11 H11A 110.4 . . ? N8 C11 H11B 110.4 . . ? C12 C11 H11B 110.4 . . ? H11A C11 H11B 108.6 . . ? C12 C12 C11 113.3(11) 10_656 . ? C12 C12 H12A 108.9 10_656 . ? C11 C12 H12A 108.9 . . ? C12 C12 H12B 108.9 10_656 . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.7 . . ? C1 N1 C2 102.1(5) . . ? C1 N1 Fe1 129.5(4) . . ? C2 N1 Fe1 128.4(4) . . ? C1 N2 N3 110.0(4) . . ? C1 N2 C5 129.0(5) . . ? N3 N2 C5 120.9(5) . . ? C2 N3 N2 101.7(5) . . ? C4 N4 C3 101.7(5) . . ? C4 N4 Fe1 130.0(4) . . ? C3 N4 Fe1 127.8(4) . . ? C4 N5 N6 109.4(5) . . ? C4 N5 C7 127.2(5) . . ? N6 N5 C7 123.3(5) . . ? C3 N6 N5 102.6(5) . . ? C9 N7 C10 102.1(7) . . ? C9 N7 Fe2 125.6(6) . . ? C10 N7 Fe2 130.9(6) . . ? C9 N8 N9 111.5(7) . . ? C9 N8 C11 128.9(8) . . ? N9 N8 C11 119.6(8) . . ? C10 N9 N8 102.0(7) . . ? F1 B1 F3' 95.2(10) . . ? F1 B1 F2 114.0(12) . . ? F3' B1 F2 117.1(13) . . ? F1 B1 F3 132.3(12) . . ? F3' B1 F3 60.1(11) . . ? F2 B1 F3 113.7(15) . . ? F1 B1 F4 101.0(8) . . ? F3' B1 F4 116.6(14) . . ? F2 B1 F4 110.8(11) . . ? F3 B1 F4 64.2(15) . . ? F1 B1 F4' 92.2(11) . . ? F3' B1 F4' 166(2) . . ? F2 B1 F4' 70.4(12) . . ? F3 B1 F4' 106(3) . . ? F4 B1 F4' 49.7(15) . . ? F1 B1 F2' 107.8(9) . . ? F3' B1 F2' 80.4(17) . . ? F2 B1 F2' 38.9(11) . . ? F3 B1 F2' 107.0(14) . . ? F4 B1 F2' 145.1(12) . . ? F4' B1 F2' 108.9(14) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.403 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.066