data_rde121 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H10 F V' _chemical_formula_sum 'C10 H10 F V' _chemical_formula_weight 200.12 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' '-x, -y, -z' 'x-1/2, -y, z' _cell_length_a 9.7874(2) _cell_length_b 6.3569(2) _cell_length_c 14.2795(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.8677(17) _cell_angle_gamma 90.00 _cell_volume 854.58(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 1842 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408 _exptl_absorpt_coefficient_mu 1.111 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6972 _exptl_absorpt_correction_T_max 0.8970 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3246 _diffrn_reflns_av_R_equivalents 0.0147 _diffrn_reflns_av_sigmaI/netI 0.0267 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 27.45 _reflns_number_total 1935 _reflns_number_gt 1704 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _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^)+(0.0298P)^2^+0.5595P] 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 refall _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.024(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1935 _refine_ls_number_parameters 152 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0747 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.18766(19) 0.5682(3) 0.14185(12) 0.0262(4) Uani 1 1 d . . . C2 C 0.10056(18) 0.7322(3) 0.09343(12) 0.0248(4) Uani 1 1 d . . . C3 C 0.1898(2) 0.9042(3) 0.08874(12) 0.0270(4) Uani 1 1 d . . . C4 C 0.3305(2) 0.8447(3) 0.13428(13) 0.0316(4) Uani 1 1 d . . . C5 C 0.3298(2) 0.6362(3) 0.16664(12) 0.0295(4) Uani 1 1 d . . . C6 C 0.1928(2) 0.1127(3) 0.33359(13) 0.0318(4) Uani 1 1 d . . . C7 C 0.2252(2) 0.3209(3) 0.36342(13) 0.0348(5) Uani 1 1 d . . . C8 C 0.1238(2) 0.3907(3) 0.40981(13) 0.0296(4) Uani 1 1 d . . . C9 C 0.02731(18) 0.2250(3) 0.40788(12) 0.0259(4) Uani 1 1 d . . . C10 C 0.07027(18) 0.0547(3) 0.36106(12) 0.0272(4) Uani 1 1 d . . . F1 F 0.2500 0.3391(2) 0.0000 0.0298(3) Uani 1 2 d S . . F2 F 0.2500 -0.1763(2) 0.5000 0.0284(3) Uani 1 2 d S . . V1 V 0.2500 0.64004(5) 0.0000 0.01680(15) Uani 1 2 d S . . V2 V 0.2500 0.12462(5) 0.5000 0.01688(15) Uani 1 2 d S . . H1 H 0.156(2) 0.435(3) 0.1491(15) 0.033(5) Uiso 1 1 d . . . H2 H 0.002(2) 0.727(3) 0.0678(15) 0.038(6) Uiso 1 1 d . . . H3 H 0.162(2) 1.033(4) 0.0582(17) 0.043(6) Uiso 1 1 d . . . H4 H 0.408(3) 0.926(4) 0.1392(17) 0.044(6) Uiso 1 1 d . . . H5 H 0.406(2) 0.557(4) 0.1975(17) 0.042(6) Uiso 1 1 d . . . H6 H 0.242(3) 0.029(4) 0.3040(17) 0.044(6) Uiso 1 1 d . . . H7 H 0.301(3) 0.400(4) 0.3579(17) 0.046(6) Uiso 1 1 d . . . H8 H 0.122(2) 0.521(4) 0.4391(16) 0.038(6) Uiso 1 1 d . . . H9 H -0.046(2) 0.226(4) 0.4354(16) 0.045(6) Uiso 1 1 d . . . H10 H 0.031(2) -0.078(3) 0.3546(15) 0.034(5) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0328(9) 0.0254(8) 0.0245(8) 0.0038(7) 0.0145(7) -0.0002(7) C2 0.0247(8) 0.0283(8) 0.0245(8) -0.0016(7) 0.0118(7) 0.0025(7) C3 0.0421(10) 0.0212(8) 0.0220(8) -0.0030(7) 0.0159(8) 0.0004(7) C4 0.0354(10) 0.0406(10) 0.0217(8) -0.0112(7) 0.0126(8) -0.0161(8) C5 0.0262(9) 0.0453(11) 0.0165(8) 0.0039(7) 0.0052(7) 0.0051(7) C6 0.0299(9) 0.0497(12) 0.0151(8) -0.0022(7) 0.0051(7) 0.0072(8) C7 0.0310(10) 0.0471(11) 0.0235(9) 0.0153(8) 0.0028(7) -0.0109(9) C8 0.0355(10) 0.0212(8) 0.0248(9) 0.0036(7) -0.0038(7) 0.0023(7) C9 0.0213(8) 0.0305(9) 0.0245(8) 0.0041(7) 0.0039(7) 0.0044(7) C10 0.0256(8) 0.0255(9) 0.0252(8) -0.0019(7) -0.0020(7) -0.0007(7) F1 0.0381(8) 0.0167(6) 0.0377(8) 0.000 0.0157(7) 0.000 F2 0.0332(8) 0.0176(6) 0.0331(8) 0.000 0.0068(6) 0.000 V1 0.0187(2) 0.0161(2) 0.0166(2) 0.000 0.00629(15) 0.000 V2 0.0184(2) 0.0167(2) 0.0158(2) 0.000 0.00504(15) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.403(2) . ? C1 C5 1.407(3) . ? C1 V1 2.3149(16) . ? C1 H1 0.92(2) . ? C2 C3 1.413(2) . ? C2 V1 2.3086(15) . ? C2 H2 0.94(2) . ? C3 C4 1.405(3) . ? C3 V1 2.2763(17) . ? C3 H3 0.93(2) . ? C4 C5 1.405(3) . ? C4 V1 2.2725(17) . ? C4 H4 0.91(2) . ? C5 V1 2.2927(17) . ? C5 H5 0.91(2) . ? C6 C7 1.400(3) . ? C6 C10 1.409(3) . ? C6 V2 2.2887(17) . ? C6 H6 0.90(2) . ? C7 C8 1.407(3) . ? C7 V2 2.2714(17) . ? C7 H7 0.92(2) . ? C8 C9 1.410(3) . ? C8 V2 2.2751(17) . ? C8 H8 0.93(2) . ? C9 C10 1.396(2) . ? C9 V2 2.3065(16) . ? C9 H9 0.91(2) . ? C10 V2 2.3065(16) . ? C10 H10 0.92(2) . ? F1 V1 1.9128(14) . ? F2 V2 1.9131(14) . ? V1 C4 2.2725(17) 2 ? V1 C3 2.2763(17) 2 ? V1 C5 2.2926(17) 2 ? V1 C2 2.3086(15) 2 ? V1 C1 2.3150(16) 2 ? V2 C7 2.2714(17) 2_556 ? V2 C8 2.2751(17) 2_556 ? V2 C6 2.2886(17) 2_556 ? V2 C10 2.3065(16) 2_556 ? V2 C9 2.3066(16) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 108.78(16) . . ? C2 C1 V1 72.09(9) . . ? C5 C1 V1 71.36(10) . . ? C2 C1 H1 124.3(13) . . ? C5 C1 H1 126.5(13) . . ? V1 C1 H1 117.3(13) . . ? C1 C2 C3 107.35(16) . . ? C1 C2 V1 72.58(9) . . ? C3 C2 V1 70.81(9) . . ? C1 C2 H2 126.0(13) . . ? C3 C2 H2 126.6(13) . . ? V1 C2 H2 121.0(13) . . ? C4 C3 C2 108.08(16) . . ? C4 C3 V1 71.87(10) . . ? C2 C3 V1 73.31(9) . . ? C4 C3 H3 125.4(14) . . ? C2 C3 H3 126.4(14) . . ? V1 C3 H3 118.4(14) . . ? C3 C4 C5 108.30(16) . . ? C3 C4 V1 72.16(10) . . ? C5 C4 V1 72.86(10) . . ? C3 C4 H4 125.5(15) . . ? C5 C4 H4 126.2(15) . . ? V1 C4 H4 118.7(15) . . ? C4 C5 C1 107.48(17) . . ? C4 C5 V1 71.30(10) . . ? C1 C5 V1 73.09(10) . . ? C4 C5 H5 127.5(15) . . ? C1 C5 H5 125.0(15) . . ? V1 C5 H5 120.8(14) . . ? C7 C6 C10 107.57(17) . . ? C7 C6 V2 71.45(10) . . ? C10 C6 V2 72.84(10) . . ? C7 C6 H6 126.5(15) . . ? C10 C6 H6 125.9(15) . . ? V2 C6 H6 119.8(15) . . ? C6 C7 C8 108.16(17) . . ? C6 C7 V2 72.80(10) . . ? C8 C7 V2 72.12(10) . . ? C6 C7 H7 127.9(15) . . ? C8 C7 H7 123.8(15) . . ? V2 C7 H7 118.5(15) . . ? C7 C8 C9 108.03(16) . . ? C7 C8 V2 71.83(10) . . ? C9 C8 V2 73.29(10) . . ? C7 C8 H8 126.3(14) . . ? C9 C8 H8 125.6(14) . . ? V2 C8 H8 118.7(13) . . ? C10 C9 C8 107.51(16) . . ? C10 C9 V2 72.38(10) . . ? C8 C9 V2 70.86(10) . . ? C10 C9 H9 126.3(15) . . ? C8 C9 H9 126.1(15) . . ? V2 C9 H9 119.4(14) . . ? C9 C10 C6 108.73(16) . . ? C9 C10 V2 72.38(10) . . ? C6 C10 V2 71.46(10) . . ? C9 C10 H10 125.7(13) . . ? C6 C10 H10 125.4(13) . . ? V2 C10 H10 117.6(13) . . ? F1 V1 C4 124.93(5) . . ? F1 V1 C4 124.93(5) . 2 ? C4 V1 C4 110.14(10) . 2 ? F1 V1 C3 137.54(4) . . ? C4 V1 C3 35.97(7) . . ? C4 V1 C3 87.96(7) 2 . ? F1 V1 C3 137.54(4) . 2 ? C4 V1 C3 87.96(7) . 2 ? C4 V1 C3 35.97(7) 2 2 ? C3 V1 C3 84.92(9) . 2 ? F1 V1 C5 89.39(5) . 2 ? C4 V1 C5 145.38(7) . 2 ? C4 V1 C5 35.84(7) 2 2 ? C3 V1 C5 121.27(7) . 2 ? C3 V1 C5 59.78(7) 2 2 ? F1 V1 C5 89.39(5) . . ? C4 V1 C5 35.84(7) . . ? C4 V1 C5 145.38(7) 2 . ? C3 V1 C5 59.79(7) . . ? C3 V1 C5 121.27(7) 2 . ? C5 V1 C5 178.77(10) 2 . ? F1 V1 C2 104.70(4) . . ? C4 V1 C2 59.70(7) . . ? C4 V1 C2 102.36(6) 2 . ? C3 V1 C2 35.88(6) . . ? C3 V1 C2 115.84(6) 2 . ? C5 V1 C2 120.84(6) 2 . ? C5 V1 C2 59.53(6) . . ? F1 V1 C2 104.70(4) . 2 ? C4 V1 C2 102.36(6) . 2 ? C4 V1 C2 59.70(7) 2 2 ? C3 V1 C2 115.84(6) . 2 ? C3 V1 C2 35.88(6) 2 2 ? C5 V1 C2 59.52(6) 2 2 ? C5 V1 C2 120.84(6) . 2 ? C2 V1 C2 150.61(9) . 2 ? F1 V1 C1 78.63(5) . . ? C4 V1 C1 59.22(7) . . ? C4 V1 C1 137.53(6) 2 . ? C3 V1 C1 59.21(6) . . ? C3 V1 C1 143.40(6) 2 . ? C5 V1 C1 144.04(6) 2 . ? C5 V1 C1 35.54(6) . . ? C2 V1 C1 35.33(6) . . ? C2 V1 C1 156.33(6) 2 . ? F1 V1 C1 78.63(5) . 2 ? C4 V1 C1 137.53(6) . 2 ? C4 V1 C1 59.22(6) 2 2 ? C3 V1 C1 143.40(6) . 2 ? C3 V1 C1 59.21(6) 2 2 ? C5 V1 C1 35.54(6) 2 2 ? C5 V1 C1 144.04(6) . 2 ? C2 V1 C1 156.33(6) . 2 ? C2 V1 C1 35.33(6) 2 2 ? C1 V1 C1 157.26(9) . 2 ? F2 V2 C7 123.31(6) . 2_556 ? F2 V2 C7 123.31(6) . . ? C7 V2 C7 113.38(11) 2_556 . ? F2 V2 C8 138.04(5) . . ? C7 V2 C8 89.53(7) 2_556 . ? C7 V2 C8 36.05(8) . . ? F2 V2 C8 138.04(5) . 2_556 ? C7 V2 C8 36.05(8) 2_556 2_556 ? C7 V2 C8 89.53(7) . 2_556 ? C8 V2 C8 83.92(9) . 2_556 ? F2 V2 C6 88.10(5) . 2_556 ? C7 V2 C6 35.75(7) 2_556 2_556 ? C7 V2 C6 147.99(8) . 2_556 ? C8 V2 C6 123.59(7) . 2_556 ? C8 V2 C6 59.74(7) 2_556 2_556 ? F2 V2 C6 88.10(5) . . ? C7 V2 C6 147.99(8) 2_556 . ? C7 V2 C6 35.75(7) . . ? C8 V2 C6 59.74(7) . . ? C8 V2 C6 123.59(7) 2_556 . ? C6 V2 C6 176.20(11) 2_556 . ? F2 V2 C10 78.89(4) . 2_556 ? C7 V2 C10 59.33(7) 2_556 2_556 ? C7 V2 C10 136.21(7) . 2_556 ? C8 V2 C10 142.99(7) . 2_556 ? C8 V2 C10 59.21(6) 2_556 2_556 ? C6 V2 C10 35.70(7) 2_556 2_556 ? C6 V2 C10 143.06(7) . 2_556 ? F2 V2 C10 78.89(5) . . ? C7 V2 C10 136.21(7) 2_556 . ? C7 V2 C10 59.33(7) . . ? C8 V2 C10 59.21(6) . . ? C8 V2 C10 142.99(7) 2_556 . ? C6 V2 C10 143.06(7) 2_556 . ? C6 V2 C10 35.70(7) . . ? C10 V2 C10 157.77(9) 2_556 . ? F2 V2 C9 106.06(5) . . ? C7 V2 C9 101.56(7) 2_556 . ? C7 V2 C9 59.72(7) . . ? C8 V2 C9 35.85(6) . . ? C8 V2 C9 113.53(7) 2_556 . ? C6 V2 C9 121.75(7) 2_556 . ? C6 V2 C9 59.48(6) . . ? C10 V2 C9 157.43(6) 2_556 . ? C10 V2 C9 35.24(6) . . ? F2 V2 C9 106.06(5) . 2_556 ? C7 V2 C9 59.72(7) 2_556 2_556 ? C7 V2 C9 101.56(7) . 2_556 ? C8 V2 C9 113.53(7) . 2_556 ? C8 V2 C9 35.85(6) 2_556 2_556 ? C6 V2 C9 59.48(7) 2_556 2_556 ? C6 V2 C9 121.74(7) . 2_556 ? C10 V2 C9 35.24(6) 2_556 2_556 ? C10 V2 C9 157.43(6) . 2_556 ? C9 V2 C9 147.88(9) . 2_556 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -0.37(19) . . . . ? V1 C1 C2 C3 -62.69(11) . . . . ? C5 C1 C2 V1 62.31(12) . . . . ? C1 C2 C3 C4 -0.07(18) . . . . ? V1 C2 C3 C4 -63.92(12) . . . . ? C1 C2 C3 V1 63.85(11) . . . . ? C2 C3 C4 C5 0.48(19) . . . . ? V1 C3 C4 C5 -64.38(12) . . . . ? C2 C3 C4 V1 64.86(11) . . . . ? C3 C4 C5 C1 -0.7(2) . . . . ? V1 C4 C5 C1 -64.62(12) . . . . ? C3 C4 C5 V1 63.92(12) . . . . ? C2 C1 C5 C4 0.7(2) . . . . ? V1 C1 C5 C4 63.44(12) . . . . ? C2 C1 C5 V1 -62.77(12) . . . . ? C10 C6 C7 C8 0.5(2) . . . . ? V2 C6 C7 C8 -63.90(12) . . . . ? C10 C6 C7 V2 64.36(12) . . . . ? C6 C7 C8 C9 -0.5(2) . . . . ? V2 C7 C8 C9 -64.85(12) . . . . ? C6 C7 C8 V2 64.35(13) . . . . ? C7 C8 C9 C10 0.35(19) . . . . ? V2 C8 C9 C10 -63.54(12) . . . . ? C7 C8 C9 V2 63.89(12) . . . . ? C8 C9 C10 C6 -0.07(19) . . . . ? V2 C9 C10 C6 -62.62(12) . . . . ? C8 C9 C10 V2 62.55(12) . . . . ? C7 C6 C10 C9 -0.2(2) . . . . ? V2 C6 C10 C9 63.21(12) . . . . ? C7 C6 C10 V2 -63.45(12) . . . . ? C3 C4 V1 F1 -124.73(9) . . . . ? C5 C4 V1 F1 -8.34(13) . . . . ? C3 C4 V1 C4 55.27(9) . . . 2 ? C5 C4 V1 C4 171.66(13) . . . 2 ? C5 C4 V1 C3 116.39(16) . . . . ? C3 C4 V1 C3 84.16(13) . . . 2 ? C5 C4 V1 C3 -159.46(12) . . . 2 ? C3 C4 V1 C5 63.87(16) . . . 2 ? C5 C4 V1 C5 -179.74(2) . . . 2 ? C3 C4 V1 C5 -116.39(16) . . . . ? C3 C4 V1 C2 -37.58(10) . . . . ? C5 C4 V1 C2 78.81(12) . . . . ? C3 C4 V1 C2 117.25(11) . . . 2 ? C5 C4 V1 C2 -126.36(11) . . . 2 ? C3 C4 V1 C1 -78.84(11) . . . . ? C5 C4 V1 C1 37.55(11) . . . . ? C3 C4 V1 C1 121.27(12) . . . 2 ? C5 C4 V1 C1 -122.34(12) . . . 2 ? C4 C3 V1 F1 86.46(11) . . . . ? C2 C3 V1 F1 -29.59(14) . . . . ? C2 C3 V1 C4 -116.05(15) . . . . ? C4 C3 V1 C4 -129.46(11) . . . 2 ? C2 C3 V1 C4 114.49(11) . . . 2 ? C4 C3 V1 C3 -93.54(11) . . . 2 ? C2 C3 V1 C3 150.41(14) . . . 2 ? C4 C3 V1 C5 -143.37(11) . . . 2 ? C2 C3 V1 C5 100.59(11) . . . 2 ? C4 C3 V1 C5 37.37(11) . . . . ? C2 C3 V1 C5 -78.68(11) . . . . ? C4 C3 V1 C2 116.05(15) . . . . ? C4 C3 V1 C2 -74.78(12) . . . 2 ? C2 C3 V1 C2 169.17(6) . . . 2 ? C4 C3 V1 C1 78.86(11) . . . . ? C2 C3 V1 C1 -37.19(10) . . . . ? C4 C3 V1 C1 -104.53(13) . . . 2 ? C2 C3 V1 C1 139.42(11) . . . 2 ? C4 C5 V1 F1 173.17(11) . . . . ? C1 C5 V1 F1 -71.08(10) . . . . ? C1 C5 V1 C4 115.75(16) . . . . ? C4 C5 V1 C4 -13.9(2) . . . 2 ? C1 C5 V1 C4 101.88(15) . . . 2 ? C4 C5 V1 C3 -37.51(11) . . . . ? C1 C5 V1 C3 78.24(11) . . . . ? C4 C5 V1 C3 24.22(14) . . . 2 ? C1 C5 V1 C3 139.97(11) . . . 2 ? C4 C5 V1 C5 173.12(11) . . . 2 ? C1 C5 V1 C5 -71.13(10) . . . 2 ? C4 C5 V1 C2 -79.33(12) . . . . ? C1 C5 V1 C2 36.42(10) . . . . ? C4 C5 V1 C2 66.37(13) . . . 2 ? C1 C5 V1 C2 -177.89(10) . . . 2 ? C4 C5 V1 C1 -115.75(16) . . . . ? C4 C5 V1 C1 103.69(14) . . . 2 ? C1 C5 V1 C1 -140.56(16) . . . 2 ? C1 C2 V1 F1 43.74(11) . . . . ? C3 C2 V1 F1 159.84(9) . . . . ? C1 C2 V1 C4 -78.43(12) . . . . ? C3 C2 V1 C4 37.68(11) . . . . ? C1 C2 V1 C4 175.30(11) . . . 2 ? C3 C2 V1 C4 -68.59(12) . . . 2 ? C1 C2 V1 C3 -116.11(15) . . . . ? C1 C2 V1 C3 -149.23(11) . . . 2 ? C3 C2 V1 C3 -33.13(15) . . . 2 ? C1 C2 V1 C5 142.00(11) . . . 2 ? C3 C2 V1 C5 -101.90(12) . . . 2 ? C1 C2 V1 C5 -36.64(11) . . . . ? C3 C2 V1 C5 79.47(12) . . . . ? C1 C2 V1 C2 -136.27(11) . . . 2 ? C3 C2 V1 C2 -20.16(9) . . . 2 ? C3 C2 V1 C1 116.11(15) . . . . ? C1 C2 V1 C1 138.93(18) . . . 2 ? C3 C2 V1 C1 -104.96(18) . . . 2 ? C2 C1 V1 F1 -136.99(10) . . . . ? C5 C1 V1 F1 105.23(11) . . . . ? C2 C1 V1 C4 79.91(12) . . . . ? C5 C1 V1 C4 -37.87(11) . . . . ? C2 C1 V1 C4 -6.81(16) . . . 2 ? C5 C1 V1 C4 -124.58(13) . . . 2 ? C2 C1 V1 C3 37.78(10) . . . . ? C5 C1 V1 C3 -80.00(12) . . . . ? C2 C1 V1 C3 50.55(16) . . . 2 ? C5 C1 V1 C3 -67.23(15) . . . 2 ? C2 C1 V1 C5 -64.20(16) . . . 2 ? C5 C1 V1 C5 178.02(16) . . . 2 ? C2 C1 V1 C5 117.78(16) . . . . ? C5 C1 V1 C2 -117.78(16) . . . . ? C2 C1 V1 C2 122.3(2) . . . 2 ? C5 C1 V1 C2 4.5(2) . . . 2 ? C2 C1 V1 C1 -136.99(10) . . . 2 ? C5 C1 V1 C1 105.23(11) . . . 2 ? C6 C7 V2 F2 11.25(14) . . . . ? C8 C7 V2 F2 127.53(10) . . . . ? C6 C7 V2 C7 -168.75(14) . . . 2_556 ? C8 C7 V2 C7 -52.47(10) . . . 2_556 ? C6 C7 V2 C8 -116.28(16) . . . . ? C6 C7 V2 C8 163.43(12) . . . 2_556 ? C8 C7 V2 C8 -80.30(14) . . . 2_556 ? C6 C7 V2 C6 178.83(4) . . . 2_556 ? C8 C7 V2 C6 -64.89(17) . . . 2_556 ? C8 C7 V2 C6 116.28(16) . . . . ? C6 C7 V2 C10 121.87(12) . . . 2_556 ? C8 C7 V2 C10 -121.85(12) . . . 2_556 ? C6 C7 V2 C10 -37.61(11) . . . . ? C8 C7 V2 C10 78.67(12) . . . . ? C6 C7 V2 C9 -78.73(12) . . . . ? C8 C7 V2 C9 37.55(10) . . . . ? C6 C7 V2 C9 129.43(11) . . . 2_556 ? C8 C7 V2 C9 -114.29(11) . . . 2_556 ? C7 C8 V2 F2 -82.41(13) . . . . ? C9 C8 V2 F2 33.61(14) . . . . ? C7 C8 V2 C7 133.28(12) . . . 2_556 ? C9 C8 V2 C7 -110.71(12) . . . 2_556 ? C9 C8 V2 C7 116.01(16) . . . . ? C7 C8 V2 C8 97.59(13) . . . 2_556 ? C9 C8 V2 C8 -146.39(14) . . . 2_556 ? C7 C8 V2 C6 144.82(11) . . . 2_556 ? C9 C8 V2 C6 -99.16(12) . . . 2_556 ? C7 C8 V2 C6 -37.34(11) . . . . ? C9 C8 V2 C6 78.68(12) . . . . ? C7 C8 V2 C10 102.42(14) . . . 2_556 ? C9 C8 V2 C10 -141.56(11) . . . 2_556 ? C7 C8 V2 C10 -79.02(12) . . . . ? C9 C8 V2 C10 36.99(10) . . . . ? C7 C8 V2 C9 -116.01(16) . . . . ? C7 C8 V2 C9 76.89(12) . . . 2_556 ? C9 C8 V2 C9 -167.10(7) . . . 2_556 ? C7 C6 V2 F2 -170.61(11) . . . . ? C10 C6 V2 F2 73.48(10) . . . . ? C7 C6 V2 C7 19.7(2) . . . 2_556 ? C10 C6 V2 C7 -96.16(16) . . . 2_556 ? C10 C6 V2 C7 -115.91(16) . . . . ? C7 C6 V2 C8 37.66(12) . . . . ? C10 C6 V2 C8 -78.25(12) . . . . ? C7 C6 V2 C8 -20.03(15) . . . 2_556 ? C10 C6 V2 C8 -135.93(11) . . . 2_556 ? C7 C6 V2 C6 -170.61(12) . . . 2_556 ? C10 C6 V2 C6 73.48(10) . . . 2_556 ? C7 C6 V2 C10 -102.02(15) . . . 2_556 ? C10 C6 V2 C10 142.07(16) . . . 2_556 ? C7 C6 V2 C10 115.91(16) . . . . ? C7 C6 V2 C9 79.46(13) . . . . ? C10 C6 V2 C9 -36.45(10) . . . . ? C7 C6 V2 C9 -62.86(14) . . . 2_556 ? C10 C6 V2 C9 -178.77(10) . . . 2_556 ? C9 C10 V2 F2 140.06(11) . . . . ? C6 C10 V2 F2 -102.44(11) . . . . ? C9 C10 V2 C7 12.91(16) . . . 2_556 ? C6 C10 V2 C7 130.41(14) . . . 2_556 ? C9 C10 V2 C7 -79.84(12) . . . . ? C6 C10 V2 C7 37.66(12) . . . . ? C9 C10 V2 C8 -37.64(11) . . . . ? C6 C10 V2 C8 79.86(12) . . . . ? C9 C10 V2 C8 -43.23(17) . . . 2_556 ? C6 C10 V2 C8 74.27(16) . . . 2_556 ? C9 C10 V2 C6 68.57(16) . . . 2_556 ? C6 C10 V2 C6 -173.93(17) . . . 2_556 ? C9 C10 V2 C6 -117.50(16) . . . . ? C9 C10 V2 C10 140.06(11) . . . 2_556 ? C6 C10 V2 C10 -102.44(11) . . . 2_556 ? C6 C10 V2 C9 117.50(16) . . . . ? C9 C10 V2 C9 -114.8(2) . . . 2_556 ? C6 C10 V2 C9 2.7(2) . . . 2_556 ? C10 C9 V2 F2 -40.96(11) . . . . ? C8 C9 V2 F2 -157.35(10) . . . . ? C10 C9 V2 C7 -170.92(11) . . . 2_556 ? C8 C9 V2 C7 72.69(13) . . . 2_556 ? C10 C9 V2 C7 78.62(12) . . . . ? C8 C9 V2 C7 -37.77(11) . . . . ? C10 C9 V2 C8 116.39(16) . . . . ? C10 C9 V2 C8 153.28(11) . . . 2_556 ? C8 C9 V2 C8 36.89(16) . . . 2_556 ? C10 C9 V2 C6 -138.87(11) . . . 2_556 ? C8 C9 V2 C6 104.75(12) . . . 2_556 ? C10 C9 V2 C6 36.93(11) . . . . ? C8 C9 V2 C6 -79.46(12) . . . . ? C10 C9 V2 C10 -140.75(19) . . . 2_556 ? C8 C9 V2 C10 102.87(19) . . . 2_556 ? C8 C9 V2 C10 -116.39(16) . . . . ? C10 C9 V2 C9 139.03(11) . . . 2_556 ? C8 C9 V2 C9 22.65(10) . . . 2_556 ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.279 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.053 data_rde129 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H25 Cr F2 N2' _chemical_formula_sum 'C17 H25 Cr F2 N2' _chemical_formula_weight 347.39 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4526(2) _cell_length_b 8.5308(4) _cell_length_c 14.9544(8) _cell_angle_alpha 79.848(3) _cell_angle_beta 82.488(3) _cell_angle_gamma 65.649(3) _cell_volume 850.82(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 18180 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 366 _exptl_absorpt_coefficient_mu 0.690 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8304 _exptl_absorpt_correction_T_max 0.9796 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5588 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.77 _diffrn_reflns_theta_max 27.39 _reflns_number_total 3769 _reflns_number_gt 2949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _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^)+(0.0204P)^2^+1.4108P] 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 3769 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0763 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1138 _refine_ls_wR_factor_gt 0.1008 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 Cr1 Cr 0.81534(7) 0.11128(6) 0.24843(3) 0.01889(14) Uani 1 1 d . . . F1 F 0.5433(2) 0.1737(3) 0.25826(13) 0.0372(5) Uani 1 1 d . . . F2 F 0.8799(3) -0.0816(2) 0.33908(12) 0.0316(4) Uani 1 1 d . . . N1 N 0.7970(3) 0.2736(3) 0.33961(17) 0.0207(5) Uani 1 1 d . . . N2 N 0.7237(4) 0.5944(3) 0.53575(17) 0.0238(6) Uani 1 1 d . . . C1 C 1.0276(4) 0.1980(4) 0.1524(2) 0.0191(6) Uani 1 1 d . . . C2 C 0.8484(4) 0.2486(4) 0.1098(2) 0.0226(6) Uani 1 1 d . . . C3 C 0.8261(4) 0.0950(4) 0.0995(2) 0.0234(6) Uani 1 1 d . . . C4 C 0.9856(4) -0.0486(4) 0.1387(2) 0.0240(6) Uani 1 1 d . . . C5 C 1.1104(4) 0.0148(4) 0.1723(2) 0.0209(6) Uani 1 1 d . . . C6 C 1.1132(5) 0.3193(4) 0.1709(3) 0.0285(7) Uani 1 1 d . . . C7 C 0.7106(5) 0.4324(5) 0.0769(3) 0.0342(8) Uani 1 1 d . . . C8 C 0.6566(5) 0.0900(5) 0.0570(2) 0.0371(8) Uani 1 1 d . . . H8A H 0.6879 -0.0291 0.0467 0.056 Uiso 1 1 calc R . . H8B H 0.6342 0.1665 -0.0013 0.056 Uiso 1 1 calc R . . H8C H 0.5373 0.1294 0.0978 0.056 Uiso 1 1 calc R . . C9 C 1.0171(6) -0.2359(4) 0.1475(3) 0.0385(9) Uani 1 1 d . . . H9A H 0.9472 -0.2660 0.2035 0.058 Uiso 1 1 calc R . . H9B H 1.1585 -0.3091 0.1496 0.058 Uiso 1 1 calc R . . H9C H 0.9662 -0.2550 0.0950 0.058 Uiso 1 1 calc R . . C10 C 1.2973(5) -0.0962(5) 0.2201(3) 0.0336(8) Uani 1 1 d . . . C11 C 0.6929(4) 0.4475(4) 0.3257(2) 0.0233(6) Uani 1 1 d . . . C12 C 0.6680(4) 0.5573(4) 0.3868(2) 0.0236(6) Uani 1 1 d . . . C13 C 0.7496(4) 0.4907(4) 0.4726(2) 0.0198(6) Uani 1 1 d . . . C14 C 0.8602(4) 0.3096(4) 0.4870(2) 0.0222(6) Uani 1 1 d . . . C15 C 0.8808(4) 0.2106(4) 0.4206(2) 0.0237(6) Uani 1 1 d . . . C16 C 0.6137(5) 0.7828(4) 0.5170(3) 0.0285(7) Uani 1 1 d . . . C17 C 0.7927(5) 0.5232(4) 0.6267(2) 0.0276(7) Uani 1 1 d . . . H17A H 0.7599 0.4226 0.6495 0.041 Uiso 1 1 calc R . . H17B H 0.7286 0.6119 0.6675 0.041 Uiso 1 1 calc R . . H17C H 0.9361 0.4870 0.6245 0.041 Uiso 1 1 calc R . . H6A H 1.157(5) 0.376(5) 0.112(3) 0.048(11) Uiso 1 1 d . . . H6B H 1.225(5) 0.260(4) 0.209(2) 0.028(9) Uiso 1 1 d . . . H6C H 1.015(6) 0.416(5) 0.207(3) 0.050(11) Uiso 1 1 d . . . H7A H 0.718(6) 0.453(6) 0.011(3) 0.067(14) Uiso 1 1 d . . . H7B H 0.744(6) 0.513(5) 0.097(3) 0.047(12) Uiso 1 1 d . . . H7C H 0.574(7) 0.458(5) 0.099(3) 0.060(13) Uiso 1 1 d . . . H10A H 1.276(5) -0.173(5) 0.273(3) 0.043(11) Uiso 1 1 d . . . H10B H 1.393(6) -0.176(6) 0.181(3) 0.063(13) Uiso 1 1 d . . . H10C H 1.356(6) -0.028(5) 0.242(3) 0.053(12) Uiso 1 1 d . . . H11 H 0.633(5) 0.492(4) 0.268(2) 0.026(9) Uiso 1 1 d . . . H12 H 0.597(4) 0.676(4) 0.370(2) 0.023(8) Uiso 1 1 d . . . H14 H 0.920(5) 0.258(4) 0.539(2) 0.029(9) Uiso 1 1 d . . . H15 H 0.960(5) 0.085(4) 0.430(2) 0.027(9) Uiso 1 1 d . . . H16A H 0.678(5) 0.832(4) 0.466(3) 0.033(9) Uiso 1 1 d . . . H16B H 0.608(5) 0.834(5) 0.568(3) 0.048(11) Uiso 1 1 d . . . H16C H 0.477(6) 0.811(5) 0.502(3) 0.040(10) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cr1 0.0204(2) 0.0214(2) 0.0163(3) -0.00374(18) 0.00009(17) -0.00969(18) F1 0.0222(9) 0.0608(13) 0.0339(11) -0.0208(10) 0.0030(8) -0.0177(9) F2 0.0488(11) 0.0244(9) 0.0208(10) 0.0007(8) 0.0013(8) -0.0163(9) N1 0.0240(12) 0.0219(12) 0.0170(13) -0.0024(10) -0.0019(10) -0.0098(10) N2 0.0289(13) 0.0229(13) 0.0212(14) -0.0059(11) -0.0014(10) -0.0109(11) C1 0.0218(13) 0.0215(14) 0.0161(14) -0.0017(12) 0.0014(11) -0.0116(12) C2 0.0245(14) 0.0254(15) 0.0160(15) 0.0006(12) -0.0003(11) -0.0099(12) C3 0.0259(14) 0.0332(17) 0.0152(15) -0.0069(13) 0.0024(11) -0.0154(13) C4 0.0302(15) 0.0233(15) 0.0223(16) -0.0093(13) 0.0067(12) -0.0146(13) C5 0.0213(13) 0.0206(14) 0.0197(15) -0.0038(12) 0.0014(11) -0.0076(12) C6 0.0312(17) 0.0272(17) 0.034(2) -0.0044(15) -0.0016(15) -0.0182(15) C7 0.0354(19) 0.0317(19) 0.0252(19) 0.0038(15) -0.0081(15) -0.0045(16) C8 0.0389(18) 0.059(2) 0.0247(18) -0.0113(17) -0.0026(14) -0.0286(18) C9 0.055(2) 0.0284(18) 0.039(2) -0.0144(16) 0.0120(17) -0.0244(17) C10 0.0268(16) 0.0277(18) 0.038(2) 0.0026(16) -0.0044(15) -0.0045(15) C11 0.0243(14) 0.0256(15) 0.0181(16) -0.0026(13) -0.0034(12) -0.0075(12) C12 0.0217(14) 0.0223(15) 0.0246(17) -0.0037(13) -0.0023(12) -0.0061(12) C13 0.0195(13) 0.0234(15) 0.0193(15) -0.0026(12) 0.0008(11) -0.0122(12) C14 0.0271(15) 0.0221(15) 0.0185(16) 0.0004(12) -0.0029(12) -0.0117(12) C15 0.0265(15) 0.0214(15) 0.0229(17) -0.0016(13) -0.0051(12) -0.0088(13) C16 0.0311(17) 0.0249(16) 0.0284(19) -0.0094(15) 0.0026(14) -0.0089(14) C17 0.0356(17) 0.0303(17) 0.0196(16) -0.0049(13) -0.0004(13) -0.0157(14) _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 Cr1 F1 1.8638(17) . ? Cr1 F2 1.8730(18) . ? Cr1 N1 2.063(2) . ? Cr1 C4 2.232(3) . ? Cr1 C2 2.232(3) . ? Cr1 C5 2.235(3) . ? Cr1 C3 2.245(3) . ? Cr1 C1 2.261(3) . ? N1 C11 1.353(4) . ? N1 C15 1.356(4) . ? N2 C13 1.349(4) . ? N2 C17 1.456(4) . ? N2 C16 1.465(4) . ? C1 C5 1.415(4) . ? C1 C2 1.424(4) . ? C1 C6 1.498(4) . ? C2 C3 1.424(4) . ? C2 C7 1.512(4) . ? C3 C4 1.409(4) . ? C3 C8 1.505(4) . ? C4 C5 1.429(4) . ? C4 C9 1.500(4) . ? C5 C10 1.511(4) . ? C6 H6A 1.01(4) . ? C6 H6B 0.98(3) . ? C6 H6C 1.03(4) . ? C7 H7A 0.97(5) . ? C7 H7B 0.93(4) . ? C7 H7C 0.97(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.98(4) . ? C10 H10B 0.97(5) . ? C10 H10C 0.98(4) . ? C11 C12 1.364(4) . ? C11 H11 0.96(3) . ? C12 C13 1.414(4) . ? C12 H12 0.94(3) . ? C13 C14 1.411(4) . ? C14 C15 1.367(4) . ? C14 H14 0.90(4) . ? C15 H15 0.98(3) . ? C16 H16A 0.97(4) . ? C16 H16B 0.93(4) . ? C16 H16C 0.99(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? 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 F1 Cr1 F2 97.18(9) . . ? F1 Cr1 N1 92.57(9) . . ? F2 Cr1 N1 91.96(9) . . ? F1 Cr1 C4 116.44(10) . . ? F2 Cr1 C4 93.15(10) . . ? N1 Cr1 C4 149.59(10) . . ? F1 Cr1 C2 99.89(10) . . ? F2 Cr1 C2 154.11(10) . . ? N1 Cr1 C2 106.49(11) . . ? C4 Cr1 C2 61.80(11) . . ? F1 Cr1 C5 151.99(10) . . ? F2 Cr1 C5 94.60(10) . . ? N1 Cr1 C5 112.37(10) . . ? C4 Cr1 C5 37.32(11) . . ? C2 Cr1 C5 61.89(11) . . ? F1 Cr1 C3 90.70(9) . . ? F2 Cr1 C3 123.92(10) . . ? N1 Cr1 C3 143.23(11) . . ? C4 Cr1 C3 36.69(11) . . ? C2 Cr1 C3 37.09(11) . . ? C5 Cr1 C3 61.77(11) . . ? F1 Cr1 C1 135.39(10) . . ? F2 Cr1 C1 126.99(9) . . ? N1 Cr1 C1 91.89(10) . . ? C4 Cr1 C1 61.50(10) . . ? C2 Cr1 C1 36.95(10) . . ? C5 Cr1 C1 36.67(10) . . ? C3 Cr1 C1 61.45(10) . . ? C11 N1 C15 115.3(3) . . ? C11 N1 Cr1 123.0(2) . . ? C15 N1 Cr1 121.6(2) . . ? C13 N2 C17 121.4(2) . . ? C13 N2 C16 121.0(3) . . ? C17 N2 C16 117.5(3) . . ? C5 C1 C2 108.0(3) . . ? C5 C1 C6 126.6(3) . . ? C2 C1 C6 125.4(3) . . ? C5 C1 Cr1 70.66(16) . . ? C2 C1 Cr1 70.43(16) . . ? C6 C1 Cr1 125.3(2) . . ? C3 C2 C1 107.9(3) . . ? C3 C2 C7 125.8(3) . . ? C1 C2 C7 126.3(3) . . ? C3 C2 Cr1 71.94(17) . . ? C1 C2 Cr1 72.62(16) . . ? C7 C2 Cr1 123.3(2) . . ? C4 C3 C2 108.0(3) . . ? C4 C3 C8 126.7(3) . . ? C2 C3 C8 125.2(3) . . ? C4 C3 Cr1 71.15(17) . . ? C2 C3 Cr1 70.98(16) . . ? C8 C3 Cr1 121.9(2) . . ? C3 C4 C5 108.2(3) . . ? C3 C4 C9 126.4(3) . . ? C5 C4 C9 125.3(3) . . ? C3 C4 Cr1 72.15(16) . . ? C5 C4 Cr1 71.46(16) . . ? C9 C4 Cr1 120.4(2) . . ? C1 C5 C4 107.8(3) . . ? C1 C5 C10 126.8(3) . . ? C4 C5 C10 125.5(3) . . ? C1 C5 Cr1 72.66(16) . . ? C4 C5 Cr1 71.22(16) . . ? C10 C5 Cr1 121.8(2) . . ? C1 C6 H6A 111(2) . . ? C1 C6 H6B 112(2) . . ? H6A C6 H6B 109(3) . . ? C1 C6 H6C 113(2) . . ? H6A C6 H6C 108(3) . . ? H6B C6 H6C 104(3) . . ? C2 C7 H7A 110(3) . . ? C2 C7 H7B 111(2) . . ? H7A C7 H7B 108(4) . . ? C2 C7 H7C 113(3) . . ? H7A C7 H7C 109(4) . . ? H7B C7 H7C 106(3) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 112(2) . . ? C5 C10 H10B 111(3) . . ? H10A C10 H10B 103(3) . . ? C5 C10 H10C 113(2) . . ? H10A C10 H10C 106(3) . . ? H10B C10 H10C 110(3) . . ? N1 C11 C12 124.6(3) . . ? N1 C11 H11 115.2(19) . . ? C12 C11 H11 120.2(19) . . ? C11 C12 C13 120.1(3) . . ? C11 C12 H12 118(2) . . ? C13 C12 H12 122(2) . . ? N2 C13 C14 122.6(3) . . ? N2 C13 C12 121.8(3) . . ? C14 C13 C12 115.5(3) . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 119(2) . . ? C13 C14 H14 121(2) . . ? N1 C15 C14 124.4(3) . . ? N1 C15 H15 115.6(19) . . ? C14 C15 H15 120.0(19) . . ? N2 C16 H16A 111(2) . . ? N2 C16 H16B 110(2) . . ? H16A C16 H16B 108(3) . . ? N2 C16 H16C 111(2) . . ? H16A C16 H16C 109(3) . . ? H16B C16 H16C 108(3) . . ? N2 C17 H17A 109.5 . . ? N2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F1 Cr1 N1 C11 -60.4(2) . . . . ? F2 Cr1 N1 C11 -157.7(2) . . . . ? C4 Cr1 N1 C11 102.7(3) . . . . ? C2 Cr1 N1 C11 40.7(2) . . . . ? C5 Cr1 N1 C11 106.5(2) . . . . ? C3 Cr1 N1 C11 34.2(3) . . . . ? C1 Cr1 N1 C11 75.2(2) . . . . ? F1 Cr1 N1 C15 115.9(2) . . . . ? F2 Cr1 N1 C15 18.6(2) . . . . ? C4 Cr1 N1 C15 -81.0(3) . . . . ? C2 Cr1 N1 C15 -143.0(2) . . . . ? C5 Cr1 N1 C15 -77.2(2) . . . . ? C3 Cr1 N1 C15 -149.5(2) . . . . ? C1 Cr1 N1 C15 -108.5(2) . . . . ? F1 Cr1 C1 C5 -138.03(17) . . . . ? F2 Cr1 C1 C5 32.5(2) . . . . ? N1 Cr1 C1 C5 126.39(17) . . . . ? C4 Cr1 C1 C5 -38.18(17) . . . . ? C2 Cr1 C1 C5 -118.2(3) . . . . ? C3 Cr1 C1 C5 -80.17(19) . . . . ? F1 Cr1 C1 C2 -19.8(2) . . . . ? F2 Cr1 C1 C2 150.73(16) . . . . ? N1 Cr1 C1 C2 -115.39(17) . . . . ? C4 Cr1 C1 C2 80.04(19) . . . . ? C5 Cr1 C1 C2 118.2(3) . . . . ? C3 Cr1 C1 C2 38.06(17) . . . . ? F1 Cr1 C1 C6 100.2(3) . . . . ? F2 Cr1 C1 C6 -89.2(3) . . . . ? N1 Cr1 C1 C6 4.7(3) . . . . ? C4 Cr1 C1 C6 -159.9(3) . . . . ? C2 Cr1 C1 C6 120.1(3) . . . . ? C5 Cr1 C1 C6 -121.7(3) . . . . ? C3 Cr1 C1 C6 158.1(3) . . . . ? C5 C1 C2 C3 -2.8(3) . . . . ? C6 C1 C2 C3 176.2(3) . . . . ? Cr1 C1 C2 C3 -63.8(2) . . . . ? C5 C1 C2 C7 179.9(3) . . . . ? C6 C1 C2 C7 -1.1(5) . . . . ? Cr1 C1 C2 C7 119.0(3) . . . . ? C5 C1 C2 Cr1 61.0(2) . . . . ? C6 C1 C2 Cr1 -120.0(3) . . . . ? F1 Cr1 C2 C3 -77.87(17) . . . . ? F2 Cr1 C2 C3 52.7(3) . . . . ? N1 Cr1 C2 C3 -173.55(16) . . . . ? C4 Cr1 C2 C3 36.93(16) . . . . ? C5 Cr1 C2 C3 79.48(18) . . . . ? C1 Cr1 C2 C3 116.1(2) . . . . ? F1 Cr1 C2 C1 166.02(16) . . . . ? F2 Cr1 C2 C1 -63.4(3) . . . . ? N1 Cr1 C2 C1 70.34(18) . . . . ? C4 Cr1 C2 C1 -79.18(18) . . . . ? C5 Cr1 C2 C1 -36.63(16) . . . . ? C3 Cr1 C2 C1 -116.1(2) . . . . ? F1 Cr1 C2 C7 43.6(3) . . . . ? F2 Cr1 C2 C7 174.2(2) . . . . ? N1 Cr1 C2 C7 -52.1(3) . . . . ? C4 Cr1 C2 C7 158.4(3) . . . . ? C5 Cr1 C2 C7 -159.0(3) . . . . ? C3 Cr1 C2 C7 121.5(3) . . . . ? C1 Cr1 C2 C7 -122.4(4) . . . . ? C1 C2 C3 C4 2.3(3) . . . . ? C7 C2 C3 C4 179.6(3) . . . . ? Cr1 C2 C3 C4 -61.9(2) . . . . ? C1 C2 C3 C8 -179.6(3) . . . . ? C7 C2 C3 C8 -2.3(5) . . . . ? Cr1 C2 C3 C8 116.2(3) . . . . ? C1 C2 C3 Cr1 64.2(2) . . . . ? C7 C2 C3 Cr1 -118.5(3) . . . . ? F1 Cr1 C3 C4 -136.79(18) . . . . ? F2 Cr1 C3 C4 -37.7(2) . . . . ? N1 Cr1 C3 C4 127.98(19) . . . . ? C2 Cr1 C3 C4 117.6(2) . . . . ? C5 Cr1 C3 C4 37.79(17) . . . . ? C1 Cr1 C3 C4 79.70(18) . . . . ? F1 Cr1 C3 C2 105.59(17) . . . . ? F2 Cr1 C3 C2 -155.27(15) . . . . ? N1 Cr1 C3 C2 10.4(3) . . . . ? C4 Cr1 C3 C2 -117.6(2) . . . . ? C5 Cr1 C3 C2 -79.82(18) . . . . ? C1 Cr1 C3 C2 -37.92(16) . . . . ? F1 Cr1 C3 C8 -14.6(3) . . . . ? F2 Cr1 C3 C8 84.5(3) . . . . ? N1 Cr1 C3 C8 -109.9(3) . . . . ? C4 Cr1 C3 C8 122.2(3) . . . . ? C2 Cr1 C3 C8 -120.2(3) . . . . ? C5 Cr1 C3 C8 159.9(3) . . . . ? C1 Cr1 C3 C8 -158.1(3) . . . . ? C2 C3 C4 C5 -1.0(3) . . . . ? C8 C3 C4 C5 -179.0(3) . . . . ? Cr1 C3 C4 C5 -62.8(2) . . . . ? C2 C3 C4 C9 176.8(3) . . . . ? C8 C3 C4 C9 -1.1(5) . . . . ? Cr1 C3 C4 C9 115.1(3) . . . . ? C2 C3 C4 Cr1 61.8(2) . . . . ? C8 C3 C4 Cr1 -116.2(3) . . . . ? F1 Cr1 C4 C3 49.9(2) . . . . ? F2 Cr1 C4 C3 149.49(17) . . . . ? N1 Cr1 C4 C3 -111.2(2) . . . . ? C2 Cr1 C4 C3 -37.32(17) . . . . ? C5 Cr1 C4 C3 -117.0(3) . . . . ? C1 Cr1 C4 C3 -79.53(18) . . . . ? F1 Cr1 C4 C5 166.92(16) . . . . ? F2 Cr1 C4 C5 -93.46(18) . . . . ? N1 Cr1 C4 C5 5.8(3) . . . . ? C2 Cr1 C4 C5 79.73(18) . . . . ? C3 Cr1 C4 C5 117.0(3) . . . . ? C1 Cr1 C4 C5 37.52(17) . . . . ? F1 Cr1 C4 C9 -72.4(3) . . . . ? F2 Cr1 C4 C9 27.2(3) . . . . ? N1 Cr1 C4 C9 126.5(3) . . . . ? C2 Cr1 C4 C9 -159.6(3) . . . . ? C5 Cr1 C4 C9 120.6(3) . . . . ? C3 Cr1 C4 C9 -122.3(3) . . . . ? C1 Cr1 C4 C9 158.2(3) . . . . ? C2 C1 C5 C4 2.2(3) . . . . ? C6 C1 C5 C4 -176.8(3) . . . . ? Cr1 C1 C5 C4 63.0(2) . . . . ? C2 C1 C5 C10 -178.0(3) . . . . ? C6 C1 C5 C10 3.0(5) . . . . ? Cr1 C1 C5 C10 -117.2(3) . . . . ? C2 C1 C5 Cr1 -60.8(2) . . . . ? C6 C1 C5 Cr1 120.2(3) . . . . ? C3 C4 C5 C1 -0.7(3) . . . . ? C9 C4 C5 C1 -178.6(3) . . . . ? Cr1 C4 C5 C1 -63.9(2) . . . . ? C3 C4 C5 C10 179.4(3) . . . . ? C9 C4 C5 C10 1.6(5) . . . . ? Cr1 C4 C5 C10 116.2(3) . . . . ? C3 C4 C5 Cr1 63.2(2) . . . . ? C9 C4 C5 Cr1 -114.7(3) . . . . ? F1 Cr1 C5 C1 90.8(3) . . . . ? F2 Cr1 C5 C1 -154.49(17) . . . . ? N1 Cr1 C5 C1 -60.46(19) . . . . ? C4 Cr1 C5 C1 116.4(3) . . . . ? C2 Cr1 C5 C1 36.90(17) . . . . ? C3 Cr1 C5 C1 79.19(18) . . . . ? F1 Cr1 C5 C4 -25.6(3) . . . . ? F2 Cr1 C5 C4 89.16(18) . . . . ? N1 Cr1 C5 C4 -176.81(17) . . . . ? C2 Cr1 C5 C4 -79.45(19) . . . . ? C3 Cr1 C5 C4 -37.16(18) . . . . ? C1 Cr1 C5 C4 -116.4(3) . . . . ? F1 Cr1 C5 C10 -146.2(3) . . . . ? F2 Cr1 C5 C10 -31.5(3) . . . . ? N1 Cr1 C5 C10 62.5(3) . . . . ? C4 Cr1 C5 C10 -120.7(3) . . . . ? C2 Cr1 C5 C10 159.9(3) . . . . ? C3 Cr1 C5 C10 -157.8(3) . . . . ? C1 Cr1 C5 C10 123.0(3) . . . . ? C15 N1 C11 C12 -0.6(4) . . . . ? Cr1 N1 C11 C12 175.9(2) . . . . ? N1 C11 C12 C13 -1.7(5) . . . . ? C17 N2 C13 C14 -6.1(4) . . . . ? C16 N2 C13 C14 177.8(3) . . . . ? C17 N2 C13 C12 174.3(3) . . . . ? C16 N2 C13 C12 -1.8(4) . . . . ? C11 C12 C13 N2 -178.2(3) . . . . ? C11 C12 C13 C14 2.2(4) . . . . ? N2 C13 C14 C15 179.7(3) . . . . ? C12 C13 C14 C15 -0.7(4) . . . . ? C11 N1 C15 C14 2.2(4) . . . . ? Cr1 N1 C15 C14 -174.3(2) . . . . ? C13 C14 C15 N1 -1.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.431 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.082 data_rde132 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H90 Cr8 F18,4(C7 H8)' _chemical_formula_sum 'C88 H122 Cr8 F18' _chemical_formula_weight 1937.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7587(7) _cell_length_b 14.4911(12) _cell_length_c 14.8362(13) _cell_angle_alpha 97.213(4) _cell_angle_beta 111.974(5) _cell_angle_gamma 102.408(5) _cell_volume 2229.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 199149 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1004 _exptl_absorpt_coefficient_mu 1.016 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7175 _exptl_absorpt_correction_T_max 0.7999 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17089 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.66 _reflns_number_total 9615 _reflns_number_gt 6761 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _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^)+(0.0578P)^2^+3.8344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0042(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9615 _refine_ls_number_parameters 605 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0931 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1538 _refine_ls_wR_factor_gt 0.1308 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _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 Cr1 Cr 0.99765(6) 0.84960(5) 0.28659(5) 0.03125(17) Uani 1 1 d . . . Cr2 Cr 1.18860(5) 0.88967(5) 0.13247(5) 0.03071(17) Uani 1 1 d . . . Cr3 Cr 0.69975(6) 0.75604(5) 0.03446(5) 0.03198(17) Uani 1 1 d . . . Cr4 Cr 1.09452(5) 1.09622(4) 0.06128(5) 0.02954(17) Uani 1 1 d . . . F1 F 1.0231(2) 0.72777(17) 0.2919(2) 0.0432(6) Uani 1 1 d . . . F2 F 1.1312(2) 0.88598(17) 0.23853(17) 0.0351(5) Uani 1 1 d . . . F3 F 0.8612(2) 0.80931(16) 0.15244(18) 0.0370(5) Uani 1 1 d . . . F4 F 1.0133(2) 0.84429(16) 0.02967(17) 0.0341(5) Uani 1 1 d . . . F5 F 1.1981(2) 1.02699(16) 0.14393(17) 0.0350(5) Uani 1 1 d . . . F6 F 0.7589(2) 0.82948(16) -0.05032(18) 0.0366(5) Uani 1 1 d . . . F7 F 0.6255(2) 0.84868(17) 0.0668(2) 0.0423(6) Uani 1 1 d . . . F8 F 1.1129(2) 1.18348(17) 0.16898(18) 0.0402(6) Uani 1 1 d . . . F9 F 0.94203(19) 1.00692(16) 0.05407(17) 0.0330(5) Uani 1 1 d . . . C1 C 1.0911(4) 0.9202(3) 0.4453(3) 0.0375(9) Uani 1 1 d . . . C2 C 1.0786(4) 0.9943(3) 0.3906(3) 0.0379(9) Uani 1 1 d . . . C3 C 0.9465(4) 0.9806(3) 0.3338(3) 0.0349(9) Uani 1 1 d . . . C4 C 0.8766(4) 0.8993(3) 0.3555(3) 0.0359(9) Uani 1 1 d . . . C5 C 0.9657(4) 0.8624(3) 0.4243(3) 0.0345(9) Uani 1 1 d . . . C6 C 1.2130(4) 0.9027(4) 0.5118(4) 0.0504(12) Uani 1 1 d . . . H6A H 1.2282 0.9238 0.5818 0.076 Uiso 1 1 calc R . . H6B H 1.2844 0.9394 0.5001 0.076 Uiso 1 1 calc R . . H6C H 1.2059 0.8333 0.4971 0.076 Uiso 1 1 calc R . . C7 C 1.1874(5) 1.0700(3) 0.3904(4) 0.0508(12) Uani 1 1 d . . . H7A H 1.1583 1.0938 0.3291 0.076 Uiso 1 1 calc R . . H7B H 1.2570 1.0416 0.3935 0.076 Uiso 1 1 calc R . . H7C H 1.2182 1.1240 0.4484 0.076 Uiso 1 1 calc R . . C8 C 0.8876(5) 1.0379(3) 0.2597(4) 0.0470(11) Uani 1 1 d . . . H8A H 0.8598 1.0866 0.2916 0.071 Uiso 1 1 calc R . . H8B H 0.8138 0.9939 0.2021 0.071 Uiso 1 1 calc R . . H8C H 0.9511 1.0703 0.2375 0.071 Uiso 1 1 calc R . . C9 C 0.7330(4) 0.8606(4) 0.3110(4) 0.0468(11) Uani 1 1 d . . . H9A H 0.7088 0.7932 0.3167 0.070 Uiso 1 1 calc R . . H9B H 0.6982 0.8632 0.2404 0.070 Uiso 1 1 calc R . . H9C H 0.6985 0.9001 0.3468 0.070 Uiso 1 1 calc R . . C10 C 0.9352(5) 0.7761(3) 0.4664(4) 0.0474(11) Uani 1 1 d . . . H10A H 0.9874 0.7334 0.4601 0.071 Uiso 1 1 calc R . . H10B H 0.8444 0.7406 0.4297 0.071 Uiso 1 1 calc R . . H10C H 0.9541 0.7981 0.5371 0.071 Uiso 1 1 calc R . . C11 C 1.3655(4) 0.8545(3) 0.2184(3) 0.0391(10) Uani 1 1 d . . . C12 C 1.2707(4) 0.7680(3) 0.1535(3) 0.0365(9) Uani 1 1 d . . . C13 C 1.2405(4) 0.7774(3) 0.0542(3) 0.0383(10) Uani 1 1 d . . . C14 C 1.3142(4) 0.8700(3) 0.0564(3) 0.0385(10) Uani 1 1 d . . . C15 C 1.3938(4) 0.9173(3) 0.1583(3) 0.0374(10) Uani 1 1 d . . . C16 C 1.4216(4) 0.8740(4) 0.3300(4) 0.0502(12) Uani 1 1 d . . . H16A H 1.3528 0.8579 0.3525 0.075 Uiso 1 1 calc R . . H16B H 1.4692 0.9428 0.3579 0.075 Uiso 1 1 calc R . . H16C H 1.4797 0.8341 0.3528 0.075 Uiso 1 1 calc R . . C17 C 1.2175(4) 0.6823(3) 0.1880(4) 0.0485(12) Uani 1 1 d . . . H17A H 1.2864 0.6550 0.2234 0.073 Uiso 1 1 calc R . . H17B H 1.1515 0.6329 0.1302 0.073 Uiso 1 1 calc R . . H17C H 1.1799 0.7031 0.2331 0.073 Uiso 1 1 calc R . . C18 C 1.1420(4) 0.7055(4) -0.0390(4) 0.0492(12) Uani 1 1 d . . . H18A H 1.0768 0.7355 -0.0753 0.074 Uiso 1 1 calc R . . H18B H 1.1016 0.6485 -0.0210 0.074 Uiso 1 1 calc R . . H18C H 1.1834 0.6856 -0.0815 0.074 Uiso 1 1 calc R . . C19 C 1.3144(5) 0.9093(4) -0.0324(4) 0.0505(12) Uani 1 1 d . . . H19A H 1.3883 0.9011 -0.0446 0.076 Uiso 1 1 calc R . . H19B H 1.3195 0.9785 -0.0193 0.076 Uiso 1 1 calc R . . H19C H 1.2355 0.8742 -0.0911 0.076 Uiso 1 1 calc R . . C20 C 1.4862(4) 1.0149(4) 0.1931(4) 0.0532(12) Uani 1 1 d . . . H20A H 1.5627 1.0113 0.1824 0.080 Uiso 1 1 calc R . . H20B H 1.5103 1.0390 0.2643 0.080 Uiso 1 1 calc R . . H20C H 1.4470 1.0592 0.1555 0.080 Uiso 1 1 calc R . . C21 C 0.6377(5) 0.6225(3) -0.0829(4) 0.0542(13) Uani 1 1 d . . . C22 C 0.5303(4) 0.6421(3) -0.0713(4) 0.0516(13) Uani 1 1 d . . . C23 C 0.5438(4) 0.6344(3) 0.0258(4) 0.0420(10) Uani 1 1 d . . . C24 C 0.6614(4) 0.6148(3) 0.0757(4) 0.0390(10) Uani 1 1 d . . . C25 C 0.7192(4) 0.6070(3) 0.0085(4) 0.0461(11) Uani 1 1 d . . . C26 C 0.6616(9) 0.6200(5) -0.1752(6) 0.116(3) Uani 1 1 d . . . H26A H 0.5896 0.6316 -0.2281 0.174 Uiso 1 1 calc R . . H26B H 0.6706 0.5562 -0.1969 0.174 Uiso 1 1 calc R . . H26C H 0.7404 0.6704 -0.1610 0.174 Uiso 1 1 calc R . . C27 C 0.4223(6) 0.6700(5) -0.1455(6) 0.105(3) Uani 1 1 d . . . H27A H 0.4283 0.7377 -0.1214 0.158 Uiso 1 1 calc R . . H27B H 0.3403 0.6280 -0.1533 0.158 Uiso 1 1 calc R . . H27C H 0.4282 0.6623 -0.2101 0.158 Uiso 1 1 calc R . . C28 C 0.4526(5) 0.6510(4) 0.0702(6) 0.0761(19) Uani 1 1 d . . . H28A H 0.4551 0.7196 0.0796 0.114 Uiso 1 1 calc R . . H28B H 0.4772 0.6328 0.1349 0.114 Uiso 1 1 calc R . . H28C H 0.3657 0.6112 0.0253 0.114 Uiso 1 1 calc R . . C29 C 0.7137(6) 0.6016(4) 0.1808(4) 0.0742(18) Uani 1 1 d . . . H29A H 0.7105 0.5333 0.1798 0.111 Uiso 1 1 calc R . . H29B H 0.6622 0.6208 0.2147 0.111 Uiso 1 1 calc R . . H29C H 0.8025 0.6420 0.2166 0.111 Uiso 1 1 calc R . . C30 C 0.8483(5) 0.5895(4) 0.0321(7) 0.099(3) Uani 1 1 d . . . H30A H 0.9077 0.6256 0.1000 0.148 Uiso 1 1 calc R . . H30B H 0.8814 0.6116 -0.0155 0.148 Uiso 1 1 calc R . . H30C H 0.8395 0.5201 0.0270 0.148 Uiso 1 1 calc R . . C31 C 1.0877(19) 0.4497(13) 0.2584(15) 0.096(7) Uani 0.50 1 d PD A 1 H31A H 1.1032 0.3892 0.2353 0.144 Uiso 0.50 1 calc PR A 1 H31B H 1.1687 0.4954 0.3071 0.144 Uiso 0.50 1 calc PR A 1 H31C H 1.0511 0.4782 0.2015 0.144 Uiso 0.50 1 calc PR A 1 C32 C 0.9991(8) 0.4297(7) 0.3050(7) 0.066(3) Uani 0.50 1 d PGD A 1 C33 C 0.9646(12) 0.5065(5) 0.3432(9) 0.074(6) Uani 0.50 1 d PG A 1 H33 H 1.0015 0.5708 0.3409 0.089 Uiso 0.50 1 calc PR A 1 C34 C 0.8762(13) 0.4892(6) 0.3848(11) 0.094(8) Uani 0.50 1 d PG A 1 H34 H 0.8527 0.5417 0.4110 0.112 Uiso 0.50 1 calc PR A 1 C35 C 0.8223(10) 0.3952(7) 0.3882(9) 0.077(4) Uani 0.50 1 d PG A 1 H35 H 0.7619 0.3834 0.4167 0.093 Uiso 0.50 1 calc PR A 1 C36 C 0.8568(10) 0.3184(5) 0.3500(8) 0.081(5) Uani 0.50 1 d PG A 1 H36 H 0.8200 0.2541 0.3523 0.097 Uiso 0.50 1 calc PR A 1 C37 C 0.9452(10) 0.3356(6) 0.3084(8) 0.053(4) Uani 0.50 1 d PG A 1 H37 H 0.9688 0.2832 0.2822 0.063 Uiso 0.50 1 calc PR A 1 C31A C 0.821(3) 0.464(3) 0.399(2) 0.202(17) Uani 0.50 1 d P B 2 H31D H 0.8238 0.5324 0.4079 0.302 Uiso 0.50 1 calc PR B 2 H31E H 0.8479 0.4464 0.4639 0.302 Uiso 0.50 1 calc PR B 2 H31F H 0.7342 0.4237 0.3552 0.302 Uiso 0.50 1 calc PR B 2 C32A C 0.9059(7) 0.4474(5) 0.3550(6) 0.078(5) Uani 0.50 1 d PG B 2 C33A C 0.9058(8) 0.3507(5) 0.3410(7) 0.070(5) Uani 0.50 1 d PG B 2 H33A H 0.8495 0.3047 0.3568 0.085 Uiso 0.50 1 calc PR B 2 C34A C 0.9879(10) 0.3214(6) 0.3039(9) 0.084(6) Uani 0.50 1 d PG B 2 H34A H 0.9878 0.2553 0.2943 0.101 Uiso 0.50 1 calc PR B 2 C35A C 1.0702(7) 0.3888(6) 0.2808(6) 0.085(5) Uani 0.50 1 d PG B 2 H35A H 1.1263 0.3687 0.2554 0.102 Uiso 0.50 1 calc PR B 2 C36A C 1.0703(9) 0.4855(6) 0.2949(9) 0.101(8) Uani 0.50 1 d PG B 2 H36A H 1.1266 0.5315 0.2791 0.121 Uiso 0.50 1 calc PR B 2 C37A C 0.9882(10) 0.5148(5) 0.3320(10) 0.083(6) Uani 0.50 1 d PG B 2 H37A H 0.9883 0.5809 0.3416 0.100 Uiso 0.50 1 calc PR B 2 C38 C 0.3755(12) 0.4184(11) 0.5472(12) 0.070(4) Uani 0.50 1 d PG B 1 H38A H 0.4371 0.4561 0.6139 0.105 Uiso 0.50 1 calc PR B 1 H38B H 0.3021 0.3760 0.5522 0.105 Uiso 0.50 1 calc PR B 1 H38C H 0.3463 0.4627 0.5047 0.105 Uiso 0.50 1 calc PR B 1 C39 C 0.4382(9) 0.3581(6) 0.5026(7) 0.070(3) Uani 0.50 1 d PG B 1 C40 C 0.3700(6) 0.2982(7) 0.4075(8) 0.062(5) Uani 0.50 1 d PG B 1 H40 H 0.2827 0.2944 0.3711 0.075 Uiso 0.50 1 calc PR B 1 C41 C 0.4296(8) 0.2439(7) 0.3659(6) 0.083(6) Uani 0.50 1 d PG B 1 H41 H 0.3830 0.2029 0.3009 0.099 Uiso 0.50 1 calc PR B 1 C42 C 0.5573(8) 0.2495(6) 0.4192(7) 0.078(4) Uani 0.50 1 d PG B 1 H42 H 0.5981 0.2123 0.3907 0.094 Uiso 0.50 1 calc PR B 1 C43 C 0.6255(7) 0.3094(7) 0.5143(7) 0.075(4) Uani 0.50 1 d PG B 1 H43 H 0.7129 0.3132 0.5507 0.090 Uiso 0.50 1 calc PR B 1 C44 C 0.5660(10) 0.3637(7) 0.5559(6) 0.067(5) Uani 0.50 1 d PG B 1 H44 H 0.6126 0.4046 0.6209 0.080 Uiso 0.50 1 calc PR B 1 C38A C 0.4659(19) 0.2066(11) 0.3674(14) 0.090(6) Uani 0.50 1 d P C 2 H38D H 0.3863 0.1820 0.3066 0.136 Uiso 0.50 1 calc PR C 2 H38E H 0.4822 0.1537 0.4009 0.136 Uiso 0.50 1 calc PR C 2 H38F H 0.5370 0.2324 0.3498 0.136 Uiso 0.50 1 calc PR C 2 C39A C 0.4541(9) 0.2844(6) 0.4348(6) 0.061(3) Uani 0.50 1 d PG C 2 C40A C 0.5564(7) 0.3299(6) 0.5261(7) 0.061(4) Uani 0.50 1 d PG C 2 H40A H 0.6340 0.3125 0.5435 0.073 Uiso 0.50 1 calc PR C 2 C41A C 0.5452(9) 0.4009(7) 0.5919(6) 0.086(5) Uani 0.50 1 d PG C 2 H41A H 0.6151 0.4320 0.6543 0.104 Uiso 0.50 1 calc PR C 2 C42A C 0.4316(10) 0.4264(7) 0.5663(7) 0.080(5) Uani 0.50 1 d PG C 2 H42A H 0.4239 0.4749 0.6113 0.095 Uiso 0.50 1 calc PR C 2 C43A C 0.3293(7) 0.3809(7) 0.4750(8) 0.068(3) Uani 0.50 1 d PG C 2 H43A H 0.2517 0.3984 0.4576 0.082 Uiso 0.50 1 calc PR C 2 C44A C 0.3406(8) 0.3099(7) 0.4092(6) 0.059(4) Uani 0.50 1 d PG C 2 H44A H 0.2707 0.2789 0.3468 0.071 Uiso 0.50 1 calc PR C 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 Cr1 0.0299(3) 0.0351(4) 0.0353(4) 0.0119(3) 0.0170(3) 0.0135(3) Cr2 0.0263(3) 0.0367(4) 0.0380(4) 0.0157(3) 0.0169(3) 0.0157(3) Cr3 0.0276(3) 0.0311(3) 0.0409(4) 0.0120(3) 0.0155(3) 0.0107(3) Cr4 0.0261(3) 0.0322(3) 0.0349(4) 0.0118(3) 0.0140(3) 0.0123(2) F1 0.0504(14) 0.0382(14) 0.0525(16) 0.0169(12) 0.0267(12) 0.0213(11) F2 0.0312(11) 0.0440(13) 0.0387(13) 0.0145(11) 0.0194(10) 0.0156(10) F3 0.0324(11) 0.0399(13) 0.0409(14) 0.0109(11) 0.0154(10) 0.0132(10) F4 0.0309(11) 0.0339(12) 0.0415(13) 0.0136(10) 0.0144(10) 0.0154(9) F5 0.0310(11) 0.0362(12) 0.0406(14) 0.0143(10) 0.0137(10) 0.0139(9) F6 0.0315(11) 0.0380(13) 0.0425(14) 0.0154(11) 0.0147(10) 0.0117(9) F7 0.0361(12) 0.0388(13) 0.0586(16) 0.0139(12) 0.0226(12) 0.0165(10) F8 0.0440(13) 0.0379(13) 0.0414(14) 0.0056(11) 0.0199(11) 0.0153(11) F9 0.0308(11) 0.0380(13) 0.0384(13) 0.0109(10) 0.0206(10) 0.0135(9) C1 0.038(2) 0.044(2) 0.035(2) 0.0082(19) 0.0176(18) 0.0151(18) C2 0.039(2) 0.036(2) 0.041(2) 0.0052(19) 0.0214(19) 0.0073(17) C3 0.041(2) 0.034(2) 0.039(2) 0.0125(18) 0.0221(19) 0.0162(17) C4 0.038(2) 0.040(2) 0.041(2) 0.0113(19) 0.0249(19) 0.0175(18) C5 0.040(2) 0.037(2) 0.036(2) 0.0120(18) 0.0225(18) 0.0162(17) C6 0.040(2) 0.069(3) 0.039(3) 0.010(2) 0.013(2) 0.017(2) C7 0.053(3) 0.043(3) 0.057(3) 0.004(2) 0.031(2) 0.005(2) C8 0.062(3) 0.044(3) 0.050(3) 0.019(2) 0.029(2) 0.029(2) C9 0.038(2) 0.058(3) 0.054(3) 0.014(2) 0.027(2) 0.020(2) C10 0.063(3) 0.048(3) 0.046(3) 0.021(2) 0.032(2) 0.023(2) C11 0.0285(19) 0.054(3) 0.046(3) 0.022(2) 0.0184(18) 0.0218(19) C12 0.037(2) 0.041(2) 0.050(3) 0.021(2) 0.0268(19) 0.0237(18) C13 0.035(2) 0.045(2) 0.047(3) 0.015(2) 0.0209(19) 0.0255(19) C14 0.036(2) 0.049(3) 0.050(3) 0.023(2) 0.028(2) 0.0226(19) C15 0.0276(19) 0.050(3) 0.047(3) 0.020(2) 0.0207(19) 0.0192(18) C16 0.041(2) 0.072(3) 0.045(3) 0.024(3) 0.018(2) 0.026(2) C17 0.052(3) 0.050(3) 0.070(3) 0.037(3) 0.038(3) 0.030(2) C18 0.046(3) 0.056(3) 0.055(3) 0.010(2) 0.025(2) 0.027(2) C19 0.060(3) 0.065(3) 0.053(3) 0.032(3) 0.037(2) 0.034(3) C20 0.041(2) 0.057(3) 0.069(4) 0.022(3) 0.029(2) 0.013(2) C21 0.074(3) 0.033(2) 0.048(3) -0.003(2) 0.032(3) -0.005(2) C22 0.043(2) 0.029(2) 0.057(3) 0.014(2) 0.000(2) -0.0042(18) C23 0.031(2) 0.033(2) 0.066(3) 0.014(2) 0.024(2) 0.0092(17) C24 0.036(2) 0.027(2) 0.054(3) 0.0165(19) 0.016(2) 0.0102(17) C25 0.036(2) 0.031(2) 0.078(4) 0.011(2) 0.031(2) 0.0092(18) C26 0.193(9) 0.065(4) 0.085(5) -0.016(4) 0.097(6) -0.026(5) C27 0.069(4) 0.065(4) 0.112(6) 0.042(4) -0.028(4) -0.007(3) C28 0.056(3) 0.051(3) 0.141(6) 0.017(4) 0.064(4) 0.014(3) C29 0.086(4) 0.051(3) 0.057(4) 0.029(3) 0.004(3) 0.001(3) C30 0.053(3) 0.046(3) 0.207(9) 0.005(4) 0.068(5) 0.021(3) C31 0.102(12) 0.061(11) 0.075(14) 0.009(9) 0.000(10) -0.003(9) C32 0.071(7) 0.051(7) 0.047(7) 0.017(5) -0.006(6) 0.012(6) C33 0.084(12) 0.030(9) 0.065(12) 0.022(9) -0.007(10) -0.003(8) C34 0.125(19) 0.031(7) 0.079(14) 0.018(8) -0.006(11) 0.018(8) C35 0.077(9) 0.076(10) 0.055(8) 0.000(7) -0.002(7) 0.037(8) C36 0.105(12) 0.054(9) 0.052(8) 0.026(7) 0.001(8) 0.012(8) C37 0.072(9) 0.032(6) 0.047(8) 0.010(5) 0.010(6) 0.026(6) C31A 0.16(3) 0.35(5) 0.066(15) 0.00(2) -0.009(16) 0.13(3) C32A 0.050(7) 0.125(16) 0.044(7) 0.003(9) 0.004(6) 0.036(9) C33A 0.084(11) 0.053(10) 0.051(9) 0.032(8) 0.000(8) 0.012(8) C34A 0.084(12) 0.060(9) 0.085(11) 0.001(8) 0.005(9) 0.039(8) C35A 0.083(10) 0.117(14) 0.054(8) 0.009(9) 0.013(7) 0.060(11) C36A 0.080(12) 0.092(16) 0.073(14) 0.036(12) -0.009(9) -0.025(11) C37A 0.088(12) 0.058(12) 0.073(14) 0.003(10) -0.007(11) 0.041(9) C38 0.059(10) 0.065(9) 0.071(11) 0.020(8) 0.017(9) 0.002(7) C39 0.071(8) 0.054(7) 0.073(9) 0.025(7) 0.025(7) 0.000(6) C40 0.038(6) 0.057(9) 0.080(12) 0.033(9) 0.011(7) 0.005(6) C41 0.073(10) 0.051(10) 0.070(10) 0.022(8) -0.014(8) -0.013(7) C42 0.062(7) 0.062(8) 0.103(12) 0.040(8) 0.023(8) 0.008(6) C43 0.058(7) 0.067(8) 0.071(9) 0.027(7) -0.005(7) 0.010(6) C44 0.080(10) 0.047(10) 0.045(9) 0.008(9) 0.004(7) 0.001(7) C38A 0.140(16) 0.062(10) 0.109(14) 0.036(9) 0.095(14) 0.018(10) C39A 0.066(8) 0.048(7) 0.066(8) 0.021(6) 0.030(7) 0.001(6) C40A 0.070(9) 0.058(10) 0.038(7) 0.007(7) 0.006(6) 0.019(7) C41A 0.096(11) 0.062(10) 0.060(10) 0.009(7) -0.004(8) 0.013(8) C42A 0.055(10) 0.085(11) 0.074(11) 0.019(8) 0.005(8) 0.009(9) C43A 0.068(8) 0.058(8) 0.066(9) 0.026(7) 0.018(7) 0.004(6) C44A 0.058(8) 0.057(9) 0.055(9) 0.016(7) 0.022(7) 0.001(7) _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 Cr1 F1 1.859(2) . ? Cr1 F3 1.947(2) . ? Cr1 F2 1.957(2) . ? Cr1 C1 2.185(4) . ? Cr1 C5 2.204(4) . ? Cr1 C2 2.217(4) . ? Cr1 C3 2.220(4) . ? Cr1 C4 2.222(4) . ? Cr2 F2 1.932(2) . ? Cr2 F5 1.951(2) . ? Cr2 F4 1.955(2) . ? Cr2 C12 2.187(4) . ? Cr2 C11 2.201(4) . ? Cr2 C13 2.203(4) . ? Cr2 C14 2.209(4) . ? Cr2 C15 2.232(4) . ? Cr3 F7 1.857(2) . ? Cr3 F3 1.952(2) . ? Cr3 F6 1.968(2) . ? Cr3 C22 2.181(4) . ? Cr3 C23 2.206(4) . ? Cr3 C24 2.212(4) . ? Cr3 C21 2.215(5) . ? Cr3 C25 2.221(4) . ? Cr4 F8 1.821(2) . ? Cr4 F6 1.900(2) 2_775 ? Cr4 F4 1.911(2) 2_775 ? Cr4 F5 1.926(2) . ? Cr4 F9 1.930(2) . ? Cr4 F9 1.969(2) 2_775 ? F4 Cr4 1.911(2) 2_775 ? F6 Cr4 1.900(2) 2_775 ? F9 Cr4 1.969(2) 2_775 ? C1 C5 1.426(6) . ? C1 C2 1.427(6) . ? C1 C6 1.500(6) . ? C2 C3 1.417(6) . ? C2 C7 1.496(6) . ? C3 C4 1.430(6) . ? C3 C8 1.511(6) . ? C4 C5 1.415(6) . ? C4 C9 1.506(6) . ? C5 C10 1.501(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.425(6) . ? C11 C12 1.427(6) . ? C11 C16 1.497(7) . ? C12 C13 1.413(6) . ? C12 C17 1.503(6) . ? C13 C14 1.421(6) . ? C13 C18 1.504(7) . ? C14 C15 1.427(6) . ? C14 C19 1.500(6) . ? C15 C20 1.478(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.415(7) . ? C21 C22 1.417(7) . ? C21 C26 1.494(8) . ? C22 C23 1.411(7) . ? C22 C27 1.508(7) . ? C23 C24 1.413(6) . ? C23 C28 1.498(7) . ? C24 C25 1.407(6) . ? C24 C29 1.502(7) . ? C25 C30 1.511(6) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.451(15) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C33 C34 1.3900 . ? C33 H33 0.9500 . ? C34 C35 1.3900 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 C37 1.3900 . ? C36 H36 0.9500 . ? C37 H37 0.9500 . ? C31A C32A 1.42(3) . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A C33A 1.3900 . ? C32A C37A 1.3900 . ? C33A C34A 1.3900 . ? C33A H33A 0.9500 . ? C34A C35A 1.3900 . ? C34A H34A 0.9500 . ? C35A C36A 1.3900 . ? C35A H35A 0.9500 . ? C36A C37A 1.3900 . ? C36A H36A 0.9500 . ? C37A H37A 0.9500 . ? C38 C39 1.497(13) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40 0.9500 . ? C41 C42 1.3900 . ? C41 H41 0.9500 . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C38A C39A 1.476(18) . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A C40A 1.3900 . ? C39A C44A 1.3900 . ? C40A C41A 1.3900 . ? C40A H40A 0.9500 . ? C41A C42A 1.3900 . ? C41A H41A 0.9500 . ? C42A C43A 1.3900 . ? C42A H42A 0.9500 . ? C43A C44A 1.3900 . ? C43A H43A 0.9500 . ? C44A H44A 0.9500 . ? 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 F1 Cr1 F3 95.44(11) . . ? F1 Cr1 F2 91.36(10) . . ? F3 Cr1 F2 93.13(10) . . ? F1 Cr1 C1 100.23(14) . . ? F3 Cr1 C1 156.32(12) . . ? F2 Cr1 C1 104.05(13) . . ? F1 Cr1 C5 92.78(13) . . ? F3 Cr1 C5 124.20(13) . . ? F2 Cr1 C5 141.77(13) . . ? C1 Cr1 C5 37.91(15) . . ? F1 Cr1 C2 135.67(14) . . ? F3 Cr1 C2 128.84(13) . . ? F2 Cr1 C2 88.43(13) . . ? C1 Cr1 C2 37.81(16) . . ? C5 Cr1 C2 62.86(15) . . ? F1 Cr1 C3 155.30(13) . . ? F3 Cr1 C3 96.13(13) . . ? F2 Cr1 C3 109.69(12) . . ? C1 Cr1 C3 62.98(15) . . ? C5 Cr1 C3 62.73(15) . . ? C2 Cr1 C3 37.25(15) . . ? F1 Cr1 C4 119.82(13) . . ? F3 Cr1 C4 93.91(13) . . ? F2 Cr1 C4 147.12(13) . . ? C1 Cr1 C4 62.89(15) . . ? C5 Cr1 C4 37.28(15) . . ? C2 Cr1 C4 62.49(15) . . ? C3 Cr1 C4 37.57(14) . . ? F2 Cr2 F5 90.61(10) . . ? F2 Cr2 F4 92.19(10) . . ? F5 Cr2 F4 94.69(9) . . ? F2 Cr2 C12 96.09(13) . . ? F5 Cr2 C12 153.94(13) . . ? F4 Cr2 C12 110.13(14) . . ? F2 Cr2 C11 92.86(13) . . ? F5 Cr2 C11 116.76(14) . . ? F4 Cr2 C11 148.07(14) . . ? C12 Cr2 C11 37.95(17) . . ? F2 Cr2 C13 129.73(13) . . ? F5 Cr2 C13 139.21(13) . . ? F4 Cr2 C13 90.10(13) . . ? C12 Cr2 C13 37.55(16) . . ? C11 Cr2 C13 62.88(16) . . ? F2 Cr2 C14 155.53(13) . . ? F5 Cr2 C14 103.09(13) . . ? F4 Cr2 C14 106.54(14) . . ? C12 Cr2 C14 63.05(15) . . ? C11 Cr2 C14 62.92(16) . . ? C13 Cr2 C14 37.58(16) . . ? F2 Cr2 C15 123.17(13) . . ? F5 Cr2 C15 92.39(13) . . ? F4 Cr2 C15 143.85(14) . . ? C12 Cr2 C15 62.93(15) . . ? C11 Cr2 C15 37.48(15) . . ? C13 Cr2 C15 62.58(16) . . ? C14 Cr2 C15 37.49(16) . . ? F7 Cr3 F3 94.66(11) . . ? F7 Cr3 F6 92.71(10) . . ? F3 Cr3 F6 94.21(10) . . ? F7 Cr3 C22 100.79(16) . . ? F3 Cr3 C22 155.27(14) . . ? F6 Cr3 C22 104.13(16) . . ? F7 Cr3 C23 92.99(13) . . ? F3 Cr3 C23 123.13(15) . . ? F6 Cr3 C23 141.54(15) . . ? C22 Cr3 C23 37.52(19) . . ? F7 Cr3 C24 119.33(14) . . ? F3 Cr3 C24 92.72(13) . . ? F6 Cr3 C24 146.51(14) . . ? C22 Cr3 C24 62.89(17) . . ? C23 Cr3 C24 37.31(15) . . ? F7 Cr3 C21 136.37(17) . . ? F3 Cr3 C21 128.77(17) . . ? F6 Cr3 C21 88.47(15) . . ? C22 Cr3 C21 37.6(2) . . ? C23 Cr3 C21 62.08(18) . . ? C24 Cr3 C21 62.12(18) . . ? F7 Cr3 C25 154.57(13) . . ? F3 Cr3 C25 95.67(15) . . ? F6 Cr3 C25 109.60(15) . . ? C22 Cr3 C25 62.79(17) . . ? C23 Cr3 C25 61.99(15) . . ? C24 Cr3 C25 37.02(17) . . ? C21 Cr3 C25 37.21(19) . . ? F8 Cr4 F6 94.16(11) . 2_775 ? F8 Cr4 F4 92.11(10) . 2_775 ? F6 Cr4 F4 91.09(9) 2_775 2_775 ? F8 Cr4 F5 92.47(11) . . ? F6 Cr4 F5 89.89(9) 2_775 . ? F4 Cr4 F5 175.24(11) 2_775 . ? F8 Cr4 F9 94.74(10) . . ? F6 Cr4 F9 171.09(11) 2_775 . ? F4 Cr4 F9 88.18(9) 2_775 . ? F5 Cr4 F9 90.13(9) . . ? F8 Cr4 F9 173.69(10) . 2_775 ? F6 Cr4 F9 92.16(10) 2_775 2_775 ? F4 Cr4 F9 87.85(10) 2_775 2_775 ? F5 Cr4 F9 87.46(10) . 2_775 ? F9 Cr4 F9 78.94(10) . 2_775 ? Cr2 F2 Cr1 151.68(13) . . ? Cr1 F3 Cr3 166.17(13) . . ? Cr4 F4 Cr2 134.02(12) 2_775 . ? Cr4 F5 Cr2 132.98(13) . . ? Cr4 F6 Cr3 144.38(13) 2_775 . ? Cr4 F9 Cr4 101.05(10) . 2_775 ? C5 C1 C2 107.8(3) . . ? C5 C1 C6 125.0(4) . . ? C2 C1 C6 127.2(4) . . ? C5 C1 Cr1 71.8(2) . . ? C2 C1 Cr1 72.3(2) . . ? C6 C1 Cr1 120.5(3) . . ? C3 C2 C1 108.0(3) . . ? C3 C2 C7 126.6(4) . . ? C1 C2 C7 125.3(4) . . ? C3 C2 Cr1 71.5(2) . . ? C1 C2 Cr1 69.9(2) . . ? C7 C2 Cr1 122.1(3) . . ? C2 C3 C4 107.9(3) . . ? C2 C3 C8 127.0(4) . . ? C4 C3 C8 125.1(4) . . ? C2 C3 Cr1 71.3(2) . . ? C4 C3 Cr1 71.3(2) . . ? C8 C3 Cr1 121.2(3) . . ? C5 C4 C3 108.1(3) . . ? C5 C4 C9 126.9(4) . . ? C3 C4 C9 125.0(4) . . ? C5 C4 Cr1 70.7(2) . . ? C3 C4 Cr1 71.1(2) . . ? C9 C4 Cr1 123.3(3) . . ? C4 C5 C1 108.1(4) . . ? C4 C5 C10 126.6(4) . . ? C1 C5 C10 125.4(4) . . ? C4 C5 Cr1 72.0(2) . . ? C1 C5 Cr1 70.3(2) . . ? C10 C5 Cr1 122.2(3) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 108.0(4) . . ? C15 C11 C16 127.3(4) . . ? C12 C11 C16 124.7(4) . . ? C15 C11 Cr2 72.5(2) . . ? C12 C11 Cr2 70.5(2) . . ? C16 C11 Cr2 122.0(3) . . ? C13 C12 C11 108.0(4) . . ? C13 C12 C17 127.5(4) . . ? C11 C12 C17 124.5(4) . . ? C13 C12 Cr2 71.8(2) . . ? C11 C12 Cr2 71.5(2) . . ? C17 C12 Cr2 123.5(3) . . ? C12 C13 C14 108.4(4) . . ? C12 C13 C18 126.7(4) . . ? C14 C13 C18 124.8(4) . . ? C12 C13 Cr2 70.6(2) . . ? C14 C13 Cr2 71.5(2) . . ? C18 C13 Cr2 121.0(3) . . ? C13 C14 C15 107.9(4) . . ? C13 C14 C19 126.3(4) . . ? C15 C14 C19 125.6(4) . . ? C13 C14 Cr2 71.0(2) . . ? C15 C14 Cr2 72.1(2) . . ? C19 C14 Cr2 125.2(3) . . ? C11 C15 C14 107.6(4) . . ? C11 C15 C20 127.2(4) . . ? C14 C15 C20 125.1(4) . . ? C11 C15 Cr2 70.1(2) . . ? C14 C15 Cr2 70.4(2) . . ? C20 C15 Cr2 124.0(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 108.1(4) . . ? C25 C21 C26 126.0(6) . . ? C22 C21 C26 125.9(6) . . ? C25 C21 Cr3 71.6(3) . . ? C22 C21 Cr3 69.9(3) . . ? C26 C21 Cr3 123.5(4) . . ? C23 C22 C21 107.4(4) . . ? C23 C22 C27 124.8(6) . . ? C21 C22 C27 127.7(6) . . ? C23 C22 Cr3 72.2(3) . . ? C21 C22 Cr3 72.5(3) . . ? C27 C22 Cr3 119.1(4) . . ? C22 C23 C24 108.5(4) . . ? C22 C23 C28 125.4(5) . . ? C24 C23 C28 125.9(5) . . ? C22 C23 Cr3 70.3(2) . . ? C24 C23 Cr3 71.6(2) . . ? C28 C23 Cr3 120.9(3) . . ? C25 C24 C23 107.9(4) . . ? C25 C24 C29 126.0(4) . . ? C23 C24 C29 126.1(5) . . ? C25 C24 Cr3 71.8(2) . . ? C23 C24 Cr3 71.1(2) . . ? C29 C24 Cr3 124.0(3) . . ? C24 C25 C21 108.0(4) . . ? C24 C25 C30 125.6(6) . . ? C21 C25 C30 126.3(6) . . ? C24 C25 Cr3 71.1(2) . . ? C21 C25 Cr3 71.2(3) . . ? C30 C25 Cr3 121.4(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C37 120.0 . . ? C33 C32 C31 118.6(10) . . ? C37 C32 C31 121.4(10) . . ? C32 C33 C34 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 120.0 . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C37 C36 C35 120.0 . . ? C37 C36 H36 120.0 . . ? C35 C36 H36 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H37 120.0 . . ? C32 C37 H37 120.0 . . ? C32A C31A H31D 109.5 . . ? C32A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C32A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C33A C32A C37A 120.0 . . ? C33A C32A C31A 111.5(15) . . ? C37A C32A C31A 128.4(15) . . ? C32A C33A C34A 120.0 . . ? C32A C33A H33A 120.0 . . ? C34A C33A H33A 120.0 . . ? C35A C34A C33A 120.0 . . ? C35A C34A H34A 120.0 . . ? C33A C34A H34A 120.0 . . ? C34A C35A C36A 120.0 . . ? C34A C35A H35A 120.0 . . ? C36A C35A H35A 120.0 . . ? C37A C36A C35A 120.0 . . ? C37A C36A H36A 120.0 . . ? C35A C36A H36A 120.0 . . ? C36A C37A C32A 120.0 . . ? C36A C37A H37A 120.0 . . ? C32A C37A H37A 120.0 . . ? C39 C38 H38A 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C39 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 120.0 . . ? C40 C39 C38 120.3(10) . . ? C44 C39 C38 119.6(10) . . ? C41 C40 C39 120.0 . . ? C41 C40 H40 120.0 . . ? C39 C40 H40 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41 120.0 . . ? C42 C41 H41 120.0 . . ? C43 C42 C41 120.0 . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44 120.0 . . ? C39 C44 H44 120.0 . . ? C39A C38A H38D 109.5 . . ? C39A C38A H38E 109.5 . . ? H38D C38A H38E 109.5 . . ? C39A C38A H38F 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? C40A C39A C44A 120.0 . . ? C40A C39A C38A 119.3(10) . . ? C44A C39A C38A 120.6(10) . . ? C41A C40A C39A 120.0 . . ? C41A C40A H40A 120.0 . . ? C39A C40A H40A 120.0 . . ? C40A C41A C42A 120.0 . . ? C40A C41A H41A 120.0 . . ? C42A C41A H41A 120.0 . . ? C43A C42A C41A 120.0 . . ? C43A C42A H42A 120.0 . . ? C41A C42A H42A 120.0 . . ? C42A C43A C44A 120.0 . . ? C42A C43A H43A 120.0 . . ? C44A C43A H43A 120.0 . . ? C43A C44A C39A 120.0 . . ? C43A C44A H44A 120.0 . . ? C39A C44A H44A 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F5 Cr2 F2 Cr1 105.4(3) . . . . ? F4 Cr2 F2 Cr1 10.7(3) . . . . ? C12 Cr2 F2 Cr1 -99.8(3) . . . . ? C11 Cr2 F2 Cr1 -137.8(3) . . . . ? C13 Cr2 F2 Cr1 -81.3(3) . . . . ? C14 Cr2 F2 Cr1 -129.8(3) . . . . ? C15 Cr2 F2 Cr1 -161.3(3) . . . . ? F1 Cr1 F2 Cr2 86.1(3) . . . . ? F3 Cr1 F2 Cr2 -9.4(3) . . . . ? C1 Cr1 F2 Cr2 -173.0(3) . . . . ? C5 Cr1 F2 Cr2 -177.7(2) . . . . ? C2 Cr1 F2 Cr2 -138.3(3) . . . . ? C3 Cr1 F2 Cr2 -107.1(3) . . . . ? C4 Cr1 F2 Cr2 -111.6(3) . . . . ? F1 Cr1 F3 Cr3 77.2(6) . . . . ? F2 Cr1 F3 Cr3 168.9(5) . . . . ? C1 Cr1 F3 Cr3 -54.2(7) . . . . ? C5 Cr1 F3 Cr3 -19.9(6) . . . . ? C2 Cr1 F3 Cr3 -100.6(6) . . . . ? C3 Cr1 F3 Cr3 -80.9(6) . . . . ? C4 Cr1 F3 Cr3 -43.3(6) . . . . ? F7 Cr3 F3 Cr1 72.2(5) . . . . ? F6 Cr3 F3 Cr1 165.3(5) . . . . ? C22 Cr3 F3 Cr1 -56.5(7) . . . . ? C23 Cr3 F3 Cr1 -24.4(6) . . . . ? C24 Cr3 F3 Cr1 -47.5(6) . . . . ? C21 Cr3 F3 Cr1 -103.3(6) . . . . ? C25 Cr3 F3 Cr1 -84.5(6) . . . . ? F2 Cr2 F4 Cr4 109.37(17) . . . 2_775 ? F5 Cr2 F4 Cr4 18.58(18) . . . 2_775 ? C12 Cr2 F4 Cr4 -153.33(18) . . . 2_775 ? C11 Cr2 F4 Cr4 -151.7(2) . . . 2_775 ? C13 Cr2 F4 Cr4 -120.87(19) . . . 2_775 ? C14 Cr2 F4 Cr4 -86.6(2) . . . 2_775 ? C15 Cr2 F4 Cr4 -82.0(3) . . . 2_775 ? F8 Cr4 F5 Cr2 143.15(17) . . . . ? F6 Cr4 F5 Cr2 -122.70(17) 2_775 . . . ? F4 Cr4 F5 Cr2 -20.8(13) 2_775 . . . ? F9 Cr4 F5 Cr2 48.39(17) . . . . ? F9 Cr4 F5 Cr2 -30.53(16) 2_775 . . . ? F2 Cr2 F5 Cr4 -107.11(17) . . . . ? F4 Cr2 F5 Cr4 -14.87(17) . . . . ? C12 Cr2 F5 Cr4 147.6(3) . . . . ? C11 Cr2 F5 Cr4 159.38(17) . . . . ? C13 Cr2 F5 Cr4 80.7(2) . . . . ? C14 Cr2 F5 Cr4 93.33(19) . . . . ? C15 Cr2 F5 Cr4 129.66(19) . . . . ? F7 Cr3 F6 Cr4 109.8(2) . . . 2_775 ? F3 Cr3 F6 Cr4 15.0(2) . . . 2_775 ? C22 Cr3 F6 Cr4 -148.3(2) . . . 2_775 ? C23 Cr3 F6 Cr4 -151.9(2) . . . 2_775 ? C24 Cr3 F6 Cr4 -86.4(3) . . . 2_775 ? C21 Cr3 F6 Cr4 -113.8(3) . . . 2_775 ? C25 Cr3 F6 Cr4 -82.6(3) . . . 2_775 ? F8 Cr4 F9 Cr4 -179.88(10) . . . 2_775 ? F6 Cr4 F9 Cr4 2.7(6) 2_775 . . 2_775 ? F4 Cr4 F9 Cr4 88.16(10) 2_775 . . 2_775 ? F5 Cr4 F9 Cr4 -87.39(10) . . . 2_775 ? F9 Cr4 F9 Cr4 0.000(2) 2_775 . . 2_775 ? F1 Cr1 C1 C5 -81.3(2) . . . . ? F3 Cr1 C1 C5 49.4(4) . . . . ? F2 Cr1 C1 C5 -175.3(2) . . . . ? C2 Cr1 C1 C5 116.3(3) . . . . ? C3 Cr1 C1 C5 79.5(2) . . . . ? C4 Cr1 C1 C5 37.1(2) . . . . ? F1 Cr1 C1 C2 162.4(2) . . . . ? F3 Cr1 C1 C2 -67.0(4) . . . . ? F2 Cr1 C1 C2 68.4(2) . . . . ? C5 Cr1 C1 C2 -116.3(3) . . . . ? C3 Cr1 C1 C2 -36.8(2) . . . . ? C4 Cr1 C1 C2 -79.2(2) . . . . ? F1 Cr1 C1 C6 39.2(4) . . . . ? F3 Cr1 C1 C6 169.8(3) . . . . ? F2 Cr1 C1 C6 -54.9(4) . . . . ? C5 Cr1 C1 C6 120.4(5) . . . . ? C2 Cr1 C1 C6 -123.2(5) . . . . ? C3 Cr1 C1 C6 -160.1(4) . . . . ? C4 Cr1 C1 C6 157.5(4) . . . . ? C5 C1 C2 C3 -1.8(5) . . . . ? C6 C1 C2 C3 176.9(4) . . . . ? Cr1 C1 C2 C3 61.6(3) . . . . ? C5 C1 C2 C7 -179.2(4) . . . . ? C6 C1 C2 C7 -0.5(7) . . . . ? Cr1 C1 C2 C7 -115.7(4) . . . . ? C5 C1 C2 Cr1 -63.4(3) . . . . ? C6 C1 C2 Cr1 115.3(4) . . . . ? F1 Cr1 C2 C3 -143.3(2) . . . . ? F3 Cr1 C2 C3 33.6(3) . . . . ? F2 Cr1 C2 C3 126.4(2) . . . . ? C1 Cr1 C2 C3 -118.1(3) . . . . ? C5 Cr1 C2 C3 -79.8(2) . . . . ? C4 Cr1 C2 C3 -37.7(2) . . . . ? F1 Cr1 C2 C1 -25.2(3) . . . . ? F3 Cr1 C2 C1 151.7(2) . . . . ? F2 Cr1 C2 C1 -115.6(2) . . . . ? C5 Cr1 C2 C1 38.2(2) . . . . ? C3 Cr1 C2 C1 118.1(3) . . . . ? C4 Cr1 C2 C1 80.4(2) . . . . ? F1 Cr1 C2 C7 94.5(4) . . . . ? F3 Cr1 C2 C7 -88.6(4) . . . . ? F2 Cr1 C2 C7 4.2(4) . . . . ? C1 Cr1 C2 C7 119.7(5) . . . . ? C5 Cr1 C2 C7 158.0(4) . . . . ? C3 Cr1 C2 C7 -122.2(5) . . . . ? C4 Cr1 C2 C7 -159.9(4) . . . . ? C1 C2 C3 C4 1.6(5) . . . . ? C7 C2 C3 C4 179.0(4) . . . . ? Cr1 C2 C3 C4 62.3(3) . . . . ? C1 C2 C3 C8 -176.0(4) . . . . ? C7 C2 C3 C8 1.3(7) . . . . ? Cr1 C2 C3 C8 -115.4(4) . . . . ? C1 C2 C3 Cr1 -60.6(3) . . . . ? C7 C2 C3 Cr1 116.7(4) . . . . ? F1 Cr1 C3 C2 88.2(4) . . . . ? F3 Cr1 C3 C2 -154.3(2) . . . . ? F2 Cr1 C3 C2 -58.8(3) . . . . ? C1 Cr1 C3 C2 37.4(2) . . . . ? C5 Cr1 C3 C2 80.2(3) . . . . ? C4 Cr1 C3 C2 117.2(4) . . . . ? F1 Cr1 C3 C4 -29.0(5) . . . . ? F3 Cr1 C3 C4 88.4(2) . . . . ? F2 Cr1 C3 C4 -176.0(2) . . . . ? C1 Cr1 C3 C4 -79.9(3) . . . . ? C5 Cr1 C3 C4 -37.0(2) . . . . ? C2 Cr1 C3 C4 -117.2(4) . . . . ? F1 Cr1 C3 C8 -149.3(3) . . . . ? F3 Cr1 C3 C8 -31.8(3) . . . . ? F2 Cr1 C3 C8 63.7(4) . . . . ? C1 Cr1 C3 C8 159.9(4) . . . . ? C5 Cr1 C3 C8 -157.3(4) . . . . ? C2 Cr1 C3 C8 122.5(4) . . . . ? C4 Cr1 C3 C8 -120.3(4) . . . . ? C2 C3 C4 C5 -0.9(5) . . . . ? C8 C3 C4 C5 176.8(4) . . . . ? Cr1 C3 C4 C5 61.4(3) . . . . ? C2 C3 C4 C9 179.7(4) . . . . ? C8 C3 C4 C9 -2.6(7) . . . . ? Cr1 C3 C4 C9 -118.0(4) . . . . ? C2 C3 C4 Cr1 -62.2(3) . . . . ? C8 C3 C4 Cr1 115.5(4) . . . . ? F1 Cr1 C4 C5 48.6(3) . . . . ? F3 Cr1 C4 C5 147.2(2) . . . . ? F2 Cr1 C4 C5 -110.9(3) . . . . ? C1 Cr1 C4 C5 -37.7(2) . . . . ? C2 Cr1 C4 C5 -80.5(3) . . . . ? C3 Cr1 C4 C5 -117.9(4) . . . . ? F1 Cr1 C4 C3 166.5(2) . . . . ? F3 Cr1 C4 C3 -95.0(2) . . . . ? F2 Cr1 C4 C3 6.9(4) . . . . ? C1 Cr1 C4 C3 80.1(3) . . . . ? C5 Cr1 C4 C3 117.9(4) . . . . ? C2 Cr1 C4 C3 37.4(2) . . . . ? F1 Cr1 C4 C9 -73.5(4) . . . . ? F3 Cr1 C4 C9 25.1(3) . . . . ? F2 Cr1 C4 C9 127.0(3) . . . . ? C1 Cr1 C4 C9 -159.8(4) . . . . ? C5 Cr1 C4 C9 -122.1(5) . . . . ? C2 Cr1 C4 C9 157.4(4) . . . . ? C3 Cr1 C4 C9 120.0(5) . . . . ? C3 C4 C5 C1 -0.2(5) . . . . ? C9 C4 C5 C1 179.2(4) . . . . ? Cr1 C4 C5 C1 61.4(3) . . . . ? C3 C4 C5 C10 -178.8(4) . . . . ? C9 C4 C5 C10 0.6(7) . . . . ? Cr1 C4 C5 C10 -117.1(4) . . . . ? C3 C4 C5 Cr1 -61.7(3) . . . . ? C9 C4 C5 Cr1 117.7(4) . . . . ? C2 C1 C5 C4 1.2(5) . . . . ? C6 C1 C5 C4 -177.5(4) . . . . ? Cr1 C1 C5 C4 -62.5(3) . . . . ? C2 C1 C5 C10 179.8(4) . . . . ? C6 C1 C5 C10 1.1(7) . . . . ? Cr1 C1 C5 C10 116.1(4) . . . . ? C2 C1 C5 Cr1 63.7(3) . . . . ? C6 C1 C5 Cr1 -115.0(4) . . . . ? F1 Cr1 C5 C4 -139.3(2) . . . . ? F3 Cr1 C5 C4 -40.8(3) . . . . ? F2 Cr1 C5 C4 124.9(2) . . . . ? C1 Cr1 C5 C4 117.5(3) . . . . ? C2 Cr1 C5 C4 79.4(3) . . . . ? C3 Cr1 C5 C4 37.3(2) . . . . ? F1 Cr1 C5 C1 103.1(2) . . . . ? F3 Cr1 C5 C1 -158.4(2) . . . . ? F2 Cr1 C5 C1 7.4(3) . . . . ? C2 Cr1 C5 C1 -38.1(2) . . . . ? C3 Cr1 C5 C1 -80.2(3) . . . . ? C4 Cr1 C5 C1 -117.5(3) . . . . ? F1 Cr1 C5 C10 -16.9(3) . . . . ? F3 Cr1 C5 C10 81.6(4) . . . . ? F2 Cr1 C5 C10 -112.7(3) . . . . ? C1 Cr1 C5 C10 -120.1(4) . . . . ? C2 Cr1 C5 C10 -158.2(4) . . . . ? C3 Cr1 C5 C10 159.7(4) . . . . ? C4 Cr1 C5 C10 122.4(5) . . . . ? F2 Cr2 C11 C15 -146.6(3) . . . . ? F5 Cr2 C11 C15 -54.5(3) . . . . ? F4 Cr2 C11 C15 114.6(3) . . . . ? C12 Cr2 C11 C15 117.1(4) . . . . ? C13 Cr2 C11 C15 79.5(3) . . . . ? C14 Cr2 C11 C15 37.1(3) . . . . ? F2 Cr2 C11 C12 96.2(2) . . . . ? F5 Cr2 C11 C12 -171.6(2) . . . . ? F4 Cr2 C11 C12 -2.5(4) . . . . ? C13 Cr2 C11 C12 -37.7(2) . . . . ? C14 Cr2 C11 C12 -80.1(3) . . . . ? C15 Cr2 C11 C12 -117.1(4) . . . . ? F2 Cr2 C11 C16 -23.1(4) . . . . ? F5 Cr2 C11 C16 69.0(4) . . . . ? F4 Cr2 C11 C16 -121.9(4) . . . . ? C12 Cr2 C11 C16 -119.4(5) . . . . ? C13 Cr2 C11 C16 -157.0(4) . . . . ? C14 Cr2 C11 C16 160.6(4) . . . . ? C15 Cr2 C11 C16 123.5(5) . . . . ? C15 C11 C12 C13 -0.2(4) . . . . ? C16 C11 C12 C13 179.0(4) . . . . ? Cr2 C11 C12 C13 63.0(3) . . . . ? C15 C11 C12 C17 178.3(3) . . . . ? C16 C11 C12 C17 -2.6(6) . . . . ? Cr2 C11 C12 C17 -118.5(4) . . . . ? C15 C11 C12 Cr2 -63.2(3) . . . . ? C16 C11 C12 Cr2 116.0(4) . . . . ? F2 Cr2 C12 C13 156.3(2) . . . . ? F5 Cr2 C12 C13 -99.7(4) . . . . ? F4 Cr2 C12 C13 61.7(3) . . . . ? C11 Cr2 C12 C13 -116.9(3) . . . . ? C14 Cr2 C12 C13 -37.1(2) . . . . ? C15 Cr2 C12 C13 -79.4(3) . . . . ? F2 Cr2 C12 C11 -86.8(2) . . . . ? F5 Cr2 C12 C11 17.2(4) . . . . ? F4 Cr2 C12 C11 178.6(2) . . . . ? C13 Cr2 C12 C11 116.9(3) . . . . ? C14 Cr2 C12 C11 79.7(3) . . . . ? C15 Cr2 C12 C11 37.4(2) . . . . ? F2 Cr2 C12 C17 32.8(4) . . . . ? F5 Cr2 C12 C17 136.9(4) . . . . ? F4 Cr2 C12 C17 -61.8(4) . . . . ? C11 Cr2 C12 C17 119.7(5) . . . . ? C13 Cr2 C12 C17 -123.5(5) . . . . ? C14 Cr2 C12 C17 -160.6(5) . . . . ? C15 Cr2 C12 C17 157.1(5) . . . . ? C11 C12 C13 C14 -1.0(4) . . . . ? C17 C12 C13 C14 -179.4(4) . . . . ? Cr2 C12 C13 C14 61.8(3) . . . . ? C11 C12 C13 C18 -177.5(4) . . . . ? C17 C12 C13 C18 4.1(6) . . . . ? Cr2 C12 C13 C18 -114.7(4) . . . . ? C11 C12 C13 Cr2 -62.8(3) . . . . ? C17 C12 C13 Cr2 118.8(4) . . . . ? F2 Cr2 C13 C12 -31.3(3) . . . . ? F5 Cr2 C13 C12 138.5(2) . . . . ? F4 Cr2 C13 C12 -124.2(2) . . . . ? C11 Cr2 C13 C12 38.1(2) . . . . ? C14 Cr2 C13 C12 118.1(4) . . . . ? C15 Cr2 C13 C12 80.4(3) . . . . ? F2 Cr2 C13 C14 -149.4(2) . . . . ? F5 Cr2 C13 C14 20.4(3) . . . . ? F4 Cr2 C13 C14 117.7(2) . . . . ? C12 Cr2 C13 C14 -118.1(4) . . . . ? C11 Cr2 C13 C14 -80.0(3) . . . . ? C15 Cr2 C13 C14 -37.7(2) . . . . ? F2 Cr2 C13 C18 90.5(4) . . . . ? F5 Cr2 C13 C18 -99.7(4) . . . . ? F4 Cr2 C13 C18 -2.4(4) . . . . ? C12 Cr2 C13 C18 121.8(5) . . . . ? C11 Cr2 C13 C18 159.9(4) . . . . ? C14 Cr2 C13 C18 -120.1(5) . . . . ? C15 Cr2 C13 C18 -157.7(4) . . . . ? C12 C13 C14 C15 1.8(4) . . . . ? C18 C13 C14 C15 178.4(3) . . . . ? Cr2 C13 C14 C15 63.1(3) . . . . ? C12 C13 C14 C19 178.5(4) . . . . ? C18 C13 C14 C19 -4.8(6) . . . . ? Cr2 C13 C14 C19 -120.2(4) . . . . ? C12 C13 C14 Cr2 -61.3(3) . . . . ? C18 C13 C14 Cr2 115.3(4) . . . . ? F2 Cr2 C14 C13 71.0(4) . . . . ? F5 Cr2 C14 C13 -166.5(2) . . . . ? F4 Cr2 C14 C13 -67.5(2) . . . . ? C12 Cr2 C14 C13 37.1(2) . . . . ? C11 Cr2 C14 C13 79.9(3) . . . . ? C15 Cr2 C14 C13 117.0(3) . . . . ? F2 Cr2 C14 C15 -46.0(5) . . . . ? F5 Cr2 C14 C15 76.5(2) . . . . ? F4 Cr2 C14 C15 175.5(2) . . . . ? C12 Cr2 C14 C15 -79.9(3) . . . . ? C11 Cr2 C14 C15 -37.1(2) . . . . ? C13 Cr2 C14 C15 -117.0(3) . . . . ? F2 Cr2 C14 C19 -167.4(3) . . . . ? F5 Cr2 C14 C19 -44.9(4) . . . . ? F4 Cr2 C14 C19 54.1(4) . . . . ? C12 Cr2 C14 C19 158.7(5) . . . . ? C11 Cr2 C14 C19 -158.5(5) . . . . ? C13 Cr2 C14 C19 121.6(5) . . . . ? C15 Cr2 C14 C19 -121.5(5) . . . . ? C12 C11 C15 C14 1.2(4) . . . . ? C16 C11 C15 C14 -177.9(4) . . . . ? Cr2 C11 C15 C14 -60.7(3) . . . . ? C12 C11 C15 C20 -180.0(4) . . . . ? C16 C11 C15 C20 0.9(7) . . . . ? Cr2 C11 C15 C20 118.1(4) . . . . ? C12 C11 C15 Cr2 61.9(3) . . . . ? C16 C11 C15 Cr2 -117.2(4) . . . . ? C13 C14 C15 C11 -1.8(4) . . . . ? C19 C14 C15 C11 -178.7(4) . . . . ? Cr2 C14 C15 C11 60.5(3) . . . . ? C13 C14 C15 C20 179.3(4) . . . . ? C19 C14 C15 C20 2.5(6) . . . . ? Cr2 C14 C15 C20 -118.4(4) . . . . ? C13 C14 C15 Cr2 -62.3(3) . . . . ? C19 C14 C15 Cr2 120.9(4) . . . . ? F2 Cr2 C15 C11 41.0(3) . . . . ? F5 Cr2 C15 C11 133.3(3) . . . . ? F4 Cr2 C15 C11 -125.4(3) . . . . ? C12 Cr2 C15 C11 -37.9(3) . . . . ? C13 Cr2 C15 C11 -80.4(3) . . . . ? C14 Cr2 C15 C11 -118.1(4) . . . . ? F2 Cr2 C15 C14 159.2(2) . . . . ? F5 Cr2 C15 C14 -108.6(2) . . . . ? F4 Cr2 C15 C14 -7.3(4) . . . . ? C12 Cr2 C15 C14 80.2(3) . . . . ? C11 Cr2 C15 C14 118.1(4) . . . . ? C13 Cr2 C15 C14 37.8(2) . . . . ? F2 Cr2 C15 C20 -81.1(4) . . . . ? F5 Cr2 C15 C20 11.2(4) . . . . ? F4 Cr2 C15 C20 112.5(4) . . . . ? C12 Cr2 C15 C20 -160.0(4) . . . . ? C11 Cr2 C15 C20 -122.1(5) . . . . ? C13 Cr2 C15 C20 157.5(4) . . . . ? C14 Cr2 C15 C20 119.8(5) . . . . ? F7 Cr3 C21 C25 -141.5(2) . . . . ? F3 Cr3 C21 C25 32.0(3) . . . . ? F6 Cr3 C21 C25 126.2(3) . . . . ? C22 Cr3 C21 C25 -118.1(4) . . . . ? C23 Cr3 C21 C25 -79.6(3) . . . . ? C24 Cr3 C21 C25 -37.2(2) . . . . ? F7 Cr3 C21 C22 -23.5(4) . . . . ? F3 Cr3 C21 C22 150.0(3) . . . . ? F6 Cr3 C21 C22 -115.8(3) . . . . ? C23 Cr3 C21 C22 38.5(3) . . . . ? C24 Cr3 C21 C22 80.9(3) . . . . ? C25 Cr3 C21 C22 118.1(4) . . . . ? F7 Cr3 C21 C26 97.0(6) . . . . ? F3 Cr3 C21 C26 -89.5(6) . . . . ? F6 Cr3 C21 C26 4.7(6) . . . . ? C22 Cr3 C21 C26 120.4(7) . . . . ? C23 Cr3 C21 C26 158.9(7) . . . . ? C24 Cr3 C21 C26 -158.7(7) . . . . ? C25 Cr3 C21 C26 -121.5(7) . . . . ? C25 C21 C22 C23 -2.5(5) . . . . ? C26 C21 C22 C23 178.3(5) . . . . ? Cr3 C21 C22 C23 -64.2(3) . . . . ? C25 C21 C22 C27 175.4(5) . . . . ? C26 C21 C22 C27 -3.9(8) . . . . ? Cr3 C21 C22 C27 113.6(5) . . . . ? C25 C21 C22 Cr3 61.8(3) . . . . ? C26 C21 C22 Cr3 -117.5(5) . . . . ? F7 Cr3 C22 C23 -80.7(3) . . . . ? F3 Cr3 C22 C23 47.0(6) . . . . ? F6 Cr3 C22 C23 -176.3(2) . . . . ? C24 Cr3 C22 C23 36.8(2) . . . . ? C21 Cr3 C22 C23 115.5(4) . . . . ? C25 Cr3 C22 C23 78.6(3) . . . . ? F7 Cr3 C22 C21 163.8(3) . . . . ? F3 Cr3 C22 C21 -68.5(5) . . . . ? F6 Cr3 C22 C21 68.2(3) . . . . ? C23 Cr3 C22 C21 -115.5(4) . . . . ? C24 Cr3 C22 C21 -78.7(3) . . . . ? C25 Cr3 C22 C21 -36.9(3) . . . . ? F7 Cr3 C22 C27 39.8(6) . . . . ? F3 Cr3 C22 C27 167.5(5) . . . . ? F6 Cr3 C22 C27 -55.8(6) . . . . ? C23 Cr3 C22 C27 120.5(7) . . . . ? C24 Cr3 C22 C27 157.3(6) . . . . ? C21 Cr3 C22 C27 -124.0(7) . . . . ? C25 Cr3 C22 C27 -160.9(6) . . . . ? C21 C22 C23 C24 2.7(5) . . . . ? C27 C22 C23 C24 -175.2(4) . . . . ? Cr3 C22 C23 C24 -61.7(3) . . . . ? C21 C22 C23 C28 179.0(4) . . . . ? C27 C22 C23 C28 1.1(8) . . . . ? Cr3 C22 C23 C28 114.5(5) . . . . ? C21 C22 C23 Cr3 64.5(3) . . . . ? C27 C22 C23 Cr3 -113.5(5) . . . . ? F7 Cr3 C23 C22 103.9(3) . . . . ? F3 Cr3 C23 C22 -158.6(3) . . . . ? F6 Cr3 C23 C22 5.7(4) . . . . ? C24 Cr3 C23 C22 -118.3(4) . . . . ? C21 Cr3 C23 C22 -38.6(3) . . . . ? C25 Cr3 C23 C22 -80.9(3) . . . . ? F7 Cr3 C23 C24 -137.8(3) . . . . ? F3 Cr3 C23 C24 -40.3(3) . . . . ? F6 Cr3 C23 C24 124.1(3) . . . . ? C22 Cr3 C23 C24 118.3(4) . . . . ? C21 Cr3 C23 C24 79.8(3) . . . . ? C25 Cr3 C23 C24 37.4(3) . . . . ? F7 Cr3 C23 C28 -16.3(5) . . . . ? F3 Cr3 C23 C28 81.2(4) . . . . ? F6 Cr3 C23 C28 -114.5(5) . . . . ? C22 Cr3 C23 C28 -120.2(5) . . . . ? C24 Cr3 C23 C28 121.5(6) . . . . ? C21 Cr3 C23 C28 -158.8(5) . . . . ? C25 Cr3 C23 C28 158.9(5) . . . . ? C22 C23 C24 C25 -1.9(5) . . . . ? C28 C23 C24 C25 -178.2(4) . . . . ? Cr3 C23 C24 C25 -62.8(3) . . . . ? C22 C23 C24 C29 179.7(4) . . . . ? C28 C23 C24 C29 3.5(7) . . . . ? Cr3 C23 C24 C29 118.8(5) . . . . ? C22 C23 C24 Cr3 60.9(3) . . . . ? C28 C23 C24 Cr3 -115.3(5) . . . . ? F7 Cr3 C24 C25 167.3(2) . . . . ? F3 Cr3 C24 C25 -95.8(3) . . . . ? F6 Cr3 C24 C25 6.0(4) . . . . ? C22 Cr3 C24 C25 80.0(3) . . . . ? C23 Cr3 C24 C25 117.0(4) . . . . ? C21 Cr3 C24 C25 37.3(3) . . . . ? F7 Cr3 C24 C23 50.3(3) . . . . ? F3 Cr3 C24 C23 147.2(3) . . . . ? F6 Cr3 C24 C23 -111.0(3) . . . . ? C22 Cr3 C24 C23 -37.0(3) . . . . ? C21 Cr3 C24 C23 -79.6(3) . . . . ? C25 Cr3 C24 C23 -117.0(4) . . . . ? F7 Cr3 C24 C29 -71.1(5) . . . . ? F3 Cr3 C24 C29 25.8(4) . . . . ? F6 Cr3 C24 C29 127.6(4) . . . . ? C22 Cr3 C24 C29 -158.4(5) . . . . ? C23 Cr3 C24 C29 -121.4(6) . . . . ? C21 Cr3 C24 C29 159.0(5) . . . . ? C25 Cr3 C24 C29 121.6(5) . . . . ? C23 C24 C25 C21 0.4(5) . . . . ? C29 C24 C25 C21 178.7(4) . . . . ? Cr3 C24 C25 C21 -62.0(3) . . . . ? C23 C24 C25 C30 178.0(4) . . . . ? C29 C24 C25 C30 -3.7(7) . . . . ? Cr3 C24 C25 C30 115.6(5) . . . . ? C23 C24 C25 Cr3 62.4(3) . . . . ? C29 C24 C25 Cr3 -119.3(4) . . . . ? C22 C21 C25 C24 1.3(5) . . . . ? C26 C21 C25 C24 -179.5(5) . . . . ? Cr3 C21 C25 C24 61.9(3) . . . . ? C22 C21 C25 C30 -176.3(4) . . . . ? C26 C21 C25 C30 3.0(8) . . . . ? Cr3 C21 C25 C30 -115.6(5) . . . . ? C22 C21 C25 Cr3 -60.7(3) . . . . ? C26 C21 C25 Cr3 118.6(5) . . . . ? F7 Cr3 C25 C24 -26.5(5) . . . . ? F3 Cr3 C25 C24 87.0(3) . . . . ? F6 Cr3 C25 C24 -176.5(2) . . . . ? C22 Cr3 C25 C24 -80.3(3) . . . . ? C23 Cr3 C25 C24 -37.7(3) . . . . ? C21 Cr3 C25 C24 -117.5(4) . . . . ? F7 Cr3 C25 C21 91.0(5) . . . . ? F3 Cr3 C25 C21 -155.5(3) . . . . ? F6 Cr3 C25 C21 -58.9(3) . . . . ? C22 Cr3 C25 C21 37.3(3) . . . . ? C23 Cr3 C25 C21 79.8(3) . . . . ? C24 Cr3 C25 C21 117.5(4) . . . . ? F7 Cr3 C25 C30 -147.3(5) . . . . ? F3 Cr3 C25 C30 -33.8(5) . . . . ? F6 Cr3 C25 C30 62.7(6) . . . . ? C22 Cr3 C25 C30 159.0(6) . . . . ? C23 Cr3 C25 C30 -158.5(6) . . . . ? C24 Cr3 C25 C30 -120.8(7) . . . . ? C21 Cr3 C25 C30 121.7(6) . . . . ? C37 C32 C33 C34 0.0 . . . . ? C31 C32 C33 C34 177.6(12) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C32 0.0 . . . . ? C33 C32 C37 C36 0.0 . . . . ? C31 C32 C37 C36 -177.5(12) . . . . ? C37A C32A C33A C34A 0.0 . . . . ? C31A C32A C33A C34A -176.5(14) . . . . ? C32A C33A C34A C35A 0.0 . . . . ? C33A C34A C35A C36A 0.0 . . . . ? C34A C35A C36A C37A 0.0 . . . . ? C35A C36A C37A C32A 0.0 . . . . ? C33A C32A C37A C36A 0.0 . . . . ? C31A C32A C37A C36A 175.8(16) . . . . ? C44 C39 C40 C41 0.0 . . . . ? C38 C39 C40 C41 178.7(9) . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C39 0.0 . . . . ? C40 C39 C44 C43 0.0 . . . . ? C38 C39 C44 C43 -178.7(9) . . . . ? C44A C39A C40A C41A 0.0 . . . . ? C38A C39A C40A C41A -177.7(10) . . . . ? C39A C40A C41A C42A 0.0 . . . . ? C40A C41A C42A C43A 0.0 . . . . ? C41A C42A C43A C44A 0.0 . . . . ? C42A C43A C44A C39A 0.0 . . . . ? C40A C39A C44A C43A 0.0 . . . . ? C38A C39A C44A C43A 177.7(10) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.558 _refine_diff_density_min -0.796 _refine_diff_density_rms 0.089 data_rde134 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C23 H35 Fe),H2F3,HF2' _chemical_formula_sum 'C46 H73 F5 Fe2' _chemical_formula_weight 832.74 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' 'F' 'F' 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6504(2) _cell_length_b 14.6996(3) _cell_length_c 15.6216(3) _cell_angle_alpha 63.3130(11) _cell_angle_beta 81.2757(11) _cell_angle_gamma 81.5338(10) _cell_volume 2151.17(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 60197 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.286 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8116 _exptl_absorpt_correction_T_max 0.9442 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18704 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0591 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9828 _reflns_number_gt 6804 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _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^)+(0.0458P)^2^+1.3583P] 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 9828 _refine_ls_number_parameters 572 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0834 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1136 _refine_ls_wR_factor_gt 0.0980 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _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 0.47685(3) 0.47410(3) 0.72825(2) 0.02277(10) Uani 1 1 d . . . Fe2 Fe 0.13606(4) 0.04520(3) 0.73159(3) 0.02999(11) Uani 1 1 d . . . C1 C 0.5483(3) 0.5763(2) 0.59349(18) 0.0367(6) Uani 1 1 d . . . C1A C 0.2428(4) 0.1223(3) 0.7709(3) 0.0646(12) Uani 1 1 d . . . C2 C 0.4249(3) 0.5553(3) 0.58969(18) 0.0408(7) Uani 1 1 d . . . C2A C 0.3226(4) 0.0492(3) 0.7487(3) 0.0601(10) Uani 1 1 d . . . C3 C 0.4265(3) 0.4496(3) 0.61842(19) 0.0420(7) Uani 1 1 d . . . C3A C 0.2812(3) -0.0472(3) 0.8121(2) 0.0529(9) Uani 1 1 d . . . C4 C 0.5515(3) 0.4044(2) 0.63953(19) 0.0405(7) Uani 1 1 d . . . C4A C 0.1780(4) -0.0333(3) 0.8726(2) 0.0520(9) Uani 1 1 d . . . C5 C 0.6260(3) 0.4830(2) 0.62466(19) 0.0374(6) Uani 1 1 d . . . C5A C 0.1536(4) 0.0728(3) 0.8473(3) 0.0601(10) Uani 1 1 d . . . C6 C 0.5292(2) 0.52624(18) 0.82329(15) 0.0216(5) Uani 1 1 d . . . C6A C 0.0304(2) 0.16549(17) 0.62646(16) 0.0249(5) Uani 1 1 d . . . C7 C 0.3998(2) 0.55970(19) 0.80416(16) 0.0222(5) Uani 1 1 d . . . C7A C 0.1288(2) 0.12028(19) 0.58276(17) 0.0258(5) Uani 1 1 d . . . C8 C 0.3112(2) 0.49124(18) 0.81594(15) 0.0221(5) Uani 1 1 d . . . C8A C 0.1448(2) 0.01395(18) 0.61005(16) 0.0251(5) Uani 1 1 d . . . C9 C 0.3558(2) 0.38687(19) 0.84639(16) 0.0240(5) Uani 1 1 d . . . C9A C 0.0616(2) -0.04816(19) 0.68736(17) 0.0253(5) Uani 1 1 d . . . C10 C 0.4835(2) 0.34940(18) 0.86656(16) 0.0236(5) Uani 1 1 d . . . C10A C -0.0391(2) -0.00714(18) 0.73326(16) 0.0258(5) Uani 1 1 d . . . C11 C 0.5687(2) 0.42114(18) 0.85383(16) 0.0228(5) Uani 1 1 d . . . C11A C -0.0526(3) 0.10038(19) 0.70092(17) 0.0277(5) Uani 1 1 d . . . C12 C 0.6232(2) 0.59995(18) 0.81577(17) 0.0268(5) Uani 1 1 d . . . C12A C 0.0091(3) 0.28198(18) 0.59128(18) 0.0312(6) Uani 1 1 d . . . C13 C 0.7543(2) 0.5808(2) 0.7680(2) 0.0395(7) Uani 1 1 d . . . H13A H 0.7884 0.5099 0.8046 0.059 Uiso 1 1 calc R . . H13B H 0.8125 0.6273 0.7668 0.059 Uiso 1 1 calc R . . H13C H 0.7462 0.5929 0.7020 0.059 Uiso 1 1 calc R . . C13A C -0.0346(3) 0.3115(2) 0.6734(2) 0.0453(7) Uani 1 1 d . . . H13D H -0.0455 0.3861 0.6479 0.068 Uiso 1 1 calc R . . H13E H 0.0295 0.2839 0.7198 0.068 Uiso 1 1 calc R . . H13F H -0.1160 0.2834 0.7055 0.068 Uiso 1 1 calc R . . C14 C 0.5743(3) 0.71184(19) 0.7605(2) 0.0385(7) Uani 1 1 d . . . H14A H 0.5586 0.7248 0.6956 0.058 Uiso 1 1 calc R . . H14B H 0.6382 0.7558 0.7561 0.058 Uiso 1 1 calc R . . H14C H 0.4947 0.7268 0.7944 0.058 Uiso 1 1 calc R . . C14A C 0.1275(3) 0.3355(2) 0.5351(3) 0.0618(10) Uani 1 1 d . . . H14D H 0.1110 0.4088 0.5173 0.093 Uiso 1 1 calc R . . H14E H 0.1487 0.3251 0.4766 0.093 Uiso 1 1 calc R . . H14F H 0.1990 0.3070 0.5750 0.093 Uiso 1 1 calc R . . C15 C 0.6369(3) 0.5790(2) 0.91978(19) 0.0363(6) Uani 1 1 d . . . H15A H 0.5535 0.5919 0.9506 0.055 Uiso 1 1 calc R . . H15B H 0.6964 0.6242 0.9192 0.055 Uiso 1 1 calc R . . H15C H 0.6697 0.5076 0.9557 0.055 Uiso 1 1 calc R . . C15A C -0.0994(4) 0.3185(2) 0.5250(3) 0.0585(10) Uani 1 1 d . . . H15D H -0.1754 0.2837 0.5611 0.088 Uiso 1 1 calc R . . H15E H -0.0726 0.3026 0.4701 0.088 Uiso 1 1 calc R . . H15F H -0.1190 0.3925 0.5018 0.088 Uiso 1 1 calc R . . C16 C 0.1704(2) 0.52642(19) 0.79948(17) 0.0265(5) Uani 1 1 d . . . C16A C 0.2450(2) -0.03422(19) 0.55703(18) 0.0295(5) Uani 1 1 d . . . C17 C 0.1484(2) 0.6419(2) 0.7414(2) 0.0356(6) Uani 1 1 d . . . H17A H 0.1700 0.6760 0.7779 0.053 Uiso 1 1 calc R . . H17B H 0.0586 0.6606 0.7287 0.053 Uiso 1 1 calc R . . H17C H 0.2024 0.6633 0.6802 0.053 Uiso 1 1 calc R . . C17A C 0.3262(3) 0.0456(2) 0.4765(2) 0.0382(6) Uani 1 1 d . . . H17D H 0.3874 0.0123 0.4435 0.057 Uiso 1 1 calc R . . H17E H 0.3725 0.0773 0.5043 0.057 Uiso 1 1 calc R . . H17F H 0.2708 0.0982 0.4304 0.057 Uiso 1 1 calc R . . C18 C 0.0977(2) 0.4966(2) 0.90008(18) 0.0355(6) Uani 1 1 d . . . H18A H 0.1103 0.4225 0.9383 0.053 Uiso 1 1 calc R . . H18B H 0.0066 0.5175 0.8937 0.053 Uiso 1 1 calc R . . H18C H 0.1301 0.5311 0.9323 0.053 Uiso 1 1 calc R . . C18A C 0.3350(3) -0.1183(2) 0.6249(2) 0.0375(6) Uani 1 1 d . . . H18D H 0.2847 -0.1671 0.6800 0.056 Uiso 1 1 calc R . . H18E H 0.3899 -0.0876 0.6478 0.056 Uiso 1 1 calc R . . H18F H 0.3879 -0.1540 0.5903 0.056 Uiso 1 1 calc R . . C19 C 0.1177(2) 0.4741(2) 0.7483(2) 0.0360(6) Uani 1 1 d . . . H19A H 0.1664 0.4906 0.6855 0.054 Uiso 1 1 calc R . . H19B H 0.0278 0.4985 0.7393 0.054 Uiso 1 1 calc R . . H19C H 0.1253 0.3999 0.7876 0.054 Uiso 1 1 calc R . . C19A C 0.1708(3) -0.0814(2) 0.51178(19) 0.0343(6) Uani 1 1 d . . . H19D H 0.1133 -0.0280 0.4681 0.051 Uiso 1 1 calc R . . H19E H 0.1210 -0.1345 0.5628 0.051 Uiso 1 1 calc R . . H19F H 0.2311 -0.1117 0.4757 0.051 Uiso 1 1 calc R . . C20 C 0.5263(2) 0.23518(19) 0.90651(18) 0.0302(6) Uani 1 1 d . . . C20A C -0.1363(3) -0.07354(19) 0.81157(18) 0.0333(6) Uani 1 1 d . . . C21 C 0.4488(3) 0.1784(2) 0.8737(2) 0.0397(7) Uani 1 1 d . . . H21A H 0.3587 0.1848 0.8971 0.060 Uiso 1 1 calc R . . H21B H 0.4806 0.1060 0.8998 0.060 Uiso 1 1 calc R . . H21C H 0.4574 0.2081 0.8032 0.060 Uiso 1 1 calc R . . C21A C -0.0926(3) -0.1872(2) 0.8508(2) 0.0486(8) Uani 1 1 d . . . H21D H -0.0839 -0.2084 0.7988 0.073 Uiso 1 1 calc R . . H21E H -0.1557 -0.2262 0.9021 0.073 Uiso 1 1 calc R . . H21F H -0.0101 -0.2000 0.8766 0.073 Uiso 1 1 calc R . . C22 C 0.5030(3) 0.1944(2) 1.01649(19) 0.0426(7) Uani 1 1 d . . . H22A H 0.5582 0.2259 1.0384 0.064 Uiso 1 1 calc R . . H22B H 0.5225 0.1200 1.0467 0.064 Uiso 1 1 calc R . . H22C H 0.4136 0.2113 1.0345 0.064 Uiso 1 1 calc R . . C22A C -0.2595(3) -0.0519(3) 0.7623(2) 0.0632(10) Uani 1 1 d . . . H22D H -0.2416 -0.0675 0.7066 0.095 Uiso 1 1 calc R . . H22E H -0.2910 0.0202 0.7409 0.095 Uiso 1 1 calc R . . H22F H -0.3244 -0.0949 0.8081 0.095 Uiso 1 1 calc R . . C23 C 0.6672(3) 0.2144(2) 0.8784(3) 0.0509(8) Uani 1 1 d . . . H23A H 0.6823 0.2400 0.8083 0.076 Uiso 1 1 calc R . . H23B H 0.6915 0.1406 0.9091 0.076 Uiso 1 1 calc R . . H23C H 0.7185 0.2492 0.8998 0.076 Uiso 1 1 calc R . . C23A C -0.1637(4) -0.0455(2) 0.8962(2) 0.0536(9) Uani 1 1 d . . . H23D H -0.2327 -0.0841 0.9409 0.080 Uiso 1 1 calc R . . H23E H -0.1894 0.0279 0.8722 0.080 Uiso 1 1 calc R . . H23F H -0.0867 -0.0623 0.9296 0.080 Uiso 1 1 calc R . . F1 F 0.2652(2) 0.71077(17) 0.89586(18) 0.0722(6) Uani 1 1 d . . . H1F H 0.207(4) 0.698(3) 0.958(4) 0.096(14) Uiso 1 1 d . . . F2 F 0.1574(2) 0.65951(17) 1.04695(16) 0.0699(6) Uani 1 1 d . . . H2F H 0.077(4) 0.718(3) 1.055(3) 0.072(11) Uiso 1 1 d . . . F3 F -0.0108(3) 0.76248(19) 1.08279(17) 0.1038(10) Uani 1 1 d . . . F4 F 0.3751(3) 0.8021(2) 0.3674(3) 0.1267(12) Uani 1 1 d . . . H4F H 0.449(4) 0.834(3) 0.393(3) 0.081(13) Uiso 1 1 d . . . F5 F 0.5316(4) 0.8063(2) 0.4487(2) 0.1315(13) Uani 1 1 d . . . H1 H 0.568(3) 0.642(3) 0.576(2) 0.055(10) Uiso 1 1 d . . . H1A H 0.251(3) 0.190(3) 0.735(3) 0.072(12) Uiso 1 1 d . . . H2 H 0.358(3) 0.603(2) 0.574(2) 0.054(10) Uiso 1 1 d . . . H2A H 0.393(4) 0.056(3) 0.697(3) 0.093(14) Uiso 1 1 d . . . H3 H 0.363(3) 0.415(3) 0.624(2) 0.061(11) Uiso 1 1 d . . . H3A H 0.314(3) -0.109(3) 0.810(2) 0.061(10) Uiso 1 1 d . . . H4A H 0.126(3) -0.080(3) 0.919(3) 0.062(11) Uiso 1 1 d . . . H4 H 0.579(3) 0.337(2) 0.660(2) 0.049(9) Uiso 1 1 d . . . H5 H 0.713(3) 0.476(2) 0.635(2) 0.048(9) Uiso 1 1 d . . . H5A H 0.086(4) 0.105(3) 0.873(3) 0.067(11) Uiso 1 1 d . . . H7 H 0.374(2) 0.6299(19) 0.7782(17) 0.021(6) Uiso 1 1 d . . . H7A H 0.189(3) 0.158(2) 0.5388(19) 0.027(7) Uiso 1 1 d . . . H9 H 0.297(2) 0.3411(18) 0.8521(17) 0.022(6) Uiso 1 1 d . . . H9A H 0.079(2) -0.119(2) 0.7125(18) 0.028(7) Uiso 1 1 d . . . H11 H 0.653(2) 0.3994(17) 0.8638(17) 0.019(6) Uiso 1 1 d . . . H11A H -0.112(2) 0.1271(18) 0.7324(18) 0.024(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.02150(18) 0.03098(19) 0.01608(16) -0.01032(15) 0.00031(13) -0.00515(14) Fe2 0.0378(2) 0.0280(2) 0.02506(19) -0.00908(16) -0.01276(16) -0.00417(16) C1 0.0452(17) 0.0410(16) 0.0186(12) -0.0099(12) 0.0086(11) -0.0105(13) C1A 0.087(3) 0.045(2) 0.069(3) -0.013(2) -0.054(2) -0.015(2) C2 0.0403(17) 0.061(2) 0.0167(12) -0.0157(14) -0.0044(12) 0.0056(15) C2A 0.045(2) 0.083(3) 0.051(2) -0.020(2) -0.0275(17) -0.0106(19) C3 0.0455(18) 0.068(2) 0.0243(14) -0.0278(15) 0.0033(12) -0.0199(16) C3A 0.063(2) 0.054(2) 0.0472(19) -0.0235(18) -0.0356(18) 0.0144(18) C4 0.0530(19) 0.0463(18) 0.0249(14) -0.0212(14) 0.0061(13) -0.0032(15) C4A 0.072(2) 0.053(2) 0.0287(16) -0.0089(15) -0.0275(16) -0.0074(18) C5 0.0300(15) 0.0581(19) 0.0233(13) -0.0198(13) 0.0082(11) -0.0061(14) C5A 0.081(3) 0.069(2) 0.051(2) -0.040(2) -0.040(2) 0.012(2) C6 0.0204(12) 0.0287(12) 0.0144(10) -0.0078(10) -0.0004(9) -0.0053(10) C6A 0.0316(14) 0.0237(12) 0.0190(11) -0.0064(10) -0.0067(10) -0.0070(10) C7 0.0205(12) 0.0284(13) 0.0175(11) -0.0095(10) -0.0020(9) -0.0037(10) C7A 0.0260(13) 0.0275(13) 0.0215(12) -0.0060(11) -0.0053(10) -0.0079(11) C8 0.0197(12) 0.0317(13) 0.0165(11) -0.0117(10) 0.0008(9) -0.0061(10) C8A 0.0254(13) 0.0271(12) 0.0218(12) -0.0079(10) -0.0084(10) -0.0026(10) C9 0.0245(13) 0.0308(13) 0.0179(11) -0.0102(10) 0.0009(9) -0.0106(10) C9A 0.0307(14) 0.0231(13) 0.0224(12) -0.0083(11) -0.0066(10) -0.0043(10) C10 0.0242(12) 0.0302(13) 0.0167(11) -0.0099(10) 0.0021(9) -0.0083(10) C10A 0.0307(14) 0.0255(12) 0.0208(12) -0.0084(10) -0.0041(10) -0.0053(10) C11 0.0186(12) 0.0305(13) 0.0181(11) -0.0094(10) -0.0009(9) -0.0035(10) C11A 0.0352(15) 0.0266(13) 0.0226(12) -0.0117(11) -0.0022(11) -0.0042(11) C12 0.0227(13) 0.0280(13) 0.0283(13) -0.0092(11) -0.0032(10) -0.0076(10) C12A 0.0413(16) 0.0242(13) 0.0272(13) -0.0088(11) -0.0060(11) -0.0062(11) C13 0.0247(14) 0.0468(17) 0.0473(17) -0.0198(14) 0.0022(12) -0.0130(12) C13A 0.068(2) 0.0281(15) 0.0409(16) -0.0157(13) -0.0027(15) -0.0066(14) C14 0.0344(15) 0.0302(14) 0.0466(17) -0.0083(13) -0.0114(13) -0.0108(12) C14A 0.066(2) 0.0303(16) 0.076(2) -0.0166(17) 0.0221(19) -0.0177(15) C15 0.0397(16) 0.0400(15) 0.0359(15) -0.0171(13) -0.0096(12) -0.0151(12) C15A 0.087(3) 0.0311(16) 0.059(2) -0.0141(15) -0.045(2) 0.0101(16) C16 0.0186(12) 0.0373(14) 0.0267(12) -0.0158(11) -0.0021(10) -0.0056(10) C16A 0.0242(13) 0.0320(14) 0.0301(13) -0.0118(11) -0.0027(10) -0.0027(10) C17 0.0236(13) 0.0434(16) 0.0390(15) -0.0171(13) -0.0083(11) 0.0019(11) C17A 0.0313(15) 0.0430(16) 0.0352(15) -0.0141(13) 0.0030(12) -0.0050(12) C18 0.0210(13) 0.0581(18) 0.0302(14) -0.0221(14) 0.0042(10) -0.0089(12) C18A 0.0287(14) 0.0396(15) 0.0390(15) -0.0133(13) -0.0072(12) 0.0031(12) C19 0.0245(14) 0.0531(17) 0.0383(15) -0.0247(14) -0.0078(11) -0.0056(12) C19A 0.0332(15) 0.0396(15) 0.0327(14) -0.0191(13) -0.0013(11) -0.0018(12) C20 0.0294(14) 0.0279(13) 0.0319(14) -0.0104(11) -0.0044(11) -0.0055(11) C20A 0.0412(16) 0.0290(14) 0.0240(13) -0.0072(11) 0.0058(11) -0.0102(12) C21 0.0508(18) 0.0312(14) 0.0405(16) -0.0157(13) -0.0088(13) -0.0090(13) C21A 0.066(2) 0.0304(15) 0.0396(16) -0.0105(13) 0.0165(15) -0.0142(14) C22 0.058(2) 0.0310(15) 0.0331(15) -0.0057(13) -0.0150(14) -0.0052(13) C22A 0.0424(19) 0.078(3) 0.0431(18) 0.0001(18) 0.0068(15) -0.0300(18) C23 0.0375(17) 0.0324(16) 0.080(2) -0.0249(16) -0.0017(16) 0.0007(13) C23A 0.077(2) 0.0393(17) 0.0390(17) -0.0180(15) 0.0250(16) -0.0181(16) F1 0.0767(15) 0.0825(15) 0.0768(15) -0.0523(13) 0.0020(12) -0.0155(12) F2 0.0626(14) 0.0730(14) 0.0676(14) -0.0216(12) -0.0160(11) -0.0078(11) F3 0.167(3) 0.0761(16) 0.0588(14) -0.0320(13) -0.0235(16) 0.0380(17) F4 0.140(3) 0.0755(18) 0.175(3) -0.078(2) 0.021(2) -0.0005(18) F5 0.201(4) 0.0777(19) 0.097(2) -0.0174(17) 0.020(2) -0.062(2) _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 C5 2.062(3) . ? Fe1 C3 2.062(3) . ? Fe1 C2 2.065(3) . ? Fe1 C1 2.068(3) . ? Fe1 C4 2.075(3) . ? Fe1 C9 2.086(2) . ? Fe1 C11 2.097(2) . ? Fe1 C7 2.098(2) . ? Fe1 C10 2.118(2) . ? Fe1 C8 2.121(2) . ? Fe1 C6 2.122(2) . ? Fe2 C1A 2.043(3) . ? Fe2 C2A 2.057(3) . ? Fe2 C4A 2.061(3) . ? Fe2 C5A 2.061(3) . ? Fe2 C3A 2.063(3) . ? Fe2 C9A 2.080(2) . ? Fe2 C7A 2.087(2) . ? Fe2 C11A 2.095(3) . ? Fe2 C6A 2.111(2) . ? Fe2 C10A 2.112(2) . ? Fe2 C8A 2.131(2) . ? C1 C2 1.409(4) . ? C1 C5 1.411(4) . ? C1 H1 0.93(3) . ? C1A C5A 1.391(6) . ? C1A C2A 1.406(6) . ? C1A H1A 0.91(4) . ? C2 C3 1.409(5) . ? C2 H2 0.90(3) . ? C2A C3A 1.405(5) . ? C2A H2A 0.99(4) . ? C3 C4 1.413(4) . ? C3 H3 0.87(3) . ? C3A C4A 1.392(5) . ? C3A H3A 0.94(3) . ? C4 C5 1.412(4) . ? C4 H4 0.91(3) . ? C4A C5A 1.419(5) . ? C4A H4A 0.92(4) . ? C5 H5 0.95(3) . ? C5A H5A 0.94(4) . ? C6 C11 1.414(3) . ? C6 C7 1.422(3) . ? C6 C12 1.536(3) . ? C6A C11A 1.410(3) . ? C6A C7A 1.411(4) . ? C6A C12A 1.537(3) . ? C7 C8 1.413(3) . ? C7 H7 0.94(2) . ? C7A C8A 1.414(3) . ? C7A H7A 0.90(3) . ? C8 C9 1.416(3) . ? C8 C16 1.534(3) . ? C8A C9A 1.415(3) . ? C8A C16A 1.537(3) . ? C9 C10 1.416(3) . ? C9 H9 0.95(2) . ? C9A C10A 1.412(3) . ? C9A H9A 0.93(3) . ? C10 C11 1.419(3) . ? C10 C20 1.528(3) . ? C10A C11A 1.418(3) . ? C10A C20A 1.537(3) . ? C11 H11 0.92(2) . ? C11A H11A 0.89(3) . ? C12 C14 1.527(3) . ? C12 C13 1.531(4) . ? C12 C15 1.538(3) . ? C12A C13A 1.520(4) . ? C12A C14A 1.522(4) . ? C12A C15A 1.541(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? C16 C17 1.524(4) . ? C16 C19 1.536(3) . ? C16 C18 1.540(3) . ? C16A C17A 1.533(4) . ? C16A C18A 1.534(3) . ? C16A C19A 1.541(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20 C23 1.524(4) . ? C20 C21 1.536(3) . ? C20 C22 1.537(4) . ? C20A C21A 1.523(4) . ? C20A C23A 1.529(4) . ? C20A C22A 1.543(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? F1 H1F 1.03(5) . ? F2 H1F 1.30(5) . ? F2 H2F 1.15(4) . ? F3 H2F 1.21(4) . ? F4 H4F 1.18(5) . ? F5 H4F 1.22(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 Fe1 C3 66.98(12) . . ? C5 Fe1 C2 66.93(12) . . ? C3 Fe1 C2 39.93(13) . . ? C5 Fe1 C1 39.95(12) . . ? C3 Fe1 C1 67.09(12) . . ? C2 Fe1 C1 39.86(12) . . ? C5 Fe1 C4 39.91(12) . . ? C3 Fe1 C4 39.95(12) . . ? C2 Fe1 C4 67.08(12) . . ? C1 Fe1 C4 67.18(12) . . ? C5 Fe1 C9 150.02(11) . . ? C3 Fe1 C9 103.02(11) . . ? C2 Fe1 C9 124.34(11) . . ? C1 Fe1 C9 163.62(11) . . ? C4 Fe1 C9 114.31(11) . . ? C5 Fe1 C11 103.00(10) . . ? C3 Fe1 C11 149.65(12) . . ? C2 Fe1 C11 163.82(11) . . ? C1 Fe1 C11 124.44(11) . . ? C4 Fe1 C11 114.01(11) . . ? C9 Fe1 C11 70.83(9) . . ? C5 Fe1 C7 136.47(11) . . ? C3 Fe1 C7 136.69(11) . . ? C2 Fe1 C7 107.12(11) . . ? C1 Fe1 C7 106.91(11) . . ? C4 Fe1 C7 173.71(11) . . ? C9 Fe1 C7 70.70(9) . . ? C11 Fe1 C7 70.82(9) . . ? C5 Fe1 C10 118.59(11) . . ? C3 Fe1 C10 118.36(11) . . ? C2 Fe1 C10 156.38(11) . . ? C1 Fe1 C10 156.64(11) . . ? C4 Fe1 C10 101.72(11) . . ? C9 Fe1 C10 39.35(9) . . ? C11 Fe1 C10 39.35(9) . . ? C7 Fe1 C10 84.56(9) . . ? C5 Fe1 C8 169.60(11) . . ? C3 Fe1 C8 109.93(11) . . ? C2 Fe1 C8 104.08(10) . . ? C1 Fe1 C8 129.71(11) . . ? C4 Fe1 C8 143.01(11) . . ? C9 Fe1 C8 39.32(9) . . ? C11 Fe1 C8 84.50(9) . . ? C7 Fe1 C8 39.14(9) . . ? C10 Fe1 C8 71.76(9) . . ? C5 Fe1 C6 109.72(10) . . ? C3 Fe1 C6 170.04(11) . . ? C2 Fe1 C6 130.21(11) . . ? C1 Fe1 C6 104.13(10) . . ? C4 Fe1 C6 142.53(11) . . ? C9 Fe1 C6 84.36(9) . . ? C11 Fe1 C6 39.16(9) . . ? C7 Fe1 C6 39.37(9) . . ? C10 Fe1 C6 71.58(9) . . ? C8 Fe1 C6 71.54(8) . . ? C1A Fe2 C2A 40.13(16) . . ? C1A Fe2 C4A 66.78(15) . . ? C2A Fe2 C4A 66.72(16) . . ? C1A Fe2 C5A 39.63(16) . . ? C2A Fe2 C5A 67.18(17) . . ? C4A Fe2 C5A 40.26(14) . . ? C1A Fe2 C3A 66.97(15) . . ? C2A Fe2 C3A 39.87(15) . . ? C4A Fe2 C3A 39.44(14) . . ? C5A Fe2 C3A 67.13(14) . . ? C1A Fe2 C9A 168.74(15) . . ? C2A Fe2 C9A 128.62(14) . . ? C4A Fe2 C9A 111.34(12) . . ? C5A Fe2 C9A 145.05(15) . . ? C3A Fe2 C9A 104.20(12) . . ? C1A Fe2 C7A 108.91(14) . . ? C2A Fe2 C7A 103.75(13) . . ? C4A Fe2 C7A 169.68(14) . . ? C5A Fe2 C7A 141.33(13) . . ? C3A Fe2 C7A 130.50(13) . . ? C9A Fe2 C7A 70.93(9) . . ? C1A Fe2 C11A 120.14(14) . . ? C2A Fe2 C11A 157.97(14) . . ? C4A Fe2 C11A 119.81(14) . . ? C5A Fe2 C11A 103.43(14) . . ? C3A Fe2 C11A 156.74(13) . . ? C9A Fe2 C11A 70.78(10) . . ? C7A Fe2 C11A 70.51(10) . . ? C1A Fe2 C6A 102.21(12) . . ? C2A Fe2 C6A 124.11(13) . . ? C4A Fe2 C6A 149.27(13) . . ? C5A Fe2 C6A 112.97(12) . . ? C3A Fe2 C6A 163.69(13) . . ? C9A Fe2 C6A 84.77(9) . . ? C7A Fe2 C6A 39.28(9) . . ? C11A Fe2 C6A 39.18(9) . . ? C1A Fe2 C10A 151.30(16) . . ? C2A Fe2 C10A 162.51(14) . . ? C4A Fe2 C10A 103.52(13) . . ? C5A Fe2 C10A 115.51(15) . . ? C3A Fe2 C10A 123.56(13) . . ? C9A Fe2 C10A 39.34(9) . . ? C7A Fe2 C10A 84.61(9) . . ? C11A Fe2 C10A 39.40(9) . . ? C6A Fe2 C10A 71.89(9) . . ? C1A Fe2 C8A 134.58(16) . . ? C2A Fe2 C8A 105.27(14) . . ? C4A Fe2 C8A 137.25(12) . . ? C5A Fe2 C8A 172.41(14) . . ? C3A Fe2 C8A 106.82(12) . . ? C9A Fe2 C8A 39.23(9) . . ? C7A Fe2 C8A 39.16(9) . . ? C11A Fe2 C8A 83.89(9) . . ? C6A Fe2 C8A 71.43(9) . . ? C10A Fe2 C8A 71.44(9) . . ? C2 C1 C5 107.6(3) . . ? C2 C1 Fe1 69.95(16) . . ? C5 C1 Fe1 69.79(15) . . ? C2 C1 H1 122(2) . . ? C5 C1 H1 131(2) . . ? Fe1 C1 H1 126(2) . . ? C5A C1A C2A 109.1(3) . . ? C5A C1A Fe2 70.92(19) . . ? C2A C1A Fe2 70.49(19) . . ? C5A C1A H1A 130(2) . . ? C2A C1A H1A 121(2) . . ? Fe2 C1A H1A 122(2) . . ? C1 C2 C3 108.2(3) . . ? C1 C2 Fe1 70.19(15) . . ? C3 C2 Fe1 69.94(16) . . ? C1 C2 H2 124(2) . . ? C3 C2 H2 128(2) . . ? Fe1 C2 H2 124(2) . . ? C3A C2A C1A 107.4(4) . . ? C3A C2A Fe2 70.3(2) . . ? C1A C2A Fe2 69.4(2) . . ? C3A C2A H2A 121(3) . . ? C1A C2A H2A 132(3) . . ? Fe2 C2A H2A 123(2) . . ? C2 C3 C4 108.3(3) . . ? C2 C3 Fe1 70.13(15) . . ? C4 C3 Fe1 70.51(15) . . ? C2 C3 H3 128(2) . . ? C4 C3 H3 123(2) . . ? Fe1 C3 H3 124(2) . . ? C4A C3A C2A 108.2(3) . . ? C4A C3A Fe2 70.23(18) . . ? C2A C3A Fe2 69.84(18) . . ? C4A C3A H3A 127(2) . . ? C2A C3A H3A 125(2) . . ? Fe2 C3A H3A 122(2) . . ? C5 C4 C3 107.3(3) . . ? C5 C4 Fe1 69.54(16) . . ? C3 C4 Fe1 69.54(16) . . ? C5 C4 H4 126(2) . . ? C3 C4 H4 127(2) . . ? Fe1 C4 H4 125(2) . . ? C3A C4A C5A 108.4(4) . . ? C3A C4A Fe2 70.33(18) . . ? C5A C4A Fe2 69.87(17) . . ? C3A C4A H4A 130(2) . . ? C5A C4A H4A 122(2) . . ? Fe2 C4A H4A 122(2) . . ? C1 C5 C4 108.6(3) . . ? C1 C5 Fe1 70.26(15) . . ? C4 C5 Fe1 70.55(16) . . ? C1 C5 H5 124.2(18) . . ? C4 C5 H5 127.1(18) . . ? Fe1 C5 H5 123.4(18) . . ? C1A C5A C4A 107.0(4) . . ? C1A C5A Fe2 69.45(19) . . ? C4A C5A Fe2 69.87(17) . . ? C1A C5A H5A 126(2) . . ? C4A C5A H5A 127(2) . . ? Fe2 C5A H5A 122(2) . . ? C11 C6 C7 118.0(2) . . ? C11 C6 C12 120.1(2) . . ? C7 C6 C12 121.8(2) . . ? C11 C6 Fe1 69.48(13) . . ? C7 C6 Fe1 69.44(12) . . ? C12 C6 Fe1 135.22(16) . . ? C11A C6A C7A 117.6(2) . . ? C11A C6A C12A 120.6(2) . . ? C7A C6A C12A 121.7(2) . . ? C11A C6A Fe2 69.81(14) . . ? C7A C6A Fe2 69.43(13) . . ? C12A C6A Fe2 134.98(16) . . ? C8 C7 C6 122.0(2) . . ? C8 C7 Fe1 71.28(13) . . ? C6 C7 Fe1 71.19(13) . . ? C8 C7 H7 118.5(15) . . ? C6 C7 H7 119.3(15) . . ? Fe1 C7 H7 127.2(15) . . ? C6A C7A C8A 122.5(2) . . ? C6A C7A Fe2 71.29(14) . . ? C8A C7A Fe2 72.12(14) . . ? C6A C7A H7A 120.5(16) . . ? C8A C7A H7A 116.9(16) . . ? Fe2 C7A H7A 126.4(16) . . ? C7 C8 C9 117.7(2) . . ? C7 C8 C16 122.1(2) . . ? C9 C8 C16 120.2(2) . . ? C7 C8 Fe1 69.58(13) . . ? C9 C8 Fe1 69.02(13) . . ? C16 C8 Fe1 134.51(15) . . ? C7A C8A C9A 117.5(2) . . ? C7A C8A C16A 122.5(2) . . ? C9A C8A C16A 120.0(2) . . ? C7A C8A Fe2 68.73(13) . . ? C9A C8A Fe2 68.46(13) . . ? C16A C8A Fe2 136.40(16) . . ? C8 C9 C10 122.6(2) . . ? C8 C9 Fe1 71.66(13) . . ? C10 C9 Fe1 71.53(13) . . ? C8 C9 H9 117.8(14) . . ? C10 C9 H9 119.5(14) . . ? Fe1 C9 H9 130.1(15) . . ? C10A C9A C8A 122.5(2) . . ? C10A C9A Fe2 71.55(13) . . ? C8A C9A Fe2 72.31(13) . . ? C10A C9A H9A 118.9(16) . . ? C8A C9A H9A 118.3(16) . . ? Fe2 C9A H9A 124.7(15) . . ? C9 C10 C11 117.5(2) . . ? C9 C10 C20 121.4(2) . . ? C11 C10 C20 121.0(2) . . ? C9 C10 Fe1 69.12(13) . . ? C11 C10 Fe1 69.54(13) . . ? C20 C10 Fe1 136.06(17) . . ? C9A C10A C11A 117.4(2) . . ? C9A C10A C20A 122.5(2) . . ? C11A C10A C20A 120.0(2) . . ? C9A C10A Fe2 69.11(14) . . ? C11A C10A Fe2 69.65(14) . . ? C20A C10A Fe2 135.49(17) . . ? C6 C11 C10 122.1(2) . . ? C6 C11 Fe1 71.36(13) . . ? C10 C11 Fe1 71.11(13) . . ? C6 C11 H11 118.5(15) . . ? C10 C11 H11 119.3(15) . . ? Fe1 C11 H11 129.9(15) . . ? C6A C11A C10A 122.4(2) . . ? C6A C11A Fe2 71.02(15) . . ? C10A C11A Fe2 70.95(15) . . ? C6A C11A H11A 118.8(16) . . ? C10A C11A H11A 118.6(16) . . ? Fe2 C11A H11A 127.7(16) . . ? C14 C12 C13 108.8(2) . . ? C14 C12 C6 112.4(2) . . ? C13 C12 C6 111.9(2) . . ? C14 C12 C15 108.7(2) . . ? C13 C12 C15 109.0(2) . . ? C6 C12 C15 106.00(19) . . ? C13A C12A C14A 109.1(2) . . ? C13A C12A C6A 112.3(2) . . ? C14A C12A C6A 112.4(2) . . ? C13A C12A C15A 107.7(3) . . ? C14A C12A C15A 109.5(3) . . ? C6A C12A C15A 105.8(2) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12A C13A H13D 109.5 . . ? C12A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C12A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12A C14A H14D 109.5 . . ? C12A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C12A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C12A C15A H15D 109.5 . . ? C12A C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C12A C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? C17 C16 C8 112.1(2) . . ? C17 C16 C19 108.7(2) . . ? C8 C16 C19 112.0(2) . . ? C17 C16 C18 108.3(2) . . ? C8 C16 C18 106.13(19) . . ? C19 C16 C18 109.4(2) . . ? C17A C16A C18A 108.1(2) . . ? C17A C16A C8A 111.9(2) . . ? C18A C16A C8A 112.4(2) . . ? C17A C16A C19A 108.7(2) . . ? C18A C16A C19A 109.0(2) . . ? C8A C16A C19A 106.6(2) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16A C17A H17D 109.5 . . ? C16A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C16A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16A C18A H18D 109.5 . . ? C16A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C16A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C16A C19A H19D 109.5 . . ? C16A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C16A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C23 C20 C10 112.5(2) . . ? C23 C20 C21 108.3(2) . . ? C10 C20 C21 112.3(2) . . ? C23 C20 C22 109.3(2) . . ? C10 C20 C22 105.3(2) . . ? C21 C20 C22 109.2(2) . . ? C21A C20A C23A 108.2(2) . . ? C21A C20A C10A 112.3(2) . . ? C23A C20A C10A 112.0(2) . . ? C21A C20A C22A 109.4(3) . . ? C23A C20A C22A 109.2(3) . . ? C10A C20A C22A 105.6(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20A C21A H21D 109.5 . . ? C20A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? C20A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20A C22A H22D 109.5 . . ? C20A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C20A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20A C23A H23D 109.5 . . ? C20A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C20A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? H1F F2 H2F 108(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Fe1 C1 C2 118.5(3) . . . . ? C3 Fe1 C1 C2 37.55(18) . . . . ? C4 Fe1 C1 C2 81.1(2) . . . . ? C9 Fe1 C1 C2 -17.7(5) . . . . ? C11 Fe1 C1 C2 -174.65(17) . . . . ? C7 Fe1 C1 C2 -96.65(18) . . . . ? C10 Fe1 C1 C2 146.3(2) . . . . ? C8 Fe1 C1 C2 -59.9(2) . . . . ? C6 Fe1 C1 C2 -137.48(18) . . . . ? C3 Fe1 C1 C5 -80.99(19) . . . . ? C2 Fe1 C1 C5 -118.5(3) . . . . ? C4 Fe1 C1 C5 -37.47(18) . . . . ? C9 Fe1 C1 C5 -136.2(3) . . . . ? C11 Fe1 C1 C5 66.8(2) . . . . ? C7 Fe1 C1 C5 144.80(16) . . . . ? C10 Fe1 C1 C5 27.8(3) . . . . ? C8 Fe1 C1 C5 -178.46(15) . . . . ? C6 Fe1 C1 C5 103.97(17) . . . . ? C2A Fe2 C1A C5A -119.3(3) . . . . ? C4A Fe2 C1A C5A -38.4(2) . . . . ? C3A Fe2 C1A C5A -81.4(2) . . . . ? C9A Fe2 C1A C5A -121.1(7) . . . . ? C7A Fe2 C1A C5A 151.7(2) . . . . ? C11A Fe2 C1A C5A 73.7(2) . . . . ? C6A Fe2 C1A C5A 111.4(2) . . . . ? C10A Fe2 C1A C5A 36.9(4) . . . . ? C8A Fe2 C1A C5A -172.74(19) . . . . ? C4A Fe2 C1A C2A 80.9(2) . . . . ? C5A Fe2 C1A C2A 119.3(3) . . . . ? C3A Fe2 C1A C2A 37.8(2) . . . . ? C9A Fe2 C1A C2A -1.8(8) . . . . ? C7A Fe2 C1A C2A -89.0(2) . . . . ? C11A Fe2 C1A C2A -167.0(2) . . . . ? C6A Fe2 C1A C2A -129.3(2) . . . . ? C10A Fe2 C1A C2A 156.2(2) . . . . ? C8A Fe2 C1A C2A -53.5(3) . . . . ? C5 C1 C2 C3 0.0(3) . . . . ? Fe1 C1 C2 C3 -59.86(18) . . . . ? C5 C1 C2 Fe1 59.88(18) . . . . ? C5 Fe1 C2 C1 -37.81(18) . . . . ? C3 Fe1 C2 C1 -119.0(3) . . . . ? C4 Fe1 C2 C1 -81.33(19) . . . . ? C9 Fe1 C2 C1 174.05(16) . . . . ? C11 Fe1 C2 C1 16.0(5) . . . . ? C7 Fe1 C2 C1 96.09(18) . . . . ? C10 Fe1 C2 C1 -146.7(2) . . . . ? C8 Fe1 C2 C1 136.67(17) . . . . ? C6 Fe1 C2 C1 59.1(2) . . . . ? C5 Fe1 C2 C3 81.18(19) . . . . ? C1 Fe1 C2 C3 119.0(3) . . . . ? C4 Fe1 C2 C3 37.66(18) . . . . ? C9 Fe1 C2 C3 -67.0(2) . . . . ? C11 Fe1 C2 C3 135.0(4) . . . . ? C7 Fe1 C2 C3 -144.93(17) . . . . ? C10 Fe1 C2 C3 -27.7(4) . . . . ? C8 Fe1 C2 C3 -104.34(18) . . . . ? C6 Fe1 C2 C3 178.09(16) . . . . ? C5A C1A C2A C3A 0.4(4) . . . . ? Fe2 C1A C2A C3A -60.3(2) . . . . ? C5A C1A C2A Fe2 60.7(2) . . . . ? C1A Fe2 C2A C3A 118.3(3) . . . . ? C4A Fe2 C2A C3A 37.2(2) . . . . ? C5A Fe2 C2A C3A 81.1(2) . . . . ? C9A Fe2 C2A C3A -62.2(3) . . . . ? C7A Fe2 C2A C3A -138.6(2) . . . . ? C11A Fe2 C2A C3A 149.5(3) . . . . ? C6A Fe2 C2A C3A -175.77(18) . . . . ? C10A Fe2 C2A C3A -21.5(6) . . . . ? C8A Fe2 C2A C3A -98.1(2) . . . . ? C4A Fe2 C2A C1A -81.0(2) . . . . ? C5A Fe2 C2A C1A -37.1(2) . . . . ? C3A Fe2 C2A C1A -118.3(3) . . . . ? C9A Fe2 C2A C1A 179.6(2) . . . . ? C7A Fe2 C2A C1A 103.1(2) . . . . ? C11A Fe2 C2A C1A 31.3(5) . . . . ? C6A Fe2 C2A C1A 66.0(3) . . . . ? C10A Fe2 C2A C1A -139.8(4) . . . . ? C8A Fe2 C2A C1A 143.6(2) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? Fe1 C2 C3 C4 -60.47(18) . . . . ? C1 C2 C3 Fe1 60.02(18) . . . . ? C5 Fe1 C3 C2 -81.04(19) . . . . ? C1 Fe1 C3 C2 -37.49(18) . . . . ? C4 Fe1 C3 C2 -118.8(3) . . . . ? C9 Fe1 C3 C2 128.75(18) . . . . ? C11 Fe1 C3 C2 -157.1(2) . . . . ? C7 Fe1 C3 C2 53.2(2) . . . . ? C10 Fe1 C3 C2 167.76(16) . . . . ? C8 Fe1 C3 C2 88.29(19) . . . . ? C6 Fe1 C3 C2 -8.5(7) . . . . ? C5 Fe1 C3 C4 37.75(18) . . . . ? C2 Fe1 C3 C4 118.8(3) . . . . ? C1 Fe1 C3 C4 81.30(19) . . . . ? C9 Fe1 C3 C4 -112.45(18) . . . . ? C11 Fe1 C3 C4 -38.3(3) . . . . ? C7 Fe1 C3 C4 171.99(17) . . . . ? C10 Fe1 C3 C4 -73.4(2) . . . . ? C8 Fe1 C3 C4 -152.92(17) . . . . ? C6 Fe1 C3 C4 110.3(6) . . . . ? C1A C2A C3A C4A -0.3(3) . . . . ? Fe2 C2A C3A C4A -60.0(2) . . . . ? C1A C2A C3A Fe2 59.7(2) . . . . ? C1A Fe2 C3A C4A 80.9(2) . . . . ? C2A Fe2 C3A C4A 119.0(3) . . . . ? C5A Fe2 C3A C4A 37.7(2) . . . . ? C9A Fe2 C3A C4A -106.5(2) . . . . ? C7A Fe2 C3A C4A 176.67(18) . . . . ? C11A Fe2 C3A C4A -32.2(4) . . . . ? C6A Fe2 C3A C4A 131.6(4) . . . . ? C10A Fe2 C3A C4A -68.6(2) . . . . ? C8A Fe2 C3A C4A -147.1(2) . . . . ? C1A Fe2 C3A C2A -38.1(2) . . . . ? C4A Fe2 C3A C2A -119.0(3) . . . . ? C5A Fe2 C3A C2A -81.3(3) . . . . ? C9A Fe2 C3A C2A 134.5(2) . . . . ? C7A Fe2 C3A C2A 57.7(3) . . . . ? C11A Fe2 C3A C2A -151.2(3) . . . . ? C6A Fe2 C3A C2A 12.6(5) . . . . ? C10A Fe2 C3A C2A 172.4(2) . . . . ? C8A Fe2 C3A C2A 93.8(2) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? Fe1 C3 C4 C5 -59.53(18) . . . . ? C2 C3 C4 Fe1 60.23(18) . . . . ? C3 Fe1 C4 C5 118.6(3) . . . . ? C2 Fe1 C4 C5 80.93(19) . . . . ? C1 Fe1 C4 C5 37.51(18) . . . . ? C9 Fe1 C4 C5 -160.31(16) . . . . ? C11 Fe1 C4 C5 -81.46(19) . . . . ? C7 Fe1 C4 C5 57.8(11) . . . . ? C10 Fe1 C4 C5 -120.91(17) . . . . ? C8 Fe1 C4 C5 163.91(17) . . . . ? C6 Fe1 C4 C5 -46.0(3) . . . . ? C5 Fe1 C4 C3 -118.6(3) . . . . ? C2 Fe1 C4 C3 -37.64(19) . . . . ? C1 Fe1 C4 C3 -81.1(2) . . . . ? C9 Fe1 C4 C3 81.1(2) . . . . ? C11 Fe1 C4 C3 159.97(17) . . . . ? C7 Fe1 C4 C3 -60.8(10) . . . . ? C10 Fe1 C4 C3 120.51(18) . . . . ? C8 Fe1 C4 C3 45.3(3) . . . . ? C6 Fe1 C4 C3 -164.54(18) . . . . ? C2A C3A C4A C5A 0.1(3) . . . . ? Fe2 C3A C4A C5A -59.7(2) . . . . ? C2A C3A C4A Fe2 59.8(2) . . . . ? C1A Fe2 C4A C3A -81.5(3) . . . . ? C2A Fe2 C4A C3A -37.6(2) . . . . ? C5A Fe2 C4A C3A -119.3(3) . . . . ? C9A Fe2 C4A C3A 86.5(2) . . . . ? C7A Fe2 C4A C3A -14.3(8) . . . . ? C11A Fe2 C4A C3A 165.96(19) . . . . ? C6A Fe2 C4A C3A -155.7(2) . . . . ? C10A Fe2 C4A C3A 127.1(2) . . . . ? C8A Fe2 C4A C3A 49.9(3) . . . . ? C1A Fe2 C4A C5A 37.8(3) . . . . ? C2A Fe2 C4A C5A 81.6(3) . . . . ? C3A Fe2 C4A C5A 119.3(3) . . . . ? C9A Fe2 C4A C5A -154.2(2) . . . . ? C7A Fe2 C4A C5A 105.0(7) . . . . ? C11A Fe2 C4A C5A -74.8(3) . . . . ? C6A Fe2 C4A C5A -36.5(4) . . . . ? C10A Fe2 C4A C5A -113.7(2) . . . . ? C8A Fe2 C4A C5A 169.2(2) . . . . ? C2 C1 C5 C4 0.4(3) . . . . ? Fe1 C1 C5 C4 60.40(19) . . . . ? C2 C1 C5 Fe1 -59.98(18) . . . . ? C3 C4 C5 C1 -0.7(3) . . . . ? Fe1 C4 C5 C1 -60.22(18) . . . . ? C3 C4 C5 Fe1 59.53(18) . . . . ? C3 Fe1 C5 C1 81.29(19) . . . . ? C2 Fe1 C5 C1 37.73(18) . . . . ? C4 Fe1 C5 C1 119.1(3) . . . . ? C9 Fe1 C5 C1 157.00(19) . . . . ? C11 Fe1 C5 C1 -128.92(17) . . . . ? C7 Fe1 C5 C1 -53.2(2) . . . . ? C10 Fe1 C5 C1 -167.85(16) . . . . ? C8 Fe1 C5 C1 6.6(7) . . . . ? C6 Fe1 C5 C1 -88.62(18) . . . . ? C3 Fe1 C5 C4 -37.78(19) . . . . ? C2 Fe1 C5 C4 -81.3(2) . . . . ? C1 Fe1 C5 C4 -119.1(3) . . . . ? C9 Fe1 C5 C4 37.9(3) . . . . ? C11 Fe1 C5 C4 112.01(18) . . . . ? C7 Fe1 C5 C4 -172.27(17) . . . . ? C10 Fe1 C5 C4 73.1(2) . . . . ? C8 Fe1 C5 C4 -112.5(6) . . . . ? C6 Fe1 C5 C4 152.31(17) . . . . ? C2A C1A C5A C4A -0.3(3) . . . . ? Fe2 C1A C5A C4A 60.1(2) . . . . ? C2A C1A C5A Fe2 -60.4(2) . . . . ? C3A C4A C5A C1A 0.2(3) . . . . ? Fe2 C4A C5A C1A -59.8(2) . . . . ? C3A C4A C5A Fe2 60.0(2) . . . . ? C2A Fe2 C5A C1A 37.6(2) . . . . ? C4A Fe2 C5A C1A 118.0(4) . . . . ? C3A Fe2 C5A C1A 81.0(3) . . . . ? C9A Fe2 C5A C1A 163.0(2) . . . . ? C7A Fe2 C5A C1A -45.9(3) . . . . ? C11A Fe2 C5A C1A -121.4(2) . . . . ? C6A Fe2 C5A C1A -81.3(2) . . . . ? C10A Fe2 C5A C1A -161.4(2) . . . . ? C8A Fe2 C5A C1A 43.0(11) . . . . ? C1A Fe2 C5A C4A -118.0(4) . . . . ? C2A Fe2 C5A C4A -80.4(3) . . . . ? C3A Fe2 C5A C4A -37.0(2) . . . . ? C9A Fe2 C5A C4A 45.0(4) . . . . ? C7A Fe2 C5A C4A -163.9(2) . . . . ? C11A Fe2 C5A C4A 120.6(2) . . . . ? C6A Fe2 C5A C4A 160.7(2) . . . . ? C10A Fe2 C5A C4A 80.6(3) . . . . ? C8A Fe2 C5A C4A -75.0(11) . . . . ? C5 Fe1 C6 C11 -86.46(16) . . . . ? C3 Fe1 C6 C11 -155.4(6) . . . . ? C2 Fe1 C6 C11 -162.46(15) . . . . ? C1 Fe1 C6 C11 -127.91(15) . . . . ? C4 Fe1 C6 C11 -57.1(2) . . . . ? C9 Fe1 C6 C11 66.33(14) . . . . ? C7 Fe1 C6 C11 132.5(2) . . . . ? C10 Fe1 C6 C11 28.15(14) . . . . ? C8 Fe1 C6 C11 104.46(15) . . . . ? C5 Fe1 C6 C7 141.00(15) . . . . ? C3 Fe1 C6 C7 72.1(6) . . . . ? C2 Fe1 C6 C7 65.00(18) . . . . ? C1 Fe1 C6 C7 99.55(15) . . . . ? C4 Fe1 C6 C7 170.34(18) . . . . ? C9 Fe1 C6 C7 -66.21(14) . . . . ? C11 Fe1 C6 C7 -132.5(2) . . . . ? C10 Fe1 C6 C7 -104.39(15) . . . . ? C8 Fe1 C6 C7 -28.08(14) . . . . ? C5 Fe1 C6 C12 26.1(3) . . . . ? C3 Fe1 C6 C12 -42.8(7) . . . . ? C2 Fe1 C6 C12 -49.9(3) . . . . ? C1 Fe1 C6 C12 -15.3(3) . . . . ? C4 Fe1 C6 C12 55.5(3) . . . . ? C9 Fe1 C6 C12 178.9(2) . . . . ? C11 Fe1 C6 C12 112.6(3) . . . . ? C7 Fe1 C6 C12 -114.9(3) . . . . ? C10 Fe1 C6 C12 140.7(2) . . . . ? C8 Fe1 C6 C12 -143.0(2) . . . . ? C1A Fe2 C6A C11A -123.21(19) . . . . ? C2A Fe2 C6A C11A -160.24(19) . . . . ? C4A Fe2 C6A C11A -58.4(3) . . . . ? C5A Fe2 C6A C11A -83.1(2) . . . . ? C3A Fe2 C6A C11A -169.9(4) . . . . ? C9A Fe2 C6A C11A 65.73(14) . . . . ? C7A Fe2 C6A C11A 131.8(2) . . . . ? C10A Fe2 C6A C11A 27.65(14) . . . . ? C8A Fe2 C6A C11A 103.56(15) . . . . ? C1A Fe2 C6A C7A 105.0(2) . . . . ? C2A Fe2 C6A C7A 68.0(2) . . . . ? C4A Fe2 C6A C7A 169.8(2) . . . . ? C5A Fe2 C6A C7A 145.19(19) . . . . ? C3A Fe2 C6A C7A 58.3(4) . . . . ? C9A Fe2 C6A C7A -66.03(14) . . . . ? C11A Fe2 C6A C7A -131.8(2) . . . . ? C10A Fe2 C6A C7A -104.11(15) . . . . ? C8A Fe2 C6A C7A -28.20(14) . . . . ? C1A Fe2 C6A C12A -9.7(3) . . . . ? C2A Fe2 C6A C12A -46.7(3) . . . . ? C4A Fe2 C6A C12A 55.1(4) . . . . ? C5A Fe2 C6A C12A 30.5(3) . . . . ? C3A Fe2 C6A C12A -56.4(5) . . . . ? C9A Fe2 C6A C12A 179.3(3) . . . . ? C7A Fe2 C6A C12A -114.7(3) . . . . ? C11A Fe2 C6A C12A 113.5(3) . . . . ? C10A Fe2 C6A C12A 141.2(3) . . . . ? C8A Fe2 C6A C12A -142.9(3) . . . . ? C11 C6 C7 C8 0.8(3) . . . . ? C12 C6 C7 C8 -176.6(2) . . . . ? Fe1 C6 C7 C8 52.20(19) . . . . ? C11 C6 C7 Fe1 -51.41(18) . . . . ? C12 C6 C7 Fe1 131.2(2) . . . . ? C5 Fe1 C7 C8 165.70(16) . . . . ? C3 Fe1 C7 C8 58.9(2) . . . . ? C2 Fe1 C7 C8 91.43(16) . . . . ? C1 Fe1 C7 C8 133.20(15) . . . . ? C4 Fe1 C7 C8 113.7(10) . . . . ? C9 Fe1 C7 C8 -29.74(13) . . . . ? C11 Fe1 C7 C8 -105.47(15) . . . . ? C10 Fe1 C7 C8 -67.59(14) . . . . ? C6 Fe1 C7 C8 -135.0(2) . . . . ? C5 Fe1 C7 C6 -59.3(2) . . . . ? C3 Fe1 C7 C6 -166.12(16) . . . . ? C2 Fe1 C7 C6 -133.59(15) . . . . ? C1 Fe1 C7 C6 -91.82(15) . . . . ? C4 Fe1 C7 C6 -111.3(10) . . . . ? C9 Fe1 C7 C6 105.24(15) . . . . ? C11 Fe1 C7 C6 29.51(13) . . . . ? C10 Fe1 C7 C6 67.39(14) . . . . ? C8 Fe1 C7 C6 135.0(2) . . . . ? C11A C6A C7A C8A 0.9(3) . . . . ? C12A C6A C7A C8A -175.9(2) . . . . ? Fe2 C6A C7A C8A 53.1(2) . . . . ? C11A C6A C7A Fe2 -52.21(19) . . . . ? C12A C6A C7A Fe2 131.0(2) . . . . ? C1A Fe2 C7A C6A -86.22(19) . . . . ? C2A Fe2 C7A C6A -127.78(18) . . . . ? C4A Fe2 C7A C6A -149.8(6) . . . . ? C5A Fe2 C7A C6A -57.2(3) . . . . ? C3A Fe2 C7A C6A -161.68(17) . . . . ? C9A Fe2 C7A C6A 105.68(15) . . . . ? C11A Fe2 C7A C6A 29.99(13) . . . . ? C10A Fe2 C7A C6A 67.81(14) . . . . ? C8A Fe2 C7A C6A 134.8(2) . . . . ? C1A Fe2 C7A C8A 138.96(19) . . . . ? C2A Fe2 C7A C8A 97.40(19) . . . . ? C4A Fe2 C7A C8A 75.4(7) . . . . ? C5A Fe2 C7A C8A 167.9(2) . . . . ? C3A Fe2 C7A C8A 63.5(2) . . . . ? C9A Fe2 C7A C8A -29.13(14) . . . . ? C11A Fe2 C7A C8A -104.82(16) . . . . ? C6A Fe2 C7A C8A -134.8(2) . . . . ? C10A Fe2 C7A C8A -67.01(15) . . . . ? C6 C7 C8 C9 -1.0(3) . . . . ? Fe1 C7 C8 C9 51.18(18) . . . . ? C6 C7 C8 C16 177.3(2) . . . . ? Fe1 C7 C8 C16 -130.5(2) . . . . ? C6 C7 C8 Fe1 -52.16(19) . . . . ? C5 Fe1 C8 C7 -70.5(6) . . . . ? C3 Fe1 C8 C7 -141.34(15) . . . . ? C2 Fe1 C8 C7 -99.93(16) . . . . ? C1 Fe1 C8 C7 -65.06(18) . . . . ? C4 Fe1 C8 C7 -170.40(18) . . . . ? C9 Fe1 C8 C7 132.36(19) . . . . ? C11 Fe1 C8 C7 66.13(14) . . . . ? C10 Fe1 C8 C7 104.30(14) . . . . ? C6 Fe1 C8 C7 28.23(13) . . . . ? C5 Fe1 C8 C9 157.1(5) . . . . ? C3 Fe1 C8 C9 86.30(16) . . . . ? C2 Fe1 C8 C9 127.71(15) . . . . ? C1 Fe1 C8 C9 162.58(15) . . . . ? C4 Fe1 C8 C9 57.2(2) . . . . ? C11 Fe1 C8 C9 -66.23(14) . . . . ? C7 Fe1 C8 C9 -132.36(19) . . . . ? C10 Fe1 C8 C9 -28.06(13) . . . . ? C6 Fe1 C8 C9 -104.13(14) . . . . ? C5 Fe1 C8 C16 44.9(7) . . . . ? C3 Fe1 C8 C16 -25.9(3) . . . . ? C2 Fe1 C8 C16 15.5(3) . . . . ? C1 Fe1 C8 C16 50.4(3) . . . . ? C4 Fe1 C8 C16 -55.0(3) . . . . ? C9 Fe1 C8 C16 -112.2(3) . . . . ? C11 Fe1 C8 C16 -178.4(2) . . . . ? C7 Fe1 C8 C16 115.4(3) . . . . ? C10 Fe1 C8 C16 -140.3(2) . . . . ? C6 Fe1 C8 C16 143.6(2) . . . . ? C6A C7A C8A C9A -3.1(3) . . . . ? Fe2 C7A C8A C9A 49.71(19) . . . . ? C6A C7A C8A C16A 174.9(2) . . . . ? Fe2 C7A C8A C16A -132.3(2) . . . . ? C6A C7A C8A Fe2 -52.8(2) . . . . ? C1A Fe2 C8A C7A -60.7(2) . . . . ? C2A Fe2 C8A C7A -93.15(18) . . . . ? C4A Fe2 C8A C7A -165.2(2) . . . . ? C5A Fe2 C8A C7A -98.3(10) . . . . ? C3A Fe2 C8A C7A -134.69(17) . . . . ? C9A Fe2 C8A C7A 133.3(2) . . . . ? C11A Fe2 C8A C7A 66.42(15) . . . . ? C6A Fe2 C8A C7A 28.28(14) . . . . ? C10A Fe2 C8A C7A 104.80(16) . . . . ? C1A Fe2 C8A C9A 165.99(19) . . . . ? C2A Fe2 C8A C9A 133.53(17) . . . . ? C4A Fe2 C8A C9A 61.5(2) . . . . ? C5A Fe2 C8A C9A 128.3(10) . . . . ? C3A Fe2 C8A C9A 91.99(18) . . . . ? C7A Fe2 C8A C9A -133.3(2) . . . . ? C11A Fe2 C8A C9A -66.90(15) . . . . ? C6A Fe2 C8A C9A -105.04(15) . . . . ? C10A Fe2 C8A C9A -28.51(14) . . . . ? C1A Fe2 C8A C16A 54.5(3) . . . . ? C2A Fe2 C8A C16A 22.1(3) . . . . ? C4A Fe2 C8A C16A -50.0(3) . . . . ? C5A Fe2 C8A C16A 16.9(11) . . . . ? C3A Fe2 C8A C16A -19.5(3) . . . . ? C9A Fe2 C8A C16A -111.4(3) . . . . ? C7A Fe2 C8A C16A 115.2(3) . . . . ? C11A Fe2 C8A C16A -178.3(3) . . . . ? C6A Fe2 C8A C16A 143.5(3) . . . . ? C10A Fe2 C8A C16A -140.0(3) . . . . ? C7 C8 C9 C10 1.1(3) . . . . ? C16 C8 C9 C10 -177.3(2) . . . . ? Fe1 C8 C9 C10 52.51(19) . . . . ? C7 C8 C9 Fe1 -51.45(18) . . . . ? C16 C8 C9 Fe1 130.20(19) . . . . ? C5 Fe1 C9 C8 -171.92(19) . . . . ? C3 Fe1 C9 C8 -105.65(15) . . . . ? C2 Fe1 C9 C8 -68.34(17) . . . . ? C1 Fe1 C9 C8 -54.7(4) . . . . ? C4 Fe1 C9 C8 -146.28(15) . . . . ? C11 Fe1 C9 C8 105.33(14) . . . . ? C7 Fe1 C9 C8 29.62(13) . . . . ? C10 Fe1 C9 C8 135.21(19) . . . . ? C6 Fe1 C9 C8 67.57(13) . . . . ? C5 Fe1 C9 C10 52.9(2) . . . . ? C3 Fe1 C9 C10 119.14(15) . . . . ? C2 Fe1 C9 C10 156.45(15) . . . . ? C1 Fe1 C9 C10 170.1(3) . . . . ? C4 Fe1 C9 C10 78.51(16) . . . . ? C11 Fe1 C9 C10 -29.88(13) . . . . ? C7 Fe1 C9 C10 -105.59(14) . . . . ? C8 Fe1 C9 C10 -135.21(19) . . . . ? C6 Fe1 C9 C10 -67.64(14) . . . . ? C7A C8A C9A C10A 3.5(3) . . . . ? C16A C8A C9A C10A -174.5(2) . . . . ? Fe2 C8A C9A C10A 53.4(2) . . . . ? C7A C8A C9A Fe2 -49.83(19) . . . . ? C16A C8A C9A Fe2 132.2(2) . . . . ? C1A Fe2 C9A C10A 163.5(7) . . . . ? C2A Fe2 C9A C10A 162.01(17) . . . . ? C4A Fe2 C9A C10A 85.37(18) . . . . ? C5A Fe2 C9A C10A 56.0(3) . . . . ? C3A Fe2 C9A C10A 126.22(17) . . . . ? C7A Fe2 C9A C10A -105.36(15) . . . . ? C11A Fe2 C9A C10A -30.04(14) . . . . ? C6A Fe2 C9A C10A -67.62(14) . . . . ? C8A Fe2 C9A C10A -134.4(2) . . . . ? C1A Fe2 C9A C8A -62.1(7) . . . . ? C2A Fe2 C9A C8A -63.5(2) . . . . ? C4A Fe2 C9A C8A -140.19(17) . . . . ? C5A Fe2 C9A C8A -169.6(2) . . . . ? C3A Fe2 C9A C8A -99.34(17) . . . . ? C7A Fe2 C9A C8A 29.08(14) . . . . ? C11A Fe2 C9A C8A 104.40(15) . . . . ? C6A Fe2 C9A C8A 66.82(14) . . . . ? C10A Fe2 C9A C8A 134.4(2) . . . . ? C8 C9 C10 C11 -0.9(3) . . . . ? Fe1 C9 C10 C11 51.63(18) . . . . ? C8 C9 C10 C20 175.4(2) . . . . ? Fe1 C9 C10 C20 -132.1(2) . . . . ? C8 C9 C10 Fe1 -52.57(19) . . . . ? C5 Fe1 C10 C9 -153.02(15) . . . . ? C3 Fe1 C10 C9 -75.25(17) . . . . ? C2 Fe1 C10 C9 -55.4(3) . . . . ? C1 Fe1 C10 C9 -173.0(2) . . . . ? C4 Fe1 C10 C9 -114.20(15) . . . . ? C11 Fe1 C10 C9 132.1(2) . . . . ? C7 Fe1 C10 C9 65.95(14) . . . . ? C8 Fe1 C10 C9 28.04(13) . . . . ? C6 Fe1 C10 C9 104.06(14) . . . . ? C5 Fe1 C10 C11 74.90(17) . . . . ? C3 Fe1 C10 C11 152.66(16) . . . . ? C2 Fe1 C10 C11 172.5(2) . . . . ? C1 Fe1 C10 C11 55.0(3) . . . . ? C4 Fe1 C10 C11 113.72(16) . . . . ? C9 Fe1 C10 C11 -132.1(2) . . . . ? C7 Fe1 C10 C11 -66.14(14) . . . . ? C8 Fe1 C10 C11 -104.05(15) . . . . ? C6 Fe1 C10 C11 -28.02(14) . . . . ? C5 Fe1 C10 C20 -39.0(3) . . . . ? C3 Fe1 C10 C20 38.8(3) . . . . ? C2 Fe1 C10 C20 58.6(4) . . . . ? C1 Fe1 C10 C20 -58.9(4) . . . . ? C4 Fe1 C10 C20 -0.1(3) . . . . ? C9 Fe1 C10 C20 114.1(3) . . . . ? C11 Fe1 C10 C20 -113.9(3) . . . . ? C7 Fe1 C10 C20 180.0(2) . . . . ? C8 Fe1 C10 C20 142.1(3) . . . . ? C6 Fe1 C10 C20 -141.9(3) . . . . ? C8A C9A C10A C11A -1.8(3) . . . . ? Fe2 C9A C10A C11A 51.88(19) . . . . ? C8A C9A C10A C20A 174.8(2) . . . . ? Fe2 C9A C10A C20A -131.4(2) . . . . ? C8A C9A C10A Fe2 -53.7(2) . . . . ? C1A Fe2 C10A C9A -173.4(2) . . . . ? C2A Fe2 C10A C9A -53.4(5) . . . . ? C4A Fe2 C10A C9A -107.28(17) . . . . ? C5A Fe2 C10A C9A -148.26(17) . . . . ? C3A Fe2 C10A C9A -69.81(19) . . . . ? C7A Fe2 C10A C9A 66.26(15) . . . . ? C11A Fe2 C10A C9A 131.9(2) . . . . ? C6A Fe2 C10A C9A 104.34(15) . . . . ? C8A Fe2 C10A C9A 28.44(14) . . . . ? C1A Fe2 C10A C11A 54.8(3) . . . . ? C2A Fe2 C10A C11A 174.7(4) . . . . ? C4A Fe2 C10A C11A 120.87(17) . . . . ? C5A Fe2 C10A C11A 79.89(18) . . . . ? C3A Fe2 C10A C11A 158.33(17) . . . . ? C9A Fe2 C10A C11A -131.9(2) . . . . ? C7A Fe2 C10A C11A -65.59(15) . . . . ? C6A Fe2 C10A C11A -27.51(14) . . . . ? C8A Fe2 C10A C11A -103.41(15) . . . . ? C1A Fe2 C10A C20A -57.7(4) . . . . ? C2A Fe2 C10A C20A 62.2(5) . . . . ? C4A Fe2 C10A C20A 8.3(3) . . . . ? C5A Fe2 C10A C20A -32.6(3) . . . . ? C3A Fe2 C10A C20A 45.8(3) . . . . ? C9A Fe2 C10A C20A 115.6(3) . . . . ? C7A Fe2 C10A C20A -178.1(3) . . . . ? C11A Fe2 C10A C20A -112.5(3) . . . . ? C6A Fe2 C10A C20A -140.0(3) . . . . ? C8A Fe2 C10A C20A 144.1(3) . . . . ? C7 C6 C11 C10 -0.7(3) . . . . ? C12 C6 C11 C10 176.7(2) . . . . ? Fe1 C6 C11 C10 -52.0(2) . . . . ? C7 C6 C11 Fe1 51.39(18) . . . . ? C12 C6 C11 Fe1 -131.2(2) . . . . ? C9 C10 C11 C6 0.7(3) . . . . ? C20 C10 C11 C6 -175.6(2) . . . . ? Fe1 C10 C11 C6 52.2(2) . . . . ? C9 C10 C11 Fe1 -51.43(18) . . . . ? C20 C10 C11 Fe1 132.3(2) . . . . ? C5 Fe1 C11 C6 105.37(15) . . . . ? C3 Fe1 C11 C6 171.8(2) . . . . ? C2 Fe1 C11 C6 55.7(4) . . . . ? C1 Fe1 C11 C6 68.09(17) . . . . ? C4 Fe1 C11 C6 145.99(15) . . . . ? C9 Fe1 C11 C6 -105.21(15) . . . . ? C7 Fe1 C11 C6 -29.66(13) . . . . ? C10 Fe1 C11 C6 -135.1(2) . . . . ? C8 Fe1 C11 C6 -67.33(14) . . . . ? C5 Fe1 C11 C10 -119.54(15) . . . . ? C3 Fe1 C11 C10 -53.1(3) . . . . ? C2 Fe1 C11 C10 -169.2(4) . . . . ? C1 Fe1 C11 C10 -156.82(15) . . . . ? C4 Fe1 C11 C10 -78.91(17) . . . . ? C9 Fe1 C11 C10 29.89(14) . . . . ? C7 Fe1 C11 C10 105.43(15) . . . . ? C8 Fe1 C11 C10 67.76(14) . . . . ? C6 Fe1 C11 C10 135.1(2) . . . . ? C7A C6A C11A C10A 0.9(3) . . . . ? C12A C6A C11A C10A 177.8(2) . . . . ? Fe2 C6A C11A C10A -51.1(2) . . . . ? C7A C6A C11A Fe2 52.04(19) . . . . ? C12A C6A C11A Fe2 -131.1(2) . . . . ? C9A C10A C11A C6A -0.5(4) . . . . ? C20A C10A C11A C6A -177.2(2) . . . . ? Fe2 C10A C11A C6A 51.2(2) . . . . ? C9A C10A C11A Fe2 -51.63(19) . . . . ? C20A C10A C11A Fe2 131.6(2) . . . . ? C1A Fe2 C11A C6A 71.0(2) . . . . ? C2A Fe2 C11A C6A 48.2(4) . . . . ? C4A Fe2 C11A C6A 149.89(16) . . . . ? C5A Fe2 C11A C6A 110.02(18) . . . . ? C3A Fe2 C11A C6A 172.9(3) . . . . ? C9A Fe2 C11A C6A -105.97(15) . . . . ? C7A Fe2 C11A C6A -30.07(13) . . . . ? C10A Fe2 C11A C6A -136.0(2) . . . . ? C8A Fe2 C11A C6A -67.94(14) . . . . ? C1A Fe2 C11A C10A -153.02(19) . . . . ? C2A Fe2 C11A C10A -175.8(3) . . . . ? C4A Fe2 C11A C10A -74.14(18) . . . . ? C5A Fe2 C11A C10A -114.01(18) . . . . ? C3A Fe2 C11A C10A -51.2(3) . . . . ? C9A Fe2 C11A C10A 30.00(14) . . . . ? C7A Fe2 C11A C10A 105.91(15) . . . . ? C6A Fe2 C11A C10A 136.0(2) . . . . ? C8A Fe2 C11A C10A 68.03(14) . . . . ? C11 C6 C12 C14 166.8(2) . . . . ? C7 C6 C12 C14 -15.9(3) . . . . ? Fe1 C6 C12 C14 76.3(3) . . . . ? C11 C6 C12 C13 44.1(3) . . . . ? C7 C6 C12 C13 -138.6(2) . . . . ? Fe1 C6 C12 C13 -46.4(3) . . . . ? C11 C6 C12 C15 -74.5(3) . . . . ? C7 C6 C12 C15 102.7(2) . . . . ? Fe1 C6 C12 C15 -165.09(19) . . . . ? C11A C6A C12A C13A 38.7(3) . . . . ? C7A C6A C12A C13A -144.6(2) . . . . ? Fe2 C6A C12A C13A -52.7(3) . . . . ? C11A C6A C12A C14A 162.1(3) . . . . ? C7A C6A C12A C14A -21.2(3) . . . . ? Fe2 C6A C12A C14A 70.7(3) . . . . ? C11A C6A C12A C15A -78.5(3) . . . . ? C7A C6A C12A C15A 98.2(3) . . . . ? Fe2 C6A C12A C15A -169.9(2) . . . . ? C7 C8 C16 C17 17.6(3) . . . . ? C9 C8 C16 C17 -164.1(2) . . . . ? Fe1 C8 C16 C17 -74.6(3) . . . . ? C7 C8 C16 C19 140.2(2) . . . . ? C9 C8 C16 C19 -41.5(3) . . . . ? Fe1 C8 C16 C19 48.0(3) . . . . ? C7 C8 C16 C18 -100.4(3) . . . . ? C9 C8 C16 C18 77.8(3) . . . . ? Fe1 C8 C16 C18 167.32(19) . . . . ? C7A C8A C16A C17A 2.7(3) . . . . ? C9A C8A C16A C17A -179.4(2) . . . . ? Fe2 C8A C16A C17A -89.9(3) . . . . ? C7A C8A C16A C18A 124.6(2) . . . . ? C9A C8A C16A C18A -57.5(3) . . . . ? Fe2 C8A C16A C18A 32.1(3) . . . . ? C7A C8A C16A C19A -116.0(2) . . . . ? C9A C8A C16A C19A 61.9(3) . . . . ? Fe2 C8A C16A C19A 151.5(2) . . . . ? C9 C10 C20 C23 152.1(2) . . . . ? C11 C10 C20 C23 -31.7(3) . . . . ? Fe1 C10 C20 C23 60.3(3) . . . . ? C9 C10 C20 C21 29.7(3) . . . . ? C11 C10 C20 C21 -154.2(2) . . . . ? Fe1 C10 C20 C21 -62.1(3) . . . . ? C9 C10 C20 C22 -89.0(3) . . . . ? C11 C10 C20 C22 87.2(3) . . . . ? Fe1 C10 C20 C22 179.2(2) . . . . ? C9A C10A C20A C21A 14.6(3) . . . . ? C11A C10A C20A C21A -168.8(2) . . . . ? Fe2 C10A C20A C21A -78.0(3) . . . . ? C9A C10A C20A C23A 136.7(3) . . . . ? C11A C10A C20A C23A -46.7(3) . . . . ? Fe2 C10A C20A C23A 44.1(4) . . . . ? C9A C10A C20A C22A -104.5(3) . . . . ? C11A C10A C20A C22A 72.1(3) . . . . ? Fe2 C10A C20A C22A 162.9(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A F1 H1F F2 1.03(5) 1.30(5) 2.300(3) 164(4) . F2 H2F F3 1.15(4) 1.21(4) 2.339(3) 166(4) . F4 H4F F5 1.18(5) 1.22(4) 2.267(6) 141(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.587 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.065 data_rde137 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 Cr, C20 H30 Cr2 F5' _chemical_formula_sum 'C40 H60 Cr3 F5' _chemical_formula_weight 791.88 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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cr' 'Cr' 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P21212 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 12.8139(2) _cell_length_b 17.8524(4) _cell_length_c 8.6190(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1971.67(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 23676 _cell_measurement_theta_min 1.018 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 834 _exptl_absorpt_coefficient_mu 0.862 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7821 _exptl_absorpt_correction_T_max 0.8134 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _diffrn_ambient_temperature 150(1) _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 'Nonius KappaCCD Diffractometer' _diffrn_measurement_method 'Phi and Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4514 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0352 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4514 _reflns_number_gt 4107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'WinGX, Ortep3' _computing_publication_material ? _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^)+(0.0394P)^2^+0.9018P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 4514 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0.001 _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 Cr1 Cr 0.40480(3) 0.08513(2) 0.74083(4) 0.02265(10) Uani 1 1 d . . . Cr2 Cr 0.5000 0.5000 0.70912(6) 0.01966(12) Uani 1 2 d S . . F1 F 0.5000 0.0000 0.7704(3) 0.0379(5) Uani 1 2 d S . . F2 F 0.30407(15) 0.05268(10) 0.8826(2) 0.0488(5) Uani 1 1 d . . . F3 F 0.33914(14) 0.04442(10) 0.5673(2) 0.0437(4) Uani 1 1 d . . . C1 C 0.54095(19) 0.15971(14) 0.7970(3) 0.0246(5) Uani 1 1 d . . . C2 C 0.4523(2) 0.18475(15) 0.8807(3) 0.0282(6) Uani 1 1 d . . . C3 C 0.37465(18) 0.20704(12) 0.7711(3) 0.0231(5) Uani 1 1 d . . . C4 C 0.4163(2) 0.19618(13) 0.6193(3) 0.0216(5) Uani 1 1 d . . . C5 C 0.51790(18) 0.16516(13) 0.6349(3) 0.0225(5) Uani 1 1 d . . . C6 C 0.6418(2) 0.13087(17) 0.8628(4) 0.0390(7) Uani 1 1 d . . . H6A H 0.6974 0.1674 0.8437 0.058 Uiso 1 1 calc R . . H6B H 0.6598 0.0833 0.8129 0.058 Uiso 1 1 calc R . . H6C H 0.6341 0.1231 0.9748 0.058 Uiso 1 1 calc R . . C7 C 0.4406(3) 0.18562(19) 1.0541(3) 0.0442(8) Uani 1 1 d . . . H7A H 0.4902 0.1503 1.1004 0.066 Uiso 1 1 calc R . . H7B H 0.3693 0.1710 1.0819 0.066 Uiso 1 1 calc R . . H7C H 0.4547 0.2362 1.0932 0.066 Uiso 1 1 calc R . . C8 C 0.2680(2) 0.23668(15) 0.8103(3) 0.0320(6) Uani 1 1 d . . . H8A H 0.2459 0.2168 0.9111 0.048 Uiso 1 1 calc R . . H8B H 0.2182 0.2211 0.7303 0.048 Uiso 1 1 calc R . . H8C H 0.2703 0.2915 0.8152 0.048 Uiso 1 1 calc R . . C9 C 0.3623(2) 0.21121(16) 0.4690(3) 0.0297(6) Uani 1 1 d . . . H9A H 0.4068 0.2428 0.4036 0.045 Uiso 1 1 calc R . . H9B H 0.2961 0.2370 0.4889 0.045 Uiso 1 1 calc R . . H9C H 0.3486 0.1637 0.4158 0.045 Uiso 1 1 calc R . . C10 C 0.5878(2) 0.14019(16) 0.5047(3) 0.0326(6) Uani 1 1 d . . . H10A H 0.5506 0.1449 0.4059 0.049 Uiso 1 1 calc R . . H10B H 0.6080 0.0878 0.5209 0.049 Uiso 1 1 calc R . . H10C H 0.6505 0.1716 0.5025 0.049 Uiso 1 1 calc R . . C11 C 0.52207(18) 0.38180(13) 0.7725(3) 0.0290(6) Uani 1 1 d . . . C12 C 0.43092(19) 0.40934(15) 0.8477(3) 0.0271(5) Uani 1 1 d . . . C13 C 0.35762(17) 0.43172(12) 0.7304(3) 0.0217(5) Uani 1 1 d . . . C14 C 0.40543(18) 0.41737(14) 0.5829(3) 0.0219(5) Uani 1 1 d . . . C15 C 0.5066(2) 0.38675(13) 0.6099(3) 0.0259(5) Uani 1 1 d . . . C16 C 0.6185(2) 0.35265(16) 0.8524(4) 0.0432(8) Uani 1 1 d . . . H16A H 0.6066 0.3009 0.8862 0.065 Uiso 1 1 calc R . . H16B H 0.6341 0.3840 0.9428 0.065 Uiso 1 1 calc R . . H16C H 0.6775 0.3540 0.7801 0.065 Uiso 1 1 calc R . . C17 C 0.4127(2) 0.41457(19) 1.0202(3) 0.0388(7) Uani 1 1 d . . . H17A H 0.3827 0.3674 1.0578 0.058 Uiso 1 1 calc R . . H17B H 0.3643 0.4557 1.0420 0.058 Uiso 1 1 calc R . . H17C H 0.4792 0.4239 1.0730 0.058 Uiso 1 1 calc R . . C18 C 0.25109(17) 0.46357(15) 0.7582(3) 0.0285(5) Uani 1 1 d . . . H18A H 0.2008 0.4226 0.7706 0.043 Uiso 1 1 calc R . . H18B H 0.2307 0.4947 0.6695 0.043 Uiso 1 1 calc R . . H18C H 0.2520 0.4942 0.8525 0.043 Uiso 1 1 calc R . . C19 C 0.3592(2) 0.43297(16) 0.4263(3) 0.0298(6) Uani 1 1 d . . . H19A H 0.4124 0.4555 0.3592 0.045 Uiso 1 1 calc R . . H19B H 0.3003 0.4676 0.4374 0.045 Uiso 1 1 calc R . . H19C H 0.3348 0.3860 0.3800 0.045 Uiso 1 1 calc R . . C20 C 0.5829(2) 0.36337(17) 0.4865(4) 0.0383(7) Uani 1 1 d . . . H20A H 0.6498 0.3886 0.5038 0.057 Uiso 1 1 calc R . . H20B H 0.5555 0.3772 0.3843 0.057 Uiso 1 1 calc R . . H20C H 0.5931 0.3090 0.4910 0.057 Uiso 1 1 calc 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 Cr1 0.02557(18) 0.01515(17) 0.0272(2) 0.00003(16) 0.00228(16) -0.00024(15) Cr2 0.0201(2) 0.0168(2) 0.0222(3) 0.000 0.000 -0.0020(2) F1 0.0331(10) 0.0192(9) 0.0616(15) 0.000 0.000 0.0045(9) F2 0.0545(11) 0.0287(9) 0.0631(12) 0.0060(8) 0.0328(10) -0.0007(8) F3 0.0500(10) 0.0308(9) 0.0504(11) -0.0058(8) -0.0158(8) -0.0112(8) C1 0.0256(11) 0.0190(11) 0.0290(13) -0.0013(10) -0.0044(10) 0.0002(9) C2 0.0390(15) 0.0202(13) 0.0253(13) -0.0038(11) -0.0015(11) -0.0003(11) C3 0.0270(11) 0.0134(10) 0.0288(13) -0.0017(10) 0.0047(10) 0.0007(9) C4 0.0232(12) 0.0155(11) 0.0262(12) 0.0016(9) -0.0003(10) -0.0023(10) C5 0.0229(13) 0.0177(11) 0.0269(12) 0.0012(10) 0.0027(9) -0.0028(10) C6 0.0369(15) 0.0343(16) 0.0458(17) -0.0007(14) -0.0149(14) 0.0049(13) C7 0.065(2) 0.0438(18) 0.0238(14) -0.0034(13) -0.0016(13) 0.0043(15) C8 0.0313(13) 0.0252(13) 0.0395(15) -0.0025(12) 0.0094(12) 0.0028(11) C9 0.0288(12) 0.0317(14) 0.0287(13) 0.0051(11) -0.0038(11) 0.0007(12) C10 0.0278(12) 0.0308(14) 0.0392(14) 0.0023(12) 0.0086(12) 0.0033(12) C11 0.0281(12) 0.0149(10) 0.0439(15) 0.0061(11) -0.0099(12) -0.0042(9) C12 0.0292(12) 0.0241(13) 0.0279(12) 0.0068(11) -0.0040(10) -0.0077(11) C13 0.0217(10) 0.0190(10) 0.0244(12) 0.0008(10) 0.0000(10) -0.0067(9) C14 0.0216(11) 0.0179(11) 0.0262(11) -0.0016(10) -0.0006(9) -0.0022(11) C15 0.0236(11) 0.0185(11) 0.0357(13) -0.0044(10) -0.0030(12) -0.0027(10) C16 0.0381(16) 0.0263(15) 0.065(2) 0.0101(14) -0.0207(15) 0.0022(12) C17 0.0398(15) 0.0500(18) 0.0266(12) 0.0116(13) -0.0024(12) -0.0142(16) C18 0.0223(10) 0.0346(13) 0.0286(12) -0.0033(12) 0.0014(10) -0.0033(10) C19 0.0278(12) 0.0363(16) 0.0253(13) -0.0056(11) -0.0009(10) -0.0011(12) C20 0.0263(13) 0.0347(15) 0.0541(18) -0.0153(14) 0.0043(13) 0.0029(13) _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 Cr1 F3 1.8638(17) . ? Cr1 F2 1.8696(17) . ? Cr1 F1 1.9655(5) . ? Cr1 C3 2.226(2) . ? Cr1 C5 2.230(2) . ? Cr1 C2 2.233(3) . ? Cr1 C4 2.247(2) . ? Cr1 C1 2.247(2) . ? Cr2 C15 2.197(2) 2_665 ? Cr2 C15 2.197(2) . ? Cr2 C14 2.197(2) 2_665 ? Cr2 C14 2.197(2) . ? Cr2 C12 2.198(3) 2_665 ? Cr2 C12 2.198(3) . ? Cr2 C11 2.198(2) 2_665 ? Cr2 C11 2.198(2) . ? Cr2 C13 2.202(2) . ? Cr2 C13 2.202(2) 2_665 ? F1 Cr1 1.9655(5) 2_655 ? C1 C2 1.417(4) . ? C1 C5 1.431(4) . ? C1 C6 1.502(4) . ? C2 C3 1.429(4) . ? C2 C7 1.502(4) . ? C3 C4 1.427(3) . ? C3 C8 1.504(3) . ? C4 C5 1.421(3) . ? C4 C9 1.493(3) . ? C5 C10 1.504(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C15 1.418(4) . ? C11 C12 1.423(4) . ? C11 C16 1.507(3) . ? C12 C13 1.437(3) . ? C12 C17 1.508(4) . ? C13 C14 1.435(3) . ? C13 C18 1.498(3) . ? C14 C15 1.426(4) . ? C14 C19 1.500(3) . ? C15 C20 1.503(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 F3 Cr1 F2 95.29(9) . . ? F3 Cr1 F1 94.74(8) . . ? F2 Cr1 F1 95.98(8) . . ? F3 Cr1 C3 113.40(9) . . ? F2 Cr1 C3 96.11(8) . . ? F1 Cr1 C3 148.06(7) . . ? F3 Cr1 C5 102.39(9) . . ? F2 Cr1 C5 156.15(9) . . ? F1 Cr1 C5 98.34(7) . . ? C3 Cr1 C5 62.25(9) . . ? F3 Cr1 C2 150.11(9) . . ? F2 Cr1 C2 94.71(10) . . ? F1 Cr1 C2 112.12(9) . . ? C3 Cr1 C2 37.38(10) . . ? C5 Cr1 C2 62.20(9) . . ? F3 Cr1 C4 89.97(8) . . ? F2 Cr1 C4 128.58(8) . . ? F1 Cr1 C4 134.58(8) . . ? C3 Cr1 C4 37.20(9) . . ? C5 Cr1 C4 37.00(9) . . ? C2 Cr1 C4 62.05(9) . . ? F3 Cr1 C1 138.97(9) . . ? F2 Cr1 C1 125.35(10) . . ? F1 Cr1 C1 87.04(7) . . ? C3 Cr1 C1 61.98(9) . . ? C5 Cr1 C1 37.28(9) . . ? C2 Cr1 C1 36.88(10) . . ? C4 Cr1 C1 61.76(9) . . ? C15 Cr2 C15 134.17(13) 2_665 . ? C15 Cr2 C14 37.88(9) 2_665 2_665 ? C15 Cr2 C14 113.81(9) . 2_665 ? C15 Cr2 C14 113.81(9) 2_665 . ? C15 Cr2 C14 37.88(9) . . ? C14 Cr2 C14 120.64(12) 2_665 . ? C15 Cr2 C12 63.22(10) 2_665 2_665 ? C15 Cr2 C12 150.90(10) . 2_665 ? C14 Cr2 C12 63.42(9) 2_665 2_665 ? C14 Cr2 C12 170.28(9) . 2_665 ? C15 Cr2 C12 150.91(10) 2_665 . ? C15 Cr2 C12 63.22(10) . . ? C14 Cr2 C12 170.28(9) 2_665 . ? C14 Cr2 C12 63.42(9) . . ? C12 Cr2 C12 114.16(14) 2_665 . ? C15 Cr2 C11 37.66(10) 2_665 2_665 ? C15 Cr2 C11 170.14(10) . 2_665 ? C14 Cr2 C11 63.23(9) 2_665 2_665 ? C14 Cr2 C11 134.16(9) . 2_665 ? C12 Cr2 C11 37.79(10) 2_665 2_665 ? C12 Cr2 C11 121.34(11) . 2_665 ? C15 Cr2 C11 170.14(11) 2_665 . ? C15 Cr2 C11 37.66(10) . . ? C14 Cr2 C11 134.15(9) 2_665 . ? C14 Cr2 C11 63.23(9) . . ? C12 Cr2 C11 121.34(11) 2_665 . ? C12 Cr2 C11 37.79(10) . . ? C11 Cr2 C11 151.22(16) 2_665 . ? C15 Cr2 C13 120.66(9) 2_665 . ? C15 Cr2 C13 63.58(9) . . ? C14 Cr2 C13 150.45(9) 2_665 . ? C14 Cr2 C13 38.07(9) . . ? C12 Cr2 C13 134.11(9) 2_665 . ? C12 Cr2 C13 38.12(9) . . ? C11 Cr2 C13 113.84(9) 2_665 . ? C11 Cr2 C13 63.54(9) . . ? C15 Cr2 C13 63.58(9) 2_665 2_665 ? C15 Cr2 C13 120.66(9) . 2_665 ? C14 Cr2 C13 38.07(9) 2_665 2_665 ? C14 Cr2 C13 150.45(9) . 2_665 ? C12 Cr2 C13 38.11(9) 2_665 2_665 ? C12 Cr2 C13 134.11(9) . 2_665 ? C11 Cr2 C13 63.54(9) 2_665 2_665 ? C11 Cr2 C13 113.83(9) . 2_665 ? C13 Cr2 C13 170.43(13) . 2_665 ? Cr1 F1 Cr1 165.10(15) . 2_655 ? C2 C1 C5 108.1(2) . . ? C2 C1 C6 127.2(2) . . ? C5 C1 C6 124.7(2) . . ? C2 C1 Cr1 71.02(14) . . ? C5 C1 Cr1 70.71(14) . . ? C6 C1 Cr1 123.10(18) . . ? C1 C2 C3 108.0(2) . . ? C1 C2 C7 126.1(3) . . ? C3 C2 C7 125.8(3) . . ? C1 C2 Cr1 72.10(14) . . ? C3 C2 Cr1 71.02(14) . . ? C7 C2 Cr1 121.2(2) . . ? C4 C3 C2 107.9(2) . . ? C4 C3 C8 126.4(2) . . ? C2 C3 C8 125.6(2) . . ? C4 C3 Cr1 72.22(13) . . ? C2 C3 Cr1 71.60(14) . . ? C8 C3 Cr1 121.87(16) . . ? C5 C4 C3 108.0(2) . . ? C5 C4 C9 125.2(2) . . ? C3 C4 C9 126.7(2) . . ? C5 C4 Cr1 70.86(13) . . ? C3 C4 Cr1 70.58(13) . . ? C9 C4 Cr1 122.19(17) . . ? C4 C5 C1 108.0(2) . . ? C4 C5 C10 126.2(2) . . ? C1 C5 C10 125.8(2) . . ? C4 C5 Cr1 72.14(13) . . ? C1 C5 Cr1 72.00(14) . . ? C10 C5 Cr1 120.18(17) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C15 C11 C12 108.3(2) . . ? C15 C11 C16 126.0(3) . . ? C12 C11 C16 125.7(3) . . ? C15 C11 Cr2 71.13(14) . . ? C12 C11 Cr2 71.09(14) . . ? C16 C11 Cr2 123.40(17) . . ? C11 C12 C13 108.2(2) . . ? C11 C12 C17 126.7(2) . . ? C13 C12 C17 125.1(2) . . ? C11 C12 Cr2 71.12(14) . . ? C13 C12 Cr2 71.10(13) . . ? C17 C12 Cr2 123.6(2) . . ? C14 C13 C12 107.1(2) . . ? C14 C13 C18 126.8(2) . . ? C12 C13 C18 126.1(2) . . ? C14 C13 Cr2 70.80(13) . . ? C12 C13 Cr2 70.79(13) . . ? C18 C13 Cr2 123.94(16) . . ? C15 C14 C13 108.2(2) . . ? C15 C14 C19 125.2(2) . . ? C13 C14 C19 126.6(2) . . ? C15 C14 Cr2 71.04(13) . . ? C13 C14 Cr2 71.14(13) . . ? C19 C14 Cr2 122.59(18) . . ? C11 C15 C14 108.2(2) . . ? C11 C15 C20 126.2(2) . . ? C14 C15 C20 125.6(2) . . ? C11 C15 Cr2 71.22(14) . . ? C14 C15 Cr2 71.08(14) . . ? C20 C15 Cr2 123.79(19) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag F3 Cr1 F1 Cr1 36.74(6) . . . 2_655 ? F2 Cr1 F1 Cr1 132.57(7) . . . 2_655 ? C3 Cr1 F1 Cr1 -115.68(17) . . . 2_655 ? C5 Cr1 F1 Cr1 -66.55(7) . . . 2_655 ? C2 Cr1 F1 Cr1 -129.85(8) . . . 2_655 ? C4 Cr1 F1 Cr1 -57.90(11) . . . 2_655 ? C1 Cr1 F1 Cr1 -102.18(7) . . . 2_655 ? F3 Cr1 C1 C2 131.99(16) . . . . ? F2 Cr1 C1 C2 -38.96(18) . . . . ? F1 Cr1 C1 C2 -134.19(17) . . . . ? C3 Cr1 C1 C2 37.76(15) . . . . ? C5 Cr1 C1 C2 117.9(2) . . . . ? C4 Cr1 C1 C2 80.17(16) . . . . ? F3 Cr1 C1 C5 14.1(2) . . . . ? F2 Cr1 C1 C5 -156.85(14) . . . . ? F1 Cr1 C1 C5 107.92(16) . . . . ? C3 Cr1 C1 C5 -80.12(16) . . . . ? C2 Cr1 C1 C5 -117.9(2) . . . . ? C4 Cr1 C1 C5 -37.71(14) . . . . ? F3 Cr1 C1 C6 -105.3(2) . . . . ? F2 Cr1 C1 C6 83.7(2) . . . . ? F1 Cr1 C1 C6 -11.5(2) . . . . ? C3 Cr1 C1 C6 160.4(3) . . . . ? C5 Cr1 C1 C6 -119.4(3) . . . . ? C2 Cr1 C1 C6 122.7(3) . . . . ? C4 Cr1 C1 C6 -157.2(3) . . . . ? C5 C1 C2 C3 -1.0(3) . . . . ? C6 C1 C2 C3 -180.0(2) . . . . ? Cr1 C1 C2 C3 -62.32(17) . . . . ? C5 C1 C2 C7 177.3(3) . . . . ? C6 C1 C2 C7 -1.6(5) . . . . ? Cr1 C1 C2 C7 116.0(3) . . . . ? C5 C1 C2 Cr1 61.34(19) . . . . ? C6 C1 C2 Cr1 -117.6(3) . . . . ? F3 Cr1 C2 C1 -101.8(2) . . . . ? F2 Cr1 C2 C1 149.03(15) . . . . ? F1 Cr1 C2 C1 50.62(17) . . . . ? C3 Cr1 C2 C1 -117.1(2) . . . . ? C5 Cr1 C2 C1 -37.25(15) . . . . ? C4 Cr1 C2 C1 -79.33(16) . . . . ? F3 Cr1 C2 C3 15.3(3) . . . . ? F2 Cr1 C2 C3 -93.91(15) . . . . ? F1 Cr1 C2 C3 167.68(13) . . . . ? C5 Cr1 C2 C3 79.82(15) . . . . ? C4 Cr1 C2 C3 37.74(14) . . . . ? C1 Cr1 C2 C3 117.1(2) . . . . ? F3 Cr1 C2 C7 136.3(2) . . . . ? F2 Cr1 C2 C7 27.1(3) . . . . ? F1 Cr1 C2 C7 -71.3(3) . . . . ? C3 Cr1 C2 C7 121.0(3) . . . . ? C5 Cr1 C2 C7 -159.2(3) . . . . ? C4 Cr1 C2 C7 158.8(3) . . . . ? C1 Cr1 C2 C7 -121.9(3) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? C7 C2 C3 C4 -178.8(3) . . . . ? Cr1 C2 C3 C4 -63.52(16) . . . . ? C1 C2 C3 C8 179.5(2) . . . . ? C7 C2 C3 C8 1.2(4) . . . . ? Cr1 C2 C3 C8 116.5(2) . . . . ? C1 C2 C3 Cr1 63.02(18) . . . . ? C7 C2 C3 Cr1 -115.3(3) . . . . ? F3 Cr1 C3 C4 -55.18(15) . . . . ? F2 Cr1 C3 C4 -153.65(14) . . . . ? F1 Cr1 C3 C4 94.6(2) . . . . ? C5 Cr1 C3 C4 36.92(14) . . . . ? C2 Cr1 C3 C4 116.6(2) . . . . ? C1 Cr1 C3 C4 79.32(15) . . . . ? F3 Cr1 C3 C2 -171.76(15) . . . . ? F2 Cr1 C3 C2 89.77(16) . . . . ? F1 Cr1 C3 C2 -21.9(2) . . . . ? C5 Cr1 C3 C2 -79.66(16) . . . . ? C4 Cr1 C3 C2 -116.6(2) . . . . ? C1 Cr1 C3 C2 -37.26(15) . . . . ? F3 Cr1 C3 C8 67.2(2) . . . . ? F2 Cr1 C3 C8 -31.3(2) . . . . ? F1 Cr1 C3 C8 -143.0(2) . . . . ? C5 Cr1 C3 C8 159.3(2) . . . . ? C2 Cr1 C3 C8 -121.1(3) . . . . ? C4 Cr1 C3 C8 122.3(3) . . . . ? C1 Cr1 C3 C8 -158.3(2) . . . . ? C2 C3 C4 C5 1.8(3) . . . . ? C8 C3 C4 C5 -178.2(2) . . . . ? Cr1 C3 C4 C5 -61.32(17) . . . . ? C2 C3 C4 C9 179.3(2) . . . . ? C8 C3 C4 C9 -0.7(4) . . . . ? Cr1 C3 C4 C9 116.2(3) . . . . ? C2 C3 C4 Cr1 63.12(17) . . . . ? C8 C3 C4 Cr1 -116.9(2) . . . . ? F3 Cr1 C4 C5 -110.94(15) . . . . ? F2 Cr1 C4 C5 152.32(15) . . . . ? F1 Cr1 C4 C5 -14.3(2) . . . . ? C3 Cr1 C4 C5 118.0(2) . . . . ? C2 Cr1 C4 C5 80.03(16) . . . . ? C1 Cr1 C4 C5 38.00(15) . . . . ? F3 Cr1 C4 C3 131.11(14) . . . . ? F2 Cr1 C4 C3 34.37(18) . . . . ? F1 Cr1 C4 C3 -132.25(15) . . . . ? C5 Cr1 C4 C3 -118.0(2) . . . . ? C2 Cr1 C4 C3 -37.92(14) . . . . ? C1 Cr1 C4 C3 -79.95(15) . . . . ? F3 Cr1 C4 C9 9.3(2) . . . . ? F2 Cr1 C4 C9 -87.5(2) . . . . ? F1 Cr1 C4 C9 105.9(2) . . . . ? C3 Cr1 C4 C9 -121.8(3) . . . . ? C5 Cr1 C4 C9 120.2(3) . . . . ? C2 Cr1 C4 C9 -159.8(2) . . . . ? C1 Cr1 C4 C9 158.2(2) . . . . ? C3 C4 C5 C1 -2.4(3) . . . . ? C9 C4 C5 C1 -180.0(2) . . . . ? Cr1 C4 C5 C1 -63.54(18) . . . . ? C3 C4 C5 C10 175.9(2) . . . . ? C9 C4 C5 C10 -1.7(4) . . . . ? Cr1 C4 C5 C10 114.8(2) . . . . ? C3 C4 C5 Cr1 61.14(17) . . . . ? C9 C4 C5 Cr1 -116.4(2) . . . . ? C2 C1 C5 C4 2.1(3) . . . . ? C6 C1 C5 C4 -178.9(2) . . . . ? Cr1 C1 C5 C4 63.62(17) . . . . ? C2 C1 C5 C10 -176.2(2) . . . . ? C6 C1 C5 C10 2.8(4) . . . . ? Cr1 C1 C5 C10 -114.7(3) . . . . ? C2 C1 C5 Cr1 -61.54(19) . . . . ? C6 C1 C5 Cr1 117.5(3) . . . . ? F3 Cr1 C5 C4 72.99(15) . . . . ? F2 Cr1 C5 C4 -63.9(3) . . . . ? F1 Cr1 C5 C4 169.75(15) . . . . ? C3 Cr1 C5 C4 -37.12(14) . . . . ? C2 Cr1 C5 C4 -79.58(15) . . . . ? C1 Cr1 C5 C4 -116.4(2) . . . . ? F3 Cr1 C5 C1 -170.58(14) . . . . ? F2 Cr1 C5 C1 52.5(3) . . . . ? F1 Cr1 C5 C1 -73.81(16) . . . . ? C3 Cr1 C5 C1 79.32(16) . . . . ? C2 Cr1 C5 C1 36.85(15) . . . . ? C4 Cr1 C5 C1 116.4(2) . . . . ? F3 Cr1 C5 C10 -49.0(2) . . . . ? F2 Cr1 C5 C10 174.0(2) . . . . ? F1 Cr1 C5 C10 47.7(2) . . . . ? C3 Cr1 C5 C10 -159.1(2) . . . . ? C2 Cr1 C5 C10 158.4(2) . . . . ? C4 Cr1 C5 C10 -122.0(3) . . . . ? C1 Cr1 C5 C10 121.5(3) . . . . ? C15 Cr2 C11 C15 -37.3(7) 2_665 . . . ? C14 Cr2 C11 C15 -70.3(2) 2_665 . . . ? C14 Cr2 C11 C15 37.51(15) . . . . ? C12 Cr2 C11 C15 -152.31(15) 2_665 . . . ? C12 Cr2 C11 C15 117.9(2) . . . . ? C11 Cr2 C11 C15 172.10(16) 2_665 . . . ? C13 Cr2 C11 C15 80.29(17) . . . . ? C13 Cr2 C11 C15 -109.88(16) 2_665 . . . ? C15 Cr2 C11 C12 -155.2(6) 2_665 . . . ? C15 Cr2 C11 C12 -117.9(2) . . . . ? C14 Cr2 C11 C12 171.82(14) 2_665 . . . ? C14 Cr2 C11 C12 -80.38(15) . . . . ? C12 Cr2 C11 C12 89.8(2) 2_665 . . . ? C11 Cr2 C11 C12 54.22(14) 2_665 . . . ? C13 Cr2 C11 C12 -37.59(14) . . . . ? C13 Cr2 C11 C12 132.24(15) 2_665 . . . ? C15 Cr2 C11 C16 83.9(7) 2_665 . . . ? C15 Cr2 C11 C16 121.2(3) . . . . ? C14 Cr2 C11 C16 50.9(3) 2_665 . . . ? C14 Cr2 C11 C16 158.7(3) . . . . ? C12 Cr2 C11 C16 -31.1(3) 2_665 . . . ? C12 Cr2 C11 C16 -120.9(3) . . . . ? C11 Cr2 C11 C16 -66.7(3) 2_665 . . . ? C13 Cr2 C11 C16 -158.5(3) . . . . ? C13 Cr2 C11 C16 11.3(3) 2_665 . . . ? C15 C11 C12 C13 0.0(3) . . . . ? C16 C11 C12 C13 179.8(2) . . . . ? Cr2 C11 C12 C13 61.78(17) . . . . ? C15 C11 C12 C17 180.0(3) . . . . ? C16 C11 C12 C17 -0.2(4) . . . . ? Cr2 C11 C12 C17 -118.3(3) . . . . ? C15 C11 C12 Cr2 -61.75(17) . . . . ? C16 C11 C12 Cr2 118.1(2) . . . . ? C15 Cr2 C12 C11 171.5(2) 2_665 . . . ? C15 Cr2 C12 C11 37.22(15) . . . . ? C14 Cr2 C12 C11 -37.2(6) 2_665 . . . ? C14 Cr2 C12 C11 79.82(16) . . . . ? C12 Cr2 C12 C11 -110.60(16) 2_665 . . . ? C11 Cr2 C12 C11 -152.78(16) 2_665 . . . ? C13 Cr2 C12 C11 117.8(2) . . . . ? C13 Cr2 C12 C11 -70.61(19) 2_665 . . . ? C15 Cr2 C12 C13 53.7(3) 2_665 . . . ? C15 Cr2 C12 C13 -80.55(16) . . . . ? C14 Cr2 C12 C13 -155.0(5) 2_665 . . . ? C14 Cr2 C12 C13 -37.95(14) . . . . ? C12 Cr2 C12 C13 131.63(16) 2_665 . . . ? C11 Cr2 C12 C13 89.45(16) 2_665 . . . ? C11 Cr2 C12 C13 -117.8(2) . . . . ? C13 Cr2 C12 C13 171.62(12) 2_665 . . . ? C15 Cr2 C12 C17 -66.4(3) 2_665 . . . ? C15 Cr2 C12 C17 159.3(3) . . . . ? C14 Cr2 C12 C17 84.9(6) 2_665 . . . ? C14 Cr2 C12 C17 -158.1(3) . . . . ? C12 Cr2 C12 C17 11.47(19) 2_665 . . . ? C11 Cr2 C12 C17 -30.7(3) 2_665 . . . ? C11 Cr2 C12 C17 122.1(3) . . . . ? C13 Cr2 C12 C17 -120.2(3) . . . . ? C13 Cr2 C12 C17 51.5(3) 2_665 . . . ? C11 C12 C13 C14 0.0(3) . . . . ? C17 C12 C13 C14 -179.9(3) . . . . ? Cr2 C12 C13 C14 61.83(15) . . . . ? C11 C12 C13 C18 179.7(2) . . . . ? C17 C12 C13 C18 -0.3(4) . . . . ? Cr2 C12 C13 C18 -118.5(2) . . . . ? C11 C12 C13 Cr2 -61.80(17) . . . . ? C17 C12 C13 Cr2 118.3(3) . . . . ? C15 Cr2 C13 C14 90.24(15) 2_665 . . . ? C15 Cr2 C13 C14 -37.34(14) . . . . ? C14 Cr2 C13 C14 54.8(3) 2_665 . . . ? C12 Cr2 C13 C14 171.34(15) 2_665 . . . ? C12 Cr2 C13 C14 -116.9(2) . . . . ? C11 Cr2 C13 C14 132.15(15) 2_665 . . . ? C11 Cr2 C13 C14 -79.60(15) . . . . ? C13 Cr2 C13 C14 -155.89(13) 2_665 . . . ? C15 Cr2 C13 C12 -152.89(15) 2_665 . . . ? C15 Cr2 C13 C12 79.53(16) . . . . ? C14 Cr2 C13 C12 171.68(18) 2_665 . . . ? C14 Cr2 C13 C12 116.9(2) . . . . ? C12 Cr2 C13 C12 -71.8(2) 2_665 . . . ? C11 Cr2 C13 C12 -110.98(17) 2_665 . . . ? C11 Cr2 C13 C12 37.27(15) . . . . ? C13 Cr2 C13 C12 -39.02(14) 2_665 . . . ? C15 Cr2 C13 C18 -31.7(3) 2_665 . . . ? C15 Cr2 C13 C18 -159.3(2) . . . . ? C14 Cr2 C13 C18 -67.2(3) 2_665 . . . ? C14 Cr2 C13 C18 -122.0(3) . . . . ? C12 Cr2 C13 C18 49.4(3) 2_665 . . . ? C12 Cr2 C13 C18 121.2(3) . . . . ? C11 Cr2 C13 C18 10.2(2) 2_665 . . . ? C11 Cr2 C13 C18 158.4(3) . . . . ? C13 Cr2 C13 C18 82.2(2) 2_665 . . . ? C12 C13 C14 C15 -0.1(3) . . . . ? C18 C13 C14 C15 -179.7(2) . . . . ? Cr2 C13 C14 C15 61.73(17) . . . . ? C12 C13 C14 C19 -178.9(3) . . . . ? C18 C13 C14 C19 1.5(4) . . . . ? Cr2 C13 C14 C19 -117.1(3) . . . . ? C12 C13 C14 Cr2 -61.83(15) . . . . ? C18 C13 C14 Cr2 118.5(2) . . . . ? C15 Cr2 C14 C15 132.31(16) 2_665 . . . ? C14 Cr2 C14 C15 90.15(14) 2_665 . . . ? C12 Cr2 C14 C15 -157.6(6) 2_665 . . . ? C12 Cr2 C14 C15 -79.78(16) . . . . ? C11 Cr2 C14 C15 171.26(16) 2_665 . . . ? C11 Cr2 C14 C15 -37.29(15) . . . . ? C13 Cr2 C14 C15 -117.8(2) . . . . ? C13 Cr2 C14 C15 54.3(2) 2_665 . . . ? C15 Cr2 C14 C13 -109.91(14) 2_665 . . . ? C15 Cr2 C14 C13 117.8(2) . . . . ? C14 Cr2 C14 C13 -152.06(15) 2_665 . . . ? C12 Cr2 C14 C13 -39.8(6) 2_665 . . . ? C12 Cr2 C14 C13 38.00(13) . . . . ? C11 Cr2 C14 C13 -70.96(18) 2_665 . . . ? C11 Cr2 C14 C13 80.49(15) . . . . ? C13 Cr2 C14 C13 172.08(12) 2_665 . . . ? C15 Cr2 C14 C19 12.0(2) 2_665 . . . ? C15 Cr2 C14 C19 -120.3(3) . . . . ? C14 Cr2 C14 C19 -30.13(17) 2_665 . . . ? C12 Cr2 C14 C19 82.1(6) 2_665 . . . ? C12 Cr2 C14 C19 159.9(2) . . . . ? C11 Cr2 C14 C19 51.0(2) 2_665 . . . ? C11 Cr2 C14 C19 -157.6(2) . . . . ? C13 Cr2 C14 C19 121.9(3) . . . . ? C13 Cr2 C14 C19 -66.0(3) 2_665 . . . ? C12 C11 C15 C14 -0.1(3) . . . . ? C16 C11 C15 C14 -179.9(2) . . . . ? Cr2 C11 C15 C14 -61.82(17) . . . . ? C12 C11 C15 C20 -179.7(2) . . . . ? C16 C11 C15 C20 0.5(4) . . . . ? Cr2 C11 C15 C20 118.6(3) . . . . ? C12 C11 C15 Cr2 61.73(17) . . . . ? C16 C11 C15 Cr2 -118.1(2) . . . . ? C13 C14 C15 C11 0.1(3) . . . . ? C19 C14 C15 C11 178.9(2) . . . . ? Cr2 C14 C15 C11 61.91(17) . . . . ? C13 C14 C15 C20 179.7(2) . . . . ? C19 C14 C15 C20 -1.5(4) . . . . ? Cr2 C14 C15 C20 -118.5(3) . . . . ? C13 C14 C15 Cr2 -61.79(16) . . . . ? C19 C14 C15 Cr2 117.0(3) . . . . ? C15 Cr2 C15 C11 171.69(17) 2_665 . . . ? C14 Cr2 C15 C11 132.42(15) 2_665 . . . ? C14 Cr2 C15 C11 -117.7(2) . . . . ? C12 Cr2 C15 C11 54.7(3) 2_665 . . . ? C12 Cr2 C15 C11 -37.35(15) . . . . ? C11 Cr2 C15 C11 -157.3(5) 2_665 . . . ? C13 Cr2 C15 C11 -80.18(16) . . . . ? C13 Cr2 C15 C11 90.04(17) 2_665 . . . ? C15 Cr2 C15 C14 -70.61(13) 2_665 . . . ? C14 Cr2 C15 C14 -109.88(17) 2_665 . . . ? C12 Cr2 C15 C14 172.41(18) 2_665 . . . ? C12 Cr2 C15 C14 80.36(15) . . . . ? C11 Cr2 C15 C14 -39.6(7) 2_665 . . . ? C11 Cr2 C15 C14 117.7(2) . . . . ? C13 Cr2 C15 C14 37.53(14) . . . . ? C13 Cr2 C15 C14 -152.25(14) 2_665 . . . ? C15 Cr2 C15 C20 50.1(2) 2_665 . . . ? C14 Cr2 C15 C20 10.8(2) 2_665 . . . ? C14 Cr2 C15 C20 120.7(3) . . . . ? C12 Cr2 C15 C20 -66.9(3) 2_665 . . . ? C12 Cr2 C15 C20 -158.9(3) . . . . ? C11 Cr2 C15 C20 81.2(7) 2_665 . . . ? C11 Cr2 C15 C20 -121.6(3) . . . . ? C13 Cr2 C15 C20 158.2(2) . . . . ? C13 Cr2 C15 C20 -31.5(3) 2_665 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.714 _refine_diff_density_min -0.388 _refine_diff_density_rms 0.058