data_MR266_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H21 P S' _chemical_formula_weight 432.49 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.76910(10) _cell_length_b 14.6930(3) _cell_length_c 15.2033(2) _cell_angle_alpha 90 _cell_angle_beta 96.5688(8) _cell_angle_gamma 90 _cell_volume 2167.92(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8716 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 26.43 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_F_000 904 _exptl_transmission_factor_min 0.8773 _exptl_transmission_factor_max 0.9582 _exptl_crystal_size_max 0.410 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 0.238 _shelx_estimated_absorpt_T_min 0.909 _shelx_estimated_absorpt_T_max 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'D8 Venture, Bruker Photon CMOS Detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18563 _diffrn_reflns_av_unetI/netI 0.0372 _diffrn_reflns_av_R_equivalents 0.0476 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.515 _diffrn_reflns_theta_max 26.427 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4455 _reflns_number_gt 3660 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Diamond 2.1e' _computing_publication_material 'Microsoft Word' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0368P)^2^+1.3681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4455 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0881 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.43445(16) 0.28784(12) 0.50105(11) 0.0119(3) Uani 1 1 d . . . . . C2 C 0.47176(16) 0.34444(11) 0.56807(11) 0.0123(3) Uani 1 1 d . . . . . H2 H 0.5670 0.3545 0.5858 0.015 Uiso 1 1 calc R U . . . C3 C 0.36475(16) 0.39378(11) 0.61722(11) 0.0116(3) Uani 1 1 d . . . . . C4 C 0.26915(16) 0.32019(12) 0.64822(11) 0.0121(3) Uani 1 1 d . . . . . H4 H 0.2557 0.3165 0.7090 0.015 Uiso 1 1 calc R U . . . C5 C 0.20493(16) 0.26145(11) 0.59069(11) 0.0110(3) Uani 1 1 d . . . . . C6 C 0.10567(16) 0.19180(12) 0.61392(11) 0.0112(3) Uani 1 1 d . . . . . C7 C 0.00885(17) 0.21476(12) 0.67114(11) 0.0149(4) Uani 1 1 d . . . . . H7 H 0.0033 0.2757 0.6912 0.018 Uiso 1 1 calc R U . . . C8 C -0.07927(17) 0.14931(13) 0.69889(12) 0.0189(4) Uani 1 1 d . . . . . H8 H -0.1445 0.1654 0.7380 0.023 Uiso 1 1 calc R U . . . C9 C -0.07184(18) 0.06052(13) 0.66936(13) 0.0207(4) Uani 1 1 d . . . . . H9 H -0.1312 0.0155 0.6890 0.025 Uiso 1 1 calc R U . . . C10 C 0.02162(17) 0.03704(12) 0.61141(12) 0.0179(4) Uani 1 1 d . . . . . H10 H 0.0259 -0.0239 0.5911 0.022 Uiso 1 1 calc R U . . . C11 C 0.10935(17) 0.10247(12) 0.58289(12) 0.0142(4) Uani 1 1 d . . . . . H11 H 0.1721 0.0864 0.5421 0.017 Uiso 1 1 calc R U . . . C12 C 0.53405(16) 0.24029(11) 0.45087(11) 0.0122(3) Uani 1 1 d . . . . . C13 C 0.64960(18) 0.19830(12) 0.49672(12) 0.0175(4) Uani 1 1 d . . . . . H13 H 0.6582 0.1946 0.5595 0.021 Uiso 1 1 calc R U . . . C14 C 0.75137(19) 0.16215(14) 0.45080(13) 0.0235(4) Uani 1 1 d . . . . . H14 H 0.8294 0.1336 0.4823 0.028 Uiso 1 1 calc R U . . . C15 C 0.74037(19) 0.16723(13) 0.35930(13) 0.0227(4) Uani 1 1 d . . . . . H15 H 0.8111 0.1431 0.3282 0.027 Uiso 1 1 calc R U . . . C16 C 0.62530(18) 0.20776(13) 0.31339(12) 0.0200(4) Uani 1 1 d . . . . . H16 H 0.6171 0.2112 0.2506 0.024 Uiso 1 1 calc R U . . . C17 C 0.52226(18) 0.24327(12) 0.35878(12) 0.0157(4) Uani 1 1 d . . . . . H17 H 0.4430 0.2699 0.3268 0.019 Uiso 1 1 calc R U . . . C18 C 0.43347(17) 0.45369(11) 0.69169(11) 0.0127(3) Uani 1 1 d . . . . . C19 C 0.38222(17) 0.46067(12) 0.77298(12) 0.0166(4) Uani 1 1 d . . . . . H19 H 0.3038 0.4259 0.7835 0.020 Uiso 1 1 calc R U . . . C20 C 0.44334(18) 0.51751(13) 0.83910(13) 0.0199(4) Uani 1 1 d . . . . . H20 H 0.4061 0.5218 0.8940 0.024 Uiso 1 1 calc R U . . . C21 C 0.55831(18) 0.56784(13) 0.82516(12) 0.0189(4) Uani 1 1 d . . . . . H21 H 0.6000 0.6071 0.8701 0.023 Uiso 1 1 calc R U . . . C22 C 0.61221(17) 0.56055(13) 0.74516(12) 0.0184(4) Uani 1 1 d . . . . . H22 H 0.6927 0.5938 0.7357 0.022 Uiso 1 1 calc R U . . . C23 C 0.54944(17) 0.50511(12) 0.67884(12) 0.0158(4) Uani 1 1 d . . . . . H23 H 0.5860 0.5020 0.6236 0.019 Uiso 1 1 calc R U . . . C24 C 0.20985(16) 0.40177(12) 0.47375(11) 0.0122(3) Uani 1 1 d . . . . . C25 C 0.27365(16) 0.45056(12) 0.54610(11) 0.0123(3) Uani 1 1 d . . . . . C26 C 0.25123(17) 0.54358(12) 0.55063(12) 0.0166(4) Uani 1 1 d . . . . . H26 H 0.2943 0.5781 0.5989 0.020 Uiso 1 1 calc R U . . . C27 C 0.16427(18) 0.58602(13) 0.48313(13) 0.0204(4) Uani 1 1 d . . . . . H27 H 0.1480 0.6496 0.4862 0.025 Uiso 1 1 calc R U . . . C28 C 0.10195(18) 0.53679(13) 0.41223(13) 0.0205(4) Uani 1 1 d . . . . . H28 H 0.0438 0.5667 0.3668 0.025 Uiso 1 1 calc R U . . . C29 C 0.12407(17) 0.44335(13) 0.40707(12) 0.0162(4) Uani 1 1 d . . . . . H29 H 0.0810 0.4089 0.3587 0.019 Uiso 1 1 calc R U . . . P1 P 0.24667(4) 0.28102(3) 0.47790(3) 0.01066(11) Uani 1 1 d . . . . . S1 S 0.15949(4) 0.20635(3) 0.38250(3) 0.01639(12) Uani 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 0.0095(7) 0.0113(9) 0.0149(8) 0.0035(7) 0.0009(6) 0.0000(6) C2 0.0091(7) 0.0114(8) 0.0162(9) 0.0031(7) 0.0003(6) -0.0002(6) C3 0.0109(8) 0.0096(8) 0.0143(9) 0.0002(7) 0.0009(6) -0.0005(6) C4 0.0123(8) 0.0128(9) 0.0113(8) 0.0016(7) 0.0015(6) 0.0018(6) C5 0.0112(8) 0.0092(8) 0.0126(8) 0.0019(6) 0.0009(6) 0.0022(6) C6 0.0098(7) 0.0124(9) 0.0103(8) 0.0022(6) -0.0039(6) -0.0009(6) C7 0.0146(8) 0.0146(9) 0.0147(9) 0.0005(7) -0.0018(7) 0.0002(7) C8 0.0124(8) 0.0249(10) 0.0193(9) 0.0032(8) 0.0019(7) -0.0010(7) C9 0.0158(9) 0.0180(10) 0.0271(10) 0.0069(8) -0.0028(8) -0.0080(7) C10 0.0164(8) 0.0109(9) 0.0245(10) -0.0004(7) -0.0064(7) -0.0007(7) C11 0.0125(8) 0.0135(9) 0.0158(9) 0.0007(7) -0.0025(7) 0.0010(7) C12 0.0111(8) 0.0095(8) 0.0163(9) -0.0013(7) 0.0022(7) -0.0017(6) C13 0.0180(9) 0.0169(10) 0.0171(9) -0.0002(7) -0.0003(7) 0.0023(7) C14 0.0171(9) 0.0250(11) 0.0281(11) -0.0003(9) 0.0007(8) 0.0089(8) C15 0.0176(9) 0.0230(11) 0.0289(11) -0.0047(8) 0.0092(8) 0.0028(8) C16 0.0208(9) 0.0217(10) 0.0181(9) -0.0030(8) 0.0055(7) -0.0042(8) C17 0.0134(8) 0.0154(9) 0.0180(9) -0.0002(7) 0.0004(7) -0.0009(7) C18 0.0121(8) 0.0086(8) 0.0166(9) -0.0013(7) -0.0012(7) 0.0020(6) C19 0.0127(8) 0.0147(9) 0.0230(10) -0.0067(7) 0.0044(7) -0.0025(7) C20 0.0198(9) 0.0193(10) 0.0215(10) -0.0076(8) 0.0067(8) -0.0015(7) C21 0.0175(9) 0.0166(10) 0.0212(10) -0.0072(8) -0.0033(7) -0.0005(7) C22 0.0133(8) 0.0158(10) 0.0253(10) 0.0009(8) -0.0004(7) -0.0033(7) C23 0.0161(8) 0.0149(9) 0.0162(9) 0.0009(7) 0.0016(7) -0.0026(7) C24 0.0092(7) 0.0123(9) 0.0158(9) 0.0028(7) 0.0041(6) -0.0004(6) C25 0.0088(7) 0.0131(9) 0.0157(9) 0.0032(7) 0.0043(7) -0.0005(6) C26 0.0138(8) 0.0136(9) 0.0232(10) 0.0002(7) 0.0052(7) -0.0012(7) C27 0.0174(9) 0.0114(9) 0.0333(11) 0.0069(8) 0.0064(8) 0.0020(7) C28 0.0155(9) 0.0200(10) 0.0259(10) 0.0104(8) 0.0022(8) 0.0033(7) C29 0.0118(8) 0.0203(10) 0.0166(9) 0.0052(7) 0.0023(7) -0.0014(7) P1 0.0089(2) 0.0117(2) 0.0111(2) -0.00022(17) 0.00024(15) -0.00028(16) S1 0.0148(2) 0.0207(3) 0.0133(2) -0.00419(18) -0.00004(16) -0.00261(17) _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 1.333(2) . ? C1 C12 1.479(2) . ? C1 P1 1.8306(16) . ? C2 C3 1.535(2) . ? C2 H2 0.9500 . ? C3 C18 1.528(2) . ? C3 C4 1.538(2) . ? C3 C25 1.561(2) . ? C4 C5 1.333(2) . ? C4 H4 0.9500 . ? C5 C6 1.480(2) . ? C5 P1 1.8301(17) . ? C6 C11 1.397(2) . ? C6 C7 1.398(2) . ? C7 C8 1.388(2) . ? C7 H7 0.9500 . ? C8 C9 1.384(3) . ? C8 H8 0.9500 . ? C9 C10 1.383(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.392(2) . ? C12 C13 1.400(2) . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 C17 1.386(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.389(2) . ? C18 C23 1.394(2) . ? C19 C20 1.388(2) . ? C19 H19 0.9500 . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.382(2) . ? C24 C25 1.398(2) . ? C24 P1 1.8099(18) . ? C25 C26 1.387(2) . ? C26 C27 1.401(3) . ? C26 H26 0.9500 . ? C27 C28 1.380(3) . ? C27 H27 0.9500 . ? C28 C29 1.393(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? P1 S1 1.9366(6) . ? 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 C12 123.40(15) . . ? C2 C1 P1 111.18(12) . . ? C12 C1 P1 125.38(12) . . ? C1 C2 C3 121.66(14) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C18 C3 C2 111.53(13) . . ? C18 C3 C4 114.13(14) . . ? C2 C3 C4 106.77(13) . . ? C18 C3 C25 111.89(14) . . ? C2 C3 C25 106.34(13) . . ? C4 C3 C25 105.66(12) . . ? C5 C4 C3 120.72(15) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 124.26(15) . . ? C4 C5 P1 111.99(12) . . ? C6 C5 P1 123.67(12) . . ? C11 C6 C7 118.85(15) . . ? C11 C6 C5 121.76(15) . . ? C7 C6 C5 119.35(15) . . ? C8 C7 C6 120.62(17) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 119.80(17) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C10 C9 C8 120.31(17) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.11(17) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.27(16) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C17 C12 C13 118.93(16) . . ? C17 C12 C1 121.35(15) . . ? C13 C12 C1 119.46(16) . . ? C14 C13 C12 120.16(17) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.54(17) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 119.58(17) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C17 C16 C15 120.25(18) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C12 120.51(17) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C19 C18 C23 117.78(16) . . ? C19 C18 C3 121.96(15) . . ? C23 C18 C3 120.25(15) . . ? C20 C19 C18 121.31(16) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C21 C20 C19 120.06(17) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C20 C21 C22 119.43(17) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C21 C22 C23 120.31(16) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 121.10(16) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C29 C24 C25 121.93(16) . . ? C29 C24 P1 124.09(14) . . ? C25 C24 P1 113.97(12) . . ? C26 C25 C24 119.05(16) . . ? C26 C25 C3 124.95(15) . . ? C24 C25 C3 116.00(14) . . ? C25 C26 C27 119.20(17) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C28 C27 C26 120.99(17) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 120.18(17) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C24 C29 C28 118.64(17) . . ? C24 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C24 P1 C5 97.01(8) . . ? C24 P1 C1 98.27(8) . . ? C5 P1 C1 98.87(7) . . ? C24 P1 S1 117.43(6) . . ? C5 P1 S1 119.12(6) . . ? C1 P1 S1 121.34(6) . . ? 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 C12 C1 C2 C3 178.82(15) . . . . ? P1 C1 C2 C3 1.0(2) . . . . ? C1 C2 C3 C18 179.37(16) . . . . ? C1 C2 C3 C4 54.1(2) . . . . ? C1 C2 C3 C25 -58.4(2) . . . . ? C18 C3 C4 C5 -178.30(15) . . . . ? C2 C3 C4 C5 -54.59(19) . . . . ? C25 C3 C4 C5 58.34(19) . . . . ? C3 C4 C5 C6 -176.62(15) . . . . ? C3 C4 C5 P1 0.2(2) . . . . ? C4 C5 C6 C11 -135.97(18) . . . . ? P1 C5 C6 C11 47.5(2) . . . . ? C4 C5 C6 C7 41.5(2) . . . . ? P1 C5 C6 C7 -134.98(14) . . . . ? C11 C6 C7 C8 2.0(2) . . . . ? C5 C6 C7 C8 -175.57(15) . . . . ? C6 C7 C8 C9 -0.3(3) . . . . ? C7 C8 C9 C10 -0.9(3) . . . . ? C8 C9 C10 C11 0.4(3) . . . . ? C9 C10 C11 C6 1.3(3) . . . . ? C7 C6 C11 C10 -2.5(2) . . . . ? C5 C6 C11 C10 175.02(15) . . . . ? C2 C1 C12 C17 -128.76(19) . . . . ? P1 C1 C12 C17 48.8(2) . . . . ? C2 C1 C12 C13 45.4(2) . . . . ? P1 C1 C12 C13 -137.08(15) . . . . ? C17 C12 C13 C14 1.3(3) . . . . ? C1 C12 C13 C14 -172.97(17) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 -0.9(3) . . . . ? C14 C15 C16 C17 0.2(3) . . . . ? C15 C16 C17 C12 1.2(3) . . . . ? C13 C12 C17 C16 -2.0(3) . . . . ? C1 C12 C17 C16 172.17(16) . . . . ? C2 C3 C18 C19 -140.45(16) . . . . ? C4 C3 C18 C19 -19.3(2) . . . . ? C25 C3 C18 C19 100.58(18) . . . . ? C2 C3 C18 C23 41.0(2) . . . . ? C4 C3 C18 C23 162.06(15) . . . . ? C25 C3 C18 C23 -78.01(19) . . . . ? C23 C18 C19 C20 0.6(3) . . . . ? C3 C18 C19 C20 -178.03(16) . . . . ? C18 C19 C20 C21 -0.7(3) . . . . ? C19 C20 C21 C22 -0.4(3) . . . . ? C20 C21 C22 C23 1.7(3) . . . . ? C21 C22 C23 C18 -1.8(3) . . . . ? C19 C18 C23 C22 0.6(3) . . . . ? C3 C18 C23 C22 179.28(16) . . . . ? C29 C24 C25 C26 -0.6(2) . . . . ? P1 C24 C25 C26 -179.10(12) . . . . ? C29 C24 C25 C3 178.56(14) . . . . ? P1 C24 C25 C3 0.09(18) . . . . ? C18 C3 C25 C26 -2.8(2) . . . . ? C2 C3 C25 C26 -124.78(17) . . . . ? C4 C3 C25 C26 121.99(17) . . . . ? C18 C3 C25 C24 178.08(14) . . . . ? C2 C3 C25 C24 56.08(17) . . . . ? C4 C3 C25 C24 -57.15(18) . . . . ? C24 C25 C26 C27 0.6(2) . . . . ? C3 C25 C26 C27 -178.49(15) . . . . ? C25 C26 C27 C28 -0.5(3) . . . . ? C26 C27 C28 C29 0.5(3) . . . . ? C25 C24 C29 C28 0.5(2) . . . . ? P1 C24 C29 C28 178.84(13) . . . . ? C27 C28 C29 C24 -0.4(3) . . . . ? C29 C24 P1 C5 -128.10(14) . . . . ? C25 C24 P1 C5 50.33(13) . . . . ? C29 C24 P1 C1 131.83(14) . . . . ? C25 C24 P1 C1 -49.74(13) . . . . ? C29 C24 P1 S1 -0.06(16) . . . . ? C25 C24 P1 S1 178.37(10) . . . . ? C4 C5 P1 C24 -50.89(13) . . . . ? C6 C5 P1 C24 125.99(14) . . . . ? C4 C5 P1 C1 48.66(14) . . . . ? C6 C5 P1 C1 -134.46(14) . . . . ? C4 C5 P1 S1 -177.74(10) . . . . ? C6 C5 P1 S1 -0.86(16) . . . . ? C2 C1 P1 C24 49.37(14) . . . . ? C12 C1 P1 C24 -128.45(15) . . . . ? C2 C1 P1 C5 -49.11(14) . . . . ? C12 C1 P1 C5 133.07(15) . . . . ? C2 C1 P1 S1 178.68(10) . . . . ? C12 C1 P1 S1 0.86(17) . . . . ? _refine_diff_density_max 0.320 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.056 _shelx_res_file ; MR266_a.res created by SHELXL-2014/7 TITL MR266_a.res in P2(1)/c REM Old TITL MR266 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.094, Rweak 0.004, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C29 P S CELL 0.71073 9.7691 14.6930 15.2033 90.000 96.5688 90.000 ZERR 4.000 0.0001 0.0003 0.0002 0.0000 0.0008 0.000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H P S UNIT 116 84 4 4 TEMP -173.150 SIZE 0.06 0.16 0.41 L.S. 30 BOND $H LIST 6 acta conf FMAP 2 PLAN 20 WGHT 0.036800 1.368100 FVAR 0.42398 C1 1 0.434452 0.287837 0.501051 11.00000 0.00953 0.01133 = 0.01487 0.00352 0.00092 0.00003 C2 1 0.471759 0.344441 0.568072 11.00000 0.00915 0.01144 = 0.01616 0.00311 0.00026 -0.00015 AFIX 43 H2 2 0.566974 0.354481 0.585850 11.00000 -1.20000 AFIX 0 C3 1 0.364745 0.393784 0.617220 11.00000 0.01089 0.00957 = 0.01434 0.00018 0.00087 -0.00046 C4 1 0.269146 0.320193 0.648223 11.00000 0.01233 0.01279 = 0.01131 0.00163 0.00146 0.00179 AFIX 43 H4 2 0.255686 0.316538 0.709025 11.00000 -1.20000 AFIX 0 C5 1 0.204930 0.261451 0.590692 11.00000 0.01120 0.00915 = 0.01262 0.00191 0.00094 0.00225 C6 1 0.105667 0.191804 0.613917 11.00000 0.00979 0.01239 = 0.01032 0.00223 -0.00388 -0.00090 C7 1 0.008851 0.214759 0.671140 11.00000 0.01458 0.01455 = 0.01470 0.00047 -0.00182 0.00017 AFIX 43 H7 2 0.003300 0.275726 0.691233 11.00000 -1.20000 AFIX 0 C8 1 -0.079274 0.149307 0.698889 11.00000 0.01240 0.02486 = 0.01932 0.00321 0.00194 -0.00097 AFIX 43 H8 2 -0.144481 0.165399 0.738028 11.00000 -1.20000 AFIX 0 C9 1 -0.071845 0.060523 0.669357 11.00000 0.01585 0.01795 = 0.02711 0.00688 -0.00284 -0.00803 AFIX 43 H9 2 -0.131220 0.015510 0.688983 11.00000 -1.20000 AFIX 0 C10 1 0.021623 0.037039 0.611406 11.00000 0.01639 0.01087 = 0.02454 -0.00035 -0.00637 -0.00072 AFIX 43 H10 2 0.025865 -0.023918 0.591061 11.00000 -1.20000 AFIX 0 C11 1 0.109352 0.102474 0.582887 11.00000 0.01250 0.01347 = 0.01579 0.00072 -0.00252 0.00096 AFIX 43 H11 2 0.172077 0.086367 0.542121 11.00000 -1.20000 AFIX 0 C12 1 0.534048 0.240288 0.450868 11.00000 0.01106 0.00946 = 0.01626 -0.00131 0.00217 -0.00172 C13 1 0.649597 0.198301 0.496723 11.00000 0.01797 0.01686 = 0.01711 -0.00016 -0.00029 0.00233 AFIX 43 H13 2 0.658178 0.194611 0.559497 11.00000 -1.20000 AFIX 0 C14 1 0.751367 0.162153 0.450804 11.00000 0.01705 0.02495 = 0.02810 -0.00029 0.00065 0.00886 AFIX 43 H14 2 0.829386 0.133633 0.482317 11.00000 -1.20000 AFIX 0 C15 1 0.740368 0.167226 0.359304 11.00000 0.01763 0.02297 = 0.02888 -0.00468 0.00916 0.00276 AFIX 43 H15 2 0.811139 0.143111 0.328167 11.00000 -1.20000 AFIX 0 C16 1 0.625301 0.207764 0.313389 11.00000 0.02080 0.02173 = 0.01812 -0.00305 0.00555 -0.00416 AFIX 43 H16 2 0.617138 0.211186 0.250608 11.00000 -1.20000 AFIX 0 C17 1 0.522258 0.243271 0.358784 11.00000 0.01342 0.01541 = 0.01803 -0.00022 0.00043 -0.00091 AFIX 43 H17 2 0.442971 0.269851 0.326820 11.00000 -1.20000 AFIX 0 C18 1 0.433466 0.453693 0.691693 11.00000 0.01213 0.00857 = 0.01665 -0.00132 -0.00118 0.00204 C19 1 0.382221 0.460669 0.772981 11.00000 0.01270 0.01466 = 0.02303 -0.00672 0.00444 -0.00252 AFIX 43 H19 2 0.303797 0.425852 0.783528 11.00000 -1.20000 AFIX 0 C20 1 0.443339 0.517508 0.839103 11.00000 0.01978 0.01933 = 0.02145 -0.00763 0.00665 -0.00151 AFIX 43 H20 2 0.406056 0.521789 0.893991 11.00000 -1.20000 AFIX 0 C21 1 0.558313 0.567845 0.825156 11.00000 0.01754 0.01663 = 0.02124 -0.00722 -0.00330 -0.00047 AFIX 43 H21 2 0.600020 0.607134 0.870102 11.00000 -1.20000 AFIX 0 C22 1 0.612213 0.560548 0.745157 11.00000 0.01332 0.01584 = 0.02532 0.00094 -0.00039 -0.00331 AFIX 43 H22 2 0.692690 0.593751 0.735719 11.00000 -1.20000 AFIX 0 C23 1 0.549437 0.505114 0.678840 11.00000 0.01610 0.01493 = 0.01618 0.00089 0.00157 -0.00263 AFIX 43 H23 2 0.585978 0.502047 0.623632 11.00000 -1.20000 AFIX 0 C24 1 0.209851 0.401770 0.473753 11.00000 0.00916 0.01226 = 0.01583 0.00277 0.00407 -0.00038 C25 1 0.273648 0.450560 0.546099 11.00000 0.00884 0.01311 = 0.01567 0.00323 0.00428 -0.00050 C26 1 0.251227 0.543579 0.550634 11.00000 0.01376 0.01356 = 0.02317 0.00018 0.00524 -0.00120 AFIX 43 H26 2 0.294296 0.578103 0.598916 11.00000 -1.20000 AFIX 0 C27 1 0.164272 0.586017 0.483131 11.00000 0.01738 0.01139 = 0.03331 0.00691 0.00642 0.00203 AFIX 43 H27 2 0.147972 0.649617 0.486216 11.00000 -1.20000 AFIX 0 C28 1 0.101950 0.536794 0.412226 11.00000 0.01547 0.01997 = 0.02594 0.01041 0.00225 0.00326 AFIX 43 H28 2 0.043822 0.566709 0.366821 11.00000 -1.20000 AFIX 0 C29 1 0.124067 0.443349 0.407067 11.00000 0.01178 0.02026 = 0.01658 0.00522 0.00230 -0.00138 AFIX 43 H29 2 0.081044 0.408938 0.358690 11.00000 -1.20000 AFIX 0 P1 3 0.246674 0.281021 0.477904 11.00000 0.00890 0.01174 = 0.01114 -0.00022 0.00024 -0.00028 S1 4 0.159486 0.206347 0.382499 11.00000 0.01481 0.02068 = 0.01330 -0.00419 -0.00004 -0.00261 HKLF 4 REM MR266_a.res in P2(1)/c REM R1 = 0.0364 for 3660 Fo > 4sig(Fo) and 0.0500 for all 4455 data REM 280 parameters refined using 0 restraints END WGHT 0.0368 1.3681 REM Highest difference peak 0.320, deepest hole -0.314, 1-sigma level 0.056 Q1 1 0.3553 0.2814 0.4902 11.00000 0.05 0.32 Q2 1 0.1634 0.2211 0.6064 11.00000 0.05 0.31 Q3 1 0.2241 0.2621 0.5382 11.00000 0.05 0.30 Q4 1 0.3192 0.3554 0.6330 11.00000 0.05 0.29 Q5 1 0.4166 0.3728 0.5915 11.00000 0.05 0.29 Q6 1 0.3190 0.4244 0.5845 11.00000 0.05 0.28 Q7 1 0.3999 0.4199 0.6547 11.00000 0.05 0.27 Q8 1 0.2268 0.3452 0.4734 11.00000 0.05 0.27 Q9 1 0.4804 0.5576 0.8232 11.00000 0.05 0.26 Q10 1 0.1792 0.2447 0.4444 11.00000 0.05 0.26 Q11 1 0.0773 0.1939 0.6574 11.00000 0.05 0.25 Q12 1 0.4809 0.2641 0.4782 11.00000 0.05 0.24 Q13 1 0.2415 0.4885 0.5697 11.00000 0.05 0.23 Q14 1 0.5440 0.2599 0.4035 11.00000 0.05 0.23 Q15 1 0.2009 0.4368 0.4358 11.00000 0.05 0.23 Q16 1 0.2124 0.2542 0.4188 11.00000 0.05 0.23 Q17 1 0.0861 0.0627 0.6132 11.00000 0.05 0.22 Q18 1 0.4327 0.4703 0.8123 11.00000 0.05 0.21 Q19 1 0.4501 0.2881 0.5475 11.00000 0.05 0.21 Q20 1 0.4863 0.4786 0.6853 11.00000 0.05 0.21 ; _shelx_res_checksum 83729 _shelx_hkl_file ; 2 0 0 42.20 1.60 -2 0 0 47.60 2.20 3 0 0 1304.77 30.10 -3 0 0 1468.25 31.30 -4 0 0 32.00 3.00 4 0 0 32.30 1.80 5 0 0 75.49 3.10 -5 0 0 72.59 4.50 6 0 0 656.23 15.40 -6 0 0 600.14 18.30 7 0 0 139.39 5.10 -7 0 0 135.89 7.00 -8 0 0 452.45 14.20 8 0 0 418.16 11.80 9 0 0 14.10 2.30 -9 0 0 14.20 4.40 -10 0 0 504.05 16.40 10 0 0 458.25 13.50 11 0 0 372.86 11.80 -11 0 0 377.36 14.40 -12 0 0 76.39 8.20 12 0 0 73.59 6.50 1 -1 0 2048.40 46.00 1 1 0 2238.38 45.60 2 -1 0 689.33 15.80 2 -1 0 690.13 16.20 -2 -1 0 737.13 15.90 -2 1 0 701.33 16.10 2 1 0 767.72 16.10 -2 1 0 681.53 15.80 -3 -1 0 118.39 3.90 3 -1 0 112.39 3.50 3 1 0 109.09 3.10 -3 1 0 115.39 3.50 -3 1 0 118.69 4.70 -3 1 0 106.39 3.30 4 -1 0 655.23 15.70 -4 -1 0 692.73 16.40 -4 1 0 692.03 17.40 4 1 0 657.73 15.30 -5 -1 0 21.90 2.80 5 -1 0 24.40 2.00 5 1 0 25.50 1.80 6 -1 0 18.80 2.00 -6 -1 0 19.30 3.00 -6 1 0 19.10 3.30 6 1 0 17.40 2.00 -7 -1 0 39.00 4.60 7 -1 0 43.80 3.10 -7 1 0 44.70 5.10 7 1 0 40.20 2.80 8 -1 0 129.29 5.50 -8 -1 0 141.89 7.10 8 1 0 123.99 5.20 -8 1 0 137.79 7.90 9 -1 0 27.40 3.20 -9 -1 0 37.30 4.90 -9 1 0 33.80 5.00 9 1 0 25.90 3.30 10 -1 0 67.79 5.00 -10 -1 0 73.99 7.10 10 1 0 76.89 4.70 -10 1 0 65.69 7.80 11 -1 0 33.80 4.10 -11 -1 0 40.10 5.90 11 1 0 35.20 3.90 -11 1 0 36.90 6.60 -12 -1 0 16.30 6.20 12 -1 0 24.40 4.20 -12 1 0 21.00 6.60 12 1 0 16.60 3.80 0 2 0 556.44 12.90 1 -2 0 3.50 0.90 1 -2 0 4.80 0.80 -1 2 0 3.80 0.80 -1 2 0 3.90 0.70 1 2 0 4.80 0.70 2 -2 0 1117.99 25.70 2 2 0 1235.08 25.60 -2 2 0 1159.58 25.70 -2 2 0 1129.99 26.20 -3 -2 0 396.06 9.40 3 -2 0 372.86 9.50 3 2 0 406.16 10.10 -3 2 0 363.76 9.40 -3 2 0 366.86 9.90 -4 -2 0 643.84 14.80 4 -2 0 619.84 14.70 4 2 0 600.14 14.00 -4 2 0 605.44 14.90 -4 2 0 591.34 14.40 5 -2 0 5.40 1.30 -5 -2 0 7.40 1.70 5 2 0 6.40 1.20 -5 2 0 4.50 1.20 -5 2 0 4.80 1.10 -5 2 0 3.80 2.30 6 -2 0 205.58 6.70 -6 -2 0 217.48 7.20 6 2 0 205.88 6.30 -6 2 0 203.88 8.80 7 -2 0 32.90 3.00 -7 -2 0 37.40 4.00 -7 2 0 41.80 5.20 7 2 0 39.10 2.80 -8 -2 0 187.28 7.70 8 -2 0 183.08 6.80 8 2 0 186.38 6.50 -8 2 0 165.28 9.30 9 -2 0 22.60 3.10 -9 -2 0 23.60 4.20 9 2 0 23.60 2.90 -9 2 0 24.10 5.00 -10 -2 0 131.69 7.90 10 -2 0 135.59 6.70 -10 2 0 148.39 10.10 10 2 0 134.99 6.10 -11 -2 0 2.80 4.50 11 -2 0 3.80 3.00 -11 2 0 8.30 5.90 11 2 0 1.20 2.60 12 -2 0 192.28 9.30 12 2 0 196.98 8.50 -12 2 0 168.88 12.80 0 3 0 0.50 0.70 1 -3 0 124.89 4.10 -1 3 0 127.89 4.00 1 3 0 123.29 4.10 -1 3 0 127.39 4.60 2 -3 0 3524.25 74.79 -2 3 0 3416.76 74.69 -2 3 0 3484.75 75.59 3 -3 0 1330.27 29.80 -3 3 0 1321.07 30.60 3 3 0 1322.97 29.20 -3 3 0 1324.57 29.70 -4 -3 0 -0.10 1.10 4 -3 0 0.00 1.00 -4 3 0 0.00 1.00 4 3 0 1.00 0.90 -4 3 0 -0.70 1.10 -5 -3 0 77.59 3.60 5 -3 0 74.09 3.60 -5 3 0 68.39 3.30 5 3 0 72.79 3.10 -5 3 0 73.69 3.80 -5 3 0 66.59 5.30 6 -3 0 3.50 1.40 -6 -3 0 1.60 1.80 -6 3 0 3.40 1.50 6 3 0 3.80 1.20 -6 3 0 -0.70 2.90 -6 3 0 4.50 1.30 -7 -3 0 9.80 2.50 7 -3 0 8.10 1.80 -7 3 0 7.50 3.40 7 3 0 9.70 1.90 8 -3 0 106.39 5.40 -8 -3 0 115.59 6.00 8 3 0 109.59 5.00 -8 3 0 106.39 8.20 9 -3 0 1.40 2.20 -9 3 0 5.00 4.40 9 3 0 3.20 2.00 10 -3 0 0.70 2.60 -10 -3 0 3.60 5.50 -10 3 0 12.40 5.60 10 3 0 2.80 2.30 11 -3 0 584.34 17.40 11 3 0 573.84 16.10 -11 3 0 607.34 21.40 0 4 0 2593.84 57.09 1 -4 0 547.25 13.60 1 4 0 560.94 13.80 -1 4 0 552.34 13.40 -1 4 0 542.85 14.30 2 -4 0 378.66 10.20 -2 4 0 388.46 10.10 2 4 0 402.46 10.10 -2 4 0 368.86 10.90 3 -4 0 82.19 3.80 -3 4 0 88.09 4.40 -3 4 0 84.09 3.70 3 4 0 84.79 3.40 4 -4 0 317.27 9.20 -4 4 0 320.47 9.10 4 4 0 318.67 8.60 -4 4 0 329.87 10.10 5 -4 0 146.49 5.60 -5 4 0 142.49 5.40 -5 4 0 149.29 6.20 5 4 0 141.99 5.00 6 -4 0 4.30 1.60 6 4 0 6.80 1.50 -6 4 0 4.80 1.70 -6 4 0 5.30 1.70 -6 4 0 2.70 3.30 7 -4 0 114.29 5.50 -7 4 0 125.79 5.20 7 4 0 129.19 5.30 -7 4 0 126.09 8.40 -7 4 0 113.89 4.70 8 -4 0 21.40 3.10 8 4 0 24.80 2.90 -8 4 0 23.20 5.00 9 -4 0 24.10 3.60 9 4 0 35.10 3.90 -9 4 0 22.60 6.10 10 -4 0 100.99 6.70 10 4 0 103.19 5.70 -10 4 0 104.29 9.90 11 -4 0 5.80 3.40 -11 4 0 7.30 6.00 11 4 0 1.40 2.90 0 5 0 0.60 1.10 -1 5 0 1284.37 29.80 -1 5 0 1322.17 31.10 1 5 0 1315.77 30.50 2 -5 0 21.30 2.40 -2 5 0 22.50 2.80 -2 5 0 21.90 2.30 2 5 0 21.00 2.30 3 -5 0 76.69 4.00 -3 5 0 81.99 4.70 3 5 0 80.39 3.80 -3 5 0 80.39 4.00 4 -5 0 67.29 3.90 4 5 0 73.79 3.70 -4 5 0 72.09 4.50 -4 5 0 66.29 3.90 5 -5 0 24.20 3.00 5 5 0 27.30 2.60 -5 5 0 26.40 3.50 -5 5 0 24.50 3.00 6 -5 0 99.79 5.20 -6 5 0 99.39 7.60 -6 5 0 99.09 5.00 -6 5 0 116.69 6.00 6 5 0 103.09 4.80 7 -5 0 175.68 7.20 -7 5 0 176.08 10.10 -7 5 0 171.38 7.30 7 5 0 177.98 6.70 -7 5 0 172.68 6.60 8 -5 0 189.38 8.00 -8 5 0 186.18 6.40 8 5 0 187.18 7.30 -8 5 0 192.58 6.90 -8 5 0 183.98 11.00 9 -5 0 3.40 2.70 9 5 0 1.00 2.40 -9 5 0 2.50 5.10 10 -5 0 81.79 6.70 10 5 0 86.99 5.80 -10 5 0 76.39 9.90 11 -5 0 44.40 5.50 11 5 0 50.09 5.60 -11 5 0 45.10 8.60 0 6 0 307.77 9.10 0 6 0 315.67 10.10 -1 6 0 1.60 1.40 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140.89 9.00 7 8 0 130.69 7.20 -7 8 0 151.08 7.60 8 -8 0 56.29 6.50 -8 8 0 68.19 7.50 -8 8 0 64.19 6.20 8 8 0 62.59 5.90 -8 8 0 56.49 8.10 -9 8 0 75.49 7.90 -9 8 0 78.49 10.30 9 8 0 78.99 6.90 -9 8 0 79.29 6.50 10 -8 0 17.40 5.00 -10 8 0 22.40 8.00 10 8 0 30.20 5.20 -10 8 0 27.60 3.50 0 9 0 -0.20 1.80 0 9 0 -2.40 2.00 -1 9 0 280.97 9.70 -1 9 0 281.57 11.30 1 9 0 289.37 11.00 -2 9 0 312.77 12.30 -2 9 0 326.67 10.60 2 9 0 312.57 11.60 3 9 0 34.90 4.40 -3 9 0 37.60 4.20 -3 9 0 40.30 5.30 4 -9 0 58.79 5.30 -4 9 0 64.29 5.20 4 9 0 59.49 5.20 -4 9 0 61.69 6.40 5 -9 0 62.69 5.50 -5 9 0 58.79 5.30 5 9 0 73.69 5.60 -5 9 0 69.09 7.00 6 -9 0 288.37 11.30 6 9 0 294.67 11.20 -6 9 0 285.87 10.80 -6 9 0 274.17 12.70 7 -9 0 14.90 4.10 -7 9 0 13.60 4.60 -7 9 0 9.30 3.60 7 9 0 12.50 3.20 -8 9 0 -2.50 4.30 8 9 0 0.90 3.20 -8 9 0 5.90 3.60 -8 9 0 -0.40 5.80 9 -9 0 -4.80 3.90 -9 9 0 6.90 3.90 9 9 0 -8.10 3.60 -9 9 0 -2.50 6.20 -9 9 0 9.40 5.20 10 -9 0 0.00 4.60 -10 9 0 7.70 5.00 -10 9 0 9.90 4.40 10 9 0 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6.40 0 -5 9 285.67 9.60 0 -5 -9 274.97 12.40 0 5 9 279.57 11.50 0 5 -9 287.27 10.90 0 5 9 267.47 11.70 -1 -5 -9 26.20 5.10 1 -5 9 33.10 4.00 1 5 9 37.80 5.40 -1 5 -9 24.10 3.90 1 5 9 28.40 4.40 -2 -5 -9 13.00 4.00 2 -5 9 18.90 3.30 -2 5 -9 12.80 3.70 2 5 9 19.10 3.60 2 5 9 13.30 3.90 3 -5 9 -0.10 2.40 -3 -5 -9 -3.00 3.10 -3 5 -9 -1.80 2.90 3 5 9 2.10 3.00 3 5 9 -2.70 2.40 -4 -5 -9 499.35 17.70 4 -5 9 508.45 16.20 4 5 9 536.95 13.50 -4 5 -9 414.56 22.90 4 5 9 529.35 18.20 5 -5 9 158.28 8.90 -5 -5 -9 159.48 10.10 -5 5 -9 161.58 10.60 5 5 9 171.78 10.20 -6 -5 -9 220.28 11.10 6 -5 9 180.18 12.40 6 5 9 213.78 11.80 -6 5 -9 183.78 11.50 7 -5 9 163.38 9.90 -7 -5 -9 153.98 9.80 7 5 9 156.08 16.10 -7 5 -9 161.68 11.70 8 -5 9 49.30 6.40 -8 -5 -9 44.90 5.50 -8 5 -9 36.60 7.50 8 5 9 42.20 6.50 9 -5 9 199.18 12.70 9 5 9 191.38 13.30 -9 5 -9 196.98 13.50 -9 5 -9 195.48 14.40 10 -6 -9 80.79 9.40 -10 -6 9 84.19 10.60 -10 6 9 67.09 10.80 10 6 -9 75.59 5.30 -9 -6 9 33.60 6.60 9 -6 -9 19.20 6.30 -9 6 9 37.60 7.90 9 6 -9 34.40 4.50 -8 -6 9 -1.80 4.50 8 -6 -9 0.40 4.90 8 6 -9 6.30 2.40 -8 6 9 -3.70 5.30 -7 -6 9 162.88 10.60 7 -6 -9 175.38 11.50 -7 6 9 168.08 6.00 7 6 -9 163.38 6.90 -7 6 9 140.59 11.90 -7 6 9 159.48 6.70 6 -6 -9 258.07 15.20 -6 -6 9 275.37 13.20 -6 6 9 271.07 8.90 -6 6 9 281.67 15.40 6 6 -9 267.37 9.10 -6 6 9 265.97 10.20 5 -6 -9 192.68 11.10 -5 -6 9 194.78 10.90 -5 6 9 186.58 7.70 -5 6 9 175.68 11.40 -5 6 9 195.58 9.00 5 6 -9 200.58 7.70 4 -6 -9 13.00 3.80 4 6 -9 6.50 2.50 -4 6 9 13.60 3.60 -4 6 9 8.70 5.10 -3 -6 9 37.10 2.90 3 -6 -9 32.80 5.10 -3 6 9 31.50 4.30 -3 6 9 30.20 5.80 3 6 -9 35.20 4.30 2 -6 -9 268.77 12.30 -2 -6 9 253.57 8.30 2 6 -9 244.78 9.60 -2 6 9 243.28 11.20 -2 6 9 243.48 12.10 -1 -6 9 88.79 4.90 1 -6 -9 75.99 7.30 1 6 -9 87.89 6.20 -1 6 9 91.49 7.40 -1 6 9 87.69 7.40 0 -6 -9 140.89 9.20 0 -6 9 137.59 6.50 0 6 9 141.09 8.50 0 6 9 136.49 8.70 0 6 -9 130.79 7.50 -1 -6 -9 58.29 7.10 1 -6 9 68.59 5.10 -1 6 -9 64.39 6.20 1 6 9 59.79 6.00 1 6 9 64.09 6.90 2 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7.80 5 -7 -9 109.19 9.60 -5 7 9 110.99 7.90 -5 7 9 110.49 10.20 5 7 -9 100.19 5.90 -5 7 9 107.19 6.30 -4 7 9 253.77 11.50 4 7 -9 251.37 9.40 -4 7 9 257.77 14.10 3 -7 -9 254.67 12.70 3 7 -9 225.58 9.00 -3 7 9 216.58 12.40 -3 7 9 242.48 11.50 -2 -7 9 411.16 11.90 2 -7 -9 390.46 16.10 -2 7 9 421.66 15.80 2 7 -9 429.46 13.40 -2 7 9 391.86 16.30 1 -7 -9 202.68 11.10 -1 -7 9 198.28 7.70 -1 7 9 190.18 10.60 1 7 -9 192.18 8.80 -1 7 9 219.38 11.10 0 -7 -9 20.60 5.20 0 -7 9 25.50 3.40 0 7 -9 25.60 4.20 0 7 9 23.20 5.10 0 7 9 17.00 4.80 1 -7 9 -1.00 2.10 -1 -7 -9 -0.40 3.20 1 7 9 -2.40 2.90 1 7 9 -4.50 3.40 -1 7 -9 0.20 2.80 2 -7 9 47.60 5.10 -2 -7 -9 56.99 7.30 -2 7 -9 58.79 7.50 2 7 9 53.19 5.80 2 7 9 60.59 7.20 -3 -7 -9 26.40 5.00 3 -7 9 32.90 4.50 -3 7 -9 24.00 4.50 3 7 9 39.30 5.50 3 7 9 37.90 5.00 4 -7 9 26.70 4.40 -4 -7 -9 37.60 6.30 4 7 9 42.00 6.10 4 7 9 40.70 4.50 -4 7 -9 44.50 6.40 -5 -7 -9 156.68 10.50 5 -7 9 152.08 9.20 5 7 9 172.38 11.20 -5 7 -9 149.59 10.60 6 -7 9 12.00 4.40 -6 -7 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6.80 0 8 9 40.10 5.70 0 8 -9 40.30 5.60 -1 -8 -9 28.90 7.40 1 -8 9 9.40 2.80 1 8 9 10.00 4.10 -1 8 -9 12.10 4.20 1 8 9 14.00 4.40 2 -8 9 18.20 3.60 -2 -8 -9 13.40 4.70 -2 8 -9 19.30 4.60 2 8 9 7.70 4.20 2 8 9 25.60 4.50 -3 -8 -9 48.30 6.90 3 -8 9 44.20 5.80 3 8 9 51.69 7.30 -3 8 -9 52.39 6.50 3 8 9 58.29 5.80 -4 -8 -9 113.49 9.60 4 8 9 132.59 10.40 4 8 9 138.99 6.80 -4 8 -9 136.99 10.00 5 -8 9 132.39 8.90 -5 -8 -9 124.09 9.80 -5 8 -9 133.29 16.20 5 8 9 138.29 11.50 -6 -8 -9 304.97 13.70 6 -8 9 327.77 13.80 6 8 9 300.97 15.70 -7 -8 -9 21.50 4.80 7 -8 9 9.80 5.10 -7 8 -9 7.70 7.70 7 8 9 14.20 6.10 8 -8 9 176.18 12.40 -8 -8 -9 185.58 8.60 -8 8 -9 195.98 14.80 8 8 9 203.98 14.60 9 -9 -9 12.40 7.70 -9 9 9 9.30 6.70 8 -9 -9 102.09 13.00 -8 9 9 123.59 6.90 -8 9 9 112.29 12.80 -8 9 9 101.09 8.30 8 9 -9 117.49 6.90 7 -9 -9 30.90 7.10 -7 9 9 36.10 4.60 -7 9 9 35.60 9.00 -7 9 9 32.50 5.60 7 9 -9 38.70 4.20 6 -9 -9 35.30 7.60 -6 9 9 37.90 4.70 -6 9 9 33.70 8.30 6 9 -9 42.30 5.20 -6 9 9 39.20 6.20 5 -9 -9 29.70 6.80 -5 9 9 39.80 6.00 -5 9 9 36.20 4.80 5 9 -9 32.30 4.20 -5 9 9 34.00 7.80 4 -9 -9 92.49 9.60 4 9 -9 92.79 6.40 -4 9 9 100.69 9.40 -4 9 9 79.89 9.60 3 -9 -9 836.62 26.60 3 9 -9 838.82 22.40 -3 9 9 818.42 26.10 -3 9 9 776.52 27.10 2 -9 -9 21.20 5.90 -2 -9 9 30.00 3.60 -2 9 9 39.30 7.10 -2 9 9 32.10 6.60 2 9 -9 25.80 4.20 -1 -9 9 224.38 8.70 1 -9 -9 211.08 12.40 1 9 -9 173.78 11.60 -1 9 9 204.78 12.00 -1 9 9 210.78 12.30 0 -9 -9 79.49 8.60 0 -9 9 75.59 5.90 0 9 9 69.89 8.00 0 9 -9 74.09 6.90 0 9 9 75.59 8.80 1 -9 9 1.10 2.60 -1 -9 -9 -3.40 3.90 1 9 9 7.40 4.10 -1 9 -9 -3.40 3.00 1 9 9 7.50 4.80 -2 -9 -9 21.80 5.40 2 -9 9 31.40 4.80 2 9 9 24.10 5.00 2 9 9 30.80 6.40 3 -9 9 77.39 7.30 -3 -9 -9 85.79 10.20 3 9 9 70.09 9.10 -3 9 -9 73.29 11.10 3 9 9 72.89 6.70 4 -9 9 114.59 8.40 -4 -9 -9 117.09 15.90 4 9 9 69.39 12.30 4 9 9 121.99 6.90 -5 -9 -9 156.28 10.70 5 -9 9 134.59 9.60 5 9 9 161.68 12.20 5 9 9 143.89 5.40 6 -9 9 8.70 4.90 -6 -9 -9 9.30 5.20 6 9 9 7.70 6.30 -6 9 -9 1.30 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3.30 4 -8 -10 15.70 5.20 -4 8 10 26.10 6.80 4 8 -10 24.00 4.00 -4 8 10 25.20 5.30 3 -8 -10 209.98 12.90 -3 8 10 215.58 11.80 -3 8 10 208.98 13.00 3 8 -10 230.78 9.80 -2 -8 10 430.16 12.80 2 -8 -10 432.56 17.90 -2 8 10 416.86 17.70 -2 8 10 425.56 17.10 2 8 -10 417.86 14.50 -1 -8 10 41.70 4.60 1 -8 -10 36.40 6.10 1 8 -10 43.40 5.50 -1 8 10 53.19 7.70 -1 8 10 37.10 5.90 0 -8 10 13.00 3.40 0 -8 -10 8.40 4.20 0 8 -10 16.80 4.40 0 8 10 9.80 4.70 0 8 10 10.70 4.70 -1 -8 -10 -0.10 4.50 1 -8 10 -0.10 2.30 -1 8 -10 -2.80 3.50 1 8 10 9.00 4.80 1 8 10 1.30 3.80 -2 -8 -10 4.90 4.50 2 -8 10 5.00 2.90 2 8 10 -0.10 3.90 2 8 10 2.30 3.90 -3 -8 -10 15.10 5.50 3 -8 10 9.80 5.50 3 8 10 17.30 4.10 -3 8 -10 4.40 5.30 3 8 10 15.00 5.40 -4 -8 -10 346.87 16.00 4 -8 10 360.86 14.00 4 8 10 337.67 17.60 4 8 10 351.26 11.50 -5 -8 -10 29.00 9.30 5 -8 10 29.50 5.40 5 8 10 24.90 6.50 6 -8 10 62.29 8.40 -6 -8 -10 53.19 7.30 6 8 10 45.70 7.80 -7 -8 -10 106.49 10.30 7 -8 10 102.89 10.20 -7 8 -10 100.69 13.40 7 8 10 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2 9 10 254.37 11.70 3 -9 10 38.90 5.70 -3 -9 -10 28.90 6.40 3 9 10 46.60 7.70 3 9 10 37.70 5.40 4 -9 10 -3.20 4.00 -4 -9 -10 -3.00 5.10 -4 9 -10 3.20 5.10 4 9 10 1.50 3.60 4 9 10 1.00 5.40 5 -9 10 98.69 9.10 -5 -9 -10 114.19 11.00 5 9 10 96.99 4.80 -5 9 -10 102.39 11.70 5 9 10 89.89 11.40 -6 -9 -10 58.59 9.80 6 -9 10 47.20 6.80 6 9 10 57.89 9.50 -6 9 -10 41.10 8.70 -7 -9 -10 97.39 10.70 7 -9 10 69.99 8.60 -7 9 -10 116.09 14.30 7 9 10 109.69 13.10 8 -10 -10 -0.40 7.80 -8 10 10 2.50 4.30 8 10 -10 5.90 3.90 -8 10 10 -3.90 5.30 -8 10 10 2.80 6.80 7 -10 -10 7.00 7.00 -7 10 10 -0.90 5.20 7 10 -10 10.30 4.10 -7 10 10 -7.60 6.80 -7 10 10 2.20 4.50 6 -10 -10 -3.30 6.50 -6 10 10 7.90 4.20 -6 10 10 -4.00 6.00 -6 10 10 -5.30 5.20 5 -10 -10 1.20 6.90 5 10 -10 13.30 3.90 -5 10 10 6.80 4.30 -5 10 10 11.50 5.70 -5 10 10 1.90 6.50 4 -10 -10 0.90 5.30 -4 10 10 -0.90 3.90 4 10 -10 4.90 3.40 -4 10 10 3.30 5.10 -4 10 10 -6.00 5.50 -3 10 10 15.20 6.70 -3 10 10 19.50 5.80 3 10 -10 24.10 4.40 2 10 -10 533.85 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7.90 9 -6 -12 -1.40 7.10 -9 -6 12 14.30 6.90 -9 6 12 -2.80 6.50 9 6 -12 6.10 4.60 -8 -6 12 13.40 6.00 8 -6 -12 5.10 6.60 8 6 -12 15.10 4.40 -8 6 12 5.20 6.50 -7 -6 12 0.10 5.60 7 -6 -12 6.20 6.20 -7 6 12 1.50 2.50 -7 6 12 2.10 6.30 7 6 -12 -4.30 3.50 -7 6 12 -4.80 2.70 6 -6 -12 59.39 8.40 -6 -6 12 49.60 8.10 -6 6 12 46.70 8.50 -6 6 12 57.19 6.30 6 6 -12 49.80 5.70 -6 6 12 53.59 5.70 5 -6 -12 16.50 5.70 -5 -6 12 5.20 4.90 5 6 -12 17.30 4.10 -5 6 12 4.70 3.80 -5 6 12 4.10 5.90 4 -6 -12 6.40 5.60 -4 6 12 9.10 3.90 4 6 -12 -3.80 3.40 -4 6 12 5.10 5.50 -3 -6 12 0.20 1.90 3 -6 -12 -3.10 4.20 -3 6 12 2.40 5.30 -3 6 12 2.00 3.70 2 -6 -12 79.79 9.30 -2 -6 12 79.49 5.30 -2 6 12 71.69 7.90 2 6 -12 82.89 7.90 -2 6 12 68.29 8.50 -1 -6 12 138.39 7.00 -1 6 12 112.19 9.30 1 6 -12 130.29 9.10 -1 6 12 125.69 9.50 0 -6 12 11.10 3.20 0 6 -12 10.50 3.90 0 6 12 15.40 4.70 0 6 12 18.50 4.90 -1 -6 -12 110.59 10.70 1 -6 12 116.79 7.50 1 6 12 108.19 8.40 1 6 12 115.79 9.80 -2 -6 -12 0.90 4.80 2 -6 12 1.40 3.20 2 6 12 -0.20 3.60 3 -6 12 -1.50 3.20 -3 -6 -12 1.80 4.70 3 6 12 0.70 4.30 3 6 12 -1.80 3.50 4 -6 12 27.10 5.10 -4 -6 -12 25.00 6.60 4 6 12 32.10 6.90 4 6 12 22.20 4.10 -4 6 -12 1.70 7.70 -5 -6 -12 7.30 5.80 5 -6 12 -2.20 4.10 5 6 12 4.00 6.10 -5 6 -12 8.70 6.50 6 -6 12 15.20 5.40 -6 -6 -12 33.60 7.50 6 6 12 11.80 6.50 -6 6 -12 13.40 7.20 -7 -6 -12 -7.40 7.20 7 -6 12 -10.40 5.50 7 6 12 10.80 7.10 -7 6 -12 -10.60 7.60 9 -7 -12 0.60 8.50 -9 7 12 2.70 7.00 9 7 -12 9.10 5.00 8 -7 -12 3.30 7.30 8 7 -12 9.70 4.20 7 -7 -12 8.80 7.00 -7 7 12 6.60 3.10 7 7 -12 11.20 4.40 -7 7 12 3.60 6.50 -7 7 12 8.10 3.50 6 -7 -12 305.57 16.60 6 7 -12 292.27 12.20 -6 7 12 272.77 16.80 -6 7 12 280.57 12.20 -6 7 12 276.57 10.80 5 -7 -12 52.19 8.40 -5 7 12 32.40 5.40 -5 7 12 20.90 6.80 4 -7 -12 5.00 5.50 -4 7 12 4.80 4.20 4 7 -12 2.80 3.70 -4 7 12 0.80 5.60 -3 -7 12 174.88 7.10 3 -7 -12 178.98 12.60 3 7 -12 196.08 10.30 -3 7 12 179.08 12.50 -3 7 12 183.28 11.20 -2 -7 12 16.10 3.10 2 -7 -12 17.30 5.60 -2 7 12 16.60 6.00 -2 7 12 14.50 4.90 2 7 -12 4.20 4.00 -1 -7 12 75.29 5.90 -1 7 12 66.39 8.40 1 7 -12 53.99 6.50 -1 7 12 64.39 7.70 0 -7 12 4.60 3.00 0 7 12 -2.80 3.80 0 7 12 3.60 4.60 0 7 -12 -7.90 3.80 -1 -7 -12 3.40 5.60 1 -7 12 -0.40 2.90 1 7 12 -6.80 3.90 -2 -7 -12 46.90 7.20 2 -7 12 56.59 9.60 2 7 12 70.79 9.40 2 7 12 56.69 7.40 -3 -7 -12 -4.80 4.90 3 -7 12 3.50 4.00 3 7 12 2.30 4.00 -3 7 -12 2.60 5.40 3 7 12 3.10 5.20 4 -7 12 14.00 4.80 -4 -7 -12 1.80 5.60 4 7 12 5.90 5.30 4 7 12 2.50 3.60 -4 7 -12 14.00 6.00 -5 -7 -12 31.20 7.10 5 -7 12 17.50 4.90 -5 7 -12 16.90 7.30 5 7 12 16.30 6.80 -6 -7 -12 30.60 7.80 6 -7 12 17.90 5.80 6 7 12 24.60 7.40 -6 7 -12 32.70 9.10 7 -7 12 24.50 6.30 -7 -7 -12 17.00 7.60 7 7 12 21.20 8.10 -7 7 -12 35.80 9.60 8 -8 -12 37.00 9.10 -8 8 12 38.00 4.00 -8 8 12 36.70 4.40 8 8 -12 38.50 6.90 -8 8 12 30.40 8.60 7 -8 -12 15.70 7.70 -7 8 12 16.60 7.90 -7 8 12 19.40 4.00 -7 8 12 24.20 4.90 6 -8 -12 7.40 6.90 -6 8 12 9.30 4.80 -6 8 12 4.10 4.00 -6 8 12 10.30 6.50 6 8 -12 3.00 4.30 5 -8 -12 6.60 6.40 5 8 -12 8.60 3.90 -5 8 12 12.80 4.50 -5 8 12 12.30 6.40 -5 8 12 2.40 4.60 4 -8 -12 28.40 7.00 -4 8 12 34.20 6.10 4 8 -12 31.10 5.10 -4 8 12 23.90 7.30 -3 -8 12 323.67 10.60 3 -8 -12 353.76 17.30 -3 8 12 319.17 16.70 -3 8 12 347.17 15.70 3 8 -12 328.77 13.50 -2 -8 12 -1.20 2.50 -2 8 12 2.50 5.70 2 8 -12 -1.00 4.00 -2 8 12 -3.30 4.40 -1 -8 12 103.19 6.70 1 8 -12 98.39 8.90 -1 8 12 100.79 9.70 0 -8 12 -0.40 3.00 0 8 -12 7.30 4.10 0 8 12 -6.40 4.50 0 8 12 4.60 4.60 1 -8 12 -2.00 3.30 1 8 12 -0.20 5.20 -1 8 -12 -4.80 6.60 1 8 12 -3.60 4.50 2 -8 12 234.48 11.30 2 8 12 246.58 14.70 2 8 12 238.68 11.60 3 -8 12 7.50 4.00 3 8 12 7.90 4.30 -3 8 -12 6.90 5.70 3 8 12 18.00 6.40 4 -8 12 -2.60 4.60 -4 8 -12 2.30 6.10 4 8 12 12.50 5.90 4 8 12 -1.70 3.70 5 -8 12 33.70 6.20 -5 -8 -12 31.60 8.70 5 8 12 48.00 8.00 -5 8 -12 24.50 8.00 6 -8 12 3.50 5.40 -6 -8 -12 -11.10 6.80 6 8 12 -2.50 6.80 -6 8 -12 10.90 8.60 8 -9 -12 45.80 10.70 -8 9 12 35.10 9.30 -8 9 12 49.30 5.90 8 9 -12 44.90 6.00 -8 9 12 56.49 6.70 7 -9 -12 44.50 9.70 -7 9 12 41.50 9.80 -7 9 12 34.40 6.40 -7 9 12 39.80 5.20 7 9 -12 36.50 5.70 6 -9 -12 16.70 7.70 -6 9 12 10.30 7.00 6 9 -12 -0.70 4.40 -6 9 12 5.60 4.60 -6 9 12 1.20 5.10 5 -9 -12 94.69 12.90 -5 9 12 106.09 9.00 -5 9 12 123.49 11.30 -5 9 12 100.39 11.50 5 9 -12 118.29 9.10 4 -9 -12 31.50 7.60 -4 9 12 29.30 7.50 -4 9 12 17.70 6.50 4 9 -12 33.30 5.60 3 -9 -12 7.50 6.80 -3 9 12 1.30 6.40 -3 9 12 0.90 5.80 3 9 -12 6.10 4.30 -2 -9 12 110.79 6.90 2 9 -12 124.69 9.50 -2 9 12 145.99 12.10 -2 9 12 109.29 10.70 -1 -9 12 70.29 6.30 1 9 -12 80.39 8.70 -1 9 12 83.19 11.00 -1 9 12 66.89 9.30 0 -9 12 180.18 9.40 0 9 -12 184.78 11.70 0 9 12 180.18 11.90 0 9 12 207.28 13.80 1 -9 12 87.29 7.70 1 9 12 79.09 8.80 -1 9 -12 90.29 10.10 1 9 12 86.29 11.10 2 -9 12 9.70 4.10 2 9 12 0.60 4.80 2 9 12 4.80 5.70 3 -9 12 7.30 4.50 3 9 12 15.10 4.90 3 9 12 6.50 6.20 -3 9 -12 13.40 6.40 4 -9 12 -0.40 5.10 4 9 12 -1.10 4.10 -4 9 -12 -2.00 6.30 4 9 12 -1.60 6.10 5 -9 12 10.00 6.10 5 9 12 4.50 6.70 -5 9 -12 28.30 8.60 6 -9 12 8.10 6.20 -6 -9 -12 11.50 8.20 -6 9 -12 6.50 8.90 6 9 12 5.70 7.80 7 -10 -12 12.20 9.80 -7 10 12 2.10 6.90 7 10 -12 1.70 4.90 -7 10 12 -1.70 5.00 -7 10 12 6.80 6.20 6 -10 -12 155.68 16.40 -6 10 12 157.28 10.20 -6 10 12 145.29 15.30 6 10 -12 137.89 10.30 5 -10 -12 -1.80 6.90 -5 10 12 2.60 6.70 -5 10 12 7.20 6.60 5 10 -12 2.30 4.50 -5 10 12 3.30 4.70 4 -10 -12 426.76 20.90 -4 10 12 422.56 20.80 4 10 -12 411.36 16.20 -4 10 12 451.25 19.50 3 -10 -12 168.88 14.90 -3 10 12 192.48 14.30 3 10 -12 183.38 11.10 -3 10 12 203.38 14.20 -2 -10 12 3.00 3.20 -2 10 12 -3.00 5.70 2 10 -12 -1.70 4.40 -2 10 12 -3.30 6.20 1 -10 -12 138.49 15.40 -1 -10 12 150.28 8.60 -1 10 12 130.19 11.50 1 10 -12 157.88 11.10 -1 10 12 157.08 13.60 0 -10 12 -1.20 3.50 0 -10 -12 4.60 6.30 0 10 -12 0.70 4.80 0 10 12 -2.30 5.70 0 10 12 -0.10 5.10 1 -10 12 6.80 3.90 -1 -10 -12 -0.90 6.60 -1 10 -12 0.80 5.50 1 10 12 8.60 6.50 1 10 12 1.00 5.30 2 -10 12 54.89 6.70 2 10 12 68.59 8.70 2 10 12 75.29 9.60 -3 -10 -12 19.60 7.70 3 -10 12 2.30 4.70 3 10 12 14.50 5.20 3 10 12 10.90 7.30 -3 10 -12 1.70 6.60 4 -10 12 -6.10 4.50 -4 -10 -12 -6.50 6.90 4 10 12 -1.40 4.50 -4 10 -12 8.70 7.60 4 10 12 -4.10 7.10 5 -10 12 27.00 6.20 5 10 12 8.30 7.70 -5 10 -12 17.60 9.90 6 -11 -12 -7.60 9.70 -6 11 12 0.40 6.90 -6 11 12 3.50 7.30 6 11 -12 10.90 5.20 5 -11 -12 69.49 11.90 -5 11 12 54.29 10.80 5 11 -12 92.09 9.50 -5 11 12 60.09 9.20 4 -11 -12 163.68 15.70 -4 11 12 153.28 14.30 -4 11 12 150.88 14.30 4 11 -12 158.18 11.10 3 -11 -12 78.59 10.20 -3 11 12 88.29 10.70 -3 11 12 94.49 11.90 3 11 -12 119.39 10.20 2 -11 -12 101.79 13.50 2 11 -12 121.09 10.60 -2 11 12 103.29 13.00 -2 11 12 109.59 11.90 -1 -11 12 257.27 11.40 1 -11 -12 255.37 16.70 1 11 -12 259.47 14.30 -1 11 12 283.07 17.20 -1 11 12 245.68 15.20 0 -11 -12 174.18 14.70 0 -11 12 162.18 9.90 0 11 -12 160.78 12.50 0 11 12 175.78 12.10 0 11 12 148.69 14.70 1 -11 12 114.89 9.30 -1 -11 -12 134.09 13.90 -1 11 -12 89.79 11.40 1 11 12 134.69 14.20 1 11 12 127.99 11.10 2 -11 12 29.30 5.70 -2 -11 -12 36.10 8.00 2 11 12 42.10 9.90 -2 11 -12 25.90 7.80 2 11 12 39.70 7.30 3 -11 12 20.50 5.70 -3 -11 -12 -0.30 7.70 3 11 12 8.30 7.90 3 11 12 20.10 5.90 -3 11 -12 14.90 8.40 -4 -11 -12 5.50 8.30 4 -11 12 16.00 6.10 4 11 12 4.00 8.10 -4 11 -12 7.30 8.40 4 11 12 14.10 5.20 -5 -11 -12 -1.50 8.10 5 -11 12 5.60 6.70 -5 11 -12 21.30 10.20 5 11 12 3.60 7.80 5 -12 -12 -8.60 9.20 -5 12 12 0.60 7.60 -5 12 12 2.10 6.80 -5 12 12 -11.00 6.00 5 12 -12 12.30 5.70 4 -12 -12 -4.20 8.50 4 12 -12 5.90 5.50 -4 12 12 5.30 7.10 -4 12 12 -1.60 5.90 -4 12 12 -6.50 7.70 3 -12 -12 294.07 19.90 -3 12 12 295.17 18.10 3 12 -12 309.57 15.00 -3 12 12 308.07 19.00 2 -12 -12 -14.20 7.50 -2 12 12 -5.20 6.10 2 12 -12 -1.90 5.40 -2 12 12 1.00 7.30 -1 -12 12 18.20 5.80 1 -12 -12 18.80 8.80 1 12 -12 10.30 5.80 -1 12 12 35.00 9.10 -1 12 12 18.90 7.20 0 -12 12 25.10 5.30 0 -12 -12 38.00 9.80 0 12 -12 36.50 7.80 0 12 12 17.20 7.10 0 12 12 4.70 7.80 1 -12 12 7.60 4.60 -1 -12 -12 7.30 8.40 -1 12 -12 11.20 6.80 1 12 12 0.00 5.60 1 12 12 -4.10 7.10 -2 -12 -12 219.08 17.50 2 -12 12 236.28 13.10 2 12 12 227.48 17.80 -2 12 -12 197.68 16.30 2 12 12 223.88 13.30 -3 -12 -12 22.40 8.60 3 -12 12 14.90 6.30 -3 12 -12 22.00 8.20 3 12 12 12.00 9.20 3 12 12 13.30 6.30 -4 -12 -12 7.40 8.30 4 -12 12 -8.70 5.90 4 12 12 -1.10 8.50 4 12 12 6.40 5.60 4 13 -12 6.60 6.20 -4 13 12 -2.90 8.60 -4 13 12 7.00 6.70 -4 13 12 0.40 7.50 3 -13 -12 -4.20 9.10 -3 13 12 0.40 7.30 3 13 -12 1.50 5.80 -3 13 12 0.60 9.00 2 -13 -12 238.88 19.60 -2 13 12 276.37 19.60 2 13 -12 283.27 15.20 -2 13 12 267.37 17.10 1 -13 -12 11.40 8.80 -1 13 12 6.10 7.10 1 13 -12 23.80 7.20 -1 13 12 23.00 8.80 0 -13 -12 90.89 11.90 0 -13 12 106.49 10.10 0 13 -12 112.39 14.00 0 13 12 103.09 12.30 0 13 12 132.99 16.90 1 -13 12 63.69 7.80 -1 -13 -12 37.00 9.20 1 13 12 74.49 9.80 1 13 12 50.59 10.40 -1 13 -12 45.80 8.60 -2 -13 -12 -0.60 8.80 2 -13 12 -5.60 5.10 2 13 12 -5.00 9.10 2 13 12 -11.50 6.00 -3 -13 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52.69 8.90 7 2 -14 64.99 7.80 -7 2 14 59.99 9.80 6 -2 -14 19.50 6.60 -6 -2 14 22.60 6.70 6 2 -14 22.10 5.80 -6 2 14 29.50 3.50 -6 2 14 32.00 3.70 -6 2 14 26.70 7.10 -5 -2 14 206.88 13.80 5 -2 -14 190.58 13.00 -5 -2 14 213.38 6.40 -5 2 14 203.48 13.60 5 2 -14 206.28 12.10 -5 2 14 218.48 8.30 -4 -2 14 0.90 2.10 -4 -2 14 -2.50 4.80 4 -2 -14 -3.80 4.70 -4 2 14 -4.10 4.60 4 2 -14 4.00 4.50 -4 2 14 3.00 2.90 3 -2 -14 174.68 12.30 -3 -2 14 153.08 11.20 -3 -2 14 186.38 7.90 -3 2 14 164.98 8.80 3 2 -14 173.68 11.40 -3 2 14 166.18 11.80 2 -2 -14 239.28 13.80 -2 -2 14 244.08 9.80 -2 -2 14 230.38 13.00 2 2 -14 235.88 13.10 -2 2 14 228.08 12.90 -2 2 14 243.18 11.00 1 -2 -14 23.80 5.90 -1 -2 14 14.70 4.90 -1 -2 14 22.90 4.30 -1 2 14 23.10 4.90 -1 2 14 15.60 5.30 1 2 -14 23.10 5.40 0 -2 14 15.90 3.80 0 -2 14 18.80 5.30 0 2 14 23.80 5.80 0 2 -14 29.80 6.00 0 2 14 17.60 4.90 1 -2 14 387.06 14.90 1 2 14 358.26 15.00 2 -2 14 6.80 4.10 2 2 14 1.00 4.10 2 2 14 5.20 4.20 3 -2 14 47.80 6.50 3 2 14 56.79 7.90 4 -2 14 97.79 9.30 4 2 14 75.69 8.70 -4 2 -14 66.49 10.20 5 -2 14 74.09 9.00 -5 2 -14 74.19 10.70 5 2 14 82.99 10.90 6 -2 14 11.70 5.50 -6 -2 -14 27.20 9.20 6 2 14 24.20 6.90 -6 2 -14 2.70 8.90 -7 -2 -14 40.30 10.70 7 -2 14 51.89 7.90 -7 2 -14 53.69 11.20 7 2 14 52.59 8.50 9 -3 -14 -7.80 8.20 9 3 -14 -1.90 6.10 -8 -3 14 31.70 8.70 8 -3 -14 32.60 7.80 8 3 -14 41.20 6.90 -8 3 14 24.00 9.40 7 -3 -14 4.00 6.20 -7 -3 14 0.60 5.50 -7 3 14 -4.00 6.10 7 3 -14 14.40 5.30 -6 -3 14 126.59 11.60 6 -3 -14 141.79 12.40 -6 3 14 132.39 6.20 6 3 -14 128.19 10.10 -6 3 14 139.79 12.40 -6 3 14 127.69 6.00 -5 -3 14 20.80 6.50 5 -3 -14 29.80 7.30 -5 3 14 26.10 7.30 5 3 -14 27.60 5.80 -5 3 14 31.00 4.00 -4 -3 14 36.90 7.20 4 -3 -14 26.00 6.50 -4 -3 14 33.20 3.90 -4 3 14 24.00 6.60 -4 3 14 41.30 5.10 4 3 -14 40.70 6.40 3 -3 -14 36.10 6.50 -3 -3 14 44.00 4.80 -3 -3 14 39.70 7.50 3 3 -14 37.70 6.10 -3 3 14 39.20 5.10 -3 3 14 37.80 7.50 -2 -3 14 230.08 9.30 -2 -3 14 213.28 12.80 2 -3 -14 233.58 13.90 -2 3 14 229.18 11.20 2 3 -14 228.28 12.80 -2 3 14 204.18 12.50 -1 -3 14 -0.60 2.90 -1 -3 14 1.70 4.30 1 -3 -14 9.90 5.30 1 3 -14 -2.50 4.20 -1 3 14 -4.80 4.10 -1 3 14 -1.00 3.50 0 -3 14 44.50 6.00 0 3 14 36.20 6.30 0 3 -14 26.90 5.80 0 3 14 44.00 6.60 1 -3 14 25.60 5.60 1 3 14 15.20 4.60 1 3 14 28.80 6.00 2 -3 14 21.10 4.70 2 3 14 21.50 5.00 2 3 14 20.20 5.20 3 -3 14 7.00 4.80 -3 3 -14 -5.90 6.30 3 3 14 -3.20 3.80 3 3 14 2.70 4.60 4 -3 14 101.19 9.50 -4 3 -14 88.19 10.40 4 3 14 104.69 10.90 5 -3 14 121.59 10.60 -5 -3 -14 95.59 12.20 5 3 14 118.29 12.00 -5 3 -14 111.89 14.60 6 -3 14 194.08 13.20 -6 -3 -14 217.38 17.40 -6 3 -14 204.78 17.90 6 3 14 197.48 14.90 8 -4 -14 11.10 7.70 8 4 -14 1.50 5.40 -8 4 14 7.60 7.20 7 -4 -14 13.90 7.20 -7 -4 14 9.40 6.30 -7 4 14 13.90 7.50 7 4 -14 14.80 5.20 -6 -4 14 60.69 9.60 6 -4 -14 69.19 9.50 -6 4 14 63.69 5.70 6 4 -14 68.49 8.70 -6 4 14 60.99 5.50 -6 4 14 59.59 10.30 -5 -4 14 172.28 12.70 5 -4 -14 160.18 13.30 -5 4 14 159.28 12.80 5 4 -14 163.98 11.10 -5 4 14 175.48 8.80 -4 -4 14 79.19 4.80 4 -4 -14 105.09 11.30 -4 -4 14 60.59 8.60 -4 4 14 73.99 7.40 -4 4 14 74.89 10.10 4 4 -14 83.89 9.10 -3 -4 14 -5.60 4.00 3 -4 -14 0.40 4.80 -3 -4 14 0.90 2.30 3 4 -14 -8.30 4.10 -3 4 14 3.70 3.40 -3 4 14 3.00 4.90 2 -4 -14 15.20 6.10 -2 -4 14 16.70 3.50 -2 -4 14 6.30 4.90 2 4 -14 10.70 5.30 -2 4 14 15.10 6.10 -2 4 14 13.60 4.40 -1 -4 14 55.09 5.80 -1 4 14 46.10 7.00 1 4 -14 74.39 9.00 -1 4 14 61.29 8.00 0 -4 14 103.19 7.50 0 4 14 78.29 14.20 0 4 -14 77.99 9.60 0 4 14 71.99 8.30 1 4 14 -2.30 3.90 1 4 14 0.70 4.20 2 -4 14 5.60 4.00 2 4 14 13.70 5.10 2 4 14 10.70 4.70 3 -4 14 24.00 5.30 -3 4 -14 23.40 7.40 3 4 14 17.50 5.40 3 4 14 14.10 4.70 4 -4 14 5.70 4.90 -4 -4 -14 -3.00 6.70 -4 4 -14 21.20 6.90 4 4 14 4.50 5.60 5 -4 14 184.78 12.20 -5 -4 -14 178.68 16.30 -5 4 -14 157.98 16.20 5 4 14 216.18 14.20 6 -4 14 28.60 6.30 -6 -4 -14 17.50 9.00 -6 4 -14 36.70 10.00 6 4 14 34.60 8.10 -8 -5 14 71.89 12.40 8 -5 -14 66.49 10.20 8 5 -14 74.79 10.00 -8 5 14 66.69 11.00 -7 -5 14 4.80 5.80 7 -5 -14 10.90 7.30 7 5 -14 7.40 5.40 -7 5 14 5.50 2.60 -7 5 14 10.70 8.30 -7 5 14 7.40 2.70 -6 -5 14 4.20 5.40 6 -5 -14 4.30 6.60 -6 5 14 5.60 3.40 -6 5 14 6.70 6.80 6 5 -14 4.30 5.10 -6 5 14 7.10 3.70 -5 -5 14 11.30 5.80 5 -5 -14 19.70 6.70 -5 5 14 4.40 6.00 -5 5 14 3.80 3.90 5 5 -14 15.90 5.40 -4 -5 14 68.29 4.50 4 -5 -14 60.99 8.40 -4 -5 14 62.19 8.70 -4 5 14 62.89 9.60 -4 5 14 67.99 7.90 4 5 -14 71.19 8.90 -3 -5 14 47.30 4.90 3 -5 -14 46.50 8.70 -3 -5 14 54.39 8.10 -3 5 14 53.29 6.70 3 5 -14 49.90 6.70 -3 5 14 47.00 7.70 2 -5 -14 39.70 7.30 -2 -5 14 41.70 5.10 -2 5 14 44.70 6.30 2 5 -14 40.40 6.50 -2 5 14 38.10 6.90 -1 -5 14 72.29 6.40 -1 5 14 68.89 8.80 1 5 -14 82.99 9.60 0 -5 14 -1.50 3.00 0 5 -14 -3.30 5.20 0 5 14 -9.60 3.90 0 5 14 1.10 4.80 1 -5 14 5.10 3.80 -1 -5 -14 -4.20 6.10 1 5 14 3.70 4.40 1 5 14 -7.10 4.20 2 -5 14 89.19 8.40 2 5 14 79.29 8.10 2 5 14 85.69 10.60 3 -5 14 25.90 5.40 -3 5 -14 28.20 8.20 3 5 14 35.80 5.70 3 5 14 36.10 7.00 -4 -5 -14 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0 6 14 49.99 7.70 0 6 -14 40.60 7.40 1 -6 14 54.19 6.30 1 6 14 51.19 7.30 1 6 14 75.99 9.30 2 -6 14 19.30 5.00 -2 -6 -14 2.50 6.80 2 6 14 15.50 5.80 2 6 14 12.70 5.00 3 -6 14 17.20 5.20 -3 -6 -14 31.90 8.20 3 6 14 13.10 5.20 3 6 14 17.50 7.00 -3 6 -14 24.80 7.20 -4 -6 -14 6.90 7.40 4 -6 14 10.80 5.30 4 6 14 8.00 6.40 -4 6 -14 17.90 7.80 4 6 14 8.80 4.30 -5 -6 -14 -9.10 7.40 5 -6 14 3.60 5.30 -5 6 -14 -6.10 7.50 5 6 14 2.30 6.80 -6 -6 -14 15.80 9.00 6 -6 14 15.50 6.70 -6 6 -14 11.20 10.40 6 6 14 13.20 7.50 7 -7 -14 -10.30 8.20 -7 7 14 9.50 4.40 7 7 -14 3.00 5.40 -7 7 14 -2.60 7.10 -7 7 14 4.30 3.70 6 -7 -14 29.90 8.40 6 7 -14 47.40 6.80 -6 7 14 28.20 9.00 -6 7 14 45.40 6.40 -6 7 14 46.20 5.80 5 -7 -14 -18.60 6.70 5 7 -14 4.20 4.90 -5 7 14 3.90 6.50 -5 7 14 -1.00 4.60 4 -7 -14 40.20 9.30 -4 7 14 29.60 7.90 4 7 -14 34.60 6.00 -4 7 14 33.40 6.50 3 -7 -14 39.00 8.60 -3 -7 14 52.59 5.10 -3 7 14 28.70 8.00 -3 7 14 47.10 9.00 3 7 -14 45.60 6.90 -2 -7 14 5.60 3.20 2 -7 -14 -1.50 5.80 -2 7 14 2.90 5.60 2 7 -14 10.80 5.10 -2 7 14 5.70 5.30 -1 -7 14 -1.30 3.10 1 7 -14 -1.60 4.90 -1 7 14 -4.70 5.40 -1 7 14 1.60 5.50 0 -7 -14 -4.90 5.60 0 7 -14 -5.90 4.90 0 7 14 -1.40 4.40 0 7 14 7.00 5.50 1 -7 14 0.90 3.50 -1 -7 -14 -5.30 6.50 1 7 14 -7.20 4.80 1 7 14 -6.30 5.10 -1 7 -14 8.80 6.20 2 -7 14 137.59 9.90 -2 -7 -14 129.49 13.70 2 7 14 135.39 12.60 2 7 14 107.99 9.30 -3 -7 -14 -4.80 6.50 3 -7 14 9.50 4.90 -3 7 -14 1.50 6.90 3 7 14 21.10 6.80 3 7 14 9.40 4.90 4 -7 14 -0.30 5.20 -4 -7 -14 7.60 7.50 4 7 14 2.70 4.40 4 7 14 2.20 6.60 -4 7 -14 13.40 8.00 5 -7 14 15.00 5.70 -5 -7 -14 22.50 9.10 5 7 14 14.80 8.20 -5 7 -14 19.70 9.20 7 -8 -14 57.69 10.90 -7 8 14 35.00 5.30 7 8 -14 44.30 7.20 -7 8 14 46.10 6.10 -7 8 14 45.50 10.50 6 -8 -14 17.50 9.30 6 8 -14 19.30 5.60 -6 8 14 12.00 5.90 -6 8 14 3.40 6.70 -6 8 14 16.50 5.20 5 -8 -14 1.90 7.70 -5 8 14 1.20 6.20 5 8 -14 2.20 5.10 -5 8 14 3.10 6.20 4 -8 -14 -1.20 7.20 4 8 -14 1.70 5.20 -4 8 14 1.30 6.30 -4 8 14 0.20 5.80 3 -8 -14 18.10 7.90 -3 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15 38.70 8.80 5 -6 15 24.20 6.80 -5 -6 -15 21.80 9.70 -5 6 -15 32.60 11.40 5 6 15 24.20 7.70 6 -7 -15 -2.20 8.60 6 7 -15 12.60 6.10 -6 7 15 10.30 5.40 -6 7 15 2.50 6.70 5 -7 -15 -8.70 8.70 -5 7 15 7.20 7.90 -5 7 15 15.50 5.90 5 7 -15 11.60 6.00 4 -7 -15 30.80 8.70 -4 -7 15 35.10 3.80 -4 7 15 27.20 6.30 -4 7 15 28.30 8.50 4 7 -15 37.80 7.30 -3 -7 15 143.89 7.50 3 -7 -15 137.59 14.60 3 7 -15 156.38 12.10 -3 7 15 125.79 12.00 -3 7 15 117.79 12.00 2 -7 -15 9.10 7.50 -2 -7 15 -4.90 3.40 -2 7 15 -1.20 5.70 -2 7 15 3.20 6.00 2 7 -15 -0.90 5.60 -1 -7 15 152.08 10.50 -1 7 15 129.59 11.40 1 7 -15 108.49 12.50 -1 7 15 154.68 13.20 0 -7 -15 26.40 8.50 0 -7 15 12.70 4.60 0 7 15 1.90 5.30 0 7 -15 4.40 6.40 0 7 15 18.10 7.20 -1 -7 -15 281.07 18.30 1 -7 15 316.47 13.80 1 7 15 291.97 14.80 1 7 15 312.17 17.60 -1 7 -15 296.37 17.70 -2 -7 -15 361.16 20.20 2 -7 15 395.66 15.90 2 7 15 345.17 15.60 2 7 15 393.36 19.40 -2 7 -15 374.66 20.40 3 -7 15 46.70 7.30 -3 -7 -15 25.70 9.50 3 7 15 35.30 6.50 3 7 15 18.90 7.90 -3 7 -15 37.50 9.50 -4 -7 -15 58.59 11.50 4 -7 15 60.79 8.90 4 7 15 74.49 10.30 4 7 15 61.69 8.00 -4 7 -15 80.79 12.10 6 -8 -15 8.30 10.30 6 8 -15 27.10 7.00 -6 8 15 32.40 6.40 -6 8 15 19.70 8.20 -6 8 15 42.50 7.40 5 -8 -15 5.60 9.00 5 8 -15 17.50 6.40 -5 8 15 7.00 8.90 -5 8 15 4.50 6.00 4 -8 -15 -4.40 8.50 -4 8 15 -5.50 6.00 4 8 -15 2.80 6.00 -4 8 15 -8.40 6.60 -3 -8 15 0.00 3.30 3 -8 -15 -13.40 8.40 -3 8 15 -5.40 6.20 3 8 -15 18.40 6.50 -3 8 15 1.20 6.20 -2 -8 15 197.58 9.70 2 -8 -15 173.68 16.70 -2 8 15 210.48 14.50 -2 8 15 186.68 13.90 2 8 -15 170.28 13.80 -1 -8 15 13.80 5.60 1 -8 -15 9.70 8.60 -1 8 15 15.60 6.50 1 8 -15 20.70 6.80 -1 8 15 23.30 7.10 0 -8 -15 301.37 19.60 0 -8 15 308.47 13.20 0 8 15 299.97 15.90 0 8 15 333.57 18.10 0 8 -15 299.97 17.80 1 -8 15 123.09 10.10 -1 -8 -15 91.99 11.30 1 8 15 141.99 14.40 1 8 15 96.39 10.50 -1 8 -15 111.99 14.20 -2 -8 -15 12.90 8.90 2 -8 15 15.90 5.50 2 8 15 33.10 8.30 -2 8 -15 24.80 9.10 2 8 15 18.60 6.10 -3 -8 -15 63.99 11.40 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_publ_contact_author ; Prof. Dr.Christian M\"uller Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+49/(0)3083854004' _publ_contact_author_fax '+49/(0)3083852440' _publ_contact_author_email c.mueller@fu-berlin.de loop_ _publ_author_name _publ_author_address 'M\"uller, Christian' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Rigo, Massimo' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ... see the published paper. ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END===============================================