data_mr67mul _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 'C34 H21 Cr O5 P' _chemical_formula_weight 592.48 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' 'O' 'O' 0.0106 0.0060 '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' 'Cr' 'Cr' 0.3209 0.6236 '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 11.0446(2) _cell_length_b 12.6960(2) _cell_length_c 19.9868(3) _cell_angle_alpha 90 _cell_angle_beta 91.2050(10) _cell_angle_gamma 90 _cell_volume 2801.97(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9926 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 26.41 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_F_000 1216 _exptl_transmission_factor_min 0.7084 _exptl_transmission_factor_max 0.7454 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.070 _exptl_absorpt_coefficient_mu 0.508 _shelx_estimated_absorpt_T_min 0.901 _shelx_estimated_absorpt_T_max 0.961 _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 59409 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.445 _diffrn_reflns_theta_max 26.443 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 5757 _reflns_number_gt 5101 _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 'X-STEP32, 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^)+(0.0316P)^2^+2.4464P] 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 5757 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0759 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.62233(13) 0.25152(12) 0.35476(7) 0.0111(3) Uani 1 1 d . . . . . C2 C 0.62267(14) 0.35266(12) 0.37135(7) 0.0117(3) Uani 1 1 d . . . . . H2 H 0.5578 0.3799 0.3965 0.014 Uiso 1 1 calc R U . . . C3 C 0.72487(14) 0.42651(12) 0.35098(7) 0.0112(3) Uani 1 1 d . . . . . C4 C 0.73413(13) 0.41731(12) 0.27465(7) 0.0108(3) Uani 1 1 d . . . . . H4 H 0.7296 0.4786 0.2474 0.013 Uiso 1 1 calc R U . . . C5 C 0.74851(13) 0.32315(12) 0.24700(7) 0.0108(3) Uani 1 1 d . . . . . C6 C 0.76243(14) 0.30432(12) 0.17424(7) 0.0127(3) Uani 1 1 d . . . . . C7 C 0.87675(16) 0.30534(16) 0.14663(9) 0.0246(4) Uani 1 1 d . . . . . H7 H 0.9462 0.3168 0.1745 0.030 Uiso 1 1 calc R U . . . C8 C 0.89004(19) 0.28964(18) 0.07845(10) 0.0341(5) Uani 1 1 d . . . . . H8 H 0.9684 0.2917 0.0598 0.041 Uiso 1 1 calc R U . . . C9 C 0.78969(18) 0.27096(16) 0.03762(9) 0.0271(4) Uani 1 1 d . . . . . H9 H 0.7991 0.2600 -0.0090 0.033 Uiso 1 1 calc R U . . . C10 C 0.67580(17) 0.26824(13) 0.06480(8) 0.0199(4) Uani 1 1 d . . . . . H10 H 0.6068 0.2549 0.0369 0.024 Uiso 1 1 calc R U . . . C11 C 0.66184(15) 0.28498(13) 0.13297(8) 0.0155(3) Uani 1 1 d . . . . . H11 H 0.5833 0.2832 0.1514 0.019 Uiso 1 1 calc R U . . . C12 C 0.51873(14) 0.18119(12) 0.36898(7) 0.0116(3) Uani 1 1 d . . . . . C13 C 0.53145(15) 0.09284(13) 0.41016(8) 0.0147(3) Uani 1 1 d . . . . . H13 H 0.6086 0.0755 0.4289 0.018 Uiso 1 1 calc R U . . . C14 C 0.43198(16) 0.03039(13) 0.42380(8) 0.0184(3) Uani 1 1 d . . . . . H14 H 0.4415 -0.0296 0.4518 0.022 Uiso 1 1 calc R U . . . C15 C 0.31849(15) 0.05491(13) 0.39679(8) 0.0179(3) Uani 1 1 d . . . . . H15 H 0.2506 0.0118 0.4062 0.021 Uiso 1 1 calc R U . . . C16 C 0.30493(15) 0.14258(13) 0.35600(8) 0.0169(3) Uani 1 1 d . . . . . H16 H 0.2275 0.1598 0.3375 0.020 Uiso 1 1 calc R U . . . C17 C 0.40446(14) 0.20528(12) 0.34214(8) 0.0144(3) Uani 1 1 d . . . . . H17 H 0.3946 0.2652 0.3141 0.017 Uiso 1 1 calc R U . . . C18 C 0.70151(14) 0.53594(12) 0.37956(8) 0.0127(3) Uani 1 1 d . . . . . C19 C 0.70189(15) 0.62844(13) 0.34252(8) 0.0174(3) Uani 1 1 d . . . . . H19 H 0.7165 0.6258 0.2959 0.021 Uiso 1 1 calc R U . . . C20 C 0.68102(16) 0.72526(13) 0.37322(9) 0.0225(4) Uani 1 1 d . . . . . H20 H 0.6809 0.7878 0.3471 0.027 Uiso 1 1 calc R U . . . C21 C 0.66047(16) 0.73139(14) 0.44104(9) 0.0220(4) Uani 1 1 d . . . . . H21 H 0.6471 0.7977 0.4616 0.026 Uiso 1 1 calc R U . . . C22 C 0.65959(15) 0.63957(14) 0.47875(8) 0.0192(3) Uani 1 1 d . . . . . H22 H 0.6453 0.6428 0.5254 0.023 Uiso 1 1 calc R U . . . C23 C 0.67954(15) 0.54314(13) 0.44825(8) 0.0164(3) Uani 1 1 d . . . . . H23 H 0.6783 0.4807 0.4744 0.020 Uiso 1 1 calc R U . . . C24 C 0.86878(14) 0.27348(12) 0.36266(7) 0.0108(3) Uani 1 1 d . . . . . C25 C 0.84572(14) 0.37926(12) 0.37824(7) 0.0114(3) Uani 1 1 d . . . . . C26 C 0.93209(14) 0.43665(13) 0.41425(8) 0.0141(3) Uani 1 1 d . . . . . H26 H 0.9193 0.5094 0.4229 0.017 Uiso 1 1 calc R U . . . C27 C 1.03731(15) 0.38753(13) 0.43769(8) 0.0167(3) Uani 1 1 d . . . . . H27 H 1.0962 0.4271 0.4622 0.020 Uiso 1 1 calc R U . . . C28 C 1.05700(14) 0.28186(13) 0.42565(8) 0.0163(3) Uani 1 1 d . . . . . H28 H 1.1275 0.2484 0.4435 0.020 Uiso 1 1 calc R U . . . C29 C 0.97344(14) 0.22452(13) 0.38739(8) 0.0140(3) Uani 1 1 d . . . . . H29 H 0.9877 0.1522 0.3782 0.017 Uiso 1 1 calc R U . . . C30 C 0.81731(15) -0.00117(13) 0.36205(9) 0.0173(3) Uani 1 1 d . . . . . C31 C 0.62309(16) -0.00345(14) 0.27320(9) 0.0196(4) Uani 1 1 d . . . . . C32 C 0.82933(14) -0.10310(13) 0.25039(8) 0.0154(3) Uani 1 1 d . . . . . C33 C 0.75934(16) 0.05150(13) 0.17673(9) 0.0205(4) Uani 1 1 d . . . . . C34 C 0.95402(15) 0.07086(13) 0.25573(8) 0.0173(3) Uani 1 1 d . . . . . O1 O 0.83359(12) -0.02842(10) 0.41599(6) 0.0269(3) Uani 1 1 d . . . . . O2 O 0.52594(12) -0.03369(11) 0.26895(7) 0.0338(3) Uani 1 1 d . . . . . O3 O 0.85531(12) -0.18829(9) 0.23877(6) 0.0235(3) Uani 1 1 d . . . . . O4 O 0.74107(15) 0.04512(11) 0.12057(7) 0.0360(4) Uani 1 1 d . . . . . O5 O 1.05263(11) 0.08737(10) 0.24355(7) 0.0269(3) Uani 1 1 d . . . . . P1 P 0.75579(3) 0.21147(3) 0.30661(2) 0.00921(9) Uani 1 1 d . . . . . Cr1 Cr 0.78964(2) 0.03561(2) 0.27076(2) 0.01111(7) 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 0.0099(7) 0.0150(7) 0.0084(7) 0.0012(6) 0.0006(5) 0.0009(6) C2 0.0104(7) 0.0152(7) 0.0095(7) -0.0003(6) 0.0014(5) 0.0009(6) C3 0.0125(7) 0.0112(7) 0.0100(7) -0.0005(6) 0.0010(6) -0.0004(6) C4 0.0098(7) 0.0129(7) 0.0096(7) 0.0022(6) -0.0007(5) -0.0016(6) C5 0.0085(7) 0.0144(7) 0.0095(7) 0.0014(6) -0.0004(5) -0.0009(6) C6 0.0161(8) 0.0125(7) 0.0094(7) 0.0000(6) 0.0006(6) 0.0007(6) C7 0.0166(9) 0.0412(11) 0.0162(8) -0.0080(8) 0.0026(7) -0.0051(8) C8 0.0264(10) 0.0555(14) 0.0209(9) -0.0106(9) 0.0119(8) -0.0078(9) C9 0.0388(11) 0.0331(10) 0.0096(8) -0.0045(7) 0.0045(7) -0.0035(9) C10 0.0285(9) 0.0178(8) 0.0130(8) -0.0025(6) -0.0068(7) 0.0011(7) C11 0.0155(8) 0.0165(8) 0.0145(8) -0.0006(6) -0.0008(6) 0.0019(6) C12 0.0131(7) 0.0121(7) 0.0098(7) -0.0035(6) 0.0038(6) -0.0008(6) C13 0.0151(8) 0.0158(8) 0.0133(7) 0.0004(6) -0.0010(6) -0.0006(6) C14 0.0236(9) 0.0165(8) 0.0151(8) 0.0011(6) 0.0004(6) -0.0057(7) C15 0.0161(8) 0.0205(8) 0.0172(8) -0.0046(6) 0.0039(6) -0.0085(7) C16 0.0118(8) 0.0200(8) 0.0190(8) -0.0055(7) 0.0006(6) -0.0003(6) C17 0.0147(8) 0.0136(7) 0.0151(8) 0.0000(6) 0.0014(6) 0.0009(6) C18 0.0095(7) 0.0132(7) 0.0154(8) -0.0023(6) 0.0009(6) -0.0005(6) C19 0.0188(8) 0.0150(8) 0.0184(8) -0.0006(6) 0.0040(6) -0.0002(6) C20 0.0248(9) 0.0128(8) 0.0302(10) 0.0007(7) 0.0056(7) 0.0008(7) C21 0.0186(9) 0.0158(8) 0.0316(10) -0.0101(7) 0.0029(7) 0.0009(7) C22 0.0170(8) 0.0226(9) 0.0181(8) -0.0071(7) 0.0018(6) 0.0003(7) C23 0.0181(8) 0.0155(8) 0.0157(8) -0.0019(6) 0.0014(6) -0.0001(6) C24 0.0106(7) 0.0150(7) 0.0068(7) 0.0002(6) 0.0015(5) -0.0015(6) C25 0.0119(7) 0.0155(8) 0.0070(7) 0.0006(6) 0.0024(5) -0.0005(6) C26 0.0154(8) 0.0155(8) 0.0116(7) -0.0030(6) 0.0024(6) -0.0021(6) C27 0.0135(8) 0.0249(9) 0.0116(7) -0.0046(6) -0.0010(6) -0.0033(7) C28 0.0111(8) 0.0247(9) 0.0130(7) -0.0013(6) -0.0009(6) 0.0023(6) C29 0.0136(8) 0.0166(8) 0.0119(7) -0.0001(6) 0.0016(6) 0.0020(6) C30 0.0151(8) 0.0133(8) 0.0235(9) -0.0023(7) 0.0005(6) -0.0010(6) C31 0.0193(9) 0.0186(8) 0.0209(9) -0.0073(7) 0.0010(7) 0.0011(7) C32 0.0131(8) 0.0169(8) 0.0162(8) -0.0006(6) -0.0005(6) -0.0019(6) C33 0.0257(9) 0.0139(8) 0.0218(9) -0.0030(7) -0.0005(7) 0.0063(7) C34 0.0201(9) 0.0118(8) 0.0199(8) -0.0057(6) 0.0012(7) 0.0016(6) O1 0.0339(8) 0.0271(7) 0.0195(7) 0.0060(5) -0.0037(5) -0.0005(6) O2 0.0168(7) 0.0409(8) 0.0439(8) -0.0207(7) 0.0018(6) -0.0086(6) O3 0.0285(7) 0.0140(6) 0.0281(7) -0.0048(5) 0.0005(5) 0.0034(5) O4 0.0650(11) 0.0247(7) 0.0179(7) -0.0055(5) -0.0079(6) 0.0142(7) O5 0.0155(7) 0.0252(7) 0.0403(8) -0.0087(6) 0.0089(5) -0.0031(5) P1 0.00873(18) 0.01015(18) 0.00877(18) -0.00087(14) 0.00057(14) 0.00000(14) Cr1 0.00993(13) 0.00996(13) 0.01344(13) -0.00208(9) 0.00018(9) 0.00038(9) _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 1.326(2) . ? C1 C12 1.484(2) . ? C1 P1 1.8485(15) . ? C2 C3 1.529(2) . ? C2 H2 0.9500 . ? C3 C18 1.526(2) . ? C3 C4 1.535(2) . ? C3 C25 1.552(2) . ? C4 C5 1.328(2) . ? C4 H4 0.9500 . ? C5 C6 1.485(2) . ? C5 P1 1.8527(15) . ? C6 C7 1.389(2) . ? C6 C11 1.392(2) . ? C7 C8 1.388(3) . ? C7 H7 0.9500 . ? C8 C9 1.383(3) . ? C8 H8 0.9500 . ? C9 C10 1.381(3) . ? C9 H9 0.9500 . ? C10 C11 1.391(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.395(2) . ? C12 C13 1.397(2) . ? C13 C14 1.387(2) . ? C13 H13 0.9500 . ? C14 C15 1.390(2) . ? C14 H14 0.9500 . ? C15 C16 1.386(2) . ? C15 H15 0.9500 . ? C16 C17 1.390(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.388(2) . ? C18 C23 1.402(2) . ? C19 C20 1.395(2) . ? C19 H19 0.9500 . ? C20 C21 1.381(3) . ? C20 H20 0.9500 . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.394(2) . ? C24 C25 1.403(2) . ? C24 P1 1.8367(15) . ? C25 C26 1.389(2) . ? C26 C27 1.391(2) . ? C26 H26 0.9500 . ? C27 C28 1.381(2) . ? C27 H27 0.9500 . ? C28 C29 1.392(2) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 O1 1.143(2) . ? C30 Cr1 1.9018(17) . ? C31 O2 1.141(2) . ? C31 Cr1 1.9068(18) . ? C32 O3 1.144(2) . ? C32 Cr1 1.8620(17) . ? C33 O4 1.139(2) . ? C33 Cr1 1.9126(18) . ? C34 O5 1.140(2) . ? C34 Cr1 1.8998(17) . ? P1 Cr1 2.3768(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 C2 C1 C12 122.21(14) . . ? C2 C1 P1 113.48(12) . . ? C12 C1 P1 124.11(11) . . ? C1 C2 C3 121.69(14) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C18 C3 C2 109.08(12) . . ? C18 C3 C4 117.16(13) . . ? C2 C3 C4 106.43(12) . . ? C18 C3 C25 111.80(12) . . ? C2 C3 C25 107.69(12) . . ? C4 C3 C25 104.16(12) . . ? C5 C4 C3 119.54(13) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 124.63(14) . . ? C4 C5 P1 115.16(11) . . ? C6 C5 P1 120.17(11) . . ? C7 C6 C11 119.16(15) . . ? C7 C6 C5 120.10(14) . . ? C11 C6 C5 120.74(14) . . ? C8 C7 C6 120.31(17) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C9 C8 C7 120.26(18) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.83(16) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.15(16) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.27(15) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C17 C12 C13 118.80(14) . . ? C17 C12 C1 119.32(14) . . ? C13 C12 C1 121.86(14) . . ? C14 C13 C12 120.32(15) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C15 120.50(15) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 119.60(15) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.07(15) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C16 C17 C12 120.72(15) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? C19 C18 C23 118.01(14) . . ? C19 C18 C3 124.61(14) . . ? C23 C18 C3 117.38(14) . . ? C18 C19 C20 120.55(15) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 120.89(16) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.25(16) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C23 C22 C21 119.96(15) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C18 121.34(15) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? C29 C24 C25 120.08(14) . . ? C29 C24 P1 124.96(12) . . ? C25 C24 P1 114.93(11) . . ? C26 C25 C24 119.42(14) . . ? C26 C25 C3 123.73(14) . . ? C24 C25 C3 116.80(13) . . ? C25 C26 C27 119.92(15) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.68(15) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 119.92(15) . . ? C27 C28 H28 120.0 . . ? C29 C28 H28 120.0 . . ? C28 C29 C24 119.81(15) . . ? C28 C29 H29 120.1 . . ? C24 C29 H29 120.1 . . ? O1 C30 Cr1 176.59(15) . . ? O2 C31 Cr1 172.62(15) . . ? O3 C32 Cr1 178.75(15) . . ? O4 C33 Cr1 169.87(15) . . ? O5 C34 Cr1 175.66(14) . . ? C24 P1 C1 95.95(7) . . ? C24 P1 C5 94.81(7) . . ? C1 P1 C5 95.74(7) . . ? C24 P1 Cr1 118.51(5) . . ? C1 P1 Cr1 123.20(5) . . ? C5 P1 Cr1 122.01(5) . . ? C32 Cr1 C34 87.60(7) . . ? C32 Cr1 C30 86.78(7) . . ? C34 Cr1 C30 94.29(7) . . ? C32 Cr1 C31 89.50(7) . . ? C34 Cr1 C31 172.26(7) . . ? C30 Cr1 C31 92.70(7) . . ? C32 Cr1 C33 85.53(7) . . ? C34 Cr1 C33 88.15(8) . . ? C30 Cr1 C33 171.82(7) . . ? C31 Cr1 C33 84.47(8) . . ? C32 Cr1 P1 173.54(5) . . ? C34 Cr1 P1 89.05(5) . . ? C30 Cr1 P1 87.97(5) . . ? C31 Cr1 P1 94.51(5) . . ? C33 Cr1 P1 99.89(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 C12 C1 C2 C3 -174.51(13) . . . . ? P1 C1 C2 C3 0.56(19) . . . . ? C1 C2 C3 C18 -177.96(14) . . . . ? C1 C2 C3 C4 54.78(18) . . . . ? C1 C2 C3 C25 -56.43(18) . . . . ? C18 C3 C4 C5 -176.75(14) . . . . ? C2 C3 C4 C5 -54.45(18) . . . . ? C25 C3 C4 C5 59.19(17) . . . . ? C3 C4 C5 C6 -178.01(14) . . . . ? C3 C4 C5 P1 -0.03(19) . . . . ? C4 C5 C6 C7 89.2(2) . . . . ? P1 C5 C6 C7 -88.71(18) . . . . ? C4 C5 C6 C11 -91.1(2) . . . . ? P1 C5 C6 C11 90.97(17) . . . . ? C11 C6 C7 C8 1.5(3) . . . . ? C5 C6 C7 C8 -178.85(18) . . . . ? C6 C7 C8 C9 -1.2(3) . . . . ? C7 C8 C9 C10 0.2(3) . . . . ? C8 C9 C10 C11 0.5(3) . . . . ? C9 C10 C11 C6 -0.1(3) . . . . ? C7 C6 C11 C10 -0.8(2) . . . . ? C5 C6 C11 C10 179.51(15) . . . . ? C2 C1 C12 C17 59.1(2) . . . . ? P1 C1 C12 C17 -115.48(15) . . . . ? C2 C1 C12 C13 -119.07(17) . . . . ? P1 C1 C12 C13 66.40(18) . . . . ? C17 C12 C13 C14 0.2(2) . . . . ? C1 C12 C13 C14 178.29(14) . . . . ? C12 C13 C14 C15 -0.1(2) . . . . ? C13 C14 C15 C16 -0.1(2) . . . . ? C14 C15 C16 C17 0.2(2) . . . . ? C15 C16 C17 C12 -0.1(2) . . . . ? C13 C12 C17 C16 -0.1(2) . . . . ? C1 C12 C17 C16 -178.25(14) . . . . ? C2 C3 C18 C19 -128.62(16) . . . . ? C4 C3 C18 C19 -7.7(2) . . . . ? C25 C3 C18 C19 112.39(17) . . . . ? C2 C3 C18 C23 52.14(18) . . . . ? C4 C3 C18 C23 173.06(14) . . . . ? C25 C3 C18 C23 -66.85(18) . . . . ? C23 C18 C19 C20 0.0(2) . . . . ? C3 C18 C19 C20 -179.19(15) . . . . ? C18 C19 C20 C21 0.5(3) . . . . ? C19 C20 C21 C22 -0.6(3) . . . . ? C20 C21 C22 C23 0.2(3) . . . . ? C21 C22 C23 C18 0.4(3) . . . . ? C19 C18 C23 C22 -0.5(2) . . . . ? C3 C18 C23 C22 178.82(15) . . . . ? C29 C24 C25 C26 4.7(2) . . . . ? P1 C24 C25 C26 -173.07(11) . . . . ? C29 C24 C25 C3 -177.72(13) . . . . ? P1 C24 C25 C3 4.50(17) . . . . ? C18 C3 C25 C26 -11.0(2) . . . . ? C2 C3 C25 C26 -130.79(15) . . . . ? C4 C3 C25 C26 116.47(15) . . . . ? C18 C3 C25 C24 171.58(13) . . . . ? C2 C3 C25 C24 51.76(17) . . . . ? C4 C3 C25 C24 -60.98(16) . . . . ? C24 C25 C26 C27 -3.6(2) . . . . ? C3 C25 C26 C27 179.06(14) . . . . ? C25 C26 C27 C28 -0.1(2) . . . . ? C26 C27 C28 C29 2.6(2) . . . . ? C27 C28 C29 C24 -1.5(2) . . . . ? C25 C24 C29 C28 -2.2(2) . . . . ? P1 C24 C29 C28 175.33(12) . . . . ? C29 C24 P1 C1 131.78(14) . . . . ? C25 C24 P1 C1 -50.56(12) . . . . ? C29 C24 P1 C5 -131.93(14) . . . . ? C25 C24 P1 C5 45.73(12) . . . . ? C29 C24 P1 Cr1 -1.31(15) . . . . ? C25 C24 P1 Cr1 176.35(9) . . . . ? C2 C1 P1 C24 48.28(12) . . . . ? C12 C1 P1 C24 -136.77(13) . . . . ? C2 C1 P1 C5 -47.19(12) . . . . ? C12 C1 P1 C5 127.77(13) . . . . ? C2 C1 P1 Cr1 178.19(9) . . . . ? C12 C1 P1 Cr1 -6.85(15) . . . . ? C4 C5 P1 C24 -49.17(13) . . . . ? C6 C5 P1 C24 128.91(12) . . . . ? C4 C5 P1 C1 47.32(13) . . . . ? C6 C5 P1 C1 -134.60(12) . . . . ? C4 C5 P1 Cr1 -177.30(10) . . . . ? C6 C5 P1 Cr1 0.78(14) . . . . ? _refine_diff_density_max 0.350 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.053 _shelx_res_file ; mr67mul.res created by SHELXL-2014/7 TITL MR67 multiscan in P2(1)/c CELL 0.71073 11.0446 12.6960 19.9868 90.000 91.205 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.001 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H O P CR UNIT 136 84 20 4 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.080 0.110 0.210 ACTA BOND $H CONF LIST 6 L.S. 30 TEMP -100.00 WGHT 0.031600 2.446400 FVAR 0.54008 C1 1 0.622333 0.251521 0.354757 11.00000 0.00988 0.01503 = 0.00836 0.00116 0.00063 0.00088 C2 1 0.622670 0.352663 0.371349 11.00000 0.01045 0.01517 = 0.00953 -0.00026 0.00135 0.00091 AFIX 43 H2 2 0.557755 0.379933 0.396536 11.00000 -1.20000 AFIX 0 C3 1 0.724870 0.426509 0.350980 11.00000 0.01248 0.01115 = 0.00999 -0.00054 0.00104 -0.00041 C4 1 0.734128 0.417313 0.274655 11.00000 0.00976 0.01293 = 0.00965 0.00223 -0.00074 -0.00158 AFIX 43 H4 2 0.729601 0.478556 0.247408 11.00000 -1.20000 AFIX 0 C5 1 0.748508 0.323152 0.246997 11.00000 0.00854 0.01438 = 0.00947 0.00141 -0.00038 -0.00088 C6 1 0.762432 0.304323 0.174244 11.00000 0.01605 0.01252 = 0.00944 0.00004 0.00058 0.00070 C7 1 0.876746 0.305341 0.146626 11.00000 0.01658 0.04119 = 0.01617 -0.00801 0.00259 -0.00514 AFIX 43 H7 2 0.946186 0.316837 0.174528 11.00000 -1.20000 AFIX 0 C8 1 0.890035 0.289644 0.078448 11.00000 0.02638 0.05550 = 0.02092 -0.01065 0.01191 -0.00778 AFIX 43 H8 2 0.968376 0.291744 0.059757 11.00000 -1.20000 AFIX 0 C9 1 0.789692 0.270959 0.037621 11.00000 0.03885 0.03315 = 0.00957 -0.00452 0.00446 -0.00354 AFIX 43 H9 2 0.799077 0.260021 -0.009004 11.00000 -1.20000 AFIX 0 C10 1 0.675799 0.268239 0.064801 11.00000 0.02853 0.01781 = 0.01296 -0.00245 -0.00676 0.00106 AFIX 43 H10 2 0.606840 0.254905 0.036870 11.00000 -1.20000 AFIX 0 C11 1 0.661836 0.284978 0.132972 11.00000 0.01551 0.01652 = 0.01448 -0.00056 -0.00085 0.00194 AFIX 43 H11 2 0.583305 0.283199 0.151439 11.00000 -1.20000 AFIX 0 C12 1 0.518728 0.181186 0.368977 11.00000 0.01313 0.01213 = 0.00980 -0.00346 0.00376 -0.00080 C13 1 0.531448 0.092842 0.410161 11.00000 0.01506 0.01582 = 0.01330 0.00041 -0.00103 -0.00055 AFIX 43 H13 2 0.608625 0.075455 0.428925 11.00000 -1.20000 AFIX 0 C14 1 0.431979 0.030389 0.423796 11.00000 0.02360 0.01646 = 0.01513 0.00110 0.00039 -0.00566 AFIX 43 H14 2 0.441487 -0.029620 0.451809 11.00000 -1.20000 AFIX 0 C15 1 0.318491 0.054912 0.396794 11.00000 0.01608 0.02053 = 0.01716 -0.00455 0.00390 -0.00848 AFIX 43 H15 2 0.250614 0.011849 0.406237 11.00000 -1.20000 AFIX 0 C16 1 0.304925 0.142576 0.356003 11.00000 0.01175 0.01995 = 0.01897 -0.00550 0.00056 -0.00030 AFIX 43 H16 2 0.227513 0.159827 0.337495 11.00000 -1.20000 AFIX 0 C17 1 0.404459 0.205278 0.342144 11.00000 0.01469 0.01355 = 0.01509 0.00000 0.00136 0.00095 AFIX 43 H17 2 0.394555 0.265198 0.314091 11.00000 -1.20000 AFIX 0 C18 1 0.701511 0.535940 0.379565 11.00000 0.00947 0.01321 = 0.01539 -0.00228 0.00093 -0.00047 C19 1 0.701892 0.628436 0.342520 11.00000 0.01880 0.01504 = 0.01841 -0.00062 0.00404 -0.00019 AFIX 43 H19 2 0.716488 0.625782 0.295877 11.00000 -1.20000 AFIX 0 C20 1 0.681018 0.725256 0.373219 11.00000 0.02484 0.01281 = 0.03017 0.00065 0.00558 0.00083 AFIX 43 H20 2 0.680937 0.787802 0.347128 11.00000 -1.20000 AFIX 0 C21 1 0.660468 0.731389 0.441039 11.00000 0.01860 0.01578 = 0.03163 -0.01013 0.00293 0.00087 AFIX 43 H21 2 0.647083 0.797686 0.461644 11.00000 -1.20000 AFIX 0 C22 1 0.659595 0.639575 0.478751 11.00000 0.01703 0.02258 = 0.01812 -0.00707 0.00185 0.00027 AFIX 43 H22 2 0.645345 0.642777 0.525416 11.00000 -1.20000 AFIX 0 C23 1 0.679543 0.543139 0.448249 11.00000 0.01810 0.01550 = 0.01572 -0.00195 0.00145 -0.00007 AFIX 43 H23 2 0.678293 0.480716 0.474434 11.00000 -1.20000 AFIX 0 C24 1 0.868783 0.273476 0.362657 11.00000 0.01062 0.01499 = 0.00684 0.00019 0.00146 -0.00153 C25 1 0.845722 0.379256 0.378238 11.00000 0.01188 0.01549 = 0.00700 0.00064 0.00242 -0.00051 C26 1 0.932093 0.436654 0.414253 11.00000 0.01536 0.01551 = 0.01155 -0.00301 0.00236 -0.00207 AFIX 43 H26 2 0.919326 0.509356 0.422867 11.00000 -1.20000 AFIX 0 C27 1 1.037308 0.387533 0.437691 11.00000 0.01345 0.02489 = 0.01156 -0.00464 -0.00100 -0.00330 AFIX 43 H27 2 1.096207 0.427089 0.462230 11.00000 -1.20000 AFIX 0 C28 1 1.057004 0.281862 0.425648 11.00000 0.01114 0.02468 = 0.01295 -0.00129 -0.00090 0.00232 AFIX 43 H28 2 1.127511 0.248351 0.443461 11.00000 -1.20000 AFIX 0 C29 1 0.973435 0.224525 0.387386 11.00000 0.01359 0.01665 = 0.01185 -0.00012 0.00159 0.00204 AFIX 43 H29 2 0.987684 0.152230 0.378151 11.00000 -1.20000 AFIX 0 C30 1 0.817306 -0.001169 0.362050 11.00000 0.01515 0.01326 = 0.02351 -0.00226 0.00049 -0.00101 C31 1 0.623089 -0.003449 0.273203 11.00000 0.01928 0.01861 = 0.02092 -0.00729 0.00101 0.00112 C32 1 0.829334 -0.103102 0.250386 11.00000 0.01310 0.01693 = 0.01615 -0.00055 -0.00052 -0.00189 C33 1 0.759344 0.051504 0.176733 11.00000 0.02571 0.01391 = 0.02180 -0.00299 -0.00055 0.00627 C34 1 0.954018 0.070860 0.255726 11.00000 0.02008 0.01185 = 0.01987 -0.00567 0.00118 0.00160 O1 3 0.833585 -0.028421 0.415989 11.00000 0.03385 0.02713 = 0.01953 0.00598 -0.00373 -0.00053 O2 3 0.525944 -0.033692 0.268952 11.00000 0.01680 0.04092 = 0.04386 -0.02072 0.00177 -0.00856 O3 3 0.855313 -0.188289 0.238766 11.00000 0.02852 0.01402 = 0.02807 -0.00478 0.00052 0.00345 O4 3 0.741069 0.045121 0.120573 11.00000 0.06496 0.02468 = 0.01787 -0.00554 -0.00795 0.01417 O5 3 1.052629 0.087366 0.243551 11.00000 0.01548 0.02524 = 0.04026 -0.00873 0.00894 -0.00312 P1 4 0.755787 0.211468 0.306610 11.00000 0.00873 0.01015 = 0.00877 -0.00087 0.00057 0.00000 CR1 5 0.789645 0.035613 0.270762 11.00000 0.00993 0.00996 = 0.01344 -0.00208 0.00018 0.00038 HKLF 4 REM MR67 multiscan in P2(1)/c REM R1 = 0.0294 for 5101 Fo > 4sig(Fo) and 0.0359 for all 5757 data REM 370 parameters refined using 0 restraints END WGHT 0.0316 2.4463 REM Highest difference peak 0.350, deepest hole -0.420, 1-sigma level 0.053 Q1 1 0.7845 0.4063 0.3679 11.00000 0.05 0.35 Q2 1 0.7117 0.4813 0.3623 11.00000 0.05 0.34 Q3 1 0.6402 0.6806 0.4541 11.00000 0.05 0.29 Q4 1 0.5716 0.2173 0.3629 11.00000 0.05 0.29 Q5 1 0.6664 0.5781 0.3588 11.00000 0.05 0.29 Q6 1 0.8590 0.3299 0.3696 11.00000 0.05 0.29 Q7 1 0.7180 0.3016 0.1549 11.00000 0.05 0.28 Q8 1 0.6872 0.6785 0.3574 11.00000 0.05 0.28 Q9 1 0.7486 0.2707 0.2701 11.00000 0.05 0.27 Q10 1 0.7352 0.4217 0.3140 11.00000 0.05 0.27 Q11 1 0.7510 0.3170 0.2083 11.00000 0.05 0.27 Q12 1 0.7309 0.5803 0.3659 11.00000 0.05 0.27 Q13 1 0.6751 0.3948 0.3602 11.00000 0.05 0.27 Q14 1 0.8160 0.2440 0.3396 11.00000 0.05 0.27 Q15 1 0.6691 0.5941 0.4634 11.00000 0.05 0.26 Q16 1 0.4672 0.1827 0.3486 11.00000 0.05 0.26 Q17 1 0.6949 0.5429 0.4124 11.00000 0.05 0.26 Q18 1 0.6773 0.2269 0.3399 11.00000 0.05 0.25 Q19 1 0.3558 0.1724 0.3492 11.00000 0.05 0.25 Q20 1 0.8142 0.2996 0.1615 11.00000 0.05 0.24 ; _shelx_res_checksum 60583 _shelx_hkl_file ; 3 0 0 313.47 12.40 3 0 0 297.67 12.30 3 0 0 326.87 12.40 -3 0 0 311.87 12.20 -3 0 0 320.87 12.30 4 0 0 1502.45 48.00 4 0 0 1547.95 47.90 -4 0 0 1526.45 47.50 -4 0 0 1545.05 47.80 4 0 0 1529.65 48.00 5 0 0 18.80 4.60 5 0 0 12.00 3.70 -5 0 0 15.00 4.00 5 0 0 5.90 4.10 -5 0 0 12.10 4.20 6 0 0 104.79 9.70 6 0 0 93.89 9.20 6 0 0 83.49 8.40 6 0 0 96.09 9.40 7 0 0 844.92 32.90 -7 0 0 859.81 32.10 7 0 0 854.71 31.60 -7 0 0 878.01 32.60 7 0 0 883.71 33.50 7 0 0 861.71 33.10 8 0 0 16.60 6.00 -8 0 0 21.50 6.60 8 0 0 8.00 6.60 8 0 0 17.00 9.10 -8 0 0 18.10 6.80 9 0 0 23.10 9.70 9 0 0 20.00 8.90 -9 0 0 20.20 7.80 9 0 0 20.30 7.70 -9 0 0 27.20 7.80 -10 0 0 268.07 19.90 10 0 0 298.97 22.50 10 0 0 246.78 21.00 10 0 0 317.57 20.20 -10 0 0 327.27 21.00 11 0 0 916.81 41.70 11 0 0 951.40 39.20 -11 0 0 967.10 40.10 11 0 0 909.11 49.80 12 0 0 89.69 17.00 -12 0 0 143.69 17.50 12 0 0 114.29 12.80 12 0 0 102.69 18.50 12 0 0 124.89 16.30 -12 0 0 90.69 15.30 -13 0 0 40.00 15.60 -13 0 0 72.39 16.50 13 0 0 58.49 11.70 13 0 0 34.10 16.50 -13 0 0 42.40 17.10 13 0 0 57.09 15.70 1 -1 0 3496.95 106.79 1 -1 0 4011.90 106.79 2 -1 0 1330.77 38.50 -2 -1 0 1240.68 37.70 2 -1 0 1305.47 38.40 -2 -1 0 1223.18 37.50 -2 -1 0 1260.07 38.10 2 -1 0 1288.07 38.50 2 1 0 1223.38 37.70 -2 1 0 1279.07 38.40 -2 1 0 1285.67 38.50 -2 1 0 1315.47 38.50 2 1 0 1253.17 37.90 3 -1 0 1507.35 48.20 -3 -1 0 1636.74 47.90 -3 -1 0 1660.13 47.70 3 -1 0 1506.25 48.30 3 -1 0 1558.94 48.40 -3 1 0 1632.74 48.50 -3 1 0 1589.64 48.50 -3 1 0 1553.84 48.50 3 1 0 1659.43 48.30 3 1 0 1587.54 47.90 4 -1 0 1521.65 46.70 4 -1 0 1507.45 46.60 -4 -1 0 1474.45 45.70 4 -1 0 1530.95 46.60 -4 -1 0 1478.75 45.40 -4 1 0 1488.05 46.50 -4 1 0 1498.15 46.40 4 1 0 1370.66 45.70 4 1 0 1391.06 45.90 5 -1 0 1934.91 60.49 5 -1 0 1945.21 60.29 -5 -1 0 1890.91 58.99 -5 -1 0 1886.81 59.39 5 1 0 1960.80 60.19 5 1 0 1928.81 59.89 -5 1 0 1933.41 60.09 -5 1 0 1891.51 60.19 6 -1 0 185.88 10.60 6 -1 0 189.38 12.40 6 -1 0 183.68 12.50 6 -1 0 208.18 13.00 -6 -1 0 203.08 11.60 -6 -1 0 184.68 11.50 6 1 0 184.98 12.00 6 1 0 191.78 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15.10 -1 -3 -24 9.90 14.20 -1 -3 -24 57.29 22.60 1 -3 24 -2.50 15.70 -1 3 -24 -20.20 15.90 1 3 24 23.80 15.00 -1 3 -24 11.10 12.80 -1 3 -24 13.60 16.10 -2 -3 -24 91.99 19.20 -2 -3 -24 110.29 27.80 2 -3 24 58.89 19.00 -2 -3 -24 102.79 17.40 -2 3 -24 93.19 19.60 -2 3 -24 68.99 20.20 -2 3 -24 103.89 14.70 2 3 24 67.79 18.40 -2 -4 24 64.79 16.90 2 4 -24 76.69 18.20 1 -4 -24 14.30 16.30 -1 -4 24 36.00 15.30 1 -4 -24 37.00 16.40 1 4 -24 42.70 14.50 1 4 -24 36.90 16.70 -1 4 24 22.50 16.60 0 -4 -24 167.98 19.90 0 -4 24 164.48 21.40 0 -4 -24 161.48 20.30 0 4 -24 224.98 20.70 0 4 -24 194.78 22.30 0 4 24 153.38 20.10 -1 -4 -24 41.60 17.10 -1 -4 -24 27.60 15.00 1 -4 24 -9.00 15.80 1 4 24 11.70 15.10 -1 4 -24 4.20 16.70 -1 4 -24 -5.20 11.40 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 9805 #============================================================================== _publ_requested_journal '??????' _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 ; 'Wiecko, Jelena' ; 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====================================================