data_MK09_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 'C34 H21 Mo O5 P' _chemical_formula_weight 636.42 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' 'Mo' 'Mo' -1.6832 0.6857 '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' _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 11.2067(2) _cell_length_b 12.8656(2) _cell_length_c 19.9607(5) _cell_angle_alpha 90 _cell_angle_beta 91.1287(8) _cell_angle_gamma 90 _cell_volume 2877.39(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9867 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.40 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_F_000 1288 _exptl_transmission_factor_min 0.7617 _exptl_transmission_factor_max 0.8495 _exptl_crystal_size_max 0.310 _exptl_crystal_size_mid 0.220 _exptl_crystal_size_min 0.140 _exptl_absorpt_coefficient_mu 0.553 _shelx_estimated_absorpt_T_min 0.847 _shelx_estimated_absorpt_T_max 0.927 _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 29939 _diffrn_reflns_av_unetI/netI 0.0353 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.410 _diffrn_reflns_theta_max 26.426 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 5859 _reflns_number_gt 4924 _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^)+(0.0245P)^2^+2.2273P] 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 5859 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0286 _refine_ls_wR_factor_ref 0.0662 _refine_ls_wR_factor_gt 0.0605 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 0.62239(18) 0.25248(16) 0.35710(10) 0.0113(4) Uani 1 1 d . . . . . C2 C 0.62262(17) 0.35260(17) 0.37371(10) 0.0116(4) Uani 1 1 d . . . . . H2 H 0.5588 0.3795 0.3991 0.014 Uiso 1 1 calc R U . . . C3 C 0.72363(18) 0.42581(16) 0.35279(10) 0.0110(4) Uani 1 1 d . . . . . C4 C 0.73264(17) 0.41605(16) 0.27647(10) 0.0109(4) Uani 1 1 d . . . . . H4 H 0.7284 0.4764 0.2491 0.013 Uiso 1 1 calc R U . . . C5 C 0.74634(18) 0.32303(16) 0.24873(10) 0.0112(4) Uani 1 1 d . . . . . C6 C 0.75909(19) 0.30441(16) 0.17584(10) 0.0125(4) Uani 1 1 d . . . . . C7 C 0.8703(2) 0.3092(2) 0.14694(12) 0.0278(6) Uani 1 1 d . . . . . H7 H 0.9391 0.3225 0.1742 0.033 Uiso 1 1 calc R U . . . C8 C 0.8820(2) 0.2948(2) 0.07836(13) 0.0385(7) Uani 1 1 d . . . . . H8 H 0.9584 0.2994 0.0588 0.046 Uiso 1 1 calc R U . . . C9 C 0.7826(2) 0.2739(2) 0.03860(12) 0.0292(6) Uani 1 1 d . . . . . H9 H 0.7908 0.2640 -0.0083 0.035 Uiso 1 1 calc R U . . . C10 C 0.6723(2) 0.26721(18) 0.06667(11) 0.0207(5) Uani 1 1 d . . . . . H10 H 0.6042 0.2518 0.0393 0.025 Uiso 1 1 calc R U . . . C11 C 0.6597(2) 0.28296(17) 0.13512(11) 0.0162(5) Uani 1 1 d . . . . . H11 H 0.5828 0.2791 0.1542 0.019 Uiso 1 1 calc R U . . . C12 C 0.52116(18) 0.18225(16) 0.37103(10) 0.0114(4) Uani 1 1 d . . . . . C13 C 0.40716(19) 0.20653(17) 0.34537(11) 0.0147(5) Uani 1 1 d . . . . . H13 H 0.3959 0.2671 0.3188 0.018 Uiso 1 1 calc R U . . . C14 C 0.31065(19) 0.14247(18) 0.35862(11) 0.0182(5) Uani 1 1 d . . . . . H14 H 0.2337 0.1595 0.3411 0.022 Uiso 1 1 calc R U . . . C15 C 0.3259(2) 0.05421(18) 0.39713(11) 0.0181(5) Uani 1 1 d . . . . . H15 H 0.2597 0.0105 0.4060 0.022 Uiso 1 1 calc R U . . . C16 C 0.4380(2) 0.02965(18) 0.42280(11) 0.0193(5) Uani 1 1 d . . . . . H16 H 0.4486 -0.0311 0.4493 0.023 Uiso 1 1 calc R U . . . C17 C 0.53510(19) 0.09306(17) 0.41005(11) 0.0162(5) Uani 1 1 d . . . . . H17 H 0.6116 0.0756 0.4280 0.019 Uiso 1 1 calc R U . . . C18 C 0.70080(18) 0.53403(16) 0.38120(11) 0.0132(4) Uani 1 1 d . . . . . C19 C 0.69922(19) 0.62469(17) 0.34371(12) 0.0170(5) Uani 1 1 d . . . . . H19 H 0.7119 0.6215 0.2968 0.020 Uiso 1 1 calc R U . . . C20 C 0.6792(2) 0.72052(18) 0.37404(13) 0.0232(5) Uani 1 1 d . . . . . H20 H 0.6783 0.7820 0.3476 0.028 Uiso 1 1 calc R U . . . C21 C 0.6607(2) 0.72698(19) 0.44221(13) 0.0232(5) Uani 1 1 d . . . . . H21 H 0.6477 0.7925 0.4627 0.028 Uiso 1 1 calc R U . . . C22 C 0.66123(19) 0.63702(18) 0.48032(12) 0.0199(5) Uani 1 1 d . . . . . H22 H 0.6485 0.6407 0.5272 0.024 Uiso 1 1 calc R U . . . C23 C 0.68032(19) 0.54177(17) 0.45016(11) 0.0170(5) Uani 1 1 d . . . . . H23 H 0.6795 0.4804 0.4766 0.020 Uiso 1 1 calc R U . . . C24 C 0.86579(18) 0.27485(17) 0.36470(10) 0.0111(4) Uani 1 1 d . . . . . C25 C 0.84300(18) 0.37897(16) 0.38011(10) 0.0117(4) Uani 1 1 d . . . . . C26 C 0.92882(19) 0.43549(18) 0.41586(11) 0.0153(5) Uani 1 1 d . . . . . H26 H 0.9163 0.5072 0.4248 0.018 Uiso 1 1 calc R U . . . C27 C 1.03313(19) 0.38685(18) 0.43857(11) 0.0177(5) Uani 1 1 d . . . . . H27 H 1.0918 0.4259 0.4626 0.021 Uiso 1 1 calc R U . . . C28 C 1.05217(19) 0.28292(19) 0.42658(11) 0.0180(5) Uani 1 1 d . . . . . H28 H 1.1218 0.2497 0.4441 0.022 Uiso 1 1 calc R U . . . C29 C 0.96873(18) 0.22655(18) 0.38853(11) 0.0143(4) Uani 1 1 d . . . . . H29 H 0.9825 0.1553 0.3790 0.017 Uiso 1 1 calc R U . . . C30 C 0.8206(2) -0.01009(17) 0.36973(12) 0.0179(5) Uani 1 1 d . . . . . C31 C 0.6144(2) -0.01264(19) 0.27384(12) 0.0228(5) Uani 1 1 d . . . . . C32 C 0.83272(19) -0.11773(18) 0.24893(11) 0.0161(5) Uani 1 1 d . . . . . C33 C 0.7601(2) 0.04762(18) 0.16993(13) 0.0254(6) Uani 1 1 d . . . . . C34 C 0.9663(2) 0.06519(17) 0.25614(12) 0.0184(5) Uani 1 1 d . . . . . O1 O 0.83683(16) -0.03652(14) 0.42361(9) 0.0305(4) Uani 1 1 d . . . . . O2 O 0.51867(15) -0.04134(16) 0.26960(11) 0.0413(5) Uani 1 1 d . . . . . O3 O 0.85918(15) -0.20174(12) 0.23770(9) 0.0257(4) Uani 1 1 d . . . . . O4 O 0.7426(2) 0.04323(15) 0.11372(9) 0.0477(6) Uani 1 1 d . . . . . O5 O 1.06336(14) 0.08078(14) 0.24433(10) 0.0342(5) Uani 1 1 d . . . . . Mo1 Mo 0.79105(2) 0.02907(2) 0.27127(2) 0.01129(6) Uani 1 1 d . . . . . P1 P 0.75403(5) 0.21323(4) 0.30877(3) 0.00981(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 0.0101(10) 0.0148(11) 0.0090(10) 0.0017(8) 0.0001(8) 0.0008(8) C2 0.0096(10) 0.0157(11) 0.0097(10) 0.0001(9) 0.0021(8) 0.0007(8) C3 0.0124(10) 0.0091(10) 0.0116(11) 0.0008(8) 0.0003(8) -0.0007(8) C4 0.0091(10) 0.0133(11) 0.0104(10) 0.0032(8) -0.0004(8) -0.0019(8) C5 0.0085(9) 0.0157(11) 0.0094(10) 0.0011(8) -0.0013(8) -0.0011(8) C6 0.0167(11) 0.0118(11) 0.0090(11) -0.0004(8) 0.0006(8) 0.0003(9) C7 0.0181(12) 0.0494(17) 0.0159(13) -0.0099(12) 0.0021(10) -0.0061(11) C8 0.0276(14) 0.067(2) 0.0218(15) -0.0125(14) 0.0146(11) -0.0124(14) C9 0.0418(16) 0.0367(16) 0.0093(12) -0.0067(11) 0.0060(11) -0.0061(12) C10 0.0290(13) 0.0209(13) 0.0119(11) -0.0021(9) -0.0065(10) 0.0013(10) C11 0.0157(11) 0.0193(12) 0.0135(11) -0.0008(9) -0.0003(9) 0.0020(9) C12 0.0122(10) 0.0120(11) 0.0100(10) -0.0039(8) 0.0028(8) -0.0011(8) C13 0.0151(11) 0.0152(11) 0.0138(11) -0.0010(9) 0.0014(9) 0.0007(9) C14 0.0134(11) 0.0217(12) 0.0196(12) -0.0056(10) -0.0001(9) -0.0002(9) C15 0.0180(11) 0.0186(12) 0.0178(12) -0.0039(9) 0.0047(9) -0.0086(9) C16 0.0263(12) 0.0171(12) 0.0145(11) 0.0007(9) 0.0013(9) -0.0057(10) C17 0.0169(11) 0.0179(12) 0.0136(11) 0.0000(9) -0.0010(9) -0.0009(9) C18 0.0093(10) 0.0149(11) 0.0154(11) -0.0027(9) -0.0004(8) -0.0015(9) C19 0.0195(11) 0.0132(11) 0.0186(12) 0.0001(9) 0.0056(9) -0.0007(9) C20 0.0259(13) 0.0123(12) 0.0315(14) 0.0011(10) 0.0065(11) 0.0010(10) C21 0.0198(12) 0.0171(12) 0.0329(15) -0.0089(11) 0.0043(10) -0.0002(10) C22 0.0179(11) 0.0229(13) 0.0191(12) -0.0091(10) 0.0032(9) -0.0003(10) C23 0.0201(11) 0.0153(12) 0.0158(12) -0.0026(9) 0.0013(9) -0.0016(9) C24 0.0107(10) 0.0156(11) 0.0070(10) 0.0004(8) 0.0023(8) -0.0031(8) C25 0.0125(10) 0.0162(11) 0.0066(10) 0.0016(8) 0.0030(8) -0.0015(8) C26 0.0172(11) 0.0166(11) 0.0120(11) -0.0025(9) 0.0015(9) -0.0018(9) C27 0.0132(10) 0.0285(13) 0.0115(11) -0.0057(10) -0.0007(9) -0.0034(9) C28 0.0118(10) 0.0293(14) 0.0129(11) -0.0012(10) -0.0009(9) 0.0021(10) C29 0.0131(10) 0.0189(12) 0.0108(11) 0.0001(9) 0.0017(8) 0.0004(9) C30 0.0179(11) 0.0142(11) 0.0214(13) -0.0002(9) -0.0005(9) -0.0022(9) C31 0.0207(13) 0.0241(13) 0.0235(13) -0.0120(10) 0.0007(10) 0.0010(10) C32 0.0155(10) 0.0191(13) 0.0136(11) 0.0012(9) 0.0005(9) -0.0031(9) C33 0.0362(14) 0.0163(13) 0.0236(14) -0.0027(10) -0.0026(11) 0.0112(11) C34 0.0215(13) 0.0086(11) 0.0253(13) -0.0060(9) 0.0045(10) -0.0002(9) O1 0.0377(10) 0.0317(11) 0.0221(10) 0.0062(8) -0.0036(8) -0.0013(8) O2 0.0162(9) 0.0546(14) 0.0532(14) -0.0259(11) 0.0032(9) -0.0118(9) O3 0.0347(10) 0.0122(9) 0.0302(10) -0.0046(7) 0.0022(8) 0.0037(7) O4 0.0925(17) 0.0332(12) 0.0170(11) -0.0069(8) -0.0111(11) 0.0249(11) O5 0.0168(9) 0.0266(10) 0.0596(14) -0.0138(9) 0.0138(9) -0.0048(8) Mo1 0.01026(9) 0.01062(10) 0.01298(10) -0.00219(8) 0.00024(7) 0.00047(7) P1 0.0095(2) 0.0108(3) 0.0091(3) -0.0011(2) 0.0002(2) 0.0004(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 C1 C2 1.330(3) . ? C1 C12 1.481(3) . ? C1 P1 1.849(2) . ? C2 C3 1.537(3) . ? C2 H2 0.9500 . ? C3 C18 1.527(3) . ? C3 C4 1.534(3) . ? C3 C25 1.556(3) . ? C4 C5 1.329(3) . ? C4 H4 0.9500 . ? C5 C6 1.484(3) . ? C5 P1 1.853(2) . ? C6 C7 1.385(3) . ? C6 C11 1.394(3) . ? C7 C8 1.390(3) . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C8 H8 0.9500 . ? C9 C10 1.370(4) . ? C9 H9 0.9500 . ? C10 C11 1.391(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.394(3) . ? C12 C13 1.402(3) . ? C13 C14 1.389(3) . ? C13 H13 0.9500 . ? C14 C15 1.380(3) . ? C14 H14 0.9500 . ? C15 C16 1.384(3) . ? C15 H15 0.9500 . ? C16 C17 1.387(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.386(3) . ? C18 C23 1.403(3) . ? C19 C20 1.394(3) . ? C19 H19 0.9500 . ? C20 C21 1.383(4) . ? C20 H20 0.9500 . ? C21 C22 1.385(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.386(3) . ? C24 C25 1.399(3) . ? C24 P1 1.841(2) . ? C25 C26 1.391(3) . ? C26 C27 1.394(3) . ? C26 H26 0.9500 . ? C27 C28 1.376(3) . ? C27 H27 0.9500 . ? C28 C29 1.396(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 O1 1.139(3) . ? C30 Mo1 2.049(2) . ? C31 O2 1.137(3) . ? C31 Mo1 2.052(2) . ? C32 O3 1.144(3) . ? C32 Mo1 1.998(2) . ? C33 O4 1.137(3) . ? C33 Mo1 2.060(3) . ? C34 O5 1.135(3) . ? C34 Mo1 2.047(2) . ? Mo1 P1 2.5215(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 122.81(19) . . ? C2 C1 P1 113.38(15) . . ? C12 C1 P1 123.60(15) . . ? C1 C2 C3 121.59(19) . . ? C1 C2 H2 119.2 . . ? C3 C2 H2 119.2 . . ? C18 C3 C4 117.29(17) . . ? C18 C3 C2 109.17(17) . . ? C4 C3 C2 106.43(16) . . ? C18 C3 C25 111.85(16) . . ? C4 C3 C25 104.08(16) . . ? C2 C3 C25 107.46(16) . . ? C5 C4 C3 119.88(19) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 124.62(19) . . ? C4 C5 P1 114.91(16) . . ? C6 C5 P1 120.44(15) . . ? C7 C6 C11 118.8(2) . . ? C7 C6 C5 120.40(19) . . ? C11 C6 C5 120.82(19) . . ? C6 C7 C8 120.5(2) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C10 C9 C8 120.1(2) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.2(2) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.4(2) . . ? C10 C11 H11 119.8 . . ? C6 C11 H11 119.8 . . ? C17 C12 C13 118.60(19) . . ? C17 C12 C1 121.97(18) . . ? C13 C12 C1 119.42(19) . . ? C14 C13 C12 120.4(2) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.4(2) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C16 119.7(2) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.5(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.5(2) . . ? C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 C23 118.0(2) . . ? C19 C18 C3 124.6(2) . . ? C23 C18 C3 117.44(19) . . ? C18 C19 C20 120.7(2) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 120.6(2) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.4(2) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 120.0(2) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C18 121.3(2) . . ? C22 C23 H23 119.4 . . ? C18 C23 H23 119.4 . . ? C29 C24 C25 120.53(19) . . ? C29 C24 P1 124.53(17) . . ? C25 C24 P1 114.88(15) . . ? C26 C25 C24 119.07(19) . . ? C26 C25 C3 123.92(19) . . ? C24 C25 C3 116.95(18) . . ? C25 C26 C27 119.9(2) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C28 C27 C26 120.8(2) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 119.7(2) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C24 C29 C28 119.9(2) . . ? C24 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? O1 C30 Mo1 176.9(2) . . ? O2 C31 Mo1 173.1(2) . . ? O3 C32 Mo1 177.9(2) . . ? O4 C33 Mo1 170.5(2) . . ? O5 C34 Mo1 175.5(2) . . ? C32 Mo1 C34 87.27(9) . . ? C32 Mo1 C30 87.00(9) . . ? C34 Mo1 C30 93.44(9) . . ? C32 Mo1 C31 89.32(9) . . ? C34 Mo1 C31 172.70(9) . . ? C30 Mo1 C31 92.83(10) . . ? C32 Mo1 C33 85.75(9) . . ? C34 Mo1 C33 88.41(10) . . ? C30 Mo1 C33 172.42(9) . . ? C31 Mo1 C33 84.89(10) . . ? C32 Mo1 P1 174.26(6) . . ? C34 Mo1 P1 89.69(6) . . ? C30 Mo1 P1 88.33(6) . . ? C31 Mo1 P1 94.24(7) . . ? C33 Mo1 P1 99.04(7) . . ? C24 P1 C1 96.10(9) . . ? C24 P1 C5 94.95(9) . . ? C1 P1 C5 95.84(9) . . ? C24 P1 Mo1 118.08(7) . . ? C1 P1 Mo1 123.31(7) . . ? C5 P1 Mo1 122.01(7) . . ? 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 -174.19(18) . . . . ? P1 C1 C2 C3 0.8(3) . . . . ? C1 C2 C3 C18 -178.07(19) . . . . ? C1 C2 C3 C4 54.4(2) . . . . ? C1 C2 C3 C25 -56.6(2) . . . . ? C18 C3 C4 C5 -176.58(18) . . . . ? C2 C3 C4 C5 -54.1(2) . . . . ? C25 C3 C4 C5 59.3(2) . . . . ? C3 C4 C5 C6 -178.40(18) . . . . ? C3 C4 C5 P1 -0.4(2) . . . . ? C4 C5 C6 C7 86.6(3) . . . . ? P1 C5 C6 C7 -91.3(2) . . . . ? C4 C5 C6 C11 -92.7(3) . . . . ? P1 C5 C6 C11 89.5(2) . . . . ? C11 C6 C7 C8 1.2(4) . . . . ? C5 C6 C7 C8 -178.1(2) . . . . ? C6 C7 C8 C9 -1.1(5) . . . . ? C7 C8 C9 C10 0.0(5) . . . . ? C8 C9 C10 C11 0.9(4) . . . . ? C9 C10 C11 C6 -0.7(4) . . . . ? C7 C6 C11 C10 -0.3(3) . . . . ? C5 C6 C11 C10 179.0(2) . . . . ? C2 C1 C12 C17 -121.4(2) . . . . ? P1 C1 C12 C17 64.2(3) . . . . ? C2 C1 C12 C13 57.5(3) . . . . ? P1 C1 C12 C13 -117.0(2) . . . . ? C17 C12 C13 C14 -0.2(3) . . . . ? C1 C12 C13 C14 -179.11(19) . . . . ? C12 C13 C14 C15 0.0(3) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C14 C15 C16 C17 0.0(3) . . . . ? C15 C16 C17 C12 -0.2(3) . . . . ? C13 C12 C17 C16 0.3(3) . . . . ? C1 C12 C17 C16 179.2(2) . . . . ? C4 C3 C18 C19 -6.5(3) . . . . ? C2 C3 C18 C19 -127.6(2) . . . . ? C25 C3 C18 C19 113.6(2) . . . . ? C4 C3 C18 C23 173.62(18) . . . . ? C2 C3 C18 C23 52.5(2) . . . . ? C25 C3 C18 C23 -66.3(2) . . . . ? C23 C18 C19 C20 0.7(3) . . . . ? C3 C18 C19 C20 -179.1(2) . . . . ? C18 C19 C20 C21 0.1(4) . . . . ? C19 C20 C21 C22 -0.5(4) . . . . ? C20 C21 C22 C23 0.1(3) . . . . ? C21 C22 C23 C18 0.8(3) . . . . ? C19 C18 C23 C22 -1.2(3) . . . . ? C3 C18 C23 C22 178.70(19) . . . . ? C29 C24 C25 C26 4.3(3) . . . . ? P1 C24 C25 C26 -172.93(16) . . . . ? C29 C24 C25 C3 -178.39(19) . . . . ? P1 C24 C25 C3 4.3(2) . . . . ? C18 C3 C25 C26 -11.2(3) . . . . ? C4 C3 C25 C26 116.4(2) . . . . ? C2 C3 C25 C26 -131.0(2) . . . . ? C18 C3 C25 C24 171.71(18) . . . . ? C4 C3 C25 C24 -60.7(2) . . . . ? C2 C3 C25 C24 51.9(2) . . . . ? C24 C25 C26 C27 -3.1(3) . . . . ? C3 C25 C26 C27 179.8(2) . . . . ? C25 C26 C27 C28 -0.5(3) . . . . ? C26 C27 C28 C29 3.0(3) . . . . ? C25 C24 C29 C28 -1.9(3) . . . . ? P1 C24 C29 C28 175.10(17) . . . . ? C27 C28 C29 C24 -1.8(3) . . . . ? C29 C24 P1 C1 132.20(19) . . . . ? C25 C24 P1 C1 -50.65(17) . . . . ? C29 C24 P1 C5 -131.37(19) . . . . ? C25 C24 P1 C5 45.78(17) . . . . ? C29 C24 P1 Mo1 -0.9(2) . . . . ? C25 C24 P1 Mo1 176.27(13) . . . . ? C2 C1 P1 C24 48.20(17) . . . . ? C12 C1 P1 C24 -136.89(17) . . . . ? C2 C1 P1 C5 -47.44(17) . . . . ? C12 C1 P1 C5 127.47(17) . . . . ? C2 C1 P1 Mo1 177.74(12) . . . . ? C12 C1 P1 Mo1 -7.3(2) . . . . ? C4 C5 P1 C24 -48.89(17) . . . . ? C6 C5 P1 C24 129.20(16) . . . . ? C4 C5 P1 C1 47.78(17) . . . . ? C6 C5 P1 C1 -134.14(16) . . . . ? C4 C5 P1 Mo1 -176.58(12) . . . . ? C6 C5 P1 Mo1 1.51(19) . . . . ? _refine_diff_density_max 0.397 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.078 _shelx_res_file ; MK09_a.res created by SHELXL-2014/7 TITL MK09_a.res in P2(1)/c REM Old TITL MK09 in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.172, Rweak 0.009, Alpha 0.047, Orientation as input REM Formula found by SHELXT: C36 O4 Mo CELL 0.71073 11.2067 12.8656 19.9607 90.0000 91.1287 90.0000 ZERR 4.000 0.0002 0.0002 0.0005 0.0000 0.0008 0.0000 LATT 1 SYMM -X, 1/2+Y, 1/2-Z SFAC C H O MO P UNIT 136 84 20 4 4 TEMP -173.130 SIZE 0.140 0.220 0.310 L.S. 30 BOND $H LIST 6 acta conf FMAP 2 PLAN 20 WGHT 0.024500 2.227300 FVAR 0.35413 C1 1 0.622389 0.252479 0.357103 11.00000 0.01007 0.01480 = 0.00903 0.00174 0.00006 0.00082 C2 1 0.622624 0.352600 0.373705 11.00000 0.00964 0.01572 = 0.00966 0.00015 0.00208 0.00071 AFIX 43 H2 2 0.558815 0.379498 0.399107 11.00000 -1.20000 AFIX 0 C3 1 0.723626 0.425814 0.352786 11.00000 0.01242 0.00911 = 0.01160 0.00075 0.00034 -0.00066 C4 1 0.732639 0.416045 0.276473 11.00000 0.00908 0.01330 = 0.01040 0.00325 -0.00036 -0.00191 AFIX 43 H4 2 0.728432 0.476382 0.249093 11.00000 -1.20000 AFIX 0 C5 1 0.746343 0.323032 0.248727 11.00000 0.00845 0.01567 = 0.00940 0.00111 -0.00126 -0.00112 C6 1 0.759094 0.304411 0.175841 11.00000 0.01672 0.01179 = 0.00896 -0.00040 0.00061 0.00028 C7 1 0.870298 0.309216 0.146936 11.00000 0.01809 0.04938 = 0.01585 -0.00989 0.00212 -0.00608 AFIX 43 H7 2 0.939096 0.322450 0.174174 11.00000 -1.20000 AFIX 0 C8 1 0.881972 0.294814 0.078360 11.00000 0.02763 0.06661 = 0.02181 -0.01247 0.01463 -0.01236 AFIX 43 H8 2 0.958401 0.299390 0.058813 11.00000 -1.20000 AFIX 0 C9 1 0.782597 0.273856 0.038596 11.00000 0.04181 0.03669 = 0.00934 -0.00675 0.00600 -0.00613 AFIX 43 H9 2 0.790753 0.264044 -0.008263 11.00000 -1.20000 AFIX 0 C10 1 0.672287 0.267209 0.066673 11.00000 0.02899 0.02085 = 0.01187 -0.00210 -0.00655 0.00128 AFIX 43 H10 2 0.604229 0.251805 0.039329 11.00000 -1.20000 AFIX 0 C11 1 0.659675 0.282958 0.135119 11.00000 0.01568 0.01926 = 0.01349 -0.00077 -0.00035 0.00202 AFIX 43 H11 2 0.582828 0.279067 0.154221 11.00000 -1.20000 AFIX 0 C12 1 0.521165 0.182247 0.371034 11.00000 0.01223 0.01202 = 0.00998 -0.00394 0.00276 -0.00108 C13 1 0.407157 0.206534 0.345374 11.00000 0.01514 0.01518 = 0.01383 -0.00098 0.00142 0.00065 AFIX 43 H13 2 0.395854 0.267120 0.318792 11.00000 -1.20000 AFIX 0 C14 1 0.310652 0.142469 0.358615 11.00000 0.01337 0.02173 = 0.01962 -0.00564 -0.00005 -0.00019 AFIX 43 H14 2 0.233717 0.159519 0.341051 11.00000 -1.20000 AFIX 0 C15 1 0.325888 0.054211 0.397133 11.00000 0.01801 0.01860 = 0.01779 -0.00389 0.00473 -0.00859 AFIX 43 H15 2 0.259719 0.010505 0.405993 11.00000 -1.20000 AFIX 0 C16 1 0.438043 0.029651 0.422803 11.00000 0.02632 0.01707 = 0.01450 0.00073 0.00128 -0.00574 AFIX 43 H16 2 0.448608 -0.031069 0.449345 11.00000 -1.20000 AFIX 0 C17 1 0.535101 0.093057 0.410052 11.00000 0.01692 0.01794 = 0.01360 0.00002 -0.00099 -0.00087 AFIX 43 H17 2 0.611607 0.075569 0.428039 11.00000 -1.20000 AFIX 0 C18 1 0.700803 0.534031 0.381203 11.00000 0.00926 0.01488 = 0.01542 -0.00269 -0.00037 -0.00152 C19 1 0.699215 0.624686 0.343707 11.00000 0.01945 0.01320 = 0.01860 0.00008 0.00565 -0.00069 AFIX 43 H19 2 0.711896 0.621476 0.296834 11.00000 -1.20000 AFIX 0 C20 1 0.679210 0.720518 0.374038 11.00000 0.02589 0.01233 = 0.03154 0.00107 0.00654 0.00100 AFIX 43 H20 2 0.678289 0.781968 0.347644 11.00000 -1.20000 AFIX 0 C21 1 0.660685 0.726984 0.442212 11.00000 0.01977 0.01709 = 0.03288 -0.00885 0.00426 -0.00020 AFIX 43 H21 2 0.647705 0.792547 0.462715 11.00000 -1.20000 AFIX 0 C22 1 0.661228 0.637022 0.480322 11.00000 0.01790 0.02293 = 0.01907 -0.00907 0.00318 -0.00031 AFIX 43 H22 2 0.648493 0.640701 0.527175 11.00000 -1.20000 AFIX 0 C23 1 0.680320 0.541770 0.450156 11.00000 0.02006 0.01525 = 0.01576 -0.00259 0.00128 -0.00163 AFIX 43 H23 2 0.679544 0.480431 0.476640 11.00000 -1.20000 AFIX 0 C24 1 0.865790 0.274847 0.364697 11.00000 0.01074 0.01558 = 0.00704 0.00036 0.00234 -0.00306 C25 1 0.843001 0.378967 0.380108 11.00000 0.01250 0.01624 = 0.00656 0.00164 0.00300 -0.00150 C26 1 0.928821 0.435486 0.415855 11.00000 0.01721 0.01661 = 0.01203 -0.00246 0.00145 -0.00184 AFIX 43 H26 2 0.916337 0.507158 0.424770 11.00000 -1.20000 AFIX 0 C27 1 1.033126 0.386848 0.438574 11.00000 0.01315 0.02849 = 0.01149 -0.00571 -0.00070 -0.00339 AFIX 43 H27 2 1.091759 0.425925 0.462622 11.00000 -1.20000 AFIX 0 C28 1 1.052172 0.282924 0.426583 11.00000 0.01184 0.02930 = 0.01287 -0.00117 -0.00092 0.00213 AFIX 43 H28 2 1.121751 0.249683 0.444106 11.00000 -1.20000 AFIX 0 C29 1 0.968726 0.226551 0.388532 11.00000 0.01312 0.01893 = 0.01079 0.00005 0.00174 0.00043 AFIX 43 H29 2 0.982463 0.155253 0.378997 11.00000 -1.20000 AFIX 0 C30 1 0.820572 -0.010091 0.369726 11.00000 0.01787 0.01422 = 0.02145 -0.00024 -0.00047 -0.00219 C31 1 0.614441 -0.012639 0.273838 11.00000 0.02067 0.02410 = 0.02350 -0.01196 0.00073 0.00103 C32 1 0.832716 -0.117729 0.248931 11.00000 0.01554 0.01911 = 0.01361 0.00122 0.00048 -0.00308 C33 1 0.760106 0.047619 0.169927 11.00000 0.03622 0.01634 = 0.02362 -0.00271 -0.00262 0.01123 C34 1 0.966348 0.065187 0.256143 11.00000 0.02155 0.00860 = 0.02534 -0.00601 0.00446 -0.00024 O1 3 0.836829 -0.036521 0.423610 11.00000 0.03768 0.03167 = 0.02213 0.00620 -0.00361 -0.00126 O2 3 0.518669 -0.041340 0.269596 11.00000 0.01617 0.05458 = 0.05318 -0.02588 0.00325 -0.01179 O3 3 0.859183 -0.201745 0.237696 11.00000 0.03473 0.01223 = 0.03018 -0.00463 0.00224 0.00373 O4 3 0.742600 0.043231 0.113715 11.00000 0.09247 0.03317 = 0.01699 -0.00686 -0.01113 0.02494 O5 3 1.063361 0.080777 0.244328 11.00000 0.01678 0.02662 = 0.05962 -0.01383 0.01381 -0.00483 MO1 4 0.791051 0.029074 0.271272 11.00000 0.01026 0.01062 = 0.01298 -0.00219 0.00024 0.00047 P1 5 0.754032 0.213228 0.308767 11.00000 0.00952 0.01079 = 0.00911 -0.00110 0.00018 0.00039 HKLF 4 REM MK09_a.res in P2(1)/c REM R1 = 0.0286 for 4924 Fo > 4sig(Fo) and 0.0405 for all 5859 data REM 370 parameters refined using 0 restraints END WGHT 0.0245 2.2273 REM Highest difference peak 0.397, deepest hole -0.462, 1-sigma level 0.078 Q1 1 0.6818 0.3814 0.3611 11.00000 0.05 0.40 Q2 1 0.6005 0.3038 0.3473 11.00000 0.05 0.37 Q3 1 0.4755 0.1789 0.3429 11.00000 0.05 0.37 Q4 1 0.9271 0.2613 0.3683 11.00000 0.05 0.36 Q5 1 0.7135 0.4907 0.3694 11.00000 0.05 0.35 Q6 1 0.7158 0.3080 0.1546 11.00000 0.05 0.35 Q7 1 0.5774 0.2200 0.3637 11.00000 0.05 0.34 Q8 1 0.8234 0.2529 0.3426 11.00000 0.05 0.33 Q9 1 0.7642 0.1368 0.2845 11.00000 0.05 0.33 Q10 1 0.7838 0.3938 0.3675 11.00000 0.05 0.33 Q11 1 0.6729 0.2399 0.3385 11.00000 0.05 0.32 Q12 1 0.8434 0.3198 0.3770 11.00000 0.05 0.31 Q13 1 0.8058 0.3000 0.1606 11.00000 0.05 0.30 Q14 1 0.7390 0.5679 0.3666 11.00000 0.05 0.30 Q15 1 0.6610 0.5651 0.3582 11.00000 0.05 0.29 Q16 1 0.6202 0.2947 0.1427 11.00000 0.05 0.29 Q17 1 1.0191 0.2594 0.3965 11.00000 0.05 0.28 Q18 1 1.0112 -0.0006 0.3838 11.00000 0.05 0.28 Q19 1 0.8270 -0.0633 0.2357 11.00000 0.05 0.27 Q20 1 0.7281 0.4262 0.3174 11.00000 0.05 0.27 ; _shelx_res_checksum 96454 _shelx_hkl_file ; -2 0 0 9999.00 250.47 -3 0 0 16.90 2.90 3 0 0 18.70 3.10 3 0 0 17.50 3.10 -3 0 0 17.60 2.70 -3 0 0 16.80 3.10 -4 0 0 925.71 28.00 -4 0 0 957.20 27.90 4 0 0 921.81 28.10 -4 0 0 957.70 28.00 -5 0 0 218.08 11.60 -5 0 0 217.38 11.30 5 0 0 235.68 12.00 -5 0 0 199.68 10.90 -6 0 0 49.50 6.80 6 0 0 56.99 7.40 -6 0 0 60.29 7.60 -6 0 0 69.09 7.80 -7 0 0 983.00 32.90 -7 0 0 947.61 32.60 -7 0 0 975.30 32.60 7 0 0 935.61 33.00 -8 0 0 55.19 9.20 8 0 0 46.60 9.10 -8 0 0 54.39 8.50 -8 0 0 51.69 8.50 9 0 0 162.38 20.90 -9 0 0 160.38 14.90 -9 0 0 158.68 15.10 -9 0 0 155.98 15.20 -10 0 0 5.40 8.30 -10 0 0 7.00 8.10 10 0 0 4.30 9.10 -11 0 0 534.25 28.60 -11 0 0 552.84 30.60 -11 0 0 529.25 29.10 -12 0 0 197.18 22.10 12 0 0 173.08 21.80 -12 0 0 217.38 23.00 13 0 0 -18.30 16.70 -13 0 0 13.20 12.90 -13 0 0 -3.80 15.70 -13 0 0 31.50 20.80 -14 0 0 -1.50 15.30 -1 -1 0 2318.57 54.89 1 -1 0 2175.88 52.99 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22.60 -7 2 0 639.34 25.30 -7 2 0 613.84 22.70 -8 -2 0 1413.46 43.10 -8 -2 0 1359.36 46.20 -8 -2 0 1394.96 46.40 8 -2 0 1414.36 44.00 8 2 0 1370.86 48.20 -8 2 0 1442.36 46.20 -8 2 0 1336.77 42.90 -8 2 0 1399.36 42.70 -9 -2 0 -5.80 6.30 -9 -2 0 4.50 7.10 -9 -2 0 14.10 9.00 9 -2 0 6.00 6.90 -9 2 0 6.50 8.50 -9 2 0 14.90 6.90 -9 2 0 5.90 6.20 9 2 0 11.00 8.70 -10 -2 0 1068.99 40.60 -10 -2 0 1031.00 41.60 10 -2 0 1078.79 39.80 -10 -2 0 1101.99 42.80 -10 2 0 1108.09 38.30 -10 2 0 1044.00 41.50 -10 2 0 1120.89 39.70 -11 -2 0 65.29 12.90 -11 -2 0 53.49 13.40 -11 2 0 38.30 10.70 -11 2 0 48.90 13.00 -12 -2 0 621.74 36.10 12 -2 0 381.96 29.90 -12 -2 0 592.44 30.80 -12 -2 0 542.65 32.50 12 2 0 437.26 33.60 -12 2 0 508.55 30.70 -12 2 0 499.55 27.50 -12 2 0 377.96 31.50 -13 -2 0 54.59 20.10 -13 -2 0 10.60 14.20 -13 -2 0 4.20 15.00 13 -2 0 -0.40 15.50 13 2 0 -0.10 18.70 -13 2 0 41.40 16.30 -13 2 0 -5.00 11.30 -13 2 0 -8.20 15.90 0 -3 0 -0.30 1.20 0 -3 0 -0.10 1.20 0 3 0 -2.00 1.10 0 3 0 -0.10 1.20 1 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6.80 -7 3 0 10.60 4.30 -8 -3 0 36.90 9.60 8 -3 0 42.20 7.40 -8 -3 0 47.10 9.70 -8 -3 0 26.00 6.20 -8 3 0 45.80 7.60 -8 3 0 34.50 9.90 -8 3 0 34.10 6.50 -9 -3 0 190.68 17.80 -9 -3 0 196.98 18.90 9 -3 0 204.98 19.10 -9 -3 0 207.18 14.90 -9 3 0 171.68 17.10 9 3 0 199.68 18.70 -9 3 0 199.78 14.00 -9 3 0 208.98 15.00 -10 -3 0 9.00 7.50 -10 -3 0 0.80 9.20 10 -3 0 11.40 8.60 -10 3 0 8.50 7.90 -10 3 0 5.20 6.40 -10 3 0 4.50 10.50 11 -3 0 173.48 19.60 -11 -3 0 161.08 22.70 -11 -3 0 159.48 19.90 -11 -3 0 150.48 18.70 -11 3 0 121.19 15.10 -12 -3 0 43.50 15.00 -12 -3 0 45.90 17.00 12 -3 0 3.20 12.40 -12 -3 0 30.20 12.10 -12 3 0 35.00 10.70 -12 3 0 20.20 16.10 -12 3 0 39.90 13.40 12 3 0 -4.00 15.50 13 -3 0 317.37 28.70 -13 -3 0 255.77 28.70 -13 -3 0 265.87 30.60 -13 3 0 269.87 33.20 -13 3 0 289.77 24.50 -13 3 0 225.48 28.60 13 3 0 316.27 36.70 0 -4 0 6251.67 166.88 0 -4 0 7155.48 165.28 0 4 0 7121.99 165.38 0 4 0 7068.69 165.58 -1 -4 0 0.10 2.00 1 -4 0 3.00 1.10 -1 -4 0 -0.30 2.00 1 4 0 0.70 2.20 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32.30 0 4 24 251.27 30.00 0 4 -24 263.07 28.60 1 -4 24 17.00 17.00 1 -4 24 23.20 18.50 -1 -4 -24 39.70 20.00 1 4 24 18.70 20.60 -1 4 -24 46.60 19.70 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 97522 #============================================================================== _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 ; 'Kleoff, Merlin' ; 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====================================================