data_MR262_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 O P' _chemical_formula_weight 416.43 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' _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 2ab' _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+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 29.6409(5) _cell_length_b 7.40940(10) _cell_length_c 19.1055(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4195.97(11) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9931 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.03 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_F_000 1744 _exptl_transmission_factor_min 0.6117 _exptl_transmission_factor_max 0.9705 _exptl_crystal_size_max 0.430 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 0.150 _shelx_estimated_absorpt_T_min 0.938 _shelx_estimated_absorpt_T_max 0.991 _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 23744 _diffrn_reflns_av_unetI/netI 0.0474 _diffrn_reflns_av_R_equivalents 0.0656 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.240 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_full 25.009 _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 3702 _reflns_number_gt 2980 _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^)+(0.0409P)^2^+2.9708P] 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 3702 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 0.36139(6) 0.7534(2) 0.39219(10) 0.0137(4) Uani 1 1 d . . . . . C2 C 0.37275(6) 0.6223(3) 0.34718(10) 0.0139(4) Uani 1 1 d . . . . . H2 H 0.3614 0.6246 0.3007 0.017 Uiso 1 1 calc R U . . . C3 C 0.40408(6) 0.4680(2) 0.37061(10) 0.0125(4) Uani 1 1 d . . . . . C4 C 0.38149(6) 0.3849(3) 0.43567(10) 0.0126(4) Uani 1 1 d . . . . . H4 H 0.3749 0.2594 0.4362 0.015 Uiso 1 1 calc R U . . . C5 C 0.37096(6) 0.4851(3) 0.49134(10) 0.0124(4) Uani 1 1 d . . . . . C6 C 0.34731(6) 0.4227(3) 0.55486(10) 0.0135(4) Uani 1 1 d . . . . . C7 C 0.35056(7) 0.2427(2) 0.57612(10) 0.0150(4) Uani 1 1 d . . . . . H7 H 0.3689 0.1613 0.5503 0.018 Uiso 1 1 calc R U . . . C8 C 0.32744(7) 0.1820(3) 0.63400(10) 0.0191(5) Uani 1 1 d . . . . . H8 H 0.3297 0.0589 0.6475 0.023 Uiso 1 1 calc R U . . . C9 C 0.30083(7) 0.2991(3) 0.67281(11) 0.0204(5) Uani 1 1 d . . . . . H9 H 0.2853 0.2572 0.7132 0.024 Uiso 1 1 calc R U . . . C10 C 0.29714(7) 0.4767(3) 0.65234(11) 0.0214(5) Uani 1 1 d . . . . . H10 H 0.2786 0.5568 0.6784 0.026 Uiso 1 1 calc R U . . . C11 C 0.32017(7) 0.5399(3) 0.59414(10) 0.0184(5) Uani 1 1 d . . . . . H11 H 0.3175 0.6630 0.5809 0.022 Uiso 1 1 calc R U . . . C12 C 0.33228(6) 0.9107(2) 0.37805(10) 0.0137(4) Uani 1 1 d . . . . . C13 C 0.30559(6) 0.9874(3) 0.43023(11) 0.0160(4) Uani 1 1 d . . . . . H13 H 0.3064 0.9391 0.4763 0.019 Uiso 1 1 calc R U . . . C14 C 0.27785(7) 1.1331(3) 0.41578(11) 0.0198(5) Uani 1 1 d . . . . . H14 H 0.2596 1.1832 0.4517 0.024 Uiso 1 1 calc R U . . . C15 C 0.27669(7) 1.2061(3) 0.34904(11) 0.0232(5) Uani 1 1 d . . . . . H15 H 0.2580 1.3072 0.3392 0.028 Uiso 1 1 calc R U . . . C16 C 0.30302(7) 1.1303(3) 0.29687(11) 0.0201(5) Uani 1 1 d . . . . . H16 H 0.3019 1.1782 0.2508 0.024 Uiso 1 1 calc R U . . . C17 C 0.33082(6) 0.9856(3) 0.31129(10) 0.0165(4) Uani 1 1 d . . . . . H17 H 0.3492 0.9366 0.2752 0.020 Uiso 1 1 calc R U . . . C18 C 0.41361(6) 0.3234(3) 0.31586(10) 0.0129(4) Uani 1 1 d . . . . . C19 C 0.43471(6) 0.1639(3) 0.33775(10) 0.0160(4) Uani 1 1 d . . . . . H19 H 0.4416 0.1481 0.3859 0.019 Uiso 1 1 calc R U . . . C20 C 0.44566(7) 0.0294(3) 0.29076(11) 0.0197(5) Uani 1 1 d . . . . . H20 H 0.4600 -0.0776 0.3066 0.024 Uiso 1 1 calc R U . . . C21 C 0.43563(7) 0.0507(3) 0.22015(11) 0.0220(5) Uani 1 1 d . . . . . H21 H 0.4429 -0.0417 0.1876 0.026 Uiso 1 1 calc R U . . . C22 C 0.41490(7) 0.2077(3) 0.19771(11) 0.0211(5) Uani 1 1 d . . . . . H22 H 0.4079 0.2228 0.1495 0.025 Uiso 1 1 calc R U . . . C23 C 0.40429(7) 0.3432(3) 0.24503(10) 0.0171(5) Uani 1 1 d . . . . . H23 H 0.3905 0.4510 0.2288 0.021 Uiso 1 1 calc R U . . . C24 C 0.44478(6) 0.6838(3) 0.44850(10) 0.0139(4) Uani 1 1 d . . . . . C25 C 0.44888(6) 0.5587(2) 0.39447(10) 0.0129(4) Uani 1 1 d . . . . . C26 C 0.49129(6) 0.5270(3) 0.36590(10) 0.0150(4) Uani 1 1 d . . . . . H26 H 0.4948 0.4433 0.3287 0.018 Uiso 1 1 calc R U . . . C27 C 0.52849(7) 0.6192(3) 0.39239(11) 0.0193(5) Uani 1 1 d . . . . . H27 H 0.5575 0.5978 0.3729 0.023 Uiso 1 1 calc R U . . . C28 C 0.52389(7) 0.7416(3) 0.44678(11) 0.0197(5) Uani 1 1 d . . . . . H28 H 0.5496 0.8028 0.4645 0.024 Uiso 1 1 calc R U . . . C29 C 0.48177(7) 0.7744(3) 0.47527(10) 0.0167(4) Uani 1 1 d . . . . . H29 H 0.4783 0.8578 0.5126 0.020 Uiso 1 1 calc R U . . . O1 O 0.38122(5) 0.85353(18) 0.53314(7) 0.0177(3) Uani 1 1 d . . . . . P1 P 0.38781(2) 0.71824(7) 0.47734(3) 0.01270(15) 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 0.0126(10) 0.0125(10) 0.0160(10) 0.0018(8) -0.0002(8) -0.0017(8) C2 0.0142(10) 0.0143(10) 0.0131(10) 0.0026(8) -0.0024(8) -0.0013(8) C3 0.0123(10) 0.0118(10) 0.0133(10) -0.0004(8) -0.0006(8) -0.0012(8) C4 0.0111(10) 0.0099(10) 0.0168(10) 0.0011(8) -0.0020(8) -0.0010(8) C5 0.0094(9) 0.0108(10) 0.0170(10) -0.0010(8) -0.0021(8) 0.0015(8) C6 0.0112(10) 0.0136(10) 0.0157(10) -0.0024(8) -0.0008(8) -0.0018(8) C7 0.0143(10) 0.0120(10) 0.0188(10) -0.0031(8) 0.0004(8) 0.0018(8) C8 0.0216(11) 0.0150(11) 0.0207(11) 0.0025(9) 0.0009(9) -0.0029(9) C9 0.0187(11) 0.0230(11) 0.0194(11) -0.0018(9) 0.0052(9) -0.0054(9) C10 0.0185(11) 0.0217(11) 0.0240(12) -0.0071(9) 0.0071(9) 0.0007(9) C11 0.0167(11) 0.0130(10) 0.0256(11) -0.0009(9) 0.0004(9) 0.0007(8) C12 0.0101(10) 0.0111(10) 0.0199(11) -0.0004(8) -0.0029(8) -0.0026(8) C13 0.0138(10) 0.0144(10) 0.0198(11) -0.0001(9) -0.0022(8) -0.0016(8) C14 0.0158(11) 0.0191(11) 0.0245(12) -0.0065(9) -0.0014(9) 0.0025(9) C15 0.0181(11) 0.0177(11) 0.0336(13) 0.0004(10) -0.0058(10) 0.0067(9) C16 0.0180(11) 0.0185(11) 0.0237(11) 0.0048(9) -0.0035(9) 0.0004(9) C17 0.0120(10) 0.0150(10) 0.0224(11) 0.0004(9) 0.0001(9) 0.0007(8) C18 0.0094(10) 0.0149(10) 0.0145(10) -0.0025(8) 0.0014(8) -0.0042(8) C19 0.0139(10) 0.0177(11) 0.0163(11) -0.0024(9) 0.0018(9) -0.0021(8) C20 0.0158(11) 0.0152(11) 0.0280(12) -0.0026(9) 0.0047(9) 0.0002(8) C21 0.0183(11) 0.0229(12) 0.0247(12) -0.0104(10) 0.0077(9) -0.0040(9) C22 0.0182(11) 0.0291(12) 0.0159(11) -0.0039(10) 0.0025(9) -0.0042(9) C23 0.0157(10) 0.0188(11) 0.0169(11) 0.0005(9) 0.0012(9) -0.0034(8) C24 0.0174(11) 0.0097(10) 0.0145(10) 0.0039(8) -0.0026(8) -0.0005(8) C25 0.0143(10) 0.0099(10) 0.0144(10) 0.0044(8) -0.0024(8) -0.0014(8) C26 0.0163(11) 0.0118(10) 0.0170(10) 0.0029(8) 0.0001(8) -0.0001(8) C27 0.0142(11) 0.0181(11) 0.0255(12) 0.0047(9) 0.0004(9) 0.0007(9) C28 0.0156(11) 0.0161(11) 0.0273(12) 0.0015(9) -0.0060(9) -0.0042(9) C29 0.0200(11) 0.0114(10) 0.0189(10) 0.0005(9) -0.0045(9) -0.0020(8) O1 0.0237(8) 0.0118(7) 0.0178(7) -0.0031(6) -0.0029(6) 0.0016(6) P1 0.0145(3) 0.0087(3) 0.0149(3) -0.0004(2) -0.0020(2) 0.0005(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 1.340(3) . ? C1 C12 1.475(3) . ? C1 P1 1.8241(19) . ? C2 C3 1.539(3) . ? C2 H2 0.9500 . ? C3 C18 1.524(3) . ? C3 C4 1.540(3) . ? C3 C25 1.557(3) . ? C4 C5 1.334(3) . ? C4 H4 0.9500 . ? C5 C6 1.476(3) . ? C5 P1 1.8181(19) . ? C6 C7 1.398(3) . ? C6 C11 1.402(3) . ? C7 C8 1.376(3) . ? C7 H7 0.9500 . ? C8 C9 1.388(3) . ? C8 H8 0.9500 . ? C9 C10 1.377(3) . ? C9 H9 0.9500 . ? C10 C11 1.386(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.392(3) . ? C12 C13 1.394(3) . ? C13 C14 1.385(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.380(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.389(3) . ? C18 C19 1.401(3) . ? C19 C20 1.380(3) . ? C19 H19 0.9500 . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.383(3) . ? C24 C25 1.393(3) . ? C24 P1 1.795(2) . ? C25 C26 1.390(3) . ? C26 C27 1.392(3) . ? C26 H26 0.9500 . ? C27 C28 1.386(3) . ? C27 H27 0.9500 . ? C28 C29 1.384(3) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? O1 P1 1.4764(14) . ? 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 127.03(18) . . ? C2 C1 P1 111.15(14) . . ? C12 C1 P1 121.81(14) . . ? C1 C2 C3 120.22(17) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C18 C3 C4 110.70(15) . . ? C18 C3 C2 115.75(16) . . ? C4 C3 C2 105.62(15) . . ? C18 C3 C25 110.28(15) . . ? C4 C3 C25 107.88(15) . . ? C2 C3 C25 106.20(15) . . ? C5 C4 C3 121.51(17) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 126.33(17) . . ? C4 C5 P1 110.31(14) . . ? C6 C5 P1 123.31(14) . . ? C7 C6 C11 118.39(18) . . ? C7 C6 C5 120.35(17) . . ? C11 C6 C5 121.24(17) . . ? C8 C7 C6 120.73(18) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.53(19) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C10 C9 C8 119.40(19) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 120.78(19) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C6 120.16(18) . . ? C10 C11 H11 119.9 . . ? C6 C11 H11 119.9 . . ? C17 C12 C13 118.39(18) . . ? C17 C12 C1 120.06(17) . . ? C13 C12 C1 121.55(17) . . ? C14 C13 C12 120.81(19) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 120.17(19) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.33(19) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.54(19) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C12 120.75(19) . . ? C16 C17 H17 119.6 . . ? C12 C17 H17 119.6 . . ? C23 C18 C19 117.96(18) . . ? C23 C18 C3 123.90(17) . . ? C19 C18 C3 118.09(16) . . ? C20 C19 C18 121.33(18) . . ? C20 C19 H19 119.3 . . ? C18 C19 H19 119.3 . . ? C19 C20 C21 119.92(19) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 119.41(19) . . ? C22 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C23 C22 C21 120.47(19) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 120.90(19) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? C29 C24 C25 121.85(18) . . ? C29 C24 P1 124.29(15) . . ? C25 C24 P1 113.84(14) . . ? C26 C25 C24 118.83(17) . . ? C26 C25 C3 125.68(17) . . ? C24 C25 C3 115.48(16) . . ? C25 C26 C27 119.37(18) . . ? C25 C26 H26 120.3 . . ? C27 C26 H26 120.3 . . ? C28 C27 C26 121.04(19) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C29 C28 C27 119.91(19) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C24 C29 C28 118.98(19) . . ? C24 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? O1 P1 C24 116.27(9) . . ? O1 P1 C5 120.17(8) . . ? C24 P1 C5 99.71(9) . . ? O1 P1 C1 119.36(8) . . ? C24 P1 C1 98.65(9) . . ? C5 P1 C1 98.57(9) . . ? 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 179.38(17) . . . . ? P1 C1 C2 C3 0.4(2) . . . . ? C1 C2 C3 C18 178.24(17) . . . . ? C1 C2 C3 C4 55.4(2) . . . . ? C1 C2 C3 C25 -59.0(2) . . . . ? C18 C3 C4 C5 178.36(17) . . . . ? C2 C3 C4 C5 -55.6(2) . . . . ? C25 C3 C4 C5 57.6(2) . . . . ? C3 C4 C5 C6 176.72(17) . . . . ? C3 C4 C5 P1 -0.8(2) . . . . ? C4 C5 C6 C7 27.8(3) . . . . ? P1 C5 C6 C7 -154.92(15) . . . . ? C4 C5 C6 C11 -150.4(2) . . . . ? P1 C5 C6 C11 26.9(3) . . . . ? C11 C6 C7 C8 0.4(3) . . . . ? C5 C6 C7 C8 -177.86(18) . . . . ? C6 C7 C8 C9 -0.7(3) . . . . ? C7 C8 C9 C10 1.0(3) . . . . ? C8 C9 C10 C11 -0.9(3) . . . . ? C9 C10 C11 C6 0.6(3) . . . . ? C7 C6 C11 C10 -0.3(3) . . . . ? C5 C6 C11 C10 177.91(18) . . . . ? C2 C1 C12 C17 -30.9(3) . . . . ? P1 C1 C12 C17 147.99(16) . . . . ? C2 C1 C12 C13 148.8(2) . . . . ? P1 C1 C12 C13 -32.3(2) . . . . ? C17 C12 C13 C14 0.8(3) . . . . ? C1 C12 C13 C14 -178.87(18) . . . . ? C12 C13 C14 C15 -0.7(3) . . . . ? C13 C14 C15 C16 0.9(3) . . . . ? C14 C15 C16 C17 -1.2(3) . . . . ? C15 C16 C17 C12 1.3(3) . . . . ? C13 C12 C17 C16 -1.1(3) . . . . ? C1 C12 C17 C16 178.57(18) . . . . ? C4 C3 C18 C23 134.58(19) . . . . ? C2 C3 C18 C23 14.5(3) . . . . ? C25 C3 C18 C23 -106.1(2) . . . . ? C4 C3 C18 C19 -48.2(2) . . . . ? C2 C3 C18 C19 -168.29(16) . . . . ? C25 C3 C18 C19 71.2(2) . . . . ? C23 C18 C19 C20 -0.5(3) . . . . ? C3 C18 C19 C20 -177.96(17) . . . . ? C18 C19 C20 C21 -0.2(3) . . . . ? C19 C20 C21 C22 0.3(3) . . . . ? C20 C21 C22 C23 0.2(3) . . . . ? C21 C22 C23 C18 -0.9(3) . . . . ? C19 C18 C23 C22 1.1(3) . . . . ? C3 C18 C23 C22 178.34(18) . . . . ? C29 C24 C25 C26 -1.3(3) . . . . ? P1 C24 C25 C26 177.26(14) . . . . ? C29 C24 C25 C3 179.71(17) . . . . ? P1 C24 C25 C3 -1.8(2) . . . . ? C18 C3 C25 C26 5.8(3) . . . . ? C4 C3 C25 C26 126.81(19) . . . . ? C2 C3 C25 C26 -120.3(2) . . . . ? C18 C3 C25 C24 -175.25(16) . . . . ? C4 C3 C25 C24 -54.2(2) . . . . ? C2 C3 C25 C24 58.6(2) . . . . ? C24 C25 C26 C27 0.7(3) . . . . ? C3 C25 C26 C27 179.62(17) . . . . ? C25 C26 C27 C28 0.1(3) . . . . ? C26 C27 C28 C29 -0.4(3) . . . . ? C25 C24 C29 C28 1.0(3) . . . . ? P1 C24 C29 C28 -177.38(15) . . . . ? C27 C28 C29 C24 -0.2(3) . . . . ? C29 C24 P1 O1 0.2(2) . . . . ? C25 C24 P1 O1 -178.25(13) . . . . ? C29 C24 P1 C5 -130.53(17) . . . . ? C25 C24 P1 C5 50.98(15) . . . . ? C29 C24 P1 C1 129.16(17) . . . . ? C25 C24 P1 C1 -49.33(15) . . . . ? C4 C5 P1 O1 -177.55(13) . . . . ? C6 C5 P1 O1 4.80(19) . . . . ? C4 C5 P1 C24 -49.31(15) . . . . ? C6 C5 P1 C24 133.04(16) . . . . ? C4 C5 P1 C1 51.06(15) . . . . ? C6 C5 P1 C1 -126.59(16) . . . . ? C2 C1 P1 O1 177.00(13) . . . . ? C12 C1 P1 O1 -2.05(19) . . . . ? C2 C1 P1 C24 50.17(16) . . . . ? C12 C1 P1 C24 -128.87(16) . . . . ? C2 C1 P1 C5 -51.10(15) . . . . ? C12 C1 P1 C5 129.86(16) . . . . ? _refine_diff_density_max 0.313 _refine_diff_density_min -0.415 _refine_diff_density_rms 0.053 _shelx_res_file ; MR262_a.res created by SHELXL-2014/7 TITL MR262_a.res in Pbcn REM Old TITL MR262 in Pbcn REM SHELXT solution in Pbcn REM R1 0.109, Rweak 0.004, Alpha 0.024, Orientation as input REM Formula found by SHELXT: C29 O P CELL 0.71073 29.6409 7.4094 19.1055 90.000 90.000 90.000 ZERR 8.000 0.0005 0.0001 0.0003 0.000 0.000 0.000 LATT 1 SYMM 1/2-X, 1/2-Y, 1/2+Z SYMM -X, Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H O P UNIT 232 168 8 8 TEMP -173.150 SIZE 0.06 0.30 0.43 L.S. 30 BOND $H acta conf LIST 6 FMAP 2 PLAN 20 WGHT 0.040900 2.970800 FVAR 0.32833 C1 1 0.361394 0.753398 0.392187 11.00000 0.01256 0.01246 = 0.01603 0.00178 -0.00023 -0.00169 C2 1 0.372751 0.622276 0.347185 11.00000 0.01419 0.01434 = 0.01312 0.00263 -0.00239 -0.00128 AFIX 43 H2 2 0.361428 0.624571 0.300676 11.00000 -1.20000 AFIX 0 C3 1 0.404081 0.467965 0.370609 11.00000 0.01231 0.01175 = 0.01334 -0.00039 -0.00056 -0.00118 C4 1 0.381494 0.384870 0.435665 11.00000 0.01107 0.00994 = 0.01680 0.00108 -0.00199 -0.00100 AFIX 43 H4 2 0.374914 0.259393 0.436163 11.00000 -1.20000 AFIX 0 C5 1 0.370957 0.485078 0.491340 11.00000 0.00940 0.01080 = 0.01700 -0.00100 -0.00205 0.00149 C6 1 0.347313 0.422668 0.554864 11.00000 0.01122 0.01360 = 0.01570 -0.00236 -0.00075 -0.00175 C7 1 0.350564 0.242655 0.576123 11.00000 0.01428 0.01199 = 0.01884 -0.00309 0.00039 0.00184 AFIX 43 H7 2 0.368935 0.161289 0.550347 11.00000 -1.20000 AFIX 0 C8 1 0.327441 0.181957 0.633998 11.00000 0.02160 0.01505 = 0.02072 0.00255 0.00090 -0.00286 AFIX 43 H8 2 0.329720 0.058878 0.647476 11.00000 -1.20000 AFIX 0 C9 1 0.300829 0.299089 0.672814 11.00000 0.01868 0.02302 = 0.01942 -0.00185 0.00516 -0.00545 AFIX 43 H9 2 0.285297 0.257151 0.713153 11.00000 -1.20000 AFIX 0 C10 1 0.297136 0.476658 0.652338 11.00000 0.01852 0.02169 = 0.02400 -0.00713 0.00709 0.00072 AFIX 43 H10 2 0.278587 0.556765 0.678398 11.00000 -1.20000 AFIX 0 C11 1 0.320168 0.539915 0.594144 11.00000 0.01672 0.01296 = 0.02560 -0.00095 0.00037 0.00067 AFIX 43 H11 2 0.317548 0.663019 0.580851 11.00000 -1.20000 AFIX 0 C12 1 0.332278 0.910749 0.378054 11.00000 0.01014 0.01111 = 0.01992 -0.00035 -0.00294 -0.00263 C13 1 0.305585 0.987416 0.430228 11.00000 0.01379 0.01436 = 0.01984 -0.00005 -0.00217 -0.00165 AFIX 43 H13 2 0.306426 0.939116 0.476270 11.00000 -1.20000 AFIX 0 C14 1 0.277852 1.133137 0.415779 11.00000 0.01581 0.01914 = 0.02449 -0.00650 -0.00144 0.00249 AFIX 43 H14 2 0.259579 1.183188 0.451724 11.00000 -1.20000 AFIX 0 C15 1 0.276686 1.206121 0.349041 11.00000 0.01814 0.01774 = 0.03361 0.00040 -0.00579 0.00673 AFIX 43 H15 2 0.258014 1.307166 0.339158 11.00000 -1.20000 AFIX 0 C16 1 0.303022 1.130266 0.296872 11.00000 0.01801 0.01850 = 0.02372 0.00483 -0.00348 0.00037 AFIX 43 H16 2 0.301934 1.178231 0.250789 11.00000 -1.20000 AFIX 0 C17 1 0.330821 0.985616 0.311293 11.00000 0.01201 0.01504 = 0.02238 0.00036 0.00011 0.00067 AFIX 43 H17 2 0.349174 0.936571 0.275238 11.00000 -1.20000 AFIX 0 C18 1 0.413606 0.323373 0.315858 11.00000 0.00939 0.01493 = 0.01450 -0.00249 0.00145 -0.00422 C19 1 0.434707 0.163934 0.337748 11.00000 0.01386 0.01774 = 0.01632 -0.00242 0.00181 -0.00213 AFIX 43 H19 2 0.441620 0.148070 0.385910 11.00000 -1.20000 AFIX 0 C20 1 0.445659 0.029402 0.290761 11.00000 0.01581 0.01522 = 0.02801 -0.00259 0.00470 0.00021 AFIX 43 H20 2 0.460035 -0.077624 0.306644 11.00000 -1.20000 AFIX 0 C21 1 0.435625 0.050701 0.220151 11.00000 0.01828 0.02286 = 0.02472 -0.01043 0.00769 -0.00397 AFIX 43 H21 2 0.442935 -0.041716 0.187604 11.00000 -1.20000 AFIX 0 C22 1 0.414896 0.207733 0.197710 11.00000 0.01822 0.02909 = 0.01590 -0.00389 0.00245 -0.00417 AFIX 43 H22 2 0.407878 0.222850 0.149548 11.00000 -1.20000 AFIX 0 C23 1 0.404294 0.343193 0.245027 11.00000 0.01574 0.01881 = 0.01686 0.00046 0.00120 -0.00343 AFIX 43 H23 2 0.390473 0.451013 0.228770 11.00000 -1.20000 AFIX 0 C24 1 0.444782 0.683824 0.448505 11.00000 0.01741 0.00970 = 0.01450 0.00393 -0.00260 -0.00049 C25 1 0.448879 0.558705 0.394472 11.00000 0.01431 0.00989 = 0.01441 0.00442 -0.00237 -0.00143 C26 1 0.491287 0.527009 0.365902 11.00000 0.01628 0.01176 = 0.01697 0.00292 0.00010 -0.00011 AFIX 43 H26 2 0.494844 0.443260 0.328658 11.00000 -1.20000 AFIX 0 C27 1 0.528485 0.619159 0.392389 11.00000 0.01418 0.01811 = 0.02555 0.00471 0.00036 0.00072 AFIX 43 H27 2 0.557477 0.597803 0.372876 11.00000 -1.20000 AFIX 0 C28 1 0.523890 0.741564 0.446777 11.00000 0.01557 0.01611 = 0.02733 0.00146 -0.00601 -0.00425 AFIX 43 H28 2 0.549628 0.802849 0.464473 11.00000 -1.20000 AFIX 0 C29 1 0.481767 0.774381 0.475265 11.00000 0.01997 0.01139 = 0.01886 0.00053 -0.00446 -0.00200 AFIX 43 H29 2 0.478298 0.857827 0.512631 11.00000 -1.20000 AFIX 0 O1 3 0.381216 0.853530 0.533143 11.00000 0.02365 0.01182 = 0.01776 -0.00310 -0.00286 0.00163 P1 4 0.387806 0.718241 0.477338 11.00000 0.01451 0.00868 = 0.01489 -0.00042 -0.00205 0.00046 HKLF 4 REM MR262_a.res in Pbcn REM R1 = 0.0412 for 2980 Fo > 4sig(Fo) and 0.0590 for all 3702 data REM 280 parameters refined using 0 restraints END WGHT 0.0392 2.8220 REM Highest difference peak 0.313, deepest hole -0.415, 1-sigma level 0.053 Q1 1 0.3789 0.5882 0.4851 11.00000 0.05 0.31 Q2 1 0.4199 0.7075 0.4653 11.00000 0.05 0.29 Q3 1 0.3239 0.5731 0.3684 11.00000 0.05 0.27 Q4 1 0.3609 0.3476 0.5797 11.00000 0.05 0.22 Q5 1 0.3934 0.4371 0.4791 11.00000 0.05 0.22 Q6 1 0.3805 0.7240 0.3597 11.00000 0.05 0.21 Q7 1 0.3676 0.7494 0.4311 11.00000 0.05 0.20 Q8 1 0.3404 0.4785 0.5813 11.00000 0.05 0.19 Q9 1 0.4289 0.5211 0.3792 11.00000 0.05 0.19 Q10 1 0.3783 0.7480 0.4236 11.00000 0.05 0.19 Q11 1 0.4082 0.9665 0.4998 11.00000 0.05 0.19 Q12 1 0.3501 0.6642 0.3812 11.00000 0.05 0.18 Q13 1 0.4402 0.6552 0.4093 11.00000 0.05 0.18 Q14 1 0.3604 0.4710 0.4538 11.00000 0.05 0.18 Q15 1 0.3544 0.3914 0.6442 11.00000 0.05 0.17 Q16 1 0.3519 0.2268 0.6183 11.00000 0.05 0.17 Q17 1 0.3735 0.8522 0.4870 11.00000 0.05 0.17 Q18 1 0.3656 0.4752 0.5336 11.00000 0.05 0.17 Q19 1 0.3827 0.8579 0.5675 11.00000 0.05 0.16 Q20 1 0.3587 0.4425 0.6235 11.00000 0.05 0.16 ; _shelx_res_checksum 85976 _shelx_hkl_file ; 0 1 0 -0.20 0.50 0 1 0 -0.20 0.80 0 -1 0 -1.20 0.80 0 -1 0 0.30 0.50 0 -2 0 547.05 31.90 0 2 0 522.55 32.40 0 2 0 539.65 31.70 0 -2 0 494.05 32.40 0 3 0 1.40 1.30 0 -3 0 -0.70 2.30 0 -3 0 -0.20 1.70 0 3 0 -0.10 2.10 0 -4 0 1135.49 67.09 0 -4 0 1043.80 67.89 0 4 0 1132.79 67.89 0 5 0 -3.60 3.30 0 -5 0 4.80 4.90 0 -5 0 -1.30 3.60 0 6 0 69.29 9.20 0 -6 0 69.39 8.40 0 -7 0 -7.20 4.90 0 7 0 8.80 7.10 0 8 0 99.49 13.10 0 -1 1 0.30 0.70 0 -1 -1 0.20 0.90 0 -1 -1 0.00 1.00 0 1 -1 0.30 0.70 0 1 1 -0.30 0.80 0 1 1 0.80 1.20 0 -2 -1 1545.55 93.19 0 2 -1 1525.45 92.79 0 2 1 1566.44 93.19 0 2 1 1582.44 92.69 0 -2 1 1462.95 92.79 0 -2 -1 1581.24 92.79 0 -2 1 1585.04 92.29 0 3 1 -0.10 2.20 0 -3 1 -1.30 2.50 0 3 -1 1.30 2.20 0 -3 1 0.60 1.50 0 -3 -1 1.00 2.10 0 -3 -1 4.10 2.50 0 3 1 -1.50 1.60 0 -4 1 48.90 6.00 0 4 1 37.40 5.40 0 -4 1 43.30 4.90 0 -4 -1 39.00 6.10 0 4 -1 40.90 5.00 0 -4 -1 39.40 5.40 0 4 1 40.20 4.30 0 5 -1 5.00 3.20 0 -5 1 -1.20 4.40 0 -5 -1 1.90 3.60 0 -5 1 4.20 3.50 0 -5 -1 -1.70 5.40 0 5 1 0.70 4.40 0 -6 1 14.30 4.60 0 -6 -1 17.60 5.40 0 6 -1 18.00 5.60 0 6 1 19.50 5.90 0 7 -1 0.80 5.90 0 -7 1 -5.90 4.60 0 7 1 20.90 9.90 0 -7 -1 9.00 5.60 0 8 -1 3.40 7.80 0 8 1 16.90 9.20 0 -1 -2 -1.30 1.20 0 1 2 0.80 1.30 0 1 -2 -0.10 0.70 0 -1 2 -0.60 0.60 0 -1 2 -1.20 0.50 0 1 2 0.00 1.40 0 -1 -2 -2.10 1.20 0 1 -2 -0.40 0.50 0 -2 -2 1839.82 110.09 0 2 -2 1777.72 109.29 0 -2 2 1823.52 108.89 0 2 2 1833.62 109.59 0 2 2 1917.21 110.19 0 -2 2 1775.22 109.39 0 -2 -2 1856.91 109.79 0 -3 2 -1.90 2.00 0 3 2 0.00 2.30 0 -3 -2 2.20 2.70 0 -3 2 -0.50 1.30 0 -3 -2 -2.20 2.70 0 3 2 0.70 2.00 0 -4 2 328.57 22.10 0 4 -2 329.77 21.60 0 4 2 321.87 21.10 0 -4 2 338.87 20.80 0 4 2 334.47 22.50 0 -4 -2 349.96 22.00 0 -4 -2 303.57 22.40 0 5 -2 -1.80 3.10 0 -5 -2 6.00 4.00 0 -5 2 -4.70 2.60 0 5 2 -2.00 3.90 0 -5 2 3.00 5.00 0 5 2 -0.40 3.00 0 6 -2 356.56 24.00 0 -6 -2 357.96 23.90 0 6 2 343.67 25.20 0 -6 2 321.17 23.40 0 7 2 4.10 7.50 0 -7 -2 -2.10 5.90 0 -7 2 1.10 8.50 0 7 -2 -1.20 5.60 0 8 2 108.49 15.80 0 8 -2 132.29 14.50 0 0 3 -1.10 1.20 0 0 -3 -0.90 1.40 0 -1 3 0.70 1.10 0 -1 -3 0.00 1.80 0 1 3 0.10 1.30 0 1 3 -0.60 1.50 0 -1 3 -0.20 0.50 0 -1 -3 0.30 1.70 0 1 -3 0.10 1.00 0 2 -3 642.24 39.20 0 -2 3 617.74 39.30 0 -2 -3 648.74 40.30 0 -2 3 677.53 39.10 0 2 3 665.43 40.10 0 2 3 627.24 41.10 0 -2 -3 673.93 40.30 0 -3 3 -0.40 2.20 0 -3 -3 -1.70 3.00 0 3 3 2.30 3.00 0 -3 3 2.00 1.30 0 -3 -3 0.40 3.60 0 3 3 -2.30 2.30 0 3 -3 1.30 1.70 0 -4 3 389.56 23.40 0 4 3 385.76 24.50 0 4 3 380.36 25.70 0 4 -3 391.36 24.30 0 -4 3 359.46 24.60 0 -4 3 397.66 23.60 0 -4 -3 339.87 25.50 0 -4 -3 389.26 25.20 0 5 3 4.70 4.70 0 5 3 -1.10 3.10 0 -5 3 3.50 2.80 0 5 -3 -0.70 3.30 0 -5 -3 5.10 4.20 0 -5 3 -3.90 4.70 0 -5 3 0.90 1.90 0 -6 3 60.29 7.00 0 6 -3 53.99 7.70 0 -6 3 60.89 5.70 0 6 3 51.09 7.50 0 6 3 54.69 9.50 0 -6 -3 57.79 7.90 0 7 3 -5.40 8.10 0 -7 -3 4.10 6.20 0 -7 3 -2.00 4.00 0 7 -3 7.80 6.10 0 8 3 4.20 9.30 0 8 -3 0.20 7.80 0 0 4 1745.93 100.49 0 0 -4 1635.84 100.79 0 0 4 1660.13 100.79 0 -1 4 -2.40 1.40 0 1 4 -1.70 1.90 0 -1 -4 -3.00 1.80 0 1 -4 0.70 0.60 0 1 -4 -1.50 1.30 0 2 4 1144.09 70.19 0 -2 -4 1054.49 70.79 0 2 -4 1163.18 68.69 0 -2 4 1172.98 69.09 0 -2 -4 1171.78 70.19 0 2 -4 1213.68 68.89 0 2 4 1185.28 69.99 0 -2 4 1100.39 68.89 0 3 -4 -0.50 1.60 0 3 4 3.30 3.30 0 3 4 3.80 3.20 0 -3 -4 1.60 3.50 0 -3 -4 6.10 3.00 0 -3 4 0.90 1.50 0 -3 4 2.70 2.10 0 4 -4 62.99 5.80 0 4 4 57.79 7.70 0 4 4 59.39 6.50 0 -4 -4 51.29 7.30 0 -4 -4 64.99 8.00 0 -4 4 69.49 5.10 0 -4 4 66.69 5.00 0 -4 4 64.69 6.70 0 5 4 -3.40 3.90 0 5 -4 -1.50 2.70 0 5 4 -4.10 5.00 0 -5 -4 0.90 4.70 0 -5 4 6.40 4.50 0 -5 4 1.70 2.10 0 -5 4 -1.00 2.30 0 -6 -4 7.20 5.30 0 -6 4 -3.70 7.20 0 6 -4 5.10 3.90 0 -6 4 2.00 2.80 0 6 4 4.80 4.80 0 6 4 4.10 7.10 0 -6 4 -4.80 3.10 0 7 -4 -1.30 5.50 0 -7 -4 9.60 7.00 0 7 4 15.50 8.80 0 8 -4 4.50 7.50 0 8 4 -9.30 10.10 0 0 5 1.00 2.30 0 0 5 3.90 1.60 0 0 -5 4.20 2.20 0 1 5 0.00 2.10 0 -1 -5 -1.70 2.00 0 -1 5 1.50 1.90 0 -1 -5 0.20 2.30 0 -1 5 1.10 0.60 0 1 -5 0.10 1.70 0 1 5 -3.20 2.00 0 2 -5 29.80 2.30 0 2 5 28.30 4.50 0 2 -5 30.20 3.10 0 -2 -5 30.30 4.50 0 2 5 24.00 4.20 0 -2 5 25.70 2.60 0 -2 5 27.60 3.50 0 -2 -5 28.50 4.50 0 -3 -5 -0.60 3.40 0 3 5 11.90 3.80 0 3 -5 3.10 1.50 0 -3 -5 8.30 3.80 0 3 5 6.00 3.60 0 -3 5 2.70 1.90 0 -3 5 0.30 2.10 0 -4 5 16.30 3.60 0 4 5 15.80 4.90 0 -4 -5 15.20 5.00 0 -4 5 21.00 2.80 0 4 5 14.00 3.90 0 4 -5 9.80 2.40 0 -4 -5 15.20 5.50 0 5 5 2.90 4.40 0 -5 5 -8.70 4.10 0 -5 -5 -2.80 4.10 0 -5 5 1.50 2.30 0 5 5 -0.80 5.20 0 -5 5 4.50 2.20 0 5 -5 3.10 2.70 0 -6 5 108.59 8.40 0 6 5 101.39 13.60 0 6 -5 110.09 9.50 0 -6 5 101.09 7.90 0 -6 5 82.19 10.60 0 6 5 111.09 10.70 0 -6 -5 95.09 11.70 0 7 5 4.70 9.00 0 -7 -5 -7.10 6.50 0 7 -5 -4.90 5.00 0 8 5 23.00 12.20 0 8 -5 56.19 9.10 0 -8 -5 75.89 13.30 0 0 6 691.03 41.50 0 0 -6 677.73 42.30 0 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146.89 14.30 -20 -5 -7 152.78 18.40 20 -5 -7 109.09 12.80 20 5 7 105.49 15.80 -20 5 -7 151.38 12.20 -20 6 7 -3.60 7.40 -20 -6 -7 -13.50 11.20 20 -6 -7 -8.00 6.20 20 6 7 -7.30 10.50 -20 6 -7 -5.70 5.80 -20 0 8 62.79 5.30 20 0 -8 52.49 6.80 -20 0 -8 60.59 8.90 -20 -1 -8 13.40 6.40 20 1 -8 19.20 4.10 -20 1 8 16.20 3.40 -20 -1 8 14.70 2.60 -20 1 -8 9.80 3.90 20 -1 -8 11.20 5.10 -20 1 -8 9.10 5.70 20 2 -8 10.60 3.30 -20 2 8 16.90 4.60 -20 -2 -8 21.20 7.70 -20 2 -8 7.90 6.10 -20 2 -8 8.10 4.50 20 -2 -8 10.40 5.40 -20 3 8 95.79 10.50 -20 -3 -8 99.59 14.00 20 3 -8 70.29 7.60 20 3 -8 91.79 7.40 -20 3 -8 83.19 8.60 -20 3 -8 90.89 10.90 20 -3 -8 85.09 10.40 -20 4 8 0.90 5.70 -20 -4 -8 -3.10 8.10 20 -4 -8 -2.60 4.80 -20 4 -8 -2.70 5.80 20 4 8 -2.80 9.50 -20 4 -8 3.20 4.40 -20 5 8 102.19 12.90 -20 -5 -8 95.89 15.30 -20 5 -8 106.69 10.40 20 -5 -8 96.59 12.00 20 5 8 88.49 14.10 -20 -6 -8 4.30 13.50 -20 6 8 -7.40 8.10 20 -6 -8 -9.00 7.20 -20 6 -8 -4.10 5.20 20 6 8 -9.30 11.20 20 0 -9 -4.10 4.10 -20 0 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-35 1 -1 -14.20 9.80 -35 0 2 232.98 19.10 -35 0 -2 265.67 24.30 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 34133 #=================================================================== _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 ; _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==================================================