data_MR249_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 'C14.50 H16.50 P0.50 Se0.50 Si' _chemical_formula_weight 273.83 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' 'Si' 'Si' 0.0817 0.0704 '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' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 11.2328(2) _cell_length_b 11.5305(2) _cell_length_c 12.5506(2) _cell_angle_alpha 97.0293(5) _cell_angle_beta 99.6595(5) _cell_angle_gamma 116.5661(5) _cell_volume 1396.92(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9398 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 25.71 _exptl_crystal_description 'platelet' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.302 _exptl_crystal_F_000 568 _exptl_transmission_factor_min 0.6071 _exptl_transmission_factor_max 0.7037 _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 1.502 _shelx_estimated_absorpt_T_min 0.714 _shelx_estimated_absorpt_T_max 0.889 _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 24191 _diffrn_reflns_av_unetI/netI 0.0202 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.329 _diffrn_reflns_theta_max 25.708 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 5299 _reflns_number_gt 4975 _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^)+(0.0234P)^2^+0.9373P] 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 5299 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0241 _refine_ls_R_factor_gt 0.0217 _refine_ls_wR_factor_ref 0.0552 _refine_ls_wR_factor_gt 0.0540 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.062 _refine_ls_shift/su_max 0.002 _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 0.75138(15) 0.78848(15) 0.30796(12) 0.0094(3) Uani 1 1 d . . . . . C2 C 0.68521(15) 0.68164(15) 0.34937(12) 0.0088(3) Uani 1 1 d . . . . . C3 C 0.54675(15) 0.65273(15) 0.37682(12) 0.0087(3) Uani 1 1 d . . . . . H3 H 0.5092 0.5694 0.4053 0.010 Uiso 1 1 calc R U . . . C4 C 0.44459(15) 0.63960(15) 0.27102(12) 0.0089(3) Uani 1 1 d . . . . . C5 C 0.48109(15) 0.74019(15) 0.21764(12) 0.0095(3) Uani 1 1 d . . . . . C6 C 0.31298(15) 0.51294(15) 0.23785(12) 0.0114(3) Uani 1 1 d . . . . . C7 C 0.31352(17) 0.39133(16) 0.21669(13) 0.0155(3) Uani 1 1 d . . . . . H7 H 0.3985 0.3901 0.2246 0.019 Uiso 1 1 calc R U . . . C8 C 0.19137(19) 0.27262(17) 0.18431(14) 0.0230(4) Uani 1 1 d . . . . . H8 H 0.1927 0.1906 0.1681 0.028 Uiso 1 1 calc R U . . . C9 C 0.06704(19) 0.27360(19) 0.17555(15) 0.0266(4) Uani 1 1 d . . . . . H9 H -0.0168 0.1922 0.1533 0.032 Uiso 1 1 calc R U . . . C10 C 0.06513(17) 0.3926(2) 0.19914(14) 0.0243(4) Uani 1 1 d . . . . . H10 H -0.0201 0.3928 0.1945 0.029 Uiso 1 1 calc R U . . . C11 C 0.18727(17) 0.51275(17) 0.22975(13) 0.0163(3) Uani 1 1 d . . . . . H11 H 0.1851 0.5944 0.2451 0.020 Uiso 1 1 calc R U . . . C12 C 0.73013(15) 0.58132(15) 0.37122(12) 0.0092(3) Uani 1 1 d . . . . . C13 C 0.70076(15) 0.47712(15) 0.28456(12) 0.0106(3) Uani 1 1 d . . . . . H13 H 0.6545 0.4720 0.2120 0.013 Uiso 1 1 calc R U . . . C14 C 0.73871(16) 0.38054(15) 0.30351(13) 0.0131(3) Uani 1 1 d . . . . . H14 H 0.7176 0.3094 0.2441 0.016 Uiso 1 1 calc R U . . . C15 C 0.80723(16) 0.38771(16) 0.40884(13) 0.0142(3) Uani 1 1 d . . . . . H15 H 0.8345 0.3226 0.4216 0.017 Uiso 1 1 calc R U . . . C16 C 0.83569(17) 0.49087(17) 0.49568(13) 0.0160(3) Uani 1 1 d . . . . . H16 H 0.8827 0.4960 0.5679 0.019 Uiso 1 1 calc R U . . . C17 C 0.79606(16) 0.58664(16) 0.47787(13) 0.0135(3) Uani 1 1 d . . . . . H17 H 0.8138 0.6555 0.5381 0.016 Uiso 1 1 calc R U . . . C18 C 0.62631(15) 0.89343(15) 0.43328(12) 0.0097(3) Uani 1 1 d . . . . . C19 C 0.57109(15) 0.77104(15) 0.46355(12) 0.0094(3) Uani 1 1 d . . . . . C20 C 0.54310(16) 0.76309(16) 0.56666(12) 0.0125(3) Uani 1 1 d . . . . . H20 H 0.5047 0.6799 0.5874 0.015 Uiso 1 1 calc R U . . . C21 C 0.57243(16) 0.87961(17) 0.63952(13) 0.0150(3) Uani 1 1 d . . . . . H21 H 0.5531 0.8754 0.7102 0.018 Uiso 1 1 calc R U . . . C22 C 0.62937(16) 1.00132(16) 0.60982(13) 0.0145(3) Uani 1 1 d . . . . . H22 H 0.6500 1.0798 0.6607 0.017 Uiso 1 1 calc R U . . . C23 C 0.65670(15) 1.00946(16) 0.50555(13) 0.0115(3) Uani 1 1 d . . . . . H23 H 0.6952 1.0926 0.4847 0.014 Uiso 1 1 calc R U . . . C24 C 1.00259(18) 0.74149(17) 0.29210(17) 0.0225(4) Uani 1 1 d . . . . . H24A H 0.9433 0.6541 0.2418 0.034 Uiso 1 1 calc R U . . . H24B H 1.0121 0.7314 0.3690 0.034 Uiso 1 1 calc R U . . . H24C H 1.0934 0.7808 0.2764 0.034 Uiso 1 1 calc R U . . . C25 C 1.04365(16) 1.02129(16) 0.36095(14) 0.0158(3) Uani 1 1 d . . . . . H25A H 1.1276 1.0613 0.3349 0.024 Uiso 1 1 calc R U . . . H25B H 1.0671 1.0138 0.4377 0.024 Uiso 1 1 calc R U . . . H25C H 0.9991 1.0774 0.3574 0.024 Uiso 1 1 calc R U . . . C26 C 0.89929(19) 0.85968(19) 0.12178(14) 0.0225(4) Uani 1 1 d . . . . . H26A H 0.8351 0.7705 0.0760 0.034 Uiso 1 1 calc R U . . . H26B H 0.9879 0.8919 0.1024 0.034 Uiso 1 1 calc R U . . . H26C H 0.8619 0.9203 0.1085 0.034 Uiso 1 1 calc R U . . . C27 C 0.52701(17) 0.77436(18) -0.00957(13) 0.0192(4) Uani 1 1 d . . . . . H27A H 0.5533 0.7038 -0.0131 0.029 Uiso 1 1 calc R U . . . H27B H 0.6084 0.8604 0.0255 0.029 Uiso 1 1 calc R U . . . H27C H 0.4877 0.7763 -0.0848 0.029 Uiso 1 1 calc R U . . . C28 C 0.3396(2) 0.87029(19) 0.07991(15) 0.0244(4) Uani 1 1 d . . . . . H28A H 0.3040 0.8744 0.0045 0.037 Uiso 1 1 calc R U . . . H28B H 0.4178 0.9570 0.1188 0.037 Uiso 1 1 calc R U . . . H28C H 0.2671 0.8473 0.1198 0.037 Uiso 1 1 calc R U . . . C29 C 0.24507(17) 0.57695(18) -0.00020(13) 0.0202(4) Uani 1 1 d . . . . . H29A H 0.2190 0.5768 -0.0788 0.030 Uiso 1 1 calc R U . . . H29B H 0.1677 0.5622 0.0328 0.030 Uiso 1 1 calc R U . . . H29C H 0.2692 0.5059 0.0067 0.030 Uiso 1 1 calc R U . . . Si1 Si 0.92410(4) 0.85269(4) 0.27127(4) 0.01129(9) Uani 1 1 d . . . . . Si2 Si 0.39653(4) 0.74119(4) 0.07366(3) 0.01143(9) Uani 1 1 d . . . . . P1 P 0.65087(4) 0.87780(4) 0.29412(3) 0.00804(8) Uani 1 1 d . . . . . Se1 Se 0.72749(2) 1.05692(2) 0.24012(2) 0.01320(5) 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 0.0093(7) 0.0083(7) 0.0103(7) 0.0003(6) 0.0024(6) 0.0045(6) C2 0.0088(7) 0.0087(7) 0.0073(7) -0.0013(6) 0.0002(5) 0.0043(6) C3 0.0080(7) 0.0083(7) 0.0094(7) 0.0031(6) 0.0023(6) 0.0034(6) C4 0.0084(7) 0.0099(7) 0.0083(7) 0.0001(6) 0.0020(6) 0.0047(6) C5 0.0097(7) 0.0088(7) 0.0096(7) 0.0006(6) 0.0022(6) 0.0046(6) C6 0.0112(8) 0.0132(8) 0.0068(7) 0.0032(6) 0.0030(6) 0.0029(6) C7 0.0156(8) 0.0127(8) 0.0147(8) 0.0034(6) 0.0028(6) 0.0040(7) C8 0.0258(10) 0.0114(8) 0.0200(9) 0.0030(7) 0.0039(7) -0.0003(7) C9 0.0177(9) 0.0230(10) 0.0172(9) 0.0032(7) 0.0032(7) -0.0080(8) C10 0.0088(8) 0.0373(11) 0.0187(9) 0.0059(8) 0.0046(7) 0.0038(8) C11 0.0138(8) 0.0220(9) 0.0125(8) 0.0044(7) 0.0044(6) 0.0075(7) C12 0.0071(7) 0.0090(7) 0.0128(7) 0.0039(6) 0.0043(6) 0.0039(6) C13 0.0101(7) 0.0111(7) 0.0105(7) 0.0026(6) 0.0017(6) 0.0051(6) C14 0.0138(8) 0.0091(7) 0.0166(8) 0.0023(6) 0.0053(6) 0.0054(6) C15 0.0131(8) 0.0138(8) 0.0207(8) 0.0082(6) 0.0064(6) 0.0090(7) C16 0.0166(8) 0.0220(9) 0.0122(8) 0.0073(7) 0.0026(6) 0.0112(7) C17 0.0134(8) 0.0139(8) 0.0122(7) 0.0002(6) 0.0020(6) 0.0066(7) C18 0.0078(7) 0.0129(8) 0.0102(7) 0.0022(6) 0.0018(6) 0.0066(6) C19 0.0065(7) 0.0124(7) 0.0098(7) 0.0015(6) 0.0007(6) 0.0055(6) C20 0.0101(7) 0.0165(8) 0.0117(7) 0.0052(6) 0.0029(6) 0.0065(6) C21 0.0119(8) 0.0236(9) 0.0094(7) 0.0010(6) 0.0032(6) 0.0088(7) C22 0.0109(8) 0.0181(8) 0.0130(8) -0.0038(6) -0.0001(6) 0.0084(7) C23 0.0077(7) 0.0122(8) 0.0141(7) 0.0003(6) 0.0004(6) 0.0059(6) C24 0.0147(8) 0.0153(9) 0.0416(11) 0.0067(8) 0.0137(8) 0.0082(7) C25 0.0118(8) 0.0120(8) 0.0198(8) 0.0023(6) 0.0029(6) 0.0033(6) C26 0.0215(9) 0.0267(10) 0.0169(8) 0.0025(7) 0.0096(7) 0.0086(8) C27 0.0182(9) 0.0212(9) 0.0111(8) 0.0012(7) 0.0035(6) 0.0041(7) C28 0.0369(11) 0.0284(10) 0.0164(8) 0.0056(7) 0.0021(8) 0.0241(9) C29 0.0174(9) 0.0222(9) 0.0110(8) 0.0030(7) -0.0006(6) 0.0025(7) Si1 0.0091(2) 0.0093(2) 0.0147(2) 0.00147(16) 0.00542(16) 0.00319(17) Si2 0.0140(2) 0.0122(2) 0.00817(19) 0.00271(16) 0.00182(16) 0.00660(18) P1 0.00954(19) 0.00603(18) 0.00901(18) 0.00188(14) 0.00302(14) 0.00383(15) Se1 0.01762(9) 0.00664(8) 0.01538(9) 0.00455(6) 0.00548(6) 0.00487(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.344(2) . ? C1 P1 1.8394(15) . ? C1 Si1 1.9034(15) . ? C2 C12 1.490(2) . ? C2 C3 1.547(2) . ? C3 C19 1.524(2) . ? C3 C4 1.545(2) . ? C3 H3 1.0000 . ? C4 C5 1.349(2) . ? C4 C6 1.485(2) . ? C5 P1 1.8391(15) . ? C5 Si2 1.8991(15) . ? C6 C7 1.398(2) . ? C6 C11 1.398(2) . ? C7 C8 1.385(2) . ? C7 H7 0.9500 . ? C8 C9 1.388(3) . ? C8 H8 0.9500 . ? C9 C10 1.379(3) . ? C9 H9 0.9500 . ? C10 C11 1.393(2) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.393(2) . ? C12 C17 1.397(2) . ? C13 C14 1.391(2) . ? C13 H13 0.9500 . ? C14 C15 1.386(2) . ? C14 H14 0.9500 . ? C15 C16 1.389(2) . ? C15 H15 0.9500 . ? C16 C17 1.391(2) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.386(2) . ? C18 C19 1.396(2) . ? C18 P1 1.8133(15) . ? C19 C20 1.386(2) . ? C20 C21 1.397(2) . ? C20 H20 0.9500 . ? C21 C22 1.387(2) . ? C21 H21 0.9500 . ? C22 C23 1.398(2) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 Si1 1.8723(18) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 Si1 1.8633(16) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 Si1 1.8669(18) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Si2 1.8697(17) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 Si2 1.8630(18) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 Si2 1.8706(17) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? P1 Se1 2.1009(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 P1 109.23(11) . . ? C2 C1 Si1 129.32(12) . . ? P1 C1 Si1 121.41(8) . . ? C1 C2 C12 126.48(14) . . ? C1 C2 C3 119.68(13) . . ? C12 C2 C3 113.83(12) . . ? C19 C3 C4 108.17(12) . . ? C19 C3 C2 108.28(12) . . ? C4 C3 C2 108.88(12) . . ? C19 C3 H3 110.5 . . ? C4 C3 H3 110.5 . . ? C2 C3 H3 110.5 . . ? C5 C4 C6 126.26(14) . . ? C5 C4 C3 118.83(13) . . ? C6 C4 C3 114.90(12) . . ? C4 C5 P1 109.83(11) . . ? C4 C5 Si2 128.66(12) . . ? P1 C5 Si2 120.69(8) . . ? C7 C6 C11 118.91(15) . . ? C7 C6 C4 120.13(14) . . ? C11 C6 C4 120.94(14) . . ? C8 C7 C6 120.66(16) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C7 C8 C9 119.93(17) . . ? C7 C8 H8 120.0 . . ? C9 C8 H8 120.0 . . ? C10 C9 C8 120.03(16) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.49(17) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 119.93(16) . . ? C10 C11 H11 120.0 . . ? C6 C11 H11 120.0 . . ? C13 C12 C17 119.32(14) . . ? C13 C12 C2 119.40(13) . . ? C17 C12 C2 121.23(13) . . ? C14 C13 C12 120.43(14) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C15 C14 C13 120.22(14) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.52(15) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C17 120.65(15) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 119.83(14) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C23 C18 C19 121.19(14) . . ? C23 C18 P1 126.79(12) . . ? C19 C18 P1 112.02(11) . . ? C20 C19 C18 120.25(14) . . ? C20 C19 C3 124.43(14) . . ? C18 C19 C3 115.32(13) . . ? C19 C20 C21 118.81(15) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C22 C21 C20 120.76(14) . . ? C22 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? C21 C22 C23 120.54(14) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 118.44(15) . . ? C18 C23 H23 120.8 . . ? C22 C23 H23 120.8 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? Si2 C28 H28A 109.5 . . ? Si2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? Si2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 C29 H29A 109.5 . . ? Si2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? Si2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 Si1 C26 110.62(8) . . ? C25 Si1 C24 108.76(8) . . ? C26 Si1 C24 107.28(9) . . ? C25 Si1 C1 108.75(7) . . ? C26 Si1 C1 109.21(7) . . ? C24 Si1 C1 112.24(7) . . ? C28 Si2 C27 111.22(9) . . ? C28 Si2 C29 108.45(9) . . ? C27 Si2 C29 106.38(8) . . ? C28 Si2 C5 110.97(7) . . ? C27 Si2 C5 106.67(7) . . ? C29 Si2 C5 113.08(7) . . ? C18 P1 C5 100.43(7) . . ? C18 P1 C1 98.93(7) . . ? C5 P1 C1 100.43(7) . . ? C18 P1 Se1 114.40(5) . . ? C5 P1 Se1 118.83(5) . . ? C1 P1 Se1 120.23(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 P1 C1 C2 C12 178.69(12) . . . . ? Si1 C1 C2 C12 -3.6(2) . . . . ? P1 C1 C2 C3 -0.07(17) . . . . ? Si1 C1 C2 C3 177.63(11) . . . . ? C1 C2 C3 C19 -60.08(17) . . . . ? C12 C2 C3 C19 121.00(13) . . . . ? C1 C2 C3 C4 57.31(17) . . . . ? C12 C2 C3 C4 -121.60(13) . . . . ? C19 C3 C4 C5 62.29(17) . . . . ? C2 C3 C4 C5 -55.17(17) . . . . ? C19 C3 C4 C6 -118.10(14) . . . . ? C2 C3 C4 C6 124.44(13) . . . . ? C6 C4 C5 P1 177.77(12) . . . . ? C3 C4 C5 P1 -2.67(17) . . . . ? C6 C4 C5 Si2 -12.7(2) . . . . ? C3 C4 C5 Si2 166.81(11) . . . . ? C5 C4 C6 C7 121.68(17) . . . . ? C3 C4 C6 C7 -57.90(18) . . . . ? C5 C4 C6 C11 -59.8(2) . . . . ? C3 C4 C6 C11 120.60(15) . . . . ? C11 C6 C7 C8 2.3(2) . . . . ? C4 C6 C7 C8 -179.16(15) . . . . ? C6 C7 C8 C9 -1.8(3) . . . . ? C7 C8 C9 C10 0.0(3) . . . . ? C8 C9 C10 C11 1.3(3) . . . . ? C9 C10 C11 C6 -0.7(3) . . . . ? C7 C6 C11 C10 -1.1(2) . . . . ? C4 C6 C11 C10 -179.60(14) . . . . ? C1 C2 C12 C13 -82.9(2) . . . . ? C3 C2 C12 C13 95.92(16) . . . . ? C1 C2 C12 C17 99.79(19) . . . . ? C3 C2 C12 C17 -81.39(17) . . . . ? C17 C12 C13 C14 -1.1(2) . . . . ? C2 C12 C13 C14 -178.44(14) . . . . ? C12 C13 C14 C15 -0.5(2) . . . . ? C13 C14 C15 C16 1.1(2) . . . . ? C14 C15 C16 C17 0.0(2) . . . . ? C15 C16 C17 C12 -1.7(2) . . . . ? C13 C12 C17 C16 2.2(2) . . . . ? C2 C12 C17 C16 179.47(14) . . . . ? C23 C18 C19 C20 1.2(2) . . . . ? P1 C18 C19 C20 -178.98(11) . . . . ? C23 C18 C19 C3 -178.35(13) . . . . ? P1 C18 C19 C3 1.48(16) . . . . ? C4 C3 C19 C20 120.27(15) . . . . ? C2 C3 C19 C20 -121.88(15) . . . . ? C4 C3 C19 C18 -60.21(16) . . . . ? C2 C3 C19 C18 57.64(16) . . . . ? C18 C19 C20 C21 -0.6(2) . . . . ? C3 C19 C20 C21 178.88(14) . . . . ? C19 C20 C21 C22 -0.4(2) . . . . ? C20 C21 C22 C23 0.9(2) . . . . ? C19 C18 C23 C22 -0.7(2) . . . . ? P1 C18 C23 C22 179.52(11) . . . . ? C21 C22 C23 C18 -0.4(2) . . . . ? C4 C5 Si2 C28 120.95(15) . . . . ? P1 C5 Si2 C28 -70.56(11) . . . . ? C4 C5 Si2 C27 -117.75(15) . . . . ? P1 C5 Si2 C27 50.73(11) . . . . ? C4 C5 Si2 C29 -1.16(17) . . . . ? P1 C5 Si2 C29 167.32(9) . . . . ? C23 C18 P1 C5 -130.61(14) . . . . ? C19 C18 P1 C5 49.57(12) . . . . ? C23 C18 P1 C1 126.96(14) . . . . ? C19 C18 P1 C1 -52.86(12) . . . . ? C23 C18 P1 Se1 -2.16(15) . . . . ? C19 C18 P1 Se1 178.02(9) . . . . ? C4 C5 P1 C18 -48.52(12) . . . . ? Si2 C5 P1 C18 141.02(9) . . . . ? C4 C5 P1 C1 52.69(12) . . . . ? Si2 C5 P1 C1 -117.77(9) . . . . ? C4 C5 P1 Se1 -174.02(9) . . . . ? Si2 C5 P1 Se1 15.52(11) . . . . ? C2 C1 P1 C18 51.45(12) . . . . ? Si1 C1 P1 C18 -126.47(9) . . . . ? C2 C1 P1 C5 -50.98(12) . . . . ? Si1 C1 P1 C5 131.10(9) . . . . ? C2 C1 P1 Se1 176.59(9) . . . . ? Si1 C1 P1 Se1 -1.34(11) . . . . ? _refine_diff_density_max 0.303 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.058 _shelx_res_file ; MR249_a.res created by SHELXL-2014/7 TITL unvoll_a.res in P-1 REM Old TITL unvoll in P-1 REM SHELXT solution in P-1 REM R1 0.082, Rweak 0.006, Alpha 0.058, Orientation as input REM Formula found by SHELXT: C29 Si2 P Se CELL 0.71073 11.2328 11.5305 12.5506 97.0293 99.6595 116.5661 ZERR 4.000 0.0002 0.0002 0.0002 0.0005 0.0005 0.0005 LATT 1 SFAC C H SI P SE UNIT 58 66 4 2 2 TEMP -173.150 SIZE 0.08 0.16 0.24 L.S. 30 BOND $H LIST 6 FMAP 2 PLAN 20 acta conf WGHT 0.023400 0.937300 FVAR 0.71432 C1 1 0.751378 0.788485 0.307962 11.00000 0.00928 0.00829 = 0.01033 0.00034 0.00235 0.00451 C2 1 0.685210 0.681642 0.349369 11.00000 0.00878 0.00875 = 0.00727 -0.00135 0.00015 0.00430 C3 1 0.546749 0.652728 0.376819 11.00000 0.00800 0.00835 = 0.00943 0.00314 0.00230 0.00340 AFIX 13 H3 2 0.509174 0.569422 0.405256 11.00000 -1.20000 AFIX 0 C4 1 0.444589 0.639600 0.271021 11.00000 0.00838 0.00989 = 0.00826 0.00009 0.00204 0.00473 C5 1 0.481091 0.740187 0.217642 11.00000 0.00970 0.00881 = 0.00965 0.00057 0.00219 0.00459 C6 1 0.312979 0.512939 0.237855 11.00000 0.01118 0.01319 = 0.00682 0.00325 0.00296 0.00292 C7 1 0.313517 0.391329 0.216694 11.00000 0.01561 0.01267 = 0.01474 0.00345 0.00284 0.00403 AFIX 43 H7 2 0.398521 0.390091 0.224605 11.00000 -1.20000 AFIX 0 C8 1 0.191365 0.272616 0.184310 11.00000 0.02584 0.01139 = 0.01999 0.00298 0.00390 -0.00028 AFIX 43 H8 2 0.192697 0.190599 0.168113 11.00000 -1.20000 AFIX 0 C9 1 0.067044 0.273600 0.175547 11.00000 0.01769 0.02299 = 0.01722 0.00317 0.00316 -0.00803 AFIX 43 H9 2 -0.016791 0.192221 0.153283 11.00000 -1.20000 AFIX 0 C10 1 0.065131 0.392641 0.199140 11.00000 0.00884 0.03732 = 0.01873 0.00593 0.00461 0.00384 AFIX 43 H10 2 -0.020102 0.392763 0.194487 11.00000 -1.20000 AFIX 0 C11 1 0.187267 0.512749 0.229753 11.00000 0.01381 0.02203 = 0.01246 0.00444 0.00436 0.00747 AFIX 43 H11 2 0.185099 0.594434 0.245104 11.00000 -1.20000 AFIX 0 C12 1 0.730129 0.581324 0.371222 11.00000 0.00710 0.00896 = 0.01281 0.00391 0.00429 0.00389 C13 1 0.700758 0.477123 0.284557 11.00000 0.01007 0.01107 = 0.01046 0.00259 0.00170 0.00508 AFIX 43 H13 2 0.654506 0.472012 0.212042 11.00000 -1.20000 AFIX 0 C14 1 0.738706 0.380536 0.303506 11.00000 0.01385 0.00911 = 0.01660 0.00227 0.00526 0.00541 AFIX 43 H14 2 0.717600 0.309398 0.244065 11.00000 -1.20000 AFIX 0 C15 1 0.807229 0.387715 0.408842 11.00000 0.01310 0.01382 = 0.02071 0.00816 0.00638 0.00897 AFIX 43 H15 2 0.834528 0.322578 0.421557 11.00000 -1.20000 AFIX 0 C16 1 0.835689 0.490866 0.495681 11.00000 0.01664 0.02196 = 0.01222 0.00727 0.00260 0.01122 AFIX 43 H16 2 0.882678 0.496029 0.567933 11.00000 -1.20000 AFIX 0 C17 1 0.796061 0.586638 0.477866 11.00000 0.01337 0.01389 = 0.01216 0.00022 0.00199 0.00656 AFIX 43 H17 2 0.813797 0.655498 0.538091 11.00000 -1.20000 AFIX 0 C18 1 0.626315 0.893428 0.433276 11.00000 0.00776 0.01285 = 0.01021 0.00216 0.00176 0.00657 C19 1 0.571092 0.771044 0.463548 11.00000 0.00654 0.01235 = 0.00979 0.00151 0.00073 0.00553 C20 1 0.543100 0.763092 0.566657 11.00000 0.01011 0.01653 = 0.01171 0.00523 0.00292 0.00650 AFIX 43 H20 2 0.504667 0.679914 0.587402 11.00000 -1.20000 AFIX 0 C21 1 0.572429 0.879612 0.639522 11.00000 0.01187 0.02364 = 0.00943 0.00102 0.00316 0.00883 AFIX 43 H21 2 0.553138 0.875404 0.710230 11.00000 -1.20000 AFIX 0 C22 1 0.629366 1.001315 0.609820 11.00000 0.01088 0.01810 = 0.01304 -0.00376 -0.00008 0.00843 AFIX 43 H22 2 0.649975 1.079809 0.660737 11.00000 -1.20000 AFIX 0 C23 1 0.656698 1.009465 0.505547 11.00000 0.00770 0.01223 = 0.01410 0.00026 0.00038 0.00586 AFIX 43 H23 2 0.695193 1.092600 0.484738 11.00000 -1.20000 AFIX 0 C24 1 1.002587 0.741494 0.292099 11.00000 0.01466 0.01529 = 0.04160 0.00673 0.01372 0.00821 AFIX 137 H24A 2 0.943335 0.654100 0.241795 11.00000 -1.50000 H24B 2 1.012108 0.731354 0.368984 11.00000 -1.50000 H24C 2 1.093403 0.780824 0.276423 11.00000 -1.50000 AFIX 0 C25 1 1.043650 1.021294 0.360955 11.00000 0.01180 0.01204 = 0.01977 0.00230 0.00286 0.00328 AFIX 137 H25A 2 1.127609 1.061346 0.334908 11.00000 -1.50000 H25B 2 1.067109 1.013787 0.437703 11.00000 -1.50000 H25C 2 0.999111 1.077428 0.357425 11.00000 -1.50000 AFIX 0 C26 1 0.899293 0.859679 0.121784 11.00000 0.02154 0.02671 = 0.01686 0.00249 0.00960 0.00860 AFIX 137 H26A 2 0.835083 0.770520 0.075996 11.00000 -1.50000 H26B 2 0.987873 0.891878 0.102363 11.00000 -1.50000 H26C 2 0.861902 0.920306 0.108527 11.00000 -1.50000 AFIX 0 C27 1 0.527009 0.774362 -0.009572 11.00000 0.01819 0.02118 = 0.01112 0.00117 0.00348 0.00410 AFIX 137 H27A 2 0.553288 0.703849 -0.013082 11.00000 -1.50000 H27B 2 0.608407 0.860368 0.025535 11.00000 -1.50000 H27C 2 0.487723 0.776260 -0.084794 11.00000 -1.50000 AFIX 0 C28 1 0.339599 0.870290 0.079912 11.00000 0.03689 0.02845 = 0.01639 0.00555 0.00211 0.02412 AFIX 137 H28A 2 0.303985 0.874445 0.004451 11.00000 -1.50000 H28B 2 0.417784 0.957002 0.118788 11.00000 -1.50000 H28C 2 0.267081 0.847336 0.119786 11.00000 -1.50000 AFIX 0 C29 1 0.245074 0.576947 -0.000200 11.00000 0.01741 0.02221 = 0.01101 0.00304 -0.00055 0.00251 AFIX 137 H29A 2 0.218972 0.576770 -0.078774 11.00000 -1.50000 H29B 2 0.167745 0.562168 0.032781 11.00000 -1.50000 H29C 2 0.269159 0.505860 0.006699 11.00000 -1.50000 AFIX 0 SI1 3 0.924096 0.852691 0.271266 11.00000 0.00910 0.00927 = 0.01470 0.00147 0.00542 0.00319 SI2 3 0.396529 0.741185 0.073662 11.00000 0.01403 0.01222 = 0.00817 0.00271 0.00182 0.00660 P1 4 0.650868 0.877804 0.294116 11.00000 0.00954 0.00603 = 0.00901 0.00188 0.00302 0.00383 SE1 5 0.727490 1.056917 0.240125 11.00000 0.01762 0.00664 = 0.01538 0.00455 0.00548 0.00487 HKLF 4 REM unvoll_a.res in P-1 REM R1 = 0.0217 for 4975 Fo > 4sig(Fo) and 0.0241 for all 5299 data REM 304 parameters refined using 0 restraints END WGHT 0.0224 0.9370 REM Highest difference peak 0.303, deepest hole -0.361, 1-sigma level 0.058 Q1 1 0.4420 0.7418 0.1585 11.00000 0.05 0.30 Q2 1 0.7141 0.6367 0.3616 11.00000 0.05 0.28 Q3 1 0.5586 0.7151 0.4222 11.00000 0.05 0.27 Q4 1 0.3786 0.5808 0.2566 11.00000 0.05 0.26 Q5 1 0.7233 0.8314 0.3035 11.00000 0.05 0.26 Q6 1 0.6374 0.8957 0.3728 11.00000 0.05 0.25 Q7 1 0.6286 0.6743 0.3652 11.00000 0.05 0.24 Q8 1 0.4887 0.6427 0.3196 11.00000 0.05 0.24 Q9 1 0.7411 0.7512 0.3587 11.00000 0.05 0.23 Q10 1 0.7530 0.5866 0.4210 11.00000 0.05 0.23 Q11 1 0.4393 0.7040 0.2554 11.00000 0.05 0.22 Q12 1 0.5763 0.8265 0.6047 11.00000 0.05 0.22 Q13 1 0.7269 0.4324 0.2991 11.00000 0.05 0.21 Q14 1 0.7351 0.5431 0.3286 11.00000 0.05 0.21 Q15 1 0.6121 0.8378 0.4549 11.00000 0.05 0.21 Q16 1 0.5437 0.7981 0.2469 11.00000 0.05 0.21 Q17 1 0.2604 0.5113 0.2509 11.00000 0.05 0.21 Q18 1 0.7627 0.3793 0.3586 11.00000 0.05 0.20 Q19 1 0.2931 0.2453 0.2802 11.00000 0.05 0.20 Q20 1 0.3231 0.6517 0.0343 11.00000 0.05 0.20 ; _shelx_res_checksum 16088 _shelx_hkl_file ; -2 0 0 1932.31 52.49 -2 0 0 2046.80 52.39 -2 0 0 1983.20 52.89 2 0 0 1975.40 52.39 2 0 0 1934.51 52.79 2 0 0 1921.31 52.49 -3 0 0 1934.41 52.39 -3 0 0 1971.00 51.89 -3 0 0 1913.51 51.59 3 0 0 1935.01 51.69 3 0 0 1864.91 51.89 3 0 0 1841.32 52.29 -4 0 0 556.54 18.00 -4 0 0 542.75 17.00 -4 0 0 538.25 17.20 4 0 0 544.45 17.40 4 0 0 529.85 17.80 4 0 0 570.64 17.10 -5 0 0 418.76 15.30 -5 0 0 387.36 13.90 -5 0 0 413.96 14.30 5 0 0 400.06 14.60 5 0 0 383.06 15.00 5 0 0 416.66 14.20 -6 0 0 474.85 16.70 -6 0 0 479.05 16.90 -6 0 0 459.65 17.80 6 0 0 477.75 18.20 6 0 0 473.15 17.50 6 0 0 487.15 16.80 -7 0 0 7.50 4.80 -7 0 0 4.60 3.40 -7 0 0 15.90 4.20 7 0 0 9.60 4.00 7 0 0 14.30 4.70 7 0 0 10.20 4.40 -8 0 0 70.79 8.10 -8 0 0 51.99 7.30 -8 0 0 44.50 6.00 8 0 0 47.80 6.10 8 0 0 41.10 6.90 -9 0 0 401.76 17.80 -9 0 0 414.56 18.00 9 0 0 410.46 19.60 -10 0 0 61.99 8.40 10 0 0 57.09 9.70 -11 0 0 683.13 27.80 -11 0 0 763.42 28.50 -11 0 0 687.93 30.90 11 0 0 737.93 28.80 11 0 0 703.03 30.70 11 0 0 698.73 26.40 12 -1 0 21.40 10.20 -12 1 0 15.70 8.60 -12 1 0 1.40 7.80 11 -1 0 8.10 8.30 11 -1 0 7.50 6.90 -11 1 0 19.20 7.20 -11 1 0 25.00 7.50 -11 1 0 -1.50 7.30 10 -1 0 169.98 15.40 10 -1 0 194.88 15.10 -10 1 0 160.08 14.40 9 -1 0 327.47 17.70 9 -1 0 324.87 16.90 -9 1 0 335.57 15.30 -9 1 0 347.47 15.60 8 -1 0 41.10 7.20 8 -1 0 33.30 5.90 8 -1 0 60.59 6.80 -8 1 0 49.20 6.30 -8 1 0 45.40 6.80 -8 1 0 47.70 5.90 7 -1 0 312.77 13.80 7 -1 0 312.07 14.40 7 -1 0 305.47 12.70 -7 1 0 319.37 12.90 -7 1 0 313.47 12.90 -7 1 0 291.67 14.00 6 -1 0 304.87 12.50 6 -1 0 281.37 12.80 6 -1 0 304.97 11.90 -6 1 0 311.87 13.20 -6 1 0 314.87 12.00 -6 1 0 308.97 12.00 5 -1 0 164.18 8.50 5 -1 0 162.48 7.50 5 -1 0 148.09 7.60 -5 1 0 163.68 7.50 -5 1 0 168.48 7.60 -5 1 0 170.48 8.60 4 -1 0 10.80 2.30 4 -1 0 16.60 2.60 4 -1 0 12.10 2.20 -4 1 0 9.10 2.00 -4 1 0 15.30 2.40 -4 1 0 13.50 2.80 3 -1 0 8371.06 219.78 2 -1 0 871.01 23.20 2 -1 0 857.31 23.30 2 -1 0 811.72 23.60 -2 1 0 854.01 23.20 -2 1 0 845.42 23.60 -2 1 0 851.81 23.20 -1 -1 0 1121.99 30.20 -1 -1 0 1184.88 31.00 -1 -1 0 1137.59 30.70 1 1 0 1046.10 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1285.27 35.10 3 -3 -4 1232.78 35.00 -3 3 4 1301.87 35.40 -3 3 4 1202.78 35.20 2 -3 -4 16.80 2.50 2 -3 -4 18.30 2.50 -2 3 4 17.60 2.90 -2 3 4 13.90 2.50 1 -3 -4 1177.38 34.50 1 -3 -4 1262.47 35.20 -1 3 4 1256.67 35.30 -1 3 4 1272.87 35.10 0 -3 -4 431.16 14.40 0 -3 -4 442.46 13.30 0 -3 -4 437.96 13.70 0 3 4 406.46 14.00 0 3 4 401.26 14.40 -1 -3 -4 169.78 7.30 -1 -3 -4 162.58 8.10 -1 -3 -4 161.58 7.30 1 3 4 156.18 8.30 1 3 4 165.48 8.10 -2 -3 -4 972.70 28.80 -2 -3 -4 1025.00 29.50 -2 -3 -4 969.10 29.80 2 3 4 986.10 30.30 2 3 4 967.10 29.70 -3 -3 -4 181.28 9.70 -3 -3 -4 186.88 8.80 -3 -3 -4 172.78 9.40 3 3 4 178.18 5.80 3 3 4 175.28 10.10 3 3 4 177.58 9.70 -4 -3 -4 198.98 10.70 -4 -3 -4 189.08 9.70 -4 -3 -4 195.48 10.90 4 3 4 190.28 6.80 4 3 4 141.69 14.70 4 3 4 189.18 11.20 -5 -3 -4 4.50 4.60 -5 -3 -4 -1.80 4.90 -5 -3 -4 -1.30 3.80 5 3 4 -1.50 4.10 5 3 4 0.30 4.60 5 3 4 2.10 2.10 -6 -3 -4 412.86 17.70 -6 -3 -4 394.36 18.60 -6 -3 -4 401.56 16.70 6 3 4 350.66 18.70 6 3 4 433.16 18.40 6 3 4 387.76 13.30 -7 -3 -4 22.90 6.30 -7 -3 -4 24.00 6.40 7 3 4 28.00 4.00 7 3 4 -2.60 7.60 7 3 4 17.60 6.70 -8 -3 -4 831.82 32.70 -8 -3 -4 827.12 30.00 -8 -3 -4 806.62 30.40 8 3 4 841.22 32.00 8 3 4 842.42 33.70 8 3 4 855.81 26.00 13 -4 -4 -10.60 7.00 13 -4 -4 17.50 9.70 13 -4 -4 2.90 9.60 -13 4 4 7.30 8.30 -13 4 4 5.60 9.40 -13 4 4 0.00 8.40 12 -4 -4 213.08 17.00 12 -4 -4 235.08 17.00 12 -4 -4 197.58 14.00 -12 4 4 226.58 17.40 -12 4 4 213.28 15.30 -12 4 4 205.48 15.20 11 -4 -4 9.80 9.10 11 -4 -4 8.10 6.40 -11 4 4 10.20 6.10 -11 4 4 9.70 6.30 10 -4 -4 887.91 31.30 10 -4 -4 916.71 31.40 10 -4 -4 939.51 29.90 -10 4 4 896.41 30.50 -10 4 4 903.81 31.60 9 -4 -4 7.70 4.50 9 -4 -4 -0.40 3.60 9 -4 -4 3.70 4.80 -9 4 4 5.90 4.20 -9 4 4 1.20 4.80 -9 4 4 4.10 4.00 8 -4 -4 65.69 7.80 8 -4 -4 62.19 6.80 8 -4 -4 70.49 7.50 -8 4 4 71.19 7.30 -8 4 4 76.49 7.60 -8 4 4 59.79 7.70 7 -4 -4 330.27 13.20 7 -4 -4 337.37 12.90 7 -4 -4 327.07 13.40 -7 4 4 317.77 13.40 -7 4 4 335.77 13.40 -7 4 4 326.57 13.20 6 -4 -4 2013.00 56.39 6 -4 -4 2053.09 55.99 6 -4 -4 1904.71 55.79 -6 4 4 2026.10 56.19 -6 4 4 2054.89 56.39 -6 4 4 2024.60 56.39 5 -4 -4 1587.54 43.70 5 -4 -4 1578.24 43.30 5 -4 -4 1533.05 42.90 -5 4 4 1470.55 42.90 -5 4 4 1542.65 43.60 -5 4 4 1518.85 43.70 4 -4 -4 386.86 12.40 4 -4 -4 362.76 13.20 4 -4 -4 398.56 13.30 -4 4 4 389.16 13.40 -4 4 4 409.26 13.80 3 -4 -4 228.48 9.20 3 -4 -4 231.48 7.80 3 -4 -4 230.38 9.00 -3 4 4 220.48 9.30 -3 4 4 223.68 9.20 2 -4 -4 623.14 19.30 2 -4 -4 626.24 19.80 -2 4 4 634.54 19.80 -2 4 4 639.44 19.80 1 -4 -4 2087.79 57.79 1 -4 -4 2067.69 57.09 -1 4 4 2107.09 57.89 -1 4 4 2070.99 57.49 0 -4 -4 339.67 13.30 0 -4 -4 347.87 12.40 0 4 4 366.86 13.20 0 4 4 347.87 13.30 -1 -4 -4 90.59 7.10 -1 -4 -4 86.89 6.00 -1 -4 -4 86.99 6.00 1 4 4 87.59 7.10 1 4 4 81.09 6.70 -2 -4 -4 156.18 9.50 -2 -4 -4 155.38 8.30 -2 -4 -4 160.28 8.80 2 4 4 167.18 10.00 2 4 4 162.98 9.30 -3 -4 -4 989.40 30.40 -3 -4 -4 950.70 30.50 -3 -4 -4 918.51 29.30 3 4 4 959.40 31.20 -4 -4 -4 247.88 12.00 -4 -4 -4 242.08 13.00 4 4 4 240.88 8.10 4 4 4 257.07 12.90 4 4 4 257.97 14.10 -5 -4 -4 371.46 16.10 -5 -4 -4 368.96 17.50 -5 -4 -4 373.76 17.20 5 4 4 359.16 17.10 5 4 4 381.06 18.60 5 4 4 389.86 12.10 -6 -4 -4 123.09 12.10 -6 -4 -4 103.59 10.70 -6 -4 -4 128.99 12.60 6 4 4 107.19 12.10 6 4 4 129.59 6.50 6 4 4 131.49 14.00 -7 -4 -4 686.83 28.90 -7 -4 -4 695.63 26.80 7 4 4 735.53 28.70 7 4 4 746.13 30.40 7 4 4 723.93 22.00 -8 -4 -4 12.50 7.90 -8 -4 -4 11.70 9.40 -8 -4 -4 2.00 8.00 8 4 4 13.70 3.80 8 4 4 22.80 10.40 13 -5 -4 43.10 8.40 13 -5 -4 38.40 10.00 13 -5 -4 40.10 10.50 -13 5 4 51.39 9.60 -13 5 4 35.40 9.10 -13 5 4 56.89 10.90 12 -5 -4 27.80 8.40 12 -5 -4 30.60 8.80 12 -5 -4 37.40 7.60 -12 5 4 35.50 8.20 -12 5 4 31.90 8.10 -12 5 4 41.50 9.30 11 -5 -4 0.70 7.40 11 -5 -4 -0.10 5.80 -11 5 4 4.80 5.90 -11 5 4 2.90 5.80 10 -5 -4 2056.89 56.99 10 -5 -4 2030.70 58.39 10 -5 -4 1903.31 57.89 -10 5 4 1909.61 57.29 -10 5 4 1838.02 57.99 9 -5 -4 102.89 9.70 9 -5 -4 109.79 9.50 9 -5 -4 106.09 8.70 -9 5 4 112.49 9.70 -9 5 4 112.19 9.30 -9 5 4 114.59 9.40 8 -5 -4 228.38 11.10 8 -5 -4 228.08 11.80 8 -5 -4 234.38 11.80 -8 5 4 235.08 11.40 -8 5 4 218.88 11.70 7 -5 -4 2044.50 57.39 7 -5 -4 1921.01 56.89 7 -5 -4 2062.99 56.89 -7 5 4 2020.40 57.09 -7 5 4 1986.00 57.09 -7 5 4 2071.79 57.39 6 -5 -4 152.78 8.60 6 -5 -4 136.49 7.40 6 -5 -4 129.99 7.70 -6 5 4 135.59 8.30 -6 5 4 136.69 8.10 -6 5 4 131.99 7.60 5 -5 -4 65.19 5.90 5 -5 -4 55.69 5.60 5 -5 -4 77.59 5.30 -5 5 4 81.29 6.20 -5 5 4 62.39 6.00 4 -5 -4 1467.95 41.70 4 -5 -4 1510.55 41.70 4 -5 -4 1449.35 40.60 -4 5 4 1455.45 41.80 -4 5 4 1421.36 41.80 3 -5 -4 802.62 22.90 3 -5 -4 765.42 24.00 3 -5 -4 777.52 24.30 -3 5 4 799.12 24.50 -3 5 4 802.82 24.50 2 -5 -4 134.69 7.10 2 -5 -4 140.89 7.90 -2 5 4 114.59 7.30 -2 5 4 128.69 7.50 1 -5 -4 2078.29 57.69 1 -5 -4 2036.80 56.79 -1 5 4 2045.20 57.39 -1 5 4 2037.90 57.59 0 -5 -4 22.00 3.70 0 -5 -4 23.00 4.40 0 5 4 28.60 4.60 0 5 4 20.60 4.20 -1 -5 -4 789.02 25.80 -1 -5 -4 769.92 24.50 -1 -5 -4 748.33 24.30 1 5 4 770.62 25.70 1 5 4 792.82 25.40 -2 -5 -4 32.50 5.40 -2 -5 -4 28.30 4.90 -2 -5 -4 40.50 5.20 2 5 4 29.40 6.10 2 5 4 39.50 5.70 -3 -5 -4 813.92 28.50 -3 -5 -4 862.41 28.00 -3 -5 -4 829.72 27.10 3 5 4 838.32 28.30 3 5 4 839.92 29.10 -4 -5 -4 980.50 32.40 -4 -5 -4 962.30 32.00 -4 -5 -4 924.31 30.70 4 5 4 934.31 33.10 4 5 4 963.30 36.40 -5 -5 -4 1045.40 34.30 -5 -5 -4 962.20 32.80 -5 -5 -4 988.60 34.20 5 5 4 973.70 27.40 5 5 4 948.81 35.00 -6 -5 -4 429.86 19.80 6 5 4 438.56 21.30 6 5 4 428.86 22.50 6 5 4 425.46 13.70 -7 -5 -4 72.09 10.30 -7 -5 -4 56.89 9.20 -7 -5 -4 40.70 10.00 7 5 4 83.29 12.40 7 5 4 67.99 5.70 13 -6 -4 272.37 20.40 13 -6 -4 293.07 20.10 13 -6 -4 331.27 17.80 -13 6 4 229.68 18.00 -13 6 4 279.67 20.30 -13 6 4 298.37 18.70 12 -6 -4 146.39 15.20 12 -6 -4 146.59 15.00 12 -6 -4 177.08 13.20 -12 6 4 153.28 13.60 -12 6 4 146.69 15.20 -12 6 4 170.38 14.00 11 -6 -4 8.60 6.20 11 -6 -4 9.20 6.30 -11 6 4 3.40 5.90 -11 6 4 -0.60 5.90 10 -6 -4 1024.10 35.10 10 -6 -4 1012.00 34.90 10 -6 -4 1106.39 34.20 -10 6 4 1155.18 35.90 -10 6 4 1029.60 34.50 9 -6 -4 50.89 6.70 9 -6 -4 66.39 7.00 9 -6 -4 55.69 6.90 -9 6 4 47.50 6.60 -9 6 4 40.30 6.00 -9 6 4 50.09 6.50 8 -6 -4 1387.86 40.70 8 -6 -4 1143.29 41.10 8 -6 -4 1336.47 40.20 -8 6 4 1398.96 40.50 -8 6 4 1332.97 40.20 -8 6 4 1376.46 40.40 7 -6 -4 1058.59 33.40 7 -6 -4 1122.89 33.50 7 -6 -4 1108.99 34.10 -7 6 4 1080.09 33.30 -7 6 4 1121.79 33.90 -7 6 4 1152.78 34.20 6 -6 -4 18.60 4.30 6 -6 -4 20.20 4.10 6 -6 -4 24.70 3.90 -6 6 4 24.70 4.60 -6 6 4 15.90 3.90 5 -6 -4 110.59 6.40 5 -6 -4 110.89 7.40 5 -6 -4 106.19 7.30 -5 6 4 109.79 7.80 -5 6 4 97.99 7.30 4 -6 -4 653.63 21.60 4 -6 -4 641.04 20.50 4 -6 -4 664.43 21.60 -4 6 4 689.73 22.10 -4 6 4 680.33 21.90 3 -6 -4 79.49 6.40 3 -6 -4 75.49 5.20 3 -6 -4 59.69 6.40 -3 6 4 81.69 6.90 -3 6 4 67.19 6.60 2 -6 -4 463.35 17.10 2 -6 -4 467.45 16.40 -2 6 4 483.75 17.00 -2 6 4 454.05 16.90 1 -6 -4 585.14 20.40 1 -6 -4 547.25 19.20 1 -6 -4 570.84 16.10 -1 6 4 600.54 20.20 -1 6 4 562.44 20.00 0 -6 -4 280.47 12.00 0 -6 -4 276.77 13.30 0 6 4 277.37 12.90 0 6 4 268.17 13.00 -1 -6 -4 1477.55 44.50 -1 -6 -4 1455.95 43.00 1 6 4 1435.16 44.20 -2 -6 -4 133.79 9.60 -2 -6 -4 121.79 10.60 -2 -6 -4 128.09 9.40 2 6 4 140.39 10.40 2 6 4 117.49 10.60 -3 -6 -4 225.68 12.50 -3 -6 -4 213.48 15.30 -3 -6 -4 205.08 13.90 3 6 4 223.18 14.30 -4 -6 -4 153.08 12.90 -4 -6 -4 131.09 17.20 4 6 4 135.79 13.60 -5 -6 -4 78.39 9.40 5 6 4 102.59 12.30 5 6 4 102.29 10.80 -6 -6 -4 0.00 7.20 -6 -6 -4 12.30 8.50 -6 -6 -4 -1.40 8.30 6 6 4 5.70 8.50 6 6 4 9.70 8.80 13 -7 -4 471.15 24.40 13 -7 -4 470.75 24.50 13 -7 -4 459.75 22.00 -13 7 4 431.66 22.30 -13 7 4 493.75 24.70 -13 7 4 423.76 22.30 12 -7 -4 103.49 11.70 12 -7 -4 86.79 9.00 12 -7 -4 94.39 11.60 -12 7 4 65.09 9.60 -12 7 4 72.69 10.20 -12 7 4 45.90 8.40 11 -7 -4 2.50 4.40 11 -7 -4 16.00 6.50 11 -7 -4 21.80 7.40 -11 7 4 21.20 6.40 -11 7 4 14.90 6.40 10 -7 -4 135.39 10.60 10 -7 -4 139.89 12.10 10 -7 -4 153.28 11.90 -10 7 4 126.69 11.60 -10 7 4 130.79 11.40 9 -7 -4 323.57 14.50 9 -7 -4 317.67 15.50 9 -7 -4 288.07 14.70 -9 7 4 357.66 16.00 -9 7 4 281.87 14.50 -9 7 4 312.77 14.90 8 -7 -4 34.00 5.50 8 -7 -4 33.80 5.40 8 -7 -4 40.30 5.80 -8 7 4 37.10 6.20 -8 7 4 43.20 5.70 -8 7 4 36.70 5.90 7 -7 -4 1034.40 33.10 7 -7 -4 1057.29 32.50 -7 7 4 1111.39 33.30 -7 7 4 1026.60 33.10 6 -7 -4 74.89 7.40 6 -7 -4 75.69 7.30 6 -7 -4 74.59 6.60 -6 7 4 77.49 7.50 -6 7 4 79.79 8.60 5 -7 -4 7.00 3.10 5 -7 -4 5.00 3.70 5 -7 -4 10.30 3.60 -5 7 4 5.60 3.50 -5 7 4 8.20 4.10 4 -7 -4 668.13 21.50 4 -7 -4 684.33 22.50 4 -7 -4 694.13 23.00 -4 7 4 672.03 22.80 -4 7 4 680.33 22.80 3 -7 -4 124.89 8.30 3 -7 -4 134.59 9.30 -3 7 4 129.59 8.90 -3 7 4 143.19 9.10 2 -7 -4 898.21 28.80 2 -7 -4 902.51 27.80 -2 7 4 775.32 30.10 -2 7 4 911.61 28.50 1 -7 -4 418.66 16.50 1 -7 -4 437.36 12.90 1 -7 -4 438.96 18.30 -1 7 4 437.96 17.20 -1 7 4 436.06 17.30 0 -7 -4 1321.87 39.80 0 -7 -4 1184.58 37.90 0 7 4 1321.77 39.30 0 7 4 1201.78 39.00 -1 -7 -4 1818.22 53.99 1 7 4 1753.02 53.59 -2 -7 -4 33.90 6.30 -2 -7 -4 39.70 10.40 -2 -7 -4 17.00 6.40 2 7 4 30.70 7.00 -3 -7 -4 284.07 16.00 -3 -7 -4 301.57 15.50 3 7 4 315.27 17.60 -4 -7 -4 173.88 13.60 -4 -7 -4 163.38 15.10 4 7 4 156.68 15.40 4 7 4 151.88 14.40 -5 -7 -4 3.20 8.80 -5 -7 -4 7.30 7.30 -5 -7 -4 -0.20 8.00 5 7 4 3.70 8.00 5 7 4 12.00 9.30 13 -8 -4 456.65 24.00 13 -8 -4 441.86 21.90 13 -8 -4 478.95 24.50 -13 8 4 443.26 23.00 -13 8 4 469.35 22.90 -13 8 4 449.86 24.20 12 -8 -4 72.29 10.60 12 -8 -4 72.39 9.10 12 -8 -4 69.19 10.50 -12 8 4 93.79 10.90 -12 8 4 101.19 11.40 -12 8 4 85.39 10.90 11 -8 -4 20.70 7.20 11 -8 -4 14.40 7.20 11 -8 -4 8.20 5.80 -11 8 4 4.20 6.10 -11 8 4 10.30 6.90 -11 8 4 15.90 6.50 10 -8 -4 471.15 19.60 10 -8 -4 406.26 25.10 -10 8 4 408.56 20.80 -10 8 4 466.85 19.40 9 -8 -4 265.37 13.60 9 -8 -4 270.07 13.90 9 -8 -4 232.08 14.10 -9 8 4 272.17 14.20 -9 8 4 258.87 13.60 -9 8 4 226.38 13.60 8 -8 -4 481.55 18.60 8 -8 -4 460.45 18.30 8 -8 -4 458.55 19.00 -8 8 4 479.85 19.00 -8 8 4 466.25 18.80 7 -8 -4 353.96 15.70 7 -8 -4 350.66 15.40 7 -8 -4 380.56 15.10 -7 8 4 371.76 16.10 -7 8 4 349.27 15.60 6 -8 -4 1167.48 35.30 6 -8 -4 1160.68 36.10 6 -8 -4 1178.28 35.90 -6 8 4 1113.09 35.90 -6 8 4 1198.08 36.50 5 -8 -4 3.20 3.50 5 -8 -4 7.90 4.30 5 -8 -4 -1.50 4.30 -5 8 4 -2.00 3.70 4 -8 -4 2065.59 58.19 4 -8 -4 2034.30 58.99 4 -8 -4 2125.89 59.89 -4 8 4 2089.09 59.59 -4 8 4 2020.10 59.49 3 -8 -4 572.24 20.60 3 -8 -4 597.64 21.70 -3 8 4 561.74 21.00 -3 8 4 562.64 21.00 2 -8 -4 616.94 18.20 2 -8 -4 610.04 22.70 2 -8 -4 577.34 21.50 -2 8 4 613.84 22.40 -2 8 4 618.34 22.40 1 -8 -4 26.80 6.40 1 -8 -4 33.20 3.70 1 -8 -4 25.90 5.20 -1 8 4 31.80 6.00 0 -8 -4 22.40 6.40 0 -8 -4 15.10 5.30 0 8 4 15.70 5.50 -1 -8 -4 170.18 12.60 1 8 4 168.78 13.70 -2 -8 -4 242.18 14.90 2 8 4 213.58 15.70 -3 -8 -4 188.78 14.20 -3 -8 -4 170.98 16.30 3 8 4 167.48 15.40 3 8 4 192.38 16.10 -4 -8 -4 24.90 8.10 -4 -8 -4 11.20 9.80 -4 -8 -4 22.70 9.00 4 8 4 33.30 15.70 4 8 4 13.00 9.20 13 -9 -4 33.20 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304.17 14.70 7 0 -10 8.20 2.40 7 0 -10 6.70 5.20 7 0 -10 8.90 2.80 -7 0 10 7.10 4.60 -7 0 10 15.10 4.50 -7 0 10 8.90 4.60 6 0 -10 309.07 14.60 -6 0 10 338.67 13.50 -6 0 10 321.17 13.50 -6 0 10 341.37 13.50 5 0 -10 100.69 8.40 -5 0 10 91.69 6.90 -5 0 10 101.89 7.10 -5 0 10 90.39 6.70 4 0 -10 182.78 9.90 -4 0 10 168.58 8.30 -4 0 10 187.98 7.90 -4 0 10 177.48 8.50 3 0 -10 1.80 3.10 -3 0 10 -0.30 2.40 -3 0 10 3.20 2.30 -3 0 10 4.70 2.10 -3 0 10 4.60 2.00 2 0 -10 387.56 14.10 -2 0 10 394.16 11.80 -2 0 10 376.36 12.90 -2 0 10 408.56 13.00 -1 0 10 103.79 5.90 -1 0 10 100.89 4.70 -1 0 10 94.59 5.70 -1 0 10 96.89 6.80 0 0 10 9.00 2.80 0 0 10 10.20 2.40 0 0 10 7.30 3.00 0 0 10 6.70 2.70 1 0 10 102.79 6.10 1 0 10 110.29 6.80 1 0 10 93.59 6.60 1 0 10 99.59 6.20 2 0 10 50.59 5.30 2 0 10 46.40 4.90 2 0 10 44.80 4.70 2 0 10 41.90 5.20 -3 0 -10 36.50 5.20 3 0 10 36.10 5.20 3 0 10 41.90 5.60 3 0 10 33.90 5.20 3 0 10 32.70 3.60 -4 0 -10 178.08 11.10 4 0 10 174.88 11.20 4 0 10 167.58 10.60 4 0 10 167.28 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6.60 -4 -1 15 71.99 7.80 -3 -1 15 446.26 16.00 -3 -1 15 435.46 15.90 -2 -1 15 4.90 3.90 -2 -1 15 6.60 3.70 -1 -1 15 485.55 16.50 -1 -1 15 455.65 16.40 -4 0 15 240.68 12.20 -4 0 15 258.87 12.60 -3 0 15 184.58 10.40 -2 0 15 126.79 9.10 -4 1 15 8.40 5.20 -4 1 15 -9.90 4.70 -3 1 15 337.37 14.90 -3 1 15 323.37 14.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 86799 #============================================================================== _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====================================================