data_MR15_a _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H21 P Se' _chemical_formula_weight 479.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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 9.8524(2) _cell_length_b 12.4381(2) _cell_length_c 18.8967(3) _cell_angle_alpha 87.7967(7) _cell_angle_beta 89.7792(8) _cell_angle_gamma 75.5730(6) _cell_volume 2240.98(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 26.35 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.421 _exptl_crystal_F_000 976 _exptl_transmission_factor_min 0.3483 _exptl_transmission_factor_max 0.4077 _exptl_crystal_size_max 0.380 _exptl_crystal_size_mid 0.290 _exptl_crystal_size_min 0.170 _exptl_absorpt_coefficient_mu 1.761 _shelx_estimated_absorpt_T_min 0.554 _shelx_estimated_absorpt_T_max 0.754 _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 76227 _diffrn_reflns_av_unetI/netI 0.0375 _diffrn_reflns_av_R_equivalents 0.0725 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.134 _diffrn_reflns_theta_max 26.473 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 9231 _reflns_number_gt 7511 _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^)+(0.0336P)^2^+2.2795P] 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 9231 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0357 _refine_ls_wR_factor_ref 0.0831 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _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 0.6902(2) 0.43582(19) 0.23668(13) 0.0127(5) Uani 1 1 d . . . . . C2 C 0.6853(2) 0.5370(2) 0.20957(13) 0.0139(5) Uani 1 1 d . . . . . H2 H 0.7209 0.5870 0.2365 0.017 Uiso 1 1 calc R U . . . C3 C 0.6235(2) 0.5743(2) 0.13580(13) 0.0142(5) Uani 1 1 d . . . . . C4 C 0.4739(2) 0.5577(2) 0.13625(13) 0.0144(5) Uani 1 1 d . . . . . H4 H 0.3973 0.6181 0.1228 0.017 Uiso 1 1 calc R U . . . C5 C 0.4504(3) 0.4596(2) 0.15521(13) 0.0153(5) Uani 1 1 d . . . . . C6 C 0.3111(2) 0.4368(2) 0.16190(13) 0.0150(5) Uani 1 1 d . . . . . C7 C 0.2027(3) 0.5136(2) 0.19474(13) 0.0180(5) Uani 1 1 d . . . . . H7 H 0.2198 0.5793 0.2129 0.022 Uiso 1 1 calc R U . . . C8 C 0.0709(3) 0.4939(2) 0.20072(14) 0.0221(6) Uani 1 1 d . . . . . H8 H -0.0021 0.5456 0.2234 0.026 Uiso 1 1 calc R U . . . C9 C 0.0453(3) 0.3989(2) 0.17375(14) 0.0226(6) Uani 1 1 d . . . . . H9 H -0.0454 0.3857 0.1779 0.027 Uiso 1 1 calc R U . . . C10 C 0.1511(3) 0.3227(2) 0.14062(14) 0.0209(6) Uani 1 1 d . . . . . H10 H 0.1328 0.2581 0.1216 0.025 Uiso 1 1 calc R U . . . C11 C 0.2838(3) 0.3416(2) 0.13545(13) 0.0173(5) Uani 1 1 d . . . . . H11 H 0.3568 0.2888 0.1136 0.021 Uiso 1 1 calc R U . . . C12 C 0.7595(2) 0.3915(2) 0.30497(13) 0.0148(5) Uani 1 1 d . . . . . C13 C 0.7383(3) 0.4565(2) 0.36420(14) 0.0199(6) Uani 1 1 d . . . . . H13 H 0.6702 0.5258 0.3624 0.024 Uiso 1 1 calc R U . . . C14 C 0.8152(3) 0.4214(2) 0.42593(15) 0.0254(6) Uani 1 1 d . . . . . H14 H 0.7993 0.4664 0.4661 0.030 Uiso 1 1 calc R U . . . C15 C 0.9152(3) 0.3208(2) 0.42883(15) 0.0271(6) Uani 1 1 d . . . . . H15 H 0.9696 0.2973 0.4706 0.033 Uiso 1 1 calc R U . . . C16 C 0.9356(3) 0.2546(2) 0.37059(15) 0.0252(6) Uani 1 1 d . . . . . H16 H 1.0035 0.1853 0.3726 0.030 Uiso 1 1 calc R U . . . C17 C 0.8577(3) 0.2887(2) 0.30941(14) 0.0200(6) Uani 1 1 d . . . . . H17 H 0.8710 0.2419 0.2701 0.024 Uiso 1 1 calc R U . . . C18 C 0.6264(3) 0.6916(2) 0.11061(13) 0.0152(5) Uani 1 1 d . . . . . C19 C 0.5583(3) 0.7334(2) 0.04728(14) 0.0190(6) Uani 1 1 d . . . . . H19 H 0.5025 0.6923 0.0248 0.023 Uiso 1 1 calc R U . . . C20 C 0.5699(3) 0.8334(2) 0.01619(15) 0.0234(6) Uani 1 1 d . . . . . H20 H 0.5233 0.8599 -0.0273 0.028 Uiso 1 1 calc R U . . . C21 C 0.6497(3) 0.8944(2) 0.04898(16) 0.0289(7) Uani 1 1 d . . . . . H21 H 0.6589 0.9628 0.0279 0.035 Uiso 1 1 calc R U . . . C22 C 0.7162(3) 0.8554(2) 0.11262(17) 0.0297(7) Uani 1 1 d . . . . . H22 H 0.7695 0.8978 0.1357 0.036 Uiso 1 1 calc R U . . . C23 C 0.7053(3) 0.7539(2) 0.14303(15) 0.0222(6) Uani 1 1 d . . . . . H23 H 0.7525 0.7272 0.1864 0.027 Uiso 1 1 calc R U . . . C24 C 0.7126(2) 0.3778(2) 0.09777(13) 0.0145(5) Uani 1 1 d . . . . . C25 C 0.7116(2) 0.4887(2) 0.08437(13) 0.0134(5) Uani 1 1 d . . . . . C26 C 0.7914(3) 0.5154(2) 0.02920(13) 0.0158(5) Uani 1 1 d . . . . . H26 H 0.7933 0.5905 0.0196 0.019 Uiso 1 1 calc R U . . . C27 C 0.8692(3) 0.4314(2) -0.01237(14) 0.0174(5) Uani 1 1 d . . . . . H27 H 0.9232 0.4501 -0.0505 0.021 Uiso 1 1 calc R U . . . C28 C 0.8687(3) 0.3222(2) 0.00107(14) 0.0187(5) Uani 1 1 d . . . . . H28 H 0.9220 0.2660 -0.0276 0.022 Uiso 1 1 calc R U . . . C29 C 0.7896(3) 0.2938(2) 0.05704(13) 0.0159(5) Uani 1 1 d . . . . . H29 H 0.7885 0.2186 0.0670 0.019 Uiso 1 1 calc R U . . . C30 C 0.3202(2) 0.00518(19) 0.26189(13) 0.0132(5) Uani 1 1 d . . . . . C31 C 0.3233(2) 0.1037(2) 0.28605(13) 0.0131(5) Uani 1 1 d . . . . . H31 H 0.2796 0.1697 0.2596 0.016 Uiso 1 1 calc R U . . . C32 C 0.3971(2) 0.11126(19) 0.35646(13) 0.0128(5) Uani 1 1 d . . . . . C33 C 0.5474(2) 0.0382(2) 0.35153(13) 0.0134(5) Uani 1 1 d . . . . . H33 H 0.6239 0.0699 0.3600 0.016 Uiso 1 1 calc R U . . . C34 C 0.5733(3) -0.0686(2) 0.33563(13) 0.0140(5) Uani 1 1 d . . . . . C35 C 0.7164(2) -0.1420(2) 0.33035(13) 0.0142(5) Uani 1 1 d . . . . . C36 C 0.8209(3) -0.1027(2) 0.29550(14) 0.0183(5) Uani 1 1 d . . . . . H36 H 0.7978 -0.0319 0.2716 0.022 Uiso 1 1 calc R U . . . C37 C 0.9582(3) -0.1665(2) 0.29555(15) 0.0224(6) Uani 1 1 d . . . . . H37 H 1.0285 -0.1391 0.2717 0.027 Uiso 1 1 calc R U . . . C38 C 0.9932(3) -0.2698(2) 0.33004(15) 0.0230(6) Uani 1 1 d . . . . . H38 H 1.0876 -0.3127 0.3306 0.028 Uiso 1 1 calc R U . . . C39 C 0.8904(3) -0.3102(2) 0.36362(15) 0.0232(6) Uani 1 1 d . . . . . H39 H 0.9143 -0.3815 0.3868 0.028 Uiso 1 1 calc R U . . . C40 C 0.7524(3) -0.2474(2) 0.36376(14) 0.0183(5) Uani 1 1 d . . . . . H40 H 0.6822 -0.2763 0.3866 0.022 Uiso 1 1 calc R U . . . C41 C 0.2365(3) -0.0123(2) 0.20082(13) 0.0143(5) Uani 1 1 d . . . . . C42 C 0.2948(3) -0.0828(2) 0.14703(14) 0.0197(6) Uani 1 1 d . . . . . H42 H 0.3917 -0.1195 0.1483 0.024 Uiso 1 1 calc R U . . . C43 C 0.2111(3) -0.0992(2) 0.09159(15) 0.0254(6) Uani 1 1 d . . . . . H43 H 0.2515 -0.1463 0.0547 0.030 Uiso 1 1 calc R U . . . C44 C 0.0694(3) -0.0476(2) 0.08952(15) 0.0243(6) Uani 1 1 d . . . . . H44 H 0.0125 -0.0608 0.0520 0.029 Uiso 1 1 calc R U . . . C45 C 0.0108(3) 0.0233(2) 0.14226(15) 0.0223(6) Uani 1 1 d . . . . . H45 H -0.0863 0.0595 0.1408 0.027 Uiso 1 1 calc R U . . . C46 C 0.0942(3) 0.0411(2) 0.19709(14) 0.0174(5) Uani 1 1 d . . . . . H46 H 0.0538 0.0907 0.2328 0.021 Uiso 1 1 calc R U . . . C47 C 0.3968(3) 0.2281(2) 0.37714(13) 0.0155(5) Uani 1 1 d . . . . . C48 C 0.4802(3) 0.2393(2) 0.43442(16) 0.0270(7) Uani 1 1 d . . . . . H48 H 0.5365 0.1746 0.4578 0.032 Uiso 1 1 calc R U . . . C49 C 0.4828(3) 0.3425(3) 0.45791(18) 0.0328(7) Uani 1 1 d . . . . . H49 H 0.5399 0.3482 0.4973 0.039 Uiso 1 1 calc R U . . . C50 C 0.4030(3) 0.4366(2) 0.42444(16) 0.0318(7) Uani 1 1 d . . . . . H50 H 0.4061 0.5078 0.4398 0.038 Uiso 1 1 calc R U . . . C51 C 0.3188(4) 0.4274(2) 0.36860(16) 0.0402(9) Uani 1 1 d . . . . . H51 H 0.2629 0.4927 0.3457 0.048 Uiso 1 1 calc R U . . . C52 C 0.3142(3) 0.3238(2) 0.34505(15) 0.0284(7) Uani 1 1 d . . . . . H52 H 0.2540 0.3188 0.3068 0.034 Uiso 1 1 calc R U . . . C53 C 0.3189(2) -0.0567(2) 0.40091(13) 0.0146(5) Uani 1 1 d . . . . . C54 C 0.3197(2) 0.0536(2) 0.41271(13) 0.0138(5) Uani 1 1 d . . . . . C55 C 0.2488(3) 0.1051(2) 0.47045(13) 0.0168(5) Uani 1 1 d . . . . . H55 H 0.2487 0.1798 0.4794 0.020 Uiso 1 1 calc R U . . . C56 C 0.1774(3) 0.0467(2) 0.51558(14) 0.0210(6) Uani 1 1 d . . . . . H56 H 0.1288 0.0821 0.5552 0.025 Uiso 1 1 calc R U . . . C57 C 0.1767(3) -0.0616(2) 0.50326(14) 0.0219(6) Uani 1 1 d . . . . . H57 H 0.1277 -0.1003 0.5344 0.026 Uiso 1 1 calc R U . . . C58 C 0.2473(3) -0.1144(2) 0.44546(14) 0.0176(5) Uani 1 1 d . . . . . H58 H 0.2466 -0.1889 0.4366 0.021 Uiso 1 1 calc R U . . . P1 P 0.61439(6) 0.35463(5) 0.17572(3) 0.01337(14) Uani 1 1 d . . . . . P2 P 0.41042(6) -0.11041(5) 0.32149(3) 0.01326(14) Uani 1 1 d . . . . . Se1 Se 0.61174(3) 0.18998(2) 0.20126(2) 0.01959(8) Uani 1 1 d . . . . . Se2 Se 0.41331(3) -0.27397(2) 0.29756(2) 0.01913(7) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0084(11) 0.0139(12) 0.0147(13) -0.0022(9) 0.0027(9) -0.0004(9) C2 0.0081(11) 0.0150(12) 0.0174(13) -0.0021(10) 0.0023(10) -0.0008(9) C3 0.0110(12) 0.0143(12) 0.0165(13) -0.0019(10) 0.0004(10) -0.0015(9) C4 0.0104(12) 0.0150(12) 0.0159(13) -0.0007(9) -0.0011(10) 0.0002(9) C5 0.0107(12) 0.0174(13) 0.0162(13) -0.0005(10) 0.0005(10) -0.0003(10) C6 0.0091(12) 0.0196(13) 0.0150(13) 0.0035(10) -0.0017(10) -0.0020(10) C7 0.0147(13) 0.0234(14) 0.0149(13) -0.0016(10) -0.0012(10) -0.0027(10) C8 0.0102(12) 0.0343(16) 0.0195(14) 0.0000(11) 0.0022(11) -0.0016(11) C9 0.0104(13) 0.0358(16) 0.0218(15) 0.0098(12) -0.0022(11) -0.0075(11) C10 0.0186(14) 0.0240(14) 0.0216(15) 0.0071(11) -0.0070(11) -0.0092(11) C11 0.0145(13) 0.0202(13) 0.0168(13) 0.0027(10) -0.0005(10) -0.0039(10) C12 0.0103(12) 0.0174(13) 0.0169(13) 0.0027(10) 0.0013(10) -0.0040(10) C13 0.0186(13) 0.0186(13) 0.0225(15) 0.0019(10) 0.0011(11) -0.0052(10) C14 0.0331(16) 0.0298(16) 0.0165(14) -0.0006(11) -0.0009(12) -0.0137(13) C15 0.0267(16) 0.0345(17) 0.0207(15) 0.0106(12) -0.0067(12) -0.0102(13) C16 0.0192(14) 0.0254(15) 0.0275(16) 0.0084(12) 0.0004(12) -0.0005(11) C17 0.0167(13) 0.0202(14) 0.0210(14) 0.0006(10) 0.0023(11) -0.0011(10) C18 0.0122(12) 0.0140(12) 0.0176(13) 0.0005(10) 0.0033(10) -0.0005(10) C19 0.0163(13) 0.0154(13) 0.0223(14) -0.0009(10) 0.0011(11) 0.0012(10) C20 0.0244(15) 0.0191(14) 0.0213(15) 0.0056(11) 0.0034(12) 0.0037(11) C21 0.0364(17) 0.0134(13) 0.0348(18) 0.0049(12) 0.0031(14) -0.0035(12) C22 0.0342(17) 0.0205(15) 0.0377(18) 0.0017(12) -0.0021(14) -0.0136(13) C23 0.0228(14) 0.0197(14) 0.0249(15) 0.0059(11) -0.0022(12) -0.0077(11) C24 0.0091(12) 0.0181(13) 0.0167(13) 0.0006(10) -0.0003(10) -0.0040(10) C25 0.0083(11) 0.0150(12) 0.0164(13) -0.0006(9) -0.0019(10) -0.0022(9) C26 0.0137(12) 0.0160(12) 0.0176(13) 0.0019(10) -0.0018(10) -0.0038(10) C27 0.0120(12) 0.0246(14) 0.0149(13) 0.0001(10) 0.0006(10) -0.0034(10) C28 0.0152(13) 0.0221(14) 0.0180(14) -0.0071(10) 0.0008(11) -0.0025(10) C29 0.0144(12) 0.0140(12) 0.0196(14) -0.0018(10) -0.0015(10) -0.0041(10) C30 0.0101(12) 0.0141(12) 0.0151(13) -0.0005(9) 0.0005(10) -0.0023(9) C31 0.0102(12) 0.0153(12) 0.0132(13) -0.0007(9) 0.0021(10) -0.0019(9) C32 0.0123(12) 0.0136(12) 0.0124(12) -0.0020(9) -0.0005(10) -0.0027(9) C33 0.0107(12) 0.0172(12) 0.0124(12) 0.0013(9) -0.0012(10) -0.0037(9) C34 0.0123(12) 0.0171(12) 0.0129(13) -0.0012(9) -0.0015(10) -0.0043(10) C35 0.0121(12) 0.0144(12) 0.0162(13) -0.0039(10) -0.0020(10) -0.0029(9) C36 0.0182(13) 0.0172(13) 0.0189(14) -0.0008(10) 0.0003(11) -0.0031(10) C37 0.0164(13) 0.0244(14) 0.0279(16) -0.0047(11) 0.0066(11) -0.0074(11) C38 0.0124(13) 0.0199(14) 0.0339(17) -0.0069(11) 0.0018(12) 0.0018(10) C39 0.0183(14) 0.0159(13) 0.0331(17) 0.0018(11) -0.0030(12) -0.0004(11) C40 0.0135(13) 0.0179(13) 0.0242(15) -0.0020(10) -0.0015(11) -0.0051(10) C41 0.0158(13) 0.0131(12) 0.0146(13) -0.0009(9) -0.0009(10) -0.0047(10) C42 0.0163(13) 0.0232(14) 0.0193(14) -0.0066(11) -0.0003(11) -0.0033(11) C43 0.0277(15) 0.0297(15) 0.0206(15) -0.0108(12) 0.0003(12) -0.0093(12) C44 0.0277(15) 0.0251(15) 0.0221(15) 0.0008(11) -0.0112(12) -0.0101(12) C45 0.0174(13) 0.0195(14) 0.0284(16) 0.0040(11) -0.0073(12) -0.0021(11) C46 0.0185(13) 0.0138(12) 0.0185(14) -0.0009(10) -0.0023(11) -0.0013(10) C47 0.0149(13) 0.0150(12) 0.0173(13) -0.0045(10) 0.0029(10) -0.0048(10) C48 0.0200(14) 0.0219(14) 0.0367(18) -0.0117(12) -0.0080(13) 0.0012(11) C49 0.0240(16) 0.0339(17) 0.0426(19) -0.0207(14) -0.0041(14) -0.0080(13) C50 0.050(2) 0.0203(15) 0.0311(17) -0.0159(12) 0.0087(15) -0.0173(14) C51 0.074(3) 0.0153(15) 0.0252(17) -0.0018(12) -0.0070(16) 0.0008(15) C52 0.0439(18) 0.0161(14) 0.0212(15) -0.0038(11) -0.0093(13) 0.0006(12) C53 0.0112(12) 0.0194(13) 0.0119(13) 0.0006(10) -0.0027(10) -0.0016(10) C54 0.0093(12) 0.0168(12) 0.0143(13) 0.0019(9) -0.0049(10) -0.0015(9) C55 0.0126(12) 0.0212(13) 0.0146(13) -0.0018(10) -0.0046(10) -0.0004(10) C56 0.0141(13) 0.0349(16) 0.0121(13) -0.0016(11) -0.0019(10) -0.0026(11) C57 0.0131(13) 0.0319(16) 0.0206(15) 0.0080(11) -0.0020(11) -0.0069(11) C58 0.0129(12) 0.0188(13) 0.0205(14) 0.0048(10) -0.0054(10) -0.0036(10) P1 0.0099(3) 0.0124(3) 0.0175(3) 0.0010(2) 0.0013(3) -0.0026(2) P2 0.0108(3) 0.0119(3) 0.0167(3) -0.0012(2) -0.0011(3) -0.0020(2) Se1 0.01642(14) 0.01334(13) 0.02875(16) 0.00303(10) 0.00329(11) -0.00383(10) Se2 0.01616(14) 0.01199(13) 0.02958(16) -0.00381(10) -0.00137(11) -0.00366(10) _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 1.483(3) . ? C1 P1 1.837(2) . ? C2 C3 1.531(3) . ? C2 H2 0.9500 . ? C3 C18 1.524(3) . ? C3 C4 1.539(3) . ? C3 C25 1.563(3) . ? C4 C5 1.332(3) . ? C4 H4 0.9500 . ? C5 C6 1.474(3) . ? C5 P1 1.839(2) . ? C6 C11 1.389(4) . ? C6 C7 1.404(3) . ? C7 C8 1.384(4) . ? C7 H7 0.9500 . ? C8 C9 1.384(4) . ? C8 H8 0.9500 . ? C9 C10 1.387(4) . ? C9 H9 0.9500 . ? C10 C11 1.387(4) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 C17 1.398(3) . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 C16 1.384(4) . ? C15 H15 0.9500 . ? C16 C17 1.383(4) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C23 1.386(4) . ? C18 C19 1.392(4) . ? C19 C20 1.385(4) . ? C19 H19 0.9500 . ? C20 C21 1.384(4) . ? C20 H20 0.9500 . ? C21 C22 1.383(4) . ? C21 H21 0.9500 . ? C22 C23 1.395(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C29 1.386(3) . ? C24 C25 1.391(3) . ? C24 P1 1.812(3) . ? C25 C26 1.383(3) . ? C26 C27 1.399(3) . ? C26 H26 0.9500 . ? C27 C28 1.373(4) . ? C27 H27 0.9500 . ? C28 C29 1.397(4) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? C30 C31 1.331(3) . ? C30 C41 1.475(3) . ? C30 P2 1.836(2) . ? C31 C32 1.536(3) . ? C31 H31 0.9500 . ? C32 C47 1.518(3) . ? C32 C33 1.537(3) . ? C32 C54 1.560(3) . ? C33 C34 1.334(3) . ? C33 H33 0.9500 . ? C34 C35 1.483(3) . ? C34 P2 1.829(2) . ? C35 C40 1.396(3) . ? C35 C36 1.398(4) . ? C36 C37 1.387(4) . ? C36 H36 0.9500 . ? C37 C38 1.382(4) . ? C37 H37 0.9500 . ? C38 C39 1.380(4) . ? C38 H38 0.9500 . ? C39 C40 1.389(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C46 1.394(3) . ? C41 C42 1.395(3) . ? C42 C43 1.388(4) . ? C42 H42 0.9500 . ? C43 C44 1.384(4) . ? C43 H43 0.9500 . ? C44 C45 1.383(4) . ? C44 H44 0.9500 . ? C45 C46 1.383(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C52 1.383(4) . ? C47 C48 1.394(4) . ? C48 C49 1.380(4) . ? C48 H48 0.9500 . ? C49 C50 1.370(4) . ? C49 H49 0.9500 . ? C50 C51 1.371(4) . ? C50 H50 0.9500 . ? C51 C52 1.391(4) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C58 1.386(4) . ? C53 C54 1.400(3) . ? C53 P2 1.811(3) . ? C54 C55 1.384(3) . ? C55 C56 1.397(4) . ? C55 H55 0.9500 . ? C56 C57 1.378(4) . ? C56 H56 0.9500 . ? C57 C58 1.389(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? P1 Se1 2.0924(7) . ? P2 Se2 2.0943(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C12 123.7(2) . . ? C2 C1 P1 111.64(19) . . ? C12 C1 P1 124.46(18) . . ? C1 C2 C3 121.2(2) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C18 C3 C2 115.9(2) . . ? C18 C3 C4 111.97(19) . . ? C2 C3 C4 106.5(2) . . ? C18 C3 C25 109.5(2) . . ? C2 C3 C25 105.28(18) . . ? C4 C3 C25 107.11(19) . . ? C5 C4 C3 120.8(2) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 C6 125.2(2) . . ? C4 C5 P1 111.76(18) . . ? C6 C5 P1 123.02(18) . . ? C11 C6 C7 119.1(2) . . ? C11 C6 C5 121.5(2) . . ? C7 C6 C5 119.4(2) . . ? C8 C7 C6 120.0(2) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C9 C8 C7 120.1(2) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 120.4(2) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C11 C10 C9 119.6(3) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C6 120.7(2) . . ? C10 C11 H11 119.6 . . ? C6 C11 H11 119.6 . . ? C13 C12 C17 118.5(2) . . ? C13 C12 C1 120.3(2) . . ? C17 C12 C1 120.8(2) . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 119.9(3) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 120.4(3) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C16 C17 C12 120.5(3) . . ? C16 C17 H17 119.7 . . ? C12 C17 H17 119.7 . . ? C23 C18 C19 118.1(2) . . ? C23 C18 C3 123.6(2) . . ? C19 C18 C3 118.0(2) . . ? C20 C19 C18 121.7(3) . . ? C20 C19 H19 119.1 . . ? C18 C19 H19 119.1 . . ? C21 C20 C19 119.5(3) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C22 C21 C20 119.7(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.3(3) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 120.7(3) . . ? C18 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C29 C24 C25 122.0(2) . . ? C29 C24 P1 124.24(19) . . ? C25 C24 P1 113.64(18) . . ? C26 C25 C24 118.7(2) . . ? C26 C25 C3 124.6(2) . . ? C24 C25 C3 116.6(2) . . ? C25 C26 C27 119.8(2) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.0(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.9(2) . . ? C27 C28 H28 120.1 . . ? C29 C28 H28 120.1 . . ? C24 C29 C28 118.6(2) . . ? C24 C29 H29 120.7 . . ? C28 C29 H29 120.7 . . ? C31 C30 C41 125.2(2) . . ? C31 C30 P2 112.37(18) . . ? C41 C30 P2 121.79(17) . . ? C30 C31 C32 120.4(2) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C47 C32 C31 115.2(2) . . ? C47 C32 C33 111.1(2) . . ? C31 C32 C33 107.20(19) . . ? C47 C32 C54 111.1(2) . . ? C31 C32 C54 104.76(19) . . ? C33 C32 C54 106.88(19) . . ? C34 C33 C32 121.7(2) . . ? C34 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C33 C34 C35 123.5(2) . . ? C33 C34 P2 111.18(18) . . ? C35 C34 P2 125.33(18) . . ? C40 C35 C36 118.7(2) . . ? C40 C35 C34 121.4(2) . . ? C36 C35 C34 119.7(2) . . ? C37 C36 C35 120.4(2) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.4(3) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 119.7(2) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 120.6(2) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C35 120.2(2) . . ? C39 C40 H40 119.9 . . ? C35 C40 H40 119.9 . . ? C46 C41 C42 118.7(2) . . ? C46 C41 C30 119.4(2) . . ? C42 C41 C30 121.9(2) . . ? C43 C42 C41 119.9(2) . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C44 C43 C42 120.7(3) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C45 C44 C43 119.8(2) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.7(2) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? C45 C46 C41 121.2(2) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? C52 C47 C48 117.9(2) . . ? C52 C47 C32 124.3(2) . . ? C48 C47 C32 117.7(2) . . ? C49 C48 C47 121.4(3) . . ? C49 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? C50 C49 C48 120.0(3) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 119.6(3) . . ? C49 C50 H50 120.2 . . ? C51 C50 H50 120.2 . . ? C50 C51 C52 120.9(3) . . ? C50 C51 H51 119.6 . . ? C52 C51 H51 119.6 . . ? C47 C52 C51 120.2(3) . . ? C47 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C58 C53 C54 121.3(2) . . ? C58 C53 P2 124.9(2) . . ? C54 C53 P2 113.76(18) . . ? C55 C54 C53 119.1(2) . . ? C55 C54 C32 124.6(2) . . ? C53 C54 C32 116.3(2) . . ? C54 C55 C56 119.6(2) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C57 C56 C55 120.8(2) . . ? C57 C56 H56 119.6 . . ? C55 C56 H56 119.6 . . ? C56 C57 C58 120.2(2) . . ? C56 C57 H57 119.9 . . ? C58 C57 H57 119.9 . . ? C53 C58 C57 119.0(2) . . ? C53 C58 H58 120.5 . . ? C57 C58 H58 120.5 . . ? C24 P1 C1 97.43(11) . . ? C24 P1 C5 98.41(11) . . ? C1 P1 C5 97.88(11) . . ? C24 P1 Se1 116.60(8) . . ? C1 P1 Se1 121.17(8) . . ? C5 P1 Se1 120.49(8) . . ? C53 P2 C34 98.73(11) . . ? C53 P2 C30 95.97(11) . . ? C34 P2 C30 99.16(11) . . ? C53 P2 Se2 117.13(9) . . ? C34 P2 Se2 121.05(8) . . ? C30 P2 Se2 119.88(8) . . ? 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 174.6(2) . . . . ? P1 C1 C2 C3 -0.5(3) . . . . ? C1 C2 C3 C18 -179.1(2) . . . . ? C1 C2 C3 C4 55.6(3) . . . . ? C1 C2 C3 C25 -57.9(3) . . . . ? C18 C3 C4 C5 178.5(2) . . . . ? C2 C3 C4 C5 -53.8(3) . . . . ? C25 C3 C4 C5 58.4(3) . . . . ? C3 C4 C5 C6 175.8(2) . . . . ? C3 C4 C5 P1 -2.1(3) . . . . ? C4 C5 C6 C11 135.9(3) . . . . ? P1 C5 C6 C11 -46.4(3) . . . . ? C4 C5 C6 C7 -43.0(4) . . . . ? P1 C5 C6 C7 134.7(2) . . . . ? C11 C6 C7 C8 0.3(4) . . . . ? C5 C6 C7 C8 179.3(2) . . . . ? C6 C7 C8 C9 -0.6(4) . . . . ? C7 C8 C9 C10 0.1(4) . . . . ? C8 C9 C10 C11 0.8(4) . . . . ? C9 C10 C11 C6 -1.2(4) . . . . ? C7 C6 C11 C10 0.6(4) . . . . ? C5 C6 C11 C10 -178.4(2) . . . . ? C2 C1 C12 C13 45.3(4) . . . . ? P1 C1 C12 C13 -140.3(2) . . . . ? C2 C1 C12 C17 -128.3(3) . . . . ? P1 C1 C12 C17 46.1(3) . . . . ? C17 C12 C13 C14 1.5(4) . . . . ? C1 C12 C13 C14 -172.2(2) . . . . ? C12 C13 C14 C15 0.4(4) . . . . ? C13 C14 C15 C16 -1.5(4) . . . . ? C14 C15 C16 C17 0.6(4) . . . . ? C15 C16 C17 C12 1.4(4) . . . . ? C13 C12 C17 C16 -2.4(4) . . . . ? C1 C12 C17 C16 171.3(2) . . . . ? C2 C3 C18 C23 13.9(3) . . . . ? C4 C3 C18 C23 136.4(3) . . . . ? C25 C3 C18 C23 -105.0(3) . . . . ? C2 C3 C18 C19 -173.4(2) . . . . ? C4 C3 C18 C19 -50.9(3) . . . . ? C25 C3 C18 C19 67.7(3) . . . . ? C23 C18 C19 C20 1.0(4) . . . . ? C3 C18 C19 C20 -172.1(2) . . . . ? C18 C19 C20 C21 -0.7(4) . . . . ? C19 C20 C21 C22 -0.5(4) . . . . ? C20 C21 C22 C23 1.3(5) . . . . ? C19 C18 C23 C22 -0.2(4) . . . . ? C3 C18 C23 C22 172.5(3) . . . . ? C21 C22 C23 C18 -1.0(4) . . . . ? C29 C24 C25 C26 -0.8(4) . . . . ? P1 C24 C25 C26 175.42(18) . . . . ? C29 C24 C25 C3 -178.3(2) . . . . ? P1 C24 C25 C3 -2.1(3) . . . . ? C18 C3 C25 C26 6.3(3) . . . . ? C2 C3 C25 C26 -119.0(2) . . . . ? C4 C3 C25 C26 127.9(2) . . . . ? C18 C3 C25 C24 -176.3(2) . . . . ? C2 C3 C25 C24 58.4(3) . . . . ? C4 C3 C25 C24 -54.7(3) . . . . ? C24 C25 C26 C27 0.9(4) . . . . ? C3 C25 C26 C27 178.3(2) . . . . ? C25 C26 C27 C28 -0.6(4) . . . . ? C26 C27 C28 C29 0.0(4) . . . . ? C25 C24 C29 C28 0.2(4) . . . . ? P1 C24 C29 C28 -175.57(19) . . . . ? C27 C28 C29 C24 0.2(4) . . . . ? C41 C30 C31 C32 170.9(2) . . . . ? P2 C30 C31 C32 0.2(3) . . . . ? C30 C31 C32 C47 178.4(2) . . . . ? C30 C31 C32 C33 54.1(3) . . . . ? C30 C31 C32 C54 -59.2(3) . . . . ? C47 C32 C33 C34 178.5(2) . . . . ? C31 C32 C33 C34 -54.8(3) . . . . ? C54 C32 C33 C34 57.1(3) . . . . ? C32 C33 C34 C35 -180.0(2) . . . . ? C32 C33 C34 P2 0.1(3) . . . . ? C33 C34 C35 C40 132.1(3) . . . . ? P2 C34 C35 C40 -48.0(3) . . . . ? C33 C34 C35 C36 -43.4(4) . . . . ? P2 C34 C35 C36 136.6(2) . . . . ? C40 C35 C36 C37 -1.4(4) . . . . ? C34 C35 C36 C37 174.2(2) . . . . ? C35 C36 C37 C38 0.0(4) . . . . ? C36 C37 C38 C39 1.0(4) . . . . ? C37 C38 C39 C40 -0.8(4) . . . . ? C38 C39 C40 C35 -0.6(4) . . . . ? C36 C35 C40 C39 1.7(4) . . . . ? C34 C35 C40 C39 -173.8(2) . . . . ? C31 C30 C41 C46 -50.1(4) . . . . ? P2 C30 C41 C46 119.8(2) . . . . ? C31 C30 C41 C42 131.3(3) . . . . ? P2 C30 C41 C42 -58.9(3) . . . . ? C46 C41 C42 C43 -0.5(4) . . . . ? C30 C41 C42 C43 178.2(2) . . . . ? C41 C42 C43 C44 -1.0(4) . . . . ? C42 C43 C44 C45 1.6(4) . . . . ? C43 C44 C45 C46 -0.6(4) . . . . ? C44 C45 C46 C41 -0.9(4) . . . . ? C42 C41 C46 C45 1.5(4) . . . . ? C30 C41 C46 C45 -177.2(2) . . . . ? C31 C32 C47 C52 13.0(4) . . . . ? C33 C32 C47 C52 135.2(3) . . . . ? C54 C32 C47 C52 -106.0(3) . . . . ? C31 C32 C47 C48 -170.2(2) . . . . ? C33 C32 C47 C48 -48.1(3) . . . . ? C54 C32 C47 C48 70.8(3) . . . . ? C52 C47 C48 C49 -1.1(4) . . . . ? C32 C47 C48 C49 -178.1(3) . . . . ? C47 C48 C49 C50 -0.5(5) . . . . ? C48 C49 C50 C51 1.4(5) . . . . ? C49 C50 C51 C52 -0.6(5) . . . . ? C48 C47 C52 C51 1.9(4) . . . . ? C32 C47 C52 C51 178.7(3) . . . . ? C50 C51 C52 C47 -1.1(5) . . . . ? C58 C53 C54 C55 0.7(4) . . . . ? P2 C53 C54 C55 177.73(18) . . . . ? C58 C53 C54 C32 -176.7(2) . . . . ? P2 C53 C54 C32 0.3(3) . . . . ? C47 C32 C54 C55 5.6(3) . . . . ? C31 C32 C54 C55 -119.5(2) . . . . ? C33 C32 C54 C55 127.0(2) . . . . ? C47 C32 C54 C53 -177.2(2) . . . . ? C31 C32 C54 C53 57.8(3) . . . . ? C33 C32 C54 C53 -55.8(3) . . . . ? C53 C54 C55 C56 -0.3(3) . . . . ? C32 C54 C55 C56 176.9(2) . . . . ? C54 C55 C56 C57 0.0(4) . . . . ? C55 C56 C57 C58 0.0(4) . . . . ? C54 C53 C58 C57 -0.7(4) . . . . ? P2 C53 C58 C57 -177.44(19) . . . . ? C56 C57 C58 C53 0.4(4) . . . . ? C29 C24 P1 C1 127.4(2) . . . . ? C25 C24 P1 C1 -48.7(2) . . . . ? C29 C24 P1 C5 -133.4(2) . . . . ? C25 C24 P1 C5 50.4(2) . . . . ? C29 C24 P1 Se1 -3.1(2) . . . . ? C25 C24 P1 Se1 -179.19(15) . . . . ? C2 C1 P1 C24 50.69(19) . . . . ? C12 C1 P1 C24 -124.3(2) . . . . ? C2 C1 P1 C5 -48.9(2) . . . . ? C12 C1 P1 C5 136.0(2) . . . . ? C2 C1 P1 Se1 178.05(14) . . . . ? C12 C1 P1 Se1 3.0(2) . . . . ? C4 C5 P1 C24 -48.5(2) . . . . ? C6 C5 P1 C24 133.5(2) . . . . ? C4 C5 P1 C1 50.2(2) . . . . ? C6 C5 P1 C1 -127.7(2) . . . . ? C4 C5 P1 Se1 -176.32(16) . . . . ? C6 C5 P1 Se1 5.7(2) . . . . ? C58 C53 P2 C34 -133.8(2) . . . . ? C54 C53 P2 C34 49.24(19) . . . . ? C58 C53 P2 C30 125.9(2) . . . . ? C54 C53 P2 C30 -51.01(19) . . . . ? C58 C53 P2 Se2 -2.1(2) . . . . ? C54 C53 P2 Se2 -179.07(14) . . . . ? C33 C34 P2 C53 -49.7(2) . . . . ? C35 C34 P2 C53 130.4(2) . . . . ? C33 C34 P2 C30 47.9(2) . . . . ? C35 C34 P2 C30 -132.0(2) . . . . ? C33 C34 P2 Se2 -178.78(15) . . . . ? C35 C34 P2 Se2 1.3(2) . . . . ? C31 C30 P2 C53 51.4(2) . . . . ? C41 C30 P2 C53 -119.7(2) . . . . ? C31 C30 P2 C34 -48.5(2) . . . . ? C41 C30 P2 C34 140.5(2) . . . . ? C31 C30 P2 Se2 177.49(15) . . . . ? C41 C30 P2 Se2 6.4(2) . . . . ? _refine_diff_density_max 0.754 _refine_diff_density_min -0.529 _refine_diff_density_rms 0.078 _shelx_res_file ; MR15_a.res created by SHELXL-2014/7 TITL MR15_a.res in P-1 REM Old TITL MR15 in P-1 REM SHELXT solution in P-1 REM R1 0.104, Rweak 0.008, Alpha 0.059, Orientation as input REM Formula found by SHELXT: C58 P2 Se2 CELL 0.71073 9.8524 12.4381 18.8967 87.7967 89.7792 75.5730 ZERR 4.000 0.0002 0.0002 0.0003 0.0007 0.0008 0.0006 LATT 1 SFAC C H P SE UNIT 116 84 4 4 TEMP -173.150 SIZE 0.170 0.290 0.380 L.S. 30 BOND $H acta conf LIST 6 FMAP 2 PLAN 20 WGHT 0.033600 2.279500 FVAR 0.35375 C1 1 0.690180 0.435816 0.236675 11.00000 0.00843 0.01387 = 0.01469 -0.00222 0.00266 -0.00041 C2 1 0.685347 0.536966 0.209567 11.00000 0.00813 0.01503 = 0.01744 -0.00213 0.00230 -0.00079 AFIX 43 H2 2 0.720896 0.586999 0.236460 11.00000 -1.20000 AFIX 0 C3 1 0.623538 0.574303 0.135800 11.00000 0.01100 0.01426 = 0.01648 -0.00192 0.00037 -0.00148 C4 1 0.473909 0.557678 0.136248 11.00000 0.01043 0.01500 = 0.01590 -0.00067 -0.00109 0.00025 AFIX 43 H4 2 0.397308 0.618078 0.122839 11.00000 -1.20000 AFIX 0 C5 1 0.450430 0.459636 0.155206 11.00000 0.01066 0.01739 = 0.01622 -0.00050 0.00055 -0.00032 C6 1 0.311088 0.436757 0.161902 11.00000 0.00908 0.01965 = 0.01503 0.00353 -0.00169 -0.00204 C7 1 0.202698 0.513650 0.194740 11.00000 0.01472 0.02337 = 0.01486 -0.00156 -0.00121 -0.00274 AFIX 43 H7 2 0.219838 0.579270 0.212857 11.00000 -1.20000 AFIX 0 C8 1 0.070869 0.493857 0.200719 11.00000 0.01021 0.03430 = 0.01953 -0.00002 0.00219 -0.00159 AFIX 43 H8 2 -0.002130 0.545560 0.223379 11.00000 -1.20000 AFIX 0 C9 1 0.045251 0.398888 0.173746 11.00000 0.01041 0.03576 = 0.02184 0.00983 -0.00219 -0.00755 AFIX 43 H9 2 -0.045428 0.385734 0.177939 11.00000 -1.20000 AFIX 0 C10 1 0.151110 0.322746 0.140618 11.00000 0.01861 0.02398 = 0.02157 0.00708 -0.00699 -0.00924 AFIX 43 H10 2 0.132836 0.258120 0.121603 11.00000 -1.20000 AFIX 0 C11 1 0.283762 0.341612 0.135450 11.00000 0.01447 0.02019 = 0.01683 0.00267 -0.00047 -0.00390 AFIX 43 H11 2 0.356771 0.288848 0.113565 11.00000 -1.20000 AFIX 0 C12 1 0.759475 0.391542 0.304971 11.00000 0.01032 0.01736 = 0.01686 0.00267 0.00126 -0.00404 C13 1 0.738252 0.456504 0.364202 11.00000 0.01862 0.01859 = 0.02254 0.00191 0.00107 -0.00520 AFIX 43 H13 2 0.670242 0.525761 0.362427 11.00000 -1.20000 AFIX 0 C14 1 0.815206 0.421438 0.425928 11.00000 0.03307 0.02978 = 0.01649 -0.00056 -0.00089 -0.01370 AFIX 43 H14 2 0.799326 0.466392 0.466133 11.00000 -1.20000 AFIX 0 C15 1 0.915235 0.320764 0.428829 11.00000 0.02665 0.03447 = 0.02065 0.01064 -0.00671 -0.01021 AFIX 43 H15 2 0.969562 0.297336 0.470606 11.00000 -1.20000 AFIX 0 C16 1 0.935569 0.254570 0.370589 11.00000 0.01917 0.02541 = 0.02748 0.00842 0.00044 -0.00048 AFIX 43 H16 2 1.003452 0.185250 0.372646 11.00000 -1.20000 AFIX 0 C17 1 0.857673 0.288715 0.309409 11.00000 0.01668 0.02023 = 0.02101 0.00063 0.00233 -0.00112 AFIX 43 H17 2 0.870996 0.241927 0.270086 11.00000 -1.20000 AFIX 0 C18 1 0.626387 0.691565 0.110608 11.00000 0.01225 0.01400 = 0.01763 0.00048 0.00331 -0.00054 C19 1 0.558338 0.733417 0.047281 11.00000 0.01634 0.01543 = 0.02235 -0.00093 0.00115 0.00121 AFIX 43 H19 2 0.502534 0.692333 0.024793 11.00000 -1.20000 AFIX 0 C20 1 0.569852 0.833410 0.016189 11.00000 0.02437 0.01910 = 0.02129 0.00556 0.00341 0.00367 AFIX 43 H20 2 0.523265 0.859948 -0.027331 11.00000 -1.20000 AFIX 0 C21 1 0.649722 0.894387 0.048981 11.00000 0.03644 0.01338 = 0.03484 0.00486 0.00309 -0.00353 AFIX 43 H21 2 0.658853 0.962772 0.027870 11.00000 -1.20000 AFIX 0 C22 1 0.716200 0.855350 0.112623 11.00000 0.03419 0.02048 = 0.03769 0.00168 -0.00210 -0.01358 AFIX 43 H22 2 0.769460 0.897827 0.135713 11.00000 -1.20000 AFIX 0 C23 1 0.705346 0.753872 0.143027 11.00000 0.02279 0.01969 = 0.02490 0.00591 -0.00218 -0.00774 AFIX 43 H23 2 0.752531 0.727195 0.186379 11.00000 -1.20000 AFIX 0 C24 1 0.712595 0.377780 0.097775 11.00000 0.00910 0.01807 = 0.01670 0.00059 -0.00026 -0.00402 C25 1 0.711593 0.488694 0.084375 11.00000 0.00834 0.01504 = 0.01636 -0.00057 -0.00193 -0.00221 C26 1 0.791360 0.515385 0.029202 11.00000 0.01372 0.01595 = 0.01755 0.00189 -0.00177 -0.00380 AFIX 43 H26 2 0.793313 0.590510 0.019570 11.00000 -1.20000 AFIX 0 C27 1 0.869161 0.431359 -0.012372 11.00000 0.01202 0.02460 = 0.01488 0.00007 0.00064 -0.00343 AFIX 43 H27 2 0.923169 0.450115 -0.050494 11.00000 -1.20000 AFIX 0 C28 1 0.868678 0.322152 0.001071 11.00000 0.01523 0.02212 = 0.01803 -0.00707 0.00078 -0.00252 AFIX 43 H28 2 0.922031 0.265981 -0.027628 11.00000 -1.20000 AFIX 0 C29 1 0.789561 0.293836 0.057040 11.00000 0.01439 0.01402 = 0.01961 -0.00180 -0.00146 -0.00406 AFIX 43 H29 2 0.788547 0.218584 0.066968 11.00000 -1.20000 AFIX 0 C30 1 0.320239 0.005175 0.261889 11.00000 0.01008 0.01405 = 0.01507 -0.00053 0.00048 -0.00230 C31 1 0.323320 0.103694 0.286054 11.00000 0.01018 0.01534 = 0.01322 -0.00065 0.00208 -0.00194 AFIX 43 H31 2 0.279632 0.169665 0.259605 11.00000 -1.20000 AFIX 0 C32 1 0.397124 0.111258 0.356457 11.00000 0.01235 0.01360 = 0.01239 -0.00197 -0.00054 -0.00272 C33 1 0.547419 0.038189 0.351529 11.00000 0.01066 0.01719 = 0.01242 0.00127 -0.00115 -0.00373 AFIX 43 H33 2 0.623903 0.069863 0.360018 11.00000 -1.20000 AFIX 0 C34 1 0.573253 -0.068597 0.335633 11.00000 0.01227 0.01708 = 0.01294 -0.00123 -0.00148 -0.00432 C35 1 0.716415 -0.142047 0.330352 11.00000 0.01205 0.01437 = 0.01621 -0.00387 -0.00195 -0.00286 C36 1 0.820925 -0.102737 0.295496 11.00000 0.01822 0.01721 = 0.01885 -0.00083 0.00032 -0.00305 AFIX 43 H36 2 0.797793 -0.031874 0.271619 11.00000 -1.20000 AFIX 0 C37 1 0.958188 -0.166544 0.295552 11.00000 0.01637 0.02442 = 0.02790 -0.00474 0.00662 -0.00744 AFIX 43 H37 2 1.028514 -0.139119 0.271738 11.00000 -1.20000 AFIX 0 C38 1 0.993206 -0.269757 0.330044 11.00000 0.01237 0.01992 = 0.03391 -0.00692 0.00180 0.00183 AFIX 43 H38 2 1.087596 -0.312717 0.330647 11.00000 -1.20000 AFIX 0 C39 1 0.890420 -0.310165 0.363621 11.00000 0.01830 0.01589 = 0.03311 0.00178 -0.00302 -0.00040 AFIX 43 H39 2 0.914283 -0.381520 0.386850 11.00000 -1.20000 AFIX 0 C40 1 0.752351 -0.247417 0.363755 11.00000 0.01345 0.01795 = 0.02424 -0.00204 -0.00148 -0.00512 AFIX 43 H40 2 0.682244 -0.276299 0.386636 11.00000 -1.20000 AFIX 0 C41 1 0.236453 -0.012269 0.200818 11.00000 0.01581 0.01308 = 0.01455 -0.00090 -0.00090 -0.00475 C42 1 0.294774 -0.082772 0.147032 11.00000 0.01630 0.02321 = 0.01928 -0.00660 -0.00029 -0.00329 AFIX 43 H42 2 0.391652 -0.119522 0.148348 11.00000 -1.20000 AFIX 0 C43 1 0.211094 -0.099166 0.091591 11.00000 0.02766 0.02969 = 0.02061 -0.01079 0.00033 -0.00927 AFIX 43 H43 2 0.251544 -0.146304 0.054660 11.00000 -1.20000 AFIX 0 C44 1 0.069351 -0.047591 0.089518 11.00000 0.02769 0.02506 = 0.02211 0.00079 -0.01120 -0.01014 AFIX 43 H44 2 0.012466 -0.060816 0.051973 11.00000 -1.20000 AFIX 0 C45 1 0.010755 0.023259 0.142262 11.00000 0.01741 0.01950 = 0.02836 0.00400 -0.00730 -0.00209 AFIX 43 H45 2 -0.086295 0.059468 0.140849 11.00000 -1.20000 AFIX 0 C46 1 0.094194 0.041131 0.197090 11.00000 0.01852 0.01384 = 0.01848 -0.00086 -0.00231 -0.00128 AFIX 43 H46 2 0.053825 0.090688 0.232847 11.00000 -1.20000 AFIX 0 C47 1 0.396784 0.228079 0.377136 11.00000 0.01494 0.01500 = 0.01735 -0.00447 0.00292 -0.00476 C48 1 0.480235 0.239299 0.434416 11.00000 0.01999 0.02194 = 0.03669 -0.01167 -0.00800 0.00119 AFIX 43 H48 2 0.536519 0.174575 0.457772 11.00000 -1.20000 AFIX 0 C49 1 0.482807 0.342481 0.457915 11.00000 0.02402 0.03392 = 0.04259 -0.02074 -0.00407 -0.00804 AFIX 43 H49 2 0.539881 0.348227 0.497298 11.00000 -1.20000 AFIX 0 C50 1 0.403044 0.436611 0.424440 11.00000 0.04973 0.02034 = 0.03115 -0.01587 0.00867 -0.01734 AFIX 43 H50 2 0.406092 0.507793 0.439832 11.00000 -1.20000 AFIX 0 C51 1 0.318819 0.427411 0.368596 11.00000 0.07381 0.01529 = 0.02518 -0.00177 -0.00704 0.00081 AFIX 43 H51 2 0.262875 0.492680 0.345662 11.00000 -1.20000 AFIX 0 C52 1 0.314155 0.323797 0.345051 11.00000 0.04388 0.01608 = 0.02121 -0.00382 -0.00933 0.00062 AFIX 43 H52 2 0.254020 0.318757 0.306808 11.00000 -1.20000 AFIX 0 C53 1 0.318869 -0.056665 0.400906 11.00000 0.01120 0.01942 = 0.01185 0.00060 -0.00273 -0.00157 C54 1 0.319730 0.053577 0.412709 11.00000 0.00928 0.01684 = 0.01434 0.00188 -0.00493 -0.00154 C55 1 0.248806 0.105126 0.470454 11.00000 0.01258 0.02119 = 0.01460 -0.00180 -0.00456 -0.00035 AFIX 43 H55 2 0.248653 0.179807 0.479363 11.00000 -1.20000 AFIX 0 C56 1 0.177425 0.046717 0.515579 11.00000 0.01413 0.03488 = 0.01212 -0.00162 -0.00193 -0.00261 AFIX 43 H56 2 0.128802 0.082114 0.555239 11.00000 -1.20000 AFIX 0 C57 1 0.176692 -0.061592 0.503261 11.00000 0.01309 0.03189 = 0.02057 0.00797 -0.00202 -0.00688 AFIX 43 H57 2 0.127729 -0.100309 0.534393 11.00000 -1.20000 AFIX 0 C58 1 0.247322 -0.114366 0.445464 11.00000 0.01292 0.01882 = 0.02055 0.00479 -0.00536 -0.00361 AFIX 43 H58 2 0.246608 -0.188890 0.436602 11.00000 -1.20000 AFIX 0 P1 3 0.614386 0.354631 0.175723 11.00000 0.00991 0.01245 = 0.01753 0.00097 0.00133 -0.00258 P2 3 0.410423 -0.110410 0.321492 11.00000 0.01077 0.01194 = 0.01671 -0.00123 -0.00115 -0.00205 SE1 4 0.611737 0.189982 0.201258 11.00000 0.01642 0.01334 = 0.02875 0.00303 0.00329 -0.00383 SE2 4 0.413309 -0.273974 0.297563 11.00000 0.01616 0.01199 = 0.02958 -0.00381 -0.00137 -0.00366 HKLF 4 REM MR15_a.res in P-1 REM R1 = 0.0357 for 7511 Fo > 4sig(Fo) and 0.0519 for all 9231 data REM 559 parameters refined using 0 restraints END WGHT 0.0336 2.2795 REM Highest difference peak 0.754, deepest hole -0.529, 1-sigma level 0.078 Q1 1 0.6079 0.2765 0.1894 11.00000 0.05 0.75 Q2 1 0.3982 -0.2799 0.3426 11.00000 0.05 0.73 Q3 1 0.4254 -0.1909 0.3199 11.00000 0.05 0.62 Q4 1 0.4058 -0.1963 0.2902 11.00000 0.05 0.57 Q5 1 0.6464 0.1844 0.2537 11.00000 0.05 0.54 Q6 1 0.6152 0.1132 0.2103 11.00000 0.05 0.50 Q7 1 0.4273 -0.3481 0.3079 11.00000 0.05 0.50 Q8 1 0.3591 -0.0456 0.2949 11.00000 0.05 0.43 Q9 1 0.3780 -0.0919 0.3649 11.00000 0.05 0.43 Q10 1 0.3910 -0.2393 0.2373 11.00000 0.05 0.38 Q11 1 0.6524 0.3947 0.2190 11.00000 0.05 0.37 Q12 1 0.7303 -0.1832 0.3558 11.00000 0.05 0.35 Q13 1 0.4917 -0.0962 0.3233 11.00000 0.05 0.35 Q14 1 0.6150 0.2029 0.1427 11.00000 0.05 0.35 Q15 1 0.3429 0.0864 0.3783 11.00000 0.05 0.34 Q16 1 0.7374 0.4168 0.3358 11.00000 0.05 0.34 Q17 1 0.7150 0.7992 0.1243 11.00000 0.05 0.33 Q18 1 0.6507 0.5546 0.1707 11.00000 0.05 0.33 Q19 1 0.6219 0.6348 0.1256 11.00000 0.05 0.33 Q20 1 0.2865 0.4178 0.1346 11.00000 0.05 0.33 ; _shelx_res_checksum 42387 _shelx_hkl_file ; 1 0 0 4110.99 115.99 -2 0 0 573.74 18.50 -2 0 0 570.34 18.10 -2 0 0 545.35 18.70 -2 0 0 536.45 18.60 -2 0 0 587.54 19.10 -2 0 0 586.24 18.00 2 0 0 579.24 18.10 2 0 0 566.74 18.50 2 0 0 576.14 18.20 2 0 0 516.95 18.50 2 0 0 527.45 18.60 -3 0 0 1110.29 36.10 -3 0 0 1129.19 36.40 -3 0 0 1111.39 35.40 -3 0 0 1068.39 35.80 -3 0 0 1116.19 35.00 -3 0 0 1175.68 35.00 3 0 0 1168.98 35.90 3 0 0 1197.98 35.50 3 0 0 1101.29 36.00 3 0 0 1100.79 36.20 -4 0 0 693.23 25.90 -4 0 0 671.93 25.40 -4 0 0 682.23 24.60 -4 0 0 680.73 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25.50 9 0 0 324.87 23.90 9 0 0 378.16 26.30 -10 0 0 518.35 35.90 -10 0 0 468.65 27.10 -10 0 0 439.16 31.60 -10 0 0 526.95 30.10 -10 0 0 536.95 28.30 -10 0 0 498.85 33.00 10 0 0 477.75 33.40 10 0 0 488.25 34.60 10 0 0 481.35 32.80 10 0 0 482.65 31.50 -11 0 0 157.48 24.00 -11 0 0 187.98 20.70 -11 0 0 186.68 20.00 -11 0 0 141.19 23.10 11 0 0 142.89 22.00 11 0 0 207.88 26.50 11 0 0 189.68 25.80 11 0 0 152.18 23.10 11 -1 0 38.00 18.80 11 -1 0 51.29 19.00 11 -1 0 45.50 19.40 11 -1 0 31.90 20.30 -11 1 0 2.50 20.50 -11 1 0 52.39 20.40 -11 1 0 51.59 15.60 -11 1 0 25.20 13.40 10 -1 0 -13.20 14.40 10 -1 0 8.80 21.60 10 -1 0 -3.60 14.50 10 -1 0 -6.40 12.90 -10 1 0 -4.40 14.20 -10 1 0 4.90 11.80 -10 1 0 -1.30 10.50 -10 1 0 -8.80 10.10 -10 1 0 -2.60 15.40 -10 1 0 -3.80 13.80 9 -1 0 148.69 18.80 9 -1 0 156.28 18.10 9 -1 0 158.48 17.60 9 -1 0 147.39 19.40 -9 1 0 203.28 21.90 -9 1 0 160.58 17.70 -9 1 0 174.58 18.10 -9 1 0 153.78 19.00 -9 1 0 164.18 16.70 -9 1 0 164.38 20.40 8 -1 0 312.77 22.50 8 -1 0 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24.80 6.40 -5 -3 0 15.60 6.10 -5 -3 0 21.90 6.60 -5 -3 0 33.00 3.50 -5 -3 0 17.10 5.50 -5 -3 0 26.20 4.20 5 3 0 20.70 6.00 5 3 0 21.80 5.80 5 3 0 29.90 7.20 5 3 0 16.90 6.40 -6 -3 0 19.40 7.30 -6 -3 0 23.80 7.40 -6 -3 0 22.50 4.30 -6 -3 0 28.10 8.70 -6 -3 0 20.90 6.40 6 3 0 15.90 6.80 6 3 0 23.00 7.30 6 3 0 20.20 7.00 6 3 0 17.00 7.90 -7 -3 0 77.99 11.60 -7 -3 0 74.19 12.50 -7 -3 0 72.19 10.60 -7 -3 0 52.99 11.00 -7 -3 0 74.59 7.60 7 3 0 61.89 11.20 7 3 0 86.59 12.80 7 3 0 66.89 10.80 7 3 0 75.09 10.90 -8 -3 0 105.39 10.50 -8 -3 0 104.69 12.80 -8 -3 0 102.29 14.00 -8 -3 0 105.69 13.20 -8 -3 0 132.79 17.00 -8 -3 0 112.39 14.90 8 3 0 139.89 16.90 8 3 0 142.99 17.20 8 3 0 85.99 13.70 -9 -3 0 366.16 17.60 -9 -3 0 377.46 28.80 -9 -3 0 327.97 24.20 -9 -3 0 356.56 26.40 -9 -3 0 390.26 23.80 9 3 0 355.66 23.70 9 3 0 371.46 27.30 9 3 0 373.46 26.20 -10 -3 0 58.69 14.50 -10 -3 0 73.49 17.80 -10 -3 0 57.49 14.80 -10 -3 0 54.09 17.50 -10 -3 0 79.49 10.50 10 3 0 63.29 18.10 10 3 0 92.09 16.60 -11 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7.80 6.30 6 -4 0 -2.40 5.70 -6 4 0 -0.10 3.60 -6 4 0 -1.80 5.90 -6 4 0 -4.60 7.80 -6 4 0 3.90 3.40 -6 4 0 6.10 7.00 -6 4 0 5.10 8.60 5 -4 0 72.69 8.80 5 -4 0 69.09 8.80 5 -4 0 83.69 9.50 5 -4 0 73.29 8.30 5 -4 0 90.19 12.20 -5 4 0 72.89 5.30 -5 4 0 88.19 12.80 -5 4 0 81.39 11.70 -5 4 0 77.89 5.50 -5 4 0 76.99 9.30 -5 4 0 75.89 9.50 4 -4 0 12.50 4.20 4 -4 0 9.30 4.40 4 -4 0 15.60 6.30 4 -4 0 19.80 4.80 4 -4 0 5.40 4.50 -4 4 0 12.10 1.70 -4 4 0 3.60 6.20 -4 4 0 14.00 4.40 -4 4 0 5.60 4.50 -4 4 0 11.30 1.60 -4 4 0 18.20 7.40 3 -4 0 125.49 7.80 3 -4 0 118.69 10.50 3 -4 0 127.49 7.00 3 -4 0 137.69 7.70 3 -4 0 140.19 14.80 3 -4 0 120.69 7.80 -3 4 0 123.69 7.50 -3 4 0 115.19 8.20 -3 4 0 124.69 10.50 -3 4 0 113.49 10.70 -3 4 0 134.19 11.20 2 -4 0 197.58 14.20 2 -4 0 180.28 7.70 2 -4 0 165.18 6.80 2 -4 0 170.68 6.50 2 -4 0 175.18 7.40 2 -4 0 192.78 11.60 -2 4 0 163.98 11.40 -2 4 0 161.18 7.70 -2 4 0 165.08 7.30 -2 4 0 182.58 11.70 -2 4 0 178.48 12.00 1 -4 0 26.00 4.80 1 -4 0 38.50 6.90 1 -4 0 20.50 4.20 1 -4 0 26.20 1.80 1 -4 0 29.40 2.00 -1 4 0 31.40 5.30 -1 4 0 29.60 5.80 -1 4 0 26.60 1.80 -1 4 0 32.10 6.10 -1 4 0 25.70 2.10 -1 4 0 22.20 5.10 0 -4 0 95.19 6.90 0 -4 0 114.09 8.80 0 -4 0 100.29 3.70 0 -4 0 104.29 3.50 0 -4 0 84.99 7.50 0 4 0 97.89 3.50 0 4 0 113.29 8.90 0 4 0 95.79 8.50 0 4 0 97.29 7.30 0 4 0 98.59 3.70 -1 -4 0 2.70 1.50 -1 -4 0 4.70 2.00 -1 -4 0 4.20 3.00 -1 -4 0 1.30 1.40 -1 -4 0 2.10 1.80 1 4 0 2.00 1.80 1 4 0 5.20 2.90 1 4 0 -0.20 3.40 1 4 0 1.80 1.70 1 4 0 4.00 3.30 1 4 0 4.70 4.00 -2 -4 0 222.88 12.70 -2 -4 0 255.77 9.30 -2 -4 0 228.68 10.50 -2 -4 0 229.78 11.60 -2 -4 0 248.08 10.20 -2 -4 0 224.48 9.60 -2 -4 0 219.68 10.50 2 4 0 228.28 9.00 2 4 0 226.38 9.20 2 4 0 228.08 10.70 2 4 0 245.88 8.70 2 4 0 238.78 12.10 2 4 0 229.38 12.00 -3 -4 0 1.80 3.40 -3 -4 0 7.10 5.20 -3 -4 0 0.70 3.00 -3 -4 0 -1.10 3.00 -3 -4 0 -0.30 3.20 -3 -4 0 0.30 3.30 3 4 0 -1.50 2.70 3 4 0 1.00 3.40 3 4 0 -0.80 3.30 3 4 0 -3.80 3.20 3 4 0 -3.10 3.40 3 4 0 0.20 2.60 -4 -4 0 11.10 4.80 -4 -4 0 4.40 4.70 -4 -4 0 5.20 4.70 -4 -4 0 4.30 4.00 -4 -4 0 8.20 4.30 4 4 0 8.30 4.70 4 4 0 4.10 4.20 4 4 0 4.20 4.60 4 4 0 2.20 4.10 4 4 0 5.10 4.10 4 4 0 8.80 4.10 -5 -4 0 378.86 20.00 -5 -4 0 387.76 16.20 -5 -4 0 406.96 18.60 -5 -4 0 397.76 19.20 -5 -4 0 379.76 19.70 5 4 0 392.16 18.60 5 4 0 391.86 20.10 5 4 0 391.26 18.90 5 4 0 386.36 18.10 5 4 0 399.76 20.10 -6 -4 0 65.79 12.20 -6 -4 0 64.79 9.50 -6 -4 0 58.59 9.70 -6 -4 0 62.39 10.50 -6 -4 0 70.89 7.70 6 4 0 79.09 9.70 6 4 0 56.49 9.80 6 4 0 48.50 9.70 6 4 0 67.69 9.70 6 4 0 58.79 9.30 -7 -4 0 100.19 6.50 -7 -4 0 84.29 12.60 -7 -4 0 97.29 12.10 -7 -4 0 87.39 12.90 -7 -4 0 71.09 11.10 7 4 0 75.19 11.50 7 4 0 94.39 13.30 7 4 0 89.69 11.40 7 4 0 77.69 11.20 7 4 0 84.29 12.40 -8 -4 0 37.50 9.90 -8 -4 0 37.80 12.50 -8 -4 0 47.70 5.80 -8 -4 0 33.10 11.40 8 4 0 31.60 11.30 8 4 0 42.40 10.10 8 4 0 41.40 11.50 8 4 0 43.20 10.60 -9 -4 0 -11.90 12.10 -9 -4 0 -3.00 9.30 -9 -4 0 -14.50 9.30 -9 -4 0 7.20 11.60 -9 -4 0 12.90 11.70 9 4 0 23.50 12.00 9 4 0 3.80 10.20 9 4 0 0.60 9.30 -10 -4 0 184.78 22.30 -10 -4 0 154.08 19.50 -10 -4 0 197.18 23.10 -10 -4 0 143.69 21.80 10 4 0 172.18 21.50 10 4 0 154.68 18.90 10 4 0 130.99 18.10 10 4 0 147.89 21.30 -11 -4 0 91.89 22.20 -11 -4 0 88.49 18.80 -11 -4 0 100.39 18.10 -11 -4 0 48.10 21.30 -11 -4 0 82.69 17.10 11 4 0 105.49 18.90 11 4 0 99.59 19.80 11 4 0 81.79 21.50 11 4 0 120.39 23.70 11 4 0 73.99 19.30 -12 -4 0 23.70 20.80 -12 -4 0 53.79 24.50 -12 -4 0 37.60 24.10 -12 -4 0 53.79 20.40 12 4 0 40.10 18.50 12 4 0 23.10 19.50 12 4 0 51.19 22.60 12 4 0 25.70 26.40 10 -5 0 40.70 17.80 10 -5 0 15.10 18.10 10 -5 0 37.50 17.70 10 -5 0 47.70 20.90 -10 5 0 21.90 15.50 -10 5 0 -18.50 23.80 9 -5 0 10.80 13.00 9 -5 0 27.30 12.90 9 -5 0 34.10 22.70 9 -5 0 -14.20 13.40 -9 5 0 18.80 13.60 -9 5 0 18.70 14.40 -9 5 0 4.80 4.30 -9 5 0 -17.50 17.90 -9 5 0 -2.70 4.00 8 -5 0 59.89 12.90 8 -5 0 52.39 12.60 8 -5 0 59.59 12.80 8 -5 0 43.80 12.20 -8 5 0 63.29 14.80 -8 5 0 57.29 18.00 7 -5 0 194.38 17.20 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226.38 26.10 11 6 0 210.08 24.30 11 6 0 258.67 30.00 -12 -6 0 204.48 27.10 -12 -6 0 235.58 33.80 -12 -6 0 234.78 33.80 -12 -6 0 201.88 25.00 12 6 0 254.97 29.10 12 6 0 223.18 33.40 12 6 0 258.17 32.40 12 6 0 174.58 25.80 9 -7 0 27.10 13.80 9 -7 0 0.30 14.40 9 -7 0 4.40 15.30 9 -7 0 -0.40 16.50 -9 7 0 1.90 14.30 -9 7 0 34.00 25.50 8 -7 0 -4.50 10.50 8 -7 0 5.30 10.80 8 -7 0 9.90 11.40 8 -7 0 8.90 12.60 -8 7 0 17.70 14.10 -8 7 0 -20.20 10.70 -8 7 0 -16.90 18.80 -8 7 0 24.40 11.10 7 -7 0 184.68 18.50 7 -7 0 187.58 17.30 7 -7 0 178.28 20.50 7 -7 0 165.48 16.90 -7 7 0 236.08 27.40 6 -7 0 106.79 12.90 6 -7 0 108.59 11.90 6 -7 0 102.79 12.50 6 -7 0 126.79 13.00 6 -7 0 115.99 17.30 -6 7 0 107.49 18.90 -6 7 0 94.29 17.00 -6 7 0 103.79 12.60 -6 7 0 112.89 12.20 5 -7 0 56.19 7.60 5 -7 0 44.60 8.40 5 -7 0 73.39 8.60 5 -7 0 58.09 9.40 5 -7 0 82.89 13.70 -5 7 0 41.10 13.40 -5 7 0 55.29 7.40 -5 7 0 53.09 8.20 -5 7 0 43.80 12.80 4 -7 0 -0.70 4.00 4 -7 0 4.10 3.80 4 -7 0 -1.50 4.60 4 -7 0 2.60 7.60 4 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15.70 8 7 0 61.79 12.40 -9 -7 0 404.46 31.60 -9 -7 0 471.25 29.60 -9 -7 0 427.96 28.90 -9 -7 0 468.85 31.00 9 7 0 478.05 31.90 9 7 0 407.76 29.80 9 7 0 415.36 27.10 9 7 0 462.25 29.50 9 7 0 447.06 31.60 -10 -7 0 224.78 27.70 -10 -7 0 240.58 27.00 -10 -7 0 224.88 24.20 10 7 0 229.08 26.70 10 7 0 210.88 22.30 10 7 0 238.48 28.10 10 7 0 187.68 24.00 -11 -7 0 -15.30 16.80 -11 -7 0 -3.40 16.20 -11 -7 0 -16.00 19.40 -11 -7 0 5.10 14.30 -11 -7 0 20.30 20.50 11 7 0 -13.90 21.10 11 7 0 3.50 17.80 11 7 0 -8.50 16.30 11 7 0 -17.90 17.70 11 7 0 -4.10 19.80 -12 -7 0 17.70 18.80 -12 -7 0 -25.60 23.80 -12 -7 0 -10.50 25.50 12 7 0 23.10 27.20 12 7 0 -4.60 24.30 12 7 0 5.50 20.60 12 7 0 36.40 21.60 8 -8 0 17.20 11.10 8 -8 0 18.10 13.20 8 -8 0 3.00 11.60 8 -8 0 1.30 14.20 -8 8 0 -4.20 22.10 -8 8 0 10.70 14.90 -8 8 0 -2.70 12.00 -8 8 0 7.90 11.40 7 -8 0 -4.90 8.50 7 -8 0 -5.10 9.90 7 -8 0 8.70 8.50 -7 8 0 -0.60 13.30 -7 8 0 -6.40 9.10 -7 8 0 19.90 19.00 -7 8 0 16.50 8.90 6 -8 0 19.30 7.00 6 -8 0 9.60 7.90 6 -8 0 10.90 9.40 6 -8 0 8.40 7.00 6 -8 0 35.80 14.20 -6 8 0 31.30 12.60 -6 8 0 26.00 16.30 -6 8 0 19.90 7.80 5 -8 0 2.30 5.80 5 -8 0 0.20 5.00 5 -8 0 -4.90 4.50 5 -8 0 -13.50 5.80 5 -8 0 -12.60 10.00 -5 8 0 2.00 4.90 -5 8 0 17.70 12.20 -5 8 0 4.30 5.70 -5 8 0 9.40 13.20 4 -8 0 580.74 21.80 4 -8 0 627.44 31.30 4 -8 0 570.04 20.00 4 -8 0 637.64 30.70 4 -8 0 596.24 19.90 4 -8 0 603.44 22.90 -4 8 0 620.14 20.60 -4 8 0 579.04 33.00 -4 8 0 600.54 32.30 3 -8 0 29.40 4.80 3 -8 0 42.00 19.50 3 -8 0 22.00 3.90 -3 8 0 23.30 10.00 -3 8 0 17.40 10.60 2 -8 0 6.70 7.30 2 -8 0 0.10 7.70 2 -8 0 5.20 1.70 2 -8 0 10.40 2.40 -2 8 0 3.10 8.00 -2 8 0 6.00 9.10 -2 8 0 11.20 9.00 1 -8 0 -1.60 6.90 1 -8 0 -0.20 6.50 -1 8 0 4.00 7.80 -1 8 0 -2.00 7.10 0 -8 0 76.29 10.70 0 -8 0 83.39 10.60 0 8 0 71.79 12.60 0 8 0 70.19 12.40 0 8 0 83.59 11.20 -1 -8 0 35.40 4.20 -1 -8 0 49.50 4.10 -1 -8 0 36.10 4.40 -1 -8 0 40.80 9.60 -1 -8 0 37.30 4.40 -1 -8 0 50.79 8.30 1 8 0 25.50 6.80 1 8 0 38.90 4.50 1 8 0 50.19 11.70 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149.49 13.50 -11 -5 4 161.78 24.30 -11 -5 4 127.89 19.60 -11 -5 4 127.49 22.60 10 5 -4 27.70 15.80 10 5 -4 52.29 18.00 10 5 -4 1.10 16.20 10 5 -4 24.90 14.60 -10 -5 4 39.10 15.40 -10 -5 4 12.50 18.40 -10 -5 4 40.80 16.30 -10 -5 4 40.20 18.10 9 5 -4 21.00 11.90 9 5 -4 42.50 15.30 9 5 -4 45.10 14.50 -9 -5 4 34.80 8.40 -9 -5 4 40.10 14.60 -9 -5 4 19.00 12.60 -9 -5 4 26.70 12.30 8 5 -4 156.78 17.70 8 5 -4 181.48 18.70 8 5 -4 175.88 19.70 8 5 -4 187.68 31.70 8 5 -4 153.48 12.20 -8 -5 4 154.38 19.20 -8 -5 4 170.38 16.60 -8 -5 4 153.68 18.90 -8 -5 4 166.18 19.20 -8 -5 4 173.58 12.30 7 5 -4 156.68 18.00 7 5 -4 121.79 16.60 7 5 -4 164.88 12.40 7 5 -4 121.99 15.20 7 5 -4 116.39 15.10 -7 -5 4 142.89 15.00 -7 -5 4 139.29 15.70 -7 -5 4 142.39 16.80 -7 -5 4 147.39 17.00 6 5 -4 232.48 17.40 6 5 -4 233.78 16.50 6 5 -4 219.88 14.30 6 5 -4 219.88 17.50 6 5 -4 235.68 15.80 6 5 -4 240.78 16.40 -6 -5 4 234.88 16.90 -6 -5 4 216.78 16.20 -6 -5 4 211.58 15.30 -6 -5 4 226.88 18.40 5 5 -4 391.16 18.80 5 5 -4 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48.10 14.00 9 -4 4 50.89 13.10 -10 4 -4 -3.80 15.80 -10 4 -4 -1.10 7.00 -10 4 -4 7.00 13.80 -10 4 -4 -2.00 8.00 -10 4 -4 47.00 22.50 10 -4 4 -1.00 18.80 10 -4 4 -9.80 16.90 10 -4 4 6.30 15.70 10 -4 4 -4.00 13.80 12 3 -4 177.28 30.00 12 3 -4 210.68 34.10 12 3 -4 120.49 32.70 -12 -3 4 120.49 25.20 -12 -3 4 195.08 32.00 -12 -3 4 181.58 26.90 -12 -3 4 216.18 23.60 11 3 -4 95.09 23.60 11 3 -4 80.79 19.40 11 3 -4 109.79 22.00 11 3 -4 113.09 21.60 -11 -3 4 95.49 20.60 -11 -3 4 116.79 22.80 -11 -3 4 109.59 15.70 -11 -3 4 105.19 21.50 -11 -3 4 131.79 19.90 10 3 -4 3.10 15.50 10 3 -4 -5.10 13.30 -10 -3 4 25.90 15.60 -10 -3 4 6.90 10.60 -10 -3 4 -10.00 11.60 -10 -3 4 22.70 15.20 -10 -3 4 14.40 16.90 -10 -3 4 3.10 14.30 9 3 -4 3.50 12.00 9 3 -4 10.70 11.10 9 3 -4 7.20 12.50 -9 -3 4 -3.10 8.10 -9 -3 4 -17.90 10.10 -9 -3 4 4.20 13.10 -9 -3 4 9.60 11.90 -9 -3 4 3.80 9.60 8 3 -4 15.40 10.10 8 3 -4 4.90 9.00 8 3 -4 16.50 10.20 -8 -3 4 0.90 8.60 -8 -3 4 17.30 10.10 -8 -3 4 -9.80 10.80 -8 -3 4 -3.90 6.70 -8 -3 4 0.30 7.90 7 3 -4 414.56 34.50 7 3 -4 379.86 18.50 7 3 -4 437.96 23.20 7 3 -4 448.26 25.40 7 3 -4 448.76 24.80 -7 -3 4 450.95 24.10 -7 -3 4 450.55 19.60 -7 -3 4 459.25 24.70 -7 -3 4 487.85 26.70 6 3 -4 166.68 10.00 6 3 -4 183.48 15.60 6 3 -4 175.18 16.20 6 3 -4 181.68 14.40 6 3 -4 184.28 14.20 -6 -3 4 174.58 14.90 -6 -3 4 201.18 11.30 -6 -3 4 185.88 13.00 -6 -3 4 184.48 14.70 -6 -3 4 186.48 16.80 5 3 -4 70.89 9.60 5 3 -4 95.19 7.90 5 3 -4 102.79 10.30 5 3 -4 91.39 10.40 5 3 -4 66.89 9.20 -5 -3 4 89.29 8.90 -5 -3 4 101.59 10.60 -5 -3 4 91.49 10.50 -5 -3 4 94.49 11.00 4 3 -4 335.37 14.40 4 3 -4 305.37 15.10 4 3 -4 341.47 16.90 4 3 -4 324.37 16.00 4 3 -4 340.77 15.30 -4 -3 4 343.17 17.20 -4 -3 4 330.27 15.10 -4 -3 4 315.27 15.70 -4 -3 4 310.97 15.60 3 3 -4 62.49 6.60 3 3 -4 61.29 6.30 3 3 -4 61.99 6.90 3 3 -4 67.99 7.10 3 3 -4 66.09 6.70 -3 -3 4 61.49 7.00 -3 -3 4 51.69 6.50 -3 -3 4 65.69 6.80 -3 -3 4 58.19 6.10 2 3 -4 444.96 15.80 2 3 -4 435.46 16.60 2 3 -4 443.26 17.00 2 3 -4 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7.60 7 -3 4 5.50 7.80 7 -3 4 3.90 7.60 7 -3 4 2.80 8.50 7 -3 4 14.10 9.80 -8 3 -4 53.99 7.90 -8 3 -4 37.20 11.70 -8 3 -4 48.60 12.40 -8 3 -4 20.00 13.80 -8 3 -4 35.40 8.20 8 -3 4 38.50 10.70 8 -3 4 58.79 12.00 8 -3 4 30.40 12.00 8 -3 4 41.30 12.50 -9 3 -4 4.90 12.40 -9 3 -4 16.90 16.60 -9 3 -4 12.50 11.00 -9 3 -4 0.50 12.60 -9 3 -4 9.60 7.30 -9 3 -4 -7.80 8.30 9 -3 4 -9.10 13.60 9 -3 4 8.60 11.60 9 -3 4 2.50 13.40 9 -3 4 -11.60 10.90 -10 3 -4 -7.80 15.90 -10 3 -4 -1.60 10.70 -10 3 -4 -2.50 8.10 -10 3 -4 -7.10 20.20 -10 3 -4 -2.30 12.80 -10 3 -4 -1.40 15.20 10 -3 4 18.00 16.50 10 -3 4 25.00 16.70 10 -3 4 -5.60 14.40 10 -3 4 5.70 13.70 12 2 -4 23.60 25.20 12 2 -4 21.10 24.10 -12 -2 4 5.50 24.70 -12 -2 4 27.70 21.20 -12 -2 4 34.50 15.70 -12 -2 4 26.20 24.80 11 2 -4 23.70 17.20 11 2 -4 -12.80 17.80 11 2 -4 10.50 22.40 11 2 -4 -15.30 20.00 -11 -2 4 -18.20 20.00 -11 -2 4 -6.40 11.80 -11 -2 4 -1.20 15.60 -11 -2 4 15.00 14.50 -11 -2 4 17.80 18.10 -11 -2 4 22.20 18.50 10 2 -4 146.89 21.00 10 2 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28.20 -10 -2 10 206.38 25.30 -10 -2 10 195.18 25.10 9 2 -10 12.90 15.10 9 2 -10 20.90 18.40 9 2 -10 9.10 14.30 9 2 -10 10.20 8.70 -9 -2 10 30.10 14.80 -9 -2 10 34.80 18.20 -9 -2 10 9.30 11.30 -9 -2 10 2.40 11.30 -9 -2 10 10.70 15.20 8 2 -10 16.60 13.00 8 2 -10 37.50 12.60 8 2 -10 14.30 13.90 -8 -2 10 21.20 16.10 -8 -2 10 33.60 13.60 -8 -2 10 19.60 12.90 7 2 -10 918.31 39.40 7 2 -10 888.81 39.60 7 2 -10 955.30 42.60 -7 -2 10 827.32 38.90 -7 -2 10 979.10 56.49 -7 -2 10 860.51 41.60 -7 -2 10 918.51 36.10 6 2 -10 1040.20 40.60 6 2 -10 955.00 39.30 6 2 -10 972.30 42.10 6 2 -10 980.20 38.50 -6 -2 10 998.70 37.20 -6 -2 10 968.40 41.10 -6 -2 10 1000.50 42.60 -6 -2 10 959.40 39.50 5 2 -10 597.24 28.50 5 2 -10 590.04 26.30 5 2 -10 583.24 27.10 5 2 -10 644.34 28.20 -5 -2 10 583.84 25.70 -5 -2 10 537.15 28.90 -5 -2 10 618.34 26.90 -5 -2 10 579.84 28.80 4 2 -10 80.99 10.10 4 2 -10 106.69 11.90 4 2 -10 75.89 10.20 -4 -2 10 87.59 11.90 -4 -2 10 83.79 10.50 -4 -2 10 73.09 10.20 -4 -2 10 106.29 9.80 3 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'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 38129 #============================================================================== _publ_requested_journal '??????' _publ_contact_author ; Prof. Dr.Christian M\"uller Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_contact_letter ; ; _publ_requested_coeditor_name ? _publ_contact_author_phone '+49/(0)3083854004' _publ_contact_author_fax '+49/(0)3083852440' _publ_contact_author_email c.mueller@fu-berlin.de loop_ _publ_author_name _publ_author_address 'M\"uller, Christian' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Rigo, Massimo' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Weber, Manuela' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; 'Wiecko, Jelena' ; Freie Universit\"at Berlin Institut f\"ur Chemie und Biochemie Anorganische Chemie Fabeckstr. 34-36 14195 Berlin Germany ; _publ_section_title ; ... see the published paper. ; _publ_section_abstract ; ... and following paragraphs: see the published paper. ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; #END====================================================