data_MR335_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 'C27 H29 F6 P Si2' _chemical_formula_weight 554.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.2955 0.4335 '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 10.78717(8) _cell_length_b 15.23382(10) _cell_length_c 18.26277(13) _cell_angle_alpha 97.4263(3) _cell_angle_beta 103.9082(3) _cell_angle_gamma 99.6371(3) _cell_volume 2826.62(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9866 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 66.80 _exptl_crystal_description 'block' _exptl_crystal_colour 'colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_F_000 1152 _exptl_transmission_factor_min 0.6008 _exptl_transmission_factor_max 0.7046 _exptl_crystal_size_max 0.280 _exptl_crystal_size_mid 0.280 _exptl_crystal_size_min 0.140 _exptl_absorpt_coefficient_mu 2.159 _shelx_estimated_absorpt_T_min 0.583 _shelx_estimated_absorpt_T_max 0.752 _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 1.54178 _diffrn_radiation_type CuK\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 29818 _diffrn_reflns_av_unetI/netI 0.0355 _diffrn_reflns_av_R_equivalents 0.0347 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.532 _diffrn_reflns_theta_max 66.837 _diffrn_reflns_theta_full 66.837 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.994 _reflns_number_total 9977 _reflns_number_gt 8562 _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^)+(0.0325P)^2^+1.9471P] 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 9977 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0841 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _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 1.15345(18) 0.29210(12) 0.29907(11) 0.0170(4) Uani 1 1 d . . . . . C2 C 1.07713(18) 0.33329(12) 0.33388(10) 0.0163(4) Uani 1 1 d . . . . . C3 C 0.93268(18) 0.28541(12) 0.31686(11) 0.0170(4) Uani 1 1 d . . . . . H3 H 0.8834 0.3238 0.3427 0.020 Uiso 1 1 calc R U . . . C4 C 0.93474(17) 0.19629(12) 0.34850(10) 0.0151(4) Uani 1 1 d . . . . . C5 C 0.99441(18) 0.13677(12) 0.31767(11) 0.0167(4) Uani 1 1 d . . . . . C6 C 0.87752(18) 0.18945(12) 0.41468(11) 0.0153(4) Uani 1 1 d . . . . . C7 C 0.74284(19) 0.17264(13) 0.40409(11) 0.0198(4) Uani 1 1 d . . . . . H7 H 0.6863 0.1641 0.3539 0.024 Uiso 1 1 calc R U . . . C8 C 0.69046(19) 0.16823(13) 0.46627(11) 0.0218(4) Uani 1 1 d . . . . . H8 H 0.5985 0.1554 0.4583 0.026 Uiso 1 1 calc R U . . . C9 C 0.7717(2) 0.18247(13) 0.53974(11) 0.0210(4) Uani 1 1 d . . . . . H9 H 0.7357 0.1802 0.5823 0.025 Uiso 1 1 calc R U . . . C10 C 0.9060(2) 0.20012(13) 0.55112(11) 0.0207(4) Uani 1 1 d . . . . . H10 H 0.9620 0.2100 0.6016 0.025 Uiso 1 1 calc R U . . . C11 C 0.95877(19) 0.20331(12) 0.48895(11) 0.0182(4) Uani 1 1 d . . . . . H11 H 1.0508 0.2150 0.4971 0.022 Uiso 1 1 calc R U . . . C12 C 1.1187(2) 0.41730(12) 0.39232(11) 0.0201(4) Uani 1 1 d . . . . . C13 C 1.0444(2) 0.48443(14) 0.38964(14) 0.0307(5) Uani 1 1 d . . . . . H13 H 0.9656 0.4763 0.3503 0.037 Uiso 1 1 calc R U . . . C14 C 1.0855(3) 0.56268(15) 0.44427(15) 0.0415(6) Uani 1 1 d . . . . . H14 H 1.0351 0.6083 0.4417 0.050 Uiso 1 1 calc R U . . . C15 C 1.1982(3) 0.57500(15) 0.50205(15) 0.0437(7) Uani 1 1 d . . . . . H15 H 1.2265 0.6295 0.5386 0.052 Uiso 1 1 calc R U . . . C16 C 1.2709(3) 0.50800(16) 0.50716(13) 0.0376(6) Uani 1 1 d . . . . . H16 H 1.3479 0.5159 0.5478 0.045 Uiso 1 1 calc R U . . . C17 C 1.2303(2) 0.42909(14) 0.45250(12) 0.0270(5) Uani 1 1 d . . . . . H17 H 1.2795 0.3828 0.4564 0.032 Uiso 1 1 calc R U . . . C18 C 0.92794(19) 0.21344(13) 0.18886(11) 0.0213(4) Uani 1 1 d . . . . . C19 C 0.87115(19) 0.26299(13) 0.23082(11) 0.0207(4) Uani 1 1 d . . . . . C20 C 0.8879(2) 0.18681(17) 0.10286(13) 0.0339(5) Uani 1 1 d . . . . . C21 C 0.7541(2) 0.30337(15) 0.20433(13) 0.0298(5) Uani 1 1 d . . . . . C22 C 1.3785(2) 0.45715(14) 0.31078(13) 0.0283(5) Uani 1 1 d . . . . . H22A H 1.4645 0.4732 0.3015 0.042 Uiso 1 1 calc R U . . . H22B H 1.3834 0.4820 0.3639 0.042 Uiso 1 1 calc R U . . . H22C H 1.3152 0.4822 0.2759 0.042 Uiso 1 1 calc R U . . . C23 C 1.3302(2) 0.28533(15) 0.19470(12) 0.0281(5) Uani 1 1 d . . . . . H23A H 1.2631 0.3044 0.1572 0.042 Uiso 1 1 calc R U . . . H23B H 1.3137 0.2191 0.1872 0.042 Uiso 1 1 calc R U . . . H23C H 1.4163 0.3084 0.1878 0.042 Uiso 1 1 calc R U . . . C24 C 1.4392(2) 0.28206(15) 0.36344(13) 0.0288(5) Uani 1 1 d . . . . . H24A H 1.4048 0.2171 0.3577 0.043 Uiso 1 1 calc R U . . . H24B H 1.4471 0.3116 0.4158 0.043 Uiso 1 1 calc R U . . . H24C H 1.5253 0.2916 0.3534 0.043 Uiso 1 1 calc R U . . . C25 C 1.0414(2) -0.04805(14) 0.26231(12) 0.0284(5) Uani 1 1 d . . . . . H25A H 0.9651 -0.0544 0.2187 0.043 Uiso 1 1 calc R U . . . H25B H 1.0494 -0.1078 0.2750 0.043 Uiso 1 1 calc R U . . . H25C H 1.1202 -0.0209 0.2489 0.043 Uiso 1 1 calc R U . . . C26 C 1.1779(2) 0.05070(14) 0.42393(13) 0.0317(5) Uani 1 1 d . . . . . H26A H 1.2015 -0.0062 0.4358 0.048 Uiso 1 1 calc R U . . . H26B H 1.1670 0.0860 0.4699 0.048 Uiso 1 1 calc R U . . . H26C H 1.2472 0.0854 0.4067 0.048 Uiso 1 1 calc R U . . . C27 C 0.8808(2) -0.03138(15) 0.37686(16) 0.0368(6) Uani 1 1 d . . . . . H27A H 0.8012 -0.0416 0.3348 0.055 Uiso 1 1 calc R U . . . H27B H 0.8706 0.0069 0.4216 0.055 Uiso 1 1 calc R U . . . H27C H 0.8966 -0.0895 0.3903 0.055 Uiso 1 1 calc R U . . . C28 C 0.47051(18) 0.83459(12) 0.20658(11) 0.0170(4) Uani 1 1 d . . . . . C29 C 0.53841(17) 0.78717(12) 0.17012(10) 0.0158(4) Uani 1 1 d . . . . . C30 C 0.54178(17) 0.68973(12) 0.18455(10) 0.0152(4) Uani 1 1 d . . . . . H30 H 0.5980 0.6619 0.1560 0.018 Uiso 1 1 calc R U . . . C31 C 0.39916(17) 0.63716(12) 0.15571(10) 0.0154(4) Uani 1 1 d . . . . . C32 C 0.31254(18) 0.66527(12) 0.18987(10) 0.0159(4) Uani 1 1 d . . . . . C33 C 0.36999(17) 0.56287(12) 0.08877(11) 0.0171(4) Uani 1 1 d . . . . . C34 C 0.4089(2) 0.48148(14) 0.09665(12) 0.0253(4) Uani 1 1 d . . . . . H34 H 0.4582 0.4735 0.1451 0.030 Uiso 1 1 calc R U . . . C35 C 0.3762(2) 0.41161(14) 0.03403(13) 0.0306(5) Uani 1 1 d . . . . . H35 H 0.4006 0.3553 0.0400 0.037 Uiso 1 1 calc R U . . . C36 C 0.3080(2) 0.42418(15) -0.03678(13) 0.0303(5) Uani 1 1 d . . . . . H36 H 0.2846 0.3761 -0.0794 0.036 Uiso 1 1 calc R U . . . C37 C 0.2739(2) 0.50601(16) -0.04590(13) 0.0310(5) Uani 1 1 d . . . . . H37 H 0.2300 0.5150 -0.0952 0.037 Uiso 1 1 calc R U . . . C38 C 0.3034(2) 0.57525(14) 0.01669(12) 0.0246(4) Uani 1 1 d . . . . . H38 H 0.2782 0.6312 0.0104 0.030 Uiso 1 1 calc R U . . . C39 C 0.60460(18) 0.81573(12) 0.11184(11) 0.0169(4) Uani 1 1 d . . . . . C40 C 0.73677(19) 0.81636(13) 0.12062(11) 0.0213(4) Uani 1 1 d . . . . . H40 H 0.7856 0.7979 0.1645 0.026 Uiso 1 1 calc R U . . . C41 C 0.7979(2) 0.84355(14) 0.06616(12) 0.0264(5) Uani 1 1 d . . . . . H41 H 0.8884 0.8449 0.0734 0.032 Uiso 1 1 calc R U . . . C42 C 0.7270(2) 0.86870(14) 0.00144(12) 0.0282(5) Uani 1 1 d . . . . . H42 H 0.7687 0.8874 -0.0359 0.034 Uiso 1 1 calc R U . . . C43 C 0.5949(2) 0.86656(15) -0.00890(12) 0.0297(5) Uani 1 1 d . . . . . H43 H 0.5460 0.8830 -0.0538 0.036 Uiso 1 1 calc R U . . . C44 C 0.5337(2) 0.84046(14) 0.04597(12) 0.0243(4) Uani 1 1 d . . . . . H44 H 0.4432 0.8395 0.0386 0.029 Uiso 1 1 calc R U . . . C45 C 0.52634(18) 0.72869(13) 0.31498(11) 0.0179(4) Uani 1 1 d . . . . . C46 C 0.59072(18) 0.69061(12) 0.26980(11) 0.0173(4) Uani 1 1 d . . . . . C47 C 0.5608(2) 0.74357(14) 0.40084(11) 0.0250(4) Uani 1 1 d . . . . . C48 C 0.70780(19) 0.64949(14) 0.29387(12) 0.0232(4) Uani 1 1 d . . . . . C49 C 0.5950(2) 1.02830(14) 0.19023(13) 0.0294(5) Uani 1 1 d . . . . . H49A H 0.5998 1.0078 0.1381 0.044 Uiso 1 1 calc R U . . . H49B H 0.6755 1.0241 0.2271 0.044 Uiso 1 1 calc R U . . . H49C H 0.5844 1.0913 0.1957 0.044 Uiso 1 1 calc R U . . . C50 C 0.4427(2) 0.99831(14) 0.30761(12) 0.0283(5) Uani 1 1 d . . . . . H50A H 0.4364 1.0621 0.3121 0.042 Uiso 1 1 calc R U . . . H50B H 0.5210 0.9922 0.3453 0.042 Uiso 1 1 calc R U . . . H50C H 0.3653 0.9630 0.3171 0.042 Uiso 1 1 calc R U . . . C51 C 0.2975(2) 0.95941(15) 0.13791(13) 0.0296(5) Uani 1 1 d . . . . . H51A H 0.3081 0.9477 0.0859 0.044 Uiso 1 1 calc R U . . . H51B H 0.2766 1.0193 0.1476 0.044 Uiso 1 1 calc R U . . . H51C H 0.2265 0.9132 0.1429 0.044 Uiso 1 1 calc R U . . . C52 C 0.0495(2) 0.68425(18) 0.09797(17) 0.0480(7) Uani 1 1 d . . . . . H52A H 0.0723 0.6720 0.0494 0.072 Uiso 1 1 calc R U . . . H52B H 0.0780 0.7490 0.1193 0.072 Uiso 1 1 calc R U . . . H52C H -0.0452 0.6664 0.0890 0.072 Uiso 1 1 calc R U . . . C53 C 0.0828(2) 0.6380(2) 0.25684(15) 0.0478(7) Uani 1 1 d . . . . . H53A H 0.0926 0.7031 0.2737 0.072 Uiso 1 1 calc R U . . . H53B H 0.1382 0.6133 0.2964 0.072 Uiso 1 1 calc R U . . . H53C H -0.0086 0.6080 0.2481 0.072 Uiso 1 1 calc R U . . . C54 C 0.0889(2) 0.49505(15) 0.12699(15) 0.0359(6) Uani 1 1 d . . . . . H54A H -0.0029 0.4716 0.1238 0.054 Uiso 1 1 calc R U . . . H54B H 0.1442 0.4635 0.1606 0.054 Uiso 1 1 calc R U . . . H54C H 0.1028 0.4851 0.0757 0.054 Uiso 1 1 calc R U . . . F1 F 0.97598(17) 0.15012(16) 0.07736(8) 0.0739(6) Uani 1 1 d . . . . . F2 F 0.87366(18) 0.25735(12) 0.06723(8) 0.0622(5) Uani 1 1 d . . . . . F3 F 0.77508(14) 0.12739(10) 0.07612(7) 0.0465(4) Uani 1 1 d . . . . . F4 F 0.78737(14) 0.39313(9) 0.21307(9) 0.0490(4) Uani 1 1 d . . . . . F5 F 0.68552(16) 0.27326(12) 0.13266(9) 0.0597(5) Uani 1 1 d . . . . . F6 F 0.67004(14) 0.28694(12) 0.24676(10) 0.0572(5) Uani 1 1 d . . . . . F7 F 0.52167(14) 0.81605(11) 0.42908(7) 0.0463(4) Uani 1 1 d . . . . . F8 F 0.5079(2) 0.67430(12) 0.42715(8) 0.0723(6) Uani 1 1 d . . . . . F9 F 0.68862(13) 0.76039(11) 0.43381(8) 0.0479(4) Uani 1 1 d . . . . . F10 F 0.81817(13) 0.70943(10) 0.30514(12) 0.0673(6) Uani 1 1 d . . . . . F11 F 0.71485(16) 0.61362(11) 0.35638(8) 0.0528(4) Uani 1 1 d . . . . . F12 F 0.71052(14) 0.58207(10) 0.24004(8) 0.0444(4) Uani 1 1 d . . . . . Si1 Si 1.32569(5) 0.33143(3) 0.29388(3) 0.01806(12) Uani 1 1 d . . . . . Si2 Si 1.02176(5) 0.02590(3) 0.34645(3) 0.01860(12) Uani 1 1 d . . . . . Si3 Si 0.45277(5) 0.95563(3) 0.20906(3) 0.01971(12) Uani 1 1 d . . . . . Si4 Si 0.13209(5) 0.61839(4) 0.16666(3) 0.01882(12) Uani 1 1 d . . . . . P1 P 1.07250(5) 0.17624(3) 0.24388(3) 0.01753(11) Uani 1 1 d . . . . . P2 P 0.38075(5) 0.76885(3) 0.26446(3) 0.01626(11) 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 0.0187(9) 0.0156(9) 0.0163(9) 0.0045(7) 0.0039(8) 0.0029(7) C2 0.0200(9) 0.0150(9) 0.0151(9) 0.0055(7) 0.0053(8) 0.0037(7) C3 0.0178(9) 0.0168(9) 0.0182(10) 0.0054(8) 0.0060(8) 0.0053(7) C4 0.0144(9) 0.0147(9) 0.0154(9) 0.0038(7) 0.0029(7) 0.0014(7) C5 0.0177(9) 0.0157(9) 0.0166(9) 0.0031(7) 0.0057(8) 0.0016(7) C6 0.0194(9) 0.0098(8) 0.0186(10) 0.0027(7) 0.0071(8) 0.0051(7) C7 0.0197(10) 0.0218(10) 0.0169(10) 0.0025(8) 0.0038(8) 0.0045(8) C8 0.0179(10) 0.0249(10) 0.0246(11) 0.0043(8) 0.0087(8) 0.0053(8) C9 0.0298(11) 0.0190(9) 0.0202(10) 0.0052(8) 0.0137(9) 0.0097(8) C10 0.0265(10) 0.0202(10) 0.0157(10) 0.0025(8) 0.0038(8) 0.0086(8) C11 0.0186(9) 0.0172(9) 0.0194(10) 0.0030(8) 0.0052(8) 0.0054(8) C12 0.0281(10) 0.0139(9) 0.0203(10) 0.0036(8) 0.0121(8) 0.0010(8) C13 0.0416(13) 0.0188(10) 0.0374(13) 0.0064(9) 0.0186(11) 0.0092(9) C14 0.0637(17) 0.0159(11) 0.0527(16) 0.0023(11) 0.0322(14) 0.0087(11) C15 0.0713(19) 0.0185(11) 0.0400(15) -0.0084(10) 0.0319(14) -0.0086(12) C16 0.0472(14) 0.0335(13) 0.0241(12) -0.0043(10) 0.0116(11) -0.0099(11) C17 0.0337(12) 0.0239(11) 0.0225(11) 0.0020(9) 0.0102(9) 0.0013(9) C18 0.0208(10) 0.0242(10) 0.0170(10) 0.0061(8) 0.0041(8) -0.0016(8) C19 0.0180(9) 0.0225(10) 0.0215(10) 0.0111(8) 0.0034(8) 0.0014(8) C20 0.0288(12) 0.0495(14) 0.0197(11) 0.0062(10) 0.0047(9) 0.0002(11) C21 0.0249(11) 0.0358(12) 0.0299(12) 0.0153(10) 0.0033(9) 0.0079(9) C22 0.0279(11) 0.0240(11) 0.0319(12) 0.0077(9) 0.0086(9) -0.0006(9) C23 0.0265(11) 0.0335(12) 0.0254(11) 0.0033(9) 0.0132(9) 0.0018(9) C24 0.0241(11) 0.0329(12) 0.0318(12) 0.0088(10) 0.0069(9) 0.0112(9) C25 0.0360(12) 0.0186(10) 0.0298(12) -0.0016(9) 0.0102(10) 0.0063(9) C26 0.0409(13) 0.0224(11) 0.0286(12) 0.0030(9) 0.0000(10) 0.0123(10) C27 0.0435(14) 0.0226(11) 0.0601(16) 0.0207(11) 0.0318(13) 0.0135(10) C28 0.0165(9) 0.0169(9) 0.0162(9) 0.0014(7) 0.0037(7) 0.0016(7) C29 0.0140(9) 0.0159(9) 0.0157(9) 0.0021(7) 0.0024(7) 0.0004(7) C30 0.0136(9) 0.0159(9) 0.0168(9) 0.0014(7) 0.0056(7) 0.0037(7) C31 0.0147(9) 0.0148(9) 0.0163(9) 0.0038(7) 0.0035(7) 0.0022(7) C32 0.0156(9) 0.0163(9) 0.0157(9) 0.0037(7) 0.0044(7) 0.0022(7) C33 0.0131(9) 0.0178(9) 0.0197(10) 0.0008(8) 0.0072(8) -0.0005(7) C34 0.0293(11) 0.0228(10) 0.0267(11) 0.0051(9) 0.0116(9) 0.0074(9) C35 0.0377(12) 0.0177(10) 0.0414(13) -0.0006(9) 0.0244(11) 0.0038(9) C36 0.0231(11) 0.0320(12) 0.0314(12) -0.0126(10) 0.0162(10) -0.0054(9) C37 0.0246(11) 0.0421(13) 0.0217(11) -0.0035(10) 0.0048(9) 0.0036(10) C38 0.0243(10) 0.0272(11) 0.0217(11) 0.0009(9) 0.0056(9) 0.0069(9) C39 0.0175(9) 0.0146(9) 0.0173(9) 0.0000(7) 0.0056(8) 0.0006(7) C40 0.0214(10) 0.0211(10) 0.0220(10) 0.0058(8) 0.0065(8) 0.0035(8) C41 0.0216(10) 0.0280(11) 0.0316(12) 0.0061(9) 0.0125(9) 0.0019(9) C42 0.0345(12) 0.0290(11) 0.0245(11) 0.0074(9) 0.0166(9) 0.0013(9) C43 0.0336(12) 0.0360(12) 0.0191(11) 0.0091(9) 0.0057(9) 0.0049(10) C44 0.0217(10) 0.0305(11) 0.0212(10) 0.0054(9) 0.0060(8) 0.0055(9) C45 0.0160(9) 0.0188(9) 0.0175(10) 0.0031(8) 0.0040(8) 0.0006(7) C46 0.0145(9) 0.0160(9) 0.0191(10) 0.0032(8) 0.0029(8) -0.0005(7) C47 0.0242(11) 0.0322(11) 0.0172(10) 0.0015(9) 0.0044(8) 0.0057(9) C48 0.0198(10) 0.0261(10) 0.0221(11) 0.0032(9) 0.0023(8) 0.0063(8) C49 0.0335(12) 0.0213(10) 0.0320(12) 0.0044(9) 0.0099(10) 0.0001(9) C50 0.0346(12) 0.0192(10) 0.0309(12) -0.0021(9) 0.0125(10) 0.0044(9) C51 0.0303(12) 0.0295(11) 0.0309(12) 0.0071(10) 0.0069(10) 0.0116(9) C52 0.0195(11) 0.0495(15) 0.074(2) 0.0359(15) -0.0004(12) 0.0033(11) C53 0.0344(13) 0.0613(18) 0.0468(16) -0.0034(13) 0.0274(12) -0.0069(12) C54 0.0189(11) 0.0261(11) 0.0572(16) -0.0033(11) 0.0090(11) -0.0003(9) F1 0.0543(10) 0.1476(19) 0.0209(8) -0.0065(9) 0.0116(7) 0.0377(11) F2 0.0824(12) 0.0668(11) 0.0272(8) 0.0272(8) 0.0012(8) -0.0078(9) F3 0.0468(8) 0.0550(9) 0.0220(7) -0.0005(6) -0.0008(6) -0.0127(7) F4 0.0422(8) 0.0326(7) 0.0736(11) 0.0210(7) 0.0067(8) 0.0160(6) F5 0.0491(9) 0.0758(11) 0.0425(9) 0.0038(8) -0.0185(7) 0.0305(9) F6 0.0287(7) 0.0937(13) 0.0728(11) 0.0518(10) 0.0254(7) 0.0318(8) F7 0.0508(9) 0.0672(10) 0.0207(7) -0.0075(7) 0.0051(6) 0.0305(8) F8 0.1140(15) 0.0600(10) 0.0215(7) 0.0110(7) 0.0129(8) -0.0361(10) F9 0.0316(7) 0.0775(11) 0.0245(7) -0.0084(7) -0.0073(6) 0.0187(7) F10 0.0152(7) 0.0407(9) 0.1375(17) 0.0168(10) 0.0051(8) 0.0039(6) F11 0.0672(10) 0.0769(11) 0.0348(8) 0.0278(8) 0.0175(7) 0.0523(9) F12 0.0486(8) 0.0514(9) 0.0337(8) -0.0047(6) 0.0005(6) 0.0360(7) Si1 0.0167(3) 0.0193(3) 0.0189(3) 0.0049(2) 0.0057(2) 0.0031(2) Si2 0.0233(3) 0.0134(2) 0.0212(3) 0.0031(2) 0.0086(2) 0.0057(2) Si3 0.0226(3) 0.0151(2) 0.0215(3) 0.0018(2) 0.0068(2) 0.0040(2) Si4 0.0136(2) 0.0199(3) 0.0242(3) 0.0053(2) 0.0070(2) 0.0029(2) P1 0.0203(2) 0.0162(2) 0.0171(2) 0.00156(19) 0.00819(19) 0.00310(19) P2 0.0162(2) 0.0177(2) 0.0156(2) 0.00127(19) 0.00628(19) 0.00393(18) _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 1.341(3) . ? C1 P1 1.8693(19) . ? C1 Si1 1.8833(19) . ? C2 C12 1.484(3) . ? C2 C3 1.544(3) . ? C3 C19 1.520(3) . ? C3 C4 1.544(2) . ? C3 H3 1.0000 . ? C4 C5 1.338(3) . ? C4 C6 1.491(3) . ? C5 P1 1.8635(19) . ? C5 Si2 1.8809(19) . ? C6 C7 1.393(3) . ? C6 C11 1.395(3) . ? C7 C8 1.389(3) . ? C7 H7 0.9500 . ? C8 C9 1.382(3) . ? C8 H8 0.9500 . ? C9 C10 1.387(3) . ? C9 H9 0.9500 . ? C10 C11 1.390(3) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C17 1.390(3) . ? C12 C13 1.400(3) . ? C13 C14 1.384(3) . ? C13 H13 0.9500 . ? C14 C15 1.372(4) . ? C14 H14 0.9500 . ? C15 C16 1.387(4) . ? C15 H15 0.9500 . ? C16 C17 1.392(3) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.328(3) . ? C18 C20 1.506(3) . ? C18 P1 1.858(2) . ? C19 C21 1.500(3) . ? C20 F1 1.325(3) . ? C20 F3 1.330(3) . ? C20 F2 1.338(3) . ? C21 F5 1.318(3) . ? C21 F4 1.332(3) . ? C21 F6 1.341(3) . ? C22 Si1 1.867(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 Si1 1.871(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 Si1 1.867(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 Si2 1.861(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 Si2 1.867(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Si2 1.862(2) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.338(3) . ? C28 P2 1.8705(19) . ? C28 Si3 1.8813(19) . ? C29 C39 1.488(3) . ? C29 C30 1.546(2) . ? C30 C46 1.517(3) . ? C30 C31 1.541(2) . ? C30 H30 1.0000 . ? C31 C32 1.338(3) . ? C31 C33 1.487(3) . ? C32 P2 1.8603(19) . ? C32 Si4 1.8810(19) . ? C33 C34 1.388(3) . ? C33 C38 1.393(3) . ? C34 C35 1.389(3) . ? C34 H34 0.9500 . ? C35 C36 1.380(3) . ? C35 H35 0.9500 . ? C36 C37 1.377(3) . ? C36 H36 0.9500 . ? C37 C38 1.386(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C40 1.394(3) . ? C39 C44 1.395(3) . ? C40 C41 1.388(3) . ? C40 H40 0.9500 . ? C41 C42 1.382(3) . ? C41 H41 0.9500 . ? C42 C43 1.385(3) . ? C42 H42 0.9500 . ? C43 C44 1.390(3) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? C45 C46 1.337(3) . ? C45 C47 1.499(3) . ? C45 P2 1.8609(19) . ? C46 C48 1.500(3) . ? C47 F8 1.316(3) . ? C47 F9 1.331(2) . ? C47 F7 1.333(2) . ? C48 F11 1.320(2) . ? C48 F10 1.328(2) . ? C48 F12 1.336(2) . ? C49 Si3 1.866(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 Si3 1.868(2) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 Si3 1.871(2) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 Si4 1.861(2) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 Si4 1.853(2) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 Si4 1.861(2) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? 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 114.02(14) . . ? C2 C1 Si1 131.43(15) . . ? P1 C1 Si1 114.52(10) . . ? C1 C2 C12 126.84(17) . . ? C1 C2 C3 117.39(16) . . ? C12 C2 C3 115.59(16) . . ? C19 C3 C4 108.85(15) . . ? C19 C3 C2 109.97(15) . . ? C4 C3 C2 105.64(14) . . ? C19 C3 H3 110.8 . . ? C4 C3 H3 110.8 . . ? C2 C3 H3 110.8 . . ? C5 C4 C6 127.06(16) . . ? C5 C4 C3 117.44(16) . . ? C6 C4 C3 115.34(15) . . ? C4 C5 P1 114.32(14) . . ? C4 C5 Si2 128.00(14) . . ? P1 C5 Si2 117.39(10) . . ? C7 C6 C11 118.80(17) . . ? C7 C6 C4 120.97(16) . . ? C11 C6 C4 120.18(16) . . ? C8 C7 C6 120.57(18) . . ? C8 C7 H7 119.7 . . ? C6 C7 H7 119.7 . . ? C9 C8 C7 120.24(18) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C8 C9 C10 119.75(18) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C9 C10 C11 120.18(18) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C10 C11 C6 120.44(18) . . ? C10 C11 H11 119.8 . . ? C6 C11 H11 119.8 . . ? C17 C12 C13 118.76(19) . . ? C17 C12 C2 120.19(18) . . ? C13 C12 C2 121.00(19) . . ? C14 C13 C12 120.1(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.7(2) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 119.6(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C12 C17 C16 120.7(2) . . ? C12 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C20 126.53(19) . . ? C19 C18 P1 115.16(15) . . ? C20 C18 P1 118.30(16) . . ? C18 C19 C21 128.39(19) . . ? C18 C19 C3 117.40(17) . . ? C21 C19 C3 114.18(17) . . ? F1 C20 F3 106.7(2) . . ? F1 C20 F2 105.7(2) . . ? F3 C20 F2 105.96(19) . . ? F1 C20 C18 111.89(18) . . ? F3 C20 C18 113.30(18) . . ? F2 C20 C18 112.7(2) . . ? F5 C21 F4 107.32(18) . . ? F5 C21 F6 105.52(19) . . ? F4 C21 F6 105.7(2) . . ? F5 C21 C19 115.7(2) . . ? F4 C21 C19 111.30(18) . . ? F6 C21 C19 110.64(17) . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 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 . . ? C29 C28 P2 113.87(14) . . ? C29 C28 Si3 130.29(15) . . ? P2 C28 Si3 115.84(10) . . ? C28 C29 C39 126.73(17) . . ? C28 C29 C30 117.87(16) . . ? C39 C29 C30 115.24(15) . . ? C46 C30 C31 109.09(15) . . ? C46 C30 C29 109.74(15) . . ? C31 C30 C29 105.71(14) . . ? C46 C30 H30 110.7 . . ? C31 C30 H30 110.7 . . ? C29 C30 H30 110.7 . . ? C32 C31 C33 126.22(17) . . ? C32 C31 C30 117.66(16) . . ? C33 C31 C30 116.01(15) . . ? C31 C32 P2 114.31(14) . . ? C31 C32 Si4 128.12(15) . . ? P2 C32 Si4 117.40(10) . . ? C34 C33 C38 119.24(18) . . ? C34 C33 C31 121.19(17) . . ? C38 C33 C31 119.57(17) . . ? C33 C34 C35 120.3(2) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 119.8(2) . . ? C36 C35 H35 120.1 . . ? C34 C35 H35 120.1 . . ? C37 C36 C35 120.3(2) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.1(2) . . ? C36 C37 H37 119.9 . . ? C38 C37 H37 119.9 . . ? C37 C38 C33 120.1(2) . . ? C37 C38 H38 120.0 . . ? C33 C38 H38 120.0 . . ? C40 C39 C44 118.67(18) . . ? C40 C39 C29 121.26(17) . . ? C44 C39 C29 120.05(17) . . ? C41 C40 C39 120.87(18) . . ? C41 C40 H40 119.6 . . ? C39 C40 H40 119.6 . . ? C42 C41 C40 119.97(19) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C41 C42 C43 119.83(19) . . ? C41 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C42 C43 C44 120.4(2) . . ? C42 C43 H43 119.8 . . ? C44 C43 H43 119.8 . . ? C43 C44 C39 120.24(19) . . ? C43 C44 H44 119.9 . . ? C39 C44 H44 119.9 . . ? C46 C45 C47 126.93(18) . . ? C46 C45 P2 115.46(14) . . ? C47 C45 P2 117.60(14) . . ? C45 C46 C48 127.36(18) . . ? C45 C46 C30 116.78(16) . . ? C48 C46 C30 115.86(16) . . ? F8 C47 F9 106.95(19) . . ? F8 C47 F7 107.39(19) . . ? F9 C47 F7 104.29(17) . . ? F8 C47 C45 112.70(17) . . ? F9 C47 C45 113.73(17) . . ? F7 C47 C45 111.23(17) . . ? F11 C48 F10 107.49(18) . . ? F11 C48 F12 104.82(17) . . ? F10 C48 F12 105.76(18) . . ? F11 C48 C46 114.88(17) . . ? F10 C48 C46 111.51(17) . . ? F12 C48 C46 111.75(16) . . ? Si3 C49 H49A 109.5 . . ? Si3 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? Si3 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Si3 C50 H50A 109.5 . . ? Si3 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Si3 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Si3 C51 H51A 109.5 . . ? Si3 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Si3 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? Si4 C52 H52A 109.5 . . ? Si4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? Si4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? Si4 C53 H53A 109.5 . . ? Si4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? Si4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? Si4 C54 H54A 109.5 . . ? Si4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? Si4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C22 Si1 C24 110.51(10) . . ? C22 Si1 C23 108.43(10) . . ? C24 Si1 C23 108.44(10) . . ? C22 Si1 C1 113.43(9) . . ? C24 Si1 C1 109.40(9) . . ? C23 Si1 C1 106.44(9) . . ? C25 Si2 C27 109.04(11) . . ? C25 Si2 C26 108.59(10) . . ? C27 Si2 C26 112.63(12) . . ? C25 Si2 C5 108.25(9) . . ? C27 Si2 C5 111.14(9) . . ? C26 Si2 C5 107.06(9) . . ? C49 Si3 C50 108.65(10) . . ? C49 Si3 C51 110.69(10) . . ? C50 Si3 C51 109.19(10) . . ? C49 Si3 C28 112.39(9) . . ? C50 Si3 C28 106.65(9) . . ? C51 Si3 C28 109.14(9) . . ? C53 Si4 C52 109.15(14) . . ? C53 Si4 C54 109.16(12) . . ? C52 Si4 C54 111.51(13) . . ? C53 Si4 C32 107.40(10) . . ? C52 Si4 C32 107.14(10) . . ? C54 Si4 C32 112.34(9) . . ? C18 P1 C5 95.53(8) . . ? C18 P1 C1 94.16(9) . . ? C5 P1 C1 96.75(8) . . ? C32 P2 C45 95.80(8) . . ? C32 P2 C28 96.32(8) . . ? C45 P2 C28 94.12(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 P1 C1 C2 C12 168.36(15) . . . . ? Si1 C1 C2 C12 -13.5(3) . . . . ? P1 C1 C2 C3 -6.5(2) . . . . ? Si1 C1 C2 C3 171.71(14) . . . . ? C1 C2 C3 C19 -53.2(2) . . . . ? C12 C2 C3 C19 131.39(17) . . . . ? C1 C2 C3 C4 64.1(2) . . . . ? C12 C2 C3 C4 -111.31(17) . . . . ? C19 C3 C4 C5 56.2(2) . . . . ? C2 C3 C4 C5 -61.8(2) . . . . ? C19 C3 C4 C6 -128.09(17) . . . . ? C2 C3 C4 C6 113.86(17) . . . . ? C6 C4 C5 P1 -172.26(15) . . . . ? C3 C4 C5 P1 2.9(2) . . . . ? C6 C4 C5 Si2 1.3(3) . . . . ? C3 C4 C5 Si2 176.43(13) . . . . ? C5 C4 C6 C7 -109.1(2) . . . . ? C3 C4 C6 C7 75.7(2) . . . . ? C5 C4 C6 C11 73.4(3) . . . . ? C3 C4 C6 C11 -101.83(19) . . . . ? C11 C6 C7 C8 -1.1(3) . . . . ? C4 C6 C7 C8 -178.67(17) . . . . ? C6 C7 C8 C9 1.4(3) . . . . ? C7 C8 C9 C10 -0.8(3) . . . . ? C8 C9 C10 C11 -0.1(3) . . . . ? C9 C10 C11 C6 0.4(3) . . . . ? C7 C6 C11 C10 0.2(3) . . . . ? C4 C6 C11 C10 177.77(17) . . . . ? C1 C2 C12 C17 -44.8(3) . . . . ? C3 C2 C12 C17 130.07(19) . . . . ? C1 C2 C12 C13 137.5(2) . . . . ? C3 C2 C12 C13 -47.6(2) . . . . ? C17 C12 C13 C14 2.9(3) . . . . ? C2 C12 C13 C14 -179.4(2) . . . . ? C12 C13 C14 C15 -0.8(4) . . . . ? C13 C14 C15 C16 -1.3(4) . . . . ? C14 C15 C16 C17 1.3(4) . . . . ? C13 C12 C17 C16 -2.9(3) . . . . ? C2 C12 C17 C16 179.35(19) . . . . ? C15 C16 C17 C12 0.8(3) . . . . ? C20 C18 C19 C21 0.9(3) . . . . ? P1 C18 C19 C21 179.81(17) . . . . ? C20 C18 C19 C3 -177.04(19) . . . . ? P1 C18 C19 C3 1.9(2) . . . . ? C4 C3 C19 C18 -59.2(2) . . . . ? C2 C3 C19 C18 56.1(2) . . . . ? C4 C3 C19 C21 122.64(18) . . . . ? C2 C3 C19 C21 -122.08(18) . . . . ? C19 C18 C20 F1 169.7(2) . . . . ? P1 C18 C20 F1 -9.2(3) . . . . ? C19 C18 C20 F3 -69.6(3) . . . . ? P1 C18 C20 F3 111.5(2) . . . . ? C19 C18 C20 F2 50.7(3) . . . . ? P1 C18 C20 F2 -128.20(18) . . . . ? C18 C19 C21 F5 13.1(3) . . . . ? C3 C19 C21 F5 -168.97(18) . . . . ? C18 C19 C21 F4 -109.8(2) . . . . ? C3 C19 C21 F4 68.2(2) . . . . ? C18 C19 C21 F6 133.0(2) . . . . ? C3 C19 C21 F6 -49.1(2) . . . . ? P2 C28 C29 C39 171.11(15) . . . . ? Si3 C28 C29 C39 -9.4(3) . . . . ? P2 C28 C29 C30 -4.1(2) . . . . ? Si3 C28 C29 C30 175.40(13) . . . . ? C28 C29 C30 C46 -55.3(2) . . . . ? C39 C29 C30 C46 128.94(16) . . . . ? C28 C29 C30 C31 62.2(2) . . . . ? C39 C29 C30 C31 -113.55(17) . . . . ? C46 C30 C31 C32 56.4(2) . . . . ? C29 C30 C31 C32 -61.5(2) . . . . ? C46 C30 C31 C33 -127.18(17) . . . . ? C29 C30 C31 C33 114.88(17) . . . . ? C33 C31 C32 P2 -172.97(15) . . . . ? C30 C31 C32 P2 3.0(2) . . . . ? C33 C31 C32 Si4 2.2(3) . . . . ? C30 C31 C32 Si4 178.14(13) . . . . ? C32 C31 C33 C34 -109.5(2) . . . . ? C30 C31 C33 C34 74.4(2) . . . . ? C32 C31 C33 C38 71.1(3) . . . . ? C30 C31 C33 C38 -105.0(2) . . . . ? C38 C33 C34 C35 -3.2(3) . . . . ? C31 C33 C34 C35 177.41(18) . . . . ? C33 C34 C35 C36 2.0(3) . . . . ? C34 C35 C36 C37 0.9(3) . . . . ? C35 C36 C37 C38 -2.5(3) . . . . ? C36 C37 C38 C33 1.3(3) . . . . ? C34 C33 C38 C37 1.6(3) . . . . ? C31 C33 C38 C37 -179.00(18) . . . . ? C28 C29 C39 C40 125.3(2) . . . . ? C30 C29 C39 C40 -59.3(2) . . . . ? C28 C29 C39 C44 -56.2(3) . . . . ? C30 C29 C39 C44 119.09(19) . . . . ? C44 C39 C40 C41 1.9(3) . . . . ? C29 C39 C40 C41 -179.67(18) . . . . ? C39 C40 C41 C42 -1.3(3) . . . . ? C40 C41 C42 C43 -0.1(3) . . . . ? C41 C42 C43 C44 0.9(3) . . . . ? C42 C43 C44 C39 -0.3(3) . . . . ? C40 C39 C44 C43 -1.1(3) . . . . ? C29 C39 C44 C43 -179.53(19) . . . . ? C47 C45 C46 C48 3.6(3) . . . . ? P2 C45 C46 C48 -177.71(15) . . . . ? C47 C45 C46 C30 -175.51(18) . . . . ? P2 C45 C46 C30 3.2(2) . . . . ? C31 C30 C46 C45 -59.9(2) . . . . ? C29 C30 C46 C45 55.5(2) . . . . ? C31 C30 C46 C48 120.92(17) . . . . ? C29 C30 C46 C48 -123.71(17) . . . . ? C46 C45 C47 F8 -88.9(3) . . . . ? P2 C45 C47 F8 92.4(2) . . . . ? C46 C45 C47 F9 33.0(3) . . . . ? P2 C45 C47 F9 -145.70(15) . . . . ? C46 C45 C47 F7 150.40(19) . . . . ? P2 C45 C47 F7 -28.3(2) . . . . ? C45 C46 C48 F11 30.1(3) . . . . ? C30 C46 C48 F11 -150.78(17) . . . . ? C45 C46 C48 F10 -92.5(2) . . . . ? C30 C46 C48 F10 86.6(2) . . . . ? C45 C46 C48 F12 149.4(2) . . . . ? C30 C46 C48 F12 -31.5(2) . . . . ? C2 C1 Si1 C22 -23.1(2) . . . . ? P1 C1 Si1 C22 155.07(10) . . . . ? C2 C1 Si1 C24 100.8(2) . . . . ? P1 C1 Si1 C24 -81.05(12) . . . . ? C2 C1 Si1 C23 -142.23(19) . . . . ? P1 C1 Si1 C23 35.93(12) . . . . ? C4 C5 Si2 C25 155.82(18) . . . . ? P1 C5 Si2 C25 -30.79(13) . . . . ? C4 C5 Si2 C27 36.1(2) . . . . ? P1 C5 Si2 C27 -150.52(12) . . . . ? C4 C5 Si2 C26 -87.29(19) . . . . ? P1 C5 Si2 C26 86.10(13) . . . . ? C29 C28 Si3 C49 -25.6(2) . . . . ? P2 C28 Si3 C49 153.86(11) . . . . ? C29 C28 Si3 C50 -144.59(18) . . . . ? P2 C28 Si3 C50 34.90(13) . . . . ? C29 C28 Si3 C51 97.6(2) . . . . ? P2 C28 Si3 C51 -82.94(12) . . . . ? C31 C32 Si4 C53 150.16(19) . . . . ? P2 C32 Si4 C53 -34.85(15) . . . . ? C31 C32 Si4 C52 -92.7(2) . . . . ? P2 C32 Si4 C52 82.31(15) . . . . ? C31 C32 Si4 C54 30.1(2) . . . . ? P2 C32 Si4 C54 -154.89(12) . . . . ? C19 C18 P1 C5 46.91(16) . . . . ? C20 C18 P1 C5 -134.06(16) . . . . ? C19 C18 P1 C1 -50.30(16) . . . . ? C20 C18 P1 C1 128.73(16) . . . . ? C4 C5 P1 C18 -48.98(16) . . . . ? Si2 C5 P1 C18 136.73(11) . . . . ? C4 C5 P1 C1 45.89(15) . . . . ? Si2 C5 P1 C1 -128.39(11) . . . . ? C2 C1 P1 C18 52.21(15) . . . . ? Si1 C1 P1 C18 -126.28(10) . . . . ? C2 C1 P1 C5 -43.87(15) . . . . ? Si1 C1 P1 C5 137.64(10) . . . . ? C31 C32 P2 C45 -48.52(15) . . . . ? Si4 C32 P2 C45 135.81(11) . . . . ? C31 C32 P2 C28 46.30(15) . . . . ? Si4 C32 P2 C28 -129.38(11) . . . . ? C46 C45 P2 C32 45.72(16) . . . . ? C47 C45 P2 C32 -135.43(15) . . . . ? C46 C45 P2 C28 -51.07(16) . . . . ? C47 C45 P2 C28 127.78(15) . . . . ? C29 C28 P2 C32 -45.60(15) . . . . ? Si3 C28 P2 C32 134.82(10) . . . . ? C29 C28 P2 C45 50.70(15) . . . . ? Si3 C28 P2 C45 -128.87(11) . . . . ? _refine_diff_density_max 0.359 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.050 _shelx_res_file ; MR335_a.res created by SHELXL-2014/7 TITL MR335_a.res in P-1 REM Old TITL MR335 in P-1 REM SHELXT solution in P-1 REM R1 0.130, Rweak 0.008, Alpha 0.057, Orientation as input REM Formula found by SHELXT: C54 F12 Si4 P2 CELL 1.54178 10.78717 15.23382 18.26277 97.4263 103.9082 99.6371 ZERR 4.000 0.00008 0.00010 0.00013 0.0003 0.0003 0.0003 LATT 1 SFAC C H F SI P UNIT 108 116 24 8 4 TEMP -173.140 SIZE 0.14 0.28 0.28 L.S. 30 BOND $H LIST 6 acta conf FMAP 2 PLAN 20 WGHT 0.032500 1.947100 FVAR 0.60816 C1 1 1.153450 0.292095 0.299071 11.00000 0.01871 0.01561 = 0.01635 0.00445 0.00393 0.00288 C2 1 1.077127 0.333291 0.333881 11.00000 0.01997 0.01500 = 0.01512 0.00551 0.00533 0.00374 C3 1 0.932678 0.285407 0.316864 11.00000 0.01778 0.01679 = 0.01819 0.00538 0.00603 0.00525 AFIX 13 H3 2 0.883414 0.323828 0.342653 11.00000 -1.20000 AFIX 0 C4 1 0.934739 0.196285 0.348499 11.00000 0.01437 0.01473 = 0.01542 0.00385 0.00288 0.00145 C5 1 0.994408 0.136770 0.317675 11.00000 0.01766 0.01571 = 0.01662 0.00314 0.00565 0.00163 C6 1 0.877515 0.189452 0.414680 11.00000 0.01937 0.00975 = 0.01863 0.00268 0.00705 0.00512 C7 1 0.742838 0.172639 0.404093 11.00000 0.01972 0.02183 = 0.01694 0.00252 0.00377 0.00447 AFIX 43 H7 2 0.686350 0.164119 0.353906 11.00000 -1.20000 AFIX 0 C8 1 0.690455 0.168228 0.466271 11.00000 0.01792 0.02488 = 0.02464 0.00434 0.00875 0.00530 AFIX 43 H8 2 0.598456 0.155377 0.458292 11.00000 -1.20000 AFIX 0 C9 1 0.771714 0.182471 0.539737 11.00000 0.02976 0.01895 = 0.02016 0.00520 0.01369 0.00966 AFIX 43 H9 2 0.735722 0.180181 0.582261 11.00000 -1.20000 AFIX 0 C10 1 0.905993 0.200117 0.551124 11.00000 0.02654 0.02015 = 0.01571 0.00254 0.00384 0.00861 AFIX 43 H10 2 0.962040 0.210046 0.601560 11.00000 -1.20000 AFIX 0 C11 1 0.958765 0.203311 0.488945 11.00000 0.01864 0.01721 = 0.01945 0.00295 0.00523 0.00536 AFIX 43 H11 2 1.050803 0.215013 0.497090 11.00000 -1.20000 AFIX 0 C12 1 1.118678 0.417304 0.392320 11.00000 0.02808 0.01386 = 0.02028 0.00364 0.01207 0.00101 C13 1 1.044358 0.484429 0.389638 11.00000 0.04161 0.01876 = 0.03745 0.00643 0.01857 0.00919 AFIX 43 H13 2 0.965580 0.476268 0.350260 11.00000 -1.20000 AFIX 0 C14 1 1.085469 0.562681 0.444273 11.00000 0.06371 0.01594 = 0.05269 0.00234 0.03218 0.00867 AFIX 43 H14 2 1.035146 0.608307 0.441740 11.00000 -1.20000 AFIX 0 C15 1 1.198182 0.575000 0.502049 11.00000 0.07130 0.01851 = 0.04000 -0.00835 0.03194 -0.00862 AFIX 43 H15 2 1.226467 0.629519 0.538606 11.00000 -1.20000 AFIX 0 C16 1 1.270874 0.507998 0.507164 11.00000 0.04721 0.03349 = 0.02408 -0.00429 0.01159 -0.00989 AFIX 43 H16 2 1.347941 0.515916 0.547768 11.00000 -1.20000 AFIX 0 C17 1 1.230329 0.429095 0.452498 11.00000 0.03370 0.02390 = 0.02249 0.00204 0.01023 0.00127 AFIX 43 H17 2 1.279468 0.382836 0.456360 11.00000 -1.20000 AFIX 0 C18 1 0.927940 0.213443 0.188855 11.00000 0.02079 0.02418 = 0.01695 0.00614 0.00407 -0.00160 C19 1 0.871155 0.262991 0.230824 11.00000 0.01803 0.02250 = 0.02152 0.01107 0.00344 0.00144 C20 1 0.887883 0.186813 0.102859 11.00000 0.02876 0.04954 = 0.01973 0.00624 0.00472 0.00024 C21 1 0.754125 0.303372 0.204329 11.00000 0.02487 0.03582 = 0.02994 0.01532 0.00325 0.00791 C22 1 1.378475 0.457146 0.310784 11.00000 0.02794 0.02395 = 0.03188 0.00774 0.00859 -0.00058 AFIX 137 H22A 2 1.464500 0.473186 0.301474 11.00000 -1.50000 H22B 2 1.383447 0.482000 0.363898 11.00000 -1.50000 H22C 2 1.315188 0.482249 0.275852 11.00000 -1.50000 AFIX 0 C23 1 1.330244 0.285332 0.194701 11.00000 0.02648 0.03347 = 0.02543 0.00328 0.01317 0.00176 AFIX 137 H23A 2 1.263122 0.304389 0.157229 11.00000 -1.50000 H23B 2 1.313659 0.219113 0.187162 11.00000 -1.50000 H23C 2 1.416336 0.308353 0.187771 11.00000 -1.50000 AFIX 0 C24 1 1.439202 0.282064 0.363441 11.00000 0.02407 0.03285 = 0.03182 0.00877 0.00690 0.01120 AFIX 137 H24A 2 1.404850 0.217061 0.357671 11.00000 -1.50000 H24B 2 1.447073 0.311610 0.415779 11.00000 -1.50000 H24C 2 1.525262 0.291611 0.353383 11.00000 -1.50000 AFIX 0 C25 1 1.041412 -0.048052 0.262305 11.00000 0.03595 0.01862 = 0.02979 -0.00164 0.01015 0.00626 AFIX 137 H25A 2 0.965075 -0.054388 0.218674 11.00000 -1.50000 H25B 2 1.049351 -0.107788 0.275011 11.00000 -1.50000 H25C 2 1.120157 -0.020916 0.248929 11.00000 -1.50000 AFIX 0 C26 1 1.177901 0.050704 0.423928 11.00000 0.04094 0.02235 = 0.02863 0.00304 -0.00002 0.01225 AFIX 137 H26A 2 1.201461 -0.006244 0.435823 11.00000 -1.50000 H26B 2 1.166992 0.086010 0.469915 11.00000 -1.50000 H26C 2 1.247219 0.085369 0.406721 11.00000 -1.50000 AFIX 0 C27 1 0.880839 -0.031376 0.376861 11.00000 0.04348 0.02257 = 0.06010 0.02068 0.03183 0.01352 AFIX 137 H27A 2 0.801185 -0.041626 0.334755 11.00000 -1.50000 H27B 2 0.870582 0.006893 0.421557 11.00000 -1.50000 H27C 2 0.896587 -0.089537 0.390276 11.00000 -1.50000 AFIX 0 C28 1 0.470505 0.834591 0.206575 11.00000 0.01650 0.01690 = 0.01617 0.00141 0.00366 0.00159 C29 1 0.538410 0.787170 0.170118 11.00000 0.01396 0.01593 = 0.01569 0.00214 0.00244 0.00040 C30 1 0.541782 0.689725 0.184546 11.00000 0.01360 0.01589 = 0.01685 0.00136 0.00555 0.00368 AFIX 13 H30 2 0.597967 0.661920 0.155969 11.00000 -1.20000 AFIX 0 C31 1 0.399160 0.637157 0.155705 11.00000 0.01472 0.01479 = 0.01629 0.00379 0.00351 0.00221 C32 1 0.312538 0.665266 0.189873 11.00000 0.01560 0.01628 = 0.01569 0.00369 0.00437 0.00222 C33 1 0.369990 0.562867 0.088770 11.00000 0.01308 0.01780 = 0.01974 0.00077 0.00722 -0.00053 C34 1 0.408928 0.481476 0.096647 11.00000 0.02934 0.02280 = 0.02674 0.00511 0.01164 0.00742 AFIX 43 H34 2 0.458192 0.473493 0.145061 11.00000 -1.20000 AFIX 0 C35 1 0.376173 0.411613 0.034031 11.00000 0.03772 0.01772 = 0.04140 -0.00062 0.02437 0.00384 AFIX 43 H35 2 0.400636 0.355331 0.039962 11.00000 -1.20000 AFIX 0 C36 1 0.308033 0.424180 -0.036779 11.00000 0.02312 0.03198 = 0.03139 -0.01265 0.01619 -0.00540 AFIX 43 H36 2 0.284559 0.376139 -0.079443 11.00000 -1.20000 AFIX 0 C37 1 0.273898 0.506010 -0.045899 11.00000 0.02464 0.04207 = 0.02175 -0.00345 0.00475 0.00364 AFIX 43 H37 2 0.230016 0.515046 -0.095195 11.00000 -1.20000 AFIX 0 C38 1 0.303420 0.575254 0.016693 11.00000 0.02426 0.02715 = 0.02169 0.00094 0.00560 0.00688 AFIX 43 H38 2 0.278201 0.631238 0.010408 11.00000 -1.20000 AFIX 0 C39 1 0.604599 0.815729 0.111843 11.00000 0.01748 0.01458 = 0.01727 0.00002 0.00561 0.00065 C40 1 0.736772 0.816360 0.120620 11.00000 0.02141 0.02111 = 0.02200 0.00577 0.00654 0.00353 AFIX 43 H40 2 0.785642 0.797933 0.164461 11.00000 -1.20000 AFIX 0 C41 1 0.797879 0.843548 0.066161 11.00000 0.02165 0.02796 = 0.03156 0.00614 0.01253 0.00188 AFIX 43 H41 2 0.888417 0.844870 0.073370 11.00000 -1.20000 AFIX 0 C42 1 0.726981 0.868700 0.001438 11.00000 0.03453 0.02901 = 0.02449 0.00744 0.01664 0.00130 AFIX 43 H42 2 0.768685 0.887411 -0.035870 11.00000 -1.20000 AFIX 0 C43 1 0.594945 0.866562 -0.008905 11.00000 0.03356 0.03603 = 0.01910 0.00909 0.00567 0.00493 AFIX 43 H43 2 0.545973 0.883031 -0.053759 11.00000 -1.20000 AFIX 0 C44 1 0.533686 0.840457 0.045966 11.00000 0.02172 0.03046 = 0.02118 0.00540 0.00603 0.00552 AFIX 43 H44 2 0.443191 0.839453 0.038571 11.00000 -1.20000 AFIX 0 C45 1 0.526338 0.728688 0.314975 11.00000 0.01596 0.01879 = 0.01747 0.00308 0.00402 0.00062 C46 1 0.590721 0.690613 0.269796 11.00000 0.01448 0.01598 = 0.01914 0.00316 0.00286 -0.00047 C47 1 0.560787 0.743572 0.400844 11.00000 0.02418 0.03219 = 0.01718 0.00147 0.00440 0.00568 C48 1 0.707795 0.649490 0.293867 11.00000 0.01980 0.02614 = 0.02212 0.00317 0.00226 0.00628 C49 1 0.594969 1.028302 0.190228 11.00000 0.03345 0.02127 = 0.03200 0.00439 0.00991 0.00013 AFIX 137 H49A 2 0.599770 1.007760 0.138059 11.00000 -1.50000 H49B 2 0.675481 1.024061 0.227077 11.00000 -1.50000 H49C 2 0.584357 1.091259 0.195655 11.00000 -1.50000 AFIX 0 C50 1 0.442664 0.998308 0.307612 11.00000 0.03460 0.01921 = 0.03089 -0.00215 0.01253 0.00437 AFIX 137 H50A 2 0.436417 1.062125 0.312100 11.00000 -1.50000 H50B 2 0.521018 0.992234 0.345340 11.00000 -1.50000 H50C 2 0.365258 0.962952 0.317098 11.00000 -1.50000 AFIX 0 C51 1 0.297515 0.959410 0.137907 11.00000 0.03025 0.02945 = 0.03086 0.00708 0.00693 0.01161 AFIX 137 H51A 2 0.308102 0.947717 0.085949 11.00000 -1.50000 H51B 2 0.276609 1.019287 0.147566 11.00000 -1.50000 H51C 2 0.226531 0.913204 0.142945 11.00000 -1.50000 AFIX 0 C52 1 0.049497 0.684253 0.097966 11.00000 0.01954 0.04952 = 0.07361 0.03590 -0.00037 0.00328 AFIX 137 H52A 2 0.072269 0.672033 0.049360 11.00000 -1.50000 H52B 2 0.077962 0.748986 0.119311 11.00000 -1.50000 H52C 2 -0.045247 0.666432 0.089047 11.00000 -1.50000 AFIX 0 C53 1 0.082776 0.638025 0.256838 11.00000 0.03445 0.06130 = 0.04678 -0.00339 0.02739 -0.00688 AFIX 137 H53A 2 0.092630 0.703147 0.273718 11.00000 -1.50000 H53B 2 0.138203 0.613308 0.296447 11.00000 -1.50000 H53C 2 -0.008593 0.608007 0.248054 11.00000 -1.50000 AFIX 0 C54 1 0.088946 0.495048 0.126988 11.00000 0.01891 0.02609 = 0.05721 -0.00333 0.00897 -0.00028 AFIX 137 H54A 2 -0.002887 0.471619 0.123773 11.00000 -1.50000 H54B 2 0.144243 0.463476 0.160604 11.00000 -1.50000 H54C 2 0.102765 0.485116 0.075702 11.00000 -1.50000 AFIX 0 F1 3 0.975977 0.150116 0.077362 11.00000 0.05426 0.14764 = 0.02093 -0.00646 0.01165 0.03772 F2 3 0.873656 0.257346 0.067234 11.00000 0.08237 0.06681 = 0.02717 0.02722 0.00119 -0.00780 F3 3 0.775078 0.127393 0.076122 11.00000 0.04677 0.05499 = 0.02197 -0.00052 -0.00081 -0.01272 F4 3 0.787372 0.393128 0.213075 11.00000 0.04224 0.03256 = 0.07365 0.02100 0.00669 0.01597 F5 3 0.685517 0.273258 0.132659 11.00000 0.04915 0.07577 = 0.04253 0.00377 -0.01851 0.03053 F6 3 0.670045 0.286940 0.246756 11.00000 0.02872 0.09370 = 0.07281 0.05179 0.02536 0.03177 F7 3 0.521673 0.816050 0.429076 11.00000 0.05081 0.06724 = 0.02073 -0.00749 0.00507 0.03045 F8 3 0.507858 0.674300 0.427153 11.00000 0.11405 0.05997 = 0.02146 0.01100 0.01285 -0.03610 F9 3 0.688617 0.760393 0.433813 11.00000 0.03164 0.07754 = 0.02449 -0.00842 -0.00735 0.01874 F10 3 0.818174 0.709435 0.305139 11.00000 0.01519 0.04068 = 0.13752 0.01681 0.00509 0.00391 F11 3 0.714854 0.613621 0.356382 11.00000 0.06720 0.07690 = 0.03482 0.02776 0.01747 0.05232 F12 3 0.710519 0.582066 0.240039 11.00000 0.04863 0.05135 = 0.03368 -0.00474 0.00046 0.03602 SI1 4 1.325693 0.331429 0.293883 11.00000 0.01669 0.01931 = 0.01888 0.00487 0.00573 0.00309 SI2 4 1.021760 0.025899 0.346450 11.00000 0.02332 0.01342 = 0.02116 0.00310 0.00858 0.00570 SI3 4 0.452767 0.955632 0.209059 11.00000 0.02265 0.01508 = 0.02152 0.00183 0.00677 0.00403 SI4 4 0.132094 0.618389 0.166655 11.00000 0.01359 0.01993 = 0.02415 0.00532 0.00696 0.00292 P1 5 1.072501 0.176239 0.243885 11.00000 0.02032 0.01625 = 0.01707 0.00156 0.00819 0.00310 P2 5 0.380753 0.768847 0.264458 11.00000 0.01621 0.01772 = 0.01561 0.00127 0.00628 0.00393 HKLF 4 REM MR335_a.res in P-1 REM R1 = 0.0373 for 8562 Fo > 4sig(Fo) and 0.0463 for all 9977 data REM 661 parameters refined using 0 restraints END WGHT 0.0325 1.9471 REM Highest difference peak 0.359, deepest hole -0.355, 1-sigma level 0.050 Q1 1 0.4251 0.6947 0.4069 11.00000 0.05 0.36 Q2 1 0.6373 0.7058 0.4340 11.00000 0.05 0.31 Q3 1 1.2331 0.3212 0.3109 11.00000 0.05 0.28 Q4 1 0.4703 0.7598 0.4307 11.00000 0.05 0.27 Q5 1 0.7662 0.6801 0.3649 11.00000 0.05 0.27 Q6 1 0.9370 0.2213 0.0677 11.00000 0.05 0.27 Q7 1 0.2353 0.6402 0.1787 11.00000 0.05 0.27 Q8 1 1.0201 0.0975 0.3372 11.00000 0.05 0.26 Q9 1 0.5725 0.6943 0.2332 11.00000 0.05 0.26 Q10 1 0.5809 0.7303 0.2936 11.00000 0.05 0.25 Q11 1 0.9476 0.0006 0.3636 11.00000 0.05 0.25 Q12 1 0.7016 0.3487 0.2671 11.00000 0.05 0.25 Q13 1 0.9228 0.2577 0.2047 11.00000 0.05 0.24 Q14 1 0.9024 0.2809 0.2716 11.00000 0.05 0.24 Q15 1 0.9430 0.0947 0.0974 11.00000 0.05 0.24 Q16 1 0.4629 0.7420 0.2966 11.00000 0.05 0.24 Q17 1 0.9085 0.2028 0.1508 11.00000 0.05 0.23 Q18 1 1.1132 0.0387 0.4453 11.00000 0.05 0.23 Q19 1 0.9931 0.1785 0.3514 11.00000 0.05 0.23 Q20 1 0.5423 0.6823 0.2876 11.00000 0.05 0.23 ; _shelx_res_checksum 35978 _shelx_hkl_file ; 1 0 0 56.39 2.50 2 0 0 144.99 6.00 -3 0 0 1457.55 45.00 3 0 0 1446.36 46.50 -4 0 0 12.30 1.80 4 0 0 11.20 2.90 -5 0 0 1978.10 61.99 5 0 0 1966.00 62.99 5 0 0 2035.10 65.79 -6 0 0 226.28 14.70 -6 0 0 220.68 13.70 6 0 0 220.68 15.80 6 0 0 191.58 12.20 -7 0 0 62.39 8.10 -7 0 0 62.79 9.10 7 0 0 65.29 6.50 -8 0 0 244.48 16.60 -8 0 0 225.58 14.10 8 0 0 253.27 12.20 -9 0 0 34.80 7.50 -9 0 0 26.40 8.80 9 0 0 34.40 5.40 -10 0 0 28.10 6.50 10 0 0 14.30 4.30 -11 0 0 16.70 6.00 -11 0 0 24.10 5.60 11 0 0 25.70 4.60 -12 0 0 142.59 9.10 -12 0 0 162.88 10.90 12 -1 0 3.00 5.50 -12 1 0 23.50 6.20 -12 1 0 18.30 4.70 11 -1 0 11.50 4.30 -11 1 0 5.60 5.10 -11 1 0 10.60 6.50 10 -1 0 352.26 15.30 -10 1 0 338.17 17.60 9 -1 0 90.59 7.80 -9 1 0 90.99 11.10 8 -1 0 9.10 3.80 -8 1 0 15.50 6.00 -8 1 0 12.80 7.30 7 -1 0 1027.30 35.10 -7 1 0 1046.50 39.20 -7 1 0 1048.80 37.30 6 -1 0 498.95 22.70 -6 1 0 453.35 20.40 -6 1 0 472.25 22.40 -6 1 0 469.45 18.50 -5 1 0 1946.21 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11.10 9 -3 0 415.26 17.00 9 -3 0 391.56 25.10 -9 3 0 405.66 20.20 8 -3 0 27.90 4.50 8 -3 0 40.70 11.30 -8 3 0 27.10 6.60 7 -3 0 15.60 9.30 7 -3 0 -1.00 3.10 7 -3 0 6.80 11.30 -7 3 0 2.20 5.80 6 -3 0 2507.65 78.99 -6 3 0 2280.87 77.69 5 -3 0 508.05 19.60 5 -3 0 492.25 23.40 5 -3 0 510.95 17.70 -5 3 0 487.35 19.40 -5 3 0 474.45 18.00 4 -3 0 1186.68 39.10 4 -3 0 1210.68 39.90 4 -3 0 1190.38 38.40 3 -3 0 6.30 2.20 2 -3 0 5.80 1.60 -2 3 0 5.40 1.80 1 -3 0 148.39 5.50 1 -3 0 159.08 6.30 -1 3 0 152.08 6.20 0 -3 0 2.20 1.30 0 -3 0 0.30 0.90 0 3 0 1.90 0.90 0 3 0 1.30 1.20 -1 -3 0 2027.30 60.79 1 3 0 1868.01 60.79 1 3 0 1939.11 60.59 -2 -3 0 191.18 8.70 2 3 0 212.08 8.90 3 3 0 26.20 3.90 4 3 0 4097.19 129.19 -5 -3 0 147.89 12.40 -5 -3 0 120.89 12.80 5 3 0 118.59 12.40 5 3 0 126.79 9.10 -6 -3 0 558.54 28.00 -6 -3 0 555.24 22.70 -6 -3 0 568.04 24.80 6 3 0 560.64 21.30 -7 -3 0 1720.33 70.09 -7 -3 0 1906.21 63.59 -7 -3 0 1844.42 60.69 7 3 0 1833.92 59.79 -8 -3 0 680.83 26.10 -8 -3 0 666.63 29.00 8 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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===============================================