data_L1.DMF _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H13 N3 O5, C3 H7 N O' _chemical_formula_sum 'C18 H20 N4 O6' _chemical_formula_weight 388.38 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 7.7434(3) _cell_length_b 12.1722(5) _cell_length_c 20.2617(7) _cell_angle_alpha 95.227(3) _cell_angle_beta 93.915(2) _cell_angle_gamma 98.882(2) _cell_volume 1872.41(12) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2642 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 22.58 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_F_000 816 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 0.105 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.970 _exptl_absorpt_correction_T_max 0.987 _exptl_absorpt_process_details multi-scan _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23947 _diffrn_reflns_av_unetI/netI 0.0581 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.013 _diffrn_reflns_theta_max 25.050 _diffrn_reflns_theta_full 25.050 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measured_fraction_theta_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.981 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.981 _diffrn_reflns_point_group_measured_fraction_full 0.981 _reflns_number_total 6504 _reflns_number_gt 3582 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0100P)^2^+1.5000P] 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 6504 _refine_ls_number_parameters 511 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1107 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1357 _refine_ls_wR_factor_gt 0.0966 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C5 C 0.0623(4) 0.1971(3) 0.12544(15) 0.0542(9) Uani 1 1 d . . . . . H5 H -0.0056 0.1265 0.1173 0.065 Uiso 1 1 calc R U . . . C8 C 0.2613(4) 0.4064(3) 0.14949(15) 0.0523(8) Uani 1 1 d . . . . . H8 H 0.3282 0.4773 0.1576 0.063 Uiso 1 1 calc R U . . . C2 C 0.2005(4) 0.4397(3) 0.02996(16) 0.0516(8) Uani 1 1 d . . . . . C7 C 0.2439(4) 0.3387(3) 0.20095(15) 0.0522(8) Uani 1 1 d . . . . . H7 H 0.2981 0.3642 0.2431 0.063 Uiso 1 1 calc R U . . . C28 C 0.6968(4) 0.5418(3) 0.40932(15) 0.0498(8) Uani 1 1 d . . . . . C3 C 0.1811(4) 0.3707(3) 0.08609(14) 0.0480(8) Uani 1 1 d . . . . . C13 C 0.2537(4) -0.0193(3) 0.51958(16) 0.0543(9) Uani 1 1 d . . . . . C6 C 0.1449(4) 0.2325(3) 0.18898(15) 0.0495(8) Uani 1 1 d . . . . . C25 C 0.7572(4) 0.4755(3) 0.53429(15) 0.0484(8) Uani 1 1 d . . . . . C18 C 0.7322(4) 0.1459(3) 0.84121(15) 0.0507(8) Uani 1 1 d . . . . . C19 C 0.6449(4) 0.1149(3) 0.77837(15) 0.0541(9) Uani 1 1 d . . . . . H19 H 0.5707 0.0465 0.7702 0.065 Uiso 1 1 calc R U . . . C20 C 0.6662(4) 0.1836(3) 0.72781(16) 0.0551(9) Uani 1 1 d . . . . . H20 H 0.6063 0.1616 0.6862 0.066 Uiso 1 1 calc R U . . . C15 C 0.2828(4) 0.1209(3) 0.44423(16) 0.0567(9) Uani 1 1 d . . . . . H15 H 0.3271 0.1927 0.4349 0.068 Uiso 1 1 calc R U . . . C33 C 0.1402(5) 0.6610(3) 0.70566(16) 0.0580(9) Uani 1 1 d . . . . . H33 H 0.1351 0.7062 0.6712 0.070 Uiso 1 1 calc R U . . . C24 C 0.7323(4) 0.3569(3) 0.62823(16) 0.0521(8) Uani 1 1 d . . . . . C21 C 0.7778(4) 0.2860(3) 0.73946(15) 0.0497(8) Uani 1 1 d . . . . . C26 C 0.6533(4) 0.4032(3) 0.48505(15) 0.0536(9) Uani 1 1 d . . . . . H26 H 0.6048 0.3319 0.4940 0.064 Uiso 1 1 calc R U . . . C4 C 0.0796(4) 0.2647(3) 0.07491(15) 0.0541(9) Uani 1 1 d . . . . . H4 H 0.0234 0.2397 0.0330 0.065 Uiso 1 1 calc R U . . . C29 C 0.8027(5) 0.6147(3) 0.45715(16) 0.0596(9) Uani 1 1 d . . . . . H29 H 0.8534 0.6850 0.4474 0.072 Uiso 1 1 calc R U . . . C11 C 0.1198(5) -0.0621(3) 0.40941(16) 0.0575(9) Uani 1 1 d . . . . . H11 H 0.0537 -0.1127 0.3766 0.069 Uiso 1 1 calc R U . . . C34 C 0.8109(5) 0.8534(3) 0.21825(17) 0.0607(9) Uani 1 1 d . . . . . H34 H 0.8001 0.8171 0.2565 0.073 Uiso 1 1 calc R U . . . C22 C 0.8662(4) 0.3164(3) 0.80241(16) 0.0550(9) Uani 1 1 d . . . . . H22 H 0.9423 0.3841 0.8106 0.066 Uiso 1 1 calc R U . . . C27 C 0.6218(4) 0.4373(3) 0.42258(16) 0.0545(9) Uani 1 1 d . . . . . H27 H 0.5503 0.3896 0.3898 0.065 Uiso 1 1 calc R U . . . C23 C 0.8431(4) 0.2482(3) 0.85243(16) 0.0553(9) Uani 1 1 d . . . . . H23 H 0.9020 0.2706 0.8942 0.066 Uiso 1 1 calc R U . . . C10 C 0.1812(4) 0.0460(3) 0.39518(15) 0.0499(8) Uani 1 1 d . . . . . C12 C 0.1556(5) -0.0949(3) 0.47124(16) 0.0575(9) Uani 1 1 d . . . . . H12 H 0.1142 -0.1673 0.4804 0.069 Uiso 1 1 calc R U . . . C17 C 0.7095(5) 0.0756(3) 0.89611(17) 0.0561(9) Uani 1 1 d . . . . . C9 C 0.1900(5) 0.1668(3) 0.30176(16) 0.0554(9) Uani 1 1 d . . . . . C14 C 0.3178(5) 0.0882(3) 0.50688(16) 0.0587(9) Uani 1 1 d . . . . . H14 H 0.3837 0.1383 0.5400 0.070 Uiso 1 1 calc R U . . . C35 C 0.6357(5) 0.6864(3) 0.15993(17) 0.0699(11) Uani 1 1 d . . . . . H35A H 0.6377 0.6627 0.2039 0.105 Uiso 1 1 calc R U . . . H35B H 0.6888 0.6365 0.1312 0.105 Uiso 1 1 calc R U . . . H35C H 0.5165 0.6856 0.1431 0.105 Uiso 1 1 calc R U . . . C30 C 0.8317(5) 0.5816(3) 0.51919(16) 0.0600(9) Uani 1 1 d . . . . . H30 H 0.9021 0.6303 0.5518 0.072 Uiso 1 1 calc R U . . . C31 C 0.2573(5) 0.6341(3) 0.81465(17) 0.0726(11) Uani 1 1 d . . . . . H31A H 0.2064 0.6669 0.8520 0.109 Uiso 1 1 calc R U . . . H31B H 0.3785 0.6314 0.8267 0.109 Uiso 1 1 calc R U . . . H31C H 0.1958 0.5597 0.8018 0.109 Uiso 1 1 calc R U . . . C36 C 0.7459(5) 0.8505(3) 0.10057(17) 0.0786(12) Uani 1 1 d . . . . . H36A H 0.8141 0.9239 0.1091 0.118 Uiso 1 1 calc R U . . . H36B H 0.6305 0.8558 0.0820 0.118 Uiso 1 1 calc R U . . . H36C H 0.8015 0.8055 0.0698 0.118 Uiso 1 1 calc R U . . . C32 C 0.3464(5) 0.8140(3) 0.76498(19) 0.0794(12) Uani 1 1 d . . . . . H32A H 0.3289 0.8470 0.7243 0.119 Uiso 1 1 calc R U . . . H32B H 0.4685 0.8097 0.7736 0.119 Uiso 1 1 calc R U . . . H32C H 0.3090 0.8592 0.8009 0.119 Uiso 1 1 calc R U . . . O2 O 0.3047(3) 0.53824(18) 0.04610(10) 0.0639(7) Uani 1 1 d . . . . . O9 O 0.6184(3) 0.28250(18) 0.60295(11) 0.0666(7) Uani 1 1 d . . . . . O10 O 0.6058(4) -0.0211(2) 0.87943(11) 0.0736(7) Uani 1 1 d . . . . . O1 O 0.1316(3) 0.41111(19) -0.02584(11) 0.0723(7) Uani 1 1 d . . . . . O12 O 0.0493(3) 0.5677(2) 0.69768(11) 0.0728(7) Uani 1 1 d . . . . . O3 O 0.2848(4) 0.2490(2) 0.32923(11) 0.0781(8) Uani 1 1 d . . . . . O7 O 0.5583(4) 0.5198(2) 0.30264(12) 0.0770(8) Uani 1 1 d . . . . . O4 O 0.8970(4) 0.9482(2) 0.22417(12) 0.0803(8) Uani 1 1 d . . . . . O11 O 0.7766(4) 0.1023(2) 0.95196(13) 0.0970(10) Uani 1 1 d . . . . . O8 O 0.7583(4) 0.6642(2) 0.33024(13) 0.0928(9) Uani 1 1 d . . . . . O6 O 0.2373(5) -0.1517(2) 0.59422(13) 0.1051(11) Uani 1 1 d . . . . . O5 O 0.3581(5) 0.0142(3) 0.63009(14) 0.1126(12) Uani 1 1 d . . . . . N1 N 0.1201(4) 0.1568(2) 0.23657(12) 0.0580(8) Uani 1 1 d . . . . . H1 H 0.0514 0.0950 0.2234 0.070 Uiso 1 1 calc R U . . . N4 N 0.8115(4) 0.3609(2) 0.69187(13) 0.0601(8) Uani 1 1 d . . . . . H4A H 0.8927 0.4173 0.7038 0.072 Uiso 1 1 calc R U . . . N7 N 0.7331(4) 0.7994(2) 0.16242(12) 0.0536(7) Uani 1 1 d . . . . . N6 N 0.2439(4) 0.7016(2) 0.75914(13) 0.0555(7) Uani 1 1 d . . . . . N2 N 0.1364(4) 0.0716(2) 0.33111(12) 0.0598(8) Uani 1 1 d . . . . . H2 H 0.0651 0.0205 0.3066 0.072 Uiso 1 1 calc R U . . . N5 N 0.7986(4) 0.4494(2) 0.59849(13) 0.0587(8) Uani 1 1 d . . . . . H5A H 0.8759 0.4975 0.6226 0.070 Uiso 1 1 calc R U . . . N3 N 0.2864(4) -0.0544(3) 0.58580(15) 0.0717(9) Uani 1 1 d . . . . . N8 N 0.6679(4) 0.5773(3) 0.34300(14) 0.0621(8) Uani 1 1 d . . . . . C1 C 0.3290(5) 0.6109(3) -0.00604(17) 0.0782(12) Uani 1 1 d . . . . . H1A H 0.3823 0.5748 -0.0416 0.117 Uiso 1 1 calc R U . . . H1B H 0.4037 0.6794 0.0113 0.117 Uiso 1 1 calc R U . . . H1C H 0.2173 0.6270 -0.0225 0.117 Uiso 1 1 calc R U . . . C16 C 0.5693(7) -0.0958(3) 0.9313(2) 0.1041(16) Uani 1 1 d . . . . . H16A H 0.6707 -0.0881 0.9624 0.156 Uiso 1 1 calc R U . . . H16B H 0.5414 -0.1717 0.9114 0.156 Uiso 1 1 calc R U . . . H16C H 0.4717 -0.0765 0.9541 0.156 Uiso 1 1 calc R U . . . 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 C5 0.064(2) 0.0467(19) 0.046(2) 0.0018(16) -0.0034(16) -0.0036(16) C8 0.054(2) 0.0470(19) 0.054(2) 0.0094(16) -0.0019(16) -0.0009(15) C2 0.050(2) 0.056(2) 0.049(2) 0.0063(17) 0.0037(16) 0.0092(16) C7 0.053(2) 0.055(2) 0.0452(19) 0.0080(16) -0.0052(15) 0.0008(16) C28 0.048(2) 0.060(2) 0.0421(19) 0.0115(16) 0.0060(15) 0.0084(16) C3 0.049(2) 0.052(2) 0.0425(19) 0.0091(15) 0.0006(15) 0.0046(15) C13 0.060(2) 0.056(2) 0.048(2) 0.0159(17) 0.0033(16) 0.0051(17) C6 0.051(2) 0.049(2) 0.0468(19) 0.0097(16) 0.0040(15) 0.0021(15) C25 0.048(2) 0.051(2) 0.0453(19) 0.0095(16) 0.0026(15) 0.0037(15) C18 0.051(2) 0.053(2) 0.047(2) 0.0074(16) 0.0012(15) 0.0078(16) C19 0.061(2) 0.0481(19) 0.049(2) 0.0074(16) 0.0004(16) -0.0017(16) C20 0.060(2) 0.055(2) 0.046(2) 0.0043(16) -0.0033(16) 0.0003(17) C15 0.066(2) 0.047(2) 0.053(2) 0.0096(17) -0.0009(17) -0.0036(16) C33 0.058(2) 0.065(2) 0.050(2) 0.0123(18) 0.0046(17) 0.0026(18) C24 0.049(2) 0.054(2) 0.052(2) 0.0093(17) 0.0012(16) 0.0043(17) C21 0.046(2) 0.055(2) 0.049(2) 0.0117(16) 0.0014(15) 0.0050(15) C26 0.057(2) 0.049(2) 0.053(2) 0.0081(16) 0.0065(16) 0.0000(16) C4 0.061(2) 0.056(2) 0.0414(19) 0.0042(16) -0.0018(15) 0.0014(17) C29 0.066(2) 0.052(2) 0.058(2) 0.0158(17) 0.0030(18) -0.0040(17) C11 0.071(3) 0.046(2) 0.051(2) 0.0004(16) 0.0017(17) -0.0015(17) C34 0.065(2) 0.056(2) 0.057(2) 0.0055(18) -0.0020(18) -0.0006(18) C22 0.053(2) 0.053(2) 0.056(2) 0.0075(17) -0.0063(16) -0.0004(16) C27 0.058(2) 0.054(2) 0.049(2) 0.0044(16) 0.0038(16) 0.0020(16) C23 0.053(2) 0.060(2) 0.049(2) 0.0044(17) -0.0047(16) 0.0026(17) C10 0.057(2) 0.0463(19) 0.0446(19) 0.0072(15) 0.0040(15) 0.0029(15) C12 0.067(2) 0.048(2) 0.056(2) 0.0129(17) 0.0077(17) -0.0002(17) C17 0.060(2) 0.056(2) 0.050(2) 0.0054(18) 0.0014(17) 0.0017(17) C9 0.058(2) 0.056(2) 0.051(2) 0.0092(17) 0.0003(17) 0.0022(17) C14 0.061(2) 0.058(2) 0.051(2) 0.0066(17) -0.0041(16) -0.0037(17) C35 0.073(3) 0.057(2) 0.071(2) 0.0027(19) -0.0015(19) -0.0104(19) C30 0.065(3) 0.054(2) 0.056(2) 0.0074(17) -0.0015(17) -0.0060(17) C31 0.081(3) 0.079(3) 0.058(2) 0.018(2) -0.0005(19) 0.011(2) C36 0.091(3) 0.085(3) 0.059(2) 0.023(2) -0.001(2) 0.008(2) C32 0.081(3) 0.062(2) 0.086(3) 0.008(2) -0.003(2) -0.013(2) O2 0.0770(18) 0.0589(15) 0.0513(14) 0.0191(12) -0.0064(12) -0.0057(12) O9 0.0757(18) 0.0592(15) 0.0569(15) 0.0120(12) -0.0105(12) -0.0108(13) O10 0.096(2) 0.0642(16) 0.0560(15) 0.0210(12) -0.0031(13) -0.0053(14) O1 0.092(2) 0.0719(17) 0.0469(15) 0.0076(12) -0.0070(13) -0.0029(13) O12 0.0747(18) 0.0656(16) 0.0680(16) 0.0065(13) -0.0043(13) -0.0159(14) O3 0.099(2) 0.0634(16) 0.0587(16) 0.0150(13) -0.0175(14) -0.0227(14) O7 0.086(2) 0.0902(19) 0.0502(15) 0.0104(13) -0.0100(14) 0.0033(15) O4 0.090(2) 0.0569(16) 0.0825(18) 0.0034(13) -0.0054(14) -0.0168(14) O11 0.124(3) 0.096(2) 0.0567(17) 0.0154(15) -0.0163(16) -0.0210(18) O8 0.108(2) 0.090(2) 0.0758(19) 0.0397(16) 0.0018(16) -0.0146(17) O6 0.163(3) 0.075(2) 0.0734(19) 0.0359(16) -0.0037(18) -0.0057(19) O5 0.153(3) 0.105(2) 0.0604(18) 0.0215(17) -0.0299(18) -0.030(2) N1 0.069(2) 0.0495(16) 0.0488(17) 0.0092(13) -0.0067(14) -0.0079(14) N4 0.0577(19) 0.0640(18) 0.0522(17) 0.0168(14) -0.0077(14) -0.0107(14) N7 0.0585(19) 0.0514(16) 0.0469(16) 0.0066(13) -0.0022(13) -0.0011(13) N6 0.0579(19) 0.0528(17) 0.0529(17) 0.0111(14) -0.0014(14) -0.0013(13) N2 0.077(2) 0.0487(17) 0.0471(17) 0.0088(13) -0.0037(14) -0.0097(14) N5 0.062(2) 0.0569(18) 0.0511(17) 0.0130(14) -0.0059(13) -0.0100(14) N3 0.083(2) 0.074(2) 0.056(2) 0.0214(18) -0.0020(17) 0.0010(18) N8 0.064(2) 0.070(2) 0.0559(19) 0.0168(16) 0.0083(16) 0.0120(16) C1 0.093(3) 0.077(3) 0.064(2) 0.031(2) 0.000(2) -0.001(2) C16 0.134(5) 0.092(3) 0.085(3) 0.036(3) 0.012(3) -0.001(3) _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 C5 C4 1.372(4) . ? C5 C6 1.398(4) . ? C8 C7 1.388(4) . ? C8 C3 1.389(4) . ? C2 O1 1.214(3) . ? C2 O2 1.338(4) . ? C2 C3 1.477(4) . ? C7 C6 1.389(4) . ? C28 C27 1.373(4) . ? C28 C29 1.381(4) . ? C28 N8 1.462(4) . ? C3 C4 1.394(4) . ? C13 C12 1.379(4) . ? C13 C14 1.380(4) . ? C13 N3 1.462(4) . ? C6 N1 1.396(4) . ? C25 C26 1.389(4) . ? C25 N5 1.395(4) . ? C25 C30 1.400(4) . ? C18 C23 1.389(4) . ? C18 C19 1.392(4) . ? C18 C17 1.468(4) . ? C19 C20 1.383(4) . ? C20 C21 1.393(4) . ? C15 C14 1.386(4) . ? C15 C10 1.394(4) . ? C33 O12 1.231(4) . ? C33 N6 1.313(4) . ? C24 O9 1.212(3) . ? C24 N5 1.371(4) . ? C24 N4 1.383(4) . ? C21 C22 1.396(4) . ? C21 N4 1.397(4) . ? C26 C27 1.385(4) . ? C29 C30 1.369(4) . ? C11 C12 1.372(4) . ? C11 C10 1.391(4) . ? C34 O4 1.231(4) . ? C34 N7 1.313(4) . ? C22 C23 1.371(4) . ? C10 N2 1.396(4) . ? C17 O11 1.207(4) . ? C17 O10 1.320(4) . ? C9 O3 1.210(4) . ? C9 N2 1.371(4) . ? C9 N1 1.380(4) . ? C35 N7 1.458(4) . ? C31 N6 1.459(4) . ? C36 N7 1.451(4) . ? C32 N6 1.463(4) . ? O2 C1 1.443(4) . ? O10 C16 1.465(4) . ? O7 N8 1.223(3) . ? O8 N8 1.233(3) . ? O6 N3 1.218(3) . ? O5 N3 1.210(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 C5 C6 121.1(3) . . ? C7 C8 C3 121.6(3) . . ? O1 C2 O2 122.3(3) . . ? O1 C2 C3 124.4(3) . . ? O2 C2 C3 113.3(3) . . ? C8 C7 C6 119.4(3) . . ? C27 C28 C29 121.5(3) . . ? C27 C28 N8 119.9(3) . . ? C29 C28 N8 118.6(3) . . ? C8 C3 C4 118.5(3) . . ? C8 C3 C2 122.8(3) . . ? C4 C3 C2 118.7(3) . . ? C12 C13 C14 121.3(3) . . ? C12 C13 N3 118.7(3) . . ? C14 C13 N3 120.0(3) . . ? C7 C6 N1 124.5(3) . . ? C7 C6 C5 119.0(3) . . ? N1 C6 C5 116.5(3) . . ? C26 C25 N5 124.7(3) . . ? C26 C25 C30 118.9(3) . . ? N5 C25 C30 116.3(3) . . ? C23 C18 C19 118.5(3) . . ? C23 C18 C17 119.0(3) . . ? C19 C18 C17 122.5(3) . . ? C20 C19 C18 121.4(3) . . ? C19 C20 C21 119.7(3) . . ? C14 C15 C10 120.0(3) . . ? O12 C33 N6 125.0(3) . . ? O9 C24 N5 125.0(3) . . ? O9 C24 N4 124.3(3) . . ? N5 C24 N4 110.6(3) . . ? C20 C21 C22 118.7(3) . . ? C20 C21 N4 124.6(3) . . ? C22 C21 N4 116.7(3) . . ? C27 C26 C25 120.0(3) . . ? C5 C4 C3 120.3(3) . . ? C30 C29 C28 118.9(3) . . ? C12 C11 C10 120.8(3) . . ? O4 C34 N7 125.5(3) . . ? C23 C22 C21 121.2(3) . . ? C28 C27 C26 119.6(3) . . ? C22 C23 C18 120.5(3) . . ? C11 C10 C15 119.2(3) . . ? C11 C10 N2 116.5(3) . . ? C15 C10 N2 124.3(3) . . ? C11 C12 C13 119.3(3) . . ? O11 C17 O10 121.9(3) . . ? O11 C17 C18 124.2(3) . . ? O10 C17 C18 113.9(3) . . ? O3 C9 N2 124.8(3) . . ? O3 C9 N1 124.4(3) . . ? N2 C9 N1 110.8(3) . . ? C13 C14 C15 119.3(3) . . ? C29 C30 C25 121.0(3) . . ? C2 O2 C1 116.7(2) . . ? C17 O10 C16 118.2(3) . . ? C9 N1 C6 129.3(3) . . ? C24 N4 C21 128.9(3) . . ? C34 N7 C36 120.3(3) . . ? C34 N7 C35 121.7(3) . . ? C36 N7 C35 117.9(3) . . ? C33 N6 C31 119.8(3) . . ? C33 N6 C32 121.6(3) . . ? C31 N6 C32 118.6(3) . . ? C9 N2 C10 129.1(3) . . ? C24 N5 C25 128.5(3) . . ? O5 N3 O6 122.7(3) . . ? O5 N3 C13 119.0(3) . . ? O6 N3 C13 118.3(3) . . ? O7 N8 O8 123.0(3) . . ? O7 N8 C28 119.3(3) . . ? O8 N8 C28 117.7(3) . . ? _refine_diff_density_max 0.227 _refine_diff_density_min -0.270 _refine_diff_density_rms 0.068 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 7.7434 12.1722 20.2617 95.227 93.915 98.882 ZERR 4.00 0.0003 0.0005 0.0007 0.003 0.002 0.002 LATT 1 SFAC C H N O UNIT 72 80 16 24 OMIT -3 50.1 L.S. 10 ACTA BOND FMAP 2 PLAN 1 TEMP 23.000 WGHT 0.010000 1.500000 FVAR 0.23034 MOLE 1 C5 1 0.062254 0.197056 0.125442 11.00000 0.06418 0.04668 = 0.04614 0.00177 -0.00338 -0.00361 AFIX 43 H5 2 -0.005634 0.126457 0.117281 11.00000 -1.20000 AFIX 0 C8 1 0.261279 0.406360 0.149488 11.00000 0.05351 0.04698 = 0.05355 0.00943 -0.00192 -0.00090 AFIX 43 H8 2 0.328160 0.477277 0.157630 11.00000 -1.20000 AFIX 0 C2 1 0.200477 0.439724 0.029964 11.00000 0.04983 0.05605 = 0.04933 0.00626 0.00370 0.00916 C7 1 0.243902 0.338694 0.200953 11.00000 0.05306 0.05486 = 0.04525 0.00795 -0.00515 0.00075 AFIX 43 H7 2 0.298106 0.364235 0.243113 11.00000 -1.20000 AFIX 0 C28 1 0.696768 0.541845 0.409324 11.00000 0.04840 0.06010 = 0.04213 0.01150 0.00600 0.00841 C3 1 0.181148 0.370694 0.086088 11.00000 0.04895 0.05184 = 0.04245 0.00913 0.00065 0.00462 C13 1 0.253735 -0.019301 0.519583 11.00000 0.06026 0.05559 = 0.04760 0.01590 0.00327 0.00515 C6 1 0.144860 0.232475 0.188977 11.00000 0.05139 0.04917 = 0.04682 0.00967 0.00404 0.00207 C25 1 0.757237 0.475489 0.534294 11.00000 0.04848 0.05058 = 0.04530 0.00954 0.00261 0.00374 C18 1 0.732194 0.145927 0.841211 11.00000 0.05142 0.05334 = 0.04722 0.00744 0.00123 0.00782 C19 1 0.644924 0.114910 0.778366 11.00000 0.06113 0.04806 = 0.04944 0.00740 0.00041 -0.00173 AFIX 43 H19 2 0.570725 0.046510 0.770187 11.00000 -1.20000 AFIX 0 C20 1 0.666194 0.183648 0.727812 11.00000 0.06014 0.05476 = 0.04617 0.00430 -0.00327 0.00034 AFIX 43 H20 2 0.606256 0.161615 0.686208 11.00000 -1.20000 AFIX 0 C15 1 0.282790 0.120860 0.444228 11.00000 0.06572 0.04692 = 0.05346 0.00955 -0.00087 -0.00361 AFIX 43 H15 2 0.327141 0.192720 0.434907 11.00000 -1.20000 AFIX 0 C33 1 0.140235 0.660994 0.705663 11.00000 0.05823 0.06490 = 0.04963 0.01231 0.00460 0.00262 AFIX 43 H33 2 0.135120 0.706169 0.671185 11.00000 -1.20000 AFIX 0 C24 1 0.732292 0.356936 0.628234 11.00000 0.04913 0.05436 = 0.05186 0.00928 0.00120 0.00432 C21 1 0.777751 0.286012 0.739459 11.00000 0.04565 0.05458 = 0.04883 0.01175 0.00140 0.00500 C26 1 0.653271 0.403187 0.485054 11.00000 0.05688 0.04871 = 0.05315 0.00811 0.00648 0.00005 AFIX 43 H26 2 0.604789 0.331880 0.494035 11.00000 -1.20000 AFIX 0 C4 1 0.079647 0.264707 0.074908 11.00000 0.06096 0.05634 = 0.04138 0.00416 -0.00176 0.00137 AFIX 43 H4 2 0.023433 0.239716 0.032991 11.00000 -1.20000 AFIX 0 C29 1 0.802673 0.614671 0.457149 11.00000 0.06630 0.05183 = 0.05805 0.01583 0.00300 -0.00398 AFIX 43 H29 2 0.853406 0.685040 0.447371 11.00000 -1.20000 AFIX 0 C11 1 0.119806 -0.062072 0.409411 11.00000 0.07068 0.04595 = 0.05100 0.00042 0.00173 -0.00149 AFIX 43 H11 2 0.053700 -0.112735 0.376632 11.00000 -1.20000 AFIX 0 C34 1 0.810938 0.853448 0.218249 11.00000 0.06484 0.05639 = 0.05657 0.00553 -0.00201 -0.00060 AFIX 43 H34 2 0.800103 0.817071 0.256535 11.00000 -1.20000 AFIX 0 C22 1 0.866242 0.316371 0.802405 11.00000 0.05267 0.05263 = 0.05583 0.00748 -0.00629 -0.00042 AFIX 43 H22 2 0.942285 0.384057 0.810554 11.00000 -1.20000 AFIX 0 C27 1 0.621792 0.437266 0.422584 11.00000 0.05760 0.05396 = 0.04942 0.00444 0.00378 0.00205 AFIX 43 H27 2 0.550277 0.389582 0.389806 11.00000 -1.20000 AFIX 0 C23 1 0.843065 0.248200 0.852427 11.00000 0.05286 0.06022 = 0.04937 0.00441 -0.00471 0.00262 AFIX 43 H23 2 0.902000 0.270590 0.894174 11.00000 -1.20000 AFIX 0 C10 1 0.181179 0.046050 0.395178 11.00000 0.05734 0.04635 = 0.04461 0.00718 0.00404 0.00294 C12 1 0.155643 -0.094858 0.471236 11.00000 0.06671 0.04849 = 0.05597 0.01291 0.00771 -0.00024 AFIX 43 H12 2 0.114213 -0.167256 0.480423 11.00000 -1.20000 AFIX 0 C17 1 0.709550 0.075583 0.896105 11.00000 0.05968 0.05550 = 0.05033 0.00540 0.00137 0.00171 C9 1 0.190005 0.166827 0.301758 11.00000 0.05758 0.05593 = 0.05061 0.00916 0.00028 0.00225 C14 1 0.317765 0.088216 0.506882 11.00000 0.06140 0.05846 = 0.05093 0.00661 -0.00409 -0.00370 AFIX 43 H14 2 0.383697 0.138260 0.540009 11.00000 -1.20000 AFIX 0 C35 1 0.635716 0.686413 0.159934 11.00000 0.07325 0.05731 = 0.07064 0.00270 -0.00147 -0.01039 AFIX 137 H35A 2 0.637654 0.662703 0.203851 11.00000 -1.50000 H35B 2 0.688830 0.636547 0.131215 11.00000 -1.50000 H35C 2 0.516533 0.685570 0.143101 11.00000 -1.50000 AFIX 0 C30 1 0.831748 0.581572 0.519189 11.00000 0.06494 0.05354 = 0.05590 0.00740 -0.00150 -0.00596 AFIX 43 H30 2 0.902085 0.630318 0.551799 11.00000 -1.20000 AFIX 0 C31 1 0.257303 0.634140 0.814651 11.00000 0.08149 0.07854 = 0.05818 0.01795 -0.00051 0.01092 AFIX 137 H31A 2 0.206442 0.666948 0.852004 11.00000 -1.50000 H31B 2 0.378520 0.631363 0.826674 11.00000 -1.50000 H31C 2 0.195793 0.559743 0.801806 11.00000 -1.50000 AFIX 0 C36 1 0.745868 0.850503 0.100567 11.00000 0.09091 0.08544 = 0.05922 0.02288 -0.00074 0.00756 AFIX 137 H36A 2 0.814120 0.923940 0.109051 11.00000 -1.50000 H36B 2 0.630451 0.855846 0.081953 11.00000 -1.50000 H36C 2 0.801470 0.805503 0.069787 11.00000 -1.50000 AFIX 0 C32 1 0.346388 0.814032 0.764977 11.00000 0.08132 0.06161 = 0.08629 0.00786 -0.00256 -0.01251 AFIX 137 H32A 2 0.328940 0.846996 0.724263 11.00000 -1.50000 H32B 2 0.468508 0.809744 0.773557 11.00000 -1.50000 H32C 2 0.308989 0.859156 0.800943 11.00000 -1.50000 AFIX 0 O2 4 0.304693 0.538240 0.046096 11.00000 0.07696 0.05892 = 0.05131 0.01912 -0.00639 -0.00570 O9 4 0.618353 0.282498 0.602952 11.00000 0.07572 0.05924 = 0.05692 0.01205 -0.01052 -0.01079 O10 4 0.605768 -0.021112 0.879425 11.00000 0.09613 0.06417 = 0.05598 0.02102 -0.00308 -0.00535 O1 4 0.131645 0.411109 -0.025842 11.00000 0.09157 0.07191 = 0.04689 0.00764 -0.00697 -0.00292 O12 4 0.049332 0.567729 0.697680 11.00000 0.07468 0.06564 = 0.06798 0.00650 -0.00425 -0.01594 O3 4 0.284762 0.249011 0.329234 11.00000 0.09890 0.06342 = 0.05875 0.01505 -0.01747 -0.02270 O7 4 0.558258 0.519837 0.302636 11.00000 0.08558 0.09020 = 0.05024 0.01036 -0.01003 0.00331 O4 4 0.897040 0.948197 0.224169 11.00000 0.08997 0.05689 = 0.08254 0.00342 -0.00536 -0.01682 O11 4 0.776574 0.102272 0.951958 11.00000 0.12410 0.09592 = 0.05668 0.01537 -0.01630 -0.02103 O8 4 0.758275 0.664192 0.330245 11.00000 0.10821 0.08966 = 0.07576 0.03970 0.00176 -0.01460 O6 4 0.237337 -0.151737 0.594218 11.00000 0.16261 0.07460 = 0.07344 0.03586 -0.00371 -0.00574 O5 4 0.358142 0.014219 0.630093 11.00000 0.15268 0.10525 = 0.06037 0.02149 -0.02985 -0.03039 N1 3 0.120068 0.156780 0.236566 11.00000 0.06934 0.04947 = 0.04883 0.00922 -0.00669 -0.00791 AFIX 43 H1 2 0.051384 0.095038 0.223386 11.00000 -1.20000 AFIX 0 N4 3 0.811498 0.360934 0.691872 11.00000 0.05774 0.06397 = 0.05223 0.01680 -0.00766 -0.01074 AFIX 43 H4A 2 0.892661 0.417280 0.703777 11.00000 -1.20000 AFIX 0 N7 3 0.733112 0.799432 0.162420 11.00000 0.05850 0.05138 = 0.04695 0.00658 -0.00221 -0.00111 N6 3 0.243860 0.701558 0.759137 11.00000 0.05794 0.05279 = 0.05286 0.01109 -0.00141 -0.00126 N2 3 0.136383 0.071647 0.331105 11.00000 0.07676 0.04869 = 0.04709 0.00882 -0.00372 -0.00969 AFIX 43 H2 2 0.065079 0.020482 0.306580 11.00000 -1.20000 AFIX 0 N5 3 0.798613 0.449358 0.598491 11.00000 0.06170 0.05695 = 0.05109 0.01295 -0.00587 -0.00998 AFIX 43 H5A 2 0.875862 0.497542 0.622576 11.00000 -1.20000 AFIX 0 N3 3 0.286447 -0.054404 0.585796 11.00000 0.08282 0.07395 = 0.05625 0.02138 -0.00202 0.00101 N8 3 0.667942 0.577270 0.342998 11.00000 0.06366 0.06968 = 0.05587 0.01679 0.00828 0.01204 C1 1 0.329035 0.610949 -0.006044 11.00000 0.09298 0.07694 = 0.06353 0.03099 0.00025 -0.00092 AFIX 137 H1A 2 0.382276 0.574842 -0.041623 11.00000 -1.50000 H1B 2 0.403678 0.679395 0.011267 11.00000 -1.50000 H1C 2 0.217350 0.626995 -0.022475 11.00000 -1.50000 AFIX 0 C16 1 0.569267 -0.095785 0.931307 11.00000 0.13441 0.09178 = 0.08508 0.03563 0.01177 -0.00135 AFIX 137 H16A 2 0.670688 -0.088109 0.962407 11.00000 -1.50000 H16B 2 0.541446 -0.171692 0.911397 11.00000 -1.50000 H16C 2 0.471749 -0.076484 0.954114 11.00000 -1.50000 AFIX 0 HKLF 4 REM 1 in P-1 REM R1 = 0.0532 for 3582 Fo > 4sig(Fo) and 0.1107 for all 6504 data REM 511 parameters refined using 0 restraints END WGHT 0.0933 0.0455 REM Highest difference peak 0.227, deepest hole -0.270, 1-sigma level 0.068 Q1 1 0.9040 0.8758 0.0872 11.00000 0.05 0.23 ; _shelx_res_checksum 30293 _shelx_hkl_file ; 5 0 0 1.50 0.59 6 0 0 0.57 0.63 -6 0 0 0.21 0.56 -7 0 0 0.06 0.57 7 0 0 0.51 0.74 7 -1 0 3.80 0.97 -7 1 0 3.56 0.90 6 -1 0 2.22 0.72 5 -1 0 0.99 0.54 -1 1 0 0.12 0.05 -1 1 0 0.00 0.05 0 1 0 7.62 0.40 0 -1 0 7.04 0.40 0 -1 0 7.48 0.41 0 -1 0 5.29 0.41 1 1 0 0.15 0.06 -1 -1 0 0.12 0.05 1 1 0 0.23 0.06 -1 -1 0 0.20 0.05 -4 -1 0 12.73 1.11 -5 -1 0 20.26 1.61 -6 -1 0 0.51 0.56 6 1 0 -0.18 0.55 7 1 0 -0.19 0.63 -7 -1 0 1.20 0.70 8 1 0 0.22 0.74 7 -2 0 0.09 0.66 6 -2 0 -0.18 0.48 5 -2 0 0.15 0.40 -2 2 0 25.45 1.35 -2 2 0 24.78 1.35 -2 2 0 24.53 1.29 -2 2 0 23.72 1.28 1 -2 0 14.07 0.79 -1 2 0 14.77 0.80 1 -2 0 13.34 0.83 1 -2 0 13.80 0.82 -1 2 0 13.21 0.79 0 -2 0 63.42 3.81 0 2 0 79.31 3.83 0 -2 0 79.71 3.74 0 2 0 75.37 3.72 0 -2 0 74.67 3.80 1 2 0 69.61 3.57 1 2 0 69.99 3.58 -1 -2 0 69.38 3.49 1 2 0 67.35 3.30 -1 -2 0 70.05 3.50 1 2 0 69.79 3.47 -1 -2 0 70.33 3.55 -2 -2 0 4.05 0.30 2 2 0 3.60 0.30 -2 -2 0 3.76 0.30 2 2 0 4.23 0.31 2 2 0 3.86 0.30 3 2 0 20.08 1.06 3 2 0 19.15 1.05 -4 -2 0 2.90 0.57 4 2 0 3.40 0.67 -5 -2 0 0.02 0.42 5 2 0 0.96 0.55 -6 -2 0 0.13 0.52 6 2 0 0.53 0.59 -7 -2 0 1.59 0.70 7 2 0 -0.13 0.53 8 2 0 3.37 1.12 -8 -2 0 1.14 0.85 8 2 0 1.92 0.36 7 -3 0 0.08 0.64 6 -3 0 2.19 0.68 5 -3 0 2.01 0.59 -4 3 0 84.93 4.18 -4 3 0 83.42 4.18 -3 3 0 0.24 0.15 -3 3 0 0.21 0.18 3 -3 0 0.00 0.15 -3 3 0 0.25 0.13 2 -3 0 7.15 0.45 2 -3 0 5.47 0.52 -2 3 0 6.52 0.51 2 -3 0 6.71 0.44 2 -3 0 6.49 0.42 -2 3 0 6.63 0.57 2 -3 0 6.91 0.54 -1 3 0 2.75 0.35 1 -3 0 2.30 0.33 1 -3 0 3.15 0.32 -1 3 0 2.52 0.31 1 -3 0 2.30 0.32 0 3 0 2.54 0.35 0 3 0 3.04 0.33 0 -3 0 2.56 0.34 0 -3 0 2.30 0.30 -1 -3 0 2.52 0.32 -1 -3 0 1.85 0.29 1 3 0 2.44 0.29 -1 -3 0 1.58 0.25 1 3 0 1.15 0.24 1 3 0 2.01 0.30 1 3 0 1.29 0.24 -2 -3 0 23.25 1.33 2 3 0 23.79 1.17 2 3 0 24.28 1.36 2 3 0 22.22 1.35 -2 -3 0 24.04 1.33 3 3 0 45.23 2.17 3 3 0 45.25 2.40 -3 -3 0 43.27 2.34 -3 -3 0 43.78 2.63 3 3 0 44.82 2.38 3 3 0 44.46 2.18 -3 -3 0 43.93 2.33 3 3 0 47.06 2.73 -4 -3 0 19.21 1.35 -4 -3 0 14.58 0.94 4 3 0 15.18 0.97 -4 -3 0 16.81 0.95 4 3 0 15.97 0.99 4 3 0 15.12 1.39 5 3 0 25.28 1.46 5 3 0 27.92 2.05 -5 -3 0 22.76 1.82 -5 -3 0 25.64 1.41 -6 -3 0 0.10 0.21 6 3 0 0.51 0.62 -6 -3 0 -0.06 0.49 6 3 0 0.14 0.25 -7 -3 0 0.04 0.64 7 3 0 0.12 0.68 7 3 0 0.46 0.32 -7 -3 0 0.15 0.25 -8 -3 0 3.67 1.07 8 3 0 2.13 1.00 -8 -3 0 2.66 0.46 -9 4 0 0.39 0.38 -8 4 0 0.90 0.34 -7 4 0 0.13 0.24 -6 4 0 0.74 0.27 6 -4 0 1.19 0.65 -5 4 0 1.68 0.30 -5 4 0 1.54 0.27 5 -4 0 0.61 0.52 -4 4 0 2.14 0.32 -4 4 0 1.81 0.32 -4 4 0 1.22 0.34 4 -4 0 2.97 0.28 4 -4 0 2.46 0.27 3 -4 0 62.91 2.93 -3 4 0 62.82 3.26 3 -4 0 60.69 2.93 -3 4 0 59.67 3.23 3 -4 0 63.65 3.33 3 -4 0 62.33 3.09 2 -4 0 6.39 0.53 -2 4 0 7.01 0.59 -2 4 0 5.53 0.59 2 -4 0 6.67 0.52 2 -4 0 8.47 0.67 2 -4 0 6.45 0.57 2 -4 0 6.06 0.59 1 -4 0 121.46 6.28 1 -4 0 123.76 6.45 -1 4 0 125.57 6.30 1 -4 0 127.10 5.98 -1 4 0 128.64 6.47 0 -4 0 201.28 9.32 0 4 0 197.86 9.30 0 4 0 193.38 10.03 0 -4 0 195.98 9.80 0 -4 0 196.20 10.00 0 4 0 204.58 9.80 1 4 0 2.44 0.41 1 4 0 2.62 0.35 -1 -4 0 1.95 0.31 1 4 0 1.35 0.28 -1 -4 0 1.33 0.33 -2 -4 0 358.91 17.80 2 4 0 357.09 16.36 2 4 0 361.90 17.90 -2 -4 0 353.17 17.30 -2 -4 0 359.39 17.32 2 4 0 361.30 17.69 -2 -4 0 337.37 17.58 2 4 0 349.54 17.70 3 4 0 1.34 0.49 -3 -4 0 1.14 0.32 -3 -4 0 0.80 0.28 3 4 0 1.19 0.27 -3 -4 0 1.51 0.43 3 4 0 1.38 0.31 3 4 0 1.31 0.30 -4 -4 0 28.23 1.61 -4 -4 0 27.25 1.91 4 4 0 27.12 1.64 4 4 0 25.66 1.98 5 4 0 -0.25 0.23 -5 -4 0 0.07 0.25 -5 -4 0 -0.42 0.45 5 4 0 0.35 0.52 -6 -4 0 14.37 1.06 -6 -4 0 16.15 1.61 6 4 0 16.00 1.13 6 4 0 14.71 1.67 7 4 0 -0.50 0.65 -7 -4 0 0.38 0.69 -7 -4 0 0.31 0.34 7 4 0 -0.01 0.36 8 4 0 1.38 0.95 -8 -4 0 2.83 1.03 -8 -4 0 0.70 0.43 -9 5 0 0.04 0.41 -8 5 0 -0.05 0.36 -7 5 0 -0.38 0.28 6 -5 0 0.22 0.59 -6 5 0 0.06 0.27 -5 5 0 0.83 0.31 5 -5 0 2.77 0.64 4 -5 0 -0.01 0.23 4 -5 0 -0.06 0.30 4 -5 0 -0.03 0.34 -4 5 0 -0.09 0.19 -3 5 0 25.23 1.57 3 -5 0 26.67 1.48 3 -5 0 25.90 1.65 3 -5 0 26.86 1.42 -3 5 0 25.53 1.61 3 -5 0 25.10 1.52 -2 5 0 0.65 0.27 2 -5 0 0.28 0.30 2 -5 0 0.84 0.33 2 -5 0 1.34 0.31 2 -5 0 0.44 0.23 2 -5 0 1.55 0.36 -1 5 0 11.51 0.87 1 -5 0 10.83 0.87 -1 5 0 10.70 0.92 -1 5 0 10.81 0.86 1 -5 0 10.42 0.91 1 -5 0 11.74 0.82 0 -5 0 1.80 0.40 0 5 0 3.16 0.45 0 5 0 2.42 0.45 0 5 0 2.28 0.41 0 -5 0 2.31 0.40 0 -5 0 1.01 0.31 1 5 0 0.62 0.26 -1 -5 0 0.35 0.27 1 5 0 0.71 0.31 -1 -5 0 0.16 0.25 -1 -5 0 0.55 0.24 1 5 0 0.23 0.23 -2 -5 0 0.50 0.23 -2 -5 0 0.82 0.35 2 5 0 1.00 0.26 -2 -5 0 0.13 0.25 2 5 0 0.55 0.30 2 5 0 0.49 0.29 2 5 0 0.22 0.41 3 5 0 0.93 0.17 3 5 0 1.28 0.53 -3 -5 0 0.42 0.36 -3 -5 0 1.19 0.36 3 5 0 0.70 0.17 3 5 0 0.70 0.29 3 5 0 0.60 0.30 -4 -5 0 6.05 0.89 4 5 0 5.59 0.48 4 5 0 3.96 0.79 4 5 0 5.31 0.47 4 5 0 3.79 0.57 -4 -5 0 3.61 0.54 5 5 0 3.10 0.55 -5 -5 0 4.53 0.60 -5 -5 0 6.86 1.04 5 5 0 4.51 0.94 6 5 0 11.39 1.53 -6 -5 0 10.64 1.39 6 5 0 10.96 1.02 -6 -5 0 11.48 0.97 7 5 0 0.85 0.54 7 5 0 -0.26 0.69 -7 -5 0 0.99 0.46 -7 -5 0 0.51 0.77 8 5 0 1.73 1.00 -8 -5 0 0.85 0.84 -8 -5 0 0.13 0.44 -8 6 0 0.74 0.49 -7 6 0 0.74 0.39 6 -6 0 -0.46 0.52 -6 6 0 -0.07 0.31 -5 6 0 1.31 0.40 5 -6 0 3.03 0.71 5 -6 0 2.54 0.38 -4 6 0 2.51 0.49 4 -6 0 2.61 0.45 4 -6 0 1.81 0.53 4 -6 0 1.58 0.25 4 -6 0 1.60 0.27 3 -6 0 -0.03 0.24 3 -6 0 0.04 0.20 -3 6 0 0.37 0.28 3 -6 0 0.64 0.39 3 -6 0 0.06 0.29 3 -6 0 0.24 0.23 2 -6 0 5.91 0.73 -2 6 0 6.15 0.69 -2 6 0 7.18 0.76 2 -6 0 7.10 0.65 2 -6 0 6.13 0.71 2 -6 0 6.74 0.72 2 -6 0 6.85 0.69 1 -6 0 7.21 0.71 -1 6 0 5.44 0.68 -1 6 0 7.50 0.78 1 -6 0 7.22 0.74 -1 6 0 7.43 0.73 1 -6 0 5.48 0.63 1 -6 0 7.93 0.83 1 -6 0 4.60 0.64 0 -6 0 4.85 0.65 0 6 0 6.15 0.74 0 -6 0 5.22 0.64 0 -6 0 6.07 0.67 0 -6 0 5.49 0.63 0 6 0 4.15 0.60 0 6 0 5.73 0.67 -1 -6 0 133.36 7.00 1 6 0 139.00 6.96 1 6 0 138.80 6.61 -1 -6 0 136.28 6.69 -1 -6 0 140.25 7.10 1 6 0 135.67 7.17 -1 -6 0 133.49 7.14 2 6 0 35.69 1.94 -2 -6 0 34.79 2.16 2 6 0 37.88 2.25 -2 -6 0 35.26 2.26 3 6 0 0.18 0.33 3 6 0 -0.07 0.19 3 6 0 -0.03 0.43 -3 -6 0 -0.14 0.33 -3 -6 0 0.20 0.33 -4 -6 0 21.15 1.47 4 6 0 21.84 1.31 4 6 0 21.35 1.88 -4 -6 0 20.64 1.74 4 6 0 20.36 1.51 -5 -6 0 1.48 0.42 -5 -6 0 0.67 0.60 5 6 0 0.46 0.61 5 6 0 0.90 0.43 6 6 0 13.50 1.23 -6 -6 0 15.67 1.65 6 6 0 10.55 1.60 -6 -6 0 12.33 1.13 -7 -6 0 0.24 0.44 -7 -6 0 -0.26 0.69 7 6 0 0.06 0.73 -8 -6 0 1.96 1.01 8 6 0 0.22 0.88 -8 7 0 -0.31 0.46 -7 7 0 0.26 0.44 6 -7 0 0.62 0.62 -6 7 0 0.79 0.42 -5 7 0 2.28 0.54 5 -7 0 2.65 0.49 5 -7 0 2.04 0.64 4 -7 0 4.98 0.77 -4 7 0 4.57 0.71 4 -7 0 4.29 0.66 4 -7 0 5.17 0.52 3 -7 0 24.47 1.59 3 -7 0 26.55 1.76 -3 7 0 32.21 1.88 2 -7 0 1.95 0.48 2 -7 0 1.57 0.39 -2 7 0 1.94 0.47 2 -7 0 1.26 0.50 2 -7 0 2.32 0.47 -2 7 0 2.78 0.58 1 -7 0 13.31 1.15 1 -7 0 11.30 0.98 -1 7 0 10.85 1.00 1 -7 0 11.42 1.00 1 -7 0 11.27 1.04 1 -7 0 9.52 0.96 -1 7 0 11.02 1.09 -1 7 0 9.97 0.98 0 -7 0 11.51 1.12 0 -7 0 13.75 1.13 0 7 0 10.87 1.11 0 -7 0 12.92 1.08 0 -7 0 10.97 1.01 0 7 0 11.18 1.02 0 7 0 9.83 0.97 0 -7 0 12.69 1.05 1 7 0 0.17 0.34 1 7 0 -0.25 0.29 -1 -7 0 0.03 0.36 -1 -7 0 0.55 0.37 -1 -7 0 -0.18 0.26 -2 -7 0 -0.18 0.32 2 7 0 -0.11 0.25 -2 -7 0 0.20 0.31 2 7 0 -0.05 0.30 3 7 0 0.30 0.25 -3 -7 0 0.32 0.44 3 7 0 -0.49 0.33 -3 -7 0 0.30 0.34 4 7 0 0.94 0.45 4 7 0 0.11 0.52 -4 -7 0 0.06 0.40 4 7 0 0.50 0.33 -4 -7 0 -0.04 0.50 -5 -7 0 10.31 1.03 5 7 0 8.35 1.04 5 7 0 8.00 0.64 5 7 0 9.76 1.44 -5 -7 0 7.98 1.23 -6 -7 0 0.87 0.55 6 7 0 3.07 0.92 -6 -7 0 2.42 0.83 -7 -7 0 1.91 0.91 7 7 0 3.02 1.09 -7 -7 0 2.11 0.70 8 7 0 -0.08 0.96 -8 -7 0 0.39 0.97 -8 8 0 -0.07 0.51 -7 8 0 0.32 0.53 6 -8 0 0.62 0.62 -6 8 0 0.15 0.42 6 -8 0 0.71 0.34 5 -8 0 1.19 0.42 -5 8 0 0.75 0.48 5 -8 0 0.61 0.56 4 -8 0 -0.03 0.27 4 -8 0 -0.08 0.35 4 -8 0 0.37 0.40 -4 8 0 -0.15 0.36 3 -8 0 -0.04 0.27 3 -8 0 0.57 0.45 -3 8 0 0.02 0.33 3 -8 0 0.44 0.40 -2 8 0 24.33 1.75 2 -8 0 29.29 1.87 -2 8 0 26.12 1.81 2 -8 0 26.17 1.67 2 -8 0 26.08 1.80 2 -8 0 25.16 1.77 1 -8 0 0.39 0.34 -1 8 0 0.39 0.39 1 -8 0 0.17 0.36 -1 8 0 0.79 0.47 1 -8 0 -0.22 0.47 -1 8 0 0.55 0.47 1 -8 0 0.35 0.47 1 -8 0 -0.29 0.33 0 -8 0 15.79 1.47 0 -8 0 16.96 1.43 0 8 0 17.22 1.32 0 8 0 15.64 1.33 0 -8 0 17.09 1.32 0 -8 0 17.60 1.37 0 -8 0 17.08 1.37 0 8 0 18.11 1.49 1 8 0 14.49 1.15 1 8 0 15.09 1.35 -1 -8 0 13.79 1.27 -1 -8 0 14.50 1.31 -2 -8 0 29.23 2.04 2 8 0 29.49 1.78 2 8 0 27.25 2.02 -2 -8 0 30.84 2.04 3 8 0 -0.10 0.29 3 8 0 -0.49 0.36 -3 -8 0 0.96 0.51 -3 -8 0 0.80 0.50 -4 -8 0 13.28 1.26 -4 -8 0 13.81 1.50 4 8 0 13.48 1.10 4 8 0 11.31 1.24 5 8 0 8.04 0.72 5 8 0 7.04 1.05 -5 -8 0 4.86 0.86 -5 -8 0 6.31 1.18 -6 -8 0 0.09 0.67 6 8 0 -0.38 0.67 -6 -8 0 -0.03 0.52 7 8 0 1.33 0.97 -7 -8 0 -0.80 0.70 -8 -8 0 0.41 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0.78 1 0 23 -0.19 0.62 2 0 23 0.70 0.76 2 0 23 0.49 0.65 3 0 23 0.89 0.80 3 0 23 0.56 0.64 4 0 23 0.19 0.75 4 0 23 0.78 0.60 5 -1 -23 1.59 0.82 5 -1 -23 1.37 1.23 5 -1 -23 0.81 0.59 4 -1 -23 -0.17 1.10 4 -1 -23 0.31 0.71 4 -1 -23 -0.25 0.57 3 -1 -23 1.42 0.88 3 -1 -23 0.20 0.75 2 -1 -23 1.19 0.87 2 -1 -23 0.16 0.72 1 -1 -23 -0.16 0.75 0 1 23 0.14 0.66 1 1 23 1.06 0.80 1 1 23 2.50 0.95 2 1 23 0.68 0.63 2 1 23 0.45 0.78 3 1 23 0.50 0.57 3 1 23 -0.26 0.75 4 1 23 0.35 0.57 4 1 23 0.66 0.75 5 -2 -23 1.05 0.76 5 -2 -23 0.97 0.63 5 -2 -23 0.32 1.11 4 -2 -23 -0.06 1.06 4 -2 -23 1.46 0.83 4 -2 -23 0.47 0.66 3 -2 -23 -0.71 0.70 3 -2 -23 1.28 1.09 3 -2 -23 -0.69 0.70 2 -2 -23 0.54 0.80 2 -2 -23 0.14 0.76 1 -2 -23 -0.37 0.73 0 2 23 0.98 0.74 1 2 23 0.45 0.80 1 2 23 -0.11 0.65 2 2 23 0.24 0.83 2 2 23 0.55 0.67 3 2 23 1.45 0.69 3 2 23 0.23 0.80 5 -3 -23 0.37 0.61 5 -3 -23 -0.60 0.67 5 -3 -23 0.48 1.11 4 -3 -23 2.37 1.29 4 -3 -23 0.15 0.64 4 -3 -23 1.04 0.81 3 -3 -23 -0.04 0.73 3 -3 -23 0.90 1.07 3 -3 -23 0.90 0.90 2 -3 -23 0.01 0.79 2 -3 -23 1.01 0.85 1 -3 -23 0.45 0.81 0 3 23 -0.10 0.68 1 3 23 -0.37 0.81 1 3 23 0.16 0.71 2 3 23 0.71 0.85 2 3 23 -0.41 0.55 3 3 23 -0.47 0.66 3 3 23 -0.39 0.55 5 -4 -23 0.14 0.66 5 -4 -23 0.19 0.79 5 -4 -23 -0.78 1.25 4 -4 -23 0.06 0.76 4 -4 -23 1.27 0.85 4 -4 -23 1.23 1.23 3 -4 -23 0.56 1.17 3 -4 -23 -0.04 0.73 3 -4 -23 -0.01 0.76 2 -4 -23 -0.33 0.76 1 -4 -23 0.01 0.88 0 4 23 0.39 0.74 1 4 23 0.72 0.86 1 4 23 -0.89 0.68 2 4 23 0.20 0.64 2 4 23 0.18 0.74 4 -5 -23 0.36 0.75 4 -5 -23 -0.21 0.75 4 -5 -23 1.65 1.34 3 -5 -23 -0.23 1.11 3 -5 -23 0.94 0.94 3 -5 -23 1.25 0.90 2 -5 -23 0.31 0.81 1 -5 -23 0.23 0.94 0 5 23 0.57 0.81 1 5 23 0.49 0.77 1 5 23 -0.26 0.90 2 5 23 0.22 0.71 2 5 23 0.20 0.87 4 -6 -23 0.20 1.21 4 -6 -23 -0.25 0.73 4 -6 -23 0.68 0.87 3 -6 -23 1.63 1.03 3 -6 -23 0.08 1.04 3 -6 -23 0.74 0.84 2 -6 -23 -0.08 0.81 1 -6 -23 0.66 0.97 0 6 23 -0.44 0.81 1 6 23 1.04 1.04 1 6 23 0.02 0.73 2 -7 -23 0.95 0.94 0 8 -24 0.73 1.14 1 -8 24 1.18 0.97 3 7 -24 -0.40 0.74 2 7 -24 1.00 0.94 2 7 -24 0.60 0.98 1 7 -24 -0.57 0.83 0 7 -24 0.06 1.09 1 -7 24 0.46 0.78 2 -7 24 0.53 0.80 2 -7 24 0.57 0.92 3 6 -24 0.24 0.82 3 6 -24 -0.34 0.78 2 6 -24 0.33 0.84 2 6 -24 1.43 0.97 1 6 -24 -1.33 0.81 0 6 -24 4.12 1.29 1 -6 24 1.21 0.84 2 -6 24 0.11 0.83 2 -6 24 1.31 0.84 3 -6 24 1.65 0.85 3 -6 24 1.09 0.89 4 5 -24 0.12 0.77 4 5 -24 1.57 0.79 3 5 -24 0.07 0.83 2 5 -24 4.63 1.20 2 5 -24 1.12 0.93 1 5 -24 0.85 1.02 0 5 -24 1.43 1.06 1 -5 24 -0.20 0.76 2 -5 24 0.92 0.86 2 -5 24 0.68 0.73 3 -5 24 0.67 0.80 3 -5 24 -0.71 0.65 4 4 -24 0.10 0.80 4 4 -24 -0.22 0.68 3 4 -24 -0.82 0.66 3 4 -24 -0.63 0.73 2 4 -24 -0.49 0.77 2 4 -24 -0.47 0.89 1 4 -24 0.35 0.84 0 -4 24 -0.75 0.75 0 4 -24 -0.02 0.90 1 -4 24 -0.26 0.76 2 -4 24 0.50 0.83 2 -4 24 0.30 0.70 3 -4 24 1.03 0.81 3 -4 24 2.50 0.88 4 3 -24 0.10 0.79 3 3 -24 0.34 0.76 3 3 -24 -0.11 0.70 2 3 -24 1.94 0.93 2 3 -24 -0.37 0.80 1 3 -24 1.55 0.95 0 -3 24 1.01 0.79 1 -3 24 0.94 0.77 2 -3 24 0.00 0.68 2 -3 24 -0.63 0.79 3 -3 24 -0.45 0.71 3 -3 24 0.47 0.66 4 -3 24 -0.10 0.60 4 -3 24 -0.19 0.67 5 2 -24 -0.20 1.29 5 2 -24 0.22 0.60 5 2 -24 0.49 0.70 4 2 -24 -0.10 0.82 4 2 -24 0.57 0.68 3 2 -24 0.47 0.78 3 2 -24 -0.40 0.68 2 2 -24 -0.52 0.81 2 2 -24 -0.12 0.70 1 2 -24 1.32 0.84 0 -2 24 1.48 0.78 1 -2 24 2.43 0.93 2 -2 24 -0.46 0.62 2 -2 24 0.34 0.74 3 -2 24 1.58 0.86 3 -2 24 0.64 0.65 4 -2 24 0.10 0.82 4 -2 24 -0.10 0.60 5 1 -24 0.67 1.32 5 1 -24 0.16 0.62 5 1 -24 -0.27 0.69 4 1 -24 1.64 0.74 4 1 -24 2.26 0.93 3 1 -24 -0.14 0.73 3 1 -24 0.18 0.72 2 1 -24 2.13 0.89 2 1 -24 1.35 0.93 1 1 -24 -0.18 0.78 0 -1 24 1.94 0.86 1 -1 24 1.22 0.78 2 -1 24 0.91 0.79 2 -1 24 2.14 0.82 3 -1 24 -0.37 0.63 3 -1 24 0.86 0.74 5 0 -24 0.75 0.62 5 0 -24 1.01 0.79 5 0 -24 -0.33 1.13 4 0 -24 -0.34 1.14 4 0 -24 -0.19 0.68 4 0 -24 1.54 0.73 3 0 -24 -0.47 0.71 3 0 -24 -0.09 0.76 2 0 -24 1.05 0.86 2 0 -24 -1.34 0.69 1 0 -24 -0.33 0.81 0 0 24 -0.23 0.69 1 0 24 0.51 0.71 1 0 24 0.79 0.80 2 0 24 0.39 0.68 2 0 24 -0.33 0.73 3 0 24 5.53 1.25 3 0 24 2.65 0.84 5 -1 -24 -0.23 0.71 5 -1 -24 0.49 0.63 5 -1 -24 -0.07 1.25 4 -1 -24 1.10 1.27 4 -1 -24 0.22 0.63 4 -1 -24 0.22 0.80 3 -1 -24 -0.10 0.77 3 -1 -24 -0.46 0.66 2 -1 -24 1.34 0.89 2 -1 -24 1.36 0.89 1 -1 -24 1.50 0.94 0 1 24 0.65 0.75 1 1 24 0.65 0.86 1 1 24 0.56 0.83 2 1 24 0.13 0.65 2 1 24 -0.55 0.71 3 1 24 -0.17 0.75 3 1 24 0.49 0.68 5 -2 -24 -0.46 1.19 5 -2 -24 0.82 0.86 5 -2 -24 0.96 0.65 4 -2 -24 0.54 0.85 4 -2 -24 1.60 1.34 4 -2 -24 0.82 0.74 3 -2 -24 -0.20 0.74 3 -2 -24 0.81 0.89 2 -2 -24 0.56 0.88 2 -2 -24 0.23 0.76 1 -2 -24 -0.27 0.79 0 2 24 0.41 0.79 1 2 24 0.60 0.73 1 2 24 -0.10 0.85 2 2 24 1.67 0.94 2 2 24 0.23 0.69 3 2 24 -1.49 0.74 3 2 24 -0.33 0.62 4 -3 -24 3.33 1.41 4 -3 -24 -0.21 0.83 4 -3 -24 0.61 0.79 3 -3 -24 0.18 0.78 3 -3 -24 0.49 0.86 2 -3 -24 0.26 0.86 1 -3 -24 1.04 0.93 0 3 24 1.55 0.88 1 3 24 -0.36 0.79 1 3 24 -0.82 0.62 2 3 24 -0.61 0.61 2 3 24 0.69 0.87 4 -4 -24 -0.17 0.73 4 -4 -24 -0.51 0.80 4 -4 -24 -0.22 1.23 3 -4 -24 1.29 0.93 3 -4 -24 0.84 0.90 2 -4 -24 0.31 0.82 1 -4 -24 0.65 0.94 0 4 24 0.40 0.86 1 4 24 0.93 0.97 1 4 24 0.89 0.77 2 4 24 0.62 0.73 2 4 24 -1.12 0.73 3 -5 -24 1.75 1.06 3 -5 -24 1.01 1.19 3 -5 -24 0.75 0.90 2 -5 -24 0.76 0.94 1 -5 -24 0.25 1.01 0 5 24 -0.63 0.77 1 5 24 0.80 0.83 1 5 24 0.24 0.88 1 -6 -24 -0.10 0.95 1 7 -25 -0.78 0.97 0 7 -25 -0.16 1.09 1 -7 25 -0.79 0.84 2 6 -25 0.89 0.93 2 6 -25 -0.47 0.85 1 6 -25 -0.46 0.89 0 6 -25 0.27 1.11 1 -6 25 0.69 0.91 2 -6 25 0.65 1.01 2 -6 25 0.31 0.82 3 5 -25 1.41 1.03 2 5 -25 -0.16 0.88 2 5 -25 0.31 0.93 1 5 -25 0.27 0.99 1 -5 25 0.62 0.86 2 -5 25 -0.96 0.82 2 -5 25 0.24 0.70 3 4 -25 1.15 0.84 3 4 -25 0.50 0.84 2 4 -25 0.07 0.84 2 4 -25 -0.51 0.86 1 4 -25 -0.18 0.82 0 -4 25 0.27 0.89 1 -4 25 1.35 0.88 2 -4 25 2.34 0.84 2 -4 25 0.43 0.87 3 -4 25 0.79 0.78 3 -4 25 0.79 0.87 4 3 -25 0.83 0.90 3 3 -25 1.26 0.90 3 3 -25 -0.16 0.76 2 3 -25 0.57 0.91 2 3 -25 -0.09 0.88 1 3 -25 0.08 0.92 0 -3 25 0.38 0.86 1 -3 25 1.28 0.88 2 -3 25 -0.44 0.79 2 -3 25 0.31 0.72 3 -3 25 -0.12 0.67 3 -3 25 1.04 0.81 4 2 -25 -0.32 0.80 4 2 -25 0.66 0.72 3 2 -25 0.69 0.81 3 2 -25 0.27 0.86 2 2 -25 2.36 1.04 2 2 -25 0.06 0.85 1 2 -25 -0.04 0.92 0 -2 25 0.23 0.83 1 -2 25 -0.47 0.72 2 -2 25 3.20 1.06 2 -2 25 2.91 0.94 3 -2 25 1.12 0.76 3 -2 25 0.23 0.77 4 1 -25 1.07 0.83 4 1 -25 -0.56 0.67 3 1 -25 1.51 0.91 3 1 -25 1.29 0.85 2 1 -25 0.29 0.86 2 1 -25 -0.59 0.82 1 1 -25 0.27 0.90 0 -1 25 0.12 0.76 1 -1 25 -0.70 0.68 2 -1 25 0.45 0.84 2 -1 25 -0.40 0.69 3 -1 25 -0.25 0.80 3 -1 25 -0.36 0.68 4 0 -25 0.15 0.71 4 0 -25 0.54 0.83 3 0 -25 0.06 0.80 3 0 -25 0.73 0.85 2 0 -25 1.48 0.93 2 0 -25 -0.40 0.85 1 0 -25 -0.21 0.86 0 0 25 0.89 0.80 1 0 25 0.39 0.82 2 0 25 0.46 0.72 2 0 25 0.45 0.84 4 -1 -25 1.99 0.81 4 -1 -25 0.29 0.84 3 -1 -25 1.14 0.82 3 -1 -25 -0.13 0.79 2 -1 -25 2.33 1.01 2 -1 -25 1.58 1.00 1 -1 -25 -0.53 0.86 0 1 25 -0.74 0.77 1 1 25 0.61 0.80 2 1 25 0.15 0.86 2 1 25 -0.34 0.71 4 -2 -25 -0.22 0.82 4 -2 -25 -0.21 0.67 3 -2 -25 0.28 0.83 3 -2 -25 0.47 0.85 2 -2 -25 -0.13 0.84 1 -2 -25 0.40 0.88 0 2 25 0.83 0.91 1 2 25 0.45 0.80 2 2 25 -0.18 0.81 2 2 25 0.27 0.77 3 -3 -25 1.98 1.04 3 -3 -25 -0.16 0.86 2 -3 -25 0.08 0.90 1 -3 -25 0.58 0.97 0 3 25 -0.46 0.81 1 3 25 -0.05 0.78 2 -4 -25 0.28 0.91 1 -4 -25 1.04 1.03 0 4 25 -0.20 0.86 1 5 -26 -1.09 0.90 1 -5 26 0.82 0.97 2 4 -26 3.50 1.18 2 4 -26 1.75 1.06 1 4 -26 1.26 1.07 1 -4 26 -0.45 0.84 3 3 -26 1.03 0.96 3 3 -26 0.98 0.91 2 3 -26 1.61 1.02 2 3 -26 1.22 0.99 1 3 -26 0.78 1.06 0 -3 26 0.02 0.87 1 -3 26 0.46 0.89 2 -3 26 -0.06 0.81 3 2 -26 0.11 0.83 3 2 -26 -0.07 0.82 2 2 -26 0.67 0.95 2 2 -26 -0.57 0.86 1 2 -26 0.26 0.89 0 -2 26 0.60 0.94 1 -2 26 2.81 1.01 2 -2 26 2.94 0.98 2 -2 26 3.11 1.15 3 1 -26 -0.24 0.82 3 1 -26 1.17 0.91 2 1 -26 -0.09 0.88 2 1 -26 1.03 0.98 1 1 -26 -0.41 0.88 0 -1 26 0.01 0.81 1 -1 26 -0.23 0.77 3 0 -26 -0.71 0.73 3 0 -26 0.38 0.90 2 0 -26 0.51 0.97 2 0 -26 0.10 0.94 1 0 -26 1.16 1.04 0 0 26 0.98 0.97 1 0 26 0.49 0.87 3 -1 -26 -0.56 0.84 3 -1 -26 0.09 0.86 2 -1 -26 0.15 0.93 1 -1 -26 0.87 1.01 0 1 26 1.03 0.95 1 1 26 1.71 0.93 2 -2 -26 -0.22 0.99 1 -2 -26 0.51 0.98 0 2 26 -0.18 0.86 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 55626 data_L1.DMA _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H13 N3 O5, C4 H9 N O' _chemical_formula_sum 'C19 H22 N4 O6' _chemical_formula_weight 402.41 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 8.8491(7) _cell_length_b 10.9303(15) _cell_length_c 10.9736(10) _cell_angle_alpha 105.249(10) _cell_angle_beta 93.074(7) _cell_angle_gamma 103.966(9) _cell_volume 985.96(19) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1178 _cell_measurement_theta_min 3.91 _cell_measurement_theta_max 21.77 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_F_000 424 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_absorpt_coefficient_mu 0.103 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91433 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details multi-scan _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7017 _diffrn_reflns_av_unetI/netI 0.0702 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.884 _diffrn_reflns_theta_max 25.247 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 3567 _reflns_number_gt 1418 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0100P)^2^+0.9000P] 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 3567 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.0839 _refine_ls_wR_factor_ref 0.1730 _refine_ls_wR_factor_gt 0.1332 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O6 O 0.9186(4) 0.3113(4) 0.5129(4) 0.1217(15) Uani 1 1 d . . . . . O3 O 0.3127(4) 0.1192(4) 0.3738(3) 0.1076(13) Uani 1 1 d . . . . . O2 O 0.3896(5) -0.1466(4) 0.8787(4) 0.1377(18) Uani 1 1 d . . . . . O1 O 0.2144(4) -0.0694(4) 0.9808(4) 0.1021(12) Uani 1 1 d . . . . . C9 C 0.2090(6) 0.1715(5) 0.4108(5) 0.0813(16) Uani 1 1 d . . . . . C2 C 0.2932(6) -0.0842(6) 0.8844(6) 0.0917(18) Uani 1 1 d . . . . . N2 N 0.1438(4) 0.2442(4) 0.3506(4) 0.0869(13) Uani 1 1 d . . . . . H2 H 0.0695 0.2727 0.3856 0.104 Uiso 1 1 calc R U . . . C6 C 0.1879(5) 0.1021(5) 0.6090(5) 0.0737(14) Uani 1 1 d . . . . . N1 N 0.1493(4) 0.1645(4) 0.5213(4) 0.0864(13) Uani 1 1 d . . . . . H1 H 0.0772 0.2045 0.5395 0.104 Uiso 1 1 calc R U . . . O5 O 0.3989(6) 0.3865(5) -0.1301(4) 0.1407(18) Uani 1 1 d . . . . . N5 N 0.7050(6) 0.3445(5) 0.5871(6) 0.135(2) Uani 1 1 d . . . . . C3 C 0.2560(6) -0.0198(5) 0.7909(5) 0.0808(15) Uani 1 1 d . . . . . C13 C 0.2499(7) 0.3610(6) 0.0282(6) 0.0939(18) Uani 1 1 d . . . . . N3 N 0.2800(8) 0.4082(6) -0.0839(6) 0.125(2) Uani 1 1 d . . . . . C10 C 0.1805(6) 0.2784(5) 0.2411(5) 0.0821(15) Uani 1 1 d . . . . . C5 C 0.3090(5) 0.0390(5) 0.6003(5) 0.0862(16) Uani 1 1 d . . . . . H5 H 0.3685 0.0373 0.5328 0.103 Uiso 1 1 calc R U . . . C7 C 0.1033(5) 0.0989(5) 0.7125(5) 0.0856(16) Uani 1 1 d . . . . . H7 H 0.0212 0.1388 0.7198 0.103 Uiso 1 1 calc R U . . . C8 C 0.1337(5) 0.0414(5) 0.8025(5) 0.0850(16) Uani 1 1 d . . . . . H8 H 0.0750 0.0426 0.8704 0.102 Uiso 1 1 calc R U . . . C17 C 0.5615(5) 0.3859(5) 0.6040(5) 0.113(2) Uani 1 1 d . . . . . H17A H 0.5870 0.4772 0.6508 0.169 Uiso 1 1 calc R U . . . H17B H 0.4969 0.3346 0.6500 0.169 Uiso 1 1 calc R U . . . H17C H 0.5058 0.3731 0.5222 0.169 Uiso 1 1 calc R U . . . C11 C 0.3095(6) 0.2527(5) 0.1802(5) 0.0886(17) Uani 1 1 d . . . . . H11 H 0.3724 0.2074 0.2105 0.106 Uiso 1 1 calc R U . . . C15 C 0.0887(6) 0.3435(5) 0.1913(6) 0.0915(17) Uani 1 1 d . . . . . H15 H 0.0018 0.3593 0.2304 0.110 Uiso 1 1 calc R U . . . C4 C 0.3396(6) -0.0200(5) 0.6907(5) 0.0891(17) Uani 1 1 d . . . . . H4 H 0.4203 -0.0616 0.6834 0.107 Uiso 1 1 calc R U . . . C18 C 0.7955(8) 0.3483(7) 0.5183(9) 0.150(4) Uani 1 1 d . . . . . C12 C 0.3412(6) 0.2953(6) 0.0759(6) 0.0982(19) Uani 1 1 d . . . . . H12 H 0.4274 0.2793 0.0359 0.118 Uiso 1 1 calc R U . . . C14 C 0.1207(6) 0.3852(6) 0.0875(6) 0.1008(18) Uani 1 1 d . . . . . H14 H 0.0573 0.4295 0.0562 0.121 Uiso 1 1 calc R U . . . O4 O 0.1947(7) 0.4626(6) -0.1253(6) 0.171(3) Uani 1 1 d . . . . . C19 C 0.7453(6) 0.4146(6) 0.4124(6) 0.117(2) Uani 1 1 d . . . . . H19A H 0.6764 0.3480 0.3433 0.176 Uiso 1 1 calc R U . . . H19B H 0.8374 0.4558 0.3808 0.176 Uiso 1 1 calc R U . . . H19C H 0.6923 0.4795 0.4501 0.176 Uiso 1 1 calc R U . . . C16 C 0.7543(7) 0.2783(6) 0.6943(6) 0.119(2) Uani 1 1 d . . . . . H16A H 0.7236 0.1843 0.6604 0.179 Uiso 1 1 calc R U . . . H16B H 0.7025 0.3035 0.7679 0.179 Uiso 1 1 calc R U . . . H16C H 0.8659 0.3081 0.7180 0.179 Uiso 1 1 calc R U . . . C1 C 0.2451(7) -0.1254(7) 1.0732(6) 0.131(2) Uani 1 1 d . . . . . H1A H 0.2229 -0.2189 1.0372 0.197 Uiso 1 1 calc R U . . . H1B H 0.1804 -0.1062 1.1394 0.197 Uiso 1 1 calc R U . . . H1C H 0.3536 -0.0906 1.1081 0.197 Uiso 1 1 calc R U . . . 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 O6 0.073(2) 0.126(3) 0.170(4) 0.021(3) 0.039(2) 0.052(2) O3 0.094(3) 0.134(3) 0.105(3) 0.014(2) 0.029(2) 0.069(3) O2 0.145(4) 0.171(4) 0.152(4) 0.067(3) 0.063(3) 0.111(4) O1 0.104(3) 0.123(3) 0.099(3) 0.045(3) 0.019(2) 0.051(3) C9 0.066(3) 0.087(4) 0.075(4) -0.003(3) 0.012(3) 0.019(3) C2 0.075(4) 0.093(4) 0.094(5) -0.001(4) 0.028(3) 0.024(3) N2 0.068(3) 0.091(3) 0.108(4) 0.020(3) 0.019(2) 0.039(3) C6 0.050(3) 0.072(3) 0.088(4) -0.001(3) 0.014(3) 0.018(3) N1 0.069(3) 0.094(3) 0.098(4) 0.014(3) 0.011(2) 0.038(2) O5 0.146(4) 0.154(4) 0.118(4) 0.034(3) 0.061(3) 0.029(3) N5 0.066(3) 0.111(4) 0.186(6) -0.032(4) 0.022(4) 0.027(3) C3 0.072(4) 0.078(4) 0.088(4) 0.015(3) -0.001(3) 0.023(3) C13 0.083(4) 0.086(4) 0.097(5) 0.001(4) 0.015(3) 0.020(3) N3 0.141(6) 0.118(5) 0.097(5) 0.024(4) 0.035(4) 0.002(4) C10 0.070(3) 0.082(4) 0.085(4) 0.006(3) 0.018(3) 0.020(3) C5 0.075(4) 0.090(4) 0.096(4) 0.016(3) 0.023(3) 0.034(3) C7 0.060(3) 0.095(4) 0.103(4) 0.015(4) 0.018(3) 0.037(3) C8 0.064(3) 0.094(4) 0.096(4) 0.015(3) 0.018(3) 0.031(3) C17 0.062(3) 0.120(5) 0.150(6) 0.012(4) 0.032(3) 0.036(3) C11 0.072(3) 0.088(4) 0.098(4) 0.005(3) 0.016(3) 0.032(3) C15 0.066(3) 0.102(4) 0.118(5) 0.030(4) 0.017(3) 0.044(3) C4 0.074(4) 0.095(4) 0.106(5) 0.019(4) 0.033(3) 0.041(3) C18 0.075(5) 0.108(6) 0.214(9) -0.042(6) 0.038(5) 0.015(4) C12 0.079(4) 0.095(5) 0.108(5) 0.004(4) 0.029(4) 0.023(3) C14 0.093(4) 0.107(5) 0.109(5) 0.033(4) 0.017(4) 0.033(4) O4 0.168(5) 0.213(6) 0.178(6) 0.091(5) 0.034(4) 0.095(5) C19 0.102(5) 0.137(6) 0.133(6) 0.041(5) 0.027(4) 0.063(4) C16 0.115(5) 0.114(5) 0.139(6) 0.031(5) 0.017(4) 0.056(4) C1 0.127(5) 0.159(7) 0.119(6) 0.043(5) 0.042(4) 0.050(5) _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 O6 C18 1.249(7) . ? O3 C9 1.227(5) . ? O2 C2 1.209(6) . ? O1 C2 1.294(5) . ? O1 C1 1.362(6) . ? C9 N1 1.362(6) . ? C9 N2 1.363(6) . ? C2 C3 1.453(7) . ? N2 C10 1.382(6) . ? C6 N1 1.390(6) . ? C6 C7 1.396(6) . ? C6 C5 1.403(6) . ? O5 N3 1.239(6) . ? N5 C18 1.130(7) . ? N5 C17 1.453(6) . ? N5 C16 1.626(7) . ? C3 C4 1.358(6) . ? C3 C8 1.398(6) . ? C13 C12 1.370(7) . ? C13 C14 1.391(6) . ? C13 N3 1.467(7) . ? N3 O4 1.205(6) . ? C10 C15 1.380(6) . ? C10 C11 1.402(6) . ? C5 C4 1.366(6) . ? C7 C8 1.350(6) . ? C11 C12 1.364(7) . ? C15 C14 1.353(6) . ? C18 C19 1.619(10) . ? 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 O1 C1 117.7(5) . . ? O3 C9 N1 122.1(6) . . ? O3 C9 N2 125.3(5) . . ? N1 C9 N2 112.6(5) . . ? O2 C2 O1 119.8(6) . . ? O2 C2 C3 125.6(5) . . ? O1 C2 C3 114.6(5) . . ? C9 N2 C10 128.9(4) . . ? N1 C6 C7 120.0(4) . . ? N1 C6 C5 123.7(4) . . ? C7 C6 C5 116.3(5) . . ? C9 N1 C6 129.3(4) . . ? C18 N5 C17 136.2(9) . . ? C18 N5 C16 109.8(7) . . ? C17 N5 C16 114.0(5) . . ? C4 C3 C8 119.6(5) . . ? C4 C3 C2 119.8(5) . . ? C8 C3 C2 120.6(5) . . ? C12 C13 C14 119.3(6) . . ? C12 C13 N3 123.5(6) . . ? C14 C13 N3 117.2(6) . . ? O4 N3 O5 124.4(7) . . ? O4 N3 C13 121.7(7) . . ? O5 N3 C13 113.9(6) . . ? C15 C10 N2 118.6(5) . . ? C15 C10 C11 118.5(5) . . ? N2 C10 C11 122.8(5) . . ? C4 C5 C6 120.1(5) . . ? C8 C7 C6 123.9(5) . . ? C7 C8 C3 118.1(5) . . ? C12 C11 C10 118.9(5) . . ? C14 C15 C10 122.2(5) . . ? C3 C4 C5 122.0(5) . . ? N5 C18 O6 131.5(11) . . ? N5 C18 C19 109.3(7) . . ? O6 C18 C19 119.3(7) . . ? C11 C12 C13 121.9(5) . . ? C15 C14 C13 119.1(6) . . ? _refine_diff_density_max 0.273 _refine_diff_density_min -0.161 _refine_diff_density_rms 0.039 _shelx_res_file ; exp_2318.res created by SHELXL-2014/7 TITL CF solution in P-1 CELL 0.71073 8.84906 10.93035 10.97358 105.2486 93.0741 103.9664 ZERR 2 0.00073 0.0015 0.00096 0.0097 0.0071 0.0092 LATT 1 SFAC C H N O UNIT 38 44 8 12 OMIT -3 50.5 REM C:/JBB2/ARUP%20TARAI/exp_2318/struct/olex2_exp_2318/exp_2318.hkl L.S. 10 ACTA BOND FMAP 2 PLAN 1 WGHT 0.010000 0.900000 FVAR 3.98944 MOLE 1 O6 4 0.918620 0.311262 0.512926 11.00000 0.07322 0.12618 = 0.16972 0.02072 0.03900 0.05248 O3 4 0.312750 0.119234 0.373779 11.00000 0.09444 0.13384 = 0.10516 0.01362 0.02944 0.06874 O2 4 0.389638 -0.146559 0.878748 11.00000 0.14485 0.17083 = 0.15209 0.06655 0.06285 0.11099 O1 4 0.214393 -0.069400 0.980776 11.00000 0.10400 0.12338 = 0.09877 0.04453 0.01872 0.05144 C9 1 0.209020 0.171529 0.410810 11.00000 0.06643 0.08683 = 0.07482 -0.00298 0.01163 0.01861 C2 1 0.293217 -0.084183 0.884418 11.00000 0.07464 0.09338 = 0.09409 -0.00099 0.02824 0.02448 N2 3 0.143754 0.244193 0.350649 11.00000 0.06752 0.09086 = 0.10825 0.01996 0.01900 0.03937 AFIX 43 H2 2 0.069481 0.272705 0.385650 11.00000 -1.20000 AFIX 0 C6 1 0.187900 0.102131 0.609042 11.00000 0.04968 0.07153 = 0.08776 -0.00122 0.01444 0.01841 N1 3 0.149256 0.164541 0.521347 11.00000 0.06877 0.09373 = 0.09761 0.01369 0.01137 0.03807 AFIX 43 H1 2 0.077198 0.204525 0.539491 11.00000 -1.20000 AFIX 0 O5 4 0.398897 0.386526 -0.130144 11.00000 0.14559 0.15437 = 0.11826 0.03372 0.06108 0.02855 N5 3 0.705030 0.344485 0.587083 11.00000 0.06601 0.11135 = 0.18566 -0.03185 0.02221 0.02693 C3 1 0.255998 -0.019833 0.790863 11.00000 0.07151 0.07839 = 0.08750 0.01465 -0.00084 0.02269 C13 1 0.249856 0.361042 0.028191 11.00000 0.08263 0.08620 = 0.09723 0.00091 0.01494 0.02006 N3 3 0.279999 0.408188 -0.083918 11.00000 0.14065 0.11771 = 0.09695 0.02422 0.03504 0.00244 C10 1 0.180525 0.278356 0.241124 11.00000 0.07027 0.08186 = 0.08463 0.00622 0.01804 0.02008 C5 1 0.309015 0.039001 0.600274 11.00000 0.07488 0.08987 = 0.09624 0.01635 0.02348 0.03446 AFIX 43 H5 2 0.368538 0.037319 0.532827 11.00000 -1.20000 AFIX 0 C7 1 0.103311 0.098935 0.712463 11.00000 0.06008 0.09549 = 0.10300 0.01454 0.01771 0.03719 AFIX 43 H7 2 0.021168 0.138758 0.719778 11.00000 -1.20000 AFIX 0 C8 1 0.133708 0.041440 0.802505 11.00000 0.06392 0.09405 = 0.09625 0.01542 0.01850 0.03071 AFIX 43 H8 2 0.074955 0.042560 0.870371 11.00000 -1.20000 AFIX 0 C17 1 0.561515 0.385869 0.603960 11.00000 0.06236 0.11974 = 0.14970 0.01235 0.03187 0.03627 AFIX 137 H17A 2 0.587021 0.477243 0.650846 11.00000 -1.50000 H17B 2 0.496874 0.334642 0.650029 11.00000 -1.50000 H17C 2 0.505806 0.373071 0.522156 11.00000 -1.50000 AFIX 0 C11 1 0.309528 0.252686 0.180243 11.00000 0.07226 0.08848 = 0.09843 0.00493 0.01626 0.03180 AFIX 43 H11 2 0.372391 0.207370 0.210518 11.00000 -1.20000 AFIX 0 C15 1 0.088683 0.343532 0.191301 11.00000 0.06637 0.10159 = 0.11803 0.03018 0.01734 0.04366 AFIX 43 H15 2 0.001827 0.359335 0.230374 11.00000 -1.20000 AFIX 0 C4 1 0.339649 -0.020001 0.690657 11.00000 0.07372 0.09458 = 0.10617 0.01938 0.03300 0.04082 AFIX 43 H4 2 0.420253 -0.061560 0.683355 11.00000 -1.20000 AFIX 0 C18 1 0.795528 0.348262 0.518349 11.00000 0.07459 0.10763 = 0.21355 -0.04191 0.03767 0.01519 C12 1 0.341221 0.295316 0.075872 11.00000 0.07857 0.09477 = 0.10840 0.00383 0.02941 0.02279 AFIX 43 H12 2 0.427412 0.279291 0.035886 11.00000 -1.20000 AFIX 0 C14 1 0.120736 0.385238 0.087489 11.00000 0.09264 0.10655 = 0.10885 0.03341 0.01658 0.03320 AFIX 43 H14 2 0.057263 0.429487 0.056221 11.00000 -1.20000 AFIX 0 O4 4 0.194668 0.462601 -0.125318 11.00000 0.16788 0.21326 = 0.17765 0.09073 0.03390 0.09475 C19 1 0.745302 0.414646 0.412365 11.00000 0.10201 0.13671 = 0.13301 0.04119 0.02727 0.06300 AFIX 137 H19A 2 0.676434 0.348033 0.343328 11.00000 -1.50000 H19B 2 0.837419 0.455751 0.380805 11.00000 -1.50000 H19C 2 0.692270 0.479520 0.450112 11.00000 -1.50000 AFIX 0 C16 1 0.754312 0.278326 0.694310 11.00000 0.11526 0.11379 = 0.13898 0.03052 0.01726 0.05597 AFIX 137 H16A 2 0.723610 0.184310 0.660369 11.00000 -1.50000 H16B 2 0.702515 0.303542 0.767889 11.00000 -1.50000 H16C 2 0.865915 0.308055 0.717996 11.00000 -1.50000 AFIX 0 C1 1 0.245085 -0.125417 1.073192 11.00000 0.12694 0.15940 = 0.11949 0.04346 0.04188 0.05007 AFIX 137 H1A 2 0.222909 -0.218926 1.037229 11.00000 -1.50000 H1B 2 0.180367 -0.106249 1.139360 11.00000 -1.50000 H1C 2 0.353618 -0.090567 1.108135 11.00000 -1.50000 AFIX 0 HKLF 4 REM CF solution in P-1 REM R1 = 0.0839 for 1418 Fo > 4sig(Fo) and 0.1879 for all 3567 data REM 266 parameters refined using 0 restraints END WGHT 0.0574 0.8902 REM Highest difference peak 0.273, deepest hole -0.161, 1-sigma level 0.039 Q1 1 0.6990 0.3932 0.5026 11.00000 0.05 0.27 ; _shelx_res_checksum 28351 _shelx_hkl_file ; 0 0 2 16275.2 344.159 1 0 0 -2 15927.5 343.014 1 0 0 -3 1961.09 152.344 1 0 0 3 1981.55 148.678 1 0 0 -4 17561.6 517.300 1 0 0 -5 37.2500 23.7604 1 0 0 -6 962.547 149.656 1 0 0 7 409.994 86.6270 5 0 0 -7 635.372 127.792 1 0 0 -8 355.926 99.2946 1 0 0 -9 44.3824 31.7495 1 0 0 -10 872.138 192.233 1 0 0 -11 165.127 104.965 1 0 0 -12 214.027 106.736 1 0 0 -13 69.1164 89.9535 1 0 1 -13-44.3455 88.6724 1 0 1 -12-5.36563 38.8153 1 0 1 -11 42.2113 68.3594 1 0 1 -10 210.686 90.6531 1 0 1 -9 121.642 78.2638 1 0 -1 8 39.5757 29.7364 4 0 1 -8 27.2369 48.4473 1 0 -1 8 9.91090 13.6163 5 0 -1 7 1.43948 19.9708 5 0 1 -7-14.8087 35.2987 1 0 -1 7 26.4344 25.5378 4 0 -1 6 9515.45 324.840 5 0 -1 6 9675.11 305.559 4 0 1 -6 10586.6 487.449 1 0 -1 5 494.912 62.0225 4 0 1 -5 477.628 94.5700 1 0 -1 5 502.328 63.8334 5 0 -1 4 1463.57 99.2901 5 0 -1 4 1558.85 93.9904 4 0 -1 4 1426.08 128.215 2 0 1 -4 1469.42 145.208 1 0 1 -3 8569.62 278.244 2 0 1 -3 8732.92 299.997 1 0 -1 3 8166.50 195.105 5 0 -1 3 8460.01 291.350 1 0 -1 3 8511.49 282.590 2 0 -1 2 110.788 27.7715 2 0 1 -2 23.6295 20.8458 2 0 1 -2 83.7142 21.4057 1 0 1 2 39682.1 616.416 1 0 -1 -2 40250.1 615.812 1 0 -1 -3 7661.65 323.210 1 0 1 3 7613.44 309.959 1 0 -1 -4 117.816 27.5731 1 0 1 4 163.696 53.5083 3 0 -1 -5 4579.28 312.932 1 0 -1 -6 1721.95 206.233 1 0 -1 -7 49.1039 46.8480 1 0 -1 -8-14.4782 41.6402 1 0 -1 -9 91.5357 68.2461 1 0 -1 -10 217.388 116.447 1 0 -1 -11 132.369 83.7849 1 0 -1 -12 76.4078 104.655 1 0 2 -13-73.9123 66.5081 1 0 2 -12 41.9690 41.6795 1 0 2 -11-51.1951 55.6378 1 0 2 -10 930.127 193.457 1 0 2 -9 1387.46 221.847 1 0 2 -8 83.7854 65.7942 1 0 -2 8 50.9281 31.1646 5 0 2 -7 85.4855 52.1908 1 0 -2 7 67.8732 27.1073 5 0 -2 6 2855.33 146.177 5 0 2 -6 3326.91 276.223 1 0 2 -5 3206.85 240.950 1 0 2 -5 3446.92 236.605 2 0 2 -4 4748.16 168.239 5 0 2 -4 5282.58 260.599 2 0 2 -4 4469.34 132.553 4 0 -2 4 5140.41 263.252 2 0 2 -4 5161.47 269.880 1 0 2 -3 16652.7 301.143 5 0 2 -3 16759.4 417.819 2 0 -2 3 16687.7 427.461 2 0 2 -2 91.7989 23.8392 2 0 -2 2 109.537 30.7415 2 0 -2 1 29755.5 434.229 6 0 -2 1 29769.1 371.449 3 0 2 -1 30292.6 619.581 7 0 -2 1 30508.5 626.518 7 0 2 -1 30891.0 483.454 2 0 -2 1 30314.2 495.651 2 0 2 -1 29783.8 443.097 6 0 2 0 646.493 87.0497 7 0 -2 0 675.634 89.9274 7 0 -2 -1 3847.78 201.762 1 0 2 1 3620.73 195.224 1 0 -2 -1 3701.29 234.219 7 0 -2 -2 104.231 44.2774 1 0 2 2 105.042 33.4712 1 0 -2 -3 6690.50 332.372 1 0 2 3 6643.96 263.987 3 0 -2 -4 442.917 94.1759 1 0 2 4 490.994 84.7910 3 0 -2 -5 5776.53 375.339 1 0 -2 -6 251.077 84.5862 1 0 -2 -7 1565.37 225.645 1 0 -2 -8 93.1362 66.4694 1 0 -2 -9 15.9895 54.1758 1 0 -2 -10-26.1681 54.2326 1 0 -2 -11 66.8352 54.3639 1 0 -2 -12 40.2433 50.8047 1 0 3 -13-9.95051 40.9531 1 0 3 -12 143.644 90.3711 1 0 3 -11 0.15085 22.6848 1 0 3 -10 634.127 154.753 1 0 3 -9 298.701 109.694 1 0 3 -8 135.337 54.2758 1 0 3 -7 48.8106 44.4380 1 0 3 -7 107.129 64.8436 2 0 3 -6 295.830 73.4062 1 0 3 -6 248.835 44.9631 5 0 3 -6 348.773 85.0514 2 0 3 -5 4303.11 270.274 2 0 3 -5 3926.67 178.125 5 0 3 -5 4051.89 268.776 1 0 3 -5 3416.90 145.151 4 0 3 -4 14165.1 343.875 5 0 3 -4 15458.4 474.542 2 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268.551 2 -2 -1 4 7530.54 272.951 2 2 1 -4 7380.63 254.520 2 2 1 -4 7679.07 326.852 1 2 1 -4 7835.32 397.123 3 2 1 -4 7256.64 341.926 4 2 1 -3 1785.72 129.823 1 2 1 -3 1712.09 116.892 2 2 1 -3 1650.04 107.040 5 2 1 -3 1650.42 171.543 4 2 1 -3 1766.78 170.337 3 2 1 -2 2348.52 157.854 5 2 1 -2 2433.58 124.556 1 2 1 -2 2505.44 244.270 6 -2 -1 1-30.2584 43.9620 6 2 1 -1-14.4943 28.9111 6 2 1 -1-0.10128 27.0401 5 2 1 -1 4.77887 7.29959 7 -2 -1 0 38660.9 596.054 7 2 1 0 38955.0 412.632 1 -2 -1 0 40167.0 940.654 6 2 1 0 39150.8 915.363 6 -2 -1 -1 17441.7 358.191 1 2 1 1 16527.8 334.576 1 -2 -1 -1 16838.8 649.335 6 2 1 2 7542.47 269.918 1 -2 -1 -2 7876.63 290.404 1 -2 -1 -3 1942.03 167.002 1 2 1 3 1932.98 164.317 1 -2 -1 -4 65.2615 39.8339 1 -2 -1 -5 1208.25 162.801 1 -2 -1 -6 1005.80 166.316 1 -2 -1 -7 162.975 81.9014 1 -2 -1 -8 76.1729 59.1505 1 -2 -1 -9 25.0127 50.2049 1 -2 -1 -10 63.4828 57.8922 1 -2 -1 -11 162.023 104.035 1 -2 -1 -12 123.190 110.977 1 2 2 -13 72.4857 64.0748 1 2 2 -12 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46.1786 2 -2 -3 2 2870.35 293.510 6 2 3 -2 2868.19 289.512 6 2 3 -2 2663.11 238.310 7 2 3 -2 2784.96 203.305 3 -2 -3 1 50.2408 37.5666 7 2 3 -1 22.7602 15.5284 7 -2 -3 1-16.5501 44.4060 6 2 3 -1 23.5882 47.2025 6 2 3 0 5781.84 269.687 1 -2 -3 0 6063.94 366.488 7 -2 -3 0 5945.19 425.027 6 2 3 1 6513.71 306.293 1 -2 -3 -1 6812.50 479.016 6 -2 -3 -1 6655.16 404.245 7 -2 -3 -2 174.969 57.5844 1 -2 -3 -3 215.202 73.9046 1 -2 -3 -4 205.773 74.0734 1 -2 -3 -5-1.55202 18.7743 1 -2 -3 -6-35.7579 40.1277 1 -2 -3 -7-34.1116 38.2006 1 -2 -3 -8 459.929 137.298 1 -2 -3 -9-60.0220 66.2907 1 -2 -3 -10-73.0888 65.1774 1 -2 -3 -11 74.6118 77.5876 1 2 4 -13 95.9953 90.5052 1 2 4 -12 41.6528 55.3344 1 2 4 -11 96.6037 82.0753 1 2 4 -10 115.299 77.5758 2 2 4 -10-8.51190 52.4292 1 2 4 -9 926.640 160.859 2 2 4 -9 992.410 193.474 1 2 4 -9 844.687 114.980 4 2 4 -8 1694.73 228.647 1 2 4 -8 1653.07 195.015 2 2 4 -8 1741.20 184.320 4 2 4 -7 389.267 110.551 1 2 4 -7 471.999 105.655 2 2 4 -7 381.154 91.1710 4 2 4 -6 524.913 121.567 3 2 4 -6 448.008 99.1533 2 2 4 -6 476.754 106.164 1 2 4 -5 674.088 127.919 3 2 4 -5 623.311 109.408 2 2 4 -4 1678.70 184.719 3 2 4 -4 1655.78 179.050 2 2 4 -3-23.0442 41.8987 2 2 4 -3 6.50145 21.9248 3 -2 -4 2 2529.92 267.909 7 -2 -4 2 2473.72 281.189 6 2 4 -2 2460.75 189.415 3 -2 -4 1 1169.32 177.802 7 -2 -4 1 1159.38 200.503 6 -2 -4 0 1388.85 223.108 6 -2 -4 0 1328.53 195.634 7 -2 -4 -1 1953.43 250.205 7 -2 -4 -1 1828.28 264.995 6 -2 -4 -2 100190. 1845.95 7 -2 -4 -3 87.8841 64.0490 7 -2 -4 -3 108.137 65.2438 1 -2 -4 -4 163.456 74.7509 1 -2 -4 -5-28.7436 43.2447 1 -2 -4 -6 63.7046 37.9211 1 -2 -4 -7 81.4113 63.0867 1 -2 -4 -8-93.2645 80.0068 1 -2 -4 -9-150.163 91.5571 1 -2 -4 -10-152.255 97.4485 1 -2 -4 -11 32.8613 37.1620 1 2 5 -13 59.9665 73.9758 1 2 5 -12 95.3641 65.3263 1 2 5 -11 165.848 86.6970 2 2 5 -11 76.0836 57.1347 1 2 5 -10-22.8028 31.7246 1 2 5 -10 48.2946 56.1119 2 2 5 -9 270.343 93.2905 1 2 5 -9 113.307 42.7186 2 2 5 -9 248.614 69.4042 4 2 5 -8 423.911 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147.175 3 -3 7 2 1615.29 177.585 2 3 -7 -2 1636.99 277.967 7 3 -7 -1 19.8040 40.1224 7 -3 7 1 21.1420 20.2333 2 -3 7 0 33.1235 10.3933 2 3 -7 0 44.5051 43.7082 7 -3 7 -1 1548.78 183.966 2 3 -7 1 926.193 82.9516 6 3 -7 1 1488.18 259.134 7 -3 7 -2 1546.69 192.129 2 -3 7 -3-40.4808 67.8488 5 -3 7 -3 90.9623 54.8741 2 -3 7 -4 1111.09 184.702 5 -3 7 -4 1059.34 168.249 2 -3 7 -5 312.992 57.0260 6 -3 7 -5 297.259 76.0323 2 -3 7 -6 71.1018 58.0784 2 -3 7 -6 95.8035 66.5128 5 -3 7 -7 121.947 94.7098 2 -3 7 -7-14.4489 42.6186 5 -3 7 -8 1147.07 220.452 2 -3 7 -8 838.763 172.159 5 -3 7 -9 112.306 90.9524 2 -3 7 -9 54.4703 45.0057 5 -3 7 -9-70.6251 63.5350 1 -3 7 -10 65.2517 59.9969 1 -3 7 -11 39.4788 55.2632 1 -3 7 -12 17.3834 47.1422 1 3 -6 -10 55.3300 67.3195 1 3 -6 -9-57.4377 70.0210 1 3 -6 -8 19.0112 35.8611 1 3 -6 -7 26.3566 40.8068 1 3 -6 -7 69.7736 79.3286 7 3 -6 -6 132.753 104.273 7 3 -6 -6 157.570 79.5066 1 3 -6 -5 33.7466 47.6730 7 3 -6 -5 13.1282 35.1222 1 3 -6 -4 38.2191 24.8678 3 -3 6 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351.227 151.879 4 -9 2 0 65.5164 68.2571 6 -9 2 0 3.58048 55.8291 5 -9 2 -1-28.1355 89.0395 6 -9 2 -1 48.7825 43.4955 5 9 -2 1-66.7353 52.0167 4 -9 2 -2 396.357 213.215 6 9 -2 2 392.911 162.678 4 -9 2 -3 48.0078 59.0168 6 9 -2 3 26.0498 46.3353 4 -9 2 -4 64.3326 48.2812 6 9 -2 4 34.1220 37.2621 4 -9 2 -5 36.7799 117.025 6 9 -2 5 48.1464 71.7625 4 -9 2 -6 46.6872 79.1980 6 -9 2 -7 63.3273 158.705 6 9 -1 -8 113.120 88.2213 4 9 -1 -8 153.416 98.2337 3 9 -1 -7 63.4994 64.7135 4 9 -1 -7 138.026 101.672 3 9 -1 -6 1.70385 44.7783 3 9 -1 -6 17.5223 28.2877 4 9 -1 -5 179.939 100.469 3 9 -1 -5 259.490 137.419 4 9 -1 -4 166.809 117.474 4 9 -1 -3 160.816 127.627 4 9 -1 -2 158.593 107.203 4 -9 1 1-9.71394 58.3338 6 9 -1 -1-40.8844 35.0824 4 -9 1 0-13.8791 83.3504 6 9 -1 0 60.6629 81.8407 4 -9 1 -1 106.551 91.9229 6 9 -1 1 52.7691 35.5702 4 -9 1 -2 329.858 194.727 6 9 -1 2 407.751 164.369 4 -9 1 -3 61.2889 101.455 6 9 -1 3-64.0883 33.3528 4 -9 1 -4-20.0940 45.2318 6 9 -1 4 69.3592 69.8141 4 -9 1 -5 84.8339 98.7742 6 9 -1 5 1.82286 44.3555 4 -9 1 -6-196.446 154.335 6 -9 1 -7-276.158 187.063 6 9 0 -9-62.2724 65.3107 4 9 0 -8-81.6081 93.2165 4 9 0 -8-52.1952 54.3003 3 9 0 -7-37.1319 52.2361 3 9 0 -7-33.3349 60.5130 4 9 0 -6-19.3159 36.0754 3 9 0 -6 86.5471 88.2461 4 9 0 -5 33.1986 44.8499 3 9 0 -5 154.119 114.962 4 9 0 -4 1015.85 258.378 4 9 0 -3 458.247 184.994 4 9 0 -2 15.4445 22.5744 4 -9 0 1 212.891 179.658 6 9 0 -1 3.03872 53.9379 4 -9 0 0 153.839 132.237 6 9 0 0 40.7905 70.2653 4 -9 0 -1 35.4371 67.0769 6 9 0 1 14.4481 61.0667 4 -9 0 -2 72.2739 60.8745 6 9 0 2-158.737 106.697 4 -9 0 -3 111.342 131.017 6 9 0 3 146.680 129.435 4 -9 0 -4 300.804 212.814 6 9 0 4 177.651 122.414 4 -9 0 -5 206.934 159.003 6 9 0 5 26.8261 47.6916 4 -9 0 -6-99.7580 116.009 6 9 1 -10 12.4773 53.0275 4 9 1 -9-73.1596 72.1777 4 9 1 -8-56.0358 65.3089 3 9 1 -8 88.6821 65.1060 4 9 1 -7 42.5416 32.6959 3 9 1 -7 127.111 101.771 4 9 1 -6-70.1150 36.7267 3 9 1 -6 161.009 116.816 4 9 1 -5-14.2874 51.5690 3 9 1 -5 432.827 199.685 4 9 1 -4 112.250 74.5718 4 9 1 -3 680.692 226.122 4 -9 -1 2 793.911 305.704 6 9 1 -2 599.741 208.105 4 -9 -1 1 1.27475 104.260 6 9 1 -1-9.48127 64.8626 4 -9 -1 0-72.9041 51.3071 6 9 1 0-80.8797 91.5922 4 -9 -1 -1 26.7500 91.4617 6 9 1 1-81.4714 101.797 4 -9 -1 -2 22.4239 59.8991 6 9 1 2 59.4703 63.7829 4 -9 -1 -3 87.7866 138.213 6 9 1 3-87.8481 83.9417 4 -9 -1 -4-75.1530 100.688 6 9 1 4-184.355 119.990 4 -9 -1 -5 222.650 170.548 6 9 1 5-249.062 139.346 4 9 2 -9 28.2549 46.9568 4 9 2 -8 112.682 105.478 3 9 2 -8 169.853 128.533 4 9 2 -7-12.2514 40.8123 3 9 2 -7 204.777 147.897 4 9 2 -6 36.6515 49.1417 3 9 2 -6-15.3861 60.6851 4 9 2 -5 16.5423 36.9148 3 9 2 -5 33.4246 45.3198 4 9 2 -4 132.907 103.103 4 9 2 -3 298.185 141.856 4 -9 -2 2 86.7501 88.3675 6 9 2 -2-34.8786 61.2540 4 -9 -2 1 155.298 117.700 6 9 2 -1 212.867 135.721 4 -9 -2 0 304.134 216.998 6 9 2 0 118.692 104.345 4 -9 -2 -1 116.320 142.650 6 9 2 1-133.817 110.313 4 -9 -2 -2 71.2538 129.338 6 9 2 2 14.9805 50.9542 4 -9 -2 -3 33.9773 71.5376 6 -9 -2 -4 61.2060 86.3257 6 9 3 -9 12.2873 56.9395 4 9 3 -8 37.8054 95.4334 4 9 3 -7 29.4043 55.7200 3 9 3 -7-5.03405 39.3039 4 9 3 -6 3.13309 27.1083 3 9 3 -6 10.0334 84.5368 4 9 3 -5-129.263 93.2694 3 9 3 -5 110.477 89.4035 4 9 3 -4-60.2721 64.0820 3 9 3 -4-56.7792 73.4043 4 9 3 -3 3.40997 59.4331 4 -9 -3 2 112.715 116.161 6 9 3 -2 46.2335 78.6146 4 -9 -3 1 31.8752 61.2306 6 9 3 -1 99.8919 85.1936 4 -9 -3 0 59.4895 137.443 6 9 3 0-46.8581 69.9008 4 -9 -3 -1-43.4614 82.0081 6 -9 -3 -2 117.535 138.646 6 9 4 -8 18.4836 94.1381 4 9 4 -7 48.3657 60.5209 3 9 4 -7 151.255 126.602 4 9 4 -6-132.145 94.9659 3 9 4 -6 95.0992 98.1961 4 9 4 -5 28.5756 85.2318 3 9 4 -5-109.760 99.1068 4 9 4 -4 41.0659 91.0236 3 9 4 -4 80.9038 86.0670 4 9 4 -3 35.6680 77.1692 4 -9 -4 2 110.973 121.282 6 9 4 -2 216.203 151.324 4 -9 -4 1 67.5829 112.675 6 -9 -4 0 118.688 122.689 6 -9 -4 -1 6.66843 40.6637 6 9 5 -6-53.2714 61.9888 3 9 5 -5 18.8860 32.1819 3 9 5 -5-56.0903 101.469 4 9 5 -4-90.5578 78.2705 3 9 5 -4 37.3442 76.6135 4 9 5 -3-73.3737 70.2396 3 9 5 -3-100.864 83.6920 4 -9 -5 2 107.752 149.274 6 -9 -5 1 36.0317 139.345 6 9 6 -6 8.30116 29.4616 3 9 6 -5-52.2464 60.3801 3 9 6 -4-17.8617 37.5848 3 9 6 -4 47.7704 67.5694 2 -10 8 5-8.53075 38.4498 5 10 -8 -4 36.3131 52.1128 3 -10 8 4 8.96674 28.7841 5 -10 8 3 138.057 109.180 5 -10 8 2 7.39356 60.1206 5 -10 8 1-9.68323 49.3390 5 -10 8 0 211.553 127.767 5 -10 8 -1 175.188 145.401 5 -10 8 -2 92.7745 75.1179 5 -10 8 -3 79.4799 76.6973 5 10 -7 -6 7.78845 29.3398 3 10 -7 -5 25.1015 81.9652 3 -10 7 5-37.7424 29.8737 5 -10 7 4 59.4816 84.8381 5 -10 7 3-114.900 94.2617 5 -10 7 2 157.806 113.417 5 -10 7 1 4.52190 65.2117 5 -10 7 0 126.852 128.480 5 -10 7 -1 25.6085 64.2972 5 -10 7 -2 11.3767 42.9569 5 -10 7 -3-6.95724 29.2199 5 -10 7 -4-32.5703 45.8232 5 10 -6 -6 80.4145 103.949 3 10 -6 -5 106.765 112.579 3 -10 6 5 151.773 133.634 5 -10 6 4 63.8980 92.7870 5 -10 6 3 133.378 112.749 5 -10 6 2-43.9029 43.3512 5 -10 6 1 86.0383 60.3941 5 -10 6 0 50.5588 66.2522 5 -10 6 -1 0.17855 31.2766 5 -10 6 -2-41.5264 25.1465 5 -10 6 -3-0.47427 52.3391 5 -10 6 -4 22.5800 51.8831 5 -10 6 -5 130.283 124.419 5 10 -5 -6-23.1798 76.3614 3 10 -5 -5 77.7496 84.7251 3 -10 5 5 5.70154 44.2357 5 -10 5 4 28.1955 68.8799 5 -10 5 3 124.785 81.5006 5 -10 5 2 104.617 77.5984 5 10 -5 -1 327.524 136.287 4 -10 5 1 316.501 146.257 5 10 -5 0 372.661 149.975 4 -10 5 0 322.975 158.836 5 10 -5 1-141.415 91.6236 4 -10 5 -1 8.26575 74.5561 5 10 -5 2-147.288 92.7434 4 -10 5 -2-5.10005 53.7509 6 -10 5 -2 4.23571 76.5825 5 10 -5 3 84.9867 94.2879 4 -10 5 -3 151.846 141.694 6 -10 5 -3-0.19261 64.0789 5 10 -5 4-192.644 103.031 4 -10 5 -4-12.4635 40.9440 6 -10 5 -4-25.7078 93.7628 5 -10 5 -5 25.7230 64.7730 6 -10 5 -5-31.0420 53.8246 5 10 -4 -6 21.3532 58.6004 3 10 -4 -5 10.9005 43.9825 3 -10 4 5 13.0168 41.3072 5 -10 4 4-51.2800 30.0003 5 10 -4 -3-9.14156 50.9273 4 -10 4 3 114.372 89.1278 5 10 -4 -2 50.9181 23.9317 4 -10 4 2 42.5415 73.1289 5 10 -4 -1-96.6560 82.5077 4 -10 4 1-23.5065 89.8803 5 -10 4 0 76.2220 51.1153 5 10 -4 0 229.290 129.877 4 -10 4 -1-103.429 99.0043 5 10 -4 1-122.325 87.6038 4 -10 4 -2-13.3628 45.9488 6 -10 4 -2 146.460 117.649 5 10 -4 2 69.3239 68.1117 4 -10 4 -3 83.5993 130.872 6 -10 4 -3 65.6812 63.2961 5 10 -4 3 11.0477 66.9509 4 -10 4 -4 1.51895 75.8573 6 -10 4 -4 79.2852 70.0540 5 10 -4 4 21.2209 66.6000 4 -10 4 -5-62.3455 84.9063 6 -10 4 -6 68.4261 86.1954 6 -10 4 -7-144.787 134.510 6 10 -3 -6 24.7001 51.0586 3 10 -3 -5-84.0656 68.9395 4 10 -3 -5 121.344 99.5879 3 -10 3 5 22.5167 66.7482 5 10 -3 -4 98.1360 72.9801 4 -10 3 4-8.33810 33.4093 5 -10 3 3 411.642 174.234 5 10 -3 -3 382.345 148.192 4 -10 3 2 2.06573 58.2280 5 10 -3 -2 43.4709 63.9989 4 -10 3 1 210.033 126.000 5 10 -3 -1 74.8545 84.5931 4 -10 3 0-42.1625 89.5920 5 10 -3 0 54.4575 94.3411 4 -10 3 -1 19.2614 97.2275 6 -10 3 -1-82.2653 96.1780 5 10 -3 1 67.7848 86.4338 4 -10 3 -2 75.5802 90.3584 6 10 -3 2 46.8247 88.0184 4 -10 3 -3 84.1911 92.0367 6 10 -3 3 114.999 96.3655 4 -10 3 -4-6.10800 66.5013 6 10 -3 4 133.245 116.696 4 -10 3 -5 4.44712 65.0487 6 -10 3 -6 13.5271 107.849 6 10 -2 -6-75.4507 96.5557 4 10 -2 -6-7.89113 32.8620 3 -10 2 5-23.0411 52.9659 5 10 -2 -5-146.035 101.197 4 -10 2 4 76.2341 59.8236 5 10 -2 -4-68.5382 65.9059 4 -10 2 3-14.6496 94.4233 5 10 -2 -3 24.5769 65.7551 4 -10 2 2-8.82136 58.3121 5 10 -2 -2 86.1517 103.908 4 10 -2 -1 112.858 90.1988 4 -10 2 0-66.3721 92.2851 6 10 -2 0 86.7288 96.7759 4 -10 2 -1-8.36760 47.8565 6 10 -2 1 55.3639 54.3563 4 -10 2 -2-50.1646 113.327 6 10 -2 2 101.903 118.157 4 -10 2 -3 122.462 165.127 6 10 -2 3 314.354 162.546 4 -10 2 -4-82.9333 101.302 6 10 -2 4 8.37761 71.4948 4 -10 2 -5-40.7813 75.7464 6 10 -1 -6 70.0277 84.8423 3 10 -1 -6-122.001 95.2003 4 10 -1 -5 1.63683 41.1957 3 10 -1 -5 55.3168 73.8290 4 10 -1 -4 98.1972 114.565 4 10 -1 -3 302.877 149.319 4 10 -1 -2 21.8520 52.6275 4 10 -1 -1-16.3517 64.3610 4 -10 1 0-90.5350 100.511 6 10 -1 0 0.79777 34.7104 4 -10 1 -1-48.9559 77.7378 6 10 -1 1-43.2944 58.8400 4 -10 1 -2 218.093 174.079 6 10 -1 2 124.675 109.639 4 -10 1 -3-61.0006 105.072 6 10 -1 3-0.39925 20.9041 4 -10 1 -4-32.3599 69.1930 6 10 -1 4 86.6341 91.7672 4 -10 1 -5 34.6481 179.526 6 10 -1 5 14.6610 31.8012 4 10 0 -6-21.9420 44.3376 3 10 0 -6 0.85143 32.8920 4 10 0 -5 17.4530 39.6423 3 10 0 -5 229.532 141.880 4 10 0 -4 157.362 126.634 4 10 0 -3 77.6960 128.813 4 10 0 -2 42.4954 48.6679 4 -10 0 1 4.28506 60.0295 6 10 0 -1 149.372 115.236 4 -10 0 0 119.763 163.556 6 10 0 0 127.556 109.250 4 -10 0 -1-34.0471 68.6747 6 10 0 1-60.7119 54.1296 4 -10 0 -2-44.9761 71.8231 6 10 0 2 67.0488 74.5200 4 -10 0 -3 130.058 152.658 6 10 0 3 49.6353 79.3519 4 10 0 4 10.0963 35.5285 4 10 0 5-0.09030 55.0731 4 10 1 -6 64.9689 93.1445 3 10 1 -6 234.745 151.369 4 10 1 -5-3.18071 24.4721 3 10 1 -5-23.1589 47.4229 4 10 1 -4 138.075 109.298 4 10 1 -3 61.2973 84.8150 4 10 1 -2-41.2803 29.5803 4 -10 -1 1 18.7719 65.3542 6 10 1 -1 39.6486 71.9575 4 -10 -1 0-59.5275 101.370 6 10 1 0 70.4336 90.7698 4 -10 -1 -1 31.6387 106.638 6 10 1 1-74.9056 99.2837 4 -10 -1 -2-8.06112 87.3330 6 10 1 2 91.2225 93.2090 4 10 1 3-31.3406 56.1887 4 10 1 4-18.2173 45.7976 4 10 2 -5-51.4965 64.1050 3 10 2 -5-42.9879 67.7816 4 10 2 -4 44.6549 92.1580 4 10 2 -3 124.450 110.806 4 10 2 -2 167.990 132.284 4 -10 -2 1 18.9603 43.7720 6 10 2 -1-71.2494 66.2697 4 -10 -2 0 29.9094 130.985 6 10 2 0-53.1831 82.7902 4 10 2 1-51.1320 110.300 4 10 2 2 19.7572 57.3420 4 10 3 -4 13.5380 52.4808 3 10 4 -4 45.0458 74.3270 3 -11 6 4-19.5525 27.9875 5 -11 6 3 9.37714 55.9178 5 -11 6 2 203.759 151.712 5 -11 6 1 35.2352 100.670 5 -11 6 0 10.4514 59.7078 5 -11 5 4 106.224 94.0803 5 -11 5 3-12.6134 38.1709 5 -11 5 2 153.725 111.450 5 11 -5 -1 41.1863 54.4517 4 -11 5 1 13.4197 85.9330 5 11 -5 0-63.8512 75.1185 4 -11 5 0 168.017 119.820 5 11 -5 1-94.8201 80.9617 4 -11 5 -1-77.4010 71.8931 5 11 -5 2-169.200 105.297 4 11 -5 3-3.38976 23.9084 4 -11 5 -3 86.5985 74.5368 6 -11 4 4 151.150 126.170 5 -11 4 3-48.6040 80.6087 5 11 -4 -2-83.9704 115.116 4 -11 4 2-197.701 129.872 5 11 -4 -1-78.7834 82.2625 4 -11 4 1 31.8084 41.9288 5 -11 4 0-77.3279 109.251 5 11 -4 0 60.9280 43.5050 4 -11 4 -1-3.48588 104.743 5 11 -4 1-80.6158 76.8801 4 -11 4 -2-67.9356 88.5548 6 11 -4 2 0.07720 73.0912 4 -11 4 -3 1.91087 74.2372 6 11 -4 3 35.6654 58.3498 4 -11 4 -4-210.894 158.624 6 -11 4 -5 8.24229 81.7002 6 -11 3 4 15.6093 53.0336 5 -11 3 3-36.9076 31.1311 5 -11 3 2-132.536 108.074 5 11 -3 -2 50.0324 21.3540 4 -11 3 1-260.485 152.422 5 11 -3 -1 22.2885 66.6912 4 11 -3 0 191.286 129.053 4 -11 3 -1 185.893 174.082 6 11 -3 1 236.728 156.054 4 -11 3 -2 29.7300 80.9739 6 11 -3 2 84.4898 87.6956 4 -11 3 -3 45.4253 74.8575 6 11 -3 3 60.3763 89.8401 4 -11 3 -4-48.0550 81.7933 6 11 -3 4 72.7899 85.6822 4 11 -2 -2 93.3672 95.3193 4 11 -2 -1 219.922 147.557 4 11 -2 0 90.4771 88.9206 4 -11 2 -1 92.2478 130.637 6 11 -2 1 188.767 134.435 4 -11 2 -2 141.801 146.935 6 11 -2 2 193.841 138.731 4 11 -2 3 101.381 102.532 4 11 -2 4-62.1231 70.8463 4 11 -1 -1 176.404 140.091 4 -11 1 0 42.7989 123.358 6 11 -1 0 72.6382 91.6056 4 -11 1 -1 58.6060 89.7324 6 11 -1 1-113.092 97.2469 4 11 -1 2 61.2106 110.467 4 11 -1 3-45.8108 63.7700 4 0 0 0 0.00 0.00 0 TITL exp_2318 in P-1 REM P-1 (#2 in standard setting) CELL 0.71073 8.849063 10.930353 10.973584 105.2486 93.0741 103.9664 ZERR 2.00 0.000731 0.001499 0.000958 0.0097 0.0071 0.0092 LATT 1 SFAC C H N O UNIT 40.00 40.00 12.00 16.00 TREF HKLF 4 END ; _shelx_hkl_checksum 34815 data_L1.DMSO _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H13 N3 O5, C2 H6 O S' _chemical_formula_sum 'C17 H19 N3 O6 S' _chemical_formula_weight 393.41 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 8.2476(16) _cell_length_b 9.1570(17) _cell_length_c 13.002(3) _cell_angle_alpha 80.729(15) _cell_angle_beta 80.544(14) _cell_angle_gamma 80.501(14) _cell_volume 946.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 1381 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 20.37 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.381 _exptl_crystal_F_000 412 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 0.210 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_T_max 0.975 _exptl_absorpt_process_details multi-scan _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9645 _diffrn_reflns_av_unetI/netI 0.0828 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.603 _diffrn_reflns_theta_max 25.045 _diffrn_reflns_theta_full 25.045 _diffrn_measured_fraction_theta_max 0.951 _diffrn_measured_fraction_theta_full 0.951 _diffrn_reflns_Laue_measured_fraction_max 0.951 _diffrn_reflns_Laue_measured_fraction_full 0.951 _diffrn_reflns_point_group_measured_fraction_max 0.951 _diffrn_reflns_point_group_measured_fraction_full 0.951 _reflns_number_total 3191 _reflns_number_gt 1878 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0100P)^2^+1.5000P] 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 3191 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1280 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1689 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.1512(2) 0.32459(15) 0.16755(12) 0.0819(5) Uani 1 1 d . . . . . C10 C -0.0512(6) 0.6980(5) 0.4075(3) 0.0526(11) Uani 1 1 d . . . . . C2 C 1.0047(6) 0.8166(5) 0.0985(4) 0.0612(12) Uani 1 1 d . . . . . C5 C 0.6350(6) 0.6089(5) 0.1681(4) 0.0647(13) Uani 1 1 d . . . . . H5 H 0.6030 0.5209 0.1562 0.078 Uiso 1 1 calc R U . . . C6 C 0.5242(6) 0.7034(5) 0.2287(3) 0.0532(11) Uani 1 1 d . . . . . C3 C 0.8408(6) 0.7720(5) 0.1426(3) 0.0549(12) Uani 1 1 d . . . . . C14 C -0.2539(6) 0.8527(5) 0.5130(4) 0.0636(13) Uani 1 1 d . . . . . H14 H -0.2879 0.9413 0.5417 0.076 Uiso 1 1 calc R U . . . C13 C -0.3551(6) 0.7431(5) 0.5322(4) 0.0565(12) Uani 1 1 d . . . . . C9 C 0.2363(6) 0.7379(5) 0.3272(4) 0.0573(12) Uani 1 1 d . . . . . C8 C 0.7301(6) 0.8647(5) 0.2057(4) 0.0587(12) Uani 1 1 d . . . . . H8 H 0.7628 0.9514 0.2192 0.070 Uiso 1 1 calc R U . . . C7 C 0.5751(6) 0.8321(5) 0.2485(4) 0.0596(12) Uani 1 1 d . . . . . H7 H 0.5044 0.8957 0.2907 0.072 Uiso 1 1 calc R U . . . C11 C -0.1578(6) 0.5903(5) 0.4270(4) 0.0578(12) Uani 1 1 d . . . . . H11 H -0.1260 0.5023 0.3972 0.069 Uiso 1 1 calc R U . . . C12 C -0.3080(6) 0.6117(5) 0.4888(4) 0.0620(13) Uani 1 1 d . . . . . H12 H -0.3778 0.5387 0.5016 0.074 Uiso 1 1 calc R U . . . C4 C 0.7907(6) 0.6417(5) 0.1252(4) 0.0613(13) Uani 1 1 d . . . . . H4 H 0.8624 0.5767 0.0846 0.074 Uiso 1 1 calc R U . . . C15 C -0.1020(6) 0.8304(5) 0.4509(4) 0.0618(13) Uani 1 1 d . . . . . H15 H -0.0332 0.9042 0.4378 0.074 Uiso 1 1 calc R U . . . C1 C 1.2582(7) 0.7549(7) -0.0081(5) 0.101(2) Uani 1 1 d . . . . . H1A H 1.2487 0.8523 -0.0489 0.151 Uiso 1 1 calc R U . . . H1B H 1.3113 0.6818 -0.0528 0.151 Uiso 1 1 calc R U . . . H1C H 1.3232 0.7533 0.0470 0.151 Uiso 1 1 calc R U . . . C16 C 0.3070(7) 0.1737(6) 0.1397(5) 0.0939(19) Uani 1 1 d . . . . . H16A H 0.3992 0.2108 0.0936 0.141 Uiso 1 1 calc R U . . . H16B H 0.2630 0.1058 0.1062 0.141 Uiso 1 1 calc R U . . . H16C H 0.3436 0.1224 0.2040 0.141 Uiso 1 1 calc R U . . . C17 C 0.0049(8) 0.2236(7) 0.2514(5) 0.107(2) Uani 1 1 d . . . . . H17A H 0.0566 0.1634 0.3079 0.160 Uiso 1 1 calc R U . . . H17B H -0.0354 0.1602 0.2122 0.160 Uiso 1 1 calc R U . . . H17C H -0.0862 0.2921 0.2796 0.160 Uiso 1 1 calc R U . . . O5 O 1.0953(4) 0.7207(4) 0.0374(3) 0.0775(10) Uani 1 1 d . . . . . O4 O 1.0553(4) 0.9243(4) 0.1158(3) 0.0846(11) Uani 1 1 d . . . . . O3 O 0.2411(4) 0.8528(4) 0.3603(3) 0.0815(11) Uani 1 1 d . . . . . O2 O -0.5517(5) 0.8745(4) 0.6442(3) 0.0990(13) Uani 1 1 d . . . . . O6 O 0.2196(5) 0.4101(4) 0.2352(3) 0.0897(12) Uani 1 1 d . . . . . O1 O -0.6028(5) 0.6661(5) 0.6142(4) 0.1105(15) Uani 1 1 d . . . . . N2 N 0.3679(5) 0.6618(4) 0.2678(3) 0.0624(11) Uani 1 1 d . . . . . H2 H 0.3514 0.5777 0.2530 0.075 Uiso 1 1 calc R U . . . N1 N 0.0997(5) 0.6644(4) 0.3447(3) 0.0594(10) Uani 1 1 d . . . . . H1 H 0.1088 0.5877 0.3127 0.071 Uiso 1 1 calc R U . . . N3 N -0.5134(5) 0.7630(5) 0.6008(4) 0.0727(12) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S1 0.0901(11) 0.0661(8) 0.0941(11) -0.0254(7) -0.0116(8) -0.0122(7) C10 0.049(3) 0.052(2) 0.059(3) -0.012(2) -0.007(2) -0.010(2) C2 0.062(3) 0.063(3) 0.061(3) -0.010(2) -0.012(3) -0.012(3) C5 0.070(4) 0.051(3) 0.077(3) -0.020(2) 0.002(3) -0.020(2) C6 0.056(3) 0.048(2) 0.058(3) -0.008(2) -0.008(2) -0.012(2) C3 0.052(3) 0.055(3) 0.059(3) -0.006(2) -0.008(2) -0.013(2) C14 0.064(3) 0.052(3) 0.078(3) -0.019(2) -0.006(3) -0.011(2) C13 0.052(3) 0.056(3) 0.064(3) -0.015(2) -0.004(2) -0.011(2) C9 0.054(3) 0.052(3) 0.068(3) -0.013(2) -0.009(2) -0.011(2) C8 0.056(3) 0.051(3) 0.074(3) -0.011(2) -0.014(3) -0.014(2) C7 0.057(3) 0.054(3) 0.071(3) -0.017(2) -0.008(3) -0.011(2) C11 0.055(3) 0.050(3) 0.072(3) -0.016(2) -0.006(3) -0.011(2) C12 0.055(3) 0.055(3) 0.081(3) -0.015(2) -0.009(3) -0.015(2) C4 0.065(3) 0.056(3) 0.063(3) -0.017(2) 0.001(3) -0.011(2) C15 0.067(3) 0.050(3) 0.071(3) -0.014(2) -0.002(3) -0.020(2) C1 0.069(4) 0.118(5) 0.116(5) -0.033(4) 0.011(4) -0.025(4) C16 0.075(4) 0.078(4) 0.136(5) -0.041(4) -0.009(4) -0.010(3) C17 0.093(5) 0.116(5) 0.124(5) -0.047(4) 0.016(4) -0.052(4) O5 0.057(2) 0.079(2) 0.098(3) -0.027(2) 0.008(2) -0.0191(18) O4 0.075(3) 0.085(2) 0.104(3) -0.034(2) 0.002(2) -0.035(2) O3 0.068(2) 0.071(2) 0.116(3) -0.048(2) 0.007(2) -0.0248(18) O2 0.080(3) 0.087(3) 0.134(4) -0.061(3) 0.017(2) -0.012(2) O6 0.096(3) 0.070(2) 0.117(3) -0.042(2) -0.009(2) -0.032(2) O1 0.079(3) 0.096(3) 0.160(4) -0.063(3) 0.037(3) -0.036(2) N2 0.062(3) 0.049(2) 0.080(3) -0.0211(19) 0.001(2) -0.0173(19) N1 0.060(3) 0.052(2) 0.071(3) -0.0189(19) -0.002(2) -0.0179(18) N3 0.058(3) 0.072(3) 0.091(3) -0.028(2) -0.001(2) -0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O6 1.495(4) . ? S1 C17 1.764(6) . ? S1 C16 1.765(5) . ? C10 N1 1.390(5) . ? C10 C15 1.392(6) . ? C10 C11 1.394(6) . ? C2 O4 1.198(5) . ? C2 O5 1.333(6) . ? C2 C3 1.474(6) . ? C5 C4 1.375(6) . ? C5 C6 1.389(6) . ? C6 C7 1.389(6) . ? C6 N2 1.396(6) . ? C3 C4 1.387(6) . ? C3 C8 1.397(6) . ? C14 C13 1.376(6) . ? C14 C15 1.378(6) . ? C13 C12 1.382(6) . ? C13 N3 1.458(6) . ? C9 O3 1.208(5) . ? C9 N1 1.375(5) . ? C9 N2 1.381(5) . ? C8 C7 1.368(6) . ? C11 C12 1.365(6) . ? C1 O5 1.439(6) . ? O2 N3 1.217(5) . ? O1 N3 1.218(5) . ? 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 O6 S1 C17 106.6(3) . . ? O6 S1 C16 106.0(3) . . ? C17 S1 C16 98.8(3) . . ? N1 C10 C15 124.7(4) . . ? N1 C10 C11 116.6(4) . . ? C15 C10 C11 118.7(4) . . ? O4 C2 O5 122.5(5) . . ? O4 C2 C3 125.3(5) . . ? O5 C2 C3 112.2(4) . . ? C4 C5 C6 121.7(4) . . ? C5 C6 C7 118.6(4) . . ? C5 C6 N2 117.7(4) . . ? C7 C6 N2 123.7(4) . . ? C4 C3 C8 118.0(4) . . ? C4 C3 C2 123.4(4) . . ? C8 C3 C2 118.6(4) . . ? C13 C14 C15 119.6(4) . . ? C14 C13 C12 121.0(4) . . ? C14 C13 N3 120.2(4) . . ? C12 C13 N3 118.8(4) . . ? O3 C9 N1 124.5(4) . . ? O3 C9 N2 124.5(4) . . ? N1 C9 N2 111.0(4) . . ? C7 C8 C3 122.2(4) . . ? C8 C7 C6 119.5(4) . . ? C12 C11 C10 121.2(4) . . ? C11 C12 C13 119.2(4) . . ? C5 C4 C3 119.9(4) . . ? C14 C15 C10 120.3(4) . . ? C2 O5 C1 115.9(4) . . ? C9 N2 C6 128.5(4) . . ? C9 N1 C10 128.4(4) . . ? O2 N3 O1 121.8(4) . . ? O2 N3 C13 119.3(4) . . ? O1 N3 C13 118.9(4) . . ? _refine_diff_density_max 1.247 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.056 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL 1 in P-1 CELL 0.71073 8.2476 9.1570 13.0019 80.729 80.544 80.501 ZERR 2.00 0.0016 0.0017 0.0026 0.015 0.014 0.014 LATT 1 SFAC C H N O S UNIT 34 38 6 12 2 OMIT -3 50.1 L.S. 10 ACTA BOND FMAP 2 PLAN 1 TEMP 23.000 WGHT 0.010000 1.500000 FVAR 0.41662 MOLE 1 S1 5 0.151215 0.324593 0.167551 11.00000 0.09012 0.06612 = 0.09413 -0.02545 -0.01158 -0.01218 C10 1 -0.051163 0.698019 0.407546 11.00000 0.04899 0.05169 = 0.05940 -0.01190 -0.00714 -0.00973 C2 1 1.004679 0.816625 0.098500 11.00000 0.06164 0.06334 = 0.06098 -0.00985 -0.01162 -0.01198 C5 1 0.634993 0.608862 0.168108 11.00000 0.07003 0.05056 = 0.07700 -0.02029 0.00249 -0.02015 AFIX 43 H5 2 0.603017 0.520948 0.156238 11.00000 -1.20000 AFIX 0 C6 1 0.524150 0.703449 0.228685 11.00000 0.05592 0.04770 = 0.05776 -0.00761 -0.00832 -0.01165 C3 1 0.840803 0.772032 0.142558 11.00000 0.05179 0.05501 = 0.05947 -0.00616 -0.00815 -0.01317 C14 1 -0.253930 0.852702 0.512965 11.00000 0.06433 0.05195 = 0.07763 -0.01949 -0.00649 -0.01084 AFIX 43 H14 2 -0.287867 0.941336 0.541689 11.00000 -1.20000 AFIX 0 C13 1 -0.355086 0.743117 0.532234 11.00000 0.05182 0.05569 = 0.06404 -0.01516 -0.00392 -0.01073 C9 1 0.236314 0.737865 0.327195 11.00000 0.05446 0.05243 = 0.06793 -0.01332 -0.00872 -0.01118 C8 1 0.730086 0.864674 0.205747 11.00000 0.05572 0.05126 = 0.07401 -0.01112 -0.01389 -0.01425 AFIX 43 H8 2 0.762832 0.951398 0.219161 11.00000 -1.20000 AFIX 0 C7 1 0.575148 0.832126 0.248548 11.00000 0.05723 0.05420 = 0.07099 -0.01730 -0.00811 -0.01060 AFIX 43 H7 2 0.504410 0.895709 0.290667 11.00000 -1.20000 AFIX 0 C11 1 -0.157785 0.590323 0.426973 11.00000 0.05508 0.04985 = 0.07158 -0.01650 -0.00625 -0.01111 AFIX 43 H11 2 -0.126013 0.502312 0.397249 11.00000 -1.20000 AFIX 0 C12 1 -0.308014 0.611687 0.488843 11.00000 0.05516 0.05468 = 0.08055 -0.01503 -0.00869 -0.01543 AFIX 43 H12 2 -0.377791 0.538725 0.501629 11.00000 -1.20000 AFIX 0 C4 1 0.790731 0.641728 0.125220 11.00000 0.06466 0.05645 = 0.06304 -0.01721 0.00092 -0.01093 AFIX 43 H4 2 0.862427 0.576717 0.084642 11.00000 -1.20000 AFIX 0 C15 1 -0.101996 0.830437 0.450855 11.00000 0.06747 0.05013 = 0.07118 -0.01427 -0.00217 -0.01969 AFIX 43 H15 2 -0.033175 0.904179 0.437833 11.00000 -1.20000 AFIX 0 C1 1 1.258173 0.754874 -0.008100 11.00000 0.06907 0.11776 = 0.11616 -0.03321 0.01123 -0.02456 AFIX 137 H1A 2 1.248693 0.852330 -0.048865 11.00000 -1.50000 H1B 2 1.311315 0.681833 -0.052774 11.00000 -1.50000 H1C 2 1.323182 0.753288 0.047019 11.00000 -1.50000 AFIX 0 C16 1 0.307018 0.173704 0.139665 11.00000 0.07458 0.07777 = 0.13578 -0.04069 -0.00881 -0.00985 AFIX 137 H16A 2 0.399167 0.210810 0.093625 11.00000 -1.50000 H16B 2 0.263032 0.105797 0.106167 11.00000 -1.50000 H16C 2 0.343614 0.122420 0.204031 11.00000 -1.50000 AFIX 0 C17 1 0.004864 0.223566 0.251381 11.00000 0.09260 0.11594 = 0.12361 -0.04700 0.01575 -0.05200 AFIX 137 H17A 2 0.056644 0.163401 0.307936 11.00000 -1.50000 H17B 2 -0.035450 0.160204 0.212180 11.00000 -1.50000 H17C 2 -0.086242 0.292116 0.279644 11.00000 -1.50000 AFIX 0 O5 4 1.095272 0.720656 0.037351 11.00000 0.05732 0.07931 = 0.09791 -0.02716 0.00752 -0.01906 O4 4 1.055312 0.924317 0.115815 11.00000 0.07515 0.08514 = 0.10378 -0.03422 0.00207 -0.03517 O3 4 0.241126 0.852764 0.360286 11.00000 0.06750 0.07104 = 0.11617 -0.04850 0.00713 -0.02479 O2 4 -0.551712 0.874522 0.644177 11.00000 0.08032 0.08705 = 0.13437 -0.06147 0.01690 -0.01245 O6 4 0.219639 0.410089 0.235222 11.00000 0.09637 0.07046 = 0.11688 -0.04226 -0.00882 -0.03154 O1 4 -0.602778 0.666136 0.614166 11.00000 0.07947 0.09630 = 0.16042 -0.06311 0.03727 -0.03572 N2 3 0.367904 0.661770 0.267815 11.00000 0.06227 0.04868 = 0.07964 -0.02107 0.00138 -0.01729 AFIX 43 H2 2 0.351431 0.577667 0.252999 11.00000 -1.20000 AFIX 0 N1 3 0.099718 0.664388 0.344725 11.00000 0.05980 0.05201 = 0.07072 -0.01894 -0.00167 -0.01795 AFIX 43 H1 2 0.108830 0.587674 0.312657 11.00000 -1.20000 AFIX 0 N3 3 -0.513409 0.763003 0.600810 11.00000 0.05791 0.07174 = 0.09144 -0.02775 -0.00143 -0.01077 HKLF 4 REM 1 in P-1 REM R1 = 0.0790 for 1878 Fo > 4sig(Fo) and 0.1280 for all 3191 data REM 247 parameters refined using 0 restraints END WGHT 0.0867 0.9496 REM Highest difference peak 1.247, deepest hole -0.358, 1-sigma level 0.056 Q1 1 0.2107 0.2353 0.2505 11.00000 0.05 1.25 ; _shelx_res_checksum 48993 _shelx_hkl_file ; 1 0 0 91.15 11.58 1 0 0 92.61 11.58 1 0 0 92.72 10.74 -1 0 0 90.60 10.73 -1 0 0 92.83 11.58 -1 0 0 94.50 11.58 -2 0 0 69.16 8.72 -2 0 0 68.66 8.06 2 0 0 69.42 8.06 3 0 0 15.99 2.01 -3 0 0 13.86 1.89 3 0 0 12.28 1.71 -3 0 0 13.69 1.69 4 0 0 -0.14 0.40 -4 0 0 0.32 0.23 -4 0 0 0.36 0.39 4 0 0 0.77 0.40 5 0 0 0.24 0.61 -5 0 0 0.44 0.35 -5 0 0 0.03 0.46 -6 0 0 1.03 0.58 6 0 0 1.34 0.91 -7 0 0 -0.53 0.73 7 0 0 0.34 0.94 8 0 0 3.28 1.56 9 0 0 0.39 1.47 10 0 0 -0.26 1.86 10 -1 0 0.45 1.82 9 -1 0 -0.29 1.62 8 -1 0 7.70 2.01 7 -1 0 28.87 4.33 -6 1 0 15.89 2.68 6 -1 0 23.47 3.07 -5 1 0 75.50 9.11 5 -1 0 78.72 9.99 4 -1 0 74.59 8.26 -4 1 0 70.55 8.21 4 -1 0 69.30 7.34 4 -1 0 67.83 8.94 4 -1 0 66.91 7.33 3 -1 0 0.16 0.22 3 -1 0 1.14 0.40 -3 1 0 0.27 0.27 3 -1 0 0.49 0.40 -3 1 0 0.51 0.34 2 -1 0 208.95 26.23 2 -1 0 208.50 21.93 2 -1 0 208.24 24.23 -2 1 0 203.62 24.22 -2 1 0 211.81 26.08 1 -1 0 293.45 34.12 -1 1 0 298.87 36.75 -1 1 0 289.19 34.12 0 -1 0 59.35 8.03 0 1 0 61.07 8.03 0 1 0 59.80 7.45 1 1 0 269.38 35.26 1 1 0 278.52 32.70 -1 -1 0 298.73 32.72 -2 -1 0 4.37 0.68 2 1 0 3.22 0.64 -3 -1 0 127.39 14.91 -3 -1 0 126.93 16.21 3 1 0 130.50 16.21 3 1 0 130.65 16.31 4 1 0 324.90 39.59 4 1 0 306.91 39.84 -4 -1 0 312.82 39.60 -4 -1 0 317.67 36.60 -5 -1 0 33.89 4.37 5 1 0 35.26 4.35 -5 -1 0 30.87 3.83 5 1 0 32.95 4.51 6 1 0 5.74 1.36 -6 -1 0 4.54 0.70 -6 -1 0 5.23 1.16 -7 -1 0 11.38 2.10 7 1 0 15.87 2.52 8 1 0 10.65 2.33 9 1 0 0.80 1.65 10 -2 0 -2.61 1.70 9 -2 0 0.47 1.60 8 -2 0 2.18 1.39 7 -2 0 18.45 3.14 6 -2 0 2.55 1.02 -6 2 0 1.13 0.74 5 -2 0 2.72 0.91 -5 2 0 3.20 0.80 5 -2 0 2.32 0.52 4 -2 0 37.90 4.48 4 -2 0 37.44 4.80 -4 2 0 42.68 4.46 4 -2 0 32.65 3.92 -4 2 0 32.38 4.70 3 -2 0 52.15 5.44 3 -2 0 52.04 6.54 -3 2 0 49.61 6.05 -3 2 0 47.77 6.47 3 -2 0 50.57 6.08 -2 2 0 187.89 21.30 -2 2 0 179.58 22.90 2 -2 0 185.25 19.27 2 -2 0 179.95 23.02 2 -2 0 180.44 21.30 1 -2 0 92.70 11.78 1 -2 0 91.71 10.92 -1 2 0 96.32 10.92 1 -2 0 94.34 9.88 -1 2 0 90.24 11.73 0 2 0 2608.12 300.16 0 2 0 2630.47 269.14 0 2 0 2605.64 323.45 0 2 0 2530.83 272.09 1 2 0 19.45 2.59 -1 -2 0 19.02 2.11 -1 -2 0 20.05 2.37 1 2 0 20.39 2.11 2 2 0 63.84 8.37 -2 -2 0 68.11 7.62 2 2 0 62.72 8.33 -2 -2 0 65.11 8.34 -2 -2 0 64.42 7.62 -2 -2 0 66.49 6.83 -3 -2 0 6.01 1.27 3 2 0 9.53 1.33 3 2 0 10.18 1.41 -4 -2 0 80.01 10.07 4 2 0 84.05 10.15 4 2 0 72.78 10.02 5 2 0 6.25 1.39 5 2 0 7.19 1.33 -5 -2 0 7.66 1.33 6 2 0 3.75 1.16 6 2 0 3.69 0.97 -6 -2 0 1.14 0.78 7 2 0 31.98 4.03 -7 -2 0 21.63 3.62 8 2 0 7.40 2.11 10 -3 0 -1.09 1.76 9 -3 0 0.78 1.54 8 -3 0 1.40 1.26 7 -3 0 11.79 1.39 7 -3 0 12.76 2.44 -6 3 0 2.39 0.92 6 -3 0 1.91 0.54 6 -3 0 2.22 1.01 5 -3 0 0.74 0.78 -5 3 0 1.08 0.65 5 -3 0 0.48 0.42 4 -3 0 102.02 10.95 4 -3 0 102.10 13.14 -4 3 0 103.04 13.03 -3 3 0 179.42 20.84 3 -3 0 175.75 22.50 -3 3 0 178.29 18.80 3 -3 0 175.87 18.84 3 -3 0 179.77 20.86 -2 3 0 1.71 0.59 -2 3 0 2.38 0.47 2 -3 0 3.91 0.74 2 -3 0 2.16 0.51 -2 3 0 3.51 0.72 2 -3 0 2.72 0.67 -1 3 0 236.02 24.64 1 -3 0 234.68 24.68 -1 3 0 237.66 29.34 1 -3 0 226.00 29.45 1 -3 0 236.21 27.27 0 3 0 22.64 3.20 0 3 0 25.20 2.64 0 3 0 24.34 2.65 0 -3 0 24.29 3.16 1 3 0 79.81 8.43 1 3 0 81.49 10.20 -1 -3 0 80.22 10.18 1 3 0 79.97 8.48 -1 -3 0 80.64 9.43 2 3 0 0.39 0.37 -2 -3 0 0.20 0.17 -2 -3 0 0.96 0.26 -2 -3 0 0.43 0.29 2 3 0 0.62 0.36 -3 -3 0 64.16 6.72 -3 -3 0 65.09 8.25 3 3 0 61.41 8.29 3 3 0 67.00 8.28 -4 -3 0 204.89 26.62 4 3 0 225.58 26.79 4 3 0 204.01 26.61 5 3 0 0.73 0.61 -5 -3 0 1.91 0.72 5 3 0 -0.12 0.71 6 3 0 19.06 2.61 6 3 0 17.65 2.75 -6 -3 0 12.68 2.49 7 3 0 1.06 0.91 7 3 0 0.30 1.07 -7 -3 0 0.83 0.82 8 3 0 0.83 1.40 9 -4 0 1.67 1.85 8 -4 0 -1.72 1.28 7 -4 0 -0.68 0.91 7 -4 0 0.62 0.49 6 -4 0 1.04 0.52 -6 4 0 1.59 0.86 6 -4 0 -0.03 0.93 -5 4 0 3.07 0.93 5 -4 0 1.90 0.79 5 -4 0 0.19 0.50 4 -4 0 2.88 0.89 -4 4 0 1.84 0.80 4 -4 0 2.54 0.66 -3 4 0 23.02 2.84 -3 4 0 26.58 3.50 3 -4 0 29.18 3.46 3 -4 0 19.17 3.28 3 -4 0 26.86 2.95 2 -4 0 94.55 12.75 -2 4 0 103.68 10.66 -2 4 0 98.32 12.72 2 -4 0 100.64 11.88 2 -4 0 102.70 10.72 -1 4 0 40.09 5.32 -1 4 0 39.19 4.40 1 -4 0 43.80 4.49 1 -4 0 42.89 5.29 1 -4 0 37.66 4.97 -1 4 0 39.90 4.43 0 4 0 219.80 22.90 0 4 0 223.30 22.72 0 4 0 212.22 27.32 0 -4 0 213.94 27.39 -1 -4 0 193.94 22.28 1 4 0 190.93 19.95 1 4 0 191.83 20.10 1 4 0 187.74 24.04 -1 -4 0 190.06 24.07 2 4 0 28.21 3.10 2 4 0 29.79 3.89 -2 -4 0 29.77 3.81 -2 -4 0 28.08 3.51 2 4 0 30.39 3.90 3 4 0 41.62 5.61 -3 -4 0 42.27 4.52 -3 -4 0 44.22 5.05 -3 -4 0 39.81 5.52 3 4 0 45.22 5.62 -3 -4 0 42.48 5.03 4 4 0 31.29 4.43 -4 -4 0 31.63 4.32 -4 -4 0 30.60 4.46 4 4 0 31.89 4.40 -4 -4 0 34.02 3.45 -5 -4 0 1.43 0.76 5 4 0 1.99 0.75 -5 -4 0 1.38 0.78 5 4 0 0.44 0.80 -6 -4 0 19.01 2.65 6 4 0 20.29 2.83 -6 -4 0 10.26 2.36 6 4 0 17.62 2.59 -7 -4 0 8.25 2.33 7 4 0 22.51 2.79 -7 -4 0 20.74 2.77 7 4 0 18.58 2.92 -8 -4 0 -0.06 1.22 8 4 0 -0.60 1.06 9 -5 0 0.12 1.90 8 -5 0 -1.08 1.26 8 -5 0 0.73 0.57 7 -5 0 -0.79 1.12 7 -5 0 -0.13 0.55 6 -5 0 8.45 1.97 6 -5 0 8.18 1.40 -5 5 0 0.93 0.92 5 -5 0 0.36 0.78 5 -5 0 0.44 0.55 -4 5 0 0.34 0.77 4 -5 0 -0.71 0.49 4 -5 0 -0.64 0.52 -3 5 0 26.15 2.70 -3 5 0 20.96 3.24 3 -5 0 22.42 2.75 3 -5 0 33.24 3.36 3 -5 0 16.18 3.19 -2 5 0 83.97 8.90 2 -5 0 87.84 9.00 -2 5 0 79.60 8.89 -2 5 0 83.40 10.67 2 -5 0 83.13 9.99 2 -5 0 79.67 10.66 1 -5 0 27.89 3.14 1 -5 0 22.23 2.71 1 -5 0 23.77 3.18 -1 5 0 21.68 2.60 -1 5 0 20.83 3.22 -1 5 0 22.92 2.69 0 5 0 6.93 1.30 0 5 0 7.80 1.05 0 -5 0 6.96 1.19 0 -5 0 4.24 1.11 0 5 0 8.05 0.93 0 -5 0 6.76 1.06 1 5 0 9.33 1.40 1 5 0 7.42 0.99 -1 -5 0 6.93 1.17 -1 -5 0 6.11 1.14 1 5 0 6.89 0.89 2 5 0 -0.20 0.45 -2 -5 0 0.17 0.37 2 5 0 0.45 0.25 -2 -5 0 0.04 0.32 -3 -5 0 0.40 0.33 3 5 0 1.27 0.67 3 5 0 -0.03 0.52 -3 -5 0 -0.06 0.40 4 5 0 29.74 3.54 -4 -5 0 22.63 3.30 -4 -5 0 22.76 2.83 4 5 0 23.15 3.43 -4 -5 0 23.76 2.84 -5 -5 0 44.02 5.40 5 5 0 35.93 5.29 5 5 0 38.42 5.38 -5 -5 0 37.01 5.12 6 5 0 0.48 1.05 6 5 0 -0.43 0.76 -6 -5 0 -0.25 0.81 -6 -5 0 -0.15 0.77 7 5 0 0.91 1.25 -7 -5 0 3.39 1.30 7 5 0 0.86 1.06 -7 -5 0 3.69 1.31 8 5 0 1.96 1.34 8 -6 0 -0.66 0.64 8 -6 0 1.34 1.80 7 -6 0 0.52 0.74 7 -6 0 1.40 1.37 6 -6 0 0.02 0.73 6 -6 0 -0.39 0.95 5 -6 0 0.69 0.92 5 -6 0 0.38 0.67 -5 6 0 0.68 0.93 4 -6 0 11.88 1.73 4 -6 0 12.88 2.12 -4 6 0 9.05 1.96 3 -6 0 0.40 0.68 3 -6 0 -0.10 0.54 -3 6 0 1.57 0.86 -3 6 0 1.35 0.58 -2 6 0 0.34 0.40 2 -6 0 0.58 0.68 2 -6 0 0.35 0.63 -2 6 0 0.25 0.67 2 -6 0 -0.28 0.54 -1 6 0 13.90 1.73 1 -6 0 14.53 2.19 1 -6 0 17.43 2.29 1 -6 0 15.28 1.94 -1 6 0 10.67 2.21 0 -6 0 17.67 2.58 0 6 0 19.22 2.77 0 6 0 20.64 2.12 0 -6 0 15.21 2.60 -1 -6 0 6.90 1.22 1 6 0 4.24 1.21 -1 -6 0 6.32 1.17 1 6 0 7.89 0.89 2 6 0 0.61 0.53 2 6 0 0.20 0.16 -2 -6 0 0.39 0.47 -2 -6 0 0.41 0.45 3 6 0 0.12 0.64 -3 -6 0 -0.08 0.49 -3 -6 0 0.77 0.47 4 6 0 5.74 1.61 -4 -6 0 9.39 1.50 -4 -6 0 9.54 1.20 -4 -6 0 7.63 1.18 4 6 0 7.29 1.62 -5 -6 0 1.83 1.02 5 6 0 0.08 0.86 -5 -6 0 2.82 0.86 5 6 0 1.66 1.11 -6 -6 0 4.68 1.32 6 6 0 5.69 1.68 -6 -6 0 8.58 1.71 6 6 0 4.21 1.53 7 6 0 12.63 2.44 -7 -6 0 11.70 2.41 8 6 0 4.92 1.84 -8 -6 0 5.74 1.78 7 -7 0 0.62 0.89 7 -7 0 -0.02 1.37 6 -7 0 4.96 1.33 6 -7 0 6.76 1.94 -5 7 0 0.22 1.21 5 -7 0 0.32 0.87 5 -7 0 0.89 0.80 -4 7 0 0.47 0.95 4 -7 0 -0.24 0.73 4 -7 0 -0.28 0.76 -3 7 0 0.03 0.86 -3 7 0 0.24 0.48 3 -7 0 -0.20 0.66 3 -7 0 -0.08 0.64 2 -7 0 1.93 0.87 2 -7 0 1.85 0.99 -2 7 0 3.46 0.73 -2 7 0 1.40 0.99 2 -7 0 4.03 1.15 -1 7 0 0.31 0.68 1 -7 0 1.23 0.72 1 -7 0 2.85 0.95 -1 7 0 1.39 0.46 0 7 0 5.36 1.28 0 -7 0 2.60 1.02 0 7 0 5.34 0.82 0 -7 0 7.15 1.26 1 7 0 0.98 0.36 -1 -7 0 1.22 0.71 -1 -7 0 1.39 0.72 1 7 0 0.67 0.75 2 7 0 45.61 5.12 -2 -7 0 49.62 5.93 -2 -7 0 52.59 6.33 2 7 0 49.28 6.47 3 7 0 8.28 1.58 -3 -7 0 4.35 1.07 -3 -7 0 7.18 1.27 4 7 0 19.53 3.15 -4 -7 0 19.72 2.92 -4 -7 0 19.91 2.59 5 7 0 22.37 3.20 5 7 0 22.22 3.22 -5 -7 0 13.27 2.73 -5 -7 0 19.78 2.33 -6 -7 0 1.45 1.12 6 7 0 0.21 1.02 6 7 0 -0.40 1.12 -6 -7 0 0.82 0.80 7 7 0 -0.52 1.16 -7 -7 0 -0.24 1.15 -8 -7 0 1.45 1.49 8 7 0 0.42 1.46 7 -8 0 0.83 1.09 6 -8 0 -0.51 1.02 6 -8 0 -1.28 1.10 5 -8 0 1.21 0.97 5 -8 0 0.69 1.09 4 -8 0 11.06 1.90 -4 8 0 7.79 2.13 4 -8 0 10.50 2.13 -3 8 0 5.77 1.55 3 -8 0 7.35 1.41 -3 8 0 5.13 0.98 3 -8 0 2.82 1.20 -2 8 0 26.33 3.89 -2 8 0 28.43 3.08 2 -8 0 21.67 3.74 -1 8 0 1.71 0.61 1 -8 0 0.10 1.00 1 -8 0 4.72 1.10 -1 8 0 0.91 0.88 0 8 0 0.39 0.84 0 -8 0 1.82 0.95 0 8 0 0.46 0.38 0 -8 0 -0.32 0.71 -1 -8 0 29.84 4.50 1 8 0 33.73 3.58 1 8 0 33.02 4.67 -1 -8 0 31.51 4.29 -2 -8 0 1.15 0.70 -2 -8 0 0.42 0.68 2 8 0 -0.17 0.22 2 8 0 0.43 0.78 -3 -8 0 4.13 0.97 3 8 0 1.17 0.95 -3 -8 0 1.64 0.84 -4 -8 0 1.67 0.72 -4 -8 0 1.02 0.74 4 8 0 0.77 0.98 -5 -8 0 0.71 0.59 -5 -8 0 -0.34 0.80 5 8 0 0.71 0.99 -6 -8 0 1.06 1.26 6 8 0 1.08 1.28 -7 -8 0 0.03 1.37 7 8 0 -1.25 1.27 6 -9 0 -0.28 1.22 5 -9 0 1.49 1.17 5 -9 0 0.05 1.27 -4 9 0 0.54 1.42 4 -9 0 -0.15 1.02 4 -9 0 -0.96 1.10 3 -9 0 4.58 1.65 -3 9 0 6.33 1.77 -3 9 0 6.20 1.20 -2 9 0 2.21 1.23 -2 9 0 -0.35 0.59 2 -9 0 -0.20 0.92 -1 9 0 -0.55 0.97 1 -9 0 -0.74 0.78 1 -9 0 0.12 1.01 -1 9 0 0.68 0.56 0 -9 0 0.64 1.08 0 9 0 1.04 0.50 0 9 0 1.22 1.02 0 -9 0 0.92 0.88 -1 -9 0 1.94 1.04 -1 -9 0 2.46 1.19 1 9 0 2.69 0.57 1 9 0 3.25 1.21 -2 -9 0 2.96 1.03 -2 -9 0 0.06 0.78 2 9 0 1.73 0.36 2 9 0 1.09 1.02 -3 -9 0 1.90 0.92 3 9 0 1.28 1.10 -4 -9 0 10.36 1.87 4 9 0 9.32 2.13 5 9 0 0.97 1.32 -4 10 0 0.11 0.97 4 -10 0 2.29 1.51 3 -10 0 0.71 1.29 -3 10 0 -0.29 0.73 2 -10 0 8.51 2.08 1 -10 0 3.17 1.31 -1 10 0 0.70 0.62 0 -10 0 2.18 1.09 0 10 0 0.74 0.54 0 10 0 0.29 1.13 -1 -10 0 -0.54 0.90 1 10 0 0.44 0.43 1 10 0 -0.92 1.03 -2 -10 0 1.82 1.10 -3 -10 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1.05 1 5 -14 -0.83 0.60 0 5 -14 0.26 0.75 -1 5 -14 0.06 0.81 -2 5 -14 0.33 0.97 2 4 -14 -0.62 0.55 1 4 -14 1.83 0.74 0 4 -14 -0.36 0.75 -1 4 -14 -0.41 0.70 -2 4 -14 0.05 0.90 -3 4 -14 0.50 0.98 3 3 -14 0.46 0.52 2 3 -14 3.28 0.90 1 3 -14 -0.35 0.60 0 3 -14 -0.10 0.70 -1 3 -14 0.15 0.85 -2 3 -14 -0.95 0.81 3 2 -14 0.67 0.58 2 2 -14 1.13 0.67 1 2 -14 0.44 0.69 0 2 -14 0.23 0.73 -1 2 -14 1.10 0.83 -2 2 -14 0.56 0.91 6 -2 14 0.18 0.96 4 1 -14 0.22 0.48 3 1 -14 -0.94 0.53 2 1 -14 1.68 0.82 -2 -1 14 5.39 1.79 1 1 -14 -0.66 0.66 0 1 -14 0.66 0.73 -1 1 -14 1.60 0.93 -2 1 -14 -0.30 0.90 6 -1 14 -0.12 0.83 7 -1 14 0.61 0.80 4 0 -14 -0.33 0.54 3 0 -14 -0.74 0.61 -2 0 14 1.26 1.52 2 0 -14 0.00 0.65 1 0 -14 0.49 0.77 0 0 -14 1.52 0.89 -1 0 -14 1.10 0.84 7 0 14 0.44 2.07 7 0 14 0.98 0.75 4 -1 -14 -0.42 0.61 3 -1 -14 0.80 0.82 -2 1 14 -0.63 1.31 2 -1 -14 -0.30 0.73 -1 1 14 2.25 1.43 1 -1 -14 3.03 1.02 0 -1 -14 -0.26 0.75 -1 -1 -14 0.54 0.89 6 1 14 2.91 2.03 7 1 14 0.19 1.86 7 1 14 -0.83 0.59 4 -2 -14 0.77 0.77 3 -2 -14 1.86 0.88 2 -2 -14 0.18 0.77 -2 2 14 0.64 1.36 1 -2 -14 1.98 0.96 -1 2 14 3.28 1.44 0 -2 -14 11.86 1.96 1 2 14 0.69 0.77 -1 -2 -14 2.07 1.00 6 2 14 0.05 2.03 -6 -2 -14 -0.57 1.11 7 2 14 0.34 0.55 -7 -2 -14 0.66 1.30 7 2 14 -1.63 2.04 4 -3 -14 -0.60 0.73 3 -3 -14 1.14 0.89 2 -3 -14 4.33 1.22 -1 3 14 -1.37 1.04 1 -3 -14 0.96 0.87 0 -3 -14 3.08 1.13 1 3 14 0.90 0.76 5 3 14 3.37 1.93 6 3 14 3.03 2.08 -6 -3 -14 1.26 1.23 -7 -3 -14 0.21 1.17 7 3 14 0.47 2.12 4 -4 -14 0.51 0.94 3 -4 -14 0.49 0.95 2 -4 -14 1.06 0.93 -1 4 14 2.64 1.49 1 -4 -14 5.13 1.22 0 4 14 9.09 1.60 0 -4 -14 7.89 1.60 1 4 14 -0.09 0.72 2 4 14 2.48 0.83 5 4 14 -1.98 1.51 -5 -4 -14 -0.28 0.94 -6 -4 -14 0.88 1.24 6 4 14 -0.74 1.89 -7 -4 -14 2.50 1.56 7 4 14 3.04 2.35 3 -5 -14 -0.13 0.86 2 -5 -14 -0.79 0.92 1 -5 -14 0.38 0.95 0 5 14 0.41 0.78 1 5 14 -0.14 0.65 2 5 14 1.22 0.77 4 5 14 -0.92 1.67 -4 -5 -14 -0.74 0.86 -5 -5 -14 0.45 0.96 5 5 14 -0.90 1.68 6 5 14 -1.01 1.76 -6 -5 -14 0.75 1.16 7 5 14 0.99 2.25 -7 -5 -14 1.31 1.51 2 -6 -14 0.80 1.09 1 -6 -14 1.33 1.11 0 6 14 0.29 0.76 1 6 14 0.22 0.77 2 6 14 0.36 0.69 3 6 14 0.57 1.70 4 6 14 0.66 1.78 -4 -6 -14 1.71 1.09 5 6 14 0.47 1.94 -5 -6 -14 0.87 1.16 6 6 14 -0.85 1.94 -6 -6 -14 -0.13 1.16 7 6 14 1.04 2.38 -1 7 14 1.54 0.98 0 7 14 0.00 0.84 1 7 14 -0.92 0.66 2 7 14 0.24 0.70 -3 -7 -14 0.16 0.97 -4 -7 -14 0.25 1.02 4 7 14 2.33 2.02 -5 -7 -14 0.78 1.05 5 7 14 0.18 1.93 -6 -7 -14 1.83 1.39 6 7 14 2.14 2.26 0 8 14 1.02 0.90 1 8 14 0.09 0.78 2 8 14 0.09 0.68 -3 -8 -14 0.39 1.01 -4 -8 -14 0.16 1.08 5 8 14 -3.42 2.02 0 4 -15 0.75 0.87 -1 4 -15 1.19 0.97 -2 4 -15 1.45 0.99 2 3 -15 1.07 0.73 1 3 -15 0.35 0.75 0 3 -15 0.05 0.75 -1 3 -15 -0.70 0.81 -2 3 -15 -0.10 0.90 3 2 -15 0.56 0.63 2 2 -15 0.33 0.68 1 2 -15 0.76 0.78 0 2 -15 0.13 0.79 -1 2 -15 2.02 1.07 -2 2 -15 0.81 1.02 3 1 -15 1.03 0.70 2 1 -15 -0.57 0.71 1 1 -15 -1.22 0.71 0 1 -15 0.10 0.89 -1 1 -15 2.07 1.11 -2 1 -15 3.26 1.24 3 0 -15 -0.05 0.68 2 0 -15 0.78 0.85 1 0 -15 -1.12 0.83 0 0 -15 -0.90 0.86 -1 0 -15 -1.08 0.85 3 -1 -15 0.58 0.85 2 -1 -15 0.73 0.80 1 -1 -15 0.17 0.80 0 -1 -15 1.10 1.03 -1 -1 -15 0.59 1.02 3 -2 -15 -0.47 0.77 2 -2 -15 0.12 0.92 1 -2 -15 4.14 1.31 0 -2 -15 2.95 1.10 -1 -2 -15 1.59 1.01 7 2 15 -0.29 2.32 7 2 15 0.50 0.63 3 -3 -15 -1.69 0.80 2 -3 -15 0.58 0.96 1 -3 -15 -1.36 0.90 0 -3 -15 1.71 1.11 1 3 15 -0.28 0.79 7 3 15 1.96 2.44 3 -4 -15 0.92 1.15 2 -4 -15 -0.63 0.93 1 -4 -15 0.00 1.01 0 -4 -15 2.85 1.23 0 4 15 2.35 1.05 1 4 15 2.52 0.97 6 4 15 -1.89 1.95 -6 -4 -15 1.44 1.26 2 -5 -15 -0.03 1.04 1 -5 -15 -1.66 0.92 0 5 15 -0.75 0.82 1 5 15 0.66 0.83 2 5 15 0.94 0.76 5 5 15 -1.59 1.77 -6 -5 -15 -0.32 1.20 6 5 15 -2.73 2.10 1 -6 -15 1.36 1.24 0 6 15 0.57 0.83 1 6 15 1.45 0.92 2 6 15 1.12 0.85 -5 -6 -15 0.62 1.23 5 6 15 -0.24 1.95 0 7 15 2.27 1.06 1 7 15 0.72 0.95 2 7 15 -0.86 0.74 4 7 15 -1.17 2.00 1 2 -16 1.42 0.96 0 2 -16 0.93 0.95 -1 2 -16 -0.87 0.89 -2 2 -16 -0.88 1.10 1 1 -16 0.75 0.88 0 1 -16 0.05 0.93 -1 1 -16 -0.87 0.93 -2 1 -16 0.98 1.17 2 0 -16 0.98 0.96 1 0 -16 0.64 0.95 0 0 -16 0.32 0.95 -1 0 -16 0.65 1.04 2 -1 -16 -0.33 0.95 1 -1 -16 0.07 0.87 0 -1 -16 -0.21 1.00 -1 -1 -16 -0.07 1.09 2 -2 -16 0.20 1.00 1 -2 -16 -0.80 0.93 0 -2 -16 0.35 1.04 -1 -2 -16 -2.11 0.92 2 -3 -16 0.36 1.05 1 -3 -16 -0.87 0.95 0 -3 -16 0.19 1.02 1 3 16 1.52 0.99 1 -4 -16 0.19 1.11 0 -4 -16 -1.13 1.03 1 4 16 0.46 0.92 0 5 16 0.79 1.04 1 5 16 -0.19 0.91 1 6 16 0.30 0.94 2 6 16 1.15 0.87 -1 0 -17 0.01 1.19 0 -1 -17 0.22 1.03 -1 -1 -17 1.55 1.28 0 -2 -17 0.09 1.12 1 4 17 0.59 1.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 49336 data_L2.DMSO _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H19 N3 O5 S2' _chemical_formula_sum 'C17 H19 N3 O5 S2' _chemical_formula_weight 409.47 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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 8.9102(6) _cell_length_b 9.9426(7) _cell_length_c 11.7194(8) _cell_angle_alpha 91.392(4) _cell_angle_beta 104.200(4) _cell_angle_gamma 106.984(4) _cell_volume 957.44(12) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2024 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 19.95 _exptl_crystal_description Needle _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_F_000 428 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 0.312 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.914 _exptl_absorpt_correction_T_max 0.963 _exptl_absorpt_process_details multi-scan _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11484 _diffrn_reflns_av_unetI/netI 0.0523 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.802 _diffrn_reflns_theta_max 25.050 _diffrn_reflns_theta_full 25.050 _diffrn_measured_fraction_theta_max 0.947 _diffrn_measured_fraction_theta_full 0.947 _diffrn_reflns_Laue_measured_fraction_max 0.947 _diffrn_reflns_Laue_measured_fraction_full 0.947 _diffrn_reflns_point_group_measured_fraction_max 0.947 _diffrn_reflns_point_group_measured_fraction_full 0.947 _reflns_number_total 3215 _reflns_number_gt 1874 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0780P)^2^] 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 3215 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.1478 _refine_ls_wR_factor_gt 0.1255 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group S1 S 0.19053(11) 0.40342(9) 0.91548(8) 0.0689(3) Uani 1 1 d . . . . . S2 S 0.03126(12) 0.98266(9) 0.85400(8) 0.0733(4) Uani 1 1 d . . . . . N2 N 0.1778(3) 0.6573(2) 0.9871(2) 0.0564(7) Uani 1 1 d . . . . . H2 H 0.1274 0.7190 0.9702 0.068 Uiso 1 1 calc R U . . . N3 N 0.0205(3) 0.5681(2) 0.8047(2) 0.0582(7) Uani 1 1 d . . . . . H3 H -0.0020 0.6456 0.8129 0.070 Uiso 1 1 calc R U . . . N1 N 0.6292(4) 0.8237(3) 1.4320(3) 0.0705(8) Uani 1 1 d . . . . . O4 O -0.4529(3) 0.3198(3) 0.30201(19) 0.0818(8) Uani 1 1 d . . . . . O5 O -0.0205(3) 0.8294(2) 0.8729(2) 0.0762(7) Uani 1 1 d . . . . . O3 O -0.2983(3) 0.1797(3) 0.3078(2) 0.0936(9) Uani 1 1 d . . . . . O2 O 0.6075(3) 0.9031(3) 1.5012(2) 0.1047(10) Uani 1 1 d . . . . . O1 O 0.7479(3) 0.7806(3) 1.4541(2) 0.1035(10) Uani 1 1 d . . . . . C8 C -0.0628(4) 0.4874(3) 0.6953(3) 0.0500(8) Uani 1 1 d . . . . . C2 C 0.5265(4) 0.6755(3) 1.2420(3) 0.0621(9) Uani 1 1 d . . . . . H2A H 0.6099 0.6356 1.2660 0.075 Uiso 1 1 calc R U . . . C4 C 0.2916(3) 0.6894(3) 1.0971(3) 0.0500(8) Uani 1 1 d . . . . . C11 C -0.2411(4) 0.3470(3) 0.4724(3) 0.0553(8) Uani 1 1 d . . . . . C1 C 0.5129(3) 0.7783(3) 1.3164(3) 0.0524(8) Uani 1 1 d . . . . . C12 C -0.2862(4) 0.4520(3) 0.5233(3) 0.0595(9) Uani 1 1 d . . . . . H12 H -0.3772 0.4754 0.4826 0.071 Uiso 1 1 calc R U . . . C7 C 0.1299(3) 0.5465(3) 0.9000(3) 0.0522(8) Uani 1 1 d . . . . . C3 C 0.4183(4) 0.6318(3) 1.1332(3) 0.0571(8) Uani 1 1 d . . . . . H3A H 0.4294 0.5634 1.0832 0.069 Uiso 1 1 calc R U . . . C13 C -0.1986(4) 0.5210(3) 0.6318(3) 0.0573(8) Uani 1 1 d . . . . . H13 H -0.2300 0.5916 0.6639 0.069 Uiso 1 1 calc R U . . . C9 C -0.0143(4) 0.3850(3) 0.6444(3) 0.0597(9) Uani 1 1 d . . . . . H9 H 0.0785 0.3634 0.6841 0.072 Uiso 1 1 calc R U . . . C10 C -0.1041(4) 0.3159(3) 0.5350(3) 0.0626(9) Uani 1 1 d . . . . . H10 H -0.0720 0.2463 0.5021 0.075 Uiso 1 1 calc R U . . . C5 C 0.2801(4) 0.7925(3) 1.1743(3) 0.0587(9) Uani 1 1 d . . . . . H5 H 0.1964 0.8323 1.1514 0.070 Uiso 1 1 calc R U . . . C6 C 0.3888(4) 0.8367(3) 1.2830(3) 0.0608(9) Uani 1 1 d . . . . . H6 H 0.3789 0.9052 1.3335 0.073 Uiso 1 1 calc R U . . . C14 C -0.3307(4) 0.2728(4) 0.3547(3) 0.0635(9) Uani 1 1 d . . . . . C17 C 0.2453(5) 1.0376(4) 0.9056(3) 0.0998(14) Uani 1 1 d . . . . . H17A H 0.2763 1.0253 0.9881 0.150 Uiso 1 1 calc R U . . . H17B H 0.2877 1.1356 0.8948 0.150 Uiso 1 1 calc R U . . . H17C H 0.2884 0.9820 0.8619 0.150 Uiso 1 1 calc R U . . . C15 C -0.5473(5) 0.2523(5) 0.1860(3) 0.1031(14) Uani 1 1 d . . . . . H15A H -0.4794 0.2691 0.1324 0.155 Uiso 1 1 calc R U . . . H15B H -0.6356 0.2904 0.1587 0.155 Uiso 1 1 calc R U . . . H15C H -0.5899 0.1524 0.1895 0.155 Uiso 1 1 calc R U . . . C16 C 0.0148(5) 0.9912(5) 0.7009(3) 0.1056(15) Uani 1 1 d . . . . . H16A H 0.0744 0.9352 0.6757 0.158 Uiso 1 1 calc R U . . . H16B H 0.0587 1.0876 0.6865 0.158 Uiso 1 1 calc R U . . . H16C H -0.0976 0.9555 0.6575 0.158 Uiso 1 1 calc R U . . . 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 S1 0.0777(6) 0.0602(6) 0.0715(7) -0.0007(5) 0.0062(5) 0.0368(5) S2 0.0942(7) 0.0593(6) 0.0793(7) 0.0038(5) 0.0261(6) 0.0406(5) N2 0.0601(16) 0.0512(16) 0.0602(18) -0.0003(14) 0.0067(14) 0.0286(12) N3 0.0672(17) 0.0507(16) 0.0583(18) 0.0026(14) 0.0078(15) 0.0278(13) N1 0.070(2) 0.071(2) 0.062(2) -0.0028(16) 0.0048(17) 0.0209(16) O4 0.0853(17) 0.0946(19) 0.0563(16) -0.0091(13) -0.0065(14) 0.0360(14) O5 0.0824(16) 0.0565(14) 0.0945(18) 0.0105(13) 0.0206(14) 0.0307(12) O3 0.099(2) 0.109(2) 0.0745(18) -0.0231(15) 0.0086(15) 0.0491(17) O2 0.109(2) 0.126(2) 0.0755(19) -0.0369(17) -0.0030(16) 0.0581(19) O1 0.095(2) 0.120(2) 0.090(2) -0.0149(16) -0.0165(16) 0.0603(18) C8 0.0544(18) 0.0468(18) 0.047(2) 0.0046(16) 0.0142(16) 0.0115(15) C2 0.056(2) 0.069(2) 0.066(2) 0.0030(19) 0.0111(18) 0.0310(17) C4 0.0486(18) 0.0487(18) 0.053(2) 0.0046(16) 0.0112(16) 0.0177(14) C11 0.057(2) 0.061(2) 0.050(2) 0.0031(17) 0.0173(17) 0.0179(16) C1 0.0487(18) 0.0552(19) 0.051(2) 0.0030(16) 0.0112(16) 0.0146(15) C12 0.0526(19) 0.072(2) 0.056(2) 0.0037(18) 0.0115(17) 0.0246(17) C7 0.0485(18) 0.0501(19) 0.059(2) 0.0031(17) 0.0174(16) 0.0142(14) C3 0.0566(19) 0.062(2) 0.056(2) -0.0054(17) 0.0095(17) 0.0285(16) C13 0.060(2) 0.061(2) 0.056(2) 0.0028(17) 0.0121(18) 0.0298(16) C9 0.061(2) 0.066(2) 0.058(2) 0.0023(18) 0.0111(17) 0.0312(17) C10 0.069(2) 0.067(2) 0.059(2) -0.0014(18) 0.0163(19) 0.0328(18) C5 0.0557(19) 0.053(2) 0.071(2) -0.0019(17) 0.0123(18) 0.0278(16) C6 0.066(2) 0.055(2) 0.060(2) -0.0084(17) 0.0109(19) 0.0218(16) C14 0.069(2) 0.071(2) 0.054(2) 0.0038(19) 0.019(2) 0.0243(19) C17 0.115(3) 0.081(3) 0.077(3) -0.003(2) 0.004(2) 0.009(2) C15 0.099(3) 0.112(4) 0.077(3) -0.016(3) -0.010(2) 0.030(3) C16 0.131(4) 0.119(4) 0.072(3) 0.023(2) 0.009(3) 0.061(3) _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 S1 C7 1.662(3) . ? S2 O5 1.496(2) . ? S2 C17 1.764(4) . ? S2 C16 1.770(4) . ? N2 C7 1.377(4) . ? N2 C4 1.394(3) . ? N3 C7 1.357(4) . ? N3 C8 1.405(3) . ? N1 O2 1.206(3) . ? N1 O1 1.228(3) . ? N1 C1 1.456(4) . ? O4 C14 1.329(4) . ? O4 C15 1.439(4) . ? O3 C14 1.204(4) . ? C8 C9 1.391(4) . ? C8 C13 1.392(4) . ? C2 C3 1.367(4) . ? C2 C1 1.378(4) . ? C4 C3 1.391(4) . ? C4 C5 1.393(4) . ? C11 C10 1.385(4) . ? C11 C12 1.392(4) . ? C11 C14 1.467(4) . ? C1 C6 1.373(4) . ? C12 C13 1.362(4) . ? C9 C10 1.374(4) . ? C5 C6 1.368(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 S2 C17 104.74(17) . . ? O5 S2 C16 107.00(18) . . ? C17 S2 C16 98.4(2) . . ? C7 N2 C4 132.8(2) . . ? C7 N3 C8 132.0(3) . . ? O2 N1 O1 122.5(3) . . ? O2 N1 C1 119.5(3) . . ? O1 N1 C1 118.0(3) . . ? C14 O4 C15 116.7(3) . . ? C9 C8 C13 118.9(3) . . ? C9 C8 N3 125.2(3) . . ? C13 C8 N3 115.8(3) . . ? C3 C2 C1 120.5(3) . . ? C3 C4 C5 118.0(3) . . ? C3 C4 N2 125.5(3) . . ? C5 C4 N2 116.4(3) . . ? C10 C11 C12 118.0(3) . . ? C10 C11 C14 119.7(3) . . ? C12 C11 C14 122.2(3) . . ? C6 C1 C2 120.4(3) . . ? C6 C1 N1 119.7(3) . . ? C2 C1 N1 119.9(3) . . ? C13 C12 C11 120.9(3) . . ? N3 C7 N2 110.2(3) . . ? N3 C7 S1 125.9(2) . . ? N2 C7 S1 123.8(2) . . ? C2 C3 C4 120.2(3) . . ? C12 C13 C8 120.8(3) . . ? C10 C9 C8 119.6(3) . . ? C9 C10 C11 121.7(3) . . ? C6 C5 C4 121.7(3) . . ? C5 C6 C1 119.0(3) . . ? O3 C14 O4 122.2(3) . . ? O3 C14 C11 124.7(3) . . ? O4 C14 C11 113.1(3) . . ? _refine_diff_density_max 0.243 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.044 _shelx_res_file ; corr.res created by SHELXL-2014/7 TITL corr in P-1 CELL 0.71073 8.9102 9.9426 11.7194 91.392 104.200 106.984 ZERR 2.00 0.0006 0.0007 0.0008 0.004 0.004 0.004 LATT 1 SFAC C H N O S UNIT 34 38 6 10 4 OMIT -3 50.1 L.S. 10 ACTA BOND FMAP 2 PLAN 1 TEMP 23.000 WGHT 0.078000 FVAR 0.54772 MOLE 1 S1 5 0.190526 0.403420 0.915479 11.00000 0.07766 0.06015 = 0.07152 -0.00070 0.00618 0.03682 S2 5 0.031257 0.982658 0.854001 11.00000 0.09420 0.05929 = 0.07931 0.00382 0.02612 0.04064 N2 3 0.177787 0.657298 0.987068 11.00000 0.06010 0.05122 = 0.06022 -0.00034 0.00666 0.02859 AFIX 43 H2 2 0.127409 0.718970 0.970250 11.00000 -1.20000 AFIX 0 N3 3 0.020498 0.568109 0.804728 11.00000 0.06715 0.05067 = 0.05834 0.00257 0.00777 0.02784 AFIX 43 H3 2 -0.002048 0.645615 0.812877 11.00000 -1.20000 AFIX 0 N1 3 0.629151 0.823664 1.431952 11.00000 0.07038 0.07091 = 0.06221 -0.00278 0.00483 0.02087 O4 4 -0.452887 0.319786 0.302008 11.00000 0.08529 0.09462 = 0.05630 -0.00913 -0.00646 0.03598 O5 4 -0.020461 0.829423 0.872882 11.00000 0.08243 0.05649 = 0.09452 0.01050 0.02059 0.03073 O3 4 -0.298279 0.179710 0.307828 11.00000 0.09894 0.10925 = 0.07452 -0.02308 0.00862 0.04913 O2 4 0.607540 0.903128 1.501234 11.00000 0.10925 0.12622 = 0.07553 -0.03687 -0.00300 0.05813 O1 4 0.747944 0.780557 1.454118 11.00000 0.09494 0.12002 = 0.08974 -0.01492 -0.01650 0.06034 C8 1 -0.062800 0.487373 0.695311 11.00000 0.05439 0.04680 = 0.04660 0.00459 0.01419 0.01148 C2 1 0.526459 0.675526 1.241974 11.00000 0.05570 0.06916 = 0.06640 0.00300 0.01109 0.03098 AFIX 43 H2A 2 0.609917 0.635598 1.265951 11.00000 -1.20000 AFIX 0 C4 1 0.291604 0.689424 1.097077 11.00000 0.04860 0.04872 = 0.05321 0.00455 0.01125 0.01769 C11 1 -0.241146 0.347010 0.472438 11.00000 0.05679 0.06062 = 0.04992 0.00312 0.01732 0.01791 C1 1 0.512883 0.778257 1.316374 11.00000 0.04874 0.05525 = 0.05113 0.00303 0.01116 0.01461 C12 1 -0.286166 0.452019 0.523291 11.00000 0.05260 0.07189 = 0.05605 0.00374 0.01150 0.02460 AFIX 43 H12 2 -0.377223 0.475351 0.482616 11.00000 -1.20000 AFIX 0 C7 1 0.129939 0.546501 0.899955 11.00000 0.04855 0.05013 = 0.05880 0.00309 0.01737 0.01421 C3 1 0.418275 0.631845 1.133243 11.00000 0.05663 0.06235 = 0.05557 -0.00541 0.00946 0.02855 AFIX 43 H3A 2 0.429361 0.563380 1.083237 11.00000 -1.20000 AFIX 0 C13 1 -0.198642 0.521050 0.631820 11.00000 0.06043 0.06057 = 0.05636 0.00278 0.01207 0.02978 AFIX 43 H13 2 -0.230036 0.591581 0.663915 11.00000 -1.20000 AFIX 0 C9 1 -0.014254 0.385000 0.644393 11.00000 0.06053 0.06593 = 0.05769 0.00231 0.01107 0.03120 AFIX 43 H9 2 0.078462 0.363435 0.684130 11.00000 -1.20000 AFIX 0 C10 1 -0.104073 0.315875 0.535013 11.00000 0.06943 0.06685 = 0.05864 -0.00135 0.01630 0.03279 AFIX 43 H10 2 -0.071954 0.246346 0.502145 11.00000 -1.20000 AFIX 0 C5 1 0.280123 0.792467 1.174328 11.00000 0.05569 0.05346 = 0.07135 -0.00189 0.01227 0.02783 AFIX 43 H5 2 0.196371 0.832264 1.151422 11.00000 -1.20000 AFIX 0 C6 1 0.388839 0.836657 1.283019 11.00000 0.06575 0.05499 = 0.05977 -0.00836 0.01087 0.02178 AFIX 43 H6 2 0.378857 0.905222 1.333543 11.00000 -1.20000 AFIX 0 C14 1 -0.330686 0.272807 0.354667 11.00000 0.06859 0.07104 = 0.05430 0.00383 0.01949 0.02427 C17 1 0.245294 1.037645 0.905571 11.00000 0.11512 0.08133 = 0.07700 -0.00302 0.00427 0.00937 AFIX 137 H17A 2 0.276320 1.025254 0.988102 11.00000 -1.50000 H17B 2 0.287709 1.135591 0.894780 11.00000 -1.50000 H17C 2 0.288358 0.982020 0.861901 11.00000 -1.50000 AFIX 0 C15 1 -0.547310 0.252337 0.186001 11.00000 0.09910 0.11206 = 0.07653 -0.01604 -0.01044 0.02978 AFIX 137 H15A 2 -0.479417 0.269129 0.132365 11.00000 -1.50000 H15B 2 -0.635627 0.290440 0.158720 11.00000 -1.50000 H15C 2 -0.589878 0.152445 0.189528 11.00000 -1.50000 AFIX 0 C16 1 0.014795 0.991206 0.700912 11.00000 0.13147 0.11927 = 0.07154 0.02322 0.00875 0.06086 AFIX 137 H16A 2 0.074408 0.935153 0.675739 11.00000 -1.50000 H16B 2 0.058650 1.087626 0.686509 11.00000 -1.50000 H16C 2 -0.097599 0.955477 0.657461 11.00000 -1.50000 AFIX 0 HKLF 4 REM corr in P-1 REM R1 = 0.0479 for 1874 Fo > 4sig(Fo) and 0.0941 for all 3215 data REM 247 parameters refined using 0 restraints END WGHT 0.0636 0.0000 REM Highest difference peak 0.243, deepest hole -0.273, 1-sigma level 0.044 Q1 1 0.1464 1.0032 0.8977 11.00000 0.05 0.24 ; _shelx_res_checksum 73077 _shelx_hkl_file ; 1 0 0 182.51 5.28 1 0 0 182.67 5.47 1 0 0 188.47 5.51 1 0 0 184.14 5.29 1 0 0 187.12 5.77 -1 0 0 178.91 5.99 -1 0 0 182.00 5.47 -1 0 0 195.69 5.51 -2 0 0 44.13 2.33 2 0 0 50.56 2.08 2 0 0 46.55 2.45 -2 0 0 53.23 3.30 -2 0 0 48.30 2.45 2 0 0 51.63 2.86 2 0 0 48.61 2.05 2 0 0 48.50 2.50 3 0 0 205.52 7.88 3 0 0 197.41 6.50 -3 0 0 205.77 7.00 3 0 0 195.50 7.17 3 0 0 194.46 7.17 3 0 0 188.75 6.44 -3 0 0 195.32 5.78 -3 0 0 198.20 6.93 4 0 0 403.16 14.24 -4 0 0 395.50 13.39 4 0 0 418.14 12.58 4 0 0 402.71 12.47 4 0 0 386.00 13.23 -4 0 0 400.94 12.78 -4 0 0 403.46 10.84 -4 0 0 409.25 12.88 4 0 0 401.01 12.73 -5 0 0 100.80 5.31 -5 0 0 104.15 5.13 5 0 0 100.42 5.64 5 0 0 95.95 4.84 -5 0 0 98.78 6.38 5 0 0 98.40 4.85 5 0 0 99.75 5.69 -5 0 0 94.05 4.08 5 0 0 105.56 6.42 -6 0 0 15.95 2.50 -6 0 0 17.97 1.97 -6 0 0 12.49 3.38 6 0 0 20.53 2.74 6 0 0 9.90 2.78 6 0 0 13.59 2.74 7 0 0 5.95 2.34 7 0 0 6.16 2.65 -7 0 0 3.03 2.53 -7 0 0 10.53 1.69 -8 0 0 -0.36 1.22 8 0 0 1.59 2.43 8 0 0 -0.93 2.03 -8 0 0 0.75 2.86 9 0 0 2.17 2.69 9 0 0 2.46 3.23 -9 0 0 1.15 3.30 10 0 0 0.80 2.96 -10 0 0 -2.03 3.56 -11 1 0 0.37 4.32 11 -1 0 -2.06 2.99 10 -1 0 -0.71 2.85 -10 1 0 3.94 4.29 9 -1 0 -0.06 2.73 -9 1 0 1.32 3.28 9 -1 0 1.34 2.49 8 -1 0 0.01 2.19 -8 1 0 1.76 0.98 8 -1 0 -2.30 1.80 -8 1 0 1.14 2.52 -7 1 0 1.96 1.08 7 -1 0 0.62 1.96 -7 1 0 7.27 3.12 7 -1 0 2.37 2.20 7 -1 0 1.32 1.69 -6 1 0 26.11 4.72 -6 1 0 22.47 1.97 -6 1 0 25.74 2.63 -6 1 0 17.94 3.48 6 -1 0 23.93 3.86 6 -1 0 30.51 2.93 -6 1 0 27.13 2.76 -5 1 0 0.19 0.94 5 -1 0 -0.06 0.94 -5 1 0 -0.41 1.45 5 -1 0 1.14 1.08 -5 1 0 -0.34 0.90 5 -1 0 -0.03 1.30 5 -1 0 -0.70 1.19 -5 1 0 -0.60 1.73 -5 1 0 -0.64 0.70 4 -1 0 113.03 4.38 -4 1 0 100.26 6.43 4 -1 0 112.67 5.25 -4 1 0 104.46 5.76 4 -1 0 110.49 4.40 -4 1 0 108.95 4.74 -4 1 0 109.18 3.86 4 -1 0 117.73 5.38 4 -1 0 121.51 6.26 -4 1 0 107.20 4.74 -3 1 0 918.86 26.86 3 -1 0 902.88 26.08 3 -1 0 906.35 24.86 -3 1 0 895.49 24.52 -3 1 0 918.20 24.53 3 -1 0 903.69 24.91 -3 1 0 884.35 21.08 3 -1 0 885.46 24.38 3 -1 0 880.15 24.33 2 -1 0 353.76 10.31 -2 1 0 349.74 11.40 2 -1 0 351.63 9.85 -2 1 0 351.67 10.16 -2 1 0 358.96 10.23 2 -1 0 356.05 9.86 2 -1 0 342.13 10.33 2 -1 0 357.92 11.20 1 -1 0 473.15 12.91 1 -1 0 481.34 12.86 1 -1 0 482.32 12.87 -1 1 0 463.12 12.83 -1 1 0 453.01 12.77 -1 1 0 469.16 13.33 -1 1 0 467.77 12.87 0 -1 0 291.49 8.19 0 1 0 289.68 8.38 0 1 0 303.93 8.41 0 -1 0 301.92 8.55 0 1 0 285.77 8.17 0 1 0 282.45 8.47 0 -1 0 294.97 8.40 0 -1 0 298.58 8.42 -1 -1 0 157.26 5.47 1 1 0 169.65 5.21 1 1 0 161.35 5.50 -1 -1 0 153.82 5.06 -1 -1 0 155.14 5.48 1 1 0 158.11 5.30 1 1 0 156.75 5.13 -1 -1 0 156.64 5.09 -2 -1 0 130.93 4.37 -2 -1 0 116.93 4.97 2 1 0 128.78 5.20 2 1 0 124.25 4.65 2 1 0 124.00 4.63 2 1 0 123.51 5.09 -2 -1 0 126.69 4.34 -2 -1 0 125.78 5.04 -3 -1 0 524.07 16.10 -3 -1 0 526.01 13.71 -3 -1 0 518.56 14.66 3 1 0 531.69 16.38 -3 -1 0 531.70 16.12 -3 -1 0 523.45 14.66 3 1 0 523.61 16.40 3 1 0 531.50 16.68 3 1 0 521.81 15.67 3 1 0 533.38 15.71 -4 -1 0 132.59 5.10 4 1 0 133.62 5.83 4 1 0 142.35 7.01 -4 -1 0 142.49 6.39 4 1 0 129.83 5.77 4 1 0 139.70 6.69 4 1 0 130.17 6.18 -4 -1 0 131.24 6.23 -4 -1 0 125.19 6.74 -5 -1 0 -0.07 1.24 -5 -1 0 -0.66 0.90 5 1 0 0.17 1.45 -5 -1 0 0.07 1.59 -5 -1 0 -0.58 1.08 5 1 0 0.80 1.19 5 1 0 1.31 1.52 -6 -1 0 28.79 4.76 -6 -1 0 44.46 4.09 6 1 0 41.08 3.77 6 1 0 33.24 4.55 6 1 0 38.64 4.56 -6 -1 0 45.39 3.13 7 1 0 3.42 2.27 -7 -1 0 3.07 1.42 7 1 0 2.51 2.12 -7 -1 0 1.38 2.50 8 1 0 25.28 4.57 -8 -1 0 27.26 5.54 -8 -1 0 32.77 2.88 8 1 0 28.87 5.24 -9 -1 0 2.60 3.93 9 1 0 -0.43 2.69 9 1 0 1.09 2.65 -9 -1 0 1.99 1.52 10 1 0 0.24 2.96 -10 -1 0 2.77 4.30 -11 2 0 -0.55 4.30 11 -2 0 -3.28 2.43 -10 2 0 1.50 3.56 10 -2 0 6.53 3.47 9 -2 0 1.67 2.82 9 -2 0 5.30 3.55 -9 2 0 -0.29 3.24 -8 2 0 1.84 2.70 8 -2 0 0.76 2.36 7 -2 0 9.10 2.30 7 -2 0 16.35 3.78 -7 2 0 8.59 1.24 -7 2 0 21.94 4.36 -7 2 0 12.40 4.08 -6 2 0 -0.98 1.00 -6 2 0 -0.72 1.80 -6 2 0 0.25 1.20 -6 2 0 -0.38 0.78 -6 2 0 0.95 0.95 6 -2 0 0.01 1.54 -6 2 0 0.70 1.84 6 -2 0 -1.67 1.07 -5 2 0 423.93 16.68 5 -2 0 417.19 12.94 5 -2 0 405.48 12.84 -5 2 0 410.11 12.95 5 -2 0 415.07 14.05 -5 2 0 405.69 10.84 -5 2 0 416.28 12.96 5 -2 0 385.84 15.30 -5 2 0 430.67 14.57 -4 2 0 26.59 1.72 -4 2 0 25.83 3.17 4 -2 0 20.54 2.40 -4 2 0 22.23 2.00 -4 2 0 23.27 3.45 4 -2 0 23.72 1.80 4 -2 0 27.10 3.29 -4 2 0 24.95 2.06 4 -2 0 25.34 1.91 3 -2 0 523.99 14.69 3 -2 0 515.20 15.41 -3 2 0 501.37 12.77 -3 2 0 513.74 14.97 -3 2 0 518.19 15.03 -3 2 0 502.05 16.82 3 -2 0 509.08 14.68 3 -2 0 540.79 16.89 2 -2 0 5.92 1.13 2 -2 0 6.55 0.89 -2 2 0 6.63 0.69 -2 2 0 4.10 1.18 -2 2 0 5.73 0.62 -2 2 0 4.43 1.05 2 -2 0 6.13 0.91 -1 2 0 4216.93 109.59 1 -2 0 4279.09 109.82 -1 2 0 4240.89 107.91 1 -2 0 4114.99 109.68 1 -2 0 4244.86 107.68 -1 2 0 4090.26 109.66 -1 2 0 4149.95 107.71 0 -2 0 21.41 1.87 0 -2 0 21.82 1.57 0 2 0 17.33 1.47 0 2 0 18.42 1.73 0 2 0 19.07 1.41 0 -2 0 24.25 1.60 0 2 0 20.82 1.55 -1 -2 0 972.71 26.35 -1 -2 0 958.41 26.64 1 2 0 984.17 26.44 -1 -2 0 980.57 26.38 1 2 0 949.67 25.92 1 2 0 972.56 26.68 1 2 0 825.69 26.28 -2 -2 0 167.95 6.97 2 2 0 170.35 6.74 2 2 0 168.62 6.47 2 2 0 173.15 6.53 -2 -2 0 163.01 6.95 -2 -2 0 175.72 6.23 2 2 0 170.82 7.05 -2 -2 0 175.82 6.21 -3 -2 0 17.88 2.75 -3 -2 0 17.54 2.47 -3 -2 0 18.82 1.77 3 2 0 24.21 2.72 3 2 0 16.67 2.33 3 2 0 21.97 2.32 3 2 0 20.47 2.70 -3 -2 0 18.35 2.41 3 2 0 18.34 2.67 4 2 0 5.10 1.64 -4 -2 0 7.56 2.14 -4 -2 0 5.93 1.16 -4 -2 0 5.69 1.91 4 2 0 4.33 1.78 -4 -2 0 5.27 1.45 -4 -2 0 2.79 1.58 4 2 0 4.33 1.78 4 2 0 6.96 1.73 4 2 0 7.15 2.05 5 2 0 17.33 3.24 -5 -2 0 17.58 2.18 -5 -2 0 16.15 3.26 5 2 0 11.84 2.71 5 2 0 16.93 2.66 -5 -2 0 17.11 2.89 6 2 0 3.78 2.05 6 2 0 5.65 2.45 -6 -2 0 -1.01 1.96 6 2 0 -0.52 1.77 -6 -2 0 2.48 1.37 7 2 0 2.77 2.37 -7 -2 0 7.11 1.92 -7 -2 0 2.14 2.68 7 2 0 2.46 2.09 8 2 0 -3.40 2.28 -8 -2 0 -1.81 2.53 -8 -2 0 5.24 1.91 8 2 0 1.34 2.88 -9 -2 0 3.42 3.76 -9 -2 0 2.93 1.80 9 2 0 -0.21 2.67 -10 -2 0 -0.41 4.08 10 2 0 1.72 3.38 11 -3 0 1.09 2.86 -11 3 0 4.17 4.48 -10 3 0 -3.09 2.97 10 -3 0 4.21 2.70 -9 3 0 1.95 4.01 -9 3 0 5.15 3.52 9 -3 0 2.91 2.76 -8 3 0 21.58 4.56 -8 3 0 15.31 5.17 8 -3 0 14.17 3.86 -7 3 0 7.04 1.12 -7 3 0 7.85 1.79 -7 3 0 5.63 3.28 7 -3 0 1.84 1.99 7 -3 0 8.81 2.20 -7 3 0 2.71 2.44 -6 3 0 29.94 2.72 -6 3 0 29.43 5.18 6 -3 0 36.74 4.73 -6 3 0 31.04 4.40 -6 3 0 30.84 2.07 -6 3 0 25.30 2.60 6 -3 0 32.32 2.87 -5 3 0 36.69 2.77 -5 3 0 49.53 4.67 5 -3 0 37.85 2.79 -5 3 0 35.47 2.18 -5 3 0 41.24 5.03 -5 3 0 43.84 3.05 5 -3 0 37.36 4.34 5 -3 0 43.25 3.77 5 -3 0 37.20 2.76 -4 3 0 0.72 0.79 4 -3 0 4.36 1.10 -4 3 0 1.17 1.33 -4 3 0 -0.08 1.20 4 -3 0 0.67 1.27 4 -3 0 3.13 1.19 -4 3 0 3.56 0.93 4 -3 0 2.49 1.32 -4 3 0 3.22 1.12 -3 3 0 465.60 12.36 -3 3 0 469.65 14.64 3 -3 0 482.21 15.05 -3 3 0 482.50 16.30 -3 3 0 487.49 13.09 3 -3 0 479.93 14.36 3 -3 0 483.74 14.31 -2 3 0 251.04 8.07 2 -3 0 265.96 8.64 -2 3 0 257.16 8.11 2 -3 0 255.33 8.48 -2 3 0 252.42 9.37 -2 3 0 252.83 7.48 2 -3 0 264.51 9.16 1 -3 0 505.06 15.16 -1 3 0 496.94 14.97 -1 3 0 524.43 15.29 1 -3 0 523.05 15.70 1 -3 0 473.86 14.94 -1 3 0 498.27 15.44 -1 3 0 491.05 14.79 0 3 0 115.14 5.50 0 -3 0 122.53 5.09 0 3 0 123.40 5.04 0 3 0 116.58 5.00 0 3 0 116.41 4.84 0 -3 0 116.57 5.02 0 -3 0 121.72 5.71 1 3 0 10.18 1.56 1 3 0 12.46 1.77 1 3 0 8.14 1.76 1 3 0 7.58 1.48 -1 -3 0 9.09 1.54 -1 -3 0 11.03 1.95 -1 -3 0 9.21 1.56 2 3 0 55.38 4.13 -2 -3 0 62.78 4.33 2 3 0 63.10 3.81 -2 -3 0 59.44 4.13 2 3 0 47.60 3.26 -2 -3 0 54.13 3.37 2 3 0 48.34 3.39 2 3 0 53.34 3.47 3 3 0 1.42 1.24 3 3 0 1.21 1.13 3 3 0 -0.49 1.16 3 3 0 1.70 1.19 -3 -3 0 1.88 1.47 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7.64 5 -4 0 189.61 9.89 -4 4 0 393.78 13.06 4 -4 0 386.82 13.77 4 -4 0 395.26 12.87 -4 4 0 381.55 10.95 4 -4 0 393.80 12.88 -4 4 0 392.11 15.24 -4 4 0 404.40 13.31 -3 4 0 100.01 3.99 -3 4 0 98.28 4.80 3 -4 0 100.70 5.39 -3 4 0 95.44 5.19 3 -4 0 102.05 4.80 -3 4 0 91.45 4.08 3 -4 0 98.47 4.68 -3 4 0 98.31 5.77 2 -4 0 13.20 1.84 2 -4 0 13.75 2.18 -2 4 0 11.76 2.05 -2 4 0 16.07 1.74 2 -4 0 16.06 1.97 -2 4 0 14.54 1.76 -2 4 0 14.02 2.25 -1 4 0 -0.30 0.65 -1 4 0 0.50 0.96 -1 4 0 -0.90 0.76 1 -4 0 -0.95 0.78 1 -4 0 -0.49 0.49 -1 4 0 0.24 0.73 1 -4 0 1.18 0.94 -1 4 0 -0.77 0.71 0 -4 0 6.45 1.44 0 4 0 7.91 1.65 0 4 0 7.85 1.57 0 4 0 4.60 1.23 0 -4 0 5.12 1.72 0 -4 0 9.66 1.85 0 4 0 4.23 1.59 1 4 0 181.77 7.68 -1 -4 0 167.71 7.37 1 4 0 188.08 7.79 1 4 0 195.42 8.70 1 4 0 179.35 6.58 -1 -4 0 176.46 8.46 1 4 0 192.10 7.59 2 4 0 132.80 6.34 2 4 0 117.28 6.77 -2 -4 0 102.24 6.41 -2 -4 0 116.52 5.73 2 4 0 124.16 6.03 2 4 0 95.01 5.62 2 4 0 111.65 5.18 3 4 0 28.95 3.13 3 4 0 20.63 3.06 3 4 0 21.16 3.02 3 4 0 21.21 3.08 -3 -4 0 25.12 3.63 4 4 0 0.46 1.43 4 4 0 0.04 1.45 4 4 0 -0.03 1.37 -4 -4 0 0.46 1.95 -4 -4 0 0.18 1.81 -5 -4 0 38.09 3.71 5 4 0 35.89 4.29 5 4 0 32.75 4.45 5 4 0 35.95 4.33 -5 -4 0 29.58 4.67 6 4 0 6.11 2.57 -6 -4 0 2.24 1.62 -6 -4 0 5.15 3.10 6 4 0 6.13 2.91 7 4 0 0.51 2.15 -7 -4 0 2.27 3.15 7 4 0 0.85 2.17 -7 -4 0 2.67 1.93 8 4 0 0.62 2.34 -8 -4 0 -1.90 3.25 -8 -4 0 -2.35 1.70 -9 -4 0 0.50 2.20 9 4 0 1.48 3.04 -9 -4 0 2.40 4.13 -11 5 0 1.88 4.46 -10 5 0 -2.45 3.03 -9 5 0 19.63 6.01 -9 5 0 16.16 4.97 9 -5 0 16.83 5.11 -8 5 0 3.47 3.69 -8 5 0 0.80 2.51 8 -5 0 2.06 2.31 7 -5 0 2.78 2.66 -7 5 0 1.56 2.11 -7 5 0 0.91 0.97 -7 5 0 2.95 2.89 6 -5 0 17.70 3.84 -6 5 0 18.71 4.38 6 -5 0 21.92 2.95 -6 5 0 16.81 3.57 -6 5 0 25.00 2.94 -6 5 0 23.88 2.16 -5 5 0 170.93 6.24 -5 5 0 162.30 8.28 -5 5 0 165.88 9.77 5 -5 0 177.55 7.76 -4 5 0 0.02 1.16 4 -5 0 -0.25 0.98 -4 5 0 -0.41 1.06 -4 5 0 -0.30 0.83 4 -5 0 0.79 1.12 -4 5 0 -0.09 0.70 -4 5 0 -0.89 1.33 4 -5 0 -0.54 1.34 -3 5 0 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2.16 0 1 12 0.29 4.51 1 1 12 7.21 3.08 2 1 12 -0.09 2.88 -8 2 12 1.99 2.61 -7 2 12 3.22 2.85 -6 2 12 5.00 3.31 -5 2 12 1.21 2.93 -4 2 12 0.22 2.96 -3 2 12 0.86 1.67 -3 2 12 5.21 3.80 -2 2 12 5.36 3.87 -2 2 12 1.73 1.96 -1 2 12 5.38 2.55 -1 2 12 1.97 4.05 0 2 12 6.34 2.87 0 2 12 9.09 5.43 1 2 12 -1.30 2.32 2 2 12 0.03 3.38 -7 3 12 -0.38 2.55 -6 3 12 27.52 4.73 -5 3 12 16.79 4.37 -4 3 12 7.06 3.73 -3 3 12 0.49 1.79 -3 3 12 0.76 3.16 -2 3 12 -2.12 3.38 -2 3 12 -1.21 1.64 -1 3 12 4.82 2.52 -1 3 12 9.65 4.72 0 3 12 1.79 2.46 1 3 12 1.52 2.83 2 3 12 -0.63 2.92 -4 4 12 1.99 1.51 -3 4 12 9.69 2.49 -2 4 12 -1.05 1.95 -1 4 12 -0.04 2.09 0 4 12 1.22 2.51 1 4 12 -1.09 2.58 2 4 12 0.38 3.23 -4 5 12 14.47 2.41 -3 5 12 7.97 2.42 -2 5 12 0.15 2.02 -1 5 12 2.00 2.44 0 5 12 -1.73 2.21 1 5 12 2.48 3.42 2 5 12 0.48 3.72 -4 6 12 4.15 2.08 -3 6 12 2.37 2.22 -2 6 12 -0.74 2.20 -1 6 12 -0.13 2.33 0 6 12 1.69 2.90 1 6 12 0.32 3.24 -4 7 12 6.91 2.46 -3 7 12 4.29 2.54 -2 7 12 -0.14 2.39 -1 7 12 -1.75 2.64 -4 8 12 -1.81 2.34 -3 8 12 1.51 2.52 -2 -7 13 -0.56 5.99 -4 -6 13 -2.85 4.22 -3 -6 13 -0.12 5.26 -2 -6 13 4.45 5.12 -1 -6 13 -8.52 4.37 -5 -5 13 0.36 4.09 -4 -5 13 0.36 4.19 -3 -5 13 -5.78 3.82 -2 -5 13 -0.91 4.02 -1 -5 13 4.18 4.69 2 -5 13 0.20 3.53 -6 -4 13 4.18 4.35 -5 -4 13 0.52 4.00 -4 -4 13 -0.02 3.91 -3 -4 13 -0.94 3.67 -2 -4 13 -1.94 4.02 -1 -4 13 10.08 5.35 1 -4 13 3.31 2.75 2 -4 13 -0.93 3.17 -7 -3 13 2.06 3.95 -6 -3 13 0.27 3.56 -5 -3 13 1.90 3.52 -4 -3 13 2.83 3.78 -3 -3 13 2.49 3.89 -2 -3 13 -2.76 4.02 -1 -3 13 -0.68 4.51 0 -3 13 3.21 2.60 1 -3 13 -1.29 2.50 2 -3 13 1.11 3.02 -7 -2 13 -0.40 3.46 -6 -2 13 5.76 3.68 -5 -2 13 -1.56 3.03 -4 -2 13 0.49 3.49 -3 -2 13 1.27 4.22 -2 -2 13 1.43 3.83 -1 -2 13 2.25 4.43 -1 -2 13 1.02 2.10 0 -2 13 -3.78 4.10 0 -2 13 1.17 2.66 1 -2 13 -0.02 2.52 2 -2 13 3.46 3.43 -8 -1 13 0.00 3.38 -7 -1 13 -1.97 3.03 -6 -1 13 8.54 3.94 -5 -1 13 8.20 4.18 -4 -1 13 2.01 3.74 -3 -1 13 18.10 5.35 -2 -1 13 20.20 5.68 -1 -1 13 2.98 4.16 -1 -1 13 4.65 2.55 0 -1 13 1.02 4.74 0 -1 13 1.40 2.45 1 -1 13 5.11 3.20 2 -1 13 2.31 3.38 -8 0 13 1.68 3.21 -7 0 13 -1.42 2.96 -6 0 13 -0.84 3.26 -5 0 13 0.05 3.33 -4 0 13 35.98 5.94 -3 0 13 2.82 3.82 -2 0 13 5.71 2.36 -2 0 13 1.04 3.93 -1 0 13 -1.20 1.88 -1 0 13 -1.41 4.02 0 0 13 6.50 2.83 0 0 13 15.07 6.19 1 0 13 4.96 3.13 2 0 13 0.95 2.98 -8 1 13 -1.56 2.82 -7 1 13 1.93 2.98 -6 1 13 9.25 3.94 -5 1 13 8.17 3.75 -4 1 13 1.42 3.21 -3 1 13 6.55 4.21 -3 1 13 3.00 1.84 -2 1 13 12.62 3.00 -2 1 13 8.10 4.64 -1 1 13 6.89 2.70 -1 1 13 4.05 4.79 0 1 13 1.31 2.42 0 1 13 -1.35 4.47 1 1 13 -2.15 2.54 2 1 13 2.00 3.30 -8 2 13 -3.33 2.91 -7 2 13 2.45 3.19 -6 2 13 1.25 3.29 -5 2 13 12.22 4.68 -4 2 13 2.72 3.66 -3 2 13 6.05 2.23 -3 2 13 4.46 4.12 -2 2 13 0.24 3.58 -2 2 13 0.61 1.89 -1 2 13 3.96 4.54 -1 2 13 4.02 2.36 0 2 13 3.20 3.00 1 2 13 4.52 3.20 2 2 13 0.30 3.44 -7 3 13 0.17 3.16 -6 3 13 2.79 3.31 -5 3 13 7.20 3.88 -4 3 13 1.93 3.56 -3 3 13 6.98 4.39 -3 3 13 -0.49 1.76 -2 3 13 3.60 2.32 -2 3 13 1.01 4.22 -1 3 13 -1.02 2.15 -1 3 13 -1.69 4.35 0 3 13 -0.78 2.48 1 3 13 -2.45 2.81 2 3 13 -1.20 3.09 -4 4 13 1.17 1.64 -3 4 13 3.44 2.23 -2 4 13 2.60 2.39 -1 4 13 2.61 2.64 0 4 13 1.15 3.05 1 4 13 2.30 3.11 -4 5 13 3.53 2.04 -3 5 13 0.08 1.92 -2 5 13 0.42 2.42 -1 5 13 -0.36 2.51 0 5 13 2.20 3.24 -4 6 13 -0.05 1.91 -3 6 13 -1.47 1.97 -2 6 13 5.62 2.80 -1 6 13 3.51 3.19 -4 7 13 -0.36 2.10 -3 7 13 2.39 2.60 -3 -5 14 -1.00 4.37 -2 -5 14 -1.82 4.59 -1 -5 14 -2.08 5.71 -5 -4 14 1.84 4.30 -4 -4 14 0.54 4.59 -3 -4 14 2.22 4.67 -2 -4 14 4.66 5.40 -1 -4 14 7.15 6.37 1 -4 14 -1.20 3.20 2 -4 14 1.11 3.38 -5 -3 14 1.18 3.68 -4 -3 14 4.32 4.80 -3 -3 14 -5.57 4.07 -2 -3 14 1.48 4.82 -1 -3 14 5.40 5.44 0 -3 14 0.25 2.64 1 -3 14 2.81 3.39 2 -3 14 -3.73 3.36 -6 -2 14 1.25 4.05 -5 -2 14 -2.11 3.46 -4 -2 14 3.29 4.02 -3 -2 14 -0.41 4.11 -2 -2 14 7.02 4.63 -1 -2 14 4.90 5.10 -1 -2 14 -0.38 2.25 0 -2 14 2.12 2.72 1 -2 14 0.11 3.02 2 -2 14 -0.37 3.11 -7 -1 14 -1.03 3.83 -6 -1 14 0.88 3.55 -5 -1 14 1.55 4.12 -4 -1 14 3.22 4.12 -3 -1 14 0.24 4.31 -2 -1 14 5.61 4.56 -1 -1 14 0.42 4.43 -1 -1 14 0.97 2.44 0 -1 14 3.17 2.96 1 -1 14 -2.21 3.04 2 -1 14 0.86 3.15 -7 0 14 3.66 3.80 -6 0 14 2.08 3.66 -5 0 14 11.58 4.65 -4 0 14 0.25 3.83 -3 0 14 -0.17 3.92 -2 0 14 0.53 2.33 -2 0 14 -1.44 3.67 -1 0 14 2.60 2.52 -1 0 14 3.05 4.93 0 0 14 -3.55 2.41 1 0 14 0.46 3.09 2 0 14 0.83 2.95 -7 1 14 1.81 3.74 -6 1 14 4.37 3.81 -5 1 14 0.74 3.73 -4 1 14 -0.09 3.97 -3 1 14 2.88 4.45 -2 1 14 2.35 2.37 -2 1 14 2.18 4.78 -1 1 14 5.18 2.80 -1 1 14 0.51 5.26 0 1 14 2.55 2.93 1 1 14 0.86 2.86 -7 2 14 3.44 3.68 -6 2 14 3.12 3.82 -5 2 14 3.66 4.31 -4 2 14 0.58 3.92 -3 2 14 0.48 2.06 -3 2 14 2.80 4.32 -2 2 14 -0.76 2.22 -2 2 14 2.42 4.66 -1 2 14 6.02 6.00 -1 2 14 0.92 2.57 0 2 14 0.35 2.93 1 2 14 -0.57 2.89 -7 3 14 -0.51 3.38 -6 3 14 0.21 3.51 -5 3 14 -2.89 3.48 -4 3 14 1.46 4.58 -3 3 14 -1.86 4.04 -3 3 14 1.16 2.01 -2 3 14 -0.68 2.41 -2 3 14 0.69 4.65 -1 3 14 2.24 6.11 -1 3 14 6.09 3.09 0 3 14 0.19 3.08 -4 4 14 -1.00 1.64 -3 4 14 3.82 2.45 -2 4 14 2.06 2.68 -1 4 14 2.46 3.03 -4 5 14 0.83 1.87 -3 5 14 4.61 2.72 -2 5 14 -0.80 2.38 -3 -3 15 5.02 5.24 -2 -3 15 1.37 5.00 -1 -3 15 -2.73 5.80 0 -3 15 -3.92 2.47 -4 -2 15 -1.01 4.68 -3 -2 15 -2.57 4.57 -2 -2 15 -1.66 5.38 -1 -2 15 -0.60 5.68 0 -2 15 -0.16 2.82 -5 -1 15 -1.96 4.00 -4 -1 15 0.40 4.23 -3 -1 15 3.49 4.53 -2 -1 15 -0.03 4.74 -1 -1 15 -1.35 2.49 -1 -1 15 -2.50 5.27 0 -1 15 -0.37 2.90 -5 0 15 2.81 4.19 -4 0 15 0.83 4.08 -3 0 15 1.73 4.56 -2 0 15 -1.14 2.29 -2 0 15 -1.02 5.32 -1 0 15 -3.94 6.11 -1 0 15 -1.72 2.34 0 0 15 1.85 2.99 -5 1 15 -0.32 3.99 -4 1 15 -3.17 4.08 -3 1 15 -2.06 4.59 -2 1 15 -5.39 4.86 -2 1 15 1.92 2.67 -1 1 15 9.71 6.79 -1 1 15 1.67 2.67 -5 2 15 0.49 3.89 -4 2 15 0.57 4.60 -3 2 15 -0.31 2.22 -3 2 15 -1.54 4.12 -2 2 15 0.41 2.50 -2 2 15 -2.95 4.88 -1 2 15 -0.27 2.69 -3 3 15 0.69 2.33 -2 3 15 -0.04 2.86 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 49713 data_4L1.4TBA.2SIF6 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C15 H13 N3 O5), 2(C16 H36 N), F6 Si' _chemical_formula_sum 'C62 H98 F6 N8 O10 Si' _chemical_formula_weight 1257.57 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 13.6859(6) _cell_length_b 17.7916(7) _cell_length_c 30.7988(14) _cell_angle_alpha 93.988(4) _cell_angle_beta 96.865(4) _cell_angle_gamma 109.357(4) _cell_volume 6976.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 10540 _cell_measurement_theta_min 3.40 _cell_measurement_theta_max 23.01 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.197 _exptl_crystal_F_000 2696 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.11 _exptl_absorpt_coefficient_mu 0.107 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.967 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details multi-scan _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 55807 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.921 _diffrn_reflns_theta_max 25.250 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 25235 _reflns_number_gt 12117 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0100P)^2^+10.3591P] 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 25235 _refine_ls_number_parameters 1587 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1709 _refine_ls_R_factor_gt 0.0935 _refine_ls_wR_factor_ref 0.1862 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.111 _refine_ls_shift/su_mean 0.003 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 C126 C 1.0283(12) -0.1040(10) 0.4011(4) 0.388(15) Uani 1 1 d . . . . . H203 H 0.9826 -0.1277 0.3739 0.583 Uiso 1 1 calc R U . . . H202 H 1.0231 -0.1441 0.4208 0.583 Uiso 1 1 calc R U . . . H201 H 1.0992 -0.0823 0.3955 0.583 Uiso 1 1 calc R U . . . Si1 Si 0.31019(10) 0.27041(7) 0.25704(4) 0.0598(3) Uani 1 1 d . . . . . C10 C 0.7890(3) 0.6844(3) 0.39778(14) 0.0628(11) Uani 1 1 d . . . . . C14 C 0.7985(4) 0.6236(3) 0.46465(15) 0.0720(13) Uani 1 1 d . . . . . H14 H 0.7871 0.6202 0.4937 0.086 Uiso 1 1 calc R U . . . C6 C 0.6847(3) 0.9074(3) 0.34922(14) 0.0635(11) Uani 1 1 d . . . . . C3 C 0.6337(3) 1.0463(3) 0.34423(16) 0.0685(12) Uani 1 1 d . . . . . C7 C 0.6866(4) 0.9549(3) 0.38738(15) 0.0731(13) Uani 1 1 d . . . . . H7 H 0.7055 0.9407 0.4148 0.088 Uiso 1 1 calc R U . . . C2 C 0.6072(4) 1.1201(3) 0.3428(2) 0.0812(15) Uani 1 1 d . . . . . C4 C 0.6327(4) 0.9988(3) 0.30662(16) 0.0761(14) Uani 1 1 d . . . . . H4 H 0.6145 1.0134 0.2792 0.091 Uiso 1 1 calc R U . . . C13 C 0.8421(3) 0.5736(3) 0.44466(15) 0.0610(11) Uani 1 1 d . . . . . C9 C 0.7263(4) 0.7981(3) 0.38379(16) 0.0687(12) Uani 1 1 d . . . . . C15 C 0.7721(4) 0.6788(3) 0.44116(14) 0.0694(12) Uani 1 1 d . . . . . H15 H 0.7425 0.7128 0.4545 0.083 Uiso 1 1 calc R U . . . C8 C 0.6604(4) 1.0233(3) 0.38451(16) 0.0758(13) Uani 1 1 d . . . . . H8 H 0.6608 1.0542 0.4102 0.091 Uiso 1 1 calc R U . . . C5 C 0.6579(4) 0.9305(3) 0.30887(15) 0.0756(13) Uani 1 1 d . . . . . H5 H 0.6571 0.8996 0.2831 0.091 Uiso 1 1 calc R U . . . C12 C 0.8601(4) 0.5782(3) 0.40230(16) 0.0746(13) Uani 1 1 d . . . . . H12 H 0.8903 0.5442 0.3894 0.090 Uiso 1 1 calc R U . . . C11 C 0.8338(4) 0.6328(3) 0.37859(15) 0.0767(14) Uani 1 1 d . . . . . H103 H 0.8457 0.6356 0.3496 0.092 Uiso 1 1 calc R U . . . C1 C 0.5731(5) 1.2117(4) 0.2955(2) 0.124(2) Uani 1 1 d . . . . . H1A H 0.5029 1.2035 0.3010 0.186 Uiso 1 1 calc R U . . . H1B H 0.5788 1.2238 0.2658 0.186 Uiso 1 1 calc R U . . . H1C H 0.6213 1.2556 0.3156 0.186 Uiso 1 1 calc R U . . . C21 C 0.2039(3) 0.4234(3) 0.35669(14) 0.0621(11) Uani 1 1 d . . . . . C24 C 0.2493(3) 0.3175(3) 0.39401(15) 0.0620(11) Uani 1 1 d . . . . . C27 C 0.3578(4) 0.0856(3) 0.41339(16) 0.0786(14) Uani 1 1 d . . . . . H27 H 0.3869 0.0503 0.4012 0.094 Uiso 1 1 calc R U . . . C26 C 0.3438(3) 0.1455(3) 0.39052(15) 0.0672(12) Uani 1 1 d . . . . . H26 H 0.3640 0.1511 0.3628 0.081 Uiso 1 1 calc R U . . . C18 C 0.1380(3) 0.5542(3) 0.34752(18) 0.0710(13) Uani 1 1 d . . . . . C22 C 0.1626(4) 0.4528(3) 0.39046(15) 0.0693(12) Uani 1 1 d . . . . . H22 H 0.1571 0.4289 0.4164 0.083 Uiso 1 1 calc R U . . . C28 C 0.3287(4) 0.0780(3) 0.45434(17) 0.0792(14) Uani 1 1 d . . . . . C30 C 0.2716(3) 0.1901(3) 0.45054(14) 0.0677(12) Uani 1 1 d . . . . . H30 H 0.2432 0.2255 0.4632 0.081 Uiso 1 1 calc R U . . . C23 C 0.1302(4) 0.5170(3) 0.38539(16) 0.0741(13) Uani 1 1 d . . . . . H23 H 0.1023 0.5361 0.4081 0.089 Uiso 1 1 calc R U . . . C19 C 0.1757(4) 0.5231(3) 0.31286(17) 0.0821(14) Uani 1 1 d . . . . . H19 H 0.1787 0.5459 0.2866 0.099 Uiso 1 1 calc R U . . . C25 C 0.2995(3) 0.1981(2) 0.40851(13) 0.0561(10) Uani 1 1 d . . . . . C17 C 0.1085(4) 0.6256(4) 0.3449(2) 0.0897(17) Uani 1 1 d . . . . . C20 C 0.2083(4) 0.4587(3) 0.31785(16) 0.0778(14) Uani 1 1 d . . . . . H20 H 0.2337 0.4383 0.2948 0.093 Uiso 1 1 calc R U . . . C29 C 0.2860(4) 0.1298(3) 0.47329(15) 0.0796(14) Uani 1 1 d . . . . . H29 H 0.2670 0.1241 0.5012 0.096 Uiso 1 1 calc R U . . . C16 C 0.0745(5) 0.7211(4) 0.3028(3) 0.167(3) Uani 1 1 d . . . . . H16A H 0.0042 0.7070 0.2878 0.251 Uiso 1 1 calc R U . . . H16B H 0.1218 0.7582 0.2872 0.251 Uiso 1 1 calc R U . . . H16C H 0.0791 0.7456 0.3321 0.251 Uiso 1 1 calc R U . . . C40 C 0.2794(3) 0.3325(3) 0.10351(16) 0.0686(12) Uani 1 1 d . . . . . C39 C 0.3373(4) 0.2158(3) 0.11517(16) 0.0708(13) Uani 1 1 d . . . . . C36 C 0.3953(3) 0.1114(3) 0.14905(16) 0.0694(13) Uani 1 1 d . . . . . C32 C 0.5012(5) -0.0871(4) 0.1531(3) 0.108(2) Uani 1 1 d . . . . . C45 C 0.2479(4) 0.3892(3) 0.12490(18) 0.0868(15) Uani 1 1 d . . . . . H45 H 0.2445 0.3893 0.1549 0.104 Uiso 1 1 calc R U . . . C34 C 0.4570(4) 0.0155(3) 0.11414(19) 0.0862(15) Uani 1 1 d . . . . . H34 H 0.4738 -0.0063 0.0890 0.103 Uiso 1 1 calc R U . . . C44 C 0.2214(4) 0.4454(3) 0.1027(2) 0.0985(17) Uani 1 1 d . . . . . H44 H 0.2005 0.4837 0.1173 0.118 Uiso 1 1 calc R U . . . C42 C 0.2583(5) 0.3896(4) 0.03638(19) 0.105(2) Uani 1 1 d . . . . . H42 H 0.2618 0.3903 0.0064 0.126 Uiso 1 1 calc R U . . . C35 C 0.4215(4) 0.0786(3) 0.11158(17) 0.0789(14) Uani 1 1 d . . . . . H35 H 0.4149 0.0996 0.0850 0.095 Uiso 1 1 calc R U . . . C37 C 0.4083(4) 0.0801(3) 0.18852(16) 0.0820(14) Uani 1 1 d . . . . . H37 H 0.3923 0.1021 0.2139 0.098 Uiso 1 1 calc R U . . . C41 C 0.2854(4) 0.3334(3) 0.05888(17) 0.0906(16) Uani 1 1 d . . . . . H41 H 0.3076 0.2960 0.0442 0.109 Uiso 1 1 calc R U . . . C38 C 0.4446(4) 0.0170(4) 0.19032(19) 0.0916(16) Uani 1 1 d . . . . . H38 H 0.4533 -0.0033 0.2170 0.110 Uiso 1 1 calc R U . . . C33 C 0.4686(4) -0.0168(3) 0.1530(2) 0.0865(16) Uani 1 1 d . . . . . C43 C 0.2264(5) 0.4437(4) 0.0584(2) 0.0965(17) Uani 1 1 d . . . . . C31 C 0.5526(6) -0.1814(5) 0.1923(3) 0.190(4) Uani 1 1 d . . . . . H31A H 0.5181 -0.2168 0.1659 0.285 Uiso 1 1 calc R U . . . H31B H 0.5319 -0.2082 0.2175 0.285 Uiso 1 1 calc R U . . . H31C H 0.6271 -0.1665 0.1935 0.285 Uiso 1 1 calc R U . . . C51 C 0.0834(4) 0.3890(3) 0.85775(18) 0.0791(14) Uani 1 1 d . . . . . C48 C 0.0354(5) 0.5293(5) 0.8537(3) 0.111(2) Uani 1 1 d . . . . . C52 C 0.0976(4) 0.4401(3) 0.8958(2) 0.0931(16) Uani 1 1 d . . . . . H52 H 0.1231 0.4280 0.9228 0.112 Uiso 1 1 calc R U . . . C54 C 0.1399(4) 0.2847(3) 0.89189(18) 0.0742(13) Uani 1 1 d . . . . . C58 C 0.2758(4) 0.0670(3) 0.94829(18) 0.0840(15) Uani 1 1 d . . . . . C60 C 0.2175(4) 0.1793(3) 0.94920(16) 0.0896(16) Uani 1 1 d . . . . . H60 H 0.2004 0.2187 0.9648 0.107 Uiso 1 1 calc R U . . . C49 C 0.0206(5) 0.4775(5) 0.8164(3) 0.118(2) Uani 1 1 d . . . . . H49 H -0.0062 0.4893 0.7895 0.141 Uiso 1 1 calc R U . . . C55 C 0.2090(4) 0.1742(3) 0.90409(16) 0.0728(13) Uani 1 1 d . . . . . C50 C 0.0450(4) 0.4083(4) 0.81809(19) 0.0966(17) Uani 1 1 d . . . . . H50 H 0.0355 0.3744 0.7924 0.116 Uiso 1 1 calc R U . . . C53 C 0.0732(5) 0.5097(4) 0.8929(2) 0.109(2) Uani 1 1 d . . . . . H53 H 0.0828 0.5441 0.9185 0.130 Uiso 1 1 calc R U . . . C47 C 0.0163(7) 0.6057(6) 0.8537(5) 0.155(5) Uani 1 1 d . . . . . C57 C 0.2672(5) 0.0608(4) 0.90417(19) 0.1055(19) Uani 1 1 d . . . . . H57 H 0.2834 0.0207 0.8888 0.127 Uiso 1 1 calc R U . . . C59 C 0.2520(5) 0.1246(3) 0.97135(17) 0.1003(19) Uani 1 1 d . . . . . H59 H 0.2586 0.1278 1.0019 0.120 Uiso 1 1 calc R U . . . C56 C 0.2343(5) 0.1145(4) 0.88228(18) 0.1033(19) Uani 1 1 d . . . . . H56 H 0.2288 0.1105 0.8518 0.124 Uiso 1 1 calc R U . . . C46 C -0.0374(6) 0.6923(5) 0.8057(4) 0.245(6) Uani 1 1 d . . . . . H46A H -0.0863 0.7005 0.8238 0.367 Uiso 1 1 calc R U . . . H46B H -0.0641 0.6913 0.7753 0.367 Uiso 1 1 calc R U . . . H46C H 0.0286 0.7353 0.8134 0.367 Uiso 1 1 calc R U . . . O8 O 0.2278(3) 0.3311(2) 0.42990(10) 0.0925(11) Uani 1 1 d . . . . . O13 O 0.3502(3) 0.2012(2) 0.07783(11) 0.0980(12) Uani 1 1 d . . . . . O18 O 0.1349(3) 0.3039(2) 0.92994(11) 0.0915(11) Uani 1 1 d . . . . . O2 O 0.5977(3) 1.1394(2) 0.30176(13) 0.1033(12) Uani 1 1 d . . . . . O7 O 0.1030(3) 0.6480(2) 0.30498(15) 0.1119(13) Uani 1 1 d . . . . . O3 O 0.7071(3) 0.8113(2) 0.42032(11) 0.0906(11) Uani 1 1 d . . . . . O1 O 0.5989(3) 1.1599(2) 0.37452(14) 0.1124(14) Uani 1 1 d . . . . . O17 O -0.0226(4) 0.6154(4) 0.8127(2) 0.182(3) Uani 1 1 d . . . . . O6 O 0.0904(3) 0.6624(2) 0.37577(16) 0.1120(14) Uani 1 1 d . . . . . O20 O 0.3317(4) -0.0423(3) 0.95090(17) 0.1491(19) Uani 1 1 d . . . . . O9 O 0.3079(6) 0.0015(3) 0.51181(16) 0.190(3) Uani 1 1 d . . . . . O4 O 0.8455(3) 0.5072(2) 0.50633(12) 0.0966(11) Uani 1 1 d . . . . . O10 O 0.3775(6) -0.0318(4) 0.4614(2) 0.209(3) Uani 1 1 d . . . . . O19 O 0.3120(5) 0.0130(3) 1.01132(16) 0.164(2) Uani 1 1 d . . . . . O14 O 0.5053(4) -0.1258(3) 0.11997(19) 0.1411(19) Uani 1 1 d . . . . . O5 O 0.9052(3) 0.4692(2) 0.45075(13) 0.1029(12) Uani 1 1 d . . . . . O12 O 0.2151(7) 0.5090(3) -0.0035(2) 0.211(3) Uani 1 1 d . . . . . O15 O 0.5221(4) -0.1065(3) 0.19239(18) 0.1400(18) Uani 1 1 d . . . . . O16 O 0.0343(6) 0.6551(4) 0.8837(3) 0.202(4) Uani 1 1 d . . . . . O11 O 0.1628(6) 0.5492(4) 0.0537(2) 0.198(3) Uani 1 1 d . . . . . N5 N 0.2852(3) 0.2555(2) 0.38259(11) 0.0604(9) Uani 1 1 d . . . . . H5B H 0.3004 0.2523 0.3564 0.073 Uiso 1 1 calc R U . . . N4 N 0.2410(3) 0.3598(2) 0.35941(12) 0.0707(10) Uani 1 1 d . . . . . H4B H 0.2615 0.3451 0.3360 0.085 Uiso 1 1 calc R U . . . N10 N 0.1094(3) 0.3202(3) 0.85702(13) 0.0819(12) Uani 1 1 d . . . . . H10 H 0.1061 0.2965 0.8313 0.098 Uiso 1 1 calc R U . . . N8 N 0.3045(3) 0.2772(2) 0.12883(12) 0.0733(11) Uani 1 1 d . . . . . H8A H 0.2986 0.2823 0.1563 0.088 Uiso 1 1 calc R U . . . N9 N 0.3558(3) 0.1743(2) 0.14919(12) 0.0770(11) Uani 1 1 d . . . . . H9 H 0.3411 0.1891 0.1740 0.092 Uiso 1 1 calc R U . . . N1 N 0.7120(3) 0.8390(2) 0.34897(12) 0.0747(11) Uani 1 1 d . . . . . H1 H 0.7211 0.8200 0.3239 0.090 Uiso 1 1 calc R U . . . N2 N 0.7637(3) 0.7377(2) 0.37142(12) 0.0752(11) Uani 1 1 d . . . . . H2 H 0.7723 0.7325 0.3443 0.090 Uiso 1 1 calc R U . . . N6 N 0.3415(5) 0.0127(3) 0.47847(18) 0.123(2) Uani 1 1 d . . . . . N3 N 0.8671(3) 0.5131(2) 0.46910(15) 0.0755(11) Uani 1 1 d . . . . . N11 N 0.1746(3) 0.2243(2) 0.87821(12) 0.0793(11) Uani 1 1 d . . . . . H11A H 0.1752 0.2165 0.8504 0.095 Uiso 1 1 calc R U . . . N12 N 0.3120(5) 0.0097(3) 0.9725(2) 0.1091(17) Uani 1 1 d . . . . . N7 N 0.1964(7) 0.5037(4) 0.0337(3) 0.148(3) Uani 1 1 d . . . . . N16 N 1.0019(3) 0.0650(2) 0.30975(13) 0.0759(11) Uani 1 1 d . . . . . N13 N 0.3855(3) 0.5307(2) 0.80443(15) 0.0869(13) Uani 1 1 d . . . . . N14 N 0.8169(3) 0.2043(3) 0.94306(17) 0.0954(14) Uani 1 1 d . . . . . N15 N 0.6425(3) 0.2877(2) 0.51860(14) 0.0799(11) Uani 1 1 d . . . . . C68 C 0.4765(4) 0.5253(3) 0.7821(2) 0.1008(18) Uani 1 1 d . . . . . H68A H 0.4879 0.5623 0.7601 0.121 Uiso 1 1 calc R U . . . H68B H 0.5393 0.5425 0.8039 0.121 Uiso 1 1 calc R U . . . C66 C 0.3645(4) 0.4756(3) 0.8403(2) 0.1058(19) Uani 1 1 d . . . . . H66A H 0.3433 0.4208 0.8265 0.127 Uiso 1 1 calc R U . . . H66B H 0.3053 0.4812 0.8530 0.127 Uiso 1 1 calc R U . . . C63 C 0.4153(4) 0.6181(3) 0.82364(19) 0.0989(18) Uani 1 1 d . . . . . H63A H 0.4774 0.6311 0.8455 0.119 Uiso 1 1 calc R U . . . H63B H 0.4340 0.6515 0.8003 0.119 Uiso 1 1 calc R U . . . C69 C 0.4616(5) 0.4427(4) 0.7604(2) 0.130(2) Uani 1 1 d . . . . . H69A H 0.4508 0.4052 0.7823 0.156 Uiso 1 1 calc R U . . . H69B H 0.3995 0.4252 0.7383 0.156 Uiso 1 1 calc R U . . . C61 C 0.2848(4) 0.5053(3) 0.77141(18) 0.0917(16) Uani 1 1 d . . . . . H61A H 0.2655 0.4486 0.7616 0.110 Uiso 1 1 calc R U . . . H61B H 0.2295 0.5121 0.7865 0.110 Uiso 1 1 calc R U . . . C62 C 0.2891(5) 0.5499(4) 0.7311(2) 0.122(2) Uani 1 1 d . . . . . H62A H 0.3268 0.5305 0.7108 0.147 Uiso 1 1 calc R U . . . H62B H 0.3271 0.6066 0.7398 0.147 Uiso 1 1 calc R U . . . C64 C 0.3327(5) 0.6402(4) 0.8448(2) 0.118(2) Uani 1 1 d . . . . . H64A H 0.2684 0.6245 0.8239 0.141 Uiso 1 1 calc R U . . . H64B H 0.3180 0.6112 0.8701 0.141 Uiso 1 1 calc R U . . . C70 C 0.5539(6) 0.4414(4) 0.7392(3) 0.155(3) Uani 1 1 d . . . . . H70A H 0.6152 0.4570 0.7617 0.186 Uiso 1 1 calc R U . . . H70B H 0.5666 0.4811 0.7185 0.186 Uiso 1 1 calc R U . . . C67 C 0.4541(6) 0.4878(4) 0.8781(3) 0.159(3) Uani 1 1 d D . . . . H67A H 0.4545 0.5288 0.9007 0.191 Uiso 1 1 calc R U . . . H67B H 0.5207 0.5053 0.8673 0.191 Uiso 1 1 calc R U . . . C65 C 0.3685(5) 0.7291(4) 0.8591(2) 0.129(3) Uani 1 1 d . . . . . H65A H 0.4310 0.7437 0.8809 0.155 Uiso 1 1 calc R U . . . H65B H 0.3875 0.7575 0.8339 0.155 Uiso 1 1 calc R U . . . C72 C 0.9079(4) 0.2322(4) 0.9810(2) 0.108(2) Uani 1 1 d . . . . . H72A H 0.9725 0.2414 0.9689 0.130 Uiso 1 1 calc R U . . . H72B H 0.9102 0.2832 0.9953 0.130 Uiso 1 1 calc R U . . . C75 C 0.7131(4) 0.1913(4) 0.9601(2) 0.1044(19) Uani 1 1 d . . . . . H75A H 0.6571 0.1713 0.9353 0.125 Uiso 1 1 calc R U . . . H75B H 0.7035 0.1497 0.9796 0.125 Uiso 1 1 calc R U . . . C71 C 0.8382(5) 0.2671(4) 0.9122(2) 0.122(2) Uani 1 1 d . . . . . H71A H 0.9049 0.2727 0.9026 0.146 Uiso 1 1 calc R U . . . H71B H 0.8454 0.3179 0.9284 0.146 Uiso 1 1 calc R U . . . C74 C 0.9011(5) 0.1185(4) 0.9002(2) 0.120(2) Uani 1 1 d . . . . . H74A H 0.9626 0.1356 0.9226 0.144 Uiso 1 1 calc R U . . . H74B H 0.9149 0.1525 0.8767 0.144 Uiso 1 1 calc R U . . . C73 C 0.8071(4) 0.1234(3) 0.9194(2) 0.1003(18) Uani 1 1 d . . . . . H73A H 0.7905 0.0839 0.9401 0.120 Uiso 1 1 calc R U . . . H73B H 0.7481 0.1083 0.8958 0.120 Uiso 1 1 calc R U . . . C76 C 0.7011(6) 0.2630(4) 0.9843(3) 0.141(3) Uani 1 1 d . . . . . H76A H 0.7123 0.3063 0.9659 0.169 Uiso 1 1 calc R U . . . H76B H 0.7522 0.2815 1.0109 0.169 Uiso 1 1 calc R U . . . C82 C 0.7582(3) 0.3004(3) 0.52037(17) 0.0803(14) Uani 1 1 d . . . . . H82A H 0.7902 0.3485 0.5069 0.096 Uiso 1 1 calc R U . . . H82B H 0.7900 0.3101 0.5510 0.096 Uiso 1 1 calc R U . . . C77 C 0.5875(4) 0.2741(3) 0.47145(17) 0.0861(15) Uani 1 1 d . . . . . H77A H 0.5143 0.2674 0.4719 0.103 Uiso 1 1 calc R U . . . H77B H 0.5902 0.2245 0.4573 0.103 Uiso 1 1 calc R U . . . C86 C 0.6348(4) 0.3624(3) 0.54292(18) 0.0903(16) Uani 1 1 d . . . . . H86A H 0.6659 0.3671 0.5734 0.108 Uiso 1 1 calc R U . . . H86B H 0.6762 0.4089 0.5303 0.108 Uiso 1 1 calc R U . . . C79 C 0.5584(4) 0.3387(3) 0.40325(19) 0.0988(18) Uani 1 1 d . . . . . H79A H 0.5369 0.2860 0.3866 0.119 Uiso 1 1 calc R U . . . H79B H 0.4963 0.3460 0.4122 0.119 Uiso 1 1 calc R U . . . C81 C 0.7847(4) 0.2326(3) 0.49822(19) 0.0933(16) Uani 1 1 d . . . . . H81A H 0.7534 0.2216 0.4675 0.112 Uiso 1 1 calc R U . . . H81B H 0.7565 0.1843 0.5122 0.112 Uiso 1 1 calc R U . . . C80 C 0.6032(5) 0.4007(4) 0.3739(2) 0.126(2) Uani 1 1 d . . . . . H80A H 0.6194 0.4532 0.3893 0.189 Uiso 1 1 calc R U . . . H80B H 0.5531 0.3938 0.3480 0.189 Uiso 1 1 calc R U . . . H80C H 0.6660 0.3949 0.3656 0.189 Uiso 1 1 calc R U . . . C85 C 0.5883(4) 0.2143(3) 0.5407(2) 0.0992(18) Uani 1 1 d . . . . . H85A H 0.5158 0.2103 0.5407 0.119 Uiso 1 1 calc R U . . . H85B H 0.5882 0.1669 0.5232 0.119 Uiso 1 1 calc R U . . . C78 C 0.6332(4) 0.3413(3) 0.44374(18) 0.0906(16) Uani 1 1 d . . . . . H78A H 0.6512 0.3925 0.4615 0.109 Uiso 1 1 calc R U . . . H78B H 0.6971 0.3370 0.4350 0.109 Uiso 1 1 calc R U . . . C83 C 0.9032(5) 0.2553(4) 0.5018(2) 0.114(2) Uani 1 1 d . . . . . H83A H 0.9305 0.3028 0.4872 0.137 Uiso 1 1 calc R U . . . H83B H 0.9340 0.2684 0.5326 0.137 Uiso 1 1 calc R U . . . C84 C 0.9355(5) 0.1889(4) 0.4816(3) 0.152(3) Uani 1 1 d . . . . . H84A H 0.9189 0.1448 0.4989 0.228 Uiso 1 1 calc R U . . . H84B H 1.0095 0.2085 0.4808 0.228 Uiso 1 1 calc R U . . . H84C H 0.8985 0.1711 0.4521 0.228 Uiso 1 1 calc R U . . . C96 C 1.1051(4) 0.0627(3) 0.29710(18) 0.0872(15) Uani 1 1 d . . . . . H96A H 1.1269 0.1010 0.2762 0.105 Uiso 1 1 calc R U . . . H96B H 1.1578 0.0800 0.3232 0.105 Uiso 1 1 calc R U . . . C90 C 0.9637(4) 0.0056(3) 0.34246(16) 0.0858(16) Uani 1 1 d . . . . . H90A H 0.8961 0.0066 0.3484 0.103 Uiso 1 1 calc R U . . . H90B H 0.9531 -0.0478 0.3287 0.103 Uiso 1 1 calc R U . . . C93 C 1.0230(4) 0.1499(3) 0.33006(16) 0.0812(15) Uani 1 1 d . . . . . H93A H 1.0544 0.1864 0.3096 0.097 Uiso 1 1 calc R U . . . H93B H 1.0742 0.1608 0.3564 0.097 Uiso 1 1 calc R U . . . C94 C 0.9288(4) 0.1687(3) 0.34215(18) 0.0899(16) Uani 1 1 d . . . . . H94A H 0.8763 0.1579 0.3162 0.108 Uiso 1 1 calc R U . . . H94B H 0.8981 0.1345 0.3637 0.108 Uiso 1 1 calc R U . . . C87 C 0.9172(4) 0.0415(3) 0.27028(16) 0.0870(15) Uani 1 1 d . . . . . H87A H 0.8525 0.0417 0.2800 0.104 Uiso 1 1 calc R U . . . H87B H 0.9066 -0.0131 0.2584 0.104 Uiso 1 1 calc R U . . . C95 C 0.9603(4) 0.2555(3) 0.3608(2) 0.110(2) Uani 1 1 d . . . . . H95A H 0.9930 0.2891 0.3394 0.132 Uiso 1 1 calc R U . . . H95B H 1.0121 0.2655 0.3869 0.132 Uiso 1 1 calc R U . . . C97 C 1.1026(5) -0.0181(3) 0.2772(2) 0.114(2) Uani 1 1 d . . . . . H97A H 1.0821 -0.0570 0.2979 0.137 Uiso 1 1 calc R U . . . H97B H 1.0509 -0.0360 0.2508 0.137 Uiso 1 1 calc R U . . . C91 C 1.0358(5) 0.0201(4) 0.3862(2) 0.121(2) Uani 1 1 d D . . . . H91A H 1.0473 0.0739 0.3995 0.145 Uiso 1 1 calc R U . . . H91B H 1.1030 0.0185 0.3801 0.145 Uiso 1 1 calc R U . . . C88 C 0.9388(5) 0.0947(4) 0.23364(19) 0.114(2) Uani 1 1 d . . . . . H88A H 0.9587 0.1502 0.2461 0.137 Uiso 1 1 calc R U . . . H88B H 0.9975 0.0886 0.2209 0.137 Uiso 1 1 calc R U . . . C89 C 0.8474(8) 0.0764(5) 0.1980(3) 0.177(4) Uani 1 1 d . . . . . H89A H 0.8719 0.1021 0.1727 0.213 Uiso 1 1 calc R U . . . H89B H 0.8200 0.0190 0.1893 0.213 Uiso 1 1 calc R U . . . Si2 Si 0.18399(10) 0.23257(7) 0.75232(4) 0.0602(3) Uani 1 1 d . . . . . F3 F 0.19616(19) 0.26456(16) 0.27380(8) 0.0801(7) Uani 1 1 d . . . . . F5 F 0.4230(2) 0.27564(16) 0.23979(9) 0.0830(8) Uani 1 1 d . . . . . F1 F 0.2895(2) 0.32478(17) 0.21674(9) 0.0889(8) Uani 1 1 d . . . . . F4 F 0.2499(2) 0.18637(16) 0.22279(9) 0.1047(10) Uani 1 1 d . . . . . F6 F 0.3314(2) 0.21751(17) 0.29787(9) 0.0957(9) Uani 1 1 d . . . . . F2 F 0.3692(2) 0.35451(16) 0.29131(9) 0.0898(8) Uani 1 1 d . . . . . F8 F 0.0829(3) 0.2418(3) 0.77066(11) 0.178(2) Uani 1 1 d . . . . . F7 F 0.2902(3) 0.2267(3) 0.73435(11) 0.1720(19) Uani 1 1 d . . . . . F10 F 0.2617(2) 0.2862(2) 0.79720(9) 0.1137(11) Uani 1 1 d . . . . . F12 F 0.2024(3) 0.3097(2) 0.72500(14) 0.1676(18) Uani 1 1 d . . . . . F9 F 0.1681(4) 0.1558(2) 0.77891(16) 0.211(3) Uani 1 1 d . . . . . F11 F 0.1084(3) 0.1797(2) 0.70747(10) 0.1326(13) Uani 1 1 d . . . . . C99 C 0.9046(5) 0.1759(4) 1.0155(2) 0.137(3) Uani 1 1 d . . . . . H99A H 0.8921 0.1226 1.0012 0.164 Uiso 1 1 calc R U . . . H99B H 0.8466 0.1733 1.0313 0.164 Uiso 1 1 calc R U . . . C98 C 0.7564(6) 0.2521(5) 0.8716(3) 0.161(3) Uani 1 1 d . . . . . H98A H 0.7449 0.1998 0.8562 0.193 Uiso 1 1 calc R U . . . H98B H 0.6907 0.2515 0.8807 0.193 Uiso 1 1 calc R U . . . C100 C 1.0048(6) 0.2017(6) 1.0478(3) 0.180(4) Uani 1 1 d . . . . . H10A H 1.0623 0.2034 1.0318 0.216 Uiso 1 1 calc R U . . . H10B H 1.0179 0.2557 1.0614 0.216 Uiso 1 1 calc R U . . . C101 C 0.8697(5) 0.2794(4) 0.3727(2) 0.134(2) Uani 1 1 d . . . . . H10C H 0.8216 0.2752 0.3466 0.201 Uiso 1 1 calc R U . . . H10D H 0.8958 0.3338 0.3866 0.201 Uiso 1 1 calc R U . . . H10E H 0.8344 0.2446 0.3927 0.201 Uiso 1 1 calc R U . . . C103 C 0.5878(6) 0.2381(5) 0.9962(3) 0.171(4) Uani 1 1 d . . . . . H10F H 0.5373 0.2146 0.9699 0.205 Uiso 1 1 calc R U . . . H10G H 0.5791 0.1981 1.0167 0.205 Uiso 1 1 calc R U . . . C102 C 0.7875(8) 0.3135(8) 0.8413(4) 0.257(7) Uani 1 1 d . . . . . H10H H 0.7963 0.3646 0.8575 0.308 Uiso 1 1 calc R U . . . H10I H 0.8563 0.3160 0.8351 0.308 Uiso 1 1 calc R U . . . C104 C 0.5686(8) 0.3084(7) 1.0163(4) 0.270(7) Uani 1 1 d . . . . . H10J H 0.6279 0.3392 1.0377 0.405 Uiso 1 1 calc R U . . . H10K H 0.5073 0.2910 1.0303 0.405 Uiso 1 1 calc R U . . . H10L H 0.5582 0.3410 0.9938 0.405 Uiso 1 1 calc R U . . . C106 C 1.2095(7) -0.0896(5) 0.2457(3) 0.206(4) Uani 1 1 d . . . . . H10M H 1.1855 -0.1303 0.2647 0.309 Uiso 1 1 calc R U . . . H10N H 1.2796 -0.0843 0.2412 0.309 Uiso 1 1 calc R U . . . H10O H 1.1642 -0.1044 0.2179 0.309 Uiso 1 1 calc R U . . . C105 C 1.2084(6) -0.0137(4) 0.2659(3) 0.163(4) Uani 1 1 d . . . . . H10P H 1.2294 0.0264 0.2458 0.195 Uiso 1 1 calc R U . . . H10Q H 1.2595 0.0034 0.2925 0.195 Uiso 1 1 calc R U . . . C107 C 0.7647(7) 0.1011(9) 0.2093(4) 0.311(10) Uani 1 1 d . . . . . H10R H 0.7171 0.0593 0.2223 0.466 Uiso 1 1 calc R U . . . H10S H 0.7281 0.1121 0.1833 0.466 Uiso 1 1 calc R U . . . H10T H 0.7927 0.1488 0.2299 0.466 Uiso 1 1 calc R U . . . C110 C 0.5293(9) 0.4366(7) 0.6019(5) 0.264(8) Uani 1 1 d . . . . . H11B H 0.4661 0.3929 0.6033 0.396 Uiso 1 1 calc R U . . . H11C H 0.5324 0.4822 0.6214 0.396 Uiso 1 1 calc R U . . . H102 H 0.5888 0.4210 0.6107 0.396 Uiso 1 1 calc R U . . . C108 C 0.5252(5) 0.3647(4) 0.5419(3) 0.154(3) Uani 1 1 d . . . . . H10U H 0.4873 0.3262 0.5601 0.185 Uiso 1 1 calc R U . . . H10V H 0.4881 0.3502 0.5120 0.185 Uiso 1 1 calc R U . . . C109 C 0.5302(10) 0.4561(9) 0.5603(3) 0.234(9) Uani 1 1 d . . . . . H10W H 0.5942 0.4980 0.5564 0.280 Uiso 1 1 calc R U . . . H200 H 0.4692 0.4688 0.5487 0.280 Uiso 1 1 calc R U . . . C113 C 0.6191(6) 0.1583(6) 0.6583(3) 0.217(5) Uani 1 1 d . . . . . H11E H 0.6470 0.2118 0.6733 0.325 Uiso 1 1 calc R U . . . H11F H 0.6742 0.1361 0.6581 0.325 Uiso 1 1 calc R U . . . H11G H 0.5657 0.1257 0.6734 0.325 Uiso 1 1 calc R U . . . C112 C 0.5730(6) 0.1601(6) 0.6120(3) 0.185(4) Uani 1 1 d . . . . . H11H H 0.5533 0.1067 0.5964 0.222 Uiso 1 1 calc R U . . . H11I H 0.5093 0.1725 0.6127 0.222 Uiso 1 1 calc R U . . . C111 C 0.6375(5) 0.2147(4) 0.5876(2) 0.130(2) Uani 1 1 d . . . . . H11J H 0.7014 0.2027 0.5867 0.156 Uiso 1 1 calc R U . . . H11K H 0.6567 0.2683 0.6028 0.156 Uiso 1 1 calc R U . . . C114 C 0.5413(6) 0.3614(5) 0.7152(3) 0.189(4) Uani 1 1 d . . . . . H11L H 0.5191 0.3203 0.7342 0.284 Uiso 1 1 calc R U . . . H11M H 0.6070 0.3626 0.7068 0.284 Uiso 1 1 calc R U . . . H11N H 0.4896 0.3501 0.6894 0.284 Uiso 1 1 calc R U . . . C115 C 0.2890(6) 0.7568(5) 0.8781(3) 0.186(4) Uani 1 1 d . . . . . H11O H 0.2301 0.7486 0.8557 0.279 Uiso 1 1 calc R U . . . H11P H 0.3198 0.8128 0.8888 0.279 Uiso 1 1 calc R U . . . H11Q H 0.2663 0.7267 0.9020 0.279 Uiso 1 1 calc R U . . . C116 C 0.7303(9) 0.3093(10) 0.8033(4) 0.334(10) Uani 1 1 d . . . . . H11R H 0.6842 0.2551 0.7946 0.501 Uiso 1 1 calc R U . . . H101 H 0.7751 0.3260 0.7815 0.501 Uiso 1 1 calc R U . . . H11T H 0.6897 0.3438 0.8060 0.501 Uiso 1 1 calc R U . . . C117 C 1.0037(9) 0.1502(8) 1.0818(4) 0.322(9) Uani 1 1 d . . . . . H11U H 0.9354 0.1323 1.0905 0.482 Uiso 1 1 calc R U . . . H11V H 1.0548 0.1792 1.1067 0.482 Uiso 1 1 calc R U . . . H11W H 1.0202 0.1047 1.0708 0.482 Uiso 1 1 calc R U . . . C118 C 0.8738(7) 0.0284(6) 0.8817(4) 0.215(6) Uani 1 1 d . . . . . H105 H 0.8694 -0.0038 0.9061 0.258 Uiso 1 1 calc R U . . . H104 H 0.8060 0.0097 0.8632 0.258 Uiso 1 1 calc R U . . . C121 C 0.4372(12) 0.4016(7) 0.8993(4) 0.371(15) Uani 1 1 d D . . . . H12A H 0.3687 0.3613 0.8895 0.446 Uiso 1 1 calc R U . . . H12B H 0.4924 0.3798 0.8959 0.446 Uiso 1 1 calc R U . . . C123 C 0.1791(7) 0.5389(5) 0.7076(2) 0.146(3) Uani 1 1 d . . . . . H12C H 0.1821 0.5449 0.6767 0.176 Uiso 1 1 calc R U . . . H12D H 0.1329 0.4849 0.7096 0.176 Uiso 1 1 calc R U . . . C124 C 0.1358(6) 0.5960(5) 0.7262(3) 0.185(4) Uani 1 1 d . . . . . H12E H 0.1131 0.5803 0.7535 0.277 Uiso 1 1 calc R U . . . H12F H 0.0772 0.5969 0.7060 0.277 Uiso 1 1 calc R U . . . H12G H 0.1884 0.6484 0.7313 0.277 Uiso 1 1 calc R U . . . C125 C 0.9977(12) -0.0396(6) 0.4211(5) 0.261(8) Uani 1 1 d D . . . . H12H H 1.0352 -0.0187 0.4505 0.313 Uiso 1 1 calc R U . . . H12I H 0.9228 -0.0556 0.4213 0.313 Uiso 1 1 calc R U . . . C127 C 0.9454(9) 0.0190(6) 0.8586(4) 0.238(5) Uani 1 1 d . . . . . H12M H 0.9611 0.0592 0.8388 0.357 Uiso 1 1 calc R U . . . H12N H 0.9191 -0.0333 0.8421 0.357 Uiso 1 1 calc R U . . . H12O H 1.0079 0.0243 0.8783 0.357 Uiso 1 1 calc R U . . . C128 C 0.4468(15) 0.4403(8) 0.9397(5) 0.395(12) Uani 1 1 d D . . . . H12P H 0.5066 0.4888 0.9439 0.592 Uiso 1 1 calc R U . . . H12Q H 0.4558 0.4064 0.9617 0.592 Uiso 1 1 calc R U . . . H12R H 0.3848 0.4532 0.9423 0.592 Uiso 1 1 calc R U . . . 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 C126 0.317(19) 0.45(3) 0.170(12) 0.195(15) -0.099(12) -0.161(18) Si1 0.0741(8) 0.0613(8) 0.0502(7) 0.0167(6) 0.0217(6) 0.0251(6) C10 0.075(3) 0.061(3) 0.056(3) 0.009(2) 0.018(2) 0.023(2) C14 0.094(4) 0.073(3) 0.052(3) 0.011(2) 0.019(2) 0.029(3) C6 0.072(3) 0.073(3) 0.051(3) 0.010(2) 0.014(2) 0.030(2) C3 0.070(3) 0.076(3) 0.068(3) 0.016(3) 0.014(2) 0.034(3) C7 0.095(4) 0.079(3) 0.055(3) 0.014(2) 0.011(2) 0.041(3) C2 0.085(4) 0.091(4) 0.079(4) 0.024(3) 0.019(3) 0.041(3) C4 0.080(3) 0.096(4) 0.062(3) 0.018(3) 0.007(2) 0.042(3) C13 0.068(3) 0.055(3) 0.056(3) 0.006(2) 0.007(2) 0.018(2) C9 0.087(3) 0.069(3) 0.058(3) 0.012(2) 0.015(3) 0.034(3) C15 0.096(4) 0.071(3) 0.053(3) 0.007(2) 0.023(2) 0.039(3) C8 0.092(4) 0.079(3) 0.064(3) 0.008(3) 0.019(3) 0.038(3) C5 0.090(4) 0.089(4) 0.058(3) 0.007(3) 0.011(3) 0.044(3) C12 0.098(4) 0.068(3) 0.070(3) 0.010(3) 0.029(3) 0.039(3) C11 0.111(4) 0.080(3) 0.057(3) 0.016(3) 0.037(3) 0.047(3) C1 0.146(6) 0.124(5) 0.135(6) 0.044(4) 0.011(4) 0.086(5) C21 0.067(3) 0.065(3) 0.053(3) 0.007(2) 0.012(2) 0.021(2) C24 0.072(3) 0.063(3) 0.048(3) 0.004(2) 0.005(2) 0.022(2) C27 0.096(4) 0.071(3) 0.072(4) 0.014(3) 0.016(3) 0.031(3) C26 0.077(3) 0.072(3) 0.057(3) 0.013(2) 0.020(2) 0.027(3) C18 0.058(3) 0.067(3) 0.087(4) 0.006(3) 0.000(3) 0.023(2) C22 0.087(3) 0.059(3) 0.058(3) 0.004(2) 0.012(2) 0.021(3) C28 0.109(4) 0.062(3) 0.064(3) 0.018(3) 0.008(3) 0.025(3) C30 0.089(3) 0.070(3) 0.046(3) 0.009(2) 0.013(2) 0.029(3) C23 0.080(3) 0.071(3) 0.069(3) 0.002(3) 0.012(3) 0.024(3) C19 0.094(4) 0.086(4) 0.074(4) 0.026(3) 0.013(3) 0.037(3) C25 0.056(3) 0.056(3) 0.048(3) 0.005(2) 0.0068(19) 0.009(2) C17 0.071(4) 0.084(4) 0.112(5) 0.024(4) -0.002(3) 0.027(3) C20 0.093(4) 0.087(4) 0.064(3) 0.018(3) 0.024(3) 0.040(3) C29 0.113(4) 0.076(3) 0.047(3) 0.013(2) 0.015(3) 0.025(3) C16 0.150(7) 0.129(6) 0.216(9) 0.078(6) -0.023(6) 0.045(5) C40 0.063(3) 0.072(3) 0.061(3) 0.007(3) 0.009(2) 0.009(2) C39 0.076(3) 0.076(3) 0.054(3) 0.002(3) 0.009(2) 0.019(3) C36 0.065(3) 0.070(3) 0.061(3) 0.003(2) 0.009(2) 0.009(2) C32 0.080(4) 0.108(6) 0.127(7) 0.014(5) -0.009(4) 0.029(4) C45 0.099(4) 0.099(4) 0.074(4) 0.018(3) 0.027(3) 0.043(3) C34 0.086(4) 0.081(4) 0.087(4) -0.001(3) 0.018(3) 0.024(3) C44 0.116(5) 0.099(4) 0.093(5) 0.025(4) 0.031(4) 0.045(4) C42 0.152(6) 0.089(4) 0.061(4) 0.009(3) 0.006(4) 0.027(4) C35 0.087(4) 0.077(4) 0.068(3) 0.006(3) 0.014(3) 0.021(3) C37 0.087(4) 0.100(4) 0.058(3) 0.010(3) 0.005(3) 0.033(3) C41 0.124(5) 0.083(4) 0.059(3) 0.007(3) 0.010(3) 0.029(3) C38 0.082(4) 0.109(5) 0.076(4) 0.020(3) -0.001(3) 0.026(3) C33 0.064(3) 0.084(4) 0.102(5) 0.006(4) -0.001(3) 0.020(3) C43 0.120(5) 0.080(4) 0.080(4) 0.018(3) 0.001(3) 0.025(3) C31 0.168(8) 0.159(8) 0.238(10) 0.052(7) -0.042(7) 0.069(6) C51 0.074(3) 0.097(4) 0.075(4) 0.023(3) 0.026(3) 0.033(3) C48 0.081(4) 0.116(6) 0.160(8) 0.061(5) 0.050(5) 0.046(4) C52 0.100(4) 0.100(4) 0.093(5) 0.025(4) 0.028(3) 0.045(4) C54 0.072(3) 0.080(4) 0.068(4) 0.018(3) 0.021(3) 0.018(3) C58 0.104(4) 0.074(4) 0.065(4) 0.011(3) 0.008(3) 0.019(3) C60 0.134(5) 0.076(4) 0.056(3) 0.003(3) 0.010(3) 0.035(3) C49 0.085(4) 0.148(7) 0.138(7) 0.080(6) 0.038(4) 0.045(5) C55 0.082(3) 0.078(3) 0.054(3) 0.011(3) 0.016(2) 0.019(3) C50 0.089(4) 0.125(5) 0.085(4) 0.038(4) 0.027(3) 0.038(4) C53 0.103(5) 0.100(5) 0.136(6) 0.020(4) 0.037(4) 0.045(4) C47 0.099(6) 0.134(9) 0.273(15) 0.103(9) 0.066(8) 0.065(6) C57 0.157(6) 0.112(5) 0.069(4) 0.022(3) 0.031(4) 0.068(4) C59 0.150(5) 0.093(4) 0.047(3) 0.006(3) -0.001(3) 0.032(4) C56 0.156(6) 0.122(5) 0.057(4) 0.024(3) 0.033(3) 0.072(4) C46 0.156(8) 0.182(9) 0.455(18) 0.186(11) 0.077(9) 0.095(7) O8 0.149(3) 0.103(3) 0.049(2) 0.0137(18) 0.030(2) 0.070(2) O13 0.142(3) 0.118(3) 0.049(2) 0.005(2) 0.024(2) 0.062(3) O18 0.123(3) 0.102(3) 0.056(2) 0.0130(19) 0.029(2) 0.043(2) O2 0.126(3) 0.102(3) 0.099(3) 0.028(2) 0.009(2) 0.062(2) O7 0.130(3) 0.095(3) 0.123(4) 0.028(3) -0.003(3) 0.059(3) O3 0.149(3) 0.094(3) 0.055(2) 0.0186(18) 0.039(2) 0.066(2) O1 0.152(4) 0.118(3) 0.107(3) 0.028(3) 0.043(3) 0.087(3) O17 0.138(4) 0.164(5) 0.289(8) 0.127(6) 0.059(5) 0.083(4) O6 0.126(3) 0.100(3) 0.130(4) 0.019(3) 0.022(3) 0.064(3) O20 0.223(6) 0.135(4) 0.126(4) 0.043(3) 0.039(4) 0.101(4) O9 0.407(9) 0.136(4) 0.077(3) 0.053(3) 0.075(5) 0.139(5) O4 0.147(3) 0.085(3) 0.068(2) 0.023(2) 0.026(2) 0.047(2) O10 0.401(10) 0.172(5) 0.157(5) 0.091(4) 0.113(6) 0.197(6) O19 0.298(7) 0.108(4) 0.077(3) 0.015(3) -0.019(4) 0.073(4) O14 0.148(4) 0.132(4) 0.160(5) 0.006(4) 0.007(4) 0.079(3) O5 0.140(3) 0.096(3) 0.102(3) 0.024(2) 0.035(2) 0.070(3) O12 0.399(10) 0.145(5) 0.098(4) 0.035(4) 0.003(5) 0.115(6) O15 0.148(4) 0.123(4) 0.147(5) 0.011(3) -0.038(3) 0.066(3) O16 0.175(6) 0.128(6) 0.341(13) 0.060(6) 0.073(7) 0.085(5) O11 0.314(9) 0.164(6) 0.178(6) 0.076(5) 0.079(6) 0.141(6) N5 0.068(2) 0.070(2) 0.048(2) 0.0093(18) 0.0142(17) 0.0266(19) N4 0.097(3) 0.077(3) 0.052(2) 0.0109(19) 0.025(2) 0.043(2) N10 0.098(3) 0.099(3) 0.060(3) 0.014(2) 0.019(2) 0.046(3) N8 0.085(3) 0.086(3) 0.050(2) 0.006(2) 0.013(2) 0.031(2) N9 0.098(3) 0.087(3) 0.048(2) 0.003(2) 0.019(2) 0.033(2) N1 0.109(3) 0.077(3) 0.055(2) 0.011(2) 0.019(2) 0.051(2) N2 0.108(3) 0.080(3) 0.054(2) 0.015(2) 0.024(2) 0.049(2) N6 0.226(7) 0.088(4) 0.072(4) 0.020(3) 0.026(4) 0.071(4) N3 0.088(3) 0.067(3) 0.070(3) 0.010(2) 0.011(2) 0.025(2) N11 0.105(3) 0.094(3) 0.049(2) 0.017(2) 0.021(2) 0.043(3) N12 0.154(5) 0.087(4) 0.081(4) 0.014(3) 0.004(4) 0.039(3) N7 0.234(8) 0.104(5) 0.111(6) 0.027(4) 0.011(5) 0.068(5) N16 0.074(3) 0.063(3) 0.075(3) 0.007(2) 0.016(2) 0.001(2) N13 0.070(3) 0.072(3) 0.102(3) 0.013(2) 0.024(2) -0.002(2) N14 0.078(3) 0.088(3) 0.116(4) 0.016(3) 0.033(3) 0.014(2) N15 0.071(3) 0.069(3) 0.089(3) 0.002(2) 0.005(2) 0.013(2) C68 0.083(4) 0.077(4) 0.135(5) 0.018(4) 0.039(4) 0.009(3) C66 0.097(4) 0.085(4) 0.113(5) 0.025(3) 0.027(4) -0.004(3) C63 0.084(4) 0.073(4) 0.112(5) 0.002(3) 0.018(3) -0.010(3) C69 0.116(5) 0.087(5) 0.188(7) 0.015(5) 0.067(5) 0.021(4) C61 0.077(4) 0.082(4) 0.095(4) -0.006(3) 0.015(3) 0.003(3) C62 0.124(6) 0.136(6) 0.100(5) 0.021(4) 0.029(4) 0.031(4) C64 0.092(4) 0.110(5) 0.125(6) -0.022(4) 0.031(4) 0.004(4) C70 0.144(6) 0.095(5) 0.239(10) 0.014(5) 0.102(6) 0.033(5) C67 0.121(6) 0.170(7) 0.148(7) 0.052(6) -0.012(5) 0.002(5) C65 0.103(5) 0.104(5) 0.157(7) -0.035(4) 0.030(4) 0.012(4) C72 0.074(4) 0.106(5) 0.125(6) -0.012(4) 0.019(4) 0.009(3) C75 0.078(4) 0.111(5) 0.127(5) 0.041(4) 0.040(4) 0.023(3) C71 0.110(5) 0.113(5) 0.152(7) 0.049(5) 0.068(5) 0.027(4) C74 0.093(5) 0.129(6) 0.130(6) -0.010(4) 0.019(4) 0.030(4) C73 0.077(4) 0.093(4) 0.117(5) 0.006(4) 0.015(3) 0.012(3) C76 0.143(6) 0.126(6) 0.179(8) 0.042(5) 0.087(6) 0.053(5) C82 0.061(3) 0.080(4) 0.090(4) 0.012(3) 0.002(3) 0.013(3) C77 0.068(3) 0.079(4) 0.093(4) -0.004(3) -0.011(3) 0.012(3) C86 0.074(4) 0.083(4) 0.101(4) -0.007(3) 0.011(3) 0.014(3) C79 0.080(4) 0.097(4) 0.105(5) 0.005(3) -0.010(3) 0.022(3) C81 0.091(4) 0.087(4) 0.102(4) 0.014(3) 0.018(3) 0.030(3) C80 0.125(5) 0.119(5) 0.115(5) 0.035(4) -0.007(4) 0.021(4) C85 0.084(4) 0.086(4) 0.115(5) 0.018(3) 0.016(3) 0.011(3) C78 0.081(4) 0.087(4) 0.092(4) 0.008(3) 0.001(3) 0.017(3) C83 0.096(5) 0.126(5) 0.130(6) 0.012(4) 0.012(4) 0.052(4) C84 0.139(6) 0.171(7) 0.180(8) 0.031(6) 0.026(5) 0.095(6) C96 0.087(4) 0.069(3) 0.099(4) 0.013(3) 0.027(3) 0.013(3) C90 0.087(4) 0.070(3) 0.080(4) 0.016(3) 0.016(3) -0.003(3) C93 0.082(4) 0.063(3) 0.079(4) -0.001(3) 0.014(3) 0.000(3) C94 0.074(4) 0.091(4) 0.087(4) -0.005(3) 0.018(3) 0.007(3) C87 0.095(4) 0.075(3) 0.072(4) -0.004(3) 0.003(3) 0.010(3) C95 0.094(4) 0.089(4) 0.136(6) -0.007(4) 0.021(4) 0.020(3) C97 0.134(6) 0.083(4) 0.127(6) 0.014(4) 0.051(4) 0.029(4) C91 0.124(5) 0.111(5) 0.099(5) 0.036(4) -0.001(4) 0.004(4) C88 0.143(6) 0.118(5) 0.077(4) 0.014(4) 0.018(4) 0.037(4) C89 0.229(10) 0.141(7) 0.097(6) 0.011(5) -0.043(7) 0.001(7) Si2 0.0769(9) 0.0534(7) 0.0495(7) 0.0056(6) 0.0068(6) 0.0224(6) F3 0.0707(17) 0.0957(19) 0.0739(18) 0.0091(14) 0.0257(13) 0.0238(14) F5 0.0837(18) 0.101(2) 0.085(2) 0.0344(16) 0.0408(15) 0.0453(16) F1 0.110(2) 0.106(2) 0.0715(19) 0.0420(16) 0.0261(15) 0.0546(18) F4 0.129(2) 0.0811(19) 0.086(2) -0.0141(16) 0.0492(18) 0.0056(17) F6 0.127(2) 0.115(2) 0.080(2) 0.0559(17) 0.0459(17) 0.0679(19) F2 0.091(2) 0.088(2) 0.0758(19) -0.0079(15) 0.0219(15) 0.0118(15) F8 0.116(3) 0.350(6) 0.083(3) -0.028(3) 0.009(2) 0.112(4) F7 0.154(3) 0.315(6) 0.084(3) -0.037(3) 0.008(2) 0.145(4) F10 0.097(2) 0.139(3) 0.0656(19) -0.0164(18) 0.0056(16) -0.0032(19) F12 0.191(4) 0.098(3) 0.170(4) 0.068(3) -0.031(3) 0.001(3) F9 0.251(5) 0.091(3) 0.212(5) 0.078(3) -0.086(4) -0.016(3) F11 0.148(3) 0.125(3) 0.073(2) -0.0181(19) -0.015(2) -0.006(2) C99 0.106(5) 0.146(7) 0.132(6) 0.016(5) -0.008(5) 0.017(5) C98 0.134(7) 0.194(8) 0.171(8) 0.099(7) 0.048(6) 0.053(6) C100 0.124(7) 0.209(10) 0.147(8) 0.002(7) -0.028(6) -0.003(6) C101 0.125(6) 0.141(6) 0.144(6) -0.005(5) 0.026(5) 0.057(5) C103 0.154(7) 0.212(10) 0.193(9) 0.029(7) 0.090(6) 0.099(7) C102 0.173(10) 0.327(15) 0.247(14) 0.194(13) 0.050(9) 0.015(10) C104 0.268(13) 0.347(17) 0.308(16) 0.159(13) 0.177(12) 0.185(13) C106 0.238(10) 0.175(9) 0.273(12) 0.090(8) 0.136(9) 0.114(8) C105 0.206(8) 0.088(5) 0.229(9) 0.026(5) 0.135(7) 0.060(5) C107 0.116(8) 0.54(3) 0.256(15) 0.182(15) 0.008(8) 0.066(11) C110 0.152(9) 0.143(9) 0.47(3) -0.045(15) 0.024(15) 0.039(7) C108 0.095(5) 0.149(7) 0.203(8) -0.064(6) 0.025(5) 0.037(4) C109 0.150(8) 0.35(2) 0.184(11) -0.137(13) -0.008(8) 0.115(10) C113 0.138(7) 0.314(13) 0.169(9) 0.142(9) 0.028(6) 0.016(7) C112 0.125(7) 0.260(11) 0.167(9) 0.096(8) 0.055(6) 0.039(7) C111 0.105(5) 0.153(6) 0.118(6) 0.049(5) 0.021(4) 0.018(4) C114 0.182(8) 0.137(7) 0.274(12) 0.029(7) 0.123(8) 0.057(6) C115 0.148(7) 0.166(8) 0.228(10) -0.042(7) 0.019(7) 0.050(6) C116 0.185(12) 0.51(2) 0.282(17) 0.260(18) 0.024(11) 0.046(13) C117 0.241(13) 0.349(18) 0.261(15) 0.139(13) -0.121(11) -0.014(11) C118 0.138(8) 0.192(9) 0.271(13) -0.111(9) 0.098(8) 0.003(6) C121 0.274(16) 0.48(3) 0.163(11) 0.193(15) -0.056(12) -0.130(16) C123 0.158(8) 0.164(8) 0.106(6) -0.022(5) -0.002(5) 0.055(6) C124 0.150(8) 0.197(10) 0.202(10) 0.050(8) 0.019(7) 0.050(7) C125 0.244(13) 0.129(9) 0.37(2) 0.073(11) 0.069(13) -0.008(9) C127 0.231(13) 0.211(11) 0.213(12) -0.036(9) -0.001(10) 0.022(10) C128 0.48(3) 0.303(18) 0.39(3) 0.153(19) 0.25(3) 0.043(19) _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 C126 C125 1.46(2) . ? Si1 F2 1.668(3) . ? Si1 F5 1.668(3) . ? Si1 F4 1.668(3) . ? Si1 F3 1.675(3) . ? Si1 F6 1.676(3) . ? Si1 F1 1.679(3) . ? C10 C15 1.388(6) . ? C10 N2 1.391(5) . ? C10 C11 1.397(6) . ? C14 C13 1.375(6) . ? C14 C15 1.375(6) . ? C6 C5 1.382(6) . ? C6 N1 1.387(5) . ? C6 C7 1.391(6) . ? C3 C8 1.379(6) . ? C3 C4 1.381(6) . ? C3 C2 1.477(7) . ? C7 C8 1.383(6) . ? C2 O1 1.204(6) . ? C2 O2 1.336(6) . ? C4 C5 1.373(6) . ? C13 C12 1.359(6) . ? C13 N3 1.461(5) . ? C9 O3 1.210(5) . ? C9 N1 1.368(5) . ? C9 N2 1.384(5) . ? C12 C11 1.370(6) . ? C1 O2 1.454(6) . ? C21 C20 1.388(6) . ? C21 N4 1.388(5) . ? C21 C22 1.391(6) . ? C24 O8 1.207(5) . ? C24 N4 1.362(5) . ? C24 N5 1.388(5) . ? C27 C26 1.370(6) . ? C27 C28 1.369(6) . ? C26 C25 1.390(6) . ? C18 C23 1.378(6) . ? C18 C19 1.397(6) . ? C18 C17 1.460(7) . ? C22 C23 1.368(6) . ? C28 C29 1.378(6) . ? C28 N6 1.467(6) . ? C30 C29 1.375(6) . ? C30 C25 1.396(5) . ? C19 C20 1.372(6) . ? C25 N5 1.388(5) . ? C17 O6 1.213(7) . ? C17 O7 1.320(7) . ? C16 O7 1.479(7) . ? C40 C45 1.380(6) . ? C40 C41 1.388(6) . ? C40 N8 1.401(6) . ? C39 O13 1.208(5) . ? C39 N9 1.369(6) . ? C39 N8 1.370(6) . ? C36 C37 1.388(6) . ? C36 C35 1.394(6) . ? C36 N9 1.396(6) . ? C32 O14 1.209(8) . ? C32 O15 1.305(8) . ? C32 C33 1.462(8) . ? C45 C44 1.368(7) . ? C34 C35 1.367(6) . ? C34 C33 1.378(7) . ? C44 C43 1.374(7) . ? C42 C43 1.355(8) . ? C42 C41 1.378(7) . ? C37 C38 1.373(7) . ? C38 C33 1.383(7) . ? C43 N7 1.488(8) . ? C31 O15 1.524(8) . ? C51 C50 1.382(7) . ? C51 N10 1.383(6) . ? C51 C52 1.384(7) . ? C48 C53 1.370(8) . ? C48 C49 1.374(9) . ? C48 C47 1.466(11) . ? C52 C53 1.392(7) . ? C54 O18 1.214(5) . ? C54 N11 1.372(6) . ? C54 N10 1.374(6) . ? C58 C57 1.343(7) . ? C58 C59 1.355(7) . ? C58 N12 1.481(7) . ? C60 C55 1.374(6) . ? C60 C59 1.398(7) . ? C49 C50 1.382(8) . ? C55 C56 1.379(7) . ? C55 N11 1.393(6) . ? C47 O16 1.175(14) . ? C47 O17 1.355(14) . ? C57 C56 1.368(7) . ? C46 O17 1.476(8) . ? O20 N12 1.222(6) . ? O9 N6 1.177(6) . ? O4 N3 1.221(5) . ? O10 N6 1.186(6) . ? O19 N12 1.192(6) . ? O5 N3 1.218(5) . ? O12 N7 1.208(8) . ? O11 N7 1.221(8) . ? N16 C87 1.506(6) . ? N16 C93 1.515(5) . ? N16 C96 1.521(6) . ? N16 C90 1.521(5) . ? N13 C66 1.518(6) . ? N13 C68 1.519(6) . ? N13 C63 1.525(6) . ? N13 C61 1.525(6) . ? N14 C71 1.494(7) . ? N14 C73 1.524(6) . ? N14 C72 1.525(7) . ? N14 C75 1.525(6) . ? N15 C82 1.516(5) . ? N15 C77 1.518(6) . ? N15 C86 1.521(6) . ? N15 C85 1.523(6) . ? C68 C69 1.510(7) . ? C66 C67 1.535(8) . ? C63 C64 1.514(7) . ? C69 C70 1.494(7) . ? C61 C62 1.518(7) . ? C62 C123 1.533(9) . ? C64 C65 1.508(7) . ? C70 C114 1.505(8) . ? C67 C121 1.665(10) . ? C65 C115 1.495(8) . ? C72 C99 1.502(8) . ? C75 C76 1.499(8) . ? C71 C98 1.519(9) . ? C74 C73 1.504(7) . ? C74 C118 1.567(9) . ? C76 C103 1.561(8) . ? C82 C81 1.513(6) . ? C77 C78 1.524(6) . ? C86 C108 1.511(7) . ? C79 C80 1.494(7) . ? C79 C78 1.504(6) . ? C81 C83 1.523(7) . ? C85 C111 1.517(7) . ? C83 C84 1.513(8) . ? C96 C97 1.511(7) . ? C90 C91 1.523(7) . ? C93 C94 1.516(6) . ? C94 C95 1.508(6) . ? C87 C88 1.517(7) . ? C95 C101 1.513(7) . ? C97 C105 1.509(8) . ? C91 C125 1.575(12) . ? C88 C89 1.491(9) . ? C89 C107 1.413(13) . ? Si2 F9 1.607(4) . ? Si2 F8 1.608(3) . ? Si2 F12 1.624(3) . ? Si2 F11 1.642(3) . ? Si2 F7 1.648(4) . ? Si2 F10 1.657(3) . ? C99 C100 1.509(8) . ? C98 C102 1.475(10) . ? C100 C117 1.437(11) . ? C103 C104 1.471(11) . ? C102 C116 1.310(12) . ? C106 C105 1.452(9) . ? C110 C109 1.353(17) . ? C108 C109 1.662(14) . ? C113 C112 1.498(9) . ? C112 C111 1.407(8) . ? C118 C127 1.324(11) . ? C121 C128 1.349(10) . ? C123 C124 1.453(9) . ? 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 F2 Si1 F5 91.25(15) . . ? F2 Si1 F4 179.37(17) . . ? F5 Si1 F4 89.35(15) . . ? F2 Si1 F3 89.33(14) . . ? F5 Si1 F3 179.34(17) . . ? F4 Si1 F3 90.06(15) . . ? F2 Si1 F6 89.14(16) . . ? F5 Si1 F6 91.87(14) . . ? F4 Si1 F6 91.03(17) . . ? F3 Si1 F6 88.43(14) . . ? F2 Si1 F1 89.92(15) . . ? F5 Si1 F1 88.35(14) . . ? F4 Si1 F1 89.91(16) . . ? F3 Si1 F1 91.37(14) . . ? F6 Si1 F1 179.04(17) . . ? C15 C10 N2 124.7(4) . . ? C15 C10 C11 118.5(4) . . ? N2 C10 C11 116.9(4) . . ? C13 C14 C15 119.2(4) . . ? C5 C6 N1 117.2(4) . . ? C5 C6 C7 118.9(4) . . ? N1 C6 C7 123.9(4) . . ? C8 C3 C4 118.3(5) . . ? C8 C3 C2 119.1(5) . . ? C4 C3 C2 122.6(5) . . ? C8 C7 C6 120.0(4) . . ? O1 C2 O2 123.9(5) . . ? O1 C2 C3 125.0(5) . . ? O2 C2 C3 111.1(5) . . ? C5 C4 C3 121.3(5) . . ? C12 C13 C14 121.2(4) . . ? C12 C13 N3 119.5(4) . . ? C14 C13 N3 119.3(4) . . ? O3 C9 N1 125.1(4) . . ? O3 C9 N2 124.2(4) . . ? N1 C9 N2 110.7(4) . . ? C14 C15 C10 120.7(4) . . ? C3 C8 C7 121.1(5) . . ? C4 C5 C6 120.4(5) . . ? C13 C12 C11 120.0(4) . . ? C12 C11 C10 120.4(4) . . ? C20 C21 N4 117.5(4) . . ? C20 C21 C22 118.9(4) . . ? N4 C21 C22 123.7(4) . . ? O8 C24 N4 124.9(4) . . ? O8 C24 N5 123.9(4) . . ? N4 C24 N5 111.1(4) . . ? C26 C27 C28 119.7(5) . . ? C27 C26 C25 120.4(4) . . ? C23 C18 C19 118.9(5) . . ? C23 C18 C17 119.4(5) . . ? C19 C18 C17 121.7(5) . . ? C23 C22 C21 119.8(4) . . ? C27 C28 C29 121.3(5) . . ? C27 C28 N6 119.8(5) . . ? C29 C28 N6 118.9(5) . . ? C29 C30 C25 120.1(4) . . ? C22 C23 C18 121.6(5) . . ? C20 C19 C18 119.6(5) . . ? N5 C25 C26 116.6(4) . . ? N5 C25 C30 124.3(4) . . ? C26 C25 C30 119.1(4) . . ? O6 C17 O7 121.6(6) . . ? O6 C17 C18 124.8(6) . . ? O7 C17 C18 113.6(6) . . ? C19 C20 C21 121.2(5) . . ? C30 C29 C28 119.4(5) . . ? C45 C40 C41 119.1(5) . . ? C45 C40 N8 117.1(5) . . ? C41 C40 N8 123.8(5) . . ? O13 C39 N9 124.3(5) . . ? O13 C39 N8 124.0(5) . . ? N9 C39 N8 111.7(4) . . ? C37 C36 C35 119.0(5) . . ? C37 C36 N9 117.5(5) . . ? C35 C36 N9 123.5(5) . . ? O14 C32 O15 122.6(7) . . ? O14 C32 C33 123.4(7) . . ? O15 C32 C33 113.9(7) . . ? C44 C45 C40 121.1(5) . . ? C35 C34 C33 121.8(5) . . ? C45 C44 C43 118.3(6) . . ? C43 C42 C41 119.2(6) . . ? C34 C35 C36 119.6(5) . . ? C38 C37 C36 120.3(5) . . ? C42 C41 C40 120.0(5) . . ? C37 C38 C33 120.9(5) . . ? C34 C33 C38 118.4(6) . . ? C34 C33 C32 119.3(6) . . ? C38 C33 C32 122.3(6) . . ? C42 C43 C44 122.3(6) . . ? C42 C43 N7 118.8(6) . . ? C44 C43 N7 118.9(6) . . ? C50 C51 N10 117.6(6) . . ? C50 C51 C52 119.2(6) . . ? N10 C51 C52 123.1(5) . . ? C53 C48 C49 118.2(7) . . ? C53 C48 C47 118.2(10) . . ? C49 C48 C47 123.6(9) . . ? C51 C52 C53 118.9(6) . . ? O18 C54 N11 124.5(5) . . ? O18 C54 N10 123.9(5) . . ? N11 C54 N10 111.6(5) . . ? C57 C58 C59 121.6(6) . . ? C57 C58 N12 119.5(6) . . ? C59 C58 N12 118.9(5) . . ? C55 C60 C59 119.3(5) . . ? C48 C49 C50 121.0(7) . . ? C60 C55 C56 118.4(5) . . ? C60 C55 N11 124.8(5) . . ? C56 C55 N11 116.8(5) . . ? C49 C50 C51 120.5(6) . . ? C48 C53 C52 122.1(7) . . ? O16 C47 O17 122.0(10) . . ? O16 C47 C48 127.0(14) . . ? O17 C47 C48 110.9(11) . . ? C58 C57 C56 118.8(6) . . ? C58 C59 C60 120.0(5) . . ? C57 C56 C55 122.0(5) . . ? C2 O2 C1 117.1(5) . . ? C17 O7 C16 113.2(5) . . ? C47 O17 C46 118.4(9) . . ? C32 O15 C31 113.8(6) . . ? C24 N5 C25 127.6(4) . . ? C24 N4 C21 129.0(4) . . ? C54 N10 C51 128.6(5) . . ? C39 N8 C40 127.8(4) . . ? C39 N9 C36 128.9(4) . . ? C9 N1 C6 127.8(4) . . ? C9 N2 C10 127.5(4) . . ? O9 N6 O10 121.8(6) . . ? O9 N6 C28 119.9(6) . . ? O10 N6 C28 117.9(6) . . ? O5 N3 O4 123.1(4) . . ? O5 N3 C13 118.3(4) . . ? O4 N3 C13 118.6(4) . . ? C54 N11 C55 127.6(4) . . ? O19 N12 O20 123.9(6) . . ? O19 N12 C58 118.2(6) . . ? O20 N12 C58 117.6(6) . . ? O12 N7 O11 123.9(8) . . ? O12 N7 C43 118.1(8) . . ? O11 N7 C43 117.6(7) . . ? C87 N16 C93 111.4(4) . . ? C87 N16 C96 111.3(4) . . ? C93 N16 C96 106.4(3) . . ? C87 N16 C90 106.5(3) . . ? C93 N16 C90 110.6(4) . . ? C96 N16 C90 110.8(4) . . ? C66 N13 C68 111.7(4) . . ? C66 N13 C63 110.7(4) . . ? C68 N13 C63 106.4(4) . . ? C66 N13 C61 106.6(4) . . ? C68 N13 C61 110.8(4) . . ? C63 N13 C61 110.6(4) . . ? C71 N14 C73 110.4(5) . . ? C71 N14 C72 106.9(5) . . ? C73 N14 C72 111.3(5) . . ? C71 N14 C75 112.2(5) . . ? C73 N14 C75 105.5(4) . . ? C72 N14 C75 110.6(5) . . ? C82 N15 C77 111.4(4) . . ? C82 N15 C86 107.0(4) . . ? C77 N15 C86 110.5(4) . . ? C82 N15 C85 110.9(4) . . ? C77 N15 C85 107.3(4) . . ? C86 N15 C85 109.8(4) . . ? C69 C68 N13 114.7(4) . . ? N13 C66 C67 117.7(5) . . ? C64 C63 N13 116.4(4) . . ? C70 C69 C68 112.0(5) . . ? C62 C61 N13 116.0(4) . . ? C61 C62 C123 111.6(6) . . ? C65 C64 C63 111.1(5) . . ? C69 C70 C114 114.2(6) . . ? C66 C67 C121 109.1(7) . . ? C115 C65 C64 114.5(6) . . ? C99 C72 N14 116.0(5) . . ? C76 C75 N14 116.4(5) . . ? N14 C71 C98 116.1(6) . . ? C73 C74 C118 106.3(5) . . ? C74 C73 N14 116.8(5) . . ? C75 C76 C103 108.2(6) . . ? C81 C82 N15 116.2(4) . . ? N15 C77 C78 114.7(4) . . ? C108 C86 N15 115.4(4) . . ? C80 C79 C78 113.8(5) . . ? C82 C81 C83 109.8(5) . . ? C111 C85 N15 114.8(5) . . ? C79 C78 C77 112.4(4) . . ? C84 C83 C81 112.7(5) . . ? C97 C96 N16 115.3(4) . . ? C91 C90 N16 115.7(4) . . ? N16 C93 C94 116.2(4) . . ? C95 C94 C93 110.6(4) . . ? N16 C87 C88 115.2(4) . . ? C94 C95 C101 113.7(5) . . ? C105 C97 C96 111.0(5) . . ? C90 C91 C125 116.9(7) . . ? C89 C88 C87 113.5(6) . . ? C107 C89 C88 115.2(9) . . ? F9 Si2 F8 87.4(3) . . ? F9 Si2 F12 178.6(3) . . ? F8 Si2 F12 94.0(3) . . ? F9 Si2 F11 93.7(2) . . ? F8 Si2 F11 89.7(2) . . ? F12 Si2 F11 86.3(2) . . ? F9 Si2 F7 93.9(3) . . ? F8 Si2 F7 177.8(3) . . ? F12 Si2 F7 84.8(3) . . ? F11 Si2 F7 92.0(2) . . ? F9 Si2 F10 86.6(2) . . ? F8 Si2 F10 91.12(18) . . ? F12 Si2 F10 93.42(19) . . ? F11 Si2 F10 179.1(2) . . ? F7 Si2 F10 87.13(18) . . ? C72 C99 C100 112.4(6) . . ? C102 C98 C71 112.5(8) . . ? C117 C100 C99 113.9(8) . . ? C104 C103 C76 110.3(8) . . ? C116 C102 C98 122.1(11) . . ? C106 C105 C97 113.1(7) . . ? C86 C108 C109 109.9(6) . . ? C110 C109 C108 90.9(13) . . ? C111 C112 C113 116.3(7) . . ? C112 C111 C85 114.7(6) . . ? C127 C118 C74 111.3(9) . . ? C128 C121 C67 89.2(11) . . ? C124 C123 C62 112.7(7) . . ? C126 C125 C91 95.9(11) . . ? _refine_diff_density_max 0.947 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.044 _shelx_res_file ; corrr.res created by SHELXL-2014/7 TITL corrr in P-1 CELL 0.71073 13.6859 17.7916 30.7988 93.988 96.865 109.357 ZERR 4.00 0.0006 0.0007 0.0014 0.004 0.004 0.004 LATT 1 SFAC C H N O F Si UNIT 248 392 32 40 24 4 OMIT -3 50.5 L.S. 10 ACTA BOND FMAP 2 PLAN 1 FREE C98 C116 FREE C128 C67 DFIX 1.47 0.02 C128 C121 DFIX 1.54 0.02 C121 C67 DFIX 1.54 0.02 C67 C121 DFIX 1.54 0.02 C121 C67 DFIX 1.54 0.02 C128 C121 DFIX 1.54 0.02 C128 C121 DFIX 1.44 0.02 C125 C91 WGHT 0.010000 10.359100 FVAR 0.15617 MOLE 2 C126 1 1.028261 -0.103977 0.401105 11.00000 0.31729 0.44563 = 0.16974 0.19453 -0.09878 -0.16076 AFIX 137 H203 2 0.982584 -0.127672 0.373898 11.00000 -1.50000 H202 2 1.023070 -0.144119 0.420839 11.00000 -1.50000 H201 2 1.099171 -0.082319 0.395494 11.00000 -1.50000 AFIX 0 MOLE 1 SI1 6 0.310189 0.270408 0.257036 11.00000 0.07412 0.06135 = 0.05022 0.01667 0.02169 0.02511 C10 1 0.789002 0.684435 0.397782 11.00000 0.07464 0.06061 = 0.05553 0.00911 0.01823 0.02298 C14 1 0.798502 0.623631 0.464654 11.00000 0.09401 0.07286 = 0.05208 0.01116 0.01928 0.02895 AFIX 43 H14 2 0.787057 0.620183 0.493728 11.00000 -1.20000 AFIX 0 C6 1 0.684668 0.907392 0.349219 11.00000 0.07164 0.07279 = 0.05137 0.00957 0.01413 0.02950 C3 1 0.633730 1.046265 0.344232 11.00000 0.06996 0.07614 = 0.06818 0.01613 0.01378 0.03400 C7 1 0.686619 0.954913 0.387380 11.00000 0.09483 0.07940 = 0.05465 0.01407 0.01131 0.04147 AFIX 43 H7 2 0.705530 0.940702 0.414800 11.00000 -1.20000 AFIX 0 C2 1 0.607217 1.120143 0.342842 11.00000 0.08535 0.09143 = 0.07887 0.02413 0.01913 0.04108 C4 1 0.632681 0.998781 0.306616 11.00000 0.07997 0.09603 = 0.06189 0.01818 0.00716 0.04235 AFIX 43 H4 2 0.614494 1.013366 0.279208 11.00000 -1.20000 AFIX 0 C13 1 0.842052 0.573578 0.444658 11.00000 0.06849 0.05495 = 0.05650 0.00609 0.00746 0.01773 C9 1 0.726255 0.798074 0.383793 11.00000 0.08671 0.06864 = 0.05788 0.01196 0.01549 0.03359 C15 1 0.772063 0.678849 0.441163 11.00000 0.09578 0.07052 = 0.05262 0.00682 0.02250 0.03890 AFIX 43 H15 2 0.742505 0.712822 0.454497 11.00000 -1.20000 AFIX 0 C8 1 0.660428 1.023267 0.384513 11.00000 0.09223 0.07905 = 0.06427 0.00762 0.01928 0.03767 AFIX 43 H8 2 0.660824 1.054246 0.410175 11.00000 -1.20000 AFIX 0 C5 1 0.657939 0.930501 0.308866 11.00000 0.09011 0.08879 = 0.05773 0.00727 0.01067 0.04407 AFIX 43 H5 2 0.657057 0.899622 0.283089 11.00000 -1.20000 AFIX 0 C12 1 0.860056 0.578197 0.402304 11.00000 0.09819 0.06849 = 0.06951 0.01015 0.02911 0.03892 AFIX 43 H12 2 0.890258 0.544235 0.389417 11.00000 -1.20000 AFIX 0 C11 1 0.833750 0.632831 0.378594 11.00000 0.11065 0.08039 = 0.05713 0.01594 0.03739 0.04666 AFIX 43 H103 2 0.845747 0.635588 0.349559 11.00000 -1.20000 AFIX 0 C1 1 0.573080 1.211716 0.295536 11.00000 0.14599 0.12382 = 0.13464 0.04357 0.01124 0.08629 AFIX 137 H1A 2 0.502916 1.203542 0.301032 11.00000 -1.50000 H1B 2 0.578779 1.223762 0.265843 11.00000 -1.50000 H1C 2 0.621279 1.255615 0.315624 11.00000 -1.50000 AFIX 0 C21 1 0.203862 0.423373 0.356693 11.00000 0.06704 0.06504 = 0.05343 0.00725 0.01166 0.02083 C24 1 0.249327 0.317471 0.394007 11.00000 0.07185 0.06344 = 0.04833 0.00429 0.00516 0.02201 C27 1 0.357799 0.085625 0.413392 11.00000 0.09629 0.07076 = 0.07179 0.01363 0.01591 0.03056 AFIX 43 H27 2 0.386929 0.050299 0.401162 11.00000 -1.20000 AFIX 0 C26 1 0.343795 0.145540 0.390522 11.00000 0.07671 0.07229 = 0.05673 0.01272 0.01971 0.02657 AFIX 43 H26 2 0.364036 0.151090 0.362813 11.00000 -1.20000 AFIX 0 C18 1 0.137964 0.554182 0.347520 11.00000 0.05782 0.06685 = 0.08665 0.00631 -0.00035 0.02338 C22 1 0.162624 0.452823 0.390459 11.00000 0.08741 0.05914 = 0.05806 0.00421 0.01156 0.02124 AFIX 43 H22 2 0.157104 0.428923 0.416394 11.00000 -1.20000 AFIX 0 C28 1 0.328717 0.077975 0.454340 11.00000 0.10907 0.06206 = 0.06356 0.01799 0.00850 0.02500 C30 1 0.271569 0.190051 0.450537 11.00000 0.08938 0.07003 = 0.04588 0.00861 0.01313 0.02885 AFIX 43 H30 2 0.243174 0.225517 0.463161 11.00000 -1.20000 AFIX 0 C23 1 0.130229 0.517035 0.385390 11.00000 0.08029 0.07088 = 0.06876 0.00159 0.01226 0.02392 AFIX 43 H23 2 0.102302 0.536093 0.408050 11.00000 -1.20000 AFIX 0 C19 1 0.175684 0.523059 0.312862 11.00000 0.09367 0.08617 = 0.07361 0.02560 0.01290 0.03688 AFIX 43 H19 2 0.178694 0.545864 0.286565 11.00000 -1.20000 AFIX 0 C25 1 0.299487 0.198096 0.408511 11.00000 0.05600 0.05635 = 0.04788 0.00549 0.00680 0.00908 C17 1 0.108504 0.625613 0.344896 11.00000 0.07070 0.08420 = 0.11208 0.02351 -0.00180 0.02663 C20 1 0.208253 0.458673 0.317848 11.00000 0.09312 0.08729 = 0.06428 0.01756 0.02403 0.04014 AFIX 43 H20 2 0.233739 0.438302 0.294782 11.00000 -1.20000 AFIX 0 C29 1 0.285963 0.129821 0.473295 11.00000 0.11267 0.07583 = 0.04658 0.01309 0.01499 0.02523 AFIX 43 H29 2 0.267027 0.124123 0.501216 11.00000 -1.20000 AFIX 0 C16 1 0.074516 0.721103 0.302823 11.00000 0.14974 0.12914 = 0.21577 0.07846 -0.02316 0.04518 AFIX 137 H16A 2 0.004169 0.706972 0.287774 11.00000 -1.50000 H16B 2 0.121751 0.758175 0.287166 11.00000 -1.50000 H16C 2 0.079131 0.745576 0.332127 11.00000 -1.50000 AFIX 0 C40 1 0.279418 0.332503 0.103511 11.00000 0.06255 0.07210 = 0.06052 0.00724 0.00897 0.00925 C39 1 0.337303 0.215792 0.115171 11.00000 0.07588 0.07616 = 0.05400 0.00242 0.00893 0.01892 C36 1 0.395275 0.111380 0.149045 11.00000 0.06494 0.07024 = 0.06124 0.00293 0.00896 0.00878 C32 1 0.501216 -0.087125 0.153145 11.00000 0.07977 0.10792 = 0.12655 0.01442 -0.00902 0.02894 C45 1 0.247854 0.389226 0.124897 11.00000 0.09864 0.09902 = 0.07422 0.01808 0.02700 0.04282 AFIX 43 H45 2 0.244515 0.389270 0.154881 11.00000 -1.20000 AFIX 0 C34 1 0.456992 0.015491 0.114145 11.00000 0.08618 0.08107 = 0.08733 -0.00112 0.01822 0.02392 AFIX 43 H34 2 0.473794 -0.006289 0.088953 11.00000 -1.20000 AFIX 0 C44 1 0.221378 0.445418 0.102743 11.00000 0.11553 0.09899 = 0.09274 0.02464 0.03051 0.04452 AFIX 43 H44 2 0.200511 0.483743 0.117308 11.00000 -1.20000 AFIX 0 C42 1 0.258263 0.389570 0.036376 11.00000 0.15242 0.08858 = 0.06065 0.00896 0.00560 0.02690 AFIX 43 H42 2 0.261775 0.390334 0.006432 11.00000 -1.20000 AFIX 0 C35 1 0.421489 0.078625 0.111580 11.00000 0.08660 0.07733 = 0.06770 0.00596 0.01386 0.02111 AFIX 43 H35 2 0.414863 0.099601 0.084999 11.00000 -1.20000 AFIX 0 C37 1 0.408302 0.080145 0.188524 11.00000 0.08663 0.10033 = 0.05805 0.01012 0.00547 0.03264 AFIX 43 H37 2 0.392343 0.102095 0.213878 11.00000 -1.20000 AFIX 0 C41 1 0.285362 0.333353 0.058877 11.00000 0.12358 0.08349 = 0.05859 0.00708 0.00971 0.02925 AFIX 43 H41 2 0.307617 0.296012 0.044158 11.00000 -1.20000 AFIX 0 C38 1 0.444641 0.016989 0.190316 11.00000 0.08173 0.10927 = 0.07637 0.01986 -0.00109 0.02564 AFIX 43 H38 2 0.453270 -0.003347 0.216964 11.00000 -1.20000 AFIX 0 C33 1 0.468570 -0.016764 0.153024 11.00000 0.06438 0.08397 = 0.10244 0.00617 -0.00130 0.01982 C43 1 0.226430 0.443737 0.058411 11.00000 0.12004 0.07956 = 0.08041 0.01849 0.00140 0.02469 C31 1 0.552617 -0.181446 0.192310 11.00000 0.16797 0.15888 = 0.23842 0.05231 -0.04202 0.06913 AFIX 137 H31A 2 0.518109 -0.216841 0.165886 11.00000 -1.50000 H31B 2 0.531874 -0.208208 0.217461 11.00000 -1.50000 H31C 2 0.627125 -0.166500 0.193532 11.00000 -1.50000 AFIX 0 MOLE 3 C51 1 0.083431 0.389016 0.857748 11.00000 0.07407 0.09689 = 0.07523 0.02298 0.02584 0.03337 C48 1 0.035408 0.529326 0.853733 11.00000 0.08135 0.11637 = 0.15957 0.06132 0.04999 0.04558 C52 1 0.097626 0.440061 0.895789 11.00000 0.09965 0.10025 = 0.09280 0.02528 0.02820 0.04463 AFIX 43 H52 2 0.123077 0.428022 0.922813 11.00000 -1.20000 AFIX 0 C54 1 0.139888 0.284735 0.891890 11.00000 0.07213 0.08045 = 0.06809 0.01769 0.02107 0.01836 C58 1 0.275778 0.066993 0.948295 11.00000 0.10355 0.07386 = 0.06497 0.01120 0.00760 0.01905 C60 1 0.217458 0.179297 0.949199 11.00000 0.13423 0.07603 = 0.05555 0.00300 0.01038 0.03452 AFIX 43 H60 2 0.200441 0.218688 0.964818 11.00000 -1.20000 AFIX 0 C49 1 0.020602 0.477549 0.816364 11.00000 0.08479 0.14805 = 0.13824 0.07972 0.03791 0.04454 AFIX 43 H49 2 -0.006228 0.489279 0.789504 11.00000 -1.20000 AFIX 0 C55 1 0.208969 0.174195 0.904091 11.00000 0.08193 0.07804 = 0.05399 0.01124 0.01602 0.01897 C50 1 0.044987 0.408286 0.818091 11.00000 0.08851 0.12469 = 0.08514 0.03836 0.02679 0.03797 AFIX 43 H50 2 0.035454 0.374387 0.792372 11.00000 -1.20000 AFIX 0 C53 1 0.073185 0.509728 0.892942 11.00000 0.10325 0.09977 = 0.13625 0.02004 0.03655 0.04526 AFIX 43 H53 2 0.082825 0.544069 0.918495 11.00000 -1.20000 AFIX 0 C47 1 0.016272 0.605652 0.853701 11.00000 0.09892 0.13390 = 0.27273 0.10333 0.06607 0.06537 C57 1 0.267201 0.060785 0.904175 11.00000 0.15662 0.11244 = 0.06944 0.02182 0.03073 0.06845 AFIX 43 H57 2 0.283352 0.020693 0.888783 11.00000 -1.20000 AFIX 0 C59 1 0.251969 0.124597 0.971351 11.00000 0.14970 0.09257 = 0.04665 0.00611 -0.00138 0.03156 AFIX 43 H59 2 0.258576 0.127753 1.001889 11.00000 -1.20000 AFIX 0 C56 1 0.234300 0.114456 0.882283 11.00000 0.15600 0.12181 = 0.05722 0.02350 0.03251 0.07240 AFIX 43 H56 2 0.228849 0.110537 0.851759 11.00000 -1.20000 AFIX 0 C46 1 -0.037381 0.692333 0.805661 11.00000 0.15563 0.18224 = 0.45474 0.18639 0.07681 0.09542 AFIX 137 H46A 2 -0.086258 0.700514 0.823756 11.00000 -1.50000 H46B 2 -0.064072 0.691251 0.775260 11.00000 -1.50000 H46C 2 0.028569 0.735300 0.813380 11.00000 -1.50000 AFIX 0 MOLE 1 O8 4 0.227808 0.331128 0.429904 11.00000 0.14903 0.10345 = 0.04935 0.01370 0.02986 0.06952 O13 4 0.350193 0.201201 0.077827 11.00000 0.14160 0.11809 = 0.04947 0.00502 0.02446 0.06219 MOLE 3 O18 4 0.134884 0.303869 0.929936 11.00000 0.12349 0.10221 = 0.05639 0.01295 0.02906 0.04260 MOLE 1 O2 4 0.597715 1.139362 0.301762 11.00000 0.12618 0.10227 = 0.09940 0.02798 0.00877 0.06243 O7 4 0.103019 0.648038 0.304985 11.00000 0.12991 0.09474 = 0.12348 0.02818 -0.00287 0.05945 O3 4 0.707052 0.811330 0.420320 11.00000 0.14890 0.09422 = 0.05505 0.01857 0.03924 0.06621 O1 4 0.598871 1.159910 0.374519 11.00000 0.15216 0.11753 = 0.10678 0.02760 0.04304 0.08705 MOLE 3 O17 4 -0.022597 0.615377 0.812714 11.00000 0.13764 0.16402 = 0.28911 0.12659 0.05904 0.08253 MOLE 1 O6 4 0.090375 0.662392 0.375774 11.00000 0.12617 0.10035 = 0.13034 0.01931 0.02230 0.06412 MOLE 3 O20 4 0.331667 -0.042264 0.950899 11.00000 0.22323 0.13536 = 0.12648 0.04320 0.03905 0.10145 MOLE 1 O9 4 0.307910 0.001490 0.511811 11.00000 0.40742 0.13626 = 0.07747 0.05278 0.07496 0.13918 O4 4 0.845541 0.507224 0.506330 11.00000 0.14697 0.08523 = 0.06788 0.02296 0.02620 0.04733 O10 4 0.377450 -0.031756 0.461405 11.00000 0.40128 0.17188 = 0.15735 0.09111 0.11292 0.19692 MOLE 3 O19 4 0.312038 0.012969 1.011319 11.00000 0.29832 0.10779 = 0.07664 0.01452 -0.01902 0.07307 MOLE 1 O14 4 0.505338 -0.125774 0.119968 11.00000 0.14850 0.13202 = 0.16024 0.00593 0.00654 0.07921 O5 4 0.905197 0.469169 0.450750 11.00000 0.13980 0.09606 = 0.10179 0.02396 0.03550 0.07032 O12 4 0.215132 0.508981 -0.003525 11.00000 0.39940 0.14503 = 0.09818 0.03461 0.00274 0.11534 O15 4 0.522053 -0.106514 0.192389 11.00000 0.14825 0.12330 = 0.14703 0.01116 -0.03774 0.06636 MOLE 3 O16 4 0.034325 0.655107 0.883749 11.00000 0.17541 0.12767 = 0.34060 0.05958 0.07270 0.08545 MOLE 1 O11 4 0.162785 0.549169 0.053698 11.00000 0.31444 0.16444 = 0.17828 0.07637 0.07890 0.14146 N5 3 0.285226 0.255515 0.382590 11.00000 0.06798 0.06973 = 0.04760 0.00926 0.01423 0.02655 AFIX 43 H5B 2 0.300421 0.252321 0.356382 11.00000 -1.20000 AFIX 0 N4 3 0.240951 0.359796 0.359409 11.00000 0.09657 0.07711 = 0.05233 0.01091 0.02491 0.04272 AFIX 43 H4B 2 0.261504 0.345086 0.335975 11.00000 -1.20000 AFIX 0 MOLE 3 N10 3 0.109436 0.320204 0.857015 11.00000 0.09800 0.09883 = 0.06049 0.01408 0.01899 0.04571 AFIX 43 H10 2 0.106099 0.296461 0.831305 11.00000 -1.20000 AFIX 0 MOLE 1 N8 3 0.304482 0.277165 0.128834 11.00000 0.08471 0.08604 = 0.05042 0.00576 0.01321 0.03051 AFIX 43 H8A 2 0.298554 0.282332 0.156270 11.00000 -1.20000 AFIX 0 N9 3 0.355810 0.174347 0.149187 11.00000 0.09769 0.08742 = 0.04815 0.00305 0.01920 0.03297 AFIX 43 H9 2 0.341112 0.189125 0.174045 11.00000 -1.20000 AFIX 0 N1 3 0.712012 0.838956 0.348965 11.00000 0.10941 0.07673 = 0.05461 0.01104 0.01866 0.05087 AFIX 43 H1 2 0.721093 0.819964 0.323910 11.00000 -1.20000 AFIX 0 N2 3 0.763703 0.737694 0.371418 11.00000 0.10790 0.07998 = 0.05428 0.01495 0.02424 0.04859 AFIX 43 H2 2 0.772314 0.732523 0.344307 11.00000 -1.20000 AFIX 0 N6 3 0.341505 0.012746 0.478471 11.00000 0.22595 0.08787 = 0.07191 0.01960 0.02641 0.07082 N3 3 0.867071 0.513140 0.469097 11.00000 0.08767 0.06735 = 0.07023 0.01017 0.01114 0.02499 MOLE 3 N11 3 0.174599 0.224322 0.878213 11.00000 0.10495 0.09445 = 0.04926 0.01696 0.02138 0.04347 AFIX 43 H11A 2 0.175205 0.216484 0.850391 11.00000 -1.20000 AFIX 0 N12 3 0.312018 0.009733 0.972525 11.00000 0.15374 0.08727 = 0.08135 0.01426 0.00354 0.03887 MOLE 1 N7 3 0.196397 0.503677 0.033710 11.00000 0.23450 0.10427 = 0.11129 0.02725 0.01069 0.06764 N16 3 1.001946 0.064966 0.309746 11.00000 0.07377 0.06308 = 0.07484 0.00683 0.01625 0.00096 MOLE 2 N13 3 0.385512 0.530717 0.804427 11.00000 0.06990 0.07224 = 0.10189 0.01316 0.02391 -0.00211 MOLE 4 N14 3 0.816904 0.204344 0.943055 11.00000 0.07765 0.08769 = 0.11556 0.01603 0.03302 0.01409 MOLE 5 N15 3 0.642541 0.287679 0.518599 11.00000 0.07053 0.06903 = 0.08912 0.00217 0.00510 0.01326 MOLE 2 C68 1 0.476532 0.525278 0.782141 11.00000 0.08269 0.07744 = 0.13482 0.01829 0.03895 0.00889 AFIX 23 H68A 2 0.487883 0.562342 0.760066 11.00000 -1.20000 H68B 2 0.539261 0.542456 0.803939 11.00000 -1.20000 AFIX 0 C66 1 0.364475 0.475614 0.840300 11.00000 0.09730 0.08529 = 0.11253 0.02469 0.02680 -0.00446 AFIX 23 H66A 2 0.343291 0.420809 0.826502 11.00000 -1.20000 H66B 2 0.305305 0.481188 0.852957 11.00000 -1.20000 AFIX 0 C63 1 0.415270 0.618075 0.823644 11.00000 0.08432 0.07275 = 0.11153 0.00160 0.01833 -0.00956 AFIX 23 H63A 2 0.477369 0.631139 0.845527 11.00000 -1.20000 H63B 2 0.433970 0.651545 0.800272 11.00000 -1.20000 AFIX 0 C69 1 0.461645 0.442702 0.760373 11.00000 0.11558 0.08658 = 0.18769 0.01503 0.06690 0.02093 AFIX 23 H69A 2 0.450781 0.405250 0.782252 11.00000 -1.20000 H69B 2 0.399497 0.425242 0.738254 11.00000 -1.20000 AFIX 0 C61 1 0.284825 0.505308 0.771408 11.00000 0.07746 0.08240 = 0.09450 -0.00633 0.01545 0.00252 AFIX 23 H61A 2 0.265481 0.448580 0.761637 11.00000 -1.20000 H61B 2 0.229542 0.512075 0.786537 11.00000 -1.20000 AFIX 0 C62 1 0.289076 0.549947 0.731054 11.00000 0.12423 0.13629 = 0.10010 0.02079 0.02896 0.03150 AFIX 23 H62A 2 0.326781 0.530469 0.710801 11.00000 -1.20000 H62B 2 0.327069 0.606616 0.739828 11.00000 -1.20000 AFIX 0 C64 1 0.332651 0.640203 0.844788 11.00000 0.09214 0.11042 = 0.12517 -0.02219 0.03092 0.00372 AFIX 23 H64A 2 0.268388 0.624500 0.823943 11.00000 -1.20000 H64B 2 0.318011 0.611232 0.870149 11.00000 -1.20000 AFIX 0 C70 1 0.553885 0.441449 0.739187 11.00000 0.14381 0.09530 = 0.23879 0.01389 0.10206 0.03300 AFIX 23 H70A 2 0.615157 0.457005 0.761698 11.00000 -1.20000 H70B 2 0.566556 0.481125 0.718528 11.00000 -1.20000 AFIX 0 C67 1 0.454053 0.487817 0.878140 11.00000 0.12096 0.17018 = 0.14769 0.05171 -0.01166 0.00221 AFIX 23 H67A 2 0.454457 0.528825 0.900697 11.00000 -1.20000 H67B 2 0.520731 0.505316 0.867272 11.00000 -1.20000 AFIX 0 C65 1 0.368499 0.729135 0.859086 11.00000 0.10326 0.10414 = 0.15698 -0.03511 0.02977 0.01158 AFIX 23 H65A 2 0.431020 0.743665 0.880864 11.00000 -1.20000 H65B 2 0.387508 0.757492 0.833874 11.00000 -1.20000 AFIX 0 MOLE 4 C72 1 0.907858 0.232155 0.981049 11.00000 0.07394 0.10583 = 0.12470 -0.01180 0.01853 0.00853 AFIX 23 H72A 2 0.972531 0.241427 0.968923 11.00000 -1.20000 H72B 2 0.910152 0.283182 0.995329 11.00000 -1.20000 AFIX 0 C75 1 0.713052 0.191276 0.960125 11.00000 0.07825 0.11126 = 0.12713 0.04067 0.04035 0.02325 AFIX 23 H75A 2 0.657056 0.171282 0.935273 11.00000 -1.20000 H75B 2 0.703480 0.149674 0.979596 11.00000 -1.20000 AFIX 0 C71 1 0.838176 0.267102 0.912193 11.00000 0.11026 0.11266 = 0.15214 0.04893 0.06803 0.02684 AFIX 23 H71A 2 0.904927 0.272665 0.902577 11.00000 -1.20000 H71B 2 0.845364 0.317862 0.928393 11.00000 -1.20000 AFIX 0 C74 1 0.901069 0.118481 0.900165 11.00000 0.09272 0.12869 = 0.12959 -0.00970 0.01923 0.02953 AFIX 23 H74A 2 0.962556 0.135556 0.922620 11.00000 -1.20000 H74B 2 0.914884 0.152505 0.876726 11.00000 -1.20000 AFIX 0 C73 1 0.807117 0.123429 0.919420 11.00000 0.07727 0.09292 = 0.11660 0.00592 0.01507 0.01157 AFIX 23 H73A 2 0.790499 0.083896 0.940052 11.00000 -1.20000 H73B 2 0.748137 0.108310 0.895818 11.00000 -1.20000 AFIX 0 C76 1 0.701069 0.263025 0.984284 11.00000 0.14323 0.12628 = 0.17912 0.04168 0.08728 0.05283 AFIX 23 H76A 2 0.712349 0.306325 0.965892 11.00000 -1.20000 H76B 2 0.752205 0.281457 1.010861 11.00000 -1.20000 AFIX 0 MOLE 5 C82 1 0.758184 0.300358 0.520374 11.00000 0.06091 0.07964 = 0.08952 0.01187 0.00186 0.01274 AFIX 23 H82A 2 0.790166 0.348475 0.506906 11.00000 -1.20000 H82B 2 0.790034 0.310071 0.551041 11.00000 -1.20000 AFIX 0 C77 1 0.587476 0.274116 0.471450 11.00000 0.06793 0.07916 = 0.09312 -0.00385 -0.01127 0.01216 AFIX 23 H77A 2 0.514321 0.267387 0.471888 11.00000 -1.20000 H77B 2 0.590214 0.224536 0.457338 11.00000 -1.20000 AFIX 0 C86 1 0.634829 0.362419 0.542924 11.00000 0.07415 0.08293 = 0.10111 -0.00742 0.01128 0.01443 AFIX 23 H86A 2 0.665946 0.367065 0.573426 11.00000 -1.20000 H86B 2 0.676167 0.408901 0.530345 11.00000 -1.20000 AFIX 0 C79 1 0.558380 0.338669 0.403246 11.00000 0.08032 0.09691 = 0.10535 0.00498 -0.00962 0.02158 AFIX 23 H79A 2 0.536930 0.286011 0.386628 11.00000 -1.20000 H79B 2 0.496288 0.346048 0.412224 11.00000 -1.20000 AFIX 0 C81 1 0.784744 0.232553 0.498217 11.00000 0.09135 0.08710 = 0.10197 0.01432 0.01764 0.02952 AFIX 23 H81A 2 0.753446 0.221642 0.467458 11.00000 -1.20000 H81B 2 0.756452 0.184341 0.512159 11.00000 -1.20000 AFIX 0 C80 1 0.603219 0.400691 0.373910 11.00000 0.12490 0.11897 = 0.11488 0.03484 -0.00679 0.02134 AFIX 137 H80A 2 0.619401 0.453161 0.389305 11.00000 -1.50000 H80B 2 0.553088 0.393813 0.348018 11.00000 -1.50000 H80C 2 0.665976 0.394945 0.365561 11.00000 -1.50000 AFIX 0 C85 1 0.588268 0.214339 0.540680 11.00000 0.08411 0.08621 = 0.11467 0.01813 0.01569 0.01091 AFIX 23 H85A 2 0.515833 0.210265 0.540747 11.00000 -1.20000 H85B 2 0.588243 0.166872 0.523155 11.00000 -1.20000 AFIX 0 C78 1 0.633201 0.341262 0.443736 11.00000 0.08090 0.08696 = 0.09169 0.00823 0.00118 0.01724 AFIX 23 H78A 2 0.651205 0.392539 0.461473 11.00000 -1.20000 H78B 2 0.697100 0.337007 0.434970 11.00000 -1.20000 AFIX 0 C83 1 0.903164 0.255267 0.501787 11.00000 0.09611 0.12576 = 0.13036 0.01195 0.01186 0.05218 AFIX 23 H83A 2 0.930488 0.302785 0.487168 11.00000 -1.20000 H83B 2 0.933975 0.268351 0.532595 11.00000 -1.20000 AFIX 0 C84 1 0.935467 0.188851 0.481561 11.00000 0.13943 0.17062 = 0.18036 0.03053 0.02586 0.09529 AFIX 137 H84A 2 0.918886 0.144773 0.498918 11.00000 -1.50000 H84B 2 1.009506 0.208540 0.480796 11.00000 -1.50000 H84C 2 0.898501 0.171102 0.452137 11.00000 -1.50000 AFIX 0 MOLE 1 C96 1 1.105117 0.062667 0.297101 11.00000 0.08663 0.06940 = 0.09887 0.01321 0.02659 0.01300 AFIX 23 H96A 2 1.126896 0.101048 0.276216 11.00000 -1.20000 H96B 2 1.157827 0.080000 0.323197 11.00000 -1.20000 AFIX 0 C90 1 0.963665 0.005582 0.342459 11.00000 0.08694 0.06992 = 0.07993 0.01552 0.01568 -0.00265 AFIX 23 H90A 2 0.896078 0.006604 0.348419 11.00000 -1.20000 H90B 2 0.953052 -0.047830 0.328728 11.00000 -1.20000 AFIX 0 C93 1 1.022969 0.149891 0.330056 11.00000 0.08226 0.06293 = 0.07868 -0.00105 0.01407 0.00020 AFIX 23 H93A 2 1.054368 0.186367 0.309568 11.00000 -1.20000 H93B 2 1.074172 0.160818 0.356443 11.00000 -1.20000 AFIX 0 C94 1 0.928763 0.168738 0.342149 11.00000 0.07406 0.09116 = 0.08735 -0.00478 0.01823 0.00667 AFIX 23 H94A 2 0.876345 0.157867 0.316185 11.00000 -1.20000 H94B 2 0.898126 0.134528 0.363712 11.00000 -1.20000 AFIX 0 C87 1 0.917222 0.041472 0.270278 11.00000 0.09485 0.07529 = 0.07214 -0.00436 0.00315 0.01022 AFIX 23 H87A 2 0.852459 0.041721 0.279992 11.00000 -1.20000 H87B 2 0.906561 -0.013054 0.258364 11.00000 -1.20000 AFIX 0 C95 1 0.960286 0.255458 0.360817 11.00000 0.09396 0.08858 = 0.13634 -0.00707 0.02128 0.02002 AFIX 23 H95A 2 0.993031 0.289052 0.339404 11.00000 -1.20000 H95B 2 1.012050 0.265477 0.386937 11.00000 -1.20000 AFIX 0 C97 1 1.102608 -0.018144 0.277197 11.00000 0.13394 0.08295 = 0.12671 0.01414 0.05138 0.02874 AFIX 23 H97A 2 1.082093 -0.057043 0.297926 11.00000 -1.20000 H97B 2 1.050895 -0.035970 0.250785 11.00000 -1.20000 AFIX 0 C91 1 1.035788 0.020111 0.386200 11.00000 0.12419 0.11085 = 0.09944 0.03552 -0.00054 0.00375 AFIX 23 H91A 2 1.047257 0.073946 0.399533 11.00000 -1.20000 H91B 2 1.103011 0.018481 0.380094 11.00000 -1.20000 AFIX 0 C88 1 0.938764 0.094727 0.233642 11.00000 0.14301 0.11754 = 0.07712 0.01400 0.01763 0.03737 AFIX 23 H88A 2 0.958717 0.150236 0.246116 11.00000 -1.20000 H88B 2 0.997530 0.088628 0.220870 11.00000 -1.20000 AFIX 0 C89 1 0.847397 0.076443 0.198045 11.00000 0.22893 0.14123 = 0.09688 0.01082 -0.04339 0.00113 AFIX 23 H89A 2 0.871876 0.102061 0.172685 11.00000 -1.20000 H89B 2 0.819998 0.019000 0.189328 11.00000 -1.20000 AFIX 0 MOLE 2 SI2 6 0.183989 0.232570 0.752323 11.00000 0.07691 0.05337 = 0.04951 0.00560 0.00682 0.02235 MOLE 1 F3 5 0.196165 0.264563 0.273800 11.00000 0.07069 0.09574 = 0.07390 0.00914 0.02566 0.02383 F5 5 0.423008 0.275637 0.239790 11.00000 0.08368 0.10112 = 0.08539 0.03445 0.04079 0.04529 F1 5 0.289517 0.324779 0.216739 11.00000 0.11037 0.10600 = 0.07147 0.04204 0.02614 0.05458 F4 5 0.249897 0.186371 0.222785 11.00000 0.12859 0.08107 = 0.08643 -0.01410 0.04917 0.00560 F6 5 0.331407 0.217515 0.297867 11.00000 0.12671 0.11460 = 0.08047 0.05595 0.04587 0.06793 F2 5 0.369175 0.354507 0.291312 11.00000 0.09059 0.08848 = 0.07585 -0.00790 0.02188 0.01184 MOLE 2 F8 5 0.082909 0.241813 0.770664 11.00000 0.11602 0.34966 = 0.08313 -0.02759 0.00941 0.11210 F7 5 0.290216 0.226657 0.734354 11.00000 0.15405 0.31480 = 0.08449 -0.03702 0.00789 0.14519 F10 5 0.261744 0.286157 0.797197 11.00000 0.09686 0.13933 = 0.06563 -0.01640 0.00561 -0.00321 F12 5 0.202427 0.309733 0.725002 11.00000 0.19095 0.09829 = 0.16956 0.06818 -0.03149 0.00136 F9 5 0.168130 0.155839 0.778911 11.00000 0.25084 0.09132 = 0.21248 0.07759 -0.08578 -0.01621 F11 5 0.108446 0.179657 0.707471 11.00000 0.14754 0.12477 = 0.07282 -0.01809 -0.01521 -0.00585 MOLE 4 C99 1 0.904567 0.175920 1.015481 11.00000 0.10559 0.14580 = 0.13209 0.01583 -0.00822 0.01655 AFIX 23 H99A 2 0.892054 0.122566 1.001161 11.00000 -1.20000 H99B 2 0.846627 0.173298 1.031344 11.00000 -1.20000 AFIX 0 C98 1 0.756362 0.252110 0.871606 11.00000 0.13397 0.19377 = 0.17119 0.09912 0.04786 0.05335 AFIX 23 H98A 2 0.744925 0.199803 0.856161 11.00000 -1.20000 H98B 2 0.690689 0.251472 0.880726 11.00000 -1.20000 AFIX 0 C100 1 1.004837 0.201730 1.047800 11.00000 0.12384 0.20866 = 0.14668 0.00153 -0.02770 -0.00268 AFIX 23 H10A 2 1.062329 0.203446 1.031823 11.00000 -1.20000 H10B 2 1.017936 0.255650 1.061442 11.00000 -1.20000 AFIX 0 MOLE 1 C101 1 0.869747 0.279446 0.372749 11.00000 0.12454 0.14098 = 0.14359 -0.00544 0.02647 0.05704 AFIX 137 H10C 2 0.821620 0.275157 0.346554 11.00000 -1.50000 H10D 2 0.895794 0.333814 0.386560 11.00000 -1.50000 H10E 2 0.834392 0.244585 0.392701 11.00000 -1.50000 AFIX 0 MOLE 4 C103 1 0.587830 0.238123 0.996238 11.00000 0.15357 0.21195 = 0.19260 0.02931 0.09035 0.09903 AFIX 23 H10F 2 0.537254 0.214588 0.969853 11.00000 -1.20000 H10G 2 0.579148 0.198146 1.016689 11.00000 -1.20000 AFIX 0 C102 1 0.787535 0.313491 0.841277 11.00000 0.17272 0.32681 = 0.24675 0.19398 0.05033 0.01460 AFIX 23 H10H 2 0.796319 0.364581 0.857521 11.00000 -1.20000 H10I 2 0.856346 0.316025 0.835104 11.00000 -1.20000 AFIX 0 C104 1 0.568644 0.308430 1.016262 11.00000 0.26799 0.34713 = 0.30771 0.15869 0.17682 0.18477 AFIX 137 H10J 2 0.627934 0.339219 1.037706 11.00000 -1.50000 H10K 2 0.507316 0.290950 1.030331 11.00000 -1.50000 H10L 2 0.558157 0.341012 0.993819 11.00000 -1.50000 AFIX 0 MOLE 1 C106 1 1.209512 -0.089626 0.245695 11.00000 0.23796 0.17477 = 0.27275 0.08963 0.13610 0.11375 AFIX 137 H10M 2 1.185503 -0.130325 0.264688 11.00000 -1.50000 H10N 2 1.279579 -0.084350 0.241188 11.00000 -1.50000 H10O 2 1.164158 -0.104391 0.217882 11.00000 -1.50000 AFIX 0 C105 1 1.208446 -0.013725 0.265853 11.00000 0.20584 0.08791 = 0.22873 0.02556 0.13525 0.05991 AFIX 23 H10P 2 1.229373 0.026433 0.245824 11.00000 -1.20000 H10Q 2 1.259511 0.003367 0.292481 11.00000 -1.20000 AFIX 0 C107 1 0.764682 0.101130 0.209303 11.00000 0.11648 0.53966 = 0.25615 0.18162 0.00775 0.06648 AFIX 137 H10R 2 0.717103 0.059315 0.222339 11.00000 -1.50000 H10S 2 0.728088 0.112052 0.183270 11.00000 -1.50000 H10T 2 0.792662 0.148796 0.229947 11.00000 -1.50000 AFIX 0 MOLE 5 C110 1 0.529331 0.436641 0.601939 11.00000 0.15193 0.14271 = 0.47120 -0.04467 0.02434 0.03940 AFIX 137 H11B 2 0.466118 0.392932 0.603253 11.00000 -1.50000 H11C 2 0.532432 0.482177 0.621418 11.00000 -1.50000 H102 2 0.588806 0.420971 0.610712 11.00000 -1.50000 AFIX 0 C108 1 0.525166 0.364697 0.541861 11.00000 0.09459 0.14883 = 0.20335 -0.06440 0.02493 0.03660 AFIX 23 H10U 2 0.487288 0.326195 0.560092 11.00000 -1.20000 H10V 2 0.488110 0.350151 0.511952 11.00000 -1.20000 AFIX 0 C109 1 0.530230 0.456145 0.560275 11.00000 0.15003 0.35482 = 0.18369 -0.13748 -0.00758 0.11496 AFIX 23 H10W 2 0.594186 0.498040 0.556396 11.00000 -1.20000 H200 2 0.469189 0.468802 0.548669 11.00000 -1.20000 AFIX 0 C113 1 0.619141 0.158273 0.658347 11.00000 0.13833 0.31408 = 0.16865 0.14167 0.02812 0.01568 AFIX 137 H11E 2 0.647031 0.211828 0.673304 11.00000 -1.50000 H11F 2 0.674243 0.136140 0.658106 11.00000 -1.50000 H11G 2 0.565700 0.125688 0.673353 11.00000 -1.50000 AFIX 0 C112 1 0.573043 0.160086 0.611984 11.00000 0.12522 0.26047 = 0.16693 0.09563 0.05529 0.03913 AFIX 23 H11H 2 0.553333 0.106708 0.596398 11.00000 -1.20000 H11I 2 0.509341 0.172482 0.612748 11.00000 -1.20000 AFIX 0 C111 1 0.637470 0.214728 0.587563 11.00000 0.10489 0.15276 = 0.11770 0.04874 0.02113 0.01785 AFIX 23 H11J 2 0.701390 0.202675 0.586727 11.00000 -1.20000 H11K 2 0.656696 0.268330 0.602803 11.00000 -1.20000 AFIX 0 MOLE 2 C114 1 0.541257 0.361378 0.715213 11.00000 0.18247 0.13689 = 0.27408 0.02865 0.12284 0.05750 AFIX 137 H11L 2 0.519105 0.320345 0.734193 11.00000 -1.50000 H11M 2 0.606992 0.362586 0.706758 11.00000 -1.50000 H11N 2 0.489619 0.350122 0.689393 11.00000 -1.50000 AFIX 0 C115 1 0.289046 0.756779 0.878096 11.00000 0.14820 0.16643 = 0.22815 -0.04208 0.01922 0.05002 AFIX 137 H11O 2 0.230077 0.748579 0.855746 11.00000 -1.50000 H11P 2 0.319752 0.812779 0.888800 11.00000 -1.50000 H11Q 2 0.266274 0.726736 0.901951 11.00000 -1.50000 AFIX 0 MOLE 4 C116 1 0.730311 0.309332 0.803317 11.00000 0.18535 0.50898 = 0.28217 0.25995 0.02411 0.04589 AFIX 137 H11R 2 0.684155 0.255082 0.794645 11.00000 -1.50000 H101 2 0.775117 0.326046 0.781495 11.00000 -1.50000 H11T 2 0.689728 0.343819 0.805995 11.00000 -1.50000 AFIX 0 C117 1 1.003704 0.150175 1.081762 11.00000 0.24078 0.34916 = 0.26148 0.13875 -0.12056 -0.01407 AFIX 137 H11U 2 0.935414 0.132255 1.090480 11.00000 -1.50000 H11V 2 1.054775 0.179166 1.106688 11.00000 -1.50000 H11W 2 1.020164 0.104650 1.070813 11.00000 -1.50000 AFIX 0 C118 1 0.873805 0.028405 0.881743 11.00000 0.13812 0.19193 = 0.27139 -0.11068 0.09832 0.00317 AFIX 23 H105 2 0.869363 -0.003837 0.906054 11.00000 -1.20000 H104 2 0.805988 0.009720 0.863183 11.00000 -1.20000 AFIX 0 MOLE 2 C121 1 0.437211 0.401583 0.899333 11.00000 0.27372 0.48129 = 0.16265 0.19329 -0.05601 -0.12971 AFIX 23 H12A 2 0.368703 0.361303 0.889497 11.00000 -1.20000 H12B 2 0.492429 0.379764 0.895894 11.00000 -1.20000 AFIX 0 C123 1 0.179101 0.538892 0.707624 11.00000 0.15787 0.16425 = 0.10566 -0.02226 -0.00217 0.05498 AFIX 23 H12C 2 0.182085 0.544910 0.676699 11.00000 -1.20000 H12D 2 0.132889 0.484911 0.709611 11.00000 -1.20000 AFIX 0 C124 1 0.135779 0.595988 0.726188 11.00000 0.15039 0.19670 = 0.20199 0.04955 0.01914 0.04987 AFIX 137 H12E 2 0.113119 0.580331 0.753546 11.00000 -1.50000 H12F 2 0.077150 0.596928 0.706005 11.00000 -1.50000 H12G 2 0.188435 0.648439 0.731281 11.00000 -1.50000 AFIX 0 C125 1 0.997679 -0.039613 0.421068 11.00000 0.24394 0.12896 = 0.36816 0.07265 0.06898 -0.00800 AFIX 23 H12H 2 1.035209 -0.018690 0.450536 11.00000 -1.20000 H12I 2 0.922757 -0.055551 0.421273 11.00000 -1.20000 AFIX 0 C127 1 0.945426 0.018999 0.858640 11.00000 0.23111 0.21069 = 0.21312 -0.03587 -0.00108 0.02217 AFIX 137 H12M 2 0.961129 0.059189 0.838789 11.00000 -1.50000 H12N 2 0.919115 -0.033267 0.842123 11.00000 -1.50000 H12O 2 1.007949 0.024258 0.878261 11.00000 -1.50000 AFIX 0 C128 1 0.446802 0.440294 0.939698 11.00000 0.48304 0.30304 = 0.39474 0.15309 0.25482 0.04336 AFIX 137 H12P 2 0.506620 0.488752 0.943853 11.00000 -1.50000 H12Q 2 0.455762 0.406440 0.961670 11.00000 -1.50000 H12R 2 0.384849 0.453244 0.942302 11.00000 -1.50000 AFIX 0 HKLF 4 REM corrr in P-1 REM R1 = 0.0935 for 12117 Fo > 4sig(Fo) and 0.1709 for all 25235 data REM 1587 parameters refined using 7 restraints END WGHT 0.0991 7.5641 REM Highest difference peak 0.947, deepest hole -0.489, 1-sigma level 0.044 Q1 1 0.2156 0.1581 0.7372 11.00000 0.05 0.95 ; _shelx_res_checksum 10797 _shelx_hkl_file ; 0 0 5 92.42 2.31 0 0 6 34.85 1.58 0 0 -6 33.22 1.52 0 0 -7 13.25 1.06 0 0 7 14.24 1.13 0 0 -7 15.25 0.65 0 0 -8 466.67 6.63 0 0 -8 464.15 3.75 0 0 8 482.94 6.72 0 0 9 39.17 2.08 0 0 -9 34.28 1.08 0 0 -9 33.61 1.87 0 0 -10 93.83 2.69 0 0 -10 91.58 1.84 0 0 -10 88.09 3.21 0 0 10 88.74 3.27 0 0 11 8.67 1.21 0 0 -11 4.97 0.89 0 0 -11 5.31 0.69 0 0 -11 6.53 0.54 0 0 -12 495.64 6.87 0 0 -12 516.39 4.74 0 0 12 500.84 8.57 0 0 13 21.32 1.96 0 0 -13 14.46 1.27 0 0 -13 15.24 0.87 0 0 14 13.20 1.54 0 0 -14 14.19 0.85 0 0 -14 11.45 1.16 0 0 -15 6.34 0.59 0 0 -15 5.02 0.80 0 0 15 6.03 1.12 0 0 -16 1.60 0.34 0 0 16 1.74 0.71 0 0 17 7.64 1.33 0 0 -17 7.16 0.65 0 0 18 2.33 0.76 0 0 19 1.22 0.62 0 0 20 55.21 3.79 0 0 21 2.45 1.01 0 0 22 23.55 2.62 0 0 23 5.72 1.41 0 0 24 6.34 1.60 0 0 25 14.48 2.30 0 0 26 19.28 2.65 0 0 27 4.85 1.54 0 0 28 6.13 1.66 0 0 29 3.87 1.46 0 0 30 10.62 2.17 0 0 31 2.25 0.99 0 0 32 0.46 0.52 0 0 33 2.31 1.11 0 0 34 2.11 1.05 0 0 35 2.59 1.15 0 0 36 3.42 1.43 0 0 37 3.14 1.45 0 0 38 2.30 1.13 0 -1 38 0.32 0.54 0 -1 37 -0.62 0.78 0 -1 36 0.15 0.33 0 -1 35 -0.49 0.55 0 -1 34 -0.97 0.86 0 -1 33 0.35 0.62 0 -1 32 0.18 0.29 0 -1 31 0.21 0.52 0 -1 30 14.29 2.51 0 -1 29 0.19 0.40 0 -1 28 -0.42 0.47 0 -1 27 -0.63 0.57 0 -1 26 2.39 0.97 0 -1 25 5.31 1.38 0 -1 24 2.64 0.93 0 -1 23 2.37 0.91 0 -1 22 27.53 2.83 0 -1 21 0.21 0.40 0 -1 20 1.77 0.68 0 -1 19 1.07 0.52 0 -1 18 14.42 1.78 0 -1 17 2.65 0.79 0 -1 16 31.52 2.48 0 -1 15 9.55 1.34 0 -1 14 0.63 0.48 0 -1 13 55.22 3.00 0 -1 12 2.88 0.71 0 1 -11 46.21 2.47 0 -1 11 44.03 1.15 0 -1 11 47.98 2.55 0 -1 10 38.23 2.18 0 -1 10 33.31 0.95 0 1 -10 35.74 2.09 0 1 -9 11.39 1.11 0 -1 9 9.66 1.03 0 -1 8 29.32 1.67 0 1 -8 31.23 1.74 0 1 -7 20.33 1.32 0 -1 7 19.67 1.30 0 1 -6 4.00 0.54 0 -1 6 4.09 0.54 0 1 -5 305.83 4.38 0 -1 5 292.82 4.23 0 1 4 0.64 0.18 0 1 5 35.34 1.18 0 1 6 49.47 1.52 0 -1 -6 48.89 1.48 0 1 7 11.11 0.78 0 1 7 11.20 0.97 0 -1 -7 11.97 0.82 0 1 8 6.07 0.76 0 -1 -8 5.78 0.54 0 1 8 5.61 0.60 0 -1 -8 6.54 0.63 0 -1 -9 0.56 0.18 0 1 9 0.32 0.16 0 -1 -9 0.76 0.24 0 1 10 37.07 2.12 0 -1 -10 34.39 1.60 0 -1 -10 33.28 1.40 0 1 11 37.30 2.26 0 -1 -11 41.76 1.58 0 -1 -11 41.01 1.83 0 -1 -12 31.71 1.68 0 -1 -12 31.69 1.42 0 1 12 30.45 2.13 0 -1 -13 0.14 0.17 0 -1 -13 0.02 0.06 0 1 14 24.19 2.05 0 -1 -14 22.82 1.26 0 -1 -14 22.91 1.56 0 -1 -15 2.18 0.43 0 -1 -15 1.75 0.44 0 1 15 1.63 0.58 0 -1 -16 14.13 1.04 0 1 16 14.11 1.72 0 -1 -17 8.33 0.79 0 1 17 8.13 1.35 0 -1 -18 14.35 1.08 0 1 18 15.21 1.88 0 -1 -19 2.71 0.46 0 1 19 2.67 0.83 0 1 20 0.26 0.44 0 -1 -20 0.28 0.14 0 -1 -21 3.15 0.53 0 1 21 3.84 1.04 0 -1 -22 -0.15 0.11 0 1 22 -0.14 0.40 0 -1 -23 0.75 0.28 0 1 23 0.74 0.71 0 1 24 1.16 0.52 0 1 25 3.15 1.20 0 1 26 13.16 2.18 0 1 27 3.70 1.49 0 1 28 33.86 3.76 0 1 29 2.50 1.24 0 1 30 2.79 1.35 0 1 31 3.25 1.20 0 1 32 0.32 0.56 0 1 33 2.14 1.12 0 1 34 -0.91 0.84 0 1 35 -1.22 1.11 0 1 36 -0.30 0.66 0 1 37 -0.81 0.74 0 -2 38 -0.08 0.31 0 -2 37 -0.36 0.58 0 -2 36 0.38 0.29 0 -2 35 0.14 0.54 0 -2 34 0.78 0.74 0 -2 33 0.09 0.51 0 -2 32 -0.27 0.58 0 -2 31 2.91 1.12 0 -2 30 11.33 2.23 0 -2 29 -0.59 0.78 0 -2 28 0.08 0.51 0 -2 27 -0.31 0.45 0 -2 26 0.29 0.56 0 -2 25 1.09 0.27 0 -2 24 36.02 3.31 0 -2 23 1.54 0.74 0 -2 22 26.84 2.77 0 -2 21 3.09 0.95 0 -2 20 0.89 0.21 0 -2 19 -0.35 0.41 0 -2 18 35.90 2.85 0 -2 17 0.39 0.28 0 -2 16 9.19 1.33 0 -2 15 1.86 0.24 0 -2 15 1.32 0.45 0 -2 14 0.32 0.10 0 -2 14 -0.98 0.81 0 -2 13 -0.94 0.61 0 -2 13 -0.01 0.03 0 -2 12 112.29 1.77 0 -2 12 120.60 4.20 0 -2 11 11.02 0.54 0 -2 11 11.06 1.23 0 2 -10 19.29 1.57 0 -2 10 18.54 1.52 0 -2 9 0.73 0.19 0 2 -9 1.59 0.46 0 -2 8 553.64 7.45 0 2 -8 563.79 7.68 0 -2 7 301.88 5.24 0 2 -7 309.27 5.37 0 -2 6 25.83 1.42 0 2 -6 25.46 1.43 0 2 -5 0.35 0.18 0 -2 5 0.45 0.17 0 2 -4 79.81 2.19 0 -2 4 81.43 2.15 0 -2 3 27.39 0.91 0 2 2 356.92 3.31 0 2 3 0.57 0.16 0 -2 -4 1.48 0.26 0 2 4 1.26 0.23 0 2 5 6.79 0.56 0 -2 -5 7.13 0.56 0 -2 -6 457.91 4.72 0 2 6 442.19 4.80 0 2 7 101.88 2.47 0 -2 -7 99.55 2.30 0 -2 -8 17.72 1.03 0 2 8 19.80 1.15 0 -2 -9 8.70 0.76 0 2 9 8.47 0.79 0 2 10 188.43 4.00 0 -2 -10 173.59 3.60 0 2 11 -0.11 0.21 0 -2 -11 0.06 0.10 0 2 11 0.04 0.23 0 -2 -12 127.60 3.35 0 2 12 128.73 4.49 0 -2 -12 125.25 3.33 0 2 12 123.15 3.57 0 -2 -13 15.00 1.19 0 2 13 16.42 1.65 0 -2 -13 15.23 1.21 0 -2 -14 138.05 3.62 0 -2 -14 133.16 3.73 0 2 14 136.62 4.95 0 -2 -15 0.32 0.24 0 2 15 0.63 0.73 0 2 16 89.34 4.31 0 -2 -16 82.08 2.88 0 2 17 2.56 1.02 0 -2 -17 1.77 0.47 0 2 18 4.99 1.15 0 -2 -18 4.75 0.71 0 -2 -19 0.05 0.15 0 2 19 0.06 0.22 0 2 20 9.41 1.57 0 -2 -20 9.52 1.02 0 2 21 0.74 0.43 0 -2 -21 1.07 0.33 0 -2 -22 1.22 0.36 0 2 22 1.23 0.58 0 -2 -23 0.33 0.20 0 2 23 0.36 0.30 0 -2 -24 9.78 1.08 0 2 24 9.77 1.83 0 2 25 5.62 1.50 0 -2 -25 4.43 0.74 0 2 26 29.39 3.29 0 2 27 17.58 2.67 0 2 28 5.25 1.59 0 2 29 2.09 1.16 0 2 30 11.77 2.35 0 2 31 0.13 0.60 0 2 32 1.54 1.01 0 2 33 0.37 0.58 0 2 34 1.26 0.86 0 2 35 -0.49 0.66 0 2 36 -0.11 0.57 0 2 37 -0.24 0.41 0 -3 38 0.36 0.31 0 -3 37 -0.34 0.34 0 -3 36 0.16 0.50 0 -3 35 -0.26 0.36 0 -3 34 -0.42 0.65 0 -3 33 0.68 0.61 0 -3 32 -0.10 0.25 0 -3 31 0.37 0.46 0 -3 30 4.58 1.35 0 -3 29 1.76 0.88 0 -3 28 -0.71 0.67 0 -3 27 0.06 0.39 0 -3 26 1.01 0.61 0 -3 25 3.58 1.11 0 -3 24 44.03 3.64 0 -3 23 1.11 0.67 0 -3 22 1.46 0.66 0 -3 21 1.73 0.67 0 -3 20 1.42 0.66 0 -3 19 8.92 1.38 0 -3 18 2.54 0.62 0 -3 17 0.76 0.16 0 -3 17 0.84 0.37 0 -3 16 0.49 0.33 0 -3 16 0.45 0.13 0 -3 15 26.00 2.21 0 -3 15 24.21 0.90 0 -3 14 0.33 0.37 0 -3 13 19.61 1.78 0 -3 12 7.01 1.03 0 -3 11 213.71 5.46 0 -3 10 0.09 0.18 0 3 -10 0.18 0.20 0 3 -9 182.99 4.75 0 -3 9 175.02 4.54 0 -3 8 20.43 1.47 0 3 -8 18.01 1.41 0 3 -7 494.77 7.10 0 -3 7 498.32 7.01 0 3 -6 113.00 3.25 0 -3 6 103.79 3.06 0 3 -5 4.36 0.61 0 -3 5 4.50 0.61 0 3 -5 5.30 0.67 0 -3 5 4.87 0.47 0 -3 4 15.89 1.07 0 3 -4 15.51 1.06 0 -3 4 16.36 0.86 0 3 -4 16.30 1.09 0 3 -3 415.56 4.44 0 -3 3 405.96 5.38 0 3 -3 405.17 5.28 0 -3 3 420.73 4.34 0 -3 3 417.35 5.15 0 -3 3 417.11 4.40 0 3 -3 418.74 5.25 0 3 -2 1.10 0.23 0 3 -2 1.07 0.25 0 -3 2 1.05 0.29 0 -3 2 1.09 0.24 0 3 -2 1.03 0.25 0 3 -1 30.62 1.24 0 -3 1 31.14 1.38 0 3 -1 31.25 0.93 0 3 -1 31.92 1.34 0 3 0 0.03 0.09 0 -3 0 -0.06 0.11 0 -3 0 0.25 0.11 0 3 0 0.18 0.11 0 -3 -1 196.01 3.22 0 -3 -1 198.86 3.18 0 3 1 197.83 3.13 0 3 1 206.63 3.13 0 3 2 20.10 1.05 0 3 2 20.04 0.82 0 3 2 19.11 0.95 0 -3 -2 18.54 0.96 0 3 3 1.08 0.22 0 -3 -3 0.99 0.21 0 3 3 1.35 0.25 0 3 4 6.57 0.58 0 -3 -4 6.31 0.56 0 3 5 3.16 0.44 0 -3 -5 2.80 0.40 0 3 6 30.47 1.35 0 -3 -6 31.47 1.34 0 -3 -7 5.52 0.60 0 3 7 4.85 0.57 0 -3 -8 11.00 0.87 0 3 8 10.26 0.88 0 3 9 29.05 1.56 0 -3 -9 26.46 1.41 0 3 10 12.84 1.10 0 -3 -10 11.94 0.97 0 -3 -11 7.62 0.78 0 3 11 7.81 0.84 0 -3 -12 34.80 1.77 0 3 12 37.02 1.98 0 3 13 -0.07 0.22 0 -3 -13 -0.02 0.15 0 3 14 6.29 1.07 0 3 14 5.87 0.83 0 -3 -14 5.69 0.76 0 -3 -14 5.65 0.82 0 -3 -15 2.59 0.53 0 3 15 2.61 0.70 0 3 15 2.11 0.46 0 -3 -16 19.10 1.55 0 3 16 20.00 2.11 0 -3 -17 22.34 1.70 0 3 17 22.76 2.34 0 -3 -18 0.60 0.33 0 3 18 0.71 0.54 0 3 19 0.56 0.30 0 -3 -19 0.82 0.33 0 3 20 1.31 0.44 0 -3 -20 2.07 0.52 0 -3 -21 1.08 0.44 0 3 21 0.09 0.23 0 3 22 21.23 2.56 0 -3 -22 19.78 1.69 0 3 23 1.00 0.60 0 -3 -23 0.93 0.47 0 3 24 -0.05 0.54 0 -3 -24 -0.16 0.30 0 -3 -25 0.09 0.12 0 3 25 -1.56 0.78 0 3 26 4.72 1.26 0 -3 -26 4.54 0.79 0 3 27 0.25 0.48 0 3 28 0.14 0.41 0 3 29 0.82 0.65 0 3 30 0.61 0.52 0 3 31 1.82 0.93 0 3 32 1.19 0.92 0 3 33 0.02 0.45 0 3 34 2.86 1.38 0 3 35 1.47 1.12 0 3 36 0.22 0.36 0 3 37 0.94 0.93 0 -4 38 -0.33 0.58 0 -4 37 0.66 0.60 0 -4 36 0.20 0.53 0 -4 35 0.35 0.63 0 -4 34 0.16 0.60 0 -4 33 -0.06 0.39 0 -4 32 0.09 0.44 0 -4 31 -0.47 0.62 0 -4 30 4.07 1.22 0 -4 29 0.71 0.40 0 -4 28 1.72 0.84 0 -4 27 1.57 0.67 0 -4 26 1.68 0.54 0 -4 25 2.26 0.98 0 -4 24 46.19 3.81 0 -4 23 3.56 1.01 0 -4 22 -0.32 0.60 0 -4 21 0.03 0.37 0 -4 20 1.58 0.64 0 -4 19 1.59 0.25 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38.03 2.38 0 -6 8 38.43 1.89 0 -6 8 38.34 2.11 0 -6 7 12.67 1.08 0 6 -7 13.95 1.43 0 -6 7 11.96 1.22 0 -6 7 13.54 1.18 0 6 -6 123.47 3.47 0 -6 6 125.94 3.44 0 -6 6 125.17 3.38 0 6 -6 124.90 4.20 0 6 -5 6.68 0.95 0 -6 5 7.63 0.77 0 6 -5 7.16 0.83 0 -6 5 7.20 0.73 0 -6 4 33.39 1.51 0 6 -4 35.62 1.86 0 -6 4 35.85 1.50 0 6 -4 36.44 2.12 0 -6 3 42.93 1.53 0 6 -3 42.84 2.25 0 6 -3 43.10 2.09 0 -6 3 42.00 2.36 0 -6 3 41.91 1.51 0 6 -2 536.83 7.75 0 6 -2 498.55 7.21 0 -6 2 504.03 4.55 0 -6 2 505.12 6.69 0 -6 1 15.11 1.35 0 6 -1 13.62 1.23 0 -6 1 13.17 0.62 0 6 -1 12.88 0.80 0 6 -1 13.94 1.23 0 -6 1 13.10 1.07 0 -6 0 277.02 5.72 0 6 0 291.01 5.50 0 6 0 274.14 3.55 0 -6 0 277.49 3.57 0 -6 0 274.19 5.07 0 6 1 58.75 2.34 0 -6 -1 60.89 2.62 0 -6 -1 61.87 1.78 0 6 1 63.01 2.52 0 -6 -1 62.00 2.46 0 6 2 0.10 0.09 0 -6 -2 -0.06 0.14 0 6 2 0.11 0.13 0 -6 -2 0.08 0.11 0 6 3 5.14 0.70 0 6 3 5.55 0.75 0 -6 -3 5.48 0.77 0 -6 -4 17.35 1.37 0 6 4 17.35 1.27 0 6 4 17.24 1.08 0 6 4 18.42 1.44 0 6 5 30.13 1.92 0 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288.92 7.39 0 8 -8 671.06 11.03 0 -8 8 646.25 9.00 0 -8 8 644.53 8.42 0 -8 7 7.82 0.94 0 8 -7 8.78 1.48 0 -8 7 7.84 0.97 0 -8 6 475.12 6.85 0 -8 6 460.02 6.42 0 8 -6 469.17 8.91 0 8 -5 78.62 3.57 0 -8 5 79.14 2.49 0 -8 5 79.31 2.62 0 -8 4 72.33 2.26 0 -8 4 72.51 2.25 0 8 -4 70.08 3.33 0 8 -3 64.01 3.11 0 -8 3 62.16 1.91 0 -8 2 40.15 1.35 0 8 -2 41.15 2.49 0 8 -1 15.18 1.01 0 -8 1 14.65 0.66 0 8 -1 14.19 1.44 0 -8 0 11.79 0.88 0 8 0 13.62 1.39 0 8 0 11.48 0.85 0 8 1 -0.54 0.61 0 -8 -1 0.79 0.23 0 8 1 0.44 0.17 0 8 2 22.03 1.66 0 8 2 20.39 1.60 0 -8 -2 22.03 1.28 0 8 3 0.58 0.30 0 8 3 0.69 0.29 0 8 4 0.39 0.32 0 8 4 -0.15 0.30 0 8 5 0.48 0.34 0 8 5 1.02 0.47 0 8 6 71.98 3.06 0 8 6 79.86 3.52 0 8 6 71.12 2.59 0 8 7 12.56 0.64 0 8 7 15.68 1.46 0 8 7 15.47 1.27 0 8 7 16.04 1.64 0 8 8 136.60 4.26 0 8 8 136.80 5.00 0 8 8 133.23 3.94 0 8 8 124.77 2.41 0 8 9 159.91 5.52 0 8 9 142.34 2.92 0 8 9 151.02 4.62 0 8 10 0.24 0.21 0 8 10 1.53 0.66 0 8 11 60.66 2.28 0 8 11 68.09 3.23 0 8 12 1.03 0.35 0 8 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4.47 0.94 0 -10 1 2.93 0.45 0 10 -1 3.71 0.55 0 -10 0 0.23 0.14 0 10 0 0.26 0.21 0 10 0 -0.28 0.37 0 10 1 117.97 3.02 0 -10 -1 123.21 3.27 0 10 1 121.43 4.59 0 10 2 98.86 4.13 0 10 2 92.37 2.68 0 -10 -2 93.94 3.03 0 10 3 170.14 5.27 0 10 3 164.22 5.23 0 10 4 2.36 0.77 0 10 4 2.44 0.68 0 10 5 31.23 2.27 0 10 5 28.77 2.28 0 10 6 0.07 0.18 0 10 6 0.94 0.52 0 10 7 33.49 2.34 0 10 7 32.92 2.51 0 10 8 2.98 0.76 0 10 8 2.80 0.79 0 10 9 33.19 2.37 0 10 9 33.19 2.68 0 10 10 13.76 0.77 0 10 10 19.71 2.15 0 10 10 17.38 1.78 0 10 11 40.75 2.76 0 10 11 43.64 3.23 0 10 11 34.71 1.41 0 10 12 2.76 0.87 0 10 12 2.26 0.41 0 10 12 3.49 0.90 0 10 13 1.44 0.34 0 10 13 2.39 0.71 0 10 13 1.20 0.49 0 10 14 2.75 0.85 0 10 14 3.75 0.86 0 10 15 1.64 0.56 0 10 16 1.60 0.51 0 10 17 9.96 1.48 0 10 18 0.71 0.61 0 10 19 2.77 0.85 0 10 20 4.02 0.99 0 10 21 1.76 0.75 0 -10 -21 0.61 0.70 0 10 22 1.10 0.59 0 -10 -22 1.52 0.74 0 10 23 0.35 0.25 0 -10 -23 1.00 0.82 0 -10 -24 4.43 1.27 0 10 24 3.17 0.94 0 10 25 2.14 0.77 0 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