# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_1 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl6 N6 O14 Pr2' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1717.70 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pr Pr -0.2180 2.8214 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _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+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.470(4) _cell_length_b 25.550(7) _cell_length_c 9.964(3) _cell_angle_alpha 90 _cell_angle_beta 91.569(4) _cell_angle_gamma 90 _cell_volume 3427.8(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 37356 _cell_measurement_theta_min 4.389 _cell_measurement_theta_max 56.073 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.664 _exptl_crystal_F_000 1712 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 1.710 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6566 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36852 _diffrn_reflns_av_unetI/netI 0.0585 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.512 _diffrn_reflns_theta_max 30.153 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.934 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.934 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.934 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 9445 _reflns_number_gt 7136 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0254P)^2^+2.9838P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 9445 _refine_ls_number_parameters 459 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0576 _refine_ls_R_factor_gt 0.0347 _refine_ls_wR_factor_ref 0.0766 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pr1 Pr 0.96815(2) 0.09989(2) 0.01516(2) 0.01401(5) Uani 1 1 d . . . . . Cl3 Cl 0.43183(7) -0.08699(4) 0.15974(11) 0.0462(2) Uani 1 1 d . . . . . Cl2 Cl 0.38298(7) 0.25981(5) 0.13584(11) 0.0511(3) Uani 1 1 d . . . . . Cl1 Cl 1.41352(12) 0.04914(6) -0.61864(15) 0.0939(6) Uani 1 1 d . . . . . O2 O 1.03293(15) 0.05309(7) -0.1993(2) 0.0208(4) Uani 1 1 d . . . . . O3 O 0.81790(15) 0.13589(8) 0.1098(2) 0.0212(4) Uani 1 1 d . . . . . OW1 O 0.94565(17) 0.05742(8) 0.2452(2) 0.0213(5) Uani 1 1 d D . . . . O1 O 1.09815(15) 0.13051(7) -0.1502(2) 0.0211(4) Uani 1 1 d . . . . . O5 O 0.84997(15) 0.03091(7) -0.0221(2) 0.0204(4) Uani 1 1 d . . . . . O6 O 1.11387(15) 0.05059(7) 0.0821(2) 0.0198(4) Uani 1 1 d . . . . . O4 O 0.76024(16) 0.09626(8) 0.2930(2) 0.0237(4) Uani 1 1 d . . . . . N1 N 1.06957(18) 0.16457(9) 0.1760(2) 0.0186(5) Uani 1 1 d . . . . . N3 N 0.86492(18) 0.13322(9) -0.1964(2) 0.0190(5) Uani 1 1 d . . . . . N2 N 0.94874(17) 0.20391(9) -0.0208(2) 0.0158(5) Uani 1 1 d . . . . . C30 C 0.8279(2) -0.01652(11) -0.0359(3) 0.0163(6) Uani 1 1 d . . . . . C21 C 1.2298(4) 0.03722(15) -0.5227(4) 0.0530(12) Uani 1 1 d . . . . . H21 H 1.2186 0.0147 -0.5950 0.064 Uiso 1 1 calc R U . . . C31 C 0.7269(2) -0.03371(11) 0.0058(3) 0.0183(6) Uani 1 1 d . . . . . C23 C 0.7514(2) 0.12661(11) 0.1953(3) 0.0184(6) Uani 1 1 d . . . . . C11 C 0.8323(2) 0.18301(11) -0.2043(3) 0.0181(6) Uani 1 1 d . . . . . C6 C 0.9977(2) 0.23861(11) 0.0581(3) 0.0166(6) Uani 1 1 d . . . . . C17 C 1.1723(2) 0.08105(11) -0.3247(3) 0.0236(7) Uani 1 1 d . . . . . C4 C 1.1244(2) 0.24984(12) 0.2471(3) 0.0223(6) Uani 1 1 d . . . . . H4 H 1.1221 0.2860 0.2365 0.027 Uiso 1 1 calc R U . . . C10 C 0.8856(2) 0.22212(11) -0.1174(3) 0.0169(6) Uani 1 1 d . . . . . C9 C 0.8717(2) 0.27573(12) -0.1397(3) 0.0229(6) Uani 1 1 d . . . . . H9 H 0.8290 0.2874 -0.2082 0.028 Uiso 1 1 calc R U . . . C24 C 0.6562(2) 0.15752(11) 0.1769(3) 0.0198(6) Uani 1 1 d . . . . . C5 C 1.0664(2) 0.21731(11) 0.1639(3) 0.0169(6) Uani 1 1 d . . . . . C15 C 0.8237(2) 0.09800(12) -0.2821(3) 0.0236(6) Uani 1 1 d . . . . . H15 H 0.8460 0.0636 -0.2773 0.028 Uiso 1 1 calc R U . . . C2 C 1.1880(2) 0.17361(12) 0.3586(3) 0.0246(7) Uani 1 1 d . . . . . H2 H 1.2287 0.1579 0.4237 0.030 Uiso 1 1 calc R U . . . C1 C 1.1292(2) 0.14371(12) 0.2728(3) 0.0228(6) Uani 1 1 d . . . . . H1 H 1.1307 0.1075 0.2822 0.027 Uiso 1 1 calc R U . . . C8 C 0.9225(2) 0.31111(11) -0.0585(3) 0.0243(7) Uani 1 1 d . . . . . H8 H 0.9145 0.3469 -0.0718 0.029 Uiso 1 1 calc R U . . . C28 C 0.4969(2) 0.18553(15) 0.2589(3) 0.0338(8) Uani 1 1 d . . . . . H28 H 0.4474 0.1835 0.3220 0.041 Uiso 1 1 calc R U . . . C26 C 0.5580(2) 0.22156(12) 0.0531(3) 0.0259(7) Uani 1 1 d . . . . . H26 H 0.5492 0.2435 -0.0209 0.031 Uiso 1 1 calc R U . . . C14 C 0.7505(2) 0.11015(12) -0.3763(3) 0.0267(7) Uani 1 1 d . . . . . H14 H 0.7264 0.0851 -0.4367 0.032 Uiso 1 1 calc R U . . . C32 C 0.6900(2) -0.08301(12) -0.0281(3) 0.0258(7) Uani 1 1 d . . . . . H32 H 0.7272 -0.1053 -0.0807 0.031 Uiso 1 1 calc R U . . . C7 C 0.9851(2) 0.29268(11) 0.0423(3) 0.0213(6) Uani 1 1 d . . . . . H7 H 1.0186 0.3159 0.0994 0.026 Uiso 1 1 calc R U . . . C35 C 0.5794(2) -0.01691(13) 0.1318(4) 0.0330(8) Uani 1 1 d . . . . . H35 H 0.5424 0.0050 0.1858 0.040 Uiso 1 1 calc R U . . . C25 C 0.6421(2) 0.19053(11) 0.0668(3) 0.0226(6) Uani 1 1 d . . . . . H25 H 0.6900 0.1918 0.0014 0.027 Uiso 1 1 calc R U . . . C16 C 1.0961(2) 0.08904(11) -0.2193(3) 0.0191(6) Uani 1 1 d . . . . . C12 C 0.7547(2) 0.19740(12) -0.2909(3) 0.0259(7) Uani 1 1 d . . . . . H12 H 0.7302 0.2314 -0.2905 0.031 Uiso 1 1 calc R U . . . C29 C 0.5817(2) 0.15456(13) 0.2711(3) 0.0256(7) Uani 1 1 d . . . . . H29 H 0.5888 0.1316 0.3431 0.031 Uiso 1 1 calc R U . . . C27 C 0.4876(2) 0.21937(14) 0.1514(3) 0.0307(8) Uani 1 1 d . . . . . C36 C 0.6705(2) -0.00092(12) 0.0844(3) 0.0277(7) Uani 1 1 d . . . . . H36 H 0.6941 0.0323 0.1057 0.033 Uiso 1 1 calc R U . . . C19 C 1.3380(3) 0.09675(16) -0.4029(4) 0.0424(10) Uani 1 1 d . . . . . H19 H 1.3995 0.1130 -0.3933 0.051 Uiso 1 1 calc R U . . . C3 C 1.1851(2) 0.22767(12) 0.3454(3) 0.0252(7) Uani 1 1 d . . . . . H3 H 1.2236 0.2487 0.4023 0.030 Uiso 1 1 calc R U . . . C33 C 0.5974(2) -0.09909(13) 0.0165(3) 0.0323(8) Uani 1 1 d . . . . . H33 H 0.5718 -0.1316 -0.0078 0.039 Uiso 1 1 calc R U . . . C18 C 1.2629(2) 0.10734(13) -0.3137(3) 0.0295(7) Uani 1 1 d . . . . . H18 H 1.2732 0.1321 -0.2463 0.035 Uiso 1 1 calc R U . . . C34 C 0.5449(2) -0.06601(13) 0.0969(3) 0.0296(7) Uani 1 1 d . . . . . C13 C 0.7142(3) 0.16036(13) -0.3781(3) 0.0304(8) Uani 1 1 d . . . . . H13 H 0.6627 0.1695 -0.4376 0.036 Uiso 1 1 calc R U . . . C20 C 1.3198(4) 0.06180(16) -0.5055(4) 0.0516(12) Uani 1 1 d . . . . . C22 C 1.1550(3) 0.04618(12) -0.4308(3) 0.0377(9) Uani 1 1 d . . . . . H22 H 1.0943 0.0291 -0.4403 0.045 Uiso 1 1 calc R U . . . H37 H 0.953(3) 0.0204(8) 0.239(5) 0.073(15) Uiso 1 1 d D . . . . H38 H 0.888(3) 0.0625(16) 0.268(4) 0.049(13) Uiso 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 Pr1 0.01753(8) 0.00819(7) 0.01645(8) 0.00043(6) 0.00306(5) -0.00005(6) Cl3 0.0292(5) 0.0535(6) 0.0565(6) -0.0085(5) 0.0150(4) -0.0191(4) Cl2 0.0254(5) 0.0707(7) 0.0572(6) -0.0053(5) 0.0016(4) 0.0169(5) Cl1 0.1212(12) 0.0721(9) 0.0931(10) 0.0236(8) 0.0869(10) 0.0416(8) O2 0.0256(11) 0.0129(10) 0.0242(11) -0.0011(8) 0.0044(9) -0.0024(8) O3 0.0225(11) 0.0157(10) 0.0258(11) 0.0006(8) 0.0095(9) -0.0011(8) OW1 0.0248(12) 0.0178(11) 0.0214(11) 0.0025(9) 0.0039(9) 0.0004(9) O1 0.0259(11) 0.0115(9) 0.0264(11) -0.0004(8) 0.0080(9) -0.0002(8) O5 0.0227(11) 0.0111(9) 0.0275(11) 0.0001(8) 0.0024(9) -0.0022(8) O6 0.0209(11) 0.0150(10) 0.0238(11) -0.0001(8) 0.0037(8) 0.0016(8) O4 0.0264(11) 0.0236(11) 0.0212(11) 0.0000(9) 0.0042(9) -0.0037(9) N1 0.0233(13) 0.0120(11) 0.0204(13) -0.0032(9) 0.0013(10) 0.0027(9) N3 0.0234(13) 0.0142(12) 0.0194(12) 0.0017(10) 0.0011(10) -0.0001(10) N2 0.0190(12) 0.0111(11) 0.0177(12) -0.0005(9) 0.0052(9) 0.0015(9) C30 0.0188(14) 0.0156(13) 0.0145(13) 0.0028(11) -0.0011(11) -0.0007(11) C21 0.102(4) 0.0230(19) 0.036(2) 0.0005(16) 0.037(2) 0.009(2) C31 0.0207(15) 0.0137(13) 0.0203(14) 0.0009(11) -0.0016(11) -0.0023(11) C23 0.0194(14) 0.0155(14) 0.0205(15) -0.0058(11) 0.0038(11) -0.0065(11) C11 0.0198(15) 0.0199(14) 0.0148(13) 0.0055(11) 0.0049(11) 0.0034(11) C6 0.0183(14) 0.0133(13) 0.0184(14) -0.0009(11) 0.0068(11) 0.0001(11) C17 0.0363(18) 0.0120(13) 0.0230(16) 0.0043(12) 0.0095(13) 0.0071(12) C4 0.0234(16) 0.0176(14) 0.0263(16) -0.0041(12) 0.0063(13) -0.0017(12) C10 0.0210(15) 0.0140(13) 0.0161(14) 0.0033(11) 0.0087(11) 0.0027(11) C9 0.0272(16) 0.0193(15) 0.0226(15) 0.0062(12) 0.0053(13) 0.0069(12) C24 0.0174(14) 0.0200(15) 0.0220(15) -0.0080(12) 0.0035(12) -0.0039(11) C5 0.0140(13) 0.0148(13) 0.0223(15) -0.0039(11) 0.0077(11) 0.0002(10) C15 0.0307(16) 0.0200(15) 0.0202(15) -0.0011(12) 0.0012(12) -0.0028(13) C2 0.0243(16) 0.0276(17) 0.0220(16) -0.0036(13) -0.0014(13) 0.0039(13) C1 0.0286(17) 0.0163(14) 0.0235(16) -0.0023(12) -0.0001(13) 0.0033(12) C8 0.0353(18) 0.0116(14) 0.0263(16) 0.0023(12) 0.0089(14) 0.0056(12) C28 0.0185(16) 0.056(2) 0.0268(18) -0.0086(16) 0.0051(13) -0.0033(15) C26 0.0246(16) 0.0233(16) 0.0298(17) -0.0020(13) 0.0000(13) -0.0010(13) C14 0.0327(18) 0.0271(17) 0.0199(15) -0.0008(12) -0.0022(13) -0.0054(13) C32 0.0281(17) 0.0212(15) 0.0285(17) -0.0072(13) 0.0041(14) -0.0066(13) C7 0.0277(17) 0.0106(13) 0.0262(16) -0.0036(11) 0.0086(13) -0.0020(11) C35 0.0262(17) 0.0300(18) 0.043(2) -0.0124(16) 0.0106(15) -0.0028(14) C25 0.0209(15) 0.0206(15) 0.0264(16) -0.0041(12) 0.0053(12) -0.0051(12) C16 0.0281(16) 0.0124(14) 0.0168(14) 0.0041(10) 0.0031(12) 0.0040(11) C12 0.0284(17) 0.0227(16) 0.0265(16) 0.0020(13) -0.0010(13) 0.0079(13) C29 0.0198(16) 0.0376(19) 0.0194(15) -0.0040(13) 0.0023(12) -0.0056(13) C27 0.0171(15) 0.041(2) 0.0338(19) -0.0115(15) 0.0005(14) 0.0027(14) C36 0.0232(16) 0.0183(15) 0.042(2) -0.0084(14) 0.0055(14) -0.0033(12) C19 0.034(2) 0.051(2) 0.042(2) 0.023(2) 0.0163(17) 0.0161(18) C3 0.0229(16) 0.0266(17) 0.0260(16) -0.0089(13) 0.0003(13) -0.0045(13) C33 0.0319(18) 0.0287(17) 0.0365(19) -0.0096(15) 0.0034(14) -0.0165(15) C18 0.0287(17) 0.0316(19) 0.0286(17) 0.0106(14) 0.0070(14) 0.0105(14) C34 0.0220(16) 0.0319(18) 0.0353(19) -0.0038(15) 0.0041(14) -0.0104(14) C13 0.0313(18) 0.038(2) 0.0217(17) 0.0046(14) -0.0052(14) 0.0028(15) C20 0.072(3) 0.035(2) 0.049(3) 0.0189(19) 0.044(2) 0.027(2) C22 0.071(3) 0.0149(15) 0.0280(18) 0.0023(13) 0.0159(18) -0.0038(16) _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 Pr1 O5 2.397(2) . ? Pr1 O6 2.411(2) . ? Pr1 O3 2.436(2) . ? Pr1 O1 2.560(2) . ? Pr1 OW1 2.561(2) . ? Pr1 O2 2.619(2) . ? Pr1 N3 2.635(2) . ? Pr1 N1 2.654(2) . ? Pr1 N2 2.694(2) . ? Pr1 C16 2.954(3) . ? Cl3 C34 1.747(3) . ? Cl2 C27 1.751(3) . ? Cl1 C20 1.746(4) . ? O2 C16 1.272(3) . ? O3 C23 1.275(3) . ? OW1 H37 0.952(19) . ? OW1 H38 0.82(4) . ? O1 C16 1.263(3) . ? O5 C30 1.254(3) . ? O6 C30 1.267(3) 3_755 ? O4 C23 1.248(3) . ? N1 C1 1.347(4) . ? N1 C5 1.354(3) . ? N3 C11 1.347(4) . ? N3 C15 1.349(4) . ? N2 C6 1.345(4) . ? N2 C10 1.350(4) . ? C30 O6 1.267(3) 3_755 ? C30 C31 1.499(4) . ? C21 C20 1.372(7) . ? C21 C22 1.398(5) . ? C21 H21 0.9300 . ? C31 C36 1.387(4) . ? C31 C32 1.392(4) . ? C23 C24 1.514(4) . ? C11 C12 1.386(4) . ? C11 C10 1.493(4) . ? C6 C7 1.400(4) . ? C6 C5 1.486(4) . ? C17 C18 1.395(5) . ? C17 C22 1.397(5) . ? C17 C16 1.502(4) . ? C4 C3 1.380(4) . ? C4 C5 1.398(4) . ? C4 H4 0.9300 . ? C10 C9 1.399(4) . ? C9 C8 1.382(4) . ? C9 H9 0.9300 . ? C24 C25 1.392(4) . ? C24 C29 1.394(4) . ? C15 C14 1.379(4) . ? C15 H15 0.9300 . ? C2 C1 1.380(4) . ? C2 C3 1.388(4) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C8 C7 1.377(4) . ? C8 H8 0.9300 . ? C28 C27 1.380(5) . ? C28 C29 1.393(5) . ? C28 H28 0.9300 . ? C26 C27 1.383(4) . ? C26 C25 1.386(4) . ? C26 H26 0.9300 . ? C14 C13 1.373(4) . ? C14 H14 0.9300 . ? C32 C33 1.397(4) . ? C32 H32 0.9300 . ? C7 H7 0.9300 . ? C35 C34 1.379(4) . ? C35 C36 1.389(4) . ? C35 H35 0.9300 . ? C25 H25 0.9300 . ? C12 C13 1.387(4) . ? C12 H12 0.9300 . ? C29 H29 0.9300 . ? C36 H36 0.9300 . ? C19 C20 1.375(6) . ? C19 C18 1.392(5) . ? C19 H19 0.9300 . ? C3 H3 0.9300 . ? C33 C34 1.374(5) . ? C33 H33 0.9300 . ? C18 H18 0.9300 . ? C13 H13 0.9300 . ? C22 H22 0.9300 . ? 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 Pr1 O6 101.01(7) . . ? O5 Pr1 O3 77.43(7) . . ? O6 Pr1 O3 140.27(7) . . ? O5 Pr1 O1 126.03(7) . . ? O6 Pr1 O1 76.79(7) . . ? O3 Pr1 O1 136.38(7) . . ? O5 Pr1 OW1 74.49(7) . . ? O6 Pr1 OW1 69.31(7) . . ? O3 Pr1 OW1 72.17(7) . . ? O1 Pr1 OW1 143.64(7) . . ? O5 Pr1 O2 76.86(7) . . ? O6 Pr1 O2 72.55(7) . . ? O3 Pr1 O2 141.90(7) . . ? O1 Pr1 O2 50.60(6) . . ? OW1 Pr1 O2 125.93(7) . . ? O5 Pr1 N3 77.29(7) . . ? O6 Pr1 N3 142.93(7) . . ? O3 Pr1 N3 76.21(7) . . ? O1 Pr1 N3 75.02(7) . . ? OW1 Pr1 N3 141.27(7) . . ? O2 Pr1 N3 71.04(7) . . ? O5 Pr1 N1 151.62(7) . . ? O6 Pr1 N1 75.92(7) . . ? O3 Pr1 N1 87.17(7) . . ? O1 Pr1 N1 81.29(7) . . ? OW1 Pr1 N1 78.17(7) . . ? O2 Pr1 N1 126.83(7) . . ? N3 Pr1 N1 122.24(7) . . ? O5 Pr1 N2 130.04(7) . . ? O6 Pr1 N2 128.87(7) . . ? O3 Pr1 N2 66.43(7) . . ? O1 Pr1 N2 71.25(6) . . ? OW1 Pr1 N2 121.57(7) . . ? O2 Pr1 N2 112.05(6) . . ? N3 Pr1 N2 61.81(7) . . ? N1 Pr1 N2 60.82(7) . . ? O5 Pr1 C16 102.00(8) . . ? O6 Pr1 C16 71.42(7) . . ? O3 Pr1 C16 148.25(7) . . ? O1 Pr1 C16 25.21(7) . . ? OW1 Pr1 C16 138.92(7) . . ? O2 Pr1 C16 25.48(7) . . ? N3 Pr1 C16 72.79(8) . . ? N1 Pr1 C16 103.54(8) . . ? N2 Pr1 C16 92.53(7) . . ? C16 O2 Pr1 92.14(16) . . ? C23 O3 Pr1 142.59(19) . . ? Pr1 OW1 H37 110(3) . . ? Pr1 OW1 H38 108(3) . . ? H37 OW1 H38 106(4) . . ? C16 O1 Pr1 95.13(17) . . ? C30 O5 Pr1 151.83(19) . . ? C30 O6 Pr1 140.01(18) 3_755 . ? C1 N1 C5 118.3(3) . . ? C1 N1 Pr1 118.20(18) . . ? C5 N1 Pr1 123.45(19) . . ? C11 N3 C15 117.7(3) . . ? C11 N3 Pr1 121.04(18) . . ? C15 N3 Pr1 119.30(19) . . ? C6 N2 C10 118.6(2) . . ? C6 N2 Pr1 121.89(18) . . ? C10 N2 Pr1 119.46(18) . . ? O5 C30 O6 123.8(3) . 3_755 ? O5 C30 C31 117.8(3) . . ? O6 C30 C31 118.4(2) 3_755 . ? C20 C21 C22 119.5(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C36 C31 C32 119.1(3) . . ? C36 C31 C30 119.6(3) . . ? C32 C31 C30 121.2(3) . . ? O4 C23 O3 125.7(3) . . ? O4 C23 C24 118.8(3) . . ? O3 C23 C24 115.5(3) . . ? N3 C11 C12 121.7(3) . . ? N3 C11 C10 116.6(2) . . ? C12 C11 C10 121.7(3) . . ? N2 C6 C7 121.9(3) . . ? N2 C6 C5 117.3(2) . . ? C7 C6 C5 120.8(3) . . ? C18 C17 C22 119.6(3) . . ? C18 C17 C16 119.5(3) . . ? C22 C17 C16 120.9(3) . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N2 C10 C9 122.0(3) . . ? N2 C10 C11 117.8(2) . . ? C9 C10 C11 120.2(3) . . ? C8 C9 C10 119.1(3) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C25 C24 C29 118.6(3) . . ? C25 C24 C23 120.5(3) . . ? C29 C24 C23 120.9(3) . . ? N1 C5 C4 121.5(3) . . ? N1 C5 C6 116.5(2) . . ? C4 C5 C6 122.0(3) . . ? N3 C15 C14 123.7(3) . . ? N3 C15 H15 118.2 . . ? C14 C15 H15 118.2 . . ? C1 C2 C3 118.5(3) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? N1 C1 C2 123.0(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C7 C8 C9 119.1(3) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C27 C28 C29 118.7(3) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C27 C26 C25 118.8(3) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C13 C14 C15 117.8(3) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C31 C32 C33 120.3(3) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C8 C7 C6 119.3(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C34 C35 C36 118.5(3) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C26 C25 C24 121.2(3) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? O1 C16 O2 121.7(3) . . ? O1 C16 C17 119.3(3) . . ? O2 C16 C17 119.0(3) . . ? O1 C16 Pr1 59.66(15) . . ? O2 C16 Pr1 62.38(15) . . ? C17 C16 Pr1 172.0(2) . . ? C11 C12 C13 119.1(3) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C28 C29 C24 120.9(3) . . ? C28 C29 H29 119.5 . . ? C24 C29 H29 119.5 . . ? C28 C27 C26 121.8(3) . . ? C28 C27 Cl2 119.6(3) . . ? C26 C27 Cl2 118.7(3) . . ? C35 C36 C31 121.1(3) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C20 C19 C18 118.9(4) . . ? C20 C19 H19 120.6 . . ? C18 C19 H19 120.6 . . ? C4 C3 C2 119.4(3) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C34 C33 C32 118.9(3) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C19 C18 C17 120.4(4) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C33 C34 C35 122.1(3) . . ? C33 C34 Cl3 119.2(2) . . ? C35 C34 Cl3 118.7(3) . . ? C14 C13 C12 119.7(3) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C19 C20 C21 122.0(3) . . ? C19 C20 Cl1 118.9(4) . . ? C21 C20 Cl1 119.1(4) . . ? C17 C22 C21 119.5(4) . . ? C17 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? _refine_diff_density_max 0.965 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.113 _shelxl_version_number 2013-4 _shelx_res_file ; TITL P21onC in P2(1)/c CELL 0.71073 13.4698 25.5504 9.9637 90.000 91.569 90.000 ZERR 2.00 0.0037 0.0071 0.0028 0.000 0.004 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL PR UNIT 144 100 12 28 12 4 MERG 2 FMAP 2 PLAN 10 ACTA 51.00 BOND $H DFIX 0.98 OW1 H37 L.S. 12 WGHT 0.025400 2.983800 FVAR 0.08545 PR1 6 0.968150 0.099891 0.015157 11.00000 0.01753 0.00819 = 0.01645 0.00043 0.00306 -0.00005 CL3 5 0.431827 -0.086985 0.159744 11.00000 0.02922 0.05353 = 0.05648 -0.00850 0.01500 -0.01908 CL2 5 0.382976 0.259806 0.135839 11.00000 0.02537 0.07071 = 0.05720 -0.00535 0.00163 0.01690 CL1 5 1.413519 0.049140 -0.618639 11.00000 0.12115 0.07206 = 0.09313 0.02356 0.08687 0.04165 O2 4 1.032933 0.053093 -0.199305 11.00000 0.02565 0.01286 = 0.02416 -0.00113 0.00445 -0.00237 O3 4 0.817899 0.135891 0.109755 11.00000 0.02251 0.01565 = 0.02580 0.00060 0.00953 -0.00114 OW1 4 0.945647 0.057417 0.245158 11.00000 0.02483 0.01779 = 0.02144 0.00248 0.00390 0.00044 O1 4 1.098155 0.130511 -0.150223 11.00000 0.02589 0.01155 = 0.02639 -0.00045 0.00799 -0.00022 O5 4 0.849965 0.030911 -0.022102 11.00000 0.02270 0.01106 = 0.02747 0.00009 0.00243 -0.00219 O6 4 1.113869 0.050594 0.082051 11.00000 0.02087 0.01499 = 0.02378 -0.00009 0.00372 0.00162 O4 4 0.760243 0.096258 0.292989 11.00000 0.02640 0.02361 = 0.02122 0.00001 0.00418 -0.00366 N1 3 1.069566 0.164566 0.176030 11.00000 0.02332 0.01204 = 0.02042 -0.00321 0.00130 0.00266 N3 3 0.864920 0.133224 -0.196429 11.00000 0.02342 0.01421 = 0.01940 0.00167 0.00115 -0.00009 N2 3 0.948737 0.203912 -0.020763 11.00000 0.01901 0.01109 = 0.01766 -0.00053 0.00522 0.00151 C30 1 0.827907 -0.016522 -0.035865 11.00000 0.01882 0.01556 = 0.01454 0.00278 -0.00112 -0.00068 C21 1 1.229784 0.037220 -0.522709 11.00000 0.10185 0.02299 = 0.03616 0.00049 0.03696 0.00881 AFIX 43 H21 2 1.218571 0.014748 -0.594969 11.00000 -1.20000 AFIX 0 C31 1 0.726902 -0.033706 0.005783 11.00000 0.02069 0.01372 = 0.02031 0.00088 -0.00161 -0.00232 C23 1 0.751433 0.126614 0.195306 11.00000 0.01942 0.01554 = 0.02047 -0.00575 0.00376 -0.00649 C11 1 0.832301 0.183013 -0.204257 11.00000 0.01985 0.01993 = 0.01484 0.00549 0.00490 0.00336 C6 1 0.997684 0.238607 0.058138 11.00000 0.01832 0.01330 = 0.01840 -0.00085 0.00678 0.00009 C17 1 1.172272 0.081047 -0.324697 11.00000 0.03632 0.01198 = 0.02303 0.00432 0.00953 0.00712 C4 1 1.124364 0.249845 0.247135 11.00000 0.02336 0.01760 = 0.02627 -0.00415 0.00629 -0.00173 AFIX 43 H4 2 1.122055 0.285988 0.236450 11.00000 -1.20000 AFIX 0 C10 1 0.885581 0.222123 -0.117408 11.00000 0.02103 0.01396 = 0.01612 0.00329 0.00865 0.00269 C9 1 0.871739 0.275732 -0.139714 11.00000 0.02721 0.01932 = 0.02256 0.00624 0.00532 0.00691 AFIX 43 H9 2 0.828979 0.287380 -0.208236 11.00000 -1.20000 AFIX 0 C24 1 0.656158 0.157518 0.176906 11.00000 0.01738 0.02003 = 0.02201 -0.00800 0.00352 -0.00386 C5 1 1.066396 0.217311 0.163860 11.00000 0.01399 0.01476 = 0.02228 -0.00393 0.00773 0.00015 C15 1 0.823731 0.097997 -0.282112 11.00000 0.03066 0.02004 = 0.02023 -0.00110 0.00120 -0.00278 AFIX 43 H15 2 0.846021 0.063580 -0.277341 11.00000 -1.20000 AFIX 0 C2 1 1.188014 0.173612 0.358570 11.00000 0.02429 0.02757 = 0.02196 -0.00360 -0.00145 0.00395 AFIX 43 H2 2 1.228744 0.157874 0.423748 11.00000 -1.20000 AFIX 0 C1 1 1.129156 0.143714 0.272784 11.00000 0.02865 0.01626 = 0.02353 -0.00231 -0.00014 0.00327 AFIX 43 H1 2 1.130708 0.107509 0.282213 11.00000 -1.20000 AFIX 0 C8 1 0.922482 0.311113 -0.058521 11.00000 0.03529 0.01165 = 0.02634 0.00229 0.00893 0.00562 AFIX 43 H8 2 0.914476 0.346909 -0.071812 11.00000 -1.20000 AFIX 0 C28 1 0.496881 0.185532 0.258898 11.00000 0.01846 0.05644 = 0.02678 -0.00863 0.00507 -0.00326 AFIX 43 H28 2 0.447416 0.183451 0.321991 11.00000 -1.20000 AFIX 0 C26 1 0.558049 0.221565 0.053076 11.00000 0.02458 0.02331 = 0.02984 -0.00205 0.00003 -0.00101 AFIX 43 H26 2 0.549161 0.243452 -0.020859 11.00000 -1.20000 AFIX 0 C14 1 0.750474 0.110147 -0.376323 11.00000 0.03273 0.02715 = 0.01995 -0.00079 -0.00222 -0.00545 AFIX 43 H14 2 0.726389 0.085135 -0.436703 11.00000 -1.20000 AFIX 0 C32 1 0.690044 -0.083005 -0.028122 11.00000 0.02807 0.02116 = 0.02846 -0.00724 0.00410 -0.00660 AFIX 43 H32 2 0.727209 -0.105333 -0.080705 11.00000 -1.20000 AFIX 0 C7 1 0.985064 0.292683 0.042333 11.00000 0.02766 0.01056 = 0.02617 -0.00363 0.00864 -0.00202 AFIX 43 H7 2 1.018603 0.315903 0.099364 11.00000 -1.20000 AFIX 0 C35 1 0.579350 -0.016906 0.131757 11.00000 0.02615 0.02999 = 0.04338 -0.01237 0.01062 -0.00285 AFIX 43 H35 2 0.542423 0.004994 0.185779 11.00000 -1.20000 AFIX 0 C25 1 0.642121 0.190534 0.066836 11.00000 0.02094 0.02060 = 0.02636 -0.00411 0.00525 -0.00511 AFIX 43 H25 2 0.689992 0.191787 0.001403 11.00000 -1.20000 AFIX 0 C16 1 1.096114 0.089043 -0.219302 11.00000 0.02814 0.01236 = 0.01683 0.00412 0.00306 0.00402 C12 1 0.754736 0.197401 -0.290879 11.00000 0.02840 0.02273 = 0.02655 0.00205 -0.00098 0.00789 AFIX 43 H12 2 0.730208 0.231423 -0.290481 11.00000 -1.20000 AFIX 0 C29 1 0.581727 0.154559 0.271131 11.00000 0.01981 0.03757 = 0.01940 -0.00398 0.00235 -0.00559 AFIX 43 H29 2 0.588833 0.131584 0.343150 11.00000 -1.20000 AFIX 0 C27 1 0.487638 0.219367 0.151351 11.00000 0.01710 0.04127 = 0.03377 -0.01147 0.00050 0.00271 C36 1 0.670486 -0.000919 0.084369 11.00000 0.02318 0.01831 = 0.04175 -0.00843 0.00550 -0.00329 AFIX 43 H36 2 0.694112 0.032342 0.105681 11.00000 -1.20000 AFIX 0 C19 1 1.338022 0.096750 -0.402925 11.00000 0.03431 0.05144 = 0.04218 0.02281 0.01631 0.01611 AFIX 43 H19 2 1.399541 0.113049 -0.393302 11.00000 -1.20000 AFIX 0 C3 1 1.185077 0.227666 0.345424 11.00000 0.02293 0.02662 = 0.02605 -0.00894 0.00030 -0.00453 AFIX 43 H3 2 1.223647 0.248745 0.402294 11.00000 -1.20000 AFIX 0 C33 1 0.597449 -0.099086 0.016513 11.00000 0.03194 0.02870 = 0.03651 -0.00965 0.00344 -0.01654 AFIX 43 H33 2 0.571832 -0.131642 -0.007761 11.00000 -1.20000 AFIX 0 C18 1 1.262919 0.107340 -0.313683 11.00000 0.02871 0.03156 = 0.02864 0.01064 0.00698 0.01049 AFIX 43 H18 2 1.273209 0.132092 -0.246294 11.00000 -1.20000 AFIX 0 C34 1 0.544875 -0.066005 0.096856 11.00000 0.02199 0.03186 = 0.03526 -0.00379 0.00412 -0.01041 C13 1 0.714237 0.160359 -0.378119 11.00000 0.03127 0.03784 = 0.02175 0.00462 -0.00524 0.00276 AFIX 43 H13 2 0.662723 0.169502 -0.437613 11.00000 -1.20000 AFIX 0 C20 1 1.319768 0.061799 -0.505538 11.00000 0.07245 0.03542 = 0.04922 0.01891 0.04427 0.02693 C22 1 1.155036 0.046184 -0.430826 11.00000 0.07117 0.01491 = 0.02796 0.00229 0.01594 -0.00382 AFIX 43 H22 2 1.094310 0.029072 -0.440277 11.00000 -1.20000 AFIX 0 H37 2 0.952756 0.020442 0.239022 11.00000 0.07284 H38 2 0.888359 0.062509 0.267515 11.00000 0.04898 HKLF 4 REM P21onC in P2(1)/c REM R1 = 0.0347 for 7136 Fo > 4sig(Fo) and 0.0576 for all 9445 data REM 459 parameters refined using 1 restraints END WGHT 0.0228 2.2798 REM Highest difference peak 0.965, deepest hole -1.001, 1-sigma level 0.113 Q1 1 1.3456 0.0286 -0.6600 11.00000 0.05 0.96 Q2 1 1.0184 0.1029 -0.1021 11.00000 0.05 0.67 Q3 1 0.4591 -0.1081 0.2171 11.00000 0.05 0.54 Q4 1 0.9336 0.1004 0.1404 11.00000 0.05 0.49 Q5 1 0.5041 0.2066 0.2089 11.00000 0.05 0.48 Q6 1 0.5466 0.1800 0.2541 11.00000 0.05 0.46 Q7 1 0.9851 0.1299 0.0935 11.00000 0.05 0.45 Q8 1 1.1773 0.0611 -0.3756 11.00000 0.05 0.45 Q9 1 0.6448 -0.0883 -0.0166 11.00000 0.05 0.44 Q10 1 0.8032 0.1920 -0.2659 11.00000 0.05 0.44 ; _shelx_res_checksum 23108 _shelx_hkl_file ; 0 0 1 0.01 0.21 0 0 1 -0.01 0.20 0 0 1 -0.27 0.15 0 0 2 114.64 5.75 0 0 2 111.97 5.12 0 0 3 0.34 0.52 0 0 -3 -0.36 0.36 0 0 -3 -0.03 0.40 0 0 3 -0.34 0.55 0 0 4 95.59 4.66 0 0 -4 97.48 4.59 0 0 4 96.78 5.25 0 0 -4 96.76 4.64 0 0 -5 0.06 0.46 0 0 -5 0.32 0.46 0 0 5 -1.00 0.61 0 0 5 -0.94 0.53 0 0 6 200.06 10.57 0 0 -6 202.67 9.49 0 0 6 208.86 9.47 0 0 -6 198.78 9.36 0 0 7 -0.40 0.80 0 0 -7 -0.10 0.55 0 0 7 -0.88 0.59 0 0 8 88.40 5.28 0 0 -8 80.93 4.37 0 0 -9 1.26 1.04 0 0 9 -0.31 0.99 0 0 10 17.24 2.40 0 0 -10 16.12 2.19 0 0 11 1.51 1.49 0 0 -11 -2.11 0.87 0 0 -12 -0.81 1.23 0 0 12 1.35 1.54 0 0 -13 -0.33 1.33 0 1 1 586.61 25.08 0 1 1 593.85 28.18 0 -1 -1 578.60 25.75 0 -1 1 538.13 28.16 0 -1 1 604.51 25.06 0 -1 1 596.00 25.66 0 1 2 56.69 2.78 0 1 2 58.49 3.12 0 -1 2 58.47 2.76 0 -1 2 57.98 2.75 0 -1 -2 56.51 2.71 0 -1 2 59.01 3.12 0 1 3 185.31 8.24 0 1 3 179.74 9.23 0 -1 3 175.65 8.20 0 -1 -3 182.62 8.25 0 -1 3 183.06 8.29 0 -1 3 192.09 9.24 0 1 4 54.59 3.34 0 1 4 56.13 3.00 0 -1 -4 58.84 2.85 0 -1 4 56.55 2.98 0 -1 4 59.46 2.88 0 -1 4 53.94 3.35 0 1 -5 195.43 8.89 0 1 -5 199.69 9.01 0 1 5 186.75 8.89 0 1 5 202.28 10.00 0 -1 5 187.79 8.87 0 -1 5 185.27 9.95 0 -1 -5 189.10 8.82 0 1 -6 10.18 1.05 0 1 6 9.16 1.38 0 1 6 7.72 1.10 0 1 -6 8.67 1.03 0 -1 -6 8.09 0.94 0 -1 6 8.87 1.36 0 -1 6 10.29 1.25 0 1 7 66.53 4.25 0 1 -7 64.75 3.55 0 1 7 70.17 3.83 0 1 -7 66.71 3.62 0 -1 7 68.44 3.79 0 -1 -7 66.59 3.50 0 -1 7 63.71 4.20 0 1 8 20.04 2.34 0 1 -8 19.86 1.66 0 -1 -8 18.76 1.59 0 -1 -8 20.53 2.10 0 -1 8 23.68 2.46 0 1 9 10.12 1.88 0 1 -9 15.80 1.98 0 -1 9 9.74 1.83 0 -1 -9 11.35 1.77 0 1 -10 1.94 1.21 0 1 10 3.06 1.44 0 -1 10 2.05 1.44 0 -1 -10 1.93 1.21 0 1 -11 19.86 2.52 0 1 11 17.14 2.61 0 -1 -11 19.47 2.49 0 -1 11 20.15 2.76 0 1 12 16.96 2.64 0 1 -12 16.28 2.41 0 -1 -12 12.97 2.19 0 -1 12 12.46 2.48 0 1 -13 -0.13 1.37 0 -1 -13 4.05 1.73 0 -2 0 24.17 1.12 0 -2 0 25.53 1.21 0 2 1 0.13 0.21 0 2 1 0.03 0.29 0 -2 -1 -0.01 0.20 0 -2 1 0.35 0.21 0 -2 1 -0.46 0.23 0 -2 1 0.46 0.32 0 2 2 182.69 8.74 0 2 2 174.11 7.78 0 -2 2 172.73 7.91 0 -2 -2 168.59 7.83 0 -2 2 177.60 7.74 0 2 3 15.09 1.34 0 2 3 15.19 1.12 0 -2 -3 14.63 1.00 0 -2 3 14.67 1.33 0 -2 3 13.99 1.05 0 -2 3 13.17 1.12 0 2 4 77.79 4.57 0 2 4 83.35 4.12 0 -2 4 78.97 4.02 0 -2 4 81.66 4.06 0 -2 4 87.71 4.62 0 -2 -4 87.92 3.97 0 2 5 107.21 6.20 0 2 5 117.46 5.58 0 -2 5 116.71 5.53 0 -2 5 111.66 5.45 0 -2 -5 121.65 5.40 0 -2 5 107.01 6.17 0 2 6 4.98 1.10 0 2 -6 4.90 0.81 0 2 -6 4.81 0.83 0 2 6 3.41 0.88 0 -2 6 3.83 0.90 0 -2 -6 4.04 0.71 0 -2 6 6.72 1.18 0 2 7 16.52 1.97 0 2 -7 18.15 1.49 0 2 -7 15.44 1.50 0 -2 7 16.41 1.72 0 -2 7 18.59 2.05 0 -2 -7 17.57 1.38 0 2 8 6.80 1.47 0 2 -8 4.64 1.01 0 2 -8 6.46 1.05 0 -2 8 3.25 1.04 0 -2 8 5.19 1.34 0 -2 -8 8.66 1.46 0 -2 -8 5.30 0.89 0 2 9 42.56 3.55 0 2 -9 51.98 3.35 0 -2 9 48.05 3.63 0 -2 -9 45.55 3.30 0 2 10 24.44 2.88 0 2 -10 22.37 2.51 0 -2 10 25.66 2.91 0 -2 -10 21.91 2.55 0 2 -11 18.97 2.37 0 2 11 16.98 2.49 0 -2 11 11.80 2.24 0 -2 -11 13.15 2.09 0 2 -12 2.74 1.48 0 2 12 -0.86 1.58 0 -2 -12 3.67 1.58 0 -2 12 4.75 1.87 0 2 -13 23.25 3.05 0 -2 -13 32.89 3.49 0 3 0 -0.99 0.26 0 3 0 -0.83 0.16 0 -3 0 -0.83 0.23 0 -3 0 -0.91 0.17 0 3 -1 14.85 1.14 0 3 1 15.02 1.13 0 -3 -1 18.05 0.94 0 -3 -1 16.61 0.98 0 -3 1 18.02 1.05 0 -3 1 16.56 0.87 0 3 2 32.82 1.73 0 3 2 31.48 2.00 0 -3 2 33.76 1.79 0 -3 -2 29.95 1.64 0 -3 2 36.08 1.99 0 -3 2 31.27 1.68 0 3 3 4.51 0.81 0 3 3 6.19 0.76 0 -3 3 4.59 0.70 0 -3 3 4.79 0.68 0 -3 3 6.96 0.93 0 -3 -3 5.86 0.61 0 3 4 118.84 6.14 0 3 4 117.88 5.48 0 -3 4 116.44 5.41 0 -3 -4 101.67 5.30 0 -3 4 120.97 5.48 0 3 5 26.41 1.79 0 3 5 22.65 1.94 0 -3 5 21.23 1.66 0 -3 -5 22.96 1.48 0 -3 5 24.67 1.94 0 -3 5 25.08 1.60 0 3 6 26.08 2.22 0 -3 6 25.71 1.77 0 -3 -6 27.01 1.67 0 -3 6 24.81 1.87 0 -3 6 27.07 2.17 0 3 -7 19.11 1.69 0 3 7 18.49 2.08 0 3 -7 20.16 1.63 0 -3 7 18.80 1.83 0 -3 -7 18.12 1.88 0 -3 7 18.33 2.07 0 -3 -7 18.03 1.43 0 3 8 18.52 2.25 0 3 -8 19.79 1.79 0 3 -8 20.17 1.83 0 -3 -8 18.39 2.09 0 -3 8 18.09 2.23 0 -3 8 19.31 2.00 0 3 9 1.22 1.19 0 3 -9 0.33 0.76 0 3 -9 1.29 0.85 0 3 -9 1.01 1.02 0 -3 9 0.34 1.09 0 -3 -9 0.11 0.97 0 3 10 24.61 3.00 0 3 -10 30.18 2.92 0 -3 -10 33.31 3.10 0 -3 10 28.26 3.13 0 3 11 9.67 2.19 0 3 -11 8.68 1.81 0 -3 -11 13.39 2.11 0 -3 11 9.44 2.09 0 3 12 44.99 4.07 0 3 -12 45.60 3.65 0 -3 -12 43.00 3.62 0 -3 12 42.17 3.90 0 3 -13 1.62 1.44 0 -3 -13 0.71 1.43 0 4 0 202.06 10.19 0 4 0 211.18 8.95 0 -4 0 210.18 9.27 0 -4 0 204.61 8.94 0 4 -1 106.94 5.25 0 4 1 106.07 5.27 0 -4 1 104.70 4.53 0 -4 -1 98.48 4.63 0 -4 1 98.04 4.78 0 -4 -1 105.26 4.72 0 4 2 3.18 0.70 0 -4 2 3.33 0.68 0 -4 -2 2.91 0.61 0 -4 2 3.85 0.50 0 -4 -2 3.07 0.47 0 -4 2 2.59 0.54 0 4 3 7.11 0.97 0 -4 3 7.37 0.80 0 -4 3 6.40 0.81 0 -4 -3 7.62 0.68 0 -4 3 9.53 1.07 0 4 4 133.39 7.61 0 -4 4 138.85 7.60 0 -4 4 144.54 6.87 0 -4 -4 162.11 6.72 0 -4 4 148.31 6.73 0 4 5 58.26 3.72 0 -4 5 57.51 3.24 0 -4 5 61.75 3.26 0 -4 5 62.66 3.74 0 -4 -5 67.21 3.13 0 4 6 107.00 5.51 0 -4 -6 92.70 4.91 0 -4 6 93.26 4.73 0 -4 -6 86.88 4.52 0 -4 6 88.61 5.33 0 -4 6 95.34 4.76 0 4 7 -0.30 0.82 0 -4 -7 0.18 0.55 0 -4 7 0.74 0.72 0 -4 -7 0.99 0.85 0 -4 7 1.20 0.96 0 4 -8 11.41 1.41 0 4 -8 10.97 1.37 0 4 8 11.39 1.81 0 -4 8 11.19 1.53 0 -4 8 10.02 1.72 0 -4 -8 11.94 1.71 0 4 9 26.03 2.85 0 4 -9 28.65 2.18 0 4 -9 26.10 2.12 0 -4 9 22.03 2.67 0 -4 -9 22.43 2.44 0 4 10 44.55 3.70 0 4 -10 44.14 3.31 0 -4 10 43.30 3.65 0 -4 -10 50.53 3.54 0 4 11 45.34 3.92 0 4 -11 43.33 3.43 0 -4 11 50.01 3.99 0 -4 -11 41.82 3.49 0 4 -12 2.28 1.45 0 4 12 3.30 1.86 0 -4 -12 2.00 1.47 0 4 -13 7.46 1.88 0 -4 -13 9.45 2.24 0 5 0 -0.20 0.46 0 -5 0 -0.16 0.39 0 -5 0 0.25 0.29 0 5 -1 200.05 10.68 0 5 1 210.01 10.71 0 -5 -1 221.76 9.46 0 -5 1 224.06 9.35 0 -5 -1 225.83 9.69 0 -5 1 209.19 9.75 0 5 2 11.31 1.13 0 5 -2 12.84 1.16 0 -5 2 11.28 0.88 0 -5 -2 11.79 0.89 0 -5 -2 10.24 0.98 0 -5 2 11.31 1.01 0 5 3 157.63 7.94 0 -5 -3 156.65 6.98 0 -5 3 154.55 6.92 0 -5 3 144.91 7.87 0 -5 3 156.86 7.19 0 -5 -3 148.65 7.06 0 5 4 5.05 0.98 0 -5 -4 5.41 0.93 0 -5 -4 5.77 0.66 0 -5 4 5.85 0.85 0 -5 4 5.71 0.99 0 -5 4 5.38 0.79 0 5 5 121.49 6.42 0 -5 -5 119.81 5.47 0 -5 -5 120.72 5.78 0 -5 5 114.34 5.69 0 -5 5 110.98 6.33 0 -5 5 110.79 5.57 0 5 6 10.76 1.54 0 -5 -6 12.67 1.08 0 -5 6 13.15 1.61 0 -5 -6 11.73 1.49 0 -5 6 9.95 1.21 0 -5 6 10.29 1.30 0 5 7 112.36 6.42 0 -5 -7 119.98 5.38 0 -5 -7 109.70 5.81 0 -5 7 110.83 5.63 0 -5 7 107.71 5.59 0 -5 7 100.21 6.28 0 5 8 -0.83 0.92 0 5 -8 0.82 0.81 0 5 -8 0.16 0.65 0 -5 8 0.03 0.75 0 -5 -8 -0.28 0.83 0 -5 8 -0.79 0.89 0 5 -9 24.70 2.15 0 5 9 27.43 2.89 0 5 -9 22.76 2.20 0 -5 -9 26.56 2.63 0 -5 9 27.52 2.89 0 5 -10 -0.95 0.96 0 5 10 0.36 1.24 0 -5 10 -0.35 1.16 0 -5 -10 -0.03 1.11 0 5 -11 2.90 1.41 0 5 11 1.32 1.53 0 -5 -11 2.56 1.41 0 -5 11 6.54 1.82 0 5 12 8.88 2.32 0 5 -12 15.07 2.31 0 -5 -12 12.91 2.25 0 5 -13 7.59 1.90 0 -5 -13 7.45 1.97 0 6 0 752.19 37.89 0 -6 0 795.53 33.55 0 -6 0 795.86 34.52 0 6 -1 18.56 1.66 0 6 1 25.45 1.78 0 -6 -1 27.36 1.50 0 -6 1 26.13 1.59 0 -6 1 27.85 1.28 0 -6 -1 27.49 1.46 0 6 2 90.54 5.11 0 -6 2 98.30 4.67 0 -6 -2 100.33 4.53 0 -6 -2 93.60 4.52 0 -6 2 99.85 4.37 0 6 3 3.43 0.85 0 -6 -3 4.53 0.59 0 -6 3 4.35 0.88 0 -6 3 4.46 0.62 0 -6 3 2.76 0.71 0 -6 -3 4.82 0.80 0 6 4 69.55 4.12 0 -6 -4 69.70 3.43 0 -6 4 70.74 3.68 0 -6 4 69.42 3.50 0 -6 4 73.09 4.10 0 -6 -4 73.89 3.74 0 6 5 39.58 2.74 0 -6 -5 36.46 2.47 0 -6 5 39.76 2.39 0 -6 5 41.52 2.34 0 -6 5 38.55 2.69 0 -6 -5 38.75 2.12 0 6 6 88.69 5.22 0 -6 6 91.52 4.64 0 -6 6 89.08 4.54 0 -6 -6 88.79 4.76 0 -6 -6 87.55 4.31 0 -6 6 88.48 5.19 0 6 7 21.50 2.30 0 -6 7 19.95 1.69 0 -6 7 19.24 1.86 0 -6 -7 21.99 2.13 0 -6 -7 18.72 1.46 0 -6 7 22.70 2.31 0 6 8 47.71 3.65 0 -6 8 59.66 3.78 0 -6 -8 46.18 3.33 0 -6 8 47.70 3.15 0 6 -9 3.58 1.11 0 6 9 3.63 1.37 0 6 -9 2.63 1.04 0 -6 -9 4.68 1.35 0 -6 9 2.88 1.35 0 6 -10 12.61 1.84 0 6 10 9.17 2.01 0 -6 -10 9.71 1.78 0 -6 10 7.21 1.88 0 6 -11 45.27 3.34 0 6 11 37.18 3.60 0 -6 -11 40.11 3.78 0 -6 11 44.18 3.73 0 6 -12 3.00 1.52 0 6 12 4.71 1.90 0 -6 -12 4.69 1.73 0 6 -13 9.39 2.03 0 -6 -13 9.81 2.11 0 7 0 -0.27 0.55 0 -7 0 0.29 0.34 0 -7 0 0.28 0.47 0 7 1 4.30 0.78 0 7 -1 3.78 0.75 0 -7 1 5.47 0.73 0 -7 -1 3.97 0.63 0 -7 1 4.83 0.45 0 -7 -1 4.14 0.59 0 7 -2 85.58 4.33 0 7 2 74.56 4.32 0 -7 2 76.13 3.60 0 -7 2 78.22 3.93 0 -7 -2 77.19 3.78 0 -7 -2 80.67 3.79 0 7 3 86.89 4.70 0 7 -3 80.42 4.65 0 -7 -3 85.95 4.17 0 -7 3 83.24 4.26 0 -7 3 84.85 3.96 0 -7 -3 85.11 4.04 0 7 4 39.98 2.78 0 -7 4 42.86 2.48 0 -7 4 41.05 2.28 0 -7 -4 42.39 2.52 0 -7 -4 39.13 2.20 0 -7 4 49.16 2.82 0 7 5 12.77 1.53 0 -7 -5 12.00 1.01 0 -7 5 12.97 1.53 0 -7 5 11.23 1.17 0 -7 -5 10.84 1.37 0 -7 5 12.16 1.30 0 7 6 24.61 2.17 0 -7 6 22.65 2.10 0 -7 6 23.50 1.75 0 -7 -6 25.87 2.05 0 -7 6 24.61 1.84 0 -7 -6 24.60 1.54 0 7 7 4.29 1.16 0 -7 -7 2.94 1.03 0 -7 -7 4.03 0.72 0 -7 7 4.81 1.02 0 -7 7 3.74 1.18 0 -7 7 4.13 0.96 0 7 8 46.12 3.45 0 -7 8 47.07 2.93 0 -7 8 42.77 3.42 0 -7 8 44.47 2.92 0 -7 -8 44.97 3.13 0 7 -9 5.77 1.23 0 7 9 2.87 1.37 0 7 -9 4.92 1.18 0 -7 9 3.99 1.44 0 -7 -9 3.22 1.32 0 7 10 78.95 5.57 0 7 -10 88.09 4.99 0 -7 -10 86.12 5.14 0 -7 10 77.78 5.44 0 7 -11 0.36 1.09 0 7 11 0.12 1.39 0 -7 -11 -0.81 1.12 0 -7 11 0.76 1.49 0 7 12 36.89 3.87 0 7 -12 30.97 3.17 0 -7 -12 27.13 3.28 0 7 -13 0.86 1.45 0 -7 -13 2.64 1.63 0 8 0 0.31 0.55 0 -8 0 0.24 0.50 0 -8 0 0.24 0.35 0 8 1 96.46 5.07 0 8 -1 99.01 5.05 0 -8 -1 95.63 4.52 0 -8 1 94.97 4.60 0 -8 -1 88.35 4.32 0 -8 1 90.71 4.18 0 8 -2 2.33 0.76 0 8 2 3.80 0.86 0 -8 2 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1.79 0 -10 8 14.45 2.06 0 -10 8 15.52 1.87 0 -10 -8 14.39 1.97 0 10 9 3.64 1.45 0 -10 9 3.45 1.06 0 -10 -9 1.84 1.22 0 -10 9 0.75 1.26 0 -10 9 1.47 0.98 0 10 10 19.07 2.68 0 10 -10 22.23 2.30 0 -10 10 14.68 2.44 0 -10 -10 21.90 2.60 0 10 11 0.64 1.57 0 10 -11 1.69 1.08 0 -10 11 -0.04 1.41 0 -10 -11 0.60 1.36 0 10 -12 3.29 1.45 0 10 12 0.38 1.75 0 -10 -12 -0.18 1.38 0 11 0 0.21 0.59 0 -11 0 -0.04 0.39 0 -11 0 0.21 0.55 0 11 -1 122.31 7.12 0 11 1 127.56 7.15 0 -11 1 129.14 6.49 0 -11 -1 137.57 6.45 0 -11 1 147.67 5.99 0 -11 -1 140.32 6.14 0 11 -2 0.60 0.61 0 11 2 0.60 0.68 0 -11 2 0.44 0.33 0 -11 -2 0.25 0.54 0 -11 2 0.16 0.52 0 -11 -2 0.27 0.51 0 11 -3 203.71 9.37 0 11 3 177.69 9.33 0 -11 3 168.85 8.46 0 -11 3 171.27 7.87 0 -11 -3 175.64 8.23 0 -11 -3 168.41 8.14 0 11 -4 5.11 1.06 0 11 4 6.89 1.24 0 -11 -4 6.96 1.06 0 -11 4 6.66 0.78 0 -11 -4 6.63 0.86 0 -11 4 6.47 1.08 0 11 5 51.93 3.52 0 11 -5 42.86 3.30 0 -11 5 53.43 2.79 0 -11 -5 53.36 2.75 0 -11 5 55.29 3.14 0 -11 -5 50.82 3.10 0 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0.68 0.61 0 -14 -1 0.48 0.48 0 -14 1 0.83 0.38 0 -14 1 0.10 0.57 0 14 2 152.47 7.61 0 14 -2 140.00 7.53 0 -14 -2 138.21 6.68 0 -14 -2 136.41 6.42 0 -14 2 135.97 6.12 0 -14 2 125.97 6.80 0 14 -3 2.68 0.94 0 14 3 3.25 1.03 0 -14 -3 4.24 0.86 0 -14 -3 3.14 0.73 0 -14 3 2.12 0.47 0 -14 3 2.51 0.80 0 14 4 126.17 7.21 0 14 -4 147.54 7.24 0 -14 -4 122.98 6.25 0 -14 4 131.42 6.60 0 -14 -4 121.74 6.17 0 -14 4 122.24 5.85 0 14 -5 14.02 1.86 0 14 5 14.95 1.97 0 -14 -5 15.18 1.73 0 -14 5 18.55 1.90 0 -14 -5 17.18 1.41 0 -14 5 16.33 1.29 0 14 6 50.06 3.64 0 14 -6 48.91 3.54 0 -14 -6 50.23 3.19 0 -14 6 49.59 2.78 0 -14 6 45.14 3.17 0 14 -7 80.23 4.80 0 14 7 64.96 4.74 0 -14 7 65.57 3.80 0 -14 -7 72.57 4.28 0 -14 7 71.21 4.27 0 14 8 27.57 3.11 0 14 -8 38.85 3.08 0 -14 8 31.19 2.62 0 -14 -8 28.72 2.86 0 14 -9 7.47 1.78 0 14 9 7.89 1.96 0 -14 -9 8.49 1.74 0 -14 9 10.05 1.80 0 14 -10 12.06 2.21 0 14 10 10.29 2.24 0 -14 -10 12.98 2.13 0 -14 10 13.13 2.03 0 14 11 9.95 2.32 0 -14 -11 12.45 2.25 0 14 12 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70.13 4.19 0 21 1 44.85 3.79 0 -21 -1 53.62 3.42 0 -21 1 53.59 3.52 0 21 2 21.22 2.53 0 21 -2 25.87 2.71 0 -21 -2 18.83 2.02 0 -21 2 20.60 2.19 0 21 3 102.15 6.38 0 21 -3 116.38 6.50 0 -21 -3 102.74 5.52 0 -21 3 93.78 5.72 0 -21 -3 104.61 5.24 0 21 -4 -0.32 0.90 0 21 4 0.22 1.00 0 -21 -4 0.02 0.77 0 -21 4 0.18 0.97 0 -21 -4 1.18 0.81 0 21 -5 27.38 3.11 0 21 5 36.52 3.24 0 -21 -5 33.54 2.56 0 -21 5 35.41 2.88 0 21 -6 5.39 1.62 0 21 6 7.30 1.89 0 -21 -6 6.07 1.42 0 -21 6 5.06 1.41 0 21 7 21.84 2.98 0 21 -7 18.65 2.65 0 -21 -7 19.28 2.36 0 -21 7 23.18 2.69 0 21 -8 17.84 2.62 0 21 8 13.56 2.59 0 -21 8 18.65 2.43 0 -21 -8 14.42 2.24 0 21 -9 8.06 2.08 0 21 9 13.89 2.66 0 -21 -9 11.91 2.12 0 -21 9 11.47 2.12 0 21 10 14.54 2.80 0 -21 10 12.70 2.32 0 -21 -10 9.28 2.16 0 21 11 11.30 2.77 0 -21 11 6.07 2.03 0 -21 -11 11.02 2.42 0 22 0 70.86 4.78 0 -22 0 70.25 4.24 0 22 -1 2.31 1.25 0 22 1 1.49 1.19 0 -22 1 1.06 0.99 0 -22 -1 3.52 1.07 0 22 -2 3.38 1.30 0 22 2 0.50 1.03 0 -22 -2 2.58 1.01 0 -22 2 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13.32 2.29 0 23 6 14.41 2.43 0 -23 6 13.25 2.08 0 -23 -6 12.52 1.85 0 23 -7 3.13 1.61 0 23 7 1.62 1.60 0 -23 7 0.82 1.20 0 -23 -7 0.02 1.06 0 23 8 24.95 3.42 0 23 -8 20.08 2.92 0 -23 -8 22.79 2.67 0 -23 8 25.56 2.95 0 23 9 0.14 1.59 0 23 -9 0.79 1.67 0 -23 9 -1.03 1.25 0 -23 -9 -1.02 1.22 0 23 10 23.75 3.63 0 -23 -10 22.21 2.94 0 -23 10 17.77 2.79 0 24 0 44.73 3.70 0 -24 0 47.27 3.28 0 24 -1 1.74 1.25 0 24 1 2.53 1.27 0 -24 -1 1.60 0.94 0 -24 1 1.27 1.03 0 24 2 57.54 4.21 0 24 -2 55.63 4.14 0 -24 -2 51.02 3.47 0 -24 2 52.51 3.69 0 24 -3 15.68 2.35 0 24 3 20.60 2.63 0 -24 -3 16.67 1.95 0 -24 3 14.39 2.08 0 24 4 50.19 4.09 0 24 -4 54.58 4.10 0 -24 4 48.70 3.67 0 -24 -4 49.55 3.29 0 24 5 2.64 1.49 0 24 -5 2.47 1.49 0 -24 5 2.65 1.16 0 24 -6 16.56 2.50 0 24 6 13.76 2.43 0 -24 6 8.90 1.91 0 24 7 3.62 1.79 0 24 -7 2.61 1.52 0 -24 7 2.76 1.42 0 24 8 20.33 3.22 0 24 -8 21.16 3.00 0 -24 -8 21.34 2.62 0 -24 8 25.20 3.03 0 24 9 26.08 3.57 0 24 -9 21.50 3.16 0 -24 -9 20.84 2.69 0 -24 9 23.53 2.99 0 -24 -10 6.44 1.92 0 -24 10 5.45 1.92 0 25 0 -0.78 1.10 0 -25 0 0.99 1.02 0 25 1 119.68 7.02 0 25 -1 117.47 6.90 0 -25 -1 106.32 6.05 0 -25 1 95.05 6.00 0 25 -2 1.85 1.26 0 25 2 0.13 1.16 0 -25 2 1.22 0.96 0 -25 -2 1.31 0.98 0 25 3 57.65 4.40 0 25 -3 53.84 4.29 0 -25 3 57.97 3.97 0 -25 -3 57.53 3.67 0 25 -4 6.59 1.78 0 25 4 5.64 1.67 0 -25 4 10.41 1.85 0 25 -5 36.61 3.73 0 25 5 33.56 3.67 0 -25 5 34.48 3.39 0 25 6 1.41 1.60 0 25 -6 -0.10 1.33 0 -25 6 1.98 1.11 0 25 7 36.46 3.99 0 25 -7 27.76 3.50 0 -25 7 34.80 3.51 0 25 8 1.33 1.68 0 25 -8 1.05 1.51 0 -25 8 0.50 1.25 0 25 -9 24.01 3.13 0 25 9 13.71 2.82 0 -25 9 17.23 2.73 0 26 0 94.73 6.12 0 -26 0 87.56 5.30 0 26 -1 4.67 1.50 0 26 1 5.16 1.69 0 -26 -1 5.12 1.39 0 -26 1 6.50 1.49 0 26 -2 20.72 2.84 0 26 2 20.71 2.83 0 -26 2 21.77 2.58 0 -26 -2 27.74 2.63 0 26 3 1.83 1.39 0 26 -3 -0.82 1.19 0 -26 -3 0.99 1.01 0 -26 3 -0.14 1.01 0 26 4 43.19 3.91 0 26 -4 42.66 3.77 0 -26 4 47.35 3.61 0 26 -5 1.19 1.38 0 26 5 -0.53 1.28 0 -26 5 1.22 1.23 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2.15 0 -28 4 9.18 1.95 0 28 5 5.87 1.94 0 28 -5 3.48 1.63 0 -28 5 3.51 1.39 0 28 -6 0.88 1.58 0 28 6 -1.83 1.36 0 -28 6 2.10 1.33 0 28 7 3.48 1.96 0 28 -7 4.78 1.97 0 -28 7 6.68 1.85 0 28 -8 7.98 2.31 0 29 0 0.54 1.37 0 -29 0 -0.71 1.06 0 29 -1 39.54 3.72 0 29 1 41.08 3.68 0 -29 1 39.90 3.31 0 -29 -1 37.63 3.17 0 29 2 -1.22 1.15 0 29 -2 0.18 1.29 0 -29 2 1.77 1.26 0 -29 -2 -1.37 0.91 0 29 3 58.95 4.75 0 29 -3 57.26 4.68 0 -29 3 59.63 4.31 0 29 -4 2.38 1.65 0 29 4 2.95 1.65 0 -29 4 1.95 1.40 0 29 5 18.58 2.96 0 29 -5 22.02 3.09 0 -29 5 15.97 2.49 0 29 -6 1.34 1.63 0 29 6 3.26 1.77 0 -29 6 4.68 1.66 0 29 7 18.45 3.11 0 29 -7 18.88 2.98 0 -29 7 14.39 2.56 0 29 -8 0.65 1.81 0 30 0 69.33 5.16 0 -30 0 59.31 4.35 0 30 1 -0.12 1.35 0 30 -1 0.64 1.38 0 -30 1 0.61 1.20 0 -30 -1 0.44 1.18 0 30 -2 92.07 6.01 0 30 2 79.41 5.93 0 -30 -2 78.75 5.15 0 -30 2 80.36 5.36 0 30 -3 4.24 1.73 0 30 3 -0.13 1.43 0 -30 3 -0.74 1.08 0 30 4 45.07 4.40 0 30 -4 51.26 4.38 0 -30 4 54.37 4.14 0 30 -5 3.04 1.73 0 30 5 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2 6 8 85.90 5.33 -2 6 -8 82.37 4.79 2 -6 8 88.34 4.81 2 -6 8 89.99 5.24 -2 -6 -8 89.85 4.64 -2 6 -9 7.05 1.49 2 6 9 6.68 1.62 -2 6 -9 5.86 1.34 2 -6 9 9.24 1.57 2 -6 9 9.32 1.66 2 6 10 22.81 2.71 -2 6 -10 20.70 2.28 -2 -6 -10 22.50 2.62 2 -6 10 20.88 2.45 2 -6 11 12.66 1.99 -2 -6 -11 13.96 2.24 -2 -6 -12 11.31 2.24 -2 6 -13 6.57 2.00 -2 -6 -13 5.21 1.95 2 7 -13 -0.32 1.30 -2 7 13 0.77 1.78 2 -7 -13 3.90 1.68 -2 -7 13 0.13 1.90 2 7 -12 19.29 2.50 -2 7 12 15.87 2.84 2 -7 -12 15.65 2.46 -2 -7 12 19.97 3.06 -2 7 11 0.10 1.44 2 7 -11 -0.32 1.13 2 -7 -11 0.34 1.20 -2 -7 11 1.05 1.64 2 7 -10 58.91 3.84 -2 7 10 63.06 4.69 2 -7 -10 61.62 4.13 -2 -7 10 57.91 4.55 -2 7 9 1.09 1.20 2 7 -9 2.80 1.03 -2 -7 9 1.97 1.36 -2 -7 9 0.45 0.81 2 -7 -9 4.04 1.20 2 7 -8 28.33 2.26 -2 7 8 33.40 2.83 -2 -7 8 32.16 2.87 2 -7 -8 27.19 2.65 -2 -7 8 28.60 2.12 -2 7 7 1.53 1.11 2 7 -7 3.12 0.84 2 -7 -7 1.45 0.94 -2 -7 7 0.57 1.08 -2 -7 7 2.50 0.82 -2 7 6 68.16 4.45 2 7 -6 66.45 3.66 2 -7 -6 74.53 4.03 -2 -7 6 74.04 4.52 -2 -7 6 69.91 3.81 -2 7 5 30.61 2.42 2 7 -5 30.24 1.89 -2 -7 5 27.92 2.38 -2 -7 5 30.56 2.01 2 -7 -5 30.37 2.15 -2 7 4 51.01 3.39 2 7 -4 54.63 2.75 -2 -7 4 48.35 3.34 -2 -7 4 56.17 2.99 2 -7 -4 57.53 3.08 -2 7 3 29.40 2.09 2 7 -3 26.83 1.52 -2 -7 3 25.09 1.76 2 -7 -3 26.38 1.35 2 -7 -3 25.55 1.82 -2 -7 3 26.14 2.05 2 7 -2 107.26 4.69 2 7 -2 115.35 5.75 -2 7 2 91.12 5.58 2 -7 -2 106.95 5.03 -2 -7 2 105.34 5.14 2 -7 -2 107.38 4.85 2 7 -1 17.20 1.65 -2 7 1 22.43 1.61 -2 -7 1 21.05 1.52 2 -7 -1 19.91 1.26 2 -7 -1 20.44 1.39 2 7 0 84.41 3.64 -2 7 0 71.04 4.35 2 7 0 86.39 4.47 2 -7 0 87.22 4.00 -2 -7 0 84.89 4.09 2 -7 0 78.92 3.90 2 7 1 349.35 14.64 -2 7 -1 294.94 16.51 2 7 1 344.54 16.66 -2 -7 -1 360.83 15.23 2 -7 1 335.87 14.76 2 7 2 45.27 2.80 -2 7 -2 45.80 2.67 2 7 2 46.87 2.40 -2 -7 -2 46.06 2.57 2 -7 2 46.56 2.57 2 -7 2 46.01 2.42 -2 7 -3 47.70 2.87 2 7 3 50.27 2.66 2 7 3 45.36 2.97 2 -7 3 53.49 2.82 -2 -7 -3 50.06 2.75 2 -7 3 50.82 2.62 2 7 4 29.59 2.19 -2 7 -4 29.85 2.04 2 7 4 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11 0 76.14 4.73 2 -11 0 85.61 4.23 -2 -11 0 79.38 4.28 2 -11 0 85.80 4.05 -2 -11 0 87.67 3.73 2 11 1 139.95 7.24 -2 11 -1 129.31 7.11 -2 -11 -1 138.03 6.10 2 -11 1 138.81 6.59 -2 -11 -1 142.26 6.61 2 -11 1 126.38 6.21 -2 11 -2 1.17 0.65 2 11 2 1.35 0.76 2 -11 2 1.00 0.52 2 -11 2 1.99 0.66 -2 -11 -2 0.32 0.47 -2 -11 -2 0.78 0.67 2 11 3 21.33 1.92 -2 11 -3 23.04 1.79 -2 -11 -3 23.18 1.70 2 -11 3 20.02 1.73 2 -11 3 23.87 1.54 2 11 4 2.81 0.96 -2 11 -4 1.55 0.66 2 -11 4 1.13 0.66 2 -11 4 2.18 0.62 -2 -11 -4 2.06 0.74 2 11 5 102.77 5.95 -2 11 -5 104.61 5.77 2 -11 5 108.14 5.51 -2 -11 -5 103.58 5.21 2 -11 5 98.25 5.07 -2 11 -6 0.55 0.73 2 11 6 0.43 0.88 -2 -11 -6 0.90 0.75 -2 -11 -6 -1.16 0.69 2 -11 6 0.23 0.67 2 -11 6 0.44 0.74 2 11 7 106.32 6.69 -2 11 -7 119.03 6.59 2 -11 7 114.55 6.16 -2 -11 -7 119.44 6.16 2 -11 7 110.52 5.81 -2 -11 -7 119.98 5.83 -2 11 -8 5.42 1.33 2 11 8 1.44 1.16 -2 -11 -8 3.04 1.24 2 -11 8 4.84 1.25 2 -11 8 4.08 1.08 -2 11 -9 54.11 3.97 -2 11 -9 54.84 3.86 2 11 9 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2.52 2 -15 -2 31.06 2.08 2 -15 -2 31.09 2.05 -2 -15 2 31.73 2.27 2 15 -1 273.15 14.98 2 -15 -1 308.25 13.49 2 -15 -1 286.70 13.06 -2 -15 1 299.62 13.69 2 15 0 15.23 1.78 -2 15 0 15.20 1.69 -2 -15 0 11.83 0.80 2 -15 0 15.51 1.29 -2 -15 0 17.01 1.68 2 -15 0 11.55 1.31 2 15 1 155.98 8.17 -2 15 -1 122.63 7.89 -2 -15 -1 153.96 6.72 2 -15 1 157.90 6.90 -2 -15 -1 149.05 7.35 2 -15 1 153.85 7.37 -2 15 -2 10.95 1.47 2 15 2 10.62 1.58 -2 -15 -2 10.76 1.36 2 -15 2 12.59 1.10 2 -15 2 10.81 1.37 -2 -15 -2 11.02 1.08 2 15 3 50.95 3.49 -2 15 -3 51.80 3.43 2 -15 3 48.34 2.70 2 -15 3 51.96 3.20 -2 -15 -3 56.00 3.14 -2 -15 -3 49.98 2.85 2 15 4 0.28 0.88 -2 15 -4 0.35 0.75 -2 -15 -4 1.45 0.76 -2 -15 -4 1.44 0.74 2 -15 4 1.71 0.82 2 -15 4 1.51 0.62 -2 15 -5 142.03 7.68 2 15 5 138.55 7.88 2 -15 5 134.41 6.58 2 -15 5 137.54 7.22 -2 -15 -5 139.09 6.88 -2 -15 -5 138.90 6.87 2 15 6 5.55 1.57 -2 15 -6 6.20 1.28 2 -15 6 6.55 1.37 -2 -15 -6 7.11 1.34 2 -15 6 8.16 1.18 -2 -15 -6 5.52 1.13 -2 15 -7 62.76 4.14 2 15 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8 24.40 2.50 4 -6 8 27.78 2.58 -4 -6 -8 28.00 2.29 4 6 9 2.08 1.20 -4 6 -9 0.38 1.08 4 -6 9 -0.02 0.92 -4 -6 -9 1.81 1.17 -4 6 -10 28.73 2.89 4 6 10 26.53 2.86 4 -6 10 25.37 2.77 4 6 11 0.30 1.24 4 -6 11 3.77 1.53 4 -6 12 11.14 2.23 -4 -6 -12 9.96 2.20 4 -6 13 0.52 1.47 -4 7 13 1.90 2.01 -4 -7 13 -0.54 1.86 -4 7 12 31.71 4.07 4 7 -12 41.78 3.29 -4 -7 12 43.50 4.51 4 -7 -12 38.58 3.85 -4 7 11 1.21 1.51 4 7 -11 0.83 1.23 -4 -7 11 0.40 1.58 4 -7 -11 0.76 1.25 -4 7 10 49.99 4.14 4 7 -10 49.61 3.39 -4 -7 10 43.10 4.02 4 -7 -10 46.39 3.57 -4 7 9 3.09 1.53 4 7 -9 2.26 1.01 4 -7 -9 1.21 1.17 -4 -7 9 2.45 1.57 4 7 -8 60.76 3.71 -4 7 8 64.28 4.63 -4 -7 8 69.86 4.73 4 -7 -8 71.40 4.20 -4 -7 8 60.63 3.62 -4 7 7 42.95 3.59 4 7 -7 49.10 2.95 4 -7 -7 55.93 3.37 -4 -7 7 46.35 3.59 -4 -7 7 47.09 2.90 4 7 -6 236.13 10.68 -4 7 6 248.29 12.45 4 -7 -6 236.31 11.02 -4 -7 6 212.83 12.32 -4 -7 6 231.18 10.92 -4 7 5 5.67 1.28 4 7 -5 5.31 0.84 -4 -7 5 6.30 0.98 4 -7 -5 5.95 1.06 -4 -7 5 5.05 1.18 -4 7 4 262.12 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14.43 2.04 5 6 -6 16.92 1.63 -5 -6 6 17.73 2.18 5 -6 -6 14.63 1.74 -5 -6 6 18.48 1.50 5 6 -5 86.59 4.24 -5 6 5 80.88 5.03 -5 -6 5 88.02 5.17 -5 -6 5 82.14 4.31 5 -6 -5 78.37 4.46 -5 6 4 24.18 2.20 5 6 -4 23.51 1.71 -5 -6 4 30.84 2.41 -5 -6 4 31.11 1.95 5 -6 -4 27.33 1.97 -5 6 3 34.30 2.43 -5 6 3 34.37 1.85 5 6 -3 35.69 1.99 5 -6 -3 29.44 2.21 -5 -6 3 32.41 2.47 -5 -6 3 36.80 2.19 5 6 -2 0.49 0.53 -5 6 2 0.82 0.70 -5 6 2 1.91 0.54 -5 -6 2 0.64 0.75 5 -6 -2 0.10 0.61 -5 -6 2 0.62 0.57 -5 6 1 190.92 10.29 5 6 -1 205.61 9.10 -5 6 1 208.71 9.39 5 6 -1 203.32 10.43 5 -6 -1 206.92 9.38 -5 -6 1 207.66 9.58 5 6 0 120.15 5.44 -5 6 0 121.15 6.08 5 6 0 120.36 6.23 -5 6 0 116.45 5.70 -5 6 0 117.51 5.78 5 -6 0 114.92 5.69 -5 -6 0 110.50 5.80 5 6 1 4.87 0.86 -5 6 -1 4.41 0.86 5 6 1 4.62 0.73 -5 6 -1 5.31 0.94 -5 6 -1 5.40 0.68 5 -6 1 3.97 0.83 -5 -6 -1 3.30 0.92 5 6 2 112.30 5.24 -5 6 -2 107.61 5.59 -5 6 -2 112.59 5.49 -5 6 -2 107.74 5.51 5 6 2 107.78 5.74 -5 -6 -2 106.59 5.56 5 -6 2 109.20 5.34 -5 6 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6.17 1.44 5 -7 8 7.21 1.49 -5 7 -9 -0.75 1.12 5 7 9 -0.68 1.05 5 -7 9 1.25 1.06 -5 -7 -9 -0.91 1.05 5 7 10 2.67 1.36 -5 7 -10 -1.12 1.06 5 -7 10 -1.24 1.06 5 7 11 7.93 1.88 -5 7 -11 2.33 1.55 5 -7 11 7.22 1.87 5 -7 12 -2.46 1.30 -5 8 12 1.49 1.86 5 -8 -12 -1.07 1.23 -5 -8 12 -0.12 1.79 -5 8 11 26.65 3.43 5 -8 -11 24.06 2.91 -5 -8 11 23.95 3.25 -5 8 10 1.61 1.37 -5 -8 10 0.34 1.59 5 -8 -10 1.47 1.28 5 8 -9 12.70 1.74 -5 8 9 10.05 2.11 5 -8 -9 8.21 1.75 -5 -8 9 12.70 2.37 -5 8 8 6.41 1.65 5 8 -8 12.47 1.58 -5 -8 8 7.48 1.91 5 -8 -8 11.74 1.80 -5 -8 8 11.96 1.48 5 8 -7 93.47 4.67 -5 8 7 86.04 5.67 -5 -8 7 88.08 4.69 5 -8 -7 84.33 4.97 -5 -8 7 85.30 5.63 -5 8 6 0.77 1.00 5 8 -6 0.32 0.62 -5 -8 6 -0.56 0.59 5 -8 -6 -0.12 0.82 -5 -8 6 1.03 1.08 5 8 -5 309.18 13.55 -5 8 5 300.74 15.65 -5 -8 5 308.21 15.74 -5 -8 5 290.80 13.98 5 -8 -5 302.84 13.92 5 8 -4 4.76 0.73 -5 8 4 6.22 1.23 -5 8 4 3.87 0.42 5 -8 -4 3.73 0.98 -5 -8 4 3.00 1.13 -5 -8 4 5.20 0.95 5 8 -3 65.19 3.17 -5 8 3 63.95 3.12 -5 8 3 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41.06 2.91 5 8 5 42.73 2.75 5 8 5 42.94 2.68 -5 8 -5 39.19 2.83 -5 8 -5 37.81 2.43 5 -8 5 42.89 2.66 -5 -8 -5 40.20 2.76 5 8 6 -0.54 0.71 -5 8 -6 -0.21 0.86 -5 8 -6 0.34 0.87 5 8 6 0.72 0.83 -5 8 -6 0.07 0.56 -5 -8 -6 1.44 0.96 5 -8 6 -0.46 0.70 -5 8 -7 21.52 2.40 5 8 7 21.59 2.19 -5 8 -7 23.27 2.44 5 8 7 22.58 2.28 5 -8 7 20.74 2.16 -5 -8 -7 21.44 2.23 -5 8 -8 36.67 3.03 -5 8 -8 35.92 2.92 5 8 8 37.65 2.85 -5 -8 -8 32.75 2.69 5 -8 8 30.12 2.63 -5 8 -9 11.65 1.95 5 8 9 13.28 2.03 5 -8 9 9.66 1.72 -5 -8 -9 10.92 1.77 5 8 10 1.94 1.36 -5 8 -10 2.87 1.44 5 -8 10 4.09 1.47 -5 8 -11 -0.33 1.34 5 8 11 -0.47 1.27 5 -8 11 -0.94 1.20 5 -8 12 1.73 1.47 -5 9 12 8.09 2.35 5 -9 -12 4.06 1.76 -5 -9 12 8.28 2.60 -5 9 11 4.10 1.77 -5 -9 11 5.23 2.16 5 -9 -11 4.00 1.63 -5 9 10 33.70 3.66 5 -9 -10 26.91 2.99 -5 -9 10 24.88 3.39 5 9 -9 0.92 0.97 -5 9 9 0.63 1.28 -5 -9 9 0.64 1.40 5 -9 -9 -0.12 1.00 -5 9 8 5.90 1.72 5 9 -8 11.42 1.54 5 -9 -8 6.54 1.45 -5 -9 8 14.06 2.31 -5 -9 8 12.68 1.56 5 9 -7 12.72 1.42 -5 9 7 10.80 1.91 -5 -9 7 10.09 1.38 5 -9 -7 7.83 1.49 -5 -9 7 8.65 1.86 -5 9 6 133.62 7.83 5 9 -6 139.05 6.59 -5 -9 6 143.39 6.90 5 -9 -6 137.42 6.99 -5 -9 6 128.98 7.85 5 9 -5 1.82 0.61 -5 9 5 0.75 0.94 -5 -9 5 -1.22 0.81 5 -9 -5 1.56 0.89 -5 -9 5 0.48 0.65 5 9 -4 81.30 4.03 -5 9 4 88.61 5.03 -5 -9 4 81.63 4.41 5 -9 -4 78.51 4.41 -5 -9 4 86.23 5.11 -5 9 3 31.85 2.37 5 9 -3 29.49 2.43 5 9 -3 28.85 1.73 -5 9 3 28.13 1.68 -5 -9 3 30.31 2.11 5 -9 -3 30.86 2.17 5 9 -2 43.91 3.01 5 9 -2 43.72 2.29 -5 9 2 52.62 3.07 -5 9 2 47.06 2.53 -5 9 2 46.79 2.49 -5 -9 2 41.73 2.70 5 -9 -2 43.20 2.72 -5 9 1 52.40 3.39 5 9 -1 58.80 2.79 5 9 -1 60.20 3.57 -5 9 1 58.83 3.08 -5 9 1 57.96 3.13 -5 -9 1 60.61 3.36 5 -9 -1 55.36 3.20 -5 9 0 146.61 7.89 5 9 0 156.67 6.90 -5 9 0 155.35 7.35 5 9 0 153.25 8.09 -5 9 0 151.76 7.42 -5 -9 0 159.52 7.54 5 -9 0 151.55 7.28 5 9 1 34.93 2.36 -5 9 -1 32.07 2.04 5 9 1 30.42 1.81 -5 -9 -1 34.06 2.27 5 -9 1 29.03 2.09 -5 9 -2 148.78 7.05 5 9 2 140.84 6.52 5 9 2 140.33 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0.32 1.50 -5 10 12 5.36 2.16 5 -10 -12 5.25 1.91 -5 -10 12 3.33 2.10 -5 10 11 2.04 1.58 5 -10 -11 -0.29 1.26 -5 -10 11 0.31 1.74 -5 10 10 8.75 2.20 -5 -10 10 5.79 2.16 5 -10 -10 4.82 1.50 -5 10 9 0.89 1.41 -5 -10 9 -0.55 1.14 5 -10 -9 -0.34 1.09 -5 10 8 8.14 1.89 5 10 -8 4.87 1.13 -5 -10 8 6.14 1.23 5 -10 -8 5.91 1.44 -5 -10 8 4.49 1.78 -5 10 7 0.33 1.15 5 10 -7 0.91 0.67 5 -10 -7 0.56 0.98 -5 -10 7 -0.01 1.08 -5 -10 7 1.71 0.88 5 10 -6 5.49 0.96 -5 10 6 4.62 1.32 5 -10 -6 5.24 1.22 -5 -10 6 7.22 1.21 -5 -10 6 3.57 1.29 -5 10 5 4.36 1.23 5 10 -5 3.94 0.77 -5 -10 5 2.92 0.93 -5 -10 5 3.93 1.29 5 -10 -5 3.26 1.08 -5 10 4 37.96 1.97 5 10 -4 40.16 2.15 -5 10 4 43.41 2.95 5 -10 -4 37.58 2.60 -5 -10 4 34.34 2.47 -5 10 3 2.61 0.56 5 10 -3 3.44 1.05 -5 10 3 2.49 0.92 -5 10 3 2.23 0.56 5 10 -3 3.29 0.56 5 -10 -3 1.88 0.87 -5 -10 3 1.82 0.78 -5 10 2 108.30 5.24 5 10 -2 106.86 4.88 5 10 -2 102.07 6.03 -5 10 2 105.75 5.17 -5 10 2 125.45 6.09 -5 -10 2 99.94 5.45 5 -10 -2 104.75 5.38 5 10 -1 5.85 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5 30.48 2.21 -5 11 -5 30.20 2.45 -5 -11 -5 31.16 2.40 5 -11 5 27.61 2.13 5 11 6 -0.35 0.85 5 11 6 1.55 0.92 -5 11 -6 -0.43 0.93 -5 11 -6 0.48 0.99 -5 -11 -6 1.94 1.04 5 -11 6 1.41 0.90 5 11 7 74.81 4.72 -5 11 -7 67.53 4.63 -5 11 -7 79.99 4.74 5 11 7 73.72 4.44 5 -11 7 81.63 4.45 -5 -11 -7 73.14 4.44 5 11 8 0.73 1.04 5 11 8 0.87 1.05 -5 11 -8 2.44 1.33 -5 11 -8 2.25 1.24 5 -11 8 0.17 0.99 -5 -11 -8 0.08 1.12 -5 11 -9 31.82 3.28 5 11 9 32.26 3.17 -5 11 -9 35.87 3.36 5 -11 9 34.35 2.86 5 11 10 2.14 1.44 -5 11 -10 -0.32 1.24 5 -11 10 0.87 1.15 -5 11 -11 27.51 3.25 5 -11 11 32.31 3.27 -5 -11 -11 30.96 3.36 -5 -11 -12 3.89 1.82 5 -11 12 1.05 1.64 -5 12 12 -1.67 1.64 5 -12 -12 -0.30 1.43 -5 -12 12 -1.29 1.90 -5 12 11 26.23 3.63 5 -12 -11 30.03 3.29 -5 -12 11 33.88 4.04 -5 12 10 7.16 2.14 5 -12 -10 5.35 1.59 -5 -12 10 2.97 1.85 -5 12 9 41.84 3.86 5 -12 -9 43.62 3.39 -5 -12 9 40.64 4.24 -5 12 8 2.77 1.33 -5 -12 8 1.66 0.95 -5 -12 8 1.16 1.47 5 -12 -8 3.07 1.27 -5 12 7 115.36 7.22 -5 -12 7 120.95 6.30 -5 12 6 26.84 2.93 5 -12 -6 24.73 2.48 -5 -12 6 30.72 2.29 5 12 -5 135.87 6.35 5 12 -5 134.56 7.90 -5 12 5 147.77 7.93 5 -12 -5 128.59 6.91 -5 -12 5 138.52 7.00 5 12 -4 14.14 1.86 -5 12 4 14.47 1.87 5 12 -4 13.14 1.04 5 -12 -4 10.19 1.51 -5 -12 4 12.48 1.57 5 12 -3 46.99 3.53 5 12 -3 58.32 2.64 -5 12 3 53.08 3.62 5 -12 -3 54.20 3.24 -5 -12 3 54.78 3.29 5 12 -2 15.47 0.94 -5 12 2 17.73 1.86 5 12 -2 16.02 1.87 -5 -12 2 16.62 1.72 5 -12 -2 15.98 1.66 5 -12 -2 16.38 1.25 5 12 -1 84.08 3.62 -5 12 1 71.34 4.55 5 12 -1 83.24 4.78 5 -12 -1 77.90 4.09 -5 -12 1 84.10 4.41 5 -12 -1 74.93 4.17 5 12 0 21.83 1.26 -5 12 0 18.55 1.71 5 12 0 21.23 1.95 5 -12 0 23.50 1.77 -5 -12 0 24.88 2.14 5 -12 0 20.03 1.61 5 12 1 89.70 5.27 -5 12 -1 88.20 5.05 5 12 1 92.04 4.34 5 -12 1 99.09 4.87 5 -12 1 84.24 4.69 -5 -12 -1 102.03 5.01 5 12 2 6.91 1.19 5 12 2 4.45 0.76 -5 12 -2 4.87 0.92 5 -12 2 5.14 1.03 -5 -12 -2 4.44 1.10 5 -12 2 5.76 1.01 -5 12 -3 23.40 1.80 5 12 3 25.67 1.76 5 12 3 25.84 2.12 -5 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3.44 5 13 -7 7.74 1.80 -5 13 7 14.05 2.21 -5 -13 7 14.35 1.77 5 -13 -7 14.53 1.93 -5 13 6 115.69 6.82 5 13 -6 101.85 6.77 5 -13 -6 110.50 5.99 -5 -13 6 115.41 5.99 -5 13 5 24.19 2.72 5 13 -5 26.77 2.89 5 -13 -5 29.78 2.35 -5 -13 5 25.44 2.38 5 13 -4 30.47 2.74 -5 13 4 32.58 2.63 -5 -13 4 30.42 2.35 5 -13 -4 32.14 2.36 5 13 -3 1.02 0.91 5 13 -3 0.33 0.31 -5 13 3 0.16 0.77 5 -13 -3 -0.57 0.42 -5 -13 3 -0.64 0.66 5 -13 -3 0.09 0.77 5 13 -2 51.81 3.48 -5 13 2 51.17 3.40 5 -13 -2 51.47 3.07 5 -13 -2 49.90 2.77 -5 -13 2 48.41 3.16 -5 13 1 2.13 0.89 5 13 -1 4.54 1.07 5 13 -1 5.40 0.46 5 -13 -1 4.80 0.85 -5 -13 1 7.41 1.24 5 -13 -1 3.16 0.92 5 13 0 161.26 7.34 -5 13 0 176.68 8.74 5 13 0 164.34 8.90 -5 -13 0 166.49 8.20 5 -13 0 163.90 7.88 5 -13 0 161.76 7.97 5 13 1 18.46 1.28 5 13 1 21.46 1.94 -5 13 -1 21.66 1.75 5 -13 1 19.31 1.78 -5 -13 -1 25.85 2.01 5 -13 1 18.12 1.60 -5 13 -2 59.94 3.52 5 13 2 57.28 3.76 5 13 2 61.25 3.06 5 -13 2 59.81 3.47 5 -13 2 52.67 3.26 -5 -13 -2 62.61 3.64 5 13 3 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2.04 1.79 5 -15 -10 1.61 1.45 5 15 -9 16.85 2.75 -5 15 9 16.79 2.76 -5 -15 9 15.06 2.08 5 -15 -9 19.37 2.47 -5 15 8 13.38 2.35 5 15 -8 9.83 2.19 5 -15 -8 7.53 1.74 -5 -15 8 14.33 1.93 -5 15 7 4.32 1.60 5 15 -7 5.84 1.72 -5 -15 7 3.33 1.18 5 -15 -7 3.54 1.34 5 15 -6 2.74 1.32 -5 15 6 0.66 1.22 -5 -15 6 1.22 0.96 5 -15 -6 1.03 1.05 -5 15 5 2.34 1.30 5 15 -5 2.48 1.22 -5 -15 5 5.17 1.16 5 -15 -5 2.21 1.08 5 15 -4 4.80 1.32 -5 15 4 4.02 1.26 -5 -15 4 3.95 1.12 5 -15 -4 3.35 1.09 5 15 -3 16.63 2.13 -5 15 3 21.59 2.25 5 -15 -3 18.30 1.89 5 -15 -3 17.35 1.37 -5 -15 3 18.74 1.95 -5 15 2 -0.09 0.78 5 15 -2 -0.47 0.82 5 -15 -2 0.64 0.58 -5 -15 2 -1.27 0.62 5 -15 -2 -0.18 0.77 -5 15 1 36.04 2.71 5 15 -1 39.49 2.94 5 -15 -1 35.53 2.47 -5 -15 1 39.10 2.72 5 -15 -1 35.88 2.34 5 15 0 1.66 0.38 -5 15 0 2.59 0.86 5 15 0 1.03 0.94 5 -15 0 0.61 0.78 5 -15 0 1.29 0.70 -5 -15 0 1.13 0.90 5 15 1 20.95 1.38 -5 15 -1 23.44 1.96 5 15 1 23.84 2.09 5 -15 1 23.95 1.90 -5 -15 -1 26.40 2.32 5 -15 1 20.72 1.91 5 15 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2.46 5 16 -11 9.32 2.52 5 -16 -11 5.44 1.88 5 16 -10 16.77 2.95 -5 16 10 15.41 2.79 5 -16 -10 13.47 2.26 5 16 -9 38.45 4.09 -5 -16 9 39.81 3.09 5 -16 -9 33.59 3.41 5 16 -8 5.22 1.87 -5 16 8 7.84 2.00 -5 -16 8 6.95 1.54 5 -16 -8 8.36 1.79 5 16 -7 14.83 2.44 -5 16 7 16.36 2.49 5 -16 -7 15.55 2.11 -5 -16 7 16.12 2.06 -5 16 6 -1.49 1.04 5 16 -6 -1.27 1.04 -5 -16 6 1.15 0.96 5 -16 -6 2.57 1.11 5 16 -5 21.54 2.62 -5 16 5 22.43 2.60 5 -16 -5 27.08 2.47 -5 -16 5 20.64 2.29 -5 16 4 9.15 1.72 5 16 -4 8.93 1.71 -5 -16 4 7.18 1.37 5 -16 -4 9.40 1.51 5 16 -3 45.25 3.49 -5 16 3 53.46 3.57 5 -16 -3 43.73 2.97 -5 -16 3 44.05 3.14 5 -16 -3 46.73 2.65 -5 16 2 41.38 3.07 5 16 -2 40.34 3.17 5 -16 -2 41.97 2.49 -5 -16 2 39.41 2.85 5 -16 -2 41.65 2.78 5 16 -1 23.96 2.51 -5 16 1 25.07 2.22 5 -16 -1 24.30 1.83 -5 -16 1 26.15 2.16 5 -16 -1 28.93 2.05 -5 16 0 38.84 2.60 5 16 0 31.93 2.66 5 -16 0 31.87 2.25 5 -16 0 34.08 2.34 -5 -16 0 28.65 2.45 5 16 1 20.12 1.31 5 16 1 20.02 2.25 -5 16 -1 23.47 1.97 -5 -16 -1 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1.15 -7 8 8 4.04 1.64 -7 -8 8 3.03 1.59 7 -8 -8 3.95 1.39 7 8 -7 54.04 3.32 -7 8 7 52.70 4.08 7 -8 -7 56.35 3.72 -7 -8 7 56.80 3.33 -7 -8 7 52.71 4.18 7 8 -6 2.42 0.87 -7 8 6 1.95 1.24 -7 -8 6 2.70 1.26 -7 -8 6 1.68 0.83 7 -8 -6 2.48 1.14 7 8 -5 191.78 8.97 -7 8 5 190.93 10.48 7 -8 -5 194.13 9.36 -7 -8 5 188.41 9.26 -7 -8 5 196.93 10.61 -7 8 4 28.65 2.41 7 8 -4 26.82 1.89 -7 -8 4 27.35 2.45 7 -8 -4 23.60 2.27 -7 -8 4 24.84 2.01 -7 8 3 173.14 7.84 -7 8 3 165.74 8.96 7 8 -3 168.28 7.74 7 -8 -3 159.19 8.11 -7 -8 3 166.60 9.11 -7 -8 3 167.10 8.17 -7 8 2 9.07 1.34 7 8 -2 11.90 1.16 -7 8 2 11.49 1.19 7 8 -2 7.91 1.36 7 -8 -2 9.12 1.38 -7 -8 2 9.03 1.34 -7 8 1 108.82 5.52 -7 8 1 115.68 6.03 7 8 -1 110.64 6.13 7 8 -1 109.21 5.26 7 -8 -1 109.22 5.61 -7 -8 1 108.77 5.75 -7 8 0 3.32 0.89 7 8 0 3.78 0.96 -7 8 0 4.22 0.85 7 8 0 5.97 0.84 7 -8 0 4.21 1.01 -7 -8 0 5.21 1.09 -7 8 -1 145.81 7.11 -7 8 -1 137.96 7.28 7 8 1 145.77 7.56 7 8 1 146.58 6.71 -7 -8 -1 134.89 7.19 7 -8 1 144.28 7.01 -7 8 -2 0.64 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2.34 1.73 7 -10 11 -1.17 1.32 -7 10 -12 12.40 2.55 7 -10 12 15.62 2.59 -7 11 11 8.12 2.12 7 -11 -11 7.12 1.97 -7 -11 11 4.73 2.04 -7 11 10 13.93 2.56 7 -11 -10 9.71 2.04 -7 -11 10 12.03 2.59 -7 11 9 12.50 2.41 -7 -11 9 18.39 2.89 7 -11 -9 19.88 2.52 -7 11 8 12.75 2.29 7 -11 -8 14.27 2.06 -7 -11 8 13.06 2.31 -7 11 7 5.62 1.66 -7 -11 7 10.47 2.03 -7 -11 7 8.17 1.40 7 -11 -7 5.34 1.44 -7 11 6 52.22 4.05 -7 -11 6 57.10 3.46 -7 -11 6 49.39 4.08 7 -11 -6 57.78 3.68 7 11 -5 0.46 0.64 -7 11 5 1.34 1.03 -7 -11 5 1.01 0.81 7 -11 -5 1.65 1.03 7 11 -4 44.66 2.38 7 11 -4 42.52 3.30 -7 11 4 33.38 3.00 -7 -11 4 42.11 2.81 7 -11 -4 40.50 2.90 7 11 -3 39.32 2.96 7 11 -3 36.23 2.15 -7 11 3 39.49 2.31 -7 11 3 37.21 2.86 7 -11 -3 39.80 2.76 -7 -11 3 36.69 2.65 -7 11 2 120.49 5.85 7 11 -2 115.38 6.70 -7 11 2 115.74 6.59 7 11 -2 117.04 5.51 -7 -11 2 119.89 6.20 7 -11 -2 122.11 6.11 7 11 -1 30.01 2.50 -7 11 1 29.64 2.30 7 11 -1 28.47 1.81 -7 11 1 32.73 2.20 -7 11 1 31.85 2.16 -7 -11 1 32.42 2.44 7 -11 -1 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1.60 -8 7 5 12.23 1.93 8 -7 -5 12.06 1.77 -8 -7 5 13.72 2.08 -8 -7 5 15.43 1.63 -8 7 4 26.68 2.37 8 7 -4 24.72 1.89 -8 -7 4 20.66 2.46 8 -7 -4 25.18 2.30 -8 -7 4 23.49 1.94 -8 7 3 0.32 0.82 8 7 -3 -0.76 0.60 -8 7 3 1.43 0.67 -8 -7 3 0.70 0.95 -8 -7 3 0.51 0.74 8 -7 -3 1.06 0.89 8 7 -2 125.60 6.86 8 7 -2 123.68 5.93 -8 7 2 126.90 6.78 -8 7 2 127.71 6.12 -8 -7 2 114.37 6.28 8 -7 -2 118.03 6.21 -8 7 1 4.53 1.01 -8 7 1 3.33 0.90 8 7 -1 5.06 0.91 8 7 -1 5.64 1.11 -8 -7 1 5.38 1.07 8 -7 -1 4.90 1.12 -8 7 0 141.84 6.80 8 7 0 135.45 6.45 -8 7 0 141.18 7.08 8 7 0 131.75 7.22 8 -7 0 123.89 6.68 -8 -7 0 134.66 6.95 8 7 1 0.68 0.61 -8 7 -1 0.66 0.83 8 7 1 0.99 0.69 -8 7 -1 1.05 0.54 8 -7 1 0.48 0.81 -8 -7 -1 1.56 0.96 8 7 2 78.17 4.57 -8 7 -2 85.05 4.62 8 7 2 80.44 4.30 -8 -7 -2 86.89 4.75 8 -7 2 84.42 4.56 8 7 3 5.03 1.01 8 7 3 5.89 0.93 -8 7 -3 3.64 1.11 -8 -7 -3 6.32 1.37 8 -7 3 2.29 1.00 -8 7 -4 81.89 4.88 8 7 4 87.87 4.66 8 7 4 83.12 4.65 8 -7 4 83.47 4.69 -8 -7 -4 90.48 4.97 -8 7 -5 10.13 1.77 8 7 5 12.74 1.67 8 -7 5 13.05 1.70 -8 -7 -5 9.80 1.76 8 7 6 64.12 3.96 -8 7 -6 65.41 4.23 8 -7 6 65.59 4.03 -8 -7 -6 63.35 4.22 -8 7 -7 1.72 1.33 8 7 7 1.84 1.17 8 -7 7 5.15 1.39 -8 -7 -7 2.87 1.40 -8 7 -8 3.33 1.58 8 7 8 5.43 1.51 -8 -7 -8 5.02 1.61 8 -7 8 2.94 1.38 -8 7 -9 3.31 1.59 8 7 9 4.84 1.55 -8 -7 -9 4.70 1.64 8 -7 9 5.28 1.58 -8 7 -10 4.99 1.86 8 7 10 9.22 2.02 8 -7 10 13.26 2.22 8 7 11 2.17 1.66 -8 7 -11 2.93 1.71 8 -7 11 0.28 1.39 -8 7 -12 -1.07 1.68 -8 8 11 8.35 2.33 8 -8 -11 4.71 1.65 -8 -8 11 3.37 2.12 -8 8 10 3.23 1.72 8 -8 -10 2.88 1.46 -8 -8 10 2.40 1.76 -8 8 9 14.86 2.57 8 -8 -9 12.54 2.00 -8 -8 9 11.48 2.47 8 8 -8 -0.95 0.91 -8 8 8 0.23 1.30 8 -8 -8 0.47 1.04 -8 -8 8 -0.62 1.33 8 8 -7 70.39 3.74 -8 8 7 60.74 4.50 -8 -8 7 51.77 4.43 8 -8 -7 56.53 3.90 8 8 -6 0.83 0.89 -8 8 6 1.30 1.16 -8 -8 6 0.23 1.23 -8 -8 6 -0.62 0.67 8 -8 -6 1.30 1.04 8 8 -5 112.23 5.32 -8 8 5 98.92 6.24 -8 -8 5 104.19 5.46 -8 -8 5 100.66 6.29 8 -8 -5 95.46 5.58 8 8 -4 7.20 1.12 -8 8 4 6.22 1.37 -8 -8 4 6.07 1.41 -8 -8 4 6.06 1.15 8 -8 -4 6.18 1.35 8 8 -3 36.16 2.24 -8 8 3 37.35 2.22 -8 8 3 35.17 2.68 -8 -8 3 27.42 2.35 8 -8 -3 35.92 2.62 -8 8 2 1.81 0.92 8 8 -2 0.93 0.88 -8 8 2 1.97 0.78 8 8 -2 1.26 0.69 -8 -8 2 2.57 0.99 8 -8 -2 4.00 1.04 -8 8 1 167.75 8.64 -8 8 1 159.39 7.97 8 8 -1 163.49 8.77 8 8 -1 159.40 7.64 8 -8 -1 170.21 8.07 -8 -8 1 168.09 8.25 -8 8 0 45.67 3.01 -8 8 0 51.50 2.99 8 8 0 49.61 2.76 8 8 0 48.76 3.20 -8 -8 0 44.18 3.15 8 -8 0 50.97 3.12 -8 8 -1 69.42 3.82 8 8 1 67.66 4.08 8 8 1 69.84 3.69 -8 8 -1 69.27 3.98 -8 -8 -1 70.50 4.19 8 -8 1 72.46 4.03 -8 8 -2 10.94 1.53 -8 8 -2 13.45 1.05 8 8 2 13.10 1.42 8 8 2 14.05 1.46 -8 -8 -2 12.39 1.70 8 -8 2 14.46 1.69 8 8 3 63.09 3.68 -8 8 -3 64.47 4.03 8 8 3 68.34 3.88 -8 -8 -3 67.49 4.14 8 -8 3 67.60 3.90 8 8 4 0.92 0.81 -8 8 -4 0.30 0.95 8 8 4 0.99 0.73 -8 -8 -4 2.18 1.14 8 -8 4 1.87 0.99 -8 8 -5 112.76 6.17 8 8 5 107.83 5.74 -8 -8 -5 108.24 6.09 8 -8 5 106.74 5.79 -8 8 -6 12.21 1.89 8 8 6 14.89 1.86 8 -8 6 12.04 1.74 -8 -8 -6 7.50 1.64 -8 8 -7 30.70 3.08 8 8 7 32.57 2.68 8 -8 7 32.63 2.96 -8 -8 -7 28.85 2.95 8 8 8 2.55 1.24 -8 8 -8 1.30 1.38 -8 -8 -8 2.32 1.39 8 -8 8 1.49 1.25 -8 8 -9 15.96 2.48 8 8 9 18.29 2.45 -8 -8 -9 15.94 2.33 8 -8 9 17.71 2.39 8 8 10 1.98 1.51 -8 8 -10 -0.23 1.53 8 -8 10 2.34 1.44 8 8 11 3.75 1.82 -8 8 -11 7.08 2.08 8 -8 11 5.48 1.82 -8 8 -12 0.34 1.76 -8 9 11 14.39 2.88 -8 -9 11 21.29 3.27 8 -9 -11 19.42 2.73 -8 9 10 3.91 1.90 -8 -9 10 7.99 2.29 8 -9 -10 8.09 1.86 -8 9 9 26.85 3.37 8 -9 -9 30.12 3.13 -8 -9 9 37.92 4.05 -8 9 8 24.66 3.05 -8 -9 8 23.15 3.10 8 -9 -8 25.29 2.73 8 9 -7 18.89 1.94 -8 9 7 16.98 2.44 8 -9 -7 18.65 2.21 -8 -9 7 17.57 2.59 -8 -9 7 20.33 2.02 8 9 -6 24.67 2.08 -8 9 6 30.66 2.76 -8 -9 6 25.11 2.12 -8 -9 6 21.56 2.84 8 -9 -6 29.16 2.70 -8 9 5 1.12 1.10 8 9 -5 1.91 0.90 -8 -9 5 0.54 1.15 8 -9 -5 1.70 1.02 -8 -9 5 0.52 0.81 -8 9 4 26.33 2.44 8 9 -4 27.44 1.89 -8 -9 4 27.29 2.79 8 -9 -4 25.68 2.44 -8 -9 4 26.28 2.16 8 9 -3 24.86 2.42 -8 9 3 20.37 1.64 8 9 -3 22.33 1.64 -8 9 3 17.41 2.05 8 -9 -3 21.52 2.12 -8 -9 3 20.39 2.04 -8 9 2 64.53 3.74 -8 9 2 58.26 3.27 8 9 -2 56.04 3.10 8 9 -2 53.60 3.76 8 -9 -2 56.93 3.48 -8 -9 2 57.91 3.51 -8 9 1 22.55 2.00 8 9 -1 30.28 1.87 -8 9 1 30.04 2.14 8 9 -1 25.68 2.22 -8 -9 1 25.77 2.24 8 -9 -1 27.58 2.22 8 9 0 61.97 3.26 -8 9 0 58.69 3.53 8 9 0 58.29 3.75 -8 9 0 59.42 3.55 -8 -9 0 64.22 3.77 8 -9 0 60.96 3.58 -8 9 -1 11.07 1.18 -8 9 -1 12.76 1.53 8 9 1 11.73 1.47 8 9 1 13.75 1.36 8 -9 1 9.59 1.51 -8 -9 -1 15.62 1.85 -8 9 -2 18.19 1.97 8 9 2 17.81 1.49 8 9 2 16.53 1.71 -8 9 -2 16.98 1.28 8 -9 2 17.80 1.89 -8 -9 -2 16.14 1.97 8 9 3 13.68 1.52 -8 9 -3 10.30 1.65 8 9 3 17.53 1.65 -8 -9 -3 15.55 1.96 8 -9 3 12.75 1.64 -8 9 -4 30.05 2.74 8 9 4 26.42 2.02 8 9 4 26.97 2.09 8 -9 4 20.10 2.18 -8 -9 -4 28.09 2.66 8 9 5 3.59 1.09 -8 9 -5 1.78 1.23 -8 -9 -5 4.55 1.33 8 -9 5 2.63 1.00 8 9 6 16.22 1.98 -8 9 -6 14.99 2.12 -8 -9 -6 12.74 1.96 8 -9 6 11.43 1.77 8 9 7 8.94 1.65 -8 9 -7 6.22 1.65 -8 -9 -7 7.81 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6.99 1.81 8 12 9 19.24 2.55 -8 12 -9 12.76 2.29 -8 -12 -9 11.95 2.24 8 -12 9 10.60 2.04 8 12 10 1.58 1.42 -8 12 -10 0.48 1.60 8 -12 10 -0.81 1.26 -8 12 -11 7.06 2.23 8 12 11 4.16 1.74 8 -12 11 2.69 1.68 -8 13 10 16.79 3.05 8 -13 -10 20.20 2.72 -8 13 9 1.77 1.71 8 -13 -9 1.37 1.40 -8 13 8 35.02 3.74 8 -13 -8 30.76 3.17 8 13 -7 3.30 1.42 -8 13 7 0.96 1.41 8 -13 -7 3.14 1.40 -8 -13 7 3.51 1.18 8 13 -6 5.22 1.76 -8 13 6 3.73 1.58 -8 -13 6 2.81 1.19 8 -13 -6 6.61 1.57 -8 13 5 7.77 1.73 8 13 -5 8.06 1.73 -8 -13 5 8.61 1.47 8 -13 -5 8.32 1.56 8 13 -4 42.25 3.41 -8 13 4 40.68 3.26 -8 -13 4 39.03 2.92 8 -13 -4 42.57 3.10 -8 13 3 -0.24 0.89 8 13 -3 0.64 0.98 8 -13 -3 0.88 1.04 -8 -13 3 0.15 0.80 8 13 -2 119.71 6.88 -8 13 2 108.55 6.62 -8 13 2 114.90 5.92 8 -13 -2 119.45 6.20 -8 -13 2 124.99 6.38 8 13 -1 5.00 1.25 -8 13 1 2.37 0.93 -8 13 1 2.68 0.95 -8 -13 1 2.16 1.14 8 -13 -1 5.02 1.24 8 13 0 70.11 4.63 -8 13 0 79.74 4.48 -8 13 0 71.80 4.25 8 13 0 75.36 3.77 -8 13 0 74.17 4.34 -8 -13 0 79.16 4.53 8 -13 0 74.69 4.31 8 13 1 6.13 1.30 -8 13 -1 5.93 1.27 8 13 1 5.61 0.90 -8 13 -1 5.37 1.14 -8 13 -1 6.31 1.08 -8 -13 -1 5.72 1.40 8 -13 1 3.93 1.19 -8 13 -2 29.64 2.44 8 13 2 27.89 2.43 8 13 2 27.42 2.00 -8 13 -2 31.97 2.43 -8 -13 -2 29.55 2.84 8 -13 2 35.30 2.47 8 13 3 0.13 0.70 -8 13 -3 -0.15 0.85 -8 13 -3 -0.40 0.89 8 13 3 0.30 0.91 -8 -13 -3 -0.18 1.07 8 -13 3 0.52 0.83 -8 13 -4 97.22 5.69 8 13 4 94.49 5.14 8 13 4 93.59 5.67 -8 13 -4 96.75 5.59 8 -13 4 99.43 5.37 -8 -13 -4 106.30 5.77 -8 13 -5 1.13 1.02 -8 13 -5 1.21 1.03 8 13 5 0.63 0.90 8 -13 5 0.16 0.94 -8 -13 -5 2.26 1.35 -8 13 -6 66.83 4.36 8 13 6 59.83 3.86 -8 13 -6 62.90 4.39 -8 -13 -6 61.72 4.23 8 -13 6 61.22 3.99 8 13 7 0.70 1.15 -8 13 -7 2.18 1.38 8 -13 7 5.23 1.40 -8 -13 -7 1.63 1.34 8 13 8 17.66 2.27 -8 13 -8 13.57 2.33 8 -13 8 13.72 2.09 -8 -13 -8 12.03 2.13 8 13 9 0.77 1.35 -8 13 -9 -2.95 1.15 8 -13 9 0.21 1.23 8 13 10 13.22 2.37 -8 13 -10 7.52 2.06 8 -13 10 16.73 2.46 -8 13 -11 0.15 1.72 8 -13 11 2.36 1.57 8 14 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1.71 -17 -10 2 21.27 3.01 -17 -10 1 0.10 1.58 17 -10 -1 1.08 1.46 17 -10 0 31.47 3.50 -17 -10 0 23.47 3.25 -17 10 -1 1.60 1.73 17 -10 1 0.84 1.53 -17 -10 -1 3.60 1.89 -17 10 -2 16.89 2.87 -17 10 -3 -0.52 1.85 -17 -11 3 1.77 1.83 -17 -11 2 3.28 1.90 17 -11 -1 18.19 2.76 -17 -11 1 17.68 2.80 -17 -11 0 -0.40 1.65 17 -11 0 -0.09 1.47 -17 11 -1 17.66 2.93 -17 -11 -1 19.34 3.05 -17 11 -2 -1.06 1.60 -17 11 -3 5.41 2.12 -17 -12 3 3.94 1.87 -17 -12 2 1.92 1.75 -17 -12 1 6.30 2.23 -17 -12 0 3.31 1.89 -17 12 -1 3.96 2.00 -17 12 -2 6.74 2.29 -17 -13 3 3.93 2.03 -17 -13 2 5.91 2.12 -17 -13 1 6.45 2.25 -17 -13 0 5.47 1.97 -17 13 -2 0.28 1.90 -17 -14 3 0.80 1.74 -17 14 -2 4.19 2.21 18 0 -4 15.06 2.58 18 0 -3 -0.26 1.42 18 0 -2 27.10 3.20 18 0 -1 -0.18 1.39 18 0 0 7.38 1.95 -18 0 0 8.72 2.21 18 0 1 -0.01 1.50 -18 0 -1 4.32 2.00 -18 0 -2 8.93 2.30 18 0 2 5.12 1.77 18 1 -4 8.76 2.18 18 -1 -4 7.25 2.05 18 1 -3 10.60 2.23 18 -1 -3 9.57 2.16 18 1 -2 2.78 1.72 18 -1 -2 1.08 1.68 18 1 -1 10.93 2.23 18 -1 -1 7.35 2.05 -18 -1 1 9.00 2.34 -18 1 0 0.58 1.75 18 1 0 -0.23 1.47 18 -1 0 -0.89 1.36 -18 -1 0 -0.14 1.71 -18 1 -1 10.07 2.41 18 1 1 7.07 1.96 -18 -1 -1 9.87 2.40 18 -1 1 7.82 2.04 18 1 2 1.81 1.50 -18 1 -2 3.41 2.03 18 -1 2 2.48 1.68 -18 -1 -2 3.79 1.91 18 2 -4 1.09 1.60 18 2 -3 6.65 2.06 18 -2 -3 15.40 2.60 18 2 -2 -1.25 1.27 18 -2 -2 1.01 1.48 18 2 -1 9.82 2.06 -18 -2 1 10.20 2.38 18 -2 -1 16.26 2.52 18 2 0 4.02 1.80 -18 2 0 5.42 2.01 -18 -2 0 3.22 1.95 18 -2 0 4.00 1.73 -18 2 -1 -0.78 1.62 18 2 1 -1.69 1.28 18 -2 1 3.06 1.73 -18 -2 -1 3.06 1.93 -18 2 -2 4.78 2.08 18 2 2 0.56 1.52 -18 -2 -2 4.45 1.96 18 3 -3 3.98 1.78 18 -3 -3 5.56 2.05 18 3 -2 14.12 2.39 18 -3 -2 18.47 2.72 18 3 -1 0.33 1.42 18 -3 -1 2.29 1.58 -18 -3 1 2.59 1.78 -18 3 0 3.16 1.89 18 3 0 6.46 1.94 -18 -3 0 7.99 2.31 18 -3 0 4.79 1.79 18 3 1 3.35 1.65 -18 3 -1 2.85 1.82 18 -3 1 0.50 1.60 -18 -3 -1 1.04 1.88 18 3 2 4.63 1.78 -18 3 -2 1.30 1.82 18 -4 -2 13.45 2.45 18 4 -1 2.61 1.59 -18 -4 1 1.15 1.76 18 -4 -1 3.56 1.86 -18 4 0 25.69 3.28 18 4 0 30.58 3.21 18 -4 0 31.74 3.43 -18 -4 0 32.76 3.69 -18 4 -1 3.98 1.84 18 4 1 1.70 1.53 -18 -4 -1 4.45 2.02 18 4 2 10.55 2.08 -18 4 -2 8.22 2.31 18 4 3 -0.11 1.46 -18 -5 1 37.85 3.95 18 5 0 1.57 1.46 -18 -5 0 0.49 1.78 18 5 1 20.54 2.68 -18 5 -1 25.03 3.23 -18 -5 -1 17.97 2.94 18 5 2 1.86 1.52 -18 5 -2 2.60 1.83 18 5 3 13.05 2.37 -18 -6 1 2.73 1.86 -18 -6 0 5.55 2.10 18 6 1 -1.17 1.31 -18 6 -1 0.02 1.75 -18 -6 -1 -1.79 1.54 18 6 2 7.41 1.97 -18 6 -2 8.31 2.28 18 6 3 -3.55 1.21 -18 -7 2 9.93 2.35 -18 -7 1 0.34 1.69 -18 -7 0 4.79 1.99 -18 7 -1 1.89 1.96 -18 7 -2 2.48 2.01 18 7 3 1.57 1.65 -18 -8 2 3.25 1.93 -18 -8 1 13.65 2.65 -18 -8 0 0.56 1.80 -18 8 -1 3.25 1.88 -18 -9 2 9.22 2.35 -18 -9 1 9.82 2.45 -18 9 -1 8.76 2.50 -18 -10 2 14.72 2.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 48494 _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m 'P 21/c' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969299' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_2 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl6 N6 Nd2 O14' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1724.36 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nd Nd -0.1943 3.0179 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8762(14) _cell_length_b 13.3762(19) _cell_length_c 13.760(2) _cell_angle_alpha 85.263(2) _cell_angle_beta 85.703(2) _cell_angle_gamma 71.627(2) _cell_volume 1717.0(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 25210 _cell_measurement_theta_min 4.352 _cell_measurement_theta_max 47.019 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_F_000 858 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.800 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6543 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 25209 _diffrn_reflns_av_unetI/netI 0.0801 _diffrn_reflns_av_R_equivalents 0.0637 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.487 _diffrn_reflns_theta_max 30.199 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.922 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.922 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.922 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 9391 _reflns_number_gt 7458 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0406P)^2^+0.4454P] 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 9391 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Nd1 Nd 0.13844(2) 0.29973(2) 0.49382(2) 0.01565(7) Uani 1 1 d . . . . . O5 O 0.1562(3) 0.4436(2) 0.38835(19) 0.0213(6) Uani 1 1 d . . . . . O3 O 0.1047(3) 0.2432(2) 0.33750(19) 0.0223(6) Uani 1 1 d . . . . . O1 O 0.2847(3) 0.2267(2) 0.63845(19) 0.0204(6) Uani 1 1 d . . . . . O6 O 0.0241(3) 0.4070(2) 0.62477(19) 0.0271(7) Uani 1 1 d . . . . . N1 N 0.3877(3) 0.2211(2) 0.4033(2) 0.0165(6) Uani 1 1 d . . . . . O4 O -0.1184(3) 0.2728(3) 0.2953(2) 0.0306(7) Uani 1 1 d . . . . . O2 O 0.3178(4) 0.3740(2) 0.5705(2) 0.0319(7) Uani 1 1 d . . . . . N2 N 0.2442(3) 0.0914(2) 0.4871(2) 0.0154(6) Uani 1 1 d . . . . . N3 N -0.0018(3) 0.1835(3) 0.5924(2) 0.0193(7) Uani 1 1 d . . . . . OW1 O -0.1226(3) 0.3829(3) 0.4541(2) 0.0324(7) Uani 1 1 d . . . . . C6 C 0.3570(4) 0.0482(3) 0.4252(3) 0.0155(7) Uani 1 1 d . . . . . C17 C 0.4045(4) 0.3119(3) 0.7306(3) 0.0203(8) Uani 1 1 d . . . . . C16 C 0.3325(4) 0.3040(3) 0.6408(3) 0.0209(8) Uani 1 1 d . . . . . C9 C 0.2175(4) -0.0806(3) 0.5230(3) 0.0208(8) Uani 1 1 d . . . . . H9 H 0.1686 -0.1227 0.5571 0.025 Uiso 1 1 calc R U . . . C23 C 0.0135(4) 0.2403(3) 0.2795(3) 0.0190(8) Uani 1 1 d . . . . . C5 C 0.4334(4) 0.1202(3) 0.3770(3) 0.0163(7) Uani 1 1 d . . . . . C10 C 0.1777(4) 0.0272(3) 0.5363(3) 0.0168(7) Uani 1 1 d . . . . . C1 C 0.4566(4) 0.2878(3) 0.3647(3) 0.0206(8) Uani 1 1 d . . . . . H1 H 0.4260 0.3566 0.3842 0.025 Uiso 1 1 calc R U . . . C11 C 0.0586(4) 0.0782(3) 0.6064(3) 0.0177(8) Uani 1 1 d . . . . . C2 C 0.5708(4) 0.2595(3) 0.2972(3) 0.0230(8) Uani 1 1 d . . . . . H2 H 0.6165 0.3078 0.2718 0.028 Uiso 1 1 calc R U . . . C3 C 0.6146(4) 0.1570(4) 0.2688(3) 0.0269(9) Uani 1 1 d . . . . . H3 H 0.6898 0.1355 0.2225 0.032 Uiso 1 1 calc R U . . . C31 C 0.0989(4) 0.5239(3) 0.2297(3) 0.0174(7) Uani 1 1 d . . . . . C7 C 0.4019(4) -0.0589(3) 0.4093(3) 0.0196(8) Uani 1 1 d . . . . . H7 H 0.4791 -0.0867 0.3660 0.024 Uiso 1 1 calc R U . . . C30 C 0.0747(4) 0.5197(3) 0.3392(3) 0.0185(8) Uani 1 1 d . . . . . C18 C 0.4104(5) 0.2386(3) 0.8091(3) 0.0249(9) Uani 1 1 d . . . . . H18 H 0.3708 0.1847 0.8046 0.030 Uiso 1 1 calc R U . . . C8 C 0.3315(4) -0.1238(3) 0.4580(3) 0.0226(8) Uani 1 1 d . . . . . H8 H 0.3599 -0.1954 0.4474 0.027 Uiso 1 1 calc R U . . . C34 C 0.1436(4) 0.5335(3) 0.0294(3) 0.0220(8) Uani 1 1 d . . . . . C14 C -0.1675(4) 0.1781(3) 0.7285(3) 0.0265(9) Uani 1 1 d . . . . . H14 H -0.2452 0.2137 0.7683 0.032 Uiso 1 1 calc R U . . . C25 C 0.2196(5) 0.1534(3) 0.1649(3) 0.0246(9) Uani 1 1 d . . . . . H25 H 0.2801 0.1650 0.2083 0.029 Uiso 1 1 calc R U . . . C19 C 0.4740(5) 0.2445(4) 0.8936(3) 0.0282(9) Uani 1 1 d . . . . . H19 H 0.4767 0.1956 0.9461 0.034 Uiso 1 1 calc R U . . . C32 C 0.0227(4) 0.6124(3) 0.1741(3) 0.0221(8) Uani 1 1 d . . . . . H32 H -0.0432 0.6683 0.2047 0.027 Uiso 1 1 calc R U . . . C33 C 0.0441(5) 0.6180(3) 0.0733(3) 0.0249(9) Uani 1 1 d . . . . . H33 H -0.0070 0.6771 0.0359 0.030 Uiso 1 1 calc R U . . . C20 C 0.5337(4) 0.3244(4) 0.8985(3) 0.0272(9) Uani 1 1 d . . . . . C4 C 0.5465(4) 0.0866(3) 0.3093(3) 0.0227(8) Uani 1 1 d . . . . . H4 H 0.5764 0.0172 0.2912 0.027 Uiso 1 1 calc R U . . . C12 C 0.0114(4) 0.0193(3) 0.6823(3) 0.0263(9) Uani 1 1 d . . . . . H12 H 0.0552 -0.0531 0.6914 0.032 Uiso 1 1 calc R U . . . C24 C 0.0720(4) 0.1902(3) 0.1843(3) 0.0224(8) Uani 1 1 d . . . . . C13 C -0.1026(5) 0.0715(4) 0.7441(3) 0.0289(10) Uani 1 1 d . . . . . H13 H -0.1347 0.0341 0.7958 0.035 Uiso 1 1 calc R U . . . C22 C 0.4655(5) 0.3918(3) 0.7379(3) 0.0253(9) Uani 1 1 d . . . . . H22 H 0.4627 0.4411 0.6857 0.030 Uiso 1 1 calc R U . . . C15 C -0.1145(4) 0.2312(3) 0.6518(3) 0.0239(9) Uani 1 1 d . . . . . H15 H -0.1588 0.3034 0.6409 0.029 Uiso 1 1 calc R U . . . C29 C -0.0176(5) 0.1741(3) 0.1181(3) 0.0262(9) Uani 1 1 d . . . . . H29 H -0.1161 0.1995 0.1297 0.031 Uiso 1 1 calc R U . . . C21 C 0.5296(5) 0.3985(4) 0.8216(3) 0.0290(10) Uani 1 1 d . . . . . H21 H 0.5697 0.4521 0.8263 0.035 Uiso 1 1 calc R U . . . C26 C 0.2776(6) 0.0996(4) 0.0814(3) 0.0351(11) Uani 1 1 d . . . . . H26 H 0.3759 0.0746 0.0686 0.042 Uiso 1 1 calc R U . . . C27 C 0.1842(6) 0.0845(4) 0.0182(3) 0.0383(12) Uani 1 1 d . . . . . C28 C 0.0387(6) 0.1206(4) 0.0346(3) 0.0338(11) Uani 1 1 d . . . . . H28 H -0.0213 0.1094 -0.0094 0.041 Uiso 1 1 calc R U . . . Cl3 Cl 0.17303(11) 0.54206(9) -0.09714(7) 0.0285(2) Uani 1 1 d . . . . . Cl1 Cl 0.61217(13) 0.33214(12) 1.00607(9) 0.0419(3) Uani 1 1 d . . . . . Cl2 Cl 0.2575(2) 0.01525(13) -0.08575(10) 0.0668(5) Uani 1 1 d . . . . . C36 C 0.1947(4) 0.4396(3) 0.1833(3) 0.0195(8) Uani 1 1 d . . . . . H36 H 0.2440 0.3794 0.2202 0.023 Uiso 1 1 calc R U . . . C35 C 0.2176(4) 0.4440(3) 0.0829(3) 0.0215(8) Uani 1 1 d . . . . . H35 H 0.2819 0.3874 0.0521 0.026 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 Nd1 0.02011(11) 0.01254(10) 0.01029(10) -0.00284(7) 0.00122(7) 0.00069(7) O5 0.0284(15) 0.0182(14) 0.0122(13) -0.0004(10) -0.0010(11) -0.0001(11) O3 0.0186(14) 0.0277(15) 0.0187(14) -0.0061(12) -0.0035(11) -0.0028(12) O1 0.0231(14) 0.0172(13) 0.0184(14) -0.0047(11) -0.0040(11) -0.0011(11) O6 0.0416(18) 0.0168(14) 0.0141(14) -0.0035(11) 0.0043(12) 0.0026(13) N1 0.0147(15) 0.0168(15) 0.0160(16) -0.0035(12) -0.0017(12) -0.0012(12) O4 0.0192(15) 0.050(2) 0.0230(16) -0.0029(14) -0.0014(12) -0.0106(14) O2 0.054(2) 0.0288(16) 0.0159(15) -0.0016(12) -0.0048(14) -0.0173(15) N2 0.0168(15) 0.0163(15) 0.0128(15) -0.0026(12) -0.0025(12) -0.0040(12) N3 0.0200(16) 0.0203(16) 0.0164(16) -0.0050(13) 0.0006(13) -0.0039(13) OW1 0.0237(15) 0.0441(19) 0.0204(15) 0.0004(14) 0.0018(12) 0.0012(14) C6 0.0143(17) 0.0158(17) 0.0140(17) -0.0028(14) -0.0004(14) -0.0006(14) C17 0.0210(19) 0.023(2) 0.0186(19) -0.0093(16) 0.0035(15) -0.0079(16) C16 0.026(2) 0.0181(19) 0.0168(19) -0.0065(15) 0.0011(16) -0.0035(16) C9 0.0205(19) 0.0186(18) 0.022(2) -0.0019(15) -0.0061(16) -0.0026(15) C23 0.023(2) 0.0222(19) 0.0127(18) 0.0016(15) -0.0013(15) -0.0096(16) C5 0.0168(18) 0.0171(18) 0.0134(17) -0.0047(14) -0.0032(14) -0.0016(14) C10 0.0181(18) 0.0169(18) 0.0134(17) 0.0006(14) -0.0026(14) -0.0024(15) C1 0.0211(19) 0.0202(19) 0.020(2) 0.0015(15) -0.0037(16) -0.0059(16) C11 0.0146(17) 0.0221(19) 0.0170(18) -0.0027(15) -0.0011(14) -0.0063(15) C2 0.0190(19) 0.029(2) 0.022(2) 0.0029(17) -0.0016(16) -0.0098(17) C3 0.021(2) 0.040(3) 0.020(2) -0.0064(18) 0.0062(16) -0.0102(19) C31 0.0229(19) 0.0144(17) 0.0135(18) -0.0018(14) 0.0006(15) -0.0038(15) C7 0.0196(19) 0.0172(18) 0.0190(19) -0.0051(15) -0.0028(15) 0.0001(15) C30 0.026(2) 0.0137(17) 0.0136(18) -0.0033(14) 0.0030(15) -0.0027(15) C18 0.032(2) 0.030(2) 0.017(2) -0.0021(17) -0.0013(17) -0.0153(19) C8 0.022(2) 0.0191(19) 0.024(2) -0.0068(16) -0.0086(16) 0.0005(16) C34 0.026(2) 0.031(2) 0.0103(17) -0.0032(16) 0.0012(15) -0.0117(18) C14 0.022(2) 0.033(2) 0.024(2) -0.0105(18) 0.0073(17) -0.0079(18) C25 0.028(2) 0.030(2) 0.020(2) -0.0053(17) 0.0018(17) -0.0157(18) C19 0.028(2) 0.039(3) 0.020(2) -0.0012(18) 0.0009(17) -0.015(2) C32 0.028(2) 0.0165(19) 0.0169(19) -0.0020(15) 0.0019(16) 0.0003(16) C33 0.031(2) 0.021(2) 0.0169(19) 0.0045(16) -0.0025(17) -0.0006(17) C20 0.022(2) 0.042(3) 0.019(2) -0.0122(19) 0.0014(16) -0.0097(19) C4 0.0196(19) 0.028(2) 0.022(2) -0.0088(17) 0.0009(16) -0.0070(17) C12 0.025(2) 0.027(2) 0.023(2) 0.0029(17) -0.0013(17) -0.0043(18) C24 0.032(2) 0.023(2) 0.0162(19) 0.0012(15) -0.0014(16) -0.0134(17) C13 0.032(2) 0.035(2) 0.020(2) 0.0027(18) 0.0044(18) -0.013(2) C22 0.033(2) 0.026(2) 0.019(2) -0.0071(16) 0.0062(17) -0.0124(18) C15 0.0188(19) 0.027(2) 0.024(2) -0.0083(17) 0.0044(16) -0.0041(16) C29 0.040(2) 0.031(2) 0.0146(19) 0.0057(16) -0.0039(18) -0.022(2) C21 0.029(2) 0.032(2) 0.029(2) -0.0101(19) 0.0039(18) -0.0142(19) C26 0.045(3) 0.035(3) 0.030(2) -0.010(2) 0.018(2) -0.021(2) C27 0.073(4) 0.036(3) 0.017(2) -0.0073(19) 0.010(2) -0.035(3) C28 0.058(3) 0.035(3) 0.019(2) -0.0010(19) -0.004(2) -0.029(2) Cl3 0.0328(6) 0.0430(6) 0.0111(4) -0.0033(4) 0.0024(4) -0.0140(5) Cl1 0.0323(6) 0.0711(9) 0.0283(6) -0.0170(6) -0.0049(5) -0.0203(6) Cl2 0.1167(14) 0.0732(10) 0.0338(7) -0.0313(7) 0.0349(8) -0.0645(10) C36 0.0190(19) 0.0198(19) 0.0156(18) -0.0036(15) 0.0010(15) -0.0002(15) C35 0.024(2) 0.022(2) 0.0167(19) -0.0111(16) 0.0033(15) -0.0035(16) _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 Nd1 O5 2.357(3) . ? Nd1 O6 2.384(3) . ? Nd1 O3 2.418(3) . ? Nd1 O1 2.495(3) . ? Nd1 OW1 2.546(3) . ? Nd1 O2 2.609(3) . ? Nd1 N1 2.616(3) . ? Nd1 N3 2.628(3) . ? Nd1 N2 2.657(3) . ? Nd1 C16 2.905(4) . ? O5 C30 1.262(4) . ? O3 C23 1.259(4) . ? O1 C16 1.268(5) . ? O6 C30 1.251(4) 2_566 ? N1 C1 1.339(5) . ? N1 C5 1.352(5) . ? O4 C23 1.245(5) . ? O2 C16 1.273(5) . ? N2 C10 1.348(5) . ? N2 C6 1.354(4) . ? N3 C15 1.348(5) . ? N3 C11 1.349(5) . ? C6 C7 1.391(5) . ? C6 C5 1.488(5) . ? C17 C18 1.389(6) . ? C17 C22 1.396(5) . ? C17 C16 1.498(5) . ? C9 C8 1.388(5) . ? C9 C10 1.393(5) . ? C9 H9 0.9300 . ? C23 C24 1.513(5) . ? C5 C4 1.383(5) . ? C10 C11 1.489(5) . ? C1 C2 1.382(5) . ? C1 H1 0.9300 . ? C11 C12 1.396(5) . ? C2 C3 1.382(6) . ? C2 H2 0.9300 . ? C3 C4 1.381(6) . ? C3 H3 0.9300 . ? C31 C32 1.389(5) . ? C31 C36 1.389(5) . ? C31 C30 1.508(5) . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C30 O6 1.251(4) 2_566 ? C18 C19 1.382(6) . ? C18 H18 0.9300 . ? C8 H8 0.9300 . ? C34 C35 1.377(6) . ? C34 C33 1.391(6) . ? C34 Cl3 1.744(4) . ? C14 C13 1.373(6) . ? C14 C15 1.386(6) . ? C14 H14 0.9300 . ? C25 C26 1.394(6) . ? C25 C24 1.396(6) . ? C25 H25 0.9300 . ? C19 C20 1.382(6) . ? C19 H19 0.9300 . ? C32 C33 1.386(5) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C20 C21 1.383(6) . ? C20 Cl1 1.746(4) . ? C4 H4 0.9300 . ? C12 C13 1.391(6) . ? C12 H12 0.9300 . ? C24 C29 1.390(6) . ? C13 H13 0.9300 . ? C22 C21 1.377(6) . ? C22 H22 0.9300 . ? C15 H15 0.9300 . ? C29 C28 1.390(6) . ? C29 H29 0.9300 . ? C21 H21 0.9300 . ? C26 C27 1.384(7) . ? C26 H26 0.9300 . ? C27 C28 1.371(7) . ? C27 Cl2 1.752(5) . ? C28 H28 0.9300 . ? C36 C35 1.382(5) . ? C36 H36 0.9300 . ? C35 H35 0.9300 . ? 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 Nd1 O6 94.05(9) . . ? O5 Nd1 O3 78.66(9) . . ? O6 Nd1 O3 144.59(10) . . ? O5 Nd1 O1 125.22(9) . . ? O6 Nd1 O1 73.68(9) . . ? O3 Nd1 O1 138.23(9) . . ? O5 Nd1 OW1 80.10(10) . . ? O6 Nd1 OW1 73.14(10) . . ? O3 Nd1 OW1 71.48(9) . . ? O1 Nd1 OW1 139.29(9) . . ? O5 Nd1 O2 74.03(9) . . ? O6 Nd1 O2 69.31(10) . . ? O3 Nd1 O2 138.09(9) . . ? O1 Nd1 O2 51.49(9) . . ? OW1 Nd1 O2 132.05(10) . . ? O5 Nd1 N1 77.88(10) . . ? O6 Nd1 N1 141.99(10) . . ? O3 Nd1 N1 70.82(9) . . ? O1 Nd1 N1 80.94(9) . . ? OW1 Nd1 N1 139.23(9) . . ? O2 Nd1 N1 72.77(10) . . ? O5 Nd1 N3 153.88(10) . . ? O6 Nd1 N3 77.71(10) . . ? O3 Nd1 N3 93.68(10) . . ? O1 Nd1 N3 76.65(10) . . ? OW1 Nd1 N3 73.80(10) . . ? O2 Nd1 N3 123.90(9) . . ? N1 Nd1 N3 123.46(10) . . ? O5 Nd1 N2 134.17(9) . . ? O6 Nd1 N2 131.02(9) . . ? O3 Nd1 N2 68.67(9) . . ? O1 Nd1 N2 71.03(9) . . ? OW1 Nd1 N2 116.51(10) . . ? O2 Nd1 N2 110.48(9) . . ? N1 Nd1 N2 61.76(10) . . ? N3 Nd1 N2 61.97(10) . . ? O5 Nd1 C16 100.02(11) . . ? O6 Nd1 C16 66.64(11) . . ? O3 Nd1 C16 148.57(10) . . ? O1 Nd1 C16 25.76(10) . . ? OW1 Nd1 C16 139.71(10) . . ? O2 Nd1 C16 26.00(10) . . ? N1 Nd1 C16 78.16(10) . . ? N3 Nd1 C16 99.27(11) . . ? N2 Nd1 C16 92.44(10) . . ? C30 O5 Nd1 138.2(3) . . ? C23 O3 Nd1 144.8(2) . . ? C16 O1 Nd1 95.5(2) . . ? C30 O6 Nd1 152.4(3) 2_566 . ? C1 N1 C5 118.8(3) . . ? C1 N1 Nd1 118.2(2) . . ? C5 N1 Nd1 121.5(2) . . ? C16 O2 Nd1 90.1(2) . . ? C10 N2 C6 118.4(3) . . ? C10 N2 Nd1 121.0(2) . . ? C6 N2 Nd1 120.2(2) . . ? C15 N3 C11 118.1(3) . . ? C15 N3 Nd1 118.5(3) . . ? C11 N3 Nd1 120.6(2) . . ? N2 C6 C7 121.6(3) . . ? N2 C6 C5 116.9(3) . . ? C7 C6 C5 121.4(3) . . ? C18 C17 C22 118.8(4) . . ? C18 C17 C16 119.5(4) . . ? C22 C17 C16 121.6(4) . . ? O1 C16 O2 121.6(4) . . ? O1 C16 C17 117.7(3) . . ? O2 C16 C17 120.6(4) . . ? O1 C16 Nd1 58.8(2) . . ? O2 C16 Nd1 63.9(2) . . ? C17 C16 Nd1 167.9(3) . . ? C8 C9 C10 118.7(4) . . ? C8 C9 H9 120.6 . . ? C10 C9 H9 120.6 . . ? O4 C23 O3 125.5(4) . . ? O4 C23 C24 118.4(3) . . ? O3 C23 C24 116.0(3) . . ? N1 C5 C4 121.0(4) . . ? N1 C5 C6 116.6(3) . . ? C4 C5 C6 122.4(3) . . ? N2 C10 C9 122.5(3) . . ? N2 C10 C11 116.0(3) . . ? C9 C10 C11 121.5(3) . . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? N3 C11 C12 122.0(4) . . ? N3 C11 C10 116.7(3) . . ? C12 C11 C10 121.4(3) . . ? C3 C2 C1 117.6(4) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 C4 119.8(4) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C32 C31 C36 119.4(3) . . ? C32 C31 C30 119.6(3) . . ? C36 C31 C30 121.0(3) . . ? C8 C7 C6 119.8(4) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? O6 C30 O5 124.5(3) 2_566 . ? O6 C30 C31 117.5(3) 2_566 . ? O5 C30 C31 118.0(3) . . ? C19 C18 C17 121.1(4) . . ? C19 C18 H18 119.4 . . ? C17 C18 H18 119.4 . . ? C7 C8 C9 118.9(4) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C35 C34 C33 121.8(4) . . ? C35 C34 Cl3 119.7(3) . . ? C33 C34 Cl3 118.5(3) . . ? C13 C14 C15 118.3(4) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C26 C25 C24 121.0(4) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C18 C19 C20 118.7(4) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? C33 C32 C31 120.5(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 118.6(4) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C19 C20 C21 121.5(4) . . ? C19 C20 Cl1 118.5(4) . . ? C21 C20 Cl1 120.0(3) . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C13 C12 C11 118.5(4) . . ? C13 C12 H12 120.7 . . ? C11 C12 H12 120.7 . . ? C29 C24 C25 119.0(4) . . ? C29 C24 C23 121.4(4) . . ? C25 C24 C23 119.4(4) . . ? C14 C13 C12 119.9(4) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C21 C22 C17 120.7(4) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? N3 C15 C14 123.2(4) . . ? N3 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C28 C29 C24 120.6(4) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? C22 C21 C20 119.1(4) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C27 C26 C25 117.9(5) . . ? C27 C26 H26 121.1 . . ? C25 C26 H26 121.1 . . ? C28 C27 C26 122.6(4) . . ? C28 C27 Cl2 119.7(4) . . ? C26 C27 Cl2 117.7(4) . . ? C27 C28 C29 118.9(4) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C35 C36 C31 120.8(4) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? C34 C35 C36 118.8(4) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? _refine_diff_density_max 2.576 _refine_diff_density_min -1.398 _refine_diff_density_rms 0.148 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 9.8762 13.3762 13.7605 85.263 85.703 71.627 ZERR 1.00 0.0014 0.0019 0.0020 0.002 0.002 0.002 LATT 1 SFAC C H N O CL ND UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 10 WGHT 0.040600 0.445400 FVAR 0.12503 ND1 6 0.138439 0.299727 0.493820 11.00000 0.02011 0.01254 = 0.01029 -0.00284 0.00122 0.00069 O5 4 0.156201 0.443633 0.388351 11.00000 0.02836 0.01817 = 0.01223 -0.00043 -0.00098 -0.00013 O3 4 0.104716 0.243191 0.337505 11.00000 0.01864 0.02773 = 0.01873 -0.00608 -0.00353 -0.00284 O1 4 0.284730 0.226652 0.638454 11.00000 0.02315 0.01722 = 0.01836 -0.00474 -0.00401 -0.00112 O6 4 0.024096 0.406989 0.624767 11.00000 0.04158 0.01681 = 0.01412 -0.00346 0.00434 0.00263 N1 3 0.387715 0.221085 0.403287 11.00000 0.01474 0.01679 = 0.01603 -0.00346 -0.00174 -0.00117 O4 4 -0.118449 0.272832 0.295311 11.00000 0.01920 0.04974 = 0.02295 -0.00293 -0.00139 -0.01060 O2 4 0.317845 0.374029 0.570513 11.00000 0.05443 0.02882 = 0.01590 -0.00164 -0.00479 -0.01726 N2 3 0.244229 0.091351 0.487131 11.00000 0.01683 0.01631 = 0.01277 -0.00256 -0.00249 -0.00404 N3 3 -0.001810 0.183489 0.592445 11.00000 0.01996 0.02034 = 0.01642 -0.00501 0.00062 -0.00387 OW1 4 -0.122571 0.382890 0.454117 11.00000 0.02366 0.04411 = 0.02041 0.00043 0.00177 0.00117 C6 1 0.356953 0.048221 0.425213 11.00000 0.01429 0.01576 = 0.01399 -0.00282 -0.00042 -0.00064 C17 1 0.404544 0.311884 0.730584 11.00000 0.02095 0.02287 = 0.01858 -0.00935 0.00352 -0.00793 C16 1 0.332453 0.303985 0.640844 11.00000 0.02598 0.01808 = 0.01682 -0.00647 0.00108 -0.00348 C9 1 0.217484 -0.080581 0.523000 11.00000 0.02048 0.01856 = 0.02182 -0.00190 -0.00613 -0.00260 AFIX 43 H9 2 0.168571 -0.122723 0.557061 11.00000 -1.20000 AFIX 0 C23 1 0.013453 0.240326 0.279524 11.00000 0.02350 0.02216 = 0.01271 0.00164 -0.00131 -0.00963 C5 1 0.433385 0.120193 0.376981 11.00000 0.01678 0.01711 = 0.01338 -0.00473 -0.00323 -0.00157 C10 1 0.177750 0.027170 0.536257 11.00000 0.01805 0.01689 = 0.01343 0.00057 -0.00264 -0.00236 C1 1 0.456576 0.287812 0.364679 11.00000 0.02111 0.02020 = 0.02006 0.00155 -0.00366 -0.00592 AFIX 43 H1 2 0.426032 0.356648 0.384237 11.00000 -1.20000 AFIX 0 C11 1 0.058559 0.078166 0.606438 11.00000 0.01461 0.02207 = 0.01698 -0.00265 -0.00108 -0.00625 C2 1 0.570785 0.259518 0.297209 11.00000 0.01898 0.02939 = 0.02158 0.00291 -0.00155 -0.00981 AFIX 43 H2 2 0.616514 0.307751 0.271846 11.00000 -1.20000 AFIX 0 C3 1 0.614638 0.157037 0.268764 11.00000 0.02099 0.03986 = 0.01986 -0.00636 0.00624 -0.01021 AFIX 43 H3 2 0.689831 0.135524 0.222462 11.00000 -1.20000 AFIX 0 C31 1 0.098947 0.523852 0.229691 11.00000 0.02287 0.01445 = 0.01355 -0.00182 0.00055 -0.00381 C7 1 0.401859 -0.058941 0.409331 11.00000 0.01963 0.01716 = 0.01895 -0.00514 -0.00279 0.00007 AFIX 43 H7 2 0.479116 -0.086698 0.366029 11.00000 -1.20000 AFIX 0 C30 1 0.074696 0.519696 0.339231 11.00000 0.02566 0.01371 = 0.01358 -0.00325 0.00300 -0.00271 C18 1 0.410412 0.238637 0.809053 11.00000 0.03205 0.02970 = 0.01703 -0.00210 -0.00126 -0.01530 AFIX 43 H18 2 0.370843 0.184724 0.804645 11.00000 -1.20000 AFIX 0 C8 1 0.331461 -0.123831 0.457990 11.00000 0.02231 0.01909 = 0.02355 -0.00676 -0.00863 0.00048 AFIX 43 H8 2 0.359881 -0.195445 0.447429 11.00000 -1.20000 AFIX 0 C34 1 0.143619 0.533503 0.029400 11.00000 0.02620 0.03147 = 0.01027 -0.00321 0.00119 -0.01167 C14 1 -0.167535 0.178073 0.728455 11.00000 0.02237 0.03306 = 0.02378 -0.01049 0.00733 -0.00786 AFIX 43 H14 2 -0.245152 0.213695 0.768280 11.00000 -1.20000 AFIX 0 C25 1 0.219578 0.153409 0.164866 11.00000 0.02839 0.02998 = 0.02014 -0.00532 0.00184 -0.01566 AFIX 43 H25 2 0.280100 0.164971 0.208267 11.00000 -1.20000 AFIX 0 C19 1 0.474036 0.244484 0.893571 11.00000 0.02800 0.03871 = 0.02048 -0.00117 0.00094 -0.01477 AFIX 43 H19 2 0.476657 0.195586 0.946094 11.00000 -1.20000 AFIX 0 C32 1 0.022730 0.612406 0.174113 11.00000 0.02758 0.01653 = 0.01689 -0.00199 0.00190 0.00028 AFIX 43 H32 2 -0.043162 0.668344 0.204733 11.00000 -1.20000 AFIX 0 C33 1 0.044128 0.618047 0.073348 11.00000 0.03102 0.02074 = 0.01685 0.00448 -0.00248 -0.00064 AFIX 43 H33 2 -0.006987 0.677137 0.035928 11.00000 -1.20000 AFIX 0 C20 1 0.533697 0.324390 0.898549 11.00000 0.02191 0.04199 = 0.01900 -0.01218 0.00141 -0.00972 C4 1 0.546483 0.086625 0.309292 11.00000 0.01963 0.02750 = 0.02156 -0.00882 0.00086 -0.00700 AFIX 43 H4 2 0.576372 0.017232 0.291227 11.00000 -1.20000 AFIX 0 C12 1 0.011388 0.019347 0.682300 11.00000 0.02549 0.02691 = 0.02299 0.00294 -0.00134 -0.00426 AFIX 43 H12 2 0.055182 -0.053069 0.691355 11.00000 -1.20000 AFIX 0 C24 1 0.071959 0.190237 0.184283 11.00000 0.03158 0.02250 = 0.01622 0.00121 -0.00143 -0.01343 C13 1 -0.102589 0.071461 0.744060 11.00000 0.03208 0.03516 = 0.01966 0.00267 0.00440 -0.01294 AFIX 43 H13 2 -0.134737 0.034139 0.795835 11.00000 -1.20000 AFIX 0 C22 1 0.465485 0.391835 0.737893 11.00000 0.03321 0.02551 = 0.01932 -0.00712 0.00623 -0.01241 AFIX 43 H22 2 0.462743 0.441139 0.685700 11.00000 -1.20000 AFIX 0 C15 1 -0.114483 0.231249 0.651847 11.00000 0.01884 0.02681 = 0.02420 -0.00829 0.00445 -0.00409 AFIX 43 H15 2 -0.158769 0.303386 0.640891 11.00000 -1.20000 AFIX 0 C29 1 -0.017573 0.174149 0.118072 11.00000 0.04012 0.03063 = 0.01457 0.00566 -0.00394 -0.02180 AFIX 43 H29 2 -0.116084 0.199479 0.129737 11.00000 -1.20000 AFIX 0 C21 1 0.529633 0.398478 0.821581 11.00000 0.02935 0.03226 = 0.02911 -0.01006 0.00394 -0.01415 AFIX 43 H21 2 0.569689 0.452073 0.826278 11.00000 -1.20000 AFIX 0 C26 1 0.277587 0.099587 0.081427 11.00000 0.04503 0.03499 = 0.02977 -0.01008 0.01797 -0.02131 AFIX 43 H26 2 0.375900 0.074639 0.068644 11.00000 -1.20000 AFIX 0 C27 1 0.184190 0.084463 0.018208 11.00000 0.07343 0.03583 = 0.01720 -0.00727 0.00953 -0.03475 C28 1 0.038704 0.120576 0.034606 11.00000 0.05807 0.03528 = 0.01878 -0.00098 -0.00441 -0.02929 AFIX 43 H28 2 -0.021295 0.109396 -0.009407 11.00000 -1.20000 AFIX 0 CL3 5 0.173032 0.542063 -0.097140 11.00000 0.03283 0.04298 = 0.01106 -0.00326 0.00243 -0.01401 CL1 5 0.612169 0.332137 1.006072 11.00000 0.03233 0.07112 = 0.02828 -0.01696 -0.00494 -0.02027 CL2 5 0.257548 0.015250 -0.085755 11.00000 0.11670 0.07317 = 0.03376 -0.03126 0.03486 -0.06448 C36 1 0.194724 0.439559 0.183272 11.00000 0.01903 0.01984 = 0.01558 -0.00361 0.00104 -0.00022 AFIX 43 H36 2 0.244037 0.379428 0.220193 11.00000 -1.20000 AFIX 0 C35 1 0.217622 0.443954 0.082941 11.00000 0.02402 0.02231 = 0.01668 -0.01107 0.00333 -0.00346 AFIX 43 H35 2 0.281900 0.387407 0.052121 11.00000 -1.20000 AFIX 0 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0434 for 7458 Fo > 4sig(Fo) and 0.0615 for all 9391 data REM 451 parameters refined using 0 restraints END WGHT 0.0408 0.4205 REM Highest difference peak 2.576, deepest hole -1.398, 1-sigma level 0.148 Q1 1 0.5853 0.4605 0.5042 11.00000 0.05 2.58 Q2 1 0.4141 -0.1010 0.4876 11.00000 0.05 1.15 Q3 1 0.1782 0.0623 -0.1167 11.00000 0.05 1.09 Q4 1 -0.1420 0.3346 0.4280 11.00000 0.05 0.79 Q5 1 -0.1849 0.4552 0.4510 11.00000 0.05 0.66 Q6 1 -0.1729 0.3757 0.4002 11.00000 0.05 0.64 Q7 1 0.2420 0.1606 0.4998 11.00000 0.05 0.62 Q8 1 0.5308 0.3980 0.4724 11.00000 0.05 0.61 Q9 1 0.3858 0.3212 0.5623 11.00000 0.05 0.60 Q10 1 0.4527 0.4598 0.4957 11.00000 0.05 0.58 ; _shelx_res_checksum 89944 _shelx_hkl_file ; -1 0 0 222.29 11.49 -1 0 0 240.30 11.11 1 0 0 242.66 11.50 1 0 0 249.05 11.10 -2 0 0 10.47 1.07 -2 0 0 8.71 0.78 2 0 0 8.67 0.89 2 0 0 9.36 1.00 -3 0 0 158.97 8.05 -3 0 0 168.63 7.99 3 0 0 152.07 7.96 3 0 0 157.96 7.88 -4 0 0 174.85 8.90 -4 0 0 174.78 8.69 4 0 0 174.43 8.82 4 0 0 166.99 8.66 -5 0 0 2.74 0.95 -5 0 0 3.67 0.68 5 0 0 3.04 0.96 5 0 0 5.38 1.00 -6 0 0 17.57 1.46 -6 0 0 15.42 2.10 6 0 0 20.45 2.07 6 0 0 15.18 2.11 -7 0 0 99.24 6.33 -7 0 0 107.34 5.63 7 0 0 103.88 6.03 7 0 0 100.50 6.31 -8 0 0 39.74 4.06 8 0 0 44.70 3.69 8 0 0 39.57 3.21 -9 0 0 -1.66 0.72 9 0 0 -1.21 0.78 9 0 0 0.59 0.90 -10 0 0 2.32 1.35 10 0 0 5.12 1.76 -11 0 0 9.48 2.35 11 0 0 10.14 2.55 -12 0 0 3.88 1.94 12 0 0 6.19 2.24 12 -1 0 4.62 2.17 -12 1 0 2.82 1.82 11 -1 0 -0.41 1.28 -11 1 0 -0.34 1.09 10 -1 0 18.84 3.11 -10 1 0 16.79 2.99 9 -1 0 30.26 3.74 -9 1 0 29.99 3.71 8 -1 0 8.76 1.85 8 -1 0 9.00 1.69 -8 1 0 9.60 2.00 7 -1 0 10.42 1.87 7 -1 0 10.28 1.63 -7 1 0 6.90 1.60 6 -1 0 136.98 7.36 6 -1 0 135.27 7.68 -6 1 0 131.55 7.72 -6 1 0 137.56 7.15 5 -1 0 5.54 1.08 5 -1 0 6.68 1.33 -5 1 0 6.63 1.27 -5 1 0 5.46 0.85 4 -1 0 57.89 3.49 4 -1 0 57.51 3.24 -4 1 0 51.29 3.03 -4 1 0 46.99 3.35 3 -1 0 117.07 5.85 3 -1 0 112.54 6.02 -3 1 0 110.81 5.87 -3 1 0 120.15 6.07 2 -1 0 17.89 1.56 2 -1 0 21.19 1.48 -2 1 0 25.99 1.48 -2 1 0 21.34 1.68 1 -1 0 68.67 3.28 1 -1 0 59.25 3.16 0 -1 0 13.78 0.81 0 -1 0 13.28 0.88 0 -1 0 14.01 0.83 0 -1 0 13.48 0.74 -1 -1 0 346.37 15.72 -1 -1 0 366.60 16.46 1 1 0 319.08 15.80 1 1 0 328.74 15.60 -2 -1 0 153.68 7.46 -2 -1 0 151.81 7.32 2 1 0 154.07 7.24 2 1 0 140.68 7.26 -3 -1 0 95.73 4.95 3 1 0 97.49 5.01 3 1 0 94.75 5.02 -4 -1 0 93.83 5.09 -4 -1 0 90.89 4.75 4 1 0 84.32 4.91 4 1 0 91.29 4.91 -5 -1 0 33.38 2.18 -5 -1 0 37.53 2.75 5 1 0 36.11 2.64 5 1 0 33.21 2.46 -6 -1 0 3.42 1.09 -6 -1 0 4.35 0.77 6 1 0 5.03 1.10 6 1 0 5.39 1.22 -7 -1 0 5.99 1.44 -7 -1 0 10.09 1.16 7 1 0 7.87 1.60 7 1 0 8.58 1.53 -8 -1 0 16.49 2.41 8 1 0 18.69 2.32 8 1 0 14.21 2.26 -9 -1 0 8.60 2.01 9 1 0 14.21 2.36 9 1 0 14.89 2.15 -10 -1 0 6.11 1.78 10 1 0 2.30 1.38 -11 -1 0 4.09 1.75 11 1 0 13.49 2.66 -12 -1 0 14.87 2.98 12 1 0 19.33 3.30 -12 2 0 13.14 3.06 11 -2 0 19.94 3.30 -11 2 0 13.44 2.87 10 -2 0 2.37 1.64 -10 2 0 1.71 1.44 9 -2 0 14.32 2.65 -9 2 0 15.12 2.61 8 -2 0 47.30 4.69 8 -2 0 54.70 3.93 -8 2 0 50.49 4.25 7 -2 0 67.35 4.98 7 -2 0 76.00 4.70 -7 2 0 69.70 5.03 6 -2 0 15.62 1.93 6 -2 0 13.61 2.05 -6 2 0 17.90 1.56 -6 2 0 14.51 2.13 5 -2 0 127.53 7.44 5 -2 0 133.31 7.19 -5 2 0 138.59 7.17 -5 2 0 141.54 7.58 4 -2 0 146.57 7.93 4 -2 0 151.94 8.20 -4 2 0 161.02 8.07 -4 2 0 165.60 8.29 3 -2 0 3.77 0.76 3 -2 0 1.76 0.75 -3 2 0 1.61 0.74 -3 2 0 1.81 0.59 2 -2 0 111.99 5.76 2 -2 0 111.89 5.88 2 -2 0 112.23 5.92 -2 2 0 118.10 6.20 -2 2 0 117.96 5.96 1 -2 0 1.09 0.51 1 -2 0 1.42 0.54 1 -2 0 0.62 0.48 1 -2 0 0.77 0.48 0 -2 0 90.55 4.77 0 -2 0 94.65 4.39 0 -2 0 91.04 4.55 0 -2 0 90.13 4.51 -1 -2 0 10.97 0.96 -1 -2 0 11.05 0.69 -1 -2 0 11.44 0.95 1 2 0 11.52 0.93 1 2 0 7.64 0.65 -2 -2 0 28.23 1.85 -2 -2 0 28.97 1.88 2 2 0 31.97 1.97 2 2 0 30.10 1.74 -3 -2 0 6.17 0.82 -3 -2 0 6.14 1.00 3 2 0 5.60 0.90 3 2 0 4.72 0.81 -4 -2 0 112.52 6.03 -4 -2 0 112.82 5.85 4 2 0 105.75 5.83 4 2 0 114.15 5.93 -5 -2 0 7.18 1.31 -5 -2 0 7.66 0.99 5 2 0 10.06 1.39 5 2 0 6.61 1.20 -6 -2 0 50.60 3.57 -6 -2 0 45.00 2.89 6 2 0 45.80 3.31 6 2 0 51.08 3.33 -7 -2 0 42.01 2.69 -7 -2 0 50.19 3.56 7 2 0 34.83 2.97 7 2 0 41.57 3.24 -8 -2 0 39.77 3.39 8 2 0 37.67 3.06 8 2 0 32.34 3.50 -9 -2 0 1.16 1.05 9 2 0 1.14 1.07 9 2 0 0.72 0.93 -10 -2 0 15.65 2.68 10 2 0 20.95 3.05 10 2 0 20.14 2.68 -11 -2 0 10.79 2.41 11 2 0 11.33 2.50 -12 -2 0 1.68 1.38 12 2 0 0.00 1.43 13 2 0 5.05 2.28 11 -3 0 18.84 3.38 -11 3 0 18.17 3.37 10 -3 0 10.94 2.53 -10 3 0 14.18 2.91 9 -3 0 6.44 1.82 -9 3 0 4.43 1.69 8 -3 0 9.72 2.20 -8 3 0 12.91 2.50 7 -3 0 46.12 3.42 7 -3 0 43.14 3.72 -7 3 0 42.00 4.20 6 -3 0 58.22 4.24 6 -3 0 56.52 3.80 -6 3 0 53.27 4.15 -6 3 0 60.31 3.67 5 -3 0 4.93 1.04 5 -3 0 6.82 1.41 -5 3 0 4.69 0.94 -5 3 0 5.01 1.26 4 -3 0 36.78 2.56 4 -3 0 35.94 2.77 -4 3 0 35.01 2.73 -4 3 0 37.75 2.49 3 -3 0 174.36 8.62 -3 3 0 169.64 9.22 -3 3 0 170.37 8.86 2 -3 0 27.14 2.03 2 -3 0 30.68 2.08 2 -3 0 27.97 1.95 2 -3 0 27.03 2.09 1 -3 0 55.14 3.11 1 -3 0 54.97 3.28 1 -3 0 56.27 3.13 1 -3 0 55.23 3.18 0 -3 0 106.76 5.29 0 -3 0 116.94 5.51 0 -3 0 103.34 5.79 0 3 0 111.27 5.49 -1 -3 0 4.33 0.46 -1 -3 0 2.67 0.72 -1 -3 0 4.25 0.73 1 3 0 5.59 0.77 1 3 0 6.66 0.54 -2 -3 0 25.58 1.74 -2 -3 0 25.78 1.89 2 3 0 26.80 1.86 2 3 0 25.02 1.50 -3 -3 0 44.56 2.85 -3 -3 0 42.41 2.83 3 3 0 54.18 2.98 3 3 0 48.75 2.69 -4 -3 0 110.06 5.67 -4 -3 0 103.98 5.70 4 3 0 101.09 5.47 4 3 0 102.73 5.66 -5 -3 0 90.57 5.11 -5 -3 0 94.94 5.40 5 3 0 100.36 5.38 5 3 0 88.53 5.13 -6 -3 0 19.41 1.65 -6 -3 0 20.22 2.31 6 3 0 18.91 2.11 6 3 0 21.39 2.18 -7 -3 0 23.25 2.71 -7 -3 0 25.22 1.93 7 3 0 23.75 2.53 7 3 0 20.70 2.49 -8 -3 0 78.38 5.14 8 3 0 70.78 4.71 8 3 0 68.61 4.86 -9 -3 0 8.66 1.94 9 3 0 11.44 2.11 9 3 0 8.72 1.76 -10 -3 0 3.57 1.53 10 3 0 3.90 1.50 10 3 0 3.88 1.43 -11 -3 0 10.74 2.34 11 3 0 11.38 2.45 -12 -3 0 25.93 3.91 12 3 0 39.32 4.56 -13 -3 0 0.40 1.37 13 3 0 -1.02 1.49 11 -4 0 4.13 2.03 -11 4 0 2.82 1.96 10 -4 0 2.40 1.58 -10 4 0 4.55 1.90 9 -4 0 32.25 4.02 -9 4 0 25.27 3.67 8 -4 0 34.72 4.03 -8 4 0 37.76 4.25 7 -4 0 16.09 2.56 7 -4 0 17.76 2.29 -7 4 0 19.11 2.72 6 -4 0 42.81 3.11 6 -4 0 37.46 3.80 -6 4 0 37.84 2.86 -6 4 0 45.70 3.66 5 -4 0 129.16 7.12 5 -4 0 131.46 7.51 -5 4 0 130.66 7.20 -5 4 0 130.56 7.48 4 -4 0 59.74 3.73 4 -4 0 59.99 4.06 -4 4 0 59.07 3.75 -4 4 0 65.72 4.10 3 -4 0 14.04 1.55 3 -4 0 10.41 1.53 3 -4 0 12.87 1.66 -3 4 0 11.19 1.47 -3 4 0 12.79 1.47 2 -4 0 111.93 5.86 2 -4 0 108.49 6.03 2 -4 0 105.99 5.86 2 -4 0 107.58 5.75 1 -4 0 213.01 11.01 1 -4 0 216.76 10.51 1 -4 0 210.61 10.48 1 -4 0 213.74 10.35 0 -4 0 23.46 1.51 0 -4 0 21.31 1.75 0 -4 0 22.76 1.87 0 4 0 21.82 1.66 -1 -4 0 32.55 2.20 -1 -4 0 26.81 1.89 1 4 0 29.26 1.59 1 4 0 25.82 1.94 -2 -4 0 293.17 14.55 -2 -4 0 298.01 13.80 2 4 0 278.70 13.34 2 4 0 285.32 13.93 -3 -4 0 119.06 6.30 -3 -4 0 120.29 6.59 3 4 0 117.80 5.99 3 4 0 133.74 6.51 -4 -4 0 24.77 1.94 -4 -4 0 22.34 1.94 4 4 0 21.03 1.71 4 4 0 26.51 2.05 -5 -4 0 52.33 3.37 -5 -4 0 52.07 3.56 5 4 0 58.76 3.61 5 4 0 52.46 3.29 -6 -4 0 45.69 3.44 -6 -4 0 49.28 3.16 6 4 0 46.37 3.36 6 4 0 49.14 3.25 -7 -4 0 5.53 1.46 -7 -4 0 7.40 1.17 7 4 0 6.47 1.38 7 4 0 6.09 1.32 -8 -4 0 6.98 1.68 8 4 0 8.37 1.65 8 4 0 6.56 1.54 -9 -4 0 43.54 3.78 9 4 0 37.78 3.87 9 4 0 43.81 3.50 -10 -4 0 3.35 1.47 10 4 0 9.30 1.95 10 4 0 5.08 1.54 -11 -4 0 10.75 2.33 11 4 0 13.26 2.37 11 4 0 7.06 2.03 -12 -4 0 7.06 2.06 12 4 0 6.94 2.20 -13 -4 0 0.28 1.31 13 4 0 2.04 1.69 -11 5 0 32.70 4.68 10 -5 0 12.24 2.73 -10 5 0 10.25 2.56 9 -5 0 1.54 1.31 -9 5 0 1.28 1.27 8 -5 0 7.04 1.95 -8 5 0 7.03 1.92 7 -5 0 22.54 3.11 -7 5 0 27.36 3.37 6 -5 0 -0.22 0.78 6 -5 0 2.36 1.16 -6 5 0 1.92 1.15 -6 5 0 1.61 0.86 5 -5 0 9.90 1.83 5 -5 0 11.06 1.66 -5 5 0 12.04 2.02 -5 5 0 12.85 1.71 4 -5 0 156.56 8.59 4 -5 0 155.42 8.31 -4 5 0 154.13 8.85 -4 5 0 162.60 8.63 -4 5 0 156.98 8.53 3 -5 0 123.05 7.15 3 -5 0 130.92 7.00 3 -5 0 135.51 7.18 -3 5 0 133.99 7.57 -3 5 0 130.07 7.24 2 -5 0 1.25 0.67 2 -5 0 -0.37 0.50 2 -5 0 1.14 0.73 2 -5 0 0.11 0.67 1 -5 0 2.91 0.89 1 -5 0 2.75 0.73 1 -5 0 2.61 0.78 1 -5 0 2.13 0.75 0 -5 0 94.21 4.74 0 -5 0 92.78 5.37 0 -5 0 94.21 5.04 0 5 0 88.14 5.00 -1 -5 0 30.60 2.16 1 5 0 31.91 2.22 1 5 0 30.04 1.75 -2 -5 0 52.14 3.18 -2 -5 0 54.75 3.50 2 5 0 53.20 2.72 2 5 0 54.66 3.33 -3 -5 0 187.57 9.59 -3 -5 0 182.75 9.09 3 5 0 170.62 9.20 3 5 0 180.34 8.57 -4 -5 0 196.89 10.08 -4 -5 0 206.62 10.51 4 5 0 193.87 10.20 4 5 0 199.88 9.64 -5 -5 0 10.42 1.49 -5 -5 0 11.47 1.65 5 5 0 12.61 1.67 5 5 0 11.33 1.34 -6 -5 0 14.05 2.00 -6 -5 0 18.90 1.97 6 5 0 18.39 1.90 6 5 0 19.56 2.28 -7 -5 0 23.21 2.15 -7 -5 0 27.99 2.94 7 5 0 26.08 2.84 7 5 0 24.22 2.47 -8 -5 0 17.38 1.98 -8 -5 0 17.43 2.51 8 5 0 17.45 2.38 8 5 0 17.17 2.22 -9 -5 0 6.67 1.74 9 5 0 8.35 1.83 9 5 0 7.81 1.69 -10 -5 0 40.91 4.32 10 5 0 36.17 3.75 10 5 0 30.61 3.53 -11 -5 0 4.39 1.71 11 5 0 7.06 1.78 11 5 0 6.54 1.90 -12 -5 0 6.72 2.12 12 5 0 8.06 2.20 -13 -5 0 4.42 1.93 13 5 0 3.46 1.86 10 -6 0 23.75 3.74 -10 6 0 17.86 3.42 9 -6 0 32.09 4.31 -9 6 0 47.43 5.18 8 -6 0 3.06 1.63 -8 6 0 1.25 1.38 7 -6 0 11.51 2.37 -7 6 0 9.42 2.17 6 -6 0 57.20 4.05 6 -6 0 61.61 4.55 -6 6 0 48.16 4.21 -6 6 0 58.32 4.04 5 -6 0 32.07 2.75 5 -6 0 29.79 3.29 -5 6 0 31.91 3.39 -5 6 0 34.77 2.81 4 -6 0 -0.94 0.67 4 -6 0 -0.10 0.65 -4 6 0 0.95 0.76 -4 6 0 0.18 0.61 3 -6 0 18.44 2.07 3 -6 0 16.98 2.10 3 -6 0 20.81 2.32 2 -6 0 139.42 7.41 2 -6 0 138.33 7.31 2 -6 0 132.58 7.65 2 -6 0 131.14 7.18 1 -6 0 11.16 1.51 1 -6 0 8.33 1.45 1 -6 0 9.92 1.46 1 -6 0 11.56 1.35 0 -6 0 2.40 0.63 0 -6 0 4.15 0.97 0 -6 0 2.55 0.92 0 6 0 3.01 0.81 -1 -6 0 23.05 1.85 -1 -6 0 21.63 2.30 1 6 0 18.72 1.97 1 6 0 19.74 1.37 -2 -6 0 82.63 5.00 -2 -6 0 76.83 4.54 2 6 0 78.35 3.99 2 6 0 89.44 4.79 -3 -6 0 54.15 3.30 -3 -6 0 56.89 3.60 3 6 0 49.74 2.69 3 6 0 46.84 3.32 -4 -6 0 69.36 4.34 -4 -6 0 71.13 4.53 4 6 0 76.79 4.48 4 6 0 72.09 3.80 -5 -6 0 9.60 1.52 -5 -6 0 8.79 1.47 5 6 0 10.81 1.24 5 6 0 9.94 1.57 -6 -6 0 19.97 2.31 -6 -6 0 17.59 2.09 6 6 0 17.31 2.20 6 6 0 19.92 1.92 -7 -6 0 -0.54 0.59 -7 -6 0 -0.01 0.78 7 6 0 -0.63 0.62 7 6 0 -0.06 0.58 -8 -6 0 41.52 3.51 -8 -6 0 38.11 3.05 8 6 0 38.79 3.16 8 6 0 42.77 3.51 -9 -6 0 9.02 2.09 9 6 0 14.75 2.18 9 6 0 10.55 2.01 -10 -6 0 32.59 3.82 10 6 0 25.65 3.21 10 6 0 20.96 2.81 -11 -6 0 0.85 1.43 11 6 0 1.44 1.20 11 6 0 0.83 1.21 -12 -6 0 7.94 2.32 12 6 0 6.52 1.90 12 6 0 9.98 2.33 -13 -6 0 2.88 1.64 10 -7 0 -0.81 1.33 -10 7 0 0.26 1.62 9 -7 0 13.00 2.82 -9 7 0 9.91 2.54 8 -7 0 6.75 2.03 -8 7 0 8.76 2.28 7 -7 0 30.78 3.80 -7 7 0 28.21 3.70 6 -7 0 2.47 1.34 -6 7 0 2.37 1.27 5 -7 0 28.16 2.95 5 -7 0 27.14 3.15 -5 7 0 32.18 3.50 -5 7 0 28.51 2.95 4 -7 0 32.14 3.23 4 -7 0 31.81 2.72 4 -7 0 31.52 3.29 -4 7 0 29.27 3.02 -4 7 0 28.80 2.76 3 -7 0 56.25 3.74 3 -7 0 54.80 3.92 3 -7 0 50.42 3.68 2 -7 0 11.38 1.65 2 -7 0 11.14 1.59 2 -7 0 10.24 1.77 2 -7 0 12.24 1.84 1 -7 0 51.94 3.55 1 -7 0 51.68 3.29 1 -7 0 56.44 3.87 -1 7 0 50.90 3.46 0 -7 0 40.80 2.87 0 -7 0 40.20 3.19 0 7 0 37.58 2.78 -1 -7 0 13.39 1.88 -1 -7 0 11.19 1.54 1 7 0 12.93 1.67 1 7 0 12.26 1.15 -2 -7 0 88.12 5.35 -2 -7 0 96.78 5.92 2 7 0 100.92 5.60 2 7 0 98.97 4.75 -3 -7 0 86.71 4.78 -3 -7 0 87.52 5.14 3 7 0 72.05 4.71 3 7 0 76.04 3.95 -4 -7 0 16.70 1.91 -4 -7 0 15.53 2.03 4 7 0 14.11 1.19 4 7 0 15.23 1.95 -5 -7 0 20.70 2.29 -5 -7 0 16.74 2.17 5 7 0 18.69 2.26 5 7 0 19.77 1.55 -6 -7 0 94.48 5.86 -6 -7 0 95.61 5.85 6 7 0 92.73 5.83 6 7 0 97.55 5.22 -7 -7 0 61.30 4.29 -7 -7 0 63.53 4.46 7 7 0 61.66 3.88 7 7 0 63.32 4.46 -8 -7 0 20.71 2.78 -8 -7 0 18.44 2.24 8 7 0 13.47 2.20 8 7 0 11.55 1.76 -9 -7 0 5.34 1.58 9 7 0 6.50 1.62 9 7 0 6.11 1.44 -10 -7 0 64.60 5.33 10 7 0 76.48 5.45 10 7 0 70.51 4.91 -11 -7 0 1.10 1.19 11 7 0 3.05 1.46 11 7 0 4.37 1.57 -12 -7 0 -0.71 1.20 12 7 0 1.16 1.20 -13 -7 0 11.61 2.78 9 -8 0 15.50 3.09 -9 8 0 17.61 3.42 8 -8 0 6.15 2.07 -8 8 0 5.90 2.06 7 -8 0 3.94 1.66 -7 8 0 8.73 2.17 6 -8 0 47.19 4.08 -6 8 0 42.22 4.54 5 -8 0 38.19 3.84 5 -8 0 31.20 3.31 -5 8 0 33.90 3.03 -5 8 0 32.38 3.14 -5 8 0 33.68 3.66 4 -8 0 21.13 2.79 4 -8 0 15.72 2.34 4 -8 0 17.01 2.25 -4 8 0 15.30 2.32 -4 8 0 14.29 2.17 3 -8 0 108.96 6.37 3 -8 0 107.02 6.35 3 -8 0 105.96 6.53 2 -8 0 74.26 5.14 2 -8 0 78.56 5.02 2 -8 0 79.86 4.76 2 -8 0 73.41 4.85 1 -8 0 1.84 0.90 1 -8 0 0.55 0.81 1 -8 0 0.21 0.56 -1 8 0 0.55 0.69 0 -8 0 57.16 3.68 0 -8 0 53.56 4.00 0 8 0 58.86 3.27 0 8 0 46.88 3.59 -1 -8 0 114.49 7.10 -1 -8 0 116.72 6.51 1 8 0 123.63 6.72 1 8 0 118.70 5.96 -2 -8 0 17.71 2.00 -2 -8 0 16.41 2.26 2 8 0 17.59 2.14 2 8 0 17.73 1.27 -3 -8 0 33.99 2.92 -3 -8 0 30.95 2.51 3 8 0 29.23 1.76 3 8 0 32.70 2.70 -4 -8 0 176.05 9.54 -4 -8 0 166.74 8.87 4 8 0 173.10 9.18 4 8 0 158.49 7.97 -5 -8 0 3.20 1.13 -5 -8 0 4.95 1.26 5 8 0 5.95 1.40 5 8 0 5.19 0.81 -6 -8 0 3.45 1.17 -6 -8 0 4.54 1.24 6 8 0 2.30 0.73 6 8 0 2.51 1.08 -7 -8 0 14.90 2.14 -7 -8 0 9.00 1.81 7 8 0 11.82 2.00 7 8 0 11.87 1.49 -8 -8 0 17.76 2.61 -8 -8 0 13.53 2.14 8 8 0 15.17 2.34 8 8 0 14.65 1.90 -9 -8 0 1.91 1.19 9 8 0 1.36 1.25 -10 -8 0 2.38 1.41 10 8 0 2.60 1.41 -11 -8 0 11.00 2.49 11 8 0 9.73 2.14 -12 -8 0 6.24 2.24 12 8 0 6.75 2.00 -13 -8 0 -1.07 1.25 13 8 0 0.03 1.33 9 -9 0 22.12 3.63 -9 9 0 17.65 3.43 8 -9 0 27.18 3.90 -8 9 0 23.64 3.79 7 -9 0 1.03 1.37 -7 9 0 0.80 1.28 6 -9 0 10.61 2.22 -6 9 0 11.54 2.40 5 -9 0 61.15 4.72 -5 9 0 54.77 4.64 -5 9 0 60.75 4.74 -5 9 0 63.14 4.62 4 -9 0 8.03 1.79 4 -9 0 9.56 1.94 4 -9 0 8.55 1.71 -4 9 0 9.14 1.82 -4 9 0 8.50 1.83 3 -9 0 11.35 2.07 3 -9 0 15.54 2.22 3 -9 0 21.20 2.49 2 -9 0 144.78 8.26 2 -9 0 151.99 8.81 2 -9 0 146.85 7.95 -2 9 0 135.37 8.02 1 -9 0 108.28 6.01 1 -9 0 107.34 6.89 1 -9 0 100.36 6.28 -1 9 0 113.99 6.39 0 -9 0 1.07 0.79 0 -9 0 -0.34 0.72 0 9 0 0.00 0.65 0 9 0 -0.12 0.46 -1 -9 0 5.18 1.48 -1 -9 0 10.39 1.62 1 9 0 10.32 1.67 1 9 0 11.98 1.22 -2 -9 0 35.83 3.19 -2 -9 0 36.78 2.87 2 9 0 30.67 2.82 2 9 0 37.16 2.14 -3 -9 0 53.04 3.64 -3 -9 0 45.35 3.87 3 9 0 52.41 2.70 -4 -9 0 -0.38 0.72 -4 -9 0 -0.45 0.71 4 9 0 0.93 0.85 -5 -9 0 27.51 2.91 -5 -9 0 33.85 2.99 5 9 0 29.37 3.11 -6 -9 0 43.79 3.48 -6 -9 0 42.68 3.60 6 9 0 46.78 3.71 -7 -9 0 0.93 0.97 -7 -9 0 1.93 1.12 7 9 0 1.96 1.10 -8 -9 0 10.37 1.96 -8 -9 0 9.66 2.08 8 9 0 8.60 1.88 -9 -9 0 -0.27 0.96 -9 -9 0 0.06 1.02 9 9 0 -0.15 0.89 -10 -9 0 11.22 2.46 10 9 0 10.93 2.35 -11 -9 0 -0.47 1.18 11 9 0 1.43 1.31 -12 -9 0 7.57 2.29 12 9 0 4.88 2.05 -13 -9 0 6.56 2.25 13 9 0 5.63 2.22 8 -10 0 21.49 3.65 -8 10 0 16.25 3.34 7 -10 0 26.70 3.85 -7 10 0 21.80 3.58 6 -10 0 11.72 2.50 -6 10 0 8.61 2.23 5 -10 0 7.93 2.03 -5 10 0 9.45 2.14 -5 10 0 12.21 2.33 -5 10 0 7.96 1.89 4 -10 0 19.56 2.94 4 -10 0 23.86 2.98 -4 10 0 17.83 2.69 -4 10 0 23.13 3.12 3 -10 0 5.92 1.53 3 -10 0 4.50 1.55 -3 10 0 4.66 1.30 2 -10 0 10.87 2.01 2 -10 0 10.94 1.79 2 -10 0 9.57 2.06 -2 10 0 8.69 1.67 1 -10 0 71.32 5.18 1 -10 0 67.81 4.72 -1 10 0 66.97 4.65 0 -10 0 57.97 4.15 0 -10 0 61.78 4.72 0 10 0 55.24 4.11 0 10 0 60.05 3.64 -1 -10 0 1.80 1.11 -1 -10 0 2.23 0.95 1 10 0 3.26 1.14 1 10 0 3.36 0.75 -2 -10 0 9.01 1.59 -2 -10 0 7.51 1.80 2 10 0 9.36 1.70 -3 -10 0 33.47 3.58 -3 -10 0 32.03 3.12 3 10 0 30.87 3.21 -4 -10 0 2.83 1.23 -4 -10 0 2.28 1.07 4 10 0 3.51 1.23 -5 -10 0 45.18 3.88 -5 -10 0 44.05 3.50 5 10 0 42.89 3.62 -6 -10 0 3.52 1.30 -6 -10 0 4.86 1.36 6 10 0 1.99 1.12 -7 -10 0 35.36 3.73 -7 -10 0 36.05 3.63 7 10 0 30.90 3.49 -8 -10 0 3.65 1.44 -8 -10 0 3.79 1.54 8 10 0 3.34 1.37 -9 -10 0 -1.28 1.06 -9 -10 0 0.83 1.04 9 10 0 0.58 1.10 -10 -10 0 29.39 3.80 10 10 0 31.01 3.82 -11 -10 0 12.16 2.73 11 10 0 14.66 2.70 -12 -10 0 9.76 2.58 12 10 0 15.44 2.94 -13 -10 0 -1.62 1.31 13 10 0 -0.32 1.46 8 -11 0 0.64 1.65 -8 11 0 3.43 2.02 7 -11 0 3.92 1.95 -7 11 0 5.63 2.13 6 -11 0 17.15 3.08 -6 11 0 22.35 3.44 5 -11 0 12.20 2.58 -5 11 0 19.21 3.03 4 -11 0 1.15 1.29 4 -11 0 -0.37 1.03 -4 11 0 -0.34 0.90 -4 11 0 -0.22 0.96 3 -11 0 3.38 1.41 3 -11 0 8.89 2.02 -3 11 0 5.01 1.47 2 -11 0 2.13 1.20 2 -11 0 1.66 1.27 -2 11 0 1.37 1.05 1 -11 0 35.18 4.17 1 -11 0 50.26 3.86 -1 11 0 43.22 3.21 -1 11 0 45.53 3.67 0 -11 0 -0.27 0.83 0 -11 0 0.80 1.05 0 11 0 0.04 0.76 -1 -11 0 14.97 2.51 -1 -11 0 15.19 2.23 1 11 0 15.38 2.28 -2 -11 0 18.69 2.91 -2 -11 0 27.53 2.89 2 11 0 23.40 2.83 -3 -11 0 17.97 2.78 -3 -11 0 28.57 2.95 3 11 0 21.68 2.74 -4 -11 0 43.41 3.36 -4 -11 0 41.31 4.24 4 11 0 28.79 3.43 -5 -11 0 31.62 3.21 -5 -11 0 27.24 3.41 5 11 0 25.35 3.20 -6 -11 0 29.77 3.25 -6 -11 0 30.02 3.57 6 11 0 25.98 3.28 -7 -11 0 2.19 1.20 -7 -11 0 1.01 1.17 7 11 0 1.39 1.08 -8 -11 0 46.38 4.03 -8 -11 0 45.64 3.90 8 11 0 32.48 3.94 -9 -11 0 24.00 3.23 -9 -11 0 23.20 3.33 9 11 0 22.12 3.17 -10 -11 0 6.57 2.13 10 11 0 0.81 1.22 -11 -11 0 8.57 2.49 11 11 0 5.21 2.03 -12 -11 0 18.31 3.39 13 11 0 4.24 1.99 7 -12 0 8.38 2.62 -7 12 0 5.43 2.18 6 -12 0 -0.84 1.33 -6 12 0 2.01 1.57 -5 12 0 20.10 3.33 4 -12 0 45.63 4.88 -4 12 0 44.76 4.83 -4 12 0 47.50 4.47 3 -12 0 5.83 1.92 -3 12 0 12.28 2.42 -3 12 0 10.49 2.40 -3 12 0 11.53 2.12 2 -12 0 -0.28 1.19 2 -12 0 0.63 1.11 -2 12 0 0.48 0.95 1 -12 0 28.34 3.40 1 -12 0 29.82 3.78 -1 12 0 28.49 3.30 0 -12 0 30.60 3.96 0 -12 0 35.40 3.63 0 12 0 34.81 3.64 -1 -12 0 2.34 1.26 -1 -12 0 6.76 1.87 1 12 0 5.96 1.63 -2 -12 0 12.30 2.38 -2 -12 0 11.25 2.02 2 12 0 9.92 1.94 -3 -12 0 58.51 4.11 -3 -12 0 48.86 5.10 3 12 0 47.44 4.06 -4 -12 0 34.00 3.37 -4 -12 0 27.36 3.59 4 12 0 16.66 2.67 -5 -12 0 2.72 1.27 -5 -12 0 3.49 1.47 5 12 0 3.09 1.41 -6 -12 0 50.50 4.38 -6 -12 0 49.54 3.98 6 12 0 41.37 4.37 -7 -12 0 18.96 2.99 -7 -12 0 16.76 2.62 7 12 0 20.31 2.98 -8 -12 0 0.32 1.25 -8 -12 0 1.09 1.29 8 12 0 1.90 1.26 -9 -12 0 4.63 1.78 -9 -12 0 7.25 1.96 9 12 0 2.96 1.56 -10 -12 0 33.87 4.17 10 12 0 30.10 3.89 -11 -12 0 4.60 2.11 11 12 0 8.88 2.47 -12 -12 0 -1.57 1.46 12 12 0 0.75 1.43 -6 13 0 15.43 3.22 -5 13 0 2.19 1.67 4 -13 0 3.74 1.91 -4 13 0 5.55 1.97 -4 13 0 4.79 2.01 3 -13 0 42.48 4.58 -3 13 0 41.03 4.83 -3 13 0 45.72 4.85 2 -13 0 26.28 3.73 2 -13 0 17.53 2.97 -2 13 0 23.64 3.16 1 -13 0 0.86 1.32 1 -13 0 0.31 1.17 -1 13 0 0.02 0.98 0 -13 0 88.98 5.91 0 -13 0 80.68 6.39 0 13 0 81.41 5.84 -1 -13 0 51.65 4.18 -1 -13 0 45.43 5.03 1 13 0 51.84 4.34 -2 -13 0 2.24 1.18 -2 -13 0 1.31 1.34 2 13 0 1.20 1.13 -3 -13 0 4.09 1.42 -3 -13 0 1.26 1.35 3 13 0 4.19 1.49 -4 -13 0 41.54 4.10 -4 -13 0 43.82 4.76 4 13 0 44.66 4.55 -5 -13 0 30.28 3.90 -5 -13 0 30.76 3.46 5 13 0 25.97 3.45 -6 -13 0 -1.02 0.86 -6 -13 0 0.07 1.09 6 13 0 -0.53 0.86 -7 -13 0 26.18 3.30 -7 -13 0 16.86 2.98 7 13 0 21.30 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8.65 2.02 4 10 -4 85.06 5.68 4 10 -4 77.81 4.85 -4 -10 4 80.60 5.97 3 10 -4 141.04 7.73 -3 -10 4 143.95 8.98 2 10 -4 29.34 3.38 2 10 -4 32.41 2.69 -2 -10 4 38.08 4.13 1 10 -4 57.16 4.26 1 10 -4 49.33 3.60 -1 -10 4 53.84 4.44 0 10 -4 42.26 3.64 0 10 -4 40.29 3.14 0 -10 4 41.23 4.34 -1 10 -4 25.26 2.79 1 -10 4 27.47 3.37 1 -10 4 22.26 3.10 -2 10 -4 0.49 0.93 2 -10 4 -0.02 0.97 2 -10 4 1.12 1.11 -3 10 -4 49.39 4.03 3 -10 4 45.22 4.01 3 -10 4 45.66 4.63 -4 10 -4 39.13 4.10 4 -10 4 37.67 4.21 -5 10 -4 6.69 1.91 5 -10 4 3.92 1.71 -6 10 -4 -0.89 1.21 6 -10 4 2.91 1.53 -7 10 -4 8.76 2.47 -8 10 -4 6.69 2.27 -12 -9 4 1.96 1.70 11 9 -4 0.99 1.40 -11 -9 4 -0.96 1.31 10 9 -4 35.89 3.98 -10 -9 4 42.75 4.46 -10 -9 4 31.79 4.05 9 9 -4 33.71 3.73 -9 -9 4 35.05 4.10 -9 -9 4 30.71 3.63 8 9 -4 -1.12 0.80 8 9 -4 0.47 0.97 -8 -9 4 0.22 1.12 -8 -9 4 0.01 0.97 7 9 -4 38.10 3.79 7 9 -4 34.42 2.98 -7 -9 4 37.26 4.10 -7 -9 4 32.53 3.36 6 9 -4 48.90 3.56 6 9 -4 53.71 4.06 -6 -9 4 44.42 3.52 -6 -9 4 48.96 4.29 5 9 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4 2.86 1.42 8 8 -4 37.48 3.71 8 8 -4 33.06 3.42 -8 -8 4 33.19 3.60 -8 -8 4 33.51 3.86 7 8 -4 12.09 1.85 7 8 -4 4.06 1.34 -7 -8 4 5.81 1.54 -7 -8 4 5.19 1.61 6 8 -4 16.90 2.37 6 8 -4 17.52 2.14 -6 -8 4 12.94 1.93 -6 -8 4 18.80 2.76 5 8 -4 14.68 2.13 5 8 -4 15.71 1.97 -5 -8 4 19.06 2.06 -5 -8 4 17.96 2.66 4 8 -4 48.08 3.49 4 8 -4 64.23 4.21 -4 -8 4 58.46 4.36 -4 -8 4 49.99 3.33 3 8 -4 28.35 2.26 3 8 -4 29.19 2.97 -3 -8 4 21.72 2.85 -3 -8 4 21.36 1.81 2 8 -4 9.87 1.45 2 8 -4 5.81 1.42 -2 -8 4 8.67 1.76 -2 -8 4 8.31 1.09 1 8 -4 20.25 2.19 1 8 -4 16.94 2.34 -1 -8 4 29.00 3.10 -1 -8 4 23.12 1.72 0 8 -4 58.82 3.87 0 -8 4 55.43 3.44 0 -8 4 64.89 4.49 0 -8 4 61.00 4.34 -1 8 -4 7.91 1.41 1 -8 4 4.70 1.42 1 -8 4 4.13 1.37 1 -8 4 4.50 0.97 -2 8 -4 17.11 1.89 -2 8 -4 15.49 2.20 2 -8 4 15.05 2.27 2 -8 4 14.01 2.23 -3 8 -4 40.16 2.99 -3 8 -4 38.37 3.26 3 -8 4 41.70 3.48 3 -8 4 33.63 3.70 -4 8 -4 22.07 2.83 -4 8 -4 19.74 2.46 4 -8 4 20.10 2.79 4 -8 4 19.95 2.59 -5 8 -4 -0.98 0.66 5 -8 4 0.03 0.94 -6 8 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1.67 -2 -2 -17 0.91 1.52 2 2 17 -0.98 1.42 -3 -2 -17 23.72 3.67 -4 -2 -17 15.99 3.03 4 2 17 14.68 2.94 -5 -2 -17 -0.08 1.32 5 2 17 2.21 1.69 -6 -2 -17 1.55 1.68 6 2 17 0.71 1.68 -7 -2 -17 12.94 3.11 4 -3 -17 4.75 2.23 3 -3 -17 6.57 2.34 -3 3 17 5.07 2.30 2 -3 -17 53.94 5.73 -2 3 17 52.61 6.31 1 -3 -17 4.79 1.89 -1 3 17 3.43 1.89 0 -3 -17 1.37 1.55 0 3 17 3.71 1.99 -1 -3 -17 14.45 2.96 1 3 17 15.83 3.21 -2 -3 -17 34.05 4.46 2 3 17 46.39 5.29 -3 -3 -17 11.58 2.64 -4 -3 -17 1.86 1.49 -5 -3 -17 48.66 5.33 5 3 17 41.77 5.08 -6 -3 -17 18.73 3.43 6 3 17 22.71 3.90 -7 -3 -17 0.18 1.76 7 3 17 0.98 1.73 3 -4 -17 4.84 2.09 -3 4 17 1.35 1.71 2 -4 -17 2.14 1.73 -2 4 17 1.12 1.69 1 -4 -17 43.37 5.00 -1 4 17 41.19 5.32 0 -4 -17 51.81 5.31 0 4 17 44.90 5.52 -1 -4 -17 4.08 1.82 1 4 17 3.33 1.80 -2 -4 -17 22.78 3.63 2 4 17 27.63 4.01 -3 -4 -17 48.20 5.17 -4 -4 -17 2.50 1.84 -5 -4 -17 10.06 2.58 5 4 17 5.93 2.12 6 4 17 15.74 3.23 7 4 17 41.57 5.32 3 -5 -17 15.30 3.27 2 -5 -17 6.67 2.25 -2 5 17 5.22 2.35 1 -5 -17 -0.92 1.19 -1 5 17 -0.35 1.44 0 -5 -17 26.74 3.76 0 5 17 18.15 3.64 -1 -5 -17 29.59 4.02 1 5 17 41.55 5.13 -2 -5 -17 14.53 2.87 2 5 17 20.49 3.62 -3 -5 -17 11.40 2.63 3 5 17 9.51 2.70 6 5 17 0.68 1.48 7 5 17 12.31 3.15 3 -6 -17 15.48 3.23 2 -6 -17 27.92 4.08 1 -6 -17 4.99 2.07 -1 6 17 11.73 3.06 0 6 17 13.00 3.14 1 6 17 2.01 1.74 2 6 17 7.74 2.50 3 6 17 9.97 2.61 6 6 17 11.71 2.77 7 6 17 15.68 3.32 0 7 17 62.14 6.79 1 7 17 15.92 3.30 2 7 17 1.87 1.84 3 7 17 -0.82 1.54 7 7 17 33.70 4.58 1 8 17 38.83 5.16 2 8 17 27.67 4.27 3 8 17 -0.09 1.71 0 -9 -17 17.23 3.48 -1 -9 -17 -0.79 1.69 -2 -9 -17 20.34 3.84 2 9 17 18.66 3.64 -3 -9 -17 9.14 2.79 3 9 17 10.50 2.93 -4 -9 -17 1.37 1.88 -5 -9 -17 3.45 2.13 -6 -9 -17 6.21 2.57 -2 -10 -17 2.59 2.12 -3 -10 -17 1.89 1.97 3 10 17 -0.48 1.68 -4 -10 -17 14.28 3.37 0 -5 18 13.53 3.25 -1 -4 18 8.03 2.63 0 -4 18 0.53 1.74 2 -4 18 18.06 3.56 -2 -3 18 -0.97 1.63 -1 -3 18 3.27 2.07 0 -3 18 2.94 2.19 1 -3 18 21.46 3.75 2 -3 18 -0.49 1.51 3 -3 18 8.24 2.58 -2 -2 18 44.42 5.85 1 2 -18 16.16 3.34 -1 -2 18 21.97 4.08 0 2 -18 9.79 2.72 0 -2 18 10.43 3.00 -1 2 -18 10.37 2.74 1 -2 18 11.87 2.91 -2 2 -18 26.25 4.32 3 -2 18 2.62 1.91 4 -2 18 6.38 2.44 2 1 -18 9.40 2.68 -2 -1 18 11.78 3.13 1 1 -18 33.40 4.59 -1 -1 18 18.10 3.68 0 1 -18 20.68 3.65 0 -1 18 20.44 3.80 -1 1 -18 0.43 1.41 1 -1 18 -1.13 1.36 -2 1 -18 33.65 4.72 -3 1 -18 14.46 3.29 3 -1 18 17.85 3.33 4 -1 18 3.68 2.00 2 0 -18 0.21 1.43 -2 0 18 -1.05 1.65 1 0 -18 0.95 1.83 -1 0 18 6.03 2.35 0 0 -18 11.41 2.88 0 0 18 15.34 3.33 -1 0 -18 19.32 3.59 1 0 18 18.89 3.62 -2 0 -18 6.51 2.35 -3 0 -18 0.50 1.68 -4 0 -18 25.07 4.04 4 0 18 22.57 3.82 5 0 18 7.17 2.61 2 -1 -18 7.61 2.53 -2 1 18 17.35 3.65 1 -1 -18 8.47 2.64 -1 1 18 13.18 3.15 0 -1 -18 0.41 1.44 0 1 18 1.04 1.49 -1 -1 -18 1.19 1.53 1 1 18 -0.67 1.60 -2 -1 -18 26.23 4.10 -3 -1 -18 6.65 2.32 -4 -1 -18 0.31 1.61 4 1 18 1.44 1.79 5 1 18 11.52 3.02 2 -2 -18 10.38 2.89 -2 2 18 8.69 2.77 1 -2 -18 1.11 1.58 -1 2 18 5.24 2.39 0 -2 -18 22.89 3.71 0 2 18 22.48 4.03 -1 -2 -18 39.00 5.05 1 2 18 49.40 5.82 -2 -2 -18 2.96 1.91 2 2 18 0.25 1.57 -3 -2 -18 20.15 3.51 -4 -2 -18 21.71 3.68 -5 -2 -18 0.54 1.65 5 2 18 0.43 1.65 2 -3 -18 21.13 3.81 1 -3 -18 20.70 3.68 -1 3 18 31.32 4.67 0 -3 -18 3.15 1.93 0 3 18 1.48 1.82 -1 -3 -18 26.26 3.91 1 3 18 29.22 4.38 -2 -3 -18 35.19 4.73 2 3 18 43.86 5.35 -3 -3 -18 0.74 1.63 -4 -3 -18 12.00 2.85 -5 -3 -18 11.64 2.80 -6 -3 -18 10.91 2.91 6 3 18 8.76 2.83 2 -4 -18 25.59 4.25 1 -4 -18 37.16 4.71 -1 4 18 36.60 5.20 0 -4 -18 5.69 2.34 0 4 18 8.66 2.72 -1 -4 -18 1.33 1.66 1 4 18 -0.02 1.62 -2 -4 -18 10.22 2.65 2 4 18 11.97 2.96 -3 -4 -18 19.60 3.41 -4 -4 -18 2.69 1.87 6 4 18 8.43 2.70 2 -5 -18 8.44 2.54 1 -5 -18 -0.47 1.48 0 -5 -18 19.31 3.38 0 5 18 6.68 2.50 -1 -5 -18 25.45 3.75 1 5 18 23.12 4.05 2 5 18 6.96 2.49 1 6 18 5.03 2.38 2 6 18 23.93 4.17 2 7 18 4.09 2.38 3 7 18 10.70 2.88 3 8 18 1.04 1.84 0 -1 19 20.67 4.11 1 -1 19 0.59 1.78 0 0 19 9.41 2.83 1 0 19 72.46 6.61 0 1 19 7.59 2.69 1 1 19 6.51 2.60 1 2 19 -0.67 1.55 -2 -2 -19 1.67 1.81 -1 -3 -19 2.06 1.93 1 3 19 1.76 1.91 -2 -3 -19 3.30 2.13 -3 -3 -19 2.30 1.97 0 -4 -19 42.46 5.25 -1 -4 -19 2.49 1.94 -2 -4 -19 6.11 2.36 2 4 19 12.17 3.13 -3 -4 -19 29.48 4.31 2 5 19 13.19 3.26 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 99202 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969300' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_3 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl6 N6 O14 Sm2' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1736.58 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.870(4) _cell_length_b 13.299(5) _cell_length_c 13.741(5) _cell_angle_alpha 85.436(6) _cell_angle_beta 85.671(5) _cell_angle_gamma 71.838(5) _cell_volume 1706.0(11) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24410 _cell_measurement_theta_min 4.340 _cell_measurement_theta_max 56.748 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.690 _exptl_crystal_F_000 862 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 2.011 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6674 _exptl_absorpt_correction_T_max 0.7458 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23963 _diffrn_reflns_av_unetI/netI 0.1180 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.489 _diffrn_reflns_theta_max 28.869 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.985 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.985 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.985 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8835 _reflns_number_gt 6647 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0386P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8835 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1245 _refine_ls_wR_factor_gt 0.1133 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.003 _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 Sm1 Sm 0.13955(3) 0.29909(2) 0.99357(2) 0.01404(9) Uani 1 1 d . . . . . Cl3 Cl -0.17254(16) 0.45685(12) 1.59534(10) 0.0266(3) Uani 1 1 d . . . . . Cl1 Cl 0.61179(17) 0.33025(16) 1.50648(12) 0.0405(4) Uani 1 1 d . . . . . Cl2 Cl 0.2603(3) 0.01294(17) 0.41439(13) 0.0604(6) Uani 1 1 d . . . . . O3 O 0.1056(4) 0.2423(3) 0.8391(3) 0.0190(8) Uani 1 1 d . . . . . C16 C 0.3305(5) 0.3046(4) 1.1399(4) 0.0175(11) Uani 1 1 d . . . . . O2 O 0.3180(4) 0.3745(3) 1.0700(3) 0.0274(10) Uani 1 1 d . . . . . O1 O 0.2825(4) 0.2275(3) 1.1366(3) 0.0198(8) Uani 1 1 d . . . . . OW1 O -0.1176(4) 0.3819(4) 0.9560(3) 0.0281(10) Uani 1 1 d . . . . . O5 O 0.0276(4) 0.4076(3) 1.1222(3) 0.0248(9) Uani 1 1 d . . . . . O6 O 0.1534(4) 0.4433(3) 0.8904(3) 0.0190(8) Uani 1 1 d . . . . . O4 O -0.1165(4) 0.2724(3) 0.7953(3) 0.0283(10) Uani 1 1 d . . . . . N1 N 0.3856(4) 0.2230(3) 0.9033(3) 0.0137(9) Uani 1 1 d . . . . . C12 C 0.0116(6) 0.0205(5) 1.1824(4) 0.0220(12) Uani 1 1 d . . . . . H12 H 0.0560 -0.0520 1.1918 0.026 Uiso 1 1 calc R U . . . N2 N 0.2444(4) 0.0921(3) 0.9873(3) 0.0142(9) Uani 1 1 d . . . . . C30 C -0.0724(6) 0.4811(4) 1.1584(4) 0.0162(11) Uani 1 1 d . . . . . C14 C -0.1659(6) 0.1796(5) 1.2270(4) 0.0234(13) Uani 1 1 d . . . . . H14 H -0.2435 0.2161 1.2666 0.028 Uiso 1 1 calc R U . . . N3 N -0.0006(5) 0.1845(4) 1.0913(3) 0.0184(10) Uani 1 1 d . . . . . C31 C -0.0968(6) 0.4763(4) 1.2682(4) 0.0166(11) Uani 1 1 d . . . . . C6 C 0.3569(5) 0.0489(4) 0.9252(4) 0.0165(11) Uani 1 1 d . . . . . C17 C 0.4040(6) 0.3119(4) 1.2302(4) 0.0201(12) Uani 1 1 d . . . . . C8 C 0.3317(6) -0.1241(4) 0.9578(4) 0.0193(12) Uani 1 1 d . . . . . H8 H 0.3597 -0.1961 0.9474 0.023 Uiso 1 1 calc R U . . . C11 C 0.0588(5) 0.0789(4) 1.1059(4) 0.0178(11) Uani 1 1 d . . . . . C15 C -0.1126(6) 0.2324(4) 1.1503(4) 0.0207(12) Uani 1 1 d . . . . . H15 H -0.1566 0.3048 1.1391 0.025 Uiso 1 1 calc R U . . . C10 C 0.1779(5) 0.0281(4) 1.0350(4) 0.0159(11) Uani 1 1 d . . . . . C26 C 0.2784(7) 0.0995(5) 0.5832(5) 0.0318(15) Uani 1 1 d . . . . . H26 H 0.3768 0.0751 0.5707 0.038 Uiso 1 1 calc R U . . . C32 C -0.1932(5) 0.5607(4) 1.3149(4) 0.0177(11) Uani 1 1 d . . . . . H32 H -0.2425 0.6210 1.2780 0.021 Uiso 1 1 calc R U . . . C34 C -0.1431(6) 0.4653(5) 1.4691(4) 0.0195(12) Uani 1 1 d . . . . . C5 C 0.4329(5) 0.1223(4) 0.8764(4) 0.0141(10) Uani 1 1 d . . . . . C25 C 0.2215(6) 0.1522(5) 0.6657(4) 0.0228(13) Uani 1 1 d . . . . . H25 H 0.2821 0.1635 0.7094 0.027 Uiso 1 1 calc R U . . . C24 C 0.0755(6) 0.1890(4) 0.6852(4) 0.0162(11) Uani 1 1 d . . . . . C28 C 0.0404(7) 0.1203(5) 0.5342(4) 0.0311(15) Uani 1 1 d . . . . . H28 H -0.0194 0.1098 0.4895 0.037 Uiso 1 1 calc R U . . . C22 C 0.4648(6) 0.3929(4) 1.2384(4) 0.0216(12) Uani 1 1 d . . . . . H22 H 0.4618 0.4431 1.1868 0.026 Uiso 1 1 calc R U . . . C3 C 0.6161(6) 0.1590(5) 0.7700(4) 0.0228(13) Uani 1 1 d . . . . . H3 H 0.6928 0.1376 0.7246 0.027 Uiso 1 1 calc R U . . . C36 C -0.0221(6) 0.3880(4) 1.3234(4) 0.0205(12) Uani 1 1 d . . . . . H36 H 0.0437 0.3320 1.2924 0.025 Uiso 1 1 calc R U . . . C9 C 0.2183(6) -0.0803(4) 1.0225(4) 0.0191(12) Uani 1 1 d . . . . . H9 H 0.1697 -0.1226 1.0572 0.023 Uiso 1 1 calc R U . . . C13 C -0.1022(6) 0.0717(5) 1.2441(4) 0.0281(14) Uani 1 1 d . . . . . H13 H -0.1350 0.0345 1.2958 0.034 Uiso 1 1 calc R U . . . C23 C 0.0143(6) 0.2399(4) 0.7807(4) 0.0188(12) Uani 1 1 d . . . . . C7 C 0.4027(6) -0.0594(4) 0.9089(4) 0.0217(12) Uani 1 1 d . . . . . H7 H 0.4800 -0.0872 0.8656 0.026 Uiso 1 1 calc R U . . . C4 C 0.5477(6) 0.0878(4) 0.8092(4) 0.0185(12) Uani 1 1 d . . . . . H4 H 0.5779 0.0181 0.7911 0.022 Uiso 1 1 calc R U . . . C21 C 0.5287(6) 0.3985(5) 1.3224(4) 0.0251(13) Uani 1 1 d . . . . . H21 H 0.5692 0.4522 1.3276 0.030 Uiso 1 1 calc R U . . . C29 C -0.0152(6) 0.1734(5) 0.6181(4) 0.0221(12) Uani 1 1 d . . . . . H29 H -0.1136 0.1989 0.6300 0.027 Uiso 1 1 calc R U . . . C20 C 0.5327(6) 0.3235(5) 1.3996(4) 0.0238(13) Uani 1 1 d . . . . . C19 C 0.4729(6) 0.2423(5) 1.3935(4) 0.0272(14) Uani 1 1 d . . . . . H19 H 0.4756 0.1927 1.4456 0.033 Uiso 1 1 calc R U . . . C1 C 0.4551(5) 0.2912(4) 0.8641(4) 0.0174(11) Uani 1 1 d . . . . . H1 H 0.4236 0.3608 0.8826 0.021 Uiso 1 1 calc R U . . . C2 C 0.5703(6) 0.2617(5) 0.7982(4) 0.0241(13) Uani 1 1 d . . . . . H2 H 0.6164 0.3101 0.7732 0.029 Uiso 1 1 calc R U . . . C18 C 0.4092(6) 0.2368(5) 1.3079(4) 0.0225(12) Uani 1 1 d . . . . . H18 H 0.3697 0.1826 1.3025 0.027 Uiso 1 1 calc R U . . . C35 C -0.0434(6) 0.3812(4) 1.4241(4) 0.0240(13) Uani 1 1 d . . . . . H35 H 0.0080 0.3217 1.4609 0.029 Uiso 1 1 calc R U . . . C33 C -0.2168(6) 0.5563(4) 1.4153(4) 0.0197(12) Uani 1 1 d . . . . . H33 H -0.2808 0.6132 1.4463 0.024 Uiso 1 1 calc R U . . . C27 C 0.1873(8) 0.0833(5) 0.5187(4) 0.0329(16) Uani 1 1 d . . . . . H37 H -0.177(8) 0.454(6) 0.964(5) 0.06(2) Uiso 1 1 d . . . . . H38 H -0.134(7) 0.343(5) 0.921(5) 0.03(2) Uiso 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 Sm1 0.01669(14) 0.01191(14) 0.01003(14) -0.00267(9) 0.00096(10) 0.00074(10) Cl3 0.0302(8) 0.0401(9) 0.0109(6) -0.0026(6) 0.0016(6) -0.0132(7) Cl1 0.0289(9) 0.0708(13) 0.0267(9) -0.0153(8) -0.0051(7) -0.0186(8) Cl2 0.1005(17) 0.0690(14) 0.0315(10) -0.0278(10) 0.0305(10) -0.0566(13) O3 0.0156(19) 0.025(2) 0.016(2) -0.0039(16) -0.0028(15) -0.0034(16) C16 0.015(3) 0.019(3) 0.015(3) -0.008(2) 0.000(2) 0.001(2) O2 0.041(3) 0.026(2) 0.016(2) -0.0003(18) -0.0014(18) -0.012(2) O1 0.019(2) 0.018(2) 0.020(2) -0.0038(16) -0.0042(16) -0.0003(16) OW1 0.021(2) 0.035(3) 0.022(2) -0.003(2) -0.0022(18) 0.003(2) O5 0.035(2) 0.016(2) 0.017(2) -0.0045(16) 0.0039(17) 0.0017(18) O6 0.024(2) 0.0137(19) 0.0161(19) 0.0014(15) -0.0024(16) -0.0011(16) O4 0.015(2) 0.044(3) 0.025(2) -0.004(2) 0.0022(17) -0.0077(19) N1 0.012(2) 0.015(2) 0.012(2) -0.0012(17) -0.0053(17) -0.0016(17) C12 0.026(3) 0.023(3) 0.018(3) 0.001(2) 0.001(2) -0.010(2) N2 0.015(2) 0.015(2) 0.012(2) -0.0030(18) -0.0016(17) -0.0033(18) C30 0.023(3) 0.015(3) 0.012(3) -0.004(2) 0.004(2) -0.007(2) C14 0.017(3) 0.032(3) 0.022(3) -0.011(3) 0.004(2) -0.006(2) N3 0.015(2) 0.020(2) 0.019(2) -0.0070(19) 0.0015(18) -0.0020(19) C31 0.022(3) 0.014(3) 0.012(3) 0.002(2) -0.002(2) -0.002(2) C6 0.012(2) 0.019(3) 0.015(3) -0.003(2) -0.002(2) 0.002(2) C17 0.017(3) 0.022(3) 0.019(3) -0.007(2) 0.003(2) -0.003(2) C8 0.023(3) 0.011(3) 0.021(3) -0.006(2) -0.008(2) 0.001(2) C11 0.014(3) 0.020(3) 0.019(3) -0.002(2) -0.002(2) -0.005(2) C15 0.022(3) 0.019(3) 0.022(3) -0.005(2) -0.001(2) -0.006(2) C10 0.016(3) 0.016(3) 0.015(3) 0.000(2) -0.002(2) -0.003(2) C26 0.034(4) 0.035(4) 0.032(4) -0.009(3) 0.015(3) -0.020(3) C32 0.014(3) 0.017(3) 0.016(3) -0.005(2) 0.000(2) 0.004(2) C34 0.025(3) 0.029(3) 0.008(2) 0.000(2) -0.001(2) -0.013(3) C5 0.010(2) 0.017(3) 0.015(3) -0.002(2) -0.005(2) -0.003(2) C25 0.029(3) 0.029(3) 0.017(3) -0.003(2) 0.001(2) -0.018(3) C24 0.023(3) 0.020(3) 0.010(2) 0.002(2) -0.001(2) -0.014(2) C28 0.050(4) 0.036(4) 0.020(3) 0.001(3) -0.007(3) -0.030(3) C22 0.029(3) 0.018(3) 0.018(3) -0.001(2) 0.001(2) -0.008(2) C3 0.016(3) 0.033(3) 0.017(3) -0.007(2) 0.008(2) -0.005(2) C36 0.022(3) 0.019(3) 0.014(3) -0.003(2) 0.001(2) 0.002(2) C9 0.023(3) 0.014(3) 0.020(3) 0.000(2) -0.008(2) -0.004(2) C13 0.032(3) 0.035(4) 0.019(3) 0.002(3) 0.006(3) -0.016(3) C23 0.020(3) 0.017(3) 0.020(3) 0.003(2) 0.000(2) -0.008(2) C7 0.020(3) 0.022(3) 0.019(3) -0.006(2) -0.002(2) 0.001(2) C4 0.019(3) 0.019(3) 0.015(3) -0.012(2) 0.003(2) -0.002(2) C21 0.018(3) 0.027(3) 0.034(4) -0.014(3) 0.002(2) -0.010(2) C29 0.025(3) 0.028(3) 0.017(3) 0.002(2) 0.002(2) -0.014(3) C20 0.016(3) 0.039(4) 0.016(3) -0.009(3) 0.002(2) -0.007(3) C19 0.024(3) 0.037(4) 0.020(3) 0.002(3) -0.006(2) -0.007(3) C1 0.014(3) 0.020(3) 0.020(3) 0.001(2) -0.009(2) -0.005(2) C2 0.021(3) 0.030(3) 0.021(3) 0.004(3) -0.002(2) -0.008(3) C18 0.024(3) 0.028(3) 0.017(3) -0.004(2) 0.004(2) -0.010(3) C35 0.029(3) 0.019(3) 0.016(3) 0.008(2) 0.002(2) 0.001(2) C33 0.020(3) 0.018(3) 0.018(3) -0.006(2) 0.004(2) -0.003(2) C27 0.063(5) 0.031(4) 0.013(3) -0.009(3) 0.018(3) -0.028(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 Sm1 O6 2.325(4) . ? Sm1 O5 2.354(4) . ? Sm1 O3 2.389(4) . ? Sm1 O1 2.458(4) . ? Sm1 OW1 2.507(4) . ? Sm1 N1 2.583(4) . ? Sm1 N3 2.598(5) . ? Sm1 O2 2.600(4) . ? Sm1 N2 2.627(4) . ? Sm1 C16 2.878(5) . ? Cl3 C34 1.738(5) . ? Cl1 C20 1.736(6) . ? Cl2 C27 1.757(6) . ? O3 C23 1.260(6) . ? C16 O1 1.261(6) . ? C16 O2 1.267(6) . ? C16 C17 1.508(7) . ? OW1 H37 0.97(8) . ? OW1 H38 0.79(7) . ? O5 C30 1.258(6) . ? O6 C30 1.254(6) 2_567 ? O4 C23 1.233(6) . ? N1 C5 1.346(6) . ? N1 C1 1.356(7) . ? C12 C13 1.384(8) . ? C12 C11 1.395(7) . ? C12 H12 0.9300 . ? N2 C10 1.335(6) . ? N2 C6 1.352(6) . ? C30 O6 1.254(6) 2_567 ? C30 C31 1.509(7) . ? C14 C15 1.382(8) . ? C14 C13 1.384(8) . ? C14 H14 0.9300 . ? N3 C15 1.339(7) . ? N3 C11 1.347(7) . ? C31 C36 1.378(7) . ? C31 C32 1.391(7) . ? C6 C7 1.399(7) . ? C6 C5 1.498(7) . ? C17 C18 1.395(8) . ? C17 C22 1.402(7) . ? C8 C7 1.376(8) . ? C8 C9 1.381(8) . ? C8 H8 0.9300 . ? C11 C10 1.491(7) . ? C15 H15 0.9300 . ? C10 C9 1.391(7) . ? C26 C25 1.370(8) . ? C26 C27 1.383(9) . ? C26 H26 0.9300 . ? C32 C33 1.382(7) . ? C32 H32 0.9300 . ? C34 C33 1.389(8) . ? C34 C35 1.390(8) . ? C5 C4 1.390(7) . ? C25 C24 1.382(8) . ? C25 H25 0.9300 . ? C24 C29 1.402(7) . ? C24 C23 1.520(7) . ? C28 C27 1.384(9) . ? C28 C29 1.386(8) . ? C28 H28 0.9300 . ? C22 C21 1.374(8) . ? C22 H22 0.9300 . ? C3 C2 1.376(8) . ? C3 C4 1.380(8) . ? C3 H3 0.9300 . ? C36 C35 1.384(7) . ? C36 H36 0.9300 . ? C9 H9 0.9300 . ? C13 H13 0.9300 . ? C7 H7 0.9300 . ? C4 H4 0.9300 . ? C21 C20 1.391(8) . ? C21 H21 0.9300 . ? C29 H29 0.9300 . ? C20 C19 1.393(8) . ? C19 C18 1.392(8) . ? C19 H19 0.9300 . ? C1 C2 1.375(7) . ? C1 H1 0.9300 . ? C2 H2 0.9300 . ? C18 H18 0.9300 . ? C35 H35 0.9300 . ? C33 H33 0.9300 . ? 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 Sm1 O5 92.55(13) . . ? O6 Sm1 O3 79.02(13) . . ? O5 Sm1 O3 144.49(13) . . ? O6 Sm1 O1 125.72(13) . . ? O5 Sm1 O1 73.75(13) . . ? O3 Sm1 O1 138.40(12) . . ? O6 Sm1 OW1 79.22(14) . . ? O5 Sm1 OW1 72.64(15) . . ? O3 Sm1 OW1 71.91(14) . . ? O1 Sm1 OW1 138.66(13) . . ? O6 Sm1 N1 78.39(13) . . ? O5 Sm1 N1 141.38(14) . . ? O3 Sm1 N1 71.04(12) . . ? O1 Sm1 N1 81.38(13) . . ? OW1 Sm1 N1 139.55(14) . . ? O6 Sm1 N3 152.73(14) . . ? O5 Sm1 N3 78.22(14) . . ? O3 Sm1 N3 93.59(13) . . ? O1 Sm1 N3 76.64(13) . . ? OW1 Sm1 N3 73.54(15) . . ? N1 Sm1 N3 124.29(14) . . ? O6 Sm1 O2 74.26(13) . . ? O5 Sm1 O2 68.79(14) . . ? O3 Sm1 O2 138.30(12) . . ? O1 Sm1 O2 51.65(12) . . ? OW1 Sm1 O2 131.44(16) . . ? N1 Sm1 O2 72.62(13) . . ? N3 Sm1 O2 123.97(13) . . ? O6 Sm1 N2 135.10(13) . . ? O5 Sm1 N2 131.59(13) . . ? O3 Sm1 N2 68.85(13) . . ? O1 Sm1 N2 70.91(12) . . ? OW1 Sm1 N2 117.10(16) . . ? N1 Sm1 N2 62.23(13) . . ? N3 Sm1 N2 62.29(13) . . ? O2 Sm1 N2 110.41(13) . . ? O6 Sm1 C16 100.37(15) . . ? O5 Sm1 C16 66.29(14) . . ? O3 Sm1 C16 148.97(13) . . ? O1 Sm1 C16 25.82(14) . . ? OW1 Sm1 C16 138.89(15) . . ? N1 Sm1 C16 78.41(14) . . ? N3 Sm1 C16 99.23(15) . . ? O2 Sm1 C16 26.12(14) . . ? N2 Sm1 C16 92.38(14) . . ? C23 O3 Sm1 144.9(4) . . ? O1 C16 O2 121.6(5) . . ? O1 C16 C17 118.1(5) . . ? O2 C16 C17 120.3(5) . . ? O1 C16 Sm1 58.1(3) . . ? O2 C16 Sm1 64.6(3) . . ? C17 C16 Sm1 168.5(4) . . ? C16 O2 Sm1 89.3(3) . . ? C16 O1 Sm1 96.0(3) . . ? Sm1 OW1 H37 128(4) . . ? Sm1 OW1 H38 106(5) . . ? H37 OW1 H38 124(7) . . ? C30 O5 Sm1 152.4(4) . . ? C30 O6 Sm1 138.9(3) 2_567 . ? C5 N1 C1 118.0(4) . . ? C5 N1 Sm1 121.9(3) . . ? C1 N1 Sm1 118.6(3) . . ? C13 C12 C11 119.3(5) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C10 N2 C6 118.1(4) . . ? C10 N2 Sm1 121.2(3) . . ? C6 N2 Sm1 120.2(3) . . ? O6 C30 O5 124.5(5) 2_567 . ? O6 C30 C31 118.4(5) 2_567 . ? O5 C30 C31 117.2(5) . . ? C15 C14 C13 119.0(5) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C15 N3 C11 117.8(5) . . ? C15 N3 Sm1 118.7(4) . . ? C11 N3 Sm1 120.7(3) . . ? C36 C31 C32 119.3(5) . . ? C36 C31 C30 120.0(5) . . ? C32 C31 C30 120.7(5) . . ? N2 C6 C7 122.0(5) . . ? N2 C6 C5 116.6(5) . . ? C7 C6 C5 121.4(5) . . ? C18 C17 C22 119.6(5) . . ? C18 C17 C16 118.8(5) . . ? C22 C17 C16 121.7(5) . . ? C7 C8 C9 118.9(5) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? N3 C11 C12 122.1(5) . . ? N3 C11 C10 115.9(5) . . ? C12 C11 C10 122.0(5) . . ? N3 C15 C14 123.2(5) . . ? N3 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? N2 C10 C9 122.8(5) . . ? N2 C10 C11 115.9(5) . . ? C9 C10 C11 121.2(5) . . ? C25 C26 C27 119.0(6) . . ? C25 C26 H26 120.5 . . ? C27 C26 H26 120.5 . . ? C33 C32 C31 120.9(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C33 C34 C35 121.3(5) . . ? C33 C34 Cl3 119.7(4) . . ? C35 C34 Cl3 119.0(4) . . ? N1 C5 C4 122.1(5) . . ? N1 C5 C6 116.0(4) . . ? C4 C5 C6 122.0(5) . . ? C26 C25 C24 121.2(5) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C24 C29 119.0(5) . . ? C25 C24 C23 120.5(5) . . ? C29 C24 C23 120.3(5) . . ? C27 C28 C29 118.2(6) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C21 C22 C17 120.3(5) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C2 C3 C4 119.7(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C31 C36 C35 121.1(5) . . ? C31 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C8 C9 C10 119.0(5) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C12 C13 C14 118.5(5) . . ? C12 C13 H13 120.7 . . ? C14 C13 H13 120.7 . . ? O4 C23 O3 126.1(5) . . ? O4 C23 C24 118.7(5) . . ? O3 C23 C24 115.1(5) . . ? C8 C7 C6 119.1(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C3 C4 C5 118.8(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C22 C21 C20 119.7(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C28 C29 C24 120.6(6) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? C21 C20 C19 121.2(5) . . ? C21 C20 Cl1 120.2(5) . . ? C19 C20 Cl1 118.6(5) . . ? C18 C19 C20 118.7(6) . . ? C18 C19 H19 120.6 . . ? C20 C19 H19 120.6 . . ? N1 C1 C2 122.7(5) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? C1 C2 C3 118.7(5) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C19 C18 C17 120.5(6) . . ? C19 C18 H18 119.7 . . ? C17 C18 H18 119.7 . . ? C36 C35 C34 118.6(5) . . ? C36 C35 H35 120.7 . . ? C34 C35 H35 120.7 . . ? C32 C33 C34 118.7(5) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C26 C27 C28 122.0(5) . . ? C26 C27 Cl2 119.0(5) . . ? C28 C27 Cl2 119.0(5) . . ? _refine_diff_density_max 2.580 _refine_diff_density_min -1.225 _refine_diff_density_rms 0.189 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 9.8702 13.2991 13.7411 85.436 85.671 71.838 ZERR 1.00 0.0037 0.0050 0.0051 0.006 0.005 0.005 LATT 1 SFAC C H N O CL SM UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 20 WGHT 0.038600 FVAR 0.12530 SM1 6 0.139549 0.299090 0.993574 11.00000 0.01669 0.01191 = 0.01003 -0.00267 0.00096 0.00074 CL3 5 -0.172539 0.456849 1.595341 11.00000 0.03023 0.04014 = 0.01087 -0.00263 0.00157 -0.01319 CL1 5 0.611786 0.330250 1.506485 11.00000 0.02894 0.07080 = 0.02670 -0.01528 -0.00507 -0.01856 CL2 5 0.260339 0.012943 0.414391 11.00000 0.10052 0.06897 = 0.03150 -0.02783 0.03047 -0.05656 O3 4 0.105622 0.242326 0.839082 11.00000 0.01555 0.02474 = 0.01564 -0.00391 -0.00283 -0.00339 C16 1 0.330539 0.304593 1.139931 11.00000 0.01474 0.01928 = 0.01524 -0.00768 -0.00030 0.00103 O2 4 0.317955 0.374489 1.070031 11.00000 0.04118 0.02583 = 0.01608 -0.00031 -0.00139 -0.01173 O1 4 0.282548 0.227544 1.136590 11.00000 0.01914 0.01792 = 0.01961 -0.00378 -0.00420 -0.00033 OW1 4 -0.117599 0.381943 0.956028 11.00000 0.02052 0.03463 = 0.02196 -0.00294 -0.00222 0.00254 O5 4 0.027646 0.407563 1.122151 11.00000 0.03470 0.01577 = 0.01718 -0.00449 0.00388 0.00172 O6 4 0.153400 0.443299 0.890428 11.00000 0.02388 0.01375 = 0.01609 0.00142 -0.00236 -0.00111 O4 4 -0.116485 0.272413 0.795261 11.00000 0.01486 0.04418 = 0.02464 -0.00406 0.00216 -0.00765 N1 3 0.385563 0.222981 0.903334 11.00000 0.01250 0.01520 = 0.01228 -0.00116 -0.00531 -0.00163 C12 1 0.011584 0.020503 1.182384 11.00000 0.02586 0.02343 = 0.01783 0.00087 0.00062 -0.01000 AFIX 43 H12 2 0.056044 -0.052044 1.191786 11.00000 -1.20000 AFIX 0 N2 3 0.244406 0.092116 0.987290 11.00000 0.01510 0.01484 = 0.01229 -0.00301 -0.00155 -0.00328 C30 1 -0.072418 0.481140 1.158437 11.00000 0.02271 0.01501 = 0.01170 -0.00443 0.00422 -0.00737 C14 1 -0.165923 0.179623 1.227041 11.00000 0.01683 0.03191 = 0.02150 -0.01100 0.00415 -0.00626 AFIX 43 H14 2 -0.243507 0.216059 1.266631 11.00000 -1.20000 AFIX 0 N3 3 -0.000567 0.184455 1.091328 11.00000 0.01461 0.02011 = 0.01881 -0.00696 0.00154 -0.00202 C31 1 -0.096764 0.476322 1.268197 11.00000 0.02157 0.01414 = 0.01174 0.00173 -0.00249 -0.00220 C6 1 0.356850 0.048863 0.925235 11.00000 0.01175 0.01906 = 0.01456 -0.00314 -0.00226 0.00209 C17 1 0.404034 0.311890 1.230233 11.00000 0.01739 0.02209 = 0.01935 -0.00712 0.00318 -0.00334 C8 1 0.331715 -0.124051 0.957769 11.00000 0.02306 0.01145 = 0.02111 -0.00645 -0.00819 0.00103 AFIX 43 H8 2 0.359665 -0.196070 0.947386 11.00000 -1.20000 AFIX 0 C11 1 0.058847 0.078911 1.105924 11.00000 0.01417 0.02048 = 0.01853 -0.00208 -0.00184 -0.00451 C15 1 -0.112560 0.232412 1.150326 11.00000 0.02159 0.01867 = 0.02226 -0.00490 -0.00082 -0.00583 AFIX 43 H15 2 -0.156593 0.304794 1.139130 11.00000 -1.20000 AFIX 0 C10 1 0.177903 0.028053 1.035026 11.00000 0.01609 0.01551 = 0.01507 0.00031 -0.00210 -0.00323 C26 1 0.278420 0.099524 0.583179 11.00000 0.03403 0.03463 = 0.03154 -0.00882 0.01481 -0.01970 AFIX 43 H26 2 0.376803 0.075050 0.570733 11.00000 -1.20000 AFIX 0 C32 1 -0.193194 0.560732 1.314860 11.00000 0.01403 0.01740 = 0.01610 -0.00470 -0.00023 0.00377 AFIX 43 H32 2 -0.242458 0.620968 1.277969 11.00000 -1.20000 AFIX 0 C34 1 -0.143096 0.465320 1.469071 11.00000 0.02544 0.02851 = 0.00773 0.00029 -0.00142 -0.01308 C5 1 0.432873 0.122300 0.876419 11.00000 0.01018 0.01658 = 0.01544 -0.00172 -0.00469 -0.00281 C25 1 0.221472 0.152228 0.665704 11.00000 0.02922 0.02878 = 0.01688 -0.00301 0.00085 -0.01816 AFIX 43 H25 2 0.282137 0.163453 0.709361 11.00000 -1.20000 AFIX 0 C24 1 0.075525 0.188996 0.685223 11.00000 0.02296 0.02030 = 0.00996 0.00214 -0.00070 -0.01430 C28 1 0.040378 0.120310 0.534196 11.00000 0.05004 0.03576 = 0.01991 0.00106 -0.00726 -0.03050 AFIX 43 H28 2 -0.019446 0.109828 0.489505 11.00000 -1.20000 AFIX 0 C22 1 0.464787 0.392942 1.238403 11.00000 0.02850 0.01847 = 0.01791 -0.00145 0.00138 -0.00766 AFIX 43 H22 2 0.461788 0.443114 1.186776 11.00000 -1.20000 AFIX 0 C3 1 0.616075 0.158987 0.769976 11.00000 0.01649 0.03291 = 0.01677 -0.00737 0.00767 -0.00473 AFIX 43 H3 2 0.692759 0.137631 0.724621 11.00000 -1.20000 AFIX 0 C36 1 -0.022103 0.388015 1.323363 11.00000 0.02229 0.01918 = 0.01417 -0.00282 0.00098 0.00195 AFIX 43 H36 2 0.043699 0.332023 1.292370 11.00000 -1.20000 AFIX 0 C9 1 0.218327 -0.080293 1.022485 11.00000 0.02322 0.01365 = 0.02008 -0.00016 -0.00805 -0.00358 AFIX 43 H9 2 0.169737 -0.122617 1.057152 11.00000 -1.20000 AFIX 0 C13 1 -0.102169 0.071729 1.244056 11.00000 0.03205 0.03533 = 0.01900 0.00154 0.00616 -0.01589 AFIX 43 H13 2 -0.135050 0.034501 1.295777 11.00000 -1.20000 AFIX 0 C23 1 0.014333 0.239899 0.780684 11.00000 0.02015 0.01661 = 0.02003 0.00306 0.00017 -0.00763 C7 1 0.402653 -0.059362 0.908909 11.00000 0.02038 0.02163 = 0.01885 -0.00596 -0.00157 0.00092 AFIX 43 H7 2 0.480035 -0.087234 0.865600 11.00000 -1.20000 AFIX 0 C4 1 0.547723 0.087806 0.809222 11.00000 0.01943 0.01936 = 0.01547 -0.01160 0.00330 -0.00243 AFIX 43 H4 2 0.577916 0.018052 0.791064 11.00000 -1.20000 AFIX 0 C21 1 0.528728 0.398540 1.322368 11.00000 0.01802 0.02716 = 0.03374 -0.01402 0.00155 -0.00982 AFIX 43 H21 2 0.569171 0.452250 1.327579 11.00000 -1.20000 AFIX 0 C29 1 -0.015218 0.173413 0.618105 11.00000 0.02470 0.02760 = 0.01722 0.00161 0.00154 -0.01395 AFIX 43 H29 2 -0.113638 0.198947 0.629999 11.00000 -1.20000 AFIX 0 C20 1 0.532709 0.323514 1.399556 11.00000 0.01573 0.03942 = 0.01592 -0.00903 0.00244 -0.00691 C19 1 0.472924 0.242319 1.393459 11.00000 0.02377 0.03655 = 0.01999 0.00155 -0.00562 -0.00718 AFIX 43 H19 2 0.475556 0.192744 1.445558 11.00000 -1.20000 AFIX 0 C1 1 0.455111 0.291201 0.864150 11.00000 0.01356 0.01967 = 0.01966 0.00147 -0.00853 -0.00477 AFIX 43 H1 2 0.423587 0.360839 0.882635 11.00000 -1.20000 AFIX 0 C2 1 0.570338 0.261661 0.798202 11.00000 0.02058 0.03011 = 0.02108 0.00402 -0.00231 -0.00832 AFIX 43 H2 2 0.616427 0.310147 0.773182 11.00000 -1.20000 AFIX 0 C18 1 0.409152 0.236788 1.307890 11.00000 0.02393 0.02798 = 0.01681 -0.00373 0.00355 -0.01020 AFIX 43 H18 2 0.369659 0.182600 1.302465 11.00000 -1.20000 AFIX 0 C35 1 -0.043373 0.381229 1.424101 11.00000 0.02920 0.01875 = 0.01642 0.00786 0.00212 0.00085 AFIX 43 H35 2 0.007965 0.321672 1.460927 11.00000 -1.20000 AFIX 0 C33 1 -0.216828 0.556341 1.415305 11.00000 0.02035 0.01814 = 0.01819 -0.00619 0.00412 -0.00252 AFIX 43 H33 2 -0.280825 0.613190 1.446298 11.00000 -1.20000 AFIX 0 C27 1 0.187312 0.083307 0.518711 11.00000 0.06252 0.03134 = 0.01284 -0.00944 0.01792 -0.02845 H37 2 -0.177084 0.454134 0.964216 11.00000 0.05766 H38 2 -0.134462 0.343454 0.921399 11.00000 0.03480 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0560 for 6647 Fo > 4sig(Fo) and 0.0801 for all 8835 data REM 459 parameters refined using 0 restraints END WGHT 0.0389 0.0000 REM Highest difference peak 2.580, deepest hole -1.225, 1-sigma level 0.189 Q1 1 -0.4205 0.4563 1.0039 11.00000 0.05 2.58 Q2 1 0.1758 0.0531 0.3809 11.00000 0.05 1.03 Q3 1 0.4207 -0.0958 0.9758 11.00000 0.05 0.85 Q4 1 0.4815 0.4811 1.0096 11.00000 0.05 0.82 Q5 1 -0.0807 0.0555 1.1029 11.00000 0.05 0.73 Q6 1 -0.2613 0.1145 1.3466 11.00000 0.05 0.72 Q7 1 0.2880 0.1987 0.8510 11.00000 0.05 0.72 Q8 1 0.0073 0.4001 1.5635 11.00000 0.05 0.71 Q9 1 -0.1316 0.3796 0.8782 11.00000 0.05 0.70 Q10 1 -0.1407 0.3162 1.1615 11.00000 0.05 0.69 ; _shelx_res_checksum 10890 _shelx_hkl_file ; -1 0 0 245.25 16.48 -1 0 0 240.71 16.85 -1 0 0 248.31 15.96 1 0 0 244.35 15.95 1 0 0 235.02 15.27 -2 0 0 11.29 1.97 -2 0 0 8.16 1.39 2 0 0 6.93 1.24 2 0 0 10.13 1.04 -3 0 0 165.45 12.02 -3 0 0 154.24 12.66 3 0 0 169.45 11.18 -4 0 0 194.00 15.21 -4 0 0 197.72 14.31 4 0 0 187.96 13.30 4 0 0 194.24 13.18 -5 0 0 1.02 1.47 -5 0 0 0.50 1.01 5 0 0 2.06 1.18 5 0 0 1.69 0.70 -6 0 0 21.97 4.43 -6 0 0 20.07 3.57 6 0 0 24.00 3.14 -7 0 0 110.78 9.05 -7 0 0 111.37 9.96 -7 0 0 105.67 11.15 7 0 0 130.10 9.75 -8 0 0 46.77 7.11 8 0 0 51.23 5.70 -9 0 0 1.38 2.46 9 0 0 0.43 1.53 -10 0 0 13.81 4.88 10 0 0 8.50 2.86 -11 0 0 4.24 3.42 11 0 0 7.20 3.12 -12 0 0 7.78 4.79 12 0 0 8.52 3.55 12 -1 0 1.33 2.43 -12 1 0 3.72 4.06 11 -1 0 1.96 2.04 -11 1 0 0.31 2.94 10 -1 0 24.18 4.93 -10 1 0 21.76 6.22 9 -1 0 24.10 4.63 9 -1 0 38.35 5.41 -9 1 0 20.65 5.59 8 -1 0 10.52 2.84 -8 1 0 15.95 3.84 -8 1 0 15.10 4.38 7 -1 0 7.91 2.29 -7 1 0 6.48 2.44 -7 1 0 7.82 3.02 6 -1 0 168.47 11.36 -6 1 0 132.15 11.89 -6 1 0 133.69 12.82 -6 1 0 141.03 10.37 5 -1 0 8.74 2.11 -5 1 0 16.04 1.96 -5 1 0 11.93 2.68 -5 1 0 14.53 3.34 4 -1 0 54.73 4.70 -4 1 0 56.40 5.90 -4 1 0 57.13 5.31 -4 1 0 50.57 4.18 3 -1 0 120.40 8.71 -3 1 0 125.70 8.50 -3 1 0 127.80 10.18 -3 1 0 118.97 9.57 2 -1 0 24.84 2.34 -2 1 0 26.88 2.74 -2 1 0 23.15 1.74 -2 1 0 17.85 2.76 -2 1 0 25.20 1.87 1 -1 0 78.03 5.38 -1 1 0 81.04 6.12 0 1 0 16.03 1.46 0 1 0 15.66 1.23 0 1 0 15.89 1.41 0 1 0 15.18 1.23 -1 -1 0 409.62 27.62 1 1 0 410.22 25.11 1 1 0 389.14 26.52 -2 -1 0 163.62 12.80 -2 -1 0 180.91 12.00 2 1 0 172.36 11.42 2 1 0 178.87 11.93 -3 -1 0 105.92 7.53 -3 -1 0 108.35 8.47 3 1 0 99.77 7.31 3 1 0 95.79 7.25 -4 -1 0 97.07 7.68 -4 -1 0 93.47 8.63 4 1 0 98.04 7.47 4 1 0 107.09 7.36 -5 -1 0 41.54 5.25 -5 -1 0 37.83 4.06 5 1 0 43.81 4.21 5 1 0 43.26 3.64 -6 -1 0 3.36 2.23 -6 -1 0 2.63 1.52 6 1 0 4.44 1.62 6 1 0 6.53 1.41 -7 -1 0 10.28 2.52 -7 -1 0 5.60 2.82 7 1 0 11.76 2.64 7 1 0 13.55 1.90 -8 -1 0 21.66 5.08 8 1 0 23.02 3.96 -9 -1 0 18.64 5.15 9 1 0 15.42 3.61 -10 -1 0 4.83 3.60 10 1 0 8.00 2.94 -11 -1 0 12.30 4.79 11 1 0 9.36 3.32 -12 -1 0 25.38 7.54 12 1 0 24.64 5.29 12 -2 0 33.41 6.36 -12 2 0 17.96 6.45 11 -2 0 20.99 4.88 -11 2 0 16.57 5.80 10 -2 0 2.16 1.94 -10 2 0 5.10 3.49 9 -2 0 11.38 3.37 9 -2 0 15.10 4.15 -9 2 0 11.62 4.32 8 -2 0 66.14 6.61 -8 2 0 47.29 7.49 -8 2 0 67.65 7.71 7 -2 0 87.19 7.80 -7 2 0 93.58 9.77 -7 2 0 75.03 8.45 6 -2 0 6.48 2.08 -6 2 0 17.75 3.65 -6 2 0 10.93 3.39 5 -2 0 129.57 10.28 -5 2 0 140.87 12.40 -5 2 0 149.07 11.87 4 -2 0 184.00 12.92 -4 2 0 171.36 14.68 -4 2 0 193.65 14.45 3 -2 0 7.24 1.58 -3 2 0 8.75 2.20 -3 2 0 5.72 1.95 2 -2 0 108.24 7.86 -2 2 0 117.52 8.92 -2 2 0 111.96 9.03 1 -2 0 2.67 0.87 1 -2 0 2.08 0.52 -1 2 0 3.12 0.52 -1 2 0 0.57 0.83 -1 2 0 1.96 1.06 0 2 0 109.02 7.98 0 2 0 107.27 7.91 0 2 0 106.65 7.41 0 2 0 108.74 7.15 -1 -2 0 10.92 1.64 1 2 0 9.96 1.14 1 2 0 11.47 1.39 -2 -2 0 22.19 2.71 2 2 0 22.86 2.23 2 2 0 23.90 2.15 -3 -2 0 9.48 2.20 -3 -2 0 9.55 1.11 3 2 0 8.52 1.51 3 2 0 7.91 1.43 -4 -2 0 115.24 8.28 -4 -2 0 123.99 9.82 4 2 0 102.99 8.19 4 2 0 116.26 8.47 -5 -2 0 11.64 1.91 -5 -2 0 15.51 3.27 5 2 0 13.89 2.12 5 2 0 12.17 2.26 -6 -2 0 73.80 7.41 -6 -2 0 67.85 5.69 6 2 0 63.71 5.82 6 2 0 58.23 5.29 -7 -2 0 43.80 4.39 -7 -2 0 29.72 5.80 7 2 0 39.99 3.92 7 2 0 40.83 4.53 -8 -2 0 30.35 6.27 8 2 0 32.80 3.59 8 2 0 33.36 4.27 -9 -2 0 -2.43 1.50 9 2 0 1.57 1.74 -10 -2 0 17.00 5.25 10 2 0 19.33 4.02 -11 -2 0 10.64 4.64 11 2 0 15.95 3.99 -12 -2 0 1.72 3.35 12 2 0 1.44 2.04 11 -3 0 22.78 5.12 -11 3 0 24.85 7.09 10 -3 0 22.13 4.82 -10 3 0 17.42 5.82 9 -3 0 12.73 4.06 9 -3 0 8.57 3.04 -9 3 0 8.29 4.10 8 -3 0 4.51 2.24 -8 3 0 7.23 3.60 7 -3 0 52.57 5.75 -7 3 0 57.30 7.50 -7 3 0 50.11 6.66 6 -3 0 63.48 6.41 -6 3 0 79.28 8.51 -6 3 0 76.58 8.03 5 -3 0 8.47 2.09 -5 3 0 5.44 2.33 -5 3 0 5.77 2.44 4 -3 0 29.85 3.41 -4 3 0 23.33 4.25 -4 3 0 35.49 4.59 3 -3 0 214.71 13.88 -3 3 0 198.16 15.43 -3 3 0 185.19 15.55 2 -3 0 36.65 3.62 2 -3 0 39.88 2.98 -2 3 0 39.85 4.46 -2 3 0 49.39 4.69 -2 3 0 40.58 2.86 1 -3 0 55.52 4.45 -1 3 0 59.96 5.20 -1 3 0 57.60 4.09 -1 3 0 47.40 5.00 0 3 0 121.69 8.48 0 3 0 116.01 9.25 0 3 0 124.80 9.17 0 3 0 121.43 8.22 1 3 0 7.71 1.16 1 3 0 9.46 1.35 1 3 0 6.08 1.29 -2 -3 0 26.72 3.20 -2 -3 0 29.87 2.34 2 3 0 26.15 2.47 2 3 0 30.09 2.86 -3 -3 0 34.89 4.34 3 3 0 47.94 3.67 3 3 0 39.47 3.73 -4 -3 0 127.62 9.02 -4 -3 0 132.03 11.05 4 3 0 125.10 9.35 4 3 0 136.93 9.82 4 3 0 135.40 9.04 -5 -3 0 113.07 7.94 -5 -3 0 102.12 9.76 5 3 0 113.34 8.36 5 3 0 105.73 8.49 -6 -3 0 18.20 3.98 6 3 0 22.17 2.71 6 3 0 21.38 2.99 -7 -3 0 30.16 5.66 7 3 0 32.00 3.51 7 3 0 27.83 3.29 7 3 0 37.77 4.08 -8 -3 0 82.94 9.36 8 3 0 80.19 7.44 8 3 0 80.73 6.94 -9 -3 0 10.97 4.25 9 3 0 13.11 3.23 9 3 0 13.00 2.62 -10 -3 0 7.42 4.14 10 3 0 6.09 2.44 -11 -3 0 18.77 5.68 11 3 0 7.92 3.00 -12 -3 0 20.34 6.44 12 3 0 36.73 6.30 -13 -3 0 3.49 4.14 13 3 0 2.12 2.60 11 -4 0 8.47 3.57 -11 4 0 5.44 4.39 10 -4 0 9.67 3.54 10 -4 0 3.89 3.46 -10 4 0 5.16 3.85 9 -4 0 34.73 5.68 9 -4 0 20.63 5.42 -9 4 0 37.88 7.84 8 -4 0 52.90 6.30 -8 4 0 57.44 8.38 7 -4 0 24.09 4.24 -7 4 0 22.37 5.42 -7 4 0 31.91 6.00 6 -4 0 41.20 4.68 -6 4 0 48.74 6.51 -6 4 0 35.07 6.27 5 -4 0 132.80 10.72 -5 4 0 137.85 12.45 -5 4 0 150.61 13.01 4 -4 0 66.81 6.01 -4 4 0 73.26 7.42 -4 4 0 66.19 7.36 3 -4 0 14.16 2.41 -3 4 0 16.07 3.31 -3 4 0 15.32 3.41 2 -4 0 117.98 8.51 -2 4 0 112.55 9.75 -2 4 0 116.32 7.90 -2 4 0 110.54 9.73 1 -4 0 228.63 15.35 -1 4 0 231.49 17.08 -1 4 0 231.57 15.54 -1 4 0 225.61 17.14 0 4 0 28.41 3.32 0 4 0 24.13 2.63 0 4 0 26.93 2.57 0 4 0 30.07 3.36 1 4 0 27.77 2.60 1 4 0 24.31 3.13 1 4 0 34.23 3.19 1 4 0 26.19 2.78 -2 -4 0 287.68 21.79 -2 -4 0 312.74 22.87 2 4 0 332.13 21.82 2 4 0 343.34 20.45 -3 -4 0 128.45 10.22 -3 -4 0 128.26 8.60 3 4 0 115.51 9.25 3 4 0 120.88 8.65 -4 -4 0 21.30 3.77 4 4 0 21.92 2.59 4 4 0 23.87 2.83 -5 -4 0 70.44 7.22 5 4 0 73.09 6.07 5 4 0 63.92 5.69 -6 -4 0 56.50 6.57 6 4 0 50.31 4.98 6 4 0 51.49 5.00 -7 -4 0 5.51 2.64 7 4 0 5.18 1.65 7 4 0 4.21 1.75 -8 -4 0 5.19 3.03 8 4 0 10.54 2.64 8 4 0 14.70 2.78 -9 -4 0 44.63 8.00 9 4 0 48.60 5.69 9 4 0 53.90 5.25 -10 -4 0 6.79 3.44 10 4 0 11.60 3.36 -11 -4 0 4.04 3.73 11 4 0 21.72 4.55 -12 -4 0 6.51 4.20 12 4 0 3.80 2.50 -13 -4 0 -1.77 3.04 13 4 0 4.87 3.04 11 -5 0 40.36 7.04 -11 5 0 35.70 9.19 10 -5 0 17.35 5.59 10 -5 0 21.33 5.00 -10 5 0 22.84 6.81 9 -5 0 2.47 2.46 9 -5 0 -2.91 2.14 -9 5 0 2.14 3.25 8 -5 0 6.69 3.08 8 -5 0 5.02 2.36 -8 5 0 11.69 4.64 7 -5 0 40.73 4.95 -7 5 0 32.92 6.54 -7 5 0 45.94 7.94 6 -5 0 1.38 1.53 -6 5 0 1.02 2.10 -6 5 0 -0.23 1.44 5 -5 0 6.12 2.06 -5 5 0 7.40 2.94 -5 5 0 7.71 3.07 4 -5 0 174.19 12.84 -4 5 0 165.51 14.88 -4 5 0 182.06 15.00 3 -5 0 132.92 10.22 -3 5 0 151.26 12.25 -3 5 0 134.79 12.00 2 -5 0 0.95 1.07 -2 5 0 1.20 1.32 -2 5 0 0.78 1.31 -2 5 0 1.66 0.64 1 -5 0 2.06 1.17 -1 5 0 0.83 1.31 -1 5 0 2.48 0.85 -1 5 0 3.85 1.81 0 5 0 105.09 8.96 0 5 0 114.35 8.06 0 5 0 101.66 7.86 0 5 0 111.57 9.16 1 5 0 34.34 3.62 1 5 0 27.69 3.61 1 5 0 29.13 2.98 1 5 0 32.63 3.17 -2 -5 0 46.45 4.42 -2 -5 0 51.76 5.18 2 5 0 51.18 4.10 2 5 0 52.64 4.56 -3 -5 0 187.45 14.56 -3 -5 0 184.65 13.01 3 5 0 187.63 12.55 3 5 0 183.77 13.53 -4 -5 0 229.36 16.89 4 5 0 203.57 15.38 4 5 0 209.92 14.43 -5 -5 0 10.88 3.00 5 5 0 18.90 2.66 5 5 0 11.69 2.21 -6 -5 0 15.96 3.95 6 5 0 18.61 3.21 6 5 0 25.37 3.03 -7 -5 0 21.29 4.89 7 5 0 26.18 3.55 7 5 0 28.41 3.54 -8 -5 0 13.89 4.27 8 5 0 19.34 3.31 8 5 0 19.65 3.61 -9 -5 0 10.26 3.92 9 5 0 6.36 2.46 9 5 0 7.87 2.34 -10 -5 0 43.77 8.45 10 5 0 46.98 5.87 10 5 0 46.63 5.23 -11 -5 0 9.66 4.42 11 5 0 13.95 3.84 -12 -5 0 8.46 4.70 12 5 0 4.22 2.78 -13 -5 0 1.82 3.68 13 5 0 3.51 2.77 10 -6 0 31.85 6.01 10 -6 0 22.58 6.34 -10 6 0 24.43 7.23 9 -6 0 54.08 9.32 9 -6 0 64.22 7.38 -9 6 0 45.87 9.62 8 -6 0 1.70 2.70 8 -6 0 3.88 2.24 -8 6 0 0.59 2.50 7 -6 0 11.84 3.17 -7 6 0 10.77 4.31 6 -6 0 71.65 6.74 -6 6 0 57.57 7.89 -6 6 0 60.44 8.20 5 -6 0 36.27 4.53 -5 6 0 44.29 7.16 -5 6 0 36.50 6.50 4 -6 0 -0.28 0.95 -4 6 0 3.70 2.22 -4 6 0 -1.06 1.13 3 -6 0 17.20 2.92 -3 6 0 18.83 4.20 -3 6 0 15.57 3.83 2 -6 0 151.69 11.53 -2 6 0 156.04 13.37 -2 6 0 164.23 13.44 -2 6 0 160.38 11.06 1 -6 0 15.97 2.58 -1 6 0 9.86 1.71 -1 6 0 14.20 3.20 -1 6 0 14.30 3.18 0 6 0 5.61 1.90 0 6 0 2.47 1.46 0 6 0 2.40 1.07 1 6 0 26.57 2.92 1 6 0 21.05 3.26 1 6 0 22.75 2.76 1 6 0 27.31 3.60 -2 -6 0 101.00 8.27 2 6 0 99.38 8.10 2 6 0 107.34 7.56 -3 -6 0 51.15 5.49 -3 -6 0 47.65 4.39 3 6 0 48.36 4.72 3 6 0 51.73 4.30 -4 -6 0 77.59 5.69 -4 -6 0 68.16 7.35 4 6 0 74.07 6.67 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59.02 4.79 0 -7 0 50.23 4.70 0 7 0 48.41 5.57 0 7 0 47.64 5.53 0 7 0 50.16 4.50 1 7 0 17.23 2.42 1 7 0 10.97 2.86 1 7 0 17.23 2.69 1 7 0 17.81 3.41 -2 -7 0 91.98 8.31 2 7 0 106.86 9.13 2 7 0 105.71 7.59 2 7 0 94.36 8.00 -3 -7 0 103.85 7.70 -3 -7 0 86.45 8.53 3 7 0 96.52 7.14 3 7 0 81.05 7.61 -4 -7 0 16.04 2.19 -4 -7 0 23.01 4.19 4 7 0 16.80 2.34 4 7 0 21.98 2.97 -5 -7 0 11.31 3.35 5 7 0 20.00 2.63 5 7 0 20.11 3.42 -6 -7 0 115.03 11.34 6 7 0 131.95 9.52 6 7 0 110.03 9.92 -7 -7 0 70.41 8.45 7 7 0 67.54 6.54 7 7 0 76.03 7.07 -8 -7 0 10.64 3.84 8 7 0 20.61 3.74 8 7 0 13.33 3.00 -9 -7 0 8.56 3.67 9 7 0 7.26 2.39 9 7 0 6.10 2.42 -10 -7 0 90.21 10.71 10 7 0 79.90 8.12 10 7 0 86.35 8.34 -11 -7 0 0.66 2.91 11 7 0 6.69 2.61 11 7 0 8.08 3.19 -12 -7 0 2.32 3.30 12 7 0 -0.26 1.72 -13 -7 0 17.43 6.53 13 7 0 15.53 4.33 9 -8 0 12.44 5.06 9 -8 0 19.64 4.91 -9 8 0 14.51 5.88 8 -8 0 0.59 1.98 8 -8 0 2.20 3.06 -8 8 0 1.11 3.17 7 -8 0 12.49 3.48 7 -8 0 6.20 3.39 -7 8 0 8.26 4.04 6 -8 0 57.24 6.23 -6 8 0 46.33 8.58 5 -8 0 43.10 5.37 -5 8 0 51.97 7.28 -5 8 0 56.23 7.74 4 -8 0 17.79 3.39 -4 8 0 10.27 3.70 -4 8 0 12.52 4.03 3 -8 0 107.47 9.54 -3 8 0 138.62 12.20 -3 8 0 124.42 11.89 2 -8 0 85.77 7.56 -2 8 0 77.13 8.89 -2 8 0 90.27 6.82 -2 8 0 95.91 9.41 1 -8 0 1.77 1.28 -1 8 0 -0.60 1.22 -1 8 0 -0.48 1.37 -1 8 0 2.90 1.15 0 -8 0 59.75 5.56 0 8 0 57.29 6.53 0 8 0 57.85 6.70 0 8 0 63.18 5.44 1 8 0 107.37 9.25 1 8 0 139.63 9.94 1 8 0 128.64 11.18 -2 -8 0 27.09 3.72 2 8 0 26.34 3.13 2 8 0 30.30 4.39 2 8 0 22.20 3.19 -3 -8 0 49.51 4.56 -3 -8 0 36.54 4.96 3 8 0 34.97 3.81 3 8 0 35.47 4.22 -4 -8 0 187.61 16.18 -4 -8 0 211.09 14.40 4 8 0 181.12 14.77 4 8 0 193.61 13.73 -5 -8 0 7.66 2.78 -5 -8 0 4.68 1.21 5 8 0 5.85 2.02 5 8 0 5.76 1.73 -6 -8 0 3.72 2.18 6 8 0 4.41 1.88 6 8 0 2.84 1.58 -7 -8 0 22.58 4.95 7 8 0 22.66 3.67 7 8 0 14.82 3.41 -8 -8 0 15.10 4.60 8 8 0 27.01 4.19 8 8 0 14.23 3.43 -9 -8 0 2.50 2.57 9 8 0 -0.69 1.40 9 8 0 0.83 1.66 -10 -8 0 4.44 3.25 10 8 0 0.43 1.63 10 8 0 8.09 2.64 -11 -8 0 22.62 6.35 11 8 0 25.56 4.85 11 8 0 14.56 3.77 -12 -8 0 8.62 4.59 12 8 0 5.85 2.92 -13 -8 0 4.22 4.06 13 8 0 -0.35 2.26 8 -9 0 26.56 5.18 8 -9 0 18.13 5.86 -8 9 0 31.16 7.95 7 -9 0 -0.19 1.54 7 -9 0 -0.86 2.23 -7 9 0 0.67 3.15 6 -9 0 5.64 2.68 6 -9 0 12.18 4.27 -6 9 0 15.31 4.98 5 -9 0 70.73 7.43 -5 9 0 86.40 10.04 4 -9 0 9.82 2.66 -4 9 0 6.48 3.33 -4 9 0 10.04 3.73 3 -9 0 17.65 3.38 -3 9 0 11.42 3.80 -3 9 0 10.11 3.63 2 -9 0 166.03 12.34 -2 9 0 159.23 14.36 -2 9 0 148.69 14.36 1 -9 0 121.79 9.37 -1 9 0 98.20 10.61 -1 9 0 109.05 10.90 -1 9 0 116.86 8.84 0 -9 0 2.79 1.46 0 9 0 1.30 1.07 0 9 0 2.29 1.75 0 9 0 1.97 1.64 -1 -9 0 13.22 3.20 1 9 0 9.50 2.38 1 9 0 14.48 3.52 1 9 0 9.81 2.27 -2 -9 0 51.41 5.46 2 9 0 42.15 4.61 2 9 0 36.06 4.24 2 9 0 43.00 5.53 -3 -9 0 52.35 5.80 -3 -9 0 58.33 6.96 3 9 0 61.49 5.42 3 9 0 62.53 5.96 -4 -9 0 0.71 1.13 -4 -9 0 0.84 1.53 4 9 0 -0.03 0.98 4 9 0 1.14 1.29 -5 -9 0 34.52 4.95 5 9 0 27.02 3.50 5 9 0 29.32 4.14 -6 -9 0 38.58 6.29 6 9 0 58.05 5.40 6 9 0 55.08 5.92 -7 -9 0 1.38 2.07 7 9 0 -0.08 1.17 7 9 0 1.43 1.46 -8 -9 0 9.73 3.74 8 9 0 8.95 2.68 8 9 0 12.54 3.17 -9 -9 0 -0.75 2.23 9 9 0 0.92 1.55 9 9 0 1.28 1.67 -10 -9 0 13.35 4.54 10 9 0 7.99 2.74 10 9 0 12.21 3.31 -11 -9 0 1.88 3.02 11 9 0 0.77 1.79 11 9 0 1.19 2.01 -12 -9 0 6.97 4.35 12 9 0 6.79 3.01 12 9 0 10.41 3.54 13 9 0 17.10 4.60 8 -10 0 34.53 5.90 8 -10 0 13.38 5.62 -8 10 0 30.41 8.03 7 -10 0 26.79 5.20 7 -10 0 27.83 6.91 -7 10 0 38.89 8.30 6 -10 0 0.57 2.52 6 -10 0 13.02 3.50 -6 10 0 12.23 4.94 5 -10 0 10.95 4.18 5 -10 0 8.59 2.83 -5 10 0 6.16 3.79 4 -10 0 25.10 5.94 4 -10 0 29.24 4.68 -4 10 0 23.13 5.91 3 -10 0 9.86 2.75 -3 10 0 12.42 4.08 2 -10 0 4.50 2.10 -2 10 0 5.82 2.78 1 -10 0 65.11 6.57 -1 10 0 79.00 8.42 -1 10 0 67.23 6.03 0 -10 0 89.61 8.32 0 -10 0 60.36 6.22 0 10 0 60.98 5.84 0 10 0 53.56 7.10 -1 -10 0 2.56 2.05 1 10 0 3.92 1.78 1 10 0 3.53 1.77 1 10 0 1.46 2.07 -2 -10 0 11.90 2.97 2 10 0 5.05 2.49 2 10 0 7.89 2.27 2 10 0 8.49 2.35 -3 -10 0 37.72 5.47 -3 -10 0 40.79 4.84 3 10 0 33.35 4.33 3 10 0 32.34 4.05 -4 -10 0 2.10 1.98 -4 -10 0 4.77 1.83 4 10 0 1.97 1.37 4 10 0 3.05 1.73 -5 -10 0 48.35 6.48 5 10 0 44.09 5.35 5 10 0 42.64 4.71 -6 -10 0 0.79 1.95 6 10 0 -0.13 1.22 6 10 0 2.78 1.80 -7 -10 0 46.44 6.81 7 10 0 64.05 5.83 7 10 0 42.28 5.64 -8 -10 0 5.00 3.04 8 10 0 6.25 2.38 8 10 0 3.20 1.87 -9 -10 0 0.34 2.37 9 10 0 -0.29 1.50 9 10 0 -1.10 1.39 -10 -10 0 49.21 8.76 10 10 0 30.18 5.58 10 10 0 34.29 5.55 -11 -10 0 26.39 6.82 11 10 0 9.79 3.25 11 10 0 10.17 3.36 -12 -10 0 10.96 5.09 12 10 0 15.44 4.28 12 10 0 19.61 4.60 7 -11 0 3.57 3.55 -7 11 0 -2.18 2.81 6 -11 0 30.89 5.36 6 -11 0 17.95 5.97 -6 11 0 21.27 6.30 5 -11 0 18.06 5.29 5 -11 0 15.35 3.81 -5 11 0 17.26 5.58 4 -11 0 -1.57 1.90 4 -11 0 -0.14 1.53 -4 11 0 1.41 2.57 3 -11 0 7.14 3.60 3 -11 0 1.81 1.74 -3 11 0 2.92 2.67 2 -11 0 4.55 2.99 2 -11 0 3.33 2.04 -2 11 0 0.01 1.94 1 -11 0 57.51 6.10 1 -11 0 72.09 8.14 -1 11 0 50.08 7.38 0 -11 0 -0.15 1.75 0 -11 0 1.78 1.53 0 11 0 0.75 1.08 0 11 0 1.85 1.99 -1 -11 0 19.35 3.61 -1 -11 0 29.02 5.18 1 11 0 24.68 3.40 1 11 0 10.23 3.63 -2 -11 0 29.91 5.37 2 11 0 30.04 4.11 2 11 0 34.58 4.36 2 11 0 38.15 5.50 -3 -11 0 29.59 4.31 -3 -11 0 21.71 4.95 3 11 0 23.41 4.09 3 11 0 19.53 3.67 -4 -11 0 34.60 4.75 -4 -11 0 43.35 6.09 4 11 0 57.23 5.67 4 11 0 34.61 4.45 -5 -11 0 28.90 6.05 5 11 0 31.54 4.50 5 11 0 33.03 4.13 -6 -11 0 29.44 6.13 6 11 0 30.13 4.18 6 11 0 40.18 5.02 -7 -11 0 -0.78 1.80 7 11 0 4.98 2.19 7 11 0 1.33 1.52 -8 -11 0 43.18 7.90 8 11 0 55.09 5.78 8 11 0 37.25 5.44 -9 -11 0 23.55 6.36 9 11 0 25.65 4.61 9 11 0 19.09 4.40 -10 -11 0 4.33 3.28 10 11 0 6.22 2.88 10 11 0 1.54 2.16 -11 -11 0 10.85 4.67 11 11 0 5.77 2.90 11 11 0 9.40 3.53 -12 -11 0 10.16 4.96 12 11 0 21.98 4.81 12 11 0 23.18 4.90 6 -12 0 0.95 2.95 -6 12 0 3.94 4.11 5 -12 0 21.92 6.24 -5 12 0 28.90 7.02 4 -12 0 47.25 8.65 -4 12 0 45.50 8.70 3 -12 0 14.64 3.51 3 -12 0 7.07 3.58 -3 12 0 16.66 5.20 2 -12 0 2.29 2.53 2 -12 0 3.13 2.08 -2 12 0 1.38 2.70 1 -12 0 27.96 6.15 1 -12 0 36.58 4.67 -1 12 0 20.11 5.49 0 -12 0 42.91 7.15 0 -12 0 30.63 5.05 0 12 0 45.39 4.68 0 12 0 29.72 6.27 -1 -12 0 3.36 2.50 -1 -12 0 3.32 1.96 1 12 0 4.34 1.94 1 12 0 4.56 2.81 -2 -12 0 7.78 3.02 2 12 0 12.27 2.96 2 12 0 11.28 2.94 2 12 0 10.64 3.65 -3 -12 0 68.21 7.57 -3 -12 0 69.07 8.56 3 12 0 65.21 6.71 3 12 0 74.59 7.28 -4 -12 0 32.97 4.74 -4 -12 0 23.53 5.55 4 12 0 36.96 4.78 4 12 0 38.79 4.63 -5 -12 0 6.11 3.12 5 12 0 2.89 1.92 5 12 0 1.58 1.67 -6 -12 0 67.69 8.46 6 12 0 54.73 6.83 6 12 0 70.22 6.69 -7 -12 0 24.77 5.91 7 12 0 24.03 4.63 7 12 0 19.53 3.99 -8 -12 0 0.42 2.46 8 12 0 -0.42 1.62 8 12 0 1.78 1.95 -9 -12 0 4.76 3.28 9 12 0 5.26 2.59 9 12 0 10.96 3.24 -10 -12 0 39.33 8.40 10 12 0 49.01 6.13 -11 -12 0 9.90 4.72 11 12 0 6.95 3.17 11 12 0 10.57 3.49 -12 -12 0 1.00 3.44 12 12 0 1.32 2.52 12 12 0 2.03 2.41 5 -13 0 5.84 3.81 -5 13 0 2.16 3.88 4 -13 0 3.31 3.52 -4 13 0 1.48 3.23 3 -13 0 46.99 8.94 -3 13 0 72.19 9.57 2 -13 0 16.32 4.94 -2 13 0 19.23 5.54 1 -13 0 -1.63 2.22 -1 13 0 -1.41 1.77 0 -13 0 95.75 10.76 0 13 0 96.30 11.00 -1 -13 0 57.77 7.36 1 13 0 48.11 5.55 1 13 0 45.12 7.00 -2 -13 0 4.61 2.64 2 13 0 5.48 2.25 2 13 0 8.42 3.48 -3 -13 0 3.62 2.43 -3 -13 0 0.55 2.23 3 13 0 2.80 2.22 3 13 0 2.77 2.03 -4 -13 0 63.94 8.37 4 13 0 52.01 6.43 4 13 0 66.53 6.72 -5 -13 0 33.94 7.05 5 13 0 39.03 4.97 5 13 0 37.72 5.25 -6 -13 0 1.48 2.36 6 13 0 1.20 1.76 6 13 0 -0.41 1.55 -7 -13 0 26.60 6.25 7 13 0 20.39 4.11 7 13 0 11.65 3.47 -8 -13 0 17.36 5.29 8 13 0 10.26 3.31 8 13 0 19.30 4.34 -9 -13 0 8.19 4.34 9 13 0 4.84 2.80 9 13 0 7.59 2.70 -10 -13 0 2.47 3.46 10 13 0 -0.93 1.85 10 13 0 -0.69 2.04 -11 -13 0 9.58 5.02 11 13 0 5.88 2.87 11 13 0 1.62 2.49 4 -14 0 13.89 5.32 -4 14 0 11.37 5.39 3 -14 0 0.16 2.87 -3 14 0 -1.31 3.00 2 -14 0 3.92 3.48 -2 14 0 2.60 3.24 1 -14 0 66.08 9.39 -1 14 0 65.67 9.07 0 -14 0 -0.99 2.21 0 14 0 -1.16 1.81 -1 -14 0 46.77 8.05 1 14 0 42.37 8.14 1 14 0 54.34 6.00 -2 -14 0 34.30 6.57 2 14 0 40.15 7.74 2 14 0 50.74 5.71 -3 -14 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3.98 1 -8 -16 -1.73 3.04 -1 8 16 0.19 3.23 0 -8 -16 0.72 3.05 0 8 16 -0.95 2.64 -1 -8 -16 6.61 4.07 1 8 16 8.85 4.69 -2 -8 -16 0.33 2.94 2 8 16 3.93 3.05 -3 -8 -16 30.86 7.30 3 8 16 27.39 6.94 -4 -8 -16 0.06 3.04 4 8 16 0.74 2.86 -5 -8 -16 35.45 7.91 5 8 16 19.28 5.91 -6 -8 -16 8.48 4.61 6 8 16 12.58 5.16 0 -9 -16 21.52 7.03 0 9 16 42.52 8.46 -1 -9 -16 14.50 5.46 1 9 16 7.31 4.63 -2 -9 -16 12.72 5.38 2 9 16 15.35 5.58 -3 -9 -16 25.06 6.85 3 9 16 23.04 6.57 -4 -9 -16 7.30 4.35 4 9 16 13.39 4.96 -5 -9 -16 -0.63 3.25 5 9 16 5.80 3.98 -6 -9 -16 14.74 5.61 1 10 16 59.82 10.32 -2 -10 -16 13.79 5.67 2 10 16 18.63 6.02 -3 -10 -16 1.33 3.40 3 10 16 6.61 4.19 -4 -10 -16 20.29 6.63 1 6 -17 12.34 4.94 1 6 -17 4.19 3.95 -1 -6 17 22.63 6.79 0 6 -17 19.43 6.12 0 -6 17 16.25 6.21 0 -6 17 20.50 5.91 3 5 -17 15.20 5.30 2 5 -17 3.51 3.94 2 5 -17 10.26 4.34 -2 -5 17 1.71 3.79 1 5 -17 0.25 2.80 1 5 -17 4.80 3.74 -1 -5 17 1.54 3.68 0 5 -17 15.47 5.68 0 -5 17 15.69 5.97 -1 5 -17 28.78 7.40 1 -5 17 34.29 6.86 1 -5 17 27.78 7.56 2 -5 17 4.64 3.56 2 -5 17 3.78 4.44 3 4 -17 3.13 3.11 3 4 -17 4.48 3.49 -3 -4 17 1.54 3.51 2 4 -17 18.17 5.31 2 4 -17 22.15 6.14 -2 -4 17 21.69 6.70 1 4 -17 25.03 6.64 1 4 -17 16.38 5.18 -1 -4 17 20.24 6.31 0 4 -17 27.49 7.01 0 -4 17 30.10 7.56 -1 4 -17 26.51 6.89 1 -4 17 17.10 5.08 1 -4 17 19.64 6.34 -2 4 -17 7.48 4.60 2 -4 17 8.42 4.03 2 -4 17 10.36 5.12 3 -4 17 22.16 6.66 3 -4 17 10.62 4.39 -4 -3 17 10.31 5.23 3 3 -17 24.20 6.33 -3 -3 17 8.53 4.85 2 3 -17 -1.20 2.84 -2 -3 17 2.72 3.86 1 3 -17 20.39 6.01 1 3 -17 13.33 4.49 -1 -3 17 34.94 7.74 0 3 -17 18.77 5.77 0 -3 17 20.90 6.64 -1 3 -17 25.46 6.96 1 -3 17 14.97 4.54 1 -3 17 27.47 7.03 -2 3 -17 1.89 3.43 2 -3 17 1.29 3.00 2 -3 17 -2.47 3.07 -3 3 -17 15.12 6.04 3 -3 17 15.24 5.55 3 -3 17 17.04 5.37 4 -3 17 1.28 4.04 4 -3 17 5.36 3.15 4 2 -17 -0.42 3.11 -4 -2 17 -0.29 3.82 3 2 -17 20.57 5.97 -3 -2 17 23.26 7.13 2 2 -17 18.23 5.58 -2 -2 17 17.82 6.23 1 2 -17 0.03 2.91 -1 -2 17 1.83 3.26 0 2 -17 -2.21 2.22 0 -2 17 -2.15 2.98 -1 2 -17 10.17 4.72 1 -2 17 17.06 5.80 -2 2 -17 8.37 4.29 2 -2 17 15.61 5.56 -3 2 -17 -0.93 2.97 3 -2 17 4.48 4.20 -4 2 -17 1.75 3.46 4 -2 17 1.03 3.77 4 1 -17 17.21 6.17 -4 -1 17 23.36 7.15 3 1 -17 11.90 4.93 -3 -1 17 5.68 4.68 2 1 -17 7.56 4.14 -2 -1 17 6.44 4.38 1 1 -17 14.65 5.51 -1 -1 17 12.78 5.32 0 1 -17 20.33 6.07 0 -1 17 24.30 6.77 -1 1 -17 -3.30 2.20 1 -1 17 -1.15 2.36 -2 1 -17 6.66 4.32 2 -1 17 6.46 4.27 -3 1 -17 78.02 11.01 3 -1 17 95.01 11.89 -4 1 -17 14.29 5.58 4 -1 17 31.63 7.55 5 -1 17 -0.29 3.31 4 0 -17 3.73 3.77 -4 0 17 2.74 4.15 3 0 -17 21.68 6.42 -3 0 17 30.51 7.76 2 0 -17 58.12 10.24 -2 0 17 52.93 9.95 1 0 -17 2.96 3.58 -1 0 17 1.31 3.03 0 0 -17 13.52 5.10 0 0 17 18.34 5.76 -1 0 -17 30.13 7.20 1 0 17 28.35 7.36 -2 0 -17 -0.03 2.54 2 0 17 7.50 4.20 -3 0 -17 6.17 3.88 3 0 17 16.90 6.25 -4 0 -17 30.36 7.52 4 0 17 20.00 6.30 -5 0 -17 10.60 4.69 5 0 17 12.22 5.39 4 -1 -17 12.23 5.18 -4 1 17 9.23 5.08 3 -1 -17 2.48 3.58 -3 1 17 3.65 4.28 2 -1 -17 39.19 8.43 -2 1 17 19.97 6.70 1 -1 -17 16.03 5.34 -1 1 17 14.66 5.75 0 -1 -17 -0.06 3.11 0 1 17 2.60 3.68 -1 -1 -17 27.08 7.17 1 1 17 26.56 7.03 -2 -1 -17 20.62 5.86 2 1 17 24.29 6.95 -3 -1 -17 11.44 4.83 3 1 17 15.66 5.58 -4 -1 -17 2.56 3.03 4 1 17 2.79 3.87 -5 -1 -17 3.67 4.11 5 1 17 5.77 4.45 6 1 17 3.26 3.82 4 -2 -17 31.26 8.18 -4 2 17 53.42 10.63 3 -2 -17 19.43 6.39 -3 2 17 13.57 5.72 2 -2 -17 -0.59 2.95 -2 2 17 -1.12 2.87 1 -2 -17 8.36 4.46 -1 2 17 8.60 4.83 0 -2 -17 1.47 3.14 0 2 17 1.09 3.53 -1 -2 -17 -1.22 2.10 1 2 17 -0.62 2.50 -2 -2 -17 2.36 3.39 2 2 17 -2.61 2.65 -3 -2 -17 28.70 6.88 3 2 17 19.24 6.03 -4 -2 -17 24.61 6.59 4 2 17 22.73 6.79 -5 -2 -17 -0.86 2.75 5 2 17 0.38 3.25 -6 -2 -17 1.92 3.13 6 2 17 -1.13 2.90 3 -3 -17 8.36 4.78 -3 3 17 1.86 3.90 2 -3 -17 71.85 10.32 -2 3 17 45.28 9.97 1 -3 -17 6.23 3.92 -1 3 17 7.29 4.03 0 -3 -17 3.45 4.06 0 3 17 6.12 4.18 -1 -3 -17 17.15 5.54 1 3 17 23.96 6.89 -2 -3 -17 30.96 7.52 2 3 17 48.72 8.86 -3 -3 -17 11.87 4.95 3 3 17 21.22 6.30 -4 -3 -17 -0.73 2.53 4 3 17 -3.52 2.38 -5 -3 -17 38.44 8.28 5 3 17 41.23 8.42 -6 -3 -17 36.98 8.33 6 3 17 23.66 6.59 3 -4 -17 1.90 3.28 -3 4 17 15.72 6.09 2 -4 -17 7.07 4.50 -2 4 17 -0.16 3.56 1 -4 -17 40.32 8.91 -1 4 17 60.38 10.52 0 -4 -17 59.29 10.15 0 4 17 40.61 8.78 -1 -4 -17 2.29 3.10 1 4 17 9.50 4.62 -2 -4 -17 17.22 5.95 2 4 17 32.36 7.57 -3 -4 -17 35.17 7.95 3 4 17 45.38 9.11 -4 -4 -17 3.17 3.50 4 4 17 16.18 5.36 -5 -4 -17 12.48 4.84 5 4 17 7.82 4.45 -6 -4 -17 26.63 7.03 6 4 17 24.62 6.85 2 -5 -17 5.90 4.08 -2 5 17 -4.75 2.97 1 -5 -17 -1.42 2.63 -1 5 17 0.77 3.36 0 -5 -17 25.13 6.69 0 5 17 11.50 5.21 -1 -5 -17 42.39 8.75 1 5 17 58.20 10.14 -2 -5 -17 12.29 5.30 2 5 17 15.27 5.63 -3 -5 -17 9.38 4.50 3 5 17 18.41 5.68 -4 -5 -17 15.30 5.68 4 5 17 24.82 6.66 -5 -5 -17 5.27 3.70 5 5 17 8.39 4.54 -6 -5 -17 4.26 3.80 6 5 17 -2.16 2.90 1 -6 -17 18.82 5.99 -1 6 17 14.73 5.98 0 -6 -17 2.81 3.72 0 6 17 15.25 5.80 -1 -6 -17 4.01 3.66 1 6 17 2.17 3.10 -2 -6 -17 9.17 4.35 2 6 17 21.69 6.20 -3 -6 -17 16.59 5.93 3 6 17 7.93 4.18 -4 -6 -17 -0.15 3.31 4 6 17 -0.32 2.86 -5 -6 -17 11.52 5.00 5 6 17 3.29 3.92 -1 7 17 1.50 3.98 0 -7 -17 69.92 10.62 0 7 17 76.86 10.65 -1 -7 -17 18.55 6.17 1 7 17 20.22 6.53 -2 -7 -17 5.27 4.10 2 7 17 0.21 2.90 -3 -7 -17 2.20 3.81 3 7 17 1.63 3.10 -4 -7 -17 48.79 9.49 4 7 17 61.03 10.28 -5 -7 -17 6.11 4.24 5 7 17 0.44 3.13 1 8 17 47.11 9.23 -2 -8 -17 34.62 8.11 -3 -8 -17 -1.29 2.82 3 8 17 -0.74 3.20 -4 -8 -17 2.33 3.59 1 3 -18 7.40 4.27 0 3 -18 0.44 3.30 0 -3 18 -0.43 3.86 1 -3 18 29.49 7.75 2 2 -18 61.12 10.90 1 2 -18 28.48 7.14 -1 -2 18 22.26 6.90 0 2 -18 5.03 3.88 0 -2 18 9.23 4.91 -1 2 -18 11.32 5.01 1 -2 18 11.84 5.30 2 -2 18 29.59 7.95 2 1 -18 24.49 7.15 1 1 -18 34.77 8.14 -1 -1 18 38.15 8.72 0 1 -18 17.59 5.85 0 -1 18 14.69 6.06 -1 1 -18 2.56 3.14 1 -1 18 2.18 3.83 -2 1 -18 21.62 6.78 2 -1 18 27.87 7.30 3 -1 18 14.37 5.96 2 0 -18 3.02 3.61 -2 0 18 4.90 3.86 1 0 -18 -3.16 3.07 -1 0 18 0.00 3.38 0 0 -18 6.99 4.51 0 0 18 3.95 4.00 -1 0 -18 16.10 5.77 1 0 18 15.55 5.90 -2 0 -18 9.49 4.67 2 0 18 10.25 5.17 -3 0 -18 1.23 3.43 3 0 18 2.03 3.80 2 -1 -18 15.70 5.62 1 -1 -18 15.68 5.94 -1 1 18 12.91 5.36 0 -1 -18 2.63 3.67 0 1 18 0.11 3.69 -1 -1 -18 -1.13 2.62 1 1 18 1.06 3.25 -2 -1 -18 14.12 5.45 2 1 18 29.81 7.62 -3 -1 -18 11.11 5.14 3 1 18 12.79 5.92 4 1 18 -1.46 3.54 2 -2 -18 11.79 5.71 1 -2 -18 9.77 4.94 -1 2 18 15.51 5.93 0 -2 -18 31.83 8.15 0 2 18 34.43 8.38 -1 -2 -18 42.19 8.83 1 2 18 41.10 9.05 -2 -2 -18 0.05 2.99 2 2 18 3.77 4.40 -3 -2 -18 31.59 7.74 3 2 18 25.06 6.91 4 2 18 45.21 9.57 1 -3 -18 11.78 5.31 -1 3 18 34.53 8.29 0 -3 -18 6.64 4.05 0 3 18 8.66 4.97 -1 -3 -18 24.63 6.94 1 3 18 26.97 7.52 -2 -3 -18 28.25 7.54 2 3 18 47.33 9.02 -3 -3 -18 1.88 3.29 3 3 18 2.20 3.36 4 3 18 18.27 6.39 0 -4 -18 6.71 4.14 0 4 18 6.54 4.38 -1 -4 -18 8.21 4.74 1 4 18 4.53 3.87 -2 -4 -18 5.66 3.96 2 4 18 15.00 5.78 -3 -4 -18 16.64 6.08 3 4 18 24.45 7.01 4 4 18 -1.92 2.97 -1 -5 -18 28.96 7.59 1 5 18 30.20 7.71 -2 -5 -18 4.76 4.05 2 5 18 11.08 5.28 3 5 18 -1.88 2.74 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 2124 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969301' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_3Prime _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 N3 O7 Sm' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 868.29 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sm Sm -0.1638 3.4418 '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 8.676(5) _cell_length_b 13.215(5) _cell_length_c 14.791(5) _cell_angle_alpha 100.259(5) _cell_angle_beta 98.005(5) _cell_angle_gamma 92.052(5) _cell_volume 1649.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 60873 _cell_measurement_theta_min 4.750 _cell_measurement_theta_max 55.382 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.748 _exptl_crystal_F_000 862 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 2.080 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6027 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'TWINABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 60839 _diffrn_reflns_av_unetI/netI 0.0362 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 1.415 _diffrn_reflns_theta_max 27.756 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 7768 _reflns_number_gt 7053 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. 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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0275P)^2^+0.8375P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7768 _refine_ls_number_parameters 459 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0255 _refine_ls_wR_factor_ref 0.0601 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _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 Sm1 Sm 0.06596(2) 0.01372(2) 0.70090(2) 0.00999(4) Uani 1 1 d . . . . . Cl1 Cl 0.29568(8) 0.61998(5) 1.07100(5) 0.02311(14) Uani 1 1 d . . . . . Cl3 Cl 0.70851(9) 0.52369(5) 0.74125(5) 0.02990(16) Uani 1 1 d . . . . . Cl2 Cl -0.25078(10) -0.59699(6) 0.35400(6) 0.03761(19) Uani 1 1 d . . . . . O3 O 0.0633(2) -0.12598(13) 0.56020(11) 0.0146(3) Uani 1 1 d . . . . . O2 O 0.0384(2) 0.19957(13) 0.75699(12) 0.0164(4) Uani 1 1 d . . . . . OW1 O -0.1368(2) 0.05933(15) 0.59088(12) 0.0143(4) Uani 1 1 d . . . . . O1 O 0.2136(2) 0.12762(13) 0.84543(11) 0.0150(3) Uani 1 1 d . . . . . O5 O 0.2371(2) 0.09415(13) 0.62488(12) 0.0158(4) Uani 1 1 d . . . . . O6 O 0.3533(2) 0.08153(14) 0.49792(12) 0.0189(4) Uani 1 1 d . . . . . O4 O -0.0913(2) -0.15318(13) 0.66026(11) 0.0149(3) Uani 1 1 d . . . . . N2 N 0.0726(2) -0.08603(15) 0.83970(13) 0.0116(4) Uani 1 1 d . . . . . N1 N 0.2985(2) -0.09727(15) 0.72926(13) 0.0124(4) Uani 1 1 d . . . . . N3 N -0.1594(2) 0.03875(15) 0.79928(14) 0.0138(4) Uani 1 1 d . . . . . C10 C -0.0492(3) -0.08486(18) 0.88756(16) 0.0130(5) Uani 1 1 d . . . . . C6 C 0.1817(3) -0.15447(18) 0.85145(16) 0.0135(5) Uani 1 1 d . . . . . C5 C 0.3130(3) -0.15331(18) 0.79737(16) 0.0122(5) Uani 1 1 d . . . . . C11 C -0.1701(3) -0.01106(18) 0.86997(16) 0.0128(5) Uani 1 1 d . . . . . C4 C 0.4451(3) -0.20829(19) 0.81452(17) 0.0163(5) Uani 1 1 d . . . . . H4 H 0.4544 -0.2457 0.8624 0.020 Uiso 1 1 calc R U . . . C32 C 0.3773(3) 0.29449(19) 0.68888(17) 0.0164(5) Uani 1 1 d . . . . . H32 H 0.2864 0.2783 0.7114 0.020 Uiso 1 1 calc R U . . . C24 C -0.0924(3) -0.28497(18) 0.52692(17) 0.0145(5) Uani 1 1 d . . . . . C31 C 0.4263(3) 0.22558(18) 0.61736(16) 0.0136(5) Uani 1 1 d . . . . . C23 C -0.0380(3) -0.18222(18) 0.58576(16) 0.0121(5) Uani 1 1 d . . . . . C16 C 0.1425(3) 0.20501(18) 0.82591(17) 0.0135(5) Uani 1 1 d . . . . . C1 C 0.4116(3) -0.09864(19) 0.67565(17) 0.0152(5) Uani 1 1 d . . . . . H1 H 0.3995 -0.0619 0.6273 0.018 Uiso 1 1 calc R U . . . C13 C -0.4072(3) 0.0677(2) 0.89928(18) 0.0191(5) Uani 1 1 d . . . . . H13 H -0.4901 0.0773 0.9329 0.023 Uiso 1 1 calc R U . . . C30 C 0.3323(3) 0.12620(19) 0.57618(17) 0.0143(5) Uani 1 1 d . . . . . C18 C 0.3069(3) 0.32332(19) 0.95913(17) 0.0179(5) Uani 1 1 d . . . . . H18 H 0.3665 0.2683 0.9697 0.022 Uiso 1 1 calc R U . . . C8 C 0.0466(3) -0.2226(2) 0.95990(19) 0.0224(6) Uani 1 1 d . . . . . H8 H 0.0379 -0.2685 1.0000 0.027 Uiso 1 1 calc R U . . . C20 C 0.2534(3) 0.50024(19) 0.99848(18) 0.0184(5) Uani 1 1 d . . . . . C17 C 0.1843(3) 0.30857(19) 0.88697(16) 0.0150(5) Uani 1 1 d . . . . . C36 C 0.5614(3) 0.2511(2) 0.58327(18) 0.0184(5) Uani 1 1 d . . . . . H36 H 0.5941 0.2062 0.5347 0.022 Uiso 1 1 calc R U . . . C15 C -0.2708(3) 0.10189(19) 0.77825(17) 0.0151(5) Uani 1 1 d . . . . . H15 H -0.2623 0.1371 0.7299 0.018 Uiso 1 1 calc R U . . . C3 C 0.5620(3) -0.20678(19) 0.75987(18) 0.0175(5) Uani 1 1 d . . . . . H3 H 0.6511 -0.2425 0.7710 0.021 Uiso 1 1 calc R U . . . C19 C 0.3426(3) 0.4186(2) 1.01600(18) 0.0207(5) Uani 1 1 d . . . . . H19 H 0.4246 0.4280 1.0650 0.025 Uiso 1 1 calc R U . . . C26 C -0.0757(3) -0.4166(2) 0.39376(19) 0.0235(6) Uani 1 1 d . . . . . H26 H -0.0316 -0.4411 0.3409 0.028 Uiso 1 1 calc R U . . . C12 C -0.2918(3) 0.00360(19) 0.92280(17) 0.0169(5) Uani 1 1 d . . . . . H12 H -0.2950 -0.0293 0.9731 0.020 Uiso 1 1 calc R U . . . C34 C 0.5969(3) 0.4089(2) 0.69309(18) 0.0196(5) Uani 1 1 d . . . . . C2 C 0.5446(3) -0.15158(19) 0.68853(17) 0.0168(5) Uani 1 1 d . . . . . H2 H 0.6206 -0.1501 0.6501 0.020 Uiso 1 1 calc R U . . . C9 C -0.0634(3) -0.1516(2) 0.94984(17) 0.0176(5) Uani 1 1 d . . . . . H9 H -0.1460 -0.1481 0.9839 0.021 Uiso 1 1 calc R U . . . C28 C -0.2546(3) -0.4425(2) 0.50019(19) 0.0232(6) Uani 1 1 d . . . . . H28 H -0.3314 -0.4832 0.5171 0.028 Uiso 1 1 calc R U . . . C14 C -0.3983(3) 0.1174(2) 0.82515(18) 0.0181(5) Uani 1 1 d . . . . . H14 H -0.4754 0.1599 0.8073 0.022 Uiso 1 1 calc R U . . . C35 C 0.6474(3) 0.3426(2) 0.62120(19) 0.0213(6) Uani 1 1 d . . . . . H35 H 0.7380 0.3594 0.5987 0.026 Uiso 1 1 calc R U . . . C27 C -0.1881(3) -0.4765(2) 0.42146(19) 0.0225(6) Uani 1 1 d . . . . . C22 C 0.0975(3) 0.3921(2) 0.86991(17) 0.0181(5) Uani 1 1 d . . . . . H22 H 0.0156 0.3830 0.8209 0.022 Uiso 1 1 calc R U . . . C21 C 0.1328(3) 0.4883(2) 0.92559(18) 0.0199(5) Uani 1 1 d . . . . . H21 H 0.0758 0.5441 0.9139 0.024 Uiso 1 1 calc R U . . . C33 C 0.4616(3) 0.3868(2) 0.72708(17) 0.0177(5) Uani 1 1 d . . . . . H33 H 0.4280 0.4328 0.7745 0.021 Uiso 1 1 calc R U . . . C29 C -0.2049(3) -0.3468(2) 0.55352(18) 0.0198(5) Uani 1 1 d . . . . . H29 H -0.2469 -0.3237 0.6075 0.024 Uiso 1 1 calc R U . . . C7 C 0.1700(3) -0.2252(2) 0.91017(18) 0.0198(5) Uani 1 1 d . . . . . H7 H 0.2444 -0.2736 0.9157 0.024 Uiso 1 1 calc R U . . . C25 C -0.0300(3) -0.3198(2) 0.44597(18) 0.0189(5) Uani 1 1 d . . . . . H25 H 0.0428 -0.2779 0.4269 0.023 Uiso 1 1 calc R U . . . H37 H -0.208(4) 0.014(3) 0.564(2) 0.037(10) Uiso 1 1 d . . . . . H38 H -0.114(4) 0.085(3) 0.555(2) 0.028(10) Uiso 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 Sm1 0.01059(6) 0.01072(6) 0.00917(6) 0.00244(4) 0.00265(4) -0.00001(4) Cl1 0.0288(4) 0.0153(3) 0.0223(3) -0.0001(2) -0.0021(3) 0.0016(3) Cl3 0.0349(4) 0.0210(3) 0.0324(4) 0.0018(3) 0.0069(3) -0.0089(3) Cl2 0.0471(5) 0.0185(3) 0.0380(4) -0.0061(3) -0.0100(4) -0.0018(3) O3 0.0153(9) 0.0145(8) 0.0137(8) 0.0014(7) 0.0031(7) -0.0011(7) O2 0.0164(9) 0.0150(9) 0.0180(9) 0.0032(7) 0.0028(7) 0.0007(7) OW1 0.0151(9) 0.0160(9) 0.0123(9) 0.0048(7) 0.0017(7) -0.0013(7) O1 0.0178(9) 0.0138(8) 0.0139(8) 0.0026(7) 0.0037(7) 0.0002(7) O5 0.0163(9) 0.0160(9) 0.0170(9) 0.0051(7) 0.0069(7) -0.0025(7) O6 0.0190(9) 0.0215(9) 0.0161(9) 0.0014(7) 0.0060(7) -0.0033(7) O4 0.0160(9) 0.0149(9) 0.0137(8) 0.0012(7) 0.0043(7) 0.0000(7) N2 0.0116(10) 0.0118(10) 0.0114(9) 0.0019(7) 0.0015(8) 0.0005(8) N1 0.0144(10) 0.0127(10) 0.0103(9) 0.0015(8) 0.0035(8) -0.0001(8) N3 0.0136(10) 0.0144(10) 0.0137(10) 0.0037(8) 0.0019(8) -0.0001(8) C10 0.0148(12) 0.0131(11) 0.0106(11) 0.0010(9) 0.0021(9) -0.0019(9) C6 0.0138(12) 0.0146(12) 0.0116(11) 0.0010(9) 0.0026(9) 0.0002(9) C5 0.0124(11) 0.0105(11) 0.0135(11) 0.0016(9) 0.0024(9) -0.0020(9) C11 0.0128(11) 0.0123(11) 0.0123(11) -0.0008(9) 0.0023(9) -0.0003(9) C4 0.0159(12) 0.0162(12) 0.0170(12) 0.0048(10) 0.0007(10) 0.0006(10) C32 0.0155(12) 0.0194(13) 0.0166(12) 0.0085(10) 0.0036(10) 0.0004(10) C24 0.0133(12) 0.0127(12) 0.0163(12) 0.0029(9) -0.0018(9) 0.0011(9) C31 0.0131(12) 0.0149(12) 0.0142(11) 0.0074(9) 0.0009(9) 0.0011(9) C23 0.0093(11) 0.0141(12) 0.0134(11) 0.0039(9) 0.0011(9) 0.0029(9) C16 0.0144(12) 0.0125(12) 0.0158(11) 0.0030(9) 0.0098(9) -0.0020(9) C1 0.0168(12) 0.0149(12) 0.0147(11) 0.0036(9) 0.0043(9) -0.0006(10) C13 0.0151(13) 0.0220(13) 0.0221(13) 0.0028(10) 0.0113(10) 0.0015(10) C30 0.0115(11) 0.0161(12) 0.0162(12) 0.0067(9) 0.0001(9) 0.0022(9) C18 0.0202(13) 0.0145(12) 0.0196(12) 0.0043(10) 0.0026(10) 0.0026(10) C8 0.0271(15) 0.0210(14) 0.0252(14) 0.0148(11) 0.0107(11) 0.0036(11) C20 0.0229(14) 0.0135(12) 0.0184(12) 0.0009(10) 0.0046(10) -0.0006(10) C17 0.0170(12) 0.0159(12) 0.0122(11) 0.0004(9) 0.0058(9) -0.0019(10) C36 0.0163(13) 0.0187(13) 0.0216(13) 0.0033(10) 0.0077(10) 0.0006(10) C15 0.0146(12) 0.0162(12) 0.0149(12) 0.0042(9) 0.0016(9) 0.0026(9) C3 0.0138(12) 0.0162(12) 0.0219(13) 0.0024(10) 0.0018(10) 0.0030(10) C19 0.0213(14) 0.0199(13) 0.0201(13) 0.0046(10) -0.0012(11) 0.0015(10) C26 0.0248(14) 0.0241(14) 0.0187(13) -0.0032(11) 0.0013(11) 0.0041(11) C12 0.0186(13) 0.0165(12) 0.0173(12) 0.0036(10) 0.0080(10) 0.0019(10) C34 0.0204(13) 0.0148(12) 0.0227(13) 0.0049(10) -0.0001(10) -0.0057(10) C2 0.0150(12) 0.0158(12) 0.0187(12) -0.0018(10) 0.0062(10) -0.0010(10) C9 0.0172(13) 0.0216(13) 0.0170(12) 0.0070(10) 0.0085(10) 0.0010(10) C28 0.0242(14) 0.0171(13) 0.0272(14) 0.0066(11) -0.0008(11) -0.0051(11) C14 0.0161(13) 0.0182(13) 0.0202(13) 0.0035(10) 0.0022(10) 0.0043(10) C35 0.0153(13) 0.0185(13) 0.0314(15) 0.0044(11) 0.0092(11) -0.0010(10) C27 0.0272(15) 0.0112(12) 0.0241(14) -0.0009(10) -0.0076(11) 0.0018(10) C22 0.0207(13) 0.0192(13) 0.0146(12) 0.0041(10) 0.0018(10) 0.0006(10) C21 0.0251(14) 0.0169(13) 0.0176(12) 0.0037(10) 0.0012(10) 0.0062(11) C33 0.0226(13) 0.0172(13) 0.0142(12) 0.0037(10) 0.0044(10) 0.0022(10) C29 0.0221(14) 0.0170(13) 0.0203(13) 0.0027(10) 0.0039(11) 0.0000(10) C7 0.0204(13) 0.0205(13) 0.0223(13) 0.0107(11) 0.0066(11) 0.0058(10) C25 0.0167(13) 0.0202(13) 0.0189(13) 0.0014(10) 0.0022(10) 0.0014(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O5 2.3188(18) . ? Sm1 OW1 2.3946(19) . ? Sm1 O2 2.4795(19) . ? Sm1 O4 2.4844(19) . ? Sm1 O3 2.5210(18) . ? Sm1 O1 2.5355(18) . ? Sm1 N1 2.568(2) . ? Sm1 N3 2.592(2) . ? Sm1 N2 2.625(2) . ? Sm1 C16 2.850(3) . ? Sm1 C23 2.873(3) . ? Cl1 C20 1.742(3) . ? Cl3 C34 1.750(3) . ? Cl2 C27 1.746(3) . ? O3 C23 1.270(3) . ? O2 C16 1.254(3) . ? OW1 H37 0.85(4) . ? OW1 H38 0.73(4) . ? O1 C16 1.269(3) . ? O5 C30 1.277(3) . ? O6 C30 1.243(3) . ? O4 C23 1.257(3) . ? N2 C6 1.348(3) . ? N2 C10 1.350(3) . ? N1 C1 1.343(3) . ? N1 C5 1.348(3) . ? N3 C15 1.339(3) . ? N3 C11 1.343(3) . ? C10 C9 1.398(3) . ? C10 C11 1.485(3) . ? C6 C7 1.395(3) . ? C6 C5 1.481(3) . ? C5 C4 1.397(3) . ? C11 C12 1.398(3) . ? C4 C3 1.384(4) . ? C4 H4 0.9300 . ? C32 C33 1.385(4) . ? C32 C31 1.393(3) . ? C32 H32 0.9300 . ? C24 C29 1.392(4) . ? C24 C25 1.393(3) . ? C24 C23 1.498(3) . ? C31 C36 1.392(3) . ? C31 C30 1.504(3) . ? C16 C17 1.501(3) . ? C1 C2 1.379(4) . ? C1 H1 0.9300 . ? C13 C12 1.382(4) . ? C13 C14 1.384(4) . ? C13 H13 0.9300 . ? C18 C17 1.380(4) . ? C18 C19 1.383(4) . ? C18 H18 0.9300 . ? C8 C9 1.373(4) . ? C8 C7 1.379(4) . ? C8 H8 0.9300 . ? C20 C21 1.377(4) . ? C20 C19 1.390(4) . ? C17 C22 1.398(4) . ? C36 C35 1.383(4) . ? C36 H36 0.9300 . ? C15 C14 1.388(4) . ? C15 H15 0.9300 . ? C3 C2 1.381(4) . ? C3 H3 0.9300 . ? C19 H19 0.9300 . ? C26 C27 1.384(4) . ? C26 C25 1.385(4) . ? C26 H26 0.9300 . ? C12 H12 0.9300 . ? C34 C33 1.381(4) . ? C34 C35 1.384(4) . ? C2 H2 0.9300 . ? C9 H9 0.9300 . ? C28 C27 1.382(4) . ? C28 C29 1.385(4) . ? C28 H28 0.9300 . ? C14 H14 0.9300 . ? C35 H35 0.9300 . ? C22 C21 1.385(4) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? C33 H33 0.9300 . ? C29 H29 0.9300 . ? C7 H7 0.9300 . ? C25 H25 0.9300 . ? 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 Sm1 OW1 86.04(7) . . ? O5 Sm1 O2 76.66(6) . . ? OW1 Sm1 O2 75.54(6) . . ? O5 Sm1 O4 133.19(6) . . ? OW1 Sm1 O4 81.21(7) . . ? O2 Sm1 O4 140.62(6) . . ? O5 Sm1 O3 81.21(6) . . ? OW1 Sm1 O3 76.86(6) . . ? O2 Sm1 O3 145.51(6) . . ? O4 Sm1 O3 52.07(6) . . ? O5 Sm1 O1 83.91(6) . . ? OW1 Sm1 O1 127.99(6) . . ? O2 Sm1 O1 52.47(6) . . ? O4 Sm1 O1 137.76(5) . . ? O3 Sm1 O1 149.95(6) . . ? O5 Sm1 N1 82.06(7) . . ? OW1 Sm1 N1 147.08(6) . . ? O2 Sm1 N1 130.23(6) . . ? O4 Sm1 N1 84.84(7) . . ? O3 Sm1 N1 71.06(6) . . ? O1 Sm1 N1 81.15(6) . . ? O5 Sm1 N3 145.41(6) . . ? OW1 Sm1 N3 78.97(7) . . ? O2 Sm1 N3 69.50(6) . . ? O4 Sm1 N3 75.19(6) . . ? O3 Sm1 N3 124.31(6) . . ? O1 Sm1 N3 81.24(7) . . ? N1 Sm1 N3 125.73(7) . . ? O5 Sm1 N2 139.44(6) . . ? OW1 Sm1 N2 134.51(7) . . ? O2 Sm1 N2 109.81(6) . . ? O4 Sm1 N2 66.55(6) . . ? O3 Sm1 N2 104.24(6) . . ? O1 Sm1 N2 71.58(6) . . ? N1 Sm1 N2 62.97(6) . . ? N3 Sm1 N2 62.76(6) . . ? O5 Sm1 C16 78.55(7) . . ? OW1 Sm1 C16 101.59(7) . . ? O2 Sm1 C16 26.04(6) . . ? O4 Sm1 C16 148.13(6) . . ? O3 Sm1 C16 159.76(6) . . ? O1 Sm1 C16 26.44(6) . . ? N1 Sm1 C16 105.90(7) . . ? N3 Sm1 C16 74.27(7) . . ? N2 Sm1 C16 91.28(7) . . ? O5 Sm1 C23 107.38(7) . . ? OW1 Sm1 C23 77.71(7) . . ? O2 Sm1 C23 152.60(6) . . ? O4 Sm1 C23 25.86(6) . . ? O3 Sm1 C23 26.21(6) . . ? O1 Sm1 C23 153.37(6) . . ? N1 Sm1 C23 76.81(7) . . ? N3 Sm1 C23 99.67(7) . . ? N2 Sm1 C23 85.08(7) . . ? C16 Sm1 C23 173.89(6) . . ? C23 O3 Sm1 92.55(14) . . ? C16 O2 Sm1 93.70(14) . . ? Sm1 OW1 H37 119(2) . . ? Sm1 OW1 H38 118(3) . . ? H37 OW1 H38 106(3) . . ? C16 O1 Sm1 90.74(14) . . ? C30 O5 Sm1 172.10(16) . . ? C23 O4 Sm1 94.60(14) . . ? C6 N2 C10 118.9(2) . . ? C6 N2 Sm1 119.62(15) . . ? C10 N2 Sm1 120.13(15) . . ? C1 N1 C5 118.4(2) . . ? C1 N1 Sm1 119.26(16) . . ? C5 N1 Sm1 122.33(15) . . ? C15 N3 C11 118.6(2) . . ? C15 N3 Sm1 119.25(16) . . ? C11 N3 Sm1 122.15(16) . . ? N2 C10 C9 121.6(2) . . ? N2 C10 C11 117.3(2) . . ? C9 C10 C11 121.1(2) . . ? N2 C6 C7 121.6(2) . . ? N2 C6 C5 117.1(2) . . ? C7 C6 C5 121.2(2) . . ? N1 C5 C4 121.0(2) . . ? N1 C5 C6 116.7(2) . . ? C4 C5 C6 122.2(2) . . ? N3 C11 C12 121.6(2) . . ? N3 C11 C10 116.9(2) . . ? C12 C11 C10 121.5(2) . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C33 C32 C31 121.1(2) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C29 C24 C25 119.6(2) . . ? C29 C24 C23 120.0(2) . . ? C25 C24 C23 120.4(2) . . ? C36 C31 C32 119.1(2) . . ? C36 C31 C30 120.6(2) . . ? C32 C31 C30 120.3(2) . . ? O4 C23 O3 120.8(2) . . ? O4 C23 C24 119.8(2) . . ? O3 C23 C24 119.4(2) . . ? O4 C23 Sm1 59.54(12) . . ? O3 C23 Sm1 61.24(12) . . ? C24 C23 Sm1 179.21(17) . . ? O2 C16 O1 123.0(2) . . ? O2 C16 C17 117.7(2) . . ? O1 C16 C17 119.2(2) . . ? O2 C16 Sm1 60.25(12) . . ? O1 C16 Sm1 62.82(12) . . ? C17 C16 Sm1 176.65(16) . . ? N1 C1 C2 123.5(2) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C12 C13 C14 119.4(2) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? O6 C30 O5 125.1(2) . . ? O6 C30 C31 117.8(2) . . ? O5 C30 C31 117.1(2) . . ? C17 C18 C19 121.0(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C9 C8 C7 119.6(2) . . ? C9 C8 H8 120.2 . . ? C7 C8 H8 120.2 . . ? C21 C20 C19 121.5(2) . . ? C21 C20 Cl1 119.5(2) . . ? C19 C20 Cl1 118.9(2) . . ? C18 C17 C22 119.3(2) . . ? C18 C17 C16 121.5(2) . . ? C22 C17 C16 119.2(2) . . ? C35 C36 C31 120.4(2) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? N3 C15 C14 123.2(2) . . ? N3 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C2 C3 C4 119.1(2) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C18 C19 C20 118.7(2) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C27 C26 C25 119.0(3) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C13 C12 C11 119.1(2) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C33 C34 C35 121.8(2) . . ? C33 C34 Cl3 119.7(2) . . ? C35 C34 Cl3 118.5(2) . . ? C1 C2 C3 118.3(2) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C8 C9 C10 119.0(2) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C27 C28 C29 118.9(3) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C13 C14 C15 118.1(2) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C36 C35 C34 119.2(2) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C28 C27 C26 121.7(2) . . ? C28 C27 Cl2 119.0(2) . . ? C26 C27 Cl2 119.2(2) . . ? C21 C22 C17 120.4(2) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? C20 C21 C22 119.0(2) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C34 C33 C32 118.4(2) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C28 C29 C24 120.4(3) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C8 C7 C6 119.1(2) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C26 C25 C24 120.3(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? _refine_diff_density_max 0.850 _refine_diff_density_min -0.672 _refine_diff_density_rms 0.096 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1_twin in P-1 CELL 0.71073 8.6760 13.2150 14.7910 100.259 98.005 92.052 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N O CL SM UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 BOND $H ACTA 51.00 L.S. 10 WGHT 0.027500 0.837500 FVAR 0.12278 SM1 6 0.065957 0.013724 0.700904 11.00000 0.01059 0.01072 = 0.00917 0.00244 0.00265 -0.00001 CL1 5 0.295677 0.619975 1.071001 11.00000 0.02879 0.01527 = 0.02226 -0.00012 -0.00208 0.00164 CL3 5 0.708509 0.523689 0.741249 11.00000 0.03490 0.02102 = 0.03238 0.00175 0.00691 -0.00894 CL2 5 -0.250781 -0.596993 0.354001 11.00000 0.04708 0.01849 = 0.03802 -0.00608 -0.01002 -0.00178 O3 4 0.063279 -0.125981 0.560198 11.00000 0.01530 0.01448 = 0.01367 0.00135 0.00313 -0.00112 O2 4 0.038423 0.199566 0.756986 11.00000 0.01637 0.01501 = 0.01798 0.00316 0.00283 0.00071 OW1 4 -0.136792 0.059332 0.590877 11.00000 0.01510 0.01602 = 0.01233 0.00477 0.00170 -0.00126 O1 4 0.213571 0.127618 0.845429 11.00000 0.01775 0.01379 = 0.01392 0.00261 0.00374 0.00015 O5 4 0.237115 0.094151 0.624879 11.00000 0.01628 0.01595 = 0.01704 0.00513 0.00694 -0.00248 O6 4 0.353289 0.081531 0.497919 11.00000 0.01896 0.02153 = 0.01606 0.00141 0.00602 -0.00332 O4 4 -0.091349 -0.153176 0.660265 11.00000 0.01600 0.01491 = 0.01369 0.00123 0.00431 -0.00005 N2 3 0.072556 -0.086034 0.839704 11.00000 0.01158 0.01181 = 0.01137 0.00193 0.00148 0.00049 N1 3 0.298475 -0.097265 0.729256 11.00000 0.01442 0.01269 = 0.01026 0.00148 0.00353 -0.00011 N3 3 -0.159450 0.038755 0.799277 11.00000 0.01359 0.01436 = 0.01368 0.00366 0.00186 -0.00009 C10 1 -0.049243 -0.084863 0.887559 11.00000 0.01483 0.01307 = 0.01060 0.00098 0.00211 -0.00189 C6 1 0.181718 -0.154471 0.851449 11.00000 0.01383 0.01456 = 0.01165 0.00102 0.00262 0.00023 C5 1 0.312960 -0.153306 0.797371 11.00000 0.01239 0.01053 = 0.01346 0.00160 0.00238 -0.00198 C11 1 -0.170104 -0.011060 0.869967 11.00000 0.01283 0.01232 = 0.01228 -0.00075 0.00225 -0.00032 C4 1 0.445076 -0.208287 0.814524 11.00000 0.01586 0.01619 = 0.01703 0.00479 0.00074 0.00064 AFIX 43 H4 2 0.454441 -0.245718 0.862424 11.00000 -1.20000 AFIX 0 C32 1 0.377262 0.294489 0.688877 11.00000 0.01550 0.01936 = 0.01657 0.00846 0.00364 0.00040 AFIX 43 H32 2 0.286366 0.278251 0.711361 11.00000 -1.20000 AFIX 0 C24 1 -0.092407 -0.284967 0.526921 11.00000 0.01335 0.01271 = 0.01633 0.00290 -0.00180 0.00110 C31 1 0.426334 0.225579 0.617356 11.00000 0.01309 0.01495 = 0.01415 0.00742 0.00094 0.00110 C23 1 -0.038021 -0.182219 0.585760 11.00000 0.00934 0.01411 = 0.01342 0.00389 0.00106 0.00286 C16 1 0.142471 0.205006 0.825908 11.00000 0.01437 0.01251 = 0.01580 0.00302 0.00980 -0.00203 C1 1 0.411551 -0.098643 0.675646 11.00000 0.01681 0.01490 = 0.01472 0.00362 0.00425 -0.00056 AFIX 43 H1 2 0.399484 -0.061937 0.627259 11.00000 -1.20000 AFIX 0 C13 1 -0.407215 0.067665 0.899278 11.00000 0.01511 0.02201 = 0.02212 0.00277 0.01126 0.00150 AFIX 43 H13 2 -0.490120 0.077302 0.932922 11.00000 -1.20000 AFIX 0 C30 1 0.332333 0.126196 0.576178 11.00000 0.01154 0.01611 = 0.01620 0.00671 0.00010 0.00224 C18 1 0.306933 0.323319 0.959135 11.00000 0.02021 0.01447 = 0.01959 0.00427 0.00261 0.00256 AFIX 43 H18 2 0.366529 0.268313 0.969681 11.00000 -1.20000 AFIX 0 C8 1 0.046580 -0.222555 0.959898 11.00000 0.02711 0.02100 = 0.02519 0.01484 0.01073 0.00359 AFIX 43 H8 2 0.037885 -0.268537 1.000027 11.00000 -1.20000 AFIX 0 C20 1 0.253433 0.500242 0.998483 11.00000 0.02292 0.01353 = 0.01842 0.00093 0.00464 -0.00059 C17 1 0.184265 0.308566 0.886972 11.00000 0.01700 0.01587 = 0.01224 0.00041 0.00582 -0.00191 C36 1 0.561432 0.251066 0.583267 11.00000 0.01627 0.01866 = 0.02159 0.00332 0.00773 0.00057 AFIX 43 H36 2 0.594077 0.206226 0.534677 11.00000 -1.20000 AFIX 0 C15 1 -0.270782 0.101887 0.778253 11.00000 0.01463 0.01624 = 0.01486 0.00423 0.00162 0.00263 AFIX 43 H15 2 -0.262275 0.137083 0.729862 11.00000 -1.20000 AFIX 0 C3 1 0.562005 -0.206781 0.759868 11.00000 0.01377 0.01621 = 0.02194 0.00244 0.00176 0.00296 AFIX 43 H3 2 0.651065 -0.242455 0.771045 11.00000 -1.20000 AFIX 0 C19 1 0.342584 0.418637 1.015996 11.00000 0.02134 0.01987 = 0.02009 0.00461 -0.00120 0.00147 AFIX 43 H19 2 0.424594 0.427958 1.064990 11.00000 -1.20000 AFIX 0 C26 1 -0.075717 -0.416649 0.393758 11.00000 0.02475 0.02407 = 0.01867 -0.00320 0.00130 0.00408 AFIX 43 H26 2 -0.031577 -0.441107 0.340888 11.00000 -1.20000 AFIX 0 C12 1 -0.291796 0.003601 0.922801 11.00000 0.01857 0.01646 = 0.01730 0.00359 0.00797 0.00185 AFIX 43 H12 2 -0.295042 -0.029336 0.973135 11.00000 -1.20000 AFIX 0 C34 1 0.596865 0.408930 0.693092 11.00000 0.02036 0.01478 = 0.02268 0.00491 -0.00010 -0.00570 C2 1 0.544581 -0.151583 0.688526 11.00000 0.01500 0.01581 = 0.01871 -0.00177 0.00624 -0.00098 AFIX 43 H2 2 0.620597 -0.150137 0.650142 11.00000 -1.20000 AFIX 0 C9 1 -0.063360 -0.151648 0.949836 11.00000 0.01719 0.02159 = 0.01702 0.00699 0.00855 0.00104 AFIX 43 H9 2 -0.145989 -0.148074 0.983919 11.00000 -1.20000 AFIX 0 C28 1 -0.254566 -0.442500 0.500191 11.00000 0.02424 0.01714 = 0.02721 0.00658 -0.00083 -0.00513 AFIX 43 H28 2 -0.331364 -0.483227 0.517104 11.00000 -1.20000 AFIX 0 C14 1 -0.398251 0.117365 0.825150 11.00000 0.01608 0.01820 = 0.02021 0.00355 0.00217 0.00426 AFIX 43 H14 2 -0.475442 0.159906 0.807294 11.00000 -1.20000 AFIX 0 C35 1 0.647371 0.342624 0.621199 11.00000 0.01530 0.01855 = 0.03142 0.00441 0.00921 -0.00101 AFIX 43 H35 2 0.737973 0.359447 0.598691 11.00000 -1.20000 AFIX 0 C27 1 -0.188146 -0.476461 0.421456 11.00000 0.02721 0.01122 = 0.02411 -0.00094 -0.00761 0.00178 C22 1 0.097531 0.392096 0.869915 11.00000 0.02065 0.01924 = 0.01455 0.00409 0.00175 0.00062 AFIX 43 H22 2 0.015638 0.382984 0.820862 11.00000 -1.20000 AFIX 0 C21 1 0.132774 0.488328 0.925594 11.00000 0.02513 0.01695 = 0.01757 0.00374 0.00125 0.00619 AFIX 43 H21 2 0.075786 0.544092 0.913929 11.00000 -1.20000 AFIX 0 C33 1 0.461623 0.386819 0.727076 11.00000 0.02265 0.01716 = 0.01422 0.00372 0.00440 0.00219 AFIX 43 H33 2 0.427964 0.432836 0.774498 11.00000 -1.20000 AFIX 0 C29 1 -0.204873 -0.346779 0.553524 11.00000 0.02208 0.01697 = 0.02026 0.00267 0.00385 0.00003 AFIX 43 H29 2 -0.246913 -0.323653 0.607454 11.00000 -1.20000 AFIX 0 C7 1 0.169990 -0.225225 0.910171 11.00000 0.02042 0.02055 = 0.02233 0.01066 0.00659 0.00577 AFIX 43 H7 2 0.244412 -0.273551 0.915707 11.00000 -1.20000 AFIX 0 C25 1 -0.029973 -0.319842 0.445973 11.00000 0.01672 0.02019 = 0.01891 0.00145 0.00223 0.00137 AFIX 43 H25 2 0.042764 -0.277899 0.426928 11.00000 -1.20000 AFIX 0 H37 2 -0.208395 0.013725 0.563937 11.00000 0.03731 H38 2 -0.113880 0.085441 0.555103 11.00000 0.02774 HKLF 4 REM Pbar1_twin in P-1 REM R1 = 0.0255 for 7053 Fo > 4sig(Fo) and 0.0299 for all 7768 data REM 459 parameters refined using 0 restraints END WGHT 0.0275 0.8375 REM Highest difference peak 0.850, deepest hole -0.672, 1-sigma level 0.096 Q1 1 0.4009 0.6223 1.0459 11.00000 0.05 0.85 Q2 1 -0.3154 -0.6279 0.3982 11.00000 0.05 0.71 Q3 1 0.7368 0.5164 0.8000 11.00000 0.05 0.64 Q4 1 0.6218 0.5703 0.7819 11.00000 0.05 0.62 Q5 1 0.8261 0.5040 0.7427 11.00000 0.05 0.56 Q6 1 -0.2044 -0.5864 0.2800 11.00000 0.05 0.53 Q7 1 0.3885 0.1720 0.6051 11.00000 0.05 0.46 Q8 1 0.2549 -0.1524 0.8379 11.00000 0.05 0.46 Q9 1 -0.0563 -0.2339 0.5568 11.00000 0.05 0.43 Q10 1 0.5498 -0.1808 0.7243 11.00000 0.05 0.41 ; _shelx_res_checksum 64684 _shelx_hkl_file ; 1 0 0 272.72 5.09 2 0 0 0.39 0.13 3 0 0 85.77 1.75 4 0 0 0.14 0.16 5 0 0 56.58 1.29 6 0 0 118.79 2.62 7 0 0 31.83 1.18 9 0 0 62.08 3.37 10 0 0 13.97 1.30 11 0 0 1.10 0.76 -11 1 0 3.49 0.88 -10 1 0 12.43 1.24 -9 1 0 28.78 1.70 -8 1 0 130.56 4.92 -7 1 0 65.71 1.72 -6 1 0 10.66 0.49 -5 1 0 0.24 0.18 -4 1 0 16.80 0.55 -3 1 0 42.96 0.96 -2 1 0 508.72 9.03 -1 1 0 378.06 6.42 0 1 0 353.50 5.66 1 1 0 212.76 3.40 2 1 0 118.90 1.84 3 1 0 18.75 0.53 4 1 0 59.58 1.31 5 1 0 12.21 0.47 6 1 0 93.88 2.10 7 1 0 99.03 2.73 8 1 0 35.88 1.38 9 1 0 43.82 2.03 10 1 0 25.93 1.72 11 1 0 4.26 0.93 -11 2 0 7.45 1.03 -10 2 0 2.89 0.74 -9 2 0 28.80 1.53 -8 2 0 41.82 1.89 -7 2 0 43.86 1.46 -6 2 0 27.65 0.84 -5 2 0 20.91 0.64 -4 2 0 11.30 0.49 -3 2 0 2.19 0.27 -2 2 0 33.13 0.84 -1 2 0 157.89 2.55 0 2 0 330.12 6.73 1 2 0 144.46 2.03 2 2 0 9.99 0.34 3 2 0 57.78 1.09 4 2 0 11.48 0.41 5 2 0 135.11 2.67 6 2 0 85.93 2.28 7 2 0 32.60 1.32 8 2 0 13.06 0.91 9 2 0 72.50 2.33 10 2 0 7.68 0.99 11 2 0 0.00 0.66 -11 3 0 4.15 0.95 -10 3 0 6.97 0.95 -9 3 0 23.97 1.81 -8 3 0 92.40 5.02 -7 3 0 20.19 0.94 -6 3 0 1.65 0.25 -5 3 0 5.36 0.32 -4 3 0 0.60 0.15 -3 3 0 27.53 0.82 -2 3 0 79.68 1.26 -1 3 0 38.99 0.72 0 3 0 13.04 0.37 1 3 0 161.98 2.59 2 3 0 0.74 0.15 3 3 0 3.51 0.23 4 3 0 18.91 0.57 5 3 0 31.33 0.93 6 3 0 55.93 1.57 7 3 0 104.06 2.61 8 3 0 0.64 0.39 9 3 0 29.76 1.34 10 3 0 0.30 0.58 -11 4 0 2.35 0.76 -10 4 0 32.45 1.83 -9 4 0 44.51 2.07 -8 4 0 56.44 2.33 -7 4 0 8.46 0.65 -6 4 0 0.72 0.29 -5 4 0 0.02 0.22 -4 4 0 0.95 0.27 -3 4 0 21.73 0.71 -2 4 0 116.60 1.99 -1 4 0 132.11 1.93 0 4 0 1.89 0.22 1 4 0 138.49 2.44 2 4 0 82.10 1.42 3 4 0 0.96 0.17 4 4 0 18.96 0.58 5 4 0 22.69 0.86 6 4 0 66.87 1.82 7 4 0 17.78 0.91 8 4 0 17.30 0.97 9 4 0 19.35 1.15 10 4 0 3.38 0.62 -10 5 0 43.53 2.15 -9 5 0 43.83 2.02 -8 5 0 43.85 2.03 -7 5 0 16.36 0.90 -6 5 0 20.41 0.87 -5 5 0 5.16 0.46 -4 5 0 83.03 1.90 -3 5 0 0.63 0.23 -2 5 0 72.52 1.31 -1 5 0 173.24 2.85 0 5 0 85.87 1.59 1 5 0 31.46 0.75 2 5 0 166.18 2.63 3 5 0 0.77 0.18 4 5 0 54.12 1.24 5 5 0 36.94 1.19 6 5 0 48.45 1.49 7 5 0 22.79 1.00 8 5 0 45.61 1.56 9 5 0 4.40 0.64 10 5 0 1.45 0.53 -10 6 0 7.37 1.05 -9 6 0 30.55 1.68 -8 6 0 60.23 2.22 -7 6 0 22.96 1.03 -6 6 0 8.67 0.62 -5 6 0 0.56 0.28 -4 6 0 14.31 0.66 -3 6 0 123.42 2.19 -2 6 0 78.50 1.41 -1 6 0 28.16 0.69 0 6 0 46.97 1.02 1 6 0 380.89 5.95 2 6 0 0.25 0.16 3 6 0 62.73 1.20 4 6 0 12.93 0.50 5 6 0 82.78 1.97 6 6 0 28.86 1.05 7 6 0 40.40 1.34 8 6 0 38.36 1.38 9 6 0 10.61 0.84 10 6 0 0.09 0.49 -10 7 0 18.97 1.41 -9 7 0 50.59 1.85 -8 7 0 2.38 0.51 -7 7 0 56.34 1.90 -6 7 0 19.31 0.86 -5 7 0 24.54 0.94 -4 7 0 60.69 1.51 -3 7 0 34.47 0.81 -2 7 0 65.01 1.20 -1 7 0 368.84 6.32 0 7 0 36.77 0.95 1 7 0 1.40 0.21 2 7 0 7.32 0.36 3 7 0 1.31 0.22 4 7 0 88.19 1.82 5 7 0 128.37 2.83 6 7 0 41.62 1.35 7 7 0 95.14 2.37 8 7 0 70.77 2.04 9 7 0 0.13 0.42 -10 8 0 24.03 1.53 -9 8 0 42.27 1.63 -8 8 0 78.99 2.17 -7 8 0 12.66 0.96 -6 8 0 4.47 0.59 -5 8 0 2.00 0.38 -4 8 0 70.77 1.75 -3 8 0 214.56 3.70 -2 8 0 33.42 0.84 -1 8 0 8.72 0.41 0 8 0 114.01 1.86 1 8 0 42.50 0.95 2 8 0 23.98 0.66 3 8 0 88.05 1.81 4 8 0 22.31 0.87 5 8 0 87.51 2.11 6 8 0 76.38 1.99 7 8 0 20.25 1.01 8 8 0 8.03 0.74 9 8 0 0.84 0.66 -9 9 0 44.35 1.63 -8 9 0 45.24 1.57 -7 9 0 35.79 1.31 -6 9 0 5.06 0.65 -5 9 0 37.35 1.41 -4 9 0 16.78 0.87 -3 9 0 33.14 1.08 -2 9 0 86.60 1.52 -1 9 0 75.08 1.48 0 9 0 29.93 0.75 1 9 0 2.94 0.29 2 9 0 1.10 0.24 3 9 0 0.57 0.23 4 9 0 18.30 0.83 5 9 0 30.79 1.12 6 9 0 15.40 0.87 7 9 0 15.38 1.13 8 9 0 17.99 1.36 9 9 0 0.73 0.67 -9 10 0 57.77 1.89 -8 10 0 12.32 0.92 -7 10 0 0.58 0.44 -6 10 0 11.95 0.81 -5 10 0 2.54 0.46 -4 10 0 48.54 1.44 -3 10 0 62.78 1.49 -2 10 0 28.05 0.77 -1 10 0 59.46 1.36 0 10 0 130.89 2.20 1 10 0 5.20 0.37 2 10 0 2.55 0.31 3 10 0 0.65 0.27 4 10 0 12.25 0.76 5 10 0 40.59 1.59 6 10 0 55.13 1.98 7 10 0 15.66 1.20 8 10 0 2.26 0.91 -9 11 0 26.04 1.64 -8 11 0 15.19 1.10 -7 11 0 1.22 0.47 -6 11 0 0.46 0.41 -5 11 0 0.15 0.35 -4 11 0 17.85 0.86 -3 11 0 106.51 2.67 -2 11 0 80.02 1.67 -1 11 0 51.72 1.34 0 11 0 4.67 0.35 1 11 0 0.22 0.28 2 11 0 5.94 0.54 3 11 0 9.21 0.84 4 11 0 16.29 1.08 5 11 0 33.55 1.48 6 11 0 24.70 1.41 7 11 0 26.49 1.74 8 11 0 6.14 1.15 -8 12 0 4.14 0.71 -7 12 0 10.28 0.84 -6 12 0 1.77 0.59 -5 12 0 14.13 0.94 -4 12 0 25.48 1.12 -3 12 0 34.04 1.21 -2 12 0 63.33 1.53 -1 12 0 36.46 1.21 0 12 0 16.53 0.99 1 12 0 1.72 0.38 2 12 0 13.56 0.79 3 12 0 4.12 0.78 4 12 0 20.31 1.25 5 12 0 33.42 1.69 6 12 0 58.24 2.14 7 12 0 18.25 1.38 -7 13 0 3.98 0.65 -6 13 0 0.50 0.45 -5 13 0 1.23 0.71 -4 13 0 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163.62 3.48 4 -1 2 44.88 1.07 5 -1 2 0.90 0.21 6 -1 2 7.60 0.43 7 -1 2 11.17 0.74 8 -1 2 14.67 1.18 9 -1 2 37.44 1.90 -11 0 2 12.15 1.68 -10 0 2 2.57 1.10 -9 0 2 7.00 0.88 -8 0 2 71.34 2.71 -7 0 2 9.05 0.49 -6 0 2 120.05 2.69 -5 0 2 163.55 3.27 -4 0 2 82.62 1.75 -3 0 2 2.01 0.20 -2 0 2 156.30 3.27 -1 0 2 11.93 0.26 0 0 2 125.04 1.64 1 0 2 71.43 1.17 2 0 2 26.62 0.72 3 0 2 5.15 0.29 4 0 2 94.73 1.88 5 0 2 29.80 0.81 6 0 2 8.67 0.57 7 0 2 13.12 1.22 8 0 2 16.51 0.94 9 0 2 52.23 2.32 10 0 2 23.01 1.63 -11 1 2 9.50 1.16 -10 1 2 6.11 0.98 -9 1 2 0.20 0.50 -8 1 2 49.36 1.93 -7 1 2 45.45 1.24 -6 1 2 98.87 2.87 -5 1 2 11.11 0.46 -4 1 2 56.78 1.26 -3 1 2 18.30 0.51 -2 1 2 92.06 1.70 -1 1 2 18.24 0.38 0 1 2 258.92 3.43 1 1 2 231.88 3.40 2 1 2 80.44 1.36 3 1 2 58.69 1.35 4 1 2 15.95 0.50 5 1 2 0.07 0.14 6 1 2 0.52 0.29 7 1 2 41.91 1.38 8 1 2 50.53 1.74 9 1 2 42.45 2.00 10 1 2 33.57 1.87 -11 2 2 4.37 0.90 -10 2 2 5.85 0.85 -9 2 2 10.43 1.05 -8 2 2 97.73 2.64 -7 2 2 81.35 2.21 -6 2 2 41.72 1.56 -5 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1.73 8 -11 3 27.70 1.26 -9 -10 3 29.67 2.25 -8 -10 3 12.47 1.17 -7 -10 3 3.14 0.91 -6 -10 3 34.74 1.53 -5 -10 3 20.31 1.14 -4 -10 3 0.86 0.34 -3 -10 3 0.34 0.30 -2 -10 3 10.15 0.60 -1 -10 3 16.74 0.70 0 -10 3 175.71 3.21 1 -10 3 63.56 1.26 2 -10 3 3.75 0.33 3 -10 3 34.27 1.02 4 -10 3 9.80 0.64 5 -10 3 9.01 0.67 6 -10 3 30.70 1.17 7 -10 3 20.10 1.04 8 -10 3 30.04 1.28 9 -10 3 50.24 1.83 -9 -9 3 8.97 0.99 -8 -9 3 70.09 2.39 -7 -9 3 74.12 2.39 -6 -9 3 13.91 0.99 -5 -9 3 17.16 1.02 -4 -9 3 38.67 1.22 -3 -9 3 12.47 0.60 -2 -9 3 66.81 1.46 -1 -9 3 35.20 0.85 0 -9 3 9.56 0.43 1 -9 3 189.18 3.10 2 -9 3 94.41 1.71 3 -9 3 16.49 0.56 4 -9 3 0.83 0.32 5 -9 3 0.41 0.33 6 -9 3 27.11 1.06 7 -9 3 41.88 1.41 8 -9 3 23.32 1.12 9 -9 3 18.45 1.26 -9 -8 3 43.65 1.86 -8 -8 3 29.30 1.45 -7 -8 3 30.58 1.38 -6 -8 3 95.30 2.58 -5 -8 3 5.37 0.50 -4 -8 3 0.99 0.25 -3 -8 3 6.58 0.36 -2 -8 3 3.39 0.26 -1 -8 3 27.33 0.69 0 -8 3 253.82 4.07 1 -8 3 45.02 0.99 2 -8 3 46.77 1.00 3 -8 3 75.20 1.44 4 -8 3 3.75 0.42 5 -8 3 55.75 1.55 6 -8 3 14.08 0.80 7 -8 3 8.29 0.67 8 -8 3 34.04 1.30 9 -8 3 5.63 0.83 -10 -7 3 17.97 1.41 -9 -7 3 13.39 1.09 -8 -7 3 42.12 1.45 -7 -7 3 60.48 1.74 -6 -7 3 47.92 1.43 -5 -7 3 20.98 0.71 -4 -7 3 17.46 0.57 -3 -7 3 22.48 0.63 -2 -7 3 136.34 2.18 -1 -7 3 34.42 0.70 0 -7 3 119.55 2.05 1 -7 3 158.10 2.53 2 -7 3 92.64 1.65 3 -7 3 20.26 0.59 4 -7 3 3.66 0.29 5 -7 3 18.59 0.81 6 -7 3 42.08 1.31 7 -7 3 56.23 1.65 8 -7 3 42.24 1.44 9 -7 3 13.96 1.10 10 -7 3 5.33 0.93 -10 -6 3 26.72 1.34 -9 -6 3 23.03 1.10 -8 -6 3 52.57 1.69 -7 -6 3 105.38 2.43 -6 -6 3 0.90 0.32 -5 -6 3 12.90 0.55 -4 -6 3 17.28 0.55 -3 -6 3 40.37 0.94 -2 -6 3 102.60 1.79 -1 -6 3 274.09 4.48 0 -6 3 144.00 2.34 1 -6 3 101.49 1.70 2 -6 3 36.88 0.81 3 -6 3 8.56 0.38 4 -6 3 29.73 0.73 5 -6 3 54.24 1.44 6 -6 3 53.38 1.50 7 -6 3 46.22 1.44 8 -6 3 37.28 1.32 9 -6 3 25.69 1.48 10 -6 3 3.01 0.78 -10 -5 3 25.14 1.31 -9 -5 3 34.15 1.39 -8 -5 3 30.50 1.21 -7 -5 3 51.87 1.60 -6 -5 3 40.11 1.24 -5 -5 3 1.38 0.23 -4 -5 3 49.13 1.11 -3 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3 3.71 0.86 -11 3 3 36.64 2.18 -10 3 3 28.88 1.66 -9 3 3 69.53 2.56 -8 3 3 26.77 1.12 -7 3 3 0.83 0.34 -6 3 3 0.47 0.28 -5 3 3 0.29 0.15 -4 3 3 72.92 1.45 -3 3 3 252.11 4.59 -2 3 3 52.36 0.93 -1 3 3 236.94 3.82 0 3 3 167.36 2.58 1 3 3 12.09 0.39 2 3 3 156.68 2.50 3 3 3 6.18 0.39 4 3 3 98.67 1.88 5 3 3 90.04 2.13 6 3 3 5.62 0.51 7 3 3 39.80 1.29 8 3 3 8.22 0.69 9 3 3 0.64 0.55 10 3 3 23.88 1.62 -11 4 3 60.07 2.70 -10 4 3 30.19 1.71 -9 4 3 22.28 1.10 -8 4 3 19.23 0.96 -7 4 3 73.74 2.14 -6 4 3 17.64 0.80 -5 4 3 101.92 2.43 -4 4 3 50.36 1.25 -3 4 3 127.71 2.37 -2 4 3 262.65 3.92 -1 4 3 134.06 2.31 0 4 3 64.31 1.19 1 4 3 82.26 1.44 2 4 3 14.28 0.46 3 4 3 5.43 0.36 4 4 3 44.33 1.27 5 4 3 74.99 1.88 6 4 3 74.90 1.87 7 4 3 5.36 0.57 8 4 3 2.66 0.50 9 4 3 9.15 0.82 10 4 3 2.60 0.75 -10 5 3 26.13 1.63 -9 5 3 30.90 1.31 -8 5 3 10.47 0.79 -7 5 3 0.36 0.34 -6 5 3 8.55 0.63 -5 5 3 29.41 1.04 -4 5 3 116.12 2.15 -3 5 3 20.70 0.57 -2 5 3 145.73 2.13 -1 5 3 227.48 3.75 0 5 3 128.16 2.09 1 5 3 1.88 0.22 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1.73 0.76 -1 16 3 0.03 0.59 0 16 3 23.36 3.71 1 16 3 21.14 2.09 -1 -17 4 37.53 1.91 0 -17 4 45.01 2.25 1 -17 4 7.47 1.04 2 -17 4 4.46 0.89 -3 -16 4 47.17 2.15 -2 -16 4 16.76 1.30 -1 -16 4 8.15 0.81 0 -16 4 36.55 1.89 1 -16 4 6.89 0.95 2 -16 4 0.45 0.61 3 -16 4 4.74 0.87 4 -16 4 4.12 0.87 -5 -15 4 1.54 0.74 -4 -15 4 6.43 0.96 -3 -15 4 3.53 0.72 -2 -15 4 16.61 1.19 -1 -15 4 29.16 1.28 0 -15 4 22.45 1.31 1 -15 4 9.72 1.01 2 -15 4 0.09 0.53 3 -15 4 2.26 0.72 4 -15 4 29.86 1.70 5 -15 4 10.63 1.34 -6 -14 4 5.69 1.00 -5 -14 4 4.99 0.87 -4 -14 4 7.20 0.93 -3 -14 4 32.24 1.62 -2 -14 4 20.79 1.11 -1 -14 4 5.24 0.61 0 -14 4 38.64 1.35 1 -14 4 22.30 1.42 2 -14 4 15.71 1.17 3 -14 4 2.07 0.66 4 -14 4 14.89 1.22 5 -14 4 20.94 1.44 6 -14 4 15.28 1.44 -7 -13 4 6.80 1.04 -6 -13 4 0.08 0.55 -5 -13 4 3.10 0.71 -4 -13 4 6.67 0.93 -3 -13 4 7.22 0.72 -2 -13 4 31.18 1.25 -1 -13 4 48.67 1.50 0 -13 4 30.69 1.16 1 -13 4 48.01 1.55 2 -13 4 1.84 0.58 3 -13 4 12.27 1.05 4 -13 4 27.67 1.47 5 -13 4 18.48 1.39 6 -13 4 32.51 1.89 7 -13 4 14.38 1.31 -7 -12 4 8.37 1.28 -6 -12 4 3.22 1.00 -5 -12 4 5.76 0.82 -4 -12 4 37.80 1.99 -3 -12 4 32.99 1.49 -2 -12 4 91.82 2.39 -1 -12 4 86.26 2.21 0 -12 4 56.18 1.72 1 -12 4 48.02 1.80 2 -12 4 1.74 0.76 3 -12 4 32.94 1.54 4 -12 4 15.63 1.15 5 -12 4 30.38 1.75 6 -12 4 50.75 2.23 7 -12 4 36.37 1.80 8 -12 4 4.11 0.84 -8 -11 4 21.12 1.59 -7 -11 4 3.79 0.85 -6 -11 4 0.06 0.47 -5 -11 4 19.58 1.27 -4 -11 4 52.86 1.70 -3 -11 4 94.99 2.49 -2 -11 4 88.05 2.09 -1 -11 4 31.77 1.09 0 -11 4 16.98 0.81 1 -11 4 6.30 0.62 2 -11 4 10.03 0.67 3 -11 4 22.74 1.21 4 -11 4 64.67 2.53 5 -11 4 139.97 4.25 6 -11 4 38.06 1.44 7 -11 4 16.36 1.03 8 -11 4 6.26 0.77 -9 -10 4 12.08 1.25 -8 -10 4 19.17 1.44 -7 -10 4 14.64 1.23 -6 -10 4 0.83 0.52 -5 -10 4 27.62 1.36 -4 -10 4 63.04 1.80 -3 -10 4 34.05 1.10 -2 -10 4 45.17 1.25 -1 -10 4 45.24 1.25 0 -10 4 1.16 0.31 1 -10 4 14.13 0.64 2 -10 4 11.71 0.49 3 -10 4 55.24 1.36 4 -10 4 34.92 1.18 5 -10 4 49.46 1.48 6 -10 4 75.92 2.02 7 -10 4 18.15 0.99 8 -10 4 0.69 0.45 9 -10 4 0.78 0.60 -9 -9 4 59.04 2.36 -8 -9 4 0.07 0.52 -7 -9 4 0.61 0.51 -6 -9 4 1.39 0.51 -5 -9 4 27.27 1.23 -4 -9 4 91.00 2.12 -3 -9 4 38.42 1.07 -2 -9 4 19.79 0.72 -1 -9 4 71.38 1.58 0 -9 4 4.42 0.35 1 -9 4 1.44 0.23 2 -9 4 5.59 0.35 3 -9 4 10.07 0.47 4 -9 4 76.64 1.84 5 -9 4 69.98 1.81 6 -9 4 11.35 0.75 7 -9 4 22.15 1.05 8 -9 4 9.70 0.79 9 -9 4 12.40 1.10 -9 -8 4 7.17 0.92 -8 -8 4 14.10 1.07 -7 -8 4 4.06 0.71 -6 -8 4 22.80 1.13 -5 -8 4 83.21 1.99 -4 -8 4 4.46 0.42 -3 -8 4 137.68 2.44 -2 -8 4 60.65 1.32 -1 -8 4 3.13 0.34 0 -8 4 35.14 0.73 1 -8 4 0.53 0.18 2 -8 4 38.13 0.89 3 -8 4 17.41 0.58 4 -8 4 18.16 0.77 5 -8 4 70.69 1.79 6 -8 4 33.83 1.18 7 -8 4 0.16 0.36 8 -8 4 1.61 0.47 9 -8 4 2.71 0.67 -10 -7 4 21.33 1.49 -9 -7 4 20.10 1.30 -8 -7 4 2.53 0.64 -7 -7 4 3.50 0.49 -6 -7 4 2.15 0.39 -5 -7 4 83.92 1.79 -4 -7 4 178.24 2.85 -3 -7 4 67.54 1.29 -2 -7 4 11.39 0.40 -1 -7 4 21.76 0.67 0 -7 4 23.90 0.65 1 -7 4 9.89 0.38 2 -7 4 34.26 0.80 3 -7 4 27.14 0.71 4 -7 4 68.16 1.38 5 -7 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6 -2 4 23.64 0.79 7 -2 4 13.60 0.82 8 -2 4 5.27 0.79 9 -2 4 15.17 1.29 10 -2 4 8.07 1.05 -11 -1 4 23.01 1.65 -10 -1 4 6.68 0.95 -9 -1 4 8.33 0.93 -8 -1 4 3.51 0.49 -7 -1 4 28.82 0.88 -6 -1 4 29.12 0.88 -5 -1 4 39.94 1.01 -4 -1 4 113.32 2.19 -3 -1 4 137.01 2.23 -2 -1 4 11.26 0.37 -1 -1 4 0.40 0.13 0 -1 4 0.41 0.14 1 -1 4 202.22 2.89 2 -1 4 67.48 1.19 3 -1 4 98.81 1.66 4 -1 4 60.38 1.27 5 -1 4 30.06 0.81 6 -1 4 2.93 0.41 7 -1 4 0.25 0.31 8 -1 4 3.88 0.79 9 -1 4 10.60 1.33 10 -1 4 43.37 2.87 -11 0 4 27.11 1.79 -10 0 4 12.31 1.17 -9 0 4 1.03 0.58 -8 0 4 5.79 0.58 -7 0 4 0.49 0.26 -6 0 4 41.24 1.09 -5 0 4 140.35 2.73 -4 0 4 4.32 0.39 -3 0 4 1.24 0.23 -2 0 4 43.40 0.84 -1 0 4 27.68 0.61 0 0 4 0.46 0.10 1 0 4 2.53 0.20 2 0 4 165.33 2.62 3 0 4 311.95 5.05 4 0 4 38.40 0.93 5 0 4 0.56 0.20 6 0 4 26.87 0.96 7 0 4 2.20 0.43 8 0 4 8.52 0.74 9 0 4 6.21 0.92 10 0 4 23.64 1.71 -11 1 4 20.20 1.60 -10 1 4 16.61 1.36 -9 1 4 3.92 0.72 -8 1 4 23.74 1.05 -7 1 4 36.34 2.19 -6 1 4 38.60 1.02 -5 1 4 91.45 1.94 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38.22 1.61 10 3 4 21.74 1.55 -11 4 4 24.11 1.69 -10 4 4 11.61 1.16 -9 4 4 0.23 0.39 -8 4 4 13.25 0.86 -7 4 4 158.02 3.90 -6 4 4 134.82 3.21 -5 4 4 202.94 4.09 -4 4 4 81.98 1.56 -3 4 4 1.50 0.19 -2 4 4 78.49 1.37 -1 4 4 0.13 0.16 0 4 4 246.56 3.55 1 4 4 419.70 5.82 2 4 4 76.49 1.37 3 4 4 77.50 1.40 4 4 4 131.03 2.63 5 4 4 12.95 0.71 6 4 4 21.96 0.91 7 4 4 10.18 0.75 8 4 4 10.26 0.92 9 4 4 32.02 1.39 10 4 4 26.06 1.41 -10 5 4 0.21 0.54 -9 5 4 0.08 0.39 -8 5 4 2.48 0.47 -7 5 4 153.34 3.52 -6 5 4 201.91 4.12 -5 5 4 31.43 1.07 -4 5 4 52.85 1.18 -3 5 4 34.37 0.79 -2 5 4 10.28 0.39 -1 5 4 86.33 1.50 0 5 4 1.37 0.23 1 5 4 9.15 0.40 2 5 4 552.98 7.64 3 5 4 44.16 0.95 4 5 4 6.12 0.50 5 5 4 63.43 1.68 6 5 4 5.45 0.55 7 5 4 18.10 0.95 8 5 4 26.26 1.16 9 5 4 2.82 0.73 -10 6 4 6.04 0.93 -9 6 4 0.16 0.39 -8 6 4 34.60 1.30 -7 6 4 10.36 0.72 -6 6 4 163.82 3.42 -5 6 4 47.51 1.41 -4 6 4 6.10 0.33 -3 6 4 8.22 0.38 -2 6 4 0.89 0.19 -1 6 4 27.26 0.71 0 6 4 163.53 2.64 1 6 4 4.74 0.31 2 6 4 65.67 1.29 3 6 4 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43.97 1.35 1 -11 5 22.68 1.26 2 -11 5 38.92 1.24 3 -11 5 139.05 3.94 4 -11 5 49.33 2.04 5 -11 5 4.32 0.71 6 -11 5 2.18 0.65 7 -11 5 4.55 0.67 8 -11 5 11.77 0.96 -9 -10 5 0.19 1.03 -8 -10 5 11.79 1.30 -7 -10 5 0.68 0.61 -6 -10 5 9.08 0.94 -5 -10 5 109.31 3.27 -4 -10 5 60.86 1.81 -3 -10 5 0.20 0.31 -2 -10 5 4.23 0.46 -1 -10 5 0.28 0.28 0 -10 5 34.95 1.13 1 -10 5 65.64 1.67 2 -10 5 34.47 1.12 3 -10 5 35.88 1.43 4 -10 5 12.01 0.76 5 -10 5 9.78 0.73 6 -10 5 0.53 0.42 7 -10 5 13.13 0.93 8 -10 5 10.04 0.87 -9 -9 5 0.59 0.64 -8 -9 5 5.54 0.86 -7 -9 5 13.97 1.12 -6 -9 5 9.16 0.89 -5 -9 5 48.36 1.44 -4 -9 5 11.00 0.67 -3 -9 5 80.54 1.81 -2 -9 5 0.86 0.29 -1 -9 5 43.16 1.25 0 -9 5 6.98 0.48 1 -9 5 52.18 1.21 2 -9 5 45.14 1.02 3 -9 5 36.85 0.92 4 -9 5 2.01 0.39 5 -9 5 7.50 0.62 6 -9 5 1.31 0.42 7 -9 5 11.08 0.80 8 -9 5 24.84 1.19 9 -9 5 17.48 1.25 -9 -8 5 0.27 0.53 -8 -8 5 35.26 1.58 -7 -8 5 11.63 0.94 -6 -8 5 13.49 0.95 -5 -8 5 151.73 3.10 -4 -8 5 8.00 0.51 -3 -8 5 0.45 0.25 -2 -8 5 22.21 0.73 -1 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2 16 5.29 0.78 3 2 16 21.76 1.54 4 2 16 30.17 1.82 -6 3 16 16.87 1.32 -5 3 16 30.12 1.68 -4 3 16 39.17 1.30 -3 3 16 11.33 0.76 -2 3 16 14.21 1.14 -1 3 16 46.44 1.72 0 3 16 0.35 0.43 1 3 16 6.69 0.88 2 3 16 32.04 1.75 3 3 16 20.73 1.57 -6 4 16 35.44 1.79 -5 4 16 23.75 1.41 -4 4 16 34.89 1.35 -3 4 16 36.10 1.19 -2 4 16 11.18 1.01 -1 4 16 9.62 0.80 0 4 16 0.24 0.41 1 4 16 7.03 0.88 2 4 16 31.98 1.72 3 4 16 46.15 2.09 -5 5 16 20.90 1.43 -4 5 16 37.57 1.40 -3 5 16 12.87 0.79 -2 5 16 9.12 0.95 -1 5 16 19.61 1.10 0 5 16 0.88 0.60 1 5 16 27.06 1.57 2 5 16 12.91 1.18 -4 6 16 27.08 1.28 -3 6 16 44.96 1.56 -2 6 16 4.90 0.61 -1 6 16 0.32 0.46 0 6 16 5.63 0.87 1 6 16 16.78 1.35 -2 7 16 14.77 0.97 -1 7 16 1.30 0.97 -3 -10 17 20.69 1.58 -2 -10 17 19.28 1.54 -1 -10 17 0.62 0.63 0 -10 17 13.48 1.28 1 -10 17 12.94 1.23 -4 -9 17 26.24 1.73 -3 -9 17 11.81 1.17 -2 -9 17 2.22 0.73 -1 -9 17 2.73 0.75 0 -9 17 0.82 0.64 1 -9 17 4.58 0.87 2 -9 17 21.72 1.52 -5 -8 17 13.88 1.24 -4 -8 17 32.80 1.75 -3 -8 17 18.98 1.39 -2 -8 17 13.80 1.22 -1 -8 17 0.06 0.57 0 -8 17 0.89 0.65 1 -8 17 11.07 1.09 2 -8 17 29.20 1.63 -5 -7 17 33.15 1.78 -4 -7 17 37.13 1.81 -3 -7 17 6.23 0.92 -2 -7 17 6.79 0.90 -1 -7 17 1.21 0.63 0 -7 17 13.71 1.19 1 -7 17 15.52 1.25 2 -7 17 14.42 1.22 3 -7 17 42.21 1.93 -6 -6 17 42.20 1.99 -5 -6 17 15.62 1.27 -4 -6 17 50.48 2.15 -3 -6 17 37.46 1.78 -2 -6 17 0.69 0.54 -1 -6 17 0.45 0.59 0 -6 17 2.10 0.69 1 -6 17 13.20 1.15 2 -6 17 52.70 2.19 3 -6 17 23.57 1.49 -6 -5 17 41.66 1.94 -5 -5 17 50.71 2.16 -4 -5 17 16.48 1.28 -3 -5 17 2.14 0.68 -2 -5 17 15.62 1.23 -1 -5 17 12.70 1.13 0 -5 17 34.49 1.69 1 -5 17 5.77 0.87 2 -5 17 33.03 1.64 3 -5 17 49.69 2.08 -6 -4 17 19.37 1.40 -5 -4 17 27.75 1.63 -4 -4 17 19.99 1.40 -3 -4 17 10.81 1.09 -2 -4 17 2.59 0.69 -1 -4 17 5.22 0.81 0 -4 17 18.58 1.29 1 -4 17 41.07 1.83 2 -4 17 18.36 1.32 3 -4 17 10.46 1.43 -6 -3 17 38.33 1.83 -5 -3 17 34.55 1.70 -4 -3 17 12.00 1.10 -3 -3 17 18.64 1.29 -2 -3 17 0.87 0.58 -1 -3 17 21.03 1.38 0 -3 17 16.10 0.99 1 -3 17 2.80 0.56 2 -3 17 15.93 1.01 3 -3 17 32.70 1.65 4 -3 17 5.04 0.89 -6 -2 17 28.41 1.60 -5 -2 17 28.95 1.76 -4 -2 17 25.02 1.50 -3 -2 17 11.41 0.76 -2 -2 17 3.67 0.70 -1 -2 17 0.54 0.44 0 -2 17 13.73 0.92 1 -2 17 32.29 1.40 2 -2 17 28.12 1.29 3 -2 17 12.32 1.30 -6 -1 17 25.78 1.52 -5 -1 17 27.35 1.29 -4 -1 17 40.94 1.56 -3 -1 17 10.94 0.75 -2 -1 17 3.76 0.74 -1 -1 17 3.10 0.78 0 -1 17 10.26 0.90 1 -1 17 33.75 1.43 2 -1 17 42.40 1.89 3 -1 17 19.44 1.49 -6 0 17 61.46 2.42 -5 0 17 21.35 1.26 -4 0 17 9.44 1.02 -3 0 17 9.02 0.73 -2 0 17 2.02 0.63 -1 0 17 35.82 1.96 0 0 17 18.59 1.10 1 0 17 29.88 1.30 2 0 17 50.64 2.11 3 0 17 14.45 1.28 -6 1 17 18.78 1.38 -5 1 17 55.94 2.12 -4 1 17 16.66 0.95 -3 1 17 2.11 0.46 -2 1 17 33.98 1.49 -1 1 17 17.96 1.04 0 1 17 26.64 1.21 1 1 17 53.58 1.77 2 1 17 9.04 0.99 3 1 17 11.19 1.16 -6 2 17 38.89 8.29 -5 2 17 7.37 0.91 -4 2 17 0.64 0.40 -3 2 17 0.18 0.34 -2 2 17 6.98 0.86 -1 2 17 59.71 1.85 0 2 17 16.91 1.05 1 2 17 21.32 1.33 2 2 17 28.89 1.64 -5 3 17 31.95 1.69 -4 3 17 0.77 0.42 -3 3 17 2.12 0.47 -2 3 17 0.02 0.59 -1 3 17 17.79 1.12 0 3 17 38.92 1.53 1 3 17 33.88 1.60 2 3 17 5.92 0.99 -4 4 17 1.30 0.53 -3 4 17 0.17 0.38 -2 4 17 10.14 1.07 -1 4 17 17.02 1.06 0 4 17 31.92 1.57 1 4 17 20.67 1.47 -3 5 17 1.51 0.48 -2 5 17 8.22 0.74 -1 5 17 21.22 1.18 0 5 17 39.00 1.88 -2 -9 18 12.04 1.71 -1 -9 18 5.64 0.95 -3 -8 18 0.65 0.67 -2 -8 18 14.87 1.27 -1 -8 18 17.56 1.37 0 -8 18 24.52 1.59 1 -8 18 16.35 1.40 -4 -7 18 1.89 0.70 -3 -7 18 6.41 0.93 -2 -7 18 19.53 1.43 -1 -7 18 13.78 1.23 0 -7 18 35.26 1.80 1 -7 18 13.40 1.22 -4 -6 18 1.74 0.68 -3 -6 18 28.43 1.64 -2 -6 18 7.83 0.99 -1 -6 18 72.27 2.71 0 -6 18 40.05 1.92 1 -6 18 11.99 1.17 2 -6 18 4.88 0.89 -5 -5 18 0.28 0.60 -4 -5 18 2.33 0.75 -3 -5 18 31.94 1.70 -2 -5 18 20.52 1.42 -1 -5 18 54.08 2.24 0 -5 18 54.01 2.21 1 -5 18 25.90 1.59 2 -5 18 2.22 0.73 -5 -4 18 1.50 0.70 -4 -4 18 4.36 0.83 -3 -4 18 4.95 0.86 -2 -4 18 40.61 1.91 -1 -4 18 60.41 2.37 0 -4 18 44.50 1.99 1 -4 18 5.83 0.87 2 -4 18 7.77 0.96 -5 -3 18 7.91 1.00 -4 -3 18 0.41 0.58 -3 -3 18 32.44 1.69 -2 -3 18 42.47 1.94 -1 -3 18 27.10 1.58 0 -3 18 31.13 1.62 1 -3 18 9.55 1.03 2 -3 18 0.78 0.60 -5 -2 18 2.00 0.72 -4 -2 18 4.09 0.79 -3 -2 18 13.99 1.23 -2 -2 18 27.71 1.57 -1 -2 18 33.80 1.41 0 -2 18 24.17 1.31 1 -2 18 11.69 0.90 2 -2 18 0.00 1.05 -5 -1 18 0.33 0.59 -4 -1 18 1.72 0.69 -3 -1 18 14.00 0.87 -2 -1 18 26.24 1.13 -1 -1 18 33.46 1.74 0 -1 18 17.88 1.19 1 -1 18 20.58 1.19 2 -1 18 1.34 0.92 -5 0 18 0.25 0.88 -4 0 18 6.30 0.81 -3 0 18 22.12 1.09 -2 0 18 29.70 1.66 -1 0 18 8.55 0.99 0 0 18 17.23 1.09 1 0 18 10.10 0.89 2 0 18 0.36 0.64 -4 1 18 25.78 1.21 -3 1 18 13.71 0.88 -2 1 18 17.90 1.41 -1 1 18 2.77 0.58 0 1 18 4.43 0.66 1 1 18 7.44 0.96 -4 2 18 16.52 0.95 -3 2 18 13.11 0.83 -2 2 18 6.65 0.85 -1 2 18 39.29 1.56 0 2 18 6.95 0.79 -3 3 18 25.02 1.09 -2 3 18 19.49 1.07 -1 3 18 19.73 1.18 -2 -6 19 6.55 0.97 -1 -6 19 14.03 1.26 -3 -5 19 19.65 1.47 -2 -5 19 25.36 1.64 -1 -5 19 12.74 1.21 0 -5 19 2.61 0.79 -3 -4 19 39.88 1.93 -2 -4 19 10.77 1.13 -1 -4 19 1.28 0.65 0 -4 19 1.80 0.69 -3 -3 19 17.30 1.37 -2 -3 19 30.84 1.69 -1 -3 19 7.76 1.00 0 -3 19 2.72 0.74 -3 -2 19 17.94 1.40 -2 -2 19 4.46 0.86 -1 -2 19 1.90 1.08 0 -2 19 0.48 0.66 -3 -1 19 27.02 1.68 -2 -1 19 15.77 1.04 -1 -1 19 0.00 0.77 0 -1 19 5.90 0.96 -2 0 19 1.13 0.75 -1 0 19 0.20 0.58 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 45142 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969302' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_4 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C72 H50 Cl6 Eu2 N6 O14' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 1739.80 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.938(3) _cell_length_b 13.296(3) _cell_length_c 13.692(3) _cell_angle_alpha 85.412(4) _cell_angle_beta 85.738(4) _cell_angle_gamma 71.375(4) _cell_volume 1706.6(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21895 _cell_measurement_theta_min 5.1128 _cell_measurement_theta_max 44.367 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_F_000 864 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 2.127 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6253 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21893 _diffrn_reflns_av_unetI/netI 0.0865 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.494 _diffrn_reflns_theta_max 27.252 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 7586 _reflns_number_gt 6276 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0325P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7586 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.0978 _refine_ls_wR_factor_gt 0.0917 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Eu1 Eu 0.13925(2) 0.29926(2) 0.99384(2) 0.01298(8) Uani 1 1 d . . . . . Cl3 Cl 0.17312(14) 0.54218(11) 0.40263(8) 0.0265(3) Uani 1 1 d . . . . . Cl1 Cl 0.61275(15) 0.33305(13) 1.50514(10) 0.0382(4) Uani 1 1 d . . . . . Cl2 Cl 0.2566(2) 0.01370(14) 0.41318(12) 0.0589(5) Uani 1 1 d . . . . . O5 O 0.1533(3) 0.4430(2) 0.8904(2) 0.0165(7) Uani 1 1 d . . . . . O3 O 0.1055(3) 0.2433(2) 0.8395(2) 0.0174(7) Uani 1 1 d . . . . . O1 O 0.2816(3) 0.2264(2) 1.1374(2) 0.0190(7) Uani 1 1 d . . . . . O2 O 0.3138(4) 0.3752(3) 1.0700(2) 0.0236(8) Uani 1 1 d . . . . . O4 O -0.1174(3) 0.2723(3) 0.7980(2) 0.0255(8) Uani 1 1 d . . . . . O6 O 0.0266(3) 0.4067(2) 1.1231(2) 0.0199(7) Uani 1 1 d . . . . . OW1 O -0.1164(4) 0.3835(3) 0.9563(3) 0.0230(8) Uani 1 1 d D . . . . N1 N 0.3845(4) 0.2241(3) 0.9036(3) 0.0142(8) Uani 1 1 d . . . . . N3 N -0.0008(4) 0.1860(3) 1.0903(3) 0.0154(8) Uani 1 1 d . . . . . N2 N 0.2452(4) 0.0925(3) 0.9862(3) 0.0143(8) Uani 1 1 d . . . . . C16 C 0.3284(5) 0.3052(4) 1.1402(3) 0.0178(10) Uani 1 1 d . . . . . C30 C 0.0728(5) 0.5196(3) 0.8408(3) 0.0151(10) Uani 1 1 d . . . . . C5 C 0.4317(5) 0.1236(4) 0.8772(3) 0.0157(10) Uani 1 1 d . . . . . C17 C 0.4021(5) 0.3117(4) 1.2301(3) 0.0164(10) Uani 1 1 d . . . . . C23 C 0.0142(5) 0.2402(4) 0.7809(3) 0.0182(10) Uani 1 1 d . . . . . C7 C 0.4034(5) -0.0585(4) 0.9078(3) 0.0171(10) Uani 1 1 d . . . . . H7 H 0.4803 -0.0865 0.8642 0.021 Uiso 1 1 calc R U . . . C6 C 0.3574(5) 0.0498(4) 0.9242(3) 0.0160(10) Uani 1 1 d . . . . . C31 C 0.0971(5) 0.5240(3) 0.7317(3) 0.0144(9) Uani 1 1 d . . . . . C10 C 0.1788(5) 0.0287(3) 1.0354(3) 0.0124(9) Uani 1 1 d . . . . . C11 C 0.0591(5) 0.0788(3) 1.1052(3) 0.0157(10) Uani 1 1 d . . . . . C9 C 0.2194(5) -0.0809(4) 1.0215(4) 0.0187(10) Uani 1 1 d . . . . . H9 H 0.1705 -0.1235 1.0547 0.022 Uiso 1 1 calc R U . . . C1 C 0.4534(5) 0.2920(4) 0.8665(3) 0.0174(10) Uani 1 1 d . . . . . H1 H 0.4220 0.3612 0.8867 0.021 Uiso 1 1 calc R U . . . C24 C 0.0735(5) 0.1884(4) 0.6859(3) 0.0161(10) Uani 1 1 d . . . . . C25 C 0.2199(5) 0.1518(4) 0.6653(4) 0.0237(11) Uani 1 1 d . . . . . H25 H 0.2808 0.1637 0.7082 0.028 Uiso 1 1 calc R U . . . C27 C 0.1839(6) 0.0834(4) 0.5175(4) 0.0296(13) Uani 1 1 d . . . . . C15 C -0.1140(5) 0.2335(4) 1.1486(3) 0.0189(10) Uani 1 1 d . . . . . H15 H -0.1602 0.3057 1.1364 0.023 Uiso 1 1 calc R U . . . C28 C 0.0393(6) 0.1203(4) 0.5343(4) 0.0277(12) Uani 1 1 d . . . . . H28 H -0.0209 0.1103 0.4898 0.033 Uiso 1 1 calc R U . . . C34 C 0.1419(5) 0.5342(4) 0.5297(3) 0.0186(10) Uani 1 1 d . . . . . C32 C 0.1942(5) 0.4383(4) 0.6849(4) 0.0193(10) Uani 1 1 d . . . . . H32 H 0.2439 0.3778 0.7218 0.023 Uiso 1 1 calc R U . . . C22 C 0.4632(5) 0.3924(4) 1.2366(4) 0.0222(11) Uani 1 1 d . . . . . H22 H 0.4602 0.4414 1.1838 0.027 Uiso 1 1 calc R U . . . C14 C -0.1663(5) 0.1804(4) 1.2265(4) 0.0214(11) Uani 1 1 d . . . . . H14 H -0.2432 0.2168 1.2667 0.026 Uiso 1 1 calc R U . . . C12 C 0.0116(5) 0.0205(4) 1.1810(3) 0.0207(11) Uani 1 1 d . . . . . H12 H 0.0553 -0.0524 1.1900 0.025 Uiso 1 1 calc R U . . . C18 C 0.4093(5) 0.2377(4) 1.3090(4) 0.0236(11) Uani 1 1 d . . . . . H18 H 0.3693 0.1838 1.3052 0.028 Uiso 1 1 calc R U . . . C8 C 0.3336(5) -0.1235(4) 0.9571(4) 0.0214(11) Uani 1 1 d . . . . . H8 H 0.3635 -0.1959 0.9471 0.026 Uiso 1 1 calc R U . . . C19 C 0.4753(5) 0.2432(4) 1.3930(4) 0.0276(12) Uani 1 1 d . . . . . H19 H 0.4815 0.1930 1.4452 0.033 Uiso 1 1 calc R U . . . C21 C 0.5276(5) 0.4000(4) 1.3204(4) 0.0266(12) Uani 1 1 d . . . . . H21 H 0.5670 0.4541 1.3248 0.032 Uiso 1 1 calc R U . . . C3 C 0.6141(5) 0.1617(4) 0.7703(4) 0.0243(11) Uani 1 1 d . . . . . H3 H 0.6896 0.1410 0.7242 0.029 Uiso 1 1 calc R U . . . C33 C 0.2163(5) 0.4432(4) 0.5840(3) 0.0194(10) Uani 1 1 d . . . . . H33 H 0.2804 0.3862 0.5528 0.023 Uiso 1 1 calc R U . . . C29 C -0.0157(6) 0.1731(4) 0.6191(3) 0.0226(11) Uani 1 1 d . . . . . H29 H -0.1137 0.1985 0.6314 0.027 Uiso 1 1 calc R U . . . C2 C 0.5685(5) 0.2639(4) 0.7999(4) 0.0222(11) Uani 1 1 d . . . . . H2 H 0.6139 0.3128 0.7758 0.027 Uiso 1 1 calc R U . . . C35 C 0.0425(5) 0.6180(4) 0.5737(3) 0.0213(11) Uani 1 1 d . . . . . H35 H -0.0089 0.6771 0.5358 0.026 Uiso 1 1 calc R U . . . C36 C 0.0196(5) 0.6138(4) 0.6749(4) 0.0214(11) Uani 1 1 d . . . . . H36 H -0.0470 0.6703 0.7052 0.026 Uiso 1 1 calc R U . . . C20 C 0.5322(5) 0.3254(4) 1.3977(4) 0.0227(11) Uani 1 1 d . . . . . C4 C 0.5472(5) 0.0895(4) 0.8094(4) 0.0237(11) Uani 1 1 d . . . . . H4 H 0.5786 0.0196 0.7909 0.028 Uiso 1 1 calc R U . . . C13 C -0.1011(5) 0.0721(4) 1.2426(4) 0.0241(11) Uani 1 1 d . . . . . H13 H -0.1331 0.0346 1.2945 0.029 Uiso 1 1 calc R U . . . C26 C 0.2755(6) 0.0981(4) 0.5820(4) 0.0316(13) Uani 1 1 d . . . . . H26 H 0.3733 0.0722 0.5694 0.038 Uiso 1 1 calc R U . . . H37 H -0.185(6) 0.449(3) 0.977(6) 0.10(3) Uiso 1 1 d D . . . . H38 H -0.123(9) 0.335(5) 0.910(5) 0.10(3) Uiso 1 1 d 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 Eu1 0.01503(12) 0.01104(12) 0.01075(12) -0.00251(8) 0.00018(8) -0.00087(9) Cl3 0.0318(7) 0.0383(7) 0.0113(6) -0.0022(5) 0.0018(5) -0.0142(6) Cl1 0.0316(8) 0.0631(10) 0.0258(7) -0.0129(7) -0.0075(6) -0.0196(7) Cl2 0.0999(15) 0.0609(11) 0.0334(9) -0.0307(8) 0.0328(9) -0.0512(11) O5 0.0198(17) 0.0142(16) 0.0121(16) 0.0004(13) -0.0025(13) -0.0006(13) O3 0.0176(17) 0.0176(17) 0.0159(17) -0.0050(13) -0.0013(14) -0.0031(14) O1 0.0193(17) 0.0137(17) 0.0220(18) -0.0018(14) -0.0075(14) -0.0010(14) O2 0.032(2) 0.0245(19) 0.0138(17) -0.0043(15) 0.0002(15) -0.0085(16) O4 0.0167(18) 0.039(2) 0.0227(19) -0.0068(16) 0.0002(15) -0.0105(16) O6 0.0232(18) 0.0182(17) 0.0140(17) -0.0046(14) 0.0005(14) -0.0001(14) OW1 0.0174(18) 0.025(2) 0.0199(19) -0.0039(16) -0.0009(15) 0.0033(15) N1 0.0116(19) 0.017(2) 0.0129(19) -0.0009(16) -0.0063(15) -0.0012(16) N3 0.0135(19) 0.016(2) 0.016(2) -0.0046(16) 0.0010(16) -0.0044(16) N2 0.0129(19) 0.0136(19) 0.016(2) -0.0036(16) -0.0033(15) -0.0020(15) C16 0.017(2) 0.016(2) 0.016(2) -0.0038(19) 0.0035(19) 0.0009(19) C30 0.019(2) 0.014(2) 0.015(2) -0.0058(19) 0.0005(19) -0.0083(19) C5 0.009(2) 0.019(2) 0.016(2) -0.0039(19) -0.0049(18) 0.0004(18) C17 0.017(2) 0.018(2) 0.012(2) -0.0044(19) 0.0012(19) -0.0020(19) C23 0.021(3) 0.017(2) 0.018(2) 0.003(2) 0.000(2) -0.009(2) C7 0.014(2) 0.017(2) 0.016(2) -0.0023(19) -0.0034(19) 0.0018(19) C6 0.015(2) 0.016(2) 0.015(2) -0.0051(19) -0.0042(19) 0.0002(19) C31 0.014(2) 0.015(2) 0.014(2) -0.0043(18) 0.0014(18) -0.0042(18) C10 0.015(2) 0.010(2) 0.011(2) 0.0025(17) -0.0039(18) -0.0024(18) C11 0.016(2) 0.013(2) 0.018(2) 0.0012(19) -0.0073(19) -0.0031(18) C9 0.018(2) 0.012(2) 0.024(3) 0.001(2) -0.003(2) -0.0024(19) C1 0.016(2) 0.018(2) 0.017(2) 0.0010(19) -0.0022(19) -0.005(2) C24 0.025(3) 0.014(2) 0.013(2) -0.0002(18) -0.0004(19) -0.011(2) C25 0.029(3) 0.024(3) 0.020(3) -0.008(2) 0.005(2) -0.010(2) C27 0.055(4) 0.024(3) 0.017(3) -0.005(2) 0.011(3) -0.025(3) C15 0.016(2) 0.016(2) 0.022(3) -0.005(2) 0.000(2) -0.0004(19) C28 0.048(4) 0.030(3) 0.015(3) 0.000(2) -0.006(2) -0.026(3) C34 0.023(3) 0.022(3) 0.013(2) -0.0041(19) 0.0029(19) -0.009(2) C32 0.019(2) 0.015(2) 0.024(3) -0.004(2) -0.003(2) -0.004(2) C22 0.026(3) 0.025(3) 0.016(2) 0.000(2) -0.001(2) -0.009(2) C14 0.019(3) 0.022(3) 0.021(3) -0.005(2) 0.005(2) -0.005(2) C12 0.025(3) 0.018(2) 0.018(3) 0.003(2) 0.001(2) -0.007(2) C18 0.027(3) 0.024(3) 0.023(3) -0.002(2) 0.000(2) -0.013(2) C8 0.021(3) 0.018(3) 0.024(3) -0.008(2) -0.007(2) -0.002(2) C19 0.029(3) 0.036(3) 0.018(3) -0.003(2) 0.000(2) -0.010(2) C21 0.027(3) 0.029(3) 0.028(3) -0.008(2) 0.003(2) -0.013(2) C3 0.018(3) 0.035(3) 0.021(3) -0.007(2) 0.001(2) -0.009(2) C33 0.018(2) 0.020(2) 0.019(3) -0.010(2) 0.005(2) -0.003(2) C29 0.030(3) 0.024(3) 0.019(3) 0.002(2) -0.004(2) -0.015(2) C2 0.018(2) 0.029(3) 0.022(3) 0.002(2) -0.003(2) -0.011(2) C35 0.029(3) 0.020(3) 0.012(2) 0.001(2) -0.003(2) -0.004(2) C36 0.024(3) 0.016(2) 0.021(3) -0.006(2) 0.001(2) -0.002(2) C20 0.014(2) 0.036(3) 0.020(3) -0.009(2) -0.004(2) -0.008(2) C4 0.017(3) 0.027(3) 0.025(3) -0.010(2) 0.000(2) -0.003(2) C13 0.027(3) 0.024(3) 0.022(3) 0.004(2) 0.003(2) -0.010(2) C26 0.035(3) 0.032(3) 0.032(3) -0.007(3) 0.016(3) -0.018(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 Eu1 O5 2.321(3) . ? Eu1 O6 2.348(3) . ? Eu1 O3 2.376(3) . ? Eu1 O1 2.457(3) . ? Eu1 OW1 2.502(3) . ? Eu1 N1 2.581(4) . ? Eu1 O2 2.583(3) . ? Eu1 N3 2.587(4) . ? Eu1 N2 2.619(4) . ? Eu1 C16 2.870(5) . ? Eu1 H38 2.81(7) . ? Cl3 C34 1.745(5) . ? Cl1 C20 1.751(5) . ? Cl2 C27 1.747(5) . ? O5 C30 1.260(5) . ? O3 C23 1.267(5) . ? O1 C16 1.278(5) . ? O2 C16 1.266(6) . ? O4 C23 1.250(6) . ? O6 C30 1.252(5) 2_567 ? OW1 H37 0.97(2) . ? OW1 H38 0.96(2) . ? N1 C5 1.338(6) . ? N1 C1 1.346(6) . ? N3 C15 1.340(6) . ? N3 C11 1.363(6) . ? N2 C10 1.346(6) . ? N2 C6 1.348(6) . ? C16 C17 1.500(6) . ? C30 O6 1.251(5) 2_567 ? C30 C31 1.495(6) . ? C5 C4 1.401(6) . ? C5 C6 1.487(6) . ? C17 C18 1.392(7) . ? C17 C22 1.402(6) . ? C23 C24 1.511(6) . ? C7 C8 1.380(7) . ? C7 C6 1.396(6) . ? C7 H7 0.9300 . ? C31 C32 1.402(6) . ? C31 C36 1.406(6) . ? C10 C9 1.406(6) . ? C10 C11 1.483(6) . ? C11 C12 1.390(6) . ? C9 C8 1.381(6) . ? C9 H9 0.9300 . ? C1 C2 1.381(6) . ? C1 H1 0.9300 . ? C24 C29 1.389(6) . ? C24 C25 1.393(7) . ? C25 C26 1.378(7) . ? C25 H25 0.9300 . ? C27 C28 1.370(8) . ? C27 C26 1.382(8) . ? C15 C14 1.392(7) . ? C15 H15 0.9300 . ? C28 C29 1.390(7) . ? C28 H28 0.9300 . ? C34 C35 1.377(6) . ? C34 C33 1.390(7) . ? C32 C33 1.382(7) . ? C32 H32 0.9300 . ? C22 C21 1.380(7) . ? C22 H22 0.9300 . ? C14 C13 1.384(7) . ? C14 H14 0.9300 . ? C12 C13 1.378(7) . ? C12 H12 0.9300 . ? C18 C19 1.384(7) . ? C18 H18 0.9300 . ? C8 H8 0.9300 . ? C19 C20 1.388(7) . ? C19 H19 0.9300 . ? C21 C20 1.385(7) . ? C21 H21 0.9300 . ? C3 C2 1.372(7) . ? C3 C4 1.387(7) . ? C3 H3 0.9300 . ? C33 H33 0.9300 . ? C29 H29 0.9300 . ? C2 H2 0.9300 . ? C35 C36 1.387(6) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C4 H4 0.9300 . ? C13 H13 0.9300 . ? C26 H26 0.9300 . ? 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 Eu1 O6 93.22(11) . . ? O5 Eu1 O3 78.90(11) . . ? O6 Eu1 O3 144.23(11) . . ? O5 Eu1 O1 125.80(11) . . ? O6 Eu1 O1 73.77(11) . . ? O3 Eu1 O1 138.40(10) . . ? O5 Eu1 OW1 79.38(11) . . ? O6 Eu1 OW1 72.33(11) . . ? O3 Eu1 OW1 71.93(11) . . ? O1 Eu1 OW1 138.55(11) . . ? O5 Eu1 N1 77.68(11) . . ? O6 Eu1 N1 141.36(11) . . ? O3 Eu1 N1 71.41(11) . . ? O1 Eu1 N1 81.43(11) . . ? OW1 Eu1 N1 139.68(11) . . ? O5 Eu1 O2 73.81(11) . . ? O6 Eu1 O2 68.94(11) . . ? O3 Eu1 O2 138.38(10) . . ? O1 Eu1 O2 52.23(10) . . ? OW1 Eu1 O2 130.81(11) . . ? N1 Eu1 O2 72.47(11) . . ? O5 Eu1 N3 152.48(12) . . ? O6 Eu1 N3 77.71(12) . . ? O3 Eu1 N3 93.26(11) . . ? O1 Eu1 N3 76.99(11) . . ? OW1 Eu1 N3 73.12(12) . . ? N1 Eu1 N3 125.08(12) . . ? O2 Eu1 N3 124.61(11) . . ? O5 Eu1 N2 134.44(11) . . ? O6 Eu1 N2 131.60(11) . . ? O3 Eu1 N2 68.65(11) . . ? O1 Eu1 N2 71.00(11) . . ? OW1 Eu1 N2 117.34(12) . . ? N1 Eu1 N2 62.39(12) . . ? O2 Eu1 N2 110.89(11) . . ? N3 Eu1 N2 62.90(12) . . ? O5 Eu1 C16 99.99(12) . . ? O6 Eu1 C16 66.34(12) . . ? O3 Eu1 C16 149.20(12) . . ? O1 Eu1 C16 26.33(11) . . ? OW1 Eu1 C16 138.58(12) . . ? N1 Eu1 C16 78.25(12) . . ? O2 Eu1 C16 26.18(11) . . ? N3 Eu1 C16 99.95(13) . . ? N2 Eu1 C16 92.83(12) . . ? O5 Eu1 H38 84.3(16) . . ? O6 Eu1 H38 90.9(10) . . ? O3 Eu1 H38 53.8(11) . . ? O1 Eu1 H38 146.1(16) . . ? OW1 Eu1 H38 19.7(9) . . ? N1 Eu1 H38 124.7(12) . . ? O2 Eu1 H38 148.8(11) . . ? N3 Eu1 H38 70.1(16) . . ? N2 Eu1 H38 100.3(11) . . ? C16 Eu1 H38 156.9(11) . . ? C30 O5 Eu1 139.1(3) . . ? C23 O3 Eu1 145.0(3) . . ? C16 O1 Eu1 95.2(3) . . ? C16 O2 Eu1 89.7(3) . . ? C30 O6 Eu1 152.4(3) 2_567 . ? Eu1 OW1 H37 130(5) . . ? Eu1 OW1 H38 99(5) . . ? H37 OW1 H38 130(7) . . ? C5 N1 C1 118.8(4) . . ? C5 N1 Eu1 121.2(3) . . ? C1 N1 Eu1 118.8(3) . . ? C15 N3 C11 117.2(4) . . ? C15 N3 Eu1 119.5(3) . . ? C11 N3 Eu1 120.7(3) . . ? C10 N2 C6 119.2(4) . . ? C10 N2 Eu1 120.3(3) . . ? C6 N2 Eu1 120.1(3) . . ? O2 C16 O1 121.6(4) . . ? O2 C16 C17 120.9(4) . . ? O1 C16 C17 117.5(4) . . ? O2 C16 Eu1 64.2(3) . . ? O1 C16 Eu1 58.5(2) . . ? C17 C16 Eu1 168.8(3) . . ? O6 C30 O5 124.3(4) 2_567 . ? O6 C30 C31 117.3(4) 2_567 . ? O5 C30 C31 118.4(4) . . ? N1 C5 C4 121.2(4) . . ? N1 C5 C6 117.0(4) . . ? C4 C5 C6 121.8(4) . . ? C18 C17 C22 119.1(4) . . ? C18 C17 C16 120.0(4) . . ? C22 C17 C16 120.9(4) . . ? O4 C23 O3 125.1(4) . . ? O4 C23 C24 119.2(4) . . ? O3 C23 C24 115.7(4) . . ? C8 C7 C6 119.2(4) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? N2 C6 C7 121.5(4) . . ? N2 C6 C5 116.4(4) . . ? C7 C6 C5 122.1(4) . . ? C32 C31 C36 119.4(4) . . ? C32 C31 C30 120.6(4) . . ? C36 C31 C30 119.9(4) . . ? N2 C10 C9 122.0(4) . . ? N2 C10 C11 117.1(4) . . ? C9 C10 C11 120.9(4) . . ? N3 C11 C12 122.3(4) . . ? N3 C11 C10 115.4(4) . . ? C12 C11 C10 122.3(4) . . ? C8 C9 C10 118.3(4) . . ? C8 C9 H9 120.9 . . ? C10 C9 H9 120.9 . . ? N1 C1 C2 123.2(4) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C29 C24 C25 118.7(4) . . ? C29 C24 C23 121.0(4) . . ? C25 C24 C23 120.3(4) . . ? C26 C25 C24 120.7(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C28 C27 C26 121.7(5) . . ? C28 C27 Cl2 119.9(4) . . ? C26 C27 Cl2 118.4(5) . . ? N3 C15 C14 123.5(4) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? C27 C28 C29 118.7(5) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C35 C34 C33 121.5(4) . . ? C35 C34 Cl3 119.1(4) . . ? C33 C34 Cl3 119.4(4) . . ? C33 C32 C31 120.3(4) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C21 C22 C17 120.9(5) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C13 C14 C15 118.4(4) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C19 C18 C17 120.8(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C7 C8 C9 119.8(4) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C18 C19 C20 118.6(5) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C22 C21 C20 118.6(5) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C2 C3 C4 119.9(5) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C32 C33 C34 119.3(4) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? C24 C29 C28 120.9(5) . . ? C24 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C3 C2 C1 118.0(5) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 121.0 . . ? C34 C35 C36 119.6(4) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C31 119.9(4) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C21 C20 C19 122.0(5) . . ? C21 C20 Cl1 119.7(4) . . ? C19 C20 Cl1 118.3(4) . . ? C3 C4 C5 118.8(5) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C12 C13 C14 119.3(4) . . ? C12 C13 H13 120.4 . . ? C14 C13 H13 120.4 . . ? C25 C26 C27 119.1(5) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? _refine_diff_density_max 1.621 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.152 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 9.9376 13.2957 13.6919 85.412 85.738 71.375 ZERR 1.00 0.0025 0.0033 0.0034 0.004 0.004 0.004 LATT 1 SFAC C H N O CL EU UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H38 DFIX 0.98 OW1 H37 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 12 WGHT 0.032500 FVAR 0.11985 EU1 6 0.139255 0.299259 0.993841 11.00000 0.01503 0.01104 = 0.01075 -0.00251 0.00018 -0.00087 CL3 5 0.173124 0.542176 0.402634 11.00000 0.03178 0.03834 = 0.01128 -0.00218 0.00177 -0.01419 CL1 5 0.612753 0.333046 1.505140 11.00000 0.03159 0.06314 = 0.02582 -0.01287 -0.00750 -0.01959 CL2 5 0.256630 0.013699 0.413177 11.00000 0.09987 0.06093 = 0.03341 -0.03071 0.03277 -0.05119 O5 4 0.153258 0.443020 0.890418 11.00000 0.01981 0.01417 = 0.01209 0.00041 -0.00250 -0.00058 O3 4 0.105466 0.243346 0.839495 11.00000 0.01760 0.01761 = 0.01590 -0.00500 -0.00131 -0.00310 O1 4 0.281611 0.226431 1.137439 11.00000 0.01934 0.01365 = 0.02199 -0.00176 -0.00753 -0.00098 O2 4 0.313769 0.375208 1.070034 11.00000 0.03237 0.02449 = 0.01378 -0.00432 0.00019 -0.00846 O4 4 -0.117436 0.272253 0.797968 11.00000 0.01670 0.03909 = 0.02274 -0.00679 0.00021 -0.01054 O6 4 0.026551 0.406707 1.123085 11.00000 0.02317 0.01825 = 0.01395 -0.00457 0.00045 -0.00007 OW1 4 -0.116427 0.383468 0.956267 11.00000 0.01742 0.02502 = 0.01993 -0.00387 -0.00092 0.00332 N1 3 0.384507 0.224113 0.903586 11.00000 0.01164 0.01661 = 0.01291 -0.00094 -0.00627 -0.00124 N3 3 -0.000779 0.186050 1.090251 11.00000 0.01346 0.01645 = 0.01635 -0.00460 0.00102 -0.00437 N2 3 0.245224 0.092486 0.986154 11.00000 0.01286 0.01363 = 0.01567 -0.00358 -0.00327 -0.00200 C16 1 0.328363 0.305188 1.140245 11.00000 0.01715 0.01560 = 0.01614 -0.00379 0.00353 0.00090 C30 1 0.072784 0.519583 0.840809 11.00000 0.01871 0.01403 = 0.01540 -0.00579 0.00051 -0.00827 C5 1 0.431659 0.123566 0.877198 11.00000 0.00947 0.01904 = 0.01629 -0.00391 -0.00488 0.00036 C17 1 0.402111 0.311718 1.230133 11.00000 0.01696 0.01761 = 0.01235 -0.00435 0.00124 -0.00198 C23 1 0.014247 0.240162 0.780941 11.00000 0.02129 0.01678 = 0.01767 0.00340 -0.00042 -0.00863 C7 1 0.403444 -0.058497 0.907815 11.00000 0.01439 0.01684 = 0.01602 -0.00226 -0.00338 0.00177 AFIX 43 H7 2 0.480294 -0.086505 0.864186 11.00000 -1.20000 AFIX 0 C6 1 0.357381 0.049788 0.924175 11.00000 0.01548 0.01565 = 0.01455 -0.00513 -0.00422 0.00024 C31 1 0.097117 0.524046 0.731678 11.00000 0.01412 0.01459 = 0.01449 -0.00434 0.00137 -0.00415 C10 1 0.178760 0.028660 1.035386 11.00000 0.01507 0.01027 = 0.01058 0.00254 -0.00389 -0.00238 C11 1 0.059071 0.078795 1.105209 11.00000 0.01590 0.01306 = 0.01791 0.00115 -0.00732 -0.00312 C9 1 0.219354 -0.080878 1.021453 11.00000 0.01793 0.01243 = 0.02411 0.00076 -0.00343 -0.00242 AFIX 43 H9 2 0.170510 -0.123470 1.054691 11.00000 -1.20000 AFIX 0 C1 1 0.453418 0.292043 0.866508 11.00000 0.01631 0.01827 = 0.01692 0.00097 -0.00223 -0.00471 AFIX 43 H1 2 0.421980 0.361233 0.886735 11.00000 -1.20000 AFIX 0 C24 1 0.073505 0.188416 0.685949 11.00000 0.02452 0.01405 = 0.01297 -0.00019 -0.00043 -0.01084 C25 1 0.219887 0.151781 0.665319 11.00000 0.02884 0.02409 = 0.01988 -0.00760 0.00463 -0.01043 AFIX 43 H25 2 0.280760 0.163676 0.708226 11.00000 -1.20000 AFIX 0 C27 1 0.183860 0.083393 0.517499 11.00000 0.05522 0.02377 = 0.01747 -0.00501 0.01133 -0.02502 C15 1 -0.114045 0.233508 1.148578 11.00000 0.01588 0.01632 = 0.02155 -0.00459 0.00048 -0.00039 AFIX 43 H15 2 -0.160150 0.305742 1.136361 11.00000 -1.20000 AFIX 0 C28 1 0.039310 0.120342 0.534298 11.00000 0.04846 0.02959 = 0.01527 0.00002 -0.00552 -0.02604 AFIX 43 H28 2 -0.020859 0.110311 0.489783 11.00000 -1.20000 AFIX 0 C34 1 0.141901 0.534225 0.529699 11.00000 0.02258 0.02160 = 0.01265 -0.00415 0.00293 -0.00857 C32 1 0.194199 0.438271 0.684867 11.00000 0.01905 0.01496 = 0.02365 -0.00396 -0.00306 -0.00377 AFIX 43 H32 2 0.243910 0.377811 0.721838 11.00000 -1.20000 AFIX 0 C22 1 0.463152 0.392410 1.236611 11.00000 0.02569 0.02478 = 0.01646 0.00020 -0.00067 -0.00891 AFIX 43 H22 2 0.460205 0.441441 1.183763 11.00000 -1.20000 AFIX 0 C14 1 -0.166319 0.180400 1.226472 11.00000 0.01949 0.02243 = 0.02102 -0.00513 0.00457 -0.00517 AFIX 43 H14 2 -0.243190 0.216793 1.266688 11.00000 -1.20000 AFIX 0 C12 1 0.011551 0.020535 1.181022 11.00000 0.02456 0.01835 = 0.01844 0.00313 0.00086 -0.00702 AFIX 43 H12 2 0.055340 -0.052430 1.190037 11.00000 -1.20000 AFIX 0 C18 1 0.409332 0.237664 1.308979 11.00000 0.02730 0.02403 = 0.02288 -0.00222 0.00010 -0.01294 AFIX 43 H18 2 0.369330 0.183783 1.305176 11.00000 -1.20000 AFIX 0 C8 1 0.333648 -0.123540 0.957123 11.00000 0.02136 0.01829 = 0.02363 -0.00757 -0.00708 -0.00213 AFIX 43 H8 2 0.363493 -0.195878 0.947059 11.00000 -1.20000 AFIX 0 C19 1 0.475330 0.243229 1.392997 11.00000 0.02893 0.03569 = 0.01829 -0.00336 -0.00033 -0.01016 AFIX 43 H19 2 0.481487 0.192969 1.445186 11.00000 -1.20000 AFIX 0 C21 1 0.527561 0.400030 1.320394 11.00000 0.02651 0.02864 = 0.02828 -0.00826 0.00347 -0.01330 AFIX 43 H21 2 0.567023 0.454103 1.324815 11.00000 -1.20000 AFIX 0 C3 1 0.614056 0.161743 0.770333 11.00000 0.01766 0.03530 = 0.02067 -0.00658 0.00150 -0.00879 AFIX 43 H3 2 0.689640 0.140971 0.724165 11.00000 -1.20000 AFIX 0 C33 1 0.216347 0.443177 0.584010 11.00000 0.01836 0.01970 = 0.01865 -0.01034 0.00535 -0.00313 AFIX 43 H33 2 0.280367 0.386179 0.552816 11.00000 -1.20000 AFIX 0 C29 1 -0.015743 0.173115 0.619144 11.00000 0.02961 0.02399 = 0.01870 0.00159 -0.00379 -0.01500 AFIX 43 H29 2 -0.113719 0.198547 0.631370 11.00000 -1.20000 AFIX 0 C2 1 0.568534 0.263921 0.799888 11.00000 0.01762 0.02889 = 0.02200 0.00234 -0.00327 -0.01055 AFIX 43 H2 2 0.613865 0.312800 0.775767 11.00000 -1.20000 AFIX 0 C35 1 0.042509 0.618042 0.573709 11.00000 0.02868 0.01995 = 0.01237 0.00131 -0.00288 -0.00366 AFIX 43 H35 2 -0.008912 0.677104 0.535814 11.00000 -1.20000 AFIX 0 C36 1 0.019577 0.613819 0.674910 11.00000 0.02419 0.01641 = 0.02075 -0.00589 0.00120 -0.00163 AFIX 43 H36 2 -0.047001 0.670301 0.705159 11.00000 -1.20000 AFIX 0 C20 1 0.532151 0.325402 1.397745 11.00000 0.01444 0.03591 = 0.01988 -0.00933 -0.00419 -0.00823 C4 1 0.547219 0.089476 0.809392 11.00000 0.01713 0.02680 = 0.02542 -0.00995 -0.00043 -0.00267 AFIX 43 H4 2 0.578555 0.019619 0.790900 11.00000 -1.20000 AFIX 0 C13 1 -0.101134 0.072110 1.242640 11.00000 0.02662 0.02360 = 0.02173 0.00434 0.00263 -0.00977 AFIX 43 H13 2 -0.133059 0.034596 1.294520 11.00000 -1.20000 AFIX 0 C26 1 0.275464 0.098115 0.582036 11.00000 0.03515 0.03152 = 0.03173 -0.00729 0.01581 -0.01817 AFIX 43 H26 2 0.373330 0.072154 0.569444 11.00000 -1.20000 AFIX 0 H37 2 -0.184769 0.449189 0.976721 11.00000 0.09635 H38 2 -0.123010 0.335462 0.909669 11.00000 0.10087 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0446 for 6276 Fo > 4sig(Fo) and 0.0578 for all 7586 data REM 459 parameters refined using 2 restraints END WGHT 0.0325 0.0000 REM Highest difference peak 1.621, deepest hole -1.378, 1-sigma level 0.152 Q1 1 -0.4347 0.4597 1.0072 11.00000 0.05 1.62 Q2 1 0.1741 0.0581 0.3759 11.00000 0.05 1.13 Q3 1 0.0710 0.2745 0.9950 11.00000 0.05 0.67 Q4 1 0.3877 0.0046 0.4306 11.00000 0.05 0.67 Q5 1 0.1016 0.1383 0.4989 11.00000 0.05 0.60 Q6 1 0.0550 0.2053 0.7345 11.00000 0.05 0.59 Q7 1 -0.1157 0.7054 0.4386 11.00000 0.05 0.58 Q8 1 0.4269 0.1886 1.4861 11.00000 0.05 0.57 Q9 1 0.4420 0.4802 1.0330 11.00000 0.05 0.55 Q10 1 0.5572 -0.1581 0.8260 11.00000 0.05 0.53 ; _shelx_res_checksum 38825 _shelx_hkl_file ; -1 0 0 241.76 13.33 -1 0 0 232.91 13.66 1 0 0 249.95 13.67 1 0 0 239.62 12.13 1 0 0 240.40 12.15 -2 0 0 7.53 1.10 -2 0 0 5.97 1.17 2 0 0 6.92 0.89 2 0 0 6.63 0.98 -3 0 0 168.85 10.27 -3 0 0 163.93 10.34 3 0 0 166.25 9.21 3 0 0 172.93 9.03 -4 0 0 176.49 11.11 -4 0 0 193.87 11.51 4 0 0 174.41 9.66 4 0 0 172.22 9.97 -5 0 0 3.49 1.33 -5 0 0 2.34 1.37 5 0 0 2.78 1.03 5 0 0 1.79 0.77 -6 0 0 17.08 2.80 -6 0 0 19.07 3.48 6 0 0 18.45 2.66 6 0 0 23.40 2.44 -7 0 0 113.12 9.37 -7 0 0 113.39 8.56 7 0 0 121.64 7.31 7 0 0 124.50 8.01 -8 0 0 45.06 6.40 8 0 0 48.09 5.20 8 0 0 50.12 4.42 -9 0 0 -0.11 1.50 9 0 0 -1.61 0.83 -10 0 0 9.22 3.57 10 0 0 13.19 2.92 -11 0 0 10.99 3.92 11 0 0 11.93 3.01 -12 0 0 11.08 4.13 12 0 0 7.04 2.69 11 -1 0 1.34 1.42 -11 1 0 0.18 2.05 10 -1 0 23.01 3.97 -10 1 0 22.55 5.30 9 -1 0 29.88 4.29 -9 1 0 34.30 5.92 8 -1 0 14.64 2.81 8 -1 0 21.89 2.75 -8 1 0 12.79 3.48 7 -1 0 9.22 2.05 7 -1 0 7.60 1.59 -7 1 0 8.09 1.91 -7 1 0 11.95 2.99 6 -1 0 151.21 8.64 6 -1 0 152.49 9.20 -6 1 0 131.71 9.53 -6 1 0 150.94 10.74 5 -1 0 8.12 1.68 5 -1 0 9.06 1.53 -5 1 0 10.72 2.41 -5 1 0 8.93 1.76 4 -1 0 50.49 3.72 4 -1 0 47.32 3.42 -4 1 0 53.79 5.20 -4 1 0 49.57 3.85 3 -1 0 105.59 6.35 3 -1 0 106.14 6.10 -3 1 0 106.92 7.26 -3 1 0 110.21 6.85 2 -1 0 23.90 1.81 -2 1 0 27.99 2.10 -2 1 0 29.94 2.60 -2 1 0 23.81 2.62 1 -1 0 70.56 3.98 -1 1 0 75.80 4.20 -1 1 0 74.00 4.47 -1 1 0 74.82 4.57 0 -1 0 13.87 1.14 0 1 0 14.77 1.00 0 1 0 15.98 1.03 0 1 0 16.20 0.97 -1 -1 0 418.03 22.63 -1 -1 0 402.28 21.62 1 1 0 380.60 19.89 1 1 0 393.35 19.79 -2 -1 0 156.79 9.60 -2 -1 0 162.84 9.90 2 1 0 174.99 8.60 2 1 0 163.32 8.65 -3 -1 0 81.73 5.52 -3 -1 0 79.44 5.59 3 1 0 81.04 4.64 3 1 0 85.47 4.90 -4 -1 0 100.43 6.75 -4 -1 0 107.66 7.10 4 1 0 95.64 5.67 4 1 0 97.94 6.00 -5 -1 0 48.57 4.10 -5 -1 0 44.11 5.02 5 1 0 53.03 3.39 5 1 0 44.60 3.61 -6 -1 0 6.60 1.72 -6 -1 0 8.94 2.30 6 1 0 3.67 1.24 6 1 0 5.34 1.15 -7 -1 0 13.56 2.60 -7 -1 0 13.29 3.03 7 1 0 15.56 2.02 7 1 0 12.11 2.27 -8 -1 0 25.19 3.87 -8 -1 0 20.24 4.12 8 1 0 26.31 3.50 8 1 0 27.73 2.98 -9 -1 0 10.37 3.33 9 1 0 20.65 3.37 -10 -1 0 2.93 2.26 10 1 0 5.97 2.08 -11 -1 0 12.38 3.90 11 1 0 16.08 3.33 -12 -1 0 17.49 4.92 12 1 0 27.28 4.46 11 -2 0 19.42 3.79 -11 2 0 9.73 3.81 10 -2 0 0.70 1.33 -10 2 0 0.84 2.04 9 -2 0 13.65 2.95 -9 2 0 17.99 4.29 8 -2 0 61.80 4.75 8 -2 0 56.45 5.89 -8 2 0 63.27 7.96 7 -2 0 84.81 6.31 7 -2 0 73.01 5.52 -7 2 0 97.26 9.32 6 -2 0 14.10 2.13 6 -2 0 13.28 2.35 -6 2 0 9.80 1.92 -6 2 0 11.11 2.79 5 -2 0 121.29 7.72 5 -2 0 130.74 8.18 -5 2 0 132.40 8.48 -5 2 0 134.40 9.55 4 -2 0 177.69 9.60 -4 2 0 168.21 11.24 -4 2 0 166.94 10.56 3 -2 0 3.83 0.91 -3 2 0 4.89 1.34 -3 2 0 2.70 1.26 -3 2 0 3.67 0.97 2 -2 0 107.22 5.85 -2 2 0 106.27 6.49 -2 2 0 95.73 6.69 -1 2 0 3.05 0.65 -1 2 0 3.95 0.94 -1 2 0 2.12 0.70 -1 2 0 3.08 0.75 0 -2 0 101.85 6.43 0 2 0 104.27 5.99 0 2 0 108.39 5.57 0 2 0 104.70 5.65 -1 -2 0 10.49 1.50 -1 -2 0 10.28 0.96 1 2 0 12.27 1.08 1 2 0 10.26 1.11 1 2 0 11.54 1.00 -2 -2 0 18.63 1.89 -2 -2 0 20.29 2.31 2 2 0 19.76 1.50 2 2 0 23.61 1.63 -3 -2 0 7.66 1.44 -3 -2 0 9.92 1.72 3 2 0 9.34 1.23 3 2 0 10.05 1.24 -4 -2 0 100.23 7.15 -4 -2 0 106.68 7.17 4 2 0 108.80 6.20 4 2 0 104.32 6.02 -5 -2 0 13.85 2.43 -5 -2 0 14.08 2.33 5 2 0 10.62 1.47 5 2 0 8.81 1.57 -6 -2 0 63.01 5.42 -6 -2 0 67.02 6.71 6 2 0 67.42 4.78 6 2 0 70.05 4.47 -7 -2 0 44.50 5.62 -7 -2 0 44.96 5.00 7 2 0 45.91 3.48 7 2 0 44.18 4.35 -8 -2 0 27.58 4.74 -8 -2 0 35.63 4.60 8 2 0 30.69 3.29 8 2 0 33.85 3.95 -9 -2 0 3.78 2.25 9 2 0 0.49 1.00 -10 -2 0 22.34 5.04 10 2 0 34.88 4.47 -11 -2 0 18.39 4.85 11 2 0 19.76 3.66 -12 -2 0 2.59 2.63 12 2 0 -0.13 1.30 11 -3 0 16.07 3.69 -11 3 0 26.96 6.13 10 -3 0 23.36 4.08 -10 3 0 15.57 4.48 9 -3 0 4.65 1.87 -9 3 0 6.61 2.88 8 -3 0 10.34 2.09 -8 3 0 3.58 2.28 7 -3 0 63.88 4.83 7 -3 0 55.91 5.81 -7 3 0 51.96 6.99 6 -3 0 59.86 5.70 6 -3 0 60.94 4.62 -6 3 0 56.81 4.66 -6 3 0 68.35 7.39 5 -3 0 9.74 2.01 5 -3 0 6.63 1.46 -5 3 0 6.44 2.27 -5 3 0 9.46 1.67 4 -3 0 33.37 3.08 -4 3 0 33.41 2.90 -4 3 0 30.71 4.09 -4 3 0 36.61 3.95 3 -3 0 172.87 9.94 -3 3 0 189.50 11.61 -3 3 0 185.88 10.61 -3 3 0 180.27 11.07 2 -3 0 29.19 2.42 -2 3 0 38.43 3.65 -2 3 0 35.90 2.74 -2 3 0 34.81 3.25 -1 3 0 51.70 3.46 -1 3 0 49.40 3.14 -1 3 0 45.48 3.50 -1 3 0 45.48 3.23 0 -3 0 115.33 7.40 0 3 0 117.89 6.79 0 3 0 117.40 6.47 0 3 0 114.28 6.30 -1 -3 0 5.40 1.28 -1 -3 0 6.36 0.80 1 3 0 6.44 1.01 1 3 0 7.68 0.94 -2 -3 0 23.27 1.94 -2 -3 0 23.41 2.72 2 3 0 23.00 1.89 2 3 0 25.77 1.79 -3 -3 0 41.87 3.66 -3 -3 0 38.62 3.09 3 3 0 37.01 2.71 3 3 0 41.10 2.68 -4 -3 0 111.02 7.87 -4 -3 0 119.43 7.56 4 3 0 112.24 6.47 4 3 0 109.24 6.49 -5 -3 0 99.65 7.47 -5 -3 0 101.93 7.31 5 3 0 109.14 6.33 5 3 0 99.60 6.10 -6 -3 0 20.01 3.12 -6 -3 0 20.60 3.32 6 3 0 22.99 2.68 6 3 0 19.87 2.30 -7 -3 0 25.93 4.17 -7 -3 0 28.14 3.93 7 3 0 30.36 3.05 7 3 0 31.82 3.43 -8 -3 0 93.92 7.59 -8 -3 0 83.45 8.77 8 3 0 86.48 5.97 8 3 0 98.25 6.62 -9 -3 0 13.20 3.45 -9 -3 0 13.34 3.04 9 3 0 9.23 1.86 9 3 0 9.43 2.27 -10 -3 0 11.37 3.65 10 3 0 7.68 2.15 -11 -3 0 24.73 5.37 11 3 0 20.30 3.61 -12 -3 0 41.71 7.39 12 3 0 33.77 4.89 10 -4 0 7.33 2.42 -10 4 0 2.88 2.79 9 -4 0 33.63 4.85 -9 4 0 22.80 5.36 8 -4 0 50.72 5.87 -8 4 0 53.63 7.34 7 -4 0 18.96 2.86 7 -4 0 20.82 3.41 -7 4 0 18.02 3.98 6 -4 0 44.48 4.74 6 -4 0 44.81 4.26 -6 4 0 34.84 5.42 5 -4 0 147.00 8.78 -5 4 0 137.76 9.59 -5 4 0 145.67 10.69 -5 4 0 146.23 9.46 4 -4 0 74.14 4.84 -4 4 0 60.70 6.55 -4 4 0 69.89 5.16 -4 4 0 74.67 5.60 3 -4 0 11.80 1.73 -3 4 0 14.70 2.54 -3 4 0 13.41 2.26 -3 4 0 12.91 1.88 -2 4 0 110.24 6.86 -2 4 0 107.01 7.13 -2 4 0 115.38 7.48 -1 4 0 223.44 13.33 -1 4 0 222.98 11.91 -1 4 0 213.08 12.99 -1 4 0 226.52 11.99 0 -4 0 23.72 2.76 0 4 0 23.01 2.15 0 4 0 26.99 2.10 0 4 0 23.89 2.37 -1 -4 0 36.41 2.34 -1 -4 0 29.79 3.40 1 4 0 29.94 2.24 1 4 0 33.13 2.52 -2 -4 0 317.91 19.59 -2 -4 0 336.38 17.97 2 4 0 316.04 16.71 2 4 0 325.77 16.95 -3 -4 0 136.22 9.03 -3 -4 0 133.46 7.94 3 4 0 130.51 7.41 3 4 0 123.38 7.16 -4 -4 0 25.81 2.87 -4 -4 0 27.48 3.57 4 4 0 25.04 2.49 4 4 0 21.57 2.23 -5 -4 0 58.74 5.43 -5 -4 0 64.24 5.15 5 4 0 67.92 4.38 5 4 0 66.84 4.39 -6 -4 0 64.65 5.27 -6 -4 0 54.39 5.82 6 4 0 57.05 4.11 6 4 0 55.89 4.17 -7 -4 0 11.67 2.65 -7 -4 0 8.72 2.28 7 4 0 5.56 1.29 7 4 0 6.40 1.53 -8 -4 0 8.72 2.52 -8 -4 0 4.52 1.93 8 4 0 8.45 1.84 8 4 0 13.12 1.96 -9 -4 0 52.20 6.91 -9 -4 0 49.36 6.27 9 4 0 60.53 4.47 9 4 0 53.80 5.34 -10 -4 0 11.22 3.43 10 4 0 12.24 2.62 -11 -4 0 11.56 3.96 11 4 0 16.31 3.15 -12 -4 0 16.43 4.71 12 4 0 7.01 2.39 10 -5 0 15.82 3.55 -10 5 0 14.68 4.65 9 -5 0 4.15 1.85 -9 5 0 1.43 2.36 8 -5 0 4.39 1.96 -8 5 0 5.26 2.60 7 -5 0 32.35 3.95 7 -5 0 34.84 4.59 -7 5 0 38.74 5.89 6 -5 0 0.39 0.89 6 -5 0 -0.30 0.80 -6 5 0 0.55 1.38 5 -5 0 5.45 1.51 -5 5 0 6.60 1.95 -5 5 0 7.35 1.63 -5 5 0 5.20 2.08 4 -5 0 167.38 9.68 -4 5 0 153.98 10.34 -4 5 0 165.14 11.35 -4 5 0 165.23 10.52 3 -5 0 133.04 8.04 -3 5 0 135.72 8.59 -3 5 0 126.50 8.62 -3 5 0 142.14 9.35 -2 5 0 -0.43 0.64 -2 5 0 0.87 0.90 -2 5 0 0.20 0.70 -2 5 0 0.04 0.55 1 -5 0 1.89 0.96 -1 5 0 1.54 0.90 -1 5 0 4.24 1.09 -1 5 0 -0.13 0.55 0 -5 0 96.83 6.91 0 5 0 98.41 5.90 0 5 0 94.49 5.69 0 5 0 93.31 6.02 -1 -5 0 35.84 2.54 -1 -5 0 30.40 3.73 1 5 0 35.61 2.78 1 5 0 34.32 2.50 -2 -5 0 56.59 4.84 -2 -5 0 60.21 3.64 2 5 0 49.98 3.78 2 5 0 55.74 3.61 -3 -5 0 188.12 11.91 -3 -5 0 176.87 10.29 3 5 0 165.25 9.57 3 5 0 179.29 9.86 -4 -5 0 209.24 12.55 -4 -5 0 214.77 13.98 4 5 0 221.81 11.73 4 5 0 201.73 11.39 -5 -5 0 21.20 3.37 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1.76 9 7 0 5.48 1.71 -10 -7 0 84.66 9.76 -10 -7 0 102.12 10.18 10 7 0 97.59 7.07 -11 -7 0 6.74 3.04 11 7 0 8.72 2.36 -12 -7 0 0.62 2.16 12 7 0 0.75 1.40 8 -8 0 2.41 1.82 -8 8 0 7.39 3.25 7 -8 0 4.99 2.06 -7 8 0 5.90 2.90 6 -8 0 49.84 5.35 -6 8 0 47.96 6.30 -6 8 0 52.05 7.07 5 -8 0 34.30 4.17 -5 8 0 31.12 4.64 4 -8 0 12.08 2.41 4 -8 0 18.67 3.21 -4 8 0 17.56 3.34 -4 8 0 12.32 3.10 3 -8 0 116.68 7.90 3 -8 0 126.77 9.14 -3 8 0 116.40 8.98 -3 8 0 116.13 8.43 2 -8 0 90.49 7.10 -2 8 0 72.33 5.96 -2 8 0 81.83 5.87 -2 8 0 88.56 6.67 1 -8 0 0.96 1.19 -1 8 0 2.41 1.25 -1 8 0 2.14 1.10 -1 8 0 3.10 1.16 0 -8 0 62.60 4.54 0 -8 0 60.52 4.47 0 -8 0 68.05 5.92 0 8 0 60.34 4.70 0 8 0 57.34 4.50 -1 -8 0 137.12 8.27 -1 -8 0 133.41 10.03 1 8 0 131.09 8.40 1 8 0 129.75 7.96 -2 -8 0 26.62 4.09 -2 -8 0 19.13 1.99 2 8 0 19.49 2.75 2 8 0 24.17 2.57 -3 -8 0 35.52 4.89 -3 -8 0 31.56 2.60 3 8 0 30.98 3.54 3 8 0 41.09 3.53 -4 -8 0 209.83 14.17 -4 -8 0 187.47 11.47 4 8 0 198.09 11.07 4 8 0 192.67 11.51 -5 -8 0 8.03 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0 35.79 5.79 0 12 0 38.41 4.53 0 12 0 33.65 4.44 -1 -12 0 8.44 2.86 1 12 0 4.94 1.84 1 12 0 3.07 1.50 -2 -12 0 6.50 2.69 2 12 0 11.17 2.32 2 12 0 7.63 2.20 -3 -12 0 74.05 9.06 3 12 0 67.64 6.78 3 12 0 74.10 5.60 -4 -12 0 39.60 6.46 4 12 0 42.62 5.00 4 12 0 33.64 3.94 -5 -12 0 3.37 2.35 5 12 0 4.54 1.89 5 12 0 2.82 1.41 -6 -12 0 85.29 9.99 6 12 0 80.53 6.00 6 12 0 73.98 7.24 -7 -12 0 28.52 5.73 7 12 0 28.12 4.12 7 12 0 26.81 3.66 -8 -12 0 2.64 2.47 8 12 0 3.27 1.65 8 12 0 2.06 1.69 -9 -12 0 13.40 4.33 9 12 0 4.52 2.06 9 12 0 7.04 2.37 -10 -12 0 29.33 6.35 10 12 0 41.56 5.34 -11 -12 0 12.41 4.38 4 -13 0 4.03 2.12 -4 13 0 2.13 2.14 3 -13 0 42.70 5.62 -3 13 0 45.89 6.08 2 -13 0 21.96 3.87 -2 13 0 26.26 4.42 1 -13 0 2.46 2.17 -1 13 0 0.92 1.41 -1 13 0 -1.15 1.00 0 -13 0 80.47 9.47 0 13 0 86.33 7.87 0 13 0 89.01 7.92 -1 -13 0 57.40 7.87 1 13 0 56.18 6.10 1 13 0 59.49 6.01 -2 -13 0 6.71 2.84 2 13 0 1.35 1.37 2 13 0 3.12 1.58 -3 -13 0 1.85 2.26 3 13 0 2.00 1.45 3 13 0 5.47 2.00 -4 -13 0 48.85 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-2 0 -16 11.33 3.57 2 0 16 8.98 2.61 -3 0 -16 0.66 1.72 3 0 16 0.27 1.65 -4 0 -16 25.34 5.46 4 0 16 19.62 4.06 -5 0 -16 3.90 2.88 5 0 16 14.02 3.47 4 -1 -16 17.12 4.74 -4 1 16 27.28 6.37 3 -1 -16 1.08 2.46 -3 1 16 0.40 2.55 2 -1 -16 45.89 7.05 -2 1 16 31.09 6.75 1 -1 -16 34.86 6.02 -1 1 16 33.87 6.82 0 -1 -16 0.25 2.01 0 1 16 4.18 2.87 -1 -1 -16 1.21 2.01 1 1 16 -2.04 1.83 -2 -1 -16 28.26 5.30 2 1 16 37.88 6.10 2 1 16 27.51 4.33 -3 -1 -16 44.40 6.80 3 1 16 28.87 4.63 -4 -1 -16 0.90 2.02 4 1 16 0.26 1.51 -5 -1 -16 16.00 4.72 5 1 16 14.79 3.54 3 -2 -16 64.49 8.73 -3 2 16 40.03 7.82 2 -2 -16 -0.31 2.33 -2 2 16 -0.26 2.28 1 -2 -16 15.17 4.21 -1 2 16 16.67 4.76 0 -2 -16 18.84 4.57 0 2 16 33.32 6.36 -1 -2 -16 7.37 3.02 1 2 16 5.01 2.83 -2 -2 -16 15.54 4.12 2 2 16 9.73 2.71 2 2 16 18.16 4.65 -3 -2 -16 34.51 6.22 3 2 16 38.45 5.18 -4 -2 -16 59.79 8.45 4 2 16 54.27 6.52 -5 -2 -16 1.43 2.40 5 2 16 1.91 1.94 -6 -2 -16 14.82 4.56 6 2 16 11.59 3.44 3 -3 -16 2.09 2.71 -3 3 16 5.33 3.44 2 -3 -16 31.36 6.29 -2 3 16 9.96 4.20 1 -3 -16 9.82 3.72 -1 3 16 8.91 3.86 0 -3 -16 21.46 4.87 0 3 16 11.98 4.29 -1 -3 -16 38.83 6.66 1 3 16 55.34 8.15 -2 -3 -16 21.50 4.90 2 3 16 14.95 3.26 2 3 16 25.21 5.37 -3 -3 -16 2.52 2.05 3 3 16 3.25 1.92 -4 -3 -16 9.85 3.58 4 3 16 20.43 3.85 -5 -3 -16 12.94 4.19 5 3 16 12.35 3.36 -6 -3 -16 4.67 3.08 6 3 16 2.52 2.28 3 -4 -16 3.90 3.04 -3 4 16 6.13 3.54 2 -4 -16 -0.03 2.49 -2 4 16 0.35 2.19 1 -4 -16 6.36 3.37 -1 4 16 12.51 4.56 0 -4 -16 3.80 2.55 0 4 16 4.99 3.39 -1 -4 -16 4.76 2.79 1 4 16 6.28 3.23 -2 -4 -16 8.74 3.71 2 4 16 9.84 3.36 -3 -4 -16 26.88 5.47 3 4 16 22.94 5.06 3 4 16 24.22 4.26 -4 -4 -16 3.33 2.47 4 4 16 4.27 2.26 -5 -4 -16 0.85 1.92 5 4 16 2.68 2.12 -6 -4 -16 24.17 5.85 6 4 16 17.09 4.00 2 -5 -16 25.87 6.25 -2 5 16 31.98 6.81 1 -5 -16 1.24 2.31 -1 5 16 -1.43 2.25 0 -5 -16 13.44 4.02 0 5 16 17.76 4.98 -1 -5 -16 20.20 4.95 1 5 16 36.32 6.53 -2 -5 -16 1.29 2.10 2 5 16 3.74 2.35 -3 -5 -16 8.22 3.30 3 5 16 5.76 2.45 3 5 16 3.73 2.70 -4 -5 -16 35.50 6.47 4 5 16 34.65 5.17 -5 -5 -16 22.63 5.44 5 5 16 25.32 4.62 -6 -5 -16 2.69 2.52 1 -6 -16 89.21 11.01 -1 6 16 59.86 9.78 0 -6 -16 8.62 3.77 0 6 16 8.82 3.95 -1 -6 -16 31.24 6.12 1 6 16 28.26 6.08 -2 -6 -16 57.43 8.27 2 6 16 43.65 7.47 -3 -6 -16 27.42 5.93 3 6 16 23.15 4.15 3 6 16 30.80 6.05 -4 -6 -16 9.94 3.69 4 6 16 12.10 3.63 4 6 16 9.87 3.19 -5 -6 -16 9.94 3.98 5 6 16 12.10 3.50 0 -7 -16 25.07 5.67 0 7 16 30.41 6.68 -1 -7 -16 19.95 5.10 1 7 16 21.50 5.66 -2 -7 -16 7.05 3.31 2 7 16 6.83 3.60 -3 -7 -16 51.23 8.22 3 7 16 53.04 7.82 3 7 16 49.40 6.22 -4 -7 -16 13.68 4.35 4 7 16 21.06 4.73 4 7 16 19.72 3.90 -5 -7 -16 -0.04 2.17 5 7 16 -1.08 1.64 -1 -8 -16 21.22 5.31 -2 -8 -16 -0.67 2.09 2 8 16 3.40 3.06 -3 -8 -16 26.67 6.08 3 8 16 15.30 4.58 -4 -8 -16 7.95 3.66 -1 -2 17 1.93 2.69 0 -2 17 2.81 2.76 2 -2 17 13.48 3.37 2 1 -17 3.09 2.52 -2 -1 17 1.06 2.92 1 1 -17 20.03 4.70 -1 -1 17 23.83 5.76 0 1 -17 12.76 3.94 0 -1 17 14.13 4.64 -1 1 -17 -0.21 1.98 -2 1 -17 4.98 2.98 -3 1 -17 81.20 9.78 3 -1 17 75.49 8.13 2 0 -17 45.22 7.04 -2 0 17 49.46 8.46 1 0 -17 -0.83 1.97 -1 0 17 1.79 2.60 0 0 -17 16.86 4.48 0 0 17 16.01 4.71 -1 0 -17 24.47 5.26 1 0 17 26.20 5.78 -2 0 -17 12.85 3.86 -3 0 -17 16.48 4.37 3 0 17 10.71 3.02 -2 1 17 29.77 6.66 1 -1 -17 16.91 4.35 -1 1 17 11.08 4.38 0 -1 -17 4.48 2.85 0 1 17 11.02 3.97 -1 -1 -17 27.47 5.43 1 1 17 25.72 5.70 -2 -1 -17 22.47 4.96 -3 -1 -17 15.50 4.36 3 1 17 11.75 3.18 2 -2 -17 2.54 2.58 1 -2 -17 11.02 3.82 -1 2 17 12.22 4.37 0 -2 -17 1.51 2.37 0 2 17 0.99 2.49 -1 -2 -17 -2.47 1.63 1 2 17 -0.43 2.28 -2 -2 -17 -0.19 1.63 -3 -2 -17 19.87 4.80 3 2 17 23.15 3.98 -4 -2 -17 13.71 4.29 4 2 17 19.16 3.96 1 -3 -17 6.25 3.35 -1 3 17 2.97 2.84 0 -3 -17 4.46 3.19 0 3 17 5.34 3.26 -1 -3 -17 13.38 4.00 1 3 17 15.76 4.53 -2 -3 -17 29.90 5.85 2 3 17 31.83 6.21 -3 -3 -17 13.26 4.04 3 3 17 11.23 3.17 -4 -3 -17 2.50 2.68 4 3 17 5.03 2.51 0 -4 -17 59.04 8.53 0 4 17 40.58 7.68 -1 -4 -17 2.30 2.65 1 4 17 10.83 4.22 -2 -4 -17 24.40 5.64 2 4 17 23.80 5.48 -3 -4 -17 47.52 7.46 3 4 17 48.82 6.16 -4 -4 -17 10.66 3.91 -1 -5 -17 43.46 7.56 1 5 17 52.62 8.40 -2 -5 -17 10.25 4.10 2 5 17 12.81 4.35 -3 -5 -17 20.13 5.02 3 5 17 7.99 3.35 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 62723 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969303' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_4Prime _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 Eu N3 O7' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 869.90 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Eu Eu -0.1578 3.6682 '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 8.694(3) _cell_length_b 13.210(4) _cell_length_c 14.787(5) _cell_angle_alpha 100.236(6) _cell_angle_beta 97.994(6) _cell_angle_gamma 92.172(6) _cell_volume 1651.5(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23366 _cell_measurement_theta_min 4.719 _cell_measurement_theta_max 38.474 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.749 _exptl_crystal_F_000 864 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 2.198 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6784 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22940 _diffrn_reflns_av_unetI/netI 0.1154 _diffrn_reflns_av_R_equivalents 0.0897 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.415 _diffrn_reflns_theta_max 28.592 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8370 _reflns_number_gt 6060 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0335P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8370 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0820 _refine_ls_R_factor_gt 0.0516 _refine_ls_wR_factor_ref 0.1033 _refine_ls_wR_factor_gt 0.0907 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_restrained_S_all 0.974 _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 Eu1 Eu 0.06527(3) 0.01351(2) 0.20109(2) 0.01397(8) Uani 1 1 d . . . . . Cl1 Cl 0.29597(17) 0.61996(11) 0.57103(10) 0.0282(3) Uani 1 1 d . . . . . Cl3 Cl 0.70871(18) 0.52406(12) 0.24162(11) 0.0349(4) Uani 1 1 d . . . . . Cl2 Cl -0.2505(2) -0.59768(12) -0.14569(12) 0.0425(4) Uani 1 1 d . . . . . O3 O 0.0631(4) -0.1253(3) 0.0601(2) 0.0184(8) Uani 1 1 d . . . . . OW1 O -0.1366(4) 0.0586(3) 0.0909(2) 0.0165(8) Uani 1 1 d D . . . . O2 O 0.0376(4) 0.1987(3) 0.2564(2) 0.0190(8) Uani 1 1 d . . . . . O1 O 0.2125(4) 0.1264(3) 0.3445(2) 0.0179(8) Uani 1 1 d . . . . . O5 O 0.2358(4) 0.0946(3) 0.1265(2) 0.0194(8) Uani 1 1 d . . . . . O4 O -0.0926(4) -0.1522(3) 0.1601(2) 0.0183(8) Uani 1 1 d . . . . . N3 N -0.1591(5) 0.0387(3) 0.2985(3) 0.0145(9) Uani 1 1 d . . . . . O6 O 0.3527(4) 0.0812(3) -0.0015(2) 0.0228(9) Uani 1 1 d . . . . . N1 N 0.2972(5) -0.0966(3) 0.2287(3) 0.0160(9) Uani 1 1 d . . . . . N2 N 0.0721(5) -0.0864(3) 0.3395(3) 0.0149(9) Uani 1 1 d . . . . . C11 C -0.1706(6) -0.0113(4) 0.3700(4) 0.0162(11) Uani 1 1 d . . . . . C6 C 0.1816(6) -0.1541(4) 0.3507(3) 0.0150(11) Uani 1 1 d . . . . . C10 C -0.0490(6) -0.0848(4) 0.3872(3) 0.0152(11) Uani 1 1 d . . . . . C5 C 0.3128(6) -0.1526(4) 0.2975(3) 0.0145(11) Uani 1 1 d . . . . . C32 C 0.3772(6) 0.2951(4) 0.1894(3) 0.0171(11) Uani 1 1 d . . . . . H32 H 0.2862 0.2791 0.2118 0.020 Uiso 1 1 calc R U . . . C4 C 0.4448(6) -0.2079(4) 0.3133(3) 0.0179(11) Uani 1 1 d . . . . . H4 H 0.4548 -0.2457 0.3610 0.021 Uiso 1 1 calc R U . . . C13 C -0.4062(6) 0.0670(4) 0.3986(4) 0.0217(12) Uani 1 1 d . . . . . H13 H -0.4891 0.0761 0.4321 0.026 Uiso 1 1 calc R U . . . C16 C 0.1419(6) 0.2049(4) 0.3259(4) 0.0169(11) Uani 1 1 d . . . . . C31 C 0.4256(6) 0.2254(4) 0.1178(4) 0.0162(11) Uani 1 1 d . . . . . C8 C 0.0483(6) -0.2218(4) 0.4603(4) 0.0235(13) Uani 1 1 d . . . . . H8 H 0.0411 -0.2674 0.5010 0.028 Uiso 1 1 calc R U . . . C17 C 0.1835(6) 0.3073(4) 0.3867(4) 0.0167(11) Uani 1 1 d . . . . . C30 C 0.3312(6) 0.1261(4) 0.0774(4) 0.0172(11) Uani 1 1 d . . . . . C12 C -0.2924(6) 0.0037(4) 0.4222(4) 0.0203(12) Uani 1 1 d . . . . . H12 H -0.2962 -0.0291 0.4726 0.024 Uiso 1 1 calc R U . . . C1 C 0.4100(6) -0.0977(4) 0.1744(4) 0.0191(12) Uani 1 1 d . . . . . H1 H 0.3975 -0.0614 0.1257 0.023 Uiso 1 1 calc R U . . . C24 C -0.0932(6) -0.2842(4) 0.0268(4) 0.0193(12) Uani 1 1 d . . . . . C18 C 0.3065(6) 0.3226(4) 0.4579(4) 0.0207(12) Uani 1 1 d . . . . . H18 H 0.3667 0.2679 0.4679 0.025 Uiso 1 1 calc R U . . . C23 C -0.0378(6) -0.1813(4) 0.0852(4) 0.0158(11) Uani 1 1 d . . . . . C20 C 0.2518(6) 0.4995(4) 0.4980(4) 0.0224(12) Uani 1 1 d . . . . . C33 C 0.4614(6) 0.3877(4) 0.2277(4) 0.0212(12) Uani 1 1 d . . . . . H33 H 0.4278 0.4341 0.2749 0.025 Uiso 1 1 calc R U . . . C28 C -0.2547(6) -0.4423(4) -0.0005(4) 0.0268(13) Uani 1 1 d . . . . . H28 H -0.3315 -0.4833 0.0161 0.032 Uiso 1 1 calc R U . . . C3 C 0.5604(6) -0.2063(4) 0.2583(4) 0.0214(12) Uani 1 1 d . . . . . H3 H 0.6487 -0.2426 0.2688 0.026 Uiso 1 1 calc R U . . . C19 C 0.3427(6) 0.4182(4) 0.5152(4) 0.0245(13) Uani 1 1 d . . . . . H19 H 0.4253 0.4278 0.5637 0.029 Uiso 1 1 calc R U . . . C9 C -0.0635(6) -0.1515(4) 0.4498(4) 0.0207(12) Uani 1 1 d . . . . . H9 H -0.1465 -0.1485 0.4834 0.025 Uiso 1 1 calc R U . . . C22 C 0.0966(6) 0.3914(4) 0.3698(4) 0.0193(11) Uani 1 1 d . . . . . H22 H 0.0143 0.3823 0.3211 0.023 Uiso 1 1 calc R U . . . C14 C -0.3980(6) 0.1179(4) 0.3244(4) 0.0210(12) Uani 1 1 d . . . . . H14 H -0.4743 0.1611 0.3070 0.025 Uiso 1 1 calc R U . . . C26 C -0.0754(6) -0.4171(4) -0.1064(4) 0.0272(13) Uani 1 1 d . . . . . H26 H -0.0317 -0.4413 -0.1595 0.033 Uiso 1 1 calc R U . . . C36 C 0.5608(6) 0.2502(4) 0.0847(4) 0.0218(12) Uani 1 1 d . . . . . H36 H 0.5938 0.2045 0.0368 0.026 Uiso 1 1 calc R U . . . C15 C -0.2710(6) 0.1013(4) 0.2779(4) 0.0195(12) Uani 1 1 d . . . . . H15 H -0.2629 0.1359 0.2290 0.023 Uiso 1 1 calc R U . . . C29 C -0.2060(6) -0.3454(4) 0.0537(4) 0.0241(13) Uani 1 1 d . . . . . H29 H -0.2489 -0.3221 0.1072 0.029 Uiso 1 1 calc R U . . . C27 C -0.1880(7) -0.4762(4) -0.0782(4) 0.0255(13) Uani 1 1 d . . . . . C21 C 0.1331(6) 0.4879(4) 0.4256(4) 0.0216(12) Uani 1 1 d . . . . . H21 H 0.0772 0.5439 0.4137 0.026 Uiso 1 1 calc R U . . . C35 C 0.6484(6) 0.3425(4) 0.1218(4) 0.0261(13) Uani 1 1 d . . . . . H35 H 0.7387 0.3590 0.0991 0.031 Uiso 1 1 calc R U . . . C34 C 0.5973(6) 0.4090(4) 0.1935(4) 0.0240(13) Uani 1 1 d . . . . . C2 C 0.5441(6) -0.1508(4) 0.1879(4) 0.0187(12) Uani 1 1 d . . . . . H2 H 0.6207 -0.1486 0.1501 0.022 Uiso 1 1 calc R U . . . C7 C 0.1704(6) -0.2237(4) 0.4102(4) 0.0210(12) Uani 1 1 d . . . . . H7 H 0.2454 -0.2714 0.4161 0.025 Uiso 1 1 calc R U . . . C25 C -0.0294(6) -0.3201(4) -0.0529(4) 0.0214(12) Uani 1 1 d . . . . . H25 H 0.0453 -0.2787 -0.0709 0.026 Uiso 1 1 calc R U . . . H37 H -0.087(6) 0.089(4) 0.047(3) 0.032(17) Uiso 1 1 d D . . . . H38 H -0.216(7) 0.010(5) 0.052(5) 0.11(3) Uiso 1 1 d 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 Eu1 0.01349(13) 0.01547(14) 0.01328(13) 0.00326(10) 0.00250(9) 0.00034(9) Cl1 0.0336(8) 0.0204(7) 0.0273(8) 0.0002(6) -0.0012(6) 0.0018(6) Cl3 0.0411(9) 0.0261(8) 0.0358(9) 0.0022(7) 0.0078(7) -0.0111(7) Cl2 0.0524(11) 0.0214(8) 0.0433(10) -0.0058(7) -0.0125(8) -0.0007(7) O3 0.0161(19) 0.021(2) 0.0176(19) 0.0043(16) 0.0017(15) -0.0010(15) OW1 0.0138(19) 0.024(2) 0.0139(19) 0.0062(16) 0.0037(15) 0.0031(16) O2 0.0182(19) 0.019(2) 0.0180(19) 0.0023(16) -0.0009(15) 0.0016(16) O1 0.0207(19) 0.0146(19) 0.019(2) 0.0053(16) 0.0031(15) 0.0016(15) O5 0.0183(19) 0.022(2) 0.020(2) 0.0062(16) 0.0060(16) -0.0004(16) O4 0.0197(19) 0.0173(19) 0.018(2) 0.0028(16) 0.0043(16) 0.0003(15) N3 0.013(2) 0.014(2) 0.015(2) 0.0013(18) -0.0027(17) 0.0013(17) O6 0.026(2) 0.027(2) 0.016(2) 0.0044(17) 0.0060(16) -0.0061(17) N1 0.013(2) 0.017(2) 0.016(2) 0.0010(18) 0.0002(17) -0.0050(18) N2 0.014(2) 0.020(2) 0.011(2) 0.0016(18) 0.0014(17) 0.0009(18) C11 0.014(3) 0.012(3) 0.020(3) -0.003(2) -0.001(2) 0.004(2) C6 0.014(3) 0.019(3) 0.012(3) 0.001(2) 0.003(2) 0.001(2) C10 0.020(3) 0.012(3) 0.013(3) 0.000(2) 0.004(2) 0.000(2) C5 0.016(3) 0.016(3) 0.011(2) -0.001(2) 0.004(2) 0.001(2) C32 0.010(2) 0.027(3) 0.016(3) 0.010(2) 0.002(2) 0.001(2) C4 0.020(3) 0.019(3) 0.013(3) 0.002(2) 0.000(2) 0.001(2) C13 0.017(3) 0.024(3) 0.025(3) 0.001(2) 0.010(2) 0.002(2) C16 0.019(3) 0.019(3) 0.015(3) 0.003(2) 0.008(2) 0.002(2) C31 0.014(3) 0.020(3) 0.017(3) 0.010(2) 0.000(2) 0.004(2) C8 0.026(3) 0.024(3) 0.029(3) 0.016(3) 0.012(3) 0.008(2) C17 0.016(3) 0.018(3) 0.018(3) 0.004(2) 0.008(2) -0.003(2) C30 0.016(3) 0.013(3) 0.023(3) 0.008(2) -0.002(2) 0.003(2) C12 0.015(3) 0.026(3) 0.021(3) 0.004(2) 0.006(2) 0.004(2) C1 0.021(3) 0.018(3) 0.018(3) 0.002(2) 0.005(2) 0.001(2) C24 0.019(3) 0.020(3) 0.018(3) 0.004(2) -0.002(2) 0.004(2) C18 0.023(3) 0.016(3) 0.023(3) 0.006(2) -0.001(2) 0.000(2) C23 0.012(3) 0.021(3) 0.015(3) 0.007(2) -0.001(2) 0.003(2) C20 0.027(3) 0.019(3) 0.018(3) -0.001(2) -0.001(2) -0.001(2) C33 0.025(3) 0.018(3) 0.021(3) 0.002(2) 0.007(2) -0.001(2) C28 0.022(3) 0.025(3) 0.033(3) 0.007(3) 0.004(3) -0.007(2) C3 0.020(3) 0.019(3) 0.024(3) 0.004(2) -0.002(2) 0.006(2) C19 0.020(3) 0.024(3) 0.027(3) 0.001(3) 0.000(2) 0.004(2) C9 0.024(3) 0.022(3) 0.020(3) 0.007(2) 0.013(2) 0.001(2) C22 0.020(3) 0.022(3) 0.016(3) 0.006(2) 0.002(2) 0.002(2) C14 0.016(3) 0.019(3) 0.028(3) 0.006(2) 0.002(2) 0.005(2) C26 0.023(3) 0.029(3) 0.026(3) -0.003(3) 0.003(2) 0.003(3) C36 0.017(3) 0.022(3) 0.027(3) 0.004(2) 0.006(2) 0.000(2) C15 0.019(3) 0.020(3) 0.020(3) 0.004(2) 0.005(2) 0.000(2) C29 0.031(3) 0.016(3) 0.026(3) 0.003(2) 0.007(3) 0.001(2) C27 0.031(3) 0.014(3) 0.027(3) 0.001(2) -0.010(3) 0.004(2) C21 0.023(3) 0.020(3) 0.021(3) 0.006(2) 0.000(2) 0.003(2) C35 0.017(3) 0.027(3) 0.037(4) 0.008(3) 0.013(3) -0.002(2) C34 0.027(3) 0.023(3) 0.021(3) 0.007(2) -0.001(2) -0.009(2) C2 0.011(3) 0.015(3) 0.028(3) -0.001(2) 0.005(2) -0.001(2) C7 0.023(3) 0.021(3) 0.023(3) 0.010(2) 0.006(2) 0.007(2) C25 0.020(3) 0.024(3) 0.020(3) 0.004(2) 0.002(2) 0.002(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 Eu1 O5 2.305(3) . ? Eu1 OW1 2.392(3) . ? Eu1 O2 2.470(4) . ? Eu1 O4 2.472(3) . ? Eu1 O3 2.518(4) . ? Eu1 O1 2.517(3) . ? Eu1 N1 2.560(4) . ? Eu1 N3 2.579(4) . ? Eu1 N2 2.620(4) . ? Eu1 C16 2.849(5) . ? Eu1 C23 2.862(5) . ? Cl1 C20 1.753(5) . ? Cl3 C34 1.751(5) . ? Cl2 C27 1.755(6) . ? O3 C23 1.263(6) . ? OW1 H37 0.964(19) . ? OW1 H38 0.97(2) . ? O2 C16 1.261(6) . ? O1 C16 1.277(6) . ? O5 C30 1.280(6) . ? O4 C23 1.269(6) . ? N3 C15 1.339(6) . ? N3 C11 1.354(6) . ? O6 C30 1.254(6) . ? N1 C1 1.350(6) . ? N1 C5 1.355(6) . ? N2 C6 1.343(6) . ? N2 C10 1.346(6) . ? C11 C12 1.395(7) . ? C11 C10 1.489(7) . ? C6 C7 1.390(7) . ? C6 C5 1.475(7) . ? C10 C9 1.400(7) . ? C5 C4 1.398(7) . ? C32 C33 1.387(7) . ? C32 C31 1.397(7) . ? C32 H32 0.9300 . ? C4 C3 1.380(7) . ? C4 H4 0.9300 . ? C13 C12 1.368(7) . ? C13 C14 1.393(7) . ? C13 H13 0.9300 . ? C16 C17 1.486(7) . ? C31 C36 1.385(7) . ? C31 C30 1.501(7) . ? C8 C7 1.375(7) . ? C8 C9 1.382(7) . ? C8 H8 0.9300 . ? C17 C18 1.374(7) . ? C17 C22 1.405(7) . ? C12 H12 0.9300 . ? C1 C2 1.391(7) . ? C1 H1 0.9300 . ? C24 C25 1.387(7) . ? C24 C29 1.391(7) . ? C24 C23 1.498(7) . ? C18 C19 1.388(7) . ? C18 H18 0.9300 . ? C20 C21 1.362(7) . ? C20 C19 1.395(7) . ? C33 C34 1.386(7) . ? C33 H33 0.9300 . ? C28 C27 1.370(8) . ? C28 C29 1.400(7) . ? C28 H28 0.9300 . ? C3 C2 1.371(7) . ? C3 H3 0.9300 . ? C19 H19 0.9300 . ? C9 H9 0.9300 . ? C22 C21 1.389(7) . ? C22 H22 0.9300 . ? C14 C15 1.384(7) . ? C14 H14 0.9300 . ? C26 C27 1.384(8) . ? C26 C25 1.393(7) . ? C26 H26 0.9300 . ? C36 C35 1.394(7) . ? C36 H36 0.9300 . ? C15 H15 0.9300 . ? C29 H29 0.9300 . ? C21 H21 0.9300 . ? C35 C34 1.387(8) . ? C35 H35 0.9300 . ? C2 H2 0.9300 . ? C7 H7 0.9300 . ? C25 H25 0.9300 . ? 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 Eu1 OW1 86.21(12) . . ? O5 Eu1 O2 76.27(12) . . ? OW1 Eu1 O2 75.45(12) . . ? O5 Eu1 O4 133.61(12) . . ? OW1 Eu1 O4 80.77(12) . . ? O2 Eu1 O4 140.26(11) . . ? O5 Eu1 O3 81.31(12) . . ? OW1 Eu1 O3 76.62(12) . . ? O2 Eu1 O3 145.03(11) . . ? O4 Eu1 O3 52.40(11) . . ? O5 Eu1 O1 83.38(12) . . ? OW1 Eu1 O1 128.25(12) . . ? O2 Eu1 O1 52.82(11) . . ? O4 Eu1 O1 138.01(11) . . ? O3 Eu1 O1 149.69(11) . . ? O5 Eu1 N1 81.78(13) . . ? OW1 Eu1 N1 146.77(13) . . ? O2 Eu1 N1 130.33(12) . . ? O4 Eu1 N1 85.38(12) . . ? O3 Eu1 N1 71.02(12) . . ? O1 Eu1 N1 81.02(12) . . ? O5 Eu1 N3 144.98(13) . . ? OW1 Eu1 N3 78.84(12) . . ? O2 Eu1 N3 69.41(12) . . ? O4 Eu1 N3 75.10(12) . . ? O3 Eu1 N3 124.54(12) . . ? O1 Eu1 N3 81.50(12) . . ? N1 Eu1 N3 126.28(13) . . ? O5 Eu1 N2 139.17(12) . . ? OW1 Eu1 N2 134.62(12) . . ? O2 Eu1 N2 110.11(12) . . ? O4 Eu1 N2 66.79(12) . . ? O3 Eu1 N2 104.43(12) . . ? O1 Eu1 N2 71.63(12) . . ? N1 Eu1 N2 63.17(13) . . ? N3 Eu1 N2 63.13(13) . . ? O5 Eu1 C16 78.08(13) . . ? OW1 Eu1 C16 101.66(14) . . ? O2 Eu1 C16 26.21(13) . . ? O4 Eu1 C16 148.14(13) . . ? O3 Eu1 C16 159.39(13) . . ? O1 Eu1 C16 26.62(12) . . ? N1 Eu1 C16 105.92(14) . . ? N3 Eu1 C16 74.28(13) . . ? N2 Eu1 C16 91.43(14) . . ? O5 Eu1 C23 107.43(14) . . ? OW1 Eu1 C23 77.39(13) . . ? O2 Eu1 C23 152.28(13) . . ? O4 Eu1 C23 26.25(12) . . ? O3 Eu1 C23 26.16(12) . . ? O1 Eu1 C23 153.55(13) . . ? N1 Eu1 C23 76.91(13) . . ? N3 Eu1 C23 99.99(14) . . ? N2 Eu1 C23 85.40(14) . . ? C16 Eu1 C23 174.25(14) . . ? C23 O3 Eu1 92.3(3) . . ? Eu1 OW1 H37 107(3) . . ? Eu1 OW1 H38 124(5) . . ? H37 OW1 H38 104(6) . . ? C16 O2 Eu1 93.9(3) . . ? C16 O1 Eu1 91.4(3) . . ? C30 O5 Eu1 171.3(3) . . ? C23 O4 Eu1 94.3(3) . . ? C15 N3 C11 117.8(4) . . ? C15 N3 Eu1 120.0(3) . . ? C11 N3 Eu1 122.2(3) . . ? C1 N1 C5 118.5(4) . . ? C1 N1 Eu1 119.2(3) . . ? C5 N1 Eu1 122.3(3) . . ? C6 N2 C10 119.8(4) . . ? C6 N2 Eu1 119.2(3) . . ? C10 N2 Eu1 119.8(3) . . ? N3 C11 C12 121.4(5) . . ? N3 C11 C10 116.2(4) . . ? C12 C11 C10 122.4(5) . . ? N2 C6 C7 120.9(5) . . ? N2 C6 C5 117.9(4) . . ? C7 C6 C5 121.2(5) . . ? N2 C10 C9 121.6(5) . . ? N2 C10 C11 117.9(4) . . ? C9 C10 C11 120.5(5) . . ? N1 C5 C4 120.7(4) . . ? N1 C5 C6 116.2(4) . . ? C4 C5 C6 123.1(5) . . ? C33 C32 C31 121.6(5) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C3 C4 C5 120.0(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C12 C13 C14 120.1(5) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? O2 C16 O1 121.9(5) . . ? O2 C16 C17 118.4(5) . . ? O1 C16 C17 119.8(5) . . ? O2 C16 Eu1 59.9(3) . . ? O1 C16 Eu1 62.0(3) . . ? C17 C16 Eu1 176.9(4) . . ? C36 C31 C32 118.7(5) . . ? C36 C31 C30 121.0(5) . . ? C32 C31 C30 120.3(4) . . ? C7 C8 C9 119.4(5) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C18 C17 C22 119.0(5) . . ? C18 C17 C16 121.9(5) . . ? C22 C17 C16 119.1(5) . . ? O6 C30 O5 125.6(5) . . ? O6 C30 C31 117.2(4) . . ? O5 C30 C31 117.2(5) . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N1 C1 C2 123.0(5) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C25 C24 C29 119.7(5) . . ? C25 C24 C23 120.2(5) . . ? C29 C24 C23 120.1(5) . . ? C17 C18 C19 121.4(5) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? O3 C23 O4 121.0(5) . . ? O3 C23 C24 120.0(5) . . ? O4 C23 C24 119.1(4) . . ? O3 C23 Eu1 61.5(3) . . ? O4 C23 Eu1 59.5(3) . . ? C24 C23 Eu1 178.4(4) . . ? C21 C20 C19 121.9(5) . . ? C21 C20 Cl1 119.8(4) . . ? C19 C20 Cl1 118.3(4) . . ? C32 C33 C34 117.9(5) . . ? C32 C33 H33 121.1 . . ? C34 C33 H33 121.1 . . ? C27 C28 C29 119.4(5) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C2 C3 C4 119.5(5) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C18 C19 C20 118.2(5) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C8 C9 C10 118.5(5) . . ? C8 C9 H9 120.8 . . ? C10 C9 H9 120.8 . . ? C21 C22 C17 120.3(5) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C15 C14 C13 116.9(5) . . ? C15 C14 H14 121.5 . . ? C13 C14 H14 121.5 . . ? C27 C26 C25 117.9(5) . . ? C27 C26 H26 121.1 . . ? C25 C26 H26 121.1 . . ? C31 C36 C35 121.1(5) . . ? C31 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? N3 C15 C14 124.3(5) . . ? N3 C15 H15 117.8 . . ? C14 C15 H15 117.8 . . ? C24 C29 C28 119.5(5) . . ? C24 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C28 C27 C26 122.3(5) . . ? C28 C27 Cl2 118.9(5) . . ? C26 C27 Cl2 118.7(5) . . ? C20 C21 C22 119.2(5) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C34 C35 C36 118.3(5) . . ? C34 C35 H35 120.8 . . ? C36 C35 H35 120.8 . . ? C33 C34 C35 122.3(5) . . ? C33 C34 Cl3 119.2(4) . . ? C35 C34 Cl3 118.4(4) . . ? C3 C2 C1 118.4(5) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? C8 C7 C6 119.9(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C24 C25 C26 121.1(5) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? _refine_diff_density_max 1.250 _refine_diff_density_min -1.179 _refine_diff_density_rms 0.188 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.6936 13.2096 14.7872 100.236 97.994 92.172 ZERR 2.00 0.0029 0.0044 0.0049 0.006 0.006 0.006 LATT 1 SFAC C H N O CL EU UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 10 WGHT 0.033500 FVAR 0.12294 EU1 6 0.065272 0.013510 0.201085 11.00000 0.01349 0.01547 = 0.01328 0.00326 0.00250 0.00034 CL1 5 0.295969 0.619956 0.571027 11.00000 0.03359 0.02045 = 0.02729 0.00022 -0.00117 0.00176 CL3 5 0.708705 0.524059 0.241617 11.00000 0.04111 0.02612 = 0.03584 0.00221 0.00776 -0.01105 CL2 5 -0.250480 -0.597681 -0.145694 11.00000 0.05245 0.02138 = 0.04334 -0.00578 -0.01248 -0.00075 O3 4 0.063096 -0.125276 0.060059 11.00000 0.01606 0.02130 = 0.01758 0.00432 0.00171 -0.00103 OW1 4 -0.136625 0.058650 0.090873 11.00000 0.01381 0.02352 = 0.01387 0.00620 0.00371 0.00309 O2 4 0.037575 0.198724 0.256391 11.00000 0.01820 0.01936 = 0.01802 0.00231 -0.00092 0.00163 O1 4 0.212460 0.126423 0.344450 11.00000 0.02067 0.01458 = 0.01929 0.00531 0.00308 0.00164 O5 4 0.235815 0.094585 0.126514 11.00000 0.01826 0.02182 = 0.01967 0.00620 0.00599 -0.00044 O4 4 -0.092643 -0.152187 0.160095 11.00000 0.01972 0.01735 = 0.01807 0.00277 0.00427 0.00025 N3 3 -0.159126 0.038683 0.298511 11.00000 0.01342 0.01355 = 0.01462 0.00135 -0.00267 0.00128 O6 4 0.352685 0.081154 -0.001494 11.00000 0.02587 0.02705 = 0.01600 0.00444 0.00602 -0.00607 N1 3 0.297237 -0.096616 0.228690 11.00000 0.01269 0.01740 = 0.01613 0.00097 0.00018 -0.00500 N2 3 0.072132 -0.086442 0.339451 11.00000 0.01361 0.01956 = 0.01092 0.00157 0.00145 0.00086 C11 1 -0.170551 -0.011272 0.369968 11.00000 0.01392 0.01152 = 0.02016 -0.00305 -0.00084 0.00419 C6 1 0.181557 -0.154096 0.350678 11.00000 0.01418 0.01867 = 0.01165 0.00063 0.00300 0.00127 C10 1 -0.048952 -0.084817 0.387247 11.00000 0.01986 0.01165 = 0.01334 -0.00036 0.00377 0.00008 C5 1 0.312818 -0.152614 0.297462 11.00000 0.01608 0.01560 = 0.01132 -0.00051 0.00405 0.00084 C32 1 0.377167 0.295132 0.189353 11.00000 0.01016 0.02697 = 0.01638 0.01033 0.00195 0.00112 AFIX 43 H32 2 0.286244 0.279106 0.211788 11.00000 -1.20000 AFIX 0 C4 1 0.444810 -0.207872 0.313338 11.00000 0.02030 0.01912 = 0.01323 0.00249 -0.00039 0.00138 AFIX 43 H4 2 0.454756 -0.245679 0.360994 11.00000 -1.20000 AFIX 0 C13 1 -0.406184 0.067028 0.398556 11.00000 0.01683 0.02421 = 0.02479 0.00120 0.00959 0.00196 AFIX 43 H13 2 -0.489138 0.076117 0.432069 11.00000 -1.20000 AFIX 0 C16 1 0.141867 0.204949 0.325901 11.00000 0.01872 0.01855 = 0.01523 0.00336 0.00833 0.00174 C31 1 0.425562 0.225372 0.117820 11.00000 0.01395 0.01962 = 0.01717 0.00972 0.00040 0.00361 C8 1 0.048328 -0.221765 0.460322 11.00000 0.02561 0.02360 = 0.02865 0.01630 0.01246 0.00800 AFIX 43 H8 2 0.041083 -0.267387 0.500973 11.00000 -1.20000 AFIX 0 C17 1 0.183543 0.307327 0.386672 11.00000 0.01602 0.01780 = 0.01783 0.00410 0.00775 -0.00289 C30 1 0.331177 0.126145 0.077399 11.00000 0.01619 0.01303 = 0.02310 0.00832 -0.00162 0.00263 C12 1 -0.292382 0.003698 0.422171 11.00000 0.01492 0.02566 = 0.02131 0.00407 0.00584 0.00365 AFIX 43 H12 2 -0.296200 -0.029088 0.472583 11.00000 -1.20000 AFIX 0 C1 1 0.409997 -0.097722 0.174356 11.00000 0.02096 0.01832 = 0.01818 0.00154 0.00544 0.00101 AFIX 43 H1 2 0.397503 -0.061380 0.125699 11.00000 -1.20000 AFIX 0 C24 1 -0.093151 -0.284246 0.026848 11.00000 0.01902 0.01961 = 0.01807 0.00389 -0.00220 0.00378 C18 1 0.306508 0.322648 0.457865 11.00000 0.02265 0.01620 = 0.02285 0.00593 -0.00060 -0.00035 AFIX 43 H18 2 0.366727 0.267864 0.467869 11.00000 -1.20000 AFIX 0 C23 1 -0.037790 -0.181307 0.085203 11.00000 0.01169 0.02098 = 0.01503 0.00662 -0.00137 0.00265 C20 1 0.251843 0.499475 0.497962 11.00000 0.02656 0.01949 = 0.01808 -0.00089 -0.00063 -0.00124 C33 1 0.461442 0.387738 0.227740 11.00000 0.02504 0.01804 = 0.02057 0.00199 0.00667 -0.00077 AFIX 43 H33 2 0.427849 0.434067 0.274913 11.00000 -1.20000 AFIX 0 C28 1 -0.254657 -0.442326 -0.000485 11.00000 0.02201 0.02476 = 0.03331 0.00699 0.00376 -0.00715 AFIX 43 H28 2 -0.331458 -0.483346 0.016101 11.00000 -1.20000 AFIX 0 C3 1 0.560382 -0.206300 0.258253 11.00000 0.02003 0.01878 = 0.02441 0.00445 -0.00210 0.00557 AFIX 43 H3 2 0.648657 -0.242634 0.268811 11.00000 -1.20000 AFIX 0 C19 1 0.342714 0.418189 0.515158 11.00000 0.02046 0.02364 = 0.02728 0.00095 0.00002 0.00416 AFIX 43 H19 2 0.425332 0.427792 0.563720 11.00000 -1.20000 AFIX 0 C9 1 -0.063492 -0.151461 0.449773 11.00000 0.02418 0.02181 = 0.01996 0.00716 0.01283 0.00096 AFIX 43 H9 2 -0.146479 -0.148494 0.483434 11.00000 -1.20000 AFIX 0 C22 1 0.096615 0.391381 0.369839 11.00000 0.02048 0.02171 = 0.01643 0.00613 0.00200 0.00164 AFIX 43 H22 2 0.014280 0.382338 0.321132 11.00000 -1.20000 AFIX 0 C14 1 -0.397997 0.117909 0.324402 11.00000 0.01621 0.01936 = 0.02826 0.00635 0.00244 0.00549 AFIX 43 H14 2 -0.474310 0.161056 0.306951 11.00000 -1.20000 AFIX 0 C26 1 -0.075360 -0.417079 -0.106446 11.00000 0.02312 0.02905 = 0.02643 -0.00269 0.00281 0.00259 AFIX 43 H26 2 -0.031716 -0.441339 -0.159505 11.00000 -1.20000 AFIX 0 C36 1 0.560810 0.250218 0.084668 11.00000 0.01687 0.02247 = 0.02652 0.00373 0.00645 0.00012 AFIX 43 H36 2 0.593751 0.204534 0.036798 11.00000 -1.20000 AFIX 0 C15 1 -0.271035 0.101300 0.277870 11.00000 0.01897 0.02012 = 0.02020 0.00404 0.00550 -0.00010 AFIX 43 H15 2 -0.262939 0.135934 0.229034 11.00000 -1.20000 AFIX 0 C29 1 -0.206029 -0.345436 0.053684 11.00000 0.03074 0.01623 = 0.02598 0.00322 0.00711 0.00079 AFIX 43 H29 2 -0.248867 -0.322115 0.107245 11.00000 -1.20000 AFIX 0 C27 1 -0.188042 -0.476176 -0.078185 11.00000 0.03100 0.01354 = 0.02680 0.00054 -0.01010 0.00355 C21 1 0.133126 0.487887 0.425619 11.00000 0.02325 0.02039 = 0.02127 0.00621 0.00006 0.00270 AFIX 43 H21 2 0.077202 0.543919 0.413726 11.00000 -1.20000 AFIX 0 C35 1 0.648366 0.342482 0.121802 11.00000 0.01741 0.02707 = 0.03693 0.00760 0.01310 -0.00214 AFIX 43 H35 2 0.738749 0.359034 0.099061 11.00000 -1.20000 AFIX 0 C34 1 0.597304 0.408997 0.193531 11.00000 0.02707 0.02262 = 0.02142 0.00716 -0.00054 -0.00908 C2 1 0.544061 -0.150770 0.187854 11.00000 0.01130 0.01529 = 0.02831 -0.00081 0.00501 -0.00096 AFIX 43 H2 2 0.620704 -0.148615 0.150060 11.00000 -1.20000 AFIX 0 C7 1 0.170417 -0.223674 0.410182 11.00000 0.02274 0.02086 = 0.02256 0.00967 0.00580 0.00740 AFIX 43 H7 2 0.245381 -0.271416 0.416068 11.00000 -1.20000 AFIX 0 C25 1 -0.029396 -0.320098 -0.052883 11.00000 0.01963 0.02407 = 0.02043 0.00427 0.00224 0.00237 AFIX 43 H25 2 0.045309 -0.278677 -0.070882 11.00000 -1.20000 AFIX 0 H37 2 -0.086680 0.088998 0.046963 11.00000 0.03213 H38 2 -0.216088 0.009528 0.052155 11.00000 0.11088 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0516 for 6060 Fo > 4sig(Fo) and 0.0820 for all 8370 data REM 459 parameters refined using 2 restraints END WGHT 0.0330 0.0000 REM Highest difference peak 1.250, deepest hole -1.179, 1-sigma level 0.188 Q1 1 -0.1986 -0.0427 0.3984 11.00000 0.05 1.25 Q2 1 0.4000 0.6230 0.5513 11.00000 0.05 0.87 Q3 1 -0.4086 -0.4409 -0.0326 11.00000 0.05 0.82 Q4 1 -0.0534 -0.0643 0.1893 11.00000 0.05 0.76 Q5 1 0.4201 0.4993 0.1584 11.00000 0.05 0.75 Q6 1 -0.2772 0.1559 0.4433 11.00000 0.05 0.73 Q7 1 -0.2690 -0.0487 0.4555 11.00000 0.05 0.71 Q8 1 0.0798 -0.1803 0.2770 11.00000 0.05 0.70 Q9 1 0.1513 0.2405 0.2429 11.00000 0.05 0.69 Q10 1 0.3465 0.1959 0.0926 11.00000 0.05 0.68 ; _shelx_res_checksum 60979 _shelx_hkl_file ; -1 0 0 285.43 8.60 -1 0 0 260.76 8.05 -1 0 0 271.89 7.64 1 0 0 270.35 7.64 1 0 0 296.70 7.81 -2 0 0 1.53 1.33 -2 0 0 -0.43 0.98 2 0 0 1.27 0.90 2 0 0 -0.66 0.83 -3 0 0 77.79 4.25 -3 0 0 85.12 5.22 3 0 0 84.11 4.27 3 0 0 93.20 3.92 -4 0 0 -1.36 1.19 -4 0 0 0.77 1.81 4 0 0 0.35 1.18 4 0 0 0.69 1.09 -5 0 0 46.68 4.49 -5 0 0 63.79 6.52 5 0 0 48.50 3.36 5 0 0 62.87 4.45 -6 0 0 103.43 9.36 -6 0 0 119.99 6.78 6 0 0 104.97 5.31 6 0 0 101.34 6.46 -7 0 0 29.26 5.55 -7 0 0 25.93 4.10 7 0 0 32.84 4.72 -8 0 0 140.50 8.33 -8 0 0 114.48 11.62 8 0 0 125.03 8.43 -9 0 0 53.06 8.78 9 0 0 63.12 7.30 -10 0 0 10.21 5.42 10 0 0 16.93 4.61 -11 0 0 0.32 4.51 11 0 0 4.28 3.47 11 -1 0 -0.43 3.04 -11 1 0 1.81 4.63 10 -1 0 10.19 3.81 -10 1 0 13.42 5.57 9 -1 0 23.14 4.71 -9 1 0 29.35 6.97 8 -1 0 118.42 7.90 -8 1 0 128.52 12.23 7 -1 0 57.89 5.90 7 -1 0 68.10 5.47 -7 1 0 75.14 8.75 -7 1 0 60.53 5.73 6 -1 0 13.08 2.45 6 -1 0 11.89 2.73 -6 1 0 16.15 2.78 -6 1 0 9.14 3.43 5 -1 0 1.33 1.30 5 -1 0 0.02 1.16 -5 1 0 1.09 2.00 -5 1 0 -0.39 1.29 4 -1 0 17.47 2.54 4 -1 0 15.03 2.30 -4 1 0 13.54 3.28 -4 1 0 13.73 2.22 3 -1 0 47.22 3.12 3 -1 0 42.49 2.98 -3 1 0 46.30 4.61 -3 1 0 49.26 3.00 2 -1 0 541.50 15.23 2 -1 0 552.81 15.70 -2 1 0 528.35 17.12 -2 1 0 545.58 15.42 1 -1 0 362.63 10.62 1 -1 0 356.34 10.17 1 -1 0 374.74 10.05 -1 1 0 366.01 10.18 -1 1 0 391.88 11.50 0 -1 0 358.99 9.72 0 -1 0 354.65 10.00 0 1 0 342.70 10.25 0 1 0 360.69 9.38 -1 -1 0 218.08 7.23 1 1 0 218.09 6.56 1 1 0 223.62 7.06 -2 -1 0 122.69 3.61 -2 -1 0 122.65 5.26 2 1 0 109.28 4.63 2 1 0 116.75 3.63 -3 -1 0 24.03 2.88 3 1 0 21.02 1.63 3 1 0 20.25 2.43 -4 -1 0 46.79 5.21 -4 -1 0 54.58 4.71 4 1 0 50.92 2.67 4 1 0 50.34 4.25 -5 -1 0 13.34 3.29 -5 -1 0 12.19 2.73 5 1 0 9.76 1.59 5 1 0 10.59 2.50 -6 -1 0 79.34 8.26 -6 -1 0 83.71 5.95 6 1 0 79.54 5.70 6 1 0 92.66 4.42 -7 -1 0 90.57 9.52 -7 -1 0 107.93 7.25 7 1 0 90.68 7.69 -8 -1 0 31.13 6.39 -8 -1 0 37.08 5.43 8 1 0 40.76 5.63 -9 -1 0 50.62 8.52 9 1 0 53.96 6.94 -10 -1 0 31.59 7.52 10 1 0 23.17 4.92 -11 -1 0 4.28 5.18 11 1 0 7.28 3.90 11 -2 0 8.56 3.91 -11 2 0 -1.20 4.33 10 -2 0 5.09 3.25 -10 2 0 -0.78 3.61 9 -2 0 22.60 4.54 -9 2 0 28.06 6.56 8 -2 0 44.97 5.55 -8 2 0 43.38 7.33 7 -2 0 43.03 4.71 7 -2 0 30.39 4.26 -7 2 0 38.41 4.28 -7 2 0 42.12 6.70 6 -2 0 32.55 4.03 6 -2 0 30.56 3.74 -6 2 0 32.57 5.54 -6 2 0 23.87 3.20 5 -2 0 18.49 2.83 5 -2 0 22.96 3.09 -5 2 0 17.69 2.45 -5 2 0 19.57 4.22 4 -2 0 12.80 2.43 4 -2 0 10.05 1.94 -4 2 0 12.72 1.89 -4 2 0 11.24 3.05 3 -2 0 2.61 1.26 3 -2 0 1.41 1.46 -3 2 0 2.49 1.91 -3 2 0 2.52 1.09 2 -2 0 28.70 2.74 2 -2 0 30.87 2.37 -2 2 0 23.43 3.21 -2 2 0 27.23 1.71 1 -2 0 156.74 4.95 1 -2 0 149.21 5.73 -1 2 0 167.29 6.35 -1 2 0 159.49 5.02 0 -2 0 312.03 9.37 0 -2 0 331.55 9.79 0 2 0 316.15 9.03 0 2 0 320.63 10.17 -1 -2 0 148.15 5.89 -1 -2 0 143.31 4.45 1 2 0 156.78 5.21 1 2 0 148.22 4.50 -2 -2 0 8.87 2.02 2 2 0 7.56 1.62 2 2 0 8.87 1.84 -3 -2 0 54.61 4.17 3 2 0 59.53 3.75 3 2 0 52.68 3.81 -4 -2 0 7.51 2.20 4 2 0 10.77 1.01 4 2 0 10.84 2.33 4 2 0 10.47 2.41 -5 -2 0 106.68 6.78 -5 -2 0 130.37 7.87 5 2 0 118.36 6.58 5 2 0 124.94 4.29 -6 -2 0 69.65 7.64 -6 -2 0 80.99 5.99 6 2 0 69.84 6.27 -7 -2 0 31.43 5.68 -7 -2 0 38.67 5.35 7 2 0 40.33 5.03 -8 -2 0 12.21 3.53 -8 -2 0 12.69 4.58 8 2 0 6.62 2.92 -9 -2 0 74.49 8.18 -9 -2 0 79.23 10.21 9 2 0 61.74 7.55 -10 -2 0 3.40 4.58 10 2 0 8.63 4.03 -11 -2 0 0.04 4.51 11 2 0 0.56 2.98 11 -3 0 6.15 3.74 -11 3 0 -1.52 4.10 10 -3 0 7.27 3.41 -10 3 0 7.07 4.84 9 -3 0 29.22 5.15 -9 3 0 27.49 6.49 8 -3 0 96.53 8.24 8 -3 0 108.15 7.22 -8 3 0 113.28 11.69 7 -3 0 25.12 3.95 7 -3 0 11.01 2.96 -7 3 0 17.66 4.95 6 -3 0 3.05 1.96 6 -3 0 3.71 1.77 -6 3 0 0.12 2.23 -6 3 0 3.93 1.63 5 -3 0 8.31 2.43 5 -3 0 0.28 1.42 -5 3 0 3.15 1.33 -5 3 0 3.73 2.33 4 -3 0 0.99 1.26 4 -3 0 -0.70 1.36 -4 3 0 0.72 1.98 -4 3 0 0.19 0.95 3 -3 0 35.80 3.06 3 -3 0 36.10 3.70 -3 3 0 32.61 4.26 -3 3 0 36.70 2.18 2 -3 0 75.85 4.46 2 -3 0 78.37 3.64 -2 3 0 86.42 5.36 -2 3 0 81.99 3.24 1 -3 0 40.48 2.43 1 -3 0 38.74 2.11 1 -3 0 39.43 3.14 -1 3 0 43.16 3.79 0 -3 0 16.34 2.11 0 -3 0 16.15 1.86 0 3 0 12.04 1.70 0 3 0 10.84 2.10 -1 -3 0 164.91 5.36 -1 -3 0 169.11 6.90 1 3 0 157.17 5.89 1 3 0 160.63 6.64 -2 -3 0 1.17 0.62 -2 -3 0 1.52 1.67 2 3 0 1.05 0.65 2 3 0 1.77 1.29 2 3 0 2.44 1.53 -3 -3 0 3.54 1.89 3 3 0 4.48 1.67 3 3 0 4.20 1.63 -4 -3 0 20.75 3.62 4 3 0 17.21 2.97 4 3 0 17.18 2.79 -5 -3 0 26.41 4.04 5 3 0 30.61 3.94 5 3 0 25.04 3.83 -6 -3 0 43.36 5.44 -6 -3 0 46.28 6.22 6 3 0 50.22 5.30 -7 -3 0 96.56 8.65 -7 -3 0 117.29 10.50 7 3 0 102.27 7.29 -8 -3 0 -1.66 2.15 -8 -3 0 2.55 3.32 8 3 0 1.41 2.19 -9 -3 0 30.40 5.70 -9 -3 0 29.17 6.76 9 3 0 32.61 5.69 -10 -3 0 -1.56 4.10 10 3 0 -2.03 2.34 -11 -3 0 2.38 4.70 11 3 0 0.52 3.29 11 -4 0 -1.40 2.63 -11 4 0 4.29 5.30 10 -4 0 23.03 4.97 -10 4 0 22.88 6.82 9 -4 0 47.41 6.22 -9 4 0 45.24 8.29 8 -4 0 52.02 6.03 8 -4 0 58.57 6.44 -8 4 0 60.98 9.11 7 -4 0 8.92 3.03 7 -4 0 2.72 2.01 -7 4 0 2.81 3.37 6 -4 0 0.42 1.61 6 -4 0 0.41 1.45 -6 4 0 -0.33 1.22 -6 4 0 3.14 3.08 5 -4 0 -1.74 1.03 5 -4 0 -1.29 1.47 -5 4 0 -0.39 2.08 -5 4 0 0.39 1.08 4 -4 0 0.24 1.08 4 -4 0 2.70 1.88 -4 4 0 -0.57 2.14 -4 4 0 1.76 0.96 3 -4 0 23.29 2.52 3 -4 0 21.09 3.07 -3 4 0 21.07 3.78 -3 4 0 24.52 1.83 2 -4 0 117.89 4.88 2 -4 0 126.97 6.07 -2 4 0 129.30 4.86 -2 4 0 126.38 6.81 1 -4 0 126.28 5.31 1 -4 0 126.75 5.89 -1 4 0 132.74 6.69 -1 4 0 142.01 5.51 0 -4 0 0.09 1.41 0 -4 0 2.60 1.35 0 4 0 1.31 1.65 0 4 0 0.27 1.29 -1 -4 0 138.94 5.19 -1 -4 0 143.62 6.62 1 4 0 130.87 6.38 1 4 0 136.14 5.52 -2 -4 0 88.55 5.56 -2 -4 0 88.18 3.36 2 4 0 70.98 4.25 2 4 0 88.64 5.20 -3 -4 0 0.43 1.69 3 4 0 2.00 1.54 3 4 0 2.16 1.46 -4 -4 0 12.59 2.99 4 4 0 17.11 2.96 4 4 0 18.86 3.30 -5 -4 0 21.41 4.15 5 4 0 18.06 3.29 5 4 0 22.49 3.70 -6 -4 0 68.36 7.16 6 4 0 63.72 6.10 6 4 0 70.22 6.88 -7 -4 0 21.64 4.52 -7 -4 0 8.42 3.63 7 4 0 20.29 3.89 -8 -4 0 13.27 4.20 -8 -4 0 15.55 4.84 8 4 0 23.81 4.59 -9 -4 0 12.19 4.37 -9 -4 0 29.32 6.68 9 4 0 19.87 4.57 -10 -4 0 -1.24 3.92 -10 -4 0 7.47 4.34 10 4 0 -2.34 2.50 -11 -4 0 -3.99 4.22 11 4 0 -1.14 3.55 11 -5 0 3.19 3.34 -11 5 0 3.97 5.16 10 -5 0 46.95 6.64 -10 5 0 40.86 8.80 9 -5 0 32.42 5.53 9 -5 0 37.63 5.47 -9 5 0 36.60 7.39 8 -5 0 54.51 6.00 8 -5 0 36.37 5.56 -8 5 0 40.96 7.53 7 -5 0 11.25 2.82 7 -5 0 12.76 3.54 -7 5 0 13.52 4.59 6 -5 0 14.33 3.54 6 -5 0 14.90 2.83 -6 5 0 18.81 4.78 5 -5 0 3.54 2.13 5 -5 0 3.63 1.72 -5 5 0 4.82 2.98 -5 5 0 4.30 1.33 4 -5 0 80.31 5.67 4 -5 0 72.76 4.43 -4 5 0 79.74 7.76 -4 5 0 77.77 3.62 3 -5 0 -0.55 0.99 3 -5 0 1.53 1.76 -3 5 0 -0.33 0.94 -3 5 0 3.25 2.31 2 -5 0 77.77 3.92 2 -5 0 79.81 5.09 2 -5 0 75.36 3.79 -2 5 0 72.08 5.58 1 -5 0 161.21 6.80 1 -5 0 171.11 7.34 -1 5 0 169.77 6.61 -1 5 0 166.77 8.20 0 -5 0 98.89 5.35 0 -5 0 92.00 4.79 0 5 0 86.53 4.43 0 5 0 88.59 5.70 -1 -5 0 30.90 2.78 -1 -5 0 33.69 3.84 1 5 0 28.87 2.95 1 5 0 33.26 3.87 -2 -5 0 171.38 5.95 -2 -5 0 165.83 8.39 2 5 0 169.22 8.03 2 5 0 161.86 6.99 -3 -5 0 1.54 0.76 -3 -5 0 2.42 1.94 3 5 0 2.71 1.82 3 5 0 -1.43 1.21 -4 -5 0 53.55 6.07 4 5 0 57.39 5.64 4 5 0 54.71 5.06 -5 -5 0 30.58 5.00 5 5 0 38.40 4.51 5 5 0 36.33 4.76 -6 -5 0 50.55 6.46 6 5 0 41.83 5.06 6 5 0 55.65 6.19 -7 -5 0 20.00 4.67 7 5 0 26.89 4.66 -8 -5 0 50.26 7.80 -8 -5 0 44.58 6.88 8 5 0 46.29 6.30 -9 -5 0 10.40 4.54 -9 -5 0 -0.85 3.15 9 5 0 0.71 2.66 -10 -5 0 0.03 3.87 -10 -5 0 -3.03 3.27 10 5 0 -3.75 2.36 11 -6 0 11.29 4.36 -11 6 0 11.43 6.52 10 -6 0 16.71 4.28 -10 6 0 4.45 5.05 9 -6 0 40.74 6.27 9 -6 0 33.55 5.43 -9 6 0 33.53 7.77 8 -6 0 56.47 6.19 8 -6 0 47.51 6.28 -8 6 0 48.39 8.21 7 -6 0 22.37 4.45 7 -6 0 21.37 3.74 -7 6 0 3.49 3.40 6 -6 0 11.96 2.72 6 -6 0 5.92 2.69 -6 6 0 10.88 4.40 5 -6 0 1.16 1.48 5 -6 0 -0.82 1.77 -5 6 0 -0.23 2.39 4 -6 0 10.33 2.75 4 -6 0 14.27 2.32 -4 6 0 14.09 1.93 -4 6 0 21.30 4.30 3 -6 0 116.77 5.17 3 -6 0 115.99 6.81 3 -6 0 124.78 5.62 -3 6 0 120.99 8.07 2 -6 0 74.30 4.27 2 -6 0 82.78 5.42 -2 6 0 80.82 4.79 -2 6 0 85.58 6.25 1 -6 0 32.89 3.73 1 -6 0 25.57 3.15 -1 6 0 31.25 3.20 -1 6 0 31.89 4.55 0 -6 0 50.46 3.78 0 -6 0 52.48 4.79 0 6 0 59.61 5.71 0 6 0 52.89 3.59 -1 -6 0 359.26 13.89 -1 -6 0 364.08 12.03 1 6 0 363.60 12.08 1 6 0 375.61 14.20 -2 -6 0 1.28 2.13 -2 -6 0 -0.05 1.05 2 6 0 2.15 1.96 2 6 0 0.66 1.34 -3 -6 0 54.37 2.85 -3 -6 0 52.53 5.77 3 6 0 53.34 5.55 3 6 0 51.80 4.67 -4 -6 0 9.88 3.18 4 6 0 14.73 2.96 4 6 0 14.35 3.26 -5 -6 0 82.01 8.33 5 6 0 65.65 6.80 5 6 0 80.97 5.78 -6 -6 0 43.13 6.38 6 6 0 24.26 4.13 6 6 0 25.81 4.62 -7 -6 0 46.52 6.91 7 6 0 46.31 5.94 7 6 0 33.60 5.68 -8 -6 0 29.90 6.40 -8 -6 0 34.74 6.15 8 6 0 29.87 5.25 -9 -6 0 9.40 4.30 -9 -6 0 6.01 4.33 9 6 0 13.11 4.16 -10 -6 0 -3.61 3.23 -10 -6 0 0.18 3.70 10 6 0 0.31 3.06 10 -7 0 15.01 4.17 -10 7 0 7.17 5.59 9 -7 0 52.21 6.51 9 -7 0 39.98 6.41 -9 7 0 40.58 8.79 8 -7 0 5.48 3.07 8 -7 0 1.52 2.17 -8 7 0 2.58 4.05 7 -7 0 33.26 5.42 7 -7 0 48.81 5.39 -7 7 0 40.77 7.60 6 -7 0 17.76 3.20 6 -7 0 19.01 4.20 -6 7 0 25.84 5.64 5 -7 0 24.95 4.36 5 -7 0 29.41 3.62 -5 7 0 24.30 5.40 4 -7 0 59.67 6.23 4 -7 0 64.29 4.25 4 -7 0 60.62 3.53 -4 7 0 57.11 7.25 3 -7 0 38.18 3.41 3 -7 0 27.14 4.07 -3 7 0 38.61 5.73 2 -7 0 63.16 4.09 2 -7 0 57.84 5.41 -2 7 0 62.07 4.36 -2 7 0 59.14 6.45 1 -7 0 355.77 13.05 1 -7 0 352.70 13.12 -1 7 0 340.76 12.01 -1 7 0 350.20 14.93 0 -7 0 38.99 3.96 0 -7 0 45.75 4.64 0 7 0 44.48 5.41 0 7 0 36.23 3.64 -1 -7 0 4.42 1.69 -1 -7 0 4.00 2.09 1 7 0 1.45 1.52 1 7 0 0.15 1.70 -2 -7 0 8.00 1.86 -2 -7 0 12.96 3.16 2 7 0 10.62 2.34 2 7 0 8.24 2.68 -3 -7 0 1.34 1.99 -3 -7 0 1.03 1.08 3 7 0 -0.87 1.76 3 7 0 -1.82 1.27 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0 48.58 5.51 3 -10 0 57.32 5.34 3 -10 0 58.13 6.65 -3 10 0 57.44 7.90 -3 10 0 57.32 5.61 2 -10 0 25.89 3.90 2 -10 0 29.93 4.66 -2 10 0 18.47 4.79 -2 10 0 25.17 3.73 1 -10 0 62.41 6.40 1 -10 0 54.93 5.85 -1 10 0 54.77 7.21 -1 10 0 64.16 5.44 0 -10 0 125.04 8.17 0 -10 0 138.19 7.75 0 10 0 127.23 7.02 0 10 0 145.37 9.81 -1 -10 0 2.27 2.47 -1 -10 0 6.03 2.43 1 10 0 5.83 2.25 1 10 0 8.65 3.45 -2 -10 0 1.13 1.80 -2 -10 0 5.10 2.91 2 10 0 -4.28 1.83 2 10 0 0.47 1.73 -3 -10 0 -1.09 2.66 3 10 0 1.58 2.51 3 10 0 4.40 2.48 -4 -10 0 10.67 3.85 4 10 0 8.64 2.96 4 10 0 7.77 3.36 -5 -10 0 31.55 6.33 5 10 0 40.28 6.45 5 10 0 36.76 5.24 -6 -10 0 57.24 8.55 6 10 0 54.20 6.54 6 10 0 49.23 7.07 -7 -10 0 17.93 5.51 7 10 0 19.67 5.05 7 10 0 16.75 4.23 -8 -10 0 6.34 4.28 8 10 0 0.54 3.47 8 10 0 2.63 3.21 -9 -10 0 0.36 3.65 9 10 0 0.56 3.30 9 -11 0 23.20 5.82 -9 11 0 18.36 7.22 8 -11 0 10.52 4.37 -8 11 0 12.07 5.98 7 -11 0 -2.50 2.89 -7 11 0 0.65 4.20 6 -11 0 -1.03 2.15 -6 11 0 0.72 3.54 5 -11 0 -2.47 2.05 -5 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5.92 1 3 -19 1.88 4.40 -1 -3 19 5.75 4.53 0 3 -19 4.86 4.76 0 -3 19 -1.86 3.32 -1 3 -19 6.69 4.97 1 -3 19 9.34 4.83 3 2 -19 9.03 5.04 -3 -2 19 17.34 5.94 2 2 -19 4.82 4.28 -2 -2 19 -1.91 3.33 1 2 -19 1.29 4.17 -1 -2 19 -1.11 3.14 0 2 -19 -4.20 4.12 0 -2 19 -0.27 3.62 -1 2 -19 10.20 5.50 1 -2 19 1.58 4.20 4 1 -19 20.97 6.38 -4 -1 19 23.99 6.42 2 1 -19 13.70 5.59 -2 -1 19 8.57 4.86 1 1 -19 -0.62 3.94 -1 -1 19 -1.26 3.35 0 1 -19 1.46 3.90 0 -1 19 5.90 4.82 -1 1 -19 -1.14 3.92 1 -1 19 6.12 4.29 4 0 -19 38.21 7.94 -4 0 19 35.25 7.36 3 0 -19 2.40 3.95 -3 0 19 2.16 4.17 2 0 -19 -0.65 4.34 -2 0 19 0.00 3.92 1 0 -19 1.47 4.34 -1 0 19 0.67 3.83 -1 0 19 1.02 4.00 0 0 -19 0.03 4.07 0 0 19 2.00 3.46 -1 0 -19 10.49 5.57 1 0 19 25.76 6.49 3 -1 -19 -1.31 3.68 -3 1 19 1.87 4.11 2 -1 -19 3.79 4.20 -2 1 19 -1.50 3.82 1 -1 -19 0.14 4.10 -1 1 19 4.80 4.23 0 -1 -19 0.09 4.06 0 1 19 -4.34 3.20 0 1 19 -1.92 3.70 -2 2 19 0.37 4.40 1 -2 -19 7.34 5.10 -1 2 19 5.66 4.48 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 80978 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969304' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_5 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 Gd N3 O7' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 875.19 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Gd Gd -0.1653 3.9035 '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 8.6934(9) _cell_length_b 13.1762(13) _cell_length_c 14.7709(15) _cell_angle_alpha 100.2350(10) _cell_angle_beta 97.9400(10) _cell_angle_gamma 92.1760(10) _cell_volume 1645.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23549 _cell_measurement_theta_min 4.741 _cell_measurement_theta_max 51.081 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_F_000 866 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.07 _exptl_absorpt_coefficient_mu 2.315 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6180 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23549 _diffrn_reflns_av_unetI/netI 0.0727 _diffrn_reflns_av_R_equivalents 0.0541 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.416 _diffrn_reflns_theta_max 30.062 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.916 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.916 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.916 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8862 _reflns_number_gt 7210 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0323P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8862 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0556 _refine_ls_R_factor_gt 0.0387 _refine_ls_wR_factor_ref 0.0812 _refine_ls_wR_factor_gt 0.0751 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Gd1 Gd 0.43552(2) 0.48669(2) 0.79874(2) 0.01133(5) Uani 1 1 d . . . . . Cl2 Cl 0.75016(14) 1.09822(8) 1.14541(8) 0.0395(3) Uani 1 1 d . . . . . Cl3 Cl -0.20838(13) -0.02460(8) 0.75796(8) 0.0326(2) Uani 1 1 d . . . . . Cl1 Cl 0.20389(12) -0.12005(8) 0.42909(7) 0.0268(2) Uani 1 1 d . . . . . O4 O 0.4378(3) 0.62498(19) 0.93955(17) 0.0165(5) Uani 1 1 d . . . . . OW1 O 0.6344(3) 0.4416(2) 0.90886(17) 0.0157(5) Uani 1 1 d D . . . . O3 O 0.5934(3) 0.65214(19) 0.83985(16) 0.0152(5) Uani 1 1 d . . . . . O2 O 0.4627(3) 0.30179(19) 0.74369(17) 0.0178(5) Uani 1 1 d . . . . . O5 O 0.2662(3) 0.4053(2) 0.87346(17) 0.0180(5) Uani 1 1 d . . . . . O1 O 0.2875(3) 0.37405(19) 0.65592(17) 0.0166(5) Uani 1 1 d . . . . . N1 N 0.6599(3) 0.4618(2) 0.7018(2) 0.0133(6) Uani 1 1 d . . . . . N2 N 0.4278(3) 0.5858(2) 0.6611(2) 0.0128(6) Uani 1 1 d . . . . . N3 N 0.2039(3) 0.5961(2) 0.7722(2) 0.0139(6) Uani 1 1 d . . . . . O6 O 0.1497(3) 0.4192(2) 1.00041(17) 0.0200(6) Uani 1 1 d . . . . . C11 C 0.1877(4) 0.6527(3) 0.7038(2) 0.0139(7) Uani 1 1 d . . . . . C5 C 0.6700(4) 0.5118(3) 0.6309(2) 0.0159(7) Uani 1 1 d . . . . . C6 C 0.5489(4) 0.5852(3) 0.6128(2) 0.0133(7) Uani 1 1 d . . . . . C24 C 0.5932(4) 0.7846(3) 0.9730(3) 0.0163(7) Uani 1 1 d . . . . . C31 C 0.0754(4) 0.2742(3) 0.8809(2) 0.0149(7) Uani 1 1 d . . . . . C10 C 0.3197(4) 0.6541(3) 0.6491(2) 0.0145(7) Uani 1 1 d . . . . . C1 C 0.7714(4) 0.3986(3) 0.7229(3) 0.0168(8) Uani 1 1 d . . . . . H1 H 0.7632 0.3638 0.7717 0.020 Uiso 1 1 calc R U . . . C32 C 0.1241(4) 0.2041(3) 0.8103(2) 0.0166(7) Uani 1 1 d . . . . . H32 H 0.2155 0.2195 0.7880 0.020 Uiso 1 1 calc R U . . . C23 C 0.5396(4) 0.6810(3) 0.9145(2) 0.0136(7) Uani 1 1 d . . . . . C20 C 0.2471(5) 0.0000(3) 0.5017(3) 0.0210(8) Uani 1 1 d . . . . . C3 C 0.9071(4) 0.4321(3) 0.6019(3) 0.0193(8) Uani 1 1 d . . . . . H3 H 0.9899 0.4221 0.5684 0.023 Uiso 1 1 calc R U . . . C12 C 0.0561(4) 0.7071(3) 0.6873(2) 0.0164(7) Uani 1 1 d . . . . . H12 H 0.0459 0.7447 0.6394 0.020 Uiso 1 1 calc R U . . . C19 C 0.1572(5) 0.0820(3) 0.4847(3) 0.0226(8) Uani 1 1 d . . . . . H19 H 0.0744 0.0726 0.4362 0.027 Uiso 1 1 calc R U . . . C18 C 0.1939(4) 0.1780(3) 0.5418(3) 0.0213(8) Uani 1 1 d . . . . . H18 H 0.1347 0.2332 0.5313 0.026 Uiso 1 1 calc R U . . . C17 C 0.3162(4) 0.1929(3) 0.6135(2) 0.0177(8) Uani 1 1 d . . . . . C16 C 0.3579(4) 0.2960(3) 0.6743(2) 0.0149(7) Uani 1 1 d . . . . . C34 C -0.0958(4) 0.0902(3) 0.8059(3) 0.0212(8) Uani 1 1 d . . . . . C30 C 0.1702(4) 0.3737(3) 0.9224(2) 0.0152(7) Uani 1 1 d . . . . . C15 C 0.0916(4) 0.5972(3) 0.8266(3) 0.0162(7) Uani 1 1 d . . . . . H15 H 0.1043 0.5606 0.8752 0.019 Uiso 1 1 calc R U . . . C14 C -0.0417(4) 0.6500(3) 0.8137(3) 0.0181(8) Uani 1 1 d . . . . . H14 H -0.1174 0.6482 0.8523 0.022 Uiso 1 1 calc R U . . . C4 C 0.7920(4) 0.4967(3) 0.5780(3) 0.0186(8) Uani 1 1 d . . . . . H4 H 0.7958 0.5296 0.5276 0.022 Uiso 1 1 calc R U . . . C33 C 0.0394(4) 0.1117(3) 0.7723(3) 0.0198(8) Uani 1 1 d . . . . . H33 H 0.0730 0.0651 0.7251 0.024 Uiso 1 1 calc R U . . . C29 C 0.7068(4) 0.8462(3) 0.9469(3) 0.0195(8) Uani 1 1 d . . . . . H29 H 0.7506 0.8224 0.8937 0.023 Uiso 1 1 calc R U . . . C7 C 0.5623(4) 0.6519(3) 0.5506(3) 0.0209(8) Uani 1 1 d . . . . . H7 H 0.6451 0.6486 0.5167 0.025 Uiso 1 1 calc R U . . . C8 C 0.4521(5) 0.7226(3) 0.5398(3) 0.0243(9) Uani 1 1 d . . . . . H8 H 0.4598 0.7683 0.4991 0.029 Uiso 1 1 calc R U . . . C26 C 0.5744(5) 0.9175(3) 1.1053(3) 0.0235(9) Uani 1 1 d . . . . . H26 H 0.5290 0.9424 1.1577 0.028 Uiso 1 1 calc R U . . . C13 C -0.0600(4) 0.7051(3) 0.7428(3) 0.0205(8) Uani 1 1 d . . . . . H13 H -0.1491 0.7406 0.7320 0.025 Uiso 1 1 calc R U . . . C35 C -0.1465(5) 0.1577(3) 0.8769(3) 0.0236(9) Uani 1 1 d . . . . . H35 H -0.2377 0.1414 0.8991 0.028 Uiso 1 1 calc R U . . . C28 C 0.7551(5) 0.9431(3) 1.0000(3) 0.0247(9) Uani 1 1 d . . . . . H28 H 0.8315 0.9842 0.9831 0.030 Uiso 1 1 calc R U . . . C27 C 0.6880(5) 0.9772(3) 1.0780(3) 0.0238(9) Uani 1 1 d . . . . . C2 C 0.8973(4) 0.3827(3) 0.6760(3) 0.0191(8) Uani 1 1 d . . . . . H2 H 0.9737 0.3397 0.6938 0.023 Uiso 1 1 calc R U . . . C22 C 0.4028(5) 0.1087(3) 0.6304(3) 0.0210(8) Uani 1 1 d . . . . . H22 H 0.4846 0.1177 0.6794 0.025 Uiso 1 1 calc R U . . . C21 C 0.3670(5) 0.0128(3) 0.5746(3) 0.0237(9) Uani 1 1 d . . . . . H21 H 0.4239 -0.0431 0.5863 0.028 Uiso 1 1 calc R U . . . C36 C -0.0607(4) 0.2497(3) 0.9148(3) 0.0211(8) Uani 1 1 d . . . . . H36 H -0.0938 0.2953 0.9628 0.025 Uiso 1 1 calc R U . . . C9 C 0.3294(4) 0.7244(3) 0.5904(3) 0.0208(8) Uani 1 1 d . . . . . H9 H 0.2543 0.7723 0.5851 0.025 Uiso 1 1 calc R U . . . C25 C 0.5295(4) 0.8199(3) 1.0531(3) 0.0199(8) Uani 1 1 d . . . . . H25 H 0.4562 0.7779 1.0718 0.024 Uiso 1 1 calc R U . . . H37 H 0.709(5) 0.494(3) 0.945(3) 0.063(17) Uiso 1 1 d D . . . . H38 H 0.606(6) 0.401(4) 0.952(3) 0.067(18) Uiso 1 1 d 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 Gd1 0.01033(8) 0.01257(9) 0.01194(9) 0.00299(6) 0.00368(6) 0.00090(6) Cl2 0.0483(7) 0.0197(5) 0.0418(7) -0.0048(5) -0.0090(5) -0.0001(5) Cl3 0.0369(6) 0.0232(5) 0.0368(6) 0.0029(5) 0.0085(5) -0.0090(5) Cl1 0.0316(5) 0.0191(5) 0.0272(5) 0.0009(4) -0.0009(4) 0.0036(4) O4 0.0152(12) 0.0190(14) 0.0163(13) 0.0050(11) 0.0040(10) 0.0004(10) OW1 0.0142(13) 0.0174(14) 0.0163(13) 0.0047(11) 0.0028(10) 0.0004(10) O3 0.0155(12) 0.0160(13) 0.0143(12) 0.0021(10) 0.0045(10) -0.0003(10) O2 0.0181(13) 0.0155(13) 0.0198(13) 0.0028(11) 0.0029(11) 0.0006(11) O5 0.0187(13) 0.0188(14) 0.0190(13) 0.0075(11) 0.0069(11) -0.0022(11) O1 0.0205(13) 0.0131(13) 0.0171(13) 0.0032(10) 0.0055(10) 0.0012(10) N1 0.0125(14) 0.0121(15) 0.0154(15) 0.0013(12) 0.0038(12) 0.0010(11) N2 0.0117(14) 0.0123(15) 0.0145(15) 0.0019(12) 0.0032(11) 0.0012(11) N3 0.0135(14) 0.0141(15) 0.0146(15) 0.0038(12) 0.0025(12) 0.0013(12) O6 0.0179(13) 0.0249(15) 0.0176(13) 0.0035(11) 0.0061(11) -0.0033(11) C11 0.0107(16) 0.0138(18) 0.0169(18) 0.0022(14) 0.0021(13) 0.0005(13) C5 0.0181(18) 0.0158(19) 0.0136(17) 0.0020(14) 0.0038(14) -0.0046(15) C6 0.0156(17) 0.0106(17) 0.0133(17) 0.0011(14) 0.0030(13) -0.0016(13) C24 0.0143(17) 0.0148(18) 0.0194(19) 0.0035(15) -0.0001(14) 0.0027(14) C31 0.0114(17) 0.0198(19) 0.0155(18) 0.0082(15) 0.0019(14) 0.0030(14) C10 0.0159(17) 0.0146(18) 0.0127(17) 0.0019(14) 0.0014(14) 0.0015(14) C1 0.0158(18) 0.0171(19) 0.0189(19) 0.0053(15) 0.0040(15) 0.0024(15) C32 0.0157(18) 0.0182(19) 0.0186(18) 0.0068(15) 0.0074(14) 0.0025(14) C23 0.0138(17) 0.0132(18) 0.0152(17) 0.0070(14) 0.0006(14) 0.0024(14) C20 0.026(2) 0.0146(19) 0.022(2) 0.0026(16) 0.0034(16) 0.0007(16) C3 0.0192(19) 0.020(2) 0.0197(19) 0.0021(16) 0.0080(15) 0.0011(15) C12 0.0171(18) 0.0163(19) 0.0164(18) 0.0032(15) 0.0035(14) 0.0032(15) C19 0.024(2) 0.022(2) 0.020(2) 0.0026(16) -0.0007(16) -0.0004(16) C18 0.025(2) 0.0156(19) 0.025(2) 0.0072(16) 0.0029(16) 0.0022(16) C17 0.0197(19) 0.019(2) 0.0157(18) 0.0030(15) 0.0073(15) -0.0027(15) C16 0.0158(17) 0.0162(19) 0.0150(18) 0.0021(14) 0.0109(14) 0.0006(14) C34 0.0209(19) 0.017(2) 0.027(2) 0.0070(16) 0.0042(16) -0.0034(16) C30 0.0142(17) 0.0168(19) 0.0168(18) 0.0086(15) 0.0020(14) 0.0038(14) C15 0.0134(17) 0.0191(19) 0.0176(18) 0.0037(15) 0.0073(14) -0.0008(14) C14 0.0163(18) 0.0177(19) 0.0212(19) 0.0031(15) 0.0072(15) -0.0026(15) C4 0.0194(19) 0.022(2) 0.0171(18) 0.0062(16) 0.0082(15) 0.0034(15) C33 0.024(2) 0.0164(19) 0.0196(19) 0.0028(15) 0.0055(16) 0.0011(16) C29 0.0214(19) 0.019(2) 0.0199(19) 0.0071(16) 0.0050(15) 0.0000(15) C7 0.0198(19) 0.026(2) 0.021(2) 0.0093(17) 0.0110(16) 0.0021(16) C8 0.026(2) 0.025(2) 0.028(2) 0.0150(18) 0.0083(17) 0.0052(17) C26 0.027(2) 0.020(2) 0.021(2) -0.0038(16) 0.0010(16) 0.0050(17) C13 0.0134(18) 0.018(2) 0.029(2) 0.0032(17) 0.0013(15) 0.0040(15) C35 0.0187(19) 0.019(2) 0.034(2) 0.0062(18) 0.0076(17) -0.0004(16) C28 0.025(2) 0.0143(19) 0.034(2) 0.0055(17) 0.0004(18) -0.0049(16) C27 0.025(2) 0.016(2) 0.024(2) -0.0019(16) -0.0083(17) 0.0014(16) C2 0.0169(18) 0.0154(19) 0.025(2) 0.0025(16) 0.0027(15) 0.0060(15) C22 0.025(2) 0.0167(19) 0.021(2) 0.0053(16) 0.0032(16) 0.0009(16) C21 0.026(2) 0.020(2) 0.026(2) 0.0054(17) 0.0029(17) 0.0072(17) C36 0.0193(19) 0.020(2) 0.025(2) 0.0032(16) 0.0082(16) 0.0019(16) C9 0.022(2) 0.022(2) 0.022(2) 0.0104(17) 0.0069(16) 0.0080(16) C25 0.0209(19) 0.020(2) 0.0179(19) 0.0020(16) 0.0018(15) 0.0007(16) _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 Gd1 O5 2.299(2) . ? Gd1 OW1 2.373(2) . ? Gd1 O2 2.459(3) . ? Gd1 O3 2.465(2) . ? Gd1 O4 2.507(3) . ? Gd1 O1 2.510(2) . ? Gd1 N3 2.548(3) . ? Gd1 N1 2.572(3) . ? Gd1 N2 2.599(3) . ? Gd1 C16 2.835(4) . ? Gd1 C23 2.853(4) . ? Cl2 C27 1.746(4) . ? Cl3 C34 1.750(4) . ? Cl1 C20 1.742(4) . ? O4 C23 1.266(4) . ? OW1 H37 0.96(2) . ? OW1 H38 0.947(19) . ? O3 C23 1.259(4) . ? O2 C16 1.263(4) . ? O5 C30 1.281(4) . ? O1 C16 1.268(4) . ? N1 C1 1.342(4) . ? N1 C5 1.343(4) . ? N2 C10 1.342(4) . ? N2 C6 1.351(4) . ? N3 C15 1.346(4) . ? N3 C11 1.355(4) . ? O6 C30 1.240(4) . ? C11 C12 1.389(5) . ? C11 C10 1.493(5) . ? C5 C4 1.401(5) . ? C5 C6 1.485(5) . ? C6 C7 1.392(5) . ? C24 C25 1.388(5) . ? C24 C29 1.393(5) . ? C24 C23 1.499(5) . ? C31 C32 1.390(5) . ? C31 C36 1.395(5) . ? C31 C30 1.506(5) . ? C10 C9 1.384(5) . ? C1 C2 1.378(5) . ? C1 H1 0.9300 . ? C32 C33 1.384(5) . ? C32 H32 0.9300 . ? C20 C21 1.374(5) . ? C20 C19 1.395(5) . ? C3 C2 1.378(5) . ? C3 C4 1.387(5) . ? C3 H3 0.9300 . ? C12 C13 1.387(5) . ? C12 H12 0.9300 . ? C19 C18 1.388(5) . ? C19 H19 0.9300 . ? C18 C17 1.374(5) . ? C18 H18 0.9300 . ? C17 C22 1.403(5) . ? C17 C16 1.491(5) . ? C34 C33 1.376(5) . ? C34 C35 1.383(6) . ? C15 C14 1.382(5) . ? C15 H15 0.9300 . ? C14 C13 1.373(5) . ? C14 H14 0.9300 . ? C4 H4 0.9300 . ? C33 H33 0.9300 . ? C29 C28 1.391(5) . ? C29 H29 0.9300 . ? C7 C8 1.375(5) . ? C7 H7 0.9300 . ? C8 C9 1.383(5) . ? C8 H8 0.9300 . ? C26 C27 1.386(6) . ? C26 C25 1.388(5) . ? C26 H26 0.9300 . ? C13 H13 0.9300 . ? C35 C36 1.383(5) . ? C35 H35 0.9300 . ? C28 C27 1.375(6) . ? C28 H28 0.9300 . ? C2 H2 0.9300 . ? C22 C21 1.380(5) . ? C22 H22 0.9300 . ? C21 H21 0.9300 . ? C36 H36 0.9300 . ? C9 H9 0.9300 . ? C25 H25 0.9300 . ? 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 Gd1 OW1 85.60(9) . . ? O5 Gd1 O2 76.07(9) . . ? OW1 Gd1 O2 75.52(9) . . ? O5 Gd1 O3 133.59(8) . . ? OW1 Gd1 O3 80.82(8) . . ? O2 Gd1 O3 140.25(8) . . ? O5 Gd1 O4 81.27(8) . . ? OW1 Gd1 O4 76.32(8) . . ? O2 Gd1 O4 144.88(8) . . ? O3 Gd1 O4 52.44(8) . . ? O5 Gd1 O1 83.26(8) . . ? OW1 Gd1 O1 128.47(8) . . ? O2 Gd1 O1 52.96(8) . . ? O3 Gd1 O1 138.20(8) . . ? O4 Gd1 O1 149.47(8) . . ? O5 Gd1 N3 81.61(9) . . ? OW1 Gd1 N3 146.25(9) . . ? O2 Gd1 N3 130.23(9) . . ? O3 Gd1 N3 85.68(9) . . ? O4 Gd1 N3 70.95(9) . . ? O1 Gd1 N3 80.88(9) . . ? O5 Gd1 N1 144.89(9) . . ? OW1 Gd1 N1 79.13(9) . . ? O2 Gd1 N1 69.59(9) . . ? O3 Gd1 N1 74.94(9) . . ? O4 Gd1 N1 124.39(9) . . ? O1 Gd1 N1 81.95(8) . . ? N3 Gd1 N1 126.74(9) . . ? O5 Gd1 N2 139.18(9) . . ? OW1 Gd1 N2 135.21(9) . . ? O2 Gd1 N2 110.08(9) . . ? O3 Gd1 N2 67.09(8) . . ? O4 Gd1 N2 104.64(8) . . ? O1 Gd1 N2 71.50(8) . . ? N3 Gd1 N2 63.44(9) . . ? N1 Gd1 N2 63.30(9) . . ? O5 Gd1 C16 77.93(9) . . ? OW1 Gd1 C16 101.92(10) . . ? O2 Gd1 C16 26.41(9) . . ? O3 Gd1 C16 148.30(9) . . ? O4 Gd1 C16 159.20(9) . . ? O1 Gd1 C16 26.56(9) . . ? N3 Gd1 C16 105.68(10) . . ? N1 Gd1 C16 74.64(9) . . ? N2 Gd1 C16 91.24(10) . . ? O5 Gd1 C23 107.54(9) . . ? OW1 Gd1 C23 77.15(9) . . ? O2 Gd1 C23 152.06(9) . . ? O3 Gd1 C23 26.12(9) . . ? O4 Gd1 C23 26.32(9) . . ? O1 Gd1 C23 153.66(9) . . ? N3 Gd1 C23 77.20(10) . . ? N1 Gd1 C23 99.65(10) . . ? N2 Gd1 C23 85.63(9) . . ? C16 Gd1 C23 174.27(10) . . ? C23 O4 Gd1 92.3(2) . . ? Gd1 OW1 H37 120(3) . . ? Gd1 OW1 H38 118(3) . . ? H37 OW1 H38 105(4) . . ? C23 O3 Gd1 94.4(2) . . ? C16 O2 Gd1 93.6(2) . . ? C30 O5 Gd1 171.2(2) . . ? C16 O1 Gd1 91.1(2) . . ? C1 N1 C5 118.8(3) . . ? C1 N1 Gd1 119.6(2) . . ? C5 N1 Gd1 121.7(2) . . ? C10 N2 C6 118.3(3) . . ? C10 N2 Gd1 120.1(2) . . ? C6 N2 Gd1 120.3(2) . . ? C15 N3 C11 118.2(3) . . ? C15 N3 Gd1 119.6(2) . . ? C11 N3 Gd1 122.3(2) . . ? N3 C11 C12 121.2(3) . . ? N3 C11 C10 116.2(3) . . ? C12 C11 C10 122.7(3) . . ? N1 C5 C4 121.0(3) . . ? N1 C5 C6 117.1(3) . . ? C4 C5 C6 121.8(3) . . ? N2 C6 C7 121.8(3) . . ? N2 C6 C5 116.9(3) . . ? C7 C6 C5 121.3(3) . . ? C25 C24 C29 119.6(4) . . ? C25 C24 C23 120.4(3) . . ? C29 C24 C23 120.0(3) . . ? C32 C31 C36 118.9(3) . . ? C32 C31 C30 120.7(3) . . ? C36 C31 C30 120.4(3) . . ? N2 C10 C9 122.4(3) . . ? N2 C10 C11 116.8(3) . . ? C9 C10 C11 120.7(3) . . ? N1 C1 C2 123.3(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C33 C32 C31 121.4(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? O3 C23 O4 120.9(3) . . ? O3 C23 C24 119.6(3) . . ? O4 C23 C24 119.5(3) . . ? O3 C23 Gd1 59.50(18) . . ? O4 C23 Gd1 61.42(18) . . ? C24 C23 Gd1 178.4(2) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 Cl1 120.1(3) . . ? C19 C20 Cl1 118.8(3) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C18 C19 C20 118.5(4) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.7 . . ? C17 C18 C19 121.2(4) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C17 C22 119.2(4) . . ? C18 C17 C16 121.6(3) . . ? C22 C17 C16 119.2(3) . . ? O2 C16 O1 122.2(3) . . ? O2 C16 C17 118.0(3) . . ? O1 C16 C17 119.8(3) . . ? O2 C16 Gd1 59.96(18) . . ? O1 C16 Gd1 62.29(18) . . ? C17 C16 Gd1 176.8(2) . . ? C33 C34 C35 121.6(4) . . ? C33 C34 Cl3 119.8(3) . . ? C35 C34 Cl3 118.6(3) . . ? O6 C30 O5 124.9(3) . . ? O6 C30 C31 118.3(3) . . ? O5 C30 C31 116.8(3) . . ? N3 C15 C14 123.2(3) . . ? N3 C15 H15 118.4 . . ? C14 C15 H15 118.4 . . ? C13 C14 C15 118.6(3) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C3 C4 C5 119.2(3) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C34 C33 C32 118.5(4) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C28 C29 C24 120.3(4) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C8 C7 C6 119.4(3) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 H8 120.6 . . ? C9 C8 H8 120.6 . . ? C27 C26 C25 118.8(4) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C14 C13 C12 119.2(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C34 C35 C36 119.5(4) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C27 C28 C29 118.9(4) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C28 C27 C26 121.8(4) . . ? C28 C27 Cl2 119.0(3) . . ? C26 C27 Cl2 119.2(3) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C21 C22 C17 120.2(4) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C35 C36 C31 120.0(4) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C8 C9 C10 119.2(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C24 C25 C26 120.4(4) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? _refine_diff_density_max 0.912 _refine_diff_density_min -1.640 _refine_diff_density_rms 0.153 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.6934 13.1762 14.7709 100.235 97.940 92.176 ZERR 2.00 0.0009 0.0013 0.0015 0.001 0.001 0.001 LATT 1 SFAC C H N O CL GD UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 ACTA 51.00 BOND $H DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 L.S. 12 WGHT 0.032300 FVAR 0.12279 GD1 6 0.435525 0.486695 0.798743 11.00000 0.01033 0.01257 = 0.01194 0.00299 0.00368 0.00090 CL2 5 0.750163 1.098220 1.145409 11.00000 0.04825 0.01974 = 0.04179 -0.00481 -0.00904 -0.00006 CL3 5 -0.208383 -0.024601 0.757958 11.00000 0.03695 0.02316 = 0.03685 0.00290 0.00846 -0.00902 CL1 5 0.203893 -0.120049 0.429087 11.00000 0.03157 0.01909 = 0.02723 0.00095 -0.00087 0.00356 O4 4 0.437823 0.624978 0.939548 11.00000 0.01520 0.01900 = 0.01630 0.00502 0.00396 0.00042 OW1 4 0.634401 0.441575 0.908860 11.00000 0.01421 0.01736 = 0.01634 0.00470 0.00279 0.00037 O3 4 0.593429 0.652137 0.839850 11.00000 0.01551 0.01602 = 0.01430 0.00214 0.00451 -0.00032 O2 4 0.462748 0.301786 0.743692 11.00000 0.01806 0.01548 = 0.01984 0.00284 0.00293 0.00058 O5 4 0.266208 0.405339 0.873461 11.00000 0.01872 0.01880 = 0.01902 0.00748 0.00692 -0.00223 O1 4 0.287537 0.374052 0.655916 11.00000 0.02049 0.01308 = 0.01710 0.00323 0.00553 0.00124 N1 3 0.659913 0.461848 0.701802 11.00000 0.01246 0.01215 = 0.01540 0.00129 0.00379 0.00100 N2 3 0.427794 0.585799 0.661076 11.00000 0.01170 0.01230 = 0.01451 0.00195 0.00323 0.00118 N3 3 0.203929 0.596143 0.772242 11.00000 0.01354 0.01406 = 0.01457 0.00383 0.00251 0.00126 O6 4 0.149678 0.419202 1.000409 11.00000 0.01792 0.02494 = 0.01760 0.00353 0.00606 -0.00327 C11 1 0.187685 0.652702 0.703759 11.00000 0.01070 0.01380 = 0.01686 0.00222 0.00207 0.00050 C5 1 0.669965 0.511785 0.630883 11.00000 0.01811 0.01579 = 0.01363 0.00198 0.00385 -0.00461 C6 1 0.548914 0.585160 0.612756 11.00000 0.01561 0.01060 = 0.01334 0.00111 0.00296 -0.00162 C24 1 0.593170 0.784554 0.973050 11.00000 0.01429 0.01476 = 0.01940 0.00351 -0.00008 0.00273 C31 1 0.075396 0.274241 0.880915 11.00000 0.01138 0.01977 = 0.01554 0.00821 0.00189 0.00297 C10 1 0.319654 0.654113 0.649084 11.00000 0.01589 0.01462 = 0.01271 0.00194 0.00144 0.00150 C1 1 0.771362 0.398630 0.722926 11.00000 0.01583 0.01708 = 0.01886 0.00533 0.00399 0.00239 AFIX 43 H1 2 0.763218 0.363788 0.771739 11.00000 -1.20000 AFIX 0 C32 1 0.124097 0.204066 0.810269 11.00000 0.01571 0.01817 = 0.01861 0.00684 0.00739 0.00248 AFIX 43 H32 2 0.215546 0.219545 0.788049 11.00000 -1.20000 AFIX 0 C23 1 0.539646 0.680981 0.914511 11.00000 0.01377 0.01318 = 0.01518 0.00700 0.00059 0.00245 C20 1 0.247078 0.000012 0.501668 11.00000 0.02608 0.01462 = 0.02202 0.00256 0.00341 0.00070 C3 1 0.907060 0.432052 0.601941 11.00000 0.01921 0.01973 = 0.01973 0.00206 0.00803 0.00112 AFIX 43 H3 2 0.989929 0.422123 0.568364 11.00000 -1.20000 AFIX 0 C12 1 0.056089 0.707125 0.687327 11.00000 0.01710 0.01633 = 0.01640 0.00321 0.00349 0.00322 AFIX 43 H12 2 0.045872 0.744728 0.639410 11.00000 -1.20000 AFIX 0 C19 1 0.157166 0.081997 0.484690 11.00000 0.02395 0.02180 = 0.02041 0.00256 -0.00067 -0.00037 AFIX 43 H19 2 0.074422 0.072567 0.436213 11.00000 -1.20000 AFIX 0 C18 1 0.193941 0.177956 0.541755 11.00000 0.02491 0.01562 = 0.02459 0.00720 0.00291 0.00223 AFIX 43 H18 2 0.134746 0.233185 0.531260 11.00000 -1.20000 AFIX 0 C17 1 0.316161 0.192871 0.613454 11.00000 0.01972 0.01865 = 0.01574 0.00301 0.00726 -0.00266 C16 1 0.357888 0.295971 0.674310 11.00000 0.01580 0.01618 = 0.01495 0.00211 0.01091 0.00056 C34 1 -0.095778 0.090178 0.805938 11.00000 0.02089 0.01698 = 0.02659 0.00696 0.00421 -0.00336 C30 1 0.170227 0.373739 0.922414 11.00000 0.01422 0.01683 = 0.01677 0.00864 0.00197 0.00380 C15 1 0.091571 0.597192 0.826593 11.00000 0.01336 0.01914 = 0.01761 0.00368 0.00734 -0.00085 AFIX 43 H15 2 0.104262 0.560597 0.875181 11.00000 -1.20000 AFIX 0 C14 1 -0.041706 0.649992 0.813711 11.00000 0.01627 0.01766 = 0.02124 0.00312 0.00721 -0.00264 AFIX 43 H14 2 -0.117367 0.648228 0.852285 11.00000 -1.20000 AFIX 0 C4 1 0.791989 0.496683 0.578049 11.00000 0.01943 0.02185 = 0.01711 0.00619 0.00824 0.00341 AFIX 43 H4 2 0.795784 0.529579 0.527593 11.00000 -1.20000 AFIX 0 C33 1 0.039362 0.111659 0.772309 11.00000 0.02400 0.01638 = 0.01961 0.00283 0.00545 0.00114 AFIX 43 H33 2 0.072993 0.065130 0.725138 11.00000 -1.20000 AFIX 0 C29 1 0.706810 0.846166 0.946929 11.00000 0.02139 0.01913 = 0.01985 0.00707 0.00496 0.00005 AFIX 43 H29 2 0.750634 0.822386 0.893737 11.00000 -1.20000 AFIX 0 C7 1 0.562330 0.651860 0.550575 11.00000 0.01983 0.02572 = 0.02143 0.00928 0.01101 0.00207 AFIX 43 H7 2 0.645108 0.648626 0.516664 11.00000 -1.20000 AFIX 0 C8 1 0.452055 0.722566 0.539762 11.00000 0.02550 0.02520 = 0.02762 0.01504 0.00835 0.00523 AFIX 43 H8 2 0.459816 0.768314 0.499125 11.00000 -1.20000 AFIX 0 C26 1 0.574356 0.917499 1.105311 11.00000 0.02660 0.01962 = 0.02108 -0.00385 0.00103 0.00501 AFIX 43 H26 2 0.529026 0.942361 1.157679 11.00000 -1.20000 AFIX 0 C13 1 -0.059986 0.705088 0.742759 11.00000 0.01340 0.01842 = 0.02906 0.00320 0.00125 0.00403 AFIX 43 H13 2 -0.149119 0.740620 0.731985 11.00000 -1.20000 AFIX 0 C35 1 -0.146520 0.157718 0.876925 11.00000 0.01867 0.01929 = 0.03409 0.00616 0.00763 -0.00042 AFIX 43 H35 2 -0.237687 0.141405 0.899063 11.00000 -1.20000 AFIX 0 C28 1 0.755080 0.943116 1.000029 11.00000 0.02468 0.01431 = 0.03386 0.00553 0.00037 -0.00486 AFIX 43 H28 2 0.831542 0.984215 0.983057 11.00000 -1.20000 AFIX 0 C27 1 0.687951 0.977209 1.078000 11.00000 0.02548 0.01624 = 0.02422 -0.00194 -0.00832 0.00140 C2 1 0.897272 0.382704 0.675977 11.00000 0.01687 0.01542 = 0.02478 0.00251 0.00269 0.00596 AFIX 43 H2 2 0.973741 0.339736 0.693793 11.00000 -1.20000 AFIX 0 C22 1 0.402808 0.108748 0.630414 11.00000 0.02527 0.01670 = 0.02146 0.00534 0.00320 0.00088 AFIX 43 H22 2 0.484608 0.117689 0.679433 11.00000 -1.20000 AFIX 0 C21 1 0.367012 0.012762 0.574568 11.00000 0.02585 0.01967 = 0.02612 0.00542 0.00293 0.00725 AFIX 43 H21 2 0.423891 -0.043082 0.586254 11.00000 -1.20000 AFIX 0 C36 1 -0.060736 0.249721 0.914786 11.00000 0.01931 0.02010 = 0.02505 0.00317 0.00820 0.00188 AFIX 43 H36 2 -0.093816 0.295264 0.962848 11.00000 -1.20000 AFIX 0 C9 1 0.329379 0.724435 0.590401 11.00000 0.02201 0.02203 = 0.02238 0.01040 0.00687 0.00802 AFIX 43 H9 2 0.254345 0.772346 0.585093 11.00000 -1.20000 AFIX 0 C25 1 0.529457 0.819897 1.053078 11.00000 0.02092 0.02008 = 0.01785 0.00202 0.00181 0.00075 AFIX 43 H25 2 0.456194 0.777923 1.071846 11.00000 -1.20000 AFIX 0 H37 2 0.709467 0.493524 0.944779 11.00000 0.06296 H38 2 0.605745 0.401291 0.951715 11.00000 0.06724 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0387 for 7210 Fo > 4sig(Fo) and 0.0556 for all 8862 data REM 459 parameters refined using 2 restraints END WGHT 0.0323 0.0000 REM Highest difference peak 0.912, deepest hole -1.640, 1-sigma level 0.153 Q1 1 0.1011 -0.1198 0.4538 11.00000 0.05 0.91 Q2 1 0.3570 0.4790 0.7167 11.00000 0.05 0.77 Q3 1 0.8030 1.1436 1.0983 11.00000 0.05 0.75 Q4 1 0.4987 0.4355 0.7289 11.00000 0.05 0.72 Q5 1 0.4416 0.5380 0.8037 11.00000 0.05 0.71 Q6 1 0.4651 0.5834 0.8599 11.00000 0.05 0.70 Q7 1 0.3618 0.5460 0.8571 11.00000 0.05 0.69 Q8 1 0.3264 0.4293 0.7605 11.00000 0.05 0.67 Q9 1 -0.3290 -0.0260 0.7443 11.00000 0.05 0.66 Q10 1 0.0595 0.0793 0.5067 11.00000 0.05 0.63 ; _shelx_res_checksum 80997 _shelx_hkl_file ; -1 0 0 301.79 8.34 -1 0 0 297.21 8.51 1 0 0 304.05 8.67 1 0 0 306.55 8.16 -2 0 0 0.15 0.56 -2 0 0 -0.06 0.68 2 0 0 0.05 0.56 2 0 0 0.51 0.70 -3 0 0 92.07 3.69 -3 0 0 95.70 3.57 3 0 0 92.61 3.28 3 0 0 94.08 3.81 -4 0 0 -1.02 0.77 -4 0 0 0.45 0.83 4 0 0 0.30 0.67 4 0 0 0.45 0.89 -5 0 0 52.55 3.13 -5 0 0 52.81 2.84 5 0 0 49.10 2.49 5 0 0 48.72 3.11 -6 0 0 113.12 4.79 -6 0 0 113.78 5.34 6 0 0 130.00 5.63 6 0 0 120.42 4.47 -7 0 0 37.54 3.54 -7 0 0 32.21 2.75 7 0 0 38.03 3.70 7 0 0 34.93 2.41 -8 0 0 136.86 6.62 -8 0 0 136.09 5.88 8 0 0 148.63 6.98 -9 0 0 72.27 5.00 9 0 0 66.02 4.86 -10 0 0 16.71 3.24 10 0 0 19.76 3.37 -11 0 0 4.26 2.28 11 0 0 1.18 1.86 11 -1 0 5.85 2.38 -11 1 0 9.14 2.99 10 -1 0 15.78 3.03 -10 1 0 16.79 3.28 9 -1 0 36.41 4.11 -9 1 0 41.13 4.37 8 -1 0 134.44 6.78 -8 1 0 139.43 6.74 7 -1 0 69.43 3.51 7 -1 0 67.96 4.30 -7 1 0 68.15 4.11 -7 1 0 63.87 3.44 6 -1 0 13.09 2.13 6 -1 0 13.54 1.68 -6 1 0 8.94 1.82 -6 1 0 11.30 1.50 5 -1 0 1.84 0.90 5 -1 0 1.59 1.03 -5 1 0 1.10 1.00 -5 1 0 0.44 0.79 4 -1 0 14.16 1.48 4 -1 0 14.90 1.82 -4 1 0 14.97 1.38 -4 1 0 12.87 1.58 3 -1 0 48.39 2.45 3 -1 0 48.36 2.66 3 -1 0 50.00 2.41 -3 1 0 47.10 2.18 -3 1 0 48.76 2.48 2 -1 0 554.25 15.47 2 -1 0 520.09 14.17 2 -1 0 519.78 14.73 -2 1 0 529.19 14.59 -2 1 0 553.07 15.25 1 -1 0 378.65 10.36 1 -1 0 378.77 10.13 -1 1 0 366.78 10.13 -1 1 0 367.91 10.61 -1 1 0 395.34 10.73 0 -1 0 351.51 9.46 0 1 0 351.75 9.68 -1 -1 0 244.77 6.93 -1 -1 0 245.15 6.96 1 1 0 231.26 7.07 -2 -1 0 120.20 4.12 -2 -1 0 120.79 4.15 2 1 0 118.80 4.28 2 1 0 119.95 3.45 -3 -1 0 15.83 1.49 -3 -1 0 14.12 1.51 3 1 0 13.83 1.57 3 1 0 14.94 1.13 -4 -1 0 52.26 2.86 -4 -1 0 51.63 2.87 4 1 0 50.52 2.11 4 1 0 48.56 2.91 -5 -1 0 14.20 1.79 -5 -1 0 12.30 1.64 5 1 0 10.65 1.79 5 1 0 12.61 1.17 -6 -1 0 74.71 4.02 -6 -1 0 91.92 4.53 6 1 0 88.94 3.36 6 1 0 90.68 4.69 -7 -1 0 105.66 4.95 -7 -1 0 109.40 5.46 7 1 0 108.80 5.64 -8 -1 0 42.46 3.32 -8 -1 0 47.40 3.78 8 1 0 38.44 4.02 -9 -1 0 51.32 4.17 9 1 0 40.80 4.34 -10 -1 0 32.96 4.16 10 1 0 28.05 3.90 -11 -1 0 9.90 2.78 11 1 0 8.34 2.75 11 -2 0 6.16 2.57 -11 2 0 6.99 2.91 10 -2 0 3.89 2.06 -10 2 0 9.35 2.76 9 -2 0 36.07 4.08 -9 2 0 38.19 4.26 8 -2 0 53.40 3.52 8 -2 0 50.93 4.01 -8 2 0 52.69 3.99 7 -2 0 39.34 3.37 7 -2 0 45.49 3.16 -7 2 0 44.32 3.41 6 -2 0 36.30 3.25 6 -2 0 30.59 2.44 -6 2 0 25.55 2.07 -6 2 0 25.06 2.70 5 -2 0 22.09 2.37 5 -2 0 23.16 2.14 -5 2 0 21.49 1.62 -5 2 0 16.99 2.06 4 -2 0 13.10 1.76 4 -2 0 12.64 1.58 4 -2 0 14.97 1.65 -4 2 0 11.35 1.65 -4 2 0 11.02 1.09 3 -2 0 3.18 1.04 3 -2 0 2.61 0.91 3 -2 0 3.77 1.04 -3 2 0 3.67 0.67 -3 2 0 4.91 1.09 2 -2 0 20.70 1.63 -2 2 0 20.34 1.57 -2 2 0 21.13 1.58 -2 2 0 18.86 1.05 1 -2 0 160.74 5.05 1 -2 0 166.24 4.61 -1 2 0 167.41 5.03 -1 2 0 165.54 5.08 -1 2 0 156.47 4.60 0 -2 0 339.18 9.48 0 -2 0 341.65 9.37 0 2 0 316.37 9.53 0 2 0 356.42 9.72 -1 -2 0 165.51 4.98 -1 -2 0 161.62 5.17 -1 -2 0 161.86 4.55 1 2 0 155.61 5.13 -2 -2 0 8.33 1.28 -2 -2 0 7.96 1.03 2 2 0 8.36 1.20 -3 -2 0 63.02 3.21 -3 -2 0 65.13 3.01 3 2 0 70.70 3.32 -4 -2 0 8.17 1.35 -4 -2 0 10.49 1.58 4 2 0 9.06 1.60 4 2 0 8.60 0.75 -5 -2 0 118.81 5.01 -5 -2 0 111.19 4.94 5 2 0 122.97 3.80 5 2 0 119.86 5.30 -6 -2 0 73.33 4.07 -6 -2 0 80.68 4.19 6 2 0 81.93 4.43 -7 -2 0 39.00 3.12 -7 -2 0 42.27 3.28 7 2 0 41.47 3.41 -8 -2 0 16.86 2.47 -8 -2 0 16.63 2.75 8 2 0 19.93 2.93 -9 -2 0 76.65 5.07 -9 -2 0 75.32 4.61 9 2 0 68.29 5.00 -10 -2 0 17.55 3.16 10 2 0 10.66 2.68 -11 -2 0 0.45 2.08 11 2 0 -0.84 1.57 11 -3 0 7.86 2.60 -11 3 0 10.15 2.93 10 -3 0 11.21 2.78 -10 3 0 10.28 2.97 9 -3 0 30.16 3.85 -9 3 0 33.27 3.94 8 -3 0 106.76 5.19 8 -3 0 101.77 5.72 -8 3 0 102.42 5.81 7 -3 0 24.39 2.65 7 -3 0 24.56 3.02 -7 3 0 26.09 3.12 6 -3 0 3.15 1.30 6 -3 0 1.85 1.25 -6 3 0 0.91 0.78 -6 3 0 -0.73 1.06 5 -3 0 1.10 1.12 5 -3 0 2.32 1.18 5 -3 0 5.91 1.30 -5 3 0 2.34 0.74 -5 3 0 3.05 1.14 4 -3 0 -0.22 0.83 4 -3 0 2.30 1.03 4 -3 0 0.36 1.02 -4 3 0 -0.61 0.79 -4 3 0 0.76 0.56 3 -3 0 40.94 2.59 -3 3 0 35.54 2.25 -3 3 0 36.37 1.49 -3 3 0 37.86 2.45 2 -3 0 86.67 2.64 2 -3 0 85.98 3.61 -2 3 0 89.14 3.39 -2 3 0 82.60 3.48 1 -3 0 45.70 1.86 1 -3 0 45.53 2.37 -1 3 0 43.90 2.05 -1 3 0 45.04 2.26 0 -3 0 15.46 1.30 0 -3 0 18.84 1.53 0 3 0 19.89 1.42 0 3 0 19.87 1.46 -1 -3 0 168.15 5.61 -1 -3 0 166.62 5.05 1 3 0 174.83 5.57 1 3 0 172.43 5.39 -2 -3 0 2.11 0.78 -2 -3 0 0.98 1.05 2 3 0 0.94 0.86 -3 -3 0 6.65 1.39 -3 -3 0 5.07 1.05 3 3 0 6.09 1.29 -4 -3 0 19.42 1.89 -4 -3 0 18.35 2.04 4 3 0 16.42 2.01 -5 -3 0 28.42 2.62 -5 -3 0 28.32 2.55 5 3 0 28.09 2.79 -6 -3 0 54.18 3.59 -6 -3 0 52.85 3.31 6 3 0 57.62 3.76 -7 -3 0 112.52 5.53 -7 -3 0 108.23 5.47 7 3 0 128.57 6.14 -8 -3 0 0.05 1.30 -8 -3 0 4.57 1.76 8 3 0 3.77 1.66 -9 -3 0 39.66 4.13 -9 -3 0 31.33 3.47 9 3 0 32.38 3.93 -10 -3 0 4.14 2.14 10 3 0 1.27 1.79 -11 -3 0 3.66 2.23 11 3 0 1.02 1.90 11 -4 0 2.13 2.05 -11 4 0 4.42 2.36 10 -4 0 48.41 5.07 -10 4 0 41.90 4.73 9 -4 0 44.80 4.69 -9 4 0 37.60 4.21 8 -4 0 55.50 3.97 8 -4 0 59.50 4.30 -8 4 0 60.36 4.49 7 -4 0 8.32 1.98 7 -4 0 13.50 2.32 -7 4 0 8.60 2.04 6 -4 0 1.72 1.28 6 -4 0 1.35 1.07 6 -4 0 0.48 1.25 -6 4 0 0.57 1.09 5 -4 0 -0.54 0.88 5 -4 0 -2.06 0.93 5 -4 0 0.46 1.07 -5 4 0 0.42 1.00 4 -4 0 1.03 1.16 -4 4 0 0.19 0.89 -4 4 0 0.61 0.91 3 -4 0 19.26 1.97 -3 4 0 18.12 1.85 -3 4 0 16.61 1.77 2 -4 0 127.18 4.85 2 -4 0 130.57 3.95 -2 4 0 129.67 4.66 -2 4 0 128.66 4.79 1 -4 0 134.56 4.36 1 -4 0 134.59 4.80 -1 4 0 139.36 4.66 -1 4 0 130.10 4.67 0 -4 0 3.95 1.01 0 -4 0 3.19 1.04 0 4 0 3.71 0.94 -1 -4 0 153.08 5.34 -1 -4 0 137.25 4.72 1 4 0 152.07 5.19 1 4 0 157.00 5.04 -2 -4 0 82.48 2.89 -2 -4 0 88.64 3.92 2 4 0 86.78 3.70 -3 -4 0 1.07 0.84 -3 -4 0 2.47 1.20 3 4 0 2.52 1.07 -4 -4 0 14.32 1.96 -4 -4 0 18.21 1.86 4 4 0 15.41 2.03 -5 -4 0 22.81 2.46 -5 -4 0 20.83 2.24 5 4 0 20.62 2.46 -6 -4 0 72.92 4.02 -6 -4 0 67.52 4.11 6 4 0 73.33 4.35 -7 -4 0 22.81 2.82 -7 -4 0 27.55 3.06 7 4 0 19.96 2.90 -8 -4 0 24.69 3.03 -8 -4 0 18.16 2.80 8 4 0 21.85 3.23 -9 -4 0 21.33 3.18 -9 -4 0 21.99 3.20 9 4 0 21.01 3.29 -10 -4 0 5.73 2.37 10 4 0 1.63 1.85 -11 -4 0 -1.25 1.76 11 4 0 -0.54 1.70 11 -5 0 5.63 2.46 -11 5 0 5.59 2.74 10 -5 0 57.24 5.55 -10 5 0 63.39 5.81 9 -5 0 47.15 4.81 9 -5 0 48.65 4.35 -9 5 0 47.14 4.70 8 -5 0 46.77 3.91 8 -5 0 51.50 3.93 -8 5 0 48.44 4.62 7 -5 0 21.82 2.85 7 -5 0 16.19 2.56 7 -5 0 15.38 2.35 -7 5 0 15.75 2.56 6 -5 0 20.66 2.61 6 -5 0 22.49 2.69 6 -5 0 21.75 2.45 -6 5 0 19.61 2.56 5 -5 0 5.42 1.58 -5 5 0 5.19 1.46 4 -5 0 80.90 4.19 -4 5 0 82.44 3.84 -4 5 0 79.99 4.05 3 -5 0 1.69 1.19 -3 5 0 0.02 0.88 -3 5 0 0.29 0.89 2 -5 0 77.19 2.85 2 -5 0 84.83 3.82 -2 5 0 78.36 3.51 -2 5 0 79.99 3.44 1 -5 0 181.60 6.22 1 -5 0 177.99 5.76 -1 5 0 185.76 6.12 -1 5 0 178.01 6.16 0 -5 0 92.80 3.81 0 -5 0 94.70 3.81 0 5 0 103.13 3.85 0 5 0 89.18 3.79 -1 -5 0 31.57 2.50 -1 -5 0 33.92 2.13 1 5 0 37.15 2.28 1 5 0 32.53 2.11 -2 -5 0 180.79 6.46 -2 -5 0 176.51 5.47 2 5 0 180.46 6.39 2 5 0 172.46 6.07 -3 -5 0 1.75 0.88 -3 -5 0 2.64 1.28 -3 -5 0 2.20 0.64 3 5 0 1.27 1.01 -4 -5 0 47.45 3.34 -4 -5 0 48.31 2.87 4 5 0 51.99 3.36 -5 -5 0 32.88 2.59 -5 -5 0 38.78 3.17 5 5 0 34.89 3.00 -6 -5 0 56.01 3.94 -6 -5 0 47.90 3.32 6 5 0 49.60 3.69 -7 -5 0 32.29 3.32 -7 -5 0 26.77 3.15 7 5 0 23.45 3.15 -8 -5 0 57.70 4.26 -8 -5 0 49.04 3.96 8 5 0 56.23 4.39 -9 -5 0 7.68 2.35 -9 -5 0 6.46 2.07 9 5 0 4.57 2.00 -10 -5 0 6.14 2.34 -10 -5 0 4.31 2.11 10 5 0 2.44 1.99 -11 -5 0 1.48 2.07 11 -6 0 8.82 2.83 -11 6 0 11.82 3.32 10 -6 0 11.83 2.96 -10 6 0 11.22 3.09 9 -6 0 38.04 4.26 9 -6 0 32.30 3.77 -9 6 0 34.24 4.17 8 -6 0 60.48 4.45 8 -6 0 65.02 4.58 -8 6 0 55.52 4.38 7 -6 0 26.88 2.90 7 -6 0 31.35 3.46 7 -6 0 23.79 3.04 -7 6 0 28.92 3.40 6 -6 0 11.16 1.91 6 -6 0 15.48 2.50 6 -6 0 12.91 2.19 -6 6 0 15.11 2.43 5 -6 0 -1.13 1.27 -5 6 0 -0.96 0.99 -5 6 0 1.15 1.11 4 -6 0 17.77 2.37 -4 6 0 19.44 2.16 -4 6 0 18.54 2.19 3 -6 0 129.81 5.54 3 -6 0 135.09 4.23 -3 6 0 134.49 5.49 -3 6 0 136.41 5.25 2 -6 0 85.08 3.26 2 -6 0 91.38 4.23 -2 6 0 87.87 3.82 -2 6 0 87.14 3.92 1 -6 0 31.25 2.12 1 -6 0 29.37 2.47 -1 6 0 31.39 2.32 -1 6 0 32.11 2.19 0 -6 0 49.05 2.85 0 -6 0 52.16 2.87 0 6 0 49.92 2.76 0 6 0 50.48 2.79 -1 -6 0 405.55 12.25 -1 -6 0 398.42 11.61 1 6 0 381.07 11.98 1 6 0 398.02 12.32 -2 -6 0 0.15 1.17 -2 -6 0 2.13 0.91 2 6 0 0.67 0.99 2 6 0 0.80 0.91 -3 -6 0 54.74 2.28 -3 -6 0 54.87 3.53 3 6 0 54.66 3.26 3 6 0 53.82 3.05 -4 -6 0 12.93 1.80 -4 -6 0 13.01 2.15 4 6 0 11.90 1.99 -5 -6 0 71.42 4.44 -5 -6 0 74.18 4.09 5 6 0 89.33 4.70 -6 -6 0 33.05 3.49 -6 -6 0 29.86 2.98 6 6 0 31.26 3.40 -7 -6 0 48.92 3.94 -7 -6 0 43.88 3.51 7 6 0 39.27 4.01 -8 -6 0 49.94 3.93 -8 -6 0 44.28 4.33 8 6 0 41.77 4.47 -9 -6 0 16.96 3.06 -9 -6 0 12.21 2.65 9 6 0 10.01 2.59 -10 -6 0 0.08 1.99 -10 -6 0 -1.63 1.61 10 6 0 -3.07 1.48 -11 -6 0 2.18 2.12 11 -7 0 0.79 2.04 10 -7 0 25.03 3.83 10 -7 0 20.70 3.43 -10 7 0 25.83 4.10 9 -7 0 55.57 4.96 9 -7 0 53.30 4.49 -9 7 0 42.18 4.72 8 -7 0 8.00 2.04 8 -7 0 1.32 1.75 8 -7 0 5.00 2.17 -8 7 0 5.23 2.21 7 -7 0 49.47 3.99 7 -7 0 53.33 3.69 7 -7 0 59.84 4.38 -7 7 0 51.90 4.23 6 -7 0 19.80 2.84 -6 7 0 20.87 2.86 5 -7 0 26.98 3.11 -5 7 0 24.09 2.68 -5 7 0 21.92 2.63 4 -7 0 59.72 3.95 -4 7 0 62.68 3.53 -4 7 0 66.97 3.88 3 -7 0 39.94 1.93 3 -7 0 35.39 3.08 -3 7 0 36.50 2.55 -3 7 0 37.10 2.88 2 -7 0 66.96 3.90 2 -7 0 73.85 3.09 -2 7 0 75.45 3.79 -2 7 0 73.47 3.57 1 -7 0 369.24 11.19 1 -7 0 359.52 11.59 -1 7 0 375.47 11.69 -1 7 0 372.83 11.70 0 -7 0 44.88 2.89 0 -7 0 43.90 2.82 0 7 0 43.58 2.74 0 7 0 50.56 2.91 -1 -7 0 -1.04 1.02 -1 -7 0 2.72 1.13 1 7 0 0.92 1.04 1 7 0 0.93 0.99 -2 -7 0 9.76 1.75 -2 -7 0 9.68 1.34 2 7 0 8.69 1.47 2 7 0 12.54 1.85 -3 -7 0 -0.01 0.76 -3 -7 0 1.19 1.34 3 7 0 0.03 1.01 3 7 0 0.30 1.09 -4 -7 0 85.08 4.69 4 7 0 80.11 4.12 4 7 0 83.53 4.55 -5 -7 0 131.31 5.85 -5 -7 0 133.17 6.25 5 7 0 124.32 6.18 -6 -7 0 44.73 3.51 -6 -7 0 44.35 4.08 6 7 0 44.36 4.27 -7 -7 0 84.91 5.35 -7 -7 0 95.58 5.20 7 7 0 89.44 5.56 -8 -7 0 78.41 5.33 -8 -7 0 72.58 4.80 8 7 0 76.46 5.40 -9 -7 0 -0.40 1.52 -9 -7 0 -0.08 2.08 9 7 0 1.15 1.77 -10 -7 0 2.95 2.11 -10 -7 0 2.41 2.29 10 7 0 0.11 2.07 11 -8 0 13.79 3.48 10 -8 0 23.19 3.70 10 -8 0 28.45 3.96 -10 8 0 23.86 4.15 9 -8 0 37.32 4.30 9 -8 0 43.57 4.63 -9 8 0 41.08 4.68 8 -8 0 77.56 5.35 8 -8 0 81.65 5.26 8 -8 0 77.93 4.71 -8 8 0 74.23 5.42 7 -8 0 12.26 2.24 7 -8 0 15.15 2.63 7 -8 0 15.41 2.89 -7 8 0 15.47 2.74 6 -8 0 0.09 1.58 -6 8 0 3.22 1.76 -6 8 0 1.65 1.65 5 -8 0 3.30 1.77 -5 8 0 -1.01 1.38 -5 8 0 0.48 1.26 4 -8 0 83.87 4.79 -4 8 0 73.66 4.37 -4 8 0 84.46 4.25 3 -8 0 231.22 8.47 -3 8 0 214.44 8.22 -3 8 0 222.86 8.03 2 -8 0 38.87 2.33 2 -8 0 39.79 3.14 -2 8 0 36.78 2.89 -2 8 0 32.74 2.53 1 -8 0 11.50 1.64 1 -8 0 13.57 1.99 -1 8 0 13.47 1.83 -1 8 0 11.61 1.74 0 -8 0 124.63 5.11 0 -8 0 119.93 5.10 0 8 0 119.35 5.10 0 8 0 124.70 5.16 -1 -8 0 47.10 2.90 -1 -8 0 47.71 3.32 1 8 0 54.84 3.23 1 8 0 45.88 3.06 -2 -8 0 17.61 1.84 -2 -8 0 18.70 2.37 2 8 0 23.29 2.53 2 8 0 18.46 2.10 -3 -8 0 78.85 4.54 -3 -8 0 79.11 3.36 3 8 0 90.20 4.21 3 8 0 85.54 4.46 -4 -8 0 17.03 2.51 4 8 0 21.44 2.45 4 8 0 19.26 2.62 -5 -8 0 77.25 4.88 5 8 0 73.14 4.74 5 8 0 91.23 4.60 -6 -8 0 83.83 5.20 6 8 0 73.14 5.00 -7 -8 0 31.20 3.74 -7 -8 0 21.62 2.94 7 8 0 17.49 3.06 -8 -8 0 9.20 2.70 -8 -8 0 7.50 2.22 8 8 0 13.84 3.06 -9 -8 0 3.12 2.39 -9 -8 0 0.35 1.71 9 8 0 2.29 2.03 -10 -8 0 10.34 2.89 10 -9 0 36.94 4.65 10 -9 0 32.58 4.41 -10 9 0 36.63 4.73 9 -9 0 46.07 4.89 9 -9 0 48.80 4.90 -9 9 0 43.50 4.91 8 -9 0 41.20 4.45 8 -9 0 52.32 4.43 8 -9 0 43.51 4.67 -8 9 0 43.65 4.77 7 -9 0 40.90 3.77 7 -9 0 41.20 4.35 7 -9 0 36.03 3.86 -7 9 0 42.76 4.44 6 -9 0 0.31 1.90 -6 9 0 5.89 2.19 -6 9 0 8.01 2.05 5 -9 0 44.90 4.27 -5 9 0 42.18 3.32 -5 9 0 46.04 3.77 4 -9 0 23.67 3.11 -4 9 0 23.58 2.68 -4 9 0 19.93 2.69 3 -9 0 38.99 2.30 3 -9 0 39.72 3.69 -3 9 0 41.84 3.01 -3 9 0 37.79 3.18 2 -9 0 95.12 4.84 2 -9 0 89.74 3.92 -2 9 0 88.84 4.52 -2 9 0 87.29 4.36 1 -9 0 79.59 4.39 1 -9 0 79.45 3.95 -1 9 0 90.47 4.24 -1 9 0 76.27 4.07 0 -9 0 34.07 2.77 0 -9 0 34.73 2.98 0 9 0 30.92 2.63 0 9 0 32.73 2.75 -1 -9 0 4.90 1.45 -1 -9 0 5.48 1.63 1 9 0 4.39 1.41 1 9 0 3.19 1.44 -2 -9 0 4.34 1.61 -2 -9 0 -0.12 1.14 2 9 0 1.62 1.24 2 9 0 1.27 1.30 -3 -9 0 1.26 1.60 3 9 0 0.02 1.11 3 9 0 -0.58 1.26 -4 -9 0 16.64 2.73 4 9 0 16.38 2.27 4 9 0 14.90 2.41 -5 -9 0 37.20 3.89 5 9 0 36.16 3.89 5 9 0 29.22 3.04 -6 -9 0 19.55 3.11 6 9 0 20.92 2.86 6 9 0 21.03 3.14 -7 -9 0 18.08 3.15 7 9 0 16.33 2.75 7 9 0 17.45 3.10 -8 -9 0 19.38 3.39 8 9 0 31.03 3.69 8 9 0 21.09 3.51 -9 -9 0 0.14 2.19 9 9 0 1.66 2.25 10 -10 0 12.41 3.18 9 -10 0 56.83 5.66 9 -10 0 62.78 4.69 9 -10 0 67.36 5.24 -9 10 0 57.08 5.69 8 -10 0 15.04 3.32 8 -10 0 14.04 2.59 8 -10 0 9.99 2.56 -8 10 0 22.96 3.62 7 -10 0 1.89 2.15 -7 10 0 3.69 2.26 6 -10 0 9.42 2.61 -6 10 0 14.08 2.79 -6 10 0 9.68 2.34 5 -10 0 2.96 2.06 -5 10 0 4.17 2.02 -5 10 0 4.91 1.88 4 -10 0 57.70 4.43 -4 10 0 56.02 4.04 -4 10 0 50.17 3.69 3 -10 0 61.55 4.42 -3 10 0 61.89 4.00 -3 10 0 68.34 4.00 2 -10 0 30.32 3.27 2 -10 0 30.81 2.52 -2 10 0 32.58 3.03 -2 10 0 26.69 2.87 1 -10 0 63.04 3.67 1 -10 0 63.27 4.07 -1 10 0 65.10 3.89 -1 10 0 63.63 3.92 0 -10 0 143.79 6.04 0 -10 0 136.97 6.00 0 10 0 142.24 6.11 0 10 0 146.84 6.21 -1 -10 0 6.96 1.73 -1 -10 0 8.38 2.02 1 10 0 7.14 1.69 1 10 0 7.32 1.83 -2 -10 0 0.78 1.20 -2 -10 0 2.03 1.71 2 10 0 2.17 1.43 2 10 0 2.53 1.57 -3 -10 0 -1.16 1.59 3 10 0 0.91 1.33 3 10 0 -0.17 1.34 -4 -10 0 7.72 2.42 4 10 0 9.22 2.29 4 10 0 15.02 2.30 -5 -10 0 42.25 4.33 5 10 0 37.66 3.54 5 10 0 36.42 3.90 -6 -10 0 50.96 4.86 6 10 0 57.21 4.59 6 10 0 58.59 4.17 -7 -10 0 15.61 3.14 7 10 0 23.28 3.59 7 10 0 25.08 3.32 -8 -10 0 5.88 2.47 8 10 0 2.74 2.26 -9 -10 0 0.65 2.39 9 10 0 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3.99 -1 0 17 31.52 3.93 0 0 -17 15.88 3.06 0 0 17 23.83 3.64 -1 0 -17 30.52 3.97 1 0 17 27.85 3.87 -2 0 -17 40.55 4.53 2 0 17 45.70 4.81 -3 0 -17 7.48 2.88 3 0 17 16.73 3.43 -4 0 -17 1.70 2.62 4 0 17 2.69 2.52 7 -1 -17 16.01 3.06 -7 1 17 13.43 3.26 6 -1 -17 18.25 3.37 -6 1 17 17.15 3.46 5 -1 -17 46.41 4.74 -5 1 17 44.75 4.76 -4 1 17 10.27 2.67 3 -1 -17 4.78 2.25 -3 1 17 2.19 2.21 2 -1 -17 35.10 4.04 -2 1 17 32.75 4.16 1 -1 -17 18.36 3.33 -1 1 17 18.39 3.39 0 -1 -17 25.35 3.70 0 1 17 23.30 3.70 -1 -1 -17 44.44 4.86 1 1 17 50.79 5.09 -2 -1 -17 11.22 3.08 2 1 17 4.63 2.58 -3 -1 -17 6.29 2.93 3 1 17 16.84 3.40 4 1 17 5.15 2.69 7 -2 -17 21.69 3.71 -7 2 17 29.58 4.34 6 -2 -17 24.01 3.80 -6 2 17 22.51 3.76 5 -2 -17 4.99 2.54 -5 2 17 3.69 2.46 4 -2 -17 -1.30 1.97 -4 2 17 -0.25 1.87 3 -2 -17 1.82 2.03 -3 2 17 1.55 2.18 -3 2 17 -3.83 1.79 2 -2 -17 9.98 2.64 -2 2 17 10.31 2.90 -2 2 17 1.89 2.18 1 -2 -17 51.79 4.95 -1 2 17 56.12 4.83 -1 2 17 61.51 5.05 0 -2 -17 17.76 3.34 0 2 17 14.94 3.17 -1 -2 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4 17 1.87 2.39 -5 5 17 6.40 2.89 4 -5 -17 0.46 2.23 -4 5 17 0.05 2.29 3 -5 -17 -0.85 2.17 -3 5 17 0.48 2.28 2 -5 -17 9.91 2.92 -2 5 17 12.08 3.55 1 -5 -17 23.48 3.72 -1 5 17 21.29 3.73 0 -5 -17 34.84 4.38 0 5 17 23.40 3.96 -1 -5 -17 15.29 3.50 1 5 17 12.94 3.26 1 5 17 14.19 3.26 2 5 17 8.95 2.99 2 5 17 5.72 2.77 3 5 17 12.79 3.52 -4 6 17 2.05 2.47 -3 6 17 -0.48 2.17 2 -6 -17 3.81 2.40 -2 6 17 4.94 2.86 1 -6 -17 22.02 3.73 1 -6 -17 19.99 3.65 -1 6 17 18.31 3.79 0 -6 -17 19.43 3.68 0 -6 -17 25.76 4.06 0 6 17 16.11 3.64 -1 -6 -17 27.40 4.22 1 6 17 20.34 3.89 0 -7 -17 10.18 3.26 1 12 -18 2.79 2.91 3 11 -18 4.00 2.85 2 11 -18 9.55 3.25 -1 -11 18 10.35 3.09 0 -11 18 14.19 3.52 4 10 -18 0.28 2.54 -2 -10 18 49.66 5.16 -1 -10 18 32.58 4.29 0 -10 18 9.44 3.08 5 9 -18 2.99 2.56 2 9 -18 12.27 3.51 -2 -9 18 11.66 3.20 1 9 -18 4.54 2.59 -1 -9 18 3.31 2.59 0 9 -18 10.84 3.01 0 -9 18 21.39 3.77 -1 9 -18 6.96 2.77 1 -9 18 9.35 3.03 6 8 -18 11.63 3.16 -5 -8 18 4.33 2.68 3 8 -18 3.09 2.66 -3 -8 18 -0.42 2.23 2 8 -18 10.32 3.20 -2 -8 18 4.73 2.52 1 8 -18 12.67 3.30 -1 -8 18 12.21 3.20 0 8 -18 30.73 4.30 0 -8 18 28.14 4.23 -1 8 -18 12.50 3.23 1 -8 18 12.36 3.32 -2 8 -18 6.54 2.73 2 -8 18 2.47 2.57 -6 -7 18 9.69 3.12 4 7 -18 1.93 2.65 3 7 -18 7.26 2.99 -3 -7 18 13.49 3.05 2 7 -18 15.89 3.37 -2 -7 18 15.52 3.18 1 7 -18 16.50 3.47 -1 -7 18 12.78 3.38 0 7 -18 34.80 4.42 0 -7 18 31.44 4.39 -1 7 -18 8.89 2.98 1 -7 18 12.62 3.18 -2 7 -18 -1.63 1.97 2 -7 18 -1.65 2.10 5 6 -18 3.28 2.87 4 6 -18 -1.77 2.27 -4 -6 18 1.83 2.20 3 6 -18 26.09 4.01 -3 -6 18 33.90 4.30 2 6 -18 6.65 2.68 -2 -6 18 7.52 2.82 1 6 -18 65.46 5.40 -1 -6 18 66.24 5.35 0 6 -18 41.49 4.69 0 -6 18 27.66 4.11 -1 6 -18 7.47 2.82 1 -6 18 8.31 2.84 -2 6 -18 7.20 2.77 2 -6 18 7.62 2.75 -3 6 -18 -0.41 2.27 6 5 -18 5.75 2.90 5 5 -18 0.24 2.31 4 5 -18 -0.81 2.27 -4 -5 18 -1.49 2.04 3 5 -18 38.90 4.64 -3 -5 18 34.24 4.25 2 5 -18 27.79 3.94 -2 -5 18 26.27 4.02 1 5 -18 49.29 5.02 -1 -5 18 39.93 4.66 0 5 -18 53.20 5.15 0 -5 18 53.01 5.36 -1 5 -18 28.74 4.03 1 -5 18 25.67 3.98 -2 5 -18 6.89 2.60 2 -5 18 1.76 2.52 -3 5 -18 2.29 2.26 3 -5 18 -2.75 1.95 6 4 -18 19.89 3.55 5 4 -18 -1.67 2.07 -5 -4 18 0.59 2.22 4 4 -18 5.32 2.68 -4 -4 18 7.24 2.74 3 4 -18 4.10 2.52 -3 -4 18 7.01 2.66 2 4 -18 39.05 4.36 -2 -4 18 38.72 4.58 1 4 -18 57.28 5.25 -1 -4 18 47.07 5.00 0 4 -18 27.81 3.91 0 -4 18 37.00 4.55 -1 4 -18 -0.42 2.17 1 -4 18 8.26 2.78 -2 4 -18 3.47 2.36 2 -4 18 9.12 2.95 -3 4 -18 -1.25 2.01 3 -4 18 -0.93 2.10 5 3 -18 2.83 2.41 -5 -3 18 6.38 2.56 4 3 -18 1.06 2.15 -4 -3 18 0.23 2.17 3 3 -18 33.55 4.20 -3 -3 18 33.22 4.26 2 3 -18 48.99 4.89 -2 -3 18 33.70 4.18 1 3 -18 24.87 3.75 -1 -3 18 20.37 3.55 0 3 -18 22.26 3.63 0 -3 18 27.92 4.03 -1 3 -18 5.71 2.63 1 -3 18 7.75 2.84 -2 3 -18 0.58 2.03 2 -3 18 0.42 2.24 -3 3 -18 -0.96 2.02 3 -3 18 0.01 2.34 5 2 -18 0.23 2.08 -5 -2 18 0.08 2.16 4 2 -18 3.83 2.34 -4 -2 18 4.13 2.44 3 2 -18 22.47 3.58 -3 -2 18 14.96 3.22 2 2 -18 27.11 3.86 -2 -2 18 24.08 3.85 1 2 -18 36.41 4.30 -1 -2 18 24.21 3.74 0 2 -18 16.87 3.24 0 -2 18 23.20 3.70 -1 2 -18 9.77 3.02 1 -2 18 12.01 3.13 -2 2 -18 -0.47 1.99 2 -2 18 -1.68 1.94 -3 2 -18 2.82 2.47 3 -2 18 5.39 2.70 6 1 -18 5.59 2.45 4 1 -18 5.62 2.44 -4 -1 18 3.95 2.38 3 1 -18 13.55 3.06 -3 -1 18 13.45 3.01 2 1 -18 33.26 4.14 -2 -1 18 27.67 3.96 1 1 -18 29.84 4.01 -1 -1 18 26.97 4.03 0 1 -18 12.27 3.04 0 -1 18 11.21 2.94 -1 1 -18 14.11 3.27 1 -1 18 18.32 3.48 -2 1 -18 0.23 2.06 2 -1 18 4.20 2.48 3 -1 18 4.38 2.66 6 0 -18 0.38 2.02 4 0 -18 8.43 2.71 -4 0 18 7.70 2.74 3 0 -18 29.98 3.96 -3 0 18 20.18 3.65 2 0 -18 31.22 4.03 -2 0 18 28.95 4.04 1 0 -18 5.69 2.64 -1 0 18 3.03 2.49 0 0 -18 11.87 3.13 0 0 18 7.38 2.68 -1 0 -18 5.94 2.80 1 0 18 7.81 2.63 -2 0 -18 1.53 2.33 2 0 18 2.91 2.55 3 0 18 7.72 3.00 7 -1 -18 6.01 2.62 6 -1 -18 0.64 2.27 5 -1 -18 3.77 2.43 3 -1 -18 14.54 3.13 -3 1 18 16.88 3.35 2 -1 -18 12.91 3.12 -2 1 18 10.61 2.98 1 -1 -18 3.31 2.44 -1 1 18 5.26 2.53 0 -1 -18 4.60 2.54 0 1 18 6.83 2.73 -1 -1 -18 6.41 2.83 1 1 18 5.95 2.71 -2 -1 -18 -0.34 2.32 2 1 18 -1.93 2.16 6 -2 -18 -0.30 2.17 -6 2 18 0.98 2.24 5 -2 -18 12.74 3.15 -5 2 18 9.97 3.06 4 -2 -18 18.55 3.57 3 -2 -18 20.06 3.38 -3 2 18 15.94 3.38 2 -2 -18 4.59 2.61 -2 2 18 11.23 2.97 1 -2 -18 30.17 4.20 -1 2 18 36.09 4.58 0 -2 -18 7.09 2.83 0 2 18 5.06 2.50 -1 -2 -18 -3.27 2.08 1 2 18 1.48 2.29 2 2 18 -2.00 2.13 -6 3 18 4.78 2.86 5 -3 -18 10.80 3.16 -5 3 18 5.95 2.94 4 -3 -18 11.28 3.04 -4 3 18 7.89 2.82 3 -3 -18 33.84 4.28 -3 3 18 17.44 3.52 2 -3 -18 19.45 3.56 -2 3 18 17.92 3.56 -2 3 18 26.97 4.09 1 -3 -18 20.98 3.71 -1 3 18 13.48 3.26 0 -3 -18 3.30 2.67 0 3 18 6.11 2.70 -1 -3 -18 -2.12 2.36 1 3 18 3.25 2.50 -5 4 18 8.48 3.09 -4 4 18 19.01 3.77 3 -4 -18 22.29 3.76 -3 4 18 16.54 3.61 2 -4 -18 13.47 3.23 -2 4 18 12.08 3.35 1 -4 -18 39.36 4.72 -1 4 18 39.89 5.01 0 -4 -18 19.63 3.69 0 4 18 14.74 3.45 0 4 18 14.81 3.40 -1 -4 -18 -4.32 2.32 -4 5 18 20.25 3.94 -3 5 18 19.67 4.00 -2 5 18 17.41 3.73 1 -5 -18 17.48 3.55 -1 5 18 7.20 2.83 0 -5 -18 10.40 3.35 0 5 18 9.41 3.25 1 5 18 -0.17 2.27 -2 -10 19 9.93 3.17 -2 -9 19 23.40 3.87 -1 -9 19 6.86 2.92 -3 -8 19 6.98 2.90 -2 -8 19 19.16 3.68 -1 -8 19 7.40 3.03 0 -8 19 3.19 2.54 4 7 -19 14.43 3.61 3 7 -19 13.78 3.55 -3 -7 19 10.57 3.06 2 7 -19 9.98 3.23 -2 -7 19 14.43 3.44 1 7 -19 6.67 2.93 -1 -7 19 9.11 3.02 0 7 -19 -2.49 2.00 0 -7 19 -0.83 2.47 5 6 -19 14.59 3.64 4 6 -19 21.96 4.00 -4 -6 19 11.77 3.04 3 6 -19 39.97 4.88 -3 -6 19 32.67 4.27 2 6 -19 7.24 2.74 -2 -6 19 1.87 2.46 1 6 -19 10.72 3.03 -1 -6 19 12.37 3.31 0 6 -19 -0.56 2.25 0 -6 19 0.01 2.21 1 -6 19 6.82 2.99 6 5 -19 23.58 4.22 5 5 -19 35.37 4.74 4 5 -19 22.70 3.88 -4 -5 19 22.66 3.81 3 5 -19 18.72 3.60 -3 -5 19 16.02 3.33 2 5 -19 22.20 3.74 -2 -5 19 25.44 3.99 1 5 -19 5.82 2.83 -1 -5 19 8.13 2.95 0 5 -19 2.69 2.46 0 -5 19 1.25 2.39 -1 5 -19 18.77 3.71 1 -5 19 16.77 3.68 5 4 -19 22.47 3.90 4 4 -19 20.78 3.69 -4 -4 19 8.21 2.81 3 4 -19 37.14 4.62 -3 -4 19 36.25 4.54 2 4 -19 8.52 2.94 -2 -4 19 6.57 2.78 1 4 -19 -0.59 2.15 -1 -4 19 -0.53 2.20 0 4 -19 1.77 2.32 0 -4 19 1.94 2.36 -1 4 -19 0.37 2.23 1 -4 19 -4.24 1.94 5 3 -19 35.07 4.47 -5 -3 19 27.25 4.16 4 3 -19 10.51 3.13 -4 -3 19 12.34 3.31 3 3 -19 22.81 3.82 -3 -3 19 15.43 3.39 2 3 -19 24.73 3.85 -2 -3 19 17.14 3.51 1 3 -19 4.86 2.55 -1 -3 19 6.63 2.76 0 3 -19 1.53 2.49 0 -3 19 3.66 2.56 -1 3 -19 3.98 2.44 1 -3 19 8.91 2.99 -5 -2 19 17.12 3.55 4 2 -19 34.73 4.39 -4 -2 19 34.42 4.51 3 2 -19 12.21 3.16 -3 -2 19 14.38 3.37 2 2 -19 1.66 2.48 -2 -2 19 0.97 2.30 1 2 -19 -1.52 2.37 -1 -2 19 0.58 2.21 0 2 -19 -2.34 2.09 0 -2 19 -0.90 2.18 -1 2 -19 6.78 2.82 1 -2 19 6.74 2.77 6 1 -19 16.67 3.40 4 1 -19 23.13 3.79 -4 -1 19 18.25 3.53 3 1 -19 18.98 3.55 -3 -1 19 24.70 3.94 2 1 -19 9.85 2.93 -2 -1 19 10.68 3.02 1 1 -19 -0.29 2.20 -1 -1 19 -1.40 2.18 0 1 -19 7.62 2.82 0 -1 19 4.23 2.61 -1 1 -19 0.76 2.39 1 -1 19 5.48 2.74 5 0 -19 22.74 3.74 -4 0 19 33.42 4.48 3 0 -19 4.27 2.63 -3 0 19 2.87 2.52 2 0 -19 1.00 2.34 -2 0 19 -0.58 2.25 1 0 -19 -1.91 2.35 -1 0 19 -0.56 2.15 0 0 -19 -0.82 2.32 0 0 19 2.45 2.39 -1 0 -19 19.68 3.80 3 -1 -19 4.89 2.60 -3 1 19 3.84 2.45 2 -1 -19 1.44 2.49 -2 1 19 -0.33 2.26 1 -1 -19 1.21 2.53 -1 1 19 -0.71 2.14 0 -1 -19 -2.72 2.11 2 -2 -19 1.58 2.54 1 -2 -19 1.16 2.49 0 -2 -19 6.62 2.90 2 -3 -19 -0.49 2.32 1 -3 -19 3.14 2.63 -3 4 19 9.74 3.21 1 -4 -19 11.85 3.36 -3 -7 20 0.50 2.53 -3 -6 20 0.85 2.39 -4 -5 20 1.72 2.39 -3 -5 20 1.90 2.65 -4 -4 20 2.29 2.47 3 4 -20 2.08 2.62 -3 -4 20 1.60 2.66 2 4 -20 11.79 3.27 -2 -4 20 11.48 3.39 4 3 -20 2.08 2.55 -4 -3 20 6.11 2.76 3 3 -20 1.56 2.45 -3 -3 20 -1.06 2.27 2 3 -20 18.28 3.84 4 2 -20 -0.62 2.41 3 2 -20 0.23 2.51 2 2 -20 19.45 3.70 4 1 -20 5.79 2.85 3 1 -20 11.67 3.19 2 1 -20 41.21 4.91 3 0 -20 8.02 2.95 2 0 -20 11.10 3.21 2 -1 -20 19.89 3.85 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 7352 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969305' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_6 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 N3 O7 Tb' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 876.86 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 '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 8.684(5) _cell_length_b 13.130(5) _cell_length_c 14.770(5) _cell_angle_alpha 100.221(5) _cell_angle_beta 97.912(5) _cell_angle_gamma 92.257(5) _cell_volume 1638.1(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 44103 _cell_measurement_theta_min 4.746 _cell_measurement_theta_max 54.441 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.778 _exptl_crystal_F_000 868 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.09 _exptl_absorpt_coefficient_mu 2.460 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6053 _exptl_absorpt_correction_T_max 0.7459 _exptl_absorpt_process_details 'TWINABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 44101 _diffrn_reflns_av_unetI/netI 0.0520 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 1.416 _diffrn_reflns_theta_max 29.566 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8909 _reflns_number_gt 7553 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. 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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0381P)^2^+0.7663P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8909 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.56365(2) 0.51308(2) 0.70140(2) 0.01322(5) Uani 1 1 d . . . . . O6 O 0.8491(3) 0.58113(19) 0.50060(16) 0.0217(5) Uani 1 1 d . . . . . O4 O 0.4068(3) 0.34854(18) 0.66069(15) 0.0176(5) Uani 1 1 d . . . . . O1 O 0.7120(3) 0.62478(17) 0.84363(16) 0.0168(5) Uani 1 1 d . . . . . O3 O 0.5620(3) 0.37594(18) 0.56040(15) 0.0171(5) Uani 1 1 d . . . . . OW1 O 0.3681(3) 0.55931(18) 0.59170(16) 0.0163(5) Uani 1 1 d D . . . . O2 O 0.5378(3) 0.69773(18) 0.75653(16) 0.0178(5) Uani 1 1 d . . . . . C16 C 0.6418(4) 0.7034(2) 0.8252(2) 0.0167(6) Uani 1 1 d . . . . . N1 N 0.7943(3) 0.4039(2) 0.72676(18) 0.0148(5) Uani 1 1 d . . . . . O5 O 0.7312(3) 0.59523(18) 0.62743(16) 0.0192(5) Uani 1 1 d . . . . . C23 C 0.4608(4) 0.3191(2) 0.5864(2) 0.0149(6) Uani 1 1 d . . . . . N3 N 0.3395(3) 0.5379(2) 0.79712(18) 0.0147(5) Uani 1 1 d . . . . . C24 C 0.4059(4) 0.2155(2) 0.5275(2) 0.0161(6) Uani 1 1 d . . . . . N2 N 0.5710(3) 0.4139(2) 0.83788(18) 0.0138(5) Uani 1 1 d . . . . . C17 C 0.6841(4) 0.8072(3) 0.8867(2) 0.0191(7) Uani 1 1 d . . . . . C14 C 0.1016(4) 0.6169(3) 0.8226(2) 0.0214(7) Uani 1 1 d . . . . . H14 H 0.0248 0.6596 0.8044 0.026 Uiso 1 1 calc R U . . . C1 C 0.9057(4) 0.4030(3) 0.6721(2) 0.0168(6) Uani 1 1 d . . . . . H1 H 0.8922 0.4397 0.6235 0.020 Uiso 1 1 calc R U . . . C10 C 0.4498(4) 0.4154(2) 0.8864(2) 0.0154(6) Uani 1 1 d . . . . . C32 C 0.8742(4) 0.7965(3) 0.6899(2) 0.0190(7) Uani 1 1 d . . . . . H32 H 0.7823 0.7813 0.7120 0.023 Uiso 1 1 calc R U . . . C5 C 0.8106(4) 0.3477(2) 0.7949(2) 0.0153(6) Uani 1 1 d . . . . . C12 C 0.2073(4) 0.5033(3) 0.9212(2) 0.0191(7) Uani 1 1 d . . . . . H12 H 0.2042 0.4709 0.9721 0.023 Uiso 1 1 calc R U . . . C13 C 0.0915(4) 0.5673(3) 0.8970(2) 0.0217(7) Uani 1 1 d . . . . . H13 H 0.0081 0.5768 0.9302 0.026 Uiso 1 1 calc R U . . . C15 C 0.2283(4) 0.6014(3) 0.7764(2) 0.0172(6) Uani 1 1 d . . . . . H15 H 0.2372 0.6369 0.7281 0.021 Uiso 1 1 calc R U . . . C6 C 0.6798(4) 0.3464(2) 0.8502(2) 0.0153(6) Uani 1 1 d . . . . . C30 C 0.8272(4) 0.6264(3) 0.5782(2) 0.0160(6) Uani 1 1 d . . . . . C31 C 0.9226(4) 0.7260(3) 0.6197(2) 0.0161(6) Uani 1 1 d . . . . . C18 C 0.8064(4) 0.8220(3) 0.9583(2) 0.0218(7) Uani 1 1 d . . . . . H18 H 0.8659 0.7666 0.9685 0.026 Uiso 1 1 calc R U . . . C19 C 0.8427(4) 0.9178(3) 1.0155(2) 0.0229(7) Uani 1 1 d . . . . . H19 H 0.9248 0.9272 1.0643 0.027 Uiso 1 1 calc R U . . . C20 C 0.7535(4) 0.9993(3) 0.9981(3) 0.0233(7) Uani 1 1 d . . . . . C4 C 0.9430(4) 0.2934(3) 0.8119(2) 0.0188(7) Uani 1 1 d . . . . . H4 H 0.9536 0.2560 0.8601 0.023 Uiso 1 1 calc R U . . . C21 C 0.6321(4) 0.9877(3) 0.9254(2) 0.0241(8) Uani 1 1 d . . . . . H21 H 0.5750 1.0438 0.9142 0.029 Uiso 1 1 calc R U . . . C9 C 0.4369(4) 0.3494(3) 0.9496(2) 0.0200(7) Uani 1 1 d . . . . . H9 H 0.3545 0.3531 0.9838 0.024 Uiso 1 1 calc R U . . . Cl1 Cl 0.79651(11) 1.12001(7) 1.07089(6) 0.02730(19) Uani 1 1 d . . . . . C11 C 0.3283(4) 0.4882(3) 0.8685(2) 0.0165(6) Uani 1 1 d . . . . . C36 C 1.0594(4) 0.7497(3) 0.5860(3) 0.0225(7) Uani 1 1 d . . . . . H36 H 1.0923 0.7037 0.5382 0.027 Uiso 1 1 calc R U . . . C7 C 0.6718(4) 0.2763(3) 0.9103(2) 0.0212(7) Uani 1 1 d . . . . . H7 H 0.7479 0.2291 0.9167 0.025 Uiso 1 1 calc R U . . . C25 C 0.4708(4) 0.1795(3) 0.4474(2) 0.0210(7) Uani 1 1 d . . . . . H25 H 0.5452 0.2212 0.4290 0.025 Uiso 1 1 calc R U . . . C27 C 0.3124(4) 0.0223(3) 0.4225(3) 0.0253(8) Uani 1 1 d . . . . . C26 C 0.4249(4) 0.0820(3) 0.3952(3) 0.0256(8) Uani 1 1 d . . . . . H26 H 0.4695 0.0573 0.3425 0.031 Uiso 1 1 calc R U . . . C3 C 1.0592(4) 0.2957(3) 0.7561(2) 0.0199(7) Uani 1 1 d . . . . . H3 H 1.1490 0.2608 0.7672 0.024 Uiso 1 1 calc R U . . . C35 C 1.1467(4) 0.8421(3) 0.6239(3) 0.0256(8) Uani 1 1 d . . . . . H35 H 1.2383 0.8580 0.6019 0.031 Uiso 1 1 calc R U . . . C22 C 0.5973(4) 0.8914(3) 0.8698(2) 0.0217(7) Uani 1 1 d . . . . . H22 H 0.5156 0.8822 0.8207 0.026 Uiso 1 1 calc R U . . . C8 C 0.5476(4) 0.2787(3) 0.9606(2) 0.0238(8) Uani 1 1 d . . . . . H8 H 0.5393 0.2329 1.0013 0.029 Uiso 1 1 calc R U . . . C33 C 0.9593(4) 0.8889(3) 0.7278(2) 0.0215(7) Uani 1 1 d . . . . . H33 H 0.9254 0.9359 0.7747 0.026 Uiso 1 1 calc R U . . . C28 C 0.2441(5) 0.0566(3) 0.5007(3) 0.0268(8) Uani 1 1 d . . . . . H28 H 0.1672 0.0153 0.5175 0.032 Uiso 1 1 calc R U . . . C2 C 1.0398(4) 0.3502(3) 0.6843(2) 0.0185(7) Uani 1 1 d . . . . . H2 H 1.1146 0.3516 0.6450 0.022 Uiso 1 1 calc R U . . . C29 C 0.2926(4) 0.1539(3) 0.5537(2) 0.0223(7) Uani 1 1 d . . . . . H29 H 0.2489 0.1777 0.6070 0.027 Uiso 1 1 calc R U . . . C34 C 1.0960(4) 0.9102(3) 0.6947(3) 0.0222(7) Uani 1 1 d . . . . . Cl3 Cl 1.20891(12) 1.02492(7) 0.74264(7) 0.0328(2) Uani 1 1 d . . . . . Cl2 Cl 0.24955(14) -0.09913(8) 0.35519(8) 0.0400(3) Uani 1 1 d . . . . . H37 H 0.293(4) 0.505(2) 0.560(3) 0.032(12) Uiso 1 1 d D . . . . H38 H 0.404(5) 0.597(3) 0.550(3) 0.042(13) Uiso 1 1 d 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 Tb1 0.01346(8) 0.01545(8) 0.01178(8) 0.00343(5) 0.00425(5) 0.00112(5) O6 0.0215(13) 0.0259(13) 0.0187(12) 0.0051(10) 0.0071(10) -0.0030(10) O4 0.0185(12) 0.0195(12) 0.0156(11) 0.0032(9) 0.0054(9) 0.0005(9) O1 0.0178(12) 0.0163(11) 0.0173(11) 0.0027(9) 0.0059(9) 0.0021(9) O3 0.0166(11) 0.0198(12) 0.0159(11) 0.0049(9) 0.0048(9) -0.0001(9) OW1 0.0158(11) 0.0199(12) 0.0148(11) 0.0063(9) 0.0038(9) 0.0007(9) O2 0.0169(12) 0.0208(12) 0.0168(11) 0.0046(9) 0.0043(9) 0.0014(9) C16 0.0196(16) 0.0151(15) 0.0175(16) 0.0022(12) 0.0115(13) 0.0007(12) N1 0.0161(13) 0.0155(13) 0.0127(13) 0.0025(10) 0.0023(10) -0.0001(10) O5 0.0201(12) 0.0217(12) 0.0180(12) 0.0055(10) 0.0090(9) -0.0014(9) C23 0.0144(15) 0.0166(16) 0.0146(15) 0.0063(12) -0.0005(12) 0.0037(12) N3 0.0162(13) 0.0147(13) 0.0141(13) 0.0034(10) 0.0042(10) 0.0009(10) C24 0.0174(16) 0.0146(15) 0.0160(15) 0.0027(12) 0.0004(12) 0.0039(12) N2 0.0140(13) 0.0132(13) 0.0141(13) 0.0003(10) 0.0047(10) 0.0002(10) C17 0.0205(17) 0.0214(17) 0.0157(16) 0.0009(13) 0.0081(13) -0.0027(13) C14 0.0179(17) 0.0232(18) 0.0226(17) 0.0027(14) 0.0022(14) 0.0046(13) C1 0.0172(16) 0.0182(16) 0.0168(15) 0.0043(13) 0.0070(13) 0.0011(12) C10 0.0190(16) 0.0156(15) 0.0123(14) 0.0027(12) 0.0047(12) -0.0005(12) C32 0.0183(16) 0.0211(17) 0.0202(16) 0.0089(13) 0.0055(13) 0.0018(13) C5 0.0155(15) 0.0156(15) 0.0142(15) 0.0014(12) 0.0027(12) 0.0012(12) C12 0.0213(17) 0.0202(17) 0.0180(16) 0.0042(13) 0.0100(13) 0.0003(13) C13 0.0195(17) 0.0216(17) 0.0260(18) 0.0021(14) 0.0127(14) 0.0028(13) C15 0.0186(16) 0.0199(16) 0.0133(15) 0.0033(12) 0.0025(12) 0.0023(13) C6 0.0160(15) 0.0177(16) 0.0127(14) 0.0015(12) 0.0049(12) 0.0025(12) C30 0.0133(15) 0.0203(16) 0.0166(15) 0.0079(13) 0.0028(12) 0.0029(12) C31 0.0168(16) 0.0198(16) 0.0135(15) 0.0091(12) 0.0010(12) 0.0013(12) C18 0.0242(18) 0.0205(17) 0.0219(17) 0.0044(14) 0.0065(14) 0.0023(14) C19 0.0242(18) 0.0226(18) 0.0208(17) 0.0055(14) -0.0012(14) -0.0020(14) C20 0.0273(19) 0.0178(17) 0.0245(18) 0.0032(14) 0.0039(15) 0.0001(14) C4 0.0173(16) 0.0214(17) 0.0184(16) 0.0062(13) 0.0018(13) 0.0020(13) C21 0.032(2) 0.0215(18) 0.0191(17) 0.0063(14) 0.0013(15) 0.0044(15) C9 0.0197(17) 0.0269(18) 0.0172(16) 0.0082(14) 0.0093(13) 0.0054(14) Cl1 0.0346(5) 0.0200(4) 0.0246(4) 0.0008(3) -0.0011(4) 0.0029(4) C11 0.0165(16) 0.0160(16) 0.0148(15) -0.0030(12) 0.0016(12) 0.0017(12) C36 0.0208(17) 0.0241(18) 0.0248(18) 0.0061(14) 0.0081(14) 0.0033(14) C7 0.0206(17) 0.0235(18) 0.0237(18) 0.0116(14) 0.0075(14) 0.0075(14) C25 0.0187(17) 0.0216(17) 0.0214(17) 0.0003(14) 0.0025(14) 0.0024(13) C27 0.030(2) 0.0165(17) 0.0242(18) -0.0022(14) -0.0079(15) 0.0037(14) C26 0.029(2) 0.0232(18) 0.0229(18) -0.0015(14) 0.0038(15) 0.0037(15) C3 0.0159(16) 0.0194(17) 0.0244(17) 0.0028(14) 0.0034(13) 0.0037(13) C35 0.0194(18) 0.0224(18) 0.036(2) 0.0054(16) 0.0087(15) -0.0029(14) C22 0.0221(18) 0.0244(18) 0.0187(16) 0.0042(14) 0.0030(14) 0.0007(14) C8 0.031(2) 0.0240(18) 0.0223(18) 0.0133(15) 0.0122(15) 0.0032(15) C33 0.0219(18) 0.0218(17) 0.0215(17) 0.0045(14) 0.0054(14) 0.0017(14) C28 0.029(2) 0.0225(18) 0.028(2) 0.0090(15) -0.0005(16) -0.0052(15) C2 0.0143(16) 0.0203(17) 0.0214(17) -0.0001(13) 0.0087(13) 0.0029(12) C29 0.0246(18) 0.0213(17) 0.0212(17) 0.0041(14) 0.0045(14) -0.0007(14) C34 0.0211(17) 0.0206(17) 0.0251(18) 0.0074(14) 0.0022(14) -0.0044(13) Cl3 0.0364(5) 0.0252(5) 0.0357(5) 0.0026(4) 0.0083(4) -0.0086(4) Cl2 0.0500(6) 0.0215(5) 0.0402(6) -0.0046(4) -0.0084(5) 0.0002(4) _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 Tb1 O5 2.282(2) . ? Tb1 OW1 2.356(2) . ? Tb1 O4 2.442(2) . ? Tb1 O2 2.446(2) . ? Tb1 O1 2.497(2) . ? Tb1 O3 2.498(2) . ? Tb1 N1 2.534(3) . ? Tb1 N3 2.557(3) . ? Tb1 N2 2.582(3) . ? Tb1 C16 2.819(3) . ? Tb1 C23 2.835(3) . ? O6 C30 1.237(4) . ? O4 C23 1.256(4) . ? O1 C16 1.271(4) . ? O3 C23 1.273(4) . ? OW1 H37 0.957(19) . ? OW1 H38 0.939(19) . ? O2 C16 1.251(4) . ? C16 C17 1.499(4) . ? N1 C1 1.342(4) . ? N1 C5 1.346(4) . ? O5 C30 1.279(4) . ? C23 C24 1.499(4) . ? N3 C15 1.339(4) . ? N3 C11 1.348(4) . ? C24 C29 1.388(5) . ? C24 C25 1.395(5) . ? N2 C6 1.337(4) . ? N2 C10 1.351(4) . ? C17 C18 1.373(5) . ? C17 C22 1.402(5) . ? C14 C15 1.376(5) . ? C14 C13 1.383(5) . ? C14 H14 0.9300 . ? C1 C2 1.385(5) . ? C1 H1 0.9300 . ? C10 C9 1.394(4) . ? C10 C11 1.479(5) . ? C32 C33 1.381(5) . ? C32 C31 1.386(5) . ? C32 H32 0.9300 . ? C5 C4 1.394(5) . ? C5 C6 1.488(4) . ? C12 C13 1.386(5) . ? C12 C11 1.391(5) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C15 H15 0.9300 . ? C6 C7 1.394(5) . ? C30 C31 1.504(5) . ? C31 C36 1.394(5) . ? C18 C19 1.383(5) . ? C18 H18 0.9300 . ? C19 C20 1.385(5) . ? C19 H19 0.9300 . ? C20 C21 1.380(5) . ? C20 Cl1 1.745(4) . ? C4 C3 1.391(5) . ? C4 H4 0.9300 . ? C21 C22 1.377(5) . ? C21 H21 0.9300 . ? C9 C8 1.376(5) . ? C9 H9 0.9300 . ? C36 C35 1.389(5) . ? C36 H36 0.9300 . ? C7 C8 1.390(5) . ? C7 H7 0.9300 . ? C25 C26 1.385(5) . ? C25 H25 0.9300 . ? C27 C26 1.376(5) . ? C27 C28 1.384(5) . ? C27 Cl2 1.745(4) . ? C26 H26 0.9300 . ? C3 C2 1.377(5) . ? C3 H3 0.9300 . ? C35 C34 1.382(5) . ? C35 H35 0.9300 . ? C22 H22 0.9300 . ? C8 H8 0.9300 . ? C33 C34 1.382(5) . ? C33 H33 0.9300 . ? C28 C29 1.391(5) . ? C28 H28 0.9300 . ? C2 H2 0.9300 . ? C29 H29 0.9300 . ? C34 Cl3 1.745(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 Tb1 OW1 84.78(9) . . ? O5 Tb1 O4 133.86(8) . . ? OW1 Tb1 O4 81.38(8) . . ? O5 Tb1 O2 75.61(8) . . ? OW1 Tb1 O2 75.42(8) . . ? O4 Tb1 O2 140.44(8) . . ? O5 Tb1 O1 83.16(8) . . ? OW1 Tb1 O1 128.47(8) . . ? O4 Tb1 O1 138.04(7) . . ? O2 Tb1 O1 53.05(8) . . ? O5 Tb1 O3 81.12(8) . . ? OW1 Tb1 O3 76.20(8) . . ? O4 Tb1 O3 52.87(7) . . ? O2 Tb1 O3 144.58(7) . . ? O1 Tb1 O3 149.16(8) . . ? O5 Tb1 N1 81.73(9) . . ? OW1 Tb1 N1 145.87(8) . . ? O4 Tb1 N1 85.69(9) . . ? O2 Tb1 N1 130.10(8) . . ? O1 Tb1 N1 80.79(8) . . ? O3 Tb1 N1 70.82(8) . . ? O5 Tb1 N3 144.41(9) . . ? OW1 Tb1 N3 79.30(9) . . ? O4 Tb1 N3 74.88(8) . . ? O2 Tb1 N3 69.66(8) . . ? O1 Tb1 N3 82.27(8) . . ? O3 Tb1 N3 124.57(8) . . ? N1 Tb1 N3 127.28(9) . . ? O5 Tb1 N2 139.43(9) . . ? OW1 Tb1 N2 135.78(8) . . ? O4 Tb1 N2 66.96(8) . . ? O2 Tb1 N2 110.12(8) . . ? O1 Tb1 N2 71.43(8) . . ? O3 Tb1 N2 104.96(8) . . ? N1 Tb1 N2 63.72(8) . . ? N3 Tb1 N2 63.57(9) . . ? O5 Tb1 C16 77.58(9) . . ? OW1 Tb1 C16 101.70(9) . . ? O4 Tb1 C16 148.37(8) . . ? O2 Tb1 C16 26.28(9) . . ? O1 Tb1 C16 26.78(9) . . ? O3 Tb1 C16 158.69(8) . . ? N1 Tb1 C16 105.74(9) . . ? N3 Tb1 C16 74.83(9) . . ? N2 Tb1 C16 91.37(9) . . ? O5 Tb1 C23 107.74(9) . . ? OW1 Tb1 C23 77.66(9) . . ? O4 Tb1 C23 26.21(8) . . ? O2 Tb1 C23 152.45(8) . . ? O1 Tb1 C23 153.25(8) . . ? O3 Tb1 C23 26.66(8) . . ? N1 Tb1 C23 76.89(9) . . ? N3 Tb1 C23 99.69(9) . . ? N2 Tb1 C23 85.46(9) . . ? C16 Tb1 C23 174.48(9) . . ? C23 O4 Tb1 94.63(19) . . ? C16 O1 Tb1 90.87(19) . . ? C23 O3 Tb1 91.62(19) . . ? Tb1 OW1 H37 116(3) . . ? Tb1 OW1 H38 115(3) . . ? H37 OW1 H38 111(4) . . ? C16 O2 Tb1 93.74(19) . . ? O2 C16 O1 122.3(3) . . ? O2 C16 C17 118.1(3) . . ? O1 C16 C17 119.6(3) . . ? O2 C16 Tb1 59.98(17) . . ? O1 C16 Tb1 62.34(17) . . ? C17 C16 Tb1 177.0(2) . . ? C1 N1 C5 118.5(3) . . ? C1 N1 Tb1 119.5(2) . . ? C5 N1 Tb1 122.0(2) . . ? C30 O5 Tb1 170.6(2) . . ? O4 C23 O3 120.9(3) . . ? O4 C23 C24 119.8(3) . . ? O3 C23 C24 119.4(3) . . ? O4 C23 Tb1 59.17(17) . . ? O3 C23 Tb1 61.71(16) . . ? C24 C23 Tb1 178.7(2) . . ? C15 N3 C11 118.1(3) . . ? C15 N3 Tb1 120.0(2) . . ? C11 N3 Tb1 121.9(2) . . ? C29 C24 C25 119.6(3) . . ? C29 C24 C23 120.0(3) . . ? C25 C24 C23 120.3(3) . . ? C6 N2 C10 119.0(3) . . ? C6 N2 Tb1 120.0(2) . . ? C10 N2 Tb1 119.9(2) . . ? C18 C17 C22 119.3(3) . . ? C18 C17 C16 121.7(3) . . ? C22 C17 C16 119.0(3) . . ? C15 C14 C13 118.2(3) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? N1 C1 C2 123.4(3) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? N2 C10 C9 121.6(3) . . ? N2 C10 C11 117.7(3) . . ? C9 C10 C11 120.8(3) . . ? C33 C32 C31 121.4(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 116.5(3) . . ? C4 C5 C6 122.2(3) . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? N3 C15 C14 123.7(3) . . ? N3 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? N2 C6 C7 122.4(3) . . ? N2 C6 C5 116.8(3) . . ? C7 C6 C5 120.7(3) . . ? O6 C30 O5 125.6(3) . . ? O6 C30 C31 117.8(3) . . ? O5 C30 C31 116.6(3) . . ? C32 C31 C36 119.1(3) . . ? C32 C31 C30 120.7(3) . . ? C36 C31 C30 120.2(3) . . ? C17 C18 C19 121.1(3) . . ? C17 C18 H18 119.4 . . ? C19 C18 H18 119.4 . . ? C18 C19 C20 118.3(3) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? C21 C20 C19 122.0(3) . . ? C21 C20 Cl1 119.3(3) . . ? C19 C20 Cl1 118.7(3) . . ? C3 C4 C5 119.3(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C22 C21 C20 118.7(3) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C8 C9 C10 119.2(3) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? N3 C11 C12 121.6(3) . . ? N3 C11 C10 116.3(3) . . ? C12 C11 C10 122.1(3) . . ? C35 C36 C31 120.1(3) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C8 C7 C6 118.4(3) . . ? C8 C7 H7 120.8 . . ? C6 C7 H7 120.8 . . ? C26 C25 C24 120.3(3) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C26 C27 C28 121.9(3) . . ? C26 C27 Cl2 119.4(3) . . ? C28 C27 Cl2 118.7(3) . . ? C27 C26 C25 119.0(3) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C34 C35 C36 119.3(3) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C21 C22 C17 120.5(3) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? C9 C8 C7 119.4(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C32 C33 C34 118.6(3) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C27 C28 C29 118.7(3) . . ? C27 C28 H28 120.6 . . ? C29 C28 H28 120.6 . . ? C3 C2 C1 118.2(3) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C24 C29 C28 120.4(3) . . ? C24 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C33 C34 C35 121.4(3) . . ? C33 C34 Cl3 119.9(3) . . ? C35 C34 Cl3 118.7(3) . . ? _refine_diff_density_max 1.306 _refine_diff_density_min -1.254 _refine_diff_density_rms 0.148 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1_twin in P-1 CELL 0.71073 8.6840 13.1300 14.7700 100.221 97.912 92.257 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N O CL TB UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 12 WGHT 0.038100 0.766300 FVAR 0.11923 TB1 6 0.563650 0.513077 0.701405 11.00000 0.01346 0.01545 = 0.01178 0.00343 0.00425 0.00112 O6 4 0.849125 0.581133 0.500602 11.00000 0.02155 0.02587 = 0.01874 0.00508 0.00711 -0.00301 O4 4 0.406816 0.348535 0.660694 11.00000 0.01852 0.01950 = 0.01561 0.00322 0.00540 0.00050 O1 4 0.712028 0.624782 0.843626 11.00000 0.01781 0.01626 = 0.01729 0.00274 0.00590 0.00212 O3 4 0.561950 0.375942 0.560405 11.00000 0.01662 0.01978 = 0.01594 0.00487 0.00483 -0.00007 OW1 4 0.368131 0.559308 0.591704 11.00000 0.01584 0.01991 = 0.01483 0.00630 0.00377 0.00072 O2 4 0.537821 0.697729 0.756527 11.00000 0.01692 0.02081 = 0.01677 0.00464 0.00433 0.00145 C16 1 0.641806 0.703359 0.825155 11.00000 0.01957 0.01507 = 0.01754 0.00218 0.01149 0.00066 N1 3 0.794304 0.403854 0.726762 11.00000 0.01609 0.01547 = 0.01275 0.00254 0.00226 -0.00011 O5 4 0.731212 0.595229 0.627427 11.00000 0.02008 0.02174 = 0.01800 0.00550 0.00897 -0.00137 C23 1 0.460789 0.319074 0.586428 11.00000 0.01439 0.01659 = 0.01460 0.00634 -0.00054 0.00370 N3 3 0.339495 0.537924 0.797120 11.00000 0.01617 0.01467 = 0.01414 0.00340 0.00425 0.00095 C24 1 0.405933 0.215519 0.527538 11.00000 0.01739 0.01463 = 0.01604 0.00272 0.00045 0.00392 N2 3 0.570962 0.413880 0.837878 11.00000 0.01404 0.01323 = 0.01413 0.00032 0.00467 0.00015 C17 1 0.684134 0.807190 0.886683 11.00000 0.02046 0.02137 = 0.01572 0.00087 0.00807 -0.00268 C14 1 0.101552 0.616923 0.822640 11.00000 0.01791 0.02319 = 0.02265 0.00271 0.00222 0.00465 AFIX 43 H14 2 0.024798 0.659629 0.804398 11.00000 -1.20000 AFIX 0 C1 1 0.905703 0.402994 0.672092 11.00000 0.01719 0.01820 = 0.01681 0.00426 0.00696 0.00107 AFIX 43 H1 2 0.892188 0.439730 0.623532 11.00000 -1.20000 AFIX 0 C10 1 0.449820 0.415434 0.886365 11.00000 0.01898 0.01559 = 0.01232 0.00272 0.00473 -0.00050 C32 1 0.874155 0.796501 0.689945 11.00000 0.01832 0.02107 = 0.02023 0.00893 0.00551 0.00177 AFIX 43 H32 2 0.782314 0.781261 0.712041 11.00000 -1.20000 AFIX 0 C5 1 0.810561 0.347675 0.794932 11.00000 0.01553 0.01564 = 0.01423 0.00135 0.00268 0.00117 C12 1 0.207283 0.503290 0.921225 11.00000 0.02129 0.02017 = 0.01802 0.00421 0.01002 0.00032 AFIX 43 H12 2 0.204182 0.470851 0.972094 11.00000 -1.20000 AFIX 0 C13 1 0.091481 0.567294 0.896968 11.00000 0.01953 0.02158 = 0.02597 0.00209 0.01267 0.00283 AFIX 43 H13 2 0.008068 0.576760 0.930231 11.00000 -1.20000 AFIX 0 C15 1 0.228314 0.601354 0.776423 11.00000 0.01858 0.01991 = 0.01330 0.00328 0.00249 0.00227 AFIX 43 H15 2 0.237220 0.636926 0.728070 11.00000 -1.20000 AFIX 0 C6 1 0.679777 0.346368 0.850169 11.00000 0.01603 0.01765 = 0.01268 0.00146 0.00494 0.00246 C30 1 0.827215 0.626431 0.578224 11.00000 0.01325 0.02026 = 0.01656 0.00789 0.00276 0.00295 C31 1 0.922612 0.725987 0.619701 11.00000 0.01677 0.01982 = 0.01354 0.00910 0.00102 0.00129 C18 1 0.806425 0.821966 0.958291 11.00000 0.02419 0.02050 = 0.02192 0.00438 0.00651 0.00229 AFIX 43 H18 2 0.865899 0.766609 0.968515 11.00000 -1.20000 AFIX 0 C19 1 0.842672 0.917772 1.015478 11.00000 0.02420 0.02261 = 0.02076 0.00549 -0.00122 -0.00197 AFIX 43 H19 2 0.924846 0.927227 1.064339 11.00000 -1.20000 AFIX 0 C20 1 0.753479 0.999268 0.998124 11.00000 0.02729 0.01777 = 0.02453 0.00325 0.00389 0.00013 C4 1 0.943039 0.293389 0.811926 11.00000 0.01731 0.02136 = 0.01844 0.00616 0.00183 0.00200 AFIX 43 H4 2 0.953632 0.256012 0.860094 11.00000 -1.20000 AFIX 0 C21 1 0.632143 0.987682 0.925422 11.00000 0.03210 0.02152 = 0.01908 0.00631 0.00129 0.00442 AFIX 43 H21 2 0.575034 1.043752 0.914191 11.00000 -1.20000 AFIX 0 C9 1 0.436917 0.349419 0.949558 11.00000 0.01971 0.02687 = 0.01722 0.00822 0.00933 0.00543 AFIX 43 H9 2 0.354501 0.353144 0.983849 11.00000 -1.20000 AFIX 0 CL1 5 0.796506 1.120013 1.070895 11.00000 0.03461 0.01997 = 0.02463 0.00078 -0.00106 0.00290 C11 1 0.328258 0.488168 0.868516 11.00000 0.01655 0.01600 = 0.01477 -0.00302 0.00164 0.00172 C36 1 1.059431 0.749741 0.586049 11.00000 0.02078 0.02407 = 0.02481 0.00607 0.00808 0.00326 AFIX 43 H36 2 1.092288 0.703652 0.538175 11.00000 -1.20000 AFIX 0 C7 1 0.671846 0.276287 0.910346 11.00000 0.02062 0.02354 = 0.02372 0.01155 0.00746 0.00747 AFIX 43 H7 2 0.747889 0.229080 0.916704 11.00000 -1.20000 AFIX 0 C25 1 0.470770 0.179531 0.447419 11.00000 0.01871 0.02156 = 0.02135 0.00034 0.00248 0.00240 AFIX 43 H25 2 0.545167 0.221246 0.428992 11.00000 -1.20000 AFIX 0 C27 1 0.312355 0.022264 0.422456 11.00000 0.02990 0.01649 = 0.02421 -0.00215 -0.00788 0.00366 C26 1 0.424925 0.082037 0.395204 11.00000 0.02885 0.02322 = 0.02291 -0.00145 0.00381 0.00374 AFIX 43 H26 2 0.469547 0.057312 0.342495 11.00000 -1.20000 AFIX 0 C3 1 1.059199 0.295711 0.756094 11.00000 0.01586 0.01941 = 0.02436 0.00285 0.00342 0.00374 AFIX 43 H3 2 1.149047 0.260824 0.767153 11.00000 -1.20000 AFIX 0 C35 1 1.146705 0.842131 0.623923 11.00000 0.01939 0.02237 = 0.03596 0.00543 0.00872 -0.00294 AFIX 43 H35 2 1.238343 0.858037 0.601907 11.00000 -1.20000 AFIX 0 C22 1 0.597342 0.891420 0.869843 11.00000 0.02214 0.02441 = 0.01869 0.00424 0.00300 0.00070 AFIX 43 H22 2 0.515599 0.882218 0.820740 11.00000 -1.20000 AFIX 0 C8 1 0.547599 0.278656 0.960602 11.00000 0.03089 0.02405 = 0.02233 0.01331 0.01224 0.00316 AFIX 43 H8 2 0.539308 0.232869 1.001310 11.00000 -1.20000 AFIX 0 C33 1 0.959349 0.888915 0.727826 11.00000 0.02189 0.02181 = 0.02152 0.00453 0.00541 0.00172 AFIX 43 H33 2 0.925432 0.935858 0.774696 11.00000 -1.20000 AFIX 0 C28 1 0.244073 0.056552 0.500721 11.00000 0.02944 0.02247 = 0.02817 0.00900 -0.00047 -0.00522 AFIX 43 H28 2 0.167232 0.015335 0.517549 11.00000 -1.20000 AFIX 0 C2 1 1.039753 0.350220 0.684261 11.00000 0.01429 0.02026 = 0.02143 -0.00011 0.00870 0.00287 AFIX 43 H2 2 1.114565 0.351556 0.645009 11.00000 -1.20000 AFIX 0 C29 1 0.292624 0.153859 0.553710 11.00000 0.02458 0.02126 = 0.02125 0.00409 0.00451 -0.00072 AFIX 43 H29 2 0.248927 0.177731 0.606961 11.00000 -1.20000 AFIX 0 C34 1 1.096015 0.910201 0.694660 11.00000 0.02114 0.02063 = 0.02510 0.00743 0.00223 -0.00436 CL3 5 1.208914 1.024920 0.742639 11.00000 0.03641 0.02523 = 0.03573 0.00255 0.00829 -0.00864 CL2 5 0.249554 -0.099131 0.355193 11.00000 0.04996 0.02145 = 0.04024 -0.00458 -0.00839 0.00020 H37 2 0.293398 0.504607 0.560115 11.00000 0.03233 H38 2 0.403877 0.597091 0.549503 11.00000 0.04235 HKLF 4 REM Pbar1_twin in P-1 REM R1 = 0.0368 for 7553 Fo > 4sig(Fo) and 0.0493 for all 8909 data REM 459 parameters refined using 2 restraints END WGHT 0.0374 0.8984 REM Highest difference peak 1.306, deepest hole -1.254, 1-sigma level 0.148 Q1 1 0.3061 0.4596 0.8984 11.00000 0.05 1.31 Q2 1 0.9009 1.1264 1.0457 11.00000 0.05 1.05 Q3 1 0.5687 0.5817 0.7055 11.00000 0.05 0.84 Q4 1 0.6493 0.5140 0.7206 11.00000 0.05 0.81 Q5 1 0.1953 -0.1409 0.3984 11.00000 0.05 0.80 Q6 1 0.5537 0.4567 0.7011 11.00000 0.05 0.72 Q7 1 0.4592 0.5052 0.6726 11.00000 0.05 0.71 Q8 1 0.7355 0.9957 0.9380 11.00000 0.05 0.68 Q9 1 0.4699 0.4272 0.6660 11.00000 0.05 0.67 Q10 1 0.5705 0.4607 0.5441 11.00000 0.05 0.65 ; _shelx_res_checksum 27707 _shelx_hkl_file ; 1 0 0 298.81 2.84 2 0 0 0.81 0.16 3 0 0 92.93 1.36 4 0 0 0.59 0.21 5 0 0 47.45 1.02 6 0 0 105.31 1.90 7 0 0 33.68 1.17 8 0 0 127.94 2.81 9 0 0 66.94 2.62 10 0 0 13.68 1.54 11 0 0 1.52 0.93 -11 1 0 5.97 1.59 -10 1 0 14.00 1.74 -9 1 0 27.78 2.10 -8 1 0 122.79 3.57 -7 1 0 64.93 2.22 -6 1 0 9.11 0.63 -5 1 0 1.49 0.38 -4 1 0 10.05 0.51 -3 1 0 45.79 1.24 -2 1 0 505.67 5.05 -1 1 0 380.75 4.89 0 1 0 348.01 3.65 1 1 0 232.86 2.40 2 1 0 115.19 1.41 3 1 0 11.33 0.41 4 1 0 43.80 0.87 5 1 0 8.40 0.48 6 1 0 79.14 1.44 7 1 0 104.89 2.01 8 1 0 42.22 1.93 9 1 0 43.00 2.09 10 1 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103.30 2.44 9 -4 2 45.34 1.99 10 -4 2 16.96 1.54 11 -4 2 17.36 2.12 -11 -3 2 2.14 1.10 -10 -3 2 0.43 0.82 -9 -3 2 1.39 0.80 -8 -3 2 11.95 1.34 -7 -3 2 68.87 1.88 -6 -3 2 52.27 1.19 -5 -3 2 53.38 1.11 -4 -3 2 72.03 1.25 -3 -3 2 45.68 0.87 -2 -3 2 26.16 0.59 -1 -3 2 3.57 0.21 0 -3 2 55.26 0.82 1 -3 2 36.91 0.65 2 -3 2 291.92 3.69 3 -3 2 58.03 0.99 4 -3 2 51.88 0.98 5 -3 2 75.60 1.31 6 -3 2 35.30 1.18 7 -3 2 2.65 0.81 8 -3 2 7.73 1.03 9 -3 2 49.25 2.18 10 -3 2 47.72 2.94 11 -3 2 5.18 1.64 -11 -2 2 9.23 1.49 -10 -2 2 3.33 0.98 -9 -2 2 19.92 1.65 -8 -2 2 23.25 1.63 -7 -2 2 72.98 1.93 -6 -2 2 168.85 2.68 -5 -2 2 106.62 1.69 -4 -2 2 34.11 0.75 -3 -2 2 18.31 0.49 -2 -2 2 0.14 0.15 -1 -2 2 2.24 0.18 0 -2 2 45.58 0.67 1 -2 2 307.52 3.22 2 -2 2 834.49 8.90 3 -2 2 180.51 2.22 4 -2 2 0.55 0.21 5 -2 2 56.32 1.27 6 -2 2 3.60 0.58 7 -2 2 5.25 0.83 8 -2 2 42.99 1.90 9 -2 2 52.46 2.24 10 -2 2 13.61 1.90 11 -2 2 23.71 2.25 -11 -1 2 3.53 1.16 -10 -1 2 1.53 0.85 -9 -1 2 7.14 1.12 -8 -1 2 32.89 1.79 -7 -1 2 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12.17 2.07 1 -10 18 20.94 4.70 -5 -9 18 4.89 5.96 -4 -9 18 3.27 1.56 -3 -9 18 7.17 1.35 -2 -9 18 11.89 1.56 -1 -9 18 5.81 1.31 0 -9 18 20.21 1.83 1 -9 18 14.47 1.62 2 -9 18 1.00 3.67 -5 -8 18 0.67 2.77 -4 -8 18 3.05 1.36 -3 -8 18 3.69 1.10 -2 -8 18 11.55 1.48 -1 -8 18 15.06 1.67 0 -8 18 21.43 1.80 1 -8 18 11.89 1.57 2 -8 18 3.65 1.55 3 -8 18 0.35 4.66 -6 -7 18 5.81 1.70 -5 -7 18 0.00 1.19 -4 -7 18 1.99 1.05 -3 -7 18 9.38 1.43 -2 -7 18 17.35 1.79 -1 -7 18 14.16 1.64 0 -7 18 30.19 2.22 1 -7 18 10.86 1.46 2 -7 18 1.06 0.95 3 -7 18 1.87 4.85 -6 -6 18 5.38 1.75 -5 -6 18 2.69 1.12 -4 -6 18 2.81 1.12 -3 -6 18 28.61 2.10 -2 -6 18 10.12 1.42 -1 -6 18 62.65 2.75 0 -6 18 36.14 2.37 1 -6 18 5.96 1.18 2 -6 18 3.21 1.08 3 -6 18 1.38 1.40 -6 -5 18 2.69 1.57 -5 -5 18 0.00 0.91 -4 -5 18 4.87 1.14 -3 -5 18 29.54 2.12 -2 -5 18 23.34 1.92 -1 -5 18 43.68 2.53 0 -5 18 50.86 2.47 1 -5 18 18.59 1.77 2 -5 18 1.96 1.00 3 -5 18 0.05 0.90 -6 -4 18 2.94 4.34 -5 -4 18 0.03 1.16 -4 -4 18 8.77 1.48 -3 -4 18 4.93 1.22 -2 -4 18 41.93 2.46 -1 -4 18 52.76 2.50 0 -4 18 36.86 2.33 1 -4 18 6.36 1.22 2 -4 18 5.57 1.20 3 -4 18 0.36 0.92 -7 -3 18 3.53 1.73 -6 -3 18 0.00 3.98 -5 -3 18 4.08 1.11 -4 -3 18 0.38 0.87 -3 -3 18 35.50 2.28 -2 -3 18 41.70 2.47 -1 -3 18 21.77 1.83 0 -3 18 27.75 2.05 1 -3 18 8.77 1.32 2 -3 18 0.93 0.89 3 -3 18 0.09 0.87 -7 -2 18 6.36 2.01 -6 -2 18 2.09 4.31 -5 -2 18 0.30 0.86 -4 -2 18 6.96 1.28 -3 -2 18 18.38 1.70 -2 -2 18 28.92 2.11 -1 -2 18 28.62 2.05 0 -2 18 17.90 1.72 1 -2 18 8.98 1.37 2 -2 18 0.22 0.81 3 -2 18 4.62 1.18 -7 -1 18 0.00 1.37 -6 -1 18 2.19 1.52 -5 -1 18 1.15 0.99 -4 -1 18 5.04 1.17 -3 -1 18 12.52 1.55 -2 -1 18 26.42 2.01 -1 -1 18 26.52 2.00 0 -1 18 10.60 1.42 1 -1 18 13.27 1.58 2 -1 18 1.55 0.95 3 -1 18 3.75 1.14 -6 0 18 0.00 1.29 -5 0 18 1.70 2.87 -4 0 18 7.23 1.24 -3 0 18 23.08 1.86 -2 0 18 30.99 2.15 -1 0 18 5.80 1.17 0 0 18 15.60 1.64 1 0 18 8.85 1.38 2 0 18 1.84 1.01 3 0 18 5.89 2.01 -6 1 18 1.15 1.41 -5 1 18 8.07 1.89 -4 1 18 27.55 2.04 -3 1 18 16.57 1.67 -2 1 18 15.31 1.61 -1 1 18 3.25 1.06 0 1 18 3.11 1.03 1 1 18 5.49 1.21 2 1 18 1.74 0.99 3 1 18 8.17 2.14 -6 2 18 0.34 1.38 -5 2 18 16.68 1.94 -4 2 18 22.62 1.87 -3 2 18 11.59 1.49 -2 2 18 5.78 1.21 -1 2 18 39.33 2.43 0 2 18 3.77 1.12 1 2 18 0.60 0.92 2 2 18 1.23 1.61 3 2 18 4.35 1.98 -5 3 18 5.46 1.88 -4 3 18 7.61 1.35 -3 3 18 18.96 1.78 -2 3 18 17.42 1.43 -1 3 18 16.77 1.75 0 3 18 4.64 1.21 1 3 18 2.28 1.19 2 3 18 1.82 1.64 -5 4 18 7.24 2.09 -4 4 18 21.72 3.06 -3 4 18 23.60 2.08 -2 4 18 12.04 1.32 -1 4 18 40.32 2.12 0 4 18 17.84 1.93 1 4 18 0.00 1.29 -3 5 18 26.39 3.14 -2 5 18 24.70 2.16 -1 5 18 11.21 1.69 0 5 18 9.05 2.19 -3 -9 19 6.04 4.43 -2 -9 19 29.47 5.40 -1 -9 19 7.34 3.91 0 -9 19 1.46 4.32 -3 -8 19 8.96 19.18 -2 -8 19 16.78 4.21 -1 -8 19 2.95 4.31 0 -8 19 1.24 1.55 -4 -7 19 10.81 1.70 -3 -7 19 18.20 1.92 -2 -7 19 11.89 1.55 -1 -7 19 5.63 1.28 0 -7 19 2.43 1.06 -5 -6 19 14.64 1.85 -4 -6 19 13.69 1.72 -3 -6 19 35.64 2.39 -2 -6 19 4.55 1.23 -1 -6 19 10.38 1.48 0 -6 19 1.73 0.99 1 -6 19 2.87 3.09 -5 -5 19 41.70 2.86 -4 -5 19 23.46 2.14 -3 -5 19 17.74 1.85 -2 -5 19 16.62 1.81 -1 -5 19 7.34 1.43 0 -5 19 2.37 1.21 1 -5 19 12.91 2.09 -5 -4 19 16.79 2.53 -4 -4 19 14.78 1.85 -3 -4 19 35.01 2.34 -2 -4 19 8.57 1.48 -1 -4 19 0.15 1.05 0 -4 19 0.83 1.08 1 -4 19 0.00 1.18 -6 -3 19 4.02 4.86 -5 -3 19 31.90 2.91 -4 -3 19 10.82 1.71 -3 -3 19 13.78 1.76 -2 -3 19 22.21 1.94 -1 -3 19 3.98 1.11 0 -3 19 1.06 0.91 1 -3 19 8.58 1.43 -5 -2 19 13.56 1.59 -4 -2 19 30.90 2.22 -3 -2 19 15.84 1.77 -2 -2 19 1.34 1.01 -1 -2 19 1.00 0.92 0 -2 19 0.98 0.90 1 -2 19 4.33 1.21 -5 -1 19 24.18 6.68 -4 -1 19 17.99 1.90 -3 -1 19 15.90 1.76 -2 -1 19 8.63 1.41 -1 -1 19 0.21 0.88 0 -1 19 4.24 1.21 1 -1 19 4.30 1.24 -5 0 19 20.20 6.34 -4 0 19 42.39 2.70 -3 0 19 3.70 1.19 -2 0 19 0.50 0.89 -1 0 19 0.00 0.82 0 0 19 2.02 1.05 1 0 19 21.49 3.05 -4 1 19 17.81 2.30 -3 1 19 3.17 1.11 -2 1 19 0.40 0.94 -1 1 19 1.19 0.97 0 1 19 2.03 1.10 -4 2 19 20.79 6.48 -3 2 19 2.43 1.60 -2 2 19 1.49 1.44 -1 2 19 5.11 1.82 -3 3 19 3.02 1.60 -2 3 19 1.98 1.61 -3 -6 20 40.42 18.05 -2 -6 20 0.00 21.51 -3 -5 20 5.70 65.74 -2 -5 20 18.88 18.22 -4 -4 20 1.93 4.41 -3 -4 20 2.08 4.39 -2 -4 20 13.73 5.24 -4 -3 20 1.22 1.49 -3 -3 20 0.81 1.38 -2 -3 20 17.49 2.52 -4 -2 20 0.00 1.38 -3 -2 20 1.44 1.52 -2 -2 20 9.72 2.36 -3 -1 20 17.73 2.90 -3 0 20 15.49 2.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 91069 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969306' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_7 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 Dy N3 O7' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 880.44 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Dy Dy -0.1892 4.4098 '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 8.689(5) _cell_length_b 13.109(5) _cell_length_c 14.771(5) _cell_angle_alpha 100.206(5) _cell_angle_beta 97.819(5) _cell_angle_gamma 92.396(5) _cell_volume 1636.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21851 _cell_measurement_theta_min 4.744 _cell_measurement_theta_max 52.468 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.787 _exptl_crystal_F_000 870 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_absorpt_coefficient_mu 2.584 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6246 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'TWINABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21456 _diffrn_reflns_av_unetI/netI 0.0754 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 1.416 _diffrn_reflns_theta_max 26.415 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6703 _reflns_number_gt 5354 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. 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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0452P)^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 6703 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0635 _refine_ls_R_factor_gt 0.0460 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Dy1 Dy 0.56291(3) 0.51321(2) 0.70147(2) 0.01530(9) Uani 1 1 d . . . . . Cl3 Cl 1.20968(19) 1.02554(12) 0.74329(11) 0.0346(4) Uani 1 1 d . . . . . Cl2 Cl 0.2492(2) -0.09973(12) 0.35628(12) 0.0420(4) Uani 1 1 d . . . . . Cl1 Cl 0.79651(18) 1.12007(11) 1.07062(10) 0.0293(3) Uani 1 1 d . . . . . O4 O 0.4060(4) 0.3497(3) 0.6608(2) 0.0164(8) Uani 1 1 d . . . . . O3 O 0.5615(4) 0.3770(3) 0.5610(2) 0.0193(8) Uani 1 1 d . . . . . O1 O 0.7105(4) 0.6244(3) 0.8430(2) 0.0182(8) Uani 1 1 d . . . . . OW1 O 0.3677(4) 0.5586(3) 0.5916(2) 0.0183(8) Uani 1 1 d . . . . . O2 O 0.5358(4) 0.6977(3) 0.7558(2) 0.0198(8) Uani 1 1 d . . . . . O5 O 0.7302(4) 0.5957(3) 0.6282(2) 0.0207(9) Uani 1 1 d . . . . . N3 N 0.3396(5) 0.5381(3) 0.7963(3) 0.0159(10) Uani 1 1 d . . . . . O6 O 0.8487(4) 0.5810(3) 0.5013(3) 0.0235(9) Uani 1 1 d . . . . . C11 C 0.3276(6) 0.4885(4) 0.8686(4) 0.0185(12) Uani 1 1 d . . . . . N2 N 0.5704(5) 0.4141(3) 0.8376(3) 0.0140(9) Uani 1 1 d . . . . . N1 N 0.7924(5) 0.4054(3) 0.7262(3) 0.0165(10) Uani 1 1 d . . . . . C5 C 0.8095(6) 0.3491(4) 0.7950(4) 0.0152(11) Uani 1 1 d . . . . . C10 C 0.4495(6) 0.4156(4) 0.8862(3) 0.0141(11) Uani 1 1 d . . . . . C24 C 0.4062(6) 0.2161(4) 0.5281(4) 0.0172(12) Uani 1 1 d . . . . . C31 C 0.9218(6) 0.7259(4) 0.6199(4) 0.0165(11) Uani 1 1 d . . . . . C6 C 0.6798(6) 0.3468(4) 0.8502(3) 0.0159(11) Uani 1 1 d . . . . . C4 C 0.9428(6) 0.2941(4) 0.8107(4) 0.0180(12) Uani 1 1 d . . . . . H4 H 0.9537 0.2564 0.8587 0.022 Uiso 1 1 calc R U . . . C15 C 0.2286(6) 0.6015(4) 0.7753(4) 0.0189(12) Uani 1 1 d . . . . . H15 H 0.2371 0.6367 0.7267 0.023 Uiso 1 1 calc R U . . . C30 C 0.8268(6) 0.6267(4) 0.5796(4) 0.0171(12) Uani 1 1 d . . . . . C13 C 0.0908(6) 0.5681(4) 0.8963(4) 0.0225(13) Uani 1 1 d . . . . . H13 H 0.0073 0.5778 0.9295 0.027 Uiso 1 1 calc R U . . . C17 C 0.6839(6) 0.8057(4) 0.8857(4) 0.0187(12) Uani 1 1 d . . . . . C23 C 0.4591(6) 0.3202(4) 0.5862(3) 0.0148(11) Uani 1 1 d . . . . . C32 C 0.8727(6) 0.7976(4) 0.6901(4) 0.0175(12) Uani 1 1 d . . . . . H32 H 0.7803 0.7829 0.7119 0.021 Uiso 1 1 calc R U . . . C20 C 0.7530(7) 1.0004(4) 0.9978(4) 0.0231(13) Uani 1 1 d . . . . . C16 C 0.6420(6) 0.7034(4) 0.8249(4) 0.0163(12) Uani 1 1 d . . . . . C18 C 0.8058(7) 0.8214(5) 0.9574(4) 0.0257(13) Uani 1 1 d . . . . . H18 H 0.8660 0.7665 0.9676 0.031 Uiso 1 1 calc R U . . . C19 C 0.8411(7) 0.9177(5) 1.0148(4) 0.0246(13) Uani 1 1 d . . . . . H19 H 0.9224 0.9269 1.0640 0.030 Uiso 1 1 calc R U . . . C12 C 0.2057(6) 0.5040(4) 0.9207(4) 0.0199(12) Uani 1 1 d . . . . . H12 H 0.2017 0.4715 0.9715 0.024 Uiso 1 1 calc R U . . . C33 C 0.9589(7) 0.8904(4) 0.7278(4) 0.0231(13) Uani 1 1 d . . . . . H33 H 0.9251 0.9378 0.7744 0.028 Uiso 1 1 calc R U . . . C8 C 0.5481(7) 0.2785(5) 0.9602(4) 0.0265(14) Uani 1 1 d . . . . . H8 H 0.5406 0.2323 1.0007 0.032 Uiso 1 1 calc R U . . . C34 C 1.0960(6) 0.9108(4) 0.6949(4) 0.0216(12) Uani 1 1 d . . . . . C2 C 1.0382(6) 0.3512(4) 0.6834(4) 0.0196(12) Uani 1 1 d . . . . . H2 H 1.1134 0.3533 0.6445 0.024 Uiso 1 1 calc R U . . . C1 C 0.9038(7) 0.4035(4) 0.6711(4) 0.0219(13) Uani 1 1 d . . . . . H1 H 0.8898 0.4393 0.6219 0.026 Uiso 1 1 calc R U . . . C21 C 0.6333(7) 0.9870(5) 0.9249(4) 0.0253(13) Uani 1 1 d . . . . . H21 H 0.5776 1.0434 0.9128 0.030 Uiso 1 1 calc R U . . . C9 C 0.4361(7) 0.3488(5) 0.9496(4) 0.0244(13) Uani 1 1 d . . . . . H9 H 0.3536 0.3518 0.9838 0.029 Uiso 1 1 calc R U . . . C29 C 0.2918(7) 0.1540(4) 0.5535(4) 0.0230(13) Uani 1 1 d . . . . . H29 H 0.2482 0.1779 0.6068 0.028 Uiso 1 1 calc R U . . . C22 C 0.5954(7) 0.8916(5) 0.8701(4) 0.0232(13) Uani 1 1 d . . . . . H22 H 0.5116 0.8826 0.8224 0.028 Uiso 1 1 calc R U . . . C26 C 0.4253(7) 0.0818(5) 0.3952(4) 0.0261(14) Uani 1 1 d . . . . . H26 H 0.4699 0.0573 0.3424 0.031 Uiso 1 1 calc R U . . . C14 C 0.1016(6) 0.6172(4) 0.8224(4) 0.0196(12) Uani 1 1 d . . . . . H14 H 0.0252 0.6602 0.8044 0.024 Uiso 1 1 calc R U . . . C3 C 1.0573(6) 0.2959(4) 0.7550(4) 0.0207(12) Uani 1 1 d . . . . . H3 H 1.1465 0.2604 0.7655 0.025 Uiso 1 1 calc R U . . . C7 C 0.6707(6) 0.2772(4) 0.9103(4) 0.0218(13) Uani 1 1 d . . . . . H7 H 0.7469 0.2302 0.9168 0.026 Uiso 1 1 calc R U . . . C35 C 1.1470(7) 0.8418(5) 0.6245(4) 0.0252(13) Uani 1 1 d . . . . . H35 H 1.2391 0.8570 0.6026 0.030 Uiso 1 1 calc R U . . . C27 C 0.3111(7) 0.0216(4) 0.4229(4) 0.0268(14) Uani 1 1 d . . . . . C36 C 1.0590(6) 0.7502(4) 0.5875(4) 0.0219(13) Uani 1 1 d . . . . . H36 H 1.0921 0.7038 0.5399 0.026 Uiso 1 1 calc R U . . . C25 C 0.4712(6) 0.1795(4) 0.4483(4) 0.0219(13) Uani 1 1 d . . . . . H25 H 0.5465 0.2211 0.4303 0.026 Uiso 1 1 calc R U . . . C28 C 0.2416(7) 0.0572(5) 0.5007(4) 0.0268(14) Uani 1 1 d . . . . . H28 H 0.1629 0.0169 0.5170 0.032 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 Dy1 0.01379(14) 0.01588(15) 0.01665(14) 0.00301(10) 0.00392(9) 0.00028(9) Cl3 0.0373(9) 0.0251(9) 0.0398(9) 0.0029(7) 0.0075(7) -0.0088(7) Cl2 0.0500(11) 0.0206(9) 0.0458(10) -0.0065(7) -0.0094(8) 0.0001(8) Cl1 0.0339(9) 0.0213(8) 0.0298(8) 0.0006(6) -0.0010(6) 0.0027(6) O4 0.015(2) 0.016(2) 0.019(2) 0.0032(15) 0.0038(15) 0.0006(15) O3 0.018(2) 0.020(2) 0.021(2) 0.0047(16) 0.0075(16) -0.0024(16) O1 0.019(2) 0.014(2) 0.021(2) 0.0029(16) 0.0035(16) 0.0006(16) OW1 0.015(2) 0.023(2) 0.019(2) 0.0063(16) 0.0054(15) 0.0043(16) O2 0.019(2) 0.018(2) 0.022(2) 0.0012(16) 0.0048(16) 0.0002(16) O5 0.020(2) 0.022(2) 0.023(2) 0.0076(17) 0.0079(16) -0.0002(17) N3 0.016(2) 0.014(2) 0.016(2) -0.0002(18) 0.0040(18) -0.0013(19) O6 0.022(2) 0.029(2) 0.020(2) 0.0056(18) 0.0063(17) -0.0068(18) C11 0.012(3) 0.013(3) 0.023(3) -0.010(2) -0.003(2) 0.000(2) N2 0.011(2) 0.013(2) 0.017(2) 0.0020(18) 0.0012(17) 0.0003(18) N1 0.014(2) 0.016(2) 0.019(2) 0.0015(19) 0.0040(18) -0.0011(19) C5 0.015(3) 0.010(3) 0.020(3) 0.001(2) 0.005(2) -0.002(2) C10 0.011(3) 0.014(3) 0.018(3) 0.000(2) 0.006(2) 0.000(2) C24 0.018(3) 0.015(3) 0.018(3) 0.003(2) -0.001(2) 0.004(2) C31 0.014(3) 0.016(3) 0.021(3) 0.010(2) 0.001(2) 0.001(2) C6 0.014(3) 0.016(3) 0.015(3) -0.002(2) 0.001(2) -0.002(2) C4 0.018(3) 0.019(3) 0.018(3) 0.008(2) 0.002(2) 0.001(2) C15 0.020(3) 0.011(3) 0.026(3) 0.002(2) 0.005(2) 0.000(2) C30 0.011(3) 0.019(3) 0.022(3) 0.010(2) 0.000(2) 0.004(2) C13 0.015(3) 0.023(3) 0.030(3) 0.001(3) 0.009(2) -0.001(2) C17 0.022(3) 0.018(3) 0.018(3) 0.006(2) 0.007(2) -0.006(2) C23 0.012(3) 0.018(3) 0.014(3) 0.006(2) 0.000(2) 0.004(2) C32 0.014(3) 0.020(3) 0.020(3) 0.010(2) 0.002(2) 0.002(2) C20 0.024(3) 0.019(3) 0.026(3) 0.001(2) 0.006(2) -0.001(3) C16 0.016(3) 0.015(3) 0.021(3) 0.002(2) 0.016(2) -0.002(2) C18 0.029(3) 0.022(3) 0.026(3) 0.006(3) 0.006(3) -0.001(3) C19 0.019(3) 0.027(3) 0.026(3) 0.003(3) 0.002(2) 0.002(3) C12 0.019(3) 0.018(3) 0.026(3) 0.004(2) 0.014(2) 0.005(2) C33 0.024(3) 0.020(3) 0.027(3) 0.006(2) 0.007(2) 0.003(3) C8 0.020(3) 0.034(4) 0.032(3) 0.019(3) 0.010(3) 0.005(3) C34 0.015(3) 0.020(3) 0.029(3) 0.006(2) 0.000(2) -0.003(2) C2 0.015(3) 0.021(3) 0.024(3) 0.002(2) 0.009(2) 0.001(2) C1 0.031(3) 0.016(3) 0.018(3) 0.002(2) 0.004(2) -0.003(3) C21 0.032(4) 0.019(3) 0.025(3) 0.003(2) 0.004(3) 0.006(3) C9 0.024(3) 0.029(4) 0.023(3) 0.008(3) 0.010(2) -0.002(3) C29 0.024(3) 0.022(3) 0.024(3) 0.004(2) 0.008(2) 0.000(3) C22 0.024(3) 0.029(3) 0.017(3) 0.007(2) 0.001(2) 0.002(3) C26 0.028(3) 0.026(3) 0.023(3) 0.001(3) 0.001(3) 0.003(3) C14 0.011(3) 0.019(3) 0.028(3) 0.004(2) 0.005(2) 0.002(2) C3 0.013(3) 0.019(3) 0.030(3) 0.003(2) 0.003(2) 0.002(2) C7 0.020(3) 0.021(3) 0.027(3) 0.008(2) 0.005(2) 0.006(2) C35 0.013(3) 0.026(3) 0.039(4) 0.010(3) 0.008(3) -0.001(2) C27 0.034(4) 0.012(3) 0.028(3) -0.002(2) -0.013(3) 0.004(3) C36 0.012(3) 0.024(3) 0.030(3) 0.001(2) 0.006(2) 0.002(2) C25 0.013(3) 0.026(3) 0.025(3) -0.001(2) 0.003(2) 0.003(2) C28 0.020(3) 0.022(3) 0.037(4) 0.007(3) -0.001(3) -0.004(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 Dy1 O5 2.273(4) . ? Dy1 OW1 2.354(4) . ? Dy1 O4 2.427(4) . ? Dy1 O2 2.441(4) . ? Dy1 O3 2.485(4) . ? Dy1 O1 2.484(4) . ? Dy1 N1 2.515(4) . ? Dy1 N3 2.542(4) . ? Dy1 N2 2.575(4) . ? Dy1 C16 2.814(5) . ? Dy1 C23 2.825(5) . ? Cl3 C34 1.747(6) . ? Cl2 C27 1.737(6) . ? Cl1 C20 1.733(6) . ? O4 C23 1.257(6) . ? O3 C23 1.272(6) . ? O1 C16 1.267(6) . ? O2 C16 1.268(6) . ? O5 C30 1.273(6) . ? N3 C15 1.339(7) . ? N3 C11 1.358(7) . ? O6 C30 1.249(6) . ? C11 C12 1.393(7) . ? C11 C10 1.484(7) . ? N2 C6 1.340(7) . ? N2 C10 1.350(6) . ? N1 C1 1.345(7) . ? N1 C5 1.354(7) . ? C5 C4 1.404(7) . ? C5 C6 1.481(7) . ? C10 C9 1.403(7) . ? C24 C29 1.390(7) . ? C24 C25 1.393(7) . ? C24 C23 1.495(7) . ? C31 C36 1.390(7) . ? C31 C32 1.396(7) . ? C31 C30 1.493(7) . ? C6 C7 1.389(7) . ? C4 C3 1.376(7) . ? C4 H4 0.9300 . ? C15 C14 1.386(7) . ? C15 H15 0.9300 . ? C13 C14 1.373(8) . ? C13 C12 1.383(8) . ? C13 H13 0.9300 . ? C17 C18 1.373(8) . ? C17 C22 1.424(8) . ? C17 C16 1.477(7) . ? C32 C33 1.386(8) . ? C32 H32 0.9300 . ? C20 C21 1.373(8) . ? C20 C19 1.391(8) . ? C18 C19 1.387(8) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C12 H12 0.9300 . ? C33 C34 1.379(8) . ? C33 H33 0.9300 . ? C8 C7 1.374(8) . ? C8 C9 1.380(8) . ? C8 H8 0.9300 . ? C34 C35 1.387(8) . ? C2 C3 1.380(8) . ? C2 C1 1.386(8) . ? C2 H2 0.9300 . ? C1 H1 0.9300 . ? C21 C22 1.366(8) . ? C21 H21 0.9300 . ? C9 H9 0.9300 . ? C29 C28 1.385(8) . ? C29 H29 0.9300 . ? C22 H22 0.9300 . ? C26 C27 1.390(8) . ? C26 C25 1.389(8) . ? C26 H26 0.9300 . ? C14 H14 0.9300 . ? C3 H3 0.9300 . ? C7 H7 0.9300 . ? C35 C36 1.379(8) . ? C35 H35 0.9300 . ? C27 C28 1.388(9) . ? C36 H36 0.9300 . ? C25 H25 0.9300 . ? C28 H28 0.9300 . ? 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 Dy1 OW1 84.95(13) . . ? O5 Dy1 O4 134.06(12) . . ? OW1 Dy1 O4 80.93(12) . . ? O5 Dy1 O2 75.55(13) . . ? OW1 Dy1 O2 75.31(12) . . ? O4 Dy1 O2 139.97(12) . . ? O5 Dy1 O3 81.13(13) . . ? OW1 Dy1 O3 75.93(12) . . ? O4 Dy1 O3 53.07(11) . . ? O2 Dy1 O3 144.21(12) . . ? O5 Dy1 O1 83.03(13) . . ? OW1 Dy1 O1 128.79(12) . . ? O4 Dy1 O1 138.10(12) . . ? O2 Dy1 O1 53.48(12) . . ? O3 Dy1 O1 149.09(12) . . ? O5 Dy1 N1 81.42(14) . . ? OW1 Dy1 N1 145.59(13) . . ? O4 Dy1 N1 86.16(13) . . ? O2 Dy1 N1 130.29(13) . . ? O3 Dy1 N1 70.85(13) . . ? O1 Dy1 N1 80.67(13) . . ? O5 Dy1 N3 144.18(14) . . ? OW1 Dy1 N3 79.16(13) . . ? O4 Dy1 N3 74.79(13) . . ? O2 Dy1 N3 69.45(13) . . ? O3 Dy1 N3 124.65(13) . . ? O1 Dy1 N3 82.36(13) . . ? N1 Dy1 N3 127.75(14) . . ? O5 Dy1 N2 139.22(13) . . ? OW1 Dy1 N2 135.82(13) . . ? O4 Dy1 N2 67.18(12) . . ? O2 Dy1 N2 110.31(13) . . ? O3 Dy1 N2 105.11(13) . . ? O1 Dy1 N2 71.30(13) . . ? N1 Dy1 N2 63.89(13) . . ? N3 Dy1 N2 63.87(14) . . ? O5 Dy1 C16 77.26(14) . . ? OW1 Dy1 C16 102.04(15) . . ? O4 Dy1 C16 148.47(13) . . ? O2 Dy1 C16 26.74(14) . . ? O3 Dy1 C16 158.40(13) . . ? O1 Dy1 C16 26.76(14) . . ? N1 Dy1 C16 105.48(15) . . ? N3 Dy1 C16 75.01(14) . . ? N2 Dy1 C16 91.37(15) . . ? O5 Dy1 C23 107.81(14) . . ? OW1 Dy1 C23 77.04(14) . . ? O4 Dy1 C23 26.33(13) . . ? O2 Dy1 C23 151.73(14) . . ? O3 Dy1 C23 26.74(13) . . ? O1 Dy1 C23 153.55(13) . . ? N1 Dy1 C23 77.35(14) . . ? N3 Dy1 C23 99.65(14) . . ? N2 Dy1 C23 85.80(14) . . ? C16 Dy1 C23 174.64(14) . . ? C23 O4 Dy1 94.8(3) . . ? C23 O3 Dy1 91.7(3) . . ? C16 O1 Dy1 91.3(3) . . ? C16 O2 Dy1 93.3(3) . . ? C30 O5 Dy1 170.4(4) . . ? C15 N3 C11 117.8(4) . . ? C15 N3 Dy1 120.0(3) . . ? C11 N3 Dy1 122.1(3) . . ? N3 C11 C12 121.5(5) . . ? N3 C11 C10 115.7(5) . . ? C12 C11 C10 122.7(5) . . ? C6 N2 C10 119.0(4) . . ? C6 N2 Dy1 120.1(3) . . ? C10 N2 Dy1 119.9(3) . . ? C1 N1 C5 117.9(5) . . ? C1 N1 Dy1 120.1(4) . . ? C5 N1 Dy1 121.9(3) . . ? N1 C5 C4 120.9(5) . . ? N1 C5 C6 116.7(5) . . ? C4 C5 C6 122.4(5) . . ? N2 C10 C9 121.6(5) . . ? N2 C10 C11 117.7(5) . . ? C9 C10 C11 120.7(5) . . ? C29 C24 C25 119.0(5) . . ? C29 C24 C23 120.3(5) . . ? C25 C24 C23 120.7(5) . . ? C36 C31 C32 118.4(5) . . ? C36 C31 C30 121.1(5) . . ? C32 C31 C30 120.5(5) . . ? N2 C6 C7 121.9(5) . . ? N2 C6 C5 116.4(5) . . ? C7 C6 C5 121.7(5) . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? N3 C15 C14 123.4(5) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? O6 C30 O5 125.4(5) . . ? O6 C30 C31 117.3(5) . . ? O5 C30 C31 117.2(5) . . ? C14 C13 C12 119.1(5) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C18 C17 C22 118.4(5) . . ? C18 C17 C16 122.4(5) . . ? C22 C17 C16 119.3(5) . . ? O4 C23 O3 120.5(5) . . ? O4 C23 C24 120.0(5) . . ? O3 C23 C24 119.5(5) . . ? O4 C23 Dy1 58.9(3) . . ? O3 C23 Dy1 61.6(3) . . ? C24 C23 Dy1 177.8(4) . . ? C33 C32 C31 121.3(5) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C21 C20 C19 120.5(5) . . ? C21 C20 Cl1 120.7(5) . . ? C19 C20 Cl1 118.8(5) . . ? O1 C16 O2 121.9(5) . . ? O1 C16 C17 119.9(5) . . ? O2 C16 C17 118.1(5) . . ? O1 C16 Dy1 62.0(3) . . ? O2 C16 Dy1 60.0(3) . . ? C17 C16 Dy1 177.3(4) . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C20 119.1(5) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C13 C12 C11 119.4(5) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C34 C33 C32 118.6(5) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C7 C8 C9 119.5(5) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C33 C34 C35 121.6(5) . . ? C33 C34 Cl3 119.6(4) . . ? C35 C34 Cl3 118.8(4) . . ? C3 C2 C1 118.2(5) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? N1 C1 C2 123.7(5) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C22 C21 C20 120.4(6) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C8 C9 C10 118.6(5) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C28 C29 C24 121.1(5) . . ? C28 C29 H29 119.4 . . ? C24 C29 H29 119.4 . . ? C21 C22 C17 120.2(5) . . ? C21 C22 H22 119.9 . . ? C17 C22 H22 119.9 . . ? C27 C26 C25 118.4(5) . . ? C27 C26 H26 120.8 . . ? C25 C26 H26 120.8 . . ? C13 C14 C15 118.7(5) . . ? C13 C14 H14 120.7 . . ? C15 C14 H14 120.7 . . ? C4 C3 C2 119.2(5) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C8 C7 C6 119.4(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C36 C35 C34 119.0(5) . . ? C36 C35 H35 120.5 . . ? C34 C35 H35 120.5 . . ? C26 C27 C28 121.8(5) . . ? C26 C27 Cl2 119.2(5) . . ? C28 C27 Cl2 119.0(5) . . ? C35 C36 C31 121.2(5) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C26 C25 C24 121.0(5) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C29 C28 C27 118.6(6) . . ? C29 C28 H28 120.7 . . ? C27 C28 H28 120.7 . . ? _refine_diff_density_max 1.154 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.166 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1_twin in P-1 CELL 0.71073 8.6890 13.1090 14.7710 100.206 97.819 92.396 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N O CL DY UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 BOND $H ACTA 51.00 L.S. 12 WGHT 0.045200 FVAR 0.12351 DY1 6 0.562910 0.513205 0.701475 11.00000 0.01379 0.01588 = 0.01665 0.00301 0.00392 0.00028 CL3 5 1.209679 1.025537 0.743294 11.00000 0.03731 0.02508 = 0.03982 0.00291 0.00751 -0.00875 CL2 5 0.249154 -0.099731 0.356278 11.00000 0.05003 0.02057 = 0.04578 -0.00653 -0.00939 0.00015 CL1 5 0.796507 1.120070 1.070618 11.00000 0.03389 0.02133 = 0.02977 0.00064 -0.00097 0.00268 O4 4 0.405999 0.349671 0.660828 11.00000 0.01523 0.01573 = 0.01858 0.00317 0.00376 0.00057 O3 4 0.561543 0.376955 0.560990 11.00000 0.01792 0.02039 = 0.02081 0.00467 0.00746 -0.00239 O1 4 0.710476 0.624384 0.842981 11.00000 0.01883 0.01435 = 0.02122 0.00285 0.00346 0.00063 OW1 4 0.367708 0.558597 0.591610 11.00000 0.01508 0.02326 = 0.01863 0.00632 0.00536 0.00432 O2 4 0.535835 0.697674 0.755810 11.00000 0.01916 0.01799 = 0.02177 0.00121 0.00476 0.00017 O5 4 0.730244 0.595693 0.628188 11.00000 0.02018 0.02194 = 0.02258 0.00757 0.00788 -0.00016 N3 3 0.339608 0.538066 0.796258 11.00000 0.01622 0.01439 = 0.01615 -0.00017 0.00397 -0.00133 O6 4 0.848750 0.580954 0.501298 11.00000 0.02214 0.02926 = 0.01974 0.00563 0.00630 -0.00680 C11 1 0.327610 0.488542 0.868586 11.00000 0.01222 0.01340 = 0.02321 -0.00987 -0.00325 0.00016 N2 3 0.570433 0.414110 0.837591 11.00000 0.01134 0.01287 = 0.01717 0.00200 0.00118 0.00035 N1 3 0.792389 0.405414 0.726176 11.00000 0.01380 0.01586 = 0.01941 0.00149 0.00403 -0.00106 C5 1 0.809531 0.349086 0.794984 11.00000 0.01461 0.01040 = 0.02041 0.00112 0.00463 -0.00215 C10 1 0.449453 0.415553 0.886205 11.00000 0.01095 0.01351 = 0.01754 -0.00048 0.00577 -0.00008 C24 1 0.406172 0.216068 0.528117 11.00000 0.01753 0.01522 = 0.01801 0.00294 -0.00143 0.00352 C31 1 0.921767 0.725910 0.619886 11.00000 0.01393 0.01623 = 0.02106 0.00977 0.00059 0.00091 C6 1 0.679797 0.346804 0.850173 11.00000 0.01397 0.01602 = 0.01524 -0.00211 0.00051 -0.00170 C4 1 0.942811 0.294069 0.810708 11.00000 0.01823 0.01940 = 0.01781 0.00773 0.00191 0.00082 AFIX 43 H4 2 0.953738 0.256410 0.858701 11.00000 -1.20000 AFIX 0 C15 1 0.228566 0.601451 0.775315 11.00000 0.01957 0.01062 = 0.02644 0.00194 0.00550 0.00013 AFIX 43 H15 2 0.237103 0.636710 0.726664 11.00000 -1.20000 AFIX 0 C30 1 0.826755 0.626705 0.579643 11.00000 0.01143 0.01944 = 0.02226 0.01005 -0.00039 0.00440 C13 1 0.090770 0.568103 0.896303 11.00000 0.01467 0.02275 = 0.03011 0.00051 0.00943 -0.00109 AFIX 43 H13 2 0.007273 0.577813 0.929469 11.00000 -1.20000 AFIX 0 C17 1 0.683874 0.805695 0.885710 11.00000 0.02169 0.01794 = 0.01803 0.00573 0.00744 -0.00572 C23 1 0.459066 0.320210 0.586164 11.00000 0.01222 0.01846 = 0.01449 0.00557 0.00032 0.00364 C32 1 0.872671 0.797632 0.690066 11.00000 0.01433 0.02043 = 0.02001 0.00965 0.00250 0.00246 AFIX 43 H32 2 0.780297 0.782895 0.711885 11.00000 -1.20000 AFIX 0 C20 1 0.753032 1.000389 0.997793 11.00000 0.02406 0.01895 = 0.02552 0.00093 0.00572 -0.00121 C16 1 0.642008 0.703442 0.824855 11.00000 0.01602 0.01468 = 0.02108 0.00192 0.01574 -0.00168 C18 1 0.805843 0.821447 0.957382 11.00000 0.02928 0.02245 = 0.02616 0.00561 0.00592 -0.00081 AFIX 43 H18 2 0.866042 0.766453 0.967630 11.00000 -1.20000 AFIX 0 C19 1 0.841064 0.917733 1.014800 11.00000 0.01913 0.02737 = 0.02623 0.00318 0.00167 0.00168 AFIX 43 H19 2 0.922442 0.926919 1.064013 11.00000 -1.20000 AFIX 0 C12 1 0.205740 0.504004 0.920734 11.00000 0.01899 0.01837 = 0.02585 0.00426 0.01427 0.00472 AFIX 43 H12 2 0.201697 0.471517 0.971537 11.00000 -1.20000 AFIX 0 C33 1 0.958933 0.890371 0.727848 11.00000 0.02375 0.02015 = 0.02711 0.00627 0.00666 0.00298 AFIX 43 H33 2 0.925132 0.937843 0.774398 11.00000 -1.20000 AFIX 0 C8 1 0.548100 0.278467 0.960180 11.00000 0.01962 0.03426 = 0.03250 0.01856 0.01045 0.00510 AFIX 43 H8 2 0.540602 0.232313 1.000734 11.00000 -1.20000 AFIX 0 C34 1 1.095984 0.910768 0.694946 11.00000 0.01530 0.02023 = 0.02864 0.00624 0.00025 -0.00264 C2 1 1.038159 0.351185 0.683427 11.00000 0.01456 0.02097 = 0.02411 0.00158 0.00936 0.00100 AFIX 43 H2 2 1.113416 0.353261 0.644521 11.00000 -1.20000 AFIX 0 C1 1 0.903782 0.403498 0.671079 11.00000 0.03069 0.01615 = 0.01832 0.00221 0.00397 -0.00264 AFIX 43 H1 2 0.889826 0.439324 0.621890 11.00000 -1.20000 AFIX 0 C21 1 0.633279 0.987044 0.924911 11.00000 0.03155 0.01900 = 0.02546 0.00293 0.00431 0.00646 AFIX 43 H21 2 0.577600 1.043401 0.912819 11.00000 -1.20000 AFIX 0 C9 1 0.436141 0.348782 0.949597 11.00000 0.02406 0.02919 = 0.02267 0.00780 0.01040 -0.00189 AFIX 43 H9 2 0.353590 0.351828 0.983784 11.00000 -1.20000 AFIX 0 C29 1 0.291765 0.154015 0.553467 11.00000 0.02361 0.02201 = 0.02439 0.00395 0.00822 0.00002 AFIX 43 H29 2 0.248163 0.177881 0.606761 11.00000 -1.20000 AFIX 0 C22 1 0.595402 0.891560 0.870065 11.00000 0.02432 0.02924 = 0.01650 0.00728 0.00072 0.00199 AFIX 43 H22 2 0.511569 0.882590 0.822353 11.00000 -1.20000 AFIX 0 C26 1 0.425290 0.081836 0.395228 11.00000 0.02784 0.02578 = 0.02271 0.00132 0.00052 0.00300 AFIX 43 H26 2 0.469853 0.057325 0.342442 11.00000 -1.20000 AFIX 0 C14 1 0.101586 0.617199 0.822423 11.00000 0.01144 0.01946 = 0.02850 0.00449 0.00451 0.00235 AFIX 43 H14 2 0.025231 0.660161 0.804355 11.00000 -1.20000 AFIX 0 C3 1 1.057284 0.295933 0.755007 11.00000 0.01330 0.01872 = 0.02951 0.00287 0.00314 0.00211 AFIX 43 H3 2 1.146465 0.260372 0.765495 11.00000 -1.20000 AFIX 0 C7 1 0.670699 0.277185 0.910346 11.00000 0.01977 0.02078 = 0.02703 0.00828 0.00464 0.00579 AFIX 43 H7 2 0.746864 0.230163 0.916833 11.00000 -1.20000 AFIX 0 C35 1 1.146981 0.841757 0.624495 11.00000 0.01303 0.02553 = 0.03926 0.00992 0.00757 -0.00130 AFIX 43 H35 2 1.239069 0.856991 0.602582 11.00000 -1.20000 AFIX 0 C27 1 0.311143 0.021628 0.422885 11.00000 0.03379 0.01155 = 0.02808 -0.00250 -0.01330 0.00444 C36 1 1.059011 0.750211 0.587453 11.00000 0.01170 0.02353 = 0.03003 0.00074 0.00642 0.00197 AFIX 43 H36 2 1.092150 0.703843 0.539858 11.00000 -1.20000 AFIX 0 C25 1 0.471170 0.179473 0.448328 11.00000 0.01297 0.02601 = 0.02474 -0.00111 0.00301 0.00301 AFIX 43 H25 2 0.546464 0.221086 0.430348 11.00000 -1.20000 AFIX 0 C28 1 0.241600 0.057218 0.500680 11.00000 0.01976 0.02212 = 0.03683 0.00666 -0.00117 -0.00432 AFIX 43 H28 2 0.162928 0.016908 0.517039 11.00000 -1.20000 AFIX 0 HKLF 4 REM Pbar1_twin in P-1 REM R1 = 0.0460 for 5354 Fo > 4sig(Fo) and 0.0635 for all 6703 data REM 451 parameters refined using 0 restraints END WGHT 0.0427 0.0000 REM Highest difference peak 1.154, deepest hole -0.880, 1-sigma level 0.166 Q1 1 0.3061 0.4476 0.8966 11.00000 0.05 1.15 Q2 1 0.3928 0.9252 0.7578 11.00000 0.05 0.87 Q3 1 0.4120 0.5682 0.5430 11.00000 0.05 0.80 Q4 1 0.9011 1.1312 1.0385 11.00000 0.05 0.77 Q5 1 0.6731 0.9420 0.8586 11.00000 0.05 0.67 Q6 1 1.3438 1.0219 0.7596 11.00000 0.05 0.67 Q7 1 0.2891 0.4871 0.5202 11.00000 0.05 0.65 Q8 1 1.1498 1.1015 0.7857 11.00000 0.05 0.65 Q9 1 0.2876 0.4963 0.5631 11.00000 0.05 0.65 Q10 1 0.2746 0.4867 0.8347 11.00000 0.05 0.65 ; _shelx_res_checksum 2219 _shelx_hkl_file ; 1 0 0 315.95 6.61 2 0 0 0.83 0.55 3 0 0 101.45 3.30 4 0 0 0.56 0.88 5 0 0 49.40 2.41 6 0 0 112.89 5.80 7 0 0 35.63 3.64 8 0 0 155.02 8.07 9 0 0 75.32 5.92 10 0 0 22.40 5.38 -10 1 0 9.89 3.40 -9 1 0 33.33 3.71 -8 1 0 154.23 6.72 -7 1 0 69.69 4.87 -6 1 0 9.90 1.66 -5 1 0 1.06 1.14 -4 1 0 8.08 1.14 -3 1 0 51.49 1.63 -2 1 0 569.35 7.28 -1 1 0 406.71 4.20 0 1 0 373.50 6.09 1 1 0 261.76 3.13 2 1 0 137.63 3.14 3 1 0 11.34 1.64 4 1 0 46.19 3.04 5 1 0 3.96 1.65 6 1 0 83.49 4.98 7 1 0 117.46 6.48 8 1 0 42.72 4.27 9 1 0 54.92 5.16 10 1 0 30.01 4.46 -10 2 0 3.12 2.38 -9 2 0 45.47 4.35 -8 2 0 54.39 3.41 -7 2 0 35.78 2.82 -6 2 0 27.21 1.86 -5 2 0 19.74 1.31 -4 2 0 14.78 1.08 -3 2 0 7.88 0.80 -2 2 0 12.39 0.77 -1 2 0 178.01 2.34 0 2 0 361.68 4.88 1 2 0 169.10 2.67 2 2 0 5.87 0.64 3 2 0 72.44 2.62 4 2 0 5.84 1.20 5 2 0 114.73 5.64 6 2 0 86.15 5.16 7 2 0 50.19 4.35 8 2 0 22.96 3.52 9 2 0 76.55 6.15 10 2 0 12.68 3.77 -10 3 0 6.51 2.67 -9 3 0 32.92 3.83 -8 3 0 98.07 5.89 -7 3 0 15.83 1.90 -6 3 0 2.14 0.88 -5 3 0 1.91 0.75 -4 3 0 0.28 0.59 -3 3 0 53.45 1.60 -2 3 0 93.31 1.54 -1 3 0 58.37 1.18 0 3 0 23.58 0.99 1 3 0 177.03 2.77 2 3 0 1.98 0.57 3 3 0 10.43 0.87 4 3 0 13.89 1.74 5 3 0 32.57 2.79 6 3 0 58.48 4.34 7 3 0 127.15 7.06 8 3 0 2.67 3.37 9 3 0 35.51 6.00 10 3 0 9.38 4.62 -10 4 0 28.43 4.03 -9 4 0 46.15 4.60 -8 4 0 56.25 4.66 -7 4 0 9.45 1.63 -6 4 0 1.87 0.86 -5 4 0 1.17 0.69 -4 4 0 0.86 0.59 -3 4 0 12.27 0.83 -2 4 0 140.43 2.75 -1 4 0 144.04 2.47 0 4 0 4.38 0.68 1 4 0 159.74 2.78 2 4 0 88.00 2.05 3 4 0 3.33 0.70 4 4 0 11.94 0.93 5 4 0 17.21 2.21 6 4 0 77.24 3.79 7 4 0 25.97 2.54 8 4 0 28.25 2.82 9 4 0 19.54 3.49 10 4 0 8.95 4.34 -10 5 0 40.65 4.66 -9 5 0 44.03 4.57 -8 5 0 47.42 4.33 -7 5 0 11.87 1.83 -6 5 0 15.63 1.84 -5 5 0 2.51 0.77 -4 5 0 89.49 2.17 -3 5 0 0.78 0.84 -2 5 0 90.07 1.78 -1 5 0 184.52 3.13 0 5 0 92.59 2.11 1 5 0 34.73 1.51 2 5 0 190.08 3.41 3 5 0 3.28 0.79 4 5 0 45.03 1.87 5 5 0 34.49 2.42 6 5 0 50.90 3.15 7 5 0 28.30 2.66 8 5 0 65.07 4.03 9 5 0 6.88 2.06 -10 6 0 13.35 3.36 -9 6 0 32.12 4.11 -8 6 0 44.72 4.38 -7 6 0 18.91 2.24 -6 6 0 13.24 1.89 -5 6 0 1.62 1.08 -4 6 0 19.97 2.00 -3 6 0 139.14 3.75 -2 6 0 90.24 2.38 -1 6 0 30.46 1.44 0 6 0 59.33 1.99 1 6 0 411.67 5.99 2 6 0 3.91 0.83 3 6 0 49.85 2.07 4 6 0 9.38 1.10 5 6 0 76.58 3.65 6 6 0 33.83 2.69 7 6 0 48.64 3.40 8 6 0 40.13 3.36 9 6 0 16.69 2.66 -9 7 0 33.76 4.22 -8 7 0 4.02 2.21 -7 7 0 38.55 3.02 -6 7 0 12.46 1.87 -5 7 0 27.71 2.35 -4 7 0 74.98 3.80 -3 7 0 41.15 2.48 -2 7 0 76.08 2.13 -1 7 0 366.83 5.61 0 7 0 50.51 2.03 1 7 0 0.72 0.67 2 7 0 14.79 1.28 3 7 0 0.46 0.72 4 7 0 87.66 2.84 5 7 0 138.71 4.77 6 7 0 47.24 3.26 7 7 0 90.11 4.68 8 7 0 96.94 5.65 9 7 0 8.20 2.34 -9 8 0 35.43 4.35 -8 8 0 70.10 4.31 -7 8 0 8.36 1.92 -6 8 0 3.33 1.46 -5 8 0 1.19 1.17 -4 8 0 93.02 4.03 -3 8 0 223.60 5.39 -2 8 0 34.86 1.69 -1 8 0 17.27 1.33 0 8 0 134.95 3.11 1 8 0 56.07 2.31 2 8 0 15.17 1.38 3 8 0 78.71 2.92 4 8 0 21.28 1.67 5 8 0 83.46 4.07 6 8 0 88.30 4.47 7 8 0 24.10 2.78 8 8 0 8.37 2.26 -9 9 0 48.82 5.36 -8 9 0 30.94 3.18 -7 9 0 31.61 2.95 -6 9 0 2.21 1.54 -5 9 0 44.45 3.52 -4 9 0 21.05 2.20 -3 9 0 47.43 2.94 -2 9 0 95.03 2.81 -1 9 0 83.45 2.79 0 9 0 33.36 1.90 1 9 0 5.94 1.07 2 9 0 1.45 0.94 3 9 0 0.52 0.89 4 9 0 19.77 1.78 5 9 0 34.71 2.89 6 9 0 21.13 2.54 7 9 0 16.41 2.76 8 9 0 18.72 3.68 -8 10 0 22.94 4.12 -7 10 0 4.97 3.87 -6 10 0 3.95 2.55 -5 10 0 10.06 2.38 -4 10 0 61.49 3.62 -3 10 0 66.23 3.59 -2 10 0 35.71 2.65 -1 10 0 68.08 2.76 0 10 0 141.63 3.61 1 10 0 6.28 1.20 2 10 0 0.80 0.98 3 10 0 0.86 1.00 4 10 0 8.96 1.93 5 10 0 41.49 4.16 6 10 0 61.32 5.30 7 10 0 29.80 4.17 -8 11 0 22.72 3.92 -7 11 0 0.00 3.74 -6 11 0 2.64 3.52 -5 11 0 5.41 3.67 -4 11 0 20.21 3.59 -3 11 0 107.10 4.79 -2 11 0 74.65 3.80 -1 11 0 56.79 3.04 0 11 0 8.71 1.38 1 11 0 1.94 1.13 2 11 0 2.26 1.24 3 11 0 7.52 1.68 4 11 0 8.89 2.46 5 11 0 25.34 3.57 6 11 0 26.32 3.89 7 11 0 30.46 4.40 -7 12 0 10.88 3.52 -6 12 0 4.55 3.27 -5 12 0 22.60 4.67 -4 12 0 23.91 4.49 -3 12 0 34.47 3.37 -2 12 0 85.69 4.42 -1 12 0 39.85 4.15 0 12 0 19.30 3.73 1 12 0 5.43 2.48 2 12 0 5.32 2.12 3 12 0 2.18 1.86 4 12 0 17.56 3.15 5 12 0 36.25 4.54 6 12 0 66.47 5.79 -6 13 0 0.00 3.29 -5 13 0 0.00 3.67 -4 13 0 44.08 5.14 -3 13 0 59.72 4.39 -2 13 0 42.78 5.92 -1 13 0 24.98 4.52 0 13 0 41.30 4.90 1 13 0 0.00 3.46 2 13 0 20.12 4.20 3 13 0 7.01 2.88 4 13 0 37.04 5.40 5 13 0 43.23 5.20 -5 14 0 26.37 4.86 -4 14 0 3.81 4.00 -3 14 0 45.35 5.49 -2 14 0 47.14 5.67 -1 14 0 9.12 4.72 0 14 0 4.85 4.74 1 14 0 3.87 4.60 2 14 0 4.71 3.42 3 14 0 44.20 5.68 4 14 0 32.91 5.07 -4 15 0 29.53 5.79 -3 15 0 50.75 6.01 -2 15 0 35.76 5.67 -1 15 0 32.56 6.09 0 15 0 17.10 5.11 1 15 0 4.54 5.36 2 15 0 4.37 5.50 3 15 0 9.41 3.77 -2 16 0 22.90 5.74 -1 16 0 4.09 3.76 0 16 0 3.62 3.58 -1 -16 1 15.74 4.42 0 -16 1 1.70 5.16 1 -16 1 56.93 6.32 2 -16 1 20.08 4.78 -3 -15 1 7.76 4.92 -2 -15 1 19.53 5.10 -1 -15 1 26.55 5.39 0 -15 1 11.56 4.81 1 -15 1 37.71 5.97 2 -15 1 8.10 5.08 3 -15 1 6.52 5.14 4 -15 1 12.20 5.43 -4 -14 1 0.48 4.88 -3 -14 1 8.93 5.42 -2 -14 1 12.68 3.32 -1 -14 1 3.30 4.06 0 -14 1 16.85 4.62 1 -14 1 31.85 5.03 2 -14 1 11.48 4.51 3 -14 1 10.90 4.35 4 -14 1 2.68 3.17 5 -14 1 0.00 3.92 6 -14 1 25.39 7.16 -5 -13 1 5.29 5.77 -4 -13 1 4.54 4.91 -3 -13 1 2.70 3.07 -2 -13 1 37.08 3.87 -1 -13 1 43.56 3.66 0 -13 1 6.75 3.11 1 -13 1 5.65 3.00 2 -13 1 69.46 4.79 3 -13 1 0.00 2.81 4 -13 1 0.99 3.79 5 -13 1 6.17 3.21 6 -13 1 10.05 3.28 -6 -12 1 17.91 4.50 -5 -12 1 3.85 2.63 -4 -12 1 25.74 4.01 -3 -12 1 18.20 3.18 -2 -12 1 0.00 2.70 -1 -12 1 46.46 3.06 0 -12 1 98.77 4.44 1 -12 1 35.86 3.57 2 -12 1 4.08 4.29 3 -12 1 0.01 3.43 4 -12 1 8.50 3.07 5 -12 1 11.74 4.72 6 -12 1 13.86 3.74 7 -12 1 22.81 3.75 -7 -11 1 61.93 5.65 -6 -11 1 0.97 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158.80 3.06 3 5 1 98.45 2.45 4 5 1 61.67 2.18 5 5 1 106.33 3.93 6 5 1 60.66 3.44 7 5 1 0.76 1.34 8 5 1 2.01 1.62 9 5 1 2.18 1.79 -10 6 1 6.65 2.85 -9 6 1 1.30 2.11 -8 6 1 10.77 2.56 -7 6 1 10.75 1.84 -6 6 1 76.51 3.77 -5 6 1 158.69 4.53 -4 6 1 98.28 2.40 -3 6 1 109.91 2.57 -2 6 1 63.61 2.61 -1 6 1 4.05 0.78 0 6 1 78.52 2.13 1 6 1 10.20 1.01 2 6 1 26.58 1.49 3 6 1 154.53 3.29 4 6 1 71.94 2.53 5 6 1 2.06 1.17 6 6 1 23.48 2.39 7 6 1 53.09 3.58 8 6 1 1.28 1.59 9 6 1 25.72 3.13 -10 7 1 5.39 4.30 -9 7 1 1.57 2.02 -8 7 1 0.04 1.84 -7 7 1 28.03 2.71 -6 7 1 29.39 2.54 -5 7 1 50.94 3.06 -4 7 1 131.73 4.68 -3 7 1 42.63 1.65 -2 7 1 47.81 1.85 -1 7 1 1.89 0.74 0 7 1 1.25 0.71 1 7 1 82.18 2.52 2 7 1 60.50 2.34 3 7 1 34.96 1.88 4 7 1 42.83 2.14 5 7 1 149.76 5.17 6 7 1 90.60 4.42 7 7 1 0.90 1.45 8 7 1 0.52 1.69 9 7 1 6.93 3.06 -9 8 1 2.64 2.49 -8 8 1 3.01 1.78 -7 8 1 4.41 1.68 -6 8 1 26.70 2.55 -5 8 1 85.15 4.09 -4 8 1 73.53 4.07 -3 8 1 44.19 2.30 -2 8 1 41.92 1.92 -1 8 1 5.76 0.98 0 8 1 48.05 2.11 1 8 1 13.94 1.29 2 8 1 81.39 2.78 3 8 1 162.34 3.69 4 8 1 57.58 2.59 5 8 1 5.83 1.59 6 8 1 3.68 1.62 7 8 1 3.56 1.90 8 8 1 9.79 3.09 -9 9 1 6.26 2.70 -8 9 1 15.10 2.44 -7 9 1 44.05 3.43 -6 9 1 24.94 2.63 -5 9 1 27.56 2.55 -4 9 1 71.37 3.73 -3 9 1 66.36 3.46 -2 9 1 5.65 1.03 -1 9 1 1.73 0.85 0 9 1 2.81 0.93 1 9 1 82.58 2.87 2 9 1 84.99 3.00 3 9 1 29.47 1.95 4 9 1 53.04 2.63 5 9 1 30.62 3.02 6 9 1 1.58 2.02 7 9 1 1.23 2.23 8 9 1 2.23 2.48 -8 10 1 5.02 3.70 -7 10 1 4.95 2.67 -6 10 1 49.81 3.55 -5 10 1 100.66 4.69 -4 10 1 31.54 2.93 -3 10 1 41.76 2.91 -2 10 1 40.21 2.43 -1 10 1 0.93 0.93 0 10 1 69.35 2.81 1 10 1 62.51 2.73 2 10 1 87.58 3.47 3 10 1 120.44 4.89 4 10 1 22.49 3.10 5 10 1 14.92 2.99 6 10 1 2.43 2.46 7 10 1 0.60 2.25 -8 11 1 2.15 3.90 -7 11 1 20.44 3.67 -6 11 1 27.31 3.36 -5 11 1 32.63 3.41 -4 11 1 43.99 3.82 -3 11 1 34.61 3.15 -2 11 1 2.70 1.48 -1 11 1 20.39 1.76 0 11 1 36.17 2.41 1 11 1 46.22 3.08 2 11 1 46.01 3.18 3 11 1 79.62 4.13 4 11 1 32.12 3.72 5 11 1 1.32 2.11 6 11 1 3.87 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79.53 4.41 5 -11 2 11.65 4.07 6 -11 2 5.51 3.90 7 -11 2 18.36 4.41 8 -11 2 8.35 3.83 -8 -10 2 1.13 2.11 -7 -10 2 11.22 2.40 -6 -10 2 85.31 4.67 -5 -10 2 34.77 2.95 -4 -10 2 35.54 2.77 -3 -10 2 85.25 3.33 -2 -10 2 36.26 2.18 -1 -10 2 9.95 1.36 0 -10 2 2.94 1.00 1 -10 2 49.75 2.34 2 -10 2 87.34 4.01 3 -10 2 35.59 2.74 4 -10 2 62.53 3.71 5 -10 2 101.08 5.15 6 -10 2 22.16 3.74 7 -10 2 1.43 2.50 8 -10 2 4.66 2.75 -8 -9 2 1.24 1.91 -7 -9 2 7.17 2.07 -6 -9 2 35.61 3.09 -5 -9 2 105.43 4.70 -4 -9 2 154.04 4.01 -3 -9 2 73.05 2.91 -2 -9 2 5.55 1.14 -1 -9 2 8.15 1.20 0 -9 2 9.54 1.22 1 -9 2 80.18 2.68 2 -9 2 72.89 3.51 3 -9 2 152.10 4.79 4 -9 2 103.11 4.51 5 -9 2 35.41 2.87 6 -9 2 0.31 1.54 7 -9 2 1.10 1.52 8 -9 2 1.83 1.88 9 -9 2 7.21 3.22 -9 -8 2 1.96 1.97 -8 -8 2 0.98 1.75 -7 -8 2 33.21 3.13 -6 -8 2 46.26 3.30 -5 -8 2 64.85 3.59 -4 -8 2 52.40 2.45 -3 -8 2 42.34 2.15 -2 -8 2 20.97 1.54 -1 -8 2 6.09 1.00 0 -8 2 38.41 1.90 1 -8 2 92.42 2.60 2 -8 2 38.50 1.49 3 -8 2 59.93 3.14 4 -8 2 125.80 4.49 5 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0.57 1 -5 2 175.11 2.97 2 -5 2 254.74 5.01 3 -5 2 14.67 1.48 4 -5 2 80.28 3.32 5 -5 2 72.41 2.30 6 -5 2 0.85 1.09 7 -5 2 1.68 1.31 8 -5 2 2.42 1.96 9 -5 2 14.01 3.10 10 -5 2 55.18 5.30 -10 -4 2 5.85 4.76 -9 -4 2 3.19 4.07 -8 -4 2 24.03 4.88 -7 -4 2 22.66 2.36 -6 -4 2 77.11 3.71 -5 -4 2 26.30 2.05 -4 -4 2 30.25 1.46 -3 -4 2 20.45 1.18 -2 -4 2 21.49 1.17 -1 -4 2 35.65 1.40 0 -4 2 23.74 1.12 1 -4 2 1.12 0.49 2 -4 2 190.26 3.96 3 -4 2 188.74 3.51 4 -4 2 4.85 0.76 5 -4 2 4.58 0.89 6 -4 2 38.25 2.02 7 -4 2 4.87 1.43 8 -4 2 98.10 6.05 9 -4 2 38.25 4.31 10 -4 2 12.20 3.24 -10 -3 2 1.56 3.73 -9 -3 2 4.07 2.82 -8 -3 2 15.94 3.13 -7 -3 2 88.20 5.68 -6 -3 2 61.23 3.93 -5 -3 2 66.34 3.71 -4 -3 2 81.89 3.75 -3 -3 2 46.62 1.49 -2 -3 2 29.00 1.21 -1 -3 2 4.34 0.70 0 -3 2 61.37 1.43 1 -3 2 47.10 1.22 2 -3 2 316.27 4.77 3 -3 2 69.06 1.80 4 -3 2 64.27 2.16 5 -3 2 86.61 2.53 6 -3 2 35.01 1.94 7 -3 2 2.36 1.27 8 -3 2 7.37 2.27 9 -3 2 44.73 4.47 10 -3 2 52.65 5.06 -10 -2 2 1.35 2.52 -9 -2 2 26.96 3.88 -8 -2 2 28.48 3.54 -7 -2 2 87.05 5.47 -6 -2 2 186.00 8.03 -5 -2 2 114.02 5.51 -4 -2 2 39.74 2.55 -3 -2 2 23.79 1.02 -2 -2 2 0.43 0.58 -1 -2 2 1.38 0.51 0 -2 2 51.82 1.12 1 -2 2 346.24 4.10 2 -2 2 909.60 11.94 3 -2 2 201.49 3.32 4 -2 2 0.78 0.60 5 -2 2 67.16 2.33 6 -2 2 4.84 1.01 7 -2 2 4.27 1.35 8 -2 2 42.20 3.08 9 -2 2 37.34 4.16 10 -2 2 9.26 2.80 -10 -1 2 0.33 2.40 -9 -1 2 11.27 2.78 -8 -1 2 41.88 3.97 -7 -1 2 63.79 4.53 -6 -1 2 141.96 6.62 -5 -1 2 125.90 5.75 -4 -1 2 8.06 1.02 -3 -1 2 168.07 3.18 -2 -1 2 24.12 1.00 -1 -1 2 200.88 2.87 0 -1 2 312.53 3.74 1 -1 2 255.88 4.06 2 -1 2 20.79 1.31 3 -1 2 178.61 3.35 4 -1 2 63.12 2.11 5 -1 2 0.73 0.77 6 -1 2 2.09 0.88 7 -1 2 5.54 1.46 8 -1 2 9.76 1.91 9 -1 2 38.47 4.07 10 -1 2 17.83 3.34 -10 0 2 0.56 3.62 -9 0 2 15.31 3.31 -8 0 2 73.03 5.27 -7 0 2 15.68 2.61 -6 0 2 144.64 5.03 -5 0 2 145.59 4.86 -4 0 2 85.26 2.31 -3 0 2 0.96 0.57 -2 0 2 171.00 2.86 -1 0 2 7.73 0.52 0 0 2 156.38 2.08 1 0 2 90.57 1.61 2 0 2 34.06 1.36 3 0 2 9.56 0.98 4 0 2 121.33 2.78 5 0 2 41.77 2.22 6 0 2 2.74 1.33 7 0 2 8.35 1.88 8 0 2 7.90 2.07 9 0 2 50.97 3.71 10 0 2 24.64 3.74 -10 1 2 11.01 4.85 -9 1 2 1.24 2.62 -8 1 2 70.70 5.17 -7 1 2 53.34 4.22 -6 1 2 111.01 3.99 -5 1 2 11.91 1.18 -4 1 2 50.93 1.89 -3 1 2 10.38 1.01 -2 1 2 100.90 2.30 -1 1 2 31.29 1.01 0 1 2 283.76 3.41 1 1 2 268.50 3.55 2 1 2 86.46 1.80 3 1 2 74.27 1.84 4 1 2 27.81 1.59 5 1 2 1.44 0.87 6 1 2 0.35 1.06 7 1 2 33.75 2.96 8 1 2 45.70 3.73 9 1 2 43.82 3.74 10 1 2 40.21 3.88 -10 2 2 0.41 2.04 -9 2 2 15.31 2.94 -8 2 2 135.02 5.10 -7 2 2 96.01 3.98 -6 2 2 54.22 2.25 -5 2 2 145.64 3.08 -4 2 2 1.23 0.62 -3 2 2 12.25 0.93 -2 2 2 0.68 0.57 -1 2 2 18.93 0.77 0 2 2 277.18 4.43 1 2 2 953.11 10.96 2 2 2 3.49 0.63 3 2 2 42.00 1.53 4 2 2 101.15 2.32 5 2 2 14.23 1.01 6 2 2 26.94 2.27 7 2 2 0.98 1.21 8 2 2 47.40 3.39 9 2 2 83.17 4.71 10 2 2 30.89 3.35 -10 3 2 16.05 3.34 -9 3 2 38.72 4.11 -8 3 2 54.08 4.48 -7 3 2 212.84 4.41 -6 3 2 54.05 2.34 -5 3 2 32.42 1.69 -4 3 2 77.81 2.22 -3 3 2 16.13 1.06 -2 3 2 114.91 2.21 -1 3 2 94.27 2.05 0 3 2 2.58 0.42 1 3 2 1000.00 11.65 2 3 2 228.16 3.59 3 3 2 21.99 1.23 4 3 2 1.00 0.62 5 3 2 2.58 0.71 6 3 2 0.83 1.05 7 3 2 92.38 4.41 8 3 2 7.88 1.91 9 3 2 23.14 2.83 10 3 2 62.89 4.52 -10 4 2 12.36 3.18 -9 4 2 13.07 2.85 -8 4 2 25.50 3.25 -7 4 2 131.48 4.00 -6 4 2 54.70 2.39 -5 4 2 76.49 2.40 -4 4 2 2.90 0.77 -3 4 2 20.75 1.21 -2 4 2 5.55 0.73 -1 4 2 214.52 3.39 0 4 2 161.72 2.72 1 4 2 351.85 4.93 2 4 2 159.87 2.95 3 4 2 181.42 3.37 4 4 2 7.76 0.92 5 4 2 51.40 2.91 6 4 2 7.20 1.66 7 4 2 16.69 2.64 8 4 2 37.37 3.90 9 4 2 48.35 4.59 -10 5 2 11.24 3.07 -9 5 2 5.62 2.40 -8 5 2 27.66 3.43 -7 5 2 64.68 3.52 -6 5 2 49.09 2.60 -5 5 2 13.19 1.24 -4 5 2 5.75 0.88 -3 5 2 0.54 0.59 -2 5 2 134.40 2.32 -1 5 2 136.99 2.65 0 5 2 440.35 6.04 1 5 2 355.80 5.18 2 5 2 297.51 4.70 3 5 2 6.77 0.92 4 5 2 1.33 0.76 5 5 2 0.71 1.06 6 5 2 78.33 3.94 7 5 2 60.11 3.73 8 5 2 72.07 4.35 9 5 2 13.35 2.59 -10 6 2 4.36 2.72 -9 6 2 16.03 3.21 -8 6 2 51.96 4.54 -7 6 2 66.20 3.69 -6 6 2 44.03 2.89 -5 6 2 3.41 1.08 -4 6 2 10.58 1.04 -3 6 2 0.22 0.63 -2 6 2 90.85 2.41 -1 6 2 260.48 4.28 0 6 2 125.49 2.67 1 6 2 9.18 0.93 2 6 2 187.47 3.57 3 6 2 11.16 1.22 4 6 2 15.03 1.35 5 6 2 15.29 1.86 6 6 2 16.31 2.10 7 6 2 43.37 3.32 8 6 2 59.22 3.99 9 6 2 17.31 2.82 -9 7 2 58.43 5.16 -8 7 2 13.19 2.24 -7 7 2 87.56 4.36 -6 7 2 36.67 2.83 -5 7 2 2.62 1.25 -4 7 2 1.69 0.93 -3 7 2 6.63 1.03 -2 7 2 6.51 1.00 -1 7 2 72.33 2.25 0 7 2 169.22 3.36 1 7 2 61.95 2.11 2 7 2 51.28 2.07 3 7 2 26.19 1.66 4 7 2 0.86 0.89 5 7 2 8.07 1.62 6 7 2 19.10 2.28 7 7 2 20.00 2.56 8 7 2 21.97 3.85 9 7 2 8.47 3.14 -9 8 2 19.66 3.59 -8 8 2 65.98 4.16 -7 8 2 53.61 3.59 -6 8 2 4.51 1.62 -5 8 2 2.16 1.24 -4 8 2 21.83 2.10 -3 8 2 32.23 1.75 -2 8 2 39.01 1.93 -1 8 2 11.46 1.17 0 8 2 30.84 1.70 1 8 2 108.38 2.92 2 8 2 47.60 2.19 3 8 2 2.45 0.96 4 8 2 1.01 0.94 5 8 2 5.63 1.72 6 8 2 24.06 3.47 7 8 2 14.05 3.24 8 8 2 5.83 2.83 -9 9 2 25.32 3.95 -8 9 2 28.68 3.12 -7 9 2 8.88 2.11 -6 9 2 35.05 2.95 -5 9 2 0.72 1.23 -4 9 2 5.27 1.48 -3 9 2 0.11 1.17 -2 9 2 2.01 0.92 -1 9 2 120.01 3.18 0 9 2 76.43 2.72 1 9 2 7.83 1.13 2 9 2 45.40 2.52 3 9 2 29.04 2.45 4 9 2 12.72 2.19 5 9 2 23.57 3.31 6 9 2 12.77 3.05 7 9 2 8.01 2.89 8 9 2 18.97 3.83 -8 10 2 46.37 4.05 -7 10 2 4.65 2.02 -6 10 2 8.00 1.97 -5 10 2 4.70 1.57 -4 10 2 1.22 1.36 -3 10 2 99.51 4.63 -2 10 2 142.18 4.03 -1 10 2 0.63 0.91 0 10 2 134.69 3.87 1 10 2 116.62 4.52 2 10 2 1.78 1.31 3 10 2 1.65 1.30 4 10 2 0.36 1.77 5 10 2 4.92 2.34 6 10 2 87.59 6.49 7 10 2 7.66 3.02 -8 11 2 20.74 3.61 -7 11 2 11.80 2.91 -6 11 2 6.83 2.27 -5 11 2 4.34 1.99 -4 11 2 30.78 2.74 -3 11 2 20.37 2.57 -2 11 2 60.45 3.92 -1 11 2 78.86 3.89 0 11 2 16.33 2.08 1 11 2 19.53 2.21 2 11 2 38.45 3.00 3 11 2 0.62 1.35 4 11 2 25.16 3.54 5 11 2 21.81 3.50 6 11 2 13.21 3.28 -7 12 2 19.42 4.18 -6 12 2 13.51 3.54 -5 12 2 10.32 3.83 -4 12 2 16.91 3.74 -3 12 2 39.34 4.33 -2 12 2 16.76 3.04 -1 12 2 37.00 3.96 0 12 2 33.53 2.83 1 12 2 45.60 3.33 2 12 2 2.83 1.64 3 12 2 2.27 1.65 4 12 2 1.11 1.97 5 12 2 22.03 3.75 6 12 2 54.78 5.55 -6 13 2 7.88 4.46 -5 13 2 2.75 3.73 -4 13 2 6.46 3.36 -3 13 2 20.36 4.08 -2 13 2 58.56 5.39 -1 13 2 13.65 3.19 0 13 2 20.98 3.45 1 13 2 40.19 3.28 2 13 2 1.66 1.71 3 13 2 1.61 2.31 4 13 2 2.99 2.49 5 13 2 11.72 3.18 -5 14 2 4.16 3.58 -4 14 2 2.77 3.28 -3 14 2 7.67 3.43 -2 14 2 54.26 5.44 -1 14 2 59.57 5.27 0 14 2 17.31 3.35 1 14 2 11.81 3.02 2 14 2 4.24 2.04 3 14 2 1.26 2.35 4 14 2 1.09 2.56 -3 15 2 26.64 4.14 -2 15 2 17.86 3.55 -1 15 2 18.61 3.72 0 15 2 59.35 5.59 1 15 2 11.52 3.24 2 15 2 1.99 2.55 -1 -16 3 55.85 6.73 0 -16 3 11.12 5.54 1 -16 3 13.47 5.22 2 -16 3 28.23 5.61 -3 -15 3 2.15 9.00 -2 -15 3 2.07 4.30 -1 -15 3 13.69 4.55 0 -15 3 29.70 4.99 1 -15 3 59.57 5.85 2 -15 3 1.12 3.41 3 -15 3 12.64 3.80 4 -15 3 37.19 4.67 -5 -14 3 28.15 5.00 -4 -14 3 13.83 4.65 -3 -14 3 0.00 4.43 -2 -14 3 7.30 3.92 -1 -14 3 33.66 3.73 0 -14 3 23.99 4.22 1 -14 3 32.61 3.83 2 -14 3 67.83 4.44 3 -14 3 20.03 3.63 4 -14 3 0.00 3.18 5 -14 3 0.00 4.15 -6 -13 3 56.50 6.33 -5 -13 3 12.50 4.85 -4 -13 3 4.94 3.43 -3 -13 3 2.89 2.51 -2 -13 3 0.13 2.67 -1 -13 3 21.88 3.67 0 -13 3 38.32 3.84 1 -13 3 28.00 3.43 2 -13 3 65.77 4.19 3 -13 3 9.83 3.03 4 -13 3 8.36 3.46 5 -13 3 2.42 3.70 6 -13 3 2.35 4.85 -7 -12 3 0.74 3.49 -6 -12 3 39.70 4.87 -5 -12 3 31.65 4.40 -4 -12 3 12.01 3.91 -3 -12 3 5.82 3.02 -2 -12 3 0.00 3.22 -1 -12 3 42.30 3.30 0 -12 3 155.59 5.95 1 -12 3 54.05 4.05 2 -12 3 27.02 3.65 3 -12 3 2.88 3.46 4 -12 3 15.11 3.16 5 -12 3 3.95 3.87 6 -12 3 4.59 5.32 7 -12 3 10.90 4.07 -7 -11 3 13.32 2.77 -6 -11 3 13.50 2.36 -5 -11 3 1.29 1.47 -4 -11 3 5.99 1.60 -3 -11 3 1.21 1.10 -2 -11 3 98.95 3.92 -1 -11 3 135.31 3.95 0 -11 3 19.29 2.10 1 -11 3 12.30 2.50 2 -11 3 46.09 3.49 3 -11 3 10.96 3.26 4 -11 3 0.00 4.06 5 -11 3 2.63 4.81 6 -11 3 5.63 4.40 7 -11 3 43.07 4.45 8 -11 3 25.65 4.22 -8 -10 3 10.53 2.61 -7 -10 3 3.34 1.99 -6 -10 3 28.59 3.01 -5 -10 3 12.78 2.11 -4 -10 3 1.96 1.15 -3 -10 3 2.80 1.09 -2 -10 3 3.79 1.15 -1 -10 3 13.76 1.48 0 -10 3 182.08 4.06 1 -10 3 79.09 2.73 2 -10 3 0.27 1.05 3 -10 3 32.66 2.65 4 -10 3 8.31 1.75 5 -10 3 4.87 1.77 6 -10 3 21.92 2.95 7 -10 3 18.91 2.78 8 -10 3 26.91 3.42 -8 -9 3 71.67 4.67 -7 -9 3 78.52 4.61 -6 -9 3 9.43 1.98 -5 -9 3 7.26 1.70 -4 -9 3 29.45 2.02 -3 -9 3 8.64 1.26 -2 -9 3 80.20 3.00 -1 -9 3 39.28 2.08 0 -9 3 11.87 1.26 1 -9 3 186.23 3.84 2 -9 3 111.86 4.06 3 -9 3 21.83 2.12 4 -9 3 0.79 1.15 5 -9 3 1.00 1.31 6 -9 3 22.62 2.76 7 -9 3 44.94 3.54 8 -9 3 15.21 2.58 9 -9 3 18.00 3.55 -9 -8 3 50.69 4.17 -8 -8 3 26.09 2.96 -7 -8 3 23.05 2.63 -6 -8 3 91.48 4.48 -5 -8 3 3.68 1.38 -4 -8 3 1.39 0.92 -3 -8 3 0.50 0.79 -2 -8 3 9.65 1.16 -1 -8 3 33.56 1.81 0 -8 3 271.64 4.76 1 -8 3 58.85 2.09 2 -8 3 50.72 1.72 3 -8 3 64.01 3.26 4 -8 3 4.84 1.39 5 -8 3 44.99 3.05 6 -8 3 18.90 2.81 7 -8 3 7.37 1.88 8 -8 3 29.60 3.97 9 -8 3 5.89 2.78 -9 -7 3 17.50 2.76 -8 -7 3 43.84 3.57 -7 -7 3 61.72 3.85 -6 -7 3 30.92 2.65 -5 -7 3 13.12 1.78 -4 -7 3 10.75 1.23 -3 -7 3 37.30 1.90 -2 -7 3 164.34 3.43 -1 -7 3 53.63 2.15 0 -7 3 121.77 2.76 1 -7 3 163.23 3.21 2 -7 3 98.52 2.68 3 -7 3 19.59 1.85 4 -7 3 1.13 1.07 5 -7 3 13.56 1.89 6 -7 3 34.07 3.15 7 -7 3 70.77 4.02 8 -7 3 41.57 4.40 9 -7 3 17.03 3.32 -9 -6 3 31.26 3.19 -8 -6 3 55.83 3.82 -7 -6 3 89.84 4.46 -6 -6 3 0.80 1.17 -5 -6 3 6.62 1.37 -4 -6 3 32.96 1.73 -3 -6 3 53.09 2.11 -2 -6 3 108.65 2.56 -1 -6 3 309.75 4.88 0 -6 3 165.65 3.15 1 -6 3 99.91 2.28 2 -6 3 33.65 1.42 3 -6 3 9.62 1.35 4 -6 3 24.01 2.03 5 -6 3 48.10 2.91 6 -6 3 61.27 3.47 7 -6 3 43.55 3.12 8 -6 3 39.14 4.18 9 -6 3 23.03 3.65 -10 -5 3 16.86 3.99 -9 -5 3 37.94 4.29 -8 -5 3 41.67 3.62 -7 -5 3 39.16 3.73 -6 -5 3 29.89 3.07 -5 -5 3 0.30 0.84 -4 -5 3 61.55 2.07 -3 -5 3 92.56 2.33 -2 -5 3 92.11 2.28 -1 -5 3 357.66 5.19 0 -5 3 159.66 2.90 1 -5 3 14.10 0.95 2 -5 3 21.60 1.18 3 -5 3 62.52 2.81 4 -5 3 34.43 2.23 5 -5 3 58.81 2.36 6 -5 3 23.48 2.20 7 -5 3 142.50 5.04 8 -5 3 65.83 5.13 9 -5 3 16.53 3.18 10 -5 3 5.58 2.71 -10 -4 3 14.01 4.90 -9 -4 3 37.65 5.99 -8 -4 3 144.53 8.19 -7 -4 3 35.77 2.81 -6 -4 3 7.09 1.46 -5 -4 3 1.32 0.97 -4 -4 3 8.33 0.91 -3 -4 3 203.17 3.48 -2 -4 3 107.92 2.25 -1 -4 3 59.47 1.64 0 -4 3 54.02 1.55 1 -4 3 148.98 2.58 2 -4 3 16.58 0.92 3 -4 3 10.96 1.01 4 -4 3 11.44 1.02 5 -4 3 51.01 2.23 6 -4 3 106.33 3.10 7 -4 3 78.80 3.85 8 -4 3 22.40 3.21 9 -4 3 27.28 3.76 10 -4 3 3.02 2.57 -10 -3 3 62.73 5.93 -9 -3 3 59.79 5.46 -8 -3 3 46.51 4.55 -7 -3 3 61.83 4.80 -6 -3 3 59.33 3.78 -5 -3 3 12.26 1.65 -4 -3 3 10.15 0.86 -3 -3 3 6.08 0.74 -2 -3 3 34.66 1.31 -1 -3 3 319.40 4.34 0 -3 3 84.61 1.71 1 -3 3 129.16 2.26 2 -3 3 212.10 3.36 3 -3 3 34.84 1.45 4 -3 3 1.86 0.69 5 -3 3 6.62 0.99 6 -3 3 38.90 2.07 7 -3 3 44.86 3.25 8 -3 3 41.12 3.98 9 -3 3 5.85 2.40 10 -3 3 6.68 2.89 -10 -2 3 12.72 3.59 -9 -2 3 71.11 5.63 -8 -2 3 68.26 5.23 -7 -2 3 6.08 2.25 -6 -2 3 4.27 2.00 -5 -2 3 58.51 3.84 -4 -2 3 29.45 1.28 -3 -2 3 162.85 2.95 -2 -2 3 80.41 1.72 -1 -2 3 195.10 2.59 0 -2 3 299.29 4.16 1 -2 3 749.70 8.29 2 -2 3 75.47 1.74 3 -2 3 2.71 0.66 4 -2 3 1.01 0.62 5 -2 3 27.43 1.60 6 -2 3 89.94 2.84 7 -2 3 90.90 4.14 8 -2 3 59.25 3.99 9 -2 3 41.18 4.31 10 -2 3 1.21 2.31 -10 -1 3 31.16 4.45 -9 -1 3 46.43 4.62 -8 -1 3 3.82 2.35 -7 -1 3 78.09 5.11 -6 -1 3 16.61 2.42 -5 -1 3 7.27 0.86 -4 -1 3 138.80 3.05 -3 -1 3 30.03 1.25 -2 -1 3 799.95 9.44 -1 -1 3 990.23 9.95 0 -1 3 2.60 0.38 1 -1 3 137.37 2.29 2 -1 3 20.22 1.07 3 -1 3 5.31 0.86 4 -1 3 64.81 2.09 5 -1 3 58.10 2.17 6 -1 3 113.26 3.11 7 -1 3 84.54 4.03 8 -1 3 39.42 3.07 9 -1 3 20.78 3.29 10 -1 3 2.64 2.45 -10 0 3 29.75 4.48 -9 0 3 33.70 4.21 -8 0 3 12.17 2.89 -7 0 3 9.74 2.49 -6 0 3 28.35 2.14 -5 0 3 0.84 0.71 -4 0 3 154.37 3.13 -3 0 3 381.19 5.77 -2 0 3 79.77 1.69 -1 0 3 16.19 0.79 0 0 3 142.13 1.97 1 0 3 14.31 0.83 2 0 3 16.01 0.99 3 0 3 4.86 0.73 4 0 3 51.52 2.19 5 0 3 114.68 2.83 6 0 3 125.72 4.35 7 0 3 70.36 3.73 8 0 3 13.25 2.08 9 0 3 8.33 2.01 10 0 3 0.83 2.27 -10 1 3 14.15 5.41 -9 1 3 23.75 3.87 -8 1 3 19.74 2.91 -7 1 3 2.99 1.65 -6 1 3 9.41 1.26 -5 1 3 2.18 0.86 -4 1 3 92.82 2.58 -3 1 3 256.49 4.33 -2 1 3 229.18 3.43 -1 1 3 101.85 2.02 0 1 3 8.54 0.63 1 1 3 26.73 1.05 2 1 3 0.36 0.48 3 1 3 89.15 2.11 4 1 3 92.90 2.37 5 1 3 154.27 3.22 6 1 3 47.40 2.92 7 1 3 20.67 2.24 8 1 3 54.50 3.65 9 1 3 4.58 1.88 10 1 3 5.23 2.26 -10 2 3 29.80 3.97 -9 2 3 10.01 2.45 -8 2 3 6.43 1.65 -7 2 3 6.18 1.46 -6 2 3 1.54 0.82 -5 2 3 78.97 2.42 -4 2 3 57.58 2.04 -3 2 3 58.19 1.82 -2 2 3 144.29 2.56 -1 2 3 62.44 1.35 0 2 3 36.47 1.62 1 2 3 75.60 1.61 2 2 3 40.33 1.49 3 2 3 149.84 3.06 4 2 3 22.16 1.33 5 2 3 100.22 2.70 6 2 3 85.33 3.92 7 2 3 17.81 2.19 8 2 3 4.78 1.63 9 2 3 6.16 2.00 10 2 3 0.53 1.92 -10 3 3 24.56 3.76 -9 3 3 71.54 5.41 -8 3 3 22.71 2.69 -7 3 3 0.38 0.91 -6 3 3 0.72 0.78 -5 3 3 1.10 0.72 -4 3 3 83.45 2.25 -3 3 3 280.51 4.36 -2 3 3 62.17 1.76 -1 3 3 232.89 3.70 0 3 3 158.09 3.34 1 3 3 6.76 0.62 2 3 3 149.31 2.77 3 3 3 5.53 0.81 4 3 3 95.97 2.53 5 3 3 108.50 3.01 6 3 3 11.01 1.68 7 3 3 54.33 3.47 8 3 3 11.24 2.10 9 3 3 0.35 1.70 -10 4 3 22.77 3.84 -9 4 3 16.03 3.17 -8 4 3 15.18 2.74 -7 4 3 48.62 2.46 -6 4 3 27.14 1.79 -5 4 3 129.62 3.07 -4 4 3 70.05 2.31 -3 4 3 151.03 2.97 -2 4 3 297.70 4.18 -1 4 3 147.29 2.64 0 4 3 64.82 2.50 1 4 3 88.98 1.88 2 4 3 7.00 0.82 3 4 3 7.03 0.90 4 4 3 53.67 2.13 5 4 3 81.63 3.65 6 4 3 82.92 3.97 7 4 3 10.15 1.90 8 4 3 7.87 2.04 9 4 3 6.71 2.21 -10 5 3 12.79 3.26 -9 5 3 33.45 4.06 -8 5 3 9.44 2.47 -7 5 3 2.96 1.32 -6 5 3 2.70 0.97 -5 5 3 45.17 2.07 -4 5 3 141.91 3.08 -3 5 3 34.09 1.62 -2 5 3 150.49 2.58 -1 5 3 230.43 4.18 0 5 3 137.99 2.91 1 5 3 0.12 0.51 2 5 3 0.85 0.59 3 5 3 2.32 0.77 4 5 3 79.49 2.59 5 5 3 74.30 3.57 6 5 3 118.46 4.71 7 5 3 84.94 4.42 8 5 3 18.40 2.57 9 5 3 0.58 1.75 -10 6 3 22.62 3.87 -9 6 3 16.29 3.14 -8 6 3 10.20 2.56 -7 6 3 1.69 1.38 -6 6 3 5.07 1.42 -5 6 3 8.18 1.11 -4 6 3 12.18 1.19 -3 6 3 139.27 3.02 -2 6 3 261.91 3.88 -1 6 3 23.76 1.47 0 6 3 3.50 0.70 1 6 3 3.34 0.68 2 6 3 0.50 0.66 3 6 3 16.27 1.33 4 6 3 100.48 3.05 5 6 3 167.30 4.98 6 6 3 166.58 5.35 7 6 3 28.53 2.82 8 6 3 1.41 2.32 9 6 3 0.61 2.31 -9 7 3 21.86 3.52 -8 7 3 1.48 1.59 -7 7 3 0.91 1.38 -6 7 3 2.00 1.33 -5 7 3 22.57 2.17 -4 7 3 49.68 2.17 -3 7 3 69.39 2.41 -2 7 3 122.07 4.14 -1 7 3 81.68 2.67 0 7 3 29.85 1.50 1 7 3 14.18 1.13 2 7 3 2.98 0.85 3 7 3 20.04 1.52 4 7 3 82.88 2.95 5 7 3 86.89 4.06 6 7 3 31.84 3.83 7 7 3 13.75 3.16 8 7 3 1.86 2.39 -9 8 3 16.83 3.40 -8 8 3 3.98 1.81 -7 8 3 18.15 2.43 -6 8 3 4.65 1.62 -5 8 3 7.21 1.63 -4 8 3 93.64 4.02 -3 8 3 85.58 2.72 -2 8 3 65.25 2.57 -1 8 3 68.62 2.42 0 8 3 0.21 0.71 1 8 3 0.37 0.71 2 8 3 1.86 0.95 3 8 3 47.59 2.95 4 8 3 55.10 3.26 5 8 3 29.18 3.52 6 8 3 21.10 3.40 7 8 3 45.51 4.80 8 8 3 0.00 2.31 -9 9 3 2.36 2.30 -8 9 3 4.56 2.01 -7 9 3 2.15 1.65 -6 9 3 27.77 2.72 -5 9 3 10.08 1.77 -4 9 3 39.58 2.81 -3 9 3 127.05 3.88 -2 9 3 70.32 2.64 -1 9 3 14.02 1.36 0 9 3 2.32 1.01 1 9 3 7.02 1.52 2 9 3 33.52 2.61 3 9 3 8.26 1.68 4 9 3 37.84 3.84 5 9 3 55.09 4.91 6 9 3 9.24 2.90 7 9 3 2.85 2.59 -8 10 3 1.69 1.93 -7 10 3 2.53 1.80 -6 10 3 4.92 1.82 -5 10 3 58.99 3.62 -4 10 3 140.49 5.00 -3 10 3 87.06 4.49 -2 10 3 15.92 1.68 -1 10 3 1.40 1.23 0 10 3 4.59 1.46 1 10 3 6.73 1.57 2 10 3 8.38 1.78 3 10 3 49.79 3.32 4 10 3 37.59 4.01 5 10 3 4.06 2.36 6 10 3 19.73 3.66 7 10 3 24.63 4.29 -8 11 3 0.00 2.01 -7 11 3 18.45 2.76 -6 11 3 58.36 4.31 -5 11 3 43.13 3.64 -4 11 3 62.98 5.04 -3 11 3 63.58 5.00 -2 11 3 2.26 1.84 -1 11 3 11.19 1.93 0 11 3 0.45 1.35 1 11 3 19.87 2.37 2 11 3 39.21 3.08 3 11 3 43.04 3.26 4 11 3 40.34 4.27 5 11 3 27.48 3.93 6 11 3 3.21 2.62 -7 12 3 1.68 3.49 -6 12 3 11.89 3.09 -5 12 3 58.08 5.22 -4 12 3 30.89 3.89 -3 12 3 12.52 2.86 -2 12 3 10.60 2.59 -1 12 3 3.11 2.04 0 12 3 2.33 1.56 1 12 3 12.41 2.12 2 12 3 22.20 2.67 3 12 3 38.26 3.27 4 12 3 25.42 3.72 5 12 3 15.13 3.41 -6 13 3 2.22 3.12 -5 13 3 16.01 3.59 -4 13 3 63.51 5.51 -3 13 3 18.87 3.42 -2 13 3 19.51 3.36 -1 13 3 2.87 2.19 0 13 3 0.58 1.86 1 13 3 6.87 1.98 2 13 3 26.38 2.90 3 13 3 32.78 4.11 4 13 3 35.54 4.42 -5 14 3 26.50 4.25 -4 14 3 36.40 4.58 -3 14 3 16.29 3.38 -2 14 3 21.60 3.68 -1 14 3 16.36 3.38 0 14 3 4.08 2.53 1 14 3 24.87 3.34 2 14 3 22.87 3.01 3 14 3 5.51 2.79 -3 15 3 17.92 3.77 -2 15 3 8.03 3.16 -1 15 3 0.25 2.38 0 15 3 3.28 2.65 1 15 3 9.24 3.13 -1 -16 4 10.93 7.67 0 -16 4 30.67 5.84 1 -16 4 7.93 4.99 2 -16 4 2.71 4.16 -3 -15 4 0.00 14.94 -2 -15 4 15.00 4.59 -1 -15 4 15.49 3.83 0 -15 4 17.56 3.96 1 -15 4 6.83 4.62 2 -15 4 9.32 3.65 3 -15 4 8.47 3.55 4 -15 4 19.47 4.70 -5 -14 4 0.00 5.04 -4 -14 4 8.87 5.44 -3 -14 4 33.28 4.26 -2 -14 4 25.27 3.88 -1 -14 4 4.35 3.02 0 -14 4 45.65 4.36 1 -14 4 20.26 3.90 2 -14 4 11.37 4.05 3 -14 4 2.43 3.95 4 -14 4 18.28 3.65 5 -14 4 17.30 4.06 -6 -13 4 9.33 6.98 -5 -13 4 9.67 3.92 -4 -13 4 6.00 3.82 -3 -13 4 9.15 2.58 -2 -13 4 42.51 2.97 -1 -13 4 46.03 3.87 0 -13 4 35.66 4.65 1 -13 4 24.74 4.09 2 -13 4 13.25 3.51 3 -13 4 14.28 3.32 4 -13 4 12.70 3.82 5 -13 4 25.11 3.94 6 -13 4 44.81 5.34 -7 -12 4 3.26 3.52 -6 -12 4 1.09 4.81 -5 -12 4 10.08 4.19 -4 -12 4 48.92 4.40 -3 -12 4 39.92 3.11 -2 -12 4 91.95 3.64 -1 -12 4 75.93 3.63 0 -12 4 47.94 4.25 1 -12 4 34.98 3.93 2 -12 4 1.91 3.99 3 -12 4 34.48 4.00 4 -12 4 12.88 3.28 5 -12 4 31.08 3.91 6 -12 4 48.95 5.61 7 -12 4 36.28 5.02 -7 -11 4 5.38 2.25 -6 -11 4 1.77 1.64 -5 -11 4 26.73 2.74 -4 -11 4 67.58 3.77 -3 -11 4 94.71 3.66 -2 -11 4 92.32 3.66 -1 -11 4 37.87 2.75 0 -11 4 12.65 1.61 1 -11 4 2.31 1.54 2 -11 4 6.64 2.00 3 -11 4 17.02 2.88 4 -11 4 60.10 4.03 5 -11 4 123.34 5.71 6 -11 4 27.96 3.51 7 -11 4 9.37 3.35 8 -11 4 7.67 2.82 -8 -10 4 8.35 2.47 -7 -10 4 2.28 1.83 -6 -10 4 5.05 1.84 -5 -10 4 28.62 2.68 -4 -10 4 69.87 3.09 -3 -10 4 43.55 2.42 -2 -10 4 37.33 2.22 -1 -10 4 36.61 2.14 0 -10 4 1.46 0.93 1 -10 4 9.84 1.25 2 -10 4 18.15 2.07 3 -10 4 43.11 3.00 4 -10 4 30.51 2.72 5 -10 4 36.40 3.09 6 -10 4 74.61 4.91 7 -10 4 22.67 2.89 8 -10 4 0.70 1.87 -8 -9 4 1.87 1.83 -7 -9 4 0.78 1.48 -6 -9 4 6.39 1.83 -5 -9 4 39.81 2.99 -4 -9 4 82.32 3.20 -3 -9 4 39.36 2.20 -2 -9 4 25.87 1.78 -1 -9 4 70.64 2.74 0 -9 4 4.05 0.98 1 -9 4 2.38 0.83 2 -9 4 6.34 1.37 3 -9 4 7.59 1.58 4 -9 4 77.24 3.93 5 -9 4 62.71 3.73 6 -9 4 13.89 2.21 7 -9 4 20.48 2.62 8 -9 4 12.34 2.42 -9 -8 4 4.02 2.16 -8 -8 4 5.10 1.93 -7 -8 4 2.33 1.59 -6 -8 4 33.19 2.85 -5 -8 4 97.18 4.34 -4 -8 4 9.82 1.32 -3 -8 4 135.99 3.41 -2 -8 4 51.62 2.28 -1 -8 4 2.60 0.85 0 -8 4 39.71 1.94 1 -8 4 0.87 0.70 2 -8 4 48.26 1.72 3 -8 4 17.17 1.86 4 -8 4 15.41 1.92 5 -8 4 80.00 4.05 6 -8 4 40.38 3.12 7 -8 4 1.47 1.57 8 -8 4 3.97 2.33 9 -8 4 3.80 2.66 -9 -7 4 12.72 2.47 -8 -7 4 0.66 1.55 -7 -7 4 0.45 1.43 -6 -7 4 8.68 1.79 -5 -7 4 106.92 4.19 -4 -7 4 191.20 3.97 -3 -7 4 79.25 2.60 -2 -7 4 12.11 1.18 -1 -7 4 19.49 1.38 0 -7 4 22.41 1.40 1 -7 4 11.45 1.03 2 -7 4 40.12 1.51 3 -7 4 35.43 2.38 4 -7 4 74.86 3.58 5 -7 4 57.46 3.34 6 -7 4 41.75 3.27 7 -7 4 13.51 2.21 8 -7 4 3.41 2.27 9 -7 4 3.49 2.48 -9 -6 4 2.24 1.69 -8 -6 4 9.19 1.98 -7 -6 4 2.94 1.44 -6 -6 4 104.68 4.29 -5 -6 4 56.34 3.09 -4 -6 4 61.13 2.28 -3 -6 4 150.28 3.22 -2 -6 4 64.94 2.22 -1 -6 4 1.79 0.71 0 -6 4 0.52 0.60 1 -6 4 76.83 2.12 2 -6 4 61.10 1.81 3 -6 4 38.97 1.63 4 -6 4 72.30 3.35 5 -6 4 74.82 3.64 6 -6 4 29.78 2.82 7 -6 4 16.67 2.20 8 -6 4 0.16 1.89 9 -6 4 1.63 2.14 -10 -5 4 6.86 3.48 -9 -5 4 5.66 2.12 -8 -5 4 0.08 1.42 -7 -5 4 13.95 2.26 -6 -5 4 27.65 3.01 -5 -5 4 56.74 2.95 -4 -5 4 148.92 3.12 -3 -5 4 152.62 3.06 -2 -5 4 108.35 2.42 -1 -5 4 14.63 1.07 0 -5 4 0.96 0.58 1 -5 4 29.79 1.35 2 -5 4 179.55 3.17 3 -5 4 43.72 1.53 4 -5 4 108.89 2.64 5 -5 4 199.44 4.61 6 -5 4 107.77 4.30 7 -5 4 11.64 1.94 8 -5 4 5.68 2.29 9 -5 4 1.24 2.29 -10 -4 4 12.60 3.67 -9 -4 4 8.03 2.87 -8 -4 4 10.01 1.96 -7 -4 4 7.38 1.66 -6 -4 4 74.75 3.65 -5 -4 4 49.94 1.80 -4 -4 4 174.79 3.33 -3 -4 4 374.02 5.46 -2 -4 4 198.52 3.34 -1 -4 4 15.42 0.98 0 -4 4 25.64 1.18 1 -4 4 72.12 1.78 2 -4 4 82.15 1.98 3 -4 4 520.73 7.17 4 -4 4 291.35 4.81 5 -4 4 34.85 1.84 6 -4 4 17.57 1.69 7 -4 4 12.33 2.16 8 -4 4 1.82 1.85 9 -4 4 20.52 3.40 10 -4 4 3.83 2.71 -10 -3 4 24.74 4.40 -9 -3 4 12.17 3.53 -8 -3 4 2.82 2.64 -7 -3 4 45.85 3.78 -6 -3 4 50.02 2.94 -5 -3 4 34.45 1.47 -4 -3 4 158.76 3.06 -3 -3 4 266.31 4.15 -2 -3 4 28.20 1.21 -1 -3 4 131.43 2.31 0 -3 4 4.31 0.63 1 -3 4 212.51 3.54 2 -3 4 85.69 1.71 3 -3 4 56.46 1.91 4 -3 4 30.03 1.60 5 -3 4 97.09 2.79 6 -3 4 33.09 1.95 7 -3 4 1.34 1.25 8 -3 4 0.00 1.71 9 -3 4 3.30 2.34 10 -3 4 15.58 3.41 -10 -2 4 25.14 4.39 -9 -2 4 0.04 2.54 -8 -2 4 4.44 2.68 -7 -2 4 2.16 2.30 -6 -2 4 39.27 2.87 -5 -2 4 59.14 1.94 -4 -2 4 79.31 2.14 -3 -2 4 321.51 4.70 -2 -2 4 538.58 6.83 -1 -2 4 10.62 1.01 0 -2 4 168.54 2.61 1 -2 4 132.29 2.10 2 -2 4 58.99 1.81 3 -2 4 387.52 6.03 4 -2 4 29.19 1.57 5 -2 4 2.41 0.85 6 -2 4 37.14 2.05 7 -2 4 14.67 1.93 8 -2 4 0.04 1.77 9 -2 4 9.36 2.70 10 -2 4 2.36 2.46 -10 -1 4 1.79 3.10 -9 -1 4 1.30 2.81 -8 -1 4 8.42 2.72 -7 -1 4 39.77 3.80 -6 -1 4 36.79 2.64 -5 -1 4 59.90 2.00 -4 -1 4 119.08 2.56 -3 -1 4 136.39 2.58 -2 -1 4 11.19 0.81 -1 -1 4 0.77 0.34 0 -1 4 1.24 0.45 1 -1 4 204.02 3.17 2 -1 4 74.91 1.85 3 -1 4 110.74 2.46 4 -1 4 78.52 2.28 5 -1 4 40.01 1.97 6 -1 4 9.82 1.23 7 -1 4 0.65 1.25 8 -1 4 3.59 1.60 9 -1 4 3.20 1.99 10 -1 4 33.39 4.27 -10 0 4 3.95 3.41 -9 0 4 2.79 2.94 -8 0 4 7.12 2.80 -7 0 4 2.01 1.76 -6 0 4 55.06 2.29 -5 0 4 162.91 3.53 -4 0 4 5.91 0.83 -3 0 4 0.69 0.57 -2 0 4 45.95 1.46 -1 0 4 22.24 0.98 0 0 4 0.30 0.44 1 0 4 6.21 0.70 2 0 4 163.47 2.91 3 0 4 322.93 5.22 4 0 4 67.31 2.29 5 0 4 2.06 0.79 6 0 4 37.85 2.64 7 0 4 4.01 1.43 8 0 4 4.10 1.69 9 0 4 2.43 1.74 10 0 4 17.45 3.45 -10 1 4 5.65 3.11 -9 1 4 1.84 2.18 -8 1 4 36.47 3.64 -7 1 4 41.49 3.38 -6 1 4 62.60 2.43 -5 1 4 110.01 2.72 -4 1 4 86.00 2.29 -3 1 4 6.44 0.82 -2 1 4 46.32 1.54 -1 1 4 1.42 0.56 0 1 4 3.73 0.61 1 1 4 30.85 1.24 2 1 4 155.64 3.08 3 1 4 180.66 3.30 4 1 4 67.81 2.24 5 1 4 10.21 1.14 6 1 4 8.50 1.56 7 1 4 1.46 1.36 8 1 4 0.58 1.40 9 1 4 29.29 3.06 10 1 4 15.97 3.36 -10 2 4 2.38 2.33 -9 2 4 7.88 2.20 -8 2 4 12.61 1.96 -7 2 4 36.11 2.62 -6 2 4 36.44 1.95 -5 2 4 149.26 3.23 -4 2 4 58.70 2.14 -3 2 4 1.26 0.64 -2 2 4 32.08 1.38 -1 2 4 35.46 1.17 0 2 4 1.20 0.44 1 2 4 231.23 3.51 2 2 4 112.95 2.35 3 2 4 46.58 1.91 4 2 4 146.09 3.12 5 2 4 63.72 2.36 6 2 4 0.21 1.06 7 2 4 5.43 1.58 8 2 4 6.68 1.83 9 2 4 7.92 2.15 -10 3 4 3.23 2.51 -9 3 4 1.58 2.07 -8 3 4 4.41 1.60 -7 3 4 94.89 3.28 -6 3 4 92.99 2.98 -5 3 4 91.93 2.74 -4 3 4 72.33 2.32 -3 3 4 126.13 2.67 -2 3 4 21.55 1.21 -1 3 4 4.66 0.68 0 3 4 1.13 0.72 1 3 4 215.58 3.35 2 3 4 606.54 7.94 3 3 4 114.02 2.62 4 3 4 23.82 1.50 5 3 4 48.19 2.25 6 3 4 7.42 1.87 7 3 4 0.88 1.38 8 3 4 63.39 4.46 9 3 4 29.97 3.89 -10 4 4 0.94 2.27 -9 4 4 1.58 2.09 -8 4 4 21.67 3.13 -7 4 4 191.54 4.33 -6 4 4 130.13 3.37 -5 4 4 207.01 4.08 -4 4 4 83.57 2.59 -3 4 4 1.99 0.70 -2 4 4 73.56 1.85 -1 4 4 0.85 0.52 0 4 4 247.47 4.92 1 4 4 455.61 7.71 2 4 4 104.07 2.38 3 4 4 81.49 2.38 4 4 4 139.33 3.20 5 4 4 20.98 1.98 6 4 4 13.29 1.89 7 4 4 4.08 1.55 8 4 4 4.90 1.86 9 4 4 26.09 3.12 -10 5 4 0.00 2.33 -9 5 4 1.54 2.11 -8 5 4 13.51 2.73 -7 5 4 184.04 5.32 -6 5 4 220.51 4.53 -5 5 4 38.34 2.01 -4 5 4 51.59 2.16 -3 5 4 36.38 1.74 -2 5 4 11.61 0.91 -1 5 4 91.55 2.13 0 5 4 5.45 1.06 1 5 4 17.12 1.58 2 5 4 595.81 8.10 3 5 4 49.66 1.99 4 5 4 8.83 1.14 5 5 4 76.17 3.66 6 5 4 11.29 1.85 7 5 4 9.81 2.02 8 5 4 21.20 3.52 9 5 4 2.97 2.77 -10 6 4 5.83 2.77 -9 6 4 2.31 2.26 -8 6 4 46.97 4.38 -7 6 4 20.98 2.34 -6 6 4 172.85 5.03 -5 6 4 42.95 2.17 -4 6 4 9.40 1.15 -3 6 4 10.74 1.14 -2 6 4 0.55 0.59 -1 6 4 34.34 1.46 0 6 4 160.78 4.15 1 6 4 11.42 1.49 2 6 4 85.47 2.35 3 6 4 141.62 3.30 4 6 4 136.99 3.49 5 6 4 0.76 1.16 6 6 4 13.38 2.71 7 6 4 3.14 2.24 8 6 4 23.08 3.81 -9 7 4 2.73 2.41 -8 7 4 13.74 2.29 -7 7 4 35.18 2.94 -6 7 4 90.38 4.27 -5 7 4 18.80 2.02 -4 7 4 18.38 1.49 -3 7 4 3.46 0.93 -2 7 4 11.47 1.19 -1 7 4 38.43 1.70 0 7 4 46.68 1.92 1 7 4 21.75 1.43 2 7 4 77.75 3.55 3 7 4 54.86 3.09 4 7 4 2.25 1.22 5 7 4 6.35 2.31 6 7 4 1.53 1.90 7 7 4 20.35 3.66 8 7 4 16.65 3.57 -9 8 4 36.61 4.47 -8 8 4 30.24 3.04 -7 8 4 26.57 2.78 -6 8 4 54.77 3.48 -5 8 4 26.15 2.40 -4 8 4 14.38 1.68 -3 8 4 19.35 1.54 -2 8 4 4.84 1.15 -1 8 4 60.47 3.16 0 8 4 45.36 2.79 1 8 4 34.40 2.51 2 8 4 62.74 3.38 3 8 4 138.96 4.73 4 8 4 3.80 1.54 5 8 4 0.37 1.64 6 8 4 2.55 2.27 7 8 4 6.42 2.70 8 8 4 17.98 3.85 -9 9 4 8.21 3.01 -8 9 4 10.05 2.30 -7 9 4 20.40 2.61 -6 9 4 53.16 3.58 -5 9 4 51.93 3.33 -4 9 4 1.17 1.23 -3 9 4 0.85 1.10 -2 9 4 4.97 1.57 -1 9 4 48.68 2.98 0 9 4 65.26 3.52 1 9 4 115.16 4.55 2 9 4 14.23 1.91 3 9 4 66.13 3.70 4 9 4 17.27 2.93 5 9 4 3.28 2.29 6 9 4 2.90 2.32 7 9 4 6.30 2.88 -8 10 4 16.58 2.77 -7 10 4 25.17 2.93 -6 10 4 27.87 2.89 -5 10 4 28.23 3.07 -4 10 4 18.09 2.98 -3 10 4 1.39 1.78 -2 10 4 48.36 3.43 -1 10 4 1.79 1.32 0 10 4 23.65 2.36 1 10 4 92.61 4.44 2 10 4 63.86 3.74 3 10 4 16.64 2.27 4 10 4 5.14 2.17 5 10 4 1.60 2.09 6 10 4 6.01 2.88 -7 11 4 23.50 3.93 -6 11 4 83.43 6.08 -5 11 4 28.68 3.81 -4 11 4 1.00 1.90 -3 11 4 2.59 1.85 -2 11 4 10.49 2.53 -1 11 4 28.40 2.67 0 11 4 85.98 4.38 1 11 4 34.51 2.94 2 11 4 39.37 3.16 3 11 4 37.27 3.22 4 11 4 1.14 2.15 5 11 4 17.17 3.58 6 11 4 1.79 2.60 -7 12 4 48.01 5.23 -6 12 4 1.83 2.46 -5 12 4 22.30 3.70 -4 12 4 4.31 2.42 -3 12 4 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5 42.92 3.34 9 1 5 19.53 2.76 -10 2 5 27.69 3.90 -9 2 5 59.73 4.49 -8 2 5 101.25 4.61 -7 2 5 8.75 1.35 -6 2 5 68.67 2.71 -5 2 5 24.84 1.59 -4 2 5 22.03 1.42 -3 2 5 302.22 4.74 -2 2 5 121.76 2.50 -1 2 5 38.54 1.31 0 2 5 298.48 4.32 1 2 5 47.99 1.51 2 2 5 16.59 1.10 3 2 5 0.68 0.64 4 2 5 32.98 1.83 5 2 5 12.67 1.42 6 2 5 65.00 3.50 7 2 5 25.33 2.53 8 2 5 37.04 3.20 9 2 5 11.34 2.45 -10 3 5 18.73 3.53 -9 3 5 15.00 2.97 -8 3 5 52.19 3.35 -7 3 5 33.06 2.13 -6 3 5 23.68 1.72 -5 3 5 0.61 0.78 -4 3 5 7.32 0.99 -3 3 5 84.02 2.29 -2 3 5 131.48 2.90 -1 3 5 145.49 2.45 0 3 5 163.73 3.75 1 3 5 70.99 2.17 2 3 5 18.65 1.17 3 3 5 17.65 1.29 4 3 5 1.31 0.78 5 3 5 7.66 1.16 6 3 5 32.45 2.58 7 3 5 73.86 4.31 8 3 5 73.01 4.63 9 3 5 38.62 3.56 -10 4 5 25.90 3.87 -9 4 5 18.45 3.16 -8 4 5 19.38 2.98 -7 4 5 69.43 3.00 -6 4 5 1.75 0.99 -5 4 5 2.54 0.91 -4 4 5 11.31 1.17 -3 4 5 39.08 1.80 -2 4 5 151.74 2.69 -1 4 5 393.14 5.91 0 4 5 89.90 3.09 1 4 5 14.72 1.49 2 4 5 39.35 1.56 3 4 5 0.34 0.66 4 4 5 2.21 0.88 5 4 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15 8.91 2.22 4 -6 15 7.89 2.68 -7 -5 15 10.89 3.14 -6 -5 15 20.21 3.57 -5 -5 15 11.79 2.27 -4 -5 15 6.46 1.94 -3 -5 15 1.55 1.55 -2 -5 15 6.08 1.81 -1 -5 15 22.91 2.56 0 -5 15 23.83 2.66 1 -5 15 46.40 3.42 2 -5 15 31.01 3.08 3 -5 15 16.08 2.97 4 -5 15 1.16 3.52 -7 -4 15 35.49 4.52 -6 -4 15 33.42 3.56 -5 -4 15 15.13 2.66 -4 -4 15 1.03 1.64 -3 -4 15 1.90 1.65 -2 -4 15 24.22 2.73 -1 -4 15 21.92 2.59 0 -4 15 39.51 3.30 1 -4 15 81.16 4.47 2 -4 15 24.34 3.29 3 -4 15 20.45 3.47 4 -4 15 0.00 5.23 5 -4 15 2.56 3.96 -7 -3 15 42.89 4.80 -6 -3 15 11.50 2.44 -5 -3 15 2.43 2.04 -4 -3 15 2.32 1.80 -3 -3 15 20.47 2.70 -2 -3 15 22.55 2.79 -1 -3 15 10.09 2.51 0 -3 15 48.30 4.34 1 -3 15 84.11 5.20 2 -3 15 16.57 3.56 3 -3 15 2.23 3.51 4 -3 15 1.07 3.82 5 -3 15 6.06 5.94 -7 -2 15 50.87 5.02 -6 -2 15 29.52 3.20 -5 -2 15 0.76 1.59 -4 -2 15 3.44 1.90 -3 -2 15 16.83 2.80 -2 -2 15 33.12 3.58 -1 -2 15 29.26 3.62 0 -2 15 49.72 4.65 1 -2 15 25.65 4.01 2 -2 15 29.42 4.35 3 -2 15 4.10 3.56 4 -2 15 0.08 3.63 5 -2 15 8.21 2.66 -7 -1 15 36.03 4.31 -6 -1 15 11.25 2.31 -5 -1 15 10.30 2.18 -4 -1 15 5.54 1.88 -3 -1 15 33.01 3.35 -2 -1 15 42.49 4.26 -1 -1 15 11.91 3.14 0 -1 15 46.45 4.83 1 -1 15 42.97 4.91 2 -1 15 11.92 4.48 3 -1 15 0.05 3.82 4 -1 15 0.00 4.02 -7 0 15 48.53 4.89 -6 0 15 14.41 2.70 -5 0 15 2.32 1.95 -4 0 15 1.05 1.86 -3 0 15 3.63 1.98 -2 0 15 29.74 3.97 -1 0 15 59.75 5.53 0 0 15 29.21 3.82 1 0 15 19.45 3.74 2 0 15 18.47 2.97 3 0 15 9.22 2.80 4 0 15 3.72 3.83 -7 1 15 18.88 4.01 -6 1 15 10.35 2.87 -5 1 15 2.66 2.15 -4 1 15 1.00 1.95 -3 1 15 24.29 3.43 -2 1 15 8.63 2.53 -1 1 15 72.96 5.90 0 1 15 80.29 5.71 1 1 15 29.10 3.70 2 1 15 21.31 2.78 3 1 15 5.66 2.18 4 1 15 1.57 2.06 -6 2 15 7.05 2.71 -5 2 15 1.66 2.17 -4 2 15 2.34 2.08 -3 2 15 19.19 3.21 -2 2 15 39.24 4.03 -1 2 15 51.45 4.57 0 2 15 11.43 2.75 1 2 15 3.07 1.87 2 2 15 11.26 2.38 3 2 15 1.18 1.71 4 2 15 1.13 1.74 -6 3 15 5.46 2.54 -5 3 15 4.16 2.47 -4 3 15 2.47 2.17 -3 3 15 10.73 2.71 -2 3 15 19.64 3.22 -1 3 15 8.19 2.41 0 3 15 16.02 3.06 1 3 15 12.91 2.45 2 3 15 3.62 1.90 3 3 15 1.89 1.88 -6 4 15 1.19 2.30 -5 4 15 2.73 2.35 -4 4 15 14.59 3.03 -3 4 15 14.81 3.02 -2 4 15 40.67 4.26 -1 4 15 21.23 3.46 0 4 15 18.45 2.90 1 4 15 2.25 1.80 2 4 15 4.21 2.11 3 4 15 1.82 2.03 -5 5 15 0.68 2.16 -4 5 15 1.80 2.16 -3 5 15 21.39 3.45 -2 5 15 42.85 4.56 -1 5 15 15.49 3.16 0 5 15 9.15 2.49 1 5 15 12.02 2.48 2 5 15 0.50 1.92 -4 6 15 11.54 3.10 -3 6 15 31.29 4.10 -2 6 15 26.79 3.90 -1 6 15 35.16 4.28 0 6 15 6.34 2.28 1 6 15 3.73 2.21 -2 7 15 30.89 4.79 -1 7 15 10.55 3.56 -2 -10 16 24.20 3.04 -1 -10 16 49.95 4.98 0 -10 16 36.26 4.49 -4 -9 16 19.03 2.79 -3 -9 16 19.67 2.73 -2 -9 16 60.91 4.21 -1 -9 16 45.07 3.69 0 -9 16 24.86 3.19 1 -9 16 3.11 2.55 2 -9 16 0.72 2.33 -4 -8 16 22.01 3.22 -3 -8 16 18.40 2.96 -2 -8 16 35.15 3.73 -1 -8 16 61.74 4.14 0 -8 16 9.32 2.19 1 -8 16 2.47 1.90 2 -8 16 2.49 2.43 -5 -7 16 2.24 1.98 -4 -7 16 11.53 2.67 -3 -7 16 30.79 3.45 -2 -7 16 18.65 2.81 -1 -7 16 30.30 3.23 0 -7 16 14.47 2.47 1 -7 16 8.51 2.48 2 -7 16 2.20 2.31 3 -7 16 5.78 2.70 -5 -6 16 12.17 2.74 -4 -6 16 18.66 2.96 -3 -6 16 11.67 2.40 -2 -6 16 26.16 3.06 -1 -6 16 54.60 3.90 0 -6 16 2.06 1.93 1 -6 16 2.80 1.84 2 -6 16 6.36 2.47 3 -6 16 6.17 2.69 -6 -5 16 0.91 3.39 -5 -5 16 3.70 3.40 -4 -5 16 8.39 3.60 -3 -5 16 24.86 3.44 -2 -5 16 46.46 3.90 -1 -5 16 11.20 2.90 0 -5 16 9.24 2.88 1 -5 16 0.00 2.19 2 -5 16 1.65 3.40 3 -5 16 4.08 3.42 -6 -4 16 3.77 4.51 -5 -4 16 31.96 4.23 -4 -4 16 50.93 4.27 -3 -4 16 28.96 4.42 -2 -4 16 22.92 4.04 -1 -4 16 9.37 3.52 0 -4 16 14.36 3.29 1 -4 16 1.70 2.94 2 -4 16 6.46 3.98 3 -4 16 13.63 5.60 4 -4 16 18.55 9.53 -6 -3 16 9.29 3.95 -5 -3 16 24.36 4.22 -4 -3 16 6.87 4.05 -3 -3 16 53.12 4.78 -2 -3 16 26.87 3.91 -1 -3 16 26.02 4.05 0 -3 16 0.00 3.64 1 -3 16 1.15 2.99 2 -3 16 0.00 4.07 3 -3 16 13.80 5.15 4 -3 16 27.14 7.41 -6 -2 16 9.13 3.48 -5 -2 16 14.49 4.08 -4 -2 16 30.88 4.77 -3 -2 16 34.45 5.39 -2 -2 16 12.07 4.59 -1 -2 16 2.56 4.01 0 -2 16 18.47 4.24 1 -2 16 0.00 3.47 2 -2 16 28.33 4.78 3 -2 16 9.68 5.17 4 -2 16 18.20 4.01 -6 -1 16 9.14 3.26 -5 -1 16 20.82 4.08 -4 -1 16 30.93 5.13 -3 -1 16 43.36 5.29 -2 -1 16 45.60 5.13 -1 -1 16 3.61 3.15 0 -1 16 1.24 4.17 1 -1 16 6.04 4.16 2 -1 16 13.43 4.85 3 -1 16 38.55 5.50 -6 0 16 2.14 2.57 -5 0 16 14.69 3.24 -4 0 16 58.08 5.97 -3 0 16 18.77 3.38 -2 0 16 17.80 3.28 -1 0 16 11.07 2.93 0 0 16 8.77 3.04 1 0 16 15.57 4.05 2 0 16 13.16 4.01 3 0 16 7.34 5.50 -6 1 16 7.50 2.80 -5 1 16 20.96 3.50 -4 1 16 18.81 3.19 -3 1 16 50.16 4.69 -2 1 16 73.58 5.55 -1 1 16 11.67 2.78 0 1 16 0.59 1.86 1 1 16 0.10 1.92 2 1 16 6.55 2.38 3 1 16 31.93 3.97 -5 2 16 28.62 3.86 -4 2 16 33.91 3.99 -3 2 16 18.26 3.33 -2 2 16 7.88 2.57 -1 2 16 21.04 3.42 0 2 16 2.42 2.26 1 2 16 7.23 2.63 2 2 16 6.26 2.21 -5 3 16 21.44 3.64 -4 3 16 34.58 4.18 -3 3 16 7.49 2.66 -2 3 16 9.74 2.83 -1 3 16 23.88 3.65 0 3 16 0.38 2.08 1 3 16 5.49 2.27 2 3 16 25.68 3.26 -4 4 16 30.09 3.93 -3 4 16 31.20 4.05 -2 4 16 4.08 2.43 -1 4 16 3.11 2.36 0 4 16 0.51 2.23 1 4 16 3.72 2.19 -3 5 16 6.53 2.71 -2 5 16 4.33 2.53 -1 5 16 13.57 3.25 0 5 16 0.68 2.33 -1 -9 17 0.00 2.86 -3 -8 17 5.86 2.52 -2 -8 17 6.43 2.46 -1 -8 17 0.20 1.78 0 -8 17 0.71 1.75 1 -8 17 10.40 3.15 -4 -7 17 32.85 3.72 -3 -7 17 5.03 2.16 -2 -7 17 3.18 2.10 -1 -7 17 0.32 1.79 0 -7 17 14.74 2.57 1 -7 17 11.31 3.05 -4 -6 17 36.18 3.81 -3 -6 17 21.08 3.19 -2 -6 17 4.19 2.45 -1 -6 17 1.09 2.53 0 -6 17 3.15 2.82 1 -6 17 7.31 3.47 2 -6 17 36.17 4.67 -5 -5 17 47.95 4.16 -4 -5 17 10.73 3.95 -3 -5 17 2.40 3.42 -2 -5 17 0.10 3.23 -1 -5 17 9.17 3.79 0 -5 17 24.28 4.37 1 -5 17 9.61 5.92 2 -5 17 26.34 5.79 -5 -4 17 18.88 4.29 -4 -4 17 17.91 3.79 -3 -4 17 10.85 3.44 -2 -4 17 5.83 3.19 -1 -4 17 10.86 4.12 0 -4 17 20.30 4.41 1 -4 17 37.84 5.92 2 -4 17 27.40 5.56 -5 -3 17 19.81 4.24 -4 -3 17 8.59 4.21 -3 -3 17 12.71 4.08 -2 -3 17 0.95 3.43 -1 -3 17 20.51 4.54 0 -3 17 4.67 4.33 1 -3 17 15.47 5.28 2 -3 17 0.00 5.47 -5 -2 17 22.89 4.85 -4 -2 17 13.45 3.99 -3 -2 17 11.46 4.45 -2 -2 17 0.15 3.81 -1 -2 17 2.11 4.38 0 -2 17 14.24 4.68 1 -2 17 27.73 5.66 2 -2 17 55.02 6.36 -5 -1 17 16.82 4.57 -4 -1 17 32.07 4.32 -3 -1 17 7.19 3.61 -2 -1 17 0.39 2.93 -1 -1 17 2.80 3.60 0 -1 17 9.93 4.73 1 -1 17 34.49 5.90 2 -1 17 44.13 6.79 -5 0 17 16.07 3.60 -4 0 17 1.78 2.47 -3 0 17 4.84 2.53 -2 0 17 2.80 2.42 -1 0 17 28.00 4.21 0 0 17 18.79 3.85 1 0 17 28.23 4.60 2 0 17 43.97 5.37 -4 1 17 5.94 2.71 -3 1 17 1.57 2.23 -2 1 17 32.08 4.19 -1 1 17 16.14 3.22 0 1 17 21.38 3.56 1 1 17 36.09 4.34 -4 2 17 0.49 2.10 -3 2 17 0.76 2.13 -2 2 17 8.04 2.79 -1 2 17 41.72 5.10 0 2 17 16.37 3.31 1 2 17 14.35 3.24 -3 3 17 1.51 2.38 -2 3 17 4.79 2.62 -1 3 17 8.11 2.75 0 3 17 36.53 4.62 -2 -6 18 11.86 3.37 -1 -6 18 60.70 5.25 -3 -5 18 28.89 4.56 -2 -5 18 21.17 4.69 -1 -5 18 38.37 6.51 0 -5 18 35.46 4.32 -3 -4 18 5.31 4.75 -2 -4 18 29.63 5.33 -1 -4 18 43.02 6.22 0 -4 18 49.25 6.10 -3 -3 18 23.85 5.26 -2 -3 18 38.08 5.92 -1 -3 18 19.82 5.58 0 -3 18 18.29 5.71 1 -3 18 9.86 2.87 -3 -2 18 18.46 5.23 -2 -2 18 20.71 5.48 -1 -2 18 22.41 5.64 0 -2 18 18.45 5.32 -3 -1 18 12.24 3.56 -2 -1 18 25.29 4.29 -1 -1 18 29.49 5.05 0 -1 18 18.97 4.02 -3 0 18 24.88 3.85 -2 0 18 25.84 3.85 -1 0 18 3.54 2.70 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 70218 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969307' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_8 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 Ho N3 O7' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 882.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ho Ho -0.2175 4.6783 '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 8.703(2) _cell_length_b 13.100(3) _cell_length_c 14.761(4) _cell_angle_alpha 100.253(4) _cell_angle_beta 97.766(4) _cell_angle_gamma 92.399(4) _cell_volume 1637.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24059 _cell_measurement_theta_min 4.735 _cell_measurement_theta_max 43.387 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.791 _exptl_crystal_F_000 872 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 2.718 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6840 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24059 _diffrn_reflns_av_unetI/netI 0.1015 _diffrn_reflns_av_R_equivalents 0.0756 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.417 _diffrn_reflns_theta_max 30.273 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.915 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.915 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.915 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8961 _reflns_number_gt 6840 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0281P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8961 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0729 _refine_ls_R_factor_gt 0.0468 _refine_ls_wR_factor_ref 0.0907 _refine_ls_wR_factor_gt 0.0812 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.994 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ho1 Ho 0.56235(3) 0.51297(2) 0.70165(2) 0.01146(6) Uani 1 1 d . . . . . O1 O 0.7112(4) 0.6230(2) 0.8426(2) 0.0174(7) Uani 1 1 d . . . . . C23 C 0.4598(5) 0.3198(4) 0.5861(3) 0.0123(9) Uani 1 1 d . . . . . O3 O 0.5615(4) 0.3771(2) 0.5613(2) 0.0159(7) Uani 1 1 d . . . . . O4 O 0.4044(4) 0.3497(2) 0.6608(2) 0.0159(7) Uani 1 1 d . . . . . O2 O 0.5361(4) 0.6965(2) 0.7555(2) 0.0170(7) Uani 1 1 d . . . . . C16 C 0.6415(6) 0.7026(4) 0.8247(3) 0.0155(10) Uani 1 1 d . . . . . N1 N 0.7912(4) 0.4055(3) 0.7254(3) 0.0136(8) Uani 1 1 d . . . . . C24 C 0.4057(5) 0.2167(4) 0.5279(3) 0.0138(9) Uani 1 1 d . . . . . N3 N 0.3396(4) 0.5385(3) 0.7961(3) 0.0137(8) Uani 1 1 d . . . . . N2 N 0.5695(4) 0.4144(3) 0.8368(2) 0.0120(8) Uani 1 1 d . . . . . C17 C 0.6830(5) 0.8059(4) 0.8856(3) 0.0157(10) Uani 1 1 d . . . . . C13 C 0.0907(6) 0.5676(4) 0.8955(3) 0.0201(11) Uani 1 1 d . . . . . H13 H 0.0068 0.5766 0.9284 0.024 Uiso 1 1 calc R U . . . C14 C 0.1024(6) 0.6173(4) 0.8216(3) 0.0180(10) Uani 1 1 d . . . . . H14 H 0.0266 0.6606 0.8037 0.022 Uiso 1 1 calc R U . . . C5 C 0.8102(5) 0.3487(4) 0.7943(3) 0.0136(9) Uani 1 1 d . . . . . C12 C 0.2067(5) 0.5040(4) 0.9195(3) 0.0185(10) Uani 1 1 d . . . . . H12 H 0.2038 0.4715 0.9705 0.022 Uiso 1 1 calc R U . . . C10 C 0.4486(5) 0.4156(3) 0.8860(3) 0.0122(9) Uani 1 1 d . . . . . C4 C 0.9424(5) 0.2948(4) 0.8097(3) 0.0151(10) Uani 1 1 d . . . . . H4 H 0.9533 0.2568 0.8574 0.018 Uiso 1 1 calc R U . . . C15 C 0.2290(5) 0.6016(4) 0.7745(3) 0.0153(10) Uani 1 1 d . . . . . H15 H 0.2376 0.6364 0.7256 0.018 Uiso 1 1 calc R U . . . C1 C 0.9026(5) 0.4042(4) 0.6701(3) 0.0170(10) Uani 1 1 d . . . . . H1 H 0.8887 0.4402 0.6210 0.020 Uiso 1 1 calc R U . . . C3 C 1.0572(5) 0.2974(4) 0.7545(3) 0.0186(10) Uani 1 1 d . . . . . H3 H 1.1471 0.2629 0.7653 0.022 Uiso 1 1 calc R U . . . C29 C 0.2917(6) 0.1542(4) 0.5534(3) 0.0194(10) Uani 1 1 d . . . . . H29 H 0.2478 0.1779 0.6067 0.023 Uiso 1 1 calc R U . . . C18 C 0.8060(6) 0.8210(4) 0.9574(3) 0.0203(11) Uani 1 1 d . . . . . H18 H 0.8653 0.7656 0.9675 0.024 Uiso 1 1 calc R U . . . C19 C 0.8425(6) 0.9179(4) 1.0148(3) 0.0219(11) Uani 1 1 d . . . . . H19 H 0.9245 0.9276 1.0636 0.026 Uiso 1 1 calc R U . . . C2 C 1.0364(5) 0.3523(4) 0.6827(3) 0.0189(10) Uani 1 1 d . . . . . H2 H 1.1112 0.3543 0.6435 0.023 Uiso 1 1 calc R U . . . C9 C 0.4366(6) 0.3504(4) 0.9493(3) 0.0199(11) Uani 1 1 d . . . . . H9 H 0.3544 0.3541 0.9837 0.024 Uiso 1 1 calc R U . . . Cl1 Cl 0.79690(15) 1.12023(9) 1.07056(9) 0.0252(3) Uani 1 1 d . . . . . O5 O 0.7287(4) 0.5958(2) 0.6287(2) 0.0167(7) Uani 1 1 d . . . . . OW1 O 0.3705(4) 0.5587(3) 0.5927(2) 0.0158(7) Uani 1 1 d D . . . . C6 C 0.6806(5) 0.3465(3) 0.8492(3) 0.0129(9) Uani 1 1 d . . . . . C20 C 0.7541(6) 0.9990(4) 0.9976(3) 0.0209(11) Uani 1 1 d . . . . . C25 C 0.4708(5) 0.1794(4) 0.4482(3) 0.0171(10) Uani 1 1 d . . . . . H25 H 0.5450 0.2210 0.4294 0.020 Uiso 1 1 calc R U . . . C21 C 0.6325(6) 0.9871(4) 0.9251(3) 0.0216(11) Uani 1 1 d . . . . . H21 H 0.5761 1.0435 0.9141 0.026 Uiso 1 1 calc R U . . . C8 C 0.5478(6) 0.2795(4) 0.9608(4) 0.0239(12) Uani 1 1 d . . . . . H8 H 0.5400 0.2338 1.0017 0.029 Uiso 1 1 calc R U . . . C7 C 0.6714(6) 0.2780(4) 0.9101(3) 0.0208(11) Uani 1 1 d . . . . . H7 H 0.7477 0.2312 0.9170 0.025 Uiso 1 1 calc R U . . . C22 C 0.5961(6) 0.8912(4) 0.8697(3) 0.0189(10) Uani 1 1 d . . . . . H22 H 0.5136 0.8822 0.8213 0.023 Uiso 1 1 calc R U . . . C28 C 0.2427(6) 0.0571(4) 0.5003(4) 0.0232(11) Uani 1 1 d . . . . . H28 H 0.1641 0.0167 0.5165 0.028 Uiso 1 1 calc R U . . . C26 C 0.4264(6) 0.0814(4) 0.3967(3) 0.0217(11) Uani 1 1 d . . . . . H26 H 0.4728 0.0561 0.3448 0.026 Uiso 1 1 calc R U . . . C11 C 0.3276(5) 0.4891(3) 0.8668(3) 0.0139(9) Uani 1 1 d . . . . . C27 C 0.3121(6) 0.0213(4) 0.4232(4) 0.0237(12) Uani 1 1 d . . . . . Cl2 Cl 0.24995(18) -0.10000(11) 0.35614(10) 0.0383(4) Uani 1 1 d . . . . . O6 O 0.8472(4) 0.5803(3) 0.5017(2) 0.0206(8) Uani 1 1 d . . . . . C32 C 0.8722(5) 0.7978(4) 0.6904(3) 0.0169(10) Uani 1 1 d . . . . . H32 H 0.7803 0.7829 0.7126 0.020 Uiso 1 1 calc R U . . . C31 C 0.9206(5) 0.7265(4) 0.6204(3) 0.0153(10) Uani 1 1 d . . . . . C30 C 0.8247(5) 0.6266(4) 0.5799(3) 0.0159(10) Uani 1 1 d . . . . . C36 C 1.0583(5) 0.7496(4) 0.5872(3) 0.0193(10) Uani 1 1 d . . . . . H36 H 1.0912 0.7029 0.5397 0.023 Uiso 1 1 calc R U . . . C35 C 1.1460(6) 0.8417(4) 0.6248(4) 0.0226(11) Uani 1 1 d . . . . . H35 H 1.2378 0.8571 0.6028 0.027 Uiso 1 1 calc R U . . . C33 C 0.9583(6) 0.8907(4) 0.7279(3) 0.0184(10) Uani 1 1 d . . . . . H33 H 0.9242 0.9387 0.7741 0.022 Uiso 1 1 calc R U . . . C34 C 1.0958(6) 0.9103(4) 0.6952(3) 0.0186(10) Uani 1 1 d . . . . . Cl3 Cl 1.20917(16) 1.02572(10) 0.74321(10) 0.0315(3) Uani 1 1 d . . . . . H37 H 0.388(7) 0.596(4) 0.544(3) 0.052(19) Uiso 1 1 d D . . . . H38 H 0.297(5) 0.503(3) 0.557(4) 0.048(19) Uiso 1 1 d 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 Ho1 0.01092(10) 0.01220(11) 0.01159(10) 0.00220(7) 0.00289(7) 0.00063(7) O1 0.0196(18) 0.0161(18) 0.0168(17) 0.0012(14) 0.0058(14) 0.0018(14) C23 0.011(2) 0.016(2) 0.010(2) 0.0040(18) -0.0006(17) 0.0024(18) O3 0.0160(17) 0.0174(17) 0.0146(16) 0.0020(13) 0.0050(13) -0.0015(14) O4 0.0187(17) 0.0143(17) 0.0152(16) 0.0026(13) 0.0038(14) 0.0007(14) O2 0.0158(17) 0.0169(18) 0.0178(17) 0.0006(14) 0.0038(14) 0.0017(14) C16 0.019(3) 0.013(2) 0.017(2) 0.0038(19) 0.010(2) -0.0009(19) N1 0.014(2) 0.012(2) 0.0140(19) -0.0001(15) 0.0021(16) 0.0003(16) C24 0.013(2) 0.014(2) 0.015(2) 0.0033(18) -0.0001(18) 0.0027(18) N3 0.014(2) 0.0118(19) 0.016(2) 0.0033(16) 0.0039(16) 0.0027(15) N2 0.0133(19) 0.0086(19) 0.0130(19) -0.0015(15) 0.0031(15) -0.0006(15) C17 0.016(2) 0.014(2) 0.018(2) 0.0007(19) 0.0112(19) 0.0003(19) C13 0.016(3) 0.021(3) 0.024(3) 0.000(2) 0.009(2) 0.000(2) C14 0.018(3) 0.018(3) 0.018(2) 0.000(2) 0.003(2) 0.008(2) C5 0.013(2) 0.013(2) 0.014(2) 0.0009(18) 0.0027(18) -0.0026(18) C12 0.018(3) 0.023(3) 0.016(2) 0.003(2) 0.009(2) 0.001(2) C10 0.011(2) 0.015(2) 0.012(2) 0.0014(18) 0.0064(17) 0.0009(18) C4 0.013(2) 0.016(2) 0.017(2) 0.0059(19) 0.0009(19) 0.0030(19) C15 0.014(2) 0.018(3) 0.013(2) 0.0024(19) 0.0022(19) 0.0018(19) C1 0.019(3) 0.014(2) 0.019(2) 0.0037(19) 0.007(2) 0.002(2) C3 0.014(2) 0.019(3) 0.022(3) 0.001(2) 0.003(2) 0.004(2) C29 0.024(3) 0.014(2) 0.021(3) 0.005(2) 0.003(2) 0.004(2) C18 0.021(3) 0.018(3) 0.022(3) 0.006(2) 0.001(2) 0.005(2) C19 0.020(3) 0.025(3) 0.020(3) 0.002(2) 0.000(2) 0.008(2) C2 0.016(2) 0.018(3) 0.025(3) 0.003(2) 0.009(2) 0.004(2) C9 0.020(3) 0.021(3) 0.021(3) 0.006(2) 0.011(2) 0.001(2) Cl1 0.0307(7) 0.0166(6) 0.0250(7) -0.0007(5) -0.0017(5) 0.0033(5) O5 0.0174(17) 0.0180(18) 0.0162(17) 0.0046(14) 0.0064(14) 0.0002(14) OW1 0.0175(18) 0.0167(18) 0.0133(17) 0.0019(14) 0.0028(14) 0.0021(14) C6 0.014(2) 0.013(2) 0.011(2) 0.0003(18) 0.0021(18) 0.0008(18) C20 0.026(3) 0.016(3) 0.018(2) -0.001(2) 0.002(2) -0.004(2) C25 0.013(2) 0.018(3) 0.018(2) -0.001(2) 0.0014(19) 0.0019(19) C21 0.029(3) 0.018(3) 0.019(3) 0.007(2) 0.001(2) 0.004(2) C8 0.030(3) 0.022(3) 0.025(3) 0.012(2) 0.011(2) 0.004(2) C7 0.021(3) 0.021(3) 0.021(3) 0.007(2) 0.005(2) 0.005(2) C22 0.018(3) 0.022(3) 0.019(2) 0.008(2) 0.004(2) -0.002(2) C28 0.021(3) 0.019(3) 0.030(3) 0.007(2) 0.003(2) -0.006(2) C26 0.022(3) 0.021(3) 0.017(2) -0.006(2) -0.002(2) 0.003(2) C11 0.015(2) 0.010(2) 0.016(2) 0.0008(18) 0.0032(19) -0.0035(18) C27 0.024(3) 0.016(3) 0.027(3) 0.000(2) -0.007(2) 0.003(2) Cl2 0.0468(9) 0.0188(7) 0.0405(8) -0.0055(6) -0.0098(7) -0.0010(6) O6 0.0198(18) 0.025(2) 0.0167(17) 0.0018(15) 0.0046(14) -0.0034(15) C32 0.016(2) 0.021(3) 0.016(2) 0.008(2) 0.0029(19) -0.002(2) C31 0.016(2) 0.018(2) 0.014(2) 0.0100(19) 0.0000(19) 0.0001(19) C30 0.012(2) 0.020(3) 0.018(2) 0.010(2) 0.0027(19) 0.0019(19) C36 0.019(3) 0.022(3) 0.019(2) 0.005(2) 0.007(2) 0.002(2) C35 0.012(2) 0.023(3) 0.034(3) 0.005(2) 0.006(2) 0.002(2) C33 0.022(3) 0.017(3) 0.017(2) 0.004(2) 0.007(2) 0.001(2) C34 0.019(3) 0.017(3) 0.020(3) 0.006(2) 0.001(2) -0.003(2) Cl3 0.0350(8) 0.0239(7) 0.0334(8) 0.0013(6) 0.0056(6) -0.0084(6) _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 Ho1 O5 2.266(3) . ? Ho1 OW1 2.331(3) . ? Ho1 O2 2.425(3) . ? Ho1 O4 2.429(3) . ? Ho1 O1 2.476(3) . ? Ho1 O3 2.478(3) . ? Ho1 N1 2.509(4) . ? Ho1 N3 2.536(4) . ? Ho1 N2 2.557(4) . ? Ho1 C16 2.803(5) . ? Ho1 C23 2.823(5) . ? O1 C16 1.279(5) . ? C23 O4 1.267(5) . ? C23 O3 1.270(5) . ? C23 C24 1.486(6) . ? O2 C16 1.265(5) . ? C16 C17 1.486(6) . ? N1 C1 1.348(6) . ? N1 C5 1.359(6) . ? C24 C29 1.392(6) . ? C24 C25 1.394(6) . ? N3 C11 1.336(6) . ? N3 C15 1.337(6) . ? N2 C10 1.357(5) . ? N2 C6 1.357(5) . ? C17 C18 1.382(7) . ? C17 C22 1.411(6) . ? C13 C14 1.378(7) . ? C13 C12 1.385(7) . ? C13 H13 0.9300 . ? C14 C15 1.384(6) . ? C14 H14 0.9300 . ? C5 C4 1.389(6) . ? C5 C6 1.478(6) . ? C12 C11 1.391(6) . ? C12 H12 0.9300 . ? C10 C9 1.384(6) . ? C10 C11 1.489(6) . ? C4 C3 1.375(6) . ? C4 H4 0.9300 . ? C15 H15 0.9300 . ? C1 C2 1.381(6) . ? C1 H1 0.9300 . ? C3 C2 1.379(7) . ? C3 H3 0.9300 . ? C29 C28 1.387(7) . ? C29 H29 0.9300 . ? C18 C19 1.394(7) . ? C18 H18 0.9300 . ? C19 C20 1.376(7) . ? C19 H19 0.9300 . ? C2 H2 0.9300 . ? C9 C8 1.383(7) . ? C9 H9 0.9300 . ? Cl1 C20 1.748(5) . ? O5 C30 1.272(5) . ? OW1 H37 0.96(2) . ? OW1 H38 0.97(2) . ? C6 C7 1.386(6) . ? C20 C21 1.382(7) . ? C25 C26 1.381(6) . ? C25 H25 0.9300 . ? C21 C22 1.371(7) . ? C21 H21 0.9300 . ? C8 C7 1.390(7) . ? C8 H8 0.9300 . ? C7 H7 0.9300 . ? C22 H22 0.9300 . ? C28 C27 1.379(7) . ? C28 H28 0.9300 . ? C26 C27 1.382(7) . ? C26 H26 0.9300 . ? C27 Cl2 1.737(5) . ? O6 C30 1.250(5) . ? C32 C33 1.386(6) . ? C32 C31 1.387(6) . ? C32 H32 0.9300 . ? C31 C36 1.396(6) . ? C31 C30 1.503(7) . ? C36 C35 1.384(7) . ? C36 H36 0.9300 . ? C35 C34 1.380(7) . ? C35 H35 0.9300 . ? C33 C34 1.380(6) . ? C33 H33 0.9300 . ? C34 Cl3 1.751(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 O5 Ho1 OW1 84.55(11) . . ? O5 Ho1 O2 75.20(11) . . ? OW1 Ho1 O2 75.14(11) . . ? O5 Ho1 O4 134.28(11) . . ? OW1 Ho1 O4 81.01(11) . . ? O2 Ho1 O4 139.84(11) . . ? O5 Ho1 O1 82.74(11) . . ? OW1 Ho1 O1 129.04(11) . . ? O2 Ho1 O1 53.90(11) . . ? O4 Ho1 O1 138.16(10) . . ? O5 Ho1 O3 81.16(11) . . ? OW1 Ho1 O3 76.01(11) . . ? O2 Ho1 O3 144.05(11) . . ? O4 Ho1 O3 53.30(10) . . ? O1 Ho1 O3 148.49(10) . . ? O5 Ho1 N1 81.34(12) . . ? OW1 Ho1 N1 145.32(11) . . ? O2 Ho1 N1 130.24(11) . . ? O4 Ho1 N1 86.51(11) . . ? O1 Ho1 N1 80.29(11) . . ? O3 Ho1 N1 70.63(11) . . ? O5 Ho1 N3 143.77(12) . . ? OW1 Ho1 N3 79.21(12) . . ? O2 Ho1 N3 69.43(11) . . ? O4 Ho1 N3 74.74(11) . . ? O1 Ho1 N3 82.79(11) . . ? O3 Ho1 N3 124.84(11) . . ? N1 Ho1 N3 128.25(12) . . ? O5 Ho1 N2 139.34(12) . . ? OW1 Ho1 N2 136.11(12) . . ? O2 Ho1 N2 110.46(11) . . ? O4 Ho1 N2 67.25(11) . . ? O1 Ho1 N2 71.26(11) . . ? O3 Ho1 N2 105.15(11) . . ? N1 Ho1 N2 64.18(12) . . ? N3 Ho1 N2 64.08(12) . . ? O5 Ho1 C16 77.04(12) . . ? OW1 Ho1 C16 101.91(13) . . ? O2 Ho1 C16 26.78(12) . . ? O4 Ho1 C16 148.43(12) . . ? O1 Ho1 C16 27.14(12) . . ? O3 Ho1 C16 158.20(12) . . ? N1 Ho1 C16 105.49(13) . . ? N3 Ho1 C16 75.00(13) . . ? N2 Ho1 C16 91.43(12) . . ? O5 Ho1 C23 107.83(12) . . ? OW1 Ho1 C23 77.35(12) . . ? O2 Ho1 C23 151.90(12) . . ? O4 Ho1 C23 26.58(11) . . ? O1 Ho1 C23 153.12(12) . . ? O3 Ho1 C23 26.72(11) . . ? N1 Ho1 C23 77.13(12) . . ? N3 Ho1 C23 99.92(13) . . ? N2 Ho1 C23 85.78(12) . . ? C16 Ho1 C23 174.90(13) . . ? C16 O1 Ho1 90.8(3) . . ? O4 C23 O3 120.4(4) . . ? O4 C23 C24 119.6(4) . . ? O3 C23 C24 120.1(4) . . ? O4 C23 Ho1 59.1(2) . . ? O3 C23 Ho1 61.3(2) . . ? C24 C23 Ho1 178.2(3) . . ? C23 O3 Ho1 92.0(3) . . ? C23 O4 Ho1 94.4(3) . . ? C16 O2 Ho1 93.5(3) . . ? O2 C16 O1 121.7(4) . . ? O2 C16 C17 118.1(4) . . ? O1 C16 C17 120.3(4) . . ? O2 C16 Ho1 59.7(2) . . ? O1 C16 Ho1 62.0(2) . . ? C17 C16 Ho1 177.0(3) . . ? C1 N1 C5 117.5(4) . . ? C1 N1 Ho1 120.1(3) . . ? C5 N1 Ho1 122.4(3) . . ? C29 C24 C25 118.7(4) . . ? C29 C24 C23 120.5(4) . . ? C25 C24 C23 120.8(4) . . ? C11 N3 C15 118.4(4) . . ? C11 N3 Ho1 121.7(3) . . ? C15 N3 Ho1 119.9(3) . . ? C10 N2 C6 119.0(4) . . ? C10 N2 Ho1 120.2(3) . . ? C6 N2 Ho1 119.8(3) . . ? C18 C17 C22 118.9(4) . . ? C18 C17 C16 121.6(4) . . ? C22 C17 C16 119.6(4) . . ? C14 C13 C12 118.5(4) . . ? C14 C13 H13 120.8 . . ? C12 C13 H13 120.8 . . ? C13 C14 C15 118.8(4) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? N1 C5 C4 121.3(4) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.9(4) . . ? C13 C12 C11 119.4(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? N2 C10 C9 121.8(4) . . ? N2 C10 C11 116.4(4) . . ? C9 C10 C11 121.8(4) . . ? C3 C4 C5 120.2(4) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? N3 C15 C14 123.0(4) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? N1 C1 C2 123.3(4) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C4 C3 C2 118.7(4) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C28 C29 C24 120.8(5) . . ? C28 C29 H29 119.6 . . ? C24 C29 H29 119.6 . . ? C17 C18 C19 121.0(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 118.4(5) . . ? C20 C19 H19 120.8 . . ? C18 C19 H19 120.8 . . ? C3 C2 C1 118.8(4) . . ? C3 C2 H2 120.6 . . ? C1 C2 H2 120.6 . . ? C8 C9 C10 119.5(4) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C30 O5 Ho1 170.1(3) . . ? Ho1 OW1 H37 126(4) . . ? Ho1 OW1 H38 117(4) . . ? H37 OW1 H38 100(5) . . ? N2 C6 C7 121.3(4) . . ? N2 C6 C5 116.8(4) . . ? C7 C6 C5 121.9(4) . . ? C19 C20 C21 122.1(5) . . ? C19 C20 Cl1 118.7(4) . . ? C21 C20 Cl1 119.3(4) . . ? C26 C25 C24 120.9(5) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C22 C21 C20 119.2(5) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C9 C8 C7 118.8(5) . . ? C9 C8 H8 120.6 . . ? C7 C8 H8 120.6 . . ? C6 C7 C8 119.7(5) . . ? C6 C7 H7 120.1 . . ? C8 C7 H7 120.1 . . ? C21 C22 C17 120.4(5) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? C27 C28 C29 119.2(5) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C25 C26 C27 119.3(5) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? N3 C11 C12 121.9(4) . . ? N3 C11 C10 117.0(4) . . ? C12 C11 C10 121.2(4) . . ? C28 C27 C26 121.2(5) . . ? C28 C27 Cl2 119.2(4) . . ? C26 C27 Cl2 119.6(4) . . ? C33 C32 C31 121.3(4) . . ? C33 C32 H32 119.4 . . ? C31 C32 H32 119.4 . . ? C32 C31 C36 119.0(4) . . ? C32 C31 C30 120.4(4) . . ? C36 C31 C30 120.6(4) . . ? O6 C30 O5 125.5(4) . . ? O6 C30 C31 117.3(4) . . ? O5 C30 C31 117.2(4) . . ? C35 C36 C31 120.3(5) . . ? C35 C36 H36 119.9 . . ? C31 C36 H36 119.9 . . ? C34 C35 C36 119.3(5) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C34 C33 C32 118.4(4) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C35 C34 C33 121.7(5) . . ? C35 C34 Cl3 118.8(4) . . ? C33 C34 Cl3 119.4(4) . . ? _refine_diff_density_max 0.996 _refine_diff_density_min -1.514 _refine_diff_density_rms 0.195 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.7028 13.0998 14.7613 100.253 97.766 92.399 ZERR 2.00 0.0021 0.0032 0.0036 0.004 0.004 0.004 LATT 1 SFAC C H N O CL HO UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 12 WGHT 0.028100 FVAR 0.11854 HO1 6 0.562348 0.512966 0.701652 11.00000 0.01092 0.01220 = 0.01159 0.00220 0.00289 0.00063 O1 4 0.711223 0.622966 0.842567 11.00000 0.01964 0.01615 = 0.01680 0.00122 0.00575 0.00178 C23 1 0.459753 0.319799 0.586139 11.00000 0.01055 0.01632 = 0.01007 0.00405 -0.00061 0.00240 O3 4 0.561535 0.377147 0.561283 11.00000 0.01597 0.01745 = 0.01458 0.00204 0.00499 -0.00152 O4 4 0.404432 0.349695 0.660788 11.00000 0.01866 0.01431 = 0.01517 0.00264 0.00377 0.00070 O2 4 0.536120 0.696487 0.755515 11.00000 0.01577 0.01686 = 0.01776 0.00060 0.00383 0.00172 C16 1 0.641503 0.702634 0.824672 11.00000 0.01911 0.01279 = 0.01698 0.00377 0.01033 -0.00092 N1 3 0.791166 0.405469 0.725421 11.00000 0.01353 0.01215 = 0.01401 -0.00013 0.00210 0.00031 C24 1 0.405665 0.216659 0.527935 11.00000 0.01279 0.01399 = 0.01456 0.00327 -0.00015 0.00274 N3 3 0.339556 0.538498 0.796098 11.00000 0.01406 0.01180 = 0.01612 0.00329 0.00393 0.00269 N2 3 0.569458 0.414375 0.836772 11.00000 0.01329 0.00860 = 0.01301 -0.00153 0.00310 -0.00056 C17 1 0.683017 0.805903 0.885556 11.00000 0.01626 0.01432 = 0.01812 0.00069 0.01116 0.00029 C13 1 0.090679 0.567626 0.895466 11.00000 0.01608 0.02059 = 0.02381 0.00027 0.00875 0.00041 AFIX 43 H13 2 0.006835 0.576607 0.928376 11.00000 -1.20000 AFIX 0 C14 1 0.102403 0.617306 0.821594 11.00000 0.01794 0.01796 = 0.01760 0.00042 0.00302 0.00772 AFIX 43 H14 2 0.026576 0.660641 0.803730 11.00000 -1.20000 AFIX 0 C5 1 0.810181 0.348691 0.794275 11.00000 0.01318 0.01256 = 0.01450 0.00091 0.00269 -0.00258 C12 1 0.206707 0.504003 0.919544 11.00000 0.01801 0.02293 = 0.01607 0.00292 0.00941 0.00100 AFIX 43 H12 2 0.203771 0.471535 0.970476 11.00000 -1.20000 AFIX 0 C10 1 0.448565 0.415566 0.886047 11.00000 0.01098 0.01482 = 0.01161 0.00135 0.00637 0.00086 C4 1 0.942399 0.294769 0.809662 11.00000 0.01341 0.01558 = 0.01731 0.00587 0.00093 0.00304 AFIX 43 H4 2 0.953302 0.256762 0.857429 11.00000 -1.20000 AFIX 0 C15 1 0.229032 0.601552 0.774476 11.00000 0.01438 0.01807 = 0.01325 0.00238 0.00216 0.00178 AFIX 43 H15 2 0.237604 0.636421 0.725552 11.00000 -1.20000 AFIX 0 C1 1 0.902622 0.404216 0.670129 11.00000 0.01889 0.01444 = 0.01922 0.00367 0.00721 0.00161 AFIX 43 H1 2 0.888671 0.440157 0.621000 11.00000 -1.20000 AFIX 0 C3 1 1.057188 0.297423 0.754484 11.00000 0.01435 0.01875 = 0.02204 0.00078 0.00332 0.00353 AFIX 43 H3 2 1.147135 0.262872 0.765342 11.00000 -1.20000 AFIX 0 C29 1 0.291670 0.154221 0.553410 11.00000 0.02397 0.01370 = 0.02127 0.00522 0.00275 0.00449 AFIX 43 H29 2 0.247786 0.177896 0.606691 11.00000 -1.20000 AFIX 0 C18 1 0.806005 0.820968 0.957370 11.00000 0.02141 0.01817 = 0.02185 0.00617 0.00100 0.00493 AFIX 43 H18 2 0.865345 0.765577 0.967535 11.00000 -1.20000 AFIX 0 C19 1 0.842471 0.917928 1.014804 11.00000 0.01999 0.02482 = 0.01984 0.00234 -0.00014 0.00767 AFIX 43 H19 2 0.924516 0.927623 1.063559 11.00000 -1.20000 AFIX 0 C2 1 1.036428 0.352277 0.682749 11.00000 0.01574 0.01809 = 0.02459 0.00316 0.00904 0.00357 AFIX 43 H2 2 1.111220 0.354265 0.643549 11.00000 -1.20000 AFIX 0 C9 1 0.436580 0.350350 0.949266 11.00000 0.02043 0.02083 = 0.02134 0.00605 0.01102 0.00056 AFIX 43 H9 2 0.354405 0.354098 0.983722 11.00000 -1.20000 AFIX 0 CL1 5 0.796898 1.120233 1.070563 11.00000 0.03073 0.01660 = 0.02499 -0.00065 -0.00169 0.00331 O5 4 0.728693 0.595752 0.628706 11.00000 0.01742 0.01795 = 0.01615 0.00463 0.00636 0.00023 OW1 4 0.370522 0.558723 0.592670 11.00000 0.01746 0.01667 = 0.01330 0.00186 0.00279 0.00208 C6 1 0.680570 0.346496 0.849221 11.00000 0.01440 0.01278 = 0.01075 0.00026 0.00212 0.00081 C20 1 0.754118 0.998966 0.997611 11.00000 0.02634 0.01593 = 0.01829 -0.00051 0.00189 -0.00404 C25 1 0.470753 0.179364 0.448197 11.00000 0.01333 0.01794 = 0.01815 -0.00084 0.00140 0.00186 AFIX 43 H25 2 0.545031 0.221025 0.429447 11.00000 -1.20000 AFIX 0 C21 1 0.632512 0.987085 0.925143 11.00000 0.02936 0.01792 = 0.01871 0.00726 0.00141 0.00435 AFIX 43 H21 2 0.576056 1.043466 0.914124 11.00000 -1.20000 AFIX 0 C8 1 0.547806 0.279522 0.960817 11.00000 0.02957 0.02248 = 0.02458 0.01151 0.01140 0.00378 AFIX 43 H8 2 0.540014 0.233785 1.001735 11.00000 -1.20000 AFIX 0 C7 1 0.671418 0.278002 0.910118 11.00000 0.02138 0.02141 = 0.02150 0.00708 0.00499 0.00496 AFIX 43 H7 2 0.747682 0.231199 0.917040 11.00000 -1.20000 AFIX 0 C22 1 0.596101 0.891166 0.869682 11.00000 0.01796 0.02196 = 0.01859 0.00784 0.00423 -0.00191 AFIX 43 H22 2 0.513553 0.882246 0.821273 11.00000 -1.20000 AFIX 0 C28 1 0.242733 0.057124 0.500296 11.00000 0.02094 0.01851 = 0.03023 0.00747 0.00252 -0.00630 AFIX 43 H28 2 0.164101 0.016709 0.516509 11.00000 -1.20000 AFIX 0 C26 1 0.426367 0.081372 0.396699 11.00000 0.02191 0.02127 = 0.01720 -0.00609 -0.00212 0.00313 AFIX 43 H26 2 0.472835 0.056103 0.344790 11.00000 -1.20000 AFIX 0 C11 1 0.327637 0.489127 0.866849 11.00000 0.01467 0.01041 = 0.01588 0.00075 0.00319 -0.00351 C27 1 0.312104 0.021258 0.423161 11.00000 0.02353 0.01609 = 0.02730 0.00021 -0.00661 0.00284 CL2 5 0.249952 -0.099999 0.356140 11.00000 0.04681 0.01879 = 0.04048 -0.00553 -0.00979 -0.00099 O6 4 0.847241 0.580339 0.501689 11.00000 0.01979 0.02483 = 0.01668 0.00183 0.00462 -0.00337 C32 1 0.872238 0.797779 0.690408 11.00000 0.01567 0.02091 = 0.01604 0.00838 0.00295 -0.00153 AFIX 43 H32 2 0.780348 0.782945 0.712590 11.00000 -1.20000 AFIX 0 C31 1 0.920573 0.726479 0.620396 11.00000 0.01587 0.01785 = 0.01418 0.01001 -0.00003 0.00008 C30 1 0.824735 0.626602 0.579936 11.00000 0.01204 0.02003 = 0.01806 0.00957 0.00274 0.00187 C36 1 1.058279 0.749609 0.587211 11.00000 0.01910 0.02177 = 0.01857 0.00481 0.00709 0.00196 AFIX 43 H36 2 1.091223 0.702947 0.539658 11.00000 -1.20000 AFIX 0 C35 1 1.145956 0.841676 0.624780 11.00000 0.01156 0.02304 = 0.03404 0.00543 0.00605 0.00159 AFIX 43 H35 2 1.237756 0.857128 0.602765 11.00000 -1.20000 AFIX 0 C33 1 0.958307 0.890733 0.727946 11.00000 0.02195 0.01701 = 0.01749 0.00358 0.00681 0.00080 AFIX 43 H33 2 0.924221 0.938750 0.774067 11.00000 -1.20000 AFIX 0 C34 1 1.095771 0.910308 0.695236 11.00000 0.01883 0.01660 = 0.02023 0.00553 0.00052 -0.00348 CL3 5 1.209173 1.025715 0.743209 11.00000 0.03504 0.02389 = 0.03336 0.00130 0.00557 -0.00835 H37 2 0.388463 0.596441 0.544443 11.00000 0.05176 H38 2 0.296944 0.503361 0.556696 11.00000 0.04828 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0468 for 6840 Fo > 4sig(Fo) and 0.0729 for all 8961 data REM 459 parameters refined using 2 restraints END WGHT 0.0285 0.0000 REM Highest difference peak 0.996, deepest hole -1.514, 1-sigma level 0.195 Q1 1 0.5759 0.5657 0.7244 11.00000 0.05 1.00 Q2 1 1.3118 0.9979 0.7199 11.00000 0.05 0.90 Q3 1 0.7955 0.7641 0.9723 11.00000 0.05 0.88 Q4 1 0.5643 0.4971 0.7343 11.00000 0.05 0.84 Q5 1 0.6617 0.4789 0.7750 11.00000 0.05 0.84 Q6 1 0.3944 0.1372 0.9009 11.00000 0.05 0.78 Q7 1 1.0460 0.9039 0.9837 11.00000 0.05 0.77 Q8 1 0.4917 0.5335 0.6119 11.00000 0.05 0.74 Q9 1 0.4437 0.5673 0.7382 11.00000 0.05 0.73 Q10 1 0.3029 -0.1785 0.4022 11.00000 0.05 0.73 ; _shelx_res_checksum 50425 _shelx_hkl_file ; -1 0 0 300.32 9.56 -1 0 0 312.07 8.97 -1 0 0 312.92 9.00 1 0 0 303.82 9.24 1 0 0 306.82 8.98 -2 0 0 -0.66 1.10 -2 0 0 1.44 1.12 -2 0 0 1.02 0.87 2 0 0 1.32 1.21 -3 0 0 94.93 3.98 -3 0 0 92.21 4.76 -3 0 0 96.28 4.47 3 0 0 98.15 4.73 -4 0 0 -0.55 1.36 -4 0 0 1.03 1.47 -4 0 0 0.15 1.08 4 0 0 0.72 1.47 -5 0 0 45.90 4.47 -5 0 0 49.66 3.21 -5 0 0 46.40 4.20 5 0 0 47.47 4.42 -6 0 0 97.31 4.89 -6 0 0 102.18 6.15 -6 0 0 107.38 6.65 6 0 0 105.66 6.27 -7 0 0 38.02 5.05 -7 0 0 42.60 4.82 7 0 0 36.70 4.70 -8 0 0 139.36 9.11 -8 0 0 168.39 8.89 8 0 0 140.26 8.68 -9 0 0 76.38 7.50 -9 0 0 69.63 7.72 9 0 0 69.20 7.13 -10 0 0 19.04 4.59 10 0 0 21.57 4.55 -11 0 0 12.23 4.47 11 0 0 5.08 4.44 -11 1 0 15.26 4.50 10 -1 0 29.94 5.34 -10 1 0 20.15 4.66 -10 1 0 18.43 4.68 9 -1 0 42.16 5.91 -9 1 0 49.53 6.38 -9 1 0 43.81 5.71 8 -1 0 125.76 8.26 -8 1 0 124.34 7.73 -8 1 0 142.95 8.68 7 -1 0 68.27 6.41 7 -1 0 67.14 4.33 7 -1 0 63.67 4.23 -7 1 0 76.34 6.34 -7 1 0 67.15 5.55 6 -1 0 10.89 2.73 -6 1 0 8.98 2.44 -6 1 0 9.46 2.57 5 -1 0 -1.45 1.53 -5 1 0 -0.65 1.44 -5 1 0 2.42 1.41 -5 1 0 0.89 1.50 4 -1 0 5.54 1.97 -4 1 0 4.83 1.87 -4 1 0 4.78 1.47 -4 1 0 7.83 1.85 -3 1 0 54.31 3.65 -3 1 0 48.29 3.16 -3 1 0 52.24 3.02 -2 1 0 550.24 15.99 -2 1 0 512.81 16.68 -2 1 0 540.59 16.35 -2 1 0 521.08 15.46 1 -1 0 363.68 11.02 1 -1 0 368.66 11.31 1 -1 0 386.33 10.61 -1 1 0 382.30 10.61 -1 1 0 389.53 11.39 -1 1 0 361.98 11.53 0 -1 0 363.90 10.97 0 1 0 375.43 11.16 0 1 0 375.95 10.84 -1 -1 0 248.15 7.64 -1 -1 0 237.41 7.46 1 1 0 252.66 7.67 1 1 0 260.57 8.33 -2 -1 0 125.17 5.10 -2 -1 0 128.96 4.41 -2 -1 0 129.39 5.41 2 1 0 123.23 4.93 -3 -1 0 11.12 1.43 -3 -1 0 9.58 1.94 -3 -1 0 12.05 2.06 3 1 0 11.01 1.89 -4 -1 0 37.22 3.74 -4 -1 0 37.69 2.49 -4 -1 0 44.98 3.90 4 1 0 38.10 3.50 -5 -1 0 7.65 1.55 -5 -1 0 8.47 2.14 -5 -1 0 5.96 2.13 5 1 0 7.12 2.08 -6 -1 0 75.91 5.61 -6 -1 0 82.58 5.53 -6 -1 0 79.16 4.07 6 1 0 77.37 5.31 -7 -1 0 114.41 7.18 -7 -1 0 126.95 7.94 7 1 0 113.29 7.07 -8 -1 0 40.84 5.42 8 1 0 43.72 5.26 -9 -1 0 56.95 6.63 9 1 0 56.17 7.50 9 1 0 44.44 5.78 -10 -1 0 42.47 6.11 10 1 0 24.58 5.93 -11 -1 0 10.69 4.14 11 1 0 4.86 4.50 -12 -1 0 2.20 3.60 11 -2 0 13.35 4.77 -11 2 0 12.12 4.55 10 -2 0 4.35 3.54 -10 2 0 11.32 3.75 -10 2 0 4.72 3.23 9 -2 0 42.29 6.13 -9 2 0 51.12 6.53 -9 2 0 48.77 5.89 8 -2 0 59.92 6.62 -8 2 0 62.09 5.96 -8 2 0 54.51 6.26 7 -2 0 38.50 3.78 7 -2 0 42.66 5.27 7 -2 0 35.81 3.82 -7 2 0 38.82 4.84 -7 2 0 46.02 4.81 6 -2 0 34.48 4.40 6 -2 0 26.63 3.00 6 -2 0 28.14 3.19 -6 2 0 19.63 3.33 -6 2 0 28.87 3.54 5 -2 0 16.35 2.41 5 -2 0 18.32 2.44 5 -2 0 22.93 3.44 -5 2 0 13.38 2.64 -5 2 0 22.58 2.79 4 -2 0 13.99 2.02 4 -2 0 17.03 2.36 -4 2 0 14.21 2.41 -4 2 0 15.04 2.12 -4 2 0 13.72 2.44 3 -2 0 5.77 1.52 3 -2 0 5.71 1.63 -3 2 0 6.16 1.65 -3 2 0 5.47 1.73 -3 2 0 7.06 1.51 2 -2 0 9.48 1.74 2 -2 0 8.17 1.51 -2 2 0 6.65 1.47 -2 2 0 12.65 2.02 -2 2 0 9.39 1.25 1 -2 0 178.37 6.26 1 -2 0 170.38 5.12 1 -2 0 177.48 5.12 -1 2 0 173.63 6.17 -1 2 0 167.61 6.00 0 -2 0 367.47 10.78 0 -2 0 351.61 9.83 0 2 0 341.52 10.49 0 2 0 306.18 10.70 -1 -2 0 164.25 5.95 -1 -2 0 175.75 5.91 1 2 0 180.64 6.63 1 2 0 177.65 5.97 -2 -2 0 4.29 1.50 -2 -2 0 2.54 1.12 2 2 0 6.38 1.43 2 2 0 6.08 1.86 -3 -2 0 68.06 3.15 -3 -2 0 64.50 3.96 3 2 0 62.32 3.78 3 2 0 69.77 4.51 -4 -2 0 3.77 1.76 -4 -2 0 6.22 1.32 4 2 0 0.99 1.50 -5 -2 0 103.94 4.49 -5 -2 0 98.82 5.78 5 2 0 98.40 5.54 -6 -2 0 83.56 4.23 -6 -2 0 82.86 5.69 6 2 0 90.89 5.73 -7 -2 0 58.41 5.86 7 2 0 46.43 6.23 7 2 0 41.92 4.88 -8 -2 0 23.72 4.40 8 2 0 23.08 4.23 8 2 0 28.63 5.68 -9 -2 0 78.27 7.74 9 2 0 90.13 8.08 9 2 0 96.38 10.11 -10 -2 0 28.88 5.51 10 2 0 20.14 5.39 -11 -2 0 1.73 3.23 11 2 0 3.70 4.04 11 -3 0 8.95 4.55 -11 3 0 11.52 4.22 10 -3 0 10.86 4.24 -10 3 0 13.58 4.03 9 -3 0 23.53 5.03 -9 3 0 35.26 4.92 -9 3 0 45.73 6.08 8 -3 0 97.71 7.67 -8 3 0 119.24 7.68 -8 3 0 101.44 6.67 7 -3 0 23.48 3.32 7 -3 0 13.96 3.55 -7 3 0 20.66 3.40 -7 3 0 15.85 3.39 6 -3 0 3.68 1.70 6 -3 0 3.51 1.79 6 -3 0 3.78 2.34 -6 3 0 3.96 2.21 -6 3 0 2.83 1.87 5 -3 0 0.79 1.39 5 -3 0 2.33 1.54 -5 3 0 -0.67 1.49 -5 3 0 0.89 1.63 -5 3 0 1.01 1.39 4 -3 0 -0.56 1.38 4 -3 0 -0.14 1.27 -4 3 0 -0.88 1.17 -4 3 0 -1.21 1.13 -4 3 0 1.29 1.74 3 -3 0 58.76 3.74 3 -3 0 47.91 3.50 -3 3 0 48.25 3.64 -3 3 0 53.04 3.55 -3 3 0 49.02 2.79 2 -3 0 95.61 4.69 -2 3 0 91.91 4.75 -2 3 0 87.04 4.32 1 -3 0 53.97 2.08 1 -3 0 59.62 3.47 -1 3 0 53.63 3.11 -1 3 0 54.98 3.29 0 -3 0 21.95 2.36 0 -3 0 24.12 1.78 0 3 0 23.53 2.26 0 3 0 27.21 2.38 -1 -3 0 175.32 6.36 -1 -3 0 164.66 6.02 1 3 0 154.22 6.61 1 3 0 181.99 6.25 -2 -3 0 3.37 1.56 -2 -3 0 3.43 1.32 2 3 0 -0.09 1.19 2 3 0 2.97 1.62 -3 -3 0 13.46 2.43 -3 -3 0 12.90 1.78 3 3 0 11.40 1.97 3 3 0 11.51 2.61 -4 -3 0 11.17 2.38 -4 -3 0 13.40 1.75 4 3 0 11.59 2.82 4 3 0 13.07 2.24 -5 -3 0 26.95 3.71 -5 -3 0 26.93 2.49 5 3 0 26.19 3.27 5 3 0 30.35 4.29 -6 -3 0 58.19 5.80 6 3 0 44.37 4.65 6 3 0 63.54 6.85 -7 -3 0 117.56 7.54 7 3 0 128.37 9.03 7 3 0 130.96 7.55 -8 -3 0 2.77 2.70 8 3 0 3.90 3.39 8 3 0 4.60 2.60 -9 -3 0 36.11 5.48 9 3 0 30.28 5.93 -10 -3 0 4.21 3.75 10 3 0 7.25 4.12 -11 -3 0 -2.37 2.53 11 3 0 -4.96 3.29 11 -4 0 3.74 4.19 -11 4 0 11.79 4.42 10 -4 0 47.55 7.18 -10 4 0 33.90 5.74 9 -4 0 50.76 6.94 -9 4 0 56.90 6.77 8 -4 0 57.99 6.86 -8 4 0 65.11 6.86 -8 4 0 65.53 5.91 7 -4 0 5.27 2.98 7 -4 0 14.75 3.06 -7 4 0 8.50 2.45 -7 4 0 2.18 2.43 6 -4 0 3.22 1.97 -6 4 0 2.75 1.75 -6 4 0 0.54 1.71 5 -4 0 -0.41 1.37 -5 4 0 0.17 1.61 -5 4 0 -1.33 1.21 -5 4 0 -1.98 1.37 4 -4 0 0.02 1.54 -4 4 0 2.34 1.57 -4 4 0 -0.18 1.10 -4 4 0 0.68 1.78 3 -4 0 7.19 2.16 -3 4 0 9.87 2.24 -3 4 0 15.02 2.36 2 -4 0 138.68 4.41 2 -4 0 135.00 6.29 -2 4 0 128.26 5.72 -2 4 0 130.22 6.32 1 -4 0 137.50 6.27 1 -4 0 138.69 4.56 -1 4 0 147.48 5.93 -1 4 0 135.30 5.97 0 -4 0 5.93 1.95 0 -4 0 4.01 1.19 0 4 0 4.02 1.68 0 4 0 4.89 1.64 -1 -4 0 155.18 5.86 -1 -4 0 146.29 6.31 1 4 0 148.22 5.98 1 4 0 147.57 6.57 -2 -4 0 86.28 4.37 -2 -4 0 85.47 4.63 2 4 0 87.16 5.10 2 4 0 91.41 4.49 -3 -4 0 3.02 1.35 -3 -4 0 6.53 1.88 3 4 0 4.61 2.22 3 4 0 2.51 1.57 -4 -4 0 12.43 1.83 -4 -4 0 10.33 2.57 4 4 0 12.95 2.27 4 4 0 12.33 2.98 -5 -4 0 15.06 2.11 -5 -4 0 15.69 2.99 5 4 0 18.65 2.91 5 4 0 17.57 3.57 -6 -4 0 74.05 5.69 6 4 0 76.55 7.55 6 4 0 78.24 5.43 -7 -4 0 26.30 4.50 7 4 0 29.42 4.19 7 4 0 33.46 5.51 -8 -4 0 29.98 5.13 8 4 0 23.74 4.19 8 4 0 27.35 5.30 -9 -4 0 31.40 5.30 9 4 0 31.11 6.29 -10 -4 0 15.75 4.57 10 4 0 11.11 4.94 -11 -4 0 0.92 3.37 11 4 0 2.19 3.98 11 -5 0 13.19 4.99 -11 5 0 24.14 5.37 10 -5 0 60.14 7.81 -10 5 0 53.86 7.16 9 -5 0 44.83 6.41 -9 5 0 39.86 5.90 8 -5 0 36.36 5.85 8 -5 0 46.22 5.43 -8 5 0 46.01 5.94 7 -5 0 10.46 3.38 7 -5 0 11.98 3.10 -7 5 0 12.55 2.75 -7 5 0 8.81 3.00 6 -5 0 12.01 2.96 -6 5 0 17.39 3.51 -6 5 0 13.05 2.96 -6 5 0 16.19 2.60 5 -5 0 2.25 1.98 -5 5 0 2.58 1.91 -5 5 0 2.47 1.40 -5 5 0 5.98 2.47 4 -5 0 84.70 3.81 4 -5 0 85.95 5.58 -4 5 0 85.16 5.72 -4 5 0 92.05 5.22 3 -5 0 0.84 1.83 3 -5 0 1.68 0.85 -3 5 0 1.86 1.76 -3 5 0 0.14 1.37 2 -5 0 87.12 3.09 2 -5 0 91.49 5.36 -2 5 0 77.12 4.49 -2 5 0 78.44 5.05 1 -5 0 199.93 8.09 1 -5 0 179.37 5.77 -1 5 0 164.33 7.21 -1 5 0 162.84 7.42 0 -5 0 92.45 4.02 0 -5 0 89.89 5.17 0 5 0 87.22 4.90 0 5 0 96.57 4.75 -1 -5 0 32.48 2.87 -1 -5 0 32.30 3.36 1 5 0 38.09 3.75 1 5 0 41.27 3.39 -2 -5 0 177.27 7.38 -2 -5 0 180.51 7.34 2 5 0 191.56 8.38 2 5 0 174.63 7.29 -3 -5 0 5.71 1.68 -3 -5 0 3.85 1.82 3 5 0 2.61 2.19 3 5 0 6.91 1.88 -4 -5 0 40.24 3.37 -4 -5 0 45.33 4.48 4 5 0 34.73 3.55 4 5 0 44.54 5.11 -5 -5 0 27.40 3.98 -5 -5 0 31.60 3.03 5 5 0 33.50 3.78 5 5 0 37.39 5.11 -6 -5 0 53.49 5.82 6 5 0 47.64 4.88 6 5 0 48.77 6.07 -7 -5 0 31.78 4.85 7 5 0 31.51 4.38 7 5 0 33.82 5.66 -8 -5 0 57.74 6.80 8 5 0 50.10 7.17 -9 -5 0 10.49 3.72 9 5 0 8.19 4.06 -10 -5 0 1.39 3.28 10 5 0 6.22 4.02 11 -6 0 20.89 5.92 -11 6 0 11.36 4.62 10 -6 0 9.16 4.54 -10 6 0 18.31 4.67 9 -6 0 31.14 5.95 -9 6 0 48.81 6.39 8 -6 0 59.15 6.33 8 -6 0 52.24 6.72 -8 6 0 53.31 6.24 7 -6 0 20.70 4.06 -7 6 0 26.67 4.08 -7 6 0 9.18 3.14 6 -6 0 18.32 3.71 -6 6 0 15.78 3.22 -6 6 0 14.14 3.62 5 -6 0 2.12 2.07 5 -6 0 0.52 1.10 -5 6 0 3.43 1.95 -5 6 0 -0.08 2.00 4 -6 0 18.84 1.83 4 -6 0 19.36 3.38 -4 6 0 21.21 3.12 -4 6 0 22.90 3.59 3 -6 0 129.27 4.53 3 -6 0 133.96 7.21 -3 6 0 136.68 7.01 -3 6 0 131.84 6.45 2 -6 0 95.61 3.54 2 -6 0 97.95 6.03 -2 6 0 96.02 5.19 -2 6 0 102.75 5.86 1 -6 0 29.76 2.05 1 -6 0 35.45 3.78 -1 6 0 31.09 3.39 -1 6 0 27.73 3.18 0 -6 0 58.51 4.28 0 -6 0 54.47 3.21 0 6 0 53.80 4.05 0 6 0 63.13 4.27 -1 -6 0 376.05 12.71 1 6 0 391.57 13.46 1 6 0 396.26 14.31 -2 -6 0 5.99 1.90 -2 -6 0 5.64 2.07 2 6 0 6.01 2.35 2 6 0 6.30 1.94 -3 -6 0 48.84 4.43 -3 -6 0 49.08 4.10 3 6 0 41.38 3.80 3 6 0 33.07 4.22 -4 -6 0 9.95 2.62 -4 -6 0 11.94 2.32 4 6 0 10.70 3.11 4 6 0 8.51 2.31 -5 -6 0 64.86 6.02 -5 -6 0 66.15 4.24 5 6 0 66.23 6.72 5 6 0 70.45 4.99 -6 -6 0 30.52 4.69 6 6 0 25.81 3.77 6 6 0 39.10 5.57 -7 -6 0 42.57 5.76 7 6 0 59.69 7.27 -8 -6 0 57.78 6.94 8 6 0 43.22 6.83 -9 -6 0 20.05 4.72 9 6 0 24.73 5.69 -10 -6 0 3.62 3.40 10 6 0 -2.78 2.95 11 -7 0 7.76 4.56 -11 7 0 1.97 3.85 10 -7 0 25.92 5.95 -10 7 0 31.94 5.93 9 -7 0 51.67 7.34 -9 7 0 43.22 6.11 8 -7 0 2.71 3.00 -8 7 0 0.81 2.59 7 -7 0 43.32 5.64 -7 7 0 48.06 6.08 -7 7 0 40.49 5.25 6 -7 0 15.66 3.69 -6 7 0 14.27 3.67 -6 7 0 11.28 2.96 5 -7 0 28.93 4.56 -5 7 0 31.84 4.69 -5 7 0 31.39 4.01 4 -7 0 80.62 3.33 4 -7 0 75.41 5.98 -4 7 0 85.31 5.35 -4 7 0 73.18 5.62 3 -7 0 39.47 1.98 3 -7 0 34.23 4.45 -3 7 0 31.54 4.06 -3 7 0 34.50 3.80 2 -7 0 83.00 5.64 2 -7 0 82.51 3.31 -2 7 0 73.43 4.77 -2 7 0 84.40 5.59 1 -7 0 350.82 13.68 1 -7 0 350.62 10.85 -1 7 0 330.82 12.81 -1 7 0 349.59 13.16 0 -7 0 43.96 4.71 0 -7 0 49.69 3.24 0 7 0 49.05 4.46 0 7 0 53.69 4.70 -1 -7 0 -0.76 1.76 -1 -7 0 1.30 1.38 1 7 0 2.66 1.78 1 7 0 4.12 2.07 -2 -7 0 18.15 3.00 -2 -7 0 12.99 2.52 2 7 0 15.43 3.15 2 7 0 23.13 3.00 -3 -7 0 -1.34 1.49 -3 -7 0 -0.84 1.45 3 7 0 1.20 2.06 3 7 0 -1.67 1.36 -4 -7 0 80.71 5.57 -4 -7 0 77.08 4.86 4 7 0 80.56 5.12 4 7 0 89.31 6.61 -5 -7 0 132.35 6.50 -5 -7 0 120.68 7.53 5 7 0 129.71 7.02 5 7 0 128.82 8.62 -6 -7 0 36.20 5.19 6 7 0 37.36 5.74 6 7 0 50.24 5.12 -7 -7 0 98.87 7.51 7 7 0 84.13 8.95 -8 -7 0 81.60 8.29 8 7 0 83.70 9.38 -9 -7 0 6.52 3.59 9 7 0 1.14 3.31 -10 -7 0 -1.83 3.07 10 7 0 2.56 4.32 -11 8 0 11.14 4.72 10 -8 0 28.92 5.94 -10 8 0 23.08 5.29 9 -8 0 36.13 6.48 -9 8 0 44.99 6.35 8 -8 0 63.34 7.36 -8 8 0 76.31 8.10 -8 8 0 60.54 6.72 7 -8 0 12.99 3.73 -7 8 0 13.85 3.54 -7 8 0 17.52 4.27 6 -8 0 0.06 2.44 -6 8 0 1.54 2.49 -6 8 0 5.50 2.41 5 -8 0 1.12 2.44 -5 8 0 -2.04 1.84 -5 8 0 1.30 1.96 4 -8 0 77.35 6.23 -4 8 0 82.72 6.24 -4 8 0 87.98 5.63 3 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5.14 2.65 5 -9 0 52.22 6.39 -5 9 0 55.10 6.43 -5 9 0 46.46 5.27 4 -9 0 33.23 5.03 -4 9 0 19.81 4.22 -4 9 0 25.96 3.88 3 -9 0 61.15 6.33 -3 9 0 40.37 5.03 -3 9 0 39.42 4.49 2 -9 0 113.44 7.43 2 -9 0 98.58 4.17 -2 9 0 95.27 6.56 -2 9 0 89.71 5.88 1 -9 0 80.82 4.14 1 -9 0 86.58 6.50 -1 9 0 84.37 5.67 -1 9 0 91.66 6.10 0 -9 0 37.12 4.84 0 -9 0 37.91 3.45 0 9 0 39.66 4.53 0 9 0 42.07 4.63 -1 -9 0 8.93 2.85 -1 -9 0 8.29 2.25 1 9 0 11.49 2.69 1 9 0 8.05 2.79 -2 -9 0 -1.61 1.79 -2 -9 0 -0.30 1.62 2 9 0 4.49 2.41 2 9 0 2.14 1.95 -3 -9 0 1.65 1.98 -3 -9 0 2.33 2.22 3 9 0 0.97 2.43 3 9 0 3.76 2.15 -4 -9 0 20.38 3.47 -4 -9 0 23.66 3.94 4 9 0 13.93 3.74 4 9 0 13.47 3.12 -5 -9 0 31.88 4.77 5 9 0 30.21 5.12 5 9 0 34.06 4.38 -6 -9 0 11.34 3.63 6 9 0 28.70 5.45 -7 -9 0 19.21 4.54 7 9 0 18.22 4.88 -8 -9 0 24.92 5.31 8 9 0 28.31 5.98 -9 -9 0 5.86 4.00 9 9 0 -0.79 3.42 10 -10 0 16.33 5.44 -10 10 0 20.38 5.37 -9 10 0 51.92 6.97 8 -10 0 26.78 5.59 -8 10 0 13.26 4.42 -8 10 0 23.43 4.76 7 -10 0 2.09 3.21 -7 10 0 0.10 2.44 -7 10 0 8.93 3.59 6 -10 0 13.68 4.12 -6 10 0 5.40 2.66 -6 10 0 12.94 4.07 5 -10 0 12.75 3.97 -5 10 0 14.71 3.81 -5 10 0 14.34 3.46 4 -10 0 56.71 6.89 -4 10 0 57.96 5.83 -4 10 0 71.01 7.15 3 -10 0 53.93 6.46 -3 10 0 65.14 6.56 -3 10 0 68.56 5.23 2 -10 0 26.57 4.68 -2 10 0 29.76 4.43 -2 10 0 32.27 4.21 1 -10 0 66.29 6.68 1 -10 0 77.08 4.11 -1 10 0 63.87 5.99 -1 10 0 73.45 5.81 0 -10 0 135.80 8.49 0 -10 0 146.17 6.55 0 10 0 137.26 7.97 0 10 0 142.07 7.97 -1 -10 0 8.96 2.33 -1 -10 0 4.69 2.70 1 10 0 12.43 3.38 1 10 0 5.27 2.62 -2 -10 0 -0.87 2.02 -2 -10 0 0.55 1.87 2 10 0 -1.24 1.81 2 10 0 3.48 2.75 -3 -10 0 0.01 2.02 -3 -10 0 1.65 2.08 3 10 0 -1.00 2.00 3 10 0 -0.22 2.16 -4 -10 0 15.32 3.27 -4 -10 0 12.64 3.38 4 10 0 10.33 3.72 4 10 0 12.30 3.18 -5 -10 0 44.72 5.69 5 10 0 38.99 6.13 -6 -10 0 63.83 7.05 6 10 0 48.59 7.03 -7 -10 0 27.34 5.34 7 10 0 28.62 5.68 -8 -10 0 12.63 4.36 8 10 0 11.14 4.66 9 10 0 4.79 4.12 9 -11 0 26.53 6.10 8 -11 0 12.17 4.75 -8 11 0 21.59 5.47 -8 11 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7.51 -4 13 0 57.79 6.33 3 -13 0 63.89 8.01 -3 13 0 62.29 7.46 -3 13 0 73.44 7.02 2 -13 0 47.73 6.60 -2 13 0 40.23 6.06 -2 13 0 45.02 5.49 1 -13 0 26.00 5.02 -1 13 0 28.34 4.68 -1 13 0 29.04 5.28 0 -13 0 34.50 5.70 0 13 0 43.12 5.80 0 13 0 42.52 5.79 -1 -13 0 2.10 2.79 1 13 0 -0.89 2.59 1 13 0 -0.64 2.62 -2 -13 0 17.23 3.73 -2 -13 0 17.10 4.25 2 13 0 13.13 3.95 2 13 0 9.82 3.61 -3 -13 0 4.78 3.12 -3 -13 0 10.77 3.25 3 13 0 9.96 3.75 -4 -13 0 37.71 5.54 4 13 0 28.26 5.44 -5 -13 0 49.51 6.44 5 13 0 39.39 6.55 -6 -13 0 31.18 5.75 6 13 0 19.59 5.31 -7 -13 0 28.86 5.77 7 13 0 16.89 5.34 8 -14 0 6.05 4.93 7 -14 0 6.48 4.61 -7 14 0 9.81 4.58 6 -14 0 8.15 4.62 -6 14 0 15.19 5.22 5 -14 0 15.09 5.40 -5 14 0 21.44 5.50 4 -14 0 5.35 3.92 -4 14 0 3.74 3.58 3 -14 0 44.94 7.00 -3 14 0 49.03 6.90 2 -14 0 61.64 7.97 -2 14 0 60.66 7.31 -2 14 0 50.10 6.07 1 -14 0 11.59 4.00 -1 14 0 23.71 4.87 -1 14 0 17.52 4.01 0 -14 0 -0.08 2.77 0 14 0 5.22 3.42 0 14 0 10.31 3.56 -1 -14 0 3.77 3.36 1 14 0 2.73 3.03 1 14 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-5.16 2.77 1 -1 19 -1.90 3.47 -2 1 -19 13.48 4.45 2 -1 19 17.85 5.48 4 0 -19 30.13 5.90 -4 0 19 45.32 7.17 3 0 -19 4.15 3.54 -3 0 19 4.86 3.67 2 0 -19 -0.58 2.96 -2 0 19 -0.53 3.17 1 0 -19 3.07 3.16 0 0 -19 1.53 3.09 0 0 19 3.55 3.72 -1 0 -19 23.44 5.39 1 0 19 12.51 4.86 2 0 19 20.83 5.77 -4 1 19 11.28 4.81 3 -1 -19 4.17 3.20 -3 1 19 2.09 3.68 2 -1 -19 1.75 3.22 -2 1 19 -0.54 3.19 1 -1 -19 0.31 2.62 0 -1 -19 3.34 3.12 0 1 19 -2.44 3.44 1 1 19 -0.34 3.78 -4 2 19 11.60 4.78 -3 2 19 6.91 4.35 -2 2 19 0.14 3.39 -1 2 19 4.05 4.08 0 2 19 17.76 5.51 1 2 19 15.12 5.19 -3 3 19 -1.43 3.31 -2 3 19 3.18 3.65 -1 3 19 6.37 4.34 0 3 19 19.31 5.79 -3 4 19 10.49 4.80 -2 4 19 -1.07 3.74 -1 4 19 19.09 5.68 0 -8 20 2.33 3.80 3 7 -20 -2.28 3.12 -1 -7 20 1.50 3.65 3 6 -20 1.54 3.57 2 6 -20 4.11 3.66 -2 -6 20 4.59 4.24 1 6 -20 6.27 3.89 -1 -6 20 18.53 5.10 3 5 -20 7.03 4.02 2 5 -20 2.47 3.36 -2 -5 20 9.72 4.64 1 5 -20 18.82 4.76 -1 -5 20 37.93 6.74 0 5 -20 18.33 4.86 3 4 -20 1.29 3.33 -3 -4 20 1.03 3.81 2 4 -20 17.01 4.71 -2 -4 20 12.77 4.83 1 4 -20 5.74 3.50 -1 -4 20 8.04 4.10 0 4 -20 22.65 5.29 -1 4 -20 6.92 4.00 3 3 -20 1.44 3.03 -3 -3 20 -1.22 3.53 2 3 -20 21.65 5.07 -2 -3 20 22.45 5.36 1 3 -20 15.68 4.64 -1 -3 20 19.23 5.32 0 3 -20 7.31 3.65 -1 3 -20 30.71 5.89 -3 -2 20 2.96 3.83 2 2 -20 21.77 5.14 -2 -2 20 11.59 4.70 1 2 -20 13.06 4.22 0 2 -20 21.11 5.14 -3 -1 20 21.01 5.54 -2 -1 20 39.98 6.70 -3 0 20 24.20 5.94 -2 0 20 26.55 5.76 1 0 20 15.37 5.29 -2 1 20 16.56 5.22 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 42343 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969308' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_9 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 Er N3 O7' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 885.20 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 '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 8.7004(18) _cell_length_b 13.066(3) _cell_length_c 14.779(3) _cell_angle_alpha 100.219(3) _cell_angle_beta 97.697(3) _cell_angle_gamma 92.384(3) _cell_volume 1634.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 21264 _cell_measurement_theta_min 4.735 _cell_measurement_theta_max 41.357 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.798 _exptl_crystal_F_000 874 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_absorpt_coefficient_mu 2.869 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6393 _exptl_absorpt_correction_T_max 0.7455 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21263 _diffrn_reflns_av_unetI/netI 0.1056 _diffrn_reflns_av_R_equivalents 0.0865 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.415 _diffrn_reflns_theta_max 27.479 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 7461 _reflns_number_gt 5583 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0509P)^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 7461 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1180 _refine_ls_wR_factor_gt 0.1049 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Er1 Er 0.56182(3) 0.51291(2) 0.70164(2) 0.01488(9) Uani 1 1 d . . . . . O3 O 0.5598(5) 0.3779(3) 0.5614(3) 0.0185(10) Uani 1 1 d . . . . . O1 O 0.7087(5) 0.6230(3) 0.8416(3) 0.0199(10) Uani 1 1 d . . . . . O2 O 0.5349(5) 0.6966(3) 0.7552(3) 0.0190(10) Uani 1 1 d . . . . . O4 O 0.4048(5) 0.3501(3) 0.6608(3) 0.0182(10) Uani 1 1 d . . . . . C23 C 0.4589(7) 0.3208(5) 0.5872(4) 0.0159(13) Uani 1 1 d . . . . . N1 N 0.7899(6) 0.4060(4) 0.7255(4) 0.0164(11) Uani 1 1 d . . . . . OW1 O 0.3710(5) 0.5586(3) 0.5924(3) 0.0174(10) Uani 1 1 d . . . . . C16 C 0.6389(8) 0.7025(5) 0.8239(4) 0.0162(13) Uani 1 1 d . . . . . C24 C 0.4065(8) 0.2165(5) 0.5283(4) 0.0187(14) Uani 1 1 d . . . . . N3 N 0.3397(6) 0.5382(4) 0.7952(3) 0.0155(11) Uani 1 1 d . . . . . O5 O 0.7275(5) 0.5956(3) 0.6293(3) 0.0200(10) Uani 1 1 d . . . . . C17 C 0.6824(7) 0.8058(5) 0.8853(4) 0.0176(14) Uani 1 1 d . . . . . C13 C 0.0906(8) 0.5672(5) 0.8943(5) 0.0238(15) Uani 1 1 d . . . . . H13 H 0.0071 0.5763 0.9275 0.029 Uiso 1 1 calc R U . . . N2 N 0.5686(6) 0.4145(4) 0.8361(3) 0.0143(11) Uani 1 1 d . . . . . C14 C 0.1005(8) 0.6172(5) 0.8205(5) 0.0217(15) Uani 1 1 d . . . . . H14 H 0.0237 0.6598 0.8021 0.026 Uiso 1 1 calc R U . . . C20 C 0.7514(8) 0.9993(5) 0.9973(5) 0.0227(15) Uani 1 1 d . . . . . C22 C 0.5953(7) 0.8901(5) 0.8696(4) 0.0165(13) Uani 1 1 d . . . . . H22 H 0.5124 0.8807 0.8215 0.020 Uiso 1 1 calc R U . . . C32 C 0.8719(7) 0.7979(5) 0.6901(4) 0.0181(14) Uani 1 1 d . . . . . H32 H 0.7796 0.7829 0.7118 0.022 Uiso 1 1 calc R U . . . C5 C 0.8090(7) 0.3496(5) 0.7935(4) 0.0155(13) Uani 1 1 d . . . . . C31 C 0.9210(7) 0.7264(5) 0.6199(4) 0.0154(13) Uani 1 1 d . . . . . C21 C 0.6313(8) 0.9873(5) 0.9250(5) 0.0234(15) Uani 1 1 d . . . . . H21 H 0.5750 1.0438 0.9134 0.028 Uiso 1 1 calc R U . . . C10 C 0.4487(7) 0.4162(5) 0.8860(4) 0.0158(13) Uani 1 1 d . . . . . C15 C 0.2290(7) 0.6019(5) 0.7743(5) 0.0204(14) Uani 1 1 d . . . . . H15 H 0.2386 0.6378 0.7262 0.024 Uiso 1 1 calc R U . . . C1 C 0.9002(8) 0.4037(5) 0.6692(5) 0.0194(14) Uani 1 1 d . . . . . H1 H 0.8849 0.4393 0.6199 0.023 Uiso 1 1 calc R U . . . C18 C 0.8061(8) 0.8201(5) 0.9575(4) 0.0208(14) Uani 1 1 d . . . . . H18 H 0.8654 0.7647 0.9677 0.025 Uiso 1 1 calc R U . . . C6 C 0.6802(7) 0.3472(5) 0.8497(4) 0.0155(13) Uani 1 1 d . . . . . C29 C 0.2910(8) 0.1536(5) 0.5535(5) 0.0226(15) Uani 1 1 d . . . . . H29 H 0.2460 0.1773 0.6064 0.027 Uiso 1 1 calc R U . . . C12 C 0.2058(7) 0.5036(5) 0.9187(5) 0.0196(14) Uani 1 1 d . . . . . H12 H 0.2024 0.4712 0.9697 0.024 Uiso 1 1 calc R U . . . C19 C 0.8405(8) 0.9164(5) 1.0136(5) 0.0245(15) Uani 1 1 d . . . . . H19 H 0.9227 0.9262 1.0622 0.029 Uiso 1 1 calc R U . . . C8 C 0.5510(8) 0.2817(6) 0.9613(5) 0.0270(16) Uani 1 1 d . . . . . H8 H 0.5454 0.2377 1.0040 0.032 Uiso 1 1 calc R U . . . C30 C 0.8231(7) 0.6262(5) 0.5801(5) 0.0188(14) Uani 1 1 d . . . . . C4 C 0.9411(7) 0.2948(5) 0.8083(5) 0.0204(14) Uani 1 1 d . . . . . H4 H 0.9519 0.2561 0.8556 0.024 Uiso 1 1 calc R U . . . C33 C 0.9572(8) 0.8906(5) 0.7280(5) 0.0231(15) Uani 1 1 d . . . . . H33 H 0.9230 0.9382 0.7744 0.028 Uiso 1 1 calc R U . . . C9 C 0.4380(8) 0.3506(5) 0.9490(5) 0.0229(15) Uani 1 1 d . . . . . H9 H 0.3550 0.3530 0.9828 0.027 Uiso 1 1 calc R U . . . C3 C 1.0561(7) 0.2978(5) 0.7528(5) 0.0206(14) Uani 1 1 d . . . . . H3 H 1.1467 0.2641 0.7642 0.025 Uiso 1 1 calc R U . . . Cl1 Cl 0.7968(2) 1.12028(13) 1.07055(12) 0.0280(4) Uani 1 1 d . . . . . Cl3 Cl 1.2093(2) 1.02579(14) 0.74337(13) 0.0346(4) Uani 1 1 d . . . . . O6 O 0.8459(5) 0.5803(4) 0.5020(3) 0.0230(11) Uani 1 1 d . . . . . C35 C 1.1462(8) 0.8417(5) 0.6255(5) 0.0265(16) Uani 1 1 d . . . . . H35 H 1.2387 0.8569 0.6041 0.032 Uiso 1 1 calc R U . . . C25 C 0.4711(8) 0.1789(5) 0.4484(5) 0.0223(15) Uani 1 1 d . . . . . H25 H 0.5458 0.2202 0.4296 0.027 Uiso 1 1 calc R U . . . C26 C 0.4255(8) 0.0819(5) 0.3975(5) 0.0234(15) Uani 1 1 d . . . . . H26 H 0.4714 0.0568 0.3454 0.028 Uiso 1 1 calc R U . . . C28 C 0.2433(8) 0.0563(5) 0.5002(5) 0.0272(16) Uani 1 1 d . . . . . H28 H 0.1655 0.0151 0.5165 0.033 Uiso 1 1 calc R U . . . C36 C 1.0571(7) 0.7489(5) 0.5879(5) 0.0204(14) Uani 1 1 d . . . . . H36 H 1.0903 0.7018 0.5407 0.025 Uiso 1 1 calc R U . . . C11 C 0.3263(7) 0.4884(5) 0.8664(4) 0.0178(14) Uani 1 1 d . . . . . C7 C 0.6715(8) 0.2782(5) 0.9105(4) 0.0214(15) Uani 1 1 d . . . . . H7 H 0.7465 0.2302 0.9166 0.026 Uiso 1 1 calc R U . . . C2 C 1.0351(8) 0.3513(5) 0.6805(5) 0.0215(15) Uani 1 1 d . . . . . H2 H 1.1088 0.3524 0.6404 0.026 Uiso 1 1 calc R U . . . C34 C 1.0940(8) 0.9106(5) 0.6954(5) 0.0217(15) Uani 1 1 d . . . . . C27 C 0.3120(9) 0.0214(5) 0.4233(5) 0.0277(17) Uani 1 1 d . . . . . Cl2 Cl 0.2500(3) -0.10071(15) 0.35670(15) 0.0435(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Er1 0.01157(15) 0.01615(16) 0.01727(15) 0.00332(11) 0.00269(10) 0.00193(10) O3 0.020(2) 0.019(2) 0.018(2) 0.0047(19) 0.0055(19) 0.0032(19) O1 0.018(2) 0.019(2) 0.024(2) 0.004(2) 0.0053(19) -0.0002(19) O2 0.015(2) 0.022(2) 0.018(2) 0.0013(19) 0.0021(18) 0.0010(19) O4 0.017(2) 0.018(2) 0.019(2) 0.0027(19) 0.0039(18) 0.0027(19) C23 0.012(3) 0.012(3) 0.024(4) 0.008(3) -0.002(3) 0.003(3) N1 0.015(3) 0.014(3) 0.019(3) 0.001(2) 0.002(2) 0.001(2) OW1 0.014(2) 0.021(2) 0.017(2) 0.0050(19) -0.0010(18) 0.0023(19) C16 0.021(3) 0.014(3) 0.016(3) 0.004(3) 0.011(3) 0.002(3) C24 0.017(3) 0.016(3) 0.021(3) 0.003(3) -0.003(3) 0.002(3) N3 0.015(3) 0.016(3) 0.015(3) 0.001(2) 0.001(2) 0.003(2) O5 0.021(2) 0.020(2) 0.024(2) 0.011(2) 0.0093(19) 0.001(2) C17 0.013(3) 0.022(4) 0.019(3) 0.007(3) 0.006(3) 0.000(3) C13 0.018(4) 0.025(4) 0.031(4) 0.003(3) 0.013(3) 0.002(3) N2 0.006(2) 0.021(3) 0.016(3) 0.003(2) 0.003(2) 0.004(2) C14 0.022(4) 0.018(3) 0.023(4) 0.000(3) 0.001(3) 0.004(3) C20 0.030(4) 0.019(4) 0.020(3) 0.005(3) 0.006(3) -0.002(3) C22 0.014(3) 0.020(3) 0.016(3) 0.004(3) 0.003(2) 0.000(3) C32 0.014(3) 0.018(3) 0.025(4) 0.009(3) 0.006(3) 0.001(3) C5 0.016(3) 0.014(3) 0.015(3) -0.001(3) 0.001(2) -0.001(3) C31 0.011(3) 0.019(3) 0.016(3) 0.006(3) 0.000(2) 0.001(3) C21 0.022(4) 0.023(4) 0.027(4) 0.008(3) 0.002(3) 0.010(3) C10 0.013(3) 0.014(3) 0.020(3) 0.004(3) 0.001(3) -0.003(3) C15 0.018(3) 0.019(4) 0.024(4) 0.003(3) 0.002(3) 0.006(3) C1 0.026(4) 0.012(3) 0.021(3) 0.004(3) 0.008(3) -0.001(3) C18 0.019(3) 0.020(3) 0.024(4) 0.002(3) 0.006(3) 0.002(3) C6 0.014(3) 0.014(3) 0.017(3) 0.001(3) -0.001(2) 0.001(3) C29 0.027(4) 0.019(4) 0.022(4) 0.002(3) 0.004(3) 0.004(3) C12 0.017(3) 0.021(4) 0.022(3) 0.004(3) 0.009(3) 0.007(3) C19 0.026(4) 0.024(4) 0.022(4) 0.006(3) -0.004(3) 0.006(3) C8 0.022(4) 0.032(4) 0.033(4) 0.016(3) 0.011(3) 0.005(3) C30 0.010(3) 0.020(3) 0.031(4) 0.014(3) 0.006(3) 0.003(3) C4 0.013(3) 0.026(4) 0.023(4) 0.007(3) 0.000(3) 0.005(3) C33 0.030(4) 0.019(4) 0.022(4) 0.002(3) 0.010(3) 0.007(3) C9 0.024(4) 0.025(4) 0.023(4) 0.009(3) 0.012(3) 0.005(3) C3 0.011(3) 0.020(4) 0.030(4) 0.004(3) 0.003(3) 0.004(3) Cl1 0.0306(10) 0.0205(9) 0.0295(9) -0.0002(7) -0.0012(7) 0.0027(7) Cl3 0.0357(11) 0.0272(10) 0.0387(11) 0.0026(8) 0.0049(8) -0.0068(8) O6 0.021(3) 0.029(3) 0.020(2) 0.005(2) 0.006(2) -0.001(2) C35 0.017(4) 0.025(4) 0.041(4) 0.011(3) 0.011(3) -0.001(3) C25 0.019(4) 0.020(4) 0.027(4) 0.003(3) 0.000(3) 0.003(3) C26 0.026(4) 0.023(4) 0.021(4) 0.002(3) 0.003(3) 0.007(3) C28 0.028(4) 0.021(4) 0.031(4) 0.007(3) -0.001(3) -0.008(3) C36 0.017(3) 0.022(4) 0.024(4) 0.006(3) 0.007(3) 0.004(3) C11 0.012(3) 0.013(3) 0.023(3) -0.008(3) 0.000(3) 0.002(3) C7 0.019(4) 0.022(4) 0.024(4) 0.008(3) 0.003(3) 0.008(3) C2 0.017(3) 0.021(4) 0.028(4) 0.002(3) 0.011(3) 0.006(3) C34 0.018(3) 0.020(4) 0.027(4) 0.007(3) -0.002(3) -0.002(3) C27 0.032(4) 0.020(4) 0.027(4) 0.002(3) -0.007(3) 0.006(3) Cl2 0.0508(13) 0.0224(10) 0.0480(13) -0.0047(9) -0.0115(10) 0.0014(9) _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 Er1 O5 2.255(4) . ? Er1 OW1 2.329(4) . ? Er1 O4 2.416(4) . ? Er1 O2 2.421(4) . ? Er1 O1 2.463(4) . ? Er1 O3 2.470(4) . ? Er1 N1 2.496(5) . ? Er1 N3 2.523(5) . ? Er1 N2 2.547(5) . ? Er1 C16 2.793(6) . ? Er1 C23 2.805(6) . ? O3 C23 1.268(7) . ? O1 C16 1.274(7) . ? O2 C16 1.255(7) . ? O4 C23 1.247(7) . ? C23 C24 1.497(9) . ? N1 C5 1.346(8) . ? N1 C1 1.350(8) . ? C16 C17 1.489(9) . ? C24 C25 1.394(9) . ? C24 C29 1.403(9) . ? N3 C15 1.339(8) . ? N3 C11 1.348(8) . ? O5 C30 1.271(7) . ? C17 C18 1.391(9) . ? C17 C22 1.397(9) . ? C13 C14 1.378(9) . ? C13 C12 1.380(9) . ? C13 H13 0.9300 . ? N2 C10 1.355(8) . ? N2 C6 1.356(8) . ? C14 C15 1.389(9) . ? C14 H14 0.9300 . ? C20 C21 1.374(9) . ? C20 C19 1.394(9) . ? C20 Cl1 1.747(7) . ? C22 C21 1.383(9) . ? C22 H22 0.9300 . ? C32 C33 1.380(9) . ? C32 C31 1.392(9) . ? C32 H32 0.9300 . ? C5 C4 1.393(9) . ? C5 C6 1.484(9) . ? C31 C36 1.372(9) . ? C31 C30 1.511(9) . ? C21 H21 0.9300 . ? C10 C9 1.381(9) . ? C10 C11 1.484(9) . ? C15 H15 0.9300 . ? C1 C2 1.389(9) . ? C1 H1 0.9300 . ? C18 C19 1.376(9) . ? C18 H18 0.9300 . ? C6 C7 1.388(9) . ? C29 C28 1.386(9) . ? C29 H29 0.9300 . ? C12 C11 1.384(9) . ? C12 H12 0.9300 . ? C19 H19 0.9300 . ? C8 C7 1.366(9) . ? C8 C9 1.377(9) . ? C8 H8 0.9300 . ? C30 O6 1.248(8) . ? C4 C3 1.379(9) . ? C4 H4 0.9300 . ? C33 C34 1.374(9) . ? C33 H33 0.9300 . ? C9 H9 0.9300 . ? C3 C2 1.374(9) . ? C3 H3 0.9300 . ? Cl3 C34 1.755(7) . ? C35 C34 1.384(10) . ? C35 C36 1.396(9) . ? C35 H35 0.9300 . ? C25 C26 1.368(9) . ? C25 H25 0.9300 . ? C26 C27 1.373(10) . ? C26 H26 0.9300 . ? C28 C27 1.371(10) . ? C28 H28 0.9300 . ? C36 H36 0.9300 . ? C7 H7 0.9300 . ? C2 H2 0.9300 . ? C27 Cl2 1.742(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Er1 OW1 84.39(15) . . ? O5 Er1 O4 134.24(15) . . ? OW1 Er1 O4 80.95(15) . . ? O5 Er1 O2 75.22(15) . . ? OW1 Er1 O2 75.16(14) . . ? O4 Er1 O2 139.75(14) . . ? O5 Er1 O1 82.74(15) . . ? OW1 Er1 O1 128.92(15) . . ? O4 Er1 O1 138.33(14) . . ? O2 Er1 O1 53.77(14) . . ? O5 Er1 O3 81.22(15) . . ? OW1 Er1 O3 75.41(15) . . ? O4 Er1 O3 53.18(14) . . ? O2 Er1 O3 143.70(14) . . ? O1 Er1 O3 149.08(15) . . ? O5 Er1 N1 81.28(16) . . ? OW1 Er1 N1 145.19(16) . . ? O4 Er1 N1 86.66(16) . . ? O2 Er1 N1 130.21(16) . . ? O1 Er1 N1 80.42(16) . . ? O3 Er1 N1 71.15(15) . . ? O5 Er1 N3 143.74(16) . . ? OW1 Er1 N3 79.37(16) . . ? O4 Er1 N3 74.75(15) . . ? O2 Er1 N3 69.38(15) . . ? O1 Er1 N3 82.70(15) . . ? O3 Er1 N3 124.58(15) . . ? N1 Er1 N3 128.32(17) . . ? O5 Er1 N2 139.33(16) . . ? OW1 Er1 N2 136.28(15) . . ? O4 Er1 N2 67.37(15) . . ? O2 Er1 N2 110.45(15) . . ? O1 Er1 N2 71.33(15) . . ? O3 Er1 N2 105.46(15) . . ? N1 Er1 N2 64.23(16) . . ? N3 Er1 N2 64.10(16) . . ? O5 Er1 C16 77.12(17) . . ? OW1 Er1 C16 101.81(17) . . ? O4 Er1 C16 148.35(16) . . ? O2 Er1 C16 26.65(16) . . ? O1 Er1 C16 27.12(16) . . ? O3 Er1 C16 158.33(16) . . ? N1 Er1 C16 105.62(18) . . ? N3 Er1 C16 74.84(17) . . ? N2 Er1 C16 91.45(17) . . ? O5 Er1 C23 108.04(17) . . ? OW1 Er1 C23 77.10(16) . . ? O4 Er1 C23 26.32(16) . . ? O2 Er1 C23 151.60(16) . . ? O1 Er1 C23 153.45(16) . . ? O3 Er1 C23 26.87(16) . . ? N1 Er1 C23 77.49(17) . . ? N3 Er1 C23 99.64(17) . . ? N2 Er1 C23 85.81(17) . . ? C16 Er1 C23 174.48(18) . . ? C23 O3 Er1 91.5(4) . . ? C16 O1 Er1 91.1(4) . . ? C16 O2 Er1 93.4(4) . . ? C23 O4 Er1 94.5(4) . . ? O4 C23 O3 120.8(6) . . ? O4 C23 C24 120.3(6) . . ? O3 C23 C24 118.9(6) . . ? O4 C23 Er1 59.2(3) . . ? O3 C23 Er1 61.7(3) . . ? C24 C23 Er1 178.2(4) . . ? C5 N1 C1 117.5(5) . . ? C5 N1 Er1 122.5(4) . . ? C1 N1 Er1 120.0(4) . . ? O2 C16 O1 121.7(6) . . ? O2 C16 C17 118.8(6) . . ? O1 C16 C17 119.5(6) . . ? O2 C16 Er1 59.9(3) . . ? O1 C16 Er1 61.8(3) . . ? C17 C16 Er1 177.2(4) . . ? C25 C24 C29 118.4(6) . . ? C25 C24 C23 121.7(6) . . ? C29 C24 C23 120.0(6) . . ? C15 N3 C11 117.7(5) . . ? C15 N3 Er1 120.3(4) . . ? C11 N3 Er1 122.1(4) . . ? C30 O5 Er1 169.8(4) . . ? C18 C17 C22 119.5(6) . . ? C18 C17 C16 121.9(6) . . ? C22 C17 C16 118.6(6) . . ? C14 C13 C12 119.5(6) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C10 N2 C6 118.5(5) . . ? C10 N2 Er1 120.5(4) . . ? C6 N2 Er1 120.2(4) . . ? C13 C14 C15 117.7(6) . . ? C13 C14 H14 121.1 . . ? C15 C14 H14 121.1 . . ? C21 C20 C19 121.3(6) . . ? C21 C20 Cl1 120.2(5) . . ? C19 C20 Cl1 118.5(5) . . ? C21 C22 C17 120.6(6) . . ? C21 C22 H22 119.7 . . ? C17 C22 H22 119.7 . . ? C33 C32 C31 121.4(6) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? N1 C5 C4 121.4(6) . . ? N1 C5 C6 116.3(5) . . ? C4 C5 C6 122.3(6) . . ? C36 C31 C32 119.1(6) . . ? C36 C31 C30 121.4(6) . . ? C32 C31 C30 119.5(5) . . ? C20 C21 C22 119.0(6) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N2 C10 C9 121.4(6) . . ? N2 C10 C11 116.7(5) . . ? C9 C10 C11 121.9(6) . . ? N3 C15 C14 123.7(6) . . ? N3 C15 H15 118.1 . . ? C14 C15 H15 118.1 . . ? N1 C1 C2 123.9(6) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? C19 C18 C17 120.0(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? N2 C6 C7 121.8(6) . . ? N2 C6 C5 115.9(5) . . ? C7 C6 C5 122.2(6) . . ? C28 C29 C24 120.4(6) . . ? C28 C29 H29 119.8 . . ? C24 C29 H29 119.8 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C18 C19 C20 119.6(6) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C7 C8 C9 119.7(6) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? O6 C30 O5 126.0(6) . . ? O6 C30 C31 116.4(5) . . ? O5 C30 C31 117.5(6) . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C34 C33 C32 118.3(6) . . ? C34 C33 H33 120.9 . . ? C32 C33 H33 120.9 . . ? C8 C9 C10 119.6(6) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C2 C3 C4 119.3(6) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.4 . . ? C34 C35 C36 118.5(6) . . ? C34 C35 H35 120.7 . . ? C36 C35 H35 120.7 . . ? C26 C25 C24 120.7(7) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 120.2(7) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C27 C28 C29 119.3(7) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C31 C36 C35 120.7(6) . . ? C31 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? N3 C11 C12 122.0(6) . . ? N3 C11 C10 116.2(5) . . ? C12 C11 C10 121.7(6) . . ? C8 C7 C6 119.0(6) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C3 C2 C1 117.7(6) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C33 C34 C35 122.0(6) . . ? C33 C34 Cl3 120.1(5) . . ? C35 C34 Cl3 117.9(5) . . ? C28 C27 C26 121.0(6) . . ? C28 C27 Cl2 118.8(6) . . ? C26 C27 Cl2 120.2(6) . . ? _refine_diff_density_max 1.551 _refine_diff_density_min -1.898 _refine_diff_density_rms 0.203 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.7004 13.0663 14.7790 100.219 97.697 92.384 ZERR 2.00 0.0018 0.0027 0.0030 0.003 0.003 0.003 LATT 1 SFAC C H N O CL ER UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 12 WGHT 0.050900 FVAR 0.12152 ER1 6 0.561818 0.512911 0.701645 11.00000 0.01157 0.01615 = 0.01727 0.00332 0.00269 0.00193 O3 4 0.559799 0.377861 0.561419 11.00000 0.01957 0.01932 = 0.01792 0.00474 0.00546 0.00318 O1 4 0.708661 0.623043 0.841596 11.00000 0.01782 0.01865 = 0.02391 0.00413 0.00529 -0.00019 O2 4 0.534872 0.696555 0.755201 11.00000 0.01544 0.02246 = 0.01813 0.00129 0.00206 0.00096 O4 4 0.404814 0.350123 0.660781 11.00000 0.01691 0.01846 = 0.01936 0.00266 0.00386 0.00270 C23 1 0.458863 0.320784 0.587167 11.00000 0.01154 0.01225 = 0.02441 0.00805 -0.00207 0.00255 N1 3 0.789923 0.406040 0.725500 11.00000 0.01492 0.01442 = 0.01908 0.00122 0.00180 0.00128 OW1 4 0.371009 0.558607 0.592434 11.00000 0.01389 0.02082 = 0.01737 0.00503 -0.00095 0.00229 C16 1 0.638855 0.702537 0.823924 11.00000 0.02114 0.01421 = 0.01606 0.00397 0.01084 0.00199 C24 1 0.406534 0.216548 0.528266 11.00000 0.01705 0.01609 = 0.02137 0.00327 -0.00252 0.00151 N3 3 0.339660 0.538239 0.795201 11.00000 0.01460 0.01612 = 0.01471 0.00097 0.00071 0.00281 O5 4 0.727533 0.595640 0.629297 11.00000 0.02072 0.01970 = 0.02380 0.01061 0.00927 0.00130 C17 1 0.682386 0.805810 0.885271 11.00000 0.01345 0.02184 = 0.01950 0.00697 0.00552 0.00029 C13 1 0.090647 0.567241 0.894319 11.00000 0.01831 0.02457 = 0.03066 0.00296 0.01342 0.00228 AFIX 43 H13 2 0.007066 0.576341 0.927468 11.00000 -1.20000 AFIX 0 N2 3 0.568581 0.414499 0.836096 11.00000 0.00603 0.02117 = 0.01616 0.00292 0.00309 0.00415 C14 1 0.100501 0.617233 0.820466 11.00000 0.02168 0.01828 = 0.02323 -0.00032 0.00123 0.00422 AFIX 43 H14 2 0.023737 0.659816 0.802143 11.00000 -1.20000 AFIX 0 C20 1 0.751369 0.999305 0.997338 11.00000 0.03017 0.01902 = 0.01966 0.00460 0.00562 -0.00207 C22 1 0.595315 0.890068 0.869605 11.00000 0.01416 0.01975 = 0.01617 0.00432 0.00291 0.00008 AFIX 43 H22 2 0.512441 0.880651 0.821491 11.00000 -1.20000 AFIX 0 C32 1 0.871911 0.797904 0.690055 11.00000 0.01351 0.01784 = 0.02535 0.00857 0.00559 0.00141 AFIX 43 H32 2 0.779620 0.782924 0.711814 11.00000 -1.20000 AFIX 0 C5 1 0.808988 0.349589 0.793513 11.00000 0.01564 0.01432 = 0.01461 -0.00142 0.00074 -0.00069 C31 1 0.920977 0.726365 0.619940 11.00000 0.01114 0.01932 = 0.01618 0.00600 0.00036 0.00126 C21 1 0.631253 0.987322 0.924990 11.00000 0.02152 0.02343 = 0.02689 0.00755 0.00237 0.00996 AFIX 43 H21 2 0.574980 1.043758 0.913446 11.00000 -1.20000 AFIX 0 C10 1 0.448653 0.416239 0.886033 11.00000 0.01348 0.01389 = 0.01983 0.00445 0.00148 -0.00327 C15 1 0.228977 0.601866 0.774318 11.00000 0.01753 0.01938 = 0.02367 0.00259 0.00164 0.00567 AFIX 43 H15 2 0.238647 0.637813 0.726190 11.00000 -1.20000 AFIX 0 C1 1 0.900184 0.403713 0.669175 11.00000 0.02643 0.01191 = 0.02134 0.00444 0.00803 -0.00051 AFIX 43 H1 2 0.884911 0.439316 0.619854 11.00000 -1.20000 AFIX 0 C18 1 0.806050 0.820141 0.957460 11.00000 0.01938 0.01969 = 0.02377 0.00217 0.00650 0.00208 AFIX 43 H18 2 0.865435 0.764652 0.967736 11.00000 -1.20000 AFIX 0 C6 1 0.680209 0.347199 0.849749 11.00000 0.01388 0.01443 = 0.01655 0.00113 -0.00125 0.00101 C29 1 0.290973 0.153618 0.553537 11.00000 0.02736 0.01851 = 0.02181 0.00226 0.00405 0.00387 AFIX 43 H29 2 0.246041 0.177317 0.606390 11.00000 -1.20000 AFIX 0 C12 1 0.205767 0.503568 0.918711 11.00000 0.01722 0.02118 = 0.02235 0.00366 0.00852 0.00674 AFIX 43 H12 2 0.202393 0.471234 0.969693 11.00000 -1.20000 AFIX 0 C19 1 0.840475 0.916427 1.013647 11.00000 0.02635 0.02408 = 0.02232 0.00636 -0.00384 0.00623 AFIX 43 H19 2 0.922660 0.926166 1.062196 11.00000 -1.20000 AFIX 0 C8 1 0.551023 0.281690 0.961300 11.00000 0.02229 0.03182 = 0.03291 0.01634 0.01065 0.00475 AFIX 43 H8 2 0.545397 0.237745 1.004002 11.00000 -1.20000 AFIX 0 C30 1 0.823120 0.626221 0.580128 11.00000 0.00972 0.01987 = 0.03109 0.01374 0.00603 0.00319 C4 1 0.941112 0.294757 0.808284 11.00000 0.01304 0.02568 = 0.02298 0.00727 -0.00049 0.00521 AFIX 43 H4 2 0.951855 0.256061 0.855585 11.00000 -1.20000 AFIX 0 C33 1 0.957235 0.890557 0.727971 11.00000 0.02980 0.01883 = 0.02193 0.00152 0.01022 0.00667 AFIX 43 H33 2 0.923039 0.938222 0.774356 11.00000 -1.20000 AFIX 0 C9 1 0.437994 0.350602 0.948959 11.00000 0.02433 0.02540 = 0.02299 0.00860 0.01166 0.00471 AFIX 43 H9 2 0.355002 0.352956 0.982761 11.00000 -1.20000 AFIX 0 C3 1 1.056063 0.297821 0.752779 11.00000 0.01148 0.02039 = 0.02971 0.00373 0.00300 0.00388 AFIX 43 H3 2 1.146717 0.264051 0.764180 11.00000 -1.20000 AFIX 0 CL1 5 0.796841 1.120283 1.070553 11.00000 0.03057 0.02053 = 0.02950 -0.00022 -0.00124 0.00272 CL3 5 1.209323 1.025788 0.743367 11.00000 0.03571 0.02717 = 0.03873 0.00261 0.00493 -0.00677 O6 4 0.845862 0.580281 0.501987 11.00000 0.02058 0.02882 = 0.02019 0.00453 0.00633 -0.00145 C35 1 1.146239 0.841688 0.625526 11.00000 0.01700 0.02492 = 0.04111 0.01096 0.01131 -0.00121 AFIX 43 H35 2 1.238716 0.856883 0.604057 11.00000 -1.20000 AFIX 0 C25 1 0.471063 0.178922 0.448419 11.00000 0.01859 0.02014 = 0.02677 0.00259 -0.00018 0.00314 AFIX 43 H25 2 0.545847 0.220225 0.429568 11.00000 -1.20000 AFIX 0 C26 1 0.425476 0.081884 0.397546 11.00000 0.02620 0.02298 = 0.02082 0.00226 0.00336 0.00700 AFIX 43 H26 2 0.471429 0.056798 0.345405 11.00000 -1.20000 AFIX 0 C28 1 0.243287 0.056318 0.500242 11.00000 0.02801 0.02136 = 0.03097 0.00734 -0.00067 -0.00830 AFIX 43 H28 2 0.165480 0.015147 0.516529 11.00000 -1.20000 AFIX 0 C36 1 1.057093 0.748887 0.587934 11.00000 0.01653 0.02234 = 0.02432 0.00575 0.00684 0.00437 AFIX 43 H36 2 1.090272 0.701831 0.540713 11.00000 -1.20000 AFIX 0 C11 1 0.326342 0.488358 0.866437 11.00000 0.01201 0.01349 = 0.02308 -0.00763 -0.00012 0.00162 C7 1 0.671459 0.278158 0.910541 11.00000 0.01923 0.02238 = 0.02438 0.00750 0.00284 0.00825 AFIX 43 H7 2 0.746490 0.230215 0.916613 11.00000 -1.20000 AFIX 0 C2 1 1.035126 0.351319 0.680465 11.00000 0.01690 0.02066 = 0.02845 0.00215 0.01057 0.00610 AFIX 43 H2 2 1.108792 0.352420 0.640430 11.00000 -1.20000 AFIX 0 C34 1 1.093993 0.910592 0.695449 11.00000 0.01846 0.01974 = 0.02653 0.00733 -0.00161 -0.00151 C27 1 0.312018 0.021396 0.423262 11.00000 0.03221 0.02050 = 0.02673 0.00165 -0.00659 0.00561 CL2 5 0.250038 -0.100709 0.356700 11.00000 0.05078 0.02241 = 0.04804 -0.00471 -0.01145 0.00136 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0507 for 5583 Fo > 4sig(Fo) and 0.0785 for all 7461 data REM 451 parameters refined using 0 restraints END WGHT 0.0509 0.0000 REM Highest difference peak 1.551, deepest hole -1.898, 1-sigma level 0.203 Q1 1 0.5269 0.4345 0.6962 11.00000 0.05 1.55 Q2 1 0.5799 0.5058 0.7657 11.00000 0.05 1.31 Q3 1 0.5032 0.4985 0.6025 11.00000 0.05 1.19 Q4 1 0.5620 0.4363 0.7832 11.00000 0.05 1.11 Q5 1 0.6070 0.6039 0.7054 11.00000 0.05 1.09 Q6 1 0.5708 0.5874 0.6234 11.00000 0.05 1.02 Q7 1 0.3507 0.5385 0.8809 11.00000 0.05 0.99 Q8 1 0.6117 0.6519 0.7030 11.00000 0.05 0.98 Q9 1 0.4117 0.5986 0.5567 11.00000 0.05 0.96 Q10 1 0.3126 0.4576 0.8958 11.00000 0.05 0.89 ; _shelx_res_checksum 13207 _shelx_hkl_file ; -1 0 0 446.72 13.37 -1 0 0 389.01 13.15 -1 0 0 385.49 12.78 1 0 0 375.56 12.95 1 0 0 395.41 12.79 -2 0 0 3.24 1.95 -2 0 0 2.59 0.97 -2 0 0 4.93 1.77 2 0 0 2.70 1.45 -3 0 0 127.52 6.76 -3 0 0 126.47 5.04 -3 0 0 122.94 6.65 3 0 0 116.09 6.24 -4 0 0 4.89 2.56 -4 0 0 1.19 1.08 -4 0 0 -0.03 1.90 4 0 0 0.57 1.80 -5 0 0 57.75 6.16 -5 0 0 49.45 5.88 -5 0 0 52.46 3.14 5 0 0 51.89 5.26 -6 0 0 117.32 8.46 -6 0 0 112.78 8.37 6 0 0 113.69 7.71 -7 0 0 41.42 6.53 7 0 0 40.37 5.69 -8 0 0 152.73 11.44 8 0 0 157.20 10.70 8 0 0 172.92 11.82 -9 0 0 68.85 9.59 9 0 0 61.32 8.94 9 0 0 78.83 8.91 -10 0 0 20.10 6.29 10 0 0 12.14 5.47 -11 0 0 -6.65 4.19 11 0 0 5.99 5.53 11 -1 0 4.10 4.63 -11 1 0 11.77 6.31 10 -1 0 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5.23 1 4 -19 -2.65 3.76 -1 -4 19 -0.38 4.34 2 3 -19 16.32 5.99 -2 -3 19 20.22 6.53 1 3 -19 -2.68 4.13 -1 -3 19 3.66 4.52 2 2 -19 4.97 4.69 -2 -2 19 5.20 4.47 1 2 -19 -1.27 3.83 -1 -2 19 -1.27 4.09 2 1 -19 8.08 5.12 -2 -1 19 1.35 4.74 -1 -1 19 -2.79 4.17 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 6823 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969309' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_10 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 N3 O7 Tm' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 886.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tm Tm -0.3139 5.2483 '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 8.692(5) _cell_length_b 13.033(5) _cell_length_c 14.775(5) _cell_angle_alpha 100.252(5) _cell_angle_beta 97.701(5) _cell_angle_gamma 92.426(5) _cell_volume 1628.4(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 28883 _cell_measurement_theta_min 4.740 _cell_measurement_theta_max 50.141 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_F_000 876 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 3.027 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6044 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details 'TWINABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 28797 _diffrn_reflns_av_unetI/netI 0.0696 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min ? _diffrn_reflns_limit_h_max ? _diffrn_reflns_limit_k_min ? _diffrn_reflns_limit_k_max ? _diffrn_reflns_limit_l_min ? _diffrn_reflns_limit_l_max ? _diffrn_reflns_theta_min 1.415 _diffrn_reflns_theta_max 25.591 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 6099 _reflns_number_gt 5045 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Data were apparently pre-merged, so _diffrn_reflns_number etc. will have to be added later. 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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0329P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6099 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.967 _refine_ls_restrained_S_all 0.967 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tm1 Tm 0.56101(3) 0.51288(2) 0.70171(2) 0.01247(7) Uani 1 1 d . . . . . O6 O 0.8436(4) 0.5799(3) 0.5026(2) 0.0189(8) Uani 1 1 d . . . . . O3 O 0.5601(4) 0.3780(2) 0.5611(2) 0.0157(7) Uani 1 1 d . . . . . O1 O 0.7086(4) 0.6223(2) 0.8409(2) 0.0179(8) Uani 1 1 d . . . . . O4 O 0.4048(4) 0.3510(2) 0.6610(2) 0.0164(8) Uani 1 1 d . . . . . O2 O 0.5346(4) 0.6961(2) 0.7551(2) 0.0164(8) Uani 1 1 d . . . . . C16 C 0.6393(6) 0.7016(4) 0.8237(3) 0.0156(11) Uani 1 1 d . . . . . C23 C 0.4594(6) 0.3210(3) 0.5875(3) 0.0124(10) Uani 1 1 d . . . . . N1 N 0.7878(5) 0.4060(3) 0.7237(3) 0.0152(9) Uani 1 1 d . . . . . O5 O 0.7253(4) 0.5958(2) 0.6292(2) 0.0184(8) Uani 1 1 d . . . . . OW1 O 0.3730(4) 0.5586(3) 0.5935(2) 0.0159(7) Uani 1 1 d D . . . . C24 C 0.4068(6) 0.2158(4) 0.5287(3) 0.0149(11) Uani 1 1 d . . . . . N3 N 0.3380(5) 0.5386(3) 0.7945(2) 0.0119(9) Uani 1 1 d . . . . . C17 C 0.6818(6) 0.8060(4) 0.8853(3) 0.0157(11) Uani 1 1 d . . . . . C13 C 0.0899(6) 0.5673(4) 0.8939(3) 0.0213(12) Uani 1 1 d . . . . . H13 H 0.0068 0.5770 0.9274 0.026 Uiso 1 1 calc R U . . . N2 N 0.5685(5) 0.4153(3) 0.8357(2) 0.0123(9) Uani 1 1 d . . . . . C14 C 0.1002(6) 0.6170(4) 0.8191(3) 0.0201(12) Uani 1 1 d . . . . . H14 H 0.0231 0.6592 0.8004 0.024 Uiso 1 1 calc R U . . . C5 C 0.8081(6) 0.3496(3) 0.7932(3) 0.0142(11) Uani 1 1 d . . . . . C10 C 0.4490(6) 0.4168(3) 0.8855(3) 0.0113(10) Uani 1 1 d . . . . . C15 C 0.2278(6) 0.6022(4) 0.7731(3) 0.0164(11) Uani 1 1 d . . . . . H15 H 0.2376 0.6382 0.7250 0.020 Uiso 1 1 calc R U . . . C12 C 0.2041(6) 0.5036(4) 0.9177(3) 0.0166(11) Uani 1 1 d . . . . . H12 H 0.1997 0.4703 0.9680 0.020 Uiso 1 1 calc R U . . . C31 C 0.9185(6) 0.7269(4) 0.6208(3) 0.0133(10) Uani 1 1 d . . . . . C1 C 0.8994(6) 0.4041(4) 0.6683(3) 0.0164(11) Uani 1 1 d . . . . . H1 H 0.8849 0.4401 0.6191 0.020 Uiso 1 1 calc R U . . . C18 C 0.8044(6) 0.8204(4) 0.9567(3) 0.0186(11) Uani 1 1 d . . . . . H18 H 0.8636 0.7646 0.9664 0.022 Uiso 1 1 calc R U . . . C32 C 0.8687(6) 0.7990(4) 0.6904(3) 0.0173(11) Uani 1 1 d . . . . . H32 H 0.7755 0.7849 0.7116 0.021 Uiso 1 1 calc R U . . . C30 C 0.8219(6) 0.6269(3) 0.5808(3) 0.0141(10) Uani 1 1 d . . . . . C3 C 1.0556(6) 0.2981(4) 0.7525(3) 0.0190(11) Uani 1 1 d . . . . . H3 H 1.1460 0.2638 0.7632 0.023 Uiso 1 1 calc R U . . . C4 C 0.9413(6) 0.2958(4) 0.8086(3) 0.0173(11) Uani 1 1 d . . . . . H4 H 0.9532 0.2583 0.8567 0.021 Uiso 1 1 calc R U . . . C2 C 1.0332(6) 0.3526(3) 0.6798(3) 0.0175(11) Uani 1 1 d . . . . . H2 H 1.1069 0.3542 0.6398 0.021 Uiso 1 1 calc R U . . . C20 C 0.7537(6) 0.9996(4) 0.9973(3) 0.0185(11) Uani 1 1 d . . . . . C21 C 0.6321(6) 0.9880(4) 0.9253(3) 0.0189(11) Uani 1 1 d . . . . . H21 H 0.5752 1.0446 0.9146 0.023 Uiso 1 1 calc R U . . . C6 C 0.6799(6) 0.3479(4) 0.8486(3) 0.0148(11) Uani 1 1 d . . . . . C8 C 0.5504(6) 0.2823(4) 0.9615(3) 0.0229(12) Uani 1 1 d . . . . . H8 H 0.5444 0.2375 1.0036 0.028 Uiso 1 1 calc R U . . . C25 C 0.4726(6) 0.1798(4) 0.4497(3) 0.0201(12) Uani 1 1 d . . . . . H25 H 0.5473 0.2219 0.4315 0.024 Uiso 1 1 calc R U . . . C7 C 0.6724(6) 0.2796(4) 0.9102(3) 0.0178(11) Uani 1 1 d . . . . . H7 H 0.7487 0.2324 0.9169 0.021 Uiso 1 1 calc R U . . . C28 C 0.2421(7) 0.0557(4) 0.5013(4) 0.0246(13) Uani 1 1 d . . . . . H28 H 0.1646 0.0144 0.5179 0.030 Uiso 1 1 calc R U . . . C19 C 0.8409(6) 0.9170(4) 1.0144(3) 0.0201(11) Uani 1 1 d . . . . . H19 H 0.9222 0.9260 1.0635 0.024 Uiso 1 1 calc R U . . . C35 C 1.1446(6) 0.8412(4) 0.6260(4) 0.0221(12) Uani 1 1 d . . . . . H35 H 1.2370 0.8563 0.6043 0.027 Uiso 1 1 calc R U . . . C29 C 0.2907(6) 0.1545(4) 0.5538(3) 0.0193(11) Uani 1 1 d . . . . . H29 H 0.2450 0.1795 0.6061 0.023 Uiso 1 1 calc R U . . . C33 C 0.9565(6) 0.8916(4) 0.7283(3) 0.0198(12) Uani 1 1 d . . . . . H33 H 0.9230 0.9398 0.7747 0.024 Uiso 1 1 calc R U . . . C11 C 0.3258(6) 0.4892(3) 0.8664(3) 0.0149(11) Uani 1 1 d . . . . . C26 C 0.4273(7) 0.0810(4) 0.3976(3) 0.0263(13) Uani 1 1 d . . . . . H26 H 0.4738 0.0556 0.3457 0.032 Uiso 1 1 calc R U . . . C9 C 0.4385(6) 0.3515(4) 0.9499(3) 0.0196(12) Uani 1 1 d . . . . . H9 H 0.3565 0.3550 0.9845 0.023 Uiso 1 1 calc R U . . . C36 C 1.0558(6) 0.7486(4) 0.5880(3) 0.0194(11) Uani 1 1 d . . . . . H36 H 1.0887 0.7013 0.5407 0.023 Uiso 1 1 calc R U . . . C27 C 0.3125(7) 0.0209(4) 0.4238(3) 0.0221(12) Uani 1 1 d . . . . . C34 C 1.0944(6) 0.9108(4) 0.6962(3) 0.0191(11) Uani 1 1 d . . . . . C22 C 0.5959(6) 0.8907(4) 0.8692(3) 0.0177(11) Uani 1 1 d . . . . . H22 H 0.5138 0.8817 0.8205 0.021 Uiso 1 1 calc R U . . . Cl1 Cl 0.79719(17) 1.12080(9) 1.07046(9) 0.0248(3) Uani 1 1 d . . . . . Cl3 Cl 1.20910(18) 1.02630(10) 0.74377(9) 0.0320(3) Uani 1 1 d . . . . . Cl2 Cl 0.2501(2) -0.10123(10) 0.35670(10) 0.0396(4) Uani 1 1 d . . . . . H37 H 0.404(6) 0.591(4) 0.544(3) 0.029(15) Uiso 1 1 d D . . . . H38 H 0.293(6) 0.509(4) 0.556(4) 0.07(2) Uiso 1 1 d 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 Tm1 0.01115(13) 0.01398(11) 0.01240(11) 0.00231(8) 0.00230(8) 0.00082(8) O6 0.017(2) 0.0221(18) 0.0177(18) 0.0030(15) 0.0040(15) -0.0040(15) O3 0.014(2) 0.0166(17) 0.0163(17) 0.0035(14) 0.0016(14) -0.0007(14) O1 0.016(2) 0.0177(18) 0.0222(18) 0.0061(14) 0.0058(15) 0.0042(15) O4 0.016(2) 0.0198(17) 0.0135(17) 0.0018(14) 0.0059(14) 0.0006(15) O2 0.016(2) 0.0145(17) 0.0185(18) 0.0016(14) 0.0036(15) -0.0012(14) C16 0.019(3) 0.013(2) 0.018(3) 0.006(2) 0.010(2) -0.001(2) C23 0.010(3) 0.015(2) 0.014(2) 0.0058(19) 0.001(2) 0.007(2) N1 0.016(3) 0.012(2) 0.017(2) 0.0019(16) 0.0031(18) 0.0026(17) O5 0.017(2) 0.0197(18) 0.0207(18) 0.0058(14) 0.0069(15) 0.0012(15) OW1 0.013(2) 0.0213(18) 0.0143(17) 0.0054(14) 0.0019(15) 0.0011(15) C24 0.013(3) 0.014(2) 0.017(2) 0.006(2) -0.003(2) 0.003(2) N3 0.011(2) 0.0114(19) 0.013(2) 0.0016(16) 0.0037(16) -0.0010(16) C17 0.020(3) 0.016(2) 0.012(2) 0.0009(19) 0.008(2) -0.002(2) C13 0.014(3) 0.025(3) 0.024(3) 0.000(2) 0.009(2) 0.002(2) N2 0.013(2) 0.0105(19) 0.0113(19) 0.0003(15) -0.0015(17) 0.0007(16) C14 0.015(3) 0.020(3) 0.024(3) 0.001(2) 0.002(2) 0.004(2) C5 0.017(3) 0.012(2) 0.012(2) 0.0019(18) -0.001(2) -0.002(2) C10 0.005(3) 0.016(2) 0.012(2) 0.0010(18) 0.0033(19) 0.0000(19) C15 0.013(3) 0.018(2) 0.018(3) 0.003(2) 0.000(2) 0.004(2) C12 0.014(3) 0.017(2) 0.020(3) 0.003(2) 0.009(2) 0.005(2) C31 0.008(3) 0.018(2) 0.014(2) 0.0076(19) -0.002(2) 0.002(2) C1 0.012(3) 0.019(3) 0.019(3) 0.003(2) 0.007(2) 0.003(2) C18 0.020(3) 0.017(2) 0.021(3) 0.006(2) 0.006(2) 0.001(2) C32 0.010(3) 0.023(3) 0.022(3) 0.009(2) 0.005(2) 0.001(2) C30 0.006(3) 0.016(2) 0.022(3) 0.011(2) -0.002(2) 0.0032(19) C3 0.017(3) 0.017(2) 0.020(3) -0.007(2) 0.001(2) 0.000(2) C4 0.014(3) 0.021(3) 0.017(3) 0.006(2) 0.000(2) 0.005(2) C2 0.016(3) 0.016(2) 0.020(3) -0.001(2) 0.005(2) -0.001(2) C20 0.023(3) 0.012(2) 0.020(3) 0.003(2) 0.005(2) -0.002(2) C21 0.020(3) 0.018(3) 0.018(3) 0.004(2) 0.001(2) 0.004(2) C6 0.013(3) 0.018(2) 0.013(2) 0.0014(19) 0.003(2) 0.001(2) C8 0.022(3) 0.029(3) 0.023(3) 0.013(2) 0.009(2) 0.006(2) C25 0.014(3) 0.020(3) 0.025(3) 0.000(2) 0.001(2) 0.000(2) C7 0.022(3) 0.014(2) 0.021(3) 0.008(2) 0.006(2) 0.008(2) C28 0.025(4) 0.014(3) 0.034(3) 0.009(2) -0.003(3) -0.005(2) C19 0.018(3) 0.025(3) 0.017(3) 0.005(2) 0.001(2) 0.006(2) C35 0.010(3) 0.023(3) 0.037(3) 0.011(2) 0.006(2) -0.001(2) C29 0.020(3) 0.016(2) 0.021(3) 0.004(2) 0.000(2) 0.005(2) C33 0.024(3) 0.019(3) 0.017(3) 0.006(2) 0.002(2) 0.004(2) C11 0.009(3) 0.014(2) 0.017(2) -0.0070(19) 0.001(2) -0.003(2) C26 0.031(4) 0.026(3) 0.019(3) -0.003(2) 0.001(2) 0.008(3) C9 0.018(3) 0.025(3) 0.017(3) 0.004(2) 0.008(2) 0.000(2) C36 0.015(3) 0.025(3) 0.020(3) 0.003(2) 0.008(2) 0.006(2) C27 0.028(4) 0.012(2) 0.022(3) 0.000(2) -0.010(2) 0.005(2) C34 0.014(3) 0.018(3) 0.024(3) 0.005(2) 0.001(2) -0.003(2) C22 0.017(3) 0.019(3) 0.017(3) 0.006(2) 0.000(2) 0.000(2) Cl1 0.0287(9) 0.0176(6) 0.0252(7) -0.0001(5) -0.0018(6) 0.0034(5) Cl3 0.0362(10) 0.0245(7) 0.0330(8) 0.0016(6) 0.0056(6) -0.0083(6) Cl2 0.0480(11) 0.0193(7) 0.0420(9) -0.0052(6) -0.0126(7) 0.0008(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tm1 O5 2.246(3) . ? Tm1 OW1 2.303(3) . ? Tm1 O4 2.396(3) . ? Tm1 O2 2.409(3) . ? Tm1 O1 2.450(3) . ? Tm1 O3 2.469(3) . ? Tm1 N1 2.481(4) . ? Tm1 N3 2.520(4) . ? Tm1 N2 2.531(4) . ? Tm1 C16 2.777(5) . ? Tm1 C23 2.792(5) . ? O6 C30 1.250(6) . ? O3 C23 1.269(6) . ? O1 C16 1.265(6) . ? O4 C23 1.249(5) . ? O2 C16 1.258(6) . ? C16 C17 1.498(6) . ? C23 C24 1.503(6) . ? N1 C1 1.349(6) . ? N1 C5 1.363(6) . ? O5 C30 1.272(6) . ? OW1 H37 0.96(2) . ? OW1 H38 0.97(2) . ? C24 C25 1.383(7) . ? C24 C29 1.390(7) . ? N3 C15 1.336(6) . ? N3 C11 1.350(6) . ? C17 C18 1.376(7) . ? C17 C22 1.396(7) . ? C13 C12 1.369(7) . ? C13 C14 1.389(7) . ? C13 H13 0.9300 . ? N2 C10 1.350(6) . ? N2 C6 1.353(6) . ? C14 C15 1.379(7) . ? C14 H14 0.9300 . ? C5 C4 1.392(7) . ? C5 C6 1.470(7) . ? C10 C9 1.393(6) . ? C10 C11 1.489(7) . ? C15 H15 0.9300 . ? C12 C11 1.382(7) . ? C12 H12 0.9300 . ? C31 C36 1.383(7) . ? C31 C32 1.392(7) . ? C31 C30 1.501(6) . ? C1 C2 1.373(7) . ? C1 H1 0.9300 . ? C18 C19 1.387(7) . ? C18 H18 0.9300 . ? C32 C33 1.385(7) . ? C32 H32 0.9300 . ? C3 C4 1.379(7) . ? C3 C2 1.386(7) . ? C3 H3 0.9300 . ? C4 H4 0.9300 . ? C2 H2 0.9300 . ? C20 C21 1.379(7) . ? C20 C19 1.382(7) . ? C20 Cl1 1.743(5) . ? C21 C22 1.384(7) . ? C21 H21 0.9300 . ? C6 C7 1.387(6) . ? C8 C9 1.369(7) . ? C8 C7 1.382(7) . ? C8 H8 0.9300 . ? C25 C26 1.390(7) . ? C25 H25 0.9300 . ? C7 H7 0.9300 . ? C28 C27 1.384(8) . ? C28 C29 1.396(7) . ? C28 H28 0.9300 . ? C19 H19 0.9300 . ? C35 C34 1.381(7) . ? C35 C36 1.390(7) . ? C35 H35 0.9300 . ? C29 H29 0.9300 . ? C33 C34 1.376(7) . ? C33 H33 0.9300 . ? C26 C27 1.380(8) . ? C26 H26 0.9300 . ? C9 H9 0.9300 . ? C36 H36 0.9300 . ? C27 Cl2 1.741(5) . ? C34 Cl3 1.750(5) . ? C22 H22 0.9300 . ? 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 Tm1 OW1 83.85(13) . . ? O5 Tm1 O4 134.17(11) . . ? OW1 Tm1 O4 81.12(12) . . ? O5 Tm1 O2 75.08(11) . . ? OW1 Tm1 O2 75.09(11) . . ? O4 Tm1 O2 139.78(12) . . ? O5 Tm1 O1 82.78(12) . . ? OW1 Tm1 O1 129.07(11) . . ? O4 Tm1 O1 138.36(10) . . ? O2 Tm1 O1 53.98(11) . . ? O5 Tm1 O3 80.86(11) . . ? OW1 Tm1 O3 75.43(11) . . ? O4 Tm1 O3 53.50(11) . . ? O2 Tm1 O3 143.52(11) . . ? O1 Tm1 O3 148.58(12) . . ? O5 Tm1 N1 81.23(13) . . ? OW1 Tm1 N1 144.54(12) . . ? O4 Tm1 N1 86.58(13) . . ? O2 Tm1 N1 130.45(12) . . ? O1 Tm1 N1 80.58(12) . . ? O3 Tm1 N1 70.56(12) . . ? O5 Tm1 N3 143.42(12) . . ? OW1 Tm1 N3 79.28(13) . . ? O4 Tm1 N3 74.75(11) . . ? O2 Tm1 N3 69.33(11) . . ? O1 Tm1 N3 83.13(12) . . ? O3 Tm1 N3 124.78(12) . . ? N1 Tm1 N3 129.08(13) . . ? O5 Tm1 N2 139.44(13) . . ? OW1 Tm1 N2 136.71(13) . . ? O4 Tm1 N2 67.63(11) . . ? O2 Tm1 N2 110.33(11) . . ? O1 Tm1 N2 71.08(11) . . ? O3 Tm1 N2 105.82(11) . . ? N1 Tm1 N2 64.63(13) . . ? N3 Tm1 N2 64.45(13) . . ? O5 Tm1 C16 77.07(13) . . ? OW1 Tm1 C16 101.97(14) . . ? O4 Tm1 C16 148.47(12) . . ? O2 Tm1 C16 26.89(13) . . ? O1 Tm1 C16 27.09(13) . . ? O3 Tm1 C16 157.93(13) . . ? N1 Tm1 C16 105.71(14) . . ? N3 Tm1 C16 75.07(13) . . ? N2 Tm1 C16 91.15(13) . . ? O5 Tm1 C23 107.84(13) . . ? OW1 Tm1 C23 77.34(12) . . ? O4 Tm1 C23 26.47(12) . . ? O2 Tm1 C23 151.79(13) . . ? O1 Tm1 C23 153.17(12) . . ? O3 Tm1 C23 27.03(12) . . ? N1 Tm1 C23 76.96(13) . . ? N3 Tm1 C23 99.80(13) . . ? N2 Tm1 C23 86.02(12) . . ? C16 Tm1 C23 174.84(14) . . ? C23 O3 Tm1 90.8(3) . . ? C16 O1 Tm1 91.0(3) . . ? C23 O4 Tm1 94.7(3) . . ? C16 O2 Tm1 93.1(3) . . ? O2 C16 O1 122.0(4) . . ? O2 C16 C17 118.0(4) . . ? O1 C16 C17 120.1(5) . . ? O2 C16 Tm1 60.0(2) . . ? O1 C16 Tm1 61.9(2) . . ? C17 C16 Tm1 177.1(3) . . ? O4 C23 O3 120.9(4) . . ? O4 C23 C24 120.3(4) . . ? O3 C23 C24 118.7(4) . . ? O4 C23 Tm1 58.8(2) . . ? O3 C23 Tm1 62.2(2) . . ? C24 C23 Tm1 178.0(3) . . ? C1 N1 C5 117.2(4) . . ? C1 N1 Tm1 120.7(3) . . ? C5 N1 Tm1 122.0(3) . . ? C30 O5 Tm1 170.0(3) . . ? Tm1 OW1 H37 120(3) . . ? Tm1 OW1 H38 123(4) . . ? H37 OW1 H38 98(5) . . ? C25 C24 C29 119.8(4) . . ? C25 C24 C23 120.6(4) . . ? C29 C24 C23 119.6(4) . . ? C15 N3 C11 118.2(4) . . ? C15 N3 Tm1 120.2(3) . . ? C11 N3 Tm1 121.6(3) . . ? C18 C17 C22 119.3(4) . . ? C18 C17 C16 121.6(4) . . ? C22 C17 C16 119.1(4) . . ? C12 C13 C14 119.0(5) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.5 . . ? C10 N2 C6 118.6(4) . . ? C10 N2 Tm1 120.6(3) . . ? C6 N2 Tm1 119.9(3) . . ? C15 C14 C13 118.3(5) . . ? C15 C14 H14 120.8 . . ? C13 C14 H14 120.8 . . ? N1 C5 C4 121.3(5) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.9(4) . . ? N2 C10 C9 121.8(4) . . ? N2 C10 C11 116.9(4) . . ? C9 C10 C11 121.3(4) . . ? N3 C15 C14 123.1(5) . . ? N3 C15 H15 118.5 . . ? C14 C15 H15 118.5 . . ? C13 C12 C11 119.7(5) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C36 C31 C32 119.7(4) . . ? C36 C31 C30 120.4(4) . . ? C32 C31 C30 119.9(4) . . ? N1 C1 C2 124.2(5) . . ? N1 C1 H1 117.9 . . ? C2 C1 H1 117.9 . . ? C17 C18 C19 121.0(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C33 C32 C31 120.7(5) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? O6 C30 O5 124.9(4) . . ? O6 C30 C31 117.4(4) . . ? O5 C30 C31 117.7(4) . . ? C4 C3 C2 118.8(5) . . ? C4 C3 H3 120.6 . . ? C2 C3 H3 120.6 . . ? C3 C4 C5 120.1(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C1 C2 C3 118.4(5) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C21 C20 C19 121.7(4) . . ? C21 C20 Cl1 119.4(4) . . ? C19 C20 Cl1 118.8(4) . . ? C20 C21 C22 118.9(5) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? N2 C6 C7 121.6(5) . . ? N2 C6 C5 116.7(4) . . ? C7 C6 C5 121.7(4) . . ? C9 C8 C7 119.4(5) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C24 C25 C26 120.2(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C8 C7 C6 119.3(5) . . ? C8 C7 H7 120.4 . . ? C6 C7 H7 120.4 . . ? C27 C28 C29 118.2(5) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C20 C19 C18 118.5(5) . . ? C20 C19 H19 120.7 . . ? C18 C19 H19 120.7 . . ? C34 C35 C36 119.5(5) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C24 C29 C28 120.6(5) . . ? C24 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C34 C33 C32 118.8(5) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? N3 C11 C12 121.7(4) . . ? N3 C11 C10 116.0(4) . . ? C12 C11 C10 122.3(4) . . ? C27 C26 C25 119.2(5) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C8 C9 C10 119.2(5) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C31 C36 C35 119.8(5) . . ? C31 C36 H36 120.1 . . ? C35 C36 H36 120.1 . . ? C26 C27 C28 121.9(5) . . ? C26 C27 Cl2 119.6(4) . . ? C28 C27 Cl2 118.5(4) . . ? C33 C34 C35 121.5(5) . . ? C33 C34 Cl3 119.8(4) . . ? C35 C34 Cl3 118.7(4) . . ? C21 C22 C17 120.4(5) . . ? C21 C22 H22 119.8 . . ? C17 C22 H22 119.8 . . ? _refine_diff_density_max 1.129 _refine_diff_density_min -1.347 _refine_diff_density_rms 0.142 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1_twin2 in P-1 CELL 0.71073 8.6920 13.0330 14.7750 100.252 97.701 92.426 ZERR 2.00 0.0050 0.0050 0.0050 0.005 0.005 0.005 LATT 1 SFAC C H N O CL TM UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 12 WGHT 0.032900 FVAR 0.12061 TM1 6 0.561010 0.512878 0.701710 11.00000 0.01115 0.01398 = 0.01240 0.00231 0.00230 0.00082 O6 4 0.843620 0.579905 0.502556 11.00000 0.01669 0.02214 = 0.01768 0.00300 0.00398 -0.00398 O3 4 0.560055 0.378039 0.561123 11.00000 0.01395 0.01660 = 0.01628 0.00345 0.00163 -0.00071 O1 4 0.708600 0.622313 0.840935 11.00000 0.01575 0.01771 = 0.02218 0.00611 0.00584 0.00417 O4 4 0.404848 0.351042 0.661005 11.00000 0.01637 0.01978 = 0.01348 0.00182 0.00587 0.00063 O2 4 0.534600 0.696149 0.755093 11.00000 0.01593 0.01451 = 0.01848 0.00164 0.00364 -0.00117 C16 1 0.639348 0.701567 0.823653 11.00000 0.01859 0.01329 = 0.01788 0.00552 0.00998 -0.00073 C23 1 0.459367 0.320964 0.587505 11.00000 0.00963 0.01491 = 0.01425 0.00583 0.00109 0.00702 N1 3 0.787842 0.405958 0.723692 11.00000 0.01624 0.01246 = 0.01699 0.00194 0.00311 0.00262 O5 4 0.725334 0.595770 0.629229 11.00000 0.01682 0.01974 = 0.02071 0.00584 0.00685 0.00124 OW1 4 0.373046 0.558597 0.593458 11.00000 0.01304 0.02128 = 0.01428 0.00543 0.00195 0.00115 C24 1 0.406840 0.215790 0.528679 11.00000 0.01260 0.01420 = 0.01747 0.00583 -0.00348 0.00256 N3 3 0.338045 0.538611 0.794510 11.00000 0.01121 0.01141 = 0.01327 0.00162 0.00370 -0.00100 C17 1 0.681847 0.805951 0.885287 11.00000 0.01983 0.01552 = 0.01233 0.00088 0.00762 -0.00203 C13 1 0.089913 0.567281 0.893941 11.00000 0.01437 0.02530 = 0.02439 -0.00011 0.00903 0.00220 AFIX 43 H13 2 0.006762 0.577047 0.927447 11.00000 -1.20000 AFIX 0 N2 3 0.568460 0.415328 0.835659 11.00000 0.01347 0.01049 = 0.01130 0.00030 -0.00154 0.00075 C14 1 0.100249 0.617017 0.819083 11.00000 0.01502 0.02024 = 0.02383 0.00123 0.00156 0.00421 AFIX 43 H14 2 0.023055 0.659249 0.800418 11.00000 -1.20000 AFIX 0 C5 1 0.808063 0.349602 0.793223 11.00000 0.01661 0.01244 = 0.01221 0.00189 -0.00083 -0.00197 C10 1 0.448987 0.416792 0.885512 11.00000 0.00536 0.01637 = 0.01209 0.00097 0.00326 0.00003 C15 1 0.227827 0.602223 0.773119 11.00000 0.01280 0.01754 = 0.01839 0.00334 -0.00018 0.00444 AFIX 43 H15 2 0.237594 0.638216 0.724972 11.00000 -1.20000 AFIX 0 C12 1 0.204050 0.503636 0.917655 11.00000 0.01425 0.01723 = 0.02049 0.00325 0.00941 0.00506 AFIX 43 H12 2 0.199651 0.470291 0.967999 11.00000 -1.20000 AFIX 0 C31 1 0.918475 0.726924 0.620750 11.00000 0.00772 0.01848 = 0.01434 0.00756 -0.00207 0.00174 C1 1 0.899444 0.404139 0.668264 11.00000 0.01210 0.01906 = 0.01932 0.00311 0.00720 0.00329 AFIX 43 H1 2 0.884861 0.440097 0.619099 11.00000 -1.20000 AFIX 0 C18 1 0.804357 0.820431 0.956680 11.00000 0.01985 0.01686 = 0.02090 0.00617 0.00550 0.00094 AFIX 43 H18 2 0.863608 0.764575 0.966395 11.00000 -1.20000 AFIX 0 C32 1 0.868663 0.799006 0.690385 11.00000 0.00995 0.02293 = 0.02164 0.00907 0.00511 0.00088 AFIX 43 H32 2 0.775470 0.784877 0.711646 11.00000 -1.20000 AFIX 0 C30 1 0.821945 0.626851 0.580788 11.00000 0.00625 0.01578 = 0.02209 0.01099 -0.00193 0.00324 C3 1 1.055592 0.298120 0.752458 11.00000 0.01667 0.01674 = 0.01952 -0.00664 0.00127 0.00049 AFIX 43 H3 2 1.146017 0.263771 0.763172 11.00000 -1.20000 AFIX 0 C4 1 0.941280 0.295816 0.808564 11.00000 0.01399 0.02148 = 0.01704 0.00607 0.00023 0.00505 AFIX 43 H4 2 0.953208 0.258273 0.856722 11.00000 -1.20000 AFIX 0 C2 1 1.033156 0.352603 0.679794 11.00000 0.01636 0.01564 = 0.01966 -0.00087 0.00540 -0.00147 AFIX 43 H2 2 1.106908 0.354203 0.639822 11.00000 -1.20000 AFIX 0 C20 1 0.753749 0.999608 0.997313 11.00000 0.02331 0.01241 = 0.02013 0.00272 0.00545 -0.00204 C21 1 0.632062 0.987970 0.925279 11.00000 0.02019 0.01806 = 0.01839 0.00367 0.00115 0.00380 AFIX 43 H21 2 0.575239 1.044581 0.914554 11.00000 -1.20000 AFIX 0 C6 1 0.679897 0.347905 0.848633 11.00000 0.01287 0.01834 = 0.01299 0.00140 0.00347 0.00112 C8 1 0.550435 0.282316 0.961507 11.00000 0.02202 0.02924 = 0.02254 0.01301 0.00856 0.00650 AFIX 43 H8 2 0.544385 0.237528 1.003564 11.00000 -1.20000 AFIX 0 C25 1 0.472584 0.179816 0.449736 11.00000 0.01361 0.01965 = 0.02493 -0.00017 0.00089 0.00014 AFIX 43 H25 2 0.547320 0.221921 0.431513 11.00000 -1.20000 AFIX 0 C7 1 0.672436 0.279574 0.910212 11.00000 0.02214 0.01374 = 0.02058 0.00779 0.00598 0.00762 AFIX 43 H7 2 0.748696 0.232446 0.916894 11.00000 -1.20000 AFIX 0 C28 1 0.242146 0.055699 0.501262 11.00000 0.02517 0.01410 = 0.03362 0.00914 -0.00314 -0.00512 AFIX 43 H28 2 0.164608 0.014392 0.517871 11.00000 -1.20000 AFIX 0 C19 1 0.840882 0.917017 1.014390 11.00000 0.01816 0.02510 = 0.01739 0.00523 0.00114 0.00553 AFIX 43 H19 2 0.922202 0.926006 1.063488 11.00000 -1.20000 AFIX 0 C35 1 1.144561 0.841233 0.626004 11.00000 0.00970 0.02282 = 0.03656 0.01092 0.00644 -0.00134 AFIX 43 H35 2 1.237032 0.856259 0.604330 11.00000 -1.20000 AFIX 0 C29 1 0.290728 0.154498 0.553798 11.00000 0.01990 0.01614 = 0.02147 0.00358 0.00021 0.00509 AFIX 43 H29 2 0.244982 0.179533 0.606082 11.00000 -1.20000 AFIX 0 C33 1 0.956522 0.891571 0.728326 11.00000 0.02444 0.01868 = 0.01731 0.00577 0.00225 0.00409 AFIX 43 H33 2 0.922964 0.939807 0.774665 11.00000 -1.20000 AFIX 0 C11 1 0.325801 0.489203 0.866411 11.00000 0.00946 0.01365 = 0.01732 -0.00703 0.00112 -0.00279 C26 1 0.427312 0.080966 0.397579 11.00000 0.03120 0.02628 = 0.01856 -0.00336 0.00114 0.00782 AFIX 43 H26 2 0.473792 0.055613 0.345664 11.00000 -1.20000 AFIX 0 C9 1 0.438545 0.351541 0.949875 11.00000 0.01767 0.02516 = 0.01736 0.00433 0.00774 -0.00037 AFIX 43 H9 2 0.356528 0.354963 0.984538 11.00000 -1.20000 AFIX 0 C36 1 1.055815 0.748578 0.588029 11.00000 0.01492 0.02485 = 0.01995 0.00338 0.00769 0.00556 AFIX 43 H36 2 1.088691 0.701272 0.540748 11.00000 -1.20000 AFIX 0 C27 1 0.312468 0.020883 0.423809 11.00000 0.02841 0.01163 = 0.02171 0.00032 -0.01047 0.00458 C34 1 1.094362 0.910815 0.696173 11.00000 0.01413 0.01847 = 0.02426 0.00524 0.00066 -0.00323 C22 1 0.595860 0.890680 0.869201 11.00000 0.01747 0.01851 = 0.01724 0.00553 0.00044 -0.00044 AFIX 43 H22 2 0.513808 0.881683 0.820534 11.00000 -1.20000 AFIX 0 CL1 5 0.797192 1.120801 1.070465 11.00000 0.02869 0.01763 = 0.02523 -0.00012 -0.00185 0.00342 CL3 5 1.209102 1.026304 0.743773 11.00000 0.03621 0.02453 = 0.03299 0.00160 0.00558 -0.00833 CL2 5 0.250060 -0.101231 0.356695 11.00000 0.04805 0.01926 = 0.04199 -0.00519 -0.01258 0.00083 H37 2 0.403603 0.591088 0.544313 11.00000 0.02923 H38 2 0.292699 0.509059 0.555922 11.00000 0.06836 HKLF 4 REM Pbar1_twin2 in P-1 REM R1 = 0.0359 for 5045 Fo > 4sig(Fo) and 0.0472 for all 6099 data REM 459 parameters refined using 2 restraints END WGHT 0.0328 0.0000 REM Highest difference peak 1.129, deepest hole -1.347, 1-sigma level 0.142 Q1 1 0.6072 0.5504 0.7609 11.00000 0.05 1.13 Q2 1 0.5240 0.4818 0.6524 11.00000 0.05 1.11 Q3 1 0.4412 0.5309 0.6241 11.00000 0.05 0.73 Q4 1 0.5463 0.4684 0.7284 11.00000 0.05 0.71 Q5 1 0.4624 0.4118 0.7003 11.00000 0.05 0.70 Q6 1 0.5651 0.5342 0.5992 11.00000 0.05 0.66 Q7 1 0.3090 0.4581 0.8977 11.00000 0.05 0.66 Q8 1 0.5558 0.4876 0.7999 11.00000 0.05 0.61 Q9 1 0.6184 0.4674 0.6163 11.00000 0.05 0.60 Q10 1 1.1077 1.0639 0.7642 11.00000 0.05 0.60 ; _shelx_res_checksum 53097 _shelx_hkl_file ; 1 0 0 341.92 6.74 2 0 0 2.47 0.80 3 0 0 115.87 3.36 4 0 0 2.42 0.99 5 0 0 50.32 2.53 6 0 0 102.37 3.93 7 0 0 39.33 4.11 8 0 0 159.37 8.34 9 0 0 87.75 6.55 10 0 0 26.68 6.47 -10 1 0 20.33 6.01 -9 1 0 45.45 5.10 -8 1 0 158.15 8.39 -7 1 0 76.54 5.44 -6 1 0 10.11 1.49 -5 1 0 0.27 0.87 -4 1 0 5.19 1.00 -3 1 0 60.73 3.45 -2 1 0 585.63 9.81 -1 1 0 427.87 8.28 0 1 0 392.68 7.63 1 1 0 285.45 4.23 2 1 0 150.10 3.99 3 1 0 6.46 1.11 4 1 0 33.94 2.08 5 1 0 5.00 1.40 6 1 0 81.47 3.60 7 1 0 128.87 6.95 8 1 0 54.29 4.98 9 1 0 64.95 8.53 10 1 0 39.77 7.47 -10 2 0 10.56 3.69 -9 2 0 54.28 5.50 -8 2 0 67.69 5.66 -7 2 0 36.14 4.10 -6 2 0 23.89 3.41 -5 2 0 15.63 1.33 -4 2 0 17.20 1.43 -3 2 0 11.47 1.32 -2 2 0 5.79 1.32 -1 2 0 198.71 2.82 0 2 0 395.10 4.70 1 2 0 197.19 3.92 2 2 0 2.75 0.60 3 2 0 84.49 3.11 4 2 0 2.36 1.16 5 2 0 96.64 3.75 6 2 0 80.93 3.67 7 2 0 64.45 4.91 8 2 0 29.82 6.01 9 2 0 94.55 10.30 10 2 0 26.09 6.63 -10 3 0 22.58 6.76 -9 3 0 38.06 7.30 -8 3 0 127.63 11.09 -7 3 0 17.35 3.39 -6 3 0 4.54 2.56 -5 3 0 1.81 0.90 -4 3 0 2.22 1.39 -3 3 0 63.63 3.05 -2 3 0 105.79 2.87 -1 3 0 67.42 1.77 0 3 0 30.70 1.26 1 3 0 188.43 2.77 2 3 0 2.53 0.97 3 3 0 17.13 1.04 4 3 0 10.75 1.40 5 3 0 25.56 2.18 6 3 0 53.63 3.09 7 3 0 140.76 6.71 8 3 0 2.23 4.83 9 3 0 39.45 7.59 10 3 0 12.17 6.37 -10 4 0 48.91 8.68 -9 4 0 71.21 9.37 -8 4 0 76.10 9.13 -7 4 0 7.53 4.45 -6 4 0 4.07 4.12 -5 4 0 0.97 0.70 -4 4 0 0.78 1.19 -3 4 0 6.35 1.52 -2 4 0 166.09 3.12 -1 4 0 155.61 2.96 0 4 0 4.81 0.91 1 4 0 159.42 2.67 2 4 0 94.53 3.21 3 4 0 7.34 1.42 4 4 0 11.01 1.19 5 4 0 18.48 1.35 6 4 0 70.97 4.67 7 4 0 39.43 3.36 8 4 0 25.14 4.02 9 4 0 36.76 4.85 -10 5 0 67.48 7.04 -9 5 0 50.81 5.89 -8 5 0 45.34 5.34 -7 5 0 11.73 3.52 -6 5 0 15.30 3.47 -5 5 0 0.37 1.43 -4 5 0 96.34 3.81 -3 5 0 3.05 1.25 -2 5 0 102.11 2.59 -1 5 0 201.52 3.68 0 5 0 102.72 2.46 1 5 0 36.71 1.45 2 5 0 204.83 5.21 3 5 0 8.65 1.55 4 5 0 42.32 2.62 5 5 0 30.53 2.06 6 5 0 53.55 2.81 7 5 0 36.59 3.35 8 5 0 71.40 6.27 9 5 0 16.43 3.61 -9 6 0 37.13 5.62 -8 6 0 53.40 5.86 -7 6 0 17.29 4.09 -6 6 0 18.97 3.87 -5 6 0 2.59 0.91 -4 6 0 24.27 2.10 -3 6 0 150.90 3.42 -2 6 0 107.14 2.84 -1 6 0 34.17 1.69 0 6 0 70.63 2.03 1 6 0 427.84 5.49 2 6 0 3.96 1.13 3 6 0 45.71 2.66 4 6 0 5.54 1.32 5 6 0 71.42 3.71 6 6 0 36.39 2.43 7 6 0 48.30 3.28 8 6 0 44.07 4.97 9 6 0 27.83 4.55 -9 7 0 42.51 6.68 -8 7 0 5.07 3.81 -7 7 0 43.48 5.36 -6 7 0 10.65 2.40 -5 7 0 35.59 2.06 -4 7 0 98.89 2.75 -3 7 0 41.28 2.02 -2 7 0 93.60 2.59 -1 7 0 382.25 5.55 0 7 0 48.54 1.94 1 7 0 0.60 0.63 2 7 0 23.08 2.03 3 7 0 0.26 0.96 4 7 0 84.09 3.59 5 7 0 131.15 4.51 6 7 0 39.48 2.75 7 7 0 95.65 4.43 8 7 0 85.32 6.72 9 7 0 9.84 19.12 -9 8 0 42.48 5.07 -8 8 0 65.18 5.68 -7 8 0 9.38 2.86 -6 8 0 1.32 1.78 -5 8 0 1.24 0.91 -4 8 0 104.46 2.98 -3 8 0 240.99 4.51 -2 8 0 41.84 2.11 -1 8 0 22.31 1.60 0 8 0 131.29 3.05 1 8 0 56.82 2.10 2 8 0 14.37 1.82 3 8 0 71.59 3.45 4 8 0 14.49 1.99 5 8 0 83.22 4.39 6 8 0 83.08 3.68 7 8 0 32.13 2.51 8 8 0 18.66 2.82 -8 9 0 34.12 4.50 -7 9 0 37.58 3.86 -6 9 0 1.83 1.72 -5 9 0 57.99 3.86 -4 9 0 29.90 2.03 -3 9 0 58.18 2.65 -2 9 0 107.56 3.07 -1 9 0 84.69 2.73 0 9 0 42.33 2.13 1 9 0 11.69 1.23 2 9 0 4.66 1.42 3 9 0 1.07 1.19 4 9 0 12.84 2.03 5 9 0 30.16 2.93 6 9 0 22.99 2.20 7 9 0 20.55 2.16 8 9 0 35.35 3.09 -8 10 0 16.89 3.89 -7 10 0 1.32 2.39 -6 10 0 5.91 2.13 -5 10 0 11.46 2.36 -4 10 0 70.47 3.23 -3 10 0 71.98 2.97 -2 10 0 36.11 2.22 -1 10 0 85.27 2.98 0 10 0 148.59 3.59 1 10 0 11.71 1.83 2 10 0 0.77 1.17 3 10 0 1.45 1.26 4 10 0 13.30 2.13 5 10 0 36.01 3.22 6 10 0 53.63 3.18 7 10 0 26.57 2.53 -7 11 0 1.35 1.97 -6 11 0 0.43 1.52 -5 11 0 1.43 1.61 -4 11 0 27.96 2.25 -3 11 0 125.08 3.77 -2 11 0 86.70 3.34 -1 11 0 64.35 2.95 0 11 0 10.36 1.45 1 11 0 0.98 1.29 2 11 0 3.93 1.52 3 11 0 4.71 1.59 4 11 0 8.99 1.96 5 11 0 30.72 3.15 6 11 0 27.09 2.52 -7 12 0 5.89 2.33 -6 12 0 5.00 2.15 -5 12 0 25.54 3.13 -4 12 0 28.83 2.40 -3 12 0 37.36 2.61 -2 12 0 94.48 3.57 -1 12 0 44.25 2.67 0 12 0 13.87 2.16 1 12 0 1.67 1.40 2 12 0 4.27 1.65 3 12 0 3.64 1.63 4 12 0 15.50 2.46 5 12 0 30.44 3.28 6 12 0 54.44 3.49 -6 13 0 3.25 2.17 -5 13 0 0.76 1.83 -4 13 0 55.63 3.29 -3 13 0 68.05 3.47 -2 13 0 43.33 2.78 -1 13 0 30.24 2.99 0 13 0 35.61 3.26 1 13 0 0.26 1.19 2 13 0 15.86 2.46 3 13 0 5.96 2.01 4 13 0 29.56 3.25 5 13 0 43.38 3.97 -5 14 0 22.76 3.31 -4 14 0 1.44 1.84 -3 14 0 49.28 3.11 -2 14 0 57.07 4.07 -1 14 0 11.80 2.24 0 14 0 4.41 1.82 1 14 0 3.44 1.79 2 14 0 1.09 1.61 3 14 0 47.44 4.58 -3 15 0 31.43 3.26 -2 15 0 21.80 2.79 -1 15 0 23.82 2.97 0 15 0 11.41 2.41 1 15 0 3.05 1.80 -2 -15 1 13.53 2.52 -1 -15 1 25.52 3.06 0 -15 1 13.37 2.31 1 -15 1 34.63 3.35 2 -15 1 11.32 2.24 3 -15 1 13.32 2.42 -4 -14 1 2.72 1.88 -3 -14 1 16.61 2.63 -2 -14 1 12.72 2.36 -1 -14 1 4.35 1.82 0 -14 1 24.71 2.86 1 -14 1 31.85 3.15 2 -14 1 6.31 1.95 3 -14 1 4.53 1.52 4 -14 1 1.32 1.91 5 -14 1 12.68 2.78 -5 -13 1 1.26 1.79 -4 -13 1 0.68 1.59 -3 -13 1 1.64 1.54 -2 -13 1 33.89 3.12 -1 -13 1 51.08 3.82 0 -13 1 12.78 2.17 1 -13 1 5.60 1.71 2 -13 1 60.94 3.23 3 -13 1 1.38 1.24 4 -13 1 0.42 1.43 5 -13 1 1.33 1.83 6 -13 1 15.04 2.75 -6 -12 1 10.39 2.26 -5 -12 1 2.66 1.85 -4 -12 1 22.74 2.72 -3 -12 1 28.92 2.96 -2 -12 1 4.47 1.60 -1 -12 1 55.95 3.67 0 -12 1 112.73 4.48 1 -12 1 35.52 2.42 2 -12 1 7.79 1.43 3 -12 1 4.36 1.32 4 -12 1 1.14 1.06 5 -12 1 14.89 2.57 6 -12 1 17.76 2.89 7 -12 1 37.76 4.06 -7 -11 1 48.95 4.05 -6 -11 1 0.97 1.60 -5 -11 1 1.47 1.51 -4 -11 1 1.07 1.37 -3 -11 1 39.79 3.18 -2 -11 1 89.40 4.23 -1 -11 1 71.48 3.66 0 -11 1 85.34 3.03 1 -11 1 96.82 3.15 2 -11 1 1.47 1.02 3 -11 1 5.03 1.30 4 -11 1 5.16 1.30 5 -11 1 9.11 2.10 6 -11 1 39.87 3.83 7 -11 1 46.39 4.30 -7 -10 1 13.67 2.03 -6 -10 1 6.08 1.87 -5 -10 1 3.48 1.58 -4 -10 1 33.89 2.90 -3 -10 1 83.65 4.29 -2 -10 1 62.77 3.66 -1 -10 1 206.88 5.51 0 -10 1 79.14 2.69 1 -10 1 1.23 0.92 2 -10 1 6.49 1.26 3 -10 1 1.99 1.06 4 -10 1 12.90 1.57 5 -10 1 32.10 3.28 6 -10 1 67.63 4.72 7 -10 1 59.80 4.75 8 -10 1 19.13 3.76 -8 -9 1 23.79 2.38 -7 -9 1 9.88 1.79 -6 -9 1 1.13 1.35 -5 -9 1 7.23 1.75 -4 -9 1 36.55 2.89 -3 -9 1 143.41 4.59 -2 -9 1 124.83 4.17 -1 -9 1 47.07 2.04 0 -9 1 66.44 2.50 1 -9 1 34.81 2.02 2 -9 1 0.49 0.83 3 -9 1 17.08 1.60 4 -9 1 18.64 1.67 5 -9 1 49.18 3.57 6 -9 1 107.43 5.99 7 -9 1 47.46 4.14 8 -9 1 41.25 5.03 -8 -8 1 78.31 3.83 -7 -8 1 11.19 1.72 -6 -8 1 0.29 1.07 -5 -8 1 10.23 1.83 -4 -8 1 4.13 1.36 -3 -8 1 44.82 2.84 -2 -8 1 210.83 5.20 -1 -8 1 98.20 2.49 0 -8 1 47.67 2.09 1 -8 1 2.63 0.90 2 -8 1 20.87 1.56 3 -8 1 0.01 0.73 4 -8 1 12.26 1.37 5 -8 1 71.73 4.18 6 -8 1 107.60 5.77 7 -8 1 48.09 4.55 8 -8 1 53.65 4.93 9 -8 1 24.70 4.05 -9 -7 1 60.53 5.99 -8 -7 1 9.45 2.22 -7 -7 1 5.37 1.48 -6 -7 1 11.70 1.76 -5 -7 1 0.54 1.09 -4 -7 1 75.74 4.29 -3 -7 1 36.88 2.57 -2 -7 1 127.88 3.83 -1 -7 1 329.10 5.08 0 -7 1 78.19 2.26 1 -7 1 95.62 2.55 2 -7 1 56.61 2.21 3 -7 1 1.74 0.83 4 -7 1 79.24 2.47 5 -7 1 44.83 3.77 6 -7 1 64.63 4.69 7 -7 1 84.72 6.79 8 -7 1 14.27 4.43 9 -7 1 17.26 4.94 -9 -6 1 27.83 4.45 -8 -6 1 40.65 4.70 -7 -6 1 10.63 1.66 -6 -6 1 1.93 1.16 -5 -6 1 4.21 1.29 -4 -6 1 20.47 1.91 -3 -6 1 219.74 4.99 -2 -6 1 317.58 6.87 -1 -6 1 103.88 2.44 0 -6 1 78.31 2.29 1 -6 1 164.74 3.45 2 -6 1 32.17 1.64 3 -6 1 3.70 0.85 4 -6 1 51.64 2.03 5 -6 1 79.38 5.65 6 -6 1 56.68 5.32 7 -6 1 29.22 4.64 8 -6 1 33.24 5.12 9 -6 1 36.38 5.57 -9 -5 1 12.12 3.18 -8 -5 1 1.40 2.03 -7 -5 1 4.20 1.82 -6 -5 1 29.71 2.45 -5 -5 1 85.76 3.74 -4 -5 1 95.43 3.74 -3 -5 1 29.92 2.35 -2 -5 1 274.00 7.98 -1 -5 1 148.22 2.76 0 -5 1 26.01 1.45 1 -5 1 39.64 1.78 2 -5 1 9.76 1.07 3 -5 1 135.65 3.93 4 -5 1 78.92 3.34 5 -5 1 86.73 3.11 6 -5 1 78.27 5.81 7 -5 1 58.54 8.14 8 -5 1 19.68 6.28 9 -5 1 21.56 6.75 10 -5 1 9.09 7.12 -10 -4 1 22.37 22.05 -9 -4 1 27.27 6.61 -8 -4 1 13.82 5.11 -7 -4 1 0.05 2.37 -6 -4 1 5.21 1.83 -5 -4 1 14.47 1.82 -4 -4 1 80.90 2.49 -3 -4 1 285.86 6.22 -2 -4 1 115.64 4.50 -1 -4 1 3.70 0.64 0 -4 1 131.37 2.61 1 -4 1 7.61 0.93 2 -4 1 48.38 1.72 3 -4 1 153.78 4.76 4 -4 1 86.48 3.69 5 -4 1 122.53 9.59 6 -4 1 82.67 8.48 7 -4 1 43.65 6.89 8 -4 1 67.88 8.90 9 -4 1 1.49 5.36 10 -4 1 5.89 6.45 -10 -3 1 46.53 8.18 -9 -3 1 1.96 3.30 -8 -3 1 1.51 3.37 -7 -3 1 19.85 2.93 -6 -3 1 6.96 1.76 -5 -3 1 198.74 5.09 -4 -3 1 112.17 3.96 -3 -3 1 114.82 2.24 -2 -3 1 277.05 5.58 -1 -3 1 78.28 1.73 0 -3 1 53.78 1.59 1 -3 1 44.02 1.49 2 -3 1 5.61 1.15 3 -3 1 323.02 9.65 4 -3 1 218.34 12.17 5 -3 1 127.81 6.51 6 -3 1 108.80 6.44 7 -3 1 33.99 4.21 8 -3 1 5.99 3.29 9 -3 1 0.03 3.06 10 -3 1 3.52 5.50 -10 -2 1 34.54 7.16 -9 -2 1 24.44 5.90 -8 -2 1 4.02 3.44 -7 -2 1 1.91 1.54 -6 -2 1 29.46 2.29 -5 -2 1 213.99 5.27 -4 -2 1 262.79 6.96 -3 -2 1 115.59 3.68 -2 -2 1 63.46 1.80 -1 -2 1 22.48 0.97 0 -2 1 1.22 0.46 1 -2 1 171.32 2.28 2 -2 1 497.00 6.14 3 -2 1 183.39 6.85 4 -2 1 87.41 4.84 5 -2 1 147.54 6.85 6 -2 1 92.93 5.78 7 -2 1 41.60 4.37 8 -2 1 1.06 2.76 9 -2 1 0.10 3.06 10 -2 1 2.87 3.51 -10 -1 1 24.22 6.15 -9 -1 1 17.07 5.27 -8 -1 1 0.16 2.41 -7 -1 1 2.91 2.42 -6 -1 1 52.45 2.89 -5 -1 1 43.39 2.41 -4 -1 1 98.45 2.96 -3 -1 1 163.49 4.35 -2 -1 1 52.05 1.95 -1 -1 1 36.22 1.27 0 -1 1 56.97 1.35 1 -1 1 0.85 0.21 2 -1 1 0.34 1.57 3 -1 1 1.49 1.92 4 -1 1 333.74 10.81 5 -1 1 135.18 6.36 6 -1 1 54.76 4.45 7 -1 1 31.64 3.89 8 -1 1 2.38 2.87 9 -1 1 6.21 3.41 10 -1 1 3.66 5.15 -10 0 1 25.23 6.36 -9 0 1 0.00 2.73 -8 0 1 2.22 2.52 -7 0 1 1.01 2.29 -6 0 1 48.60 2.68 -5 0 1 161.11 4.90 -4 0 1 118.81 3.75 -3 0 1 175.11 4.75 -2 0 1 468.99 10.06 -1 0 1 151.89 3.36 0 0 1 48.23 2.36 1 0 1 23.73 0.77 2 0 1 72.34 2.29 3 0 1 72.64 2.59 4 0 1 102.99 3.43 5 0 1 126.83 4.16 6 0 1 251.65 6.96 7 0 1 85.37 5.78 8 0 1 1.08 2.81 9 0 1 4.40 4.89 10 0 1 0.58 5.40 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5 3 1 124.11 4.43 6 3 1 34.97 2.75 7 3 1 29.29 5.82 8 3 1 5.68 5.05 9 3 1 1.47 2.42 -10 4 1 1.35 5.27 -9 4 1 0.13 4.76 -8 4 1 2.69 4.57 -7 4 1 3.82 4.25 -6 4 1 81.22 8.12 -5 4 1 72.20 3.33 -4 4 1 98.03 3.76 -3 4 1 311.55 8.14 -2 4 1 150.57 3.01 -1 4 1 0.75 0.69 0 4 1 96.20 2.27 1 4 1 1.88 0.73 2 4 1 0.76 0.88 3 4 1 196.70 4.04 4 4 1 145.35 2.83 5 4 1 71.27 2.83 6 4 1 82.50 4.45 7 4 1 0.11 1.53 8 4 1 0.00 1.92 9 4 1 0.00 1.86 -10 5 1 18.87 4.87 -9 5 1 0.42 3.20 -8 5 1 5.63 3.38 -7 5 1 10.18 3.46 -6 5 1 40.28 4.51 -5 5 1 216.75 6.89 -4 5 1 284.81 8.07 -3 5 1 174.00 4.61 -2 5 1 51.68 2.00 -1 5 1 1.67 0.78 0 5 1 45.65 1.80 1 5 1 54.07 1.77 2 5 1 153.04 3.31 3 5 1 110.16 3.49 4 5 1 72.27 2.74 5 5 1 134.76 4.10 6 5 1 76.41 3.59 7 5 1 0.83 1.69 8 5 1 1.56 2.15 9 5 1 0.19 2.14 -9 6 1 3.26 4.36 -8 6 1 24.74 4.71 -7 6 1 26.46 4.45 -6 6 1 93.91 6.49 -5 6 1 183.46 6.43 -4 6 1 119.70 3.98 -3 6 1 120.16 2.83 -2 6 1 59.15 2.09 -1 6 1 4.30 0.89 0 6 1 69.69 2.11 1 6 1 12.09 1.03 2 6 1 30.87 1.65 3 6 1 166.87 4.54 4 6 1 87.19 3.48 5 6 1 4.78 1.16 6 6 1 34.71 2.79 7 6 1 65.18 3.81 8 6 1 0.70 2.07 9 6 1 22.65 4.32 -9 7 1 0.00 4.24 -8 7 1 0.95 4.06 -7 7 1 53.95 4.52 -6 7 1 49.17 4.25 -5 7 1 58.95 2.59 -4 7 1 156.25 3.50 -3 7 1 52.92 2.24 -2 7 1 54.78 2.26 -1 7 1 1.26 0.80 0 7 1 0.43 0.70 1 7 1 83.99 2.32 2 7 1 63.58 1.94 3 7 1 45.54 2.90 4 7 1 57.27 3.40 5 7 1 153.96 4.45 6 7 1 85.13 4.33 7 7 1 0.62 1.36 8 7 1 1.02 2.03 -9 8 1 1.65 2.69 -8 8 1 6.46 2.89 -7 8 1 6.76 2.64 -6 8 1 38.67 4.14 -5 8 1 113.25 3.31 -4 8 1 84.82 2.86 -3 8 1 43.41 2.26 -2 8 1 47.51 2.30 -1 8 1 5.04 1.02 0 8 1 42.88 2.01 1 8 1 16.23 1.33 2 8 1 77.44 2.60 3 8 1 181.79 5.24 4 8 1 60.33 3.70 5 8 1 9.68 1.58 6 8 1 6.90 1.52 7 8 1 7.05 1.83 8 8 1 10.52 3.21 -8 9 1 25.86 4.08 -7 9 1 56.20 5.39 -6 9 1 35.82 3.57 -5 9 1 35.54 2.35 -4 9 1 76.42 3.02 -3 9 1 67.76 2.90 -2 9 1 4.50 1.09 -1 9 1 1.64 0.92 0 9 1 1.41 0.88 1 9 1 78.23 2.61 2 9 1 103.66 3.98 3 9 1 39.44 3.09 4 9 1 55.51 3.70 5 9 1 33.50 2.48 6 9 1 0.85 1.15 7 9 1 1.20 1.34 -8 10 1 12.98 3.71 -7 10 1 9.75 3.02 -6 10 1 62.71 4.69 -5 10 1 111.56 4.52 -4 10 1 33.28 2.35 -3 10 1 47.04 2.65 -2 10 1 43.12 2.51 -1 10 1 1.35 0.95 0 10 1 71.60 2.83 1 10 1 63.02 3.66 2 10 1 101.46 4.25 3 10 1 132.99 5.65 4 10 1 32.17 3.05 5 10 1 23.32 2.25 6 10 1 5.85 1.61 7 10 1 1.05 1.42 -7 11 1 31.79 3.74 -6 11 1 20.23 2.99 -5 11 1 39.06 3.67 -4 11 1 49.96 2.93 -3 11 1 35.99 2.46 -2 11 1 2.60 1.15 -1 11 1 18.98 1.84 0 11 1 31.79 2.19 1 11 1 50.94 3.48 2 11 1 60.74 3.89 3 11 1 90.03 4.90 4 11 1 35.29 3.35 5 11 1 7.26 1.74 6 11 1 1.76 1.49 -7 12 1 16.49 3.01 -6 12 1 24.08 3.23 -5 12 1 84.58 5.27 -4 12 1 34.07 2.60 -3 12 1 0.38 1.13 -2 12 1 10.24 1.62 -1 12 1 5.32 1.31 0 12 1 27.63 2.82 1 12 1 85.07 4.80 2 12 1 37.09 3.18 3 12 1 26.59 3.02 4 12 1 61.14 5.20 5 12 1 7.52 1.68 -6 13 1 50.70 4.59 -5 13 1 32.61 3.67 -4 13 1 7.42 1.64 -3 13 1 12.01 1.78 -2 13 1 0.25 1.11 -1 13 1 21.59 2.65 0 13 1 18.39 2.49 1 13 1 27.53 2.96 2 13 1 89.99 5.86 3 13 1 36.76 3.53 4 13 1 4.64 2.04 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3.00 -6 -8 2 58.54 3.74 -5 -8 2 72.48 4.52 -4 -8 2 59.59 3.41 -3 -8 2 44.84 2.87 -2 -8 2 18.86 1.37 -1 -8 2 4.45 0.86 0 -8 2 43.40 2.02 1 -8 2 103.12 3.06 2 -8 2 50.44 2.24 3 -8 2 60.24 2.40 4 -8 2 150.98 3.47 5 -8 2 54.50 3.63 6 -8 2 2.29 1.56 7 -8 2 1.23 1.96 8 -8 2 0.51 1.62 9 -8 2 8.24 2.44 -9 -7 2 2.23 1.94 -8 -7 2 12.72 1.80 -7 -7 2 21.71 2.30 -6 -7 2 29.13 2.61 -5 -7 2 39.74 2.79 -4 -7 2 195.40 5.08 -3 -7 2 112.59 3.70 -2 -7 2 4.49 1.15 -1 -7 2 7.71 0.92 0 -7 2 6.45 0.95 1 -7 2 71.85 2.27 2 -7 2 125.07 2.90 3 -7 2 86.17 2.47 4 -7 2 127.44 2.96 5 -7 2 55.77 3.95 6 -7 2 26.41 3.22 7 -7 2 1.57 2.00 8 -7 2 6.44 2.72 9 -7 2 1.61 4.32 -9 -6 2 0.12 1.97 -8 -6 2 18.91 2.22 -7 -6 2 53.37 2.99 -6 -6 2 21.59 2.17 -5 -6 2 138.43 4.31 -4 -6 2 94.55 3.89 -3 -6 2 31.71 2.62 -2 -6 2 63.39 2.74 -1 -6 2 12.06 1.09 0 -6 2 42.06 1.92 1 -6 2 37.65 1.89 2 -6 2 114.65 2.85 3 -6 2 337.65 4.94 4 -6 2 128.60 3.24 5 -6 2 8.01 3.02 6 -6 2 13.72 3.68 7 -6 2 3.33 3.38 8 -6 2 6.52 4.05 9 -6 2 16.12 4.67 -9 -5 2 1.05 2.39 -8 -5 2 14.02 5.38 -7 -5 2 66.25 4.12 -6 -5 2 18.82 3.22 -5 -5 2 56.50 3.43 -4 -5 2 150.77 4.64 -3 -5 2 4.47 1.34 -2 -5 2 0.10 0.96 -1 -5 2 2.63 0.73 0 -5 2 2.67 0.81 1 -5 2 193.94 3.73 2 -5 2 286.08 5.05 3 -5 2 19.70 1.52 4 -5 2 95.94 2.38 5 -5 2 105.42 6.24 6 -5 2 4.99 4.65 7 -5 2 2.93 4.86 8 -5 2 2.75 5.37 9 -5 2 19.62 6.69 -10 -4 2 11.01 6.47 -9 -4 2 9.35 5.59 -8 -4 2 47.12 7.21 -7 -4 2 21.09 2.55 -6 -4 2 83.08 5.36 -5 -4 2 29.28 2.30 -4 -4 2 24.92 2.18 -3 -4 2 18.13 1.81 -2 -4 2 19.08 1.14 -1 -4 2 40.89 1.44 0 -4 2 27.68 1.40 1 -4 2 2.27 0.78 2 -4 2 217.28 3.28 3 -4 2 222.87 4.76 4 -4 2 10.78 4.30 5 -4 2 6.25 4.07 6 -4 2 55.14 7.29 7 -4 2 2.53 4.56 8 -4 2 106.69 10.97 9 -4 2 48.17 8.47 10 -4 2 22.55 7.58 -10 -3 2 4.27 5.31 -9 -3 2 7.38 5.10 -8 -3 2 23.39 5.43 -7 -3 2 95.25 5.40 -6 -3 2 71.89 3.05 -5 -3 2 58.85 3.06 -4 -3 2 76.89 3.07 -3 -3 2 44.76 1.80 -2 -3 2 21.80 1.25 -1 -3 2 5.84 0.89 0 -3 2 68.14 1.70 1 -3 2 57.76 1.47 2 -3 2 330.27 4.86 3 -3 2 88.41 3.46 4 -3 2 72.04 4.67 5 -3 2 111.53 6.20 6 -3 2 29.63 3.90 7 -3 2 1.80 2.76 8 -3 2 4.91 3.36 9 -3 2 56.75 6.01 10 -3 2 55.60 6.35 -10 -2 2 0.27 4.09 -9 -2 2 29.06 5.85 -8 -2 2 32.79 5.69 -7 -2 2 108.73 4.54 -6 -2 2 204.30 5.44 -5 -2 2 114.14 4.33 -4 -2 2 34.32 2.12 -3 -2 2 20.72 1.66 -2 -2 2 1.02 0.77 -1 -2 2 0.87 0.62 0 -2 2 55.82 1.35 1 -2 2 341.82 4.59 2 -2 2 1000.00 8.77 3 -2 2 238.25 5.71 4 -2 2 3.09 2.11 5 -2 2 77.75 5.02 6 -2 2 7.02 2.73 7 -2 2 4.01 2.80 8 -2 2 43.80 4.88 9 -2 2 65.42 6.22 10 -2 2 18.13 4.55 -10 -1 2 0.04 4.30 -9 -1 2 21.60 5.33 -8 -1 2 48.33 4.59 -7 -1 2 79.31 3.79 -6 -1 2 153.56 5.15 -5 -1 2 124.05 3.71 -4 -1 2 5.63 1.33 -3 -1 2 145.82 5.32 -2 -1 2 19.77 1.97 -1 -1 2 206.60 2.83 0 -1 2 334.57 5.40 1 -1 2 271.79 3.38 2 -1 2 26.94 0.76 3 -1 2 192.24 4.90 4 -1 2 82.41 4.68 5 -1 2 6.60 2.49 6 -1 2 1.14 2.36 7 -1 2 3.03 2.72 8 -1 2 11.57 3.52 9 -1 2 50.93 5.62 10 -1 2 24.20 6.99 -10 0 2 1.49 4.02 -9 0 2 21.40 3.78 -8 0 2 98.88 6.39 -7 0 2 32.53 3.63 -6 0 2 163.06 5.31 -5 0 2 132.18 3.76 -4 0 2 73.32 3.07 -3 0 2 0.91 1.26 -2 0 2 186.62 4.53 -1 0 2 6.23 0.58 0 0 2 163.89 2.49 1 0 2 101.80 1.72 2 0 2 39.89 1.24 3 0 2 9.57 1.33 4 0 2 134.96 4.13 5 0 2 52.91 2.58 6 0 2 0.58 2.35 7 0 2 4.67 2.82 8 0 2 10.08 3.47 9 0 2 72.24 9.24 10 0 2 27.10 7.16 -10 1 2 14.06 5.19 -9 1 2 9.65 3.04 -8 1 2 96.30 6.42 -7 1 2 72.15 5.19 -6 1 2 123.66 4.50 -5 1 2 11.22 2.26 -4 1 2 43.33 2.30 -3 1 2 9.89 1.17 -2 1 2 102.87 4.18 -1 1 2 36.28 1.22 0 1 2 296.06 3.81 1 1 2 289.75 4.51 2 1 2 101.03 2.38 3 1 2 82.26 3.02 4 1 2 33.99 2.22 5 1 2 5.47 1.60 6 1 2 0.52 1.49 7 1 2 31.47 4.16 8 1 2 38.88 4.78 9 1 2 61.97 8.80 10 1 2 51.55 8.84 -10 2 2 0.65 4.30 -9 2 2 21.02 5.75 -8 2 2 162.32 8.55 -7 2 2 119.35 6.83 -6 2 2 61.07 4.56 -5 2 2 144.18 5.61 -4 2 2 0.82 1.23 -3 2 2 13.80 1.93 -2 2 2 0.80 1.15 -1 2 2 22.46 1.16 0 2 2 281.18 4.25 1 2 2 947.10 12.82 2 2 2 1.77 0.83 3 2 2 45.27 1.91 4 2 2 119.22 4.15 5 2 2 8.13 1.83 6 2 2 28.17 2.58 7 2 2 0.63 2.72 8 2 2 51.99 7.83 9 2 2 92.16 10.73 10 2 2 43.96 21.73 -10 3 2 35.27 7.51 -9 3 2 57.97 8.31 -8 3 2 79.15 8.86 -7 3 2 249.17 15.12 -6 3 2 57.63 3.65 -5 3 2 29.77 2.70 -4 3 2 65.60 2.98 -3 3 2 10.02 1.62 -2 3 2 125.06 2.61 -1 3 2 98.91 2.34 0 3 2 1.87 0.71 1 3 2 997.14 10.54 2 3 2 238.74 4.56 3 3 2 27.13 1.75 4 3 2 1.06 0.95 5 3 2 5.53 1.83 6 3 2 1.68 2.34 7 3 2 96.42 9.80 8 3 2 15.19 3.38 9 3 2 23.96 4.17 -10 4 2 13.00 4.35 -9 4 2 24.15 6.34 -8 4 2 51.14 7.59 -7 4 2 147.82 8.11 -6 4 2 50.46 3.15 -5 4 2 81.57 3.65 -4 4 2 5.93 1.56 -3 4 2 25.13 1.81 -2 4 2 11.43 1.10 -1 4 2 225.09 4.00 0 4 2 141.29 3.13 1 4 2 358.22 6.17 2 4 2 180.85 3.22 3 4 2 205.73 4.50 4 4 2 13.77 1.15 5 4 2 44.59 2.06 6 4 2 4.63 2.03 7 4 2 17.23 3.35 8 4 2 53.72 5.51 9 4 2 49.80 5.77 -10 5 2 16.89 5.26 -9 5 2 15.81 4.35 -8 5 2 48.97 5.47 -7 5 2 79.92 6.25 -6 5 2 52.43 4.85 -5 5 2 16.22 2.15 -4 5 2 7.44 1.80 -3 5 2 0.82 1.02 -2 5 2 151.97 3.29 -1 5 2 139.23 3.09 0 5 2 449.09 5.85 1 5 2 385.07 6.41 2 5 2 330.64 4.35 3 5 2 2.01 0.68 4 5 2 4.88 0.89 5 5 2 0.18 0.92 6 5 2 72.32 3.48 7 5 2 60.17 3.56 8 5 2 77.18 6.47 9 5 2 13.48 3.55 -9 6 2 30.31 5.81 -8 6 2 61.02 6.90 -7 6 2 88.55 6.74 -6 6 2 40.70 4.64 -5 6 2 5.92 1.50 -4 6 2 8.60 1.39 -3 6 2 1.12 0.74 -2 6 2 114.53 2.77 -1 6 2 254.96 4.25 0 6 2 130.08 2.84 1 6 2 15.54 1.33 2 6 2 202.98 3.54 3 6 2 15.64 1.34 4 6 2 7.81 1.26 5 6 2 17.83 2.09 6 6 2 16.82 2.19 7 6 2 43.91 3.25 8 6 2 60.97 6.11 9 6 2 41.52 24.08 -9 7 2 71.53 6.23 -8 7 2 21.98 3.61 -7 7 2 101.91 6.19 -6 7 2 40.11 4.05 -5 7 2 3.02 1.04 -4 7 2 0.46 0.79 -3 7 2 8.57 1.18 -2 7 2 4.09 0.96 -1 7 2 83.55 2.52 0 7 2 186.89 3.67 1 7 2 65.76 2.18 2 7 2 61.00 2.17 3 7 2 39.28 2.53 4 7 2 1.24 0.98 5 7 2 6.44 1.66 6 7 2 19.29 2.16 7 7 2 21.68 2.55 8 7 2 31.04 4.83 -9 8 2 24.81 4.14 -8 8 2 82.33 6.43 -7 8 2 82.52 6.21 -6 8 2 9.88 2.73 -5 8 2 1.39 0.99 -4 8 2 19.66 1.75 -3 8 2 38.00 2.13 -2 8 2 50.15 2.28 -1 8 2 11.99 1.32 0 8 2 41.46 2.11 1 8 2 134.10 3.12 2 8 2 53.10 2.56 3 8 2 3.51 1.25 4 8 2 1.30 1.08 5 8 2 5.81 1.42 6 8 2 26.22 2.82 7 8 2 19.22 2.56 8 8 2 4.91 2.93 -8 9 2 35.63 4.69 -7 9 2 8.27 2.95 -6 9 2 33.59 3.52 -5 9 2 0.68 1.02 -4 9 2 8.59 1.39 -3 9 2 1.07 0.97 -2 9 2 1.60 0.93 -1 9 2 129.58 3.40 0 9 2 79.84 2.71 1 9 2 8.45 1.18 2 9 2 57.69 3.66 3 9 2 45.60 3.39 4 9 2 11.46 1.68 5 9 2 20.75 2.09 6 9 2 12.05 1.90 7 9 2 22.18 2.77 -8 10 2 43.79 4.55 -7 10 2 9.60 3.18 -6 10 2 5.48 2.08 -5 10 2 4.92 1.35 -4 10 2 1.04 1.06 -3 10 2 106.91 3.50 -2 10 2 148.11 3.99 -1 10 2 2.03 1.03 0 10 2 148.09 3.71 1 10 2 128.96 4.54 2 10 2 4.25 1.56 3 10 2 1.07 1.38 4 10 2 0.91 1.20 5 10 2 4.32 1.42 6 10 2 78.34 3.89 7 10 2 15.09 2.60 -7 11 2 8.33 2.51 -6 11 2 1.59 1.70 -5 11 2 9.06 1.91 -4 11 2 38.51 2.65 -3 11 2 27.75 2.25 -2 11 2 63.95 3.18 -1 11 2 90.54 3.43 0 11 2 22.81 2.28 1 11 2 22.15 2.51 2 11 2 42.60 3.46 3 11 2 2.09 1.45 4 11 2 15.88 1.97 5 11 2 24.68 2.39 6 11 2 21.72 2.41 -6 12 2 9.41 2.50 -5 12 2 9.42 2.31 -4 12 2 23.24 2.27 -3 12 2 41.81 2.79 -2 12 2 19.09 2.00 -1 12 2 46.33 2.80 0 12 2 39.21 3.35 1 12 2 48.12 3.77 2 12 2 3.54 1.68 3 12 2 1.03 1.49 4 12 2 0.95 1.30 5 12 2 23.11 2.47 -6 13 2 9.32 3.73 -5 13 2 1.01 1.81 -4 13 2 6.69 1.69 -3 13 2 19.82 2.13 -2 13 2 71.89 3.64 -1 13 2 20.22 2.61 0 13 2 29.34 3.06 1 13 2 46.34 3.80 2 13 2 2.69 1.65 3 13 2 2.46 1.73 4 13 2 6.64 2.10 -4 14 2 3.59 1.47 -3 14 2 7.08 1.73 -2 14 2 55.19 4.13 -1 14 2 67.27 4.57 0 14 2 16.26 2.59 1 14 2 14.09 2.46 2 14 2 5.81 1.97 3 14 2 2.77 1.89 -2 15 2 15.52 2.61 -1 15 2 23.66 3.05 0 15 2 73.32 5.00 -2 -15 3 0.31 1.36 -1 -15 3 6.68 2.01 0 -15 3 25.48 2.89 1 -15 3 53.99 4.01 2 -15 3 15.52 2.43 3 -15 3 12.12 2.50 -4 -14 3 2.47 1.80 -3 -14 3 6.49 2.04 -2 -14 3 10.38 2.10 -1 -14 3 32.55 3.04 0 -14 3 17.39 2.45 1 -14 3 34.87 3.17 2 -14 3 74.36 3.92 3 -14 3 20.73 2.17 4 -14 3 0.42 1.78 5 -14 3 0.36 1.85 -5 -13 3 9.21 2.30 -4 -13 3 1.77 1.73 -3 -13 3 1.09 1.49 -2 -13 3 2.02 1.50 -1 -13 3 21.98 2.54 0 -13 3 45.97 3.31 1 -13 3 22.65 2.49 2 -13 3 81.33 3.64 3 -13 3 7.20 1.54 4 -13 3 7.77 2.13 5 -13 3 0.31 1.72 6 -13 3 1.93 2.04 -6 -12 3 29.41 3.28 -5 -12 3 26.11 2.98 -4 -12 3 2.51 1.67 -3 -12 3 4.13 1.61 -2 -12 3 2.66 1.47 -1 -12 3 57.55 3.70 0 -12 3 171.26 5.30 1 -12 3 63.32 3.00 2 -12 3 32.96 2.30 3 -12 3 7.53 1.48 4 -12 3 5.14 1.85 5 -12 3 0.35 1.44 6 -12 3 9.15 2.42 7 -12 3 15.49 2.90 -7 -11 3 18.45 2.65 -6 -11 3 16.07 2.45 -5 -11 3 0.77 1.40 -4 -11 3 0.58 1.33 -3 -11 3 0.60 1.26 -2 -11 3 108.94 4.35 -1 -11 3 154.11 5.60 0 -11 3 20.95 1.75 1 -11 3 22.42 1.85 2 -11 3 50.09 2.62 3 -11 3 7.74 1.40 4 -11 3 1.55 1.45 5 -11 3 0.90 1.39 6 -11 3 3.75 1.97 7 -11 3 49.38 4.39 -7 -10 3 6.68 1.96 -6 -10 3 32.43 3.13 -5 -10 3 13.99 2.17 -4 -10 3 0.75 1.19 -3 -10 3 2.93 1.34 -2 -10 3 2.50 1.32 -1 -10 3 14.22 1.39 0 -10 3 191.75 4.05 1 -10 3 99.06 3.04 2 -10 3 0.21 0.88 3 -10 3 40.27 2.31 4 -10 3 13.75 1.56 5 -10 3 5.80 1.83 6 -10 3 23.81 2.89 7 -10 3 24.87 3.15 8 -10 3 33.73 3.81 -8 -9 3 67.18 3.56 -7 -9 3 73.22 5.18 -6 -9 3 11.48 2.01 -5 -9 3 8.91 1.80 -4 -9 3 30.03 2.63 -3 -9 3 5.00 1.47 -2 -9 3 91.59 3.57 -1 -9 3 49.03 2.09 0 -9 3 20.75 1.58 1 -9 3 194.78 3.99 2 -9 3 126.69 3.24 3 -9 3 25.79 1.81 4 -9 3 0.13 0.85 5 -9 3 1.67 1.48 6 -9 3 30.58 3.08 7 -9 3 43.23 3.82 8 -9 3 20.93 3.05 -8 -8 3 28.14 2.42 -7 -8 3 24.27 2.64 -6 -8 3 83.05 4.93 -5 -8 3 1.97 1.32 -4 -8 3 1.09 1.11 -3 -8 3 0.39 0.96 -2 -8 3 13.93 1.09 -1 -8 3 43.33 1.90 0 -8 3 299.55 4.83 1 -8 3 73.02 2.48 2 -8 3 55.32 2.34 3 -8 3 68.52 2.48 4 -8 3 10.50 1.26 5 -8 3 47.47 3.40 6 -8 3 20.45 2.58 7 -8 3 12.36 2.31 8 -8 3 43.93 3.84 9 -8 3 12.54 2.69 -9 -7 3 16.65 2.78 -8 -7 3 47.40 2.89 -7 -7 3 58.14 3.70 -6 -7 3 20.11 2.25 -5 -7 3 11.43 1.73 -4 -7 3 3.27 1.22 -3 -7 3 50.14 2.83 -2 -7 3 197.35 3.33 -1 -7 3 69.95 2.15 0 -7 3 136.50 2.97 1 -7 3 198.07 3.69 2 -7 3 103.70 2.66 3 -7 3 18.06 1.40 4 -7 3 1.99 0.79 5 -7 3 9.74 1.76 6 -7 3 40.00 3.74 7 -7 3 86.21 5.80 8 -7 3 54.81 4.87 9 -7 3 20.82 3.74 -9 -6 3 21.58 3.65 -8 -6 3 63.13 3.93 -7 -6 3 79.03 4.82 -6 -6 3 0.88 1.13 -5 -6 3 5.75 1.34 -4 -6 3 46.21 3.09 -3 -6 3 65.48 3.54 -2 -6 3 124.38 2.88 -1 -6 3 359.62 4.88 0 -6 3 172.48 3.55 1 -6 3 115.60 2.61 2 -6 3 46.10 1.89 3 -6 3 15.29 1.23 4 -6 3 23.34 1.36 5 -6 3 54.90 3.84 6 -6 3 59.98 4.37 7 -6 3 57.44 5.77 8 -6 3 38.65 5.37 9 -6 3 38.23 4.34 -9 -5 3 50.32 7.84 -8 -5 3 44.16 3.67 -7 -5 3 31.36 3.94 -6 -5 3 28.21 3.65 -5 -5 3 0.49 0.93 -4 -5 3 75.13 2.31 -3 -5 3 100.66 3.67 -2 -5 3 100.92 2.26 -1 -5 3 377.90 6.13 0 -5 3 173.31 3.33 1 -5 3 18.86 1.37 2 -5 3 30.96 1.50 3 -5 3 61.38 1.89 4 -5 3 31.17 1.34 5 -5 3 58.50 7.41 6 -5 3 23.90 6.01 7 -5 3 166.03 13.46 8 -5 3 95.36 10.93 9 -5 3 30.01 4.75 -10 -4 3 16.33 5.93 -9 -4 3 48.94 7.60 -8 -4 3 145.63 11.78 -7 -4 3 33.97 2.96 -6 -4 3 4.68 2.31 -5 -4 3 0.63 1.75 -4 -4 3 12.27 1.29 -3 -4 3 207.19 4.47 -2 -4 3 121.99 3.05 -1 -4 3 69.14 1.87 0 -4 3 58.93 1.80 1 -4 3 150.52 2.57 2 -4 3 23.20 1.20 3 -4 3 8.33 0.89 4 -4 3 12.25 1.88 5 -4 3 53.39 6.96 6 -4 3 118.82 7.12 7 -4 3 91.42 6.59 8 -4 3 40.81 7.62 9 -4 3 30.94 7.53 -10 -3 3 74.30 9.61 -9 -3 3 63.76 8.37 -8 -3 3 36.27 6.17 -7 -3 3 54.97 3.46 -6 -3 3 53.16 3.20 -5 -3 3 20.07 1.98 -4 -3 3 18.00 1.77 -3 -3 3 11.58 1.17 -2 -3 3 39.72 1.88 -1 -3 3 320.45 5.53 0 -3 3 93.46 2.09 1 -3 3 118.07 2.07 2 -3 3 217.63 3.30 3 -3 3 41.85 2.60 4 -3 3 4.02 1.31 5 -3 3 7.47 2.79 6 -3 3 47.79 4.72 7 -3 3 54.14 5.25 8 -3 3 52.30 5.48 9 -3 3 10.66 3.92 10 -3 3 13.45 6.75 -10 -2 3 22.63 5.68 -9 -2 3 86.91 9.41 -8 -2 3 65.14 7.59 -7 -2 3 6.53 1.71 -6 -2 3 3.13 1.25 -5 -2 3 41.37 2.54 -4 -2 3 43.61 2.40 -3 -2 3 179.86 4.93 -2 -2 3 93.42 2.30 -1 -2 3 219.64 3.15 0 -2 3 309.62 3.57 1 -2 3 762.86 8.67 2 -2 3 84.56 1.78 3 -2 3 6.50 1.39 4 -2 3 0.51 1.12 5 -2 3 25.60 3.44 6 -2 3 90.85 5.89 7 -2 3 86.85 6.17 8 -2 3 68.90 6.01 9 -2 3 51.83 5.71 10 -2 3 4.23 4.24 -10 -1 3 36.81 6.99 -9 -1 3 57.45 7.77 -8 -1 3 5.24 2.62 -7 -1 3 73.46 3.70 -6 -1 3 13.84 1.55 -5 -1 3 16.68 1.87 -4 -1 3 151.72 6.63 -3 -1 3 40.73 2.23 -2 -1 3 861.82 10.42 -1 -1 3 988.24 10.85 0 -1 3 1.53 0.71 1 -1 3 146.47 2.33 2 -1 3 21.94 1.00 3 -1 3 5.81 0.62 4 -1 3 68.55 3.28 5 -1 3 58.27 4.54 6 -1 3 117.61 6.62 7 -1 3 94.91 6.43 8 -1 3 56.70 5.47 9 -1 3 31.34 4.93 10 -1 3 2.55 5.79 -10 0 3 37.74 7.05 -9 0 3 42.63 4.67 -8 0 3 11.86 2.85 -7 0 3 9.85 1.66 -6 0 3 20.03 1.67 -5 0 3 3.86 1.44 -4 0 3 176.98 5.43 -3 0 3 401.39 8.90 -2 0 3 89.43 2.35 -1 0 3 18.71 1.08 0 0 3 146.53 2.83 1 0 3 15.41 0.88 2 0 3 14.23 0.94 3 0 3 3.91 0.70 4 0 3 49.44 2.42 5 0 3 125.47 2.78 6 0 3 137.67 7.16 7 0 3 80.63 5.99 8 0 3 20.35 4.09 9 0 3 17.68 6.19 10 0 3 12.00 16.37 -10 1 3 19.93 3.85 -9 1 3 29.94 4.02 -8 1 3 16.01 3.20 -7 1 3 0.45 1.18 -6 1 3 5.42 2.26 -5 1 3 5.92 1.53 -4 1 3 107.68 3.19 -3 1 3 275.45 9.05 -2 1 3 251.66 4.40 -1 1 3 104.37 2.63 0 1 3 11.56 1.02 1 1 3 17.69 1.05 2 1 3 1.15 0.63 3 1 3 90.02 2.48 4 1 3 99.67 3.67 5 1 3 176.13 5.45 6 1 3 55.61 4.79 7 1 3 31.11 4.36 8 1 3 64.15 8.77 9 1 3 0.00 5.00 -10 2 3 43.81 7.62 -9 2 3 8.23 2.96 -8 2 3 6.80 2.68 -7 2 3 7.74 2.56 -6 2 3 0.13 1.37 -5 2 3 102.18 3.98 -4 2 3 61.66 3.49 -3 2 3 66.79 2.80 -2 2 3 168.99 2.88 -1 2 3 66.75 1.93 0 2 3 28.91 1.34 1 2 3 59.69 2.06 2 2 3 32.39 1.74 3 2 3 151.23 3.48 4 2 3 27.18 1.80 5 2 3 121.07 4.53 6 2 3 115.46 4.66 7 2 3 30.09 4.28 8 2 3 9.04 5.45 9 2 3 8.63 6.05 -10 3 3 32.28 7.17 -9 3 3 71.69 8.96 -8 3 3 20.97 5.47 -7 3 3 2.42 3.75 -6 3 3 0.58 1.89 -5 3 3 3.36 1.60 -4 3 3 104.94 3.95 -3 3 3 329.63 8.05 -2 3 3 66.75 2.13 -1 3 3 235.65 4.05 0 3 3 140.18 3.42 1 3 3 3.62 1.00 2 3 3 133.49 3.30 3 3 3 6.55 1.17 4 3 3 109.30 3.25 5 3 3 127.88 3.62 6 3 3 20.23 1.79 7 3 3 60.95 5.54 8 3 3 16.64 3.57 9 3 3 2.41 2.63 -10 4 3 34.44 5.93 -9 4 3 20.46 4.32 -8 4 3 16.11 3.81 -7 4 3 32.95 4.30 -6 4 3 36.47 2.89 -5 4 3 153.28 5.37 -4 4 3 81.00 3.59 -3 4 3 173.39 4.39 -2 4 3 319.59 5.27 -1 4 3 142.66 3.16 0 4 3 59.01 1.76 1 4 3 95.31 2.42 2 4 3 4.32 0.89 3 4 3 9.94 1.22 4 4 3 57.68 2.16 5 4 3 102.28 2.80 6 4 3 104.08 3.71 7 4 3 20.09 3.62 8 4 3 14.79 3.54 9 4 3 11.07 3.38 -10 5 3 22.41 5.65 -9 5 3 28.39 5.57 -8 5 3 3.54 3.40 -7 5 3 4.49 3.20 -6 5 3 1.59 1.86 -5 5 3 57.16 3.37 -4 5 3 160.23 5.47 -3 5 3 52.42 2.15 -2 5 3 168.10 3.64 -1 5 3 240.82 4.08 0 5 3 140.98 2.61 1 5 3 0.54 0.56 2 5 3 0.20 0.57 3 5 3 2.50 0.78 4 5 3 86.54 2.48 5 5 3 76.03 3.54 6 5 3 128.51 4.37 7 5 3 118.35 7.99 8 5 3 36.60 4.91 9 5 3 0.87 2.56 -9 6 3 19.75 5.21 -8 6 3 11.43 4.47 -7 6 3 2.98 3.70 -6 6 3 12.81 2.11 -5 6 3 11.59 1.84 -4 6 3 19.18 1.52 -3 6 3 159.61 3.58 -2 6 3 263.11 4.58 -1 6 3 27.27 1.58 0 6 3 6.42 0.97 1 6 3 2.62 0.77 2 6 3 0.61 0.60 3 6 3 19.06 1.23 4 6 3 100.47 3.30 5 6 3 178.98 5.15 6 6 3 180.61 5.40 7 6 3 45.05 3.89 8 6 3 1.39 2.49 -9 7 3 19.26 3.83 -8 7 3 2.86 2.51 -7 7 3 1.19 2.09 -6 7 3 5.14 1.69 -5 7 3 31.91 2.14 -4 7 3 59.52 2.75 -3 7 3 73.79 2.73 -2 7 3 131.66 3.33 -1 7 3 82.88 2.39 0 7 3 36.85 2.01 1 7 3 12.92 1.19 2 7 3 2.82 0.77 3 7 3 22.13 1.75 4 7 3 74.30 3.19 5 7 3 89.86 4.29 6 7 3 40.35 3.27 7 7 3 24.12 2.74 8 7 3 4.18 2.80 -9 8 3 12.74 3.42 -8 8 3 0.92 2.43 -7 8 3 23.75 3.91 -6 8 3 7.73 2.62 -5 8 3 14.59 1.66 -4 8 3 114.78 3.43 -3 8 3 84.64 2.97 -2 8 3 64.57 2.84 -1 8 3 70.27 2.44 0 8 3 0.49 0.79 1 8 3 0.62 0.90 2 8 3 1.13 0.83 3 8 3 46.40 2.56 4 8 3 61.15 3.03 5 8 3 35.20 2.75 6 8 3 29.79 3.00 7 8 3 64.60 4.31 -8 9 3 2.05 2.69 -7 9 3 0.84 2.07 -6 9 3 38.16 3.71 -5 9 3 15.62 1.78 -4 9 3 35.68 2.37 -3 9 3 139.12 3.82 -2 9 3 83.30 3.13 -1 9 3 18.91 1.74 0 9 3 1.99 0.99 1 9 3 6.59 1.33 2 9 3 37.87 2.65 3 9 3 10.16 1.53 4 9 3 51.92 2.95 5 9 3 65.86 3.69 6 9 3 17.36 2.58 7 9 3 0.80 1.65 -8 10 3 3.31 2.24 -7 10 3 4.71 2.24 -6 10 3 5.81 2.08 -5 10 3 72.55 3.54 -4 10 3 165.59 4.43 -3 10 3 98.64 3.61 -2 10 3 16.54 1.81 -1 10 3 5.57 1.27 0 10 3 0.78 1.00 1 10 3 8.05 1.77 2 10 3 11.09 1.83 3 10 3 46.38 2.74 4 10 3 53.28 3.07 5 10 3 8.88 1.86 6 10 3 24.93 3.03 -7 11 3 22.80 3.28 -6 11 3 51.88 4.40 -5 11 3 44.92 2.95 -4 11 3 82.77 3.70 -3 11 3 57.72 3.14 -2 11 3 0.81 1.06 -1 11 3 14.01 1.73 0 11 3 0.49 1.24 1 11 3 22.84 2.72 2 11 3 42.52 3.59 3 11 3 47.51 3.30 4 11 3 47.24 3.05 5 11 3 46.36 3.42 6 11 3 6.25 2.15 -6 12 3 23.79 3.31 -5 12 3 74.50 4.45 -4 12 3 41.64 2.89 -3 12 3 11.08 1.72 -2 12 3 27.57 2.33 -1 12 3 1.20 1.17 0 12 3 0.88 1.28 1 12 3 21.13 2.73 2 12 3 23.22 2.90 3 12 3 52.35 4.08 4 12 3 33.62 3.57 5 12 3 22.98 3.11 -5 13 3 30.36 3.74 -4 13 3 73.46 3.87 -3 13 3 20.40 2.17 -2 13 3 10.86 1.75 -1 13 3 4.79 1.74 0 13 3 0.41 1.29 1 13 3 4.49 1.79 2 13 3 24.64 2.99 3 13 3 41.45 3.85 4 13 3 42.09 4.00 -4 14 3 40.47 3.09 -3 14 3 18.08 2.23 -2 14 3 25.02 3.09 -1 14 3 12.68 2.46 0 14 3 2.89 1.70 1 14 3 22.83 2.91 2 14 3 24.02 3.16 -2 -15 4 16.24 2.49 -1 -15 4 22.03 2.70 0 -15 4 18.37 2.52 1 -15 4 10.83 2.19 2 -15 4 0.56 1.43 3 -15 4 2.15 2.25 -4 -14 4 12.24 2.48 -3 -14 4 35.75 3.36 -2 -14 4 27.30 2.99 -1 -14 4 9.51 2.03 0 -14 4 37.48 3.20 1 -14 4 21.51 2.58 2 -14 4 9.05 1.78 3 -14 4 2.33 1.60 4 -14 4 22.03 3.05 5 -14 4 17.60 2.97 -5 -13 4 7.29 2.04 -4 -13 4 15.30 2.47 -3 -13 4 15.41 2.37 -2 -13 4 48.16 3.69 -1 -13 4 53.83 3.65 0 -13 4 30.96 2.85 1 -13 4 26.76 2.34 2 -13 4 5.89 1.43 3 -13 4 23.47 2.15 4 -13 4 23.06 2.94 5 -13 4 24.76 3.14 6 -13 4 52.55 4.42 -6 -12 4 0.92 1.60 -5 -12 4 15.67 2.47 -4 -12 4 53.65 3.83 -3 -12 4 54.68 3.79 -2 -12 4 100.78 4.75 -1 -12 4 72.53 4.02 0 -12 4 50.95 3.48 1 -12 4 30.85 2.21 2 -12 4 2.59 1.18 3 -12 4 37.87 2.50 4 -12 4 24.19 2.82 5 -12 4 36.97 3.54 6 -12 4 40.61 3.79 -7 -11 4 1.45 1.64 -6 -11 4 2.65 1.67 -5 -11 4 37.64 3.27 -4 -11 4 71.55 4.79 -3 -11 4 99.95 4.46 -2 -11 4 103.47 4.14 -1 -11 4 32.79 2.74 0 -11 4 10.46 1.43 1 -11 4 4.07 1.18 2 -11 4 5.24 1.25 3 -11 4 16.60 1.69 4 -11 4 69.36 4.13 5 -11 4 147.98 5.52 6 -11 4 44.07 3.84 7 -11 4 24.07 3.26 -7 -10 4 0.56 1.54 -6 -10 4 7.48 1.79 -5 -10 4 36.76 3.08 -4 -10 4 73.74 3.95 -3 -10 4 48.59 3.29 -2 -10 4 40.17 2.93 -1 -10 4 39.99 2.13 0 -10 4 1.66 0.95 1 -10 4 10.41 1.36 2 -10 4 27.57 1.95 3 -10 4 56.38 2.63 4 -10 4 39.50 3.09 5 -10 4 42.92 3.45 6 -10 4 76.78 4.68 7 -10 4 32.67 3.49 8 -10 4 0.97 1.85 -8 -9 4 1.10 1.54 -7 -9 4 0.11 1.37 -6 -9 4 13.88 2.11 -5 -9 4 53.70 3.52 -4 -9 4 83.65 3.98 -3 -9 4 43.29 2.95 -2 -9 4 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-6 4 0.42 0.64 0 -6 4 0.34 0.64 1 -6 4 88.30 2.29 2 -6 4 71.03 2.12 3 -6 4 48.64 1.92 4 -6 4 90.12 2.29 5 -6 4 96.51 4.78 6 -6 4 38.88 3.18 7 -6 4 18.36 2.49 8 -6 4 3.55 2.85 9 -6 4 0.31 2.40 -9 -5 4 2.01 5.18 -8 -5 4 0.99 2.32 -7 -5 4 26.29 3.76 -6 -5 4 31.37 3.83 -5 -5 4 60.08 2.77 -4 -5 4 173.84 3.95 -3 -5 4 159.62 4.66 -2 -5 4 108.16 2.26 -1 -5 4 21.25 1.20 0 -5 4 0.34 0.71 1 -5 4 30.08 1.42 2 -5 4 198.35 3.32 3 -5 4 55.98 1.82 4 -5 4 116.01 2.54 5 -5 4 245.04 8.90 6 -5 4 146.05 12.06 7 -5 4 20.64 2.62 8 -5 4 8.75 3.04 9 -5 4 1.68 2.58 -10 -4 4 12.22 5.61 -9 -4 4 12.57 5.07 -8 -4 4 3.78 2.24 -7 -4 4 12.84 2.92 -6 -4 4 82.03 5.01 -5 -4 4 57.50 4.04 -4 -4 4 187.30 4.46 -3 -4 4 367.78 6.82 -2 -4 4 191.04 3.49 -1 -4 4 17.65 1.15 0 -4 4 23.57 1.30 1 -4 4 79.00 1.86 2 -4 4 88.06 1.99 3 -4 4 530.89 7.44 4 -4 4 342.60 8.02 5 -4 4 49.39 3.59 6 -4 4 24.84 3.03 7 -4 4 24.09 4.26 8 -4 4 1.85 2.15 9 -4 4 14.51 3.70 -10 -3 4 18.31 6.16 -9 -3 4 5.50 5.29 -8 -3 4 2.28 1.90 -7 -3 4 50.71 4.15 -6 -3 4 59.19 3.41 -5 -3 4 42.45 2.64 -4 -3 4 185.91 6.98 -3 -3 4 254.22 4.35 -2 -3 4 25.51 1.31 -1 -3 4 114.85 2.43 0 -3 4 3.95 0.87 1 -3 4 220.48 3.38 2 -3 4 95.35 2.28 3 -3 4 61.10 1.59 4 -3 4 37.27 2.82 5 -3 4 104.51 4.67 6 -3 4 40.80 3.60 7 -3 4 0.53 2.96 8 -3 4 1.05 1.95 9 -3 4 0.53 2.21 -10 -2 4 16.81 5.82 -9 -2 4 0.41 3.73 -8 -2 4 8.00 4.18 -7 -2 4 3.74 1.47 -6 -2 4 50.33 3.16 -5 -2 4 80.89 3.56 -4 -2 4 87.72 4.44 -3 -2 4 324.58 5.35 -2 -2 4 545.24 6.98 -1 -2 4 11.71 0.75 0 -2 4 165.25 3.89 1 -2 4 127.40 2.32 2 -2 4 51.93 1.56 3 -2 4 412.98 5.35 4 -2 4 39.75 2.89 5 -2 4 6.75 1.66 6 -2 4 44.30 4.52 7 -2 4 21.74 3.96 8 -2 4 0.94 3.21 9 -2 4 11.03 4.11 -10 -1 4 2.17 4.19 -9 -1 4 0.15 3.61 -8 -1 4 8.69 2.85 -7 -1 4 53.09 3.23 -6 -1 4 58.24 2.75 -5 -1 4 75.40 4.87 -4 -1 4 123.15 4.21 -3 -1 4 142.70 3.42 -2 -1 4 13.92 1.04 -1 -1 4 0.72 0.46 0 -1 4 0.14 0.43 1 -1 4 215.15 3.17 2 -1 4 81.42 1.90 3 -1 4 108.03 2.20 4 -1 4 100.54 2.12 5 -1 4 58.13 3.69 6 -1 4 23.52 3.79 7 -1 4 0.42 2.87 8 -1 4 6.45 3.55 9 -1 4 3.20 3.88 -10 0 4 5.32 4.90 -9 0 4 8.10 2.97 -8 0 4 17.77 3.24 -7 0 4 3.81 1.51 -6 0 4 76.11 3.80 -5 0 4 187.35 6.12 -4 0 4 7.33 1.65 -3 0 4 0.72 1.36 -2 0 4 45.57 2.47 -1 0 4 14.51 1.09 0 0 4 0.48 0.68 1 0 4 8.88 0.84 2 0 4 170.10 2.99 3 0 4 345.71 4.97 4 0 4 78.75 2.09 5 0 4 6.00 0.91 6 0 4 50.20 4.80 7 0 4 1.70 3.03 8 0 4 2.37 3.43 9 0 4 2.76 5.48 -10 1 4 2.53 3.05 -9 1 4 1.23 2.33 -8 1 4 54.25 4.90 -7 1 4 54.42 4.57 -6 1 4 75.72 3.66 -5 1 4 121.66 4.23 -4 1 4 83.58 4.69 -3 1 4 9.15 1.63 -2 1 4 42.40 1.86 -1 1 4 2.72 0.89 0 1 4 1.61 0.82 1 1 4 39.25 1.56 2 1 4 162.49 3.07 3 1 4 213.41 3.78 4 1 4 82.84 2.51 5 1 4 15.15 1.32 6 1 4 19.59 3.68 7 1 4 1.98 3.08 8 1 4 0.00 4.70 9 1 4 37.66 8.07 -10 2 4 3.58 3.14 -9 2 4 17.86 3.52 -8 2 4 22.97 3.58 -7 2 4 39.99 3.61 -6 2 4 46.54 3.61 -5 2 4 158.64 6.32 -4 2 4 54.66 2.30 -3 2 4 1.35 1.48 -2 2 4 23.90 1.88 -1 2 4 29.97 1.43 0 2 4 0.71 0.79 1 2 4 241.53 4.62 2 2 4 119.07 2.75 3 2 4 55.03 2.06 4 2 4 168.74 3.99 5 2 4 77.48 2.79 6 2 4 0.84 1.08 7 2 4 1.87 4.62 8 2 4 2.46 5.32 9 2 4 5.59 3.05 -10 3 4 3.80 3.71 -9 3 4 0.78 4.21 -8 3 4 9.15 4.49 -7 3 4 109.09 6.71 -6 3 4 108.01 4.60 -5 3 4 100.32 4.19 -4 3 4 72.01 3.33 -3 3 4 125.21 4.65 -2 3 4 22.62 1.51 -1 3 4 7.23 1.05 0 3 4 0.29 0.69 1 3 4 215.45 4.53 2 3 4 645.08 10.81 3 3 4 131.92 3.51 4 3 4 29.87 1.95 5 3 4 59.54 2.44 6 3 4 17.99 1.61 7 3 4 1.77 2.12 8 3 4 63.56 6.12 9 3 4 36.60 5.35 -10 4 4 6.18 4.25 -9 4 4 4.31 3.83 -8 4 4 38.46 4.81 -7 4 4 245.01 10.84 -6 4 4 147.76 5.64 -5 4 4 224.50 6.90 -4 4 4 73.66 3.49 -3 4 4 1.50 0.84 -2 4 4 69.11 2.41 -1 4 4 1.12 0.79 0 4 4 240.12 5.35 1 4 4 468.80 6.55 2 4 4 123.48 3.14 3 4 4 92.30 2.81 4 4 4 166.04 3.46 5 4 4 30.19 1.87 6 4 4 6.89 1.47 7 4 4 1.52 2.18 8 4 4 2.12 2.53 9 4 4 31.10 4.99 -10 5 4 0.67 7.00 -9 5 4 4.76 4.10 -8 5 4 21.30 4.86 -7 5 4 203.77 11.28 -6 5 4 248.39 7.90 -5 5 4 43.10 3.08 -4 5 4 46.33 3.32 -3 5 4 38.82 2.02 -2 5 4 8.70 1.15 -1 5 4 93.58 2.57 0 5 4 8.33 1.11 1 5 4 24.02 1.48 2 5 4 642.30 7.92 3 5 4 64.52 2.34 4 5 4 12.37 1.32 5 5 4 95.24 3.74 6 5 4 29.58 2.63 7 5 4 7.82 2.93 8 5 4 19.82 4.19 -9 6 4 3.02 4.18 -8 6 4 71.90 7.43 -7 6 4 33.98 3.95 -6 6 4 204.08 6.31 -5 6 4 48.54 2.70 -4 6 4 12.83 1.43 -3 6 4 10.26 1.26 -2 6 4 0.36 0.71 -1 6 4 36.80 1.98 0 6 4 142.87 3.25 1 6 4 20.79 1.50 2 6 4 104.20 2.78 3 6 4 161.86 3.52 4 6 4 158.24 4.80 5 6 4 2.12 1.34 6 6 4 7.72 1.80 7 6 4 3.80 2.55 8 6 4 25.77 4.51 -9 7 4 12.49 3.41 -8 7 4 17.27 3.65 -7 7 4 58.75 5.09 -6 7 4 109.69 3.84 -5 7 4 24.23 1.97 -4 7 4 19.89 1.76 -3 7 4 3.36 1.04 -2 7 4 11.84 1.41 -1 7 4 41.89 2.25 0 7 4 48.61 1.87 1 7 4 26.80 1.56 2 7 4 84.10 2.46 3 7 4 62.89 3.58 4 7 4 1.55 1.30 5 7 4 9.50 1.90 6 7 4 1.98 1.53 7 7 4 17.49 3.90 8 7 4 11.86 3.83 -9 8 4 52.12 5.88 -8 8 4 35.09 4.59 -7 8 4 31.75 4.26 -6 8 4 62.24 4.21 -5 8 4 22.66 2.03 -4 8 4 14.44 1.66 -3 8 4 20.20 1.82 -2 8 4 8.14 1.30 -1 8 4 68.53 2.88 0 8 4 41.64 1.69 1 8 4 40.30 1.83 2 8 4 70.76 2.72 3 8 4 133.88 4.04 4 8 4 6.00 1.76 5 8 4 2.13 1.50 6 8 4 0.95 1.49 7 8 4 5.50 2.19 -8 9 4 18.84 4.04 -7 9 4 30.21 3.68 -6 9 4 60.38 4.59 -5 9 4 51.63 3.00 -4 9 4 3.84 1.24 -3 9 4 0.77 0.94 -2 9 4 6.12 1.30 -1 9 4 55.41 2.78 0 9 4 64.55 2.87 1 9 4 122.51 2.77 2 9 4 18.45 1.81 3 9 4 82.27 3.71 4 9 4 25.90 2.83 5 9 4 1.85 1.70 6 9 4 3.02 1.73 7 9 4 1.45 1.88 -8 10 4 28.67 3.92 -7 10 4 24.73 3.48 -6 10 4 32.86 3.55 -5 10 4 30.91 2.50 -4 10 4 23.52 2.22 -3 10 4 0.64 0.99 -2 10 4 55.38 3.00 -1 10 4 2.24 1.12 0 10 4 24.82 2.08 1 10 4 109.87 4.83 2 10 4 85.96 4.55 3 10 4 22.60 2.36 4 10 4 6.47 1.92 5 10 4 1.18 1.58 6 10 4 7.53 2.15 -7 11 4 20.43 3.32 -6 11 4 81.01 5.49 -5 11 4 38.32 2.83 -4 11 4 1.10 1.20 -3 11 4 0.56 1.03 -2 11 4 10.02 1.64 -1 11 4 34.09 2.48 0 11 4 90.69 4.99 1 11 4 29.59 2.98 2 11 4 64.06 4.38 3 11 4 54.89 4.15 4 11 4 1.30 1.61 5 11 4 15.11 2.60 -6 12 4 2.34 2.06 -5 12 4 22.86 2.40 -4 12 4 2.20 1.34 -3 12 4 22.54 2.23 -2 12 4 16.82 2.03 -1 12 4 9.60 2.10 0 12 4 40.03 3.55 1 12 4 121.91 5.32 2 12 4 21.40 2.87 3 12 4 1.47 1.63 4 12 4 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5 14.51 2.71 -7 -11 5 18.24 2.67 -6 -11 5 33.71 3.21 -5 -11 5 61.85 4.02 -4 -11 5 27.86 2.87 -3 -11 5 9.62 1.88 -2 -11 5 8.82 1.81 -1 -11 5 2.28 1.31 0 -11 5 64.78 2.89 1 -11 5 41.91 2.43 2 -11 5 21.60 1.88 3 -11 5 159.86 4.02 4 -11 5 57.24 3.80 5 -11 5 6.15 1.92 6 -11 5 2.05 1.66 7 -11 5 1.07 1.79 -7 -10 5 5.49 1.94 -6 -10 5 14.52 2.31 -5 -10 5 101.94 4.76 -4 -10 5 44.13 3.25 -3 -10 5 0.11 1.07 -2 -10 5 0.84 1.08 -1 -10 5 2.19 0.96 0 -10 5 44.75 2.34 1 -10 5 90.55 3.00 2 -10 5 44.42 2.40 3 -10 5 44.21 2.41 4 -10 5 14.58 2.14 5 -10 5 11.97 2.21 6 -10 5 2.89 1.76 7 -10 5 4.68 2.06 -8 -9 5 15.95 2.53 -7 -9 5 22.88 2.64 -6 -9 5 21.78 2.54 -5 -9 5 44.68 3.16 -4 -9 5 3.96 1.37 -3 -9 5 62.00 3.50 -2 -9 5 0.88 0.79 -1 -9 5 61.00 2.46 0 -9 5 27.78 1.83 1 -9 5 80.55 2.72 2 -9 5 58.24 2.58 3 -9 5 33.78 2.03 4 -9 5 1.08 1.36 5 -9 5 9.57 1.99 6 -9 5 2.43 1.64 7 -9 5 6.55 2.01 8 -9 5 13.51 2.63 -8 -8 5 44.12 3.54 -7 -8 5 23.17 2.58 -6 -8 5 32.99 2.80 -5 -8 5 111.74 4.28 -4 -8 5 4.96 1.36 -3 -8 5 0.87 1.01 -2 -8 5 6.02 0.95 -1 -8 5 7.57 1.05 0 -8 5 196.04 3.79 1 -8 5 203.69 3.94 2 -8 5 50.79 2.27 3 -8 5 9.32 1.23 4 -8 5 45.48 3.13 5 -8 5 1.36 1.39 6 -8 5 2.49 1.57 7 -8 5 1.05 1.57 8 -8 5 19.97 2.87 -9 -7 5 9.04 2.40 -8 -7 5 30.33 3.58 -7 -7 5 88.60 4.32 -6 -7 5 107.71 4.74 -5 -7 5 1.54 1.12 -4 -7 5 31.45 2.39 -3 -7 5 14.08 1.17 -2 -7 5 36.26 1.70 -1 -7 5 78.90 2.27 0 -7 5 86.74 2.37 1 -7 5 311.90 4.82 2 -7 5 218.91 3.95 3 -7 5 2.64 0.87 4 -7 5 10.47 1.78 5 -7 5 6.23 1.66 6 -7 5 1.90 1.52 7 -7 5 25.66 2.89 8 -7 5 20.32 2.88 9 -7 5 22.16 4.81 -9 -6 5 26.34 3.57 -8 -6 5 47.89 5.17 -7 -6 5 79.86 6.22 -6 -6 5 76.72 4.39 -5 -6 5 53.37 3.03 -4 -6 5 0.25 0.62 -3 -6 5 1.69 0.67 -2 -6 5 0.94 0.63 -1 -6 5 204.94 3.45 0 -6 5 201.47 3.46 1 -6 5 77.90 2.14 2 -6 5 72.73 2.12 3 -6 5 52.46 1.99 4 -6 5 28.25 1.52 5 -6 5 6.53 1.58 6 -6 5 12.57 2.13 7 -6 5 8.65 2.40 8 -6 5 40.78 4.25 9 -6 5 32.88 4.25 -9 -5 5 28.53 4.55 -8 -5 5 61.16 5.60 -7 -5 5 107.15 6.30 -6 -5 5 33.94 3.64 -5 -5 5 12.34 1.53 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4.21 1.90 7 2 9 1.64 2.23 -9 3 9 20.43 5.11 -8 3 9 18.09 3.25 -7 3 9 21.08 2.55 -6 3 9 128.81 4.15 -5 3 9 117.04 3.84 -4 3 9 43.45 2.61 -3 3 9 13.35 1.46 -2 3 9 25.18 1.77 -1 3 9 31.60 1.90 0 3 9 97.35 2.86 1 3 9 4.65 1.05 2 3 9 73.81 3.01 3 3 9 199.85 4.37 4 3 9 51.75 2.72 5 3 9 1.68 1.12 6 3 9 15.64 3.68 7 3 9 1.98 2.68 -9 4 9 3.31 3.06 -8 4 9 29.19 4.14 -7 4 9 45.20 3.11 -6 4 9 66.00 3.57 -5 4 9 97.43 3.50 -4 4 9 68.84 3.13 -3 4 9 6.68 1.35 -2 4 9 3.45 1.06 -1 4 9 0.60 0.85 0 4 9 22.62 1.77 1 4 9 242.58 4.79 2 4 9 270.94 5.20 3 4 9 33.93 2.28 4 4 9 22.26 2.02 5 4 9 26.97 2.44 6 4 9 1.93 2.53 7 4 9 3.33 2.92 -8 5 9 14.70 3.29 -7 5 9 46.14 3.29 -6 5 9 100.30 3.88 -5 5 9 53.03 3.02 -4 5 9 6.47 1.34 -3 5 9 15.20 2.01 -2 5 9 0.88 0.95 -1 5 9 96.32 3.30 0 5 9 117.66 3.51 1 5 9 16.61 1.69 2 5 9 148.46 3.91 3 5 9 84.97 3.41 4 5 9 9.04 1.76 5 5 9 2.00 1.53 6 5 9 3.60 3.11 -8 6 9 23.46 4.17 -7 6 9 17.96 2.15 -6 6 9 42.81 2.94 -5 6 9 73.73 3.64 -4 6 9 37.92 2.60 -3 6 9 0.90 1.10 -2 6 9 1.18 1.06 -1 6 9 0.38 0.96 0 6 9 29.86 2.27 1 6 9 145.58 4.06 2 6 9 40.57 2.63 3 6 9 24.15 2.16 4 6 9 49.27 3.60 5 6 9 12.78 2.33 6 6 9 2.98 3.11 -8 7 9 8.86 3.28 -7 7 9 53.60 3.43 -6 7 9 110.93 4.36 -5 7 9 14.04 1.89 -4 7 9 23.73 2.22 -3 7 9 39.12 2.88 -2 7 9 1.20 1.11 -1 7 9 31.51 2.39 0 7 9 21.90 2.08 1 7 9 79.33 3.48 2 7 9 79.58 3.64 3 7 9 22.62 2.76 4 7 9 16.02 2.54 5 7 9 12.72 2.48 -7 8 9 32.16 3.30 -6 8 9 38.52 2.98 -5 8 9 0.58 1.22 -4 8 9 11.07 1.77 -3 8 9 1.27 1.24 -2 8 9 1.62 1.20 -1 8 9 17.99 2.01 0 8 9 82.62 3.77 1 8 9 51.52 3.07 2 8 9 55.78 4.15 3 8 9 36.75 3.55 4 8 9 12.41 2.51 5 8 9 2.47 1.93 -6 9 9 16.42 2.21 -5 9 9 15.28 2.13 -4 9 9 0.77 1.22 -3 9 9 1.06 1.26 -2 9 9 2.78 1.40 -1 9 9 6.88 1.56 0 9 9 76.08 3.76 1 9 9 89.64 5.11 2 9 9 15.56 2.61 3 9 9 18.73 2.81 4 9 9 3.14 2.09 -6 10 9 15.18 2.67 -5 10 9 2.61 1.55 -4 10 9 1.26 1.34 -3 10 9 3.44 1.60 -2 10 9 34.60 2.80 -1 10 9 40.13 2.93 0 10 9 24.43 2.70 1 10 9 20.01 2.93 2 10 9 53.53 4.36 3 10 9 33.61 3.69 -4 11 9 0.76 1.36 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31.85 3.33 1 3 14 17.02 2.66 2 3 14 23.55 2.97 3 3 14 14.88 2.50 4 3 14 56.45 6.64 -6 4 14 17.47 2.71 -5 4 14 4.15 1.83 -4 4 14 23.52 2.92 -3 4 14 13.44 2.41 -2 4 14 9.62 2.22 -1 4 14 7.71 2.08 0 4 14 5.72 2.09 1 4 14 40.45 3.68 2 4 14 57.89 4.37 3 4 14 15.46 2.70 -5 5 14 22.06 3.02 -4 5 14 5.20 1.93 -3 5 14 1.47 1.60 -2 5 14 3.84 1.89 -1 5 14 6.87 2.11 0 5 14 35.60 3.57 1 5 14 8.76 2.33 2 5 14 18.06 2.84 -4 6 14 22.11 3.00 -3 6 14 1.38 1.70 -2 6 14 12.24 2.48 -1 6 14 6.85 2.20 0 6 14 11.00 2.54 1 6 14 64.35 4.73 2 6 14 53.50 4.35 -3 7 14 0.00 1.35 -2 7 14 8.56 2.35 -1 7 14 21.68 3.15 0 7 14 39.45 3.98 -3 -10 15 2.40 2.58 -2 -10 15 4.85 1.93 -1 -10 15 17.41 2.62 0 -10 15 19.94 2.73 1 -10 15 54.65 3.99 -4 -9 15 3.68 2.49 -3 -9 15 0.62 1.65 -2 -9 15 0.41 1.46 -1 -9 15 25.87 2.90 0 -9 15 132.28 6.66 1 -9 15 58.55 4.82 2 -9 15 9.68 3.43 -5 -8 15 11.13 3.23 -4 -8 15 17.43 2.94 -3 -8 15 1.20 1.60 -2 -8 15 23.16 2.78 -1 -8 15 44.58 3.58 0 -8 15 8.07 1.98 1 -8 15 26.63 2.88 2 -8 15 49.02 5.60 3 -8 15 3.76 2.94 -5 -7 15 19.24 3.85 -4 -7 15 2.36 1.73 -3 -7 15 0.99 1.79 -2 -7 15 1.13 1.85 -1 -7 15 3.98 1.88 0 -7 15 34.87 3.57 1 -7 15 21.78 3.14 2 -7 15 23.69 4.26 3 -7 15 18.68 4.01 -6 -6 15 14.96 3.78 -5 -6 15 17.12 3.04 -4 -6 15 29.95 3.37 -3 -6 15 1.30 1.48 -2 -6 15 14.52 2.29 -1 -6 15 15.63 2.35 0 -6 15 16.61 2.37 1 -6 15 35.18 3.12 2 -6 15 55.35 3.77 3 -6 15 11.51 3.64 4 -6 15 6.81 3.39 -6 -5 15 23.50 3.23 -5 -5 15 11.46 2.23 -4 -5 15 7.10 1.92 -3 -5 15 0.63 1.40 -2 -5 15 9.63 2.12 -1 -5 15 31.84 3.04 0 -5 15 38.35 3.27 1 -5 15 62.21 4.03 2 -5 15 31.56 3.02 3 -5 15 20.63 4.37 4 -5 15 3.29 3.04 -6 -4 15 23.61 2.82 -5 -4 15 17.66 2.54 -4 -4 15 2.86 1.62 -3 -4 15 0.90 1.35 -2 -4 15 32.35 3.10 -1 -4 15 21.70 2.68 0 -4 15 46.67 3.60 1 -4 15 89.26 4.47 2 -4 15 32.84 3.09 3 -4 15 15.48 4.07 4 -4 15 0.26 2.62 -6 -3 15 7.98 2.00 -5 -3 15 1.48 1.53 -4 -3 15 0.88 1.43 -3 -3 15 43.13 3.57 -2 -3 15 23.71 2.79 -1 -3 15 15.53 2.34 0 -3 15 66.03 4.20 1 -3 15 90.72 4.55 2 -3 15 23.65 2.71 3 -3 15 2.28 2.79 4 -3 15 4.48 3.12 -6 -2 15 25.38 2.99 -5 -2 15 1.03 1.39 -4 -2 15 5.13 1.79 -3 -2 15 21.04 2.61 -2 -2 15 41.97 3.45 -1 -2 15 39.48 3.42 0 -2 15 44.91 3.55 1 -2 15 28.71 2.97 2 -2 15 36.15 3.35 3 -2 15 9.94 3.59 4 -2 15 0.00 2.30 -6 -1 15 12.04 2.33 -5 -1 15 9.64 2.11 -4 -1 15 13.17 2.33 -3 -1 15 44.78 3.71 -2 -1 15 45.91 3.75 -1 -1 15 20.24 2.66 0 -1 15 64.11 4.25 1 -1 15 52.47 3.92 2 -1 15 20.21 2.68 3 -1 15 1.05 2.69 4 -1 15 1.73 2.83 -6 0 15 14.36 2.40 -5 0 15 0.66 1.50 -4 0 15 0.41 1.36 -3 0 15 10.47 2.26 -2 0 15 29.00 3.18 -1 0 15 65.06 4.46 0 0 15 41.51 3.57 1 0 15 25.08 2.97 2 0 15 18.47 2.62 3 0 15 14.59 2.47 4 0 15 0.80 2.80 -6 1 15 7.76 2.02 -5 1 15 7.98 2.04 -4 1 15 2.80 1.66 -3 1 15 28.77 3.22 -2 1 15 8.71 2.10 -1 1 15 78.93 5.02 0 1 15 102.17 5.63 1 1 15 47.79 3.94 2 1 15 29.83 3.18 3 1 15 8.49 2.23 -6 2 15 6.54 1.98 -5 2 15 0.31 1.40 -4 2 15 2.41 1.61 -3 2 15 34.35 3.44 -2 2 15 35.43 3.50 -1 2 15 69.47 4.73 0 2 15 23.93 3.04 1 2 15 7.98 2.23 2 2 15 10.10 2.37 3 2 15 1.38 1.66 -5 3 15 0.79 1.46 -4 3 15 8.28 2.15 -3 3 15 21.75 2.98 -2 3 15 41.84 3.88 -1 3 15 10.73 2.43 0 3 15 26.40 3.17 1 3 15 17.96 2.89 2 3 15 3.15 2.01 3 3 15 2.58 1.91 -5 4 15 1.36 1.66 -4 4 15 14.74 2.55 -3 4 15 22.40 2.92 -2 4 15 64.80 4.65 -1 4 15 23.38 3.15 0 4 15 28.66 3.45 1 4 15 3.13 1.97 2 4 15 3.36 2.02 -4 5 15 0.95 1.61 -3 5 15 26.43 3.27 -2 5 15 49.95 4.23 -1 5 15 18.78 2.99 0 5 15 11.31 2.62 1 5 15 15.12 2.89 -2 6 15 49.55 5.01 -1 6 15 51.59 4.49 -2 -9 16 65.21 5.21 -1 -9 16 48.07 3.84 0 -9 16 30.15 3.15 -3 -8 16 26.81 3.59 -2 -8 16 57.67 4.90 -1 -8 16 73.62 4.60 0 -8 16 9.19 2.13 1 -8 16 0.49 1.63 -4 -7 16 13.99 2.55 -3 -7 16 40.09 5.07 -2 -7 16 23.12 3.13 -1 -7 16 29.72 3.52 0 -7 16 15.24 2.80 1 -7 16 11.24 2.56 2 -7 16 2.51 2.73 -5 -6 16 11.56 2.79 -4 -6 16 14.82 2.79 -3 -6 16 14.92 2.55 -2 -6 16 23.57 2.86 -1 -6 16 61.13 4.15 0 -6 16 4.79 1.82 1 -6 16 0.80 1.61 2 -6 16 4.10 2.93 -5 -5 16 11.55 2.27 -4 -5 16 24.50 3.00 -3 -5 16 31.55 3.18 -2 -5 16 50.48 3.81 -1 -5 16 10.71 2.15 0 -5 16 14.39 2.32 1 -5 16 1.77 1.59 2 -5 16 2.72 2.83 3 -5 16 5.21 3.05 -5 -4 16 28.07 3.08 -4 -4 16 43.13 3.61 -3 -4 16 43.12 3.62 -2 -4 16 29.86 3.12 -1 -4 16 13.67 2.38 0 -4 16 9.78 2.16 1 -4 16 1.31 1.48 2 -4 16 6.18 1.91 3 -4 16 21.01 4.64 -5 -3 16 36.61 3.42 -4 -3 16 17.86 2.69 -3 -3 16 57.81 4.15 -2 -3 16 25.44 2.95 -1 -3 16 24.42 2.93 0 -3 16 2.79 1.70 1 -3 16 1.18 1.56 2 -3 16 5.67 1.91 3 -3 16 13.48 3.98 -5 -2 16 12.42 2.38 -4 -2 16 50.04 3.92 -3 -2 16 40.91 3.74 -2 -2 16 16.64 2.59 -1 -2 16 13.41 2.42 0 -2 16 18.83 2.62 1 -2 16 0.81 1.48 2 -2 16 29.08 3.10 3 -2 16 7.47 3.69 -5 -1 16 36.85 3.54 -4 -1 16 28.46 3.17 -3 -1 16 37.49 3.61 -2 -1 16 75.24 4.91 -1 -1 16 1.11 1.54 0 -1 16 0.04 1.42 1 -1 16 0.10 1.52 2 -1 16 9.50 2.23 3 -1 16 43.57 5.97 -5 0 16 17.90 2.70 -4 0 16 60.14 4.48 -3 0 16 25.22 3.11 -2 0 16 31.80 3.40 -1 0 16 17.08 2.77 0 0 16 6.72 2.13 1 0 16 30.59 3.33 2 0 16 16.84 2.69 3 0 16 2.72 3.30 -5 1 16 40.11 3.77 -4 1 16 23.06 3.07 -3 1 16 60.62 5.27 -2 1 16 92.05 5.53 -1 1 16 12.35 2.55 0 1 16 3.01 1.94 1 1 16 0.36 1.73 2 1 16 5.54 2.11 -5 2 16 34.97 3.65 -4 2 16 47.18 4.12 -3 2 16 23.20 3.12 -2 2 16 7.46 2.22 -1 2 16 32.89 3.59 0 2 16 1.55 1.82 1 2 16 11.73 2.54 2 2 16 11.13 2.47 -4 3 16 42.50 4.05 -3 3 16 12.97 2.54 -2 3 16 16.35 2.85 -1 3 16 34.44 3.71 0 3 16 0.72 1.76 1 3 16 7.50 2.37 -3 4 16 34.77 3.76 -2 4 16 6.62 2.31 -1 4 16 1.54 1.96 0 4 16 0.79 1.88 -2 -7 17 4.57 2.06 -1 -7 17 0.55 1.87 0 -7 17 23.22 3.31 -3 -6 17 25.01 3.06 -2 -6 17 0.53 1.61 -1 -6 17 0.51 1.59 0 -6 17 3.60 1.84 1 -6 17 18.75 2.74 -4 -5 17 16.33 2.71 -3 -5 17 0.95 1.69 -2 -5 17 3.09 1.81 -1 -5 17 11.31 2.34 0 -5 17 32.99 3.31 1 -5 17 14.66 2.49 -4 -4 17 9.20 2.19 -3 -4 17 6.47 2.03 -2 -4 17 10.71 2.28 -1 -4 17 9.84 2.21 0 -4 17 16.15 2.58 1 -4 17 50.79 3.94 -4 -3 17 9.63 2.33 -3 -3 17 7.79 2.15 -2 -3 17 2.52 1.76 -1 -3 17 27.30 3.11 0 -3 17 24.07 2.97 1 -3 17 7.40 2.10 -4 -2 17 14.53 2.57 -3 -2 17 5.20 2.05 -2 -2 17 2.22 1.81 -1 -2 17 2.16 1.81 0 -2 17 15.51 2.55 1 -2 17 33.87 3.39 -4 -1 17 19.32 2.82 -3 -1 17 3.04 1.93 -2 -1 17 4.61 2.19 -1 -1 17 10.47 2.40 0 -1 17 11.62 2.60 1 -1 17 38.78 3.72 -4 0 17 2.50 1.75 -3 0 17 0.26 1.52 -2 0 17 1.67 1.86 -1 0 17 43.76 4.07 0 0 17 31.93 3.54 1 0 17 37.92 3.86 -3 1 17 8.32 2.30 -2 1 17 43.62 4.11 -1 1 17 24.54 3.29 0 1 17 32.58 3.66 -2 2 17 7.72 2.45 -1 2 17 59.23 4.85 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 51844 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969310' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_11 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 N3 O7 Yb' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 890.98 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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 8.6999(8) _cell_length_b 13.0183(12) _cell_length_c 14.8094(14) _cell_angle_alpha 100.2070(10) _cell_angle_beta 97.5490(10) _cell_angle_gamma 92.5300(10) _cell_volume 1632.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23881 _cell_measurement_theta_min 4.734 _cell_measurement_theta_max 59.838 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_F_000 878 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_absorpt_coefficient_mu 3.167 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6848 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23879 _diffrn_reflns_av_unetI/netI 0.0617 _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.411 _diffrn_reflns_theta_max 30.263 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.909 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.909 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.909 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8886 _reflns_number_gt 7623 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0235P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8886 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0622 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.002 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Yb1 Yb 0.55994(2) 0.51327(2) 0.70153(2) 0.01003(4) Uani 1 1 d . . . . . O1 O 0.7068(2) 0.62196(17) 0.83976(15) 0.0144(5) Uani 1 1 d . . . . . O3 O 0.5603(2) 0.37897(17) 0.56136(15) 0.0144(5) Uani 1 1 d . . . . . O2 O 0.5327(2) 0.69661(17) 0.75429(15) 0.0151(5) Uani 1 1 d . . . . . C23 C 0.4589(4) 0.3216(2) 0.5868(2) 0.0126(6) Uani 1 1 d . . . . . O4 O 0.4043(2) 0.35201(17) 0.66127(14) 0.0147(5) Uani 1 1 d . . . . . C16 C 0.6378(4) 0.7020(2) 0.8227(2) 0.0126(6) Uani 1 1 d . . . . . C24 C 0.4046(4) 0.2165(2) 0.5289(2) 0.0131(6) Uani 1 1 d . . . . . C17 C 0.6806(4) 0.8062(2) 0.8848(2) 0.0138(6) Uani 1 1 d . . . . . C20 C 0.7531(4) 1.0000(3) 0.9974(2) 0.0167(7) Uani 1 1 d . . . . . C19 C 0.8400(4) 0.9164(3) 1.0135(2) 0.0176(7) Uani 1 1 d . . . . . H19 H 0.9214 0.9251 1.0622 0.021 Uiso 1 1 calc R U . . . C25 C 0.4719(4) 0.1790(3) 0.4502(2) 0.0176(7) Uani 1 1 d . . . . . H25 H 0.5484 0.2204 0.4327 0.021 Uiso 1 1 calc R U . . . C22 C 0.5952(4) 0.8915(3) 0.8689(2) 0.0164(7) Uani 1 1 d . . . . . H22 H 0.5140 0.8827 0.8201 0.020 Uiso 1 1 calc R U . . . C27 C 0.3110(4) 0.0209(3) 0.4246(2) 0.0203(7) Uani 1 1 d . . . . . C18 C 0.8037(4) 0.8200(3) 0.9558(2) 0.0171(7) Uani 1 1 d . . . . . H18 H 0.8628 0.7640 0.9651 0.020 Uiso 1 1 calc R U . . . C21 C 0.6306(4) 0.9891(3) 0.9252(2) 0.0168(7) Uani 1 1 d . . . . . H21 H 0.5737 1.0457 0.9149 0.020 Uiso 1 1 calc R U . . . C29 C 0.2900(4) 0.1542(3) 0.5544(2) 0.0181(7) Uani 1 1 d . . . . . H29 H 0.2455 0.1782 0.6073 0.022 Uiso 1 1 calc R U . . . C26 C 0.4261(4) 0.0808(3) 0.3978(2) 0.0220(8) Uani 1 1 d . . . . . H26 H 0.4718 0.0557 0.3457 0.026 Uiso 1 1 calc R U . . . C28 C 0.2415(4) 0.0567(3) 0.5017(2) 0.0225(8) Uani 1 1 d . . . . . H28 H 0.1631 0.0158 0.5180 0.027 Uiso 1 1 calc R U . . . Cl1 Cl 0.79727(10) 1.12118(6) 1.07014(6) 0.02003(17) Uani 1 1 d . . . . . Cl2 Cl 0.24910(13) -0.10157(7) 0.35819(7) 0.0364(2) Uani 1 1 d . . . . . N1 N 0.7876(3) 0.40670(19) 0.72287(17) 0.0119(5) Uani 1 1 d . . . . . N2 N 0.5669(3) 0.41582(19) 0.83529(17) 0.0104(5) Uani 1 1 d . . . . . N3 N 0.3378(3) 0.53839(19) 0.79374(18) 0.0123(5) Uani 1 1 d . . . . . C15 C 0.2266(4) 0.6022(2) 0.7717(2) 0.0144(6) Uani 1 1 d . . . . . H15 H 0.2360 0.6377 0.7233 0.017 Uiso 1 1 calc R U . . . C5 C 0.8071(4) 0.3507(2) 0.7922(2) 0.0116(6) Uani 1 1 d . . . . . C10 C 0.4477(4) 0.4171(2) 0.8845(2) 0.0121(6) Uani 1 1 d . . . . . C1 C 0.8971(4) 0.4051(2) 0.6674(2) 0.0138(6) Uani 1 1 d . . . . . H1 H 0.8820 0.4412 0.6184 0.017 Uiso 1 1 calc R U . . . C6 C 0.6785(4) 0.3493(2) 0.8485(2) 0.0132(6) Uani 1 1 d . . . . . C11 C 0.3249(3) 0.4893(2) 0.8652(2) 0.0130(6) Uani 1 1 d . . . . . C4 C 0.9401(4) 0.2973(2) 0.8080(2) 0.0153(7) Uani 1 1 d . . . . . H4 H 0.9525 0.2603 0.8564 0.018 Uiso 1 1 calc R U . . . C14 C 0.0985(4) 0.6171(3) 0.8184(2) 0.0173(7) Uani 1 1 d . . . . . H14 H 0.0217 0.6595 0.8000 0.021 Uiso 1 1 calc R U . . . C12 C 0.2028(4) 0.5042(3) 0.9168(2) 0.0162(7) Uani 1 1 d . . . . . H12 H 0.1987 0.4716 0.9675 0.019 Uiso 1 1 calc R U . . . C3 C 1.0545(4) 0.2995(2) 0.7508(2) 0.0156(7) Uani 1 1 d . . . . . H3 H 1.1449 0.2653 0.7613 0.019 Uiso 1 1 calc R U . . . C2 C 1.0318(4) 0.3531(2) 0.6785(2) 0.0147(6) Uani 1 1 d . . . . . H2 H 1.1050 0.3543 0.6382 0.018 Uiso 1 1 calc R U . . . C9 C 0.4376(4) 0.3522(3) 0.9493(2) 0.0172(7) Uani 1 1 d . . . . . H9 H 0.3556 0.3558 0.9839 0.021 Uiso 1 1 calc R U . . . C7 C 0.6714(4) 0.2805(3) 0.9104(2) 0.0173(7) Uani 1 1 d . . . . . H7 H 0.7476 0.2335 0.9171 0.021 Uiso 1 1 calc R U . . . C8 C 0.5493(4) 0.2834(3) 0.9614(2) 0.0209(7) Uani 1 1 d . . . . . H8 H 0.5432 0.2389 1.0037 0.025 Uiso 1 1 calc R U . . . C13 C 0.0874(4) 0.5679(3) 0.8923(2) 0.0198(7) Uani 1 1 d . . . . . H13 H 0.0037 0.5773 0.9253 0.024 Uiso 1 1 calc R U . . . OW1 O 0.3728(3) 0.55835(17) 0.59367(15) 0.0133(5) Uani 1 1 d D . . . . O5 O 0.7238(2) 0.59667(17) 0.63038(15) 0.0143(5) Uani 1 1 d . . . . . C30 C 0.8206(3) 0.6267(2) 0.5809(2) 0.0132(6) Uani 1 1 d . . . . . O6 O 0.8425(3) 0.58031(18) 0.50324(15) 0.0172(5) Uani 1 1 d . . . . . C32 C 0.8684(4) 0.8000(3) 0.6904(2) 0.0151(7) Uani 1 1 d . . . . . H32 H 0.7751 0.7859 0.7115 0.018 Uiso 1 1 calc R U . . . C31 C 0.9174(3) 0.7273(2) 0.6208(2) 0.0124(6) Uani 1 1 d . . . . . C36 C 1.0565(4) 0.7496(3) 0.5890(2) 0.0173(7) Uani 1 1 d . . . . . H36 H 1.0895 0.7026 0.5416 0.021 Uiso 1 1 calc R U . . . C33 C 0.9555(4) 0.8926(3) 0.7286(2) 0.0169(7) Uani 1 1 d . . . . . H33 H 0.9213 0.9407 0.7748 0.020 Uiso 1 1 calc R U . . . C35 C 1.1458(4) 0.8413(3) 0.6273(2) 0.0203(7) Uani 1 1 d . . . . . H35 H 1.2396 0.8551 0.6066 0.024 Uiso 1 1 calc R U . . . C34 C 1.0957(4) 0.9125(3) 0.6966(2) 0.0171(7) Uani 1 1 d . . . . . Cl3 Cl 1.21020(11) 1.02679(7) 0.74438(6) 0.0278(2) Uani 1 1 d . . . . . H37 H 0.410(4) 0.590(3) 0.548(2) 0.036(12) Uiso 1 1 d D . . . . H38 H 0.296(4) 0.507(3) 0.558(3) 0.059(15) Uiso 1 1 d 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 Yb1 0.01062(7) 0.01041(7) 0.00937(7) 0.00197(5) 0.00253(5) 0.00015(5) O1 0.0158(11) 0.0123(11) 0.0155(11) 0.0024(9) 0.0042(9) 0.0005(9) O3 0.0161(11) 0.0129(11) 0.0141(11) 0.0021(9) 0.0030(9) -0.0028(9) O2 0.0157(11) 0.0140(11) 0.0145(11) 0.0016(9) 0.0003(9) -0.0003(9) C23 0.0130(15) 0.0113(15) 0.0130(15) 0.0033(12) -0.0014(12) 0.0022(12) O4 0.0163(11) 0.0166(12) 0.0108(11) 0.0001(9) 0.0037(9) -0.0006(9) C16 0.0132(15) 0.0130(15) 0.0125(15) 0.0007(12) 0.0084(12) -0.0012(12) C24 0.0136(15) 0.0108(15) 0.0141(15) 0.0013(12) -0.0013(12) 0.0037(12) C17 0.0153(16) 0.0153(16) 0.0113(15) 0.0020(12) 0.0058(12) -0.0028(12) C20 0.0208(17) 0.0167(17) 0.0130(16) 0.0020(13) 0.0038(13) 0.0023(13) C19 0.0142(16) 0.0199(18) 0.0174(17) 0.0032(14) -0.0013(13) -0.0007(13) C25 0.0122(16) 0.0201(18) 0.0188(17) 0.0013(14) -0.0004(13) -0.0024(13) C22 0.0163(16) 0.0197(17) 0.0134(15) 0.0047(13) 0.0011(13) 0.0017(13) C27 0.0267(19) 0.0110(16) 0.0192(17) 0.0003(13) -0.0088(15) 0.0046(14) C18 0.0199(17) 0.0153(16) 0.0167(16) 0.0031(13) 0.0042(13) 0.0025(13) C21 0.0198(17) 0.0137(16) 0.0170(16) 0.0035(13) 0.0011(13) 0.0056(13) C29 0.0206(17) 0.0171(17) 0.0165(16) 0.0034(14) 0.0026(13) 0.0007(14) C26 0.0240(19) 0.0172(18) 0.0219(18) -0.0038(14) 0.0016(15) 0.0059(14) C28 0.0250(19) 0.0170(18) 0.0249(19) 0.0074(15) -0.0018(15) -0.0039(14) Cl1 0.0243(4) 0.0137(4) 0.0196(4) -0.0001(3) -0.0016(3) 0.0016(3) Cl2 0.0464(6) 0.0168(5) 0.0372(6) -0.0054(4) -0.0113(5) -0.0009(4) N1 0.0115(13) 0.0102(13) 0.0135(13) 0.0009(10) 0.0023(10) -0.0014(10) N2 0.0119(13) 0.0097(13) 0.0095(12) 0.0007(10) 0.0027(10) -0.0009(10) N3 0.0141(13) 0.0086(13) 0.0141(13) 0.0015(10) 0.0029(10) -0.0008(10) C15 0.0145(16) 0.0146(16) 0.0144(16) 0.0024(13) 0.0032(12) 0.0010(13) C5 0.0123(15) 0.0099(15) 0.0112(14) -0.0015(12) 0.0017(12) -0.0007(12) C10 0.0125(15) 0.0118(15) 0.0124(15) 0.0020(12) 0.0042(12) -0.0007(12) C1 0.0167(16) 0.0112(15) 0.0135(15) 0.0013(12) 0.0043(12) -0.0005(12) C6 0.0146(16) 0.0122(15) 0.0122(15) 0.0013(12) 0.0017(12) -0.0009(12) C11 0.0096(15) 0.0132(16) 0.0134(15) -0.0035(12) 0.0010(12) -0.0033(12) C4 0.0177(16) 0.0150(16) 0.0125(15) 0.0020(13) 0.0006(13) 0.0025(13) C14 0.0149(16) 0.0186(17) 0.0191(17) 0.0035(14) 0.0031(13) 0.0069(13) C12 0.0164(16) 0.0163(17) 0.0165(16) 0.0036(13) 0.0046(13) -0.0009(13) C3 0.0116(15) 0.0139(16) 0.0201(17) -0.0003(13) 0.0026(13) 0.0008(12) C2 0.0141(16) 0.0125(16) 0.0176(16) 0.0008(13) 0.0059(13) -0.0004(12) C9 0.0161(16) 0.0216(18) 0.0165(16) 0.0063(14) 0.0074(13) 0.0036(13) C7 0.0196(17) 0.0207(18) 0.0149(16) 0.0084(14) 0.0062(13) 0.0061(14) C8 0.0235(18) 0.0252(19) 0.0202(17) 0.0156(15) 0.0085(14) 0.0065(15) C13 0.0179(17) 0.0183(18) 0.0252(18) 0.0033(14) 0.0104(14) 0.0036(14) OW1 0.0143(11) 0.0142(12) 0.0113(11) 0.0026(9) 0.0014(9) -0.0005(9) O5 0.0158(11) 0.0136(11) 0.0149(11) 0.0030(9) 0.0071(9) -0.0012(9) C30 0.0098(15) 0.0137(16) 0.0169(16) 0.0053(13) 0.0003(12) 0.0033(12) O6 0.0163(12) 0.0202(12) 0.0147(11) 0.0005(10) 0.0063(9) -0.0042(9) C32 0.0140(16) 0.0182(17) 0.0151(16) 0.0074(13) 0.0039(13) -0.0010(13) C31 0.0108(15) 0.0155(16) 0.0119(15) 0.0054(12) 0.0009(12) 0.0001(12) C36 0.0169(17) 0.0178(17) 0.0179(17) 0.0022(13) 0.0066(13) 0.0003(13) C33 0.0230(18) 0.0171(17) 0.0112(15) 0.0026(13) 0.0050(13) 0.0006(14) C35 0.0136(16) 0.0190(18) 0.030(2) 0.0067(15) 0.0059(14) 0.0007(13) C34 0.0177(17) 0.0155(17) 0.0174(16) 0.0049(13) -0.0007(13) -0.0035(13) Cl3 0.0321(5) 0.0209(5) 0.0282(5) 0.0016(4) 0.0041(4) -0.0088(4) _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 Yb1 O5 2.232(2) . ? Yb1 OW1 2.298(2) . ? Yb1 O4 2.385(2) . ? Yb1 O2 2.408(2) . ? Yb1 O1 2.439(2) . ? Yb1 O3 2.466(2) . ? Yb1 N1 2.486(3) . ? Yb1 N3 2.509(3) . ? Yb1 N2 2.530(2) . ? Yb1 C16 2.773(3) . ? Yb1 C23 2.792(3) . ? Yb1 H37 2.83(3) . ? O1 C16 1.272(4) . ? O3 C23 1.268(4) . ? O2 C16 1.262(4) . ? C23 O4 1.264(4) . ? C23 C24 1.500(4) . ? C16 C17 1.499(4) . ? C24 C29 1.390(4) . ? C24 C25 1.393(4) . ? C17 C18 1.380(4) . ? C17 C22 1.401(4) . ? C20 C21 1.390(4) . ? C20 C19 1.390(5) . ? C20 Cl1 1.741(3) . ? C19 C18 1.385(4) . ? C19 H19 0.9300 . ? C25 C26 1.384(4) . ? C25 H25 0.9300 . ? C22 C21 1.387(4) . ? C22 H22 0.9300 . ? C27 C26 1.383(5) . ? C27 C28 1.379(5) . ? C27 Cl2 1.741(3) . ? C18 H18 0.9300 . ? C21 H21 0.9300 . ? C29 C28 1.383(5) . ? C29 H29 0.9300 . ? C26 H26 0.9300 . ? C28 H28 0.9300 . ? N1 C1 1.335(4) . ? N1 C5 1.358(4) . ? N2 C10 1.342(4) . ? N2 C6 1.346(4) . ? N3 C11 1.344(4) . ? N3 C15 1.348(4) . ? C15 C14 1.390(4) . ? C15 H15 0.9300 . ? C5 C4 1.391(4) . ? C5 C6 1.482(4) . ? C10 C9 1.395(4) . ? C10 C11 1.487(4) . ? C1 C2 1.385(4) . ? C1 H1 0.9300 . ? C6 C7 1.396(4) . ? C11 C12 1.388(4) . ? C4 C3 1.391(4) . ? C4 H4 0.9300 . ? C14 C13 1.373(5) . ? C14 H14 0.9300 . ? C12 C13 1.382(5) . ? C12 H12 0.9300 . ? C3 C2 1.375(4) . ? C3 H3 0.9300 . ? C2 H2 0.9300 . ? C9 C8 1.367(5) . ? C9 H9 0.9300 . ? C7 C8 1.380(4) . ? C7 H7 0.9300 . ? C8 H8 0.9300 . ? C13 H13 0.9300 . ? OW1 H37 0.941(18) . ? OW1 H38 0.954(19) . ? O5 C30 1.278(4) . ? C30 O6 1.243(4) . ? C30 C31 1.507(4) . ? C32 C33 1.383(4) . ? C32 C31 1.394(4) . ? C32 H32 0.9300 . ? C31 C36 1.393(4) . ? C36 C35 1.383(5) . ? C36 H36 0.9300 . ? C33 C34 1.395(4) . ? C33 H33 0.9300 . ? C35 C34 1.385(5) . ? C35 H35 0.9300 . ? C34 Cl3 1.737(3) . ? 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 Yb1 OW1 84.05(8) . . ? O5 Yb1 O4 134.57(7) . . ? OW1 Yb1 O4 80.92(8) . . ? O5 Yb1 O2 74.82(8) . . ? OW1 Yb1 O2 75.06(8) . . ? O4 Yb1 O2 139.56(7) . . ? O5 Yb1 O1 82.48(7) . . ? OW1 Yb1 O1 129.39(7) . . ? O4 Yb1 O1 138.26(7) . . ? O2 Yb1 O1 54.34(7) . . ? O5 Yb1 O3 80.96(7) . . ? OW1 Yb1 O3 75.31(8) . . ? O4 Yb1 O3 53.80(7) . . ? O2 Yb1 O3 143.25(7) . . ? O1 Yb1 O3 148.31(7) . . ? O5 Yb1 N1 80.96(8) . . ? OW1 Yb1 N1 144.26(8) . . ? O4 Yb1 N1 86.86(8) . . ? O2 Yb1 N1 130.53(8) . . ? O1 Yb1 N1 80.44(8) . . ? O3 Yb1 N1 70.41(8) . . ? O5 Yb1 N3 143.29(8) . . ? OW1 Yb1 N3 79.33(8) . . ? O4 Yb1 N3 74.59(8) . . ? O2 Yb1 N3 69.36(8) . . ? O1 Yb1 N3 83.23(8) . . ? O3 Yb1 N3 124.95(8) . . ? N1 Yb1 N3 129.33(8) . . ? O5 Yb1 N2 139.28(8) . . ? OW1 Yb1 N2 136.67(8) . . ? O4 Yb1 N2 67.71(8) . . ? O2 Yb1 N2 110.37(8) . . ? O1 Yb1 N2 70.89(7) . . ? O3 Yb1 N2 106.05(8) . . ? N1 Yb1 N2 64.97(8) . . ? N3 Yb1 N2 64.36(8) . . ? O5 Yb1 C16 76.67(8) . . ? OW1 Yb1 C16 102.09(9) . . ? O4 Yb1 C16 148.46(8) . . ? O2 Yb1 C16 27.05(8) . . ? O1 Yb1 C16 27.30(8) . . ? O3 Yb1 C16 157.63(8) . . ? N1 Yb1 C16 105.69(9) . . ? N3 Yb1 C16 75.18(8) . . ? N2 Yb1 C16 91.14(8) . . ? O5 Yb1 C23 107.89(8) . . ? OW1 Yb1 C23 76.97(8) . . ? O4 Yb1 C23 26.81(8) . . ? O2 Yb1 C23 151.45(8) . . ? O1 Yb1 C23 153.25(8) . . ? O3 Yb1 C23 26.99(8) . . ? N1 Yb1 C23 77.11(9) . . ? N3 Yb1 C23 99.93(9) . . ? N2 Yb1 C23 86.42(8) . . ? C16 Yb1 C23 175.11(9) . . ? O5 Yb1 H37 66.7(6) . . ? OW1 Yb1 H37 17.4(6) . . ? O4 Yb1 H37 92.5(7) . . ? O2 Yb1 H37 73.3(8) . . ? O1 Yb1 H37 124.7(8) . . ? O3 Yb1 H37 71.9(8) . . ? N1 Yb1 H37 133.3(7) . . ? N3 Yb1 H37 94.9(7) . . ? N2 Yb1 H37 154.0(6) . . ? C16 Yb1 H37 98.8(8) . . ? C23 Yb1 H37 81.7(8) . . ? C16 O1 Yb1 91.10(18) . . ? C23 O3 Yb1 90.99(18) . . ? C16 O2 Yb1 92.77(18) . . ? O4 C23 O3 120.3(3) . . ? O4 C23 C24 119.8(3) . . ? O3 C23 C24 119.9(3) . . ? O4 C23 Yb1 58.34(16) . . ? O3 C23 Yb1 62.01(16) . . ? C24 C23 Yb1 177.5(2) . . ? C23 O4 Yb1 94.85(18) . . ? O2 C16 O1 121.7(3) . . ? O2 C16 C17 118.3(3) . . ? O1 C16 C17 120.0(3) . . ? O2 C16 Yb1 60.18(16) . . ? O1 C16 Yb1 61.60(16) . . ? C17 C16 Yb1 177.6(2) . . ? C29 C24 C25 119.2(3) . . ? C29 C24 C23 120.5(3) . . ? C25 C24 C23 120.3(3) . . ? C18 C17 C22 119.5(3) . . ? C18 C17 C16 121.5(3) . . ? C22 C17 C16 119.0(3) . . ? C21 C20 C19 121.6(3) . . ? C21 C20 Cl1 119.2(3) . . ? C19 C20 Cl1 119.2(3) . . ? C18 C19 C20 119.0(3) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C26 C25 C24 120.8(3) . . ? C26 C25 H25 119.6 . . ? C24 C25 H25 119.6 . . ? C21 C22 C17 120.7(3) . . ? C21 C22 H22 119.6 . . ? C17 C22 H22 119.6 . . ? C26 C27 C28 121.6(3) . . ? C26 C27 Cl2 119.3(3) . . ? C28 C27 Cl2 119.0(3) . . ? C17 C18 C19 120.7(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C22 C21 C20 118.4(3) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? C28 C29 C24 120.5(3) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? C27 C26 C25 118.7(3) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C29 C28 C27 119.2(3) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C1 N1 C5 117.9(3) . . ? C1 N1 Yb1 120.6(2) . . ? C5 N1 Yb1 121.49(19) . . ? C10 N2 C6 118.9(3) . . ? C10 N2 Yb1 120.4(2) . . ? C6 N2 Yb1 119.82(19) . . ? C11 N3 C15 118.1(3) . . ? C11 N3 Yb1 121.9(2) . . ? C15 N3 Yb1 120.0(2) . . ? N3 C15 C14 122.7(3) . . ? N3 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? N1 C5 C4 121.3(3) . . ? N1 C5 C6 116.1(3) . . ? C4 C5 C6 122.6(3) . . ? N2 C10 C9 121.6(3) . . ? N2 C10 C11 116.9(3) . . ? C9 C10 C11 121.4(3) . . ? N1 C1 C2 123.9(3) . . ? N1 C1 H1 118.0 . . ? C2 C1 H1 118.0 . . ? N2 C6 C7 121.7(3) . . ? N2 C6 C5 116.8(3) . . ? C7 C6 C5 121.5(3) . . ? N3 C11 C12 121.8(3) . . ? N3 C11 C10 115.9(3) . . ? C12 C11 C10 122.3(3) . . ? C3 C4 C5 119.6(3) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C13 C14 C15 118.8(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C13 C12 C11 119.6(3) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C2 C3 C4 119.0(3) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C3 C2 C1 118.2(3) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C8 C9 C10 119.4(3) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C8 C7 C6 118.9(3) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.4(3) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C14 C13 C12 118.9(3) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? Yb1 OW1 H37 116(2) . . ? Yb1 OW1 H38 120(3) . . ? H37 OW1 H38 103(4) . . ? C30 O5 Yb1 168.9(2) . . ? O6 C30 O5 126.0(3) . . ? O6 C30 C31 117.2(3) . . ? O5 C30 C31 116.8(3) . . ? C33 C32 C31 121.5(3) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C31 C36 118.8(3) . . ? C32 C31 C30 120.3(3) . . ? C36 C31 C30 120.9(3) . . ? C35 C36 C31 120.4(3) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C32 C33 C34 118.7(3) . . ? C32 C33 H33 120.7 . . ? C34 C33 H33 120.7 . . ? C36 C35 C34 120.1(3) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C35 C34 C33 120.6(3) . . ? C35 C34 Cl3 119.3(3) . . ? C33 C34 Cl3 120.1(3) . . ? _refine_diff_density_max 1.021 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.148 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.6999 13.0183 14.8094 100.207 97.549 92.530 ZERR 2.00 0.0008 0.0012 0.0014 0.001 0.001 0.001 LATT 1 SFAC C H N O CL YB UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 FMAP 2 PLAN 10 ACTA 51.00 BOND $H L.S. 12 WGHT 0.023500 FVAR 0.11587 YB1 6 0.559944 0.513275 0.701528 11.00000 0.01062 0.01041 = 0.00937 0.00197 0.00253 0.00015 O1 4 0.706755 0.621961 0.839764 11.00000 0.01583 0.01235 = 0.01552 0.00245 0.00415 0.00049 O3 4 0.560274 0.378966 0.561361 11.00000 0.01607 0.01287 = 0.01406 0.00210 0.00299 -0.00278 O2 4 0.532739 0.696607 0.754293 11.00000 0.01568 0.01397 = 0.01453 0.00157 0.00027 -0.00027 C23 1 0.458902 0.321597 0.586815 11.00000 0.01297 0.01134 = 0.01302 0.00326 -0.00140 0.00220 O4 4 0.404302 0.352007 0.661268 11.00000 0.01627 0.01659 = 0.01077 0.00012 0.00366 -0.00056 C16 1 0.637850 0.702010 0.822709 11.00000 0.01317 0.01298 = 0.01253 0.00066 0.00836 -0.00117 C24 1 0.404583 0.216533 0.528861 11.00000 0.01357 0.01077 = 0.01409 0.00126 -0.00129 0.00375 C17 1 0.680599 0.806153 0.884809 11.00000 0.01528 0.01530 = 0.01128 0.00198 0.00578 -0.00284 C20 1 0.753061 1.000034 0.997371 11.00000 0.02076 0.01673 = 0.01296 0.00204 0.00377 0.00233 C19 1 0.840023 0.916439 1.013485 11.00000 0.01422 0.01986 = 0.01742 0.00319 -0.00135 -0.00075 AFIX 43 H19 2 0.921393 0.925105 1.062236 11.00000 -1.20000 AFIX 0 C25 1 0.471857 0.179018 0.450228 11.00000 0.01216 0.02012 = 0.01879 0.00132 -0.00039 -0.00236 AFIX 43 H25 2 0.548439 0.220414 0.432709 11.00000 -1.20000 AFIX 0 C22 1 0.595246 0.891536 0.868902 11.00000 0.01632 0.01971 = 0.01343 0.00473 0.00110 0.00174 AFIX 43 H22 2 0.514003 0.882748 0.820069 11.00000 -1.20000 AFIX 0 C27 1 0.310973 0.020925 0.424625 11.00000 0.02671 0.01099 = 0.01921 0.00028 -0.00875 0.00463 C18 1 0.803693 0.819991 0.955839 11.00000 0.01986 0.01531 = 0.01666 0.00315 0.00418 0.00250 AFIX 43 H18 2 0.862840 0.763997 0.965089 11.00000 -1.20000 AFIX 0 C21 1 0.630579 0.989062 0.925195 11.00000 0.01977 0.01372 = 0.01701 0.00351 0.00108 0.00559 AFIX 43 H21 2 0.573681 1.045731 0.914885 11.00000 -1.20000 AFIX 0 C29 1 0.289965 0.154199 0.554375 11.00000 0.02060 0.01713 = 0.01649 0.00338 0.00257 0.00068 AFIX 43 H29 2 0.245499 0.178238 0.607281 11.00000 -1.20000 AFIX 0 C26 1 0.426086 0.080848 0.397844 11.00000 0.02402 0.01724 = 0.02186 -0.00376 0.00158 0.00594 AFIX 43 H26 2 0.471812 0.055677 0.345682 11.00000 -1.20000 AFIX 0 C28 1 0.241529 0.056698 0.501690 11.00000 0.02497 0.01695 = 0.02486 0.00744 -0.00184 -0.00387 AFIX 43 H28 2 0.163107 0.015768 0.518027 11.00000 -1.20000 AFIX 0 CL1 5 0.797272 1.121177 1.070143 11.00000 0.02427 0.01375 = 0.01963 -0.00009 -0.00160 0.00155 CL2 5 0.249098 -0.101566 0.358188 11.00000 0.04642 0.01681 = 0.03716 -0.00540 -0.01133 -0.00092 N1 3 0.787639 0.406703 0.722873 11.00000 0.01151 0.01022 = 0.01349 0.00092 0.00232 -0.00137 N2 3 0.566943 0.415823 0.835290 11.00000 0.01193 0.00967 = 0.00949 0.00073 0.00274 -0.00087 N3 3 0.337822 0.538391 0.793742 11.00000 0.01407 0.00865 = 0.01410 0.00145 0.00288 -0.00083 C15 1 0.226610 0.602183 0.771746 11.00000 0.01452 0.01458 = 0.01436 0.00235 0.00322 0.00098 AFIX 43 H15 2 0.235961 0.637728 0.723311 11.00000 -1.20000 AFIX 0 C5 1 0.807075 0.350695 0.792190 11.00000 0.01227 0.00994 = 0.01122 -0.00153 0.00165 -0.00075 C10 1 0.447711 0.417146 0.884457 11.00000 0.01252 0.01182 = 0.01237 0.00203 0.00416 -0.00068 C1 1 0.897108 0.405133 0.667434 11.00000 0.01672 0.01121 = 0.01353 0.00126 0.00427 -0.00054 AFIX 43 H1 2 0.882009 0.441153 0.618426 11.00000 -1.20000 AFIX 0 C6 1 0.678463 0.349331 0.848471 11.00000 0.01459 0.01220 = 0.01221 0.00128 0.00175 -0.00091 C11 1 0.324861 0.489303 0.865184 11.00000 0.00965 0.01319 = 0.01340 -0.00351 0.00101 -0.00326 C4 1 0.940093 0.297273 0.807957 11.00000 0.01770 0.01504 = 0.01254 0.00202 0.00065 0.00248 AFIX 43 H4 2 0.952490 0.260297 0.856410 11.00000 -1.20000 AFIX 0 C14 1 0.098515 0.617061 0.818436 11.00000 0.01493 0.01856 = 0.01910 0.00348 0.00312 0.00690 AFIX 43 H14 2 0.021715 0.659535 0.799999 11.00000 -1.20000 AFIX 0 C12 1 0.202820 0.504236 0.916771 11.00000 0.01640 0.01625 = 0.01653 0.00364 0.00459 -0.00091 AFIX 43 H12 2 0.198741 0.471599 0.967496 11.00000 -1.20000 AFIX 0 C3 1 1.054476 0.299514 0.750774 11.00000 0.01157 0.01387 = 0.02015 -0.00033 0.00257 0.00078 AFIX 43 H3 2 1.144909 0.265295 0.761256 11.00000 -1.20000 AFIX 0 C2 1 1.031820 0.353076 0.678532 11.00000 0.01411 0.01247 = 0.01762 0.00080 0.00593 -0.00035 AFIX 43 H2 2 1.104998 0.354319 0.638193 11.00000 -1.20000 AFIX 0 C9 1 0.437592 0.352242 0.949274 11.00000 0.01606 0.02163 = 0.01652 0.00626 0.00737 0.00364 AFIX 43 H9 2 0.355564 0.355772 0.983892 11.00000 -1.20000 AFIX 0 C7 1 0.671400 0.280502 0.910366 11.00000 0.01958 0.02075 = 0.01491 0.00837 0.00619 0.00606 AFIX 43 H7 2 0.747646 0.233470 0.917084 11.00000 -1.20000 AFIX 0 C8 1 0.549347 0.283400 0.961448 11.00000 0.02345 0.02523 = 0.02021 0.01559 0.00852 0.00647 AFIX 43 H8 2 0.543201 0.238937 1.003747 11.00000 -1.20000 AFIX 0 C13 1 0.087435 0.567883 0.892302 11.00000 0.01785 0.01825 = 0.02516 0.00333 0.01045 0.00364 AFIX 43 H13 2 0.003684 0.577258 0.925302 11.00000 -1.20000 AFIX 0 OW1 4 0.372809 0.558352 0.593667 11.00000 0.01431 0.01418 = 0.01135 0.00264 0.00142 -0.00049 O5 4 0.723782 0.596668 0.630377 11.00000 0.01578 0.01359 = 0.01486 0.00302 0.00706 -0.00122 C30 1 0.820610 0.626673 0.580938 11.00000 0.00978 0.01373 = 0.01693 0.00526 0.00033 0.00327 O6 4 0.842507 0.580314 0.503241 11.00000 0.01629 0.02023 = 0.01471 0.00054 0.00633 -0.00420 C32 1 0.868448 0.799985 0.690375 11.00000 0.01398 0.01823 = 0.01511 0.00744 0.00392 -0.00099 AFIX 43 H32 2 0.775138 0.785888 0.711532 11.00000 -1.20000 AFIX 0 C31 1 0.917402 0.727287 0.620839 11.00000 0.01078 0.01547 = 0.01188 0.00541 0.00095 0.00006 C36 1 1.056525 0.749613 0.588961 11.00000 0.01693 0.01783 = 0.01789 0.00216 0.00656 0.00026 AFIX 43 H36 2 1.089545 0.702617 0.541614 11.00000 -1.20000 AFIX 0 C33 1 0.955496 0.892610 0.728622 11.00000 0.02295 0.01711 = 0.01124 0.00264 0.00499 0.00063 AFIX 43 H33 2 0.921294 0.940654 0.774755 11.00000 -1.20000 AFIX 0 C35 1 1.145803 0.841262 0.627325 11.00000 0.01358 0.01898 = 0.02994 0.00667 0.00588 0.00070 AFIX 43 H35 2 1.239605 0.855092 0.606609 11.00000 -1.20000 AFIX 0 C34 1 1.095655 0.912508 0.696594 11.00000 0.01770 0.01545 = 0.01742 0.00492 -0.00068 -0.00347 CL3 5 1.210205 1.026786 0.744383 11.00000 0.03206 0.02092 = 0.02824 0.00156 0.00413 -0.00875 H37 2 0.410185 0.590495 0.547917 11.00000 0.03602 H38 2 0.296425 0.506853 0.558261 11.00000 0.05949 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0323 for 7623 Fo > 4sig(Fo) and 0.0416 for all 8886 data REM 459 parameters refined using 2 restraints END WGHT 0.0233 0.0000 REM Highest difference peak 1.021, deepest hole -0.660, 1-sigma level 0.148 Q1 1 0.3194 0.4591 0.8975 11.00000 0.05 1.02 Q2 1 0.1787 -0.1189 0.3985 11.00000 0.05 0.89 Q3 1 0.4847 0.3776 0.7112 11.00000 0.05 0.64 Q4 1 1.1138 1.0600 0.7602 11.00000 0.05 0.64 Q5 1 0.7862 0.9565 1.0119 11.00000 0.05 0.63 Q6 1 1.3224 1.0072 0.7292 11.00000 0.05 0.62 Q7 1 1.2557 1.0222 0.8028 11.00000 0.05 0.61 Q8 1 0.9549 0.8159 0.7789 11.00000 0.05 0.58 Q9 1 0.6542 0.5371 0.6393 11.00000 0.05 0.57 Q10 1 0.6676 0.7416 0.8694 11.00000 0.05 0.57 ; _shelx_res_checksum 70224 _shelx_hkl_file ; -1 0 0 330.00 9.64 -1 0 0 331.71 9.73 1 0 0 332.75 9.80 1 0 0 331.08 9.83 -2 0 0 2.90 0.50 -2 0 0 3.03 0.61 2 0 0 2.54 0.59 2 0 0 2.41 0.46 -3 0 0 115.89 4.21 -3 0 0 114.39 4.50 3 0 0 125.13 4.68 3 0 0 114.94 4.18 -4 0 0 2.36 0.82 -4 0 0 3.05 0.73 4 0 0 5.22 0.82 4 0 0 3.46 0.93 -5 0 0 39.41 2.37 -5 0 0 44.36 2.89 5 0 0 47.29 2.44 5 0 0 50.33 3.08 -6 0 0 84.43 4.63 -6 0 0 91.10 4.14 6 0 0 87.03 3.96 6 0 0 91.37 4.85 -7 0 0 35.03 3.04 -7 0 0 33.21 2.43 7 0 0 38.60 3.21 7 0 0 35.94 2.40 -8 0 0 153.68 7.45 8 0 0 140.58 7.40 -9 0 0 85.60 5.64 9 0 0 87.06 5.77 -10 0 0 24.93 3.37 10 0 0 27.24 3.46 -11 0 0 9.07 2.59 11 0 0 5.54 2.19 11 -1 0 14.92 3.22 -11 1 0 21.92 3.74 10 -1 0 20.09 3.02 -10 1 0 24.76 3.23 9 -1 0 49.64 4.31 -9 1 0 44.84 4.02 8 -1 0 147.78 7.55 -8 1 0 148.03 7.40 7 -1 0 68.32 3.45 7 -1 0 67.54 4.44 -7 1 0 68.25 3.63 -7 1 0 73.29 4.51 6 -1 0 7.05 1.03 6 -1 0 6.14 1.42 -6 1 0 6.38 1.48 -6 1 0 8.34 1.19 5 -1 0 0.51 0.63 5 -1 0 0.48 0.47 -5 1 0 -0.03 0.58 -5 1 0 -0.03 0.41 4 -1 0 2.35 0.81 4 -1 0 3.12 0.65 -4 1 0 4.11 0.98 -4 1 0 2.73 0.67 3 -1 0 52.48 2.75 3 -1 0 59.34 2.40 -3 1 0 58.75 2.46 2 -1 0 578.25 17.27 2 -1 0 581.21 17.20 -2 1 0 575.20 17.06 1 -1 0 430.20 12.44 1 -1 0 418.67 12.41 -1 1 0 408.98 12.25 -1 1 0 432.05 12.54 0 -1 0 400.58 11.74 -1 -1 0 272.43 8.14 -1 -1 0 282.98 8.37 1 1 0 273.18 8.27 -2 -1 0 144.80 4.78 -2 -1 0 141.86 4.72 2 1 0 133.24 4.79 2 1 0 136.86 4.75 -3 -1 0 5.88 0.83 -3 -1 0 6.76 1.05 3 1 0 6.55 0.97 3 1 0 6.95 0.86 -4 -1 0 25.58 1.99 -4 -1 0 28.41 1.79 4 1 0 27.78 2.07 4 1 0 27.64 1.76 -5 -1 0 3.32 0.84 -5 -1 0 2.86 0.93 5 1 0 2.84 0.95 5 1 0 2.65 0.77 -6 -1 0 70.76 4.09 -6 -1 0 63.91 3.43 6 1 0 65.13 4.03 6 1 0 67.10 3.41 -7 -1 0 129.02 5.70 -7 -1 0 129.73 6.38 7 1 0 138.86 6.70 7 1 0 128.41 5.57 -8 -1 0 51.29 3.38 -8 -1 0 59.50 4.28 8 1 0 53.58 4.21 -9 -1 0 69.84 5.05 9 1 0 76.28 5.35 -10 -1 0 39.49 4.05 10 1 0 44.98 4.33 -11 -1 0 28.64 3.85 11 1 0 20.82 3.73 11 -2 0 9.07 2.58 -11 2 0 18.26 3.39 10 -2 0 16.68 3.15 -10 2 0 9.67 2.54 9 -2 0 56.04 4.64 -9 2 0 56.79 4.53 8 -2 0 62.89 4.61 -8 2 0 66.43 4.64 7 -2 0 35.57 3.14 7 -2 0 36.71 2.35 -7 2 0 31.58 2.92 -7 2 0 35.75 2.50 6 -2 0 24.43 1.76 6 -2 0 24.14 2.43 -6 2 0 26.07 1.95 -6 2 0 21.00 2.25 5 -2 0 12.87 1.22 5 -2 0 10.59 1.57 -5 2 0 11.82 1.59 -5 2 0 11.23 1.24 4 -2 0 22.44 1.44 4 -2 0 21.66 1.88 -4 2 0 20.89 1.88 -4 2 0 20.92 1.48 3 -2 0 12.70 1.29 -3 2 0 10.19 1.00 -3 2 0 13.62 1.05 -3 2 0 12.63 1.10 -3 2 0 12.39 1.25 2 -2 0 4.08 0.64 2 -2 0 2.99 0.66 -2 2 0 5.02 0.84 -2 2 0 4.59 0.67 1 -2 0 201.26 6.25 1 -2 0 191.80 6.30 -1 2 0 198.57 6.35 -1 2 0 199.83 6.19 0 -2 0 387.07 11.07 0 -2 0 374.41 11.49 0 2 0 370.86 11.62 0 2 0 386.50 10.96 -1 -2 0 194.77 6.36 -1 -2 0 191.91 5.98 1 2 0 199.94 6.49 1 2 0 195.54 6.08 -2 -2 0 1.95 0.59 -2 -2 0 2.27 0.59 2 2 0 1.54 0.54 2 2 0 2.04 0.59 -3 -2 0 81.77 3.52 -3 -2 0 84.60 3.52 3 2 0 83.51 3.62 3 2 0 83.29 3.53 -4 -2 0 2.37 0.75 -4 -2 0 1.67 0.68 4 2 0 2.81 0.83 4 2 0 2.26 0.71 -5 -2 0 90.04 4.36 -5 -2 0 91.20 4.15 5 2 0 89.47 4.10 5 2 0 84.94 4.40 -6 -2 0 67.55 4.09 -6 -2 0 76.65 3.88 6 2 0 76.05 3.83 6 2 0 76.99 4.34 -7 -2 0 57.90 3.46 -7 -2 0 62.57 4.12 7 2 0 55.82 3.33 7 2 0 54.12 3.91 -8 -2 0 28.70 2.56 -8 -2 0 29.53 3.04 8 2 0 25.12 2.89 -9 -2 0 89.34 5.78 9 2 0 82.91 5.70 -10 -2 0 26.78 3.44 10 2 0 22.39 3.19 -11 -2 0 7.67 2.60 11 2 0 8.62 2.63 11 -3 0 17.38 3.37 -11 3 0 16.74 3.23 10 -3 0 20.59 3.07 -10 3 0 26.96 3.33 9 -3 0 35.94 3.84 -9 3 0 37.78 3.80 8 -3 0 105.52 6.33 -8 3 0 122.94 6.56 7 -3 0 15.75 1.76 7 -3 0 18.09 2.30 -7 3 0 16.67 2.14 6 -3 0 1.05 0.66 6 -3 0 1.03 0.86 -6 3 0 1.55 0.73 -6 3 0 3.10 1.13 -6 3 0 1.13 0.61 5 -3 0 0.56 0.52 5 -3 0 -0.51 0.49 -5 3 0 0.98 0.75 -5 3 0 0.22 0.52 -5 3 0 0.23 0.50 4 -3 0 0.60 0.49 4 -3 0 0.73 0.63 -4 3 0 0.78 0.54 -4 3 0 0.96 0.50 -4 3 0 1.05 0.70 3 -3 0 69.02 3.07 3 -3 0 74.76 3.45 -3 3 0 70.81 3.36 -3 3 0 71.51 3.01 2 -3 0 103.57 4.03 2 -3 0 104.97 4.10 -2 3 0 110.84 4.02 -2 3 0 107.66 4.13 1 -3 0 58.90 2.67 1 -3 0 67.74 2.56 -1 3 0 58.83 2.65 -1 3 0 67.91 2.60 0 -3 0 33.49 1.46 0 -3 0 31.73 1.78 0 3 0 31.24 1.49 0 3 0 36.23 1.92 -1 -3 0 177.23 6.16 -1 -3 0 171.22 5.61 1 3 0 176.93 5.68 1 3 0 187.97 6.32 -2 -3 0 3.69 0.71 -2 -3 0 2.36 0.66 2 3 0 2.94 0.67 2 3 0 2.94 0.76 -3 -3 0 16.83 1.43 -3 -3 0 17.32 1.54 3 3 0 17.12 1.49 3 3 0 18.22 1.49 -4 -3 0 7.26 1.22 -4 -3 0 8.01 1.22 4 3 0 10.18 1.32 4 3 0 7.53 1.18 -5 -3 0 21.52 1.98 -5 -3 0 26.05 2.03 5 3 0 25.35 2.16 5 3 0 22.37 1.95 -6 -3 0 54.39 3.55 -6 -3 0 56.37 3.39 6 3 0 58.04 3.38 6 3 0 55.57 3.67 -7 -3 0 138.23 6.32 -7 -3 0 150.02 6.97 7 3 0 137.47 6.29 7 3 0 146.24 6.99 -8 -3 0 7.45 1.82 -8 -3 0 8.88 1.77 8 3 0 5.35 1.60 -9 -3 0 39.30 3.79 9 3 0 39.48 3.80 -10 -3 0 15.36 2.90 10 3 0 14.26 2.97 -11 -3 0 -1.28 1.33 11 3 0 -0.55 1.28 11 -4 0 11.81 2.98 -11 4 0 14.97 3.19 10 -4 0 50.32 4.64 -10 4 0 41.88 4.26 9 -4 0 65.56 4.98 -9 4 0 56.61 4.61 8 -4 0 55.57 4.34 -8 4 0 54.70 4.21 7 -4 0 7.17 1.83 7 -4 0 7.34 1.42 -7 4 0 2.86 1.19 6 -4 0 2.87 0.92 6 -4 0 2.89 1.13 -6 4 0 2.03 0.76 -6 4 0 1.78 0.98 5 -4 0 1.00 0.66 5 -4 0 1.07 0.79 -5 4 0 1.05 0.57 -5 4 0 0.50 0.68 4 -4 0 0.15 0.53 4 -4 0 0.12 0.56 -4 4 0 -0.25 0.44 -4 4 0 0.30 0.56 3 -4 0 3.85 0.90 3 -4 0 2.65 0.74 -3 4 0 5.48 1.03 -3 4 0 5.15 0.91 2 -4 0 184.56 6.22 2 -4 0 169.43 6.03 -2 4 0 161.61 6.06 -2 4 0 163.68 5.98 1 -4 0 155.13 5.63 1 -4 0 150.93 5.19 -1 4 0 149.57 5.62 -1 4 0 154.33 5.27 0 -4 0 5.94 0.97 0 -4 0 6.29 0.74 0 4 0 4.82 0.74 0 4 0 5.17 0.95 -1 -4 0 151.18 5.77 1 4 0 159.90 5.18 -2 -4 0 101.84 3.75 -2 -4 0 89.42 4.08 2 4 0 96.25 3.76 2 4 0 94.17 4.19 -3 -4 0 5.77 1.14 -3 -4 0 6.96 1.06 3 4 0 6.09 1.19 3 4 0 6.42 1.03 -4 -4 0 10.99 1.35 -4 -4 0 10.62 1.36 4 4 0 7.61 1.33 4 4 0 8.20 1.29 -5 -4 0 15.07 1.70 -5 -4 0 15.82 1.74 5 4 0 11.22 1.56 5 4 0 11.36 1.60 -6 -4 0 80.50 4.28 -6 -4 0 73.46 4.25 6 4 0 73.91 4.40 6 4 0 78.48 4.29 -7 -4 0 39.15 3.19 -7 -4 0 35.79 2.92 7 4 0 34.92 3.08 7 4 0 33.76 2.80 -8 -4 0 24.50 2.82 -8 -4 0 30.31 2.79 8 4 0 30.06 2.75 8 4 0 24.85 2.85 -9 -4 0 32.62 3.46 9 4 0 36.13 3.70 -10 -4 0 23.51 3.35 10 4 0 19.87 3.44 -11 -4 0 -1.11 1.47 11 4 0 -0.21 1.41 11 -5 0 16.51 3.46 -11 5 0 19.11 3.51 10 -5 0 77.80 5.96 -10 5 0 64.17 5.38 9 -5 0 48.94 4.44 -9 5 0 50.71 4.34 8 -5 0 35.70 3.50 -8 5 0 37.14 3.49 7 -5 0 5.71 1.54 7 -5 0 7.42 1.50 -7 5 0 11.96 2.19 6 -5 0 13.90 1.63 6 -5 0 12.73 1.84 -6 5 0 12.90 1.89 -6 5 0 13.94 1.58 5 -5 0 -0.53 0.53 5 -5 0 -0.47 0.52 -5 5 0 0.27 0.63 -5 5 0 1.37 0.81 4 -5 0 99.78 4.82 4 -5 0 105.10 4.62 -4 5 0 107.23 4.50 -4 5 0 102.41 4.84 3 -5 0 6.93 1.20 3 -5 0 5.48 1.06 -3 5 0 6.63 1.15 -3 5 0 8.19 1.18 2 -5 0 103.33 4.14 2 -5 0 94.78 4.28 -2 5 0 101.33 4.31 -2 5 0 99.43 4.12 1 -5 0 207.13 7.16 1 -5 0 201.21 6.53 -1 5 0 199.22 6.59 -1 5 0 162.28 6.89 0 -5 0 94.96 4.27 0 -5 0 99.37 3.64 0 5 0 100.95 3.73 0 5 0 96.36 4.32 -1 -5 0 33.03 2.23 -1 -5 0 31.85 1.70 1 5 0 33.55 1.77 1 5 0 34.42 2.31 -2 -5 0 192.13 6.71 -2 -5 0 208.07 7.57 2 5 0 195.18 7.57 2 5 0 202.22 6.81 -3 -5 0 9.60 1.22 -3 -5 0 12.27 1.55 3 5 0 11.57 1.53 3 5 0 15.01 1.42 -4 -5 0 43.53 2.87 -4 -5 0 38.78 2.54 4 5 0 37.06 2.52 4 5 0 39.71 2.75 -5 -5 0 34.47 2.62 -5 -5 0 29.81 2.42 5 5 0 28.93 2.50 5 5 0 34.14 2.57 -6 -5 0 48.99 3.38 -6 -5 0 52.91 3.49 6 5 0 44.33 3.31 6 5 0 47.13 3.35 -7 -5 0 34.29 3.04 -7 -5 0 37.45 3.08 7 5 0 29.97 3.00 7 5 0 34.52 2.99 -8 -5 0 79.69 4.82 -8 -5 0 74.82 5.01 8 5 0 81.74 5.27 8 5 0 75.75 4.74 -9 -5 0 12.58 2.53 9 5 0 14.94 2.73 -10 -5 0 9.42 2.50 10 5 0 12.56 2.84 -11 -5 0 1.45 1.86 11 5 0 -0.82 1.53 11 -6 0 21.88 4.00 -11 6 0 17.86 3.63 10 -6 0 28.53 3.72 -10 6 0 25.65 3.46 9 -6 0 30.16 3.57 -9 6 0 34.53 3.69 8 -6 0 45.10 4.03 -8 6 0 43.19 3.89 7 -6 0 14.96 2.32 7 -6 0 15.21 1.90 -7 6 0 17.63 2.39 6 -6 0 22.80 2.48 6 -6 0 25.16 2.23 -6 6 0 21.75 2.47 -6 6 0 21.35 1.95 5 -6 0 5.37 1.23 5 -6 0 4.65 1.33 -5 6 0 4.17 1.09 -5 6 0 4.02 1.20 4 -6 0 26.05 2.23 4 -6 0 30.79 2.31 -4 6 0 30.07 2.38 -4 6 0 28.78 2.16 3 -6 0 144.71 6.16 3 -6 0 151.31 6.10 -3 6 0 157.64 6.19 -3 6 0 161.94 6.27 2 -6 0 97.03 4.14 2 -6 0 92.47 4.43 -2 6 0 100.58 4.54 -2 6 0 102.03 4.27 1 -6 0 29.20 1.81 1 -6 0 30.95 2.28 -1 6 0 29.29 2.21 -1 6 0 32.51 1.97 0 -6 0 68.44 2.87 0 -6 0 63.83 3.47 0 6 0 64.30 2.89 0 6 0 68.05 3.61 -1 -6 0 402.20 14.02 -1 -6 0 431.58 12.99 1 6 0 421.67 12.88 1 6 0 425.22 14.35 -2 -6 0 5.93 0.99 -2 -6 0 6.57 1.31 2 6 0 7.29 1.37 2 6 0 6.92 1.05 -3 -6 0 39.58 2.84 -3 -6 0 39.18 2.40 3 6 0 45.68 3.03 3 6 0 42.54 2.49 -4 -6 0 5.74 1.40 -4 -6 0 6.15 1.24 4 6 0 5.61 1.17 4 6 0 5.33 1.31 -5 -6 0 60.41 3.63 -5 -6 0 64.93 3.98 5 6 0 67.23 3.80 5 6 0 65.18 4.02 -6 -6 0 48.07 3.34 -6 -6 0 47.07 3.43 6 6 0 38.12 3.18 6 6 0 42.32 3.19 -7 -6 0 46.13 3.56 -7 -6 0 48.50 3.64 7 6 0 50.61 3.76 7 6 0 49.44 3.80 -8 -6 0 55.81 4.20 -8 -6 0 55.85 4.26 8 6 0 49.82 3.95 8 6 0 61.11 4.46 -9 -6 0 38.65 3.78 9 6 0 38.54 3.84 -10 -6 0 7.92 2.38 10 6 0 8.87 2.49 10 -7 0 39.14 4.38 -10 7 0 37.89 4.19 9 -7 0 41.13 4.12 -9 7 0 40.93 4.05 8 -7 0 -0.19 1.03 -8 7 0 3.04 1.51 7 -7 0 35.21 3.28 7 -7 0 29.25 2.65 -7 7 0 29.69 3.14 6 -7 0 5.34 1.59 6 -7 0 6.24 1.47 -6 7 0 4.28 1.37 -6 7 0 7.10 1.42 5 -7 0 38.46 2.98 5 -7 0 37.27 2.79 -5 7 0 37.43 3.01 -5 7 0 37.12 2.67 4 -7 0 102.55 4.95 4 -7 0 101.97 4.95 -4 7 0 99.61 4.94 -4 7 0 97.53 4.74 3 -7 0 37.75 2.54 3 -7 0 40.79 2.81 -3 7 0 37.14 2.62 -3 7 0 39.75 2.73 2 -7 0 87.97 4.04 2 -7 0 85.82 4.47 -2 7 0 94.75 4.25 -2 7 0 102.31 4.75 1 -7 0 355.71 12.50 1 -7 0 364.56 11.51 -1 7 0 367.71 11.58 -1 7 0 337.17 12.52 0 -7 0 51.28 2.53 0 -7 0 53.66 3.28 0 7 0 54.73 2.69 0 7 0 53.25 3.37 -1 -7 0 1.49 0.55 -1 -7 0 0.77 0.68 1 7 0 1.12 0.52 1 7 0 -0.11 0.56 -2 -7 0 20.42 2.13 -2 -7 0 23.59 1.74 2 7 0 24.58 2.28 2 7 0 20.35 1.63 -3 -7 0 -0.08 0.53 -3 -7 0 0.19 0.63 3 7 0 -0.21 0.50 3 7 0 -0.15 0.58 -4 -7 0 79.68 4.66 -4 -7 0 90.97 4.24 4 7 0 77.72 4.08 4 7 0 85.79 4.80 -5 -7 0 134.65 6.58 -5 -7 0 137.03 6.02 5 7 0 132.83 6.04 5 7 0 137.38 6.71 -6 -7 0 44.43 3.42 -6 -7 0 36.65 3.05 6 7 0 36.13 3.27 6 7 0 41.93 3.20 -7 -7 0 104.76 5.70 -7 -7 0 102.65 5.89 7 7 0 116.17 6.08 7 7 0 103.09 5.99 -8 -7 0 124.60 6.47 -8 -7 0 105.92 6.25 8 7 0 111.74 6.44 8 7 0 108.69 6.29 9 7 0 11.62 2.55 10 -8 0 30.12 3.89 -10 8 0 31.56 3.86 9 -8 0 35.85 3.88 -9 8 0 36.31 3.92 8 -8 0 67.82 5.06 -8 8 0 61.06 4.83 7 -8 0 6.67 1.87 -7 8 0 6.85 1.81 6 -8 0 0.64 0.85 6 -8 0 -0.51 0.68 -6 8 0 0.94 0.95 -6 8 0 0.23 0.81 5 -8 0 0.76 0.84 5 -8 0 0.48 0.86 -5 8 0 1.96 1.02 -5 8 0 1.28 0.88 4 -8 0 103.91 5.34 4 -8 0 106.49 5.20 -4 8 0 111.08 5.32 -4 8 0 109.52 5.35 3 -8 0 243.62 9.08 3 -8 0 246.13 9.60 -3 8 0 259.71 9.71 -3 8 0 246.47 9.24 2 -8 0 41.24 2.52 2 -8 0 36.86 2.91 -2 8 0 42.71 2.72 -2 8 0 45.27 3.07 1 -8 0 29.39 1.94 1 -8 0 22.34 2.26 -1 8 0 27.46 2.01 -1 8 0 22.53 2.27 0 -8 0 127.65 4.88 0 8 0 125.86 6.00 0 8 0 124.72 4.97 -1 -8 0 57.64 2.84 -1 -8 0 65.65 3.91 1 8 0 51.04 3.61 1 8 0 62.40 2.98 -2 -8 0 13.07 1.80 -2 -8 0 15.82 1.53 2 8 0 12.75 1.84 2 8 0 15.74 1.49 -3 -8 0 75.37 3.68 -3 -8 0 66.16 4.24 3 8 0 75.86 3.68 3 8 0 73.54 4.50 -4 -8 0 20.96 2.38 -4 -8 0 18.90 1.95 4 8 0 15.72 1.76 4 8 0 20.29 2.36 -5 -8 0 82.24 4.40 -5 -8 0 79.75 4.90 5 8 0 82.06 4.39 5 8 0 72.89 4.79 -6 -8 0 90.56 5.49 -6 -8 0 100.27 5.19 6 8 0 96.65 5.71 6 8 0 90.15 5.06 -7 -8 0 43.31 3.79 -7 -8 0 42.88 3.48 7 8 0 44.88 3.68 7 8 0 41.14 3.80 -8 -8 0 20.78 2.69 8 8 0 20.29 2.83 10 -9 0 37.73 4.31 -10 9 0 33.09 4.10 9 -9 0 52.56 4.85 -9 9 0 51.75 4.73 8 -9 0 27.45 3.37 -8 9 0 28.81 3.42 7 -9 0 31.03 3.27 -7 9 0 32.06 3.36 6 -9 0 -0.91 0.79 6 -9 0 0.20 0.98 -6 9 0 1.78 1.18 5 -9 0 60.40 4.13 5 -9 0 63.57 4.16 -5 9 0 69.64 4.39 -5 9 0 72.18 4.22 4 -9 0 29.24 2.60 4 -9 0 35.23 2.91 -4 9 0 30.29 2.66 -4 9 0 32.38 2.80 3 -9 0 76.26 4.44 3 -9 0 68.94 3.82 -3 9 0 72.36 4.02 -3 9 0 64.22 4.09 2 -9 0 109.59 4.90 2 -9 0 112.55 5.75 -2 9 0 111.31 5.08 -2 9 0 114.96 5.79 1 -9 0 91.62 5.03 1 -9 0 82.29 3.92 -1 9 0 90.60 4.19 -1 9 0 94.38 5.12 0 -9 0 54.05 3.67 0 -9 0 47.85 2.59 0 9 0 45.45 3.41 0 9 0 43.05 2.66 -1 -9 0 12.10 1.28 -1 -9 0 7.85 1.69 1 9 0 9.10 1.87 1 9 0 8.87 1.23 -2 -9 0 2.03 0.79 -2 -9 0 1.49 0.97 2 9 0 1.88 0.78 2 9 0 3.01 1.20 -3 -9 0 0.39 0.83 -3 -9 0 0.73 0.68 3 9 0 0.52 0.68 3 9 0 0.25 0.85 -4 -9 0 23.33 2.15 -4 -9 0 16.73 2.24 4 9 0 18.78 1.93 4 9 0 13.53 2.16 -5 -9 0 37.05 3.40 -5 -9 0 30.01 2.65 5 9 0 28.61 3.03 -6 -9 0 33.91 3.39 6 9 0 30.48 3.29 -7 -9 0 24.32 2.92 7 9 0 19.98 2.91 -8 -9 0 45.03 4.11 8 9 0 43.77 4.23 10 -10 0 20.55 3.85 -10 10 0 30.22 4.05 9 -10 0 48.38 4.61 -9 10 0 35.98 4.19 8 -10 0 11.95 2.61 -8 10 0 7.99 2.18 7 -10 0 0.92 1.30 -7 10 0 1.80 1.39 6 -10 0 2.07 1.16 6 -10 0 5.54 1.71 -6 10 0 2.41 1.27 5 -10 0 19.73 2.35 5 -10 0 16.82 2.33 -5 10 0 19.05 2.47 -5 10 0 20.81 2.42 4 -10 0 66.69 4.12 4 -10 0 71.41 4.63 -4 10 0 75.86 4.58 -4 10 0 72.67 4.43 3 -10 0 74.60 4.04 3 -10 0 77.48 4.73 -3 10 0 72.41 4.20 -3 10 0 65.25 4.45 2 -10 0 44.10 3.50 2 -10 0 38.37 2.67 -2 10 0 44.23 3.50 -2 10 0 37.37 2.79 1 -10 0 84.61 4.00 1 -10 0 84.92 5.04 -1 10 0 83.01 5.03 -1 10 0 87.90 4.24 0 -10 0 153.92 5.98 0 -10 0 161.02 7.57 0 10 0 140.19 7.29 0 10 0 157.69 6.18 -1 -10 0 8.62 1.25 -1 -10 0 10.57 2.05 1 10 0 6.12 1.62 1 10 0 9.80 1.34 -2 -10 0 0.44 0.80 -2 -10 0 1.02 0.75 2 10 0 0.84 0.94 -3 -10 0 -0.20 0.85 -3 -10 0 0.90 0.83 3 10 0 -0.54 0.97 -4 -10 0 16.31 2.35 4 10 0 13.82 2.58 -5 -10 0 38.11 3.61 5 10 0 41.40 3.74 -6 -10 0 66.70 4.97 6 10 0 63.91 4.91 -7 -10 0 33.30 3.59 7 10 0 30.00 3.52 -8 -10 0 10.65 2.50 8 10 0 17.41 3.16 9 -11 0 26.90 3.67 -9 11 0 23.98 3.57 8 -11 0 13.62 2.75 -8 11 0 16.16 3.02 7 -11 0 1.25 1.33 -7 11 0 1.11 1.34 6 -11 0 0.58 1.17 6 -11 0 1.69 1.23 -6 11 0 0.90 1.20 5 -11 0 0.72 1.11 5 -11 0 3.82 1.41 -5 11 0 2.08 1.26 -5 11 0 0.02 1.06 4 -11 0 34.69 3.32 4 -11 0 33.54 2.90 -4 11 0 33.76 3.26 -4 11 0 33.07 3.02 3 -11 0 130.22 6.05 3 -11 0 136.76 7.06 -3 11 0 135.73 6.96 -3 11 0 130.33 6.24 2 -11 0 86.74 5.30 2 -11 0 81.21 4.23 -2 11 0 81.91 5.22 -2 11 0 82.52 4.48 1 -11 0 57.21 3.25 1 -11 0 56.72 4.27 -1 11 0 53.83 4.18 -1 11 0 60.88 3.52 0 -11 0 15.74 2.29 0 11 0 14.13 2.23 0 11 0 14.21 1.71 -1 -11 0 0.25 0.92 1 11 0 3.71 1.06 1 11 0 2.21 1.34 -2 -11 0 3.51 1.39 2 11 0 4.73 1.56 -3 -11 0 7.20 1.95 3 11 0 6.50 1.94 -4 -11 0 9.00 2.12 4 11 0 6.10 1.93 -5 -11 0 32.11 3.46 5 11 0 33.61 3.53 -6 -11 0 38.65 3.89 6 11 0 41.57 4.05 -7 -11 0 43.88 4.29 7 11 0 44.43 4.44 -8 -11 0 21.65 3.30 8 11 0 21.51 3.32 9 -12 0 9.65 2.78 -9 12 0 7.05 2.44 8 -12 0 2.16 1.66 -8 12 0 0.07 1.42 7 -12 0 6.09 2.05 -7 12 0 1.84 1.56 6 -12 0 4.63 1.79 6 -12 0 6.64 1.91 -6 12 0 11.19 2.43 5 -12 0 36.45 3.29 5 -12 0 38.14 3.69 -5 12 0 40.04 3.57 -5 12 0 35.41 3.47 4 -12 0 35.16 3.57 4 -12 0 32.76 2.98 -4 12 0 30.68 3.05 -4 12 0 42.48 3.71 3 -12 0 37.12 3.57 -3 12 0 41.42 3.30 -3 12 0 43.96 3.89 2 -12 0 110.86 6.29 -2 12 0 89.44 4.98 -2 12 0 106.42 6.22 1 -12 0 52.00 4.16 -1 12 0 42.42 3.92 -1 12 0 38.85 2.97 0 -12 0 14.76 2.37 0 12 0 20.97 2.79 -1 -12 0 1.67 1.17 1 12 0 0.45 1.02 -2 -12 0 5.28 1.78 2 12 0 4.33 1.61 -3 -12 0 3.78 1.60 3 12 0 4.34 1.66 -4 -12 0 18.26 2.75 4 12 0 22.62 3.18 -5 -12 0 32.98 3.77 5 12 0 37.60 3.90 -6 -12 0 74.74 5.68 6 12 0 65.25 5.45 -7 -12 0 39.62 4.21 7 12 0 30.37 3.96 -8 -12 0 2.74 1.97 8 12 0 5.76 2.40 -8 13 0 5.64 2.38 -7 13 0 10.52 2.67 6 -13 0 3.18 1.68 -6 13 0 7.38 2.17 5 -13 0 1.43 1.42 -5 13 0 1.19 1.27 -5 13 0 1.04 1.26 4 -13 0 60.01 4.85 -4 13 0 60.27 4.78 -4 13 0 61.95 4.43 3 -13 0 85.87 5.79 -3 13 0 83.39 5.66 2 -13 0 49.60 4.31 -2 13 0 48.40 4.26 1 -13 0 27.24 3.25 -1 13 0 26.80 3.32 0 -13 0 43.04 4.04 0 13 0 36.57 3.80 -1 -13 0 0.60 1.12 1 13 0 1.91 1.34 -2 -13 0 21.69 3.05 2 13 0 26.16 3.36 -3 -13 0 9.41 2.36 3 13 0 11.64 2.64 -4 -13 0 38.55 3.99 4 13 0 33.29 3.88 -5 -13 0 61.45 5.23 5 13 0 55.33 5.06 -6 -13 0 25.46 3.56 6 13 0 33.29 4.09 -7 -13 0 34.20 4.18 7 13 0 20.98 3.84 -8 14 0 6.03 2.23 -7 14 0 6.08 2.12 5 -14 0 21.47 3.10 4 -14 0 2.80 1.59 -4 14 0 1.71 1.58 3 -14 0 52.05 4.72 -3 14 0 60.71 4.96 2 -14 0 79.08 5.82 -2 14 0 71.62 5.56 1 -14 0 11.62 2.64 -1 14 0 22.38 3.11 0 -14 0 6.32 2.05 0 14 0 6.02 2.08 -1 -14 0 4.71 1.86 1 14 0 4.68 1.92 -2 -14 0 1.82 1.39 2 14 0 0.17 1.15 -3 -14 0 46.04 4.50 3 14 0 48.23 4.77 -4 -14 0 41.76 4.33 4 14 0 34.04 4.19 -5 -14 0 35.39 4.23 5 14 0 34.11 4.23 -6 -14 0 42.43 4.74 6 14 0 40.22 4.67 5 -15 0 13.54 2.99 4 -15 0 44.16 4.50 -4 15 0 52.55 4.83 3 -15 0 43.30 4.54 -3 15 0 46.89 4.52 2 -15 0 42.24 4.29 -2 15 0 34.39 3.98 1 -15 0 33.03 3.87 -1 15 0 28.31 3.74 0 -15 0 16.10 3.15 0 15 0 12.48 2.89 -1 -15 0 3.24 1.64 1 15 0 2.89 1.80 -2 -15 0 9.82 2.68 2 15 0 4.45 2.17 -3 -15 0 22.22 3.37 3 15 0 16.97 3.44 -4 -15 0 14.08 3.13 4 15 0 30.02 3.98 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-5 0 18 6.55 2.50 4 0 -18 20.63 3.62 -4 0 18 17.77 3.45 -4 0 18 11.21 3.11 3 0 -18 27.16 3.60 -3 0 18 35.09 4.38 -3 0 18 37.02 4.20 2 0 -18 41.48 4.18 -2 0 18 37.80 4.17 -2 0 18 50.22 4.97 1 0 -18 10.52 2.56 -1 0 18 12.14 2.70 0 0 -18 19.50 3.07 0 0 18 20.36 3.23 -1 0 -18 10.28 2.57 1 0 18 10.50 2.65 -2 0 -18 0.86 1.61 2 0 18 2.50 1.82 -3 0 -18 3.47 1.93 3 0 18 4.67 2.30 6 -1 -18 0.34 1.53 5 -1 -18 21.24 3.32 -5 1 18 15.22 3.34 -5 1 18 17.05 3.77 4 -1 -18 36.32 4.11 -4 1 18 36.71 4.38 -4 1 18 34.93 4.59 3 -1 -18 16.49 3.25 -3 1 18 24.31 3.53 2 -1 -18 24.05 3.46 -2 1 18 17.02 3.29 1 -1 -18 9.46 2.62 -1 1 18 9.95 2.65 0 1 18 0.69 1.45 -1 -1 -18 5.66 2.21 1 1 18 3.81 2.08 -2 -1 -18 1.50 1.76 2 1 18 0.52 1.61 -3 -1 -18 15.24 3.27 3 1 18 5.75 2.33 6 -2 -18 4.57 2.23 5 -2 -18 24.13 3.59 -5 2 18 20.97 3.86 -5 2 18 24.02 4.01 4 -2 -18 33.78 4.20 -4 2 18 29.13 4.05 3 -2 -18 23.22 3.46 -3 2 18 32.61 4.08 2 -2 -18 11.31 2.81 -2 2 18 8.74 2.55 1 -2 -18 56.85 5.17 -1 2 18 57.77 5.18 -1 -2 -18 -0.30 1.50 1 2 18 -1.05 1.34 -2 -2 -18 1.11 1.69 2 2 18 1.67 1.78 5 -3 -18 24.29 3.71 4 -3 -18 15.99 3.51 -4 3 18 11.99 3.12 3 -3 -18 28.93 4.00 -3 3 18 23.28 3.63 2 -3 -18 34.31 4.13 -2 3 18 31.37 4.12 1 -3 -18 32.77 4.15 -1 3 18 18.96 3.54 -1 -3 -18 2.71 1.88 1 3 18 1.80 1.80 -2 -3 -18 5.17 2.22 3 -4 -18 20.73 3.86 -3 4 18 30.57 4.20 2 -4 -18 26.63 3.77 -2 4 18 14.25 3.23 1 -4 -18 46.27 4.87 -1 4 18 50.76 5.05 -1 -4 -18 0.06 1.59 -2 -4 -18 0.29 1.57 -2 5 18 42.07 4.89 -1 5 18 22.89 3.70 -1 6 18 3.90 2.34 0 -10 19 4.17 2.37 3 9 -19 15.48 3.47 -2 -9 19 38.84 4.45 0 9 -19 0.49 1.57 0 -9 19 -0.54 1.77 1 -9 19 1.34 1.98 4 8 -19 28.45 4.09 3 8 -19 17.53 3.45 -3 -8 19 19.70 3.65 -2 -8 19 21.46 3.80 0 8 -19 0.36 1.72 0 -8 19 2.71 2.02 -1 8 -19 17.27 3.36 1 -8 19 9.85 2.88 -2 8 -19 8.68 2.70 4 7 -19 17.86 3.50 -4 -7 19 18.42 3.61 3 7 -19 28.45 3.82 -3 -7 19 23.29 3.92 -2 -7 19 9.81 2.75 -1 -7 19 13.18 3.08 0 7 -19 0.94 1.43 0 -7 19 2.35 1.96 -1 7 -19 9.80 2.68 1 -7 19 9.02 2.62 2 -7 19 10.83 3.13 -5 -6 19 22.34 3.93 4 6 -19 25.94 3.77 -4 -6 19 17.22 3.44 3 6 -19 50.73 4.93 -3 -6 19 48.89 4.78 -2 -6 19 9.37 2.59 -1 -6 19 9.46 2.60 0 6 -19 0.63 1.56 0 -6 19 -0.51 1.33 1 -6 19 9.01 2.67 2 -6 19 18.42 3.75 5 5 -19 36.71 4.56 -5 -5 19 59.95 5.27 4 5 -19 39.29 4.46 -4 -5 19 39.17 4.29 3 5 -19 17.62 3.53 -3 -5 19 18.06 3.30 -2 -5 19 22.98 3.29 0 -5 19 1.04 1.75 1 -5 19 16.80 3.37 2 -5 19 10.38 3.12 -6 -4 19 29.33 4.06 5 4 -19 30.49 4.12 -5 -4 19 27.27 3.73 4 4 -19 23.61 3.62 -4 -4 19 20.99 3.25 -2 -4 19 8.71 2.44 -2 -4 19 12.62 3.04 0 -4 19 -0.07 1.44 1 -4 19 0.60 1.53 -2 4 -19 21.73 3.90 -3 -3 19 11.65 3.05 -3 -3 19 9.34 2.62 -2 -3 19 24.95 3.72 -2 -3 19 20.87 3.29 -1 3 -19 7.81 2.52 1 -3 19 11.78 2.75 -2 3 -19 8.24 2.64 2 -3 19 4.53 2.20 3 -3 19 49.54 5.06 -5 -2 19 9.67 3.04 -5 -2 19 15.69 3.80 -4 -2 19 47.20 4.90 -4 -2 19 30.29 4.42 -3 -2 19 26.15 3.73 -3 -2 19 21.53 3.79 2 2 -19 0.88 1.47 -2 -2 19 5.41 2.19 -2 -2 19 3.67 2.03 -1 -2 19 -0.47 1.25 0 -2 19 -0.22 1.33 -1 2 -19 3.48 1.90 1 -2 19 3.81 2.04 -2 2 -19 20.08 3.66 2 -2 19 26.22 3.75 3 -2 19 22.23 4.06 5 1 -19 34.96 4.05 -5 -1 19 18.79 3.86 -5 -1 19 26.71 4.29 4 1 -19 21.52 3.28 -4 -1 19 19.23 3.79 -4 -1 19 22.84 3.93 3 1 -19 23.15 3.47 -3 -1 19 16.86 3.39 -3 -1 19 19.32 3.88 2 1 -19 18.04 3.32 -2 -1 19 16.53 3.54 -2 -1 19 11.97 2.91 0 -1 19 10.02 2.63 -1 1 -19 1.62 1.64 1 -1 19 2.84 1.93 -2 1 -19 19.78 3.77 2 -1 19 16.88 3.51 6 0 -19 31.43 4.13 5 0 -19 34.44 4.26 4 0 -19 54.58 5.17 -4 0 19 44.09 5.24 -4 0 19 49.19 5.13 3 0 -19 1.72 1.76 -3 0 19 4.00 1.94 -3 0 19 2.29 1.90 2 0 -19 -0.25 1.37 -2 0 19 -0.83 1.48 1 0 -19 0.81 1.47 0 0 19 7.91 2.53 -1 0 -19 25.10 3.67 1 0 19 20.56 3.89 -2 0 -19 24.17 3.77 2 0 19 24.33 3.68 5 -1 -19 40.71 4.63 4 -1 -19 12.77 3.15 -4 1 19 18.45 3.65 3 -1 -19 3.21 1.98 -3 1 19 2.24 1.91 2 -1 -19 -0.17 1.47 -2 1 19 0.54 1.58 1 -1 -19 1.13 1.69 0 1 19 3.20 1.94 -1 -1 -19 12.15 3.01 1 1 19 12.73 3.18 -2 -1 -19 23.92 3.81 4 -2 -19 10.63 2.90 3 -2 -19 3.48 1.86 -3 2 19 3.50 2.23 2 -2 -19 0.74 1.67 -2 2 19 0.31 1.73 1 -2 -19 3.60 2.05 -1 2 19 6.33 2.33 0 2 19 20.02 3.85 -1 -2 -19 17.01 3.42 -3 3 19 -1.50 1.56 -2 3 19 -0.35 1.56 -1 3 19 1.79 1.95 -2 4 19 0.27 1.79 -1 4 19 10.75 3.09 -3 -7 20 -1.02 1.69 -2 -7 20 8.46 2.71 -1 -7 20 4.33 2.18 -4 -6 20 0.68 1.79 3 6 -20 -0.18 1.68 -3 -6 20 0.38 1.81 -2 -6 20 3.26 1.98 1 -6 20 46.89 5.04 3 5 -20 5.68 2.33 1 -5 20 22.29 3.94 -3 -4 20 8.74 3.02 -3 -4 20 4.66 2.36 1 -4 20 10.41 3.05 -4 -3 20 1.12 1.85 -4 -3 20 4.31 2.46 -3 -3 20 2.68 1.99 -3 -3 20 1.52 1.92 -1 3 -20 43.20 4.75 -4 -2 20 0.75 1.99 -4 -2 20 2.55 2.31 -3 -2 20 2.96 2.23 -3 -2 20 1.60 1.86 -1 -2 20 27.07 3.60 0 -2 20 32.12 4.09 -1 2 -20 12.22 3.00 1 -2 20 9.16 2.79 3 1 -20 20.13 3.72 -3 -1 20 21.52 3.90 -3 -1 20 28.56 4.26 2 1 -20 42.53 4.68 -2 -1 20 54.18 5.11 -1 -1 20 25.06 3.69 0 -1 20 21.85 3.46 1 -1 20 39.63 4.68 4 0 -20 7.87 2.59 3 0 -20 27.44 3.89 -3 0 20 28.00 4.05 2 0 -20 16.43 3.46 -2 0 20 20.74 3.79 0 0 20 33.78 4.38 -2 1 20 21.49 4.01 -2 2 20 11.27 3.07 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 32997 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969311' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_12 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 Lu N3 O7' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 892.91 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Lu Lu -0.4720 5.8584 '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 8.7010(8) _cell_length_b 13.0007(12) _cell_length_c 14.7847(14) _cell_angle_alpha 100.220(2) _cell_angle_beta 97.514(2) _cell_angle_gamma 92.537(2) _cell_volume 1627.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 23906 _cell_measurement_theta_min 5.160 _cell_measurement_theta_max 50.153 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.822 _exptl_crystal_F_000 880 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_absorpt_coefficient_mu 3.336 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6614 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23481 _diffrn_reflns_av_unetI/netI 0.0927 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.414 _diffrn_reflns_theta_max 30.244 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.916 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.916 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.916 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8903 _reflns_number_gt 7001 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0292P)^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 8903 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0648 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0888 _refine_ls_wR_factor_gt 0.0797 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Lu1 Lu 0.55977(2) 0.51313(2) 0.70162(2) 0.01174(6) Uani 1 1 d . . . . . O6 O 0.8418(4) 0.5797(3) 0.5036(2) 0.0194(7) Uani 1 1 d . . . . . OW1 O 0.3742(4) 0.5581(2) 0.5934(2) 0.0140(7) Uani 1 1 d . . . . . O3 O 0.5603(4) 0.3794(2) 0.5610(2) 0.0153(7) Uani 1 1 d . . . . . O1 O 0.7070(4) 0.6217(2) 0.8396(2) 0.0164(7) Uani 1 1 d . . . . . O4 O 0.4042(4) 0.3519(2) 0.6608(2) 0.0146(7) Uani 1 1 d . . . . . C23 C 0.4592(5) 0.3224(4) 0.5863(3) 0.0127(9) Uani 1 1 d . . . . . O2 O 0.5326(4) 0.6959(2) 0.7545(2) 0.0148(7) Uani 1 1 d . . . . . C16 C 0.6373(5) 0.7018(4) 0.8223(3) 0.0136(9) Uani 1 1 d . . . . . N1 N 0.7860(4) 0.4069(3) 0.7228(2) 0.0122(8) Uani 1 1 d . . . . . O5 O 0.7230(4) 0.5968(2) 0.6309(2) 0.0159(7) Uani 1 1 d . . . . . N3 N 0.3386(4) 0.5384(3) 0.7929(3) 0.0126(8) Uani 1 1 d . . . . . N2 N 0.5669(4) 0.4156(3) 0.8347(3) 0.0125(8) Uani 1 1 d . . . . . C24 C 0.4061(5) 0.2170(4) 0.5281(3) 0.0144(9) Uani 1 1 d . . . . . C5 C 0.8074(5) 0.3511(3) 0.7917(3) 0.0125(9) Uani 1 1 d . . . . . C17 C 0.6808(5) 0.8060(4) 0.8841(3) 0.0144(10) Uani 1 1 d . . . . . C13 C 0.0869(5) 0.5679(4) 0.8923(3) 0.0179(10) Uani 1 1 d . . . . . H13 H 0.0028 0.5769 0.9250 0.022 Uiso 1 1 calc R U . . . C14 C 0.0993(5) 0.6177(4) 0.8176(3) 0.0171(10) Uani 1 1 d . . . . . H14 H 0.0235 0.6609 0.7991 0.021 Uiso 1 1 calc R U . . . C15 C 0.2272(5) 0.6018(4) 0.7711(3) 0.0161(10) Uani 1 1 d . . . . . H15 H 0.2363 0.6368 0.7222 0.019 Uiso 1 1 calc R U . . . C32 C 0.8678(5) 0.8003(4) 0.6909(3) 0.0155(10) Uani 1 1 d . . . . . H32 H 0.7748 0.7864 0.7125 0.019 Uiso 1 1 calc R U . . . C10 C 0.4467(5) 0.4168(4) 0.8844(3) 0.0139(9) Uani 1 1 d . . . . . C30 C 0.8204(5) 0.6269(4) 0.5815(3) 0.0141(9) Uani 1 1 d . . . . . C12 C 0.2035(5) 0.5041(4) 0.9167(3) 0.0173(10) Uani 1 1 d . . . . . H12 H 0.2000 0.4717 0.9678 0.021 Uiso 1 1 calc R U . . . C20 C 0.7538(6) 0.9999(4) 0.9967(3) 0.0182(10) Uani 1 1 d . . . . . C33 C 0.9553(6) 0.8929(4) 0.7286(3) 0.0174(10) Uani 1 1 d . . . . . H33 H 0.9215 0.9414 0.7746 0.021 Uiso 1 1 calc R U . . . C19 C 0.8414(5) 0.9168(4) 1.0135(3) 0.0177(10) Uani 1 1 d . . . . . H19 H 0.9234 0.9258 1.0619 0.021 Uiso 1 1 calc R U . . . C18 C 0.8031(5) 0.8197(4) 0.9559(3) 0.0172(10) Uani 1 1 d . . . . . H18 H 0.8608 0.7632 0.9658 0.021 Uiso 1 1 calc R U . . . C3 C 1.0536(5) 0.3004(4) 0.7510(3) 0.0170(10) Uani 1 1 d . . . . . H3 H 1.1444 0.2667 0.7620 0.020 Uiso 1 1 calc R U . . . C4 C 0.9398(5) 0.2975(4) 0.8074(3) 0.0166(10) Uani 1 1 d . . . . . H4 H 0.9517 0.2600 0.8556 0.020 Uiso 1 1 calc R U . . . C31 C 0.9162(5) 0.7276(4) 0.6214(3) 0.0135(9) Uani 1 1 d . . . . . C1 C 0.8959(5) 0.4056(4) 0.6662(3) 0.0154(10) Uani 1 1 d . . . . . H1 H 0.8801 0.4412 0.6169 0.018 Uiso 1 1 calc R U . . . C6 C 0.6793(5) 0.3492(4) 0.8485(3) 0.0136(9) Uani 1 1 d . . . . . C22 C 0.5953(6) 0.8911(4) 0.8690(3) 0.0192(10) Uani 1 1 d . . . . . H22 H 0.5128 0.8823 0.8208 0.023 Uiso 1 1 calc R U . . . Cl1 Cl 0.79741(15) 1.12125(9) 1.07027(8) 0.0218(3) Uani 1 1 d . . . . . Cl3 Cl 1.20934(16) 1.02717(10) 0.74430(9) 0.0290(3) Uani 1 1 d . . . . . C35 C 1.1456(6) 0.8418(4) 0.6265(4) 0.0216(11) Uani 1 1 d . . . . . H35 H 1.2384 0.8566 0.6050 0.026 Uiso 1 1 calc R U . . . C25 C 0.4724(6) 0.1792(4) 0.4501(3) 0.0186(10) Uani 1 1 d . . . . . H25 H 0.5492 0.2204 0.4324 0.022 Uiso 1 1 calc R U . . . C26 C 0.4263(6) 0.0806(4) 0.3974(3) 0.0219(11) Uani 1 1 d . . . . . H26 H 0.4719 0.0554 0.3451 0.026 Uiso 1 1 calc R U . . . C7 C 0.6713(6) 0.2808(4) 0.9106(3) 0.0191(10) Uani 1 1 d . . . . . H7 H 0.7473 0.2335 0.9172 0.023 Uiso 1 1 calc R U . . . C36 C 1.0566(5) 0.7493(4) 0.5892(3) 0.0178(10) Uani 1 1 d . . . . . H36 H 1.0901 0.7013 0.5426 0.021 Uiso 1 1 calc R U . . . C34 C 1.0937(6) 0.9120(4) 0.6966(3) 0.0185(10) Uani 1 1 d . . . . . C9 C 0.4367(6) 0.3526(4) 0.9495(3) 0.0179(10) Uani 1 1 d . . . . . H9 H 0.3547 0.3559 0.9842 0.021 Uiso 1 1 calc R U . . . C8 C 0.5507(6) 0.2836(4) 0.9618(4) 0.0231(11) Uani 1 1 d . . . . . H8 H 0.5457 0.2395 1.0046 0.028 Uiso 1 1 calc R U . . . C2 C 1.0313(5) 0.3539(4) 0.6778(3) 0.0164(10) Uani 1 1 d . . . . . H2 H 1.1048 0.3552 0.6376 0.020 Uiso 1 1 calc R U . . . C21 C 0.6320(5) 0.9888(4) 0.9249(3) 0.0174(10) Uani 1 1 d . . . . . H21 H 0.5758 1.0458 0.9143 0.021 Uiso 1 1 calc R U . . . C28 C 0.2411(6) 0.0569(4) 0.5021(4) 0.0244(12) Uani 1 1 d . . . . . H28 H 0.1631 0.0159 0.5190 0.029 Uiso 1 1 calc R U . . . C27 C 0.3115(6) 0.0206(4) 0.4243(4) 0.0235(12) Uani 1 1 d . . . . . C11 C 0.3251(5) 0.4887(4) 0.8648(3) 0.0146(10) Uani 1 1 d . . . . . C29 C 0.2896(6) 0.1554(4) 0.5539(3) 0.0204(11) Uani 1 1 d . . . . . H29 H 0.2442 0.1807 0.6063 0.024 Uiso 1 1 calc R U . . . Cl2 Cl 0.25000(18) -0.10193(10) 0.35765(10) 0.0367(4) 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 Lu1 0.01133(10) 0.01270(10) 0.01179(10) 0.00289(7) 0.00316(7) 0.00012(7) O6 0.0174(18) 0.0254(19) 0.0153(17) 0.0015(15) 0.0077(14) -0.0059(15) OW1 0.0141(16) 0.0140(16) 0.0142(16) 0.0033(13) 0.0018(13) 0.0012(13) O3 0.0162(17) 0.0167(17) 0.0136(16) 0.0036(13) 0.0044(13) -0.0025(13) O1 0.0169(17) 0.0139(17) 0.0188(17) 0.0024(14) 0.0052(14) -0.0011(13) O4 0.0183(17) 0.0147(17) 0.0116(16) 0.0027(13) 0.0049(13) 0.0004(13) C23 0.011(2) 0.014(2) 0.013(2) 0.0039(18) -0.0026(18) 0.0031(18) O2 0.0148(17) 0.0161(17) 0.0145(16) 0.0044(13) 0.0036(13) 0.0006(13) C16 0.013(2) 0.015(2) 0.013(2) 0.0013(18) 0.0067(18) -0.0026(18) N1 0.0129(19) 0.0132(19) 0.0103(18) 0.0017(15) 0.0015(15) 0.0013(15) O5 0.0167(17) 0.0138(17) 0.0186(17) 0.0041(14) 0.0072(14) -0.0029(13) N3 0.013(2) 0.0092(19) 0.0155(19) 0.0015(15) 0.0038(16) 0.0003(15) N2 0.0118(19) 0.0109(19) 0.0154(19) 0.0020(15) 0.0046(15) 0.0004(15) C24 0.015(2) 0.013(2) 0.016(2) 0.0044(19) 0.0025(19) 0.0055(18) C5 0.014(2) 0.010(2) 0.014(2) 0.0019(18) 0.0037(18) -0.0006(18) C17 0.017(2) 0.016(2) 0.011(2) 0.0025(18) 0.0034(18) -0.0020(19) C13 0.011(2) 0.018(3) 0.026(3) 0.003(2) 0.007(2) 0.0018(19) C14 0.013(2) 0.019(3) 0.021(2) 0.006(2) 0.0040(19) 0.0052(19) C15 0.019(3) 0.013(2) 0.015(2) 0.0027(19) -0.0003(19) -0.0006(19) C32 0.015(2) 0.017(2) 0.017(2) 0.0065(19) 0.0062(19) 0.0008(19) C10 0.015(2) 0.015(2) 0.012(2) 0.0007(18) 0.0044(18) 0.0015(18) C30 0.014(2) 0.013(2) 0.018(2) 0.0090(19) 0.0005(19) 0.0048(18) C12 0.016(2) 0.019(3) 0.019(2) 0.004(2) 0.006(2) 0.002(2) C20 0.025(3) 0.015(2) 0.015(2) 0.0007(19) 0.005(2) 0.002(2) C33 0.026(3) 0.013(2) 0.013(2) 0.0030(19) 0.002(2) 0.001(2) C19 0.015(2) 0.018(3) 0.019(2) 0.004(2) -0.0015(19) 0.0015(19) C18 0.019(3) 0.013(2) 0.021(2) 0.0026(19) 0.008(2) 0.0021(19) C3 0.010(2) 0.017(2) 0.023(3) 0.001(2) 0.0028(19) 0.0039(19) C4 0.017(2) 0.017(2) 0.015(2) 0.0042(19) 0.0008(19) -0.0007(19) C31 0.013(2) 0.018(2) 0.011(2) 0.0068(18) -0.0006(18) 0.0007(18) C1 0.016(2) 0.017(2) 0.015(2) 0.0034(19) 0.0054(19) -0.0005(19) C6 0.011(2) 0.015(2) 0.013(2) -0.0015(18) -0.0004(18) 0.0000(18) C22 0.018(3) 0.023(3) 0.018(2) 0.005(2) 0.002(2) 0.000(2) Cl1 0.0265(7) 0.0150(6) 0.0211(6) -0.0005(5) -0.0010(5) 0.0012(5) Cl3 0.0336(8) 0.0221(7) 0.0289(7) 0.0012(6) 0.0044(6) -0.0091(6) C35 0.014(2) 0.021(3) 0.029(3) 0.002(2) 0.005(2) 0.000(2) C25 0.016(2) 0.016(2) 0.022(3) 0.001(2) 0.002(2) 0.003(2) C26 0.021(3) 0.021(3) 0.022(3) 0.001(2) 0.001(2) 0.003(2) C7 0.019(3) 0.018(3) 0.023(3) 0.008(2) 0.004(2) 0.006(2) C36 0.016(2) 0.020(3) 0.019(2) 0.005(2) 0.006(2) 0.001(2) C34 0.022(3) 0.016(2) 0.014(2) 0.0022(19) -0.003(2) -0.005(2) C9 0.020(3) 0.020(3) 0.016(2) 0.004(2) 0.009(2) 0.001(2) C8 0.027(3) 0.024(3) 0.023(3) 0.011(2) 0.010(2) 0.003(2) C2 0.015(2) 0.015(2) 0.019(2) 0.0013(19) 0.0051(19) -0.0016(19) C21 0.019(3) 0.012(2) 0.020(2) 0.0018(19) 0.000(2) 0.0000(19) C28 0.026(3) 0.017(3) 0.028(3) 0.007(2) -0.004(2) -0.006(2) C27 0.027(3) 0.014(3) 0.025(3) 0.001(2) -0.009(2) 0.000(2) C11 0.013(2) 0.013(2) 0.013(2) -0.0086(18) 0.0001(18) 0.0004(18) C29 0.022(3) 0.020(3) 0.020(3) 0.006(2) 0.003(2) 0.000(2) Cl2 0.0463(9) 0.0169(7) 0.0383(8) -0.0047(6) -0.0112(7) -0.0004(6) _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 Lu1 O5 2.224(3) . ? Lu1 OW1 2.291(3) . ? Lu1 O4 2.382(3) . ? Lu1 O2 2.398(3) . ? Lu1 O1 2.435(3) . ? Lu1 O3 2.463(3) . ? Lu1 N1 2.472(4) . ? Lu1 N3 2.492(4) . ? Lu1 N2 2.518(4) . ? Lu1 C16 2.765(5) . ? Lu1 C23 2.782(5) . ? O6 C30 1.247(5) . ? O3 C23 1.261(5) . ? O1 C16 1.276(5) . ? O4 C23 1.262(5) . ? C23 C24 1.501(6) . ? O2 C16 1.253(5) . ? C16 C17 1.495(6) . ? N1 C1 1.349(5) . ? N1 C5 1.350(5) . ? O5 C30 1.280(5) . ? N3 C15 1.343(6) . ? N3 C11 1.353(6) . ? N2 C6 1.352(6) . ? N2 C10 1.354(5) . ? C24 C25 1.380(6) . ? C24 C29 1.397(6) . ? C5 C4 1.388(6) . ? C5 C6 1.482(6) . ? C17 C18 1.383(6) . ? C17 C22 1.395(6) . ? C13 C14 1.389(6) . ? C13 C12 1.390(6) . ? C14 C15 1.386(6) . ? C32 C33 1.382(6) . ? C32 C31 1.390(6) . ? C10 C9 1.390(6) . ? C10 C11 1.478(6) . ? C30 C31 1.503(6) . ? C12 C11 1.388(6) . ? C20 C21 1.382(6) . ? C20 C19 1.388(6) . ? C20 Cl1 1.746(5) . ? C33 C34 1.378(7) . ? C19 C18 1.392(6) . ? C3 C4 1.378(6) . ? C3 C2 1.384(6) . ? C31 C36 1.402(6) . ? C1 C2 1.389(6) . ? C6 C7 1.393(6) . ? C22 C21 1.386(6) . ? Cl3 C34 1.748(5) . ? C35 C36 1.386(7) . ? C35 C34 1.391(7) . ? C25 C26 1.389(7) . ? C26 C27 1.381(7) . ? C7 C8 1.371(7) . ? C9 C8 1.382(7) . ? C28 C29 1.388(7) . ? C28 C27 1.393(7) . ? C27 Cl2 1.739(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 O5 Lu1 OW1 83.81(11) . . ? O5 Lu1 O4 134.58(11) . . ? OW1 Lu1 O4 80.85(11) . . ? O5 Lu1 O2 74.71(11) . . ? OW1 Lu1 O2 75.17(11) . . ? O4 Lu1 O2 139.53(11) . . ? O5 Lu1 O1 82.17(11) . . ? OW1 Lu1 O1 129.53(11) . . ? O4 Lu1 O1 138.57(10) . . ? O2 Lu1 O1 54.38(11) . . ? O5 Lu1 O3 80.96(11) . . ? OW1 Lu1 O3 75.01(11) . . ? O4 Lu1 O3 53.82(10) . . ? O2 Lu1 O3 143.11(10) . . ? O1 Lu1 O3 148.14(11) . . ? O5 Lu1 N1 81.08(12) . . ? OW1 Lu1 N1 144.01(11) . . ? O4 Lu1 N1 86.89(11) . . ? O2 Lu1 N1 130.56(12) . . ? O1 Lu1 N1 80.34(11) . . ? O3 Lu1 N1 70.48(11) . . ? O5 Lu1 N3 143.00(12) . . ? OW1 Lu1 N3 79.40(11) . . ? O4 Lu1 N3 74.71(11) . . ? O2 Lu1 N3 69.22(11) . . ? O1 Lu1 N3 83.54(11) . . ? O3 Lu1 N3 125.00(11) . . ? N1 Lu1 N3 129.54(12) . . ? O5 Lu1 N2 139.22(12) . . ? OW1 Lu1 N2 136.97(11) . . ? O4 Lu1 N2 67.83(11) . . ? O2 Lu1 N2 110.44(11) . . ? O1 Lu1 N2 71.06(11) . . ? O3 Lu1 N2 106.13(11) . . ? N1 Lu1 N2 64.84(12) . . ? N3 Lu1 N2 64.70(12) . . ? O5 Lu1 C16 76.39(12) . . ? OW1 Lu1 C16 102.05(12) . . ? O4 Lu1 C16 148.70(11) . . ? O2 Lu1 C16 26.91(12) . . ? O1 Lu1 C16 27.48(12) . . ? O3 Lu1 C16 157.35(12) . . ? N1 Lu1 C16 105.78(13) . . ? N3 Lu1 C16 75.25(12) . . ? N2 Lu1 C16 91.40(13) . . ? O5 Lu1 C23 107.84(12) . . ? OW1 Lu1 C23 76.72(12) . . ? O4 Lu1 C23 26.88(11) . . ? O2 Lu1 C23 151.31(12) . . ? O1 Lu1 C23 153.45(12) . . ? O3 Lu1 C23 26.94(11) . . ? N1 Lu1 C23 77.18(12) . . ? N3 Lu1 C23 100.06(13) . . ? N2 Lu1 C23 86.60(12) . . ? C16 Lu1 C23 175.31(13) . . ? C23 O3 Lu1 90.8(3) . . ? C16 O1 Lu1 90.8(3) . . ? C23 O4 Lu1 94.5(3) . . ? O3 C23 O4 120.9(4) . . ? O3 C23 C24 119.5(4) . . ? O4 C23 C24 119.6(4) . . ? O3 C23 Lu1 62.3(2) . . ? O4 C23 Lu1 58.6(2) . . ? C24 C23 Lu1 177.2(3) . . ? C16 O2 Lu1 93.1(3) . . ? O2 C16 O1 121.7(4) . . ? O2 C16 C17 118.6(4) . . ? O1 C16 C17 119.7(4) . . ? O2 C16 Lu1 60.0(2) . . ? O1 C16 Lu1 61.7(2) . . ? C17 C16 Lu1 177.5(3) . . ? C1 N1 C5 117.6(4) . . ? C1 N1 Lu1 120.2(3) . . ? C5 N1 Lu1 122.2(3) . . ? C30 O5 Lu1 168.7(3) . . ? C15 N3 C11 117.7(4) . . ? C15 N3 Lu1 120.5(3) . . ? C11 N3 Lu1 121.8(3) . . ? C6 N2 C10 118.8(4) . . ? C6 N2 Lu1 120.1(3) . . ? C10 N2 Lu1 120.4(3) . . ? C25 C24 C29 119.4(4) . . ? C25 C24 C23 120.9(4) . . ? C29 C24 C23 119.7(4) . . ? N1 C5 C4 122.1(4) . . ? N1 C5 C6 115.8(4) . . ? C4 C5 C6 122.1(4) . . ? C18 C17 C22 119.3(4) . . ? C18 C17 C16 121.6(4) . . ? C22 C17 C16 119.1(4) . . ? C14 C13 C12 118.3(4) . . ? C15 C14 C13 118.6(4) . . ? N3 C15 C14 123.6(4) . . ? C33 C32 C31 121.3(4) . . ? N2 C10 C9 121.9(4) . . ? N2 C10 C11 116.5(4) . . ? C9 C10 C11 121.6(4) . . ? O6 C30 O5 125.5(4) . . ? O6 C30 C31 117.7(4) . . ? O5 C30 C31 116.8(4) . . ? C11 C12 C13 119.8(4) . . ? C21 C20 C19 122.1(4) . . ? C21 C20 Cl1 119.3(4) . . ? C19 C20 Cl1 118.7(4) . . ? C34 C33 C32 118.7(4) . . ? C20 C19 C18 118.2(4) . . ? C17 C18 C19 121.0(4) . . ? C4 C3 C2 119.3(4) . . ? C3 C4 C5 119.4(4) . . ? C32 C31 C36 119.0(4) . . ? C32 C31 C30 120.7(4) . . ? C36 C31 C30 120.4(4) . . ? N1 C1 C2 123.4(4) . . ? N2 C6 C7 121.3(4) . . ? N2 C6 C5 116.3(4) . . ? C7 C6 C5 122.4(4) . . ? C21 C22 C17 120.7(5) . . ? C36 C35 C34 118.8(5) . . ? C24 C25 C26 121.0(5) . . ? C27 C26 C25 118.7(5) . . ? C8 C7 C6 119.5(4) . . ? C35 C36 C31 120.4(5) . . ? C33 C34 C35 121.8(4) . . ? C33 C34 Cl3 120.0(4) . . ? C35 C34 Cl3 118.2(4) . . ? C8 C9 C10 118.8(4) . . ? C7 C8 C9 119.6(5) . . ? C3 C2 C1 118.0(4) . . ? C20 C21 C22 118.6(4) . . ? C29 C28 C27 118.6(5) . . ? C26 C27 C28 121.6(5) . . ? C26 C27 Cl2 119.2(4) . . ? C28 C27 Cl2 119.1(4) . . ? N3 C11 C12 121.9(4) . . ? N3 C11 C10 116.2(4) . . ? C12 C11 C10 121.9(4) . . ? C28 C29 C24 120.6(5) . . ? _refine_diff_density_max 1.702 _refine_diff_density_min -1.532 _refine_diff_density_rms 0.203 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.7010 13.0007 14.7847 100.220 97.514 92.537 ZERR 2.00 0.0008 0.0012 0.0014 0.002 0.002 0.002 LATT 1 SFAC C H N O CL LU UNIT 72 50 6 14 6 2 MERG 2 FMAP 2 PLAN 10 ACTA 51.00 BOND L.S. 12 WGHT 0.029200 FVAR 0.11586 LU1 6 0.559772 0.513127 0.701624 11.00000 0.01133 0.01270 = 0.01179 0.00289 0.00316 0.00012 O6 4 0.841811 0.579746 0.503558 11.00000 0.01742 0.02545 = 0.01528 0.00145 0.00770 -0.00590 OW1 4 0.374166 0.558135 0.593411 11.00000 0.01415 0.01400 = 0.01421 0.00331 0.00177 0.00123 O3 4 0.560293 0.379359 0.561048 11.00000 0.01624 0.01670 = 0.01365 0.00361 0.00444 -0.00255 O1 4 0.707032 0.621697 0.839576 11.00000 0.01689 0.01392 = 0.01875 0.00244 0.00524 -0.00113 O4 4 0.404208 0.351916 0.660783 11.00000 0.01833 0.01472 = 0.01162 0.00268 0.00492 0.00042 C23 1 0.459201 0.322363 0.586339 11.00000 0.01079 0.01401 = 0.01291 0.00390 -0.00264 0.00305 O2 4 0.532614 0.695855 0.754465 11.00000 0.01476 0.01611 = 0.01452 0.00436 0.00364 0.00063 C16 1 0.637341 0.701834 0.822337 11.00000 0.01305 0.01510 = 0.01306 0.00126 0.00671 -0.00263 N1 3 0.786000 0.406909 0.722780 11.00000 0.01292 0.01316 = 0.01026 0.00174 0.00146 0.00128 O5 4 0.722993 0.596803 0.630949 11.00000 0.01665 0.01384 = 0.01860 0.00414 0.00725 -0.00292 N3 3 0.338601 0.538421 0.792900 11.00000 0.01336 0.00922 = 0.01548 0.00145 0.00379 0.00034 N2 3 0.566931 0.415587 0.834694 11.00000 0.01177 0.01095 = 0.01535 0.00202 0.00456 0.00038 C24 1 0.406148 0.216957 0.528136 11.00000 0.01487 0.01321 = 0.01619 0.00435 0.00253 0.00555 C5 1 0.807355 0.351149 0.791660 11.00000 0.01372 0.01020 = 0.01395 0.00189 0.00373 -0.00058 C17 1 0.680779 0.805953 0.884081 11.00000 0.01670 0.01593 = 0.01071 0.00252 0.00339 -0.00200 C13 1 0.086919 0.567868 0.892253 11.00000 0.01132 0.01780 = 0.02551 0.00286 0.00703 0.00179 AFIX 43 H13 2 0.002791 0.576942 0.925042 11.00000 -1.20000 AFIX 0 C14 1 0.099327 0.617732 0.817578 11.00000 0.01313 0.01904 = 0.02060 0.00552 0.00399 0.00523 AFIX 43 H14 2 0.023486 0.660906 0.799135 11.00000 -1.20000 AFIX 0 C15 1 0.227198 0.601754 0.771132 11.00000 0.01927 0.01301 = 0.01505 0.00271 -0.00026 -0.00056 AFIX 43 H15 2 0.236336 0.636794 0.722246 11.00000 -1.20000 AFIX 0 C32 1 0.867839 0.800306 0.690895 11.00000 0.01488 0.01671 = 0.01715 0.00648 0.00616 0.00079 AFIX 43 H32 2 0.774795 0.786392 0.712467 11.00000 -1.20000 AFIX 0 C10 1 0.446684 0.416771 0.884445 11.00000 0.01490 0.01490 = 0.01198 0.00070 0.00444 0.00152 C30 1 0.820375 0.626859 0.581525 11.00000 0.01362 0.01295 = 0.01778 0.00899 0.00051 0.00479 C12 1 0.203466 0.504064 0.916711 11.00000 0.01564 0.01917 = 0.01854 0.00440 0.00593 0.00201 AFIX 43 H12 2 0.199963 0.471727 0.967765 11.00000 -1.20000 AFIX 0 C20 1 0.753830 0.999877 0.996692 11.00000 0.02474 0.01492 = 0.01476 0.00071 0.00469 0.00241 C33 1 0.955335 0.892913 0.728559 11.00000 0.02579 0.01335 = 0.01308 0.00296 0.00161 0.00125 AFIX 43 H33 2 0.921495 0.941417 0.774638 11.00000 -1.20000 AFIX 0 C19 1 0.841368 0.916799 1.013452 11.00000 0.01483 0.01823 = 0.01923 0.00406 -0.00152 0.00154 AFIX 43 H19 2 0.923392 0.925791 1.061878 11.00000 -1.20000 AFIX 0 C18 1 0.803139 0.819697 0.955871 11.00000 0.01949 0.01261 = 0.02078 0.00263 0.00797 0.00207 AFIX 43 H18 2 0.860771 0.763169 0.965824 11.00000 -1.20000 AFIX 0 C3 1 1.053570 0.300392 0.750975 11.00000 0.00976 0.01711 = 0.02321 0.00055 0.00277 0.00387 AFIX 43 H3 2 1.144385 0.266707 0.761971 11.00000 -1.20000 AFIX 0 C4 1 0.939824 0.297535 0.807380 11.00000 0.01716 0.01723 = 0.01528 0.00422 0.00078 -0.00069 AFIX 43 H4 2 0.951729 0.260002 0.855566 11.00000 -1.20000 AFIX 0 C31 1 0.916233 0.727571 0.621395 11.00000 0.01251 0.01802 = 0.01093 0.00676 -0.00063 0.00070 C1 1 0.895869 0.405624 0.666206 11.00000 0.01555 0.01691 = 0.01467 0.00336 0.00541 -0.00046 AFIX 43 H1 2 0.880108 0.441241 0.616857 11.00000 -1.20000 AFIX 0 C6 1 0.679328 0.349199 0.848451 11.00000 0.01099 0.01470 = 0.01301 -0.00150 -0.00041 0.00004 C22 1 0.595322 0.891123 0.868955 11.00000 0.01780 0.02263 = 0.01756 0.00523 0.00235 0.00023 AFIX 43 H22 2 0.512832 0.882255 0.820819 11.00000 -1.20000 AFIX 0 CL1 5 0.797412 1.121254 1.070274 11.00000 0.02649 0.01503 = 0.02113 -0.00045 -0.00100 0.00116 CL3 5 1.209335 1.027168 0.744300 11.00000 0.03357 0.02213 = 0.02890 0.00117 0.00445 -0.00907 C35 1 1.145634 0.841772 0.626484 11.00000 0.01403 0.02097 = 0.02904 0.00176 0.00458 0.00023 AFIX 43 H35 2 1.238449 0.856593 0.605026 11.00000 -1.20000 AFIX 0 C25 1 0.472430 0.179193 0.450076 11.00000 0.01600 0.01637 = 0.02242 0.00113 0.00183 0.00304 AFIX 43 H25 2 0.549173 0.220426 0.432423 11.00000 -1.20000 AFIX 0 C26 1 0.426343 0.080559 0.397440 11.00000 0.02141 0.02066 = 0.02193 0.00065 0.00076 0.00335 AFIX 43 H26 2 0.471949 0.055369 0.345123 11.00000 -1.20000 AFIX 0 C7 1 0.671333 0.280794 0.910564 11.00000 0.01853 0.01800 = 0.02284 0.00758 0.00411 0.00552 AFIX 43 H7 2 0.747309 0.233515 0.917213 11.00000 -1.20000 AFIX 0 C36 1 1.056568 0.749297 0.589246 11.00000 0.01600 0.01950 = 0.01905 0.00468 0.00561 0.00117 AFIX 43 H36 2 1.090092 0.701342 0.542635 11.00000 -1.20000 AFIX 0 C34 1 1.093669 0.912044 0.696561 11.00000 0.02245 0.01627 = 0.01435 0.00222 -0.00277 -0.00522 C9 1 0.436671 0.352581 0.949542 11.00000 0.01963 0.01990 = 0.01617 0.00426 0.00923 0.00070 AFIX 43 H9 2 0.354662 0.355945 0.984246 11.00000 -1.20000 AFIX 0 C8 1 0.550720 0.283650 0.961812 11.00000 0.02707 0.02403 = 0.02262 0.01132 0.00984 0.00266 AFIX 43 H8 2 0.545651 0.239491 1.004566 11.00000 -1.20000 AFIX 0 C2 1 1.031280 0.353894 0.677806 11.00000 0.01463 0.01541 = 0.01898 0.00134 0.00510 -0.00156 AFIX 43 H2 2 1.104814 0.355158 0.637605 11.00000 -1.20000 AFIX 0 C21 1 0.632017 0.988818 0.924886 11.00000 0.01877 0.01220 = 0.01995 0.00185 -0.00027 0.00000 AFIX 43 H21 2 0.575799 1.045758 0.914298 11.00000 -1.20000 AFIX 0 C28 1 0.241055 0.056884 0.502115 11.00000 0.02634 0.01728 = 0.02781 0.00698 -0.00397 -0.00577 AFIX 43 H28 2 0.163139 0.015936 0.519007 11.00000 -1.20000 AFIX 0 C27 1 0.311520 0.020607 0.424264 11.00000 0.02655 0.01419 = 0.02524 0.00085 -0.00885 -0.00031 C11 1 0.325075 0.488731 0.864756 11.00000 0.01310 0.01264 = 0.01346 -0.00857 0.00010 0.00044 C29 1 0.289615 0.155437 0.553924 11.00000 0.02220 0.01955 = 0.01989 0.00571 0.00281 -0.00045 AFIX 43 H29 2 0.244160 0.180737 0.606275 11.00000 -1.20000 AFIX 0 CL2 5 0.249996 -0.101928 0.357647 11.00000 0.04632 0.01690 = 0.03834 -0.00471 -0.01125 -0.00041 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0444 for 7001 Fo > 4sig(Fo) and 0.0648 for all 8903 data REM 451 parameters refined using 0 restraints END WGHT 0.0291 0.0000 REM Highest difference peak 1.702, deepest hole -1.532, 1-sigma level 0.203 Q1 1 0.3200 0.4577 0.8983 11.00000 0.05 1.70 Q2 1 0.3169 0.5034 0.5611 11.00000 0.05 0.99 Q3 1 0.1410 -0.1227 0.4846 11.00000 0.05 0.93 Q4 1 1.1320 1.0747 0.7870 11.00000 0.05 0.87 Q5 1 0.3719 0.9306 0.7561 11.00000 0.05 0.87 Q6 1 0.6577 0.4413 0.6743 11.00000 0.05 0.85 Q7 1 0.4617 0.5802 0.7411 11.00000 0.05 0.82 Q8 1 1.3379 1.0200 0.7426 11.00000 0.05 0.81 Q9 1 0.6940 0.5272 0.7056 11.00000 0.05 0.79 Q10 1 0.5211 0.4392 0.4981 11.00000 0.05 0.78 ; _shelx_res_checksum 87253 _shelx_hkl_file ; 1 0 0 330.69 9.99 1 0 0 339.20 9.79 1 0 0 322.73 9.75 1 0 0 329.79 10.02 2 0 0 4.31 1.05 2 0 0 4.90 1.02 2 0 0 3.99 0.92 2 0 0 3.11 0.86 3 0 0 120.28 5.14 3 0 0 124.19 5.34 3 0 0 120.47 5.26 3 0 0 125.63 5.55 4 0 0 5.10 1.46 4 0 0 6.24 1.47 4 0 0 2.59 1.25 4 0 0 2.99 1.33 5 0 0 44.37 4.32 5 0 0 45.39 4.12 5 0 0 46.16 4.25 5 0 0 46.21 3.52 6 0 0 77.74 5.31 6 0 0 93.54 5.49 6 0 0 83.03 5.41 6 0 0 83.44 5.73 7 0 0 43.65 4.75 7 0 0 39.20 4.56 7 0 0 34.88 4.73 -8 0 0 135.48 8.49 8 0 0 150.57 8.48 8 0 0 160.24 8.77 8 0 0 156.37 9.25 -9 0 0 83.16 7.79 9 0 0 82.66 7.53 9 0 0 85.23 8.15 -10 0 0 32.10 5.39 -10 0 0 26.54 4.75 10 0 0 24.67 4.54 -11 0 0 8.06 3.82 -11 1 0 15.67 4.25 -10 1 0 20.05 4.34 9 -1 0 58.62 6.66 9 -1 0 47.62 5.63 -9 1 0 59.68 6.55 -9 1 0 45.44 5.76 8 -1 0 154.57 9.09 8 -1 0 151.09 8.50 8 -1 0 149.91 8.92 7 -1 0 64.89 5.01 7 -1 0 74.86 6.74 7 -1 0 66.60 5.33 7 -1 0 77.74 5.55 6 -1 0 7.25 2.07 6 -1 0 7.30 2.00 6 -1 0 6.49 2.05 6 -1 0 7.34 2.00 5 -1 0 -1.04 0.97 5 -1 0 0.30 1.00 5 -1 0 0.06 0.97 5 -1 0 1.06 1.20 4 -1 0 3.75 1.36 4 -1 0 1.46 1.01 4 -1 0 1.41 1.14 4 -1 0 1.73 1.12 3 -1 0 58.20 3.35 3 -1 0 55.75 3.31 3 -1 0 60.35 3.47 3 -1 0 52.93 3.11 2 -1 0 566.36 17.03 2 -1 0 543.50 17.08 2 -1 0 552.89 17.42 2 -1 0 579.82 16.63 1 -1 0 417.66 12.44 1 -1 0 420.41 12.89 -1 1 0 429.66 12.16 0 -1 0 413.13 11.89 0 -1 0 408.22 11.98 0 1 0 406.52 11.66 0 1 0 396.48 11.72 -1 -1 0 266.27 8.32 1 1 0 270.90 8.00 1 1 0 275.55 8.46 1 1 0 269.36 8.60 -2 -1 0 139.01 5.27 2 1 0 145.91 5.57 2 1 0 150.72 5.08 2 1 0 138.40 5.68 -3 -1 0 4.88 1.17 3 1 0 3.27 1.23 3 1 0 4.19 1.09 3 1 0 5.84 1.39 -4 -1 0 24.42 2.71 4 1 0 27.39 3.09 4 1 0 32.60 2.90 4 1 0 26.85 3.17 -5 -1 0 6.07 1.60 5 1 0 2.70 1.53 5 1 0 4.60 1.50 5 1 0 3.83 1.47 -6 -1 0 74.67 5.00 6 1 0 72.13 5.11 6 1 0 68.35 4.57 6 1 0 69.50 5.28 -7 -1 0 104.96 6.76 7 1 0 140.92 7.13 7 1 0 135.21 7.54 7 1 0 106.08 7.38 -8 -1 0 63.72 6.15 8 1 0 42.99 5.58 8 1 0 57.11 5.63 8 1 0 57.85 6.00 -9 -1 0 71.06 7.08 9 1 0 72.42 7.17 -10 -1 0 39.65 6.30 10 1 0 39.47 5.78 -11 -1 0 22.75 5.24 -12 -1 0 1.39 3.40 10 -2 0 8.50 3.08 -10 2 0 8.53 3.35 -10 2 0 11.64 3.56 9 -2 0 54.65 6.38 9 -2 0 69.34 7.20 -9 2 0 46.27 5.99 8 -2 0 76.37 7.18 8 -2 0 76.12 5.66 8 -2 0 69.52 6.81 -8 2 0 78.30 7.18 7 -2 0 37.62 4.70 7 -2 0 40.11 4.74 7 -2 0 38.11 4.30 6 -2 0 24.23 3.51 6 -2 0 27.76 3.33 6 -2 0 24.19 3.63 6 -2 0 32.02 4.05 5 -2 0 16.74 2.35 5 -2 0 15.35 2.55 5 -2 0 11.91 2.43 5 -2 0 15.58 2.63 4 -2 0 17.47 2.67 4 -2 0 20.58 2.34 4 -2 0 24.58 3.02 4 -2 0 23.65 2.68 3 -2 0 13.46 2.07 3 -2 0 13.93 1.82 3 -2 0 10.70 1.93 -3 2 0 13.20 1.61 2 -2 0 2.61 0.83 2 -2 0 2.82 1.05 -2 2 0 3.44 0.80 1 -2 0 198.60 6.19 1 -2 0 186.49 6.75 -1 2 0 189.70 6.05 -1 2 0 183.58 6.60 0 -2 0 379.37 11.76 0 -2 0 380.23 11.66 0 2 0 369.43 11.47 0 2 0 388.58 11.45 -1 -2 0 173.19 6.20 1 2 0 189.94 5.94 1 2 0 196.78 6.62 -2 -2 0 3.15 0.91 2 2 0 2.99 1.04 2 2 0 1.86 0.70 -3 -2 0 85.69 3.99 3 2 0 77.98 4.50 3 2 0 80.27 3.64 3 2 0 78.97 4.41 -4 -2 0 3.70 1.16 4 2 0 0.17 0.98 4 2 0 0.46 1.23 4 2 0 2.04 0.96 -5 -2 0 99.15 5.24 5 2 0 84.38 5.39 5 2 0 88.49 5.78 5 2 0 78.41 4.53 -6 -2 0 66.15 4.78 6 2 0 80.43 5.53 6 2 0 74.73 5.61 6 2 0 75.68 4.66 -7 -2 0 58.65 5.42 7 2 0 52.59 4.95 7 2 0 48.11 5.42 -8 -2 0 27.22 4.17 -8 -2 0 27.51 4.57 8 2 0 32.00 4.65 -9 -2 0 91.78 9.02 9 2 0 104.81 7.73 -10 -2 0 24.94 5.24 10 2 0 15.69 3.95 -11 -2 0 8.31 3.87 11 2 0 5.84 3.37 -11 3 0 16.43 4.42 10 -3 0 25.66 4.98 -10 3 0 19.31 4.34 9 -3 0 52.04 6.12 9 -3 0 46.37 6.06 -9 3 0 37.56 5.50 8 -3 0 109.45 7.52 8 -3 0 107.78 7.19 -8 3 0 117.52 7.76 -8 3 0 98.15 6.61 7 -3 0 15.52 3.11 7 -3 0 14.23 3.10 -7 3 0 15.22 3.21 -7 3 0 19.42 2.98 6 -3 0 1.05 1.41 6 -3 0 1.39 1.44 -6 3 0 1.49 1.18 -6 3 0 1.25 1.31 5 -3 0 -0.23 1.17 5 -3 0 1.68 1.18 -5 3 0 1.34 0.99 4 -3 0 0.88 1.09 4 -3 0 -0.70 0.85 -4 3 0 1.13 0.82 3 -3 0 75.60 3.64 3 -3 0 73.13 4.30 -3 3 0 67.90 4.12 -3 3 0 60.70 3.21 2 -3 0 101.07 4.96 2 -3 0 100.19 4.14 -2 3 0 101.21 4.89 -2 3 0 108.06 4.12 1 -3 0 65.36 3.57 1 -3 0 71.24 3.11 -1 3 0 72.26 3.08 -1 3 0 69.87 3.61 0 -3 0 40.25 2.39 0 -3 0 35.90 2.44 0 3 0 32.37 2.26 0 3 0 32.93 2.25 -1 -3 0 173.65 6.33 -1 -3 0 177.54 6.79 1 3 0 175.52 6.03 1 3 0 176.79 6.68 -2 -3 0 3.08 1.27 -2 -3 0 3.48 1.01 2 3 0 3.23 0.90 2 3 0 5.04 1.31 -3 -3 0 20.02 2.13 -3 -3 0 16.77 2.48 3 3 0 17.65 2.47 3 3 0 16.88 1.81 -4 -3 0 7.56 1.59 -4 -3 0 8.62 2.10 4 3 0 5.46 1.71 4 3 0 6.81 1.40 -5 -3 0 20.91 2.71 -5 -3 0 20.84 3.35 5 3 0 24.01 2.67 5 3 0 15.95 2.89 -6 -3 0 51.69 5.64 -6 -3 0 45.37 4.44 6 3 0 52.24 3.71 6 3 0 55.91 5.49 -7 -3 0 140.98 8.90 -7 -3 0 138.11 7.66 7 3 0 140.97 7.10 7 3 0 144.97 8.48 -8 -3 0 5.97 2.96 -8 -3 0 4.74 2.15 8 3 0 9.88 2.96 -9 -3 0 31.35 5.36 9 3 0 34.41 5.21 -10 -3 0 12.07 4.31 10 3 0 17.85 4.39 -11 -3 0 1.51 2.97 11 3 0 1.17 2.67 11 -4 0 13.87 4.32 10 -4 0 46.71 6.55 -10 4 0 59.29 7.43 9 -4 0 56.41 6.84 -9 4 0 66.87 7.48 8 -4 0 67.60 6.43 8 -4 0 66.32 6.97 -8 4 0 60.36 6.85 -8 4 0 64.87 5.89 7 -4 0 3.59 1.90 7 -4 0 6.15 2.13 -7 4 0 7.01 2.59 -7 4 0 3.16 1.61 6 -4 0 3.56 1.68 6 -4 0 1.13 1.38 -6 4 0 5.18 2.14 -6 4 0 2.67 1.27 5 -4 0 3.37 1.36 5 -4 0 1.92 1.49 -5 4 0 2.06 1.04 -5 4 0 0.76 1.19 4 -4 0 -0.30 1.15 4 -4 0 0.16 0.86 -4 4 0 -1.39 0.83 -4 4 0 -0.30 0.69 3 -4 0 3.69 1.14 3 -4 0 1.89 1.23 -3 4 0 3.34 0.99 -3 4 0 7.39 1.81 2 -4 0 170.35 6.26 2 -4 0 161.79 7.19 -2 4 0 168.24 6.17 -2 4 0 167.90 7.19 1 -4 0 148.13 6.41 1 -4 0 140.14 5.60 -1 4 0 151.85 5.65 -1 4 0 148.80 6.24 0 -4 0 4.78 1.34 0 -4 0 5.75 1.44 0 4 0 4.34 1.27 -1 -4 0 151.42 6.11 -1 -4 0 161.69 6.59 1 4 0 154.46 5.74 1 4 0 141.96 6.31 -2 -4 0 94.08 4.28 -2 -4 0 92.19 5.04 2 4 0 84.45 3.84 2 4 0 90.19 4.95 -3 -4 0 4.68 1.28 -3 -4 0 5.76 1.72 3 4 0 7.20 1.82 3 4 0 6.45 1.25 -4 -4 0 8.89 1.70 -4 -4 0 8.77 2.19 4 4 0 9.14 2.19 4 4 0 9.31 1.59 -5 -4 0 15.00 3.07 -5 -4 0 11.33 2.07 5 4 0 13.83 2.05 5 4 0 18.28 3.07 -6 -4 0 69.18 4.78 -6 -4 0 65.93 6.70 6 4 0 64.00 6.18 6 4 0 79.69 4.52 -7 -4 0 43.13 5.72 -7 -4 0 36.90 4.26 7 4 0 38.77 5.12 -8 -4 0 28.34 5.07 8 4 0 22.05 4.19 -9 -4 0 35.37 6.15 9 4 0 36.27 5.66 -10 -4 0 15.97 4.63 10 4 0 24.57 5.02 -11 -4 0 3.49 3.50 11 4 0 -1.14 2.41 11 -5 0 21.55 5.14 -11 5 0 19.74 5.05 10 -5 0 72.69 8.20 -10 5 0 72.40 8.53 9 -5 0 42.33 6.05 -9 5 0 50.12 6.67 8 -5 0 40.59 5.52 -8 5 0 40.43 5.80 7 -5 0 11.53 2.68 7 -5 0 6.97 2.56 -7 5 0 10.21 2.24 -7 5 0 9.86 2.95 6 -5 0 12.78 2.97 6 -5 0 9.67 2.18 -6 5 0 9.87 1.93 -6 5 0 11.45 2.77 5 -5 0 0.33 0.99 5 -5 0 -1.22 1.09 -5 5 0 0.39 1.14 -5 5 0 0.70 0.93 4 -5 0 101.21 5.02 4 -5 0 99.59 6.24 -4 5 0 101.99 6.22 -4 5 0 107.46 4.91 3 -5 0 6.35 1.36 3 -5 0 6.68 1.97 -3 5 0 5.54 1.22 -3 5 0 6.86 2.04 2 -5 0 102.69 4.67 2 -5 0 102.28 5.63 -2 5 0 110.72 5.71 -2 5 0 103.17 4.64 1 -5 0 190.82 7.34 1 -5 0 186.43 8.06 -1 5 0 193.25 7.90 -1 5 0 191.10 7.26 0 -5 0 101.62 5.11 0 -5 0 106.82 5.24 0 5 0 102.45 4.97 0 5 0 101.81 5.01 -1 -5 0 29.89 3.26 -1 -5 0 32.89 3.00 1 5 0 34.73 2.51 1 5 0 30.24 3.09 -2 -5 0 206.88 7.89 -2 -5 0 185.77 8.47 2 5 0 201.99 8.53 2 5 0 195.60 7.25 -3 -5 0 8.62 2.16 -3 -5 0 11.14 1.86 3 5 0 12.82 1.75 3 5 0 14.32 2.47 -4 -5 0 41.61 4.75 -4 -5 0 41.33 3.22 4 5 0 38.39 2.73 4 5 0 38.15 4.36 -5 -5 0 28.08 4.32 -5 -5 0 26.62 3.15 5 5 0 21.97 3.57 5 5 0 35.89 3.22 -6 -5 0 51.71 4.75 -6 -5 0 59.61 6.57 6 5 0 45.81 5.49 -7 -5 0 42.41 5.90 -7 -5 0 31.43 3.99 7 5 0 40.65 5.35 -8 -5 0 76.35 8.44 8 5 0 83.50 8.25 -9 -5 0 11.44 4.24 9 5 0 10.20 3.34 -10 -5 0 18.45 5.20 10 5 0 14.49 4.12 -11 -5 0 -1.53 2.98 11 5 0 1.46 3.24 11 -6 0 14.91 4.43 -11 6 0 15.81 4.84 10 -6 0 16.90 4.25 -10 6 0 25.33 5.46 9 -6 0 27.85 4.95 -9 6 0 15.56 4.12 8 -6 0 53.23 6.66 -8 6 0 61.46 7.38 7 -6 0 10.66 3.05 7 -6 0 17.98 3.17 -7 6 0 15.47 3.61 6 -6 0 19.64 3.03 6 -6 0 18.97 3.71 -6 6 0 22.14 2.83 -6 6 0 26.88 4.42 5 -6 0 5.96 1.71 5 -6 0 4.33 1.94 -5 6 0 2.64 1.23 -5 6 0 4.54 2.07 4 -6 0 24.07 3.65 4 -6 0 27.43 2.90 -4 6 0 23.13 2.54 -4 6 0 28.69 3.87 3 -6 0 152.36 6.34 3 -6 0 160.34 7.99 -3 6 0 143.84 7.56 -3 6 0 145.21 6.30 2 -6 0 110.75 6.12 2 -6 0 114.28 5.04 -2 6 0 90.05 5.67 -2 6 0 101.57 4.91 1 -6 0 33.04 3.11 1 -6 0 26.99 3.27 -1 6 0 33.17 3.15 -1 6 0 31.80 3.48 0 -6 0 76.00 4.65 0 -6 0 80.24 4.63 0 6 0 74.18 4.43 0 6 0 66.54 4.24 -1 -6 0 391.90 14.80 -1 -6 0 417.89 14.56 1 6 0 414.29 14.65 1 6 0 420.89 13.96 -2 -6 0 6.34 1.80 -2 -6 0 6.32 1.62 2 6 0 7.63 1.96 2 6 0 9.12 1.65 -3 -6 0 40.25 3.64 -3 -6 0 37.44 4.31 3 6 0 34.06 2.66 3 6 0 39.53 4.31 -4 -6 0 4.33 1.99 -4 -6 0 4.93 1.58 4 6 0 4.04 1.33 4 6 0 5.20 1.96 -5 -6 0 58.73 4.43 -5 -6 0 70.09 7.12 5 6 0 66.17 3.98 5 6 0 57.99 6.19 -6 -6 0 40.91 4.30 -6 -6 0 43.93 5.78 6 6 0 41.92 5.40 -7 -6 0 39.22 6.04 7 6 0 66.07 7.14 -8 -6 0 52.65 7.40 8 6 0 56.96 6.97 -9 -6 0 45.12 7.25 9 6 0 52.85 7.24 -10 -6 0 3.60 3.64 10 6 0 5.96 3.56 11 -7 0 3.71 3.50 -11 7 0 2.33 3.09 10 -7 0 36.82 6.31 -10 7 0 38.68 6.55 9 -7 0 33.76 5.82 -9 7 0 50.01 7.25 8 -7 0 2.63 2.28 -8 7 0 2.74 2.56 7 -7 0 24.35 4.46 -7 7 0 43.22 6.07 6 -7 0 6.78 2.10 6 -7 0 1.34 1.89 -6 7 0 7.33 1.84 -6 7 0 3.16 2.31 5 -7 0 36.39 3.71 5 -7 0 40.94 5.33 -5 7 0 39.48 3.63 -5 7 0 37.13 5.05 4 -7 0 87.64 6.52 4 -7 0 105.25 5.37 -4 7 0 104.77 6.78 -4 7 0 107.32 5.31 3 -7 0 36.48 3.39 3 -7 0 39.56 4.60 -3 7 0 38.42 4.50 -3 7 0 47.21 3.28 2 -7 0 85.27 5.74 2 -7 0 85.41 4.64 -2 7 0 86.75 5.59 -2 7 0 88.73 4.74 1 -7 0 361.39 14.09 1 -7 0 352.25 13.18 -1 7 0 376.13 13.09 -1 7 0 369.17 13.80 0 -7 0 57.89 4.15 0 -7 0 50.38 4.03 0 7 0 53.28 3.86 0 7 0 43.76 4.10 -1 -7 0 -1.26 0.99 -1 -7 0 0.59 1.08 1 7 0 2.20 1.35 1 7 0 0.86 1.03 -2 -7 0 21.77 3.36 -2 -7 0 23.73 3.05 2 7 0 22.55 2.71 2 7 0 23.26 3.25 -3 -7 0 -0.87 1.19 -3 -7 0 -0.23 1.06 3 7 0 -0.24 0.84 3 7 0 0.93 1.39 -4 -7 0 73.62 4.80 -4 -7 0 70.43 6.75 4 7 0 77.96 4.27 4 7 0 82.00 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-1 -7 18 28.37 5.78 0 7 -18 20.63 4.83 -1 7 -18 6.15 3.74 1 -7 18 15.56 4.35 -2 7 -18 2.20 3.06 2 -7 18 -1.09 2.52 -3 7 -18 0.27 2.87 3 -7 18 2.08 3.18 6 6 -18 1.54 3.75 -6 -6 18 6.93 4.30 5 6 -18 2.16 3.00 -5 -6 18 -1.66 2.65 -4 -6 18 5.47 3.32 3 6 -18 44.01 6.55 -3 -6 18 32.97 6.28 2 6 -18 10.74 3.92 -2 -6 18 19.11 4.90 1 6 -18 66.55 7.99 0 6 -18 48.08 6.79 0 -6 18 47.63 6.63 -1 6 -18 5.02 3.06 1 -6 18 9.28 3.45 -2 6 -18 16.30 4.60 2 -6 18 13.41 4.22 -3 6 -18 1.01 3.08 3 -6 18 2.03 2.96 6 5 -18 -0.28 3.04 -6 -5 18 0.54 2.69 5 5 -18 -1.51 2.88 -5 -5 18 0.89 2.97 4 5 -18 12.77 4.25 -4 -5 18 12.56 4.13 -3 -5 18 36.36 6.17 2 5 -18 38.76 6.06 -2 -5 18 34.90 6.07 1 5 -18 45.63 6.79 0 5 -18 63.20 7.73 0 -5 18 64.05 7.62 -1 5 -18 29.44 5.69 1 -5 18 28.55 5.45 -2 5 -18 8.07 3.80 2 -5 18 3.12 2.95 -3 5 -18 -0.09 2.70 3 -5 18 2.49 2.60 6 4 -18 6.37 3.88 -6 -4 18 0.69 3.08 5 4 -18 1.75 3.07 -5 -4 18 1.39 2.76 4 4 -18 29.27 5.59 -4 -4 18 23.66 5.47 3 4 -18 5.51 3.22 -3 -4 18 1.42 2.71 1 4 -18 57.72 7.29 -1 -4 18 70.90 7.83 0 4 -18 34.02 5.83 0 -4 18 42.08 6.42 -1 4 -18 5.80 3.27 1 -4 18 13.31 4.04 -2 4 -18 4.67 3.54 2 -4 18 2.68 2.74 -3 4 -18 2.37 3.20 3 -4 18 2.65 2.94 6 3 -18 -0.63 2.83 -6 -3 18 -1.69 2.64 5 3 -18 -2.68 2.42 -5 -3 18 3.87 3.24 4 3 -18 7.37 3.67 -4 -3 18 5.16 3.18 3 3 -18 37.43 6.24 -3 -3 18 53.51 7.16 2 3 -18 38.63 5.95 1 3 -18 30.55 5.42 -1 -3 18 41.24 6.00 0 3 -18 27.97 5.21 0 -3 18 31.37 5.55 -1 3 -18 13.81 4.28 1 -3 18 17.45 4.44 -2 3 -18 -2.40 2.42 2 -3 18 -0.58 1.95 -3 3 -18 -1.28 2.74 3 -3 18 1.04 2.59 6 2 -18 2.06 3.21 -6 -2 18 1.32 3.14 5 2 -18 -0.16 2.62 -5 -2 18 2.07 3.19 4 2 -18 3.45 3.30 -4 -2 18 19.06 4.67 3 2 -18 34.82 6.14 2 2 -18 37.91 6.00 -2 -2 18 31.58 5.46 -1 -2 18 12.90 3.78 0 2 -18 13.50 4.05 0 -2 18 20.97 4.87 -1 2 -18 13.65 4.12 1 -2 18 9.61 3.61 -2 2 -18 1.60 2.83 2 -2 18 0.26 2.51 -3 2 -18 6.40 3.56 3 -2 18 4.42 3.35 -7 -1 18 3.67 3.53 6 1 -18 -1.47 2.73 -6 -1 18 4.24 3.57 5 1 -18 3.70 3.31 -5 -1 18 6.13 3.80 4 1 -18 17.08 4.75 3 1 -18 28.37 5.55 -3 -1 18 23.73 4.69 2 1 -18 28.58 5.60 -2 -1 18 29.58 5.19 1 1 -18 48.25 6.61 -1 -1 18 32.93 5.70 0 -1 18 16.50 4.23 -1 1 -18 15.54 4.25 1 -1 18 16.65 4.49 -2 1 -18 3.26 3.23 2 -1 18 0.11 2.44 -3 1 -18 2.28 3.17 3 -1 18 7.40 3.53 -7 0 18 -0.31 3.05 6 0 -18 2.88 3.79 -6 0 18 4.86 3.52 5 0 -18 6.13 3.67 -5 0 18 8.64 3.88 4 0 -18 4.29 3.24 3 0 -18 33.02 6.10 -3 0 18 35.90 5.75 2 0 -18 47.03 6.89 -2 0 18 39.39 5.97 1 0 -18 10.08 3.63 -1 0 18 6.45 3.16 0 0 -18 16.23 4.38 0 0 18 15.30 4.21 1 0 18 10.03 3.92 -2 0 -18 0.84 2.90 2 0 18 -0.64 2.38 -3 0 -18 6.81 4.14 3 0 18 4.69 3.36 -6 1 18 0.91 3.19 5 -1 -18 10.69 4.56 4 -1 -18 28.38 5.73 -4 1 18 37.55 6.14 3 -1 -18 21.53 5.08 -3 1 18 7.02 3.15 2 -1 -18 31.27 6.01 -2 1 18 28.04 5.44 1 -1 -18 4.96 3.08 -1 1 18 4.48 2.82 0 -1 -18 0.19 2.68 0 1 18 1.11 2.31 -1 -1 -18 2.61 3.18 1 1 18 -0.86 2.30 -2 -1 -18 1.17 2.96 2 1 18 -0.65 2.33 -3 -1 -18 7.20 3.90 5 -2 -18 15.49 4.98 4 -2 -18 36.42 6.85 -4 2 18 23.88 5.17 3 -2 -18 17.69 4.87 -3 2 18 19.54 4.66 2 -2 -18 7.01 3.46 -2 2 18 3.32 2.88 1 -2 -18 39.86 6.63 -1 2 18 46.81 6.87 0 -2 -18 10.05 4.12 0 2 18 5.32 2.91 -1 -2 -18 -1.23 2.66 1 2 18 -0.30 2.54 -2 -2 -18 3.72 3.40 2 2 18 3.09 2.98 -3 -2 -18 7.96 3.93 -5 3 18 15.96 4.58 4 -3 -18 12.21 4.83 -4 3 18 14.85 4.46 3 -3 -18 17.77 5.19 -3 3 18 26.74 5.35 2 -3 -18 24.73 5.33 -2 3 18 24.27 5.29 1 -3 -18 17.50 4.91 -1 3 18 28.22 5.60 0 -3 -18 7.77 3.86 0 3 18 -1.62 2.15 -1 -3 -18 3.70 3.38 1 3 18 -0.09 2.60 -2 -3 -18 4.44 3.84 -5 4 18 8.50 4.06 -4 4 18 32.22 6.36 3 -4 -18 26.63 5.92 -3 4 18 22.62 5.37 2 -4 -18 21.02 5.25 -2 4 18 14.87 4.53 1 -4 -18 41.65 7.14 -1 4 18 45.15 7.26 0 -4 -18 24.13 5.55 0 4 18 23.74 5.63 -1 -4 -18 1.64 3.55 -2 -4 -18 -0.42 3.46 -3 5 18 36.36 6.57 -2 5 18 31.93 6.21 1 -5 -18 10.38 4.22 -1 -10 19 11.87 4.96 3 9 -19 16.81 5.00 -3 -9 19 9.90 4.55 2 9 -19 26.68 5.96 -2 -9 19 35.96 7.09 1 9 -19 -0.65 3.11 -1 -9 19 6.99 4.02 3 8 -19 6.37 3.80 -3 -8 19 1.29 3.57 2 8 -19 14.90 4.85 -2 -8 19 23.03 5.78 1 8 -19 8.98 4.07 0 8 -19 -0.16 3.19 2 -8 19 0.74 3.18 -4 -7 19 15.35 4.99 -3 -7 19 32.54 6.49 2 7 -19 11.58 4.24 -2 -7 19 8.69 4.09 1 7 -19 14.88 4.57 0 7 -19 1.14 3.21 -1 7 -19 11.81 4.32 2 -7 19 5.71 3.75 -5 -6 19 14.76 4.91 -4 -6 19 32.43 6.40 -3 -6 19 56.86 8.02 2 6 -19 3.50 3.31 1 6 -19 6.54 3.59 0 6 -19 1.80 3.09 -1 6 -19 3.66 3.53 1 -6 19 3.22 3.06 -2 6 -19 16.65 4.69 2 -6 19 16.58 4.67 6 5 -19 31.98 6.34 -5 -5 19 38.78 7.06 -4 -5 19 40.04 6.89 -3 -5 19 14.14 4.66 1 5 -19 0.65 3.13 0 5 -19 -2.03 2.60 0 -5 19 0.96 2.77 -1 5 -19 8.48 4.12 1 -5 19 12.64 4.09 -2 5 -19 9.79 4.03 2 -5 19 5.72 3.60 6 4 -19 30.49 6.73 5 4 -19 37.39 6.91 -5 -4 19 19.48 5.58 4 4 -19 32.06 6.04 -4 -4 19 25.50 5.52 0 4 -19 5.74 3.35 0 -4 19 -0.21 2.45 -1 4 -19 0.11 2.80 1 -4 19 -0.63 2.41 -2 4 -19 10.83 4.38 2 -4 19 8.15 3.66 -6 -3 19 7.81 4.03 5 3 -19 35.46 6.63 -5 -3 19 32.88 6.33 4 3 -19 20.28 5.13 3 3 -19 16.24 4.62 -1 -3 19 5.90 3.21 0 3 -19 7.17 3.42 0 -3 19 5.47 3.35 -1 3 -19 13.78 4.30 1 -3 19 10.26 3.92 -2 3 -19 0.40 3.17 2 -3 19 1.06 2.84 -6 -2 19 10.03 4.45 5 2 -19 11.86 4.42 -5 -2 19 4.34 3.53 4 2 -19 44.24 7.06 3 2 -19 26.84 5.74 2 2 -19 2.78 3.01 -2 -2 19 -1.76 2.35 -1 -2 19 1.78 2.63 0 -2 19 0.68 2.35 -1 2 -19 1.01 3.25 1 -2 19 2.52 2.71 -2 2 -19 16.44 4.89 2 -2 19 22.73 5.39 -6 -1 19 23.47 5.84 5 1 -19 31.61 6.50 4 1 -19 16.13 4.81 3 1 -19 22.82 5.42 2 1 -19 11.18 4.28 -2 -1 19 10.96 3.88 -1 -1 19 -2.00 2.11 0 -1 19 6.34 3.40 1 -1 19 -0.34 2.27 -2 1 -19 23.84 5.61 2 -1 19 21.14 5.34 -3 1 -19 26.99 5.74 5 0 -19 41.15 6.97 4 0 -19 35.28 6.69 3 0 -19 1.06 3.13 -3 0 19 0.60 2.63 2 0 -19 -3.01 2.72 -2 0 19 -0.77 2.31 1 0 -19 1.84 3.05 -1 0 19 2.33 2.78 0 0 19 5.14 3.04 1 0 19 22.47 5.29 4 -1 -19 18.73 5.25 3 -1 -19 4.08 3.58 -3 1 19 3.31 3.10 2 -1 -19 0.42 2.98 -2 1 19 -0.15 2.44 1 -1 -19 -2.72 2.74 -1 1 19 2.53 2.89 0 -1 -19 5.10 3.55 0 1 19 5.12 3.17 1 1 19 6.58 3.26 -4 2 19 4.00 3.47 3 -2 -19 5.85 3.45 -3 2 19 2.93 3.33 2 -2 -19 0.83 3.11 -2 2 19 -0.37 2.64 1 -2 -19 10.35 4.14 -1 2 19 3.60 3.15 0 -2 -19 14.08 4.68 0 2 19 14.24 4.33 -1 -2 -19 12.36 4.37 -4 3 19 16.12 4.84 -3 3 19 3.10 3.02 2 -3 -19 2.99 3.30 -2 3 19 1.57 2.84 1 -3 -19 6.40 3.93 0 -3 -19 32.74 6.45 -1 -3 -19 30.56 6.37 2 8 -20 1.54 3.81 -3 -7 20 2.66 3.66 1 7 -20 2.27 3.43 -4 -6 20 -5.06 2.88 1 6 -20 13.45 4.85 0 6 -20 31.09 6.30 1 -6 20 42.79 7.21 -4 -5 20 1.23 3.38 0 5 -20 26.99 5.90 -1 5 -20 27.59 5.87 1 -5 20 24.02 5.59 5 4 -20 2.65 3.70 0 -4 20 22.65 5.21 -1 4 -20 11.16 4.52 1 -4 20 8.73 4.06 4 3 -20 2.16 3.53 0 -3 20 20.07 5.05 -1 3 -20 33.02 6.26 1 -3 20 20.25 5.15 4 2 -20 0.89 3.23 3 2 -20 1.98 3.50 -1 -2 20 24.04 5.33 0 -2 20 24.57 5.51 4 1 -20 3.17 3.41 3 1 -20 18.39 5.33 -2 -1 20 47.40 7.22 -1 -1 20 16.13 4.88 0 -1 20 11.12 4.19 3 0 -20 22.93 5.69 2 0 -20 15.14 5.01 -2 0 20 15.65 4.66 -1 0 20 33.50 6.32 -3 1 20 -1.56 2.73 2 -1 -20 19.23 5.22 -2 1 20 18.51 4.95 1 -1 -20 16.97 5.05 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 63925 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? _database_code_depnum_ccdc_archive 'CCDC 969312' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_Compound_13 _audit_creation_method SHELXL-2013 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H25 Cl3 N3 O7 Y' _exptl_crystal_recrystallization_method Hydrothermal _chemical_melting_point ? _exptl_crystal_description Plate _exptl_crystal_colour Colorless _diffrn_ambient_temperature 100(2) _chemical_formula_weight 806.85 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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 8.706(3) _cell_length_b 13.108(5) _cell_length_c 14.788(5) _cell_angle_alpha 100.278(6) _cell_angle_beta 97.723(6) _cell_angle_gamma 92.392(6) _cell_volume 1641.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22884 _cell_measurement_theta_min 4.732 _cell_measurement_theta_max 41.281 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_F_000 816 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 2.077 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6539 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS, Bruker-AXS (2008)' _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX II CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22884 _diffrn_reflns_av_unetI/netI 0.1234 _diffrn_reflns_av_R_equivalents 0.0933 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.414 _diffrn_reflns_theta_max 28.391 _diffrn_reflns_theta_full 25.500 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 8206 _reflns_number_gt 5095 _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 'APEX, Bruker-AXS' _computing_cell_refinement 'SAINT, Bruker-AXS' _computing_data_reduction 'SAINT, Bruker-AXS' _computing_structure_solution 'SIR92 (Gualardi, 1994)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Crystal Maker (Palmer, 2009)' _computing_publication_material 'WINGX (Farrugia, 2012)' _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^)+(0.0447P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 8206 _refine_ls_number_parameters 459 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1031 _refine_ls_goodness_of_fit_ref 0.977 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.06240(5) 0.51347(3) 0.70111(3) 0.01310(11) Uani 1 1 d . . . . . Cl1 Cl 0.29694(13) 1.12042(8) 1.07058(7) 0.0247(3) Uani 1 1 d . . . . . Cl3 Cl 0.70952(14) 1.02602(9) 0.74346(8) 0.0314(3) Uani 1 1 d . . . . . Cl2 Cl -0.25082(15) -0.10018(9) 0.35682(9) 0.0382(3) Uani 1 1 d . . . . . O3 O 0.0621(3) 0.3773(2) 0.56148(18) 0.0159(6) Uani 1 1 d . . . . . O2 O 0.0351(3) 0.6968(2) 0.75495(18) 0.0169(6) Uani 1 1 d . . . . . O5 O 0.2290(3) 0.5957(2) 0.62856(18) 0.0172(6) Uani 1 1 d . . . . . O4 O -0.0949(3) 0.3502(2) 0.66081(18) 0.0166(6) Uani 1 1 d . . . . . OW1 O -0.1300(3) 0.5586(2) 0.59270(19) 0.0158(6) Uani 1 1 d D . . . . O1 O 0.2098(3) 0.6237(2) 0.84172(18) 0.0161(6) Uani 1 1 d . . . . . O6 O 0.3466(3) 0.5804(2) 0.50169(19) 0.0204(7) Uani 1 1 d . . . . . N2 N 0.0694(4) 0.4150(2) 0.8369(2) 0.0135(7) Uani 1 1 d . . . . . N1 N 0.2906(4) 0.4051(2) 0.7250(2) 0.0149(7) Uani 1 1 d . . . . . N3 N -0.1604(4) 0.5384(2) 0.7960(2) 0.0143(7) Uani 1 1 d . . . . . C6 C 0.1790(5) 0.3473(3) 0.8499(3) 0.0155(9) Uani 1 1 d . . . . . C5 C 0.3093(5) 0.3492(3) 0.7939(3) 0.0149(9) Uani 1 1 d . . . . . C30 C 0.3252(4) 0.6265(3) 0.5793(3) 0.0150(9) Uani 1 1 d . . . . . C3 C 0.5565(5) 0.2973(3) 0.7544(3) 0.0194(9) Uani 1 1 d . . . . . H3 H 0.6462 0.2626 0.7654 0.023 Uiso 1 1 calc R U . . . C1 C 0.4024(5) 0.4046(3) 0.6705(3) 0.0180(9) Uani 1 1 d . . . . . H1 H 0.3890 0.4416 0.6222 0.022 Uiso 1 1 calc R U . . . C4 C 0.4411(5) 0.2950(3) 0.8101(3) 0.0182(9) Uani 1 1 d . . . . . H4 H 0.4516 0.2574 0.8580 0.022 Uiso 1 1 calc R U . . . C15 C -0.2725(5) 0.6015(3) 0.7743(3) 0.0188(9) Uani 1 1 d . . . . . H15 H -0.2642 0.6363 0.7254 0.023 Uiso 1 1 calc R U . . . C10 C -0.0513(4) 0.4159(3) 0.8857(3) 0.0152(9) Uani 1 1 d . . . . . C11 C -0.1728(4) 0.4890(3) 0.8676(3) 0.0141(8) Uani 1 1 d . . . . . C32 C 0.3718(5) 0.7985(3) 0.6902(3) 0.0170(9) Uani 1 1 d . . . . . H32 H 0.2795 0.7841 0.7121 0.020 Uiso 1 1 calc R U . . . C13 C -0.4094(5) 0.5677(3) 0.8952(3) 0.0212(10) Uani 1 1 d . . . . . H13 H -0.4929 0.5771 0.9284 0.025 Uiso 1 1 calc R U . . . C20 C 0.2536(5) 0.9994(3) 0.9978(3) 0.0202(9) Uani 1 1 d . . . . . C24 C -0.0941(5) 0.2162(3) 0.5285(3) 0.0150(8) Uani 1 1 d . . . . . C12 C -0.2935(5) 0.5036(3) 0.9200(3) 0.0172(9) Uani 1 1 d . . . . . H12 H -0.2970 0.4711 0.9708 0.021 Uiso 1 1 calc R U . . . C31 C 0.4202(5) 0.7265(3) 0.6201(3) 0.0160(9) Uani 1 1 d . . . . . C23 C -0.0405(5) 0.3203(3) 0.5858(3) 0.0156(9) Uani 1 1 d . . . . . C17 C 0.1823(5) 0.8062(3) 0.8852(3) 0.0155(9) Uani 1 1 d . . . . . C36 C 0.5584(5) 0.7499(3) 0.5876(3) 0.0180(9) Uani 1 1 d . . . . . H36 H 0.5919 0.7034 0.5402 0.022 Uiso 1 1 calc R U . . . C19 C 0.3412(5) 0.9174(3) 1.0144(3) 0.0198(9) Uani 1 1 d . . . . . H19 H 0.4231 0.9270 1.0631 0.024 Uiso 1 1 calc R U . . . C2 C 0.5364(5) 0.3522(3) 0.6821(3) 0.0176(9) Uani 1 1 d . . . . . H2 H 0.6107 0.3537 0.6426 0.021 Uiso 1 1 calc R U . . . C9 C -0.0626(5) 0.3502(3) 0.9491(3) 0.0201(9) Uani 1 1 d . . . . . H9 H -0.1450 0.3534 0.9833 0.024 Uiso 1 1 calc R U . . . C14 C -0.3995(5) 0.6172(3) 0.8211(3) 0.0169(9) Uani 1 1 d . . . . . H14 H -0.4760 0.6600 0.8031 0.020 Uiso 1 1 calc R U . . . C26 C -0.0736(5) 0.0814(3) 0.3966(3) 0.0244(10) Uani 1 1 d . . . . . H26 H -0.0272 0.0560 0.3448 0.029 Uiso 1 1 calc R U . . . C8 C 0.0484(5) 0.2807(3) 0.9608(3) 0.0228(10) Uani 1 1 d . . . . . H8 H 0.0414 0.2359 1.0024 0.027 Uiso 1 1 calc R U . . . C16 C 0.1400(5) 0.7023(3) 0.8237(3) 0.0148(9) Uani 1 1 d . . . . . C29 C -0.2087(5) 0.1544(3) 0.5537(3) 0.0203(9) Uani 1 1 d . . . . . H29 H -0.2534 0.1784 0.6066 0.024 Uiso 1 1 calc R U . . . C18 C 0.3055(5) 0.8201(3) 0.9573(3) 0.0215(10) Uani 1 1 d . . . . . H18 H 0.3642 0.7646 0.9676 0.026 Uiso 1 1 calc R U . . . C7 C 0.1705(5) 0.2782(3) 0.9101(3) 0.0208(10) Uani 1 1 d . . . . . H7 H 0.2460 0.2307 0.9162 0.025 Uiso 1 1 calc R U . . . C33 C 0.4584(5) 0.8910(3) 0.7279(3) 0.0203(9) Uani 1 1 d . . . . . H33 H 0.4248 0.9388 0.7743 0.024 Uiso 1 1 calc R U . . . C27 C -0.1885(5) 0.0220(3) 0.4234(3) 0.0231(10) Uani 1 1 d . . . . . C28 C -0.2571(5) 0.0570(3) 0.5007(3) 0.0258(10) Uani 1 1 d . . . . . H28 H -0.3347 0.0161 0.5173 0.031 Uiso 1 1 calc R U . . . C34 C 0.5956(5) 0.9106(3) 0.6951(3) 0.0204(9) Uani 1 1 d . . . . . C21 C 0.1320(5) 0.9884(3) 0.9251(3) 0.0207(9) Uani 1 1 d . . . . . H21 H 0.0755 1.0446 0.9141 0.025 Uiso 1 1 calc R U . . . C35 C 0.6454(5) 0.8414(3) 0.6253(3) 0.0229(10) Uani 1 1 d . . . . . H35 H 0.7376 0.8564 0.6037 0.028 Uiso 1 1 calc R U . . . C22 C 0.0970(5) 0.8911(3) 0.8692(3) 0.0188(9) Uani 1 1 d . . . . . H22 H 0.0154 0.8821 0.8204 0.023 Uiso 1 1 calc R U . . . C25 C -0.0291(5) 0.1799(3) 0.4490(3) 0.0202(9) Uani 1 1 d . . . . . H25 H 0.0451 0.2218 0.4306 0.024 Uiso 1 1 calc R U . . . H37 H -0.217(4) 0.514(3) 0.562(3) 0.040(15) Uiso 1 1 d D . . . . H38 H -0.088(6) 0.596(4) 0.551(3) 0.057(17) Uiso 1 1 d 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 Y1 0.0144(2) 0.0144(2) 0.0108(2) 0.00238(15) 0.00320(15) -0.00033(15) Cl1 0.0311(6) 0.0180(5) 0.0223(6) -0.0002(4) -0.0008(5) 0.0017(5) Cl3 0.0373(7) 0.0238(6) 0.0310(7) 0.0012(5) 0.0062(5) -0.0101(5) Cl2 0.0471(8) 0.0207(6) 0.0382(7) -0.0047(5) -0.0092(6) -0.0030(6) O3 0.0171(15) 0.0177(15) 0.0134(14) 0.0026(12) 0.0050(12) -0.0014(12) O2 0.0172(15) 0.0177(15) 0.0150(15) 0.0028(12) 0.0008(12) -0.0020(12) O5 0.0170(15) 0.0193(16) 0.0161(15) 0.0048(12) 0.0049(12) -0.0039(12) O4 0.0190(15) 0.0187(15) 0.0135(15) 0.0033(12) 0.0067(12) 0.0014(12) OW1 0.0153(16) 0.0186(16) 0.0132(15) 0.0036(12) 0.0006(12) -0.0023(12) O1 0.0187(15) 0.0138(15) 0.0167(15) 0.0039(12) 0.0044(12) 0.0013(12) O6 0.0182(16) 0.0266(17) 0.0151(15) 0.0003(13) 0.0046(12) -0.0039(13) N2 0.0160(18) 0.0113(17) 0.0117(17) -0.0018(13) 0.0031(14) -0.0026(14) N1 0.0160(18) 0.0125(17) 0.0153(17) 0.0001(14) 0.0038(14) -0.0033(14) N3 0.0143(18) 0.0174(18) 0.0104(16) 0.0006(14) 0.0008(14) 0.0021(14) C6 0.016(2) 0.018(2) 0.012(2) 0.0011(17) 0.0037(17) -0.0015(17) C5 0.017(2) 0.013(2) 0.016(2) 0.0050(17) 0.0029(17) 0.0006(17) C30 0.014(2) 0.016(2) 0.015(2) 0.0048(17) 0.0003(17) -0.0001(17) C3 0.016(2) 0.020(2) 0.022(2) -0.0007(18) 0.0049(18) 0.0010(18) C1 0.017(2) 0.019(2) 0.018(2) 0.0027(18) 0.0053(18) -0.0013(18) C4 0.021(2) 0.016(2) 0.018(2) 0.0047(17) 0.0016(18) 0.0012(18) C15 0.019(2) 0.021(2) 0.018(2) 0.0051(18) 0.0032(18) 0.0014(18) C10 0.015(2) 0.017(2) 0.013(2) -0.0011(17) 0.0030(16) -0.0006(17) C11 0.012(2) 0.016(2) 0.013(2) 0.0003(16) 0.0029(16) -0.0035(16) C32 0.017(2) 0.018(2) 0.017(2) 0.0081(17) 0.0039(17) 0.0008(17) C13 0.021(2) 0.021(2) 0.023(2) 0.0041(19) 0.0093(19) 0.0020(19) C20 0.026(2) 0.016(2) 0.018(2) 0.0027(18) 0.0054(19) -0.0013(18) C24 0.015(2) 0.017(2) 0.013(2) 0.0035(17) -0.0014(16) 0.0029(17) C12 0.023(2) 0.015(2) 0.014(2) 0.0038(17) 0.0041(18) -0.0013(18) C31 0.014(2) 0.023(2) 0.013(2) 0.0080(17) 0.0011(16) -0.0004(17) C23 0.013(2) 0.016(2) 0.018(2) 0.0050(17) -0.0009(17) 0.0023(17) C17 0.019(2) 0.017(2) 0.0106(19) 0.0022(16) 0.0051(16) -0.0025(17) C36 0.019(2) 0.018(2) 0.019(2) 0.0050(18) 0.0070(18) 0.0004(17) C19 0.023(2) 0.019(2) 0.016(2) 0.0024(18) -0.0008(18) -0.0019(18) C2 0.014(2) 0.024(2) 0.015(2) 0.0016(18) 0.0058(17) -0.0010(18) C9 0.023(2) 0.022(2) 0.016(2) 0.0046(18) 0.0089(18) -0.0003(19) C14 0.015(2) 0.018(2) 0.018(2) 0.0042(17) 0.0030(17) 0.0015(17) C26 0.023(2) 0.027(3) 0.019(2) -0.0047(19) 0.0003(19) 0.005(2) C8 0.025(3) 0.024(2) 0.026(2) 0.015(2) 0.012(2) 0.0018(19) C16 0.016(2) 0.017(2) 0.014(2) 0.0038(17) 0.0095(17) -0.0015(17) C29 0.022(2) 0.020(2) 0.019(2) 0.0022(18) 0.0045(18) 0.0017(18) C18 0.028(3) 0.018(2) 0.021(2) 0.0074(18) 0.0049(19) 0.0031(19) C7 0.023(2) 0.020(2) 0.021(2) 0.0061(19) 0.0037(19) 0.0070(19) C33 0.024(2) 0.020(2) 0.017(2) 0.0029(18) 0.0070(18) 0.0008(18) C27 0.031(3) 0.017(2) 0.018(2) 0.0009(18) -0.0066(19) 0.0020(19) C28 0.028(3) 0.021(2) 0.028(3) 0.010(2) -0.001(2) -0.006(2) C34 0.024(2) 0.019(2) 0.017(2) 0.0035(18) -0.0013(18) -0.0055(18) C21 0.025(2) 0.019(2) 0.019(2) 0.0033(18) 0.0027(19) 0.0033(19) C35 0.016(2) 0.026(2) 0.027(2) 0.004(2) 0.0076(19) -0.0069(19) C22 0.018(2) 0.021(2) 0.019(2) 0.0065(18) 0.0020(18) -0.0001(18) C25 0.018(2) 0.023(2) 0.018(2) 0.0009(18) 0.0013(18) 0.0014(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Y1 O5 2.262(3) . ? Y1 OW1 2.329(3) . ? Y1 O2 2.425(3) . ? Y1 O4 2.427(3) . ? Y1 O1 2.473(3) . ? Y1 O3 2.477(3) . ? Y1 N1 2.513(3) . ? Y1 N3 2.541(3) . ? Y1 N2 2.570(3) . ? Y1 C16 2.793(4) . ? Y1 C23 2.825(4) . ? Cl1 C20 1.746(4) . ? Cl3 C34 1.756(4) . ? Cl2 C27 1.746(4) . ? O3 C23 1.270(4) . ? O2 C16 1.262(5) . ? O5 C30 1.279(4) . ? O4 C23 1.269(5) . ? OW1 H37 0.951(19) . ? OW1 H38 0.949(19) . ? O1 C16 1.268(5) . ? O6 C30 1.239(4) . ? N2 C6 1.348(5) . ? N2 C10 1.351(5) . ? N1 C1 1.343(5) . ? N1 C5 1.354(5) . ? N3 C15 1.348(5) . ? N3 C11 1.350(5) . ? C6 C7 1.386(5) . ? C6 C5 1.494(5) . ? C5 C4 1.390(5) . ? C30 C31 1.504(6) . ? C3 C4 1.385(5) . ? C3 C2 1.387(6) . ? C3 H3 0.9300 . ? C1 C2 1.385(5) . ? C1 H1 0.9300 . ? C4 H4 0.9300 . ? C15 C14 1.385(5) . ? C15 H15 0.9300 . ? C10 C9 1.391(5) . ? C10 C11 1.487(5) . ? C11 C12 1.387(5) . ? C32 C33 1.385(6) . ? C32 C31 1.394(5) . ? C32 H32 0.9300 . ? C13 C14 1.380(6) . ? C13 C12 1.393(6) . ? C13 H13 0.9300 . ? C20 C19 1.382(6) . ? C20 C21 1.386(6) . ? C24 C29 1.390(5) . ? C24 C25 1.390(5) . ? C24 C23 1.491(6) . ? C12 H12 0.9300 . ? C31 C36 1.396(5) . ? C17 C18 1.389(6) . ? C17 C22 1.400(5) . ? C17 C16 1.498(5) . ? C36 C35 1.376(6) . ? C36 H36 0.9300 . ? C19 C18 1.396(6) . ? C19 H19 0.9300 . ? C2 H2 0.9300 . ? C9 C8 1.370(6) . ? C9 H9 0.9300 . ? C14 H14 0.9300 . ? C26 C27 1.383(6) . ? C26 C25 1.392(6) . ? C26 H26 0.9300 . ? C8 C7 1.379(6) . ? C8 H8 0.9300 . ? C29 C28 1.390(6) . ? C29 H29 0.9300 . ? C18 H18 0.9300 . ? C7 H7 0.9300 . ? C33 C34 1.379(6) . ? C33 H33 0.9300 . ? C27 C28 1.377(6) . ? C28 H28 0.9300 . ? C34 C35 1.377(6) . ? C21 C22 1.388(6) . ? C21 H21 0.9300 . ? C35 H35 0.9300 . ? C22 H22 0.9300 . ? C25 H25 0.9300 . ? 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 Y1 OW1 84.98(10) . . ? O5 Y1 O2 75.48(9) . . ? OW1 Y1 O2 75.14(9) . . ? O5 Y1 O4 134.37(9) . . ? OW1 Y1 O4 80.94(10) . . ? O2 Y1 O4 139.68(9) . . ? O5 Y1 O1 82.82(9) . . ? OW1 Y1 O1 128.96(9) . . ? O2 Y1 O1 53.82(9) . . ? O4 Y1 O1 137.98(9) . . ? O5 Y1 O3 81.25(9) . . ? OW1 Y1 O3 76.20(9) . . ? O2 Y1 O3 144.31(9) . . ? O4 Y1 O3 53.29(9) . . ? O1 Y1 O3 148.63(9) . . ? O5 Y1 N1 81.45(10) . . ? OW1 Y1 N1 145.39(10) . . ? O2 Y1 N1 130.65(10) . . ? O4 Y1 N1 86.12(10) . . ? O1 Y1 N1 80.68(10) . . ? O3 Y1 N1 70.36(10) . . ? O5 Y1 N3 144.12(10) . . ? OW1 Y1 N3 79.22(10) . . ? O2 Y1 N3 69.41(10) . . ? O4 Y1 N3 74.59(10) . . ? O1 Y1 N3 82.52(10) . . ? O3 Y1 N3 124.80(10) . . ? N1 Y1 N3 127.79(10) . . ? O5 Y1 N2 139.19(10) . . ? OW1 Y1 N2 135.83(10) . . ? O2 Y1 N2 110.24(10) . . ? O4 Y1 N2 67.20(9) . . ? O1 Y1 N2 71.15(9) . . ? O3 Y1 N2 105.10(10) . . ? N1 Y1 N2 64.07(10) . . ? N3 Y1 N2 63.72(10) . . ? O5 Y1 C16 77.28(10) . . ? OW1 Y1 C16 101.96(11) . . ? O2 Y1 C16 26.82(10) . . ? O4 Y1 C16 148.13(10) . . ? O1 Y1 C16 27.00(10) . . ? O3 Y1 C16 158.53(10) . . ? N1 Y1 C16 105.81(11) . . ? N3 Y1 C16 74.84(11) . . ? N2 Y1 C16 91.17(11) . . ? O5 Y1 C23 107.87(11) . . ? OW1 Y1 C23 77.18(11) . . ? O2 Y1 C23 151.71(10) . . ? O4 Y1 C23 26.60(10) . . ? O1 Y1 C23 153.29(10) . . ? O3 Y1 C23 26.69(10) . . ? N1 Y1 C23 76.99(11) . . ? N3 Y1 C23 99.77(11) . . ? N2 Y1 C23 85.91(11) . . ? C16 Y1 C23 174.59(11) . . ? C23 O3 Y1 92.2(2) . . ? C16 O2 Y1 93.1(2) . . ? C30 O5 Y1 170.0(3) . . ? C23 O4 Y1 94.5(2) . . ? Y1 OW1 H37 125(3) . . ? Y1 OW1 H38 112(3) . . ? H37 OW1 H38 111(4) . . ? C16 O1 Y1 90.7(2) . . ? C6 N2 C10 118.4(3) . . ? C6 N2 Y1 120.2(2) . . ? C10 N2 Y1 120.3(3) . . ? C1 N1 C5 117.7(3) . . ? C1 N1 Y1 119.9(3) . . ? C5 N1 Y1 122.3(3) . . ? C15 N3 C11 117.9(3) . . ? C15 N3 Y1 119.9(3) . . ? C11 N3 Y1 122.2(2) . . ? N2 C6 C7 122.3(4) . . ? N2 C6 C5 116.2(3) . . ? C7 C6 C5 121.5(4) . . ? N1 C5 C4 121.7(4) . . ? N1 C5 C6 116.2(3) . . ? C4 C5 C6 122.1(4) . . ? O6 C30 O5 125.4(4) . . ? O6 C30 C31 118.0(3) . . ? O5 C30 C31 116.6(3) . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? N1 C1 C2 123.8(4) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N3 C15 C14 123.4(4) . . ? N3 C15 H15 118.3 . . ? C14 C15 H15 118.3 . . ? N2 C10 C9 121.5(4) . . ? N2 C10 C11 117.0(3) . . ? C9 C10 C11 121.4(4) . . ? N3 C11 C12 122.2(4) . . ? N3 C11 C10 116.0(3) . . ? C12 C11 C10 121.8(4) . . ? C33 C32 C31 121.3(4) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C14 C13 C12 119.5(4) . . ? C14 C13 H13 120.3 . . ? C12 C13 H13 120.3 . . ? C19 C20 C21 122.0(4) . . ? C19 C20 Cl1 119.0(3) . . ? C21 C20 Cl1 119.0(3) . . ? C29 C24 C25 119.2(4) . . ? C29 C24 C23 120.8(4) . . ? C25 C24 C23 120.1(4) . . ? C11 C12 C13 118.8(4) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C32 C31 C36 118.5(4) . . ? C32 C31 C30 121.0(4) . . ? C36 C31 C30 120.5(4) . . ? O4 C23 O3 120.1(4) . . ? O4 C23 C24 119.4(4) . . ? O3 C23 C24 120.5(4) . . ? O4 C23 Y1 58.9(2) . . ? O3 C23 Y1 61.2(2) . . ? C24 C23 Y1 177.6(3) . . ? C18 C17 C22 119.4(4) . . ? C18 C17 C16 121.2(4) . . ? C22 C17 C16 119.5(4) . . ? C35 C36 C31 120.4(4) . . ? C35 C36 H36 119.8 . . ? C31 C36 H36 119.8 . . ? C20 C19 C18 119.3(4) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C1 C2 C3 118.0(4) . . ? C1 C2 H2 121.0 . . ? C3 C2 H2 121.0 . . ? C8 C9 C10 119.6(4) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C13 C14 C15 118.2(4) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C27 C26 C25 118.6(4) . . ? C27 C26 H26 120.7 . . ? C25 C26 H26 120.7 . . ? C9 C8 C7 119.2(4) . . ? C9 C8 H8 120.4 . . ? C7 C8 H8 120.4 . . ? O2 C16 O1 122.4(4) . . ? O2 C16 C17 117.9(4) . . ? O1 C16 C17 119.7(4) . . ? O2 C16 Y1 60.1(2) . . ? O1 C16 Y1 62.3(2) . . ? C17 C16 Y1 177.0(3) . . ? C28 C29 C24 120.6(4) . . ? C28 C29 H29 119.7 . . ? C24 C29 H29 119.7 . . ? C17 C18 C19 120.1(4) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C8 C7 C6 119.0(4) . . ? C8 C7 H7 120.5 . . ? C6 C7 H7 120.5 . . ? C34 C33 C32 118.5(4) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C28 C27 C26 121.8(4) . . ? C28 C27 Cl2 118.7(4) . . ? C26 C27 Cl2 119.5(3) . . ? C27 C28 C29 119.0(4) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C33 C34 C35 121.4(4) . . ? C33 C34 Cl3 119.4(3) . . ? C35 C34 Cl3 119.2(3) . . ? C20 C21 C22 118.2(4) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C36 C35 C34 119.9(4) . . ? C36 C35 H35 120.0 . . ? C34 C35 H35 120.0 . . ? C21 C22 C17 121.1(4) . . ? C21 C22 H22 119.5 . . ? C17 C22 H22 119.5 . . ? C24 C25 C26 120.8(4) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? _refine_diff_density_max 0.565 _refine_diff_density_min -0.771 _refine_diff_density_rms 0.122 _shelxl_version_number 2013-4 _shelx_res_file ; TITL Pbar1 in P-1 CELL 0.71073 8.7063 13.1081 14.7877 100.278 97.723 92.392 ZERR 2.00 0.0031 0.0047 0.0053 0.006 0.006 0.006 LATT 1 SFAC C H N O CL Y UNIT 72 50 6 14 6 2 MERG 2 DFIX 0.98 OW1 H37 DFIX 0.98 OW1 H38 BOND $H FMAP 2 PLAN 10 ACTA 51.00 L.S. 12 WGHT 0.044700 FVAR 0.14975 Y1 6 0.062400 0.513466 0.701109 11.00000 0.01438 0.01439 = 0.01083 0.00238 0.00320 -0.00033 CL1 5 0.296937 1.120422 1.070581 11.00000 0.03115 0.01798 = 0.02226 -0.00015 -0.00084 0.00167 CL3 5 0.709515 1.026019 0.743462 11.00000 0.03731 0.02377 = 0.03100 0.00122 0.00625 -0.01012 CL2 5 -0.250819 -0.100179 0.356819 11.00000 0.04715 0.02073 = 0.03822 -0.00466 -0.00919 -0.00296 O3 4 0.062124 0.377271 0.561482 11.00000 0.01706 0.01769 = 0.01342 0.00257 0.00500 -0.00136 O2 4 0.035080 0.696800 0.754945 11.00000 0.01717 0.01775 = 0.01501 0.00278 0.00084 -0.00197 O5 4 0.228970 0.595738 0.628559 11.00000 0.01703 0.01933 = 0.01607 0.00485 0.00485 -0.00389 O4 4 -0.094901 0.350229 0.660809 11.00000 0.01896 0.01870 = 0.01354 0.00329 0.00671 0.00138 OW1 4 -0.129983 0.558585 0.592698 11.00000 0.01526 0.01862 = 0.01320 0.00361 0.00056 -0.00227 O1 4 0.209792 0.623685 0.841716 11.00000 0.01872 0.01381 = 0.01666 0.00386 0.00437 0.00134 O6 4 0.346587 0.580401 0.501694 11.00000 0.01816 0.02663 = 0.01511 0.00028 0.00462 -0.00388 N2 3 0.069352 0.415022 0.836947 11.00000 0.01603 0.01128 = 0.01171 -0.00183 0.00306 -0.00263 N1 3 0.290600 0.405070 0.724957 11.00000 0.01598 0.01248 = 0.01535 0.00013 0.00383 -0.00335 N3 3 -0.160366 0.538442 0.795987 11.00000 0.01429 0.01739 = 0.01035 0.00056 0.00083 0.00214 C6 1 0.178962 0.347341 0.849889 11.00000 0.01565 0.01807 = 0.01246 0.00113 0.00368 -0.00148 C5 1 0.309317 0.349216 0.793885 11.00000 0.01675 0.01346 = 0.01550 0.00503 0.00290 0.00060 C30 1 0.325164 0.626469 0.579269 11.00000 0.01385 0.01637 = 0.01489 0.00475 0.00034 -0.00005 C3 1 0.556507 0.297335 0.754428 11.00000 0.01564 0.01958 = 0.02188 -0.00075 0.00493 0.00102 AFIX 43 H3 2 0.646210 0.262634 0.765354 11.00000 -1.20000 AFIX 0 C1 1 0.402405 0.404571 0.670530 11.00000 0.01692 0.01891 = 0.01839 0.00265 0.00529 -0.00127 AFIX 43 H1 2 0.389032 0.441583 0.622239 11.00000 -1.20000 AFIX 0 C4 1 0.441053 0.295032 0.810086 11.00000 0.02065 0.01641 = 0.01770 0.00465 0.00164 0.00120 AFIX 43 H4 2 0.451591 0.257446 0.858037 11.00000 -1.20000 AFIX 0 C15 1 -0.272518 0.601525 0.774308 11.00000 0.01853 0.02065 = 0.01800 0.00509 0.00321 0.00143 AFIX 43 H15 2 -0.264162 0.636273 0.725394 11.00000 -1.20000 AFIX 0 C10 1 -0.051260 0.415908 0.885735 11.00000 0.01516 0.01656 = 0.01260 -0.00107 0.00297 -0.00064 C11 1 -0.172796 0.489027 0.867566 11.00000 0.01235 0.01637 = 0.01258 0.00025 0.00295 -0.00354 C32 1 0.371828 0.798477 0.690213 11.00000 0.01745 0.01836 = 0.01721 0.00813 0.00391 0.00077 AFIX 43 H32 2 0.279504 0.784120 0.712071 11.00000 -1.20000 AFIX 0 C13 1 -0.409432 0.567714 0.895242 11.00000 0.02108 0.02105 = 0.02336 0.00408 0.00933 0.00203 AFIX 43 H13 2 -0.492861 0.577092 0.928406 11.00000 -1.20000 AFIX 0 C20 1 0.253627 0.999394 0.997751 11.00000 0.02637 0.01596 = 0.01839 0.00274 0.00535 -0.00132 C24 1 -0.094128 0.216248 0.528500 11.00000 0.01482 0.01657 = 0.01306 0.00347 -0.00139 0.00286 C12 1 -0.293507 0.503563 0.919997 11.00000 0.02340 0.01508 = 0.01378 0.00375 0.00412 -0.00131 AFIX 43 H12 2 -0.296978 0.471067 0.970756 11.00000 -1.20000 AFIX 0 C31 1 0.420246 0.726471 0.620142 11.00000 0.01369 0.02266 = 0.01289 0.00800 0.00110 -0.00042 C23 1 -0.040498 0.320256 0.585811 11.00000 0.01275 0.01620 = 0.01775 0.00498 -0.00087 0.00227 C17 1 0.182278 0.806222 0.885188 11.00000 0.01927 0.01699 = 0.01058 0.00218 0.00507 -0.00251 C36 1 0.558413 0.749877 0.587609 11.00000 0.01920 0.01794 = 0.01853 0.00496 0.00705 0.00036 AFIX 43 H36 2 0.591858 0.703397 0.540192 11.00000 -1.20000 AFIX 0 C19 1 0.341208 0.917407 1.014419 11.00000 0.02280 0.01872 = 0.01631 0.00244 -0.00077 -0.00194 AFIX 43 H19 2 0.423058 0.926950 1.063138 11.00000 -1.20000 AFIX 0 C2 1 0.536412 0.352161 0.682129 11.00000 0.01378 0.02445 = 0.01461 0.00161 0.00578 -0.00095 AFIX 43 H2 2 0.610726 0.353675 0.642626 11.00000 -1.20000 AFIX 0 C9 1 -0.062604 0.350215 0.949115 11.00000 0.02317 0.02246 = 0.01646 0.00460 0.00894 -0.00027 AFIX 43 H9 2 -0.144996 0.353431 0.983336 11.00000 -1.20000 AFIX 0 C14 1 -0.399501 0.617250 0.821107 11.00000 0.01499 0.01768 = 0.01841 0.00419 0.00304 0.00154 AFIX 43 H14 2 -0.475972 0.659996 0.803095 11.00000 -1.20000 AFIX 0 C26 1 -0.073624 0.081351 0.396638 11.00000 0.02336 0.02667 = 0.01942 -0.00475 0.00028 0.00493 AFIX 43 H26 2 -0.027158 0.056035 0.344812 11.00000 -1.20000 AFIX 0 C8 1 0.048395 0.280737 0.960802 11.00000 0.02515 0.02370 = 0.02570 0.01514 0.01159 0.00180 AFIX 43 H8 2 0.041442 0.235856 1.002426 11.00000 -1.20000 AFIX 0 C16 1 0.139962 0.702290 0.823742 11.00000 0.01615 0.01698 = 0.01357 0.00376 0.00955 -0.00149 C29 1 -0.208713 0.154420 0.553734 11.00000 0.02170 0.01992 = 0.01912 0.00222 0.00453 0.00165 AFIX 43 H29 2 -0.253393 0.178448 0.606562 11.00000 -1.20000 AFIX 0 C18 1 0.305465 0.820121 0.957328 11.00000 0.02773 0.01773 = 0.02088 0.00736 0.00492 0.00309 AFIX 43 H18 2 0.364201 0.764552 0.967609 11.00000 -1.20000 AFIX 0 C7 1 0.170526 0.278155 0.910115 11.00000 0.02277 0.02028 = 0.02098 0.00613 0.00375 0.00697 AFIX 43 H7 2 0.246039 0.230741 0.916244 11.00000 -1.20000 AFIX 0 C33 1 0.458434 0.890968 0.727939 11.00000 0.02450 0.02008 = 0.01705 0.00290 0.00705 0.00081 AFIX 43 H33 2 0.424839 0.938766 0.774348 11.00000 -1.20000 AFIX 0 C27 1 -0.188477 0.021955 0.423351 11.00000 0.03103 0.01653 = 0.01802 0.00091 -0.00656 0.00205 C28 1 -0.257113 0.057020 0.500734 11.00000 0.02817 0.02101 = 0.02828 0.00983 -0.00056 -0.00621 AFIX 43 H28 2 -0.334720 0.016111 0.517276 11.00000 -1.20000 AFIX 0 C34 1 0.595578 0.910577 0.695137 11.00000 0.02399 0.01854 = 0.01697 0.00352 -0.00127 -0.00545 C21 1 0.132037 0.988358 0.925098 11.00000 0.02481 0.01873 = 0.01851 0.00333 0.00271 0.00329 AFIX 43 H21 2 0.075491 1.044647 0.914096 11.00000 -1.20000 AFIX 0 C35 1 0.645376 0.841368 0.625339 11.00000 0.01634 0.02555 = 0.02715 0.00408 0.00762 -0.00688 AFIX 43 H35 2 0.737649 0.856409 0.603709 11.00000 -1.20000 AFIX 0 C22 1 0.096952 0.891059 0.869219 11.00000 0.01819 0.02050 = 0.01855 0.00653 0.00203 -0.00010 AFIX 43 H22 2 0.015400 0.882071 0.820354 11.00000 -1.20000 AFIX 0 C25 1 -0.029083 0.179867 0.449025 11.00000 0.01788 0.02317 = 0.01805 0.00094 0.00130 0.00140 AFIX 43 H25 2 0.045096 0.221825 0.430603 11.00000 -1.20000 AFIX 0 H37 2 -0.217366 0.513933 0.561663 11.00000 0.03985 H38 2 -0.088004 0.595851 0.551207 11.00000 0.05679 HKLF 4 REM Pbar1 in P-1 REM R1 = 0.0554 for 5095 Fo > 4sig(Fo) and 0.1085 for all 8206 data REM 459 parameters refined using 2 restraints END WGHT 0.0442 0.0000 REM Highest difference peak 0.565, deepest hole -0.771, 1-sigma level 0.122 Q1 1 0.4039 1.1270 1.0428 11.00000 0.05 0.56 Q2 1 -0.0790 0.5220 0.6778 11.00000 0.05 0.51 Q3 1 0.7194 0.8523 0.5613 11.00000 0.05 0.50 Q4 1 0.8458 1.0047 0.7675 11.00000 0.05 0.50 Q5 1 -0.1363 -0.0805 0.3258 11.00000 0.05 0.50 Q6 1 -0.1098 0.4554 0.8763 11.00000 0.05 0.47 Q7 1 -0.1348 -0.1973 0.3799 11.00000 0.05 0.46 Q8 1 0.2741 0.8606 0.9232 11.00000 0.05 0.46 Q9 1 -0.0184 0.8394 0.7109 11.00000 0.05 0.45 Q10 1 0.0067 0.4221 0.8635 11.00000 0.05 0.45 ; _shelx_res_checksum 34648 _shelx_hkl_file ; -1 0 0 184.53 5.05 -1 0 0 182.19 5.40 1 0 0 185.74 5.54 1 0 0 180.57 5.25 -2 0 0 30.57 1.58 -2 0 0 29.07 2.01 2 0 0 32.98 2.23 2 0 0 27.97 1.73 -3 0 0 84.19 3.26 -3 0 0 77.95 3.93 3 0 0 89.96 3.58 3 0 0 84.79 4.22 -4 0 0 1.51 0.87 -4 0 0 3.39 1.51 4 0 0 1.10 0.99 4 0 0 0.85 1.31 -5 0 0 34.90 2.50 -5 0 0 32.34 3.52 5 0 0 38.47 3.99 5 0 0 42.93 2.79 -6 0 0 65.77 3.75 -6 0 0 71.07 4.95 6 0 0 60.32 3.77 6 0 0 69.46 5.08 -7 0 0 3.59 1.43 -7 0 0 -0.99 1.87 7 0 0 4.26 1.66 7 0 0 4.46 2.44 -8 0 0 88.21 6.41 8 0 0 77.92 7.38 -9 0 0 46.58 5.67 9 0 0 44.22 5.99 -10 0 0 9.70 3.59 10 0 0 13.50 4.09 -11 0 0 -1.46 2.68 11 0 0 -1.12 3.26 11 -1 0 0.60 3.44 -11 1 0 10.15 4.04 10 -1 0 4.09 3.23 -10 1 0 6.47 3.28 9 -1 0 15.64 3.80 -9 1 0 4.53 2.83 8 -1 0 101.09 7.28 8 -1 0 106.77 5.96 -8 1 0 95.41 6.79 7 -1 0 23.52 3.84 7 -1 0 38.73 3.77 -7 1 0 19.32 3.46 -7 1 0 25.68 2.81 6 -1 0 0.66 1.23 6 -1 0 -0.21 1.50 -6 1 0 0.68 1.52 -6 1 0 -0.39 0.99 5 -1 0 1.37 1.36 5 -1 0 2.40 1.29 -5 1 0 4.33 1.20 -5 1 0 1.52 1.43 4 -1 0 17.46 2.08 4 -1 0 21.19 2.64 -4 1 0 13.89 1.63 -4 1 0 15.74 2.27 3 -1 0 26.06 2.22 3 -1 0 27.79 2.58 -3 1 0 25.96 1.78 -3 1 0 24.83 2.35 2 -1 0 504.82 14.30 2 -1 0 496.97 14.41 -2 1 0 507.61 13.51 -2 1 0 487.89 14.18 1 -1 0 256.72 7.43 1 -1 0 260.67 7.63 -1 1 0 266.55 7.46 -1 1 0 259.29 7.18 0 -1 0 236.09 6.27 0 -1 0 224.21 6.42 0 1 0 225.08 6.22 -1 -1 0 146.31 4.54 -1 -1 0 140.06 4.17 -1 -1 0 142.06 4.18 -1 -1 0 142.63 4.18 1 1 0 136.49 4.59 -2 -1 0 72.24 2.71 -2 -1 0 68.35 3.23 2 1 0 71.96 2.71 2 1 0 71.68 3.32 -3 -1 0 40.98 2.16 -3 -1 0 39.44 2.78 3 1 0 37.78 3.17 3 1 0 38.90 2.14 -4 -1 0 52.17 2.73 -4 -1 0 49.92 3.47 4 1 0 42.77 2.60 4 1 0 54.52 3.78 -5 -1 0 0.36 0.90 -5 -1 0 2.40 1.61 5 1 0 -0.41 0.95 5 1 0 0.62 1.40 -6 -1 0 30.87 3.88 -6 -1 0 40.97 2.95 6 1 0 36.24 4.37 6 1 0 42.16 2.98 -7 -1 0 78.28 5.50 -7 -1 0 72.72 4.16 7 1 0 67.07 4.16 7 1 0 58.02 6.01 -8 -1 0 8.37 3.04 8 1 0 11.22 3.46 -9 -1 0 25.39 4.57 9 1 0 15.70 4.10 -10 -1 0 23.38 4.77 10 1 0 18.93 4.94 -11 -1 0 11.48 4.07 11 1 0 7.28 4.15 11 -2 0 -2.14 2.92 -11 2 0 -1.36 2.69 10 -2 0 1.54 2.88 -10 2 0 -1.44 2.53 9 -2 0 17.28 4.16 -9 2 0 10.29 3.51 8 -2 0 24.15 4.23 8 -2 0 22.74 3.52 -8 2 0 21.31 3.74 7 -2 0 4.67 2.32 7 -2 0 9.70 2.38 -7 2 0 8.42 2.52 -7 2 0 8.84 1.91 6 -2 0 7.79 1.96 6 -2 0 9.63 2.46 -6 2 0 7.17 2.15 -6 2 0 6.87 1.55 5 -2 0 13.63 2.14 5 -2 0 9.32 2.21 -5 2 0 12.26 2.30 -5 2 0 11.99 1.73 4 -2 0 14.27 1.97 4 -2 0 13.32 2.11 -4 2 0 13.59 2.11 -4 2 0 14.77 1.75 3 -2 0 2.41 1.07 3 -2 0 0.81 1.09 -3 2 0 2.05 1.20 -3 2 0 1.82 0.91 2 -2 0 110.31 4.14 2 -2 0 113.09 4.43 -2 2 0 107.07 3.95 -2 2 0 113.15 4.26 1 -2 0 62.06 2.24 1 -2 0 59.74 2.79 -1 2 0 63.08 2.50 0 -2 0 212.14 6.27 0 -2 0 205.98 5.98 0 -2 0 222.94 6.48 0 2 0 209.19 5.99 0 2 0 212.76 6.28 -1 -2 0 79.38 3.10 -1 -2 0 77.90 2.84 1 2 0 77.17 3.11 1 2 0 71.96 2.89 -2 -2 0 55.35 2.40 -2 -2 0 53.17 2.92 2 2 0 56.89 3.12 -3 -2 0 66.54 3.72 -3 -2 0 68.91 3.09 3 2 0 69.87 2.96 3 2 0 73.27 3.91 -4 -2 0 2.87 1.47 -4 -2 0 4.66 1.14 4 2 0 2.49 1.00 4 2 0 4.08 1.56 -5 -2 0 88.70 4.06 -5 -2 0 72.48 4.81 5 2 0 84.38 3.92 5 2 0 83.37 5.32 -6 -2 0 37.02 3.17 -6 -2 0 36.04 4.20 6 2 0 38.42 2.87 6 2 0 41.92 4.71 -7 -2 0 13.71 3.12 -7 -2 0 12.04 2.19 7 2 0 8.54 2.92 -8 -2 0 -0.90 1.98 8 2 0 4.23 2.55 -9 -2 0 57.54 6.48 9 2 0 57.12 6.86 -10 -2 0 9.67 3.72 10 2 0 12.18 4.27 -11 -2 0 2.26 3.14 11 2 0 -1.00 3.06 11 -3 0 1.62 3.35 -11 3 0 0.71 3.23 10 -3 0 6.63 3.66 -10 3 0 2.68 2.91 9 -3 0 7.25 3.11 -9 3 0 7.19 3.04 8 -3 0 62.38 5.61 8 -3 0 70.66 6.73 -8 3 0 66.11 4.44 -8 3 0 62.60 6.11 7 -3 0 3.42 1.83 7 -3 0 1.85 2.05 -7 3 0 2.19 1.42 -7 3 0 0.14 1.67 6 -3 0 0.23 1.55 6 -3 0 -0.79 1.43 -6 3 0 3.59 1.82 -6 3 0 3.34 1.39 5 -3 0 -0.29 1.15 5 -3 0 0.76 1.37 -5 3 0 -1.48 0.85 -5 3 0 0.57 1.34 4 -3 0 0.33 1.29 4 -3 0 2.76 1.41 -4 3 0 2.66 1.09 -4 3 0 2.74 1.41 3 -3 0 15.44 1.89 3 -3 0 19.33 2.30 -3 3 0 17.90 2.14 -3 3 0 16.01 1.79 2 -3 0 24.11 2.42 2 -3 0 24.49 1.92 -2 3 0 26.72 2.24 -2 3 0 25.67 2.09 -2 3 0 25.29 2.23 1 -3 0 1.55 0.84 1 -3 0 1.33 0.63 1 -3 0 1.08 0.98 -1 3 0 1.94 0.86 0 -3 0 7.67 1.30 0 -3 0 6.56 1.20 0 3 0 7.44 0.87 0 3 0 9.74 1.34 -1 -3 0 86.28 3.66 -1 -3 0 87.04 3.48 1 3 0 90.67 3.62 1 3 0 85.23 3.55 -2 -3 0 7.71 1.22 -2 -3 0 4.81 1.35 2 3 0 7.16 1.31 2 3 0 5.45 1.45 -3 -3 0 8.86 1.79 -3 -3 0 8.25 1.27 3 3 0 6.74 1.35 3 3 0 7.00 1.76 -4 -3 0 6.84 1.36 -4 -3 0 5.44 1.27 -4 -3 0 9.33 2.06 4 3 0 6.22 1.89 -5 -3 0 2.90 1.22 -5 -3 0 4.79 1.33 -5 -3 0 5.55 2.08 5 3 0 5.30 1.90 -6 -3 0 15.11 2.33 -6 -3 0 14.02 2.92 -6 -3 0 18.95 2.26 6 3 0 16.01 3.34 -7 -3 0 75.04 6.55 -7 -3 0 78.70 4.59 7 3 0 73.61 6.88 -8 -3 0 10.01 3.33 8 3 0 11.54 3.44 -9 -3 0 12.04 3.79 9 3 0 8.88 3.49 -10 -3 0 0.35 2.78 10 3 0 0.52 2.79 -11 -3 0 6.55 3.69 11 3 0 -1.95 3.19 11 -4 0 1.52 3.54 -11 4 0 -1.77 3.07 10 -4 0 16.56 4.39 -10 4 0 11.27 3.82 9 -4 0 17.30 3.72 9 -4 0 22.75 4.57 -9 4 0 22.70 4.28 8 -4 0 23.81 4.00 8 -4 0 23.11 3.73 -8 4 0 20.16 3.74 -8 4 0 28.36 3.59 7 -4 0 1.05 1.99 7 -4 0 1.45 1.83 -7 4 0 0.14 1.73 -7 4 0 3.60 1.64 6 -4 0 17.93 3.03 6 -4 0 14.05 2.71 -6 4 0 18.68 2.98 -6 4 0 18.29 2.42 5 -4 0 -0.12 1.19 5 -4 0 1.40 1.43 -5 4 0 -0.87 1.24 -5 4 0 1.72 1.26 4 -4 0 9.40 2.07 4 -4 0 10.05 1.87 -4 4 0 7.85 1.76 -4 4 0 7.11 1.55 3 -4 0 79.20 3.70 3 -4 0 72.30 4.23 -3 4 0 71.93 3.89 -3 4 0 74.99 3.69 2 -4 0 45.66 3.37 2 -4 0 58.92 2.68 -2 4 0 63.40 3.11 -2 4 0 59.43 3.17 -2 4 0 56.19 3.05 1 -4 0 40.55 2.72 1 -4 0 39.19 2.43 -1 4 0 42.84 2.60 -1 4 0 40.45 1.72 0 -4 0 42.00 2.43 0 -4 0 36.77 2.57 0 4 0 39.21 1.93 0 4 0 35.50 2.51 -1 -4 0 80.57 3.75 -1 -4 0 79.32 3.63 1 4 0 80.25 3.69 1 4 0 83.52 3.59 -2 -4 0 71.00 3.29 -2 -4 0 71.65 3.76 2 4 0 65.04 3.63 2 4 0 66.73 3.50 -3 -4 0 2.92 1.46 -3 -4 0 3.70 1.17 3 4 0 4.94 1.55 3 4 0 3.41 1.23 -4 -4 0 2.91 1.13 -4 -4 0 6.81 2.00 4 4 0 4.53 1.82 4 4 0 2.05 1.27 -5 -4 0 1.20 1.59 -5 -4 0 1.37 1.13 5 4 0 1.38 1.37 5 4 0 -0.70 1.24 -6 -4 0 27.12 3.89 6 4 0 27.39 3.13 6 4 0 25.61 3.95 -7 -4 0 1.87 2.25 7 4 0 -0.32 1.52 7 4 0 -0.75 1.76 -8 -4 0 2.05 2.45 8 4 0 2.84 2.82 -9 -4 0 5.99 3.46 9 4 0 11.99 3.90 -10 -4 0 4.46 3.36 10 4 0 1.30 3.22 11 4 0 0.88 3.53 -11 5 0 3.34 3.48 10 -5 0 41.04 5.88 -10 5 0 25.09 4.85 9 -5 0 24.38 4.54 9 -5 0 15.65 3.64 -9 5 0 18.24 3.98 8 -5 0 4.20 2.58 8 -5 0 14.58 3.41 -8 5 0 16.05 3.56 -8 5 0 13.83 2.78 7 -5 0 -2.68 1.53 7 -5 0 -0.80 1.54 -7 5 0 0.68 1.51 -7 5 0 1.69 1.91 6 -5 0 6.54 2.30 6 -5 0 9.14 2.35 -6 5 0 7.40 2.25 -6 5 0 12.38 2.22 5 -5 0 0.89 1.37 5 -5 0 2.16 1.79 -5 5 0 3.27 1.47 -5 5 0 3.91 1.70 4 -5 0 81.42 4.98 4 -5 0 77.78 4.22 -4 5 0 83.98 4.22 -4 5 0 80.63 4.52 3 -5 0 16.03 1.80 3 -5 0 13.48 2.37 -3 5 0 11.95 1.89 -3 5 0 14.26 2.10 2 -5 0 24.65 2.40 2 -5 0 21.66 1.72 2 -5 0 16.66 2.43 -2 5 0 20.36 2.28 1 -5 0 82.50 4.25 1 -5 0 77.97 3.77 -1 5 0 73.82 2.73 -1 5 0 82.46 3.90 0 -5 0 23.30 2.30 0 -5 0 22.77 2.38 0 5 0 20.53 2.25 0 5 0 21.00 1.57 -1 -5 0 2.46 1.24 -1 -5 0 3.49 1.32 1 5 0 3.72 1.10 1 5 0 -0.14 0.99 -2 -5 0 188.97 7.45 -2 -5 0 193.11 6.92 2 5 0 203.04 7.37 2 5 0 194.60 7.18 -3 -5 0 10.22 1.67 -3 -5 0 9.16 1.97 3 5 0 7.69 1.90 3 5 0 12.45 2.06 -4 -5 0 28.00 3.25 -4 -5 0 31.11 2.63 4 5 0 22.64 3.18 4 5 0 31.03 3.02 -5 -5 0 8.32 2.43 -5 -5 0 6.10 1.54 5 5 0 7.63 1.93 5 5 0 13.07 2.75 -6 -5 0 16.20 3.15 6 5 0 8.86 2.69 6 5 0 13.85 2.53 -7 -5 0 1.18 2.19 7 5 0 -0.11 2.13 7 5 0 2.90 1.75 -8 -5 0 31.42 4.92 8 5 0 20.80 4.38 -9 -5 0 3.06 2.77 9 5 0 4.98 3.37 -10 -5 0 0.33 3.21 10 5 0 1.48 3.10 -11 6 0 2.48 3.35 -10 6 0 6.09 3.22 9 -6 0 7.71 3.21 9 -6 0 3.49 2.66 -9 6 0 8.11 3.11 8 -6 0 23.17 4.09 8 -6 0 20.85 3.85 -8 6 0 25.20 4.08 -8 6 0 25.83 3.45 7 -6 0 6.08 2.68 7 -6 0 4.79 2.26 -7 6 0 9.19 2.32 -7 6 0 8.56 2.52 6 -6 0 48.85 5.01 6 -6 0 37.65 4.04 -6 6 0 42.74 4.45 -6 6 0 42.26 3.94 5 -6 0 0.84 1.31 5 -6 0 2.36 1.80 -5 6 0 0.24 1.34 -5 6 0 0.24 1.31 4 -6 0 7.16 1.64 4 -6 0 5.70 2.04 -4 6 0 5.21 1.77 -4 6 0 4.34 1.54 3 -6 0 74.52 3.59 3 -6 0 91.28 5.23 -3 6 0 83.21 4.30 -3 6 0 80.40 4.38 -3 6 0 89.97 4.51 2 -6 0 22.89 1.70 2 -6 0 33.54 3.45 2 -6 0 26.86 2.65 -2 6 0 24.23 2.64 1 -6 0 0.88 1.12 1 -6 0 0.42 1.22 -1 6 0 1.64 0.60 -1 6 0 1.28 1.09 0 -6 0 10.47 1.79 0 -6 0 8.78 1.88 0 6 0 13.77 2.06 0 6 0 6.65 1.11 -1 -6 0 418.72 13.56 -1 -6 0 438.11 13.62 1 6 0 434.03 13.60 1 6 0 421.02 12.99 -2 -6 0 0.11 1.28 -2 -6 0 0.99 1.18 2 6 0 -1.39 0.92 2 6 0 0.48 1.09 -3 -6 0 61.43 3.52 -3 -6 0 70.86 4.40 3 6 0 56.22 3.86 3 6 0 61.77 4.16 -4 -6 0 0.80 1.54 -4 -6 0 -0.09 1.22 4 6 0 1.58 1.55 4 6 0 1.15 1.37 -5 -6 0 30.02 3.95 -5 -6 0 32.83 2.99 5 6 0 27.24 3.92 5 6 0 30.46 3.44 -6 -6 0 6.80 2.40 6 6 0 4.03 2.37 6 6 0 1.96 1.88 -7 -6 0 10.81 3.15 7 6 0 9.19 3.24 7 6 0 9.76 2.64 -8 -6 0 23.84 4.46 8 6 0 16.64 4.10 -9 -6 0 12.19 3.83 9 6 0 10.64 4.04 -10 -6 0 0.92 2.98 10 6 0 0.32 3.02 10 -7 0 2.32 3.12 -10 7 0 4.54 3.43 9 -7 0 17.44 4.06 -9 7 0 12.19 3.58 8 -7 0 3.44 2.54 -8 7 0 3.25 2.33 -8 7 0 0.19 1.96 7 -7 0 37.02 4.33 7 -7 0 25.34 4.14 -7 7 0 27.27 3.86 -7 7 0 19.47 3.12 6 -7 0 8.47 2.83 6 -7 0 7.69 2.25 -6 7 0 13.02 2.62 -6 7 0 14.22 2.82 5 -7 0 37.50 4.59 5 -7 0 29.38 3.07 -5 7 0 32.15 3.45 -5 7 0 27.05 3.45 4 -7 0 58.51 3.42 4 -7 0 63.67 4.74 -4 7 0 57.14 4.07 -4 7 0 47.08 4.25 3 -7 0 6.45 2.09 3 -7 0 4.00 1.10 -3 7 0 5.20 1.69 -3 7 0 4.24 1.64 -3 7 0 3.14 1.47 2 -7 0 15.46 2.26 2 -7 0 19.15 2.84 2 -7 0 16.77 1.49 -2 7 0 10.85 2.09 1 -7 0 275.73 9.55 1 -7 0 259.11 10.10 -1 7 0 272.08 9.71 -1 7 0 265.74 7.92 0 -7 0 8.08 1.96 0 -7 0 5.60 1.68 0 7 0 6.92 1.19 0 7 0 4.71 1.65 -1 -7 0 15.17 2.33 -1 -7 0 16.27 2.45 1 7 0 21.85 2.76 1 7 0 20.51 2.20 -2 -7 0 13.13 2.21 -2 -7 0 13.04 2.40 2 7 0 11.20 2.02 2 7 0 10.54 2.13 -3 -7 0 -0.31 1.24 -3 -7 0 0.94 1.46 3 7 0 3.31 1.62 3 7 0 0.45 1.27 -4 -7 0 67.78 3.95 -4 -7 0 56.45 5.21 4 7 0 69.52 4.45 4 7 0 64.18 5.47 -5 -7 0 83.58 5.90 5 7 0 90.69 5.42 5 7 0 98.10 6.16 -6 -7 0 7.35 2.73 6 7 0 10.09 2.56 6 7 0 8.03 2.83 -7 -7 0 57.75 6.41 7 7 0 53.78 6.15 -8 -7 0 70.01 7.37 8 7 0 76.39 7.84 -9 -7 0 -0.74 2.75 9 7 0 1.08 2.81 -10 -7 0 6.25 3.88 10 7 0 -0.71 3.20 10 -8 0 4.52 3.27 -10 8 0 9.16 3.60 9 -8 0 12.72 3.84 -9 8 0 12.43 3.71 8 -8 0 39.83 5.36 -8 8 0 37.41 4.89 -8 8 0 43.98 4.81 7 -8 0 0.10 2.16 -7 8 0 0.95 2.06 -7 8 0 1.76 1.92 6 -8 0 0.87 2.05 -6 8 0 0.69 1.64 -6 8 0 4.28 2.06 5 -8 0 2.67 2.01 -5 8 0 1.58 1.76 -5 8 0 4.03 2.01 4 -8 0 67.77 5.06 -4 8 0 59.94 4.36 -4 8 0 63.33 4.38 3 -8 0 168.89 5.76 3 -8 0 163.50 8.19 -3 8 0 167.98 7.35 -3 8 0 159.34 7.06 -3 8 0 165.21 7.31 2 -8 0 0.96 0.81 2 -8 0 4.07 1.98 2 -8 0 0.93 1.31 -2 8 0 0.52 1.26 1 -8 0 1.13 1.55 1 -8 0 1.73 1.32 -1 8 0 4.18 1.55 -1 8 0 1.92 0.76 0 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3.27 1 -9 0 25.95 3.55 -1 9 0 23.86 1.73 -1 9 0 24.29 3.27 0 -9 0 12.38 2.61 0 -9 0 10.44 2.33 0 9 0 6.84 2.12 0 9 0 7.78 1.42 -1 -9 0 -1.55 1.29 -1 -9 0 1.09 1.57 1 9 0 1.13 1.17 1 9 0 2.11 1.75 -2 -9 0 1.13 1.67 -2 -9 0 0.54 1.64 2 9 0 2.19 1.53 2 9 0 -1.00 1.45 -3 -9 0 0.64 1.57 -3 -9 0 2.18 1.91 3 9 0 0.13 1.66 3 9 0 1.07 1.61 -4 -9 0 5.50 2.06 -4 -9 0 1.72 2.12 4 9 0 1.32 1.68 4 9 0 2.04 2.04 -5 -9 0 7.25 2.61 5 9 0 5.59 2.58 5 9 0 7.30 2.51 -6 -9 0 3.57 2.67 6 9 0 5.70 2.44 6 9 0 1.23 2.23 -7 -9 0 0.94 2.63 7 9 0 6.83 3.21 -8 -9 0 18.78 4.56 8 9 0 20.37 4.76 -9 -9 0 -1.37 3.42 9 9 0 2.17 3.52 9 -10 0 21.36 5.09 8 -10 0 3.79 3.09 -8 10 0 -0.41 2.26 -8 10 0 4.76 2.90 7 -10 0 0.80 2.49 -7 10 0 -0.07 2.15 -7 10 0 0.68 2.20 6 -10 0 6.36 3.04 -6 10 0 7.96 2.62 -6 10 0 9.52 2.85 5 -10 0 4.35 2.52 -5 10 0 6.64 2.42 -5 10 0 3.54 2.11 4 -10 0 31.49 4.59 -4 10 0 38.75 4.29 -4 10 0 30.76 3.99 -4 10 0 34.65 4.15 3 -10 0 15.25 3.46 -3 10 0 16.84 3.03 2 -10 0 2.06 1.77 2 -10 0 1.98 1.99 -2 10 0 0.19 1.56 1 -10 0 28.58 3.91 1 -10 0 30.05 3.62 -1 10 0 29.00 3.89 0 -10 0 116.79 6.23 0 -10 0 112.80 6.60 0 10 0 105.27 6.32 -1 -10 0 0.85 1.73 -1 -10 0 1.26 1.72 1 10 0 1.65 1.85 1 10 0 0.65 1.40 -2 -10 0 -2.33 1.56 -2 -10 0 2.01 1.94 2 10 0 -0.94 1.62 2 10 0 1.20 1.45 -3 -10 0 2.34 2.08 -3 -10 0 3.48 2.33 3 10 0 2.83 1.83 3 10 0 4.45 2.11 -4 -10 0 0.63 2.24 4 10 0 -0.65 1.80 4 10 0 2.39 1.95 -5 -10 0 14.63 3.69 5 10 0 10.00 2.98 5 10 0 10.33 3.11 -6 -10 0 21.40 4.32 6 10 0 27.78 4.23 6 10 0 25.59 4.48 -7 -10 0 9.94 3.49 7 10 0 3.09 2.96 -8 -10 0 6.07 3.42 8 10 0 0.95 3.18 9 -11 0 4.78 3.45 8 -11 0 0.65 3.03 -8 11 0 10.53 3.20 7 -11 0 -0.36 2.52 -7 11 0 -1.46 2.06 -7 11 0 -2.56 2.08 6 -11 0 -2.24 2.15 -6 11 0 2.49 2.27 -6 11 0 2.98 2.39 5 -11 0 -0.23 2.31 -5 11 0 -2.19 1.75 -5 11 0 0.73 2.02 4 -11 0 4.31 2.62 -4 11 0 4.36 2.39 -4 11 0 3.99 2.30 -4 11 0 4.10 2.30 3 -11 0 65.11 5.81 3 -11 0 68.63 6.81 -3 11 0 77.82 5.60 2 -11 0 32.72 4.66 2 -11 0 33.83 4.09 -2 11 0 37.80 4.43 1 -11 0 23.29 3.91 1 -11 0 15.96 3.06 -1 11 0 15.59 3.04 0 -11 0 0.47 1.95 0 -11 0 0.77 1.89 0 11 0 0.33 1.79 -1 -11 0 -0.47 1.90 -1 -11 0 4.30 2.14 1 11 0 -0.28 1.52 -2 -11 0 2.61 2.25 -2 -11 0 6.80 2.62 2 11 0 4.96 2.41 -3 -11 0 3.77 2.27 -3 -11 0 -0.75 2.13 3 11 0 0.81 1.82 3 11 0 1.91 2.17 -4 -11 0 2.00 2.41 4 11 0 3.98 2.50 4 11 0 0.94 2.28 -5 -11 0 8.96 3.31 5 11 0 7.70 2.91 5 11 0 9.14 3.15 -6 -11 0 5.27 3.14 6 11 0 10.37 3.56 6 11 0 7.79 3.27 -7 -11 0 9.53 4.01 7 11 0 6.07 3.55 -8 -11 0 6.55 3.86 8 11 0 6.72 3.76 8 -12 0 -4.47 2.68 -8 12 0 0.79 2.83 7 -12 0 11.20 3.82 -7 12 0 5.60 2.82 6 -12 0 5.80 3.27 -6 12 0 6.85 2.71 5 -12 0 10.72 3.62 -5 12 0 10.14 3.05 -5 12 0 10.30 3.01 4 -12 0 7.35 3.05 -4 12 0 6.19 2.55 -4 12 0 5.39 2.73 -4 12 0 9.00 2.80 3 -12 0 11.45 3.41 3 -12 0 4.19 2.58 -3 12 0 10.01 3.06 2 -12 0 32.76 4.27 2 -12 0 44.76 5.57 -2 12 0 30.16 4.26 1 -12 0 13.78 3.52 1 -12 0 12.39 3.02 -1 12 0 15.82 3.45 0 -12 0 6.40 2.40 0 -12 0 2.84 2.53 0 12 0 2.82 2.24 -1 -12 0 -0.98 2.04 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3.70 7 -14 0 14.76 4.52 -7 14 0 5.16 3.49 6 -14 0 8.27 3.97 -6 14 0 5.57 3.24 5 -14 0 7.51 3.68 -5 14 0 5.86 3.09 4 -14 0 5.27 3.23 -4 14 0 3.75 2.68 3 -14 0 20.70 4.68 -3 14 0 21.29 4.13 2 -14 0 30.55 5.34 2 -14 0 30.36 4.70 -2 14 0 28.15 4.64 1 -14 0 6.90 3.32 1 -14 0 1.02 2.58 -1 14 0 0.60 2.04 0 -14 0 -0.61 2.57 0 -14 0 1.78 2.43 0 14 0 0.90 2.41 -1 -14 0 5.08 3.19 -1 -14 0 5.31 3.16 1 14 0 8.53 3.29 -2 -14 0 2.51 2.80 2 14 0 -0.51 2.36 -3 -14 0 33.35 5.47 3 14 0 33.44 5.10 -4 -14 0 10.39 3.86 4 14 0 11.62 3.76 -5 -14 0 12.90 4.30 5 14 0 6.08 3.62 -6 -14 0 25.19 5.47 6 -15 0 3.82 3.52 -6 15 0 -3.52 2.57 5 -15 0 3.97 3.35 -5 15 0 5.14 3.11 4 -15 0 14.93 4.20 -4 15 0 19.12 4.43 3 -15 0 13.62 4.43 -3 15 0 21.04 4.32 2 -15 0 10.05 3.83 -2 15 0 9.00 3.34 1 -15 0 9.20 3.93 1 -15 0 18.21 4.07 -1 15 0 18.93 4.07 0 -15 0 8.06 3.80 0 -15 0 14.31 3.79 0 15 0 14.37 3.82 -1 -15 0 4.98 3.19 -1 -15 0 4.51 3.17 1 15 0 3.35 3.26 -2 -15 0 1.50 3.10 2 15 0 4.74 2.98 -3 -15 0 3.30 3.58 3 15 0 4.37 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41.55 4.03 4 1 -4 40.39 2.14 -4 -1 4 47.88 3.07 -4 -1 4 49.27 3.12 3 1 -4 70.27 4.08 3 1 -4 68.45 2.80 -3 -1 4 67.35 3.37 -3 -1 4 70.25 3.63 2 1 -4 61.39 3.62 2 1 -4 63.95 2.75 -2 -1 4 64.43 2.96 -2 -1 4 67.17 3.31 1 1 -4 0.73 0.83 -1 -1 4 -0.36 0.85 -1 -1 4 0.25 0.87 -1 -1 4 1.84 0.90 0 -1 4 8.56 1.20 0 -1 4 13.46 1.55 0 -1 4 11.74 1.51 0 -1 4 10.51 1.54 -1 1 -4 170.84 5.97 1 -1 4 171.59 6.32 1 -1 4 162.99 5.95 1 -1 4 165.53 4.95 -2 1 -4 18.69 2.17 2 -1 4 15.18 2.03 2 -1 4 16.63 2.17 -3 1 -4 30.95 3.06 3 -1 4 26.32 2.80 3 -1 4 28.95 2.89 -4 1 -4 14.94 2.50 4 -1 4 22.63 2.81 4 -1 4 27.44 3.19 -5 1 -4 9.10 2.32 5 -1 4 7.00 2.06 5 -1 4 13.10 2.41 -6 1 -4 1.03 1.88 6 -1 4 4.19 1.88 6 -1 4 4.82 2.14 -7 1 -4 3.19 2.24 7 -1 4 1.98 1.97 7 -1 4 -0.50 1.62 -8 1 -4 24.70 4.32 8 -1 4 20.75 4.04 8 -1 4 7.25 2.75 -9 1 -4 1.04 2.71 9 -1 4 -1.30 2.53 -10 1 -4 23.73 5.33 10 -1 4 18.30 5.16 11 0 -4 17.11 4.81 -11 0 4 12.69 4.00 10 0 -4 -3.18 2.38 -10 0 4 -1.79 2.34 9 0 -4 11.56 3.56 -9 0 4 7.76 3.07 -9 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1 -19 -4.07 3.02 1 -1 19 0.23 2.94 4 0 -19 17.51 5.07 -4 0 19 24.97 5.06 3 0 -19 0.89 3.50 -3 0 19 1.33 2.99 2 0 -19 1.49 3.73 -2 0 19 -1.70 2.25 1 0 -19 -2.90 3.24 -1 0 19 -0.82 2.86 0 0 -19 2.91 3.68 0 0 19 -2.37 2.58 3 -1 -19 6.07 3.84 -3 1 19 0.72 2.87 2 -1 -19 -0.09 3.34 -2 1 19 4.80 3.40 1 -1 -19 1.55 3.52 -1 1 19 2.57 3.08 0 -1 -19 4.29 3.93 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 14055 _symmetry_cell_setting triclinic _symmetry_space_group_name_h-m 'P -1' _symmetry_int_tables_number 2 _chemical_absolute_configuration ? #===END _database_code_depnum_ccdc_archive 'CCDC 969313'