data_publication_text _publ_contact_author_name 'Jeffrey R. Long' _publ_contact_author_address ;Department of Chemistry University of California, Berkeley USA ; _publ_contact_author_email jrlong@berkeley.edu _publ_contact_author_phone 510-642-0860 loop_ _publ_author_name _publ_author_address 'Siegelman, Rebecca L.' ;Department of Chemistry University of California, Berkeley USA ; 'McDonald, Thomas M.' ;Department of Chemistry University of California, Berkeley USA ; 'Gonzalez, Miguel I.' ;Department of Chemistry University of California, Berkeley USA ; 'Martell, Jeffrey D.' ;Department of Chemistry University of California, Berkeley USA ; 'Milner, Phillip J.' ;Department of Chemistry University of California, Berkeley USA ; 'Berger, Adam H.' ;Department of Chemistry University of California, Berkeley USA ; 'Bhown, Abhoyjit S.' ;Department of Chemistry University of California, Berkeley USA ; 'Long, Jeffrey R.' ;Department of Chemistry University of California, Berkeley USA ; data_rls045s _audit_creation_date 2017-02-23 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292) ; _shelx_SHELXL_version_number 2016/6 _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _publ_section_acknowledgements ; The Advanced Light Source is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231. ; _chemical_name_common Zn2(dobpdc)(m-2-m)1.43 _chemical_name_systematic ? _chemical_formula_moiety 'C19.72 H23.16 N2.86 O6 Zn2' _chemical_formula_sum 'C19.72 H23.16 N2.86 O6 Zn2' _chemical_formula_weight 527.02 _chemical_absolute_configuration ? _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0060 0.0030 'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13' H H 0.0000 0.0000 'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13' N N 0.0100 0.0050 'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13' O O 0.0180 0.0100 'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13' Zn Zn 0.0350 2.0980 'ANOMDisVal Program in PLATON Spek, A. L. J. Appl. Crystallogr. 2003, 36, 7-13' _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. ; _space_group_crystal_system trigonal _space_group_IT_number 154 _space_group_name_H-M_alt 'P 32 2 1' _space_group_name_Hall 'P 32 2"' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z+2/3' '-x+y, -x, z+1/3' 'y, x, -z' 'x-y, -y, -z+1/3' '-x, -x+y, -z+2/3' _cell_length_a 21.3911(9) _cell_length_b 21.3911(9) _cell_length_c 6.8959(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 2732.7(3) _cell_formula_units_Z 3 _cell_measurement_reflns_used 9793 _cell_measurement_temperature 100 _cell_measurement_theta_max 39.19 _cell_measurement_theta_min 2.74 _shelx_estimated_absorpt_T_max 0.950 _shelx_estimated_absorpt_T_min 0.903 _exptl_absorpt_coefficient_mu 2.420 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014) was used for absorption correction. wR2(int) was 0.0716 before and 0.0467 after correction. The Ratio of minimum to maximum transmission is 0.9338. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'pale yellow' _exptl_crystal_colour_primary 'pale yellow' _exptl_crystal_density_diffrn 0.977 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 824 _exptl_crystal_size_max 0.04284 _exptl_crystal_size_mid 0.02142 _exptl_crystal_size_min 0.02142 _exptl_special_details ; X-ray diffraction analyses were performed on single crystals coated with Paratone-N oil and mounted on MiTeGen loops. Crystals were frozen at a temperature of 100 K by an Oxford Cryosystems Cyrostream using N2 during the experiments. Data was collected at Beamline 11.3.1 at the Advanced Light Source, Lawrence Berkeley National Laboratory using synchrotron radiation (lamda = 0.8856 angstrom) and a Bruker D8 Diffractometer with a Bruker PHOTON100 CMOS detector. ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0338 _diffrn_reflns_av_unetI/netI 0.0246 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_number 40483 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 32.097 _diffrn_reflns_theta_max 39.254 _diffrn_reflns_theta_min 2.373 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 with PHOTON100 CMOS detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_radiation_monochromator 'silicon 111' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.8856 _diffrn_source 'Advanced Light Source station 11.3.1' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.868 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 5249 _reflns_number_total 5556 _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.804 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.116 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.479(17) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 203 _refine_ls_number_reflns 5556 _refine_ls_number_restraints 157 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.0463 _refine_ls_restrained_S_all 1.150 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+2.9560P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1340 _refine_ls_wR_factor_ref 0.1362 _refine_special_details ; Refined as a 2-component inversion twin. Thermal parameters were refined anisotropically for all non-hydrogen atoms. All hydrogen atoms were placed in ideal positions and refined using a riding model. The structure shows N1,N2-dimethylethane-1,2-diamine coordinated to Zn centers of a metal-organic framework. The diamine was found to be disordered over two positions from the nitrogen bound to Zn (N1), requiring distance (SADI for C-C and C-N bonds) and displacement parameter (SIMU and RIGU) restraints. Refinement of the chemical occupancy of each of the disordered positions resulted in occupancies of 37.4(1.3)% and 33.9(1.3), which were fixed in the final refinement. The overall diamine occupancy is 71.3%; however, the occupancy of the nitrogen bound to Zn (N1) was kept at full occupancy to account for solvent or water that is bound on sites where the diamine is absent. The reported formula, however, reflects the nitrogen content for the diamine alone. ; _vrf_PLAT602_rls045s ; PROBLEM: VERY LARGE Solvent Accessible VOID(S) in Structure ! Info RESPONSE: The structure is of a metal-organic framework with a diamine coordinated to metel centers within the pores. Depite the coordination of the diamine, there is still a considerable amount of accesible pore space that is likely filled with highly disordered solvent that could not be modeled. ; _vrf_PLAT043_rls045s ; PROBLEM: Calculated and Reported Mol. Weight Differ by .. 4.57 Check RESPONSE: Refinement of the occupancies of the two disordered diamine positions gave an overall occupancy of 71.3% for the diamine. In the absence of the diamine, solvent or water is likely bound to the Zn centers that line the framework pores. The occupancy of the metal-bound nitrogen atom (N1) was kept at 100% to account for this, but only the diamine was reported in the formula resulting in the difference in the calculated and reported molecular weight. ; _vrf_PLAT049_rls045s ; PROBLEM: Calculated Density less than 1.0 gcm-3 ......... 0.9774 Check RESPONSE: The structure is of a metal-organic framework with a diamine coordinated to metel centers within the pores. Depite the coordination of the diamine, there is still a considerable amount of accesible pore space that is likely filled with highly disordered solvent that could not be modeled. The lack of solvent in the refinement leads to the to the unusually low density. ; _vrf_PLAT220_rls045s ; PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 7.9 Ratio RESPONSE: The substantial disorder of the diamine bound to the Zn centers of the framework results in large ratios in the anisotropic displacement parameters of their constituent atoms. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.521(17) 0.479(17) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H,H) groups, All N(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances N1-C9B \\sim N1-C8A \\sim N1-C9A \\sim N1-C8B with sigma of 0.02 C9A-C10A \\sim C10B-C9B with sigma of 0.02 N2B-C10B \\sim N2A-C10A \\sim N2A-C11A \\sim N2B-C11B with sigma of 0.02 C11B-N2B \\sim C11A-N2A with sigma of 0.02 4. Uiso/Uaniso restraints and constraints N1 \\sim N2A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim N2B \\sim C8B \\sim C9B \\sim C10B \\sim C11B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 5. Rigid body (RIGU) restrains N1, N2A, C8A, C9A, C10A, C11A, N2B, C8B, C9B, C10B, C11B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others Fixed Sof: H1A(0.339) H1B(0.374) N2B(0.339) H2BA(0.339) H2BB(0.339) C8B(0.339) H8BA(0.339) H8BB(0.339) H8BC(0.339) C9B(0.339) H9BA(0.339) H9BB(0.339) C10B(0.339) H10A(0.339) H10B(0.339) C11B(0.339) H11A(0.1695) H11B(0.1695) H11C(0.1695) H11D(0.1695) H11E(0.1695) H11F(0.1695) N2A(0.374) H2AA(0.374) H2AB(0.374) C8A(0.374) H8AA(0.374) H8AB(0.374) H8AC(0.374) C9A(0.374) H9AA(0.374) H9AB(0.374) C10A(0.374) H10C(0.374) H10D(0.374) C11A(0.374) H11G(0.374) H11H(0.374) H11I(0.374) 7.a Ternary CH refined with riding coordinates: N1(H1A), N1(H1B) 7.b Secondary CH2 refined with riding coordinates: N2B(H2BA,H2BB), C9B(H9BA,H9BB), C10B(H10A,H10B), N2A(H2AA,H2AB), C9A(H9AA, H9AB), C10A(H10C,H10D) 7.c Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C6(H6) 7.d Disordered Me refined with riding coordinates: C11B(H11A,H11B,H11C,H11D,H11E,H11F) 7.e Idealised Me refined as rotating group: C8B(H8BA,H8BB,H8BC), C8A(H8AA,H8AB,H8AC), C11A(H11G,H11H,H11I) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary 'intrinsic phasing' _atom_sites_solution_secondary difmap 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 Zn1 Zn 0.66179(2) 0.38905(2) 0.97428(6) 0.01459(13) Uani 1 1 d . . . . . O1 O 0.57641(17) 0.33307(17) 0.7863(4) 0.0173(6) Uani 1 1 d . . . . . O2 O 0.64021(17) 0.35377(16) 0.4274(4) 0.0153(5) Uani 1 1 d . . . . . O3 O 0.6023(2) 0.3977(2) 0.1926(4) 0.0229(7) Uani 1 1 d . . . . . N1 N 0.6869(3) 0.4948(3) 0.8790(7) 0.0384(11) Uani 1 1 d D U . . . H1A H 0.638008 0.489307 0.860431 0.046 Uiso 0.339 1 calc R . P A -2 H1B H 0.638585 0.491461 0.873051 0.046 Uiso 0.374 1 calc R . P B -1 C1 C 0.5413(2) 0.3620(3) 0.7003(6) 0.0179(8) Uani 1 1 d . . . . . C2 C 0.5478(2) 0.3819(2) 0.5003(6) 0.0178(8) Uani 1 1 d . . . . . C3 C 0.5080(3) 0.4120(3) 0.4275(6) 0.0199(8) Uani 1 1 d . . . . . H3 H 0.512288 0.424022 0.293616 0.024 Uiso 1 1 calc R . . . . C4 C 0.4623(3) 0.4254(3) 0.5412(6) 0.0218(8) Uani 1 1 d . . . . . C5 C 0.4549(3) 0.4044(3) 0.7374(6) 0.0242(10) Uani 1 1 d . . . . . H5 H 0.422988 0.411375 0.818448 0.029 Uiso 1 1 calc R . . . . C6 C 0.4930(3) 0.3739(3) 0.8137(6) 0.0220(9) Uani 1 1 d . . . . . H6 H 0.486653 0.360455 0.946614 0.026 Uiso 1 1 calc R . . . . C7 C 0.6003(2) 0.3770(2) 0.3638(6) 0.0159(7) Uani 1 1 d . . . . . N2B N 0.6364(17) 0.5998(19) 0.868(5) 0.107(6) Uani 0.339 1 d D U P C -2 H2BA H 0.649706 0.639842 0.795034 0.128 Uiso 0.339 1 calc R . P C -2 H2BB H 0.626447 0.562896 0.785242 0.128 Uiso 0.339 1 calc R . P C -2 C8B C 0.719(3) 0.516(2) 0.688(4) 0.025(4) Uani 0.339 1 d D U P D -2 H8BA H 0.770723 0.533925 0.696062 0.037 Uiso 0.339 1 calc GR . P D -2 H8BB H 0.710748 0.554364 0.637496 0.037 Uiso 0.339 1 calc GR . P D -2 H8BC H 0.696357 0.474371 0.600510 0.037 Uiso 0.339 1 calc GR . P D -2 C9B C 0.719(4) 0.551(3) 1.029(8) 0.061(6) Uani 0.339 1 d D U P C -2 H9BA H 0.772041 0.570732 1.032296 0.073 Uiso 0.339 1 calc R . P C -2 H9BB H 0.699605 0.529553 1.157663 0.073 Uiso 0.339 1 calc R . P C -2 C10B C 0.7046(18) 0.6137(15) 0.995(5) 0.081(5) Uani 0.339 1 d D U P C -2 H10A H 0.748059 0.653363 0.932659 0.097 Uiso 0.339 1 calc R . P C -2 H10B H 0.699825 0.631467 1.123537 0.097 Uiso 0.339 1 calc R . P C -2 C11B C 0.564(2) 0.581(3) 0.977(8) 0.126(14) Uani 0.339 1 d D U P C -2 H11A H 0.526836 0.574040 0.881180 0.151 Uiso 0.1695 1 calc R . P C -2 H11B H 0.546945 0.536863 1.052853 0.151 Uiso 0.1695 1 calc R . P C -2 H11C H 0.572376 0.620993 1.063560 0.151 Uiso 0.1695 1 calc R . P C -2 H11D H 0.570602 0.580557 1.117215 0.151 Uiso 0.1695 1 calc R . P C -2 H11E H 0.550493 0.617735 0.945542 0.151 Uiso 0.1695 1 calc R . P C -2 H11F H 0.525062 0.533605 0.934835 0.151 Uiso 0.1695 1 calc R . P C -2 N2A N 0.6301(13) 0.5704(12) 0.642(3) 0.077(4) Uani 0.374 1 d D U P D -1 H2AA H 0.616192 0.562195 0.768692 0.093 Uiso 0.374 1 calc R . P D -1 H2AB H 0.600296 0.530199 0.572652 0.093 Uiso 0.374 1 calc R . P D -1 C8A C 0.726(3) 0.5495(19) 1.034(6) 0.048(5) Uani 0.374 1 d D U P D -1 H8AA H 0.697074 0.534252 1.153779 0.072 Uiso 0.374 1 calc GR . P D -1 H8AB H 0.732155 0.596289 0.992773 0.072 Uiso 0.374 1 calc GR . P D -1 H8AC H 0.772794 0.553954 1.057307 0.072 Uiso 0.374 1 calc GR . P D -1 C9A C 0.718(4) 0.524(3) 0.691(5) 0.039(5) Uani 0.374 1 d D U P D -1 H9AA H 0.695673 0.484803 0.593701 0.047 Uiso 0.374 1 calc R . P D -1 H9AB H 0.770315 0.539789 0.695751 0.047 Uiso 0.374 1 calc R . P D -1 C10A C 0.7098(13) 0.5876(11) 0.622(3) 0.059(4) Uani 0.374 1 d D U P D -1 H10C H 0.725043 0.598355 0.485102 0.071 Uiso 0.374 1 calc R . P D -1 H10D H 0.741656 0.630854 0.700352 0.071 Uiso 0.374 1 calc R . P D -1 C11A C 0.626(2) 0.6366(17) 0.564(5) 0.099(9) Uani 0.374 1 d D U P D -1 H11G H 0.660057 0.659302 0.457703 0.149 Uiso 0.374 1 calc GR . P D -1 H11H H 0.637069 0.671687 0.668787 0.149 Uiso 0.374 1 calc GR . P D -1 H11I H 0.576562 0.620347 0.516614 0.149 Uiso 0.374 1 calc GR . P D -1 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 Zn1 0.0168(2) 0.0192(2) 0.00905(19) 0.00010(15) 0.00125(16) 0.00989(19) O1 0.0206(14) 0.0253(16) 0.0109(12) 0.0001(11) -0.0016(10) 0.0152(13) O2 0.0188(14) 0.0206(13) 0.0118(12) 0.0000(10) 0.0015(11) 0.0138(12) O3 0.0333(18) 0.0360(19) 0.0099(13) 0.0059(12) 0.0062(12) 0.0254(16) N1 0.053(3) 0.027(2) 0.034(2) 0.0073(18) -0.003(2) 0.019(2) C1 0.022(2) 0.026(2) 0.0112(16) 0.0015(15) 0.0020(14) 0.0167(18) C2 0.026(2) 0.026(2) 0.0099(16) -0.0003(14) 0.0006(14) 0.0186(18) C3 0.030(2) 0.028(2) 0.0096(16) 0.0023(15) 0.0008(15) 0.0209(19) C4 0.035(2) 0.032(2) 0.0111(16) 0.0000(16) -0.0011(17) 0.026(2) C5 0.036(3) 0.042(3) 0.0089(17) 0.0017(17) 0.0037(16) 0.031(2) C6 0.029(2) 0.039(3) 0.0089(16) 0.0012(16) 0.0033(15) 0.025(2) C7 0.0204(18) 0.0176(17) 0.0124(17) 0.0012(14) 0.0031(14) 0.0116(16) N2B 0.111(11) 0.073(10) 0.105(11) 0.000(9) -0.003(9) 0.021(9) C8B 0.040(8) 0.009(8) 0.020(6) 0.007(5) -0.001(6) 0.008(7) C9B 0.089(10) 0.033(8) 0.048(8) -0.008(7) 0.015(8) 0.020(7) C10B 0.106(11) 0.040(7) 0.084(10) -0.008(8) 0.010(9) 0.027(8) C11B 0.114(17) 0.14(2) 0.09(2) -0.01(2) -0.018(16) 0.041(19) N2A 0.088(9) 0.055(8) 0.091(10) 0.015(7) -0.012(8) 0.037(7) C8A 0.094(13) 0.019(6) 0.029(6) -0.001(5) 0.009(8) 0.027(7) C9A 0.057(8) 0.026(9) 0.028(6) 0.008(6) 0.001(6) 0.015(7) C10A 0.072(8) 0.036(7) 0.059(8) 0.019(6) -0.008(7) 0.019(6) C11A 0.120(19) 0.084(15) 0.12(2) 0.037(14) 0.025(17) 0.068(14) _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 Zn1 O1 2.042(3) 3_665 ? Zn1 O1 2.065(3) . ? Zn1 O2 2.116(3) 3_665 ? Zn1 O2 2.209(3) 2_655 ? Zn1 O3 2.039(3) 1_556 ? Zn1 N1 2.149(5) . ? O1 C1 1.329(5) . ? O2 C7 1.262(5) . ? O3 C7 1.254(5) . ? N1 H1A 1.0000 . ? N1 H1B 1.0000 . ? N1 C8B 1.450(16) . ? N1 C9B 1.478(19) . ? N1 C8A 1.493(16) . ? N1 C9A 1.450(17) . ? C1 C2 1.429(6) . ? C1 C6 1.416(6) . ? C2 C3 1.395(6) . ? C2 C7 1.508(6) . ? C3 H3 0.9500 . ? C3 C4 1.389(6) . ? C4 C4 1.483(8) 4_556 ? C4 C5 1.409(5) . ? C5 H5 0.9500 . ? C5 C6 1.377(6) . ? C6 H6 0.9500 . ? N2B H2BA 0.9100 . ? N2B H2BB 0.9100 . ? N2B C10B 1.59(3) . ? N2B C11B 1.59(3) . ? C8B H8BA 0.9800 . ? C8B H8BB 0.9800 . ? C8B H8BC 0.9800 . ? C9B H9BA 0.9900 . ? C9B H9BB 0.9900 . ? C9B C10B 1.53(5) . ? C10B H10A 0.9900 . ? C10B H10B 0.9900 . ? C11B H11A 0.9800 . ? C11B H11B 0.9800 . ? C11B H11C 0.9800 . ? C11B H11D 0.9800 . ? C11B H11E 0.9800 . ? C11B H11F 0.9800 . ? N2A H2AA 0.9100 . ? N2A H2AB 0.9100 . ? N2A C10A 1.56(3) . ? N2A C11A 1.56(3) . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C9A H9AA 0.9900 . ? C9A H9AB 0.9900 . ? C9A C10A 1.53(4) . ? C10A H10C 0.9900 . ? C10A H10D 0.9900 . ? C11A H11G 0.9800 . ? C11A H11H 0.9800 . ? C11A H11I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O1 161.61(12) 3_665 . ? O1 Zn1 O2 78.74(12) 3_665 2_655 ? O1 Zn1 O2 80.41(11) . 3_665 ? O1 Zn1 O2 90.48(11) . 2_655 ? O1 Zn1 O2 82.89(11) 3_665 3_665 ? O1 Zn1 N1 95.12(18) 3_665 . ? O1 Zn1 N1 95.82(17) . . ? O2 Zn1 O2 78.90(3) 3_665 2_655 ? O2 Zn1 N1 101.91(17) 3_665 . ? O3 Zn1 O1 96.03(14) 1_556 . ? O3 Zn1 O1 99.05(13) 1_556 3_665 ? O3 Zn1 O2 169.54(14) 1_556 3_665 ? O3 Zn1 O2 91.35(13) 1_556 2_655 ? O3 Zn1 N1 88.20(18) 1_556 . ? N1 Zn1 O2 173.70(17) . 2_655 ? Zn1 O1 Zn1 100.37(14) 2_654 . ? C1 O1 Zn1 123.5(3) . . ? C1 O1 Zn1 122.9(3) . 2_654 ? Zn1 O2 Zn1 93.63(11) 2_654 3_664 ? C7 O2 Zn1 125.7(3) . 2_654 ? C7 O2 Zn1 135.8(3) . 3_664 ? C7 O3 Zn1 125.1(3) . 1_554 ? Zn1 N1 H1A 102.7 . . ? Zn1 N1 H1B 103.5 . . ? C8B N1 Zn1 116.1(14) . . ? C8B N1 H1A 102.7 . . ? C8B N1 C9B 115(4) . . ? C9B N1 Zn1 115(2) . . ? C9B N1 H1A 102.7 . . ? C8A N1 Zn1 110.8(15) . . ? C8A N1 H1B 103.5 . . ? C9A N1 Zn1 123.0(18) . . ? C9A N1 H1B 103.5 . . ? C9A N1 C8A 110(4) . . ? O1 C1 C2 125.0(4) . . ? O1 C1 C6 118.1(4) . . ? C6 C1 C2 116.9(4) . . ? C1 C2 C7 123.3(4) . . ? C3 C2 C1 119.5(4) . . ? C3 C2 C7 117.1(4) . . ? C2 C3 H3 118.4 . . ? C4 C3 C2 123.1(4) . . ? C4 C3 H3 118.4 . . ? C3 C4 C4 120.7(4) . 4_556 ? C3 C4 C5 117.1(4) . . ? C5 C4 C4 122.2(4) . 4_556 ? C4 C5 H5 119.4 . . ? C6 C5 C4 121.2(4) . . ? C6 C5 H5 119.4 . . ? C1 C6 H6 119.0 . . ? C5 C6 C1 122.1(4) . . ? C5 C6 H6 119.0 . . ? O2 C7 C2 118.9(4) . . ? O3 C7 O2 123.8(4) . . ? O3 C7 C2 117.3(4) . . ? H2BA N2B H2BB 107.1 . . ? C10B N2B H2BA 107.7 . . ? C10B N2B H2BB 107.7 . . ? C11B N2B H2BA 107.7 . . ? C11B N2B H2BB 107.7 . . ? C11B N2B C10B 119(3) . . ? N1 C8B H8BA 109.5 . . ? N1 C8B H8BB 109.5 . . ? N1 C8B H8BC 109.5 . . ? H8BA C8B H8BB 109.5 . . ? H8BA C8B H8BC 109.5 . . ? H8BB C8B H8BC 109.5 . . ? N1 C9B H9BA 109.0 . . ? N1 C9B H9BB 109.0 . . ? N1 C9B C10B 113(3) . . ? H9BA C9B H9BB 107.8 . . ? C10B C9B H9BA 109.0 . . ? C10B C9B H9BB 109.0 . . ? N2B C10B H10A 107.5 . . ? N2B C10B H10B 107.5 . . ? C9B C10B N2B 119(3) . . ? C9B C10B H10A 107.5 . . ? C9B C10B H10B 107.5 . . ? H10A C10B H10B 107.0 . . ? N2B C11B H11A 109.5 . . ? N2B C11B H11B 109.5 . . ? N2B C11B H11C 109.5 . . ? N2B C11B H11D 109.5 . . ? N2B C11B H11E 109.5 . . ? N2B C11B H11F 109.5 . . ? H11A C11B H11B 109.5 . . ? H11A C11B H11C 109.5 . . ? H11A C11B H11D 141.1 . . ? H11A C11B H11E 56.3 . . ? H11A C11B H11F 56.3 . . ? H11B C11B H11C 109.5 . . ? H11B C11B H11D 56.3 . . ? H11B C11B H11E 141.1 . . ? H11B C11B H11F 56.3 . . ? H11C C11B H11D 56.3 . . ? H11C C11B H11E 56.3 . . ? H11C C11B H11F 141.1 . . ? H11D C11B H11E 109.5 . . ? H11D C11B H11F 109.5 . . ? H11E C11B H11F 109.5 . . ? H2AA N2A H2AB 108.4 . . ? C10A N2A H2AA 110.0 . . ? C10A N2A H2AB 110.0 . . ? C10A N2A C11A 108(2) . . ? C11A N2A H2AA 110.0 . . ? C11A N2A H2AB 110.0 . . ? N1 C8A H8AA 109.5 . . ? N1 C8A H8AB 109.5 . . ? N1 C8A H8AC 109.5 . . ? H8AA C8A H8AB 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? N1 C9A H9AA 108.5 . . ? N1 C9A H9AB 108.5 . . ? N1 C9A C10A 115(3) . . ? H9AA C9A H9AB 107.5 . . ? C10A C9A H9AA 108.5 . . ? C10A C9A H9AB 108.5 . . ? N2A C10A H10C 109.4 . . ? N2A C10A H10D 109.4 . . ? C9A C10A N2A 111(3) . . ? C9A C10A H10C 109.4 . . ? C9A C10A H10D 109.4 . . ? H10C C10A H10D 108.0 . . ? N2A C11A H11G 109.5 . . ? N2A C11A H11H 109.5 . . ? N2A C11A H11I 109.5 . . ? H11G C11A H11H 109.5 . . ? H11G C11A H11I 109.5 . . ? H11H C11A H11I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn1 O1 C1 C2 -27.2(6) 2_654 . . . ? Zn1 O1 C1 C2 106.1(4) . . . . ? Zn1 O1 C1 C6 152.3(4) 2_654 . . . ? Zn1 O1 C1 C6 -74.4(5) . . . . ? Zn1 O2 C7 O3 1.5(7) 3_664 . . . ? Zn1 O2 C7 O3 -146.6(4) 2_654 . . . ? Zn1 O2 C7 C2 34.5(5) 2_654 . . . ? Zn1 O2 C7 C2 -177.3(3) 3_664 . . . ? Zn1 O3 C7 O2 6.6(7) 1_554 . . . ? Zn1 O3 C7 C2 -174.5(3) 1_554 . . . ? Zn1 N1 C9B C10B -153(4) . . . . ? Zn1 N1 C9A C10A 161(3) . . . . ? O1 C1 C2 C3 -179.9(4) . . . . ? O1 C1 C2 C7 -4.5(7) . . . . ? O1 C1 C6 C5 179.3(5) . . . . ? N1 C9B C10B N2B 24(8) . . . . ? N1 C9A C10A N2A -49(5) . . . . ? C1 C2 C3 C4 1.2(8) . . . . ? C1 C2 C7 O2 0.7(7) . . . . ? C1 C2 C7 O3 -178.2(4) . . . . ? C2 C1 C6 C5 -1.2(7) . . . . ? C2 C3 C4 C4 175.6(4) . . . 4_556 ? C2 C3 C4 C5 -2.5(8) . . . . ? C3 C2 C7 O2 176.1(4) . . . . ? C3 C2 C7 O3 -2.8(6) . . . . ? C3 C4 C5 C6 1.9(8) . . . . ? C4 C4 C5 C6 -176.2(4) 4_556 . . . ? C4 C5 C6 C1 -0.1(8) . . . . ? C6 C1 C2 C3 0.7(7) . . . . ? C6 C1 C2 C7 176.0(4) . . . . ? C7 C2 C3 C4 -174.4(5) . . . . ? C8B N1 C9B C10B 68(6) . . . . ? C11B N2B C10B C9B 96(5) . . . . ? C8A N1 C9A C10A -65(5) . . . . ? C11A N2A C10A C9A -178(3) . . . . ? _shelx_res_file ; TITL RLS045S in P3(2)21 rls045s.res created by SHELXL-2016/6 at 18:56:57 on 23-Feb-2017 CELL 0.8856 21.3911 21.3911 6.8959 90 90 120 ZERR 3 0.0009 0.0009 0.0003 0 0 0 LATT -1 SYMM -Y,+X-Y,0.667+Z SYMM +Y-X,-X,0.333+Z SYMM +Y,+X,-Z SYMM -Y+X,-Y,0.333-Z SYMM -X,-X+Y,0.667-Z SFAC C H N O Zn DISP C 0.006 0.003 18.6 DISP H -0 0 0.7 DISP N 0.01 0.005 33.8 DISP O 0.018 0.01 57.9 DISP Zn 0.035 2.098 10597.5 UNIT 59.11 73.61 10.28 18 6 EQIV $1 1-Y,+X-Y,0.667+Z EQIV $2 1-Y,+X-Y,-0.333+Z EQIV $3 1-X,-X+Y,1.667-Z EQIV $4 +X,+Y,1+Z EQIV $5 +X,+Y,-2+Z EQIV $6 1+Y-X,1-X,0.333+Z EQIV $7 1+Y-X,1-X,1.333+Z EQIV $8 +Y,+X,1-Z EQIV $9 -Y+X,1-Y,1.333-Z EQIV $10 1-Y+X,1-Y,0.333-Z SADI N1 C9B N1 C8A N1 C9A N1 C8B SADI C9A C10A C10B C9B SADI N2B C10B N2A C10A N2A C11A N2B C11B SADI C11B N2B C11A N2A SIMU 0.01 0.02 2 N1 N2A > C11A N2B > C11B RIGU N1 N2A C8A C9A C10A C11A N2B C8B C9B C10B C11B L.S. 100 PLAN 20 SIZE 0.02142 0.02142 0.04284 TEMP -173.15 BIND N2B C11B FREE Zn1 Zn1_$2 FREE Zn1 Zn1_$3 FREE Zn1 Zn1_$5 FREE Zn1 Zn1_$1 FREE Zn1 Zn1_$9 FREE Zn1 Zn1_$4 FREE Zn1 Zn1_$8 FREE Zn1 Zn1_$10 FREE Zn1 Zn1_$7 FREE Zn1 Zn1_$6 BOND $H LIST 6 MORE -1 CONF fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 2 0 OMIT -3 6 0 OMIT 3 3 0 OMIT -4 4 1 OMIT 0 2 1 OMIT 5 7 1 OMIT -5 12 1 OMIT 0 6 0 REM REM REM WGHT 0.075800 2.956000 BASF 0.47947 FVAR 0.14050 ZN1 5 0.661792 0.389048 0.974282 11.00000 0.01678 0.01916 = 0.00905 0.00010 0.00125 0.00989 O1 4 0.576412 0.333066 0.786283 11.00000 0.02061 0.02531 = 0.01086 0.00013 -0.00157 0.01523 O2 4 0.640212 0.353765 0.427388 11.00000 0.01883 0.02060 = 0.01184 -0.00004 0.00149 0.01379 O3 4 0.602310 0.397727 0.192593 11.00000 0.03332 0.03602 = 0.00993 0.00591 0.00618 0.02536 N1 3 0.686857 0.494765 0.879041 11.00000 0.05309 0.02702 = 0.03422 0.00732 -0.00330 0.01943 PART -2 AFIX 13 H1A 2 0.638008 0.489307 0.860431 10.33900 -1.20000 AFIX 13 PART 0 PART -1 H1B 2 0.638585 0.491461 0.873051 10.37400 -1.20000 AFIX 0 PART 0 C1 1 0.541257 0.362043 0.700306 11.00000 0.02231 0.02624 = 0.01119 0.00146 0.00196 0.01674 C2 1 0.547836 0.381861 0.500331 11.00000 0.02554 0.02576 = 0.00993 -0.00027 0.00060 0.01860 C3 1 0.507995 0.412025 0.427452 11.00000 0.02986 0.02848 = 0.00961 0.00230 0.00076 0.02088 AFIX 43 H3 2 0.512288 0.424022 0.293616 11.00000 -1.20000 AFIX 0 C4 1 0.462333 0.425366 0.541238 11.00000 0.03522 0.03168 = 0.01113 0.00004 -0.00107 0.02627 C5 1 0.454880 0.404384 0.737352 11.00000 0.03640 0.04221 = 0.00894 0.00170 0.00366 0.03088 AFIX 43 H5 2 0.422988 0.411375 0.818448 11.00000 -1.20000 AFIX 0 C6 1 0.492969 0.373923 0.813693 11.00000 0.02909 0.03905 = 0.00894 0.00117 0.00334 0.02525 AFIX 43 H6 2 0.486653 0.360455 0.946614 11.00000 -1.20000 AFIX 0 C7 1 0.600316 0.377025 0.363767 11.00000 0.02038 0.01765 = 0.01237 0.00119 0.00312 0.01163 PART -2 N2B 3 0.636443 0.599769 0.868408 10.33900 0.11093 0.07275 = 0.10474 -0.00031 -0.00302 0.02145 AFIX 23 H2BA 2 0.649706 0.639842 0.795034 10.33900 -1.20000 H2BB 2 0.626447 0.562896 0.785242 10.33900 -1.20000 AFIX 0 C8B 1 0.718755 0.516083 0.687784 10.33900 0.03987 0.00852 = 0.02034 0.00736 -0.00111 0.00788 AFIX 137 H8BA 2 0.770723 0.533925 0.696062 10.33900 -1.50000 H8BB 2 0.710748 0.554364 0.637496 10.33900 -1.50000 H8BC 2 0.696357 0.474371 0.600510 10.33900 -1.50000 AFIX 0 C9B 1 0.719235 0.551382 1.029441 10.33900 0.08856 0.03276 = 0.04781 -0.00849 0.01474 0.01993 AFIX 23 H9BA 2 0.772041 0.570732 1.032296 10.33900 -1.20000 H9BB 2 0.699605 0.529553 1.157663 10.33900 -1.20000 AFIX 0 C10B 1 0.704619 0.613676 0.994995 10.33900 0.10598 0.04049 = 0.08393 -0.00825 0.00968 0.02701 AFIX 23 H10A 2 0.748059 0.653363 0.932659 10.33900 -1.20000 H10B 2 0.699825 0.631467 1.123537 10.33900 -1.20000 AFIX 0 C11B 1 0.563690 0.581134 0.976877 10.33900 0.11358 0.14350 = 0.08901 -0.00974 -0.01755 0.04144 AFIX 123 H11A 2 0.526836 0.574040 0.881180 10.16950 -1.20000 H11B 2 0.546945 0.536863 1.052853 10.16950 -1.20000 H11C 2 0.572376 0.620993 1.063560 10.16950 -1.20000 H11D 2 0.570602 0.580557 1.117215 10.16950 -1.20000 H11E 2 0.550493 0.617735 0.945542 10.16950 -1.20000 H11F 2 0.525062 0.533605 0.934835 10.16950 -1.20000 AFIX 0 PART 0 PART -1 N2A 3 0.630109 0.570413 0.642197 10.37400 0.08754 0.05510 = 0.09084 0.01487 -0.01173 0.03704 AFIX 23 H2AA 2 0.616192 0.562195 0.768692 10.37400 -1.20000 H2AB 2 0.600296 0.530199 0.572652 10.37400 -1.20000 AFIX 0 C8A 1 0.725545 0.549521 1.034045 10.37400 0.09410 0.01925 = 0.02885 -0.00059 0.00906 0.02733 AFIX 137 H8AA 2 0.697074 0.534252 1.153779 10.37400 -1.50000 H8AB 2 0.732155 0.596289 0.992773 10.37400 -1.50000 H8AC 2 0.772794 0.553954 1.057307 10.37400 -1.50000 AFIX 0 C9A 1 0.718218 0.523938 0.691026 10.37400 0.05657 0.02563 = 0.02769 0.00822 0.00142 0.01504 AFIX 23 H9AA 2 0.695673 0.484803 0.593701 10.37400 -1.20000 H9AB 2 0.770315 0.539789 0.695751 10.37400 -1.20000 AFIX 0 C10A 1 0.709829 0.587551 0.622367 10.37400 0.07175 0.03622 = 0.05881 0.01861 -0.00778 0.01933 AFIX 23 H10C 2 0.725043 0.598355 0.485102 10.37400 -1.20000 H10D 2 0.741656 0.630854 0.700352 10.37400 -1.20000 AFIX 0 C11A 1 0.625521 0.636613 0.564032 10.37400 0.11991 0.08427 = 0.11527 0.03723 0.02455 0.06769 AFIX 137 H11G 2 0.660057 0.659302 0.457703 10.37400 -1.50000 H11H 2 0.637069 0.671687 0.668787 10.37400 -1.50000 H11I 2 0.576562 0.620347 0.516614 10.37400 -1.50000 AFIX 0 HKLF 4 REM RLS045S in P3(2)21 REM R1 = 0.0463 for 5249 Fo > 4sig(Fo) and 0.0497 for all 5556 data REM 203 parameters refined using 157 restraints END WGHT 0.0763 2.9299 REM Highest difference peak 0.804, deepest hole -1.075, 1-sigma level 0.116 Q1 1 0.9122 0.6854 0.7395 11.00000 0.05 0.80 Q2 1 0.6608 0.7005 0.7270 11.00000 0.05 0.73 Q3 1 0.9032 0.6641 0.5320 11.00000 0.05 0.73 Q4 1 0.9421 0.9421 1.0000 10.50000 0.05 0.70 Q5 1 0.7433 0.5227 0.4570 11.00000 0.05 0.58 Q6 1 0.5237 0.3950 0.4685 11.00000 0.05 0.43 Q7 1 0.4896 0.4063 0.7876 11.00000 0.05 0.43 Q8 1 0.6825 0.4283 1.0027 11.00000 0.05 0.39 Q9 1 0.6583 0.5325 0.9574 11.00000 0.05 0.38 Q10 1 0.6985 0.4706 0.8140 11.00000 0.05 0.38 Q11 1 0.8921 0.8927 0.9473 11.00000 0.05 0.38 Q12 1 0.8904 0.7804 0.6144 11.00000 0.05 0.37 Q13 1 0.7014 0.4080 1.0115 11.00000 0.05 0.37 Q14 1 0.9604 0.9288 1.0819 11.00000 0.05 0.37 Q15 1 0.4635 0.3080 0.5942 11.00000 0.05 0.37 Q16 1 0.6016 0.6403 0.9210 11.00000 0.05 0.37 Q17 1 0.5102 0.3610 0.7478 11.00000 0.05 0.37 Q18 1 0.4551 0.4551 0.5000 10.50000 0.05 0.37 Q19 1 0.4966 0.4372 0.4815 11.00000 0.05 0.35 Q20 1 0.4793 0.3704 1.0956 11.00000 0.05 0.35 ; _shelx_res_checksum 97969 _shelx_hkl_file ; -2 1 0 941.65 24.27 1 -2 0 1000.00 24.24 -1 -1 0 954.62 23.95 -2 2 0 106.77 2.62 -2 0 0 109.05 2.64 -2 2 0 103.84 2.64 0 2 0 112.32 2.64 2 -2 0 112.74 2.64 -3 2 0 147.59 3.63 1 -3 0 148.36 3.63 2 -3 0 149.77 3.63 2 1 0 150.16 3.63 -3 1 0 148.98 3.63 1 2 0 155.62 3.63 -2 -1 0 148.09 3.61 0 -3 0 187.97 4.57 0 3 0 193.84 4.60 3 0 0 185.39 4.56 0 3 0 187.65 4.56 2 2 0 151.35 3.74 2 -4 0 152.03 3.74 2 -4 0 155.47 3.72 -4 2 0 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0 14.18 0.61 0 -10 0 13.29 0.71 -10 10 0 13.65 0.51 10 -10 0 12.89 0.69 -10 0 0 12.80 0.64 0 -10 0 14.24 0.72 5 6 0 113.38 2.94 -11 6 0 115.93 2.94 5 6 0 116.81 2.99 5 -11 0 118.92 2.99 5 6 0 113.80 2.90 6 5 0 112.69 2.93 6 -11 0 118.61 3.00 5 -11 0 113.41 2.94 6 5 0 119.10 2.99 6 -11 0 112.82 2.93 6 5 0 114.27 2.98 -11 5 0 113.70 2.94 -6 11 0 113.32 2.89 11 -6 0 113.23 2.92 11 -5 0 112.24 2.92 -5 -6 0 119.27 2.85 -6 11 0 109.32 2.85 -6 -5 0 116.29 2.98 -6 11 0 116.61 2.97 -5 -6 0 114.56 2.99 -5 11 0 109.17 2.83 -5 11 0 116.34 2.95 -5 11 0 113.71 2.98 -6 -5 0 109.89 2.85 4 -11 0 182.18 4.48 7 4 0 174.76 4.37 4 7 0 179.42 4.44 7 4 0 180.17 4.46 -11 7 0 180.18 4.43 7 -11 0 173.83 4.42 4 -11 0 175.88 4.42 4 7 0 176.21 4.39 -11 4 0 181.16 4.31 7 4 0 175.45 4.41 -11 4 0 168.57 4.41 7 -11 0 176.00 4.45 11 -4 0 178.99 4.30 -4 -7 0 180.49 4.49 11 -4 0 175.37 4.41 -4 11 0 172.00 4.30 -4 11 0 183.84 4.50 -4 -7 0 176.91 4.31 -7 -4 0 175.14 4.37 -7 11 0 174.51 4.36 11 -4 0 172.91 4.27 -4 11 0 178.61 4.40 11 -7 0 173.29 4.41 -7 11 0 183.43 4.46 -7 11 0 179.82 4.38 8 3 0 49.96 1.37 8 -11 0 52.09 1.45 3 8 0 50.92 1.51 8 -11 0 46.83 1.44 3 -11 0 50.07 1.47 8 3 0 51.02 1.44 -11 3 0 49.12 1.44 -11 3 0 51.93 1.33 3 8 0 50.88 1.43 8 3 0 51.38 1.46 3 -11 0 50.91 1.52 -11 8 0 50.39 1.46 -8 11 0 52.19 1.38 -3 -8 0 49.68 1.27 -8 -3 0 49.61 1.39 -3 11 0 51.09 1.52 -3 -8 0 51.55 1.52 11 -3 0 49.66 1.28 -8 11 0 50.94 1.45 -3 11 0 51.95 1.28 11 -8 0 51.55 1.29 11 -3 0 47.96 1.40 -8 11 0 50.66 1.39 11 -8 0 51.06 1.45 -3 11 0 50.79 1.43 11 -8 0 50.39 1.30 11 -3 0 51.10 1.32 -8 -3 0 52.30 1.47 2 9 0 33.23 1.14 2 9 0 33.22 1.05 9 2 0 33.45 0.97 -11 2 0 34.64 1.08 9 2 0 33.92 1.06 -11 2 0 35.25 0.97 9 -11 0 33.48 1.03 2 -11 0 30.77 1.12 9 2 0 32.13 1.04 -11 9 0 32.61 1.07 2 -11 0 33.85 1.11 -11 9 0 31.85 0.89 9 -11 0 31.52 1.08 11 -2 0 32.41 0.89 11 -9 0 32.90 1.07 -9 -2 0 33.76 1.06 -2 11 0 34.37 1.06 -9 11 0 33.06 1.05 -9 -2 0 33.19 1.02 -9 11 0 33.84 1.04 11 -2 0 34.63 0.96 -2 -9 0 34.21 1.14 11 -9 0 33.57 0.93 -2 11 0 35.50 1.15 11 -9 0 33.74 0.92 11 -2 0 32.02 1.02 -2 -9 0 33.61 1.08 10 -11 0 34.41 1.09 1 -11 0 33.20 1.07 10 -11 0 32.82 1.01 1 -11 0 33.67 1.14 -11 10 0 32.85 0.92 -11 10 0 35.28 1.09 1 10 0 34.26 1.06 10 1 0 33.76 1.07 -11 1 0 31.84 1.07 10 1 0 33.60 1.04 1 10 0 34.35 1.15 -11 1 0 34.29 1.01 -1 -10 0 33.79 1.16 11 -1 0 33.04 0.92 11 -10 0 31.77 1.06 11 -10 0 32.64 0.96 -1 11 0 33.93 1.06 11 -1 0 33.53 0.99 -10 -1 0 32.01 1.05 -10 -1 0 34.74 1.06 -10 11 0 33.84 1.05 -1 11 0 33.81 1.15 -10 11 0 32.54 0.95 11 -10 0 34.17 0.96 11 -1 0 32.69 1.05 -1 -10 0 33.58 1.10 -10 11 0 32.45 1.03 0 -11 0 15.87 0.80 11 -11 0 16.85 0.63 0 -11 0 16.32 0.73 0 11 0 15.75 0.72 11 -11 0 15.53 0.76 -11 0 0 16.38 0.68 11 0 0 15.10 0.57 11 0 0 16.05 0.73 -11 11 0 15.88 0.73 0 11 0 16.08 0.79 -11 0 0 16.20 0.73 -11 11 0 15.76 0.56 11 0 0 16.35 0.65 6 -12 0 249.55 6.04 6 6 0 242.00 6.03 6 6 0 240.90 6.11 -12 6 0 239.08 6.03 6 6 0 244.69 6.00 6 -12 0 251.33 6.09 12 -6 0 245.10 6.02 -6 -6 0 249.93 6.09 -6 12 0 238.70 5.94 -6 12 0 240.37 6.11 -6 12 0 245.85 5.99 -6 -6 0 242.13 5.95 5 7 0 16.91 0.78 5 -12 0 16.50 0.75 7 5 0 17.54 0.69 7 5 0 18.43 0.79 5 7 0 17.81 0.72 -12 7 0 19.22 0.79 -12 5 0 17.18 0.76 7 -12 0 16.17 0.79 7 5 0 17.40 0.77 5 7 0 18.53 0.80 7 -12 0 17.35 0.75 5 -12 0 18.23 0.80 -7 12 0 17.31 0.63 -7 12 0 17.63 0.77 -7 -5 0 17.18 0.65 12 -7 0 16.50 0.71 -5 12 0 16.07 0.68 12 -5 0 16.28 0.73 -7 12 0 17.84 0.67 -5 -7 0 17.20 0.59 -7 -5 0 17.49 0.78 -5 12 0 17.81 0.81 -5 12 0 17.16 0.57 8 4 0 60.31 1.66 4 -12 0 57.76 1.68 4 -12 0 56.89 1.62 4 8 0 57.56 1.69 8 -12 0 59.10 1.64 -12 4 0 58.02 1.47 8 4 0 58.11 1.62 8 4 0 57.56 1.62 8 -12 0 57.00 1.64 -12 8 0 59.70 1.64 4 8 0 55.86 1.62 4 8 0 57.31 1.60 -12 4 0 57.21 1.63 -8 12 0 57.34 1.56 -4 12 0 58.75 1.69 -8 12 0 57.99 1.56 -8 -4 0 56.25 1.55 12 -4 0 58.73 1.46 12 -8 0 58.20 1.62 -4 -8 0 56.45 1.77 -4 -8 0 57.80 1.46 -8 12 0 57.65 1.65 -4 12 0 54.38 1.45 -4 12 0 57.43 1.59 -8 -4 0 58.72 1.65 12 -4 0 55.81 1.59 12 -4 0 55.49 1.42 9 -12 0 150.72 3.81 9 3 0 150.29 3.79 3 -12 0 154.13 3.87 -12 3 0 150.72 3.70 9 -12 0 149.39 3.80 -12 9 0 146.04 3.79 3 9 0 146.82 3.77 9 3 0 149.17 3.73 3 -12 0 150.68 3.81 -12 3 0 148.38 3.80 3 9 0 148.13 3.87 9 3 0 154.43 3.83 -3 12 0 149.91 3.77 -9 -3 0 148.13 3.76 12 -9 0 147.01 3.67 -9 12 0 149.23 3.81 12 -3 0 151.41 3.69 -3 12 0 150.10 3.87 12 -9 0 152.08 3.67 -9 12 0 147.69 3.75 12 -9 0 149.89 3.80 -3 -9 0 154.30 3.88 -9 -3 0 160.70 3.87 -9 12 0 149.38 3.73 12 -3 0 147.15 3.65 -3 -9 0 145.18 3.79 12 -3 0 147.23 3.77 -12 2 0 22.39 0.73 10 2 0 21.79 0.82 10 -12 0 20.75 0.83 -12 10 0 21.69 0.64 2 -12 0 22.46 0.91 -12 2 0 20.85 0.85 2 10 0 21.22 0.91 -12 10 0 21.85 0.86 10 2 0 21.37 0.73 10 -12 0 21.78 0.79 2 10 0 22.41 0.83 2 -12 0 20.94 0.85 10 2 0 20.65 0.83 12 -10 0 20.83 0.68 12 -2 0 20.69 0.83 -10 12 0 22.32 0.74 -10 12 0 21.91 0.80 12 -2 0 21.01 0.65 -2 12 0 21.31 0.84 -10 -2 0 21.99 0.82 -10 12 0 22.42 0.82 -2 -10 0 21.86 0.87 -2 12 0 21.28 0.91 12 -10 0 20.02 0.81 12 -2 0 21.88 0.71 12 -10 0 21.95 0.68 -2 -10 0 21.73 0.91 -10 -2 0 21.28 0.80 -12 11 0 5.71 0.37 1 -12 0 6.22 0.65 -12 1 0 6.58 0.64 11 -12 0 6.37 0.49 11 1 0 6.07 0.58 1 11 0 5.16 0.64 11 1 0 6.50 0.51 -12 11 0 5.54 0.61 1 -12 0 6.02 0.58 11 -12 0 5.69 0.64 1 11 0 5.00 0.53 -12 1 0 6.33 0.48 11 1 0 5.98 0.42 12 -1 0 6.44 0.45 -11 -1 0 6.86 0.57 12 -1 0 6.22 0.37 -11 -1 0 6.54 0.52 -1 -11 0 6.27 0.65 12 -1 0 5.69 0.57 -1 -11 0 6.39 0.63 12 -11 0 5.19 0.55 12 -11 0 6.13 0.42 -1 12 0 5.88 0.53 -11 12 0 6.24 0.59 -1 12 0 6.12 0.65 12 -11 0 6.08 0.41 0 12 0 -0.12 0.37 -12 0 0 0.02 0.28 12 -12 0 0.57 0.25 12 0 0 0.23 0.26 12 0 0 -0.02 0.35 -12 12 0 -0.31 0.36 12 -12 0 0.22 0.40 0 -12 0 0.64 0.44 12 -12 0 0.21 0.25 12 0 0 0.15 0.27 0 -12 0 0.17 0.38 -12 0 0 0.31 0.35 0 12 0 0.24 0.38 -12 12 0 -0.02 0.20 6 7 0 65.29 1.84 7 6 0 66.69 1.83 7 -13 0 67.11 1.88 -13 6 0 67.42 1.84 6 7 0 68.82 1.89 6 7 0 67.19 1.79 6 -13 0 67.37 1.88 7 6 0 65.51 1.87 -13 7 0 64.57 1.83 7 6 0 67.44 1.78 7 -13 0 64.03 1.82 6 -13 0 63.79 1.83 -6 -7 0 66.79 1.71 13 -7 0 61.79 1.80 13 -6 0 65.31 1.81 -7 13 0 62.86 1.72 -6 13 0 65.43 1.87 -7 -6 0 65.68 1.73 -7 -6 0 60.71 1.89 -7 13 0 67.45 1.77 -7 13 0 65.13 1.87 -6 13 0 66.20 1.78 -6 13 0 63.96 1.70 -6 -7 0 65.84 1.88 8 5 0 136.11 3.45 -13 8 0 132.85 3.50 5 -13 0 136.42 3.57 -13 5 0 136.69 3.52 5 8 0 135.46 3.51 8 5 0 138.83 3.50 8 -13 0 138.60 3.54 5 -13 0 141.89 3.53 8 -13 0 136.04 3.51 5 8 0 141.23 3.52 5 8 0 140.59 3.58 8 5 0 138.94 3.55 -8 13 0 137.55 3.45 -8 13 0 138.73 3.44 -5 -8 0 132.37 3.38 -5 -8 0 135.92 3.57 13 -5 0 136.52 3.49 -8 -5 0 136.47 3.44 -5 13 0 138.05 3.57 13 -8 0 135.81 3.49 -8 -5 0 138.77 3.55 -5 13 0 130.86 3.37 -5 13 0 140.53 3.48 9 4 0 43.35 1.31 -13 4 0 42.69 1.35 -13 9 0 41.97 1.33 9 -13 0 44.44 1.37 4 -13 0 44.72 1.37 4 -13 0 43.60 1.40 4 9 0 44.60 1.40 9 -13 0 43.90 1.34 9 4 0 43.38 1.46 -13 4 0 44.33 1.16 9 4 0 44.11 1.26 4 9 0 45.13 1.31 -9 -4 0 43.27 1.28 -4 -9 0 43.69 1.12 13 -9 0 44.31 1.34 -4 13 0 46.03 1.42 13 -4 0 40.58 1.30 -9 13 0 44.92 1.36 -4 -9 0 44.53 1.40 -4 13 0 43.02 1.30 13 -4 0 42.23 1.11 -9 13 0 43.78 1.26 -9 13 0 43.22 1.27 -4 13 0 43.69 1.14 13 -4 0 44.87 1.15 -9 -4 0 45.37 1.37 10 3 0 24.23 0.90 3 -13 0 24.22 0.96 3 10 0 24.41 0.89 10 3 0 23.46 0.81 10 -13 0 23.81 0.95 10 -13 0 24.20 0.89 -13 10 0 24.08 0.94 3 -13 0 22.77 0.96 10 3 0 23.90 0.90 -13 3 0 24.35 0.75 -13 3 0 23.95 0.95 3 10 0 24.78 1.18 -10 13 0 23.55 0.81 -10 -3 0 23.33 0.86 -10 13 0 23.55 0.90 -10 13 0 22.05 0.85 13 -10 0 22.90 0.69 -3 -10 0 23.79 0.98 13 -3 0 22.39 0.68 -3 13 0 24.84 0.99 13 -3 0 24.04 0.73 -3 -10 0 23.92 0.92 -10 -3 0 23.90 0.90 13 -10 0 23.60 0.69 13 -3 0 24.25 0.89 13 -10 0 23.47 0.92 -3 13 0 23.19 0.89 11 2 0 15.96 0.78 2 11 0 16.80 0.73 2 11 0 16.94 0.85 2 -13 0 16.92 0.84 -13 11 0 17.23 0.80 11 -13 0 15.95 0.82 11 2 0 17.47 0.66 -13 2 0 17.19 0.66 2 -13 0 17.15 0.84 11 -13 0 17.30 0.72 -13 2 0 18.31 0.84 11 2 0 17.77 0.74 -13 11 0 17.30 0.56 -2 -11 0 17.04 0.82 -11 13 0 16.60 0.67 -11 13 0 17.08 0.76 13 -11 0 17.48 0.81 13 -11 0 16.40 0.60 -2 13 0 16.91 0.85 -11 13 0 15.39 0.88 13 -2 0 16.81 0.57 13 -11 0 17.17 0.60 -2 13 0 16.28 0.76 -11 -2 0 17.01 0.81 -11 -2 0 17.43 0.77 13 -2 0 17.43 0.63 -2 -11 0 17.10 0.85 13 -2 0 17.27 0.77 -13 1 0 5.42 0.66 -13 12 0 5.58 0.41 1 -13 0 6.62 0.62 -13 1 0 5.40 0.50 1 12 0 6.55 0.62 12 1 0 5.99 0.45 1 -13 0 5.46 0.65 -13 12 0 6.32 0.67 12 1 0 6.24 0.53 1 12 0 5.64 0.65 12 -13 0 5.55 0.61 12 1 0 4.85 0.62 12 -13 0 5.87 0.49 -12 13 0 5.68 0.63 13 -12 0 6.51 0.60 -1 13 0 5.44 0.65 13 -1 0 5.60 0.46 -1 -12 0 5.00 0.65 -1 -12 0 5.52 0.68 -1 13 0 6.14 0.61 -12 -1 0 5.25 0.62 -12 -1 0 5.51 0.54 -12 13 0 5.94 0.49 13 -12 0 5.89 0.45 13 -12 0 5.62 0.43 13 -1 0 5.18 0.40 13 -1 0 4.60 0.59 -13 0 0 31.47 1.10 0 13 0 29.14 1.04 -13 13 0 30.90 1.10 13 -13 0 31.58 1.00 13 -13 0 32.12 1.13 -13 13 0 28.43 1.08 0 -13 0 31.99 1.09 13 -13 0 30.87 0.99 13 0 0 31.27 1.07 13 0 0 31.39 0.94 13 0 0 32.06 1.02 0 -13 0 29.27 1.16 -13 0 0 31.46 1.04 0 13 0 30.44 1.16 7 -14 0 183.76 4.59 7 -14 0 183.13 4.63 7 7 0 183.26 4.54 7 7 0 182.88 4.58 -14 7 0 186.05 4.59 7 7 0 185.02 4.64 -7 -7 0 179.09 4.63 14 -7 0 173.88 4.55 -7 14 0 180.71 4.64 -7 14 0 178.17 4.48 -7 -7 0 179.95 4.49 -7 14 0 182.81 4.53 6 8 0 44.49 1.39 6 -14 0 44.61 1.41 8 6 0 45.13 1.41 6 -14 0 44.13 1.41 6 8 0 45.19 1.43 8 6 0 44.49 1.32 6 8 0 44.86 1.33 8 -14 0 44.08 1.40 8 -14 0 44.52 1.39 -14 8 0 46.50 1.41 8 6 0 44.31 1.38 -14 6 0 45.04 1.37 -8 14 0 43.82 1.26 -6 -8 0 45.06 1.43 -8 -6 0 45.21 1.28 -6 14 0 45.14 1.43 -8 14 0 45.48 1.32 14 -6 0 40.88 1.31 -8 -6 0 44.88 1.41 -6 14 0 44.85 1.33 14 -8 0 43.87 1.35 -6 14 0 42.52 1.21 -6 -8 0 42.46 1.22 -8 14 0 43.44 1.40 5 9 0 32.66 1.09 5 9 0 33.34 1.16 9 5 0 36.13 1.16 5 -14 0 33.64 1.17 9 -14 0 32.89 1.18 -14 5 0 33.07 1.18 5 9 0 32.51 1.20 9 5 0 33.46 1.08 -14 9 0 34.25 1.18 9 5 0 33.66 1.17 5 -14 0 34.31 1.19 -5 14 0 34.33 1.11 -5 14 0 34.87 1.20 -9 14 0 35.48 1.07 -5 -9 0 34.29 1.21 14 -9 0 36.57 1.14 -5 -9 0 33.67 0.94 14 -5 0 32.38 1.08 -9 14 0 34.03 1.07 -9 14 0 35.67 1.18 -5 14 0 33.16 0.93 -9 -5 0 34.40 1.07 -9 -5 0 35.09 1.18 10 4 0 43.30 1.36 4 -14 0 45.07 1.38 10 -14 0 41.73 1.33 -14 4 0 42.12 1.37 4 10 0 42.03 1.29 -14 4 0 43.75 1.15 4 10 0 41.46 1.40 10 -14 0 40.03 1.32 10 4 0 43.18 1.26 -14 10 0 44.43 1.38 4 -14 0 43.60 1.40 10 4 0 42.90 1.31 14 -4 0 43.49 1.11 -10 -4 0 41.10 1.29 -4 14 0 41.19 1.40 -10 -4 0 37.03 1.44 14 -4 0 41.59 1.28 14 -10 0 43.77 1.34 -10 14 0 43.99 1.29 -4 -10 0 44.17 1.41 14 -4 0 43.39 1.13 -4 14 0 42.64 1.29 -10 14 0 43.57 1.27 -4 -10 0 42.78 1.33 11 -14 0 13.02 0.67 -14 11 0 12.16 0.78 11 -14 0 12.32 0.77 -14 3 0 12.31 0.53 -14 3 0 12.24 0.80 11 3 0 10.40 0.80 3 -14 0 12.22 0.76 3 11 0 11.98 0.75 3 -14 0 11.71 0.72 3 11 0 10.98 0.69 11 3 0 11.43 0.60 11 3 0 11.39 0.67 -11 14 0 11.89 0.62 -3 14 0 10.57 0.68 -3 -11 0 11.62 0.73 14 -3 0 10.71 0.44 -11 14 0 11.06 0.70 -11 -3 0 10.90 0.68 14 -11 0 11.57 0.75 -11 14 0 11.55 0.71 -11 -3 0 10.84 0.68 14 -3 0 11.71 0.67 14 -11 0 11.63 0.45 -3 14 0 11.21 0.76 14 -3 0 12.04 0.50 -3 -11 0 11.98 0.77 12 -14 0 24.36 0.90 -14 12 0 26.50 1.03 -14 2 0 26.02 1.02 12 2 0 26.27 0.97 2 12 0 24.25 0.96 -14 12 0 24.66 0.75 12 2 0 24.75 0.94 2 -14 0 24.91 1.03 12 -14 0 25.06 1.02 2 -14 0 25.53 1.02 2 12 0 25.87 1.04 12 2 0 24.89 0.86 -14 2 0 25.16 0.86 14 -2 0 24.71 0.83 14 -12 0 24.72 0.78 14 -12 0 25.04 0.79 -12 14 0 25.35 0.86 -2 14 0 24.42 0.96 -12 14 0 24.43 0.98 14 -2 0 24.73 0.76 -2 -12 0 23.54 1.05 -2 14 0 24.76 1.03 14 -2 0 25.71 0.95 14 -12 0 25.37 1.01 -12 -2 0 25.36 0.96 -2 -12 0 23.75 1.00 -12 -2 0 24.45 0.97 1 13 0 41.05 1.44 1 -14 0 40.86 1.43 13 1 0 41.07 1.34 1 -14 0 43.45 1.40 -14 1 0 43.52 1.38 13 -14 0 43.91 1.30 -14 13 0 42.62 1.19 13 1 0 44.40 1.34 -14 1 0 42.68 1.30 13 1 0 46.08 1.33 13 -14 0 42.12 1.39 -14 13 0 42.73 1.38 13 -14 0 43.28 1.31 1 13 0 42.38 1.34 14 -13 0 43.30 1.24 -13 14 0 40.97 1.23 -1 -13 0 44.26 1.45 -1 14 0 43.50 1.35 -13 -1 0 42.96 1.38 -13 14 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70.96 1.99 6 -15 0 69.00 2.01 6 -15 0 71.42 1.99 9 6 0 71.53 1.97 -6 -9 0 68.45 2.02 15 -9 0 68.86 1.94 -9 15 0 68.37 1.87 -9 15 0 69.53 2.01 -9 -6 0 69.66 2.01 -6 15 0 68.83 1.92 -9 15 0 69.28 1.90 15 -6 0 69.03 1.93 -6 -9 0 68.99 1.80 -6 15 0 66.66 1.79 -6 15 0 67.64 2.01 -9 -6 0 68.20 1.88 10 5 0 12.01 0.66 10 5 0 12.57 0.75 5 -15 0 13.33 0.80 10 -15 0 12.05 0.75 5 10 0 13.56 0.74 -15 10 0 13.64 0.84 5 10 0 12.89 0.78 10 5 0 12.89 0.77 10 -15 0 12.20 0.71 5 -15 0 13.44 0.84 -15 5 0 12.87 0.84 -10 15 0 13.43 0.78 15 -10 0 12.74 0.75 -10 -5 0 13.83 0.76 -5 -10 0 12.38 0.79 -10 15 0 12.76 0.68 15 -5 0 11.81 0.67 -5 15 0 12.45 0.79 -10 -5 0 12.43 0.69 -5 15 0 12.68 0.72 -10 15 0 12.92 0.69 -15 4 0 23.95 1.03 11 4 0 24.12 0.88 4 11 0 22.96 1.01 11 -15 0 24.56 1.02 4 11 0 23.61 0.94 11 4 0 23.46 0.96 4 -15 0 23.87 1.02 -15 11 0 24.56 1.03 4 -15 0 23.93 0.96 -15 4 0 24.50 0.74 11 4 0 24.84 0.98 -4 15 0 23.36 0.92 15 -4 0 24.36 0.72 -11 -4 0 23.47 0.93 -11 -4 0 24.67 0.98 -11 15 0 24.02 0.98 15 -4 0 24.66 0.94 15 -11 0 26.26 0.99 -4 -11 0 23.10 0.93 -11 15 0 23.95 0.88 -4 15 0 23.29 1.04 -11 15 0 23.64 0.91 -4 -11 0 24.08 1.03 12 3 0 22.95 0.85 -15 3 0 23.42 0.79 12 3 0 23.49 0.95 12 3 0 22.46 0.96 3 -15 0 22.98 1.01 12 -15 0 22.51 0.92 3 -15 0 23.02 1.01 3 12 0 23.14 1.02 12 -15 0 21.92 0.93 -15 3 0 23.15 1.01 3 12 0 23.52 0.94 -15 12 0 23.70 1.01 15 -3 0 23.70 0.76 -3 -12 0 23.85 0.98 -3 -12 0 22.33 1.02 15 -12 0 23.29 0.70 -3 15 0 22.43 1.02 -12 15 0 23.07 0.86 -12 -3 0 22.11 1.10 15 -3 0 23.06 0.93 -12 15 0 19.14 1.30 -12 -3 0 23.45 0.96 -12 15 0 23.16 0.96 -3 15 0 22.81 0.93 15 -12 0 23.62 0.97 2 -15 0 6.12 0.75 -15 13 0 4.85 0.45 13 -15 0 5.37 0.74 -15 2 0 5.84 0.73 2 13 0 5.12 0.71 -15 2 0 4.65 0.50 13 2 0 5.43 0.67 13 2 0 5.37 0.55 2 13 0 5.21 0.63 -15 13 0 6.43 0.77 2 -15 0 5.28 0.69 13 2 0 5.52 0.60 13 -15 0 5.84 0.57 -13 15 0 5.19 0.71 -13 -2 0 6.01 0.68 -13 -2 0 4.73 0.62 15 -2 0 4.45 0.47 15 -13 0 5.70 0.41 -2 -13 0 5.36 0.72 15 -13 0 4.78 0.42 -2 -13 0 5.43 0.70 -2 15 0 5.77 0.67 15 -13 0 5.68 0.73 15 -2 0 4.83 0.65 -13 15 0 4.81 0.55 -2 15 0 5.21 0.70 15 -2 0 4.61 0.42 14 1 0 17.57 0.87 14 1 0 18.14 0.82 1 14 0 18.70 0.88 14 -15 0 18.98 0.94 -15 1 0 18.44 0.97 -15 1 0 18.65 0.81 14 -15 0 17.74 0.80 14 1 0 18.43 0.74 -15 14 0 19.12 0.71 1 -15 0 19.30 0.97 1 14 0 17.41 0.94 1 -15 0 17.11 0.94 -15 14 0 18.40 0.97 15 -14 0 19.68 0.72 -1 15 0 18.04 0.86 15 -14 0 18.41 0.73 -14 -1 0 18.46 0.86 15 -1 0 18.09 0.87 -14 15 0 19.14 0.94 -1 15 0 16.78 0.94 15 -1 0 18.14 0.77 -1 -14 0 18.52 0.95 -1 -14 0 18.52 0.96 15 -14 0 18.30 0.93 15 -1 0 17.81 0.70 -14 -1 0 20.63 0.93 -14 15 0 18.47 0.73 0 15 0 45.59 1.64 -15 15 0 51.31 1.62 0 -15 0 46.85 1.65 -15 0 0 51.28 1.62 15 0 0 53.89 1.59 -15 0 0 52.64 1.58 0 15 0 48.90 1.55 15 -15 0 52.77 1.61 0 -15 0 50.45 1.61 15 -15 0 51.31 1.51 -15 15 0 51.17 1.45 15 0 0 53.33 1.48 15 0 0 51.73 1.54 8 -16 0 61.72 1.82 8 8 0 61.32 1.85 8 -16 0 61.83 1.84 -16 8 0 60.84 1.82 8 8 0 59.96 1.78 8 8 0 60.68 1.74 16 -8 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9.34 0.71 -16 5 0 9.86 0.83 11 5 0 9.85 0.76 11 5 0 9.14 0.73 5 -16 0 9.55 0.81 -16 11 0 10.31 0.83 -11 -5 0 9.03 0.71 -5 -11 0 9.89 0.76 -11 16 0 9.17 0.75 16 -11 0 9.46 0.74 -5 16 0 10.60 0.73 -5 -11 0 9.06 0.76 16 -5 0 10.83 0.71 -5 16 0 9.28 0.77 -11 16 0 10.67 0.69 -11 16 0 9.50 0.66 -11 -5 0 10.33 0.72 -16 12 0 6.71 0.80 -16 4 0 4.91 0.39 12 -16 0 5.38 0.64 -16 4 0 5.44 0.76 12 4 0 4.84 0.71 4 -16 0 5.11 0.77 4 -16 0 5.88 0.71 4 12 0 6.20 0.67 12 4 0 4.86 0.60 12 -16 0 4.41 0.66 4 12 0 6.55 0.71 12 4 0 5.06 0.64 -12 16 0 5.83 0.66 -4 -12 0 5.56 0.69 -4 16 0 5.65 0.66 -12 16 0 4.79 0.67 -12 -4 0 5.55 0.69 16 -12 0 5.31 0.64 -12 16 0 5.60 0.60 -12 -4 0 4.89 0.67 -4 -12 0 5.81 0.60 -4 16 0 5.36 0.72 16 -4 0 4.80 0.65 13 3 0 10.23 0.73 3 13 0 10.99 0.81 13 -16 0 11.51 0.83 -16 13 0 12.01 0.87 3 13 0 11.44 0.76 3 -16 0 10.92 0.82 13 3 0 12.06 0.68 13 3 0 10.57 0.79 3 -16 0 11.49 0.87 -16 3 0 10.86 0.57 -16 3 0 11.60 0.85 16 -3 0 11.53 0.77 -13 16 0 12.98 0.81 16 -13 0 10.98 0.82 16 -3 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10.52 0.86 16 -16 0 29.61 1.21 0 -16 0 29.61 1.20 16 0 0 29.96 1.10 -16 0 0 27.93 1.11 -16 0 0 29.95 1.21 0 16 0 27.63 1.12 -16 16 0 29.33 1.22 9 8 0 10.23 0.77 -17 8 0 10.70 0.88 8 -17 0 10.77 0.87 9 8 0 11.62 0.83 9 -17 0 10.74 0.78 9 -17 0 9.86 0.87 9 8 0 10.49 0.72 8 9 0 11.64 0.84 8 -17 0 9.81 0.79 -17 9 0 11.15 0.86 8 9 0 11.32 0.75 8 9 0 10.26 0.79 17 -9 0 9.90 0.70 -9 17 0 10.76 0.75 -9 17 0 11.36 0.82 -8 17 0 10.42 0.76 17 -8 0 10.25 0.69 -8 -9 0 10.86 0.79 -9 17 0 10.23 0.65 -9 -8 0 10.51 0.69 -9 -8 0 9.61 0.78 -8 17 0 10.70 0.81 7 -17 0 45.62 1.46 10 7 0 45.52 1.46 7 10 0 46.07 1.51 7 10 0 45.96 1.41 -17 7 0 43.95 1.48 10 7 0 45.05 1.48 10 7 0 45.81 1.38 10 -17 0 44.58 1.49 10 -17 0 42.70 1.47 -17 10 0 43.11 1.48 7 -17 0 44.38 1.50 -10 17 0 43.56 1.36 -10 -7 0 44.00 1.48 -10 17 0 44.96 1.40 17 -7 0 43.51 1.40 17 -10 0 44.48 1.41 -7 -10 0 42.42 1.50 -10 -7 0 46.95 1.40 -7 17 0 41.35 1.50 -10 17 0 44.41 1.49 -7 17 0 45.35 1.42 11 -17 0 18.21 0.96 11 6 0 17.09 0.90 11 6 0 16.10 0.83 11 -17 0 16.59 0.88 6 11 0 16.62 0.84 6 -17 0 18.97 0.99 11 6 0 16.94 0.87 6 -17 0 17.58 0.93 -17 6 0 18.13 0.99 6 11 0 15.06 0.93 -17 11 0 17.76 0.95 -11 17 0 18.06 0.84 -6 17 0 17.56 0.87 17 -6 0 18.93 0.87 -11 -6 0 17.76 0.89 -6 -11 0 16.98 0.93 17 -11 0 17.92 0.91 -11 17 0 17.15 0.93 -6 17 0 17.26 0.94 -11 17 0 18.74 0.86 -11 -6 0 17.33 0.90 12 5 0 8.31 0.74 -17 5 0 9.18 0.86 12 5 0 7.81 0.78 5 12 0 8.58 0.72 5 -17 0 9.00 0.77 5 -17 0 8.42 0.84 -17 12 0 8.82 0.87 12 -17 0 8.66 0.84 12 -17 0 8.49 0.71 5 12 0 8.08 0.79 12 5 0 7.86 0.69 -12 17 0 8.54 0.76 -5 17 0 7.55 0.75 -12 -5 0 8.36 0.75 -5 -12 0 8.22 0.77 17 -5 0 8.41 0.73 -12 17 0 8.36 0.69 17 -12 0 9.22 0.77 -5 -12 0 9.07 0.78 -5 17 0 7.35 0.78 -12 -5 0 8.47 0.75 -12 17 0 8.57 0.78 -17 13 0 8.43 0.86 13 4 0 7.45 0.66 13 -17 0 6.31 0.81 4 13 0 7.90 0.74 4 13 0 9.10 1.07 -17 4 0 7.74 0.83 13 -17 0 7.85 0.71 4 -17 0 7.62 0.79 4 -17 0 5.95 0.75 13 4 0 7.04 0.79 13 4 0 7.49 0.71 17 -13 0 7.72 0.79 -4 17 0 6.72 0.78 -13 -4 0 7.00 0.73 -4 17 0 8.05 0.77 -13 -4 0 6.85 0.76 -13 17 0 6.73 0.68 17 -4 0 8.16 0.75 -4 -13 0 6.94 0.79 -13 17 0 7.24 0.76 -13 17 0 7.78 0.78 -4 -13 0 7.42 0.79 14 3 0 10.32 0.81 -17 3 0 11.23 0.89 14 -17 0 10.21 0.73 14 3 0 9.33 0.68 -17 3 0 9.08 0.58 3 -17 0 9.63 0.94 -17 14 0 10.71 0.90 14 3 0 9.34 0.74 -14 17 0 9.40 0.73 -14 -3 0 9.68 0.81 17 -3 0 10.26 0.79 -14 -3 0 9.61 0.85 -3 17 0 8.88 0.87 -14 17 0 8.99 0.81 17 -14 0 9.58 0.88 15 2 0 29.78 1.17 15 -17 0 29.77 1.20 15 -17 0 28.24 1.15 2 15 0 28.03 1.13 15 2 0 30.22 1.46 2 -17 0 30.50 1.23 15 2 0 30.04 1.06 -17 15 0 30.98 1.27 15 -17 0 31.59 1.22 -17 2 0 31.37 1.24 -15 -2 0 29.54 1.19 -2 17 0 29.48 1.14 -15 17 0 30.86 1.07 -15 -2 0 30.86 1.23 -2 -15 0 30.54 1.22 17 -15 0 29.59 1.21 -15 17 0 31.46 1.22 1 16 0 75.60 2.13 16 1 0 77.64 2.06 16 -17 0 73.22 2.16 -17 1 0 74.97 2.19 1 -17 0 72.74 2.14 16 1 0 74.10 2.17 -17 16 0 76.23 2.19 16 1 0 75.94 2.14 17 -1 0 74.81 2.13 -16 -1 0 72.01 2.41 -1 -16 0 73.35 2.16 -1 17 0 72.26 2.11 -16 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0.51 12 -18 0 10.37 0.84 6 -18 0 11.81 0.91 6 12 0 10.55 0.80 12 -18 0 10.72 0.81 12 6 0 9.61 0.82 12 6 0 10.03 0.74 6 -18 0 9.80 0.82 -6 18 0 9.49 0.87 18 -6 0 9.13 0.75 -12 18 0 10.55 0.85 -12 -6 0 10.30 0.81 -12 18 0 10.39 0.79 -12 -6 0 10.04 0.82 -6 -12 0 10.16 0.84 -6 18 0 11.45 0.81 -12 18 0 9.95 0.77 13 5 0 19.17 0.99 13 -18 0 20.61 1.04 13 5 0 19.71 0.92 5 13 0 20.40 1.19 5 -18 0 19.30 1.06 13 5 0 20.62 1.01 13 -18 0 19.15 0.96 18 -5 0 18.40 1.31 -13 18 0 17.97 1.00 18 -13 0 20.90 1.01 -13 18 0 19.34 0.98 -13 -5 0 19.57 1.01 -5 -13 0 20.84 1.01 -13 -5 0 19.56 1.01 -13 18 0 20.29 0.91 14 4 0 22.53 1.04 -18 14 0 20.06 1.21 14 -18 0 23.04 1.09 14 4 0 20.74 1.03 4 14 0 21.20 1.00 -18 4 0 20.52 1.25 14 -18 0 21.79 1.01 14 4 0 22.20 0.94 4 -18 0 24.16 1.13 18 -14 0 22.02 1.04 -14 -4 0 22.61 1.08 -4 18 0 23.91 1.02 -4 -14 0 21.39 0.98 18 -4 0 22.04 0.99 -14 18 0 21.66 1.06 -14 18 0 22.65 0.99 -14 -4 0 19.95 1.04 15 -18 0 38.95 1.41 15 3 0 41.22 1.44 15 3 0 41.91 1.43 15 -18 0 41.92 1.46 -18 15 0 40.27 1.48 3 15 0 40.56 1.39 -18 3 0 38.77 1.47 3 -18 0 38.78 1.40 15 -18 0 39.20 1.39 15 3 0 43.69 1.35 18 -15 0 41.28 1.42 -3 18 0 41.54 1.41 -15 -3 0 41.10 1.45 -15 -3 0 39.41 1.45 -15 18 0 41.20 1.46 18 -3 0 42.23 1.39 -3 -15 0 41.15 1.45 -15 18 0 42.35 1.35 2 -18 0 17.46 1.05 -18 16 0 17.49 1.08 16 -18 0 17.37 0.96 16 2 0 18.31 1.00 16 2 0 18.21 0.88 2 16 0 17.21 0.96 16 2 0 18.12 1.46 -18 2 0 19.04 1.06 -2 -16 0 18.54 1.04 -16 -2 0 19.70 1.06 -16 -2 0 18.71 1.11 18 -16 0 18.52 1.02 -16 18 0 20.19 1.10 -2 18 0 19.60 1.01 -16 18 0 18.74 0.91 18 -2 0 17.72 0.96 17 1 0 31.36 1.24 17 -18 0 29.04 1.27 1 17 0 30.77 1.18 -18 17 0 30.75 1.34 -18 1 0 29.97 1.32 1 -18 0 32.20 1.30 -1 -17 0 31.36 1.27 -17 18 0 30.46 1.33 -17 -1 0 30.33 1.34 -1 18 0 30.16 1.23 18 -1 0 31.94 1.23 18 -17 0 31.38 1.26 0 -18 0 75.09 2.21 18 0 0 73.79 2.16 18 -18 0 74.55 2.21 -18 0 0 75.14 2.26 -18 18 0 74.13 2.24 0 18 0 74.32 2.17 10 -19 0 7.59 0.86 10 -19 0 7.76 0.83 10 9 0 8.41 0.86 -19 10 0 9.09 0.92 10 9 0 7.66 0.82 -19 9 0 7.58 0.87 9 -19 0 7.60 0.85 9 -19 0 7.89 0.91 10 9 0 8.89 0.77 9 10 0 9.15 0.79 9 10 0 7.73 0.89 -9 19 0 7.00 0.81 -9 19 0 8.47 0.87 -10 -9 0 8.13 0.82 -9 -10 0 9.29 0.83 19 -9 0 8.46 0.79 19 -10 0 7.69 0.77 -10 19 0 8.49 0.92 -10 19 0 8.76 0.82 -19 11 0 36.76 1.39 11 8 0 36.35 1.34 11 -19 0 39.32 1.39 8 -19 0 33.55 1.37 11 8 0 33.50 1.36 11 -19 0 35.07 1.36 -19 8 0 36.66 1.38 8 -19 0 36.98 1.38 11 8 0 37.58 1.27 19 -8 0 37.19 1.28 19 -11 0 37.46 1.30 -11 -8 0 35.11 1.35 -11 19 0 34.30 1.39 -8 19 0 37.25 1.32 -11 19 0 37.98 1.29 12 7 0 34.97 1.29 -19 7 0 33.31 1.31 7 12 0 32.75 1.22 12 7 0 30.45 1.30 7 -19 0 32.51 1.26 12 -19 0 34.73 1.31 12 7 0 33.80 1.23 -19 12 0 35.15 1.34 12 -19 0 31.62 1.28 -12 19 0 32.37 1.21 19 -12 0 31.87 1.18 -12 -7 0 33.84 1.30 -7 -12 0 34.92 1.27 -12 19 0 33.59 1.24 19 -7 0 35.33 1.22 -12 -7 0 31.89 1.30 -12 19 0 31.85 1.33 13 6 0 2.43 0.51 6 13 0 2.12 0.52 13 6 0 3.45 0.58 6 -19 0 2.02 0.59 13 6 0 2.46 0.63 -19 13 0 1.84 0.58 13 -19 0 3.09 0.53 -19 6 0 2.09 0.57 13 -19 0 2.94 0.63 19 -13 0 1.43 0.52 -6 -13 0 1.12 0.50 -6 19 0 2.71 0.57 -13 -6 0 3.62 0.59 19 -6 0 3.04 0.54 -13 19 0 1.88 0.48 -13 -6 0 2.03 0.50 -13 19 0 2.77 0.55 -13 19 0 2.07 0.52 14 -19 0 9.35 0.83 14 5 0 9.11 0.89 14 -19 0 7.61 0.84 14 5 0 9.42 0.85 -19 14 0 10.77 0.95 5 14 0 9.41 0.80 5 -19 0 9.27 0.92 14 5 0 9.69 0.79 -19 5 0 10.15 0.96 -14 -5 0 9.50 0.87 -14 19 0 9.41 0.90 19 -5 0 9.31 0.82 19 -14 0 10.11 0.86 -14 19 0 9.99 0.82 -14 -5 0 9.68 0.95 -5 19 0 10.61 0.85 -5 -14 0 9.68 0.88 4 -19 0 25.02 1.18 -19 4 0 23.12 1.17 15 -19 0 25.38 1.56 4 15 0 23.84 1.04 15 4 0 26.45 1.05 15 4 0 23.71 1.11 15 4 0 24.41 1.14 15 -19 0 23.96 1.14 -19 15 0 24.82 1.16 19 -15 0 22.91 1.06 -15 -4 0 23.75 1.19 -15 19 0 24.35 1.17 -15 19 0 25.02 1.05 19 -4 0 25.39 1.07 -15 -4 0 21.08 1.13 -4 -15 0 24.03 1.13 -4 19 0 23.26 1.08 -19 3 0 24.69 1.20 3 -19 0 24.73 1.11 -19 16 0 25.66 1.22 3 16 0 23.86 1.07 16 3 0 25.12 1.16 16 -19 0 25.69 1.17 16 3 0 26.38 1.05 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29.11 1.19 -14 20 0 29.73 1.19 -14 -6 0 26.40 1.25 15 -20 0 6.49 0.73 -20 5 0 6.36 0.93 15 5 0 5.57 0.71 -20 15 0 6.45 0.94 5 -20 0 4.94 0.69 15 5 0 6.01 0.80 5 15 0 5.89 0.83 15 5 0 6.02 0.90 -15 20 0 5.88 0.87 20 -15 0 6.73 0.71 -15 -5 0 4.89 0.84 -15 -5 0 6.91 0.97 -15 20 0 6.65 0.74 20 -5 0 5.72 0.80 -5 -15 0 4.33 0.63 -5 20 0 5.81 0.84 16 4 0 11.51 0.85 4 -20 0 11.44 1.02 -20 4 0 10.48 1.04 16 -20 0 11.06 0.97 4 16 0 10.60 0.89 16 4 0 9.92 0.96 -20 16 0 12.39 1.05 -4 -16 0 11.98 0.97 -16 20 0 12.01 1.06 -4 20 0 11.67 0.91 -16 -4 0 12.17 1.12 -16 20 0 10.86 0.93 20 -16 0 11.80 0.91 20 -4 0 10.74 0.88 3 -20 0 17.07 1.07 -20 17 0 15.66 1.11 3 17 0 17.11 1.00 17 -20 0 16.23 1.06 -20 3 0 15.89 1.14 17 3 0 17.02 1.05 -3 20 0 17.16 1.02 -3 -17 0 17.34 1.07 -17 20 0 16.45 1.82 20 -17 0 16.41 1.04 20 -3 0 15.96 0.97 2 -20 0 15.68 1.05 2 18 0 15.32 1.00 18 2 0 15.87 1.03 -20 2 0 15.89 1.18 18 -20 0 14.73 1.05 -20 18 0 14.83 1.12 20 -2 0 15.13 1.01 20 -18 0 14.01 1.02 -18 -2 0 16.25 1.20 -2 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11.48 0.98 -6 -10 4 11.54 1.09 -16 9 4 36.65 1.50 7 -16 4 34.63 1.32 9 7 4 34.42 1.35 7 -16 4 35.92 1.34 9 7 4 36.71 1.34 9 -16 -4 35.64 1.35 -16 9 4 33.60 1.39 7 9 -4 31.95 1.21 -9 16 4 36.00 1.43 -9 -7 -4 32.59 1.33 -7 -9 4 36.03 1.51 16 -9 -4 34.29 1.31 -9 16 4 34.98 1.31 16 -9 -4 34.27 1.23 -7 -9 4 37.21 1.30 16 -7 4 34.33 1.27 16 -9 -4 30.80 1.40 -7 16 -4 33.15 1.24 8 8 4 19.20 1.04 8 8 -4 17.82 0.94 8 8 4 16.16 1.27 -16 8 4 18.54 1.22 8 -16 4 15.85 1.06 8 -16 4 19.73 1.07 8 -16 -4 17.82 1.00 -16 8 4 16.58 1.04 8 -16 4 18.78 1.05 -8 16 4 20.55 1.14 16 -8 4 18.53 0.95 16 -8 -4 20.14 1.03 -8 -8 4 18.90 0.99 -8 -8 4 18.19 1.22 16 -8 -4 19.04 1.25 16 -8 -4 15.88 1.09 -8 16 4 19.29 1.00 -8 16 -4 18.50 0.95 9 -16 4 3.00 0.63 7 -16 -4 1.43 0.60 9 -16 4 2.38 0.62 7 9 4 3.02 0.67 -16 7 4 3.68 0.79 9 -16 4 1.66 0.56 -16 7 4 1.22 0.55 9 7 -4 2.34 0.53 7 9 4 2.76 0.54 16 -7 -4 2.74 0.58 16 -7 -4 0.73 0.55 16 -9 4 2.58 0.54 -9 16 -4 2.66 0.55 -9 16 -4 2.58 0.50 -9 -7 4 1.98 0.53 -9 -7 4 3.03 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0.68 -11 1 9 0.87 0.95 1 10 9 1.99 1.01 -10 -1 9 1.39 0.91 11 -1 -9 2.84 0.73 -1 -10 -9 2.41 0.70 11 -10 9 2.57 0.83 -1 11 9 2.63 0.99 8 4 9 18.01 1.40 4 -12 9 18.64 1.38 -12 8 9 19.58 1.51 4 8 -9 18.56 1.20 8 -12 -9 17.85 1.20 12 -8 -9 16.95 1.22 -4 -8 9 16.56 1.49 -8 -4 -9 17.85 1.40 12 -4 9 19.39 1.36 -8 12 9 18.80 1.61 -4 12 -9 19.60 1.23 7 -12 -9 15.47 1.15 -12 7 9 13.93 1.46 5 7 -9 13.67 1.08 7 5 9 13.09 1.39 5 -12 9 14.06 1.29 12 -7 -9 11.02 1.18 -7 12 9 15.67 1.50 -7 -5 -9 12.23 1.27 -5 -7 9 10.80 1.41 12 -5 9 14.25 1.24 -5 12 -9 13.63 1.16 6 6 -9 3.53 0.70 6 -12 9 3.99 0.85 6 -12 -9 3.02 0.71 6 6 9 3.94 0.99 -12 6 9 4.44 1.09 -6 -6 -9 4.78 0.89 12 -6 9 2.19 0.82 -6 12 -9 8.48 1.21 -6 -6 9 4.97 1.05 -6 12 9 3.32 1.04 12 -6 -9 2.46 0.76 7 5 -9 27.09 1.34 5 7 9 26.80 1.63 7 -12 9 25.67 1.47 -12 5 9 27.30 1.64 12 -5 -9 25.97 1.35 -7 12 -9 30.36 1.52 -5 -7 -9 28.69 1.61 -7 -5 9 26.73 1.61 -5 12 9 27.70 1.72 12 -7 9 26.26 1.47 -12 4 9 16.12 1.45 8 -12 9 15.83 1.30 8 4 -9 14.82 1.17 4 8 9 15.65 1.50 12 -8 9 17.02 1.31 12 -4 -9 18.44 1.19 -4 12 9 21.84 1.54 -8 12 -9 16.91 1.41 -4 -8 -9 17.84 1.25 -8 -4 9 17.39 1.44 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 73263 _olex2_submission_special_instructions 'No special instructions were received' loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.521(17) 2 0.479(17)