data_X8_15165 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H12 N P' _chemical_formula_weight 225.22 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 42 _space_group_name_H-M_alt 'F m m 2' _space_group_name_Hall 'F 2 -2' _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' 'x, -y, z' '-x, y, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x, -y+1/2, z+1/2' '-x, y+1/2, z+1/2' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' _cell_length_a 9.779(3) _cell_length_b 16.542(6) _cell_length_c 6.543(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1058.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1890 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 29.38 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.413 _exptl_crystal_F_000 472 _exptl_transmission_factor_min 0.6748 _exptl_transmission_factor_max 0.7463 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.110 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.226 _shelx_estimated_absorpt_T_min 0.969 _shelx_estimated_absorpt_T_max 0.989 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'I\mS micro-focus sealed tube, multilayer optics' _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_reflns_number 7834 _diffrn_reflns_av_unetI/netI 0.0252 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.462 _diffrn_reflns_theta_max 30.517 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_point_group_measured_fraction_full 0.969 _reflns_number_total 834 _reflns_number_gt 755 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.745 _reflns_Friedel_fraction_max 0.875 _reflns_Friedel_fraction_full 0.936 _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 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Bruker X8 Kappa DUO four-circle diffractometer, Bruker APEX2 CCD. The instrument was purchased with the help of funding from the National Science Foundation (NSF) under Grant Number CHE-0946721. Please acknowledge this grant in all publications of this structure. ; _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^)+(0.0440P)^2^+0.8809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 288 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.07(7) _chemical_absolute_configuration ? _refine_ls_number_reflns 834 _refine_ls_number_parameters 54 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0361 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0879 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.021 _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 P1 P 1.0000 1.01803(6) 0.44697(16) 0.0241(3) Uani 0.25 1 d DS U P A -1 N1 N 1.0000 0.9285(3) 0.3271(6) 0.0285(9) Uani 0.25 1 d DS U P A -1 H1A H 1.0000 0.9282(18) 0.195(3) 0.034 Uiso 0.25 1 d DS U P B -1 H1B H 1.0000 0.8851(12) 0.405(4) 0.034 Uiso 0.25 1 d DS U P C -1 C1 C 0.8752(2) 1.0000 0.6696(4) 0.0265(5) Uani 1 2 d S TU P . . H1 H 0.7756 1.0000 0.6345 0.032 Uiso 1 2 d R U P A . C2 C 0.92792(14) 0.92618(11) 0.7804(2) 0.0259(3) Uani 1 1 d . U . . . C3 C 0.85636(16) 0.86377(11) 0.8708(3) 0.0295(4) Uani 1 1 d . U . . . H3 H 0.7592 0.8634 0.8697 0.035 Uiso 1 1 calc R U . . . C4 C 0.92867(16) 0.80153(10) 0.9632(3) 0.0345(4) Uani 1 1 d . U . . . H4 H 0.8806 0.7585 1.0271 0.041 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 P1 0.0140(4) 0.0344(9) 0.0241(4) -0.0016(5) 0.004(4) -0.002(6) N1 0.0233(18) 0.0394(19) 0.0227(18) -0.0063(17) 0.001(15) -0.001(12) C1 0.0102(8) 0.0448(13) 0.0245(10) 0.000 0.0013(7) 0.000 C2 0.0158(7) 0.0383(7) 0.0238(7) -0.0031(7) 0.0003(6) -0.0004(6) C3 0.0164(6) 0.0413(8) 0.0307(8) -0.0028(7) 0.0016(6) -0.0022(7) C4 0.0256(8) 0.0396(8) 0.0382(9) 0.0020(9) 0.0015(9) -0.0016(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 P1 N1 1.676(4) . ? P1 C1 1.924(2) . ? N1 H1A 0.865(17) . ? N1 H1B 0.881(18) . ? C1 C2 1.511(2) . ? C1 C2 1.511(2) 3_575 ? C1 H1 1.0000 . ? C2 C3 1.380(2) . ? C2 C2 1.410(3) 4_755 ? C3 C4 1.388(2) . ? C3 H3 0.9500 . ? C4 C4 1.395(3) 4_755 ? C4 H4 0.9500 . ? 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 N1 P1 C1 102.55(12) . . ? P1 N1 H1A 118(2) . . ? P1 N1 H1B 116.6(17) . . ? H1A N1 H1B 125(3) . . ? C2 C1 C2 107.84(19) . 3_575 ? C2 C1 P1 105.78(12) . . ? C2 C1 P1 91.23(11) 3_575 . ? C2 C1 H1 116.3 . . ? C2 C1 H1 116.3 3_575 . ? P1 C1 H1 116.3 . . ? C3 C2 C2 120.46(9) . 4_755 ? C3 C2 C1 129.57(15) . . ? C2 C2 C1 109.96(10) 4_755 . ? C2 C3 C4 118.90(15) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C4 120.64(9) . 4_755 ? C3 C4 H4 119.7 . . ? C4 C4 H4 119.7 4_755 . ? _refine_diff_density_max 0.245 _refine_diff_density_min -0.165 _refine_diff_density_rms 0.045 _shelx_res_file ; X8_15165.res created by SHELXL-2014/7 TITL X8_15165 in Fmm2 CELL 0.71073 9.77916 16.54203 6.54323 90.0000 90.0000 90.0000 ZERR 4.00 0.00262 0.00618 0.00262 0.0000 0.0000 0.0000 LATT -4 SYMM -X, -Y, Z SYMM X, -Y, Z SYMM -X, Y, Z SFAC C H N P UNIT 56 48 4 4 TEMP -173 SIZE 0.05 0.11 0.14 omit 6 0 0 ! Fo >> Fc; outlier DFIX 0.88 n1 h1a n1 h1b sadi p1 h1a p1 h1b dfix 1.55 h1a h1b damp 400 l.s. 30 BOND $H LIST 4 FMAP 2 PLAN 20 acta htab simu rigu WGHT 0.044000 0.880900 FVAR 0.20808 part -1 P1 4 11.000000 1.018025 0.446973 10.25000 0.01399 0.03438 = 0.02406 -0.00165 0.00393 -0.00249 N1 3 11.000000 0.928461 0.327089 10.25000 0.02331 0.03936 = 0.02269 -0.00625 0.00096 -0.00139 H1A 2 11.000000 0.928171 0.194845 10.25000 -1.20000 H1B 2 11.000000 0.885120 0.405337 10.25000 -1.20000 REM Q1 1 1.0000 0.9264 0.2065 10.50000 0.05 0.38 REM Q4 1 1.0000 0.8791 0.4489 10.50000 0.05 0.26 part 0 C1 1 0.875171 1.000000 0.669628 10.50000 0.01019 0.04477 = 0.02448 0.00000 0.00132 0.00000 AFIX 3 H1 2 0.775650 1.000000 0.634509 10.50000 -1.20000 AFIX 0 C2 1 0.927915 0.926182 0.780423 11.00000 0.01576 0.03826 = 0.02380 -0.00310 0.00034 -0.00035 C3 1 0.856358 0.863770 0.870771 11.00000 0.01641 0.04127 = 0.03075 -0.00282 0.00160 -0.00218 AFIX 43 H3 2 0.759217 0.863426 0.869707 11.00000 -1.20000 AFIX 0 C4 1 0.928674 0.801527 0.963193 11.00000 0.02561 0.03957 = 0.03825 0.00200 0.00151 -0.00155 AFIX 43 H4 2 0.880570 0.758504 1.027072 11.00000 -1.20000 AFIX 0 HKLF 4 REM X8_15165 in Fmm2 REM R1 = 0.0361 for 755 Fo > 4sig(Fo) and 0.0414 for all 834 data REM 54 parameters refined using 62 restraints END WGHT 0.0440 0.8809 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.245, deepest hole -0.165, 1-sigma level 0.045 Q1 1 1.0000 0.9256 0.7891 10.50000 0.05 0.24 Q2 1 1.0000 0.8007 0.9697 10.50000 0.05 0.19 Q3 1 0.9334 1.0000 0.5737 10.50000 0.05 0.16 Q4 1 0.8958 0.8293 0.8859 11.00000 0.05 0.16 Q5 1 1.0000 0.8469 0.2758 10.50000 0.05 0.16 Q6 1 1.0000 0.7782 0.7906 10.50000 0.05 0.16 Q7 1 0.9005 0.8972 0.8669 11.00000 0.05 0.15 Q8 1 0.8994 0.9653 0.7775 11.00000 0.05 0.15 Q9 1 0.8942 0.8477 0.9713 11.00000 0.05 0.15 Q10 1 0.8090 1.0000 0.6597 10.50000 0.05 0.13 Q11 1 0.8991 0.7625 0.9567 11.00000 0.05 0.13 Q12 1 1.0000 1.0181 0.3293 10.50000 0.05 0.12 Q13 1 1.0000 0.9358 0.6491 10.50000 0.05 0.12 Q14 1 0.8735 0.7398 1.0937 11.00000 0.05 0.11 Q15 1 0.8961 1.0309 0.6783 11.00000 0.05 0.11 Q16 1 1.0000 0.8811 0.5237 10.50000 0.05 0.11 Q17 1 1.0000 0.8660 0.0977 10.50000 0.05 0.11 Q18 1 0.6723 1.0000 0.8112 10.50000 0.05 0.11 Q19 1 1.0000 0.8025 0.2520 10.50000 0.05 0.11 Q20 1 1.0000 0.9777 0.1050 10.50000 0.05 0.10 ; _shelx_res_checksum 24139 _shelx_hkl_file ; -1 1 -1 270.98 4.35 -1 1 -1 265.24 4.21 -1 1 -1 256.59 4.15 -1 1 -1 260.15 4.11 1 -1 1 270.38 4.58 1 -1 1 276.24 4.42 1 -1 1 273.25 4.59 1 -1 1 275.57 4.37 1 -1 1 272.28 4.55 1 -1 1 273.60 4.33 1 -1 1 272.83 4.53 -2 2 -2 71.46 1.61 -2 2 -2 67.91 1.66 -2 2 -2 69.89 1.67 -2 2 -2 69.65 1.86 2 -2 2 67.91 1.93 2 -2 2 67.87 1.99 2 -2 2 69.06 1.80 2 -2 2 69.25 1.50 2 -2 2 70.94 1.68 2 -2 2 67.09 1.95 -3 3 -3 129.86 3.23 -3 3 -3 128.16 2.86 -3 3 -3 132.48 3.00 3 -3 3 130.38 3.45 3 -3 3 126.54 3.29 3 -3 3 126.27 2.55 3 -3 3 126.96 3.10 3 -3 3 126.28 2.92 3 -3 3 130.00 3.37 -4 4 -4 6.82 0.88 -4 4 -4 7.73 1.10 4 -4 4 6.94 1.06 4 -4 4 5.41 0.80 4 -4 4 5.04 0.85 4 -4 4 5.23 0.98 4 -4 4 4.74 0.97 -5 5 -5 17.57 1.28 -5 5 -5 17.21 1.75 5 -5 5 21.02 1.39 5 -5 5 16.33 1.86 5 -5 5 19.64 1.98 5 -5 5 18.51 1.99 -6 6 -6 14.65 1.61 6 -6 6 10.64 1.66 6 -6 6 12.51 1.82 7 -7 7 0.85 0.84 8 -6 6 8.59 1.73 8 -6 6 3.23 1.09 -8 6 -6 3.69 0.93 7 -5 5 18.33 1.44 7 -5 5 20.14 2.25 7 -5 5 19.70 2.19 -7 5 -5 19.98 2.08 -7 5 -5 20.18 1.46 6 -4 4 16.19 1.72 6 -4 4 18.55 1.91 6 -4 4 18.77 1.27 6 -4 4 21.99 1.45 -6 4 -4 20.70 1.53 -6 4 -4 21.99 1.37 5 -3 3 6.74 1.06 5 -3 3 7.68 0.91 5 -3 3 9.36 0.83 5 -3 3 7.14 0.94 5 -3 3 6.77 1.01 5 -3 3 6.64 0.85 -5 3 -3 7.07 0.86 -5 3 -3 7.92 1.16 4 -2 2 180.55 4.30 4 -2 2 185.38 3.76 4 -2 2 186.65 3.36 4 -2 2 184.62 4.17 4 -2 2 185.10 4.26 4 -2 2 179.94 3.77 4 -2 2 183.66 3.84 -4 2 -2 188.05 3.67 -4 2 -2 191.29 4.36 -4 2 -2 186.57 3.87 3 -1 1 320.86 5.71 3 -1 1 321.87 5.95 3 -1 1 334.28 6.04 3 -1 1 330.84 5.40 3 -1 1 330.43 5.81 3 -1 1 319.86 5.62 -3 1 -1 350.39 6.00 -3 1 -1 347.56 6.01 -3 1 -1 350.20 6.45 2 0 0 935.06 14.36 2 0 0 997.69 14.80 2 0 0 943.51 14.69 -2 0 0 1000.00 14.52 -2 0 0 943.04 14.84 -2 0 0 972.75 14.99 -2 0 0 985.22 14.85 -2 0 0 979.46 14.55 1 1 -1 264.38 4.52 1 1 -1 269.88 4.74 -1 -1 1 269.65 4.71 -1 -1 1 271.98 4.77 -1 -1 1 265.41 4.69 -1 -1 1 276.31 4.52 -1 -1 1 269.89 4.76 -1 -1 1 275.58 4.66 0 2 -2 264.00 4.66 0 2 -2 271.68 4.91 0 -2 2 275.24 4.56 0 -2 2 265.73 4.82 0 -2 2 267.06 5.15 0 -2 2 266.84 4.91 0 -2 2 269.12 5.02 0 -2 2 266.85 5.13 0 -2 2 272.13 5.04 -1 3 -3 177.65 3.63 -1 3 -3 173.76 3.67 -1 3 -3 176.80 3.71 -1 3 -3 174.70 3.70 1 -3 3 173.01 3.70 1 -3 3 167.85 3.66 1 -3 3 173.09 4.05 1 -3 3 173.21 4.08 1 -3 3 175.51 3.36 1 -3 3 168.74 4.11 1 -3 3 179.63 3.78 -2 4 -4 35.31 1.54 -2 4 -4 35.06 1.41 -2 4 -4 34.45 1.58 2 -4 4 35.29 1.81 2 -4 4 34.69 1.60 2 -4 4 38.75 1.94 2 -4 4 34.67 1.66 2 -4 4 37.76 1.55 2 -4 4 35.82 1.88 -3 5 -5 13.99 1.17 -3 5 -5 12.59 1.39 3 -5 5 12.78 1.02 3 -5 5 18.99 1.87 3 -5 5 15.19 1.75 3 -5 5 13.33 1.49 3 -5 5 13.75 1.49 3 -5 5 13.52 1.67 -4 6 -6 25.24 1.76 4 -6 6 27.36 1.98 4 -6 6 25.79 1.75 4 -6 6 29.61 2.25 4 -6 6 31.81 2.25 4 -6 6 25.87 1.60 5 -7 7 1.51 1.04 5 -7 7 0.73 1.06 5 -7 7 0.70 0.69 10 -6 6 5.35 1.52 9 -5 5 18.92 2.40 9 -5 5 16.08 2.09 -9 5 -5 17.81 2.16 -9 5 -5 16.90 1.83 8 -4 4 21.70 1.58 8 -4 4 25.06 2.47 8 -4 4 23.66 2.48 -8 4 -4 18.74 1.45 -8 4 -4 20.17 2.12 7 -3 3 31.88 2.08 7 -3 3 34.53 1.76 7 -3 3 29.56 1.94 7 -3 3 34.94 1.97 -7 3 -3 41.84 2.30 -7 3 -3 35.75 1.83 6 -2 2 133.63 4.00 6 -2 2 138.71 3.77 6 -2 2 134.08 2.56 6 -2 2 137.12 3.95 6 -2 2 134.56 3.13 6 -2 2 134.97 3.57 -6 2 -2 138.34 3.42 -6 2 -2 142.80 4.18 -6 2 -2 139.54 3.68 5 -1 1 271.92 5.66 5 -1 1 265.99 5.48 5 -1 1 274.23 5.58 5 -1 1 274.71 5.87 5 -1 1 280.86 4.94 5 -1 1 278.47 5.92 -5 1 -1 289.19 4.66 -5 1 -1 289.44 5.83 -5 1 -1 287.90 6.28 -5 1 -1 289.53 5.83 4 0 0 66.15 1.85 4 0 0 67.95 2.32 4 0 0 67.76 2.22 -4 0 0 65.89 1.70 -4 0 0 72.50 1.82 -4 0 0 63.66 2.08 -4 0 0 65.65 2.13 -4 0 0 68.74 2.28 3 1 -1 330.93 5.50 3 1 -1 330.28 6.40 -3 -1 1 328.14 6.31 -3 -1 1 340.20 6.05 -3 -1 1 335.45 5.95 -3 -1 1 328.85 6.44 -3 -1 1 335.91 5.93 -3 -1 1 331.14 6.10 -3 -1 1 341.08 6.34 2 2 -2 68.82 2.29 2 2 -2 68.44 2.05 -2 -2 2 68.27 2.23 -2 -2 2 68.46 2.14 -2 -2 2 71.72 2.17 -2 -2 2 69.31 1.95 -2 -2 2 68.63 2.13 -2 -2 2 64.31 2.20 1 3 -3 169.01 4.13 1 3 -3 176.82 3.82 1 3 -3 175.14 4.02 -1 -3 3 170.40 3.91 -1 -3 3 169.67 4.19 -1 -3 3 170.63 4.01 -1 -3 3 171.99 3.68 -1 -3 3 171.87 4.30 -1 -3 3 168.29 4.05 -1 -3 3 170.27 4.28 0 4 -4 158.94 3.89 0 4 -4 156.71 3.73 0 4 -4 156.56 4.00 0 -4 4 161.28 4.50 0 -4 4 165.07 4.52 0 -4 4 165.77 4.12 0 -4 4 167.93 3.83 0 -4 4 166.74 4.45 0 -4 4 158.24 4.17 -1 5 -5 11.57 1.28 1 -5 5 10.13 1.45 1 -5 5 10.77 1.30 1 -5 5 12.59 1.65 1 -5 5 13.94 1.63 1 -5 5 10.41 1.17 1 -5 5 8.49 1.38 -2 6 -6 3.91 0.90 2 -6 6 4.95 1.25 2 -6 6 2.89 0.81 2 -6 6 4.06 1.08 2 -6 6 1.98 1.01 2 -6 6 3.82 1.07 3 -7 7 0.13 0.87 3 -7 7 0.60 0.65 3 -7 7 -0.29 0.78 3 -7 7 2.08 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54.48 2.47 6 -2 0 54.24 2.38 -7 3 -1 40.49 2.36 -7 3 -1 39.97 2.07 -7 3 -1 37.37 2.06 7 -3 1 37.52 2.03 7 -3 1 36.22 1.61 7 -3 1 35.40 2.09 7 -3 1 38.73 2.20 7 -3 1 37.23 1.78 -8 4 -2 5.95 1.21 -8 4 -2 6.67 1.34 8 -4 2 5.46 1.23 8 -4 2 9.32 1.31 8 -4 2 6.08 1.28 8 -4 2 6.23 1.31 -9 5 -3 33.86 2.17 -9 5 -3 30.30 2.38 9 -5 3 33.44 2.39 9 -5 3 33.68 2.12 9 -5 3 32.96 2.42 -10 6 -4 8.77 1.75 -10 6 -4 9.61 1.52 10 -6 4 8.56 1.53 10 -6 4 9.44 1.89 10 -6 4 10.75 1.93 -11 7 -5 1.07 1.09 11 -7 5 1.52 1.12 4 -6 8 1.11 0.77 3 -5 7 16.70 2.21 3 -5 7 12.87 1.43 3 -5 7 19.45 2.33 3 -5 7 16.19 1.89 2 -4 6 4.35 0.88 2 -4 6 4.79 0.86 2 -4 6 5.27 1.18 2 -4 6 6.29 1.26 2 -4 6 6.59 1.13 2 -4 6 6.38 1.24 1 -3 5 36.74 1.58 1 -3 5 37.05 1.82 1 -3 5 30.57 1.65 1 -3 5 31.23 1.97 1 -3 5 33.90 1.96 1 -3 5 35.45 2.03 -1 3 -5 32.32 1.52 0 -2 4 1.92 0.59 0 -2 4 1.39 0.64 0 -2 4 1.92 0.63 0 -2 4 2.76 0.75 0 -2 4 1.97 0.46 0 -2 4 1.27 0.54 0 2 -4 1.51 0.55 0 2 -4 1.82 0.54 0 2 -4 2.33 0.52 -1 -1 3 71.23 1.96 -1 -1 3 74.09 2.32 -1 -1 3 66.12 2.21 -1 -1 3 66.76 2.35 -1 -1 3 73.54 2.48 1 1 -3 70.85 2.24 1 1 -3 69.25 2.18 1 1 -3 71.18 1.93 -2 0 2 130.84 2.88 -2 0 2 130.09 3.23 -2 0 2 130.11 3.18 -2 0 2 130.52 3.30 -2 0 2 124.08 3.04 -2 0 2 123.80 3.12 -2 0 2 133.46 3.12 2 0 -2 134.46 3.33 -3 1 1 335.70 6.31 -3 1 1 328.08 6.14 -3 1 1 331.12 6.26 -3 1 1 330.87 6.05 -3 1 1 341.57 5.90 -3 1 1 329.24 5.96 3 -1 -1 334.87 6.44 3 -1 -1 332.18 5.30 3 -1 -1 327.45 6.37 -4 2 0 70.28 1.72 -4 2 0 72.38 2.26 -4 2 0 70.52 2.40 -4 2 0 68.54 2.28 -4 2 0 69.43 1.94 -4 2 0 70.62 2.39 4 -2 0 65.40 1.77 4 -2 0 63.60 2.32 4 -2 0 67.08 2.23 -5 3 -1 17.03 1.19 -5 3 -1 18.85 1.27 -5 3 -1 16.96 1.68 5 -3 1 15.28 0.95 5 -3 1 13.36 0.96 5 -3 1 18.14 1.62 5 -3 1 15.89 1.26 -6 4 -2 1.69 0.71 -6 4 -2 4.14 0.82 -6 4 -2 2.90 0.78 6 -4 2 1.64 0.70 6 -4 2 3.93 0.71 6 -4 2 4.85 0.93 6 -4 2 2.78 0.83 -7 5 -3 115.03 3.59 -7 5 -3 102.94 3.87 7 -5 3 104.21 3.30 7 -5 3 108.75 3.97 7 -5 3 106.36 3.88 7 -5 3 108.57 3.45 -8 6 -4 6.18 1.34 -8 6 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272.61 4.63 1 -1 -1 267.42 4.67 -2 2 0 121.83 2.62 -2 2 0 123.24 2.44 -2 2 0 121.37 2.22 -2 2 0 124.96 2.79 -2 2 0 118.71 2.60 -2 2 0 118.48 2.69 2 -2 0 125.04 2.71 2 -2 0 125.71 2.80 2 -2 0 124.29 2.31 -3 3 -1 0.82 0.41 -3 3 -1 1.35 0.47 -3 3 -1 1.52 0.51 3 -3 1 1.44 0.48 3 -3 1 1.13 0.43 3 -3 1 2.25 0.59 3 -3 1 1.24 0.38 -4 4 -2 165.24 3.86 -4 4 -2 176.52 3.84 -4 4 -2 172.41 4.21 4 -4 2 176.07 4.18 4 -4 2 169.68 3.88 4 -4 2 169.33 4.25 4 -4 2 157.92 3.76 4 -4 2 163.74 3.80 -5 5 -3 127.47 3.43 -5 5 -3 125.73 3.79 5 -5 3 124.12 3.20 5 -5 3 129.02 3.48 5 -5 3 130.84 3.98 5 -5 3 130.73 3.65 5 -5 3 132.97 3.93 -6 6 -4 3.65 0.86 -6 6 -4 4.19 1.04 6 -6 4 3.77 0.96 6 -6 4 3.87 0.96 6 -6 4 4.57 1.08 6 -6 4 1.90 0.62 -7 7 -5 6.10 1.16 -7 7 -5 7.15 1.43 7 -7 5 4.83 1.26 7 -7 5 4.97 1.06 7 -7 5 7.36 1.40 -8 8 -6 6.15 1.24 8 -8 6 7.70 1.75 8 -8 6 7.02 1.50 7 -5 7 2.00 1.02 6 -4 6 22.20 2.34 6 -4 6 25.25 2.06 -6 4 -6 20.04 1.37 5 -3 5 3.56 0.93 5 -3 5 1.67 0.80 5 -3 5 3.78 0.91 5 -3 5 3.48 0.67 -5 3 -5 3.74 0.68 -5 3 -5 3.46 0.82 4 -2 4 7.89 1.05 4 -2 4 7.71 1.13 4 -2 4 6.89 0.76 4 -2 4 8.11 1.10 4 -2 4 7.89 0.87 -4 2 -4 8.46 0.65 -4 2 -4 8.62 1.05 -4 2 -4 8.57 0.70 3 -1 3 80.03 2.51 3 -1 3 79.19 2.46 3 -1 3 81.47 2.08 3 -1 3 80.89 2.37 3 -1 3 82.69 1.82 3 -1 3 78.14 2.29 -3 1 -3 86.00 2.32 -3 1 -3 86.70 1.92 -3 1 -3 86.67 1.86 2 0 2 126.66 2.67 2 0 2 128.28 2.39 2 0 2 127.90 2.89 2 0 2 127.70 2.53 2 0 2 131.78 2.93 2 0 2 127.87 2.69 -2 0 -2 130.49 2.15 -2 0 -2 132.21 2.21 -2 0 -2 130.77 2.68 1 1 1 271.03 4.50 1 1 1 271.55 4.16 1 1 1 267.35 4.28 1 1 1 266.51 4.28 1 1 1 263.82 4.23 1 1 1 270.44 4.49 0 2 0 250.08 4.17 0 2 0 253.49 4.10 0 2 0 255.34 4.01 0 -2 0 246.46 3.99 0 -2 0 253.33 4.05 0 -2 0 256.90 4.08 -1 3 -1 779.59 12.00 -1 3 -1 776.64 12.06 -1 3 -1 763.66 11.97 -1 3 -1 766.61 11.88 1 -3 1 747.38 11.58 1 -3 1 758.23 11.55 1 -3 1 762.73 11.87 1 -3 1 754.00 11.92 1 -3 1 753.32 11.72 -2 4 -2 133.13 3.11 -2 4 -2 131.12 2.88 -2 4 -2 131.26 3.09 -2 4 -2 128.65 2.99 2 -4 2 128.91 3.17 2 -4 2 129.67 3.01 2 -4 2 131.76 3.29 2 -4 2 128.66 2.97 2 -4 2 132.60 3.04 -3 5 -3 44.83 1.67 -3 5 -3 44.57 1.76 -3 5 -3 46.38 1.77 -3 5 -3 45.52 1.89 3 -5 3 44.42 2.03 3 -5 3 45.11 1.78 3 -5 3 44.93 1.84 3 -5 3 45.85 1.41 3 -5 3 43.40 1.93 3 -5 3 45.74 1.84 -4 6 -4 20.20 1.40 -4 6 -4 21.11 1.50 4 -6 4 22.10 1.44 4 -6 4 21.27 1.55 4 -6 4 23.18 1.73 4 -6 4 20.59 1.48 4 -6 4 19.23 1.36 -5 7 -5 16.58 1.39 -5 7 -5 13.40 1.66 5 -7 5 17.83 1.83 5 -7 5 16.58 2.01 5 -7 5 15.49 2.01 5 -7 5 15.88 1.80 -6 8 -6 13.93 1.86 -6 8 -6 12.02 1.61 6 -8 6 15.60 2.17 6 -8 6 12.01 1.75 6 -8 6 16.24 2.15 6 -8 6 12.70 1.77 7 -9 7 0.51 0.83 7 -9 7 1.10 1.02 7 -9 7 1.44 1.03 8 -4 6 9.65 1.67 -8 4 -6 10.07 1.29 7 -3 5 2.32 0.89 7 -3 5 2.41 1.01 -7 3 -5 2.46 0.66 -7 3 -5 2.47 0.93 6 -2 4 55.25 1.92 6 -2 4 54.30 2.59 6 -2 4 53.66 2.49 6 -2 4 51.55 2.36 -6 2 -4 53.92 2.38 -6 2 -4 56.56 1.94 5 -1 3 9.71 0.94 5 -1 3 11.62 1.16 5 -1 3 8.76 0.71 5 -1 3 8.41 1.09 5 -1 3 12.05 1.38 5 -1 3 10.34 0.76 -5 1 -3 9.08 1.10 -5 1 -3 8.31 0.71 4 0 2 38.09 1.62 4 0 2 36.28 1.64 4 0 2 38.87 1.30 4 0 2 35.05 1.47 4 0 2 37.66 1.14 4 0 2 37.64 1.26 -4 0 -2 40.42 1.71 -4 0 -2 40.06 1.32 3 1 1 322.64 6.03 3 1 1 339.83 5.67 3 1 1 335.00 5.72 3 1 1 334.47 6.00 3 1 1 340.46 5.04 3 1 1 333.26 5.87 -3 -1 -1 338.58 5.71 -3 -1 -1 349.89 5.79 2 2 0 116.71 2.37 2 2 0 117.95 2.54 -2 -2 0 121.64 2.52 -2 -2 0 123.82 2.61 -2 -2 0 123.39 2.16 -2 -2 0 119.96 2.33 1 3 -1 755.15 12.18 1 3 -1 775.09 11.98 -1 -3 1 789.65 12.30 -1 -3 1 785.55 12.35 -1 -3 1 775.69 12.38 -1 -3 1 784.39 12.38 -1 -3 1 778.90 12.12 -1 -3 1 791.55 12.26 0 4 -2 329.01 6.09 0 4 -2 318.79 5.85 0 -4 2 336.80 5.56 0 -4 2 332.55 5.82 0 -4 2 332.20 6.30 0 -4 2 331.27 6.21 0 -4 2 338.16 6.33 0 -4 2 338.60 6.05 0 -4 2 340.68 6.34 -1 5 -3 65.25 2.20 -1 5 -3 63.64 2.06 -1 5 -3 60.52 1.95 -1 5 -3 60.39 2.06 1 -5 3 64.79 2.01 1 -5 3 62.62 1.89 1 -5 3 62.68 2.30 1 -5 3 61.64 2.34 1 -5 3 63.53 2.33 1 -5 3 63.34 2.19 1 -5 3 58.66 1.83 -2 6 -4 61.16 2.32 -2 6 -4 57.16 2.25 -2 6 -4 60.20 2.26 2 -6 4 60.42 2.06 2 -6 4 68.64 2.80 2 -6 4 61.83 2.41 2 -6 4 61.09 2.56 2 -6 4 56.63 2.55 2 -6 4 61.23 2.21 2 -6 4 65.48 2.17 -3 7 -5 6.43 1.10 -3 7 -5 8.13 1.20 3 -7 5 8.04 1.40 3 -7 5 8.07 1.38 3 -7 5 6.93 1.28 3 -7 5 7.70 1.15 3 -7 5 6.98 1.02 3 -7 5 8.53 1.29 -4 8 -6 29.64 2.03 4 -8 6 29.31 1.86 4 -8 6 28.92 1.98 4 -8 6 36.26 2.50 4 -8 6 26.21 1.99 4 -8 6 31.18 2.45 5 -9 7 1.78 1.14 5 -9 7 2.78 1.34 5 -9 7 3.62 1.07 5 -9 7 1.96 1.05 10 -4 6 0.11 0.92 9 -3 5 8.58 1.69 -9 3 -5 10.80 1.36 8 -2 4 58.58 2.88 8 -2 4 61.98 2.85 8 -2 4 63.65 2.41 8 -2 4 63.34 3.18 -8 2 -4 76.56 3.28 -8 2 -4 69.48 2.61 7 -1 3 -0.21 0.45 7 -1 3 0.62 0.52 7 -1 3 0.32 0.63 7 -1 3 0.98 0.61 -7 1 -3 0.49 0.58 -7 1 -3 0.95 0.49 6 0 2 37.07 1.92 6 0 2 35.34 1.79 6 0 2 38.56 1.79 6 0 2 34.93 1.11 6 0 2 32.06 1.54 6 0 2 33.69 1.60 -6 0 -2 36.55 2.00 -6 0 -2 37.39 1.64 5 1 1 278.92 4.46 5 1 1 273.34 5.16 5 1 1 273.50 5.65 5 1 1 278.31 5.91 5 1 1 278.00 5.77 5 1 1 268.09 5.60 5 1 1 282.56 5.60 -5 -1 -1 277.32 5.53 -5 -1 -1 283.79 4.86 -5 -1 -1 281.19 4.45 -5 -1 -1 282.65 5.61 4 2 0 62.15 2.15 4 2 0 65.90 2.19 4 2 0 62.57 1.89 -4 -2 0 69.04 2.11 -4 -2 0 67.71 2.15 -4 -2 0 65.03 2.21 -4 -2 0 66.55 1.76 -4 -2 0 66.66 1.57 3 3 -1 0.58 0.45 3 3 -1 0.96 0.56 -3 -3 1 2.63 0.73 -3 -3 1 0.93 0.50 -3 -3 1 1.36 0.43 -3 -3 1 1.38 0.49 2 4 -2 137.40 3.62 -2 -4 2 134.32 3.16 -2 -4 2 128.31 3.28 -2 -4 2 133.13 3.37 -2 -4 2 130.38 3.50 -2 -4 2 136.58 3.50 -2 -4 2 134.34 3.32 1 5 -3 63.38 2.18 1 5 -3 65.11 2.43 -1 -5 3 63.85 2.24 -1 -5 3 62.27 2.50 -1 -5 3 58.76 2.33 -1 -5 3 65.33 2.08 -1 -5 3 62.24 2.38 -1 -5 3 60.76 2.39 -1 -5 3 60.89 2.20 0 6 -4 187.04 4.79 0 6 -4 187.54 4.50 0 -6 4 191.35 4.76 0 -6 4 197.33 5.16 0 -6 4 198.16 5.24 0 -6 4 188.75 5.21 0 -6 4 191.51 4.52 0 -6 4 192.09 4.89 -1 7 -5 156.63 4.35 1 -7 5 150.63 4.49 1 -7 5 153.23 4.14 1 -7 5 149.65 4.20 1 -7 5 151.77 4.88 1 -7 5 148.41 4.83 1 -7 5 156.01 4.90 -2 8 -6 2.43 0.91 2 -8 6 1.47 1.02 2 -8 6 3.63 1.17 2 -8 6 1.18 0.86 2 -8 6 1.78 0.90 2 -8 6 1.00 0.77 3 -9 7 2.04 0.92 3 -9 7 1.13 1.05 3 -9 7 2.66 1.27 3 -9 7 2.39 1.17 4 -10 8 1.65 1.34 4 -10 8 1.77 1.23 4 -10 8 0.84 0.90 11 -3 5 5.11 1.50 -11 3 -5 7.06 1.22 10 -2 4 8.05 1.61 10 -2 4 8.75 1.53 10 -2 4 8.73 1.41 -10 2 -4 10.13 1.47 -10 2 -4 6.04 1.46 9 -1 3 6.25 1.22 9 -1 3 7.88 1.54 9 -1 3 7.20 1.35 9 -1 3 7.55 1.31 -9 1 -3 8.44 1.29 -9 1 -3 7.52 1.54 8 0 2 8.69 1.38 8 0 2 7.89 1.26 8 0 2 8.94 1.34 8 0 2 10.39 1.51 -8 0 -2 10.74 1.39 -8 0 -2 11.21 1.74 7 1 1 66.55 2.78 7 1 1 66.98 2.55 7 1 1 68.75 2.77 7 1 1 71.79 2.75 -7 -1 -1 69.00 2.66 -7 -1 -1 71.03 1.94 -7 -1 -1 67.89 2.56 6 2 0 54.13 2.40 6 2 0 56.91 2.08 6 2 0 57.47 2.45 -6 -2 0 52.43 2.22 -6 -2 0 59.86 2.49 -6 -2 0 55.46 1.82 -6 -2 0 57.78 2.29 -6 -2 0 55.32 1.87 5 3 -1 16.94 1.80 5 3 -1 16.48 1.02 -5 -3 1 15.55 0.96 -5 -3 1 15.44 1.05 -5 -3 1 12.75 1.44 -5 -3 1 15.81 1.54 -5 -3 1 15.33 1.06 -5 -3 1 13.41 1.18 4 4 -2 171.24 4.63 4 4 -2 159.19 4.31 -4 -4 2 172.18 4.57 -4 -4 2 171.72 4.12 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1.35 -10 0 -2 9.45 1.93 9 1 1 62.73 3.10 9 1 1 58.49 2.96 9 1 1 64.79 2.74 9 1 1 64.41 3.03 -9 -1 -1 64.06 3.00 8 2 0 70.76 3.18 8 2 0 67.94 2.65 8 2 0 68.96 2.98 8 2 0 69.41 3.15 -8 -2 0 69.36 3.04 -8 -2 0 69.12 3.07 -8 -2 0 68.35 2.34 7 3 -1 37.38 2.28 7 3 -1 41.89 2.41 7 3 -1 35.11 1.71 -7 -3 1 39.84 2.18 -7 -3 1 38.24 1.88 -7 -3 1 38.89 1.69 -7 -3 1 40.72 2.41 -7 -3 1 38.08 1.87 6 4 -2 1.86 0.53 6 4 -2 2.80 0.87 -6 -4 2 1.88 0.66 -6 -4 2 2.09 0.70 -6 -4 2 3.25 0.83 -6 -4 2 4.87 0.89 -6 -4 2 3.35 1.07 -6 -4 2 2.46 0.82 5 5 -3 129.38 4.20 5 5 -3 130.76 4.52 -5 -5 3 120.01 3.93 -5 -5 3 125.32 4.05 -5 -5 3 123.79 3.72 -5 -5 3 133.47 4.15 -5 -5 3 126.52 3.84 -5 -5 3 126.71 4.34 -5 -5 3 125.34 4.38 4 6 -4 17.42 2.26 4 6 -4 19.65 1.97 -4 -6 4 18.56 2.02 -4 -6 4 21.59 2.27 -4 -6 4 27.96 2.87 -4 -6 4 23.44 1.74 -4 -6 4 22.44 1.62 3 7 -5 5.80 1.17 3 7 -5 5.68 1.30 -3 -7 5 7.48 1.47 -3 -7 5 5.70 1.32 -3 -7 5 7.19 1.23 -3 -7 5 5.66 1.26 -3 -7 5 7.36 1.31 2 8 -6 1.34 0.79 -2 -8 6 2.02 0.90 -2 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10 -2 6 2.26 1.11 -10 2 -6 3.80 0.83 9 -1 5 22.79 2.63 9 -1 5 22.40 2.43 -9 1 -5 22.01 1.41 8 0 4 63.93 2.30 8 0 4 64.69 3.06 8 0 4 64.32 3.17 -8 0 -4 70.00 3.06 -8 0 -4 63.38 2.35 7 1 3 1.74 0.62 7 1 3 2.10 0.67 7 1 3 0.60 0.56 7 1 3 1.66 0.73 -7 -1 -3 1.41 0.70 -7 -1 -3 1.32 0.54 6 2 2 135.90 3.58 6 2 2 141.23 4.02 6 2 2 135.60 3.09 6 2 2 138.37 3.89 6 2 2 133.73 3.49 -6 -2 -2 144.28 3.56 5 3 1 14.63 0.89 5 3 1 12.90 1.02 5 3 1 16.20 1.12 5 3 1 12.54 1.01 5 3 1 13.52 1.04 -5 -3 -1 14.99 1.05 -5 -3 -1 15.52 0.65 -5 -3 -1 14.67 1.01 4 4 0 49.25 1.97 4 4 0 49.62 1.67 4 4 0 45.62 1.71 -4 -4 0 49.46 1.32 -4 -4 0 45.32 1.78 -4 -4 0 45.51 1.89 -4 -4 0 46.85 1.58 3 5 -1 3.64 0.74 3 5 -1 5.35 0.85 -3 -5 1 3.42 0.67 -3 -5 1 4.49 0.78 -3 -5 1 5.03 0.69 -3 -5 1 4.14 0.78 2 6 -2 135.49 3.52 2 6 -2 134.20 3.79 -2 -6 2 144.75 3.85 -2 -6 2 145.01 3.71 -2 -6 2 143.47 3.80 -2 -6 2 151.01 3.74 -2 -6 2 143.22 3.50 -2 -6 2 141.99 3.91 1 7 -3 22.61 1.41 1 7 -3 22.41 1.59 -1 -7 3 21.82 1.38 -1 -7 3 22.91 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2.51 0.67 6 4 0 1.02 0.51 6 4 0 1.89 0.66 6 4 0 0.12 0.45 -6 -4 0 1.98 0.72 -6 -4 0 2.01 0.56 -6 -4 0 1.55 0.40 -6 -4 0 1.68 0.63 -6 -4 0 1.54 0.61 5 5 -1 36.63 1.61 5 5 -1 35.09 2.00 -5 -5 1 36.96 1.98 -5 -5 1 36.77 2.03 -5 -5 1 37.14 1.50 -5 -5 1 38.48 1.91 -5 -5 1 36.95 1.73 4 6 -2 29.26 1.70 4 6 -2 29.38 1.90 -4 -6 2 34.53 1.87 -4 -6 2 29.92 1.89 -4 -6 2 30.63 1.76 -4 -6 2 29.08 1.55 -4 -6 2 32.48 1.68 3 7 -3 40.09 2.03 3 7 -3 38.06 2.23 -3 -7 3 42.25 2.12 -3 -7 3 39.47 2.04 -3 -7 3 41.74 2.26 -3 -7 3 39.44 1.90 -3 -7 3 43.80 2.11 -3 -7 3 40.28 2.23 2 8 -4 10.71 1.40 2 8 -4 12.28 1.67 -2 -8 4 11.18 1.64 -2 -8 4 14.52 1.65 -2 -8 4 15.60 1.69 -2 -8 4 15.65 1.82 -2 -8 4 13.35 1.76 1 9 -5 17.07 1.86 -1 -9 5 16.58 2.01 -1 -9 5 16.36 2.08 -1 -9 5 18.95 1.93 -1 -9 5 20.85 2.38 -1 -9 5 17.22 2.11 -1 -9 5 16.05 1.79 0 10 -6 21.98 2.30 0 -10 6 16.22 2.17 0 -10 6 20.99 1.78 0 -10 6 25.59 2.89 0 -10 6 21.43 2.15 0 -10 6 20.58 2.56 0 -10 6 26.80 2.88 -1 11 -7 2.67 1.10 1 -11 7 3.73 1.37 1 -11 7 2.00 0.87 1 -11 7 3.26 1.36 1 -11 7 3.29 1.37 1 -11 7 4.63 1.53 12 0 4 13.18 2.10 12 0 4 10.08 1.92 -12 0 -4 12.87 1.85 11 1 3 18.45 2.41 11 1 3 14.85 2.07 11 1 3 16.12 2.04 -11 -1 -3 15.42 1.94 -11 -1 -3 20.55 2.61 10 2 2 20.38 2.38 10 2 2 24.47 1.95 10 2 2 22.85 2.39 10 2 2 17.04 2.02 -10 -2 -2 24.12 2.78 -10 -2 -2 21.47 1.83 9 3 1 10.19 1.59 9 3 1 7.56 1.36 9 3 1 5.67 1.10 9 3 1 8.53 1.62 -9 -3 -1 9.60 1.55 8 4 0 13.21 1.61 8 4 0 15.99 1.91 8 4 0 17.38 1.83 8 4 0 13.29 1.85 -8 -4 0 18.88 2.01 -8 -4 0 15.89 1.82 -8 -4 0 15.17 1.20 7 5 -1 95.23 3.78 7 5 -1 92.87 3.71 7 5 -1 91.07 3.07 -7 -5 1 92.44 3.14 -7 -5 1 91.72 3.06 -7 -5 1 94.66 3.70 -7 -5 1 92.50 3.51 -7 -5 1 93.68 2.71 6 6 -2 10.12 1.65 -6 -6 2 17.34 1.59 -6 -6 2 11.83 1.70 -6 -6 2 16.60 2.21 -6 -6 2 17.03 1.92 -6 -6 2 15.76 1.69 -6 -6 2 16.30 1.74 5 7 -3 41.38 2.56 5 7 -3 35.99 2.26 -5 -7 3 38.08 2.29 -5 -7 3 42.16 2.26 -5 -7 3 38.20 2.07 -5 -7 3 38.87 2.31 -5 -7 3 38.36 2.45 4 8 -4 28.19 2.04 4 8 -4 30.21 2.32 -4 -8 4 27.98 1.98 -4 -8 4 31.73 2.18 -4 -8 4 29.83 2.29 -4 -8 4 28.63 2.16 3 9 -5 0.56 0.78 3 9 -5 1.14 0.76 -3 -9 5 1.05 0.71 -3 -9 5 0.31 0.69 -3 -9 5 0.83 0.80 -3 -9 5 2.22 0.89 -3 -9 5 0.46 0.82 2 10 -6 1.53 0.86 -2 -10 6 1.42 1.03 -2 -10 6 2.32 1.08 -2 -10 6 3.55 1.06 -2 -10 6 2.63 1.08 -2 -10 6 2.21 1.04 1 11 -7 2.80 1.13 -1 -11 7 4.23 1.38 -1 -11 7 1.99 1.23 -1 -11 7 2.78 1.21 -1 -11 7 1.41 0.94 -1 -11 7 2.27 0.99 0 -12 8 4.28 1.46 0 -12 8 7.22 2.01 13 1 3 18.75 2.62 13 1 3 21.62 2.65 -13 -1 -3 21.98 3.03 12 2 2 10.55 2.01 12 2 2 12.62 1.91 12 2 2 12.08 2.17 -12 -2 -2 9.33 1.99 -12 -2 -2 15.77 2.23 11 3 1 2.59 1.02 11 3 1 2.78 1.01 11 3 1 3.05 1.11 11 3 1 4.97 1.48 -11 -3 -1 1.23 0.88 10 4 0 46.47 2.52 10 4 0 44.10 2.87 10 4 0 46.69 2.98 10 4 0 41.20 2.58 -10 -4 0 47.06 2.87 9 5 -1 31.60 2.09 9 5 -1 32.80 2.47 9 5 -1 31.33 2.47 9 5 -1 32.83 1.97 -9 -5 1 29.20 2.17 -9 -5 1 27.24 1.82 -9 -5 1 30.86 2.47 8 6 -2 8.50 1.27 8 6 -2 8.33 1.81 -8 -6 2 7.69 1.32 -8 -6 2 6.87 1.21 -8 -6 2 5.89 1.29 -8 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12.16 1.85 -9 -7 3 10.36 1.73 8 8 -4 15.12 2.67 -8 -8 4 14.05 2.00 -8 -8 4 16.47 2.06 -8 -8 4 11.77 1.99 -8 -8 4 15.70 2.73 7 9 -5 7.01 1.86 -7 -9 5 4.05 1.28 -7 -9 5 3.44 1.30 -7 -9 5 5.74 1.55 -7 -9 5 5.82 1.41 -7 -9 5 6.51 1.48 6 10 -6 1.32 0.97 -6 -10 6 1.62 1.18 -6 -10 6 0.50 0.86 -6 -10 6 0.54 0.95 -6 -10 6 1.46 1.07 -6 -10 6 1.35 0.98 5 11 -7 4.23 1.49 -5 -11 7 3.55 1.23 -5 -11 7 1.77 1.24 -5 -11 7 1.91 1.27 -5 -11 7 1.80 1.24 -5 -11 7 2.90 1.34 13 5 -1 11.45 2.45 13 5 -1 10.43 2.31 13 5 -1 10.93 2.02 -13 -5 1 10.00 2.21 12 6 -2 26.39 3.37 12 6 -2 29.61 3.66 11 7 -3 12.62 2.53 11 7 -3 8.45 2.13 -11 -7 3 8.53 1.65 10 8 -4 17.88 3.32 -10 -8 4 10.03 1.82 -10 -8 4 14.90 2.28 -10 -8 4 14.69 2.49 9 9 -5 5.94 1.95 -9 -9 5 2.87 1.33 -9 -9 5 1.40 1.20 -9 -9 5 3.25 1.24 -9 -9 5 3.15 1.29 -8 -10 6 0.20 0.88 -8 -10 6 0.33 1.02 -8 -10 6 0.37 1.01 -8 -10 6 -0.09 1.14 -9 -1 7 4.21 1.59 -9 -1 7 2.53 1.27 -9 -1 7 5.65 1.73 -9 -1 7 3.91 1.45 -10 0 6 12.20 2.19 -10 0 6 10.48 2.09 -10 0 6 15.37 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12.83 2.14 -1 -3 9 16.83 2.69 -1 -3 9 8.93 1.56 -1 -3 9 14.01 2.33 -1 -3 9 11.78 2.21 -2 -2 8 4.49 1.48 -2 -2 8 2.57 1.25 -2 -2 8 3.64 1.06 -2 -2 8 3.18 1.03 -2 -2 8 4.13 1.29 -2 -2 8 3.39 1.37 -3 -1 7 5.64 1.46 -3 -1 7 9.36 1.81 -3 -1 7 6.76 1.64 -3 -1 7 6.43 1.42 -3 -1 7 8.25 1.41 -3 -1 7 9.80 1.64 -4 0 6 29.20 2.00 -4 0 6 32.98 2.45 -4 0 6 31.76 2.23 -4 0 6 32.43 2.34 -4 0 6 34.28 2.59 -4 0 6 35.00 2.63 -5 1 5 18.41 2.23 -5 1 5 19.87 2.23 -5 1 5 19.54 2.34 -5 1 5 15.05 2.18 -5 1 5 19.18 2.07 -5 1 5 13.39 1.79 5 -1 -5 14.99 1.98 -6 2 4 60.29 3.03 -6 2 4 57.47 3.02 -6 2 4 53.88 2.99 -6 2 4 57.74 3.34 -6 2 4 58.75 2.72 -6 2 4 57.08 2.73 6 -2 -4 59.41 3.25 6 -2 -4 59.96 3.15 -7 3 3 33.53 2.21 -7 3 3 36.37 2.72 -7 3 3 36.62 2.43 -7 3 3 39.03 2.17 7 -3 -3 36.76 2.51 7 -3 -3 31.63 2.44 -8 4 2 8.40 1.58 -8 4 2 8.15 1.91 -8 4 2 3.72 1.14 -8 4 2 7.32 1.41 -8 4 2 5.33 1.25 -8 4 2 5.55 1.06 8 -4 -2 3.79 1.24 8 -4 -2 6.00 1.31 -9 5 1 33.87 2.52 -9 5 1 31.49 2.57 -9 5 1 35.35 2.53 -9 5 1 33.99 2.05 9 -5 -1 30.17 2.36 9 -5 -1 29.09 2.95 -10 6 0 1.23 0.95 -10 6 0 1.36 0.98 10 -6 0 1.52 1.00 10 -6 0 1.22 1.01 -11 7 -1 31.03 2.53 -11 7 -1 26.72 3.06 11 -7 1 26.46 2.94 11 -7 1 21.68 2.83 11 -7 1 27.93 2.90 -12 8 -2 5.86 1.55 -12 8 -2 5.43 1.64 12 -8 2 5.98 1.58 12 -8 2 7.71 1.78 12 -8 2 6.38 1.69 1 -3 9 10.72 1.47 1 -3 9 11.97 2.27 1 -3 9 10.46 1.60 0 -2 8 11.94 1.57 0 -2 8 12.72 1.68 0 -2 8 11.73 1.74 0 -2 8 14.36 2.23 0 -2 8 14.36 2.03 0 -2 8 16.93 2.33 -1 -1 7 4.45 1.33 -1 -1 7 7.36 1.43 -1 -1 7 6.35 1.39 -1 -1 7 6.59 1.55 -1 -1 7 6.41 1.22 -1 -1 7 6.05 1.15 -2 0 6 84.47 3.77 -2 0 6 70.63 3.19 -2 0 6 78.99 3.43 -2 0 6 78.86 3.23 -2 0 6 75.81 2.87 -2 0 6 73.87 3.48 -3 1 5 9.09 1.50 -3 1 5 9.39 1.54 -3 1 5 10.75 1.48 -3 1 5 10.77 1.29 -3 1 5 9.82 1.57 -3 1 5 9.71 1.44 3 -1 -5 12.43 1.67 -4 2 4 6.03 1.16 -4 2 4 6.55 1.19 -4 2 4 5.02 1.22 -4 2 4 4.96 0.96 -4 2 4 6.23 1.17 -4 2 4 8.56 1.28 4 -2 -4 7.47 1.27 -5 3 3 9.62 1.37 -5 3 3 7.36 1.13 -5 3 3 7.44 1.10 -5 3 3 8.63 1.29 -5 3 3 8.52 1.26 -5 3 3 10.96 1.82 -5 3 3 8.08 1.36 5 -3 -3 5.18 1.15 5 -3 -3 11.35 1.71 -6 4 2 2.72 0.87 -6 4 2 3.97 1.04 -6 4 2 3.79 0.93 -6 4 2 5.53 0.96 -6 4 2 4.41 1.00 -6 4 2 2.04 0.81 6 -4 -2 3.85 1.08 6 -4 -2 1.73 0.86 -7 5 1 87.63 3.54 -7 5 1 98.99 3.73 -7 5 1 97.27 2.90 -7 5 1 99.62 4.04 -7 5 1 94.21 3.77 -7 5 1 99.34 3.34 7 -5 -1 84.91 3.48 7 -5 -1 87.64 3.65 -8 6 0 67.68 3.40 -8 6 0 71.70 3.36 -8 6 0 63.63 3.10 8 -6 0 54.06 2.98 8 -6 0 58.99 2.97 -9 7 -1 11.57 1.88 -9 7 -1 10.92 1.72 9 -7 1 11.48 1.80 9 -7 1 14.04 1.88 9 -7 1 12.01 1.88 9 -7 1 13.05 1.58 -10 8 -2 9.65 1.81 -10 8 -2 3.95 1.31 10 -8 2 7.30 1.69 10 -8 2 5.98 1.49 10 -8 2 5.56 1.41 -11 9 -3 2.70 1.23 -11 9 -3 2.52 1.09 11 -9 3 2.52 1.15 11 -9 3 2.85 1.19 11 -9 3 2.24 1.16 3 -3 9 2.55 0.90 2 -2 8 4.06 0.90 2 -2 8 4.23 0.85 2 -2 8 4.51 1.41 1 -1 7 4.96 1.32 1 -1 7 6.76 1.37 1 -1 7 7.04 1.14 1 -1 7 7.32 1.31 1 -1 7 8.33 1.40 1 -1 7 4.01 0.84 0 0 6 50.57 2.00 0 0 6 54.78 2.31 0 0 6 48.04 2.37 0 0 6 47.04 2.41 0 0 6 48.50 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2.87 0.74 -3 5 1 6.21 0.93 -3 5 1 2.66 0.66 -3 5 1 4.08 0.76 3 -5 -1 4.47 0.79 3 -5 -1 4.63 0.84 -4 6 0 3.70 0.80 -4 6 0 3.17 0.83 -4 6 0 2.23 0.65 4 -6 0 2.06 0.66 4 -6 0 2.27 0.68 -5 7 -1 4.37 0.89 -5 7 -1 5.33 1.05 -5 7 -1 3.77 1.00 5 -7 1 4.56 0.78 5 -7 1 3.38 0.86 5 -7 1 5.59 1.04 5 -7 1 5.22 0.90 -6 8 -2 40.63 2.15 -6 8 -2 37.60 2.18 -6 8 -2 39.06 2.27 6 -8 2 34.26 2.06 6 -8 2 37.08 2.10 6 -8 2 37.35 2.05 6 -8 2 37.20 2.31 -7 9 -3 11.75 1.64 -7 9 -3 18.27 2.03 7 -9 3 18.54 1.98 7 -9 3 20.13 2.19 7 -9 3 17.27 2.12 7 -9 3 18.03 1.92 -8 10 -4 2.66 1.08 -8 10 -4 0.16 0.69 8 -10 4 0.47 0.73 8 -10 4 0.45 0.74 8 -10 4 0.71 0.81 8 -10 4 3.38 1.13 -9 11 -5 7.83 1.65 -9 11 -5 4.08 1.36 9 -11 5 4.63 1.29 9 -11 5 5.23 1.57 9 -11 5 5.86 1.42 4 0 6 36.60 2.17 3 1 5 10.15 1.10 3 1 5 11.25 1.37 3 1 5 9.59 1.22 3 1 5 11.08 1.21 3 1 5 11.29 1.28 -3 -1 -5 10.70 0.60 2 2 4 0.71 0.45 2 2 4 2.27 0.60 2 2 4 1.53 0.54 2 2 4 0.75 0.38 2 2 4 1.39 0.46 -2 -2 -4 0.77 0.22 -2 -2 -4 0.39 0.23 1 3 3 171.07 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0 22 0 2.70 1.16 0 22 0 2.71 1.42 0 -22 0 1.92 1.08 -1 23 -1 1.30 1.07 1 -23 1 0.52 0.90 1 -23 1 0.43 1.06 1 -23 1 -0.82 0.82 6 18 4 4.62 1.37 5 19 3 0.25 0.66 5 19 3 3.29 1.39 -5 -19 -3 1.12 0.94 4 20 2 0.32 1.01 4 20 2 0.69 0.83 -4 -20 -2 2.00 0.98 -4 -20 -2 0.19 0.98 3 21 1 -0.53 0.87 -3 -21 -1 1.05 0.91 -3 -21 -1 1.52 1.10 2 22 0 10.26 2.47 2 22 0 7.10 1.61 -2 -22 0 11.97 2.17 -2 -22 0 10.10 1.94 1 23 -1 1.06 1.04 -1 -23 1 0.73 1.09 -1 -23 1 0.11 1.08 7 19 3 1.16 1.19 6 20 2 7.32 1.82 6 20 2 5.25 1.42 -6 -20 -2 8.63 1.70 5 21 1 -0.40 1.08 5 21 1 0.05 0.84 -5 -21 -1 3.17 1.32 4 22 0 6.29 1.67 -4 -22 0 4.83 1.58 3 -19 -5 0.88 0.97 0 18 6 1.74 1.14 -1 19 5 2.17 1.26 1 -19 -5 0.01 0.81 -2 20 4 0.41 1.06 2 -20 -4 0.08 1.00 3 -21 -3 -0.53 0.85 4 -22 -2 1.97 1.12 1 19 5 1.93 1.23 -1 -19 -5 0.49 0.74 0 20 4 3.22 1.34 0 -20 -4 3.40 1.04 -1 21 3 7.80 1.86 1 -21 -3 9.88 1.87 1 -21 -3 9.39 1.87 2 -22 -2 3.13 1.26 3 19 5 0.79 1.02 2 20 4 -0.15 1.05 -2 -20 -4 0.76 0.81 1 21 3 8.68 2.13 1 21 3 8.32 1.92 -1 -21 -3 9.88 1.79 0 22 2 3.62 1.64 0 22 2 0.57 1.16 0 -22 -2 2.42 1.12 0 -22 -2 1.84 1.03 1 -23 -1 0.73 0.99 4 20 4 1.94 1.09 4 20 4 -0.78 0.90 3 21 3 0.83 1.06 3 21 3 0.45 0.85 -3 -21 -3 1.22 0.88 2 22 2 0.87 1.26 2 22 2 3.22 1.18 -2 -22 -2 2.29 1.16 -1 -23 -1 0.28 0.88 4 22 2 1.08 0.91 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 13239 # start Validation Reply Form _vrf_CHEMW03_X8_15165 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The PNH2 moiety is one-quarter occupied, disordered across two mirror planes, and is modelled in part -1. This seems to have thrown off calculation of molecular weight. ; _vrf_PLAT073_X8_15165 ; PROBLEM: H-atoms ref, but _hydrogen_treatment reported as constr Check RESPONSE: The hydrogen atoms lie on a mirror plane and are 50/50 disordered across a second mirror plane. This particular geometry prevented use of AFIX commands to position hydrogens at calculated positions. Instead, they were constrained to lie on the mirror plane, and held at appropriate distances using DFIX restraints. Without fail, allowing the hydrogen atoms to deviate from the mirror plane resulted in an unstable refinement. ; _vrf_PLAT936_X8_15165 ; PROBLEM: The Embedded .res File Includes a DAMP Command . 400.0 Report RESPONSE: The instabilities in this refinement due to the high symmetry and positional disorder required the use of a DAMP command to obtain convergence. ; # end Validation Reply Form