data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27.73 H20 B Cl0.27 Hg N3.73 P' _chemical_formula_weight 657.39 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' 'B' 'B' 0.0013 0.0007 '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' 'Hg' 'Hg' -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7352(2) _cell_length_b 9.7331(3) _cell_length_c 27.4616(8) _cell_angle_alpha 90 _cell_angle_beta 97.735(3) _cell_angle_gamma 90 _cell_volume 2578.41(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4346 _cell_measurement_theta_min 2.9610 _cell_measurement_theta_max 28.2250 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_F_000 1268 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.4194 _exptl_crystal_size_mid 0.1714 _exptl_crystal_size_min 0.0644 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 0 0 1 0.0322 -0.0000 0.0000 1.0000 0.0007 -0.0250 0.0074 0 0 -1 0.0322 0.0000 -0.0000 -1.0000 -0.0007 0.0250 -0.0074 -1 0 0 0.0669 -1.0000 0.0000 0.0000 0.0707 0.0065 -0.0190 1 0 0 0.0944 1.0000 -0.0000 -0.0000 -0.0707 -0.0065 0.0190 0 -13 9 0.1869 -0.0000 -13.0000 9.0000 0.2186 0.0428 0.9504 0 13 -9 0.2047 0.0000 13.0000 -9.0000 -0.2186 -0.0428 -0.9504 _exptl_absorpt_coefficient_mu 6.082 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_T_min 0.225 _exptl_absorpt_correction_T_max 0.687 _exptl_absorpt_correction_type 'analytical' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube Enhanced (Mo)' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Gemini E Ultra,Xcalibur,2K*2K EOS CCD detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.2705 _diffrn_reflns_number 14780 _diffrn_reflns_av_unetI/netI 0.0364 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.111 _diffrn_reflns_theta_max 29.405 _diffrn_reflns_theta_full 26.400 _diffrn_measured_fraction_theta_max 0.858 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.858 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.858 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 6109 _reflns_number_gt 4774 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrysAlisPro171.36.24, Oxford Diffraction' _computing_cell_refinement 'CrysAlisPro171.36.24, Oxford Diffraction' _computing_data_reduction 'CrysAlisPro171.36.24, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Diamond, v.2.1e (Brandenburg, 2001)' _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0204P)^2^+0.8691P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 6109 _refine_ls_number_parameters 320 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0496 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.047 _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 Hg Hg -0.01391(2) 0.05005(2) 0.30787(2) 0.04597(6) Uani 1 1 d . . . . . C1 C -0.071(3) -0.001(3) 0.3771(10) 0.064(4) Uani 0.730(12) 1 d . U P . . N1 N -0.0941(6) -0.0499(7) 0.4126(3) 0.0596(16) Uani 0.730(12) 1 d . . P . . Cl Cl -0.078(2) -0.0226(18) 0.3859(7) 0.064(4) Uani 0.270(12) 1 d . U P . . B B 0.0575(4) 0.1072(4) 0.23866(15) 0.0403(9) Uani 1 1 d . . . . . C2 C 0.1205(4) -0.0267(4) 0.21780(14) 0.0469(9) Uani 1 1 d . . . . . N2 N 0.1590(4) -0.1259(4) 0.20244(14) 0.0697(10) Uani 1 1 d . . . . . C3 C -0.0682(4) 0.1614(4) 0.20206(15) 0.0521(10) Uani 1 1 d . . . . . N3 N -0.1588(4) 0.2010(4) 0.17539(14) 0.0801(12) Uani 1 1 d . . . . . C4 C 0.1678(4) 0.2256(4) 0.25102(14) 0.0496(9) Uani 1 1 d . . . . . N4 N 0.2420(4) 0.3151(4) 0.26065(14) 0.0714(11) Uani 1 1 d . . . . . P P 0.47995(8) 0.29387(8) 0.41166(3) 0.03064(18) Uani 1 1 d . . . . . C5 C 0.5538(3) 0.4499(3) 0.39184(12) 0.0314(7) Uani 1 1 d . . . . . C6 C 0.5049(4) 0.5046(4) 0.34567(13) 0.0404(8) Uani 1 1 d . . . . . H6 H 0.4339 0.4610 0.3254 0.049 Uiso 1 1 calc R U . . . C7 C 0.5624(4) 0.6231(4) 0.33060(14) 0.0489(9) Uani 1 1 d . . . . . H7 H 0.5293 0.6601 0.3000 0.059 Uiso 1 1 calc R U . . . C8 C 0.6689(4) 0.6884(4) 0.36015(15) 0.0511(10) Uani 1 1 d . . . . . H8 H 0.7067 0.7689 0.3495 0.061 Uiso 1 1 calc R U . . . C9 C 0.7186(4) 0.6343(4) 0.40513(14) 0.0476(9) Uani 1 1 d . . . . . H9 H 0.7909 0.6779 0.4248 0.057 Uiso 1 1 calc R U . . . C10 C 0.6619(3) 0.5150(3) 0.42148(13) 0.0379(8) Uani 1 1 d . . . . . H10 H 0.6957 0.4786 0.4521 0.046 Uiso 1 1 calc R U . . . C11 C 0.5832(3) 0.2380(3) 0.46715(12) 0.0320(7) Uani 1 1 d . . . . . C12 C 0.6939(3) 0.1509(4) 0.46467(13) 0.0403(8) Uani 1 1 d . . . . . H12 H 0.7093 0.1128 0.4348 0.048 Uiso 1 1 calc R U . . . C13 C 0.7822(4) 0.1207(4) 0.50769(15) 0.0494(10) Uani 1 1 d . . . . . H13 H 0.8574 0.0626 0.5064 0.059 Uiso 1 1 calc R U . . . C14 C 0.7594(4) 0.1758(4) 0.55181(15) 0.0535(10) Uani 1 1 d . . . . . H14 H 0.8199 0.1558 0.5801 0.064 Uiso 1 1 calc R U . . . C15 C 0.6481(4) 0.2601(4) 0.55442(14) 0.0585(11) Uani 1 1 d . . . . . H15 H 0.6311 0.2952 0.5845 0.070 Uiso 1 1 calc R U . . . C16 C 0.5616(4) 0.2926(4) 0.51216(13) 0.0493(9) Uani 1 1 d . . . . . H16 H 0.4875 0.3520 0.5138 0.059 Uiso 1 1 calc R U . . . C17 C 0.3046(3) 0.3185(3) 0.42462(12) 0.0358(8) Uani 1 1 d . . . . . C18 C 0.2209(4) 0.4172(4) 0.39973(15) 0.0580(11) Uani 1 1 d . . . . . H18 H 0.2552 0.4734 0.3768 0.070 Uiso 1 1 calc R U . . . C19 C 0.0857(4) 0.4320(5) 0.40918(19) 0.0790(15) Uani 1 1 d . . . . . H19 H 0.0288 0.4982 0.3924 0.095 Uiso 1 1 calc R U . . . C20 C 0.0353(4) 0.3499(5) 0.44307(18) 0.0708(13) Uani 1 1 d . . . . . H20 H -0.0557 0.3608 0.4492 0.085 Uiso 1 1 calc R U . . . C21 C 0.1172(4) 0.2522(4) 0.46806(16) 0.0614(11) Uani 1 1 d . . . . . H21 H 0.0826 0.1975 0.4914 0.074 Uiso 1 1 calc R U . . . C22 C 0.2527(4) 0.2352(4) 0.45838(15) 0.0519(10) Uani 1 1 d . . . . . H22 H 0.3084 0.1674 0.4747 0.062 Uiso 1 1 calc R U . . . C23 C 0.4829(3) 0.1684(3) 0.36418(12) 0.0327(7) Uani 1 1 d . . . . . C24 C 0.3860(4) 0.0633(3) 0.35854(14) 0.0433(8) Uani 1 1 d . . . . . H24 H 0.3177 0.0585 0.3791 0.052 Uiso 1 1 calc R U . . . C25 C 0.3909(4) -0.0345(4) 0.32233(15) 0.0527(10) Uani 1 1 d . . . . . H25 H 0.3263 -0.1055 0.3188 0.063 Uiso 1 1 calc R U . . . C26 C 0.4904(4) -0.0269(4) 0.29173(14) 0.0488(9) Uani 1 1 d . . . . . H26 H 0.4923 -0.0922 0.2671 0.059 Uiso 1 1 calc R U . . . C27 C 0.5874(4) 0.0758(4) 0.29703(13) 0.0464(9) Uani 1 1 d . . . . . H27 H 0.6552 0.0792 0.2762 0.056 Uiso 1 1 calc R U . . . C28 C 0.5851(3) 0.1745(3) 0.33308(12) 0.0387(8) Uani 1 1 d . . . . . H28 H 0.6510 0.2442 0.3366 0.046 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 Hg 0.03964(8) 0.05504(10) 0.04409(9) -0.00162(7) 0.00877(6) 0.00092(7) C1 0.056(3) 0.067(6) 0.070(7) 0.006(5) 0.008(4) 0.004(3) N1 0.063(3) 0.068(3) 0.051(4) 0.006(3) 0.020(3) 0.006(3) Cl 0.056(3) 0.067(6) 0.070(7) 0.006(5) 0.008(4) 0.004(3) B 0.037(2) 0.042(2) 0.042(2) -0.0008(19) 0.0046(17) 0.0039(18) C2 0.044(2) 0.052(2) 0.046(2) 0.0054(19) 0.0091(17) 0.0086(18) N2 0.073(2) 0.066(2) 0.074(3) -0.002(2) 0.025(2) 0.022(2) C3 0.060(3) 0.048(2) 0.047(2) -0.0101(19) 0.0057(19) 0.015(2) N3 0.085(3) 0.085(3) 0.062(3) -0.014(2) -0.016(2) 0.041(2) C4 0.056(2) 0.054(2) 0.040(2) 0.0027(19) 0.0124(18) 0.001(2) N4 0.072(2) 0.069(2) 0.076(3) -0.001(2) 0.018(2) -0.021(2) P 0.0297(4) 0.0307(4) 0.0320(5) 0.0012(4) 0.0061(3) 0.0019(3) C5 0.0306(16) 0.0306(16) 0.0338(18) -0.0026(15) 0.0075(13) 0.0008(14) C6 0.046(2) 0.0401(18) 0.034(2) -0.0004(16) 0.0015(16) -0.0039(16) C7 0.068(3) 0.041(2) 0.038(2) 0.0064(18) 0.0074(18) -0.0028(19) C8 0.063(2) 0.042(2) 0.051(3) -0.0011(19) 0.018(2) -0.0121(19) C9 0.049(2) 0.047(2) 0.048(2) -0.0112(19) 0.0095(17) -0.0178(18) C10 0.0384(18) 0.0414(19) 0.035(2) -0.0016(16) 0.0077(15) -0.0006(15) C11 0.0309(16) 0.0311(16) 0.0345(19) 0.0016(15) 0.0061(13) 0.0050(13) C12 0.0380(18) 0.0457(19) 0.039(2) 0.0045(17) 0.0102(15) 0.0081(16) C13 0.039(2) 0.047(2) 0.063(3) 0.012(2) 0.0096(18) 0.0118(17) C14 0.054(2) 0.057(2) 0.046(3) 0.012(2) -0.0030(18) 0.004(2) C15 0.069(3) 0.069(3) 0.036(2) -0.001(2) 0.0015(19) 0.016(2) C16 0.055(2) 0.055(2) 0.038(2) -0.0001(18) 0.0083(17) 0.0190(18) C17 0.0317(17) 0.0380(18) 0.039(2) -0.0009(16) 0.0081(14) 0.0013(14) C18 0.041(2) 0.071(3) 0.064(3) 0.025(2) 0.0122(19) 0.0124(19) C19 0.040(2) 0.097(4) 0.102(4) 0.042(3) 0.015(2) 0.023(2) C20 0.030(2) 0.093(3) 0.093(4) 0.014(3) 0.020(2) 0.005(2) C21 0.044(2) 0.067(3) 0.078(3) 0.012(2) 0.025(2) -0.003(2) C22 0.041(2) 0.049(2) 0.067(3) 0.016(2) 0.0157(18) 0.0038(17) C23 0.0333(17) 0.0320(17) 0.0319(19) 0.0016(15) 0.0007(13) -0.0009(14) C24 0.047(2) 0.0378(19) 0.046(2) 0.0020(17) 0.0090(16) -0.0058(16) C25 0.068(3) 0.033(2) 0.055(3) -0.0010(19) 0.001(2) -0.0134(18) C26 0.070(3) 0.037(2) 0.038(2) -0.0066(17) 0.0005(18) 0.0066(18) C27 0.054(2) 0.051(2) 0.035(2) -0.0033(17) 0.0086(16) 0.0097(18) C28 0.0373(18) 0.0375(18) 0.041(2) 0.0008(16) 0.0038(15) 0.0001(15) _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 Hg C1 2.11(3) . ? Hg B 2.182(4) . ? Hg Cl 2.416(18) . ? C1 N1 1.13(3) . ? N1 Cl 0.82(2) . ? B C3 1.567(5) . ? B C2 1.581(5) . ? B C4 1.581(6) . ? C2 N2 1.137(5) . ? C3 N3 1.135(5) . ? C4 N4 1.139(5) . ? P C23 1.789(3) . ? P C11 1.794(3) . ? P C5 1.796(3) . ? P C17 1.806(3) . ? C5 C10 1.393(4) . ? C5 C6 1.399(4) . ? C6 C7 1.370(5) . ? C6 H6 0.9300 . ? C7 C8 1.382(5) . ? C7 H7 0.9300 . ? C8 C9 1.370(5) . ? C8 H8 0.9300 . ? C9 C10 1.387(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.380(4) . ? C11 C16 1.388(5) . ? C12 C13 1.396(5) . ? C12 H12 0.9300 . ? C13 C14 1.370(5) . ? C13 H13 0.9300 . ? C14 C15 1.369(5) . ? C14 H14 0.9300 . ? C15 C16 1.376(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.378(5) . ? C17 C18 1.380(5) . ? C18 C19 1.383(5) . ? C18 H18 0.9300 . ? C19 C20 1.367(6) . ? C19 H19 0.9300 . ? C20 C21 1.365(6) . ? C20 H20 0.9300 . ? C21 C22 1.390(5) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.386(4) . ? C23 C28 1.397(4) . ? C24 C25 1.382(5) . ? C24 H24 0.9300 . ? C25 C26 1.368(5) . ? C25 H25 0.9300 . ? C26 C27 1.369(5) . ? C26 H26 0.9300 . ? C27 C28 1.381(5) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Hg B 176.6(9) . . ? C1 Hg Cl 3.3(12) . . ? B Hg Cl 175.9(5) . . ? N1 C1 Hg 169(2) . . ? Cl N1 C1 6(3) . . ? N1 Cl Hg 176.1(19) . . ? C3 B C2 110.7(3) . . ? C3 B C4 110.0(3) . . ? C2 B C4 113.1(3) . . ? C3 B Hg 109.4(2) . . ? C2 B Hg 106.9(3) . . ? C4 B Hg 106.6(2) . . ? N2 C2 B 176.4(4) . . ? N3 C3 B 179.6(5) . . ? N4 C4 B 176.4(4) . . ? C23 P C11 110.50(15) . . ? C23 P C5 108.05(14) . . ? C11 P C5 108.20(15) . . ? C23 P C17 110.02(15) . . ? C11 P C17 108.03(15) . . ? C5 P C17 112.04(14) . . ? C10 C5 C6 119.7(3) . . ? C10 C5 P 120.6(3) . . ? C6 C5 P 119.7(2) . . ? C7 C6 C5 119.4(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C6 C7 C8 121.0(3) . . ? C6 C7 H7 119.5 . . ? C8 C7 H7 119.5 . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.0 . . ? C7 C8 H8 120.0 . . ? C8 C9 C10 120.4(3) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? C9 C10 C5 119.6(3) . . ? C9 C10 H10 120.2 . . ? C5 C10 H10 120.2 . . ? C12 C11 C16 119.5(3) . . ? C12 C11 P 119.8(2) . . ? C16 C11 P 120.4(2) . . ? C11 C12 C13 118.9(3) . . ? C11 C12 H12 120.5 . . ? C13 C12 H12 120.5 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 119.5(4) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C11 120.9(3) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? C22 C17 C18 119.9(3) . . ? C22 C17 P 119.8(3) . . ? C18 C17 P 120.4(3) . . ? C17 C18 C19 119.5(4) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 120.3(4) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 C19 120.7(4) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C17 C22 C21 120.1(4) . . ? C17 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C24 C23 C28 119.5(3) . . ? C24 C23 P 120.5(2) . . ? C28 C23 P 120.0(2) . . ? C25 C24 C23 120.0(3) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C26 C25 C24 120.1(3) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 120.6(3) . . ? C25 C26 H26 119.7 . . ? C27 C26 H26 119.7 . . ? C26 C27 C28 120.4(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 119.4(3) . . ? C27 C28 H28 120.3 . . ? C23 C28 H28 120.3 . . ? _refine_diff_density_max 0.488 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.085 _shelxl_version_number 2013-2 _shelx_res_file ; TITL exp_3313 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 9.735176 9.733150 27.461553 90.0000 97.7355 90.0000 ZERR 4.00 0.000238 0.000283 0.000815 0.0000 0.0025 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H B N P Hg Cl UNIT 110.92 80 4 14.92 4 4 1.08 L.S. 5 ACTA 52.8 TEMP 20 BOND $H FMAP 2 PLAN 40 REM DFIX 1.14 0.01 C1 N1 REM DFIX 2.12 0.01 Hg C1 REM DFIX 3.26 0.01 Hg N1 REM DFIX 2.37 0.01 Hg Cl EADP C1 Cl ISOR 0.01 0.01 C1 Cl WGHT 0.020400 0.869100 FVAR 2.77981 0.73013 MOLE 1 HG 6 -0.013911 0.050052 0.307875 11.00000 0.03964 0.05504 = 0.04409 -0.00162 0.00877 0.00092 C1 1 -0.071485 -0.001340 0.377064 21.00000 0.05587 0.06695 = 0.07021 0.00608 0.00756 0.00388 N1 4 -0.094143 -0.049867 0.412643 21.00000 0.06334 0.06783 = 0.05080 0.00631 0.01969 0.00595 CL 7 -0.077679 -0.022603 0.385909 -21.00000 0.05587 0.06695 = 0.07021 0.00608 0.00756 0.00388 B 3 0.057470 0.107216 0.238663 11.00000 0.03693 0.04204 = 0.04172 -0.00080 0.00462 0.00385 C2 1 0.120549 -0.026693 0.217800 11.00000 0.04374 0.05199 = 0.04569 0.00539 0.00906 0.00864 N2 4 0.159025 -0.125905 0.202437 11.00000 0.07290 0.06612 = 0.07427 -0.00247 0.02517 0.02204 C3 1 -0.068247 0.161404 0.202056 11.00000 0.06031 0.04817 = 0.04737 -0.01006 0.00568 0.01521 N3 4 -0.158790 0.200962 0.175391 11.00000 0.08512 0.08548 = 0.06244 -0.01427 -0.01635 0.04051 C4 1 0.167837 0.225605 0.251020 11.00000 0.05558 0.05440 = 0.04041 0.00267 0.01240 0.00077 N4 4 0.241992 0.315089 0.260654 11.00000 0.07152 0.06913 = 0.07569 -0.00140 0.01760 -0.02128 MOLE 2 P 5 0.479947 0.293868 0.411657 11.00000 0.02971 0.03074 = 0.03200 0.00119 0.00611 0.00186 C5 1 0.553839 0.449869 0.391838 11.00000 0.03058 0.03056 = 0.03377 -0.00259 0.00747 0.00079 C6 1 0.504873 0.504600 0.345666 11.00000 0.04582 0.04010 = 0.03435 -0.00039 0.00149 -0.00394 AFIX 43 H6 2 0.433887 0.460960 0.325372 11.00000 -1.20000 AFIX 0 C7 1 0.562397 0.623053 0.330601 11.00000 0.06803 0.04065 = 0.03806 0.00640 0.00736 -0.00281 AFIX 43 H7 2 0.529323 0.660080 0.300046 11.00000 -1.20000 AFIX 0 C8 1 0.668895 0.688359 0.360152 11.00000 0.06267 0.04210 = 0.05125 -0.00108 0.01761 -0.01206 AFIX 43 H8 2 0.706729 0.768913 0.349503 11.00000 -1.20000 AFIX 0 C9 1 0.718630 0.634307 0.405126 11.00000 0.04864 0.04667 = 0.04819 -0.01122 0.00953 -0.01776 AFIX 43 H9 2 0.790901 0.677892 0.424815 11.00000 -1.20000 AFIX 0 C10 1 0.661873 0.514990 0.421479 11.00000 0.03838 0.04137 = 0.03483 -0.00156 0.00771 -0.00063 AFIX 43 H10 2 0.695748 0.478645 0.452067 11.00000 -1.20000 AFIX 0 C11 1 0.583240 0.237990 0.467152 11.00000 0.03093 0.03107 = 0.03452 0.00159 0.00615 0.00498 C12 1 0.693866 0.150861 0.464675 11.00000 0.03797 0.04575 = 0.03859 0.00447 0.01021 0.00806 AFIX 43 H12 2 0.709313 0.112815 0.434824 11.00000 -1.20000 AFIX 0 C13 1 0.782212 0.120748 0.507690 11.00000 0.03892 0.04748 = 0.06271 0.01154 0.00961 0.01180 AFIX 43 H13 2 0.857445 0.062617 0.506387 11.00000 -1.20000 AFIX 0 C14 1 0.759437 0.175795 0.551812 11.00000 0.05417 0.05732 = 0.04646 0.01210 -0.00302 0.00396 AFIX 43 H14 2 0.819853 0.155787 0.580115 11.00000 -1.20000 AFIX 0 C15 1 0.648129 0.260127 0.554420 11.00000 0.06859 0.06919 = 0.03618 -0.00142 0.00152 0.01570 AFIX 43 H15 2 0.631135 0.295206 0.584539 11.00000 -1.20000 AFIX 0 C16 1 0.561555 0.292635 0.512163 11.00000 0.05500 0.05515 = 0.03830 -0.00014 0.00832 0.01902 AFIX 43 H16 2 0.487495 0.352046 0.513795 11.00000 -1.20000 AFIX 0 C17 1 0.304587 0.318515 0.424622 11.00000 0.03167 0.03803 = 0.03851 -0.00089 0.00806 0.00128 C18 1 0.220927 0.417224 0.399725 11.00000 0.04071 0.07116 = 0.06356 0.02524 0.01220 0.01241 AFIX 43 H18 2 0.255209 0.473386 0.376752 11.00000 -1.20000 AFIX 0 C19 1 0.085745 0.432034 0.409181 11.00000 0.03952 0.09698 = 0.10203 0.04181 0.01500 0.02273 AFIX 43 H19 2 0.028847 0.498170 0.392397 11.00000 -1.20000 AFIX 0 C20 1 0.035327 0.349950 0.443074 11.00000 0.02954 0.09257 = 0.09339 0.01391 0.01986 0.00515 AFIX 43 H20 2 -0.055722 0.360802 0.449177 11.00000 -1.20000 AFIX 0 C21 1 0.117188 0.252214 0.468061 11.00000 0.04414 0.06678 = 0.07785 0.01208 0.02461 -0.00268 AFIX 43 H21 2 0.082597 0.197472 0.491366 11.00000 -1.20000 AFIX 0 C22 1 0.252712 0.235195 0.458376 11.00000 0.04135 0.04936 = 0.06723 0.01568 0.01570 0.00381 AFIX 43 H22 2 0.308438 0.167446 0.474714 11.00000 -1.20000 AFIX 0 C23 1 0.482866 0.168440 0.364178 11.00000 0.03331 0.03196 = 0.03194 0.00155 0.00074 -0.00092 C24 1 0.386007 0.063292 0.358538 11.00000 0.04702 0.03778 = 0.04574 0.00199 0.00896 -0.00583 AFIX 43 H24 2 0.317733 0.058550 0.379131 11.00000 -1.20000 AFIX 0 C25 1 0.390851 -0.034476 0.322334 11.00000 0.06798 0.03330 = 0.05500 -0.00099 0.00132 -0.01340 AFIX 43 H25 2 0.326343 -0.105471 0.318766 11.00000 -1.20000 AFIX 0 C26 1 0.490447 -0.026936 0.291732 11.00000 0.06972 0.03714 = 0.03761 -0.00660 0.00050 0.00656 AFIX 43 H26 2 0.492346 -0.092205 0.267098 11.00000 -1.20000 AFIX 0 C27 1 0.587385 0.075831 0.297034 11.00000 0.05421 0.05071 = 0.03487 -0.00326 0.00861 0.00968 AFIX 43 H27 2 0.655188 0.079240 0.276225 11.00000 -1.20000 AFIX 0 C28 1 0.585121 0.174452 0.333081 11.00000 0.03727 0.03747 = 0.04097 0.00076 0.00377 0.00005 AFIX 43 H28 2 0.651020 0.244186 0.336623 11.00000 -1.20000 AFIX 0 HKLF 4 REM exp_3313 in P2(1)/c REM R1 = 0.0314 for 4774 Fo > 4sig(Fo) and 0.0496 for all 6109 data REM 320 parameters refined using 12 restraints END WGHT 0.0204 0.8683 REM Highest difference peak 0.488, deepest hole -0.874, 1-sigma level 0.085 Q1 1 0.0015 0.1419 0.3186 11.00000 0.05 0.49 Q2 1 0.3838 0.3023 0.4191 11.00000 0.05 0.47 Q3 1 -0.0124 0.1395 0.2809 11.00000 0.05 0.44 Q4 1 0.5355 0.2655 0.4422 11.00000 0.05 0.44 Q5 1 -0.0166 -0.0366 0.3292 11.00000 0.05 0.42 Q6 1 0.0793 0.0991 0.3064 11.00000 0.05 0.41 Q7 1 0.5159 0.3722 0.3967 11.00000 0.05 0.40 Q8 1 0.0640 -0.0004 0.3091 11.00000 0.05 0.40 Q9 1 -0.1279 0.0652 0.3010 11.00000 0.05 0.39 Q10 1 0.4590 0.2242 0.3909 11.00000 0.05 0.39 Q11 1 -0.0746 0.0379 0.3269 11.00000 0.05 0.37 Q12 1 0.0433 0.0784 0.3411 11.00000 0.05 0.36 Q13 1 0.6219 0.2070 0.3379 11.00000 0.05 0.34 Q14 1 0.3858 0.0544 0.3303 11.00000 0.05 0.34 Q15 1 0.0034 0.2525 0.3186 11.00000 0.05 0.33 Q16 1 -0.0072 0.0383 0.4012 11.00000 0.05 0.32 Q17 1 0.5486 0.1570 0.3630 11.00000 0.05 0.32 Q18 1 -0.0417 0.3553 0.2048 11.00000 0.05 0.31 Q19 1 0.6985 0.5511 0.4047 11.00000 0.05 0.31 Q20 1 -0.1194 0.1195 0.2073 11.00000 0.05 0.30 Q21 1 -0.1201 -0.0359 0.3982 11.00000 0.05 0.30 Q22 1 0.4364 0.1275 0.3663 11.00000 0.05 0.30 Q23 1 0.2312 0.6325 0.3821 11.00000 0.05 0.30 Q24 1 -0.0761 0.0278 0.2692 11.00000 0.05 0.29 Q25 1 0.2037 -0.2334 0.1754 11.00000 0.05 0.29 Q26 1 -0.1216 0.1867 0.2153 11.00000 0.05 0.29 Q27 1 0.1978 0.0456 0.3940 11.00000 0.05 0.29 Q28 1 0.0882 0.3576 0.2000 11.00000 0.05 0.29 Q29 1 -0.0729 0.1010 0.3800 11.00000 0.05 0.29 Q30 1 0.6408 0.7346 0.3526 11.00000 0.05 0.29 Q31 1 -0.0703 -0.0922 0.3621 11.00000 0.05 0.29 Q32 1 0.9025 0.1253 0.5290 11.00000 0.05 0.28 Q33 1 0.7759 0.1732 0.4774 11.00000 0.05 0.28 Q34 1 0.0545 0.0295 0.2830 11.00000 0.05 0.28 Q35 1 0.6418 0.2324 0.4646 11.00000 0.05 0.28 Q36 1 0.3957 -0.1793 0.3456 11.00000 0.05 0.28 Q37 1 0.7115 0.1115 0.4912 11.00000 0.05 0.27 Q38 1 -0.0973 0.2088 0.1762 11.00000 0.05 0.27 Q39 1 0.5875 0.6599 0.3531 11.00000 0.05 0.27 Q40 1 0.1345 0.0588 0.2274 11.00000 0.05 0.27 ; _shelx_res_checksum 27929 _shelx_hkl_file ; 0 0 3 172.076 81.7021 1 0 0 3 39.9705 117.278 3 0 0 4 2266.87 261.853 3 0 0 4 1612.49 212.349 1 0 0 5 517.510 195.267 3 0 0 5 1071.62 207.072 1 0 0 6 70955.3 1735.90 3 0 0 6 73822.7 1665.06 1 0 0 7 461.828 285.311 3 0 0 7 655.997 233.711 1 0 0 8 747807. 10010.6 1 0 0 8 689670. 10135.1 3 0 0 9 950.007 362.772 1 0 0 9 1042.29 371.097 3 0 0 10 439921. 7081.01 3 0 0 10 450507. 6855.36 1 0 0 11 168.744 298.431 3 0 0 11 635.617 344.217 1 0 0 12 14110.2 852.860 1 0 0 12 13046.6 894.744 3 0 0 13 77.1038 243.205 1 0 0 13 22.6672 289.518 3 0 0 14 63133.8 2000.43 1 0 0 14 59282.4 2106.59 3 0 0 15 812.004 349.718 1 0 0 16 109302. 2880.51 1 0 0 -17 1036.65 608.862 3 0 0 17 1195.94 449.444 1 0 0 18 243648. 3559.79 4 0 0 -18 249587. 5232.46 3 0 0 19 620.593 150.341 4 0 0 -19 2127.16 683.890 3 0 0 -20 66372.2 2469.65 3 0 0 20 65219.2 1251.46 4 0 0 -21 684.250 510.234 3 0 0 21 217.829 87.8062 4 0 0 -22 7044.22 896.771 3 0 0 -23-516.065 586.666 3 0 0 -24 12481.1 1214.18 3 0 0 -25 1027.36 629.699 3 0 0 -26 34458.0 1940.80 3 0 0 -27 440.065 620.253 3 0 0 -28 23804.5 1703.85 3 0 0 -29 300.042 682.585 3 0 0 -30-136.654 588.164 3 0 0 -31 842.148 643.908 3 0 0 -32 3947.46 873.662 3 0 0 -33 613.840 622.979 3 0 0 -34 7201.53 1138.76 3 0 -1 0 222.633 58.9146 5 0 -1 -1 30747.2 580.092 5 0 1 2 140401. 1899.96 3 0 -1 2 138568. 2023.06 3 0 -1 -3 379407. 4898.68 2 0 1 3 396519. 5006.76 3 0 1 3 402782. 4899.40 2 0 -1 3 387429. 5181.89 3 0 1 4 2362.38 192.805 3 0 -1 -4 1889.72 132.681 2 0 -1 4 2248.53 226.589 3 0 1 5 796625. 10021.1 3 0 -1 5 775024. 10221.6 3 0 1 -6 71224.6 1345.45 1 0 -1 6 71720.0 1641.24 3 0 1 6 67109.8 1475.22 3 0 -1 7 30433.2 1083.79 3 0 1 -7 31445.8 883.391 1 0 -1 -7 29639.4 944.613 3 0 1 7 30488.9 989.304 3 0 1 -8 14698.8 638.513 1 0 -1 8 14070.6 787.601 3 0 -1 -8 16582.5 756.263 3 0 1 8 16885.0 767.719 3 0 1 9 12261.3 730.067 3 0 -1 -9 11387.0 682.194 3 0 1 -9 11045.9 595.869 1 0 -1 9 10533.6 723.464 3 0 1 -10 168.728 190.764 1 0 1 10 363.630 271.263 3 0 -1 -10 698.061 309.390 3 0 -1 10 874.764 334.551 3 0 -1 10 381.322 191.587 1 0 1 -11 117620. 2558.14 1 0 -1 -11 114774. 2715.87 3 0 -1 11 114835. 2567.61 1 0 1 11 123215. 2855.64 3 0 -1 11 118370. 2937.58 3 0 -1 -12 36758.7 1493.96 3 0 -1 12 35485.2 1350.96 1 0 1 12 39712.7 1557.81 3 0 -1 12 36293.4 1569.12 3 0 -1 13 403145. 6773.56 1 0 -1 -13 403283. 6929.90 3 0 1 13 446150. 7128.32 1 0 1 13 432758. 7135.20 3 0 -1 13 425498. 7229.70 3 0 -1 14 7980.85 745.114 1 0 1 14 7405.17 735.422 1 0 1 14 9018.68 834.925 3 0 1 15 205948. 4354.90 1 0 -1 15 200211. 4169.33 1 0 -1 16 8604.10 762.091 1 0 -1 17 348.024 290.063 1 0 -1 -17 674.063 437.281 3 0 -1 -18 3578.52 642.180 3 0 -1 18 3732.11 524.778 1 0 1 -18 3507.32 636.738 3 0 -1 -19 54135.6 2164.62 3 0 1 -19 51684.6 2213.11 3 0 -1 -20 43022.1 1943.53 3 0 1 -20 47463.2 2145.44 3 0 -1 -21 96418.9 3057.42 3 0 1 -21 93418.9 3133.43 3 0 1 -22 1862.07 701.483 3 0 -1 -22 2178.90 681.280 3 0 -1 -23 50849.7 2210.75 3 0 1 -23 46934.1 2241.37 3 0 1 -24 10345.8 1116.56 3 0 -1 -24 10555.4 1064.68 3 0 -1 -25 6876.57 959.682 3 0 1 -25 6180.27 880.707 3 0 -1 -26 98.6391 516.817 3 0 1 -26 332.310 466.022 3 0 -1 -27 6103.93 912.266 3 0 1 -27 6422.68 968.717 3 0 1 -28 1940.79 704.296 3 0 -1 -28 1611.08 713.245 3 0 1 -29 18903.1 1573.18 3 0 -1 -29 18714.9 1523.35 3 0 -1 -30 4688.88 868.804 3 0 1 -30 5493.46 1009.40 3 0 -1 -31 20970.1 1649.58 3 0 1 -31 18589.6 1622.31 3 0 -1 -32 2402.51 810.739 3 0 1 -32 1282.01 754.852 3 0 1 -33 4127.37 956.567 3 0 -1 -33 2887.66 776.592 3 0 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1319.54 3 2 5 8 26545.6 1044.96 2 2 5 9-119.836 191.297 3 -2 5 -9 180.426 352.516 3 2 5 9-281.622 282.024 2 2 5 10 35443.8 1263.79 3 -2 5 -10 33104.0 1497.21 3 2 5 10 34051.8 1218.74 2 -2 5 -11 8922.73 825.561 3 2 5 11 8706.81 663.724 3 2 5 11 8379.54 615.411 2 -2 5 -12 118692. 3187.82 3 2 5 12 121642. 2810.82 3 2 5 12 117431. 2596.63 2 2 5 13 1039.03 360.804 3 -2 5 -13 1289.06 507.944 3 2 5 14 65285.2 2084.86 3 -2 -5 -14 69775.0 1858.04 3 -2 5 -14 64290.7 2383.53 3 2 5 15 3029.91 502.679 3 -2 5 -15 2347.02 614.884 3 -2 -5 -15 4312.38 548.188 3 -2 5 -16 31679.5 1741.58 3 -2 -5 -16 27360.4 869.653 6 -2 5 -17 4055.34 788.829 3 -2 5 -18 1598.43 694.499 3 -2 5 -18 1819.45 477.156 1 -2 -5 -18 1755.99 492.390 3 -2 5 -19 1512.30 693.153 3 -2 5 -19 1205.43 471.167 1 -2 -5 -19 1155.73 463.428 3 -2 5 -20 36815.1 2135.27 3 -2 -5 -20 35536.9 1726.91 3 -2 5 -20 36340.3 1730.08 1 -2 5 -21 1169.72 558.259 1 -2 -5 -21 1957.59 599.384 3 -2 -5 -22 39594.5 1992.06 3 -2 5 -22 38823.1 1902.58 1 -2 5 -22 41318.6 2393.89 3 -2 5 -23 503.492 558.004 1 -2 -5 -23 288.835 550.860 3 -2 5 -23 623.057 747.443 3 -2 5 -24 28544.1 1709.85 1 -2 -5 -24 31305.0 1906.46 3 -2 5 -24 27321.0 2104.79 3 -2 5 -25-582.853 695.285 3 -2 5 -25 91.0650 549.832 1 -2 -5 -25-115.099 555.956 3 -2 5 -26 168.315 835.785 3 -2 5 -26-462.885 620.865 1 -2 -5 -26-239.129 644.643 3 -2 5 -27 661.544 659.898 3 -2 5 -27 458.330 627.554 1 -2 -5 -27 417.013 576.557 3 -2 5 -28 3080.59 980.839 3 -2 -5 -28 6371.96 968.473 3 -2 5 -29 3146.50 995.796 3 -2 -5 -29 1019.35 574.914 3 -2 -5 -30 10392.0 1235.60 3 2 6 -30-501.097 707.512 3 2 6 -29 1168.28 705.485 3 2 6 -28 182.413 637.482 3 2 6 -27 10549.9 1290.11 3 2 6 -26 4579.95 960.557 3 2 6 -25 31329.3 2042.92 3 2 6 -24 1406.72 699.803 3 2 6 -23 20123.2 1662.41 3 2 6 -22 926.375 584.101 3 2 6 -21 2.19336 552.924 3 2 6 -20-125.074 657.806 3 2 6 -19 23707.8 1632.67 3 2 6 -18 6785.70 956.158 3 2 6 -18 6628.92 443.299 1 2 6 -17 66947.9 2669.67 3 2 6 -17 62815.1 1460.23 1 2 6 -16 8937.10 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2 6 -1 71859.9 2105.75 5 2 6 0 9704.44 453.622 3 -2 6 0 10860.1 673.408 5 2 6 0 9724.21 758.770 5 2 6 1 71299.9 1964.30 2 -2 6 -1 73102.1 1857.83 5 2 6 1 70282.5 1347.21 3 -2 6 -2 8287.51 620.512 5 2 6 2 7326.54 339.938 3 2 6 2 7050.66 655.271 5 2 6 2 7393.10 621.581 2 -2 6 -3 56328.0 1655.14 5 2 6 3 58902.0 1712.27 2 2 6 3 57799.9 1470.27 6 2 6 3 56443.2 1045.22 3 2 6 4 8444.30 670.793 2 2 6 4 9325.88 533.809 6 2 6 4 9684.65 374.977 3 2 6 5 266.522 181.484 6 2 6 5 198.079 111.439 3 2 6 5 245.434 262.714 2 2 6 6 61.3001 134.071 3 2 6 6 396.060 213.286 6 2 6 7 101518. 1943.73 3 -2 6 -7 96068.3 2670.37 3 2 6 7 98667.4 2329.95 2 2 6 8 19663.6 948.239 2 2 6 8 18751.2 778.624 3 -2 6 -8 21263.0 1206.84 3 2 6 9 59729.2 1733.62 2 -2 6 -9 61436.4 2124.54 3 2 6 9 60484.2 1605.86 3 2 6 10 16180.7 877.582 2 -2 6 -10 15253.8 1080.42 3 2 6 10 16966.1 854.629 3 -2 6 -11 44005.8 1845.88 3 2 6 11 40926.0 1432.88 3 2 6 11 40440.8 1409.69 2 2 6 12 246.097 305.485 2 2 6 12 39.5784 278.375 3 -2 6 -12 194.203 431.223 3 -2 6 -13 11985.8 1049.65 3 2 6 13 11987.0 841.564 3 2 6 13 12568.1 787.068 2 2 6 14 1272.43 368.569 3 -2 6 -14 1050.19 525.506 3 2 6 15 21290.4 1193.25 3 -2 6 -15 20352.5 1424.56 3 -2 6 -16 3929.64 778.290 3 -2 6 -17 47597.3 2280.81 3 -2 6 -18 7778.10 1077.88 3 -2 6 -19 15444.5 1424.54 3 -2 6 -19 17688.7 1207.59 1 -2 6 -20 1179.23 485.169 1 -2 6 -20 2264.46 842.537 3 -2 6 -21 8639.34 916.892 1 -2 6 -21 7767.27 1152.49 3 -2 6 -22 573.807 696.572 3 -2 6 -22 276.550 490.293 1 -2 6 -23 684.069 498.859 1 -2 6 -23 1033.22 709.729 3 -2 6 -24 3335.41 1073.40 3 -2 6 -24 2008.36 670.312 1 -2 6 -25 24726.2 1626.36 1 -2 6 -25 23424.5 2023.30 3 -2 6 -26 2576.72 1010.90 3 -2 6 -26 881.495 557.906 1 -2 6 -27 6723.65 1254.84 3 -2 6 -28 299.160 798.389 3 2 7 -29 122.767 626.925 3 2 7 -28 2816.41 768.124 3 2 7 -27 650.218 583.439 3 2 7 -26 751.661 707.121 3 2 7 -25 369.450 648.396 3 2 7 -24 598.896 638.073 3 2 7 -23 7186.04 1045.01 3 2 7 -22 15024.3 1421.62 3 2 7 -21 6102.41 1000.68 3 2 7 -20 26268.7 1812.94 3 2 7 -19 2243.70 690.756 3 2 7 -18 12037.3 1228.87 3 2 7 -17 357.170 526.405 3 2 7 -16 2011.27 624.085 3 2 7 -15 9822.23 1089.92 3 2 7 -14 37369.9 1959.99 3 2 7 -13 33317.8 1780.22 3 2 7 -13 32696.5 1685.98 5 2 7 -12 50991.2 2071.41 5 2 7 -12 54039.1 2236.04 3 2 7 -11 7678.32 851.905 3 2 7 -11 7251.44 854.311 5 -2 7 11 7174.22 350.573 2 -2 7 10 15470.3 553.769 2 2 7 -10 15066.5 1089.04 5 2 7 -10 15756.4 1119.57 3 -2 7 9 6453.86 389.348 2 2 7 -9 5500.46 722.234 5 2 7 -9 5559.35 671.821 3 -2 7 8 65.4171 151.722 2 2 7 -8-331.980 521.895 5 2 7 -8-172.376 316.814 3 2 7 -7 611.857 344.566 3 -2 7 7 537.693 209.964 2 2 7 -7 118.982 441.445 5 2 7 -6 32077.7 1517.82 5 2 7 -6 35626.9 1424.25 3 2 7 -5 50058.2 1639.56 3 2 7 -5 47473.3 1872.20 5 2 7 -4 78402.2 2009.95 3 2 7 -4 77884.1 2377.81 5 2 7 -3 34659.6 1554.01 5 -2 7 3 34087.7 1270.33 5 2 7 -3 34335.0 1215.95 3 -2 7 2 57298.9 1712.50 5 2 7 -2 57800.8 2014.10 5 2 7 -2 59129.4 1527.77 3 -2 7 1 1815.02 383.670 5 2 7 -1 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656.010 6 -10 4 18 1562.80 936.045 4 10 4 -18 1167.82 647.365 2 10 4 -17 21661.0 1685.71 6 10 4 -17 21985.0 1629.44 2 -10 4 17 17154.6 1905.52 4 10 4 -16 3739.61 988.109 6 -10 4 16 1223.83 903.326 4 10 4 -16 4261.46 917.307 2 10 4 -15 19774.8 1610.10 6 10 4 -15 18021.7 1472.74 2 -10 4 15 16333.0 1895.39 4 10 4 -14 1404.54 748.270 6 -10 4 14 365.992 772.918 4 10 4 -14 1226.54 700.168 2 -10 4 13 9130.52 1458.06 4 10 4 -13 11921.6 1189.34 2 -10 4 12 740.281 826.169 4 10 4 -12 1134.08 649.471 2 -10 4 11 2612.59 963.884 4 10 4 -11 2115.85 641.117 2 -10 4 10-181.274 716.601 4 10 4 -10 637.980 621.159 2 10 4 -9 15457.2 1323.70 2 -10 4 9 15380.7 1804.89 4 -10 4 8 6114.14 1319.67 4 10 4 -8 6156.60 933.177 2 10 4 -7 27820.7 1708.06 2 -10 4 7 26215.2 2197.31 4 10 4 -6 5475.08 909.011 2 -10 4 6 6010.00 1268.26 4 10 4 -5 17117.1 1357.81 2 -10 4 5 17380.7 1793.75 4 10 4 -4 1010.68 654.238 2 -10 4 4 998.380 834.084 4 10 4 -3 4514.75 763.446 2 -10 4 3 5301.64 1017.19 4 10 4 -2 736.067 632.625 2 -10 4 2-430.462 696.046 4 10 4 -1 1454.95 635.912 2 -10 4 1 1917.40 838.010 4 10 4 0 1364.86 690.778 2 -10 4 0-26.4753 606.312 4 -10 4 -1 22905.0 1884.89 4 10 4 1 23852.4 1612.30 2 10 4 2 7150.76 1010.80 2 -10 4 -2 6591.79 1106.86 4 -10 4 -3 15999.7 1525.83 4 10 4 3 15669.0 1334.19 2 10 4 4 25.5246 660.189 2 -10 4 -4 551.345 615.805 4 -10 4 -5 1591.34 667.884 4 10 4 5 2253.02 707.698 2 -10 4 -6 1230.94 701.970 4 -10 4 -7-111.520 636.864 4 -10 4 -8-681.284 619.680 4 -10 4 -9 6508.85 1006.26 4 -10 4 -9 9273.67 1172.39 3 -10 4 -10 1024.50 581.992 4 -10 4 -10 1414.43 727.110 3 -10 4 -11 27303.2 2044.48 1 -10 4 -11 20468.2 1573.89 4 -10 4 -11 24626.6 1819.91 3 -10 4 -12 1459.44 750.566 3 -10 4 -13 4879.86 991.329 3 -10 4 -14 216.604 691.984 3 10 5 -22 4978.72 1004.97 2 10 5 -21 2034.64 895.384 2 10 5 -20 15548.6 1522.70 2 10 5 -19 1290.59 695.120 2 10 5 -18 14542.5 1431.68 2 10 5 -17 1081.61 669.034 6 10 5 -17 870.085 612.340 5 -10 5 17-380.490 885.838 4 10 5 -17 364.664 726.482 2 10 5 -16 2169.90 826.858 6 10 5 -16 1762.90 655.331 5 -10 5 16-97.6918 882.140 4 10 5 -16 1087.25 703.195 2 10 5 -15 987.366 749.963 6 -10 5 15 531.071 795.847 4 10 5 -15 1099.10 716.035 2 10 5 -14 2987.92 891.281 6 -10 5 14 2049.42 1042.86 4 10 5 -14 2571.09 833.795 2 10 5 -13 938.879 750.371 6 -10 5 13-410.542 864.490 4 10 5 -13 684.674 653.493 2 10 5 -12 16369.6 1460.15 6 10 5 -12 15873.1 1392.80 2 -10 5 12 15510.1 1909.68 4 -10 5 11 1365.29 974.443 4 10 5 -11 477.251 591.323 2 10 5 -10 20130.2 1548.30 2 -10 5 10 21110.4 2098.50 4 -10 5 9 927.182 846.130 4 10 5 -9 1755.66 708.382 2 -10 5 8 7243.13 1258.50 4 10 5 -8 8503.25 1089.19 2 -10 5 7 1976.34 991.611 4 10 5 -7 3825.23 788.328 2 -10 5 6 0.84509 797.411 4 10 5 -6 2676.77 764.634 2 10 5 -5 152.116 535.671 2 -10 5 5 204.029 668.161 4 10 5 -4 14234.9 1341.79 2 -10 5 4 13462.9 1638.08 4 10 5 -3 1403.00 719.451 2 -10 5 3 1713.25 798.021 4 10 5 -2 23863.7 1627.64 2 -10 5 2 23396.7 2039.88 4 10 5 -1 1589.81 677.337 2 -10 5 1 2669.24 1038.84 4 10 5 0 19796.3 1539.16 2 -10 5 0 19150.7 1793.52 4 10 5 1 407.938 638.041 2 -10 5 -1-433.456 617.138 4 10 5 2 2211.61 720.605 2 -10 5 -2 1397.01 698.014 4 10 5 3 1239.75 678.666 2 -10 5 -3 96.9488 568.475 4 10 5 4 4980.68 918.544 2 -10 5 -4 6133.58 1091.80 4 10 5 5 679.568 608.717 2 -10 5 -5 414.008 624.575 4 -10 5 -6 13970.5 1489.58 4 10 5 6 15307.9 1422.26 2 -10 5 -7 1489.78 789.384 4 -10 5 -8 13185.7 1389.05 4 -10 5 -9 766.867 612.739 4 -10 5 -9 1164.30 647.382 3 -10 5 -10 2360.38 710.905 4 -10 5 -10 1520.27 714.606 3 -10 5 -11 184.184 580.748 3 10 6 -19 202.102 650.625 5 10 6 -18 1520.44 705.113 5 10 6 -17 3529.49 822.671 5 10 6 -16 1523.59 695.967 5 10 6 -16 2815.88 924.134 2 10 6 -15 20543.8 1692.22 2 10 6 -14 3737.73 997.033 2 10 6 -13 13312.3 1405.76 6 -10 6 13 12255.4 1756.29 4 10 6 -13 12896.8 1377.89 2 10 6 -12 979.241 793.410 6 -10 6 12-782.960 874.027 4 10 6 -12 2180.85 855.662 2 10 6 -11 1770.66 785.977 6 -10 6 11-337.222 916.183 4 10 6 -11 880.084 741.672 2 -10 6 10 1855.87 1036.95 4 10 6 -10 1260.12 740.605 2 -10 6 9 1337.15 875.750 4 10 6 -9 1259.07 640.216 2 -10 6 8 2190.17 902.960 4 10 6 -8 1677.73 734.392 2 -10 6 7 7714.92 1383.88 4 10 6 -7 9795.44 1190.73 2 -10 6 6 2803.92 1020.87 4 10 6 -6 2808.41 767.842 2 10 6 -5 20016.3 1570.80 2 -10 6 5 17139.5 1815.38 4 10 6 -4-821.983 662.228 2 -10 6 4 1059.65 840.767 4 10 6 -3 1125.33 630.926 2 -10 6 3 1048.72 704.779 4 10 6 -2 946.319 703.283 2 -10 6 2-925.191 824.815 4 10 6 -1 2240.60 708.021 2 -10 6 1 1933.09 928.625 4 10 6 0 40.0160 643.705 2 -10 6 0 208.997 666.930 4 10 6 1 4796.72 952.136 2 -10 6 -1 5066.14 1121.79 4 10 6 2 1546.07 754.312 2 -10 6 -2 1617.23 861.544 4 -10 6 -3 19338.1 1771.61 4 10 6 3 17126.4 1490.99 2 10 6 4 887.337 758.892 2 -10 6 -4 922.715 759.707 4 10 6 5 3395.76 760.402 2 -10 6 -5 3637.68 952.456 4 -10 6 -6 399.340 655.939 4 -10 6 -7 335.762 616.519 4 -10 6 -8 876.960 618.614 4 -10 6 -9 3313.02 806.919 4 10 7 -17 3454.54 901.165 5 10 7 -16 1186.12 713.149 5 -10 7 6 464.277 674.078 4 -10 7 5 739.943 809.633 4 -10 7 4 590.875 745.597 4 -10 7 3 9508.88 1448.37 4 -10 7 2 9058.15 1443.23 4 -10 7 1 562.375 779.112 4 -10 7 0 4722.67 1052.98 4 -10 7 -1 713.679 733.075 4 -10 7 -2 2123.62 893.389 4 -10 7 -3-1229.41 806.142 4 -10 7 -4 636.802 742.805 4 -10 7 -5 2974.65 949.197 4 -10 7 -6 5273.01 1048.27 4 -10 7 -7 3805.34 915.021 4 -10 7 -8 3531.80 906.021 4 -10 8 -4 2371.21 835.759 4 -10 8 -5 214.087 741.347 4 -10 8 -6-362.559 672.233 4 -10 8 -7-207.873 686.294 4 -11 0 21 464.202 836.896 4 -11 0 20 455.077 819.716 4 -11 0 19 266.260 829.718 4 -11 0 18 2990.90 966.650 4 -11 0 17-46.3442 708.519 4 -11 0 16 12168.7 1695.04 4 -11 0 15 1290.77 858.334 4 -11 0 14 39935.2 2923.61 4 11 0 -13-117.397 508.147 2 -11 0 13 741.762 776.182 4 11 0 -12 10251.0 1002.31 2 -11 0 12 10732.7 1529.95 4 11 0 -11-13.6994 513.181 2 -11 0 11-1150.17 948.349 4 11 0 -10 4694.51 736.309 2 -11 0 10 4587.67 1152.23 4 -11 0 9 1449.06 911.844 4 11 0 -9 359.483 501.410 2 -11 0 8 8782.43 1458.52 4 -11 0 7 705.088 876.767 4 -11 0 6 42183.6 2247.71 1 -11 0 6 36019.6 2576.64 4 -11 0 5 1715.56 885.052 4 -11 0 5 2016.61 814.224 1 -11 0 4 33219.8 2027.17 1 -11 0 4 34123.3 2438.68 4 -11 0 3 1161.48 750.862 1 -11 0 3 624.118 683.233 4 -11 0 2 2555.74 790.667 1 -11 0 2 3154.57 999.360 4 -11 0 1 540.229 820.390 4 -11 0 1 35.1035 593.983 1 -11 0 0 3801.51 1019.88 4 -11 0 0 2573.13 874.811 1 -11 0 -1 963.183 739.038 1 -11 0 -1 1082.40 741.226 4 -11 0 -2 10149.6 1336.36 1 -11 0 -3-191.160 686.225 1 -11 0 -4 20477.7 1785.33 1 -11 0 -5 906.095 804.481 1 -11 0 -6 7505.86 1205.48 1 -11 0 -6 7800.65 969.666 3 -11 0 -7 1517.43 948.091 1 -11 0 -7 253.258 486.307 3 -11 0 -8 5080.52 1070.98 1 -11 0 -8 4527.34 802.322 3 -11 0 -9-51.4315 746.542 1 -11 0 -9-115.970 507.606 3 -11 0 -10 11797.1 1561.85 1 -11 0 -11 437.687 794.156 1 -11 -1 22 3131.29 943.660 4 -11 -1 21 7231.57 1363.60 4 -11 -1 20 1758.91 1033.85 4 -11 1 20 2084.65 1035.71 4 -11 -1 19 23985.9 2251.70 4 -11 1 19 21839.3 2204.76 4 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-1 -8 1144.34 842.598 1 -11 1 -8 907.862 737.220 1 -11 1 -8 2108.64 698.362 3 -11 1 -9 10718.5 1177.01 3 -11 1 -9 10615.7 1502.72 1 -11 -1 -9 11159.6 1511.16 1 -11 1 -10 332.431 735.264 1 -11 -1 -10-927.478 937.156 1 -11 1 -10 617.966 561.830 3 -11 -1 -11-243.627 827.192 1 -11 1 -11 1239.43 653.833 3 -11 1 -12 667.408 624.288 3 -11 1 -13 5512.45 979.205 3 -11 1 -14 599.546 641.153 3 -11 1 -15 7310.52 1111.15 3 -11 2 19-235.944 693.762 4 -11 2 18 4021.52 1192.73 4 11 2 -18 4219.43 775.250 2 -11 2 17 5697.67 1331.06 4 11 2 -17 7062.40 973.459 2 11 2 -16 16265.3 1346.55 2 -11 2 16 14096.8 1906.43 4 -11 2 15 8562.88 1583.53 4 11 2 -15 10004.8 1108.23 2 11 2 -14 12540.0 1209.07 2 -11 2 14 9363.95 1613.34 4 -11 2 13 9160.85 1609.26 4 11 2 -13 5698.66 883.235 2 11 2 -12 5461.13 844.401 2 -11 2 12 6840.40 1384.48 4 11 2 -11 3920.73 728.176 2 -11 2 11 4768.83 1147.47 4 11 2 -10-131.791 511.545 2 -11 2 10-195.132 745.318 4 11 2 -9 4094.58 785.558 2 -11 2 9 3569.16 1060.41 4 -11 2 8 9989.48 1438.84 4 11 2 -8 16063.7 1304.77 2 -11 2 7 12930.7 1642.80 4 11 2 -7 12991.0 1226.82 2 -11 2 6 14560.1 1735.15 4 11 2 -6 17024.0 1354.97 2 -11 -2 5 6644.60 1133.82 1 11 2 -5 5720.06 886.365 2 -11 2 5 4824.07 1161.96 4 -11 -2 4 11329.1 1375.72 1 11 2 -4 9720.22 1094.20 2 -11 2 4 11753.6 1567.41 4 11 2 -3 1846.49 688.440 2 -11 2 3 1099.33 841.956 4 -11 -2 3 1043.03 686.806 1 11 2 -2 2602.87 747.058 2 -11 2 2 319.750 654.019 4 -11 -2 2 965.784 720.908 1 -11 2 1-512.648 640.990 4 11 2 -1 667.895 500.119 2 -11 -2 1-597.674 820.200 1 -11 2 0 8914.46 1275.69 4 -11 -2 0 5729.98 1053.70 1 -11 2 -1 12634.2 1493.25 4 -11 -2 -1 11776.2 1392.66 1 -11 2 -2 14450.0 1552.01 4 -11 -2 -2 14214.9 1614.64 1 -11 2 -3 6665.89 1131.37 4 -11 -2 -3 4396.69 1086.35 1 -11 -2 -4 4924.94 1049.92 1 -11 2 -4 6295.86 1100.97 4 -11 2 -4 7479.31 1185.49 1 -11 2 -5 3755.27 975.599 1 -11 -2 -5 2472.51 862.765 1 -11 2 -5 3595.68 914.260 4 -11 -2 -6 1712.07 821.148 1 -11 2 -6 3480.81 1011.27 1 -11 2 -6 2640.11 775.310 4 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19470.8 1980.59 4 11 3 -9 5082.45 939.496 2 -11 3 9 6019.10 1310.18 4 11 3 -8 11497.8 1204.58 2 -11 3 8 10383.6 1535.30 4 11 3 -7 4542.63 904.579 2 -11 3 7 3909.36 1061.19 4 11 3 -6 34.1797 556.367 2 -11 3 6 306.762 799.222 4 11 3 -5-143.518 495.599 2 -11 3 5 1660.74 874.338 4 11 3 -4 7993.19 1062.51 2 -11 3 4 6661.75 1274.13 4 -11 3 3 13552.9 1615.35 4 11 3 -3 12391.4 1240.13 2 -11 -3 2 12826.8 1543.08 1 -11 3 2 10840.5 1469.85 4 11 3 -2 13097.7 1267.12 2 -11 -3 1 4166.18 1015.02 1 11 3 -1 7177.42 1066.04 2 -11 3 1 5698.64 1191.44 4 -11 -3 0 16841.7 1811.44 1 -11 3 0 17904.3 1747.22 4 11 3 0 14968.0 1346.30 2 -11 3 -1 1103.45 666.990 4 11 3 1 604.731 571.658 2 -11 -3 -2-2739.98 1133.85 1 -11 3 -2-1335.83 771.816 4 -11 -3 -3-1198.12 923.230 1 -11 3 -3 97.5167 567.308 4 -11 -3 -4-244.361 1033.93 1 -11 3 -4 1447.90 713.624 4 -11 3 -5 7614.04 1165.73 4 -11 3 -6 7983.86 1184.49 4 -11 3 -7 3610.04 895.696 4 -11 3 -7 7131.32 1229.19 1 -11 3 -8 10788.5 1425.56 1 -11 3 -8 10940.2 1283.95 4 -11 3 -8 8924.50 1154.95 3 -11 3 -9 1250.68 685.327 4 -11 3 -9 2861.54 804.585 3 -11 3 -10 4248.41 926.550 4 -11 3 -10 5072.79 935.218 3 -11 3 -11 1593.31 714.973 4 -11 3 -11-94.3634 568.514 3 -11 3 -12 570.323 693.723 3 11 4 -22 3702.09 944.585 2 11 4 -21 6330.90 1069.85 2 11 4 -20 1444.41 757.466 2 11 4 -19 652.186 690.509 2 11 4 -18 489.572 698.061 2 11 4 -17 1905.13 786.830 2 11 4 -16 574.721 591.938 2 11 4 -15 17489.0 1499.27 2 11 4 -14 3461.84 892.056 2 11 4 -13 14741.2 1396.80 2 -11 4 13 14532.5 1899.36 4 -11 4 12-94.0385 708.702 4 11 4 -12 194.008 541.142 2 -11 4 11 141.626 717.968 4 11 4 -11-114.649 518.002 2 -11 4 10-347.228 885.792 4 11 4 -10 241.254 513.603 2 -11 4 9 2372.26 1047.68 4 11 4 -9 3240.76 823.209 2 11 4 -8 1032.55 699.850 2 -11 4 8-233.300 758.117 4 11 4 -7 13519.9 1307.72 2 -11 4 7 13196.8 1715.38 4 11 4 -6 3362.07 819.357 2 -11 4 6 2735.34 1066.93 4 11 4 -5 27232.3 1802.18 2 -11 4 5 25488.1 2195.56 4 11 4 -4 2253.06 802.508 2 -11 4 4 4854.94 1233.79 4 11 4 -3 3445.34 755.060 2 -11 4 3 4774.66 1045.94 4 11 4 -2 910.453 742.606 2 -11 4 2 803.206 775.278 4 11 4 -1 1967.26 751.553 2 -11 4 1 4118.40 1123.99 4 11 4 0 1540.40 624.305 2 -11 4 0 1124.52 802.764 4 11 4 1 3987.89 865.734 2 -11 4 -1 5285.66 1057.09 4 11 4 2 695.863 643.717 2 -11 4 -2 16.3533 582.110 4 -11 4 -3 17960.5 1725.89 4 11 4 3 20212.3 1641.50 2 -11 4 -4 3524.40 928.144 4 -11 4 -5 5525.05 1079.29 4 -11 4 -6 637.652 798.964 4 -11 4 -7 1511.95 781.218 4 -11 4 -8 651.892 599.521 4 -11 4 -8 1239.22 764.600 3 -11 4 -9 3923.86 932.177 4 -11 4 -10 289.557 619.550 4 11 5 -15 1219.05 775.070 2 11 5 -14 755.639 672.283 2 11 5 -13-463.178 646.542 2 11 5 -12 9600.72 1160.48 2 11 5 -11 242.980 622.567 2 11 5 -10 17523.4 1526.64 2 11 5 -9 558.042 623.680 2 -11 5 8 6390.90 1346.42 4 11 5 -8 9166.85 1159.17 2 11 5 -7 843.647 707.248 2 -11 5 7-234.900 804.659 4 11 5 -6-323.469 593.659 2 -11 5 6-964.853 744.827 4 11 5 -5 507.858 544.461 2 -11 5 5 676.889 884.714 4 11 5 -4 7984.84 1153.54 2 -11 5 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-12 3 1 6506.48 1286.66 4 -12 3 0 3635.44 896.308 4 -12 3 -1 4750.67 1103.30 4 -12 3 -2 2643.35 921.462 4 -12 3 -3 1057.12 843.859 4 -12 3 -4 600.684 767.566 4 -12 3 -5 2356.97 858.403 4 -12 3 -6 5795.19 1106.14 4 -12 3 -7 1360.94 752.678 4 -12 3 -8 5232.68 1090.31 4 -12 3 -9 6925.72 1148.77 4 -12 4 -8 127.901 669.339 4 -13 0 2-406.767 742.432 1 -13 0 1 617.254 805.021 1 -13 0 0 2912.75 1010.10 1 -13 0 -1-352.119 828.947 1 -13 1 5 3237.75 1055.96 1 -13 1 4 2466.10 923.839 1 -13 1 3 9276.76 1343.31 1 -13 1 2 3775.30 1098.58 1 -13 1 1 11854.7 1526.09 1 -13 -1 -1 2844.36 1029.46 1 -13 -1 -2 508.243 881.735 1 13 2 -11 1396.01 711.316 2 0 0 0 0.00 0.00 0 TITL exp_3313 in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 9.735176 9.733150 27.461553 90.0000 97.7355 90.0000 ZERR 4.00 0.000238 0.000283 0.000815 0.0000 0.0025 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H B N P Cl Hg UNIT 111.00 80.00 4.00 15.00 4.00 1.00 4.00 TREF HKLF 4 END ; _shelx_hkl_checksum 64162