data_psu-963(md-691) _audit_creation_date 2019-06-29 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/1' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C18 H22 Br1.15 Cl0.85 N2 Pd' _chemical_formula_sum 'C18 H22 Br1.15 Cl0.85 N2 Pd' _chemical_formula_weight 494.69 _chemical_melting_point ? _chemical_oxdiff_formula 'C H N Br Pd' 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' 'Br' 'Br' -0.2901 2.4595 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pd' 'Pd' -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' 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 10.2263(17) _cell_length_b 12.604(3) _cell_length_c 14.912(3) _cell_angle_alpha 90 _cell_angle_beta 94.833(16) _cell_angle_gamma 90 _cell_volume 1915.2(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2666 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 28.7420 _cell_measurement_theta_min 4.1690 _shelx_estimated_absorpt_T_max 0.375 _shelx_estimated_absorpt_T_min 0.229 _exptl_absorpt_coefficient_mu 3.482 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.16123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear red' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier . _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.716 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description 'rect. Prism' _exptl_crystal_F_000 979 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.35 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0914 _diffrn_reflns_av_unetI/netI 0.1028 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.855 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 9004 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.855 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.205 _diffrn_reflns_theta_min 3.512 _diffrn_ambient_temperature 295.15 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.4752 _diffrn_detector_type Ruby _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.855 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 5.00 43.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -14.7103 57.0000 -120.0000 38 #__ type_ start__ end____ width___ exp.time_ 2 omega -5.00 24.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -14.7103 -99.0000 0.0000 29 #__ type_ start__ end____ width___ exp.time_ 3 omega 69.00 100.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - 14.1634 -178.0000 0.0000 31 #__ type_ start__ end____ width___ exp.time_ 4 omega -46.00 62.00 1.0000 9.0000 omega____ theta____ kappa____ phi______ frames - -14.7103 38.0000 150.0000 108 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'New Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0109687000 _diffrn_orient_matrix_UB_12 -0.0435316000 _diffrn_orient_matrix_UB_13 0.0298804000 _diffrn_orient_matrix_UB_21 -0.0018612000 _diffrn_orient_matrix_UB_22 0.0349905000 _diffrn_orient_matrix_UB_23 0.0371424000 _diffrn_orient_matrix_UB_31 -0.0686013000 _diffrn_orient_matrix_UB_32 -0.0080911000 _diffrn_orient_matrix_UB_33 -0.0002070000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 3084 _reflns_number_total 4434 _reflns_odcompleteness_completeness 99.66 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET) (compiled Mar 27 2014,17:12:48) ; _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 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 1.093 _refine_diff_density_min -1.287 _refine_diff_density_rms 0.152 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 4434 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0645 _refine_ls_restrained_S_all 1.023 _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^)+(0.0649P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1452 _refine_ls_wR_factor_ref 0.1654 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Others Sof(Cl2)=1-FVAR(1) Sof(Br2)=FVAR(1) Sof(Cl1)=1-FVAR(2) Sof(Br1)=FVAR(2) 3.a Ternary CH refined with riding coordinates: C13(H13), C16(H16) 3.b Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C3(H3), C4(H4), C6(H6), C9(H9), C10(H10), C11(H11) 3.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B, H18C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary ? 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 C1 C 0.2840(6) 0.5502(6) 0.1018(5) 0.0576(19) Uani 1 1 d . . . . . H1 H 0.293390 0.600533 0.057209 0.069 Uiso 1 1 calc R . . . . N1 N 0.3919(4) 0.5136(4) 0.1486(3) 0.0390(11) Uani 1 1 d . . . . . Pd1 Pd 0.58182(4) 0.55695(3) 0.13986(3) 0.03592(19) Uani 1 1 d . . . . . Br1 Br 0.5312(5) 0.6966(3) 0.0369(3) 0.0651(12) Uani 0.533(6) 1 d . . P A 1 Cl1 Cl 0.5384(15) 0.6880(11) 0.0351(9) 0.093(6) Uani 0.467(6) 1 d . . P A 2 C2 C 0.1600(6) 0.5166(6) 0.1167(5) 0.0579(18) Uani 1 1 d . . . . . H2 H 0.087505 0.543601 0.082265 0.070 Uiso 1 1 calc R . . . . N2 N 0.6051(4) 0.4435(3) 0.2356(3) 0.0352(11) Uani 1 1 d . . . . . Br2 Br 0.8126(5) 0.5880(5) 0.1327(5) 0.0593(11) Uani 0.615(5) 1 d . . P A 1 Cl2 Cl 0.7907(16) 0.6076(17) 0.1438(19) 0.053(3) Uani 0.385(5) 1 d . . P A 2 C3 C 0.1435(6) 0.4439(6) 0.1820(5) 0.0575(19) Uani 1 1 d . . . . . H3 H 0.059670 0.422499 0.193858 0.069 Uiso 1 1 calc R . . . . C4 C 0.2538(6) 0.4014(5) 0.2313(5) 0.0525(16) Uani 1 1 d . . . . . H4 H 0.245583 0.349409 0.274684 0.063 Uiso 1 1 calc R . . . . C5 C 0.3759(5) 0.4399(4) 0.2129(4) 0.0401(14) Uani 1 1 d . . . . . C6 C 0.4980(5) 0.4036(4) 0.2583(4) 0.0393(13) Uani 1 1 d . . . . . H6 H 0.498566 0.352228 0.303142 0.047 Uiso 1 1 calc R . . . . C7 C 0.7297(5) 0.4058(4) 0.2788(4) 0.0321(12) Uani 1 1 d . . . . . C8 C 0.7878(5) 0.3207(4) 0.2384(4) 0.0361(12) Uani 1 1 d . . . . . C9 C 0.9033(6) 0.2811(5) 0.2819(4) 0.0480(15) Uani 1 1 d . . . . . H9 H 0.944792 0.223579 0.257369 0.058 Uiso 1 1 calc R . . . . C10 C 0.9567(6) 0.3258(5) 0.3603(4) 0.0496(16) Uani 1 1 d . . . . . H10 H 1.032410 0.297225 0.389740 0.060 Uiso 1 1 calc R . . . . C11 C 0.8987(6) 0.4127(6) 0.3954(4) 0.0513(17) Uani 1 1 d . . . . . H11 H 0.937616 0.443605 0.447676 0.062 Uiso 1 1 calc R . . . . C12 C 0.7825(6) 0.4562(4) 0.3550(4) 0.0417(14) Uani 1 1 d . . . . . C13 C 0.7201(6) 0.5513(5) 0.3957(5) 0.0542(18) Uani 1 1 d . . . . . H13 H 0.639866 0.568249 0.357767 0.065 Uiso 1 1 calc R . . . . C14 C 0.6819(9) 0.5305(7) 0.4894(7) 0.096(3) Uani 1 1 d . . . . . H14A H 0.621215 0.472333 0.488207 0.145 Uiso 1 1 calc GR . . . . H14B H 0.641292 0.592788 0.511689 0.145 Uiso 1 1 calc GR . . . . H14C H 0.758773 0.513287 0.528062 0.145 Uiso 1 1 calc GR . . . . C15 C 0.8091(8) 0.6492(6) 0.3979(6) 0.082(3) Uani 1 1 d . . . . . H15A H 0.829059 0.666302 0.337846 0.123 Uiso 1 1 calc GR . . . . H15B H 0.888938 0.634605 0.434365 0.123 Uiso 1 1 calc GR . . . . H15C H 0.764940 0.708055 0.422949 0.123 Uiso 1 1 calc GR . . . . C16 C 0.7294(6) 0.2746(5) 0.1518(4) 0.0455(15) Uani 1 1 d . . . . . H16 H 0.671464 0.328790 0.123007 0.055 Uiso 1 1 calc R . . . . C17 C 0.8292(7) 0.2482(7) 0.0869(5) 0.068(2) Uani 1 1 d . . . . . H17A H 0.879920 0.310278 0.076155 0.102 Uiso 1 1 calc GR . . . . H17B H 0.785165 0.224132 0.031210 0.102 Uiso 1 1 calc GR . . . . H17C H 0.886235 0.193261 0.111891 0.102 Uiso 1 1 calc GR . . . . C18 C 0.6449(8) 0.1789(6) 0.1674(5) 0.071(2) Uani 1 1 d . . . . . H18A H 0.698665 0.123043 0.194275 0.107 Uiso 1 1 calc GR . . . . H18B H 0.603065 0.154994 0.110937 0.107 Uiso 1 1 calc GR . . . . H18C H 0.579180 0.197921 0.206867 0.107 Uiso 1 1 calc GR . . . . 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 C1 0.037(3) 0.079(5) 0.055(4) 0.009(4) -0.009(3) 0.003(3) N1 0.031(2) 0.046(3) 0.038(3) -0.005(2) -0.005(2) -0.002(2) Pd1 0.0268(3) 0.0403(3) 0.0403(3) 0.00594(19) 0.0013(2) -0.00287(17) Br1 0.0558(19) 0.0550(13) 0.081(3) 0.0293(14) -0.0120(16) -0.0107(12) Cl1 0.087(9) 0.124(10) 0.071(7) 0.067(6) 0.019(5) 0.025(6) C2 0.028(3) 0.078(5) 0.068(5) 0.005(4) 0.003(3) 0.007(3) N2 0.031(2) 0.034(2) 0.040(3) 0.000(2) -0.002(2) -0.0016(19) Br2 0.0267(17) 0.079(2) 0.0731(18) 0.0190(15) 0.0089(12) -0.0036(12) Cl2 0.015(4) 0.063(6) 0.081(7) 0.013(5) 0.011(4) -0.011(5) C3 0.026(3) 0.076(5) 0.071(5) -0.006(4) 0.009(3) -0.013(3) C4 0.035(3) 0.057(4) 0.067(5) 0.002(4) 0.008(3) -0.012(3) C5 0.034(3) 0.035(3) 0.052(4) -0.007(3) 0.001(3) -0.004(2) C6 0.037(3) 0.034(3) 0.047(4) 0.010(3) 0.007(3) -0.007(2) C7 0.028(3) 0.029(3) 0.039(3) 0.003(2) -0.001(2) 0.000(2) C8 0.036(3) 0.037(3) 0.035(3) 0.010(2) -0.002(2) 0.005(2) C9 0.038(3) 0.054(4) 0.053(4) 0.005(3) 0.007(3) 0.015(3) C10 0.038(3) 0.054(4) 0.056(4) 0.012(3) -0.002(3) 0.013(3) C11 0.044(4) 0.064(4) 0.043(4) 0.002(3) -0.019(3) 0.009(3) C12 0.038(3) 0.035(3) 0.052(4) -0.006(3) 0.003(3) 0.000(2) C13 0.045(4) 0.054(4) 0.059(4) -0.004(3) -0.016(3) 0.007(3) C14 0.107(7) 0.067(5) 0.124(8) 0.019(6) 0.061(6) 0.028(5) C15 0.103(6) 0.046(4) 0.097(7) -0.016(4) 0.016(5) 0.003(4) C16 0.037(3) 0.050(4) 0.050(4) 0.002(3) 0.004(3) 0.005(3) C17 0.062(4) 0.087(6) 0.055(5) -0.012(4) 0.007(4) 0.005(4) C18 0.085(5) 0.063(5) 0.065(5) -0.002(4) -0.001(4) -0.026(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.337(7) . ? C1 C2 1.373(9) . ? N1 Pd1 2.032(4) . ? N1 C5 1.356(8) . ? Pd1 Br1 2.364(4) . ? Pd1 Cl1 2.291(12) . ? Pd1 N2 2.021(5) . ? Pd1 Br2 2.404(5) . ? Pd1 Cl2 2.225(17) . ? C2 C3 1.358(10) . ? N2 C6 1.277(7) . ? N2 C7 1.457(6) . ? C3 C4 1.400(9) . ? C4 C5 1.388(8) . ? C5 C6 1.443(8) . ? C7 C8 1.388(7) . ? C7 C12 1.372(8) . ? C8 C9 1.391(8) . ? C8 C16 1.493(8) . ? C9 C10 1.370(9) . ? C10 C11 1.370(9) . ? C11 C12 1.398(8) . ? C12 C13 1.509(8) . ? C13 C14 1.505(11) . ? C13 C15 1.532(9) . ? C16 C17 1.501(9) . ? C16 C18 1.513(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 122.8(7) . . ? C1 N1 Pd1 128.7(5) . . ? C1 N1 C5 117.5(5) . . ? C5 N1 Pd1 113.7(4) . . ? N1 Pd1 Br1 94.80(17) . . ? N1 Pd1 Cl1 96.1(4) . . ? N1 Pd1 Br2 173.7(2) . . ? N1 Pd1 Cl2 174.7(7) . . ? Br1 Pd1 Br2 90.7(2) . . ? N2 Pd1 N1 79.68(18) . . ? N2 Pd1 Br1 172.79(19) . . ? N2 Pd1 Cl1 175.2(4) . . ? N2 Pd1 Br2 95.1(2) . . ? N2 Pd1 Cl2 97.4(7) . . ? Cl2 Pd1 Cl1 86.6(8) . . ? C3 C2 C1 119.8(6) . . ? C6 N2 Pd1 114.4(4) . . ? C6 N2 C7 119.5(5) . . ? C7 N2 Pd1 126.1(3) . . ? C2 C3 C4 119.4(6) . . ? C5 C4 C3 117.5(6) . . ? N1 C5 C4 122.9(6) . . ? N1 C5 C6 113.5(5) . . ? C4 C5 C6 123.6(6) . . ? N2 C6 C5 118.6(5) . . ? C8 C7 N2 116.8(5) . . ? C12 C7 N2 118.9(5) . . ? C12 C7 C8 124.3(5) . . ? C7 C8 C9 116.9(5) . . ? C7 C8 C16 121.4(5) . . ? C9 C8 C16 121.7(5) . . ? C10 C9 C8 120.8(6) . . ? C9 C10 C11 120.1(6) . . ? C10 C11 C12 121.8(6) . . ? C7 C12 C11 115.9(5) . . ? C7 C12 C13 123.4(5) . . ? C11 C12 C13 120.7(6) . . ? C12 C13 C15 112.2(6) . . ? C14 C13 C12 112.8(6) . . ? C14 C13 C15 108.6(7) . . ? C8 C16 C17 113.6(5) . . ? C8 C16 C18 111.7(5) . . ? C17 C16 C18 110.5(6) . . ? _shelx_res_file ; TITL PSU-963(Md-691) in P21/c #14 psu-963(md-691).res created by SHELXL-2018/1 at 22:43:20 on 29-Jun-2019 REM reset to P21/c #14 CELL 0.71073 10.22631 12.60395 14.91192 90 94.8333 90 ZERR 4 0.0017 0.00264 0.00286 0 0.0162 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br Cl N Pd UNIT 72 88 4.59 3.41 8 4 L.S. 10 PLAN 20 SIZE 0.35 0.45 0.6 TEMP 22 BOND fmap 2 acta 52 REM REM REM WGHT 0.064900 FVAR 3.62973 0.61461 0.53286 C1 1 0.284028 0.550170 0.101796 11.00000 0.03679 0.07866 = 0.05517 0.00866 -0.00898 0.00325 AFIX 43 H1 2 0.293390 0.600533 0.057209 11.00000 -1.20000 AFIX 0 N1 5 0.391925 0.513579 0.148571 11.00000 0.03118 0.04634 = 0.03812 -0.00473 -0.00462 -0.00154 PD1 6 0.581822 0.556950 0.139860 11.00000 0.02682 0.04034 = 0.04034 0.00594 0.00126 -0.00287 PART 1 BR1 3 0.531219 0.696610 0.036909 31.00000 0.05580 0.05503 = 0.08134 0.02925 -0.01199 -0.01074 PART 0 PART 2 CL1 4 0.538397 0.688018 0.035113 -31.00000 0.08719 0.12433 = 0.07060 0.06711 0.01855 0.02514 PART 0 C2 1 0.159979 0.516618 0.116731 11.00000 0.02795 0.07815 = 0.06757 0.00509 0.00332 0.00730 AFIX 43 H2 2 0.087505 0.543601 0.082265 11.00000 -1.20000 AFIX 0 N2 5 0.605105 0.443491 0.235608 11.00000 0.03061 0.03378 = 0.04036 0.00043 -0.00158 -0.00158 PART 1 BR2 3 0.812604 0.588035 0.132740 21.00000 0.02666 0.07895 = 0.07314 0.01899 0.00890 -0.00362 PART 0 PART 2 CL2 4 0.790665 0.607612 0.143795 -21.00000 0.01528 0.06327 = 0.08067 0.01267 0.01050 -0.01097 PART 0 C3 1 0.143520 0.443906 0.181996 11.00000 0.02569 0.07634 = 0.07132 -0.00586 0.00908 -0.01289 AFIX 43 H3 2 0.059670 0.422499 0.193858 11.00000 -1.20000 AFIX 0 C4 1 0.253807 0.401427 0.231286 11.00000 0.03473 0.05665 = 0.06665 0.00174 0.00763 -0.01211 AFIX 43 H4 2 0.245583 0.349409 0.274684 11.00000 -1.20000 AFIX 0 C5 1 0.375908 0.439881 0.212938 11.00000 0.03360 0.03483 = 0.05155 -0.00681 0.00131 -0.00350 C6 1 0.497958 0.403578 0.258323 11.00000 0.03669 0.03443 = 0.04749 0.01004 0.00693 -0.00718 AFIX 43 H6 2 0.498566 0.352228 0.303142 11.00000 -1.20000 AFIX 0 C7 1 0.729652 0.405786 0.278751 11.00000 0.02764 0.02890 = 0.03929 0.00263 -0.00076 -0.00010 C8 1 0.787759 0.320669 0.238393 11.00000 0.03609 0.03667 = 0.03457 0.01004 -0.00191 0.00477 C9 1 0.903311 0.281092 0.281862 11.00000 0.03769 0.05386 = 0.05284 0.00473 0.00661 0.01467 AFIX 43 H9 2 0.944792 0.223579 0.257369 11.00000 -1.20000 AFIX 0 C10 1 0.956699 0.325833 0.360302 11.00000 0.03807 0.05403 = 0.05574 0.01210 -0.00232 0.01317 AFIX 43 H10 2 1.032410 0.297225 0.389740 11.00000 -1.20000 AFIX 0 C11 1 0.898653 0.412706 0.395439 11.00000 0.04362 0.06369 = 0.04273 0.00163 -0.01866 0.00859 AFIX 43 H11 2 0.937616 0.443605 0.447676 11.00000 -1.20000 AFIX 0 C12 1 0.782507 0.456180 0.354955 11.00000 0.03800 0.03512 = 0.05177 -0.00644 0.00320 -0.00017 C13 1 0.720094 0.551260 0.395678 11.00000 0.04536 0.05447 = 0.05934 -0.00356 -0.01620 0.00658 AFIX 13 H13 2 0.639866 0.568249 0.357767 11.00000 -1.20000 AFIX 0 C14 1 0.681883 0.530541 0.489397 11.00000 0.10746 0.06657 = 0.12387 0.01930 0.06119 0.02835 AFIX 137 H14A 2 0.621215 0.472333 0.488207 11.00000 -1.50000 H14B 2 0.641292 0.592788 0.511689 11.00000 -1.50000 H14C 2 0.758773 0.513287 0.528062 11.00000 -1.50000 AFIX 0 C15 1 0.809064 0.649199 0.397919 11.00000 0.10271 0.04642 = 0.09733 -0.01650 0.01644 0.00273 AFIX 137 H15A 2 0.829059 0.666302 0.337846 11.00000 -1.50000 H15B 2 0.888938 0.634605 0.434365 11.00000 -1.50000 H15C 2 0.764940 0.708055 0.422949 11.00000 -1.50000 AFIX 0 C16 1 0.729442 0.274565 0.151829 11.00000 0.03732 0.04985 = 0.04960 0.00152 0.00449 0.00454 AFIX 13 H16 2 0.671464 0.328790 0.123007 11.00000 -1.20000 AFIX 0 C17 1 0.829182 0.248181 0.086920 11.00000 0.06207 0.08728 = 0.05486 -0.01162 0.00667 0.00469 AFIX 137 H17A 2 0.879920 0.310278 0.076155 11.00000 -1.50000 H17B 2 0.785165 0.224132 0.031210 11.00000 -1.50000 H17C 2 0.886235 0.193261 0.111891 11.00000 -1.50000 AFIX 0 C18 1 0.644855 0.178884 0.167400 11.00000 0.08463 0.06327 = 0.06483 -0.00171 -0.00081 -0.02623 AFIX 137 H18A 2 0.698665 0.123043 0.194275 11.00000 -1.50000 H18B 2 0.603065 0.154994 0.110937 11.00000 -1.50000 H18C 2 0.579180 0.197921 0.206867 11.00000 -1.50000 AFIX 0 HKLF 4 REM PSU-963(Md-691) in P21/c #14 REM R1 = 0.0645 for 3084 Fo > 4sig(Fo) and 0.0948 for all 4434 data REM 232 parameters refined using 0 restraints END WGHT 0.0649 0.0000 REM Highest difference peak 1.093, deepest hole -1.287, 1-sigma level 0.152 Q1 1 0.6453 0.5004 0.0937 11.00000 0.05 0.96 Q2 1 0.6278 0.5982 0.0998 11.00000 0.05 0.90 Q3 1 0.6960 0.5696 0.1254 11.00000 0.05 0.85 Q4 1 0.4774 0.5431 0.1340 11.00000 0.05 0.81 Q5 1 0.5420 0.4732 0.1024 11.00000 0.05 0.76 Q6 1 0.5551 0.4400 0.1026 11.00000 0.05 0.74 Q7 1 0.4664 0.7583 0.0834 11.00000 0.05 0.74 Q8 1 0.6221 0.4676 0.1844 11.00000 0.05 0.72 Q9 1 0.5416 0.1231 0.2951 11.00000 0.05 0.66 Q10 1 0.6173 0.6605 0.1793 11.00000 0.05 0.64 Q11 1 0.4758 0.4768 0.2085 11.00000 0.05 0.63 Q12 1 0.5163 0.6178 0.1865 11.00000 0.05 0.60 Q13 1 0.7637 0.5464 0.1739 11.00000 0.05 0.60 Q14 1 0.5090 0.5623 -0.0051 11.00000 0.05 0.57 Q15 1 0.4950 0.5594 0.2973 11.00000 0.05 0.57 Q16 1 0.3288 0.4397 0.0136 11.00000 0.05 0.57 Q17 1 0.5018 0.4624 0.2202 11.00000 0.05 0.55 Q18 1 0.5017 0.5945 0.1155 11.00000 0.05 0.55 Q19 1 0.5572 0.4967 0.0271 11.00000 0.05 0.54 Q20 1 0.6661 0.5943 0.1645 11.00000 0.05 0.53 ; _shelx_res_checksum 58146 _shelx_hkl_file ; 0 0 3 271.072 173.456 4 0 0 -3 68.9776 124.756 4 0 0 -4 551792. 8977.61 4 0 0 -4 551248. 6237.81 2 0 0 -5 373.274 287.158 1 0 0 -5 330.417 255.552 4 0 0 5 821.217 406.760 4 0 0 -5 563.080 219.733 2 0 0 -6 43842.8 2009.42 2 0 0 -6 47612.1 3127.46 4 0 0 -7 50.9012 180.281 2 0 0 -7-116.186 197.723 1 0 0 -7 20.3797 170.985 4 0 0 -8 249897. 12036.7 1 0 0 -8 367393. 9786.36 4 0 0 -9 862.323 694.224 4 0 0 -9 169.801 535.450 1 0 0 -10 108724. 8386.32 1 0 0 -11-379.194 699.653 1 0 0 -12 31173.7 4863.98 1 0 0 -13 227.636 952.401 1 0 0 -14 22293.7 4533.36 1 0 0 -15 602.331 800.630 1 0 0 -16 1720.91 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3245.45 969.314 2 2 2 -13 3058.55 1241.15 1 -2 2 12 582.429 361.367 4 2 2 -12 652.897 737.915 1 -2 2 11 6080.35 1533.65 4 2 2 -11 4129.33 1524.17 1 -2 2 10 694.277 109.005 4 2 2 -10 785.253 742.769 1 2 2 -9 18351.6 2839.17 1 -2 2 9 26815.6 2981.13 4 -2 2 8 9105.34 1632.30 4 2 2 -8 7457.22 1747.06 1 2 -2 -8 14448.1 2372.48 4 2 2 -8 10198.6 1850.69 4 2 2 -8 7897.70 1524.05 2 2 2 -7 8302.25 1887.03 1 2 -2 -7 12284.4 2123.61 4 -2 2 7 10875.9 1652.50 4 2 2 -7 8818.26 1662.91 4 2 2 -7 8044.69 1532.60 2 2 2 -6 49778.2 3772.93 4 2 2 -6 41257.9 3410.11 2 2 2 -6 40339.8 3919.80 1 -2 2 6 44765.1 3113.16 4 2 2 -5 13839.7 1871.43 4 -2 2 5 13165.2 1598.21 4 2 2 -5 11264.9 1777.70 2 -2 -2 5 17109.2 1946.92 2 2 -2 -5 18662.3 2197.14 4 -2 2 4 38471.4 2476.70 4 2 2 -4 32764.4 2795.20 2 -2 -2 4 46040.1 3353.10 2 2 -2 -4 48140.2 3162.58 4 2 2 -4 39510.1 2866.32 4 2 -2 -3 12566.9 1462.22 4 -2 -2 3 10527.8 1497.05 2 2 2 -3 8070.50 808.695 3 -2 2 3 9136.13 1191.64 4 2 2 -3 6824.92 1232.69 2 2 -2 -2 6776.12 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2498.53 3 -2 2 -6 76407.4 4733.06 1 2 -2 6 128469. 5808.30 1 -2 -2 -6 57268.3 5430.89 1 -2 -2 -6 102194. 4281.65 4 -2 -2 -6 91137.0 2840.42 2 2 2 6 107769. 4524.37 4 -2 -2 -7 67656.5 3802.93 4 -2 -2 -7 36585.5 4571.73 1 2 2 7 71720.2 4079.97 4 2 -2 7 75397.8 4722.03 1 -2 2 -7 41675.0 3817.19 1 -2 2 -8 1126.50 1009.97 1 -2 -2 -8 955.490 509.912 4 -2 -2 -8 471.783 558.422 1 2 2 8 1302.27 608.534 4 -2 2 -9 1529.00 577.411 4 2 -2 9 2541.54 419.861 2 -2 -2 -9 1345.92 1026.96 1 -2 2 -9 1991.48 1139.70 1 -2 -2 -9 2566.52 859.537 4 -2 -2 -10 8119.27 2467.53 1 -2 -2 -10 12994.8 2054.53 4 -2 2 -10 5955.01 1704.61 1 -2 -2 -11 6367.08 2176.64 1 -2 2 -11 4744.65 1593.70 1 -2 2 -12 13351.5 2948.44 1 -2 -2 -12 20524.8 4326.55 1 -2 2 -13-41.2922 114.372 1 -2 -2 -13 290.240 1051.27 1 -2 -2 -14 10664.1 3408.28 1 -2 2 -14 6497.83 2222.63 1 -2 2 -15 3788.19 1601.85 1 -2 -2 -15 5978.21 2484.91 1 -2 -2 -16 2229.71 1737.94 1 -2 2 -16 871.011 571.781 1 -2 2 -17-338.783 1099.20 1 -2 -2 -17 2937.35 1968.06 1 -2 2 -18 391.029 627.324 1 -2 -2 -18 2632.47 1779.84 1 2 3 -19 226.662 508.833 1 2 -3 -18 2889.63 1617.84 1 2 3 -18 3688.12 1717.03 1 2 -3 -17 1382.20 1215.80 1 2 3 -17 771.633 664.557 1 2 -3 -16 2247.11 1588.08 1 2 3 -16 1663.52 1231.41 1 -2 3 16 4703.77 1910.04 4 -2 3 15 9517.54 2334.48 4 2 3 -15 5655.44 2106.32 1 2 3 -14 7457.49 2271.81 1 2 -3 -14 8148.23 1456.20 2 -2 3 14 8517.45 2094.68 4 -2 3 13 2595.93 956.355 4 2 3 -13 2492.47 1179.29 1 2 3 -12 202.998 184.194 1 -2 3 12 335.873 529.380 4 2 3 -11 7467.08 1950.24 1 -2 3 11 9301.60 1785.02 4 -2 3 10 3822.17 1089.05 4 2 3 -10 3030.83 1149.57 1 2 3 -9 12267.9 2239.83 1 -2 3 9 15470.5 2083.00 4 2 3 -8 15811.9 2308.01 1 -2 3 8 20948.5 2283.06 4 -2 -3 7 2899.39 673.093 2 2 3 -7 2587.74 954.164 4 -2 3 7 2744.93 738.483 4 2 -3 -7 3574.41 1000.98 4 2 3 -7 1004.13 796.783 1 2 -3 -6 89107.2 5092.81 4 -2 3 6 65477.7 3684.44 4 -2 -3 6 92266.6 5182.35 2 2 3 -6 53321.6 3535.28 1 -2 -3 5 97875.3 5265.02 2 -2 3 5 60611.1 3368.26 4 2 -3 -5 93697.6 5032.03 4 2 3 -5 59139.5 3034.97 1 -2 3 4 26749.3 2248.37 4 2 3 -4 26294.5 1501.29 1 2 -3 -4 35246.4 2858.88 4 -2 -3 4 37299.6 3084.53 2 2 3 -4 24999.0 1344.58 3 -2 -3 3 117505. 5449.33 2 2 3 -3 81748.1 2407.56 3 2 -3 -3 103583. 4363.28 4 -2 3 3 76521.9 3408.10 4 2 -3 -2 23496.2 1905.61 4 -2 3 2 21270.7 1816.69 4 -2 -3 2 21487.3 1250.51 3 2 -3 -1 78332.3 3251.16 4 -2 -3 1 73996.5 2485.07 3 -2 -3 0 5844.73 886.778 1 -2 3 0 4267.58 693.073 4 -2 -3 0 5408.99 1172.91 2 2 -3 0 5416.80 801.796 4 2 3 1 130652. 2733.13 4 -2 3 -1 121849. 3925.32 4 2 -3 2 16877.6 1089.63 3 2 3 2 15456.2 959.853 4 -2 -3 -3 158589. 3626.10 4 2 3 3 150069. 3327.31 4 2 -3 3 158490. 3351.02 3 -2 -3 -4 106289. 7731.98 1 -2 -3 -4 136513. 3923.86 4 2 -3 4 138539. 4636.91 1 -2 3 -4 118717. 3430.16 3 2 3 4 120352. 3221.24 4 -2 -3 -5 19963.0 1718.44 4 2 3 5 16932.5 1359.77 4 -2 3 -5 16845.6 1386.99 3 -2 -3 -5 15062.7 3003.97 1 -2 -3 -6 4623.93 1731.67 1 2 3 6 5789.58 926.963 4 -2 -3 -6 8065.97 1193.16 4 2 -3 6 5719.31 1137.21 1 -2 3 -6 4762.86 768.358 3 -2 3 -7 69721.2 3399.01 3 -2 -3 -7 52323.9 6150.77 1 2 3 7 78378.8 3891.40 4 2 -3 7 106048. 5557.56 1 -2 -3 -7 76161.2 3304.44 2 -2 -3 -7 84828.5 4257.83 4 -2 -3 -8 6382.41 2119.40 1 -2 -3 -8 9648.12 1005.48 2 -2 -3 -8 12289.2 1780.23 4 2 3 8 10584.4 1540.93 4 -2 -3 -9 1392.26 1053.37 1 2 3 9 2774.79 736.496 4 -2 -3 -9 3965.44 1058.89 4 -2 -3 -9 2454.69 399.009 2 2 3 10 16605.9 2295.87 4 -2 -3 -10 7209.20 2252.13 1 2 -3 10 12771.7 1101.67 2 -2 3 -10 7714.49 2108.03 1 -2 -3 -10 14964.1 2199.49 4 -2 -3 -11-188.442 398.250 1 -2 3 -11 677.269 954.573 1 -2 -3 -11 798.160 522.374 4 2 -3 11 951.778 247.820 2 -2 -3 -12 1914.77 1191.06 1 -2 3 -12 1585.71 816.925 1 -2 -3 -13 16389.6 4005.10 1 -2 3 -13 13533.2 3020.25 1 -2 3 -14 6764.17 2180.29 1 -2 -3 -14 12803.6 3743.47 1 -2 -3 -15 3363.82 1970.98 1 -2 3 -15 1939.97 1331.23 1 -2 3 -16-873.985 1303.11 1 -2 -3 -16 1887.35 1869.30 1 -2 -3 -17 2461.25 1980.51 1 -2 3 -17 397.062 1347.60 1 2 4 -19-261.744 428.046 1 2 -4 -18 3313.21 2498.27 1 2 4 -18 109.100 434.141 1 2 -4 -17 16523.6 4279.50 1 -2 4 17 19560.3 3412.99 4 2 4 -17 10902.7 2915.14 1 -2 4 16 1525.69 1065.95 4 2 4 -16 681.372 713.729 1 2 4 -15 1735.46 1005.95 1 -2 4 15 1337.60 756.171 4 2 4 -14 659.172 710.300 1 -2 4 14-638.762 890.254 4 -2 4 13 35308.9 3807.19 4 2 4 -13 26311.7 4001.54 1 2 4 -12 14980.7 2872.17 1 -2 4 12 20412.4 2703.16 4 2 4 -11 2586.94 1007.06 1 -2 4 11 3398.44 1085.26 4 -2 4 10 196.535 246.642 4 2 4 -10 16.6218 252.314 1 -2 -4 10 588.611 218.751 2 2 4 -9 455.797 531.488 1 -2 4 9-279.728 452.431 4 -2 -4 9-263.014 615.732 2 -2 -4 8 4874.02 1253.23 2 2 4 -8 3718.19 1046.37 1 -2 4 8 3541.38 964.398 4 2 -4 -7 77849.5 5546.01 4 -2 4 7 46804.5 3341.75 4 -2 -4 7 75726.5 4787.51 2 2 4 -7 43204.6 3003.04 1 -2 4 6 2732.73 756.840 4 2 4 -6 2699.60 454.996 3 2 4 -6 3641.50 840.357 1 -2 -4 6 4345.46 1187.12 2 2 -4 -6 5125.94 1327.48 4 -2 4 5 71258.3 4014.31 4 2 4 -5 69806.6 2177.89 3 -2 -4 5 104561. 5529.47 2 2 -4 -5 97079.8 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632.671 1 2 4 10 23149.1 2572.07 4 -2 -4 -10 22694.7 1597.54 2 -2 4 -10 22987.6 2247.72 3 -2 -4 -10 16872.7 3676.04 1 -2 4 -11 59747.5 3933.73 3 2 -4 11 60057.4 2754.63 2 2 4 11 66867.9 4790.06 4 2 4 12 50.9293 404.754 4 2 -4 12-3.44129 132.436 2 -2 -4 -12 256.832 283.024 1 -2 -4 -13 669.650 67.2063 1 -2 -4 -14 2706.45 1280.88 1 -2 -4 -15 33260.9 5604.23 1 -2 -4 -16 1783.70 1783.21 1 -2 -4 -17 1520.32 1537.34 1 -2 5 18 2704.42 1443.91 4 2 5 -18 1004.72 1166.30 1 2 5 -17-519.264 907.616 1 -2 5 17-81.3640 458.310 4 2 5 -16 2362.25 1289.95 1 -2 5 16 3166.27 1171.49 4 2 5 -15 2787.35 1139.68 1 -2 5 15 3394.09 1131.64 4 -2 5 14 22274.1 3050.76 4 2 5 -14 15832.2 2884.91 1 2 5 -13 2610.03 1097.62 1 -2 5 13 3415.88 1002.43 4 -2 5 12 1273.53 491.668 4 2 5 -12 410.207 587.285 1 2 5 -11 785.512 821.977 1 -2 5 11 56.6026 408.311 4 2 5 -10 8998.20 1820.44 1 -2 5 10 8823.68 1611.68 4 -2 5 9-316.692 427.557 4 2 5 -9 215.122 104.213 3 -2 5 8 2721.00 836.123 4 -2 -5 8 3781.07 1193.83 2 2 5 -8 2848.36 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3 11 1676.10 1210.99 4 10 3 -10 911.399 1165.16 2 -10 3 10-212.513 625.052 4 10 3 -9 4319.25 1928.61 2 -10 3 9 6897.89 1968.89 4 -10 3 8 16772.5 3185.36 4 10 3 -8 13334.6 3569.82 2 -10 3 7 263.768 653.027 4 10 3 -7-164.556 646.298 2 -10 3 6 4109.53 1402.76 4 10 3 -6 3699.68 1875.98 2 -10 3 5 2571.06 1080.67 4 10 3 -5 1351.46 1128.34 2 -10 3 4 9063.51 2127.34 4 10 3 -4 5997.67 2294.90 2 -10 3 3 4743.91 1535.74 4 10 3 -3 2928.48 1441.95 2 -10 3 2 31103.2 3628.84 4 10 3 -2 21687.6 4051.00 2 -10 3 1 2686.36 1036.82 4 10 3 -1 1896.81 1243.67 2 -10 3 0 12166.7 2279.30 4 10 3 0 10121.7 2459.55 2 -10 3 -1 13471.2 2196.42 4 10 3 1 9865.14 2305.97 2 -10 3 -2 31599.7 3311.85 4 -10 -3 -2 39397.7 4967.79 3 10 3 3 6869.23 1822.64 2 -10 -3 -3 9733.91 2693.54 3 10 3 4 795.321 560.358 2 -10 -3 -4 1974.86 1522.69 3 10 3 5 580.800 591.769 2 -10 -3 -5 1973.71 1309.42 3 10 3 6 19846.5 2541.26 2 -10 -3 -6 31889.9 4877.31 3 -10 -3 -7 1977.67 1493.63 3 -10 -3 -8 956.705 1456.14 3 -10 -3 -9 8322.02 2698.59 3 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2 -10 -4 -5 2875.17 1724.17 3 -10 -4 -6 4250.40 1999.17 3 -10 -4 -7 14588.6 3503.86 3 -10 -4 -8 668.977 1061.11 3 -10 -4 -9 10952.4 3412.39 3 -10 5 12 1299.74 799.852 4 10 5 -11 829.997 993.660 2 -10 5 11 1108.85 575.348 4 10 5 -10 120.354 712.571 2 -10 5 10 523.020 242.104 4 10 5 -9-248.581 536.448 2 -10 5 9 153.953 589.156 4 10 5 -8 13577.5 3569.01 2 -10 5 8 13142.5 2826.33 4 10 5 -7 239.754 632.647 2 -10 5 7 839.008 900.655 4 10 5 -6-458.232 733.616 2 -10 5 6 291.653 589.021 4 10 5 -5 1485.69 1038.14 2 -10 5 5 3505.14 1551.12 4 -10 5 4 15544.5 2962.08 4 10 5 -4 12879.4 3269.42 2 10 5 -3 2749.66 1755.95 2 -10 5 3 3973.47 1471.94 4 10 5 -2 7236.60 2304.04 2 -10 5 2 7404.26 1870.27 4 10 5 -1 4745.61 1900.32 2 -10 5 1 5972.16 1723.23 4 -10 5 0 24393.6 3454.88 4 10 5 0 17440.4 3279.45 2 -10 -5 -1 4978.78 1985.00 3 10 5 1 3492.68 1438.67 2 -10 5 -1 1775.22 682.647 4 -10 5 -2 17368.1 2845.93 4 -10 -5 -2 21836.6 3806.45 3 -10 -5 -3 1570.80 1665.57 3 -10 5 -3 814.508 884.304 4 -10 -5 -4 10695.7 2842.52 3 -10 5 -4 7571.83 1932.28 4 -10 -5 -5 1760.26 1814.68 3 -10 -5 -6 17889.5 3889.69 3 -10 -5 -7 11294.0 3174.77 3 -10 -5 -8 2794.40 2017.32 3 -10 6 11 4067.28 1575.69 4 -10 6 10 2373.28 1192.07 4 -10 6 9-52.0987 781.210 4 -10 6 8 407.526 533.015 4 -10 6 7 11868.8 2665.84 4 -10 6 6 1625.29 1124.85 4 -10 6 5 13343.0 2743.66 4 -10 6 4 3539.32 1367.68 4 -10 6 3 10911.2 2427.83 4 -10 6 2 565.781 640.461 4 -10 6 1 3761.28 1290.30 4 -10 6 0 12867.4 2495.32 4 -10 -6 0 19277.1 3571.72 3 -10 -6 -1 4119.37 1827.04 3 -10 6 -1 2481.18 1256.62 4 -10 -6 -2 2446.95 1677.57 3 -10 6 -2 1440.53 885.335 4 -10 6 -3 26482.3 3827.64 4 -10 -6 -3 40268.3 5279.13 3 -10 -6 -4 12109.4 3132.88 3 -10 6 -4 8148.57 2100.98 4 -10 -6 -5 231.032 951.551 3 -10 -6 -6 882.009 1290.94 3 -10 -6 -7 19987.7 4276.45 3 -10 7 10 5542.39 1959.85 4 -10 7 9 828.098 775.838 4 -10 7 8 4778.82 1831.52 4 -10 7 7 4758.88 1732.61 4 -10 7 6 652.612 735.627 4 -10 7 5 3425.96 1471.04 4 -10 7 4 10655.6 2421.61 4 -10 7 3 2491.97 858.351 4 -10 7 2 971.095 425.579 4 -10 7 1-304.150 1096.17 4 -10 -7 1 1645.23 1542.88 3 -10 -7 0 3507.78 1732.51 3 -10 7 0 3121.79 1440.04 4 -10 -7 -1 8588.86 2588.03 3 -10 7 -1 4954.59 1735.05 4 -10 -7 -2 2094.05 1416.95 3 -10 7 -2 520.713 806.837 4 -10 -7 -3 3140.32 2037.22 3 -10 7 -3 1475.84 1089.18 4 -10 7 -4 7885.72 2378.96 4 -10 -7 -4 13168.4 3302.77 3 -10 -7 -5 20239.0 4145.04 3 -10 -7 -6 4326.12 2211.68 3 -10 8 9 1001.91 966.996 4 -10 8 8 1411.75 1080.21 4 -10 8 7 1784.15 1225.22 4 -10 8 6 4412.65 1708.82 4 -10 8 5 370.117 583.941 4 -10 8 4-151.861 334.905 4 -10 8 3 3321.66 1343.84 4 -10 8 2 11647.6 2738.09 4 -10 -8 1 4803.43 1904.69 3 -10 8 1 4984.98 1856.70 4 -10 -8 0 1670.44 1410.39 3 -10 8 0 1721.33 1082.90 4 -10 -8 -1 8574.55 2643.96 3 -10 8 -1 4909.34 1889.30 4 -10 -8 -2 8579.91 2702.29 3 -10 8 -2 5432.38 1907.41 4 -10 -8 -3 7692.86 2495.92 3 -10 8 -3 3194.85 1525.79 4 -10 8 -4 8300.66 2344.64 4 -10 -8 -4 12765.9 3262.65 3 -10 8 -5 1759.09 1079.83 4 -10 -8 -5 4545.79 2333.72 3 -10 9 7 592.873 817.998 4 -10 9 6 2157.85 1152.50 4 -10 9 5 7028.70 2185.97 4 -10 9 4 21.1131 409.804 4 -10 9 3 6099.19 1983.35 4 -10 9 2 619.117 893.046 4 -10 9 1 7805.66 2409.23 4 -10 -9 1 11122.3 2805.05 3 -10 -9 0 4069.36 1854.76 3 -10 9 0 2828.41 1498.35 4 -10 9 -1 14594.8 3269.05 4 -10 -9 -1 22539.3 3937.70 3 -10 -9 -2 5190.46 2301.33 3 -10 9 -2 4398.65 1881.67 4 -10 -9 -3 2708.91 2023.82 3 -10 9 -3-96.8847 333.939 4 -10 9 -4 109.287 337.400 4 -10 -9 -4 1324.47 1595.10 3 -10 9 -5 8246.29 2499.20 4 -10 10 6 5310.03 2074.92 4 -10 10 5 1454.47 1022.79 4 -10 10 4-1131.06 1247.23 4 -10 10 3-1005.59 1134.41 4 -10 10 2 11112.7 2956.36 4 -10 -10 1 2803.90 1644.66 3 -10 10 1 1700.46 1296.24 4 -10 -10 0 5400.99 2242.59 3 -10 10 0 2270.49 1588.77 4 -10 -10 -1 2395.53 1846.28 3 -10 10 -1 896.134 1190.20 4 -10 10 -2 13298.9 3518.22 4 -10 -10 -2 19725.1 3818.48 3 -10 10 -3 539.248 733.093 4 -10 -10 -3 1971.95 1818.49 3 -10 10 -4-341.435 508.289 4 -10 10 -5-984.160 1399.81 4 -10 11 3 546.426 1159.49 4 -10 11 2 2962.62 1966.14 4 -10 -11 2 3609.02 1924.54 3 -10 -11 1 6919.43 2360.17 3 -10 11 1 3406.71 1767.00 4 -10 -11 0 8745.54 2669.68 3 -10 11 0 5160.09 2283.35 4 -10 -11 -1 7445.58 2555.24 3 -10 11 -1 3893.93 1976.51 4 -10 -11 -2 962.318 1393.49 3 -10 11 -2 105.941 683.625 4 -10 11 -3 2022.69 1510.59 4 -10 11 -4 1858.21 922.253 4 -10 -12 0 4652.39 1716.54 3 11 0 -11 73.8098 723.256 2 11 0 -10 4519.05 2166.82 2 11 0 -9-146.856 725.886 2 11 0 -8-23.3267 153.454 2 11 0 -7-815.149 721.805 2 -11 0 7 1186.90 1356.20 4 11 0 -6 12599.0 3604.99 2 -11 0 6 23589.3 3670.18 4 11 0 -5 888.840 1190.78 2 -11 0 5 1533.68 1160.45 4 11 0 -4 310.293 367.198 2 -11 0 4 910.356 732.710 4 11 0 -3-803.625 1279.82 2 -11 0 3 332.988 577.200 4 11 0 -2 5698.93 1999.61 2 11 0 -1-863.278 1248.70 2 11 0 0-297.578 1166.20 2 11 0 1-311.265 1013.05 2 11 0 2-608.169 1023.82 2 11 0 3-656.478 1057.45 2 11 0 4 9270.06 2241.61 2 11 0 5-177.586 649.321 2 11 0 6 279.579 344.222 2 -11 0 -7 1136.55 1630.97 3 -11 0 -8 9334.90 3098.99 3 -11 0 -9 2582.73 1952.34 3 11 -1 -11 1126.00 1442.43 2 -11 1 11 4424.29 2241.23 4 11 1 -11 1596.20 1478.27 2 11 -1 -10 639.353 754.419 2 -11 1 10 4116.50 1977.61 4 11 1 -10 1494.43 1700.19 2 11 -1 -9 732.980 174.922 2 11 1 -9 1482.35 1129.92 2 11 -1 -8 1609.30 1554.63 2 -11 1 8 1790.83 1309.97 4 11 1 -8 1374.89 1429.81 2 -11 1 7 2169.43 1281.57 4 11 1 -7 1568.30 1661.29 2 -11 1 6 3943.71 1584.59 4 11 1 -6 1935.94 1352.92 2 -11 1 5 3184.84 1308.16 4 11 1 -5 1972.02 1402.87 2 -11 1 4 995.358 726.862 4 11 1 -4-174.277 839.510 2 -11 1 3 8720.28 2106.78 4 11 1 -3 5760.29 2000.92 2 -11 1 2 1094.75 441.779 4 11 1 -2 506.457 1077.65 2 11 1 -1-1028.06 1456.94 2 11 1 0-399.404 968.092 2 11 1 1 1774.13 853.914 2 11 1 2 2889.26 1273.79 2 11 -1 3 2615.55 1045.78 2 11 1 3 2226.35 1103.04 2 11 -1 4 66.8621 255.277 2 11 1 4-338.746 199.098 2 11 -1 5 4788.25 1310.27 2 11 1 5 5908.10 1692.26 2 -11 -1 -6 2230.12 1712.53 3 11 -1 6 1283.81 608.933 2 11 1 6 1595.69 946.727 2 -11 -1 -7 6646.89 2564.06 3 -11 -1 -8 1729.81 1893.67 3 -11 1 -9 3477.89 2233.53 3 -11 2 12 5165.96 2371.13 4 11 -2 -11 1737.82 1418.67 2 -11 2 11 959.027 872.517 4 11 2 -11 2087.94 1584.64 2 -11 2 10 14156.8 3366.22 4 11 2 -10 10356.7 3336.52 2 -11 2 9 12.2296 725.141 4 11 2 -9 881.160 1513.33 2 -11 2 8 1967.47 1345.16 4 11 2 -8 1006.85 1061.27 2 -11 2 7-434.783 730.849 4 11 2 -7 685.452 1034.95 2 -11 2 6 9584.87 2440.30 4 11 2 -6 7879.07 3064.38 2 -11 2 5 428.290 427.159 4 11 2 -5 508.328 803.522 2 -11 2 4 2447.78 1095.86 4 11 2 -4 1296.70 1181.22 2 -11 2 3 2743.73 1263.07 4 11 2 -3 1565.82 738.657 2 -11 2 2 7909.46 1967.16 4 11 2 -2 4311.09 1826.75 2 -11 2 1 956.525 798.634 4 11 2 -1 380.432 503.478 2 11 2 0 8649.28 2409.98 2 11 2 1 38.2488 691.475 2 11 2 2 3465.27 1496.48 2 11 2 3-131.370 591.067 2 11 2 4 2313.91 1024.16 2 -11 -2 -4 4566.10 2275.72 3 11 2 5 1284.42 856.899 2 -11 -2 -5 2511.28 1730.79 3 11 2 6 1926.05 943.385 2 -11 -2 -6 1940.13 1661.42 3 -11 -2 -7 1454.68 1458.23 3 -11 -2 -8 11933.1 3460.07 3 -11 3 11 2353.83 1211.16 4 11 3 -10 1476.30 1540.94 2 -11 3 10 979.848 983.246 4 11 3 -9 6565.91 2907.21 2 -11 3 9 5733.18 2031.02 4 -11 3 8 4738.61 1761.32 4 11 3 -8 6669.00 2787.01 2 -11 3 7 3717.06 1464.99 4 11 3 -7 2449.56 1668.20 2 -11 3 6-413.892 590.568 4 11 3 -6 227.671 775.165 2 -11 3 5 214.343 226.176 4 11 3 -5 114.332 92.9037 2 -11 3 4 997.677 384.134 4 11 3 -4 1096.57 634.870 2 -11 3 3 6358.38 1810.62 4 11 3 -3 3825.31 1816.73 2 -11 3 2 1844.21 1026.55 4 11 3 -2 1900.18 1377.97 2 -11 3 1 673.767 827.819 4 11 3 -1-192.136 604.792 2 11 3 0 4190.74 1686.95 2 11 3 1 14040.2 3000.71 2 11 3 2 1111.32 893.054 2 11 3 3 821.817 774.278 2 -11 -3 -3 2606.08 1815.20 3 11 3 4 470.011 535.660 2 -11 -3 -4 1436.04 1523.08 3 -11 -3 -5 640.801 728.215 3 11 3 5 1505.15 984.478 2 -11 -3 -6 4424.93 2522.09 3 -11 -3 -7 10285.2 3144.28 3 -11 4 11 4540.76 1978.19 4 -11 4 10 1477.10 833.072 4 11 4 -9 3395.68 2122.16 2 -11 4 9 1075.80 445.139 4 11 4 -8 281.230 1378.87 2 -11 4 8 296.214 410.164 4 11 4 -7 5170.10 2359.62 2 -11 4 7 5255.22 1722.80 4 11 4 -6 3575.49 2059.36 2 -11 4 6 3568.35 1471.98 4 11 4 -5 1632.90 1531.03 2 -11 4 5 1425.96 712.602 4 11 4 -4 614.457 1101.02 2 -11 4 4 959.237 1223.92 4 11 4 -3 1046.75 1428.54 2 -11 4 3 517.863 955.085 4 11 4 -2 4418.56 1877.05 2 -11 4 2 4772.68 1716.70 4 11 4 -1 11023.7 2873.28 2 -11 4 1 15063.5 2822.19 4 11 4 0 3123.84 1571.74 2 -11 4 0 3324.03 1423.28 4 11 4 1 840.218 1023.59 2 11 4 2 2007.80 1206.58 2 -11 -4 -2 3523.09 1974.25 3 -11 -4 -3 9799.20 2866.71 3 11 4 3 6185.11 1896.18 2 -11 -4 -4 8499.08 2874.21 3 11 4 4 6134.03 1740.47 2 -11 -4 -5 3862.38 2117.38 3 -11 -4 -6 1639.73 1765.08 3 -11 5 10 551.964 388.410 4 -11 5 9 407.511 475.166 4 11 5 -8 11428.0 3475.19 2 -11 5 8 14399.6 3043.19 4 11 5 -7 797.728 1106.33 2 -11 5 7-2.40682 598.628 4 11 5 -6 201.614 663.795 2 -11 5 6 956.645 1080.73 4 11 5 -5 648.062 659.429 2 -11 5 5 2651.53 1481.75 4 11 5 -4 6604.55 2580.16 2 -11 5 4 11259.3 2724.14 4 11 5 -3 2334.81 1681.67 2 -11 5 3 2385.45 1387.46 4 11 5 -2 4243.88 2184.11 2 -11 5 2 5405.59 1807.20 4 11 5 -1 1406.48 1272.92 2 -11 5 1 1142.93 874.406 4 11 5 0 8110.75 2426.39 2 -11 5 0 8543.94 2172.35 4 11 5 1 829.047 938.288 2 -11 -5 -1 3164.90 1894.44 3 -11 -5 -2 15023.7 3359.32 3 -11 -5 -3 2405.65 1640.64 3 -11 -5 -4 3576.85 2117.77 3 -11 -5 -5 4004.10 2295.21 3 -11 -5 -6 17439.7 4187.77 3 -11 6 9 5486.73 1953.43 4 -11 6 8 852.850 942.872 4 -11 6 7 5328.03 2058.02 4 -11 6 6 2025.87 1436.27 4 -11 6 5 18175.2 3519.92 4 -11 6 4 1028.40 953.499 4 -11 6 3 5453.45 1884.19 4 -11 6 2 424.106 446.938 4 -11 6 1 11602.8 2475.96 4 -11 6 0 518.746 550.807 4 -11 -6 -1 3168.54 1896.33 3 -11 6 -1-156.202 736.937 4 -11 -6 -2 2185.70 1825.63 3 -11 -6 -3 22196.5 4280.72 3 -11 -6 -4 2262.19 1863.85 3 -11 -6 -5 6310.62 2863.77 3 -11 7 8 9319.25 2615.73 4 -11 7 7 2343.35 1417.17 4 -11 7 6 4699.31 1837.74 4 -11 7 5 5102.84 1812.86 4 -11 7 4 14803.8 3026.47 4 -11 7 3 3259.93 1384.68 4 -11 7 2 4304.71 1483.99 4 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1096.74 1315.59 2 12 0 -4 1441.74 968.137 2 12 0 -3-461.595 1002.63 2 12 0 -2 12398.9 3205.47 2 12 0 -1-1737.48 1757.89 2 12 0 0 3647.83 1531.28 2 12 0 1-1606.61 1448.63 2 12 0 2 978.127 281.481 2 12 0 3-404.097 938.871 2 12 0 4 20926.1 3587.80 2 12 0 5-214.642 423.245 2 -12 1 9 5703.25 2328.46 4 -12 1 8 4690.38 2126.84 4 12 -1 -7 15322.9 4272.10 2 12 1 -7 17517.6 4813.62 2 -12 1 7 23542.3 4242.66 4 12 -1 -6 953.714 1277.06 2 -12 1 6 1490.83 1181.07 4 12 1 -6 1203.49 1530.78 2 12 -1 -5 1644.25 1694.69 2 12 1 -5 1740.36 1526.73 2 12 -1 -4 6245.49 2593.94 2 12 1 -4 6991.97 2675.61 2 12 -1 -3 17245.9 4147.15 2 12 1 -3 19091.8 4277.84 2 12 -1 -2-1172.71 1559.96 2 12 1 -2-1413.08 1784.66 2 12 -1 -1-1070.17 1728.60 2 12 1 -1-658.093 1383.69 2 12 -1 0-1416.54 1491.53 2 12 1 0-359.211 791.640 2 12 -1 1 16249.7 3462.98 2 12 1 1 18472.8 3783.82 2 12 -1 2-50.7860 798.261 2 12 1 2-40.9141 722.318 2 12 -1 3 2343.35 1117.83 2 12 1 3 1717.23 754.834 2 12 -1 4-1191.59 1063.03 2 12 1 4 7.39908 105.256 2 12 -1 5 15643.6 3011.51 2 12 1 5 15497.7 2796.54 2 -12 2 11 9126.19 3031.39 4 -12 2 10 14693.5 3753.01 4 -12 2 9 8774.59 2745.19 4 -12 2 8 1487.02 1158.10 4 -12 2 7 2108.20 1250.28 4 12 2 -7 1998.09 1583.24 2 -12 2 6 6678.91 2178.41 4 12 2 -6 3506.13 1974.42 2 12 2 -5 9722.79 3413.74 2 12 2 -4 3486.19 2062.73 2 12 2 -3 779.341 94.4964 2 12 2 -2 2790.55 1705.09 2 12 2 -1 6545.54 2237.15 2 12 2 0 9738.46 2708.16 2 12 2 1 74.1596 243.351 2 12 2 2 2217.00 1176.52 2 12 2 3 7099.32 2025.88 2 12 2 4 5661.29 1677.30 2 12 2 5 2684.24 1205.95 2 12 -2 5 2663.51 1077.15 2 -12 3 10-736.617 1014.86 4 -12 3 9-549.042 781.449 4 -12 3 8 15836.6 3450.42 4 -12 3 7 2927.82 1466.62 4 12 3 -6 2212.91 1755.79 2 -12 3 6 437.723 618.020 4 -12 3 5-6.93193 579.230 4 12 3 -5 692.865 777.491 2 12 3 -4 8965.94 2887.56 2 12 3 -3 3476.44 1914.31 2 12 3 -2 8351.72 2706.24 2 12 3 -1 3357.40 1738.57 2 12 3 0 9142.57 2637.45 2 12 3 1 5799.11 2093.50 2 12 3 2 9237.61 2476.15 2 12 3 3 1054.43 970.353 2 12 3 4 971.318 792.126 2 -12 4 10-559.811 715.463 4 -12 4 9 12066.4 3136.68 4 -12 4 8 1160.01 841.071 4 -12 4 7 6532.77 2098.68 4 -12 4 6-174.309 581.688 4 12 4 -5 12878.4 3554.13 2 -12 4 5 13492.1 3073.60 4 12 4 -4 3440.78 2209.49 2 -12 4 4 1528.90 1110.51 4 12 4 -3 1771.35 1410.15 2 12 4 -2 2285.44 1663.67 2 12 4 -1 20986.1 4229.38 2 12 4 0 1889.93 1387.77 2 12 4 1 1946.47 1258.26 2 12 4 2 1202.88 1097.22 2 12 4 3 8368.90 2183.27 2 -12 5 9 2083.71 1320.52 4 -12 5 8 10595.4 2733.78 4 -12 5 7-37.6143 363.055 4 -12 5 6 5829.05 1905.91 4 -12 5 5 1356.34 693.319 4 12 5 -4 8895.59 3004.66 2 -12 5 4 9612.34 2613.90 4 12 5 -3 1509.14 1641.40 2 12 5 -2 15043.9 3755.92 2 12 5 -1 2471.57 1706.76 2 12 5 0 1858.67 1394.60 2 -12 6 8-645.470 1071.47 4 -12 6 7-1144.98 1519.57 4 -12 6 6 8643.26 2629.48 4 -12 6 5 16511.8 3445.30 4 -12 6 4 2525.33 1532.62 4 -12 6 3 3084.22 1665.33 4 -12 7 7 11532.2 3255.37 4 -12 7 6 9033.51 2766.33 4 -12 7 5 1297.98 1307.90 4 -12 7 4 1597.27 1316.57 4 -12 7 3 9359.40 2530.44 4 -12 8 5 906.962 1148.09 4 -12 8 4 7812.70 2457.65 4 -12 8 3 2802.98 1493.97 4 13 0 -2-2004.98 1889.91 2 13 0 -1-1466.24 1744.06 2 13 0 0 21593.8 4367.04 2 13 0 1-1669.51 1535.51 2 13 0 2 9032.70 2705.03 2 13 0 3-334.555 567.461 2 13 0 4 21525.7 3888.01 2 13 -1 -2 2193.72 543.651 2 13 1 -2 1212.20 1504.47 2 13 -1 -1 8319.12 2688.10 2 13 1 -1 10976.8 3015.82 2 13 -1 0-3482.83 2238.83 2 13 1 0-561.176 1569.58 2 13 -1 1 860.092 220.679 2 13 1 1 467.021 660.477 2 13 -1 2 1933.88 435.781 2 13 1 2 4198.57 1851.40 2 13 -1 3 13753.9 3241.76 2 13 1 3 14319.0 3085.27 2 13 -1 4-99.1803 907.566 2 13 1 4 1118.62 878.306 2 13 2 -2 3339.10 2079.64 2 13 2 -1 2734.03 1510.34 2 13 2 0 7955.87 2599.77 2 13 -2 1 9465.78 2736.70 2 13 2 1 8909.42 2748.89 2 13 2 2 1618.54 711.298 2 13 -2 2 417.163 890.231 2 13 2 3 1370.83 1152.62 2 13 -2 3 478.463 938.173 2 13 -2 4-977.698 1568.66 2 13 3 -1 5064.11 2178.31 2 13 3 0 2217.14 1327.36 2 13 3 1 1164.13 1403.96 2 13 3 2 18623.5 3658.46 2 13 3 3 236.539 489.012 2 13 4 0 5437.77 2221.37 2 13 4 1 21333.4 4101.50 2 13 4 2 483.336 883.150 2 13 4 3 1539.32 1082.03 2 0 0 0 0.00 0.00 0 TITL PSU-963(Md-691) in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 10.226312 12.603948 14.911924 90.0000 94.8333 90.0000 ZERR 27.00 0.001698 0.002641 0.002857 0.0000 0.0162 0.0000 LATT 1 SYMM -x, y+1/2,-z+1/2 SFAC C H N Br Pd UNIT 27.00 27.00 27.00 27.00 27.00 TREF HKLF 4 END ; _shelx_hkl_checksum 91177 _olex2_submission_special_instructions 'No special instructions were received'