data_psu-976(md-693) _audit_creation_date 2019-07-22 _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 Br0.58 Cl1.42 N2 Pd' _chemical_formula_sum 'C18 H22 Br0.58 Cl1.42 N2 Pd' _chemical_formula_weight 469.35 _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 10.0989(12) _cell_length_b 12.5877(18) _cell_length_c 14.931(2) _cell_angle_alpha 90 _cell_angle_beta 94.416(13) _cell_angle_gamma 90 _cell_volume 1892.4(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3892 _cell_measurement_temperature 295 _cell_measurement_theta_max 28.7670 _cell_measurement_theta_min 3.8470 _shelx_estimated_absorpt_T_max 0.487 _shelx_estimated_absorpt_T_min 0.327 _exptl_absorpt_coefficient_mu 2.401 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.57514 _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 1.647 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 938 _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.35 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.842 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 9147 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.842 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 29.464 _diffrn_reflns_theta_min 2.856 _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 0.999 _diffrn_measured_fraction_theta_max 0.842 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -14.00 68.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 14.0072 77.0000 -90.0000 82 #__ type_ start__ end____ width___ exp.time_ 2 omega 6.00 98.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - 14.0072 77.0000 0.0000 92 #__ type_ start__ end____ width___ exp.time_ 3 omega -43.00 -18.00 1.0000 12.0000 omega____ theta____ kappa____ phi______ frames - -14.5541 77.0000 120.0000 25 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'New Xcalibur, Ruby' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0670161000 _diffrn_orient_matrix_UB_12 0.0075527000 _diffrn_orient_matrix_UB_13 -0.0095273000 _diffrn_orient_matrix_UB_21 -0.0211357000 _diffrn_orient_matrix_UB_22 0.0333190000 _diffrn_orient_matrix_UB_23 -0.0367833000 _diffrn_orient_matrix_UB_31 0.0040307000 _diffrn_orient_matrix_UB_32 0.0448654000 _diffrn_orient_matrix_UB_33 0.0287482000 _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 3661 _reflns_number_total 4424 _reflns_odcompleteness_completeness 99.78 _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 0.556 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.105 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 232 _refine_ls_number_reflns 4424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0383 _refine_ls_restrained_S_all 1.063 _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^)+(0.0420P)^2^+0.3086P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0855 _refine_ls_wR_factor_ref 0.0931 _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(Br2)=1-FVAR(1) Sof(Cl2)=FVAR(1) Sof(Br1)=1-FVAR(2) Sof(Cl1)=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), C3(H3), C4(H4), C5(H5), 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(H17C,H17A,H17B), 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 0.4963(3) 0.4053(2) 0.7581(2) 0.0350(7) Uani 1 1 d . . . . . H1 H 0.496175 0.354384 0.803182 0.042 Uiso 1 1 calc R . . . . N1 N 0.3896(2) 0.5164(2) 0.64827(17) 0.0338(6) Uani 1 1 d . . . . . Pd1 Pd 0.58173(2) 0.55870(2) 0.63968(2) 0.03182(10) Uani 1 1 d . . . . . Cl1 Cl 0.5286(8) 0.6879(7) 0.5355(5) 0.071(2) Uani 0.756(3) 1 d . . P A 1 Br1 Br 0.5407(10) 0.7024(9) 0.5409(6) 0.0545(12) Uani 0.244(3) 1 d . . P A 2 C2 C 0.3730(3) 0.4414(2) 0.7120(2) 0.0347(7) Uani 1 1 d . . . . . N2 N 0.6044(2) 0.44469(18) 0.73550(17) 0.0310(6) Uani 1 1 d . . . . . Cl2 Cl 0.8075(11) 0.5859(13) 0.6322(9) 0.058(2) Uani 0.667(3) 1 d . . P A 1 Br2 Br 0.8052(10) 0.5987(11) 0.6382(8) 0.0633(17) Uani 0.333(3) 1 d . . P A 2 C3 C 0.2505(3) 0.4050(3) 0.7294(2) 0.0467(8) Uani 1 1 d . . . . . H3 H 0.241204 0.353393 0.773026 0.056 Uiso 1 1 calc R . . . . C4 C 0.1399(4) 0.4466(3) 0.6808(3) 0.0584(11) Uani 1 1 d . . . . . H4 H 0.055014 0.424292 0.692004 0.070 Uiso 1 1 calc R . . . . C5 C 0.1575(3) 0.5206(4) 0.6164(3) 0.0588(10) Uani 1 1 d . . . . . H5 H 0.084424 0.548785 0.582829 0.071 Uiso 1 1 calc R . . . . C6 C 0.2834(3) 0.5535(3) 0.6010(3) 0.0486(9) Uani 1 1 d . . . . . H6 H 0.294253 0.603313 0.556085 0.058 Uiso 1 1 calc R . . . . C7 C 0.7282(3) 0.4065(2) 0.7784(2) 0.0322(6) Uani 1 1 d . . . . . C8 C 0.7884(3) 0.3215(2) 0.7377(2) 0.0339(7) Uani 1 1 d . . . . . C9 C 0.9034(3) 0.2816(3) 0.7815(2) 0.0419(8) Uani 1 1 d . . . . . H9 H 0.945079 0.223442 0.757572 0.050 Uiso 1 1 calc R . . . . C10 C 0.9571(3) 0.3267(3) 0.8599(2) 0.0458(8) Uani 1 1 d . . . . . H10 H 1.033628 0.297966 0.888999 0.055 Uiso 1 1 calc R . . . . C11 C 0.8989(3) 0.4131(3) 0.8950(2) 0.0450(8) Uani 1 1 d . . . . . H11 H 0.938848 0.444011 0.946864 0.054 Uiso 1 1 calc R . . . . C12 C 0.7814(3) 0.4567(2) 0.8559(2) 0.0369(7) Uani 1 1 d . . . . . C13 C 0.7183(4) 0.5527(2) 0.8963(3) 0.0473(9) Uani 1 1 d . . . . . H13 H 0.636346 0.569134 0.859497 0.057 Uiso 1 1 calc R . . . . C14 C 0.6825(6) 0.5308(4) 0.9900(4) 0.0919(18) Uani 1 1 d . . . . . H14A H 0.620443 0.472959 0.989297 0.138 Uiso 1 1 calc GR . . . . H14B H 0.643046 0.593005 1.013901 0.138 Uiso 1 1 calc GR . . . . H14C H 0.761144 0.512269 1.027002 0.138 Uiso 1 1 calc GR . . . . C15 C 0.8082(5) 0.6504(3) 0.8968(3) 0.0803(14) Uani 1 1 d . . . . . H15A H 0.885902 0.638417 0.936722 0.120 Uiso 1 1 calc GR . . . . H15B H 0.761018 0.711087 0.916877 0.120 Uiso 1 1 calc GR . . . . H15C H 0.834058 0.663128 0.837236 0.120 Uiso 1 1 calc GR . . . . C16 C 0.7285(3) 0.2757(3) 0.6500(2) 0.0397(7) Uani 1 1 d . . . . . H16 H 0.670954 0.330578 0.621355 0.048 Uiso 1 1 calc R . . . . C17 C 0.6414(4) 0.1811(3) 0.6662(3) 0.0653(11) Uani 1 1 d . . . . . H17C H 0.576488 0.200702 0.706914 0.098 Uiso 1 1 calc GR . . . . H17A H 0.695184 0.124198 0.691719 0.098 Uiso 1 1 calc GR . . . . H17B H 0.597254 0.158374 0.610248 0.098 Uiso 1 1 calc GR . . . . C18 C 0.8303(4) 0.2479(4) 0.5851(3) 0.0636(11) Uani 1 1 d . . . . . H18A H 0.885507 0.308519 0.576542 0.095 Uiso 1 1 calc GR . . . . H18B H 0.786004 0.227261 0.528601 0.095 Uiso 1 1 calc GR . . . . H18C H 0.884188 0.190084 0.608931 0.095 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 0.0342(17) 0.0317(15) 0.0390(17) 0.0073(13) 0.0015(13) -0.0027(14) N1 0.0255(12) 0.0385(14) 0.0368(14) 0.0024(11) -0.0007(11) -0.0031(12) Pd1 0.02310(14) 0.03713(15) 0.03494(15) 0.00781(9) 0.00043(9) -0.00392(10) Cl1 0.0552(19) 0.075(4) 0.080(2) 0.049(3) -0.0213(14) -0.0206(16) Br1 0.050(2) 0.0426(14) 0.071(2) 0.0249(12) 0.003(2) -0.008(2) C2 0.0267(15) 0.0340(16) 0.0432(18) -0.0051(13) 0.0017(13) -0.0029(13) N2 0.0237(12) 0.0324(13) 0.0365(14) 0.0026(10) -0.0006(10) -0.0027(11) Cl2 0.024(3) 0.086(5) 0.064(2) 0.022(2) 0.0097(19) -0.005(3) Br2 0.030(3) 0.074(2) 0.084(3) 0.0239(19) -0.006(2) -0.022(2) C3 0.0312(17) 0.0506(19) 0.059(2) 0.0008(17) 0.0066(16) -0.0136(17) C4 0.0259(18) 0.073(3) 0.076(3) -0.003(2) 0.0015(18) -0.0140(18) C5 0.0263(17) 0.082(3) 0.066(3) 0.005(2) -0.0107(17) -0.001(2) C6 0.0274(17) 0.065(2) 0.052(2) 0.0099(17) -0.0068(15) 0.0007(16) C7 0.0260(15) 0.0333(15) 0.0369(16) 0.0076(13) -0.0001(12) 0.0000(13) C8 0.0299(15) 0.0345(16) 0.0374(16) 0.0071(13) 0.0045(13) -0.0003(14) C9 0.0372(18) 0.0432(18) 0.0457(19) 0.0071(15) 0.0061(15) 0.0097(15) C10 0.0332(17) 0.056(2) 0.047(2) 0.0078(16) -0.0004(15) 0.0142(17) C11 0.0389(19) 0.0518(19) 0.0420(19) 0.0014(16) -0.0113(15) 0.0052(17) C12 0.0315(16) 0.0365(16) 0.0419(18) 0.0010(13) -0.0010(14) 0.0037(14) C13 0.043(2) 0.0435(19) 0.053(2) -0.0068(15) -0.0117(17) 0.0118(16) C14 0.119(5) 0.066(3) 0.100(4) 0.011(3) 0.066(4) 0.032(3) C15 0.099(4) 0.047(2) 0.098(4) -0.004(2) 0.025(3) -0.007(3) C16 0.0398(18) 0.0413(18) 0.0379(17) -0.0003(14) 0.0032(14) 0.0025(15) C17 0.070(3) 0.062(3) 0.064(3) -0.005(2) 0.008(2) -0.020(2) C18 0.059(2) 0.084(3) 0.048(2) -0.012(2) 0.0102(19) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.449(4) . ? C1 N2 1.268(4) . ? N1 Pd1 2.026(2) . ? N1 C2 1.359(4) . ? N1 C6 1.324(4) . ? Pd1 Cl1 2.287(7) . ? Pd1 Br1 2.351(9) . ? Pd1 N2 2.027(2) . ? Pd1 Cl2 2.316(11) . ? Pd1 Br2 2.314(10) . ? C2 C3 1.364(4) . ? N2 C7 1.442(4) . ? C3 C4 1.387(5) . ? C4 C5 1.359(6) . ? C5 C6 1.373(5) . ? C7 C8 1.393(4) . ? C7 C12 1.390(4) . ? C8 C9 1.383(4) . ? C8 C16 1.513(4) . ? C9 C10 1.373(5) . ? C10 C11 1.361(5) . ? C11 C12 1.395(4) . ? C12 C13 1.513(4) . ? C13 C14 1.498(6) . ? C13 C15 1.528(5) . ? C16 C17 1.510(5) . ? C16 C18 1.508(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 C2 118.5(3) . . ? C2 N1 Pd1 113.4(2) . . ? C6 N1 Pd1 127.9(2) . . ? C6 N1 C2 118.7(3) . . ? N1 Pd1 Cl1 93.1(2) . . ? N1 Pd1 Br1 96.8(3) . . ? N1 Pd1 N2 79.98(10) . . ? N1 Pd1 Cl2 173.2(4) . . ? N1 Pd1 Br2 175.9(3) . . ? Cl1 Pd1 Cl2 92.4(4) . . ? N2 Pd1 Cl1 172.8(2) . . ? N2 Pd1 Br1 173.1(2) . . ? N2 Pd1 Cl2 94.6(4) . . ? N2 Pd1 Br2 95.9(3) . . ? Br2 Pd1 Br1 87.2(4) . . ? N1 C2 C1 113.8(3) . . ? N1 C2 C3 122.0(3) . . ? C3 C2 C1 124.3(3) . . ? C1 N2 Pd1 114.3(2) . . ? C1 N2 C7 119.1(2) . . ? C7 N2 Pd1 126.62(19) . . ? C2 C3 C4 118.6(3) . . ? C5 C4 C3 119.0(3) . . ? C4 C5 C6 119.9(4) . . ? N1 C6 C5 121.8(3) . . ? C8 C7 N2 117.0(3) . . ? C12 C7 N2 119.0(3) . . ? C12 C7 C8 124.0(3) . . ? C7 C8 C16 120.7(3) . . ? C9 C8 C7 116.8(3) . . ? C9 C8 C16 122.4(3) . . ? C10 C9 C8 121.0(3) . . ? C11 C10 C9 120.3(3) . . ? C10 C11 C12 122.1(3) . . ? C7 C12 C11 115.6(3) . . ? C7 C12 C13 123.2(3) . . ? C11 C12 C13 121.2(3) . . ? C12 C13 C15 112.1(3) . . ? C14 C13 C12 111.4(3) . . ? C14 C13 C15 109.2(4) . . ? C17 C16 C8 111.2(3) . . ? C18 C16 C8 113.4(3) . . ? C18 C16 C17 110.7(3) . . ? _shelx_res_file ; TITL PSU-976(Md-693) in P21/c #14 psu-976(md-693).res created by SHELXL-2018/1 at 01:18:47 on 22-Jul-2019 REM reset to P21/c #14 CELL 0.71073 10.09885 12.58769 14.93092 90 94.4158 90 ZERR 4 0.00124 0.00184 0.00238 0 0.0125 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Br Cl N Pd UNIT 72 88 2.31 5.69 8 4 L.S. 4 PLAN 20 SIZE 0.35 0.45 0.6 TEMP 22 BOND fmap 2 acta 52 OMIT 5 16 0 OMIT -6 15 6 OMIT -1 15 10 OMIT 2 15 9 REM REM REM WGHT 0.042000 0.308600 FVAR 4.57711 0.66727 0.75593 C1 1 0.496325 0.405306 0.758061 11.00000 0.03416 0.03170 = 0.03895 0.00727 0.00146 -0.00266 AFIX 43 H1 2 0.496175 0.354384 0.803182 11.00000 -1.20000 AFIX 0 N1 5 0.389615 0.516363 0.648272 11.00000 0.02550 0.03848 = 0.03682 0.00236 -0.00069 -0.00307 PD1 6 0.581730 0.558701 0.639681 11.00000 0.02310 0.03713 = 0.03494 0.00781 0.00043 -0.00392 PART 1 CL1 4 0.528566 0.687949 0.535458 31.00000 0.05516 0.07543 = 0.07955 0.04864 -0.02134 -0.02060 PART 0 PART 2 BR1 3 0.540715 0.702402 0.540876 -31.00000 0.04961 0.04262 = 0.07119 0.02491 0.00324 -0.00758 PART 0 C2 1 0.373044 0.441444 0.711956 11.00000 0.02672 0.03402 = 0.04317 -0.00508 0.00173 -0.00287 N2 5 0.604448 0.444688 0.735495 11.00000 0.02374 0.03241 = 0.03651 0.00257 -0.00060 -0.00268 PART 1 CL2 4 0.807475 0.585915 0.632248 21.00000 0.02359 0.08648 = 0.06414 0.02213 0.00973 -0.00514 PART 0 PART 2 BR2 3 0.805203 0.598734 0.638213 -21.00000 0.03022 0.07397 = 0.08427 0.02391 -0.00563 -0.02156 PART 0 C3 1 0.250470 0.405039 0.729409 11.00000 0.03123 0.05055 = 0.05877 0.00081 0.00665 -0.01360 AFIX 43 H3 2 0.241204 0.353393 0.773026 11.00000 -1.20000 AFIX 0 C4 1 0.139926 0.446644 0.680753 11.00000 0.02595 0.07307 = 0.07593 -0.00276 0.00152 -0.01403 AFIX 43 H4 2 0.055014 0.424292 0.692004 11.00000 -1.20000 AFIX 0 C5 1 0.157513 0.520575 0.616378 11.00000 0.02631 0.08203 = 0.06596 0.00531 -0.01067 -0.00131 AFIX 43 H5 2 0.084424 0.548785 0.582829 11.00000 -1.20000 AFIX 0 C6 1 0.283366 0.553541 0.600960 11.00000 0.02744 0.06492 = 0.05177 0.00991 -0.00683 0.00068 AFIX 43 H6 2 0.294253 0.603313 0.556085 11.00000 -1.20000 AFIX 0 C7 1 0.728213 0.406507 0.778397 11.00000 0.02604 0.03326 = 0.03689 0.00756 -0.00009 -0.00003 C8 1 0.788378 0.321483 0.737706 11.00000 0.02993 0.03454 = 0.03741 0.00708 0.00450 -0.00035 C9 1 0.903425 0.281646 0.781532 11.00000 0.03719 0.04323 = 0.04573 0.00714 0.00613 0.00974 AFIX 43 H9 2 0.945079 0.223442 0.757572 11.00000 -1.20000 AFIX 0 C10 1 0.957127 0.326661 0.859856 11.00000 0.03324 0.05612 = 0.04738 0.00783 -0.00040 0.01419 AFIX 43 H10 2 1.033628 0.297966 0.888999 11.00000 -1.20000 AFIX 0 C11 1 0.898942 0.413062 0.895040 11.00000 0.03893 0.05181 = 0.04205 0.00136 -0.01135 0.00521 AFIX 43 H11 2 0.938848 0.444011 0.946864 11.00000 -1.20000 AFIX 0 C12 1 0.781421 0.456720 0.855923 11.00000 0.03151 0.03654 = 0.04191 0.00097 -0.00104 0.00372 C13 1 0.718335 0.552697 0.896309 11.00000 0.04346 0.04352 = 0.05259 -0.00680 -0.01167 0.01178 AFIX 13 H13 2 0.636346 0.569134 0.859497 11.00000 -1.20000 AFIX 0 C14 1 0.682527 0.530763 0.990042 11.00000 0.11857 0.06647 = 0.09964 0.01122 0.06558 0.03243 AFIX 137 H14A 2 0.620443 0.472959 0.989297 11.00000 -1.50000 H14B 2 0.643046 0.593005 1.013901 11.00000 -1.50000 H14C 2 0.761144 0.512269 1.027002 11.00000 -1.50000 AFIX 0 C15 1 0.808179 0.650415 0.896835 11.00000 0.09907 0.04652 = 0.09782 -0.00394 0.02469 -0.00716 AFIX 137 H15A 2 0.885902 0.638417 0.936722 11.00000 -1.50000 H15B 2 0.761018 0.711087 0.916877 11.00000 -1.50000 H15C 2 0.834058 0.663128 0.837236 11.00000 -1.50000 AFIX 0 C16 1 0.728453 0.275655 0.650050 11.00000 0.03982 0.04128 = 0.03788 -0.00034 0.00318 0.00246 AFIX 13 H16 2 0.670954 0.330578 0.621355 11.00000 -1.20000 AFIX 0 C17 1 0.641423 0.181128 0.666203 11.00000 0.06998 0.06247 = 0.06396 -0.00529 0.00814 -0.02046 AFIX 137 H17C 2 0.576488 0.200702 0.706914 11.00000 -1.50000 H17A 2 0.695184 0.124198 0.691719 11.00000 -1.50000 H17B 2 0.597254 0.158374 0.610248 11.00000 -1.50000 AFIX 0 C18 1 0.830285 0.247855 0.585136 11.00000 0.05905 0.08422 = 0.04848 -0.01188 0.01022 0.00561 AFIX 137 H18A 2 0.885507 0.308519 0.576542 11.00000 -1.50000 H18B 2 0.786004 0.227261 0.528601 11.00000 -1.50000 H18C 2 0.884188 0.190084 0.608931 11.00000 -1.50000 AFIX 0 HKLF 4 REM PSU-976(Md-693) in P21/c #14 REM R1 = 0.0383 for 3661 Fo > 4sig(Fo) and 0.0507 for all 4424 data REM 232 parameters refined using 0 restraints END WGHT 0.0420 0.3086 REM Highest difference peak 0.556, deepest hole -1.128, 1-sigma level 0.105 Q1 1 0.4787 0.5513 0.5818 11.00000 0.05 0.56 Q2 1 0.6883 0.5570 0.7042 11.00000 0.05 0.50 Q3 1 0.5348 0.1069 0.7512 11.00000 0.05 0.49 Q4 1 0.4967 0.5550 0.7065 11.00000 0.05 0.46 Q5 1 0.4415 0.5556 0.5354 11.00000 0.05 0.44 Q6 1 0.6669 0.5565 0.5750 11.00000 0.05 0.43 Q7 1 0.6893 0.6184 0.5237 11.00000 0.05 0.36 Q8 1 0.5370 0.5544 0.7775 11.00000 0.05 0.36 Q9 1 0.6327 0.6943 0.5790 11.00000 0.05 0.35 Q10 1 0.5972 0.1619 0.7218 11.00000 0.05 0.35 Q11 1 0.6820 0.6064 0.7585 11.00000 0.05 0.34 Q12 1 0.5899 0.0411 0.6954 11.00000 0.05 0.31 Q13 1 0.6957 0.6822 0.7041 11.00000 0.05 0.31 Q14 1 0.3368 0.5596 0.7250 11.00000 0.05 0.30 Q15 1 0.6742 0.5043 0.7500 11.00000 0.05 0.30 Q16 1 0.7306 0.6327 0.8500 11.00000 0.05 0.30 Q17 1 0.6604 0.7667 0.9618 11.00000 0.05 0.30 Q18 1 0.2572 0.4306 0.5178 11.00000 0.05 0.30 Q19 1 0.6563 0.7014 0.6482 11.00000 0.05 0.30 Q20 1 0.7180 0.1041 0.6486 11.00000 0.05 0.29 ; _shelx_res_checksum 91247 _shelx_hkl_file ; 0 0 -3 101.763 96.8353 1 0 0 3 37.6997 66.7468 1 0 0 -4 840759. 16878.1 1 0 0 4 796324. 16864.3 1 0 0 -5 70.4171 152.064 1 0 0 5 176.358 140.690 1 0 0 -6 53194.9 2007.05 1 0 0 6 50076.8 2003.71 1 0 0 -7 221.927 187.760 1 0 0 7 103.472 125.272 1 0 0 -8 533401. 12466.0 1 0 0 8 566471. 12701.9 1 0 0 -9 354.829 298.636 1 0 0 -10 232693. 6115.43 1 0 0 -10 194943. 4247.53 3 0 0 -11 841.536 388.316 1 0 0 -12 53930.9 2774.71 1 0 0 -13 170.609 349.251 1 0 0 -14 60645.6 3202.03 1 0 0 -15 103.825 312.582 1 0 0 -16 2802.22 844.080 1 0 0 -17 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8053.59 1339.00 1 2 -3 -18 9066.25 1502.11 1 2 -3 -17 1042.19 692.150 1 2 3 -17 1621.36 645.016 1 2 3 -16 2652.76 781.672 1 2 -3 -16 2408.20 798.219 1 2 -3 -15 8558.40 1303.55 1 2 3 -15 8035.19 1157.06 1 2 3 -14 18362.9 1656.02 1 2 -3 -14 18729.5 1837.53 1 2 3 -13 1632.72 531.461 1 2 -3 -13 2935.46 759.495 1 2 -3 -12 2011.79 690.307 1 2 3 -12 732.483 333.030 1 2 3 -11 16771.4 1359.16 1 2 -3 -11 14708.9 1430.08 1 2 3 -10 18775.7 1359.01 1 2 -3 -10 17530.1 1487.68 1 -2 -3 9 29259.2 1720.75 1 2 3 -9 26815.6 1557.89 1 2 -3 -9 27836.1 1823.22 1 2 -3 -8 35979.3 2000.82 1 2 3 -8 37373.2 1766.79 1 -2 -3 8 37033.6 1826.69 1 -2 3 8 35184.9 1329.56 3 2 3 -8 39727.2 2004.53 2 2 3 -7 7124.06 750.550 2 2 -3 -7 4606.38 608.413 1 -2 3 7 5431.41 482.537 3 -2 -3 7 5924.61 640.056 1 2 3 -7 5905.86 608.401 1 2 3 -6 147270. 4211.66 2 -2 -3 6 136462. 3818.93 1 2 3 -6 137488. 3773.64 1 -2 -3 6 145166. 4338.31 2 -2 -3 5 79506.0 2802.91 2 -2 -3 5 74245.6 2158.82 3 2 3 -5 79532.5 2322.44 1 -2 -3 5 76853.0 2329.53 1 2 3 -5 78757.3 2660.56 2 -2 -3 4 74441.5 2572.48 2 2 3 -4 73993.7 2493.41 2 -2 -3 4 70584.5 2078.27 3 -2 -3 4 72540.7 2047.35 1 2 3 -4 71017.7 2022.34 1 -2 -3 3 110832. 2610.02 1 -2 -3 3 107616. 3220.14 2 2 3 -3 109965. 2602.65 1 -2 -3 3 108590. 2887.04 3 2 3 -3 107156. 3192.10 2 -2 -3 2 16068.1 839.176 3 -2 -3 2 16784.6 957.342 2 2 3 -2 16252.8 965.154 2 2 -3 -2 16387.2 728.607 2 2 3 -2 17705.4 552.965 1 -2 -3 1 133967. 3746.27 2 2 3 -1 135389. 3833.49 2 2 3 0 23784.8 1186.45 2 -2 -3 0 25684.6 1209.73 2 -2 -3 -1 154083. 4053.52 2 2 3 1 150450. 3377.24 1 -2 -3 -1 157474. 3398.81 1 -2 -3 -2 7686.30 660.383 2 -2 -3 -2 8291.15 489.589 1 2 3 2 7773.18 476.473 1 2 -3 2 7321.55 666.200 1 -2 -3 -3 215379. 4863.88 1 2 3 3 198070. 4837.26 1 2 -3 3 204447. 5416.20 1 2 -3 4 240889. 6343.49 1 -2 3 -4 246825. 6109.65 1 -2 -3 -4 243959. 5719.46 1 2 3 4 232000. 5734.06 1 2 -3 5 29564.7 1640.00 1 -2 3 -5 29786.7 1530.35 1 2 3 5 27374.5 1372.94 1 -2 -3 -5 28020.4 1363.45 1 2 3 6 10227.9 864.656 1 -2 3 -6 9699.09 869.082 1 2 -3 6 9845.11 946.695 1 -2 -3 -6 8762.21 794.081 1 2 3 7 114328. 3711.47 1 -2 -3 -7 108735. 3541.97 1 -2 3 -7 106166. 3690.89 1 2 -3 7 116948. 4100.79 1 2 3 8 40612.5 2079.04 1 -2 3 -8 39392.5 2056.21 1 -2 -3 -8 38566.4 1936.61 1 -2 3 -9 4988.10 727.684 1 -2 -3 -9 5277.35 731.629 1 -2 3 -10 14061.2 1310.75 1 -2 -3 -10 12703.5 1202.52 1 -2 -3 -11 2302.74 405.093 3 -2 -3 -11 3471.55 633.792 1 -2 3 -11 2436.83 559.717 1 -2 -3 -12 9084.34 1111.81 1 -2 3 -12 9529.53 1175.02 1 -2 -3 -12 8582.10 796.715 3 -2 3 -13 29375.4 2160.04 1 -2 -3 -13 32645.6 2205.48 1 -2 3 -14 19684.4 1800.91 1 -2 -3 -14 19289.0 1796.52 1 -2 -3 -15 4366.04 925.147 1 -2 3 -15 2240.21 782.634 1 -2 3 -16 2210.41 727.123 1 -2 -3 -16 2740.74 851.395 1 -2 -3 -17 3816.41 959.958 1 -2 3 -17 2515.40 726.030 1 2 4 -19-260.500 414.077 1 2 4 -18 2020.05 843.506 1 2 -4 -18 1274.45 683.238 1 2 -4 -17 24946.0 2421.48 1 2 4 -17 25636.3 2204.09 1 2 -4 -16 127.408 459.383 1 2 4 -16 744.452 575.145 1 2 4 -15 3905.27 815.621 1 2 -4 -15 4353.38 993.528 1 2 4 -14 1035.02 586.400 1 2 -4 -14 775.576 451.569 1 2 4 -13 56655.7 2904.02 1 2 -4 -13 55960.1 3203.11 1 2 4 -12 22049.3 1605.45 1 2 -4 -12 21330.0 1839.65 1 2 -4 -11 16793.2 1509.69 1 2 4 -11 18418.5 1396.45 1 2 4 -10 2642.20 470.161 1 2 -4 -10 553.720 315.513 1 -2 4 9 1454.88 300.916 3 -2 -4 9 2220.09 466.678 1 2 4 -9 1770.12 391.640 1 2 -4 -9 878.096 366.003 1 -2 4 8 1800.58 336.906 3 -2 -4 8 2658.57 484.307 1 2 -4 -8 1973.54 472.393 1 2 4 -8 1810.67 382.581 1 -2 -4 7 90142.9 3331.42 2 -2 -4 7 83473.0 2865.67 1 2 4 -7 82520.5 2746.99 1 -2 4 7 82367.3 2659.36 3 -2 -4 6 3735.73 577.141 2 2 4 -6 3989.66 541.291 2 -2 -4 6 2908.91 416.700 1 2 4 -6 3468.32 420.636 1 -2 -4 5 100882. 2878.41 3 2 4 -5 107336. 3382.70 2 2 4 -5 103886. 2845.88 1 -2 -4 5 100518. 2849.68 1 -2 -4 5 104952. 3415.39 2 -2 -4 4 19178.0 1189.01 2 2 4 -4 18600.6 1145.36 2 2 4 -4 19300.6 851.397 1 -2 -4 4 18930.2 965.626 3 -2 -4 4 17653.4 822.031 1 2 4 -3 56558.1 1579.13 1 2 4 -3 55144.3 2123.18 2 -2 -4 3 57791.2 1561.29 1 -2 -4 3 56587.4 1926.28 3 -2 -4 3 57449.9 2143.61 2 -2 -4 2 2843.78 413.630 2 -2 -4 2 2772.27 189.286 1 -2 -4 2 2730.42 358.496 3 2 4 -2 2588.38 387.426 2 -2 -4 1 7644.02 662.410 2 -2 -4 1 8711.66 646.304 3 2 4 -1 6673.11 656.563 2 -2 -4 0 22850.0 1184.10 2 2 4 0 20419.0 1161.73 2 -2 -4 0 22052.1 1117.75 3 -2 -4 -1 3780.57 267.981 1 -2 -4 -1 3360.59 454.440 2 -2 -4 -1 2889.82 391.402 3 -2 -4 -2 25775.8 971.708 1 -2 -4 -2 23662.7 1263.17 2 2 -4 3 157157. 4448.10 1 -2 -4 -3 162217. 3846.53 1 2 -4 4 5120.30 641.090 1 -2 -4 -4 4830.92 502.455 1 -2 4 -4 3958.35 355.292 2 -2 -4 -5 240415. 5989.47 1 -2 4 -5 244542. 6371.02 1 2 4 5 243625. 6043.32 1 2 -4 5 244253. 6669.37 1 2 4 6 788.937 256.642 1 -2 -4 -6 288.705 228.831 1 2 -4 6-96.7780 266.152 1 -2 4 -6-14.5907 267.583 1 -2 -4 -7 57613.8 2395.47 1 -2 4 -7 54667.9 2489.94 1 2 -4 7 60622.4 2820.23 1 -2 -4 -8 177.547 145.636 3 -2 4 -8 160.286 226.005 1 2 4 8 576.734 301.331 1 -2 -4 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1 27124.0 1252.95 3 2 5 -1 25546.1 1317.99 2 2 5 0 244661. 6265.00 2 -2 -5 0 261367. 6248.21 3 -2 -5 0 244609. 6241.87 2 -2 -5 -1 99458.1 2439.26 1 -2 -5 -1 100863. 3170.86 2 -2 -5 -1 97228.5 3093.83 3 -2 -5 -2 30151.7 1478.55 3 -2 -5 -2 29075.0 1099.01 1 -2 -5 -2 28744.0 1474.19 2 2 -5 3 1209.32 322.583 1 -2 5 -3 1017.87 140.769 2 -2 -5 -3 1615.71 267.056 1 -2 -5 -3 1055.15 327.052 2 -2 -5 -3 1023.37 296.288 3 -2 5 -4 221051. 5084.89 2 2 -5 4 234221. 6321.06 1 -2 -5 -4 236689. 5602.68 1 -2 -5 -4 230676. 5917.67 3 -2 5 -5 10776.4 678.495 2 -2 -5 -5 11342.5 863.434 1 2 -5 5 11707.7 1105.37 1 -2 -5 -5 10904.5 923.315 3 -2 5 -6 195.302 138.924 2 -2 -5 -6 113.252 187.274 1 2 -5 6-59.1979 141.012 1 -2 -5 -7 2078.26 447.642 1 -2 5 -7 1902.13 383.882 2 -2 -5 -7 1643.36 364.643 3 -2 5 -7 2131.38 496.495 1 -2 -5 -8 78153.2 3062.19 1 -2 5 -8 77962.7 3207.14 1 -2 -5 -8 75129.7 2836.56 3 -2 5 -8 82563.1 2798.79 2 -2 5 -9 1370.03 373.913 2 -2 -5 -9 1011.53 316.436 3 -2 5 -9 1248.72 415.866 1 -2 -5 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208837. 4723.02 1 -2 -6 -2 32273.9 1243.31 1 -2 -6 -2 32393.8 1623.98 3 -2 -6 -2 30363.4 1620.47 2 2 -6 3 738.548 326.099 1 -2 -6 -3 929.668 220.834 1 -2 6 -3 745.158 121.798 2 -2 -6 -3 460.701 190.542 3 -2 -6 -3 513.197 219.365 2 -2 -6 -4 10812.6 790.765 1 -2 6 -4 10402.4 567.408 2 2 -6 4 10865.6 1048.23 1 -2 -6 -4 10651.2 930.591 3 2 -6 5 73949.0 3162.35 1 -2 -6 -5 70184.2 2732.30 3 -2 -6 -5 71638.0 2551.09 1 -2 6 -5 71497.6 2114.73 2 -2 6 -6 3779.28 419.819 2 -2 -6 -6 4324.65 589.579 1 -2 -6 -6 4040.29 592.658 3 -2 -6 -7 126804. 4224.57 1 -2 6 -7 145592. 3862.04 2 -2 -6 -8 7065.04 855.871 1 -2 6 -8 6632.10 694.823 2 -2 -6 -9 42001.1 2278.87 1 -2 6 -9 39266.9 2283.65 1 -2 6 -10 7390.35 1032.00 1 -2 -6 -10 5879.30 876.756 1 -2 -6 -11 62629.9 3120.19 1 -2 6 -11 69157.9 3258.67 1 -2 6 -12 30631.5 2140.82 1 -2 -6 -12 29323.0 2102.26 1 -2 6 -13 10314.7 1296.53 1 -2 -6 -13 11422.0 1385.96 1 -2 6 -14 533.896 520.045 1 -2 -6 -14 128.278 355.587 1 -2 6 -15 16123.6 1694.74 1 -2 -6 -15 15181.1 1719.71 1 -2 -6 -16 847.965 581.576 1 -2 6 -16 403.891 502.450 1 -2 -6 -17 551.756 568.780 1 -2 6 -17 755.171 654.950 1 2 7 -18 3541.41 862.241 1 2 7 -17-431.593 430.676 1 2 7 -16-179.165 394.983 1 2 -7 -16 2260.43 957.414 1 2 7 -15 8665.47 1194.47 1 2 -7 -15 9415.71 1457.93 1 2 7 -14 12746.7 1380.70 1 2 -7 -14 14763.5 1749.47 1 2 -7 -13 6874.28 1160.26 1 2 7 -13 7987.31 1031.52 1 2 7 -12 7205.21 924.721 1 2 -7 -12 6628.10 1117.87 1 2 -7 -11 57046.1 3138.87 1 2 7 -11 58512.4 2687.81 1 2 7 -10 68405.2 2796.97 1 2 -7 -10 61195.8 3257.47 1 2 7 -9 16245.5 1170.51 1 2 -7 -9 14726.7 1448.36 1 -2 -7 9 14867.6 1296.17 1 -2 7 9 14823.8 1279.34 3 2 7 -8 1212.10 340.310 1 -2 -7 8 1025.24 313.528 1 -2 -7 8 764.549 413.420 2 -2 7 8 1001.31 437.408 3 -2 -7 7 11577.0 972.121 1 2 7 -7 12202.7 907.707 1 -2 7 7 10345.9 1047.88 3 -2 -7 7 13422.9 1215.90 2 -2 -7 6 33912.0 1903.31 2 -2 7 6 29195.7 1838.03 3 -2 -7 6 34238.5 1569.04 1 2 7 -6 35389.6 1891.95 2 -2 -7 5 55683.7 1995.18 1 2 7 -5 57013.9 2463.70 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519.925 2 -12 -2 8 5194.43 1312.03 2 -12 2 7 1296.51 638.224 2 -12 -2 7 2304.83 961.758 2 -12 2 6 7676.50 1211.66 2 -12 -2 6 6629.85 1211.30 2 -12 2 5 15576.9 1658.34 2 -12 -2 5 16245.7 1915.13 2 -12 2 4 6402.24 1116.44 2 -12 -2 4 4792.65 1030.67 2 -12 2 3 2120.58 665.090 2 -12 -2 3 1948.28 689.971 2 -12 2 2 5170.53 880.809 2 -12 -2 2 5722.90 1110.19 2 -12 2 1 12041.9 1414.56 2 -12 -2 1 13139.9 1639.26 2 -12 2 0 16861.1 1677.44 2 -12 -2 0 19046.3 1971.22 2 -12 2 -1 1031.15 576.825 2 -12 -2 -1 1021.68 603.043 2 -12 2 -2 1903.02 598.882 2 -12 -2 -2 2751.56 839.729 2 -12 2 -3 11663.9 1365.88 2 -12 -2 -3 12626.5 1565.35 2 -12 -2 -4 10618.2 1480.43 2 -12 -2 -5 8396.75 1385.68 2 -12 -2 -6 950.325 750.901 2 -12 -2 -7 1951.73 808.301 2 -12 -2 -8 16022.1 1928.41 2 -12 -3 8 20088.7 2297.05 2 -12 -3 7 1175.57 602.211 2 -12 3 7 1332.17 481.307 2 -12 3 6 667.180 547.232 2 -12 -3 6 1518.93 697.782 2 -12 3 5 237.057 382.123 2 -12 -3 5 896.004 514.589 2 -12 3 4 15261.8 1586.73 2 -12 -3 4 16534.6 1935.77 2 -12 3 3 6244.29 1046.54 2 -12 -3 3 8973.55 1453.86 2 -12 3 2 16537.6 1537.90 2 -12 -3 2 18448.2 2018.75 2 -12 -3 1 7272.90 1328.11 2 -12 -3 0 12624.9 1700.92 2 -12 -3 -1 8435.08 1393.40 2 -12 -3 -2 21526.9 2126.75 2 -12 -3 -3-47.7829 539.836 2 -12 -3 -4 2268.99 843.388 2 -12 -3 -5 2142.86 829.883 2 -12 -3 -6 12611.1 1694.53 2 -12 -4 6-981.144 756.500 2 -12 -4 5 29072.4 2681.10 2 -12 -4 4 3954.42 1011.42 2 -12 -4 3 1880.76 750.904 2 -12 -4 2 1262.43 862.028 2 -12 -4 1 35739.3 2886.46 2 -12 -4 0 2709.27 925.130 2 -12 -4 -1 2846.74 957.685 2 -12 -4 -2 288.481 436.475 2 -12 -4 -3 16720.2 1910.92 2 -12 -4 -4 2714.80 967.522 2 -12 -4 -5 12727.4 1738.72 2 -12 -5 4 12449.9 1777.45 2 -12 -5 3 1106.31 715.017 2 -12 -5 2 29549.6 2643.31 2 -12 -5 1 3301.20 1080.22 2 -12 -5 0 2285.77 882.301 2 -12 -5 -1 6668.01 1296.06 2 -12 -5 -2 31159.1 2690.23 2 -12 -5 -3 1183.13 711.804 2 -13 0 7-2.93716 583.086 2 -13 0 6 2208.54 863.244 2 -13 0 5-745.199 602.643 2 -13 0 4 47291.8 3294.99 2 -13 0 3-615.992 647.206 2 -13 0 2-475.446 695.430 2 -13 0 1-716.707 615.866 2 -13 0 0 38132.0 2735.41 2 -13 0 -1-124.904 442.997 2 -13 0 -2 15414.0 1760.17 2 -13 0 -3 605.701 627.574 2 -13 0 -4 30682.5 2465.98 2 -13 1 8-790.811 804.345 2 -13 1 7 24263.6 2360.08 2 -13 1 6 6019.33 1232.26 2 -13 -1 6 7546.29 1473.98 2 -13 1 5 14122.2 1776.94 2 -13 -1 5 16038.1 1953.98 2 -13 1 4 1530.76 603.159 2 -13 -1 4 1555.36 680.482 2 -13 1 3 10228.2 1402.20 2 -13 -1 3 12037.3 1688.13 2 -13 1 2 6643.27 1145.80 2 -13 -1 2 6941.60 1207.43 2 -13 1 1 21049.3 1994.87 2 -13 -1 1 20242.9 2041.79 2 -13 1 0 266.404 502.762 2 -13 -1 0 942.922 596.911 2 -13 1 -1 2668.15 793.929 2 -13 -1 -1 1702.09 770.944 2 -13 -1 -2 5785.31 1143.53 2 -13 -1 -3 26873.2 2346.36 2 -13 -1 -4 3170.18 946.823 2 -13 -1 -5 913.201 571.369 2 -13 -1 -6 2322.39 781.202 2 -13 2 8 2777.62 726.715 2 -13 2 7 504.375 446.992 2 -13 2 6 512.888 441.766 2 -13 2 5 12647.8 1560.20 2 -13 -2 5 14773.5 1953.57 2 -13 -2 4 19181.7 2167.57 2 -13 -2 3 8644.42 1482.84 2 -13 -2 2 5454.72 1136.66 2 -13 -2 1 7112.75 1321.85 2 -13 -2 0 12779.7 1741.75 2 -13 -2 -1 20211.7 2200.01 2 -13 -2 -2 3771.09 999.477 2 -13 -2 -3 4862.03 1041.64 2 -13 -2 -4 1354.13 727.182 2 -13 -3 3 685.334 662.791 2 -13 -3 2 50316.9 3459.42 2 -13 -3 1 10040.0 1562.98 2 -13 -3 0 1196.16 684.551 2 -13 -3 -1 1005.81 747.148 2 -13 -3 -2 36708.1 2908.05 2 0 0 0 0.00 0.00 0 TITL PSU-976(Md-693) in P2(1)/c REM P2(1)/c (#14 in standard setting) CELL 0.71073 10.098848 12.587685 14.930919 90.0000 94.4158 90.0000 ZERR 27.00 0.001239 0.001837 0.002382 0.0000 0.0125 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 14477 _olex2_submission_special_instructions 'No special instructions were received'