data_05 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H34 As2 Cl4 Pd2' _chemical_formula_weight 923.03 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 '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' _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_H-M_alt 'R -3 :H' _space_group_name_Hall '-R 3' _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' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 34.074(5) _cell_length_b 34.074(5) _cell_length_c 7.4287(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 7470(3) _cell_formula_units_Z 9 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2493 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 22.14 _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.847 _exptl_crystal_F_000 4068 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 3.405 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2083 _exptl_absorpt_correction_T_max 0.7449 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20694 _diffrn_reflns_av_unetI/netI 0.1132 _diffrn_reflns_av_R_equivalents 0.1750 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.070 _diffrn_reflns_theta_max 23.619 _diffrn_reflns_theta_full 23.619 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 2476 _reflns_number_gt 1455 _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'SHELXL-2014 (Sheldrick 2014)' _computing_publication_material 'Bruker SHELXTL' _refine_special_details 'Bruker SHELXTL' _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^)+(0.0713P)^2^+595.2180P] 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 2476 _refine_ls_number_parameters 158 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1510 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2609 _refine_ls_wR_factor_gt 0.1833 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _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 C7 C 0.5796(5) 0.9090(5) 0.4941(19) 0.061(6) Uani 1 1 d G . . . . C8 C 0.5838(5) 0.8713(5) 0.459(2) 0.065(6) Uani 1 1 d G . . . . C9 C 0.6033(6) 0.8685(6) 0.298(2) 0.107(9) Uani 1 1 d G U . . . H9 H 0.6061 0.8426 0.2738 0.129 Uiso 1 1 calc R U . . . C10 C 0.6185(6) 0.9034(9) 0.1732(19) 0.159(14) Uani 1 1 d G U . . . H10 H 0.6318 0.9015 0.0635 0.191 Uiso 1 1 calc R U . . . C11 C 0.6143(6) 0.9412(7) 0.209(2) 0.131(11) Uani 1 1 d G U . . . H11 H 0.6247 0.9651 0.1234 0.157 Uiso 1 1 calc R U . . . C12 C 0.5949(6) 0.9440(5) 0.369(3) 0.106(10) Uani 1 1 d G . . . . H12 H 0.5920 0.9699 0.3936 0.127 Uiso 1 1 calc R U . . . Pd1 Pd 0.61003(4) 0.81527(5) 0.8142(2) 0.0479(5) Uani 1 1 d . . . . . As1 As 0.56146(6) 0.82884(6) 0.6427(3) 0.0498(6) Uani 1 1 d . . . . . C1 C 0.5437(5) 0.8659(4) 0.7645(19) 0.057(5) Uani 1 1 d G . . . . C2 C 0.5217(5) 0.8597(6) 0.9286(19) 0.105(11) Uani 1 1 d G . . . . H2 H 0.5128 0.8329 0.9965 0.127 Uiso 1 1 calc R U . . . C3 C 0.5127(6) 0.8927(9) 0.9935(19) 0.138(15) Uani 1 1 d G . . . . H3 H 0.4977 0.8884 1.1056 0.166 Uiso 1 1 calc R U . . . C4 C 0.5257(7) 0.9319(7) 0.894(3) 0.142(17) Uani 1 1 d G . . . . H4 H 0.5196 0.9544 0.9386 0.170 Uiso 1 1 calc R U . . . C5 C 0.5477(6) 0.9381(4) 0.730(3) 0.104(11) Uani 1 1 d G . . . . H5 H 0.5565 0.9649 0.6623 0.125 Uiso 1 1 calc R U . . . C6 C 0.5566(4) 0.9051(4) 0.6653(17) 0.056(6) Uani 1 1 d G . . . . C13 C 0.5092(8) 0.7768(8) 0.542(6) 0.144(16) Uani 1 1 d . . . . . H13A H 0.5193 0.7653 0.4399 0.173 Uiso 1 1 calc R U . . . H13B H 0.4962 0.7527 0.6343 0.173 Uiso 1 1 calc R U . . . C14 C 0.4724(7) 0.7854(7) 0.476(4) 0.084(8) Uani 1 1 d D . . . . H14A H 0.4841 0.8072 0.3747 0.101 Uiso 1 1 calc R U . . . H14B H 0.4634 0.7989 0.5739 0.101 Uiso 1 1 calc R U . . . C15 C 0.4298(8) 0.7400(9) 0.411(5) 0.146(12) Uani 1 1 d D U . . . H15A H 0.4376 0.7286 0.3018 0.175 Uiso 1 1 calc R U . . . H15B H 0.4206 0.7166 0.5062 0.175 Uiso 1 1 calc R U . . . C16 C 0.3911(11) 0.7484(13) 0.370(6) 0.185(19) Uani 1 1 d D . . . . H16A H 0.3869 0.7643 0.4719 0.277 Uiso 1 1 calc R U . . . H16B H 0.3632 0.7194 0.3509 0.277 Uiso 1 1 calc R U . . . H16C H 0.3982 0.7671 0.2616 0.277 Uiso 1 1 calc R U . . . Cl1 Cl 0.67357(15) 0.86110(16) 0.6469(6) 0.0506(12) Uani 1 1 d . . . . . Cl2 Cl 0.54631(19) 0.7703(3) 0.9727(13) 0.131(4) Uani 1 1 d . . . . . 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 C7 0.035(11) 0.066(14) 0.072(14) 0.013(12) -0.011(10) 0.018(10) C8 0.045(12) 0.120(19) 0.065(14) 0.008(12) 0.009(10) 0.067(13) C9 0.106(15) 0.157(18) 0.106(16) 0.013(13) -0.010(12) 0.102(14) C10 0.14(2) 0.21(2) 0.15(2) 0.024(17) -0.004(15) 0.095(17) C11 0.095(16) 0.16(2) 0.114(17) 0.057(15) -0.006(13) 0.043(14) C12 0.072(18) 0.12(2) 0.15(3) 0.02(2) -0.027(17) 0.059(18) Pd1 0.0319(8) 0.0371(8) 0.0743(11) 0.0075(7) -0.0008(7) 0.0171(7) As1 0.0383(11) 0.0393(11) 0.0767(14) -0.0079(9) -0.0116(9) 0.0230(9) C1 0.047(11) 0.068(14) 0.068(14) -0.022(11) -0.010(10) 0.037(11) C2 0.093(19) 0.22(3) 0.054(15) 0.025(18) 0.009(13) 0.11(2) C3 0.13(3) 0.29(5) 0.08(2) -0.03(3) -0.002(19) 0.16(3) C4 0.18(3) 0.26(5) 0.08(2) -0.09(3) -0.07(2) 0.19(4) C5 0.10(2) 0.087(19) 0.16(3) -0.064(19) -0.08(2) 0.071(17) C6 0.045(11) 0.034(10) 0.099(16) -0.023(11) -0.035(11) 0.027(9) C13 0.070(17) 0.041(13) 0.32(5) -0.06(2) -0.11(2) 0.023(13) C14 0.049(13) 0.077(15) 0.14(2) -0.054(15) -0.058(14) 0.041(12) C15 0.106(16) 0.19(2) 0.19(2) -0.032(16) -0.050(14) 0.111(16) C16 0.10(3) 0.17(4) 0.26(5) -0.05(4) -0.07(3) 0.05(3) Cl1 0.040(2) 0.057(3) 0.061(3) 0.019(2) 0.007(2) 0.029(2) Cl2 0.045(3) 0.142(6) 0.208(8) 0.128(6) 0.042(4) 0.048(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 C7 C8 1.3900 . ? C7 C12 1.3900 . ? C7 C6 1.464(18) . ? C8 C9 1.3900 . ? C8 As1 1.855(13) . ? C9 C10 1.3900 . ? C9 H9 0.9500 . ? C10 C11 1.3900 . ? C10 H10 0.9500 . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? Pd1 Cl2 2.264(6) . ? Pd1 Cl1 2.300(5) . ? Pd1 As1 2.311(2) . ? Pd1 Cl1 2.424(5) 16_666 ? As1 C1 1.884(11) . ? As1 C13 1.93(2) . ? C1 C2 1.3900 . ? C1 C6 1.3900 . ? C2 C3 1.3900 . ? C2 H2 0.9500 . ? C3 C4 1.3900 . ? C3 H3 0.9500 . ? C4 C5 1.3900 . ? C4 H4 0.9500 . ? C5 C6 1.3900 . ? C5 H5 0.9500 . ? C13 C14 1.50(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.577(18) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.515(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? Cl1 Pd1 2.424(5) 16_666 ? 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 C8 C7 C12 120.0 . . ? C8 C7 C6 112.3(12) . . ? C12 C7 C6 127.7(12) . . ? C9 C8 C7 120.0 . . ? C9 C8 As1 127.1(10) . . ? C7 C8 As1 112.9(10) . . ? C10 C9 C8 120.0 . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 120.0 . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C7 120.0 . . ? C11 C12 H12 120.0 . . ? C7 C12 H12 120.0 . . ? Cl2 Pd1 Cl1 178.4(2) . . ? Cl2 Pd1 As1 83.21(17) . . ? Cl1 Pd1 As1 95.26(13) . . ? Cl2 Pd1 Cl1 94.5(2) . 16_666 ? Cl1 Pd1 Cl1 87.01(16) . 16_666 ? As1 Pd1 Cl1 173.81(14) . 16_666 ? C8 As1 C1 88.7(6) . . ? C8 As1 C13 105.1(13) . . ? C1 As1 C13 110.1(10) . . ? C8 As1 Pd1 120.4(4) . . ? C1 As1 Pd1 111.9(4) . . ? C13 As1 Pd1 117.1(8) . . ? C2 C1 C6 120.0 . . ? C2 C1 As1 130.4(9) . . ? C6 C1 As1 109.6(9) . . ? C1 C2 C3 120.0 . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? C2 C3 C4 120.0 . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 120.0 . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C6 C5 C4 120.0 . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.0 . . ? C5 C6 C7 123.4(11) . . ? C1 C6 C7 116.6(11) . . ? C14 C13 As1 115.2(15) . . ? C14 C13 H13A 108.5 . . ? As1 C13 H13A 108.5 . . ? C14 C13 H13B 108.5 . . ? As1 C13 H13B 108.5 . . ? H13A C13 H13B 107.5 . . ? C13 C14 C15 110.9(18) . . ? C13 C14 H14A 109.5 . . ? C15 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 108.1 . . ? C16 C15 C14 110(2) . . ? C16 C15 H15A 109.8 . . ? C14 C15 H15A 109.8 . . ? C16 C15 H15B 109.8 . . ? C14 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Pd1 Cl1 Pd1 92.98(16) . 16_666 ? _refine_diff_density_max 1.801 _refine_diff_density_min -1.281 _refine_diff_density_rms 0.212 _shelx_res_file ; 1.res created by SHELXL-2014/7 TITL AO_ASF1_Pd1_0m_a.res in R-3 CELL 0.71073 34.0744 34.0744 7.4287 90.000 90.000 120.000 ZERR 9.000 0.0051 0.0051 0.0016 0.000 0.000 0.000 LATT 3 SYMM -Y, X-Y, Z SYMM -X+Y, -X, Z SFAC C H Cl As Pd UNIT 288 306 36 18 18 OMIT -3 50 L.S. 12 ACTA BOND $H FMAP 2 PLAN 10 DFIX 1.54 0.02 C14 C15 C15 C16 ISOR 0.02 C9 C10 C11 C15 TEMP -173.000 WGHT 0.071300 595.217957 FVAR 0.09124 AFIX 66 C7 1 0.579650 0.909048 0.494133 11.00000 0.03525 0.06608 = 0.07156 0.01339 -0.01112 0.01826 C8 1 0.583843 0.871261 0.458546 11.00000 0.04527 0.11957 = 0.06488 0.00769 0.00949 0.06685 C9 1 0.603279 0.868455 0.298077 11.00000 0.10620 0.15734 = 0.10635 0.01322 -0.01011 0.10201 AFIX 43 H9 2 0.606145 0.842630 0.273756 11.00000 -1.20000 AFIX 65 C10 1 0.618521 0.903436 0.173194 11.00000 0.13654 0.20581 = 0.14721 0.02430 -0.00441 0.09544 AFIX 43 H10 2 0.631804 0.901518 0.063521 11.00000 -1.20000 AFIX 65 C11 1 0.614328 0.941223 0.208778 11.00000 0.09499 0.15594 = 0.11438 0.05703 -0.00587 0.04255 AFIX 43 H11 2 0.624746 0.965131 0.123426 11.00000 -1.20000 AFIX 65 C12 1 0.594893 0.944029 0.369247 11.00000 0.07246 0.11512 = 0.14680 0.02383 -0.02716 0.05874 AFIX 43 H12 2 0.592027 0.969855 0.393567 11.00000 -1.20000 AFIX 0 PD1 5 0.610029 0.815274 0.814153 11.00000 0.03188 0.03710 = 0.07433 0.00753 -0.00081 0.01705 AS1 4 0.561457 0.828843 0.642679 11.00000 0.03825 0.03927 = 0.07674 -0.00793 -0.01158 0.02299 AFIX 66 C1 1 0.543651 0.865919 0.764520 11.00000 0.04655 0.06842 = 0.06759 -0.02189 -0.00954 0.03726 C2 1 0.521700 0.859706 0.928625 11.00000 0.09333 0.21858 = 0.05353 0.02543 0.00929 0.11480 AFIX 43 H2 2 0.512830 0.832919 0.996458 11.00000 -1.20000 AFIX 65 C3 1 0.512728 0.892686 0.993482 11.00000 0.12701 0.28507 = 0.08345 -0.02528 -0.00240 0.16312 AFIX 43 H3 2 0.497725 0.888440 1.105641 11.00000 -1.20000 AFIX 65 C4 1 0.525706 0.931879 0.894234 11.00000 0.18192 0.25973 = 0.08425 -0.09418 -0.07085 0.18555 AFIX 43 H4 2 0.519573 0.954420 0.938562 11.00000 -1.20000 AFIX 65 C5 1 0.547656 0.938093 0.730129 11.00000 0.10036 0.08663 = 0.15858 -0.06424 -0.08424 0.07109 AFIX 43 H5 2 0.556526 0.964880 0.662299 11.00000 -1.20000 AFIX 65 C6 1 0.556629 0.905113 0.665270 11.00000 0.04514 0.03439 = 0.09944 -0.02291 -0.03488 0.02718 AFIX 0 C13 1 0.509187 0.776848 0.541733 11.00000 0.06959 0.04135 = 0.31619 -0.06482 -0.10531 0.02349 AFIX 23 H13A 2 0.519291 0.765315 0.439943 11.00000 -1.20000 H13B 2 0.496192 0.752729 0.634262 11.00000 -1.20000 AFIX 0 C14 1 0.472420 0.785397 0.475792 11.00000 0.04854 0.07749 = 0.13755 -0.05421 -0.05835 0.04058 AFIX 23 H14A 2 0.484071 0.807246 0.374718 11.00000 -1.20000 H14B 2 0.463385 0.798908 0.573941 11.00000 -1.20000 AFIX 0 C15 1 0.429812 0.739960 0.411092 11.00000 0.10574 0.19355 = 0.18692 -0.03168 -0.04998 0.11058 AFIX 23 H15A 2 0.437584 0.728649 0.301783 11.00000 -1.20000 H15B 2 0.420560 0.716630 0.506218 11.00000 -1.20000 AFIX 0 C16 1 0.391104 0.748448 0.370281 11.00000 0.09921 0.16814 = 0.26139 -0.04985 -0.07313 0.04792 AFIX 137 H16A 2 0.386854 0.764287 0.471913 11.00000 -1.50000 H16B 2 0.363249 0.719441 0.350899 11.00000 -1.50000 H16C 2 0.398178 0.767106 0.261639 11.00000 -1.50000 AFIX 0 CL1 3 0.673570 0.861097 0.646903 11.00000 0.04031 0.05672 = 0.06052 0.01884 0.00734 0.02866 CL2 3 0.546305 0.770294 0.972732 11.00000 0.04501 0.14218 = 0.20762 0.12833 0.04166 0.04791 HKLF 4 REM AO_ASF1_Pd1_0m_a.res in R-3 REM R1 = 0.0792 for 1455 Fo > 4sig(Fo) and 0.1510 for all 2476 data REM 158 parameters refined using 26 restraints END WGHT 0.0644 668.2753 REM Highest difference peak 1.801, deepest hole -1.281, 1-sigma level 0.212 Q1 1 0.4120 0.7097 0.4046 11.00000 0.05 1.80 Q2 1 0.4438 0.7590 0.3046 11.00000 0.05 1.63 Q3 1 0.6097 0.8859 0.1517 11.00000 0.05 1.31 Q4 1 0.5126 0.9270 0.6943 11.00000 0.05 1.28 Q5 1 0.6147 0.9247 0.1870 11.00000 0.05 1.21 Q6 1 0.5508 0.7618 0.9087 11.00000 0.05 1.07 Q7 1 0.4194 0.7400 0.4862 11.00000 0.05 0.97 Q8 1 0.5489 0.7790 1.0428 11.00000 0.05 0.97 Q9 1 0.4101 0.7803 0.1729 11.00000 0.05 0.90 Q10 1 0.5770 0.8944 0.8267 11.00000 0.05 0.88 ; _shelx_res_checksum 6061 _shelx_hkl_file ; -3 3 0 2460.25 545.95 0 -3 0 2831.02 546.55 0 -3 0 2880.41 546.05 3 0 0 2646.44 545.95 3 -3 0 2249.07 546.45 3 -3 0 2654.53 546.15 -3 0 0 2547.95 546.15 0 3 0 2843.62 546.45 2 2 0 1643.44 364.36 -4 2 0 1808.82 364.86 4 -2 0 1782.42 364.66 -2 -2 0 1797.72 364.36 4 -5 0 2296.47 558.04 1 4 0 2893.01 557.74 -5 1 0 2750.22 557.44 -4 5 0 2541.95 557.14 -4 5 0 2983.00 558.34 -1 -4 0 2848.92 557.24 -4 5 0 2321.97 557.44 -1 -4 0 2933.11 557.94 4 1 0 335.27 59.79 1 -5 0 340.57 62.59 -5 4 0 261.07 59.89 -1 5 0 299.97 61.39 -1 5 0 190.98 60.49 -4 -1 0 286.87 59.69 3 3 0 727.73 135.19 3 -6 0 558.54 136.69 -6 3 0 569.34 134.99 6 -3 0 810.82 136.09 -3 6 0 579.14 136.29 -3 -3 0 618.24 134.79 0 -6 0 173.48 26.90 -6 6 0 75.09 24.20 -6 6 0 91.59 28.80 0 -6 0 99.49 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