data_publication_text _publ_contact_author_name 'Christine M. Beavers' _publ_contact_author_address ;Advanced Light Source Lawrence Berkeley National Lab One Cyclotron Rd MS 15-317 Berkeley, CA 94720 ; _publ_contact_author_email cmbeavers@lbl.gov _publ_contact_author_phone (510)495-2448 _publ_author_id_iucr 12919 _publ_section_acknowledgements ; The Advanced Light Source is supported by the Director, Office of Science, Office of Basic Energy Sciences, of the U.S. Department of Energy under Contract No. DE-AC02-05CH11231. CMB & beamline 12.2.2 are partially supported by COMPRES, the Consortium for Materials Properties Research in Earth Sciences under NSF Cooperative Agreement EAR 11-57758 ; data_MAPbI3_0p7GPa _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common MAPbI3 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C H6 N I3 Pb' _chemical_formula_weight 619.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' -0.0005 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' -0.0002 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -1.9845 3.2173 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -0.6716 3.2892 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system cubic _space_group_IT_number 204 _space_group_name_H-M_alt 'I m -3' _space_group_name_Hall '-I 2 2 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' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' _cell_length_a 12.3053(9) _cell_length_b 12.3053(9) _cell_length_c 12.3053(9) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1863.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4328 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 14.6 _exptl_crystal_description lath _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 4.420 _exptl_crystal_F_000 2080 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.020 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 11.456 _shelx_estimated_absorpt_T_min 0.803 _shelx_estimated_absorpt_T_max 0.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2323 _exptl_absorpt_correction_T_max 0.4221 _exptl_absorpt_process_details 'SADABS-2014/5 (Sheldrick, 2014)' _exptl_absorpt_special_details ; Additional spherical absorption correction applied with mu*r = 0.6000 ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.35424 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source Beamline 12.2.2' _diffrn_radiation_monochromator silicon(111) _diffrn_measurement_device_type 'Perkin-Elmer a-Si Detector' _diffrn_measurement_method \f _diffrn_detector_area_resol_mean 5 _diffrn_reflns_number 5640 _diffrn_reflns_av_unetI/netI 0.0274 _diffrn_reflns_av_R_equivalents 0.0608 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.650 _diffrn_reflns_theta_max 13.629 _diffrn_reflns_theta_full 12.271 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measured_fraction_theta_full 0.949 _diffrn_reflns_Laue_measured_fraction_max 0.948 _diffrn_reflns_Laue_measured_fraction_full 0.949 _diffrn_reflns_point_group_measured_fraction_max 0.948 _diffrn_reflns_point_group_measured_fraction_full 0.949 _reflns_number_total 418 _reflns_number_gt 251 _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. The program ECLIPSE was used to mask the diffraction images, in order to avoid integrating detector regions that were blocked by the diamond anvil cell. ; _computing_data_collection 'Apex2 v2014.11-0 (Bruker, 2014)' _computing_cell_refinement 'SAINT V8.34A(Bruker, 2013)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXT (Sheldrick, 2012)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ; SHELXTL 5.1, XP (Sheldrick, 1994) ShelXle Rev 699 (Hubschle, 2011) ; _computing_publication_material SHELXL-2014/7 _refine_special_details ; This data collection was done while the crystal was subjected to 0.73GPa of pressure, within a Merrill-Bassett diamond anvil cell, equipped with Boehler-Almax cut diamonds. The gasket material was tungsten, and the pressure medium was DuPont Krytox 1525. Hydrogen atoms were not found in the difference map, so were not refined in the structure. N3 & C3 occur on the shared special positions, and have been refined as such, using EXYZ and EADP. N1 & C1 were found to have a reasonable distance of approx 1.5Ang, but a DFIX was employed to aide in convergence, since the light atoms in the structure were very sensitive to any change, i.e., adding another light atom for refining. The second term of the weighting scheme was chosen for the reasonable Goof it produced. It is indicative of the errors in the data,i.e., high pressure data is rarely perfect, and this dataset is typical of high pressure data on an extremely high Z compound. ; _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^)+(0.2000P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_extinction_coef 0.066(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 418 _refine_ls_number_parameters 51 _refine_ls_number_restraints 38 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0949 _refine_ls_wR_factor_ref 0.3255 _refine_ls_wR_factor_gt 0.2824 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.2500 0.2500 0.7500 0.0587(14) Uani 1 6 d S T P . . I1A I 0.2834(16) 0.5000 0.7736(16) 0.063(4) Uani 0.2886 2 d S TU P . . I1B I 0.3201(16) 0.5000 0.766(3) 0.067(4) Uani 0.2063 2 d S TU P . . I1C I 0.256(2) 0.5000 0.802(3) 0.067(5) Uani 0.1627 2 d S TU P . . I1D I 0.299(3) 0.5000 0.811(2) 0.062(4) Uani 0.1506 2 d S TU P . . I1E I 0.205(2) 0.5000 0.7586(17) 0.069(5) Uani 0.1045 2 d S TU P . . I1F I 0.292(2) 0.5000 0.7232(16) 0.043(4) Uani 0.0873 2 d S TU P . . C1 C 0.5000 0.5000 0.5000 0.23(10) Uiso 1 24 d DS U P . . N1 N 0.623(5) 0.5000 0.5000 0.23(11) Uiso 0.1667 4 d DS U P . . C2 C 0.061(6) 0.5000 1.0000 0.16(2) Uiso 0.5 4 d S . P . . N2 N 0.061(6) 0.5000 1.0000 0.16(2) Uiso 0.5 4 d S . P . . 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 Pb1 0.0587(14) 0.0587(14) 0.0587(14) 0.0002(2) 0.0002(2) -0.0002(2) I1A 0.060(7) 0.069(4) 0.061(7) 0.000 0.004(7) 0.000 I1B 0.067(7) 0.058(4) 0.077(8) 0.000 0.005(7) 0.000 I1C 0.070(10) 0.059(6) 0.073(9) 0.000 0.002(8) 0.000 I1D 0.065(9) 0.058(5) 0.062(8) 0.000 -0.018(7) 0.000 I1E 0.087(9) 0.006(4) 0.114(10) 0.000 -0.008(7) 0.000 I1F 0.066(8) 0.011(4) 0.053(7) 0.000 0.009(7) 0.000 _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 Pb1 I1A 3.117(3) 37_556 ? Pb1 I1A 3.117(3) 30_655 ? Pb1 I1A 3.117(3) 18_456 ? Pb1 I1A 3.117(3) 33_666 ? Pb1 I1A 3.117(3) 21_445 ? Pb1 I1A 3.117(3) . ? Pb1 I1E 3.128(5) . ? Pb1 I1E 3.128(5) 33_666 ? Pb1 I1E 3.128(5) 21_445 ? Pb1 I1E 3.128(5) 30_655 ? Pb1 I1E 3.128(5) 18_456 ? Pb1 I1E 3.128(5) 37_556 ? I1A I1D 0.50(2) . ? I1A I1F 0.63(2) . ? I1A I1E 0.98(4) . ? I1A Pb1 3.117(3) 15_556 ? I1B I1D 0.61(4) . ? I1B I1F 0.63(3) . ? I1B I1C 0.91(3) . ? I1B I1E 1.42(4) . ? I1B Pb1 3.201(6) 15_556 ? I1C I1D 0.54(3) . ? I1C I1E 0.83(4) . ? I1C I1F 1.07(4) . ? I1C Pb1 3.144(8) 15_556 ? I1D I1F 1.09(3) . ? I1D I1E 1.32(3) . ? I1D Pb1 3.224(6) 15_556 ? I1E I1F 1.16(4) . ? I1E Pb1 3.128(5) 15_556 ? I1F Pb1 3.137(5) 15_556 ? C1 N1 1.52(6) . ? C1 N1 1.52(6) 33_666 ? C1 N1 1.52(6) 25_666 ? C1 N1 1.52(6) 5 ? C1 N1 1.52(6) 29_666 ? C1 N1 1.52(6) 9 ? C2 N2 1.51(16) 25_567 ? C2 C2 1.51(16) 25_567 ? 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 I1A Pb1 I1A 91.5(5) 37_556 30_655 ? I1A Pb1 I1A 88.5(5) 37_556 18_456 ? I1A Pb1 I1A 180.0 30_655 18_456 ? I1A Pb1 I1A 91.5(5) 37_556 33_666 ? I1A Pb1 I1A 88.5(5) 30_655 33_666 ? I1A Pb1 I1A 91.5(5) 18_456 33_666 ? I1A Pb1 I1A 88.5(5) 37_556 21_445 ? I1A Pb1 I1A 91.5(5) 30_655 21_445 ? I1A Pb1 I1A 88.5(5) 18_456 21_445 ? I1A Pb1 I1A 180.0 33_666 21_445 ? I1A Pb1 I1A 180.0 37_556 . ? I1A Pb1 I1A 88.5(5) 30_655 . ? I1A Pb1 I1A 91.5(5) 18_456 . ? I1A Pb1 I1A 88.5(5) 33_666 . ? I1A Pb1 I1A 91.5(5) 21_445 . ? I1A Pb1 I1E 161.9(7) 37_556 . ? I1A Pb1 I1E 83.5(5) 30_655 . ? I1A Pb1 I1E 96.5(5) 18_456 . ? I1A Pb1 I1E 105.7(7) 33_666 . ? I1A Pb1 I1E 74.3(7) 21_445 . ? I1A Pb1 I1E 18.1(7) . . ? I1A Pb1 I1E 96.5(5) 37_556 33_666 ? I1A Pb1 I1E 105.7(7) 30_655 33_666 ? I1A Pb1 I1E 74.3(7) 18_456 33_666 ? I1A Pb1 I1E 18.1(7) 33_666 33_666 ? I1A Pb1 I1E 161.9(7) 21_445 33_666 ? I1A Pb1 I1E 83.5(5) . 33_666 ? I1E Pb1 I1E 101.6(5) . 33_666 ? I1A Pb1 I1E 83.5(5) 37_556 21_445 ? I1A Pb1 I1E 74.3(7) 30_655 21_445 ? I1A Pb1 I1E 105.7(7) 18_456 21_445 ? I1A Pb1 I1E 161.9(7) 33_666 21_445 ? I1A Pb1 I1E 18.1(7) 21_445 21_445 ? I1A Pb1 I1E 96.5(5) . 21_445 ? I1E Pb1 I1E 78.4(5) . 21_445 ? I1E Pb1 I1E 180.0 33_666 21_445 ? I1A Pb1 I1E 74.3(7) 37_556 30_655 ? I1A Pb1 I1E 18.1(7) 30_655 30_655 ? I1A Pb1 I1E 161.9(7) 18_456 30_655 ? I1A Pb1 I1E 83.5(5) 33_666 30_655 ? I1A Pb1 I1E 96.5(5) 21_445 30_655 ? I1A Pb1 I1E 105.7(7) . 30_655 ? I1E Pb1 I1E 101.6(5) . 30_655 ? I1E Pb1 I1E 101.6(5) 33_666 30_655 ? I1E Pb1 I1E 78.4(5) 21_445 30_655 ? I1A Pb1 I1E 105.7(7) 37_556 18_456 ? I1A Pb1 I1E 161.9(7) 30_655 18_456 ? I1A Pb1 I1E 18.1(7) 18_456 18_456 ? I1A Pb1 I1E 96.5(5) 33_666 18_456 ? I1A Pb1 I1E 83.5(5) 21_445 18_456 ? I1A Pb1 I1E 74.3(7) . 18_456 ? I1E Pb1 I1E 78.4(5) . 18_456 ? I1E Pb1 I1E 78.4(5) 33_666 18_456 ? I1E Pb1 I1E 101.6(5) 21_445 18_456 ? I1E Pb1 I1E 180.0 30_655 18_456 ? I1A Pb1 I1E 18.1(7) 37_556 37_556 ? I1A Pb1 I1E 96.5(5) 30_655 37_556 ? I1A Pb1 I1E 83.5(5) 18_456 37_556 ? I1A Pb1 I1E 74.3(7) 33_666 37_556 ? I1A Pb1 I1E 105.7(7) 21_445 37_556 ? I1A Pb1 I1E 161.9(7) . 37_556 ? I1E Pb1 I1E 180.0 . 37_556 ? I1E Pb1 I1E 78.4(5) 33_666 37_556 ? I1E Pb1 I1E 101.6(5) 21_445 37_556 ? I1E Pb1 I1E 78.4(5) 30_655 37_556 ? I1E Pb1 I1E 101.6(5) 18_456 37_556 ? I1D I1A I1F 148(8) . . ? I1D I1A I1E 123(8) . . ? I1F I1A I1E 89(4) . . ? I1D I1A Pb1 97.8(7) . . ? I1F I1A Pb1 86.0(7) . . ? I1E I1A Pb1 81.5(4) . . ? I1D I1A Pb1 97.8(7) . 15_556 ? I1F I1A Pb1 86.0(7) . 15_556 ? I1E I1A Pb1 81.5(4) . 15_556 ? Pb1 I1A Pb1 161.4(7) . 15_556 ? I1D I1B I1F 122(5) . . ? I1D I1B I1C 35(3) . . ? I1F I1B I1C 86(4) . . ? I1D I1B I1E 68(4) . . ? I1F I1B I1E 53(3) . . ? I1C I1B I1E 33(3) . . ? I1D I1B Pb1 86.6(10) . . ? I1F I1B Pb1 78.5(7) . . ? I1C I1B Pb1 78.2(7) . . ? I1E I1B Pb1 74.2(4) . . ? I1D I1B Pb1 86.6(10) . 15_556 ? I1F I1B Pb1 78.5(7) . 15_556 ? I1C I1B Pb1 78.2(7) . 15_556 ? I1E I1B Pb1 74.2(4) . 15_556 ? Pb1 I1B Pb1 147.9(8) . 15_556 ? I1D I1C I1E 151(9) . . ? I1D I1C I1B 41(5) . . ? I1E I1C I1B 110(5) . . ? I1D I1C I1F 77(6) . . ? I1E I1C I1F 74(4) . . ? I1B I1C I1F 36(2) . . ? I1D I1C Pb1 93.7(12) . . ? I1E I1C Pb1 81.3(8) . . ? I1B I1C Pb1 85.4(8) . . ? I1F I1C Pb1 79.8(7) . . ? I1D I1C Pb1 93.7(12) . 15_556 ? I1E I1C Pb1 81.3(8) . 15_556 ? I1B I1C Pb1 85.4(8) . 15_556 ? I1F I1C Pb1 79.8(7) . 15_556 ? Pb1 I1C Pb1 156.3(14) . 15_556 ? I1A I1D I1C 56(3) . . ? I1A I1D I1B 48(4) . . ? I1C I1D I1B 103(7) . . ? I1A I1D I1F 18(5) . . ? I1C I1D I1F 74(6) . . ? I1B I1D I1F 30(3) . . ? I1A I1D I1E 38(5) . . ? I1C I1D I1E 17(6) . . ? I1B I1D I1E 86(4) . . ? I1F I1D I1E 56(2) . . ? I1A I1D Pb1 73.3(5) . . ? I1C I1D Pb1 76.7(11) . . ? I1B I1D Pb1 82.4(10) . . ? I1F I1D Pb1 75.7(5) . . ? I1E I1D Pb1 73.9(4) . . ? I1A I1D Pb1 73.3(5) . 15_556 ? I1C I1D Pb1 76.7(11) . 15_556 ? I1B I1D Pb1 82.4(10) . 15_556 ? I1F I1D Pb1 75.7(5) . 15_556 ? I1E I1D Pb1 73.9(4) . 15_556 ? Pb1 I1D Pb1 145.2(7) . 15_556 ? I1C I1E I1A 30(2) . . ? I1C I1E I1F 63(3) . . ? I1A I1E I1F 33.0(18) . . ? I1C I1E I1D 11(3) . . ? I1A I1E I1D 18(2) . . ? I1F I1E I1D 51(2) . . ? I1C I1E I1B 37(3) . . ? I1A I1E I1B 7(2) . . ? I1F I1E I1B 25.9(16) . . ? I1D I1E I1B 25.6(19) . . ? I1C I1E Pb1 83.5(7) . 15_556 ? I1A I1E Pb1 80.4(5) . 15_556 ? I1F I1E Pb1 79.8(5) . 15_556 ? I1D I1E Pb1 82.1(6) . 15_556 ? I1B I1E Pb1 79.9(5) . 15_556 ? I1C I1E Pb1 83.5(7) . . ? I1A I1E Pb1 80.4(5) . . ? I1F I1E Pb1 79.8(5) . . ? I1D I1E Pb1 82.1(6) . . ? I1B I1E Pb1 79.9(5) . . ? Pb1 I1E Pb1 159.2(10) 15_556 . ? I1A I1F I1B 43(2) . . ? I1A I1F I1C 15(3) . . ? I1B I1F I1C 58(3) . . ? I1A I1F I1D 14(4) . . ? I1B I1F I1D 29(3) . . ? I1C I1F I1D 28.9(17) . . ? I1A I1F I1E 58(3) . . ? I1B I1F I1E 101(4) . . ? I1C I1F I1E 43.3(19) . . ? I1D I1F I1E 72(3) . . ? I1A I1F Pb1 82.4(6) . . ? I1B I1F Pb1 90.1(7) . . ? I1C I1F Pb1 80.5(5) . . ? I1D I1F Pb1 84.7(6) . . ? I1E I1F Pb1 78.9(5) . . ? I1A I1F Pb1 82.4(6) . 15_556 ? I1B I1F Pb1 90.1(7) . 15_556 ? I1C I1F Pb1 80.5(5) . 15_556 ? I1D I1F Pb1 84.7(6) . 15_556 ? I1E I1F Pb1 78.9(5) . 15_556 ? Pb1 I1F Pb1 157.4(9) . 15_556 ? N1 C1 N1 90.000(6) . 33_666 ? N1 C1 N1 180.0 . 25_666 ? N1 C1 N1 90.000(15) 33_666 25_666 ? N1 C1 N1 90.000(17) . 5 ? N1 C1 N1 90.0 33_666 5 ? N1 C1 N1 90.000(9) 25_666 5 ? N1 C1 N1 90.000(8) . 29_666 ? N1 C1 N1 90.000(8) 33_666 29_666 ? N1 C1 N1 90.000(18) 25_666 29_666 ? N1 C1 N1 180.0 5 29_666 ? N1 C1 N1 90.000(6) . 9 ? N1 C1 N1 180.000(10) 33_666 9 ? N1 C1 N1 90.000(9) 25_666 9 ? N1 C1 N1 90.000(3) 5 9 ? N1 C1 N1 90.000(5) 29_666 9 ? N2 C2 C2 0.0 25_567 25_567 ? _refine_diff_density_max 4.672 _refine_diff_density_min -3.224 _refine_diff_density_rms 0.553 _shelx_res_file ; sad8_y.res created by SHELXL-2014/7 TITL sad7_a.res in Im-3 REM Old TITL sad7 in Im-3 REM SHELXT solution in Im-3 REM R1 0.272, Rweak 0.001, Alpha 0.005, Orientation as input REM Formula found by SHELXT: I3 Pb CELL 0.35424 12.3053 12.3053 12.3053 90.000 90.000 90.000 ZERR 8.000 0.0009 0.0009 0.0009 0.000 0.000 0.000 LATT 2 SYMM -X, -Y, Z SYMM -X, Y, -Z SYMM X, -Y, -Z SYMM Z, X, Y SYMM Z, -X, -Y SYMM -Z, -X, Y SYMM -Z, X, -Y SYMM Y, Z, X SYMM -Y, Z, -X SYMM Y, -Z, -X SYMM -Y, -Z, X SFAC C H N I PB DISP $C -0.00053 0.00034 4.57161!source kissel DISP $H -0.00003 0.00000 0.62751!source kissel DISP $N -0.00022 0.00070 6.11009!source kissel DISP $I -1.98446 3.21726 6584.02776!source kissel DISP $Pb -0.67162 3.28917 6916.16902!source kissel UNIT 8 48 8 24 8 LIST 6 ! automatically inserted. Change 6 to 4 for CHECKCIF!! OMIT 0 0 4 OMIT 0 0 14 OMIT 0 0 10 OMIT 6 8 8 OMIT 0 1 1 TEMP 23.000 L.S. 30 Shel 999 0.75 size 0.020 0.020 0.01 !black lath BOND ACTA REM LIST 6 FMAP 2 PLAN 20 EXYZ C2 N2 EADP C2 N2 SIMU C1 N1 DFIX 1.53 0.06 N1 C1 ISOR 0.01 I1a I1b I1c I1d I1E I1F REM SUMP 1.00000 0.00001 1 2 1 3 1 4 1 5 1 6 1 7 WGHT 0.200000 35.000000 EXTI 0.065603 FVAR 0.21170 0.20634 0.15058 0.28857 0.16269 0.08731 0.10451 PB1 5 0.250000 0.250000 0.750000 10.16667 0.05866 0.05866 = 0.05866 0.00022 0.00022 -0.00022 I1A 4 0.283371 0.500000 0.773639 10.14429 0.05994 0.06865 = 0.06114 0.00000 0.00424 0.00000 I1B 4 0.320119 0.500000 0.766148 10.10317 0.06664 0.05842 = 0.07721 0.00000 0.00502 0.00000 I1C 4 0.255881 0.500000 0.802229 10.08135 0.07028 0.05875 = 0.07262 0.00000 0.00225 0.00000 I1D 4 0.298776 0.500000 0.811333 10.07529 0.06498 0.05758 = 0.06245 0.00000 -0.01798 0.00000 I1E 4 0.204975 0.500000 0.758569 10.05225 0.08720 0.00625 = 0.11425 0.00000 -0.00784 0.00000 I1F 4 0.292028 0.500000 0.723168 10.04365 0.06641 0.01076 = 0.05301 0.00000 0.00941 0.00000 C1 1 0.500000 0.500000 0.500000 10.04167 0.23417 N1 3 0.623260 0.500000 0.500000 10.04167 0.23123 C2 1 0.061479 0.500000 1.000000 10.12500 0.16347 N2 3 0.061479 0.500000 1.000000 10.12500 0.16347 HKLF 4 REM sad7_a.res in Im-3 REM R1 = 0.0949 for 251 Fo > 4sig(Fo) and 0.1138 for all 418 data REM 51 parameters refined using 38 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 4.672, deepest hole -3.224, 1-sigma level 0.553 Q1 1 0.2577 0.5000 0.6830 10.50000 0.05 2.67 Q2 1 0.0000 0.4179 1.0000 10.25000 0.05 1.70 Q3 1 0.0623 0.5000 0.7678 10.50000 0.05 1.48 Q4 1 0.0000 0.5000 1.1487 10.25000 0.05 1.22 Q5 1 0.1149 0.4654 1.0000 10.50000 0.05 1.10 Q6 1 0.1400 0.5000 1.0000 10.25000 0.05 1.07 Q7 1 0.2907 0.5000 0.6143 10.50000 0.05 1.03 Q8 1 0.2096 0.5795 0.7168 11.00000 0.05 1.03 Q9 1 0.1233 0.6017 0.7508 11.00000 0.05 0.87 Q10 1 0.1809 0.5000 0.9132 10.50000 0.05 0.83 Q11 1 0.0000 0.3392 1.0000 10.25000 0.05 0.83 Q12 1 0.2224 0.4871 1.0000 10.50000 0.05 0.81 Q13 1 0.4591 0.5150 0.8422 11.00000 0.05 0.78 Q14 1 0.3464 0.5000 0.8749 10.50000 0.05 0.68 Q15 1 0.0551 0.3639 1.0294 11.00000 0.05 0.66 Q16 1 0.6123 0.5000 0.5665 10.50000 0.05 0.65 Q17 1 0.4039 0.5538 0.7603 11.00000 0.05 0.65 Q18 1 0.5894 0.5000 0.5000 10.25000 0.05 0.63 Q19 1 0.2513 0.3525 0.7510 11.00000 0.05 0.61 Q20 1 0.1589 0.6207 0.7521 11.00000 0.05 0.59 ; _shelx_res_checksum 99456 _shelx_hkl_file ; 0 -1 -1 0.00 0.10 0 1 1 0.00 0.10 0 1 1 0.00 0.10 0 -1 -1 0.00 0.10 0 0 2 3608.44 40.10 0 0 -2 3638.84 37.70 0 -2 0 4054.29 46.90 -1 1 2 9.90 2.80 -1 1 2 12.90 3.70 -1 2 1 9.70 3.30 -1 -1 -2 10.80 2.50 -1 1 2 10.80 2.90 -1 -2 -1 12.40 2.80 -1 -2 -1 12.60 3.50 -1 -1 -2 11.10 2.90 1 -1 -2 12.10 3.40 1 1 2 9.80 2.30 1 1 2 10.90 2.80 1 -2 -1 10.20 2.70 1 -1 -2 8.50 2.40 1 2 1 8.50 2.40 1 -2 -1 8.90 2.70 1 -1 -2 11.40 3.20 0 -2 -2 1710.93 37.40 0 2 2 1541.65 39.10 0 2 2 1680.93 39.80 0 -3 -1 1165.28 32.80 0 -3 1 1172.98 26.30 0 3 -1 1226.18 28.80 0 3 1 1169.98 34.70 1 0 3 1217.88 25.70 0 -3 -1 1215.38 35.50 1 0 -3 1134.99 29.30 -1 -3 0 1359.96 34.80 0 -1 3 1380.66 19.00 0 1 3 1644.84 38.10 1 -3 0 1574.14 36.30 1 3 0 1718.23 38.30 -1 3 0 1518.75 47.70 0 -1 -3 1352.56 31.40 -1 -3 0 1521.35 34.80 -1 3 0 1673.23 37.10 -1 -3 -2 927.91 36.50 1 -3 2 841.32 22.50 1 3 -2 907.81 22.30 -1 -3 -2 873.11 31.90 -1 3 2 957.50 44.80 -1 3 2 820.82 30.60 1 3 2 879.71 32.90 1 -3 -2 839.52 33.50 1 -3 -2 1015.50 49.80 -1 -2 -3 1472.35 39.00 -1 2 3 1600.24 55.69 -1 2 3 1676.03 42.80 1 2 3 1749.53 44.40 1 -2 -3 1636.74 44.50 2 -3 -1 1858.21 52.99 2 3 1 1664.13 43.30 0 3 -3 340.97 12.30 0 -3 -3 386.76 28.00 0 -3 -3 346.57 20.60 0 -3 3 336.07 9.40 0 3 -3 376.26 11.00 0 3 3 366.96 23.00 0 -3 -3 350.56 23.10 0 3 3 356.06 23.70 0 3 3 403.06 30.30 0 -3 3 312.37 10.70 0 -3 3 379.96 13.80 0 3 -3 353.76 10.30 -2 -3 -3 48.10 7.70 -2 3 3 62.99 13.10 -2 -3 -3 50.59 9.20 -2 3 3 47.10 8.90 -2 3 3 65.69 12.40 2 3 3 44.80 7.80 2 3 3 55.99 10.40 2 -3 -3 53.09 8.80 2 -3 -3 50.69 9.80 0 0 -4 7605.74 75.89 0 -4 0 9440.96 100.69 0 0 4 8553.34 89.99 0 4 0 9999.00 113.19 0 -4 2 5745.73 67.99 0 -4 -2 5665.63 87.99 0 4 -2 6131.29 75.49 0 4 2 6061.69 99.49 1 -4 1 0.20 0.60 -1 1 4 0.50 0.90 1 -4 1 0.10 0.10 1 1 -4 0.20 0.40 -1 -1 -4 0.00 0.10 -1 1 4 0.00 0.10 -1 4 1 0.00 0.10 1 -4 1 0.00 0.10 1 -1 4 0.30 0.40 1 1 -4 0.00 0.10 1 4 -1 0.00 0.10 -1 -1 -4 0.40 0.70 1 4 -1 0.40 0.90 -1 -4 -1 0.00 0.10 -1 -4 -1 0.60 1.30 1 -4 -1 0.00 0.10 -1 4 -1 0.30 0.50 1 1 4 0.00 0.10 -1 -4 1 0.10 0.20 -1 -4 1 0.30 0.60 1 -4 -1 0.20 0.60 -1 -1 4 0.30 0.60 -1 1 -4 0.10 0.20 -1 4 -1 0.10 0.10 -1 -4 1 0.00 0.10 1 -1 -4 0.00 0.10 1 4 1 0.00 0.10 1 -1 -4 0.10 0.20 -1 -4 -3 198.68 17.60 -1 4 3 192.28 17.80 1 -4 3 199.18 11.10 -1 4 3 197.98 20.50 1 4 -3 200.38 13.10 -1 -4 -3 191.68 19.10 -1 4 3 187.18 20.60 1 4 -3 216.58 11.60 1 -4 3 190.98 12.90 1 4 3 175.28 18.70 1 -4 -3 182.58 19.00 -1 4 -3 213.98 15.50 1 4 3 193.28 17.30 1 -4 -3 212.78 27.60 -1 -4 3 232.88 12.40 0 -2 -4 5017.30 77.59 2 -4 0 6063.59 93.49 0 2 4 5670.03 91.19 2 4 0 5632.64 86.09 -2 -4 -2 3515.55 70.09 -2 -2 -4 3905.11 70.69 -2 4 2 4065.29 85.09 2 -2 -4 3588.34 71.09 2 -4 -2 3879.11 78.99 2 -2 -4 3534.55 85.49 2 2 4 3908.21 73.29 2 4 2 3992.20 79.29 -1 -3 -4 464.25 27.00 -1 -3 -4 543.55 38.80 -1 3 4 510.05 28.10 -1 -3 -4 491.25 29.90 -1 3 4 454.35 30.50 1 -3 -4 454.45 34.60 1 -3 -4 435.76 33.50 1 -3 -4 488.75 30.50 -3 -4 -3 217.78 20.50 -3 3 4 208.98 20.60 -3 -4 -3 222.88 24.40 -3 4 3 195.28 20.70 -3 4 3 247.48 29.90 3 3 4 239.18 20.20 3 -4 -3 196.38 25.90 3 -3 -4 214.08 21.20 3 4 3 222.18 19.20 3 4 3 203.28 23.10 3 -4 -3 202.08 20.50 3 3 4 198.78 19.90 3 4 3 173.48 17.40 0 4 -4 6384.26 55.29 0 -4 -4 6670.13 105.39 -2 4 4 6110.59 151.48 -2 4 4 5781.52 108.19 2 -4 -4 5903.31 113.29 2 4 4 6814.62 115.19 1 0 -5 296.27 16.60 1 0 5 307.47 16.30 0 -5 1 267.97 17.10 0 5 -1 301.47 19.90 0 5 1 295.57 22.30 -1 0 -5 335.97 19.20 -1 0 5 300.57 22.10 0 -5 1 296.57 20.90 0 5 -1 288.77 21.10 1 0 -5 301.97 18.60 -1 0 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836.72 63.79 0 12 -4 860.41 47.00 0 12 4 802.52 68.19 0 -12 4 843.32 44.20 0 -12 4 745.73 48.10 0 12 -6 672.83 32.90 0 12 6 723.43 73.09 0 12 6 709.23 61.09 0 -12 6 599.34 33.80 0 -12 -6 674.63 84.19 0 -12 6 683.43 49.00 0 -12 -6 739.33 58.89 0 -12 6 656.33 32.80 0 12 -6 690.83 35.50 0 12 -6 567.24 35.80 0 12 8 119.99 25.50 0 12 -8 132.49 13.60 0 12 -8 165.08 15.80 0 -12 -8 154.08 27.80 0 12 8 116.09 27.00 0 -12 8 156.38 18.10 0 -12 8 150.48 15.40 0 12 -8 151.28 17.50 0 -12 -10 160.38 29.70 0 12 10 139.09 28.60 0 -12 -10 181.58 36.60 -1 -12 -1 0.00 0.20 -1 -1 -12 0.00 0.10 -1 1 12 0.00 0.10 1 12 -1 0.00 0.10 1 -12 1 0.00 0.20 -1 1 12 0.00 0.10 -1 -1 -12 0.00 0.10 -1 -12 -1 0.00 0.10 -1 12 1 0.00 0.20 1 -12 1 0.00 0.10 -1 12 1 0.00 0.20 1 12 -1 0.00 0.20 -1 12 1 0.00 0.10 1 -1 12 0.00 0.10 1 -1 12 0.00 0.10 1 12 -1 0.00 0.10 1 -1 12 0.00 0.10 -1 -1 -12 0.00 0.10 1 1 -12 0.00 0.10 -1 1 12 0.00 0.20 1 1 -12 0.00 0.10 1 -12 1 0.00 0.10 1 1 -12 0.00 0.10 1 1 12 0.00 0.10 -1 1 -12 0.00 0.10 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-12 5 0.00 0.10 1 -12 -5 0.00 0.30 1 -12 -5 0.30 1.00 -1 12 -5 0.10 0.10 -1 12 7 -0.20 0.30 -1 12 7 1.90 4.20 1 12 -7 0.40 0.70 1 -12 7 0.70 0.90 -1 -12 -7 0.00 0.30 1 12 -7 0.20 0.10 1 -12 -7 0.00 0.30 -1 12 -7 0.30 0.80 -1 12 -7 0.30 0.20 1 12 7 0.80 2.40 1 -12 -7 1.40 3.00 1 12 7 -0.30 0.40 -1 -12 -9 0.00 0.40 -1 -12 -9 0.00 0.10 -1 12 9 0.00 0.10 -1 12 9 0.00 0.10 1 12 -9 0.00 0.10 -1 -12 -9 0.00 0.10 1 12 -9 0.00 0.10 -1 12 9 0.00 0.40 1 -12 9 0.00 0.10 1 -12 9 0.00 0.10 1 -12 -9 0.00 0.10 1 12 9 0.00 0.10 -1 12 -9 0.00 0.10 1 12 9 0.00 0.10 1 12 9 0.00 0.40 1 -12 -9 0.00 0.20 1 -12 -9 0.00 0.40 -1 -12 9 0.00 0.10 -1 12 11 0.00 0.40 -1 -12 -11 0.00 0.40 -1 -12 -11 0.00 0.20 -1 12 11 0.00 0.10 -1 -12 -11 0.00 0.30 1 -12 -11 0.00 0.10 1 -12 -11 0.00 0.20 1 -12 -11 0.00 0.40 1 12 11 0.00 0.50 1 12 11 0.00 0.20 0 2 12 1889.61 67.19 2 -12 0 1760.02 73.69 0 2 -12 2021.30 60.19 0 -2 -12 1565.44 72.39 2 -12 0 1764.22 88.69 -2 -12 0 1947.11 89.89 2 12 0 1926.31 80.29 0 -2 12 1941.31 52.69 0 -2 -12 2030.50 100.09 -2 -12 0 1770.32 72.59 2 -12 0 1601.94 81.19 -2 -12 0 2157.78 84.29 -2 12 0 1746.83 76.29 0 -2 12 2013.00 50.79 0 -2 -12 1720.03 64.79 0 2 -12 1628.54 43.30 0 2 12 2027.40 79.09 2 2 -12 1759.62 57.89 -2 2 12 2113.29 78.99 -2 2 12 1922.51 86.19 2 -2 12 1967.40 53.99 -2 2 12 2365.36 92.19 -2 12 2 1797.02 93.29 -2 -2 -12 2281.57 85.59 2 -12 2 2062.49 72.39 -2 -12 -2 2076.09 86.09 -2 -12 -2 1975.30 99.79 2 12 -2 2154.68 79.39 -2 -2 -12 2107.29 67.69 -2 12 2 2206.58 92.29 2 2 -12 2010.00 54.29 2 -12 2 1985.40 85.09 -2 12 -2 1938.91 83.99 2 2 12 2360.86 80.39 2 -12 -2 2023.30 116.09 2 -2 -12 2154.68 87.59 2 2 12 1844.42 80.19 2 -2 -12 2128.59 72.79 2 -12 -2 2108.69 86.79 2 12 2 2316.57 118.09 2 12 2 2154.28 91.99 -2 -12 2 2172.98 75.09 2 -12 -2 1856.11 94.09 -2 2 -12 2408.26 71.19 2 2 12 2140.29 74.49 -2 12 -2 1798.32 84.89 -2 12 -2 2097.29 78.59 -2 -12 2 2099.29 87.09 2 -12 4 879.31 42.00 -2 12 4 1017.90 79.29 -2 -12 -4 943.31 60.49 -4 -2 -12 980.60 62.29 4 -2 12 884.51 37.10 -2 12 4 909.21 60.49 -2 -12 -4 867.91 64.89 2 12 -4 792.42 52.19 2 12 -4 771.62 43.20 2 12 -4 893.01 48.00 4 -2 12 765.02 39.30 2 -12 4 938.61 56.99 -4 2 12 889.61 70.59 -2 12 -4 884.21 55.79 -2 12 -4 809.72 56.39 2 12 4 847.52 61.19 2 -12 -4 754.32 71.69 4 2 12 955.90 49.90 -4 2 -12 953.80 40.10 4 2 12 836.02 53.59 2 -12 -4 971.50 61.29 -2 -12 4 808.22 48.10 -2 12 -4 886.11 50.49 -4 -2 12 880.71 56.39 -2 -12 4 978.90 55.99 -2 -12 4 884.61 42.70 2 -12 -4 888.81 67.69 2 -12 6 558.74 36.20 2 12 -6 565.34 40.40 2 12 -6 596.54 35.60 2 -12 6 566.54 49.10 -2 12 6 669.83 68.39 -2 -12 -6 662.53 53.89 -2 12 6 685.23 55.19 -2 -12 6 611.14 42.90 2 -12 -6 716.83 55.79 2 12 6 632.64 56.19 -2 12 -6 542.35 41.00 -2 12 -6 588.54 43.20 2 12 6 615.74 64.49 2 -12 -6 641.24 61.09 2 12 -8 126.69 15.30 -2 12 8 123.19 24.00 -2 -12 -8 137.49 25.40 2 12 -8 133.49 19.00 2 -12 8 128.19 15.50 2 -12 8 129.99 13.10 2 12 8 102.09 23.50 -2 12 -8 112.59 16.50 2 -12 -8 126.49 23.40 2 12 8 121.49 29.00 -2 -12 8 123.89 18.80 -2 -12 -10 101.19 22.40 -2 -12 -10 119.49 28.10 2 -12 10 94.09 9.40 2 12 -10 117.99 13.20 -2 12 10 117.69 28.70 2 -12 10 113.39 9.60 -2 12 10 96.69 22.70 2 12 -10 118.09 11.10 2 -12 -10 126.79 28.50 -2 12 -10 107.19 10.40 2 -12 -10 88.39 20.70 -3 -12 -1 0.00 0.10 1 -3 12 0.00 0.10 -3 12 1 0.00 0.30 -1 -3 -12 0.00 0.20 3 -12 1 0.00 0.10 -1 3 12 0.00 0.10 -1 3 12 0.00 0.20 -3 12 1 0.00 0.10 -3 -12 -1 0.00 0.10 -3 12 1 0.00 0.10 -1 -3 -12 0.00 0.10 3 -12 1 0.00 0.20 3 12 -1 0.00 0.10 1 3 -12 0.00 0.10 -1 3 12 0.00 0.10 3 -12 1 0.00 0.10 3 12 -1 0.00 0.10 -3 -12 -1 0.00 0.20 -1 -3 -12 0.00 0.10 1 -3 12 0.00 0.10 3 12 -1 0.00 0.20 1 3 -12 0.00 0.10 1 3 12 0.00 0.10 1 3 12 0.00 0.10 3 -12 -1 0.00 0.10 -1 3 -12 0.00 0.10 3 -12 -1 0.00 0.20 3 12 1 0.00 0.10 -3 -12 1 0.00 0.10 3 12 1 0.00 0.10 -3 12 -1 0.00 0.10 -3 12 -1 0.00 0.10 -3 -12 1 0.00 0.20 3 -12 -1 0.00 0.10 1 -3 -12 0.00 0.10 -1 -3 12 0.00 0.10 -3 -12 1 0.00 0.10 -3 12 -1 0.00 0.30 1 -3 -12 0.00 0.20 3 12 1 0.00 0.20 1 3 12 0.00 0.20 1 -3 -12 0.00 0.10 3 -3 12 5.40 2.50 3 3 -12 3.40 2.20 -3 -3 -12 0.60 1.20 3 12 -3 1.50 2.30 -3 12 3 1.20 2.80 3 -12 3 2.20 3.90 -3 -3 -12 5.30 3.70 -3 3 -12 1.50 1.60 -3 12 -3 1.40 2.50 -3 12 -3 1.10 0.40 3 -12 -3 3.00 4.30 3 -3 -12 1.80 2.90 3 12 3 1.70 3.40 3 3 12 1.20 2.00 3 12 -5 0.40 1.10 -3 12 5 0.00 0.30 -3 12 5 0.90 2.40 -3 -12 -5 0.00 0.30 -3 -12 -5 0.70 2.00 3 -12 5 0.00 0.20 3 -12 5 0.20 0.70 3 12 -5 0.00 0.20 5 3 12 0.00 0.30 5 -3 -12 0.00 0.30 3 -12 -5 0.00 0.30 3 12 5 0.90 2.20 3 12 5 0.00 0.30 3 -12 -5 0.30 1.20 5 3 12 0.50 1.70 -3 12 7 0.00 0.30 3 12 -7 0.40 0.10 -3 12 7 0.60 2.00 3 12 -7 1.10 1.70 -3 -12 -7 0.00 0.30 -3 -12 -7 2.20 4.10 3 12 7 0.00 0.30 3 -12 -7 0.40 1.20 3 -12 -7 0.00 0.30 3 12 7 0.80 2.20 -3 -12 -9 0.00 0.10 3 -12 9 0.00 0.10 -3 12 9 0.00 0.10 -3 12 9 0.00 0.20 -3 12 9 0.00 0.40 -3 -12 -9 0.00 0.30 3 -12 9 0.00 0.10 -3 -12 -9 0.00 0.20 3 12 -9 0.00 0.10 3 12 -9 0.00 0.10 -3 -12 9 0.00 0.10 3 -12 -9 0.00 0.10 -3 12 -9 0.00 0.10 3 12 9 0.00 0.10 3 -12 -9 0.00 0.20 3 -12 -9 0.00 0.30 3 12 9 0.00 0.40 -3 -12 -11 0.00 0.40 3 12 -11 0.00 0.10 -3 12 11 0.00 0.40 3 12 -11 0.00 0.10 3 -12 11 0.00 0.10 -3 12 11 0.00 0.10 -3 -12 11 0.00 0.10 3 12 11 0.00 0.40 3 12 11 0.00 0.10 3 -12 -11 0.00 0.10 -3 12 -11 0.00 0.10 3 -12 -11 0.00 0.30 0 4 12 809.12 50.29 0 4 12 787.82 58.99 0 -4 -12 725.73 47.40 0 4 12 747.53 56.99 4 -12 0 738.53 65.39 -4 -12 0 683.33 54.79 -4 -12 0 729.83 59.19 4 -12 0 774.72 57.09 4 -12 0 756.82 63.49 -4 12 0 757.42 54.79 0 -4 -12 735.73 56.49 0 -4 -12 783.72 69.49 -4 12 0 746.73 68.19 -2 -4 -12 925.61 59.69 -2 4 12 784.52 57.69 4 -12 2 879.91 56.59 -4 -12 -2 851.11 53.89 -4 -12 -2 827.32 62.49 2 4 -12 714.93 27.10 2 -4 12 851.01 25.20 -2 -4 -12 918.21 50.89 4 -12 2 769.32 60.29 -2 4 12 891.11 58.99 -4 12 2 905.31 66.69 -2 -4 -12 784.42 52.69 -2 4 12 897.01 53.49 -4 -12 -2 815.32 68.19 2 4 -12 782.42 24.80 -4 12 2 743.43 67.79 2 4 12 843.32 46.80 2 -4 -12 866.51 51.39 2 -4 -12 878.31 59.09 4 -12 -2 894.61 67.49 4 12 2 861.91 59.99 -4 -12 2 791.32 60.49 2 -4 -12 788.02 54.89 -4 12 -2 804.82 68.39 4 -12 -2 854.91 66.19 -2 -4 12 913.21 34.20 4 12 2 787.02 64.89 2 4 12 795.62 58.59 2 4 12 856.91 52.19 -4 -12 -4 414.76 45.70 4 -12 4 404.76 40.80 -4 -4 -12 458.55 46.60 4 -4 12 420.56 21.10 -4 4 12 436.66 49.40 4 -12 4 414.56 35.30 4 -4 12 415.06 25.50 -4 -4 -12 420.96 41.40 -4 12 4 399.66 53.39 -4 -12 -4 387.86 38.00 -4 12 4 426.56 47.40 -4 -12 -4 381.36 46.70 -4 -12 4 392.26 40.10 4 -12 -4 473.35 61.19 4 12 4 407.16 42.50 4 -4 -12 435.66 54.39 4 12 4 435.56 50.59 4 4 12 426.06 42.30 4 4 12 446.96 38.10 -4 12 -4 396.66 44.20 4 -12 -4 345.17 42.90 4 -12 6 323.97 34.10 4 -12 6 303.57 27.60 -4 -12 -6 381.56 39.30 -4 12 6 334.47 41.90 -4 12 6 296.87 44.80 -4 -12 -6 272.87 39.80 -4 12 6 316.47 46.00 4 -12 -6 287.37 40.00 -4 -12 6 280.27 31.20 6 4 12 314.27 40.20 4 12 6 368.26 40.60 -4 12 -6 304.37 33.70 6 4 12 327.87 34.40 4 12 6 287.07 36.50 -4 12 8 128.39 34.10 -4 -12 -8 127.09 23.80 4 -12 8 113.99 16.50 4 12 -8 116.69 14.40 -4 -12 -8 132.59 28.20 4 12 -8 119.09 17.10 4 -12 8 103.79 13.50 4 -12 -8 108.19 24.30 -4 -12 8 93.39 17.00 -4 12 -8 99.69 16.60 4 -12 -8 136.59 32.40 4 12 8 92.89 21.10 -4 12 10 61.59 21.60 4 12 -10 110.59 12.00 4 -12 10 95.69 11.30 4 12 -10 98.89 12.70 4 -12 10 101.59 10.40 -4 -12 -10 110.29 22.70 -4 12 10 103.39 28.10 4 12 10 103.79 23.70 4 -12 -10 89.49 26.20 -4 12 -10 76.49 11.80 4 -12 -10 71.59 19.90 -5 12 1 0.00 0.20 -1 -5 -12 0.00 0.10 5 12 -1 0.00 0.10 5 -12 1 0.00 0.30 -1 5 12 0.00 0.20 5 -12 1 0.00 0.10 -1 -5 -12 0.00 0.10 -1 -5 -12 0.00 0.20 5 12 -1 0.00 0.30 -1 5 12 0.00 0.10 -1 5 12 0.00 0.10 -5 -12 1 0.00 0.10 1 5 12 0.00 0.10 1 -5 -12 0.00 0.20 5 -12 -1 0.00 0.30 5 12 1 0.00 0.30 -5 12 -1 0.00 0.20 1 5 12 0.00 0.10 1 -5 -12 0.00 0.20 5 12 1 0.00 0.10 1 5 12 0.00 0.30 5 -12 -1 0.00 0.10 5 -12 3 19.10 8.80 -3 5 12 9.60 6.40 -3 -5 -12 30.00 10.60 -3 -5 -12 17.10 8.30 -3 5 12 14.30 7.60 5 12 3 15.10 8.90 3 5 12 17.20 7.70 3 -5 -12 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0.00 0.10 -3 17 -2 0.00 0.40 -3 17 -2 0.00 0.20 -3 -17 2 0.00 0.20 3 17 2 0.00 0.50 4 17 -1 0.00 0.10 -4 17 1 0.00 0.20 1 4 -17 0.00 0.10 -1 4 17 0.00 0.30 4 -17 1 0.00 0.10 -4 -17 -1 0.00 0.30 4 17 -1 0.00 0.40 4 -17 1 0.00 0.20 4 17 -1 0.00 0.20 -1 -4 -17 0.00 0.20 -1 4 17 0.00 0.10 -1 4 17 0.00 0.10 -4 17 1 0.00 0.50 -4 17 1 0.00 0.10 -1 -4 -17 0.00 0.10 -4 -17 -1 0.00 0.20 -1 -4 -17 0.00 0.20 4 -17 1 0.00 0.30 4 -17 -1 0.00 0.20 -4 17 -1 0.00 0.20 -4 -17 1 0.00 0.20 1 -4 -17 0.00 0.10 -4 17 -1 0.00 0.40 -4 17 -1 0.00 0.10 -4 -17 1 0.00 0.10 1 -4 -17 0.00 0.30 1 4 17 0.00 0.30 4 -17 -1 0.00 0.30 1 4 17 0.00 0.10 4 -17 -1 0.00 0.10 4 17 1 0.00 0.40 1 4 17 0.00 0.10 4 17 1 0.00 0.10 1 -4 -17 0.00 0.10 4 17 1 0.00 0.10 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46408 # start Validation Reply Form _vrf_PLAT971_I ; PROBLEM: Check Calcd Residual Density 0.27A From I1D 5.02 eA-3 RESPONSE: There were other possible split iodine positions, but they did not refine sensibly. Only the final six positions would refine, so the residual density could be due to fourier termination effects. ; # end Validation Reply Form