data_MAPbBr3_RT _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 'C H6 Br3 N Pb' _chemical_formula_weight 478.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0034 0.0017 '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' 0.0066 0.0034 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2713 2.4705 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.4194 10.2008 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system cubic _space_group_IT_number 221 _space_group_name_H-M_alt 'P m -3 m' _space_group_name_Hall '-P 4 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' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-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' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' _cell_length_a 5.9328(14) _cell_length_b 5.9328(14) _cell_length_c 5.9328(14) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 208.82(15) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 567 _cell_measurement_theta_min 3.52 _cell_measurement_theta_max 21.3 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.809 _exptl_crystal_F_000 206 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.030 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 34.335 _shelx_estimated_absorpt_T_min 0.426 _shelx_estimated_absorpt_T_max 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3199 _exptl_absorpt_correction_T_max 0.4404 _exptl_absorpt_process_details 'SADABS-2014/5 (Sheldrick, 2015)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.7293 _diffrn_radiation_type synchrotron _diffrn_source ; Advanced Light Source, station 11.3.1 ; _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker D8 with PHOTON 100 detector' _diffrn_measurement_method '\f and \w shutterless scans' _diffrn_detector_area_resol_mean 10.42 _diffrn_reflns_number 4451 _diffrn_reflns_av_unetI/netI 0.0076 _diffrn_reflns_av_R_equivalents 0.0313 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 3.524 _diffrn_reflns_theta_max 34.053 _diffrn_reflns_theta_full 25.950 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 113 _reflns_number_gt 113 _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 '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) WinCoot, (P.Emsley, B.Lohkamp W.G.Scott and K.Cowtand, 2010) ; _computing_publication_material SHELXL-2014/7 _refine_special_details ; Hydrogen atoms were not found in the difference map, so were not refined in the structure. The methylammonium positions were found in the difference map. The carbon and the nitrogens share the same position in all three sites. They were refined with EADP & EXYZ. A DFIX was initially used, but then as the refinement progressed, a SADI was employed over all three. ; _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^)+(0.0263P)^2^+0.0660P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'intrinsic phasing' _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens . _refine_ls_hydrogen_treatment undef _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 113 _refine_ls_number_parameters 10 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0153 _refine_ls_R_factor_gt 0.0153 _refine_ls_wR_factor_ref 0.0408 _refine_ls_wR_factor_gt 0.0408 _refine_ls_goodness_of_fit_ref 1.274 _refine_ls_restrained_S_all 1.256 _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 Pb01 Pb 0.5000 0.5000 0.5000 0.02551(17) Uani 1 48 d S T P . . Br02 Br 0.0000 0.5000 0.5000 0.0983(7) Uani 1 16 d S T P . . C1 C 0.0000 -0.120(5) 0.0000 0.030(12) Uiso 0.0417 8 d DS . P . 1 N1 N 0.0000 -0.120(5) 0.0000 0.030(12) Uiso 0.0417 8 d S . P . 1 C2 C 0.085(3) 0.0000 -0.085(3) 0.05(2) Uiso 0.0416 4 d DS . P . 2 N2 N 0.085(3) 0.0000 -0.085(3) 0.05(2) Uiso 0.0416 4 d S . P . 2 C3 C 0.069(3) 0.069(3) 0.069(3) 0.04(2) Uiso 0.0313 6 d DS . P A 3 N3 N 0.069(3) 0.069(3) 0.069(3) 0.04(2) Uiso 0.0313 6 d S . P B 3 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 Pb01 0.02551(17) 0.02551(17) 0.02551(17) 0.000 0.000 0.000 Br02 0.0222(5) 0.1364(11) 0.1364(11) 0.000 0.000 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 Pb01 Br02 2.9664(7) 9_556 ? Pb01 Br02 2.9664(7) . ? Pb01 Br02 2.9664(7) 1_655 ? Pb01 Br02 2.9664(7) 5 ? Pb01 Br02 2.9664(7) 5_565 ? Pb01 Br02 2.9664(7) 9 ? Br02 Pb01 2.9664(7) 1_455 ? C1 N1 1.01(4) 33 ? C1 N1 1.01(4) 29 ? C1 C1 1.01(4) 33 ? C1 C1 1.01(4) 29 ? C1 N1 1.01(4) 9 ? C1 C1 1.01(4) 9 ? C1 C1 1.01(4) 5 ? C1 N1 1.01(4) 5 ? C1 N1 1.43(6) 25 ? C1 C1 1.43(6) 25 ? C2 N2 0.71(3) 10 ? C2 N2 0.71(3) 30 ? C2 C2 0.71(3) 10 ? C2 C2 0.71(3) 30 ? C2 N2 0.71(3) 33 ? C2 N2 0.71(3) 29 ? C2 C2 0.71(3) 29 ? C2 C2 0.71(3) 33 ? C2 N2 1.01(4) 26 ? C2 N2 1.01(4) 2 ? C2 C2 1.01(4) 26 ? C2 C2 1.01(4) 2 ? C3 N3 0.82(4) 28 ? C3 N3 0.82(4) 27 ? C3 N3 0.82(4) 26 ? C3 C3 0.82(4) 28 ? C3 C3 0.82(4) 26 ? C3 C3 0.82(4) 27 ? C3 N3 1.16(5) 4 ? C3 C3 1.16(5) 4 ? C3 C3 1.16(5) 3 ? C3 N3 1.16(5) 2 ? C3 C3 1.16(5) 2 ? C3 N3 1.16(5) 3 ? 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 Br02 Pb01 Br02 90.0 9_556 . ? Br02 Pb01 Br02 90.0 9_556 1_655 ? Br02 Pb01 Br02 180.0 . 1_655 ? Br02 Pb01 Br02 90.0 9_556 5 ? Br02 Pb01 Br02 90.0 . 5 ? Br02 Pb01 Br02 90.0 1_655 5 ? Br02 Pb01 Br02 90.0 9_556 5_565 ? Br02 Pb01 Br02 90.0 . 5_565 ? Br02 Pb01 Br02 90.0 1_655 5_565 ? Br02 Pb01 Br02 180.0 5 5_565 ? Br02 Pb01 Br02 180.0 9_556 9 ? Br02 Pb01 Br02 90.0 . 9 ? Br02 Pb01 Br02 90.0 1_655 9 ? Br02 Pb01 Br02 90.0 5 9 ? Br02 Pb01 Br02 90.0 5_565 9 ? Pb01 Br02 Pb01 180.0 1_455 . ? N1 C1 N1 60.001(1) 33 29 ? N1 C1 C1 0.0 33 33 ? N1 C1 C1 60.0 29 33 ? N1 C1 C1 60.0 33 29 ? N1 C1 C1 0.0 29 29 ? C1 C1 C1 60.001(1) 33 29 ? N1 C1 N1 90.001(1) 33 9 ? N1 C1 N1 60.001(1) 29 9 ? C1 C1 N1 90.001(1) 33 9 ? C1 C1 N1 60.001(1) 29 9 ? N1 C1 C1 90.0 33 9 ? N1 C1 C1 60.0 29 9 ? C1 C1 C1 90.001(1) 33 9 ? C1 C1 C1 60.001(1) 29 9 ? N1 C1 C1 0.0 9 9 ? N1 C1 C1 60.0 33 5 ? N1 C1 C1 90.0 29 5 ? C1 C1 C1 60.0 33 5 ? C1 C1 C1 90.001(1) 29 5 ? N1 C1 C1 60.0 9 5 ? C1 C1 C1 60.001(3) 9 5 ? N1 C1 N1 60.0 33 5 ? N1 C1 N1 90.001(1) 29 5 ? C1 C1 N1 60.0 33 5 ? C1 C1 N1 90.001(1) 29 5 ? N1 C1 N1 60.001(3) 9 5 ? C1 C1 N1 60.001(3) 9 5 ? C1 C1 N1 0(2) 5 5 ? N1 C1 N1 45.001(1) 33 25 ? N1 C1 N1 45.001(1) 29 25 ? C1 C1 N1 45.001(1) 33 25 ? C1 C1 N1 45.001(1) 29 25 ? N1 C1 N1 45.001(1) 9 25 ? C1 C1 N1 45.001(1) 9 25 ? C1 C1 N1 45.001(1) 5 25 ? N1 C1 N1 45.001(1) 5 25 ? N1 C1 C1 45.0 33 25 ? N1 C1 C1 45.0 29 25 ? C1 C1 C1 45.001(1) 33 25 ? C1 C1 C1 45.001(1) 29 25 ? N1 C1 C1 45.0 9 25 ? C1 C1 C1 45.001(1) 9 25 ? C1 C1 C1 45.001(1) 5 25 ? N1 C1 C1 45.0 5 25 ? N1 C1 C1 0.0 25 25 ? N2 C2 N2 120.003(5) 10 30 ? N2 C2 C2 0.0 10 10 ? N2 C2 C2 120.0 30 10 ? N2 C2 C2 120.0 10 30 ? N2 C2 C2 0.0 30 30 ? C2 C2 C2 120.003(5) 10 30 ? N2 C2 N2 90.002(3) 10 33 ? N2 C2 N2 60.001(4) 30 33 ? C2 C2 N2 90.002(3) 10 33 ? C2 C2 N2 60.001(4) 30 33 ? N2 C2 N2 60.001(4) 10 29 ? N2 C2 N2 90.002(4) 30 29 ? C2 C2 N2 60.001(4) 10 29 ? C2 C2 N2 90.002(4) 30 29 ? N2 C2 N2 120.003(3) 33 29 ? N2 C2 C2 60.0 10 29 ? N2 C2 C2 90.0 30 29 ? C2 C2 C2 60.001(4) 10 29 ? C2 C2 C2 90.002(4) 30 29 ? N2 C2 C2 120.0 33 29 ? N2 C2 C2 0.0 29 29 ? N2 C2 C2 90.0 10 33 ? N2 C2 C2 60.0 30 33 ? C2 C2 C2 90.002(3) 10 33 ? C2 C2 C2 60.001(4) 30 33 ? N2 C2 C2 0.0 33 33 ? N2 C2 C2 120.0 29 33 ? C2 C2 C2 120.003(3) 29 33 ? N2 C2 N2 90.002(1) 10 26 ? N2 C2 N2 45.001(2) 30 26 ? C2 C2 N2 90.002(1) 10 26 ? C2 C2 N2 45.001(2) 30 26 ? N2 C2 N2 90.002(2) 33 26 ? N2 C2 N2 45.001(2) 29 26 ? C2 C2 N2 45.001(2) 29 26 ? C2 C2 N2 90.002(2) 33 26 ? N2 C2 N2 45.001(1) 10 2 ? N2 C2 N2 90.0 30 2 ? C2 C2 N2 45.001(1) 10 2 ? C2 C2 N2 90.0 30 2 ? N2 C2 N2 45.001(2) 33 2 ? N2 C2 N2 90.002(1) 29 2 ? C2 C2 N2 90.002(1) 29 2 ? C2 C2 N2 45.001(2) 33 2 ? N2 C2 N2 90.002(2) 26 2 ? N2 C2 C2 90.0 10 26 ? N2 C2 C2 45.0 30 26 ? C2 C2 C2 90.002(1) 10 26 ? C2 C2 C2 45.001(2) 30 26 ? N2 C2 C2 90.0 33 26 ? N2 C2 C2 45.0 29 26 ? C2 C2 C2 45.001(2) 29 26 ? C2 C2 C2 90.002(2) 33 26 ? N2 C2 C2 0.0 26 26 ? N2 C2 C2 90.0 2 26 ? N2 C2 C2 45.0 10 2 ? N2 C2 C2 90.0 30 2 ? C2 C2 C2 45.001(1) 10 2 ? C2 C2 C2 90.0 30 2 ? N2 C2 C2 45.0 33 2 ? N2 C2 C2 90.0 29 2 ? C2 C2 C2 90.002(1) 29 2 ? C2 C2 C2 45.001(2) 33 2 ? N2 C2 C2 90.0 26 2 ? N2 C2 C2 0.0 2 2 ? C2 C2 C2 90.002(2) 26 2 ? N3 C3 N3 90.001(1) 28 27 ? N3 C3 N3 90.001(2) 28 26 ? N3 C3 N3 90.001(2) 27 26 ? N3 C3 C3 0.0 28 28 ? N3 C3 C3 90.0 27 28 ? N3 C3 C3 90.0 26 28 ? N3 C3 C3 90.0 28 26 ? N3 C3 C3 90.0 27 26 ? N3 C3 C3 0.0 26 26 ? C3 C3 C3 90.001(2) 28 26 ? N3 C3 C3 90.0 28 27 ? N3 C3 C3 0.0 27 27 ? N3 C3 C3 90.0 26 27 ? C3 C3 C3 90.001(1) 28 27 ? C3 C3 C3 90.001(2) 26 27 ? N3 C3 N3 90.001(3) 28 4 ? N3 C3 N3 45.0 27 4 ? N3 C3 N3 45.000(1) 26 4 ? C3 C3 N3 90.001(3) 28 4 ? C3 C3 N3 45.000(1) 26 4 ? C3 C3 N3 45.0 27 4 ? N3 C3 C3 90.0 28 4 ? N3 C3 C3 45.0 27 4 ? N3 C3 C3 45.0 26 4 ? C3 C3 C3 90.001(3) 28 4 ? C3 C3 C3 45.000(1) 26 4 ? C3 C3 C3 45.0 27 4 ? N3 C3 C3 0.0 4 4 ? N3 C3 C3 45.0 28 3 ? N3 C3 C3 90.0 27 3 ? N3 C3 C3 45.0 26 3 ? C3 C3 C3 45.0 28 3 ? C3 C3 C3 45.0 26 3 ? C3 C3 C3 90.001(3) 27 3 ? N3 C3 C3 60.0 4 3 ? C3 C3 C3 60.000(2) 4 3 ? N3 C3 N3 45.0 28 2 ? N3 C3 N3 45.0 27 2 ? N3 C3 N3 90.001(4) 26 2 ? C3 C3 N3 45.0 28 2 ? C3 C3 N3 90.001(4) 26 2 ? C3 C3 N3 45.0 27 2 ? N3 C3 N3 60.000(1) 4 2 ? C3 C3 N3 60.000(1) 4 2 ? C3 C3 N3 60.000(1) 3 2 ? N3 C3 C3 45.0 28 2 ? N3 C3 C3 45.0 27 2 ? N3 C3 C3 90.0 26 2 ? C3 C3 C3 45.0 28 2 ? C3 C3 C3 90.001(4) 26 2 ? C3 C3 C3 45.0 27 2 ? N3 C3 C3 60.0 4 2 ? C3 C3 C3 60.000(1) 4 2 ? C3 C3 C3 60.000(1) 3 2 ? N3 C3 C3 0.0 2 2 ? N3 C3 N3 45.0 28 3 ? N3 C3 N3 90.001(3) 27 3 ? N3 C3 N3 45.0 26 3 ? C3 C3 N3 45.0 28 3 ? C3 C3 N3 45.0 26 3 ? C3 C3 N3 90.001(3) 27 3 ? N3 C3 N3 60.000(2) 4 3 ? C3 C3 N3 60.000(2) 4 3 ? C3 C3 N3 0.0(7) 3 3 ? N3 C3 N3 60.000(1) 2 3 ? C3 C3 N3 60.000(1) 2 3 ? _refine_diff_density_max 0.464 _refine_diff_density_min -0.593 _refine_diff_density_rms 0.151 _shelx_res_file ; sad_a.res created by SHELXL-2014/7 TITL sad_a.res in Pm-3m REM Old TITL sad in Pm-3m REM SHELXT solution in Pm-3m REM R1 0.453, Rweak 0.494, Alpha 0.034, Orientation as input REM Formula found by SHELXT: N Br3 Pb CELL 0.72930 5.9328 5.9328 5.9328 90.000 90.000 90.000 ZERR 1.000 0.0014 0.0014 0.0014 0.000 0.000 0.000 LATT 1 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 SYMM Y, X, -Z SYMM -Y, -X, -Z SYMM Y, -X, Z SYMM -Y, X, Z SYMM X, Z, -Y SYMM -X, Z, Y SYMM -X, -Z, -Y SYMM X, -Z, Y SYMM Z, Y, -X SYMM Z, -Y, X SYMM -Z, Y, X SYMM -Z, -Y, -X SFAC C H N BR PB DISP $C 0.00341 0.00169 11.32113!source kissel DISP $H -0.00002 0.00000 0.66638!source kissel DISP $N 0.00664 0.00342 19.38436!source kissel DISP $Br -0.27128 2.47050 10018.37566!source kissel DISP $Pb -3.41943 10.20082 41609.52882!source kissel UNIT 1 6 1 3 1 SIZE 0.03 0.02 0.01 !orange block REM DFIX 1.5 0.1 C1 N1 TEMP -273.150 L.S. 300 BOND $H LIST 4 ACTA FMAP 2 PLAN 20 EXYZ C1 N1 EADP C1 N1 EXYZ C2 N2 EADP C2 N2 EXYZ C3 N3 EADP C3 N3 EQIV $1 -x, -y, -z EQIV $2 +z, +y, +x EQIV $3 -z, -x, -y RTAB MA C1 N1_$1 RTAB MA C2 N2_$2 RTAB MA C3 N3_$3 SADI 0.05 C1 N1_$1 C2 N2_$2 C3 N3_$3 WGHT 0.026300 0.066000 FVAR 0.71502 PB01 5 0.500000 0.500000 0.500000 10.02083 0.02551 0.02551 = 0.02551 0.00000 0.00000 0.00000 BR02 4 0.000000 0.500000 0.500000 10.06250 0.02221 0.13642 = 0.13642 0.00000 0.00000 0.00000 part 1 C1 1 0.000000 -0.120298 0.000000 10.00521 0.02991 N1 3 0.000000 -0.120298 0.000000 10.00521 0.02991 part 2 C2 1 0.084729 0.000000 -0.084729 10.01041 0.05305 N2 3 0.084729 0.000000 -0.084729 10.01041 0.05305 Part 3 C3 1 0.069251 0.069251 0.069251 10.00521 0.04098 N3 3 0.069251 0.069251 0.069251 10.00521 0.04098 Part 0 HKLF 4 REM sad_a.res in Pm-3m REM R1 = 0.0153 for 113 Fo > 4sig(Fo) and 0.0153 for all 113 data REM 10 parameters refined using 3 restraints END WGHT 0.0250 0.0722 REM Highest difference peak 0.464, deepest hole -0.593, 1-sigma level 0.151 Q1 1 -0.0664 -0.1960 0.0000 10.50000 0.05 0.46 Q2 1 0.0000 0.3944 0.5000 10.25000 0.05 0.36 Q3 1 0.1463 0.1463 0.1463 10.16667 0.05 0.31 Q4 1 0.2070 0.0000 -0.2585 10.50000 0.05 0.24 Q5 1 0.2278 0.5000 0.2278 10.25000 0.05 0.19 Q6 1 0.2971 0.2971 0.2017 10.50000 0.05 0.17 Q7 1 0.0000 0.2164 0.5000 10.25000 0.05 0.17 Q8 1 0.2784 -0.0760 -0.2784 10.50000 0.05 0.16 Q9 1 0.2345 0.4695 0.4313 11.00000 0.05 0.15 Q10 1 0.5000 0.4036 0.5000 10.12500 0.05 0.13 Q11 1 0.3993 0.3993 0.2627 10.50000 0.05 0.12 Q12 1 0.1690 0.3736 0.3736 10.50000 0.05 0.12 Q13 1 0.1572 0.2610 0.5000 10.50000 0.05 0.12 Q14 1 0.3609 0.1562 0.2147 11.00000 0.05 0.12 Q15 1 0.1309 0.5000 0.1309 10.25000 0.05 0.11 Q16 1 0.2790 0.2790 0.5000 10.25000 0.05 0.09 Q17 1 0.0000 0.2522 0.3936 10.50000 0.05 0.08 Q18 1 0.2038 0.2038 0.4262 10.50000 0.05 0.07 Q19 1 0.2347 0.3648 0.5000 10.50000 0.05 0.07 Q20 1 0.1002 0.1945 0.5000 10.50000 0.05 0.06 ; _shelx_res_checksum 94550 _shelx_hkl_file ; 1 0 0 4054.99 71.69 1 0 0 3874.61 72.49 -1 0 0 3971.60 72.09 0 1 0 4079.99 71.99 0 0 1 4026.70 71.09 0 0 -1 4070.09 71.09 0 1 0 3999.60 72.09 0 -1 1 1257.57 25.60 0 -1 1 1371.36 32.30 0 1 1 1298.57 24.60 1 -1 0 1327.67 25.80 -1 0 -1 1293.07 25.10 -1 0 1 1304.17 24.80 -1 1 0 1370.16 27.80 0 1 -1 1377.56 26.60 1 -1 0 1239.88 23.20 1 0 -1 1288.87 24.90 1 0 1 1253.27 22.60 1 1 0 1315.87 25.70 1 -1 0 1281.97 24.50 1 0 1 1323.27 25.90 1 1 0 1300.47 27.20 0 1 1 1342.87 28.90 1 1 0 1253.37 26.10 0 -1 1 1301.57 24.50 0 1 1 1292.27 24.70 -1 -1 0 1288.87 29.80 -1 0 -1 1315.37 23.20 -1 0 1 1318.97 29.40 -1 1 0 1312.37 25.70 0 -1 -1 1302.97 24.70 -1 0 1 1315.07 25.20 1 0 1 1241.78 23.70 0 1 -1 1275.57 25.70 1 0 -1 1287.07 29.80 1 1 0 1281.37 31.50 -1 -1 -1 156.68 4.90 -1 -1 -1 157.28 8.50 -1 -1 1 159.78 10.00 1 -1 1 163.18 6.10 1 1 1 157.98 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46.40 13.60 -9 1 1 44.50 15.50 _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 56284 # start Validation Reply Form _vrf_PLAT973_I ; PROBLEM: Check Calcd Positive Residual Density on Pb01 2.62 eA-3 RESPONSE: Disorder in this site should have been seen in related disorders, and as it is less than 3% of a Pb, it was left alone. ; # end Validation Reply Form