data_FAPbBr _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'Br8 Pb2, 4(C H5 N2)' _chemical_formula_sum 'C4 H20 Br8 N8 Pb2' _chemical_formula_weight 1233.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0050 0.0020 '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' 0.0090 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.9621 2.9511 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -7.4040 10.6371 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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' _cell_length_a 8.5642(17) _cell_length_b 11.884(2) _cell_length_c 14.312(3) _cell_angle_alpha 65.92(3) _cell_angle_beta 73.01(3) _cell_angle_gamma 83.76(3) _cell_volume 1271.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 500 _cell_measurement_theta_min 3.2 _cell_measurement_theta_max 30.2 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 3.222 _exptl_crystal_F_000 1088 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 32.519 _shelx_estimated_absorpt_T_min 0.138 _shelx_estimated_absorpt_T_max 0.138 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.060 _exptl_absorpt_correction_T_max 0.060 _exptl_absorpt_process_details 'Scala (Evans, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.80246 _diffrn_radiation_type synchrotron _diffrn_source ? _diffrn_measurement_device_type 'Rayonix SX165 CCD' _diffrn_measurement_method '/f scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 23009 _diffrn_reflns_av_unetI/netI 0.1277 _diffrn_reflns_av_R_equivalents 0.1179 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.162 _diffrn_reflns_theta_max 30.872 _diffrn_reflns_theta_full 28.782 _diffrn_measured_fraction_theta_max 1.021 _diffrn_measured_fraction_theta_full 1.022 _diffrn_reflns_Laue_measured_fraction_max 1.021 _diffrn_reflns_Laue_measured_fraction_full 1.022 _diffrn_reflns_point_group_measured_fraction_max 1.021 _diffrn_reflns_point_group_measured_fraction_full 1.022 _reflns_number_total 5242 _reflns_number_gt 4435 _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 'Marccd (Doyle, 2011)' _computing_cell_refinement 'iMosflm (Battye et al., 2011)' _computing_data_reduction 'iMosflm' _computing_structure_solution 'SHELXT (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL (Sheldrick, 2015)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2015)' _computing_publication_material 'SHELXTL' _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.01P)^2^+200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary difmap _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5242 _refine_ls_number_parameters 159 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1188 _refine_ls_R_factor_gt 0.1115 _refine_ls_wR_factor_ref 0.2434 _refine_ls_wR_factor_gt 0.2395 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.67785(11) 0.69574(8) 0.15803(8) 0.0179(3) Uani 1 1 d . . . . . Pb2 Pb 0.33971(11) 0.81752(8) -0.18309(8) 0.0174(3) Uani 1 1 d . . . . . Br1 Br 1.0108(3) 0.7608(2) -0.0105(2) 0.0236(5) Uani 1 1 d . . . . . Br2 Br 0.7128(3) 0.9206(2) 0.2012(2) 0.0234(5) Uani 1 1 d . . . . . Br3 Br 0.3608(3) 0.6575(2) 0.3141(2) 0.0229(5) Uani 1 1 d . . . . . Br4 Br 0.6483(3) 0.4488(2) 0.1563(2) 0.0232(5) Uani 1 1 d . . . . . Br5 Br 0.8563(3) 0.5654(2) 0.3249(2) 0.0242(5) Uani 1 1 d . . . . . Br6 Br 0.5024(3) 0.7868(2) -0.0098(2) 0.0234(5) Uani 1 1 d . . . . . Br7 Br 0.6543(3) 0.8708(2) -0.3443(2) 0.0236(5) Uani 1 1 d . . . . . Br8 Br 0.1637(3) 0.8826(2) -0.3434(2) 0.0236(5) Uani 1 1 d . . . . . N1 N 0.757(3) 0.489(2) 0.8279(19) 0.030(2) Uani 1 1 d . . . . . H1A H 0.8388 0.4478 0.8038 0.036 Uiso 1 1 calc R U . . . H1B H 0.6575 0.4774 0.8285 0.036 Uiso 1 1 calc R U . . . N2 N 0.933(3) 0.588(2) 0.8623(19) 0.030(2) Uani 1 1 d . . . . . H2A H 1.0172 0.5485 0.8388 0.036 Uiso 1 1 calc R U . . . H2B H 0.9463 0.6429 0.8864 0.036 Uiso 1 1 calc R U . . . C1 C 0.784(3) 0.566(2) 0.861(2) 0.030(2) Uani 1 1 d . . . . . H1 H 0.6943 0.6102 0.8870 0.036 Uiso 1 1 calc R U . . . N3 N 0.825(3) -0.011(2) 0.7849(19) 0.030(2) Uani 1 1 d . . . . . H3A H 0.9307 -0.0239 0.7723 0.036 Uiso 1 1 calc R U . . . H3B H 0.7667 -0.0383 0.7564 0.036 Uiso 1 1 calc R U . . . N4 N 0.847(3) 0.088(2) 0.8895(19) 0.030(2) Uani 1 1 d . . . . . H4A H 0.9530 0.0758 0.8768 0.036 Uiso 1 1 calc R U . . . H4B H 0.7996 0.1279 0.9306 0.036 Uiso 1 1 calc R U . . . C2 C 0.755(3) 0.046(2) 0.845(2) 0.030(2) Uani 1 1 d . . . . . H2 H 0.6406 0.0597 0.8583 0.036 Uiso 1 1 calc R U . . . N5 N 0.549(3) 0.1806(18) 0.5394(18) 0.027(5) Uani 1 1 d . . . . . H5A H 0.5053 0.1709 0.6060 0.033 Uiso 1 1 calc R U . . . H5B H 0.6055 0.1206 0.5246 0.033 Uiso 1 1 calc R U . . . N6 N 0.448(3) 0.379(2) 0.4766(18) 0.027(5) Uani 1 1 d . . . . . H6A H 0.4022 0.3728 0.5421 0.033 Uiso 1 1 calc R U . . . H6B H 0.4384 0.4467 0.4224 0.033 Uiso 1 1 calc R U . . . C3 C 0.530(3) 0.287(2) 0.460(2) 0.026(5) Uani 1 1 d . . . . . H3 H 0.5781 0.2953 0.3888 0.031 Uiso 1 1 calc R U . . . N7 N -0.001(3) 0.282(2) 0.4448(19) 0.032(3) Uani 1 1 d . . . . . H7A H 0.0301 0.2202 0.4247 0.038 Uiso 1 1 calc R U . . . H7B H -0.0557 0.3433 0.4089 0.038 Uiso 1 1 calc R U . . . N8 N 0.112(3) 0.197(2) 0.5839(19) 0.032(3) Uani 1 1 d . . . . . H8A H 0.1462 0.1324 0.5679 0.038 Uiso 1 1 calc R U . . . H8B H 0.1310 0.2020 0.6390 0.038 Uiso 1 1 calc R U . . . C4 C 0.033(3) 0.282(2) 0.527(2) 0.032(3) Uani 1 1 d . . . . . H4 H -0.0027 0.3499 0.5465 0.038 Uiso 1 1 calc R U . . . 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 0.0148(5) 0.0137(4) 0.0331(5) -0.0146(4) -0.0100(4) -0.0004(3) Pb2 0.0143(5) 0.0128(4) 0.0333(5) -0.0143(4) -0.0102(4) -0.0004(3) Br1 0.0160(11) 0.0243(11) 0.0376(13) -0.0191(10) -0.0055(9) -0.0046(9) Br2 0.0264(12) 0.0133(10) 0.0402(13) -0.0180(9) -0.0125(10) 0.0014(9) Br3 0.0185(11) 0.0210(11) 0.0352(13) -0.0156(10) -0.0092(9) 0.0007(9) Br4 0.0194(11) 0.0145(10) 0.0462(14) -0.0194(10) -0.0128(10) -0.0002(9) Br5 0.0225(12) 0.0228(11) 0.0379(13) -0.0181(10) -0.0163(10) 0.0058(9) Br6 0.0197(11) 0.0241(11) 0.0342(13) -0.0138(10) -0.0150(9) -0.0003(9) Br7 0.0177(11) 0.0235(11) 0.0361(13) -0.0176(10) -0.0076(9) -0.0020(9) Br8 0.0194(11) 0.0258(12) 0.0379(13) -0.0211(10) -0.0146(10) 0.0042(9) N1 0.020(4) 0.026(5) 0.056(6) -0.022(4) -0.022(4) 0.000(4) N2 0.020(4) 0.026(5) 0.056(6) -0.022(4) -0.022(4) 0.000(4) C1 0.020(4) 0.026(5) 0.056(6) -0.022(4) -0.022(4) 0.000(4) N3 0.020(4) 0.026(5) 0.056(6) -0.022(4) -0.022(4) 0.000(4) N4 0.020(4) 0.026(5) 0.056(6) -0.022(4) -0.022(4) 0.000(4) C2 0.020(4) 0.026(5) 0.056(6) -0.022(4) -0.022(4) 0.000(4) N5 0.036(12) 0.010(8) 0.037(12) -0.007(8) -0.016(10) 0.000(8) N6 0.025(11) 0.028(11) 0.036(12) -0.019(9) -0.006(9) -0.009(9) C3 0.022(12) 0.026(12) 0.038(14) -0.012(10) -0.018(10) -0.005(10) N7 0.032(8) 0.027(6) 0.046(8) -0.021(6) -0.017(6) 0.009(6) N8 0.032(8) 0.027(6) 0.046(8) -0.021(6) -0.017(6) 0.009(6) C4 0.032(8) 0.027(6) 0.046(8) -0.021(6) -0.017(6) 0.009(6) _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 Br3 2.910(3) . ? Pb1 Br6 2.972(3) . ? Pb1 Br4 2.983(2) . ? Pb1 Br5 3.006(3) . ? Pb1 Br2 3.040(2) . ? Pb1 Br1 3.080(3) . ? Pb2 Br8 2.908(3) . ? Pb2 Br7 2.921(3) . ? Pb2 Br2 3.010(2) 2_675 ? Pb2 Br4 3.023(2) 2_665 ? Pb2 Br6 3.065(3) . ? Pb2 Br1 3.079(3) 1_455 ? Br1 Pb2 3.079(3) 1_655 ? Br2 Pb2 3.010(2) 2_675 ? Br4 Pb2 3.023(2) 2_665 ? N1 C1 1.25(3) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? N2 C1 1.33(3) . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? C1 H1 0.9500 . ? N3 C2 1.28(4) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? N4 C2 1.39(3) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? C2 H2 0.9500 . ? N5 C3 1.34(3) . ? N5 H5A 0.8800 . ? N5 H5B 0.8800 . ? N6 C3 1.30(3) . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? C3 H3 0.9500 . ? N7 C4 1.29(4) . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? N8 C4 1.28(4) . ? N8 H8A 0.8800 . ? N8 H8B 0.8800 . ? C4 H4 0.9500 . ? 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 Br3 Pb1 Br6 87.80(8) . . ? Br3 Pb1 Br4 89.81(8) . . ? Br6 Pb1 Br4 85.05(8) . . ? Br3 Pb1 Br5 93.15(8) . . ? Br6 Pb1 Br5 171.00(7) . . ? Br4 Pb1 Br5 86.01(7) . . ? Br3 Pb1 Br2 86.26(8) . . ? Br6 Pb1 Br2 104.55(8) . . ? Br4 Pb1 Br2 169.46(8) . . ? Br5 Pb1 Br2 84.45(7) . . ? Br3 Pb1 Br1 174.86(7) . . ? Br6 Pb1 Br1 91.32(8) . . ? Br4 Pb1 Br1 95.16(8) . . ? Br5 Pb1 Br1 88.52(8) . . ? Br2 Pb1 Br1 89.06(7) . . ? Br8 Pb2 Br7 91.78(8) . . ? Br8 Pb2 Br2 86.40(8) . 2_675 ? Br7 Pb2 Br2 94.31(8) . 2_675 ? Br8 Pb2 Br4 90.69(8) . 2_665 ? Br7 Pb2 Br4 91.42(8) . 2_665 ? Br2 Pb2 Br4 173.64(7) 2_675 2_665 ? Br8 Pb2 Br6 170.81(8) . . ? Br7 Pb2 Br6 91.37(7) . . ? Br2 Pb2 Br6 84.77(8) 2_675 . ? Br4 Pb2 Br6 97.85(8) 2_665 . ? Br8 Pb2 Br1 89.09(7) . 1_455 ? Br7 Pb2 Br1 179.12(7) . 1_455 ? Br2 Pb2 Br1 85.62(8) 2_675 1_455 ? Br4 Pb2 Br1 88.68(8) 2_665 1_455 ? Br6 Pb2 Br1 87.74(7) . 1_455 ? Pb2 Br1 Pb1 177.29(8) 1_655 . ? Pb2 Br2 Pb1 156.48(10) 2_675 . ? Pb1 Br4 Pb2 168.95(10) . 2_665 ? Pb1 Br6 Pb2 165.90(10) . . ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C1 N2 H2A 120.0 . . ? C1 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? N1 C1 N2 123(3) . . ? N1 C1 H1 118.7 . . ? N2 C1 H1 118.7 . . ? C2 N3 H3A 120.0 . . ? C2 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C2 N4 H4A 120.0 . . ? C2 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? N3 C2 N4 120(2) . . ? N3 C2 H2 120.1 . . ? N4 C2 H2 120.1 . . ? C3 N5 H5A 120.0 . . ? C3 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C3 N6 H6A 120.0 . . ? C3 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N6 C3 N5 123(3) . . ? N6 C3 H3 118.5 . . ? N5 C3 H3 118.5 . . ? C4 N7 H7A 120.0 . . ? C4 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C4 N8 H8A 120.0 . . ? C4 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? N8 C4 N7 124(3) . . ? N8 C4 H4 117.8 . . ? N7 C4 H4 117.8 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A Br5 0.88 2.75 3.55(2) 151.9 2_766 N1 H1B Br4 0.88 2.64 3.43(2) 149.5 2_666 N2 H2A Br4 0.88 2.89 3.51(2) 129.2 2_766 N2 H2A Br5 0.88 3.05 3.77(2) 141.1 2_766 N2 H2B Br1 0.88 2.60 3.47(2) 166.9 1_556 N3 H3A Br8 0.88 2.66 3.37(2) 139.2 1_646 N3 H3B Br7 0.88 2.55 3.41(2) 168.5 1_546 N4 H4A Br2 0.88 2.75 3.61(2) 168.0 2_766 N4 H4B Br6 0.88 2.77 3.50(2) 141.2 2_666 N5 H5A Br2 0.88 2.70 3.51(2) 155.0 2_666 N5 H5B Br7 0.88 2.86 3.51(2) 132.1 1_546 N5 H5B Br8 0.88 2.78 3.43(2) 132.3 2_665 N6 H6A Br5 0.88 2.72 3.49(2) 146.3 2_666 N6 H6B Br3 0.88 2.49 3.34(2) 162.3 . N7 H7A Br7 0.88 2.89 3.56(2) 133.6 2_665 N7 H7B Br5 0.88 2.55 3.38(2) 157.4 1_455 N8 H8A Br8 0.88 2.72 3.46(2) 142.2 1_546 N8 H8B Br2 0.88 2.79 3.52(2) 141.6 2_666 _refine_diff_density_max 6.464 _refine_diff_density_min -4.798 _refine_diff_density_rms 0.649 _shelxl_version_number 2013-4 _shelx_res_file ; TITL FAPbBr in P-1 CELL 0.80246 8.5642 11.8840 14.3121 65.918 73.013 83.758 ZERR 2.00 0.0017 0.0024 0.0029 0.030 0.030 0.030 LATT 1 SFAC C H N Br Pb DISP C 0.005 0.002 15.071 DISP H -0 0 0.629 DISP N 0.009 0.004 26.694 DISP Br -0.9621 2.9511 13715.451 DISP Pb -7.4040 10.6371 49287.003 UNIT 8 40 16 16 4 TEMP -173.0 SIZE 0.10 0.10 0.10 OMIT 2 8 2 OMIT 4 5 5 OMIT 0 12 1 OMIT 2 9 0 OMIT -2 -8 3 OMIT 2 8 8 OMIT 3 6 0 OMIT -1 -10 2 OMIT 1 10 4 OMIT 2 9 9 OMIT 4 4 2 OMIT 2 8 3 OMIT -1 -9 2 OMIT -2 -8 4 OMIT 0 12 9 OMIT 3 7 2 OMIT -3 -7 5 OMIT 5 3 8 OMIT 6 0 1 OMIT 8 8 8 OMIT 2 7 5 OMIT 1 12 8 OMIT 4 5 0 OMIT 1 10 10 OMIT 2 9 2 OMIT -8 2 4 OMIT 4 4 10 OMIT -7 2 0 OMIT 5 2 1 OMIT 3 8 10 OMIT 5 3 4 OMIT 6 12 12 OMIT 6 0 5 OMIT 6 0 7 OMIT 8 8 2 OMIT 3 7 6 OMIT 1 8 6 OMIT -3 -6 3 OMIT 2 -4 1 OMIT 7 10 4 OMIT 10 5 10 OMIT -3 -6 6 OMIT -4 -5 4 OMIT 0 12 7 OMIT 1 -3 2 OMIT -1 2 9 OMIT 9 6 6 OMIT -1 3 9 OMIT -1 2 0 OMIT 10 6 5 OMIT 9 8 7 OMIT 4 4 4 OMIT 6 1 11 OMIT 0 12 3 OMIT 10 4 8 OMIT 0 11 6 OMIT 2 8 11 OMIT 3 -6 5 OMIT 7 -1 6 OMIT 4 5 1 OMIT -5 -2 4 OMIT 4 5 11 OMIT 3 8 4 OMIT 3 7 1 OMIT 2 8 5 OMIT 8 9 5 OMIT 1 11 8 OMIT -6 0 1 OMIT 5 3 1 OMIT 0 0 12 OMIT 2 9 11 OMIT 8 9 14 OMIT -2 4 11 OMIT -5 -2 2 OMIT 4 4 7 OMIT -4 -4 2 OMIT 7 0 7 OMIT -3 6 13 OMIT -3 6 12 OMIT -1 2 11 OMIT 0 13 9 OMIT 7 0 4 OMIT 2 7 8 OMIT -5 -2 1 OMIT 7 10 10 OMIT 5 4 9 OMIT 6 -1 6 OMIT 4 5 2 OMIT 0 12 0 OMIT 9 6 3 OMIT 9 7 12 OMIT 2 9 3 OMIT -1 -10 4 OMIT -3 -6 2 OMIT 4 4 8 OMIT 1 10 7 OMIT -4 -5 2 OMIT 5 3 11 OMIT 5 3 7 OMIT 7 -1 8 OMIT 6 2 0 OMIT 3 7 10 OMIT 7 11 10 OMIT 6 1 6 OMIT 8 10 6 OMIT 3 7 4 OMIT 4 4 6 OMIT -1 -10 1 OMIT 7 0 1 OMIT -7 0 2 OMIT 8 9 9 OMIT 5 3 10 OMIT 6 1 1 OMIT 7 11 13 OMIT -5 -2 5 OMIT 3 6 3 OMIT 0 -12 1 OMIT 8 10 9 OMIT 7 10 7 OMIT 3 6 1 OMIT 4 4 12 OMIT 3 7 15 OMIT -1 2 13 OMIT 1 8 9 OMIT 6 12 9 OMIT 8 7 7 OMIT 4 14 9 OMIT -3 6 7 OMIT 9 7 11 OMIT 1 10 1 OMIT 2 8 9 OMIT -2 3 10 OMIT 6 1 2 OMIT 6 0 11 OMIT 6 12 6 OMIT 5 4 6 OMIT 6 2 1 OMIT -2 4 2 OMIT -4 -6 1 OMIT 2 -4 4 OMIT 2 -4 7 OMIT 6 11 11 OMIT -1 14 4 OMIT 2 8 14 OMIT 2 10 4 OMIT 1 -1 11 OMIT 0 12 13 OMIT 2 -4 13 OMIT 4 3 2 OMIT -3 6 9 OMIT 7 0 10 OMIT 3 6 6 OMIT 8 7 9 OMIT 9 6 5 OMIT 1 10 5 OMIT 8 -1 5 OMIT 3 7 12 OMIT -2 -7 1 OMIT 5 2 2 OMIT -2 4 8 OMIT 5 2 4 OMIT -2 5 9 OMIT 10 4 5 OMIT 0 -12 3 OMIT 4 4 9 OMIT 6 2 2 OMIT -1 2 6 OMIT 3 8 8 OMIT 1 11 14 OMIT 1 8 3 OMIT 7 -1 9 OMIT 1 -2 3 OMIT 0 13 7 OMIT -7 2 5 OMIT 3 6 12 OMIT -2 5 3 OMIT 10 6 8 OMIT 0 0 11 OMIT 1 11 12 OMIT 7 9 16 OMIT -2 -8 1 OMIT 3 7 13 OMIT -3 7 5 OMIT 1 9 7 OMIT 0 14 6 OMIT 4 -8 9 OMIT 7 12 8 OMIT -4 -4 3 OMIT 3 6 2 OMIT 7 12 11 OMIT -3 14 5 OMIT 1 -2 13 OMIT 6 2 6 OMIT 1 12 6 OMIT 2 9 6 OMIT 2 10 10 OMIT -1 14 9 OMIT 6 1 12 OMIT 0 11 7 OMIT 0 12 6 OMIT -3 -6 5 OMIT 1 11 0 OMIT 0 12 15 OMIT 3 5 3 OMIT 6 12 11 OMIT 4 6 1 OMIT -1 3 7 OMIT -2 4 5 OMIT -1 14 10 OMIT 6 -1 5 OMIT -2 -9 4 OMIT 6 13 7 OMIT -6 -1 4 OMIT 1 10 11 OMIT 2 8 10 OMIT -6 -1 7 OMIT 5 14 7 OMIT 6 -1 4 OMIT 4 6 7 OMIT 10 6 4 OMIT 7 11 12 OMIT -1 12 4 OMIT 2 10 9 OMIT 10 4 2 OMIT -2 1 14 OMIT 2 -5 3 OMIT 4 5 10 OMIT 6 -1 1 OMIT -1 -1 6 OMIT -3 6 15 OMIT 2 -3 10 OMIT 0 -10 1 OMIT 1 10 16 OMIT 6 10 5 OMIT 1 10 13 OMIT -6 -2 1 OMIT 2 9 4 OMIT 0 10 6 OMIT 5 4 5 OMIT 6 0 6 OMIT 3 8 1 OMIT 3 -7 4 OMIT 5 3 14 OMIT -1 2 3 OMIT 8 -4 1 OMIT 0 11 3 OMIT 8 11 9 OMIT 8 -4 7 OMIT 6 11 5 OMIT -4 7 8 OMIT 2 -3 1 OMIT -3 6 1 OMIT 9 -5 4 OMIT -3 6 3 OMIT -3 4 0 OMIT 4 6 5 OMIT -9 6 1 OMIT 4 -8 3 OMIT -1 1 9 OMIT 6 -2 4 OMIT 9 -4 6 OMIT 9 4 6 OMIT 6 11 7 OMIT 7 -1 3 OMIT 5 4 3 OMIT -9 4 0 OMIT -2 4 10 OMIT -2 14 4 OMIT 8 -5 2 OMIT 3 8 2 OMIT -4 8 3 OMIT -2 3 4 OMIT 5 -9 7 OMIT 8 6 7 OMIT -3 6 6 OMIT 8 -3 6 OMIT 0 14 8 OMIT -2 4 1 OMIT 5 4 11 OMIT 1 0 4 OMIT 1 -2 1 OMIT -4 9 2 OMIT 8 -2 2 OMIT -6 10 6 OMIT 4 4 13 OMIT -3 -6 4 OMIT -7 2 3 L.S. 12 BOND $H ACTA CONF TWIN -1 0 0 0 -1 0 -1 -1 1 2 EADP N1 N2 C1 N3 N4 C2 EADP N7 N8 C4 EQIV $1 -x+2, -y+1, -z+1 HTAB N1 Br5_$1 EQIV $2 -x+1, -y+1, -z+1 HTAB N1 Br3_$2 HTAB N1 Br4_$2 HTAB N2 Br4_$1 HTAB N2 Br5_$1 EQIV $3 x, y, z+1 HTAB N2 Br1_$3 EQIV $4 x+1, y-1, z+1 HTAB N3 Br8_$4 EQIV $5 x, y-1, z+1 HTAB N3 Br7_$5 HTAB N4 Br2_$1 HTAB N4 Br1_$1 HTAB N4 Br6_$2 HTAB N5 Br2_$2 HTAB N5 Br7_$5 EQIV $6 -x+1, -y+1, -z HTAB N5 Br8_$6 HTAB N6 Br5_$2 HTAB N6 Br3 HTAB C3 Br4 HTAB C3 Br8_$6 HTAB N7 Br7_$6 EQIV $7 -x, -y+1, -z HTAB N7 Br8_$7 EQIV $8 x-1, y, z HTAB N7 Br5_$8 HTAB N8 Br8_$5 HTAB N8 Br2_$2 HTAB N8 Br5_$2 HTAB C4 Br5_$2 WGHT 0.010000 200.000000 EXTI 0.002163 BASF 0.00818 FVAR 0.20042 PB1 5 0.677846 0.695739 0.158028 11.00000 0.01485 0.01366 = 0.03313 -0.01464 -0.01001 -0.00036 PB2 5 0.339712 0.817522 -0.183085 11.00000 0.01426 0.01277 = 0.03326 -0.01427 -0.01018 -0.00042 BR1 4 1.010779 0.760843 -0.010507 11.00000 0.01599 0.02430 = 0.03755 -0.01912 -0.00554 -0.00465 BR2 4 0.712812 0.920621 0.201197 11.00000 0.02638 0.01333 = 0.04018 -0.01805 -0.01251 0.00143 BR3 4 0.360826 0.657506 0.314147 11.00000 0.01851 0.02096 = 0.03515 -0.01561 -0.00923 0.00066 BR4 4 0.648275 0.448831 0.156323 11.00000 0.01938 0.01450 = 0.04616 -0.01939 -0.01279 -0.00021 BR5 4 0.856328 0.565357 0.324885 11.00000 0.02249 0.02276 = 0.03790 -0.01813 -0.01633 0.00583 BR6 4 0.502371 0.786840 -0.009796 11.00000 0.01973 0.02415 = 0.03417 -0.01384 -0.01504 -0.00033 BR7 4 0.654314 0.870784 -0.344315 11.00000 0.01771 0.02348 = 0.03610 -0.01759 -0.00760 -0.00201 BR8 4 0.163731 0.882557 -0.343419 11.00000 0.01940 0.02580 = 0.03794 -0.02110 -0.01457 0.00417 N1 3 0.757414 0.489486 0.827873 11.00000 0.02020 0.02629 = 0.05637 -0.02200 -0.02189 0.00009 AFIX 93 H1A 2 0.838825 0.447806 0.803758 11.00000 -1.20000 H1B 2 0.657462 0.477410 0.828523 11.00000 -1.20000 AFIX 0 N2 3 0.932716 0.588361 0.862303 11.00000 0.02020 0.02629 = 0.05637 -0.02200 -0.02189 0.00009 AFIX 93 H2A 2 1.017245 0.548508 0.838832 11.00000 -1.20000 H2B 2 0.946329 0.642859 0.886412 11.00000 -1.20000 AFIX 0 C1 1 0.783854 0.566147 0.861335 11.00000 0.02020 0.02629 = 0.05637 -0.02200 -0.02189 0.00009 AFIX 43 H1 2 0.694259 0.610169 0.887028 11.00000 -1.20000 AFIX 0 N3 3 0.824779 -0.011370 0.784884 11.00000 0.02020 0.02629 = 0.05637 -0.02200 -0.02189 0.00009 AFIX 93 H3A 2 0.930690 -0.023890 0.772328 11.00000 -1.20000 H3B 2 0.766749 -0.038264 0.756409 11.00000 -1.20000 AFIX 0 N4 3 0.847123 0.088429 0.889536 11.00000 0.02020 0.02629 = 0.05637 -0.02200 -0.02189 0.00009 AFIX 93 H4A 2 0.953014 0.075778 0.876842 11.00000 -1.20000 H4B 2 0.799564 0.127870 0.930598 11.00000 -1.20000 AFIX 0 C2 1 0.754960 0.046100 0.844713 11.00000 0.02020 0.02629 = 0.05637 -0.02200 -0.02189 0.00009 AFIX 43 H2 2 0.640635 0.059686 0.858342 11.00000 -1.20000 AFIX 0 N5 3 0.549061 0.180591 0.539356 11.00000 0.03637 0.01016 = 0.03726 -0.00748 -0.01572 -0.00016 AFIX 93 H5A 2 0.505255 0.170893 0.606000 11.00000 -1.20000 H5B 2 0.605520 0.120629 0.524602 11.00000 -1.20000 AFIX 0 N6 3 0.448054 0.378650 0.476624 11.00000 0.02494 0.02762 = 0.03634 -0.01900 -0.00620 -0.00917 AFIX 93 H6A 2 0.402238 0.372843 0.542067 11.00000 -1.20000 H6B 2 0.438418 0.446713 0.422368 11.00000 -1.20000 AFIX 0 C3 1 0.529745 0.286933 0.460143 11.00000 0.02189 0.02563 = 0.03781 -0.01176 -0.01789 -0.00467 AFIX 43 H3 2 0.578137 0.295305 0.388822 11.00000 -1.20000 AFIX 0 N7 3 -0.001198 0.281834 0.444761 11.00000 0.03167 0.02671 = 0.04577 -0.02116 -0.01673 0.00913 AFIX 93 H7A 2 0.030083 0.220243 0.424663 11.00000 -1.20000 H7B 2 -0.055677 0.343305 0.408919 11.00000 -1.20000 AFIX 0 N8 3 0.111637 0.196502 0.583943 11.00000 0.03167 0.02671 = 0.04577 -0.02116 -0.01673 0.00913 AFIX 93 H8A 2 0.146204 0.132420 0.567890 11.00000 -1.20000 H8B 2 0.131043 0.201969 0.639040 11.00000 -1.20000 AFIX 0 C4 1 0.032899 0.282011 0.526983 11.00000 0.03167 0.02671 = 0.04577 -0.02116 -0.01673 0.00913 AFIX 43 H4 2 -0.002669 0.349894 0.546510 11.00000 -1.20000 AFIX 0 HKLF 4 REM FAPbBr in P-1 REM R1 = 0.1115 for 4435 Fo > 4sig(Fo) and 0.1188 for all 5242 data REM 159 parameters refined using 0 restraints END WGHT 0.1253 130.9079 REM Highest difference peak 6.464, deepest hole -4.798, 1-sigma level 0.649 Q1 1 0.3017 0.7879 -0.1130 11.00000 0.05 6.46 Q2 1 0.6331 0.6639 0.2241 11.00000 0.05 5.93 Q3 1 0.8262 0.7773 0.1571 11.00000 0.05 5.69 Q4 1 0.1924 0.7366 -0.1890 11.00000 0.05 5.22 Q5 1 0.7098 0.7198 0.0965 11.00000 0.05 5.21 Q6 1 0.5006 0.8997 -0.1857 11.00000 0.05 4.97 Q7 1 0.3753 0.8432 -0.2460 11.00000 0.05 4.86 Q8 1 0.5195 0.6151 0.1546 11.00000 0.05 4.84 Q9 1 0.3152 0.6216 0.3828 11.00000 0.05 3.09 Q10 1 0.0349 -0.0023 0.5219 11.00000 0.05 3.00 Q11 1 0.2608 0.7283 -0.1011 11.00000 0.05 2.99 Q12 1 0.7035 0.4832 0.3330 11.00000 0.05 2.93 Q13 1 0.9801 0.7252 0.0560 11.00000 0.05 2.86 Q14 1 0.3761 0.8218 -0.0993 11.00000 0.05 2.79 Q15 1 0.6249 0.8392 -0.2824 11.00000 0.05 2.76 Q16 1 0.6513 0.8743 -0.0068 11.00000 0.05 2.72 Q17 1 0.1235 0.8380 -0.2756 11.00000 0.05 2.72 Q18 1 0.7617 0.9627 0.1338 11.00000 0.05 2.70 Q19 1 0.6055 0.4210 0.2188 11.00000 0.05 2.60 Q20 1 0.6597 0.8989 0.1260 11.00000 0.05 2.59 ; _shelx_res_checksum 12278 _shelx_hkl_file ; -10 -2 1 -8.44 14.47 -10 -2 1 2.63 10.84 -10 -2 1 -4.21 13.03 10 2 -1 -8.56 18.23 10 2 -1 -1.47 11.13 -10 -1 1 4.88 14.11 -10 -1 1 7.17 12.83 10 1 -1 6.57 14.91 10 1 -1 3.29 15.81 -10 0 1 9.98 16.98 -10 0 1 9.59 12.31 -10 0 1 2.99 12.81 10 0 -1 4.05 12.52 -10 0 2 -6.52 15.00 -10 0 2 6.70 13.87 -10 0 2 3.26 12.80 -10 1 1 71.79 20.49 -10 1 1 126.44 36.15 -10 1 1 141.96 37.88 10 -1 -1 5.42 16.76 10 -1 -1 70.99 18.94 10 -1 -1 122.58 35.80 -10 1 2 7.91 13.98 -10 1 2 3.39 12.14 -10 1 2 3.23 12.66 10 -1 -2 -2.38 15.63 10 -1 -2 -4.08 15.63 -10 2 1 35.47 13.55 -10 2 1 128.94 30.94 -10 2 1 123.95 32.92 10 -2 -1 -2.77 14.10 10 -2 -1 37.44 13.80 10 -2 -1 106.99 30.19 -10 2 2 10.79 13.26 -10 3 1 22.20 15.25 -10 3 1 20.90 15.42 10 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31.06 0 8 -6 213.55 30.20 0 8 -6 232.44 75.07 0 -8 7 33.00 10.17 0 -8 7 89.23 28.52 0 8 -7 64.59 16.34 0 8 -7 71.94 13.29 0 8 -7 74.36 29.50 0 -8 8 11.96 7.26 0 -8 8 39.18 18.68 0 8 -8 24.00 13.18 0 8 -8 26.28 11.02 0 8 -8 36.12 21.62 0 -8 9 7.51 10.45 0 -8 9 19.45 20.58 0 8 -9 6.27 15.79 0 8 -9 10.76 11.92 0 8 -9 13.36 16.86 0 -7 1 181.40 24.02 0 -7 1 187.63 23.87 0 -7 1 161.74 62.73 0 7 -1 180.00 23.95 0 7 -1 204.72 24.15 0 -7 2 86.39 11.14 0 -7 2 89.25 12.53 0 -7 2 81.77 30.94 0 7 -2 99.05 13.53 0 7 -2 94.96 11.27 0 7 -2 68.33 30.52 0 -7 3 281.75 38.57 0 -7 3 302.14 39.68 0 -7 3 319.21 98.66 0 7 -3 277.79 39.33 0 7 -3 293.02 38.65 0 7 -3 238.98 98.23 0 -7 4 2154.40 269.64 0 -7 4 1863.48 269.42 0 -7 4 1864.46 643.16 0 7 -4 1874.74 269.28 0 7 -4 2009.64 269.81 0 7 -4 1644.38 643.12 0 -7 5 32.31 9.08 0 -7 5 28.37 18.18 0 7 -5 40.96 13.59 0 7 -5 25.55 10.79 0 7 -5 34.53 20.10 0 -7 6 261.04 37.89 0 -7 6 304.98 94.84 0 7 -6 233.25 39.47 0 7 -6 274.66 38.74 0 7 -6 277.92 95.16 0 -7 7 4.61 9.45 0 -7 7 4.17 14.82 0 7 -7 -0.50 14.84 0 7 -7 3.17 11.14 0 7 -7 15.80 18.15 0 -7 8 3.13 10.54 0 -7 8 4.66 16.02 0 7 -8 -6.08 13.01 0 7 -8 -3.95 13.57 0 7 -8 11.09 16.96 0 -7 9 251.87 40.07 0 -7 9 383.48 98.17 0 7 -9 226.18 39.99 0 7 -9 189.40 39.54 0 7 -9 310.19 98.25 0 -7 10 549.99 81.28 0 -7 10 733.23 196.22 0 7 -10 501.35 81.05 0 7 -10 370.25 80.75 0 7 -10 618.98 195.86 0 -7 11 2.42 14.44 0 7 -11 1.13 11.26 0 7 -11 4.39 12.49 0 7 -11 3.96 14.13 0 -6 1 30.64 5.00 0 -6 1 21.57 6.19 0 -6 1 29.10 12.53 0 6 -1 24.21 6.05 0 6 -1 28.87 5.99 0 6 -1 17.70 12.42 0 -6 2 170.27 21.45 0 -6 2 190.41 22.31 0 -6 2 167.15 57.50 0 6 -2 188.94 22.88 0 6 -2 164.48 21.51 0 6 -2 129.72 57.31 0 -6 3 488.30 64.42 0 -6 3 519.98 64.62 0 -6 3 472.67 158.93 0 6 -3 509.32 64.56 0 6 -3 511.14 64.48 0 6 -3 339.21 158.77 0 -6 4 696.83 101.12 0 -6 4 698.55 100.93 0 -6 4 756.70 245.63 0 6 -4 664.71 101.05 0 6 -4 720.59 101.17 0 6 -4 747.66 245.64 0 -6 5 -2.47 9.12 0 -6 5 -0.50 13.37 0 6 -5 9.99 13.35 0 6 -5 -2.84 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143.50 0 -4 2 1125.97 143.66 0 -4 2 913.92 346.01 0 4 -2 1195.42 143.60 0 4 -2 819.45 345.99 0 -4 3 71.00 17.98 0 -4 3 107.67 18.78 0 -4 3 222.81 49.60 0 4 -3 73.64 18.45 0 4 -3 54.61 17.97 0 4 -3 234.29 49.67 0 -4 4 3077.75 388.17 0 -4 4 2938.77 387.51 0 -4 4 2409.70 924.00 0 4 -4 2953.55 388.01 0 4 -4 2906.97 388.17 0 4 -4 2415.21 924.00 0 -4 5 1732.04 229.35 0 -4 5 1551.87 548.74 0 4 -5 1682.18 229.13 0 4 -5 1552.79 229.22 0 4 -5 1595.99 548.86 0 -4 6 100.29 15.82 0 -4 6 116.23 39.74 0 4 -6 111.88 17.80 0 4 -6 89.99 14.39 0 4 -6 120.07 40.82 0 -4 7 39.45 9.23 0 -4 7 58.81 21.30 0 4 -7 42.63 13.33 0 4 -7 40.95 9.45 0 4 -7 51.25 23.71 0 -4 8 83.13 15.99 0 -4 8 140.51 41.29 0 4 -8 93.72 17.73 0 4 -8 84.26 16.16 0 4 -8 137.60 42.96 0 -4 9 16.00 8.78 0 -4 9 13.82 15.32 0 4 -9 24.04 11.11 0 4 -9 43.86 10.05 0 4 -9 24.60 19.38 0 -4 10 241.84 42.12 0 -4 10 385.12 105.10 0 4 -10 259.68 42.65 0 4 -10 231.72 42.10 0 4 -10 336.24 105.56 0 -4 11 32.85 10.45 0 -4 11 58.44 20.22 0 4 -11 30.74 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-2 -13 715.42 117.44 0 -2 -13 634.39 116.38 0 -2 -13 799.54 282.64 0 2 14 1.09 14.81 0 2 14 2.15 16.30 0 -2 -14 40.54 18.13 0 -2 -14 34.84 18.10 0 -2 -14 1.94 16.12 0 2 15 26.05 11.28 0 2 15 19.65 18.15 0 -2 -15 9.01 14.89 0 -2 -15 27.11 14.30 0 -2 -15 26.40 18.43 0 -2 -16 -0.38 10.19 0 2 16 2.95 13.41 0 2 16 7.64 13.59 0 -2 -16 5.17 19.05 0 -2 -16 13.87 19.53 0 3 0 592.31 78.42 0 3 0 608.62 78.52 0 3 0 536.09 192.02 0 -3 0 610.15 78.51 0 -3 0 491.24 191.87 0 3 1 89.03 9.54 0 3 1 82.71 9.57 0 3 1 76.59 28.54 0 -3 -1 87.76 9.25 0 -3 -1 86.08 9.59 0 -3 -1 80.09 28.79 0 3 2 3.38 3.41 0 3 2 0.40 3.87 0 -3 -2 0.05 3.68 0 -3 -2 0.33 2.64 0 3 3 726.25 98.77 0 3 3 679.92 240.50 0 -3 -3 725.60 98.89 0 -3 -3 705.84 240.50 0 3 4 10.13 7.04 0 3 4 9.91 5.02 0 -3 -4 10.25 4.13 0 3 5 6.94 9.28 0 3 5 2.52 7.22 0 3 5 2.20 5.60 0 -3 -5 4.43 6.12 0 -3 -5 1.77 5.77 0 3 6 7.51 10.46 0 3 6 6.24 5.34 0 -3 -6 8.84 6.61 0 -3 -6 5.84 5.77 0 3 7 538.07 76.29 0 3 7 501.25 187.20 0 -3 -7 498.90 76.01 0 -3 -7 653.01 187.30 0 3 8 6.39 9.69 0 3 8 1.61 7.62 0 -3 -8 0.36 7.80 0 -3 -8 7.54 8.34 0 3 9 760.54 113.80 0 3 9 888.08 275.53 0 -3 -9 631.44 113.35 0 -3 -9 871.30 275.52 0 3 10 9.72 11.98 0 3 10 5.34 12.67 0 -3 -10 6.67 14.87 0 -3 -10 7.66 9.75 0 3 11 18.00 15.24 0 3 11 25.58 12.77 0 -3 -11 26.01 14.91 0 -3 -11 27.09 13.25 0 3 12 21.16 12.60 0 -3 -12 28.90 14.31 0 -3 -12 18.92 14.28 0 3 13 890.51 119.47 0 -3 -13 740.08 119.10 0 -3 -13 871.82 287.90 0 3 14 29.75 12.03 0 3 14 30.64 19.95 0 -3 -14 27.74 14.95 0 -3 -14 15.03 11.70 0 -3 -14 22.65 18.87 0 3 15 505.05 61.37 0 3 15 439.49 147.23 0 -3 -15 381.80 60.44 0 -3 -15 360.36 59.65 0 -3 -15 426.32 147.73 0 3 16 12.62 10.88 0 3 16 8.71 14.05 0 3 16 2.43 14.07 0 -3 -16 8.74 14.94 0 -3 -16 13.45 13.70 0 -3 -16 -0.25 15.31 0 3 17 5.12 12.13 0 3 17 10.00 17.75 0 3 17 3.19 13.57 0 -3 -17 18.68 15.30 0 -3 -17 7.54 16.18 0 -3 -17 9.21 18.05 0 4 0 94.95 10.85 0 4 0 90.01 10.93 0 4 0 102.95 33.37 0 -4 0 95.53 10.83 0 -4 0 82.63 10.79 0 -4 0 83.80 31.92 0 4 3 484.51 78.99 0 4 3 506.94 78.90 0 4 3 725.41 193.32 0 -4 -3 532.16 79.09 0 4 4 800.83 110.41 0 4 4 787.11 268.01 0 -4 -4 724.65 110.56 0 -4 -4 839.30 268.01 0 4 5 291.35 34.14 0 4 5 243.25 86.46 0 4 5 238.11 86.40 0 -4 -5 255.33 33.67 0 4 6 19.80 10.67 0 4 6 25.38 11.35 0 -4 -6 25.81 5.51 0 4 7 4407.08 661.46 0 4 7 4522.87 1570.29 0 -4 -7 4021.30 661.45 0 -4 -7 5507.48 1570.35 0 4 8 2185.30 317.52 0 4 8 1831.34 757.53 0 4 8 2477.44 757.62 0 -4 -8 2021.43 317.45 0 -4 -8 2691.84 757.66 0 -4 -9 139.25 13.25 0 4 9 149.46 20.90 0 4 9 136.34 50.10 0 4 9 155.23 50.22 0 4 10 153.83 20.74 0 4 10 143.48 50.26 0 -4 -10 130.07 19.81 0 -4 -10 140.11 49.42 0 4 11 2.30 11.97 0 4 11 2.58 11.01 0 -4 -11 2.05 12.07 0 -4 -11 11.26 10.03 0 4 12 65.55 15.90 0 4 12 64.65 24.33 0 -4 -12 45.26 13.26 0 -4 -12 65.34 26.66 0 4 13 733.06 108.60 0 4 13 859.16 261.52 0 4 13 817.86 261.26 0 -4 -13 567.63 107.41 0 -4 -13 745.14 261.38 0 4 14 283.82 40.27 0 4 14 333.01 102.19 0 4 14 297.41 101.04 0 -4 -14 215.18 40.28 0 -4 -14 291.32 101.55 0 4 15 0.36 13.92 0 4 15 8.72 12.95 0 4 15 4.39 14.18 0 -4 -15 8.62 10.81 0 -4 -15 6.51 12.25 0 -4 -15 -11.35 17.83 0 4 16 5.55 14.33 0 4 16 1.41 13.18 0 4 16 4.69 14.32 0 -4 -16 12.64 15.43 0 -4 -16 7.29 13.42 0 -4 -16 2.13 15.92 0 4 17 8.33 10.59 0 4 17 6.56 14.18 0 4 17 -2.76 17.27 0 -4 -17 8.94 15.26 0 -4 -17 8.30 13.46 0 -4 -17 6.24 17.09 0 5 0 79.58 8.97 0 5 0 81.16 9.10 0 5 0 67.07 26.96 0 -5 0 83.56 9.01 0 -5 0 82.72 8.98 0 -5 0 66.33 26.98 0 5 1 642.38 85.05 0 5 1 647.35 84.97 0 5 1 507.35 207.35 0 -5 -1 661.64 84.87 0 -5 -1 601.36 84.93 0 5 2 61.38 6.17 0 5 2 57.32 6.14 0 5 2 46.98 19.13 0 -5 -2 53.66 6.74 0 -5 -2 50.21 18.74 0 5 3 2.51 3.65 0 5 3 2.07 4.42 0 5 3 2.60 4.81 0 -5 -3 4.23 3.47 0 -5 -3 1.05 3.21 0 5 4 824.51 114.74 0 5 4 796.82 114.61 0 -5 -4 826.69 114.83 0 5 5 12.30 5.57 0 5 5 11.12 4.71 0 -5 -5 7.32 4.46 0 5 6 182.27 21.50 0 5 6 151.49 54.67 0 -5 -6 152.17 20.46 0 5 7 158.05 18.58 0 5 7 100.72 43.00 0 5 7 120.70 42.83 0 -5 -7 138.61 15.84 0 5 8 763.96 90.25 0 5 8 536.32 219.45 0 5 8 626.62 219.46 0 -5 -8 725.01 90.08 0 5 9 67.64 13.13 0 5 9 49.84 21.79 0 5 9 67.98 22.31 0 -5 -9 59.93 10.73 0 5 10 468.10 63.48 0 5 10 441.37 155.16 0 5 10 496.20 155.21 0 -5 -10 404.70 63.10 0 5 11 62.30 12.69 0 5 11 63.11 22.92 0 5 11 55.88 22.23 0 -5 -11 34.27 10.86 0 -5 -11 64.84 22.33 0 5 12 113.48 19.20 0 5 12 123.88 44.58 0 5 12 138.06 44.88 0 -5 -12 106.10 18.05 0 -5 -12 145.08 44.99 0 5 13 27.42 13.51 0 5 13 17.91 18.81 0 5 13 17.00 16.29 0 -5 -13 16.43 9.92 0 -5 -13 32.73 17.88 0 5 14 1146.37 82.87 0 5 14 1197.02 369.74 0 5 14 1084.67 369.52 0 -5 -14 804.27 153.17 0 -5 -14 1080.40 369.71 0 5 15 -3.92 12.45 0 5 15 2.88 12.54 0 5 15 6.52 16.16 0 -5 -15 8.84 10.46 0 -5 -15 1.89 16.74 0 5 16 354.31 45.42 0 5 16 311.44 108.16 0 5 16 307.45 108.87 0 -5 -16 280.52 44.63 0 -5 -17 28.52 10.29 0 5 17 31.41 13.99 0 5 17 20.23 16.05 0 5 17 16.10 17.99 0 -5 -17 23.58 12.46 0 6 0 37.15 5.30 0 6 0 44.51 5.36 0 6 0 26.52 15.71 0 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13.73 0 -6 -12 31.58 10.04 0 6 13 131.13 18.83 0 6 13 116.72 42.38 0 -6 -13 111.68 17.28 0 6 14 585.63 84.47 0 6 14 689.11 204.48 0 6 14 612.91 204.32 0 -6 -14 435.51 83.57 0 6 15 61.27 15.39 0 6 15 52.50 22.77 0 6 15 51.89 22.20 0 -6 -15 31.76 10.44 0 6 16 4.27 10.06 0 6 16 0.18 15.68 0 6 16 13.08 16.68 0 -6 -16 8.35 13.64 0 6 17 5.59 13.82 0 6 17 12.55 16.88 0 6 17 21.99 18.48 0 -6 -17 -3.68 13.21 0 7 0 77.30 10.20 0 7 0 78.62 8.97 0 7 0 47.67 25.52 0 -7 0 85.24 9.00 0 -7 0 74.47 9.19 0 -7 0 65.28 25.69 0 7 1 89.53 11.52 0 7 1 95.29 11.12 0 -7 -1 96.31 11.02 0 -7 -1 96.24 11.51 0 -7 -1 84.63 32.53 0 7 2 1556.05 196.47 0 7 2 1602.48 196.51 0 7 2 893.07 470.50 0 -7 -2 1601.38 196.43 0 -7 -2 1500.03 196.50 0 -7 -2 1280.73 470.56 0 7 3 12.13 5.93 0 7 3 9.21 5.15 0 7 3 6.11 10.06 0 -7 -3 11.09 4.70 0 -7 -3 7.42 5.66 0 7 4 21.05 4.39 0 7 4 15.65 3.63 0 7 4 19.28 9.15 0 -7 -4 26.22 4.75 0 -7 -4 23.13 8.53 0 7 5 886.84 114.81 0 7 5 906.88 114.72 0 7 5 622.62 277.58 0 -7 -5 904.72 114.93 0 -7 -5 816.00 277.61 0 7 6 2.91 5.63 0 7 6 0.81 7.50 0 -7 -6 6.16 5.98 0 7 7 13.71 5.45 0 7 7 14.02 6.60 0 -7 -7 16.29 4.70 0 7 8 18.05 10.50 0 -7 -8 12.76 5.62 0 7 9 190.37 24.80 0 7 9 108.76 54.99 0 7 9 155.63 55.12 0 -7 -9 218.79 22.49 0 7 10 372.10 45.14 0 7 10 261.87 109.38 0 7 10 323.40 109.33 0 -7 -10 360.71 44.46 0 7 11 606.33 70.07 0 7 11 394.61 169.62 0 7 11 489.94 169.65 0 -7 -11 568.77 69.73 0 7 12 1.60 11.97 0 7 12 0.35 8.47 0 7 12 0.17 8.39 0 -7 -12 5.69 9.78 0 7 13 30.47 11.47 0 7 13 21.98 13.10 0 7 13 22.48 14.18 0 -7 -13 29.25 9.51 0 7 14 81.11 13.88 0 7 14 67.94 25.76 0 7 14 54.01 26.09 0 -7 -14 80.37 10.26 0 7 15 121.93 18.32 0 7 15 112.81 38.92 0 7 15 100.32 39.00 0 -7 -15 85.92 15.56 0 7 16 152.86 20.70 0 7 16 104.74 40.76 0 7 16 88.22 40.41 0 -7 -16 107.13 18.84 0 -7 -17 101.97 13.63 0 7 17 125.16 18.36 0 7 17 79.13 36.39 0 7 17 76.01 36.05 0 8 0 1379.04 174.35 0 8 0 1366.77 174.05 0 8 0 821.52 417.44 0 -8 0 1324.11 174.00 0 -8 0 1454.51 174.01 0 -8 0 1142.74 417.60 0 8 1 852.28 103.81 0 8 1 836.93 103.77 0 8 1 516.98 251.42 0 -8 -1 842.11 103.74 0 -8 -1 801.54 103.99 0 -8 -1 646.78 251.51 0 8 2 1389.81 170.32 0 8 2 1367.98 170.54 0 8 2 702.26 408.54 0 -8 -2 1433.59 170.31 0 -8 -2 1358.81 170.55 0 -8 -2 1075.99 408.59 0 8 3 4849.54 601.71 0 8 3 4982.50 601.64 0 8 3 2800.22 1427.62 0 -8 -3 4880.17 601.76 0 -8 -3 3869.38 1427.68 0 8 4 406.09 46.84 0 8 4 351.82 46.59 0 8 4 274.79 116.46 0 -8 -4 377.40 46.88 0 -8 -4 318.54 116.27 0 8 5 603.93 80.72 0 8 5 656.35 80.42 0 8 5 409.66 196.26 0 -8 -5 684.93 80.66 0 -8 -5 566.17 196.22 0 8 6 940.46 137.24 0 8 6 1005.75 137.17 0 -8 -6 972.05 137.36 0 8 7 403.78 58.74 0 8 7 481.04 58.89 0 -8 -7 398.73 58.70 0 8 8 2460.31 349.20 0 8 8 2384.15 349.05 0 -8 -8 2477.36 349.29 0 8 9 3265.03 484.23 0 -8 -9 3492.92 484.36 0 8 10 4.13 12.64 0 -8 -10 10.57 9.59 0 8 11 173.11 23.84 0 8 11 118.53 54.64 0 -8 -11 199.71 22.54 0 8 12 80.82 13.44 0 8 12 50.10 22.60 0 8 12 54.02 22.84 0 -8 -12 77.20 11.53 0 8 13 25.87 11.54 0 8 13 9.78 10.79 0 -8 -13 24.51 7.60 0 8 14 477.29 57.87 0 8 14 334.82 140.17 0 -8 -14 477.63 56.93 0 8 15 336.92 41.40 0 8 15 234.62 100.19 0 8 15 298.60 100.32 0 -8 -15 325.86 40.75 0 -8 -16 0.31 8.10 0 8 16 12.18 14.97 0 8 16 0.22 15.80 0 -8 -17 1.20 7.78 0 8 17 0.90 14.16 0 8 17 3.70 21.87 0 8 17 4.34 15.40 0 9 0 339.52 40.37 0 9 0 351.85 39.78 0 9 0 161.21 99.05 0 -9 0 352.63 39.79 0 -9 0 348.05 40.00 0 -9 0 237.39 99.52 0 9 1 273.76 28.77 0 9 1 256.45 28.36 0 9 1 115.29 73.09 0 -9 -1 231.02 28.24 0 -9 -1 249.26 29.15 0 -9 -1 190.19 73.19 0 9 2 19.87 5.78 0 9 2 32.07 14.32 0 -9 -2 13.57 4.87 0 -9 -2 15.35 6.69 0 -9 -2 27.12 14.55 0 9 3 1123.95 157.07 0 9 3 1110.45 156.98 0 -9 -3 1115.99 157.09 0 -9 -3 1086.93 377.41 0 9 4 12.01 5.13 0 9 4 15.76 4.60 0 9 4 3.65 9.73 0 -9 -4 12.71 4.83 0 -9 -4 14.87 10.46 0 9 5 51.78 7.63 0 9 5 43.09 6.56 0 9 5 44.98 19.87 0 -9 -5 74.81 7.75 0 9 6 574.90 83.01 0 9 6 619.19 83.03 0 -9 -6 590.40 83.18 0 9 7 8.26 8.60 0 9 7 10.23 10.65 0 -9 -7 7.07 8.26 0 9 8 106.39 15.47 0 9 8 104.39 13.82 0 -9 -8 106.41 16.31 0 9 9 17.91 9.93 0 9 9 28.05 12.14 0 -9 -9 18.93 8.93 0 9 10 229.97 32.18 0 9 10 218.89 32.56 0 -9 -10 245.65 32.17 0 9 11 10.22 7.88 0 9 11 8.54 12.99 0 -9 -11 14.51 10.14 0 9 12 530.11 76.02 0 -9 -12 547.47 75.75 0 9 13 94.98 16.19 0 -9 -13 100.35 15.04 0 9 14 13.15 11.25 0 -9 -14 8.13 9.40 0 9 15 172.78 23.92 0 9 15 89.25 51.61 0 -9 -15 209.73 22.93 0 9 16 96.31 17.66 0 9 16 38.15 24.87 0 9 16 37.53 25.90 0 -9 -16 96.65 13.77 0 9 17 59.42 12.61 0 -9 -17 53.43 12.84 0 10 0 190.79 52.14 0 10 0 396.75 53.18 0 10 0 715.14 130.60 0 -10 0 368.39 53.29 0 -10 0 188.76 51.97 0 -10 0 297.27 129.06 0 10 1 266.44 36.41 0 10 1 323.49 37.59 0 10 1 131.68 91.90 0 -10 -1 369.46 38.51 0 -10 -1 275.80 36.90 0 -10 -1 254.34 92.01 0 10 2 68.45 12.51 0 10 2 88.63 14.32 0 10 2 71.83 33.64 0 -10 -2 178.98 16.49 0 -10 -2 77.55 14.06 0 -10 -2 67.97 32.82 0 10 3 1101.28 133.42 0 10 3 1208.44 133.81 0 10 3 442.69 321.09 0 -10 -3 1109.69 133.72 0 -10 -3 986.59 321.32 0 10 4 409.81 60.81 0 10 4 469.57 60.91 0 -10 -4 439.42 60.96 0 10 5 435.22 39.00 0 10 5 462.16 39.06 0 10 5 139.87 95.74 0 -10 -5 198.97 38.04 0 -10 -5 225.62 95.71 0 10 6 581.39 47.82 0 10 6 662.27 47.85 0 10 6 122.28 116.04 0 10 7 200.79 27.33 0 10 7 205.32 27.59 0 -10 -7 196.01 27.83 0 10 8 185.79 27.01 0 10 8 171.26 27.05 0 -10 -8 208.56 26.26 0 10 9 1146.57 168.70 0 10 9 1215.92 168.59 0 -10 -9 1200.84 168.63 0 10 10 505.89 72.09 0 10 10 499.44 72.23 0 -10 -10 537.43 72.18 0 10 11 93.66 14.75 0 10 11 90.34 18.92 0 -10 -11 95.69 14.50 0 10 12 13.41 9.36 0 10 12 31.40 13.04 0 -10 -12 20.89 9.37 0 10 13 25.80 9.90 0 10 13 31.31 12.29 0 -10 -13 39.93 9.80 0 10 14 32.33 11.73 0 -10 -14 43.13 11.21 0 10 15 382.69 65.89 0 -10 -15 540.40 67.57 0 10 16 117.69 22.05 0 -10 -16 133.58 25.17 0 11 0 68.71 11.86 0 11 0 70.94 13.53 0 11 0 44.26 33.22 0 -11 0 55.69 15.64 0 -11 0 69.33 13.04 0 -11 0 63.23 26.03 0 11 1 65.47 15.71 0 11 1 78.72 12.70 0 11 1 48.40 31.70 0 -11 -1 81.43 13.01 0 -11 -1 68.28 12.54 0 -11 -1 62.93 28.42 0 11 2 142.67 18.00 0 11 2 156.93 18.61 0 11 2 85.36 50.36 0 -11 -2 168.82 20.24 0 -11 -2 160.81 20.30 0 -11 -2 93.67 46.71 0 11 3 786.51 90.16 0 11 3 869.80 90.30 0 11 3 350.43 218.66 0 -11 -3 773.19 90.38 0 -11 -3 553.80 218.53 0 11 4 493.26 60.26 0 11 4 567.71 60.89 0 11 4 217.94 147.48 0 -11 -4 526.71 60.14 0 -11 -4 421.52 147.52 0 11 5 110.82 15.74 0 11 5 117.14 15.01 0 -11 -5 135.43 16.09 0 -11 -5 77.10 37.50 0 11 6 539.12 73.83 0 11 6 450.46 73.32 0 -11 -6 581.70 74.14 0 11 7 777.38 111.19 0 11 7 807.25 110.89 0 -11 -7 778.01 111.07 0 11 8 123.19 16.44 0 11 8 110.71 16.85 0 -11 -8 100.80 16.03 0 11 9 57.30 12.86 0 11 9 39.23 14.27 0 -11 -9 56.03 14.51 0 11 10 35.25 13.29 0 11 10 32.02 16.36 0 -11 -10 35.17 12.86 0 11 11 12.48 13.21 0 11 11 7.58 15.33 0 -11 -11 10.83 15.25 0 11 12 728.18 83.23 0 11 12 518.52 82.42 0 -11 -12 492.84 82.60 0 11 13 197.61 30.09 0 11 13 252.97 31.67 0 -11 -13 152.89 29.26 0 11 14 -5.53 12.44 0 11 14 11.86 11.76 0 -11 -14 13.58 13.99 0 11 15 53.17 14.25 0 11 15 48.97 14.32 0 -11 -15 68.10 15.46 0 11 16 17.39 12.59 0 11 16 13.01 12.48 0 -11 -16 19.03 14.00 0 12 0 229.37 31.07 0 12 0 121.38 72.76 0 -12 0 244.30 29.85 0 -12 0 232.01 32.86 0 -12 0 218.71 72.62 0 12 1 2892.92 413.29 0 12 1 3100.87 413.42 0 -12 -1 3127.73 413.36 0 -12 -1 2963.36 413.23 0 -12 -1 2434.03 981.94 0 12 2 1187.68 152.76 0 12 2 1279.70 152.80 0 12 2 572.16 365.75 0 -12 -2 1385.50 152.76 0 -12 -2 1298.14 152.86 0 -12 -2 923.81 365.89 0 12 3 906.62 103.54 0 12 3 407.35 250.21 0 -12 -3 937.38 104.04 0 -12 -3 783.89 250.09 0 12 4 2928.23 335.58 0 12 4 1424.72 798.06 0 -12 -4 2965.41 335.60 0 -12 -4 2370.80 798.23 0 12 5 940.81 108.22 0 12 5 1013.90 108.02 0 12 5 468.00 260.29 0 -12 -5 958.28 107.98 0 -12 -5 614.32 260.11 0 12 6 1026.39 107.12 0 12 6 1023.38 106.96 0 12 6 392.53 257.41 0 -12 -6 1058.82 107.57 0 -12 -6 526.31 257.42 0 12 7 2975.36 421.74 0 12 7 2835.11 421.31 0 -12 -7 3006.05 421.65 0 12 8 1069.31 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247.45 80.76 -10 -4 -8 237.34 32.47 -10 -4 -8 210.91 80.11 10 4 9 1566.31 226.84 10 4 9 1871.14 227.24 10 4 9 1276.56 540.77 -10 -4 -9 1668.54 226.73 -10 -4 -9 1611.83 540.97 10 4 10 248.39 38.38 10 4 10 322.66 39.27 10 4 10 221.85 93.73 -10 -4 -10 239.61 38.48 -10 -4 -10 319.67 94.31 10 4 11 23.76 13.67 10 4 11 15.66 19.63 -10 -4 -11 41.59 12.01 -10 -4 -11 40.78 23.10 10 5 2 51.88 16.17 10 5 2 71.87 16.33 -10 -5 -2 60.31 15.72 -10 -5 -2 50.87 15.89 -10 -5 -2 58.39 29.94 -10 -5 -2 66.77 26.73 10 5 3 305.62 41.82 10 5 3 264.28 40.01 -10 -5 -3 263.78 40.39 -10 -5 -3 292.75 41.31 -10 -5 -3 246.51 96.11 -10 -5 -3 290.90 96.26 10 5 4 32.39 12.11 10 5 4 38.63 11.10 -10 -5 -4 26.87 9.74 -10 -5 -4 42.52 13.21 -10 -5 -4 43.45 22.73 -10 -5 -4 49.67 24.20 10 5 5 55.67 13.54 10 5 5 53.34 14.69 -10 -5 -5 68.39 16.06 -10 -5 -5 50.25 27.36 -10 -5 -5 72.21 30.18 10 5 6 34.82 13.59 10 5 6 31.11 10.88 10 5 6 27.71 18.20 -10 -5 -6 36.61 16.34 -10 -5 -6 38.23 19.59 -10 -5 -6 30.41 20.82 10 5 7 32.36 10.61 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258.96 35.22 10 6 7 240.87 35.31 -10 -6 -7 289.34 34.76 -10 -6 -7 177.27 84.13 -10 -6 -7 256.05 84.55 10 6 8 141.98 20.65 10 6 8 135.80 18.69 10 6 8 117.70 46.09 -10 -6 -8 131.67 19.05 -10 -6 -8 109.33 46.50 -10 -6 -8 129.19 46.25 10 6 9 453.07 66.48 10 6 9 588.50 67.39 10 6 9 433.77 161.99 -10 -6 -9 440.30 66.48 -10 -6 -9 411.42 162.07 -10 -6 -9 505.09 162.57 10 6 10 996.62 159.70 10 6 10 1208.28 383.16 -10 -6 -10 899.33 159.34 -10 -6 -10 1143.52 383.14 -10 -6 -10 1287.98 383.03 10 6 11 51.11 15.74 10 6 11 65.84 16.06 10 6 11 76.53 31.35 -10 -6 -11 40.61 15.51 -10 -6 -11 112.38 30.10 10 7 5 112.77 22.13 10 7 5 121.78 18.94 -10 -7 -5 73.91 17.45 -10 -7 -5 137.35 21.93 -10 -7 -5 96.87 44.12 -10 -7 -5 133.16 45.15 10 7 6 93.83 16.27 10 7 6 77.29 14.72 -10 -7 -6 94.16 16.65 -10 -7 -6 72.39 36.77 -10 -7 -6 92.38 35.43 10 7 7 32.83 10.00 10 7 7 28.02 10.62 -10 -7 -7 48.54 11.56 -10 -7 -7 27.92 21.93 -10 -7 -7 23.87 18.79 10 7 8 42.76 10.74 10 7 8 43.11 9.85 -10 -7 -8 53.77 9.99 -10 -7 -8 35.31 23.95 -10 -7 -8 45.30 21.15 10 7 9 98.09 14.98 10 7 9 99.30 15.63 -10 -7 -9 93.07 14.02 -10 -7 -9 76.11 38.28 -10 -7 -9 84.43 34.65 10 7 10 48.01 10.73 10 7 10 110.16 15.83 -10 -7 -10 39.71 10.97 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 13438