data_final _audit_creation_date 2022-01-21 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'Bi4 Br1.71 O4 Se0.29, 0.71(Se), 0.29(Br)' _chemical_formula_sum 'Bi4 Br2 O4 Se' _chemical_formula_weight 1138.70 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Bi' 'Bi' -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'tetragonal' _space_group_IT_number 139 _space_group_name_H-M_alt 'I 4/m m m' _space_group_name_Hall '-I 4 2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 3.9281(4) _cell_length_b 3.9281(4) _cell_length_c 28.190(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 434.97(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 990 _cell_measurement_temperature 150.0 _cell_measurement_theta_max 26.314 _cell_measurement_theta_min 2.890 _shelx_estimated_absorpt_T_max 0.453 _shelx_estimated_absorpt_T_min 0.089 _exptl_absorpt_coefficient_mu 94.001 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.2706 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1955 before and 0.0796 after correction. The Ratio of minimum to maximum transmission is 0.3630. The \l/2 correction factor is Not present. ; _exptl_absorpt_special_details ? _exptl_crystal_colour black _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 8.694 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 936 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.01 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_unetI/netI 0.0327 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.989 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_h_min -4 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_number 1578 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.314 _diffrn_reflns_theta_min 2.890 _diffrn_ambient_temperature 150.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.989 _diffrn_measurement_device_type 'Bruker Venture Apex' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 160 _reflns_number_total 175 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _refine_diff_density_max 3.731 _refine_diff_density_min -4.788 _refine_diff_density_rms 0.925 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_hydrogen_treatment undef _refine_ls_matrix_type full _refine_ls_number_parameters 14 _refine_ls_number_reflns 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0605 _refine_ls_R_factor_gt 0.0565 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1117P)^2^+54.0367P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1621 _refine_ls_wR_factor_ref 0.1669 _refine_special_details ? _olex2_refinement_description ; 1. Shared sites {Se04, Br04} {Se03, Br03} 2. Uiso/Uaniso restraints and constraints Uanis(Se03) = Uanis(Br03) Uanis(Se04) = Uanis(Br04) 3. Others Fixed Sof: Se03(0.04438) Se04(0.01813) Br04(0.10688) Br03(0.01813) ; _atom_sites_solution_hydrogens . _atom_sites_solution_primary dual _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi01 Bi 1.000000 1.000000 0.56768(6) 0.0090(9) Uani 1 8 d S T P . . Bi02 Bi 0.500000 0.500000 0.65595(8) 0.0189(9) Uani 1 8 d S T P . . Se03 Se 0.500000 0.500000 0.500000 0.0079(14) Uani 0.7101 16 d S T P . . Se04 Se 0.000000 0.000000 0.70681(15) 0.0063(13) Uani 0.145 8 d S T P . . O005 O 0.500000 1.000000 0.6082(7) 0.003(4) Uiso 1 4 d S . P . . Br04 Br 0.000000 0.000000 0.70681(15) 0.0063(13) Uani 0.855 8 d S T P . . Br03 Br 0.500000 0.500000 0.500000 0.0079(14) Uani 0.2901 16 d S T 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 Bi01 0.0095(10) 0.0095(10) 0.0081(14) 0.000 0.000 0.000 Bi02 0.0182(10) 0.0182(10) 0.0205(16) 0.000 0.000 0.000 Se03 0.008(2) 0.008(2) 0.007(3) 0.000 0.000 0.000 Se04 0.0076(17) 0.0076(17) 0.004(3) 0.000 0.000 0.000 Br04 0.0076(17) 0.0076(17) 0.004(3) 0.000 0.000 0.000 Br03 0.008(2) 0.008(2) 0.007(3) 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 Bi01 O005 2.273(10) . ? Bi01 O005 2.273(10) 3_765 ? Bi01 O005 2.273(10) 1_655 ? Bi01 O005 2.273(10) 3_755 ? Bi02 Se04 3.126(2) 1_565 ? Bi02 Se04 3.126(2) 1_655 ? Bi02 Se04 3.126(2) 1_665 ? Bi02 Se04 3.126(2) . ? Bi02 O005 2.380(12) 3_655 ? Bi02 O005 2.380(12) 3_755 ? Bi02 O005 2.380(12) 1_545 ? Bi02 O005 2.380(12) . ? 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 O005 Bi01 O005 75.3(4) . 3_765 ? O005 Bi01 O005 75.3(4) 3_765 1_655 ? O005 Bi01 O005 119.6(9) . 1_655 ? O005 Bi01 O005 119.6(9) 3_765 3_755 ? O005 Bi01 O005 75.3(4) . 3_755 ? O005 Bi01 O005 75.3(4) 1_655 3_755 ? Se04 Bi02 Se04 77.85(7) 1_665 1_655 ? Se04 Bi02 Se04 125.39(17) 1_665 . ? Se04 Bi02 Se04 125.39(17) 1_565 1_655 ? Se04 Bi02 Se04 77.85(7) . 1_565 ? Se04 Bi02 Se04 77.85(7) 1_665 1_565 ? Se04 Bi02 Se04 77.85(7) . 1_655 ? O005 Bi02 Se04 141.04(3) 3_755 . ? O005 Bi02 Se04 75.0(3) 1_545 1_655 ? O005 Bi02 Se04 75.0(3) 3_655 . ? O005 Bi02 Se04 141.04(3) 1_545 1_565 ? O005 Bi02 Se04 75.0(3) . 1_565 ? O005 Bi02 Se04 75.0(3) 1_545 . ? O005 Bi02 Se04 75.0(3) 3_655 1_565 ? O005 Bi02 Se04 141.04(4) 1_545 1_665 ? O005 Bi02 Se04 141.04(4) 3_755 1_565 ? O005 Bi02 Se04 75.0(3) 3_755 1_655 ? O005 Bi02 Se04 75.0(3) . 1_665 ? O005 Bi02 Se04 75.0(3) 3_755 1_665 ? O005 Bi02 Se04 141.04(3) . . ? O005 Bi02 Se04 141.04(4) 3_655 1_665 ? O005 Bi02 Se04 141.04(3) 3_655 1_655 ? O005 Bi02 Se04 141.04(4) . 1_655 ? O005 Bi02 O005 71.4(4) 3_655 . ? O005 Bi02 O005 71.4(4) 3_755 . ? O005 Bi02 O005 111.2(8) 1_545 . ? O005 Bi02 O005 71.4(4) 1_545 3_755 ? O005 Bi02 O005 71.4(4) 3_655 1_545 ? O005 Bi02 O005 111.2(8) 3_655 3_755 ? Bi02 Se04 Bi02 77.85(7) 1_445 1_545 ? Bi02 Se04 Bi02 125.40(17) 1_455 1_545 ? Bi02 Se04 Bi02 77.85(7) 1_445 1_455 ? Bi02 Se04 Bi02 125.39(17) 1_445 . ? Bi02 Se04 Bi02 77.85(7) 1_455 . ? Bi02 Se04 Bi02 77.85(7) 1_545 . ? Bi01 O005 Bi01 119.6(9) 1_455 . ? Bi01 O005 Bi02 106.52(6) 1_455 . ? Bi01 O005 Bi02 106.52(6) . . ? Bi01 O005 Bi02 106.52(6) 1_455 1_565 ? Bi01 O005 Bi02 106.52(6) . 1_565 ? Bi02 O005 Bi02 111.2(8) . 1_565 ? _shelx_res_file ; TITL final_a.res in I4/mmm final.res created by SHELXL-2018/3 at 14:25:24 on 21-Jan-2022 REM Old TITL final in I4/mmm REM SHELXT solution in I4/mmm: R1 0.064, Rweak 0.005, Alpha 0.012 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: O4 Br3 Bi4 CELL 0.71073 3.9281 3.9281 28.1901 90 90 90 ZERR 2 0.0004 0.0004 0.0029 0 0 0 LATT 2 SYMM -X,-Y,+Z SYMM -Y,+X,+Z SYMM +Y,-X,+Z SYMM -X,+Y,-Z SYMM +X,-Y,-Z SYMM +Y,+X,-Z SYMM -Y,-X,-Z SFAC Bi Br O Se UNIT 8 4 8 2 EADP Se03 Br03 EADP Se04 Br04 EXYZ Se04 Br04 EXYZ Se03 Br03 L.S. 25 PLAN 5 SIZE 0.05 0.04 0.01 TEMP -123.15 CONF list 4 MORE -1 fmap 2 ACTA REM REM REM WGHT 0.111700 54.036701 FVAR 0.15647 BI01 1 1.000000 1.000000 0.567678 10.12500 0.00947 0.00947 = 0.00811 0.00000 0.00000 0.00000 BI02 1 0.500000 0.500000 0.655947 10.12500 0.01818 0.01818 = 0.02048 0.00000 0.00000 0.00000 SE03 4 0.500000 0.500000 0.500000 10.04438 0.00834 0.00834 = 0.00702 0.00000 0.00000 0.00000 SE04 4 0.000000 0.000000 0.706809 10.01813 0.00759 0.00759 = 0.00369 0.00000 0.00000 0.00000 O005 3 0.500000 1.000000 0.608246 10.25000 0.00328 BR04 2 0.000000 0.000000 0.706809 10.10688 0.00759 0.00759 = 0.00369 0.00000 0.00000 0.00000 BR03 2 0.500000 0.500000 0.500000 10.01813 0.00834 0.00834 = 0.00702 0.00000 0.00000 0.00000 HKLF 4 REM final_a.res in I4/mmm REM wR2 = 0.1669, GooF = S = 1.161, Restrained GooF = 1.161 for all data REM R1 = 0.0565 for 160 Fo > 4sig(Fo) and 0.0605 for all 175 data REM 14 parameters refined using 0 restraints END WGHT 0.1117 54.0303 REM Highest difference peak 3.731, deepest hole -4.788, 1-sigma level 0.925 Q1 1 0.5000 0.6174 0.6804 10.50000 0.05 3.73 Q2 1 1.0000 1.0000 0.5000 10.06250 0.05 3.58 Q3 1 0.5000 0.5000 0.6885 10.12500 0.05 2.75 Q4 1 1.0000 1.0000 0.5843 10.12500 0.05 2.57 Q5 1 0.5000 0.2008 0.5000 10.25000 0.05 1.95 ; _shelx_res_checksum 5088 _shelx_hkl_file ; -1 1 0 9999.00 596.14 -1 1 0 9765.12 597.94 1 -1 0 9671.83 599.54 0 2 0 9816.12 562.34 0 -2 0 9662.83 562.34 -2 0 0 8220.38 562.14 -2 2 0 7039.20 432.06 -2 2 0 7541.15 429.66 -2 -2 0 6390.86 430.16 2 -2 0 7332.67 441.26 2 2 0 6920.41 429.36 -1 3 0 5231.78 315.37 1 -3 0 5177.08 320.47 -3 1 0 5087.89 313.07 -3 1 0 5177.48 319.67 -1 -3 0 5016.60 315.47 1 3 0 5055.99 315.27 3 -1 0 5039.00 322.57 -3 -1 0 5326.67 326.27 3 3 0 2602.04 169.28 3 -3 0 2338.47 188.88 3 3 0 2719.63 159.18 -4 0 0 3516.25 228.58 -4 0 0 3133.09 242.38 0 4 0 4015.80 227.28 0 -4 0 3897.01 233.78 2 4 0 3037.80 186.28 2 -4 0 3008.90 200.68 -4 2 0 2958.90 184.18 4 -2 0 3115.59 200.38 -4 -2 0 2663.33 202.88 -2 4 0 3062.49 186.78 -4 2 0 3005.80 188.28 0 1 1 143.49 10.60 -1 0 1 172.58 13.80 0 1 -1 149.99 10.60 0 -1 1 147.29 10.50 1 0 1 174.58 14.10 0 -1 -1 140.39 10.50 -1 0 -1 190.18 16.00 -1 0 -1 160.08 10.10 1 2 -1 110.29 9.70 -1 -2 -1 121.09 9.90 1 -2 1 123.09 13.60 2 1 1 100.79 12.00 -1 2 1 123.59 9.90 2 -1 -1 95.09 18.90 1 -2 1 114.59 9.30 -2 -1 1 114.49 8.90 -2 1 -1 121.89 8.60 -2 1 -1 140.89 14.00 2 1 1 120.39 8.40 -2 1 1 137.69 12.20 -1 2 -1 118.79 9.90 1 -2 -1 127.29 13.10 -1 -2 1 115.59 9.70 -2 1 1 115.59 8.30 -2 -1 -1 118.29 9.00 1 2 1 125.19 10.00 0 -3 1 104.79 10.20 -3 0 -1 58.19 23.10 -3 0 1 84.79 13.70 0 -3 -1 94.19 13.90 0 3 -1 95.09 10.20 0 3 1 103.79 10.50 -3 0 -1 74.29 12.90 0 -3 1 102.19 13.80 3 -2 -1 39.70 27.50 -3 2 -1 86.79 9.70 2 3 -1 93.09 10.50 2 -3 1 92.89 21.00 -3 2 -1 74.79 12.70 -2 3 1 83.19 11.10 2 -3 -1 109.49 21.00 3 -2 1 27.50 26.80 -3 2 1 93.69 17.60 -2 3 -1 93.29 11.00 2 3 1 90.39 10.40 -2 -3 1 73.69 10.80 -3 2 1 91.99 9.30 -4 1 -1 74.09 10.40 1 -4 1 60.49 17.40 -1 4 1 69.29 11.00 1 4 -1 71.19 10.70 -4 -1 1 2.00 32.10 -4 1 -1 94.39 19.00 -4 1 1 72.29 10.80 1 4 1 63.39 10.90 1 -4 -1 78.59 19.40 -4 -1 -1 151.28 37.00 -1 -4 1 50.29 13.10 -1 4 -1 86.29 13.00 -4 1 1 69.89 15.90 -1 1 2 13.20 2.00 1 -1 -2 20.10 4.40 1 -1 2 14.80 2.10 -1 1 -2 15.30 2.50 -1 -1 2 15.90 2.50 -1 1 2 16.50 3.10 -1 1 -2 22.80 5.00 1 1 2 17.90 2.70 1 -1 2 18.70 6.30 1 1 -2 15.80 2.50 0 2 -2 43.90 5.30 0 -2 2 45.50 7.60 -2 0 -2 55.79 7.00 -2 0 -2 40.20 13.90 -2 0 2 56.69 13.00 0 2 2 42.00 5.80 2 0 2 61.49 11.90 0 -2 2 47.00 5.30 2 2 2 40.80 6.00 -2 2 -2 51.89 9.40 2 -2 -2 48.20 14.90 2 -2 2 39.80 16.50 -2 2 -2 40.50 6.20 2 2 -2 43.30 5.80 -2 2 2 36.70 6.00 -3 1 -2 23.70 4.20 1 -3 2 34.90 10.00 3 -1 -2 31.40 10.60 -3 1 -2 29.60 12.10 -1 3 2 9.10 4.70 1 3 -2 23.60 5.30 -1 3 -2 23.10 5.30 -1 -3 2 14.00 4.60 3 -1 2 15.20 14.20 1 3 2 20.80 5.50 -3 1 2 28.30 7.60 1 -3 -2 19.90 8.60 -3 -1 -2 33.20 15.20 -3 1 2 25.60 3.80 -3 3 -2 17.90 7.30 3 3 2 22.70 5.90 -3 3 2 27.10 7.60 3 3 2 47.20 20.60 3 -3 -2 -39.40 35.90 3 3 -2 27.80 6.20 0 -4 2 47.80 14.20 -4 0 -2 10.90 28.80 0 4 2 24.10 7.70 -4 0 2 2.10 22.20 0 -4 -2 38.70 13.60 0 4 -2 30.90 7.90 -4 0 -2 35.70 16.20 -4 0 2 53.39 10.90 -4 2 -2 23.50 7.80 2 -4 2 49.00 23.60 -2 4 2 29.10 9.10 2 4 -2 25.60 8.40 4 -2 -2 19.20 20.10 -4 2 -2 29.20 13.40 -4 -2 2 41.70 28.30 2 -4 -2 39.20 23.40 -4 -2 -2 7.70 28.40 4 -2 2 74.39 33.10 2 4 2 26.50 8.30 -4 2 2 16.70 6.40 -2 4 -2 15.20 8.90 -4 2 2 22.50 9.90 -1 0 -3 1036.00 76.49 0 1 -3 1107.99 70.49 0 -1 3 1138.09 70.59 0 -1 3 1082.09 71.79 1 0 3 1141.49 75.89 1 0 3 1193.68 70.19 -1 0 3 1305.17 71.99 -1 0 -3 1126.49 71.29 -2 1 -3 676.73 42.80 1 -2 3 705.23 48.20 -2 -1 3 669.03 42.70 -1 2 3 672.83 43.60 1 2 -3 672.73 43.60 1 -2 3 650.33 43.30 -2 1 -3 733.63 50.39 2 1 3 660.33 42.40 1 -2 -3 653.03 46.20 -2 -1 -3 753.82 50.29 -1 2 -3 682.03 46.40 -1 2 -3 661.93 43.60 -1 -2 3 669.83 43.70 1 2 3 673.03 43.80 -2 1 3 699.03 44.20 0 3 3 397.06 28.80 0 3 -3 408.36 28.60 0 -3 3 403.16 28.50 0 -3 3 429.26 33.10 -3 -2 3 258.87 19.80 2 3 -3 274.07 20.30 -3 2 -3 280.67 19.90 2 -3 3 315.17 36.80 3 2 3 239.18 28.00 3 2 3 259.97 18.10 3 -2 -3 184.88 36.00 -3 2 -3 271.87 25.10 -2 3 3 262.47 20.70 2 -3 -3 268.57 32.70 -2 -3 3 248.58 20.50 -3 -2 -3 290.97 33.50 -3 2 3 276.57 19.10 2 3 3 241.48 20.20 -2 3 -3 301.67 21.50 -3 2 3 268.37 21.20 3 -2 3 169.58 42.80 1 -4 3 182.18 27.40 1 4 -3 169.48 17.90 -1 4 3 157.18 17.90 -4 1 -3 192.78 31.70 -4 1 -3 162.28 20.30 -4 -1 3 165.18 43.00 4 -1 3 205.18 33.70 -4 -1 -3 210.58 46.60 -1 -4 3 165.08 23.70 1 4 3 166.78 17.80 1 -4 -3 186.48 28.30 -1 4 -3 163.38 18.10 -4 1 3 203.78 20.20 0 0 4 442.46 30.90 0 0 -4 401.16 30.80 0 0 -4 436.76 30.70 0 0 4 497.45 30.30 1 1 -4 107.49 8.10 1 1 4 110.19 8.30 1 -1 4 110.79 8.00 1 -1 4 110.19 13.90 -1 1 -4 109.69 11.90 -1 -1 4 110.29 8.10 1 -1 -4 117.59 9.50 -1 1 -4 111.99 8.30 0 2 -4 406.76 27.40 -2 0 4 360.66 32.90 0 -2 4 406.46 30.00 0 -2 4 414.06 27.50 -2 0 -4 382.96 39.40 -2 0 -4 414.66 29.90 2 0 4 498.65 36.30 0 2 4 420.76 27.70 2 -2 4 268.27 32.80 -2 2 -4 255.77 18.60 -2 2 -4 251.67 22.80 2 2 4 285.27 24.50 2 2 -4 256.07 18.00 2 -2 -4 269.37 28.50 2 2 4 248.98 18.30 -2 2 4 244.98 18.00 -3 1 -4 59.09 16.70 1 -3 4 58.99 12.70 3 -1 -4 65.89 13.10 -3 1 -4 69.09 8.50 -1 3 4 61.19 9.30 1 -3 4 63.49 8.30 -3 -1 4 66.49 6.50 -3 -1 4 89.39 18.30 1 3 -4 59.29 8.60 -3 1 4 64.09 9.00 -1 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22.50 21.40 0 -1 -31 23.60 22.10 -1 0 31 25.40 23.30 0 -1 31 15.10 25.90 0 1 -31 38.40 18.70 1 0 31 -19.10 27.90 -2 -1 31 14.30 25.30 -2 1 -31 44.60 26.30 1 -2 31 -16.00 31.10 1 2 -31 15.00 21.30 2 -1 31 33.50 36.70 -1 -2 31 25.30 30.40 -1 2 -31 11.60 25.60 1 -1 -32 690.13 66.79 -1 1 -32 642.44 60.69 -1 -1 32 660.23 65.59 1 1 -32 641.14 65.59 1 -1 32 732.43 76.99 0 -2 -32 280.87 55.49 0 -2 32 339.37 59.49 -2 0 -32 426.66 54.19 2 0 32 505.25 78.89 0 2 -32 305.87 48.40 1 0 33 5.80 32.50 1 0 -33 89.99 22.70 0 1 -33 44.20 21.90 0 -1 33 79.89 32.90 -1 0 33 90.89 30.20 0 0 34 9.20 29.70 0 0 -34 23.70 23.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 56097 _olex2_submission_special_instructions 'No special instructions were received'