data_exp_1123_u _audit_creation_date 2019-02-21 _audit_creation_method ; Olex2 1.2 (compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506) ; _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 '0.25(C48 H16 Cl16 O40 U4), 4(H2 O)' _chemical_formula_sum 'C12 H12 Cl4 O14 U' _chemical_formula_weight 760.05 _chemical_melting_point ? _chemical_oxdiff_formula 'U Cl2 C6 H6 O2' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'U' 'U' -9.6767 9.6646 '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 'monoclinic' _space_group_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.8598(7) _cell_length_b 11.4960(6) _cell_length_c 12.6100(6) _cell_angle_alpha 90 _cell_angle_beta 96.415(5) _cell_angle_gamma 90 _cell_volume 1996.60(17) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3646 _cell_measurement_temperature 285(13) _cell_measurement_theta_max 29.3660 _cell_measurement_theta_min 3.5550 _shelx_estimated_absorpt_T_max 0.669 _shelx_estimated_absorpt_T_min 0.335 _exptl_absorpt_coefficient_mu 8.737 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.67542 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear dark violet' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary violet _exptl_crystal_density_diffrn 2.528 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1424 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.850 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 5341 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.850 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.733 _diffrn_reflns_theta_min 2.917 _diffrn_ambient_environment air _diffrn_ambient_temperature 285(13) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.3073 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.850 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -19.00 12.00 1.00 45.92 -- -11.73 -99.00-180.00 31 2 \w -27.00 49.00 1.00 45.92 -- -11.73 77.00 -90.00 76 3 \w -64.00 29.00 1.00 45.92 -- -11.73 -19.00 -60.00 93 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0192534000 _diffrn_orient_matrix_UB_12 0.0089164000 _diffrn_orient_matrix_UB_13 -0.0491620000 _diffrn_orient_matrix_UB_21 -0.0369684000 _diffrn_orient_matrix_UB_22 0.0413442000 _diffrn_orient_matrix_UB_23 -0.0151469000 _diffrn_orient_matrix_UB_31 0.0302937000 _diffrn_orient_matrix_UB_32 0.0448580000 _diffrn_orient_matrix_UB_33 0.0236649000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2312 _reflns_number_total 2422 _reflns_odcompleteness_completeness 99.77 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _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 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.126 _refine_diff_density_min -0.826 _refine_diff_density_rms 0.115 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 148 _refine_ls_number_reflns 2422 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0221 _refine_ls_R_factor_gt 0.0200 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0203P)^2^+0.2945P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.0445 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All O(H,H) groups 2.a Free rotating group: O6(H6A,H6B), O7(H7A,H7B) 2.b Rotating group: O5(H5A,H5B) ; _atom_sites_solution_hydrogens difmap _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 U1 U 0.500000 0.23650(2) 0.750000 0.01826(6) Uani 1 2 d S T P . . Cl1 Cl 0.30020(6) 0.39562(9) 1.05923(6) 0.0419(2) Uani 1 1 d . . . . . Cl2 Cl 0.39804(7) 0.26515(9) 0.32523(8) 0.0461(2) Uani 1 1 d . . . . . O1 O 0.40997(14) 0.33430(18) 0.87511(15) 0.0258(4) Uani 1 1 d . . . . . O4 O 0.17963(16) 0.2836(2) 0.29620(16) 0.0296(5) Uani 1 1 d . . . . . O2 O 0.42355(14) 0.58455(18) 1.16916(15) 0.0258(4) Uani 1 1 d . . . . . O3 O 0.43768(15) 0.2019(2) 0.56062(16) 0.0313(5) Uani 1 1 d . . . . . O5 O 0.42948(16) 0.0660(2) 0.82631(18) 0.0387(6) Uani 1 1 d . . . . . H5A H 0.473904 0.013269 0.842816 0.058 Uiso 1 1 d GR . . . . H5B H 0.389102 0.031672 0.778310 0.058 Uiso 1 1 d GR . . . . O6 O 0.2313(2) 0.4655(3) 0.7807(3) 0.0576(7) Uani 1 1 d . . . . . H6A H 0.216326 0.393728 0.780209 0.086 Uiso 1 1 d G . . . . H6B H 0.287029 0.473446 0.759493 0.086 Uiso 1 1 d G . . . . C3 C 0.3512(2) 0.2277(2) 0.5252(2) 0.0241(6) Uani 1 1 d . . . . . C4 C 0.2188(2) 0.2715(2) 0.3902(2) 0.0234(6) Uani 1 1 d . . . . . C6 C 0.3179(2) 0.2557(3) 0.4203(3) 0.0276(7) Uani 1 1 d . . . . . C2 C 0.4552(2) 0.5390(3) 1.0897(2) 0.0224(6) Uani 1 1 d . . . . . O7 O 0.4315(2) 0.0790(3) 1.0782(3) 0.0757(10) Uani 1 1 d . . . . . H7A H 0.369783 0.078896 1.072594 0.114 Uiso 1 1 d G . . . . H7B H 0.451341 0.143536 1.055828 0.114 Uiso 1 1 d G . . . . C1 C 0.4478(2) 0.4116(3) 0.9382(2) 0.0232(6) Uani 1 1 d . . . . . C5 C 0.4083(2) 0.4523(3) 1.0266(2) 0.0250(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 U1 0.01550(8) 0.02347(9) 0.01454(8) 0.000 -0.00400(6) 0.000 Cl1 0.0307(4) 0.0585(6) 0.0382(4) -0.0142(4) 0.0119(4) -0.0189(4) Cl2 0.0300(5) 0.0802(7) 0.0285(4) -0.0024(4) 0.0050(4) -0.0052(4) O1 0.0217(10) 0.0319(11) 0.0230(10) -0.0081(9) -0.0011(8) -0.0046(9) O4 0.0266(11) 0.0414(13) 0.0188(10) 0.0048(9) -0.0064(9) -0.0052(10) O2 0.0248(11) 0.0327(11) 0.0202(10) -0.0067(9) 0.0039(9) -0.0028(9) O3 0.0214(11) 0.0439(13) 0.0265(11) -0.0100(11) -0.0069(9) 0.0063(10) O5 0.0295(13) 0.0339(13) 0.0489(14) 0.0084(11) -0.0129(11) -0.0075(10) O6 0.0457(17) 0.0594(19) 0.0663(18) 0.0061(16) 0.0004(15) 0.0148(14) C3 0.0190(14) 0.0278(15) 0.0236(15) -0.0055(12) -0.0058(12) 0.0005(12) C4 0.0228(15) 0.0260(15) 0.0194(14) 0.0008(11) -0.0069(12) -0.0023(12) C6 0.0217(16) 0.0387(18) 0.0216(15) -0.0044(12) -0.0007(13) -0.0026(12) C2 0.0178(14) 0.0275(15) 0.0215(14) 0.0013(12) -0.0002(11) 0.0001(11) O7 0.060(2) 0.087(3) 0.080(2) 0.023(2) 0.006(2) 0.0042(19) C1 0.0200(15) 0.0282(15) 0.0203(13) -0.0006(12) -0.0023(12) -0.0005(12) C5 0.0195(15) 0.0326(16) 0.0230(14) -0.0052(13) 0.0025(12) -0.0046(12) _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 U1 O1 2.398(2) 2_656 ? U1 O1 2.398(2) . ? U1 O4 2.503(2) 7_556 ? U1 O4 2.503(2) 8_556 ? U1 O2 2.480(2) 5_667 ? U1 O2 2.480(2) 6_565 ? U1 O3 2.4793(19) . ? U1 O3 2.4792(19) 2_656 ? U1 O5 2.436(2) . ? U1 O5 2.436(2) 2_656 ? Cl1 C5 1.725(3) . ? Cl2 C6 1.726(4) . ? O1 C1 1.267(3) . ? O4 C4 1.255(3) . ? O2 C2 1.252(3) . ? O3 C3 1.267(4) . ? C3 C4 1.520(5) 7_556 ? C3 C6 1.390(4) . ? C4 C6 1.396(4) . ? C2 C1 1.537(4) 5_667 ? C2 C5 1.390(4) . ? C1 C5 1.377(4) . ? 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 O1 U1 O1 124.08(10) 2_656 . ? O1 U1 O4 117.85(6) 2_656 7_556 ? O1 U1 O4 67.62(7) . 7_556 ? O1 U1 O4 67.62(7) 2_656 8_556 ? O1 U1 O4 117.85(7) . 8_556 ? O1 U1 O2 64.56(7) . 5_667 ? O1 U1 O2 64.56(6) 2_656 6_565 ? O1 U1 O2 69.62(7) . 6_565 ? O1 U1 O2 69.62(7) 2_656 5_667 ? O1 U1 O3 123.93(7) . . ? O1 U1 O3 65.95(7) 2_656 . ? O1 U1 O3 65.95(7) . 2_656 ? O1 U1 O3 123.93(7) 2_656 2_656 ? O1 U1 O5 81.73(7) . . ? O1 U1 O5 153.95(8) . 2_656 ? O1 U1 O5 81.73(7) 2_656 2_656 ? O1 U1 O5 153.96(8) 2_656 . ? O4 U1 O4 169.42(11) 7_556 8_556 ? O2 U1 O4 67.22(7) 5_667 8_556 ? O2 U1 O4 67.22(7) 6_565 7_556 ? O2 U1 O4 122.69(7) 6_565 8_556 ? O2 U1 O4 122.69(7) 5_667 7_556 ? O2 U1 O2 67.93(9) 5_667 6_565 ? O3 U1 O4 116.09(7) . 8_556 ? O3 U1 O4 62.01(7) . 7_556 ? O3 U1 O4 62.01(7) 2_656 8_556 ? O3 U1 O4 116.09(7) 2_656 7_556 ? O3 U1 O2 69.54(7) 2_656 5_667 ? O3 U1 O2 69.54(7) . 6_565 ? O3 U1 O2 128.02(7) 2_656 6_565 ? O3 U1 O2 128.02(7) . 5_667 ? O3 U1 O3 161.51(12) 2_656 . ? O5 U1 O4 65.50(7) . 7_556 ? O5 U1 O4 105.45(8) . 8_556 ? O5 U1 O4 65.50(7) 2_656 8_556 ? O5 U1 O4 105.45(8) 2_656 7_556 ? O5 U1 O2 131.14(7) . 6_565 ? O5 U1 O2 131.14(7) 2_656 5_667 ? O5 U1 O2 132.60(7) . 5_667 ? O5 U1 O2 132.60(7) 2_656 6_565 ? O5 U1 O3 98.00(8) . . ? O5 U1 O3 98.00(8) 2_656 2_656 ? O5 U1 O3 66.56(7) . 2_656 ? O5 U1 O3 66.56(7) 2_656 . ? O5 U1 O5 72.83(12) . 2_656 ? C1 O1 U1 122.21(18) . . ? C4 O4 U1 121.5(2) . 7_556 ? C2 O2 U1 120.29(18) . 5_667 ? C3 O3 U1 121.07(19) . . ? O3 C3 C4 114.0(3) . 7_556 ? O3 C3 C6 126.2(3) . . ? C6 C3 C4 119.8(3) . 7_556 ? O4 C4 C3 114.8(3) . 7_556 ? O4 C4 C6 125.4(3) . . ? C6 C4 C3 119.8(3) . 7_556 ? C3 C6 Cl2 120.3(3) . . ? C3 C6 C4 120.0(3) . . ? C4 C6 Cl2 119.6(3) . . ? O2 C2 C1 115.0(2) . 5_667 ? O2 C2 C5 125.1(3) . . ? C5 C2 C1 119.9(3) . 5_667 ? O1 C1 C2 115.2(2) . 5_667 ? O1 C1 C5 124.9(3) . . ? C5 C1 C2 119.8(3) . 5_667 ? C2 C5 Cl1 119.8(2) . . ? C1 C5 Cl1 119.9(2) . . ? C1 C5 C2 120.3(3) . . ? _shelx_res_file ; TITL exp_1123_u_a.res in C2/c exp_1123_u.res created by SHELXL-2018/3 at 11:15:37 on 21-Feb-2019 REM Old TITL exp_1123_U in Cc REM SHELXT solution in C2/c: R1 0.070, Rweak 0.012, Alpha 0.020 REM 0.458 for 106 systematic absences, Orientation as input REM Formula found by SHELXT: C12 O14 Cl4 U CELL 0.71073 13.8598 11.496 12.61 90 96.415 90 ZERR 4 0.0007 0.0006 0.0006 0 0.005 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl O U UNIT 48 48 16 56 4 L.S. 10 PLAN 20 SIZE 0.16 0.05 0.07 BOND list 4 fmap 2 acta REM REM REM WGHT 0.020300 0.294500 FVAR 0.23157 U1 5 0.500000 0.236501 0.750000 10.50000 0.01550 0.02347 = 0.01454 0.00000 -0.00400 0.00000 CL1 3 0.300195 0.395618 1.059228 11.00000 0.03069 0.05853 = 0.03817 -0.01421 0.01194 -0.01892 CL2 3 0.398038 0.265155 0.325230 11.00000 0.02999 0.08017 = 0.02848 -0.00244 0.00495 -0.00520 O1 4 0.409974 0.334302 0.875114 11.00000 0.02167 0.03186 = 0.02300 -0.00810 -0.00106 -0.00458 O4 4 0.179631 0.283570 0.296195 11.00000 0.02658 0.04135 = 0.01883 0.00480 -0.00639 -0.00518 O2 4 0.423552 0.584548 1.169155 11.00000 0.02482 0.03274 = 0.02025 -0.00672 0.00395 -0.00282 O3 4 0.437678 0.201854 0.560618 11.00000 0.02137 0.04389 = 0.02648 -0.00999 -0.00694 0.00628 O5 4 0.429484 0.065990 0.826309 11.00000 0.02953 0.03388 = 0.04892 0.00841 -0.01287 -0.00747 AFIX 7 H5A 2 0.473904 0.013269 0.842816 11.00000 -1.50000 H5B 2 0.389102 0.031672 0.778310 11.00000 -1.50000 AFIX 6 O6 4 0.231255 0.465478 0.780656 11.00000 0.04566 0.05937 = 0.06631 0.00609 0.00045 0.01479 H6A 2 0.216326 0.393728 0.780209 11.00000 -1.50000 H6B 2 0.287029 0.473446 0.759493 11.00000 -1.50000 AFIX 0 C3 1 0.351216 0.227745 0.525185 11.00000 0.01897 0.02784 = 0.02362 -0.00553 -0.00577 0.00054 C4 1 0.218768 0.271489 0.390208 11.00000 0.02278 0.02600 = 0.01945 0.00083 -0.00688 -0.00228 C6 1 0.317924 0.255709 0.420250 11.00000 0.02174 0.03868 = 0.02157 -0.00442 -0.00069 -0.00265 C2 1 0.455159 0.538965 1.089738 11.00000 0.01777 0.02748 = 0.02147 0.00128 -0.00015 0.00010 AFIX 6 O7 4 0.431503 0.079046 1.078210 11.00000 0.05993 0.08713 = 0.07958 0.02317 0.00569 0.00417 H7A 2 0.369783 0.078896 1.072594 11.00000 -1.50000 H7B 2 0.451341 0.143536 1.055828 11.00000 -1.50000 AFIX 0 C1 1 0.447816 0.411601 0.938246 11.00000 0.02001 0.02818 = 0.02031 -0.00057 -0.00233 -0.00055 C5 1 0.408296 0.452338 1.026578 11.00000 0.01948 0.03262 = 0.02296 -0.00524 0.00253 -0.00458 HKLF 4 REM exp_1123_u_a.res in C2/c REM wR2 = 0.0445, GooF = S = 1.056, Restrained GooF = 1.056 for all data REM R1 = 0.0200 for 2312 Fo > 4sig(Fo) and 0.0221 for all 2422 data REM 148 parameters refined using 0 restraints END WGHT 0.0203 0.2945 REM Highest difference peak 1.126, deepest hole -0.826, 1-sigma level 0.115 Q1 1 0.4878 0.2953 0.7774 11.00000 0.05 1.13 Q2 1 0.4847 0.1760 0.7968 11.00000 0.05 0.68 Q3 1 0.2911 0.4577 1.0181 11.00000 0.05 0.60 Q4 1 0.5333 0.1450 0.7688 11.00000 0.05 0.50 Q5 1 0.4416 0.3213 0.8330 11.00000 0.05 0.45 Q6 1 0.3633 0.3105 0.8750 11.00000 0.05 0.44 Q7 1 0.4197 0.2671 0.8597 11.00000 0.05 0.44 Q8 1 0.3887 0.6393 1.1490 11.00000 0.05 0.43 Q9 1 0.3292 0.3522 0.2830 11.00000 0.05 0.41 Q10 1 0.1888 0.2586 0.2106 11.00000 0.05 0.40 Q11 1 0.4741 0.3369 0.8489 11.00000 0.05 0.40 Q12 1 0.3733 0.3462 0.3457 11.00000 0.05 0.39 Q13 1 0.4386 0.2601 0.5795 11.00000 0.05 0.39 Q14 1 0.4670 0.2277 0.6500 11.00000 0.05 0.38 Q15 1 0.3962 0.1193 0.8191 11.00000 0.05 0.38 Q16 1 0.3681 0.1205 0.6243 11.00000 0.05 0.37 Q17 1 0.4704 0.1256 0.8464 11.00000 0.05 0.37 Q18 1 0.4306 0.4026 0.8399 11.00000 0.05 0.36 Q19 1 0.3697 0.0444 0.8170 11.00000 0.05 0.36 Q20 1 0.4197 0.3380 0.8215 11.00000 0.05 0.36 ; _shelx_res_checksum 3069 _shelx_hkl_file ; -16 -6 7 97.73 13.83 -16 -8 6 274.29 21.15 -15 -3 9 423.50 26.68 -15 -5 6 86.46 12.08 -15 -5 7 64.71 11.23 -15 -5 8 6.19 7.76 -15 -7 5 57.67 10.29 -15 -7 6 26.62 8.44 -15 -7 7 203.84 18.47 -15 -9 6 79.89 12.40 -14 -2 9 222.99 18.80 -14 -2 10 405.37 25.88 -14 -4 6 813.85 34.21 -14 -4 7 102.43 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8 4 -8 326.37 13.10 8 4 -7 156.85 8.49 8 4 -6 1970.65 42.79 8 4 -5 187.51 13.89 8 4 -5 167.12 8.54 8 -4 -4 1721.03 46.42 8 4 -4 1685.62 47.27 8 4 -4 1726.89 38.61 8 4 -3 117.86 7.36 8 -4 -3 107.29 9.48 8 4 -3 102.87 9.37 8 4 -2 2268.96 49.15 8 -4 -2 2271.11 60.57 8 4 -2 2270.18 54.82 8 4 -1 279.96 12.36 8 -4 -1 268.76 17.32 8 4 -1 264.97 13.50 8 -4 0 2945.58 72.42 8 4 0 2920.98 62.94 8 -4 1 78.68 9.85 8 4 1 88.31 6.77 8 4 2 1006.45 30.05 8 -4 2 939.91 33.90 8 4 2 968.81 24.98 8 4 3 920.25 29.06 8 4 3 932.30 22.47 8 -4 3 925.83 33.31 8 4 4 1366.34 38.45 8 4 4 1311.81 27.35 8 -4 4 1348.90 41.80 8 -4 5 10.16 5.43 8 -4 6 601.70 26.24 8 -4 7 66.65 9.25 8 -4 8 1288.64 42.87 8 -4 8 1257.56 49.88 8 -4 9 423.23 23.52 8 -4 9 394.07 26.37 8 -4 10 1992.49 58.57 8 -4 10 1848.47 63.84 8 -4 11 86.72 13.47 8 -4 11 87.35 11.96 8 -4 12 649.36 35.52 8 -4 13 122.88 16.06 8 6 -4 2020.65 56.31 8 6 -3 272.54 16.45 8 6 -2 907.83 31.26 8 -6 -1 300.59 19.84 8 6 -1 312.53 16.00 8 -6 0 383.98 22.02 8 6 0 423.31 17.74 8 6 1 197.00 11.03 8 -6 1 233.45 16.95 8 6 2 1783.88 40.11 8 -6 2 1795.31 53.38 8 -6 3 54.08 8.95 8 -6 4 476.59 24.52 8 -6 5 113.86 12.30 8 -6 6 554.91 26.63 8 -6 7 182.09 15.61 8 -6 8 1494.24 48.92 8 -6 8 1522.02 60.33 8 -6 9 385.11 23.17 8 -6 9 373.62 28.76 8 -6 10 648.01 30.85 8 -6 10 572.90 36.16 8 -6 11 268.32 19.88 8 -6 11 200.63 22.12 8 -6 12 512.79 35.14 8 -6 13 146.99 19.55 8 8 -3 889.75 34.97 8 8 -2 849.10 32.61 8 -8 -1 631.26 30.30 8 8 -1 650.07 26.65 8 -8 0 856.00 36.01 8 -8 1 236.16 18.56 8 -8 2 818.79 34.92 8 -8 3 342.66 22.03 8 -8 4 432.16 24.97 8 -8 5 106.45 13.20 8 -8 6 172.83 15.74 8 -8 7 474.42 25.95 8 -8 8 621.43 30.78 8 -8 8 627.66 40.63 8 -8 9 400.72 24.32 8 -8 9 381.80 32.03 8 -8 10 410.39 32.90 8 -8 10 368.82 23.89 8 -8 11 337.85 23.02 8 -8 11 319.44 30.09 8 -10 -1 323.05 22.86 8 -10 0 501.28 27.95 8 -10 1 261.23 20.04 8 -10 2 76.94 11.54 8 -10 3 481.21 27.54 8 -10 4 371.15 24.38 8 -10 5 101.54 13.47 8 -10 6 286.65 21.18 8 -10 7 309.09 22.01 8 -10 7 348.95 31.48 8 -10 8 138.83 15.24 8 -10 8 134.50 21.07 8 -12 -2 120.91 16.26 8 -12 -1 375.98 25.51 8 -12 0 98.40 13.84 8 -12 1 271.00 20.84 8 -12 2 113.31 14.33 8 -12 3 226.76 19.59 8 -12 4 99.30 14.31 8 -12 5 320.30 23.79 8 -14 -2 60.35 13.33 8 -14 -1 273.48 22.84 8 -14 0 31.97 9.93 8 -14 1 266.74 21.72 9 1 -5 1003.84 33.20 9 -1 -5 1004.69 33.05 9 1 -4 8.84 4.24 9 -1 -4 1.78 3.27 9 -1 -4 8.61 5.37 9 -1 -3 826.11 27.55 9 -1 -3 780.09 29.25 9 1 -3 807.68 27.21 9 -1 -2 259.69 13.86 9 -1 -2 248.95 15.54 9 1 -2 241.76 13.06 9 1 -1 1370.27 35.59 9 -1 -1 1320.12 36.25 9 -1 -1 1332.51 39.72 9 1 -1 1259.70 36.81 9 1 0 1.73 2.74 9 -1 0 2.03 3.17 9 -1 0 0.24 3.89 9 1 0 0.77 3.37 9 1 1 629.43 23.43 9 1 1 657.85 20.91 9 -1 1 636.54 25.43 9 1 2 1.24 3.70 9 1 2 1.58 2.53 9 -1 2 4.30 4.47 9 -1 3 2788.43 67.34 9 1 3 2790.44 66.10 9 1 3 2860.42 59.41 9 -1 4 22.54 5.71 9 1 4 21.16 5.30 9 -1 5 2197.20 57.85 9 1 5 2172.73 56.84 9 -1 6 14.55 5.80 9 1 6 12.22 5.93 9 -1 7 3555.02 84.49 9 1 7 3504.92 83.55 9 -1 8 135.73 13.20 9 1 8 170.91 14.32 9 -1 8 122.54 12.70 9 -1 9 1300.03 44.27 9 -1 9 1283.17 43.49 9 -1 10 14.91 7.13 9 -1 10 13.14 6.60 9 -1 11 383.19 22.07 9 3 -7 843.96 26.35 9 3 -6 100.37 8.05 9 3 -5 2245.82 51.93 9 3 -5 2286.84 59.43 9 3 -4 6.66 4.44 9 3 -4 12.35 3.61 9 -3 -3 1050.83 33.24 9 -3 -3 1067.89 37.55 9 3 -3 1031.44 32.86 9 3 -2 12.32 4.11 9 -3 -2 23.57 5.07 9 -3 -2 10.25 6.16 9 -3 -1 593.12 26.09 9 3 -1 583.32 21.29 9 3 0 2.82 2.81 9 3 0 1.42 2.97 9 3 1 3525.28 76.46 9 -3 1 3521.89 83.23 9 3 1 3552.00 72.32 9 3 2 159.12 11.35 9 -3 2 153.44 13.05 9 3 2 172.91 9.03 9 3 3 1203.22 36.83 9 -3 3 1276.52 41.00 9 3 3 1264.31 30.04 9 3 4 313.75 17.10 9 3 4 311.40 11.14 9 -3 4 290.76 17.98 9 3 5 1860.59 38.26 9 -3 5 1764.45 51.77 9 3 5 1804.89 49.89 9 3 6 41.71 3.42 9 -3 6 52.97 8.32 9 3 6 41.68 4.25 9 3 6 44.85 7.93 9 3 7 2760.25 51.18 9 -3 7 2757.75 70.75 9 3 7 2568.72 52.40 9 -3 8 174.08 14.78 9 3 8 146.75 6.17 9 -3 9 708.83 31.47 9 -3 9 627.19 33.27 9 -3 10 122.00 15.26 9 -3 10 159.01 15.51 9 -3 11 755.18 34.23 9 -3 11 717.83 35.63 9 -3 12 16.85 8.32 9 5 -9 737.98 19.70 9 5 -8 360.96 12.27 9 5 -7 1352.52 30.62 9 5 -6 177.93 8.30 9 5 -5 1303.93 30.68 9 5 -4 265.64 11.16 9 5 -4 267.17 17.40 9 5 -3 503.60 16.76 9 5 -3 464.99 22.09 9 5 -2 7.56 3.95 9 -5 -2 19.60 7.13 9 -5 -1 422.11 23.53 9 5 -1 441.88 19.35 9 5 0 90.20 7.73 9 -5 0 101.10 11.54 9 5 0 102.46 8.71 9 5 1 624.20 22.23 9 -5 1 575.79 27.86 9 5 1 617.43 21.05 9 5 2 876.65 28.06 9 5 2 844.54 23.98 9 -5 2 808.01 33.23 9 5 3 1845.23 39.39 9 -5 3 1823.26 54.52 9 5 4 90.00 4.09 9 -5 4 118.94 12.23 9 -5 5 1119.58 40.30 9 -5 6 545.78 26.89 9 -5 7 1777.31 54.73 9 -5 8 286.41 20.07 9 -5 9 735.64 33.14 9 -5 9 658.52 38.01 9 -5 10 21.22 8.55 9 -5 10 17.28 8.78 9 -5 11 583.49 30.44 9 -5 11 511.60 34.02 9 -5 12 138.25 18.24 9 -5 13 382.36 29.49 9 7 -3 291.02 18.39 9 -7 -2 392.73 24.02 9 7 -2 397.50 20.75 9 -7 -1 817.28 35.26 9 7 -1 808.45 29.19 9 7 0 97.72 9.35 9 -7 0 103.40 12.98 9 7 1 722.10 24.51 9 -7 1 768.25 33.82 9 -7 2 249.05 19.03 9 -7 3 1151.06 43.08 9 -7 4 185.79 16.51 9 -7 5 852.98 36.47 9 -7 6 435.58 25.33 9 -7 7 636.50 31.15 9 -7 8 856.49 37.37 9 -7 9 533.24 28.85 9 -7 9 463.30 35.21 9 -7 10 122.27 14.65 9 -7 10 126.37 19.22 9 -7 11 175.26 21.95 9 -7 11 189.45 18.03 9 -7 12 209.91 19.29 9 -9 -2 412.36 26.33 9 -9 -1 423.92 25.96 9 -9 0 278.13 20.85 9 -9 1 441.08 26.56 9 -9 2 212.35 18.76 9 -9 3 227.74 19.46 9 -9 4 558.55 30.39 9 -9 5 489.13 28.65 9 -9 6 324.62 22.85 9 -9 7 310.48 22.41 9 -9 8 403.75 26.12 9 -9 8 439.87 35.85 9 -9 9 209.69 19.12 9 -9 10 242.63 20.44 9 -11 -2 162.17 17.74 9 -11 -1 145.15 16.42 9 -11 0 288.94 22.29 9 -11 1 246.70 20.71 9 -11 2 345.62 24.61 9 -11 3 64.81 12.21 9 -11 4 282.35 22.36 9 -11 5 187.94 18.76 9 -11 6 507.53 30.35 9 -11 7 248.64 21.19 9 -13 -3 39.57 11.10 9 -13 -2 169.53 18.59 9 -13 -1 80.51 13.23 9 -13 0 186.76 18.82 9 -13 1 64.82 12.72 9 -13 2 211.78 20.16 9 -13 3 74.89 11.97 9 -13 4 201.99 19.71 10 0 -6 392.53 20.72 10 0 -5 4.42 4.38 10 0 -4 982.31 33.72 10 0 -4 997.63 32.95 10 0 -3 3.05 3.96 10 0 -3 -2.45 4.84 10 0 -2 2100.79 52.37 10 0 -2 2124.70 55.34 10 0 -1 5.80 3.67 10 0 -1 -1.69 4.64 10 0 0 3659.38 78.04 10 0 0 3644.79 82.89 10 0 1 0.70 3.12 10 0 1 0.43 4.11 10 0 2 2043.87 54.60 10 0 2 2162.58 50.25 10 0 3 0.98 4.22 10 0 4 1352.09 41.91 10 0 5 2.75 5.33 10 0 6 1496.86 46.67 10 0 7 2.27 5.53 10 0 8 740.93 31.80 10 0 8 668.63 28.95 10 0 9 3.66 4.33 10 0 9 6.84 6.17 10 2 -9 9.87 5.03 10 2 -8 600.28 24.16 10 2 -7 16.23 4.93 10 2 -6 473.20 20.42 10 -2 -5 410.07 22.07 10 2 -5 321.59 16.47 10 -2 -4 395.65 21.75 10 2 -4 395.18 18.02 10 2 -4 426.14 20.42 10 2 -3 -1.95 3.94 10 -2 -3 -4.05 5.27 10 2 -3 -4.62 4.25 10 -2 -2 3274.00 73.41 10 -2 -2 3169.97 78.00 10 2 -2 3148.78 71.65 10 2 -2 3172.33 71.67 10 -2 -1 142.44 10.96 10 -2 -1 145.33 13.11 10 2 -1 136.06 10.58 10 2 -1 139.08 10.20 10 2 0 2849.70 65.68 10 -2 0 2917.40 71.77 10 2 0 2804.64 62.79 10 2 1 148.91 9.50 10 2 1 153.84 11.37 10 -2 1 142.83 13.02 10 2 2 3045.66 64.50 10 2 2 3096.57 71.23 10 -2 2 2994.58 74.41 10 2 3 41.25 6.84 10 2 3 41.30 4.95 10 -2 3 50.21 8.30 10 -2 4 1264.96 41.62 10 2 4 1340.01 32.90 10 2 4 1339.15 40.72 10 2 5 274.33 11.77 10 -2 5 270.45 17.74 10 2 5 271.74 17.00 10 2 6 1810.63 40.41 10 -2 6 1778.87 53.61 10 2 6 1776.48 52.26 10 -2 7 8.31 5.99 10 2 7 19.58 4.76 10 2 7 14.02 6.62 10 -2 8 866.44 35.65 10 2 8 922.44 35.82 10 2 8 873.53 26.32 10 -2 9 14.74 6.53 10 -2 9 23.32 7.91 10 -2 10 604.00 30.09 10 -2 10 589.33 30.69 10 -2 11 140.72 15.26 10 -2 11 179.10 17.33 10 4 -8 847.07 25.69 10 4 -7 84.98 7.34 10 4 -6 379.32 15.61 10 -4 -4 741.34 32.79 10 4 -4 755.76 29.88 10 -4 -3 376.74 23.06 10 4 -3 368.36 19.42 10 -4 -2 2666.17 71.07 10 4 -2 2646.98 64.06 10 4 -1 14.81 4.80 10 4 -1 5.66 3.74 10 -4 -1 24.77 7.36 10 4 0 1182.00 34.31 10 -4 0 1183.77 41.66 10 4 0 1175.14 33.82 10 4 1 323.67 16.39 10 -4 1 310.38 19.92 10 4 1 320.47 14.68 10 4 2 2015.78 50.63 10 -4 2 1795.64 55.73 10 4 2 1931.24 44.88 10 4 3 1223.56 37.43 10 4 3 1115.08 28.96 10 -4 3 1119.50 40.74 10 4 4 1378.32 41.16 10 4 4 1356.95 31.33 10 -4 4 1300.51 44.79 10 4 5 17.55 6.08 10 4 5 11.81 2.24 10 -4 5 5.68 5.91 10 -4 6 718.60 31.65 10 -4 7 152.04 14.96 10 -4 8 661.86 31.59 10 -4 9 0.85 6.13 10 -4 9 -9.99 9.73 10 -4 10 703.21 34.22 10 -4 10 560.81 34.30 10 -4 11 61.97 12.80 10 -4 11 58.08 11.63 10 -4 12 762.43 40.18 10 6 -7 154.37 6.57 10 6 -6 608.07 16.75 10 6 -5 18.47 3.24 10 6 -4 579.51 18.24 10 -6 -3 432.70 25.61 10 6 -3 432.99 22.34 10 -6 -2 1013.21 40.58 10 6 -2 995.49 34.45 10 6 -1 372.16 15.67 10 -6 -1 325.80 22.24 10 6 -1 337.47 17.79 10 6 0 1504.84 39.05 10 -6 0 1373.69 48.89 10 6 0 1402.09 40.05 10 6 1 424.23 17.81 10 -6 1 415.31 24.61 10 6 2 1003.63 28.32 10 -6 2 1053.49 40.43 10 6 3 451.06 14.70 10 -6 3 500.21 27.04 10 -6 4 1058.86 41.83 10 -6 5 178.07 16.30 10 -6 6 613.32 30.65 10 -6 7 361.36 23.47 10 -6 8 297.51 21.41 10 -6 9 134.56 18.92 10 -6 9 179.09 17.24 10 -6 10 633.24 33.27 10 -6 10 544.37 37.58 10 -6 11 117.61 15.31 10 -6 11 100.59 17.37 10 -6 12 461.38 29.11 10 -6 12 411.55 32.80 10 -8 -3 213.57 19.69 10 -8 -2 528.45 29.75 10 8 -2 504.65 25.10 10 -8 -1 754.09 35.84 10 8 -1 776.95 30.13 10 -8 0 884.67 39.01 10 -8 1 359.05 24.04 10 -8 2 495.26 28.83 10 -8 3 126.81 15.10 10 -8 4 453.44 27.67 10 -8 5 374.84 25.24 10 -8 6 461.90 27.77 10 -8 7 247.90 20.66 10 -8 8 127.67 15.58 10 -8 9 115.73 15.02 10 -8 9 119.44 20.09 10 -8 10 375.69 26.00 10 -8 11 326.40 25.54 10 -10 -3 201.48 19.99 10 -10 -2 461.03 29.12 10 -10 -1 416.75 27.50 10 -10 0 236.32 21.17 10 -10 1 613.35 33.27 10 -10 2 152.69 16.97 10 -10 3 390.44 26.41 10 -10 4 203.47 19.54 10 -10 5 370.05 26.18 10 -10 6 121.48 15.64 10 -10 7 364.26 25.83 10 -10 8 157.94 17.79 10 -10 9 39.64 10.49 10 -12 -3 329.77 25.91 10 -12 -2 128.89 16.87 10 -12 -1 313.64 24.63 10 -12 0 158.02 18.12 10 -12 1 189.77 19.26 10 -12 2 74.87 13.26 10 -12 3 285.46 23.72 10 -12 4 89.61 14.77 10 -12 5 190.79 19.93 11 1 -9 1050.58 37.14 11 1 -8 1.44 4.50 11 -1 -7 1024.78 38.32 11 1 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-7 1159.88 34.98 11 3 -6 2.78 3.64 11 -3 -5 1843.41 57.32 11 3 -5 1865.20 47.82 11 -3 -4 576.03 28.67 11 3 -4 597.62 22.97 11 -3 -3 1539.64 50.09 11 3 -3 1529.65 44.92 11 3 -3 1534.44 41.97 11 3 -2 123.18 10.31 11 -3 -2 116.27 13.06 11 3 -2 128.19 10.89 11 3 -1 1207.31 35.88 11 -3 -1 1200.74 42.64 11 3 -1 1175.53 35.54 11 3 0 8.26 4.74 11 3 0 11.52 3.93 11 -3 0 3.96 5.76 11 3 1 669.37 25.82 11 -3 1 686.99 30.25 11 3 1 648.12 22.79 11 3 2 272.70 16.36 11 -3 2 293.11 19.52 11 3 2 268.23 13.28 11 3 3 851.48 31.27 11 -3 3 865.92 34.87 11 3 3 875.00 25.63 11 -3 4 123.61 13.24 11 3 4 141.01 12.57 11 3 4 124.90 8.20 11 -3 5 1606.61 52.23 11 3 5 1738.51 50.88 11 3 5 1670.19 38.32 11 -3 6 79.28 11.04 11 3 6 89.52 10.86 11 -3 7 1149.56 43.65 11 3 7 1215.82 42.16 11 -3 8 38.96 9.62 11 -3 9 1098.23 43.47 11 -3 9 978.82 45.58 11 -3 10 9.61 7.69 11 -3 10 41.30 11.14 11 -3 11 638.45 33.84 11 -3 11 564.00 33.15 11 5 -8 103.93 7.37 11 5 -7 786.66 23.21 11 -5 -4 48.75 10.42 11 5 -3 2267.82 52.69 11 -5 -3 2217.88 67.07 11 5 -2 420.74 17.91 11 -5 -2 409.78 25.34 11 5 -2 406.69 20.80 11 5 -1 838.82 27.74 11 -5 -1 828.94 36.14 11 5 -1 819.51 29.69 11 5 0 124.38 10.36 11 -5 0 109.31 13.17 11 5 0 126.06 10.36 11 5 1 581.74 23.62 11 -5 1 573.88 29.16 11 5 1 544.75 21.22 11 5 2 177.35 12.92 11 5 2 165.05 10.41 11 -5 2 175.28 16.15 11 5 3 1128.23 36.85 11 5 3 1110.56 29.42 11 -5 3 1106.51 42.91 11 5 4 503.67 23.48 11 -5 4 460.29 26.73 11 -5 5 939.46 39.12 11 -5 6 129.96 14.69 11 -5 7 685.54 33.34 11 -5 8 95.19 13.15 11 -5 9 802.91 37.56 11 -5 9 706.22 42.50 11 -5 10 149.55 17.40 11 -5 10 112.10 17.51 11 -5 11 719.03 36.95 11 -5 11 611.63 39.11 11 -5 12 68.25 14.54 11 -7 -4 653.43 34.69 11 -7 -3 877.79 39.82 11 -7 -2 351.22 24.41 11 7 -2 342.98 20.04 11 -7 -1 202.37 18.65 11 7 -1 247.48 15.97 11 7 0 259.48 15.54 11 -7 0 249.33 20.87 11 -7 1 491.34 28.78 11 -7 2 219.97 19.44 11 -7 3 598.21 31.99 11 -7 4 44.61 10.34 11 -7 5 482.54 29.07 11 -7 6 472.33 28.44 11 -7 7 570.17 31.67 11 -7 8 179.66 18.36 11 -7 9 360.47 26.13 11 -7 9 336.70 31.67 11 -7 10 201.23 25.26 11 -7 10 227.15 21.11 11 -9 -4 493.03 31.47 11 -9 -3 444.37 29.53 11 -9 -2 305.52 23.90 11 -9 -1 255.81 22.08 11 -9 0 212.99 19.91 11 -9 1 125.81 15.51 11 -9 2 477.55 30.17 11 -9 3 355.14 26.23 11 -9 4 204.30 19.63 11 -9 5 319.10 24.92 11 -9 6 376.97 26.57 11 -9 7 230.82 20.99 11 -9 8 235.63 21.48 11 -9 9 375.11 27.34 11 -11 -4 119.94 17.71 11 -11 -3 69.84 13.08 11 -11 -2 457.79 30.65 11 -11 -1 251.06 22.90 11 -11 0 134.32 17.02 11 -11 1 64.89 13.47 11 -11 2 233.62 21.52 11 -11 3 74.24 13.60 11 -11 4 261.47 23.35 11 -11 5 161.04 18.68 11 -11 6 234.05 21.95 12 0 -9 -5.09 5.98 12 0 -8 1155.99 41.31 12 0 -7 1.30 5.41 12 0 -6 437.73 23.21 12 0 -5 2.13 4.95 12 0 -4 698.70 29.63 12 0 -3 5.49 5.70 12 0 -2 1186.63 40.35 12 0 -1 -6.80 5.87 12 0 0 1617.82 44.48 12 0 0 1545.94 48.15 12 0 1 2.41 4.24 12 0 1 2.66 5.70 12 0 2 3154.34 78.61 12 0 2 3256.49 73.10 12 0 3 -7.81 5.97 12 0 3 1.30 4.15 12 0 4 1488.62 48.23 12 0 4 1566.44 42.38 12 0 5 -9.17 6.45 12 0 6 438.22 24.65 12 0 7 0.90 5.62 12 0 8 1091.53 43.17 12 0 9 18.24 8.26 12 0 10 557.05 30.87 12 2 -11 6.17 5.77 12 2 -10 818.74 32.04 12 2 -9 -3.28 4.68 12 2 -8 912.49 33.09 12 -2 -7 58.87 10.36 12 2 -7 90.39 9.96 12 -2 -6 915.86 37.73 12 2 -6 911.28 32.54 12 -2 -5 17.21 7.34 12 2 -5 15.83 5.63 12 -2 -4 1076.15 40.18 12 2 -4 1052.56 35.19 12 -2 -3 180.76 15.92 12 2 -3 221.41 14.74 12 -2 -2 433.09 24.38 12 2 -2 436.39 21.03 12 2 -1 47.60 7.17 12 -2 -1 58.43 9.57 12 2 -1 58.20 8.21 12 2 0 1606.56 46.61 12 -2 0 1615.48 51.59 12 2 0 1641.30 44.30 12 2 1 6.41 5.39 12 2 1 6.14 3.93 12 -2 1 2.46 5.56 12 2 2 2024.03 49.78 12 2 2 2050.38 56.10 12 -2 2 2008.79 59.67 12 2 3 80.65 7.51 12 2 3 69.61 9.47 12 -2 3 69.67 10.59 12 2 4 944.38 28.26 12 -2 4 944.34 37.58 12 2 4 932.36 35.29 12 -2 5 24.04 7.28 12 2 5 18.82 6.78 12 -2 6 1513.66 51.37 12 2 6 1545.81 50.97 12 -2 7 3.80 6.34 12 2 7 36.79 9.64 12 -2 8 401.44 25.07 12 2 8 433.93 25.12 12 -2 9 -10.97 9.12 12 -2 9 15.11 8.43 12 -2 10 480.50 28.65 12 4 -8 394.84 17.92 12 4 -7 3.92 3.60 12 -4 -6 488.90 28.79 12 4 -6 483.81 20.16 12 -4 -5 113.91 14.37 12 4 -5 97.62 9.07 12 4 -4 1487.06 40.46 12 -4 -4 1358.29 50.07 12 4 -3 121.19 10.13 12 -4 -3 152.40 15.75 12 4 -2 235.15 14.28 12 -4 -2 267.79 20.11 12 4 -2 232.56 15.82 12 4 -1 5.01 4.18 12 4 -1 13.31 5.01 12 -4 -1 7.20 6.29 12 4 0 1319.29 40.04 12 -4 0 1339.82 48.35 12 4 0 1304.61 38.93 12 4 1 392.22 19.95 12 -4 1 363.45 23.42 12 4 1 369.56 17.59 12 4 2 1521.43 45.44 12 -4 2 1559.69 52.49 12 4 2 1496.61 40.23 12 4 3 239.55 16.52 12 -4 3 235.79 18.91 12 4 4 966.41 35.84 12 -4 4 922.31 39.16 12 -4 5 233.03 18.94 12 4 5 237.98 17.14 12 -4 6 1334.89 48.83 12 4 6 1355.82 45.97 12 -4 7 45.55 10.02 12 -4 8 354.33 24.77 12 -4 9 8.87 8.04 12 -4 9 -11.89 10.55 12 -4 10 483.23 30.14 12 -4 10 407.08 31.30 12 -6 -5 368.18 26.63 12 6 -4 433.83 17.25 12 -6 -4 425.34 27.89 12 6 -3 156.69 10.54 12 -6 -3 150.29 16.66 12 6 -2 857.32 27.96 12 -6 -2 755.48 37.07 12 6 -1 120.14 10.20 12 6 -1 135.45 12.39 12 -6 -1 111.04 14.68 12 6 0 552.65 23.02 12 -6 0 517.50 29.93 12 6 1 622.29 25.21 12 -6 1 611.20 32.74 12 6 2 1188.36 38.12 12 -6 2 1111.64 45.78 12 -6 3 86.27 13.29 12 -6 4 818.08 38.53 12 -6 5 168.26 17.84 12 -6 6 299.45 23.02 12 -6 7 134.87 15.86 12 -6 8 406.75 27.68 12 -6 9 24.94 9.10 12 -6 9 29.25 12.90 12 -6 10 244.05 26.73 12 -8 -5 89.32 14.93 12 -8 -4 176.35 19.75 12 -8 -3 369.95 27.18 12 -8 -2 317.39 24.46 12 -8 -1 104.45 15.06 12 -8 0 298.79 23.68 12 -8 1 402.75 27.60 12 -8 2 496.56 30.31 12 -8 3 438.98 28.72 12 -8 4 636.17 34.90 12 -8 5 178.26 18.54 12 -8 6 339.74 25.75 12 -8 7 170.62 18.35 12 -8 8 239.59 22.28 12 -10 -5 172.27 21.14 12 -10 -4 222.05 22.42 12 -10 -3 122.59 16.72 12 -10 -2 52.45 12.08 12 -10 -1 229.21 22.01 12 -10 0 317.57 25.20 12 -10 1 345.54 25.89 12 -10 2 172.04 18.99 12 -10 3 330.51 26.09 12 -10 4 205.51 20.76 12 -10 5 236.87 22.04 12 -10 6 196.76 20.40 13 1 -11 367.26 22.96 13 -1 -10 4.80 6.36 13 1 -10 2.83 5.62 13 -1 -9 194.09 17.36 13 1 -9 192.99 15.91 13 -1 -8 18.29 7.51 13 1 -8 0.12 5.36 13 -1 -7 614.73 30.51 13 1 -7 636.51 28.47 13 -1 -6 78.56 11.15 13 1 -6 97.94 11.24 13 -1 -5 1341.38 46.86 13 1 -5 1369.48 44.67 13 -1 -4 29.02 8.25 13 1 -4 13.60 5.92 13 -1 -3 970.78 38.24 13 1 -3 984.18 36.06 13 -1 -2 9.21 6.28 13 1 -2 10.34 6.91 13 -1 -1 1827.85 56.74 13 1 -1 1907.03 54.69 13 -1 0 166.20 15.28 13 1 0 174.98 14.39 13 1 1 1547.26 47.81 13 -1 1 1462.40 49.28 13 1 2 21.16 6.99 13 1 2 15.11 5.07 13 -1 2 17.03 6.97 13 -1 3 349.39 22.40 13 1 3 347.57 17.20 13 1 3 353.18 21.32 13 -1 4 -0.67 5.21 13 1 4 -0.77 5.97 13 -1 5 582.57 29.82 13 1 5 620.48 29.95 13 -1 6 67.04 11.13 13 1 6 78.52 11.30 13 -1 7 419.77 26.22 13 1 7 475.75 27.51 13 -1 8 9.10 6.83 13 1 8 7.85 7.64 13 -1 9 1171.72 47.79 13 1 9 1150.05 46.20 13 3 -9 525.73 23.65 13 -3 -8 -2.99 7.03 13 3 -8 -4.47 5.33 13 -3 -7 502.68 29.87 13 3 -7 553.09 23.91 13 -3 -6 38.30 9.47 13 3 -6 47.33 7.89 13 -3 -5 1205.05 46.44 13 3 -5 1281.75 39.72 13 -3 -4 140.40 15.50 13 3 -4 135.31 11.70 13 -3 -3 1395.02 50.44 13 3 -3 1461.36 43.25 13 -3 -2 27.83 8.98 13 3 -2 26.20 6.32 13 3 -1 726.09 28.84 13 -3 -1 735.79 34.45 13 3 0 73.35 9.28 13 3 0 84.26 9.08 13 -3 0 107.90 13.83 13 3 1 1313.30 41.77 13 -3 1 1289.59 47.45 13 3 1 1239.02 37.43 13 3 2 1.99 5.41 13 3 2 9.47 4.60 13 -3 2 11.20 6.45 13 3 3 453.85 23.63 13 -3 3 441.68 26.32 13 3 4 33.47 8.35 13 -3 4 28.99 8.80 13 -3 5 640.80 32.41 13 3 5 623.34 30.11 13 -3 6 51.41 10.66 13 3 6 54.83 10.20 13 -3 7 1211.33 47.50 13 3 7 1210.69 44.94 13 -3 8 24.50 9.07 13 -3 9 597.41 33.40 13 -5 -7 323.45 25.47 13 5 -6 7.96 3.94 13 -5 -6 20.28 8.98 13 5 -5 433.80 18.81 13 -5 -5 412.69 27.55 13 5 -4 358.93 17.27 13 -5 -4 319.44 24.03 13 5 -3 1325.71 38.52 13 -5 -3 1226.59 49.57 13 5 -2 281.26 16.08 13 -5 -2 249.66 21.16 13 5 -1 995.05 33.34 13 -5 -1 926.41 41.64 13 5 0 115.79 11.24 13 -5 0 118.23 15.55 13 5 1 651.31 27.25 13 -5 1 596.95 32.95 13 5 2 247.89 17.08 13 -5 2 221.44 19.76 13 5 3 433.82 22.66 13 -5 3 417.86 26.98 13 5 4 35.31 8.37 13 -5 4 24.72 9.42 13 -5 5 343.87 24.71 13 -5 6 59.08 11.93 13 -5 7 364.46 25.98 13 -5 8 97.40 14.06 13 -5 10 95.39 17.77 13 -7 -6 210.15 21.78 13 -7 -5 497.66 32.33 13 -7 -4 302.28 24.90 13 7 -3 286.37 14.67 13 -7 -3 300.27 24.32 13 7 -2 178.83 12.13 13 -7 -2 175.75 18.90 13 -7 -1 1217.47 50.28 13 -7 0 358.93 26.49 13 -7 1 344.30 25.77 13 -7 2 177.83 19.22 13 -7 3 290.18 24.07 13 -7 4 45.45 11.10 13 -7 5 659.01 36.00 13 -7 6 114.27 15.99 13 -7 7 220.54 21.13 13 -9 -5 268.69 25.23 13 -9 -4 214.84 22.31 13 -9 -3 259.56 24.13 13 -9 -2 86.73 14.93 13 -9 -1 87.53 14.75 13 -9 0 396.74 28.85 13 -9 1 259.06 23.86 13 -9 2 120.43 16.42 13 -9 3 149.80 18.71 13 -9 4 199.58 20.96 14 0 -12 113.85 14.19 14 0 -11 3.91 6.68 14 0 -10 826.00 36.72 14 0 -9 3.97 6.89 14 0 -8 631.34 31.13 14 0 -7 -5.76 6.63 14 0 -6 780.75 34.11 14 0 -5 -0.84 5.73 14 0 -4 1127.92 41.90 14 0 -3 2.12 5.75 14 0 -2 222.47 17.88 14 0 -1 -2.89 6.31 14 0 0 1025.99 39.26 14 0 1 0.27 5.53 14 0 2 1038.84 40.44 14 0 3 3.12 6.45 14 0 4 738.25 34.16 14 0 5 -0.78 5.98 14 0 6 896.06 39.34 14 0 7 3.46 7.14 14 -2 -11 2.47 7.29 14 -2 -10 325.62 24.83 14 -2 -9 194.61 18.75 14 2 -9 195.86 15.71 14 -2 -8 1080.02 44.75 14 2 -8 1160.35 40.39 14 -2 -7 -0.75 7.25 14 2 -7 13.24 6.17 14 -2 -6 793.98 36.89 14 2 -6 845.96 33.07 14 -2 -5 72.12 11.92 14 2 -5 70.88 10.02 14 -2 -4 584.10 30.57 14 2 -4 573.89 26.93 14 -2 -3 18.45 7.25 14 2 -3 19.24 6.39 14 -2 -2 329.61 22.96 14 2 -2 346.50 20.38 14 -2 -1 -5.43 6.56 14 2 -1 11.20 6.14 14 2 0 496.92 25.03 14 -2 0 480.37 27.94 14 2 1 84.53 11.20 14 -2 1 81.19 11.93 14 2 2 659.05 30.42 14 -2 2 676.95 33.34 14 2 3 2.55 5.74 14 -2 3 8.91 6.65 14 -2 4 1251.59 47.94 14 2 4 1280.43 45.80 14 -2 5 57.22 11.11 14 2 5 61.74 10.34 14 -2 6 1366.10 51.43 14 2 6 1393.67 50.68 14 -2 7 124.06 16.05 14 2 7 150.63 16.02 14 -4 -9 70.03 13.28 14 -4 -8 755.09 38.73 14 -4 -7 108.77 15.55 14 4 -7 120.61 10.89 14 -4 -6 764.10 38.44 14 4 -6 826.35 29.68 14 -4 -5 62.56 11.90 14 4 -5 64.33 8.71 14 4 -4 396.16 20.26 14 -4 -4 390.42 26.79 14 4 -3 85.74 9.93 14 -4 -3 91.21 13.85 14 4 -2 593.02 25.50 14 -4 -2 567.13 31.94 14 4 -1 59.70 8.57 14 -4 -1 53.22 11.83 14 4 0 358.58 20.37 14 -4 0 335.30 24.48 14 4 1 20.61 6.91 14 -4 1 16.32 8.26 14 4 2 443.40 23.84 14 -4 2 412.95 27.14 14 4 3 41.88 8.99 14 -4 3 42.45 10.71 14 -4 4 1160.89 47.79 14 4 4 1220.85 44.04 14 -4 5 152.04 17.10 14 4 5 133.27 14.24 14 -4 6 696.01 36.46 14 4 6 733.09 34.54 14 -4 7 102.83 15.19 14 -6 -8 307.39 26.62 14 -6 -7 195.33 21.64 14 -6 -6 256.74 23.45 14 -6 -5 92.29 15.17 14 6 -4 459.60 20.09 14 -6 -4 429.31 29.45 14 6 -3 21.48 6.09 14 -6 -3 16.02 8.93 14 6 -2 402.74 20.02 14 -6 -2 377.36 27.61 14 6 -1 319.80 18.59 14 -6 -1 281.51 24.09 14 6 0 681.97 28.37 14 -6 0 649.02 36.19 14 6 1 26.79 7.21 14 -6 1 35.18 11.07 14 6 2 364.33 21.15 14 -6 2 345.45 26.21 14 -6 3 142.57 17.31 14 -6 4 553.96 33.18 14 -6 5 272.65 22.95 14 -6 6 579.14 34.87 14 -8 -4 281.41 25.62 14 -8 -3 94.92 15.22 14 -8 -2 169.83 19.94 14 -8 -1 27.85 10.81 14 -8 0 95.30 16.03 14 -8 1 285.04 24.55 14 -8 2 293.53 25.36 14 -8 3 105.74 16.11 15 -1 -12 -0.57 6.77 15 -1 -11 327.27 24.50 15 -1 -10 -3.24 7.15 15 1 -10 0.28 6.27 15 -1 -9 310.58 23.07 15 1 -9 304.37 21.24 15 -1 -8 86.15 12.68 15 1 -8 66.50 10.23 15 -1 -7 171.70 17.04 15 1 -7 179.10 16.35 15 -1 -6 25.97 8.55 15 1 -6 12.82 5.94 15 -1 -5 313.74 22.75 15 1 -5 338.86 21.98 15 -1 -4 -8.22 7.86 15 1 -4 1.36 6.20 15 -1 -3 716.37 34.25 15 1 -3 692.31 32.07 15 -1 -2 6.82 6.99 15 1 -2 38.06 8.35 15 -1 -1 1032.58 42.58 15 1 -1 1062.61 40.42 15 -1 0 1.94 7.24 15 1 0 10.77 6.99 15 1 1 1134.29 43.44 15 -1 1 1183.03 45.64 15 1 2 11.18 6.56 15 -1 2 23.17 8.30 15 -1 3 1256.93 48.05 15 1 3 1258.52 46.78 15 -1 4 -1.17 7.43 15 1 4 -0.31 6.47 15 -1 5 572.78 31.96 15 1 5 579.20 31.02 15 -1 6 0.76 8.48 15 1 6 6.68 8.27 15 -3 -11 497.51 32.61 15 -3 -10 49.44 11.68 15 -3 -9 340.35 25.84 15 -3 -8 10.40 7.88 15 -3 -7 152.09 17.05 15 3 -7 162.14 14.13 15 -3 -6 0.40 7.21 15 3 -6 11.31 5.79 15 -3 -5 682.70 36.02 15 3 -5 679.30 29.30 15 -3 -4 -4.72 8.04 15 3 -4 12.96 5.62 15 3 -3 205.73 15.77 15 -3 -3 201.80 19.68 15 3 -2 128.41 12.94 15 -3 -2 107.41 14.92 15 3 -1 911.70 35.61 15 -3 -1 946.70 42.19 15 3 0 64.48 9.98 15 -3 0 60.28 11.96 15 3 1 941.58 37.35 15 -3 1 912.04 41.89 15 3 2 51.19 9.24 15 -3 2 74.41 13.01 15 -3 3 570.91 32.36 15 3 3 564.20 29.08 15 -3 4 56.65 11.84 15 3 4 59.96 10.71 15 -3 5 883.71 41.54 15 3 5 915.56 40.05 15 3 6 58.85 11.27 15 -5 -8 5.40 7.88 15 -5 -7 63.28 12.58 15 -5 -6 59.99 12.95 15 -5 -5 282.62 24.35 15 5 -4 39.74 7.41 15 -5 -4 41.31 11.79 15 5 -3 544.30 24.54 15 -5 -3 537.63 33.22 15 5 -2 48.06 8.05 15 -5 -2 77.56 13.31 15 5 -1 725.38 30.30 15 -5 -1 770.23 39.54 15 5 0 354.35 20.96 15 -5 0 359.31 26.73 15 5 1 1109.39 40.19 15 -5 1 1047.80 47.08 15 5 2 7.80 6.05 15 -5 2 -6.00 8.12 15 5 3 530.22 27.44 15 -5 3 521.25 32.50 15 5 4 146.13 15.04 15 -5 4 119.14 16.37 15 -7 -4 116.41 17.39 15 -7 -3 362.06 28.31 15 -7 -2 79.43 14.66 15 7 -1 614.07 26.02 15 -7 -1 502.31 33.81 15 -7 0 195.40 20.86 15 -7 1 219.64 21.71 16 0 -10 137.61 16.17 16 0 -9 6.27 7.38 16 0 -8 56.53 11.08 16 0 -7 2.42 6.77 16 0 -6 1187.51 46.68 16 0 -5 -11.15 8.72 16 0 -4 399.09 25.28 16 0 -3 -1.87 6.55 16 0 -2 938.24 40.36 16 0 -1 0.63 6.08 16 0 0 666.59 33.08 16 0 1 8.80 7.57 16 0 2 336.60 24.07 16 0 3 -6.82 7.73 16 0 4 1071.30 45.16 16 -2 -10 178.72 19.43 16 -2 -9 -23.55 9.69 16 -2 -8 295.32 23.82 16 2 -8 321.08 21.24 16 -2 -7 61.07 12.37 16 2 -7 57.52 10.66 16 -2 -6 639.34 34.86 16 2 -6 611.76 30.03 16 -2 -5 -1.59 7.50 16 2 -5 7.90 6.51 16 -2 -4 929.36 42.12 16 2 -4 883.50 36.69 16 -2 -3 0.51 7.06 16 2 -3 11.32 6.55 16 2 -2 566.66 28.62 16 -2 -2 603.48 33.30 16 2 -1 126.03 13.99 16 -2 -1 104.94 14.92 16 2 0 524.37 28.15 16 -2 0 520.67 30.92 16 2 1 4.71 6.46 16 -2 1 11.71 8.14 16 -2 2 396.38 27.13 16 2 2 410.42 25.41 16 -2 3 54.11 12.07 16 2 3 35.02 9.74 16 -2 4 712.01 36.96 16 2 4 718.46 34.92 16 -4 -8 251.01 23.20 16 -4 -7 -0.95 8.20 16 -4 -6 299.42 25.48 16 4 -5 168.28 14.32 16 -4 -5 168.29 18.83 16 4 -4 712.28 30.49 16 -4 -4 739.38 39.25 16 4 -3 53.21 9.16 16 -4 -3 61.74 12.39 16 4 -2 500.64 25.66 16 -4 -2 498.95 31.64 16 4 -1 80.62 10.92 16 -4 -1 63.01 13.24 16 4 0 294.98 20.41 16 -4 0 327.69 25.97 16 4 1 84.81 11.73 16 -4 1 74.91 14.68 16 4 2 716.08 33.38 16 -4 2 679.93 37.59 16 4 3 4.55 6.97 16 4 4 366.40 24.69 16 6 -2 654.38 28.56 16 6 -1 130.29 13.16 16 6 0 403.66 22.90 16 6 1 113.19 12.90 16 6 2 164.99 15.93 17 -1 -10 19.75 10.33 17 -1 -9 282.43 23.21 17 -1 -8 2.80 7.13 17 1 -8 12.53 7.61 17 -1 -7 232.46 21.09 17 1 -7 222.83 19.17 17 -1 -6 1.20 7.24 17 1 -6 0.16 6.83 17 -1 -5 491.67 30.22 17 1 -5 520.33 29.49 17 -1 -4 -4.40 7.37 17 1 -4 4.02 6.67 17 -1 -3 346.35 25.61 17 1 -3 339.40 23.33 17 -1 -2 3.60 7.79 17 1 -2 10.78 7.15 17 1 -1 431.84 26.77 17 -1 -1 457.55 29.30 17 1 0 74.42 11.82 17 -1 0 79.67 13.17 17 -1 1 849.71 40.53 17 1 1 817.56 38.20 17 -1 2 -3.12 7.09 17 1 2 -3.47 8.04 17 1 3 850.96 39.75 17 -3 -6 21.36 11.03 17 -3 -5 55.31 12.39 17 3 -5 89.32 11.51 17 3 -4 38.43 8.74 17 -3 -4 10.00 8.90 17 3 -3 469.42 26.12 17 -3 -3 459.72 30.82 17 3 -2 1.79 5.87 17 -3 -2 1.00 7.54 17 3 -1 458.64 26.32 17 -3 -1 445.69 30.69 17 3 0 48.35 10.29 17 -3 0 54.69 12.84 17 3 1 530.50 29.74 17 3 2 73.91 11.95 17 3 3 1142.98 45.86 17 5 -2 196.33 16.36 17 5 -1 387.36 23.10 17 5 0 59.89 10.22 17 5 1 508.40 28.36 17 5 2 99.05 13.47 18 0 -8 207.35 19.88 18 0 -7 -17.80 10.69 18 0 -6 239.84 21.44 18 0 -5 3.34 7.33 18 0 -4 725.78 37.13 18 0 -3 -3.68 7.92 18 0 -2 683.94 35.93 18 0 -1 -4.15 7.77 18 2 -6 319.66 22.83 18 2 -5 8.35 6.58 18 2 -4 440.40 27.14 18 2 -3 60.12 11.15 18 2 -2 623.91 32.68 18 2 -1 -5.63 7.00 18 2 0 575.89 31.95 18 4 -3 12.15 7.49 18 4 -2 347.27 22.87 18 4 -1 198.43 18.01 18 4 0 583.17 30.96 18 4 1 37.76 9.46 0 0 0 0.00 0.00 TITL exp_1123_U in Cc REM Cc (#9 in standard setting) CELL 0.71073 13.859844 11.496043 12.609970 90.0000 96.4146 90.0000 ZERR 10.00 0.000734 0.000575 0.000649 0.0000 0.0050 0.0000 LATT -7 SYMM x,-y, z+1/2 SFAC C H O Cl U UNIT 60.00 60.00 20.00 20.00 10.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 12558 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.639 _oxdiff_exptl_absorpt_empirical_full_min 0.765