data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; 'selenium dicyanide difluoride 12-crown-4-solvate' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H24 F2 N2 O4 Se' _chemical_formula_weight 437.34 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' 'N' 'N' 0.0061 0.0033 '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' 'F' 'F' 0.0171 0.0103 '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' _space_group_crystal_system orthorhombic _space_group_IT_number 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' _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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.404(3) _cell_length_b 12.071(2) _cell_length_c 19.750(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3910.9(15) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1019 _cell_measurement_theta_min 4.817 _cell_measurement_theta_max 55.989 _exptl_crystal_description platelett _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_F_000 1792 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.08 _exptl_absorpt_coefficient_mu 1.962 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5923 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details 'SADABS 2008/1 (Bruker AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker AXS Smart CCD' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 50710 _diffrn_reflns_av_unetI/netI 0.0254 _diffrn_reflns_av_R_equivalents 0.0484 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.062 _diffrn_reflns_theta_max 28.329 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4839 _reflns_number_gt 3597 _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 'Smart (Bruker AXS)' _computing_cell_refinement 'Saint (Bruker AXS)' _computing_data_reduction 'Saint (Bruker AXS)' _computing_structure_solution 'SHELXS-2013 (Sheldrick, 2013)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'Ortep3v2 for Windows' _computing_publication_material 'publCIF (IUCR)' _refine_special_details ; ? ; _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^)+(0.0472P)^2^+4.7351P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4839 _refine_ls_number_parameters 236 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0952 _refine_ls_wR_factor_gt 0.0831 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.001 _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 C7C C 0.49887(17) 0.8074(3) 0.45645(18) 0.0412(8) Uani 1 1 d . . . . . H7C1 H 0.5079 0.8002 0.4071 0.049 Uiso 1 1 calc R U . . . H7C2 H 0.4508 0.8555 0.4639 0.049 Uiso 1 1 calc R U . . . C6C C 0.60468(19) 0.9434(2) 0.44924(19) 0.0433(8) Uani 1 1 d . . . . . H6C1 H 0.6406 0.9873 0.4793 0.052 Uiso 1 1 calc R U . . . H6C2 H 0.5608 0.9929 0.4328 0.052 Uiso 1 1 calc R U . . . O4 O 0.56861(11) 0.85392(18) 0.48793(11) 0.0351(5) Uani 1 1 d . . . . . N1 N 0.78194(17) 0.7370(2) 0.67272(13) 0.0417(6) Uani 1 1 d . . . . . O3 O 0.71517(11) 0.83339(17) 0.41457(10) 0.0298(4) Uani 1 1 d . . . . . N2 N 0.71193(15) 0.4463(2) 0.55408(12) 0.0319(5) Uani 1 1 d . . . . . O2 O 0.69358(12) 0.59890(17) 0.40048(9) 0.0318(4) Uani 1 1 d . . . . . F2 F 0.61059(9) 0.68527(14) 0.59565(8) 0.0321(4) Uani 1 1 d . . . . . F1 F 0.80233(8) 0.68287(12) 0.50507(8) 0.0240(3) Uani 1 1 d . . . . . Se1 Se 0.69827(2) 0.69525(2) 0.53739(2) 0.01826(8) Uani 1 1 d . . . . . C2 C 0.70504(15) 0.5398(2) 0.54790(12) 0.0231(5) Uani 1 1 d . . . . . O1 O 0.55130(11) 0.61917(17) 0.47401(10) 0.0307(4) Uani 1 1 d . . . . . C6L C 0.95764(17) 0.0333(3) 0.19308(14) 0.0322(6) Uani 1 1 d . . . . . C2C C 0.62735(18) 0.5186(2) 0.39436(15) 0.0352(7) Uani 1 1 d . . . . . H2C1 H 0.6370 0.4565 0.4261 0.042 Uiso 1 1 calc R U . . . H2C2 H 0.6268 0.4880 0.3478 0.042 Uiso 1 1 calc R U . . . C3C C 0.7020(2) 0.6685(3) 0.34336(15) 0.0429(8) Uani 1 1 d . . . . . H3C1 H 0.6476 0.6931 0.3277 0.052 Uiso 1 1 calc R U . . . H3C2 H 0.7286 0.6273 0.3060 0.052 Uiso 1 1 calc R U . . . C5C C 0.65290(19) 0.9036(3) 0.39036(18) 0.0469(9) Uani 1 1 d . . . . . H5C1 H 0.6172 0.8627 0.3586 0.056 Uiso 1 1 calc R U . . . H5C2 H 0.6770 0.9673 0.3660 0.056 Uiso 1 1 calc R U . . . C2L C 1.05071(19) -0.0588(3) 0.26855(14) 0.0404(8) Uani 1 1 d . . . . . H2L H 1.0659 -0.1232 0.2931 0.049 Uiso 1 1 calc R U . . . C1L C 0.98062(18) -0.0593(3) 0.22963(14) 0.0330(6) Uani 1 1 d . . . . . H1L H 0.9478 -0.1241 0.2280 0.040 Uiso 1 1 calc R U . . . C3L C 1.09847(19) 0.0350(3) 0.27172(14) 0.0411(8) Uani 1 1 d . . . . . H3L H 1.1462 0.0357 0.2989 0.049 Uiso 1 1 calc R U . . . C1C C 0.54614(18) 0.5702(3) 0.40942(15) 0.0358(7) Uani 1 1 d . . . . . H1C1 H 0.5329 0.6270 0.3749 0.043 Uiso 1 1 calc R U . . . H1C2 H 0.5028 0.5131 0.4088 0.043 Uiso 1 1 calc R U . . . C1 C 0.75259(17) 0.7228(2) 0.62123(13) 0.0258(5) Uani 1 1 d . . . . . C5L C 1.00696(18) 0.1268(3) 0.19619(15) 0.0360(7) Uani 1 1 d . . . . . H5L H 0.9924 0.1910 0.1711 0.043 Uiso 1 1 calc R U . . . C4C C 0.7524(2) 0.7664(3) 0.36227(14) 0.0404(7) Uani 1 1 d . . . . . H4C1 H 0.8064 0.7406 0.3782 0.049 Uiso 1 1 calc R U . . . H4C2 H 0.7613 0.8127 0.3216 0.049 Uiso 1 1 calc R U . . . C7L C 0.8813(2) 0.0338(3) 0.15112(19) 0.0467(8) Uani 1 1 d . . . . . H7L1 H 0.8362 0.0645 0.1778 0.070 Uiso 1 1 calc R U . . . H7L2 H 0.8680 -0.0421 0.1375 0.070 Uiso 1 1 calc R U . . . H7L3 H 0.8898 0.0794 0.1107 0.070 Uiso 1 1 calc R U . . . C4L C 1.07668(19) 0.1280(3) 0.23517(15) 0.0392(7) Uani 1 1 d . . . . . H4L H 1.1097 0.1926 0.2369 0.047 Uiso 1 1 calc R U . . . C8C C 0.48486(15) 0.6958(3) 0.48737(17) 0.0361(7) Uani 1 1 d . . . . . H8C1 H 0.4783 0.7042 0.5369 0.043 Uiso 1 1 calc R U . . . H8C2 H 0.4336 0.6643 0.4692 0.043 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 C7C 0.0213(13) 0.0346(17) 0.068(2) 0.0033(16) -0.0097(13) 0.0015(12) C6C 0.0348(15) 0.0225(16) 0.072(2) 0.0115(15) -0.0156(15) -0.0017(12) O4 0.0218(9) 0.0343(12) 0.0493(12) -0.0013(10) -0.0038(8) 0.0020(8) N1 0.0591(16) 0.0335(15) 0.0324(13) -0.0003(11) -0.0157(12) -0.0049(13) O3 0.0286(9) 0.0338(11) 0.0271(9) 0.0076(8) -0.0038(7) -0.0057(8) N2 0.0416(14) 0.0275(15) 0.0267(11) 0.0038(10) -0.0088(10) -0.0098(10) O2 0.0383(10) 0.0357(11) 0.0212(9) -0.0023(8) -0.0057(8) -0.0027(9) F2 0.0266(8) 0.0444(10) 0.0252(8) 0.0044(7) 0.0075(6) 0.0009(7) F1 0.0181(6) 0.0243(8) 0.0296(8) 0.0014(6) 0.0012(6) -0.0004(6) Se1 0.01794(12) 0.02074(14) 0.01609(12) 0.00291(9) -0.00050(8) 0.00023(9) C2 0.0245(12) 0.0255(14) 0.0193(11) 0.0020(10) -0.0042(9) -0.0054(10) O1 0.0275(9) 0.0320(11) 0.0326(10) 0.0022(8) -0.0084(8) -0.0056(8) C6L 0.0336(14) 0.0328(16) 0.0302(14) -0.0006(12) -0.0040(11) 0.0013(12) C2C 0.0432(16) 0.0290(16) 0.0334(15) -0.0086(12) -0.0157(12) -0.0022(13) C3C 0.055(2) 0.052(2) 0.0217(13) 0.0058(13) -0.0006(13) -0.0102(16) C5C 0.0391(17) 0.045(2) 0.057(2) 0.0293(17) -0.0134(15) -0.0102(15) C2L 0.0450(18) 0.053(2) 0.0231(13) 0.0050(13) 0.0018(12) 0.0172(16) C1L 0.0374(15) 0.0332(17) 0.0286(13) 0.0039(12) 0.0053(11) 0.0001(13) C3L 0.0347(15) 0.066(2) 0.0231(13) -0.0097(14) -0.0043(11) 0.0058(15) C1C 0.0373(15) 0.0336(17) 0.0366(15) 0.0018(13) -0.0150(12) -0.0073(13) C1 0.0333(13) 0.0183(13) 0.0257(12) -0.0020(10) -0.0051(11) 0.0003(10) C5L 0.0420(16) 0.0288(16) 0.0372(16) 0.0021(12) -0.0056(13) -0.0006(13) C4C 0.0441(16) 0.055(2) 0.0218(13) 0.0074(13) 0.0066(12) -0.0163(15) C7L 0.0425(17) 0.0395(19) 0.058(2) 0.0005(16) -0.0179(16) -0.0004(15) C4L 0.0383(16) 0.0429(19) 0.0365(16) -0.0086(14) -0.0026(12) -0.0052(14) C8C 0.0150(11) 0.0392(17) 0.0539(18) 0.0060(15) -0.0032(11) -0.0018(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 C7C O4 1.418(3) . ? C7C C8C 1.497(4) . ? C6C O4 1.449(4) . ? C6C C5C 1.486(5) . ? O4 Se1 3.024(2) . ? N1 C1 1.138(3) . ? O3 C5C 1.411(4) . ? O3 C4C 1.447(4) . ? O3 Se1 2.957(2) . ? N2 C2 1.141(4) . ? O2 C3C 1.413(4) . ? O2 C2C 1.461(3) . ? O2 Se1 2.944(2) . ? F2 Se1 1.8458(15) . ? F1 Se1 1.8285(14) . ? Se1 C2 1.892(3) . ? Se1 C1 1.910(3) . ? Se1 O1 2.8675(18) . ? O1 C1C 1.408(3) . ? O1 C8C 1.453(3) . ? C6L C1L 1.383(4) . ? C6L C5L 1.390(4) . ? C6L C7L 1.502(4) . ? C2C C1C 1.501(4) . ? C3C C4C 1.491(5) . ? C2L C3L 1.378(5) . ? C2L C1L 1.383(4) . ? C3L C4L 1.382(5) . ? C5L C4L 1.379(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 O4 C7C C8C 107.5(2) . . ? O4 C6C C5C 112.9(3) . . ? C7C O4 C6C 113.2(2) . . ? C7C O4 Se1 117.28(17) . . ? C6C O4 Se1 110.80(15) . . ? C5C O3 C4C 113.5(2) . . ? C5C O3 Se1 123.30(17) . . ? C4C O3 Se1 108.07(16) . . ? C3C O2 C2C 113.6(2) . . ? C3C O2 Se1 119.73(18) . . ? C2C O2 Se1 110.95(15) . . ? F1 Se1 F2 159.99(7) . . ? F1 Se1 C2 84.40(9) . . ? F2 Se1 C2 84.99(9) . . ? F1 Se1 C1 83.18(10) . . ? F2 Se1 C1 80.47(10) . . ? C2 Se1 C1 92.90(11) . . ? F1 Se1 O1 127.33(6) . . ? F2 Se1 O1 66.18(7) . . ? C2 Se1 O1 77.26(8) . . ? C1 Se1 O1 145.76(9) . . ? F1 Se1 O2 70.83(6) . . ? F2 Se1 O2 121.76(6) . . ? C2 Se1 O2 73.17(8) . . ? C1 Se1 O2 151.32(9) . . ? O1 Se1 O2 56.68(5) . . ? F1 Se1 O3 70.86(6) . . ? F2 Se1 O3 128.41(6) . . ? C2 Se1 O3 130.10(8) . . ? C1 Se1 O3 124.70(9) . . ? O1 Se1 O3 84.34(5) . . ? O2 Se1 O3 58.12(6) . . ? F1 Se1 O4 126.55(6) . . ? F2 Se1 O4 72.23(7) . . ? C2 Se1 O4 134.84(8) . . ? C1 Se1 O4 119.85(9) . . ? O1 Se1 O4 58.03(6) . . ? O2 Se1 O4 86.28(6) . . ? O3 Se1 O4 56.20(6) . . ? N2 C2 Se1 177.7(2) . . ? C1C O1 C8C 112.7(2) . . ? C1C O1 Se1 125.47(16) . . ? C8C O1 Se1 110.33(15) . . ? C1L C6L C5L 118.3(3) . . ? C1L C6L C7L 121.2(3) . . ? C5L C6L C7L 120.4(3) . . ? O2 C2C C1C 111.6(2) . . ? O2 C3C C4C 109.0(2) . . ? O3 C5C C6C 108.3(3) . . ? C3L C2L C1L 120.1(3) . . ? C2L C1L C6L 120.9(3) . . ? C2L C3L C4L 119.8(3) . . ? O1 C1C C2C 107.5(2) . . ? N1 C1 Se1 176.8(3) . . ? C4L C5L C6L 121.0(3) . . ? O3 C4C C3C 112.8(2) . . ? C5L C4L C3L 119.9(3) . . ? O1 C8C C7C 112.6(2) . . ? _refine_diff_density_max 0.752 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.084 _shelxl_version_number 2013-2 _shelx_res_file ; TITL sf225 in Pbca CELL 0.71073 16.4040 12.0714 19.7503 90.000 90.000 90.000 ZERR 8.00 0.0031 0.0024 0.0054 0.000 0.000 0.000 LATT 1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 + X, 1/2 - Y, - Z SFAC C H N O F SE UNIT 136 192 16 32 16 8 MERG 2 FMAP 2 PLAN 5 BIND SE1 O1 BIND SE1 O2 BIND SE1 O3 BIND SE1 O4 ACTA BOND L.S. 20 TEMP -173.00 WGHT 0.047200 4.735100 FVAR 0.07682 MOLE 1 C7C 1 0.498869 0.807414 0.456445 11.00000 0.02131 0.03458 = 0.06758 0.00330 -0.00965 0.00150 AFIX 23 H7C1 2 0.507944 0.800183 0.407087 11.00000 -1.20000 H7C2 2 0.450813 0.855518 0.463863 11.00000 -1.20000 AFIX 0 C6C 1 0.604683 0.943381 0.449239 11.00000 0.03485 0.02253 = 0.07247 0.01149 -0.01558 -0.00171 AFIX 23 H6C1 2 0.640577 0.987290 0.479299 11.00000 -1.20000 H6C2 2 0.560812 0.992886 0.432828 11.00000 -1.20000 AFIX 0 O4 4 0.568613 0.853919 0.487926 11.00000 0.02176 0.03433 = 0.04932 -0.00127 -0.00378 0.00203 N1 3 0.781939 0.737013 0.672725 11.00000 0.05906 0.03352 = 0.03238 -0.00026 -0.01572 -0.00493 O3 4 0.715174 0.833385 0.414574 11.00000 0.02861 0.03383 = 0.02706 0.00758 -0.00381 -0.00571 N2 3 0.711926 0.446267 0.554079 11.00000 0.04159 0.02746 = 0.02669 0.00377 -0.00877 -0.00978 O2 4 0.693578 0.598904 0.400482 11.00000 0.03834 0.03568 = 0.02123 -0.00226 -0.00569 -0.00275 F2 5 0.610591 0.685272 0.595650 11.00000 0.02664 0.04441 = 0.02523 0.00444 0.00754 0.00086 F1 5 0.802326 0.682874 0.505074 11.00000 0.01812 0.02433 = 0.02955 0.00139 0.00116 -0.00044 SE1 6 0.698267 0.695249 0.537389 11.00000 0.01794 0.02074 = 0.01609 0.00291 -0.00050 0.00023 C2 1 0.705038 0.539771 0.547899 11.00000 0.02447 0.02549 = 0.01935 0.00201 -0.00424 -0.00542 O1 4 0.551296 0.619170 0.474009 11.00000 0.02749 0.03199 = 0.03261 0.00216 -0.00836 -0.00564 C6L 1 0.957636 0.033328 0.193085 11.00000 0.03364 0.03281 = 0.03021 -0.00057 -0.00397 0.00132 C2C 1 0.627348 0.518563 0.394355 11.00000 0.04322 0.02897 = 0.03344 -0.00857 -0.01569 -0.00218 AFIX 23 H2C1 2 0.637000 0.456521 0.426142 11.00000 -1.20000 H2C2 2 0.626802 0.488032 0.347834 11.00000 -1.20000 AFIX 0 C3C 1 0.702022 0.668453 0.343361 11.00000 0.05502 0.05215 = 0.02168 0.00581 -0.00059 -0.01019 AFIX 23 H3C1 2 0.647646 0.693088 0.327669 11.00000 -1.20000 H3C2 2 0.728585 0.627341 0.306018 11.00000 -1.20000 AFIX 0 C5C 1 0.652901 0.903627 0.390357 11.00000 0.03907 0.04465 = 0.05683 0.02925 -0.01340 -0.01021 AFIX 23 H5C1 2 0.617238 0.862686 0.358592 11.00000 -1.20000 H5C2 2 0.677009 0.967342 0.365961 11.00000 -1.20000 AFIX 0 C2L 1 1.050708 -0.058798 0.268546 11.00000 0.04500 0.05315 = 0.02312 0.00504 0.00185 0.01721 AFIX 43 H2L 2 1.065950 -0.123204 0.293118 11.00000 -1.20000 AFIX 0 C1L 1 0.980617 -0.059252 0.229632 11.00000 0.03736 0.03318 = 0.02856 0.00393 0.00532 0.00009 AFIX 43 H1L 2 0.947811 -0.124051 0.227987 11.00000 -1.20000 AFIX 0 C3L 1 1.098467 0.034989 0.271716 11.00000 0.03474 0.06554 = 0.02314 -0.00970 -0.00430 0.00584 AFIX 43 H3L 2 1.146210 0.035685 0.298938 11.00000 -1.20000 AFIX 0 C1C 1 0.546137 0.570225 0.409418 11.00000 0.03731 0.03362 = 0.03660 0.00184 -0.01497 -0.00730 AFIX 23 H1C1 2 0.532941 0.627007 0.374950 11.00000 -1.20000 H1C2 2 0.502822 0.513125 0.408846 11.00000 -1.20000 AFIX 0 C1 1 0.752593 0.722846 0.621231 11.00000 0.03329 0.01826 = 0.02572 -0.00202 -0.00507 0.00025 C5L 1 1.006963 0.126848 0.196193 11.00000 0.04203 0.02883 = 0.03725 0.00205 -0.00563 -0.00063 AFIX 43 H5L 2 0.992396 0.190964 0.171061 11.00000 -1.20000 AFIX 0 C4C 1 0.752440 0.766404 0.362269 11.00000 0.04413 0.05536 = 0.02178 0.00744 0.00661 -0.01633 AFIX 23 H4C1 2 0.806390 0.740570 0.378249 11.00000 -1.20000 H4C2 2 0.761291 0.812729 0.321564 11.00000 -1.20000 AFIX 0 C7L 1 0.881266 0.033838 0.151121 11.00000 0.04253 0.03947 = 0.05812 0.00053 -0.01786 -0.00044 AFIX 137 H7L1 2 0.836243 0.064517 0.177807 11.00000 -1.50000 H7L2 2 0.867964 -0.042105 0.137500 11.00000 -1.50000 H7L3 2 0.889767 0.079435 0.110679 11.00000 -1.50000 AFIX 0 C4L 1 1.076683 0.128014 0.235170 11.00000 0.03830 0.04289 = 0.03653 -0.00860 -0.00261 -0.00523 AFIX 43 H4L 2 1.109678 0.192628 0.236900 11.00000 -1.20000 AFIX 0 C8C 1 0.484864 0.695774 0.487369 11.00000 0.01497 0.03925 = 0.05393 0.00603 -0.00321 -0.00179 AFIX 23 H8C1 2 0.478287 0.704250 0.536927 11.00000 -1.20000 H8C2 2 0.433613 0.664348 0.469157 11.00000 -1.20000 AFIX 0 HKLF 4 REM sf225 in Pbca REM R1 = 0.0356 for 3597 Fo > 4sig(Fo) and 0.0577 for all 4839 data REM 236 parameters refined using 0 restraints END WGHT 0.0395 5.3229 REM Highest difference peak 0.752, deepest hole -0.457, 1-sigma level 0.084 Q1 1 0.6553 0.5662 0.3557 11.00000 0.05 0.75 Q2 1 0.7462 0.6778 0.5300 11.00000 0.05 0.73 Q3 1 0.7507 0.6986 0.3561 11.00000 0.05 0.66 Q4 1 0.5746 0.5578 0.4609 11.00000 0.05 0.63 Q5 1 0.5429 0.7959 0.4887 11.00000 0.05 0.55 ; _shelx_res_checksum 70424 _shelx_hkl_file ; 0 1 0 -0.04 0.03 0 -1 0 -0.14 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