data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; 'selenium dicyanide 18-crown-6 adduct' ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13.33 H24 F0 N1.33 O6 Se0.67' _chemical_formula_weight 351.64 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 monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.766(4) _cell_length_b 9.834(3) _cell_length_c 18.608(5) _cell_angle_alpha 90 _cell_angle_beta 112.511(5) _cell_angle_gamma 90 _cell_volume 2496.2(11) _cell_formula_units_Z 6 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 4.730 _cell_measurement_theta_max 50.015 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_F_000 1104 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.18 _exptl_absorpt_coefficient_mu 1.553 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4996 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_process_details 'SADABS-2008/1 (Bruker-AXS)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(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 25644 _diffrn_reflns_av_unetI/netI 0.0415 _diffrn_reflns_av_R_equivalents 0.0631 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.233 _diffrn_reflns_theta_max 25.078 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.982 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 0.982 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 0.982 _reflns_number_total 4444 _reflns_number_gt 3817 _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^)+(0.0605P)^2^+5.2754P] 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 4444 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1211 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 Se1 Se 0.00011(2) 0.36871(3) 0.77989(2) 0.02259(13) Uani 1 1 d . . . . . O3 O 0.91843(16) 0.1788(2) 0.64092(12) 0.0203(5) Uani 1 1 d . . . . . O5 O 0.78553(17) 0.5262(2) 0.75618(13) 0.0238(5) Uani 1 1 d . . . . . O8 O 0.11409(19) 0.5325(3) 0.62796(16) 0.0346(6) Uani 1 1 d . . . . . N1 N 0.0202(3) 0.6715(3) 0.7901(2) 0.0383(8) Uani 1 1 d . . . . . O2 O 1.02373(17) 0.0792(2) 0.79813(12) 0.0214(5) Uani 1 1 d . . . . . O7 O 0.20220(19) 0.3234(3) 0.57732(15) 0.0326(6) Uani 1 1 d . . . . . O4 O 0.84145(17) 0.4471(2) 0.63324(12) 0.0216(5) Uani 1 1 d . . . . . O6 O 0.89631(17) 0.4453(2) 0.91330(13) 0.0221(5) Uani 1 1 d . . . . . O9 O -0.04267(19) 0.8191(3) 0.55205(16) 0.0324(6) Uani 1 1 d . . . . . O1 O 0.97265(16) 0.1720(2) 0.92547(12) 0.0210(5) Uani 1 1 d . . . . . C6 C 0.8312(3) 0.3659(3) 0.56666(19) 0.0248(7) Uani 1 1 d . . . . . H6A H 0.8245 0.4256 0.5221 0.030 Uiso 1 1 calc R U . . . H6B H 0.7715 0.3092 0.5522 0.030 Uiso 1 1 calc R U . . . C14 C 0.2311(3) 0.3571(4) 0.6572(2) 0.0321(8) Uani 1 1 d . . . . . H14A H 0.3009 0.3338 0.6859 0.039 Uiso 1 1 calc R U . . . H14B H 0.1913 0.3055 0.6803 0.039 Uiso 1 1 calc R U . . . C1N C 0.0121(3) 0.5582(4) 0.78609(19) 0.0251(8) Uani 1 1 d . . . . . C11 C 0.9118(3) 0.3553(3) 0.97680(19) 0.0224(7) Uani 1 1 d . . . . . H11A H 0.8529 0.2981 0.9662 0.027 Uiso 1 1 calc R U . . . H11B H 0.9233 0.4083 1.0248 0.027 Uiso 1 1 calc R U . . . C18 C -0.1445(3) 0.8459(4) 0.5221(2) 0.0337(9) Uani 1 1 d . . . . . H18A H -0.1547 0.9422 0.5325 0.040 Uiso 1 1 calc R U . . . H18B H -0.1753 0.7889 0.5503 0.040 Uiso 1 1 calc R U . . . C3 C 1.0006(3) 0.0026(3) 0.72803(19) 0.0227(7) Uani 1 1 d . . . . . H3A H 0.9347 -0.0385 0.7129 0.027 Uiso 1 1 calc R U . . . H3B H 1.0488 -0.0716 0.7364 0.027 Uiso 1 1 calc R U . . . C2N C 0.1236(3) 0.3554(3) 0.8595(2) 0.0259(8) Uani 1 1 d . . . . . C17 C -0.0176(3) 0.6786(3) 0.5697(2) 0.0271(8) Uani 1 1 d . . . . . H17A H -0.0307 0.6266 0.5212 0.033 Uiso 1 1 calc R U . . . H17B H -0.0571 0.6390 0.5971 0.033 Uiso 1 1 calc R U . . . C4 C 1.0028(2) 0.0944(3) 0.66511(19) 0.0223(7) Uani 1 1 d . . . . . H4A H 1.0627 0.1511 0.6845 0.027 Uiso 1 1 calc R U . . . H4B H 1.0035 0.0400 0.6206 0.027 Uiso 1 1 calc R U . . . C8 C 0.7662(3) 0.6088(3) 0.68921(19) 0.0243(7) Uani 1 1 d . . . . . H8A H 0.8217 0.6716 0.6975 0.029 Uiso 1 1 calc R U . . . H8B H 0.7063 0.6636 0.6791 0.029 Uiso 1 1 calc R U . . . C15 C 0.2158(3) 0.5065(4) 0.6628(2) 0.0333(9) Uani 1 1 d . . . . . H15A H 0.2416 0.5352 0.7180 0.040 Uiso 1 1 calc R U . . . H15B H 0.2508 0.5579 0.6356 0.040 Uiso 1 1 calc R U . . . C10 C 0.8029(3) 0.5089(4) 0.8876(2) 0.0236(7) Uani 1 1 d . . . . . H10A H 0.7959 0.5595 0.9312 0.028 Uiso 1 1 calc R U . . . H10B H 0.7508 0.4389 0.8698 0.028 Uiso 1 1 calc R U . . . N2 N 0.1994(3) 0.3468(3) 0.9080(2) 0.0386(8) Uani 1 1 d . . . . . C9 C 0.7920(3) 0.6041(3) 0.8224(2) 0.0241(7) Uani 1 1 d . . . . . H9A H 0.7322 0.6598 0.8102 0.029 Uiso 1 1 calc R U . . . H9B H 0.8492 0.6659 0.8374 0.029 Uiso 1 1 calc R U . . . C7 C 0.7524(3) 0.5174(4) 0.62135(19) 0.0252(7) Uani 1 1 d . . . . . H7A H 0.6996 0.4510 0.6154 0.030 Uiso 1 1 calc R U . . . H7B H 0.7327 0.5721 0.5731 0.030 Uiso 1 1 calc R U . . . C2 C 1.0215(3) -0.0033(3) 0.86022(19) 0.0225(7) Uani 1 1 d . . . . . H2A H 1.0676 -0.0803 0.8687 0.027 Uiso 1 1 calc R U . . . H2B H 0.9548 -0.0408 0.8468 0.027 Uiso 1 1 calc R U . . . C12 C 0.9985(3) 0.2670(3) 0.98788(18) 0.0223(7) Uani 1 1 d . . . . . H12A H 1.0543 0.3235 0.9886 0.027 Uiso 1 1 calc R U . . . H12B H 1.0184 0.2182 1.0381 0.027 Uiso 1 1 calc R U . . . C5 C 0.9191(3) 0.2770(3) 0.58489(19) 0.0250(7) Uani 1 1 d . . . . . H5A H 0.9174 0.2309 0.5371 0.030 Uiso 1 1 calc R U . . . H5B H 0.9797 0.3323 0.6059 0.030 Uiso 1 1 calc R U . . . C1 C 1.0497(2) 0.0798(3) 0.93258(18) 0.0215(7) Uani 1 1 d . . . . . H1A H 1.0620 0.0196 0.9780 0.026 Uiso 1 1 calc R U . . . H1B H 1.1107 0.1308 0.9408 0.026 Uiso 1 1 calc R U . . . C13 C 0.1956(3) 0.1803(4) 0.5638(2) 0.0348(9) Uani 1 1 d . . . . . H13A H 0.1584 0.1375 0.5922 0.042 Uiso 1 1 calc R U . . . H13B H 0.2621 0.1400 0.5830 0.042 Uiso 1 1 calc R U . . . C16 C 0.0894(3) 0.6723(4) 0.6206(2) 0.0271(8) Uani 1 1 d . . . . . H16A H 0.1286 0.7223 0.5964 0.033 Uiso 1 1 calc R U . . . H16B H 0.1015 0.7128 0.6722 0.033 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 Se1 0.0257(2) 0.0175(2) 0.02066(19) 0.00052(13) 0.00448(14) -0.00168(13) O3 0.0252(13) 0.0187(11) 0.0167(11) 0.0016(9) 0.0078(10) 0.0004(9) O5 0.0302(14) 0.0200(12) 0.0171(11) 0.0006(9) 0.0042(10) 0.0029(10) O8 0.0264(14) 0.0234(13) 0.0473(16) -0.0021(12) 0.0067(12) -0.0018(10) N1 0.042(2) 0.0230(18) 0.042(2) 0.0004(14) 0.0062(16) 0.0000(14) O2 0.0324(13) 0.0138(11) 0.0154(11) 0.0002(9) 0.0064(10) -0.0031(10) O7 0.0345(15) 0.0244(13) 0.0335(14) -0.0003(11) 0.0070(12) 0.0006(11) O4 0.0251(13) 0.0201(12) 0.0141(11) 0.0002(9) 0.0012(9) 0.0021(9) O6 0.0257(13) 0.0217(12) 0.0191(11) 0.0016(9) 0.0088(10) 0.0013(10) O9 0.0310(14) 0.0227(13) 0.0446(16) -0.0041(12) 0.0157(12) 0.0001(11) O1 0.0229(12) 0.0185(11) 0.0156(11) -0.0038(9) 0.0007(9) -0.0001(9) C6 0.034(2) 0.0226(17) 0.0117(15) 0.0004(13) 0.0025(14) -0.0028(14) C14 0.027(2) 0.032(2) 0.032(2) 0.0003(16) 0.0047(16) -0.0009(15) C1N 0.0277(19) 0.0177(19) 0.0244(18) 0.0023(14) 0.0037(15) -0.0016(14) C11 0.0309(19) 0.0187(16) 0.0189(16) -0.0027(13) 0.0113(15) -0.0047(14) C18 0.030(2) 0.0268(19) 0.048(2) -0.0075(17) 0.0194(18) 0.0034(15) C3 0.0280(19) 0.0141(15) 0.0224(17) -0.0040(13) 0.0058(14) 0.0023(13) C2N 0.025(2) 0.0213(17) 0.0246(18) 0.0036(14) 0.0024(16) -0.0019(14) C17 0.033(2) 0.0201(17) 0.0309(19) -0.0048(15) 0.0149(16) -0.0019(15) C4 0.0226(18) 0.0243(17) 0.0190(16) -0.0054(14) 0.0068(14) -0.0002(14) C8 0.0267(19) 0.0211(17) 0.0191(16) 0.0052(13) 0.0020(14) 0.0047(14) C15 0.026(2) 0.032(2) 0.034(2) -0.0059(16) 0.0030(16) -0.0031(16) C10 0.0227(18) 0.0250(17) 0.0238(17) -0.0055(14) 0.0095(14) 0.0003(14) N2 0.038(2) 0.0284(17) 0.0390(19) 0.0039(14) 0.0026(17) -0.0014(14) C9 0.0254(19) 0.0211(17) 0.0245(17) -0.0037(14) 0.0083(15) 0.0039(14) C7 0.0253(19) 0.0249(18) 0.0191(16) 0.0048(14) 0.0014(14) 0.0036(14) C2 0.0292(19) 0.0137(15) 0.0242(17) 0.0051(13) 0.0099(15) 0.0026(13) C12 0.0307(19) 0.0185(16) 0.0140(15) -0.0024(12) 0.0043(14) -0.0063(14) C5 0.036(2) 0.0233(17) 0.0163(16) 0.0003(13) 0.0109(15) -0.0044(15) C1 0.0229(18) 0.0202(16) 0.0183(16) 0.0066(13) 0.0044(14) 0.0027(13) C13 0.034(2) 0.0243(19) 0.046(2) -0.0001(17) 0.0153(18) 0.0044(16) C16 0.035(2) 0.0242(18) 0.0246(18) -0.0045(14) 0.0140(16) -0.0031(15) _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 Se1 C2N 1.863(4) . ? Se1 C1N 1.871(4) . ? O3 C4 1.418(4) . ? O3 C5 1.424(4) . ? O5 C8 1.422(4) . ? O5 C9 1.423(4) . ? O8 C15 1.412(5) . ? O8 C16 1.416(4) . ? N1 C1N 1.121(5) . ? O2 C2 1.422(4) . ? O2 C3 1.430(4) . ? O7 C14 1.421(5) . ? O7 C13 1.426(5) . ? O4 C7 1.426(4) . ? O4 C6 1.432(4) . ? O6 C10 1.420(4) . ? O6 C11 1.423(4) . ? O9 C18 1.414(5) . ? O9 C17 1.435(4) . ? O1 C1 1.421(4) . ? O1 C12 1.424(4) . ? C6 C5 1.493(5) . ? C14 C15 1.496(5) . ? C11 C12 1.494(5) . ? C18 C13 1.504(6) 3_566 ? C3 C4 1.489(5) . ? C2N N2 1.140(5) . ? C17 C16 1.500(5) . ? C8 C7 1.499(5) . ? C10 C9 1.492(5) . ? C2 C1 1.492(5) . ? C13 C18 1.504(6) 3_566 ? 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 C2N Se1 C1N 88.88(15) . . ? C4 O3 C5 112.2(3) . . ? C8 O5 C9 112.1(2) . . ? C15 O8 C16 114.2(3) . . ? C2 O2 C3 111.6(2) . . ? C14 O7 C13 112.9(3) . . ? C7 O4 C6 110.5(2) . . ? C10 O6 C11 112.3(2) . . ? C18 O9 C17 114.4(3) . . ? C1 O1 C12 112.8(2) . . ? O4 C6 C5 109.6(3) . . ? O7 C14 C15 108.0(3) . . ? N1 C1N Se1 179.3(4) . . ? O6 C11 C12 109.4(3) . . ? O9 C18 C13 114.3(3) . 3_566 ? O2 C3 C4 109.2(3) . . ? N2 C2N Se1 179.6(4) . . ? O9 C17 C16 107.5(3) . . ? O3 C4 C3 108.9(3) . . ? O5 C8 C7 108.2(3) . . ? O8 C15 C14 108.0(3) . . ? O6 C10 C9 109.8(3) . . ? O5 C9 C10 108.5(3) . . ? O4 C7 C8 109.9(3) . . ? O2 C2 C1 109.6(3) . . ? O1 C12 C11 108.7(3) . . ? O3 C5 C6 108.3(3) . . ? O1 C1 C2 109.2(3) . . ? O7 C13 C18 109.2(3) . 3_566 ? O8 C16 C17 105.7(3) . . ? _refine_diff_density_max 2.470 _refine_diff_density_min -0.664 _refine_diff_density_rms 0.096 _shelxl_version_number 2013-2 _shelx_res_file ; TITL sf131a in P2(1)/n CELL 0.71073 14.7662 9.8344 18.6076 90.000 112.511 90.000 ZERR 6.00 0.0037 0.0025 0.0048 0.000 0.005 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O F SE UNIT 80 144 8 36 0 4 MERG 2 FMAP 2 PLAN 3 ACTA BOND L.S. 10 TEMP -140.00 WGHT 0.060500 5.275400 FVAR 0.10667 SE1 6 0.000112 0.368712 0.779889 11.00000 0.02571 0.01746 = 0.02066 0.00052 0.00448 -0.00168 O3 4 0.918427 0.178792 0.640921 11.00000 0.02521 0.01872 = 0.01674 0.00164 0.00778 0.00038 O5 4 0.785528 0.526172 0.756181 11.00000 0.03015 0.01997 = 0.01706 0.00061 0.00423 0.00290 O8 4 0.114093 0.532503 0.627959 11.00000 0.02643 0.02345 = 0.04734 -0.00208 0.00671 -0.00185 N1 3 0.020165 0.671521 0.790123 11.00000 0.04154 0.02302 = 0.04161 0.00040 0.00615 0.00003 O2 4 1.023725 0.079215 0.798130 11.00000 0.03240 0.01384 = 0.01545 0.00020 0.00637 -0.00311 O7 4 0.202204 0.323351 0.577320 11.00000 0.03453 0.02440 = 0.03355 -0.00033 0.00697 0.00064 O4 4 0.841451 0.447126 0.633242 11.00000 0.02506 0.02009 = 0.01409 0.00018 0.00121 0.00212 O6 4 0.896306 0.445337 0.913300 11.00000 0.02567 0.02168 = 0.01906 0.00163 0.00884 0.00131 O9 4 -0.042670 0.819064 0.552048 11.00000 0.03105 0.02270 = 0.04462 -0.00406 0.01572 0.00012 O1 4 0.972649 0.171970 0.925475 11.00000 0.02290 0.01847 = 0.01558 -0.00377 0.00066 -0.00013 C6 1 0.831242 0.365938 0.566662 11.00000 0.03449 0.02256 = 0.01170 0.00037 0.00253 -0.00285 AFIX 23 H6A 2 0.824494 0.425646 0.522064 11.00000 -1.20000 H6B 2 0.771509 0.309179 0.552154 11.00000 -1.20000 AFIX 0 C14 1 0.231058 0.357126 0.657243 11.00000 0.02668 0.03207 = 0.03170 0.00035 0.00469 -0.00089 AFIX 23 H14A 2 0.300924 0.333840 0.685947 11.00000 -1.20000 H14B 2 0.191280 0.305455 0.680293 11.00000 -1.20000 AFIX 0 C1N 1 0.012053 0.558169 0.786086 11.00000 0.02767 0.01773 = 0.02443 0.00229 0.00370 -0.00157 C11 1 0.911782 0.355296 0.976803 11.00000 0.03093 0.01874 = 0.01894 -0.00269 0.01128 -0.00474 AFIX 23 H11A 2 0.852883 0.298127 0.966217 11.00000 -1.20000 H11B 2 0.923321 0.408252 1.024758 11.00000 -1.20000 AFIX 0 C18 1 -0.144512 0.845931 0.522056 11.00000 0.03032 0.02679 = 0.04800 -0.00750 0.01937 0.00340 AFIX 23 H18A 2 -0.154732 0.942241 0.532501 11.00000 -1.20000 H18B 2 -0.175343 0.788887 0.550250 11.00000 -1.20000 AFIX 0 C3 1 1.000565 0.002610 0.728033 11.00000 0.02803 0.01411 = 0.02243 -0.00402 0.00584 0.00227 AFIX 23 H3A 2 0.934652 -0.038473 0.712946 11.00000 -1.20000 H3B 2 1.048798 -0.071648 0.736353 11.00000 -1.20000 AFIX 0 C2N 1 0.123613 0.355396 0.859527 11.00000 0.02546 0.02128 = 0.02459 0.00364 0.00242 -0.00193 C17 1 -0.017591 0.678614 0.569732 11.00000 0.03275 0.02010 = 0.03091 -0.00485 0.01487 -0.00193 AFIX 23 H17A 2 -0.030735 0.626553 0.521233 11.00000 -1.20000 H17B 2 -0.057140 0.639005 0.597109 11.00000 -1.20000 AFIX 0 C4 1 1.002752 0.094443 0.665109 11.00000 0.02257 0.02433 = 0.01905 -0.00542 0.00681 -0.00018 AFIX 23 H4A 2 1.062720 0.151099 0.684495 11.00000 -1.20000 H4B 2 1.003507 0.039998 0.620591 11.00000 -1.20000 AFIX 0 C8 1 0.766173 0.608768 0.689210 11.00000 0.02675 0.02107 = 0.01906 0.00516 0.00201 0.00465 AFIX 23 H8A 2 0.821687 0.671556 0.697519 11.00000 -1.20000 H8B 2 0.706313 0.663595 0.679104 11.00000 -1.20000 AFIX 0 C15 1 0.215758 0.506492 0.662815 11.00000 0.02605 0.03241 = 0.03391 -0.00589 0.00304 -0.00312 AFIX 23 H15A 2 0.241552 0.535225 0.718007 11.00000 -1.20000 H15B 2 0.250758 0.557915 0.635585 11.00000 -1.20000 AFIX 0 C10 1 0.802883 0.508854 0.887584 11.00000 0.02266 0.02502 = 0.02377 -0.00554 0.00947 0.00033 AFIX 23 H10A 2 0.795944 0.559548 0.931159 11.00000 -1.20000 H10B 2 0.750773 0.438880 0.869837 11.00000 -1.20000 AFIX 0 N2 3 0.199411 0.346793 0.907955 11.00000 0.03751 0.02843 = 0.03896 0.00387 0.00263 -0.00142 C9 1 0.792033 0.604067 0.822397 11.00000 0.02539 0.02114 = 0.02453 -0.00366 0.00825 0.00386 AFIX 23 H9A 2 0.732166 0.659816 0.810238 11.00000 -1.20000 H9B 2 0.849224 0.665878 0.837379 11.00000 -1.20000 AFIX 0 C7 1 0.752366 0.517423 0.621353 11.00000 0.02534 0.02493 = 0.01910 0.00476 0.00144 0.00357 AFIX 23 H7A 2 0.699617 0.450977 0.615429 11.00000 -1.20000 H7B 2 0.732675 0.572073 0.573086 11.00000 -1.20000 AFIX 0 C2 1 1.021527 -0.003305 0.860216 11.00000 0.02919 0.01372 = 0.02417 0.00512 0.00988 0.00256 AFIX 23 H2A 2 1.067644 -0.080329 0.868704 11.00000 -1.20000 H2B 2 0.954824 -0.040777 0.846830 11.00000 -1.20000 AFIX 0 C12 1 0.998488 0.267026 0.987880 11.00000 0.03071 0.01849 = 0.01397 -0.00245 0.00432 -0.00627 AFIX 23 H12A 2 1.054333 0.323503 0.988610 11.00000 -1.20000 H12B 2 1.018394 0.218178 1.038100 11.00000 -1.20000 AFIX 0 C5 1 0.919137 0.276971 0.584890 11.00000 0.03620 0.02332 = 0.01629 0.00030 0.01088 -0.00440 AFIX 23 H5A 2 0.917354 0.230879 0.537067 11.00000 -1.20000 H5B 2 0.979662 0.332303 0.605871 11.00000 -1.20000 AFIX 0 C1 1 1.049716 0.079777 0.932580 11.00000 0.02286 0.02016 = 0.01833 0.00662 0.00441 0.00275 AFIX 23 H1A 2 1.061985 0.019563 0.977985 11.00000 -1.20000 H1B 2 1.110665 0.130803 0.940752 11.00000 -1.20000 AFIX 0 C13 1 0.195559 0.180285 0.563767 11.00000 0.03450 0.02426 = 0.04559 -0.00008 0.01526 0.00444 AFIX 23 H13A 2 0.158380 0.137527 0.592183 11.00000 -1.20000 H13B 2 0.262059 0.140012 0.582976 11.00000 -1.20000 AFIX 0 C16 1 0.089356 0.672338 0.620575 11.00000 0.03498 0.02417 = 0.02458 -0.00453 0.01401 -0.00313 AFIX 23 H16A 2 0.128643 0.722280 0.596393 11.00000 -1.20000 H16B 2 0.101530 0.712769 0.672174 11.00000 -1.20000 AFIX 0 HKLF 4 REM sf131a in P2(1)/n REM R1 = 0.0445 for 3817 Fo > 4sig(Fo) and 0.0540 for all 4444 data REM 289 parameters refined using 0 restraints END WGHT 0.0605 5.2756 REM Highest difference peak 2.470, deepest hole -0.664, 1-sigma level 0.096 Q1 1 -0.0024 0.4521 0.7968 11.00000 0.05 2.47 Q2 1 -0.0636 0.3621 0.7905 11.00000 0.05 1.08 Q3 1 0.0609 0.3742 0.7678 11.00000 0.05 1.05 ; _shelx_res_checksum 79054 _shelx_hkl_file ; 1 0 0 -0.66 0.02 1 0 0 -0.60 0.03 2 0 0 386.72 33.33 2 0 0 456.06 29.35 3 0 0 -0.23 0.13 3 0 0 -0.19 0.05 3 0 0 -0.05 0.08 4 0 0 836.76 53.91 4 0 0 716.20 61.25 5 0 0 -0.24 0.13 5 0 0 -0.13 0.22 6 0 0 177.46 11.48 6 0 0 152.21 13.06 7 0 0 0.04 0.17 7 0 0 0.13 0.29 8 0 0 126.20 7.94 8 0 0 100.51 9.04 9 0 0 -0.12 0.39 9 0 0 0.37 0.25 10 0 0 163.73 11.79 10 0 0 174.32 13.44 11 0 0 0.44 0.35 11 0 0 -0.16 0.47 12 0 0 33.85 2.35 12 0 0 29.43 2.72 13 0 0 0.38 0.59 13 0 0 -0.55 0.40 14 0 0 30.52 2.74 14 0 0 31.95 2.34 15 0 0 -0.31 0.68 15 0 0 0.02 0.53 16 0 0 5.49 0.98 16 0 0 5.32 0.76 0 -1 0 0.01 0.04 0 -1 0 0.08 0.03 0 1 0 0.04 0.05 0 1 0 -0.02 0.04 1 -1 0 138.17 10.61 1 -1 0 147.65 8.83 1 1 0 146.60 10.62 1 1 0 130.38 8.84 -1 1 0 133.49 9.25 1 1 0 126.70 9.34 1 1 0 116.56 9.24 2 -1 0 0.42 0.11 2 -1 0 0.45 0.08 2 -1 0 0.62 0.09 -2 1 0 0.57 0.09 2 1 0 0.78 0.12 2 1 0 0.36 0.06 2 1 0 0.54 0.08 3 -1 0 177.15 12.32 3 -1 0 184.91 14.81 3 -1 0 170.33 13.03 -3 -1 0 208.18 12.91 3 1 0 199.31 13.03 3 1 0 185.64 14.81 -3 1 0 186.82 12.90 4 -1 0 121.95 8.47 4 -1 0 107.69 8.00 4 -1 0 119.75 9.63 4 1 0 133.47 8.46 -4 1 0 120.11 8.38 4 1 0 126.94 9.64 5 -1 0 66.32 4.23 5 -1 0 62.32 4.82 5 -1 0 57.27 3.98 -5 1 0 58.52 4.17 5 1 0 51.40 4.81 5 1 0 66.34 4.22 6 -1 0 49.14 3.22 6 -1 0 42.36 3.68 6 -1 0 43.19 3.02 6 1 0 50.78 3.21 -6 1 0 44.72 3.16 6 1 0 43.45 3.68 7 -1 0 0.38 0.20 7 -1 0 0.15 0.28 7 -1 0 0.31 0.13 7 1 0 0.32 0.30 7 1 0 0.18 0.18 -7 1 0 0.46 0.14 8 -1 0 1.33 0.25 8 -1 0 1.12 0.37 -8 1 0 0.96 0.18 8 1 0 1.19 0.25 8 1 0 0.98 0.39 9 -1 0 117.12 8.08 9 -1 0 113.49 7.61 9 -1 0 108.29 9.21 9 1 0 121.62 9.22 9 1 0 117.17 8.07 10 -1 0 12.29 1.27 10 -1 0 12.57 0.91 10 -1 0 12.78 1.02 10 1 0 12.56 1.25 10 1 0 13.28 1.02 11 -1 0 18.81 1.48 11 -1 0 18.76 1.76 11 1 0 19.37 1.77 11 1 0 19.54 1.46 12 -1 0 1.83 0.44 12 1 0 1.52 0.57 12 1 0 0.98 0.39 13 -1 0 13.23 1.09 13 -1 0 10.71 1.32 13 1 0 13.35 1.07 13 1 0 9.97 1.29 14 -1 0 9.70 1.20 14 -1 0 10.24 1.04 14 1 0 10.39 1.19 14 1 0 11.53 1.01 15 -1 0 3.86 0.68 15 -1 0 2.42 0.79 15 1 0 5.48 0.68 15 1 0 4.01 0.86 16 -1 0 0.66 0.58 16 -1 0 0.02 0.76 16 1 0 -0.48 0.69 0 -2 0 45.27 3.83 0 -2 0 44.78 3.38 0 2 0 52.84 3.35 0 2 0 49.65 3.20 1 -2 0 3.67 0.31 1 -2 0 3.35 0.36 1 2 0 3.60 0.30 1 2 0 4.02 0.32 -1 2 0 3.82 0.33 1 2 0 3.35 0.30 1 2 0 3.45 0.34 2 -2 0 48.71 3.99 2 -2 0 56.41 3.33 2 2 0 44.33 3.47 2 2 0 52.23 3.99 2 2 0 49.72 3.50 2 2 0 47.66 3.32 -2 2 0 52.24 3.48 3 -2 0 216.66 16.55 3 -2 0 219.98 13.78 3 -2 0 229.69 14.57 -3 -2 0 206.46 14.42 3 2 0 209.98 14.56 3 2 0 201.12 16.55 3 2 0 202.24 13.77 -3 2 0 189.71 14.42 -4 -2 0 9.19 0.64 4 -2 0 9.46 0.63 4 -2 0 9.09 0.78 4 -2 0 8.88 0.68 4 2 0 9.05 0.78 4 2 0 6.94 0.60 4 2 0 8.26 0.64 -4 2 0 9.24 0.66 5 -2 0 12.44 0.90 5 -2 0 13.36 1.12 5 -2 0 13.84 0.97 -5 -2 0 12.70 0.92 5 2 0 14.17 1.12 5 2 0 11.75 0.94 -5 2 0 12.85 0.94 6 -2 0 0.27 0.26 -6 -2 0 0.05 0.12 6 -2 0 -0.11 0.17 6 -2 0 -0.04 0.14 -6 2 0 0.02 0.15 6 2 0 -0.04 0.16 6 2 0 -0.09 0.24 7 -2 0 4.27 0.43 7 -2 0 5.36 0.65 7 -2 0 5.70 0.50 -7 2 0 5.63 0.46 7 2 0 4.92 0.48 7 2 0 5.92 0.66 8 -2 0 12.73 0.98 8 -2 0 13.84 1.07 8 -2 0 13.26 1.27 8 2 0 14.31 1.05 -8 2 0 13.94 1.03 8 2 0 15.83 1.29 9 -2 0 3.88 0.41 9 -2 0 3.83 0.61 9 -2 0 4.96 0.48 -9 2 0 4.21 0.46 9 2 0 5.45 0.63 9 2 0 4.97 0.50 10 -2 0 0.11 0.46 10 -2 0 0.13 0.30 10 -2 0 0.06 0.20 10 2 0 0.12 0.28 10 2 0 -0.03 0.42 -10 2 0 -0.02 0.21 11 -2 0 2.85 0.62 11 -2 0 2.58 0.43 11 2 0 2.08 0.40 11 2 0 2.54 0.59 12 -2 0 0.59 0.39 12 -2 0 0.57 0.56 12 2 0 1.09 0.39 12 2 0 0.56 0.56 13 -2 0 5.14 0.65 13 -2 0 4.80 0.84 13 2 0 4.06 0.81 13 2 0 6.74 0.65 14 -2 0 -0.30 0.49 14 -2 0 1.22 0.66 14 2 0 0.05 0.47 14 2 0 0.70 0.64 15 -2 0 0.14 0.53 15 -2 0 1.26 0.75 15 2 0 -0.31 0.70 16 -2 0 0.18 0.61 16 -2 0 -0.37 0.73 16 2 0 0.18 0.79 0 -3 0 0.02 0.12 0 -3 0 -0.17 0.12 0 3 0 -0.24 0.15 1 -3 0 121.76 10.52 1 -3 0 148.18 8.77 1 -3 0 113.20 9.26 1 3 0 148.12 9.18 1 3 0 130.21 8.77 -1 3 0 147.67 9.18 1 3 0 123.63 10.52 2 -3 0 0.08 0.15 2 -3 0 0.03 0.13 2 -3 0 -0.15 0.13 2 3 0 -0.01 0.12 2 3 0 0.10 0.13 -2 3 0 -0.31 0.14 2 3 0 -0.34 0.14 2 3 0 -0.08 0.11 -3 -3 0 151.55 11.65 3 -3 0 169.46 13.38 3 -3 0 190.08 11.14 3 3 0 181.06 13.37 3 3 0 168.33 11.13 -3 3 0 149.22 11.66 3 3 0 174.79 11.76 4 -3 0 2.40 0.31 4 -3 0 2.53 0.26 4 -3 0 2.42 0.24 -4 -3 0 2.42 0.23 4 3 0 1.58 0.20 -4 3 0 2.03 0.26 4 3 0 1.70 0.22 4 3 0 2.68 0.29 -5 -3 0 113.01 7.63 5 -3 0 126.16 8.79 5 -3 0 107.84 7.30 5 -3 0 98.13 7.72 -5 3 0 100.28 7.64 5 3 0 121.90 8.78 5 3 0 107.79 7.70 -6 -3 0 33.02 2.27 6 -3 0 28.54 2.32 6 -3 0 37.33 2.67 6 -3 0 33.31 2.18 6 3 0 32.43 2.65 6 3 0 32.19 2.30 -6 3 0 30.82 2.29 7 -3 0 65.51 4.47 7 -3 0 72.49 5.12 7 -3 0 62.06 4.22 -7 -3 0 59.31 4.39 7 3 0 63.19 4.45 -7 3 0 58.72 4.42 7 3 0 64.90 5.10 8 -3 0 1.73 0.43 8 -3 0 2.04 0.33 8 -3 0 1.90 0.26 8 3 0 2.06 0.43 8 3 0 1.89 0.28 -8 3 0 1.84 0.29 9 -3 0 41.90 3.55 9 -3 0 40.85 3.08 9 -3 0 42.84 2.89 9 3 0 45.70 3.06 9 3 0 47.84 3.54 -9 3 0 39.92 3.02 10 -3 0 2.41 0.57 10 -3 0 3.13 0.35 10 -3 0 3.40 0.45 10 3 0 4.05 0.60 10 3 0 3.27 0.40 -10 3 0 3.00 0.37 11 -3 0 36.28 3.21 11 -3 0 35.48 2.58 11 -3 0 39.17 2.78 11 3 0 43.55 3.21 11 3 0 40.77 2.76 -11 3 0 36.09 2.70 12 -3 0 2.02 0.47 12 -3 0 3.16 0.67 12 3 0 1.90 0.64 12 3 0 2.71 0.44 13 -3 0 21.87 1.73 13 -3 0 21.00 2.05 13 3 0 24.63 2.07 14 -3 0 -0.31 0.47 14 -3 0 0.02 0.69 14 3 0 -1.19 0.59 15 -3 0 7.96 1.20 15 -3 0 9.80 1.02 15 3 0 11.33 1.24 0 -4 0 212.33 17.28 0 -4 0 221.45 15.22 0 -4 0 230.04 14.40 0 4 0 211.85 15.08 1 -4 0 16.37 1.40 1 -4 0 17.17 1.19 1 -4 0 17.68 1.26 -1 -4 0 15.79 1.24 1 4 0 19.79 1.26 -1 4 0 16.39 1.25 1 4 0 17.40 1.40 2 -4 0 89.11 7.47 2 -4 0 91.80 6.58 2 -4 0 104.88 6.23 2 4 0 95.10 6.52 2 4 0 84.41 7.45 -2 4 0 100.16 6.52 3 -4 0 25.87 1.67 3 -4 0 25.15 2.00 3 -4 0 26.49 1.77 3 4 0 23.37 1.98 -3 4 0 24.59 1.75 3 4 0 22.23 1.74 -4 -4 0 66.14 4.49 4 -4 0 65.37 5.16 4 -4 0 69.95 4.30 4 -4 0 66.19 4.55 4 4 0 57.94 4.52 4 4 0 64.48 5.15 -4 4 0 62.92 4.50 5 -4 0 -0.19 0.19 5 -4 0 0.21 0.25 5 -4 0 0.16 0.21 -5 -4 0 0.04 0.15 -5 -4 0 0.07 0.18 5 4 0 0.03 0.15 5 4 0 0.23 0.23 -5 4 0 0.04 0.20 6 -4 0 71.73 4.74 6 -4 0 64.89 4.47 -6 -4 0 63.65 4.45 6 -4 0 69.01 5.39 -6 -4 0 72.63 4.66 6 4 0 65.26 4.71 6 4 0 68.61 5.37 -6 4 0 62.62 4.68 -7 -4 0 2.31 0.27 -7 -4 0 1.81 0.21 7 -4 0 1.26 0.27 7 -4 0 1.51 0.32 7 4 0 1.57 0.25 7 4 0 1.78 0.39 -7 4 0 1.85 0.30 8 -4 0 33.45 2.41 -8 -4 0 26.37 2.01 8 -4 0 29.75 2.07 8 -4 0 27.35 1.94 -8 4 0 27.30 2.04 8 4 0 26.66 2.37 8 4 0 29.50 2.04 9 -4 0 2.66 0.55 -9 -4 0 2.35 0.28 9 -4 0 2.59 0.40 9 -4 0 1.27 0.30 9 4 0 1.73 0.32 9 4 0 2.08 0.50 -9 4 0 2.48 0.33 10 -4 0 16.61 1.25 10 -4 0 18.09 1.37 10 -4 0 16.56 1.63 10 4 0 17.62 1.32 -10 4 0 16.75 1.31 10 4 0 19.49 1.62 11 -4 0 5.46 0.62 11 -4 0 3.85 0.75 11 -4 0 5.38 0.51 -11 4 0 5.28 0.52 11 4 0 5.30 0.76 11 4 0 6.50 0.57 12 -4 0 17.46 1.34 12 -4 0 19.89 1.76 12 -4 0 19.76 1.49 12 4 0 18.29 1.75 13 -4 0 2.53 0.53 13 -4 0 2.53 0.75 13 4 0 2.65 0.72 14 -4 0 10.30 1.26 14 -4 0 10.81 1.05 14 4 0 12.61 1.35 15 -4 0 1.50 0.78 15 -4 0 0.40 0.55 15 4 0 0.11 0.74 0 -5 0 -0.03 0.20 0 -5 0 0.30 0.21 0 -5 0 0.52 0.19 0 5 0 0.64 0.24 1 -5 0 19.41 1.32 1 -5 0 18.19 1.56 -1 -5 0 18.12 1.38 1 -5 0 19.70 1.40 -1 -5 0 17.98 1.55 -1 -5 0 18.77 1.32 1 5 0 20.62 1.40 -1 5 0 19.39 1.39 2 -5 0 28.02 2.13 -2 -5 0 27.10 2.11 2 -5 0 34.36 2.03 -2 -5 0 29.20 2.01 -2 5 0 31.12 2.11 2 5 0 30.59 2.12 2 5 0 27.94 2.39 3 -5 0 33.05 2.75 3 -5 0 33.65 2.43 -3 -5 0 33.77 2.29 3 -5 0 34.98 2.31 -3 5 0 38.81 2.42 3 5 0 30.63 2.73 -4 -5 0 15.30 1.07 4 -5 0 14.84 1.24 4 -5 0 14.76 1.03 4 -5 0 15.53 1.09 -4 -5 0 12.70 1.01 4 5 0 14.24 1.20 -4 5 0 13.89 1.08 4 5 0 12.57 1.05 -5 -5 0 9.17 0.74 5 -5 0 9.73 0.72 5 -5 0 8.86 0.87 5 -5 0 10.45 0.77 -5 -5 0 8.27 0.69 5 5 0 8.71 0.85 5 5 0 8.33 0.71 -5 5 0 9.03 0.77 -6 -5 0 8.81 0.70 6 -5 0 9.26 0.75 -6 -5 0 9.35 0.76 6 -5 0 9.77 0.93 6 -5 0 11.02 0.81 6 5 0 8.96 0.88 6 5 0 8.33 0.74 7 -5 0 15.04 1.49 -7 -5 0 16.04 1.16 7 -5 0 18.72 1.31 7 -5 0 17.55 1.21 -7 -5 0 17.15 1.24 -7 5 0 16.89 1.27 7 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