data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Roy, Kinkini' 'Wang, Chun' 'Smith, Mark' 'Dewal, Mahender' 'Wibowo, Arief' 'Brown, Julius' 'Ma, Shuguo' 'Shimizu, Linda' _publ_contact_author_name 'Shimizu, Linda' _publ_contact_author_email shimizul@mail.chem.sc.edu _publ_section_title ; Guest induced transformations of assembled pyridyl bis-urea macrocycles ; # Attachment '- CIF Host 1+ Host 1.TFE.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 781839' #TrackingRef '- CIF Host 1+ Host 1.TFE.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H18 N6 O2' _chemical_formula_sum 'C16 H18 N6 O2' _chemical_formula_weight 326.36 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5207(5) _cell_length_b 4.6948(3) _cell_length_c 16.3045(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.2010(10) _cell_angle_gamma 90.00 _cell_volume 728.77(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2525 _cell_measurement_theta_min 2.498 _cell_measurement_theta_max 26.356 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 344 _exptl_absorpt_coefficient_mu 0.104 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8648 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 26.37 _reflns_number_total 1489 _reflns_number_gt 1214 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1489 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0452 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0832 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.37600(14) 0.7876(3) 0.40923(8) 0.0189(3) Uani 1 1 d . . . C2 C 0.16253(14) 0.6850(3) 0.48732(8) 0.0222(3) Uani 1 1 d . . . H2A H 0.1583 0.5210 0.4492 0.025(4) Uiso 1 1 calc R . . H2B H 0.0714 0.7861 0.4841 0.030(4) Uiso 1 1 calc R . . C3 C 0.18345(14) 0.5754(3) 0.57381(8) 0.0196(3) Uani 1 1 d . . . C4 C 0.10596(15) 0.6794(3) 0.63882(9) 0.0231(3) Uani 1 1 d . . . H4 H 0.0345 0.8173 0.6299 0.026(4) Uiso 1 1 calc R . . C5 C 0.13423(15) 0.5791(3) 0.71734(9) 0.0248(3) Uani 1 1 d . . . H5 H 0.0825 0.6476 0.7630 0.023(4) Uiso 1 1 calc R . . C6 C 0.23854(14) 0.3788(3) 0.72793(8) 0.0223(3) Uani 1 1 d . . . H6 H 0.2599 0.3071 0.7810 0.027(4) Uiso 1 1 calc R . . C7 C 0.31230(14) 0.2831(3) 0.65935(8) 0.0196(3) Uani 1 1 d . . . C8 C 0.42455(14) 0.0598(3) 0.67133(8) 0.0211(3) Uani 1 1 d . . . H8A H 0.4805 0.1110 0.7204 0.026(4) Uiso 1 1 calc R . . H8B H 0.3781 -0.1246 0.6827 0.018(3) Uiso 1 1 calc R . . N1 N 0.48034(12) 0.9791(2) 0.39683(7) 0.0206(3) Uani 1 1 d . . . H1 H 0.4627(16) 1.153(4) 0.4082(9) 0.026(4) Uiso 1 1 d . . . N2 N 0.27305(12) 0.8758(2) 0.46122(7) 0.0218(3) Uani 1 1 d . . . H2 H 0.2906(16) 1.024(3) 0.4913(9) 0.024(4) Uiso 1 1 d . . . N3 N 0.28442(12) 0.3764(2) 0.58336(7) 0.0199(3) Uani 1 1 d . . . O1 O 0.37363(10) 0.55342(19) 0.37437(6) 0.0237(3) 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 C1 0.0233(7) 0.0163(7) 0.0172(7) 0.0014(5) -0.0037(5) 0.0030(6) C2 0.0213(8) 0.0223(7) 0.0230(7) 0.0001(6) -0.0007(6) 0.0017(6) C3 0.0183(7) 0.0175(7) 0.0230(7) -0.0012(5) -0.0015(5) -0.0029(5) C4 0.0204(7) 0.0203(7) 0.0287(8) -0.0006(6) 0.0020(6) 0.0018(6) C5 0.0251(8) 0.0250(8) 0.0245(7) -0.0013(6) 0.0065(6) -0.0019(6) C6 0.0253(8) 0.0215(7) 0.0202(7) 0.0021(6) 0.0020(6) -0.0040(6) C7 0.0207(7) 0.0157(7) 0.0226(7) -0.0007(5) 0.0002(6) -0.0043(6) C8 0.0248(8) 0.0176(7) 0.0209(7) 0.0022(5) -0.0008(6) -0.0004(6) N1 0.0247(6) 0.0133(6) 0.0238(6) -0.0017(5) 0.0005(5) 0.0014(5) N2 0.0271(7) 0.0163(6) 0.0219(6) -0.0034(5) 0.0022(5) -0.0001(5) N3 0.0214(6) 0.0172(6) 0.0213(6) -0.0005(5) 0.0001(5) -0.0009(5) O1 0.0313(6) 0.0161(5) 0.0237(5) -0.0032(4) 0.0026(4) 0.0000(4) _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 C1 O1 1.2379(15) . ? C1 N1 1.3554(17) . ? C1 N2 1.3625(17) . ? C2 N2 1.4469(18) . ? C2 C3 1.5136(18) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N3 1.3492(17) . ? C3 C4 1.3828(19) . ? C4 C5 1.389(2) . ? C4 H4 0.9500 . ? C5 C6 1.3781(19) . ? C5 H5 0.9500 . ? C6 C7 1.3969(18) . ? C6 H6 0.9500 . ? C7 N3 1.3397(17) . ? C7 C8 1.5091(18) . ? C8 N1 1.4474(17) 3_666 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C8 1.4474(17) 3_666 ? N1 H1 0.855(16) . ? N2 H2 0.867(15) . ? 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 C1 N1 122.18(13) . . ? O1 C1 N2 122.92(12) . . ? N1 C1 N2 114.88(11) . . ? N2 C2 C3 113.02(11) . . ? N2 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? N2 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? N3 C3 C4 122.54(13) . . ? N3 C3 C2 115.75(11) . . ? C4 C3 C2 121.69(13) . . ? C3 C4 C5 118.98(13) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 118.93(13) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C7 118.91(13) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? N3 C7 C6 122.44(13) . . ? N3 C7 C8 118.99(12) . . ? C6 C7 C8 118.54(12) . . ? N1 C8 C7 115.64(11) 3_666 . ? N1 C8 H8A 108.4 3_666 . ? C7 C8 H8A 108.4 . . ? N1 C8 H8B 108.4 3_666 . ? C7 C8 H8B 108.4 . . ? H8A C8 H8B 107.4 . . ? C1 N1 C8 119.46(12) . 3_666 ? C1 N1 H1 117.2(10) . . ? C8 N1 H1 114.2(10) 3_666 . ? C1 N2 C2 121.36(11) . . ? C1 N2 H2 117.3(10) . . ? C2 N2 H2 118.0(10) . . ? C7 N3 C3 118.16(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N3 -74.20(15) . . . . ? N2 C2 C3 C4 104.18(15) . . . . ? N3 C3 C4 C5 1.0(2) . . . . ? C2 C3 C4 C5 -177.23(12) . . . . ? C3 C4 C5 C6 -0.1(2) . . . . ? C4 C5 C6 C7 -0.1(2) . . . . ? C5 C6 C7 N3 -0.8(2) . . . . ? C5 C6 C7 C8 -178.91(12) . . . . ? N3 C7 C8 N1 16.50(18) . . . 3_666 ? C6 C7 C8 N1 -165.28(12) . . . 3_666 ? O1 C1 N1 C8 13.7(2) . . . 3_666 ? N2 C1 N1 C8 -164.83(12) . . . 3_666 ? O1 C1 N2 C2 8.1(2) . . . . ? N1 C1 N2 C2 -173.43(12) . . . . ? C3 C2 N2 C1 103.26(15) . . . . ? C6 C7 N3 C3 1.66(19) . . . . ? C8 C7 N3 C3 179.81(11) . . . . ? C4 C3 N3 C7 -1.81(19) . . . . ? C2 C3 N3 C7 176.56(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.855(16) 2.133(17) 2.9042(15) 149.8(14) 1_565 N2 H2 N3 0.867(15) 2.235(15) 3.0822(16) 165.6(13) 1_565 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.223 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.041 #===END data_1TFE _database_code_depnum_ccdc_archive 'CCDC 781840' #TrackingRef '- CIF Host 1+ Host 1.TFE.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H18 N6 O2, 2(C2 H3 F3 O)' _chemical_formula_sum 'C20 H24 F6 N6 O4' _chemical_formula_weight 526.45 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 4.6955(12) _cell_length_b 9.632(3) _cell_length_c 12.775(3) _cell_angle_alpha 93.970(5) _cell_angle_beta 100.219(5) _cell_angle_gamma 95.594(5) _cell_volume 563.7(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1146 _cell_measurement_theta_min 2.133 _cell_measurement_theta_max 24.632 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 272 _exptl_absorpt_coefficient_mu 0.142 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6732 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS Version 2.05 (Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5796 _diffrn_reflns_av_R_equivalents 0.0583 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.94 _reflns_number_total 1970 _reflns_number_gt 1372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART Version 5.625 (Bruker, 2001)' _computing_cell_refinement 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_data_reduction 'SAINT-Plus Version 6.45 (Bruker, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics various _computing_publication_material 'SHELXTL Version 6.14 (Bruker, 2000)' _refine_special_details ; 73 restraints used in modeling four-fold trifluoro(ethanol) disorder Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0891P)^2^+0.6402P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1970 _refine_ls_number_parameters 201 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.1004 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1908 _refine_ls_wR_factor_gt 0.1698 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.1772(7) 0.6143(3) 0.3803(3) 0.0216(8) Uani 1 1 d . A . C2 C 0.2137(8) 0.4215(4) 0.2475(3) 0.0273(9) Uani 1 1 d . . . H2A H 0.3822 0.4846 0.2357 0.033 Uiso 1 1 calc R . . H2B H 0.0767 0.4008 0.1784 0.033 Uiso 1 1 calc R . . C3 C 0.3168(7) 0.2874(4) 0.2852(3) 0.0224(8) Uani 1 1 d . . . C4 C 0.1705(8) 0.1573(4) 0.2442(3) 0.0294(9) Uani 1 1 d . . . H4 H 0.0050 0.1502 0.1884 0.035 Uiso 1 1 calc R . . C5 C 0.2698(9) 0.0385(4) 0.2859(3) 0.0318(9) Uani 1 1 d . . . H5 H 0.1735 -0.0516 0.2589 0.038 Uiso 1 1 calc R . . C6 C 0.5081(8) 0.0518(4) 0.3666(3) 0.0254(8) Uani 1 1 d . . . H6 H 0.5798 -0.0286 0.3962 0.030 Uiso 1 1 calc R . . C7 C 0.6439(7) 0.1858(3) 0.4045(3) 0.0212(8) Uani 1 1 d . . . C8 C 0.9090(7) 0.2018(4) 0.4932(3) 0.0258(8) Uani 1 1 d . . . H8A H 0.8762 0.1342 0.5459 0.031 Uiso 1 1 calc R . . H8B H 1.0788 0.1770 0.4626 0.031 Uiso 1 1 calc R . . N1 N 0.0206(7) 0.6598(3) 0.4517(2) 0.0239(7) Uani 1 1 d . . . H1 H -0.138(9) 0.622(4) 0.452(3) 0.023(10) Uiso 1 1 d . . . N2 N 0.0700(7) 0.4912(3) 0.3242(2) 0.0255(7) Uani 1 1 d . . . H2 H -0.083(9) 0.445(4) 0.343(3) 0.031(11) Uiso 1 1 d . . . N3 N 0.5525(6) 0.3011(3) 0.3644(2) 0.0223(7) Uani 1 1 d . . . O1 O 0.4066(5) 0.6841(2) 0.36883(19) 0.0264(6) Uani 1 1 d . . . O1SA O 0.7003(13) 0.7813(6) 0.2221(5) 0.0289(9) Uiso 0.35 1 d PD A 1 C1SA C 0.553(3) 0.7143(11) 0.1185(7) 0.0327(19) Uiso 0.35 1 d PD A 1 H1S1 H 0.3449 0.6869 0.1199 0.039 Uiso 0.35 1 calc PR A 1 H1S2 H 0.6426 0.6290 0.1009 0.039 Uiso 0.35 1 calc PR A 1 C2SA C 0.580(2) 0.8147(10) 0.0379(8) 0.0392(17) Uiso 0.35 1 d PD A 1 F1SA F 0.418(2) 0.7587(15) -0.0564(7) 0.039(3) Uiso 0.35 1 d PD A 1 F2SA F 0.8571(15) 0.8359(11) 0.0258(6) 0.0464(19) Uiso 0.35 1 d PD A 1 F3SA F 0.488(2) 0.9353(11) 0.0609(9) 0.101(3) Uiso 0.35 1 d PD A 1 O1SB O 0.7003(13) 0.7813(6) 0.2221(5) 0.0289(9) Uiso 0.20 1 d PD B 2 C1SB C 0.490(4) 0.754(3) 0.1224(11) 0.0327(19) Uiso 0.20 1 d PD B 2 H1S3 H 0.3308 0.8142 0.1244 0.039 Uiso 0.20 1 calc PR B 2 H1S4 H 0.4040 0.6554 0.1143 0.039 Uiso 0.20 1 calc PR B 2 C2SB C 0.630(3) 0.7836(15) 0.0298(13) 0.0392(17) Uiso 0.20 1 d PD B 2 F1SB F 0.796(4) 0.6848(19) 0.0092(14) 0.073(5) Uiso 0.20 1 d PD B 2 F2SB F 0.808(3) 0.9052(14) 0.0445(11) 0.056(4) Uiso 0.20 1 d PD B 2 F3SB F 0.436(3) 0.8025(17) -0.0580(13) 0.057(7) Uiso 0.20 1 d PD B 2 O2SA O 0.7342(15) 0.7490(7) 0.2159(6) 0.0289(9) Uiso 0.25 1 d PD A 3 C3SA C 0.495(3) 0.777(2) 0.1338(10) 0.0327(19) Uiso 0.25 1 d PD A 3 H3S1 H 0.4900 0.8785 0.1263 0.039 Uiso 0.25 1 calc PR A 3 H3S2 H 0.3041 0.7346 0.1455 0.039 Uiso 0.25 1 calc PR A 3 C4SA C 0.593(3) 0.7033(13) 0.0425(11) 0.0392(17) Uiso 0.25 1 d PD A 3 F4SA F 0.8464(18) 0.7555(14) 0.0170(7) 0.035(2) Uiso 0.25 1 d PD A 3 F5SA F 0.400(2) 0.6875(14) -0.0505(9) 0.051(3) Uiso 0.25 1 d PD A 3 F6SA F 0.623(3) 0.5678(11) 0.0593(10) 0.069(3) Uiso 0.25 1 d PD A 3 O2SB O 0.7342(15) 0.7490(7) 0.2159(6) 0.0289(9) Uiso 0.20 1 d PD C 4 C3SB C 0.581(5) 0.8076(18) 0.1244(11) 0.0327(19) Uiso 0.20 1 d PD C 4 H3S3 H 0.6929 0.8939 0.1087 0.039 Uiso 0.20 1 calc PR C 4 H3S4 H 0.3864 0.8293 0.1354 0.039 Uiso 0.20 1 calc PR C 4 C4SB C 0.559(3) 0.6939(16) 0.0379(12) 0.0392(17) Uiso 0.20 1 d PD C 4 F4SB F 0.482(3) 0.7257(17) -0.0635(10) 0.035(4) Uiso 0.20 1 d PD C 4 F5SB F 0.356(3) 0.5892(18) 0.0501(14) 0.096(6) Uiso 0.20 1 d PD C 4 F6SB F 0.785(3) 0.6202(17) 0.0331(12) 0.062(4) Uiso 0.20 1 d PD C 4 H1S H 0.623(13) 0.721(5) 0.272(5) 0.093 Uiso 1 1 d D A . 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 C1 0.0184(17) 0.0235(18) 0.0225(19) 0.0091(14) 0.0010(14) 0.0005(14) C2 0.0263(19) 0.030(2) 0.0225(19) 0.0032(15) 0.0004(15) -0.0031(15) C3 0.0206(18) 0.0260(19) 0.0209(18) 0.0046(14) 0.0062(15) -0.0023(14) C4 0.029(2) 0.031(2) 0.025(2) 0.0002(16) 0.0014(16) -0.0075(16) C5 0.038(2) 0.025(2) 0.031(2) -0.0005(16) 0.0097(18) -0.0082(16) C6 0.0273(19) 0.0228(18) 0.028(2) 0.0039(15) 0.0108(16) -0.0015(15) C7 0.0188(17) 0.0220(18) 0.0250(19) 0.0061(14) 0.0099(15) -0.0005(14) C8 0.0208(18) 0.0266(19) 0.032(2) 0.0075(15) 0.0073(16) 0.0035(15) N1 0.0142(15) 0.0270(17) 0.0301(18) 0.0065(13) 0.0055(13) -0.0055(13) N2 0.0194(16) 0.0234(16) 0.0334(18) 0.0063(13) 0.0066(14) -0.0047(13) N3 0.0205(15) 0.0230(16) 0.0241(16) 0.0048(12) 0.0073(13) -0.0011(12) O1 0.0173(12) 0.0297(14) 0.0314(15) 0.0069(11) 0.0059(10) -0.0069(10) _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 C1 O1 1.250(4) . ? C1 N1 1.345(5) . ? C1 N2 1.346(4) . ? C2 N2 1.449(5) . ? C2 C3 1.504(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N3 1.349(4) . ? C3 C4 1.389(5) . ? C4 C5 1.383(5) . ? C4 H4 0.9500 . ? C5 C6 1.370(5) . ? C5 H5 0.9500 . ? C6 C7 1.396(5) . ? C6 H6 0.9500 . ? C7 N3 1.332(4) . ? C7 C8 1.515(5) . ? C8 N1 1.443(5) 2_666 ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? N1 C8 1.443(5) 2_666 ? N1 H1 0.80(4) . ? N2 H2 0.88(4) . ? O1 O1SA 2.683(7) . ? O1 O2SA 2.762(8) . ? O1SA C1SA 1.455(10) . ? O1SA H1S 0.99(7) . ? C1SA C2SA 1.473(10) . ? C1SA H1S1 0.9900 . ? C1SA H1S2 0.9900 . ? C2SA F3SA 1.311(10) . ? C2SA F2SA 1.336(9) . ? C2SA F1SA 1.351(9) . ? C1SB C2SB 1.482(12) . ? C1SB H1S3 0.9900 . ? C1SB H1S4 0.9900 . ? C2SB F1SB 1.331(12) . ? C2SB F3SB 1.346(12) . ? C2SB F2SB 1.355(12) . ? O2SA C3SA 1.454(11) . ? O2SA H1S 1.00(7) . ? C3SA C4SA 1.489(12) . ? C3SA H3S1 0.9900 . ? C3SA H3S2 0.9900 . ? C4SA F4SA 1.349(11) . ? C4SA F5SA 1.350(11) . ? C4SA F6SA 1.354(11) . ? C3SB C4SB 1.484(12) . ? C3SB H3S3 0.9900 . ? C3SB H3S4 0.9900 . ? C4SB F6SB 1.343(12) . ? C4SB F4SB 1.347(12) . ? C4SB F5SB 1.354(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 O1 C1 N1 120.8(3) . . ? O1 C1 N2 123.6(3) . . ? N1 C1 N2 115.6(3) . . ? N2 C2 C3 111.5(3) . . ? N2 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? N3 C3 C4 122.0(3) . . ? N3 C3 C2 116.1(3) . . ? C4 C3 C2 121.9(3) . . ? C5 C4 C3 118.9(3) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 119.4(3) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C5 C6 C7 118.8(3) . . ? C5 C6 H6 120.6 . . ? C7 C6 H6 120.6 . . ? N3 C7 C6 122.5(3) . . ? N3 C7 C8 118.2(3) . . ? C6 C7 C8 119.3(3) . . ? N1 C8 C7 114.7(3) 2_666 . ? N1 C8 H8A 108.6 2_666 . ? C7 C8 H8A 108.6 . . ? N1 C8 H8B 108.6 2_666 . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C1 N1 C8 120.9(3) . 2_666 ? C1 N1 H1 121(3) . . ? C8 N1 H1 116(3) 2_666 . ? C1 N2 C2 124.0(3) . . ? C1 N2 H2 117(3) . . ? C2 N2 H2 118(3) . . ? C7 N3 C3 118.5(3) . . ? C1 O1 H1S 141.7(19) . . ? C1 O1 O1SA 143.4(3) . . ? C1 O1 O2SA 141.7(3) . . ? C1SA O1SA O1 107.4(5) . . ? C1SA O1SA H1S 103(3) . . ? O1SA C1SA C2SA 108.2(8) . . ? O1SA C1SA H1S1 110.1 . . ? C2SA C1SA H1S1 110.1 . . ? O1SA C1SA H1S2 110.1 . . ? C2SA C1SA H1S2 110.1 . . ? H1S1 C1SA H1S2 108.4 . . ? F3SA C2SA F2SA 109.3(9) . . ? F3SA C2SA F1SA 107.5(9) . . ? F2SA C2SA F1SA 108.2(8) . . ? F3SA C2SA C1SA 113.5(10) . . ? F2SA C2SA C1SA 109.7(9) . . ? F1SA C2SA C1SA 108.5(9) . . ? C2SB C1SB H1S3 109.4 . . ? C2SB C1SB H1S4 109.4 . . ? H1S3 C1SB H1S4 108.0 . . ? F1SB C2SB F3SB 111.1(13) . . ? F1SB C2SB F2SB 105.2(12) . . ? F3SB C2SB F2SB 102.2(11) . . ? F1SB C2SB C1SB 111.4(16) . . ? F3SB C2SB C1SB 112.8(14) . . ? F2SB C2SB C1SB 113.7(16) . . ? C3SA O2SA O1 97.1(8) . . ? C3SA O2SA H1S 100(3) . . ? O2SA C3SA C4SA 96.6(10) . . ? O2SA C3SA H3S1 112.4 . . ? C4SA C3SA H3S1 112.4 . . ? O2SA C3SA H3S2 112.4 . . ? C4SA C3SA H3S2 112.4 . . ? H3S1 C3SA H3S2 110.0 . . ? F4SA C4SA F5SA 104.9(10) . . ? F4SA C4SA F6SA 105.5(11) . . ? F5SA C4SA F6SA 100.7(10) . . ? F4SA C4SA C3SA 117.5(13) . . ? F5SA C4SA C3SA 115.4(11) . . ? F6SA C4SA C3SA 111.1(13) . . ? C4SB C3SB H3S3 111.2 . . ? C4SB C3SB H3S4 111.2 . . ? H3S3 C3SB H3S4 109.1 . . ? F6SB C4SB F4SB 102.8(11) . . ? F6SB C4SB F5SB 99.6(11) . . ? F4SB C4SB F5SB 105.2(12) . . ? F6SB C4SB C3SB 119.7(14) . . ? F4SB C4SB C3SB 117.7(13) . . ? F5SB C4SB C3SB 109.6(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 C2 C3 N3 -73.7(4) . . . . ? N2 C2 C3 C4 103.6(4) . . . . ? N3 C3 C4 C5 0.0(5) . . . . ? C2 C3 C4 C5 -177.1(3) . . . . ? C3 C4 C5 C6 0.3(6) . . . . ? C4 C5 C6 C7 0.1(5) . . . . ? C5 C6 C7 N3 -0.8(5) . . . . ? C5 C6 C7 C8 -179.6(3) . . . . ? N3 C7 C8 N1 19.0(5) . . . 2_666 ? C6 C7 C8 N1 -162.1(3) . . . 2_666 ? O1 C1 N1 C8 8.2(5) . . . 2_666 ? N2 C1 N1 C8 -171.9(3) . . . 2_666 ? O1 C1 N2 C2 3.0(5) . . . . ? N1 C1 N2 C2 -176.9(3) . . . . ? C3 C2 N2 C1 112.6(4) . . . . ? C6 C7 N3 C3 1.1(5) . . . . ? C8 C7 N3 C3 179.9(3) . . . . ? C4 C3 N3 C7 -0.7(5) . . . . ? C2 C3 N3 C7 176.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O1 0.80(4) 2.37(4) 2.928(4) 128(3) 1_455 N2 H2 N3 0.88(4) 2.17(4) 3.038(4) 169(4) 1_455 O1SA H1S O1 0.99(7) 1.77(7) 2.683(7) 153(4) 1_555 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.94 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.620 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.068 _vrf_PLAT431_ddtfes ; PROBLEM: Short Inter HL..A Contact F3SA .. F3SA .. 2.07 Ang. RESPONSE: The F3, F5, F6, C2 and C4 atoms are part of disorder assemblies with occupancies < 0.5. When F3SA is present in a given asymmetric unit, the symmetry-equivalent F3SA* need not be present, etc. ; #===END