# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_15BAPA #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C26 H20 N2' _chemical_formula_moiety 'C26 H20 N2' _chemical_formula_weight 360.46 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 9.9279(3) _cell_length_b 9.9281(3) _cell_length_c 10.6034(3) _cell_angle_alpha 85.8443(14) _cell_angle_beta 61.4620(12) _cell_angle_gamma 87.2191(14) _cell_volume 915.62(4) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5896 _cell_measurement_theta_min 4.46 _cell_measurement_theta_max 68.19 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.307 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380.00 _exptl_absorpt_coefficient_mu 0.589 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 9853 _diffrn_reflns_av_R_equivalents 0.0777 _diffrn_reflns_theta_max 68.20 _diffrn_reflns_theta_full 68.20 _diffrn_measured_fraction_theta_max 0.974 _diffrn_measured_fraction_theta_full 0.974 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3262 _reflns_number_gt 1717 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.2400 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 3262 _refine_ls_number_parameters 253 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0888P)^2^+0.4190P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.240 _refine_diff_density_min -0.360 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.031 0.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 N1 N 0.1556(4) 0.2749(4) -0.0325(4) 0.0662(10) Uani 1.0 2 d . . . N2 N 0.8060(4) 0.2179(4) 1.0368(4) 0.0625(10) Uani 1.0 2 d . . . C1 C 0.2680(4) 0.1232(4) 0.4382(4) 0.0438(9) Uani 1.0 2 d . . . C2 C 0.1850(4) 0.0152(4) 0.5293(4) 0.0492(10) Uani 1.0 2 d . . . C3 C 0.2000(5) -0.0298(4) 0.6515(4) 0.0494(10) Uani 1.0 2 d . . . C4 C 0.2984(4) 0.0312(4) 0.6836(4) 0.0488(10) Uani 1.0 2 d . . . C5 C 0.7126(4) 0.3596(4) 0.5537(4) 0.0446(9) Uani 1.0 2 d . . . C6 C 0.8116(5) 0.4492(4) 0.4491(4) 0.0492(10) Uani 1.0 2 d . . . C7 C 0.7972(5) 0.4926(4) 0.3267(4) 0.0527(10) Uani 1.0 2 d . . . C8 C 0.6822(4) 0.4465(4) 0.3078(4) 0.0482(9) Uani 1.0 2 d . . . C9 C 0.4700(4) 0.2917(4) 0.3806(4) 0.0439(9) Uani 1.0 2 d . . . C10 C 0.4973(4) 0.2000(4) 0.6226(4) 0.0474(9) Uani 1.0 2 d . . . C11 C 0.3740(4) 0.1885(4) 0.4700(4) 0.0419(9) Uani 1.0 2 d . . . C12 C 0.3893(4) 0.1414(4) 0.5936(4) 0.0424(9) Uani 1.0 2 d . . . C13 C 0.5794(4) 0.3489(4) 0.4074(4) 0.0443(9) Uani 1.0 2 d . . . C14 C 0.5946(4) 0.3030(4) 0.5310(4) 0.0423(9) Uani 1.0 2 d . . . C15 C 0.1905(5) 0.2397(4) 0.0792(4) 0.0511(10) Uani 1.0 2 d . . . C16 C 0.1868(5) 0.3357(4) 0.1696(4) 0.0505(10) Uani 1.0 2 d . . . C17 C 0.2129(4) 0.2991(4) 0.2840(4) 0.0490(10) Uani 1.0 2 d . . . C18 C 0.2458(4) 0.1660(4) 0.3125(4) 0.0457(9) Uani 1.0 2 d . . . C19 C 0.2514(5) 0.0706(4) 0.2198(4) 0.0525(10) Uani 1.0 2 d . . . C20 C 0.2246(5) 0.1074(4) 0.1046(4) 0.0568(11) Uani 1.0 2 d . . . C21 C 0.7806(5) 0.2561(4) 0.9212(4) 0.0501(10) Uani 1.0 2 d . . . C22 C 0.6369(5) 0.2938(4) 0.9384(4) 0.0533(10) Uani 1.0 2 d . . . C23 C 0.6146(5) 0.3263(4) 0.8207(4) 0.0521(10) Uani 1.0 2 d . . . C24 C 0.7330(4) 0.3216(4) 0.6805(4) 0.0438(9) Uani 1.0 2 d . . . C25 C 0.8777(5) 0.2829(4) 0.6644(4) 0.0492(10) Uani 1.0 2 d . . . C26 C 0.9012(5) 0.2508(4) 0.7808(4) 0.0492(10) Uani 1.0 2 d . . . H2 H 0.1167 -0.0293 0.5089 0.0591 Uiso 1.0 2 calc R . . H3 H 0.1414 -0.1026 0.7111 0.0592 Uiso 1.0 2 calc R . . H4A H 0.7300 0.2170 1.1240 0.0750 Uiso 1.0 2 calc R . . H4B H 0.8978 0.1948 1.0220 0.0750 Uiso 1.0 2 calc R . . H4 H 0.3069 0.0008 0.7657 0.0586 Uiso 1.0 2 calc R . . H5 H 0.5046 0.1696 0.7052 0.0568 Uiso 1.0 2 calc R . . H6 H 0.8923 0.4828 0.4597 0.0590 Uiso 1.0 2 calc R . . H7 H 0.8677 0.5540 0.2577 0.0633 Uiso 1.0 2 calc R . . H8 H 0.6704 0.4794 0.2281 0.0578 Uiso 1.0 2 calc R . . H9 H 0.4608 0.3241 0.2995 0.0526 Uiso 1.0 2 calc R . . H25 H 0.9612 0.2787 0.5714 0.0590 Uiso 1.0 2 calc R . . H17 H 0.2085 0.3658 0.3445 0.0588 Uiso 1.0 2 calc R . . H19 H 0.2738 -0.0202 0.2355 0.0630 Uiso 1.0 2 calc R . . H16 H 0.1663 0.4267 0.1527 0.0605 Uiso 1.0 2 calc R . . H22 H 0.5534 0.2973 1.0315 0.0640 Uiso 1.0 2 calc R . . H23 H 0.5158 0.3524 0.8360 0.0625 Uiso 1.0 2 calc R . . H20 H 0.2296 0.0413 0.0432 0.0682 Uiso 1.0 2 calc R . . H26 H 0.9999 0.2250 0.7658 0.0590 Uiso 1.0 2 calc R . . H29A H 0.1553 0.2130 -0.0864 0.0795 Uiso 1.0 2 calc R . . H29B H 0.1343 0.3585 -0.0478 0.0795 Uiso 1.0 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 N1 0.082(3) 0.073(3) 0.064(3) -0.0060(19) -0.052(2) 0.0066(18) N2 0.071(3) 0.075(3) 0.049(2) 0.0004(19) -0.0357(19) 0.0039(17) C1 0.048(2) 0.043(2) 0.042(2) -0.0002(16) -0.0231(17) -0.0007(16) C2 0.052(3) 0.051(3) 0.051(3) -0.0060(18) -0.0296(19) -0.0014(17) C3 0.057(3) 0.045(2) 0.048(3) -0.0073(17) -0.0267(19) 0.0056(17) C4 0.052(3) 0.051(3) 0.046(2) -0.0060(17) -0.0261(19) 0.0057(17) C5 0.051(3) 0.044(2) 0.043(2) -0.0025(16) -0.0259(18) -0.0004(16) C6 0.056(3) 0.048(2) 0.051(3) -0.0112(18) -0.031(2) 0.0025(17) C7 0.060(3) 0.057(3) 0.044(2) -0.0121(19) -0.026(2) 0.0046(18) C8 0.054(3) 0.048(2) 0.045(2) -0.0071(17) -0.0246(19) 0.0035(17) C9 0.053(3) 0.0388(19) 0.044(2) -0.0046(16) -0.0269(18) 0.0042(15) C10 0.056(3) 0.050(3) 0.040(2) -0.0013(17) -0.0262(18) -0.0013(17) C11 0.047(2) 0.0419(19) 0.043(2) -0.0005(16) -0.0263(17) -0.0035(15) C12 0.051(2) 0.0376(18) 0.040(2) -0.0061(15) -0.0233(17) 0.0028(15) C13 0.053(3) 0.0395(19) 0.044(2) -0.0040(16) -0.0264(18) 0.0023(15) C14 0.047(2) 0.041(2) 0.041(2) -0.0016(16) -0.0225(17) -0.0030(15) C15 0.052(3) 0.059(3) 0.046(3) -0.0065(18) -0.0270(19) 0.0082(18) C16 0.060(3) 0.045(2) 0.052(3) 0.0002(18) -0.032(2) 0.0006(17) C17 0.055(3) 0.044(2) 0.054(3) -0.0019(17) -0.0310(19) -0.0005(17) C18 0.049(3) 0.048(2) 0.042(2) -0.0052(17) -0.0233(18) -0.0017(16) C19 0.061(3) 0.049(3) 0.056(3) -0.0062(18) -0.035(2) -0.0003(18) C20 0.072(3) 0.056(3) 0.054(3) -0.007(2) -0.038(3) -0.0061(19) C21 0.061(3) 0.051(3) 0.048(3) -0.0045(18) -0.033(2) -0.0003(17) C22 0.058(3) 0.061(3) 0.043(2) -0.0032(19) -0.0260(19) -0.0015(18) C23 0.050(3) 0.056(3) 0.055(3) 0.0003(18) -0.029(2) -0.0063(18) C24 0.052(3) 0.0390(19) 0.043(2) -0.0032(16) -0.0245(18) -0.0011(15) C25 0.054(3) 0.048(2) 0.049(3) 0.0018(17) -0.0272(19) -0.0031(17) C26 0.052(3) 0.049(3) 0.053(3) -0.0069(17) -0.031(2) 0.0001(18) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 N1 C15 1.402(7) yes . . N2 C21 1.388(7) yes . . C1 C2 1.392(5) yes . . C1 C11 1.442(7) yes . . C1 C18 1.481(7) yes . . C2 C3 1.412(7) yes . . C3 C4 1.358(7) yes . . C4 C12 1.430(5) yes . . C5 C6 1.374(5) yes . . C5 C14 1.449(7) yes . . C5 C24 1.473(7) yes . . C6 C7 1.408(7) yes . . C7 C8 1.355(7) yes . . C8 C13 1.419(5) yes . . C9 C11 1.395(5) yes . . C9 C13 1.400(7) yes . . C10 C12 1.409(7) yes . . C10 C14 1.405(5) yes . . C11 C12 1.433(6) yes . . C13 C14 1.430(6) yes . . C15 C16 1.387(7) yes . . C15 C20 1.380(6) yes . . C16 C17 1.377(7) yes . . C17 C18 1.392(6) yes . . C18 C19 1.394(6) yes . . C19 C20 1.391(7) yes . . C21 C22 1.385(7) yes . . C21 C26 1.397(5) yes . . C22 C23 1.382(7) yes . . C23 C24 1.389(5) yes . . C24 C25 1.401(6) yes . . C25 C26 1.374(7) yes . . N1 H29A 0.870 no . . N1 H29B 0.870 no . . N2 H4A 0.870 no . . N2 H4B 0.870 no . . C2 H2 0.940 no . . C3 H3 0.940 no . . C4 H4 0.940 no . . C6 H6 0.940 no . . C7 H7 0.940 no . . C8 H8 0.940 no . . C9 H9 0.940 no . . C10 H5 0.940 no . . C16 H16 0.940 no . . C17 H17 0.940 no . . C19 H19 0.940 no . . C20 H20 0.940 no . . C22 H22 0.940 no . . C23 H23 0.940 no . . C25 H25 0.940 no . . C26 H26 0.940 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C2 C1 C11 118.1(4) yes . . . C2 C1 C18 119.4(4) yes . . . C11 C1 C18 122.6(3) yes . . . C1 C2 C3 122.1(5) yes . . . C2 C3 C4 120.6(4) yes . . . C3 C4 C12 120.4(4) yes . . . C6 C5 C14 117.7(4) yes . . . C6 C5 C24 119.5(4) yes . . . C14 C5 C24 122.8(3) yes . . . C5 C6 C7 122.7(5) yes . . . C6 C7 C8 120.4(4) yes . . . C7 C8 C13 120.4(4) yes . . . C11 C9 C13 122.4(4) yes . . . C12 C10 C14 121.6(4) yes . . . C1 C11 C9 122.7(4) yes . . . C1 C11 C12 119.4(3) yes . . . C9 C11 C12 117.8(4) yes . . . C4 C12 C10 120.5(4) yes . . . C4 C12 C11 119.4(4) yes . . . C10 C12 C11 120.1(3) yes . . . C8 C13 C9 120.4(4) yes . . . C8 C13 C14 119.5(4) yes . . . C9 C13 C14 120.0(3) yes . . . C5 C14 C10 122.8(4) yes . . . C5 C14 C13 119.2(3) yes . . . C10 C14 C13 118.0(4) yes . . . N1 C15 C16 121.0(4) yes . . . N1 C15 C20 120.5(4) yes . . . C16 C15 C20 118.4(5) yes . . . C15 C16 C17 120.7(4) yes . . . C16 C17 C18 121.8(4) yes . . . C1 C18 C17 122.8(4) yes . . . C1 C18 C19 120.1(4) yes . . . C17 C18 C19 117.0(4) yes . . . C18 C19 C20 121.2(4) yes . . . C15 C20 C19 120.8(5) yes . . . N2 C21 C22 122.4(3) yes . . . N2 C21 C26 119.9(4) yes . . . C22 C21 C26 117.6(5) yes . . . C21 C22 C23 121.0(4) yes . . . C22 C23 C24 122.2(4) yes . . . C5 C24 C23 123.1(4) yes . . . C5 C24 C25 120.6(3) yes . . . C23 C24 C25 116.3(4) yes . . . C24 C25 C26 121.9(3) yes . . . C21 C26 C25 121.1(4) yes . . . C15 N1 H29A 119.996 no . . . C15 N1 H29B 120.003 no . . . H29A N1 H29B 120.002 no . . . C21 N2 H4A 120.000 no . . . C21 N2 H4B 119.997 no . . . H4A N2 H4B 120.003 no . . . C1 C2 H2 118.947 no . . . C3 C2 H2 118.949 no . . . C2 C3 H3 119.717 no . . . C4 C3 H3 119.707 no . . . C3 C4 H4 119.780 no . . . C12 C4 H4 119.778 no . . . C5 C6 H6 118.651 no . . . C7 C6 H6 118.652 no . . . C6 C7 H7 119.825 no . . . C8 C7 H7 119.822 no . . . C7 C8 H8 119.787 no . . . C13 C8 H8 119.783 no . . . C11 C9 H9 118.792 no . . . C13 C9 H9 118.793 no . . . C12 C10 H5 119.196 no . . . C14 C10 H5 119.187 no . . . C15 C16 H16 119.657 no . . . C17 C16 H16 119.663 no . . . C16 C17 H17 119.076 no . . . C18 C17 H17 119.083 no . . . C18 C19 H19 119.393 no . . . C20 C19 H19 119.402 no . . . C15 C20 H20 119.603 no . . . C19 C20 H20 119.610 no . . . C21 C22 H22 119.515 no . . . C23 C22 H22 119.518 no . . . C22 C23 H23 118.877 no . . . C24 C23 H23 118.883 no . . . C24 C25 H25 119.051 no . . . C26 C25 H25 119.040 no . . . C21 C26 H26 119.469 no . . . C25 C26 H26 119.473 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C2 C1 C11 C9 175.7(3) no . . . . C2 C1 C11 C12 -0.5(5) no . . . . C11 C1 C2 C3 1.0(5) no . . . . C2 C1 C18 C17 128.2(4) no . . . . C2 C1 C18 C19 -49.3(5) no . . . . C18 C1 C2 C3 -179.4(3) no . . . . C11 C1 C18 C17 -52.4(5) no . . . . C11 C1 C18 C19 130.2(4) no . . . . C18 C1 C11 C9 -3.8(5) no . . . . C18 C1 C11 C12 180.0(3) no . . . . C1 C2 C3 C4 -0.6(5) no . . . . C2 C3 C4 C12 -0.4(5) no . . . . C3 C4 C12 C10 -176.6(3) no . . . . C3 C4 C12 C11 0.9(5) no . . . . C6 C5 C14 C10 173.1(3) no . . . . C6 C5 C14 C13 -4.2(5) no . . . . C14 C5 C6 C7 3.5(5) no . . . . C6 C5 C24 C23 129.5(4) no . . . . C6 C5 C24 C25 -48.1(5) no . . . . C24 C5 C6 C7 -178.5(3) no . . . . C14 C5 C24 C23 -52.6(5) no . . . . C14 C5 C24 C25 129.8(4) no . . . . C24 C5 C14 C10 -4.8(5) no . . . . C24 C5 C14 C13 177.9(3) no . . . . C5 C6 C7 C8 0.1(5) no . . . . C6 C7 C8 C13 -3.1(5) no . . . . C7 C8 C13 C9 -173.8(3) no . . . . C7 C8 C13 C14 2.2(5) no . . . . C11 C9 C13 C8 175.2(3) no . . . . C11 C9 C13 C14 -0.8(5) no . . . . C13 C9 C11 C1 -175.9(3) no . . . . C13 C9 C11 C12 0.4(5) no . . . . C12 C10 C14 C5 -176.4(3) no . . . . C12 C10 C14 C13 1.0(5) no . . . . C14 C10 C12 C4 176.1(3) no . . . . C14 C10 C12 C11 -1.4(5) no . . . . C1 C11 C12 C4 -0.4(5) no . . . . C1 C11 C12 C10 177.1(3) no . . . . C9 C11 C12 C4 -176.9(3) no . . . . C9 C11 C12 C10 0.7(5) no . . . . C8 C13 C14 C5 1.5(5) no . . . . C8 C13 C14 C10 -176.0(3) no . . . . C9 C13 C14 C5 177.5(3) no . . . . C9 C13 C14 C10 0.1(5) no . . . . N1 C15 C16 C17 176.4(3) no . . . . N1 C15 C20 C19 -176.6(3) no . . . . C16 C15 C20 C19 1.3(5) no . . . . C20 C15 C16 C17 -1.5(5) no . . . . C15 C16 C17 C18 0.8(5) no . . . . C16 C17 C18 C1 -177.5(3) no . . . . C16 C17 C18 C19 0.1(5) no . . . . C1 C18 C19 C20 177.3(3) no . . . . C17 C18 C19 C20 -0.3(5) no . . . . C18 C19 C20 C15 -0.4(6) no . . . . N2 C21 C22 C23 -177.5(4) no . . . . N2 C21 C26 C25 177.3(3) no . . . . C22 C21 C26 C25 0.5(6) no . . . . C26 C21 C22 C23 -0.7(6) no . . . . C21 C22 C23 C24 0.7(6) no . . . . C22 C23 C24 C5 -178.2(4) no . . . . C22 C23 C24 C25 -0.4(6) no . . . . C5 C24 C25 C26 178.0(3) no . . . . C23 C24 C25 C26 0.2(5) no . . . . C24 C25 C26 C21 -0.2(6) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C1 C4 2.842(7) no . . C2 C12 2.800(7) no . . C2 C19 3.035(6) no . . C3 C11 2.823(5) no . . C5 C8 2.835(7) no . . C6 C13 2.786(7) no . . C6 C25 3.025(7) no . . C7 C14 2.810(5) no . . C9 C10 2.791(7) no . . C9 C17 3.168(7) no . . C9 C18 2.995(7) no . . C10 C23 3.193(7) no . . C10 C24 3.010(7) no . . C11 C14 2.864(7) no . . C11 C17 3.191(7) no . . C12 C13 2.816(5) no . . C14 C23 3.196(7) no . . C15 C18 2.820(7) no . . C16 C19 2.753(6) no . . C17 C20 2.748(7) no . . C21 C24 2.836(7) no . . C22 C25 2.748(5) no . . C23 C26 2.743(7) no . . N1 N2 3.257(6) no . 1_454 N1 C7 3.598(6) no . 2_665 N2 N1 3.257(6) no . 1_656 N2 C4 3.497(5) no . 2_657 N2 C8 3.496(5) no . 1_556 C2 C10 3.478(5) no . 2_656 C3 C10 3.494(5) no . 2_656 C3 C14 3.423(5) no . 2_656 C4 N2 3.497(5) no . 2_657 C4 C11 3.571(5) no . 2_656 C4 C12 3.563(5) no . 2_656 C6 C9 3.584(5) no . 2_666 C7 N1 3.598(6) no . 2_665 C8 N2 3.496(5) no . 1_554 C8 C13 3.588(5) no . 2_666 C8 C14 3.482(5) no . 2_666 C9 C6 3.584(5) no . 2_666 C10 C2 3.478(5) no . 2_656 C10 C3 3.494(5) no . 2_656 C11 C4 3.571(5) no . 2_656 C12 C4 3.563(5) no . 2_656 C12 C12 3.563(5) no . 2_656 C13 C8 3.588(5) no . 2_666 C13 C13 3.575(5) no . 2_666 C14 C3 3.423(5) no . 2_656 C14 C8 3.482(5) no . 2_666 N1 H16 2.6040 no . . N1 H20 2.5865 no . . N2 H22 2.6169 no . . N2 H26 2.5815 no . . C1 H3 3.2917 no . . C1 H9 2.6570 no . . C1 H17 2.6863 no . . C1 H19 2.6391 no . . C2 H4 3.2546 no . . C2 H19 2.8482 no . . C4 H2 3.2414 no . . C4 H5 2.6253 no . . C5 H5 2.6784 no . . C5 H7 3.2771 no . . C5 H25 2.6460 no . . C5 H23 2.6792 no . . C6 H8 3.2464 no . . C6 H25 2.8337 no . . C8 H6 3.2318 no . . C8 H9 2.6029 no . . C9 H8 2.6257 no . . C9 H17 2.8555 no . . C10 H4 2.6416 no . . C10 H23 2.8925 no . . C11 H2 3.2817 no . . C11 H4 3.3203 no . . C11 H5 3.3063 no . . C11 H17 3.0071 no . . C12 H3 3.2698 no . . C12 H9 3.2723 no . . C13 H5 3.2811 no . . C13 H7 3.2577 no . . C14 H6 3.2676 no . . C14 H8 3.3091 no . . C14 H9 3.2936 no . . C14 H23 3.0150 no . . C15 H17 3.2432 no . . C15 H19 3.2509 no . . C16 H9 3.5823 no . . C16 H20 3.2288 no . . C16 H29A 3.2064 no . . C16 H29B 2.5888 no . . C17 H9 2.5683 no . . C17 H19 3.2295 no . . C18 H2 2.6155 no . . C18 H9 2.6557 no . . C18 H16 3.2619 no . . C18 H20 3.2683 no . . C19 H2 2.8175 no . . C19 H17 3.2278 no . . C20 H16 3.2281 no . . C20 H29A 2.5744 no . . C20 H29B 3.1958 no . . C21 H25 3.2537 no . . C21 H23 3.2466 no . . C22 H4A 2.5994 no . . C22 H4B 3.2062 no . . C22 H26 3.2310 no . . C23 H5 2.6137 no . . C23 H25 3.2227 no . . C24 H5 2.6828 no . . C24 H6 2.5899 no . . C24 H22 3.2651 no . . C24 H26 3.2675 no . . C25 H6 2.7887 no . . C25 H23 3.2237 no . . C26 H4A 3.1950 no . . C26 H4B 2.5620 no . . C26 H22 3.2331 no . . H2 H3 2.3329 no . . H2 H19 2.5498 no . . H3 H4 2.2903 no . . H4A H22 2.4626 no . . H4A H26 3.4439 no . . H4B H22 3.4765 no . . H4B H26 2.4036 no . . H4 H5 2.4561 no . . H5 H23 2.4015 no . . H6 H7 2.3262 no . . H6 H25 2.5039 no . . H7 H8 2.2897 no . . H8 H9 2.4328 no . . H9 H17 2.3373 no . . H25 H26 2.2932 no . . H17 H16 2.2994 no . . H19 H20 2.3170 no . . H16 H29A 3.4649 no . . H16 H29B 2.4402 no . . H22 H23 2.2996 no . . H20 H29A 2.4185 no . . H20 H29B 3.4480 no . . N1 H4B 2.4971 no . 1_454 N1 H4 3.4087 no . 1_554 N1 H5 3.4197 no . 1_554 N1 H7 2.9234 no . 2_665 N1 H8 3.0809 no . 2_665 N1 H23 3.2666 no . 1_554 N1 H26 3.2559 no . 1_454 N2 H3 3.0931 no . 2_657 N2 H4 2.7733 no . 2_657 N2 H8 3.2377 no . 1_556 N2 H9 3.4011 no . 1_556 N2 H20 2.8558 no . 2_656 N2 H29A 3.0663 no . 1_656 N2 H29B 3.2931 no . 1_656 C1 H5 3.5466 no . 2_656 C1 H25 3.0669 no . 1_455 C1 H26 3.4043 no . 1_455 C2 H2 3.2045 no . 2_556 C2 H5 3.4403 no . 2_656 C2 H25 3.2616 no . 1_455 C2 H26 3.1602 no . 1_455 C3 H4A 3.2283 no . 2_657 C3 H4B 3.4255 no . 2_657 C3 H26 3.0774 no . 1_455 C4 H4A 3.0172 no . 2_657 C4 H4B 3.4888 no . 2_657 C4 H20 3.5461 no . 1_556 C4 H26 3.2356 no . 1_455 C4 H29A 2.8812 no . 1_556 C5 H2 3.5735 no . 2_656 C5 H9 3.5880 no . 2_666 C5 H17 3.2642 no . 2_666 C6 H9 3.5887 no . 2_666 C6 H25 3.5318 no . 2_766 C6 H17 2.8870 no . 2_666 C6 H16 3.4323 no . 1_655 C7 H16 3.2779 no . 1_655 C7 H26 3.3383 no . 2_766 C7 H29B 2.9887 no . 2_665 C8 H4A 2.9783 no . 1_554 C8 H23 3.4952 no . 2_666 C8 H29B 3.0716 no . 2_665 C9 H4A 2.8312 no . 1_554 C9 H4 3.5343 no . 2_656 C9 H22 3.3822 no . 1_554 C10 H29A 3.3274 no . 1_556 C11 H4 3.5141 no . 2_656 C11 H26 3.5596 no . 1_455 C12 H26 3.4837 no . 1_455 C12 H29A 3.1737 no . 1_556 C13 H3 3.4214 no . 2_656 C13 H4A 3.0117 no . 1_554 C14 H3 3.3504 no . 2_656 C14 H8 3.4558 no . 2_666 C15 H3 3.2637 no . 2_556 C15 H4B 3.2959 no . 1_454 C15 H22 3.4604 no . 1_554 C15 H23 3.2102 no . 1_554 C16 H6 3.4335 no . 1_455 C16 H7 3.5225 no . 1_455 C16 H22 3.2229 no . 1_554 C16 H23 3.4836 no . 1_554 C17 H6 3.3460 no . 1_455 C17 H6 3.3293 no . 2_666 C17 H25 2.8732 no . 1_455 C17 H22 3.1539 no . 1_554 C18 H2 3.4597 no . 2_556 C18 H25 3.0814 no . 1_455 C18 H22 3.3218 no . 1_554 C19 H2 3.4251 no . 2_556 C19 H22 3.5101 no . 1_554 C20 H3 3.1998 no . 2_556 C20 H4 3.5164 no . 1_554 C20 H22 3.5750 no . 1_554 C21 H19 3.1754 no . 2_656 C21 H16 3.1964 no . 2_666 C21 H20 2.9497 no . 2_656 C22 H9 3.3950 no . 1_556 C22 H19 3.2395 no . 2_656 C22 H16 3.2841 no . 2_666 C22 H20 3.5473 no . 2_656 C23 H8 3.5667 no . 2_666 C23 H17 3.5077 no . 2_666 C23 H19 3.1819 no . 2_656 C23 H16 3.4689 no . 2_666 C24 H2 3.4994 no . 2_656 C24 H17 3.1538 no . 2_666 C24 H19 3.0548 no . 2_656 C24 H16 3.5981 no . 2_666 C25 H2 3.2066 no . 2_656 C25 H6 3.0915 no . 2_766 C25 H7 3.5040 no . 2_766 C25 H17 3.4905 no . 1_655 C25 H17 3.5560 no . 2_666 C25 H19 2.9406 no . 2_656 C25 H16 3.4847 no . 2_666 C26 H6 3.5006 no . 2_766 C26 H7 2.9341 no . 2_766 C26 H19 3.0039 no . 2_656 C26 H16 3.2957 no . 2_666 C26 H20 3.2930 no . 2_656 C26 H29A 3.4225 no . 1_656 H2 C2 3.2045 no . 2_556 H2 C5 3.5735 no . 2_656 H2 C18 3.4597 no . 2_556 H2 C19 3.4251 no . 2_556 H2 C24 3.4994 no . 2_656 H2 C25 3.2066 no . 2_656 H2 H2 2.4531 no . 2_556 H2 H25 3.3209 no . 1_455 H2 H25 2.9284 no . 2_656 H2 H19 3.5481 no . 2_556 H2 H26 3.5820 no . 1_455 H3 N2 3.0931 no . 2_657 H3 C13 3.4214 no . 2_656 H3 C14 3.3504 no . 2_656 H3 C15 3.2637 no . 2_556 H3 C20 3.1998 no . 2_556 H3 H4A 2.7726 no . 2_657 H3 H4B 2.7582 no . 2_657 H3 H20 3.4010 no . 2_556 H3 H26 3.4550 no . 1_455 H4A C3 3.2283 no . 2_657 H4A C4 3.0172 no . 2_657 H4A C8 2.9783 no . 1_556 H4A C9 2.8312 no . 1_556 H4A C13 3.0117 no . 1_556 H4A H3 2.7726 no . 2_657 H4A H4 2.3409 no . 2_657 H4A H8 2.8279 no . 1_556 H4A H9 2.6446 no . 1_556 H4A H20 3.1240 no . 2_656 H4B N1 2.4971 no . 1_656 H4B C3 3.4255 no . 2_657 H4B C4 3.4888 no . 2_657 H4B C15 3.2959 no . 1_656 H4B H3 2.7582 no . 2_657 H4B H4 2.8891 no . 2_657 H4B H20 2.9887 no . 2_656 H4B H29A 2.2576 no . 1_656 H4B H29B 2.6899 no . 1_656 H4 N1 3.4087 no . 1_556 H4 N2 2.7733 no . 2_657 H4 C9 3.5343 no . 2_656 H4 C11 3.5141 no . 2_656 H4 C20 3.5164 no . 1_556 H4 H4A 2.3409 no . 2_657 H4 H4B 2.8891 no . 2_657 H4 H20 2.7199 no . 1_556 H4 H29A 2.6612 no . 1_556 H5 N1 3.4197 no . 1_556 H5 C1 3.5466 no . 2_656 H5 C2 3.4403 no . 2_656 H5 H19 2.8821 no . 2_656 H5 H20 3.4997 no . 1_556 H5 H29A 3.1247 no . 1_556 H6 C16 3.4335 no . 1_655 H6 C17 3.3460 no . 1_655 H6 C17 3.3293 no . 2_666 H6 C25 3.0915 no . 2_766 H6 C26 3.5006 no . 2_766 H6 H6 2.6981 no . 2_766 H6 H25 2.7557 no . 2_766 H6 H17 2.9804 no . 1_655 H6 H17 2.4271 no . 2_666 H6 H16 3.1567 no . 1_655 H6 H26 3.4828 no . 2_766 H7 N1 2.9234 no . 2_665 H7 C16 3.5225 no . 1_655 H7 C25 3.5040 no . 2_766 H7 C26 2.9341 no . 2_766 H7 H25 3.5472 no . 2_766 H7 H16 2.8831 no . 1_655 H7 H26 2.5484 no . 2_766 H7 H29A 2.9045 no . 2_665 H7 H29B 2.3383 no . 2_665 H8 N1 3.0809 no . 2_665 H8 N2 3.2377 no . 1_554 H8 C14 3.4558 no . 2_666 H8 C23 3.5667 no . 2_666 H8 H4A 2.8279 no . 1_554 H8 H22 3.4685 no . 1_554 H8 H23 2.7220 no . 2_666 H8 H29A 3.4555 no . 2_665 H8 H29B 2.5140 no . 2_665 H9 N2 3.4011 no . 1_554 H9 C5 3.5880 no . 2_666 H9 C6 3.5887 no . 2_666 H9 C22 3.3950 no . 1_554 H9 H4A 2.6446 no . 1_554 H9 H22 2.5652 no . 1_554 H9 H23 3.3941 no . 2_666 H25 C1 3.0669 no . 1_655 H25 C2 3.2616 no . 1_655 H25 C6 3.5318 no . 2_766 H25 C17 2.8732 no . 1_655 H25 C18 3.0814 no . 1_655 H25 H2 3.3209 no . 1_655 H25 H2 2.9284 no . 2_656 H25 H6 2.7557 no . 2_766 H25 H7 3.5472 no . 2_766 H25 H17 2.6123 no . 1_655 H25 H19 3.3882 no . 2_656 H17 C5 3.2642 no . 2_666 H17 C6 2.8870 no . 2_666 H17 C23 3.5077 no . 2_666 H17 C24 3.1538 no . 2_666 H17 C25 3.4905 no . 1_455 H17 C25 3.5560 no . 2_666 H17 H6 2.9804 no . 1_455 H17 H6 2.4271 no . 2_666 H17 H25 2.6123 no . 1_455 H17 H22 3.5278 no . 1_554 H19 C21 3.1754 no . 2_656 H19 C22 3.2395 no . 2_656 H19 C23 3.1819 no . 2_656 H19 C24 3.0548 no . 2_656 H19 C25 2.9406 no . 2_656 H19 C26 3.0039 no . 2_656 H19 H2 3.5481 no . 2_556 H19 H5 2.8821 no . 2_656 H19 H25 3.3882 no . 2_656 H19 H26 3.4775 no . 2_656 H16 C6 3.4323 no . 1_455 H16 C7 3.2779 no . 1_455 H16 C21 3.1964 no . 2_666 H16 C22 3.2841 no . 2_666 H16 C23 3.4689 no . 2_666 H16 C24 3.5981 no . 2_666 H16 C25 3.4847 no . 2_666 H16 C26 3.2957 no . 2_666 H16 H6 3.1567 no . 1_455 H16 H7 2.8831 no . 1_455 H16 H23 3.5826 no . 1_554 H22 C9 3.3822 no . 1_556 H22 C15 3.4604 no . 1_556 H22 C16 3.2229 no . 1_556 H22 C17 3.1539 no . 1_556 H22 C18 3.3218 no . 1_556 H22 C19 3.5101 no . 1_556 H22 C20 3.5750 no . 1_556 H22 H8 3.4685 no . 1_556 H22 H9 2.5652 no . 1_556 H22 H17 3.5278 no . 1_556 H23 N1 3.2666 no . 1_556 H23 C8 3.4952 no . 2_666 H23 C15 3.2102 no . 1_556 H23 C16 3.4836 no . 1_556 H23 H8 2.7220 no . 2_666 H23 H9 3.3941 no . 2_666 H23 H16 3.5826 no . 1_556 H23 H29A 3.5922 no . 1_556 H23 H29B 3.3760 no . 1_556 H20 N2 2.8558 no . 2_656 H20 C4 3.5461 no . 1_554 H20 C21 2.9497 no . 2_656 H20 C22 3.5473 no . 2_656 H20 C26 3.2930 no . 2_656 H20 H3 3.4010 no . 2_556 H20 H4A 3.1240 no . 2_656 H20 H4B 2.9887 no . 2_656 H20 H4 2.7199 no . 1_554 H20 H5 3.4997 no . 1_554 H20 H26 3.4174 no . 2_656 H26 N1 3.2559 no . 1_656 H26 C1 3.4043 no . 1_655 H26 C2 3.1602 no . 1_655 H26 C3 3.0774 no . 1_655 H26 C4 3.2356 no . 1_655 H26 C7 3.3383 no . 2_766 H26 C11 3.5596 no . 1_655 H26 C12 3.4837 no . 1_655 H26 H2 3.5820 no . 1_655 H26 H3 3.4550 no . 1_655 H26 H6 3.4828 no . 2_766 H26 H7 2.5484 no . 2_766 H26 H19 3.4775 no . 2_656 H26 H20 3.4174 no . 2_656 H26 H29A 2.6678 no . 1_656 H26 H29B 3.2426 no . 1_656 H29A N2 3.0663 no . 1_454 H29A C4 2.8812 no . 1_554 H29A C10 3.3274 no . 1_554 H29A C12 3.1737 no . 1_554 H29A C26 3.4225 no . 1_454 H29A H4B 2.2576 no . 1_454 H29A H4 2.6612 no . 1_554 H29A H5 3.1247 no . 1_554 H29A H7 2.9045 no . 2_665 H29A H8 3.4555 no . 2_665 H29A H23 3.5922 no . 1_554 H29A H26 2.6678 no . 1_454 H29B N2 3.2931 no . 1_454 H29B C7 2.9887 no . 2_665 H29B C8 3.0716 no . 2_665 H29B H4B 2.6899 no . 1_454 H29B H7 2.3383 no . 2_665 H29B H8 2.5140 no . 2_665 H29B H23 3.3760 no . 1_554 H29B H26 3.2426 no . 1_454 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 941418' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_15BAPA_HCl_MeOH #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C15 H17 Cl N O' _chemical_formula_moiety 'C15 H17 Cl N O' _chemical_formula_weight 262.76 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 5.71305(18) _cell_length_b 9.0278(4) _cell_length_c 26.9086(11) _cell_angle_alpha 90.0000 _cell_angle_beta 90.1610(19) _cell_angle_gamma 90.0000 _cell_volume 1387.84(9) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3891 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 67.50 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour red _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.257 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 556.00 _exptl_absorpt_coefficient_mu 2.328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.312 _exptl_absorpt_correction_T_max 0.792 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 14089 _diffrn_reflns_av_R_equivalents 0.1490 _diffrn_reflns_theta_max 68.10 _diffrn_reflns_theta_full 68.10 _diffrn_measured_fraction_theta_max 0.995 _diffrn_measured_fraction_theta_full 0.995 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2516 _reflns_number_gt 1054 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1181 _refine_ls_wR_factor_ref 0.3949 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2516 _refine_ls_number_parameters 163 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.630 _refine_diff_density_min -0.510 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.031 0.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.049 0.032 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.364 0.702 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl1 Cl 0.8071(3) 0.66143(19) 0.78187(7) 0.0988(9) Uani 1.0 4 d . . . O1 O 0.5054(11) 0.8744(6) 0.7150(3) 0.120(2) Uani 1.0 4 d . . . N1 N 0.6844(11) 0.3378(6) 0.6757(2) 0.0921(19) Uani 1.0 4 d . . . C1 C 0.7943(11) 0.7446(6) 0.5155(3) 0.0742(17) Uani 1.0 4 d . . . C2 C 0.9792(12) 0.7223(7) 0.4823(3) 0.0827(19) Uani 1.0 4 d . . . C3 C 1.0123(12) 0.8177(7) 0.4417(3) 0.0773(18) Uani 1.0 4 d . . . C4 C 0.8698(12) 0.9354(8) 0.4335(3) 0.0826(19) Uani 1.0 4 d . . . C5 C 0.4607(12) 0.9084(7) 0.5421(3) 0.0793(19) Uani 1.0 4 d . . . C6 C 0.6424(11) 0.8725(6) 0.5079(3) 0.0734(18) Uani 1.0 4 d . . . C7 C 0.6800(12) 0.9662(6) 0.4661(3) 0.0740(17) Uani 1.0 4 d . . . C8 C 0.7083(12) 0.4375(7) 0.6366(3) 0.0777(18) Uani 1.0 4 d . . . C9 C 0.5323(12) 0.4573(7) 0.6020(3) 0.0831(19) Uani 1.0 4 d . . . C10 C 0.5544(12) 0.5565(7) 0.5641(3) 0.0784(18) Uani 1.0 4 d . . . C11 C 0.7565(12) 0.6423(7) 0.5581(3) 0.0719(17) Uani 1.0 4 d . . . C12 C 0.9327(13) 0.6217(6) 0.5929(3) 0.0765(18) Uani 1.0 4 d . . . C13 C 0.9119(11) 0.5221(7) 0.6317(3) 0.0788(19) Uani 1.0 4 d . . . C14 C 0.6798(13) 0.9268(8) 0.6779(3) 0.105(3) Uani 1.0 4 d . . . C15 C 0.3387(13) 0.7652(8) 0.6939(3) 0.099(3) Uani 1.0 4 d . . . H1A H 0.5564 0.2864 0.6787 0.1105 Uiso 1.0 4 calc R . . H1B H 0.7973 0.3269 0.6971 0.1105 Uiso 1.0 4 calc R . . H13 H 1.0347 0.5113 0.6547 0.0946 Uiso 1.0 4 calc R . . H12 H 1.0711 0.6775 0.5901 0.0918 Uiso 1.0 4 calc R . . H10 H 0.4303 0.5677 0.5414 0.0940 Uiso 1.0 4 calc R . . H9 H 0.3943 0.4012 0.6047 0.0997 Uiso 1.0 4 calc R . . H2 H 1.0824 0.6426 0.4872 0.0993 Uiso 1.0 4 calc R . . H3 H 1.1364 0.7995 0.4197 0.0928 Uiso 1.0 4 calc R . . H4 H 0.8965 0.9972 0.4060 0.0991 Uiso 1.0 4 calc R . . H5 H 0.4350 0.8482 0.5700 0.0951 Uiso 1.0 4 calc R . . H14A H 0.7771 0.8444 0.6676 0.1258 Uiso 1.0 4 calc R . . H14B H 0.7773 1.0030 0.6928 0.1258 Uiso 1.0 4 calc R . . H14C H 0.5987 0.9672 0.6492 0.1258 Uiso 1.0 4 calc R . . H15A H 0.4246 0.6805 0.6812 0.1187 Uiso 1.0 4 calc R . . H15B H 0.2511 0.8107 0.6670 0.1187 Uiso 1.0 4 calc R . . H15C H 0.2314 0.7327 0.7195 0.1187 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.0876(16) 0.0917(14) 0.1170(18) 0.0004(9) -0.0074(12) 0.0058(10) O1 0.130(5) 0.109(4) 0.121(5) -0.018(4) -0.014(4) -0.011(4) N1 0.096(5) 0.087(4) 0.094(5) -0.003(3) -0.012(4) 0.015(4) C1 0.073(5) 0.065(4) 0.085(5) 0.004(4) -0.011(4) 0.003(3) C2 0.070(5) 0.077(4) 0.101(6) 0.007(4) 0.004(4) -0.004(4) C3 0.069(5) 0.078(4) 0.085(5) 0.003(4) 0.001(4) -0.000(4) C4 0.084(5) 0.071(4) 0.093(5) 0.004(4) -0.004(4) 0.006(4) C5 0.080(5) 0.069(4) 0.089(5) 0.003(4) 0.001(4) -0.005(4) C6 0.079(5) 0.063(4) 0.078(5) 0.009(3) -0.012(4) -0.005(3) C7 0.079(5) 0.065(4) 0.078(4) 0.003(3) 0.004(4) 0.005(4) C8 0.078(5) 0.071(4) 0.084(5) 0.005(4) -0.005(4) -0.001(4) C9 0.074(5) 0.070(4) 0.106(6) -0.013(4) -0.006(4) -0.002(4) C10 0.080(5) 0.069(4) 0.086(5) 0.002(4) -0.007(4) -0.000(4) C11 0.077(5) 0.066(4) 0.073(5) 0.002(3) -0.001(4) 0.007(3) C12 0.090(5) 0.060(4) 0.080(5) 0.006(3) -0.013(4) 0.001(3) C13 0.072(5) 0.072(4) 0.092(5) 0.005(4) -0.012(4) -0.006(4) C14 0.091(6) 0.094(5) 0.130(7) -0.003(5) 0.015(5) -0.005(5) C15 0.088(6) 0.093(5) 0.115(6) -0.012(4) -0.011(5) -0.015(5) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 O1 C14 1.490(10) yes . . O1 C15 1.484(10) yes . . N1 C8 1.391(9) yes . . C1 C2 1.400(10) yes . . C1 C6 1.458(9) yes . . C1 C11 1.488(9) yes . . C2 C3 1.403(10) yes . . C3 C4 1.356(9) yes . . C4 C7 1.425(10) yes . . C5 C6 1.426(9) yes . . C5 C7 1.406(9) yes . 3_676 C6 C7 1.424(9) yes . . C8 C9 1.379(10) yes . . C8 C13 1.398(9) yes . . C9 C10 1.365(10) yes . . C10 C11 1.400(9) yes . . C11 C12 1.387(10) yes . . C12 C13 1.382(9) yes . . N1 H1A 0.870 no . . N1 H1B 0.870 no . . C2 H2 0.940 no . . C3 H3 0.940 no . . C4 H4 0.940 no . . C5 H5 0.940 no . . C9 H9 0.940 no . . C10 H10 0.940 no . . C12 H12 0.940 no . . C13 H13 0.940 no . . C14 H14A 0.970 no . . C14 H14B 0.970 no . . C14 H14C 0.970 no . . C15 H15A 0.970 no . . C15 H15B 0.970 no . . C15 H15C 0.970 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 C14 O1 C15 112.6(6) yes . . . C2 C1 C6 118.3(6) yes . . . C2 C1 C11 120.9(6) yes . . . C6 C1 C11 120.7(6) yes . . . C1 C2 C3 120.8(6) yes . . . C2 C3 C4 121.7(7) yes . . . C3 C4 C7 120.7(6) yes . . . C6 C5 C7 119.9(6) yes . . 3_676 C1 C6 C5 121.6(6) yes . . . C1 C6 C7 119.3(6) yes . . . C5 C6 C7 119.1(6) yes . . . C4 C7 C5 119.8(6) yes . . 3_676 C4 C7 C6 119.2(6) yes . . . C5 C7 C6 121.0(6) yes 3_676 . . N1 C8 C9 121.4(6) yes . . . N1 C8 C13 120.6(6) yes . . . C9 C8 C13 118.0(6) yes . . . C8 C9 C10 121.4(6) yes . . . C9 C10 C11 121.8(6) yes . . . C1 C11 C10 123.6(6) yes . . . C1 C11 C12 119.9(6) yes . . . C10 C11 C12 116.4(6) yes . . . C11 C12 C13 122.2(6) yes . . . C8 C13 C12 120.0(6) yes . . . C8 N1 H1A 119.998 no . . . C8 N1 H1B 120.001 no . . . H1A N1 H1B 120.001 no . . . C1 C2 H2 119.600 no . . . C3 C2 H2 119.603 no . . . C2 C3 H3 119.141 no . . . C4 C3 H3 119.166 no . . . C3 C4 H4 119.667 no . . . C7 C4 H4 119.680 no . . . C6 C5 H5 120.038 no . . . C7 C5 H5 120.040 no 3_676 . . C8 C9 H9 119.297 no . . . C10 C9 H9 119.300 no . . . C9 C10 H10 119.085 no . . . C11 C10 H10 119.086 no . . . C11 C12 H12 118.877 no . . . C13 C12 H12 118.878 no . . . C8 C13 H13 119.979 no . . . C12 C13 H13 119.989 no . . . O1 C14 H14A 109.481 no . . . O1 C14 H14B 109.483 no . . . O1 C14 H14C 109.473 no . . . H14A C14 H14B 109.468 no . . . H14A C14 H14C 109.456 no . . . H14B C14 H14C 109.465 no . . . O1 C15 H15A 109.472 no . . . O1 C15 H15B 109.469 no . . . O1 C15 H15C 109.471 no . . . H15A C15 H15B 109.473 no . . . H15A C15 H15C 109.474 no . . . H15B C15 H15C 109.469 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C2 C1 C6 C5 -175.6(5) no . . . . C2 C1 C6 C7 2.8(9) no . . . . C6 C1 C2 C3 -2.3(9) no . . . . C2 C1 C11 C10 -117.9(7) no . . . . C2 C1 C11 C12 58.3(8) no . . . . C11 C1 C2 C3 179.0(5) no . . . . C6 C1 C11 C10 63.5(8) no . . . . C6 C1 C11 C12 -120.3(6) no . . . . C11 C1 C6 C5 3.1(9) no . . . . C11 C1 C6 C7 -178.5(5) no . . . . C1 C2 C3 C4 1.0(10) no . . . . C2 C3 C4 C7 -0.0(10) no . . . . C3 C4 C7 C5 177.8(6) no . . . 3_676 C3 C4 C7 C6 0.6(10) no . . . . C6 C5 C7 C4 176.4(5) no . . 3_676 3_676 C6 C5 C7 C6 -0.8(9) no . . 3_676 3_676 C7 C5 C6 C1 179.1(5) no 3_676 . . . C7 C5 C6 C7 0.7(9) no 3_676 . . . C1 C6 C7 C4 -2.0(9) no . . . . C1 C6 C7 C5 -179.2(5) no . . . 3_676 C5 C6 C7 C4 176.5(5) no . . . . C5 C6 C7 C5 -0.7(9) no . . . 3_676 N1 C8 C9 C10 179.1(6) no . . . . N1 C8 C13 C12 -179.4(5) no . . . . C9 C8 C13 C12 -0.2(9) no . . . . C13 C8 C9 C10 -0.2(9) no . . . . C8 C9 C10 C11 0.5(10) no . . . . C9 C10 C11 C1 175.9(6) no . . . . C9 C10 C11 C12 -0.4(9) no . . . . C1 C11 C12 C13 -176.4(5) no . . . . C10 C11 C12 C13 0.1(9) no . . . . C11 C12 C13 C8 0.2(9) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C1 C4 2.833(9) no . . C2 C7 2.820(9) no . . C2 C12 3.125(10) no . . C3 C6 2.812(10) no . . C5 C5 2.841(9) no . 3_676 C5 C10 3.275(9) no . . C5 C11 2.968(9) no . . C6 C6 2.851(9) no . 3_676 C6 C10 3.268(9) no . . C7 C7 2.819(9) no . 3_676 C8 C11 2.822(9) no . . C9 C12 2.739(10) no . . C10 C13 2.749(9) no . . Cl1 O1 3.144(6) no . . Cl1 O1 3.148(6) no . 2_646 Cl1 N1 3.427(7) no . 2_656 Cl1 N1 3.502(7) no . 2_756 O1 Cl1 3.144(6) no . . O1 Cl1 3.148(6) no . 2_656 O1 N1 3.155(9) no . 2_656 N1 Cl1 3.427(7) no . 2_646 N1 Cl1 3.502(7) no . 2_746 N1 O1 3.155(9) no . 2_646 N1 C15 3.575(10) no . 2_646 C2 C5 3.599(9) no . 1_655 C3 C8 3.509(9) no . 3_766 C5 C2 3.599(9) no . 1_455 C8 C3 3.509(9) no . 3_766 C15 N1 3.575(10) no . 2_656 N1 H13 2.6042 no . . N1 H9 2.5893 no . . C1 H12 2.6241 no . . C1 H10 2.7141 no . . C1 H3 3.2771 no . . C1 H5 2.6948 no . . C2 H12 2.9757 no . . C2 H4 3.2547 no . . C4 H2 3.2472 no . . C4 H5 2.6187 no . 3_676 C5 H10 3.0807 no . . C5 H4 2.6197 no . 3_676 C6 H10 3.1397 no . . C6 H2 3.3085 no . . C6 H4 3.3052 no . . C6 H5 3.3088 no . 3_676 C7 H3 3.2624 no . . C7 H5 3.3071 no . . C8 H12 3.2507 no . . C8 H10 3.2326 no . . C9 H1A 2.5786 no . . C9 H1B 3.1937 no . . C9 H13 3.2344 no . . C10 H12 3.2227 no . . C10 H5 2.7246 no . . C11 H13 3.2659 no . . C11 H9 3.2570 no . . C11 H2 2.6688 no . . C11 H5 2.6337 no . . C12 H10 3.2219 no . . C12 H2 2.9791 no . . C12 H5 3.5545 no . . C13 H1A 3.2045 no . . C13 H1B 2.5771 no . . C13 H9 3.2331 no . . C14 H15A 2.6602 no . . C14 H15B 2.6794 no . . C14 H15C 3.3017 no . . C15 H14A 2.7006 no . . C15 H14B 3.2998 no . . C15 H14C 2.6426 no . . H1A H13 3.4660 no . . H1A H9 2.4259 no . . H1B H13 2.4328 no . . H1B H9 3.4504 no . . H13 H12 2.3060 no . . H12 H2 2.7882 no . . H10 H9 2.2818 no . . H10 H5 2.6477 no . . H2 H3 2.3255 no . . H3 H4 2.2797 no . . H4 H5 2.4411 no . 3_676 H14A H15A 2.5261 no . . H14A H15B 3.0202 no . . H14A H15C 3.5653 no . . H14B H15A 3.5532 no . . H14B H15B 3.5379 no . . H14C H15A 2.9035 no . . H14C H15B 2.4840 no . . H14C H15C 3.5328 no . . Cl1 H1A 2.5932 no . 2_656 Cl1 H1B 2.7662 no . 2_756 Cl1 H14A 3.4940 no . . Cl1 H14B 2.8534 no . 2_746 Cl1 H14C 3.4510 no . 2_646 Cl1 H15A 3.4791 no . . Cl1 H15B 3.4686 no . 2_646 Cl1 H15C 3.0214 no . 1_655 O1 H1A 2.9909 no . 2_656 O1 H1B 2.9647 no . 2_656 N1 H3 3.0298 no . 3_766 N1 H14B 3.1031 no . 1_545 N1 H14C 3.4552 no . 1_545 N1 H15A 3.4350 no . . N1 H15C 3.0129 no . 2_646 C1 H10 3.4521 no . 3_666 C1 H2 3.5660 no . 3_766 C2 H10 3.3314 no . 1_655 C2 H10 3.5669 no . 3_666 C2 H9 3.3526 no . 3_666 C2 H2 3.4137 no . 3_766 C3 H9 3.2923 no . 3_666 C4 H12 3.5685 no . 3_776 C4 H9 3.5431 no . 3_666 C4 H14C 3.5859 no . 3_676 C5 H12 3.3148 no . 1_455 C5 H2 3.5483 no . 1_455 C5 H14C 3.0343 no . . C7 H14C 3.5362 no . 3_676 C8 H3 2.7685 no . 3_766 C8 H15A 2.9824 no . . C9 H13 3.2178 no . 1_455 C9 H12 3.3157 no . 1_455 C9 H2 3.3839 no . 3_766 C9 H3 3.0501 no . 3_766 C9 H15A 2.9985 no . . C10 H12 3.0522 no . 1_455 C10 H10 3.0520 no . 3_666 C10 H2 3.4814 no . 1_455 C10 H2 3.0753 no . 3_766 C10 H15A 3.4282 no . . C11 H10 3.4455 no . 3_666 C11 H2 2.9916 no . 3_766 C11 H14A 3.4681 no . . C12 H10 3.2045 no . 1_655 C12 H9 3.3187 no . 1_655 C12 H2 3.2171 no . 3_766 C12 H4 3.5754 no . 3_776 C12 H5 3.5781 no . 1_655 C12 H14A 2.9794 no . . C12 H15B 3.1890 no . 1_655 C13 H9 3.0540 no . 1_655 C13 H2 3.5276 no . 3_766 C13 H3 3.2269 no . 3_766 C13 H14A 3.1614 no . . C13 H15A 3.4051 no . . C13 H15A 3.5187 no . 1_655 C13 H15B 3.3818 no . 1_655 C13 H15C 3.5373 no . 1_655 C14 H1A 3.3220 no . 1_565 C14 H4 3.3844 no . 3_776 C14 H5 3.2963 no . . C14 H15B 3.4413 no . 1_655 C15 H1A 3.4859 no . 2_656 C15 H1B 3.0882 no . 2_656 C15 H13 3.0609 no . 1_455 C15 H12 3.2762 no . 1_455 C15 H5 3.4606 no . . C15 H14A 3.3604 no . 1_455 H1A Cl1 2.5932 no . 2_646 H1A O1 2.9909 no . 2_646 H1A C14 3.3220 no . 1_545 H1A C15 3.4859 no . 2_646 H1A H3 3.2723 no . 3_766 H1A H14B 2.8774 no . 1_545 H1A H14C 2.9984 no . 1_545 H1A H15C 3.0316 no . 2_646 H1B Cl1 2.7662 no . 2_746 H1B O1 2.9647 no . 2_646 H1B C15 3.0882 no . 2_646 H1B H3 3.3651 no . 3_766 H1B H14B 2.9288 no . 1_545 H1B H15C 2.4050 no . 2_646 H13 C9 3.2178 no . 1_655 H13 C15 3.0609 no . 1_655 H13 H9 2.6531 no . 1_655 H13 H3 3.5807 no . 3_766 H13 H14A 3.3660 no . . H13 H15A 2.7925 no . 1_655 H13 H15B 2.9907 no . 1_655 H13 H15C 2.8794 no . 1_655 H12 C4 3.5685 no . 3_776 H12 C5 3.3148 no . 1_655 H12 C9 3.3157 no . 1_655 H12 C10 3.0522 no . 1_655 H12 C15 3.2762 no . 1_655 H12 H10 2.6329 no . 1_655 H12 H9 3.1273 no . 1_655 H12 H4 2.9444 no . 3_776 H12 H5 2.6452 no . 1_655 H12 H14A 3.0753 no . . H12 H15A 3.1723 no . 1_655 H12 H15B 2.6022 no . 1_655 H10 C1 3.4521 no . 3_666 H10 C2 3.3314 no . 1_455 H10 C2 3.5669 no . 3_666 H10 C10 3.0520 no . 3_666 H10 C11 3.4455 no . 3_666 H10 C12 3.2045 no . 1_455 H10 H12 2.6329 no . 1_455 H10 H10 2.6623 no . 3_666 H10 H2 2.5524 no . 1_455 H10 H2 3.5724 no . 3_666 H10 H2 3.4573 no . 3_766 H9 C2 3.3526 no . 3_666 H9 C3 3.2923 no . 3_666 H9 C4 3.5431 no . 3_666 H9 C12 3.3187 no . 1_455 H9 C13 3.0540 no . 1_455 H9 H13 2.6531 no . 1_455 H9 H12 3.1273 no . 1_455 H9 H3 3.5904 no . 3_666 H9 H3 3.3031 no . 3_766 H9 H15A 3.2608 no . . H2 C1 3.5660 no . 3_766 H2 C2 3.4137 no . 3_766 H2 C5 3.5483 no . 1_655 H2 C9 3.3839 no . 3_766 H2 C10 3.4814 no . 1_655 H2 C10 3.0753 no . 3_766 H2 C11 2.9916 no . 3_766 H2 C12 3.2171 no . 3_766 H2 C13 3.5276 no . 3_766 H2 H10 2.5524 no . 1_655 H2 H10 3.5724 no . 3_666 H2 H10 3.4573 no . 3_766 H2 H2 2.8272 no . 3_766 H2 H5 3.5280 no . 1_655 H3 N1 3.0298 no . 3_766 H3 C8 2.7685 no . 3_766 H3 C9 3.0501 no . 3_766 H3 C13 3.2269 no . 3_766 H3 H1A 3.2723 no . 3_766 H3 H1B 3.3651 no . 3_766 H3 H13 3.5807 no . 3_766 H3 H9 3.5904 no . 3_666 H3 H9 3.3031 no . 3_766 H3 H14B 3.5472 no . 3_776 H3 H14C 3.1909 no . 3_776 H4 C12 3.5754 no . 3_776 H4 C14 3.3844 no . 3_776 H4 H12 2.9444 no . 3_776 H4 H14A 3.0756 no . 3_776 H4 H14B 3.2492 no . 3_776 H4 H14C 3.2081 no . 3_676 H4 H14C 3.2634 no . 3_776 H4 H15B 2.7494 no . 3_676 H5 C12 3.5781 no . 1_455 H5 C14 3.2963 no . . H5 C15 3.4606 no . . H5 H12 2.6452 no . 1_455 H5 H2 3.5280 no . 1_455 H5 H14A 3.2686 no . . H5 H14C 2.5613 no . . H5 H15A 3.3537 no . . H5 H15B 2.8351 no . . H14A Cl1 3.4940 no . . H14A C11 3.4681 no . . H14A C12 2.9794 no . . H14A C13 3.1614 no . . H14A C15 3.3604 no . 1_655 H14A H13 3.3660 no . . H14A H12 3.0753 no . . H14A H4 3.0756 no . 3_776 H14A H5 3.2686 no . . H14A H15B 2.7252 no . 1_655 H14A H15C 3.1120 no . 1_655 H14B Cl1 2.8534 no . 2_756 H14B N1 3.1031 no . 1_565 H14B H1A 2.8774 no . 1_565 H14B H1B 2.9288 no . 1_565 H14B H3 3.5472 no . 3_776 H14B H4 3.2492 no . 3_776 H14B H15B 3.2913 no . 1_655 H14B H15C 3.1426 no . 2_656 H14C Cl1 3.4510 no . 2_656 H14C N1 3.4552 no . 1_565 H14C C4 3.5859 no . 3_676 H14C C5 3.0343 no . . H14C C7 3.5362 no . 3_676 H14C H1A 2.9984 no . 1_565 H14C H3 3.1909 no . 3_776 H14C H4 3.2081 no . 3_676 H14C H4 3.2634 no . 3_776 H14C H5 2.5613 no . . H15A Cl1 3.4791 no . . H15A N1 3.4350 no . . H15A C8 2.9824 no . . H15A C9 2.9985 no . . H15A C10 3.4282 no . . H15A C13 3.5187 no . 1_455 H15A C13 3.4051 no . . H15A H13 2.7925 no . 1_455 H15A H12 3.1723 no . 1_455 H15A H9 3.2608 no . . H15A H5 3.3537 no . . H15B Cl1 3.4686 no . 2_656 H15B C12 3.1890 no . 1_455 H15B C13 3.3818 no . 1_455 H15B C14 3.4413 no . 1_455 H15B H13 2.9907 no . 1_455 H15B H12 2.6022 no . 1_455 H15B H4 2.7494 no . 3_676 H15B H5 2.8351 no . . H15B H14A 2.7252 no . 1_455 H15B H14B 3.2913 no . 1_455 H15C Cl1 3.0214 no . 1_455 H15C N1 3.0129 no . 2_656 H15C C13 3.5373 no . 1_455 H15C H1A 3.0316 no . 2_656 H15C H1B 2.4050 no . 2_656 H15C H13 2.8794 no . 1_455 H15C H14A 3.1120 no . 1_455 H15C H14B 3.1426 no . 2_646 #============================================================================== #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 941419' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_15BAPA_MeSO3H #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H28 N2 O6 S2' _chemical_formula_moiety 'C28 H28 N2 O6 S2' _chemical_formula_weight 552.66 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 5.7607(9) _cell_length_b 8.8385(8) _cell_length_c 13.309(2) _cell_angle_alpha 72.933(19) _cell_angle_beta 84.68(3) _cell_angle_gamma 83.64(3) _cell_volume 642.52(17) _cell_formula_units_Z 1 _cell_measurement_reflns_used 1110 _cell_measurement_theta_min 3.21 _cell_measurement_theta_max 27.49 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 290.00 _exptl_absorpt_coefficient_mu 0.255 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.987 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku XtaLAB mini' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 13.653 _diffrn_reflns_number 6691 _diffrn_reflns_av_R_equivalents 0.0799 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2931 _reflns_number_gt 1620 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.1732 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2931 _refine_ls_number_parameters 173 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0636P)^2^+0.1458P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.770 _refine_diff_density_min -0.300 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 S1 S 0.10465(18) 0.70242(12) 0.06780(8) 0.0309(3) Uani 1.0 2 d . . . O1 O -0.1409(5) 0.7612(4) 0.0609(3) 0.0431(8) Uani 1.0 2 d . . . O2 O 0.2037(5) 0.6769(4) -0.0320(2) 0.0413(8) Uani 1.0 2 d . . . O3 O 0.1456(5) 0.5630(3) 0.1564(2) 0.0399(8) Uani 1.0 2 d . . . N1 N 0.3326(6) 1.2939(4) 0.1114(3) 0.0322(8) Uani 1.0 2 d . . . C1 C 0.2929(7) 0.7524(5) 0.4760(3) 0.0279(9) Uani 1.0 2 d . . . C2 C 0.4377(7) 0.7386(5) 0.5552(3) 0.0329(10) Uani 1.0 2 d . . . C3 C 0.4362(7) 0.6096(5) 0.6476(4) 0.0357(11) Uani 1.0 2 d . . . C4 C 0.2879(7) 0.4964(5) 0.6617(3) 0.0309(10) Uani 1.0 2 d . . . C5 C -0.0061(7) 0.3765(5) 0.5944(3) 0.0300(10) Uani 1.0 2 d . . . C6 C 0.1423(7) 0.6274(5) 0.4868(3) 0.0247(9) Uani 1.0 2 d . . . C7 C 0.1389(7) 0.5008(5) 0.5821(3) 0.0268(9) Uani 1.0 2 d . . . C8 C 0.3207(7) 1.1569(5) 0.2059(3) 0.0271(9) Uani 1.0 2 d . . . C9 C 0.1167(7) 1.1354(5) 0.2689(3) 0.0327(10) Uani 1.0 2 d . . . C10 C 0.1051(7) 1.0035(5) 0.3551(3) 0.0329(10) Uani 1.0 2 d . . . C11 C 0.2993(7) 0.8930(5) 0.3808(3) 0.0285(9) Uani 1.0 2 d . . . C12 C 0.5035(7) 0.9185(5) 0.3175(3) 0.0334(10) Uani 1.0 2 d . . . C13 C 0.5154(7) 1.0501(5) 0.2295(3) 0.0330(10) Uani 1.0 2 d . . . C14 C 0.2515(8) 0.8491(5) 0.0903(4) 0.0435(12) Uani 1.0 2 d . . . H1A H 0.2682 1.3812 0.1270 0.0386 Uiso 1.0 2 calc R . . H1B H 0.2552 1.2774 0.0612 0.0386 Uiso 1.0 2 calc R . . H1C H 0.4815 1.3061 0.0886 0.0386 Uiso 1.0 2 calc R . . H9 H -0.0124 1.2094 0.2534 0.0392 Uiso 1.0 2 calc R . . H10 H -0.0338 0.9878 0.3969 0.0395 Uiso 1.0 2 calc R . . H12 H 0.6347 0.8467 0.3340 0.0401 Uiso 1.0 2 calc R . . H13 H 0.6532 1.0660 0.1870 0.0396 Uiso 1.0 2 calc R . . H2 H 0.5396 0.8163 0.5477 0.0394 Uiso 1.0 2 calc R . . H3 H 0.5384 0.6026 0.6992 0.0428 Uiso 1.0 2 calc R . . H4 H 0.2836 0.4147 0.7244 0.0370 Uiso 1.0 2 calc R . . H5 H -0.0112 0.2957 0.6576 0.0360 Uiso 1.0 2 calc R . . H14A H 0.4154 0.8149 0.0942 0.0522 Uiso 1.0 2 calc R . . H14B H 0.1907 0.8685 0.1554 0.0522 Uiso 1.0 2 calc R . . H14C H 0.2299 0.9450 0.0336 0.0522 Uiso 1.0 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.0317(6) 0.0276(6) 0.0312(6) -0.0033(5) -0.0051(4) -0.0040(4) O1 0.0309(17) 0.0435(19) 0.053(2) 0.0008(14) -0.0072(14) -0.0111(15) O2 0.0445(19) 0.052(2) 0.0303(17) -0.0134(16) 0.0031(13) -0.0145(14) O3 0.056(2) 0.0280(16) 0.0303(17) 0.0006(15) -0.0082(14) 0.0007(13) N1 0.034(2) 0.0301(19) 0.032(2) -0.0050(16) -0.0064(15) -0.0056(15) C1 0.029(3) 0.022(2) 0.032(3) -0.0027(17) -0.0032(17) -0.0058(17) C2 0.035(3) 0.029(3) 0.035(3) -0.0108(19) -0.0055(19) -0.0065(18) C3 0.038(3) 0.036(3) 0.036(3) -0.006(2) -0.0154(19) -0.0106(19) C4 0.038(3) 0.028(3) 0.024(3) -0.0058(19) -0.0051(18) -0.0018(17) C5 0.032(3) 0.024(3) 0.031(3) -0.0046(18) -0.0055(18) -0.0022(17) C6 0.024(2) 0.025(2) 0.024(2) -0.0009(17) -0.0016(16) -0.0040(16) C7 0.024(2) 0.025(2) 0.029(3) -0.0013(17) -0.0013(16) -0.0054(17) C8 0.035(3) 0.020(2) 0.025(3) -0.0050(18) -0.0079(17) -0.0023(16) C9 0.027(3) 0.025(3) 0.041(3) 0.0020(18) -0.0043(18) -0.0030(18) C10 0.029(3) 0.032(3) 0.032(3) -0.0049(19) 0.0020(17) -0.0018(18) C11 0.033(3) 0.021(2) 0.032(3) -0.0108(18) -0.0072(17) -0.0042(17) C12 0.030(3) 0.023(3) 0.042(3) -0.0010(18) -0.0083(19) -0.0006(18) C13 0.026(3) 0.034(3) 0.038(3) -0.0073(19) -0.0014(18) -0.0078(19) C14 0.049(3) 0.038(3) 0.049(3) -0.008(3) -0.004(3) -0.018(2) #============================================================================== _computing_data_collection DTREK _computing_cell_refinement DTREK _computing_data_reduction DTREK _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 O1 1.454(3) yes . . S1 O2 1.466(3) yes . . S1 O3 1.449(3) yes . . S1 C14 1.733(6) yes . . N1 C8 1.471(4) yes . . C1 C2 1.373(6) yes . . C1 C6 1.446(6) yes . . C1 C11 1.492(5) yes . . C2 C3 1.410(5) yes . . C3 C4 1.347(6) yes . . C4 C7 1.414(6) yes . . C5 C6 1.403(6) yes . 2_566 C5 C7 1.416(6) yes . . C6 C7 1.425(5) yes . . C8 C9 1.376(6) yes . . C8 C13 1.380(6) yes . . C9 C10 1.378(5) yes . . C10 C11 1.398(6) yes . . C11 C12 1.382(6) yes . . C12 C13 1.390(5) yes . . N1 H1A 0.890 no . . N1 H1B 0.890 no . . N1 H1C 0.890 no . . C2 H2 0.930 no . . C3 H3 0.930 no . . C4 H4 0.930 no . . C5 H5 0.930 no . . C9 H9 0.930 no . . C10 H10 0.930 no . . C12 H12 0.930 no . . C13 H13 0.930 no . . C14 H14A 0.960 no . . C14 H14B 0.960 no . . C14 H14C 0.960 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O1 S1 O2 110.93(19) yes . . . O1 S1 O3 112.90(17) yes . . . O1 S1 C14 107.1(2) yes . . . O2 S1 O3 112.18(17) yes . . . O2 S1 C14 107.4(2) yes . . . O3 S1 C14 105.9(2) yes . . . C2 C1 C6 118.5(3) yes . . . C2 C1 C11 119.4(4) yes . . . C6 C1 C11 122.0(4) yes . . . C1 C2 C3 121.8(4) yes . . . C2 C3 C4 120.6(4) yes . . . C3 C4 C7 120.6(4) yes . . . C6 C5 C7 121.4(3) yes 2_566 . . C1 C6 C5 122.4(3) yes . . 2_566 C1 C6 C7 118.6(4) yes . . . C5 C6 C7 119.0(4) yes 2_566 . . C4 C7 C5 120.5(4) yes . . . C4 C7 C6 119.8(4) yes . . . C5 C7 C6 119.6(4) yes . . . N1 C8 C9 120.1(4) yes . . . N1 C8 C13 119.1(4) yes . . . C9 C8 C13 120.8(3) yes . . . C8 C9 C10 119.5(4) yes . . . C9 C10 C11 120.9(4) yes . . . C1 C11 C10 121.8(4) yes . . . C1 C11 C12 119.7(4) yes . . . C10 C11 C12 118.5(3) yes . . . C11 C12 C13 120.8(4) yes . . . C8 C13 C12 119.3(4) yes . . . C8 N1 H1A 109.466 no . . . C8 N1 H1B 109.475 no . . . C8 N1 H1C 109.467 no . . . H1A N1 H1B 109.481 no . . . H1A N1 H1C 109.464 no . . . H1B N1 H1C 109.475 no . . . C1 C2 H2 119.101 no . . . C3 C2 H2 119.096 no . . . C2 C3 H3 119.705 no . . . C4 C3 H3 119.697 no . . . C3 C4 H4 119.709 no . . . C7 C4 H4 119.713 no . . . C6 C5 H5 119.320 no 2_566 . . C7 C5 H5 119.313 no . . . C8 C9 H9 120.242 no . . . C10 C9 H9 120.238 no . . . C9 C10 H10 119.533 no . . . C11 C10 H10 119.522 no . . . C11 C12 H12 119.579 no . . . C13 C12 H12 119.574 no . . . C8 C13 H13 120.328 no . . . C12 C13 H13 120.328 no . . . S1 C14 H14A 109.476 no . . . S1 C14 H14B 109.474 no . . . S1 C14 H14C 109.467 no . . . H14A C14 H14B 109.470 no . . . H14A C14 H14C 109.469 no . . . H14B C14 H14C 109.472 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 C2 C1 C6 C5 -173.5(4) no . . . 2_566 C2 C1 C6 C7 4.3(6) no . . . . C6 C1 C2 C3 -2.5(6) no . . . . C2 C1 C11 C10 -116.4(5) no . . . . C2 C1 C11 C12 61.6(6) no . . . . C11 C1 C2 C3 178.9(4) no . . . . C6 C1 C11 C10 65.1(6) no . . . . C6 C1 C11 C12 -116.9(4) no . . . . C11 C1 C6 C5 5.0(6) no . . . 2_566 C11 C1 C6 C7 -177.2(3) no . . . . C1 C2 C3 C4 -1.2(6) no . . . . C2 C3 C4 C7 3.0(6) no . . . . C3 C4 C7 C5 176.0(4) no . . . . C3 C4 C7 C6 -1.1(6) no . . . . C6 C5 C7 C4 -175.3(3) no 2_566 . . . C6 C5 C7 C6 1.8(6) no 2_566 . . . C7 C5 C6 C1 -179.6(3) no . . 2_566 2_566 C7 C5 C6 C7 -1.8(6) no . . 2_566 2_566 C1 C6 C7 C4 -2.5(5) no . . . . C1 C6 C7 C5 -179.7(3) no . . . . C5 C6 C7 C4 175.3(3) no 2_566 . . . C5 C6 C7 C5 -1.8(6) no 2_566 . . . N1 C8 C9 C10 177.6(4) no . . . . N1 C8 C13 C12 -178.6(4) no . . . . C9 C8 C13 C12 0.6(7) no . . . . C13 C8 C9 C10 -1.6(7) no . . . . C8 C9 C10 C11 1.3(7) no . . . . C9 C10 C11 C1 177.8(4) no . . . . C9 C10 C11 C12 -0.2(7) no . . . . C1 C11 C12 C13 -178.8(4) no . . . . C10 C11 C12 C13 -0.7(7) no . . . . C11 C12 C13 C8 0.5(7) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 C1 C4 2.820(5) no . . C2 C7 2.784(6) no . . C2 C10 3.541(6) no . . C2 C12 3.104(6) no . . C3 C6 2.808(6) no . . C5 C5 2.805(5) no . 2_566 C5 C10 3.330(6) no . 2_566 C5 C11 2.993(6) no . 2_566 C6 C6 2.851(6) no . 2_566 C6 C10 3.265(5) no . . C6 C12 3.597(6) no . . C7 C7 2.831(6) no . 2_566 C8 C11 2.775(5) no . . C9 C12 2.766(6) no . . C10 C13 2.762(6) no . . S1 N1 3.600(4) no . 1_545 O1 N1 2.821(5) no . 2_575 O1 C14 3.511(6) no . 1_455 O1 C14 3.464(5) no . 2_575 O2 N1 3.400(4) no . 1_545 O2 N1 3.316(5) no . 2_575 O2 N1 2.791(5) no . 2_675 O2 C8 3.570(5) no . 2_675 O2 C13 3.422(5) no . 2_675 O3 N1 2.706(5) no . 1_545 O3 C3 3.599(5) no . 2_666 O3 C4 3.285(5) no . 2_566 O3 C5 3.519(5) no . 2_566 O3 C8 3.502(5) no . 1_545 N1 S1 3.600(4) no . 1_565 N1 O1 2.821(5) no . 2_575 N1 O2 3.400(4) no . 1_565 N1 O2 3.316(5) no . 2_575 N1 O2 2.791(5) no . 2_675 N1 O3 2.706(5) no . 1_565 C3 O3 3.599(5) no . 2_666 C4 O3 3.285(5) no . 2_566 C5 O3 3.519(5) no . 2_566 C8 O2 3.570(5) no . 2_675 C8 O3 3.502(5) no . 1_565 C8 C14 3.570(7) no . . C13 O2 3.422(5) no . 2_675 C13 C14 3.458(8) no . . C14 O1 3.511(6) no . 1_655 C14 O1 3.464(5) no . 2_575 C14 C8 3.570(7) no . . C14 C13 3.458(8) no . . O1 H14A 3.3789 no . . O1 H14B 2.7710 no . . O1 H14C 2.7588 no . . O2 H14A 2.7773 no . . O2 H14B 3.3933 no . . O2 H14C 2.7788 no . . O3 H14A 2.7399 no . . O3 H14B 2.7375 no . . O3 H14C 3.3592 no . . N1 H9 2.6237 no . . N1 H13 2.6104 no . . C1 H10 2.6820 no . . C1 H12 2.6251 no . . C1 H3 3.2609 no . . C1 H5 2.6658 no . 2_566 C2 H12 2.9726 no . . C2 H4 3.2346 no . . C4 H2 3.2219 no . . C4 H5 2.6215 no . . C5 H10 3.1710 no . 2_566 C5 H4 2.6264 no . . C6 H10 3.1436 no . . C6 H2 3.2664 no . . C6 H4 3.2937 no . . C6 H5 3.2911 no . . C7 H3 3.2374 no . . C7 H5 3.2755 no . 2_566 C8 H10 3.2164 no . . C8 H12 3.2288 no . . C9 H1A 2.5987 no . . C9 H1B 2.7619 no . . C9 H1C 3.1765 no . . C9 H13 3.2346 no . . C10 H12 3.2313 no . . C10 H5 2.8131 no . 2_566 C11 H9 3.2543 no . . C11 H13 3.2480 no . . C11 H2 2.6051 no . . C11 H5 2.6582 no . 2_566 C12 H10 3.2286 no . . C12 H2 2.9486 no . . C12 H5 3.5191 no . 2_566 C13 H1A 3.0901 no . . C13 H1B 2.9351 no . . C13 H1C 2.4811 no . . C13 H9 3.2347 no . . H1A H9 2.5076 no . . H1A H13 3.3126 no . . H1B H9 2.8020 no . . H1B H13 3.0782 no . . H1C H9 3.4518 no . . H1C H13 2.3113 no . . H9 H10 2.3047 no . . H10 H5 2.7854 no . 2_566 H12 H13 2.3186 no . . H12 H2 2.7850 no . . H2 H3 2.3234 no . . H3 H4 2.2688 no . . H4 H5 2.4510 no . . S1 H1A 2.7931 no . 1_545 S1 H1B 2.7708 no . 2_575 S1 H1C 3.0260 no . 2_675 S1 H4 3.3772 no . 2_566 S1 H14C 3.4541 no . 2_575 O1 H1A 3.2815 no . 2_575 O1 H1B 1.9405 no . 2_575 O1 H1C 3.1374 no . 2_575 O1 H4 2.9149 no . 2_566 O1 H14A 2.5691 no . 1_455 O1 H14C 2.5485 no . 2_575 O2 H1A 2.8514 no . 1_545 O2 H1A 3.2524 no . 2_575 O2 H1A 3.2310 no . 2_675 O2 H1B 3.3703 no . 1_545 O2 H1B 2.6768 no . 2_575 O2 H1B 3.1611 no . 2_675 O2 H1C 3.4790 no . 1_545 O2 H1C 1.9027 no . 2_675 O2 H9 3.0861 no . 2_575 O2 H13 2.7293 no . 2_675 O3 H1A 1.8165 no . 1_545 O3 H1B 3.1226 no . 1_545 O3 H1C 3.1010 no . 1_545 O3 H9 3.2101 no . 1_545 O3 H3 2.7491 no . 2_666 O3 H4 2.8310 no . 2_566 O3 H5 3.0878 no . 2_566 N1 H3 3.0979 no . 2_676 N1 H14A 3.3197 no . 2_675 C1 H10 3.3787 no . 2_576 C2 H9 3.4622 no . 2_576 C2 H10 3.3250 no . 2_576 C3 H9 3.1675 no . 2_576 C4 H9 3.3216 no . 2_576 C4 H12 3.0006 no . 2_666 C5 H12 2.7779 no . 2_666 C5 H3 3.5524 no . 1_455 C5 H14B 3.5393 no . 2_566 C7 H12 3.1223 no . 2_666 C8 H2 3.5272 no . 2_676 C8 H3 2.9858 no . 2_676 C8 H14B 3.0059 no . . C8 H14C 3.4645 no . . C9 H13 3.1613 no . 1_455 C9 H2 3.4285 no . 2_676 C9 H3 3.3524 no . 2_676 C9 H14B 3.1271 no . . C10 H10 3.3104 no . 2_576 C10 H12 3.2476 no . 1_455 C10 H13 3.4828 no . 1_455 C10 H2 3.2891 no . 2_676 C10 H14B 3.1970 no . . C11 H10 3.5829 no . 2_576 C11 H2 3.2399 no . 2_676 C11 H14B 3.1930 no . . C12 H10 3.1399 no . 1_655 C12 H2 3.3212 no . 2_676 C12 H4 3.2446 no . 2_666 C12 H5 3.2913 no . 2_666 C12 H14A 3.4504 no . . C12 H14B 3.0909 no . . C13 H9 3.2794 no . 1_655 C13 H10 3.4704 no . 1_655 C13 H2 3.4762 no . 2_676 C13 H3 3.4442 no . 2_676 C13 H14A 3.2477 no . . C13 H14B 2.9972 no . . C13 H14C 3.5945 no . . C14 H1B 3.5979 no . 2_675 C14 H1C 3.2694 no . 2_675 C14 H13 3.5458 no . 2_675 C14 H5 3.4389 no . 2_566 C14 H14C 3.4194 no . 2_575 H1A S1 2.7931 no . 1_565 H1A O1 3.2815 no . 2_575 H1A O2 2.8514 no . 1_565 H1A O2 3.2524 no . 2_575 H1A O2 3.2310 no . 2_675 H1A O3 1.8165 no . 1_565 H1A H3 2.7056 no . 2_676 H1B S1 2.7708 no . 2_575 H1B O1 1.9405 no . 2_575 H1B O2 3.3703 no . 1_565 H1B O2 2.6768 no . 2_575 H1B O2 3.1611 no . 2_675 H1B O3 3.1226 no . 1_565 H1B C14 3.5979 no . 2_675 H1B H14A 2.9097 no . 2_675 H1B H14B 3.5104 no . . H1B H14C 3.0862 no . . H1C S1 3.0260 no . 2_675 H1C O1 3.1374 no . 2_575 H1C O2 3.4790 no . 1_565 H1C O2 1.9027 no . 2_675 H1C O3 3.1010 no . 1_565 H1C C14 3.2694 no . 2_675 H1C H1C 3.5607 no . 2_685 H1C H3 3.1454 no . 2_676 H1C H14A 2.9227 no . 2_675 H1C H14C 3.3380 no . 2_675 H9 O2 3.0861 no . 2_575 H9 O3 3.2101 no . 1_565 H9 C2 3.4622 no . 2_576 H9 C3 3.1675 no . 2_576 H9 C4 3.3216 no . 2_576 H9 C13 3.2794 no . 1_455 H9 H13 2.7595 no . 1_455 H9 H3 3.3894 no . 2_576 H9 H3 3.5431 no . 2_676 H9 H4 3.5925 no . 2_576 H10 C1 3.3787 no . 2_576 H10 C2 3.3250 no . 2_576 H10 C10 3.3104 no . 2_576 H10 C11 3.5829 no . 2_576 H10 C12 3.1399 no . 1_455 H10 C13 3.4704 no . 1_455 H10 H10 2.8808 no . 2_576 H10 H12 2.7090 no . 1_455 H10 H13 3.3253 no . 1_455 H10 H2 3.2390 no . 1_455 H10 H2 3.3564 no . 2_576 H12 C4 3.0006 no . 2_666 H12 C5 2.7779 no . 2_666 H12 C7 3.1223 no . 2_666 H12 C10 3.2476 no . 1_655 H12 H10 2.7090 no . 1_655 H12 H4 2.6288 no . 2_666 H12 H5 2.3786 no . 2_666 H13 O2 2.7293 no . 2_675 H13 C9 3.1613 no . 1_655 H13 C10 3.4828 no . 1_655 H13 C14 3.5458 no . 2_675 H13 H9 2.7595 no . 1_655 H13 H10 3.3253 no . 1_655 H13 H14A 3.3039 no . . H13 H14B 3.4622 no . . H13 H14B 3.4356 no . 1_655 H13 H14C 2.9786 no . 2_675 H2 C8 3.5272 no . 2_676 H2 C9 3.4285 no . 2_676 H2 C10 3.2891 no . 2_676 H2 C11 3.2399 no . 2_676 H2 C12 3.3212 no . 2_676 H2 C13 3.4762 no . 2_676 H2 H10 3.2390 no . 1_655 H2 H10 3.3564 no . 2_576 H2 H2 3.1178 no . 2_676 H3 O3 2.7491 no . 2_666 H3 N1 3.0979 no . 2_676 H3 C5 3.5524 no . 1_655 H3 C8 2.9858 no . 2_676 H3 C9 3.3524 no . 2_676 H3 C13 3.4442 no . 2_676 H3 H1A 2.7056 no . 2_676 H3 H1C 3.1454 no . 2_676 H3 H9 3.3894 no . 2_576 H3 H9 3.5431 no . 2_676 H4 S1 3.3772 no . 2_566 H4 O1 2.9149 no . 2_566 H4 O3 2.8310 no . 2_566 H4 C12 3.2446 no . 2_666 H4 H9 3.5925 no . 2_576 H4 H12 2.6288 no . 2_666 H4 H14A 3.1738 no . 2_666 H5 O3 3.0878 no . 2_566 H5 C12 3.2913 no . 2_666 H5 C14 3.4389 no . 2_566 H5 H12 2.3786 no . 2_666 H5 H14B 2.6656 no . 2_566 H14A O1 2.5691 no . 1_655 H14A N1 3.3197 no . 2_675 H14A C12 3.4504 no . . H14A C13 3.2477 no . . H14A H1B 2.9097 no . 2_675 H14A H1C 2.9227 no . 2_675 H14A H13 3.3039 no . . H14A H4 3.1738 no . 2_666 H14A H14C 3.1258 no . 2_675 H14B C5 3.5393 no . 2_566 H14B C8 3.0059 no . . H14B C9 3.1271 no . . H14B C10 3.1970 no . . H14B C11 3.1930 no . . H14B C12 3.0909 no . . H14B C13 2.9972 no . . H14B H1B 3.5104 no . . H14B H13 3.4356 no . 1_455 H14B H13 3.4622 no . . H14B H5 2.6656 no . 2_566 H14B H14C 3.5681 no . 2_575 H14C S1 3.4541 no . 2_575 H14C O1 2.5485 no . 2_575 H14C C8 3.4645 no . . H14C C13 3.5945 no . . H14C C14 3.4194 no . 2_575 H14C H1B 3.0862 no . . H14C H1C 3.3380 no . 2_675 H14C H13 2.9786 no . 2_675 H14C H14A 3.1258 no . 2_675 H14C H14B 3.5681 no . 2_575 H14C H14C 2.8495 no . 2_575 H14C H14C 3.3281 no . 2_675 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O3 . . 1_565 2.706(5) 0.890 1.817 178.0 no N1 H1B O1 . . 2_575 2.821(5) 0.890 1.940 169.8 no N1 H1C O2 . . 2_675 2.791(5) 0.890 1.903 175.3 no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 941420' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_15BAPA_EtSO3H #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C15 H16 N O3 S' _chemical_formula_moiety 'C15 H16 N O3 S' _chemical_formula_weight 290.36 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 16.6824(4) _cell_length_b 9.3186(3) _cell_length_c 9.3783(3) _cell_angle_alpha 90.0000 _cell_angle_beta 100.1035(14) _cell_angle_gamma 90.0000 _cell_volume 1435.31(6) _cell_formula_units_Z 4 _cell_measurement_reflns_used 8461 _cell_measurement_theta_min 4.75 _cell_measurement_theta_max 68.20 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.340 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 612.00 _exptl_absorpt_coefficient_mu 2.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'ABSCOR (Rigaku, 1995)' _exptl_absorpt_correction_T_min 0.462 _exptl_absorpt_correction_T_max 0.902 #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 14333 _diffrn_reflns_av_R_equivalents 0.1413 _diffrn_reflns_theta_max 68.21 _diffrn_reflns_theta_full 68.21 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2614 _reflns_number_gt 1149 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1230 _refine_ls_wR_factor_ref 0.4006 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 2614 _refine_ls_number_parameters 182 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1577P)^2^+2.8927P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.520 _refine_diff_density_min -0.380 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.031 0.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.333 0.557 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.049 0.032 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 S1 S 0.53628(16) -0.0498(3) 0.7733(3) 0.0844(9) Uani 1.0 4 d . . . O1 O 0.4518(4) -0.0774(7) 0.7884(7) 0.097(2) Uani 1.0 4 d . . . O2 O 0.5509(4) -0.0794(8) 0.6289(7) 0.102(2) Uani 1.0 4 d . . . O3 O 0.5629(5) 0.0967(7) 0.8176(7) 0.108(3) Uani 1.0 4 d . . . N1 N 0.5970(5) 0.2018(8) 0.5346(7) 0.088(3) Uani 1.0 4 d . . . C1 C 0.9365(7) 0.1187(13) 0.7240(12) 0.104(4) Uani 1.0 4 d . . . C2 C 0.9924(8) 0.1640(14) 0.6356(12) 0.120(4) Uani 1.0 4 d . . . C3 C 1.0775(8) 0.1521(16) 0.6833(13) 0.134(5) Uani 1.0 4 d . . . C4 C 1.1074(8) 0.0992(16) 0.8154(13) 0.135(5) Uani 1.0 4 d . . . C5 C 0.9156(7) 0.0086(13) 0.9541(12) 0.107(4) Uani 1.0 4 d . . . C6 C 0.9697(7) 0.0592(12) 0.8612(11) 0.102(4) Uani 1.0 4 d . . . C7 C 1.0526(7) 0.0456(13) 0.9101(11) 0.104(4) Uani 1.0 4 d . . . C8 C 0.6828(6) 0.1791(10) 0.5795(10) 0.076(3) Uani 1.0 4 d . . . C9 C 0.7186(7) 0.0668(13) 0.5335(15) 0.132(5) Uani 1.0 4 d . . . C10 C 0.8025(8) 0.0444(13) 0.5827(16) 0.136(5) Uani 1.0 4 d . . . C11 C 0.8479(6) 0.1396(12) 0.6714(10) 0.088(3) Uani 1.0 4 d . . . C12 C 0.8079(7) 0.2489(16) 0.7182(16) 0.150(6) Uani 1.0 4 d . . . C13 C 0.7276(7) 0.2687(14) 0.6721(15) 0.139(5) Uani 1.0 4 d . . . C14 C 0.5979(7) -0.1647(12) 0.8929(12) 0.114(4) Uani 1.0 4 d . . . C15 C 0.6861(8) -0.1463(15) 0.8875(17) 0.163(6) Uani 1.0 4 d . . . H1A H 0.5719 0.1166 0.5162 0.1058 Uiso 1.0 4 calc R . . H1B H 0.5884 0.2560 0.4539 0.1058 Uiso 1.0 4 calc R . . H1C H 0.5769 0.2470 0.6055 0.1058 Uiso 1.0 4 calc R . . H2 H 0.9726 0.2027 0.5436 0.1444 Uiso 1.0 4 calc R . . H9 H 0.6884 0.0019 0.4683 0.1580 Uiso 1.0 4 calc R . . H10 H 0.8274 -0.0384 0.5532 0.1629 Uiso 1.0 4 calc R . . H12 H 0.8365 0.3139 0.7852 0.1800 Uiso 1.0 4 calc R . . H13 H 0.7022 0.3485 0.7064 0.1673 Uiso 1.0 4 calc R . . H3 H 1.1135 0.1814 0.6221 0.1608 Uiso 1.0 4 calc R . . H4 H 1.1640 0.0965 0.8476 0.1625 Uiso 1.0 4 calc R . . H15 H 0.8589 0.0122 0.9228 0.1279 Uiso 1.0 4 calc R . . H14A H 0.5889 -0.1461 0.9917 0.1365 Uiso 1.0 4 calc R . . H14B H 0.5822 -0.2643 0.8687 0.1365 Uiso 1.0 4 calc R . . H15A H 0.7023 -0.0483 0.9129 0.1959 Uiso 1.0 4 calc R . . H15B H 0.6956 -0.1670 0.7905 0.1959 Uiso 1.0 4 calc R . . H15C H 0.7178 -0.2117 0.9557 0.1959 Uiso 1.0 4 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.1006(19) 0.0727(15) 0.0769(16) -0.0057(13) 0.0074(12) -0.0001(12) O1 0.099(5) 0.084(5) 0.106(5) -0.003(4) 0.016(4) 0.009(4) O2 0.112(5) 0.109(5) 0.084(5) -0.028(4) 0.017(4) -0.020(4) O3 0.144(6) 0.075(4) 0.101(5) -0.024(4) 0.016(5) -0.008(4) N1 0.102(6) 0.089(6) 0.068(5) -0.004(5) -0.000(4) -0.003(4) C1 0.091(7) 0.134(10) 0.087(7) 0.019(7) 0.015(6) -0.009(7) C2 0.123(10) 0.161(12) 0.078(7) 0.015(8) 0.020(7) 0.027(7) C3 0.098(9) 0.212(15) 0.095(8) 0.010(9) 0.025(7) 0.048(9) C4 0.103(9) 0.213(15) 0.092(9) 0.028(9) 0.021(7) 0.030(9) C5 0.092(7) 0.142(10) 0.087(8) 0.014(7) 0.019(6) 0.009(7) C6 0.108(8) 0.122(9) 0.074(7) 0.013(7) 0.010(6) -0.002(6) C7 0.087(8) 0.148(10) 0.074(7) 0.004(7) 0.003(6) 0.012(7) C8 0.079(6) 0.069(6) 0.077(6) -0.000(5) 0.003(5) 0.008(5) C9 0.099(9) 0.118(10) 0.173(12) -0.002(7) 0.011(8) -0.078(9) C10 0.106(10) 0.094(9) 0.201(14) 0.011(7) 0.011(9) -0.038(9) C11 0.086(7) 0.106(8) 0.071(6) 0.013(6) 0.009(5) 0.006(6) C12 0.094(8) 0.144(11) 0.198(14) 0.008(8) -0.011(8) -0.089(11) C13 0.083(8) 0.128(10) 0.196(13) 0.017(7) -0.005(8) -0.051(10) C14 0.099(8) 0.106(8) 0.125(9) -0.007(6) -0.010(7) 0.013(7) C15 0.097(9) 0.141(12) 0.236(17) -0.007(8) -0.015(10) 0.060(11) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 O1 1.464(8) yes . . S1 O2 1.445(8) yes . . S1 O3 1.473(7) yes . . S1 C14 1.748(11) yes . . N1 C8 1.435(11) yes . . C1 C2 1.416(18) yes . . C1 C6 1.421(15) yes . . C1 C11 1.487(14) yes . . C2 C3 1.416(17) yes . . C3 C4 1.345(17) yes . . C4 C7 1.469(18) yes . . C5 C6 1.439(17) yes . . C5 C7 1.386(15) yes . 3_757 C6 C7 1.384(16) yes . . C8 C9 1.314(16) yes . . C8 C13 1.336(15) yes . . C9 C10 1.411(17) yes . . C10 C11 1.353(16) yes . . C11 C12 1.334(18) yes . . C12 C13 1.346(16) yes . . C14 C15 1.490(17) yes . . N1 H1A 0.900 no . . N1 H1B 0.900 no . . N1 H1C 0.900 no . . C2 H2 0.940 no . . C3 H3 0.940 no . . C4 H4 0.940 no . . C5 H15 0.940 no . . C9 H9 0.940 no . . C10 H10 0.940 no . . C12 H12 0.940 no . . C13 H13 0.940 no . . C14 H14A 0.980 no . . C14 H14B 0.980 no . . C15 H15A 0.970 no . . C15 H15B 0.970 no . . C15 H15C 0.970 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O1 S1 O2 112.4(4) yes . . . O1 S1 O3 112.5(5) yes . . . O1 S1 C14 107.4(5) yes . . . O2 S1 O3 110.4(5) yes . . . O2 S1 C14 107.9(5) yes . . . O3 S1 C14 105.8(5) yes . . . C2 C1 C6 117.0(10) yes . . . C2 C1 C11 119.0(10) yes . . . C6 C1 C11 123.9(11) yes . . . C1 C2 C3 121.2(10) yes . . . C2 C3 C4 120.5(12) yes . . . C3 C4 C7 120.8(11) yes . . . C6 C5 C7 119.7(10) yes . . 3_757 C1 C6 C5 119.3(10) yes . . . C1 C6 C7 122.9(11) yes . . . C5 C6 C7 117.7(10) yes . . . C4 C7 C5 120.1(10) yes . . 3_757 C4 C7 C6 117.4(10) yes . . . C5 C7 C6 122.5(11) yes 3_757 . . N1 C8 C9 120.5(9) yes . . . N1 C8 C13 120.9(9) yes . . . C9 C8 C13 118.5(10) yes . . . C8 C9 C10 119.5(11) yes . . . C9 C10 C11 121.3(12) yes . . . C1 C11 C10 122.3(11) yes . . . C1 C11 C12 121.1(10) yes . . . C10 C11 C12 116.4(11) yes . . . C11 C12 C13 121.7(12) yes . . . C8 C13 C12 122.3(13) yes . . . S1 C14 C15 112.4(9) yes . . . C8 N1 H1A 109.464 no . . . C8 N1 H1B 109.462 no . . . C8 N1 H1C 109.466 no . . . H1A N1 H1B 109.478 no . . . H1A N1 H1C 109.477 no . . . H1B N1 H1C 109.480 no . . . C1 C2 H2 119.388 no . . . C3 C2 H2 119.385 no . . . C2 C3 H3 119.736 no . . . C4 C3 H3 119.741 no . . . C3 C4 H4 119.583 no . . . C7 C4 H4 119.587 no . . . C6 C5 H15 120.142 no . . . C7 C5 H15 120.131 no 3_757 . . C8 C9 H9 120.264 no . . . C10 C9 H9 120.250 no . . . C9 C10 H10 119.349 no . . . C11 C10 H10 119.343 no . . . C11 C12 H12 119.130 no . . . C13 C12 H12 119.127 no . . . C8 C13 H13 118.838 no . . . C12 C13 H13 118.826 no . . . S1 C14 H14A 109.117 no . . . S1 C14 H14B 109.116 no . . . C15 C14 H14A 109.116 no . . . C15 C14 H14B 109.125 no . . . H14A C14 H14B 107.847 no . . . C14 C15 H15A 109.471 no . . . C14 C15 H15B 109.469 no . . . C14 C15 H15C 109.469 no . . . H15A C15 H15B 109.473 no . . . H15A C15 H15C 109.476 no . . . H15B C15 H15C 109.469 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O1 S1 C14 C15 -179.9(6) no . . . . O2 S1 C14 C15 58.7(8) no . . . . O3 S1 C14 C15 -59.5(8) no . . . . C2 C1 C6 C5 -178.6(10) no . . . . C2 C1 C6 C7 0.5(17) no . . . . C6 C1 C2 C3 -0.8(17) no . . . . C2 C1 C11 C10 84.6(14) no . . . . C2 C1 C11 C12 -100.3(12) no . . . . C11 C1 C2 C3 177.3(10) no . . . . C6 C1 C11 C10 -97.4(13) no . . . . C6 C1 C11 C12 77.8(15) no . . . . C11 C1 C6 C5 3.3(17) no . . . . C11 C1 C6 C7 -177.6(10) no . . . . C1 C2 C3 C4 -1.1(19) no . . . . C2 C3 C4 C7 3(2) no . . . . C3 C4 C7 C5 180.0(12) no . . . 3_757 C3 C4 C7 C6 -3.5(19) no . . . . C6 C5 C7 C4 -179.2(9) no . . 3_757 3_757 C6 C5 C7 C6 -2.9(17) no . . 3_757 3_757 C7 C5 C6 C1 -178.1(10) no 3_757 . . . C7 C5 C6 C7 2.8(16) no 3_757 . . . C1 C6 C7 C4 1.6(16) no . . . . C1 C6 C7 C5 178.0(10) no . . . 3_757 C5 C6 C7 C4 -179.3(9) no . . . . C5 C6 C7 C5 -2.8(16) no . . . 3_757 N1 C8 C9 C10 -178.0(9) no . . . . N1 C8 C13 C12 178.8(9) no . . . . C9 C8 C13 C12 0.8(18) no . . . . C13 C8 C9 C10 -0.1(17) no . . . . C8 C9 C10 C11 -3(2) no . . . . C9 C10 C11 C1 -179.7(11) no . . . . C9 C10 C11 C12 5.0(18) no . . . . C1 C11 C12 C13 -179.7(11) no . . . . C10 C11 C12 C13 -4.3(19) no . . . . C11 C12 C13 C8 1(3) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O2 C15 3.073(15) no . . O3 C15 3.052(15) no . . C1 C4 2.834(16) no . . C2 C7 2.819(15) no . . C2 C10 3.312(18) no . . C2 C12 3.397(19) no . . C3 C6 2.797(18) no . . C5 C5 2.801(15) no . 3_757 C5 C11 2.957(14) no . . C5 C12 3.427(17) no . . C6 C6 2.845(15) no . 3_757 C6 C10 3.474(17) no . . C6 C12 3.308(17) no . . C7 C7 2.771(17) no . 3_757 C8 C11 2.762(13) no . . C9 C12 2.683(18) no . . C10 C13 2.647(19) no . . S1 N1 3.512(8) no . . O1 O3 3.191(9) no . 2_646 O1 N1 2.851(10) no . 2_646 O1 N1 3.211(9) no . 3_656 O1 C8 3.564(12) no . 2_646 O1 C13 3.397(14) no . 2_646 O2 O2 3.077(9) no . 3_656 O2 N1 2.911(10) no . . O2 N1 2.900(9) no . 3_656 O2 C8 3.349(12) no . . O2 C9 3.370(15) no . . O2 C14 3.437(14) no . 4_544 O3 O1 3.191(9) no . 2_656 O3 N1 2.976(10) no . . O3 N1 2.754(10) no . 4_555 O3 C8 3.338(12) no . . O3 C8 3.560(11) no . 4_555 N1 S1 3.512(8) no . . N1 O1 2.851(10) no . 2_656 N1 O1 3.211(9) no . 3_656 N1 O2 2.911(10) no . . N1 O2 2.900(9) no . 3_656 N1 O3 2.976(10) no . . N1 O3 2.754(10) no . 4_554 C3 C5 3.572(18) no . 2_756 C4 C12 3.59(2) no . 2_746 C5 C3 3.572(18) no . 2_746 C8 O1 3.564(12) no . 2_656 C8 O2 3.349(12) no . . C8 O3 3.338(12) no . . C8 O3 3.560(11) no . 4_554 C9 O2 3.370(15) no . . C12 C4 3.59(2) no . 2_756 C13 O1 3.397(14) no . 2_656 C14 O2 3.437(14) no . 4_545 S1 H15A 2.8475 no . . S1 H15B 2.8516 no . . S1 H15C 3.5431 no . . O1 H14A 2.7841 no . . O1 H14B 2.7850 no . . O2 H14A 3.4074 no . . O2 H14B 2.8089 no . . O2 H15A 3.3461 no . . O2 H15B 2.7404 no . . O3 H14A 2.7793 no . . O3 H14B 3.4051 no . . O3 H15A 2.7023 no . . O3 H15B 3.3473 no . . N1 H9 2.5524 no . . N1 H13 2.5597 no . . C1 H10 2.6452 no . . C1 H12 2.5994 no . . C1 H3 3.3102 no . . C1 H15 2.6420 no . . C2 H10 3.3138 no . . C2 H12 3.4586 no . . C2 H4 3.2470 no . . C4 H2 3.2358 no . . C4 H15 2.6342 no . 3_757 C5 H12 3.4075 no . . C5 H4 2.6551 no . 3_757 C6 H2 3.2733 no . . C6 H10 3.5212 no . . C6 H12 3.2436 no . . C6 H4 3.2845 no . . C6 H15 3.2692 no . 3_757 C7 H3 3.3000 no . . C7 H15 3.2682 no . . C8 H10 3.1931 no . . C8 H12 3.1842 no . . C9 H1A 2.4678 no . . C9 H1B 2.7950 no . . C9 H1C 3.0687 no . . C9 H13 3.1227 no . . C10 H2 3.2757 no . . C10 H12 3.1400 no . . C10 H13 3.5865 no . . C10 H15 3.1773 no . . C11 H2 2.6436 no . . C11 H9 3.2512 no . . C11 H13 3.1758 no . . C11 H15 2.6168 no . . C12 H2 3.4643 no . . C12 H10 3.1379 no . . C12 H15 2.9494 no . . C13 H1A 3.0928 no . . C13 H1B 2.8158 no . . C13 H1C 2.4897 no . . C13 H9 3.1345 no . . C13 H10 3.5859 no . . H1A H9 2.3306 no . . H1A H13 3.3490 no . . H1B H9 2.8864 no . . H1B H13 2.8940 no . . H1C H9 3.3422 no . . H1C H13 2.3369 no . . H2 H10 3.3164 no . . H2 H3 2.3440 no . . H9 H10 2.3458 no . . H10 H15 3.4453 no . . H12 H13 2.2564 no . . H12 H15 3.0884 no . . H3 H4 2.2762 no . . H4 H15 2.4702 no . 3_757 H14A H15A 2.3324 no . . H14A H15B 2.8182 no . . H14A H15C 2.3163 no . . H14B H15A 2.8184 no . . H14B H15B 2.3296 no . . H14B H15C 2.3193 no . . S1 H1A 3.0127 no . . S1 H1A 3.0489 no . 3_656 S1 H1B 3.3168 no . 3_656 S1 H1B 3.2567 no . 4_555 S1 H1C 3.3108 no . . S1 H1C 3.0325 no . 2_646 S1 H14B 3.4406 no . 2_656 O1 H1A 3.4498 no . 2_646 O1 H1A 2.8373 no . 3_656 O1 H1B 3.0448 no . 2_646 O1 H1B 2.8010 no . 3_656 O1 H1C 2.0165 no . 2_646 O1 H9 3.1284 no . 3_656 O1 H13 2.6681 no . 2_646 O1 H14A 3.0897 no . 3_657 O1 H14B 3.2730 no . 2_656 O2 H1A 2.1686 no . . O2 H1A 2.2773 no . 3_656 O2 H1B 2.8416 no . 3_656 O2 H1C 3.0849 no . . O2 H1C 3.1893 no . 3_656 O2 H9 3.0525 no . . O2 H14A 2.9819 no . 4_544 O2 H14B 2.9656 no . 4_544 O3 H1A 2.8628 no . . O3 H1A 3.2450 no . 4_555 O3 H1B 1.8733 no . 4_555 O3 H1C 2.4768 no . . O3 H1C 3.0407 no . 4_555 O3 H13 3.5837 no . . O3 H14A 3.3788 no . 3_657 O3 H14B 3.0171 no . 2_656 N1 H14A 3.3801 no . 2_656 N1 H14B 3.2874 no . 2_656 C1 H2 3.3885 no . 4_555 C3 H10 3.1290 no . 3_756 C3 H12 3.4540 no . 2_746 C4 H12 3.0246 no . 2_746 C4 H3 3.5156 no . 4_555 C4 H15C 3.4663 no . 3_757 C5 H2 3.4038 no . 2_746 C5 H2 2.9270 no . 4_555 C5 H3 3.1496 no . 2_746 C5 H15A 3.5518 no . . C6 H2 3.5297 no . 2_746 C6 H2 2.7962 no . 4_555 C7 H2 3.2620 no . 2_746 C7 H2 3.0710 no . 4_555 C7 H12 3.5544 no . 2_746 C7 H3 3.2781 no . 4_555 C8 H13 3.5792 no . 4_554 C9 H12 3.4839 no . 4_554 C9 H13 3.1330 no . 4_554 C9 H15B 3.3204 no . . C9 H15C 3.3882 no . 4_544 C10 H12 3.2256 no . 4_554 C10 H3 3.3199 no . 3_756 C10 H15B 3.4754 no . . C10 H15C 3.5263 no . 4_544 C12 H4 3.3458 no . 2_756 C13 H4 3.5712 no . 2_756 C13 H15A 3.5380 no . 4_554 C14 H1C 3.0340 no . 2_646 C14 H9 3.5040 no . 4_545 C15 H9 3.3977 no . 4_545 C15 H4 3.2350 no . 3_757 C15 H15 3.2048 no . . H1A S1 3.0127 no . . H1A S1 3.0489 no . 3_656 H1A O1 3.4498 no . 2_656 H1A O1 2.8373 no . 3_656 H1A O2 2.1686 no . . H1A O2 2.2773 no . 3_656 H1A O3 2.8628 no . . H1A O3 3.2450 no . 4_554 H1A H1A 3.2107 no . 3_656 H1A H14A 3.4677 no . 2_656 H1A H14B 3.1583 no . 2_656 H1A H14B 3.5784 no . 4_544 H1B S1 3.3168 no . 3_656 H1B S1 3.2567 no . 4_554 H1B O1 3.0448 no . 2_656 H1B O1 2.8010 no . 3_656 H1B O2 2.8416 no . 3_656 H1B O3 1.8733 no . 4_554 H1B H1C 3.2395 no . 4_554 H1B H13 3.3892 no . 4_554 H1B H14A 3.2210 no . 2_656 H1B H14B 3.5437 no . 2_656 H1B H15A 3.3817 no . 4_554 H1C S1 3.3108 no . . H1C S1 3.0325 no . 2_656 H1C O1 2.0165 no . 2_656 H1C O2 3.0849 no . . H1C O2 3.1893 no . 3_656 H1C O3 2.4768 no . . H1C O3 3.0407 no . 4_554 H1C C14 3.0340 no . 2_656 H1C H1B 3.2395 no . 4_555 H1C H14A 2.9321 no . 2_656 H1C H14B 2.7091 no . 2_656 H2 C1 3.3885 no . 4_554 H2 C5 3.4038 no . 2_756 H2 C5 2.9270 no . 4_554 H2 C6 3.5297 no . 2_756 H2 C6 2.7962 no . 4_554 H2 C7 3.2620 no . 2_756 H2 C7 3.0710 no . 4_554 H2 H12 3.0205 no . 4_554 H2 H15 3.3443 no . 4_554 H9 O1 3.1284 no . 3_656 H9 O2 3.0525 no . . H9 C14 3.5040 no . 4_544 H9 C15 3.3977 no . 4_544 H9 H13 2.8689 no . 4_554 H9 H14B 2.8875 no . 4_544 H9 H15B 3.3898 no . . H9 H15B 3.5502 no . 4_544 H9 H15C 2.7547 no . 4_544 H10 C3 3.1290 no . 3_756 H10 H12 3.2940 no . 4_554 H10 H3 2.4537 no . 3_756 H10 H4 3.5235 no . 2_746 H10 H15B 3.5975 no . . H10 H15C 3.0031 no . 4_544 H12 C3 3.4540 no . 2_756 H12 C4 3.0246 no . 2_756 H12 C7 3.5544 no . 2_756 H12 C9 3.4839 no . 4_555 H12 C10 3.2256 no . 4_555 H12 H2 3.0205 no . 4_555 H12 H10 3.2940 no . 4_555 H12 H3 3.5952 no . 2_756 H12 H4 2.9127 no . 2_756 H13 O1 2.6681 no . 2_656 H13 O3 3.5837 no . . H13 C8 3.5792 no . 4_555 H13 C9 3.1330 no . 4_555 H13 H1B 3.3892 no . 4_555 H13 H9 2.8689 no . 4_555 H13 H4 3.3137 no . 2_756 H13 H15A 3.3233 no . 4_554 H3 C4 3.5156 no . 4_554 H3 C5 3.1496 no . 2_756 H3 C7 3.2781 no . 4_554 H3 C10 3.3199 no . 3_756 H3 H10 2.4537 no . 3_756 H3 H12 3.5952 no . 2_746 H3 H4 3.5191 no . 4_554 H3 H15 3.1561 no . 2_756 H3 H15B 3.4497 no . 2_756 H3 H15C 3.1886 no . 2_756 H4 C12 3.3458 no . 2_746 H4 C13 3.5712 no . 2_746 H4 C15 3.2350 no . 3_757 H4 H10 3.5235 no . 2_756 H4 H12 2.9127 no . 2_746 H4 H13 3.3137 no . 2_746 H4 H3 3.5191 no . 4_555 H4 H15A 2.9106 no . 3_757 H4 H15C 2.6775 no . 3_757 H15 C15 3.2048 no . . H15 H2 3.3443 no . 4_555 H15 H3 3.1561 no . 2_746 H15 H15A 2.6596 no . . H15 H15B 3.2509 no . . H15 H15C 3.2005 no . . H14A O1 3.0897 no . 3_657 H14A O2 2.9819 no . 4_545 H14A O3 3.3788 no . 3_657 H14A N1 3.3801 no . 2_646 H14A H1A 3.4677 no . 2_646 H14A H1B 3.2210 no . 2_646 H14A H1C 2.9321 no . 2_646 H14A H15B 3.5072 no . 4_545 H14B S1 3.4406 no . 2_646 H14B O1 3.2730 no . 2_646 H14B O2 2.9656 no . 4_545 H14B O3 3.0171 no . 2_646 H14B N1 3.2874 no . 2_646 H14B H1A 3.1583 no . 2_646 H14B H1A 3.5784 no . 4_545 H14B H1B 3.5437 no . 2_646 H14B H1C 2.7091 no . 2_646 H14B H9 2.8875 no . 4_545 H15A C5 3.5518 no . . H15A C13 3.5380 no . 4_555 H15A H1B 3.3817 no . 4_555 H15A H13 3.3233 no . 4_555 H15A H4 2.9106 no . 3_757 H15A H15 2.6596 no . . H15B C9 3.3204 no . . H15B C10 3.4754 no . . H15B H9 3.3898 no . . H15B H9 3.5502 no . 4_545 H15B H10 3.5975 no . . H15B H3 3.4497 no . 2_746 H15B H15 3.2509 no . . H15B H14A 3.5072 no . 4_544 H15B H15C 3.4181 no . 4_544 H15C C4 3.4663 no . 3_757 H15C C9 3.3882 no . 4_545 H15C C10 3.5263 no . 4_545 H15C H9 2.7547 no . 4_545 H15C H10 3.0031 no . 4_545 H15C H3 3.1886 no . 2_746 H15C H4 2.6775 no . 3_757 H15C H15 3.2005 no . . H15C H15B 3.4181 no . 4_545 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O2 . . . 2.911(10) 0.900 2.169 139.3 no N1 H1A O2 . . 3_656 2.900(9) 0.900 2.277 126.1 no N1 H1B O3 . . 4_554 2.754(10) 0.900 1.873 165.6 no N1 H1C O1 . . 2_656 2.851(10) 0.900 2.017 153.6 no N1 H1C O3 . . . 2.976(10) 0.900 2.477 115.4 no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 941421' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_15BAPA_PheSO3H_DMSO #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C42 H44 N2 O8 S4' _chemical_formula_moiety 'C42 H44 N2 O8 S4' _chemical_formula_weight 833.06 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,-Y,-Z #------------------------------------------------------------------------------ _cell_length_a 5.9458(3) _cell_length_b 8.3297(4) _cell_length_c 41.4851(19) _cell_angle_alpha 91.240(3) _cell_angle_beta 91.045(3) _cell_angle_gamma 96.474(3) _cell_volume 2040.60(16) _cell_formula_units_Z 2 _cell_measurement_reflns_used 8048 _cell_measurement_theta_min 3.19 _cell_measurement_theta_max 68.07 _cell_measurement_temperature 213 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 876.00 _exptl_absorpt_coefficient_mu 2.594 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_ambient_temperature 213 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54187 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 21284 _diffrn_reflns_av_R_equivalents 0.1441 _diffrn_reflns_theta_max 60.02 _diffrn_reflns_theta_full 60.02 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 46 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement was performed using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6031 _reflns_number_gt 2043 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1039 _refine_ls_wR_factor_ref 0.3367 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment constr _refine_ls_number_reflns 6031 _refine_ls_number_parameters 512 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.1369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.000 _refine_diff_density_max 0.370 _refine_diff_density_min -0.420 _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0044(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.018 0.009 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.031 0.018 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.049 0.032 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.333 0.557 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 S1 S 0.8031(6) 0.9425(4) 0.67070(6) 0.0820(10) Uani 1.0 2 d . . . S2 S 1.2167(6) 0.4232(4) 0.82864(7) 0.0881(10) Uani 1.0 2 d . . . S3 S 1.0610(6) 0.4028(4) 0.62462(7) 0.1108(12) Uani 1.0 2 d . . . S4 S 0.5252(7) 0.8759(4) 0.87433(8) 0.1157(13) Uani 1.0 2 d . . . O1 O 0.6815(12) 1.0850(8) 0.67167(14) 0.098(3) Uani 1.0 2 d . . . O2 O 0.7219(11) 0.8290(8) 0.64442(14) 0.086(2) Uani 1.0 2 d . . . O3 O 1.0479(12) 0.9806(8) 0.66952(14) 0.099(3) Uani 1.0 2 d . . . O4 O 1.0512(12) 0.5380(8) 0.82374(15) 0.102(3) Uani 1.0 2 d . . . O5 O 1.1383(12) 0.2915(9) 0.84966(16) 0.107(3) Uani 1.0 2 d . . . O6 O 1.4368(14) 0.5033(8) 0.83921(15) 0.102(3) Uani 1.0 2 d . . . O7 O 1.1490(13) 0.5506(9) 0.60675(16) 0.120(3) Uani 1.0 2 d . . . O8 O 0.5699(14) 1.0369(9) 0.89169(16) 0.134(3) Uani 1.0 2 d . . . N1 N 1.2874(12) -0.1366(9) 0.62086(16) 0.080(3) Uani 1.0 2 d . . . N2 N 0.7207(13) 0.3422(9) 0.87743(17) 0.085(3) Uani 1.0 2 d . . . C1 C 1.2946(16) 0.2569(11) 0.5092(3) 0.068(3) Uani 1.0 2 d . . . C2 C 1.4489(15) 0.2313(11) 0.4859(3) 0.072(3) Uani 1.0 2 d . . . C3 C 1.4530(16) 0.3202(11) 0.4571(3) 0.073(3) Uani 1.0 2 d . . . C4 C 1.3050(17) 0.4260(11) 0.4510(2) 0.073(3) Uani 1.0 2 d . . . C5 C 1.0011(15) 0.4163(10) 0.5291(2) 0.066(3) Uani 1.0 2 d . . . C6 C 1.1427(14) 0.3782(11) 0.5049(3) 0.060(3) Uani 1.0 2 d . . . C7 C 1.1453(17) 0.4641(12) 0.4748(2) 0.067(3) Uani 1.0 2 d . . . C8 C 1.295(3) -0.0367(13) 0.5923(2) 0.069(3) Uani 1.0 2 d . . . C9 C 1.0948(18) -0.0419(12) 0.5731(3) 0.077(3) Uani 1.0 2 d . . . C10 C 1.0948(19) 0.0548(13) 0.5467(3) 0.082(4) Uani 1.0 2 d . . . C11 C 1.283(3) 0.1555(12) 0.5382(3) 0.068(3) Uani 1.0 2 d . . . C12 C 1.479(2) 0.1537(12) 0.5575(3) 0.080(3) Uani 1.0 2 d . . . C13 C 1.4840(19) 0.0607(13) 0.5846(3) 0.080(3) Uani 1.0 2 d . . . C14 C 0.7909(18) 0.7531(11) 0.9906(3) 0.070(3) Uani 1.0 2 d . . . C15 C 0.9504(17) 0.7350(11) 1.0140(3) 0.074(3) Uani 1.0 2 d . . . C16 C 0.9697(19) 0.8299(12) 1.0427(3) 0.080(3) Uani 1.0 2 d . . . C17 C 0.8214(18) 0.9382(13) 1.0489(3) 0.080(3) Uani 1.0 2 d . . . C18 C 0.4818(17) 0.9140(12) 0.9708(3) 0.074(3) Uani 1.0 2 d . . . C19 C 0.6393(16) 0.8772(10) 0.9951(3) 0.064(3) Uani 1.0 2 d . . . C20 C 0.6556(18) 0.9646(11) 1.0244(3) 0.068(3) Uani 1.0 2 d . . . C21 C 0.740(3) 0.4425(12) 0.9077(3) 0.071(3) Uani 1.0 2 d . . . C22 C 0.5578(17) 0.4440(12) 0.9273(3) 0.078(3) Uani 1.0 2 d . . . C23 C 0.5790(19) 0.5475(12) 0.9544(3) 0.073(3) Uani 1.0 2 d . . . C24 C 0.7790(19) 0.6479(11) 0.9614(3) 0.067(3) Uani 1.0 2 d . . . C25 C 0.9557(18) 0.6367(12) 0.9405(3) 0.081(3) Uani 1.0 2 d . . . C26 C 0.947(2) 0.5388(13) 0.9136(3) 0.091(4) Uani 1.0 2 d . . . C27 C 0.749(2) 0.8407(12) 0.7066(3) 0.071(3) Uani 1.0 2 d . . . C28 C 0.533(3) 0.7642(14) 0.7124(3) 0.097(4) Uani 1.0 2 d . . . C29 C 0.490(3) 0.6824(14) 0.7400(3) 0.113(5) Uani 1.0 2 d . . . C30 C 0.648(3) 0.6748(15) 0.7639(3) 0.108(5) Uani 1.0 2 d . . . C31 C 0.861(3) 0.7501(16) 0.7586(3) 0.111(5) Uani 1.0 2 d . . . C32 C 0.913(2) 0.8276(13) 0.7301(4) 0.100(4) Uani 1.0 2 d . . . C33 C 1.261(2) 0.3319(11) 0.7911(3) 0.077(3) Uani 1.0 2 d . . . C34 C 1.4599(19) 0.2632(12) 0.7849(3) 0.089(4) Uani 1.0 2 d . . . C35 C 1.495(3) 0.1887(13) 0.7561(3) 0.101(4) Uani 1.0 2 d . . . C36 C 1.334(3) 0.1872(14) 0.7317(3) 0.102(4) Uani 1.0 2 d . . . C37 C 1.137(3) 0.2534(14) 0.7374(3) 0.104(4) Uani 1.0 2 d . . . C38 C 1.0956(19) 0.3270(13) 0.7663(3) 0.091(4) Uani 1.0 2 d . . . C39 C 1.2969(19) 0.3390(13) 0.6464(3) 0.122(5) Uani 1.0 2 d . . . C40 C 0.917(2) 0.4732(13) 0.6580(3) 0.135(5) Uani 1.0 2 d . . . C41 C 0.787(2) 0.8401(15) 0.8594(3) 0.143(5) Uani 1.0 2 d . . . C42 C 0.389(2) 0.9136(15) 0.8366(3) 0.144(5) Uani 1.0 2 d . . . H1A H 1.4288 -0.1388 0.6288 0.0958 Uiso 1.0 2 calc R . . H1B H 1.2270 -0.2377 0.6154 0.0958 Uiso 1.0 2 calc R . . H1C H 1.2019 -0.0948 0.6359 0.0958 Uiso 1.0 2 calc R . . H2 H 1.5518 0.1551 0.4891 0.0864 Uiso 1.0 2 calc R . . H2A H 0.6512 0.2433 0.8815 0.1022 Uiso 1.0 2 calc R . . H2B H 0.8598 0.3332 0.8699 0.1022 Uiso 1.0 2 calc R . . H2C H 0.6393 0.3894 0.8626 0.1022 Uiso 1.0 2 calc R . . H3 H 1.5634 0.3042 0.4418 0.0877 Uiso 1.0 2 calc R . . H4 H 1.3055 0.4759 0.4308 0.0876 Uiso 1.0 2 calc R . . H5 H 1.0023 0.3610 0.5486 0.0789 Uiso 1.0 2 calc R . . H9 H 0.9645 -0.1103 0.5784 0.0926 Uiso 1.0 2 calc R . . H10 H 0.9618 0.0521 0.5340 0.0986 Uiso 1.0 2 calc R . . H12 H 1.6112 0.2182 0.5518 0.0959 Uiso 1.0 2 calc R . . H13 H 1.6162 0.0648 0.5975 0.0958 Uiso 1.0 2 calc R . . H15 H 1.0505 0.6566 1.0109 0.0892 Uiso 1.0 2 calc R . . H16 H 1.0866 0.8179 1.0577 0.0961 Uiso 1.0 2 calc R . . H17 H 0.8265 0.9951 1.0687 0.0963 Uiso 1.0 2 calc R . . H18 H 0.4711 0.8548 0.9512 0.0890 Uiso 1.0 2 calc R . . H22 H 0.4223 0.3774 0.9227 0.0938 Uiso 1.0 2 calc R . . H23 H 0.4558 0.5496 0.9682 0.0872 Uiso 1.0 2 calc R . . H25 H 1.0925 0.7017 0.9453 0.0975 Uiso 1.0 2 calc R . . H26 H 1.0715 0.5360 0.9000 0.1090 Uiso 1.0 2 calc R . . H28 H 0.4159 0.7695 0.6971 0.1167 Uiso 1.0 2 calc R . . H29 H 0.3438 0.6286 0.7428 0.1352 Uiso 1.0 2 calc R . . H30 H 0.6132 0.6205 0.7831 0.1293 Uiso 1.0 2 calc R . . H31 H 0.9744 0.7490 0.7747 0.1336 Uiso 1.0 2 calc R . . H32 H 1.0627 0.8722 0.7266 0.1201 Uiso 1.0 2 calc R . . H34 H 1.5732 0.2685 0.8011 0.1074 Uiso 1.0 2 calc R . . H35 H 1.6279 0.1391 0.7529 0.1211 Uiso 1.0 2 calc R . . H36 H 1.3591 0.1412 0.7114 0.1228 Uiso 1.0 2 calc R . . H37 H 1.0255 0.2482 0.7208 0.1245 Uiso 1.0 2 calc R . . H38 H 0.9602 0.3730 0.7694 0.1088 Uiso 1.0 2 calc R . . H39A H 1.4043 0.3031 0.6312 0.1459 Uiso 1.0 2 calc R . . H39B H 1.2443 0.2507 0.6602 0.1459 Uiso 1.0 2 calc R . . H39C H 1.3698 0.4287 0.6594 0.1459 Uiso 1.0 2 calc R . . H40A H 1.0244 0.5348 0.6726 0.1621 Uiso 1.0 2 calc R . . H40B H 0.8408 0.3818 0.6691 0.1621 Uiso 1.0 2 calc R . . H40C H 0.8058 0.5417 0.6506 0.1621 Uiso 1.0 2 calc R . . H41A H 0.8387 0.9248 0.8447 0.1718 Uiso 1.0 2 calc R . . H41B H 0.7719 0.7364 0.8480 0.1718 Uiso 1.0 2 calc R . . H41C H 0.8949 0.8391 0.8771 0.1718 Uiso 1.0 2 calc R . . H42A H 0.2583 0.9709 0.8407 0.1733 Uiso 1.0 2 calc R . . H42B H 0.3398 0.8116 0.8255 0.1733 Uiso 1.0 2 calc R . . H42C H 0.4944 0.9787 0.8233 0.1733 Uiso 1.0 2 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1 0.080(3) 0.090(3) 0.078(2) 0.0142(19) 0.0230(16) 0.0049(17) S2 0.098(3) 0.083(3) 0.084(3) 0.014(2) 0.0222(19) -0.0074(18) S3 0.136(4) 0.080(3) 0.111(3) -0.008(3) -0.000(3) 0.002(2) S4 0.150(4) 0.086(3) 0.111(3) 0.004(3) 0.035(3) -0.0019(19) O1 0.119(6) 0.076(5) 0.103(6) 0.029(5) 0.027(5) 0.015(4) O2 0.086(5) 0.095(5) 0.080(5) 0.021(4) 0.002(4) 0.000(4) O3 0.074(6) 0.134(6) 0.087(5) -0.007(5) 0.034(4) -0.003(5) O4 0.114(6) 0.106(6) 0.094(5) 0.052(5) 0.008(5) -0.007(4) O5 0.120(7) 0.099(6) 0.107(6) 0.026(5) 0.044(5) 0.006(5) O6 0.115(7) 0.090(6) 0.096(5) -0.000(5) 0.007(5) -0.022(4) O7 0.164(8) 0.080(5) 0.113(6) -0.011(5) 0.010(5) 0.010(5) O8 0.204(9) 0.085(6) 0.110(6) 0.003(6) 0.039(6) -0.004(5) N1 0.089(7) 0.081(6) 0.073(6) 0.022(5) 0.011(5) 0.005(5) N2 0.097(7) 0.072(6) 0.088(6) 0.011(5) 0.018(5) -0.008(5) C1 0.061(7) 0.064(7) 0.081(7) 0.017(6) 0.015(6) -0.003(6) C2 0.057(7) 0.064(7) 0.099(8) 0.019(6) 0.016(6) 0.013(6) C3 0.068(8) 0.057(7) 0.099(8) 0.025(6) 0.019(6) 0.009(6) C4 0.095(9) 0.061(7) 0.060(6) -0.002(7) 0.022(6) -0.006(5) C5 0.072(8) 0.058(7) 0.071(7) 0.026(6) 0.007(6) -0.001(5) C6 0.044(6) 0.060(6) 0.078(7) 0.018(6) 0.007(5) -0.010(6) C7 0.083(8) 0.069(7) 0.050(6) 0.004(6) 0.018(6) 0.001(6) C8 0.083(9) 0.082(8) 0.048(6) 0.035(8) 0.005(7) 0.005(6) C9 0.079(9) 0.059(7) 0.096(9) 0.012(6) 0.023(7) 0.009(7) C10 0.078(9) 0.066(8) 0.101(9) -0.004(7) 0.017(7) 0.006(7) C11 0.089(9) 0.057(7) 0.062(7) 0.023(7) -0.002(7) 0.001(6) C12 0.099(10) 0.066(8) 0.077(8) 0.015(7) 0.022(7) 0.006(7) C13 0.064(9) 0.076(8) 0.097(9) -0.002(7) 0.010(7) -0.000(7) C14 0.085(9) 0.062(7) 0.064(7) 0.003(7) 0.013(6) 0.000(6) C15 0.074(8) 0.057(7) 0.094(8) 0.013(6) 0.007(7) 0.009(7) C16 0.103(10) 0.061(7) 0.079(8) 0.019(7) 0.009(7) 0.007(6) C17 0.099(9) 0.081(8) 0.062(7) 0.012(8) 0.002(7) 0.002(6) C18 0.066(8) 0.074(8) 0.076(7) -0.017(7) -0.007(6) -0.003(6) C19 0.059(8) 0.045(6) 0.090(8) 0.003(6) 0.032(6) -0.001(6) C20 0.075(8) 0.053(7) 0.079(8) 0.014(6) 0.038(6) -0.009(6) C21 0.096(10) 0.046(7) 0.073(7) 0.014(7) 0.021(7) 0.015(6) C22 0.064(8) 0.085(8) 0.087(8) 0.007(6) 0.018(7) 0.015(7) C23 0.086(9) 0.057(7) 0.078(8) 0.024(7) 0.014(6) -0.004(6) C24 0.076(9) 0.056(7) 0.068(7) -0.002(7) -0.002(7) 0.010(6) C25 0.065(8) 0.080(8) 0.101(9) 0.016(6) 0.028(7) 0.007(7) C26 0.108(11) 0.062(8) 0.104(9) 0.010(8) 0.039(8) -0.003(7) C27 0.067(8) 0.066(7) 0.082(8) 0.013(7) 0.027(7) 0.009(6) C28 0.109(11) 0.112(10) 0.073(8) 0.021(9) 0.010(7) 0.021(7) C29 0.147(13) 0.100(10) 0.093(10) 0.008(9) 0.017(10) 0.045(8) C30 0.145(14) 0.100(10) 0.078(9) 0.005(10) 0.031(10) 0.033(8) C31 0.134(14) 0.115(11) 0.088(10) 0.018(10) -0.004(9) 0.037(8) C32 0.087(10) 0.104(10) 0.110(10) 0.011(8) 0.012(9) 0.016(8) C33 0.079(9) 0.056(7) 0.098(9) 0.014(7) 0.027(7) 0.009(6) C34 0.091(10) 0.079(8) 0.099(9) 0.011(7) 0.021(7) -0.001(7) C35 0.106(11) 0.105(9) 0.091(9) 0.009(8) 0.032(8) -0.026(8) C36 0.109(12) 0.099(9) 0.092(10) -0.018(9) 0.033(9) -0.023(8) C37 0.095(11) 0.125(11) 0.090(9) 0.002(9) 0.023(8) -0.006(8) C38 0.069(9) 0.109(9) 0.098(9) 0.024(7) 0.023(8) 0.017(8) C39 0.139(11) 0.107(9) 0.127(10) 0.049(9) -0.002(9) 0.014(8) C40 0.147(12) 0.089(9) 0.176(12) 0.031(9) 0.052(10) 0.033(9) C41 0.139(12) 0.148(12) 0.152(12) 0.055(10) 0.021(10) -0.001(10) C42 0.159(12) 0.136(11) 0.144(11) 0.049(10) -0.038(10) 0.002(9) #============================================================================== _computing_data_collection 'RAPID AUTO (Rigaku, ????)' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'SIR2004 (Burla, et al., 2005)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'CrystalStructure 4.0' #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 S1 O1 1.458(8) yes . . S1 O2 1.466(7) yes . . S1 O3 1.457(8) yes . . S1 C27 1.745(11) yes . . S2 O4 1.462(8) yes . . S2 O5 1.457(8) yes . . S2 O6 1.456(8) yes . . S2 C33 1.756(11) yes . . S3 O7 1.500(8) yes . . S3 C39 1.791(12) yes . . S3 C40 1.766(13) yes . . S4 O8 1.503(8) yes . . S4 C41 1.737(13) yes . . S4 C42 1.800(13) yes . . N1 C8 1.460(12) yes . . N2 C21 1.488(12) yes . . C1 C2 1.373(14) yes . . C1 C6 1.441(13) yes . . C1 C11 1.484(14) yes . . C2 C3 1.421(14) yes . . C3 C4 1.338(14) yes . . C4 C7 1.438(14) yes . . C5 C6 1.376(13) yes . . C5 C7 1.405(14) yes . 2_766 C6 C7 1.452(13) yes . . C8 C9 1.413(16) yes . . C8 C13 1.359(16) yes . . C9 C10 1.375(15) yes . . C10 C11 1.376(16) yes . . C11 C12 1.402(16) yes . . C12 C13 1.381(15) yes . . C14 C15 1.370(15) yes . . C14 C19 1.458(14) yes . . C14 C24 1.473(13) yes . . C15 C16 1.410(14) yes . . C16 C17 1.354(16) yes . . C17 C20 1.440(15) yes . . C18 C19 1.425(14) yes . . C18 C20 1.383(15) yes . 2_677 C19 C20 1.396(14) yes . . C21 C22 1.370(16) yes . . C21 C26 1.406(16) yes . . C22 C23 1.396(14) yes . . C23 C24 1.397(15) yes . . C24 C25 1.384(15) yes . . C25 C26 1.366(15) yes . . C27 C28 1.396(17) yes . . C27 C32 1.381(17) yes . . C28 C29 1.359(17) yes . . C29 C30 1.36(2) yes . . C30 C31 1.37(2) yes . . C31 C32 1.382(18) yes . . C33 C34 1.397(17) yes . . C33 C38 1.406(16) yes . . C34 C35 1.366(16) yes . . C35 C36 1.381(19) yes . . C36 C37 1.37(2) yes . . C37 C38 1.374(17) yes . . N1 H1A 0.900 no . . N1 H1B 0.900 no . . N1 H1C 0.900 no . . N2 H2A 0.900 no . . N2 H2B 0.900 no . . N2 H2C 0.900 no . . C2 H2 0.940 no . . C3 H3 0.940 no . . C4 H4 0.940 no . . C5 H5 0.940 no . . C9 H9 0.940 no . . C10 H10 0.940 no . . C12 H12 0.940 no . . C13 H13 0.940 no . . C15 H15 0.940 no . . C16 H16 0.940 no . . C17 H17 0.940 no . . C18 H18 0.940 no . . C22 H22 0.940 no . . C23 H23 0.940 no . . C25 H25 0.940 no . . C26 H26 0.940 no . . C28 H28 0.940 no . . C29 H29 0.940 no . . C30 H30 0.940 no . . C31 H31 0.940 no . . C32 H32 0.940 no . . C34 H34 0.940 no . . C35 H35 0.940 no . . C36 H36 0.940 no . . C37 H37 0.940 no . . C38 H38 0.940 no . . C39 H39A 0.970 no . . C39 H39B 0.970 no . . C39 H39C 0.970 no . . C40 H40A 0.970 no . . C40 H40B 0.970 no . . C40 H40C 0.970 no . . C41 H41A 0.970 no . . C41 H41B 0.970 no . . C41 H41C 0.970 no . . C42 H42A 0.970 no . . C42 H42B 0.970 no . . C42 H42C 0.970 no . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 O1 S1 O2 112.4(4) yes . . . O1 S1 O3 113.5(5) yes . . . O1 S1 C27 107.3(5) yes . . . O2 S1 O3 110.3(4) yes . . . O2 S1 C27 106.5(5) yes . . . O3 S1 C27 106.2(5) yes . . . O4 S2 O5 113.4(5) yes . . . O4 S2 O6 112.1(5) yes . . . O4 S2 C33 107.7(5) yes . . . O5 S2 O6 111.6(5) yes . . . O5 S2 C33 105.7(5) yes . . . O6 S2 C33 105.7(5) yes . . . O7 S3 C39 106.8(5) yes . . . O7 S3 C40 105.8(5) yes . . . C39 S3 C40 97.8(6) yes . . . O8 S4 C41 104.5(6) yes . . . O8 S4 C42 106.1(5) yes . . . C41 S4 C42 98.1(6) yes . . . C2 C1 C6 120.1(9) yes . . . C2 C1 C11 119.2(9) yes . . . C6 C1 C11 120.8(9) yes . . . C1 C2 C3 120.0(9) yes . . . C2 C3 C4 122.2(9) yes . . . C3 C4 C7 120.8(9) yes . . . C6 C5 C7 121.4(9) yes . . 2_766 C1 C6 C5 121.1(9) yes . . . C1 C6 C7 118.9(9) yes . . . C5 C6 C7 120.0(9) yes . . . C4 C7 C5 123.6(9) yes . . 2_766 C4 C7 C6 117.8(9) yes . . . C5 C7 C6 118.6(9) yes 2_766 . . N1 C8 C9 117.6(10) yes . . . N1 C8 C13 121.7(10) yes . . . C9 C8 C13 120.7(10) yes . . . C8 C9 C10 118.8(10) yes . . . C9 C10 C11 122.2(10) yes . . . C1 C11 C10 124.3(10) yes . . . C1 C11 C12 118.6(10) yes . . . C10 C11 C12 117.0(9) yes . . . C11 C12 C13 122.5(10) yes . . . C8 C13 C12 118.8(10) yes . . . C15 C14 C19 118.7(9) yes . . . C15 C14 C24 119.2(10) yes . . . C19 C14 C24 122.1(9) yes . . . C14 C15 C16 122.2(10) yes . . . C15 C16 C17 120.7(10) yes . . . C16 C17 C20 118.7(9) yes . . . C19 C18 C20 121.1(9) yes . . 2_677 C14 C19 C18 122.5(9) yes . . . C14 C19 C20 117.7(9) yes . . . C18 C19 C20 119.7(9) yes . . . C17 C20 C18 119.1(9) yes . . 2_677 C17 C20 C19 121.7(10) yes . . . C18 C20 C19 119.2(9) yes 2_677 . . N2 C21 C22 119.9(10) yes . . . N2 C21 C26 116.7(10) yes . . . C22 C21 C26 123.3(10) yes . . . C21 C22 C23 118.0(9) yes . . . C22 C23 C24 121.6(10) yes . . . C14 C24 C23 118.9(10) yes . . . C14 C24 C25 124.7(10) yes . . . C23 C24 C25 116.4(9) yes . . . C24 C25 C26 125.2(10) yes . . . C21 C26 C25 115.4(11) yes . . . S1 C27 C28 120.4(9) yes . . . S1 C27 C32 123.2(10) yes . . . C28 C27 C32 116.4(10) yes . . . C27 C28 C29 120.9(12) yes . . . C28 C29 C30 122.9(13) yes . . . C29 C30 C31 116.9(12) yes . . . C30 C31 C32 121.4(13) yes . . . C27 C32 C31 121.3(12) yes . . . S2 C33 C34 121.3(9) yes . . . S2 C33 C38 120.5(9) yes . . . C34 C33 C38 118.2(10) yes . . . C33 C34 C35 122.2(11) yes . . . C34 C35 C36 119.1(12) yes . . . C35 C36 C37 119.5(12) yes . . . C36 C37 C38 122.4(12) yes . . . C33 C38 C37 118.5(11) yes . . . C8 N1 H1A 109.475 no . . . C8 N1 H1B 109.462 no . . . C8 N1 H1C 109.468 no . . . H1A N1 H1B 109.474 no . . . H1A N1 H1C 109.475 no . . . H1B N1 H1C 109.474 no . . . C21 N2 H2A 109.467 no . . . C21 N2 H2B 109.469 no . . . C21 N2 H2C 109.485 no . . . H2A N2 H2B 109.471 no . . . H2A N2 H2C 109.473 no . . . H2B N2 H2C 109.463 no . . . C1 C2 H2 120.032 no . . . C3 C2 H2 120.016 no . . . C2 C3 H3 118.881 no . . . C4 C3 H3 118.901 no . . . C3 C4 H4 119.601 no . . . C7 C4 H4 119.612 no . . . C6 C5 H5 119.286 no . . . C7 C5 H5 119.267 no 2_766 . . C8 C9 H9 120.604 no . . . C10 C9 H9 120.631 no . . . C9 C10 H10 118.900 no . . . C11 C10 H10 118.885 no . . . C11 C12 H12 118.740 no . . . C13 C12 H12 118.762 no . . . C8 C13 H13 120.587 no . . . C12 C13 H13 120.618 no . . . C14 C15 H15 118.879 no . . . C16 C15 H15 118.885 no . . . C15 C16 H16 119.658 no . . . C17 C16 H16 119.685 no . . . C16 C17 H17 120.635 no . . . C20 C17 H17 120.639 no . . . C19 C18 H18 119.426 no . . . C20 C18 H18 119.436 no 2_677 . . C21 C22 H22 120.998 no . . . C23 C22 H22 120.991 no . . . C22 C23 H23 119.214 no . . . C24 C23 H23 119.205 no . . . C24 C25 H25 117.360 no . . . C26 C25 H25 117.393 no . . . C21 C26 H26 122.325 no . . . C25 C26 H26 122.294 no . . . C27 C28 H28 119.529 no . . . C29 C28 H28 119.528 no . . . C28 C29 H29 118.560 no . . . C30 C29 H29 118.546 no . . . C29 C30 H30 121.552 no . . . C31 C30 H30 121.560 no . . . C30 C31 H31 119.299 no . . . C32 C31 H31 119.300 no . . . C27 C32 H32 119.336 no . . . C31 C32 H32 119.333 no . . . C33 C34 H34 118.900 no . . . C35 C34 H34 118.920 no . . . C34 C35 H35 120.439 no . . . C36 C35 H35 120.456 no . . . C35 C36 H36 120.237 no . . . C37 C36 H36 120.249 no . . . C36 C37 H37 118.819 no . . . C38 C37 H37 118.811 no . . . C33 C38 H38 120.746 no . . . C37 C38 H38 120.739 no . . . S3 C39 H39A 109.483 no . . . S3 C39 H39B 109.467 no . . . S3 C39 H39C 109.474 no . . . H39A C39 H39B 109.470 no . . . H39A C39 H39C 109.480 no . . . H39B C39 H39C 109.453 no . . . S3 C40 H40A 109.470 no . . . S3 C40 H40B 109.466 no . . . S3 C40 H40C 109.453 no . . . H40A C40 H40B 109.484 no . . . H40A C40 H40C 109.481 no . . . H40B C40 H40C 109.474 no . . . S4 C41 H41A 109.470 no . . . S4 C41 H41B 109.471 no . . . S4 C41 H41C 109.483 no . . . H41A C41 H41B 109.464 no . . . H41A C41 H41C 109.469 no . . . H41B C41 H41C 109.470 no . . . S4 C42 H42A 109.487 no . . . S4 C42 H42B 109.474 no . . . S4 C42 H42C 109.468 no . . . H42A C42 H42B 109.466 no . . . H42A C42 H42C 109.464 no . . . H42B C42 H42C 109.467 no . . . 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_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O1 S1 C27 C28 68.8(8) no . . . . O1 S1 C27 C32 -112.6(8) no . . . . O2 S1 C27 C28 -51.9(9) no . . . . O2 S1 C27 C32 126.7(7) no . . . . O3 S1 C27 C28 -169.5(7) no . . . . O3 S1 C27 C32 9.1(9) no . . . . O4 S2 C33 C34 156.6(6) no . . . . O4 S2 C33 C38 -23.0(8) no . . . . O5 S2 C33 C34 -81.8(8) no . . . . O5 S2 C33 C38 98.6(7) no . . . . O6 S2 C33 C34 36.7(8) no . . . . O6 S2 C33 C38 -142.9(7) no . . . . C2 C1 C6 C5 -174.0(7) no . . . . C2 C1 C6 C7 4.3(12) no . . . . C6 C1 C2 C3 -2.4(12) no . . . . C2 C1 C11 C10 -118.5(11) no . . . . C2 C1 C11 C12 57.7(12) no . . . . C11 C1 C2 C3 176.0(8) no . . . . C6 C1 C11 C10 59.9(13) no . . . . C6 C1 C11 C12 -123.8(10) no . . . . C11 C1 C6 C5 7.6(12) no . . . . C11 C1 C6 C7 -174.2(7) no . . . . C1 C2 C3 C4 -2.3(13) no . . . . C2 C3 C4 C7 5.1(13) no . . . . C3 C4 C7 C5 174.4(8) no . . . 2_766 C3 C4 C7 C6 -3.0(13) no . . . . C6 C5 C7 C4 176.5(7) no . . 2_766 2_766 C6 C5 C7 C6 -0.9(12) no . . 2_766 2_766 C7 C5 C6 C1 179.1(7) no 2_766 . . . C7 C5 C6 C7 0.9(12) no 2_766 . . . C1 C6 C7 C4 -1.6(12) no . . . . C1 C6 C7 C5 -179.1(7) no . . . 2_766 C5 C6 C7 C4 176.7(7) no . . . . C5 C6 C7 C5 -0.8(12) no . . . 2_766 N1 C8 C9 C10 178.0(8) no . . . . N1 C8 C13 C12 -179.2(8) no . . . . C9 C8 C13 C12 -0.5(16) no . . . . C13 C8 C9 C10 -0.8(15) no . . . . C8 C9 C10 C11 0.5(16) no . . . . C9 C10 C11 C1 177.3(9) no . . . . C9 C10 C11 C12 1.0(16) no . . . . C1 C11 C12 C13 -178.9(8) no . . . . C10 C11 C12 C13 -2.4(15) no . . . . C11 C12 C13 C8 2.1(16) no . . . . C15 C14 C19 C18 174.4(8) no . . . . C15 C14 C19 C20 -4.0(13) no . . . . C19 C14 C15 C16 1.3(14) no . . . . C15 C14 C24 C23 119.7(10) no . . . . C15 C14 C24 C25 -58.3(13) no . . . . C24 C14 C15 C16 -179.1(8) no . . . . C19 C14 C24 C23 -60.8(12) no . . . . C19 C14 C24 C25 121.2(11) no . . . . C24 C14 C19 C18 -5.1(14) no . . . . C24 C14 C19 C20 176.5(8) no . . . . C14 C15 C16 C17 3.5(15) no . . . . C15 C16 C17 C20 -5.2(14) no . . . . C16 C17 C20 C18 -173.7(9) no . . . 2_677 C16 C17 C20 C19 2.4(14) no . . . . C19 C18 C20 C17 -176.4(8) no . . 2_677 2_677 C19 C18 C20 C19 -0.1(14) no . . 2_677 2_677 C20 C18 C19 C14 -178.3(8) no 2_677 . . . C20 C18 C19 C20 0.1(13) no 2_677 . . . C14 C19 C20 C17 2.2(13) no . . . . C14 C19 C20 C18 178.4(8) no . . . 2_677 C18 C19 C20 C17 -176.3(8) no . . . . C18 C19 C20 C18 -0.1(13) no . . . 2_677 N2 C21 C22 C23 -176.0(8) no . . . . N2 C21 C26 C25 176.3(8) no . . . . C22 C21 C26 C25 -0.3(16) no . . . . C26 C21 C22 C23 0.4(16) no . . . . C21 C22 C23 C24 0.4(15) no . . . . C22 C23 C24 C14 -179.4(9) no . . . . C22 C23 C24 C25 -1.3(14) no . . . . C14 C24 C25 C26 179.5(9) no . . . . C23 C24 C25 C26 1.5(15) no . . . . C24 C25 C26 C21 -0.7(16) no . . . . S1 C27 C28 C29 178.9(7) no . . . . S1 C27 C32 C31 178.0(7) no . . . . C28 C27 C32 C31 -3.4(16) no . . . . C32 C27 C28 C29 0.2(16) no . . . . C27 C28 C29 C30 2.6(18) no . . . . C28 C29 C30 C31 -2.2(19) no . . . . C29 C30 C31 C32 -1.1(19) no . . . . C30 C31 C32 C27 3.9(19) no . . . . S2 C33 C34 C35 178.6(7) no . . . . S2 C33 C38 C37 -179.6(7) no . . . . C34 C33 C38 C37 0.8(14) no . . . . C38 C33 C34 C35 -1.8(14) no . . . . C33 C34 C35 C36 3.0(15) no . . . . C34 C35 C36 C37 -3.2(16) no . . . . C35 C36 C37 C38 2.3(17) no . . . . C36 C37 C38 C33 -1.1(16) no . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O1 C28 3.240(13) no . . O2 C28 3.092(13) no . . O3 C32 2.926(15) no . . O4 C38 2.964(14) no . . O5 C34 3.345(13) no . . O5 C38 3.485(14) no . . O6 C34 2.995(12) no . . C1 C4 2.821(13) no . . C2 C7 2.834(14) no . . C2 C10 3.550(15) no . . C2 C12 3.058(15) no . . C3 C6 2.804(14) no . . C5 C5 2.812(13) no . 2_766 C5 C10 3.220(14) no . . C5 C11 2.916(15) no . . C6 C6 2.819(13) no . 2_766 C6 C10 3.224(14) no . . C7 C7 2.835(14) no . 2_766 C8 C11 2.790(14) no . . C9 C12 2.746(15) no . . C10 C13 2.770(16) no . . C14 C17 2.832(14) no . . C15 C20 2.768(15) no . . C15 C23 3.507(14) no . . C15 C25 3.142(15) no . . C16 C19 2.824(15) no . . C18 C18 2.776(13) no . 2_677 C18 C23 3.232(14) no . . C18 C24 3.010(15) no . . C19 C19 2.800(14) no . 2_677 C19 C23 3.176(13) no . . C20 C20 2.832(15) no . 2_677 C21 C24 2.771(13) no . . C22 C25 2.745(14) no . . C23 C26 2.798(16) no . . C27 C30 2.817(16) no . . C28 C31 2.723(19) no . . C29 C32 2.710(18) no . . C33 C36 2.782(17) no . . C34 C37 2.723(17) no . . C35 C38 2.791(18) no . . S4 O6 3.382(8) no . 1_455 O1 N1 3.467(9) no . 1_465 O1 C36 3.419(15) no . 1_465 O1 C39 3.450(14) no . 1_465 O1 C40 3.438(13) no . 1_565 O2 N1 2.793(10) no . 1_465 O2 N1 3.501(10) no . 1_565 O2 C8 3.595(13) no . 1_465 O2 C13 3.547(13) no . 1_465 O2 C40 3.356(14) no . . O3 N1 2.718(10) no . 1_565 O3 C8 3.553(12) no . 1_565 O3 C36 3.391(14) no . 1_565 O3 C37 3.572(13) no . 1_565 O3 C39 3.347(13) no . 1_565 O4 N2 3.328(10) no . . O4 C31 3.500(15) no . . O4 C41 3.437(15) no . . O4 C42 3.546(14) no . 1_655 O5 N2 2.826(11) no . . O6 S4 3.382(8) no . 1_655 O6 N2 2.770(11) no . 1_655 O6 C21 3.416(13) no . 1_655 O6 C41 3.378(14) no . 1_655 O6 C42 3.465(14) no . 1_655 O7 N1 2.691(10) no . 1_565 O7 C4 3.600(12) no . 2_766 O7 C5 3.454(11) no . . O7 C8 3.516(13) no . 1_565 O8 N2 2.682(10) no . 1_565 O8 C17 3.441(13) no . 2_677 O8 C18 3.492(12) no . . O8 C21 3.463(12) no . 1_565 N1 O1 3.467(9) no . 1_645 N1 O2 3.501(10) no . 1_545 N1 O2 2.793(10) no . 1_645 N1 O3 2.718(10) no . 1_545 N1 O7 2.691(10) no . 1_545 N2 O4 3.328(10) no . . N2 O5 2.826(11) no . . N2 O6 2.770(11) no . 1_455 N2 O8 2.682(10) no . 1_545 C3 C6 3.593(12) no . 2_866 C3 C8 3.569(15) no . 2_856 C4 O7 3.600(12) no . 2_766 C5 O7 3.454(11) no . . C6 C3 3.593(12) no . 2_866 C8 O2 3.595(13) no . 1_645 C8 O3 3.553(12) no . 1_545 C8 O7 3.516(13) no . 1_545 C8 C3 3.569(15) no . 2_856 C13 O2 3.547(13) no . 1_645 C16 C19 3.583(14) no . 2_777 C17 O8 3.441(13) no . 2_677 C18 O8 3.492(12) no . . C19 C16 3.583(14) no . 2_777 C21 O6 3.416(13) no . 1_455 C21 O8 3.463(12) no . 1_545 C31 O4 3.500(15) no . . C36 O1 3.419(15) no . 1_645 C36 O3 3.391(14) no . 1_545 C37 O3 3.572(13) no . 1_545 C39 O1 3.450(14) no . 1_645 C39 O3 3.347(13) no . 1_545 C40 O1 3.438(13) no . 1_545 C40 O2 3.356(14) no . . C41 O4 3.437(15) no . . C41 O6 3.378(14) no . 1_455 C42 O4 3.546(14) no . 1_455 C42 O6 3.465(14) no . 1_455 S1 H28 2.8264 no . . S1 H32 2.8710 no . . S2 H34 2.8451 no . . S2 H38 2.8651 no . . O1 H28 3.1240 no . . O2 H28 2.8845 no . . O3 H32 2.5573 no . . O4 H38 2.6288 no . . O5 H34 3.3256 no . . O5 H38 3.5764 no . . O6 H34 2.6923 no . . O7 H39A 2.8863 no . . O7 H39B 3.4629 no . . O7 H39C 2.7976 no . . O7 H40A 2.8473 no . . O7 H40B 3.4316 no . . O7 H40C 2.7531 no . . O8 H41A 2.7554 no . . O8 H41B 3.3987 no . . O8 H41C 2.7438 no . . O8 H42A 2.7919 no . . O8 H42B 3.4634 no . . O8 H42C 2.8856 no . . N1 H9 2.6134 no . . N1 H13 2.6408 no . . N2 H22 2.6402 no . . N2 H26 2.6335 no . . C1 H3 3.2559 no . . C1 H5 2.6122 no . . C1 H10 2.6971 no . . C1 H12 2.6092 no . . C2 H4 3.2595 no . . C2 H12 2.8878 no . . C4 H2 3.2510 no . . C4 H5 2.6869 no . 2_766 C5 H4 2.7041 no . 2_766 C5 H10 3.0274 no . . C6 H2 3.2900 no . . C6 H4 3.3274 no . . C6 H5 3.3074 no . 2_766 C6 H10 3.0864 no . . C7 H3 3.2588 no . . C7 H5 3.2985 no . . C8 H10 3.2481 no . . C8 H12 3.2019 no . . C9 H1A 3.1945 no . . C9 H1B 2.5922 no . . C9 H1C 2.7256 no . . C9 H13 3.2633 no . . C10 H5 2.6685 no . . C10 H12 3.2163 no . . C11 H2 2.6119 no . . C11 H5 2.5567 no . . C11 H9 3.2540 no . . C11 H13 3.2858 no . . C12 H2 2.8779 no . . C12 H5 3.4971 no . . C12 H10 3.2214 no . . C13 H1A 2.5027 no . . C13 H1B 3.0825 no . . C13 H1C 2.9621 no . . C13 H9 3.2556 no . . C14 H16 3.2692 no . . C14 H18 2.7025 no . . C14 H23 2.6089 no . . C14 H25 2.6808 no . . C15 H17 3.2542 no . . C15 H25 3.0053 no . . C17 H15 3.2361 no . . C17 H18 2.5833 no . 2_677 C18 H17 2.6241 no . 2_677 C18 H23 3.0214 no . . C19 H15 3.2850 no . . C19 H17 3.3196 no . . C19 H18 3.2449 no . 2_677 C19 H23 3.0065 no . . C20 H16 3.2594 no . . C20 H18 3.2824 no . . C21 H23 3.2187 no . . C21 H25 3.1927 no . . C22 H2A 2.6118 no . . C22 H2B 3.1911 no . . C22 H2C 2.7727 no . . C22 H26 3.2918 no . . C23 H18 2.7135 no . . C23 H25 3.2081 no . . C24 H15 2.5838 no . . C24 H18 2.6860 no . . C24 H22 3.2867 no . . C24 H26 3.2889 no . . C25 H15 2.9614 no . . C25 H23 3.2173 no . . C26 H2A 3.1190 no . . C26 H2B 2.4748 no . . C26 H2C 2.9347 no . . C26 H22 3.2887 no . . C27 H29 3.2356 no . . C27 H31 3.2484 no . . C28 H30 3.2384 no . . C28 H32 3.2163 no . . C29 H31 3.1839 no . . C30 H28 3.2263 no . . C30 H32 3.2412 no . . C31 H29 3.1809 no . . C32 H28 3.2157 no . . C32 H30 3.2566 no . . C33 H35 3.2643 no . . C33 H37 3.2372 no . . C34 H36 3.2186 no . . C34 H38 3.2627 no . . C35 H37 3.2230 no . . C36 H34 3.2133 no . . C36 H38 3.2535 no . . C37 H35 3.2319 no . . C38 H34 3.2530 no . . C38 H36 3.2500 no . . C39 H40A 2.6564 no . . C39 H40B 2.9444 no . . C39 H40C 3.5392 no . . C40 H39A 3.5527 no . . C40 H39B 2.8377 no . . C40 H39C 2.7601 no . . C41 H42A 3.5177 no . . C41 H42B 2.9662 no . . C41 H42C 2.6504 no . . C42 H41A 2.6817 no . . C42 H41B 2.8888 no . . C42 H41C 3.5433 no . . H1A H9 3.4667 no . . H1A H13 2.3507 no . . H1B H9 2.5071 no . . H1B H13 3.3297 no . . H1C H9 2.7438 no . . H1C H13 3.1409 no . . H2 H3 2.3451 no . . H2 H12 2.6494 no . . H2A H22 2.5218 no . . H2A H26 3.3545 no . . H2B H22 3.4765 no . . H2B H26 2.3171 no . . H2C H22 2.8251 no . . H2C H26 3.0927 no . . H3 H4 2.2580 no . . H4 H5 2.5481 no . 2_766 H5 H10 2.6134 no . . H9 H10 2.3085 no . . H12 H13 2.3129 no . . H15 H16 2.3292 no . . H15 H25 2.7689 no . . H16 H17 2.2999 no . . H17 H18 2.4231 no . 2_677 H18 H23 2.6442 no . . H22 H23 2.3390 no . . H25 H26 2.3010 no . . H28 H29 2.2716 no . . H29 H30 2.3037 no . . H30 H31 2.3248 no . . H31 H32 2.3037 no . . H34 H35 2.2970 no . . H35 H36 2.3308 no . . H36 H37 2.3012 no . . H37 H38 2.3074 no . . H39A H40A 3.5721 no . . H39B H40A 2.8715 no . . H39B H40B 2.7737 no . . H39C H40A 2.3932 no . . H39C H40B 3.1596 no . . H39C H40C 3.5988 no . . H41A H42A 3.5163 no . . H41A H42B 3.0944 no . . H41A H42C 2.3111 no . . H41B H42B 2.8579 no . . H41B H42C 2.9368 no . . H41C H42C 3.5431 no . . S1 H1A 2.8102 no . 1_465 S1 H1C 2.8423 no . 1_565 S1 H13 3.4282 no . 1_465 S1 H37 3.3867 no . 1_565 S1 H39B 3.4976 no . 1_565 S1 H40C 3.4263 no . . S2 H2B 2.7966 no . . S2 H2C 2.9025 no . 1_655 S2 H26 3.2466 no . . S2 H30 3.3540 no . 1_655 S2 H42B 3.2418 no . 1_655 S3 H1B 3.0795 no . 1_565 S3 H4 3.3877 no . 2_766 S3 H5 3.1751 no . . S4 H2A 3.0740 no . 1_565 S4 H17 3.4188 no . 2_677 S4 H18 3.2193 no . . O1 H1A 2.8318 no . 1_465 O1 H1C 3.3710 no . 1_465 O1 H13 3.0920 no . 1_465 O1 H35 3.4171 no . 1_465 O1 H36 2.6251 no . 1_465 O1 H37 3.0486 no . 1_565 O1 H39A 3.0875 no . 1_465 O1 H39B 3.1110 no . 1_465 O1 H39B 3.5180 no . 1_565 O1 H40B 2.5511 no . 1_565 O2 H1A 1.8976 no . 1_465 O2 H1B 3.1444 no . 1_465 O2 H1B 3.3544 no . 1_565 O2 H1C 3.2403 no . 1_465 O2 H1C 2.8830 no . 1_565 O2 H9 3.1443 no . 1_565 O2 H13 2.9046 no . 1_465 O2 H40A 3.4138 no . . O2 H40C 2.5161 no . . O3 H1A 3.0887 no . 1_565 O3 H1B 3.1341 no . 1_565 O3 H1C 1.8216 no . 1_565 O3 H28 3.1707 no . 1_655 O3 H36 2.7302 no . 1_565 O3 H37 3.0644 no . 1_565 O3 H39B 2.4567 no . 1_565 O4 H2B 2.7664 no . . O4 H2C 3.1107 no . . O4 H26 3.1630 no . . O4 H30 3.2228 no . . O4 H31 2.7823 no . . O4 H34 3.5170 no . 1_455 O4 H41B 2.6663 no . . O4 H41C 3.5245 no . . O4 H42B 2.6928 no . 1_655 O5 H2A 3.1928 no . . O5 H2A 3.3708 no . 1_655 O5 H2B 1.9319 no . . O5 H2C 3.2155 no . . O5 H2C 3.0333 no . 1_655 O5 H22 3.4614 no . 1_655 O5 H26 2.9477 no . . O5 H41A 3.3586 no . 1_545 O5 H42A 2.8602 no . 1_645 O6 H2A 3.1786 no . 1_655 O6 H2B 3.2740 no . 1_655 O6 H2C 1.8833 no . 1_655 O6 H26 3.3837 no . . O6 H30 2.7248 no . 1_655 O6 H41B 2.6348 no . 1_655 O6 H42B 2.7634 no . 1_655 O7 H1A 3.0285 no . 1_565 O7 H1B 1.7986 no . 1_565 O7 H1C 3.1471 no . 1_565 O7 H3 2.8639 no . 2_866 O7 H4 3.0787 no . 2_766 O7 H5 2.9203 no . . O7 H9 3.3708 no . 1_565 O8 H2A 1.7942 no . 1_565 O8 H2B 3.0125 no . 1_565 O8 H2C 3.1854 no . 1_565 O8 H16 3.0358 no . 2_777 O8 H17 2.8886 no . 2_677 O8 H18 2.9602 no . . O8 H22 3.3030 no . 1_565 N1 H3 3.1133 no . 2_856 N1 H28 3.3695 no . 1_645 N2 H16 3.2736 no . 2_767 N2 H34 3.2949 no . 1_455 N2 H41B 3.5110 no . . C1 H10 3.3128 no . 2_756 C2 H2 3.4016 no . 2_856 C2 H10 3.2807 no . 2_756 C3 H9 3.1869 no . 2_756 C4 H9 3.1305 no . 2_756 C4 H12 2.9547 no . 2_866 C5 H3 3.4635 no . 2_866 C5 H12 2.8757 no . 1_455 C7 H12 3.1035 no . 2_866 C8 H3 2.8306 no . 2_856 C8 H39A 3.2228 no . . C9 H2 3.5374 no . 2_856 C9 H3 3.2052 no . 2_856 C9 H13 3.2476 no . 1_455 C10 H2 3.2422 no . 2_856 C10 H10 3.4464 no . 2_756 C10 H12 3.3251 no . 1_455 C10 H13 3.5793 no . 1_455 C11 H2 3.0706 no . 2_856 C12 H2 3.1709 no . 2_856 C12 H4 3.2283 no . 2_866 C12 H5 3.4168 no . 1_655 C12 H10 3.2457 no . 1_655 C12 H39A 3.3331 no . . C13 H2 3.5051 no . 2_856 C13 H3 3.1889 no . 2_856 C13 H9 3.3450 no . 1_655 C13 H10 3.5696 no . 1_655 C13 H39A 2.8495 no . . C14 H23 3.2995 no . 2_667 C15 H15 3.3999 no . 2_767 C15 H22 3.5403 no . 2_667 C15 H23 3.2936 no . 2_667 C16 H22 3.1302 no . 2_667 C17 H22 3.1214 no . 2_667 C17 H25 2.9895 no . 2_777 C18 H16 3.4507 no . 2_777 C18 H25 2.9182 no . 1_455 C20 H25 3.2245 no . 2_777 C21 H16 2.8996 no . 2_767 C21 H41B 3.5116 no . . C21 H41C 3.5913 no . . C22 H16 3.2659 no . 2_767 C22 H26 3.2637 no . 1_455 C23 H15 3.2632 no . 2_767 C23 H23 3.3343 no . 2_667 C23 H25 3.3132 no . 1_455 C24 H15 3.0724 no . 2_767 C25 H15 3.1964 no . 2_767 C25 H17 3.2258 no . 2_777 C25 H18 3.3979 no . 1_655 C25 H23 3.3288 no . 1_655 C25 H41C 3.1910 no . . C26 H15 3.5601 no . 2_767 C26 H16 3.2112 no . 2_767 C26 H22 3.2806 no . 1_655 C26 H41B 3.4175 no . . C26 H41C 2.9937 no . . C27 H35 3.2624 no . 1_465 C27 H40A 3.4679 no . . C27 H40C 3.4181 no . . C28 H32 3.0949 no . 1_455 C28 H35 3.4971 no . 1_465 C28 H36 3.4153 no . 1_465 C28 H39C 3.5545 no . 1_455 C29 H31 3.5028 no . 1_455 C29 H32 3.1847 no . 1_455 C30 H38 3.2974 no . . C30 H41B 3.5671 no . . C30 H42B 3.4213 no . . C31 H29 3.2221 no . 1_655 C31 H38 3.2986 no . . C32 H28 3.3906 no . 1_655 C32 H29 3.2450 no . 1_655 C32 H35 3.3835 no . 1_465 C32 H37 3.5229 no . 1_565 C32 H40A 3.4978 no . . C33 H29 3.2170 no . 1_655 C33 H30 3.0337 no . 1_655 C34 H2C 3.4788 no . 1_655 C34 H30 3.0152 no . 1_655 C34 H38 3.0953 no . 1_655 C34 H42A 3.5211 no . 1_645 C34 H42C 2.9082 no . 1_645 C35 H37 3.4883 no . 1_655 C35 H38 3.0417 no . 1_655 C35 H42C 3.3230 no . 1_645 C36 H32 2.9227 no . 1_545 C36 H39B 3.0727 no . . C37 H29 3.2287 no . 1_655 C37 H32 3.1771 no . 1_545 C37 H35 3.1497 no . 1_455 C37 H39B 3.2764 no . . C37 H40B 3.5535 no . . C38 H29 2.9604 no . 1_655 C38 H34 3.4396 no . 1_455 C38 H35 3.0684 no . 1_455 C39 H36 3.2285 no . . C39 H37 3.5679 no . . C39 H40B 3.3302 no . 1_655 C39 H40C 3.2942 no . 1_655 C40 H1B 3.4087 no . 1_565 C40 H37 3.3391 no . . C40 H39A 3.3701 no . 1_455 C40 H39C 3.2331 no . 1_455 C41 H42A 3.0149 no . 1_655 C42 H2A 3.4861 no . 1_565 C42 H34 3.4090 no . 1_465 C42 H41A 3.3050 no . 1_455 C42 H41C 3.4134 no . 1_455 H1A S1 2.8102 no . 1_645 H1A O1 2.8318 no . 1_645 H1A O2 1.8976 no . 1_645 H1A O3 3.0887 no . 1_545 H1A O7 3.0285 no . 1_545 H1A H3 3.2128 no . 2_856 H1A H28 2.9495 no . 1_645 H1B S3 3.0795 no . 1_545 H1B O2 3.3544 no . 1_545 H1B O2 3.1444 no . 1_645 H1B O3 3.1341 no . 1_545 H1B O7 1.7986 no . 1_545 H1B C40 3.4087 no . 1_545 H1B H3 2.7745 no . 2_856 H1B H28 3.5467 no . 1_645 H1B H39C 3.5312 no . 1_545 H1B H40A 3.2339 no . 1_545 H1B H40C 3.3141 no . 1_545 H1C S1 2.8423 no . 1_545 H1C O1 3.3710 no . 1_645 H1C O2 2.8830 no . 1_545 H1C O2 3.2403 no . 1_645 H1C O3 1.8216 no . 1_545 H1C O7 3.1471 no . 1_545 H1C H28 3.1105 no . 1_645 H1C H39A 3.4069 no . . H1C H39B 3.0107 no . . H1C H40A 3.5336 no . 1_545 H2 C2 3.4016 no . 2_856 H2 C9 3.5374 no . 2_856 H2 C10 3.2422 no . 2_856 H2 C11 3.0706 no . 2_856 H2 C12 3.1709 no . 2_856 H2 C13 3.5051 no . 2_856 H2 H2 2.7621 no . 2_856 H2 H10 3.2432 no . 1_655 H2 H10 3.4431 no . 2_756 H2 H12 3.5374 no . 2_856 H2A S4 3.0740 no . 1_545 H2A O5 3.3708 no . 1_455 H2A O5 3.1928 no . . H2A O6 3.1786 no . 1_455 H2A O8 1.7942 no . 1_545 H2A C42 3.4861 no . 1_545 H2A H16 3.0229 no . 2_767 H2A H34 3.3723 no . 1_455 H2A H41A 3.3410 no . 1_545 H2A H42A 3.4601 no . 1_545 H2A H42C 3.2830 no . 1_545 H2B S2 2.7966 no . . H2B O4 2.7664 no . . H2B O5 1.9319 no . . H2B O6 3.2740 no . 1_455 H2B O8 3.0125 no . 1_545 H2B H16 3.3057 no . 2_767 H2B H34 3.2980 no . 1_455 H2B H41A 3.5244 no . 1_545 H2B H41B 3.5900 no . . H2C S2 2.9025 no . 1_455 H2C O4 3.1107 no . . H2C O5 3.0333 no . 1_455 H2C O5 3.2155 no . . H2C O6 1.8833 no . 1_455 H2C O8 3.1854 no . 1_545 H2C C34 3.4788 no . 1_455 H2C H34 2.7262 no . 1_455 H2C H41B 2.9871 no . . H3 O7 2.8639 no . 2_866 H3 N1 3.1133 no . 2_856 H3 C5 3.4635 no . 2_866 H3 C8 2.8306 no . 2_856 H3 C9 3.2052 no . 2_856 H3 C13 3.1889 no . 2_856 H3 H1A 3.2128 no . 2_856 H3 H1B 2.7745 no . 2_856 H3 H5 3.5911 no . 2_866 H3 H9 3.4438 no . 2_756 H3 H9 3.4979 no . 2_856 H3 H13 3.4959 no . 2_856 H4 S3 3.3877 no . 2_766 H4 O7 3.0787 no . 2_766 H4 C12 3.2283 no . 2_866 H4 H9 3.2896 no . 2_756 H4 H12 2.6235 no . 2_866 H4 H39A 3.5568 no . 2_866 H4 H40C 3.4260 no . 2_766 H5 S3 3.1751 no . . H5 O7 2.9203 no . . H5 C12 3.4168 no . 1_455 H5 H3 3.5911 no . 2_866 H5 H12 2.4973 no . 1_455 H9 O2 3.1443 no . 1_545 H9 O7 3.3708 no . 1_545 H9 C3 3.1869 no . 2_756 H9 C4 3.1305 no . 2_756 H9 C13 3.3450 no . 1_455 H9 H3 3.4438 no . 2_756 H9 H3 3.4979 no . 2_856 H9 H4 3.2896 no . 2_756 H9 H13 2.7815 no . 1_455 H10 C1 3.3128 no . 2_756 H10 C2 3.2807 no . 2_756 H10 C10 3.4464 no . 2_756 H10 C12 3.2457 no . 1_455 H10 C13 3.5696 no . 1_455 H10 H2 3.2432 no . 1_455 H10 H2 3.4431 no . 2_756 H10 H10 2.9915 no . 2_756 H10 H12 2.7320 no . 1_455 H10 H13 3.3778 no . 1_455 H12 C4 2.9547 no . 2_866 H12 C5 2.8757 no . 1_655 H12 C7 3.1035 no . 2_866 H12 C10 3.3251 no . 1_655 H12 H2 3.5374 no . 2_856 H12 H4 2.6235 no . 2_866 H12 H5 2.4973 no . 1_655 H12 H10 2.7320 no . 1_655 H13 S1 3.4282 no . 1_645 H13 O1 3.0920 no . 1_645 H13 O2 2.9046 no . 1_645 H13 C9 3.2476 no . 1_655 H13 C10 3.5793 no . 1_655 H13 H3 3.4959 no . 2_856 H13 H9 2.7815 no . 1_655 H13 H10 3.3778 no . 1_655 H13 H39A 2.8271 no . . H15 C15 3.3999 no . 2_767 H15 C23 3.2632 no . 2_767 H15 C24 3.0724 no . 2_767 H15 C25 3.1964 no . 2_767 H15 C26 3.5601 no . 2_767 H15 H15 2.7404 no . 2_767 H15 H23 3.2122 no . 1_655 H15 H23 3.4286 no . 2_667 H15 H25 3.5559 no . 2_767 H16 O8 3.0358 no . 2_777 H16 N2 3.2736 no . 2_767 H16 C18 3.4507 no . 2_777 H16 C21 2.8996 no . 2_767 H16 C22 3.2659 no . 2_767 H16 C26 3.2112 no . 2_767 H16 H2A 3.0229 no . 2_767 H16 H2B 3.3057 no . 2_767 H16 H18 3.5985 no . 2_777 H16 H22 3.3915 no . 2_667 H16 H22 3.5882 no . 2_767 H16 H26 3.5095 no . 2_767 H17 S4 3.4188 no . 2_677 H17 O8 2.8886 no . 2_677 H17 C25 3.2258 no . 2_777 H17 H22 3.3124 no . 2_667 H17 H25 2.5981 no . 2_777 H17 H41C 2.9850 no . 2_777 H18 S4 3.2193 no . . H18 O8 2.9602 no . . H18 C25 3.3979 no . 1_455 H18 H16 3.5985 no . 2_777 H18 H25 2.4641 no . 1_455 H22 O5 3.4614 no . 1_455 H22 O8 3.3030 no . 1_545 H22 C15 3.5403 no . 2_667 H22 C16 3.1302 no . 2_667 H22 C17 3.1214 no . 2_667 H22 C26 3.2806 no . 1_455 H22 H16 3.3915 no . 2_667 H22 H16 3.5882 no . 2_767 H22 H17 3.3124 no . 2_667 H22 H26 2.7545 no . 1_455 H23 C14 3.2995 no . 2_667 H23 C15 3.2936 no . 2_667 H23 C23 3.3343 no . 2_667 H23 C25 3.3288 no . 1_455 H23 H15 3.2122 no . 1_455 H23 H15 3.4286 no . 2_667 H23 H23 2.8403 no . 2_667 H23 H25 2.7868 no . 1_455 H23 H26 3.5967 no . 1_455 H25 C17 2.9895 no . 2_777 H25 C18 2.9182 no . 1_655 H25 C20 3.2245 no . 2_777 H25 C23 3.3132 no . 1_655 H25 H15 3.5559 no . 2_767 H25 H17 2.5981 no . 2_777 H25 H18 2.4641 no . 1_655 H25 H23 2.7868 no . 1_655 H25 H41C 3.3173 no . . H26 S2 3.2466 no . . H26 O4 3.1630 no . . H26 O5 2.9477 no . . H26 O6 3.3837 no . . H26 C22 3.2637 no . 1_655 H26 H16 3.5095 no . 2_767 H26 H22 2.7545 no . 1_655 H26 H23 3.5967 no . 1_655 H26 H41B 3.3603 no . . H26 H41C 3.0060 no . . H28 O3 3.1707 no . 1_455 H28 N1 3.3695 no . 1_465 H28 C32 3.3906 no . 1_455 H28 H1A 2.9495 no . 1_465 H28 H1B 3.5467 no . 1_465 H28 H1C 3.1105 no . 1_465 H28 H32 2.6639 no . 1_455 H28 H36 3.1961 no . 1_465 H28 H39C 3.1925 no . 1_455 H28 H40A 3.0118 no . 1_455 H29 C31 3.2221 no . 1_455 H29 C32 3.2450 no . 1_455 H29 C33 3.2170 no . 1_455 H29 C37 3.2287 no . 1_455 H29 C38 2.9604 no . 1_455 H29 H31 2.8511 no . 1_455 H29 H32 2.8528 no . 1_455 H29 H37 3.5925 no . 1_455 H29 H38 3.1710 no . 1_455 H29 H40A 3.4696 no . 1_455 H30 S2 3.3540 no . 1_455 H30 O4 3.2228 no . . H30 O6 2.7248 no . 1_455 H30 C33 3.0337 no . 1_455 H30 C34 3.0152 no . 1_455 H30 H34 3.0256 no . 1_455 H30 H38 3.1268 no . . H30 H41B 2.9430 no . . H30 H42B 2.9727 no . . H30 H42C 3.5341 no . . H31 O4 2.7823 no . . H31 C29 3.5028 no . 1_655 H31 H29 2.8511 no . 1_655 H31 H38 3.1258 no . . H31 H41A 3.3775 no . . H31 H41B 3.2914 no . . H31 H42A 3.5588 no . 1_655 H31 H42B 2.9943 no . 1_655 H32 C28 3.0949 no . 1_655 H32 C29 3.1847 no . 1_655 H32 C36 2.9227 no . 1_565 H32 C37 3.1771 no . 1_565 H32 H28 2.6639 no . 1_655 H32 H29 2.8528 no . 1_655 H32 H36 2.7819 no . 1_565 H32 H37 3.1789 no . 1_565 H32 H40A 3.5397 no . . H34 O4 3.5170 no . 1_655 H34 N2 3.2949 no . 1_655 H34 C38 3.4396 no . 1_655 H34 C42 3.4090 no . 1_645 H34 H2A 3.3723 no . 1_655 H34 H2B 3.2980 no . 1_655 H34 H2C 2.7262 no . 1_655 H34 H30 3.0256 no . 1_655 H34 H38 2.7374 no . 1_655 H34 H42A 3.4027 no . 1_645 H34 H42C 2.5982 no . 1_645 H35 O1 3.4171 no . 1_645 H35 C27 3.2624 no . 1_645 H35 C28 3.4971 no . 1_645 H35 C32 3.3835 no . 1_645 H35 C37 3.1497 no . 1_655 H35 C38 3.0684 no . 1_655 H35 H37 2.8056 no . 1_655 H35 H38 2.6824 no . 1_655 H35 H42C 3.3097 no . 1_645 H36 O1 2.6251 no . 1_645 H36 O3 2.7302 no . 1_545 H36 C28 3.4153 no . 1_645 H36 C39 3.2285 no . . H36 H28 3.1961 no . 1_645 H36 H32 2.7819 no . 1_545 H36 H39B 2.4456 no . . H36 H39C 3.2522 no . . H37 S1 3.3867 no . 1_545 H37 O1 3.0486 no . 1_545 H37 O3 3.0644 no . 1_545 H37 C32 3.5229 no . 1_545 H37 C35 3.4883 no . 1_455 H37 C39 3.5679 no . . H37 C40 3.3391 no . . H37 H29 3.5925 no . 1_655 H37 H32 3.1789 no . 1_545 H37 H35 2.8056 no . 1_455 H37 H39B 2.8530 no . . H37 H39C 3.5497 no . . H37 H40A 3.1470 no . . H37 H40B 2.7099 no . . H38 C30 3.2974 no . . H38 C31 3.2986 no . . H38 C34 3.0953 no . 1_455 H38 C35 3.0417 no . 1_455 H38 H29 3.1710 no . 1_655 H38 H30 3.1268 no . . H38 H31 3.1258 no . . H38 H34 2.7374 no . 1_455 H38 H35 2.6824 no . 1_455 H39A O1 3.0875 no . 1_645 H39A C8 3.2228 no . . H39A C12 3.3331 no . . H39A C13 2.8495 no . . H39A C40 3.3701 no . 1_655 H39A H1C 3.4069 no . . H39A H4 3.5568 no . 2_866 H39A H13 2.8271 no . . H39A H40B 3.0093 no . 1_655 H39A H40C 3.0135 no . 1_655 H39B S1 3.4976 no . 1_545 H39B O1 3.5180 no . 1_545 H39B O1 3.1110 no . 1_645 H39B O3 2.4567 no . 1_545 H39B C36 3.0727 no . . H39B C37 3.2764 no . . H39B H1C 3.0107 no . . H39B H36 2.4456 no . . H39B H37 2.8530 no . . H39C C28 3.5545 no . 1_655 H39C C40 3.2331 no . 1_655 H39C H1B 3.5312 no . 1_565 H39C H28 3.1925 no . 1_655 H39C H36 3.2522 no . . H39C H37 3.5497 no . . H39C H40B 2.8927 no . 1_655 H39C H40C 2.6909 no . 1_655 H40A O2 3.4138 no . . H40A C27 3.4679 no . . H40A C32 3.4978 no . . H40A H1B 3.2339 no . 1_565 H40A H1C 3.5336 no . 1_565 H40A H28 3.0118 no . 1_655 H40A H29 3.4696 no . 1_655 H40A H32 3.5397 no . . H40A H37 3.1470 no . . H40B O1 2.5511 no . 1_545 H40B C37 3.5535 no . . H40B C39 3.3302 no . 1_455 H40B H37 2.7099 no . . H40B H39A 3.0093 no . 1_455 H40B H39C 2.8927 no . 1_455 H40C S1 3.4263 no . . H40C O2 2.5161 no . . H40C C27 3.4181 no . . H40C C39 3.2942 no . 1_455 H40C H1B 3.3141 no . 1_565 H40C H4 3.4260 no . 2_766 H40C H39A 3.0135 no . 1_455 H40C H39C 2.6909 no . 1_455 H41A O5 3.3586 no . 1_565 H41A C42 3.3050 no . 1_655 H41A H2A 3.3410 no . 1_565 H41A H2B 3.5244 no . 1_565 H41A H31 3.3775 no . . H41A H42A 2.4907 no . 1_655 H41A H42B 3.3301 no . 1_655 H41B O4 2.6663 no . . H41B O6 2.6348 no . 1_455 H41B N2 3.5110 no . . H41B C21 3.5116 no . . H41B C26 3.4175 no . . H41B C30 3.5671 no . . H41B H2B 3.5900 no . . H41B H2C 2.9871 no . . H41B H26 3.3603 no . . H41B H30 2.9430 no . . H41B H31 3.2914 no . . H41B H42A 3.3251 no . 1_655 H41B H42B 3.5114 no . 1_655 H41C O4 3.5245 no . . H41C C21 3.5913 no . . H41C C25 3.1910 no . . H41C C26 2.9937 no . . H41C C42 3.4134 no . 1_655 H41C H17 2.9850 no . 2_777 H41C H25 3.3173 no . . H41C H26 3.0060 no . . H41C H42A 2.7974 no . 1_655 H41C H42B 3.4592 no . 1_655 H42A O5 2.8602 no . 1_465 H42A C34 3.5211 no . 1_465 H42A C41 3.0149 no . 1_455 H42A H2A 3.4601 no . 1_565 H42A H31 3.5588 no . 1_455 H42A H34 3.4027 no . 1_465 H42A H41A 2.4907 no . 1_455 H42A H41B 3.3251 no . 1_455 H42A H41C 2.7974 no . 1_455 H42B S2 3.2418 no . 1_455 H42B O4 2.6928 no . 1_455 H42B O6 2.7634 no . 1_455 H42B C30 3.4213 no . . H42B H30 2.9727 no . . H42B H31 2.9943 no . 1_455 H42B H41A 3.3301 no . 1_455 H42B H41B 3.5114 no . 1_455 H42B H41C 3.4592 no . 1_455 H42C C34 2.9082 no . 1_465 H42C C35 3.3230 no . 1_465 H42C H2A 3.2830 no . 1_565 H42C H30 3.5341 no . . H42C H34 2.5982 no . 1_465 H42C H35 3.3097 no . 1_465 #============================================================================== loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_D _geom_hbond_site_symmetry_H _geom_hbond_site_symmetry_A _geom_hbond_distance_DA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H1A O2 . . 1_645 2.793(10) 0.900 1.898 173.0 no N1 H1B O7 . . 1_545 2.691(10) 0.900 1.799 170.9 no N1 H1C O3 . . 1_545 2.718(10) 0.900 1.822 173.9 no N2 H2A O8 . . 1_545 2.682(10) 0.900 1.794 168.3 no N2 H2B O5 . . . 2.826(11) 0.900 1.932 172.2 no N2 H2C O6 . . 1_455 2.770(11) 0.900 1.883 167.9 no #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== _database_code_depnum_ccdc_archive 'CCDC 941422'