# Supplementary Material (ESI) for Perkin Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 207/484 data_PC-2 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 5 14:23:14 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution 'DIRDIF92 (PATTY)' _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 375.54 _chemical_formula_analytical ? _chemical_formula_sum 'C22 H30 F N O S ' _chemical_formula_moiety 'C22 H30 F N O S ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.860(5) _cell_length_b 13.058(3) _cell_length_c 13.784(3) _cell_angle_alpha 90 _cell_angle_beta 98.57(2) _cell_angle_gamma 90 _cell_volume 2110(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,-z -x,-y,-z 1/2+x,1/2-y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808.00 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.75 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 2 -1 -1 2 0 0 2 0 1 _diffrn_reflns_number 5302 _reflns_number_total 5066 _reflns_number_gt 3499 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.048 _diffrn_reflns_av_sigmaI/netI 0.038 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.63 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.04924 _diffrn_orient_matrix_UB_12 -0.01017 _diffrn_orient_matrix_UB_13 0.06475 _diffrn_orient_matrix_UB_21 -0.03062 _diffrn_orient_matrix_UB_22 -0.07102 _diffrn_orient_matrix_UB_23 0.00366 _diffrn_orient_matrix_UB_31 0.06252 _diffrn_orient_matrix_UB_32 -0.02677 _diffrn_orient_matrix_UB_33 -0.03430 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S S 0.24791(6) 0.04800(5) 0.05257(4) 0.0551(2) Uani 1.00 d . . . F(1) F 0.0237(1) 0.4019(1) 0.2571(1) 0.0573(4) Uani 1.00 d . . . O O 0.3219(1) 0.2093(1) 0.2431(1) 0.0386(4) Uani 1.00 d . . . N N 0.4299(2) 0.0793(2) 0.6139(2) 0.0700(7) Uani 1.00 d . . . C(1) C 0.1148(2) 0.3419(1) 0.2240(1) 0.0339(5) Uani 1.00 d . . . C(2) C 0.0537(2) 0.2859(2) 0.1335(1) 0.0388(5) Uani 1.00 d . . . C(3) C 0.1274(2) 0.2175(2) 0.0784(1) 0.0425(6) Uani 1.00 d . . . C(4) C 0.1371(2) 0.1072(2) 0.1152(1) 0.0388(5) Uani 1.00 d . . . C(5) C 0.1578(2) 0.0910(1) 0.2276(1) 0.0346(5) Uani 1.00 d . . . C(6) C 0.2796(2) 0.1194(1) 0.3858(1) 0.0364(5) Uani 1.00 d . . . C(7) C 0.3485(2) 0.1884(2) 0.4611(1) 0.0385(5) Uani 1.00 d . . . C(8) C 0.2776(2) 0.2795(2) 0.4895(2) 0.0493(6) Uani 1.00 d . . . C(9) C 0.2351(2) 0.3349(2) 0.3927(2) 0.0457(6) Uani 1.00 d . . . C(10) C 0.1629(1) 0.2710(1) 0.3122(1) 0.0315(5) Uani 1.00 d . . . C(11) C 0.2293(1) 0.1741(1) 0.2897(1) 0.0308(5) Uani 1.00 d . . . C(12) C 0.2015(2) 0.4174(2) 0.1932(2) 0.0468(6) Uani 1.00 d . . . C(13) C 0.2535(2) -0.0795(2) 0.0984(1) 0.0434(6) Uani 1.00 d . . . C(14) C 0.3525(2) -0.1137(2) 0.1534(2) 0.0533(7) Uani 1.00 d . . . C(15) C 0.3598(3) -0.2127(2) 0.1890(2) 0.0667(8) Uani 1.00 d . . . C(16) C 0.2684(3) -0.2769(2) 0.1700(2) 0.0702(9) Uani 1.00 d . . . C(17) C 0.1694(3) -0.2431(2) 0.1154(3) 0.0755(10) Uani 1.00 d . . . C(18) C 0.1623(2) -0.1454(2) 0.0799(2) 0.0639(8) Uani 1.00 d . . . C(19) C 0.0444(2) 0.0648(2) 0.2635(2) 0.0457(6) Uani 1.00 d . . . C(20) C 0.3963(2) 0.1274(2) 0.5473(2) 0.0472(6) Uani 1.00 d . . . C(21) C 0.1805(3) 0.2443(3) 0.5421(2) 0.0770(10) Uani 1.00 d . . . C(22) C 0.3549(3) 0.3520(2) 0.5571(2) 0.088(1) Uani 1.00 d . . . H(1) H 0.0178 0.3392 0.0911 0.049(6) Uiso 1.00 calc . . . H(2) H -0.0122 0.2394 0.1484 0.035(5) Uiso 1.00 calc . . . H(3) H 0.1987 0.2435 0.0822 0.044(6) Uiso 1.00 calc . . . H(4) H 0.0951 0.2188 0.0086 0.052(6) Uiso 1.00 calc . . . H(5) H 0.0655 0.0713 0.0942 0.041(6) Uiso 1.00 calc . . . H(6) H 0.2082 0.0248 0.2399 0.033(5) Uiso 1.00 calc . . . H(7) H 0.2199 0.0887 0.4152 0.046(6) Uiso 1.00 calc . . . H(8) H 0.3283 0.0626 0.3706 0.048(6) Uiso 1.00 calc . . . H(9) H 0.3100 0.3587 0.3635 0.062(7) Uiso 1.00 calc . . . H(10) H 0.1952 0.3889 0.4094 0.058(7) Uiso 1.00 calc . . . H(11) H 0.0975 0.2431 0.3354 0.039(6) Uiso 1.00 calc . . . H(12) H 0.3684 0.1563 0.2427 0.076(9) Uiso 1.00 calc . . . H(13) H 0.2670 0.3842 0.1770 0.050(6) Uiso 1.00 calc . . . H(14) H 0.2265 0.4662 0.2432 0.053(7) Uiso 1.00 calc . . . H(15) H 0.1671 0.4545 0.1405 0.058(7) Uiso 1.00 calc . . . H(16) H 0.4167 -0.0751 0.1639 0.052(7) Uiso 1.00 calc . . . H(17) H 0.4285 -0.2304 0.2301 0.082(9) Uiso 1.00 calc . . . H(18) H 0.2737 -0.3447 0.1951 0.09(1) Uiso 1.00 calc . . . H(19) H 0.1060 -0.2880 0.1023 0.092(10) Uiso 1.00 calc . . . H(20) H 0.1031 -0.1234 0.0470 0.078(10) Uiso 1.00 calc . . . H(21) H 0.0530 0.0567 0.3375 0.058(7) Uiso 1.00 calc . . . H(22) H -0.0122 0.1142 0.2465 0.062(7) Uiso 1.00 calc . . . H(23) H 0.0153 0.0078 0.2312 0.055(7) Uiso 1.00 calc . . . H(24) H 0.1405 0.3015 0.5612 0.12(1) Uiso 1.00 calc . . . H(25) H 0.1297 0.2021 0.4988 0.09(1) Uiso 1.00 calc . . . H(26) H 0.2104 0.2052 0.5983 0.082(9) Uiso 1.00 calc . . . H(27) H 0.3929 0.3159 0.6116 0.11(1) Uiso 1.00 calc . . . H(28) H 0.4114 0.3804 0.5208 0.09(1) Uiso 1.00 calc . . . H(29) H 0.3118 0.4064 0.5778 0.12(1) Uiso 1.00 calc . . . H(30) H 0.4113 0.2154 0.4323 0.046(6) Uiso 1.00 calc . . . 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 S 0.0757(4) 0.0445(3) 0.0507(4) 0.0107(3) 0.0277(3) -0.0013(3) F(1) 0.0462(7) 0.0512(8) 0.0731(9) 0.0074(6) 0.0046(6) -0.0041(7) O 0.0328(7) 0.0352(7) 0.0502(8) 0.0033(6) 0.0146(6) 0.0083(6) N 0.078(2) 0.060(1) 0.063(1) -0.004(1) -0.017(1) 0.022(1) C(1) 0.0296(9) 0.0307(10) 0.041(1) 0.0033(7) 0.0049(8) 0.0038(8) C(2) 0.039(1) 0.040(1) 0.036(1) 0.0071(9) 0.0001(8) 0.0035(9) C(3) 0.050(1) 0.046(1) 0.031(1) 0.0076(10) 0.0058(9) 0.0031(9) C(4) 0.043(1) 0.040(1) 0.034(1) 0.0029(9) 0.0052(8) -0.0036(9) C(5) 0.039(1) 0.0312(10) 0.0345(10) 0.0008(8) 0.0073(8) -0.0003(8) C(6) 0.038(1) 0.0315(10) 0.038(1) 0.0014(8) 0.0035(8) 0.0060(8) C(7) 0.037(1) 0.036(1) 0.041(1) 0.0021(8) -0.0004(8) 0.0060(9) C(8) 0.052(1) 0.047(1) 0.043(1) 0.013(1) -0.0110(10) -0.009(1) C(9) 0.049(1) 0.032(1) 0.051(1) 0.0100(9) -0.010(1) -0.0061(9) C(10) 0.0274(9) 0.0314(9) 0.0358(10) 0.0025(7) 0.0046(7) 0.0005(8) C(11) 0.0300(9) 0.0301(9) 0.0333(9) 0.0014(7) 0.0075(7) 0.0032(8) C(12) 0.040(1) 0.042(1) 0.058(1) -0.0013(10) 0.005(1) 0.015(1) C(13) 0.053(1) 0.041(1) 0.037(1) 0.0035(10) 0.0101(9) -0.0098(9) C(14) 0.058(1) 0.050(1) 0.051(1) -0.001(1) 0.004(1) -0.011(1) C(15) 0.083(2) 0.062(2) 0.052(1) 0.014(1) -0.001(1) -0.002(1) C(16) 0.109(2) 0.046(2) 0.059(2) -0.001(2) 0.023(2) -0.003(1) C(17) 0.084(2) 0.055(2) 0.088(2) -0.018(2) 0.016(2) -0.014(2) C(18) 0.057(2) 0.058(2) 0.073(2) -0.002(1) -0.002(1) -0.013(1) C(19) 0.045(1) 0.046(1) 0.047(1) -0.012(1) 0.0079(9) 0.000(1) C(20) 0.044(1) 0.043(1) 0.051(1) -0.0019(10) -0.0071(10) 0.005(1) C(21) 0.075(2) 0.117(3) 0.039(1) 0.038(2) 0.011(1) 0.004(2) C(22) 0.108(3) 0.056(2) 0.079(2) 0.025(2) -0.050(2) -0.027(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]' _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.021(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3499 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0626 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.461 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.37 _refine_diff_density_max 0.45 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag S C(4) 1.846(2) 1_555 1_555 yes S C(13) 1.778(2) 1_555 1_555 yes F(1) C(1) 1.462(2) 1_555 1_555 yes O C(11) 1.429(2) 1_555 1_555 yes O H(12) 0.886(1) 1_555 1_555 no N C(20) 1.134(3) 1_555 1_555 yes C(1) C(2) 1.532(3) 1_555 1_555 yes C(1) C(10) 1.567(3) 1_555 1_555 yes C(1) C(12) 1.529(3) 1_555 1_555 yes C(2) C(3) 1.530(3) 1_555 1_555 yes C(2) H(1) 0.966(2) 1_555 1_555 no C(2) H(2) 1.034(2) 1_555 1_555 no C(3) C(4) 1.525(3) 1_555 1_555 yes C(3) H(3) 0.906(2) 1_555 1_555 no C(3) H(4) 0.981(2) 1_555 1_555 no C(4) C(5) 1.547(3) 1_555 1_555 yes C(4) H(5) 0.975(2) 1_555 1_555 no C(5) C(11) 1.553(3) 1_555 1_555 yes C(5) C(19) 1.539(3) 1_555 1_555 yes C(5) H(6) 1.051(2) 1_555 1_555 no C(6) C(7) 1.519(3) 1_555 1_555 yes C(6) C(11) 1.544(3) 1_555 1_555 yes C(6) H(7) 0.955(2) 1_555 1_555 no C(6) H(8) 0.982(2) 1_555 1_555 no C(7) C(8) 1.541(3) 1_555 1_555 yes C(7) C(20) 1.472(3) 1_555 1_555 yes C(7) H(30) 0.962(2) 1_555 1_555 no C(8) C(9) 1.536(3) 1_555 1_555 yes C(8) C(21) 1.521(4) 1_555 1_555 yes C(8) C(22) 1.533(3) 1_555 1_555 yes C(9) C(10) 1.542(3) 1_555 1_555 yes C(9) H(9) 1.074(2) 1_555 1_555 no C(9) H(10) 0.899(2) 1_555 1_555 no C(10) C(11) 1.547(3) 1_555 1_555 yes C(10) H(11) 0.953(2) 1_555 1_555 no C(12) H(13) 0.946(2) 1_555 1_555 no C(12) H(14) 0.952(2) 1_555 1_555 no C(12) H(15) 0.918(2) 1_555 1_555 no C(13) C(14) 1.375(3) 1_555 1_555 yes C(13) C(18) 1.376(3) 1_555 1_555 yes C(14) C(15) 1.381(4) 1_555 1_555 yes C(14) H(16) 0.906(2) 1_555 1_555 no C(15) C(16) 1.364(4) 1_555 1_555 yes C(15) H(17) 0.948(3) 1_555 1_555 no C(16) C(17) 1.370(4) 1_555 1_555 yes C(16) H(18) 0.950(3) 1_555 1_555 no C(17) C(18) 1.365(4) 1_555 1_555 yes C(17) H(19) 0.948(3) 1_555 1_555 no C(18) H(20) 0.828(3) 1_555 1_555 no C(19) H(21) 1.016(2) 1_555 1_555 no C(19) H(22) 0.936(2) 1_555 1_555 no C(19) H(23) 0.908(2) 1_555 1_555 no C(21) H(24) 0.944(3) 1_555 1_555 no C(21) H(25) 0.956(4) 1_555 1_555 no C(21) H(26) 0.951(3) 1_555 1_555 no C(22) H(27) 0.943(3) 1_555 1_555 no C(22) H(28) 0.968(5) 1_555 1_555 no C(22) H(29) 0.944(3) 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(4) S C(13) 102.60(10) 1_555 1_555 1_555 yes C(11) O H(12) 105.8(1) 1_555 1_555 1_555 no F(1) C(1) C(2) 103.1(1) 1_555 1_555 1_555 yes F(1) C(1) C(10) 105.9(1) 1_555 1_555 1_555 yes F(1) C(1) C(12) 107.4(2) 1_555 1_555 1_555 yes C(2) C(1) C(10) 115.0(2) 1_555 1_555 1_555 yes C(2) C(1) C(12) 109.8(2) 1_555 1_555 1_555 yes C(10) C(1) C(12) 114.5(2) 1_555 1_555 1_555 yes C(1) C(2) C(3) 116.5(2) 1_555 1_555 1_555 yes C(1) C(2) H(1) 105.1(2) 1_555 1_555 1_555 no C(1) C(2) H(2) 113.5(2) 1_555 1_555 1_555 no C(3) C(2) H(1) 110.7(2) 1_555 1_555 1_555 no C(3) C(2) H(2) 105.1(2) 1_555 1_555 1_555 no H(1) C(2) H(2) 105.4(2) 1_555 1_555 1_555 no C(2) C(3) C(4) 114.0(2) 1_555 1_555 1_555 yes C(2) C(3) H(3) 110.5(2) 1_555 1_555 1_555 no C(2) C(3) H(4) 107.9(2) 1_555 1_555 1_555 no C(4) C(3) H(3) 108.2(2) 1_555 1_555 1_555 no C(4) C(3) H(4) 110.0(2) 1_555 1_555 1_555 no H(3) C(3) H(4) 105.9(2) 1_555 1_555 1_555 no S C(4) C(3) 105.3(1) 1_555 1_555 1_555 yes S C(4) C(5) 113.1(1) 1_555 1_555 1_555 yes S C(4) H(5) 108.0(1) 1_555 1_555 1_555 no C(3) C(4) C(5) 117.1(2) 1_555 1_555 1_555 yes C(3) C(4) H(5) 109.7(2) 1_555 1_555 1_555 no C(5) C(4) H(5) 103.4(2) 1_555 1_555 1_555 no C(4) C(5) C(11) 116.7(2) 1_555 1_555 1_555 yes C(4) C(5) C(19) 109.7(2) 1_555 1_555 1_555 yes C(4) C(5) H(6) 106.0(2) 1_555 1_555 1_555 no C(11) C(5) C(19) 114.2(2) 1_555 1_555 1_555 yes C(11) C(5) H(6) 103.6(2) 1_555 1_555 1_555 no C(19) C(5) H(6) 105.6(2) 1_555 1_555 1_555 no C(7) C(6) C(11) 114.3(2) 1_555 1_555 1_555 yes C(7) C(6) H(7) 108.5(2) 1_555 1_555 1_555 no C(7) C(6) H(8) 108.7(2) 1_555 1_555 1_555 no C(11) C(6) H(7) 110.0(2) 1_555 1_555 1_555 no C(11) C(6) H(8) 109.3(2) 1_555 1_555 1_555 no H(7) C(6) H(8) 105.7(2) 1_555 1_555 1_555 no C(6) C(7) C(8) 111.9(2) 1_555 1_555 1_555 yes C(6) C(7) C(20) 109.5(2) 1_555 1_555 1_555 yes C(6) C(7) H(30) 107.8(2) 1_555 1_555 1_555 no C(8) C(7) C(20) 111.8(2) 1_555 1_555 1_555 yes C(8) C(7) H(30) 107.9(2) 1_555 1_555 1_555 no C(20) C(7) H(30) 107.7(2) 1_555 1_555 1_555 no C(7) C(8) C(9) 105.3(2) 1_555 1_555 1_555 yes C(7) C(8) C(21) 111.6(2) 1_555 1_555 1_555 yes C(7) C(8) C(22) 109.4(2) 1_555 1_555 1_555 yes C(9) C(8) C(21) 112.6(2) 1_555 1_555 1_555 yes C(9) C(8) C(22) 109.1(2) 1_555 1_555 1_555 yes C(21) C(8) C(22) 108.9(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 116.4(2) 1_555 1_555 1_555 yes C(8) C(9) H(9) 106.2(2) 1_555 1_555 1_555 no C(8) C(9) H(10) 105.3(2) 1_555 1_555 1_555 no C(10) C(9) H(9) 106.8(2) 1_555 1_555 1_555 no C(10) C(9) H(10) 110.6(2) 1_555 1_555 1_555 no H(9) C(9) H(10) 111.5(2) 1_555 1_555 1_555 no C(1) C(10) C(9) 109.7(2) 1_555 1_555 1_555 yes C(1) C(10) C(11) 117.7(1) 1_555 1_555 1_555 yes C(1) C(10) H(11) 105.4(2) 1_555 1_555 1_555 no C(9) C(10) C(11) 110.0(1) 1_555 1_555 1_555 yes C(9) C(10) H(11) 111.0(2) 1_555 1_555 1_555 no C(11) C(10) H(11) 102.6(2) 1_555 1_555 1_555 no O C(11) C(5) 111.7(1) 1_555 1_555 1_555 yes O C(11) C(6) 108.1(1) 1_555 1_555 1_555 yes O C(11) C(10) 106.0(1) 1_555 1_555 1_555 yes C(5) C(11) C(6) 105.0(1) 1_555 1_555 1_555 yes C(5) C(11) C(10) 115.4(1) 1_555 1_555 1_555 yes C(6) C(11) C(10) 110.5(1) 1_555 1_555 1_555 yes C(1) C(12) H(13) 112.3(2) 1_555 1_555 1_555 no C(1) C(12) H(14) 112.3(2) 1_555 1_555 1_555 no C(1) C(12) H(15) 108.8(2) 1_555 1_555 1_555 no H(13) C(12) H(14) 107.5(2) 1_555 1_555 1_555 no H(13) C(12) H(15) 109.9(2) 1_555 1_555 1_555 no H(14) C(12) H(15) 105.9(2) 1_555 1_555 1_555 no S C(13) C(14) 119.0(2) 1_555 1_555 1_555 yes S C(13) C(18) 122.2(2) 1_555 1_555 1_555 yes C(14) C(13) C(18) 118.8(2) 1_555 1_555 1_555 yes C(13) C(14) C(15) 120.2(2) 1_555 1_555 1_555 yes C(13) C(14) H(16) 122.3(3) 1_555 1_555 1_555 no C(15) C(14) H(16) 117.3(3) 1_555 1_555 1_555 no C(14) C(15) C(16) 120.1(3) 1_555 1_555 1_555 yes C(14) C(15) H(17) 116.2(3) 1_555 1_555 1_555 no C(16) C(15) H(17) 123.5(3) 1_555 1_555 1_555 no C(15) C(16) C(17) 120.0(3) 1_555 1_555 1_555 yes C(15) C(16) H(18) 119.7(3) 1_555 1_555 1_555 no C(17) C(16) H(18) 120.3(3) 1_555 1_555 1_555 no C(16) C(17) C(18) 120.0(3) 1_555 1_555 1_555 yes C(16) C(17) H(19) 119.7(3) 1_555 1_555 1_555 no C(18) C(17) H(19) 120.3(3) 1_555 1_555 1_555 no C(13) C(18) C(17) 120.9(3) 1_555 1_555 1_555 yes C(13) C(18) H(20) 117.6(3) 1_555 1_555 1_555 no C(17) C(18) H(20) 121.5(3) 1_555 1_555 1_555 no C(5) C(19) H(21) 112.6(2) 1_555 1_555 1_555 no C(5) C(19) H(22) 113.3(2) 1_555 1_555 1_555 no C(5) C(19) H(23) 108.1(2) 1_555 1_555 1_555 no H(21) C(19) H(22) 106.5(2) 1_555 1_555 1_555 no H(21) C(19) H(23) 112.4(2) 1_555 1_555 1_555 no H(22) C(19) H(23) 103.7(2) 1_555 1_555 1_555 no N C(20) C(7) 177.9(2) 1_555 1_555 1_555 yes C(8) C(21) H(24) 109.9(3) 1_555 1_555 1_555 no C(8) C(21) H(25) 109.2(2) 1_555 1_555 1_555 no C(8) C(21) H(26) 109.5(2) 1_555 1_555 1_555 no H(24) C(21) H(25) 109.4(3) 1_555 1_555 1_555 no H(24) C(21) H(26) 109.9(3) 1_555 1_555 1_555 no H(25) C(21) H(26) 108.8(4) 1_555 1_555 1_555 no C(8) C(22) H(27) 110.3(3) 1_555 1_555 1_555 no C(8) C(22) H(28) 108.6(3) 1_555 1_555 1_555 no C(8) C(22) H(29) 110.2(3) 1_555 1_555 1_555 no H(27) C(22) H(28) 108.5(3) 1_555 1_555 1_555 no H(27) C(22) H(29) 110.6(4) 1_555 1_555 1_555 no H(28) C(22) H(29) 108.5(3) 1_555 1_555 1_555 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S C(4) C(3) C(2) -170.6(1) 1_555 1_555 1_555 1_555 yes S C(4) C(5) C(11) 90.4(2) 1_555 1_555 1_555 1_555 yes S C(4) C(5) C(19) -137.8(1) 1_555 1_555 1_555 1_555 yes S C(13) C(14) C(15) -179.2(2) 1_555 1_555 1_555 1_555 yes S C(13) C(18) C(17) 179.5(2) 1_555 1_555 1_555 1_555 yes F(1) C(1) C(2) C(3) 178.2(2) 1_555 1_555 1_555 1_555 yes F(1) C(1) C(10) C(9) -74.0(2) 1_555 1_555 1_555 1_555 yes F(1) C(1) C(10) C(11) 159.3(1) 1_555 1_555 1_555 1_555 yes O C(11) C(5) C(4) -39.3(2) 1_555 1_555 1_555 1_555 yes O C(11) C(5) C(19) -168.9(2) 1_555 1_555 1_555 1_555 yes O C(11) C(6) C(7) 63.8(2) 1_555 1_555 1_555 1_555 yes O C(11) C(10) C(1) 57.9(2) 1_555 1_555 1_555 1_555 yes O C(11) C(10) C(9) -68.7(2) 1_555 1_555 1_555 1_555 yes N C(20) C(7) C(6) -51(7) 1_555 1_555 1_555 1_555 yes N C(20) C(7) C(8) 73(7) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 89.7(2) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) 173.3(2) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(11) C(5) -66.4(2) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(11) C(6) 174.7(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 172.8(2) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(11) 46.0(2) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -44.0(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) -67.0(2) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(12) 63.9(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) S C(13) -179.7(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(11) -32.3(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(19) 99.5(2) 1_555 1_555 1_555 1_555 yes C(4) S C(13) C(14) -116.6(2) 1_555 1_555 1_555 1_555 yes C(4) S C(13) C(18) 63.9(2) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(11) C(6) -156.2(2) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(11) C(10) 81.9(2) 1_555 1_555 1_555 1_555 yes C(5) C(4) S C(13) 51.3(2) 1_555 1_555 1_555 1_555 yes C(5) C(11) C(6) C(7) -176.8(2) 1_555 1_555 1_555 1_555 yes C(5) C(11) C(10) C(9) 167.0(2) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -57.1(2) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(21) 65.3(2) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(22) -174.1(2) 1_555 1_555 1_555 1_555 yes C(6) C(11) C(5) C(19) 74.1(2) 1_555 1_555 1_555 1_555 yes C(6) C(11) C(10) C(9) 48.1(2) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(11) C(10) -51.8(2) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 58.4(2) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(11) 57.9(2) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -55.7(2) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(20) 179.6(2) 1_555 1_555 1_555 1_555 yes C(9) C(10) C(1) C(12) 44.2(2) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(21) -63.3(3) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(22) 175.7(2) 1_555 1_555 1_555 1_555 yes C(10) C(11) C(5) C(19) -47.7(2) 1_555 1_555 1_555 1_555 yes C(11) C(6) C(7) C(20) -177.4(2) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(1) C(12) -82.5(2) 1_555 1_555 1_555 1_555 yes C(13) C(14) C(15) C(16) -0.4(4) 1_555 1_555 1_555 1_555 yes C(13) C(18) C(17) C(16) -0.2(5) 1_555 1_555 1_555 1_555 yes C(14) C(13) C(18) C(17) 0.0(4) 1_555 1_555 1_555 1_555 yes C(14) C(15) C(16) C(17) 0.2(4) 1_555 1_555 1_555 1_555 yes C(15) C(14) C(13) C(18) 0.3(3) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) 0.1(5) 1_555 1_555 1_555 1_555 yes C(20) C(7) C(8) C(21) -58.0(2) 1_555 1_555 1_555 1_555 yes C(20) C(7) C(8) C(22) 62.6(3) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag S H(15) 3.2225(6) 1_555 2_545 ? S H(1) 3.491(1) 1_555 4_555 ? F(1) O 2.781(2) 1_555 4_455 ? F(1) H(16) 2.809(1) 1_555 4_455 ? F(1) N 2.922(3) 1_555 2_556 ? F(1) H(8) 3.019(2) 1_555 4_455 ? F(1) H(30) 3.303(2) 1_555 4_455 ? F(1) C(14) 3.598(3) 1_555 4_455 ? O H(2) 2.604(1) 1_555 4_555 ? O H(22) 3.026(1) 1_555 4_555 ? O C(2) 3.328(3) 1_555 4_555 ? O H(11) 3.384(2) 1_555 4_555 ? O H(1) 3.411(1) 1_555 4_555 ? O C(1) 3.586(3) 1_555 4_555 ? N H(10) 2.889(2) 1_555 2_546 ? N H(24) 3.118(3) 1_555 4_555 ? N H(17) 3.204(2) 1_555 3_656 ? N H(14) 3.255(2) 1_555 2_546 ? N H(16) 3.321(2) 1_555 3_656 ? N H(8) 3.394(3) 1_555 3_656 ? C(1) H(12) 2.972(2) 1_555 4_455 ? C(2) H(12) 2.940(2) 1_555 4_455 ? C(2) H(19) 3.509(2) 1_555 3_555 ? C(2) H(20) 3.573(2) 1_555 3_555 ? C(3) H(20) 3.250(2) 1_555 3_555 ? C(3) H(19) 3.558(2) 1_555 3_555 ? C(4) H(20) 3.355(2) 1_555 3_555 ? C(5) H(29) 3.585(2) 1_555 2_546 ? C(6) H(29) 3.053(2) 1_555 2_546 ? C(7) H(24) 3.534(2) 1_555 4_555 ? C(7) H(25) 3.594(2) 1_555 4_555 ? C(12) H(18) 3.221(2) 1_555 1_565 ? C(12) H(22) 3.391(3) 1_555 4_555 ? C(13) H(3) 3.503(2) 1_555 2_545 ? C(13) H(15) 3.584(2) 1_555 2_545 ? C(14) H(4) 3.251(2) 1_555 2_545 ? C(14) H(19) 3.437(3) 1_555 4_545 ? C(15) H(4) 2.989(3) 1_555 2_545 ? C(15) H(19) 3.316(3) 1_555 4_545 ? C(15) H(26) 3.342(3) 1_555 2_546 ? C(15) H(24) 3.449(3) 1_555 2_546 ? C(16) H(4) 3.141(3) 1_555 2_545 ? C(16) H(26) 3.175(3) 1_555 2_546 ? C(16) H(14) 3.560(3) 1_555 1_545 ? C(16) H(3) 3.565(3) 1_555 2_545 ? C(17) H(3) 3.341(3) 1_555 2_545 ? C(17) H(4) 3.356(4) 1_555 3_555 ? C(17) H(17) 3.482(3) 1_555 4_445 ? C(17) H(4) 3.520(3) 1_555 2_545 ? C(17) H(1) 3.567(3) 1_555 3_555 ? C(18) H(4) 3.259(3) 1_555 3_555 ? C(18) H(3) 3.302(3) 1_555 2_545 ? C(18) H(5) 3.474(3) 1_555 3_555 ? C(18) H(2) 3.593(3) 1_555 3_555 ? C(19) H(29) 3.296(2) 1_555 2_546 ? C(19) H(13) 3.394(3) 1_555 4_455 ? C(19) H(9) 3.430(3) 1_555 4_455 ? C(20) H(24) 3.020(2) 1_555 4_555 ? C(20) H(10) 3.380(2) 1_555 2_546 ? C(21) H(30) 3.365(3) 1_555 4_455 ? C(21) H(28) 3.555(4) 1_555 4_455 ? C(21) H(17) 3.585(3) 1_555 2_556 ? C(22) H(21) 3.158(3) 1_555 2_556 ? C(22) H(7) 3.253(3) 1_555 2_556 ? C(22) H(25) 3.542(4) 1_555 4_555 ? H(1) H(19) 2.9230(2) 1_555 3_555 ? H(1) H(12) 2.9339(5) 1_555 4_455 ? H(1) H(16) 3.5060(2) 1_555 4_455 ? H(1) H(20) 3.5789(2) 1_555 3_555 ? H(2) H(20) 3.1378(1) 1_555 3_555 ? H(2) H(13) 3.1490(9) 1_555 4_455 ? H(2) H(3) 3.421(1) 1_555 4_455 ? H(2) H(19) 3.5265(1) 1_555 3_555 ? H(3) H(20) 3.5993(7) 1_555 2_555 ? H(4) H(20) 2.6701(8) 1_555 3_555 ? H(4) H(19) 2.7851(7) 1_555 3_555 ? H(4) H(18) 3.5064(4) 1_555 2_555 ? H(5) H(20) 2.6631(5) 1_555 3_555 ? H(5) H(5) 3.3808(2) 1_555 3_555 ? H(7) H(28) 3.3184(3) 1_555 2_546 ? H(7) H(10) 3.5970(1) 1_555 2_546 ? H(8) H(29) 2.7879(4) 1_555 2_546 ? H(9) H(22) 2.8604(7) 1_555 4_555 ? H(9) H(21) 3.156(1) 1_555 4_555 ? H(11) H(30) 2.7985(8) 1_555 4_455 ? H(11) H(12) 3.1159(9) 1_555 4_455 ? H(12) H(22) 3.3120(2) 1_555 4_555 ? H(13) H(22) 2.651(1) 1_555 4_555 ? H(13) H(23) 3.250(1) 1_555 4_555 ? H(14) H(18) 2.6382(1) 1_555 1_565 ? H(14) H(22) 3.266(1) 1_555 4_555 ? H(14) H(23) 3.471(1) 1_555 4_555 ? H(15) H(18) 2.9587(2) 1_555 1_565 ? H(15) H(16) 3.419(1) 1_555 4_455 ? H(15) H(19) 3.4630(1) 1_555 1_565 ? H(16) H(19) 3.0874(7) 1_555 4_545 ? H(17) H(19) 2.9502(7) 1_555 4_545 ? H(17) H(27) 3.0199(5) 1_555 3_656 ? H(17) H(24) 3.1337(1) 1_555 2_546 ? H(17) H(26) 3.1900(4) 1_555 2_546 ? H(18) H(23) 3.5456(9) 1_555 4_545 ? H(21) H(29) 2.6886(3) 1_555 2_546 ? H(21) H(28) 3.3379(4) 1_555 4_455 ? H(23) H(29) 3.3592(4) 1_555 2_546 ? H(23) H(27) 3.3849(1) 1_555 2_546 ? H(24) H(30) 3.0255(9) 1_555 4_455 ? H(24) H(27) 3.474(1) 1_555 4_455 ? H(24) H(28) 3.5888(8) 1_555 4_455 ? H(25) H(30) 2.8285(9) 1_555 4_455 ? H(25) H(28) 2.861(1) 1_555 4_455 ? H(25) H(27) 3.415(1) 1_555 4_455 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_master_file_afc7*.xtl #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 5 12:45:39 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 364.97 _chemical_formula_analytical ? _chemical_formula_sum 'C21 H29 Cl O S ' _chemical_formula_moiety 'C21 H29 Cl O S ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 11.943(7) _cell_length_b 12.196(8) _cell_length_c 7.739(2) _cell_angle_alpha 104.76(3) _cell_angle_beta 99.19(3) _cell_angle_gamma 69.53(4) _cell_volume 1018.1(9) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 392.00 _exptl_absorpt_coefficient_mu 0.295 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.61 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -1 -2 1 -3 0 1 1 -1 2 _diffrn_reflns_number 4901 _reflns_number_total 4677 _reflns_number_gt 2536 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.012 _diffrn_reflns_av_sigmaI/netI 0.059 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01822 _diffrn_orient_matrix_UB_12 -0.02929 _diffrn_orient_matrix_UB_13 0.09833 _diffrn_orient_matrix_UB_21 0.05291 _diffrn_orient_matrix_UB_22 0.03975 _diffrn_orient_matrix_UB_23 0.08704 _diffrn_orient_matrix_UB_31 -0.07003 _diffrn_orient_matrix_UB_32 0.07479 _diffrn_orient_matrix_UB_33 0.02680 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'S' 'S' 0.125 0.123 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl 0.1328(2) -0.4716(2) -1.0710(4) 0.174(1) Uani 1.00 d . . . S S -0.5062(1) -0.1922(1) -1.0125(2) 0.0788(5) Uani 1.00 d . . . O O -0.1833(3) -0.1025(3) -1.2151(5) 0.080(1) Uani 1.00 d . . . C(1) C -0.3458(3) -0.2084(4) -0.9664(6) 0.052(1) Uani 1.00 d . . . C(2) C -0.3105(4) -0.1910(5) -1.1392(6) 0.066(2) Uani 1.00 d . . . C(3) C -0.1921(4) -0.1656(4) -1.1235(6) 0.053(1) Uani 1.00 d . . . C(4) C -0.0902(3) -0.2203(3) -0.9982(5) 0.045(1) Uani 1.00 d . . . C(5) C 0.0363(4) -0.2328(4) -1.0428(6) 0.055(1) Uani 1.00 d . . . C(6) C 0.1068(5) -0.2085(7) -0.8620(8) 0.098(2) Uani 1.00 d . . . C(7) C 0.0237(5) -0.1933(7) -0.7212(7) 0.096(2) Uani 1.00 d . . . C(8) C -0.1032(4) -0.1420(4) -0.8042(6) 0.062(1) Uani 1.00 d . . . C(9) C -0.1968(4) -0.1574(5) -0.7081(6) 0.067(2) Uani 1.00 d . . . C(10) C -0.3248(4) -0.1249(4) -0.7938(7) 0.063(2) Uani 1.00 d . . . C(11) C -0.3049(6) -0.2977(8) -1.2947(8) 0.115(3) Uani 1.00 d . . . C(12) C 0.0992(4) -0.3450(4) -1.1728(8) 0.071(2) Uani 1.00 d . . . C(13) C 0.0209(6) -0.3683(7) -1.3464(9) 0.115(3) Uani 1.00 d . . . C(14) C 0.2197(5) -0.3420(5) -1.2154(9) 0.087(2) Uani 1.00 d . . . C(15) C -0.1295(6) -0.0097(5) -0.8010(9) 0.099(2) Uani 1.00 d . . . C(16) C -0.5338(3) -0.2425(4) -0.8328(6) 0.055(1) Uani 1.00 d . . . C(17) C -0.4947(4) -0.3614(4) -0.8308(7) 0.074(2) Uani 1.00 d . . . C(18) C -0.5231(5) -0.4008(5) -0.6976(9) 0.090(2) Uani 1.00 d . . . C(19) C -0.5901(5) -0.3215(7) -0.5650(8) 0.090(2) Uani 1.00 d . . . C(20) C -0.6279(5) -0.2037(6) -0.5644(8) 0.086(2) Uani 1.00 d . . . C(21) C -0.6013(4) -0.1628(4) -0.6974(8) 0.073(2) Uani 1.00 d . . . H H -0.4452 -0.4192 -0.9240 0.08(2) Uiso 1.00 d . . . H H -0.4959 -0.4875 -0.7009 0.11(2) Uiso 1.00 d . . . H H -0.6101 -0.3501 -0.4708 0.11(2) Uiso 1.00 d . . . H H -0.6745 -0.1467 -0.4671 0.11(2) Uiso 1.00 d . . . H H -0.6295 -0.0768 -0.6956 0.10(2) Uiso 1.00 d . . . H H -0.3015 -0.2895 -0.9520 0.05(1) Uiso 1.00 d . . . H H -0.3742 -0.1242 -1.1761 0.08(1) Uiso 1.00 d . . . H H -0.0911 -0.2995 -0.9970 0.04(1) Uiso 1.00 d . . . H H 0.0243 -0.1664 -1.0994 0.07(1) Uiso 1.00 d . . . H H 0.1264 -0.1342 -0.8427 0.13(2) Uiso 1.00 d . . . H H 0.1815 -0.2709 -0.8521 0.10(2) Uiso 1.00 d . . . H H 0.0401 -0.1446 -0.6077 0.11(2) Uiso 1.00 d . . . H H 0.0354 -0.2724 -0.6965 0.08(2) Uiso 1.00 d . . . H H -0.1965 -0.1119 -0.5856 0.07(1) Uiso 1.00 d . . . H H -0.1723 -0.2412 -0.7002 0.05(1) Uiso 1.00 d . . . H H -0.3793 -0.1183 -0.7105 0.08(1) Uiso 1.00 d . . . H H -0.3447 -0.0459 -0.8194 0.08(2) Uiso 1.00 d . . . H H -0.3778 -0.3176 -1.3181 0.16(2) Uiso 1.00 d . . . H H -0.2418 -0.3699 -1.2653 0.16(2) Uiso 1.00 d . . . H H -0.2856 -0.2878 -1.4029 0.17(2) Uiso 1.00 d . . . H H -0.0015 -0.3011 -1.4087 0.16(2) Uiso 1.00 d . . . H H -0.0542 -0.3730 -1.3240 0.12(2) Uiso 1.00 d . . . H H 0.0592 -0.4384 -1.4299 0.13(2) Uiso 1.00 d . . . H H 0.2607 -0.4128 -1.2962 0.11(2) Uiso 1.00 d . . . H H 0.2721 -0.3360 -1.1048 0.11(2) Uiso 1.00 d . . . H H 0.2101 -0.2740 -1.2629 0.10(2) Uiso 1.00 d . . . H H -0.0728 0.0020 -0.8621 0.13(2) Uiso 1.00 d . . . H H -0.1299 0.0374 -0.6810 0.14(2) Uiso 1.00 d . . . H H -0.2084 0.0229 -0.8600 0.14(2) Uiso 1.00 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl 0.117(1) 0.082(1) 0.345(4) 0.0214(10) 0.108(2) 0.104(2) S 0.0426(6) 0.112(1) 0.097(1) -0.0203(6) -0.0052(6) 0.0617(9) O 0.068(2) 0.087(2) 0.097(3) -0.007(2) 0.017(2) 0.057(2) C(1) 0.040(2) 0.055(3) 0.064(3) -0.011(2) 0.003(2) 0.025(2) C(2) 0.040(2) 0.092(4) 0.067(3) -0.012(2) -0.002(2) 0.038(3) C(3) 0.047(2) 0.052(3) 0.060(3) -0.005(2) 0.013(2) 0.020(2) C(4) 0.043(2) 0.043(2) 0.052(3) -0.016(2) 0.007(2) 0.012(2) C(5) 0.045(2) 0.056(3) 0.071(3) -0.020(2) 0.007(2) 0.019(2) C(6) 0.058(3) 0.154(6) 0.088(4) -0.051(4) -0.005(3) 0.016(4) C(7) 0.080(4) 0.156(6) 0.059(4) -0.061(4) -0.015(3) 0.015(4) C(8) 0.065(3) 0.072(3) 0.053(3) -0.035(2) 0.006(2) 0.002(2) C(9) 0.079(3) 0.082(4) 0.047(3) -0.039(3) 0.011(2) 0.004(3) C(10) 0.060(3) 0.063(3) 0.067(3) -0.017(2) 0.023(2) 0.009(3) C(11) 0.093(5) 0.192(8) 0.064(4) -0.083(5) 0.004(3) -0.013(5) C(12) 0.051(2) 0.056(3) 0.109(4) -0.012(2) 0.024(3) 0.021(3) C(13) 0.082(4) 0.137(6) 0.092(5) -0.032(4) 0.039(4) -0.049(5) C(14) 0.056(3) 0.078(4) 0.130(5) -0.007(3) 0.042(4) 0.024(4) C(15) 0.119(5) 0.074(4) 0.117(5) -0.059(4) 0.054(4) -0.025(4) C(16) 0.037(2) 0.060(3) 0.072(3) -0.015(2) 0.001(2) 0.023(2) C(17) 0.069(3) 0.058(3) 0.092(4) -0.011(2) 0.026(3) 0.016(3) C(18) 0.081(4) 0.081(4) 0.121(5) -0.014(3) 0.017(4) 0.054(4) C(19) 0.059(3) 0.135(6) 0.090(4) -0.023(3) 0.010(3) 0.059(4) C(20) 0.059(3) 0.110(5) 0.078(4) -0.013(3) 0.022(3) 0.012(4) C(21) 0.054(3) 0.061(3) 0.100(4) -0.011(2) 0.021(3) 0.011(3) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method 'Zachariasen(1967) type 2 Gaussian isotropic' _refine_ls_extinction_coef 0.035(2) _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2536 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0637 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.446 _refine_ls_shift/su_max 0.0000 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.35 _refine_diff_density_max 0.24 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cl C 1.803(5) 1_555 1_555 yes S C(1) 1.842(4) 1_555 1_555 yes S C(15) 1.773(4) 1_555 1_555 yes O C(3) 1.210(5) 1_555 1_555 yes C C(5) 1.507(6) 1_555 1_555 yes C C(12) 1.533(8) 1_555 1_555 yes C C(13) 1.541(6) 1_555 1_555 yes C(1) C(2) 1.548(6) 1_555 1_555 yes C(1) C(10) 1.505(6) 1_555 1_555 yes C(1) H(6) 0.970(4) 1_555 1_555 no C(2) C(3) 1.531(6) 1_555 1_555 yes C(2) C(11) 1.521(8) 1_555 1_555 yes C(2) H(7) 0.970(4) 1_555 1_555 no C(3) C(4) 1.500(5) 1_555 1_555 yes C(4) C(5) 1.551(5) 1_555 1_555 yes C(4) C(8) 1.559(6) 1_555 1_555 yes C(4) H(8) 0.972(4) 1_555 1_555 no C(5) C(6) 1.531(7) 1_555 1_555 yes C(5) H(9) 0.973(4) 1_555 1_555 no C(6) C(7) 1.524(8) 1_555 1_555 yes C(6) H(10) 0.983(7) 1_555 1_555 no C(6) H(11) 0.956(7) 1_555 1_555 no C(7) C(8) 1.527(7) 1_555 1_555 yes C(7) H(12) 0.961(6) 1_555 1_555 no C(7) H(13) 0.988(8) 1_555 1_555 no C(8) C(9) 1.523(6) 1_555 1_555 yes C(8) C(14) 1.526(7) 1_555 1_555 yes C(9) C(10) 1.523(7) 1_555 1_555 yes C(9) H(14) 0.969(5) 1_555 1_555 no C(9) H(15) 0.975(5) 1_555 1_555 no C(10) H(16) 0.958(4) 1_555 1_555 no C(10) H(17) 0.972(5) 1_555 1_555 no C(11) H(18) 0.962(6) 1_555 1_555 no C(11) H(19) 0.989(9) 1_555 1_555 no C(11) H(20) 0.949(7) 1_555 1_555 no C(12) H(21) 0.992(9) 1_555 1_555 no C(12) H(22) 0.963(7) 1_555 1_555 no C(12) H(23) 0.947(6) 1_555 1_555 no C(13) H(24) 0.951(6) 1_555 1_555 no C(13) H(25) 0.979(7) 1_555 1_555 no C(13) H(26) 0.953(6) 1_555 1_555 no C(14) H(27) 0.953(6) 1_555 1_555 no C(14) H(28) 0.960(6) 1_555 1_555 no C(14) H(29) 0.974(8) 1_555 1_555 no C(15) C(16) 1.363(6) 1_555 1_555 yes C(15) C(20) 1.377(6) 1_555 1_555 yes C(16) C(17) 1.374(7) 1_555 1_555 yes C(16) H(1) 0.976(5) 1_555 1_555 no C(17) C(18) 1.358(8) 1_555 1_555 yes C(17) H(2) 0.986(6) 1_555 1_555 no C(18) C(19) 1.346(8) 1_555 1_555 yes C(18) H(3) 0.976(5) 1_555 1_555 no C(19) C(20) 1.373(7) 1_555 1_555 yes C(19) H(4) 0.978(6) 1_555 1_555 no C(20) H(5) 0.980(5) 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) S C(15) 102.1(2) 1_555 1_555 1_555 yes Cl C C(5) 108.8(4) 1_555 1_555 1_555 yes Cl C C(12) 106.7(4) 1_555 1_555 1_555 yes Cl C C(13) 106.9(3) 1_555 1_555 1_555 yes C(5) C C(12) 112.4(4) 1_555 1_555 1_555 yes C(5) C C(13) 111.4(4) 1_555 1_555 1_555 yes C(12) C C(13) 110.3(5) 1_555 1_555 1_555 yes S C(1) C(2) 104.2(3) 1_555 1_555 1_555 yes S C(1) C(10) 110.5(3) 1_555 1_555 1_555 yes S C(1) H(6) 109.0(3) 1_555 1_555 1_555 no C(2) C(1) C(10) 117.0(4) 1_555 1_555 1_555 yes C(2) C(1) H(6) 108.7(4) 1_555 1_555 1_555 no C(10) C(1) H(6) 107.3(4) 1_555 1_555 1_555 no C(1) C(2) C(3) 116.1(4) 1_555 1_555 1_555 yes C(1) C(2) C(11) 112.2(5) 1_555 1_555 1_555 yes C(1) C(2) H(7) 107.4(4) 1_555 1_555 1_555 no C(3) C(2) C(11) 107.1(4) 1_555 1_555 1_555 yes C(3) C(2) H(7) 108.1(4) 1_555 1_555 1_555 no C(11) C(2) H(7) 105.3(5) 1_555 1_555 1_555 no O C(3) C(2) 118.4(4) 1_555 1_555 1_555 yes O C(3) C(4) 121.9(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 119.6(3) 1_555 1_555 1_555 yes C(3) C(4) C(5) 115.4(3) 1_555 1_555 1_555 yes C(3) C(4) C(8) 110.7(3) 1_555 1_555 1_555 yes C(3) C(4) H(8) 108.9(4) 1_555 1_555 1_555 no C(5) C(4) C(8) 104.7(3) 1_555 1_555 1_555 yes C(5) C(4) H(8) 108.1(3) 1_555 1_555 1_555 no C(8) C(4) H(8) 108.8(3) 1_555 1_555 1_555 no C C(5) C(4) 116.8(4) 1_555 1_555 1_555 yes C C(5) C(6) 115.0(4) 1_555 1_555 1_555 yes C C(5) H(9) 106.2(4) 1_555 1_555 1_555 no C(4) C(5) C(6) 105.8(4) 1_555 1_555 1_555 yes C(4) C(5) H(9) 105.3(3) 1_555 1_555 1_555 no C(6) C(5) H(9) 107.0(4) 1_555 1_555 1_555 no C(5) C(6) C(7) 105.5(4) 1_555 1_555 1_555 yes C(5) C(6) H(10) 111.8(6) 1_555 1_555 1_555 no C(5) C(6) H(11) 112.4(6) 1_555 1_555 1_555 no C(7) C(6) H(10) 108.6(6) 1_555 1_555 1_555 no C(7) C(6) H(11) 112.4(6) 1_555 1_555 1_555 no H(10) C(6) H(11) 106.3(5) 1_555 1_555 1_555 no C(6) C(7) C(8) 105.5(5) 1_555 1_555 1_555 yes C(6) C(7) H(12) 113.2(5) 1_555 1_555 1_555 no C(6) C(7) H(13) 109.4(6) 1_555 1_555 1_555 no C(8) C(7) H(12) 113.0(6) 1_555 1_555 1_555 no C(8) C(7) H(13) 110.4(5) 1_555 1_555 1_555 no H(12) C(7) H(13) 105.5(6) 1_555 1_555 1_555 no C(4) C(8) C(7) 99.9(4) 1_555 1_555 1_555 yes C(4) C(8) C(9) 112.9(4) 1_555 1_555 1_555 yes C(4) C(8) C(14) 111.9(4) 1_555 1_555 1_555 yes C(7) C(8) C(9) 112.0(4) 1_555 1_555 1_555 yes C(7) C(8) C(14) 109.5(5) 1_555 1_555 1_555 yes C(9) C(8) C(14) 110.3(4) 1_555 1_555 1_555 yes C(8) C(9) C(10) 116.7(4) 1_555 1_555 1_555 yes C(8) C(9) H(14) 109.4(4) 1_555 1_555 1_555 no C(8) C(9) H(15) 108.1(4) 1_555 1_555 1_555 no C(10) C(9) H(14) 109.0(4) 1_555 1_555 1_555 no C(10) C(9) H(15) 107.2(4) 1_555 1_555 1_555 no H(14) C(9) H(15) 105.8(5) 1_555 1_555 1_555 no C(1) C(10) C(9) 115.4(4) 1_555 1_555 1_555 yes C(1) C(10) H(16) 109.2(4) 1_555 1_555 1_555 no C(1) C(10) H(17) 107.5(4) 1_555 1_555 1_555 no C(9) C(10) H(16) 110.2(4) 1_555 1_555 1_555 no C(9) C(10) H(17) 107.2(4) 1_555 1_555 1_555 no H(16) C(10) H(17) 107.0(4) 1_555 1_555 1_555 no C(2) C(11) H(18) 112.8(6) 1_555 1_555 1_555 no C(2) C(11) H(19) 109.7(5) 1_555 1_555 1_555 no C(2) C(11) H(20) 113.5(7) 1_555 1_555 1_555 no H(18) C(11) H(19) 105.4(8) 1_555 1_555 1_555 no H(18) C(11) H(20) 108.6(6) 1_555 1_555 1_555 no H(19) C(11) H(20) 106.4(7) 1_555 1_555 1_555 no C C(12) H(21) 110.8(6) 1_555 1_555 1_555 no C C(12) H(22) 112.2(6) 1_555 1_555 1_555 no C C(12) H(23) 113.5(6) 1_555 1_555 1_555 no H(21) C(12) H(22) 105.0(7) 1_555 1_555 1_555 no H(21) C(12) H(23) 106.2(7) 1_555 1_555 1_555 no H(22) C(12) H(23) 108.6(7) 1_555 1_555 1_555 no C C(13) H(24) 112.2(5) 1_555 1_555 1_555 no C C(13) H(25) 109.4(5) 1_555 1_555 1_555 no C C(13) H(26) 112.1(5) 1_555 1_555 1_555 no H(24) C(13) H(25) 107.0(5) 1_555 1_555 1_555 no H(24) C(13) H(26) 109.1(6) 1_555 1_555 1_555 no H(25) C(13) H(26) 106.8(6) 1_555 1_555 1_555 no C(8) C(14) H(27) 111.8(5) 1_555 1_555 1_555 no C(8) C(14) H(28) 112.0(6) 1_555 1_555 1_555 no C(8) C(14) H(29) 110.3(5) 1_555 1_555 1_555 no H(27) C(14) H(28) 108.4(6) 1_555 1_555 1_555 no H(27) C(14) H(29) 107.3(7) 1_555 1_555 1_555 no H(28) C(14) H(29) 106.7(6) 1_555 1_555 1_555 no S C(15) C(16) 120.8(4) 1_555 1_555 1_555 yes S C(15) C(20) 120.6(4) 1_555 1_555 1_555 yes C(16) C(15) C(20) 118.5(4) 1_555 1_555 1_555 yes C(15) C(16) C(17) 120.7(5) 1_555 1_555 1_555 yes C(15) C(16) H(1) 119.7(5) 1_555 1_555 1_555 no C(17) C(16) H(1) 119.6(5) 1_555 1_555 1_555 no C(16) C(17) C(18) 120.4(5) 1_555 1_555 1_555 yes C(16) C(17) H(2) 119.3(6) 1_555 1_555 1_555 no C(18) C(17) H(2) 120.4(6) 1_555 1_555 1_555 no C(17) C(18) C(19) 119.5(5) 1_555 1_555 1_555 yes C(17) C(18) H(3) 120.0(7) 1_555 1_555 1_555 no C(19) C(18) H(3) 120.6(7) 1_555 1_555 1_555 no C(18) C(19) C(20) 121.0(5) 1_555 1_555 1_555 yes C(18) C(19) H(4) 119.2(6) 1_555 1_555 1_555 no C(20) C(19) H(4) 119.8(7) 1_555 1_555 1_555 no C(15) C(20) C(19) 120.1(5) 1_555 1_555 1_555 yes C(15) C(20) H(5) 119.8(5) 1_555 1_555 1_555 no C(19) C(20) H(5) 120.2(5) 1_555 1_555 1_555 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cl C C(5) C(4) 66.4(5) 1_555 1_555 1_555 1_555 yes Cl C C(5) C(6) -58.5(5) 1_555 1_555 1_555 1_555 yes S C(1) C(2) C(3) -163.9(3) 1_555 1_555 1_555 1_555 yes S C(1) C(2) C(11) 72.4(4) 1_555 1_555 1_555 1_555 yes S C(1) C(10) C(9) -160.1(3) 1_555 1_555 1_555 1_555 yes S C(15) C(16) C(17) 175.6(4) 1_555 1_555 1_555 1_555 yes S C(15) C(20) C(19) -176.2(4) 1_555 1_555 1_555 1_555 yes O C(3) C(2) C(1) 148.0(4) 1_555 1_555 1_555 1_555 yes O C(3) C(2) C(11) -85.7(6) 1_555 1_555 1_555 1_555 yes O C(3) C(4) C(5) 22.4(6) 1_555 1_555 1_555 1_555 yes O C(3) C(4) C(8) -96.3(5) 1_555 1_555 1_555 1_555 yes C C(5) C(4) C(3) 86.9(5) 1_555 1_555 1_555 1_555 yes C C(5) C(4) C(8) -151.1(4) 1_555 1_555 1_555 1_555 yes C C(5) C(6) C(7) 125.9(5) 1_555 1_555 1_555 1_555 yes C(1) S C(15) C(16) 74.8(4) 1_555 1_555 1_555 1_555 yes C(1) S C(15) C(20) -109.1(4) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -32.8(6) 1_555 1_555 1_555 1_555 yes C(1) C(10) C(9) C(8) -70.1(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) S C(15) -168.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(10) C(9) 80.9(5) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -156.8(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(8) 84.5(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(10) -41.6(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -143.7(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(7) 164.0(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(9) -76.9(5) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(14) 48.2(5) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(11) 93.5(5) 1_555 1_555 1_555 1_555 yes C(4) C(5) C C(12) -51.6(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C C(13) -176.0(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -4.6(6) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(7) C(6) -42.5(6) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(10) 60.3(6) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(7) 39.0(4) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(9) 158.1(4) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(14) -76.8(5) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 30.0(7) 1_555 1_555 1_555 1_555 yes C(6) C(5) C C(12) -176.4(5) 1_555 1_555 1_555 1_555 yes C(6) C(5) C C(13) 59.2(6) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(4) C(8) -21.8(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -162.2(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(14) 75.1(6) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 172.1(5) 1_555 1_555 1_555 1_555 yes C(10) C(1) S C(15) 64.9(3) 1_555 1_555 1_555 1_555 yes C(10) C(1) C(2) C(11) -165.2(4) 1_555 1_555 1_555 1_555 yes C(10) C(9) C(8) C(14) -65.7(6) 1_555 1_555 1_555 1_555 yes C(15) C(16) C(17) C(18) 0.5(9) 1_555 1_555 1_555 1_555 yes C(15) C(20) C(19) C(18) 0.9(9) 1_555 1_555 1_555 1_555 yes C(16) C(15) C(20) C(19) 0.0(7) 1_555 1_555 1_555 1_555 yes C(16) C(17) C(18) C(19) 0.4(9) 1_555 1_555 1_555 1_555 yes C(17) C(16) C(15) C(20) -0.7(8) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) -1.1(9) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag Cl H(6) 2.937(2) 1_555 2_567 ? Cl H(8) 3.182(2) 1_555 2_567 ? Cl H(15) 3.403(2) 1_555 2_567 ? Cl H(19) 3.454(2) 1_555 2_567 ? Cl H(1) 3.498(3) 1_555 2_567 ? S H(17) 3.296(1) 1_555 2_657 ? S H(29) 3.449(2) 1_555 2_657 ? S H(25) 3.549(2) 1_555 1_655 ? O H(5) 2.667(3) 1_555 2_657 ? O H(14) 2.821(3) 1_555 1_556 ? O H(10) 3.100(4) 1_555 2_557 ? O C(20) 3.505(6) 1_555 2_657 ? O H(27) 3.589(4) 1_555 2_557 ? C(3) H(5) 3.463(4) 1_555 2_657 ? C(5) H(27) 3.267(4) 1_555 2_557 ? C(6) H(27) 3.580(7) 1_555 2_557 ? C(7) H(21) 3.129(6) 1_555 1_554 ? C(7) H(28) 3.510(6) 1_555 2_556 ? C(9) H(21) 3.371(5) 1_555 1_554 ? C(9) H(4) 3.474(5) 1_555 2_656 ? C(10) H(4) 3.410(5) 1_555 2_656 ? C(12) H(23) 2.905(7) 1_555 2_568 ? C(12) H(13) 3.263(8) 1_555 1_556 ? C(12) H(22) 3.458(6) 1_555 2_568 ? C(12) H(15) 3.588(8) 1_555 1_556 ? C(13) H(3) 3.015(5) 1_555 1_456 ? C(13) H(2) 3.290(5) 1_555 2_567 ? C(13) H(1) 3.477(6) 1_555 2_567 ? C(14) H(9) 3.136(6) 1_555 2_557 ? C(14) H(4) 3.136(6) 1_555 2_656 ? C(14) H(26) 3.178(6) 1_555 2_557 ? C(14) H(12) 3.461(7) 1_555 2_556 ? C(15) H(25) 3.189(4) 1_555 1_655 ? C(15) H(11) 3.513(4) 1_555 1_655 ? C(16) H(1) 3.098(5) 1_555 2_667 ? C(16) H(25) 3.193(6) 1_555 1_655 ? C(16) H(24) 3.388(5) 1_555 2_567 ? C(17) H(24) 3.162(6) 1_555 2_567 ? C(17) H(1) 3.239(7) 1_555 2_667 ? C(17) H(18) 3.279(7) 1_555 1_554 ? C(17) H(3) 3.381(5) 1_555 2_666 ? C(17) H(11) 3.478(6) 1_555 1_655 ? C(18) H(18) 2.928(6) 1_555 1_554 ? C(18) H(11) 3.216(6) 1_555 1_655 ? C(18) H(2) 3.287(6) 1_555 2_666 ? C(18) H(26) 3.409(5) 1_555 1_654 ? C(18) H(24) 3.534(5) 1_555 1_654 ? C(19) H(11) 3.093(6) 1_555 1_655 ? C(19) H(18) 3.334(6) 1_555 1_554 ? C(19) H(10) 3.338(6) 1_555 1_655 ? C(19) H(28) 3.432(5) 1_555 2_656 ? C(20) H(10) 3.193(5) 1_555 1_655 ? C(20) H(11) 3.239(5) 1_555 1_655 ? H(1) H(1) 2.6673(5) 1_555 2_667 ? H(1) H(2) 2.9053(1) 1_555 2_667 ? H(1) H(25) 3.0182(4) 1_555 2_567 ? H(1) H(24) 3.0630(5) 1_555 2_567 ? H(1) H(25) 3.347(2) 1_555 1_655 ? H(2) H(3) 2.5182(1) 1_555 2_666 ? H(2) H(24) 2.643(1) 1_555 2_567 ? H(2) H(25) 3.106(1) 1_555 2_567 ? H(2) H(18) 3.2708(6) 1_555 2_667 ? H(2) H(18) 3.5553(4) 1_555 1_554 ? H(3) H(24) 2.6091(7) 1_555 1_654 ? H(3) H(26) 2.6484(9) 1_555 1_654 ? H(3) H(18) 2.955(1) 1_555 1_554 ? H(3) H(25) 3.2995(4) 1_555 1_654 ? H(4) H(28) 2.540(1) 1_555 2_656 ? H(4) H(17) 2.8367(1) 1_555 2_656 ? H(4) H(29) 2.8899(3) 1_555 2_656 ? H(4) H(14) 2.9383(2) 1_555 2_656 ? H(4) H(26) 3.2030(5) 1_555 1_654 ? H(4) H(12) 3.402(2) 1_555 1_655 ? H(4) H(16) 3.4134(2) 1_555 2_656 ? H(4) H(10) 3.4488(7) 1_555 1_655 ? H(4) H(11) 3.4666(5) 1_555 1_655 ? H(5) H(7) 2.8856(1) 1_555 2_657 ? H(5) H(14) 3.1455(6) 1_555 2_656 ? H(5) H(10) 3.201(2) 1_555 1_655 ? H(5) H(16) 3.4361(1) 1_555 2_656 ? H(7) H(17) 3.271(2) 1_555 2_657 ? H(7) H(16) 3.5481(8) 1_555 2_657 ? H(9) H(28) 3.2232(5) 1_555 2_557 ? H(9) H(29) 3.346(1) 1_555 2_557 ? H(9) H(10) 3.5837(2) 1_555 2_557 ? H(10) H(27) 2.9858(1) 1_555 2_557 ? H(10) H(29) 3.3671(3) 1_555 2_557 ? H(12) H(28) 2.5642(3) 1_555 2_556 ? H(12) H(21) 2.9436(2) 1_555 1_554 ? H(12) H(12) 3.3602(1) 1_555 2_556 ? H(12) H(26) 3.4508(3) 1_555 1_554 ? H(13) H(23) 3.1583(1) 1_555 1_554 ? H(14) H(21) 3.0742(6) 1_555 1_554 ? H(14) H(20) 3.3700(4) 1_555 1_554 ? H(15) H(21) 2.8482(6) 1_555 1_554 ? H(15) H(20) 3.1069(5) 1_555 1_554 ? H(15) H(22) 3.5415(1) 1_555 1_554 ? H(16) H(20) 3.3516(1) 1_555 1_554 ? H(19) H(23) 3.3249(6) 1_555 2_568 ? H(20) H(23) 3.5692(7) 1_555 2_568 ? H(21) H(23) 3.3713(2) 1_555 2_568 ? H(22) H(23) 2.5977(1) 1_555 2_568 ? H(22) H(22) 3.5651(2) 1_555 2_568 ? H(26) H(28) 2.8294(1) 1_555 2_557 ? H(26) H(29) 2.9611(1) 1_555 2_557 ? H(26) H(27) 3.1145(2) 1_555 2_557 ? H(27) H(27) 2.9419(7) 1_555 2_557 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. Zachariasen, W. H. (1967). Acta Cryst. 23, 558-564. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_1_2-cis-Z-5-CN #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 5 15:51:15 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 245.36 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H23 N O ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 20.247(7) _cell_length_b 6.339(4) _cell_length_c 23.302(4) _cell_angle_alpha 90 _cell_angle_beta 105.64(2) _cell_angle_gamma 90 _cell_volume 2879(1) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.8 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21 ' _symmetry_Int_Tables_number 4 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072.00 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.76 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 0 1 2 -3 1 1 -1 1 3 _diffrn_reflns_number 6799 _reflns_number_total 6614 _reflns_number_gt 2526 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.039 _diffrn_reflns_av_sigmaI/netI 0.080 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.01540 _diffrn_orient_matrix_UB_12 0.01222 _diffrn_orient_matrix_UB_13 0.03719 _diffrn_orient_matrix_UB_21 0.04892 _diffrn_orient_matrix_UB_22 0.00596 _diffrn_orient_matrix_UB_23 0.02426 _diffrn_orient_matrix_UB_31 -0.00066 _diffrn_orient_matrix_UB_32 0.15716 _diffrn_orient_matrix_UB_33 -0.00381 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.1330(3) 0.456(1) -0.3045(2) 0.044(1) Uani 1.00 d . . . O(2) O -0.3847(3) -0.074(2) -0.4460(3) 0.055(2) Uani 1.00 d . . . O(3) O -0.3682(3) 0.459(2) -0.8057(2) 0.054(1) Uani 1.00 d . . . O(4) O -0.8841(3) -0.076(2) -0.9473(2) 0.058(2) Uani 1.00 d . . . N(1) N 0.0396(4) 0.841(2) -0.1629(4) 0.084(3) Uani 1.00 d . . . N(2) N -0.2916(3) -0.460(2) -0.5893(3) 0.068(2) Uani 1.00 d . . . N(3) N -0.4586(4) 0.841(2) -0.6647(4) 0.069(2) Uani 1.00 d . . . N(4) N -0.7905(4) -0.452(2) -1.0888(3) 0.073(2) Uani 1.00 d . . . C(1) C 0.1708(4) -0.002(2) -0.2946(3) 0.051(2) Uani 1.00 d . . . C(2) C 0.1663(3) 0.127(2) -0.2530(3) 0.041(2) Uani 1.00 d . . . C(3) C 0.1293(3) 0.334(2) -0.2624(3) 0.039(1) Uani 1.00 d . . . C(4) C 0.0851(4) 0.388(2) -0.2237(3) 0.049(2) Uani 1.00 d . . . C(5) C 0.0304(3) 0.554(2) -0.2458(3) 0.045(2) Uani 1.00 d . . . C(6) C -0.0469(3) 0.472(2) -0.2674(3) 0.038(1) Uani 1.00 d . . . C(7) C -0.0559(3) 0.359(2) -0.3269(3) 0.046(2) Uani 1.00 d . . . C(8) C -0.0139(3) 0.178(2) -0.3354(3) 0.047(2) Uani 1.00 d . . . C(9) C 0.0148(4) 0.157(2) -0.3787(3) 0.050(2) Uani 1.00 d . . . C(10) C 0.0610(4) -0.038(2) -0.3805(3) 0.058(2) Uani 1.00 d . . . C(11) C 0.1374(5) 0.022(2) -0.3647(3) 0.067(2) Uani 1.00 d . . . C(12) C 0.1969(3) 0.068(2) -0.1879(3) 0.047(2) Uani 1.00 d . . . C(13) C 0.0365(4) 0.710(2) -0.1988(3) 0.050(2) Uani 1.00 d . . . C(14) C -0.0950(3) 0.661(2) -0.2758(3) 0.041(1) Uani 1.00 d . . . C(15) C -0.0636(3) 0.323(2) -0.2217(3) 0.039(2) Uani 1.00 d . . . C(16) C 0.0130(4) 0.308(2) -0.4266(4) 0.063(2) Uani 1.00 d . . . C(17) C -0.4178(3) 0.389(2) -0.4509(3) 0.048(2) Uani 1.00 d . . . C(18) C -0.4160(3) 0.258(2) -0.4974(3) 0.040(1) Uani 1.00 d . . . C(19) C -0.3785(3) 0.049(2) -0.4833(3) 0.036(1) Uani 1.00 d . . . C(20) C -0.3363(4) -0.007(2) -0.5273(2) 0.036(2) Uani 1.00 d . . . C(21) C -0.2788(3) -0.172(2) -0.5064(3) 0.037(1) Uani 1.00 d . . . C(22) C -0.2044(3) -0.088(2) -0.4826(3) 0.043(1) Uani 1.00 d . . . C(23) C -0.1938(4) 0.017(2) -0.4208(3) 0.056(2) Uani 1.00 d . . . C(24) C -0.2376(3) 0.211(2) -0.4191(3) 0.055(2) Uani 1.00 d . . . C(25) C -0.2676(3) 0.228(2) -0.3713(3) 0.045(2) Uani 1.00 d . . . C(26) C -0.3098(4) 0.407(2) -0.3685(3) 0.046(2) Uani 1.00 d . . . C(27) C -0.3910(4) 0.353(2) -0.3862(4) 0.072(2) Uani 1.00 d . . . C(28) C -0.4468(3) 0.314(2) -0.5598(3) 0.053(2) Uani 1.00 d . . . C(29) C -0.2854(4) -0.337(2) -0.5518(3) 0.048(2) Uani 1.00 d . . . C(30) C -0.1570(3) -0.272(2) -0.4746(3) 0.050(2) Uani 1.00 d . . . C(31) C -0.1872(4) 0.064(2) -0.5300(3) 0.060(2) Uani 1.00 d . . . C(32) C -0.2653(5) 0.052(2) -0.3219(3) 0.076(3) Uani 1.00 d . . . C(33) C -0.3310(4) -0.004(2) -0.7985(3) 0.052(2) Uani 1.00 d . . . C(34) C -0.3325(3) 0.128(2) -0.7552(3) 0.044(1) Uani 1.00 d . . . C(35) C -0.3720(3) 0.337(2) -0.7662(3) 0.041(1) Uani 1.00 d . . . C(36) C -0.4124(3) 0.381(2) -0.7208(3) 0.039(1) Uani 1.00 d . . . C(37) C -0.4685(3) 0.557(2) -0.7446(3) 0.037(1) Uani 1.00 d . . . C(38) C -0.5446(3) 0.467(2) -0.7666(2) 0.029(1) Uani 1.00 d . . . C(39) C -0.5593(4) 0.362(2) -0.8275(3) 0.046(2) Uani 1.00 d . . . C(40) C -0.5134(3) 0.179(2) -0.8366(2) 0.036(1) Uani 1.00 d . . . C(41) C -0.4864(4) 0.153(2) -0.8770(3) 0.041(2) Uani 1.00 d . . . C(42) C -0.4394(4) -0.043(2) -0.8835(3) 0.051(2) Uani 1.00 d . . . C(43) C -0.3633(4) 0.017(2) -0.8620(3) 0.051(2) Uani 1.00 d . . . C(44) C -0.3029(4) 0.069(2) -0.6900(3) 0.052(2) Uani 1.00 d . . . C(45) C -0.4647(3) 0.712(2) -0.6994(3) 0.052(2) Uani 1.00 d . . . C(46) C -0.5982(4) 0.658(2) -0.7779(4) 0.062(2) Uani 1.00 d . . . C(47) C -0.5642(4) 0.328(2) -0.7194(3) 0.048(2) Uani 1.00 d . . . C(48) C -0.4924(5) 0.310(2) -0.9262(3) 0.068(2) Uani 1.00 d . . . C(49) C -0.9162(4) 0.387(2) -0.9531(3) 0.049(2) Uani 1.00 d . . . C(50) C -0.9139(3) 0.247(2) -0.9959(3) 0.042(2) Uani 1.00 d . . . C(51) C -0.8799(3) 0.044(2) -0.9845(3) 0.040(1) Uani 1.00 d . . . C(52) C -0.8359(3) -0.005(2) -1.0279(3) 0.037(1) Uani 1.00 d . . . C(53) C -0.7791(3) -0.167(2) -1.0042(2) 0.035(1) Uani 1.00 d . . . C(54) C -0.7039(4) -0.089(2) -0.9857(3) 0.048(1) Uani 1.00 d . . . C(55) C -0.6911(4) 0.022(2) -0.9214(3) 0.059(2) Uani 1.00 d . . . C(56) C -0.7362(3) 0.205(2) -0.9154(2) 0.040(1) Uani 1.00 d . . . C(57) C -0.7682(4) 0.228(2) -0.8695(3) 0.052(2) Uani 1.00 d . . . C(58) C -0.8078(4) 0.412(2) -0.8642(4) 0.063(2) Uani 1.00 d . . . C(59) C -0.8881(4) 0.364(2) -0.8863(3) 0.045(1) Uani 1.00 d . . . C(60) C -0.9496(5) 0.306(2) -1.0631(4) 0.062(2) Uani 1.00 d . . . C(61) C -0.7856(4) -0.336(2) -1.0526(3) 0.045(2) Uani 1.00 d . . . C(62) C -0.6557(4) -0.281(2) -0.9718(3) 0.053(2) Uani 1.00 d . . . C(63) C -0.6885(3) 0.053(2) -1.0303(4) 0.064(2) Uani 1.00 d . . . C(64) C -0.7594(5) 0.060(2) -0.8201(4) 0.077(3) Uani 1.00 d . . . H(1) H 0.1906 -0.1575 -0.2890 0.146(9) Uiso 1.00 calc . . . H(2) H 0.0667 0.2374 -0.2082 0.05(1) Uiso 1.00 calc . . . H(3) H 0.1185 0.4158 -0.1811 0.151(7) Uiso 1.00 calc . . . H(4) H 0.0426 0.6406 -0.2793 0.010(9) Uiso 1.00 calc . . . H(5) H -0.1005 0.2639 -0.3313 0.196(7) Uiso 1.00 calc . . . H(6) H -0.0489 0.4784 -0.3601 0.05(1) Uiso 1.00 calc . . . H(7) H -0.0034 0.0442 -0.2959 0.189(7) Uiso 1.00 calc . . . H(8) H 0.0506 -0.1828 -0.3854 0.08(1) Uiso 1.00 calc . . . H(9) H 0.0612 -0.0994 -0.4183 0.08(1) Uiso 1.00 calc . . . H(10) H 0.1531 0.1687 -0.3843 0.174(8) Uiso 1.00 calc . . . H(11) H 0.1659 -0.0974 -0.3860 0.08(1) Uiso 1.00 calc . . . H(12) H 0.2226 -0.0894 -0.1849 0.05(1) Uiso 1.00 calc . . . H(13) H 0.2289 0.2202 -0.1645 0.11(1) Uiso 1.00 calc . . . H(14) H 0.1626 0.0317 -0.1675 0.098(10) Uiso 1.00 calc . . . H(15) H -0.0349 0.1893 -0.2126 0.124(8) Uiso 1.00 calc . . . H(16) H -0.0625 0.3950 -0.1811 0.06(1) Uiso 1.00 calc . . . H(17) H -0.1108 0.2828 -0.2268 0.335(4) Uiso 1.00 calc . . . H(18) H -0.0950 0.7183 -0.2359 0.06(1) Uiso 1.00 calc . . . H(19) H -0.1514 0.5975 -0.2996 0.337(4) Uiso 1.00 calc . . . H(20) H -0.0856 0.7674 -0.3093 0.03(1) Uiso 1.00 calc . . . H(21) H -0.0447 0.3652 -0.4442 0.06(1) Uiso 1.00 calc . . . H(22) H 0.0327 0.2118 -0.4614 0.391(4) Uiso 1.00 calc . . . H(23) H 0.0452 0.4297 -0.4135 0.275(4) Uiso 1.00 calc . . . H(24) H -0.4372 0.5354 -0.4682 0.07(1) Uiso 1.00 calc . . . H(25) H -0.3173 0.1256 -0.5424 0.083(10) Uiso 1.00 calc . . . H(26) H -0.3722 -0.0486 -0.5653 0.03(1) Uiso 1.00 calc . . . H(27) H -0.2856 -0.2244 -0.4727 0.126(9) Uiso 1.00 calc . . . H(28) H -0.1501 0.1017 -0.4188 0.026(10) Uiso 1.00 calc . . . H(29) H -0.2007 -0.1115 -0.3878 0.08(1) Uiso 1.00 calc . . . H(30) H -0.2451 0.3271 -0.4504 0.05(1) Uiso 1.00 calc . . . H(31) H -0.3069 0.5411 -0.4000 0.04(1) Uiso 1.00 calc . . . H(32) H -0.2855 0.4739 -0.3181 0.09(1) Uiso 1.00 calc . . . H(33) H -0.3935 0.1899 -0.3640 0.113(9) Uiso 1.00 calc . . . H(34) H -0.4157 0.4552 -0.3629 0.027(10) Uiso 1.00 calc . . . H(35) H -0.5015 0.2567 -0.5787 0.09(1) Uiso 1.00 calc . . . H(36) H -0.4680 0.1549 -0.5902 0.307(6) Uiso 1.00 calc . . . H(37) H -0.4115 0.3445 -0.5861 0.120(9) Uiso 1.00 calc . . . H(38) H -0.2169 0.1928 -0.5381 0.108(9) Uiso 1.00 calc . . . H(39) H -0.2021 -0.0307 -0.5790 0.05(1) Uiso 1.00 calc . . . H(40) H -0.1347 0.0967 -0.5189 0.014(9) Uiso 1.00 calc . . . H(41) H -0.1553 -0.3757 -0.5118 0.08(1) Uiso 1.00 calc . . . H(42) H -0.0991 -0.2130 -0.4545 0.03(1) Uiso 1.00 calc . . . H(43) H -0.1639 -0.4004 -0.4452 0.282(5) Uiso 1.00 calc . . . H(44) H -0.2318 -0.1023 -0.3292 0.06(1) Uiso 1.00 calc . . . H(45) H -0.2504 0.1576 -0.2805 0.05(1) Uiso 1.00 calc . . . H(46) H -0.3006 -0.0634 -0.3336 0.287(5) Uiso 1.00 calc . . . H(47) H -0.2944 -0.1195 -0.7875 0.008(7) Uiso 1.00 calc . . . H(48) H -0.3786 0.4282 -0.6817 0.134(9) Uiso 1.00 calc . . . H(49) H -0.4327 0.2379 -0.7092 0.03(1) Uiso 1.00 calc . . . H(50) H -0.4572 0.6378 -0.7785 0.03(1) Uiso 1.00 calc . . . H(51) H -0.6107 0.3060 -0.8439 0.09(1) Uiso 1.00 calc . . . H(52) H -0.5617 0.4794 -0.8589 0.08(1) Uiso 1.00 calc . . . H(53) H -0.5028 0.0426 -0.7963 0.179(7) Uiso 1.00 calc . . . H(54) H -0.4486 -0.1607 -0.8499 0.018(9) Uiso 1.00 calc . . . H(55) H -0.4354 -0.0868 -0.9241 0.06(1) Uiso 1.00 calc . . . H(56) H -0.3562 0.1712 -0.8840 0.017(9) Uiso 1.00 calc . . . H(57) H -0.3361 -0.1014 -0.8862 0.128(9) Uiso 1.00 calc . . . H(58) H -0.2774 -0.0863 -0.6861 0.03(1) Uiso 1.00 calc . . . H(59) H -0.2814 0.2052 -0.6564 0.06(1) Uiso 1.00 calc . . . H(60) H -0.3358 0.0348 -0.6681 0.05(1) Uiso 1.00 calc . . . H(61) H -0.5346 0.1898 -0.7119 0.07(1) Uiso 1.00 calc . . . H(62) H -0.5625 0.3896 -0.6807 0.142(8) Uiso 1.00 calc . . . H(63) H -0.6168 0.2839 -0.7364 0.102(9) Uiso 1.00 calc . . . H(64) H -0.5944 0.7140 -0.7357 0.09(1) Uiso 1.00 calc . . . H(65) H -0.6494 0.6010 -0.7961 0.107(9) Uiso 1.00 calc . . . H(66) H -0.5865 0.7630 -0.8079 0.06(1) Uiso 1.00 calc . . . H(67) H -0.4750 0.4428 -0.9117 0.141(9) Uiso 1.00 calc . . . H(68) H -0.5397 0.3245 -0.9484 0.119(10) Uiso 1.00 calc . . . H(69) H -0.4676 0.2575 -0.9530 0.08(1) Uiso 1.00 calc . . . H(70) H -0.9378 0.5324 -0.9705 -0.005(6) Uiso 1.00 calc . . . H(71) H -0.8183 0.1295 -1.0428 0.07(1) Uiso 1.00 calc . . . H(72) H -0.8719 -0.0511 -1.0671 0.017(9) Uiso 1.00 calc . . . H(73) H -0.7843 -0.2275 -0.9739 0.05(1) Uiso 1.00 calc . . . H(74) H -0.6383 0.0490 -0.9041 0.008(8) Uiso 1.00 calc . . . H(75) H -0.6871 -0.1016 -0.8937 0.06(1) Uiso 1.00 calc . . . H(76) H -0.7391 0.3192 -0.9498 0.018(9) Uiso 1.00 calc . . . H(77) H -0.7859 0.4776 -0.8191 0.06(1) Uiso 1.00 calc . . . H(78) H -0.8058 0.5402 -0.9011 0.153(8) Uiso 1.00 calc . . . H(79) H -0.8939 0.1940 -0.8649 0.07(1) Uiso 1.00 calc . . . H(80) H -0.9051 0.4722 -0.8724 0.04(1) Uiso 1.00 calc . . . H(81) H -0.9949 0.3918 -1.0699 0.03(1) Uiso 1.00 calc . . . H(82) H -0.9723 0.1299 -1.0874 0.095(10) Uiso 1.00 calc . . . H(83) H -0.9115 0.3449 -1.0797 0.04(1) Uiso 1.00 calc . . . H(84) H -0.7132 0.1827 -1.0392 0.016(9) Uiso 1.00 calc . . . H(85) H -0.6886 -0.0335 -1.0717 0.092(10) Uiso 1.00 calc . . . H(86) H -0.6359 0.0972 -1.0190 0.09(1) Uiso 1.00 calc . . . H(87) H -0.6564 -0.3631 -1.0140 0.03(1) Uiso 1.00 calc . . . H(88) H -0.6018 -0.2323 -0.9534 0.03(1) Uiso 1.00 calc . . . H(89) H -0.6645 -0.3976 -0.9450 0.04(1) Uiso 1.00 calc . . . H(90) H -0.7086 -0.0520 -0.8165 0.329(5) Uiso 1.00 calc . . . H(91) H -0.7929 0.1363 -0.7931 0.198(7) Uiso 1.00 calc . . . H(92) H -0.8005 -0.0564 -0.8336 0.08(1) Uiso 1.00 calc . . . 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 O(1) 0.054(3) 0.037(2) 0.046(3) -0.006(2) 0.021(2) 0.000(2) O(2) 0.040(3) 0.057(3) 0.076(3) -0.001(2) 0.026(2) 0.016(2) O(3) 0.048(3) 0.055(3) 0.062(3) -0.014(2) 0.019(3) 0.000(2) O(4) 0.073(4) 0.047(3) 0.060(3) 0.010(3) 0.029(3) 0.022(2) N(1) 0.060(5) 0.100(6) 0.085(5) 0.009(4) 0.009(4) -0.061(4) N(2) 0.051(4) 0.046(3) 0.104(5) -0.007(3) 0.014(4) -0.037(3) N(3) 0.053(4) 0.039(3) 0.101(5) -0.006(3) -0.006(4) -0.023(3) N(4) 0.068(5) 0.084(5) 0.052(4) 0.018(4) -0.010(3) -0.032(3) C(1) 0.046(4) 0.075(4) 0.027(2) 0.020(3) 0.003(2) -0.001(2) C(2) 0.044(4) 0.047(3) 0.041(2) 0.005(3) 0.025(3) -0.001(2) C(3) 0.046(3) 0.030(2) 0.037(3) -0.020(2) 0.005(2) -0.004(2) C(4) 0.042(4) 0.063(4) 0.038(3) 0.004(3) 0.003(2) 0.002(3) C(5) 0.037(3) 0.067(4) 0.033(3) 0.012(2) 0.012(2) -0.010(2) C(6) 0.044(3) 0.027(2) 0.038(3) -0.002(2) 0.006(2) 0.010(2) C(7) 0.030(3) 0.061(4) 0.037(3) 0.005(3) -0.006(2) -0.005(3) C(8) 0.027(3) 0.039(3) 0.067(4) -0.015(2) 0.000(2) 0.003(3) C(9) 0.039(4) 0.040(3) 0.067(4) -0.017(2) 0.008(3) -0.002(3) C(10) 0.087(4) 0.041(3) 0.043(4) 0.002(3) 0.011(3) -0.029(3) C(11) 0.082(4) 0.095(6) 0.022(2) 0.005(5) 0.010(3) -0.010(3) C(12) 0.033(3) 0.049(3) 0.052(3) 0.006(3) -0.003(3) 0.017(3) C(13) 0.049(4) 0.058(4) 0.043(3) -0.001(3) 0.014(3) -0.002(2) C(14) 0.018(2) 0.044(3) 0.058(4) -0.007(2) 0.006(2) 0.008(3) C(15) 0.038(4) 0.048(3) 0.037(3) 0.011(3) 0.019(2) 0.000(2) C(16) 0.042(4) 0.076(5) 0.068(5) 0.019(4) 0.012(3) 0.027(4) C(17) 0.031(3) 0.061(4) 0.053(3) 0.003(3) 0.010(3) -0.012(3) C(18) 0.028(3) 0.044(3) 0.044(3) 0.003(2) 0.003(2) 0.001(2) C(19) 0.020(2) 0.039(2) 0.053(3) -0.013(2) 0.019(2) -0.015(2) C(20) 0.051(4) 0.036(3) 0.024(3) 0.017(2) 0.013(2) 0.012(2) C(21) 0.039(3) 0.022(2) 0.050(3) -0.004(2) 0.013(2) 0.005(2) C(22) 0.035(3) 0.055(3) 0.036(3) -0.002(2) 0.004(2) -0.004(2) C(23) 0.065(4) 0.054(4) 0.045(3) -0.017(3) 0.009(3) -0.017(3) C(24) 0.034(3) 0.083(4) 0.048(3) -0.009(3) 0.011(2) -0.041(3) C(25) 0.034(3) 0.060(3) 0.037(3) 0.001(3) 0.001(2) 0.015(3) C(26) 0.063(3) 0.047(3) 0.029(3) -0.007(3) 0.014(3) -0.002(3) C(27) 0.053(3) 0.118(8) 0.051(3) 0.023(5) 0.024(3) 0.006(5) C(28) 0.028(3) 0.087(5) 0.038(3) 0.022(3) -0.002(2) -0.005(3) C(29) 0.034(3) 0.045(3) 0.053(4) -0.005(3) -0.007(3) -0.006(2) C(30) 0.030(3) 0.076(4) 0.042(4) 0.016(3) 0.007(3) -0.001(3) C(31) 0.066(5) 0.067(5) 0.041(3) -0.021(4) 0.006(3) -0.003(3) C(32) 0.114(8) 0.074(5) 0.040(4) 0.019(5) 0.020(4) 0.024(3) C(33) 0.053(4) 0.047(4) 0.067(3) 0.015(3) 0.036(3) 0.009(3) C(34) 0.029(3) 0.046(3) 0.050(3) 0.003(2) -0.003(2) 0.012(2) C(35) 0.031(3) 0.051(3) 0.038(3) 0.011(2) 0.003(2) -0.011(2) C(36) 0.031(3) 0.049(3) 0.029(3) 0.018(2) -0.007(2) 0.001(2) C(37) 0.019(2) 0.033(2) 0.053(3) -0.006(2) -0.002(2) 0.009(2) C(38) 0.016(2) 0.042(3) 0.025(2) 0.003(2) -0.002(2) 0.000(2) C(39) 0.044(4) 0.060(4) 0.030(3) 0.009(3) 0.002(2) -0.009(3) C(40) 0.059(4) 0.024(2) 0.021(2) -0.014(2) 0.004(2) -0.005(2) C(41) 0.053(4) 0.039(3) 0.027(3) 0.010(2) 0.001(2) -0.011(2) C(42) 0.054(3) 0.063(4) 0.034(3) 0.027(3) 0.008(3) -0.011(3) C(43) 0.054(3) 0.055(4) 0.060(3) 0.019(3) 0.045(3) -0.006(3) C(44) 0.054(4) 0.064(4) 0.041(3) 0.000(4) 0.020(3) 0.004(3) C(45) 0.024(3) 0.023(2) 0.095(5) 0.004(2) -0.007(3) -0.018(3) C(46) 0.062(5) 0.051(4) 0.072(5) 0.042(3) 0.018(4) 0.007(4) C(47) 0.059(4) 0.032(3) 0.061(4) -0.005(3) 0.028(3) 0.013(3) C(48) 0.099(6) 0.087(5) 0.028(3) 0.013(5) 0.034(4) 0.014(3) C(49) 0.058(4) 0.033(3) 0.056(3) 0.009(3) 0.012(3) 0.006(2) C(50) 0.039(4) 0.048(3) 0.046(3) -0.002(3) 0.021(3) 0.002(2) C(51) 0.035(3) 0.048(3) 0.031(3) 0.001(2) -0.003(2) 0.007(2) C(52) 0.024(3) 0.043(3) 0.042(3) -0.011(2) 0.005(2) -0.020(2) C(53) 0.047(3) 0.038(3) 0.016(2) 0.001(2) 0.002(2) -0.001(2) C(54) 0.042(3) 0.049(3) 0.050(3) 0.005(2) 0.009(3) -0.023(2) C(55) 0.037(3) 0.078(5) 0.048(3) 0.014(3) -0.014(3) -0.028(4) C(56) 0.039(3) 0.060(3) 0.018(2) -0.002(3) 0.000(2) 0.000(3) C(57) 0.044(4) 0.086(4) 0.028(3) -0.012(3) 0.015(2) -0.024(2) C(58) 0.048(3) 0.071(4) 0.071(5) -0.015(3) 0.018(3) -0.005(4) C(59) 0.046(3) 0.037(3) 0.051(3) 0.003(3) 0.012(3) -0.007(3) C(60) 0.064(5) 0.072(5) 0.046(3) 0.016(4) 0.009(3) 0.008(4) C(61) 0.047(4) 0.039(3) 0.046(4) 0.006(3) 0.008(3) -0.006(2) C(62) 0.063(4) 0.042(3) 0.039(3) 0.005(3) -0.011(3) -0.007(3) C(63) 0.026(3) 0.066(4) 0.102(6) 0.004(3) 0.021(3) 0.031(4) C(64) 0.068(6) 0.089(7) 0.082(6) 0.011(5) 0.032(5) 0.034(5) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3821 _refine_ls_number_parameters 741 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0498 _refine_ls_wR_factor_gt 0.0430 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.110 _refine_ls_shift/su_max 2.8850 _refine_ls_shift/su_mean 0.3630 _refine_diff_density_min -0.15 _refine_diff_density_max 0.14 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.27(1) 1_555 1_555 yes O(2) C(19) 1.20(1) 1_555 1_555 yes O(3) C(35) 1.22(1) 1_555 1_555 yes O(4) C(51) 1.17(1) 1_555 1_555 yes N(1) C(13) 1.16(1) 1_555 1_555 yes N(2) C(29) 1.15(1) 1_555 1_555 yes N(3) C(45) 1.13(1) 1_555 1_555 yes N(4) C(61) 1.10(1) 1_555 1_555 yes C(1) C(2) 1.29(1) 1_555 1_555 yes C(1) C(11) 1.60(1) 1_555 1_555 yes C(1) H(1) 1.06(2) 1_555 1_555 no C(2) C(3) 1.50(1) 1_555 1_555 yes C(2) C(12) 1.52(1) 1_555 1_555 yes C(3) C(4) 1.47(1) 1_555 1_555 yes C(4) C(5) 1.51(1) 1_555 1_555 yes C(4) H(2) 1.12(1) 1_555 1_555 no C(4) H(3) 1.053(10) 1_555 1_555 no C(5) C(6) 1.60(1) 1_555 1_555 yes C(5) C(13) 1.46(1) 1_555 1_555 yes C(5) H(4) 1.04(1) 1_555 1_555 no C(6) C(7) 1.53(1) 1_555 1_555 yes C(6) C(14) 1.52(1) 1_555 1_555 yes C(6) C(15) 1.53(1) 1_555 1_555 yes C(7) C(8) 1.48(1) 1_555 1_555 yes C(7) H(5) 1.07(1) 1_555 1_555 no C(7) H(6) 1.12(1) 1_555 1_555 no C(8) C(9) 1.30(1) 1_555 1_555 yes C(8) H(7) 1.22(1) 1_555 1_555 no C(9) C(10) 1.56(1) 1_555 1_555 yes C(9) C(16) 1.46(1) 1_555 1_555 yes C(10) C(11) 1.54(2) 1_555 1_555 yes C(10) H(8) 0.94(2) 1_555 1_555 no C(10) H(9) 0.963(10) 1_555 1_555 no C(11) H(10) 1.12(2) 1_555 1_555 no C(11) H(11) 1.14(1) 1_555 1_555 no C(12) H(12) 1.12(1) 1_555 1_555 no C(12) H(13) 1.21(1) 1_555 1_555 no C(12) H(14) 0.97(1) 1_555 1_555 no C(14) H(18) 1.00(1) 1_555 1_555 no C(14) H(19) 1.196(9) 1_555 1_555 no C(14) H(20) 1.09(1) 1_555 1_555 no C(15) H(15) 1.01(1) 1_555 1_555 no C(15) H(16) 1.048(10) 1_555 1_555 no C(15) H(17) 0.96(1) 1_555 1_555 no C(16) H(21) 1.19(1) 1_555 1_555 no C(16) H(22) 1.17(1) 1_555 1_555 no C(16) H(23) 1.00(2) 1_555 1_555 no C(17) C(18) 1.37(1) 1_555 1_555 yes C(17) C(27) 1.48(1) 1_555 1_555 yes C(17) H(24) 1.05(2) 1_555 1_555 no C(18) C(19) 1.51(1) 1_555 1_555 yes C(18) C(28) 1.46(1) 1_555 1_555 yes C(19) C(20) 1.54(1) 1_555 1_555 yes C(20) C(21) 1.54(1) 1_555 1_555 yes C(20) H(25) 1.02(1) 1_555 1_555 no C(20) H(26) 1.018(10) 1_555 1_555 no C(21) C(22) 1.55(1) 1_555 1_555 yes C(21) C(29) 1.47(1) 1_555 1_555 yes C(21) H(27) 0.897(10) 1_555 1_555 no C(22) C(23) 1.55(1) 1_555 1_555 yes C(22) C(30) 1.49(1) 1_555 1_555 yes C(22) C(31) 1.57(1) 1_555 1_555 yes C(23) C(24) 1.52(2) 1_555 1_555 yes C(23) H(28) 1.02(1) 1_555 1_555 no C(23) H(29) 1.16(1) 1_555 1_555 no C(24) C(25) 1.41(1) 1_555 1_555 yes C(24) H(30) 1.02(1) 1_555 1_555 no C(25) C(26) 1.43(1) 1_555 1_555 yes C(25) C(32) 1.60(1) 1_555 1_555 yes C(26) C(27) 1.62(2) 1_555 1_555 yes C(26) H(31) 1.13(1) 1_555 1_555 no C(26) H(32) 1.22(1) 1_555 1_555 no C(27) H(33) 1.16(2) 1_555 1_555 no C(27) H(34) 1.05(1) 1_555 1_555 no C(28) H(35) 1.14(1) 1_555 1_555 no C(28) H(36) 1.24(2) 1_555 1_555 no C(28) H(37) 1.08(1) 1_555 1_555 no C(30) H(41) 1.10(1) 1_555 1_555 no C(30) H(42) 1.20(1) 1_555 1_555 no C(30) H(43) 1.10(2) 1_555 1_555 no C(31) H(38) 1.00(2) 1_555 1_555 no C(31) H(39) 1.25(1) 1_555 1_555 no C(31) H(40) 1.04(1) 1_555 1_555 no C(32) H(44) 1.23(2) 1_555 1_555 no C(32) H(45) 1.14(2) 1_555 1_555 no C(32) H(46) 1.01(2) 1_555 1_555 no C(33) C(34) 1.32(1) 1_555 1_555 yes C(33) C(43) 1.45(1) 1_555 1_555 yes C(33) H(47) 1.02(1) 1_555 1_555 no C(34) C(35) 1.53(1) 1_555 1_555 yes C(34) C(44) 1.52(1) 1_555 1_555 yes C(35) C(36) 1.53(1) 1_555 1_555 yes C(36) C(37) 1.58(1) 1_555 1_555 yes C(36) H(48) 1.025(9) 1_555 1_555 no C(36) H(49) 1.06(1) 1_555 1_555 no C(37) C(38) 1.59(1) 1_555 1_555 yes C(37) C(45) 1.43(1) 1_555 1_555 yes C(37) H(50) 1.02(1) 1_555 1_555 no C(38) C(39) 1.52(1) 1_555 1_555 yes C(38) C(46) 1.60(1) 1_555 1_555 yes C(38) C(47) 1.54(1) 1_555 1_555 yes C(39) C(40) 1.54(1) 1_555 1_555 yes C(39) H(51) 1.07(1) 1_555 1_555 no C(39) H(52) 1.04(1) 1_555 1_555 no C(40) C(41) 1.22(1) 1_555 1_555 yes C(40) H(53) 1.25(1) 1_555 1_555 no C(41) C(42) 1.60(1) 1_555 1_555 yes C(41) C(48) 1.50(1) 1_555 1_555 yes C(42) C(43) 1.53(2) 1_555 1_555 yes C(42) H(54) 1.13(1) 1_555 1_555 no C(42) H(55) 1.009(9) 1_555 1_555 no C(43) H(56) 1.13(1) 1_555 1_555 no C(43) H(57) 1.16(1) 1_555 1_555 no C(44) H(58) 1.11(2) 1_555 1_555 no C(44) H(59) 1.17(1) 1_555 1_555 no C(44) H(60) 0.97(1) 1_555 1_555 no C(46) H(64) 1.03(1) 1_555 1_555 no C(46) H(65) 1.07(1) 1_555 1_555 no C(46) H(66) 1.04(1) 1_555 1_555 no C(47) H(61) 1.05(1) 1_555 1_555 no C(47) H(62) 0.97(1) 1_555 1_555 no C(47) H(63) 1.07(1) 1_555 1_555 no C(48) H(67) 0.94(2) 1_555 1_555 no C(48) H(68) 0.96(1) 1_555 1_555 no C(48) H(69) 0.96(1) 1_555 1_555 no C(49) C(50) 1.34(1) 1_555 1_555 yes C(49) C(59) 1.51(1) 1_555 1_555 yes C(49) H(70) 1.05(1) 1_555 1_555 no C(50) C(51) 1.45(1) 1_555 1_555 yes C(50) C(60) 1.58(1) 1_555 1_555 yes C(51) C(52) 1.55(1) 1_555 1_555 yes C(52) C(53) 1.53(1) 1_555 1_555 yes C(52) H(71) 1.02(1) 1_555 1_555 no C(52) H(72) 1.045(9) 1_555 1_555 no C(53) C(54) 1.55(1) 1_555 1_555 yes C(53) C(61) 1.53(1) 1_555 1_555 yes C(53) H(73) 0.832(10) 1_555 1_555 no C(54) C(55) 1.61(1) 1_555 1_555 yes C(54) C(62) 1.54(1) 1_555 1_555 yes C(54) C(63) 1.47(1) 1_555 1_555 yes C(55) C(56) 1.51(1) 1_555 1_555 yes C(55) H(74) 1.05(1) 1_555 1_555 no C(55) H(75) 1.00(2) 1_555 1_555 no C(56) C(57) 1.40(1) 1_555 1_555 yes C(56) H(76) 1.07(1) 1_555 1_555 no C(57) C(58) 1.44(2) 1_555 1_555 yes C(57) C(64) 1.54(2) 1_555 1_555 yes C(58) C(59) 1.60(1) 1_555 1_555 yes C(58) H(77) 1.11(1) 1_555 1_555 no C(58) H(78) 1.19(2) 1_555 1_555 no C(59) H(79) 1.21(1) 1_555 1_555 no C(59) H(80) 0.87(1) 1_555 1_555 no C(60) H(81) 1.04(1) 1_555 1_555 no C(60) H(82) 1.28(2) 1_555 1_555 no C(60) H(83) 0.98(1) 1_555 1_555 no C(62) H(87) 1.11(1) 1_555 1_555 no C(62) H(88) 1.11(1) 1_555 1_555 no C(62) H(89) 1.01(1) 1_555 1_555 no C(63) H(84) 0.96(2) 1_555 1_555 no C(63) H(85) 1.11(1) 1_555 1_555 no C(63) H(86) 1.06(1) 1_555 1_555 no C(64) H(90) 1.24(2) 1_555 1_555 no C(64) H(91) 1.15(2) 1_555 1_555 no C(64) H(92) 1.09(2) 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(2) C(1) C(11) 127(1) 1_555 1_555 1_555 yes C(2) C(1) H(1) 126.8(9) 1_555 1_555 1_555 no C(11) C(1) H(1) 104.7(9) 1_555 1_555 1_555 no C(1) C(2) C(3) 125.3(9) 1_555 1_555 1_555 yes C(1) C(2) C(12) 119.9(9) 1_555 1_555 1_555 yes C(3) C(2) C(12) 114.6(8) 1_555 1_555 1_555 yes O(1) C(3) C(2) 121.2(9) 1_555 1_555 1_555 yes O(1) C(3) C(4) 120.1(9) 1_555 1_555 1_555 yes C(2) C(3) C(4) 118.6(8) 1_555 1_555 1_555 yes C(3) C(4) C(5) 117.6(8) 1_555 1_555 1_555 yes C(3) C(4) H(2) 107.7(9) 1_555 1_555 1_555 no C(3) C(4) H(3) 105.8(9) 1_555 1_555 1_555 no C(5) C(4) H(2) 115.2(9) 1_555 1_555 1_555 no C(5) C(4) H(3) 115(1) 1_555 1_555 1_555 no H(2) C(4) H(3) 91.3(9) 1_555 1_555 1_555 no C(4) C(5) C(6) 116.7(9) 1_555 1_555 1_555 yes C(4) C(5) C(13) 108.1(8) 1_555 1_555 1_555 yes C(4) C(5) H(4) 108.9(9) 1_555 1_555 1_555 no C(6) C(5) C(13) 109.5(8) 1_555 1_555 1_555 yes C(6) C(5) H(4) 110.3(8) 1_555 1_555 1_555 no C(13) C(5) H(4) 102(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 107.7(8) 1_555 1_555 1_555 yes C(5) C(6) C(14) 109.0(7) 1_555 1_555 1_555 yes C(5) C(6) C(15) 111.2(7) 1_555 1_555 1_555 yes C(7) C(6) C(14) 109.7(7) 1_555 1_555 1_555 yes C(7) C(6) C(15) 110.2(8) 1_555 1_555 1_555 yes C(14) C(6) C(15) 108.9(8) 1_555 1_555 1_555 yes C(6) C(7) C(8) 123.8(8) 1_555 1_555 1_555 yes C(6) C(7) H(5) 104.1(9) 1_555 1_555 1_555 no C(6) C(7) H(6) 107.7(10) 1_555 1_555 1_555 no C(8) C(7) H(5) 92.9(10) 1_555 1_555 1_555 no C(8) C(7) H(6) 104.5(10) 1_555 1_555 1_555 no H(5) C(7) H(6) 125.2(8) 1_555 1_555 1_555 no C(7) C(8) C(9) 125(1) 1_555 1_555 1_555 yes C(7) C(8) H(7) 115.3(10) 1_555 1_555 1_555 no C(9) C(8) H(7) 119(1) 1_555 1_555 1_555 no C(8) C(9) C(10) 119.8(10) 1_555 1_555 1_555 yes C(8) C(9) C(16) 127(1) 1_555 1_555 1_555 yes C(10) C(9) C(16) 113.0(9) 1_555 1_555 1_555 yes C(9) C(10) C(11) 111.6(9) 1_555 1_555 1_555 yes C(9) C(10) H(8) 131(1) 1_555 1_555 1_555 no C(9) C(10) H(9) 119(1) 1_555 1_555 1_555 no C(11) C(10) H(8) 116(1) 1_555 1_555 1_555 no C(11) C(10) H(9) 93.8(10) 1_555 1_555 1_555 no H(8) C(10) H(9) 63.5(8) 1_555 1_555 1_555 no C(1) C(11) C(10) 110.0(9) 1_555 1_555 1_555 yes C(1) C(11) H(10) 113(1) 1_555 1_555 1_555 no C(1) C(11) H(11) 105.0(10) 1_555 1_555 1_555 no C(10) C(11) H(10) 119(1) 1_555 1_555 1_555 no C(10) C(11) H(11) 109(1) 1_555 1_555 1_555 no H(10) C(11) H(11) 98.1(9) 1_555 1_555 1_555 no C(2) C(12) H(12) 109.9(9) 1_555 1_555 1_555 no C(2) C(12) H(13) 106.0(8) 1_555 1_555 1_555 no C(2) C(12) H(14) 113.1(8) 1_555 1_555 1_555 no H(12) C(12) H(13) 120.1(8) 1_555 1_555 1_555 no H(12) C(12) H(14) 98(1) 1_555 1_555 1_555 no H(13) C(12) H(14) 109(1) 1_555 1_555 1_555 no N(1) C(13) C(5) 177(1) 1_555 1_555 1_555 yes C(6) C(14) H(18) 109.1(9) 1_555 1_555 1_555 no C(6) C(14) H(19) 107.1(9) 1_555 1_555 1_555 no C(6) C(14) H(20) 110.6(9) 1_555 1_555 1_555 no H(18) C(14) H(19) 108.3(8) 1_555 1_555 1_555 no H(18) C(14) H(20) 119(1) 1_555 1_555 1_555 no H(19) C(14) H(20) 101.9(7) 1_555 1_555 1_555 no C(6) C(15) H(15) 116.3(8) 1_555 1_555 1_555 no C(6) C(15) H(16) 113(1) 1_555 1_555 1_555 no C(6) C(15) H(17) 118.2(10) 1_555 1_555 1_555 no H(15) C(15) H(16) 107.7(9) 1_555 1_555 1_555 no H(15) C(15) H(17) 107(1) 1_555 1_555 1_555 no H(16) C(15) H(17) 90.2(7) 1_555 1_555 1_555 no C(9) C(16) H(21) 106.4(9) 1_555 1_555 1_555 no C(9) C(16) H(22) 104(1) 1_555 1_555 1_555 no C(9) C(16) H(23) 112(1) 1_555 1_555 1_555 no H(21) C(16) H(22) 114(1) 1_555 1_555 1_555 no H(21) C(16) H(23) 111(1) 1_555 1_555 1_555 no H(22) C(16) H(23) 107.3(10) 1_555 1_555 1_555 no C(18) C(17) C(27) 129(1) 1_555 1_555 1_555 yes C(18) C(17) H(24) 108.7(10) 1_555 1_555 1_555 no C(27) C(17) H(24) 121(1) 1_555 1_555 1_555 no C(17) C(18) C(19) 118.4(8) 1_555 1_555 1_555 yes C(17) C(18) C(28) 122.7(9) 1_555 1_555 1_555 yes C(19) C(18) C(28) 118.9(9) 1_555 1_555 1_555 yes O(2) C(19) C(18) 125.4(8) 1_555 1_555 1_555 yes O(2) C(19) C(20) 121.1(8) 1_555 1_555 1_555 yes C(18) C(19) C(20) 113.1(8) 1_555 1_555 1_555 yes C(19) C(20) C(21) 116.9(7) 1_555 1_555 1_555 yes C(19) C(20) H(25) 111.5(8) 1_555 1_555 1_555 no C(19) C(20) H(26) 104.1(8) 1_555 1_555 1_555 no C(21) C(20) H(25) 110.0(9) 1_555 1_555 1_555 no C(21) C(20) H(26) 113.4(9) 1_555 1_555 1_555 no H(25) C(20) H(26) 99.4(8) 1_555 1_555 1_555 no C(20) C(21) C(22) 117.2(7) 1_555 1_555 1_555 yes C(20) C(21) C(29) 110.0(8) 1_555 1_555 1_555 yes C(20) C(21) H(27) 104.4(10) 1_555 1_555 1_555 no C(22) C(21) C(29) 113.1(8) 1_555 1_555 1_555 yes C(22) C(21) H(27) 100.2(9) 1_555 1_555 1_555 no C(29) C(21) H(27) 111(1) 1_555 1_555 1_555 no C(21) C(22) C(23) 110.9(8) 1_555 1_555 1_555 yes C(21) C(22) C(30) 107.8(8) 1_555 1_555 1_555 yes C(21) C(22) C(31) 109.7(8) 1_555 1_555 1_555 yes C(23) C(22) C(30) 107.3(8) 1_555 1_555 1_555 yes C(23) C(22) C(31) 112.8(9) 1_555 1_555 1_555 yes C(30) C(22) C(31) 108.1(9) 1_555 1_555 1_555 yes C(22) C(23) C(24) 115.9(9) 1_555 1_555 1_555 yes C(22) C(23) H(28) 99.7(9) 1_555 1_555 1_555 no C(22) C(23) H(29) 107.7(9) 1_555 1_555 1_555 no C(24) C(23) H(28) 94(1) 1_555 1_555 1_555 no C(24) C(23) H(29) 112.1(10) 1_555 1_555 1_555 no H(28) C(23) H(29) 126(1) 1_555 1_555 1_555 no C(23) C(24) C(25) 117(1) 1_555 1_555 1_555 yes C(23) C(24) H(30) 122.6(9) 1_555 1_555 1_555 no C(25) C(24) H(30) 119(1) 1_555 1_555 1_555 no C(24) C(25) C(26) 119.3(9) 1_555 1_555 1_555 yes C(24) C(25) C(32) 125(1) 1_555 1_555 1_555 yes C(26) C(25) C(32) 114.9(9) 1_555 1_555 1_555 yes C(25) C(26) C(27) 113.4(10) 1_555 1_555 1_555 yes C(25) C(26) H(31) 115.2(9) 1_555 1_555 1_555 no C(25) C(26) H(32) 103.2(9) 1_555 1_555 1_555 no C(27) C(26) H(31) 102.8(9) 1_555 1_555 1_555 no C(27) C(26) H(32) 116.0(8) 1_555 1_555 1_555 no H(31) C(26) H(32) 106(1) 1_555 1_555 1_555 no C(17) C(27) C(26) 107.2(9) 1_555 1_555 1_555 yes C(17) C(27) H(33) 122(1) 1_555 1_555 1_555 no C(17) C(27) H(34) 109(1) 1_555 1_555 1_555 no C(26) C(27) H(33) 103.8(9) 1_555 1_555 1_555 no C(26) C(27) H(34) 109(1) 1_555 1_555 1_555 no H(33) C(27) H(34) 103(1) 1_555 1_555 1_555 no C(18) C(28) H(35) 114(1) 1_555 1_555 1_555 no C(18) C(28) H(36) 110(1) 1_555 1_555 1_555 no C(18) C(28) H(37) 116.1(8) 1_555 1_555 1_555 no H(35) C(28) H(36) 50.7(6) 1_555 1_555 1_555 no H(35) C(28) H(37) 124.2(9) 1_555 1_555 1_555 no H(36) C(28) H(37) 90.0(8) 1_555 1_555 1_555 no N(2) C(29) C(21) 177(1) 1_555 1_555 1_555 yes C(22) C(30) H(41) 121.8(9) 1_555 1_555 1_555 no C(22) C(30) H(42) 109(1) 1_555 1_555 1_555 no C(22) C(30) H(43) 118.1(9) 1_555 1_555 1_555 no H(41) C(30) H(42) 105.2(8) 1_555 1_555 1_555 no H(41) C(30) H(43) 94(1) 1_555 1_555 1_555 no H(42) C(30) H(43) 105.3(8) 1_555 1_555 1_555 no C(22) C(31) H(38) 113.3(10) 1_555 1_555 1_555 no C(22) C(31) H(39) 107.5(10) 1_555 1_555 1_555 no C(22) C(31) H(40) 110(1) 1_555 1_555 1_555 no H(38) C(31) H(39) 103.6(9) 1_555 1_555 1_555 no H(38) C(31) H(40) 113(1) 1_555 1_555 1_555 no H(39) C(31) H(40) 107.5(10) 1_555 1_555 1_555 no C(25) C(32) H(44) 111.5(9) 1_555 1_555 1_555 no C(25) C(32) H(45) 98(1) 1_555 1_555 1_555 no C(25) C(32) H(46) 115(1) 1_555 1_555 1_555 no H(44) C(32) H(45) 123(1) 1_555 1_555 1_555 no H(44) C(32) H(46) 76(1) 1_555 1_555 1_555 no H(45) C(32) H(46) 131(1) 1_555 1_555 1_555 no C(34) C(33) C(43) 128.5(9) 1_555 1_555 1_555 yes C(34) C(33) H(47) 115(1) 1_555 1_555 1_555 no C(43) C(33) H(47) 114.6(9) 1_555 1_555 1_555 no C(33) C(34) C(35) 122.6(8) 1_555 1_555 1_555 yes C(33) C(34) C(44) 121.6(9) 1_555 1_555 1_555 yes C(35) C(34) C(44) 115.2(9) 1_555 1_555 1_555 yes O(3) C(35) C(34) 122.4(9) 1_555 1_555 1_555 yes O(3) C(35) C(36) 124.3(9) 1_555 1_555 1_555 yes C(34) C(35) C(36) 113.2(8) 1_555 1_555 1_555 yes C(35) C(36) C(37) 110.7(7) 1_555 1_555 1_555 yes C(35) C(36) H(48) 108.5(8) 1_555 1_555 1_555 no C(35) C(36) H(49) 109.7(8) 1_555 1_555 1_555 no C(37) C(36) H(48) 110.4(9) 1_555 1_555 1_555 no C(37) C(36) H(49) 113.6(8) 1_555 1_555 1_555 no H(48) C(36) H(49) 103.6(9) 1_555 1_555 1_555 no C(36) C(37) C(38) 113.6(7) 1_555 1_555 1_555 yes C(36) C(37) C(45) 109.6(7) 1_555 1_555 1_555 yes C(36) C(37) H(50) 109.7(9) 1_555 1_555 1_555 no C(38) C(37) C(45) 109.8(7) 1_555 1_555 1_555 yes C(38) C(37) H(50) 109.3(7) 1_555 1_555 1_555 no C(45) C(37) H(50) 104.4(10) 1_555 1_555 1_555 no C(37) C(38) C(39) 112.7(8) 1_555 1_555 1_555 yes C(37) C(38) C(46) 109.7(8) 1_555 1_555 1_555 yes C(37) C(38) C(47) 112.8(7) 1_555 1_555 1_555 yes C(39) C(38) C(46) 103.0(7) 1_555 1_555 1_555 yes C(39) C(38) C(47) 113.1(8) 1_555 1_555 1_555 yes C(46) C(38) C(47) 104.8(8) 1_555 1_555 1_555 yes C(38) C(39) C(40) 119.1(7) 1_555 1_555 1_555 yes C(38) C(39) H(51) 113.9(9) 1_555 1_555 1_555 no C(38) C(39) H(52) 107.7(10) 1_555 1_555 1_555 no C(40) C(39) H(51) 105(1) 1_555 1_555 1_555 no C(40) C(39) H(52) 111.1(9) 1_555 1_555 1_555 no H(51) C(39) H(52) 97.5(8) 1_555 1_555 1_555 no C(39) C(40) C(41) 128.4(9) 1_555 1_555 1_555 yes C(39) C(40) H(53) 114.0(8) 1_555 1_555 1_555 no C(41) C(40) H(53) 117.6(9) 1_555 1_555 1_555 no C(40) C(41) C(42) 125.5(9) 1_555 1_555 1_555 yes C(40) C(41) C(48) 122.7(9) 1_555 1_555 1_555 yes C(42) C(41) C(48) 111.8(8) 1_555 1_555 1_555 yes C(41) C(42) C(43) 110.3(8) 1_555 1_555 1_555 yes C(41) C(42) H(54) 103.5(8) 1_555 1_555 1_555 no C(41) C(42) H(55) 120(1) 1_555 1_555 1_555 no C(43) C(42) H(54) 106.0(8) 1_555 1_555 1_555 no C(43) C(42) H(55) 92.8(8) 1_555 1_555 1_555 no H(54) C(42) H(55) 122(1) 1_555 1_555 1_555 no C(33) C(43) C(42) 116.4(8) 1_555 1_555 1_555 yes C(33) C(43) H(56) 117(1) 1_555 1_555 1_555 no C(33) C(43) H(57) 106.9(9) 1_555 1_555 1_555 no C(42) C(43) H(56) 107.8(9) 1_555 1_555 1_555 no C(42) C(43) H(57) 104.2(9) 1_555 1_555 1_555 no H(56) C(43) H(57) 101.8(7) 1_555 1_555 1_555 no C(34) C(44) H(58) 110.4(8) 1_555 1_555 1_555 no C(34) C(44) H(59) 117(1) 1_555 1_555 1_555 no C(34) C(44) H(60) 116(1) 1_555 1_555 1_555 no H(58) C(44) H(59) 121.5(10) 1_555 1_555 1_555 no H(58) C(44) H(60) 97(1) 1_555 1_555 1_555 no H(59) C(44) H(60) 90.0(8) 1_555 1_555 1_555 no N(3) C(45) C(37) 175(1) 1_555 1_555 1_555 yes C(38) C(46) H(64) 103.5(10) 1_555 1_555 1_555 no C(38) C(46) H(65) 110(1) 1_555 1_555 1_555 no C(38) C(46) H(66) 109.1(10) 1_555 1_555 1_555 no H(64) C(46) H(65) 108(1) 1_555 1_555 1_555 no H(64) C(46) H(66) 116(1) 1_555 1_555 1_555 no H(65) C(46) H(66) 108(1) 1_555 1_555 1_555 no C(38) C(47) H(61) 110.4(9) 1_555 1_555 1_555 no C(38) C(47) H(62) 118(1) 1_555 1_555 1_555 no C(38) C(47) H(63) 107.8(9) 1_555 1_555 1_555 no H(61) C(47) H(62) 107(1) 1_555 1_555 1_555 no H(61) C(47) H(63) 108(1) 1_555 1_555 1_555 no H(62) C(47) H(63) 103.5(10) 1_555 1_555 1_555 no C(41) C(48) H(67) 111.9(10) 1_555 1_555 1_555 no C(41) C(48) H(68) 109(1) 1_555 1_555 1_555 no C(41) C(48) H(69) 108(1) 1_555 1_555 1_555 no H(67) C(48) H(68) 109(1) 1_555 1_555 1_555 no H(67) C(48) H(69) 109(1) 1_555 1_555 1_555 no H(68) C(48) H(69) 107(1) 1_555 1_555 1_555 no C(50) C(49) C(59) 128.4(9) 1_555 1_555 1_555 yes C(50) C(49) H(70) 112(1) 1_555 1_555 1_555 no C(59) C(49) H(70) 118.7(9) 1_555 1_555 1_555 no C(49) C(50) C(51) 124.0(9) 1_555 1_555 1_555 yes C(49) C(50) C(60) 118.6(9) 1_555 1_555 1_555 yes C(51) C(50) C(60) 117.4(9) 1_555 1_555 1_555 yes O(4) C(51) C(50) 125.7(10) 1_555 1_555 1_555 yes O(4) C(51) C(52) 121.3(9) 1_555 1_555 1_555 yes C(50) C(51) C(52) 112.9(8) 1_555 1_555 1_555 yes C(51) C(52) C(53) 114.1(8) 1_555 1_555 1_555 yes C(51) C(52) H(71) 111.5(8) 1_555 1_555 1_555 no C(51) C(52) H(72) 103.7(7) 1_555 1_555 1_555 no C(53) C(52) H(71) 112.8(8) 1_555 1_555 1_555 no C(53) C(52) H(72) 114.2(9) 1_555 1_555 1_555 no H(71) C(52) H(72) 99.2(9) 1_555 1_555 1_555 no C(52) C(53) C(54) 118.2(8) 1_555 1_555 1_555 yes C(52) C(53) C(61) 107.1(7) 1_555 1_555 1_555 yes C(52) C(53) H(73) 111(1) 1_555 1_555 1_555 no C(54) C(53) C(61) 108.0(8) 1_555 1_555 1_555 yes C(54) C(53) H(73) 104.5(8) 1_555 1_555 1_555 no C(61) C(53) H(73) 107(1) 1_555 1_555 1_555 no C(53) C(54) C(55) 107.3(7) 1_555 1_555 1_555 yes C(53) C(54) C(62) 109.0(8) 1_555 1_555 1_555 yes C(53) C(54) C(63) 112.3(8) 1_555 1_555 1_555 yes C(55) C(54) C(62) 102.5(8) 1_555 1_555 1_555 yes C(55) C(54) C(63) 112.2(9) 1_555 1_555 1_555 yes C(62) C(54) C(63) 112.9(9) 1_555 1_555 1_555 yes C(54) C(55) C(56) 118.2(8) 1_555 1_555 1_555 yes C(54) C(55) H(74) 108.6(9) 1_555 1_555 1_555 no C(54) C(55) H(75) 102(1) 1_555 1_555 1_555 no C(56) C(55) H(74) 114(1) 1_555 1_555 1_555 no C(56) C(55) H(75) 119(1) 1_555 1_555 1_555 no H(74) C(55) H(75) 89.1(9) 1_555 1_555 1_555 no C(55) C(56) C(57) 124(1) 1_555 1_555 1_555 yes C(55) C(56) H(76) 111.4(9) 1_555 1_555 1_555 no C(57) C(56) H(76) 124(1) 1_555 1_555 1_555 no C(56) C(57) C(58) 122(1) 1_555 1_555 1_555 yes C(56) C(57) C(64) 121(1) 1_555 1_555 1_555 yes C(58) C(57) C(64) 116.6(9) 1_555 1_555 1_555 yes C(57) C(58) C(59) 111.1(9) 1_555 1_555 1_555 yes C(57) C(58) H(77) 107(1) 1_555 1_555 1_555 no C(57) C(58) H(78) 111(1) 1_555 1_555 1_555 no C(59) C(58) H(77) 119.4(10) 1_555 1_555 1_555 no C(59) C(58) H(78) 97.3(9) 1_555 1_555 1_555 no H(77) C(58) H(78) 110(1) 1_555 1_555 1_555 no C(49) C(59) C(58) 112.4(9) 1_555 1_555 1_555 yes C(49) C(59) H(79) 117.3(8) 1_555 1_555 1_555 no C(49) C(59) H(80) 103.3(9) 1_555 1_555 1_555 no C(58) C(59) H(79) 104.0(8) 1_555 1_555 1_555 no C(58) C(59) H(80) 101.7(9) 1_555 1_555 1_555 no H(79) C(59) H(80) 117(1) 1_555 1_555 1_555 no C(50) C(60) H(81) 115(1) 1_555 1_555 1_555 no C(50) C(60) H(82) 104.1(9) 1_555 1_555 1_555 no C(50) C(60) H(83) 104(1) 1_555 1_555 1_555 no H(81) C(60) H(82) 100(1) 1_555 1_555 1_555 no H(81) C(60) H(83) 124(1) 1_555 1_555 1_555 no H(82) C(60) H(83) 105(1) 1_555 1_555 1_555 no N(4) C(61) C(53) 177(1) 1_555 1_555 1_555 yes C(54) C(62) H(87) 109.2(9) 1_555 1_555 1_555 no C(54) C(62) H(88) 111(1) 1_555 1_555 1_555 no C(54) C(62) H(89) 120(1) 1_555 1_555 1_555 no H(87) C(62) H(88) 104(1) 1_555 1_555 1_555 no H(87) C(62) H(89) 104(1) 1_555 1_555 1_555 no H(88) C(62) H(89) 106.5(9) 1_555 1_555 1_555 no C(54) C(63) H(84) 118.8(10) 1_555 1_555 1_555 no C(54) C(63) H(85) 111(1) 1_555 1_555 1_555 no C(54) C(63) H(86) 112(1) 1_555 1_555 1_555 no H(84) C(63) H(85) 110(1) 1_555 1_555 1_555 no H(84) C(63) H(86) 104(1) 1_555 1_555 1_555 no H(85) C(63) H(86) 96.6(8) 1_555 1_555 1_555 no C(57) C(64) H(90) 111.8(10) 1_555 1_555 1_555 no C(57) C(64) H(91) 98(1) 1_555 1_555 1_555 no C(57) C(64) H(92) 108(1) 1_555 1_555 1_555 no H(90) C(64) H(91) 144(1) 1_555 1_555 1_555 no H(90) C(64) H(92) 100(1) 1_555 1_555 1_555 no H(91) C(64) H(92) 85.7(9) 1_555 1_555 1_555 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) 41(1) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(12) -142.0(9) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) -17(1) 1_555 1_555 1_555 1_555 yes O(2) C(19) C(18) C(17) -47(1) 1_555 1_555 1_555 1_555 yes O(2) C(19) C(18) C(28) 134(1) 1_555 1_555 1_555 1_555 yes O(2) C(19) C(20) C(21) 25(1) 1_555 1_555 1_555 1_555 yes O(3) C(35) C(34) C(33) 47(1) 1_555 1_555 1_555 1_555 yes O(3) C(35) C(34) C(44) -140(1) 1_555 1_555 1_555 1_555 yes O(3) C(35) C(36) C(37) -20(1) 1_555 1_555 1_555 1_555 yes O(4) C(51) C(50) C(49) -45(1) 1_555 1_555 1_555 1_555 yes O(4) C(51) C(50) C(60) 135(1) 1_555 1_555 1_555 1_555 yes O(4) C(51) C(52) C(53) 23(1) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(5) C(4) -167(27) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(5) C(6) 64(27) 1_555 1_555 1_555 1_555 yes N(2) C(29) C(21) C(20) -31(22) 1_555 1_555 1_555 1_555 yes N(2) C(29) C(21) C(22) 101(22) 1_555 1_555 1_555 1_555 yes N(3) C(45) C(37) C(36) -83(13) 1_555 1_555 1_555 1_555 yes N(3) C(45) C(37) C(38) 150(13) 1_555 1_555 1_555 1_555 yes N(4) C(61) C(53) C(52) -46(29) 1_555 1_555 1_555 1_555 yes N(4) C(61) C(53) C(54) 81(29) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) -135(1) 1_555 1_555 1_555 1_555 yes C(1) C(11) C(10) C(9) -90(1) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(11) C(10) 78(1) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 159.3(9) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(11) 1(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -106(1) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(13) 129.3(9) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(12) 41(1) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 72.5(10) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(14) -168.5(8) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(15) -48(1) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -57(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 132(1) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(13) -164.3(8) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -177.0(8) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(16) -1(1) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(14) -175.9(9) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(15) 64(1) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) 107(1) 1_555 1_555 1_555 1_555 yes C(11) C(1) C(2) C(12) -174(1) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(16) -69(1) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(14) -45(1) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(15) 74(1) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 139.3(10) 1_555 1_555 1_555 1_555 yes C(17) C(27) C(26) C(25) 91(1) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(27) C(26) -82(1) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) -160.6(7) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(17) C(27) 3(1) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) 99.9(10) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(29) -129.2(9) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(18) C(28) -38(1) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) -71(1) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(30) 170.8(7) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(31) 53(1) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 62(1) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) -137.2(9) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(29) 158.6(9) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 179.3(9) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(32) 5(1) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(30) -179.8(9) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(31) -60(1) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -105(1) 1_555 1_555 1_555 1_555 yes C(27) C(17) C(18) C(28) -178(1) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(32) 68(1) 1_555 1_555 1_555 1_555 yes C(29) C(21) C(22) C(30) 41(1) 1_555 1_555 1_555 1_555 yes C(29) C(21) C(22) C(31) -76(1) 1_555 1_555 1_555 1_555 yes C(33) C(34) C(35) C(36) -136(1) 1_555 1_555 1_555 1_555 yes C(33) C(43) C(42) C(41) -85(1) 1_555 1_555 1_555 1_555 yes C(34) C(33) C(43) C(42) 82(1) 1_555 1_555 1_555 1_555 yes C(34) C(35) C(36) C(37) 162.9(7) 1_555 1_555 1_555 1_555 yes C(35) C(34) C(33) C(43) 0(1) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(38) -105.0(9) 1_555 1_555 1_555 1_555 yes C(35) C(36) C(37) C(45) 131.7(9) 1_555 1_555 1_555 1_555 yes C(36) C(35) C(34) C(44) 35(1) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(39) 76.6(10) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(46) -169.2(8) 1_555 1_555 1_555 1_555 yes C(36) C(37) C(38) C(47) -52(1) 1_555 1_555 1_555 1_555 yes C(37) C(38) C(39) C(40) -56(1) 1_555 1_555 1_555 1_555 yes C(38) C(39) C(40) C(41) 132(1) 1_555 1_555 1_555 1_555 yes C(39) C(38) C(37) C(45) -160.2(8) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(42) 179.7(9) 1_555 1_555 1_555 1_555 yes C(39) C(40) C(41) C(48) -2(1) 1_555 1_555 1_555 1_555 yes C(40) C(39) C(38) C(46) -174.9(9) 1_555 1_555 1_555 1_555 yes C(40) C(39) C(38) C(47) 72(1) 1_555 1_555 1_555 1_555 yes C(40) C(41) C(42) C(43) 99(1) 1_555 1_555 1_555 1_555 yes C(43) C(33) C(34) C(44) -172.5(10) 1_555 1_555 1_555 1_555 yes C(43) C(42) C(41) C(48) -78(1) 1_555 1_555 1_555 1_555 yes C(45) C(37) C(38) C(46) -46.1(10) 1_555 1_555 1_555 1_555 yes C(45) C(37) C(38) C(47) 70.3(10) 1_555 1_555 1_555 1_555 yes C(49) C(50) C(51) C(52) 134(1) 1_555 1_555 1_555 1_555 yes C(49) C(59) C(58) C(57) 84(1) 1_555 1_555 1_555 1_555 yes C(50) C(49) C(59) C(58) -81(1) 1_555 1_555 1_555 1_555 yes C(50) C(51) C(52) C(53) -157.5(8) 1_555 1_555 1_555 1_555 yes C(51) C(50) C(49) C(59) 2(1) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(54) 108.6(9) 1_555 1_555 1_555 1_555 yes C(51) C(52) C(53) C(61) -129.1(8) 1_555 1_555 1_555 1_555 yes C(52) C(51) C(50) C(60) -44(1) 1_555 1_555 1_555 1_555 yes C(52) C(53) C(54) C(55) -77.5(10) 1_555 1_555 1_555 1_555 yes C(52) C(53) C(54) C(62) 172.2(8) 1_555 1_555 1_555 1_555 yes C(52) C(53) C(54) C(63) 46(1) 1_555 1_555 1_555 1_555 yes C(53) C(54) C(55) C(56) 58(1) 1_555 1_555 1_555 1_555 yes C(54) C(55) C(56) C(57) -133(1) 1_555 1_555 1_555 1_555 yes C(55) C(54) C(53) C(61) 160.7(8) 1_555 1_555 1_555 1_555 yes C(55) C(56) C(57) C(58) -176.5(10) 1_555 1_555 1_555 1_555 yes C(55) C(56) C(57) C(64) 0(1) 1_555 1_555 1_555 1_555 yes C(56) C(55) C(54) C(62) 172(1) 1_555 1_555 1_555 1_555 yes C(56) C(55) C(54) C(63) -65(1) 1_555 1_555 1_555 1_555 yes C(56) C(57) C(58) C(59) -103(1) 1_555 1_555 1_555 1_555 yes C(59) C(49) C(50) C(60) -177(1) 1_555 1_555 1_555 1_555 yes C(59) C(58) C(57) C(64) 79(1) 1_555 1_555 1_555 1_555 yes C(61) C(53) C(54) C(62) 50.4(10) 1_555 1_555 1_555 1_555 yes C(61) C(53) C(54) C(63) -75(1) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) H(1) 2.69(1) 1_555 1_545 ? O(1) H(58) 3.001(7) 1_555 2_546 ? O(1) H(8) 3.14(1) 1_555 1_545 ? O(1) H(39) 3.374(6) 1_555 2_546 ? O(1) H(47) 3.424(8) 1_555 2_546 ? O(1) C(1) 3.51(1) 1_555 1_545 ? O(1) C(44) 3.55(1) 1_555 2_546 ? O(1) H(11) 3.57(1) 1_555 1_545 ? O(2) H(24) 2.69(1) 1_555 1_565 ? O(2) H(35) 2.740(9) 1_555 2_656 ? O(2) H(31) 2.95(1) 1_555 1_565 ? O(2) H(62) 3.407(8) 1_555 2_656 ? O(2) C(17) 3.47(1) 1_555 1_565 ? O(2) C(28) 3.52(1) 1_555 2_656 ? O(3) H(54) 2.94(1) 1_555 1_545 ? O(3) H(12) 3.030(8) 1_555 2_546 ? O(3) H(47) 3.03(1) 1_555 1_545 ? O(3) H(85) 3.354(8) 1_555 2_647 ? O(3) C(33) 3.48(1) 1_555 1_545 ? O(3) H(13) 3.497(9) 1_555 2_546 ? O(3) H(57) 3.52(1) 1_555 1_545 ? O(3) C(12) 3.58(1) 1_555 2_546 ? O(4) H(81) 2.593(9) 1_555 2_757 ? O(4) H(70) 2.70(1) 1_555 1_565 ? O(4) H(78) 2.94(1) 1_555 1_565 ? O(4) H(80) 3.44(1) 1_555 1_565 ? O(4) H(16) 3.448(8) 1_555 2_656 ? O(4) C(49) 3.46(1) 1_555 1_565 ? O(4) C(60) 3.52(2) 1_555 2_757 ? N(1) H(72) 2.55(1) 1_555 1_444 ? N(1) H(82) 2.60(1) 1_555 1_444 ? N(1) H(15) 2.75(2) 1_555 1_545 ? N(1) H(14) 2.80(1) 1_555 1_545 ? N(1) H(2) 2.84(2) 1_555 1_545 ? N(1) H(80) 3.16(1) 1_555 2_646 ? N(1) H(7) 3.25(1) 1_555 1_545 ? N(1) H(79) 3.32(1) 1_555 2_646 ? N(1) C(59) 3.56(2) 1_555 2_646 ? N(1) C(52) 3.60(1) 1_555 1_444 ? N(2) H(59) 2.68(1) 1_555 1_565 ? N(2) H(37) 2.75(1) 1_555 1_565 ? N(2) H(38) 2.76(1) 1_555 1_565 ? N(2) H(11) 2.89(1) 1_555 2_556 ? N(2) H(25) 2.95(2) 1_555 1_565 ? N(2) H(10) 3.14(1) 1_555 2_556 ? N(2) H(58) 3.34(1) 1_555 1_555 ? N(2) H(30) 3.40(1) 1_555 1_565 ? N(2) C(36) 3.51(1) 1_555 1_565 ? N(2) C(11) 3.57(2) 1_555 2_556 ? N(3) H(26) 2.59(1) 1_555 1_545 ? N(3) H(36) 2.68(1) 1_555 1_545 ? N(3) H(61) 2.75(1) 1_555 1_545 ? N(3) H(60) 2.79(1) 1_555 1_545 ? N(3) H(49) 2.83(2) 1_555 1_545 ? N(3) H(34) 2.88(1) 1_555 2_646 ? N(3) H(53) 3.22(1) 1_555 1_545 ? N(3) H(33) 3.38(1) 1_555 2_646 ? N(3) C(27) 3.55(2) 1_555 2_646 ? N(3) H(35) 3.56(1) 1_555 1_545 ? N(4) H(3) 2.567(10) 1_555 1_666 ? N(4) H(13) 2.82(1) 1_555 1_666 ? N(4) H(83) 2.82(1) 1_555 1_565 ? N(4) H(84) 2.86(2) 1_555 1_565 ? N(4) H(57) 2.94(1) 1_555 2_657 ? N(4) H(71) 2.97(2) 1_555 1_565 ? N(4) H(12) 3.27(2) 1_555 1_656 ? N(4) H(56) 3.29(1) 1_555 2_657 ? N(4) H(76) 3.44(1) 1_555 1_565 ? N(4) H(14) 3.57(2) 1_555 1_656 ? C(1) H(59) 3.34(1) 1_555 2_556 ? C(1) H(58) 3.51(2) 1_555 2_546 ? C(1) H(4) 3.54(1) 1_555 1_565 ? C(2) H(47) 2.98(1) 1_555 2_546 ? C(2) H(58) 3.48(1) 1_555 2_546 ? C(3) H(47) 3.242(9) 1_555 2_546 ? C(3) H(58) 3.552(9) 1_555 2_546 ? C(3) H(1) 3.57(1) 1_555 1_545 ? C(4) H(83) 3.347(10) 1_555 1_454 ? C(5) H(7) 3.33(2) 1_555 1_545 ? C(7) H(28) 2.95(1) 1_555 1_555 ? C(7) H(43) 3.39(1) 1_555 1_545 ? C(8) H(28) 2.954(9) 1_555 1_555 ? C(8) H(20) 3.12(1) 1_555 1_565 ? C(9) H(28) 3.23(1) 1_555 1_555 ? C(9) H(42) 3.43(1) 1_555 1_555 ? C(10) H(4) 3.21(1) 1_555 1_565 ? C(10) H(42) 3.42(1) 1_555 1_555 ? C(10) H(23) 3.45(2) 1_555 1_565 ? C(11) H(41) 3.06(1) 1_555 2_546 ? C(11) H(59) 3.46(2) 1_555 2_556 ? C(11) H(39) 3.52(2) 1_555 2_546 ? C(12) H(47) 2.96(1) 1_555 2_546 ? C(12) H(85) 3.119(9) 1_555 1_454 ? C(12) H(71) 3.50(1) 1_555 1_454 ? C(12) H(84) 3.527(10) 1_555 1_454 ? C(12) H(72) 3.54(1) 1_555 1_454 ? C(12) H(57) 3.56(1) 1_555 2_546 ? C(13) H(7) 3.04(1) 1_555 1_545 ? C(13) H(14) 3.19(1) 1_555 1_545 ? C(13) H(15) 3.34(2) 1_555 1_545 ? C(13) H(2) 3.41(2) 1_555 1_545 ? C(13) H(72) 3.48(1) 1_555 1_444 ? C(13) H(83) 3.55(1) 1_555 1_454 ? C(13) H(79) 3.59(1) 1_555 2_646 ? C(14) H(44) 3.10(1) 1_555 1_545 ? C(14) H(91) 3.118(9) 1_555 2_646 ? C(14) H(7) 3.17(1) 1_555 1_545 ? C(14) H(29) 3.23(1) 1_555 1_545 ? C(14) H(79) 3.353(10) 1_555 2_646 ? C(15) H(80) 3.30(1) 1_555 2_656 ? C(15) H(79) 3.36(1) 1_555 2_646 ? C(15) H(82) 3.40(1) 1_555 1_454 ? C(15) H(92) 3.426(9) 1_555 2_646 ? C(15) H(81) 3.462(9) 1_555 1_454 ? C(16) H(8) 3.39(2) 1_555 1_545 ? C(16) H(40) 3.45(1) 1_555 1_555 ? C(16) H(40) 3.57(1) 1_555 2_546 ? C(16) H(9) 3.57(1) 1_555 2_546 ? C(16) H(22) 3.59(1) 1_555 2_546 ? C(17) H(35) 3.03(1) 1_555 2_646 ? C(17) H(36) 3.21(1) 1_555 2_646 ? C(18) H(24) 3.19(1) 1_555 2_656 ? C(19) H(24) 3.52(1) 1_555 1_565 ? C(19) H(24) 3.595(8) 1_555 2_656 ? C(20) H(60) 3.295(8) 1_555 1_555 ? C(21) H(31) 3.25(1) 1_555 1_565 ? C(21) H(30) 3.43(1) 1_555 1_565 ? C(23) H(5) 2.87(1) 1_555 1_555 ? C(23) H(20) 3.32(1) 1_555 1_565 ? C(24) H(5) 2.991(10) 1_555 1_555 ? C(24) H(43) 3.03(1) 1_555 1_545 ? C(25) H(5) 3.266(10) 1_555 1_555 ? C(25) H(19) 3.42(1) 1_555 1_555 ? C(26) H(19) 3.40(1) 1_555 1_555 ? C(26) H(46) 3.45(2) 1_555 1_545 ? C(26) H(44) 3.50(1) 1_555 1_545 ? C(26) H(27) 3.50(1) 1_555 1_545 ? C(27) H(64) 3.06(1) 1_555 2_656 ? C(27) H(35) 3.32(2) 1_555 2_646 ? C(27) H(36) 3.36(1) 1_555 2_646 ? C(27) H(62) 3.57(2) 1_555 2_656 ? C(28) H(24) 3.14(1) 1_555 2_656 ? C(28) H(62) 3.177(9) 1_555 1_555 ? C(28) H(48) 3.55(1) 1_555 1_555 ? C(28) H(61) 3.599(10) 1_555 1_555 ? C(29) H(30) 3.12(1) 1_555 1_565 ? C(29) H(37) 3.19(1) 1_555 1_565 ? C(29) H(38) 3.27(2) 1_555 1_565 ? C(29) H(10) 3.40(1) 1_555 2_556 ? C(29) H(48) 3.45(1) 1_555 1_565 ? C(29) H(25) 3.49(2) 1_555 1_565 ? C(29) H(60) 3.53(1) 1_555 1_555 ? C(29) H(11) 3.55(1) 1_555 2_556 ? C(29) H(58) 3.55(1) 1_555 1_555 ? C(30) H(21) 3.18(1) 1_555 1_565 ? C(30) H(30) 3.24(2) 1_555 1_565 ? C(30) H(22) 3.25(1) 1_555 2_556 ? C(30) H(10) 3.331(10) 1_555 2_556 ? C(30) H(6) 3.36(1) 1_555 1_565 ? C(31) H(11) 3.01(1) 1_555 2_546 ? C(31) H(59) 3.17(1) 1_555 1_555 ? C(31) H(10) 3.39(2) 1_555 2_556 ? C(31) H(23) 3.57(1) 1_555 2_556 ? C(31) H(21) 3.59(1) 1_555 1_555 ? C(32) H(77) 3.20(1) 1_555 2_656 ? C(32) H(63) 3.49(2) 1_555 2_656 ? C(33) H(13) 3.01(1) 1_555 2_556 ? C(33) H(12) 3.51(1) 1_555 2_546 ? C(33) H(50) 3.54(1) 1_555 1_565 ? C(34) H(1) 3.09(1) 1_555 2_546 ? C(34) H(12) 3.43(1) 1_555 2_546 ? C(35) H(12) 3.540(10) 1_555 2_546 ? C(35) H(1) 3.549(9) 1_555 2_546 ? C(36) H(37) 3.143(9) 1_555 1_555 ? C(37) H(54) 3.15(1) 1_555 1_545 ? C(37) H(53) 3.31(1) 1_555 1_545 ? C(39) H(74) 2.85(1) 1_555 1_555 ? C(39) H(89) 3.35(1) 1_555 1_545 ? C(40) H(74) 2.721(9) 1_555 1_555 ? C(40) H(66) 3.18(1) 1_555 1_565 ? C(41) H(74) 3.04(1) 1_555 1_555 ? C(41) H(88) 3.51(1) 1_555 1_555 ? C(42) H(50) 3.27(1) 1_555 1_565 ? C(42) H(67) 3.37(2) 1_555 1_565 ? C(42) H(88) 3.47(1) 1_555 1_555 ? C(43) H(87) 3.115(10) 1_555 2_647 ? C(43) H(13) 3.23(1) 1_555 2_556 ? C(43) H(85) 3.53(1) 1_555 2_647 ? C(44) H(39) 2.90(1) 1_555 1_555 ? C(44) H(1) 3.00(1) 1_555 2_546 ? C(44) H(25) 3.547(9) 1_555 1_555 ? C(44) H(11) 3.56(1) 1_555 2_546 ? C(44) H(38) 3.58(1) 1_555 1_555 ? C(45) H(53) 3.03(1) 1_555 1_545 ? C(45) H(60) 3.24(1) 1_555 1_545 ? C(45) H(61) 3.32(1) 1_555 1_545 ? C(45) H(49) 3.42(1) 1_555 1_545 ? C(45) H(37) 3.47(1) 1_555 1_555 ? C(45) H(34) 3.50(1) 1_555 2_646 ? C(45) H(26) 3.52(1) 1_555 1_545 ? C(45) H(33) 3.57(1) 1_555 2_646 ? C(46) H(90) 2.85(1) 1_555 1_545 ? C(46) H(75) 3.20(1) 1_555 1_545 ? C(46) H(53) 3.21(2) 1_555 1_545 ? C(46) H(33) 3.36(1) 1_555 2_646 ? C(47) H(34) 3.14(1) 1_555 2_656 ? C(47) H(35) 3.21(1) 1_555 1_555 ? C(47) H(33) 3.27(1) 1_555 2_646 ? C(47) H(36) 3.30(1) 1_555 1_555 ? C(47) H(46) 3.36(1) 1_555 2_646 ? C(48) H(86) 3.40(1) 1_555 1_555 ? C(48) H(55) 3.46(1) 1_555 2_647 ? C(48) H(74) 3.54(1) 1_555 1_555 ? C(48) H(88) 3.60(2) 1_555 1_545 ? C(49) H(82) 3.08(1) 1_555 2_747 ? C(50) H(70) 3.19(1) 1_555 2_757 ? C(50) H(81) 3.51(1) 1_555 2_757 ? C(51) H(81) 3.27(1) 1_555 2_757 ? C(51) H(70) 3.49(2) 1_555 1_565 ? C(51) H(70) 3.555(10) 1_555 2_757 ? C(52) H(14) 3.255(9) 1_555 1_656 ? C(53) H(78) 3.19(1) 1_555 1_565 ? C(53) H(76) 3.51(1) 1_555 1_565 ? C(55) H(51) 2.75(1) 1_555 1_555 ? C(55) H(66) 3.34(1) 1_555 1_565 ? C(56) H(51) 2.713(9) 1_555 1_555 ? C(56) H(89) 3.08(1) 1_555 1_545 ? C(57) H(51) 3.12(1) 1_555 1_555 ? C(57) H(65) 3.48(1) 1_555 1_555 ? C(58) H(65) 3.39(1) 1_555 1_555 ? C(58) H(92) 3.44(2) 1_555 1_545 ? C(58) H(73) 3.56(2) 1_555 1_545 ? C(59) H(18) 3.10(1) 1_555 2_656 ? C(59) H(82) 3.21(1) 1_555 2_747 ? C(60) H(16) 3.12(1) 1_555 1_656 ? C(60) H(70) 3.13(2) 1_555 2_757 ? C(60) H(3) 3.47(1) 1_555 1_656 ? C(60) H(2) 3.51(1) 1_555 1_656 ? C(60) H(15) 3.53(1) 1_555 1_656 ? C(61) H(83) 3.18(1) 1_555 1_565 ? C(61) H(76) 3.19(1) 1_555 1_565 ? C(61) H(84) 3.36(1) 1_555 1_565 ? C(61) H(71) 3.47(2) 1_555 1_565 ? C(61) H(3) 3.48(1) 1_555 1_666 ? C(61) H(14) 3.49(1) 1_555 1_656 ? C(61) H(12) 3.50(1) 1_555 1_656 ? C(61) H(56) 3.57(1) 1_555 2_657 ? C(61) H(57) 3.58(1) 1_555 2_657 ? C(62) H(76) 3.16(2) 1_555 1_565 ? C(62) H(52) 3.18(1) 1_555 1_565 ? C(62) H(68) 3.37(1) 1_555 1_565 ? C(62) H(69) 3.42(1) 1_555 2_657 ? C(62) H(56) 3.45(1) 1_555 2_657 ? C(63) H(57) 3.06(1) 1_555 2_647 ? C(63) H(13) 3.30(1) 1_555 1_656 ? C(63) H(56) 3.41(2) 1_555 2_657 ? C(63) H(68) 3.55(1) 1_555 1_555 ? C(64) H(32) 3.15(1) 1_555 2_656 ? C(64) H(63) 3.33(2) 1_555 1_555 ? C(64) H(45) 3.43(2) 1_555 2_656 ? C(64) H(51) 3.56(1) 1_555 1_555 ? C(64) H(17) 3.57(1) 1_555 2_656 ? H(1) H(59) 2.6495(5) 1_555 2_556 ? H(1) H(4) 3.322(1) 1_555 1_565 ? H(1) H(58) 3.3703(4) 1_555 2_556 ? H(2) H(82) 3.1957(1) 1_555 1_454 ? H(3) H(83) 2.6322(1) 1_555 1_454 ? H(4) H(7) 2.7150(1) 1_555 1_545 ? H(5) H(29) 3.1737(4) 1_555 1_555 ? H(5) H(43) 3.3744(1) 1_555 1_545 ? H(5) H(30) 3.4716(7) 1_555 1_555 ? H(5) H(44) 3.5393(7) 1_555 1_555 ? H(6) H(43) 2.7302(5) 1_555 1_545 ? H(6) H(42) 2.9138(1) 1_555 1_545 ? H(6) H(8) 3.1092(5) 1_555 1_545 ? H(6) H(28) 3.2026(4) 1_555 1_555 ? H(7) H(18) 3.3265(4) 1_555 1_565 ? H(7) H(28) 3.5447(7) 1_555 1_555 ? H(8) H(42) 3.0312(9) 1_555 1_555 ? H(8) H(40) 3.4466(4) 1_555 2_556 ? H(8) H(21) 3.5193(3) 1_555 1_565 ? H(8) H(22) 3.5755(1) 1_555 2_556 ? H(9) H(40) 3.0415(3) 1_555 2_556 ? H(9) H(41) 3.1565(5) 1_555 2_546 ? H(9) H(22) 3.1665(2) 1_555 2_556 ? H(9) H(42) 3.207(1) 1_555 1_555 ? H(10) H(58) 3.0342(6) 1_555 2_546 ? H(11) H(59) 2.6011(7) 1_555 2_556 ? H(11) H(38) 2.6363(2) 1_555 2_556 ? H(11) H(39) 3.0114(1) 1_555 2_556 ? H(12) H(85) 2.7851(2) 1_555 1_454 ? H(12) H(56) 3.1396(7) 1_555 2_556 ? H(12) H(47) 3.4502(2) 1_555 2_546 ? H(13) H(84) 2.8467(1) 1_555 1_454 ? H(13) H(85) 2.8467(2) 1_555 1_454 ? H(13) H(71) 3.2787(2) 1_555 1_454 ? H(14) H(72) 2.6695(1) 1_555 1_454 ? H(14) H(85) 3.2577(8) 1_555 1_454 ? H(14) H(83) 3.4686(3) 1_555 1_454 ? H(14) H(84) 3.4830(4) 1_555 1_454 ? H(15) H(82) 2.8742(1) 1_555 1_454 ? H(15) H(80) 2.9300(3) 1_555 2_656 ? H(15) H(18) 3.2146(1) 1_555 1_565 ? H(15) H(83) 3.5535(4) 1_555 1_454 ? H(16) H(81) 2.5820(1) 1_555 1_454 ? H(16) H(92) 2.900(1) 1_555 2_646 ? H(16) H(82) 2.9619(3) 1_555 1_454 ? H(16) H(80) 3.0999(1) 1_555 2_656 ? H(16) H(91) 3.2133(9) 1_555 2_646 ? H(16) H(83) 3.3360(8) 1_555 1_454 ? H(17) H(92) 2.7588(5) 1_555 2_646 ? H(17) H(45) 2.8777(9) 1_555 1_555 ? H(17) H(91) 3.0879(5) 1_555 2_646 ? H(17) H(77) 3.2362(5) 1_555 2_656 ? H(18) H(91) 2.5889(8) 1_555 2_646 ? H(18) H(44) 3.2317(7) 1_555 1_545 ? H(18) H(77) 3.4373(7) 1_555 2_646 ? H(18) H(92) 3.4591(6) 1_555 2_646 ? H(19) H(91) 2.7055(3) 1_555 2_646 ? H(19) H(29) 2.7406(1) 1_555 1_545 ? H(19) H(32) 2.7456(9) 1_555 1_555 ? H(19) H(31) 3.3972(8) 1_555 1_555 ? H(19) H(45) 3.5325(4) 1_555 1_555 ? H(20) H(29) 2.6586(6) 1_555 1_545 ? H(20) H(44) 2.986(1) 1_555 1_545 ? H(20) H(28) 3.3041(1) 1_555 1_545 ? H(20) H(43) 3.3127(1) 1_555 1_545 ? H(21) H(40) 2.7455(3) 1_555 1_555 ? H(21) H(43) 2.8287(7) 1_555 1_545 ? H(21) H(42) 2.8769(1) 1_555 1_545 ? H(21) H(41) 2.8795(5) 1_555 1_545 ? H(21) H(28) 2.8934(6) 1_555 1_555 ? H(22) H(42) 2.7015(3) 1_555 2_546 ? H(22) H(41) 2.7732(8) 1_555 2_546 ? H(22) H(40) 3.3083(5) 1_555 2_546 ? H(22) H(40) 3.372(1) 1_555 1_555 ? H(22) H(23) 3.4200(1) 1_555 2_556 ? H(23) H(40) 2.9041(5) 1_555 2_546 ? H(23) H(39) 3.239(1) 1_555 2_546 ? H(24) H(36) 2.7400(6) 1_555 2_646 ? H(24) H(27) 3.455(1) 1_555 1_545 ? H(25) H(59) 2.9795(1) 1_555 1_555 ? H(26) H(60) 2.7415(1) 1_555 1_555 ? H(26) H(59) 3.5461(4) 1_555 1_555 ? H(27) H(30) 2.9659(1) 1_555 1_565 ? H(29) H(31) 3.0373(5) 1_555 1_565 ? H(30) H(41) 3.2096(4) 1_555 1_545 ? H(31) H(44) 2.9652(2) 1_555 1_545 ? H(31) H(43) 3.358(1) 1_555 1_545 ? H(32) H(91) 2.8415(2) 1_555 2_646 ? H(32) H(44) 2.9357(2) 1_555 1_545 ? H(32) H(63) 3.2777(5) 1_555 2_646 ? H(32) H(64) 3.4417(7) 1_555 2_656 ? H(32) H(92) 3.4979(1) 1_555 2_646 ? H(33) H(35) 3.5086(4) 1_555 2_656 ? H(34) H(36) 2.6358(7) 1_555 2_646 ? H(34) H(35) 2.6616(3) 1_555 2_646 ? H(34) H(61) 2.6852(2) 1_555 2_646 ? H(35) H(62) 2.5096(1) 1_555 1_555 ? H(36) H(61) 2.8016(1) 1_555 1_555 ? H(36) H(62) 2.8528(3) 1_555 1_555 ? H(36) H(49) 3.0909(1) 1_555 1_555 ? H(36) H(48) 3.5924(4) 1_555 1_555 ? H(37) H(48) 2.5469(1) 1_555 1_555 ? H(37) H(62) 3.2624(8) 1_555 1_555 ? H(37) H(60) 3.3817(3) 1_555 1_555 ? H(37) H(61) 3.4386(4) 1_555 1_555 ? H(37) H(59) 3.5678(8) 1_555 1_555 ? H(38) H(59) 2.7133(1) 1_555 1_555 ? H(38) H(41) 3.0001(2) 1_555 1_545 ? H(38) H(43) 3.3517(1) 1_555 1_545 ? H(38) H(60) 3.4708(4) 1_555 1_555 ? H(39) H(59) 2.5494(3) 1_555 1_555 ? H(39) H(58) 2.5735(2) 1_555 1_555 ? H(39) H(60) 2.9637(7) 1_555 1_555 ? H(45) H(65) 3.0629(6) 1_555 2_656 ? H(45) H(90) 3.1935(1) 1_555 2_646 ? H(45) H(64) 3.283(1) 1_555 2_656 ? H(46) H(63) 2.8036(4) 1_555 2_656 ? H(46) H(62) 2.894(1) 1_555 2_656 ? H(46) H(64) 3.4731(6) 1_555 2_656 ? H(46) H(77) 3.5262(1) 1_555 2_656 ? H(46) H(65) 3.5902(2) 1_555 2_656 ? H(46) H(91) 3.5929(2) 1_555 2_656 ? H(50) H(53) 2.7212(1) 1_555 1_545 ? H(51) H(89) 2.9806(1) 1_555 1_545 ? H(51) H(76) 3.0650(6) 1_555 1_555 ? H(51) H(75) 3.0740(2) 1_555 1_555 ? H(51) H(90) 3.1877(5) 1_555 1_555 ? H(52) H(89) 2.5890(4) 1_555 1_545 ? H(52) H(74) 3.1748(2) 1_555 1_555 ? H(52) H(54) 3.1990(6) 1_555 1_545 ? H(53) H(74) 3.1810(6) 1_555 1_555 ? H(53) H(64) 3.3442(4) 1_555 1_565 ? H(54) H(66) 3.2341(9) 1_555 1_565 ? H(54) H(88) 3.4057(8) 1_555 1_555 ? H(55) H(86) 2.9824(3) 1_555 2_657 ? H(55) H(87) 2.9998(5) 1_555 2_647 ? H(55) H(67) 3.1213(1) 1_555 1_565 ? H(55) H(69) 3.1624(3) 1_555 2_657 ? H(55) H(88) 3.379(1) 1_555 1_555 ? H(57) H(84) 2.6134(2) 1_555 2_657 ? H(61) H(64) 3.2421(1) 1_555 1_565 ? H(63) H(90) 3.0979(3) 1_555 1_555 ? H(63) H(91) 3.576(1) 1_555 1_555 ? H(64) H(90) 2.9559(5) 1_555 1_545 ? H(65) H(77) 2.7822(9) 1_555 1_555 ? H(65) H(78) 3.4614(8) 1_555 1_555 ? H(66) H(75) 2.5862(4) 1_555 1_545 ? H(66) H(90) 2.6941(8) 1_555 1_545 ? H(66) H(74) 2.8548(1) 1_555 1_545 ? H(66) H(89) 3.3181(1) 1_555 1_545 ? H(67) H(88) 3.2296(7) 1_555 1_545 ? H(67) H(86) 3.2508(7) 1_555 2_647 ? H(67) H(85) 3.440(1) 1_555 2_647 ? H(68) H(86) 2.6169(4) 1_555 1_555 ? H(68) H(74) 3.0346(5) 1_555 1_555 ? H(68) H(88) 3.0671(2) 1_555 1_545 ? H(68) H(89) 3.0984(7) 1_555 1_545 ? H(68) H(87) 3.1451(5) 1_555 1_545 ? H(69) H(88) 2.8965(3) 1_555 2_647 ? H(69) H(87) 2.9190(8) 1_555 2_647 ? H(69) H(86) 3.1930(5) 1_555 2_647 ? H(69) H(85) 3.333(1) 1_555 2_647 ? H(69) H(86) 3.490(1) 1_555 1_555 ? H(70) H(82) 2.6146(5) 1_555 2_747 ? H(70) H(81) 2.9363(3) 1_555 2_747 ? H(70) H(73) 3.481(1) 1_555 1_545 ? H(73) H(76) 3.0230(1) 1_555 1_565 ? H(75) H(78) 3.2773(6) 1_555 1_565 ? H(76) H(87) 3.2329(4) 1_555 1_545 ? H(77) H(90) 3.3614(3) 1_555 1_545 ? H(78) H(89) 3.312(1) 1_555 1_545 ? H(78) H(90) 3.5150(3) 1_555 1_545 ? H(79) H(81) 3.0325(5) 1_555 2_757 ? H(80) H(82) 2.6040(8) 1_555 2_747 ? H(80) H(81) 3.3924(4) 1_555 2_747 ? H(84) H(87) 3.0978(1) 1_555 1_545 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_5-CN-C-ZMEPO-M #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 5 15:18:55 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 261.36 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H23 N O2 ' _chemical_formula_moiety 'C16 H23 N O2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 16.025(6) _cell_length_b 5.876(6) _cell_length_c 17.157(6) _cell_angle_alpha 90 _cell_angle_beta 112.60(2) _cell_angle_gamma 90 _cell_volume 1491(1) _cell_formula_units_Z 4 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 568.00 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.91 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 4 0 -4 1 1 -2 2 1 0 _diffrn_reflns_number 3542 _reflns_number_total 3422 _reflns_number_gt 2434 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_av_sigmaI/netI 0.041 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.06191 _diffrn_orient_matrix_UB_12 0.03191 _diffrn_orient_matrix_UB_13 0.00155 _diffrn_orient_matrix_UB_21 -0.02462 _diffrn_orient_matrix_UB_22 0.00304 _diffrn_orient_matrix_UB_23 -0.06311 _diffrn_orient_matrix_UB_31 -0.01137 _diffrn_orient_matrix_UB_32 0.16713 _diffrn_orient_matrix_UB_33 0.00085 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.0486(2) 0.3513(6) -0.7751(2) 0.0597(9) Uiso 1.00 d . . . O(2) O -0.0686(2) -0.1310(6) -0.6218(2) 0.0571(8) Uiso 1.00 d . . . N(2) N -0.1172(3) -0.3461(8) -1.0258(3) 0.072(1) Uiso 1.00 d . . . C(1) C 0.1651(3) -0.0318(9) -0.6851(3) 0.056(1) Uiso 1.00 d . . . C(2) C 0.1225(3) -0.0043(7) -0.7678(3) 0.0448(9) Uiso 1.00 d . . . C(3) C 0.0489(3) 0.1648(7) -0.8057(2) 0.0402(9) Uiso 1.00 d . . . C(4) C -0.0300(3) 0.0972(8) -0.8861(3) 0.0428(9) Uiso 1.00 d . . . C(5) C -0.0743(2) -0.1343(7) -0.8819(2) 0.0350(8) Uiso 1.00 d . . . C(6) C -0.1586(2) -0.1190(7) -0.8577(2) 0.0375(8) Uiso 1.00 d . . . C(7) C -0.1334(3) 0.0072(8) -0.7734(3) 0.0445(9) Uiso 1.00 d . . . C(8) C -0.0559(3) -0.0901(7) -0.6998(3) 0.0425(9) Uiso 1.00 d . . . C(9) C -0.0037(3) 0.0402(8) -0.6231(3) 0.048(1) Uiso 1.00 d . . . C(10) C 0.0937(4) -0.0173(10) -0.5750(3) 0.060(1) Uiso 1.00 d . . . C(11) C 0.1564(4) 0.095(1) -0.6124(3) 0.063(1) Uiso 1.00 d . . . C(12) C 0.1476(4) -0.151(1) -0.8281(4) 0.064(1) Uiso 1.00 d . . . C(13) C -0.0987(3) -0.2546(8) -0.9627(3) 0.0473(10) Uiso 1.00 d . . . C(14) C -0.2369(3) 0.0056(9) -0.9261(3) 0.054(1) Uiso 1.00 d . . . C(15) C -0.1889(3) -0.3626(9) -0.8491(3) 0.052(1) Uiso 1.00 d . . . C(16) C -0.0319(4) 0.2788(10) -0.6119(4) 0.062(1) Uiso 1.00 d . . . H(1) H 0.207(3) -0.161(9) -0.668(3) 0.09(2) Uiso 1.00 calc . . . H(2) H -0.071(2) 0.221(7) -0.897(2) 0.04(1) Uiso 1.00 calc . . . H(3) H -0.004(3) 0.075(9) -0.927(3) 0.08(2) Uiso 1.00 calc . . . H(4) H -0.033(2) -0.233(6) -0.844(2) 0.035(10) Uiso 1.00 calc . . . H(5) H -0.192(3) 0.001(8) -0.764(3) 0.07(1) Uiso 1.00 calc . . . H(6) H -0.118(3) 0.155(8) -0.778(2) 0.05(1) Uiso 1.00 calc . . . H(7) H -0.020(2) -0.224(7) -0.712(2) 0.04(1) Uiso 1.00 calc . . . H(8) H 0.142(2) 0.240(7) -0.626(2) 0.034(10) Uiso 1.00 calc . . . H(9) H 0.225(4) 0.114(10) -0.565(3) 0.10(2) Uiso 1.00 calc . . . H(10) H 0.156(4) -0.058(10) -0.863(3) 0.09(2) Uiso 1.00 calc . . . H(11) H 0.191(3) -0.255(9) -0.794(3) 0.08(2) Uiso 1.00 calc . . . H(12) H 0.105(3) -0.251(8) -0.865(3) 0.06(1) Uiso 1.00 calc . . . H(13) H -0.143(3) -0.430(7) -0.807(3) 0.05(1) Uiso 1.00 calc . . . H(14) H -0.208(3) -0.440(8) -0.903(3) 0.07(1) Uiso 1.00 calc . . . H(15) H -0.252(3) -0.065(7) -0.979(3) 0.05(1) Uiso 1.00 calc . . . H(16) H -0.279(3) 0.016(9) -0.907(3) 0.08(2) Uiso 1.00 calc . . . H(17) H -0.218(3) 0.158(9) -0.936(3) 0.07(2) Uiso 1.00 calc . . . H(18) H -0.096(3) 0.303(7) -0.640(3) 0.05(1) Uiso 1.00 calc . . . H(19) H 0.004(3) 0.379(9) -0.624(3) 0.07(2) Uiso 1.00 calc . . . H(20) H 0.112(4) 0.04(1) -0.513(4) 0.11(2) Uiso 1.00 calc . . . H(21) H 0.101(3) -0.176(8) -0.576(3) 0.06(1) Uiso 1.00 calc . . . H(22) H -0.006(5) 0.31(1) -0.551(5) 0.16(3) Uiso 1.00 calc . . . H(23) H -0.242(4) -0.35(1) -0.834(3) 0.10(2) Uiso 1.00 calc . . . 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 #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 2434 _refine_ls_number_parameters 169 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.1015 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0852 _refine_ls_wR_factor_gt 0.0852 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 4.267 _refine_ls_shift/su_max 0.1530 _refine_ls_shift/su_mean 0.0180 _refine_diff_density_min -0.57 _refine_diff_density_max 0.49 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.215(5) 1_555 1_555 yes O(2) C(8) 1.448(5) 1_555 1_555 yes O(2) C(9) 1.453(5) 1_555 1_555 yes N(2) C(13) 1.141(6) 1_555 1_555 yes C(1) C(2) 1.327(6) 1_555 1_555 yes C(1) C(11) 1.506(7) 1_555 1_555 yes C(1) H(1) 0.98(5) 1_555 1_555 no C(2) C(3) 1.486(6) 1_555 1_555 yes C(2) C(12) 1.515(7) 1_555 1_555 yes C(3) C(4) 1.523(5) 1_555 1_555 yes C(4) C(5) 1.549(6) 1_555 1_555 yes C(4) H(2) 0.95(4) 1_555 1_555 no C(4) H(3) 0.95(5) 1_555 1_555 no C(5) C(6) 1.562(5) 1_555 1_555 yes C(5) C(13) 1.469(6) 1_555 1_555 yes C(5) H(4) 0.94(4) 1_555 1_555 no C(6) C(7) 1.534(5) 1_555 1_555 yes C(6) C(14) 1.535(6) 1_555 1_555 yes C(6) C(15) 1.537(6) 1_555 1_555 yes C(7) C(8) 1.504(6) 1_555 1_555 yes C(7) H(5) 1.01(4) 1_555 1_555 no C(7) H(6) 0.92(4) 1_555 1_555 no C(8) C(9) 1.474(6) 1_555 1_555 yes C(8) H(7) 1.04(4) 1_555 1_555 no C(9) C(10) 1.497(6) 1_555 1_555 yes C(9) C(16) 1.508(7) 1_555 1_555 yes C(10) C(11) 1.534(7) 1_555 1_555 yes C(10) H(20) 1.05(6) 1_555 1_555 no C(10) H(21) 0.94(5) 1_555 1_555 no C(11) H(8) 0.89(4) 1_555 1_555 no C(11) H(9) 1.10(5) 1_555 1_555 no C(12) H(10) 0.86(6) 1_555 1_555 no C(12) H(11) 0.94(5) 1_555 1_555 no C(12) H(12) 0.94(5) 1_555 1_555 no C(14) H(15) 0.95(4) 1_555 1_555 no C(14) H(16) 0.86(5) 1_555 1_555 no C(14) H(17) 0.98(5) 1_555 1_555 no C(15) H(13) 0.90(4) 1_555 1_555 no C(15) H(14) 0.97(5) 1_555 1_555 no C(15) H(23) 0.98(6) 1_555 1_555 no C(16) H(18) 0.96(4) 1_555 1_555 no C(16) H(19) 0.91(5) 1_555 1_555 no C(16) H(22) 0.99(7) 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(8) O(2) C(9) 61.1(3) 1_555 1_555 1_555 yes C(2) C(1) C(11) 130.7(5) 1_555 1_555 1_555 yes C(2) C(1) H(1) 115(3) 1_555 1_555 1_555 no C(11) C(1) H(1) 113(3) 1_555 1_555 1_555 no C(1) C(2) C(3) 123.0(4) 1_555 1_555 1_555 yes C(1) C(2) C(12) 119.9(4) 1_555 1_555 1_555 yes C(3) C(2) C(12) 117.1(4) 1_555 1_555 1_555 yes O(1) C(3) C(2) 123.3(4) 1_555 1_555 1_555 yes O(1) C(3) C(4) 119.1(4) 1_555 1_555 1_555 yes C(2) C(3) C(4) 117.7(4) 1_555 1_555 1_555 yes C(3) C(4) C(5) 115.0(3) 1_555 1_555 1_555 yes C(3) C(4) H(2) 104(2) 1_555 1_555 1_555 no C(3) C(4) H(3) 104(2) 1_555 1_555 1_555 no C(5) C(4) H(2) 113(2) 1_555 1_555 1_555 no C(5) C(4) H(3) 104(3) 1_555 1_555 1_555 no H(2) C(4) H(3) 114(3) 1_555 1_555 1_555 no C(4) C(5) C(6) 114.9(3) 1_555 1_555 1_555 yes C(4) C(5) C(13) 109.8(3) 1_555 1_555 1_555 yes C(4) C(5) H(4) 111(2) 1_555 1_555 1_555 no C(6) C(5) C(13) 109.6(3) 1_555 1_555 1_555 yes C(6) C(5) H(4) 107(2) 1_555 1_555 1_555 no C(13) C(5) H(4) 102(2) 1_555 1_555 1_555 no C(5) C(6) C(7) 109.7(3) 1_555 1_555 1_555 yes C(5) C(6) C(14) 111.1(3) 1_555 1_555 1_555 yes C(5) C(6) C(15) 108.0(3) 1_555 1_555 1_555 yes C(7) C(6) C(14) 109.4(4) 1_555 1_555 1_555 yes C(7) C(6) C(15) 109.8(3) 1_555 1_555 1_555 yes C(14) C(6) C(15) 108.8(4) 1_555 1_555 1_555 yes C(6) C(7) C(8) 116.2(4) 1_555 1_555 1_555 yes C(6) C(7) H(5) 101(2) 1_555 1_555 1_555 no C(6) C(7) H(6) 111(2) 1_555 1_555 1_555 no C(8) C(7) H(5) 111(2) 1_555 1_555 1_555 no C(8) C(7) H(6) 105(2) 1_555 1_555 1_555 no H(5) C(7) H(6) 110(3) 1_555 1_555 1_555 no O(2) C(8) C(7) 118.4(3) 1_555 1_555 1_555 yes O(2) C(8) C(9) 59.7(3) 1_555 1_555 1_555 yes O(2) C(8) H(7) 109(2) 1_555 1_555 1_555 no C(7) C(8) C(9) 123.7(4) 1_555 1_555 1_555 yes C(7) C(8) H(7) 117(2) 1_555 1_555 1_555 no C(9) C(8) H(7) 113(2) 1_555 1_555 1_555 no O(2) C(9) C(8) 59.3(3) 1_555 1_555 1_555 yes O(2) C(9) C(10) 115.9(4) 1_555 1_555 1_555 yes O(2) C(9) C(16) 113.0(4) 1_555 1_555 1_555 yes C(8) C(9) C(10) 119.2(4) 1_555 1_555 1_555 yes C(8) C(9) C(16) 120.1(4) 1_555 1_555 1_555 yes C(10) C(9) C(16) 116.1(4) 1_555 1_555 1_555 yes C(9) C(10) C(11) 112.6(4) 1_555 1_555 1_555 yes C(9) C(10) H(20) 108(3) 1_555 1_555 1_555 no C(9) C(10) H(21) 108(2) 1_555 1_555 1_555 no C(11) C(10) H(20) 108(3) 1_555 1_555 1_555 no C(11) C(10) H(21) 108(2) 1_555 1_555 1_555 no H(20) C(10) H(21) 109(4) 1_555 1_555 1_555 no C(1) C(11) C(10) 114.6(5) 1_555 1_555 1_555 yes C(1) C(11) H(8) 111(2) 1_555 1_555 1_555 no C(1) C(11) H(9) 106(2) 1_555 1_555 1_555 no C(10) C(11) H(8) 111(2) 1_555 1_555 1_555 no C(10) C(11) H(9) 111(2) 1_555 1_555 1_555 no H(8) C(11) H(9) 100(3) 1_555 1_555 1_555 no C(2) C(12) H(10) 105(3) 1_555 1_555 1_555 no C(2) C(12) H(11) 106(3) 1_555 1_555 1_555 no C(2) C(12) H(12) 119(2) 1_555 1_555 1_555 no H(10) C(12) H(11) 124(4) 1_555 1_555 1_555 no H(10) C(12) H(12) 101(4) 1_555 1_555 1_555 no H(11) C(12) H(12) 100(3) 1_555 1_555 1_555 no N(2) C(13) C(5) 179.2(5) 1_555 1_555 1_555 yes C(6) C(14) H(15) 110(2) 1_555 1_555 1_555 no C(6) C(14) H(16) 105(3) 1_555 1_555 1_555 no C(6) C(14) H(17) 110(2) 1_555 1_555 1_555 no H(15) C(14) H(16) 117(3) 1_555 1_555 1_555 no H(15) C(14) H(17) 102(3) 1_555 1_555 1_555 no H(16) C(14) H(17) 109(4) 1_555 1_555 1_555 no C(6) C(15) H(13) 107(2) 1_555 1_555 1_555 no C(6) C(15) H(14) 110(2) 1_555 1_555 1_555 no C(6) C(15) H(23) 105(3) 1_555 1_555 1_555 no H(13) C(15) H(14) 115(3) 1_555 1_555 1_555 no H(13) C(15) H(23) 110(3) 1_555 1_555 1_555 no H(14) C(15) H(23) 107(3) 1_555 1_555 1_555 no C(9) C(16) H(18) 112(2) 1_555 1_555 1_555 no C(9) C(16) H(19) 109(3) 1_555 1_555 1_555 no C(9) C(16) H(22) 107(4) 1_555 1_555 1_555 no H(18) C(16) H(19) 116(3) 1_555 1_555 1_555 no H(18) C(16) H(22) 115(4) 1_555 1_555 1_555 no H(19) C(16) H(22) 94(4) 1_555 1_555 1_555 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) -36.5(7) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(12) 144.2(4) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) 128.0(4) 1_555 1_555 1_555 1_555 yes O(2) C(8) C(7) C(6) 129.3(4) 1_555 1_555 1_555 1_555 yes O(2) C(8) C(9) C(10) -104.4(5) 1_555 1_555 1_555 1_555 yes O(2) C(8) C(9) C(16) 100.4(5) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(8) C(7) -105.8(4) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(10) C(11) -150.7(4) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(5) C(4) -4(33) 1_555 1_555 1_555 1_555 yes N(2) C(13) C(5) C(6) -131(33) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 142.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(11) C(10) C(9) 83.5(6) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(11) C(10) -96.5(7) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) -51.2(5) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(11) 3.6(8) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -94.7(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(13) 141.2(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(12) -36.5(6) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 55.6(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(14) -65.5(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(15) 175.3(3) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) 56.5(5) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) -159.9(4) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(13) 179.8(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) O(2) C(9) 114.5(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) 149.8(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(16) -5.3(6) 1_555 1_555 1_555 1_555 yes C(8) O(2) C(9) C(10) 110.1(4) 1_555 1_555 1_555 1_555 yes C(8) O(2) C(9) C(16) -112.4(4) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(14) 178.6(4) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(15) -62.1(5) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -83.0(6) 1_555 1_555 1_555 1_555 yes C(11) C(1) C(2) C(12) -177.1(5) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(16) 73.1(6) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(14) 58.7(4) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(15) -60.5(4) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) H(4) 2.80(4) 1_555 1_545 ? O(1) H(7) 3.09(4) 1_555 1_545 ? O(1) H(12) 3.12(4) 1_555 1_545 ? O(1) H(13) 3.18(4) 1_555 1_545 ? O(1) H(11) 3.35(5) 1_555 1_545 ? O(2) H(20) 2.71(6) 1_555 3_556 ? O(2) H(22) 2.93(7) 1_555 3_556 ? O(2) H(19) 3.11(5) 1_555 1_565 ? O(2) H(23) 3.29(6) 1_555 2_546 ? O(2) H(18) 3.35(4) 1_555 1_565 ? O(2) H(16) 3.38(5) 1_555 2_556 ? O(2) H(22) 3.50(8) 1_555 1_565 ? O(2) C(16) 3.511(7) 1_555 1_565 ? N(2) H(9) 2.83(6) 1_555 4_555 ? N(2) H(3) 2.86(5) 1_555 3_557 ? N(2) H(1) 2.94(5) 1_555 4_555 ? N(2) H(10) 2.96(6) 1_555 3_557 ? N(2) H(12) 3.07(5) 1_555 3_567 ? N(2) H(2) 3.26(4) 1_555 1_565 ? N(2) C(4) 3.566(6) 1_555 3_557 ? N(2) C(1) 3.582(7) 1_555 4_555 ? C(1) H(11) 2.95(5) 1_555 2_446 ? C(2) H(11) 3.13(5) 1_555 2_446 ? C(4) H(3) 3.60(5) 1_555 3_557 ? C(7) H(23) 3.32(6) 1_555 2_546 ? C(7) H(13) 3.35(4) 1_555 1_545 ? C(8) H(19) 3.37(5) 1_555 1_565 ? C(9) H(20) 3.43(6) 1_555 3_556 ? C(9) H(22) 3.58(7) 1_555 3_556 ? C(10) H(14) 3.41(5) 1_555 4_454 ? C(10) H(15) 3.42(4) 1_555 4_454 ? C(10) H(22) 3.45(7) 1_555 3_556 ? C(11) H(17) 3.26(5) 1_555 4_444 ? C(11) H(11) 3.51(5) 1_555 2_446 ? C(11) H(15) 3.52(4) 1_555 4_444 ? C(11) H(14) 3.53(5) 1_555 4_454 ? C(12) H(9) 3.51(5) 1_555 2_456 ? C(12) H(11) 3.52(6) 1_555 2_446 ? C(13) H(3) 3.13(5) 1_555 3_557 ? C(13) H(2) 3.25(4) 1_555 1_565 ? C(13) H(10) 3.33(6) 1_555 3_557 ? C(13) H(9) 3.42(6) 1_555 4_555 ? C(14) H(9) 3.15(6) 1_555 4_545 ? C(14) H(14) 3.29(5) 1_555 1_545 ? C(14) H(21) 3.46(5) 1_555 4_555 ? C(14) H(18) 3.49(4) 1_555 2_556 ? C(14) H(20) 3.54(6) 1_555 4_545 ? C(14) H(8) 3.55(4) 1_555 4_545 ? C(15) H(6) 3.12(4) 1_555 1_565 ? C(15) H(17) 3.13(5) 1_555 1_565 ? C(15) H(5) 3.30(5) 1_555 2_556 ? C(15) H(2) 3.39(4) 1_555 1_565 ? C(15) H(20) 3.50(6) 1_555 4_555 ? C(15) H(18) 3.52(4) 1_555 2_556 ? C(16) H(7) 3.42(4) 1_555 1_545 ? C(16) H(20) 3.43(6) 1_555 3_556 ? C(16) H(16) 3.46(5) 1_555 2_546 ? C(16) H(23) 3.46(6) 1_555 2_546 ? C(16) H(22) 3.55(8) 1_555 3_546 ? C(16) H(13) 3.57(4) 1_555 1_545 ? H(1) H(11) 3.10(7) 1_555 2_446 ? H(1) H(10) 3.11(8) 1_555 2_456 ? H(1) H(15) 3.44(7) 1_555 4_454 ? H(2) H(14) 2.95(6) 1_555 1_545 ? H(2) H(13) 3.06(6) 1_555 1_545 ? H(2) H(4) 3.33(5) 1_555 1_545 ? H(2) H(9) 3.56(7) 1_555 4_545 ? H(3) H(3) 2.71(10) 1_555 3_557 ? H(3) H(12) 3.46(7) 1_555 3_557 ? H(3) H(10) 3.49(7) 1_555 3_557 ? H(5) H(13) 3.33(6) 1_555 2_546 ? H(5) H(18) 3.36(6) 1_555 2_556 ? H(5) H(13) 3.57(6) 1_555 1_545 ? H(6) H(14) 3.16(6) 1_555 1_545 ? H(6) H(23) 3.46(7) 1_555 1_545 ? H(6) H(23) 3.48(7) 1_555 2_546 ? H(7) H(19) 2.71(6) 1_555 1_565 ? H(7) H(18) 3.44(6) 1_555 1_565 ? H(8) H(15) 3.09(5) 1_555 4_444 ? H(8) H(17) 3.23(6) 1_555 4_444 ? H(8) H(11) 3.45(6) 1_555 2_446 ? H(8) H(10) 3.53(6) 1_555 2_446 ? H(9) H(14) 2.76(7) 1_555 4_454 ? H(9) H(15) 2.98(7) 1_555 4_444 ? H(9) H(10) 3.27(8) 1_555 2_446 ? H(9) H(11) 3.28(7) 1_555 2_446 ? H(9) H(12) 3.47(7) 1_555 2_446 ? H(9) H(16) 3.50(7) 1_555 4_444 ? H(9) H(15) 3.50(7) 1_555 4_454 ? H(10) H(11) 3.37(8) 1_555 2_446 ? H(11) H(11) 3.51(6) 1_555 2_456 ? H(11) H(11) 3.51(6) 1_555 2_446 ? H(13) H(18) 3.09(6) 1_555 1_565 ? H(13) H(17) 3.18(6) 1_555 1_565 ? H(13) H(19) 3.31(6) 1_555 1_565 ? H(14) H(20) 2.83(7) 1_555 4_555 ? H(14) H(16) 3.38(7) 1_555 1_565 ? H(14) H(21) 3.41(6) 1_555 4_555 ? H(15) H(21) 2.76(6) 1_555 4_555 ? H(15) H(20) 3.45(7) 1_555 4_555 ? H(16) H(18) 2.73(7) 1_555 2_556 ? H(16) H(20) 3.28(8) 1_555 4_545 ? H(16) H(21) 3.44(7) 1_555 4_555 ? H(16) H(22) 3.44(9) 1_555 2_556 ? H(17) H(20) 3.09(8) 1_555 4_545 ? H(17) H(23) 3.48(8) 1_555 1_545 ? H(18) H(23) 2.61(7) 1_555 2_546 ? H(18) H(20) 3.39(7) 1_555 3_556 ? H(19) H(21) 2.99(7) 1_555 1_545 ? H(19) H(22) 3.49(9) 1_555 3_546 ? H(20) H(22) 3.11(10) 1_555 3_556 ? H(20) H(23) 3.26(8) 1_555 4_454 ? H(21) H(22) 3.19(8) 1_555 3_556 ? H(21) H(22) 3.57(9) 1_555 1_565 ? H(22) H(22) 2.8(2) 1_555 3_546 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_z-5_8-thf #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 5 15:20:48 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 522.73 _chemical_formula_analytical ? _chemical_formula_sum 'C32 H46 N2 O4 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 8.090(4) _cell_length_b 39.650(8) _cell_length_c 9.371(2) _cell_angle_alpha 90.00(2) _cell_angle_beta 89.99(3) _cell_angle_gamma 90.17(3) _cell_volume 3006(1) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 2.310 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2272.00 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -1.37 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 1 -1 1 -3 -1 1 -5 -1 _diffrn_reflns_number 7377 _reflns_number_total 6886 _reflns_number_gt 4887 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.035 _diffrn_reflns_av_sigmaI/netI 0.035 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -51 _diffrn_reflns_limit_k_max 51 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 0.02153 _diffrn_orient_matrix_UB_12 -0.01510 _diffrn_orient_matrix_UB_13 -0.08339 _diffrn_orient_matrix_UB_21 -0.05485 _diffrn_orient_matrix_UB_22 0.01663 _diffrn_orient_matrix_UB_23 -0.06461 _diffrn_orient_matrix_UB_31 0.10866 _diffrn_orient_matrix_UB_32 0.01147 _diffrn_orient_matrix_UB_33 -0.01611 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 1.5531(4) 0.10727(8) 1.1936(3) 0.0750(10) Uani 1.00 d . . . O(2) O 1.1748(3) 0.12220(6) 0.9289(2) 0.0417(6) Uani 1.00 d . . . O(3) O 0.6970(4) 0.14276(8) 0.6936(3) 0.0755(9) Uani 1.00 d . . . O(4) O 1.0750(3) 0.12777(6) 0.4287(2) 0.0419(6) Uani 1.00 d . . . N(1) N 1.6647(6) 0.0120(1) 1.2080(7) 0.124(2) Uani 1.00 d . . . N(2) N 0.5854(6) 0.2381(1) 0.7076(7) 0.122(2) Uani 1.00 d . . . C(1) C 1.3322(4) 0.11963(9) 0.8560(3) 0.0422(9) Uani 1.00 d . . . C(2) C 1.4766(4) 0.12310(9) 0.9602(3) 0.0396(9) Uani 1.00 d . . . C(3) C 1.4721(4) 0.10014(9) 1.0902(3) 0.0381(8) Uani 1.00 d . . . C(4) C 1.3681(4) 0.06809(8) 1.0902(3) 0.0330(8) Uani 1.00 d . . . C(5) C 1.3944(4) 0.04708(9) 1.2261(4) 0.0429(9) Uani 1.00 d . . . C(6) C 1.2310(5) 0.02656(10) 1.2517(4) 0.054(1) Uani 1.00 d . . . C(7) C 1.1125(5) 0.0400(1) 1.1370(5) 0.059(1) Uani 1.00 d . . . C(8) C 1.1798(4) 0.07437(9) 1.0896(3) 0.0374(8) Uani 1.00 d . . . C(9) C 1.1077(4) 0.08846(9) 0.9504(3) 0.0400(9) Uani 1.00 d . . . C(10) C 1.1632(5) 0.0694(1) 0.8154(4) 0.049(1) Uani 1.00 d . . . C(11) C 1.3241(5) 0.0869(1) 0.7688(4) 0.051(1) Uani 1.00 d . . . C(12) C 1.4992(5) 0.1598(1) 1.0074(5) 0.060(1) Uani 1.00 d . . . C(13) C 1.5461(6) 0.0270(1) 1.2174(5) 0.070(1) Uani 1.00 d . . . C(14) C 1.2560(8) -0.0116(1) 1.2349(9) 0.108(2) Uani 1.00 d . . . C(15) C 1.1647(7) 0.0352(2) 1.4016(5) 0.093(2) Uani 1.00 d . . . C(16) C 0.9213(4) 0.0924(1) 0.9603(4) 0.056(1) Uani 1.00 d . . . C(17) C 0.9184(4) 0.13034(9) 0.3560(3) 0.0423(9) Uani 1.00 d . . . C(18) C 0.7730(4) 0.12692(9) 0.4600(3) 0.0395(9) Uani 1.00 d . . . C(19) C 0.7782(4) 0.14992(9) 0.5902(3) 0.0386(8) Uani 1.00 d . . . C(20) C 0.8819(4) 0.18193(8) 0.5903(3) 0.0330(8) Uani 1.00 d . . . C(21) C 0.8555(4) 0.20290(9) 0.7262(4) 0.0428(9) Uani 1.00 d . . . C(22) C 1.0185(5) 0.22341(10) 0.7520(4) 0.054(1) Uani 1.00 d . . . C(23) C 1.1378(5) 0.2100(1) 0.6369(4) 0.059(1) Uani 1.00 d . . . C(24) C 1.0697(4) 0.17562(9) 0.5898(3) 0.0373(8) Uani 1.00 d . . . C(25) C 1.1423(4) 0.16157(9) 0.4501(3) 0.0402(9) Uani 1.00 d . . . C(26) C 1.0866(5) 0.1806(1) 0.3156(4) 0.049(1) Uani 1.00 d . . . C(27) C 0.9262(5) 0.1631(1) 0.2689(4) 0.051(1) Uani 1.00 d . . . C(28) C 0.7511(5) 0.0902(1) 0.5072(5) 0.060(1) Uani 1.00 d . . . C(29) C 0.7044(6) 0.2229(1) 0.7177(5) 0.070(1) Uani 1.00 d . . . C(30) C 1.0852(7) 0.2147(2) 0.9015(5) 0.094(2) Uani 1.00 d . . . C(31) C 0.9929(8) 0.2616(1) 0.7353(9) 0.109(2) Uani 1.00 d . . . C(32) C 1.3288(4) 0.1577(1) 0.4605(4) 0.057(1) Uani 1.00 d . . . H(1) H 1.3392 0.1382 0.7893 0.040(9) Uiso 1.00 calc . . . H(2) H 1.5751 0.1174 0.9078 0.042(9) Uiso 1.00 calc . . . H(3) H 1.3968 0.0544 1.0089 0.039(9) Uiso 1.00 calc . . . H(4) H 1.4069 0.0628 1.3046 0.05(1) Uiso 1.00 calc . . . H(5) H 1.1077 0.0248 1.0566 0.08(1) Uiso 1.00 calc . . . H(6) H 1.0018 0.0420 1.1736 0.07(1) Uiso 1.00 calc . . . H(7) H 1.1566 0.0902 1.1647 0.039(9) Uiso 1.00 calc . . . H(8) H 1.1813 0.0458 0.8357 0.05(1) Uiso 1.00 calc . . . H(9) H 1.0809 0.0706 0.7417 0.06(1) Uiso 1.00 calc . . . H(10) H 1.3240 0.0912 0.6682 0.07(1) Uiso 1.00 calc . . . H(11) H 1.4183 0.0728 0.7893 0.05(1) Uiso 1.00 calc . . . H(12) H 1.5944 0.1621 1.0660 0.08(1) Uiso 1.00 calc . . . H(13) H 1.5106 0.1742 0.9263 0.08(1) Uiso 1.00 calc . . . H(14) H 1.4042 0.1669 1.0605 0.07(1) Uiso 1.00 calc . . . H(15) H 1.1551 -0.0238 1.2414 0.17(3) Uiso 1.00 calc . . . H(16) H 1.3048 -0.0166 1.1424 0.13(2) Uiso 1.00 calc . . . H(17) H 1.3309 -0.0202 1.3057 0.15(3) Uiso 1.00 calc . . . H(18) H 1.2450 0.0297 1.4745 0.10(2) Uiso 1.00 calc . . . H(19) H 1.1416 0.0589 1.4104 0.16(3) Uiso 1.00 calc . . . H(20) H 1.0654 0.0231 1.4233 0.15(2) Uiso 1.00 calc . . . H(21) H 0.8921 0.1068 1.0371 0.07(1) Uiso 1.00 calc . . . H(22) H 0.8788 0.1016 0.8735 0.07(1) Uiso 1.00 calc . . . H(23) H 0.8697 0.0708 0.9752 0.07(1) Uiso 1.00 calc . . . H(24) H 0.9116 0.1118 0.2892 0.038(9) Uiso 1.00 calc . . . H(25) H 0.6744 0.1326 0.4074 0.037(9) Uiso 1.00 calc . . . H(26) H 0.8533 0.1956 0.5085 0.035(8) Uiso 1.00 calc . . . H(27) H 0.8430 0.1872 0.8048 0.05(1) Uiso 1.00 calc . . . H(28) H 1.1426 0.2252 0.5566 0.07(1) Uiso 1.00 calc . . . H(29) H 1.2485 0.2080 0.6736 0.08(1) Uiso 1.00 calc . . . H(30) H 1.0930 0.1597 0.6648 0.037(9) Uiso 1.00 calc . . . H(31) H 1.0679 0.2042 0.3367 0.05(1) Uiso 1.00 calc . . . H(32) H 1.1691 0.1796 0.2424 0.06(1) Uiso 1.00 calc . . . H(33) H 0.9270 0.1587 0.1684 0.07(1) Uiso 1.00 calc . . . H(34) H 0.8319 0.1770 0.2892 0.05(1) Uiso 1.00 calc . . . H(35) H 0.6557 0.0878 0.5664 0.09(2) Uiso 1.00 calc . . . H(36) H 0.7396 0.0756 0.4268 0.08(1) Uiso 1.00 calc . . . H(37) H 0.8459 0.0832 0.5608 0.07(1) Uiso 1.00 calc . . . H(38) H 1.0060 0.2201 0.9744 0.11(2) Uiso 1.00 calc . . . H(39) H 1.1095 0.1910 0.9093 0.17(3) Uiso 1.00 calc . . . H(40) H 1.1851 0.2269 0.9225 0.13(2) Uiso 1.00 calc . . . H(41) H 1.0940 0.2738 0.7433 0.16(3) Uiso 1.00 calc . . . H(42) H 0.9464 0.2666 0.6420 0.13(2) Uiso 1.00 calc . . . H(43) H 0.9169 0.2701 0.8049 0.16(3) Uiso 1.00 calc . . . H(44) H 1.3576 0.1435 0.5389 0.07(1) Uiso 1.00 calc . . . H(45) H 1.3717 0.1480 0.3749 0.08(1) Uiso 1.00 calc . . . H(46) H 1.3806 0.1792 0.4744 0.07(1) Uiso 1.00 calc . . . 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 O(1) 0.093(2) 0.079(2) 0.052(2) -0.044(2) -0.032(1) 0.016(1) O(2) 0.038(1) 0.042(1) 0.045(1) 0.005(1) -0.0011(10) -0.004(1) O(3) 0.094(2) 0.080(2) 0.052(2) -0.045(2) 0.038(1) -0.018(1) O(4) 0.039(1) 0.042(1) 0.045(1) 0.006(1) 0.0073(10) 0.003(1) N(1) 0.080(3) 0.099(4) 0.192(6) 0.039(3) 0.009(3) 0.047(4) N(2) 0.078(3) 0.098(4) 0.190(6) 0.037(3) -0.001(3) -0.047(3) C(1) 0.045(2) 0.048(2) 0.033(2) 0.001(2) 0.003(1) 0.005(1) C(2) 0.034(2) 0.046(2) 0.038(2) -0.003(1) 0.008(1) 0.004(1) C(3) 0.032(2) 0.044(2) 0.039(2) -0.003(1) 0.001(1) 0.001(1) C(4) 0.030(1) 0.035(2) 0.033(2) 0.001(1) 0.001(1) 0.000(1) C(5) 0.047(2) 0.040(2) 0.041(2) -0.002(1) -0.003(1) 0.005(1) C(6) 0.058(2) 0.046(2) 0.059(2) -0.011(2) 0.006(2) 0.011(2) C(7) 0.048(2) 0.064(3) 0.065(2) -0.022(2) 0.003(2) 0.010(2) C(8) 0.029(1) 0.046(2) 0.037(2) -0.002(1) 0.002(1) -0.002(1) C(9) 0.030(2) 0.049(2) 0.041(2) 0.002(1) -0.004(1) -0.008(1) C(10) 0.047(2) 0.058(2) 0.041(2) 0.002(2) -0.007(2) -0.014(2) C(11) 0.058(2) 0.062(2) 0.031(2) 0.003(2) 0.005(2) -0.005(2) C(12) 0.063(3) 0.047(2) 0.069(3) -0.014(2) -0.002(2) 0.002(2) C(13) 0.060(3) 0.059(3) 0.089(3) 0.006(2) -0.005(2) 0.025(2) C(14) 0.106(5) 0.047(3) 0.172(7) -0.021(3) -0.005(5) 0.011(3) C(15) 0.085(4) 0.138(5) 0.057(3) -0.010(4) 0.018(3) 0.022(3) C(16) 0.029(2) 0.075(3) 0.063(2) 0.005(2) -0.007(2) -0.014(2) C(17) 0.046(2) 0.048(2) 0.033(2) 0.001(2) 0.002(1) -0.006(1) C(18) 0.034(2) 0.047(2) 0.038(2) -0.004(1) -0.002(1) -0.005(1) C(19) 0.032(2) 0.044(2) 0.039(2) -0.004(1) 0.004(1) -0.002(1) C(20) 0.032(1) 0.035(2) 0.032(1) 0.001(1) 0.004(1) 0.000(1) C(21) 0.048(2) 0.040(2) 0.041(2) -0.001(1) 0.007(1) -0.005(1) C(22) 0.058(2) 0.047(2) 0.058(2) -0.011(2) 0.000(2) -0.012(2) C(23) 0.047(2) 0.064(3) 0.065(2) -0.022(2) 0.004(2) -0.011(2) C(24) 0.029(1) 0.047(2) 0.036(2) -0.003(1) 0.003(1) 0.002(1) C(25) 0.030(2) 0.049(2) 0.041(2) 0.002(1) 0.009(1) 0.008(1) C(26) 0.048(2) 0.058(2) 0.040(2) 0.002(2) 0.012(2) 0.013(2) C(27) 0.058(2) 0.064(2) 0.031(2) 0.005(2) 0.000(2) 0.005(2) C(28) 0.062(2) 0.047(2) 0.069(3) -0.015(2) 0.008(2) -0.004(2) C(29) 0.062(3) 0.058(3) 0.088(3) 0.006(2) 0.009(2) -0.025(2) C(30) 0.086(4) 0.136(5) 0.058(3) -0.011(4) -0.013(3) -0.025(3) C(31) 0.105(5) 0.047(3) 0.174(7) -0.022(3) 0.013(5) -0.015(3) C(32) 0.031(2) 0.076(3) 0.063(2) 0.005(2) 0.012(2) 0.015(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 4887 _refine_ls_number_parameters 389 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 4.503 _refine_ls_shift/su_max 0.0010 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_min -0.12 _refine_diff_density_max 0.09 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.203(4) 1_555 1_555 yes O(2) C(1) 1.449(4) 1_555 1_555 yes O(2) C(9) 1.457(4) 1_555 1_555 yes O(3) C(19) 1.204(4) 1_555 1_555 yes O(4) C(17) 1.442(4) 1_555 1_555 yes O(4) C(25) 1.459(4) 1_555 1_555 yes N(1) C(13) 1.133(6) 1_555 1_555 yes N(2) C(29) 1.139(6) 1_555 1_555 yes C(1) C(2) 1.528(5) 1_555 1_555 yes C(1) C(11) 1.537(5) 1_555 1_555 yes C(1) H(1) 0.968(3) 1_555 1_555 no C(2) C(3) 1.521(4) 1_555 1_555 yes C(2) C(12) 1.530(5) 1_555 1_555 yes C(2) H(2) 0.964(3) 1_555 1_555 no C(3) C(4) 1.522(4) 1_555 1_555 yes C(4) C(5) 1.536(4) 1_555 1_555 yes C(4) C(8) 1.544(4) 1_555 1_555 yes C(4) H(3) 0.964(3) 1_555 1_555 no C(5) C(6) 1.569(5) 1_555 1_555 yes C(5) C(13) 1.467(6) 1_555 1_555 yes C(5) H(4) 0.970(4) 1_555 1_555 no C(6) C(7) 1.536(6) 1_555 1_555 yes C(6) C(14) 1.536(7) 1_555 1_555 yes C(6) C(15) 1.543(6) 1_555 1_555 yes C(7) C(8) 1.532(5) 1_555 1_555 yes C(7) H(5) 0.966(4) 1_555 1_555 no C(7) H(6) 0.962(4) 1_555 1_555 no C(8) C(9) 1.535(4) 1_555 1_555 yes C(8) H(7) 0.963(3) 1_555 1_555 no C(9) C(10) 1.542(5) 1_555 1_555 yes C(9) C(16) 1.519(5) 1_555 1_555 yes C(10) C(11) 1.537(5) 1_555 1_555 yes C(10) H(8) 0.966(4) 1_555 1_555 no C(10) H(9) 0.961(4) 1_555 1_555 no C(11) H(10) 0.958(3) 1_555 1_555 no C(11) H(11) 0.965(4) 1_555 1_555 no C(12) H(12) 0.951(4) 1_555 1_555 no C(12) H(13) 0.957(4) 1_555 1_555 no C(12) H(14) 0.958(4) 1_555 1_555 no C(14) H(15) 0.949(6) 1_555 1_555 no C(14) H(16) 0.973(8) 1_555 1_555 no C(14) H(17) 0.961(7) 1_555 1_555 no C(15) H(18) 0.968(6) 1_555 1_555 no C(15) H(19) 0.963(7) 1_555 1_555 no C(15) H(20) 0.956(6) 1_555 1_555 no C(16) H(21) 0.951(4) 1_555 1_555 no C(16) H(22) 0.957(4) 1_555 1_555 no C(16) H(23) 0.960(4) 1_555 1_555 no C(17) C(18) 1.534(4) 1_555 1_555 yes C(17) C(27) 1.534(5) 1_555 1_555 yes C(17) H(24) 0.967(3) 1_555 1_555 no C(18) C(19) 1.523(4) 1_555 1_555 yes C(18) C(28) 1.530(5) 1_555 1_555 yes C(18) H(25) 0.965(3) 1_555 1_555 no C(19) C(20) 1.520(4) 1_555 1_555 yes C(20) C(21) 1.537(4) 1_555 1_555 yes C(20) C(24) 1.541(4) 1_555 1_555 yes C(20) H(26) 0.967(3) 1_555 1_555 no C(21) C(22) 1.566(5) 1_555 1_555 yes C(21) C(29) 1.462(6) 1_555 1_555 yes C(21) H(27) 0.971(4) 1_555 1_555 no C(22) C(23) 1.543(6) 1_555 1_555 yes C(22) C(30) 1.540(6) 1_555 1_555 yes C(22) C(31) 1.539(7) 1_555 1_555 yes C(23) C(24) 1.533(5) 1_555 1_555 yes C(23) H(28) 0.966(4) 1_555 1_555 no C(23) H(29) 0.963(4) 1_555 1_555 no C(24) C(25) 1.540(4) 1_555 1_555 yes C(24) H(30) 0.963(3) 1_555 1_555 no C(25) C(26) 1.537(5) 1_555 1_555 yes C(25) C(32) 1.520(5) 1_555 1_555 yes C(26) C(27) 1.533(5) 1_555 1_555 yes C(26) H(31) 0.969(4) 1_555 1_555 no C(26) H(32) 0.958(3) 1_555 1_555 no C(27) H(33) 0.957(3) 1_555 1_555 no C(27) H(34) 0.963(4) 1_555 1_555 no C(28) H(35) 0.955(4) 1_555 1_555 no C(28) H(36) 0.955(4) 1_555 1_555 no C(28) H(37) 0.959(5) 1_555 1_555 no C(30) H(38) 0.961(6) 1_555 1_555 no C(30) H(39) 0.965(7) 1_555 1_555 no C(30) H(40) 0.960(6) 1_555 1_555 no C(31) H(41) 0.952(6) 1_555 1_555 no C(31) H(42) 0.973(8) 1_555 1_555 no C(31) H(43) 0.957(7) 1_555 1_555 no C(32) H(44) 0.955(4) 1_555 1_555 no C(32) H(45) 0.955(4) 1_555 1_555 no C(32) H(46) 0.960(4) 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(2) C(9) 109.0(2) 1_555 1_555 1_555 yes C(17) O(4) C(25) 109.0(2) 1_555 1_555 1_555 yes O(2) C(1) C(2) 111.4(3) 1_555 1_555 1_555 yes O(2) C(1) C(11) 106.0(3) 1_555 1_555 1_555 yes O(2) C(1) H(1) 107.5(3) 1_555 1_555 1_555 no C(2) C(1) C(11) 116.5(3) 1_555 1_555 1_555 yes C(2) C(1) H(1) 107.5(3) 1_555 1_555 1_555 no C(11) C(1) H(1) 107.6(3) 1_555 1_555 1_555 no C(1) C(2) C(3) 116.2(3) 1_555 1_555 1_555 yes C(1) C(2) C(12) 111.1(3) 1_555 1_555 1_555 yes C(1) C(2) H(2) 106.6(3) 1_555 1_555 1_555 no C(3) C(2) C(12) 109.8(3) 1_555 1_555 1_555 yes C(3) C(2) H(2) 106.5(3) 1_555 1_555 1_555 no C(12) C(2) H(2) 105.9(3) 1_555 1_555 1_555 no O(1) C(3) C(2) 119.5(3) 1_555 1_555 1_555 yes O(1) C(3) C(4) 119.7(3) 1_555 1_555 1_555 yes C(2) C(3) C(4) 120.8(3) 1_555 1_555 1_555 yes C(3) C(4) C(5) 112.0(3) 1_555 1_555 1_555 yes C(3) C(4) C(8) 114.1(3) 1_555 1_555 1_555 yes C(3) C(4) H(3) 109.6(3) 1_555 1_555 1_555 no C(5) C(4) C(8) 103.2(2) 1_555 1_555 1_555 yes C(5) C(4) H(3) 108.5(3) 1_555 1_555 1_555 no C(8) C(4) H(3) 109.1(3) 1_555 1_555 1_555 no C(4) C(5) C(6) 106.8(3) 1_555 1_555 1_555 yes C(4) C(5) C(13) 111.5(3) 1_555 1_555 1_555 yes C(4) C(5) H(4) 107.1(3) 1_555 1_555 1_555 no C(6) C(5) C(13) 115.6(3) 1_555 1_555 1_555 yes C(6) C(5) H(4) 107.7(3) 1_555 1_555 1_555 no C(13) C(5) H(4) 107.8(3) 1_555 1_555 1_555 no C(5) C(6) C(7) 103.8(3) 1_555 1_555 1_555 yes C(5) C(6) C(14) 112.5(4) 1_555 1_555 1_555 yes C(5) C(6) C(15) 108.5(4) 1_555 1_555 1_555 yes C(7) C(6) C(14) 110.8(4) 1_555 1_555 1_555 yes C(7) C(6) C(15) 110.0(4) 1_555 1_555 1_555 yes C(14) C(6) C(15) 111.0(5) 1_555 1_555 1_555 yes C(6) C(7) C(8) 106.9(3) 1_555 1_555 1_555 yes C(6) C(7) H(5) 110.7(4) 1_555 1_555 1_555 no C(6) C(7) H(6) 111.2(4) 1_555 1_555 1_555 no C(8) C(7) H(5) 110.0(3) 1_555 1_555 1_555 no C(8) C(7) H(6) 111.0(4) 1_555 1_555 1_555 no H(5) C(7) H(6) 107.1(4) 1_555 1_555 1_555 no C(4) C(8) C(7) 101.8(3) 1_555 1_555 1_555 yes C(4) C(8) C(9) 116.0(3) 1_555 1_555 1_555 yes C(4) C(8) H(7) 107.3(3) 1_555 1_555 1_555 no C(7) C(8) C(9) 115.8(3) 1_555 1_555 1_555 yes C(7) C(8) H(7) 107.4(3) 1_555 1_555 1_555 no C(9) C(8) H(7) 108.0(3) 1_555 1_555 1_555 no O(2) C(9) C(8) 108.1(2) 1_555 1_555 1_555 yes O(2) C(9) C(10) 103.3(3) 1_555 1_555 1_555 yes O(2) C(9) C(16) 106.4(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 114.0(3) 1_555 1_555 1_555 yes C(8) C(9) C(16) 111.3(3) 1_555 1_555 1_555 yes C(10) C(9) C(16) 113.0(3) 1_555 1_555 1_555 yes C(9) C(10) C(11) 105.0(3) 1_555 1_555 1_555 yes C(9) C(10) H(8) 111.1(3) 1_555 1_555 1_555 no C(9) C(10) H(9) 111.2(3) 1_555 1_555 1_555 no C(11) C(10) H(8) 111.2(3) 1_555 1_555 1_555 no C(11) C(10) H(9) 111.1(3) 1_555 1_555 1_555 no H(8) C(10) H(9) 107.2(3) 1_555 1_555 1_555 no C(1) C(11) C(10) 105.3(3) 1_555 1_555 1_555 yes C(1) C(11) H(10) 111.8(4) 1_555 1_555 1_555 no C(1) C(11) H(11) 110.5(3) 1_555 1_555 1_555 no C(10) C(11) H(10) 111.1(3) 1_555 1_555 1_555 no C(10) C(11) H(11) 110.6(4) 1_555 1_555 1_555 no H(10) C(11) H(11) 107.6(3) 1_555 1_555 1_555 no C(2) C(12) H(12) 110.9(4) 1_555 1_555 1_555 no C(2) C(12) H(13) 110.5(4) 1_555 1_555 1_555 no C(2) C(12) H(14) 109.6(3) 1_555 1_555 1_555 no H(12) C(12) H(13) 108.8(4) 1_555 1_555 1_555 no H(12) C(12) H(14) 108.7(4) 1_555 1_555 1_555 no H(13) C(12) H(14) 108.2(4) 1_555 1_555 1_555 no N(1) C(13) C(5) 178.3(5) 1_555 1_555 1_555 yes C(6) C(14) H(15) 112.2(6) 1_555 1_555 1_555 no C(6) C(14) H(16) 110.3(5) 1_555 1_555 1_555 no C(6) C(14) H(17) 111.2(6) 1_555 1_555 1_555 no H(15) C(14) H(16) 107.6(7) 1_555 1_555 1_555 no H(15) C(14) H(17) 108.6(6) 1_555 1_555 1_555 no H(16) C(14) H(17) 106.6(7) 1_555 1_555 1_555 no C(6) C(15) H(18) 111.0(5) 1_555 1_555 1_555 no C(6) C(15) H(19) 111.2(4) 1_555 1_555 1_555 no C(6) C(15) H(20) 112.0(5) 1_555 1_555 1_555 no H(18) C(15) H(19) 106.9(6) 1_555 1_555 1_555 no H(18) C(15) H(20) 107.5(5) 1_555 1_555 1_555 no H(19) C(15) H(20) 107.9(6) 1_555 1_555 1_555 no C(9) C(16) H(21) 110.9(3) 1_555 1_555 1_555 no C(9) C(16) H(22) 110.2(4) 1_555 1_555 1_555 no C(9) C(16) H(23) 110.3(4) 1_555 1_555 1_555 no H(21) C(16) H(22) 108.8(4) 1_555 1_555 1_555 no H(21) C(16) H(23) 108.5(4) 1_555 1_555 1_555 no H(22) C(16) H(23) 108.1(4) 1_555 1_555 1_555 no O(4) C(17) C(18) 111.5(3) 1_555 1_555 1_555 yes O(4) C(17) C(27) 106.1(3) 1_555 1_555 1_555 yes O(4) C(17) H(24) 107.5(3) 1_555 1_555 1_555 no C(18) C(17) C(27) 116.3(3) 1_555 1_555 1_555 yes C(18) C(17) H(24) 107.5(3) 1_555 1_555 1_555 no C(27) C(17) H(24) 107.6(3) 1_555 1_555 1_555 no C(17) C(18) C(19) 115.8(3) 1_555 1_555 1_555 yes C(17) C(18) C(28) 110.7(3) 1_555 1_555 1_555 yes C(17) C(18) H(25) 106.8(3) 1_555 1_555 1_555 no C(19) C(18) C(28) 109.9(3) 1_555 1_555 1_555 yes C(19) C(18) H(25) 106.9(3) 1_555 1_555 1_555 no C(28) C(18) H(25) 106.1(3) 1_555 1_555 1_555 no O(3) C(19) C(18) 119.2(3) 1_555 1_555 1_555 yes O(3) C(19) C(20) 119.7(3) 1_555 1_555 1_555 yes C(18) C(19) C(20) 121.0(3) 1_555 1_555 1_555 yes C(19) C(20) C(21) 112.0(3) 1_555 1_555 1_555 yes C(19) C(20) C(24) 114.0(3) 1_555 1_555 1_555 yes C(19) C(20) H(26) 109.5(3) 1_555 1_555 1_555 no C(21) C(20) C(24) 103.2(3) 1_555 1_555 1_555 yes C(21) C(20) H(26) 108.7(3) 1_555 1_555 1_555 no C(24) C(20) H(26) 109.1(3) 1_555 1_555 1_555 no C(20) C(21) C(22) 106.9(3) 1_555 1_555 1_555 yes C(20) C(21) C(29) 111.5(3) 1_555 1_555 1_555 yes C(20) C(21) H(27) 107.2(3) 1_555 1_555 1_555 no C(22) C(21) C(29) 115.5(3) 1_555 1_555 1_555 yes C(22) C(21) H(27) 107.7(3) 1_555 1_555 1_555 no C(29) C(21) H(27) 107.8(3) 1_555 1_555 1_555 no C(21) C(22) C(23) 103.8(3) 1_555 1_555 1_555 yes C(21) C(22) C(30) 108.6(4) 1_555 1_555 1_555 yes C(21) C(22) C(31) 112.4(4) 1_555 1_555 1_555 yes C(23) C(22) C(30) 109.8(4) 1_555 1_555 1_555 yes C(23) C(22) C(31) 110.8(4) 1_555 1_555 1_555 yes C(30) C(22) C(31) 111.1(5) 1_555 1_555 1_555 yes C(22) C(23) C(24) 106.5(3) 1_555 1_555 1_555 yes C(22) C(23) H(28) 110.6(4) 1_555 1_555 1_555 no C(22) C(23) H(29) 111.2(4) 1_555 1_555 1_555 no C(24) C(23) H(28) 110.3(3) 1_555 1_555 1_555 no C(24) C(23) H(29) 111.2(4) 1_555 1_555 1_555 no H(28) C(23) H(29) 107.1(4) 1_555 1_555 1_555 no C(20) C(24) C(23) 101.9(3) 1_555 1_555 1_555 yes C(20) C(24) C(25) 116.0(3) 1_555 1_555 1_555 yes C(20) C(24) H(30) 107.4(3) 1_555 1_555 1_555 no C(23) C(24) C(25) 115.5(3) 1_555 1_555 1_555 yes C(23) C(24) H(30) 107.5(3) 1_555 1_555 1_555 no C(25) C(24) H(30) 108.0(3) 1_555 1_555 1_555 no O(4) C(25) C(24) 107.9(2) 1_555 1_555 1_555 yes O(4) C(25) C(26) 103.2(3) 1_555 1_555 1_555 yes O(4) C(25) C(32) 106.4(3) 1_555 1_555 1_555 yes C(24) C(25) C(26) 114.1(3) 1_555 1_555 1_555 yes C(24) C(25) C(32) 111.2(3) 1_555 1_555 1_555 yes C(26) C(25) C(32) 113.3(3) 1_555 1_555 1_555 yes C(25) C(26) C(27) 105.1(3) 1_555 1_555 1_555 yes C(25) C(26) H(31) 110.6(3) 1_555 1_555 1_555 no C(25) C(26) H(32) 111.2(3) 1_555 1_555 1_555 no C(27) C(26) H(31) 111.2(3) 1_555 1_555 1_555 no C(27) C(26) H(32) 111.5(3) 1_555 1_555 1_555 no H(31) C(26) H(32) 107.2(3) 1_555 1_555 1_555 no C(17) C(27) C(26) 105.3(3) 1_555 1_555 1_555 yes C(17) C(27) H(33) 111.7(4) 1_555 1_555 1_555 no C(17) C(27) H(34) 110.5(3) 1_555 1_555 1_555 no C(26) C(27) H(33) 110.9(3) 1_555 1_555 1_555 no C(26) C(27) H(34) 110.8(4) 1_555 1_555 1_555 no H(33) C(27) H(34) 107.7(4) 1_555 1_555 1_555 no C(18) C(28) H(35) 110.8(4) 1_555 1_555 1_555 no C(18) C(28) H(36) 111.0(4) 1_555 1_555 1_555 no C(18) C(28) H(37) 109.7(3) 1_555 1_555 1_555 no H(35) C(28) H(36) 108.6(4) 1_555 1_555 1_555 no H(35) C(28) H(37) 108.2(4) 1_555 1_555 1_555 no H(36) C(28) H(37) 108.3(4) 1_555 1_555 1_555 no N(2) C(29) C(21) 178.0(5) 1_555 1_555 1_555 yes C(22) C(30) H(38) 111.3(5) 1_555 1_555 1_555 no C(22) C(30) H(39) 111.1(4) 1_555 1_555 1_555 no C(22) C(30) H(40) 111.7(5) 1_555 1_555 1_555 no H(38) C(30) H(39) 107.4(6) 1_555 1_555 1_555 no H(38) C(30) H(40) 107.7(5) 1_555 1_555 1_555 no H(39) C(30) H(40) 107.4(6) 1_555 1_555 1_555 no C(22) C(31) H(41) 112.0(6) 1_555 1_555 1_555 no C(22) C(31) H(42) 110.2(5) 1_555 1_555 1_555 no C(22) C(31) H(43) 111.4(6) 1_555 1_555 1_555 no H(41) C(31) H(42) 107.4(7) 1_555 1_555 1_555 no H(41) C(31) H(43) 108.7(6) 1_555 1_555 1_555 no H(42) C(31) H(43) 107.0(7) 1_555 1_555 1_555 no C(25) C(32) H(44) 110.7(3) 1_555 1_555 1_555 no C(25) C(32) H(45) 110.5(4) 1_555 1_555 1_555 no C(25) C(32) H(46) 110.4(4) 1_555 1_555 1_555 no H(44) C(32) H(45) 108.7(4) 1_555 1_555 1_555 no H(44) C(32) H(46) 108.2(4) 1_555 1_555 1_555 no H(45) C(32) H(46) 108.3(4) 1_555 1_555 1_555 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) C(2) C(1) -160.1(3) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(12) -33.0(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) -4.7(5) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(8) 112.2(4) 1_555 1_555 1_555 1_555 yes O(2) C(1) C(2) C(3) 52.0(4) 1_555 1_555 1_555 1_555 yes O(2) C(1) C(2) C(12) -74.5(4) 1_555 1_555 1_555 1_555 yes O(2) C(1) C(11) C(10) -7.8(4) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(8) C(4) -65.6(3) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(8) C(7) 175.2(3) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(10) C(11) 28.4(3) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(18) C(17) -159.9(3) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(18) C(28) -33.4(5) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(20) C(21) -4.6(5) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(20) C(24) 112.2(4) 1_555 1_555 1_555 1_555 yes O(4) C(17) C(18) C(19) 51.7(4) 1_555 1_555 1_555 1_555 yes O(4) C(17) C(18) C(28) -74.4(4) 1_555 1_555 1_555 1_555 yes O(4) C(17) C(27) C(26) -7.8(3) 1_555 1_555 1_555 1_555 yes O(4) C(25) C(24) C(20) -65.8(3) 1_555 1_555 1_555 1_555 yes O(4) C(25) C(24) C(23) 175.1(3) 1_555 1_555 1_555 1_555 yes O(4) C(25) C(26) C(27) 28.3(3) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(5) C(4) 17(19) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(5) C(6) 139(19) 1_555 1_555 1_555 1_555 yes N(2) C(29) C(21) C(20) 10(17) 1_555 1_555 1_555 1_555 yes N(2) C(29) C(21) C(22) 132(16) 1_555 1_555 1_555 1_555 yes C(1) O(2) C(9) C(8) 86.1(3) 1_555 1_555 1_555 1_555 yes C(1) O(2) C(9) C(10) -35.0(3) 1_555 1_555 1_555 1_555 yes C(1) O(2) C(9) C(16) -154.2(3) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 20.7(4) 1_555 1_555 1_555 1_555 yes C(1) C(11) C(10) C(9) -12.7(4) 1_555 1_555 1_555 1_555 yes C(2) C(1) O(2) C(9) -100.4(3) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(11) C(10) 116.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 174.6(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(8) -68.5(4) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(11) -69.8(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) 152.6(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(13) -80.3(4) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(7) -162.8(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(9) 70.6(4) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(12) 147.8(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) -6.0(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(14) 113.8(4) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(15) -123.0(4) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(7) C(6) 38.3(4) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(10) 48.6(4) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(16) 177.8(3) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(7) -41.0(3) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(9) -167.6(3) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -20.2(4) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(4) C(8) 29.3(3) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 165.1(3) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(13) -130.6(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -70.6(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(16) 58.7(4) 1_555 1_555 1_555 1_555 yes C(8) C(4) C(5) C(13) 156.5(3) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(14) -141.1(4) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(15) 95.8(4) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -88.6(4) 1_555 1_555 1_555 1_555 yes C(9) O(2) C(1) C(11) 27.3(3) 1_555 1_555 1_555 1_555 yes C(11) C(1) C(2) C(12) 163.8(3) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(16) 143.0(3) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(14) -10.8(6) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(15) 112.3(4) 1_555 1_555 1_555 1_555 yes C(17) O(4) C(25) C(24) 86.2(3) 1_555 1_555 1_555 1_555 yes C(17) O(4) C(25) C(26) -34.8(3) 1_555 1_555 1_555 1_555 yes C(17) O(4) C(25) C(32) -154.3(3) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) 21.1(4) 1_555 1_555 1_555 1_555 yes C(17) C(27) C(26) C(25) -12.7(4) 1_555 1_555 1_555 1_555 yes C(18) C(17) O(4) C(25) -100.4(3) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(27) C(26) 116.8(3) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) 174.4(3) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(24) -68.8(4) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(17) C(27) -70.1(4) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) 152.5(3) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(29) -80.4(4) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(24) C(23) -163.0(3) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(24) C(25) 70.7(4) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(18) C(28) 147.6(3) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) -5.9(4) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(30) -122.8(4) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(31) 113.8(4) 1_555 1_555 1_555 1_555 yes C(20) C(24) C(23) C(22) 38.5(4) 1_555 1_555 1_555 1_555 yes C(20) C(24) C(25) C(26) 48.2(4) 1_555 1_555 1_555 1_555 yes C(20) C(24) C(25) C(32) 177.8(3) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(24) C(23) -41.2(3) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(24) C(25) -167.5(3) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) -20.2(4) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(20) C(24) 29.4(3) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) 165.1(3) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(29) -130.6(4) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) -70.9(4) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(32) 58.7(4) 1_555 1_555 1_555 1_555 yes C(24) C(20) C(21) C(29) 156.6(3) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(30) 95.8(4) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(31) -141.0(4) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) -88.5(4) 1_555 1_555 1_555 1_555 yes C(25) O(4) C(17) C(27) 27.1(3) 1_555 1_555 1_555 1_555 yes C(27) C(17) C(18) C(28) 163.8(3) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(32) 142.9(3) 1_555 1_555 1_555 1_555 yes C(29) C(21) C(22) C(30) 112.5(4) 1_555 1_555 1_555 1_555 yes C(29) C(21) C(22) C(31) -10.9(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) H(45) 2.768(4) 1_555 1_556 ? O(1) H(36) 2.939(3) 1_555 1_656 ? O(1) H(24) 3.040(3) 1_555 1_656 ? O(1) H(21) 3.109(4) 1_555 1_655 ? O(1) C(18) 3.162(4) 1_555 1_656 ? O(1) C(28) 3.416(5) 1_555 1_656 ? O(1) C(17) 3.446(5) 1_555 1_656 ? O(1) H(23) 3.585(4) 1_555 1_655 ? O(2) H(39) 2.786(2) 1_555 1_555 ? O(2) H(30) 2.963(2) 1_555 1_555 ? O(2) H(33) 3.342(2) 1_555 1_556 ? O(3) H(22) 2.771(4) 1_555 1_555 ? O(3) H(13) 2.932(3) 1_555 1_455 ? O(3) H(1) 3.035(3) 1_555 1_455 ? O(3) H(44) 3.105(4) 1_555 1_455 ? O(3) C(2) 3.165(4) 1_555 1_455 ? O(3) C(12) 3.416(5) 1_555 1_455 ? O(3) C(1) 3.442(4) 1_555 1_455 ? O(3) H(46) 3.590(4) 1_555 1_455 ? O(4) H(19) 2.790(2) 1_555 1_554 ? O(4) H(7) 2.963(2) 1_555 1_554 ? O(4) H(10) 3.349(2) 1_555 1_555 ? N(1) H(8) 2.643(5) 1_555 2_857 ? N(1) H(6) 2.990(6) 1_555 1_655 ? N(1) H(16) 3.297(6) 1_555 2_857 ? N(1) H(36) 3.306(6) 1_555 1_656 ? N(1) H(3) 3.363(6) 1_555 2_857 ? N(1) H(5) 3.418(6) 1_555 2_857 ? N(1) H(11) 3.427(6) 1_555 2_857 ? N(1) H(18) 3.483(6) 1_555 2_858 ? N(1) C(10) 3.524(6) 1_555 2_857 ? N(1) H(23) 3.595(6) 1_555 1_655 ? N(2) H(29) 2.988(6) 1_555 1_455 ? N(2) H(13) 3.310(6) 1_555 1_455 ? N(2) H(46) 3.598(5) 1_555 1_455 ? C(1) H(30) 3.083(3) 1_555 1_555 ? C(1) H(44) 3.125(3) 1_555 1_555 ? C(1) H(39) 3.396(4) 1_555 1_555 ? C(2) H(22) 3.463(4) 1_555 1_655 ? C(2) H(21) 3.500(4) 1_555 1_655 ? C(3) H(45) 3.375(3) 1_555 1_556 ? C(3) H(21) 3.443(4) 1_555 1_655 ? C(3) H(23) 3.589(4) 1_555 1_655 ? C(5) H(36) 3.550(4) 1_555 1_656 ? C(7) H(24) 3.578(5) 1_555 1_556 ? C(8) H(24) 3.229(3) 1_555 1_556 ? C(10) H(15) 3.186(4) 1_555 2_757 ? C(10) H(37) 3.548(4) 1_555 1_555 ? C(11) H(44) 3.122(4) 1_555 1_555 ? C(11) H(35) 3.285(4) 1_555 1_655 ? C(11) H(30) 3.582(4) 1_555 1_555 ? C(12) H(39) 3.513(5) 1_555 1_555 ? C(12) H(27) 3.536(4) 1_555 1_655 ? C(12) H(32) 3.551(5) 1_555 1_556 ? C(13) H(36) 3.163(5) 1_555 1_656 ? C(14) H(23) 3.226(7) 1_555 2_757 ? C(14) H(37) 3.519(6) 1_555 2_757 ? C(14) H(9) 3.591(6) 1_555 2_757 ? C(14) H(11) 3.594(7) 1_555 2_857 ? C(15) H(20) 3.386(6) 1_555 2_758 ? C(15) H(37) 3.540(6) 1_555 1_556 ? C(15) H(9) 3.549(6) 1_555 1_556 ? C(15) H(10) 3.581(6) 1_555 1_556 ? C(16) H(2) 3.014(4) 1_555 1_455 ? C(16) H(24) 3.178(4) 1_555 1_556 ? C(16) H(33) 3.274(4) 1_555 1_556 ? C(16) H(15) 3.368(4) 1_555 2_757 ? C(17) H(7) 3.078(3) 1_555 1_554 ? C(17) H(21) 3.137(3) 1_555 1_554 ? C(17) H(19) 3.402(4) 1_555 1_554 ? C(18) H(45) 3.448(4) 1_555 1_455 ? C(18) H(44) 3.505(4) 1_555 1_455 ? C(19) H(22) 3.374(3) 1_555 1_555 ? C(19) H(44) 3.446(4) 1_555 1_455 ? C(19) H(46) 3.591(4) 1_555 1_455 ? C(21) H(13) 3.546(4) 1_555 1_455 ? C(23) H(1) 3.581(5) 1_555 1_555 ? C(24) H(1) 3.235(3) 1_555 1_555 ? C(26) H(14) 3.552(4) 1_555 1_554 ? C(27) H(21) 3.125(4) 1_555 1_554 ? C(27) H(12) 3.290(4) 1_555 1_454 ? C(27) H(7) 3.578(4) 1_555 1_554 ? C(28) H(17) 3.350(4) 1_555 2_757 ? C(28) H(19) 3.517(5) 1_555 1_554 ? C(28) H(4) 3.540(4) 1_555 1_454 ? C(28) H(9) 3.546(5) 1_555 1_555 ? C(29) H(13) 3.161(5) 1_555 1_455 ? C(30) H(14) 3.537(7) 1_555 1_555 ? C(30) H(32) 3.551(6) 1_555 1_556 ? C(30) H(33) 3.580(6) 1_555 1_556 ? C(32) H(25) 3.011(4) 1_555 1_655 ? C(32) H(1) 3.178(4) 1_555 1_555 ? C(32) H(10) 3.276(4) 1_555 1_555 ? H(1) H(39) 3.0207(6) 1_555 1_555 ? H(1) H(29) 3.0634(1) 1_555 1_555 ? H(2) H(22) 2.557(1) 1_555 1_655 ? H(2) H(21) 2.868(1) 1_555 1_655 ? H(2) H(23) 3.0843(9) 1_555 1_655 ? H(2) H(35) 3.4699(1) 1_555 1_655 ? H(3) H(16) 3.1788(9) 1_555 2_857 ? H(4) H(36) 2.968(1) 1_555 1_656 ? H(4) H(35) 3.3230(6) 1_555 1_656 ? H(5) H(5) 2.8297(5) 1_555 2_757 ? H(5) H(15) 3.5096(7) 1_555 2_757 ? H(5) H(6) 3.5272(1) 1_555 2_757 ? H(6) H(24) 3.0615(1) 1_555 1_556 ? H(6) H(36) 3.4526(7) 1_555 1_556 ? H(7) H(33) 3.2936(5) 1_555 1_556 ? H(7) H(45) 3.4828(4) 1_555 1_556 ? H(8) H(15) 2.945(1) 1_555 2_757 ? H(9) H(37) 2.5970(7) 1_555 1_555 ? H(9) H(15) 2.6624(7) 1_555 2_757 ? H(9) H(18) 3.2669(3) 1_555 1_554 ? H(10) H(35) 2.851(1) 1_555 1_655 ? H(10) H(18) 3.1055(1) 1_555 1_554 ? H(10) H(19) 3.1059(4) 1_555 1_554 ? H(10) H(30) 3.3022(5) 1_555 1_555 ? H(11) H(35) 2.8976(6) 1_555 1_655 ? H(11) H(17) 3.0471(7) 1_555 2_857 ? H(11) H(16) 3.2282(8) 1_555 2_857 ? H(12) H(33) 2.861(1) 1_555 1_656 ? H(12) H(34) 2.9000(6) 1_555 1_656 ? H(12) H(21) 3.2733(9) 1_555 1_655 ? H(12) H(27) 3.3175(6) 1_555 1_655 ? H(12) H(45) 3.4546(5) 1_555 1_556 ? H(12) H(25) 3.4681(1) 1_555 1_656 ? H(13) H(27) 2.963(1) 1_555 1_655 ? H(13) H(39) 3.318(2) 1_555 1_555 ? H(13) H(40) 3.365(1) 1_555 1_555 ? H(13) H(29) 3.4510(7) 1_555 1_555 ? H(14) H(32) 2.6045(7) 1_555 1_556 ? H(14) H(39) 2.936(1) 1_555 1_555 ? H(14) H(40) 3.2408(5) 1_555 1_555 ? H(15) H(35) 3.4722(3) 1_555 2_757 ? H(16) H(23) 2.7945(4) 1_555 2_757 ? H(17) H(37) 3.1358(3) 1_555 2_757 ? H(17) H(36) 3.3826(1) 1_555 2_757 ? H(18) H(20) 3.4021(9) 1_555 2_758 ? H(19) H(37) 2.941(1) 1_555 1_556 ? H(19) H(24) 3.0285(6) 1_555 1_556 ? H(19) H(36) 3.325(2) 1_555 1_556 ? H(20) H(20) 2.5544(2) 1_555 2_758 ? H(20) H(37) 3.2435(5) 1_555 1_556 ? H(20) H(36) 3.365(1) 1_555 1_556 ? H(22) H(35) 3.4405(5) 1_555 1_555 ? H(22) H(30) 3.4791(4) 1_555 1_555 ? H(25) H(45) 2.544(1) 1_555 1_455 ? H(25) H(44) 2.878(1) 1_555 1_455 ? H(25) H(46) 3.0791(9) 1_555 1_455 ? H(32) H(38) 3.2606(3) 1_555 1_554 ? H(33) H(38) 3.1028(1) 1_555 1_554 ? H(33) H(39) 3.1153(4) 1_555 1_554 ? H(35) H(44) 3.2848(9) 1_555 1_455 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ; data_z-5_8-thf-3_9 #------------------------------------------------------------------------------ _audit_creation_date 'Mon Jun 5 15:19:58 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'Rigaku/AFC Diffractometer Control' _computing_cell_refinement 'Rigaku/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 261.36 _chemical_formula_analytical ? _chemical_formula_sum 'C16 H23 N O2 ' _chemical_formula_moiety '?' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 13.385(3) _cell_length_b 16.622(3) _cell_length_c 13.449(3) _cell_angle_alpha 90 _cell_angle_beta 92.15(2) _cell_angle_gamma 90 _cell_volume 2990.1(9) _cell_formula_units_Z 8 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 15.0 #------------------------------------------------------------------------------ _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n ' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136.00 _exptl_absorpt_coefficient_mu 0.076 _exptl_absorpt_correction_type none _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 296.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% 0.52 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l -3 0 1 -2 -2 0 -1 -2 2 _diffrn_reflns_number 7162 _reflns_number_total 6876 _reflns_number_gt 3641 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.013 _diffrn_reflns_av_sigmaI/netI 0.082 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 27.51 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.04785 _diffrn_orient_matrix_UB_12 -0.04287 _diffrn_orient_matrix_UB_13 0.01959 _diffrn_orient_matrix_UB_21 0.02248 _diffrn_orient_matrix_UB_22 0.00674 _diffrn_orient_matrix_UB_23 0.07126 _diffrn_orient_matrix_UB_31 -0.05287 _diffrn_orient_matrix_UB_32 0.04167 _diffrn_orient_matrix_UB_33 0.00863 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O -0.0656(2) -0.1114(1) -0.6137(2) 0.0506(7) Uani 1.00 d . . . O(2) O -0.1707(1) -0.0182(1) -0.5523(1) 0.0453(6) Uani 1.00 d . . . O(3) O -0.0807(2) -0.0102(1) -0.3633(2) 0.0461(6) Uani 1.00 d . . . O(4) O -0.0294(1) -0.1357(1) -0.3143(2) 0.0518(6) Uani 1.00 d . . . N(1) N -0.1666(3) -0.1745(2) -0.9224(3) 0.104(1) Uani 1.00 d . . . N(2) N -0.3889(3) 0.0202(2) -0.2418(3) 0.100(1) Uani 1.00 d . . . C(1) C -0.3294(3) -0.1365(2) -0.5861(2) 0.056(1) Uani 1.00 d . . . C(2) C -0.2350(2) -0.1485(2) -0.6074(2) 0.0453(8) Uani 1.00 d . . . C(3) C -0.1620(2) -0.0806(2) -0.6254(2) 0.0389(8) Uani 1.00 d . . . C(4) C -0.1801(2) -0.0357(2) -0.7261(2) 0.0373(7) Uani 1.00 d . . . C(5) C -0.2519(2) -0.0726(2) -0.8055(2) 0.0440(8) Uani 1.00 d . . . C(6) C -0.3012(2) 0.0002(2) -0.8605(2) 0.0500(9) Uani 1.00 d . . . C(7) C -0.3190(3) 0.0558(2) -0.7714(2) 0.0520(10) Uani 1.00 d . . . C(8) C -0.2278(2) 0.0459(2) -0.7004(2) 0.0429(8) Uani 1.00 d . . . C(9) C -0.2416(2) 0.0430(2) -0.5862(2) 0.0498(9) Uani 1.00 d . . . C(10) C -0.3437(3) 0.0191(3) -0.5498(3) 0.065(1) Uani 1.00 d . . . C(11) C -0.3905(3) -0.0610(3) -0.5816(3) 0.070(1) Uani 1.00 d . . . C(12) C -0.1950(4) -0.2324(2) -0.6237(4) 0.074(1) Uani 1.00 d . . . C(13) C -0.2038(3) -0.1306(2) -0.8710(3) 0.064(1) Uani 1.00 d . . . C(14) C -0.2284(3) 0.0375(3) -0.9329(3) 0.063(1) Uani 1.00 d . . . C(15) C -0.3977(3) -0.0223(3) -0.9172(3) 0.075(1) Uani 1.00 d . . . C(16) C -0.2051(4) 0.1212(2) -0.5365(4) 0.082(2) Uani 1.00 d . . . C(17) C -0.0358(2) -0.0802(2) -0.1189(2) 0.0517(10) Uani 1.00 d . . . C(18) C -0.0768(2) -0.0374(2) -0.1920(2) 0.0390(8) Uani 1.00 d . . . C(19) C -0.0982(2) -0.0723(2) -0.2952(2) 0.0382(7) Uani 1.00 d . . . C(20) C -0.2030(2) -0.1123(2) -0.3135(2) 0.0385(8) Uani 1.00 d . . . C(21) C -0.2803(2) -0.1092(2) -0.2320(2) 0.0435(8) Uani 1.00 d . . . C(22) C -0.3436(2) -0.1878(2) -0.2453(2) 0.056(1) Uani 1.00 d . . . C(23) C -0.2654(3) -0.2487(2) -0.2764(4) 0.075(1) Uani 1.00 d . . . C(24) C -0.1817(2) -0.2026(2) -0.3268(3) 0.0507(10) Uani 1.00 d . . . C(25) C -0.0738(2) -0.2118(2) -0.2868(3) 0.061(1) Uani 1.00 d . . . C(26) C -0.0686(3) -0.2221(2) -0.1686(4) 0.079(1) Uani 1.00 d . . . C(27) C 0.0000(3) -0.1658(2) -0.1180(3) 0.072(1) Uani 1.00 d . . . C(28) C -0.1060(3) 0.0488(2) -0.1768(3) 0.054(1) Uani 1.00 d . . . C(29) C -0.3413(2) -0.0360(2) -0.2358(3) 0.061(1) Uani 1.00 d . . . C(30) C -0.4241(3) -0.1777(3) -0.3290(4) 0.081(2) Uani 1.00 d . . . C(31) C -0.3940(4) -0.2097(3) -0.1482(4) 0.083(2) Uani 1.00 d . . . C(32) C -0.0165(4) -0.2761(3) -0.3398(5) 0.102(2) Uani 1.00 d . . . H(1) H -0.112(2) -0.028(1) -0.755(2) 0.032(6) Uiso 1.00 calc . . . H(2) H -0.369(2) -0.185(2) -0.579(2) 0.066(10) Uiso 1.00 calc . . . H(3) H -0.443(3) -0.070(2) -0.544(3) 0.09(1) Uiso 1.00 calc . . . H(4) H -0.425(2) -0.054(2) -0.654(3) 0.08(1) Uiso 1.00 calc . . . H(5) H -0.389(3) 0.060(2) -0.568(2) 0.07(1) Uiso 1.00 calc . . . H(6) H -0.337(2) 0.019(2) -0.473(3) 0.08(1) Uiso 1.00 calc . . . H(7) H -0.177(2) 0.088(2) -0.713(2) 0.044(8) Uiso 1.00 calc . . . H(8) H -0.329(2) 0.109(2) -0.790(2) 0.062(9) Uiso 1.00 calc . . . H(9) H -0.384(2) 0.040(2) -0.740(2) 0.054(8) Uiso 1.00 calc . . . H(10) H -0.306(2) -0.100(1) -0.774(2) 0.034(7) Uiso 1.00 calc . . . H(11) H -0.169(3) -0.241(2) -0.695(3) 0.10(1) Uiso 1.00 calc . . . H(12) H -0.245(3) -0.269(2) -0.610(3) 0.09(1) Uiso 1.00 calc . . . H(13) H -0.128(3) -0.244(2) -0.576(3) 0.10(1) Uiso 1.00 calc . . . H(14) H -0.026(2) -0.078(2) -0.616(2) 0.06(1) Uiso 1.00 calc . . . H(15) H -0.213(3) 0.116(2) -0.462(3) 0.08(1) Uiso 1.00 calc . . . H(16) H -0.121(4) 0.131(3) -0.549(4) 0.15(1) Uiso 1.00 calc . . . H(17) H -0.251(3) 0.158(2) -0.555(3) 0.08(1) Uiso 1.00 calc . . . H(18) H -0.449(3) -0.043(2) -0.877(3) 0.08(1) Uiso 1.00 calc . . . H(19) H -0.388(3) -0.059(2) -0.972(3) 0.08(1) Uiso 1.00 calc . . . H(20) H -0.429(3) 0.028(3) -0.953(3) 0.11(1) Uiso 1.00 calc . . . H(21) H -0.260(2) 0.085(2) -0.965(3) 0.07(1) Uiso 1.00 calc . . . H(22) H -0.208(3) 0.000(2) -0.991(3) 0.09(1) Uiso 1.00 calc . . . H(23) H -0.163(2) 0.054(2) -0.901(2) 0.062(9) Uiso 1.00 calc . . . H(24) H -0.232(2) -0.089(1) -0.373(2) 0.029(6) Uiso 1.00 calc . . . H(25) H -0.026(2) -0.054(2) -0.057(2) 0.065(10) Uiso 1.00 calc . . . H(26) H 0.014(2) -0.183(2) -0.053(3) 0.071(10) Uiso 1.00 calc . . . H(27) H 0.072(3) -0.181(3) -0.171(3) 0.14(1) Uiso 1.00 calc . . . H(28) H -0.040(3) -0.278(3) -0.163(3) 0.10(1) Uiso 1.00 calc . . . H(29) H -0.149(4) -0.214(3) -0.123(3) 0.14(1) Uiso 1.00 calc . . . H(30) H -0.185(2) -0.215(2) -0.397(2) 0.047(8) Uiso 1.00 calc . . . H(31) H -0.293(3) -0.292(3) -0.332(3) 0.13(1) Uiso 1.00 calc . . . H(32) H -0.238(3) -0.276(2) -0.220(3) 0.07(1) Uiso 1.00 calc . . . H(33) H -0.244(2) -0.109(2) -0.165(2) 0.049(8) Uiso 1.00 calc . . . H(34) H -0.096(3) -0.021(2) -0.418(2) 0.07(1) Uiso 1.00 calc . . . H(35) H -0.178(3) 0.057(2) -0.189(3) 0.10(1) Uiso 1.00 calc . . . H(36) H -0.067(2) 0.082(2) -0.209(2) 0.064(10) Uiso 1.00 calc . . . H(37) H -0.098(2) 0.066(2) -0.107(3) 0.08(1) Uiso 1.00 calc . . . H(38) H 0.056(4) -0.274(3) -0.301(4) 0.15(1) Uiso 1.00 calc . . . H(39) H -0.010(2) -0.258(2) -0.417(2) 0.039(8) Uiso 1.00 calc . . . H(40) H -0.045(3) -0.324(3) -0.340(3) 0.12(1) Uiso 1.00 calc . . . H(41) H -0.340(3) -0.217(2) -0.093(3) 0.10(1) Uiso 1.00 calc . . . H(42) H -0.431(3) -0.255(3) -0.155(3) 0.11(1) Uiso 1.00 calc . . . H(43) H -0.451(4) -0.167(3) -0.124(4) 0.15(1) Uiso 1.00 calc . . . H(44) H -0.459(3) -0.228(3) -0.338(3) 0.10(1) Uiso 1.00 calc . . . H(45) H -0.489(4) -0.136(3) -0.310(4) 0.17(1) Uiso 1.00 calc . . . H(46) H -0.395(3) -0.166(2) -0.390(3) 0.09(1) Uiso 1.00 calc . . . 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 O(1) 0.037(1) 0.045(1) 0.070(1) 0.001(1) -0.003(1) 0.003(1) O(2) 0.054(1) 0.039(1) 0.043(1) 0.0038(9) -0.0071(9) -0.0057(9) O(3) 0.050(1) 0.048(1) 0.040(1) -0.0138(10) 0.0009(10) 0.002(1) O(4) 0.036(1) 0.048(1) 0.072(1) 0.0051(9) 0.0050(10) -0.012(1) N(1) 0.148(4) 0.084(3) 0.082(3) 0.005(2) 0.025(2) -0.031(2) N(2) 0.066(2) 0.077(2) 0.159(4) 0.027(2) 0.028(2) 0.010(2) C(1) 0.053(2) 0.067(2) 0.050(2) -0.017(2) 0.007(2) 0.010(2) C(2) 0.051(2) 0.043(2) 0.042(2) -0.012(1) 0.003(1) 0.001(1) C(3) 0.037(1) 0.035(1) 0.045(2) 0.000(1) 0.001(1) -0.003(1) C(4) 0.032(1) 0.038(2) 0.042(2) -0.003(1) 0.003(1) -0.002(1) C(5) 0.041(2) 0.048(2) 0.043(2) -0.010(1) 0.004(1) -0.001(1) C(6) 0.045(2) 0.061(2) 0.044(2) -0.005(1) -0.001(1) 0.006(2) C(7) 0.052(2) 0.054(2) 0.051(2) 0.011(2) 0.004(2) 0.013(2) C(8) 0.046(2) 0.035(2) 0.048(2) -0.002(1) 0.004(1) 0.000(1) C(9) 0.059(2) 0.045(2) 0.045(2) 0.012(1) -0.001(1) -0.005(1) C(10) 0.066(2) 0.083(3) 0.047(2) 0.027(2) 0.014(2) 0.008(2) C(11) 0.042(2) 0.097(3) 0.071(3) 0.003(2) 0.014(2) 0.030(2) C(12) 0.091(3) 0.039(2) 0.093(3) -0.015(2) 0.027(3) -0.009(2) C(13) 0.080(3) 0.061(2) 0.051(2) -0.007(2) 0.001(2) -0.009(2) C(14) 0.061(2) 0.075(3) 0.053(2) -0.005(2) 0.011(2) 0.015(2) C(15) 0.054(2) 0.108(4) 0.061(2) -0.013(2) -0.013(2) 0.008(3) C(16) 0.122(4) 0.050(2) 0.074(3) 0.025(2) -0.021(3) -0.020(2) C(17) 0.050(2) 0.058(2) 0.047(2) 0.002(2) -0.001(1) 0.001(2) C(18) 0.033(1) 0.040(2) 0.044(2) -0.002(1) 0.003(1) -0.001(1) C(19) 0.034(1) 0.035(1) 0.045(2) -0.001(1) 0.002(1) 0.000(1) C(20) 0.035(1) 0.036(2) 0.045(2) -0.001(1) -0.003(1) 0.003(1) C(21) 0.035(1) 0.045(2) 0.051(2) 0.000(1) 0.002(1) 0.005(1) C(22) 0.047(2) 0.054(2) 0.066(2) -0.015(2) 0.004(2) 0.008(2) C(23) 0.069(3) 0.048(2) 0.108(4) -0.012(2) 0.013(2) 0.006(2) C(24) 0.051(2) 0.038(2) 0.062(2) -0.002(1) 0.000(2) -0.008(2) C(25) 0.055(2) 0.036(2) 0.093(3) 0.004(1) -0.005(2) -0.009(2) C(26) 0.082(3) 0.054(2) 0.100(3) 0.000(2) -0.024(2) 0.025(2) C(27) 0.090(3) 0.060(2) 0.064(3) 0.015(2) -0.015(2) 0.011(2) C(28) 0.063(2) 0.044(2) 0.053(2) -0.003(2) 0.008(2) -0.005(2) C(29) 0.040(2) 0.060(2) 0.084(3) 0.001(2) 0.017(2) 0.006(2) C(30) 0.059(2) 0.107(4) 0.075(3) -0.029(2) -0.007(2) 0.004(3) C(31) 0.081(3) 0.086(3) 0.081(3) -0.033(3) 0.014(2) 0.023(3) C(32) 0.073(3) 0.057(3) 0.177(6) 0.013(2) 0.013(4) -0.033(3) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3641 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0465 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 1.355 _refine_ls_shift/su_max 0.1630 _refine_ls_shift/su_mean 0.0060 _refine_diff_density_min -0.20 _refine_diff_density_max 0.54 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag O(1) C(3) 1.392(3) 1_555 1_555 yes O(1) H(7) 0.77(3) 1_555 1_555 no O(2) C(3) 1.437(3) 1_555 1_555 yes O(2) C(9) 1.453(3) 1_555 1_555 yes O(3) C(19) 1.405(3) 1_555 1_555 yes O(3) H(28) 0.78(3) 1_555 1_555 no O(4) C(19) 1.429(3) 1_555 1_555 yes O(4) C(25) 1.452(4) 1_555 1_555 yes N(1) C(13) 1.133(4) 1_555 1_555 yes N(2) C(29) 1.133(4) 1_555 1_555 yes C(1) C(2) 1.321(4) 1_555 1_555 yes C(1) C(11) 1.500(5) 1_555 1_555 yes C(1) H(3) 0.98(3) 1_555 1_555 no C(2) C(3) 1.518(4) 1_555 1_555 yes C(2) C(12) 1.512(5) 1_555 1_555 yes C(3) C(4) 1.556(4) 1_555 1_555 yes C(4) C(5) 1.538(4) 1_555 1_555 yes C(4) C(8) 1.543(4) 1_555 1_555 yes C(4) H(8) 1.01(2) 1_555 1_555 no C(5) C(6) 1.553(4) 1_555 1_555 yes C(5) C(13) 1.471(5) 1_555 1_555 yes C(5) H(9) 0.97(2) 1_555 1_555 no C(6) C(7) 1.539(4) 1_555 1_555 yes C(6) C(14) 1.533(4) 1_555 1_555 yes C(6) C(15) 1.523(4) 1_555 1_555 yes C(7) C(8) 1.530(4) 1_555 1_555 yes C(7) H(16) 0.93(3) 1_555 1_555 no C(7) H(17) 1.01(3) 1_555 1_555 no C(8) C(9) 1.555(4) 1_555 1_555 yes C(8) H(18) 1.00(3) 1_555 1_555 no C(9) C(10) 1.522(5) 1_555 1_555 yes C(9) C(16) 1.532(5) 1_555 1_555 yes C(10) C(11) 1.527(6) 1_555 1_555 yes C(10) H(22) 0.94(3) 1_555 1_555 no C(10) H(23) 1.04(3) 1_555 1_555 no C(11) H(1) 1.06(3) 1_555 1_555 no C(11) H(2) 0.90(4) 1_555 1_555 no C(12) H(4) 1.04(4) 1_555 1_555 no C(12) H(5) 1.09(4) 1_555 1_555 no C(12) H(6) 0.92(4) 1_555 1_555 no C(14) H(10) 0.98(3) 1_555 1_555 no C(14) H(11) 1.00(3) 1_555 1_555 no C(14) H(12) 1.04(4) 1_555 1_555 no C(15) H(13) 1.04(4) 1_555 1_555 no C(15) H(14) 0.96(4) 1_555 1_555 no C(15) H(15) 0.97(4) 1_555 1_555 no C(16) H(19) 1.16(5) 1_555 1_555 no C(16) H(20) 0.89(4) 1_555 1_555 no C(16) H(21) 1.01(4) 1_555 1_555 no C(17) C(18) 1.317(4) 1_555 1_555 yes C(17) C(27) 1.500(5) 1_555 1_555 yes C(17) H(24) 0.94(3) 1_555 1_555 no C(18) C(19) 1.521(4) 1_555 1_555 yes C(18) C(28) 1.502(4) 1_555 1_555 yes C(19) C(20) 1.564(4) 1_555 1_555 yes C(20) C(21) 1.536(4) 1_555 1_555 yes C(20) C(24) 1.539(4) 1_555 1_555 yes C(20) H(38) 0.95(2) 1_555 1_555 no C(21) C(22) 1.563(4) 1_555 1_555 yes C(21) C(29) 1.465(4) 1_555 1_555 yes C(21) H(29) 1.01(3) 1_555 1_555 no C(22) C(23) 1.526(5) 1_555 1_555 yes C(22) C(30) 1.537(5) 1_555 1_555 yes C(22) C(31) 1.536(5) 1_555 1_555 yes C(23) C(24) 1.535(5) 1_555 1_555 yes C(23) H(36) 1.09(4) 1_555 1_555 no C(23) H(37) 0.94(3) 1_555 1_555 no C(24) C(25) 1.530(4) 1_555 1_555 yes C(24) H(41) 0.96(3) 1_555 1_555 no C(25) C(26) 1.597(6) 1_555 1_555 yes C(25) C(32) 1.510(5) 1_555 1_555 yes C(26) C(27) 1.461(5) 1_555 1_555 yes C(26) H(45) 1.26(5) 1_555 1_555 no C(26) H(47) 1.01(4) 1_555 1_555 no C(27) H(43) 1.25(5) 1_555 1_555 no C(27) H(44) 0.94(3) 1_555 1_555 no C(28) H(25) 0.98(4) 1_555 1_555 no C(28) H(26) 0.98(4) 1_555 1_555 no C(28) H(27) 0.88(3) 1_555 1_555 no C(30) H(33) 0.96(4) 1_555 1_555 no C(30) H(34) 0.95(4) 1_555 1_555 no C(30) H(35) 1.15(5) 1_555 1_555 no C(31) H(30) 1.03(4) 1_555 1_555 no C(31) H(31) 0.90(4) 1_555 1_555 no C(31) H(32) 1.10(5) 1_555 1_555 no C(32) H(39) 1.09(3) 1_555 1_555 no C(32) H(40) 1.09(5) 1_555 1_555 no C(32) H(46) 0.88(5) 1_555 1_555 no #------------------------------------------------------------------------------ loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(3) O(1) H(7) 111(2) 1_555 1_555 1_555 no C(3) O(2) C(9) 111.0(2) 1_555 1_555 1_555 yes C(19) O(3) H(28) 113(2) 1_555 1_555 1_555 no C(19) O(4) C(25) 108.9(2) 1_555 1_555 1_555 yes C(2) C(1) C(11) 131.5(3) 1_555 1_555 1_555 yes C(2) C(1) H(3) 115(1) 1_555 1_555 1_555 no C(11) C(1) H(3) 112(1) 1_555 1_555 1_555 no C(1) C(2) C(3) 123.3(3) 1_555 1_555 1_555 yes C(1) C(2) C(12) 121.2(3) 1_555 1_555 1_555 yes C(3) C(2) C(12) 115.4(3) 1_555 1_555 1_555 yes O(1) C(3) O(2) 106.6(2) 1_555 1_555 1_555 yes O(1) C(3) C(2) 108.0(2) 1_555 1_555 1_555 yes O(1) C(3) C(4) 112.9(2) 1_555 1_555 1_555 yes O(2) C(3) C(2) 111.0(2) 1_555 1_555 1_555 yes O(2) C(3) C(4) 103.6(2) 1_555 1_555 1_555 yes C(2) C(3) C(4) 114.5(2) 1_555 1_555 1_555 yes C(3) C(4) C(5) 119.1(2) 1_555 1_555 1_555 yes C(3) C(4) C(8) 106.2(2) 1_555 1_555 1_555 yes C(3) C(4) H(8) 106(1) 1_555 1_555 1_555 no C(5) C(4) C(8) 104.6(2) 1_555 1_555 1_555 yes C(5) C(4) H(8) 109(1) 1_555 1_555 1_555 no C(8) C(4) H(8) 110(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 105.3(2) 1_555 1_555 1_555 yes C(4) C(5) C(13) 113.6(3) 1_555 1_555 1_555 yes C(4) C(5) H(9) 110(1) 1_555 1_555 1_555 no C(6) C(5) C(13) 114.4(3) 1_555 1_555 1_555 yes C(6) C(5) H(9) 105(1) 1_555 1_555 1_555 no C(13) C(5) H(9) 107(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 99.9(2) 1_555 1_555 1_555 yes C(5) C(6) C(14) 110.5(3) 1_555 1_555 1_555 yes C(5) C(6) C(15) 112.6(3) 1_555 1_555 1_555 yes C(7) C(6) C(14) 111.9(3) 1_555 1_555 1_555 yes C(7) C(6) C(15) 112.6(3) 1_555 1_555 1_555 yes C(14) C(6) C(15) 109.2(3) 1_555 1_555 1_555 yes C(6) C(7) C(8) 106.2(2) 1_555 1_555 1_555 yes C(6) C(7) H(16) 113(1) 1_555 1_555 1_555 no C(6) C(7) H(17) 108(1) 1_555 1_555 1_555 no C(8) C(7) H(16) 111(1) 1_555 1_555 1_555 no C(8) C(7) H(17) 112(1) 1_555 1_555 1_555 no H(16) C(7) H(17) 104(2) 1_555 1_555 1_555 no C(4) C(8) C(7) 106.4(2) 1_555 1_555 1_555 yes C(4) C(8) C(9) 105.0(2) 1_555 1_555 1_555 yes C(4) C(8) H(18) 106(1) 1_555 1_555 1_555 no C(7) C(8) C(9) 119.9(3) 1_555 1_555 1_555 yes C(7) C(8) H(18) 110(1) 1_555 1_555 1_555 no C(9) C(8) H(18) 107(1) 1_555 1_555 1_555 no O(2) C(9) C(8) 103.4(2) 1_555 1_555 1_555 yes O(2) C(9) C(10) 107.5(3) 1_555 1_555 1_555 yes O(2) C(9) C(16) 105.3(3) 1_555 1_555 1_555 yes C(8) C(9) C(10) 117.8(3) 1_555 1_555 1_555 yes C(8) C(9) C(16) 110.9(3) 1_555 1_555 1_555 yes C(10) C(9) C(16) 110.9(3) 1_555 1_555 1_555 yes C(9) C(10) C(11) 120.1(3) 1_555 1_555 1_555 yes C(9) C(10) H(22) 107(2) 1_555 1_555 1_555 no C(9) C(10) H(23) 106(1) 1_555 1_555 1_555 no C(11) C(10) H(22) 108(2) 1_555 1_555 1_555 no C(11) C(10) H(23) 107(1) 1_555 1_555 1_555 no H(22) C(10) H(23) 106(2) 1_555 1_555 1_555 no C(1) C(11) C(10) 121.5(3) 1_555 1_555 1_555 yes C(1) C(11) H(1) 105(1) 1_555 1_555 1_555 no C(1) C(11) H(2) 108(2) 1_555 1_555 1_555 no C(10) C(11) H(1) 108(1) 1_555 1_555 1_555 no C(10) C(11) H(2) 108(2) 1_555 1_555 1_555 no H(1) C(11) H(2) 101(2) 1_555 1_555 1_555 no C(2) C(12) H(4) 113(2) 1_555 1_555 1_555 no C(2) C(12) H(5) 111(2) 1_555 1_555 1_555 no C(2) C(12) H(6) 108(2) 1_555 1_555 1_555 no H(4) C(12) H(5) 102(2) 1_555 1_555 1_555 no H(4) C(12) H(6) 111(3) 1_555 1_555 1_555 no H(5) C(12) H(6) 110(3) 1_555 1_555 1_555 no N(1) C(13) C(5) 179.1(4) 1_555 1_555 1_555 yes C(6) C(14) H(10) 109(1) 1_555 1_555 1_555 no C(6) C(14) H(11) 114(1) 1_555 1_555 1_555 no C(6) C(14) H(12) 115(2) 1_555 1_555 1_555 no H(10) C(14) H(11) 108(2) 1_555 1_555 1_555 no H(10) C(14) H(12) 105(2) 1_555 1_555 1_555 no H(11) C(14) H(12) 103(2) 1_555 1_555 1_555 no C(6) C(15) H(13) 110(2) 1_555 1_555 1_555 no C(6) C(15) H(14) 114(2) 1_555 1_555 1_555 no C(6) C(15) H(15) 113(2) 1_555 1_555 1_555 no H(13) C(15) H(14) 105(2) 1_555 1_555 1_555 no H(13) C(15) H(15) 102(2) 1_555 1_555 1_555 no H(14) C(15) H(15) 108(3) 1_555 1_555 1_555 no C(9) C(16) H(19) 110(2) 1_555 1_555 1_555 no C(9) C(16) H(20) 104(2) 1_555 1_555 1_555 no C(9) C(16) H(21) 108(2) 1_555 1_555 1_555 no H(19) C(16) H(20) 121(3) 1_555 1_555 1_555 no H(19) C(16) H(21) 106(3) 1_555 1_555 1_555 no H(20) C(16) H(21) 103(3) 1_555 1_555 1_555 no C(18) C(17) C(27) 129.9(3) 1_555 1_555 1_555 yes C(18) C(17) H(24) 116(2) 1_555 1_555 1_555 no C(27) C(17) H(24) 113(2) 1_555 1_555 1_555 no C(17) C(18) C(19) 122.3(3) 1_555 1_555 1_555 yes C(17) C(18) C(28) 121.1(3) 1_555 1_555 1_555 yes C(19) C(18) C(28) 116.6(3) 1_555 1_555 1_555 yes O(3) C(19) O(4) 107.5(2) 1_555 1_555 1_555 yes O(3) C(19) C(18) 106.5(2) 1_555 1_555 1_555 yes O(3) C(19) C(20) 112.4(2) 1_555 1_555 1_555 yes O(4) C(19) C(18) 110.1(2) 1_555 1_555 1_555 yes O(4) C(19) C(20) 103.8(2) 1_555 1_555 1_555 yes C(18) C(19) C(20) 116.3(2) 1_555 1_555 1_555 yes C(19) C(20) C(21) 119.8(2) 1_555 1_555 1_555 yes C(19) C(20) C(24) 105.3(2) 1_555 1_555 1_555 yes C(19) C(20) H(38) 106(1) 1_555 1_555 1_555 no C(21) C(20) C(24) 104.4(2) 1_555 1_555 1_555 yes C(21) C(20) H(38) 108(1) 1_555 1_555 1_555 no C(24) C(20) H(38) 111(1) 1_555 1_555 1_555 no C(20) C(21) C(22) 105.5(2) 1_555 1_555 1_555 yes C(20) C(21) C(29) 113.1(3) 1_555 1_555 1_555 yes C(20) C(21) H(29) 109(1) 1_555 1_555 1_555 no C(22) C(21) C(29) 113.0(2) 1_555 1_555 1_555 yes C(22) C(21) H(29) 109(1) 1_555 1_555 1_555 no C(29) C(21) H(29) 106(1) 1_555 1_555 1_555 no C(21) C(22) C(23) 102.2(2) 1_555 1_555 1_555 yes C(21) C(22) C(30) 110.8(3) 1_555 1_555 1_555 yes C(21) C(22) C(31) 110.8(3) 1_555 1_555 1_555 yes C(23) C(22) C(30) 109.9(4) 1_555 1_555 1_555 yes C(23) C(22) C(31) 113.8(3) 1_555 1_555 1_555 yes C(30) C(22) C(31) 109.3(3) 1_555 1_555 1_555 yes C(22) C(23) C(24) 108.0(3) 1_555 1_555 1_555 yes C(22) C(23) H(36) 113(2) 1_555 1_555 1_555 no C(22) C(23) H(37) 110(2) 1_555 1_555 1_555 no C(24) C(23) H(36) 105(2) 1_555 1_555 1_555 no C(24) C(23) H(37) 108(2) 1_555 1_555 1_555 no H(36) C(23) H(37) 110(3) 1_555 1_555 1_555 no C(20) C(24) C(23) 107.1(3) 1_555 1_555 1_555 yes C(20) C(24) C(25) 103.5(2) 1_555 1_555 1_555 yes C(20) C(24) H(41) 108(1) 1_555 1_555 1_555 no C(23) C(24) C(25) 119.3(3) 1_555 1_555 1_555 yes C(23) C(24) H(41) 108(1) 1_555 1_555 1_555 no C(25) C(24) H(41) 109(1) 1_555 1_555 1_555 no O(4) C(25) C(24) 102.3(2) 1_555 1_555 1_555 yes O(4) C(25) C(26) 110.0(3) 1_555 1_555 1_555 yes O(4) C(25) C(32) 106.1(3) 1_555 1_555 1_555 yes C(24) C(25) C(26) 111.5(3) 1_555 1_555 1_555 yes C(24) C(25) C(32) 113.2(3) 1_555 1_555 1_555 yes C(26) C(25) C(32) 113.0(4) 1_555 1_555 1_555 yes C(25) C(26) C(27) 113.5(3) 1_555 1_555 1_555 yes C(25) C(26) H(45) 117(2) 1_555 1_555 1_555 no C(25) C(26) H(47) 100(2) 1_555 1_555 1_555 no C(27) C(26) H(45) 104(2) 1_555 1_555 1_555 no C(27) C(26) H(47) 108(2) 1_555 1_555 1_555 no H(45) C(26) H(47) 113(3) 1_555 1_555 1_555 no C(17) C(27) C(26) 114.1(3) 1_555 1_555 1_555 yes C(17) C(27) H(43) 116(2) 1_555 1_555 1_555 no C(17) C(27) H(44) 110(2) 1_555 1_555 1_555 no C(26) C(27) H(43) 95(2) 1_555 1_555 1_555 no C(26) C(27) H(44) 109(2) 1_555 1_555 1_555 no H(43) C(27) H(44) 110(2) 1_555 1_555 1_555 no C(18) C(28) H(25) 113(2) 1_555 1_555 1_555 no C(18) C(28) H(26) 111(2) 1_555 1_555 1_555 no C(18) C(28) H(27) 111(2) 1_555 1_555 1_555 no H(25) C(28) H(26) 101(2) 1_555 1_555 1_555 no H(25) C(28) H(27) 103(2) 1_555 1_555 1_555 no H(26) C(28) H(27) 115(3) 1_555 1_555 1_555 no N(2) C(29) C(21) 177.8(4) 1_555 1_555 1_555 yes C(22) C(30) H(33) 108(2) 1_555 1_555 1_555 no C(22) C(30) H(34) 110(2) 1_555 1_555 1_555 no C(22) C(30) H(35) 115(2) 1_555 1_555 1_555 no H(33) C(30) H(34) 107(3) 1_555 1_555 1_555 no H(33) C(30) H(35) 100(3) 1_555 1_555 1_555 no H(34) C(30) H(35) 114(3) 1_555 1_555 1_555 no C(22) C(31) H(30) 108(2) 1_555 1_555 1_555 no C(22) C(31) H(31) 111(2) 1_555 1_555 1_555 no C(22) C(31) H(32) 115(2) 1_555 1_555 1_555 no H(30) C(31) H(31) 109(3) 1_555 1_555 1_555 no H(30) C(31) H(32) 109(3) 1_555 1_555 1_555 no H(31) C(31) H(32) 100(3) 1_555 1_555 1_555 no C(25) C(32) H(39) 108(1) 1_555 1_555 1_555 no C(25) C(32) H(40) 101(2) 1_555 1_555 1_555 no C(25) C(32) H(46) 113(3) 1_555 1_555 1_555 no H(39) C(32) H(40) 110(3) 1_555 1_555 1_555 no H(39) C(32) H(46) 107(3) 1_555 1_555 1_555 no H(40) C(32) H(46) 114(4) 1_555 1_555 1_555 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O(1) C(3) O(2) C(9) -151.0(2) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(1) -161.0(3) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(2) C(12) 23.8(4) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(5) -111.6(3) 1_555 1_555 1_555 1_555 yes O(1) C(3) C(4) C(8) 130.8(2) 1_555 1_555 1_555 1_555 yes O(2) C(3) C(2) C(1) -44.5(4) 1_555 1_555 1_555 1_555 yes O(2) C(3) C(2) C(12) 140.3(3) 1_555 1_555 1_555 1_555 yes O(2) C(3) C(4) C(5) 133.5(2) 1_555 1_555 1_555 1_555 yes O(2) C(3) C(4) C(8) 15.9(3) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(8) C(4) -21.2(3) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(8) C(7) -140.6(3) 1_555 1_555 1_555 1_555 yes O(2) C(9) C(10) C(11) 59.6(4) 1_555 1_555 1_555 1_555 yes O(3) C(19) O(4) C(25) 150.9(2) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(18) C(17) 144.1(3) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(18) C(28) -36.5(3) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(20) C(21) 118.6(3) 1_555 1_555 1_555 1_555 yes O(3) C(19) C(20) C(24) -124.4(3) 1_555 1_555 1_555 1_555 yes O(4) C(19) C(18) C(17) 27.8(4) 1_555 1_555 1_555 1_555 yes O(4) C(19) C(18) C(28) -152.8(3) 1_555 1_555 1_555 1_555 yes O(4) C(19) C(20) C(21) -125.6(3) 1_555 1_555 1_555 1_555 yes O(4) C(19) C(20) C(24) -8.6(3) 1_555 1_555 1_555 1_555 yes O(4) C(25) C(24) C(20) 33.7(3) 1_555 1_555 1_555 1_555 yes O(4) C(25) C(24) C(23) 152.4(3) 1_555 1_555 1_555 1_555 yes O(4) C(25) C(26) C(27) 14.9(4) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(5) C(4) 99(27) 1_555 1_555 1_555 1_555 yes N(1) C(13) C(5) C(6) -20(27) 1_555 1_555 1_555 1_555 yes N(2) C(29) C(21) C(20) -48(9) 1_555 1_555 1_555 1_555 yes N(2) C(29) C(21) C(22) 70(9) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(3) C(4) 72.4(4) 1_555 1_555 1_555 1_555 yes C(1) C(11) C(10) C(9) -41.2(5) 1_555 1_555 1_555 1_555 yes C(2) C(1) C(11) C(10) 32.5(6) 1_555 1_555 1_555 1_555 yes C(2) C(3) O(2) C(9) 91.7(3) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(5) 12.4(4) 1_555 1_555 1_555 1_555 yes C(2) C(3) C(4) C(8) -105.1(3) 1_555 1_555 1_555 1_555 yes C(3) O(2) C(9) C(8) 34.0(3) 1_555 1_555 1_555 1_555 yes C(3) O(2) C(9) C(10) -91.3(3) 1_555 1_555 1_555 1_555 yes C(3) O(2) C(9) C(16) 150.4(3) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(1) C(11) -5.4(6) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(6) -147.3(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(5) C(13) 86.8(3) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(7) 131.5(2) 1_555 1_555 1_555 1_555 yes C(3) C(4) C(8) C(9) 3.4(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) O(2) C(9) -31.7(3) 1_555 1_555 1_555 1_555 yes C(4) C(3) C(2) C(12) -102.8(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 41.2(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(14) -76.7(3) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(15) 160.9(3) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(7) C(6) 21.5(3) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(10) 97.1(3) 1_555 1_555 1_555 1_555 yes C(4) C(8) C(9) C(16) -133.6(3) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(7) 4.7(3) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(8) C(9) -123.4(2) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -38.2(3) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(4) C(8) -28.9(3) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 140.3(3) 1_555 1_555 1_555 1_555 yes C(7) C(6) C(5) C(13) 166.7(3) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(10) -22.4(4) 1_555 1_555 1_555 1_555 yes C(7) C(8) C(9) C(16) 107.0(4) 1_555 1_555 1_555 1_555 yes C(8) C(4) C(5) C(13) -154.8(3) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(14) 78.7(3) 1_555 1_555 1_555 1_555 yes C(8) C(7) C(6) C(15) -157.9(3) 1_555 1_555 1_555 1_555 yes C(8) C(9) C(10) C(11) -56.5(4) 1_555 1_555 1_555 1_555 yes C(11) C(1) C(2) C(12) 169.6(4) 1_555 1_555 1_555 1_555 yes C(11) C(10) C(9) C(16) 174.2(3) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(14) 48.7(4) 1_555 1_555 1_555 1_555 yes C(13) C(5) C(6) C(15) -73.6(4) 1_555 1_555 1_555 1_555 yes C(17) C(18) C(19) C(20) -89.9(3) 1_555 1_555 1_555 1_555 yes C(17) C(27) C(26) C(25) -70.9(5) 1_555 1_555 1_555 1_555 yes C(18) C(17) C(27) C(26) 44.2(6) 1_555 1_555 1_555 1_555 yes C(18) C(19) O(4) C(25) -93.4(3) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(21) -4.5(4) 1_555 1_555 1_555 1_555 yes C(18) C(19) C(20) C(24) 112.5(3) 1_555 1_555 1_555 1_555 yes C(19) O(4) C(25) C(24) -42.0(3) 1_555 1_555 1_555 1_555 yes C(19) O(4) C(25) C(26) 76.5(3) 1_555 1_555 1_555 1_555 yes C(19) O(4) C(25) C(32) -160.9(3) 1_555 1_555 1_555 1_555 yes C(19) C(18) C(17) C(27) -1.6(5) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(22) 149.4(2) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(21) C(29) -86.5(3) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(24) C(23) -142.4(3) 1_555 1_555 1_555 1_555 yes C(19) C(20) C(24) C(25) -15.5(3) 1_555 1_555 1_555 1_555 yes C(20) C(19) O(4) C(25) 31.7(3) 1_555 1_555 1_555 1_555 yes C(20) C(19) C(18) C(28) 89.6(3) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(23) -36.1(3) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(30) 81.0(3) 1_555 1_555 1_555 1_555 yes C(20) C(21) C(22) C(31) -157.6(3) 1_555 1_555 1_555 1_555 yes C(20) C(24) C(23) C(22) -7.4(4) 1_555 1_555 1_555 1_555 yes C(20) C(24) C(25) C(26) -83.9(3) 1_555 1_555 1_555 1_555 yes C(20) C(24) C(25) C(32) 147.4(4) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(24) C(23) -15.3(4) 1_555 1_555 1_555 1_555 yes C(21) C(20) C(24) C(25) 111.6(3) 1_555 1_555 1_555 1_555 yes C(21) C(22) C(23) C(24) 26.4(4) 1_555 1_555 1_555 1_555 yes C(22) C(21) C(20) C(24) 32.0(3) 1_555 1_555 1_555 1_555 yes C(22) C(23) C(24) C(25) -124.3(3) 1_555 1_555 1_555 1_555 yes C(23) C(22) C(21) C(29) -160.1(3) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(26) 34.9(4) 1_555 1_555 1_555 1_555 yes C(23) C(24) C(25) C(32) -93.8(5) 1_555 1_555 1_555 1_555 yes C(24) C(20) C(21) C(29) 156.0(3) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(30) -91.3(4) 1_555 1_555 1_555 1_555 yes C(24) C(23) C(22) C(31) 145.8(4) 1_555 1_555 1_555 1_555 yes C(24) C(25) C(26) C(27) 127.7(3) 1_555 1_555 1_555 1_555 yes C(27) C(17) C(18) C(28) 179.0(4) 1_555 1_555 1_555 1_555 yes C(27) C(26) C(25) C(32) -103.4(4) 1_555 1_555 1_555 1_555 yes C(29) C(21) C(22) C(30) -43.1(4) 1_555 1_555 1_555 1_555 yes C(29) C(21) C(22) C(31) 78.3(4) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag O(1) O(3) 2.839(3) 1_555 3_556 ? O(1) H(31) 2.92(5) 1_555 4_455 ? O(1) H(27) 3.07(3) 1_555 3_556 ? O(1) H(28) 3.07(3) 1_555 1_555 ? O(1) H(28) 3.11(3) 1_555 3_556 ? O(1) H(19) 3.27(5) 1_555 3_556 ? O(2) O(3) 2.775(3) 1_555 1_555 ? O(2) H(38) 2.84(2) 1_555 1_555 ? O(3) H(21) 3.02(4) 1_555 1_555 ? O(3) H(8) 3.04(2) 1_555 3_556 ? O(3) H(19) 3.46(5) 1_555 1_555 ? O(3) C(16) 3.562(5) 1_555 1_555 ? O(3) C(3) 3.591(3) 1_555 3_556 ? O(3) H(19) 3.60(5) 1_555 3_556 ? O(4) H(19) 2.77(5) 1_555 3_556 ? O(4) H(18) 2.88(3) 1_555 3_556 ? O(4) H(8) 3.42(2) 1_555 3_556 ? N(1) H(45) 2.80(5) 1_555 1_556 ? N(1) H(20) 3.01(4) 1_555 2_556 ? N(1) H(44) 3.04(3) 1_555 1_556 ? N(1) H(30) 3.28(4) 1_555 1_556 ? N(1) H(24) 3.33(3) 1_555 1_556 ? N(1) H(33) 3.38(4) 1_555 4_455 ? N(1) C(27) 3.514(6) 1_555 1_556 ? N(1) H(29) 3.55(3) 1_555 1_556 ? N(1) C(17) 3.584(5) 1_555 1_556 ? N(2) H(14) 2.77(4) 1_555 3_656 ? N(2) H(1) 2.87(3) 1_555 3_656 ? N(2) H(46) 2.96(5) 1_555 2_545 ? N(2) H(17) 3.20(3) 1_555 3_656 ? N(2) H(23) 3.21(4) 1_555 1_555 ? C(1) H(34) 2.85(4) 1_555 1_555 ? C(1) H(38) 3.21(2) 1_555 1_555 ? C(1) H(47) 3.29(4) 1_555 4_555 ? C(1) H(41) 3.39(3) 1_555 1_555 ? C(1) H(43) 3.48(5) 1_555 4_555 ? C(1) H(40) 3.55(5) 1_555 4_555 ? C(2) H(41) 3.09(3) 1_555 1_555 ? C(2) H(38) 3.31(2) 1_555 1_555 ? C(3) H(28) 3.06(3) 1_555 1_555 ? C(3) H(38) 3.56(2) 1_555 1_555 ? C(4) H(27) 3.54(3) 1_555 3_556 ? C(7) H(35) 3.13(6) 1_555 3_656 ? C(7) H(4) 3.40(4) 1_555 2_546 ? C(7) H(6) 3.45(4) 1_555 2_546 ? C(8) H(43) 3.56(5) 1_555 3_556 ? C(9) H(28) 3.12(3) 1_555 1_555 ? C(10) H(2) 3.27(4) 1_555 3_656 ? C(10) H(38) 3.30(2) 1_555 1_555 ? C(10) H(35) 3.46(5) 1_555 3_656 ? C(11) H(34) 3.11(4) 1_555 1_555 ? C(11) H(38) 3.49(2) 1_555 1_555 ? C(11) H(47) 3.49(4) 1_555 4_555 ? C(11) H(2) 3.58(4) 1_555 3_656 ? C(12) H(16) 2.90(3) 1_555 2_556 ? C(12) H(41) 3.06(3) 1_555 1_555 ? C(12) H(10) 3.33(3) 1_555 2_556 ? C(12) H(43) 3.47(5) 1_555 4_555 ? C(12) H(31) 3.58(4) 1_555 4_455 ? C(14) H(25) 3.02(3) 1_555 1_556 ? C(14) H(6) 3.30(4) 1_555 2_546 ? C(14) H(24) 3.43(3) 1_555 3_556 ? C(14) H(43) 3.44(5) 1_555 3_556 ? C(14) H(26) 3.55(4) 1_555 1_556 ? C(14) H(24) 3.57(3) 1_555 1_556 ? C(15) H(13) 2.85(4) 1_555 3_657 ? C(15) H(46) 3.42(5) 1_555 4_555 ? C(15) H(15) 3.46(4) 1_555 3_657 ? C(15) C(15) 3.541(8) 1_555 3_657 ? C(15) H(14) 3.56(3) 1_555 3_657 ? C(16) H(28) 3.18(3) 1_555 1_555 ? C(16) H(30) 3.25(4) 1_555 2_545 ? C(17) H(11) 2.69(3) 1_555 3_556 ? C(17) H(8) 3.20(2) 1_555 3_556 ? C(17) H(12) 3.22(4) 1_555 1_554 ? C(17) H(24) 3.34(3) 1_555 3_555 ? C(17) H(25) 3.48(4) 1_555 3_555 ? C(18) H(8) 2.86(2) 1_555 3_556 ? C(18) H(12) 3.34(4) 1_555 1_554 ? C(18) H(11) 3.41(3) 1_555 3_556 ? C(18) H(7) 3.53(3) 1_555 3_556 ? C(19) H(7) 3.25(3) 1_555 3_556 ? C(19) H(8) 3.31(2) 1_555 3_556 ? C(20) H(23) 3.51(3) 1_555 1_555 ? C(23) H(26) 3.35(4) 1_555 2_555 ? C(24) H(5) 3.53(4) 1_555 1_555 ? C(26) H(3) 3.27(3) 1_555 4_454 ? C(27) H(11) 2.86(3) 1_555 3_556 ? C(27) H(3) 3.07(3) 1_555 4_454 ? C(27) H(18) 3.58(3) 1_555 3_556 ? C(27) H(6) 3.58(4) 1_555 4_454 ? C(28) H(36) 2.98(5) 1_555 2_545 ? C(28) H(12) 3.00(4) 1_555 1_554 ? C(28) H(8) 3.11(2) 1_555 3_556 ? C(28) H(7) 3.38(3) 1_555 3_556 ? C(28) H(24) 3.56(3) 1_555 3_555 ? C(29) H(23) 3.32(4) 1_555 1_555 ? C(29) H(14) 3.50(4) 1_555 3_656 ? C(30) H(2) 3.40(4) 1_555 1_555 ? C(30) H(22) 3.43(4) 1_555 3_656 ? C(30) H(3) 3.47(3) 1_555 1_555 ? C(30) H(17) 3.59(3) 1_555 3_656 ? C(31) H(5) 3.40(4) 1_555 4_554 ? C(31) H(15) 3.45(4) 1_555 1_554 ? C(31) H(21) 3.53(4) 1_555 2_555 ? C(31) H(39) 3.57(3) 1_555 4_554 ? C(32) H(14) 3.18(4) 1_555 4_454 ? C(32) H(19) 3.41(5) 1_555 3_556 ? C(32) H(5) 3.51(4) 1_555 1_555 ? C(32) H(9) 3.57(3) 1_555 4_454 ? H(1) H(47) 3.18(5) 1_555 4_555 ? H(1) H(35) 3.39(6) 1_555 3_656 ? H(1) H(40) 3.48(6) 1_555 4_555 ? H(1) H(46) 3.56(6) 1_555 4_555 ? H(2) H(34) 2.67(5) 1_555 1_555 ? H(2) H(22) 2.75(5) 1_555 3_656 ? H(2) H(2) 3.04(8) 1_555 3_656 ? H(2) H(23) 3.07(5) 1_555 3_656 ? H(2) H(47) 3.24(6) 1_555 4_555 ? H(2) H(35) 3.40(6) 1_555 1_555 ? H(2) H(38) 3.59(4) 1_555 1_555 ? H(3) H(47) 2.58(5) 1_555 4_555 ? H(3) H(34) 2.60(5) 1_555 1_555 ? H(3) H(43) 2.65(5) 1_555 4_555 ? H(3) H(44) 2.72(5) 1_555 4_555 ? H(3) H(40) 3.19(6) 1_555 4_555 ? H(3) H(41) 3.44(4) 1_555 1_555 ? H(3) H(33) 3.57(5) 1_555 1_555 ? H(4) H(31) 3.21(6) 1_555 4_455 ? H(4) H(32) 3.39(6) 1_555 4_455 ? H(4) H(33) 3.49(6) 1_555 4_455 ? H(4) H(35) 3.55(7) 1_555 4_455 ? H(5) H(41) 2.60(5) 1_555 1_555 ? H(5) H(39) 2.63(5) 1_555 1_555 ? H(5) H(31) 2.88(6) 1_555 4_455 ? H(5) H(32) 2.89(6) 1_555 4_455 ? H(5) H(16) 3.07(5) 1_555 2_556 ? H(5) H(10) 3.27(5) 1_555 2_556 ? H(5) H(46) 3.58(6) 1_555 1_555 ? H(6) H(10) 2.64(5) 1_555 2_556 ? H(6) H(16) 2.65(5) 1_555 2_556 ? H(6) H(43) 2.69(6) 1_555 4_555 ? H(6) H(41) 3.08(5) 1_555 1_555 ? H(6) H(11) 3.20(5) 1_555 2_556 ? H(6) H(44) 3.44(5) 1_555 4_555 ? H(6) H(18) 3.50(5) 1_555 2_556 ? H(7) H(27) 2.70(5) 1_555 3_556 ? H(7) H(28) 3.02(5) 1_555 1_555 ? H(7) H(19) 3.05(6) 1_555 3_556 ? H(7) H(31) 3.10(6) 1_555 4_455 ? H(7) H(21) 3.39(5) 1_555 3_556 ? H(8) H(27) 2.62(4) 1_555 3_556 ? H(8) H(24) 3.46(4) 1_555 3_556 ? H(8) H(25) 3.48(4) 1_555 3_556 ? H(9) H(40) 2.81(6) 1_555 4_555 ? H(9) H(46) 3.52(5) 1_555 4_555 ? H(10) H(25) 2.96(5) 1_555 1_556 ? H(10) H(26) 3.27(5) 1_555 1_556 ? H(10) H(43) 3.45(6) 1_555 3_556 ? H(10) H(36) 3.51(6) 1_555 2_546 ? H(11) H(43) 2.60(5) 1_555 3_556 ? H(11) H(24) 2.61(4) 1_555 3_556 ? H(11) H(25) 2.94(5) 1_555 1_556 ? H(11) H(44) 3.01(5) 1_555 3_556 ? H(11) H(24) 3.36(4) 1_555 1_556 ? H(12) H(24) 2.77(5) 1_555 1_556 ? H(12) H(26) 2.87(5) 1_555 1_556 ? H(12) H(29) 2.99(5) 1_555 1_556 ? H(12) H(24) 3.30(5) 1_555 3_556 ? H(13) H(15) 2.66(5) 1_555 3_657 ? H(13) H(14) 2.77(5) 1_555 3_657 ? H(13) H(32) 3.02(7) 1_555 3_656 ? H(14) H(46) 2.62(6) 1_555 4_555 ? H(14) H(40) 3.21(6) 1_555 4_555 ? H(14) H(15) 3.38(5) 1_555 3_657 ? H(14) H(39) 3.44(5) 1_555 4_555 ? H(15) H(32) 2.83(6) 1_555 1_556 ? H(15) H(30) 3.17(5) 1_555 1_556 ? H(15) H(29) 3.39(5) 1_555 1_556 ? H(15) H(46) 3.41(6) 1_555 4_555 ? H(15) H(39) 3.54(5) 1_555 4_555 ? H(16) H(35) 2.86(6) 1_555 3_656 ? H(16) H(32) 3.27(6) 1_555 3_656 ? H(17) H(32) 3.52(6) 1_555 3_656 ? H(18) H(43) 2.63(5) 1_555 3_556 ? H(18) H(40) 3.48(6) 1_555 3_556 ? H(19) H(39) 2.79(6) 1_555 3_556 ? H(19) H(28) 3.10(6) 1_555 1_555 ? H(19) H(30) 3.22(6) 1_555 2_545 ? H(19) H(40) 3.25(7) 1_555 3_556 ? H(19) H(31) 3.38(6) 1_555 2_545 ? H(19) H(28) 3.48(6) 1_555 3_556 ? H(20) H(30) 3.09(5) 1_555 2_545 ? H(20) H(45) 3.51(6) 1_555 2_545 ? H(21) H(28) 2.81(5) 1_555 1_555 ? H(21) H(30) 2.95(5) 1_555 2_545 ? H(21) H(37) 3.14(5) 1_555 2_545 ? H(21) H(31) 3.24(6) 1_555 2_545 ? H(21) H(45) 3.59(6) 1_555 2_545 ? H(22) H(35) 2.59(6) 1_555 3_656 ? H(22) H(34) 3.42(5) 1_555 3_656 ? H(23) H(38) 2.63(4) 1_555 1_555 ? H(23) H(28) 3.35(5) 1_555 1_555 ? H(23) H(34) 3.37(5) 1_555 1_555 ? H(24) H(25) 2.73(5) 1_555 3_555 ? H(25) H(36) 2.88(6) 1_555 2_545 ? H(25) H(44) 3.08(5) 1_555 3_555 ? H(25) H(33) 3.59(5) 1_555 2_545 ? H(26) H(36) 2.56(6) 1_555 2_545 ? H(26) H(37) 3.23(5) 1_555 2_545 ? H(27) H(36) 2.88(6) 1_555 2_545 ? H(27) H(33) 3.24(5) 1_555 2_545 ? H(27) H(31) 3.27(5) 1_555 2_545 ? H(28) H(28) 3.53(7) 1_555 3_556 ? H(30) H(39) 3.37(5) 1_555 4_554 ? H(31) H(39) 3.41(5) 1_555 4_554 ? H(32) H(39) 3.18(6) 1_555 4_554 ? H(33) H(44) 3.25(5) 1_555 4_555 ? H(34) H(44) 3.52(5) 1_555 4_555 ? #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address' FIRST AUTHORS NAME ' ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ;