Supplementary Material (ESI) for Organic and Biomolecular Chemistry This journal is (C) The Royal Society of Chemistry 2006 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_a-2,6-diMebicyclo _database_code_depnum_ccdc_archive 'CCDC 600955' #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C16 H24 O3 ' _chemical_formula_moiety 'C16 H24 O3 ' _chemical_formula_weight 264.36 _chemical_melting_point 75C #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 8.5780(9) _cell_length_b 9.4770(9) _cell_length_c 9.818(1) _cell_angle_alpha 88.558(4) _cell_angle_beta 89.264(4) _cell_angle_gamma 73.154(4) _cell_volume 763.6(1) _cell_formula_units_Z 2 _cell_measurement_temperature 273.2 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.050 _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.077 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'MacScience DIP2030' _diffrn_reflns_number 2698 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 28.03 _diffrn_measured_fraction_theta_max 0.7315 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.7315 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2698 _reflns_number_gt 1994 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1188 _refine_ls_wR_factor_ref 0.4316 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 2520 _refine_ls_number_parameters 172 _refine_ls_goodness_of_fit_ref 1.936 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.20000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0267 _refine_diff_density_max 0.26 _refine_diff_density_min -0.37 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.3304(4) 0.5528(4) 0.7308(5) 0.082(1) Uani 1.00 d . . . O(2) O 0.8349(3) 0.0097(3) 0.8224(3) 0.0555(8) Uani 1.00 d . . . O(3) O 0.6203(4) -0.0794(4) 0.8010(5) 0.075(1) Uani 1.00 d . . . C(1) C 0.3540(5) 0.2946(5) 0.7180(5) 0.058(1) Uani 1.00 d . . . C(2) C 0.4414(8) 0.2060(7) 0.5968(6) 0.083(2) Uani 1.00 d . . . C(3) C 0.5969(7) 0.2082(6) 0.5609(5) 0.073(1) Uani 1.00 d . . . C(4) C 0.6768(7) 0.3022(7) 0.6198(6) 0.077(2) Uani 1.00 d . . . C(5) C 0.6017(5) 0.3873(5) 0.7444(5) 0.060(1) Uani 1.00 d . . . C(6) C 0.6443(5) 0.2957(5) 0.8766(5) 0.054(1) Uani 1.00 d . . . C(7) C 0.5761(5) 0.1622(5) 0.8925(4) 0.055(1) Uani 1.00 d . . . C(8) C 0.3969(5) 0.2060(5) 0.8522(5) 0.059(1) Uani 1.00 d . . . C(9) C 0.4180(5) 0.4277(5) 0.7301(5) 0.057(1) Uani 1.00 d . . . C(10) C 0.1694(6) 0.3431(7) 0.6978(9) 0.095(2) Uani 1.00 d . . . C(11) C 0.6574(7) 0.5257(7) 0.7548(9) 0.094(2) Uani 1.00 d . . . C(12) C 0.6759(5) 0.0178(5) 0.8294(5) 0.055(1) Uani 1.00 d . . . C(13) C 0.9604(5) -0.1262(4) 0.7837(4) 0.052(1) Uani 1.00 d . . . C(14) C 0.9348(7) -0.1721(7) 0.6420(6) 0.081(2) Uani 1.00 d . . . C(15) C 0.9611(6) -0.2468(6) 0.8889(5) 0.066(1) Uani 1.00 d . . . C(16) C 1.1172(6) -0.0833(5) 0.7926(6) 0.070(1) Uani 1.00 d . . . H(2) H 0.3884 0.1480 0.5472 0.0897 Uiso 1.00 calc . . . H(3) H 0.6479 0.1436 0.4894 0.0787 Uiso 1.00 calc . . . H(4A) H 0.6920 0.3712 0.5528 0.0884 Uiso 1.00 calc . . . H(4B) H 0.7845 0.2411 0.6474 0.0884 Uiso 1.00 calc . . . H(6A) H 0.6101 0.3571 0.9539 0.0598 Uiso 1.00 calc . . . H(6B) H 0.7635 0.2573 0.8824 0.0598 Uiso 1.00 calc . . . H(7) H 0.5772 0.1403 0.9878 0.0613 Uiso 1.00 calc . . . H(8A) H 0.3339 0.2623 0.9252 0.0664 Uiso 1.00 calc . . . H(8B) H 0.3638 0.1166 0.8470 0.0664 Uiso 1.00 calc . . . H(10A) H 0.1186 0.4010 0.7744 0.1062 Uiso 1.00 calc . . . H(10B) H 0.1435 0.4055 0.6177 0.1062 Uiso 1.00 calc . . . H(10C) H 0.1297 0.2622 0.6900 0.1062 Uiso 1.00 calc . . . H(11A) H 0.7750 0.4987 0.7616 0.0995 Uiso 1.00 calc . . . H(11B) H 0.6286 0.5861 0.6730 0.0995 Uiso 1.00 calc . . . H(11C) H 0.6116 0.5820 0.8305 0.0995 Uiso 1.00 calc . . . H(14A) H 0.8298 -0.1939 0.6385 0.0880 Uiso 1.00 calc . . . H(14B) H 0.9344 -0.0991 0.5768 0.0880 Uiso 1.00 calc . . . H(14C) H 1.0159 -0.2626 0.6188 0.0880 Uiso 1.00 calc . . . H(15A) H 0.8572 -0.2647 0.8894 0.0730 Uiso 1.00 calc . . . H(15B) H 1.0419 -0.3363 0.8642 0.0730 Uiso 1.00 calc . . . H(15C) H 0.9842 -0.2191 0.9757 0.0730 Uiso 1.00 calc . . . H(16A) H 1.2073 -0.1652 0.7694 0.0823 Uiso 1.00 calc . . . H(16B) H 1.1118 -0.0037 0.7311 0.0823 Uiso 1.00 calc . . . H(16C) H 1.1302 -0.0550 0.8828 0.0823 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) 0.053(2) 0.054(2) 0.130(3) -0.001(2) 0.005(2) 0.002(2) O(2) 0.037(1) 0.047(2) 0.079(2) -0.006(1) 0.001(1) -0.002(1) O(3) 0.048(2) 0.054(2) 0.124(3) -0.016(1) -0.007(2) -0.001(2) C(1) 0.045(2) 0.050(2) 0.077(3) -0.008(2) -0.007(2) 0.000(2) C(2) 0.098(4) 0.075(3) 0.072(3) -0.020(3) -0.019(3) -0.012(3) C(3) 0.070(3) 0.085(3) 0.055(2) -0.007(3) 0.004(2) -0.009(2) C(4) 0.064(3) 0.090(4) 0.066(3) -0.004(3) 0.008(2) 0.009(3) C(5) 0.044(2) 0.052(2) 0.084(3) -0.013(2) 0.003(2) 0.000(2) C(6) 0.041(2) 0.058(2) 0.062(2) -0.010(2) -0.003(2) -0.012(2) C(7) 0.041(2) 0.061(3) 0.059(2) -0.009(2) 0.001(2) 0.005(2) C(8) 0.038(2) 0.060(2) 0.079(3) -0.014(2) 0.011(2) 0.002(2) C(9) 0.049(2) 0.055(2) 0.062(2) -0.010(2) 0.001(2) 0.002(2) C(10) 0.047(3) 0.075(4) 0.161(6) -0.013(3) -0.031(3) 0.011(4) C(11) 0.061(3) 0.071(3) 0.156(6) -0.030(3) 0.005(4) 0.003(4) C(12) 0.038(2) 0.060(2) 0.066(2) -0.013(2) -0.002(2) 0.004(2) C(13) 0.039(2) 0.052(2) 0.064(2) -0.009(2) 0.004(2) -0.006(2) C(14) 0.083(4) 0.089(4) 0.066(3) -0.016(3) 0.002(3) -0.015(3) C(15) 0.052(2) 0.066(3) 0.077(3) -0.012(2) 0.007(2) 0.001(2) C(16) 0.043(2) 0.060(3) 0.107(4) -0.016(2) 0.013(2) -0.007(3) #------------------------------------------------------------------------------ _computing_data_collection Denzo _computing_cell_refinement Scalepack _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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(9) 1.206(6) . . yes O(2) C(12) 1.345(4) . . yes O(2) C(13) 1.474(5) . . yes O(3) C(12) 1.193(5) . . yes C(1) C(2) 1.532(8) . . yes C(1) C(8) 1.535(7) . . yes C(1) C(9) 1.522(6) . . yes C(1) C(10) 1.530(6) . . yes C(2) C(3) 1.381(9) . . yes C(3) C(4) 1.409(8) . . yes C(4) C(5) 1.513(8) . . yes C(5) C(6) 1.531(7) . . yes C(5) C(9) 1.518(6) . . yes C(5) C(11) 1.527(7) . . yes C(6) C(7) 1.544(6) . . yes C(7) C(8) 1.526(6) . . yes C(7) C(12) 1.529(6) . . yes C(13) C(14) 1.505(7) . . yes C(13) C(15) 1.520(7) . . yes C(13) C(16) 1.518(6) . . yes #------------------------------------------------------------------------------ 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(12) O(2) C(13) 122.2(3) . . . yes C(2) C(1) C(8) 111.3(4) . . . yes C(2) C(1) C(9) 107.4(4) . . . yes C(2) C(1) C(10) 111.0(5) . . . yes C(8) C(1) C(9) 106.2(4) . . . yes C(8) C(1) C(10) 110.1(4) . . . yes C(9) C(1) C(10) 110.8(4) . . . yes C(1) C(2) C(3) 120.2(4) . . . yes C(2) C(3) C(4) 123.6(5) . . . yes C(3) C(4) C(5) 118.7(5) . . . yes C(4) C(5) C(6) 112.7(4) . . . yes C(4) C(5) C(9) 107.7(4) . . . yes C(4) C(5) C(11) 110.1(5) . . . yes C(6) C(5) C(9) 106.6(4) . . . yes C(6) C(5) C(11) 109.1(5) . . . yes C(9) C(5) C(11) 110.6(4) . . . yes C(5) C(6) C(7) 116.3(3) . . . yes C(6) C(7) C(8) 110.4(4) . . . yes C(6) C(7) C(12) 117.0(3) . . . yes C(8) C(7) C(12) 113.0(4) . . . yes C(1) C(8) C(7) 115.9(3) . . . yes O(1) C(9) C(1) 123.0(4) . . . yes O(1) C(9) C(5) 123.5(4) . . . yes C(1) C(9) C(5) 113.5(4) . . . yes O(2) C(12) O(3) 124.8(4) . . . yes O(2) C(12) C(7) 111.3(3) . . . yes O(3) C(12) C(7) 123.6(4) . . . yes O(2) C(13) C(14) 111.9(4) . . . yes O(2) C(13) C(15) 108.7(3) . . . yes O(2) C(13) C(16) 103.0(3) . . . yes C(14) C(13) C(15) 111.6(4) . . . yes C(14) C(13) C(16) 111.3(4) . . . yes C(15) C(13) C(16) 109.9(4) . . . yes #------------------------------------------------------------------------------ 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(9) C(1) C(2) 125.2(5) . . . . yes O(1) C(9) C(1) C(8) -115.7(5) . . . . yes O(1) C(9) C(1) C(10) 3.8(7) . . . . yes O(1) C(9) C(5) C(4) -122.2(5) . . . . yes O(1) C(9) C(5) C(6) 116.6(5) . . . . yes O(1) C(9) C(5) C(11) -1.8(7) . . . . yes O(2) C(12) C(7) C(6) 27.0(5) . . . . yes O(2) C(12) C(7) C(8) 156.8(4) . . . . yes O(3) C(12) O(2) C(13) -2.8(7) . . . . yes O(3) C(12) C(7) C(6) -158.8(4) . . . . yes O(3) C(12) C(7) C(8) -29.0(6) . . . . yes C(1) C(2) C(3) C(4) -7.8(9) . . . . yes C(1) C(8) C(7) C(6) 46.8(5) . . . . yes C(1) C(8) C(7) C(12) -86.3(4) . . . . yes C(1) C(9) C(5) C(4) 59.2(5) . . . . yes C(1) C(9) C(5) C(6) -62.0(5) . . . . yes C(1) C(9) C(5) C(11) 179.6(5) . . . . yes C(2) C(1) C(8) C(7) 61.9(5) . . . . yes C(2) C(1) C(9) C(5) -56.2(5) . . . . yes C(2) C(3) C(4) C(5) 10.5(8) . . . . yes C(3) C(2) C(1) C(8) -86.5(6) . . . . yes C(3) C(2) C(1) C(9) 29.3(7) . . . . yes C(3) C(2) C(1) C(10) 150.6(5) . . . . yes C(3) C(4) C(5) C(6) 82.8(6) . . . . yes C(3) C(4) C(5) C(9) -34.6(6) . . . . yes C(3) C(4) C(5) C(11) -155.2(5) . . . . yes C(4) C(5) C(6) C(7) -65.6(5) . . . . yes C(5) C(6) C(7) C(8) -45.8(5) . . . . yes C(5) C(6) C(7) C(12) 85.3(5) . . . . yes C(5) C(9) C(1) C(8) 62.9(5) . . . . yes C(5) C(9) C(1) C(10) -177.6(5) . . . . yes C(7) C(6) C(5) C(9) 52.4(5) . . . . yes C(7) C(6) C(5) C(11) 171.9(4) . . . . yes C(7) C(8) C(1) C(9) -54.6(5) . . . . yes C(7) C(8) C(1) C(10) -174.6(4) . . . . yes C(7) C(12) O(2) C(13) 171.3(4) . . . . yes C(12) O(2) C(13) C(14) 61.3(5) . . . . yes C(12) O(2) C(13) C(15) -62.4(5) . . . . yes C(12) O(2) C(13) C(16) -179.0(4) . . . . yes C(12) O(2) C(13) C(16) -179.0(4) . . . . 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) C(16) 3.468(6) . 1_465 ? O(1) C(15) 3.548(6) . 1_465 ? O(3) C(8) 3.597(7) . 2_657 ? data_a-7-exo-Me-2,6-diMebicyclo _database_code_depnum_ccdc_archive 'CCDC 600956' #------------------------------------------------------------------------------ _audit_creation_date 'Mon May 23 21:53:09 2005' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C17 H26 O3 ' _chemical_formula_moiety 'C17 H26 O3 ' _chemical_formula_weight 278.39 _chemical_melting_point 77C #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/a ' _symmetry_Int_Tables_number 14 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 _cell_length_a 12.3010(4) _cell_length_b 11.0530(3) _cell_length_c 13.2020(4) _cell_angle_alpha 90 _cell_angle_beta 112.715(1) _cell_angle_gamma 90 _cell_volume 1655.76(9) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 #------------------------------------------------------------------------------ _exptl_crystal_description cubic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.200 _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'MacScience DIP2030' _diffrn_reflns_number 3931 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.89 _diffrn_measured_fraction_theta_max 0.9455 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.9455 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3749 _reflns_number_gt 2684 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0741 _refine_ls_wR_factor_ref 0.2924 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 3449 _refine_ls_number_parameters 181 _refine_ls_goodness_of_fit_ref 1.465 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.16700(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.2584 _refine_diff_density_max 0.18 _refine_diff_density_min -0.26 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.3728(2) 0.2960(2) 0.0938(2) 0.0725(6) Uani 1.00 d . . . O(2) O 0.1690(1) -0.0942(1) 0.2523(1) 0.0471(4) Uani 1.00 d . . . O(3) O 0.1909(2) 0.0509(2) 0.3773(1) 0.0739(6) Uani 1.00 d . . . C(1) C 0.3261(2) 0.0927(2) 0.1284(2) 0.0469(6) Uani 1.00 d . . . C(2) C 0.3975(2) 0.0254(2) 0.2335(2) 0.0526(6) Uani 1.00 d . . . C(3) C 0.4353(2) 0.0751(3) 0.3308(2) 0.0618(7) Uani 1.00 d . . . C(4) C 0.4132(2) 0.2020(3) 0.3520(2) 0.0654(8) Uani 1.00 d . . . C(5) C 0.3250(2) 0.2686(2) 0.2520(2) 0.0538(7) Uani 1.00 d . . . C(6) C 0.1946(2) 0.2370(2) 0.2302(2) 0.0547(7) Uani 1.00 d . . . C(7) C 0.1544(2) 0.1089(2) 0.1909(2) 0.0455(5) Uani 1.00 d . . . C(8) C 0.1922(2) 0.0672(2) 0.0977(2) 0.0455(5) Uani 1.00 d . . . C(9) C 0.3457(2) 0.2276(2) 0.1517(2) 0.0482(6) Uani 1.00 d . . . C(10) C 0.3659(3) 0.0528(3) 0.0375(2) 0.0760(10) Uani 1.00 d . . . C(11) C 0.3419(3) 0.4051(3) 0.2684(3) 0.082(1) Uani 1.00 d . . . C(12) C 0.1776(2) 0.0204(2) 0.2859(2) 0.0470(6) Uani 1.00 d . . . C(13) C 0.1149(2) 0.1273(3) -0.0110(2) 0.0677(7) Uani 1.00 d . . . C(14) C 0.1704(2) -0.1965(2) 0.3235(2) 0.0519(6) Uani 1.00 d . . . C(15) C 0.2837(3) -0.1991(3) 0.4255(3) 0.0787(9) Uani 1.00 d . . . C(16) C 0.0620(3) -0.1908(3) 0.3515(2) 0.0713(9) Uani 1.00 d . . . C(17) C 0.1639(3) -0.3038(3) 0.2511(3) 0.078(1) Uani 1.00 d . . . H(1) H 0.4153 -0.0580 0.2269 0.0601 Uiso 1.00 calc . . . H(2) H 0.4805 0.0245 0.3924 0.0712 Uiso 1.00 calc . . . H(3A) H 0.3808 0.2034 0.4081 0.0775 Uiso 1.00 calc . . . H(3B) H 0.4844 0.2456 0.3773 0.0775 Uiso 1.00 calc . . . H(5A) H 0.1810 0.2501 0.2952 0.0624 Uiso 1.00 calc . . . H(5B) H 0.1451 0.2903 0.1740 0.0624 Uiso 1.00 calc . . . H(6) H 0.0706 0.1141 0.1581 0.0514 Uiso 1.00 calc . . . H(7) H 0.1802 -0.0185 0.0880 0.0518 Uiso 1.00 calc . . . H(10A) H 0.3512 -0.0327 0.0229 0.0899 Uiso 1.00 calc . . . H(10B) H 0.3211 0.0947 -0.0299 0.0899 Uiso 1.00 calc . . . H(10C) H 0.4468 0.0677 0.0557 0.0899 Uiso 1.00 calc . . . H(12A) H 0.4186 0.4282 0.2775 0.1049 Uiso 1.00 calc . . . H(12B) H 0.2860 0.4461 0.2054 0.1049 Uiso 1.00 calc . . . H(12C) H 0.3267 0.4298 0.3314 0.1049 Uiso 1.00 calc . . . H(13A) H 0.1267 0.2136 -0.0036 0.0816 Uiso 1.00 calc . . . H(13B) H 0.1389 0.1009 -0.0684 0.0816 Uiso 1.00 calc . . . H(13C) H 0.0356 0.1094 -0.0290 0.0816 Uiso 1.00 calc . . . H(15A) H 0.2818 -0.2656 0.4694 0.0921 Uiso 1.00 calc . . . H(15B) H 0.3482 -0.2082 0.4026 0.0921 Uiso 1.00 calc . . . H(15C) H 0.2919 -0.1260 0.4643 0.0921 Uiso 1.00 calc . . . H(16A) H 0.0602 -0.1149 0.3868 0.0889 Uiso 1.00 calc . . . H(16B) H -0.0071 -0.1957 0.2858 0.0889 Uiso 1.00 calc . . . H(16C) H 0.0623 -0.2546 0.3992 0.0889 Uiso 1.00 calc . . . H(17A) H 0.0916 -0.2997 0.1850 0.0987 Uiso 1.00 calc . . . H(17B) H 0.2280 -0.3028 0.2261 0.0987 Uiso 1.00 calc . . . H(17C) H 0.1644 -0.3779 0.2861 0.0987 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) 0.071(1) 0.076(1) 0.073(1) -0.0221(9) 0.032(1) 0.0118(9) O(2) 0.0545(9) 0.0449(9) 0.0439(8) -0.0028(6) 0.0212(7) 0.0056(6) O(3) 0.114(2) 0.063(1) 0.057(1) -0.007(1) 0.046(1) -0.0067(8) C(1) 0.044(1) 0.055(1) 0.044(1) -0.0029(9) 0.0195(9) -0.0019(9) C(2) 0.043(1) 0.054(1) 0.057(1) 0.0081(9) 0.0140(10) 0.0054(10) C(3) 0.046(1) 0.075(2) 0.051(1) 0.007(1) 0.0048(10) 0.011(1) C(4) 0.063(2) 0.074(2) 0.047(1) -0.008(1) 0.007(1) -0.010(1) C(5) 0.055(1) 0.049(1) 0.056(1) -0.0067(10) 0.019(1) -0.0052(10) C(6) 0.057(1) 0.045(1) 0.068(1) 0.0089(10) 0.031(1) 0.002(1) C(7) 0.0364(9) 0.047(1) 0.053(1) 0.0029(8) 0.0174(9) 0.0056(8) C(8) 0.042(1) 0.051(1) 0.0377(10) -0.0057(8) 0.0092(8) 0.0043(8) C(9) 0.0372(10) 0.058(1) 0.046(1) -0.0086(9) 0.0124(9) 0.0055(9) C(10) 0.079(2) 0.094(2) 0.070(2) -0.009(2) 0.046(1) -0.015(2) C(11) 0.097(2) 0.053(2) 0.100(2) -0.016(1) 0.042(2) -0.017(1) C(12) 0.048(1) 0.052(1) 0.047(1) -0.0019(9) 0.0237(9) 0.0006(9) C(13) 0.060(1) 0.081(2) 0.045(1) -0.012(1) 0.002(1) 0.012(1) C(14) 0.051(1) 0.053(1) 0.051(1) 0.0007(9) 0.0192(10) 0.0167(10) C(15) 0.065(2) 0.088(2) 0.070(2) 0.004(1) 0.011(1) 0.027(2) C(16) 0.069(2) 0.078(2) 0.079(2) -0.003(1) 0.041(1) 0.020(1) C(17) 0.102(2) 0.048(2) 0.093(2) -0.001(1) 0.046(2) 0.007(1) #------------------------------------------------------------------------------ _computing_data_collection Denzo _computing_cell_refinement Scalepack _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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(9) 1.210(3) . . yes O(2) C(12) 1.333(3) . . yes O(2) C(14) 1.467(3) . . yes O(3) C(12) 1.201(3) . . yes C(1) C(2) 1.519(3) . . yes C(1) C(8) 1.563(3) . . yes C(1) C(9) 1.522(3) . . yes C(1) C(10) 1.526(4) . . yes C(2) C(3) 1.307(3) . . yes C(3) C(4) 1.476(4) . . yes C(4) C(5) 1.534(3) . . yes C(5) C(6) 1.556(3) . . yes C(5) C(9) 1.511(3) . . yes C(5) C(11) 1.527(4) . . yes C(6) C(7) 1.523(3) . . yes C(7) C(8) 1.544(3) . . yes C(7) C(12) 1.529(3) . . yes C(8) C(13) 1.533(3) . . yes C(14) C(15) 1.518(3) . . yes C(14) C(16) 1.516(4) . . yes C(14) C(17) 1.506(4) . . yes #------------------------------------------------------------------------------ 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(12) O(2) C(14) 122.6(2) . . . yes C(2) C(1) C(8) 109.1(2) . . . yes C(2) C(1) C(9) 107.7(2) . . . yes C(2) C(1) C(10) 109.2(2) . . . yes C(8) C(1) C(9) 107.3(2) . . . yes C(8) C(1) C(10) 111.7(2) . . . yes C(9) C(1) C(10) 111.6(2) . . . yes C(1) C(2) C(3) 123.6(2) . . . yes C(2) C(3) C(4) 124.3(2) . . . yes C(3) C(4) C(5) 114.4(2) . . . yes C(4) C(5) C(6) 112.8(2) . . . yes C(4) C(5) C(9) 107.9(2) . . . yes C(4) C(5) C(11) 109.9(2) . . . yes C(6) C(5) C(9) 106.3(2) . . . yes C(6) C(5) C(11) 108.8(2) . . . yes C(9) C(5) C(11) 111.2(2) . . . yes C(5) C(6) C(7) 116.6(2) . . . yes C(6) C(7) C(8) 113.1(2) . . . yes C(6) C(7) C(12) 112.5(2) . . . yes C(8) C(7) C(12) 116.4(2) . . . yes C(1) C(8) C(7) 110.5(2) . . . yes C(1) C(8) C(13) 112.0(2) . . . yes C(7) C(8) C(13) 110.3(2) . . . yes O(1) C(9) C(1) 123.0(2) . . . yes O(1) C(9) C(5) 123.1(2) . . . yes C(1) C(9) C(5) 113.8(2) . . . yes O(2) C(12) O(3) 124.3(2) . . . yes O(2) C(12) C(7) 111.7(2) . . . yes O(3) C(12) C(7) 123.7(2) . . . yes O(2) C(14) C(15) 111.3(2) . . . yes O(2) C(14) C(16) 109.3(2) . . . yes O(2) C(14) C(17) 102.4(2) . . . yes C(15) C(14) C(16) 112.2(2) . . . yes C(15) C(14) C(17) 110.7(2) . . . yes C(16) C(14) C(17) 110.6(2) . . . yes #------------------------------------------------------------------------------ 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(9) C(1) C(2) 130.0(2) . . . . yes O(1) C(9) C(1) C(8) -112.6(2) . . . . yes O(1) C(9) C(1) C(10) 10.1(3) . . . . yes O(1) C(9) C(5) C(4) -120.0(3) . . . . yes O(1) C(9) C(5) C(6) 118.7(2) . . . . yes O(1) C(9) C(5) C(11) 0.5(3) . . . . yes O(2) C(12) C(7) C(6) -164.9(2) . . . . yes O(2) C(12) C(7) C(8) -32.2(3) . . . . yes O(3) C(12) O(2) C(14) 2.5(3) . . . . yes O(3) C(12) C(7) C(6) 21.5(3) . . . . yes O(3) C(12) C(7) C(8) 154.2(2) . . . . yes C(1) C(2) C(3) C(4) 0.6(4) . . . . yes C(1) C(8) C(7) C(6) 49.0(2) . . . . yes C(1) C(8) C(7) C(12) -83.4(2) . . . . yes C(1) C(9) C(5) C(4) 61.5(2) . . . . yes C(1) C(9) C(5) C(6) -59.8(3) . . . . yes C(1) C(9) C(5) C(11) -178.0(2) . . . . yes C(2) C(1) C(8) C(7) 59.4(2) . . . . yes C(2) C(1) C(8) C(13) -177.1(2) . . . . yes C(2) C(1) C(9) C(5) -51.5(2) . . . . yes C(2) C(3) C(4) C(5) 9.0(4) . . . . yes C(3) C(2) C(1) C(8) -96.5(3) . . . . yes C(3) C(2) C(1) C(9) 19.7(3) . . . . yes C(3) C(2) C(1) C(10) 141.1(3) . . . . yes C(3) C(4) C(5) C(6) 79.3(3) . . . . yes C(3) C(4) C(5) C(9) -37.9(3) . . . . yes C(3) C(4) C(5) C(11) -159.2(3) . . . . yes C(4) C(5) C(6) C(7) -68.9(3) . . . . yes C(5) C(6) C(7) C(8) -46.5(3) . . . . yes C(5) C(6) C(7) C(12) 87.9(2) . . . . yes C(5) C(9) C(1) C(8) 66.0(2) . . . . yes C(5) C(9) C(1) C(10) -171.3(2) . . . . yes C(6) C(7) C(8) C(13) -75.4(2) . . . . yes C(7) C(6) C(5) C(9) 49.2(3) . . . . yes C(7) C(6) C(5) C(11) 169.0(2) . . . . yes C(7) C(8) C(1) C(9) -57.1(2) . . . . yes C(7) C(8) C(1) C(10) -179.8(2) . . . . yes C(7) C(12) O(2) C(14) -171.1(2) . . . . yes C(9) C(1) C(8) C(13) 66.4(2) . . . . yes C(10) C(1) C(8) C(13) -56.3(3) . . . . yes C(12) O(2) C(14) C(15) -59.3(3) . . . . yes C(12) O(2) C(14) C(16) 65.1(3) . . . . yes C(12) O(2) C(14) C(17) -177.6(2) . . . . yes C(12) C(7) C(8) C(13) 152.1(2) . . . . yes C(12) C(7) C(8) C(13) 152.1(2) . . . . 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) C(7) 3.364(3) . 4_555 ? data_g-3-EtO-6-(EtO2C)bicyclo _database_code_depnum_ccdc_archive 'CCDC 600957' #------------------------------------------------------------------------------ _audit_creation_date 'Fri Jul 2 21:45:00 2004' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C19 H28 O6 ' _chemical_formula_moiety 'C18 H56 O12' _chemical_formula_weight 352.43 _chemical_melting_point 78C #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 9.8930(3) _cell_length_b 11.1740(2) _cell_length_c 19.1870(7) _cell_angle_alpha 85.225(1) _cell_angle_beta 77.416(1) _cell_angle_gamma 68.107(1) _cell_volume 1920.77(10) _cell_formula_units_Z 4 _cell_measurement_temperature 273.2 #------------------------------------------------------------------------------ _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.500 _exptl_crystal_size_min 0.150 _exptl_crystal_density_diffrn 1.219 _exptl_crystal_density_method 'not measured' _exptl_absorpt_coefficient_mu 0.090 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'MacScience DIP2030' _diffrn_reflns_number 8161 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.97 _diffrn_measured_fraction_theta_max 0.8854 _diffrn_reflns_theta_full 27.97 _diffrn_measured_fraction_theta_full 0.8854 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 0.0 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 8161 _reflns_number_gt 6944 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.1225 _refine_ls_wR_factor_ref 0.4492 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 7906 _refine_ls_number_parameters 451 _refine_ls_goodness_of_fit_ref 2.132 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.20000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.1377 _refine_diff_density_max 0.34 _refine_diff_density_min -0.43 _refine_ls_extinction_method none loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 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) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O(1) O 0.4224(3) -1.0374(3) 0.9101(2) 0.0480(7) Uani 1.00 d . . . O(2) O 0.2122(3) -0.6294(3) 1.0220(2) 0.0572(9) Uani 1.00 d . . . O(3) O 0.1316(4) -1.0519(4) 0.9042(2) 0.064(1) Uani 1.00 d . . . O(4) O 0.2043(6) -1.0263(4) 0.7877(2) 0.081(1) Uani 1.00 d . . . O(5) O 0.5490(3) -0.8313(3) 0.8173(2) 0.0494(8) Uani 1.00 d . . . O(6) O 0.4707(4) -0.6328(3) 0.8648(2) 0.066(1) Uani 1.00 d . . . O(7) O 0.3415(3) -0.5365(3) 0.5937(2) 0.0494(7) Uani 1.00 d . . . O(8) O 0.2355(3) -0.1489(3) 0.4609(2) 0.0462(7) Uani 1.00 d . . . O(9) O 0.0360(4) -0.5508(3) 0.6015(2) 0.0486(8) Uani 1.00 d . . . O(10) O 0.0295(5) -0.5195(4) 0.7156(2) 0.074(1) Uani 1.00 d . . . O(11) O 0.3796(3) -0.3009(3) 0.6776(2) 0.0457(7) Uani 1.00 d . . . O(12) O 0.3433(3) -0.1194(3) 0.6114(2) 0.0513(8) Uani 1.00 d . . . C(1) C 0.2144(4) -0.8787(3) 0.8693(2) 0.0401(9) Uani 1.00 d . . . C(2) C 0.3275(4) -0.9296(3) 0.9187(2) 0.0362(8) Uani 1.00 d . . . C(3) C 0.3204(4) -0.8435(3) 0.9730(2) 0.0393(8) Uani 1.00 d . . . C(4) C 0.2206(4) -0.7206(4) 0.9776(2) 0.0442(9) Uani 1.00 d . . . C(5) C 0.1075(4) -0.6683(4) 0.9314(2) 0.052(1) Uani 1.00 d . . . C(6) C 0.1671(6) -0.6015(4) 0.8658(3) 0.061(1) Uani 1.00 d . . . C(7) C 0.3011(5) -0.6945(4) 0.8150(2) 0.050(1) Uani 1.00 d . . . C(8) C 0.2766(4) -0.8166(4) 0.8014(2) 0.0451(10) Uani 1.00 d . . . C(9) C 0.0699(4) -0.7782(4) 0.9089(2) 0.051(1) Uani 1.00 d . . . C(10) C 0.1849(4) -0.9932(4) 0.8480(2) 0.0456(10) Uani 1.00 d . . . C(11) C 0.4481(5) -0.7149(4) 0.8366(2) 0.047(1) Uani 1.00 d . . . C(12) C 0.1263(8) -1.1773(7) 0.8929(3) 0.079(2) Uani 1.00 d . . . C(13) C 0.255(1) -1.2779(7) 0.9150(5) 0.102(3) Uani 1.00 d . . . C(14) C 0.3297(6) -0.6562(4) 1.0610(3) 0.061(1) Uani 1.00 d . . . C(15) C 0.3005(8) -0.5374(6) 1.1001(5) 0.099(2) Uani 1.00 d . . . C(16) C 0.7051(5) -0.8752(4) 0.8267(2) 0.051(1) Uani 1.00 d . . . C(17) C 0.7851(7) -0.7991(7) 0.7760(4) 0.080(2) Uani 1.00 d . . . C(18) C 0.7640(6) -1.0165(5) 0.8059(3) 0.068(1) Uani 1.00 d . . . C(19) C 0.7117(5) -0.8648(5) 0.9037(3) 0.062(1) Uani 1.00 d . . . C(20) C 0.0974(3) -0.3759(3) 0.6256(2) 0.0340(8) Uani 1.00 d . . . C(21) C 0.2548(4) -0.4312(3) 0.5790(2) 0.0358(8) Uani 1.00 d . . . C(22) C 0.2971(4) -0.3533(3) 0.5206(2) 0.0375(8) Uani 1.00 d . . . C(23) C 0.2029(4) -0.2340(3) 0.5084(2) 0.0360(8) Uani 1.00 d . . . C(24) C 0.0470(3) -0.1773(3) 0.5510(2) 0.0368(8) Uani 1.00 d . . . C(25) C 0.0440(4) -0.0960(3) 0.6128(2) 0.0441(9) Uani 1.00 d . . . C(26) C 0.1319(4) -0.1765(3) 0.6673(2) 0.0387(8) Uani 1.00 d . . . C(27) C 0.0975(4) -0.2995(4) 0.6892(2) 0.0391(8) Uani 1.00 d . . . C(28) C -0.0092(4) -0.2849(3) 0.5799(2) 0.0378(8) Uani 1.00 d . . . C(29) C 0.0514(4) -0.4886(4) 0.6539(2) 0.0396(9) Uani 1.00 d . . . C(30) C 0.2964(4) -0.1946(3) 0.6471(2) 0.0387(9) Uani 1.00 d . . . C(31) C 0.0199(6) -0.6746(5) 0.6196(3) 0.062(1) Uani 1.00 d . . . C(32) C 0.169(1) -0.7783(6) 0.6024(5) 0.095(3) Uani 1.00 d . . . C(33) C 0.3903(5) -0.1754(5) 0.4283(3) 0.059(1) Uani 1.00 d . . . C(34) C 0.4035(7) -0.0551(7) 0.3951(5) 0.089(2) Uani 1.00 d . . . C(35) C 0.5417(4) -0.3361(4) 0.6722(2) 0.047(1) Uani 1.00 d . . . C(36) C 0.5665(6) -0.2367(6) 0.7128(3) 0.065(1) Uani 1.00 d . . . C(37) C 0.5837(6) -0.4669(6) 0.7080(4) 0.076(2) Uani 1.00 d . . . C(38) C 0.6217(5) -0.3461(5) 0.5950(3) 0.062(1) Uani 1.00 d . . . H(3) H 0.3839 -0.8731 1.0060 0.0421 Uiso 1.00 calc . . . H(5) H 0.0210 -0.6074 0.9579 0.0586 Uiso 1.00 calc . . . H(6A) H 0.0896 -0.5618 0.8402 0.0672 Uiso 1.00 calc . . . H(6B) H 0.1957 -0.5378 0.8815 0.0672 Uiso 1.00 calc . . . H(7) H 0.3061 -0.6506 0.7706 0.0551 Uiso 1.00 calc . . . H(8A) H 0.3682 -0.8780 0.7790 0.0507 Uiso 1.00 calc . . . H(8B) H 0.2071 -0.7949 0.7708 0.0507 Uiso 1.00 calc . . . H(9A) H 0.0006 -0.7461 0.8782 0.0574 Uiso 1.00 calc . . . H(9B) H 0.0284 -0.8164 0.9498 0.0574 Uiso 1.00 calc . . . H(12A) H 0.0353 -1.1811 0.9208 0.0889 Uiso 1.00 calc . . . H(12B) H 0.1285 -1.1859 0.8441 0.0889 Uiso 1.00 calc . . . H(13A) H 0.2484 -1.3614 0.9077 0.1192 Uiso 1.00 calc . . . H(13B) H 0.3430 -1.2751 0.8877 0.1192 Uiso 1.00 calc . . . H(13C) H 0.2495 -1.2708 0.9644 0.1192 Uiso 1.00 calc . . . H(14A) H 0.3277 -0.7242 1.0948 0.0699 Uiso 1.00 calc . . . H(14B) H 0.4227 -0.6807 1.0297 0.0699 Uiso 1.00 calc . . . H(15A) H 0.3751 -0.5519 1.1273 0.1090 Uiso 1.00 calc . . . H(15B) H 0.3025 -0.4695 1.0667 0.1090 Uiso 1.00 calc . . . H(15C) H 0.2057 -0.5121 1.1313 0.1090 Uiso 1.00 calc . . . H(17A) H 0.8850 -0.8258 0.7818 0.0915 Uiso 1.00 calc . . . H(17B) H 0.7822 -0.8108 0.7285 0.0915 Uiso 1.00 calc . . . H(17C) H 0.7360 -0.7089 0.7879 0.0915 Uiso 1.00 calc . . . H(18A) H 0.7086 -1.0595 0.8369 0.0826 Uiso 1.00 calc . . . H(18B) H 0.7561 -1.0230 0.7580 0.0826 Uiso 1.00 calc . . . H(18C) H 0.8661 -1.0546 0.8095 0.0826 Uiso 1.00 calc . . . H(19A) H 0.8125 -0.8926 0.9083 0.0715 Uiso 1.00 calc . . . H(19B) H 0.6620 -0.7768 0.9184 0.0715 Uiso 1.00 calc . . . H(19C) H 0.6644 -0.9162 0.9328 0.0715 Uiso 1.00 calc . . . H(22) H 0.3917 -0.3870 0.4904 0.0405 Uiso 1.00 calc . . . H(24) H -0.0145 -0.1231 0.5206 0.0408 Uiso 1.00 calc . . . H(25A) H 0.0850 -0.0322 0.5937 0.0479 Uiso 1.00 calc . . . H(25B) H -0.0566 -0.0536 0.6363 0.0479 Uiso 1.00 calc . . . H(26) H 0.0947 -0.1259 0.7093 0.0427 Uiso 1.00 calc . . . H(27A) H 0.0024 -0.2750 0.7194 0.0426 Uiso 1.00 calc . . . H(27B) H 0.1707 -0.3540 0.7142 0.0426 Uiso 1.00 calc . . . H(28A) H -0.0123 -0.3313 0.5414 0.0419 Uiso 1.00 calc . . . H(28B) H -0.1064 -0.2491 0.6085 0.0419 Uiso 1.00 calc . . . H(31A) H -0.0218 -0.6767 0.6687 0.0690 Uiso 1.00 calc . . . H(31B) H -0.0440 -0.6860 0.5920 0.0690 Uiso 1.00 calc . . . H(32A) H 0.1575 -0.8592 0.6138 0.1042 Uiso 1.00 calc . . . H(32B) H 0.2088 -0.7752 0.5532 0.1042 Uiso 1.00 calc . . . H(32C) H 0.2306 -0.7664 0.6300 0.1042 Uiso 1.00 calc . . . H(33A) H 0.4502 -0.2043 0.4632 0.0645 Uiso 1.00 calc . . . H(33B) H 0.4229 -0.2400 0.3924 0.0645 Uiso 1.00 calc . . . H(34A) H 0.5041 -0.0699 0.3737 0.1034 Uiso 1.00 calc . . . H(34B) H 0.3439 -0.0270 0.3598 0.1034 Uiso 1.00 calc . . . H(34C) H 0.3695 0.0095 0.4308 0.1034 Uiso 1.00 calc . . . H(36A) H 0.6701 -0.2602 0.7097 0.0716 Uiso 1.00 calc . . . H(36B) H 0.5264 -0.1548 0.6926 0.0716 Uiso 1.00 calc . . . H(36C) H 0.5185 -0.2372 0.7615 0.0716 Uiso 1.00 calc . . . H(37A) H 0.5297 -0.4582 0.7558 0.0889 Uiso 1.00 calc . . . H(37B) H 0.5590 -0.5234 0.6829 0.0889 Uiso 1.00 calc . . . H(37C) H 0.6868 -0.4999 0.7071 0.0889 Uiso 1.00 calc . . . H(38A) H 0.7249 -0.3689 0.5924 0.0714 Uiso 1.00 calc . . . H(38B) H 0.6057 -0.4102 0.5714 0.0714 Uiso 1.00 calc . . . H(38C) H 0.5838 -0.2653 0.5717 0.0714 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) 0.047(2) 0.037(1) 0.057(2) -0.005(1) -0.021(1) -0.007(1) O(2) 0.053(2) 0.048(2) 0.068(2) 0.001(1) -0.031(1) -0.026(1) O(3) 0.075(2) 0.075(2) 0.058(2) -0.045(2) -0.012(2) -0.006(1) O(4) 0.120(4) 0.095(3) 0.054(2) -0.064(3) -0.016(2) -0.019(2) O(5) 0.042(1) 0.051(2) 0.060(2) -0.017(1) -0.016(1) -0.001(1) O(6) 0.073(2) 0.046(2) 0.094(3) -0.029(1) -0.035(2) 0.002(1) O(7) 0.042(1) 0.033(1) 0.062(2) -0.0044(10) -0.006(1) 0.010(1) O(8) 0.036(1) 0.040(1) 0.056(2) -0.0112(10) -0.009(1) 0.018(1) O(9) 0.062(2) 0.047(2) 0.049(1) -0.032(1) -0.016(1) 0.006(1) O(10) 0.123(3) 0.086(3) 0.044(2) -0.074(3) -0.023(2) 0.019(2) O(11) 0.036(1) 0.046(2) 0.062(2) -0.020(1) -0.017(1) 0.010(1) O(12) 0.049(2) 0.045(2) 0.064(2) -0.024(1) -0.013(1) 0.009(1) C(1) 0.034(2) 0.045(2) 0.042(2) -0.012(1) -0.013(1) -0.010(1) C(2) 0.031(2) 0.038(2) 0.041(2) -0.011(1) -0.013(1) -0.006(1) C(3) 0.039(2) 0.039(2) 0.041(2) -0.008(1) -0.018(1) -0.005(1) C(4) 0.038(2) 0.046(2) 0.048(2) -0.008(1) -0.017(1) -0.014(1) C(5) 0.038(2) 0.052(2) 0.061(2) 0.002(1) -0.027(2) -0.018(2) C(6) 0.061(3) 0.037(2) 0.084(3) 0.002(2) -0.046(2) -0.004(2) C(7) 0.061(2) 0.042(2) 0.054(2) -0.017(2) -0.030(2) 0.009(1) C(8) 0.043(2) 0.050(2) 0.045(2) -0.013(1) -0.019(1) -0.004(1) C(9) 0.032(2) 0.060(2) 0.058(2) -0.006(1) -0.016(2) -0.019(2) C(10) 0.040(2) 0.051(2) 0.051(2) -0.016(1) -0.014(1) -0.012(1) C(11) 0.050(2) 0.041(2) 0.056(2) -0.019(1) -0.019(2) 0.007(1) C(12) 0.104(5) 0.087(4) 0.080(4) -0.067(4) -0.033(3) 0.008(3) C(13) 0.130(7) 0.066(4) 0.128(6) -0.044(4) -0.045(5) -0.006(4) C(14) 0.062(3) 0.052(2) 0.072(3) -0.005(2) -0.039(2) -0.019(2) C(15) 0.098(5) 0.071(4) 0.130(6) 0.005(3) -0.072(4) -0.045(4) C(16) 0.039(2) 0.060(2) 0.055(2) -0.020(2) -0.010(2) 0.005(2) C(17) 0.066(3) 0.104(5) 0.079(4) -0.049(3) -0.011(3) 0.025(3) C(18) 0.048(2) 0.068(3) 0.082(3) -0.011(2) -0.010(2) -0.013(2) C(19) 0.049(2) 0.070(3) 0.064(3) -0.012(2) -0.023(2) 0.005(2) C(20) 0.031(1) 0.039(2) 0.036(1) -0.015(1) -0.010(1) 0.002(1) C(21) 0.035(2) 0.031(2) 0.041(2) -0.011(1) -0.010(1) 0.000(1) C(22) 0.037(2) 0.033(2) 0.040(2) -0.011(1) -0.004(1) 0.000(1) C(23) 0.036(2) 0.034(2) 0.040(2) -0.014(1) -0.009(1) 0.005(1) C(24) 0.027(1) 0.032(2) 0.049(2) -0.007(1) -0.013(1) 0.007(1) C(25) 0.034(2) 0.031(2) 0.064(2) -0.006(1) -0.012(1) -0.002(1) C(26) 0.035(2) 0.035(2) 0.046(2) -0.012(1) -0.007(1) -0.008(1) C(27) 0.038(2) 0.047(2) 0.036(2) -0.019(1) -0.005(1) -0.003(1) C(28) 0.030(2) 0.043(2) 0.042(2) -0.015(1) -0.010(1) 0.005(1) C(29) 0.042(2) 0.043(2) 0.042(2) -0.023(1) -0.014(1) 0.007(1) C(30) 0.037(2) 0.036(2) 0.048(2) -0.015(1) -0.014(1) -0.002(1) C(31) 0.079(3) 0.058(3) 0.071(3) -0.046(2) -0.023(2) 0.006(2) C(32) 0.132(6) 0.046(3) 0.117(6) -0.034(3) -0.040(5) 0.006(3) C(33) 0.041(2) 0.055(2) 0.070(3) -0.014(2) 0.000(2) 0.019(2) C(34) 0.058(3) 0.080(4) 0.122(5) -0.031(3) -0.009(3) 0.043(4) C(35) 0.032(2) 0.050(2) 0.062(2) -0.016(1) -0.017(2) 0.006(2) C(36) 0.059(3) 0.077(3) 0.074(3) -0.038(2) -0.024(2) 0.003(2) C(37) 0.056(3) 0.064(3) 0.111(5) -0.020(2) -0.038(3) 0.032(3) C(38) 0.038(2) 0.075(3) 0.071(3) -0.017(2) -0.013(2) -0.005(2) #------------------------------------------------------------------------------ _computing_data_collection Denzo _computing_cell_refinement Scalepack _computing_data_reduction 'teXsan Ver. 1.11' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.11' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _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(2) 1.217(4) . . yes O(2) C(4) 1.349(4) . . yes O(2) C(14) 1.444(5) . . yes O(3) C(10) 1.328(6) . . yes O(3) C(12) 1.457(6) . . yes O(4) C(10) 1.198(5) . . yes O(5) C(11) 1.333(5) . . yes O(5) C(16) 1.484(5) . . yes O(6) C(11) 1.213(5) . . yes O(7) C(21) 1.224(4) . . yes O(8) C(23) 1.340(4) . . yes O(8) C(33) 1.449(5) . . yes O(9) C(29) 1.335(4) . . yes O(9) C(31) 1.456(5) . . yes O(10) C(29) 1.203(5) . . yes O(11) C(30) 1.341(4) . . yes O(11) C(35) 1.483(4) . . yes O(12) C(30) 1.202(4) . . yes C(1) C(2) 1.540(4) . . yes C(1) C(8) 1.542(6) . . yes C(1) C(9) 1.535(5) . . yes C(1) C(10) 1.519(5) . . yes C(2) C(3) 1.449(4) . . yes C(3) C(4) 1.356(5) . . yes C(4) C(5) 1.496(5) . . yes C(5) C(6) 1.530(8) . . yes C(5) C(9) 1.526(6) . . yes C(6) C(7) 1.538(7) . . yes C(7) C(8) 1.523(5) . . yes C(7) C(11) 1.530(6) . . yes C(12) C(13) 1.47(1) . . yes C(14) C(15) 1.480(6) . . yes C(16) C(17) 1.524(6) . . yes C(16) C(18) 1.520(7) . . yes C(16) C(19) 1.509(7) . . yes C(20) C(21) 1.541(4) . . yes C(20) C(27) 1.547(4) . . yes C(20) C(28) 1.540(4) . . yes C(20) C(29) 1.513(4) . . yes C(21) C(22) 1.447(4) . . yes C(22) C(23) 1.348(5) . . yes C(23) C(24) 1.503(5) . . yes C(24) C(25) 1.542(5) . . yes C(24) C(28) 1.521(5) . . yes C(25) C(26) 1.520(5) . . yes C(26) C(27) 1.540(5) . . yes C(26) C(30) 1.528(5) . . yes C(31) C(32) 1.48(1) . . yes C(33) C(34) 1.477(7) . . yes C(35) C(36) 1.527(6) . . yes C(35) C(37) 1.512(6) . . yes C(35) C(38) 1.510(7) . . yes #------------------------------------------------------------------------------ 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) O(2) C(14) 118.6(3) . . . yes C(10) O(3) C(12) 117.7(4) . . . yes C(11) O(5) C(16) 123.5(3) . . . yes C(23) O(8) C(33) 118.1(3) . . . yes C(29) O(9) C(31) 116.8(3) . . . yes C(30) O(11) C(35) 122.6(3) . . . yes C(2) C(1) C(8) 111.2(3) . . . yes C(2) C(1) C(9) 109.9(3) . . . yes C(2) C(1) C(10) 107.4(3) . . . yes C(8) C(1) C(9) 109.0(3) . . . yes C(8) C(1) C(10) 109.0(3) . . . yes C(9) C(1) C(10) 110.3(3) . . . yes O(1) C(2) C(1) 120.2(3) . . . yes O(1) C(2) C(3) 121.9(3) . . . yes C(1) C(2) C(3) 117.9(3) . . . yes C(2) C(3) C(4) 120.4(3) . . . yes O(2) C(4) C(3) 125.4(3) . . . yes O(2) C(4) C(5) 111.3(3) . . . yes C(3) C(4) C(5) 123.3(3) . . . yes C(4) C(5) C(6) 110.1(4) . . . yes C(4) C(5) C(9) 109.4(3) . . . yes C(6) C(5) C(9) 110.5(3) . . . yes C(5) C(6) C(7) 113.4(3) . . . yes C(6) C(7) C(8) 112.0(4) . . . yes C(6) C(7) C(11) 111.9(3) . . . yes C(8) C(7) C(11) 115.8(3) . . . yes C(1) C(8) C(7) 114.3(3) . . . yes C(1) C(9) C(5) 107.9(3) . . . yes O(3) C(10) O(4) 123.3(4) . . . yes O(3) C(10) C(1) 112.2(3) . . . yes O(4) C(10) C(1) 124.5(4) . . . yes O(5) C(11) O(6) 124.9(4) . . . yes O(5) C(11) C(7) 111.2(3) . . . yes O(6) C(11) C(7) 123.8(4) . . . yes O(3) C(12) C(13) 108.6(5) . . . yes O(2) C(14) C(15) 107.5(4) . . . yes O(5) C(16) C(17) 108.9(4) . . . yes O(5) C(16) C(18) 102.0(4) . . . yes O(5) C(16) C(19) 111.1(3) . . . yes C(17) C(16) C(18) 112.0(5) . . . yes C(17) C(16) C(19) 112.9(5) . . . yes C(18) C(16) C(19) 109.4(4) . . . yes C(21) C(20) C(27) 110.5(3) . . . yes C(21) C(20) C(28) 109.0(3) . . . yes C(21) C(20) C(29) 107.5(3) . . . yes C(27) C(20) C(28) 109.1(3) . . . yes C(27) C(20) C(29) 109.2(3) . . . yes C(28) C(20) C(29) 111.5(3) . . . yes O(7) C(21) C(20) 119.6(3) . . . yes O(7) C(21) C(22) 122.0(3) . . . yes C(20) C(21) C(22) 118.3(3) . . . yes C(21) C(22) C(23) 120.9(3) . . . yes O(8) C(23) C(22) 125.9(3) . . . yes O(8) C(23) C(24) 111.2(3) . . . yes C(22) C(23) C(24) 122.8(3) . . . yes C(23) C(24) C(25) 109.7(3) . . . yes C(23) C(24) C(28) 109.7(3) . . . yes C(25) C(24) C(28) 110.4(3) . . . yes C(24) C(25) C(26) 112.8(3) . . . yes C(25) C(26) C(27) 112.6(3) . . . yes C(25) C(26) C(30) 112.5(3) . . . yes C(27) C(26) C(30) 116.0(3) . . . yes C(20) C(27) C(26) 114.0(3) . . . yes C(20) C(28) C(24) 108.6(3) . . . yes O(9) C(29) O(10) 123.0(3) . . . yes O(9) C(29) C(20) 111.7(3) . . . yes O(10) C(29) C(20) 125.3(3) . . . yes O(11) C(30) O(12) 124.8(3) . . . yes O(11) C(30) C(26) 111.1(3) . . . yes O(12) C(30) C(26) 124.0(3) . . . yes O(9) C(31) C(32) 108.6(4) . . . yes O(8) C(33) C(34) 108.2(4) . . . yes O(11) C(35) C(36) 108.9(3) . . . yes O(11) C(35) C(37) 101.7(3) . . . yes O(11) C(35) C(38) 110.9(3) . . . yes C(36) C(35) C(37) 112.1(4) . . . yes C(36) C(35) C(38) 111.8(4) . . . yes C(37) C(35) C(38) 111.0(4) . . . yes #------------------------------------------------------------------------------ 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(2) C(1) C(8) -86.3(4) . . . . yes O(1) C(2) C(1) C(9) 152.9(4) . . . . yes O(1) C(2) C(1) C(10) 32.8(5) . . . . yes O(1) C(2) C(3) C(4) 174.8(4) . . . . yes O(2) C(4) C(3) C(2) -174.4(4) . . . . yes O(2) C(4) C(5) C(6) 84.4(4) . . . . yes O(2) C(4) C(5) C(9) -154.0(4) . . . . yes O(3) C(10) C(1) C(2) 59.2(4) . . . . yes O(3) C(10) C(1) C(8) 179.7(3) . . . . yes O(3) C(10) C(1) C(9) -60.6(4) . . . . yes O(4) C(10) O(3) C(12) 13.3(7) . . . . yes O(4) C(10) C(1) C(2) -122.1(5) . . . . yes O(4) C(10) C(1) C(8) -1.6(6) . . . . yes O(4) C(10) C(1) C(9) 118.1(5) . . . . yes O(5) C(11) C(7) C(6) 150.8(4) . . . . yes O(5) C(11) C(7) C(8) 20.8(5) . . . . yes O(6) C(11) O(5) C(16) -1.3(7) . . . . yes O(6) C(11) C(7) C(6) -32.3(6) . . . . yes O(6) C(11) C(7) C(8) -162.3(4) . . . . yes O(7) C(21) C(20) C(27) 87.5(4) . . . . yes O(7) C(21) C(20) C(28) -152.6(3) . . . . yes O(7) C(21) C(20) C(29) -31.6(4) . . . . yes O(7) C(21) C(22) C(23) -175.6(3) . . . . yes O(8) C(23) C(22) C(21) 172.7(3) . . . . yes O(8) C(23) C(24) C(25) -82.4(4) . . . . yes O(8) C(23) C(24) C(28) 156.1(3) . . . . yes O(9) C(29) C(20) C(21) -66.0(4) . . . . yes O(9) C(29) C(20) C(27) 174.1(3) . . . . yes O(9) C(29) C(20) C(28) 53.5(4) . . . . yes O(10) C(29) O(9) C(31) -12.0(6) . . . . yes O(10) C(29) C(20) C(21) 114.7(5) . . . . yes O(10) C(29) C(20) C(27) -5.2(5) . . . . yes O(10) C(29) C(20) C(28) -125.8(5) . . . . yes O(11) C(30) C(26) C(25) -156.0(3) . . . . yes O(11) C(30) C(26) C(27) -24.4(4) . . . . yes O(12) C(30) O(11) C(35) 1.6(6) . . . . yes O(12) C(30) C(26) C(25) 27.6(5) . . . . yes O(12) C(30) C(26) C(27) 159.3(4) . . . . yes C(1) C(2) C(3) C(4) -2.5(6) . . . . yes C(1) C(8) C(7) C(6) -46.3(4) . . . . yes C(1) C(8) C(7) C(11) 83.7(4) . . . . yes C(1) C(9) C(5) C(4) -58.2(5) . . . . yes C(1) C(9) C(5) C(6) 63.1(4) . . . . yes C(1) C(10) O(3) C(12) -168.0(4) . . . . yes C(2) C(1) C(8) C(7) -65.8(4) . . . . yes C(2) C(1) C(9) C(5) 59.6(4) . . . . yes C(2) C(3) C(4) C(5) 3.7(7) . . . . yes C(3) C(2) C(1) C(8) 91.1(4) . . . . yes C(3) C(2) C(1) C(9) -29.7(5) . . . . yes C(3) C(2) C(1) C(10) -149.7(3) . . . . yes C(3) C(4) O(2) C(14) 9.3(7) . . . . yes C(3) C(4) C(5) C(6) -93.9(5) . . . . yes C(3) C(4) C(5) C(9) 27.7(6) . . . . yes C(4) O(2) C(14) C(15) 175.0(6) . . . . yes C(4) C(5) C(6) C(7) 66.0(4) . . . . yes C(5) C(4) O(2) C(14) -169.0(4) . . . . yes C(5) C(6) C(7) C(8) 45.5(4) . . . . yes C(5) C(6) C(7) C(11) -86.5(4) . . . . yes C(5) C(9) C(1) C(8) -62.5(4) . . . . yes C(5) C(9) C(1) C(10) 177.8(3) . . . . yes C(7) C(6) C(5) C(9) -55.0(4) . . . . yes C(7) C(8) C(1) C(9) 55.5(4) . . . . yes C(7) C(8) C(1) C(10) 176.0(3) . . . . yes C(7) C(11) O(5) C(16) 175.6(3) . . . . yes C(10) O(3) C(12) C(13) 99.6(7) . . . . yes C(11) O(5) C(16) C(17) -68.7(5) . . . . yes C(11) O(5) C(16) C(18) 172.8(4) . . . . yes C(11) O(5) C(16) C(19) 56.3(5) . . . . yes C(20) C(21) C(22) C(23) 1.9(5) . . . . yes C(20) C(27) C(26) C(25) 46.4(4) . . . . yes C(20) C(27) C(26) C(30) -85.2(4) . . . . yes C(20) C(28) C(24) C(23) 57.9(4) . . . . yes C(20) C(28) C(24) C(25) -63.2(3) . . . . yes C(20) C(29) O(9) C(31) 168.7(4) . . . . yes C(21) C(20) C(27) C(26) 66.0(4) . . . . yes C(21) C(20) C(28) C(24) -59.2(3) . . . . yes C(21) C(22) C(23) C(24) -3.7(5) . . . . yes C(22) C(21) C(20) C(27) -90.0(4) . . . . yes C(22) C(21) C(20) C(28) 29.9(4) . . . . yes C(22) C(21) C(20) C(29) 150.9(3) . . . . yes C(22) C(23) O(8) C(33) -11.9(6) . . . . yes C(22) C(23) C(24) C(25) 94.4(4) . . . . yes C(22) C(23) C(24) C(28) -27.0(5) . . . . yes C(23) O(8) C(33) C(34) -164.0(5) . . . . yes C(23) C(24) C(25) C(26) -65.1(4) . . . . yes C(24) C(23) O(8) C(33) 164.9(4) . . . . yes C(24) C(25) C(26) C(27) -46.6(4) . . . . yes C(24) C(25) C(26) C(30) 86.7(3) . . . . yes C(24) C(28) C(20) C(27) 61.5(3) . . . . yes C(24) C(28) C(20) C(29) -177.8(3) . . . . yes C(26) C(25) C(24) C(28) 55.9(4) . . . . yes C(26) C(27) C(20) C(28) -53.8(4) . . . . yes C(26) C(27) C(20) C(29) -175.9(3) . . . . yes C(26) C(30) O(11) C(35) -174.7(3) . . . . yes C(29) O(9) C(31) C(32) -94.0(5) . . . . yes C(30) O(11) C(35) C(36) 67.0(5) . . . . yes C(30) O(11) C(35) C(37) -174.4(4) . . . . yes C(30) O(11) C(35) C(38) -56.4(5) . . . . yes C(30) O(11) C(35) C(38) -56.4(5) . . . . 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) C(14) 3.473(5) . 2_637 ? O(1) C(3) 3.569(4) . 2_637 ? O(4) C(30) 3.185(5) . 1_545 ? O(4) C(26) 3.306(5) . 1_545 ? O(4) O(12) 3.450(5) . 1_545 ? O(4) O(11) 3.521(5) . 1_545 ? O(4) C(36) 3.531(8) . 1_545 ? O(6) C(37) 3.590(7) . . ? O(7) C(33) 3.309(5) . 2_646 ? O(7) C(22) 3.585(4) . 2_646 ? O(8) C(25) 3.543(4) . 2_556 ? O(10) C(6) 3.366(6) . . ? O(10) C(7) 3.517(6) . . ? O(12) C(32) 3.557(7) . 1_565 ? #------------------------------------------------------------------------------ #------------------------------------------------------------------------------